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The structure determination of three inorganic and two organic compounds by x-ray diffraction Mercer, Anthony 1977

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THE  STRUCTURE DETERMISATION OF THREE  INORGANIC AND TWO  ORGANIC COMPOUNDS  BY X-RAY DIFFRACTION.  By  ANTHONY MERCER.  .Sc.,  University  of Bristol,  E n g l a n d , 1972.  A THESIS SUBMITTED IN PARTIAL FULFILMENT OF THE REQUIREMENTS  FOR THE DEGREE OF  DOCTOR OF PHILOSOPHY  i n t h e department of CHEMISTRY.  We a c c e p t t h i s t h e s i s the  THE  reguired  as conforming t o standard.  UNIVERSITY OF BRITISH  JUNE  1977.  (c) Anthony Mercer, 1977  COLUMBIA  In p r e s e n t i n g t h i s  thesis  an advanced degree at the L i b r a r y s h a l l I  in p a r t i a l  f u l f i l m e n t o f the requirements f o r  the U n i v e r s i t y of B r i t i s h Columbia,  make i t  freely available  f u r t h e r agree t h a t p e r m i s s i o n  for  I agree  that  reference and study.  f o r e x t e n s i v e copying o f  this  thesis  f o r s c h o l a r l y purposes may be granted by the Head of my Department or by h i s of  representatives.  this  thesis  It  i s understood that copying or p u b l i c a t i o n  f o r f i n a n c i a l gain s h a l l  written permission.  Department of  C m CWwSTft^f  The U n i v e r s i t y o f B r i t i s h  2075 Wesbrook Place Vancouver, Canada V6T 1W5  Date  4  Columbia  not be allowed without my  abstract  T h i s t h e s i s deals with the c u r r e n t methods a v a i l a b l e f o r X-ray  structure  molecular  determination  structure  and  with  determination  of  the  crystal  f i v e compounds  and using  these methods. The f i v e compounds are 1)  [ 2,3-Bis ( d i m e t h y l a r s i n o ) - 1, 1, 1,4, 4, 4-hexaf l u o r o b u t 2~ene-As,As3tricarbonyldiiodotungsten(II), Me^AsC (CF j~:C (CF^) AsBe*WXx (CO) 3  2)  3  Dimethylammonium t r i c h l o r o t r i s ( d i m e t h y l s u l p h o x i d e } ruthenate(II) , [ ( (CE ) SQ) R u C l r [ ( C H ^ i NH J+ %  3)  t  a  %  a  Dichlorotetrakis{dimethylsulphoxide)ruthenium(II), (Me SO)v RuCl 1  4)  f  x  1,3,7-Triraethyl-2,6-dioxypuriae h y d r o c h l o r i d e dihydrate (caffeine hydrochloride dihydrate), C H ClN 0 .lH 0 8  .5)  n  lf  1  1  1-Acetyl-3-benzamido-2-keto-4- (2,3, 4, 6 - t e t r a - O - a c e t y l P-D-glucopyranosyloxy)-k -pyrroline, 3  The  structures  determined  by  of  compounds  Patterson  syntheses,  centrosymmetric  direct  methods  centrosymmetric  direct  methods.  refined relevant  using  1 ) , 2 ) , and  full-matrix  and  3)  compound  compound  4)  5)  by  A l l structures  least-sguares  were by non-  were then  procedures.  The  c r y s t a l data f o r a l l f i v e compounds can be found i n  Table A In the tungsten seven-coordinate  compound [ 1 ) ]  with  environment, t h e capping  a  distorted  arsenic  atoms  from  tungsten capped  group being a c a r b o n y l .  f a c e c o n s i s t s of the two remaining the  the  atom i s octahedral  The  capped  c a r b o n y l groups and one o f  the b i d e n t a t e l i g a n d . The uncapped  f a c e c o n t a i n s the two i o d i n e atoms and the remaining  arsenic  iii  Table.A  C r y s t a l data f o r t h e f i v e compounds examined  Final R Factor  U n i t C e l l Dimensions  Space Group  90.0 112.03 (2) — 90.0  £2,/c  a = 15.37 (2) 9.52 9(1) b c = 15. 967(3)  ££2, a  a b c  £2 /n  8.9 39(3) a = 18.045(7) b 1 1.363(3) c  1  4)  £2,/c  a — 12.391 (4) 6.52 4(1) b c = 17. 167(6)  I  5)  P2  19.629(5) a b = 7.504(2) c 9.830(2)  = 90.0 = 90.53(2) tt = 90.0  2)  3)  4  4  I I  27.45 9(5) 9.925(1) 14.266(3)  0. 067  90.0  0. 045  = 90.0 —  =  90.0  90.0 91.52 (2) 90.0  0. 041  90.0 118.82 (3) 90.0  0. 064  1  0. 079  atom. The s t r u c t u r e of the ruthenium compound [ 2) of  two  crystallcgraphically  asymmetric  unit  dimethylammonium structurally  linked  non-equivalent by  hydrogen  ]  consists  anions  i n the  bonding  via  c a t i o n s . The c o o r d i n a t i o n geometry about the  similar  anions  is  essentially  that  octahedron with the DHSO l i g a n d s being bonded t o Ru  of via  an the  sulphur atoms. The  co-ordination  compound 3)  is  geometry about the ruthenium atom f o r  essentially  octahedral  with  cis  chlorine  atoms; Of the f o u r DMSO l i g a n d s three are S-bonded and one i s O-bonded, ligand.  the  O-bonded  ligand  being  trans  t o a S-bonded  For c a f f e i n e hydrochloride is  essentially  crystal  contains  H...C1 and The in in  the  planar two  and  types  ] the  protonated  fused  a t the  ring  system  9-positioh.  The  involving  0-  of hydrogen bonding  N-H...0 i n t e r a c t i o n s .  s t r u c t u r e o f compound 5)  c h a i r conformation  with  e q u a t o r i a l p o s i t i o n s ; the  planar  [ 4)  pyrroline ring  the  c o n s i s t s of a four 0-acetyl  pyranose  v i a a £-oxygen  ring  bridge.  pyranose  ring  substituents  i s connected  to  a  V  TABLE OF CONTENTS  Pag e TITLE PAGE ..............................................  i  ABSTRACT  i i  TftBLE OF CONTENTS ....................................... LIST OF TABLES .,  v viii  LIST OF FIGURES ..........................  ............  ACKNOWLEDGEMENTS  xi xiii  GENERAL INTRODUCTION  1  CHAPTER 1. AN INTRODUCTION TO X-RAY CRYSTALLOGRAPHY .....  4  k)  CHAPTER  ........................  5  B) A t h e o r e t i c a l viewpoint ......................  14  2.  A p r a c t i c a l viewpoint  CRYSTAL  AND  MOLECULAR  STRUCTURE  OF  [2,3-  BIS(DIHETHYLARSINO)-1,1,1,4,4,4-HEXAFLUOROBUT-2-ENEAS, AS]TRICARBONYL DIIODOTUNGSTEN(II) ..................... Introduction  ....................................  16 17  Experimental  17  S t r u c t u r e a a a l y s i s ..............................  18  Results  26  and d i s c u s s i o n ..........................  vi  CHS.PTES  3.  CRYSTAL  AND  MOLECULAR  STRUCTURE  OF DIMETHYL-  AMMONIUM TRICHLO 80TRIS (DIMETHYLS ULPH OXIDE) BOTH EN AT E (II)  CHAPTER  .  Introduction  40  Experimental  40  S t r u c t u r e a n a l y s i s ..............................  41  R e s u l t s and d i s c u s s i o n ..........................  46  4.  CRYSTAL  AND  MOLECULAR  STRUCTURE  OF  DICHLOROTETRAKIS(DIM ETHYLSULPHOXIDE) ROTH ENIUM (II) ...... .  CHAPTER  39  53  Introduction  54  Experimental ....................................  54  S t r u c t u r e a n a l y s i s ..............................  55  R e s u l t s and d i s c u s s i o n  59  5.  CRYSTAL  AND  MOLECULAR  TRIMETHYL-2,6-DIOXYPURIN E HYDROCHLORIDE  STRUCTURE DIHYDRATE  OF  1,3,7-  (CAFFEINE  HYDROCHLORIDE DIHYDRATE)  69  I n t r o d u c t i o n ....................................  70  Experimental  70  Structure analysis  71  A n a l y s i s of thermal motion ......................  77  R e s u l t s and d i s c u s s i o n  84  vii  CHAPTER  6.  CRYSTAL  AND  MOLECULAR STRUCTURE OF 1—ACETYL-3-  BENZAMIDO-2-KETO-4- (2,4, 4, 6-TETRA-O-ACETYL-p-DGLUCOPYRANOSYLOXY)-& —PYRROLINE  92  3  Introduction  ....................................  93  Experimental  93  S t r u c t u r e a n a l y s i s ..............................  94  R e s u l t s and d i s c u s s i o n .......................... 100  SUMMARY  REFERENCES .................................  113  ..117  viii  LIST OF TABLES  Table  Page  [2, 3-Bis ( d i m e t h y l a r s i n o ) - 1,1, 1, 4, 4, 4-hexaf luorobut-2-eneAs, A s ] t r i c a r b o n y l d i i o d o t u n g s t e n (II)  1  The i n t e r a t o m i c v e c t o r s and the s o l u t i o n t o the Patterson  2  function  »••••  •  22  C r y s t a l dimensions and face i n d i c e s f o r the absorption  correction  24  3  F i n a l atomic c o o r d i n a t e s  28  4  F i n a l thermal parameters .........................  29  5  Bond l e n g t h s  32  6  Bond angles  ......................................  33  7  Mean planes  ......................................  36  Dimethylammonium t r i c h l o r o t r i s { d i m e t h y l s u l p h o x i d e ) ruthenate (II)  8  F i n a l atomic c o o r d i n a t e s  .........................  44  9  F i n a l t h e r n a l parameters  45  10  Bond l e n g t h s .....................................  48  11  Bond angles  49  12  Non-bonded c o n t a c t s  51  i x  D i c h l o r o t e t r a k i s (dimethylsulphoxide) ruthenium (II)  13  F i n a l atomic c o o r d i n a t e s  57  14  F i n a l thermal  58  15  Bond l e n g t h s  61  16  Bond a n g l e s  62  17  Mean planes ......................................  63  18  Comparison of the s t r u c t u r a l  parameters .........................  data f o r some  d i m e t h y l s u l p h o x i d e complexes .....................  1,3,7-Trimethy1-2,6-dioxypurine  66  hydrochloride dihydrate  ( C a f f e i n e h y d r o c h l o r i d e dihydrate)  19  Starting  s e t of r e f l e c t i o n s  74  20  R e s u l t s o f the phase d e t e r m i n a t i o n procedure  21  F i n a l atomic  22  F i n a l thermal  23  B i g i d body thermal parameters ....................  81  24  Bond l e n g t h s  82  25  Bond a n g l e s  83  26  Structural  27  Mean planes  89  28  Non-bonded c o n t a c t s ..............................  90  ..... 76  coordinates parameters .........................  data f o r some purine d e r i v a t i v e s  78 79  87  X  1-Acetyl-3-benzamido-2- keto-4- ( 2 , 4 , a ,6-tetra-O-acetyl-^-Dglticopyranosyloxy)  pyrroline  29  S t a r t i n g set of r e f l e c t i o n s .  96  30  R e s u l t s of t h e phase d e t e r m i n a t i o n procedure ..... 9 7  31  F i n a l atomic c o o r d i n a t e s ......................... 1 0 2  32  F i n a l thermal parameters .........................  33  Bond l e n g t h s  34  Bond a n g l e s ...................................... 1 0 6  35  Mean p l a n e s  36  S t r u c t u r a l data f o r some pyranose r i n g s .......... 10 9  37  Non-bonded c o n t a c t s  10 4 105  107  .............................. 1 1 1  xi  LIST  OF FIGURES  Figure  Page Introduction  1  The s p h e r e o f r e f l e c t i o n  2  Flow c h a r t  of p r a c t i c a l  8 crystallography  ..........  13  [2,3-Bis{dimethylarsino)~1,1,1,4,4,4-hexafluorobut-2-eneA s , A s ] t r i c a r b o n y l d i i o d o t u n g s t e n (II)  3  S c h e m a t i c d i a g r a m o f compounds  4  View  |1) and (2)  o f t h e m o l e c u l e down t h e c a p p i n g  w i t h t h e c a r b o n y l g r o u p removed  26  c a r b o n y l group  ..................  27  5  A s t e r e o v i e w o f t h e molecule .....................  31  6  The s t r u c t u r e v i e w e d  37  down  b ......................  Dimethylammonium t r i c h l o r o t r i s ( d i m e t h y l s u l p h o x i d e ) r u t h e n a t e (II)  7  A g e n e r a l view o f t h e s t r u c t u r e . . . . . . . . . . . . . . . . . .  47  8  The s t r u c t u r e v i e w e d down c . . . . . . . . . . . . . . . . . . . . . .  52  D i c h l o r o t e t r a k i s (dimethylsulphoxide) ruthenium(II)  9 10  A g e n e r a l view o f t h e s t r u c t u r e  60  The s t r u c t u r e v i e w e d  67  down b . . . . . . . . . . . . . . . . . . . . . .  xii  1,3,7-Trimethyl-2,6-dioxypurine  hydrochloride  (Caffeine hydrochloride  dihydrate  dihydrate)  11  A g e n e r a l view of the s t r u c t u r e ..................  80  12  Comparison of s e v e r a l i m i d a z o l e r i n g compounds ...  85  13  The s t r u c t u r e viewed down b ......................  91  1-Acetyl-3-benzamido-2-keto-4-(2,4,4,6-tetra-O-acetyl-p-Dglucopyranosyloxy ) - A - p y r r o l i n e 3  14  (A) A stereoview  of the s t r u c t u r e  (B) The c o n v e n t i o n a l chemical 15  101  s t r u c t u r e ..........101  The s t r u c t u r e viewed down b ...................... 112  ACKNOWLEDGEMENTS  I wish Trotter  to  express  my  gratitude  to  Professor  f o r h i s h e l p and guidance throughout  James  a l l stages of  t h i s work. I am a l s o i n d e b t e d t o my fellow postdoctoral  fellows  graduate  students  who have aided me a t a l l times, and i n  p a r t i c u l a r t o Dr. Steven R e t t i g , f o r h i s a s s i s t a n c e later  stages  of  and  t h e work  and  i n the  i n the p r e p a r a t i o n of t h i s  thesis. I would a l s o l i k e t o  thank  Dr.  L.  Mihichuk  f o r the  tungsten  crystals  (Chapter  ruthenium  compounds  (Chapters 3 and 4), Dr. D. Lenard f o r the  c a f f e i n e compound pyrroline I  am  (Chapter 5 ) ,  2 ) , Dr. R. McMillan f o r the two  and  Dr.  A.  Brink  f o r the  crystals. grateful  to  support i n the form of  a  t h e K i l l a m Foundation postgraduate  for financial  scholarship  i n the  years 1973-1974 and 1974-1975. F i n a l l y , I am very g r a t e f u l t o a l l the Canadian  people I  have met who have made the past f i v e years such happy ones.  1  GENES AL INTRODUCTION  2  This  thesis  deals  principally  d e t e r m i n a t i o n by s i n g l e c r y s t a l compounds  with  X-ray  the  structure  diffraction  of  i n t h e i r c r y s t a l l i n e s t a t e . I t i l l u s t r a t e s by both  t h e o r e t i c a l and p r a c t i c a l d i s c u s s i o n the t h r e e major presently  available  Patterson  heavy  methods,  five  and  for  atom  structure  synthesis,  methods  determination v i z . centrosymmetric  non-centrosyrametric  direct  the  direct  methods, and  c o n t a i n s a b r i e f d e s c r i p t i o n of the p r a c t i c a l a s p e c t s  of  also X-  ray c r y s t a l l o g r a p h y . Chapter designed  1  to  deals  explain  with some  the of  practical the  terms  e x p e r i m e n t a l s e c t i o n s of Chapters 2-6, crystallographie to  reader  crystallography.  nomenclature  aspects  and  used  appearing  crystallographic  throughout  this  in  the  a l s o g i v e the  of t h i s thesis a l i m i t e d  All  and i s  background  symbols  thesis  non-  and  have t h e i r  c o n v e n t i o n a l meanings d e s c r i b e d i n the " I n t e r n a t i o n a l  Tables  f o r X-ray C r y s t a l l o g r a p h y " (1). Chapters  2-6  c o n t a i n the d e s c r i p t i o n of the methods o f  s t r u c t u r e a n a l y s i s used, with a d i s c u s s i o n o f  the  resulting  molecular  and  for  the  compounds  examined.  crystal  structures  found,  five  [ 2 , 3 - b i s (dimethylarsino)-1,1,1,4,4,4-  hexafluoro-but-2-ene-As,Js]tricarbonyldiiodotungsten(II), d i methylammonium t r i c h l o r o t r i s ( d i m e t h y l s u l p h o x i d e ) r u t h e n a t e ( I I ) , and  d i c h l o r o t e t r a k i s (dimethylsulphoxide) ruthenium (II)  a l l s o l v e d using dioxypurine centrosymmetric  Patterson  syntheses,  hydrochloride d i r e c t methods,  dihydrate and  were  1,3,7-trimethyl-2,6was  solved  by  1-acetyl-3-benzamido-2-  keto-4- (2,3, 4,6-tetr a-O-acetyl-p-D-glucopyranosyloxy)  3  pyrroline  was  solved  methods. T h e s e tungsten, For  methods  purine each  and of  Fc) z  where  structure  Fo  anisotropic U;;  i n the f  and  thermal  crystal  b a s e d on Fc  in  compounds  five  was  non-centrosymmetric  discussed  pyrroline  and  factors  are  the  squares refinement  using  the  are  detail  for  the  repectively. structures  minimization  the  direct  observed  the of  and  w i s the  assigned  weighting  factors  employed  i n the  least-  ^  w(Fo-  calculated factor.  The  refinement  are  expression:  = f ° e x p [ - 2 T t 2 (U +  h a* 2  M  + U ]c b*2  2  •  2  i x  2 U , h k a * b * + 2U t  u  hfa*c**  U^^c*  2  +20^k4b*c*) ]  o where £ that  i s the  corrected  parameters  for  have t h e  tabulated scattering thermal  where B i s r e l a t e d the  atom  from  The  and  isotropic  f  xs  thermal  form: t =  of  motion.  factor  f°exp [-B ( s i n e / A ) to  the  2  ]  mean-square d i s p l a c e m e n t , [ j ,  i t s mean p o s i t i o n  2  by  B = 8W2U2.  the  expression:  CHAPTER 1  INTRODUCTION  TO  X-RAY  CRYSTALLOGRAPHY  5  A)  A PRACTICAL VIEWPOINT  X-ray c r y s t a l l o g r a p h y years ago  has  grown from i t s i n f a n c y  to become what many would f e e l i s the  d e f i n i t i v e means of s t r u c t u r e d e t e r m i n a t i o n .  some 60  present  From the  day  complex  pattern  of d i f f r a c t e d X-ray i n t e n s i t i e s a c r y s t a l l o g r a p h e r  is  usually  able to piece together the i n t e r n a l s t r u c t u r e of  the  s i n g l e c r y s t a l chcsen f o r information  valuable  study.  to  both  s c i e n t i s t s and  as  accuracy  reliability.  and  crystallography several  such  are  standard  outline  necessary  of  rarely  should  crystallographer  reading  Often  good  a  contain  and  equalled  and  (2-6), ideas  be  the  given  practical  data,  results  practical  in  terms  Although the p r i n c i p l e s of  texts  the  end  theoretical  are w e l l e s t a b l i s h e d  c r y s t a l l o g r a p h i c terms and the  The  are  aspects  very  of  useful  X-ray  discussed  in  synopsis  of  brief  in this  of  chapter,  and  obtaining  the  to  the  non-  this thesis. X-ray  crystallographic  d e t e r m i n a t i o n w i l l depend upon the  skill  of  structure  the  synthetic  chemist to produce a s u i t a b l e c r y s t a l . A s a t i s f a c t o r y c r y s t a l would  be  uniform  in  internal  structure, single  twinned), with a reasonable s i z e and and  shape  are  difficult  balance o f c o n t r a d i c t o r y  to  corrected); 1 ft 0  = 2//*.  For o r g a n i c  one  define since  factors  more i n t e n s i t y but i n t r o d u c e s  shape. The  absorption  1  e f f e c t s t h a t must thickness  a  is  be  that  coefficient.  (for CuKa r a d i a t i o n )  t pfc = 0.2cm which i s a l a r g e c r y s t a l indeed. A 0  size  they depend on  i s the l i n e a r a b s o r p t i o n  compounds yuc<10cm-  perfect  (e.g. a l a r g e r s i z e produces  e q u a t i o n f o r the optimum  where  ( i . e . not  more  giving a general  6  rule 0.3  is mm  that a uniform c r o s s - s e c t i o n c r y s t a l of s i z e 0.1  i s p r e f e r r e d . O b v i o u s l y i t i s e a s i e r t o work with room  temperature and a i r s t a b l e c r y s t a l s been  developed  so  though  techniques  be determined.  Once s u i t a b l e c r y s t a l s have been found, one i s the  end  of  a  glass  f i b r e , with a l i t t l e  adhesive, and mounted on a goniometer head  have  t h a t the s t r u c t u r e s of thermal- and a i r -  unstable c r y s t a l s can s t i l l  to  to  head.  attached  non-reactive  The  goniometer  i s s p e c i a l l y designed to enable simple alignment of the  crystal.  I t has two a r c s which allow the c r y s t a l t o be  by i 20°  in  each  perpendicular  of  two  perpendicular  planes,  tipped  and  two  s l i d e s which allow f o r l a t e r a l movement o f the  crystal. The c r y s t a l l c g r a p h e r operations  on  the  must  crystal.  determine t h e s i z e and shape of provides the  additional  now  complete  Firstly the  it unit  two  is  distinct  necessary  cell  which  i n f o r m a t i o n i t would  i m p o s s i b l e to undertake the second part which e n t a i l s position  intensity  of  intensities  of  a l l diffracted  these that  can  other words the c r y s t a l  given  Law  X-rays  'reflections', be  d i s t r i b u t i o n of d i f f r a c t i n g  Bragg*s  also  i n f o r m a t i o n on the i n t e r n a l symmetry of  c r y s t a l . Without t h i s 'geometry'  the  to  since  ultimately  e l e c t r o n s i n the  be  knowing  and measuring the it  is  related unit  these to  the  cell,  in  structure.  (7) f o r X-ray d i f f r a c t i o n from a c r y s t a l i s  by: n X = 2dsinG where n i s an i n t e g e r , X i s  the  wavelength  of  X-ray  7  radiation,  d  i s the i n t e r p l a n a r  between t h e i n c i d e n t  beam and  b e i n g c o n s i d e r e d . The  planes  are  indices,  named  any  plane  these cell  by M i l l e r makes on  intercepts edge)  (h,k,i).  then  is  to  origin. from  the  1/k,  plane i s s a i d  sin©  . 1 d  =  nX 2  relationship  direct  been  produced.  sphere  for of  c*,  l a t t i c e planes  d  ( h , k , 4 ) . Now a  unit of  obtained  by  1/d  which  lattice.  c o n s i d e r i n g the  A  normals  (h,k,£) drawn from  the 1/d^  kJl  perpendicular distance the d i f f r a c t i n g  reciprocal  planes  lattice  t o the r e a l a x e s a, b and the  If  indices  reciprocal  ( f i g . 1). Whenever a  with c,  has  l a t t i c e with  the  allows for a simple v i s u a l i z a t i o n reciprocal  of  the  lattice  the s u r f a c e of t h e sphere the c o n d i t i o n s  reflection  planes i n d i r e c t  c.  at a p o i n t a d i s t a n c e  i s the  K K 1  compared  c o i n c i d e s with Bragg  X-rays  intercepts  b e t w e e n sin§ and  be d e f i n e d by  Combining  process  be  (8) , i n h i s r e c i p r o c a l  where  of reflection  diffraction point  and  (fractions  view o f d i f f r a c t i o n c a n  h a v e been r e p l a c e d by p o i n t s and b*  the  ,  t o the  t o have M i l l e r gives  l a t t i c e can  origin,  V*  B r a g g « s law  between p l a n e s o f t h e s e t  a x e s a*,  reflecting  which r e l a t e  Each n o r m a l i s t e r m i n a t e d  the  ,  plane  of the  a direct  a l l possible  that are  crystal  are  t h e c o n s t r u c t o f Ewald  reciprocal  particular  angle  and  a simplified  considering  the  8- i s the  a s e t o f r e f e r e n c e a x e s a, b,  Rearranging  and  s p a c i n g , and  are f u l f i l l e d  space  the c e n t r e of the sphere  and  f o r the c o r r e s p o n d i n g s e t  a diffracted  through  ray  passes  t h i s p o i n t of c o n t a c t .  from  B  Figure  1  S c h e m a t i c d r a w i n g o f a r e c i p r o c a l l a t t i c e l e v e l (n) i n t e r s e c t i n g the sphere of r e f l e c t i o n . D i f f r a c t e d r a y s Fass f r c n the c e n t r e of the sphere through the i n t e r s e c t i n g p o i n t s . As t h e c r y s t a l r o t a t e s o t h e r p o i n t s i n the r e c i p r o c a l l a t t i c e l e v e l c o n t a c t the s p h e r e b u t a l w a y s on t h e c i r c l e . E x t e n d e d r a y s w i l l s e e t t h e c y l i n d r i c a l f i l m a t t h e same h e i g h t i f t h e crystal i s correctly aligned.  9  The  application  methods u s e d For  this  usually  a  b o t h as they  rotation  these  Weissenberg  (e.g.  p e r p e n d i c u l a r t o the X-ray definition,  the  reciprocal  a*b*  lattice axis  oscillation  planes  must  these points w i l l  s h o u l d , when t h e d i f f r a c t e d points  are  extended,  on u n r o l l i n g straight  axis  separation identity  or  will  of  the  beam  c u t the sphere  rays through  period  o f the l a t t i c e  being  etc.) o f to  the  ( f i g . 1) .  On  i n a c i r c l e , and  these  intersecting  a t t h e same h e i g h t . Then spots w i l l  l i e  on  E r r o r s i n alignment o f  and c a n be c o r r e c t e d , on  a  lattice  perpendicular  rows on t h e f i l m .  rows  axis  f  the  In  with a r e a l  hkO, hk1, hk2  be  meet t h e f i l m  appear  cell.  used.  reciprocal  and d e v e l o p i n g t h e d i f f r a c t e d  lines  the r e a l  the  to  be  rotation  (i.e.  parallel  unit  i s co-axial  the  beam. By  points  and  of f i l m  c),  i n the  or a P r e c e s s i o n camera, b u t  a r e complementary, can  camera a c y l i n d e r axis  rotation  c o n c e p t s c a n be s e e n  f o r d e t e r m i n i n g t h e geometry o f t h e  either  Weissenberg  of  the  film  this  repeat  and  as  the  i s a function of the distance  can  be  determined. . A about and  plane o f r e f l e c t i o n s t h e axes  and and  a* and b* b u t i n a c o m p r e s s e d  as previously  however, t h i s the  different places. provides  times  the  appears  as a row on  i s moved w h i l e t h e c r y s t a l  will  This  stated  unseparable  o r any s i m i l a r row i s i s o l a t e d  film  b* axes  ( e . g . hkO) c o n t a i n s i n f o r m a t i o n  intersect and  the  sphere  s h o u l d appear  additional  (using  of  If,  a screen) the a *  reflection  on t h e f i l m  unit  film.  i s rotating  i s t h e b a s i s o f the Weissenberg necessary  the  form  at  i n different  t e c h n i q u e and i t  cell  information;  10  e.g. as  the  related  distance  to the angle r o t a t e d  measurement the f i l m  of  the  a  Buerger  distorted  precession  machining  which  plane  the  produces  (again by  Weissenberg  the  often  axes  of  by  a  b* on  less  i t  lattice.  The  a  one  complex reciprocal  of  film,  lattice.  is  that  by  of  the  precession form  for  ( e.g.  mirror axes  planes  and  a  screen  p r o d u c i n g an  Obviously though  than  this  the e x t e n t  that  photographs  of  of  the  the  a two planes  (e.g.  230  space  fold  that  are  of  groups a r i s e symmetry  rotation  lead  plus  plus  axes  translation),  translation) axes,  to systematic  which  with glide  absences,  missing  c o m b i n a t i o n o f s y s t e m a t i c a b s e n c e s and  the photograph p r o v i d e the i n f o r m a t i o n from  from  d e s i g n a t e d by  screw  systematically  the  elements  (m) , r o t a t i o n - i n v e r s i o n  presence of  lattices  absences*  determination  a, a m i r r o r  The  also provide  'systematic  (e.g. 2 j , a r o t a t i o n  centered  reflections The  motion  motion  i n the  14 B r a v a i s l a t t i c e s .  film.  i s  by t h e p l a c e m e n t  s p a c e g r o u p . The  2),  glide  i.e.  the  this  combinations of the p o s s i b l e  rotation  planes,  = 2°),  the r e c i p r o c a l  overcomes  available  allows  (e. g. 2 ) , screw  the  {1mm  o f t h e a x e s a * and  *geometric* information,  information  symbol  and  of  isolated,  H e i s s e n b e r g and  the d i s t i n c t  the  is linearly  camera.  crystallographic  i.e.,  the c r y s t a l  view o f t h e r e c i p r o c a l  similar  The  view  camera  of r e c i p r o c a l space  which  film  determined.  duplicates  film)  undistorted  symmetry  the  d i s a d v a n t a g e o f t h e H e i s s e n b e r g method  produces  lattice  by  by  distance apart  t h e a n g l e d * c a n be  The  and  travelled  on  the  symmetry the  on  space  11  group  can  be  determined.. Sometimes  i t i s not p o s s i b l e t o  uniquely d e f i n e the space group from the photographs e.g. P2, and P2, /m row  have t h e same s y s t e m a t i c absences i . e .  on the  3k0  every odd numbered k r e f l e c t i o n i s missing. T h i s absence  i s related  to the presence o f the two screw  axis  (2,) i n  group. The a d d i t i o n a l symmetry element m i n P2,/m absences  and  hence  the  two  the  produces no  groups are i n d i s t i n g u i s h a b l e .  F o r t u n a t e l y t h i s causes few problems i n the  final  structure  d e t e r m i n a t i o n process. Another of  molecules  measuring  important  p i e c e o f i n f o r m a t i o n i s Z the number  per  cell,  the  unit  which  is  can  be  calculated  molecular weight of produce  found  by  d e n s i t y of the c r y s t a l s by f l o t a t i o n methods.  Using the d e n s i t y , the t o t a l molecular contents  usually  close  to  the an  and  then  compound. integer  weight  compared  This  ratio,  of  the  cell  with  comparison  the  should  even i f the molecular  weight i s only known approximately, which corresponds to  the  number of molecules i n the c e l l . Each  space  asymmetric Z  that group.  (Chapter  group  has  a  u n i t s which g e n e r a l l y  may  assist  in  Unfortunately, 3)  or  less  space group i s s t i l l  characteristic contain  one  number  of  molecule,  so  determining or c o n f i r m i n g  asymmetric  units  can  the space  contain  more  than one molecule. I n p r a c t i c e i f the  i n q u e s t i o n , the u s u a l  approach  is  to  attempt the s o l u t i o n i n each o f the p o s s i b l e space groups and see which one succeeds. The  film  techniques  about the c r y s t a l : t h e  have  three  produced the f o l l o w i n g data  axial  lengths  a,  b,  and  c  1 2  (reciprocal  dimensions  can  be e a s i l y transformed i n t o  l a t t i c e dimensions by the use three  angles  of  standard  equations),  the  and "6 , and t h e probable space group.  With  a l l t h i s i n f o r m a t i o n i t i s now p o s s i b l e t o proceed second  with t h e  stage which i n v o l v e s measuring t h e i n t e n s i t y  independent r e f l e c t i o n . From the l a t t i c e space  real  of every  parameters  and the  group a computer can e a s i l y c a l c u l a t e s e t t i n g s f o r t h e  c r y s t a l and d e t e c t o r , with r e s p e c t t o the i n c i d e n t beam, such that the i n t e n s i t y o f a l l t h e  desired  measured. The c r y s t a l i s t r a n s f e r e d accurately  from  of axial  reflections.  prominent  reflections  the p r e v i o u s l y taken photographs)  i s carefully  determined so t h a t the c e l l  several  dimensions can be more a c c u r a t e l y  r e f i n e d . A new s e t o f v a l u e s f o r the r e l a t i v e crystal  and  intensity  can  be  positions  each  reflection  the  detector  is  measured. peak,  The  detector  recording  then  the  scans  intensity,  through and  measures the background on the other s i d e . U s u a l l y data  based  of  the  finally  from  on a l l t h e measured r e f l e c t i o n s  p o s s i b l e t o determine t h e s t r u c t u r e o f t h e c r y s t a l . summary  initially  t o one s i d e of the maximum so t h a t the background  reflection  intensity  of  d e t e c t o r c a n then be determined. To measure t h e  of  positioned  can be  to the d i f f T a c t o m e t e r and  a l i g n e d using t h e i n t e n s i t y  Then the maximum p o s i t i o n of (chosen  reflections  A  the it is brief  t h e s e p r a c t i c a l procedures i s i l l u s t r a t e d i n t h e  flow diagram F i g u r e 2.  13  A) Geometry of d i f f r a c t i o n  measurements  Choose c r y s t a l , a t t a c h to f i b r e on goniometer head  I i  Crystal  ,  mounted  Take o s c i l l a t i o n photographs  I  Crystal correctly aligned a x i a l repeat d i s t a n c e determined  Take Seissenberg  and  I  precession  photographs  Unit c e l l constants and space group determined  B) I n t e n s i t y of d i f f r a c t i o n  Mount on cell  data  d i f f r a c t o m e t e r , more a c c u r a t e l y determine c o n s t a n t s , measure i n t e n s i t i e s of a l l necessary r e f l e c t i o n s  I  S t r u c t u r e f a c t o r amplitudes |Fobs| determined  Figure 2  Flow c h a r t i l l u s t r a t i n g the important steps i n the p r a c t i c a l aspects o f X-ray c r y s t a l l o g r a p h y  14  B) A THEORETICAL VIEWPOINT An  atom  referred  to  radiation  with  fractional  unit  cell  axes  with  relative cell,  (n)  to  an  the  The atomic  atom  and  amplitude origin,  of  b,  f ,  and  and  n  dependent  its  value  is  x ,y ,z  c w i l l scatter  a  phase  constant,  dependent  sin8/X  upon  (values  can  the  be  type  of  for  the  obtained  F u r t h e r c o r r e c t i o n s are made f o r the thermal  the  atom  (f  is  tabulated  X-  on i t s p o s i t i o n i n the  s c a t t e r i n g f a c t o r v a r i e s with  r e f l e c t i o n being c o n s i d e r e d tables).  a,  co-ordinates  for  stationary  from motion  atoms)  as  mentioned i n the g e n e r a l i n t r o d u c t i o n . If  there i s more than one atom then the r e s u l t a n t from a  combination  of these d i f f r a c t e d waves i s c a l l e d the s t r u c t u r e  f a c t o r and can be expressed F(hkl) = ^  f o r a g e n e r a l plane  (h,k,t)  as  2lti (hx-• ky. + I z- ) 3  f-exp[  where the summation i s over a l l atoms i n the u n i t  cell.  An e q u i v a l e n t e x p r e s s i o n i s n  [ c o s 2 U ( h x * ky.. + A z p  F (hkft) = i.e.  F(hkl) can be represented F(hkt) =  hence amplitude  the  |F  1F  K % t t  resultant  j F | and a phase c o n s t a n t If I  about  complex  =  J A  2  +  £2  and  measured i n t e n s i t y I V < U  | and not about «  v  ^2^)3  as a complex number  A + iB  or F (hk|) =  The  • i s i n 2 i r (hx, * ky^*  j  w  t  V  1 (cos ci + i s i n * ) is  c h a r a c t e r i s e d by an  given  ^ = tan-  by 1  B/A.  u n f o r t u n a t e l y only t e l l s since generally  us  1  This problem* realized  lack  o f knowledge a b o u t p h a s e s i s c a l l e d  *the  and  i t s affect  when i t i s  that  only  becomes a p p a r e n t  i f the s t r u c t u r e f a c t o r s a r e Fourier  of the p e r i o d i c e l e c t r o n density the  electron  density  must  £ (xyz)=i £ £ £ F ( h k $ ) y  Vv  of the c r y s t a l  be t h e F o u r i e r  s t r u c t u r e f a c t o r s . The g e n e r a l  series  entire crystal used JF  V W I  to |  lattice  then of the  expression i s  exp [-2*1 (hx  + ky_ + A z ) J  * t  can  be summed  to g i v e  are  overcome  Patterson  the  fact  that 1 ^  C h a p t e r 2, c e n t r o s y m m e t r i c  atom  are  gives  and t h e y a r e d i s c u s s e d heavy  known  a representation  s t r u c t u r e . T h r e e major methods  and n o t  chapters;  phase  transforms  transform  hence once the s t r u c t u r e f a c t o r s F ( h k l ) above  5  in  methods  are  6.  presently on  following  discussed i n  d i r e c t methods i n C h a p t e r  n o n c e n t r o s y m m e t r i c d i r e c t methods i n C h a p t e r  of the  information the  the  5,  and  1  CHAPTER 2  CRYSTAL AND MOLECULAR  STRUCTURE OF  [ 2,3-BIS(DIMETHYL ARSINQ) — 1,1,1,4,4,4-HEXAFLUOROBUT-2-ENEA S , A S ] T R I C A R B O » Y L D I I O D O T O N G S T E N (II)  6  17  INTRODUCTION Preliminary Irltl*  n. m.  r.  data on [ 2 , 3 - b i s ( d i m e t h y l a r s i n o ) -  4, 4,4-hexaf luorobut-2-ene- As,As " ) t r i c a r b o n y l d i i o d o -  tungsten(II) nonrigidity  seemed (9),  consistent  the  observed  for  crystal  structure  existence  seven-coordinate  with of  stereochemical  which  tantalum  has  of  the  X-ray  HejAsC (CF ) :C ( C F ) AsMe^HIa, ( W  of  C0  probable  w  a  3  S  most  exchange processes  been  (10)., The  undertaken t o provide i n f o r m a t i o n , which c o u l d geometry  also  transition  indicate  the  s t a t e , f o r the  occuring i n s o l u t i o n . .  EXPERIMENTAL [ 2 ,3-bis ( d i r a e t h y l a r s i n o ) - 1, 1, 1, 4, 4, 4-hexaf luorobut- 2ene-As, As ] t r i c a r b o n y l d i i o d o t u n g s t e n (II) was  prepared  by  the  dropwise a d d i t i o n of i o d i n e to Me AsC (CF ) :C (CF ) AsMe^W (CO)H. x  3  3  i n CH^Cl^, with vigorous s t i r r i n g under a N flecrystallization  from  a  b p a r a l l e l to the g o n i o s t a t a x i s and with group  a  cross data  measurements.  s e c t i o n of 0.2  were  obtained  Unit-cell 2  C r y s t a l Data.  was  x 0.0 4 mm.  from  film  was  gave  mounted  c a . 0.2  mm  with  i n length  U n i t - c e l l and and  space  diffTactometer  parameters were r e f i n e d by a  squares treatment of s i n 6 on a d i f f T a c t o m e t e r  atmosphere.  methylene chloride/faexane  yellow p l a t e s . The c r y s t a l chosen f o r study  ,  least-  values f o r 24 r e f l e c t i o n s measured  with MoK«t r a d i a t i o n . C  M  H » As F a  1  f c  I 0 w, z  3  M = 893.40 o  Monoclinic, £ =  a = 15.37(2), b = 9.529(1], c = 15. 967 (3)  112.03(2)°,  0 = 2168(2)  A , 3  D= m  2.737 (3) gem- , Z = 3  A, 4,  s  18  &c = 2.735 (4) gcra-3, F(QOO) = 1608  o  A,  (20°C,  HoK*,  >\ = 0.71069  /x = 118 c m ) . Absent r e f l e c t i o n s : hOl, l#2n and  OkO ,  - 1  k#2n d e f i n e uniquely the space group P2^/c I n t e n s i t i e s were measured on a Electric  XRD  scan  degrees each  at  14). General  6 d i f f T a c t o m e t e r , with a s c i n t i l l a t i o n  counter,  2°  i n 26,  , No.  Datex-automated  Ho K<* (zirconium f i l t e r 2B  (C|  and p u l s e height a n a l y s e r ) , and  min-*  over  a range of  (1.80  a  9-  * 0. 86 tan 0)  with 20 s background counts being measured  end of the scan. Data were measured t o 2€ = 45°  at  (minimum  e  ft).  i n t e r p l a n a r spacing 0.93 every  50  reflections  throughout  g r e a t e s t d e v i a t i o n from final  intensity  and p o l a r i z a t i o n amplitudes  was  942  +10.1% and  times the i n i t i a l  intensities  2  time  less  than  = S + B * . (0.05S)  averaged  2  The the  value. Lorentz  c o r r e c t i o n s were a p p l i e d , and the  had  monitored  data c o l l e c t i o n .  the i n i t i a l v a l u e was 1.007  background where <r (I) B =  the  were d e r i v e d . Of the 2778 independent  measured,  and  A check r e f l e c t i o n was  structure reflections  3<r(l)  above  with S = scan  count  background count. These r e f l e c t i o n s  were c l a s s i f i e d as unobserved  and given zero  weight  in  the  refinement. Structure As at  previously  s t a t e d i n Chapter  a p o i n t <x,y,z) can  Fourier  series  analysis  with  1 the e l e c t r o n d e n s i t y  be represented by a three the  structure  dimensional  factors  a  s  coefficients C&,.2,z) = i ! S £ F(h,k,<)exp[-2Tti(hx K U F^ but  t  the  t  c o n t a i n s both an amplitude intensity  * ky + *z) ].  information  JF^  only  W 4  | and  gives  a phase * ^ data  on  t  the  1 9  !F^ |'s, w t  hence the phase i n f o r m a t i o n i s unknown.  Patterson  (11)  s o l v e d t h i s problem by use o f a F o u r i e r  s e r i e s with the phaseless  quantities II^v.*'  2  a  coefficients  s  i.e. f ( x , ! , z ) =1 JF y v u. <. This  summation  u ,v ,w  x " , 2 ^ 2 , and x ,2. ,z x  x  u = x,-x  t  At  first  there  are  N  This  v = y_, -y_  t  involving the  may be a symmetry  a  atoms  interpretation  and  1  the  atoms  w = z-z 4  a  related  Patterson  in  the  cell,  v e c t o r s contained  leads  for  such t h a t  position  synthesis  s o l u t i o n to the phase problem.  d i s t i n c t Patterson size.  to the i n t e r a t o m i c v e c t o r s i . e .  glance  p r o v i d e a simple  peaks a t  on the P a t t e r s o n aap there e x i s t  %  where X j _ , y . , z  + ky. + I z ) .  produced a map which c o n t a i n e d  p o s i t i o n s corresponding co-ordinates  J cos2n(hx 2  k  to  a  virtually  great  there  of  appears t o However, i f  w i l l be N{N-1)/2  in a cell  deal  of  of  the  same  o v e r l a p and makes  impossible e s p e c i a l l y f o r s t r u c t u r e s  many atoms o f the same weight because  in  addition  height o f the v e c t o r peak i s p r o p o r t i o n a l t o the product  of the atomic numbers o f t h e atoms t o which i t corresponds. consequence •heavy* lighter  of  atoms  this will  is  that  appear  vectors  between  relatively  l a r g e r than v e c t o r s between the  atoms, and here l i e s the key t o the s o l u t i o n  phase problem f o r c e r t a i n  A  of  the  molecules.  I f a molecule c o n t a i n s a few *heavy' atoms the P a t t e r s o n function  will  g i v e i n f o r m a t i o n on t h i s p a r t of the molecule.  20  If  the  heavy  structure  atom(s)  comprise  factor, a first  obtained i . e .  the  of  the be  analytically M  i  t £ « u  if  £«,»£ui  then  I ^ A  ki .+ <z .)]  H  +  H  M  exp[ 2 * i (hx . • k . * i z . ) ]  T i  L  Iu  u  exp[2TTi ( h x + JSI + I z„- ) ]. Wi  this f i r s t  summation  share  approximation to the phases may  Efc„ = ^ f . ^ e x p [ 2 « i ( h x . *  If  larger  the  Hi  approximation  difference  is  map  used  in  produced  the  may  Fouriar  provide  the  p o s i t i o n s o f another p a r t o f the molecule. These p o s i t i o n s o f new  atoms can be added t o the o l d ones and  used  the phases. The process i s then repeated and this  iterative  the complete pieces  of  structure  procedure  structure  is  determinations  this  compound  of  finding  the  and  the  two  P a t t e r s o n ' syntheses  expected  would  be  largest  s i n g l e heavy atoms and t h e i r symmetry cases.  direct  methods  ruthenium  the  three  successive  6.  ( d i s c u s s e d i n Chapters 3 and 4)  all  i t i s hoped t h a t  e s s e n t i a l l y the b a s i s f o r a l l  including  d e s c r i b e d i n Chapters .5 and For  improve  w i l l r e s u l t i n the d e t e r m i n a t i o n o f  s t r u c t u r e . T h i s process the  to  to  peaks  related  procedure  was  on  the  be between the positions  Once the tungsten and ruthenium  were determined the i t e r a t i v e  compounds  used  in  positions  to f i n d  the  r e s t of the molecules. Even  t h e process of f i n d i n g the heavy atoms i s somewhat  s i m p l i f i e d by the phenomenon (12).  He  showed  that  first  useful  pointed  out  by  Harker  information  i s contained i n  c e r t a i n planes and l i n e s i n the Patterson map  which g i v e r i s e  21  to  v e c t o r s with one  or two  presence of symmetry For P2t/c  example  (other than  the  elements  of  (IV),  The  correspond  to the  positions.  e.g.  vectors  the  crystal.  Due  to  was the  atom t h a t occurs a t the at  ( I I ) ; x, 1/2+y_, 1/2-z  Patterson  to  space group  i n the u n i t c e l l .  (I) w i l l a l s o occur  p o s i t i o n s x,y,z  y,1/2+z  i n the  compound's  the group any  g e n e r a l p o s i t i o n x,y,z related  centres)  tungsten  which has f o u r molecules  symmetry  is  constant c o - o r d i n a t e s due  the  symmetry  ( I I I ) ; and  x,1/2-  f u n c t i o n c o n t a i n s peaks which  between  these  symmetry  the v e c t o r between p o s i t i o n  related  (I) and  (III)  either (x 1/2-y, 1/2+z) "  <**Y.»z) =  #  (0,1/2-2y,1/2)  or (£,I#z) " as 1/2  (S,1/2-y,1/2 + z)  i s e g u i v a l e n t to -1/2  0, 1/2-2y, 1/2  and  0, 1/2*-2y_, 1/2  {note that these two symmetry  = (0,-1/2+2y,-1/2)  hence  centrosymmetric).  all  the two  v e c t o r s become  i . e . 0,1/2  ±  2y,1/2  v e c t o r s were r e l a t e d by a centre o f Patterson  Table  functions  must  be  1 g i v e s the g e n e r a l v e c t o r s between  a l l the f o u r symmetry r e l a t e d p o s i t i o n s ( I ) , ( I I ) , ( I I I ) ,  and  (IV) i n i t s f i r s t  column. A search of the Patterson  was  then  to  undertaken  see i f any  these v e c t o r s which would symmetry  related  tungsten  be  map  of the peaks corresponded  expected  to  be  to  between  the  atoms. The second column of  this  t a b l e i n d i c a t e s the r e s p e c t i v e peaks found on the map.  Column  three gives the p o s s i b l e values f o r the c o - o r d i n a t e s x,y_,z o f the tungsten of  W-I  atcm. The  vectors  and  map I-I  was a l s o examined f o r the vectors  and  from  an  presence overall  22  Table 1  V e c t o r s between  the symmetry  r e l a t e d p o s i t i o n s f o r the Space  Group P2, /c and the p o s s i b l e s o l u t i o n s to the  Patterson  f u n c t i o n f o r the tungsten compound  Peak on Patterson  'General v e c t o r s f o r  function  i Space Group P2 /c l(  #2* ' 0, 1/2t2y,  0.00,  1/2  ; ! ±2x, 1/2,  #3 0.35,  1/2±2z  0.28, 0.50  0.50, 0.27  ] Possible  solution]  '  '  ;  1/2t2y =0.28  |  J 2y  = 0.22 o r 0.78!  |  4.  l 2x  = 0.35 o r 0.65  !  1/2i2z=,0.27  2x = 0. 35  I  ! 2z = 0.23 o r 0. 77  #16 • i.2x, ± 2 y , i-2z  i  0.65, 0.22, 0. 23  J 2x  = 0.65 or 0. 35  J,2y = 0.23 o r 0.78  I  2z = 0.23 o r 0.77  Peaks were ordered by s i z e , i . e . #2 was the second  highest  23  examination i t was  2x = 1.35,  2y. = 0.78,  and  2z =  0.77  x = 0.68,  2 = 0.39,  and  z =  0.38  the  co-ordinates  or would tungsten  deduced t h a t  be  the  atom.  refinement  values  One  varying  for  cycle  the  of  full-matrix  isotropic  thermal  of  the  least-squares parameters  and  p o s i t i o n of the tungsten atom produced an B f a c t o r of 0.54. difference  Fourier  revealed  and  arsenic  atoms and  the two  the to  positional 0.20.  positions  A  and  and  thermal  isotropic  -3  and  this  the  parameters  0.16.  the  effects  Due  amplitudes.  computer  program  of  dimensions  the  An  to  crystal  measured.  corrected  anomalous  further  the  five  f o r the  the  high  was  were  carefully  * heavy*  of JLK  believed  probably  that  due  when c a l c u l a t i n g using  attempted indexed  (13). and  values used i n the c o r r e c t i o n  last cycles, f o r absorption,  but  the  new  produced an  f i n a l l y reached a f t e r two  dispersion  thermal parameters f o r the  cycles  value  correction  therefore  the  remaining  c y c l e s of refinement with the  0.076. Convergence was an  was  The  parameters used i n the  using  two  for  absorption  absorption  BICABS  given i n T a b l e 2. Two  amplitudes  of  varying  revealed  s i z e of the c r y s t a l i t was  structure  faces  cycles  stage  parameters  such a high d i s c r e p e n c y at t h i s stage neglecting  iodine  thermal parameters reduced R  at  thermal  atoms reduced B to only (118cm )  map  two  the remaining 20 atoms, but  with a n i s o t r o p i c atoms  p o s i t i o n s of the two  a further  anisotropic  difference  of  the  A  correction  W, I , and  to the the The the are  same atom structure  H factor  of  more c y c l e s ,  and  As atoms, and  anisotropic isotropic  Table 2 C r y s t a l dimensions and i n d i c e s of the f a c e s used i n absorption c o r r e c t i o n  ' • i  !  • • !  -!  k •  1 ! j -12 0 i - i -1 • 0 _-j • 0 0 i - i  o -4  1 0 11 0 0 1 -1  Distance t o C e n t r o i d 0.0228 0.0197 0.0045 0.0045 0.0207 0.0207  (cm.)  ' I | i J  25  thermal the  parameters f o r the  1823  observed  reflections.  i n t e n s i t y r e f l e c t i o n s 102, 604,  114,  514,  025,  c a l c u l a t i o n due The  remaining atoms, at 8 = 0.067 f o r  and  106,  225  {The  204,  202,  were not  factors  were  anomalous s c a t t e r i n g c o r r e c t i o n s  highest  306,  504,  i n the  502,  B factor  error.)  taken  from  from r e f . 15.  The  and  weighting  1  and yj w = 0.0  f o r unobserved r e f l e c t i o n s gave constant average  f  v a l u e s of W ( F o - F c ) the  final  7  ^ « ; J w ~ = 74.3/JFoJ  r e f . 14  scheme: /]T=  i  -  204,  included  to probable instrumental  scattering  thirteen  3  over ranges of  2  |Fo|  and  two  CF  groups  on  the  chelate  i s o t r o p i c temperature f a c t o r s ; however an Fo calculated  atoms  was  >  74.3  employed  in  stages of refinement.  The  map  i f |Fo|  did  using the  phases  not r e v e a l any  from  all  ring  had  electron  high density  the  other  found  evidence of d i s o r d e r  i n the  groups  or i n d i v i d u a l atoms. The Tables  final 3  structure  and  p o s i t i o n a l and 4  thermal parameters are  respectively.  Measured  f a c t o r s are a v a i l a b l e from the  and  given i n  calculated  U.B.C. L i b r a r y .  26  RESULTS AND DISCUSSION  CO X^ v\CO M  A-A 2  1  M X Y R.  = W = I = As == CH3  M X Y R  A—A = r = C  = Mo = Br = P = CftHs  A—A = CH —CH 2  2  CFj CF  3  Figure 3 Schematic  diagram  c f compounds  (1) and (2) from  The s e v e n - c o o r d i n a t e geometry about (1),  the tungsteD  for  is  In t h i s  mclecule  C ( 1 ) , C (2)  c o n s i s t s of the two regaining  arsenic  and  iodine atcm  As(1), atoms  As (2).  down the W-C(3) bond. Although describe  that  the  tungsten  d i s t o r t e d capped t r i g c n a l  distorted  capped  the c a p p i n g group i s cne c f the  c a r b o n y l s [ C ( 3 ) - 0 ( 3 ) ], the t h r e e a t o i s are  to  (16) ( F i g u r e 3 ) , t h i s type o f  geometry being d e s c r i b e d as a c o n s i d e r a b l y octahedron.  similar  (2) d i b r c m c t r i c a r b c n y l [ 1 , 2 - b i s (diphenylphosphino)  ethanejmclybdenum(II)-1-acetone  face  atcm i n  [2,3-bis(dimethylarsinc)-1,1,1,4,a,4-hexafluorobut-2-  ene-Aj,AsJtricarbonyldiiodotungsten(II) found  text  defining  while 1(1)  capped  the uncapped f a c e and  1(2)  and the  F i g u r e 4 shows a p r o j e c t i o n  i t would a l s o be  environment prisms  the  in  terms  possible of  to  various  (17), a d e t a i l e d a n a l y s i s of  C(4)  ^V-  29(4)  1.98(3)/ [ N ^ C © As(1)  2.00(3) 1(1)/  1.17(A)J  2.556(3)  |As(2)  J>.>  2.856(2)  C(2)  V  J.19C4)  '0(1)  Figure 4 P r o j e c t i o n o f the c o o r d i n a t i o n sphere of the molecule viewed dcwc the v e c t o r from the c a r t o n y l grcup i n the capping p o s i t i o n (ctritted from the diagrair) t o t h e tungsten atcm.  Table 3 F i n a l p o s i t i o n a l parameters ( f r a c t i o n a l X 10 ) with standard d e v i a t i o n s i n parentheses 4  atom w I{1) 1(2) As (1) As (2) F (1) F(2) F{3) F(4) F(5) F{6) 0(1) 0(2) 0(3) C(1) C (2) C (3) C (4) C(5) C (6) C(7) C(8) C{9) C(10) C<11)  X  2  6733 (1) 8344(1} 5627 (1) 805 3(2) 6956(2) 9743 (20) 10241 (19) 9903 (23) 7815(25) 9209 (26) 8701 (23) 6742(20) 4737(21) 6362(17) 6688 (24) 5494 (22) 6485(25) 8686(18) 8218 (19) 9677(23) 8525(40) 8997(22) 7715 (23) 6 981 (25) 6092 (24)  39 32 (1) 3338 (2) 2858 (3) 4102 (3) 1347 (3) 3296 (32) 2691 (29) 1333 (36) -1202 (36) -663 (39) -530 (37) 6410 (31) 3648 (31) 65 56 (26) 5473 (39) 3788 (33) 5613 (40) 2270 (28) 1142 (30) 2355 (36) -394 (58) 5506 (34) 4521 (37) -73 (40) 535 (38)  z 3840(1) 3427 (1) 2094(1) 5 396(2) 4439(2) 7073( 19) 6121 (18) 7008(23) 5435(22) 5574(24) 6578(24) 2526(19) 3926(19) 4800(16) 297 8(23) 3893 (20) 4431 (24) 5757 (17) 5422(18) 6418(21) 5735(36) 5546(21) 6430(21} 3550(24} 4927(22)  29  Table 4 F i n a l thermal parameters and t h e i r estimated standard deviations a) A n i s o t r o p i c thermal parameters (U-- (A ) X 10 ) 0  2  atom  U  u  D  0„  t x  U  2  0^  iX  JJ  a a  w  4.18( 6} 6.27( 7) 4. 15 ( 6) 0.16<  1(1)  5.68(11) 9.35(15) 6. 56 (1 2)-1 . 14 (10) 3.27 ( 9)-1.43(10)  1 (2)  6.39(12) 14. 10(22) 5. 15 (11) -0. 22 (13) 0 .57 ( 9) - 1. 10 (12 )  As(1)  5. 12 (14) 4.59 (15) 4. 62 (1 4)-0. 18 ( 12)  As(2)  6.37(17) 5.87(18) 5. 61 (1 6)-1. 83 (14) 2 . 21 (1 3)-0.7 4 (1 3)  lb)  Isotropic  thermal parameters  5) 1.49 ( 4) 0.17( 5)  1. 50 (11)-0. 11 (1 1)  (U x 10 ) 3  Atom  U (A )  Atom  U(A )  F(1) F(2) F(3) F(4) F(5) F(6) 0(1) 0(2) 0(3) C(1)  11.7 (7) 11.0 (7) 13.6 (9) 13.5 (9) 15 (1) 13.6 (9) 9.3 (7) 9.5(7) 7.4(5) 6.9 (8)  C(2) C{3) C(4) C(5) C{6) C (7) C(8) C(9) C(10) C(11)  5.8 (6) 7.0 (8) 4.5(5) 4.9(6) 5.9(7) 11 (1) 6.1 (7) 6.5(7) 7.4 (8) 6.9(7)  2  2  30  d i f f e r e n c e s between the b a s i c polyhedra a v a i l a b l e f o r coordinate  molecules  (18),  indicates  t h a t i n t h i s type of  molecule the i d e a l angle between the two atoms  is  capped  octahedron, and 81.5° f o r  From  180°  the  I-B-I  octahedron most  for  a  pentagonal  angle  of  would appear t o  exactly.  larger  coordinated  bipyramid, ca. 90° f o r a  a  87.3°  seven-  capped the  describe  trigonal  prism.  c h o i c e of the  the  observed  capped  geometry  F i g u r e 5 shows a general s t e r e o s c o p i c view of  the molecule, with the atom l a b e l l i n g scheme. I n d i v i d u a l bond l e n g t h s and a n g l e s , with standard  deviations  are  given  in  T a b l e s 5 and 6 r e s p e c t i v e l y . The  angles  subtended  unique carbon atom C(3) those between C(3) average  to  74  at the tungsten atom between the  and the atoms i n the capped  and  the  atoms  in  and  uncapped  125.5° i n  (2),  and  73  octahedral structures, and  128°  for  ( d i p h e n y l a r s i n o ) methane Jdibromodicarbonylmolybdenum Similarly  the  angles subtended  p a i r s of atoms i n the capped, f o r both molecules are  (1) and  an average o f 112 and  mean v a l u e s are 112.3  and  by  this  2.73  the o  capped  face.  (II)  (19) .  and p a i r s i n the uncapped f a c e s  (2) a r e comparable.  In  (1)  they  86° r e s p e c t i v e l y , while i n (2) the 89.7°.  molecule,  capped is  the  c o n t a c t s made between the capping group and in  [bis-  at the c e n t r a l metal atom by  another f e a t u r e of a d i s t o r t e d demonstrated  face,  and 128° r e s p e c t i v e l y . These a n g l e s are very  s i m i l a r t o those found i n other capped i . e . 73.6  the  f a c e , and  Hence i n (1), C{3)  octahedron close the  (17)  non-bonded three  i s 2.46,  A away from C (1) , C (2) , and A s p ) , compared to  atoms  2.26, 2.29,  and  Figure 5 g e n e r a l s t e r e o s c o p i c view o f the molecule show the c r y s t a l l o g r a p h i c numbering scheme. -  fable 5 ©  Bond l e n g t h s (A) with standard d e v i a t i o n s i n parentheses  Bond  Length  © (A)  Bond  o Length (A)  W-I(1)  2.848 (2)  C(1) -0(1)  1.17(4)  W-I(2)  2.856 (2)  C(2) -0(2)  1. 19(4)  W-As(1)  2.556 (3)  C (3)-0(3)  1. 13(4)  W-As (2)  2.618 (3)  C(4) -C(5)  1.29(4)  W-C(1)  2.00 (4)  C (4)-C (6)  1.50 (4)  H-C(2)  1.97 (4)  C (5)-C (7)  1.56 (6)  S-C (3)  1.94 (3)  C (6)-F{1)  1.35(4)  As(1)-C(4)  1.98{3)  C (6)-F(2)  1.31 (4)  As (1) -C(8)  1.92 (3)  C (6)-F{3)  1. 18(4)  As(1)-C(9)  1.95 (3)  C(7) -F{4)  1. 27(5)  As (2) -C (5)  2.00 (3)  C (7)-F(5)  1. 20 (5)  As (2) -C(10)  1.97 (4)  C(7) -F(6)  1.28(5)  As (2) -C(11)  1-93(3)  33  Table 6 Bond a n g l e s  (deg.) w i t h s t a n d a r d  Bonds  Angle  I(1)-W-I(2) I (1)-W-As (1) I (1) -W-As (2) I(1)-W-C(1) I (1)-W-C (2) I(1)-W-C(3) I (2)-W-As (1) I (2) -W-As (2) I (2)-W-C(1) I (2) -W-C (2) I (2) -W-C (3) As(1) -W-As(2) As(1)-W-C(1) As(1) -W-C (2) As (1) -W-C (3) As (2) -W-C{1) As (2) — W-C {2) As (2) -W-C (3) C(1)-W-C(2) C(1)-W-C(3) C{2) -W-C (3) W-As (1)-C (4) W-As (1)-C (8) W-As(1)-C(9) C ( 4 ) - A s ( 1 ) - C (8) C(4)-As(1)-C(9) C (8)-As(1)-C(9)  87.3 (D 78.2 (1) 83.8 [1) 78 (1) 161 (1) 128 (1) 159.4 (D 88.2 (1) 75 (1) 77 <1) 128{1) 75.9 (1) 116 (1) 113 (1) 73 (1) 155 (1) 85 (1) 128 (1) 108 (1) 77 (1; 71 (1) 111(1] 117 (1) 118(1; 108 (1 101 (1| 100 (1)  deviations  i n parentheses.  Bonds W-As(2)-C (5) W-As(2)-C (10) W-As(2) -C (11) C ( 5 ) - A s (2)-C (10) C ( 5 ) - A s (2) -C (11) C (10) - A s ( 2 ) -C (11) As(1)-C(4)-C(5) A s (1) -C (4) -C (6) C ( 5 ) - C ( 4 ) - C (6) As (2) -C (5) -C (4) A s (2) - C ( 5 ) - C ( 7 ) C ( 4 ) - C ( 5 ) - C (7) W-C (1) - 0 ( 1 ) W-C ( 2 ) - 0 ( 2 ) W-C (3) -0(3) C (4)-C(6)-F(1) C (4)-C (6)-.P(2) C (4)-C(6) - F ( 3 ) F (1)-C(6)-F(2) F (1)-C{6) -F{3) F (2)-C ( 6 ) - F ( 3 ) C (5)-C(7)-F(4) C (5)-C(7) - F ( 5 ) C (5)-C ( 7 ) - F ( 6 ) F (4)-C(7) -F{5) F (4)-C (7) -F (6) F (5)-C ( 7 ) - F ( 6 )  Angle 110| 1) 115 j 1) 120| 1) 103( 1) 105i 1) 10 3 [ 1) 119 (2) 115|[2) 127 | 3) 118|[2) 116|[3) 126 (3) 174| 3) 178 (3) 177 3) 1 10 ;3) 1 16 (3) 1 13 3) 106 3) 91 3) 1 17 [3) 109 108 ;5) 111 4) 1 19 ;5) 99 [5) 1 10 (5)  34  2.29,  and  P(1)  2.70  A f o r the r e s p e c t i v e C{1)  d i s t a n c e s i n molecule The  to C (2) ,  subtended  by  is  the  75.9(1)°. mutually  This  cis  is  The  octahedron.  atoms  The  of  j v  three  are a l s o very s i m i l a r being 155,  the geometry around the tungsten C  the  to  the  those  capped and  angles  being  l i g a n d t h e r e f o r e seems i d e a l l y s u i t e d to occupy an  edge of the capped tj:aa§  atom by  similar  uncapped f a c e s (the mean v a l u e o f the s i x such 78°).  and  (2).  angle subtended at the c e n t r a l tungsten  bidentate ligand  C (3) ,  159,  angles and  mutually  161°,  (see F i g u r e 4) a  giving  reasonable  symmetry. The  would  t u n g s t e n - i o d i n e d i s t a n c e s of 2.848 (2) and  appear  to  be  the  first  l e n g t h s i n a seven-coordinate similar  determinations  environment.  distances  in  environments  (20 and  been found  to have a mean value of 2.65  A.  ©  2,856 (2} A of W-I  bond  Tungsten-bromine 21)  have a l r e a d y  Using  a  bromine  o  covalent  1  radius  of  for  the  A (22) we can estimate a W s i n g l e  o  bond r a d i u s of 1.51 (22)  1.14  A f o r t h i s compound. With use of  iodine  1.33  covalent r a d i u s , a p r e d i c t e d H-I  e  A  bond  c  length would be 2.84 value  found  Mo(II) and  a  W-As  reasonable  agreement  with  the  value 2.852 (2) A). Assuming the r a d i i  o  are s i m i l a r the value of 2.862 A  the Mo-I distance these measured and predicts  in  o  (mean  H(II)  A,  found  of for  i n Mo(CNfi) I*- (23) i s a l s o very c l o s e t o p r e d i c t e d values., A s i m i l a r argument b  bond  length  of  2.73  e  A,  compared t o the  o 2.556 (3)  and  significant  2.618(3) shortening  bond c h a r a c t e r i n the  A is  K-As  found thought bonds  experimentally.  This  to be due t o some double caused  by  (dir-dir)  back  35  donation  from the c e n t r a l metal  atom. The  two  W-As  a l s o s i g n i f i c a n t l y d i f f e r e n t from each o t h e r ,  bonds are  which  can  be  e x p l a i n e d by c o n s i d e r a t i o n of the r e s p e c t i v e t r a n s l i g a n d s . A t£M§  l i g a n d can a f f e c t the extent of back donation  metal, hence the 1(2)  from the  atom trans to A s ( 1 ) , i s not as strong a  dir a c c e p t i n g group as the  C(1)-0{1)  group  trans  to  As(2)  which should r e s u l t i n a greater back donation to As(1). T h i s will  cause  a s h o r t e n i n g o f the H-As(1) bond with r e s p e c t to  the W-As{2) bond, the d i f f e r e n c e found The 1.16(4)  H-C ©  and  C-0  distances  A)  and  the  W-C-0  found  in  s i m i l a r t o those  j o i n e d to tungsten The  ©  being 0.062 A.  (mean  angles ether  values  1.97(4)  (mean value  compounds  176(3)°) a r e  with  carbonyls  (24).  f i v e membered r i n g i s i n a 'puckered'  conformation.  Table 7 g i v e s the eguation of a weighted  least-squares  plane,  from the p l a n e ,  with  deviations  of  the  v a l u e s f o r the d i h e d r a l angles i n •puckered*  conformation,  atoms the  with both  ring.  carbon  ring,  bend i n the r i n g  has  been found  This  for  value  of  the carbon-carbon 1.34  110.5°  2  tha  five  A }  carbonyl  c o n t a c t s (26) .  double bond l e n g t h of 1.29(4)  (27) , nor the H-As-C  bond  angle  mean  (expected t e t r a h e d r a l value of 109.5°) and  the As-C-C bond a n g l e s , mean value of sp  of  i s probably t o i n c r e a s e c o n t a c t s between the  groups r a t h e r than the methyl-iodine  A (expected  and  i n other compounds (25). The  methyl groups on the a r s e n i c atoms and the adjacent  Neither  type  mean  atoms on the same  s i d e of the weighted l e a s t - s q u a r e s mean plane membered  and  118.5°  (expected  h y b r i d i z e d carbons of 120.0°) are s i g n i f i c a n t l y  for  different  36  Table 7 a) Equation o f weighted l e a s t - s q u a r e s mean plane* f o r the f i v e membered r i n g atom B As{2) As(2) C(4) C(5)  A (A)  A/<r  0.0015 -0.0105 -0.0127 0.7055 0.6139  1.404 3.822 3.970 24.447 20.574  * plane: 0.894X - 0.151Y - 0.421Z = 4.240, where X,Y, and 2 are o r t h o g o n a l angstrom c o o r d i n a t e s d e r i v e d as f o l l o w s i-Xn III  =  *-Z-«  r a I 0 «- o  0  ccos P x-, 0 i H I c s i n p -» «-z-« n  b 0  r  b) D i h e d r a l angles i n the f i v e membered Atom 1 As (2) As (1) W W  As(1)  Atom 2 H SJ  &s(1) As (2) C(4)  Atom 3  Atom 4  As{1) As (2) C(4) C (5) C{5)  C(4) C (5) C(5) C (4) As (2)  Angle  ring  (deg.)  23(1) -20 (1) -26(2) 12 (2) 8 (2)  Figure & p r o j e c t i o n of the  6  structure  down the  h axis.  38  £rom  their  expected v a l u e s . Both the A s ( 1 ) - C ( 4 ) and  stated  o  As(2)-C(5) bond similar  to  distances  the  of  1.98(3)  and  2.00(3)  A  are  AS-CH3 bond l e n g t h s (mean, 1.98(3) A) as i s  found i n other s i m i l a r l i g a n d s (28). From the r e l a t i v e u n c e r t a i n t y of the two  CF 3  groups,  it  seems  positions  unreasonable  to  of  the  attempt  any  meaningful d i s c u s s i o n of t h e i r bond l e n g t h s and a n g l e s . The i n t e r m o l e c u l a r packing appears to be governed by van der K a a l s i n t e r a c t i o n s . A p r o j e c t i o n o f the  solely  structure  down the b a x i s i s shown i n F i g u r e 6. The  n.m.r.  data  molecular rearrangement crystal rapid  structure  f o r t h i s compound must be  would  (9) i n d i c a t e d  occuring  suggest  in  solution.  that The  t h a t the process i n v o l v e s  s c r a m b l i n g of the c a r b o n y l groups and the i o d i n e atoms,  and simultaneous m i g r a t i o n of faces spectra  of  the at  corresponding  [AstCxI^]  -70°C to  the  capping  octahedron;  indicates  that  the  The  temperature.  over  the  sharpness o f the  limiting  the s o l i d s t a t e s t r u c t u r e  only a t a much lower  group  spectrum  would be reached  CHAPTER 3  CRYSTAL AND DIMETHYLAMMONIUM  MOLECULAR STRUCTURE OF  TRICHLOROTRIS (DIMETHYLSULPHOXIDE) RUTHENATE (II) .  40  INTRODUCTION  From t h e spectral  results  data  of  the  infrared  on dimethylammonium  (dimethylsulphoxide)ruthenate(II) all  three  dimethylsulphoxide  the  anion  was  in  crystallographic assignment useful  the  study  in  explaining  l  H  n.m.r.  trichlorotris(29) i f  was  thought  fac-configuration. undertaken  structural the  that  l i g a n d s were S-bonded and t h a t  was  and d e t e r m i n e  and  The  to  X-ray  verify  this  p a r a m e t e r s w h i c h c o u l d be  catalytic  properties  of  these  materials.,  EXPERIMENTAL  Ruthenium  trichloride  dimethylsulphoxide  (1ml)  dimethylacetamide resulting  concentrated product  to  which  study  was  and  Unit  with  [ ((CH ) 3  z  c parallel  and s p a c e  and  RuCl  a  measured  on  a  and NN' -  vacuum  (or yellow dried.  ] [ (CHjJ^NH^] f r o m chosen  for  t o t h e g o n i o s t a t a x i s and  data  measurements.  in  temperature  The c r y s t a l  The  of 0.25 x  were o b t a i n e d unit-cell  by a l e a s t - s q u a r e s t r e a t m e n t  reflections  3  a cross section  group  80°C  Ru)  h y d r o g e n f o r 4 h . The  ether, SO)  39%  and gave a b r i g h t  gave y e l l o w c u b e s .  diffTactometer  at  1 atm  cooled)  i n l e n g t h with  cell  were r e f i n e d 20  and  mounted w i t h  was c a . 0.3 mm mm.  of  heated  under  washed  Recrystallization  (1g#  was s e t a s i d e a t room  10ml  was  dimethylacetamide  were  (20ml)  red solution  trihydrate  of sin © 2  d i f f r actometer  from  0.2 5 film  parameters values f o r with  MoK«*.  41  radiation. Crystal  Data.  CgH Cl<3NO RuS , ab  a = 27.459(5), D =  s  b = 9.925 ( 1 ) , 3  F(000) =  1984  cm-*  ) . Absent  the  space  c=  M = 487.9 Orthorhombic, © o 14. 266 (3) A, 0 = 3 8 8 7 ( 1 ) A , 3  1=8,  1.67(1) gem- ,  m  3  (20 °C,  D =  HoK<*  reflections:  group as e i t h e r  1. 667 (5) gcm~ , o 3  c  X=  ,  0.71069  O k l , k+1 Pnma  (D**  A,  /x =  15.036 define  * 2n,  hkO,  h # 2n  , No.  62)  o r Pn2, a  (C| , v  No. ,33) . Intensities Electric Mo  K<*  29  XBD  Datex-automated  General  6 diffTactometer, w i t h a s c i n t i l l a t i o n  counter,  (zirconium f i l t e r  scan  degrees each  were measured on  at  2°  i n 2©,  end  min"  with  and  p u l s e h e i g h t a n a l y s e r ) , and  over  1  a  a range  of  (1.80  10 s b a c k g r o u n d c o u n t s  of the scan.  Data  + 0.86  being  were measured t o 29  a  8—  tan  9)  measured  at  = 45°  (minimum  was  monitored  ©  interplanar every  50  A) .  s p a c i n g 0.93 reflections  g r e a t e s t d e v i a t i o n from final and  intensity  polarization  amplitudes due  to  the  had  low  the  v a l u e was  1.067  t h e 2637  intensities  times the  data c o l l e c t i o n .  initial  background and  a similar  the f a i r l y  than  count.  the  was  uniform  count  and  These r e f l e c t i o n s  were  manner t o t h a t  structure  reflections  g i v e n z e r o weight i n the STRUCTURE ANALYSIS described  the  value. Lorentz  applied shape  of  measured,  3«-(I) above b a c k g r o u n d  with S = scan  The  +11.1% and  absorption correction  independent  less  (0.05S)2  averaged  as u n o b s e r v e d  initial  v a l u e of /*., and  * B +  In  the  c o r r e c t i o n s were a p p l i e d , and  «" (I) = S 2  throughout  were d e r i v e d . No  t h e c r y s t a l . Of 676  was  A check r e f l e c t i o n  B =  where time  classified  refinement.  in  the  previous  chapter  a Patterson  f u n c t i o n was used t o s o l v e t h e s t r u c t u r e  o f t h e compound. However, t h e i n i t i a l structure  in  the  space  group  0,0.5-2y,0 i n t h e P a t t e r s o n  to  was t h e c a s e  attempt  was  the anion  then  made  to  four  eguivalent  l  Since  positions,  unit.  In  the  P a t t e r s o n map a r e t o be f o u n d of  refinements. refinement for  these  and  One  kept  two r u t h e n i u m  of  gave  and  only  be  two  in  the  atom v e c t o r s on t h e plane  2x,  assigned  point  1/2,  throughout  full-matrix  and i s o t r o p i c  an  the  carbon  later  least-squares parameters  atoms p r o d u c e d a n R f a c t o r  o f 0.45. A  the R  along  the y coordinate  t h e p o s i t i o n s o f the s i x c h l o r i n e  positional  and  isotropic  fourteen thermal  v a l u e o f 0.19. The d i f f e r e n c e map a t  s t a g e r e v e a l e d t h e p o s i t i o n s of the remaining  nitrogen  has  atoms. Two f u r t h e r c y c l e s f o r t h e s e  parameters  an  thermal  Fourier revealed  varying  mirror  y values unspecified. In t h i s  constant  cycle  atoms s t i l l  this  heavy  was a r b i t r a r i l y  was  s i xsulphur  molecules  i s no u n i q u e o r i g i n  of the p o s i t i o n a l  difference  have  symmetry,  must  on the H a r k e r  their  s p a c e g r o u p , however, t h e r e  which  the o r i g i n . I f  t h e map gave t h e x and z c o o r d i n a t e s o f  but l e f t  b a x i s s o Ru (2)  mirror  there  Pn2,a  0.000,  than  t h i s s p a c e group  asymmetric  the  three-dimensional  s o l v e the s t r u c t u r e i n the non-  non-equivalent  and R u ( 2 ) ,  The  possess  crystallographically  Ru(1)  the  r e q u i r e d a maximum a t  peak o t h e r  could  space group, Pn2 a.  Examination  solve  t h e atom on t h e c r y s t a l l o g r a p h i c  centric  2y.  to  t h e y c o o r d i n a t e f o r t h e Ru atom would  be 0.25, l o c a t i n g  plane. Although  Pnma  function.  P a t t e r s o n map r e v e a l e d no s u c h this  attempt  atoms.  After  several  24 o x y g e n ,  more  cycles  convergence  was  finally  reached,  s c a t t e r i n g c o r r e c t i o n f o r the  Ru,  using  C l , and  an S  anomalous  atoms,  and  v a r y i n g t h e p o s i t i o n a l and a n i s o t r o p i c t h e r m a l parameters f o r atoms,  R ~ 0.045 f o r 1943 observed  all  the  (the  f o l l o w i n g r e f l e c t i o n s were removed from the data s e t i n  the  final  stages  resulting  from  malfunction: 1  at  of  refinement  extinction,  due  to  reflections  suspected e r r o r s  absorption,  and  instrument  4 0 0, 2 4 0, 19 0 1, 21 0 1, 2 1 1, 10 0 2, 17  2, 14 0 3, 4 0 4, 9 0 4, 12 0 4, 3 0 5, 2 3 5, 8 0 7, 10 6  7, 19 0 8, 0 1 9, and 1 0 14.) Due  to  the a d d i t i o n a l  expense  involved  in  further  refinement f o r a s t r u c t u r e with so many v a r i a b l e s , b e a r i n g i n mind  the  reason  difficulty made  to  behind t h e i n v e s t i g a t i o n , and the i n h e r e n t  with so many heavy atoms present, no determine  or  hydrogen  atoms  was  r e f i n e the p o s i t i o n s of t h e hydrogen  atoms i n t h e R u C l (Me S0)^ 3  attempt  z  molecules. The  positions  o f the  bonded d i r e c t l y t o t h e n i t r o g e n atoms i n the e  c a t i o n s were c a l c u l a t e d  (assuming a N-H bond l e n g t h of 0.99 A  and a H-N-H angle of 108°.) to g i v e an i d e a o f t h e i n t e r i o n i c bonding. These atoms  were  not  included  in  the  structure  refinement. The  scattering  factors  were  anomalous s c a t t e r i n g c o r r e c t i o n s Ru,  Cl  and  |Fo| < 65; unobserved  S  atoms.  The  taken  (15) were  weighting  /w = 65/1 Foi i f |Fo| > 65 reflections  from  r e f . 14 and  applied  f o r the  scheme: /~w = 1 and J~v = 0-0  i f for  gave constant average v a l u e s of  w ( F o - F c ) over ranges o f |Foj and 2  s t a g e s of refinement. The f i n a l  was  used  in  the  p o s i t i o n a l and thermal  final  Table 8 Final positional  parameters ( f r a c t i o n a l x 10*)  with estimated standard d e v i a t i o n s i n parentheses Atom Ru(1) Ru (2) C l (11) Cl(12) Cl(13) C l (21) Cl{22) C l (23) S(11) S(12) S(13) S(21) S (22) S (23) 0(111) 0 (121) 0(131) 0(211) 0 (221) 0(231) C(111) C(112) C(121) C (122) C(131) C(132) C(211) C (212) C(221) C (222) C{231) C(232) N ( 1) N(2) C(11) C(12) C(21) C (22) H(11) H(12) H(21) H (22)  X 2560 (0) 283(0) 1670(1) 2489(2) 2563(2) 1094 (2) 469 (2) 640 (2) 3381 (1) 2556 (2) 254 8(2) 9543 (1) 16(2) 128 (2) 3657(5) 2672(5) 3 026 (5) 9154 (4) 948 7 (6) 9823 (7) 3606(8) 3638 (8) 2948(7) 1970(8) 2 335(9) 2105(8) 9575(7) 9299 (6) 293 (13) 233 (9) 9 857 (9) 675(11) 3646 (6) 1569 (6) 3 297 (8) 3790(10) 1870 (7) 1378 (9) 3944 3500 1768 1292  I 4849 (2) 0 4795(6) 3399(5) 2834 (5) 10090 (8) 2095(6) 8823 (7) 4766 (6) 6598 (5) 6206 (5) 10104(7) 1123 (6) 7954(6) 5966 (14) 7981 (14) 6846 (13) 9221(15) 1271 (18) 7888 (17) 3435 (22) 4336(23) 6334 (20) 6759(27) 5372 (22) 7535(20) -125 (37) 1795(26) 2769 (24) 491(27) 6784 (28) 7074 (24) 880 9(18) 1629(15) 9802 (28) 9068 (28) 413 (19) 1719(22) 8818 7900 2438 1624  z 3945 ( 1) 2858 (1) 3851 (3) 5299 {3) 2997 j[3) 2176 \,3) 3640 {A ) 4181| «0 3943 < [3) 4961 | [3) 2680 | [3) 3 556 |(3) 1567 (3) 2231 i[*») 4246 (11) 4620 (9) 2425 (9) 3 198 (10) 1434 (10) 1401 (11) 4669 (18) 2772 (15) 5956 (12) 5528 (16) 1655 (13) 2752 (14) 4788 (11) 3530 (17) 15 10 (21) 499 (15) 3017 (20) 2026 (26) 3556 (13) 4378 (12) 3173 (17) 4564 (17) 4212 (16) 5336 (14) 3163 3513 4248 3934  Table 9 F i n a l thermal parameters and t h e i r estimated standard anisotropic  thermal pa ra me te r s  deviations (U ^  x  10  2  o A*}  atom Ru(1) Ru (2) Cl(11) C l (12) Cl(13) C l (21) Cl{22) C l (23) S(11) S (12) S(13) S(21) S (22) S(23) 0(111) 0 (121) 0(131) 0 (211) 0(221) 0 (231) C{111) C (112) C (121) C(122) C (131) C (132) C(211) C (212) C (221) C (222) C (231) C (232) W(1) H(2) C(11) C(21) C(12) C (22)  3.28 (8) 2.82(8) 3.5(2) 6.5 (3) 6.5 (3) 3.4(2) 4.6(3) 5.5 (3) 3.2(2) 3.0 (2) 4.3 (3) 3.4 (2) 4.7(3) 5.7 (3) 2.5(7) 5.5(8) 4.8(8) 2. 1 (7) 7(1) 13(1) 4(1) 5(1) 5(1) 4(1) 9(2) 6(1) 6 (1) 1.2(9) 16 (3) 7(1) 7 (2) 9(2) 5(1) 3. 9(9) 6(1) 3(1) 10(2) 7(2)  2.10(6) 3.56(7) 4.1 (3) 3.2 (3) 2.7 (2) 7.5 (3) 4.5 (3) 6.9 (4) 3.4 (3) 3.2 (2) 2. 1 (2) 5.1 (3) 4.5 (3) 3.8 (3) 4.4(9) 3.4 (7) 3.9(8) 7.2 (9) 9 (1) 5(1) 5(1) 6(1) 4 (1) 9 (2) 5 (1) 4(1) 11(2) 9 (2) 4 (2) 10(2) 8 (2) 3(1) 3.4 (9) 2.4(9} 6 (2) 4(1) 8 (2) 6 (2)  1. 82 (5) 2.81 (6) 4. 2(2) 2.7 (2) 3.4(2) 5.3(2) 6.4(3) 4. 9(3) 3.7(2) 1.9(2) 1.9(2) 3.0(2) 3.6(3} 5.6(3) 9(1) 4.5(7) 4. 1 (7) 6. 0(8) 4. 3 (8) 5. 8(9) 9(2) 6(1) 3(1) 5(1) 2.5 (9) 5(1) 2.7 (9) 9(2) 10(2) 3(1) 10 (2) 18(3} 8(1) 6(1) 9(1) 9(2} 6(1) 3(1)  -0. 1 1 (8) -0.40 (6) -0.5 (3) - 1 . 1 (2) 0.1 (2) -0.4(3) -0.8 (2) 0.1 (3) 0.8 (2) -0.2(2) 0.1 (2) -0.4 (3) 0.3 (2) -0.4 (2) -1.0 (6) -0.7(6) -1.2 (7) -1.6 (7) 3 (1) -0(1) 2(1) 2(1) -1(1) -3 (1 ) 2(1) 1 (1) 1(2) 2(1) -3(2) 1 (1) -3(1} 0(1) 1.0(9) 0.7(7) 1(1) 0.6 (8) -3(2) -1(1)  -0.07(4) -0.12 (6) -0.2 I(2) -0.9 [2) -1.2 [2) 0.9 [2) -1.4 (3) -1.3 [3) 0. 1 (3) 0.3([2) 0.4 (2) 0.2 (2) -0.7 (2) -1.3 (3) 0.6 (?) 0.3 (6) 0.5 (6) 0.4 (6) -1.6 (8) -3(1) -2(1) -1(1) -1. 1 (9) 3(1) -2(1) -0(1) 1.6 (8) 1(1) -2(2) -0(1) -3(2) -2 (2) 2(1] 0.8 (8) 3(1) -0(1) -0(1] -1(1)  0.04(6) 0.37 (9) 0.5 ( 3) 1.4( 2) -0.5 { 2) 0.5( 3) - 1.3 ( 3) 2-0 | 3) -0.9 | 2) -0.0( 2) 0. 1 (2) 0.5 | 2) 1.3( 2) 0.3| 3) -0.8 i 8) 0.0j 7) 1.0i 6) 0.4j 8) 0.0 9) - 0 . 2 i 8) 1 (1) -3 (1) -0.3 |[9) "2 (1) - 0.6 | 9} 2 (D 1 (2) -4 (1) 3 (1) 0 (1) 5(2) -0 (2) 0.6 [9) -0.6 [8) 2 (2) -1 (D 0 (1) -0 (1)  46  parameters a r e given i n Tables 8 and 9 r e s p e c t i v e l y . Measured and  calculated  structure  factors  are a v a i l a b l e  from t h e  U.B.C. L i b r a r y . RESULTS AND DISCUSSION The s t r u c t u r e c o n s i s t s of two c r y s t a l l o g r a p h i c a l l y equivalent  anions i n the asymmetric  eguivalent  dimethylammonium  scheme  i s illustrated  non-  u n i t , l i n k e d by two non-  cations.  The  atom  labelling  i n F i g u r e 7. Most c o r r e s p o n d i n g bond  l e n g t h s and a n g l e s a r e not  significantly  different  between  the two independent formula u n i t s , a s can be seen from T a b l e s 10 and 11. A l l three DMSO l i g a n d s a r e c o o r d i n a t e d through t h e sulphur  atoms, the c o o r d i n a t i o n  geometry about  the ruthenium  atoms being e s s e n t i a l l y t h a t o f an octahedron, with each DMSO l i g a n d having a c h l o r i n e atom i n a distortion  does occur, presumably  trans  position.  due t o s t e r i c  between the DMSO groups, t h e C l - R u - C l angles smaller  than 90° [87.1-88.3(2)°,  S-Ru-S a r e s l i g h t l y  Slight  interference  being  slightly  mean 87.6°] w h i l e those f o r  l a r g e r [ 92.0-93.4(2)°,  mean 92.6°].  o The are  o  Ru-S bond l e n g t h s [ 2.25 2-2. 273 (5) A,  significantly  longer  o  while  t h e S-0  mean  2.261 A ]  d i s t a n c e s [ 1.45-  o  1.50(1) A, mean 1.48 A] are s h o r t e r  found  in o  (30) i . e . 2.188(3) A and 1.527 (8) A  2  b  These  those o  [ Ru (NH3 )s DMSO * 2 P F - J respectively.  than  changes  i n bond  length  indicate  a  decrease i n the p o s s i b l e dir-jr«r back donation from the c e n t r a l metal  t o t h e s u l p h u r atom caused by the c o m p e t i t i o n from t h e  other  DMSO  Similar  ligands  effects o  f o r the a v a i l a b l e are  seen ©  "W-donor  orbitals.  f o r trans-PdClj{DMS0) [Pd-S  2.299 (2) A, and S-0 1.476(5) A J (31) and c i s -  a  A g e n e r a l view o f the s t r u c t u r e showing the c r y s t a l l o g r a p h i c numbering scheme.  48  T a b l e J.0 Bond L e n g t h s  o (A) w i t h s t a n d a r d  deviations  i n parentheses.  o Bond  Length  (A)  Bond  Length  o (A)  Bu (1) - C l ( 1 1)  2. 450 (4)  Ru (2) - C l (21)  2. 430(4)  Ru (1) - C l (12)  2. 417(4)  Ru (2) - C l (22)  2. 414(5)  Ru (1.) - C l (13)  2. 415 (5)  Ru (2) - C l (23)  2. 427(5)  Ru (1) -S(11)  2. 256 (4)  Ru (2) -S (21)  2. 267(4)  Ru (1) -S(12)  2. 261 (5)  Ru (2) -S(22)  2. 273 (5)  Ru (1) -S(13)  2. 252 (4)  Bu(2) -S (23)  2. 260(5)  S (11) -0(111)  1. 48(1)  S (21) -0 (21 1)  1. 47 (1)  -0 (121)  1. 49 (1)  S (22) -0 (221)  1. 47(2)  S {13) -0(131)  1. 50(1)  S (23) -0 (231)  1. 45 (2)  S (11) -C(111)  1. 79 (2)  S (21) -C (21 1}  1. 77 (2)  S (11) -C (112)  1. 86 (2)  S (21) -C (212)  1. 8 1 (2)  S (12) -C(121)  1. 80 (2)  S (22) -C (221)  1. 80 (2)  S (12) -C (122)  1. 81 (2)  S (22) -C (222)  1. 75(2)  S { 13)-C (131)  1. 78 (2)  S (23) -C (231)  1. 78 (3)  S (13) -C(132)  1. 80 (2)  S (23) -C (232)  1. 7 6 (3)  N(1)  -C(11)  1. 48 (3)  N(2)  -C(21)  1. 48(2)  N(1)  -C(12)  1. 51 (3)  N{2)  -C (22)  1. 47(3)  S{12)  49  T a b l e jn Bond a n g l e s  (deg) w i t h s t a n d a r d d e v i a t i o n s i n p a r e n t h e s e s .  Bonds C l ( 1 1 ) -Ru (1) - C l (12) Cl(11) -Ru( 1) - C l ( 1 3 ) C l (1 1) -Ru(1) -s ( 11) C l (11)-Ru (1)-s j 12) Cl(11) -Ru(1) -S ( 13} C l (12) -Ru (1) - C l (13) C l ( 1 2 ) -Ru{1)-s { 11) Cl{12) -Ru{ 1)-S (12) C l (12) -Ru{1) -S |13) Cl(13) -Ru(1) -s | 11) C l ( 1 3 ) -Ru (1) -S i 12) Cl(13) -Ru (1) -s |13) S(11) -Ru(1) -s I 12) S(11) -Ru (1) -s \ 13) S(12) -Ru{ 1) -s | 13) Eu(1) -S (11) -0 i 1 11) Ru{1) -S (12) -0 i 121) Ru(1) -S(13) -0 |131) Ru(1) -S (11) -C I 1 11) Ru(1) -S (11) - c 11 12) Ru(1) -S (12) -c 121) Ru(1) -S (12) -C i 122) RU(1) -S{13) -C \131) Ru(1) -S (13) -C |132) 0(111) -S(11) -C i 1 11} 0(111) -S (1 1)-c [1 12) 0(121) -S{12) - c |121) 0(121) -S (12) -c 122) 0(131) -S (13) ~C !131} 0(131) -S (13) -C [132) C(11 1) -S(11) - c |[112) C(121) -S (12) -c 1122) C(131) -S{13) - c ;132) C(11) -13(1) -c {12)  Angle (deg) 87.1(2) 87.4(2) 175.4 (2) 92.7 (2) 87.4(2} 87.4 (2) 93.4(2) 86.8(2) 174.5 (2) 88.0(2) 174.2(2) 92.6 (2) 92.0(2) 92. 0 (2) 93. 1 (2) 118.9 (6) 119.8 (5) 115.7 (5) 111.8 (8) 1 12.8 (7) 113.0 (7) 111.1 (8) 112.7(8) 113.8 (7) 104.4 (9) 104.6(9) 105.3(8) 105 (1) 107 (1) 107.1 (9) 103 (1) 101 (1) 100 (1) 114 (2)  Bonds C l (21) -Ru (2) - C l ( 2 2 ) C l ( 2 1 ) -Ru (2) -Cl{2 3) C l (21) -Ru (2) -S (21) C l (21 j -Ru(2) -S (22) C l ( 2 1 ) -Ru (2) -S (23) C l (22) -Ru (2) - C l ( 2 3 ) C l ( 2 2 ) -Ru (2) -S (21) C l (22; -Ru (2) -S (22) C l (22) -Ru (2) -S (23) C l (23] -Ru (2) -S (21) Cl(23; -Ru (2) -S (22) C l (23] -Ru (2) -S (23) S (21) -Su (2) -S (22) S (21) -Ru (2) -S (23) S (22) -Ru (2) -S (23) Su (2) -S(21) -0 (211) Ru (2) -5(22) -0 (221) Ru (2) -S(23) -0 (231) Ru (2) -S(21) -C (2 11) Ru(2) -S(21) -C (212) Ru (2) -S (22j -C (221) Ru (2) -S(22) -C (222) Ru (2) -S(23, -C (231) Ru (2) -S(23) -C (232) 0 (211]|-S(21] -C (211) 0 (211 -S{21) -C (212) 0 (221 i-S (22] -C (221) 0 (221 -S{22; -C (222) 0 (231 i-S (23' -C (23 1) 0 (231 -S(23; -C (232) C (211 |-S(21]|-C (212) C (221 -S(22) -C (222) C (231 I -S(23]-C (232) C (21) -N (2) -C (22)  Angle (deg) 87.7 (2) 87.7 (2) 174.7 (2) 87.3(2) 92.7 (2) 88.3 (2) 86. 9(2) 91.2 (2) 175.4 (2) 92.4 (2) 175.0 (2) 87.2 (2) 92.5 (2) 92.6 (2) 9 3.4 (2) 118. 1 (6) 118.2 (7) 118. 2 (7) 112. 6 (6) 111.4 (7) 110(1} 114.8 (8) 115(1) 110(1) 108(1) 106(1) 109(1) 105(1) 104(1) 110(1) 99(1) 98 (1) 98(1) 113(2)  50  o  o  Pa (N0 ) (DMS0) 3  x  [ Pd-S 2.231(3) A, and S-0 1.463 (7) A]  2  The s t r o n g t r a n s e f f e c t o f sulphur-bonded is  illustrated  in  the 8 u-Cl bond  (32).  DMSO l i g a n d s (33) d i s t a n c e s [2.414-  2.450 (4) A, mean 2.426 A] which are s i g n i f i c a n t l y longer than ©  those f o r t h e mutually t r a n s c h l o r i n e atoms [mean 2.390(7) A ] in  the octahedral  complex  RuClj(K C H^(CHj)) z  b  (P ( C H ) ) . b  s  a  2  ( C H ) 0 (34) . 3  l  The'  geometry  about  the sulphur atoms i s the expected  d i s t o r t e d t e t r a h e d r o n with values 118.2°,  of  115.7-119.8(5)°,  mean  f o r the 8u-S-0 a n g l e s , and 110-115(1)°, mean 112°,  f o r t h e Hu-S-C angles. The values of the O-S-C 110(1)°,  mean  106°],  the C-S-C angles  angles [104-  [ 98-103 (1)°, mean o  o  100°], and t h e S-C bond l e n g t h s [1.7 5-1.86(2) A, mean 1.79 A ] are very s i m i l a r t o those found f o r f r e e DMSO [107°, 98° and e  1.80-1.82(1) A r e s p e c t i v e l y ] (35). The  hydrogen atoms attached to the n i t r o g e n atoms i n t h e  dimethylammonium both  c a t i o n s are i n v o l v e d i n hydrogen bonding t o  non-eguivalent anions, forming  throughout  chain-like  structure  the c r y s t a l l a t t i c e . H (11) and H(12) take part i n  N-H ..... 0 hydrogen involved  a  bonding,  i n N-H . . . C l  atom s e p a r a t i o n s do  while  hydrogen  not uniquely  H(21) and H(22) a r e bonding.  define  Although  heavy  the presence  of  hydrogen bonding, they can g i v e a reasonable i n d i c a t i o n , v a l u e s o f t y p i c a l heavy atom c o n t a c t d i s t a n c e s being 2.9 A o  and  3.3  A  f o r N . . . . 0.  and N . . . C l hydrogen bonded  atoms (36 and 37). From Table 12 i t can be seen  that  several  of t h e s e p a r a t i o n s a r e w e l l above these values, tending to  51  Table 12 Values o f O . . . , N, 0 . . . H, C l . . . N and C l . . . H intermolecular contacts. -Distance (A)  Atoms  . Atoms  -Distance (A)  0 (111)-N (1)  2.99 (2)  0(111] -H(12)  2.2  0 (121)  (1)  3.18(2)  0(121) -H (1 2)  2.8  0(131)-N{1)  3.05 (3)  0 (131 ] -H(12)  2.3  0 (21 1)-H{1).  2.89 (2)  0 (211) -H ( 11)  2.1  0 (221)-N (1)  3.36 (3)  0(221] -H(11)  2.9  0(231)-N (1)  3.36(3)  0(231) -H(11)  2.7  C l ( 1 1)-N(2)  3.24(3)  c i (11) -H(21)  2.4  Cl(12)-N (2)  3.35 (3)  Cl(12) -H(21)  2.7  C l (13)-N (2)  3.57 (4)  Cl(13) -H(21)  2.8  C l (21)-N (2)  3.73(4)  C l (21) -H (22)  3.0  Cl(22) —N (2)  3. 23 (3)  C l (22) -H (22)  2.3  Cl(23) -N{2)  3.79(4)  Cl(23) -H (22)  3.3  -K  Due t o the hydrogen p o s i t i o n s being c a l c u l a t e d the e r r o r s in t h e 0 ....... H, and C l . . . H d i s t a n c e s are s u b j e c t t o speculation.  Fiqure  8  A s t e r e o s c o p i c diagram o f the u n i t c e l l viewed down c; hydroqen bonds a r e i n d i c a t e d by d o t t e d l i n e s . r u l e out the  presence o f hydroqen bonding f o r these  and  atoms. U n f o r t u n a t e l y  oxygen  be somewhat s p e c u l a t i v e , but 0  the hydroqen p o s i t i o n s must  the t r e n d s  . . . H and C l . . . H s e p a r a t i o n s  the  heavy  atom  contacts.  Typical  and  3.0  would  A f o r van indicate  der the  A and  Haals contact  indicated  support  from  the  the f i n d i n g s f o r  observed  o  H . . . C l d i s t a n c e s a r e 2.0  chlorine  H . - . 0  and  *  2.4  e  A  compared  o n l y . The  p r e s e n c e o f at l e a s t  to  overall  2.6  A  results  s i x hydroqen bonds  N(1)-H{12) . . . 0 ( 1 1 1 ) , N(1)-H(12) . . . 0(131), N(1)-H(11) . . . 0 ( 2 1 1 ) , N(2)-H(21) . . . N(2)-H(21) . . . C l ( 1 2 ) shows the c o n t e n t s  and  o f the  N(2)-H(22) . . .  unit c e l l  hydrogen bonds i n d i c a t e d by  Cl(11), Cl(22). Fiqure 8  viewed along c-with  the d o t t e d  lines.  these  CHAPTER 4  CRYSTAL AND MOLECULAR  STRUCTURE OF  DXCHLOROTETRAKIS (DIMETHYLSULPHOXIDE) RUTHENIUM ( I I )  54  INTRODUCTION Infrared  and  *H  n. m. r. , s p e c t r a l  data  on  d i c h l o r o t e t r a k i s (dimethylsulphoxide) ruthenium (II) the  possibility  of  dimethylsulphoxide study  of  unusual  mixture  ligands  of  t h a t gained from  and  S-bonded  (38). The X-ray  [ (MejSO)i^RuCla, ] was  assignment,  ruthenium  a  and  O-bonded  crystallographic  undertaken  provide  indicated  to  verify  a d d i t i o n a l information to  the s t r u c t u r e presented i n Chapter  dimethylsulphoxide  this  3 (29)  on  complexes.  EXPERIMENTAL 1g o f ruthenium  trichloride  (20ml) under hydrogen a  blue  solution.  was  (1 atm) f o r approximately  a  further  from methanol gave yellow  f o r study  was  mounted  with  g o n i o s t a t a x i s and had dimensions mm.  Unit-cell  and  and d i f f r a c t o m e t e r  8hr producing  2  hours  space  of  cubes. c* ca  added  finally  reflections  measurements.  measured  The  crystal  parallel  to the  0.20 x 0.20 x 0.2 5  group data were obtained from The  unit-cell  were r e f i n e d by a l e a s t - s q u a r e s treatment 21  methanol  r e d s o l u t i o n . C o o l i n g and r e c r y s t a l l i z a t i o n o f  (MeiSO)H.RuCli chosen  in  4ml of d i m e t h y l s u l p h o x i d e were then  and t h e r e f l u x i n g continued f o r a producing  refluxed  on  a  film  parameters  of s i n © v a l u e s f o r 2  diffractometer  with  Mo K«t  radiation.. Crystal  ' Data.  a = 8.939 (3), U = 1832 (1)  CfHi* C l j O ^ u S ^ b = 18.045(7),  A , 3  0^=  ,  M = 484.54  ,  c = 11.363(3) A, P=  1.74(1) gcm-3 Z = 4,  0 = t  monoclinic, 91.52(2)°  1.76(1) gcm-3,  ©  F(000) = 984 (20°C,  Mo K*,  X = 0.71069 A,  A = 15.66 c r > ) .  55  Absent  reflections:  hOl,  h>l # 2n,  uniquely the space group P2,/n  (C|^, No.  I n t e n s i t i e s were measured on a Electric  XRD  scan  at  k # 2n  define  14).  Datex-automated  General  6 d i f f r a c t o m e t e r , with a s c i n t i l l a t i o n c o u n t e r ,  Mo K « (zirconium f i l t e r 29  QkO,  2°  and  min-*  pulse height a n a l y s e r ) , and  over  a range of  degrees i n 29, with 20 s background  {1.80  + 0.86  a  tan 9)  counts being measured  each end of the scan. Data were measured t o 29 = 45°  9-  at  (minimum  e  i n t e r planar  spacing 0.93  every 50 r e f l e c t i o n s greatest  deviation  f i n a l i n t e n s i t y was and  A) . A check r e f l e x i o n was  throughout  the  data  from the i n i t i a l 0.962 times the  monitored  collection.  value was +7.8% initial  value.  The  and the Lorentz  p o l a r i z a t i o n c o r r e c t i o n s were a p p l i e d , and the s t r u c t u r e  amplitudes were d e r i v e d . No a b s o r p t i o n c o r r e c t i o n was due to the low value of/* , and t h e f a i r l y the  crystal.  Of  the 3231  -  z  = S  +  B  *  averaged background as unobserved  (0.05S)  shape  of  independent r e f l e c t i o n s measured,  511 had i n t e n s i t i e s l e s s than 3« (I)  <r (D  uniform  applied  2  above  background  where  with S = scan count and B = time  count. These  r e f l e c t i o n s were  classified  and given z e r o weight i n the refinement. STRUCTURE ANALYSIS  The  p o s i t i o n o f the ruthenium atom was again determined  from the t h r e e - d i m e n s i o n a l P a t t e r s o n f u n c t i o n . One full-matrix  least-squares  refinement  cycle  of the p o s i t i o n a l and  i s o t r o p i c thermal parameters f o r the ruthenium atom gave a value the  of  four  0.48. sulphur  of  R  The p o s i t i o n s of the two c h l o r i n e atoms and atoms  were  revealed  from  a  difference  56  Fourier,  and  two  f u r t h e r i s o t r o p i c c y c l e s lowered R to  another d i f f e r e n c e map  then revealed  the  positions  0.20.  of  the  remaining non-hydrogen atoms, a f u r t h e r three c y c l e s using anomalous and  scattering correction  refining  parameters  the  for  positional  all  the  of  eleven  of  at  conventional  R  were  f a c t o r f o r the  12  extinction, 4,  080,  3 0 1, 181,  The  absorption,  4 2 1, 40  2,  anomalous C l , and  JFo|  < 12.8,  |Fo|  > 22.6  final  indicated  the  1 0 3,  the  allowing  (see Table 13).  for  The  final  2720 observed r e f l e c t i o n s given  zero  weight  instrument  2 0 0,  in  the  023,  malfunction:  4 0 0,  004,  02  those of r e f . 39 f o r the  scattering  corrections  S atoms. The J~i  3 2 0,  6  1  and  employed  - 0.0  p o s i t i o n a l and  in  the  (15)  < |Fo|  for  2  atoms, the  I £ ° 1/12.8  if  unobserved  /T  = 22.6/|FoJ i f  reflections  over ranges of  IFoj  f i n a l stages of refinement. The  thermal parameters are  14 r e s p e c t i v e l y .  hydrogen  Measured and  given i n T a b l e s 13  calculated structure  are a v a i l a b l e from U.B.C. L i b r a r y .  non-  were a p p l i e d f o r  > 12.8,  w (Fo-Fc)  0,  5).  weighting scheme: fit ~  = 1 i f 22.6  was  to suspected e r r o r s r e s u l t i n g or  3 4 1,  constant average values of was  thermal  s c a t t e r i n g f a c t o r s of r e f . 14 were used f o r the  hydrogen atoms and  Ru,  stage  calculated  interactions  s t a g e s o f refinement due  from  S atoms,  anisotropic  this  R = 0.041. (15 r e f l e c t i o n s were final  C l , and  the twenty-four hydrogens, and  remaining t h i r t e e n p o s i t i o n s minimum i n t r a m o l e c u l a r  and  Ru,  atoms, lowered R t o 0.047. a  d i f f e r e n c e F o u r i e r performed positions  f o r the  an  gave and final and  amplitudes  T a b l e 13 F i n a l p o s i t i o n a l parameters { f r a c t i o n a l x 10*) with estimated standard d e v i a t i o n s atom EU Cl{1) Cl(2) S(1) S (2) S{3) S (4) 0(1) 0 (2) 0(3) 0(4) C{11) C (12) C(21) C (22) C(31) C{32) C (41) C{42) H {11 1) H (112) * H(113) * H (121)* H(122) H (123)* H{211) H (212) H (213) * H (221) * H (222) H(223) H(311) H (312) * H(313)* H (321) * H (322) H{323)* H{41 1) H (412) H (413) * H (421) H{422) * H (423)*  X  2484.2(4) 5001 (1) 1570 (1) 2361 (2) 3332 (1) 63(1) 3528 (1) 1036 (6) 30 41 (6) 9657(5) 27 65 (4) 3980(8) 2596 (9) 5292(7) 2660 (7) 9396 (7) 8809 (6) 2524(8) 5262(8) 36 00 48 19 3739 20 55 2488 36 86 6027 5577 5432 1597 2950 3081 -47 -1516 -869 -754 -1170 -2150 2392 1447 2915 4397 5795 5867 •calculated  i n parentheses  I 1 217.5 (2) 701 (1) 9972 (1) 1051 (1) 2403 ( 1) 1591 (1) 766 (1) 1302 (3) 2800(2) 2378 (2) 1377(2) 1413 (4) 96 (4) 2486 (4) 2982(3) 1365 (4) 1047 (4) 843 (5) 1176 (4) 1851 1075 1460 -219 95 -39 2329 3058 2480 2888 3004 3456 1638 1654 832 959 490 1307 1321 1197 490 1421 829 1287 positions  z 2654.5 (3) 2652(1) 3040 (1) 690 (1) 2507(1) 2791 (1) 5290(1) 9984 (4) 1379(4) 2577 (4) 4515(3) 9964 (5) 349(6) 2867 (8) 3649(6) 4216 (6) 1886(6) 6619(6) 5778(7) 10 77 -887 896 -500 420 2347 3184 3753 3775 4 429 3520 4969 4370 4241 1111 2150 1770 7080 6664 721 1 6023 6304 5100  58  Table J J F i n a l thermal parameters and t h e i r estimated standard  deviations  (a) A n i s o t r o p i c thermal parameters Atom  0  fi21  fiS3  (U>- x 1Q  u  0 va  2  A) 2  fi2.Z  Hu 2. 08 ( 2) 2.59 ( 2) 3. 21 { 2) 0. 00 ( 1) 0 .09 ( 1) 0. 10 ( 1) Cl(1) 2. 33 ( 6) 4.3 8 ( 7) 5. 74 ( 8) 0. 62 ( 5) 0 .20 ( 5) 0. 09 ( 5) Cl(2) 3.72 ( 6) 2.96 ( 6) 5. 42 ( 7)-0. 58 ( 5)-0 .01 ( 5) 0. 39( 5) S(1) 3. 82 ( 7) 5.23 { 7) 3. 34 ( 6) 0. 03 ( 6)-0 .03 ( 5} 0. 16( 5) S{2) 4. 00 ( 7) 2.75 ( 6) 5. 49 { 7)-0. 28 { 5) 1.06 ( 5) 0.20 ( 5) S(3) 2. 39 ( 6) 3.84 { 7) 4. 92 ( 7) 0. 39 ( 5) 0 .28 ( 5) 0. 19 ( 5) S (4) 4. 00 ( 7) 3.51 ( 6) 3. 75 ( 6) 0. 19 ( 5)-0 .62 ( 5)-0.22 ( 5) 5. 62 (29) 12.78 (51) 4. 73 (24) 1. 51 (26) -1 .56 (21) 1.8 6 (26) 0(1) 0(2) 10. 47 (39) 4. 19 (24) 6. 45 (28) 0. 83 (25) 2 .49 (26) 1.74 (21) 4. 18 (21) 4.0 8 (22) 9. 27 (32) 1. 78 (18) 0 .15 (20) 0.7 5 (21) 0(3) 0(4) 4. 09 (20) 3.95 (19) 3. 39 (16) 0. 52 (15) -0 .27 (14) -0. 11 (14) C(11) 6. 89 (42) 5.7 8 (36) 4. 93 (32) 0. 76 (31) 2 .52 (29) 1.01 (28) C(12) 9. 73 (54) 6.32 (43) 5. 34 (3 5] -1. 56 (39) 1 .23 (34) -2.07 (32) C(21) 3. 82 (34) 5.88 (41) 13. 62 (7 0] -2. 27 (31) 1.04 (38) -2. 00 (43) C (22) 6. 14 (38) 3.79 (31) 7. 86 (4 1)-1 .15 (26) 1 .54 (31) -1. 85 (28) C (31) 4. 18 (33) 7.34 (43) 6. 08 (3 6] 0. 69 (29) 1.93 (27) 0.14 (31) C (32) 2. 44 (26) 7.20 (40) 7. 31 (4 0)-0. 2 0 (26) -0 .81 (24) -0.78 (32) C (41) 7. 67 (46) 8.00 (48) 4. 62 (3 3] 2. 60 (38) 0 .90 (31) 1.65 (32) C (42) 4. 35 (34) 6.2 2 (41) 7. 42 (4 2) 0. 14 (27) -2 .56 (30) -0.10 (30)  (b) I s o t r o p i c thermal  parameters (U x 100) o  Atom A l l Hydrogens  fi( ) A2  6.3  RESULTS AND DISCUSSION The  co-ordination  geometry about the ruthenium  e s s e n t i a l l y o c t a h e d r a l with c i s c h l o r i n e atoms. Of DMSO  ligands,  three  a r e sulphur-bonded  bonded, t h e O-bonded l i g a n d being t r a n s bonded  ligands  <S(1}).  The atom  g e n e r a l view of the molecule a r e  atom i s  the f o u r  and one i s oxygento  one  labelling  illustrated  of  t h e S--  scheme  and a  i n Figure  9.  I n d i v i d u a l bond l e n g t h s and angles, with standard d e v i a t i o n s , are given i n Tables 15 and 16 r e s p e c t i v e l y . Slight  distortion  the c e n t r a l ruthenium bonded  does  occur, the angles subtended a t  atom between the t h r e e mutually c i s  ligands  being  larger  than  94.9°, mean 94{1)°], while t h e values f o r t h e the  two  Cl-Ru-0  angles  8 8 - 7 ° , mean 88.2(5)°]. mean-planes  with  are s l i g h t l y  Equations  deviations  90°[92.6C l - R u - C l , and  l e s s than  of s e l e c t e d  S-  90°[87.8-  least-squares  o f the atoms from these  planes  are given i n Table 17. T h i s d i s t o r t i o n appears t o be governed p r i m a r i l y by s t e r i c f a c t o r s a s s o c i a t e d with the S-bonded DMSO groups. The  Ru-Cl bond  longer  than  would  T y p i c a l values of  l e n g t h s , 2.435(1) A, be expected mean  Ru-Cl  are s i g n i f i c a n t l y  f o r a p u r e l y ©"-donor l i g a n d . bond  lengths  i n octahedral ©  complexes  with  trans  chlorine  atoms  RuCl (N C H (CH ) ) ( P ( C H ) ) . (CH ) 0 5  i  v  v  1  R u C l (NO) (PMePha.)^ 3  f c  s  x  a  3  z  a r e 2. 390 (7) A i n  (34) and 2.398 (7) A i n  (40). T h i s l e n g t h e n i n g i s an i n d i c a t i o n o f  the s t r o n g t r a n s e f f e c t of a S-bonded DMSO l i g a n d (33).  A g e n e r a l view of t h e s t r u c t u r e c r y s t a l l o g r a p h i c numbering  showing the scheme.  61  Table 15 o  Bond l e n g t h s <A) with standard d e v i a t i o n s i n parentheses Bond  Length  (&)  Bond  Length  (&)  Ru  -Cl(1)  2.435(1)  S(1)-C(11)  1.779(8)  Ru  -Cl(2)  2.435(1)  S(1)-C(12)  1.808(6)  Eu  -S(1)  2. 252(1)  S (2)-C (21)  1. 795(7)  Eu  -S (2)  2. 277(1)  S(2)-C(21)  1.783(6)  Ru  -S(3)  2.276(1)  S (3)-C (31)  1.787 (6)  Ru  -0(4)  2. 142 (3)  S (3)-C (32)  1.794(6)  S{1)-0 (1)  1.483(5)  0(4)-S(4)  1.557(4)  S(2)-0(2)  1.485(5)  S(4)-C(41)  1.783(6)  S(3)-0{3)  1. 485 (5)  S (4) -C (42)  1.793(6)  62  T a b l e J6 Bond angles  (deg) with standard  Bonds  d e v i a t i o n s i n parentheses.  Angle  Bonds  Angle  C l (1) -Bu  - C l (2)  87.78 (5)  Bu  -S (2) -C(22)  112. 2(2)  C l (1) -Bu  -S(1)  88.22 (5)  Hu  -S(3) -C (31)  109. 6(2)  Cl(1) -Bu  -S(2)  92.90(5)  Bu  -S (3)-C (32)  112. 3(2)  C l (1) -Bu  -S (3)  173.49 (5)  Bu  -S(1) -0(1)  120.9(2)  Cl{1) -Bu  -0(4)  88.2(1)  Bu  -S{2) -0(2}  117. 7(2)  Cl(2) -Bu  -S(1)  92.69 (5)  Bu  -S (3)-0(3}  120. 1(2)  C l <2) -Bu  -S(2)  173.85 (5)  C (11) -S(1) -C{12)  98.6 (3)  Cl{2) -Bu  -S{3)  86.38(5)  C(21) -S (2)-C(22)  97.5 (3)  C l (2) -Bu  -0(4)  88.7 (1)  C{31) -S(2) -C {32}  100. 1 (3)  S (1) -Bu  -S{2)  9 3. 44 (5)  C(11) -S{ 1) -0(1)  106. 3(3)  S{1) -Bu  -S(3)  94.91 (5)  C{12) -S{1) -0(1)  106. 0(4)  S(1) t-Bu  -0 (4)  176.1 (1)  C(21) - S (2) -0(2)  107. 7(4)  S(2)  -Bu  -S<3)  92.61 (5)  C (22)-S (2)-0(2)  106. 9 (3)  S(2) -Bu  -0(4)  85.2 (1)  C{31) - S (3) -0 (3)  106.3 (3)  S(3) -Hu  -0 (4)  88. 8(1)  C (32)-S{3) -0(3)  106. 4(3)  Bu  -S(1) -C(11)  112.6(2)  BU  -0(4) -S (4)  Su  -S(1) -C(12)  110.0 (2)  0(4) -S(4) -C(41)  101 . 6(3)  Hu  -S (2) -C(21)  112.7 (2)  0(4) -S(4) -C (42)  104. 2(3)  C{41) - S (4) -C {42}  99.0 (4)  120. 0(2)  Table V7 S e l e c t e d Weighted Least-Squares f o r RuClj {flea,SO)H.  mean planes  Plane through Ru, C l (2) , S ( 1 ) , S (2) , and 0(4) 0.999X + 0.049Y - 0.013Z = 2.249 Atom Ru Cl(2) S<1) S(2) 0(4)  Distance (A) -0.042(1) -0. 100(1) -0. 079 (1) 0. 826 (1) 0. 139(4)  Plane through Ru, C l ( 1 ) , S ( 1 ) , S (3) , and 0(4) 0.335X + 0.933Y - 0. 129Z = 2.365 Atom Ru Cl(1) S(1) S (3) O (4)  Distance (A) 0.013 (1) -0. 102(1) 0.003 (1) -0. 104( 1) 0.075(4)  Plane through Ru, C l (1) , C l (2) , S (2) , and S(3) -0.043X * 0.024Y - 0.999Z = -3.0537 Atom Ru Cl(1) Cl(2) S(3) S (3)  Distance (A) 0. 0009 (3) -0. 166(1) -0.027(1) 0.186 (1) -0.042( 1)  In  the i n t e r a c t i o n  between  t h e Ru  s u l p h u r atom appears to be behaving  and S atoms, t h e  as a weak "^-acceptor, a s  a s h o r t e n i n g o f the bond between a metal atom and l i g a n d should be observed T-acceptor.  a tf"-donor  i f the «"-donor i s t r a n s t o a s t r o n g  For example i n £ Ru ( N 0 ) C 1 ] ~ the e q u a t o r i a l Ru-Cl 2  S  d i s t a n c e s average 2.376(2) A w h i l e the c h l o r i n e atom trans t o ©  the  nitrosyl  group  i s s i g n i f i c a n t l y s h o r t e r a t 2. 357 (1) A  <«••). However evidence s u p p o r t i n g some TT-acceptor be  obtained  from  the Ru-S  nature  can  d i s t a n c e s i n t h e S-bonded DMSO  l i g a n d s , which a r e t r a n s t o the two c h l o r i n e atoms. The mean ©  value of 2.277(1) A found the  presence  of  some  f o r the Ru-S bond l e n g t h s dtr-£TT back donation  from  indicates  the c e n t r a l  metal t o t h e s u l p h u r atom, assuming the s i n g l e bond  covalent e  radii  f o r ruthenium  respectively.,  and  (22). However,  considerably less [ Ru (NHj) (Me SO) ] 2 * (30), © s  2  2.188(3) A. sulphoxide available the  sulphur  The  increased  i s due t o tr-donor  co-ordination  are  this  than where  1-33 back  that t h e Ru-S  and  donation  is  found distance  in i s  back d o n a t i o n found  the lack  of  i n the mono-  competition  sphere.  A  comparison  of  similar  a  2  3  S  a  (30)j and  RuCl 2.(Me S0)4. can be found x  for  the  o r b i t a l s from other TT-acceptor l i g a n d s i n  l e n g t h s and a n g l e s f o r [ R U C I 3 (Me S0)3 ]-. (Chapter f Eu ( N H ) (Me SO) ] *„  1.04 A  free  bond  3, r e f . 29),  DMSO (35) with those o f  i n Table 18.  Examples o f the change i n c o - o r d i n a t i n g  atom  with t h e  v a r i a t i o n o f the number of DMSO l i g a n d s attached are somewhat limited.  In  four-co-ordinate  palladium  complexes  steric  65  influences  appear  to  [Pd(Ke^SO^d^]  be  has  of  as  c i s configuration.  importance  exclusively  [ Pd (MejSO) ^.32+ has both sulphur a  most  sulphur-bonding,  and oxygen-bonded l i g a n d s i n  t h e s i z e of t h e l i g a n d i n c r e a s e s  mixed t r a n s s t r u c t u r e s are produced, i . e . butyl  cationic  occur in  species,  while  only  i n the p r o p y l  structure,  (Chapter  while  3)  has an  the i n c l u s i o n  approaches the [ Pd (-He 2. SO) ^ ] 2 + influences  2 +  .  This  change  i s p a r a l l e l e d i n these o c t a h e d r a l  [ B u C l j (HeaSOJ-j j -  prohibit  of  all  systems.  S-bonded  another  situation,  the formation  and  oxygen-bonded l i g a n d s  i n the i s o - p e n t y l complex [Pd(Pe^SO)^ ]  co-ordination  (42) .  DMSO  such  cis  ligand  that  steric  o f an a l l sulphur-bonded  complex, but e l e c t r o n i c e f f e c t s keep the S-bonded l i g a n d s i n a  c i s configuration.  going  from  interactions  The decrease i n c e n t r a l metal s i z e i n  ruthenium  to  considerably,  iron  increases  the  i . e . , [ F e C l a (MezS0) ] a  +  steric  has a trans  c o n f i g u r a t i o n i n which a l l the DMSO l i g a n d s are oxygen-bonded (43) . The fiu-S bond l e n g t h f o r the S-bonded l i g a n d t r a n s t o the O-bonded sulphoxide  dimethylsulphoxide  o  i s 2.252 (1) .&.  This ©  s l i g h t yet s i g n i f i c a n t shortening due  (compared t o 2.277(1) A)  i s  t o t h e d i f f e r e n t atoms i n the t r a n s p o s i t i o n s . The Eu-0 o  distance i s  2.142(3) A  and  i s similar  to  the value  of  o  2.007 (6) A found f o r Fe-0 (43), c o n s i d e r i n g the d i f f e r e n c e o f o  covalent (22).  radii  of the two metals t o be approximately 0.12 A  66  Table J.8 Mean bond l e n g t h s and angles f o r (I) [ R u C l ( H e S O ) ]a  x  (II) R u C l ( M e S 0 ) a  x  i  %  (III) [Ru (NH ) (Me SO) j * 2  3  S  x  (IV) Free DMSO  A) Bond o Lengths (A)  (I)  (II)  (III)  (IV)  Ru-S  2.261 (8)  2. 277 (1)  2. 188 (3)  -  S-0  1.48(2)  1.485 (5)  1.527 (7)  1.471-1.531  S-C  1.79 (3)  1.790 (6)  1. 840(8)  1.80- 1.82 (1)  BU-C1  2.43 (1)  2.435 (1 )  Bu-S-0  118(1)  119(1)  114.9(3)  Ru-S-C  112 (2)  112(1)  116(1)  O-S-C  106(2)  106.8(6)  104.2 (8)  107  C-S-C  100 (2)  99(1)  99.4(6)  98  -  -  B) Bond Angles (deg)  -  67  F i g u r e 10 A s t e r e o s c o p i c diagram o f the u n i t c e l l  viewed  down b. There i s c o n s i d e r a b l e v a r i a t i o n distances  f o r the  dimethylsulphoxide  two  types  of  in  distance  is  sulphur-oxyqen  differently  co-ordinated  l i g a n d s . I n t h e sulphur-bonded  mean v a l u e i s 1.484(5) A, w h i l e i n t h e the  the  l i g a n d s the  oxygen-bonded  liqand  1.557(4) A . T h i s r e p r e s e n t s a c o n s i d e r a b l e  d e c r e a s e -in t h e m u l t i p l e bond c h a r a c t e r of t h e sulphur-oxygen l i n k e a g e caused this i s s t i l l  i y the d i f f e r e n c e s i n  co-ordination,  though  somewhat s h o r t o f t h e e s t i m a t e d S-0 s i n g l e bond o  l e n g t h o f 1.70 A ( 4 3 ) . The  molecular  geometry  of  the r - S-bonded  d i m e t h y l s u l p h o x i d e l i g a n d s i s very s i m i l a r t o t h a t free  dimethylsulphoxide  106.6(6)°),  C-S-C a n g l e s  (41). The 0-S-C a n g l e s (mean v a l u e  99(1)°),  found  in  (mean value  and  the  S-C  68  bona and  lengths  (mean  1.80-1.82(1) A  values  for  the  value  1.79(1) A) compare with  respectively.  O-bonded  ligand  107°, 98°  The  corresponding  are  also  103 (1)°, 99.0(4)° and 1.788 (5) A. The  other  mean  similar angles  being in  the  d i s t o r t e d t e t r a h e d r o n have mean values of 112(2)° f o r Ru-S-C, 120(2)°  f o r Ru-S-0 and 120.0(2)° f o r Bu-O-S. F i g u r e 10 shows  a s t e r e o s c o p i c view of the contents of the u n i t  cell  viewed  down b. The  this  compound  and  t r i c h l o r o t r i s (dimethylsulphoxide) complex  (Chapter  3)  consistent  crystal  with  structures  the  infrared  (29) f o r these compounds.  of  and *H n.m.r.  the were  s p e c t r a l data  5  CHAPTER 5  CRYSTAL AND  MOLECULAR  STRUCTURE OF  1 , 3,7—TRIMETHYL-2,6-DIOXY PURINE HYDROCHLORIDE (CAFFEINE HYDROCHLORIDE  DIHYDRATE)  DIHYDRATE  9  70  INTRODUCTION The  crystal  hydrochloride  dihydrate  the necessary this  structure  determination  was  The  caffeine  undertaken p r i m a r i l y to provide  i n f o r m a t i o n to complement  compound.  of  an  ENDOR  study  on  renewed i n t e r e s t i n t h i s area i s due  the d i s c o v e r y t h a t c a f f e i n e w i l l  inhibit  the  to  post-radiation  r e p a i r of chromosomal a b e r r a t i o n s i n i r r a d i a t e d  DNA  (44).  EXP ERI MENTAL The  white n e a r l y t r i g o n a l p r i s m a t i c c r y s t a l s were grown  by e v a p o r a t i o n from hydrochloric (ca 0.4  a  saturated  acid.  X 0.3  X 0.2  The  mm.)  was  solution  crystal  of  caffeine  chosen  for  in  study  mounted with b p a r a l l e l  to  the  gbniostat  a x i s . U n i t - c e l l and space group data were obtained  from f i l m  and  diffractometer  measurements.  The  unit-cell  parameters were r e f i n e d by a l e a s t - s q u a r e s treatment values  for  of  sin 8 2  22 r e f l e c t i o n s measured on a d i f f r a c t o m e t e r with  Cu K* r a d i a t i o n . Crystal  Data.  C H „ ClN^O,..2H 0,  a = 12.391(4),  b = 6. 524 (1),  $  M = 266.7,  1>  monoclinic,  c = 17.167(6) A, o  P = 118.82(3)°,  U=  z = 4,  g cm- , 3  from absent  1215.9(8) A 3 , D = m  F(000) = 560.  Space group P2,/c  r e f l e c t i o n s hOl, 1 * 2n and  r a d i a t i o n ) = 29.19  XRD  1.457  e  ( C ^ , No  k * 2n.  14)  /*(CuKo(  -1  Datex-automated  General  6 d i f f r a c t o m e t e r , with a s c i n t i l l a t i o n  counter,  Cu K ot ( n i c k e l f i l t e r scan  OkO,  D =  cm .  I n t e n s i t i e s were measured on a Electric  1.46,  a t 2° m i n  - 1  and  pulse height a n a l y s e r ) , and  over a range o f  (1.80  * 0.86  tan 8)  a  -6-29  degrees  71  i n 29, with 10 s background of  the scan.  140°  {minimum  i n t e r p l a n a r spacing 0.82 ft). A check r e f l e c t i o n was  monitored  every  40  Data  were  counts being measured at each end  reflections  measured  to  throughout  29  the  =  data c o l l e c t i o n .  g r e a t e s t d e v i a t i o n from the i n i t i a l v a l u e was +21.1% and f i n a l i n t e n s i t y was 0.85 polarization  The the  times the i n i t i a l v a l u e . L o r e n t z and  corrections  were  applied,  and  the s t r u c t u r e  amplitudes were d e r i v e d . No a b s o r p t i o n c o r r e c t i o n was  applied  due t o the low value of /* and the f a i r l y uniform shape of the c r y s t a l . Of the 2208 independent had  intensities  <f {I)  less  than  = S + B * (0.05S)  z  averaged  background  2  reflections  3 o-(I)  above  with S = scan  measured,  background  count  and  451 where  B =  time  count. These r e f l e c t i o n s were c l a s s i f i e d  as unobserved and given zero weight i n the refinement. STSDCTURE ANALYSIS Although the P a t t e r s o n compounds for  with  one or a few  synthesis 'heavy  is  numbers,  because  Patterson F o u r i e r map.  no  vectors  same  for  or  similar  w i l l stand out on the  Fortunately alternate  have been developed which r e l y on  useful  atoms', i t i s u n s u i t a b l e  molecules i n which many atoms have the  atomic  very  ' d i r e c t methods'  probability  relationships  between the phases of the ' s t r o n g e r ' r e f l e c t i o n s . In  direct  methods,  which are e s s e n t i a l l y rather  than  normalized  geometrical  factors  structure  Hj H  are used  factors  only,  c o n t a i n i n g , as does | F | , the e f f e c t s of atomic B  s c a t t e r i n g f a c t o r s and atomic thermal c a l c u l a t e d as f o l l o w s  motion.  They  can  be  where  S  is  an  integer  symmetry f a c t o r which depends  upon the space group e x t i n c t i o n s , developed  probability  flauptman  and  Karle  (45)  r e l a t i o n s h i p s , based on Sayre's work,  which c o u l d be used to determine the phases  of  reflections.  B a s i c a l l y , as seen i n the e g u a t i o n  one e s t i m a t e of t h e phase of H can be obtained from the phase  addition  of  two r e f l e c t i o n s whose i n d i c e s when added  together g i v e the i n d i c e s of H. The weight  to  be  given  to  t h i s i n d i c a t i o n i s equal t o the product of the two normalised structure phase  $  M  factors  and | E  K  H  |; the b e s t e s t i m a t e of the  w i l l be the weighted sum  Obviously  of  a l l the  r e l a t i o n s h i p s between l a r g e  dominate the produce  |E 1  a  summations phase  due  value  to  J E J and  their  somewhere  near  K  weight  indications. |E  M M  J*s  and  will  should  t h a t f o r the whole  summation. For  a centrosymmetric  space  group  (e.g.  P2,/c,  this  compound) the phases can only be 0 or i t , c o r r e s p o n d i n g t o the s i g n of + o r -. Sayres equations then become  where  S  means  * the sign  o f , ^ means 'probably equal  t o * , and the r e l a t i o n s h i p i s known as a £ - 2  (referred to  a  relationship for  Sigma  Two)  r e l a t i o n s h i p . That i s the £-2  the r e f l e c t i o n 4,2,1 of  reflections  0,1,1; 8,6,4  i s made up of t h e sum  whose  indices  and -4,-4,-3; 1,1,1  of a l l the  add t o 4,2,1  as  pairs  e.g. 4,1,0, and  and 3,1,0; e t c .  73  The  p r o b a b i l i t y , P, o f t h e  given f o r each  of  ^/°\ 'x  ideas.  program  ^ ^ l ^ i l ^ I J  developed  the structure  The  program  IJM's  prepared  parity of  rules  indices  could  each then turn  o f any p a i r ,  selected  more  signs,  and  c a s e newly of  many  (2 )  ^-2  sets  which i n t u r n  are  t o the  a l l three  was s p e c i f i e d .  A c o n s i s t e n c y index  of  used  s i g n s were n o t u s e d  there are  signs.  were  When  set, additional to  H  <IS I- S l I J I I H - « 1 >  to  t h e next  no  0 i s defined as  <II -«M,c-l«-*l> M  list),  determine  those already p r e d i c t e d . I n  reflections until until  the  + and - s i g n s i n  t o any s t a r t i n g  changes t o the l i s t .  0 =  of  relationships,  on b o t h  starting  4  determined  process i s r e i t e r a t e d  Three  and by a s s i g n i n g  the o r i g i n  a l l o w e d t o take  to redetermine  additional  relationships  { f o r P 2 , / c t h e suras  even,even,even)  i s applied  are determined,  signs  group  to  these  ( s e e T a b l e 19 f o r t h e c o m p l e t e  producing sixteen eguation  used  i n d i c e s conforming  t h e space  |EJ and  and  was  and t h e sum o f i n d i c e s o f  reflections  signs  this  J E | > 1.50.  with  the parity  having a large  (46)  o f C""2  list  s i g n s t o these r e f l e c t i o n s  more  Sayre's  a  with  chosen  d e r i v e d from  not produce  positive Four  were  by L o n g  o f c a f f e i n e h y d r o c h l o r i d e using  between t h e 297 r e f l e c t i o n s largest  i s  cell.  A computer determine  correct  i s a c o n s t a n t d e p e n d e n t on t h e c o n t e n t s  3  the unit  being  r e f l e c t i o n by  P = 0.5 + 0 . 5 t a n h l where  S  sign  new  determine  cycle.  additions  This or  74  T a b l e _19  Basic s t a r t i n g  set o f r e f l e c t i o n s f o r  C1C N .0 .H €  H  2  U  .2H^0  h  k  1  |EI  1)  -3  1  1  2.70 ^  2)  -7  2  2  3.33  3)  -4  1  2  2.42 J  4)  2  5  3  3.08  5)  -2  5  11  3,17  6)  -7  2  4  2.29  7)  -9  3  1  2.82  > origin  determining  75  where The  < true  consistency converge  solution  to  a  are  i n that  consistency  index  signs. of  E  given  0.92  of  An E map from  this  cycles  Two  hydrogen  atoms.  scattering  this  stage  correction  temperature  factors  6  and  to  with using  the  the  for  12,  -7  C  were  correction  of t h e 1 7 nonpeaks  refinement  anisotropic  temperature  A  difference  the  positions with  Fourier of the 1 5  an  anomalous  atom,  anisotropic  atoms,  isotropic  h y d r o g e n atoms and an o v e r a l l  correction  produced  errors, -1  instrumental  I  >  3  cr  (I)  convergence (5  stages of refinement 0 2,  1 2  16,  from  from  ref.  h y d r o g e n atoms f r c m  15,  ref. and  r e f . 3 9 . The  14,  anomalous  scattering weighting  at  reflections  - 1 4  due  2,  5 4 ) . The a t o m i c s c a t t e r i n g f a c t o r s f o r C l , O, taken  on  temperature  chlorine  r e f l e c t i o n s with  1752  high  assigned  highest  non-hydrogen  the  is  isotropic  0.088.  given z e r o weight i n t h e f i n a l  to s u s p e c t e d 3  the 1 7  15  set  the 2 9 7  using  refinement  for  coefficient for  0.064  equally  p o s i t i v e and 1 4 1  The p o s i t i o n s  revealed  Further  temperature f a c t o r s f o r  were  cycle  lowered the B f a c t o r at  B =  and  with a very  156  had  from  0.129  of  while a further  extinction  highest  cycles  of f u l l - m a t r i x least-squares  p r o d u c e d an B f a c t o r  computed  and  set.  and  i n 5 cycles  was computed  the  factors  of  20,  Table  i t converged  were i n d i c a t e d  factors,  number  the  which a r e a p p r o x i m a t e l y  in  h y d r o g e n atoms map.  have  between p o s i t i v e and n e g a t i v e . The r e s u l t s o f t h e  outstanding  values  usually  the l e a s t  set of signs  starting sets  negative  will  index, reguire  distributed 16  > means t h e a v e r a g e v a l u e o v e r a l l H.  N,  scattering  f a c t o r s f o r the  T a b l e 20  Comparison o f t h e 16 s o l u t i o n s from Long's s i g n  determination  program.  Set Signs o f 7 reflections 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16  +++++++ -*+ + •+ + +++•+-* —  +++*-++ «•+++—++ — • ++*-+*+ + +—#•-* +++-*— + + +-— + • + + +—++++ + + + +-  Number o f cycles 7 10 10 7 6 7 9 8 10 8 9 7 12 7 5 12  Number o f pluses  Number of minuses  267 142 182 147 143 140 156 142 150 148 139 140 149 150 156 144  30 155 115 150 154 157 141 155 147 149 158 157 148 147 141 153  Consiste index 0. 850 0. 608 0. 685 0. 684 0.717 0. 534 0. 598 0. 522 0.658 0. 523 0. 713 0. 510 0.752 0. 641 0. 917 0. 532  77  scheme w = 1/o- (F)  where o- (F)  2  defined a  2  (I) , gave c o n s t a n t average v a l u e s of w(Fo-Fc)  over  2  ranges of |Fo| and refinement. appear  i s d e r i v e d from the p r e v i o u s l y  2  The  in  was final  Tables  calculated  employed positional  21  and  structure  in  22  the  and  final thermal  respectively.  factors  stages  of  parameters  Measured  and  are a v a i l a b l e from the U.B.C.  Library. THERMAL MOTION AND  CORRECTION OF MOLECULAR GEOMETRY  Tbe e l l i p s o i d s of thermal motion atoms are  (excluding  the  shown i n F i g . 11.  for  c h l o r i d e i o n and  the  the water molecules)  The thermal motion has been analysed i n  terms of the r i g i d - b o d y modes of t r a n s l a t i o n (L) ,  and  screw  (S)  MGTLS. The r.m.s.,  non-hydrogen  motion  standard  (T) ,  libration  (47) u s i n g the computer deviation  in  the  program  temperature  o  D- j  factors  is  t  0.0017  A  i n d i c a t i n g t h a t the whole molecule  2  o  (r.m.s. the  AUj^=0.0022  thermal  remarkably  A ) 2  motion well  i s a reasonable rigid-body  of  bond  described  distances  by  23  the  (r.m.s. A U ^ =  rigid-body 0.0015  ( 4 8 and 4 9 ) using shape  of  atoms  for  corrections to the  a l l the based  on the &U::  involved.  ring  system.  not  by no more than  reported.  ) .  parameters  2  ( 5 0 and 5 1 ) have been  applied  atoms  attached  The c o r r e c t e d and uncorrected  0.05°,  q  motion  l e n g t h s appear i n T a b l e 2 4 . Bond angles, given i n changed  2  Independent  the bond l e n g t h s f o r the non-hydrogen fused  A  thermal  i n the fused r i n g system have been  corrected f o r l i b r a t i o n 0.08  that  t h e 9-membered fused r i n g system i s  parameters given i n T a b l e The  and  Table  to bond 25,  thus the c o r r e c t e d a n g l e s a r e  Table Final  positional with  parameters  6620([ 5748 [ 9 1 0 1 |[ 8592 [ 6 2 4 1 |[ 7359 [ 7 0 6 3 <t  (3) (7) (9)  (2) C(ft) C(5) C(6) C(8) C (10) C{12) C (14)  H(1  H H  1) * (12) • (21) *  H{22)  «  H(D H (2) H (3) H (4) a  (5) (6)  H H{7) H (8) H (9) H(10) H{11)  * indicates  7905 ( 6733 [ 7381 [ 6 8 5 H [ 6228 ( 7 6 9 3 |( 5591 ( 8067<( 6647 ( 937 (  9 27 ( 888 905 792 8 32 543 479 610 806 779 885  i n parentheses  35370{  2)  1275  {  2)  2) 3) 3)  699 2 ( 7633 { 5884 ( 4670 ( 1630{ 4033 {  4}  4)  2885 { 4695 ( 1420( 2095 { 2740 ( 4459 (  2) 2) 2) 2) 2) 2)  1232 ( 2827 (  5) 5)  4306 ( 19 94 {  2) 2)  2219(  5)  3503 { 3586 (  2) 2)  3) 3) 3) 3) 3)  ft) 5)  ft)  ft) 5)  6 96 ( 584 (  ft) 5)  700 (  ft)  2  4)  2) 2) 2) 3)  ft) 7} 2)  s  48847(15)  8)  ( ( { ( ( ( ( ( ( (  water  deviations  10 ,  2332 (  98388 (  0(11) 0(13) 0(1) ' 0(2) » N(1)  x 10*, C l x  I  X  Cl  N N N C  (fractional 103)  estimated standard  Atom  21  ft) ft) 6)  5) 5) 6)  5)  molecule  5) 6) 4)  4)  3971 { 5) 5 3 7 6 { 5) 2 367 ( 5) 5916{ 8) - 1 5 0 ( 7) 5 6 5 3 ( 6) 7 2 1 ( 7) 692 ( 9 ) 5 4 0 ( 8) 724 (13) 2 0 5 ( 4) 4 ( 7) 7 2 7 ( 8)  6)  2865 (  2)  4872 { 1279{ 2705 { 4848(  2}  3) 3) 3)  522 ( 432{ 19 8 {  3) 4)  149(  4) 2) 3) 3)  -16 ( 8) 548 ( 7)  547 ( 44 2 { 149( 87 ( 96 { 218 ( 282 ( 329 ( 545 (  584 ( 704 (  449 ( 473 (  520 (10) 6 0 9 ( 9) -18( 9) - 1 3 7 ( 12)  8) 8)  3)  4) 4) 4) 5)  4) 3) 3) 3)  H  Table 22 F i n a l thermal parameters and t h e i r estimated standard (a) A n i s o t r o p i c thermal parameters A) 2  Atom  2„  Cl 0(11) 0(13) 0(1) • 0(2) • N(1) N(3) N(7) N(9) C{2) C(4) C(5) C{6) C (8) C(10) C(12) C(14)  606 ( 6) 73 ( 2) 62( 2) 75 ( 2) 72 ( 2) 37 ( D 39 ( 1 ) 37 ( 1) "0 ( 1) 38( 2) 31 ( 1) 34 ( 2) 34 ( 2) 38 ( 2) 64 ( 3) 68 ( 3) 59 ( 2)  D  2»v  468 ( 6) 53 ( 2) 44 ( 2) 43 ( 2) 63 ( 2) 40 ( 2) 33 ( 1) 30 ( D 33 ( 2} 43 ( 2) 31 ( 2) 27 ( 2) 38 ( 2) 38 ( 2) 62 ( 3) 41 ( 2) 42 ( 2}  deviations  (tJ ^ ~-  H(11) » H(12)* H(21) * H (22) « H (1) H(2) H(3) H(4)  fi(A ) 2  59 (12) 97 (18) 74 (14) 152(26) 17 ( 7) 60 (13) 79 (14) 122 (23)  3  U  2.1.  72 ( 4) 479 ( 5) 43 ( D -1( 1) 56 ( 2) 25( 1) 56 ( 2) 22 ( 1} 50 ( 2) -13( 2) 36 { 1) 2( 1) 43 ( 2) M D 38 ( 1) 1( 1) 41 ( 2) 3{ 1) 39 { 2) -7( 1) 39 ( 2) -2{ 1) 37 { 2) 0{ 1) 42 ( 2) 2( D 32 ( 2) -1( 1) 42 ( 2) 16( 2) 65 ( 3) 18 ( 2) 45 ( 2) 6 ( 2)  (b) I s o t r o p i c thermal parameters Atom  x 1 0 , x 10* f o r C l  Atom H (5) H(6) H(7) H (8) H{9) H (10) H(11)  2x*  27'I ( 4) 35 ( D 32 I 1) 37 ( 2) 20 ( 2) 19 ( 1.) 24 ( 1) 21 ( 1) 20 ( 1) 22 ( 1) 18 ( D 20 ( D 21 ( 1) 14 ( 1) 24 ( 2) 40 ( 2) 32 ( 2)  (0 x 10 ) 3  2(* ) 2  103 (17) 99(19) 133(27) 89 (16) 69(13) 79(15) 79(14)  22 ( -5( 1 11( 1 10 ( 1 2( 1 5{ 1 -5( 1 -1( 1 3{ 1 -4( 1 - 1( 1 2( 1 5( 1 2( 1 12 ( 2 -2( 2 -3( 2  80  81  T a b l e 23 Rigid-body thermal parameters f o r the 9-membered f u s e d r i n g system  L(x  10 deg ) 2  P r i n c i p a l axes o f L • • !  r.m.s. amplitude 3.6° 2,6 2-0  J-8-1  J  i J i ; '  • '  ] . ; !  ;  .  o  ; r.m.s. A Uii (A*)  22{ 9) 58(12)  -37 d 3 h ; -6 (11) | 96 (35)Ji  i  [ P r i n c i p a l axes o f T r.m.s. amplitude 0.19(A) o.i7 0.17  (11)  ,  •  Direction 643 389 659  cosines 247 709 660  ( X 1 0 3)  Direction 18 355 935  cosines -82 931 355  (X1Q3)  -725 58 8 36 0  996 -83 12  0.0015  *Axes of r e f e r e n c e a r e o r t h o g o n a l Angstrom axes. E.s.d.*s of components o f L are g i v e n i n parentheses i n u n i t s of the l a s t p l a c e s shown.  T a b l e 24  Bond Lengths  Bond  (A) with standard  d e v i a t i o n s i n parentheses  uncorr,  corr.  Bond  uncorr.  N{1) -C{2)  1. 396 (4)  1.400  C{8)- H{1)  0.95(3)  C (2)-N (3)  1. 376 (4)  1 .379  N(9) -H (2)  0. 9 2 (5)  N (3)-C(4)  1. 351 (4)  1.354  C(10) -H(3)  1.01 (5)  C (4)-C<5)  1. 360 (4)  1.363  C{10) -H(4)  1.02(7)  C(5) -C{6)  1. 431 (5)  1.434  C{10) -H{5)  1.02 (6)  C (6) -N{1)  1. 4 07 (4)  1.410  C{12) -H{6)  0.89 (6)  C (4) -N (9)  1. 369 (4)  1.372  C{12) -H(7)  0.92(8)  N (9)-C{8)  1. 343(4)  1.346  C{12) -H{8)  1.00 (6)  C (8)-M(7)  1. 327 (4)  1.330  C(14) -H(9)  0.92 (5)  N (7]-C(5)  1. 392 (4)  1 .394  C(14) -H (10)  0. 89 (5)  M  (D -G{10)  1. 477 (5)  1.477  C(14) -H(11)  1.07 (5)  B  (3) -C(12)  1. 474 (5)  1.476  0(1). •-H(11) •  0.84 (4)  -C(14)  1. 469 (5)  1.471  0(1) * -H (12) '  0.89 (6)  C (2)-0(11)  1. 217 (4)  1.218  0(2) * -H(21) «  0.90 (5)  C (6' -0(13)  1. 218 (4)  1.220  0(2) * -H (22) »  1.03 (8)  83  Table 25 Bond angles  (deg.) with standard d e v i a t i o n s i n parentheses  a) Angles f o r the non-hydrogen atoms and H(1) and H(2) Bond N (1)-C (2) -N(3) c (2; -N (3) -C(4) N 13)-C (4] -C(5) C(4) -C (5) -C(6) C(5) -C (6] -N(1) C(6) — N (1]-C(2) c(u; -c (5; -N(7) C (5) -N (7] -C(8) N (7)-C(8) -N(9) C{8] - H (9) -C(4) N (9j -C(4] -C(5) N {1) -C{2] -0(11} N (3)-C (2) -0 (11)  Angle 117. 2(3) 118. 6(3} 123. 8(3) 122. 3(3) 111. 0(3) 127. 0(3) 106. 8(3) 107. 9(3) 109. 6(3) 107. 8(3) 107. 9(3} 120. 7(3) 122. 0(3)  Bond C (2) - N (3)-C(12) C (4) -N (3) -C(12) N (3)-C (4) -N(9) N (7)-C (5)-C(6) C(5) -C(6) -0(13) N{1) -C (6) -0(13) C{6) -N (1)-C(10) C (2) -N(1) -C(10) C(5) -N (7) -C(14) C (8)-N (7) -C(14) N (7)-C (8) -H{1) N (9)-C (8)-H(1) C (8) -N (9) -H (2) C (4) -N (9) -H (2)  Angle 119. 2(3) 121. 9(3) 128.4(3) 131.0(3) 126.7(3) 122. 4(3) 117. 6(3) 115. 3 (3) 125. 8(3) 126. 3(3) 123 (2) 127 (2) 128 (2) 124 (2)  b) Angles i n v o l v i n g hydrogen atoms not attached d i r e c t l y t o the fused r i n g system Bond N(1)-C(10)-H (3) N ( 1) —C (1 0) — H (4) N(1)-C(10)-H(5) H (3)-C (10)-H (4) H(3)-C(10)-H(5) H(4)-C(10)-H(5) N (3) -C (12) —H (6) N(3)-C(12)-H(7) N(3)-C(12)-H(8) H(6) -C(12)-fl(7)  Angle 105(3) 108(4) 112(3) 111(4) 111(4) 109(5) 110(4) 113(5) 106(3) 111(6)  Bond  Angle  H(6)-C(12)-H(8) 122(5) H (7) -C (12) —H (8) 94(5) N (7)-C (14)-H (9) 112(3) N (7) -C (1 4) -H (10) 108(3) N(7)-C (14)-H (11) 105(2} H(9) -C (14) -H (10) 121(4) H (9)-C (14)-H (11) 109(4) H (10)-C (14)-H (1 1) 100(4} H (11) • -0 ( 1) « - H (12) • 119(4) H(21) »-0 (2)'-H(22) » 105(5)  RESULTS AND  DISCUSSION  1,3,7-Trimethyl-2,6-dioxypurine h y d r o c h l o r i d e (caffeine  hydrochloride  dihydrate)  molecule  protonated  at  hydrogen  bonded  only  s t r o n g N-H.,,0 however,  to  hydrogen  N{9). one bond.  The  contains  caffeine  dihydra t e a  caffeine  molecule  is  of the water molecules, by a Both  water  molecules  are,  hydrogen bonded to the c h l o r i d e i o n (0-H...C1).  atom numbering chloride  scheme can be seen i n F i g . 11, except f o r  The the  i o n C l and the water molecules, H (11) »-0 (1) *-H (12) '  and H (21) *-0 (2) »-H (22) *. The e f f e c t o f p r o t o n a t i o n on the atoms  in  the  fused  ring  system  bond  lengths  i s somewhat d i f f i c u l t  determine. The i n i t i a l s t r u c t u r e d e t e r m i n a t i o n f o r (52) has f a i r l y the  to  caffeine  i n a c c u r a t e bond lengths, and m o d i f i c a t i o n s t o  s t r u c t u r e may  Shefter  between  (53).  have r e s u l t e d i n the N (9) adduct s t u d i e d by  Even so i t can be s a i d t h a t , i n terms of bond  d i s t a n c e s , a d i r e c t comparison i n d i c a t e s  little  significant  d i f f e r e n c e between the protonated and non-protonated s p e c i e s . T h i s might have been expected as Taylor and  Shigematsu  (55)  found  parallel  (54) and Kistenmacher results  for  adenine  compounds. Fig. An a f f e c t  12 does however i l l u s t r a t e one i n t e r e s t i n g anomaly. of p r o t o n a t i o n on compound  (I) ,  isocaffeine  (56) ,  would be expected to be a l e n g t h e n i n g of the C-N  double bond.  This  is  hydrobromide  (59),  but t h i s bond i s  bonds.  indeed  found  in still  (II),  methylguanine  shorter  than  the  other  P r o t o n a t i o n i n the c a f f e i n e system, i . e . from  c a f f e i n e : 5 - c h l o r o s a l i c y l i c a c i d adduct  (53), a l s o  C-N  (III),  results i n  85  H  / Ztf  V1.299 (A)  C ||  CL  C — H /1.376 8  ^  C  ^1.34 C — H \  K  \  CH  3  9  3  (II)  CH,  /. II  -  CH  3  CH,  C-""  1  \  (I,  .  /  /  x  \1.343  ^  \  c  ^ \ l . 3 2 7  II  .C  \  H  .C  H  V  H  (III)  'IV) Figure  12  Bond l e n g t h s and r e p r e s e n t a t i o n of the i m i d a z o l e r i n g f o r (I) I s o c a f f e i n e , (II) Methylguanine hydrobromide, (III) C a f f e i n e : S - c h l o r o s a l i c y l i c a c i d a d d u c t , • and (IV) C a f f e i n e h y d r o c h l o r i d e d i h y d r a t e  86  (a, l e n g t h e n i n g of the C-N (IV),  this  study,  double bond, but now,  a  at  N (9) ]  caffeine-like  h y d r o c h l o r i d e monohydrate of 1.325  A and  indicate that inadequate  in  shown  in  s h o r t e n i n g o f the N(7)-C(8) bond a l s o  occurs. , A s i m i l a r r e s u l t can be found [also  as  in  another  derivative,  protonated  7-methylxanthine  (58) which has a N(7)-C{8) d i s t a n c e  a C(8)-N(9) d i s t a n c e of 1.338  A. Such f i n d i n g s  the  in  simple  pictures  drawn  r e p r e s e n t i n g the protonated  F i g . 12  are  s p e c i e s , and  that  c o n s i d e r a b l e e l e c t r o n i c rearrangement must be o c c u r r i n g c l o s e t o the protonated transfer  to  similarity  c e n t r e . T h i s rearrangement does not seem to  the  rest  between  i n the protonated  of  the  molecule  the remaining  judging  corresponding  by  the  bond l e n g t h s  and non-protonated s p e c i e s .  For the angles, s i g n i f i c a n t changes do occur but only i n the i m i d a z o l e r i n g , a s i t u a t i o n p a r a l l e l  to  that  found  by  Kistenmacher  26  illustrates  the  endocyclic  bond  7-methyladenine  Compounds  (58) .  and  for  several  (58)  (60) ,  and  (IV)  this  as  is  at N(9) . The changes i n angles  found  to  at  N(1)  and  [  (V) J. Compounds (IV) and be expected  l i t t l e e f f e c t on the i m i d a z o l e substituents  study. (VI) ,  N (9)-C (4)-C (5) i n (IV) and similar,  7-  (IV) ,  on p r o t o n a t i o n are q u i t e l a r g e , being up to 7.6°  very  (59) ,  (VII)  (V) are unprotonated, while  (VII) are protonated  purine  (53) , (V) theobromine  dihydrochloride  hydrochloride  (III)  Table  angles  ( I l l ) caf eine adduct  methylxanthine  and  Sorrell  imidazole  derivatives. (VI)  and  ring  N(3)  comparing (VII) are  s i n c e t h e r e should  due  to  the  be  different  [hydrogen atoms f o r (VII) ,  methyl groups f o r (IV)] i n the p y r i m i d i n e  ring.  87  Table  A  comparison of  26  imidazole  the endocyclic several  purine  bond a n g l e s f o r  derivatives Angles  Atoms  (VI)  (VII)  (IV)  106. 1  105.9  106.6  106.8  105.4  105.0  107.3  107.5  107.9  N(7)-C(8)-N(9)  113.6  114. 2  110.7  110.3  109.6  C(8) -N (?) -C{4)  103.4  103.2  108.1  107.5  107.8  N(9) - C ( 4 ) - C ( 5 )  111.6  1 15.5  108. 1  108.2  107.9  (IJI)  (V)  C(4)-C{5)-N(7)  106.0  C(5)-N(7)-C(8)  (III)  Caffeine:5-chlorosalicylic  (V)  Theobromine  (VI)  7-Hethyladenine  (VII)  7-Methylxanthine  (IV)  Caffeine hydrochloride  acid  adduct  dihydrochloride hydrochloride dihydrate  , t h i s study.  88  The  mean  planes  calculated  i n d i c a t e t h a t the protonated a  planar. in  plane  the caffeine  caffeine  caffeine  calculated  molecule,  for  hydrochloride  molecule  i s essentially  u s i n g a l l t h e non-hydrogen  and  H{1)  and  atoms  H(2), indicates  a  ©  maximum ring  deviation  of only  0.19 a £ f o r C(12) ]. F o r the f u s e d  atoms o n l y , a c o m p a r i s o n  their  standard  puckered,  found  with  d e v i a t i o n s shows t h e six-membered r i n g  t o be  and t h e f i v e - m e m b e r e d  experimental  error.  distances'from Caffeine derivatives (Table  of the  Table  ring  27  hydrochloride, l i k e  27),i s also  along  the  The  crystal  about  chloride  the r i n g  contains  I . 76(5} very H...0 and  the  between  nature  hydrogen  angle angle  ring  for  caffeine  types  o f h y d r o g e n b o n d s . 0-  between t h e water  molecules  i sdistorted,  atom  0(1)'.  176(4)°, and i s p r o b a b l y  of this  angles.  oxygen  proton. The  exists  between t h e c a f f e i n e  F o r water being  supported  1, s t r o n g l y h y d r o g e n  119(5)°, whereas  i s c l o s e t o normal, being  The  H...0,  due t o t h e  proposition  i sfurther  and  between  H(2) a n d 0 ( 1 ) ' i s v e r y s t r o n g  bonding  type  h y d r o c h l o r i d e monohydrate  H(2) a n d t h e water  a , N-H.,,0 a n g l e ,  H-O-H  purine  t h e C ( 4 ) - C { 5 ) bond, t h e a n g l e  two  one o f t h e water m o l e c u l e s  water the  bond  acidic  p l a n e s and  i o n , and N-H...0 h y d r o g e n bonds o c c u r  hydrogen  hydrogen  mean  within  0.85°.  H. ..C1 h y d r o g e n b o n d s o c c u r the  planar  s e v e r a l other  between t h e i m i d a z o l e and t h e p y r i m i d i n e hydrochloride being  be  planes.  hypoxanthine  bent  to  gives  t h e atoms t o t h e s e  (61) e . g .  deviations  that  molecule by t h e bonded,  f o r water  105(5)°. T a b l e  N-  2  28 g i v e s  t h e d i s t a n c e s and a n g l e s f o r t h e p o s t u l a t e d i n t e r m o l e c u l a r  89  fable  Equations with 1)  of s e l e c t e d weighted deviations  C a l c u l a t e d using 0.833X  + 0.487Y  27  l e a s t - s q u a r e s mean  (A) o f t h e atoms f r o m  the  planes  N ( 1 ) ,8 (3) ,C (2) ,C ( 4 ) ,C (5) , a n d C (6) * 0.264Z = 7.296.*  Hypoxanthine hydrochloride  other  planes  Caffeine  monohydrate  hydrochloride  dihydrate  N(1)  0.0013  -0. 0148(32)  N(3)  -0.0006  -0.0145(32)  C(2)  -0.001 1  0.0334(38)  C{4)  0.0020  -0.0020 (35)  C(5)  -0.0017  0.0123 (36)  C(6)  0.0001  -0.0015 (38)  N(7)  -0.0183  0. 0288 (31)  C{8)  -0.0297  0.0279 (38)  8(9)  -0.0111  0.0051 (33)  atoms  2) C a l c u l a t e d u s i n g N (7) ,N (9) ,C(4) ,C (5) ,C (8) . 0.825X  + 0.493Y  • 0.275Z =  N(7)  -0.0010(30)  N(9)  -0.0013(33)  C(4)  0.0006(35)  C(5)  0.0004(36)  C(8)  0.0020(37)  A n g l e between p l a n e s o e q u a l t o 0.85  7.318  1) a n d 2) f o r t h e c a f f e i n e m o l e c u l e i s  * X,Y, and 2 a r e o r t h o g o n a l  coordinates  o i n A w.r.t.  a,b,c*.  90  Table 28  Distances and angles i n the i n t e r a t o m i c c o n t a c t s o f the type D-H...A o  ©  ©  0,.84 (8)  2 .32 (5)  3. 12(1)  162 (4)  0(1} • B{12) C l  0. 89 (6)  2 .23(6}  3. 12(1}  172 (5)  0(2) ». H(21) C l  0. 90(5)  2 .37(5)  3. 24(1)  167(4)  0 ( 2 ) ' H (22) C l  1. 0 3(9)  2 .22 (8)  3. 24(1)  169 (6)  0. 92(5}  1 .76(5)  2. 684(4)  176 (4)  A  D-H (A)  0(1) • H(11) C l  H  D  N(9)  H{2)  0(1) «  * i n d i c a t e s water  H. ..A (A) D. ..A (A) D-H...A (*)  molecules  91  Fiqure  13  A s t e r e o s c o p i c diaqram o f t h e u n i t - c e l l viewed down b, showinq the p o s t u l a t e d hydroqen bondinq as dashed l i n e s . bonding f o r t h i s compound. A s t e r e o v i e w molecules  in  the  intermolecular In  these-.crystals,  of  of hetero the  and  . the  postulated  unlike  many  other  purine  appears t o be no s i g n i f i c a n t  m o l e c u l e s and hence no s i g n i f i c a n t  type  stacking dipole  of  overlap  C - 0 and C-N bonds c o n t r i b u t i n g t o t h e s t a b i l i t y  of  crystalThe  it  lattice,  of the  hydrogen bonding can be seen i n F i g . 13.  d e r i v a t i v e s , there layers  crystal  of the packing  allowed  crystal  was u s e f u l because  f o r a c o r r e l a t i o n between the proton  hyperfine  couplinq  spectroscopy structure  s t r u c t u r e determination  tensors,  determined  from  on t h e X - i r r a d i a t e d c r y s t a l , and  (62) .  and  the  nitroqen the  ENDOR  molecular  92  CHAPTER 6  CRYSTAL AND MOLECULAR  STRUCTURE OF  1-ACETYL-3-BENZAflIDG-2-KET0-4-(2,3,4,6-TETRA-O-ACETYL£-D-GLUC0PYRAN0SYL0XY)-a -PYRR0LINE 3  INTRODUCTION From  r e a c t i o n s o f g l y c o s y l bromide with 2-phenyloxazolP-glycoside  5-one (63) a  considered  to  be  3-benzamido-1-  benzoyl-2-keto-4~ (2, 3,4,6-tetr a-O-acetyl-P-D-glucopyranosyloxy)-A -pyrroline  was  3  anhydride and sodium was  exchanged  produced.  On  refluxing  with a c e t i c  a c e t a t e i n p y r i d i n e , one benzoate  for  an  acetate  group  group  giving  1-acetyl-3-benzamido-2-keto-4-(2,3,4,6-tetra-0-acetyl-p-Dglucopyranosyloxy)-£ -pyrroline.,The  crystal  undertaken  assignment of s t r u c t u r e  3  to  verify  the  initial  structure  was  based upon mass spectrum, n.m.r., and c h e m i c a l data. EXPERIMENTAL Recrystallization  of  1-acetyl-3-benzamido-2-keto-4-  (2,3, 4, 6 - t e t r a- O-acet y l - f i - D - g l u c o p y r a n o s y l o x y ) - ^ - p y r r o l i n e 3  from hexane-acetone gave c o l o u r l e s s r e c t a n g u l a r c r y s t a l s . crystal  chosen  f o r study was mounted with b p a r a l l e l t o the  g o n i o s t a t a x i s and had dimensions mm.  Unit-cell  and  and d i f f r a c t o m e t e r were r e f i n e d 19  The  space group  of  X  0.07  data were o b t a i n e d from  film  measurements.  ca  The  0.20  X 0.20  unit-cell  parameters  by a l e a s t - s q u a r e s treatment of s i n ©  values f o r  2  reflections  measured  on  a  diffractometer  with  Cu KoC  radiation. Crystal  Data  C ^,H3©N 0ii a  ,  1  M = 590.54  ,  monoclinic,  ©  a = 19.629(5),  b=  0 = 1447.8 (6) A , 3  7. 504 (2), Z = 2,  c = 9.830 (2) A,  £ = 90.53 (2)°,  O = 1.35(1) gem- ,  F{000) = 620  3  c  ©  (20°C, Cu K « , A = OkO,  1.5418 A, /x=  9.4  cm" ) . Absent 1  reflections  k * 2n d e f i n e t h e space group £2^ (C|, No. 4 ) .  Intensities E l e c t r i c XED Cu Kot  of  measured on a Datex-automated General  6 d i f f r a c t o m e t e r , with a s c i n t i l l a t i o n  (nickel  scan a t 2° m i n in  were  filter  and  pulse height analyser) , and a  over a range of  - 1  counter,  (1.80 * 0.86  tan 9)  9-29  degrees  29, with 10 s background counts being measured at each the  scan.  Data  were  measured  to  29  = 120°  end  (minimum  o  i n t e r p l a n a r spacing 0.89 A) . A check r e f l e c t i o n was every 40 r e f l e c t i o n s greatest  deviation  throughout  from the i n i t i a l  f i n a l i n t e n s i t y was  1.04  due  to  were  the  low  value  2  and  B =  The  value was -4.5% and  applied,  of /*..  above background where o* (I) time  Of  and  the  the  2336  intensities  less  = S + B * (0.05S)  averaged  r e f l e c t i o n s were c l a s s i f i e d weight  collection.  the  structure  were d e r i v e d . No a b s o r p t i o n c o r r e c t i o n was  r e f l e c t i o n s measured, 49 8 had  count  data  times the i n i t i a l v a l u e . L o r e n t z and  polarization corrections amplitudes  the  monitored  as  2  background  unobserved  applied  independent than  3«-(I)  with S = scan count.  and  These  given  zero  i n the r e f i n e m e n t . STBOCTURE ANALYSIS  As  previously  demonstrated  in  c h a p t e r 5, methods are  a v a i l a b l e f o r the s t a t i s t i c a l d e t e r m i n a t i o n of the phases the s t r u c t u r e f a c t o r s d i r e c t l y from the s t r u c t u r e The b a s i s f o r these d i r e c t methods was for  the  centrosymmetric  space  general  group  values  case i n which the phases c o u l d o n l y  i s non-centrosymmetric and  amplitudes.  d i s c u s s e d i n chapter 5  have values of 0 or IT (corresponding t o • or the  of  cannot  always  signs).  When  the phases can have be  added  together  n u m e r i c a l l y . F o r t u n a t e l y J . Karle and I. K a r l e (64) have been  95  able  to  g e n e r a l i s e the  previous structure, procedure  is  procedure already i l l u s t r a t e d  to i n c l u d e the  acentric  similar  to that f o r c e n t r i c  normalised s t r u c t u r e  factors  were  solution. were' was  searched  for  attempted. The  zero.  The  reflections  10-9  and  be  expansion i n d i c a t e d  the  phases  of  determined  After several the  the in  terms  of  origin,  reflections,  a l l o w i n g the  between 0 and  500  mc,  and  4 11  750  mc,  30.  These s e t s were used as  giving  v a r i o u s combinations of the  l e a d i n g to sixteen  phases  Hauptman  relationship  structures. ,  (2*)  using  involved  the  the  reflections 5  6-1  250,  indicated  500, in  be  and  66) ,  used f o r  which  (given on as  the  and Table  input to a computer program  (ref 65  the  only  the tangent formula  cannot  using  1 4 4 to  phases 0,  s e t s as  produced  fixing  phase of r e f l e c t i o n and  these  enantimorph  given i n Table 29  mentioned  origin  of  70  u n s u c c e s s f u l runs u s i n g a l l  combination reflections  m a j o r i t y of the  previously  Sayre  the  were  then  o f K a r l e and  by  which were given phases  solution  98)  JEj's  largest  defined  r e s u l t s . That i s the  determines  the  a manual expansion  satisfactory  vary  basis f o r  of a group of s i x prominent r e f l e c t i o n s  symbol  enantimorph by  37 3  three  reflections and  3 11  the  t h a t i f any  symbols.  fixing,  and  could  (  the  The  structures;  and  with the  relationships  r e f l e c t i o n s c o u l d be  assigned 373  cut  calculated  were chosen as  o r i g i n i n P2  manual  symbols  largest  70  ^,-2  13 0 -6,  reflections given  > 1.35  Of t h e s e the  reflections of  JEJ  with  the  structure.  very  reflections  in  page  simple  non-centrosymmetric  96  T a b l e 29  Basic s t a r t i n g set o f r e f l e c t i o n s for 1-Acetyl-3-benzamido-2-keto-4-(2,3,4,6-tetra-O-acetylP-D-glucopyranosyloxy) - & - p y r r o l i n e 3  h  k  *  13  0  -6  3. 3 0  0'  1  0  -9  2.85  0 * origin  3  1  1  2.72  0-  1  4  4  2. 49  2 50  5  6  -1  2. 47  a  4  1  2.67  b  1  i n  phase(mc)  97  Table  30  B e s u l t s f o r the s i x t e e n s t a r t i n g s e t s i n the phase determining  ©*  Ek  0.52  116  0. 33  328  250  0.78  226  0.28  349  0  500  0.80  227  0.27  348  4  0  750  0.65  166  0.31  343  5  250  0  0.80  224  0.30  344  6  250  250  0.56  121  0.32  340  7  2 50  500  0.65  152  0.32  343  8  250  750  0.55  119  0.32  326  9  500  0  0.79  223  0. 29  345  10  500  250  0.60  141  0.31  336  11  500  500  0.59  169  0. 24  358  12  50 0  750  0.56  115  0.37  324  13  750  0  0.64  159  0. 32  339  14  750  250  0.56  125  0.33  333  15  750  50 0  0.72  200  0. 29  343  16  750  750  0.58  1 60  0.24  349  * Total N =  373  Set  a (me)  b (mc)  1  0  0  2  0  3  t  procedure  N*  98  .  § lE E . lsin(^<t> . ) K  H  K  H  K  tan Each r e f l e c t i o n i s examined i n descending and  a  phase  phases o f  i s determined  pairs  calculated  of ^-2  i n the f i r s t  f o r i t from the p r e v i o u s l y known  related  reflections.  This  process  have been determined  The  phases  c y c l e can then be used i n the  c y c l e t o g i v e more and b e t t e r approximations phases.  order of |E|,  i s continued  to  second  the c o r r e c t  u n t i l most of t h e phases  and t h e r e i s l i t t l e change i n the  values  of the c a l c u l a t e d phases from c y c l e to c y c l e . Before a new phase was accepted v a r i o u s c r i t e r i a must be s a t i s f i e d ; the c o n s i s t e n c i e s t exceed  H  and o< of the new phase had t o  the a r b i t r a r y values 0.25 and 4.0 r e s p e c t i v e l y , where  J& t„  *  2  B2  ol = JE I . V f l  =  2  + B2  HJi I.II . l K  u  K  I f a new phase angle s a t i s f i e s used  these  criteria,  i n the d e t e r m i n a t i o n o f the phases o f other  cycles  successive  i s d i f f e r e n t by 250 mc, then the phase i s c o n s i d e r e d  to be unknown i n the f o l l o w i n g c y c l e and t h e r e f o r e cannot used  i n the d e t e r m i n a t i o n  the r e l i a b i l i t y index RKarle £ Rk  =  lE jcalc M  sets  t , and  | |E | obs-|E 1 c a l c |  I  H  M  —  |E |obs  a r e derived  M  from  use of the tangent  formula, f o r the s i x t e e n s t a r t i n g s e t s , a r e given Both  of  (Rk), given by  1 where  be  o f other phases, but i t i s then  r e c a l c u l a t e d i n the next c y c l e . The f i n a l values  30.  is  reflections  i n the f o l l o w i n g c y c l e * I f the phase angle i n two :  i t  i n Table  11 and 16 looked promising but the E map was  99  calculated phases  from s e t 11 as t h i s  determined  positions  (N).  had  The  E  the  map  greater  based  on  number  of  s e t 11 gave  f o r 36 of the 42 heavy atoms i n i t s top  50  peaks.  F i x i n g the y c o - o r d i n a t e o f atom 0(1) at 0.8300 t o d e f i n e origin  in  the  space  group JP2 , and r e f i n i n g the remaining t  p o s i t i o n a l and i s o t r o p i c atoms,  gave  an  B  the  thermal  factor  of  parameters 0.230.  for  these  A difference  revealed  the p o s i t i o n s o f the remaining heavy atoms  further  cycles  of f u l l - m a t r i x l e a s t - s q u a r e s  36  Fourier and  two  r e f i n e m e n t with  a n i s o t r o p i c thermal parameters f o r a l l the non-hydrogen  atoms  reduced B to  stage  positively hydrogen  0.090.  A  revealed  atoms.  calculated  difference  the  The  positions  remaining  positions.  Fourier  Due  of  hydrogen  at  only  this 17  atoms  of the 30 were  given  to the e x c e s s i v e expense and the  nature of the problem, the refinement was concluded a f t e r more  cycles,  parameters the  varying  only  and a n i s o t r o p i c  hydrogen  atom  the  heavy  atom  two  positional  temperature f a c t o r s , but i n c l u d i n g  positions  and  isotropic  temperature  o  f a c t o r s , 0 = 63 X 10~ value was  atomic  correction ref  refinement.  The  final  s c a t t e r i n g f a c t o r s and anomalous s c a t t e r i n g  f o r the C, N, and O atoms were taken from  atoms  w = 1/o-2(F)  from  where  ref  tr  2  (F)  39. is  The  derived  weighting from  <r (I) gave uniform average v a l u e s of  ranges  of  2  refinement.  and  was  ref  14  and t h e s c a t t e r i n g f a c t o r s f o r the  defined  i£oj  E  r e f l e c t i o n s with I > 3«-(i) .  15 r e s p e c t i v e l y ,  hydrogen  i n the  z  0.079 f o r 1838  The  and  A ,  3  employed  in  the  scheme: previously  w(Fo-Fc)  2  over  the f i n a l stages o f  100  An  attempt  was  made  to  determine  the  absolute  c o n f i g u r a t i o n of the molecule through anomalous s c a t t e r i n g o f the non-hydrogen atoms. The enantimorph that  generated  by  changing y t o -y,  and Hamilton's t e s t ratios.  Unfortunately  the  chemical  parameters and  (A), and  (B), were both  refined  (67) a p p l i e d t o the neither  s i g n i f i c a n t l y more c o r r e c t . of  i n Table 31,  resulting  (A) nor  (A) was  (B) was  R  proved to be  t h e r e f o r e chosen i n  evidence. The f i n a l p o s i t i o n a l and  appear i n Tables 31 and 32 r e s p e c t i v e l y .  calculated  factor  structure  factors  are  view  thermal Measured  available  from the  U.B.C. L i b r a r y . RESULTS AMD Fig.  DISCUSSION  14 shows a g e n e r a l stereoview  of  1-acetyl-3-benz-  amido-2-keto-4-(2,3,4,6-tetra-O-acety1-P-D-glucopyranosyloxy)-& -pyrroline,  with  3  the  crystallographic  scheme. Complete l i s t s o f bond l e n g t h s and a n g l e s in  Tables  33  and  34  respectively.  membered r i n g i s i n tbe c h a i r substituents weighted  at  positions  l e a s t - s q u a r e s mean  molecular  geometry  is  As  numbering are  expected the s i x -  conformation  with  equatorial  2, 3, 4, and 5. Table 35 g i v e s a plane  compared  for  this  with  ring  similar  and  tetra-0-acetyl-<*-D-mann6pyranosyl average  chloride  its  compounds,  2,3,4,6- t e t r a - O - a c e t y l - l-cyano-p-fi-galactopyranose  The  given  (68)  and  (69) , i n Table 36.  v a l u e s f o r the bond l e n g t h s [C-C,  1.53(2) ; C-0,  o  1.45(2) A], bond angles [112(3)°] and range of t o r s i o n a n g l e s [ 51.7 (7)-69.8 (7) ° ] a r e very c l o s e to those given by Jeffrey  (70) as t y p i c a l of other pyranose  Kim  rings.  The 0 - a c e t y l groups a t t a c h e d to C ( 2 ) , C (3) , C ( 4 ) , and  and  10 1  F i g u r e 1 4 (A) A g e n e r a l s t e r e o v i e w o f the molecule showing the c r y s t a l l o g r a p h i c numbering scheme  OAc  H BzN  N—Ac  AcO Figure  14(B)  Diagram o f t h e c o n v e n t i o n a l c h e m i c a l s t r u c t u r e  102  T a b l e 3J Final positional  parameters ( f r a c t i o n a l x 1 0 * , H x 1 0 ) 3  with estimated standard d e v i a t i o n s i n parentheses Atom  X  0 0 0 0 0 0 0 0 0 0 0 0 0  (1) (2) (3) (4) (5) (6) (7) (8) (9) (10) (2») (3') (4»)  »  d')  2462 ( 24 38< 3746 ( 4063( 3194 ( 3368 ( 2739 ( 3049 { 5138{ 4195( 742 ( 1556 ( 1241 ( 1500 ( 1378 ( 2696 ( 3000 ( 3336 ( 3818 ( 3423 ( 3842 ( 2370( 1794 ( 3557 { 4101 ( 4714 ( 4883 ( 3622 ( 3068 { 1204 ( 1570 ( 2019 ( 2012 ( 1296 ( 802 ( 1183( 900 ( 1083 ( 820 ( 369 ( 174 ( 445( 229 341 293 425  N (2«) c (1) c (2) c (3) c (4) c (5) c (6) c (7) c (8) c (9) (10)  c c (11) c (12) c (13) c (14) c (2') c (3») c (4») c (5») c [6«) c (7 ) f  Ci [8') c [9*) c [10') c (11».) c (12«) c (13*) (14»)  c  H (1) H (2) H (3) H (4)  1  3) 3) 3) 3) 3) 3)  **)  5) 4) 5) 3) 3) 3) 3) 3) 4) 4)  *») <0  *»)  4) 5) 5) 6) 6) 5) 6) 5) 5) 4)  **) <0  4)  <*)  5} 4)  ") 5) 5) 5) 5) <*)  830 0 8305 (10) 6 9 9 6 (11) 3691 (12) 5947 (10) 2 6 1 8 (11) 11172 (13) 5 9 2 0 (16) 420 3 (16) 2 0 9 4 (28) 8 6 3 8 (10) 3482 (11) 1 0 2 1 4 (10} 6 3 6 8 (11) 10750 (11) 6 8 5 8 (13) 7 7 1 6 (12) 6 1 9 5 (14) 5 1 3 5 (13) 4 3 8 4 (14) 3291 (15) 10137 (16) 10462 (15) 663 9 (16) 7 3 2 7 (21) 3471 (18) 2091 (23) 2 1 1 7 (19) 1436 (20) 8 0 3 8 (13) 8 9 8 5 (13) 7866 (13) 6 118 (13) 492 9 (15) 5 2 3 4 (16) 1 1 1 6 5 (15) 13067 (13) 14088 (15) 1580 5 (16) 1 6 4 4 9 (16) 15410 (16) 13764 (14) 615 844 544 590  2 6 7 4 2 [ 5) 3 798 ( 5) 2 7 6 1 I 5) 3 8 5 4 ( 6) 6 6 5 4 ( 5} 7 8 9 7 ([ 6) 4098<[ 9) 1173 i[ 7) 4 4 1 0 [ 8) 9 2 5 3 (10) 1 0 0 6 5 [ 5) 1 0 0 6 7 1 [ 5) 5 6 7 0 j[ 5) 9 4 7 9 |[ 6) 7 9 3 7 |[ 6) 5 9 2 5 1[ 7) 4623<[ 7) 3 8 2 9 |[ 8) 4 7061[ 8) 5 9 1 4 ( 8) 6 8 8 1 |[ 8) 3 5 9 3 [ 9) 2 6 4 0 |[ 9) 1459 |[ 8) 504 |[10) 3 7 4 0 |[ 8) 2 7 0 8 ([ 8) 9 0 4 4 i[11) 9977 J O ) 93 77 L 7) 8 2 7 4 | 7) 7 7 5 3 | 7) 8459i 7) 1 0 2 6 8 i [ 7) 1 1 3 9 6 i 8) 6638 8) 6 4 9 4 1 8) 5 3 5 5 < 8) 52 14 ( 10) 6 1 5 8 < 11) 72 85< 9) 74 39 i 9) 555 486 324 502  103  Table  Atom H(5) H(6A) H (6B) * H(8A) * H (8B) * H(8C) * H (10A) H(10B) * H (10C) * fl (12A) * H (12B) H(12C) H (14A) H (1 4B) * R (14C) * H(5'A) H(5«B) * H{7»A) H(7'B) H (7»C) H(10*)* H (11«) H (12') * H (13«) H(14')* H (N2*)  31  (continued)  X  Y  Z  302 431 409 164 135 195 449 432 387 442 474 544 260 317 306 246 188 51 32 105 142 99 16 -12 31 106  357 326 216 924 1101 1142 780 619 820 127 217 172 111 2 218 551 503 600 537 525 1354 1613 1782 1600 1293 1000  543 707 633 212 316 185 127 -4 -24 248 190 269 905 1025 1092 858 776 1147 1074 221 459 424 604 826 832 795  * calculated  positions  104  Table  32  F i n a l t h e r m a l p a r a m e t e r s and t h e i r standard deviations i n parentheses A n i s o t r o p i c t h e r m a l p a r a m e t e r s (U;\ x 1 0 A ) 3  Atom 0 0 0 0 0 0 0 0 0 0 0 0 0 N  (1)  (2) (3)  ;ft)  (5) [6) (7) (8) (9) (10) (2«) (3«)  («*•) (1*)  N (2*)  C (1) C (2) c (3) c (4) c (5) c (6) c (7) c (8) c (9) c (10) c (11) c (12) c (13) c (14) (2«) c (3*) c (4») c c (5*) c (6«) c (7') c (8«) c (9') c (10*) c (11*) (12*) c (13») c (14*)  c  2  £*  In.  71 [ 3) 71 [ ft) 71 ( 4) 64| [ ft) 62 ( 3) 69 [ ft) 123 ( 6) 133|[ 7) 75 ( 5) 86 [ 6) 85 [ ft) 85|[ ft) 106 ( 5) 67|[ ft) 73 ( ft) 50 [ ft) 45 ( ft) 55 ( 5) 54 [ 5) 56 ( 5) 55|[ 5) 96 ( 7) 103 i[ 7) 87 ( 7) 106 4 ( 8) 74 ( 7) 114 [ 9 ) 48 ( 6) 90 [ 7) 60 ( 5) 68 t 5} 54 ( ft) 58j[ 5) 77 ( 6) 971[ 7) 76 ( 6) 61 ji 5) 76 ( 6) 91 ( 7) 86 ( 7) 76 i[ 6) 60 ( 5)  35{ 3) 48 ( 3) 101[ 2) 1 I 3) 40 { ft) 43 ( 3) -3 ( 2) 3 [ 3) 68 { ft) 50 ( 3) 4 [ 3) -3 | 3) 77( 5) 67 [ 3) 0 ( 3) 13 ( ft) 51 { ft) 40 ( 3) 104[ 3) -2 ( 2) 68 ( 5) 78 ( ft) -1 [ ft) -11 ( 3) 44 ( ( 6} -211[ 5) -2 ft( 5) ft) 127 147( 9) 49 [ ft) -8 ( 7) -13 ( ft) 145( 9) 29 |[ 5) 7 ( 4) 109 ( 6) 414 ( 25) 127 ( 7) -6 ( 9) -10 ( 5) 45 ( ft) 54 ( 3) 18 [ 3) IT j[ 3) 35 { ft) 62 ( 3) 5 ( 3) 15 ( 3) 44 { ft) 43 ( 3) 3j[ 4) -2 ( 3) 29( ft) 50 ( ft) 12 ( 3) 2 ( 3) 34 ( 49 ( ft) -3 2| ( 3) [•• ft) ft) 40 ( 4) 50{ 5) 0 ( ft) -5 ( 3) 41 ( 5) 46 ( 4) -9 [ ft) -2 ( 3) 55 6 [ ft) 48 | 5) ( ft) -33 [ ft) 40 { 5) 55 ( ft) 2 ( ft) ( ft) 55 ( ft) 114[ ft) 4 ( ft) 50 i 5) 68 { 7) 71 ( 5) 15 ( 5) 5 ( ft) 45 { °) 7,( 5) 52 ( 5) -1\ [ 6) 55 ( 6) 61 ( 5) 15 ( 6) -8 ( 5) 6 [ 6) 73 { 8) 45 ( 5) -9 ( 5) 64 (•• 6) 125( 11) 26 ( 8) 19 ( 6) 94 | 8) 45 ( 5) 261[ 7) -5 ( ft) 41 ( 5) 181 ( 13) 69 ( 9) -7 ( 5) 110 { 9) 92 ( 7) 15^[ 6) -18 ( 5) 84 ( 7) 109 ( 10) 4 ( 7) 0 ( 6) -9 j[ ft) -1 [ ft) 42 | 5) 43 (ft) 38 ( 5) 37 ( ft) 15 ( ft) -14 ( ft) 48 0 2 ( ft) 31 { 5) ( ft) [ ft) 38 ( 5) 48 ( 4) 8 ( ft) 3 ( ft) 39 ( 4) -5 ( ft) 43 | 5) Oi[ 5) 65( 6) 7 ( 6) 14 ( 5) 49 ( 5) 49 | 5) 43 ( 5) -11^ ( 5) -6 (ft) 38 ( 5) 61 ( 5) -5 ( ft) -14 ( ft) 49 ( 4) -9 <[ 5) -14 ( ft) 5.5 { 6) 76 ( 6) -2 ( 6) -16 ( 6) 48 j 6) 99 ( 8) 0 ( 5) -36 ( 6) 42 ( 6) 5 ( 5) -13 ( 5) 55( 7) 74 ( 6) 45 j 6) -4 ( ft) 66 { 5) 8*[ 5)  * A l l H atoms had i s o t r o p i c  thermal parameters  U  -4( 3 1 (3 1( 3 -14( 4 -5( 3 17 ( 4 14( 5 -10 { 5 - 17( 6 136( 12 3( 3 6( 3 3( 3 0( 3 6( 3 ft( 44 5( 6( 4 -9 ( 4 1( 4 12( 5 20( 5 10{ 5 -8{ 5 14( 7 ~ 1 (5 -27( 7 24( 7 34( 7 - ft(4 2{ 4 ft(4 -5( 4 8( 4 10{ 5 7( 5 8( 4 2( 4 12{ 5 6( 6 -1 < 5 -4* 5  = 63 X 1 0 -  3  ° z A  105  Table 33 Bond l e n g t h s  Bond  o (A) »ith s t a n d a r d  Length  (A)  deviations  Bond  i n parentheses  Length  (A)  C (1)- 0(1)  1.43  1. 5 4 ( 1 )  0 ( 1 ) - C (4* )  1.37(1)  C (3) - c m  1. 5 0 (1)  C ( 4 » ) -C ( 5 » )  1. 4 8 (1)  C (4) -C{5)  1. 5 3 ( 1 )  C (5«) - N ( 1 » )  1.44  C(5) - 0 ( 5 )  1. 4 5 (1)  N (T) -C(2»)  1.39(1)  0 (5) -C(1)  1. 3 9 (1)  C (2») - C { 3 ' )  1. 4 9 (1)  C(5) -C{6)  1. 5 0 ( 1 )  c ( 3 « ) -C ( 4 » )  1-32(1)  C (2) - 0 ( 2 )  1. 4 3 ( 1 )  N ( 1 *) -C ( 6 » )  1 . 3 9 ( 1)  C(3) - 0 ( 3 )  1. 4 6 ( 1 )  C ( 6 » ) - 0 ( 3 »)  1.22  (1)  c (4) - 0 ( 4 )  1. 4 5  c ( 6 « ) -C ( 7 « )  1.50  (1)  C (6) - 0 ( 6 )  1. 4 6 ( 1 )  c (2«) - 0 { 2 » )  1.22(1}  0 ( 2 ) -C(7)  1. 4 0 ( 1 )  c (3«) -N{2«)  1.42(1)  0 (3) - C ( 9 )  1. 3 6 (1)  N (2«) - C ( 8 « )  1.37(1)  0 (4) - C ( 1 1 )  1. 2 9 ( 1 )  c (8») - 0 ( 4 * )  1. 2 0 ( 1 )  0 (5) - C ( 1 3 )  1. 2 9 (1)  c ( 8 » ) -C ( 9 » )  1.54  (1)  C{7) - 0 ( 7 )  1. 17 ( 1 )  c ( 9 » ) -C ( 1 0 » )  1.41  (1)  C(9) - 0 ( 8 )  1. 17 (1)  c (10' )-C(11»)  1-39  (1)  C ( V I) - 0 ( 9 )  1 . .19 (1)  c (11' )-C(12»)  1.38  (1)  C (13)-0  1. 14 ( 1 )  c (12' )-C{13»)  1.41(1)  C(7) -C(8)  1. 4 8 (1)  c <13« ) - C ( 1 4 « )  1.35  C (9] - C { 1 0 )  1.  c (14« )-C{9*)  1.40(1)  c ( 1 3 ) -C ( 1 4 )  1- 5 2 ( 1 )  C{1) -C{2)  1. 5 5  C (2) -C(3)  C(1  (10)  1)-C(12)  52  (1)  (1)  (1)  1. 4 9 (1)  (1)  (1)  (1)  106  Table Bond  angles  (deg.) w i t h s t a n d a r d  C (1) - C -C  (2) - C { 3 ) (3) - C { 4 )  - C (4) - C { 5 ) - C (5) - 0 (5) -0(5} -C(1)  -C(1) C{1) -C(2) C ( 3 ) - C (2) C (2) - C (3) C (4] - C { 3 ) C(3) -C(4)  -C{2) - 0 (2) -0(2) -0 -0  (3) (3)  -0(4) C{5) - C (4) - 0 (4) C (4) - C ( 5 ) - C (6) 0 C C C C  (5] (5) (2) (3) (4)  c  (6; 0(2] 0(3]  o  (4; 0(5]  o  -C  (5) - C { 6 ) -C(6) -0(6) - 0 (2) - C (7) - 0 (3) - C (9) -0(4) -C(11) - 0 (6) - C ( 1 3 ) -C(7) -C(8) -C{9) -C{10) - C (1 1 ) - C { 1 2 ) -C(13)-C{14) -C(7) -0(7) -C(9) -0(8)  (2; 0(3) 0 (4] - C ( 1 1 ) - 0 ( 9 ) 0 (6) - C ( 1 3 ) - 0 ( 1 0 ) 0(7) -C{7) -C{8) 0 (8) - C ( 9 ) - C ( 1 0 ) (9; - C { 1 1 ) - C ( 1 2 ) 0 ( 1 0 ) - C { 1 3) - C ( 1 4)  o  deviations i n  Angles  Bonds  C{2) C (3) C (4) C(5) 0(5)  34  106.  3 (6) 1 1 1 . 9 (6) 1 0 8 . 5 (6) 1 1 4 . 4 (6) 1 1 1 . 0 (5) 1 1 0 . 8 [6) 1 0 7 . 2 (5) 10 5 . 9 (6) 1 0 7 . 6 17) 1 0 6 . 3 [6) 105.9  [6) (7)  110.2 1 1 4 . 4 (6) 1 0 7 . 1 (6) 1 0 5 . 9 [6) 1 1 7 . 2 (7) 1 1 6 . 7 (7) 1 1 8 . 5 (8) 1 1 7 . 2 (7) 1 0 8 . 9 (8) 1 0 9 . 2 (9) 112(1) 1 1 0 . 7 (8) 1 2 2 . 4 [9) 1 2 3 . 0 (9) 125(1) 122(1) 1 2 8 . 7 (9) 1 2 7 . 8 [9) 1 2 2 . 6 (9) 127 (1)  parentheses  Bonds  0 (1) 0 (1) C (1) 0 (1) 0 (1) (4'  -C(1)  Angle  -C{2)  - C ( 1 } - 0 ( 5 ) - 0 ( 1 ) - C (4«) - C ( 4 « ) - C ( 5 » ) - C (4» ) - C ( 3 * )  c c  ) - C { 5 ' ) - N (1«)  c c c c  (4«) (5»)  (5« ) - N ( 1 » ) - C { N ( 1 ' ) - C (2» ) - C (2« ) - C ( 3 » ) - C ( 3 ' ) - C (4» ) - C  2») (3»)  (5« ) - N ( 1 ' ) - C  (6'}  ( 2 » ) - N (1 ») - C ( 6 ' } N (1» ) - C (6» ) - 0 (3*) (1* ) - C ( 6 « ) - C ( 7 » ) 0 (3* ) - C ( 6 * ) - C (7») N (1* ) - C (2* ) - 0 (2«) C (3» ) - C ( 2 » ) - 0 { 2 » ) (2« ) - C ( 3 « ) - M ( 2 » ) (4« ) - C { 3 * } - N (2«) (3* ) - N ( 2 ) - C ( 8 « ) H (2» ) - C (8> ) - 0 ( 4 » ) N (2» ) - C ( 8 ) - C ( 9 » ) 0 (4« ) - C ( 8 « } - C ( 9 « ) C (8» ) - C { 9 » ) - C { 1 0 » ) (8» ) - C ( 9 * ) - C ( 1 4 » )  c c c  ,  F  c c c c c c c  ( 9 » ) - C (1 0' ) - C ( 1 1 • ) ( 1 0 •) - C ( 1 1 « ) - C ( 1 2 « ) ( 1 1 ' ) - C ( 1 2 « ) - C ( 1 3 «) ( 1 2 » )-TC ( 1 3 ' ) - C ( 1 4 « ) (13*) - C ( 1 4 » ) - C ( 9 » ) ( 1 4 } - C ( 9 » ) - C ( 1 0 ' ) ,  1 0 6 . 1 ( 6) 1 0 8 . 2 | 5) 1 1 6 . 1 | 6) 1 2 4 . 0 < 7) 1 2 4 . 1 I7 ) 1 0 2 . 7 { 6) 1 1 1.3 ( 6) 10 6 . 2 < 7) 10 7 . 9 { 7) 1 1 1.8 | 6) 1 1 9 . 6 ( 7) 1 2 8 . 3 ( 7) 1 1 8 . 6 (7) 1 1 9 . 1 { 8) 1 2 2 . 1 | 8) 1 2 7 . 4 ( 7) 1 2 6 . 4 ^ 8) 1 1 9 . 2 ( 7) 1 3 2 . 8 { 8) 1 2 0 . 3 { 7) 12 5. 4 ( 9) 1 1 3 . 3 ( 8) 1 2 1 . 2 ) 7) 1 1 9 . 0 ( 8) 1 2 1 . 2 { 8) 1 1 9 . 0 ( 9) 120(1) 1 2 1 (1) 119(1) 1 2 1 . 4 { 9) 1 1 9 . 7 ( 8)  107  Table 35 Weighted l e a s t - s g u a r e s mean planes a) Distances (A) o f r e l e v a n t atoms from the p l a n e s with standard d e v i a t i o n s i n parentheses Plane 1: C a l c u l a t e d u s i n g 0 (5) ,C (2), C (3) and C{5) Atom 0(5) C{5)  Distance (A) -0.030{ 6) 0.061 ( 8)  A torn C(2) C (1)  Distance 0. 050 { 8) 0.700{ 8)  Plane 2: 0(2) ,0(7) ,C (7) and C(8) 0.001 ( 5) 0 (7) 0. 003 ( 8) 0(2) 0.003( 9) C(2) 0.081( 7) C(8)  Atom C(3) C(4)  D i s t a n c e (A) -0.060 { 8) -0.740 ( 8)  C (7)  -0.010 ( 9)  -0.002 (12)  Plane 0 (3) C{10)  0(3) ,0(8) ,C(9) and C{10) 0.000 ( 8) 0 (8) 0.001(11) 0.001(15) C(3) -0.205(10)  C{9)  Plane 0(4) C(12)  0 (4) ,0 (9) ,C{11} and C(12) -0.002{ 7) 0(9) -0.005(10) -0.007 (14) C(4) 0. 172 ( 9)  C(11)  0.0 18 (11)  C(6) C(5)  -0.003 (11) •0.479 (10)  Plane 5: 0(6) ,0 (10) ,C{6) ,C (13) and C(14) 0.005{ 8) 0(10) 0.017(20) 0(6) -0.025(14) C(14) 0.004(14} C(13) N{1*),C(2«) •0.014( 6) 0.002( 8) 0.050( 6)  Plane N(1») C{4») 0{2»)  ,C(3») ,C{4«) and C(2») 0.022( C{5») 0.011( N(2») 0.007(  C(5») 8) C{3') 8) 0(1) 7) C(6»)  Plane 7: 0(4») ,N{2») ,C(8») and C (9') 0.003{ 7) 0.003( 7) N(2») 0(4') -0. 178{ 8) 0.004( 8) C(3») C(9») Plane 8: C(9«) C (12«) C(8«)  C{8 •)  f  Plane 2 3 4 5  -0.016 ( 9)  C(9») ,C(10' ) ,C{11*),C (12*) ,C(13») and C{14») -0.004( 8} C (10«) 0.013( 9) C (11*) -0.011 (11) -0.002(11) C(13 ) 0.010(10) C{14«) -0.005 ( 9) 0-041 ( 9) b) D i h e d r a l angles between s e l e c t e d  Plane 1 1 1 1  •0.013 ( 8) •0.062 ( 4) 0. 128 ( 8)  Angle (deg.) 118 83 103 39  Plane 1 6 6 7  Plane 6 7 8 8  planes Angle (deg.) 34 130 9 138  108  Table _35 (continued) c) Equations of p l a n e s : IX + mY •* nZ = £ where X, Y and Z a r e orthogonal angstrom c o o r d i n a t e s d e r i v e d as f o l l o w s rXi III  *-Z-*  =  r §. 0 | 0 b i - O O  ccos p -j x-| 0 | HJ c s i n p J *-z-" r  Plane  1  m  n  £  1 2 3 4 5 6 7 8  0.924 -0.624 -0.466 -0.048 -0.091 0.681 0.920 0.761  0.365 0.063 0.883 -0.719 0.923 0.340 0.354 0.379  0.115 0.779 -0.052 0.694 0.374 0.649 -0. 166 0.526  8.086 0.335 1.076 0.258 4.122 9.603 3.979 8.375  109  Table 36 Comparison o f s t r u c t u r a l data f o r the pyranose  ring  Distance Bond C(1)-C{2) C (2)-C(3) C(3)-C(4) C(4)-C(5) C{5)-0(5) 0(5) -C(1)  I*>.  II  1.55(1) 1.54(1) 1.50 (1) 1.53 (1) 1. 45 (1) 1.39(1)  1.528(7) 1.50 0(7) 1.523(6) 1.503 (7) 1.441 (6) 1.413 (5)  III 1.529 (9) 1.56(1) 1 .476 (9) 1.524 (9) 1. 443 (9) 1.366 (9)  Angle (deg.) Bond  I  II  III ** «fc  0{5)-C(1) -C(2) C(1)-C(2) -C{3) C(2)-C<3) -C{4) C(3)-C(4) -C{5) C(4)-C{5) -0(5) C(5)-0<5) -C(1)  110. 8 (6) 106.3(6) 111.9 (6) 10 8.5 (6) 114. 4 (6) 111.0 (5)  108.9(3) 1 10. 9 (4) 112. 2 (4) 109.4(4) 110.9 (4) 111.0(4)  1 16(1) 109(1) 110(1) 111(1) 109( 1) 117(1)  T o r s i o n Angles (deg.) Bond C(1)-C(2) -C{3) -C{4) C(2)-C{3) -C{4) -C{5) C(3)-C(4) -C(5) -0(5) C(4)-C{5) -0(5) -C(1) C(5) -0(5) -C(1) -C(2) 0{5)-C{1) -C(2) -C(3)  I -51.7(7) 58.3(8) -63.0(7) 69.8(7) -68.0(7) 55.6 (7)  II -50.5 49. 3 -55.3 65.0 -64. 1 56. 8  III 49 57 57 53 49 45  I  1-Acetyl-3-benzamido-2-keto-4-(2,3,4,6-tetra-0 -acetyl-p-D-glycopyranosyloxy) - & - p y r r o l i n e .  II  2,3,4,6-Tetra-O-acetyl-l-cyano-p-Dgalactopyranose. ~  III  Tetra-0-acetyl-*-p-mannopyranosyl c h l o r i d e  3  110  C{6)  are  planar  { f a b l e 3 5 ) . The  l e n g t h s [ C r i n g - 0 , 1.45(2);  0-C,  average  1.33(2);  v a l u e s f o r t h e bond OO,  1.17(2);  and  C-  117(1);  Q-C*0 ,  e Cmethyl,  1.50(2)  123(1);  O-C-Cmethyl,  close be  A] and  angles 110(1);  to the values expected  mentioned  exhibit  and  0*C-Cmethyl,  atoms on t h e s e O - a c e t y l  thermal  motion  (see  Table  atom 0 ( 1 0 ) . , T h i s i s somewhat e x p e c t e d  o f t h e s e c h a i n s , and  intramolecular  bonding  127(2)°] a r e  f o r such groups. I t should  the t e r m i n a l  extensive  particular length  that  [Cring-O-C,  the lack  which  due  also groups  32),  in  to  the  o f very strong i n t e r -  might  help to constrain  or  these  atoms. The ring  mean p l a n e c a l c u l a t e d f o r t h e  (linked  to  shows i t t o be Other  for  pyranose  ring  by  on  pyrroline  H (1 • ) - C (2 •) ,  rings  (71  N(1')-C(5«),  pyrroline  p-oxygen bridge)  a  planar within experimental error  studies  values  the  5-membered  and and  (Table 72)  35).  found  C^'J-O^')  mean of  o 1.343 ( 5 ) ,  1.456 (8)  and  1.2 30 (3)  A  corresponding  v a l u e s f o r t h i s compound a r e  and  A.  1.22(1)  probably for  the  due  Any  respectively. 1.39(1),  shortening i n the f i r s t  to the a c e t y l  C(2«)-C{3*),  s u b s t i t u e n t on  C(4*)-C{5»),  two  1.44(1)  distances i s  N(1').  and  The  The  values  C(3»)-C(4')  bond  o  distances to  those  of  1.48 ( 1 ) ,  found  by  1.49 (1) and B o e y e n s and  1.32(1) A a r e v e r y Kruger  1.31  A ] , The  range o f i n t r a - a n n u l a r  ring  i s from  102.7  Weighted  [1.52,  angles f o r the  1.52,  and  pyrroline  111.8°.  least-squares  benzamido group, benzene r i n g  to  (73)  similar  the a c e t y l  mean  group  planes c a l c u l a t e d  f o r the  a t t a c h e d t o N ( 1 * ) , and  show them t o be p l a n a r ( T a b l e 3 5 ) . A g a i n  the  the  I S M e 37 A) I n t e r m o l e c u l a r C-H...0 i n t e r a c t i o n s ( d i s t a n c e s i n A angles i n deg.) D-H...A C{7«)-H(7»B) ...0<2«) i C(8)-H(8C) . . . 0 ( 3 » ) 2 C (5)-H ( 5 ) . . . 0 ( 7 ) 3 C(10)-H(10A) . . . 0 ( 1 0 ) *  H. ..A 2.57(1) 2.46(1) 2.29(1) 2.68(1)  D. ..A 3.53 (1) 3.42 (1) 3.28 (1) 3.36 (1)  B) I n t r a m o l e c u l a r 0...H c o n t a c t s 2.41 (1) 2. 46 (1) 2.91 (1) 2.55 (1) 2.47 (1) 2.55(1) 2.08 (1) 2.25 (1) 2.33 (1)  0(2*)- . , H (N2*) 0(2*) . ..H(7'A) 0(3»). . . H(14A) 0(4») . ,.H (8B) 0{4»). ..H (10») 0 ( 7 ) . , ?H(2) 0 ( 8 ) . . .H{3) 0(9) ., -H(4) 0(10) . . . H (6 A) -x, x, x, 1-x,  -1/2*y, 1 y# -1+y, 1/2+y, +  1-z -1 +z z 1-z  D-H. ..A 142(1) 146 (1) 148(1) 117 (1)  112  Figure  15  A s t e r e o s c o p i c diagram o f the u n i t - c e l l viewed down b bond l e n g t h s and a n g l e s are as e x p e c t e d In H. ..0  the  crystal  i n t r a - and  there  Of p a r t i c u l a r  H(2)..-0(7)  contact  steric  e x t e n s i v e numbers of c l o s e  note i s t h e  compared  to  constraints  induced  by  the o t h e r a x i a l  and  packing  i n the c r y s t a l  in  longer  hydrogen,  probably  due  to  a postulated intermolecular  hydrogen bond between 0(7) t h e molecules  summarized  significantly  oxygen c o n t a c t s . T h i s d i f f e r e n c e i s  of  groups.  i n t e r m o l e c u l a r c o n t a c t s which are  i n T a b l e 37.  acetyl  are  f o r these  H(5).  A  stereoview  of  the  l a t t i c e can be  seen  F i g . 15. The c r y s t a l  indicated n.m.r., and  structure determination  t h a t the s t r u c t u r e s u g g e s t e d other chemical data  was  for by  in fact  this  compound  the mass spectrum, correct.  113  SOMMA BY  11 n  The aim of t h i s structures  of  research  the  has  been  to  the  three  the  f i v e molecules p r e v i o u s l y d e s c r i b e d . The  s t r u c t u r e d e t e r m i n a t i o n s themselves i n v o l v e d of  determine  major  methods  currently  c r y s t a l l o g r a p h y f o r overcoming the phase  the  utilization  a v a i l a b l e i n X-ray problem and  thereby  deducing the c r y s t a l and molecular s t r u c t u r e . For  any compound the c h o i c e of the most s u i t a b l e method  f o r s t r u c t u r e d e t e r m i n a t i o n i s e s s e n t i a l l y determined by nature  of  the compound i t s e l f .  P a t t e r s o n methods, d e s c r i b e d  i n Chapter 2, i n v o l v e a process i n which i t i s e s s e n t i a l the molecule c o n t a i n one or more 'heavy' atoms. The and  the  the  that  tungsten  two ruthenium compounds (Chapters 2, 3, and 4) with  t h e i r heavy metal atoms were t h e r e f o r e i d e a l f o r t h i s method. I f , however, a molecule c o n t a i n s only atoms the  same  or  similar  atomic  numbers,  which  e.g.  have  most o r g a n i c  molecules, the P a t t e r s o n s y n t h e s i s i s u n s u i t a b l e . Although i t may  be p o s s i b l e t o produce heavy atom  molecules  and  hence  use  the  derivatives  Patterson  possible  to  determine  the  these  method, a l t e r n a t e  ' d i r e c t methods* have f o r t u n a t e l y been developed it  of  structures  which  make  directly.  The  s t r u c t u r e o f the c a f f e i n e and p y r r o l i n e d e r i v a t i v e s d e s c r i b e d i n Chapters 5 and 6 were determined by use methods. of  the  of  these  The a c t u a l method used depends upon the space compound.  The  caffeine  structure  determined by centrosymmetric d i r e c t  was  direct group  therefore  methods ( i t c r y s t a l l i z e d  i n t h e centrosymmetric space group P2,/c) while the s t r u c t u r e of  the  p y r r o l i n e compound was solved by  d i r e c t methods ( i t c r y s t a l l i z e d  in  the  non-centrosymmetric non-centrosymmetric  115  space group  P2 ). |  Although and  any  the f i v e compounds sere e s s e n t i a l l y  meaningful  intermolecular  correlation  interactions,  in  terms  etc.,  r e s u l t s f o r the i n d i v i d u a l molecules and  unrelated;  of  was  bonding,  impossible,  were  both  the  interesting  useful. The  analysis  of the seven-coordinate  (Chapter 2) showed i t t o have a d i s t o r t e d geometry.  The  tungsten-iodine  tungsten compound capped  distances  of  octahedral  2.848(2)  and  o  2.856(2) A appeared to be the  first  bond l e n g t h s i n a seven-coordinate The  two  sulphur-bonded  t e t r a k i s compound of  (Chapter  the c h l o r i n e atoms but  atom. I t i s formation  thought  of  an  that  a  3) had  cis  all  three  configuration.  4) the e x t r a l i g a n d was  1-1  very s i m i l a r o c t a h e d r a l  (Chapter  in  of  environment.  ruthenium compounds had  s t r u c t u r e s . The t r i s complex ligands  determinations  In  the  replaced  one  c o o r d i n a t e d through  steric  influences  DMSO  the oxygen  prohibit  a l l sulphur-bonded complex, but  the  electronic  e f f e c t s keep the S-bonded l i g a n d s i n the c i s c o n f i g u r a t i o n . Caffeine hydrochloride dihydrate planar c a f f e i n e molecule interest  was  the  (Chapter 5) contained a  protonated a t  N (9) .  particular  e f f e c t o f p r o t o n a t i o n on the bond l e n g t h s  between atoms i n the fused r i n g system. I t i s considerable  Of  rearrangement  must  be  occuring  believed  c l o s e to the  protonated c e n t r e , but t h a t t h i s rearrangement does not t o be t r a n s f e r r e d to the r e s t of the The (Chapter  molecular 6) was  geometry  in  that  seem  molecule. the  very s i m i l a r to t h a t found  pyrroline f o r other  compound related  116  compounds.  This  compound  d i d , however,  e x h i b i t extensive  numbers o f c l o s e C-H..,0 i n t r a - and i n t e r m o l e c u l a r Some degree o f hydrogen of  contacts.  bonding was a l s o shown by another two  the compounds s t u d i e d . The ruthenium anions i n Chapter 3  were l i n k e d i n a chain l i k e s t r u c t u r e throughout the to  t h e dimethylammonium  hydrogen bonds, while  cations  the caffeine  H...C1 and N-H...0 hydrogen bonds.  lattice  v i a N-H...0 and N-H...C1 crystals  contained  0-  117  Eef erences I.  I n t e r n a t i o n a l T a b l e s f o r X-ray C r y s t a l l o g r a p h y , vols. I - I I I , Kynoch P r e s s , Birmingham. Vol..1, 1952; v o l . I I , 1959; and v o l . I l l , 1962.  2.,  G. H. Stout and L.H. Jensen. X-ray S t r u c t u r e D e t e r m i n a t i o n : A P r a c t i c a l Guide. The MacMillan Company; London, 1968.  3.  13.J. Buerger. C r y s t a l S t r u c t u r e A n a l y s i s . J . Wiley and Sons, Inc., New York, 1960.  4.  M.J. Buerger. 1959.  5.  M.M. S o c l f s o n . X-ray C r y s t a l l o g r a p h y . Cambridge U n i v e r s i t y Press, 1970.  6.  H. L i p s o n and W. Cochran. The C r y s t a l l i n e S t a t e , v o l . 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Z a n z a r i . Acta C r y s t . , 1974, B30, 127. 72. L. Dupont, 0. Dideberg, 1975, B31, 1018.  and A. Welter.  73. J.C.A. Boeyens and G.J. B26, 668.  Kruger.  Acta C r y s t . ,  0\ *. *  Acta C r y s t . , 1970,  James Trotter  Additional data  THE  STRUCTURE DETERMINATION OF THREE  INORGANIC AND TWO Bl  ORGANIC  COMPOUNDS  X-RAY DIFFRACTION•  By  ANTHONY MERCER.  B.Sc,  University  of Bristol,  England,  1972.  A T H E S I S SUBMITTED I N PARTIAL FULFILMENT OF T H E REQUIREMENTS  POR THE DEGREE OF  DOCTOR OF PHILOSOPHY  in  t h e department of CHEMISTBY.  He a c c e p t  this  the  THE  thesis  reguired  as conforming standard.  ONIVERSITY OF BRITISH  JUNE 1977. @  to  Anthony Mercer, 1977  COLUMBIA  (2,3-Bis(dimethylarsino)-1,1,1,4,4,4-hexafluorobut-2-ene-As,As)tricarbonyldiiodotungsten(II) jAnthony Mercer and James Trotter Observed and calculated structure factor amplitudes (reflections with intensity < 3a(I) are marked with an a s t e r i s k ) .  H  K  L  0 0 0 0 0 0 0 1 1 1 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 3 3 3 3  0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 u 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0  2 4 6 8 10 12 14 -14 -12 -10 -8 -6 -4 2 4 8 10 12 14 -14 -12 -10 -8 -6 0 2 6 8 10 12 14 -14 -12 -10 -8 -4 -2 0 2 4 6 8 10 12 14 -14 -12 -10 -8 -6 -4 -2 0 2  4 4 4 4 4 4 4 4 4 4 4 4 4  4  6 8 10  FO 83. 31 252. 25 22.58* 16.39* 23.99 186.74 25.29* 34.70 118.35 130.59 46.69 188.65 91.47 287.92 16.05 56. 22 158.41 95. 10 20.24* 183.92 42.07 41.61 36.41 31.74 244. 11 33.09 68.05 41.20 219.83 81.56 22.47* 25. 17 72.46 122.45 368.61 38.02 108.28 46.31* 186.19 275.08 89. 80 21.21* 117.85 84.81 66. 17 151.54 50.08 239.08 230.99 90.77 326.81 367.98 115. 12 335. 17 96.34 140.24 82.78 161.64  FC 50.20 209.28 5.70 10.12 24.91 179.12 27.56 40.04 113.40 137.38 52.02 189.89 86. 3 2 229. 15 10.96 55.28 156.61 96.58 15.08 182.45 45.19 45.01 39.37 34.02 249.09 40.46 67. 13 42.63 209.24 83.18 7.08 18.29 69.94 130.59 317.23 22.62 103.01 75.08 201.41 238.99 85.67 27.37 113.78 80.70 71.10 157.32 53.08 234.94 223.48 94.54 312.41 311.76 146.76 315.37 79.59 147.29 82.45 162.37  H 4 . 5 5 5 ' 5 5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 6 6 6 6 6 6 7 7 7 7 7 . 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 8 ' 8 8 8 8 9 9 9 9 9 9  K 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0  L  FO  55.09 56.04 29.03 154.55 47.16 265.36 0.00* 248.26 14.93* 93.35 125.78 55.72 10.82* 50.92 24.35* 112.57 5.71* 30.70 17.01* 413. 13 149.64 95.40 12.74* 174.00 27.74* 36.11 50.81 15.62* 25.7*4 81.67 257.23 19.71* 128.63 138.46 404.91 11.99* 211.37 57.47 18.97* 108.19 55.52 86.02 176.99 126.82 39.83 17.84* 395.37 0.00* 61.64 4 41.87 6 8 " -86.44 10 32.86 -14 19.08* 152.58 -12 204.41 -10 151.98 -8 -6 65.23 -4 67.73  12 -14 -12 -10 -8 -6 0 2 4 6 8 10 12 -14 -12 -10 -8 -6 -2 0 2 4 6 8 10 12 -14 -12 -10 -8 -6 -4 -2 0 2 4 6 8 10 -14 -12 -10 -8 -6 -4 -2 0 2  FC 49. 16 57.08 25.80 152.81 50.26 224.45 12.07 272.36 13.86 94.57 116.24 46.89 23.48 48.43 19.60 112.05 13.09 31.27 17.49 388.03 161. 14 86.08 4.23 176.67 34.88 22.93 54.71 19.52 2 1. 72 79.39 226.89 9.6 1 119.22 126. 18 392.64 1.64 196.32 53.07 8.38 110.64 55.81 84.01 171.76 129.94 40.33 19.90 382.12 7.03 66.46 46.63 77.77 31.28 13.80 154.91 201.03 142.45 49.23 59. 12  H  9 9 9 9 9 9  10 10 10 10 10 10 10 10 10 10 10 10 11 11 11 11 11 11 11 11 11 11 11 12 12 12 12 12 12 12 12 12 12 12 13 13 13 13 13 13 13 13 13 13 14 14 14 14 14 14 14 14  K  L  0 -2 0 0 0 2 0 4 0 6 0 8 0 -14 0 -12 0 -10 0 -8 0 -6 0 -4 0 -2 0 0 0 2 0 4 0 6 0 8 0 -14 0 -12 0 -10 0 -8 0 -6 0 -4 0 -2 0 0 0 2 0 4 0 6 0 -14 0 -12 0 -10 0 -8 0 -6 0 -4 0 -2 0 0 0 2 0 4 0 6 0 -14 0 -12 0 -10 0 -8 0 -6 0 -4 0 -2 0 0 0 2 0 4 0 --12 0 --10 0 -8 0 -6 0 -4 0 -2 0 0 0 2  FO  FC  86.22 92.11 163.55 153.83 13.03* 13.68 18.43* 15.97 145. 10 154.32 30.00* 28.05 141.62 142.81 60. 94 59.03 48.09 45.77 145. 17 139.78 205.83 186.70 259.76 243.68 215.31 203.77 16.68* 21.11 60.92 65.39 84.76 74.07 77.87 66.42 13.44* 1.30 0. 00* 8.52 24.20* 22.97 89.24 88.74 197.83 192.37 222.89 213.49 104.56 110.40 133.31 131.31 31.70* 43.80 62.53 60.69 116.72 106.46 39. 01 39.31 35.09 29.77 17.89* 6.97 49.62 48.79 114.59 113.39 32.01 24.94 162.50 166.4 6 156.34 167.87 103.67 103.78 56.96 54.01 103.87 89.19 60. 17 46.35 14.71* 8.22 73.70 73.09 35.62 33.73 25.21* 24.53 65.47 63. 17 108.94 103.64 150.63 147.27 0.00* 6.61 136.59 124.02 0.00* 2.27 31.91 28.26 60.71 52. 18 37.97 37.73 48.44 48. 15 135.36 133.00 3.36* 7.22 80.99 70.52 39.23 32.87  H 15 15 15 15 15 15 15 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0  K  L  0 -12 0 -10 0 -8 0 -6 0 -4 0 -2 0 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 -15 -14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 5 6 7 8 9 10 11 12 13 14 15 15 14 . - 13 — 12 — 11 — 10  FO  FC  81.72 80.94 44.66 36.78 105.68 101.18 20.60* 3.89 42.94 50.58 24.88* 13.52 22.55* 6.07 236.54 192. 10 242.78 204.34 188.28 164.27 144.52 137.36 161,72 148.28 372.87 311.87 . 150.98 146.34 129.68 121.6 1 87.28 87.73 44.37 40.68 36.05 30.62 0.00* 9.32 88. 58 82.66 0.00* 5.03 45.88 45.80 14.58* 18.41 44.74 44.03 62.13 60.79 38.71 38.84 51.06 51.07 24.39 25.46 93.29 8 8.28 0.00* 9.4 1 219.26 194.37 133.23 122.01 66.74 72.61 34.22 34.40 84.86 89.89 53.87 54.47 187.36 160.05 451.01 475.80 266.44 256. 1 1 38.71 29.31 8.28* 5.07 375.95 324.34 172.78 166.94 129.58 127.62 15.44* 16.24 73.42 74.71 52.30 43.33 79.65 80.63 104.59 103.81 12.03* 9.74 14.65* 7.22 12.03* 18.37 83.46 82.54 30.63 30.37 65.68 64.70 98.96 99. 10 137.62 134.20 104.78 103.35  H 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 4 4 4 4  K  _! -1  -1 -1 -1 -1  -1 -1 -1 -1 -1  -1 -1 -1 -1  -1 -1  -- 1i -1  -1 -1 -1 -1 -1 -1 -1 -1  -i  --1r -1 -1  -1 -1 -1 -1 -1 -1  -1 -1  -1 -1 -1 -1 -1 -1 -1  -- i1 -- 1-j -1 -1 -1 -1  -1 -1  L -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 -15 -14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 -15 -14 -13 -12  FO 90.04 110.14 67.20 . 183.82 41.85 135. 14 57.34 353.49 210.03 98.22 37. 84 251.86 190.32 151.20 39.73 110.81 162.50 40.46 31.11 164.57 154.36 111.26 38.90 28.45 26.30* 165.14 102.52 83. 03 34.85 21.58 254.95 97.87 95.05 50. 80 101.19 147.50 43.94 276.93 73.99 56. 14 75. 34 170.07 122.39 265.66 190.06 52.72 39.49 122.70 173.80 163.94 32.98 19.79* 34.62 32.71 73. 13 52. 29 41.95 25.75  FC  H  86.60 98.08 73.06 181.65 41.05 127.51 59.03 303.61 175.93 90.87 40.94 234.57 164.00 143.23 27.12 112. 15 161.03 40.38 32.92 152.67 145.81 112.17 39.94 25.03 23.16 160.40 104.43 81.35 31.31 22.82 235.06 101.33 93.16 41.18 95. 81 142.24 50.62 244.42 79.51 74.83 74.36 163.85 131.31 243.20 183.19 57.58 39.71 119.34 168.77 161.85 27.26 10.95 36.08 29.24 73.55 56.87 36.93 23.80  4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 5 5  5 5 5 5  5  5 5 5 5 5  5  5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 6 6 6 6 6  L -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 10 11 12 13 -15 -14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 10 11 12 13 -15 -14 -13 -12 -11  FO  FC  165.78 54. 30 62.28 140. 16 168.15 261.08 43.23 297.31 216.60 380.37 12.50* 138.25 79.45 48. 42 69.71 55. 65 38. 18 50. 46 93.39 65. 12 70.54 13.21* 97.78 0.00* 0.00* 24. 63 25.22 22.23* o ~>  r\ ft  i. . V H  81.04 195.27 272.89 158.27 42. 84 36.09 264.25 40. 44 62.68 102.54 79.09 173.80 267.75 201.31 121.30 21.95* 85.32 97.03 30.26 86.76 19.37* 21. 12* 46.62 33.70 20.14* 20.79* 84.85 48.62 85.34  165.43 51.60 59.43 133.37 166.82 227.45 29.60 263.10 181.25 335.74 21.43 145.48 87.38 54.85 75.24 67.39 34.47 49.00 92.47 63.82 66.28 9.92 92.17 5. 10 3.25 16.30 27.44 23.43 19. 14 79.31 190.29 247.94 155.44 45.88 38.46 230.90 33.21 48.83 102.56 81.76 186.28 276.07 195.41 114.79 23.97 81.91 93.51 30.47 83.97 7.80 11.35 40.26 30.47 19.37 19.42 84. 12 53.56 89.29  H 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8  K  L  _-| -10  -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1  -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 10 11 12 -15 -14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 10 11 -15 -14 -13 -12 -11 -10 -9 -8  FO 85. 31 59.77 46.45 97. 18 161.78 41.82 139.06 149.97 224.96 125.84 136.54 202.59 228.54 111.49 81.66 75. 13 0.00* 48.56 11.95* 81. 26 18.00* 27.35* 32.41 35. 10 56. 15 73.75 30.00 116.51 21.76* 17.16* 167.21 95.03 75. 88 184.21 219.75 33. 11 11.43* 33. 1 1 301.70 225.94 24.86* 71.68 0.02* 122.85 11.69* 139. 19 119.27 12.21* 41.57 29.52 99.52 43.74 87. 83 66.67 70.51 116.92 52. 56 42.07  FC  H  L  88.38 60.25 48. 13 100.09 154.18 40.73 129.98 141.10 232.04 127.43 138.88 217.90 259.24 116.39 94.97 70.04 19.15 45.59 12.68 81.25 7.52 25.45 28.68 37.91 52.47 72.72 32.09 117.42 19.15 13. 14 158.54 96.01 87.30 173.21 214.60 35.59 6.09 28.95 31 1.99 227.71 3.52 68.40 12.48 122.71 17.23 130.78 115.88 10.85 40.32 20.42 96.18 40.20 85.77 68.76 72.53 120.52 54.28 29.31  8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10  -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 10 15 14 13 12 11 10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 15 14 13 12 11 10 -9 -8 -7 -6 -5 -4 -3 -2 -1  FC 24. 54 80.75 52.38 123.38 17.94* 63.29 113.95 48. 89 61.90 123.54 93.66 34.96 51.83 168.21 1 12.30 69. 42 38.25 14.68* 11.29* 84.01 109.73 14.88* 56.24 57.90 151.00 72.00 133.50 170.48 26.04 160.20 46. 25 32.36 64.48 130.04 78.74 63.48 48.44 104.02 160.54 69.72 46. 26 0.00* 37.09 84.75 28.89 38.07 85.26 115.02 112.55 13.54* 127.98 140.42 182.42 25.26* 30.40 117.02 17.35* 45.98  FC 14.05 70.90 49.44 113.72 9.34 62.54 119.37 51.01 62.89 108.71 91.88 52.77 55.48 168.09 115.48 70.63 37.18 22.79 7.31 86.05 115.26 8.69 60.97 58.90 150.33 74.50 128.09 158.04 3 1.18 165.80 48.01 31.34 69.14 128.88 77.29 57.40 38.47 96.58 155.58 72.23 44.75 5.19 38.89 82.02 22.58 39.08 89.56 117.51 112.93 21.32 123.60 137.48 173.37 20.95 33.31 114.18 5.08 44.75  H 10 10 10 10 10 10 10 10 10 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 13 13 13 13  K  L  0 1 2 3 4 5 6 7 8 -15 -1" -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 -15 -14 -13 -12 -11 -10 -1 -9 -1 -8 -1 -7 -1 -6 - 1 -5 - 1 -4 -1 -3 - 1 -2 - 1 -1 -1 0 -1 1 -1 2 -1 3 -1 4 -1 5 -1 6 -1 -14 - 1 -13 - 1 -12 -1 -11  -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 —i -1 -1 -1 -1 -1 -1 -1 -1  -i  FO 88.54 66.56 32.01 27.93* 32.82* 31.07* 0.00* 52.06 26.30* 11.72* 72.28 66.28 29.09* 30.48* 21.73* 158.29 93.88 43.55 40.34 72. 1 1 137.29 41.28 150. 10 95.79 104.09 79.07 36.07 115.40 0.00* 53. 13 31.97* 21.85* 14.09* 0.00* 32.33 30.68 50. 28 0.00* 0.00* 76.49 68.53 96.89 51.89 94. 35 120.25 152.26 49. 40 25.31* 70.27 48.24 24.19* 41.32 44.09 39.78 26.14* 32.07 4 3.12 58. 68  FC  H  84.68 67. 13 20.35 33.26 31. 19 33.07 1.60 47.72 16.91 21.63 75.26 70.25 37.72 33.44 35.65 158.65 91.16 45.24 38.95 70.73 133.54 26.53 159.90 103.10 101.94 77.27 25. 14 114.93 14.30 50.67 20.34 10.75 25.62 4.12 31.52 25.21 49.38 9.76 4.16 73.69 73.44 99.04 56.25 99. 17 123.70 158.96 52.24 12.37 72.25 39.92 26.24 36.73 47.97 32.06 31.79 31.30 39.60 64.84  13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 14 14 14 14 14 14 14 14 14 14 14 14 14 14 14 14 15 15 15 15 15 15 15 15 15 15 15 15 15 0 0 0 0 0 0 0 0 0 0 0 0 0 0  K  L  -V -10 -1 -1  -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2  -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 0 1 2 3 4 6 7 8 9 10 11 12 13 14  FO 18.29* 68.75 30.27* 13.48* 0.00* 59.13 111.44 25.96* 50.22 31.93 35.30 85. 87 70.85 92. 86 64.87 61.14 48. 30 16.00* 17.18* 36.97 67.40 32.44* 0.00* 49.33 15.08* 39.06 34.83 51.54 40. 83 59.00 92.12 25.12* 57.36 77.03 49. 15 77. 52 23.54* 42. 50 21.80* 17.90* 15.09* 33. 33 42.04 44.81 76.85 317. 16 274.32 41.47 42.83 31.67 248.81 41.84 19.02* 29.79 110.51 17.09* 16.38* 67.88  FC 23. 14 65.93 29. 18 14.55 7.67 58.71 110.59 24. 10 41.82 25.76 42.65 86.22 66.09 91.00 64.98 58.30 43.85 10.33 3.76 28.93 63.75 31.33 8.72 49.91 17.73 30.17 30.99 51.31 32. 12 44.31 88.23 15.42 61.50 71.80 43.90 73.03 28.26 44.03 8.26 25.66 10.30 17.32 28.36 43. 11 96.57 258.97 229.66 29. 19 35.48 34.52 224.42 48.31 11.73 31.97 105.78 2.63 18.56 68.04  H  K  L  FO  FC  0 -r2 15 13.64* 13.64 1 -2 -15 85.10 85.53 1 -2 -14 0.00* 2.53 1 -2 -13 89.94 89.83 1 -2 -12 20.55* 22.25 1 -2-11 98.33 101.64 1 -2 -10 80.71 80.04 1 -2 -9 64.89 58.66 1 -2 -8 200.23 198.35 1 -2 -7 88.77 80.55 1 -2 -6 38.41 41.69 1 -2 -5 158.27 142.45 1 -2 -4 92.10 98.90 1 -2 -3 185.03 165.98 1 -2 -2 92.35 94.75 1 -2 -1 367.83 307.57 1-2 0 41.30* 50.99 1 -2 1 131.57 122.06 1 -2 2 33.34 38.59 1-2 3 323.04 288.39 1 -2 4 174.89 179.60 1 -2 5 122.19 123.32 1 -2 6 16.95* 19.88 1 -2 7 309.91 277.26 1-2 8 52.20 48.01 1 -2 9 94.27 87.37 1 -2 10 9.98* 9.80 1 -2 11 141.39 1 -2 12 72.66 1 -2 13 45.91 1 -2 14 44.74 1.-2 15 27.04 2 -2 -15 21.49* 2 -2 -14 8.39* 2 -2 -13 129.60 2 -2 -12 79.65 2 -2 -11 4.37* 2 -2 -10 102.29 2 -2 -9 205.12 2 - 2 - 8 16.68* 2 -2 -7 224.40 2 -2 -6 13.69* 2 -2 -5 5.65* 2 -2 -4 77.04 2 -2 -3 66.25 2 -2 -2 163.64 2 -2 -1 128.20 2-2 0 165.49 2 -2 1 104.37 2-2 2 293.23 2-2 3 31.46 2 -2 4 106.23 2-2 6 64.19 2 -2 7 78.53 2-2 8 0.00* 2-2 9 207.51 2 -2 10 12.80* 2 -2 11 52.38  140.65 76.89 51.55 46.43 18.34 19.43 6.67 131.51 83.65 12.80 106.79 196.69 1.14 214.33 25.40 , 4.59 76.19 57.42 156.27 122.72 206.49 108.80 280.32 29.89 101.78 63.77 78.47 3.62 198.91 1.55 52.58  fl  K  L  2 -2 12 2 -2 13 2 -2 14 3 -2 -15 3 -2 -14 3 -2 -13 3 -2 -12 3 -2 -11 3 -2 -10 3 -2 -9 3 -2 -8 3 -2 -7 3 -2 -6 3 -2 -5 3 -2 -4 3 -2 -3 3 -2 -2 3 -2 -1 3 -2 0 3 -2 1 3 -2 2 3 -2 3 3 -2 4 3 -2 5 3 -2 6 3 -2 7 3 -2 8 3 -2 9 3 -2 10 3 -2 .11 3 -2 12 3 -2 13 3 -2 14 4 -2-15 4 -2 -14 4 -2 -13 4 -2-12 4 -2 -11 4 -2 -10 4 -2 -9 4-2 -8 4 -2 -7 4 -2 -6 4 -2 -5 4 -2 -4 4 -2 -3 4-2 -2 4 -2 -1 4-2 0 4 -2 1 4 -2 2 4-2 3 4 -2 4 4-2 5 4-2 6 4-2 7 4-2 8 4 -2 9  FO  FC  58.80 59.46 24.06* 29.46 24.51* 15.87 91.49 96.90 8.83* 7.13 15.41* 21. 38 11.73* 7.26 191.74 191.54 68.63 67.03 100.97 101.21 37.76 36.66 213.99 197.26 167.19 160.77 20.99 23.49 197.24 170.90 134.45 122.49 46.56 51.18 37.90 29.51 91.34 95. 19 80. 10 94.66 126.68 142.29 158.43 154.99 8.21* 14.49 84. 28 80.93 78. 35 78.26 158.77 155.41 76.44 77.04 0.00* 3. 17 8.70* 8.29 156.59 156.08 7.81* 1.86 31.11 33.94 28.84* 25.74 19.51* 11.58 22.42* 24.82 102.41 105.86 17.98* 23.07 54.78 56.99 44.00 37.75 379.25 356.75 127.80 128.06 20.69 13.22 99.77 103.34 232.80 207.13 28.42* 54.28 56.46 53.18 54.64 63.34 17.06* 18.53 0.00* 26.50 * 123.35 151.41 61.93 73.13 219.20 221.50 64.17 59.68 74.64 70.83 133.94 136.81 30.57 24.82 112.96 108.96 203.09 191.68  H  K  4 -2 4 -2 4 -2 4 -2 5 -2 5 -2 5 -2 5 -2 5 -2 5 -2 5 -2 5 -2 5 -2 5 -2 5 -2 5 -2 5 -2 5 -2 5 -2 5 -2 5 -2 5 -2 5 -2 5 -2 5 -2 5 -2 5 -2 5 -2 5 -2 5 -2 5 -2 5 -2 6 -2 6 -2 6 -2 6 -2 6 -2 6 -2 6 -2 6 -2 6 -2 6 -2 6 -2 6 -2 6 -2 6 -2 6 -2 6 -2 6 -2 6 —2 6 -2 6 -2 6 -2 6 -2 6 -2 6 -2 6 -2 6 -2  L 10 11 12 13 -15 -14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 10 11 12 -15 -14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 10  FO 26.41 27.76 20.07* 61.01 31.89 0.00* 67.85 26.65 174.98 23.67 11.48* 21.57 236.01 91.36 50. 17 85. 54 416.29 164. 19 143.13 90.44 143.51 26.52 85.09 154.02 71.78 97.53 27.84 23.06* 110.92 36. 14 69.78 34.64 33.41 6.25* 52.72 91.51 110.02 35.93 177.84 30.76 32.74 125.42 392.85 71.56 92.03 105.44 63.54 39.54 229.92 24.13* 175.95 24. 14* 124.64 0.00* 187.09 32.27 13.40* 87.25  FC  H  K  L  15.37 25.80 2.28 55.48 39.44 2.73 69.49 28.58 175.95 26.83 5.73 14.28 220.44 82.36 51.67 73.53 387.36 172.93 144.41 99.39 146.14 22.07 96.77 163.21 73.05 93.05 30.05 7.57 105.37 38.98 71.67 31.83 41.58 2. 83 53.94 91.75 109.74 38.35 173.08 37.39 19.53 123.68 341.93 71.90 81.00 96. 17 62.96 40.01 225.61 15.77 193.79 17.47 129.63 16.02 180.35 31.40 14.23 81.56  6 6 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 9 9 9  -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2  11 12 -15 -14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 10 11 - 15 -14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 10 -15 -14 -13  FO 0.00* 41.45 97.35 58.61 83.65 71.73 14.52* 33. 12 58.14 49.35 72.39 15.75* 107.89 62.96 96.06 69.36 98.20 158.92 204.38 49.03 156.17 15.21* 82.69 19.32* 149. 17 79.06 57.79 39.78 8.99* 19.64* 37.60 128.66 0.00* 121.20 27.54 106.50 53.07 116.37 90.82 103.58 80.98 49.20 159.56 32.92 39.57 181.33 43.54 34.26 18.32* 196.06 27.91* 98. 19 23.77* 47.19 16.96* 120.19 26.15* 87.59  FC 5.84 41.47 96.02 56.74 84.04 72.86 17.26 31.78 59.47 46.75 61.12 17.45 103.73 54.58 100.52 74.42 100.55 162.31 208.82 42.04 161.20 6.73 87.61 5.81 149.25 75. 18 60.89 38.75 9.25 19.86 41.90 134.95 4.42 127.04 24. 38 104.06 52.39 107.33 80. 16 93.63 77.85 43.51 155.90 35.30 43. 10 183.86 43.82 34.40 16.66 204.21 21.12 99.60 26.57 43.80 21.76 119.86 27.93 89.56  H  K  L  9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 10 10 10 10 10 10 10 10 10 10 .10 10 10 10 10 10 10 10 10 10 10 10 10 10 11 11 11 11 11 11 11 11 11 11 11 11  -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2  -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 -15 -14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 -15 -14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4  FO 22.18* 161.26 69.88 35.21 80. 18 104.32 80. 16 20.35* 49.66 84. 18 21.24* 97. 29 17.20* 15.89* 46. 20 68.44 109. 12 0.00* 13.84* 120.86 8.33* 37.26 14.25* 15.46* 131.03 22.48* 0.00* 0.00* 204.26 18.92* 112.65 46.57 115.42 47. 43 55.56 50.46 112.10 85.83 35.51 88.43 82.95 55.60 123.66 30.04* 28.10* 0.00* 57.77 35.81 24.02* 9.30* 114.96 66.37 40.38 34.16 165.56 75.72 78. 31 28.65*  FC 21.98 167.93 70.10 31.96 81.40 100.51 75.93 19.93 41.46 85.46 16.98 95.06 8.57 9. 17 47.92 66.95 116.41 25.61 4.68 117.66 5.55 31.04 7.68 11.17 135.25 23.32 10.36 17.18 203. 15 25.01 107.20 44.65 106.42 33.35 63.67 54.57 125.28 83.10 30.56 88.2 8 71.40 50.35 128.00 3.72 7.46 5.66 53.68 32.73 5.62 19.42 114.51 69.66 40. 1 1 33.52 165.51 76.87 68.59 23.90  fi  11 11 11 11 11 11 11 11 11 11 11 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 14 14 14 14 14 14 14  K  L  -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2  -3 -2 -1 0 1 2 3 4 5 6 7 -15 -14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 -14 - 13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 -13 -12 -11 -10 -9 -8 -7  FO 161.60 36.70 51.48 28.49* 83.96 42.28 18.32* 14.39* 77. 36 40.78 0.00* 35. 54 5. 11* 14.77* 41.07 42.94 44. 32 144.09 16.46* 23.99* 10.89* 85.73 60.83 31.92* 21.68* 92.92 0.00* 97.64 11.54* 136.84 41.99 18. 53* 10.05* 59.73 23.29* 10.19* 53.24 19.06* 0.00* 31.28 52.02 27.89* 48.66 90. 12 38.67 66.57 0.00* 87.67 O.OC* 63.90 26.00* 82.31 36.08 74.87 0.00* 0.00* 23.56* 20.42*  FC 161.55 25. 10 52.69 29.83 82.69 44.98 7.22 12.84 74.6 1 35.51 14.99 34.25 10.72 19.74 42.59 45.18 39. 18 146.76 12.84 22. 19 5.33 87.73 56.51 38. 13 18. 38 100.35 10. 30 97.0 1 4.60 139.80 31.51 13.68 5.55 59.4 1 23.62 16.96 51.00 16.81 6.4 1 28.64 52.64 30.08 43.85 104.80 33.89 71.07 11.14 84.31 8.44 63.71 22.76 81.67 37.96 74.50 12.22 1.58 29.48 12.96  H  K  14 14 14 14 14 14 14 14 14 15 15 15 15 15 15 15 15 15 15 15 15 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1  -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3  L -6 -5 -4 -3 -2 -1 0 1 2 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 -15 -14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6  FO 56.48 28.27* 16.82* 23.03* 0. 00* 0.00* 14.97* 85. 13 24.78* 49.00 0.00* 33.94 25.69* 69.79 31.64* 39.95 18.20* 37.49 33.50 29.68* 59.41 99.71 335.62 197.85 26.84 103.79 122.60 221.62 176.37 17.62* 77.07 18.46* 24.59* 10.36* 45.62 45.79 19.13* 123.22 48.69 67.92 19.02* 70.81 4.51* 13.92* 94. 13 10.25* 75.60 169.39 82.44 311.86 237.59 205.64 170.72 36.28 98.93 82.41 308.56 66.71  FC  H  K  53. 15 32.67 3.24 31.73 3.71 4.06 28.02 88. 19 20.86 54.50 11.93 28.96 13.12 63.65 29.63 35.82 6.54 33.69 30.40 31.94 51.95 99.94 306. 17 171.71 20.23 100.85 126.62 217.05 165.5.0 19.02 74.80 15.27 31.13 7.61 54.4 5 43.08 21.48 122.35 49.22 68. 10 10.15 73.73 3.26 11.53 90.25 11.90 73.54 162.69 87.51 280.99 212.00 229.00 160.30 45.92 100.19 91.14 279.61 66.68  1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3  -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3  L  7 8 9 10 11 12 13 14 -15 -14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 . 6 7 8 9 10 11 12 13 14 -15 -14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0  1 2 3 4  FO 20. 19* 123.66 99.26 95.67 4 1.15 104.32 14.02* 38.41 34. 87 0.00* 14.54* 34. 52 131.56 4 3.74 21.51 149.73 58.52 98.67 84.94 295.52 225. 1 1 80.61 26.98 98.47 17.12* 114.76 101.56 171.71 .0.00* 189.02 133.52 87.27 65.95 18.27* 109.67 24.19* 14.61* 47.39 32.75 55.08 106.10 27.99 39.35 115.10 151.76 22.29 20.28 125.19 23.16 223.74 39.16 223.05 17.67* 206.92 84.28 189.97 56.51 110.23  FC 15.41 130.58 91.36 98.85 41.17 103.18 5.36 42.47 32.91 10.27 13.21 32.69 135.30 39.72 17.32 148.27 55.75 86.03 88.94 269.39 205.70 74.81 18.25 95.40 5.25 97.69 97.94 166.69 4..2 2 186.83 138.99 83.40 63.89 18.69 108. 12 13.45 2.43 46.26 23.49 61.51 110.43 23.20 34.64 115. 13 150. 13 23.31 18.04 140. 16 15.58 203.20 33.41 206.21 3.71 226.72 109.00 206.64 56.55 117.76  H  K  3 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5  -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3  L  FO  5 90.78 6 73.52 7 49. 17 8 57.03 9 168.00 10 98.80 11 4.06* 12 90.21 13 15.38* -15 41.96 -14 13.53* -13 21.71* -12 50.53 -11 92.58 -10 143.64 -9 54.87 -8 87. 12 -7 239.03 -6 129.68 -5 27.59 -4 165.46 -3 99.31 -2 31.30 -1 191.84 0 149.74 1 38.21 2 145.74 3 0.00* .4 137.91 5 17.99* 6 33.80 7 77.63 8 81.62 9 13.90* 10 68.03 11 39.36 12 71.44 13 33. 1 1 -15 9.05* -14 33.90 -13 10.82* -12 114. 17 -11 21.34* -10 0.00* -9 209.61 -8 12.81* -7 20.09* -6 29.91 -5 174.67 -4 253.89 -3 38.88 -2 222.55 -1 19.55* 0 162.89 1 91.99 2 118.08 3 110.04 4 87.53  FC  H  K  L  90.38 75.24 51.91 68.92 161.98 94.40 5.59 93.04 24.87 39.52 5.74 25. 18 51. 13 96.61 148.88 57.82 84.81 237. 17 119.67 26.57 160.44 100.34 39.95 206. 10 175.24 38.54 148.79 16.53 142.71 15. 14 40.44 76.02 83.94 17.66 67.65 40.32 73.30 30.38 2.89 32.3 1 4.91 117.17 24.89 3.65 205.70 12.94 4.55 25.90 166.22 233.31 34.05 206.00 21.05 181.22 100.88 127. 17 119.64 95.83  5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7  -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3  5 6 7 8 9 10 11 12 -15 -14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 10 11 -15 -14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7  FO  FC  80.25 72.64 40.20 38.50 36.79 30.35 81.39 76.78 33.32 25.83 98. 13 101.60 28.94* 31.62 43.24 43.00 22.31* 33.42 38.62 43.29 7.06* 6.65 74.48 79.06 56.74 59.72 47.80 50. 15 40.45 4 0.70 16.52* 11.89 128.56 130.14 275.96 267.67 37.36 40.82 40.80 36.35 135.52 127.97 129.12 141.06 70.96 69.58 56. 62 67.24 142.68 141.09 73.27 82.98 187.86 210.20 102.92 108.09 2 7-. 9 6 29. 5 1 138.92 142.43 35.31 32.92 64. 21 57.59 4.70* 16.51 33.06 26.98 22.91* 22.02 12.21* 18.50 72.40 75.84 65.56 68.01 64.22 66.09 30.10 27.47 12.92* 10.94 6.32* 2.29 58.49 55.92 51.99 55.75 210.19 196.30 183.33 181.59 137.07 137.86 32.82 34.96 73.66 66.54 81.36 92.35 182. 19 195.99 128.20 136.95 132.29 137.97 19.30* 35.25 80.25 92.36 79.07 83.87 70.44 67.93 90.00 89.08  H  K  L  7 7 7 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 10 10 10 10  -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -.3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3  8 9 10 -15 -14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 1.0 -15 -14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 -15 -14 -13 -12  FO 45.31 46.67 15.34* 78.60 8.88* 20.74* 63.73 75.68 27.87 18.34* 194.60 36. 26 71.51 0.02* 43.76 39.98 111.51 22.67* 65.80 27.51* 107.89 67.00 109.76 93. 10 60.77 98.58 20. 19* 17.80* 46.77 18.87* 91.74 78.48 15.84* 30.89 48.94 93.63 82.74 36.51 88.89 61.84 34.42 100.87 212.82 36.75 113.20 0.00* 34.20 30.62* 19.31* 90.63 33.79* 6.59* 51.44 13.71* 21.02* 45. 10 41.78 7.77*  FC  H  45.45 43.84 1 1.07 81.48 11.61 20.82 70.69 85.08 24.48 8.87 200.24 41.16 67.44 12. 36 43.65 39.63 118.34 23.93 73.31 29.96 106.42 66.59 116.21 96.57 58.44 106.02 22. 18 14.76 .51.61 4. 15 93.72 87. 13 6.24 35.78 49.91 99.25 81.91 37.34 89.58 58.37 29.73 111.73 226.53 38.31 114.07 5.17 32.95 22.05 13.62 102.02 31.90 13.96 52.71 27.03 31.09 51.27 37.72 14.49  10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 11 1 1 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 1 1 11 11 11 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12  K -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 _2 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 _3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3  L  FO  -11 109.62 -10 89.48 -9 29.35 -8 107.99 -7 1 16.66 -6 12.56* 52.78 -5 -4 143.69 -3 32.04* -2 56.76 -1 43.33 0 45.56 52. 18 1 2 17.36* 3 27.93* 4 91.92 5 21.92* 6 50.95 7 24.22* 8.01* -15 -14 0.00* -13 53.24 22. 14* -12 -11 16.63* -10 33.76 -9 94.98 87.23 -8 -7 11.96* -6 38.57 -5 64.30 -4 155.59 24.59* -3 -2 87.92 -1 75.77 37.88 0 89.33 1 2 65. 25 3 41.45 4 22.55* 0.00* 5 51.39 6 -14 14.20* 0.00* -13 21.27* -12 -11 23.47* -10 103.49 -9 52.89 -8 0.00* 74.69 -7 -6 79.31 -5 " 23.94* -4 0.00* -3 73.25 -2 29.62* 70.16 -1 0 50.25 1 37.97 91.06 2  FC 114.85 92.54 38.55 108.70 118.87 10.27 55. 19 149.82 21.23 57.20 38.48 48. 18 53.80 0.38 5. 15 93.42 14.47 50.09 25.45 10.95 18.53 56.71 19.21 12.18 23.58 96.67 83.96 24.20 40.. ,7 6 64.61 166.58 15.48 98.33 85.33 33.56 89.68 70.78 37.35 19.83 2.72 40.22 15.59 8.80 24.30 23.65 111.95 52.51 8.56 80.31 87.65 14.91 18.62 79.48 32. 13 71.31 4 4. 13 37.47 89.52  H  K  12 12 12 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 14 14 14 14 14 14 14 14 '14 14 14 14 14 14 15 15 15 15 15 15 15 15 15 15  -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4  0 0 0 0 0 0 0 0 0 0 0 0 0 0  L 3 4 5 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 10 11 12 13  FO 39.74 39.69 35.95* 26.68* 44.21 18.76* 56.04 51.48 34.09 27.52* 67.68 34.81* 124.78 19.18* 38.07 32.31 85.45 37.01 18.06* 72. 38 73. 28 26.30* 32.85 27.26* 36.43 32.68* 75.26 36.92* 26.20* 26.36* 51.82 26.83* 51.39 48.42 19.66* 49. 48 29.47* 0.00* 99. 19 29.47* 25.60* 0.00* 34.17* 22.50* 368.82 147.33 181.35 46.87 140.06 17.27* 20.75* 160.17 53.95 0.00* 42.70 30. 12 62.73 22.58*  FC  H  F  33.20 34.24 40.91 35.27 49. 80 11.92 50.02 43.79 31.82 24.25 59.49 42.44 124.47 6.70 33.26 29.24 83.44 31.84 6.46 65.30 75.03 22.62 27.51 7.38 39.29 14.53 82.78 34.64 24.66 18.84 49.37 3.75 48.94 44.75 26.78 45.98 3.57 18. 32 97.51 10.43 33. 18 16.57 42.79 5.62 341.67 134.08 157.81 45.82 135.62 5.40 31.33 157.40 48. 19 15.83 47.77 31.18 57.72 18.52  0 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2  -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4  L 14 -15 -14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 -15 -14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 10 11  FO  FC  77.81 77.68 18.68* 16.25 7.34* 9.27 47.43 50.78 22.46* 17.87 74.39 67.28 21.47* 21.93 128.20 134.50 124.64 121.71 61.18 63.75 39.53 36.55 100.34 99.80 115.56 129.02 178.46 176.97 146.24 129.47 123.81 113.42 36.42* 39.47 97.77 102.62 314.07 319.79 60.95 62.17 117.49 109.03 13.57* 8.08 169.82 158.82 50.73 47.20 23.09 20. 12 19.57* 6.07 40.40 35.87 16.20* 5.16 3.17 4.0 0* 88.92 85.43 59.55 61.61 16.61 27.22* 94.65 97.22 25.99 27.98 35.44 32.40 61.57 58. 15 92.83 89.09 90.80 91.91 64.74 58.17 112.28 1 12.96 27.84 35.48 17.40* 13.01 76. 13 92.62 144.19 141.42 217.67 240.62 39.87 35.21 268.59 243.77 79.58 74.96 78.79 84.96 184.56 179.62 134.86 131.30 9.74* 8.69 38.34 32.23 45.78... 41.79 55.74 54.06 13.79 12.20* 114. 14 112.47 38.37 39.51  H  K  2 2 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4  -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4  L 12 13 -15 -14 -13 -12 -1 1 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 10 1 1 12 13 -15 -14 -13 -12 -1 1 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 10 11  FO 88. 19 15.68* 34.87 11.45* 23.90 74.08 11.58* 99.49 28.83 63.20 70.26 71.12 116.85 146. 10 195.24 13.62* 228.64 113.48 151.73 15.52* 52. 15 51.92 9.96* 152.68 24.84 71. 14 77.84 39.22 31.49 50.99 17.77* 32.66 65.81 29.90 42.60 58. 46 69. 22 9.74* 50.16 94.56 69.05 82. 11 320.43 76. 65 177.93 18.47* 38.99* 67. 26 111.88 84. 13 134.36 148.40 43.73 121.66 63.78 0.00* 61.91 14.92*  FC  H  K  89.28 16.48 30.28 6.72 16.46 75.80 4.54 102.54 24.93 64.24 73.44 69. 18 104.26 122.56 185.25 13.73 225.76 134.79 167. 14 8.23 49.39 38.47 3.54 155.37 24. 15 79.91 76.73 36.61 29.00 58.60 3.77 32.92 68.6 1 26. 13 43.01 63.22 71.33 5.06 51.74 96.66 74.33 .89.87 306.85 73. 16 159.28 5.68 37.38 68.63 109.05 90.84 130.21 144.07 35. 10 117.79 58.75 5.40 68.94 10.53  4 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6  -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4  6  6 6 6 6 6 6 6 6 6  7 7 7  L  12 -15 - 14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 10 11 -15 - 14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 10 11 -15 -14 -13  FO 32.29 7.08* 21.21* 33. 17 20.25* 24.96 62. 34 0.00* 66.60 29. 86 247.39 109.95 59.63 22.28* 138.38 100.38 83.36 82.85 99. 12 144.37 105.89 64. 96 29.35 32.42 31.77 52.73 0.00* 27.32* 6. 10* 0.00* 7.47* 64.88 113.65 13.84* 0.00* 66.09 137.57 105.52 50.97 205.87 62.80 101.57 18.89* 240.72 22.16* 82.89 57.66 23.24* 15.22* 43.31 28.94 30.74 63. 88 31.30 46. 13 28.55 27.91 85.01  FC 20.97 13.75 19.16 36.63 18.96 13.75 67.54 1.74 71.53 3 5.68 230.85 110.08 54.36 18.94 145.88 104.88 93.79 88.71 115.08 151.81 108.5 3 72.24 38.34 31.54 29.22 50.87 18.45 26.28 11.15 2.39 14.01 62.42 120.39 21.21 1.90 61.78 140.28 101.61 48.87 189.87 63.92 107.33 8.03 265.91 29.20 92. 17 58.69 24.70 17.57 44.85 34.96 34.06 62.77 37.00 41.59 30.69 29.32 89.63  H 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 •8 9 9 9 9 9 9 9 9 9 9  K -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4  L -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 10 -15 -14 -13 -12 -11 -TO -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 -15 -14 -13 -12 -11 -10 -9 -8' -7 -6  FO 53.22 15.13* 18.47* 55.04 73.86 56.73 91.05 116.02 1 1.86* 22.24* 185.71 130.90 43. 47 7. 11* 132.86 61.07 19.45* 10.50* 90.87 31.09 19.93* 59.57 54.62 14.40* 92. 06 0.00* 15.25* 26. 14 26.41 10.77* 45. 22 165.10 132.50 23.41* 86.84 110.54 122.29 103.47 140.98 33.89 59.94 0.00* 73.36 32.25 .36.20 22.28* 64.13 0.00* 23.23* 15.39* 6.35* 45.48 68. 30 47.89 53.06 146.61 42.29 43.89  FC 57.36 22.81 4.96 50.98 74.55 56.46 96.94 1 17.32 15.63 14.94 176.70 145.04 52.39 6.48 127.00 68.37 2.13 12.0 1 85.21 21.72 9.96 54.64 57.55 11.88 92.53 8.66 6.68 22.36 24.03 7.08 44.29 158.65 126.59 25.03 88. 63 1 17.96 129.33 110.51 151.75 36.24 58.32 2.63 82.22 36.38 40. 82 26.42 56.84 2.00 22.74 20.3 4 12.59 49.94 65.26 51.42 48.31 150.96 40.92 41.33  H  K  L  9 9 9 9 9 9 9 9 9 9 9 9 9 9 10 10 10 10 10 10 10 10 10 10 10 10 10 10 TO 10 10 10 10 10 10 10 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 12 12  -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4  -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 -14 -13 -12 -11 -10 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 -14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 -13 -12  FO 72.99 98. 59 87.88 11.23* 97.06 39.97 3.70* 78. 14 66.74 74.03 60.64 44.55 0.00* 37.75 52.41 20.89* 0.00* 24.51* 59.52 34.39 121.83 34.94 73.91 15.21* 94.98 68.98 120.89 11.04* 54.30 93.07 52.98 82.25 22.31* 39.40 23.91* 17.13* 22.76* 19.23* 22.50* 18.02* 96.84 61.26 39.02 41.50 90.53 0.00* 84.03 44.06 68.65 68.75 54.64 27.45* 52.71 22.13* 4.29* 13.20* 19.04* 14.57*  FC 68.92 97. 16 87.07 13.56 101.95 35.42 21.80 82.93 64.85 72.30 52.91 48.02 7.98 35.09 59. 10 1G.45 3.74 18.68 58.66 37.74 126. 13 31.82 82.00 21.25 102.36 67.94 129.9 1 20. 37 52.42 98.76 53.97 86.35 4.72 39.08 17.64 5. 13 18.09 23.89 16.71 2.92 95.05 61.43 42.15 42.20 94.01 4.42 90.95 44.73 74. 12 72.21 48.03 26.72 57.86 21.50 20.04 2.53 6.49 17.22  H K L 12 -4 -11 12 -4 -10 12 -4 -9 12 -4 -8 12 -4 -7 12 -4 -6 12 -4 -5 12 -4 -4 12 -4 -3 12 -4 -2 12 -4 -1 12 -4 0 12 -4 1 12 -4 2 12 -4 3 12 -4 4 13 -4 -12 13 -4 -11 13 -4 -10 13 -4 -9 13 -4 -8 13 -4 -7 13 -4 -6 13 -4 -5 13 -4 -4 13 "4 -3 13 -4 -2 13 -4 -1 .13 -4 .0 13 -4 1 13 -4 -112 14 -4 14 -4 -10 14 -4 -9 14 -4 -8 14 -4 -7 14 -4 -6 14 -4 -5 14 -4 -4 14 -4 -3 14 -4 -2 14 -4 -1 14 -4 0 15 -4 -8 15 -4 -7 15 -4 -6 15 -4 -5 105 -4 -4 -5 1 0 5 2 0 5 3 0 5 4 0 5 5 0 5 6 0 5 7 0 5 8 0 5 9 0 -5 10  FO FC 68. 38 69.64 12.88* 8.69 16.52* 5.16 57.24 56.00 41.51 29.42 24.79* 19.25 0.00* 14.03 153.80 156.62 32.92* 29.99 52.63 68.30 24.61* 9.53 60. 14 60. 15 0.00* 1 .87 24.98* 18.30 33.13 24.96 24.20* 17.23 37.23 37. 10 25.40* 22.40 38.75 30.66 50.59 46.66 12.13* 11.23 20.36* 7.63 92.61 96.39 110.00 109. 10 17.27* 8.46 0.00* 5.57 55.66 59.91 13.87* 3.24 23.89* 16.81 17.50* 3.71 62.25 62.44 48.47 48.00 43.87 40.91 11.62* 17.27 15.66* 2.85 63.15 64.92 68.67 71.64 34.12* 15.32 58.32 60.95 27.15* 31.18 18.59* 12.25 25.36* - 8.29 70.70 69.47 66.04 71.23 28.25* 18.88 0.00* 9.49 59.54 58.96 40.05 27.68 128. 16139.97 180.36 184.42 75.80 67.41 0.00* 5.28 57.08 64.73 0.00* 9.53 22.62* 17.48 37.52 36.59 123.81 129.89 15.00* 5.63  H K L FO FC 0 -5 11 20.31* 27. 16 0 -5 12 35.30 32.79 0 -5 13 101.92 98.39 1 -5 -14 29.34 21.19 1 -5 -13 36.72 39.87 1 -5 -12 14.25* 7.00 1 -5 -11 73.30 75.45 1 -5 -10 27.10 22. 19 1 -5 -9 79.49 88.63 1 -5 -8 83. 16 87.00 1 -5 -7 178.41 171.09 1 -5 -6 51.26 58.22 1 -5 -5 96.81 92.46 1 -5 -4 71.75 70.38 1 -5 -3 187.98 186.39 1 -5 -2 25.61 26.06 1 -5 -1 48.29 46.92 1 -5 0 1 16.40121.48 1 -5 1 83.39 88.44 1 -5 2 25.37 14.95 1 -5 3 70.09 77.91 1 -5 4 112.23 103.31 1 -5 5 111.97 115.58 1 -5 6 .11.52* 22.61 1 -5 7 159.50 162.95 1 -5 8 15.71* 25.03 1 -5 9 65.72 66.03 1 -5 10 50.87 56.59 1 -5 11 52.0.9 ..59.4 3 1 -5 12 20.00* 9.11 1 -5 13 5. 19* 3.87 2 -5 -14 6.46* 4.88 2 -5 -13 41.86 41.23 2 -5 -12 26. 11 21.59 2 -5 -11 26.38 30.6 1 2 -5 -10 27.63 23.63 2 -5 -9 1 12.91119. 19 2 -5 -8 62.51 66.28 2 -5 -7 22.21 27.51 2 -5 -6 94.54 105.82 2 -5 -5 171.16 165.71 2 -5 -4 42. 11 35.54 2 -5 -3 163.31 170.32 2 -5 -2 17.45* 3.36 2 -5 -1 151.10 148.33 2 -5 0 28.78* 40.61 2 -5 1 12.23* 19.69 2 -5 2 152.55 150.78 2 -5 3 132.73 139.58 2 -5 4 37.49 29.75 2 -5 5 7.23* 4.51 2 -5 6 44.28 43.27 2 -5 7 104.81 110.91 2 -5 8 42.19 42.83 2 -5 9 35.69 32.94 2 -5 10 17.18* 10.74 2 -5 11 41.51 44.04 2 -5 12 37.06 41.61  H  K  L  2 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 5 5 5 5 5  -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5  13 -14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 10 11 12 -14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 6 7 8 9 10 11 -15 -14 -13 -12 -11  FO 59.41 36.77 19.44* 17.70* 20.21* 14. 19* 132.57 57.28 158.51 17.76* 102.01 112.04 106.73 34.76 0.00* 5.97* 99.48 9.65* 182.58 71.15 170.60 5.72* 71.72 28.09 47.68 6.47* 37.19 16.42* 23,31* 0.00* 71.67 94.42 9.56* 13.51* 31.21 31.05 103. 15 12.71* 0.00* 101.49 96.88 150.00 70.95 172.43 45.92 68.05 70.84 45.46 48.36 26.35 52.89 12.48* 82.67 25.01* 40.09 32.49 8.39* 129.87  FC  H  57.58 34.26 11.73 6.07 20.05 21.86 134.10 61. 14 157.30 13.69 100.66 120.16 101.34 20.98 10.71 27.69 104.52 3.4 3 188.14 69.08 166.78 8.03 67.92 28.62 52.58 3.05 35.99 8.32 8.76 10.85 75.70 104.27 2.53 3.46 29.30 31.28 102.09 4.21 7.00 96.97 84.90 151.89 82.46 198.76 48.07 71.78 73.41 50.69 49.90 22.33 60.05 14.28 83.68 35.32 42.43 27.60 0.21 132.89  5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 7 7 7 7 7 7 7 7 7 7 7 7 7  K  -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5  L -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 10 11 -15 -14 -12 -11 -10 -9 -8 -7 -6 ' -5 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 10 -14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2  FO 64.44 24.89 14.63* 35.27 1 19.45 129.15 88.69 48.01 80.66 97.94 71.91 29.95* 1 15.28 14.31* 69.78 32.52 118. 10 26.47* 81.79 23.87* 46.72 15.73* 0.00* 24.28* 34.80 57.73 34. 10 43.59 50.03 26.65* 118.16 54.56 166.57 93.36 48.02 66.13 25.02* 51.93 4.43* 105.36 25.49* 20.83* 42.57 89.02 22.06* 8.63* 29.66 34.22 106.76 19.21* 29.66 27.58 193.64 14.30* 35.87 47.30 45.20 27.1 1*  FC 74.36 29.90 12.35 28.87 116.20 123.34 78.22 39.94 83.39 109.59 76.04 33.27 122.67 5.08 77.81 28.79 120.73 2 1.14 79.66 13.65 45.66 9.28 5.89 31.99 38.35 61.11 32.80 43.95 54.92 26.43 120.83 52.82 173.31 97.51 53.26 67.94 28. 12 52.66 10.30 108.89 18.85 22.57 48.73 84.52 14.49 4.75 33. 12 39.23 111.18 12.99 33.87 20.20 184.79 7.55 29.30 49.41 41.61 27.30  H  K  L  FO  7 7 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 10 10 10 10 10  -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5  -1 0 1 2 3 4 5 6 7 8 9 -14 -13 -12 -11 -10 -9 -8 -7 -4 -3 -2 -1 0 2 3 4 5 .6 7 8 -14 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 -13 -12 -11 -10 -9  1  33.68* 80.41 82.28 36. 11 62.58 53. 36 91.96 21.16* 59.95 23.94* 20.51* 17.86* 86.87 4.07* 15.49* 40.76 100.08 21.87* 52. 38 23.64* 27.75* 65.54 147.63 41.58 66.82 101.12 20.28* 34. 37 15.64* 31.84* 7.04* 28.32* 59. 10 24.63* 36.88 29.93 69.58 74. 11 104.03 0.00* 27.35* 13.72* 99.05 27.86* 81.34 28.22* 99.95 27.03* 60.30 40.28 82.33 0.00* 40.55 6.72* 24.02* 31.43 27.36* 20.05*  FC 33.49 93.59 93. 17 35.54 78.45 55.43 95.47 32.70 68.08 3.59 23.75 6.93 88.45 6.74 8.65 35.71 109.76 4.45 56.07 5.61 23.89 70.28 163.08 43.83 75.31 102.30 12.18 28.86 3.47 35.26 22.00 26.86 62.89 22.3 1 37.09 25.57 73.91 76.34 104.59 6.49 28.00 21.62 99.84 19.89 94.01 23.76 100.15 26.46 68.65 31.50 91.50 15.01 39. 89 8.04 31.44 33.64 30.72 15.56  H  K  10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 13 13 13 13 13 13 13 13 13 13  -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5  L  FO  FC  -8 0.00* 6.36 -7 28. 13 30.03 -6 76.93 74.59 40.91 44.60 -5 -4 49.20 50. 19 -3 110.55 113.83 32.79* 46.00 -2 66.28 -1 59.82 0 28.28* 11.39 1 31.85* 38.55 35.28 2 24.28 3 54.30 62.02 4 45.71 36.89 28.97* 35.29 5 6 0.00* 2.30 -13 19.32* 26.53 18.34 -12 24.62* -11 37.00 44.18 -10 32.00 24.49 82.24 86.4 1 -9 38.07 -8 34.71 15.40 -7 22.37* 38.44 -6 39.22 35.28 39. 10 -5 -4 73.69 73.63 39.41 -3 29.42 -2 24.92* 12.37 40.24 -1 32.81 0 30.73* 22.7 1 20.10* 25.39 1 8.80* 5.97 2 3 100.56 99.40 2.64 4 10.43* 6.77* 20.20 -12 -11 51.86 47.45 -10 11.79* 14.79 -9 50.97 54.53 -8 13.72* 5.23 -6 40.62 45. 15 66.93 70.47 -5 -4 31.59* 33.70 45.24 46.77 -3 41.88 38. 10 -2 -1 9.36 19.20* 0 20.59* 31.26 64.09 1 59.16 15.69 2 14.16* 3 0.00* 3.63 94.34 -11 89.12 -10 25.47* 8.40 -9 • 34.04 31.45 0.00* 13.19 -8 -7 48.68 44. 17 34.73* 20.99 -6 16.79 -5 34.55* -4 27.55* 26.85 -3 43.96 37.35 28.55* 28.21 -2  H  K  13 13 13 14 14 14 14 14 14 14 0 0 0 0 0 0 0 0 0 0 0 0 0 1 1 1 1 1  -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6  1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2  L -1 0 1 -8 -7 -6 -5 -4 -3 -2 0 1 2 3 4 5 6 7 8 9 10 11 12 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 10 11 12 -13 -12 -11 -10 -9 -8 -7 -6 -5  FO 17.99* 33.75* 78.79 8.50* 22.81* 23.90* 91. 38 0.00* 25.49* 37. 11 78.57 17.46* 78.48 59.40 15. 11* 122.47 64.77 100.57 45.52 24.54* 36. 36 44.82 75. 22 25.18* 47.49 21.44* 11.26* 115.48 131. 15 24.71 111.13 75.05 47.87 0.00* 7.63* 28.68 0.00* 60.32 81.33 135.31 54. 17 15.98* 85.59 75. 17 63.05 49.23 36. 18 15.67* 40. 39 33.55 30.83 59.75 47.44 102.44 69.48 77.28 83.29 33.73  FC  H  16.86 42.80 78.23 11.32 3.70 5. 18 88.75 8.10 9.30 33.49 71.71 20.58 78.62 61.77 6.82 117.76 66.50 106.49 45.83 22. 17 36.88 47.70 74.61 27.71 42.93 20.88 16.68 114.44 132.28 23.46 116.05 76.23 42.65 3.71 20.07 23.67 36.49 54.29 82.81 136.24 55.35 - 6.09 83.76 75.47 63. 13 49.00 43.94 3.98 39.92 35.22 30. 14 54.08 47.98 103.62 66.32 78.23 76.35 33.38  2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 4  4 4 4 4 4 4 4 4 4 4 4 4 4 4 4  K  L  -4 -3 -2 -1 0 1 2 3 4 5 6 7 8 9 10 11 12 -13 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 D -2 -6 -1 -6 0 1 -6 -6 2 -6 3 4 -6 -6 5 -6 6 -6 7 8 -6 -6 9 -6 10 -6 11 -6 -13 . -6 -12 -6 -11 -6 -10 -6 -9 -6 -8 -6 -7 -6 -6 -6 -5 -6 -4 -6 -3 -6 -2 -6 -1 0 -6 -6 1 -6 2 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6  FO 10.48* 74.07 202.02 16.85* 33.65* 75.79 74. 18 1 17.41 20.40* 89.76 21.41* 19.60* 18.87* 70.01 18.91* 40.55 52.94 9. 86* 19.49* 93.43 23.15* 13.33* 100.75 32.64 63. 53 90.05 134.85 58.73 / J . Oo  41.28 47.41 73. 30 60.69 32.45 154.58 15.12* 0.00* 107.92 41.93 12.37* 33.83 55.04 29.25 33.38 24.11* 19.88* 80.05 19.39* 86.84 9.56* 109.06 20.83* 27.09 128.55 17.11* 21.51* 33.26 117.58  FC 9.03 67.7 1 182.14 8.61 35.05 80.55 74.64 109.94 5.08 90.23 22.40 21.50 19.10 75. 17 13.07 40.68 51.85 6.92 16.78 93.00 26. 17 17.22 106.87 34.46 61.01 91.34 127.05 47.05 6 3.57 35.79 59.14 87.90 66.07 25.81 159.53 23.08 4.79 109.91 41.57 12.71 27.98 51.25 33. 19 35.95 27.87 24.07 84.24 24.56 80.56 12.96 105.78 6.22 22.68 128.83 18.91 13.38 15.09 123.28  H  K  4 1 4 4 4 4 4 4 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5  -6 -6 . -6 -6 -6 -6 -6 -6 -6 -6 -6 -6  L  3 4 5 6 7 8 9 10 -13 -12 -11 -10 -6 -9 -6 -8 -6 -7 -6 -6 -6 -5 -6 -4 -6 -3 -6 -2 -6 -1 -6 0 -6 1 -6 2 -6 3 -6 4 -6 5 -6 6 -6 7 -6 8 -6 9 -6 10 6 -6 -13 6 -6 -12 6 -6 -11 6 -6 -10 6 -6 -9 6 -6 -8 6 -6 -7 6 -6 -6 6 -6 -5 6 -6 -4 6 -6 -3 6 -6 -2 6 -6 -1 6 -6 0 6 -6 1 6 -6 2 6 -6 3 6 -6 4 6 -6 5 6 -6 6 6 -6 7 6 -6 8 6 -6 9 7 -6 --13 7 -6 --12 7 -6 --11  FO  FC  75.03 73.82 0.00* 5.97 85.99 92.28 56.90 50.77 80. 19 80.55 33.61 36.74 51.86 51.68 65.98 67.69 37. 32 38.28 48.78 52. 18 63.59 61.03 82.83 87.78 19.90* 16.28 12. 1 1* 17.85 105.52 102.92 26. 34 25.97 13.98* 20.59 61.43 60.70 0.00* 22.26 56.72 64.31 21.12* 4.48 17.81* 3.32 53.83 62.96 40.37 47.62 17.60* 6.55 89. 66 93. 34 106.47 106.68 37. 12 38.46 11.86* 12.43 86.76 88.25 30.30* 25.56 9.36* 4.00 14.08* 9.30 82.98 83.76 88.60 87.70 14.54* 19.88 56.63 52.33 21.52* 20.66 53.01 56. 10 73.86 69.00 40.97 40.08 62. 50 57.23 24.76* 15. 1 1 9.89* 24.65 45.00 46.71 23.91* 11.45 96.23 96.98 61. 20 62.78 65.93 67.34 20.19* 6.23 36.21 41.23 31.76* 29.52 45. 20 45.95 52.96 54.82 45.46 43.64 82.72 76.99 57.27 59.70 7.47* 12.24  H 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9  K  L  FO  FC  -6 - 10 75.80 75.41 -6 -9 66.82 66.89 -6 -8 82. 35 84.42 -6 -7 39. 20 35.56 -6 -6 103.29 102.92 -6 -5 31.23 31.67 -6 -4 39.54 28. 17 -6 -3 59.21 55. 19 -6 -2 5.35* 23.72 -6 -1 86. 21 91.01 -6 0 49.28 62. 18 -6 1 16.97* 11.78 -6 2 4.44* 21.14 -6 3 68. 45 75.05 -6 4 13. 48* 14.85 -6 5 42.49 40.88 -6 6 43.95 46.69 -6 7 26.12* 22.08 -6 8 63. 33 54. 16 -6 -13 59.56 60.48 -6 -12 62.07 62. 11 -6 -11 54.88 54.94 -6 -10 30.75 27.28 -6 -9 4.06* 3.53 -6 -8 42.60 46.29 -6 -7 65.21 69.29 -6 -6 96.59 89.67 -6 -5 28.70* 26.28 -6 -4 46.08 37* 56 -6 -3 48.00 52.82 -6 -2 100.79 99.93 -6 -1 52.53 55.07 -6 0 36.82 49.60 -6 1 51.42 52.28 -6 2 36.87* ' 31.08 -6 3 19.81* 17.35 -6 4 22.12* 21.49 -6 5 69.36 82. 14 -6 6 31.62* 27.80 -6 7 46.71 41.43 -6 -13 13.38* 17.60 -6 -12 23.61* 19.00 -6 -11 34.43 40.42 -6 -10 0.00* 2.7 1 -6 -9 70.58 69.77 -6 -8 73.37 72.99 -6 -7 35.08 35.29 -6 -6 87.30 89.43 -6 -5 43. 89 38.93 -6 -4 34.18 41.23 -6 -3 • 37.02 35.10 -6 -2 18.74* 13.63 -6 -1 33.02* 24.74 -6 0 79.17 83. 12 -6 1 26.07* 17.26 -6 2 18.03* 18.72 -6 3 77.27 86. 19 -6 4 81.52 79.06  H 9 9 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 12 12 12 12 12 12 12 12 12 12 12 12 13 13 13 13 13 13 13 0 0 0 0 0  K  L  -6  5 6 -12 -11 -10 -9 -8 -7  -6 -6 -6 -6 -6 -6 -6  -6 -6 -6 -5 -6 -4 -6 -3 -6 -2 -6 -1 -6 0 -6 1 -6 2 -6 3 -6 4 -6 -11 -6 -10 -6 -9 -6 -8 -6 -7 -6 -6 -6 -5 -6 -4 -6 -3 -6 -2 -6 -1 -6 0 -6 1 -6 2 -6 3 -6 -10 -6 -9 -6 -8 -6 -7 -6  -6 -6 -6  -6 -6 -6  -6 -6 -6  -6 -6 -6 -6 -6 -7 -7 -7 -7 -7  -6  -5 -4 -3 -2 -1 0 1 -8 -7 -6  -5 -4 -3 -2 1 2 3 4 5  FO 38.31 36.55 13.79* 29.27 7.03* 77.68 25.47* 22.12* 25.27* 0.00* 23.81* 0.00* 86.38 43.21 34. 39 4 4.33 34.94* 71.93 27.64* 58. 54 55.40 18.64* 35.92 30. 60 27.49* 0.00* 0.00* 38.71* 10.7 8* 21.99* 0.00* 64.7428.25* 0. 00* 0.00* 36.80 35.90 25. 19* 38. 19 28.84* 22.88* 36.37* 18.80* 24.31* 24.06* 47.25 27.84* 32.09* 30.07* 33.99* 21.03* 8.76* 25.38* 52.93 49.36 87. 14 25.54 36.45  FC  H  27.43 34.98 15.70 22.06 2.97 75.39 11.12 19.48 22.31 13.11 3.98 4.4 1 87.80 42.03 32. 14 40.20 42.4 1 70.65 9.99 58.59 59.21 9.89 31.50 21.50 16. 82 9.40 7.38 45.45 14.24 10.27 21.18 56.64 27.79 3.31 16.48 40. 15 31.71 7.51 37.52 32. 12 30.38 43.79 17.76 22.97 6. 65 39.93 20. 17 30.26 33.64 37.59 18.49 5.12 2.36 48.38 52.21 82. 38 21.80 31.48  0 0 0 0 0 0 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3  K  L  FO  -7 6 79.01 -7 7 13.99* -7 8 78. 16 -7 9 35.74 -7 10 47.49 -7 11 22.64* -7 -12 54. 38 -7 -11 17.24* -7 -10 43.87 -7 -9 14.60* -7 -8 46.04 -7 -7 38.32 -7 -6 85.17 -7 -5 46.01 -7 -4 29.09 -7 -3 10.63* -7 -2 165.21 -7 -1 17.30* -7 0 1 11.67 -7 1 21.84* -7 2 22.06* -7 3 0.00* -7 4 46.37 -7 5 20.40* -7 6 27.47 -7 7 12.82* -7 8 22.70* -7 9 58.28 -7 10 0.00* -7 11 2.59* -7 -12 36.06 -7 -11 35.49 -7 -10 13.26* -7 -9 17.01* -7 -8 108.64 -7 -7 3.69* -7 -6 51.17 -7 -5 46.77 -7 -4 123.34 -7 -3 52.87 -7 -2 69.75 -7 -1 122.51 -7 0 81.40 -7 1 11.96* -7 2 20.46* -7 3 13.00* -7 4 83.58 -7 5 16.20* -7 6 46.23 -7 7 77. 16 -7 8 28.96 -7 9 0.00* -7 10 36.92 -7 -12 20.68* -7 -11 21.66* -7 -10 51.08 -7 -9 24.01* -7 -8 10.40*  FC 83.67 21.05 75.97 38.31 44.17 29.71 55.25 11.79 44.50 2.50 45.18 36.47 89.78 46.41 19.24 7.06 158.59 2.88 113.86 3.61 20.71 10.46 48.73 3.38 22.90 6.03 22.89 55.59 2.88 2.25 31.40 34.42 8.48 8.97 107.40 6.60 55.27 36.92 121.84 53.30 62.85 110.52 97.47 12.31 12.60 4.54 88.94 16.55 50.71 78.06 21.22 8.98 38.22 2.37 27.23 50.03 22.14 17.06  H  K  L  3 -7 -7 3 -7 -6 3 -7 -5 3 -7 -4 3 -7 -3 3 -7 -2 3 -7 -1 3 -7 0 3 -7 1 3 -7 2 3 -7 3 4 3 -7 3 -7 5 6 3 -7 3 -7 7 8 3 -7 9 3 -7 3 -7 10 4 -7 -12 4 -7 -11 4 -7 -10 4 -7 -9 4 -7 -8 4 -7 -7 4 -7 -6 4 -7 -5 4 -7 -4 4 -7 -3 •4 4 -7 -1 4 -7 0 4 -7 1 4 -7 2 4 -7 3 4 4 -7 4 -7 5 4 -7 6 7 4 -7 4 -7 8 4 -7 9 5 -7 -12 5 -7 -11 5 -7 -10 5 -7 -9 5 -7 -8 5 -7 -7 5 -7 -6 .5 -7 -5 5 -7 -4 5 -7 -3 5 -7 -2 5 -7 -1 0 5 -7 1 5 -7 2 5 -7 5 -7 3 4 5 -7 5 -7 5 —  /  —  FO 0.00* 49.42 0.00* 38.86 69.53 185.20 52.88 34.18* 17.12* 120.09 25.68* 35.55 17.26* 39.54 32.76 16.93* 3.49* 54.78 2.92* 36.77 50.54 11.62* 36.53 61.74 18.35* 43. 16 108.19 88.58 18.50* 47. 32 89.06 11.54* 22.12* 63.75 107.40 19.77* 11.90* 4 0.40 63.9 1 31.02 55. 10 17.06* 17.94* 22.62* 16.75* 31.46 29. 16 10.86* 74.84 22.19* 72.39 22.38* 37. 17 37.92* 98.81 37.28 12.99* 11.14*  FC 11.40 48.03 3.45 34.55 64.30 175.59 52.92 33.34 2.86 124.90 21. 10 29.07 8. 14 42.22 26. 30 20. 18 11.99 52.27 8.20 30.77 50.29 17.44 38.47 57.76 22.61 39.68 105.40 80.23 1 8.0 0 40. 86 99.23 4.48 23.90 72. 31 116.00 20.60 17.55 38. 12 68.74 31.16 58.53 3.29 2.11 15.68 22.72 30.96 23.90 12.67 75. 16 2.22 71.90 21.30 45.46 46.54 110.08 41.88 3.48 8.70  H  K  5 5 5 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 7 7 7 7 7  -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7  i  — /  1  -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7  —*  7 7 7 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 8 8 8 8 8 8 3 8  -T  L 6 7 8 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 -12 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 -11 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4  FO 44.89 27.95* 37.51 43.73 26.14* 72. 31 0.00* 56.91 87. 32 88.98 47.90 15.53* 17.83* 29.76* 0.00* 0.00* 65.60 31.84* . 43.03 38.20 41.84 42. 59 0.00* 61.63 20.23* 31.20 29.93 43.91 20.91* 92. 31 0.00* 75.79 25.79* 63.02 22.02* 67.26 22.28* 25.04* 21.64* 19.74* 36.73 13.22* 20.48* 31.95 34. 83 93.37 23.29* 83.78 45.71 61.66 36.31* 59.50 35.49* 58.83 33.39* 37.78* 55.52 33.69*  FC 45.31 1.01 41.75 43.33 21.92 69.38 1.38 55.91 81.64 87.89 42.26 3.33 7.21 32.95 12.17 12.31 58.27 43.41 50.89 43.16 44. 36 38.86 0.51 64.77 7.10 35.43 25.04 44.30 10.35 90.78 6.29 77.26 22.06 64.54 9.66 78.57 6.45 15.14 8.09 12.92 35.06 6.65 28.95 18.33 36.87 92.33 14.54 76.32 44.84 65.48 40.37 46.24 41.32 68. 12 34.38 32.97 55.70 43.59  H  K  8 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 10 10 10 10 10 10 10 10 10 10 10 10 10 11 11 11 11 11 11 11 11 11 11 12 12 12 0 0 0 0 0 0 0 0 0 0 1 1 1 1 1  -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8  L  5 -11 -10 -9 -8 -7 -6 -5 -4 -3 , -2 -1 0 1 2 3 4 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 i 2 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 -6 -5 -4 0 1 2 3 4 5 6 7 8 9 -10 -9 -8 -7 -6  FO 25.15* 14.94* 28.50* 0.00* 0. 00* 35.55 83.28 9.83* 24.08* 0.00* 103.50 33.09* 49.63 17.53* 49.00 0.00* 0.00* 38.06 27.83* 56.90 23.03* 26. 16* 0.00* 61.13 26.53* 0.00* 66.56 60.24 1.2.9 0* 5.56* 0.00* 46.98 19.77* 0.00* 24.87* 22.25* 30.83* 58.58 26.81* 0.00* 51.52 37.51 0.00* 47.83 42.74 36.22 22.26* 31.84 15.62* 41.43 83.50 24.07* 24.95* 31.12 36.72 29.70 12.04* 12.88*  FC  H  1. 16 14.19 26. 15 5.93 4.72 26.82 80. 19 10.08 24.36 4.06 1 10.42 4.38 56.31 12.04 49.90 1.70 2.57 40.58 23.87 52.87 1.49 9.65 12.26 58.74 19.27 14.65 68.91 61.03 14.08 8.25 6.46 39. 32 0.68 7.00 14.89 36.02 28.32 62. 13 8.04 8.68 47.64 26. 14 8.99 53.74 35.52 27.08 22.57 35.70 13.88 39.33 •78.92 17.53 24. 10 27.30 34.54 24.11 6. 19 3.50  ! 1 1 1 1 1 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 4 4 4 4  K  L  -8 -5 -8 -4 -8 -3 -8 -2 -8 -1 -8 0 -8 1 -8 2 -8 3 4 -8 -8 5 6 -8 -8 7 -8 8 9 -8 -8 -10 -8 -9 -8 -8 -8 -7 -8 -6 -8 -5 -8 -4 -8 -3 -8 -2 -8 -1 -8 0 -8 1 -8 2 3 -8 -8 4 -8 5 -8 6 7 -8 -8 8 -8 9 -8 -10 -8 -9 -8 -8 -8 -7 -8 -6 -8 -5 -8 -4 -8 -3 -8 -2 -8 -1 -8 0 -8 1 -8 2 -8 3 4 -8 -8 5 -8 6 -8 7 -8 8 -8 -10 -8 -9 -8 -8 -8 -7  FO  FC  49. 89 45.45 70.50 68.22 57. 19 60.20 41.22 4 1.14 135.47 124.29 44.29* 39.79 21.29* 23.06 62.74 60.93 18.43* 8.94 5.87* 12.77 47.70 42.26 19.02* 12.18 0.00* 8.76 0.00* 5.25 8.93* 15.80 22.52* 20.22 25.07* 27.78 9.93* 3.72 90.32 88.22 54.43 51.81 34. 87 32.02 0.00* 1.66 88.72 81.60 95.12 78.86 53.08 45.19 47.81* 36.86 36. 24 40.73 27. 29* 43.00 27.46 3.1.56 7. 25* 18.92 62.21 67.99 18.82* 10.95 16.30* 21.13 3.44* 2.42 0.00* 7.45 13.39* 14.80 44.53 38.73 24.41* 11.90 21.98* 16.86 1 1.46 8.93* 16.01* 3.01 77. 12 67.65 87.4-1 83.43 26.71* 1.39 101.87 101.65 76.85 87.66 32.48* 40.72 12.79* 31.86 85.26 79.13 31.48 28. 10 22.19* 15.83 6.86* 2.26 21.58* 15.85 27.77* 26.24 16.54* 2.64 37.44 40.48 0.00* 12.66 0.00* 5.71  H  K  L  4 4 4 4 4 4 4 4 4 4 4 4 4 4 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 7 7 7 7 7 7 7 7 7 7 7  -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8  -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1 0  FO 16.33* 18.77* 4 7 . 31 62.05 65.86 48.52 28.79* 45.68 57.59 8 3 . 30 30.04* 44.46 28.23* 8.87* 0.00* 24.73* 20.87* 8.60* 37.31 31.32 9.53* 70.89 32.15* 30.95* 4 6.11 7 9 . 38 27.81* 48.57 30.76* 2 2 . 4 1* 6.51* 2 8 . 39 7.71* 3 2 . 10 57.96 38.03 36.69 5 0 . 34 34.47 0.00* 0.00* 44.50 39.53* 34.88* 53.93 22.64* 31.30* 17.38* 36.43 31.71 24.03* 30.36* 95.03 51.25 19.07* 52.30 45.40 16.21*  FC  H  K  18.32 23.62 35.27 56.95 6 6 . 13 43.90 8. 1 7 30.05 55.09 93.67 18.68 43.25 30.33 19.50 9.99 1 9 . 84 13.03 20.47 37.55 35.73 6.70 71.81 3 8 . 19 9.40 62.26 74.34 1 1.28 55.20 31.47 9.90 9.61 1 9 . 16 8.41 21.78 52.67 32.76 33.76 4 6 . 80 19.35 8.71 7.20 37.80 "17.88 30.88 58.77 6.52 2 0 . 17 8. 8 5 33.37 38.65 29.52 28.00 87.93 46.36 15.46 59.56 5 3 . 18 5.04  7 7 7 7 8 8 8 8 8 8 8 8 8 8 8 8 8 9 9 9 9 9 9 9 9 9 9 10 10 10 10 10 0 0 0 0 0 0 0 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 2 2 2 2  -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9  L 1 2 3 4 -9 -8 -7 -6 -5 -4 -3 -2 -1 . 0 1 2 3 -8 -7 -6 -5 -4 -3 -2 -1 0 1 -6 -5 -4 -3 -2 1 2 3 4 5 6 7 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6 7 -8 -7 -6 -5  FO 37.43* 15.45* 0.00* 0.00* 31.10 8.42* 74.90 51.85 24.66* 34.43* 40.01 32.90* 0.00* 37.22* 59.22 24.42* 23.79* 21.02* 33.52 17.71* 5 0 . 89 66.42 48. 1 1 27.45* 9 5 . 12 16.66* 0.00* 24.39* 26.98* 0.00* 26.46* 38.45* 22.86* 16.76* 0.00* 31.71 56.50 65. 92 18.92* 85.08 18.14* 0.00* 16.39* 5 2 . 40 20.72* 0.00* 19.25* 30.04* 16.34* 0.00* 0.00* 43.55 0.00* 15.89* 49.87 25.35* 43.09 66.01  FC 53.41 14.02 12.20 3.86 2 2 . 16 13.98 70.27 52.42 3 . 11 33.34 37.40 45.69 23.64 36.53 62.43 13.32 11.75 26.84 24.81 8.36 44.85 60.07 4 6 . 15 33.37 94.73 2 9 . 15 7.53 27.65 14.87 2.33 25.94 37.90 25.12 17.09 3 . 12 3 7 . 16 54.28 57.59 13.43 78.43 4.75 10.75 5.04 49.48 7.07 6.69 19.64 39.05 9.03 2.69 3.03 43.46 7.12 33.95 43.64 26.11 41.74 54.54  H  K  2 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 4 4 4 4 4 5 5 5 5 5 5 5 5 5  -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9  FO  L -4 -3 -2 -1 0 1 2 3 4 5 6 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2 3 4 5 -8 -7 -6 -5 -4' -3 -2 -1 0 1 2 3 4 5 -7 -6 -5 -4 -3 -2 -1 0 1  15.20* 24.70* 24.28* 71.33 14.41* 40.49 45.33 43.49 42.83 20.15* 40.33 21.21* 42.68 0.00* 26.12* 0.00* 70.94 34.42 40.90* 19.23* 43.09 0.00* 45.41 11.87* 52. 36 43.72 35.59 0.00* 28.87 29.39* 54. 10 28.48* 23.97* 41.86* 41.08* 50.70 39.94 35.46 41.88 16.73* 19.96* 23.09* 19.44* 0.00* 24.37* 20.73* 0.00* 20.79*  i  FC 14.95 24.98 18.27 65.82 17.75 31.99 41.75 41.34 47.40 14.23 30.53 13.57 42.03 2.21 25. 84 2.55 58.42 23.03 47.90 0.37 32.22 7.54 52.72 3.40 51.76 34.89 29. 18 7.27 21.56 18. 80 50.68 28. 18 30.20 35.86 45.08 44.50 43.55 33. 1 1 44.80 18.49 3.30 24.64 8.65 7.4 0 5.06 16.35 8.38 12.34  H 5 5 •5 6 6 6 6 6 6 6 6 6 6 7 7 7 7 7 7 7 0 0 0 0 1 1 1 1 1 1 1 2 2 2 2 2 2 3 3 3 3 4 5 6 6 8 8 8  K  L  -9 2 -9 3 4 -9 -.9 -7 -9 -6 -9 -5 -9 -4 -9 -3 -9 -2 -9 -1 0 -9 -9 1 -9 2 -9 -6 -9 -5 -9 -4 -9 -3 -9 -2 -9 -1 0 -9 -10 0 -10 1 -10 2 -10 3 -10 -3 -10 -2 -10 -1 -10 0 -10 1 2 -TO -10 3 -10 -3 -10 -2 -10 -1 0 -10 1 -10 -10 2 -3 -10 -10 -2 -10 -1 -10 0 -5 5 -5 -10 -5 -13 -5 -4 -5 -6 -5 -5 1 -5  FO 19.22* 60.16 20.27* 7.97* 30.78 41.32 33.91* 10.77* 49. 75 0.00* 38.73 46.57 35.19* 22.26* 27.60* 0.00* 42. 35 6.36* 30.56* 24.07* 39.57 9. 26* 10.14* 13.54* 15.48* 31.31 13.59* 43.85* 41.34 0.00* 5. 37* 28.47 58.91 32.68* 44.73* 31.55* 18.78* 30.62* 30.59* 3.02* 37.16* 77.04 35.38 107.56 17.39* 75.60 86.74 28.35*  FC 12.36 66.81 9.21 5.47 19.18 42.20 36.73 16.11 34.4 5 19.94 26.57 38.51 32.49 0.68 10.74 4.63 39.44 5.22 7.14 12.42 36.42 7.40 13.92 9.37 16.65 24.97 11.83 12.98 33. 19 2.'60 14.76 18.96 48.51 24.89 23.56 16.95 17.26 17.20 18.62 0.37 13.33 76.62 27.66 109.68 12. 33 79.70 83.54 19.79  Dimethylammonium trichlorotris(dimethylsulphoxide)ruthenate(II) Anthony Mercer Observed  and James T r o t t e r .  and c a l c u l a t e d s t r u c t u r e  amplitudes  ( r e f l e c t i o n s with i n t e n s i t y < 3 (I) are marked with an asterisk). The f o l l o w i n g planes which had |Fo-Fc| > 3 (F) were given zero weight i n the f i n a l stages o f refinement due t o suspected e r r o r s r e s u l t i n g from e x t i n c t i o n , a b s o r p t i o n , or instrument m a l f u n c t i o n : h  k  1  4  0  0  2  4  0  45.8  19  0  1  21  0  1  2  1  10  Fo  Fc  h  k  1  Fo  Fc  9  0  4  64. 8  92.0  6 0.4  12  0  4  54. 4  70.2  50. 0  66.3  3  0  5  96. 3  72.6  52.4  66.0  2  3  5  63.0  44.3  1  303.9 494. 4  8  0  7  37. 9  18.6  0  2  113.6 142.5  10  6  7  28. 2  11.2  17  1  2  26.2  8.7  19  0  8  74. 9  90. 8  14  0  3  77.4  94.4  0  1  9  61.4  42. 1  4  0  4  43.8  62. 2  1  0  14  38. 4  367.5 544.8  4, 1  H  K  L  6 8 10 12 14 16 18 20 22 24 26 28 2 4 6 8 10 12 14 16 18 20 22 24 26 28 0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 2 4 6 8 10 12 14 16 18 20 22 24 26 28 0 4 6  0 0 0 0 0 0 0 0 0 0 0 0 1 1 1 1 1 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 3 3 3 3 4 4 4  0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0  FO 0. 00* 292.18 35 7. 89 164.03 252. 85 116.78 137.67 102.57 146. 10 96.27 59.84 44. 54 140.02 54. 74 73. 35 91.36 257.53 63. 03 134.59 38.09 88.24 70. 99 65.45 145.46 44. 64 105.82 279.75 10.37* 114.75 78. 07 56.75 129.18 52. 38 215.50 90.67 43.02 77. 98 88.23 34. 42 16.41* 26.86* 40.60 114.48 65.86 49.02 124.48 118.97 99.49 52. 22 49. 97 38. 53 28.89 125.42 76.50 66. 03 284.46 211.21 48. 24  FC 1 10.09 309.19 400.62 172.55 262.08 116. 14 144.95 93.97 143. 18 94.51 56. 50 46.22 150.64 55. 32 67.32 79.80 242.48 63. 43 122-02 38. 47 87.76 73.78 64.81 142. 13 46.54 102.62 285.41 10. 17 91.52 64.51 48. 25 132-94 55.30 213.85 91.94 44.01 79.82 82-33 37. 87 24.22 26. 45 31.19 1 15.34 78. 88 51.73 141.70 127.58 107.51 50.01 51.29 34. 62 24.92 120.27 76.89 61. 56 271.97 205.48 59.07  H  K  L  8 10 12 14 16 18 20 22 24 26 2 4 6 8 10 12 14 16 18 20 22 24 0 2 4 6 8 10 12 14 16 18 20 22 24 2 4 6 8 10 12 14 16 18 20 0 2 4 6 8 10 12 14 16 18 2 4 6  4 4 4 4 4 4 4 4 4 4 5 5 5 5 5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 6 6 6 6 6 6 7 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 8 8 9 9 9  0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0  FO 131.65 115.25 17.30* 236.08 13 8. 41 40. 71 47. 00 82. 17 47. 84 9. 70* 65.76 97. 16 62. 21 62. 97 172.78 103.32 110.74 37. 13 31. 78 59. 76 53. 83 97.50 361. 13 151.22 232,35 38. 81 196.51 166.85 179.29 188. 81 35.28 83-81 45. 45 113-77 66. 05 36. 45 22. 99* 38. 03 0. 00* 86.30 36. 32 93. 13 0.00* 39. 41 51. 49 173-56 48.31 90. 15 28. 87 61.40 106.07 50. 41 97. 74 0. 00* 37. 85 24.02* 47.77 63. 52  FC 133.23 117.86 13. 80 227.54 131. 62 33* 32 46, 67 79. 88 46. 87 2. 52 57. 87 91.92 5 2- 25 60. 92 157.77 105. 58 105.40 38.44 26. 18 62.20 50.66 96. 92 328. 04 137.90 213.43 43.09 185.64 165.58 172.33 188. 30 34. 23 84- 63 41-39 11 1. 54 64.72 35.72 21- 19 3 5-37 2. 40 87- 34 39. 05 92-75 7. 15 43-87 45. 09 170. 81 50.66 96. 66 25. 12 62. 85 103.22 50. 24 91.09 18. 24 40-71 19.53 44- 88 59.39  H  K  L  8 10 12 14 0 2 4 6 8 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 20 22 23 24 25 26 27 28 29 0  9 9 9 9 10 10 10 10 10 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1  0 0 0 0 0 0 0 0 0 1  1  3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23  1  1  1 1  1 1 1  1 1 1 1 1 1 1 1 1 1  1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1  1 1 1 1 1  FO 19.56* 66.79 40. 60 50.58 145.77 87. 15 76. 94 6.59* 42.59 12.29* 64.43 168.74 0.00* 138.63 102.01 114. 11 247.89 61.21* 0. 00* 212.09 125.26 0. 00* 32.04* 44.04 73.46 5.24* 103.73 65.75 51.68 0. 00* 46. 88 1 17.61 0. 00* 0. 00* 46.93 193.85 221.24 170. 99 28. 19 114.80 120.08 1 14.27 117.49 161.64 163.26 160.31 199.66 149.13 49. 02 88. 17 120.08 47.56 38.7 5 82.87 78. 80 66.64 34.02 66. 16  FC  H  K  L  13.50 65. 47 44.61 47.37 137.79 87.78 74.93 9. 11 41.70 26.69 77. 13 174.69 47.73 127. 14 106.93 142-65 246.95 89.66 44.38 213.91 127.32 27-39 35.45 47. 13 77. 51 42- 14 101-38 71. 92 53. 28 10. 15 50.09 116.36 51. 17 0.92 48-95 192.75 255.31 185.76 29.28 103.90 128. 19 123.66 100.72 162.22 160.74 158-22 193.65 142.71 47.33 87.97 114.65 45. 47 35.38 77.04 77.76 63. 60 27.97 65.66  24 25 26 27 28 29 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23  •j 1  1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1  1  1 1 1  2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3  1  1 1 1 1 1  1 1 1 1 1 1 1  1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1  FO 71.84 85.04 50.78 2.84* 23.71* 26.18* 39.19 31.80 140.17 38.57 42. 33 59.64 74.94 40.63 37.81 101.01 31.99 160.54 62.77 55.43 25.54 31.04 51.28 25.77 11.35* 22.64* 32.28 63. 43 35.07 75.67 33.72 117.75 16.35* 48.37 50,16 84.12 166-07 137.12 20.88 17-56* 155.04 61.37 17.37* 58.84 118.53 99.48 156.86 67.78 118.70 39.76 99.61 77.78 92.84 19.86* 68.11 22. 88* 23.43* 12.07*  FC 66.55 83. 46 4 7. 98 14, 11 2 1 . 83 29.38 42. 00 36.09 129.51 29- 47 38. 44 55. 91 63.93 37. 71 37.60 102.72 31. 09 164. 32 58. 46 58- 24 27.27 35. 09 52- 09 19.66 5- 89 21. 29 30.42 56. 76 34.93 71. 90 33. 35 111.64 25- 80 45. 83 3 6. 05 84.90 144.54 125,81 32.61 14. 64 160.77 56- 83 29-34 49.34 11 7. 10 100.63 160.54 67. 40 121. 61 38.71 10 0.40 79.90 94- 75 16. 18 63. 27 20. 90 22. 62 1 8. 42  H  K  24  3  1  5 7 . 0 1  25  3  1  3 3 . 8 7  26  3  1  2 3 . 7 8 *  27  3  1  1  4  1  L  FO  FC  H  K  5 4 . 7 8  3  6  1  4 2 . 2 7  3 3 .  3 0 . 5 6  4  6  1  6 6 . 1 5  6 7 .  21  17.91  5  6  1  5 5 . 7 0  49-  47  4 1 . 2 1  3 2 . 3 3  6  6  1  2 0 . 2 6 *  26.  88  1 2 6 . 2 7  1 0 1 . 8 8  7  6  1  6 4 . 7 3  6 0 - 0 6 7 3 . 7 1  L  FO  FC  2  4  1  1 1 0 . 0 4  9 7 . 4 5  8  6  1  7 7 . 1 5  3  4  1  4 5 . 5 4  46.  9  6  1  4 0 . 7 8  4  4  1  9 4 . 7 9  8 9 . 9 5  10  6  1  5  4  1  3 3 . 5 8  3 3 . 3 5  11  6  1  18  65.  69  3 8 . 3 3  16  68.  01  3 9 . 0 3  3 7 .  50  6  4  1  4 7 . 9 1  4 6 . 0 3  12  6  1  7  4  1  6 6 . 4 7  6 2 - 2 2  13  6  1  6 1 . 9 0  6 3 .  06  8  4  1  9 0 . 1 9  8 9 - 9 4  14  6  1  4 0 . 8 3  48.  09  9  4  1  2 4 . 6 2  2 1 -  15  6  1  3 3 . 1 8  2 9 . 0 3  1 1 2 . 9 3  7 2 . 3 1  72.  27  6 2 .  57  10  4  1  11  4  1  12  4  1  1 3 9 . 7 9  13  .4  1  9 0 . 9 6  1 6 . 2 4 *  26  1 1 0 . 0 3  106.  16  1 0 6 . 4 3  16  6  1  17  6  1  1 3 1 - 3 6  18  6  1  2 1 . 7 7 *  22.  02  8 7 . 3 8  19  6  1  2 5 . 1 2 *  24-  46  13.  39  63.  82  14  4  1  4 8 . 7 4  3 7 . 7 4  20  6  1  3 7 . 9 6  3 5 . 6 0  15  4  1  3 2 - 9 0  3 4 - 7 7  21  6  1  5 1 . 8 9  53-  56  16  4  1  7 0 . 4 9  6 0 . 0 7  22  6  1  5 6 . 8 2  54.  45  17  4  1  4 2 - 0 8  4 3 -  23  6  1  4 8 . 4 2  4 9 - 9 7  18  4  1  3 3 . 4 4  3 1 - 6 4  0  7  1  8 7 . 6 6  8 5 .  45  19  4  1  2 6 . 6 0  2 3 - 5 6  1  7  1  1 5 8 . 2 0  146-  00  14  20  4  1  6 . 8 1 *  8.  2  7  1  124.01  1 0 8 . 5 7  21  4  1  0 . 0 0 *  4 . 8 9  3  7  1  1 0 1 . 3 9  9 0 . 2 3  22  4  1  6 3 . 4 3  6 1 . 6 0  4  7  1  1 5 . 6 2 *  23  4  1  7 7 . 1 1  7 3 . 7 5  5  7  1  8 8 . 9 9  84.  11  24  4  1  26.  6 9 *  2 9 .  18  6  7  1  66. 1 1  5 7 .  22  25  4  1  2 5 .  9 0 *  24-  40  7  7  1  6 7 . 8 8  64.  16  26  4  1  7 8 . 4 7  7 4 . 7 0  8  7  1  2 6 . 2 2  26.  03  0  5  1  1 1 7 . 3 0  1 0 6 . 9 7  9  7  1  9 3 . 0 9  86.  99  7 7 .  31  34  1  5  1  1 6 0 . 5 2  1 4 1 . 6 9  10  7  1  8 2 . 2 2  2  5  1  2 3 6 . 3 5  2 3 1 .  11  7  1  1 0 5 . 8 2  18  7.46  1 0 0 . 7 7  3  5  1  9 9 . 6 9  9 1 . 5 2  12  7  1  9 5 . 2 5  9 5 .  4  5  1  5 1 . 3 7  4 6 . 2 5  13  7  1  6 0 . 7 5  5 8 .  81  5  5  1  7 8 . 5 7  7 8 . 9 1  14  7  1  5 5 . 2 9  52-  08  6  5  1  9 0 . 0 5  9 9 . 7 3  15  7  1  7 6 . 3 8  7 5 .  17  7  5  1  8 5 . 2 6  7 8 . 6 6  16  7  1  5 9 . 2 0  55-  45  8  5  1  4 8 . 4 4  4 1 . 3 0  17  7  1  2 2 . 9 5 *  2 0 .  86  5 1 . 0 4  5 1 . 9 0  18  7  1  3 7 . 2 5 i  3 2.  92  9 4 - 8 1  19  7  1  4 4 . 4 3  43.  10 63  08  9  5  1  10  5  1  11  5  1  1 4 6 . 2 3  1 4 0 . 8 4  20  7  1  4 9 . 6 2  4 5 .  12  5  1  1 5 9 . 7 3  1 4 9 . 6 2  21  7  1  4 6 . 9 2  4 5 . 5 0  9 3 . 3  9  13  5  1  7 6 . 6 1  14  5  1  1 0 3 . 5 3  15  5  1  16  5  1  17  5  1  18  5  19  5  20 21  7 9 .  29  1  8  1  1 8 . 6 0 *  15.  08  1 0 5 . 3 8  2  8  1  2 7 . 5 1  27.  32  8 8 . 8 3  8 6 . 3 4  3  8  1  4 1 . 1 0  3 7 .  80  1 1 0 . 1 4  1 0 7 . 1 7  4  8  1  42.41  35.  53  3 0 . 6 8  3 4 . 2 3  5  8  1  3-  84  1  3 9 . 2 4  4 0 . 7 9  6  8  1  3 6 . 9 3  3 1.  20  1  2 0 . 3 5 *  2 0 . 0 9  7  8  1  2 0 . 6 2 *  1 4 . 9 2  5  1  6 6 . 5 2  6 5 .  8  8  1  3 3 . 7 7  3 1 . 6 1  5  1  7 6 - 7 1  7 4 . 3 4  9  8  1  2 8 . 1 3  2 5 .  22  5  1  3 3 . 3 3  2 9 . 7 6  10  8  1  3 7 . 3 2  34.  84  23  5  1  5 1 . 2 6  5 0 . 6 6  11  8  1  2 1 . 1 8 *  3.  98  44  0 . 0 0 *  22  24  5  1  5 2 . 7 8  5 2 - 7 7  12  8  1  7 5 . 4 7  25  5  1  3 7 . 8 5  3 7 . 6 9  13  8  1  3 1 . 8 4  3 0 . 3 8  1  6  1  1 0 1 . 0 7  8 5 . 8 7  14  8  1  3 2 . 9 8  3 1 .  2  6  1  5 3 . 1 8  5 2 . 2 1  15  8  1  1 5 . 0 6 *  1 7 - 0 8  7 1 . 8 1 63  H  K  L  16 17 18 19 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 1 2 3 4 5 6 7 8 9 0 1 2 3 4 5 6 7 8 9 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 1  8 8 8 8 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 10 10 10 10 10 10 10 10 10 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1  1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2  FO 43.56 18.00* 29. 98 0.00* 68.21 62. 16 155.77 53.56 22.26* 31. 33 94. 14 27.88* 37.54 39.21 55.43 48.76 90.28 45.90 21.05* 24.01* 12.40* 12.27* 21.75* 49.95 15.53* 24.00* 0. 00* 59.22 31. 23 202.12 300.48 268.97 106.50 136.94 0. 00* 101.62 0. 00* 0.00* 252.84 224.22 9.39* 124.27 6. 65* 88.28 93. 53 7.21* 18.33* 21.91* 60.55 23.06* 0.00* 86.35 0. 00* 21.94* 0.00* 57. 92 0.00* 121.56  FC  H  K  L  39.94 17.28 29.47 0. 78 64.56 60.64 149.54 53. 15 10.73 25.35 91.56 28.98 36.46 37.60 52. 53 48.62 89. 13 46.68 17. 28 15.75 9. 19 17.35 18.61 49.99 8. 22 25.51 10.61 53.78 29. 92 187.70 348.79 306.24 104.01 135.31 55.72 105.74 17.04 20.33 253.45 218.21 71. 13 121.63 50.32 93.83 95. 28 35.58 25.99 31.61 61.22 34. 35 28. 16 82.63 34. 14 32.53 16. 11 55.47 14. 88 116.84  2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 18 19 20 21 22 23 24 25 26 27 28 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 1 2 3  ! 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 3 3 3  2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2  FO 47. 90 45.72 102.73 17.63* 64. 10 134.22 77.55 78.95 184. 34 164.60 172.26 43. 17 74.62 93. 33 13.63* 41.79 101.68 16.22* 53.32 36.46 71. 09 56.37 49. 90 67.49 41.61 25. 05* 92. 74 217.23 67. 14 128.25 85. 81 31.69 86. 41 7. 72* 46. 67 102.01 37. 77 113.43 79.01 173.45 101.27 13.21* 107. 12 97.51 56. 13 39.87 63. 17 47. 98 34. 29 105.26 36. 15 22.43* 10.29* 69.92 34. 10 146.47 1 13.62 158.00  FC 43.27 47.69 94. 27 17.91 59.76 128. 19 72. 46 77. 94 175.46 161.03 163.01 42- 04 64. 15 9 2. 27 1 4. 50 40. 66 99. 13 2. 48 4 7. 03 39.01 68. 08 54. 47 48. 69 65. 99 40. 95 23. 84 80.68 205.98 76, 86 136,10 74-59 3 6.49 94. 00 9.77 37. 77 108. 29 3 9.05 114.29 79. 96 172.47 95. 23 9.74 105.60 95. 44 52.70 36. 96 61. 66 44. 59 32.73 97.38 34.90 10. 83 13- 17 62. 66 30.27 129.72 98-91 140. 47  H  K  L  4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 1 2 3 4 5 6 7  3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 5 5 5 5  2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2  5 5 5  FO 151.98 144.25 50. 26 53.88 123.37 84.30 78. 83 71.64 58. 97 45.52 55.55 70.50 11.28* 29.43 52.29 70.92 17.98* 58.87 66.37 27.60* 55.54 54. 10 85.33 26.18* 2 10.64 192.66 103.83 208.94 73. 38 77.28 22.48* 44. 50 73.22 133.87 24. 71 101. 12 96. 17 195.25 73. 14 53.26 63.04 57. 35 53. 49 38. 41 55. 93 42. 46 64.36 97.43 39.56 44.75 7. 95* 106.19 75.56 90. 43 87.60 85.62 102.82 21.33*  FC  H  K  L  140.51 120.48 37.92 51. 85 126.51 79.93 84.99 71.87 63.81 43.40 54. 02 69. 15 21. 48 30.43 43.27 68.59 12.62 56.20 60.30 27. 45 49.74 51.49 81.45 25.67 207.61 171. 45 112.56 191.47 78.73 77.78 27. 13 45.30 75.78 133.83 15.70 95.95 93.31 187.89 66.09 47.91 61.34 54.47 48.21 39,73 52.95 41.85 64.08 94.95 38.80 42. 87 14.92 104.09 65. 81 85.33 76.69 84. 10 93. 15 19.35  8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 1 2 3 4  5 5 5 5 5 5 5 5 5  2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2  5 6 7  8 9 10 11 12 13 14 15 16 (  5  5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7  FO 65.44 27. 44 102. 30 99. 84 102.54 37. 11 41. 57 75.40 4 3. 81 10.76* 14.53* 33.50 12.03* 70.68 25.98* 40.45 31. 41 70. 16 57. 30 149.48 196.24 130.88 77.82 49.76 106.32 62.95 80.71 113.29 79. 05 1 15.92 122.46 146. 19 6. 91* 38. 62 92.79 18.55* 17,05* 25.78* 86. 22 26.97* 0. 00* 75.40 55. 04 21.69* 61. 65 72. 55 50. 13 33. 90 20. 97* 50. 67 33. 11 30. 05 52. 88 84.73 23.55* 23.28* 58. 45 24.20*  FC 59. 81 30. 11 92- 62 90. 57 97. 97 38. 11 43. 27 67. 82 41. 05 17- 49 1- 98 31. 58 8. 43 63. 19 24. 57 39. 16 29. 08 6 2.70 56. 99 133- 08 172. 04 123. 13 75. 02 45. 95 91. 87 65. 37 82. 46 107. 73 74. 25 115. 14 121. 51 144. 87 20, 48 38. 23 9 2. 48 19. 46 19. 71 22. 76 81. 29 29. 93 7. 72 71. 74 54- 60 15. 84 57. 83 68. 58 48. 67 33. 10 13. 44 47. 64 3 3 . 10 31. 60 50. 97 80- 75 19- 78 20. 50 57. 23 15. 57  H  K  L  17 18 19 20 21 0 1 2 3 4 5 6 7 8 9 10  7 7 7 7 7 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 9 9 9 9 9 9 9 9 9 9 9 9 9 9 10 10 10 10 10 10 10 10 10 0 0 0 0 0 0 0 0 0 0 0  2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 3  11  12 13 14 15 16 17 18 1 2 3 4 5 6 7 8 9 10 11 12 13 14 0 1 2 3 4 5 6 7 8 1 2 3 4 5 6 7 8 9 10 11  FO  FC  0.00* 1 1. 77 28.29* 31. 13 60. 82 57-81 21.28* 8. 96 16.55* 13.82 79. 06 81.00 1 10.97 100.89 30.06 28.66 43.-47 39.32 54.92 56.56 52. 84 52.96 11.54* 9-26 29. 57 32. 44 51.85 54. 21 80- 35 77-44 23.62* 21.78 72.70 68. 81 36. 98 28.24 74.93 70. 12 60.51 60. 23 29. 86 25. 19 38. 48 33.37 50.28 50-36 38.47 37.25 25.59* 33.23 29.99 27. 00 27.23* 28. 48 23.43* 21.34 15.33* 12. 63 42. 80 37-63 40. 41 38-31 31. 20 35.51 15.57* 23. 27 67.74 65. 44 70.73 66.59 27.80* 30. 42 29.95 24. 17 54.63 54-44 92. 13 90-78 101.46 97.99 37. 46 3 1 . 18 58. 62 55.76 62. 39 59-91 60.66 59.65 14.96* 20-08 41.82 39. 19 34.44 38. 26 0.00* 29.38 82.54 80. 40 82.08 85.86 90.57 85.26 0. 00* 26. 58 0.00* 6.48 81.54 89.95 0- 00* 66. 84 0.00* 119. 14 244.73 239.60 0.00* 69. 57  H 12 13 15 16 17 18 19 20 21 22 23 24 25 ' 26 27 28 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 1 2 3 4 ' 5 6 7 8 9 10 11 12 13  K  L  0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1 1 1 1  3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3  1 1  1 1 1 1 1 1  1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 2 2 2 2  FO 45.42 95. 86 70.33 0- 00* 99. 64 0. 00* 46. 50 39.96 46. 04 0. 00* 0. 00* 7 0. 44 0. 00* 0. 00* 0. 00* 42.31 195.60 77. 36 54. 44 27.34 81.89 160.63 113.86 128.78 183.44 87.86 99.90 1 10.21 96.58 20.98* 160.64 70.27 86.21 38. 26 60. 29 21.43* 57. 15 51. 00 98.64 0. 00* 37.77 58. 35 17.84* 52.48 6.47* 110.58 73.40 145. 15 133.54 66.46 85.64 74. 56 60. 85 48. 32 165.23 52. 80 42.53 71.86  FC 61. 89 10 2- 55 67. 17 14. 87 100.97 25. 69 49. 05 42. 38 50. 51 3. 66 23. 52 67. 95 15. 57 9.80 1- 18 42. 08 208. 83 89.91 54. 40 24. 48 78. 56 148.98 117-24 109.38 170. 18 76. 15 91.98 102.76 90. 69 29. 04 153. 21 64,73 81.56 32- 02 55, 84 17.20 54. 10 48. 42 92. 81 10. 43 31. 88 53. 84 25. 81 49. 84 18. 89 105. 54 84- 14 133.60 131. 22 65.71 85. 39 66.39 59. 04 51.39 155.51 58- 06 41. 23 69. 21  H  K  1  14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 0 1 2 3 4 5 6 7 8 . 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15  2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4  3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3  FO 72.02 40. 15 95. 97 98.26 19.92* 61.65 77. 47 62.05 30. 04 34. 26 118.06 28.59* 41. 86 25.73* 52. 56 434.78 137.48 198.28 50.96 201.21 56.80 103.78 88.67 96.73 49.04 160.55 119.96 142.58 8. 04* 180.90 128.55 0.00* 6.64* 70.56 51.93 33.47 65. 12 137.01 16.25* 40. 74 74.70 26.01* 19.48* 125.46 86. 04 127.25 76. 43 76. 68 127.40 44. 28 39.77 55. 89 100.59 42.28 24.60 59.74 85.64 3.08*  FC 73.02 42.77 88. 57 95.71 15. 34 57.98 69.77 56. 16 25.65 31.77 108.38 25.62 37. 45 26.87 49.66 440.67 133.09 208.75 58.97 197.81 55.30 116.40 99.83 97.72 42.40 177.37 135.02 148.56 4.29 196.05 137.43 8.83 14.24 73.21 56.98 35.01 66. 14 143.78 18.65 50.55 73.52 22.31 21.42 126. 15 86.69 130.83 80. 10 87. 19 129.78 48. 03 39.47 52.37 100.82 37.70 23.82 58. 12 84.06 10.54  EI  K  L  16 17 18 19 20 21 22 23 24 25 26 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21  4 4 4 4 4 4 4 4 4 4 4 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6  3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3  FO 38.01 51-30 23. 45* 14. 31* 30.34 0. 00* 34.68 41. 65 96.32 13.88* 13.86* 228.38 90.58 29. 06 69. 62 106,31 45.91 13.26* 100.34 112.32 47. 22 88.68 93.36 102.84 31.74 103. 28 42. 21 0. 00* 28- 00 44. 36 3. 57* 2.66* 33. 09 104. 05 21.79* 23.21* 34.98 105. 04 46.54 111. 53 76. 14 72. 51 84. 19 27. 42 41.04 18. 64* 88.40 27. 88 21.22* 20.08* 58. 12 24. 76* 31. 84 30.96 27.29* 33.55 45. 47 26.30*  FC 39. 56 52.79 29. 83 18. 90 26. 98 17. 94 32. 70 44.93 101. 37 22.26 6. 58 236.92 87. 72 20.90 66-39 117. 17 42.82 11- 69 95.51 117.60 48. 70 88. 18 91. 6 6 107.08 33.21 102-98 4 3. 27 10. 63 29. 08 47. 16 14. 58 12- 02 39.67 106. 91 18. 72 23. 68 31. 84 97. 20 45. 84 108. 09 78. 55 71.53 86. 62 23.62 45. 55 22- 72 9 4. 23 31. 81 22.25 27- 39 62- 87 20.97 28.89 32. 09 29. 26 32-97 45. 17 27- 57  H  K  L  22 23 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 1  6 6 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 10  3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3  3  3 3 3 3 3 3 3 3 3 3 3 3 3 3  3 3 3 3  FO  FC  29.30 27.79 0.00* 3. 43 160.59 154.57 46. 05 44. 73 36. 52 34.59 54. 83 51.01 60.64 61.89 34. 94 38.90 24.76* 30.72 21.12* 19.40 53.55 58.09 52.87 54.02 71. 24 8 1. 23 30. 14 18.95* 35.69 36.29 49. 03 56.52 81. 24 90.78 23.57* 31. 44 13,03* 24.75 47. 06 53. 87 38. 87 45.63 17.60* 7.81 22.9 7* 9.88 24.68* 22.96 24. 24 20.20* 30.46 33.85 30. 90 37.03 30. 23 31.75 14.68* 21.59 30.34 36.42 11.75* 19.89 33.00 33.60 29.93 30. 84 59.29 63.01 1. 11* 11. 49 48.45 49. 20 43. 05 52. 19 22.00* 27. 4 2 24.25* 18.76 23.95* 22-56 50.43 52. 42 0.00* 20.43 91. 79 98. 47 64.92 66.96 83.58 86.98 86. 80 93. 98 38.60 44.00 41.38 40.98 32.20 34.58 86. 00 92.30 48.21 50. 63 34. 16 31.41 60. 57 65.86 71.96 76.29 46. 40 49.09 42.34 48.89 56.85 60.24 16.80* 19. 03  H  K  L  2 3 4 5 6 7 0 1 2 3 5 6 7 8 10 11 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26  10 10 10 10 10 10 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1  3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4  FO 15.76* 14.50* 9. 24* 19. 76* 20.24* 14.79* 61. 50 66. 14 20,19* 98. 05 76.69 24.64* 93. 59 144.03 101.52 99. 20 9,06* 38. 98 0. 00* 39. 37 0. 00* 117.98 30.45* 45.97 45. 26 42.67 0. 00* 71. 19 0. 00* 0. 00* 54. 81 0. 00* 43. 54 100. 10 142.58 91.95 60. 00 50. 19 22. 19 139.49 63. 63 84.62 54. 14 109.92 76. 29 0. 00* 71. 75 32.85 113.20 45.75 78. 27 20.31* 63.03 50.70 24.99* 48.93 32. 15 47.71  FC 21- 43 17. 93 2 4- 36 2. 28 24. 22 7. 66 61.92 66. 81 43. 32 94. 92 84. 89 3 8. 90 97- 84 148.69 121.77 110.92 34. 20 41.36 13. 07 38. 81 10. 62 118.92 64.49 56. 12 52. 84 51. 05 43. 53 78. 16 28. 66 5. 80 5 1. 04 27. 75 43. 32 101. 44 146.00 95. 18 61. 98 50. 12 17.77 139.13 60.39 85.51 51. 62 110.69 76. 69 7.36 75- 88 35. 15 120.51 44. 43 75. 44 19. 17 6 2. 43 56. 55 17.88 4 9. 93 32. 66 50. 19  H  K  L  27 28 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 0 1  1 1 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 4 4  4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4  FO 13.82* 32. 59 173.00 156. 13 349.27 144.01 98.40 44. 17 100.39 193.52 85. 12 53. 8 2 132.77 141.75 215.81 17.56* 57. 49 126.70 108.4 1 16.72* 51.91 44.43 90. 18 68. 89 60.77 0. 00* 83.94 57. 63 42. 63 24.42* 147.81 49.48 156.79 129. 11 102.08 98.46 105.78 89, 03 37. 37 32.70 50.81 91.95 49.22 64-69 46.79 47.99 94. 36 80.45 31.82 41.56 48.76 98.54 45.05 37. 51 35.94 76.82 132.40 79. 19  FC  H  K  L  7.84 29.66 182-37 155.70 352-35 144. 15 107, 18 57. 54 100.94 206.62 91.66 50.6 2 135.63 150.40 225.53 15.57 59.78 132.81 1 12.32 7.71 48.28 48.77 93-35 66.08 62.63 3.04 85.35 60. 92 41. 68 29.20 133.31 50. 45 144.87 138.34 97.53 101.85 96. 10 92.65 4 2.43 35.09 50.36 96. 31 53.32 60.39 45. 43 48. 37 93.60 83.39 29.43 44. 17 46.75 96.92 45.70 38.25 32.44 75.58 122.97 78.08  2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 0 1 2 3 4 5 6 7 8 9  4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 6 6 6  4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4  FO 245.72 125. 89 95. 25 62. 17 116. 41 130.08 74. 67 26. 14 199.87 107.78 156.89 60. 84 115.34 74. 54 76. 13 24.30* 27. 47 25.23* 91. 82 64.51 33.74 46. 43 87.43 45. 48 86. 33 46.73 105.07 52. 50 56.33 54.66 29. 21 74.67 39. 15 44. 01 56.71 . 109.99 27. 56 4. 64* 16.90* 54.76 32. 52 21. 84* 36.07 44.97 19.73* 45. 45 16.21* 7. 86* 18.41* 41. 95 98. 38 56. 95 32. 46 39.98 55. 92 74. 92 22.94* 33.50  FC 252. 13 120.33 88. 06 59. 42 127.70 136. 14 73- 30 20. 04 205.99 114.88 16 4- 44 59. 34 120.03 72. 47 77. 19 15. 00 30. 52 24. 12 96.90 64. 58 33. 30 5 0. 59 88. 69 46. 82 97.99 47.72 109.08 51.64 57. 93 52. 85 20.73 75. 10 38.37 42.71 60. 09 112.23 25.72 10. 41 23. 49 56. 07 30. 93 15.46 37.21 45. 15 26- 47 43. 71 10. 78 4. 63 14.64 39.79 97.21 61- 98 24. 48 37-91 57. 97 76. 92 2 1. 90 41.28  H  K  L  10 11 12 13 14 15 16 17 18 19 20 21 22 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 1 2 3 4 5 6 7  6 6 6 6 6 6 6 6 6 6 6 6 6 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 9 9 9 9 9 9 9  4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4  FO  FC  65.26 66.55 68.51 78.06 69.06 71.77 29. 15 31.73 0. 00* 7. 17 51. 24 57. 60 18.04* 25. 53 9.49* 20.25 44.79 43.95 0. 00* 4.80 31.09 33.34 47. 48 48.03 31. 30 28.91 32.95 36.80 40.66 40.95 68.65 69.26 53.99 55.27 45. 42 49.93 35. 87 33.88 46. 84 50. 34 58. 01 61.14 24.93* 30. 12 38.76 37.03 0. 00* 6.53 36.80 34. 42 64. 04 66.09 32. 61 30.77 13.59 12.88* 26.76 28.52 62.09 65.36 35.68 40. 49 21.45* 20.94 28. 13 24. 68 1 13.29 109.67 20.19* 21. 85 77. 82 78.94 38. 10 35.26 45.67 53. 06 23.35* 19. 10 19.98* • 18.30 58.27 60.02 58.40 52-89 34. 45 32.59 57.54 56.70 60.91 57. 40 87. 94 87-70 24.34* 23. 38 35. 06 39-28 44. 44 42. 21 51.99 54.21 7. 71* 14.28 23. 61 31.52 14.59* 16.52 25.59* 28.03 23.55* 34.97 26.97* 30.52 24.57* 29.08 0. 00* 12.23  H  K  L  8 9 10 1 1 12 13 0 1 2 3 4 5 1 2 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19  9 9 9 9 9 9 10 10 10 10 10 10 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1  4 4 4 4 4 4 4 4 4 4 4 4 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5  FO 40. 26 10.19* 33. 92 34. 01 54. 54 34. 45 59. 85 27.28* 81.93 26.30* 27.47* 19.45* 0. 00* 37. 86 150. 15 98.58 77.55 26. 55 91.39 11.60* 0. 00* 47.31 54. 41 16.65* 0. 00* 73.39 0. 00* 128.18 0. 00* 93. 04 0. 00* 21.16* 0. 00* 21. 51* 0. 00* 16.71* 35. 41 7.75* 210. 91 139.50 45. 35 105. 28 149.00 65. 31 73. 23 1 13-75 3 8.59 174.42 51.74 29.89 27. 11 129.56 82. 01 43. 38 88. 12 54. 17 28.60 36. 44  FC 41- 56 2 0. 59 34. 44 37. 43 55. 61 36. 16 66. 86 31. 14 82. 22 24. 21 26. 67 18.77 22. 48 46. 40 153-05 88. 92 75.61 36. 54 82- 80 17, 04 10. 11 55. 74 61. 95 39.71 35. 10 75- 13 19. 43 129.02 9. 17 93. 11 39.21 30. 88 18, 47 24. 95 22. 13 2 0. 27 36. 29 23- 30 207.60 133.82 46. 12 103- 93 147.20 61. 77 69. 04 115.08 37. 44 175.30 57. 03 33. 02 29. 76 135.20 81. 76 44.58 88.. 43 54. 61 25. 68 37. 15  H  K  L  20 21 22 23 24 25 26 27 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 0 1 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23  1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3  5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5  FO 78. 67 0- 00* 84.42 97. 96 46. 84 6.61* 12.21* 39. 85 129.97 84.20 132.26 87. 31 106.05 102.27 20.29* 44.30 18.14* 60. 08 108.75 35.27 46. 32 27. 87 129.58 63.4 3 38. 41 39. 14 129.63 47.30 42. 28 18.23* 79.29 29. 60 67. 21 0. 00* 51.06 150.73 272.46 182.74 45.45 237.75 0.00* 41.51 52.37 280.92 21.68* 167.24 51.10 238.51 37.76 77. 11 51. 47 80. 84 36.49 68.26 30.63 64.37 27.40* 1 18.61  FC  H  K  L  7 4.54 21.35 84. 19 98. 12 48. 00 4. 34 10.33 41.84 119.02 78.77 131.89 81.73 106.04 106,59 14.21 44.36 26.60 61. 44 1 13.77 22.61 43. 92 25.20 132.41 60.34 37.81 38.77 125.80 51.04 39.67 21. 07 79.74 32.49 67. 22 18.71 52. 00 131.77 269.23 172.46 34.52 249.6 2 33.33 37.09 48.68 298.85 20.53 160.70 48. 18 247.81 33.68 69.21 49.06 87.73 33.68 66. 14 28.72 63.64 27.30 114.63  24 25 26 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 2.1 22 23 1 2 3 4 5 6  3 3 3 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 .5 5 5 5 5 6 6 6 6 6 6  5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5  FO  FC  0.00* 17. 45 44. 10 40. 62 14.50* 6. 04 88.64 87.91 31. 34 32.38 88. 68 99.59 17.70* 15.65 77. 98 87. 17 48. 48 47. 64 0. 00* 10.32 50. 61 49. 71 44. 93 39. 00 89.87 88. 62 75. 17 74.62 78. 07 75.78 43. 92 43. 46 48.00 47. 67 73. 93 74, 24 14.09* 6. 09 18. 85* 21.70 18.37* 17. 52 94. 16 9 1. 86 20.77* 2 5. 50 18. 44 7.83* 0. 00* 14. 03 80.78 80. 52 37. 29 35.53 34. 91 35. 22 107.60 107. 24 118.43 119.41 33. 43 32.75 24. 19 2 6.. 12 86. 96 84. 16 99. 70 97. 19 54. 95 51. 66 58. 53 50. 51 130.66 128.83 97. 23 99.02 11. 10* 13. 61 66.67 72.20 87. 80 88, 42 84.20 82. 97 31. 00 28.76 20.63* 11.21 36. 25 40. 23 26. 78 32. 45 38. 40 41.36 29. 16 28. 08 17.05* 18.73 14. 11* 16.45 37.44 34. 39 82. 14 80. 51 52. 58 47.96 29. 55 28. 10 61. 39 67.52 46. 94 49.77 74. 42 64. 10 33.69 31. 87  H  K  L  7 8 9 10 11 12 13  6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 9 9 9 9 9 9  5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5  in15  16 17 18 19 20 21 22 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 0 1 2 3 4 5  FO 36. 23 54. 55 36. 14 41. 53 52. 71 24. 92* 8. 55* 9. 91* 52. 09 29. 86 33. 29 22. 42* 71. 85 13. 97* 12. 92* 15. 76* 40. 65 112. 73 16. 78* 37. 94 5. 85* 76. 75 0. 00* 47. 76 21. 79* 107. 25 27. 45 71. 30 12. 27* 93. 29 35. 91 33. 81 27. 31 14. 20* 17. 54* 29. 85 48. 40 43. 26 41. 23 30. 50 52. 41 35. 32 14. 05* 34. 28 21. 58* 26. 59 54. 20 0. 00* 36. 06 24. 93* 61. 44 12. 24* 22. 08* 96. 46 22. 17* 56. 90 26. 97* 52. 84  , FC 38.48 56. 14 34.75 46.62 58. 81 27. 28 15.35 15.37 58. 16 25. 11 35.93 18.28 72.50 10.26 10.38 11.70 42. 13 1 12.02 18.76 35. 65 9.75 83.64 10.56 49.72 20. 54 112-61 28. 16 70. 68 9. 68 101.94 36.04 34.58 25. 23 25. 19 19. 37 30. 49 50. 74 46.75 44. 65 31.23 62. 90 35.51 14.66 39. 14 33. 25 24. 84 54.31 1.96 39.51 24.77 59. 80 9.48 19.02 100.26 26.54 62.81 30-91 53. 82  H  K  L  6 7 8 9 10 11 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25  9 9 9 9 9 9 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1  5 5 5 5 5 5 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6  6 6 6 6 6 6 6 6 6 6 6 6  6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6  FO  FC  18. 46* 22.78 37. 21 38-38 17. 58* 13.71 90. 86 89.28 28. 57 3 2. 72 56. 73 61.61 83. 97 86-33 89. 35 93. 46 136. 93 130. 41 31. 12 30, 01 24. 83* 24. 62 45, 41 44. 82 15- 88* 8. 68 75. 73 83- 41 8. 59* 5.90 31. 63 37. 21 0. 00* 18. 84 108, 73 117.53 12. 58* 25. 03 42. 85 50. 70 0. 00* 32.32 67. 68 67. 93 0. 00* 8. 92 0. 00* 1.33 34. 48 35.68 8. 39* 19. 16 0. 00* 14. 58 78. 90 94. 92 77. 48 91. 45 0. 00* 9.51 0. 00* 16. 90 68. 75 74. 06 0. 00* 24. 08 75. 09 82. 17 148. 32 142. 57 69. 92 83. 64 69. 97 72. 44 86. 49 93. 17 79. 97 90. 07 52. 20 58. 51 37. 93 33. 46 46. 49 49. 81 39. 52 45. 09 33. 27 40. 32 39. 16 38. 13 49. 13 46. 14 29. 69 30.63 14- 58* 13- 25 33. 91 33. 86 99. 05 105. 07 30. 31 31.93 62. 91 64, 82 29. 98 34. 46 70. 69 73. 18 24. 89* 25.62 25. 22* 24. 14 39. 99 41. 65 41. 66 39.22  FO 14. 41* 144. 55 150. 52 135. 36 191. 25 88. 96 71. 81 68. 01 217. 17 96. 63 57. 36 1 15.08 191. 66 96. 95 96. 15 102. 19 76. 38 56. 34 38. 99 78. 34 14. 91* i 2 . 35* 84. 34 66. 75 41. 59 25. 79* 45. 92 31. 19 73. 07 14. 25* 122. 69 14. 83* 79. 57 33. 98 50. 02 19. 9 1* 42. 91 76. 28 29. 83 17. 10* 65. 76 41. 61 17. 22* 73. 50 102. 48 18. 01* 42. 19 52. 69 93. 95 13. 02* 25. 26* 43. 64 63. 43 80. 25 101. 93 69. 54 75. 47 64. 13  FC  H  K  L  23. 36 155. 89 153. 87 133. 03 200. 66 87. 62 80. 80 71. 10 239. 42 103. 02 60. 67 119. 82 203. 96 96. 36 97. 27 100, 47 76. 80 56. 92 42. 08 81. 73 9. 66 16. 76 85. 70 72. 61 41. 31 16. 23 48. 87 29. 12 69. 61 20. 70 119. 82 12. 35 72- 24 3 1 . 04 50. 07 23. 81 49. 21 77. 18 26. 50 31. 27 71. 71 43. 25 16. 70 78- 37 104- 57 11. 20 43. 19 55. 13 95. 84 21. 61 26. 92 42. 78 62- 11 85. 94 107. 03 68. 84 76. 53 68. 97  5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14  4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6  6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6  FO 77.47 20. 97* 118. 04 106.77 30.75 23.95* 126.56 87.23 32. 56 39.79 63. 08 17.67* 18.85* 30.39 32.60 17.53* 75. 96 35.46 5. 94* 30. 10 16.42* 14.13* 39. 63 18.46* 35. 56 38. 50 37.91 24.90* 38.13 45.34 20.60* 42. 37 53.52 39, 89 26.62* 15.86* 91. 30 11.66* 56.35 15.84* 85. 64 18.47* 19.28* 56. 27 107. 65 59.73 109.29 26. 43 39. 41 12.91* 133. 15 39. 84 16.41* 59.96 106.05 33. 46 38. 64 37,66  FC 73. 23 18. 44 119. 24 110. 89 23. 89 21. 58 128. 10 90. 44 36. 62 39. 30 65. 40 17. 62 24. 07 24. 10 38. 48 2 0. 60 84. 15 36. 07 10. 58 28. 71 24. 91 17, 03 45. 73 16. 07 3 9,68 42. 94 37. 06 31- 55 31. 66 51. 31 24. 88 38. 14 55. 35 46. 85 31. 72 20. 78 94- 33 18. 93 58. 36 8. 37 88. 19 10. 99 15. 99 56. 85 104. 01 65. 30 110. 07 22. 98 39. 02 30. 19 144. 89 41. 49 2. 29 63. 74 111. 58 37. 40 37. 76 37. 52  H  K  L  15 16 17 18 19 20 21 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 1 2 3 4 5 6 7 8 9 10 1 2 3 4 5 6 7  6 6 6 6 6 6 6 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 9 9 9 9 9 9 9 9 9 9 0 0 0 0 0 0 0  6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 7 7 7 7 7 7 7  FO  FC  77. 45 72. 00 20.18* 1 1-23 32. 10 26.58 23.38* 21. 50 28. 14 29- 84 18.85* 11.49 73- 17 73-28 62. 88 63.07 28.20 22. 47 66.30 68.52 26.68* 25. 15 59.45 59. 91 32. 28 32. 58 34.50 36.66 18. 11* 8.92 20.72* 27.04 32.46 30-54 0. 00* 12.79 29-84 28.40 47. 35 54. 16 34.47 33.99 26.84* 29. 14 39. 15 44.57 56. 17 61. 43 15.39* 17. 47 80.44 80.07 96- 50 99. 11 91.21 90.05 80.22 81. 24 54.78 55.02 79. 89 82.82 80.73 87. 29 91.72 95. 27 56. 59 56.49 64. 13 63.38 83.41 85.67 116.62 119. 10 54. 51 55.54 44. 17 44.64 59.28 63.47 61.64 63.46 22.93* 30.59 12.15* 16.91 35.26 36.43 15.95* 23.04 24.16* 30. 40 24. 10 25.93* 17.06* 22. 70 0. 00* 4.63 17.88* 5.91 24.04* 31.98 63.38 63.42 59. 38 57.29 91. 47 97.81 50. 53 42. 38 1 18.72 115.80 0. 00* 2.72 22.41* 30.99  H  K  L  9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15  0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2  7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7  FO 11.36* 34. 18 24.12* 34. 46 0. 00* 44. 41 0. 00* 0. 00* 76. 14 0. 00* 63. 15 0. 00* 54. 39 41. 92 29.56* 43. 52 0. 00* 235.61 24.59* 154.68 79. 53 1 12.51 116. 18 64. 35 174.27 100. 90 84. 01 137.33 28. 50 165.46 86. 29 107.84 49.23 47. 94 48.72 27.32* 8.22* 55.90 50. 20 57.61 36. 99 73. 30 25.32* 61. 81 28. 27 121. 03 30. 79 107. 16 34.64 51. 95 25. 87 53. 28 74. 90 47. 92 62. 89 24.72* 65. 73 29. 20  FC 5.41 33. 61 19. 23 30. 24 4.35 49. 88 4. 68 33- 73 79.64 22. 86 68. 83 33. 09 55.37 50. 48 42. 22 51. 34 18.60 243.23 17.55 154.87 7 5. 13 111.44 115-23 62. 52 179. 13 103. 47 83. 79 137.52 34. 58 165- 53 87.88 109.21 45. 51 51. 17 53. 64 34. 22 18. 98 56. 22 48. 69 56.56 43. 46 74. 90 35. 10 62. 49 30. 49 122.85 27. 47 102. 94 35. 00 50. 40 27. 52 4 8. 22 77. 53 46. 37 65. 96 27. 00 67. 84 35-64  fl  16 17 18 19 20 21 22 23 24 25 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23  K  1  2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4  7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7  FO 32.04 59.79 50. 09 80.66 45. 13 44.35 59. 78 25.12* 40. 07 32. 53 153.09 41. 84 72.77 72.32 24.56 105.37 10.89* 187.54 37.68 106.79 104.60 99.80 82.75 39.94 59.21 31.96 17.70* 36. 1 1 18.35* 38.53 13.37* 66. 97 46.69 20.64* 44. 83 25.35 18.53* 31. 17 34.57 54.64 2. 05* 38.66 38.92 38. 64 26. 04 15.31* 48.97 44. 83 26.82* 48.40 16.07* 105.24 29. 10 95. 30 21.21* 67.03 46.01 36. 97  FC  H  K  L  32.32 60. 17 52. 68 81.25 45.53 43. 26 59.93 29. 26 44.69 34. 27 145.53 38. 18 83.78 74. 13 22. 99 112.90 18.09 189.33 32. 05 113.62 114.56 104.24 84. 83 45. 13 57. 13 30.51 8. 16 40-23 1 1.08 37.32 20.21 68. 59 41.30 14. 00 46.23 18-91 15.72 37. 18 31.34 57.31 9. 12 36. 11 37.47 38. 29 23.72 6. 23 51.75 42.75 31.72 46. 94 12.41 108.29 34. 19 92.93 27. 40 69.65 48.06 3 4.09  0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 1 2 3 4 5 6 7 8 9 11 12 13 14 15 16 17 18 19 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17  5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7  7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7  FO 107.17 23.27* 123. 95 18. 25* 32.56 36. 61 40- 85 74. 70 0. 00* 75.71 78.78 28. 37 69. 90 32. 15 54.47 16.68* 0. 00* 21.93* 9. 81* 45.24 23.31* 55. 78 29. 67 0. 00* 44. 46 7. 45* 49.40 13.00* 31.70 29. 17 15. 46* 31.34 34. 82 37. 62 33.29 47.85 28. 01 59. 00 14.79* 85.36 157.48 49. 05 111.71 42. 15 108.20 101. 10 60. 34 80. 01 100.09 103.55 112.05 35. 32 123.21 48. 38 8 5. 83 14.37* 57. 88 25. 07*  FC 110.80 24-58 115. 04 1 4. 37 38. 18 42. 94 36. 53 73. 06 4. 40 73. 09 78. 00 25- 84 74.78 24. 71 55. 11 14. 13 11.83 11. 86 21^25 46- 69 14.79 55. 07 27. 52 12. 84 48.61 12. 56 44. 00 16. 82 26. 45 30. 34 12. 12 35. 85 36. 22 36.24 34.22 52. 85 24. 31 59. 12 25. 78 86. 29 155. 16 5 0. 37 1 14. 62 38. 06 107.49 101.69 63. 98 86. 22 101.36 104.85 118.80 39-26 123.52 47. 58 86-97 17-21 57. 47 25.70  H  K  L  1 2 3 4 5 6 7 8 9 10 11 12 13 0 1 2 3 4 5 6 7 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 20 21 22 23 24 1 2 3 4 5 6 7 8 9 10  8 8 8 8 8 8 8 8 .8 8 8 8 8 9 9 9 9 9 9 9 9 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1 1 1 1 1 1 1 1 1 1 1 1 1  7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8  11  12 13  FO 64. 99 6. 85* 59.70 13.21* 36.61 9. 90* 32. 07 13.35* 25.19* 31-33 20.44* 25.76* 19.75* 72. 84 48. 15 71. 38 59. 37 37, 87 6.07* 4. 57* 74. 12 105.64 210.05 93. 99 101.86 105. 12 214.33 41. 57 7. 28* 44. 04 209- 51 106-89 127.26 51.70 138.57 74. 90 57.78 24.30* 71.54 0. 00* 69.45 0. 00* 0. 00* 103.30 62.67 109. 15 35.67 77. 55 55.91 96.23 54.35 96.61 86,99 31. 86 12.88* 63.89 37. 62 47.00  FC  H  K  L  69.51 7.06 67.60 10. 48 41.00 2. 17 30.71 24.71 26.55 29.63 18.74 31.05 7.27 73. 18 43.71 71.02 61.04 38.78 2. 36 17.23 78.76 109.85 206.24 90.28 95.39 90.23 216.31 41.86 8.38 40.94 208.04 1 10.34 124.00 59. 23 142.07 79.33 54, 57 46. 93 70.92 3.73 73. 46 0.52 16.32 106.73 71. 13 101.35 28.76 81. 48 51.57 98. 43 49.80 94.38 82.92 30.59 13-51 64. 09 38.09 49.64  14 15 16 17 18 19 20 21 22 23 24 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22  1 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3  8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8  FO  FC  35. 49 41. 95 54. 33 55. 66 30. 50 31. 72 16,16* 2 1 . 98 33. 15 32. 00 107. 83 106. 20 34. 03 36, 56 17.59* 14. 26 45. 07 46. 28 63.54 63. 30 31. 43 33. 94 76. 78 77. 07 125.09 122. 51 113. 73 109. 39 19. 64* 1 1. 04 53. 04 60. 66 173.44 171. 26 107. 13 99- 18 115.41 116. 88 43. 34 41. 86 180.25 182. 82 92.57 92. 52 57. 46 56. 17 78. 51 79. 66 106.63 107. 97 48. 20 49. 25 29. 09 36. 39 50.35 48. 09 29.25 26. 42 16. 03* 19. 58 47. 53 43. 33 41. 27 40. 95 27.54* 24. 25 28. 05 27. 67 58. 00 55. 88 38. 18 40. 23 43. 15 42. 96 2 8.37 24. 89 58. 27 55. 81 29. 63 28. 33 105,48 104. 38 55. 13 5 8. 17 31. 81 29. 62 28.58 32. 11 14.49* 22. 37 2 2. 17* 18- 59 14.79* 18. 41 42.05 4 5.69 6.61* 12. 15 15. 95 2 5.90* 65.27 66. 96 21.90* 7. 78 67. 86 7 0. 99 21.37* 24. 07 87. 15 92. 02 24.83* ^ 29. 47 45.21 42. 56 15.23* 12. 28  H  K  L  23 0 1 2 3 4 5 6 7 8 9 10 1 1 12 13 14 15 16 17 18 19 20 21 22 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 0 1 2 3 4 5 6 7 8 9 10 11 12 13  3 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 6 6 6 6 6 6 6  8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8  FO 58.36 88.89 84. 27 69.77 36. 46 54. 59 89.07 37.64 77.75 38.49 114.52 63. 85 14.60* 19.93* 68.74 49. 36 32.44 10.43* 8. 13* 41.43 53.48 18.35* 20.88* 12.86* 25.51* 8.37* 18.80* 14.63* 45. 80 21.74* 10.21* 21.73* 18.38* 20.24* 56.32 40. 57 24.63* 12.29* 97.87 16.53* 63.01 23.24* 94.58 16.84* 90. 95 98. 94 74. 84 58.40 40. 07 1 11.05 63.73 63.76 38.91 130.92 74. 87 63. 62 76.46 90. 54  FC  H  K  I  60.39 86.05 82. 15 63.67 35.03 56.28 90.58 33.38 78.62 38.64 116. 17 65.68 9. 17 21. 45 67.75 51. 34 33.63 18.42 6.82 42.91 59.21 22.66 27.05 16. 14 26-89 12.84 11. 25 10.32 48. 22 17.84 14. 37 26.62 24. 23 19.58 57.63 39.37 26.30 19. 93 102.01 9.90 63.67 25.62 94. 80 23. 11 93. 14 96. 68 74.48 53. 96 45. 24 1 13.74 62.63 61.96 38.95 134.60 72.45 6 0. 90 76.87 91.99  14 15 16 17 18 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 0 1 2 3 4 5 6 7 8 9 10 11 1 2 3 4 5 6 7 8 9 10 1 1 12 13 14 15 16 17 18 19 20 21 22 23 1 2 3  6 6 6 6 6 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 8 8 8 8 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1 1 1  8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9  FO 44. 57 50. 93 45. 82 16.19* 7, 30* 64.44 9. 05* 6 5. 85 38. 56 53. 49 0. 00* 20.76* 38. 08 23. 18* 5.79* 14. 32* 28.15* 26.35* 25.19* 48.74 65. 93 84. 18 49.71 50. 70 23.78* 97. 39 17.63* 42. 34 29.64* 95. 28 40. 96 38. 43 63.63 67.30 108.75 62.75 55. 11 63. 62 66. 80 37.3 6 50.24 30.14* 26.08* 26.15* 82. 17 32.10* 12.81* 0. 00* 98.37 4. 00* 9. 77* 0. 00* 91.93 0.00* 68. 35 197.07 143.41 161. 81  FC 42. 45 48. 44 48. 16 22.90 15. 52 61. 94 19.62 68- 80 39.38 52. 80 17.46 19. 52 4 2- 37 19. 80 12-97 17. 84 30.65 28.76 27.75 4 5. 03 64. 48 84. 48 54.60 54. 48 22. 16 104.36 26. 01 44.77 24. 32 98. 95 46. 12 39.08 56. 88 62. 35 107- 30 61. 61 63.31 67- 23 66. 12 36- 19 44.98 30. 60 25. 47 12.91 87. 16 38. 84 13.78 20.24 104.30 10.53 2.77 3. 66 91. 11 3.47 65. 95 185- 37 137.25 158.74  H  K  L  4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15  1  1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3  9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9  FO 73.10 0.00* 51.31 179.29 107. 14 51. 53 61.54 188.25 49, 30 74.51 48.67 109.04 48.11 0. 00* 58.82 24.31* 59.00 100.24 46. 93 35.67 80.92 19.93* 115.31 92.38 79.00 69.47 67.79 52.84 28.47 44. 29 29.75 32.50 42-21 30.98 26.96* 25.88* 73.69 38. 13 49.69 21.74* 70.33 0-00* 36.48 77.94 44. 73 70.19 31.83 77.64 19.15* 95.96 28.51 49. 19 24.22* 104.17 20-37* 14.06* 37. 13 60.56  FC 71.01 16. 01 54.20 181.65 103. 32 50.05 60.99 189.04 52. 27 73.93 46.76 109.51 47.63 16.97 57. 45 27.97 57.67 98.49 46.90 34.15 78.51 17.89 109.56 9 2,48 79.95 67.02 67.41 56.15 29.98 45. 56 30.50 32-58 42.43 32.10 29-56 24.02 72-38 35.62 44-56 21.70 67.89 11-20 32.75 74.15 37.40 67.28 28,01 78.93 17.79 94.92 27.30 51-46 21.18 106-32 20.74 16.12 41. 18 60-74  H  K  L  16 17 18 19 20 21 22 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 1 2 3 4 5 6 7 8 9 10 11  3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 6 6 6 6  9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9  FO 23.82* 26. 74 15.96* 12-89* 31.64 47.40 8. 66* 27.24 17.88* 39. 58 33. 32 44. 57 20.59* 16.26* 44. 63 41. 15 30. 46 34. 08 63. 03 56. 39 20.03* 42. 81 30- 28 81. 34 35. 45 52. 79 0. 00* 58. 55 125. 46 51.78 107. 13 58. 53 43- 95 97.31 108.09 20.81* 78. 30 78. 03 132.63 40- 87 90.95 33. 08 54.35 49.75 35.37 0. 00* 15.82* 38. 06 40.39 59. 22 33. 52 27. 48 36.21 24. 28* 33. 19 45. 62 36.49 28.51*  FC 23- 52 24. 89 17. 75 13. 93 33- 07 44. 34 8. 71 27. 17 14. 24 42- 61 33. 60 44. 99 24. 33 16. 91 40. 79 40. 93 32. 34 33- 94 62. 35 60. 89 9. 50 43. 39 30. 11 85. 40 36. 13 50. 76 4. 86 53. 56 125. 52 53. 58 106. 70 57. 81 44. 29 100. 55 112. 11 14. 07 80. 69 84. 15 131. 22 36. 62 86. 42 34. 72 54- 52 47. 35 34. 49 13. 94 19. 19 32. 16 39. 86 56- 63 33. 37 24- 31 35. 78 21. 00 36- 93 50. 44 3 7 . '20 31. 47  H  K  L  12 13 14 15 16 0 1 2 3 4 5 6 7 8 9 10 11 12 13 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 1 2 3 4 5 6 7 8  6 6 6 6 6 7 7 7 7 7 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1 1 1 1 1 1 1 1  9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10  FO 22.27* 57.27 15.35* 31.73 20.50* 51.64 96.06 28.11* 90.55 23.49* 28.06* 19.43* 96.43 23.25* 23.77* 3. 16* 108.69 29.28 48. 49 51.00 27.75* 50.72 40.65 35.38 39.00 38. 42 28.83* 124.64 63. 12 125.57 47. 31 83 . 96 70. 24 75.51 34. 06 93.72 84.56 88. 90 22.41* 1 11.72 68.36 1 14.81 19.35* 12.33* 0.00* 82.41 38. 52 14. 1 1* 0.00* 110.41 58.54 68.59 107.95 40.74 74. 92 80, 97 22.13* 22.34*  FC  H  K  L  23. 24 59.71 11.97 31.54 8.27 53. 11 95. 55 24.48 90.90 28.61 28.57 14.76 96.47 18.55 29.42 6.70 109.02 27.26 49.21 52. 20 30. 43 50.76 39. 26 33.25 31.79 43.01 29.94 114.87 60.90 126.05 45.64 83. 11 68.80 79.01 29.65 90. 46 87.00 90.62 4.30 110.74 71.64 1 14.90 14.80 8.92 2.34 80.93 38.71 16.26 38.46 108.04 59. 12 66.07 99.04 39.21 70.94 78.63 15.47 24. 60  9 10 11 12 13 14 15 16 17 18 19 20 21 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 0 1 2  1 1 1 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 4 4 4  10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10  FO  FC  9, 45* 3. 46 83.50 82. 06 54.79 54. 80 21.04* 23.25 24.34* 24.75 53. 24 46. 84 64.63 59.25 52. 44 52, 51 49. 36 47, 99 23.35* 23. 07 57. 45 54.77 47. 03 46.23 15.59* 12. 80 157.10 149.66 58.39 56. 99 47. 96 47. 99 51. 74 4 7, 79 54. 65 52.30 105. 23 101. 25 19.61* 17. 68 40. 22 39. 26 43. 49 39. 48 90. 05 91. 92 50. 81 49. 34 40.39 40. 73 50. 59 52.29 96. 81 92. 79 70. 61 72- 50 49. 46 52. 34 27. 88 28.78 49.71 51.30 49. 44 44.71 15.85* 14. 48 20.05* 16. 92 40.30 37. 68 70. 10 70.35 38.89 35. 32 68.68 69.37 34.09 32- 46 50.06 53. 23 50. 13 50. 48 34. 72 31.77 48. 14 49. 74 16. 60 0. 00* 51. 12 52. 45 37. 49 38. 99 18.30* 15. 43 24.15* 2 5. 15 27.76* 29. 82 25. 17* 26. 08 30.69 32.81 49.96 52. 42 24.77* 20. 42 46. 10 45. 48 30. 79 26. 69 153.40 155,62 50. 96 57. 63 74. 74 66-46  H  K  L  3  4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 7 7 7 7 7 7 7 7 7  10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10  n  5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 1 2 3 4 5 6 7 8 9  FO 21. 01* 92. 77 5 5 . 12 2 5 . 84* 5 7 . 16 1 16. 59 5 9 . 23 66. 4 3 5. 7 2 * 106. 36 4 8 . 43 7 6 . 31 3 3 . 42 21. 75* 26. 35* 4 7 . 51 22. 79* 4 6 . 96 24. 64* 4 9 . 14 2 8 . 51 0. 0 0 * 6 4 . 43 28. 77 20. 72* 5 3 . 82 80- 78 6 1 . 24 8. 3 3 * 29. 93* 7 3 . 03 3 4 . 12 4 7 . 70 4 2 . 71 129. 32 5 3 . 36 83. 18 3 4 . 58 8 8 . 42 3 5 . 42 4 5 . 95 52. 35 7 6 . 22 48. 04 7 8 . 39 . 4 0 .31 6 5 . 73 3 8 . 31 8 0 . 20 4 4 . 30 18. 7 3 * 4 7 . 19 3 9 . 68 48. 24 5 2 . 38 23. 23* 22. 59* 26. 85*  FC  H  K  L  6.64 95.95 51.44 19.20 57.78 120.03 59.01 65.32 13. 47 104.94 4 4 . 45 77.86 34.44 20.03 13.23 4 8 . 14 14.02 45.39 2 1 . 19 44.61 25.68 7.23 61.33 29.85 21-23 5 2 . 58 75.98 56.79 18.53 36.74 71.29 33.36 43.96 4 2 . 06 125-48 5 4 . 52 82-52 32.61 8 5 . 12 39-34 44- 46 5 4 . 33 7 7 . 61 44.39 7 8 . 83 4 3 . 72 62.65 39.88 80.06 46.73 29-54 4 7 . 23 39.91 4 7 . 37 48.89 19.06 19-31 2 2 . 56  10 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17  7 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0  10 11 11 11 11 11 11 11 11  1 1 1 1 1 1 1 1 1 1 1 1 1 1 1  11  1  1  1 1 1 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2  11 11 11 11 11 11 11 11  11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11  FO 3 6 . 13 19.69* 25.87* 7. 4 1 * 55.56 5 8 . 81 23.15* 21. 25* 6 9 . 83 3 9 . 83 20.38* 65.74 10 4. 19 28.48* 29.44* 66. 55 3 7 . 82 20.04* 50.26 24.73* 6. 16* 66.61 4 1 . 89 106.57 4 4 . 97 20.30* 43.26 3 1 . 40 26-71 21.05* 6 5 . 25 6 9 . 16 8. 10* 110.40 53. 5 1 5.54* 21.39* 75.07 18- 5 8 * 46.62 38.34 6 4 . 56 26.78* 4 9 . 59 5 1 . 32 63- 97 29- 19 2 7 . 41 6 2 . 13 0. 0 0 * 38.34 3 1 . 83 59.47 8.96* 19,20* 64.38 0. 0 0 * 20.15*  PC 34- 88 20. 42 2 2 . 67 1. 25 5 3 . 74 6 0 . 61 3 0 . 93 2 4 . 26 6 8 . 06 4 2 . 52 2 0 . 62 6 3 . 92 10 3. 26 2 7 . 32 2 2 . 97 6 9 . 62 4 2 . 67 2 4 . 61 4 9 . 35 2 4 . 30 2 3 . 02 6 0 . 65 3 7 . 48 1 0 1 . 89 3 9 . 81 18. 47 4 2 . 43 3 2 - 48 2 1 . 06 2 3 . 90 6 5 . 47 7 0 . 54 10. 24 1 0 9 . 68 5 3 . 23 2 0 . 21 16. 59 7 2 . 68 2 2 . 54 4 3 . 03 3 5 . 75 6 2 . 83 3 1 . 11 5 1 . 82 4 8 . 69 6 1 . 46 2 9 . 51 2 4 . 47 64- 67 10. 97 3 3 . 22 2 9 . 44 5 9 - 73 1 0 . 30 13. 74 6 4 . 07 1 3 , 90 1 5 . 90  H  K  L  18 19 0 1 ' 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 1 2 3 4 5 6  2 2 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 6 6 6 6 6 6  11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11  FO  FC  25.97* 27.05 40.22 37.29 39.99 39.35 29.16 26. 42 141.77 140.43 31.06 32.55 33.14 28.77 51.89 51.67 63.41 59. 19 15.09* 7. 17 26.34* 23. 18 59.60 58. 14 79.15 74.45 24.41* 18.32 85.95 85.58 70.33 70.32 38.51 36.28 31.88 25.78 57.64 54. 28 52.91 51. 37 10.94* 8. 17 72.03 74.36 20.09* 27.53 36.47 37.70 57.65 56.35 47.17 48. 98 27.81 26.41 22.70* 20. 28 70.45 67.82 37.59 38.02 0.00* 16.83 50,68 51.12 69.60 63.79 14.75* 13.48 19.91* 10.04 47.00 42.01 27.71* 26.31 80.84 74. 30 83.08 84.49 144.67 144.67 57.16 57.08 46.18 42. 22 92.07 97.47 70.04 66.43 31.83 26.73 60.61 58. 28 82.46 85.33 87.87 91. 44 51.34 50.83 96.48 98.50 58.12 61.08 37.14 43.58 48.52 52.43 20.99* 20. 11 38.45 41.20 44.26 46. 30 37.07. 39. 51 38.86 39.13  H  K  L  7 8 9 10 11 0 1 2 3 4 5 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 0 1 2 3 4 5 6 7 8 9 10 11  6 6 6 6 6 7 7 7 7 7 7 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 2 2 2  11 11 11 11 11 11 11 11 11 11 11 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12  FO 14.74* 42. 50 15.13* 27. 97 32.76 32. 09 10.67* 49.40 31. 09 11.93* 16.62* 88.21 70. 03 43. 68 66. 44 34. 50 18.26* 18.87* 48. 22 32. 10 30.88* 31.67* 70. 94 40. 88 60.68 78. 70 40. 48 69. 87 22.83* 23,61* 19.53* 26.25* 50. 87 17.65* 31. 41 11. 56* 42.95 52. 54 79. 88 21.85* 57. 61 54.97 40. 04 15.31* 16.85* 46. 62 77.73 98. 98 79. 41 62. 60 58. 87 32.70 40. 40 55. 41 72.35 51.70 20. 47* 94.30  FC 4. 39 43. 83 1 1. 98 25. 16 32.63 30. 90 11. 56 49. 25 27. 54 18. 94 8. 52 89.30 70. 34 42. 48 6 4. 27 32.61 11.77 33. 37 49. 22 30.30 26. 55 29. 10 68.46 37. 62 61. 34 79.78 42- 06 65.79 10.65 26. 30 14. 09 26. 28 54. 19 7.27 32. 27 4. 12 44. 74 52. 29 76. 40 19. 19 56. 60 58.87 39. 92 7- 67 13-36 46. 90 75. 96 98.66 78- 45 60.74 58- 06 31.21 38. 82 50.56 73.33 50. 91 10-71 95. 10  H  K  L  12 13 14 15 16 17 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 0 1 2 3 4 5 6 7 8 9 10 1 1 12 13 14 1 2 3 4 5 6 7 8 9 10 11 0 1 2 3 4 5 6 1 2 3 4  2 2 2 2 2 2 3 3 3 3 3 3 3  12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 13 13 13 13  3  3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 5 5 5  5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 0 0 0 0  FO 49. 06 41. 90 53. 01 68. 89 58. 11 23. 51* 41. 74 33. 5 8 72. 59 33. 58 26. 99 53. 74 35. 66 8. 36* 28. 14* 57. 51 27. 70* 30. 84 46. 65 28. 72* 20. 19* 125. 23 126. 89 51. 70 101. 46 75. 76 57. 12 39. 29 87. 71 40. 69 77. 19 22. 68* 1 15.31 22. 37* 71. 80 47. 00 36. 49 31. 96 45. 66 55. 62 19. 91* 46. 69 18. 98* 37. 44 39. 34 56. 51 0. 00* 60. 14 69. 38 50. 65 39. 34 16. 13* 29. 11 24. 96* 0. 00* 40. 36 18. 92* 28. 41*  FC  H  K  L  49.47 40. 41 55.87 68.70 56. 41 14. 07 45.93 29.27 73.49 35. 56 24.45 52. 47 37.33 12.63 25. 47 57.77 26. 10 31.41 45.95 3 1 . 15 28.61 124.80 125.94 53. 52 100. 10 77. 50 56. 42 35.82 90.73 37. 96 73. 56 21.72 115.36 28.56 69.04 42.79 30.50 33.26 40.04 54.03 7.39 42. 92 12. 52 39. 16 41.59 55. 85 9.49 55. 80 68.89 50.29 38. 11 16.02 24. 54 27.36 0. 46 42. 40 0.80 25.74  5 6 7 8 9 10 11 12 13 14 15 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 1 2 3 4 5 6 7 8 9 10 11 12 13 14 0 1 2  0 0 0 0 0 0 0 0 0 0 0 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 3 3 3 4 4 4 4 4  13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13  3  4 5 6 7 8 9 10 11 12 1 2 3 4 5  FO  FC  21.97* 6. 37 47.39 42. 72 51.61 51. 75 60. 03 59. 06 35. 46 35. 91 57.32 59. 35 45. 83 43. 61 46. 06 45. 84 23.08* 17. 30 64.60 64. 08 20. 93 23.92* 147. 71 142.19 84. 18 84. 00 31.28 25. 22 58. 47 54. 64 80.31 81. 12 59.21 61. 28 37.39 39. 56 50. 30 52. 91 52. 03 4 9- 78 56. 96 55.42 73.99 74. 72 76. 95 75. 19 16.29* 4. 13 54.51 56. 77 91.76 90. 10 36.69 36. 63 31. 96 30. 57 38.64 32. 10 21.46* 16. 28 23.70* 26- 59 30.78 31. 96 0.00* 6. 59 28. 18 25. 79 17- 36 24. 85* 52.78 55. 71 32.57 31. 04 30. 68 30. 36 31.00 26. 47 65.37 66. 38 118. 76 119. 58 79.55 77. 46 22.45* 31. 25 66. 54 66. 79 83. 02 82- 29 40.33 41- 59 36. 98 36- 36 36. 18 33- 74 56.92 59. 57 64.04 65. 10 56. 48 56. 15 57. 64 56.65 25-77* 25. 10 33. 86 28. 10 46.20 44. 62 16.90* 21- 65 21.37* 26. 94 37. 97 43. 56  H  K  6 7 8 9 10 0 1 2 3 4 5 6 0 2 3 4 5 6 7 8 9 10 11 1 2 3 4 5 6 7 8  4 4 4 4 4 5 5 5 5 5 5 5 0 0 0 0 0 0 0 0 0 0 0 1 1 1 1 1 1 1 1  L  FO  FC  13 50. 60 47.09 13 0.00* 11.01 37. 43 13 32-68 25.69* 13 27.71 13 52.71 50.34 13 1 13.69 116.85 13 63. 51 63.77 13 53. 83 49.73 13 66. 36 67.94 13 60. 37 60. 41 13 29.02* 33.03 17.24* 13 23- 15 14 30,83* 22. 21 14 . 159. 19 162-28 14 12.20* 9.24 14 0. 00* 1 1.85 14 25.83* 13.78 14 53. 70 50-84 14 8. 19* 21. 71 14 36. 25 38-02 14 2.47 19.50* 14 32.53* 33.07 14 21.29* 20. 11 14 22.09* 18.64 14 30.56 21.43 14 7.68* 13-42 14 37.62 37-02 14 17.61* 5.94 14 20.73* 17.88 14 8. 38* 14.98 14 41. 38 37. 11  * DENOTES AN UNOBSERVED  H  K  L  9 10 1 1 0 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 0 1 2 1 2 3 4 0 1 2 3  1 1 1 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 4 4 4 0 0 0 0 1 1 1 1  14 14 14 1.4 14 14 14 14 14 14 14 14 14 14 14 14 14 14 14 14 14 14 14 15 15 15 15 15 15 15 15  REFLECTION  FO  FC  28.22* 26. 08 35. 12 29. 92 13.81* 22. 60 55.99 55. 33 35. 82 32.38 120.59 124-71 43. 18 48. 58 41. 13 43- 67 42. 78 38. 00 57. 05 61.03 35. 48 42. 21 48. 92 53. 94 41. 1 1 43. 21 33.45 31.37 15.22* 13. 50 8.52* 8.90 41.00 37. 37 34.22 31.76 0. 00* 6. 17 10.46* 17. 52 26.05* 24- 77 40. 09 35. 15 107. 89 109-38 37. 48 38. 85 28. 89* 24. 62 15. 94* 13. 05 26.90* 24. 33 1 18,59 122. 43 67. 28 67.44 40. 12 3 8. 59 50.36 47.71  20  1 , 3 , 7 - T r i m e t h y l - 2 , 6 - d i o x y p u r i n e H y d r o c h l o r i d e Dihydrate ( C a f f e i n e H y d r o c h l o r i d e Dihydrate) Anthony Mercer and Observed and  calculated  James T r o t t e r . structure  amplitudes  ( r e f l e c t i o n s with i n t e n s i t y < 3«sr(T) are marked with an asterisk) . The f o l l o w i n g planes which had |Fo-Fc|> 3 (F) were given zero weight i n the f i n a l stages of refinement due to suspected instrumental errors. Fo  1 0 • 1 4 7  5  )  Fc  Fo  Fc  2 70.72 91.91  1  2  16  3. 87 0 . 9 3  2  6. 87  3  6  12  4. 22  4  4.78 0. 20  0. 36  1. 2C  H  K  L  -13 -13 -13 -13 -13 -13 -13 -13 -12 -12 -12 -12 -12 -12 -12 -12 -12 -11 -11 -11 -11 -11 -11 -11 -11 -11 -10 -10 -10 -10 -10 -10 -10 -10 -10 -9 -9 -9 -9 -9 -9 -9 -9 -9 -8 -8 -8 -8 -8 -8 -8 -8 -8 -7 -7 -7 -7 -7  0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0  2 4 6 8 10 12 14 16 2 4 6 8 10 12 14 16 18 2 4 6 8 10 12 14 16 18 2 4 6 8 10 12 14 16 18 2 4 6 8 10 12 14 16 18 2 4 6 8 10 12 14 16 18 2 4 6 8 10  FO  FC  10.05 9.88 8. 14 8.34 7.66 7.79 12.23 12.89 11. 23 12.00 9.62 10.06 14.30 13.42 8. 44 8.62 6.94 6. 99 15. 55 15.51 16.58 16.18 14. 4 2 15.75 3. 51* 4.77 13. 95 13.85 7. 32 7. 40 0.95* 1.17 18.60 20.11 8. 13 7.29 6.23 5.64 16. 67 16.79 10.88 11.57 10. 36 10.67 24.26 24. 19 10. 93 11. 23 9. 92 9.40 6. 14 6.11 11.10 10.69 3.35* 1.53 12.68 13.33 4. 34 5.0 2 16.47 17. 06 4.51 4.07 11. 32 11. 54 12.93 13.85 4.91 4.70 10.63 10.46 31. 79 32. 17 3.25 2. 43 28. 52 2 8.51 7. 23 6.82 4.37 3. 23 19.88 2 0.48 14.73 15.51 20.02 19.78 3. 41 4. 10 34. 93 36. 94 3.54 3. 96 6.02 5.97 3. 69 1.95 19.78 20.08 2.66* 1.83 18.53 19.29 12.39 12.30 19. 17 19.88 38.70 39.06 1. 34* 0.82 24.63 24.35 53. 74 54.29  WEIGHT  H  K  5.67 5,44 5.72 4.92 5. 11 6. 05 4. 15 5.92 6. 37 3. 75 3.68 4. 20 0.23 4. 35 5. 42 0.03 2.79 6.24 7.01 3. 50 4.50 4. 89 2.04 5. 95 6.57 6. 01 5.01 0. 33 4. 97 3. 46 3. 99 5.50 5. 80 4. 59 4. 18 6.22 1. 34 3. 95 1.60 7.41 3. 33 2.94 3.86 2. 83 3.91 1. 13 6. 21 7.71 6. 87 2.92 0.15 3.20 4.87 3. 18 0. 95 0. 10 2.13 0.50  -7 -7 -7 -7 -6 -6 -6 -6 -6 -6 -6 -6 -6 -5 -5 -5 -5 -5 -5 -5 -5 -5 -4 -4 -4 -4 -4 -4 -4 -4 -4 -3 -3 -3 -3 -3 -3 -3 -3 -3 -2 -2 -2 -2 -2 -2 -2 -2 -2 -1 -1 -1 -1 -1 -1  0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0  -1 0  L  FO  FC  WEIGHT  12 22.77 23. 75 2. 43 14 21.90 22. 56 2.41 16 2. 11* 1. 24 0. 12 18 8.15 7. 54 6.53 2 14.14 14. 63 5.24 4 64.77 66. 43 0. 35 4.34 6 4. 81 5.94 8 32.95 33. 54 1.30 10 22.36 22. 22 2. 54 11.79 11. 80 4. 82 12 14 24.37 24.45 2.08 16 22.89 23. 11 2. 38 18 6.79 6. 58 6.04 2 20.45 20. 14 3. 06 4 41.05 41. 75 0. 86 6 6.11 6. 05 8. 19 8 3.86 4. 33 6. 30 10 32.63 30. 23 1. 23 12 20.41 20. 09 2.94 14 27.16 27. 61 1.72 3.26 16 4.12 5.05 6.75 18 6. 65 5.06 2 44.36 45.75 0.74 4 4.57 11. 84 4.31 6 34.72 35.47 1.18 8 86.04 87. 24 0. 20 10 33.24 33. 44 1.27 12 18. 81 19. 16 3. 39 14 19.34 19. 09 3. 13 16 3.26* 0. 70 0.36 18 5,48 4. 86 5. 35 2 72.30 73. 10 0. 28 4 37.51 36. 99 1.03 6 78.09 79. 28 0. 24 8 20.26 20.56 3. 04 10 15.46 14. 86 4. 63 1.50* 12 1. 61 0. 09 14 21 .49 21. 09 2.75 16 6. 45 4. 33 6.28 18 17.82 17. 52 3.55 2 1. 84* 0. 72 0. 60 4 47 . 36 52. 90 0.59 6 32.74 32. 20 1.33 8 6.31 6. 91 8. 53 10 2.80* 2.42 0. 39 7.64 7. 10 7.14 12 14 8. 85 6.55 8.78 16 10.30 9. 58 6. 93 18 4.12 4. 09 3.49 4 3.55 3. 61 10.71 6 112.12 117.39 0. 12 8 24.86 25. 11 2. 16 10 39. 15 39. 24 0. 94 12 4.20 3. 73 5. 01 14 22.83 23. 73 2. 28 16 8.24 7. 30 6.29 18 5.36 4. 56 5.6 3 2 52.74 50. 94 0.52  H  K  0 0 0 0 0 0 0 0 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 4  0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0  4 4 4 4 4 4 5 5 5 5 5 5 5 6 6 6 6 6 6 6 7 ^7  L  FO  FC  WEIGHT  4 15. 5 8 14.94 3. 55 6 50.51 51.12 0.55 8 34. 36 32.73 1.16 10 34. 33 3 2.48 1.18 12 36.91 35.04 1.02 14 45. 24 44.42 0.69 16 8.74 8.01 4. 47 7.71 18 7.10 7.41 0 9.31 9.95 2. 10 2 8. 85 6.89 4.91 4 74. 64 74.39 0.27 6 30.66 29.44 1.48 8 3.64 5.47 3.97 10 46. 32 45. 92 0.68 12 33. 14 32. 58 1. 25 14 15.49 3. 89 15.48 16 7.70 7.46 6. 22 0 72.67 72.05 0. 27 2 36. 94 36.31 1.05 4 63.60 62.55 0.36 6 23. 62 2 5. 28 2.34 8 12.50 11.91 5. 58 10 8.64 8.43 5.76 12 9.98 9. 93 5.39 14 5.86 4.06 6. 88 16 6.74 6.00 7.05 0 108. 82 96.59 0.13 2 20. 69 18.99 2. 95 4 19. 82 19.22 3.17 6 17.44 17. 65 3.76 8 9.57 8.62 7. 18 10 5.51 5. 34 3.59 12 23. 13 21.02 2. 34 14 12.97 12. 28 5. 25 0 6. 49 7.70 3.03 2 8. 25 8. 30 8.75 4 31. 39 30. 74 1.40 6 26.59 26. 33 1.85 8 24.63 24. 11 2. 12 10 28.99 28.21 1. 53 12 21. 67 20. 56 2.46 14 4. 84 3.49 6.25 0 21.88 20. 92 2. 61 2 89.93 83.51 0. 18 4 20. 84 19.48 2. 86 6 6. 06 5. 83 6.02 8 3. 44* 2. 87 0.23 10 4.74 4.91 4.00 12 10. 53 10.70 5.39 14.09 0 14.36 4.90 2 20.34 20.03 2.96 4 27. 68 26.86 1.76 6 23.32 24.00 2. 20 8 2. 49* 1.52 0.15 10 9. 30 6.37 8.76 12 2. 61* 1.02 0. 22 0 14. 37 14.52 4. 98 2 21. 09 19.26 2.75  H  K  L  7 0 4 7 0 6 7 0 8 7 0 10 8 0 0 8 0 2 8 0 4 8 0 6 8 0 8 8 0 10 9 0 0 9 0 2 9 0 4 9 0 6 9 0 8 10 0 0 10 0 2 10 0 4 10 0 6 11 0 0 11 0 2 11 0 4 12 0 0 12 0 2 13 0 0 1 1 -13 1 -13 2 1 - 13 3 1 4 -13 1 5 -13 1 -13 6 1 - 13 7 1 8 -13 1 9 -13 1 10 -13 1 11 - 13 1 12 -13 1 13 -13 1 14 -13 1 15 -13 1 16 -13 1 17 -13 1 1 -12 1 2 -12 -12 - 1 3 1 4 -12 1 5 -12 1 6 -12 1 7 -12 1 8 -12 1 -12 9 1 10 -12 1 11 -12 1 12 -12 1 13 -12 1 14 -12 1 15 -12 1 16 -12  FO 27.69 16.17 0.00* 11.62 7.03 29.22 12. 26 13.65 4. 11 3.14* 19.54 10.11 1.91* 15.44 2.46* 6. 19 0.00* 3.16* 2.49* 4.34 19. 14 1.98* 2.32* 6.39 2.88* 2.17* 7.90 1.55* 6.05 7.97 6.04 3.62 4.09 6.66 3.33* 15.72 7.75 9.65 8.67 5.52 4.60 6.91 4.84 1 .37* 2. 18* 2.72* 8.24 4.84 7.95 3.65 7.07 6.61 3.29* 7.30 5.87 8.18 8.56 3.44  FC  WEIGHT  26. 79 1.72 16.77 3.56 0. 92 0. 00 10. 73 5.55 6.02 6.69 28.45 1.53 12. 64 4.28 12. 86 4. 64 4. 09 3. 12 2.65 0.33 19. 39 2. 97 10.14 5.36 0. 23 0.09 14.60 4.11 2. 32 0. 18 6. 29 4. 21 0. 88 0. 00 0.43 0.40 0.59 0.28 4.09 2.70 18. 24 2.98 1.63 0.11 1.23 0.18 6. 72 7. 10 2. 63 0. 26 2.49 0.14 7.89 6.10 0.18 0.07 6. 57 4.28 8. 50 4.46 5. 47 5.79 0.57 4.28 3. 59 3. 54 6.83 4.93 0.70 0.29 17. 03 3.46 7. 85 5.73 9.77 6.13 9.06 5.65 6.35 4.46 4. 90 4.03 7,06 6.16 3.69 6.50 0.03 0.06 1. 74 0. 10 0.52 0.19 8. 05 5. 17 3.49 3.96 9.39 3.63 1. 66 3.75 6. 61 5.66 6.19 6.98 2. 34 0.25 6. 53 5. 92 5. 08 6. 85 8. 27 5.48 7.80 8.14 0. 70 4. 64  H 12 12 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -8 -8  K  I  1 17 1 18 1 1 1 2 1 3 1 4 1 5 1 6 1 7 1 8 1 9 1 10 1 11 1 12 1 13 1 14 1 15 1 16 1 17 1 18 1 1 1 2 1 3 1 4 1 5 1 6 1 7 1 8 1 9 1 10 1 11 1 12 113 1 14 1 15 1 16 1 17 1 18 1 1 1 2 1 3 1 4 1 5 1 6 1 7 1 8 1 9 1 10 1 11 1 12 1 13 1 14 1 15 1 16 1 17 1 18 1 1 1 2  FO  FC  3. 06* 1.87 6. 05 6.03 11.79 11. 13 4. 80 4.14 2.44* 0.99 11.22 11.12 11.31 11.97 4. 56 5.94 9.06 9.12 3. 34 1.82 3.78 1.23 2.51* 1.14 4.68 2.82 5.44 5. 82 13.32 13. 33 5. 92 5.76 9. 94 10.51 5. 21 3.59 10.53 10.88 5. 14 4.25 16.20 15.74 9.70 9.49 5.19 5.32 8.79 8.70 26. 04 25. 17 8. 30 8.81 14. 96 13.90 6.77 5.52 18.72 18.84 12.00 12.08 24. 72 25.78 2.24* 1.11 3. 30* 1.98 8. 25 7. 84 16.71 16.53 7.81 7.22 2. 38* 0.86 11. 40 11. 55 19. 66 19.49 2. 59* 3.59 13. 97 13. 34 2. 50* 1. 96 4.00 3.23 13. 20 12.40 17.55 17.55 8.50 7.27 12. 57 14. 17 16. 01 16. 20 11.61 1 1. 09 7.41 7.46 4. 32 4.35 5. 28 4.66 15.65 15.38 12.32 12.33 10.98 10.94 3. 38* 2.31 16. 66 15.84 4. 48 3.80  WEIGHT  H  K  L  0.26 5. 96 6. 21 3.83 0.14 4. 64 4.72 2.42 5.39 3. 47 4. 15 0. 16 5.29 4. 89 4.71 3. 38 4.94 6.75 5.06 6.50 3.55 6.26 4.83 5.07 1.85 5.16 4. 23 6. 37 3.13 4. 86 2.01 0.14 0.26 5,14 3.79 4. 30 0. 16 5. 82 2.84 0. 13 4. 64 0. 18 3.55 5.34 3.55 6. 46 5.08 3. 80 5.42 5. 17 2.71 4.26 4.23 5. 33 5.29 0.31 3. 85 4.88  -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -5 -5 -5 -5 -5 -5  1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1  3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 1 2  1  1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1  3  4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 1 2 3 4 5 6  FO  FC  8.08 8. 66 26.71 25. 01 18.40 18. 75 10.89 10. 26 12.72 12. 84 0. 74* 2. 17 8,04 8. 25 28. 12 27. 37 23.64 23. 50 1.44* 3. 37 8.87 9. 51 16.74 16. 91 5.57 4.53 16.63 16. 90 4. 14 1. 94 3, 88 4. 29 24.72 23.64 18. 80 18. 56 13.86 13. 97 9.18 8. 89 27 . 93 28. 80 12.56 12. 40 4.93 5. 09 29.21 29. 05 13.58 13. 05 18.00 18. 22 25.24 25. 89 8.04 8. 14 9.43 9.59 3,81 2. 51 13.33 12. 93 7. 85 8. 19 2.46* 1. 09 6.45 6. 05 34.05 32.91 27.72 27. 49 48.63 46. 29 15.84 15.81 16.17 16. 21 11. 17 11. 60 44.28 46. 90 2. 13* 1. 60 11.41 10. 53 13.46 11.94 3.61 3. 76 1.83* 0. 49 14.39 13. 97 3.34* 1. 22 21.53 22. 11 7.38 6. 75 16.63 17. 04 6.67 6. 37 23.27 22. 58 12.00 11. 88 23.86 24.50 16. 12 15. 28 16. 10 16. 32 6.28 6. 11  WEIGHT 6.78 1. 86 3. 37 5.70 6.00 0.02 6.37 1.65 2. 26 0. 04 4. 92 3.57 4. 48 3.54 3.76 2.64 2. 11 3. 32 4. 86 7. 45 1.74 5.98 6. 10 1.60 5.55 3.55 2.00 6.62 6.10 3.26 4.75 5.04 0. 16 6. 04 1. 20 1.75 0.61 4.28 4. 39 6.83 0.73 0. 23 6. 68 5.41 4. 11 0.12 4.54 0. 35 2.68 7. 29 3.65 6. 14 2.42 6. 40 2.30 4.48 4. 43 8. 25  H  K  5 5 5 5 5 5 5 5 5 5 5 5 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 2 2 2 2 2 2 2 2 2 2  1  1 1 1 1 1 1 1  1 1 1 1 1 1 1 1 1 1 1 1  1 1 1 1 1 1 1 1 1 1 1 1 1 1  1 1 1 1 1 1  1 1 1 1 1 1 1 1 1  1 1 1 1 1 1 1 1 1  I  FO  FC  WEIGHT  H  K  L  7 31.71 3 2.24 1.38 8 13.06 13. 11 5.74 9 7.70 6.73 8.34 10 15. 24 15. 16 4.61 11 19.93 20.23 3. 08 12 4.54 4.55 4.65 13 7. 90 7.79 6.16 14 3. 26* 3.35 0.22 15 10. 28 10.45 5.96 16 14.10 13.58 4.73 17 15.37 15.00 4.11 18 4. 64 2.84 5.70 1 48. 32 48.82 0.63 2 116.47 115.24 0.11 3 39.41 3 8.98 0.94 4 39. 68 3 7.42 0.93 5 7. 19 7.71 10.56 6 33.43 33.31 1.26 7 54. 85 56.98 0.49 8 6.40 6.72 8.63 14.67 9 14.83 5.07 10 28. 00 26. 18 1.77 11 36. 66 37.75 1.04 12 20.59 20.87 2.93 13 3. 00* 3. 47 0. 23 14 11.61 10.88 5. 90 15 17. 15 17.50 3. 49 16 2.68* 3.02 0.13 17 12. 61 11.72 5. 38 18 1.75* 2. 80 0.07 1 176.28 177.91 0.05 2 25.74 23. 28 2. 11 3 75. 86 73. 93 0. 26 4 37.51 38.48 1.02 5 18.74 18. 1 1 3.79 6 25. 19 25.02 2. 15 7 41.41 42.89 0. 84 8 8. 82 8.28 7.46 9 14. 82 13.61 5. 01 10 20.95 19.77 2.88 11 29. 82 30.73 1. 53 12 20.75 20.47 2.87 13 7. 56 7.73 5.95 14 21. 57 21.51 2.49 15 26. 04 26.40 1.87 16 16.43 15.99 4.02 17 9.56 8. 96 5.45 18 6.70 7.22 5.68 1 45.08 4 2.71 0.71 2 25. 67 25.46 1.81 3 37. 12 38. 85 1.07 4 40. 01 41.41 0.91 5 43.00 44.63 0.78 6 20.76 19.59 3.06 7 4. 12 2.86 6.23 8 8.53 9.73 7.41 9 15.24 13.76 5.05 10 22.4 2 21.51 2.53  -2 -2 -2 -2 -2 -2 -2 -2 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1 1 1 1 1 1 1 1 1 1 1 1 1 1  1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1  11 12 13 14 15 16 17 18 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 0 1 2 3 4 5 6 7 8 9 10 11 12 13  FO  FC  WEIGHT  38.37 38. 72 0. 97 2.38* 0. 17 0.23 34.38 34. 34 1.18 14. 10 14.53 4. 52 4.89 4.56 3.04 1.84* 1. 28 0. 09 9.51 9.73 5. 66 • 5.73 5. 35 6.48 48.57 42. 93 0.61 28.53 29.52 1.41 28.89 31. 86 1.63 22.08 24. 75 2.74 47.80 53. 23 0.63 8. 55 8. 21 9. 79 51.29 56. 06 0. 55 24.70 24. 91 •2 • 2 2 5.21 4. 29 8.49 10. 51 7.04 10,87 2.14* 1.94 0. 19 3.61 2. 04 5. 65 4. 54 6. 17 2. 93 15.13 15.75 4. 30 9.51 9. 52 5. 51 1.94* 0. 28 0.11 7.25 7. 05 7. 28 3.50 2. 04 4.64 27.60 30. 18 1. 75 21 .13 24. 22 2.96 6.63 7. 25 1 3.99 14.79 16.73 5. 12 3.03 2.72 6.29 37.51 40. 34 1.02 41.99 43. 75 0.82 20.48 21.05 3. 04 19. 87 20. 38 3. 25 12.67 14. 12 5.55 9.56 10. 29 5. 27 23.24 23.87 2. 36 8.26 7. 81 7. 81 10.44 10. 72 6.10 4.04 2.58 4. 80 1 .97* 0.71 0. 13 8.46 8. 27 7.18 4.05 3. 29 7.36 83.54 82.22 0.21 20. 83 21. 18 3. 13 11.74 12. 28 7.72 63. 58 69. 94 0. 36 49.91 53.45 0,58 8.04 8. 12 9.51 2.83 2. 08 5. 93 10.25 12.57 7.32 15.34 15.09 4.68 15.94 16. 38 4. 62 4.81 3. 10 5. 00 18. 13 18. 26 3. 44 3.54 5.76 6.89 16. 22 16. 19 3. 89  H 1 1 1 1 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3  3 3  3 3 •3 3  3 3 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 5 5 5 5 5 5  K  FO 14 15 16 17 0 1 2 3  4 5 6 7 8 9 10 11 12 13 14 15 16 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 0 1 2 3 4 5  FC  7. 24 6.92 3.08* 0.25 9.56 8.93 7.96 7,18 49.39 50.43 68.70 69.59 31.20 30.08 69.94 71.77 12.00 12.49 45.82 46.29 39.08 39.02 12.39 13.17 11.07 10.99 13.97 14.02 5.74 5.40 2.93* 2.01 17.23 16.81 9.35 9.85 6. 50 6.31 4. 52 3.57 3.70 2.61 129.16 129.05 12.58 12.43 34.71 35.71 20. 22 21.07 11. 49 11.47 6. 03 5.30 3. 79 2.53 38. 86 39.60 1.48* 0. 77 12.96 12.75 2.65* 0.48 23. 37 23.62 0. 00* 0. 40 22. 46 22. 24 3. 2 8* 3.39 3. 12* 2.23 42.74 42.21 0. 00* 1.10 16. 92 18.72 50. 24 50. 77 26. 10 26.67 12. 39 12.77 18.45 18.62 15.02 14.72 4.58 5.30 15.61 15.75 8. 24 8.32 0. 87* 1. 48 12. 70 11.96 6. 83 5.67 8.53 7.66 2.78* 1.33 3. 23 3. 33 9.69 9. 41 38.82 38.07 23.24 22.78 12. 09 12.53  WEIGHT  H  K  5.77 0. 36 7,32 8.06 0.61 0. 32 1. 45 0.30 7.03 0. 68 0.94 6.24 6.21 5.48 6. 17 0.24 3.46 6. 08 7.40 4.72 4.94 0.09 6. 80 1.18 3.11 6. 99 8.79 6. 21 0.95 0.08 5.64 0. 20 2.31 0.00 2.34 0.24 0.30 0. 80 0.01  5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 6 6 6 6 6 6 7 7 7 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 8 8 9 9 9 9 9 9 9 9 9 10 10 10 10 10 10  1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1  4. 16 0.58 1.95 5. 96 3.46 4. 81 3.71 4. 13 5. 97 0.02 4 .96 8.41 9. 80 0.48 3.90 8.72 0. 98 2. 50 5.91  I  6 7 8 9 10 11 12 13 0 1 2 3 4 5 6 7 8 9 10 1 11 1 12 1 0 1 1 1 2 1 3 1 4 1 5 1 6 1 7 1 8 1 9 1 10 1 11 1 0 1 1 2 1 1 3 1 4 1 5 1 6 1 7 1 8 1 9 1~ 0 1 1 1 2 1 3 1 4 5 1 1 6 1 7 1 8 1 0 1 1 1 2 1 3 1 4 1 5  FO  FC  5,66 21.08 8.22 5.53 6.29 3,26* 14.63 3.76 10.19 16.44 0.00* 7,12 4,91 6.41 7.00 16. 21 4. 15 2.87* 3. 28 10.96 0.00* 8.39 8,26 14.59 19.36 8. 24 14. 28 6.81 5,38 2.03* 17.46 4.87 2.47* 6.01 12.87 6.71 15. 30 5.67 3.93 4.82 3.51 2.76* 3. 84 9.01 9.36 8.10 5.44 9.09 8.89 3.45 6.64 5. 33 4.17 3.24* 6.03 12.53 3.43* 8,03  4.57 21. 36 8. 81 4.96 6. 02 2.33 14.71 3. 39 10. 86 16. 32 1. 17 5. 73 4. 30 6. 36 6.71 15. 73 2.90 0.83 0. 71 10.78 0.48 8. 40 7.77 14. 26 19.41 8. 48 14. 57 6. 64 4.94 0.50 17. 63 4.45 1, 04 5. 19 13. 13 6. 50 15. 00 5. 22 1. 97 3.63 1. 69 O.07 3. 96 8.72 9. 76 •8, 67 6. 09 9. 98 8. 66 0. 54 6.78 4. 35 2. 84 0. 34 6. 04 13.23 4. 18 8, 69  WEIGHT 6.51 2. 61 5. 30 4.54 5. 14 0.26 4.72 3. 67 7.58 4. 47 0.01 8.68 4.04 5. 42 6.20 3. 30 4. 46 0.29 3.61 5, 12 0.00 9.06 8.53 4. 89 3.08 5.79 4.81 5. 56 4.42 0,11 3. 58 4.54 0.25 5.72 4.64 6. 29 4.00 4. 82 4. 14 5.45 3.95 0.24 3. 68 6.50 6. 26 5.09 4. 47 6, 10 7.59 4. 26 5.29 8. 24 • 4,50 0.35 5.07 5.02 0. 24 6.49  H  K  I  10 11 11 11 11 11 12 12 12 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 11 11 11 11 11 11 11 11 11 11 11 11 11 11  1 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2  6 0 1 2 3 0 1 2 0 1 2 "3  5 6 7 8 9 10 11 12 13 14 15 16 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 1 2 3 4 5 6 7 8 9 10 11 12 13 14  FO  FC  WEIGHT  2. 80* 2.61 0.26 3.71 1.41 3. 95 7.32 7. 97 5. 13 5. 74 5.27 7.54 0. 00* 0.48 0.00 4.36 4.35 6.02 1.95* 1.90 0. 13 1.79* 2.32 0. 08 5.54 6.12 5.44 2. 82* 3.29 0. 26 5. 04 4.91 5. 59 1.43* 1.86 0. 06 3. 15* 1.91 0.37 10. 61 11.91 5. 30 3.25* 2.97 0.25 5.42 5. 96 , 4.48 3.26* 2.04 0. 30 1.63* 1.71 0.06 4.94 4. 24 6.66 0. 00* 0.29 0.00 1. 38* 1.42 0.06 11.97 12.39 5.25 6. 94 7.88 4. 50 6.5 3 6.80 6.27 3.11* 1.01 0. 40 5.06 5.89 5.26 2.46* 0.76 0. 20 10. 52 10.90 5. 84 2.37* 2.15 0. 16 6.44 5.29 5.67 1.59* 0.39 0.07 3.76* 4. 14 0. 24 2.74* 2. 24 0. 18 11.14 12.12 5. 20 4. 24 2.99 3. 34 5. 34 4.25 6. 12 8. 63 8. 83 6. 17 9.24 5.47 9.83 6. 15 5. 86 7.30 3.10* 0.98 0.39 2.35* 0.97 0.15 6. 68 7. 47 5.27 2. 19* 2.08 0. 13 2. 27* 0.83 0.23 7. 18 6.61 5.78 2.99* 3.47 0.15 3.86 4.33 2.73 3.96 2.40 4.01 4.74 3.19 5.07 3.06* 1.97 0.21 5.25 3.44 5.65 5.96 5.89 3.83 3.78 3.36 2.63 13.08 13. 12 4.64 5.00 4.4 9 3.93 24. 97 25.34 1. 97 3.78 1.81 3. 87 17.45 17.88 3.30  —  H  K  L  11  2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2  15 16 17 18 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18  - 11 - 11 - 11 - 10  - 10 - 10 - 10 - 10 10 - 10 - 10 - 10 - 10 - 10 10 - 10 - 10 10 - 10 - 10 - 10 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -g -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8  FO  FC  2. 12* 2. 00 4.39 3. 68 2.71* 1.74 6.69 7. 19 9.45 10. 06 7. 24 7.43 15.84 16. 03 16.84 17.02 2.01* 2. 16 8.16 7. 79 7.89 7. 91 21.62 22. 07 9.74 9.09 7.24 7. 06 13.25 14. 03 8.56 9.20 13. 88 14. 51 10.34 11. 12 4.26 2. 57 8.64 8.93 0.42* 2. 52 5.20 6.20 4.44 3.46 7.63 6. 96 11. 16 11. 56 16.63 16. 78 4.24 2. 80 3.41 2. 85 7.88 7. 57 20.58 22. 11 5.60 5. 15 17.58 17. 84 9.47 10. 28 16.07 16. 16 0.00* 0. 69 3.98 3. 01 2.26* 0. 04 2.66* 1. 53 5. 23 4. 35 9.11 9. 25 21.21 20.58 14.83 14. 69 6.70 6. 89 5.07 3. 42 8.18 7. 41 7.83 8. 17 4.02 3. 83 13.69 13. 75 4.54 4.91 4.39 3. 39 4.22 3. 01 19.11 20. 19 2. 64* 2. 07 21.64 22. 04 10.22 10.72 5.75 4. 93 4.90 3. 50 11.64 11.97  WEIGHT  0.13 4. 24 0. 26 6.01 4. 52 4.63 3.57 3.55 0,08 6.17 4.48 2. 38 5. 34 5.71 4. 64 5.00 4. 18 4. 65 4.78 5.60 0.00 5.00 3. 83 6.43 5. 10 3. 64 3.35 3. 15 5.98 2.71 5.51 3.22 4. 90 3.75 0.00 4. 13 0. 12 0. 18 6.63 6.39 2. 65 4.50 6. 48 5. 32 7. 15 8. 16 5.05 4. 68 3.40 3.67 4. 06 3. 22 0. 18 2. 57 5.11 6. 23 5.79 5. 63  B  K  I  7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 4 4 4 4  2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2  1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 1 2 3 4  FO  FC  19.97 18. 81 66.68 62. 92 41.49 40.07 47. 72 47.33 15. 24 14.72 27. 43 27.07 6.69 5.61 36.45 36.18 11.08 11. 14 3.01* 2.50 6.65 6.66 11.97 12. 56 6.43 5.42 6.78 5.99 7.54 7.40 21. 22 22.07 4.85 6. 15 13. 02 13.23 49.49 47.39 27. 15 26.35 13. 51 13.07 3. 18* 2.63 15. 15 13.43 11. 14 12. 05 9.04 7.97 27. 16 28.36 19.07 18.50 8. 67 8.25 11.91 11. 07 13.15 13. 11 13. 22 13. 86 24.40 24.69 17.76 18.54 17.24 17.78 3.81 2.95 6.66 7.45 5. 60 5.99 44. 41 41.33 49.20 44. 03 7.32 8.04 20. 94 20.72 4. 89 4.26 12.26 11.58 22. 36 23.02 8. 90 8.01 41.85 42.99 6.09 5.63 21.82 22. 87 23.87 24.37 14. 67 13.52 2.21* 2.49 15.79 15.67 4.40 3.98 16.64 15.81 19.44 17.59 55. 24 49.53 12.90 12. 36 76.55 73.12  HEIGHT  H  K  L  3.03 0. 33 0.82 0.63 4.62 1. 82 7.82 1. 05 6.47 0.27 4. 86 5.37 4.92 6.94 4.69 2.55 3. 17 4.76 0.58 1. 82 5.18 0. 36 4. 45 6.84 6.86 1. 80 3.27 6.45 5.39 4. 77 4.50 2.05 3.28 3.26 2. 78 4.23 8.51 0.73 0.60 7.80 2.94 7. 41 6.45 2. 53 8.23 0.82 6.05 2.47 2.21 4. 40 0.11 3.92 4. 84 4.01 3.24 0.48 5. 84 0.25  -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -1 -1 -1 -1 -1 -1 -1 -1  2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2  5 6 7 8 9 10 11 12 13 14 15 16 17 18 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 1 2 3 4 5 6 7 8  FO  FC  8.07 8. 49 1-2.92 12. 40 26.05 25. 17 10.48 11. 56 33.65 33. 18 18. 25 17. 48 8.11 7.81 6.43 6. 98 7.57 7.27 13.92 14. 62 6.05 6. 24 16.90 16.92 2.93* 1.60 9.41 8. 82 20.73 18. 12 16.07 16. 47 46.35 41. 54 7.85 8. 39 1.60* 0. 83 4.03 3. 40 11.61 12. 32 15.42 16.57 4.19 4.36 20.92 22. 22 10.26 10. 12 3.46 3. 24 27.4 9 26.71 26.37 27. 68 2.51* 1.21 8.72 8, 85 2. 84* 1. 71 2.36* 0. 91 0.28* 1.01 37.86 33. 08 16. 25 14. 67 86.09 84.78 39.32 41. 10 46.74 4 7. 46 0.00* 2. 15 1.60* 3. 46 16.69 15. 61 30.72 32.03 6.65 6.39 9.04 8. 58 5.99 5.51 20.97 22. 00 10.51 11.52 6.50 6. 52 9.13 8. 17 11.10 10. 92 13.28 12.70 46.37 44.89 9.66 9.56 55.66 60. 91 34.76 36. 98 8.83 10. 03 42.39 42. 80 6.65 6.94  WEIGHT 7.79 6. 20 1.99 7. 34 1.25 3.67 6.99 5. 54 7.73 4. 49 4. 74 3. 85 0. 30 6. 91 2.98 4.39 0.68 8. 40 0. 19 4.62 6. 20 4.76 6.26 2. 97 6.51 3. 15 1.76 1. 93 0. 14 4. 94 0.30 0. 19 0.01 0.99 4.35 0. 20 0.92 0.66 0. 01 0. 10 4.06 1. 46 6.09 5. 83 4. 09 2. 74 5,58 5. 17 7.82 5, 83 4. 35 0.65 9. 14 0.47 1. 18 8. 03 0.81 8.64  H  0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0  2 2 2 2 2 2 2 2 2 2 2 2 2  K  1  2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2  9 10 11 12 13 14 15 16 17 18 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 0 1 2 .3 4 5 6 7 8 9 10 11 12 13 14 15 17 0 1 2 3 4 5 6 7 8 9 10 11 12  FO  FC  22.41 21.86 24.77 25.41 20. 93 21.10 1. 24* 0.88 7.50 6.77 6. 90 6.06 1. 32* 0.31 4.19 4. 17 2.97* 0.56 2. 84* 3.16 26.51 20.38 39. 84 41.81 35. 92 40.41 2.76* 3.39 27.47 33.09 1. 60* 0.34 2.40* 1.70 17. 36 16.65 3.26 3.95 3. 90 4.24 19.47 21.01 3.46 3. 82 3. 70 2.73 4. 46 2.53 14.85 15.67 7.64 8.10 4. 68 5.47 4.00 3. 32 36. 01 36.65 11. 53 11.72 51. 48 55.54 21.39 23.55 51.94 56.76 26. 50 27. 37 27. 34 2 9.36 28.45 28.46 20.79 21.31 8.61 8.27 17.55 17, 36 2.07* 1.54 5. 84 4.19 5. 12 3.89 19.65 20. 15 4. 45 3.66 0. 94* 0. 19 55. 92 56.26 2. 10* 1. 39 5. 20 4.83 17. 33 17.46 23. 23 24.74 37.80 36.75 25.15 26.54 6. 44 5.00 34. 29 35.03 12.99 13.02 6.97 7.24 4. 80 3.64 9.08 8.67  WEIGHT  H  K  I  2. 53 2.13 2.70 0.04 5. 80 6.75 0. 04 2. 69 0.42 0.23 1.58 0.85 1.09 0.42 1.81 0. 21 0.33 3.98 3.71 3.70 3. 20 3.07 2.84 4.71 4. 18 7.46 2.94 3.92 1.06 7.41 0. 55 2.89 0.54 1.93 1.81 1.66 2.88 6.76 3. 42 0. 12 6. 08 5. 19 2.92 3. 91 0.04 0. 47 0.43 5.95 4.03 2.43 1.01 2.15 7.90 1. 19 5. 26 6.25 5.35 7.00  2 2 2 2 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 5 5 5 5 5 5 5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 6 6  2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2  13 14 15 16 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 0 1 2 3 4 5 6 7 8 9 10 11 12 13 0 1 2 3 4 5 6 7 8  FO  FC  5.75 5. 74 9.56 9.90 4. 33 4. 90 2.62* 0. 65 22.05 23. 11 46.79 46. 81 10.11 9. 57 17.81 17.25 7.99 6.75 20.02 20. 97 38.75 39. 45 15.87 16.56 9.07 8. 75 4.08 4.06 7.87 7. 61 9.44 9.15 6.97 6.91 4.78 5. 01 3.49 2.08 2.48* 0. 86 2.72* 3. 95 17.63 17.15 19.59 20. 74 14.51 14.23 13.70 12. 54 15.36 14. 65 14. 44 13.55 6.59 6. 67 3.21* 0.59 2.66* 2. 83 17.45 18. 82 4.51 4. 49 0.93* 0.37 2.57* 1. 47 3.48 2. 81 46.49 49.88 11. 13 10. 63 10.00 10. 58 6.03 5. 39 11.32 11. 10 6.41 6. 70 16.92 16. 85 4.68 3. 98 0.00* 0. 86 4.39 3. 07 2.12* 1.51 6.59 6. 93 0.00* 0. 46 3.00* 0.27 44. 82 47. 34 3.47 3. 37 14.10 15. 10 4.89 4. 44 11.67 11. 10 5. 16 4. 48 22.38 23.49 2. 88* 0. 24 3.84 5.04  ¥ EIGHT 3. 77 5.07 3.79 0.37 2.72 0. 66 8.27 3.84 8. 57 3.06 0. 95 4.12 7. 08 3. 56 5.82 5.00 5. 41 3. 24 3. 35 0. 31 0. 3 1 3.83 3. 20 5.19 5. 27 4.40 5.54 6.47 0. 38 0. 12 3.49 3. 39 0.02 0.22 3. 59 0.67 6. 83 7. 91 8. 72 6.81 4. 83 3. 99 3. 91 0. 00 4.45 0.11 4. 78 0. 00 0.43 0.71 3. 89 4.70 5. 73 6. 03 4. 61 2.44 0.27 5.21  H  K  I  6 6 6 6 7 7 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 8 8 9 9 9 9 9 9 9 9 10 10 10 10 10 10 10 11 11 11 11 11 12 12 12 13 13 13 13 13 13 13 13 13 13  2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3  9 10 11 12 0 1 2 3 4 5 6 7 8 9 10 0 1 2 3 a 5 6 7 8 9 0 1 2 3 5 6 7 0 1 2 3 a 5 6 0 1 2 3 4 0 1 2 3 4 5 6 7 8 9 10 11 12  FO  5. 24 13.58 3. 40* 9.37 13. 31 2.96* 9.94 2. 74* 6.46 7.79 9.09 5.91 2. 65* 2.55* 13.17 14.65 5. 78 13.95 3. 46* 8.65 1.92* 4. 68 3.02* 10.43 8.86 4. 53 2. 90* 4. 25 6.97 9.6 5 7.59 5.95 1. 49* 11.65 8. 50 15.52 7. 87 3.97 3. 60 6.65 7. 83 4.93 11. 12 3.42 6. 41 10.74 4. 22 5. 29 1.76* 4. 47 4. 83 6.11 2. 94* 2. 17* 10. 81 2. 13* 5. 85 3. 03*  FC  WEIGHT  4.81 3.36 13.54 4. 89 3. 16 0. 29 9.68 7. 30 1 4. 30 4.59 2.83 0.31 10. 27 5.34 0.59 0.21 5.66 6.85 7.77 5.64 9.23 5.73 6.17 4.65 1.33 0. 26 1.48 0.20 13.88 4.71 16.06 4.50 5. 81 4.16 14.68 4. 18 4. 11 0.19 8.98 5.70 1.21 0.09 4. 86 3.69 1.60 0.24 10.90 5.67 8.16 10. 11 4.06 3.51 0.71 0. 27 2.63 4.25 7.36 4.29 10.41 5. 21 7.22 6,23 5. 84 6. 15 0. 90 0.07 11.54 5. 38 7.24 7. 03 16.66 4.34 8. 48 5. 32 1.86 5.30 2.41 4.01 6.16 9. 51 8.13 7. 50 2.82 6. 20 1 1.56 5.40 1.89 3.78 6.04 9.30 1 1.26 5.75 2. 27 7.73 4.25 11.55 2. 56 0. 10 4. 87 4.36 5.74 4. 05 6.95 4.96 0.53 0. 30 0. 25 0.13 11,77 4.81 0. 32 0, 13 6.02 4.70 3.06 0. 27  H  -13 -13 -12 -12 -12 -12 -12 -12 -12 - 12 -12 -12 -12 -12 -12 -12 -12 -12 -11 -11 - 11 -11 -11 -11 - 11 -11 -11 -11 -11 -11 -11 -11 -11 -11 -11 -10 -10 - 10 -10 -10 -10 - 10 -10 -10 -10 - 10 -10 - 10 -10 -10 -10 - 10 -10 -9 -9 -9 -9 -9  K  L  3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3  13 14 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 1 2 3 4 5  FO  1.57* 1 .96* 5.65 3.81 1.96* 14.16 5.81 2.02* 4.61 6.81 9.45 2.93* 10.21 1.49* 4.08 3.04* 5.67 3.70 9.62 10.74 4.41 14.56 8.99 1.14* 9.29 4 .25 5.50 9.31 8.79 13. 28 4.65 2. 95* 7.62 11 .52 3.59 4.19 11.00 11.18 16. 92 16.11 14.78 3.38* 11.64 6.90 6.61 14.64 6.08 3.82* 2.56* 4.97 9.49 2.70* 2.39* 30.27 21.08 9.42 12.56 10.50  FC  WEIGHT  1.58 2. 36 7. 81 2. 12 0. 60 16. 99 5.71 2. 24 5. 10 7.57 10. 20 2. 81 11. 30 2. 77 3. 66 1.54 5. 56 4. 62 10. 97 13. 85 5.68 17.87 8. 37 1. 96 9.63 2. 82 4. 76 9. 81 9.24 13.78 5. 17 0. 79 7. 81 12. 80 3. 17 4. 16 11. 58 11.98 17. 68 17. 31 14. 66 4. 33 11. 89 6. 20 6. 18 15.67 6. 35 4, 86 2. 60 4.73 9. 33 1.91 2.78 29.18 21. 15 8. 97 12. 25 9. 68  0. 09 0. 12 4. 12 3.96 0. 10 3.75 5.41 0. 11 3.06 4.79 4. 91 0. 17 4,58 0. 05 3. 98 0.31 7.20 2.72 5.09 4. 88 2.70 3.82 7.09 0.02 5.11 4.42 5.91 4.54 5.19 4. 41 3. 15 0.24 6.03 5.28 3.68 3.09 5.00 4.49 3. 29 3.45 3. 93 0, 18 5.44 5.30 5. 10 3.95 4. 83 0.23 0. 16 3,93 6. 15 0. 28 0. 17 1.44 2.51 4.68 4. 53 5.35  B  K  I  9 9 9 9 9 9 9 9 9 9 9 9 9 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 6 6 6 6 6 6 6 6 6  3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3  6 7 8 9 10 11 12 13 14 15 16 17 18 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 1 2 3 4 5 6 7 8 9  FO  FC  WEIGHT  2. 72* 2.50 0. 14 4. 14 5. 90 5.99 5. 30 2.77 4.54 3. 19* 2.55 0. 24 4.65 4.84 3. 72 2. 22* 2.84 0.12 13.00 12. 68 4.66 13. 6 2 13.44 4. 20 5. 86 5.54 6.39 21.72 22.39 2.52 6.72 6. 11 6.21 9.57 9.21 5.10 6. 54 6.31 6. 84 19.35 18. 28 3.05 16.69 14.98 3.70 25. 32 2 5.11 1.92 1. 29* 0. 46 0.04 10.50 8.95 6. 47 12. 80 12.65 4. 84 5.90 5.46 4.75 3.03 3.91 2.70 14.95 14.56 4.12 16.49 16.71 3.37 28.01 28.12 1.67 12. 36 12.39 4.46 13. 15 13.01 5.03 5.41 5.39 4.29 3. 92* 4. 89 ; 0.20 14. 82 14.71 4. 15 8. 85 7.07 8.52 3.18* 0. 96 0. 38 13. 36 12.41 4. 54 9.67^ 5.80 9. 88 1. 64* 1.39 0.07 2.55* 1.57 0.19 27.06 25.69 1.81 4.21 3.90 3.81 23. 68 23. 72 2.18 1.65 3.65 3. 60 9.98 9. 83 6.57 28. 26 29.52 1.61 1.94 25. 15 25.79 17.51 18. 26 3. 22 16. 33 16. 04 3.77 9.72 9.57 5.71 2. 17* 3.55 0. 08 8. 41 8.71 5. 15 1.51* 0.65 0.07 4. 33 3.81 3.29 27. 67 24.73 1.73 33. 34 30. 12 1. 21 7.23 5.24 6.60 6. 11 5. 3 9 6.06 4. 16 4.32 3. 33 30.87 29.39 1.42 23. 39 22.91 2.36 8. 51 6.29 7.22 8.40 8.01 6.40  H  K  L  -6 3 10 -6 3 11 -6 3 12 -6 3 13 -6 3 14 -6 3 15 -6 3 16 -6 3 17 -6 3 18 -5 3 1 -5 3 2 -5 3 3 -5 3 4 -5 3 5 -5 • 3 6 -5 3 7 -5 3 8 -5 3 9 -5 3 10 -5 3 11 -5 3 12 -5 3 13 -5 3 14 -5 3 15 -5 3 16 -5 3 17 -5 3 18 -4 3 1 -4 3 2 -4 3 3 -4 3 4 -4 3 5 -4 3 6 -4 3 7 -4 3 8 -4 3 9 -4 3 10 -4 3 11 -4 3 12 -4 3 13 -4 3 14 -4 3 15 -4 3 16 -4 3 17 -4 3 18 -3 3 1 -3 3 2 -3 3 3 -3 3 4 -3 3 5 -3 3 6 -3 3 7 -3 3 8 -3 3 9 -3 3 10 -3 3 11 -3 3 12 -3 3 13  FO  FC  WEIGHT  1 .42* 0. 31 3.25* 2.24 16.39 17. 35 13.92 13. 34 12.34 12. 05 19.85 20. 43 6.07 6. 42 8.01 8.36 3.79 3. 86 32.82 30. 26 14. 28 12. 14 3.38 4.51 2.32* 1. 27 36. 81 34. 01 20.68 19.52 33.54 32. 72 7.16 7. 36 7.34 6. 96 17.78 17. 24 22.79 23. 87 7.06 7. 35, 11.53 11.62 3.93 4. 08 14.48 14. 52 1.61* 0. 79 6.73 5. 87 5.36 4.38 56. 10 49. 08 33.78 29. 94 61.11 52. 45 11.35 9. 91 2. 45* 1. 46 13.75 11. 91 7.74 8. 46 28.69 27. 13 15.92 15. 27 10.65 10.31 17. 70 17.71 1.66* 0. 35 13. 87 13. 80 3.46* •1. 05 15.12 14. 32 1.98* 0.29 12.46 12. 33 1.94* 2. 36 6.71 7.37 15.55 12. 06 27.62 25. 51 36.67 32. 81 7.54 6.75 33.67 32. 49 21 .51 22.01 2. 83* 0. 39 9.93 9. 60 6.97 6.62 9.49 9. 58 7.12 7.15 12.65 12. 41  0.05 0. 28 4, 04 4.41 4.72 2. 86 4. 97 5.54 3.02 1.29 4. 55 3,21 0.23 1. 04 2.87 1.24 6. 87 7.41 3. 50 2.36 5. 55 5.36 2. 50 4, 15 0. 06 5.83 7. 90 0. 46 1. 22 0.39 6. 07 0. 23 5.29 8. 10 1.67 4. 36 5.43 3.43 0.07 4.34 0. 33 4.29 0.09 5. 18 0. 11 6.76 4,49 1.77 1.05 6.85 1. 26 2.69 0.41 6, 16 5.92 7.46 5.69 4. 65  H  K  I  -3 -3 -3 -3 -3 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -1 -1 -1 -1  3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3  14 15 16 17 18 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 0 1  -1  -1 -1 -1 -1 -1 -1 -1  -1 -1 -1 -1 -1 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1 1  FO  FC  5.49 6.20 3. 90 1.91 7.66 7.64 7.87 7. 93 3.01* 1. 95 4.19 2.80 36. 41 31.08 2.03* 4. 36 23.64 22. 22 24.41 24. 84 7. 19 6.17 50.06 50.66 4.64 2.81 13.04 13. 32 6.36 6.46 17.75 18. 15 11.79 11.75 6.69 6.60 18.91 19.87 3.67 1.44 2.14 3.68 3. 47* 3.98 3.09 1.87 55. 07 42.79 13. 12 12. 18 35.06 34. 80 5.74 6.15 3.77 3. 17 40. 20 39.82 17. 40 18.49 43. 45 45. 04 5. 27 3. 18 10. 11 9.62 14.67 15.20 1. 46* 0.39 8.34 7.41 11. 17 12. 04 12. 16 13. 15 4. 7 3 3.66 9. 95 9.40 30. 88 33.59 65. 06 68.90 18.42 .19.70 14. 17 13.90 2. 88 2.35 13. 13 13. 94 27. 35 28. 85 12.38 13.47 11.42 12.05 4.84 6.54 8.53 9.08 14. 04 15.21 13.92 14.76 16.99 16.01 3. 86 2. 91 2.65* 1.38 19. 89 20. 18 13.92 15. 06  WEIGHT  H  K  L  2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 4 4 4  3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 '3 3 3 3 3 3 3 3 3 3 3 3  2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 0 1 2 3 4 5 6 7 8 9 10 11  3. 21 3.72 7.41 5. 88 0. 37 5.36 1.08  0. 20 2.43 2.25 8.56 0. 58 6. 97 5.18 5. 38 3.41 4.95 4.98 3. 13 3. 23 3.76 0.29 4. 18 0. 48 5.69 1. 16 8.69 4.98 0.89 3.99 0.77 8.06 6.65 4. 15 0. 06 6.92 5.02 5. 10 6.69 8.06 1.46 0.35 3.62 5.64 4.66 5.42 1. 82 5.87 6. 34 3.62 6.09 4.71 4. 41 3.96 3.38 0.27 3. 18 5.63  FO  FC  12.27 13. 03 30.55 33. 99 12.03 13.40 3.25 2. 11 12.26 11.99 17.87 19.52 13.88 14. 00 6.67 7. 28 7.63 7. 93 12.86 13, 84 2.74* 2.39 10.30 10.45 5. 43 5. 09 2.87* 2.22 2.39* 1.75 13. 85 15. 54 14.30 13. 91 16.60 -17. 86 31.62 33. 45 7.45 7. 80 6.35 6. 78 3.72 3. 42 24.07 24. 81 13.86 13. 76 10.31 11.93 13.12 14. 36 6.27 4. 61 5.35 3. 46 4,52 3.10 4. 76 5, 10 3.06* 2. 52 12.79 12. 16 16.03 16. 43 8.48 9.20 27.40 28. 84 16.99 18. 62 16.28 16. 35 8.96 8. 64 6.85 7. 06 5.47 6. 37 2.30* 2. 05 6.28 6. 04 8.68 9.44 3.09* 0. 33 7. 11 7.21 5.19 4.55 11.72 12. 07 2.40* 1. 11 4.62 3. 67 16.57 15.40 1. 56* 0. 74 6.06 6. 51 14.55 14. 96 11.87 13.03 4.85 3. 98 11.68 11.63 15.17 16.45 11.72 11. 28  WEIGHT 6,73 1.51 6.31 3. 90 6.38 3.59 1,81 6.24 5.98 4. 68 0.16 6.76 4. 97 0.28 0. 23 5. 41 5. 39 4. 14 1.41 9. 14 7. 86 3.86 2.29 5. 13 4. 85 4.64 6.31 5.72 5.36 3.99 0.32 6. 14 4. 33 7.21 1.80 3. 85 4.17 7. 33 6. 43 4. 80 0. 13 6.35 5.89 0. 34 7.03 7.30 6. 17 0.31 7.74 4.39 0.08 5.34 4. 81 5.06 3. 77 5.40 4.13 5. 81  H  K  I  4 4 5 5 5 5 5 5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 6 6 6 6 6 7 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8' 8 8 9 9 9 9 9 9 9 10 10 10 10 10  3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3  12 13 0 1 2 3 H 5 6 7 8 9 10 11 12 0 1 2 3 4 5 6 7 8 9 10 11 0 1 2 3 4 5 6 7 8 9 0 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 0 1 2 3 4  FO  FC  4.31 3.94 9. 44 9.79 17.73 19.21 8.74 7. 03 10.89 11. 39 14.69 15.53 2.42* 2.31 6.54 6.20 9.31 9.98 13.25 14. 45 6.09 5.64 17.31 18. 21 6.75 6. 36 2. 35* 1.38 3. 98 3. 52 0.98* 1.72 12.92 12.85 6. 45 5.76 16. 26 17. 55 20.31 21.88 3. 92* 4.93 8.82 9.44 2.97* 0.73 5. 34 5.25 4.08 4.15 1.61* 0.33 1.41* 0.21 2.43* 0.76 10.42 11.03 8.87 8.32 26. 62 28.57 12.59 13. 27 6. 17 7.09 6.50 6.73 7. 82 9.32 4.18 3.19 4.94 4.34 9.56 10.20 0. 68* 2.74 13.42 14.09 7. 60 7.98 8. 33 8. 59 8. 94 9.78 2. 68* 1.69 3.88 4.63 2.24 3. 19 15. 14 16. 10 13. 15 13.63 6.22 5.14 4. 15 3.91 4. 90 5.28 4. 68 3.77 4. 90 4.53 4. 16 3. 37 6. 83 7.11 3. 54 1.31 9. 89 10. 11 1. 55* 1. 97  WEIGHT  H  K  L  FO  3.40 6.67 3.75 5.76 6.25 4.73 0.19 4. 80 4.63 4.57 6.19 3.59 7. 59 0. 19 5.53 0.03 5.74 6.44 3. 98 2. 92 0.24 4. 95 0.28 4.34 3.58 0.07 0. 08 0. 19 5.54 5.23 1 .80 5.15 3. 83 6.71 5. 20 5.47 6.08 5. 16 0.01 4. 85 5. 40 6.96 5. 21 0.29 3.03 3.86 3.56 4. 94 6. 30 3.12 4.37 6.65 6.32 4.28 5. 62 4.05 6.18 0.08  10 11 11 11 11 12 -13 -13 -12 -12 -12 -12 -12 -12 -12 -12 -12 -12 -12 -12 -12 - 11 -11 -11 - 11 -11 -11 -11 -11 - 11 -11 - 11 -11 -11 -11 -11 -10 -10 -10 -10 -10 -10 -10 -10 -10 - 10 -10 -10 -10 -10 -10 -10 -9 -9 -9 -9 -9 -9  3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4  5 0 1 2 3 0 8 9 2 3 4 5 6 7 8 9 10 11 12 13 14 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 1 2 3 4 5 6  2.94* 12. 34 5.16 3.39 4.11 2.63* 3.59 2.58* 11.97 2.89* 7.92 5.95 4.79 2.79* 6.19 2. 15* 5. 23 3.15* 9.42 7.37 2.88* 1.00* 1.78* 9.44 15.85 6.13 2.44* 7.95 4.84 6.58 5.34 1.50* 3. 66* 3.75 9.13 3.89 3.38* 6. 53 14.38 3.99 7.42 3.09* 5.74 10.43 0.00* 2.70* 6.09 6. 24 2.75* 3.97 7.91 7.09 3. 32* 18.44 2.42* 3.84 2.08* 5.19  FC  WEIGHT  2.29 0.44 12. 80 4.59 5.64 4.56 2. 34 3. 91 3.90 6.70 0.20 0.33 4.09 3.41 1.12 0.27 13.18 5.29 2. 45 0. 28 8.35 7.16 6.59 5.77 4.68 '4.31 2.05 0.20 6. 16 6.79 0. 87 0. 12 5. 28 6. 05 2.61 0.35 10. 16 5.73 7. 08 7.55 2.38 0.32 0.33 0.03 0.51 0.08 9. 43 6. 83 16.41 3.96 6.70 4.43 2. 02 0. 12 8. 41 4. 53 4. 73 4. 14 5.78 5.74 4. 91 6.59 1.34 0.05 2. 85 0. 28 1. 74 5.31 9.79 6.15 3. 44 4.04 2.52 0.21 6. 34 5. 39 14. 10 4. 07 0. 81 3.99 7. 85 5.47 0. 96 0.20 6. 14 3.51 9. 94 5. 03 2. 55 0.00 2.67 0.16 5. 02 6.53 6. 40 4. 29 0.72 0.20 3. 52 2.81 8. 05 5. 65 6.57 6.19 3. 20 0. 17 17.26 3. 10 0.55 0.12 2. 17 2.47 2.44 0.07 3.70 3.78  H  K  L  -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6  4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4  7 8 9 10 11 12 13 14 15 16 17 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 1 2 3 4 5 6 7 8 9 10 11 12  FO  FC  17.78 17.47 23.99 23.82 6. 94 6.43 11. 48 11.62 3.70 1.16 14. 52 15.27 6. 04 6.40 2. 66* 2.33 6.67 6.02 11.80 11.70 1.73* 0.77 9.72 8. 24 20. 39 19.65 4.76 2.63 26. 03 25.35 3. 53* 2.26 6.45 5.08 4. 39 4.01 7.89 7.00 4. 90 4.25 15.51 15. 17 11. 16 11.01 15. 03 15.85 3.60 0.40 10.75 10.45 0. 00* 0. 92 8.64 8.05 4.78 4.23 7.56 6.37 6.73 6.91 8. 13 7.71 24. 73 22.66 9. 66 9.36 3.62* 2.45 15. 17 15.80 11.11 11.75 3.02* 1.41 11.28 11.44 5. 71 5.38 3.38* 2. 25 3.95 2. 36 11.88 12.34 0. 26* 0.78 7.47 6. 68 0. 00* 1.26 6. 85 6.64 1. 96* 0.28 11.62 10.32 2. 66* 2.61 25.5 5 24.87 0. 00* 0.82 5. 33 3.11 15. 69 14.19 11. 58 11.82 14.20 13.80 4.23 3.44 17. 02 17.81 12.46 12.24  WEIGHT  H  K  L  FO  FC  WEIGHT  3. 21 2.06 5.00 4. 80 3.41 3.99 3.96 0.14 8. 25 5.55 0.11 5. 58 2. 64 2.71 1.77 0. 19 4. 92 3. 16 6.77 3. 54 4.18 4. 80 3.81 3. 36 5.84 0.00 6. 20 4. 86 5.55 4.39 5. 22 2. 11 4.70 0. 22 4. 19 5. 14 0.20 4. 81 3.30 0.32 3. 69 4. 87  -6 -6 -6 -6 -6 -6 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -2  4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 '4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4  13 14 15 16 17 18 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 1  3.81 11.91 1. 78* 3.56 2.16* 3.48 7.20 2.86* 3.46 13.75 17.31 4.23 8.30 30.23 17.01 2.49* 18.94 4. 16 4.04 13.32 5.58 4.92 3.72 24. 81 7.56 7.32 21.20 5.75 30.63 8.82 29.41 29.05 33.54 4.64 16.13 5.01 15.80 8.29 4.42 0.19* 24.35 10.06 27.32 27.34 6.77 25.97 12.03 11.12 14.43 4.44 15.74 15.39 7.59 10.18 4.04 0.00* 3. 26 14.47  3. 07 12. 42 0. 30 2. 67 1.46 3. 06 5.61 1.54 0.72 12. 91 16. 99 4.53 8. 24 28.53 16. 80 2. 40 18.71 2. 94 3.70 13. 23 5.70 3. 94 2.69 21.69 6.73 6. 75 18. 03 4.95 28. 62 7. 84 29. 19 29.70 34. 18 3.92 15. 86 3. 54 15. 53 7. 68 3. 13 0.59 20.06 7. 20 24. 05 24.68 7. 28 24. 96 12.03 11. 29 14. 92 4. 26 16. 11 15.58 8. 06 10. 25 3. 53 0.79 0. 61 11.91  3. 44 4. 80 0. 08 4. 25 0. 13 3. 81 5.76 0.21 3.38 4. 98 3.52 2.66 5. 73 1.46 3. 51 0.11 3.26 2.70 2.57 4. 47 4.57 4. 60 4.02 2. 12 5.97 5. 23 2. 59 5.54 1.45 5. 41 1.52 1.53 1.20 3.36 3.73 4. 83 4. 14 7.38 5. 80 0.00 •2. 16 7. 15 1.78 1.77 5. 13 1.97 6.06 6.19 4. 21 2. 72 3.67 4. 20 5.49 5.77 3. 24 0.00 4.02 4.50  0.-00  6. 78 0.00 8. 17 0.07 5.33 0. 12 1.96 0.00 5. 00 3.89 4.69 3.62 3.06 3. 56 4. 57  H  K  I  -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2  4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4  2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 1 3 4 5 6 7 8 9 10 11 12 13 14 15 16 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 0 1 2 3 4 5 6 7 8 9 10 11  -1 -1  -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1  -1 -1 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1 1  1 1 1 1 1 1  1 1 1 1  FO  FC  32. 64 27.05 3.32* 2.95 23. 20 22.98 11.06 11.08 3.76 2. 86 4.36 4.12 7.4 9 7.11 13. 80 13.32 7. 16 6.66 3. 26* 3.35 5. 84 5.36 3. 25* 2. 08 9.45 9.71 2. 11* 1.27 2. 84* 1.39 22. 48 18.42 25.01 23.92 21.54 22. 25 6.77 7.73 13. 37 13.48 2.73* 0.11 24.93 25. 31 7. 20 7.10 15. 57 16.20 8.05 8.59 8.62 8. 35 1.61 2.84* 15.05 15.07 1.04 3. 17 3. 3 2* 3.44 60. 56 48.96 25. 28 25.30 17.83 17.49 9. 46 10.05 2.80 4. 02 3. 13* 1.70 28. 47 28.78 3.00* 2.64 14.41 15.57 2. 40* 3. 18 2. 95* 1.77 8. 50 8. 30 6.00 6.03 9.77 9.28 5. 80 6.08 3. 83 4.01 24. 18 24.70 5. 15 5. 13 19.50 20.50 11.00 11.10 5.70 5.19 4. 58 5.33 18.69 19.78 2.10* 2.22 0. 00* 1.07 2. 33* 1.64 23.81 24.74 11. 46 12.02  HEIGHT 1. 28 0.28 2.38 6. 51 4. 40 4.75 6.51 5.33 6.93 0.16 5.72 0.31 5.19 0. 13 0.29 2. 41 2. 11 2.79 6.16 4.73 0. 26 2.08 4.93 4.24 5. 53 6.80 0.26 4. 33 4.04 0.35 0.39 2.07 3.86 7.65 4.53 0.40 1.64 0. 28 4.24 0. 14 0.19 6.77 6. 10 7. 11 4.59 3. 46 2. 17 5.13 3.19 6.27 6.09 3.54 3.41 0. 13 0.00 0.13 2.20 5. 42  H  K  L  1 1 1 1 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3  4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4  12 13 14 15 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 0 1 2 3 4 5 6 7 8 9 10 11 12 13 0 1 2 3 4 5 6 7 8 9 10 11 12 0 1 2 3 4 5 6 7 8 9 10 11  3  3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 4 4 4 4 5 5 5 5 5 5 5 5 5 5 5 5  FO  FC  3.38* 3.20 6. 19 6. 57 5.84 6. 05 2.80* 0. 37 30.18 29. 01 1. 04 2.48* 20.05 20. 43 7.98 7.71 12.32 12. 48 3.31* 3. 71 3.43 1. 96 8.81 9. 29 13.07 14. 49 3.67 4.29 25.49 26. 97 2.79* 0.46 1.56* 1. 31 4.93 4. 11 8.20 7.73 32.07 31. 47 5.66 4.65 30.91 31.32 7.85 7. 85 29.91 31. 37 21.10 22. 59 5.21 5.15 3. 21* 1. 32 3.66 2. 26 7.41 7.61 7.41 6. 47 4.31 4. 37 2.70* 2.81 8.07 8. 31 1.57* 1. 86 11.40 11. 81 10.09 9.99 4.28 4.01 29.66 30. 17 6.74 6.39 19.01 20. 11 1.13* 1. 02 8.29 8. 49 2.78* 0. 14 4.70 3.57 3.87 3. 19 7. 33 6. 95 22.37 22. 04 15. 39 15. 64 29.97 31.46 13. 19 13. 47 3.98 3. 23 6.55 6. 20 15.60 15.83 2.24* 0. 60 1.21* 2. 40 6.39 6. 03 9.19 9. 97 1.84* 0.92  HEIGHT 0. 25 5.74 6. 84 0.41 1. 53 0.26 3.01 7. 12 5.68 0.26 4.03 6. 15 4.63 4.25 1.94 0.26 0.07 5.52 9.24 1.35 9.50 1.44 6.38 1.49 2.72 4.44 0. 33 3. 39 6.78 7. 11 3.71 0. 19 7. 86 0. 08 5.94 6.07 4.05 1. 55 4. 28 3. 14 0.03 5.66 0. 26 5.72 3.92 9.02 2.65 4.05 1.48 4.69 2.82 6.35 4.45 0.11 0.03 5. 89 5, 83 0.13  H  K  I  6 6 6 6 6 6 6 6 6 6 6 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 9 9 9 9 9 9 10 10 10 10 11 11 11 11 11 11 11 11 11 11 11 11 10 10 10 10 10 10 10 10  4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5  0 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 0 1 2 3 4 5 0 1 2 3 0 1 3 4 5 6 7 8 9 10 11 12 1 2 3 4 5 6 7 8  FO  FC  WEIGHT  8. 11 7. 87 7.46 17.08 17.94 3. 48 16. 11 17.15 3.64 17. 00 17. 92 3. 58 2. 13* 3.22 0.07 9.75 9.71 5. 65 3.02* 3.00 0.20 4.73 3.65 5. 42 0.93 0.37 2.93* 0.00* 0.61 0.00 6. 29 6. 30 7.95 6. 16 5.6 8 4. 77 8.41 8. 39 6.80 3.41* 2.4 2 0. 33 9.45 9.07 5.65 6. 80 6.73 5.14 6.32 6. 27 5. 28 5.56 5.29 6.81 1.76* 0.72 0. 11 2.32* 0.29 0.24 16. 96 17. 54 3 * 5 8 8.57 8.16 5.62 11. 05 11.14 4.96 2.61* 1.92 0.16 1. 99* 1.19 0.11 1.92* 0.59 0.12 12.20 13.32 5.56 3.91 3. 15 • 4.66 5. 33 6. 40 6. 11 2. 22* 1.70 0.12 7.67 8.14 5. 30 2.46* 1.4 3 0. 19 0.00* 0.14 0. 00 3.64 3.74 3.85 3.08* 1.91 0. 26 4. 62 3.99 4. 82 7. 18 7.0 8 7.97 4.65 3.76 9.49 6.24 6.08 8. 15 4. 38 4.27 5.53 3.36 2.30 3. 62 2. 24* 1.06 0. 18 8.39 8. 92 5. 81 7. 84 8.39 6.25 7.67 7.11 8.27 1. 9 9* 0. 28 0. 13 7.68 7.83 6.23 5.19 5.3 9 4.70 2.66* 2.57 0. 25 3.02* 2.42 0. 35 6. 22 6. 49 5 • 35 0. 00* 1.01 0.00 0. 84* 2.71 0. 02 2. 46* 2. 17 0.11 2. 33* 2.65 0. 10 5.71 5. 80 5.22 6.31 6.21 6.11 4.73 4. 08 3. 59  H  K  L  -10 -10 -10 -10 -10 -10 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 * -7 -7 -7 -7 -6 -6 -6 -6 -6 -6 -6  5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5  9 10 11 12 13 14 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 1 2 3 5 6 7 8 9 10 11 12 13 14 15 16 1 2 3 4 5 6 7  FO 2. 88* 2.76* 1.19* 4.38 0.00* 3 . 76 9.88 4.54 3.77 4.62 7.74 3.09* 0.00* 9.30 5.02 9.55 13.59 3.43* 2.72* 0.84* 3.23* 8.21 3.64* 7.13 8. 36 9.80 12.83 7.82 1 3.85 4.41 5.48 1.52* 4.67 5.79 1 .79* 8.25 5.63 19.14 11.57 3.09* 3.77* 18. 15 2.38* 9.46 7.89 10.51 2.86* 5.48 3.19* 4.98 7.54 23. 20 4.61 8.72 3.56* 16.88 2.31* 25.69  FC 1. 51 0. 64 1.39 4. 18 1.28 2. 04 10.02 4.07 2. 13 4.70 7.65 0. 39 2. 68 8. 70 6. 00 8. 78 14. 54 3.15 1. 83 0.73 3. 67 8. 59 2. 56 6. 54 7. 43 9. 72 12. 45 8. 02 14. 31 3.53 4. 33 3. 28 2. 92 5.74 1. 34 8. 51 5.75 19. 23 11. 41 1. 33 4. 45 16. 62 2.29 9. 01 7. 45 10. 94 2. 59 5.02 3. 04 4. 37 7.36 20. 42 3. 03 8. 85 2. 63 16. 06 2. 95 24. 55  WEIGHT 0.25 0. 25 0.04 5.33 0.00 5.79 5. 16 3.02 2. 83 2.86 4.89 0. 22 0. 00 7. 23 2.69 7.47 4. 27 0.25 0. 1 9 0.02 0.31 3.71 0. 20 4.32 5.62 4. 94 4.60 4.59 4. 09 2.49 5. 96 0. 04 5. 71 5. 82 0.09 7.55 2.71 2.73 4. 01 0.20 0. 21 3. 11 0.09 4. 78 5. 42 4. 45 0. 14 4.92 0. 22 6. 11 7.08 2. 14 2. 46 5.51 0. 15 3.38 0.07 1.94  H  K  I  6 6  5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 t;  8 9 10 11 12 13 14 15 16 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 1 •2 3 4  6  6 6 6  6 6 6 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 2 2  5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5  5  6 7 8 9 10 11 12 13 14 15 16 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 1 2  FO 9.9 8 3. 1 0 * 1.97* 17. 52 4.95 5.77 2. 2 6 * 3.63 4.06 29.66 6.94 11.46 4.07 11.09 18. 15 5. 5 1 9.40 4.35 • 10. 04 17, 34 4.35 2.95* 2.31* 13. 12 3. 8 5 3.00* 24.69 16.47 11.69 15. 13 8.99 3. 8 1 11. 66 3.97 13.86 3.29* 6. 0 6 6.3 3 5. 3 4 3. 4 5 4.95 15.62 11.94 21. 89 10.77 4.57 7.68 16.30 12.39 3.73* 10.91 5. 6 6 7.95 2. 0 2 * 0. 0 0 * 3.61 14.44 13. 23  FC  WEIGHT  10.38 0.71 1.26 1 7 . 18 3.93 5.63 2.34 2.84 3.21 25.45 7.06 10.44 2.98 10.74 17.18 4.91 10. 29 3.60 9.62 18.55 2.35 2.71 0.52 12. 80 3.53 1.84 22.72 15.67 9.88 13.61 8. 8 3 1. 2 6 12. 29 3.95 13.72 1.03 6.54 6.69 4.31 2.60 4.95 12.78 10.05 20.00 9. 8 1 2.84 7.00 15.86 11.31 3. 7 2 10.93 5.28 7. 9 0 0.59 0.71 1.92 12.96 11.72  4.74 0. 1 8 0. 0 8 3. 8 3 5. 2 3 4.94 0.11 3. 7 8 4.55 1.50 3.59 4.41 2. 1 9 4. 9 0 3. 16 4. 0 6 4.76 2. 8 5 5. 4 5 3.30 4. 3 5 0.20 0. 1 6 5.11 4.19 0.10 2.04 3.52 5.51 3.87 4.36 2. 5 2 5.24 2.53 4. 6 1 0. 3 0 3.70 5.28 6.95 3.56 5.09 3. 6 0 4.71 2.48 4.76 5.07 5.69 3.75 5.63 0. 2 6 5.33 4.12 5.64 0. 1 1 0. 0 0 5. 9 1 3.61 4.00  H -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -1 -1  -1  -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1 1 1 1 1 1 1 1 1 1 1 1 1 1 2 2 2  K  L  5 3 4 5 5 5 5 6 7 5 8 5 5 9 5 10 5 11 5 12 5 13 5 14 5 15 1 5 5 2 5 3 4 5 5 5 5 6 5 7 5 8 9 5 5 10 5 11 5 1.32 5 1 5 14 5 1 5 2 5 3 5 4 5 5 5 6 5 7 5 8 ' 9 5 5 10 5 11 5 12 5 13 5 14 5 0 5 1 5 2 5 3 5 4 5 5 5 6 5 7 5 8 5 9 5 10 5 11 5 12 5 13 5 0 5 1 5 2  FO 5.02 11.82 0.00* 3.29* 10.75  FC  WEIGHT  4. 18 3. 8 3 1 1 . 48 4. 8 4 0. 5 2 0. 0 0 2. 6 0 0. 2 5 1 2 . 03 5.08 1 0 . 57 4.93 8.15 8. 1 9 6.75 3.07* 0.97 0.28 27.24 27.92 1.79 14.79 15.50 4.60 8.87 8. 5 7 7.92 2.41* 1. 24 0.21 0. 0 0 * 0.45 0.01 4.71 2. 06 3.07 11.23 1 1 . 54 4.75 26.46 26. 65 1. 8 3 3.28* 2. 0 9 0.29 3.48 0.50 3.81 12.39 12. 65 5. 8 8 16.86 1 8 . 21 3.65 3.92* 0. 2 3 4. 6 1 32.43 34. 48 1. 2 8 1.94* 1. 7 5 0. 0 8 3.32* 2. 2 4 0.34 4.26 3 . 34 3.49 9.90 9.70 6.07 2.28* 0. 9 2 0. 2 2 2.65* 2.89 0. 13 8.00 6. 9 0 6.76 2 4 . 14 21.92 2. 5 8 1.71* 0. 81 0.09 13.86 14.76 4.26 21.96 2 4 . 24 2. 4 4 12.82 1 3 . 38 4.63 15.30 15. 97 3.98 2.73* 1.78 0. 16 9.27 9.52 5.78 6.59 5. 2 7 7.00 1.64 3.25 3.71 4. 1 7 4. 9 3 2. 9 2 3.84 3. 35 4.38 5.44 6. 14 3. 7 2 20.15 2 1 . 16 2.86 10.43 10. 65 5. 6 8 4.51 4.73 4. 0 6 22.85 25. 53 2. 3 4 11.14 11.51 6.43 6.93 6. 6 2 5. 3 2 14.68 13.51 5.25 2.07* 2. 0 7 0.09 8.27 8. 1 0 6.94 4.33 4. 8 2 3.30 8.94 9. 4 4 6. 5 7 4.01 3.40 4.12 6.33 5 . 86 1 0 . 7 4 10.05 10.73 5. 1 8 28.21 2 8 . 32 1. 7 0 10.11 10.38 5.51  1-1.11  H  K  I  2 3 5 4 2 5 2 5 5 5 6 2 7 2 5 2 5 8 2 5 9 2 5 10 2 5 11 5 12 2 3 5 0 3 5 1 3 5 2 3 3 5 3 5 4 3 5 5 3 5 6 3 5 7 8 3 5 3 5 9 5 10 3 3 5 11 4 5 0 4 5 1 4 5 2 4 5 3 4 5 4 4 5 5 4 5 6 4 5 7 4 5 8 4 5 9 4 5 10 5 5 0 5 5 1 5 2 5 5 5 3 5 5 4 5 5 5 5 5 6 5 5 7 5 5 8 5 5 9 6 5 0 6 - 5 1 6 5 2 6 5 3 6 4 5 6 5 5 6 5 6 6 5 7 6 5 8 7 5 0 7 1 5 7 5 2 7 5 3 7 5 4 7 5 5  FO  FC  40.76 43. 27 1.65* 2.15 12.73 13.55 3. 91 2.42 12.69 13.90 5.01 4.10 8.02 8.62 4.48 4.65 6. 20 6.01 3.01* 2.31 4. 51 3.48 20. 91 21.07 16.25 15.42 3.52* 2. 88 6. 00 5.67 3.18* 2.92 13.94 14. 48 7.43 7.67 2.63* 4.03 0.00* 1.52 8.57 8.91 2. 25* 1.41 5.34 4.73 3.33* 3.98 6.12 5.46 3. 53 1.64 16. 92 17.16 7.96 7.55 1. 83* 0. 21 7.84 8.11 3. 81 3. 20 4.56 3.09 3. 12* 2.95 2. 40* 2. 85 14.48 15.16 4.76 5.89 16.31 16.61 1.97* 2. 05 5.15 5.85 5.95 5.40 5.79 5.89 9. 13 9.4 8 8. 23 8.37 4.94 3.44 8.73 8. 16 0.54 0.72* 13.83 13. 85 3. 28* 2.80 2. 80* 0.72 7.27 7.41 8. 76 9.36 3.30* 3. 11 6.88 6.62 2. 82* 2.65 2.92* 2.22 9.47 9.93 2. 37* 1. 36 9.28 9.90  WEIGHT  H  K  L  0. 86 0.05 4.69 3.72 5.05 5. 13 5.87 3. 86 8.44 0.37 3.97 2. 89 4. 10 0.27 6.15 0.30 5. 08 5.42 0.16 0.00 6. 98 0.21 4.23 0. 23 5.99 3.02 3.74 6.51 0.07 7.02 4. 17 6.29 0.28 0.09 3. 84 2.51 4.06 0. 08 2.94 6.35 5. 25 6.31 7.40 4.66 6. 53 0. 01 4. 70 0.33 0. 28 5.43 5.87 0.37 7. 10 0. 16 0.18 6. 12 0. 16 5.60  7 8 8 8 8 8 8 9 9 9 9 10 -9 -9 -9 -9 -9 -9 -9 -9 -9 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6  5 5 5 5 5 5  6 0 1 2 3 4 5 0 1 2 3 0 2 3 4 5 6 7 8 9 10 1 2 3 4  5 5 5 5 5 5 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6  5  6 7 8 9 10 11 12 1 2 3 4 5 6 7 8 9 10 11 12 13 1 2 3 4 5 6 7 8 9 10 11 12  FO 2.85* 5.71 5.48 6.14 2.77* 1.69* 4.24 5.38 3.57 2.55* 6.02 5.25 5.28 3.76* 5. 85 3.94 3.17* 3.81 3.70 2.96* 3.99 2. 87* 3.63* 3.09* 9. 14 5.90 2. 58* 8.32 9.59 1. 17* 2.90* 4.09 5.79 7.74 8.02 6. 12 4.23 10.60 5.01 1. 87* 10.76 4.32 5. 23 5.97 1.85* 0.65* 1.90* 9.17 3.75* 2.90* 5. 11 5.36 4.01 9.22 5.96 9.49 4.04 3.73  FC  WEIGHT  0. 30 4.84 4.26 6. 16 1.66 0. 56 4.66 6.09 1.99 2.36 6. 69 4. 45 5.46 4. 40 5. 90 3.30 2. 59 3. 41 2.66 2. 02 3. 44 -2. 22 2. 10 0. 80 8. 84 5.63 3.74 7. 95 8. 65 0. 45 0. 47 4. 21 5. 28 7. 38 6.27 6. 10 2.47 9. 87 4.07 3. 24 10. 54 3.95 4. 21 5.71 0. 84 0.77 0. 17 8.21 3. 31 1.23 4. 26 4.09 2. 15 9. 97 5. 32 9. 18 3.54 3.73  0.33 6. 09 5.90 5. 36 0.22 0. 08 3,82 3.91 3. 19 0. 18 5.77 6. 86 3,93 0.21 3. 88 3.19 0.20 3. 03 2. 98 0. 24 3.13 0. 15 0. 21 0. 19 4.96 4.25 0. 10 4.83 5. 85 0.03 0.27 3.59 5.32 5.05 4,97 3.20 3.02 5.05 3. 86 0.05 5. 36 2.83 4.01 5.17 0. 10 0.01 0.05 4. 85 0.16 0. 13 2. 86 3.09 2.70 4.44 3. 94 4. 91 3.68 2.90  H  K  1  6 5 5 5 5 5 5 5 5 5 5 5 5 5 4 4 4 4 4 4 4 4 4 4 4 4 4 3 3 3 3 3 3 3 3 3 3 3 3 2 2 2 2 2 2 2 2 2 2 2 2 2 1 1 1 1 1 1  6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 € 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6  13 1 2 3 4 5 6 7 8 9 10 11 12 13 1 2 3 4 5 6 7 8 9 10 11 12 13 1 2 3 4 5 6 7 8 9 10 11 13 1 2 3 4 5 6 7 8  c  10 11 12 13 1 2 3 4 5 6  FO  FC  WEIGHT  H  K  L  8.46 8.62 6. 54 4.50 1.93 2.97 4. 30 1.78 2. 10 13. 96 12.59 3.88 13.43 13.01 3. 67 10.64 10.31 4.20 8.74 8.97 4.59 2.95* 3.09 0.13 3.78 1.39 3.49 2. 99* 4.90 0.12 9.75 10.55 6. 18 10. 60 10.56 6.37 9.64 9.74 5.62 6. 24 5.73 10.00 6. 61 6.21 2. 58 10.57 10.21 3. 69 4.48 3.03 2. 18 15.06 13.62 3.66 2.71* 1.46 0. 10 0.00* 0.45 0. 00 9.00 8.44 5.67 6. 58 6. 19 5.05 3.92 3.74 2.83 13.77 13. 73 5. 06 0.62* 0.13 0.01 2.77* 0.85 0. 26 2, 64* 1.07 0.29 4. 25* 3.48 0. 19 6. 26 5.82 3.02 11.66 11.36 4.23 11. 49 10.47 4.25 0. 00* 0.72 0. 00 4.02 1.97 3.72 14.14 15.59 4.52 11.48 12.41 4. 89 5. 58 4.41 6.03 8.00 7.39 6.24 3. 69 2.99 3. 22 0. 00* 1.13 0. 00 11. 43 9.05 4.25 11. 66 9.81 4. 24 17.37 16.52 3.28 17.4 3 17.87 3.44 25. 99 27.52 1.87 12.70 13.59 4. 54 13.27 14.25 4.76 7.50 8. 22 5. 45 9.53 10.37 7.07 10. 82 11.75 6. 14 2. 84* 0. 92 0.24 5.08 4.94 6.24 1. 60* 0.70 0. 11 18. 10 16.81 2. 64 3. 4 7* 2.76 0. 17 3. 68* 3.40 0. 19 25. 76 27.77 1.90 10. 17 9.95 5.52 3. 94 3.35 2. 54  1 1 1 1 1 1 0 0 0 0 0 0 0 0 0 0 0 0 1 1 1 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4  6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6  7 8 9 10 11 12 0 1 2 3 4 5 6 7 8 9 10 11 0 1 2 3 4 5 6 7 8 9 10 11 0 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 7 8 9 0 1 2 3 4 5 6  FO 4.41 4.96 9.62 4.40 2.78* 5.31 7.92 2. 29* 22. 06 3.45* 0.00* 1.49* 6. 84 3.81 1. 87* 4.71 2.09* 3.53 12.98 4 . 36 4.53 10.55 6.72 13.02 10.41 2.98* 15.07 4.25 9.73 2.66* 18.16 12. 86 2.50* 0.00* 9.08 1.75* 13.40 5.23 3.42 14. 81 5.35 3.43* 2.03* 11.43 2.65* 7.96 8.16 13.32 15.15 3.61 7.59 13.79 0.00* 3.49* 2.06* 2.33* 2.79* 7.65  FC  WEIGHT  4. 38 4.54 9.67 4. 84 3. 57 4. 66 6. 40 1.68 24. 30 0.73 1.86 2. 60 6. 34 1. 16 0. 65 4.70 2.34 3. 04 13. 54 4.30 2.73 10. 83 4.96 13. 82 11.25 0. 17 17. 14 3. 11 10. 55 0. 85 19. 35 13. 66 1. 54 0.33 10. 02 1. 16 14.88 5.02 0. 26 15. 87 5.56 2. 69 3. 18 11. 96 2. 13 8. 67 8. 11 13. 76 15.94 2. 50 7. 80 14.41 1.21 1. 74 1. 73 3.54 2. 68 7. 82  3. 10 5.29 7.24 3.99 0. 19 7. 34 2.67 0. 11 2. 41 0.33 0.00 0.04 6. 46 3. 66 0.09 4.15 0. 11 3. 67 4. 13 2.98 3.13 5. 46 6.27 5.44 6.55 0.29 4.07 5.65 6. 01 0. 35 3. 28 4. 50 0. 13 0. 00 4. 81 0. 07 4.62 4.19 3.76 4.46 5.74 0. 16 0. 06 4.58 0. 14 4.43 6.90 4. 33 4. 12 3.46 7.30 4.57 0. 00 0. 32 0. 09 0. 09 0. 19 6. 63  HI K  *! 4 5 5 /5 5 5  h I 65  6 6 6 6 6 7 7 7 7 8 8 -7 -7 -7 -6 -6 -6 -6 -6 -6 -6 -6 -5 -5 -5 -5 -5 -5 -5 -5 -5  -a  -4 -4 -4 -4 -4 -4 -4 -4 -3 -3 -3 -3 -3 -3 -3 -3  6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7  1 7 8 0 1 2 3 4 5 6 0 1 2 3 4 5 0 1 2 3 0 1 4 5 6 1 2 3 4 5 6 7 8 1 2 3 4 5 6 7 8 9 1 2 3 a 5 6 7 8 9 1 2 3 4 5 6 7 8  FO  FC  3. 36 1.97 5. 95 6.61 20. 20 21.69 8. 13 8. 81 3. 76* 2.88 7. 61 6.79 3. 46 1.94 1.14 3.82 3. 21* 4. 09 5.0 8 4.6 3 12.54 12.55 1.43* 1.24 5.64 5.42 6. 34 5.86 7.99 7. 97 5. 52 4.88 0. 00* 2.02 5.63 5.93 5. 74 5.03 7. 30 7.73 3. 73 2. 10 0. 19 3.08* 7.32 8.66 1. 20* 1.05 3.09* 1.64 2.95* 3.86 7.04 7. 16 4. 74 3.70 3.91* 2.86 6. 18 6.93 4. 61 3.05 2. 85* 2.32 6.44 6.62 5. 21 3.63 3. 23* 1.00 4.41 5.12 8. 50 7. 94 10. 36 11.48 15.66 16.61 4.87 5.02 3. 83 3.40 11. 78 11.80 7.07 5.31 5. 59 5.57 18.53 18.98 2. 45* 2.07 2. 74* 2.76 9. 19 9.63 2. 56* 2. 90 3.79 2.56 2.21* 1.59 5. 92 5.50 9. 45 8. 29 3. 23* 2. 38 6. 85 6.33 9.86 10.32 0.63* 0.74 2. 81* 1.19  WEIGHT  H  K  L  3. 20 6.60 2.86 4.58 0. 28 7.30 3. 75 5.02 0.27 3.90 5.38 0.04 5.54 6. 94 7.39 6.91 0.00 5.02 5.95 6. 59 4.71 0.26 5 • 26 0. 04 0. 16 0. 12 4. 22 3. 01 0.25 3. 84 4.69 0.22 3. 46 3.52 0. 15 1. 96 4.78 5. 11 3. 75 3.94 3.93 3. 64 4.33 2.46 2. 94 0. 08 0. 13 5. 60 0. 14 4.72 0.05 2.45 3. 84 0. 15 4. 17 4.67 0.01 0.27  -3 -2 -2 -2 -2 -2 -2 -2 -2 -2 -1 -1 -1 -1 -1 -1 -1 -1 -1 0 0 0 0 0 0 0 0 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 3 3 3 3 3 3 4 4 4 4 4 5 5 5 6  7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7  9 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 0 1 2 3 4 5 6 0 1 2 3 4 5 0 1 2 3 4 0 1 2 0  FO 4.10 11.02 7.90 5.84 8.00 2.44* 4.31 8.34 6.08 2.00* 4.99 13. 24 3. 82* 6.21 6.31 4.92 7.83 3.29 4.34 5.54 5.95 9. 13 2.97* 2.04* 7.00 14.89 4.62 9.66 14.73 4.58 8.77 3.44* 9.74 3.50* 7 .89 7.86 6.21 9.10 3.17* 1.71* 3.92 1.95* 10.47 3.91 9.55 8.08 4.48 3.95 2.38* 2.90* 2.69* 7.43 3. 48 2.98* 1.28* 2.93* 3.08  FC  WEIGHT  3. 79 10. 90 7. 79 5. 30 7. 09 1.42 5. 27 8. 64 7. 33 1. 75 2. 79 13. 77 3. 66 6. 95 6. 81 3.40 8. 29 2. 25 3.67 3.70 6. 80 9. 79 0. 61 2. 13 7. 34 15. 80 4. 12 10. 27 15. 12 3.75 9. 30 3. 71 10. 30 3. 06 8. 65 9.04 5. 66 10.64 2. 81 1. 47 4. 07 1. 93 10. 67 0. 99 10. 09 9. 16 4. 07 4.75 0. 73 1. 05 0.76 8. 49 3. 25 1.61 0.88 0. 91 1. 51  4.00 3. 52 2.90 3. 86 6.13 0, 12 2. 98 7.15 4. 6 9 0. 13 2.46 3.99 0. 23 4.25 4. 54 6. 44 6.15 3.41 6.24 5. 91 3.83 5. 28 0. 22 0.09 6.72 4.78 4,83 5.16 4.29 3.62 5. 38 0.22 6.83 0. 29 8.57 4.40 7. 10 5.62 0. 27 0.07 4.24 0. 13 7, 19 4.78 6.01 7. 35 5.02 3. 18 0. 17 0. 27 0.25 6.95 3.52 0. 31 0.05 0. 38 3. 87  * DENOTES AN UNOBSERVED  REFLECTION  D i c h l o r o t s t r a k i s (dimethylsulphoxide)ruthenium (II) Anthony Mercer Observed  and James T r o t t e r  and c a l c u l a t e d  structure  amplitudes,  ( r e f l e c t i o n s with i n t e n s i t y < 3er(I) are marked with an asterisk) . The f o l l o w i n g planes which had j Fo-Fc| > 3<3-(F) were given zero weight i n the f i n a l stages of refinement due t c suspected e r r o r s r e s u l t i n g from e x t i n c t i o n , a b s o r p t i o n , or instrument m a l f u n c t i o n : h  k  1  1  2  4  3  0  h  k  1  120.4 197.0  0  8  0  130.6 218.0  121.6 222.9  1  8  1  131.8 1 87.5  4  2  145.4 207.2  4  0  2  143.0 186. 5  3  (i  1  132,7 182.0  i  o  3  1G0. 4 174.7  2  0  0  85.5 165. 0  0  2  3  98.7 189.3  4  0  0  143. 4 193. 6  0  0  4  136.5 289.8  3  2  0  122 .7 181.4  0  2  5  126. 2 194. 8  1  6  0  114.1 196.7  T T  Fo  Fc  Fo  Fc  H  K  1 3 1 2 3  0 -13 0 -13 1 -13 1 -13 1 -13 2 -13 2 -13 3 -13 3 -13 4 -13 4 -13 5 -13 0 -12 0 -12 1 -12 1 -12 1 -12 1 -12 1 -12 2 -12 2 -12 2 -12 2 -12 2 -12 3 -12 3 -12 3 -12 3 -12 4 -12 4 -12 4 -12 4 -12 5 -12 5 -12 5 -12 5 -12 6 -12 6 -12 6 -12 6 -12 7 -12 7 -12 7 -12 8 -12 8 -12 8 -12 9 -12 9 -12 0 -11 0 -11 0 -1 1 1 -11 1 -1 1 1 -11 1 -11 1 -11 1 -11 2 -11  2 3  1  2  1  2  1  2  4 1 2  3 4  5  1  2  3 4 5  1  2  3 4 1 2  3 4 1 2  3 4 1 2 3 4 1 2 3 1 2 3 1  2 1  3 5  1  2  3  4  5  6 1  L  FO  6.00* 5.74* 7.06* 6.03* 24.74 0.00* 2.88* 13.56 12.79 11.71 16.55 13.28 32.87 25.83 16.10 6.54* 26,19 26.98 14.74 22.34 5.01* 30.55 24.84 19.71 22.97 27.68 26 . 5 1 30.10 16.02 18.32 0.00* 16.63 3 2 . 21 21.02 2 9 . 18 33.29 6.60* 10.81 16.96 14.37 8. 34 17.53 23.00 23.81 16.43 11.68 12.54 13.26 49.53 40.09 12. 25 25.79 2. 1 1 * 13.63 31.37 22.52 2 5 . 14 5.41*  FC  5.33 4.36 6.33 7.82 23.03 0.85 0.70 13.06 12.55 11.47 15.35 12.94 32.97 2 5 . 17 15.48 6.88 26.11 26.01 13.84 22.33 5.14 2 9 . 27 24.17 19.24 23.57 28.08 26.33 28.69 16.32 17.99 1.34 15.97 32.34 21.64 28.53 32.25 7.16 11.01 16.14 13.32 7.67 16.79 2 3 . 38 23.26 15.89 11.08 12.67 12.63 51.02 40.59 1 1 . 12 26.58 0.81 14.31 31.82 21.98 24.32 6.66  H  K  2 3 4 5 6 1 2 3 4 5 6 1 2 3 4 5 6 1 2 3 4 5 1 2 3 4 5 1 2 3 4 5 1 2 3 4  2 2 2 2 2 3 3 3 3 3 3 4 4 4 4 4 4 5 5 5 5 5 6 6 6 6 6 7 7 7 7 7 8 8 8 8 9 9 9 9 10 10 10 11 11 11 12 0 0 0 1 1 1 1 1 1 1 2  1  2 3 4 1 2 3 1 2 3 1 2 4 6 1 2 3 4 5 6 7 1  L  n  - 11 - 11 - 11 - 11 - 11 - 11 11 11  - 11 n  - 11 11 - 11 i1  - 11 - 11 11  - 11 - 11  - 11 - 11 - 11 11 - 11 - 11 - 11 n  - 11 11 - 11 11  11  - 11  11  - 11 i1 - 11 - 11 - 11 - 11 11  - n11  - 11  -  -  !1 11 10 10 10 10 10 10 10 10 10 10 10  FO  4 1 . 19 1.52* 2 6 . 18 23.73 15.64 32.68 3 2 . 15 34.63 37.29 31.22 12.25 30.90 2.03* 31.66 3.92* 20.41 6.60* 3 9 . 11 39.52 37.66 32.29 33.47 46.56 28.50 14.68 27.90 0.00* 30.07 25.75 14.23 2 9 . 14 28.79 14.99 14. 15 34.57 9.51 28.97 34.24 15.85 ' 14.79 6.24* 20.21 6.92* 39.05 28.81 38.36 11.96 32.42 46.00 10.75 13. 10 7.71 38.54 45.32 42.75 17.45 45.27 33.77  FC  42.85 1.89 26.67 22.82 15.28 3 4 . 16 33. 1 1 3 6 . 15 36.94 30.48 11.84 32.37 4.22 32.13 5. 18 2 0 . 19 7.77 40.01 39.55 38.41 3 2 . 25 32.58 47.82 29.39 14.85 26.70 0 . 18 30.68 25.32 15.28 28.79 27.92 14.31 14.16 3 4 . 17 10.02 28.78 33.01 15.39 14.73 6.76 20.46 7.23 38.30 27.45 37.03 10.88 34.50 43.97 1 1. 10 13.35 8.04 37.41 44.33 42.37 16.37 43.97 34.52  H 2 3 4 5 6 7 1  2 3 4 5 6 7 1  2 3 4 5 6 7 1 2 3 4 5 6 1 2 3 4 5 6 1  2 3 4 5 6 1 2 3 4 5 6 1 2 3 4 5 1 2 3 4 5 1 2 3 4  K  L  2 -10 2 -10 2 -10 2 -10 2 -10 2 -10 3 -10 3 -10 3 -10 3 -10 3 -10 3 -10 3 -10 4 -10 4 -10 4 -10 4 -10 4 -10 4 -10 4 -10 5 -10 5 -10 5 -10 5 -10 5 -10 5 -10 6 -10 6 -10 6 -10 6 -10 6 -10 6 -10 7 -10 7 -10 7 -10 7 -10 7 -10 7 -10 8 -10 8 -10 8 -10 8 -10 8 -10 8 -10 9 -10 9 -10 9 -10 9 -10 9 -10 10 -10 10 -10 10 -10 10 -10 10 -10 1 1 -10 1 1 -10 11 -10 1 1 -10  FO 19.32 30,52 16.19 21.74 19.42 26.96 , 48.97 47. 35 43.13 72.69 30.97 36. 32 16.79 22.75 27.68 29.74 32.95 21.07 19.65 3.30* 46.30 45.28 64.94 30.42 49.84 12.88 27.36 8.66 41.52 14.72 23.55 14.06 30.30 40.59 2.4 2* 28.29 13.52 41.92 18.35 44.08 19.38 33.33 13.61 13.59 42.67 14. 15 20.73 0.00* 35.92 34.46 1.15* •35.96 14. 14 14.92 27.64 65.55 10.92 20.55  FC 19. 13 31.00 16.65 20.56 19.24 26.20 50.81 48.48 44.40 72.44 30.19 * 36. 10 15.89 23.05 30.04 29.22 32.19 20.40 19.28 4.51 48.25 45. 19 65.27 30.17 49. 13 12.77 27.66 9.13 42.59 14.60 22.65 14,34 30,06 41.42 3. 82 27.93 12.74 40. 68 18.75 46.07 19.80 33.78 12.75 12.97 43.19 13.08 20.51 1.29 35.71 35.44 2.07 37.29 13.99 13.73 28.23 65. 19 10.76 20.04  H  K  1 2 3 4 1 2 3 1 1 3 5 7 1 2 3 4 5 6 7 8 1 2 3 4 5 6 7 8 1 2 3 4 5 6 7 1 2 3 4 5 6 7 1 2 3 4 5 6 7 1 2 3 4 5 6 7 1 2  12 12 12 12 13 13 13 14 0 0 0 0 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 4 4 4 4 4 4 4 5 5 5 5 5 5 5 6 6 6 6 6 6 6 7 7  L  FO  -10 0.00* -10 27.43 -10 0.00* -10 20. 54 -10 52.20 -10 14.22 -10 38.82 -10 21.03 -9 22. 18 -9 38.38 -9 28.46 -9 17.21 -9 19.28 -9 27.07 -9 28.53 -9 49.35 -9 17.54 -9 8.03 -9 20.23 -9 36. 14 -9 27.77 -9 13.90 -9 14.78 -9 40.76 -9 42.49 -9 5.56* -9 7.19 -9 15.77 -9 36. 13 -9 31.71 -9 86.94 -9 51.65 -9 35.44 12.44 -9 -9 15.33 -9 11.67 -9 10.95 -9 ' 21.65 20. 18 -9 -9 14.67 2.44* -9 -9 21.88 -9 25. 13 -9 68.90 -9 30.59 -9 50. 17 -9 40.90 -9 16.78 -9 8.68 -9 28. 11 -9 33.48 -9 24.59 -9 23.09 -9 1.75* -9 18.77 -9 31.01 34. 30 -9 -9 5.51*  FC 4.45 27.82 4.67 19.01 5 2.53 12.81 38.00 20.72 22.08 38.75 27.37 16.52 19. 19 27. 12 28.75 49.72 16.52 7.39 19. 38 35.48 27.74 11.57 15.26 39.98 41.79 6.49 7.07 14.75 38.92 34.00 88.23 51.93 36.91 11.58 15. 10 1 1.77 12.61 21.26 20.64 13.92 1.44 22.04 24.88 71.81 32.40 50.46 40.45 15.99 7.66 28.44 36.34 25. 27 23.42 0.51 18.65 30.42 35.88 4.65  fl 3 4 c  •mJ  6 7 1 2 3 4 5 6 7 1 2 3 4 5 6 1 2 3 4 5 6 1 2 3 4 5 1 2 3 4 5 1 2 3 4 1 2 3 4 1 2 2 4 6 8 1 2 3 4 5 6 7 8 1 2  K 7 7 7 7 7 8 8 8 8 8 8 8 9 9 9 9 9 9 10 10 10 10 10 10 11 1 1 1 1 1 1 1 1 12 12 12 12, 12 13 13 13 13 14 14 14 14 15 15 0 0 0 0 1 1 1 1 1 1 1 1 2 2  I -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8  FO 26.8 1 7.72 24.64 24.98 30.92 32.07 15.27 29.48 0.00* 7. 17 5.31* 17.81 7.61 40.40 4.96* 5.07* 21. 16 47.84 10,30 42.51 3.96* 7.64 21. 12 12. 68 39.49 12,97 31.53 15.20 40.09 46.38 7. 29* 14.79 6.71* 17.92 6.23* 51.30 20.66 20.83 14.94 17,78 1.71* 20.34 23.10 12.57 27.9 6 39. 45 3.78* 26.21 35.65 11.29 17.48 22.60 3.21* 2.88* 33.72 40.61 31.99 27.52  FC 28.06 7.12 24.58 24. 14 29.42 33.76 15.59 31.03 0.87 7. 13 4.64 16.95 6.58 41.09 3.28 4. 25 20.23 47.77 10.68 44. 16 3.95 6. 33 21.07 11.14 41.40 13.52 31.33 15.46 40. 17 46.93 8. 32 16.56 5.99 17.08 6.54 53.53 20.67 19.62 15.01 18.27 0.92 19.74 23.89 13. 24 29.57 42. 27 2.22 25.57 34.21 10.28 17.60 23.04 1.65 5.03 33.07 39.98 33.60 27.60  H  K  L  3 4 5 6 7 8 1 2 3 4 5 6 7 8 1 2 3 4 5 6 7 8 1 2 3 4 5 6 7 8 1 2 3 4 5 6 7 8 1 2 3 4 5 6 7 1 2 3 4 5 6 7 1 2 3 4 5 6  2 2 2 2 2 2 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 6 7 7 7 7 7 7 7 8 8 8 8 8 8 8 9 9 9 9 9 9  -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 ' -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8  FO 26.74 17.33 10.20 15.78 19.35 9.69 27. 18 50.68 32.90 38.96 44.41 11.49 10.38 21.78 41.33 30.58 4.79* 19.20 22.90 20.72 25.21 24.95 34.23 33.52 44.53 48.20 10.86 29.41 13.77 7.45 17. 19 29.38 27. 13 2.24* 26.66 39.36 38.22 15. 16 23.77 27.39 12.56 0.00* 41.63 21.87 7.50* 20. 13 21.54 14.40 3.49* 3.42* 41.13 19.36 26.06 7.94 4.25* 29.47 23. 18 31.67  FC 29. 23 17.69 1 1.60 16. 15 18.53 8.09 26.37 50,83 34,96 40.54 44.26 11.36 10. 10 22. 10 42.84 30.61 4.48 20. 12 23.03 21.16 25.52 25.14 34.42 34.21 46.27 48.91 11.21 29.82 12.82 8.26 19.15 28.98 28.07 5.70 27,96 39. 14 38.09 14.27 23.39 28.38 12.66 2.82 40.78 21.07 7.23 20.26 22. 19 15.08 5.99 2. 10 40.46 18.44 25.82 7.79 3.97 29.64 23.21 31.58  H  K  L  7 1 2 3 4 5 6 7 1 2 3  9 10 10 10 10 10 10 10 11 11 11 11 11 11 12 12 12 12 12 12 13 13 13 13 13 14 14 14 14 14 15 15 15 15 16 16 16 17 0 0 0 0 0 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2  -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7  5 6 1 2 3 4 5 6 1 2 3 4 5 1 2 3 4 1 2 3 4 1 2 3 1 1 3 5 7 9 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6  X  FO 29.06 25.74 5.50* 13.45 11 .07 18.40 26.04 25.82 7.53 62.59 26.86 19,40 29.83 41,34 6.61* 35.9 4 1.99* 15.48 8.89 38.59 25.73 24.41 41.08 17.68 40.07 27.23 8.99 9.24 10.43 43.99 14.77 20.84 24.9 6 11.71 5.36* 20.91 5.64* 15.77 66. 14 49,50 28.61 54.38 46.41 20.60 42.50 17.00 19.05 10,75 10.44 38. 31 45.68 22. 12 19.30 • 38.75 48.50 60.08 32.55 31,37  FC 28.61 24.86 5.89 13. 17 10.79 19.10 25.00 25.44 9. 24 62.44 27.82 18.81 30.34 40.85 4.87 37.19 2.01 15. 25 8.77 38.05 25.66 v 25.38 42. 13 18.61 39.39 28.39 9.62 8.83 11.01 44.29 14.87 22.13 25.35 11.50 4. 32 20.59 5.29 15.67 70.44 51.67 29.64 53. 10 46.10 21.40 39.31 15.83 19.89 9.98 10.23 37.3 3 45.50 21.69 19.36 40. 16 46.71 60. 38 32.14 29.93  H  K  1  7 8 9 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 1 2 3 4 5 6 7 8 1 2 3 4 5 6 7 8 1 2 3 4 5 6 7 8 1 2 3 4 5  2 2 2 3 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 6 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 9 9 9 9 9  -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7  FC  FC  14. 17 13.58 59.54 60.33 18.86 19.28 14.92 12.45 15.50 14. 15 34.53 33.72 59.87 59. 15 24.46 24. 37 22.44 23.81 38.79 40.01 22.95 23.62 0.00* 0.51 5 5.17 58.69 3.46* 1. 16 67.39 67.02 11.02 10.43 46.66 47,86 0.54 0.00* 49.90 48.45 14.79 15.06 36. 16 36.95 77.77 78. 27 11.07 9.90 37.35 40.02 33.70 34.21 51.60 50.15 23.61 24.06 2.55* 0.61 7.41 6.82 105.83 107.08 59.41 63.18 9.21 8.70 57.84 56.94 1.73* 2.16 6 1 . 15 62.72 25.38 25.93 34.67 35.29 10.50* 8.78 51.31 54.07 4.32* 4.72 22.29 23.56 2. 14 2.56* 14.41 15.09 32.52 32.93 16.76 14.93 23.69 24.89 8.54 7.43 50.36 52.47 3.76* 2.97 39.96 39.81 3.79 4.52* 41.67 41.92 7.68 8.31 67,60 66.83 25,50 26.49 22.50 22,55 15.67 16.36 31.37 32.14  H  K  6 7 8  9 9 9 10 10 10 10 10 10 10  1  2 3 4 5 6 7 1  2 3 4 5 6 7 1 2 3 4 5 6 7 1 2 3 4 5 6 1 2 3 4 5 6 1 2 3 4 5 1 2 3 4 1 2 3 1 2 4 6 8 1  2 3 4 5  L  -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 11 -7 1 1 -7 1 1 -7 11 -7 11 -7 1 1 -7 11 -7 12 -7 12 -7 12 -7 12 -7 12 -7 12 -7 12 -7 13 -7 13 -7 13 -7 13 -7 13 -7 13 -7 14 -7 14 -7 14 -7 14 -7 14 -7 14 -7 15 -7 15 -7 15 -7 15 -7 15 -7 16 -7 -7 16 16 -7 16 -7 17 -7 17 -7 17 -7 18 -7 0 -6 0 -6 0 -6 -6 0 1 -6 1 -6 1 -6 1 -6 1 -6  FO  FC  25.41 25.83 20.23 19.93 13.. 90 13.93 1. 60* 1.02 55.21 56.64 10.46 11.04 29.04 29.09 37.31 38.68 44. 37 43. 20 22.24 22.46 40.72 41.48 30.97 32.55 37.08 38.24 35.62 38.67 26.39 26.01 28.20. 28.88 5. 33* 3.26 44.17 47.59 23. 35 24.46 47.26 47. 3 1 21.26 20.72 52.97 52.71 28.52 30.13 17.88 18.27 31.36 33.15 70.27 72.98 43.44 41.95 28.08 27.90 15,68 16.77 24.81 25.80 23.57 25.00 31.15 33.33 26. 16 27.32 33.87 34.94 4.71* 3.00 42. 10 42.09 23.74 24.85 23.90 24.45 16. 19 17. 12 15.00 15.43 7.27* 8.66 36.84 35.51 14.98 15.91 3,22* 4.69 13.99 14.96 0.00* 2.27 8. 11 8.46 16.96 17.30 9.4 4 8.75 18,20 7.97 130. 19 130.57 49.38 52.09 79.75 81.44 18.72 18.17 17.03 18,21 40.84 39.96 63.60 63.50 13.96 14.10  H  K  L  6 7 8 9 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 1  1 1 1 1 2 . 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 5 5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 6 6 7 7 7 7 7 7 7 7 8  -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6  FO  FC  6.30 5.88 35.66 34,90 42.74 42.59 16.30 16.92 63. 1 1 67.94 55.23 58,92 119.99 124.38 1.40* 2.52 72.48 72.29 38.00 39. 13 75.28 76.06 25.85 26.92 44.68 46.89 55. 14 52.43 45.43 44.05 28. 26 25.77 85. 19 85.35 62.99 63. 11 30.40 32.00 22.09 22.01 12.00 12.37 24.44 24.61 18.54 16.00 87.83 94.16 37.74 40.38 122.63 124.61 46.40 46.33 69.04 70.59 3.26* 2.83 50.88 52,92 16.31 17. 16 5.36* 1.95 47.08 46.45 89.44 86.55 36.78 38.37 49.55 49.93 19.61 19.76 39.80 39.85 16.40 16.52 5.98* 4.91 64. 85 70.50 16.07 16.54 115.28 117.93 23.06 22.70 64.06 65.08 0.00* 0.56 63.57 64.61 5.35* 2.49 37.41 37.36 91,99 91.51 28.00 28.96 11.32 11.46 16.93 16.75 17.39 18.28 34. 16 34.17 4.77* 2.60 23.48 23.86 45.86 44.83  H  K  2 3 4  8 8 8 8 8 8 8 9 9 9 9 9 9 9 9 10 10 10 10 10 10 10 10 11 11 11 11 11 11 11 12 12 12 12 12 12 12 13 13 13 13 13 13 13 14 14 14 14 14 14 15 15 15 15 15 15 16 16  5  6 7 8 1 2 3 4 5 6 7 8 1 2 3 a 5  6 7 8 1  2 3 4 5 6 7 1  2 3 4 5 6 7 1 2 3 4 5  6 7 1 2 3 4 5  6 1 2 3 4 5  6 1 2  L  -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6  FO  FC  95.97 96.3 8 17.50 17.08 53.08 55.08 24.31 24.59 56.77 56.39 7.14 7.77 29. 42 28.76 26.57 28.32 5. 17* 4.31 9.38 10.55 3.48* 3.70 3.93* 2.60 14.02 13.66 33.54 33.32 32.62 32.3 0 90.41 92.74 2.70* 3.68 87. 14 85.46 5.20* 5.17 28. 11 28.50 51.26 52.42 26.32 25.9 9 15.26 15.31 24. 23 25.33 60.49 60.98 11. 27 11. 17 2.40* 2.37 22.57 22.20 44.16 43.91 24.00 24.06 30. 33 31.08 91.87 94.42 27.87" 27.41 46.64 46.24 28. 38 30. 18 48,04 46.67 17.45 17.54 31.30 31.07 39.89 40.05 37.77 37.05 25, 2 1 26.76 34.63 35.44 13.01 13.53 19.70 19.23 53. 16 52. 20 64.11 61.77 33.91 33.69 11.01 11.21 54. 11 54.77 0.94 4.16* 18.46 18. 17 16.8 3 18.35 43. 15 44.29 5. 14* 4.02 2.40* 1.16 20.68 20.40 33.24 32.23 19.42 19.57  H  3 4 5 1 2 3 4 1 2 3 1 1 3 5 7 9 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6  K  L  16 -6 16 -6 16 -6 17 -6 17 -6 17 -6 17 -6 18 -6 18 -6 18 -6 19 -6 0 -5 0 -5 0 -5 0 -5 0 -5 1 -5 1 -5 1 -5 1 -5 1 -5 1 -5 1 -5 1 -5 1 -5 2 -5 2 -5 2 -5 2 -5 2 -5 2 -5 2 -5 2 -5 2 -5 3 -5 3 -5 3 -5 3 -5 3 -5 3 -5 3 -5 3 -5 3 -5 4 -5 4 -5 4 -5 4 -5 4 -5 4 -5 4 -5 4 -5 4 -5 5 -5 5 -5 5 -5 5 -5 5 ,"5 5 -5  FO  25.0 3 21.77 5.90* 11.05 7,46 2.47* 13.82 37.33 8.20 12.72 0.00* 117.28 134.78 66.57 69.68 38.96 73.97 71.58 26. 11 57.62 35.39 24. 11 27.96 36.91 36.77 9.32 104.08 13.40 152.06 54.70 48.95 15.29 60.84 18.38 71.60 9.45 108.73 80. 16 27.81 23.72 24. 15 31. 16 10.44 111.07 10.52 141.39 45.64 94.32 13.47 60.38 2.86* 29.73 59.09 94.47 10.75 91.4 1 78.20 44.33  FC  25.45 22. 14 6.50 12.30 8.45 0.60 13.79 38.78 8.83 13.64 3.77 136.78 148.80 66.52 69.50 40.62 75.81 70.52 26.92 58.38 33.46 23.36 28.52 37.62 37.40 5.53 107. 16 14.94 171.32 53.69 52.86 15. 18 62.15 19.28 74.88 12.09 113.24 78.21 26.73 22.44 24.64 31.91 10.76 124.71 11.91 164.09 45.37 94.78 15.05 61.91 1.82 29.85 59.93 98.52 12. 13 91. 17 75.43 43.80  H  K  7 8 9 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 1 2 3 4 5 6 7 8 1 2 3 4 5 6 7 8 1 2 3 4  5 5 5 6 6 6 6 6 6 6 6 6 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 8 9 9 9 9 9 9 9 9 10 10 10 10 10 10 10 10 11 11 11 11 1 1 1 1 11 11 12 12 12 12  L -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5  FO  FC  18,00 18.06 24.91 25.35 25. 97 26.38 91. 17 91. 30 91.88 93.86 44.77 45.58 76.80 76.48 28.9 5 30.01 74.40 74.44 33.50 34.4 2 45.32 44.99 4. 39* 3.08 57.44 57. 15 22. 20 21.98 39.52 38. 69 20.44 21 .1 1 21. 38 22.32 9. 13 7.49 50. 11 49.79 14.37 12.95 27.91 27.90 107.59 108.57 48.84 48.80 70.70 69.22 13.53 13.86 27.79 28.17 17.31 17.44 66.26 66.87 3.63* 4. 25 41.76 42.04 4. 15* 6. 16 49.85 51.04 35.02 35. 1 1 1.44 1.81* 31.88 31.89 36.73 36.05 7.14 9.38 25.26 24.60 3.33* 4.48 101,66 101.80 8.06 9.07 20,39 21.42 32.82 33.23 59,44 58.21 23.32 , 23.57 19.04 19.15 28.32 28.36 21.61 20.60 39.59 39.69 17.66 18.17 58.93 57.76 16.80 15.73 33. 20 34.02 16.75 16.02 63.41 65.03 43.84 43.79 47.67 46.88 0,00* 1.32  H  K  L  5 6 7 1 2 3 4 5 6 7 1 2 3 4 5 6 7 1 2 3 4 5 6 1 2 3 4 5 1 2 3 4 5 1 2 3 4 1 2 3 2 4 6 8 10 1 2 3 4 5 6 7 8 9 10 2 3 4  12 12 12 13 13 13 13 13 13 13 14 14 14 14 14 14 14 15 15 15 15 15 15 16 16 16 16 16 17 17 17 17 17 18 18 18 18 19 19 19 0 0 0 0 0 1 1 1 1 1 1 1 1 1 1 2 2 2  -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4  FO 52.80 42.92 33.34 4.49* 50.85 36.53 41.92 2.73* 64.87 0.00* 44.82 49.07 28.85 30.87 8.66* 54.83 1. 10* 12.60 33.44 10.58 2.07* 18.56 14.89 54.00 14.78 15.53 15.57 35.39 11.30 7.82 15.22 3.77* 20.89 0.00* 36.66 0.00* 33.92 14. 10 0.00* 27. 15 38.09 77.97 31.88 81. 12 14.56 85. 12 36.03 15.43 44. 38 13.83 11.29 30.52 56.05 27.54 20.31 9.01 74.54 3.64*  FC 51.22 43.21 33.43 6.82 52.02 38.24 4 1.40 2.07 63.99 2.87 46.28 48.51 28.73 29.80 7.84 55.04 1.36 14.01 34.92 10.33 0.41 19.91 13.55 54.35 15.16 15.00 15.79 36.78 11.27 8. 14 15.09 4.45 21.60 2.75 37.49 2.31 34.47 14.99 3.40 27.91 27.26 77.23 31.56 82.65 14.54 88.84 36.40 15.90 44.82 15. 14 12.18 32.05 57.55 28.00 21.17 8. 13 82.44 4.03  H  K  L  5 6 7 8 9 10 1 2 3 4 5 6 7 8 9 10 1 2 3 4 5 6 7 8 9 10 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 9 1 2 3 4 5  2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 4 5 5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 6 6 7 7 7 7 7 7 7 7 7 8 8 8 8 8  -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4  FO  FC  38.63 39.54 16.79 17. 52 39.27 41.91 21.52 21.79 30.69 31.72 1.64 0.00* 22.77 24.88 50.25 51 .77 34.27 30.66 42. 13 42.32 72.3 8 73.82 18.82 19.96 6.44 7.19 27.65 28.55 28.85 29.33 4.71* 6.31 33.91 40.97 91.77 92.89 22.86 24.50 1C9.72 113.23 7.22 6.96 50.72 52.13 27.54 28.62 46.07 45.72 14.09 14.72' 4.8 8* 3.65 4.60 3.23 69.47 67.59 66.84 66.98 52.89 51.03 36.90 37.28 14.07 14.82 68.56 70.11 4.68* 4.88 12.14 11 .74 70.66 74.01 41. 33 42.79 39.43 41 .54 12.87 12.53 59.31 59.10 42.81 42.05 61.31 61 .86 25.08 24.70 26.85 27.18 92. 27 92.86 31.45 33.77 20.89 18.94 21.94 22.25 59.53 60.65 28.67 29.08 38.72 38.05 33.22 32.90 27.21 27.21 66.85 66.95 71.88 72.58 9.4 4 7.13 29. 22 30. 26 10.17 10.37  H  K  L  6 7 8 9 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 1 2 3 4 5 6 7 8 1 2 3 4 5 6 7 8 1 2 3 4 5 6 7 1 2 3 4 5 6 7 1 2 3 4 5 6 7  8 8 8 8 9 9 9 9 9 9 9 9 9 10 10 10 10 10 10 10 10 11 11 11 11 11 11 11 11 12 12 12 12 12 12 12 12 13 13 13 13 13 13 13 14 14 14 14 14 14 14 15 15 15 15 15 15 15  -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4 -4  FO 71.30 23.80 38.25 12.40 85.79 7.20 38. 19 11.46 6. 13 2.97* 24.88 13.05 20.74 9 3.08 4.98* 67.26 31.01 60.97 42.23 53.95 5.56* 29.05 92.04 13. 19 54.69 22.92 51. 18 10,46 4.24* 10.83 75.67 12.83 49.61 30.88 87.95 12.80 16.67 21.82 19. 14 67.24 8.54 52.97 0.86* 21.01 52^96 37. 21 29.43 13.58 73.07 16.92 39.56 8.32 33.21 25,65 20.70 29.08 15.17 5.30*  FC 70.39 23.61 37.69 12.53 80.60 6.64 37.66 11.52 7.34 4.00 26.03 13.58 21. 16 93,75 3.67 69.22 30.45 6 1.03 39.98 52.54 2.86 27.48 92.82 12.77 54.38 22.88 51.59 9.89 1. 39 11.54 76.93 12.98 50.00 30.47 85.32 12. 13 15.22 21.62 19.30 67.42 8.84 5 2.50 1.56 21.55 54.69 38.43 30.51 14. 13 71.99 17.03 3 9.95 7.69 33.03 26. 12 20.31 28.65 15.06 5. 14  H  K  1 2 3 4  16 16 16 16 16 16 17 17 17  5 6 1 2 3 4 5 1 2 3 4 1 2 3 1 2 1 3 5 7 9 1 2 3 5 6 7 8 9 10 1  17 17 18 18 18 18 19 19 19 20 20 0 0 0 0 0 1 1 1 1 1 1 1 1 1 1 2  2 3 4  2 2 2  5  2 2 2 2 2 2 3 3 3  6 7 8 9 10 1 2 3 a 5  6 7 8 9 10 1 2 3  FO  L -4 -4 -4 -4 -4  0.00* 46.68 11.01 32.65 1.69* 30.34 29.20 17.46  -4 -4 -4 -4 -4 -4  20.03 21.96 2.98* 67.56  -4 -4  11.53 35.34  -4 -4  11.60 3 1 . 21 13.33  -4 -4 -4 -4  11.09 0.00* 44.20 65.86 31.41  -4 -3 - 3 -3 - 3 -3 - 3 -3 - 3 -3 - 3 -3 - 3 -3 - 3 -3 - 3 -3 - 3 -3 - 3 -3 -3 -3 -3 -  3 3 3 3  22.14  ,  54.54 5 3 . 28 17,47 41.94 29.01 39.59 34.90 1 8 . 18 39.93 13.48 31.44  FC 1 .65 47.66 10. 89  K  L  4  4 4 4 4 4  -3 -3 -3 -3 -3  4 4  -3 -3 -3  32.38 3.05  5 6 7 8  29.82 28.90 17.39  9 10 1  19.59 22.67 1.07 68.69 12. 39 36.71 11.26 32.06 13.91  2 3 4 5 6 7 8 9 10  11.22 1,76 45.50 6 8 . 14 30.49 1 9 . 19  1 2 3 4  54.27 55.46 17.76 37.77 32.00 37.85 37.21 1 9 . 17 41 . 5 4 13. 80  7 8 9 1  23.07 12.30 16.71 83.48 25.79 9.33 11.00 50.75 86.49  32.42 2. 22 15.29 42.01 60.99 94.52 21.31 12.33 15.31 86.6 9 27.20 7.59 10. 27 48.86 85.55  0 . 0 0 * 14.03 41.64 64.43 95.54  H  5 6  5 5 5 5 5 5 5 5 5 5 6 6 6 6 6 6  - 3 -3 -3 -3 -3 -3 -3 -3 -3 - 3 -3 - 3 - 3 -3 -3  18.97 105.61 4.46* 54. 1 1 17.23 27.79 2.84* 106.65  18.18 104.04 4.71 55.22 17.69 28.77 2.95 1 2 4 . 17 7.50 18.34  48.63 5 9 , 17  46.86 57.55 68.59  69.21 39.09 16.78 33.29 5.73* 49.56 48.56 3.78* 54.71 11.95 59.22 14.74  5 6 7 8 9 1 2 3 4  8 8 8  -3 - 3 -3 - 3 -3 - 3 -3 -3 -3 -3 -3 -3 -3 -3  5 6 7 8 9 1 2 3 4  8 8 8 8 8 9 9 9 9  -3 -3 - 3 -3 -3 -3 -3 -3 -3  23.22 11.62 42.35 7 . 17 3 0 . 15 4 6 . 11 64.51 52.56 10.93  3 4  FC  6.83 1 8 . 11  6 6 6 7 7 7 7 7 7 7 7 7 8  2  -3 -3  FO  43.88 0 . 0 0 * 6.91 87.65 8.67 6.33 11.39 3.01* 36.93 4 . 17* 7.96 86.38 7.01 69.43 2 4 , 16  40.02 17.52 33.65 5.51 48.61 45.70 7.36 53.16 11. 22 58.02 13.95 43.61 1.79 5.61 80.81 6.59 3.67 11.24 0.52 36.62 3 . 10 7.36 88.36 6.49 67.36 20.58 20.99 1 1.28 41.82 7 . 12 29.83 47.05 64.62 49.89 10.60  3 3 3  - 3 -3 -3  4.40* 27.64 35.50  2.78 3 0 . 16 34.78  5 6 7  9 9 9  -3 -3 -3  10.63 3.56* 3 . 17*  10.47 2.08 3.04  3 3  - 3 -3  34.81 22.76  34.68 23.01  8 9  9 9  -3 -3  1.30 39.00  3 3 4 4  - 3  14.45 0 . 0 0 * 56.03  15.19 2.74 53.05  1  10  -3  3.46* 39.35 23.05  2 3  10 10  74.27  73.73 92.99  4  10  5  10  -3 -3 -3 -3  4  -3 - 3 -3 -3  95.22  125.87 31.59 53.81 6.05 •  22.  12  127.32 30.71 52.92 5.54  H  K  L  6 7 8 9 1 2 3 4 5 6 7 8 1 2 3 4 5 6 7 8 1 2 3 4 5 6 7 8 1 2 3 4 5 6 7 1 2 3 4 5 6 7 1 2 3 4 5 6 1 2 3 4 5 6 1 2 3 4  10 10 10 10 11 11 11 11 11 11 11 11 12 12 12 12 12 12 12 12 13 13 13 13 13 13 13 13 14 14 14 14 14 14 14 15 15 15 15 15 15 15 16 16 16 16 16 16 17 17 17 17 17 17 18 18 18 18  -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 . -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3  FO 67.84 15.78 5.86* 17.32 53.98 20.55 44.39 9.60 16.50 19.82 4.88* 28.86 53.77 24.06 85. 36 5.00* 87.55 39.68 35. 03 15.59 5.49* 37.88 38. 13 8.79 7.65 22.00 17.74 0.00* 23.35 71,63 54.93 46.79 10.25 61.49 7.93 24.35 28.86 13.90 10.36 12.83 4.83* 6.85* 75.60 20.58 28. 60 9.77 36.23 3.39* 36.82 17.75 17.80 2.91* 4.65* 0.00* 4.62* 40.71 9.64* 36.85  FC 65.94 14.44 3.64 18.04 53.31 22.48 45.58 9. 83 15.64 19.75 6.94 28.82 51.70 24.62 84.99 2 • 3.2 87. 19 40.07 34.34 14.84 7.82 38.70 39.40 7.50 8. 25 21.05 17.88 2.31 25.00 73.56 56.32 46.97 10.67 60.52 8.66 25.53 28.88 13.69 9.28 14. 29 6.38 6.27 76.69 21.96 29.22 9.32 36.45 1. 32 38.30 18.32 18.56 2.75 3.89 3.54 2.27 40.81 9.69 37. 14  H  K  L  5 1 2 3 4 1 2 3 2 4 6 8 10 1 2 3 4 5 6 7 8 9 10 1 2 3 4 5 6 7 8 9 10 1 2 3 4 5 6 7 8 9 10 1 2 3 4 5 6 7 8 9 10 1 2 3 4 5  18 19 19 19 19 20 20 20 0 0 0 0 0 1 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 4 5 5 5 5 5  -3 -3 -3 -3 -3 -3 -3 -3 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2  FO * 8.69 0.00* 20.85 18.35 1.78* 36.57 1.74* 31.70 38.50 130.86 6.00* 100.71 26.03 29.85 56.20 64.63 6.78 25.59 4.20* 24.30 13.80 10.79 12.30 3.75* 37.23 126.94 19.33 108.23 27.53 57.85 22.09 52.45 3.33* 30.84 49.06 77.06 45.57 57.62 7.71 3.50* 32.78 38.31 13.52 14.22 113.85 16.41 148. 13 46.23 115.74 12.01 75.55 1.60* 14.84 76. 16 69. 15 33.96 27.65 10.71  FC 7.63 3.44 21.27 19.21 0.69 38.08 1. 17 33.40 33.53 144.30 4.37 105.44 26.83 33.47 55.60 64.69 8.37 25.28 3.58 26.78 14.66 11.45 12.88 7.91 37.86 156.61 19.34 113.65 28.04 58.84 21.81 56. 10 4.79 29.65 50. 19 70.32 44.35 57.28 7.25 3.46 33. 32 38.44 14.66 17. 17 134.60 15.57 172.79 44.28 110.33 12.24 74.49 1. 19 15.09 75.25 65.36 31.63 27.91 5.70  H  K  6 7 8 10 1 2 3 4 5 6 7 8 9 10 1 2 3 4 c u 6 7 8 9 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8  5 5 5 5 6 6 6 6 6 6 6 6 6 6 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 8 9 9 9 9 9 9 9 9 9 10 10 10 10 10 10 10 10 10 11 11 11 1 1 1 1 11 11 11  L -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2  FO 34.64 22.00 3.08* 4.22* 61.31 11.42 1 12.42 48. 12 84.24 17.38 58.55 10.43 57. 27 7.39* 107.99 47.31 10.11 22.67 63.81 4.00* 21.69 5.45* 43.69 30. 15 120.01 19.36 9.05 12.68 42. 12 9.54 36.23 2.27* 37.06 25.92 12.33 13. 28 23.44 29.37 6.40* 40.56 6. 3 3* 104.36 22.00 102.20 47.23 38.65 49.21 43. 13 6.7 0* 45. 27 9.6 2 10.47 12. 35 6.67 31.40 21.60 43.47 0.00*  FC  H  K  L  33.0 3 21.46 0.56 3.57 62.55 10.52 112.92 44.36 81.23 17.15 57. 13 9.12 57.04 7.63 115.04 45.12 5.90 21.40 58.86 4.57 21.42 0.59 43.06 30.25 128.28 17.61 4.68 12. 13 39.19 10.41 34.83 1.00 34.25 26.06 11 .67 12.57 21.69 28.22 7.27 38.58 5.04 105.37 18.87 100.84 45.77 37.65 48.88 41.00 4.89 43.88 9.26 9.50 8.78 4.51 31.53 21.31 42.91 1 .95  9 1 2 3 4 5 6 7 8 1 2 3 4 5 6 7 8 1 2 3 4 5 6 7 1 2 3 4 5 6 7 1 2 3 4 5 6 1 2 3 4 5 6 1 2 3 4 5 1 2 3 4 1 2 3 1 1 5  11 12 12 12 12 12 12 12 12 13 13 13 13 13 13 13 13 14 14 14 14 14 14 14 15 15 15 15 15 15 15 16 16 16 16 16 16 17 17 17 17 17 17 18 18 18 18 18 19 19 19 19 20 20 20 21 0 0  -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -1 -1  FO  FC  27.59 27.62 6.41 8.92 126.65 128.38 5.88* 3.25 48.21 46.85 14.66 14. 14 92.99 90.60 12. 18 12.55 23.67 21.80 25.60 24.21 48.31 47.78 19.79 19. 19 39.34 38.75 12.22 11.99 19.91 20.73 19.66 18.72 11.47 10.66 66. 18 67.31 53.31 51.55 49.31 49.48 4.98* 3.57 61.88 61.30 15.74 15.65 37.09 36.51 8.56 8.52 4.52* 5.60 85. 12 85.83 9.68 9.07 5.47* 6. 11 8.97 7.92 13.40 12. 13 46.66 48.08 56.90 58.00 19.70 19.95 32.93 3 2.58 17. 19 17. 16 31,43 31. 27 11.26 12.23 22. 11 22. 13 4.29* 3.54 15. 15 15.45 3,89* 5.66 11.45 12. 20 51.38 51.99 2.90* 2.88 42.58 42.92 3.60* 3.94 39.43 39.96 18.43 19. 15 0.00* 2.31 17.30 17.78 13.02 12.83 3.93* 3.73 30.79 32. 11 13.81 14.25 2.50* 0.43 0.00* 308.78 63. 15 65.93 (  H  K  L  7 9  0 0 1 1 1 1 1 1  -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1  1  2 3 4 5  6 7 "8 9 10 1 2 3 5  6 7 8 9 10 1  2 3 4 5  6 7 8 9 10 1 2 4 5 6 7 8 9 10 1 2 3 4 5 6 7 8 9 10 1 2 3 4 5  6 7 8  1  1 1  1 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 5 5 5  5 5 5  5 5  5 5 6 6 6 6 6 6 6 6  FO 51.90 73.70 13.05 10.46 30.64 29.40 28. 18 40.43 2.58* 13.04 27.85 13. 38 4.79* 96.68 29.83 21. 10 62. 19 10.88 106.87 16.48 28.26 38.01 60.49 109.28 38.69 54.45 23.09 7.85 18.41 9.38 12.79 78.88 46.78 49.01 167. 14 4.68* 94.55 9.01 67.75 3.64* 92.56 49.43 35. 31 10.56 100.90 4.64* 42.68 15.73 17.09 9.14 53.80 125.99 80.68 113,38 12.37 117.40 6.52* 82. 31  FC  H  K  L  55.56 77.21 11.48 6.17 34.08 24.46 28.60 39.62 0.80 13.97 28.89 13.05 2.92 109.38 25.37 22.31 58.91 7.64 108.22 15.94 29. 13 37.61 57.66 105.04 32.38 50.17 22.59 4.52 16.77 8.30 12.90 78.00 45.05 45.67 194.00 0.28 90. 14 8.96 65.96 1.50 97.59 45. 18 30.06 10.69 93. 36 4.48 41.64 15.80 16.38 9.06 58.03 168.29 74.17 109.19 9.44 113.39 6.27 80. 16  9 10 1 2 3 4 5 6 7 8 9 10 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 1 2  6 6 7 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 8 9 9 9 9 9 9 9 9 9 10 10 10 10 10 10 10 10 10 11 11 11 11 11 11 11 11 11 12 12 12 12 12 12 12 12 13 13  --I -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1  FO 13.79 49.31 37.80 38.42 7.06 61.79 46.22 8. 10 22.53 26.97 8.78 3.73* 127.46 55.40 97.77 6.43 40.36 14.09 73.58 1. 13* 62.09 0.00* 4.46* 33.06 15,28 44. 11 7.60 3,92* 5.71* 23.95 49. 13 121.76 12.90 40.81 23.61 112.35 20,92 44.59 25.45 24.40 16.78 13.00 26.51 15.68 23.88 2.45* 26.37 5.92* 59.93 50.36 77.33 8. 14 108.08 58.75 74.94 13.24 9.89 26.03  FC 14.78 49.31 36.00 34.59 10.74 55.08 43.57 5.00 22. 16 26.58 7.97 1.67 162.08 53.66 92.13 6.34 39.04 13.49 71.94 3.64 61.83 1.21 4.75 30.08 13.82 42.41 8.31 2,22 3.97 22.77 47.31 123. 32 11.37 38.57 24.22 110.29 21.24 42.89 25. 33 22.55 16.40 10.33 24.72 15.51 22.36 3.96 26.31 5. 12 59.73 45. 12 73.04 7.61 106,08 57.25 72.74 12.79 10.53 26.22  H  K  3 4  13 13 13 13 13 13 14 14 14 14 14 14 14 14 15 15 15 15 15 15 15 16 16 16 16 16 16 16 17 17 17 17 17 17 18 18 18 18 18 19 19 19 19 20 20 20 21 21 0 0 0 1 1 1 1 1 1 1  5 6  7 8 1 2 3 4 5  6 7 8 1 2 3 4 5 6  7 1 2 3 4 5 6  7 1 2 3 4  5 6  1 2 3 4 5  1 2 3 4  1 2 3 1 2 6  8 10 1 2 3 4 5 6  7  L  FO  FC  - •) 62.81 63.69 -1 12.60 11.56 -1 0.00* 4.53 -1 26. 35 26.65 -1 12.27 13. 27 -1 5.68* 5.55 -1 18.55 16. 86 -1 77.43 76.73 -1 21. 12 22.26 -1 38. 25 37.40 -1 26.53 25.97 -1 71.52 69. 13 -1 25.32 25.95 -1 35.61 35.66 -1 17.06 16.75 -1 53.57 52.87 -1 7.86 7.61 24.41 24. 18 -1 -1 7. 15 6.51 -1 11. 20 11.02 -1 13.32 13.31 -1 81.37 82. 19 23.66 -1 23.07 -1 42.94 42.88 -1 0.41* 0.87 -1 , 26.71 26.37 -1 15.54 14.19 -1 28. 23 28.56 -1 4.76* 6.92 -1 0.00* 1.50 -1 28.92 29.61 -1 5.35* 4.00 -1 27.68 27.38 -1 3.75* 4.62 -1 21.90 21.82 -1 53.84 55.01 -1 1.41 2.03* -1 43.93 45.52 -1 10.28 10.25 -1 0.70* 6.34 -1 6.69* 8.09 -1 4.08* 3.99 -1 11. 11 11.89 -1 28.99 30.45 -1 2.70* 3.40 -1 42.29 42.93 -1 10.8 3 11.27 -1 7.44 7 .36* 0 8.97* 13.57 0 131.75 128.68 0 49.22 50.82 0 0.00* 3.79 0 91.35 105.83 0 59.02 52.00 0 64.37 57.83 0 11 .24 14.85 0 6.4 5* 7. 14 21.94 0 22.01  H  K  L  8 9 10 0 1 2 4 5 6 7 8 9 10 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 7 8 9 10 1 2 3 4 5 6 7 8 9 10 0 2 3 4 5 6 7 8 9 10 1 2 3 4  1 1 1 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 4 4 5 5 5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 6 6 6 7 7 7 7  0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0  0  0 0 0 0  FO 18.41 7. 13* 18.74 4.87* 0.00* 52.25 23. 13 113.46 0.00* 105.10 29.81 77.78 4.72* 58.33 0.00* 87.74 26.81 34.04 42.70 0.00* 10.34* 38.84 0.00* 0.00* 84.95 93.58 56.95 144.11 12.82 143.83 16.48 1 11.63 16.23 25.21 87.37 71.83 1.72* 41. 10 43.50 0.00* 57.78 30.66 9.36 0.00* 83.76 20.69 134.47 28.94 130.85 0.00* 95.85 16.75 52.37 13.69 99.78 41.34 3.41* 13.22  FC 17.43 3.68 18.55 1.35 286.24 45.85 20.00 107.91 1.20 100.02 27. 15 75.41 8.34 60.13 3.70 84. 16 27.27 32.03 40.45 2.85 9.25 37.93 0.43 204.15 97.30 90.71 56.76 167. 14 12.57 140.44 15.75 106.85 15.74 24.71 88.77 67.49 2.58 39.06 42.31 1.87 54.60 29.72 9.87 0.96 103.25 17.32 159.23 24.65 124.77 0.59 92.39 16.33 51.43 13.00 110.68 28.20 5.61 9.77  H  K  L  5 6 7 8 9 10 1 2 3 4 5  7 7 7 7 7 7 8 8 8 8 8 8 8 8 8 9 9 9 9 9 9 9 9 9 10 10 10 10 10 10 10 10 10 10 1 1 11 1 1 11 1 1 11 1 1 1 1 11 12 12 12 12 12 12 12 12 12 13 13 13 13 13 13  0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0  6 7 8 9 1 2 3 5  6 7 8 9 0 1 2 3 5 6 7 8 9 1 2 3 4 5 6 7 8 9 0 1 2 3 4 c; ~j  6 7 8 1 2 3 4 5  6  FO  FC  35,4 8 36.63 16,37* 15.95 78.75 76.22 24.46 24.42 8.7 4 1 .82 11.95* 11.50 38.68 38.17 133.99 158.30 42.48 41.42 75.51 70.53 9.56 9.69 87.55 83.20 15.89 15. 30 33.94 37.67 11.29* 12. 13 30.88 27.37 10.48* 4.92 55.59 51.75 11.06 10.69 0. 0 0 * 2.57 21.79 21.66 2.64 3.89* 3.57* 1 .37 6.95* 3.47 13.36 11.55* 9 0 , 19 88.41 105.57 101.79 117.30 112.58 4.41 6.36* 85.20 8 1 . 25 51.18 49.03 7 7 . 14 74.69 11.88 11.98 30.26 31 .65 3. 2 0 * 4.73 33.80 36.46 37.86 37.06 2 3 . 18 24.21 6.78 7.35* 0.00* 2.55 5.69* 6.25 4.98* 4. 34 9. 25 8.72 0.00* 5.02 4,08* 7.62 101.94 104.09 4 0 . 11 40.35 76.90 75.26 59.97 57.21 127.52 123.80 27.15 26.09 26. 32 2 6 . 39 0.00* 2.79 0.00* 8.34 29.49 28.77 10.15* 11.68 0.00* 2.15 15.61 15.35  H  K  L  7 8 0 1 2 3 4 5 6 7 8 1 2 3 4 5 6 7 0 1 2 3 4 5 6 7 1 2 3 4 5 6 0 1 2 3 4 5 1 2 3 4 0 1 2 3 1 2 1 3 5 7 9 0 1 2 3 4  13 13 14 14 14 14 14 14 14 14 14 15 15 15 15 15 15 15 16 16 16 16 16 16 16 16 17 17 17 17 17 17 18 18 18 18 18 18 19 19 19 19 20 20 20 20 21 21 0 0 0 0 0 1 1 1 1 1  0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1 1 1 1 1 1 1 1 1 1  ,F0  FC  4. 3 6 * 4, 18 9. 1 5 * 9. 21 27.71 26.09 51.67 51.10 29.24 28.94 57.77 59.26 29.51 30.51 63.77 66.95 45.06 44.00 45.95 4 6 . 19 3.36* 0.33 25.44 24.33 15.94 18.08 4 6 . 19 48.56 8.98* 8.48 2 2 . 15 21.09 3.22* 2. 15 9. 16 8.52 87.41 87.43 27.80 26.98 61.63 61.32 34.36 35.31 32.97 3 2 . 14 20.43 19.89 22.64 21.75 6.23* 5.86 0.00* 0.70 24.64 2 5 . 11 15.39 15.53 17.53 17.35 9. 1 3 * 9.57 • 0.00* 0.56 2 6 . 15 24.92 62.34 61.52 16.23 16.63 43.61 4 2 . 10 23.06 23.93 17.56 17.52 37.94 37.56 0.00* 0.29 27.22 25.50 2.58* 0.81 26.05 28.05 0.00* 0.55 23.76 25.49 14.59 13.55 9.38* 9.95 0.00* ,1.45 0.00* 235.74 1 19.89 159.21 49.84 48.28 51.31 52.26 44.61 47.91 45.08 39.08 26.08 23.30 6 7 . 18 64.80 108.72 11 1.99 61.40 60.08  H 5 6 7 8 9 10 0 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 7 8 9 ,10 0 1 2 3 4 5 6 7  K  L  1 1 1 1 1 1 1 1 1 1 1 1 2 1 2 1 2 1 2 1 2 1 2 1 2 1 2 1 2 1 2 1 2 1 3 1 3 1 3 1 3 1 3 1 3 1 3 1 3 1 3 1 3 1 3 1 4 1 4 1 4 1 4 1 4 1 4 1 4 1 4 1 4 1 4 1 4 1 5 1 5 1 5 1 5 1 5 1 5 1 5 1 5 1 5 1 5 1 5 1 6 1 6 1 6 1 6 1 6 1 6 1 6 1 6 1  , FO  FC  9.18 8.49 "46.09 45.06 3.62* 2.58 14.39 13.53 16.04 15.67 9.82 9. 26 0.00* 271.73 52.05 49.55 27.68 3.82 47.40 45.34 133.86 142.76 20,47 16.94 53.46 52.42 10.46 6.26 98.53 95.25 7.94* 9.19 17.74 18.49 5.36 2.72 4.33 1.33 57.38 50.94 109.57 107.67 79.07 70.98 39.46 34.46 19.01 16.44 28.62 27.90 23.18 21.07 24.97 24.01 16.54 16.56 24.25 25.63 12.91 9.89 26.16 26.03 71.41 67.06 13.43 8.38 152.72 160.70 23,95 23.24 89.54 85.03 26.68 26.55 50.70 49.98 9.42 9.96 24.59 23.45 102.51 132.30 48.09 43.31 88.91 85.45 14.79 12.93 46.96 42.18 25.42 23.77 43.19 41.04 13.75 13. 36 23.56 22.37 3.05* 0.92 107.82 153.11 75.81 72.20 125.92 173.72 13.47 12.44 107.42, 104.63 2.08* 0.95 86.47 83.70 40.68 41.07  H  K  I  8 9 10 0 1 2 3 4 5 6 7 8 9 0 2 3 4 5 6 7 8 9 0 1 2 3 4 5 6 7 8 9 0 1 2 3 4 5 6 7 8 9 0 1 2 3 4 5 6 7 8 9 0 1 2 3 4 5  6 6 6 7 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 8 9 9 9 9 9 9 9 9 9 9 10 10 10 10 10 10 10 10 10 10 11 11 11 11 11 11 11 11 11 11 12 12 12 12 12 12  1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1  FO  FC  47.40 44.26 12.84 13.35 40.90 40.49 30.99 25. 15 1.92* 1.21 38.02 39.03 3.05* 2.93 32.82 30.65 4.63* 6.76 18.55 16.61 25.94 25.33 17.44 17.25 10.54 11.21 15.74 15.51 8.75 8.01 143.44 135.25 27.99 28.11 30.43 28.68 23.34 23.55 32.07 30.47 3.00* 0.59 34.72 34.93 30.02 27.51 48.34 44.88 25.50 22. 16 111.10 114.31 41.84 40.05 6.94 9.21 6.51 7.89 15.67 15.07 19. 14 18.62 31.43 30.26 90.83 83.57 31.04 30.00 140.08 152.83 37.08 33.40 48.11 47.44 23.74 23.05 76.98 75.61 8.41 7.26 13.66 11.92 7.57 7.47 11.12 11.92 45.97 40.81 68.36 63. 10 15.45 15.62 62.29 62. 19 0.00* 0.53 24.47 24.29 0.00* 2. 10 22.76 23.7 3 9.07 11.30 33.17 30.81 64.80 62.23 77.37 71.82 100.00 95.20 2.63* 1.08 90.74 89,72  H  K  L  6 7 8 0 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 0 1 2 3 a 5 6 7 0 1 2 3 4 5 6 7 0 1 2 3 4 5 6 0 1 2 3 4 5 0 1 2 3 4 0 1  12 12 12 13 13 13 13 13 13 13 13 13 14 14 14 14 14 14 14 14 15 15 15 15 15 15 15 15 16 16 16 16 16 16 16 16 17 17 17 17 17 17 17 18 18 18 18 18 18 19 19 19 19 19 20 20 20 20  <\  3  1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1  FO  49.65 59.84 1.92* 49.30 34.46 0.00* 0.00* 11.98 26.49 0.83* 2.47* 19.22 36.54 13. 54 97. 10 32.01 54. 10 21.34 65.45 5.11* 29. 17 0.00* 10.06 0.00* 21.37 9.67 10.20 5.88* 51.52 73.24 56.59 59.88 11.16 21.87 2.07* 34.04 0.00* 60.41 0.57* 0.00* 0.00* 25.89 4.65* 61.57 37.92 35. 14 28.63 38.09 18.60 20.51 4.46* 37.39 10.74 19.25 10.64 9.62 0.00* 24.75  FC  48.09 57. 19 3.69 46.75 34.26 3.95 0.99 10.54 26.01 3.32 1.03 20. 14 34.20 14.49 95.43 32.82 54.78 21.30 63. 48 5.86 30.07 0.51 13.20 1.58 20.3 1 8.00 10.59 6.83 52.15 72. 13 55.73 59.36 10. 10 21 .58 1.41 34.26 4. 32 59.29 1 .48 0.43 0.95 26.02 5.60 61.95 39.09 34.83 27.33 39.13 18.56 20.43 4.71 38.67 11.89 20.49 11.27 10. 19 1 .05 26.35  H  K  I  0 1 2 0 2 6 8 10 0 1 2 3 4 5 6 7 8 9 10 0 1  21 21 21 0 0 0 0 0 1 1 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 4 4 5 5 5 5 5 5  1 1 1 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2  2  3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5  2  2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2  FC 11.00 13.56 4.55* 0.00* 59.67 47.35 49.89 13.99 9.24 43.66 2.31* 106.79 47.50 11.53 2. 14* 12.72 5.60* 21.20 12.09 67.23 68.70 22.50 89.77 12.83 113.67 3.59* 29.08 1.94* 34.58 10.89 55.38 45.28 80.24 103.55 41.20 19.94 5.04* 18.00 23.83 29.95 2.92* 40.80 48.96 46.48 46.27 127.40 20.36 73.48 14.15 81.04 23.45 16.01 62.83 3.38* 15.77 44.44 6.93 54.61  FC 1 1.81 13.72 2.49 232. 16 59.39 47.03 52.34 14. 17 13.42 47.85 5.44 109. 15 44.61 10.88 0.29 13. 19 2.68 23.09 12.69 75.81 72.73 21.02 89.41 12. 15 108.20 6.25 28.81 0.92 34.49 12. 17 60.22 44.44 77.75 102. 13 36.81 17.32 1.34 15.80 23.70 29.88 2.08 43.01 48.89 40.55 45.50 128.44 20.31 72.24 12.97 79.27 24.26 14.70 57.39 0.23 12.04 38.09 4. 36 49. 11  I  H 6 7 8 9 10 0 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 7 8 9 0 1 2 3 4 5 6 7 8 9 0 1 2 3 4 5 6 7 8 9 0 1 2 3 4 5 6 7 8 9 0 1  K  L  5 5 5 5 5 6 6 6 6 6 6 6 6 6 6 6 7 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 8 8 9 9 9 9 9 9 9 9 9 9 10 10 10 10 10 10 10 10 10 10 11 1 1  2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2  FO  FC  22.74 22.21 4.01* 4.06 12.36 13.63 9. 18 7.98 6.47* 6.79 45.81 43.48 101.05 102.86 16.20 11.08 75.68 71.07 33.41 31.25 95.60 89.23 12. 33 12. 19 41.29 39.64 2. 13* 0. 16 42.03 42.45 7.21* 9. 13 42.40 43. 32 8.55 8.89 28. 15 25.16 53.90 51.27 2.85* 3.33 71.27 65.36 9.52 9.52 30.00 30.00 15.75 15.86 5.68* 5.13 111.98 120.91 8.83 6.92 129.33 141.88 36.03 33. 39 25.18 24.79 13.87 12.53 22.70 22.10 8.54 8.91 24.84 23.6C 19. 25 19. 13 44.64 48.15 19.86 18.86 65.39 62.42 7.95 5.03 33.88 33.49 23.70 21. 17 5.98* 7.07 0.79* 1.72 19.91 18. 72 9.50 8. 26 31.08 29.88 91. 11 90.63 74.08 66.89 50.70 47.97 25.84 25.51 25,61 26.70 21.28 21.93 48. 27 47.07 14.63 14.25 44. 17 45.36 18.47 18.78 48. 10 45.52  H  K  L  2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 0 1 2 3 4 5 6 7 0 1 2 3 4 5 6 0 1 2 3 4 5 6 0 1 2  11 11 1 1 11 11 11 11 12 12 12 12 12 12 12 12 12 13 13 13 13 13 13 13 13 13 14 14 14 14 14 14 14 14 15 15 15 15 15 15 15 15 16 16 16 16 16 16 16 17 17 17 17 17 17 17 18 18 18  2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2  FO 41.08 87.08 20. 12 18. 24 10.82 8.54 6.85* 9.42 3.06* 86.53 3.89* 32.58 18.67 91.37 15.32 44. 14 27.65 14.36 2.63* 15.65 7.08 7. 16 14.05 5.68* 5. 15* 21.55 59.38 16.27 64.64 30.41 57. 13 20.82 50.08 12.22 27.02 43.88 57. 19 4.36* 11.48 0.00* 0.00* 76.33 46.82 72.03 0.99* 46.54 7.04 23.04 14.54 27.65 9.02 5.83* 14.32 5.35* 17.49 36.24 45.99 21.80  FC 40.98 83.71 19.09 16.99 11.28 8.54 7. 12 11.63 1. 12 83.91 4.54 32.92 18.67 88.15 14.96 44. 29 25.28 13.42 4.34 14.05 8.20 7.84 13.55 4.93 5.32 23.45 61.61 15.64 63. 13 30.94 57. 27 21.96 50. 12 12.90 27.23 42.42 57.97 5.24 1 1.91 1.04 3.93 76.28 46.98 72.30 2.53 47.57 8.01 23.00 14.07 27.79 7.54 7.63 13.92 5.80 18.05 36.70 46.46 21.80  H  K  L  3 4 5 0 1 2 3 4 0 1 2 3 0 1 3 5 7 9 0 1 2 3 4 5 6 7 8 9 10 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 7  18 18 18 19 19 19 19 19 20 20 20 20 21 21 0 0 0 0 1 1 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4  2 2 2 2 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3  FO  55,60 9.26 30.54 0.00* 19.18 0.00* 13.44 0.00* 18.58 2.77* 28. 39 0.00* 0.00* 0.00* 1 13.56 18.39 7.95 36. 17 84.54 68.67 21,88 48.15 57.97 28.44 2.06* 21.71 26.78 8.39 3.96* 23.64 69.42 34.25 117.20 3.02* 3.3 0* 14.50 79.41 9.50 30.66 0.00* 1C0.06 14.72 36,00 56.55 77.68 7.80 13.90 16.46 25.29 13.45 10.45 52.45 16.48 27.11 6.63 116.34 29.15 74.04  FC  54.87 7.84 29.92 3.35 18.57 1.39 13.76 0.59 18.74 4.24 27.93 1.62 2.00 1.67 117.76 20.32 9.83 38.03 108.69 72.74 20.77 53.6 2 57.92 26.44 1 .09 22.47 27.76 8.17 5.33 21.15 64.58 32. 25 118.98 0.56 3.06 14.08 80.30 9.62 32.15 8.06 117.35 10. 19 34.35 52.31 75.98 6.79 14.44 15.83 26.04 14.70 5.16 53.53 15.75 27.67 7.24 111.56 29.61 71.93  fi 8 9 10 0 1 2 3 4 5 6 7 8 9 0 1 2 3 4 5 6 7 8 9 0 1 2 3 4 5 6 7 8 9 0 1 2 3 4 5 6 7 8 9 0 1 2 3 4 5 6 7 8 9 0 1 2 3 4  K  I  4 4 4 5 5 5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 6 6 6 7 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 8 8 9 9 9 9 9 9 9 9 9 9 10 10 10 10 10  3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3  FO  FC  4.83* 5.62 57.77 57.88 1.82* 2.07 32.82 29.05 9.28 7.36 26.54 24. 19 27.05 24.60 89.80 86.51 57.67 53.27 38.47 36.71 48.90 48.90 10.50 9.56 4.06* 0.39 29.03 29.62 13.21 11.55 88.87 85.64 42.23 42. 10 75.61 72.22 54.59 51.21 70.81 67.05 20.77 21.06 56.00 54.87 13. 15 14.40 84.04 85.52 69.49 69. 10 43.64 49.96 33. 17 31.83 61.12 60.03 4 4.65 43. 15 24.04 22.38 14.91 14.59 33.91 35.33 7.50 7.52 48.71 43.30 106.48 108.96 42.91 42.05 82.68 82.55 18.36 17.79 45.70 43.85 17.04 17.06 47.63 45.72 11.57 11.38 30.91 30.67 62.86 61.31 2. 17* 1.06 72.71 66. 29 18.68 17.81 4.56* 2.43 34.73 35.58 26.54 25.60 21.00 20.21 8.94 7.74 15.77 15.95 53.03 53.96 6.70 7.02 79.42 78.33 24.52 23.46 28.84 28.25  H 5 6 7 8 9 0 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 0 1 2 3 4 5 6 7 0 1 2 3 4 5 6 0 1 2  K  L  10 3 10 3 10 3 3 10 10 3 3 1 1 11 3 11 3 11 3 1 1 3 11 3 1 1 3 11 3 1 1 3 12 3 12 3 3 12 12 3 12 3 12 3 3 12 3 12 3 12 13 3 3 13 3 1 3 13 3 13 3 3 13 13 3 13 3 13 ' 3 14 3 14 3 14 3 14 3 14 3 14 3 14 3 14 3 3 15 15 3 3 15 15 3 3 15 15 3 3 1 5 15 3 16 3 16 3 16 3 16 3 16 3 16 3 16 3 1 7 3 17 3 17 3  FO 3,92* 82.02 5.03* 35.22 9.40 6. 8 9 30. 28 13.67 10.44 6.89 8.47 10.62 31. 25 11.98 53.75 12.18 14.97 41.37 16.53 81.20 38.50 83.31 3.22* 10.34 10.48 11. 17 44.73 6.05* 0.00* 26.33 10.21 11. 10 28.46 11.29 69.71 13.82 58.99 9.49 68.37 23. 26 7.90 39.99 18.34 7.09* 26.57 9. 20 2.49* 6.92* 23.37 72.40 8. 14 74.63 0.80* 18.46 9. 31 33.30 28.74 24.88  FC 1.51 79.64 0.65 34. 68 10.73 4.92 29.98 14.08 1 1.97 6.06 9.91 10.79 30.69 11.61 53.20 11.45 14.51 41 .06 16.03 78.28 37.98 80.07 1.23 8.37 13.06 12. 17 46.17 4.45 1.03 24.98 12.26 11.32 29.63 11.41 69.02 14.56 57.14 9.47 66.35 22.62 8.01 38. 34 17.51 9.82 26.98 8. 86 7.42 7.62 22.43 73. 30 8.04 74.75 1.85 18.12 9.46 32.97 29.86 25.41  H  K  L  3 4 5 0 1 2 3 4 5 0 1 2 3 4 0 1 2 2 4 6 8 10 0 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 7 8 9 0 1 2 3  17 17 17 18 18 18 18 18 18 19 19 19 19 19 .20 20 20 0 0 0 0 0 1 1 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 4 4 4 4  3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4  FO 0.00* 5. 13* 28.66 69.27 15.37 49.88 9.45* 38.90 21.28 19.93 9.00 '17.46 0.00* 20.81 10.56 36.20 8. 19 91.33 103.61 28.59 80.48 38. 36 71.44 108.58 26.53 28.87 82.16 10.95 5.98 2.04* 15.65 32.55 3,59* 6. 18 110.60 42.88 61.94 25.30 94.97 1.79* 80.01 10.43 68.41 5.07* 70.26 45.00 42.08 75.82 55.89 31.60 2.54* 44.86 33.27 8.24 99.24 66.76 74.20 2.36*  FC 3.80 4.20 29.73 69.55 15.54 49. 24 10.79 39.01 21.61 20.83 9.75 18. 11 0.99 21.03 10.68 35.72 8.77 88.71 104.19 30.35 86.06 41.80 74.61 149.24 25.50 28. 13 82.20 10,94 5. 15 1.48 15. 14 34.95 0.81 7.36 143.58 40.38 61.21 25.27 96.08 0.71 82. 18 11.03 71. 17 5.85 71.99 42.55 38.87 71.48 54.86 32.61 1.13 45.00 33.91 9,51 105. 12 61.80 70.82 4.44  H  K  L  4 5 6 7 8 9 0 1 2 3 4 5 6 7 8 9. 0 1 2 3 4 5 6 7 8 9 0 1 2 3  4 4 4 4 4 4 5 5 5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 6 6 6 7 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 8 8 9 9 9 9 9 9 9 9 9 9 10 10  4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 - 4 4 4 4 4 4 4 4 4 4  ii  5 6 7 8 9 0 1 2 3 4 5 6 7 8 9 0 1 2 3 4 5 6 7 8 9 0 1  FO 73.85 24.99 106.98 35.04 97.70 0.00* 9.07 67.36 38.65 17. 17 24.98 56.14 16.05 16.02 36.68 19.86 54.08 83.48 49.7 1 79.77 29.55 109.54 8.73 65.88 31.61 49.33 50.44 42.38 78. 21 7.29 54.22 26.44 34.47 44.99 5.09* 3,80* 111.96 0.00* 149.07 27.49 82.21 26.62 73.12 27.90 15.20 3.09* 11.86 74.34 0.00* 59.49 33.08 21.38 26.99 30.66 8.39 14.38 48.90 96.36  FC 73.51 23.63 105.17 35.49 96.60 0.26 5.81 64.33 36.70 17.77 24.41 54.3 9 16.75 16.37 36.06 20.13 51. 10 80.95 45. 12 76.26 28. 14 108.33 9.24 64.83 32.40 49.25 50. 19 41 .76 76. 36 7.97 53. 15 23.92 32.79 44.52 2.66 3.39 111.56 1.97 169. 1 1 26.36 78.00 26.77 72.93 27.85 15. 11 2.52 12.01 69.80 3.76 58,13 30.76 21.27 27.09 30.26 4.99 14. 17 48.08 92.97  H  K  L  2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 0 1 2 3 4 5 6 7 0 1 2 3 4 5 6 0 1 2 3 4 5 6 0 1 2  10 10 10 10 10 10 10 11 11 11 11 11 11 11 11 11 12 12 12 12 12 12 12 ' 12 12 13 13 13 13 13 13 13 13 14 14 14 14 14 14 14 14 15 15 15 15 15 15 15 16 16 16 16 16 16 16 17 17 17  4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4  FC 53.91 101.80 10.58 67.08 25.57 48.89 6.51* 4.35* 28.36 26.54 27.12 10.71 31.12 58.66 13.11 9.82 3.90* 12.77 73.82 21.25 47.63 33. 13 89.41 19.03 35.85 10. 19 9.76 13.67 12.11 23.78 40.73 0.00* 38.24 3.21* 35.91 27.74 76.08 0.00* 54.68 23.08 47.35 23.64 36.65 30. 15 39.29 27.87 0.00* 30.44 71.33 24.81 66.26 23.52 43.24 17.64 22.58 0.00* 35.92 19.36  FC 51.48 100.99 9.96 66. 11 25.22 47.61 6.63 1.30 30.85 25.64 26.95 10.68 30.90 57. 16 13.60 9.51 1.42 11.50 72.21 20. 12 45.71 32.95 87.99 20.50 34.67 9. 19 8.27 13.67 11.81 24. 13 41.19 1.21 38.17 0.21 3 5.89 27.9 3 74.46 4.92 53.61 23.44 46.88 22.91 36.79 30.86 40. 10 27.80 4.02 31.22 70.24 25. 17 66.22 24.40 42. 19 17.22 21.87 0.72 35.29 19.55  H  K  L  FO •  3 4 5 0 1 2 3 4 0 1  17 17 17 18 18 18 18 18 19 19 19 19 20 20 20 0 0 0 0 1 1 1 1 1 1 1 .1 1 1 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 4  4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5  21. 35 0.00* 13.92 0.00* 37.57 24.73 36.21 32. 17 18,94 9.73 '6.30* 5. 18* 35.44 4.88* 12.88 1 18.65 125.0 3 127.17 60.54 97.03 35. 11 39. 19 68.56 32.83 25.59 6.68 13.00 34,33 14.02 7.90 96.42 59.33 144.88 42.98 80.85 22.21 77.04 12.62 5. 1 1 76.38 37. 27 28.82 89.91 40.40 31.44 21.13 24.22 45.52 21.03 97.88 27.52 63.07 39.83 135.83 21.51 79.29 26. 10 63.35  3 0 1 2 1 3 5 7 0 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 9 0 1 2 3 4 5 6 7 8 9 0 1 2 3 4 5 6 7 8 9  FC 21.84 3. 1 1 13.29 3.26 36.93 24.38 36.96 33.61 19.09 9.86 6.88 6.70 35.92 5.15 12.78 148.10 136.50 134.44 63.97 106.08 35. 13 42.58 70.97 34.30 24. 27 8.16 13. 56 35.88 15.28 7.14 99. 34 59.13 156.31 43.67 82.69 21.99 79.40 14.10 1. 18 76.43 32.26 27.77 86.58 39.38 30.77 21.90 25.40 49.15 19.99 102.06 27.34 61 .69 38.55 138.70 21. 17 79.62 27,09 65.79  H  K  L  FO  IC  0 1 2 3 4 5 6 7 8 9 0 1 2 3 4 5 6 7 8 9 0 1 2 3 4 5 6 7 8 9 0 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 8 0  5 5 5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 6 6 6 7 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 8 9 9 9 9 9 9 9 9 9 10 10 10 10 10 10 10 10 10 11  5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5  18.92* 19.06 16.27 70.96 30.73 12.96* 38.91 25.76 25. 11 5.92* 83.06 41.97 116.29 22. 17 89.74 12.65 79.48 54.95 49.28 5.21* 18.97 75.09 45.66 62.86 29.75 30. 18 8.41 14.47 6.81* 10.61 32.70 142.44 37. 10 117.04 33.82 64.93 23.89 27.90 12.32 29.37 5.68* 104.91 94.47 13.82 25.53 31.98 14.09 13.43 98. 16 9.32 125.15 50.38 38.27 40.28 47.78 26.64 25.79 28.50  20.91 21.03 17.47 67.93 28.56 13.16 39. 18 26.60 25.63 5.95 80.04 38.53 117.48 20.37 86.49 12. 16 79.08 55.07 48.86 3.06 17.80 73.09 45.72 61.68 29.00 28.63 8.53 15.01 6.91 11.43 32.46 157.34 36.88 113.57 33.91 62.76 23.48 27.20 12.91 28.74 8.83 99. 39 90.74 13.27 23.81 3 1.89 13.00 14.42 94.57 9.69 122.46 48.86 36.90 39.21 46.41 25.28 24.80 27.42  H  K  L  1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 0 1 2 3 4 5 6 7 0 1 2 3 4 5 6 0 1 2 3 4 5 6 0 1 2 3 4 5 0 1 2 3 4 5 0 1 2 3 4 0 1 2  11 11 11 1 1 1 1 1 1 1 1 1 1 12 12 12 12 12 12 12 12 13 13 13 13 13 13 13 13 14 14 14 14 14 14 14 15 15 15 15 15 15 15 16 16 16 16 16 16 17 17 17 17 17 17 18 18 18 18 18 19 19 19  5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5  FO 18.32 34.49 30. 11 41.86 18.33 31.44 15.75 4.10* 11.20 42.14 46. 90 43. 38 9.48 39.07 31.46 44.97 18.38 13.40 41.05 11.94 20.08 17.00 39.87 0.00* 30.44 47. 48 60.96 0.00* 43.61 4.53* 41.03 23.45 38. 39 6.32* 43.30 13.77 21. 21 0.00* 33.47 40.53 39.70 66.24 7.71 22.04 28.64 17.20 36.81 5.16* 12.64 19.46 39. 35 31.54 18.73 18. 11 27.94 2.76* 15.90 6. 27*  FC 17.57 32.45 29.34 40.70 17.86 31 .95 16. 13 1.21 11.28 40.98 45.79 42.06 9.09 38.74 31.34 45. 17 17.53 12.93 39.25 11.07 19.58 17.00 40.88 2.66 28.34 47.28 59.08 2.27 43. 13 4.3 0 40.98 22.57 36.99 8.01 42.91 14.86 22.38 0.75 33.52 39.76 40.03 65.14 7.48 21 .50 29.39 16.46 36.09 7.49 12. 14 19.57 39.90 31.96 19.00 18. 27 28.59 7.59 16.51 6.06  H  K  L  0 2 4 6 8 0 1 2 3 4 5 6 . 7 8 9 0 1 2 3 4 5 6 7 8 9 0 1 2 3 4 5 6 7 8 9 0 1 2 3 4 5 6 7 8 9 0 1 2 3 4 5 6 7 8 9 0 1 2  0 0 0 0 0 1 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 4 5 5 5 5 5 5 5 5 5 5 6 6 6  6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6  FO 116.17 91.05 145.24 4.64* 23.44 65. 16 56.49 17.43 12.50 62.65 27.84 3.61* 4.91* 15.03 14.08 ' 35.11 104.87 34.60 111.45 57.31 75.62 8.73 31.78 0.00* 29.61 6.31 10.03 27.02 53.00 34.25 30.96 18.74 31.81 27.98 8.44 81.74 29.72 71. 19 52.05 95.08 7.77 51.54 18.81 50.47 17.21 61.22 13.52 26.51 13.25 15.09  FC  135.91 94.07 156.29 9. 26 24.48 65.77 55.49 17.80 13. 18 62.27 28.46 3.59 5.02 15.40 15.42 36.03 110.30 35.69 116.29 58.39 76.35 8.62 33.35 2.91 31.51 7.91 11.53 26.65 51.63 32.60 29.95 18.47 32.45 29.98 10. 19 78.07 28.66 68.50 48.94 93.69 6.09 51.56 19.51 51.43 17.95 62. 13 12. 1 1 26.69 1 1.81 13.39 44.53 44.50 0,00* 3.21 20. 19 20.22 29,04 31.03 11.89 11. 22 59.11 60. 18 79,23 80.81 16.53 14.42  H  K  L  3 4 5 6 7 8 0 1 2 3 4 5 6 7 8 0 1 2 3 a 5 6 7 8 0 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 0 1 2 3 4 5 6 7  6 6 6 6 6 6 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 8 9 9 9 9 9 9 9 9 9 10 10 10 10 10 10 10 10 10 11 11 11 11 11 11 11 11 12 12 12 12 12 12 12 12  6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6  FO 67.09 14.80 70. 12 19.31 45.9 2 8.84 21. 38 56. 15 58.34 . 49.09 21. 24 29.07 24.77 8.83 6.66* 91.19 22.63 96.09 60.42 59.51 4.87* 48.07 22.35 21.90 61.42 54. 10 67.78 35.59 30.07 11.97 15.04 2.66* 12.20 22.39 72. 87 46.08 49.35 32.69 30,79 30.97 45.56 0.00* 4.30* 20.35 38.79 44.08 28.62 32. 19 16.38 22.32 40.17 12.73 34.37 0.00* 19.08 19.01 50.40 24.93  FC 65.95 14.81 69.92 18, 18 45.61 9.58 21. 19 56.62 53,27 48,84 21.27 28.35 23.4 1 8.90 7^.04 86.21 20.56 93. 18 60.60 60.7 3 3.67 47. 32 22.62 22.06 57.55 51.87 65.41 35.47 30.91 12.76 12.35 0.68 12.06 22.24 70.82 45.99 48.08 31.36 30.36 31.29 45.76 1.99 1.09 20.84 37.37 44. 39 28.58 30.51 16.98 22. 10 39.03 12.42 33. 12 3.01 19.46 19.93 51. 26 26.59  H  K  L  0 1 2 3 4 5 6 0 1 2 3 4 5 6 0 1 2 3 4 5 0 1 2 3 4 5 0 1 2 3 4 0 1 2 3 0 1 1 3 5 7 0 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7  13 13 13 13 13 13 13 14 14 14 14 14 14 14 15 15 15 15 15 15 16 16 16 16 16 16 17 17 17 17 17 18 18 18 18 19 19 0 0 0 0 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2  6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7  FO  FC  30. 49 30. 19 29.03 28. 12 29.66 28.33 6.91* 5.60 9.18 9.09 6.99* 5.72 18.87 19.27 42. 14 41.06 23.03 22.63 20.97 22.09 52.88 52.37 15.33 15.55 30.45 31.96 18.40 18.08 26.40 25.62 40.49 40.72 46. 13 44.93 2.69* 4.42 9.61 9.51 27.71 26.88 40.70 42.27 38.50 39. 14 44.24 44.76 0.00* 2. 23 45.97 47. 18 14.47 15. 11 3.38* 0.26 41.01 41.21 15.60 15.04 21.07 21.64 20.84 21.21 14. 12 14,54 23.73 23.62 14.87 15,79 4 1.79 41.36 16,79 16.30 0.97* 2. 19 100.15 105.48 50.84 55.58 12.45* 10.76 17.23 16,25* 71.94 72.95 44.01 43.69 22.57 20.22 48.49 48.85 48. 36 47.82 15. 12 15. 10 19.22 19.47 3.53* 4.26 0.00* 2.26 100.78 101.59 27.84 27.36 49.64 50.62 30. 12 29.71 43.74 43. 36 5.90 4.93* 11.23 7.98 10.94 12. 10  H  K  L  8  2 3 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 5 5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 6 6 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 8 9 9 9  7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7  0  1 2 3 4 5 6 7 8 0  1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 8 0  1 2 3 4 5 6 7 8 0  1 2  FO 30.08 56.22 35. 31 19.66 6.78 30.72 19.62 23.34 1.78* 29.23 37.26 72.97 5.39 21.97 2.19* 35.72 21.06 34.39 11.07 6.83 3.38* 9.49 0.00* 22.29 3.07* 20. 19 37.29 11.81 32.59 26.04 55.37 19.82 40.77 63.62 47.01 13.92 21.62 83.89 31.35 21. 32 42.91 1.32* 9.82 11.72 11.67 20. 15 36. 18 47.03 29. 32 51.32 6.38 46.70 9. 15 25.04 3.56* 7.13 23.50 47.60  FC 31.43 55. 94 35. 14 19.52 5.41 32.09 19.68 24.29 2.82 29.83 38.38 73.21 7.51 22.90 1.61 35.59 21.40 35.35 12.25 8.38 4.28 7.60 0.77 23.24 2.44 19.87 38.52 11.11 33.11 27.76 54.77 21. 12 40.59 63.32 46.61 14.89 21 .80 81.06 30.74 18.98 42.86 4.01 9.91 11.46 12.05 21.51 35.65 48.15 28.28 52.15 3.49 46.04 8. 31 25.40 1.04 8.22 25.03 45.48  H  K  L  3 4 5 6 7 0 1 2 3 4 5 6 7 0 1 2 3 4 5 6 7 0 1 2 3 4 5 6 0 1 2 3 4 5 6 0 1 2 3 4 5 0 1 2 3 4 5 0 1 2 3 4 0 1 2 3 0 1  9 9 9 9 9 10 10 10 10 10 10 10 10 11 11 11 11 11 11 11 11 12 12 12 12 12 12 12 13 13 13 13 13 13 13 14 14 14 14 14 14 15 15 15 15 15 15 16 16 16 16 16 17 17 17 17 18 18  7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7  FO 38.84 3. 16* 12.34 26.00 35. 16 21.80 12.81 46.91 29.22 31.43 15.03 46. 11 14.49 30.53 0.00* 15.04 1.71* 14. 13 1.31* 34.75 32.77 20.49 13.91 17.71 34.57 2.70* 33.83 21.06 4.36* 37.30 4.89* 9.39 8.57 19.07 43.28 15.22* 17.46 32.20 0.00* 38.51 8.41 36.96 19.90 36.54 19. 12 14.21 12.30 4. 12* 19.91 18.75 50.92 11.24 26.85 26.51 30.30 20.78 47.90 3.37*  FC 38.57 3. 22 12.55 25.50 37.13 21. 15 12.77 45. 26 28.07 29.96 15.03 44.94 15.78 31.71 0.59 13.96 1.36 13.98 1.62 35.35 32.94 18.49 15.82 17.01 32.58 0.25 33. 12 22.52 1.91 36.70 5.24 8.26 7.52 18.86 42.99 16.21 16.54 32.01 2. 12 38.27 7.73 36.04 19.97 36.32 19.13 14.83 12.79 6.28 20.43 18.53 51.18 1 1.98 26.69 26.82 31.40 20.78 48.73 4.01  H  K  L  0  0 0 0 0 0  8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8  2 4 6 8 0  1  2 3 4 5 6  7 8 0  1 2 3 4 5 6  7 8 0 1 2 3 4 5 6  7 8 0 1 2 3 4 5 6  7 8 0  1  2 3 4 5 6  7 8 0 1 2 3 4 5 6 7  1  1  1  1 1 1 1 1  1  2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 5 5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 6  I  8  's 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8  FO  59.55 5. 11* 30.22 24.95 31.05 73.74 85.65 22.72 35.47 51.53 21.00 9.23 4.48* 19.95 49. 19 39.28 29.77 18.84 18.17 30.59 13.17 33.25 8.74 65,52 5.01* 6,61 15.09 19,24 22.79 8.26 25. 20 34.51 26.88 44.25 9.93 3.02* 13.38 21.80 31.04 24.53 33.11 10.90 37.36 10. 14 7.47 24.00 21.97 19. 11 25.63 16.77 41.19 52.37 28.67 12.63 20.92 43.37 22.49 20.48  FC  61.08 5.14 30.79 25.53 32.82 70.87 83. 51 22.49 35.97 51 .55 19.06 9.17 1. 17 20.80 48.21 40. 18 31.69 18.53 18.00 31.00 13.55 33.45 8.77 63.60 2.58 5. 18 16.10 17.93 22.54 8.58 26.76 36.16 25.61 42.72 11.31 1.95 13.03 21 .35 31 .33 25.36 34.23 12. 12 36.23 10. 12 6.97 22. 09 22.17 18.81 26.33 17.07 41.69 54. 17 27.65 11.71 20.69 43.35 23.34 20,34  H  K  I  0 1 2 3 4 5 6 7 0 1 2 3 4 5 6 7 0 1 2 3 4 5 6 7 0 1 2 3 4 5 6 0 1 2 3 4 5 6 0 1 2 3 4 5 6 0 1 2 3 4 5 0 1 2 3 4 0 1  7 7 7 7 7 7 7 7 8 8 8 8 8 8 8 8 9 9 9 9 9 9 9 9 10 10 10 10 10 10 10 11 11 11 11 11 11 11 12 12 12 12 12 12 12 13 13 13 13 13 13 14 14 14 14 14 15 15  8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8  FO  27,93 7,75 57. 13 44.85 27.54 19.93 37.34 14.26 20.29 33.71 55.80 3.56* 34.37 24. 17 27.25 13.97 6.74 30.80 19. 13 61.55 31.98 23.46 23.78 17.45 40. 10 55.52 5.06* 38.41 9.70 27. 15 11.33 13.94 10. 15 36.83 11.89 10.26 17.07 50,42 32.53 1.77* 48.83 1.93* 29. 11 3. 18* 24.05 16.60 5.93* 12.00 18.59 5.68* 28.91 7.91 17.95 22.45 43.93 6.99* 5.36* 32.24  FC  27. 12 8.33 54.83 42. 12 28.49 19.30 36. 15 14.89 21.36 33.76 54.40 2.92 33.68 24.65 26.84 13.49 6.09 28.86 17.41 59.77 32. 24 22.38 24.52 16.73 39.02 55.01 4.57 37.82 9.37 26. 11 11.35 12.92 10.14 35.97 10.23 9. 15 17.47 50.00 31.88 4.41 48.22 2.68 27.81 0.37 23. 12 16.00 5.63 11.57 17.69 3.63 29.51 6.92 17.62 21.34 43.80 8.52 4.34 33.41  B  K  2 3 4  15 15 15 16 16 16 16 17 17 0 0 0 0 1  0 0  2 3 0  1 1  3 5 7 0  1  2 3 4 5  6 7 0  1 2 3 4 5  6 7 0  1  2 3 4 5  6 7 0 1  2 3 4 5  6 7  1 1  1 1 1 1 1 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4  0  5  1 2 3 4  5 5 5  5  5 5 5 6 6 6 6 6  6 7 0 1  2 3 4  5  L 8 8 .8 8 8 8 8 8 8 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9  FO 30.81 3.75* 22.35 26.75 27.29 25.00 8.00* 18.39 30. 12 33.24 44.51 58.87 32.33 56.70 44.59 19.89 45.42 63.40 44.86 21.09 19.27 16.62 55.16 20.05 18.85 57.28 18.29 34.76 18.52 33. 32 39.13 4.70* 2.36* 39.06 43.87 15.70 30.71 9.48 30.52 15.81 19.52 27. 23 41.88 0.00* 25. 15 39. 18 25.77 11.43 30.92 31.70 19.51 40.23 11.41 25.83 21.55 38.45 21.57 35.97  FC 30.64 4.06 21 .87 26. 13 26. 13 24.47 9.25 17.55 29.85 34.36 45.75 59.37 32.45 55.42 44.05 21. 17 45.96 64.02 45.33 20.80 20.68 16. 24 55.06 20.70 16.77 57.52 18.49 35.24 19.13 34.31 37.74 5.20 1 .35 39. 16 44.23 15.39 32.23 9.22 31.35 15. 27 19.54 27.79 43.03 0.39 26.04 39.24 25.52 11.14 30.42 31 .03 19.07 41.17 11.12 26.13 21.12 38.18 21.71 34.85  H  E  L  5 6 7 0 1 2 3 4 5 6 0 1 2 3 4 5 6 0 1 2 3 4 5 6 0 1 2 3 4 5 6 0 1 2 3 4 5 0 1 2 3 4 5 0 1 2 3 4 0 1 2 3 0 1 2 0 0 2  6 6 6 7 7 7 7 7 7 7 8 8 8 8 8 8 8 9 9 9 9 9 9 9 10 10 10 10 10 10 10 11 11 11 11 11 11 12 12 12 12 12 12 13 13 13 13 13 14 14 14 14 15 15 15 16 0 0  9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 10 10  FO 27.34 33.82 8.80 20.88 50.28 51.30 58.33 43.69 35.95 2.39* 13. 19 49.06 16.45 25. 18 13.80 30. 11 4. 12* 26.72 20.86 82.85 43.67 35.26 10.81 35.55 48.34 25.07 39. 19 12.47 15.56 8.98 15.88 6. 10* 40.80 14.75 46.28 10.49 21.74 0.00* 36.72 3.63* 25.09 3.49* 9.32 19.63 10.76 43.00 3.61* 11.92 19.85 23.47 19.05 10.09 0.00* 39.23 0.00* 14.65 52.27 67.07  FC 27.58 34.59 8.74 21.09 48.54 50.77 58.21 42.55 35.40 1.85 13. 34 48. 13 16.72 25.23 13.39 30.70 2.03 27.14 20.06 81.14 43. 22 34.82 11.41 35.54 47. 16 25.28 38. 23 12.22 15.46 10. 12 16. 12 4.80 38.47 13.52 45.22 11.21 21.95 3.34 36. 29 3.60 25.87 3.55 9.88 18.70 9.76 42.77 2.56 12. 22 19.73 23. 18 19.12 10.08 1.58 37.51 3.01 14.64 51.94 69.81  fi  K  L  4 6 0 1 2  0 0 1  10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10  r  4 5 6 0 1 2 3 4 5 6 0 1  2 3 4 5 6 0 1 2 3 4 5 6 0 1  2 3 4 5 6 0 1  2 3 4 5 6 0 1 2 3 4 •5 6 0 1  2 3 4  c.  0  1  1 1 1 1  1 2 2 2 2 2 2 2 3 3 3 3 3 3 3 4 4 4 4 4 4 4 5 5 5 5 5 5 5 6 6 6 6 6 6 6 7 7 7 7 7 7 7 8 8 8 8 8 8 9  FO 57.97 27.62 55.85 52.78 37.46 54.88 64.02 53.99 22. 21 16.86 55. 18 5.93* 59.9 1 21.53 33.92 7.43 47.95 40.51 22.82 21.90 54.90 23.87 27.37 28.62 4.81* 54.65 37.23 37.63 11.43 27.66 46.45 45.77 21.00 39.70 16.82 39. 19 14.37 45.51 36. 32 22.25 34.98 12.86 40.82 21.22 42. 49 32.42 59,98 25.24 40.20 10.85 35.24 18.77 5.94* 26.42 27.86 26.45 7.47* 26.24  FC 58.27 28.69 55. 24 53.06 38. 10 55.80 64.90 54.92 22. 87 16.37 55.04 5.82 60.35 21.50 34.00 8.78 48.31 40. 15 24.50 21.31 54.93 24.00 27.76 27.96 4.96 54.68 37. 10 37.50 11.55 28.69 45.73 45.59 21.64 38.87 16.02 39.99 13.40 44.66 36.23 22.92 35.33 12.62 41.06 21.62 42.74 31.33 59. 18 24.31 40.27 10.74 36.34 18.29 6. 23 25.44 26.87 26.30 8.61 25.55  H  K  L  1 2 3 4 5 0 1 2 3 4 0 1 2 3 4 0 1 2 3 0 1 2 0 1 1 3 5 0 1 2 3 4 5 0 1 2 3 4 5 0 1 2 3 4 5 0 1 2 3 4 5 0 1 2 3 4 5 0  9 9 9 9 9 10 10 10 10 10 11 11 11 11 11 12 12 12 12 13 13 13 14 14 0 0 0 1 1 1 1 1 1 2 2 2 2 2 2 3 3 3 3 3 3 4 4 4 4 4 4 5 5 5 5 5 5 6  10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11 11  FO 44.90 23.35 58.76 8.50 20.37 7.63* 20.86 0.00* 16.72 18.41 32.47 18.37 42.86 6.82* 2. 17* 20. 10 1.33* 17.97 2.94* 8.25 28.02 12.24 12.95 5.67* 45.96 17.81 13.69 49.77 49.59 34.61 32.33 37.24 26.65 49. 13 22.96 34.63 4.32* 13.88 2.93* 52.00 47.28 18.80 20.33 16.28 17.09 24.70 48. 18 3.71* 27.71 5.04* 22.21 49.04 22.29 30.73 8.45 13.55 25.79 23.19  FC 43.72 22.78 57.44 7.04 20,13 6.00 20.71 2.90 17.00 18.83 31.64 16.90 42.73 6.42 1.47 20.18 3.73 16.21 3.23 7.99 27. 21 11.44 11.58 2. 18 45. 26 18.59 14.10 49.44 48.77 34.90 33.03 38.98 27.46 49.01 22.49 34.83 0.35 14.25 0.64 51.50 47.51 18.83 20.25 16.41 17.85 23.78 47.66 3.67 27.51 3.59 23.02 48.48 22.60 30.27 7.87 14.63 25.87 22.75  e  1  K  6 6 6 6 6 7 7 1 2. 7 3 7 4 7 0 8 1 8 8 2 3 8 4 8 0 9 1 9 2 9 3 9 4 9 0 10 1 10 2 10 3 10 0 11 1 11 2 11 0 12 1 12 0 0 2 0 4 0 1 0 1 1 1 2 1 3 1 4 2 0 1 2 2 2 3 2 4 2 2 3 4 5 0  L  FO  11 21.89 11 35.97 11 17.44 / 11 25. 19 11 20.92 11 15.90 11 29. 13 11 16.80 11 38.64 1 1 21.08 11 27.73 11 27.09 4.93* 11 11 21.29 11 10.09 11 10.59 11 15.79 1 1 42.27 11 17.95 11 17.80 11 20.32 11 0.00* 11 26.72 11 12.83 11 29.65 11 6.63* 11 20.94 11 0.00* 1 1 » 17..40 12 20.16 12 5. 11* 6.54* 12 37.04 12 12 23. 28 12 11.20 12 7.69 20.69 12 12 11.13 12 16.90 12 20.23 12 8. 23 12 8.36  FC 21.13 35.42 17.56 25.79 21.79 15.75 28.85 16.96 39.28 21.08 27.91 26.86 5.95 21.52 9.12 10.49 15.52 39.75 17.00 17.20 19.34 1. 12 26.01 12.27 27.64 6.3 8 19.79 0.65 16.41 19.78 4.75 6.93 35.32 22.73 12.02 7.27 20.55 10.64 16.56 19.35 7.93 7.82  H  K  L  0 1 2 3 4 0 1 2 3 4 0 1 2 3 0 1 2 3 0 1 2 3 0 1 2 0 1 0 1 0 1 2 0 1 2 0 1 2 0 1 0 1  3 3 3 3 3 4 4 4 4 4 5 5 5 5 6 6 6 6 7 7 7 7 8 8 8 9 9 -2 0 1 1 1 2 2 2 3 3 3 4 4 5 5  12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 12 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13  DENOTES AN UNOBSERVED REFLECTION  FO 36.81 25.77 0.00* 10.37 4.93* 21.27 18.67 18. 1 1 10.27 14.59 16.96 18.01 18. 30 3.50* 22.08 22.68 ' 1.74* 8.46 14.57 15.80 23.42 29.61 22.50 3.65* 11.64 15.66 10.48 7.48* 4.05* 12.50 15.47 2.02* 8.73 16.92 5.42* 25.26 5.39* 13.89 5.33* 0.00* 18.99 19.88  FC 36.03 26.29 2.28 9.95 5.07 21.03 18.72 17.78 10.00 13.78 17.87 18.04 18.03 0.60 21.29 22.29 0.06 8.09 14.05 15. 10 22. 24 28.53 21.93 2.55 12.06 15.62 9.64 6.84 4.34 12.98 15.22 1.40 6.84 16.40 7.03 24. 12 5.27 13.27 5.37 2.93 18.09 19.08  Acetyl-3-benzamido-2-keto-4-(2,4,4>6-tetra-C-acetyl glucopyranosyloxy)-A -pyrrolire 3  Anthony Mercer, and James T r o t t e r Observed and  calculated structure  amplitudes  ( r e f l e c t i o n s with i n t e n s i t y < 3o-(I) are marked w.ith asterisk) .  H  K  I  0- 11 0- 11 0- 10 0- 10 2 3 0- 10 4 0- 10 5 0- 10 6 0- 10 7 0- 10 8 0- 10 9 0- 10 1 1- 10 2 1- 10 3 1- 10 4 1- 10 5 1- 10 6 1 -10 7 1- 10 ' 8 1- 10 9 1- 10 1 2- 10 2 2- 10 3 2- 10 2- 10 « 5 2- 10 6 2- 10 7 2- 10 1 3- 10 2 o — 10 3 3- 10 a 3- 10 5 3- 10 1 0 -9 2 0 -9 3 0 -9 4 0 -9 5 0 -9 6 0 -9 7 0 -9 8 0 -9 9 0 -9 10 0 -9 11 0 -9 12 0 -9 1 1 -9 2 1 -9 3 1 -9 4 1 -9 5 1 -9 6 1 -9 1 -9 7 8 1 -9 9 1 -9 10 1 -9 11 1 -9 12 1 -9 1 2 -9 2 -9 2 1 2 1  FO  8. 45 6. 17 11. 92 7.09 8. 74 4. 07 0. 00* 3. 89 3. 83 2. 57* 5.77 9. 47 4. 45 3.36* 6. 89 9. 05 4.61 3. 35* 3. 6 0 0. 00* 3. 13* 3. 10* 4.90 2.79* 4. 10 1.30* 3. 36 4. 22 4. 15 6. 16 4.47 21. 07 12. 58 3. 04* 2. 24* 15. 07 3.87 4. 14 4.46 10. 24 0. 00* 4. 29 4. 86 9. 13 2.79* 13. 80 3. 55* 12. 97 7. 14 2. 85* 4. 05 6. 53 2. 28* 3. 81 4. 17 5.67 9. 18  FC  HEIGHT  H  K  L  8.99 6, 22 1 2. 29 8. 12 10. 32 4. 02 0.42 2. 25 3. 01 3.03 6.56 10. 23 4.31 4. 19 7. 35 10. 34 3. 23 3. 64 3, 13 0, 36 1.91 3.61 3. 43 2. 11 4. 20 2. 67 1. 79 3. 95 2.92 3. 63 6. 90 3. 60 21. 90 12. 08 3.82 1,47 16.81 3. 48 3. 84 5. 00 11.14 1. 63 4. 36 4. 96 10. 50 3. 22 15. 49 4. 33 14. 02 7.47 5.54 3. 77 5. 69 1.93 2.70 2.75 5.25 9. 29  6.18 7. 12 4. 99 5. 28 4. 68 2..84 0. 00 4. 47 3. 53 0. 17 6. 54 4. 79 3. 94 0. 19 5. 35 5. 44 5. 69 0. 26 3. 48 0. 00 0. 21 0. 21 5.98 0. 18 3.20 0.04 4. 22 3. 50 0. 10 2. 95 4. 39 4.21 2. 56 4. 23 0. 19 0. 11 3. 60 3. 02 3. 36 3. 11 5. 22 0. 00 4. C8 4. 29 5. 08 0. 16 4. 24 0. 20 4. 39 5. 12 0. 11 4. 30 5. 91 0. 12 3. 53 5. 67 4. 14 5. 04  3 4 5 6 7 8 9 10 11 1 2 3 4 5 6 7 8 9 10 1 2 3 4 5 6 7 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 1  2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 2 2  -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -9 -8 -8 -3 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8  2  FO  FC  HEIGHT  4.60 5. 26 6. 06 4. 67 7.36 7. 80 2.43* 1. 98 5. 25 5. 55 5. 28 4. 49 2.92* 3. 91 1. 56* 3. C4 5, 98 . 5. 47. 1. 46* 1. 18 12. 78 13. 67 1 . 38* 1. 94 4. 87 4. 95 2. 62* 4. 97 7. 83 8. 19 3. 52 2. 1.8 2.51* 1. 78 3. 39* 3. 32 4.59 3. 93 4. 72 4. 59 0. 00* 0. 11 1 . 30* 0. 63 4. 96 4. 66 0.49* 3. 19 2.71* 2. 19 2. 52* 2. 09 11. 12 10. 92 4.68 4. 81 21.30 2 1. 4 G 12. 55 12. H2 4. 54 3. 77 4. C4 3. 72 17. 70 18. 03 17. 96 19.31 4. 03 3. 96 0. 00* 0. 57 3. 65 2. 17 3.58* 3. C4 6. 58 6. 45 2. 83* 1. 64 0.94* 1. 15 4. 58 4. 26 5.59 5. 94 8. 32 10. 25 7. 53 9. 21 5. 24 6. 58 8.78 10. 32 6. 46 5. 92 5.41 6. 22 2.18* 4. 67 2. 62* 2. 26 3.53* 4. 68 4. 17 3. 72 4.07 4. 87 3. 24 4.10 3. 94 3. 36 6. 35 7.36 12. 56 13. 44  2. 67 5. 30 6. 09 0. 12 3.92 4. 91 0. 19 0. 05 6. 52 0. 05 4. 76 0. 04 3. 57 0. 12 5.07 2. 95 0. 16 0. 28 5. 26 3. 14 0. 00 0. 04 4. 16 0. 00 0. 16 0. 15 4. 29 3, 42 2. 50 5. 73 3. 59 3. 17 3. 51 3. 31 2. 57 0.00 3. 64 0. 25 6. 09 0. 24 0. 02 2. 94 3. 20 4. 95 5. 16 3. 12 5. 26 3. 41 3. 42 0. 08 0. 14 0. 24 2. 88 2. 95 5. 19 3. 50 5.67 4. 41  H  K  I  3 4 5 6 7 8 9 10 11 12 13 14 1 2 3 4 5 6 7 8 9 10 11 12 13 1 2 3 4 5 6 7 8 9 10 11 1 2 3 4 5 6 7 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15  2 2 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 3  -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -c -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -8 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7  3  3 4 4 4 4 4 4 4 4 4 4 4 5 5 5 5 5 5 5 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0  FO  FC  12.98 1 3. 67 7.08 6. 83 10. 68 10. 20 17. 26 16.77 3. 23* 3.32 3.57* 2. 50 6. 17 6.53 5. 44 4. 67 0. 62* 0. 86 3.42* 2. 26 3.30* 3. 05 3. 51 2. 04 8. 16 8.42 6. 00 6. 38 14. 07 13. 14 6. 65 6. 60 10. 71 10. 38 7.50 6. 11 4. 0 8 4.75 3. 92 3. 05 6.46 5. 96 2. 85* 2. 93 3. 31* 2. 45 3. 78* 3. 77 0. 00* 2. 23 6.91 6. 52 6. 21 6. 12 7. 91 8.72 6. 80 5. J C 4.02 3.02 5. 03 5. 68 4. 36 3. 94 5.35 6.4 2 4. 04 3. 37 0. 00* 1.20 3.81 4, 00 3.55* 3.49 4. 45 3.55 5. 94 6.32 5.31 5.58 3. 44* 2. 92 2. 94 3.69 3.42* 3. 32 18.73 19. 31 3. 53 2. 13 5. 19 5.06 4. 60 4. 09 0. 00* 2. 15 14. 34 16.31 3. 20* 0.45 6.00 5.40 14. 44 13. 74 2. 46* 1. 12 10. 61 11. 05 4. 99 3.98 7.39 6.88 4. 36 5. 83 2.30 0.00*  HEIGHT  H  K  L  FO  4. 54 6. 13 5. 64 3.86 0. 21 0. 30 4. 52 6. 02 0. 01 0. 31 0. 21 3.48 6. 37 3. 89 4. 15 4. 22 5. 07 3. 87 4. 06 3. 13 5. 73 0. 17 0. 30 0. 27 0. 00 3. 62 3. 93 4. 81  16 17 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 1 2 3 4 5 6 7 8 9  0 0 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 4  -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 —7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7  2. 26* 3. 94 5. 15 22. 19 12. 05 8. 35 4.18 11.57 9. 44 11.68 8. 49 20. 22 3.06* 8. 32 0. 00* 2. 87* 3. 14* 4.21 10.36 9. 47 3.64* 6. 99 15.03 4.93 19. 50 8.11  3.93  3. 28 4. 31 3. 17 3. 66 3. 10 0.00 2.79 0. 22 3.42 3. 26 3. 28 0. 23 2. 87 0. 25 3. 14 3. 59 4. 28 4. 06 0. 00 4. 60 0. 28 4. 14 4. 96 0. 14 4. 77 5. 49 5. 87 6. 47 0. 00  FC  1. 62 2. 93 5. 20 20. 39 11. 06 9. 25 5. 12 11. 56 10. 49 1 1. 95 9. 22 22. 62 3. 45 9. 68 0. 71 1.71 1. 39 3. 11 11.51 9. 58 4. 55 7. 44 15. 49 4. 50 19. €3 9. C6 19. 51 13.31 4. 32 4. 55 5. "0 6.15 4. 33 2.79* 3. 97 3. 99 2.24* 1. 75 2.22* 1. 30 2.14* 1. 17 6. 54 6. 51 6. 24 5.78 4 . 68 5. CO 23. 75 22. 33 5.42 5. 08 13.44 14. 04 6.92 7. 20 8. 05 8. 77 5. 40 5.72 7. S9 7.79 4. 33 4. 96 2. 14 2.31* 1. 74* 1. 53 0. 91 2.01* 2. 94 3.61 16. 23 19. 12 8. 17 8. 22 3. 99 3.31* 4 .00* 4. 47 10.46 10. 57 -4. 09 5. 22 8. 51 7.06 6. 55 5. 88 6. 44 6.93  HEIGHT 0.13 4. 29 4. 89 2.50 5. 11 7. 22 3. 48 5. 66 . 5. 42 5. 01 5. 40 2. 87 0. 19 5. 55 0. 00 C. 21 0. 35 5. 39 6. 67 5. 41 0.26 5. 06 4. 65 3.73 2. 77 5. 28 3. 17 3. 02 4. 59 0. 13 2. 63 0. 14 0.16 0. 13 5.01 5. 50 3, 36 2. 47 4. 48 4. 46 4. 61 4. 96 4. 26 7.27 2. 48 0. 12 0. 07 0. 11 3. 01 3. 60 5. 08 C. 19 0. 22 4.74 4. 60 3. 94 3. 73 7. 15  H  K  I  10 11 12 13 1 2 3 4  4 4 4 4  -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -7 -6 -6 -6 -6 -6 -6 -6  5  6 7 8 9  10 11 1 2 3 4 5 6  1 2 ~j  4 5  6 7 ts 9  10 11 12 13 14 15 16 17 18 1 2 3 4 5  6 7 8 9  10 11 12 13 14 15 16 17 18 1  5  5 5 5 5  5 5 5 5 5 5 6 6 6 6 6 6 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 2  -6  -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6 -6  ro  FC  WEIGHT  2. 74 4. 07 4.66 1.98 5.68 6. 06 1.81 4. 38 5.41 6. 26 2. 67 4. 21 5. 07 4. 36 0.81 8. 28 4. 23 4.88 5. 49 7. 88 0. 39 9.74 7. 51 4. 74 22.41 1 4. 99 4.98 1 8.79 12. 15 12.5 i 6. 19 7. 81 5.95 5.71 3.38* 3.32 2. 96* 3. 00 25.76 28.12 6.77 6.67 3. 83 3. 25 0. 00* 0. 96 4. 45 3. 59 0. OC* 0. 89 2. 81* 1.65 11. 30 11. 30 14. 86 13. 83 6. 42 6. 07 16. 21 16.45 17.77 16.31 14. 89 13. 35 3. 64 4. 35 12. 59 14. 38 7. 53 8. 26 9.77 8.60 15. 54 17.02 6.71 6. 10 2. 47* 0. 93 5. 53 6.45 3. 15* 3. 47 3. 85 2. 61 3. 40 3. 15 22.79 20.86  3. 51* 2.76* 4. 62 2. 43* 5.17 5.78 2. 19* 3.85 3. 63* 6. 3E 1.91* 3.52* 4.73 5.06 2. 42* 7. 05 4. 05 4. 47 3. 67* 6. 23 0. 28* 9.81 7.68 6. 35 21. 40 14. 92 6. 24 19. 99  0. 25 0. 17 3. 79 0. 17 2. 77 4.30 0. 09 2. 49 0. 16 4. 87 0. 06 0. 22 2. 85 3. 87 0. 18 4. 49 2. 62 2. 34 0. 22 3. 83 0. 00 8. 05 7. 99 6. 06 2.75 4.70 5. 46 2. 90 5. i 5  4. 95 5. 69 0. 28 0. 20 1.81 5.83 3. 03 0. 00 5.35 0. 00 0. 27 5. 82 4. 81 6. 08 3. 88 3. 66 4. 59 2. 86 6. 06 5. 67 5.07 4. 11 4. 66 0. 16 4. 10 0.21 4.51 3. 29 2.42  H  K  L  2 2 -6 3 2 -6 4 2 -6 5 2 -6 6 2 -6 7 2 -6 8 2 -6 9 2 -6 10 2 -6 11 2 -6 12 2 -6 13 2 -6 14 2 -6 15 2 -6 16 2 -6 17 2 -6 1 3 -6 2 3 -6 3 3 -6 4 3 -6 5 3 -6 6 3 -6 7 3 -6 8 3 -6 9 3 -6 10 3 -6 11 3 -6 12 3 -6 i3 3 -6 14 3 -6 15 3 -6 16 3 -6 1 4 -6 2 4 -6 3 4 -6 4 4 -6 5 4 -6 6 4 -6 7 4 -6 8 4 -6 9 4 -6 10 4 -6 11 4 -6 12 4 -6 13 4 -6 14 4 -6 15 4 -6 1 5 -6 2 5 -6 3 5 -6 4 5 -6 5 5 -6 6 . 5 -6 7 5 -6 8 5 -6 9 5 -6 10 5 -6 11 5 -6  FO  FC  4. 96 5.86 2.78* 2. 97 5. 30 6.15 4.20 4. 80 13. 46 14. 86 0. 59* 2. 08 14. 49 13.90 2. 85* 2. 22 17. 14 16.48 9. 67 9.78 3. 28* 2. 41 9.99 9. 82 4. 70 4. 55 2. 84 4.72 5.10 4. 16 0. 95 3.51 9. 96 11.95 14. 28 12. 56 4.40 3. 93 4.54 3. 70 6. 38 5. 26 5. 29 5. 44 10.67 9. 97 0.00* 2. 24 8.02 7. 63 7. 88 6. 69 6. 29 7. 09 8.98 9. 15 2. 5 7 * 0 . 5 i 5.78 4. 99 2.25* 1. 62 2. 90* 1. 02 12. 46 12.88 15. 79 14.90 3. 08* 4. 26 3.44* 5. 18 3.54* 2. 18 11.82 12. 29 7.47 7. 95 7. 79 7. 88 6. 89 6.97 6.41 6. 83 4.08 4. 32 4. 56 5. 18 6. 67 6.54 4.21 2. 68 2.53* 0. 54 6. 32 5. 99 7.37 8. 17 16. 31 15. 13 7.35 8. 33 13.76 14. 80 14. 54 13.02 6. 67 6. 67 4. 09 3.59 4.57 4. 31 2.31* -2. 66 3.87 2. 67  WEIGHT  6. 63 0. 23 5. 11 2. 71 4. 60 0. 01 4. 53 0. 18 3.78 5.42 0. 28 6. 27 2. 68 5. 31 4. 05 4, 24 5. 49 4. 52 4. 06 4. 05 5. 54 4. 54 5. 33 0. 00 5. 27 6.50 4.11 5. 66 u. 1 /  4. 45 0. 12 0. 27 4. 60 4. 27 0. 17 0. 20 0. 28 4. 52 4. 38 5.57 4. 47 4. 09 2. 69 4. 68 5. 15 4. 08 0. 23 4. 82 4. 70 3.79 3. 69 3.83 4. 16 4. 90 3. 35 2. 36 0. 10 2.80  H 12 13 1 2  3 4 5 6  1  8 9 1 2 1 2 3 4 5 '6 7 8 9 10 11 12 13 14 15 A*  K  L  5 -6 5 -6 6 -6 6  -6  6 6 6 6 6 6  -6 -6 -6  6 7 7 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0  -6 -6 -6 -6 -6 -6 -5 -5 _ t; -5 -5 _ c  -~*  -5 -5 -5 -5 -5 -5 -5 -5  ^  1 U  17 18 19 1 2 3 4 5  6  7 8 9 10 11 12 13 14 15 16 17 18 19 1 2  3 4 5 6 7  V  0 0 0 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2  _ 5  -5 -5 -5 -5  -5  -5 -5 -5 _c -5 -5 _c -5 -5 _ c  -5 -5  -5 -5 -5 -5 -5  -5 -5 -5  -5 -5 -5  FO 2. 5 2 * 2. 8 3 * 5. 4 6 4. 0 4 4. 1 5 2. 8 6 * 1. 5 6 * 4. 8 6 3. 8 7 * 4.44 3.50* 4.66 3. 1 9 * 14.38 24. 89 26. 60 2.80* 18. 05 1 5 . 86 5. 0 8 5. 3 5 10. 28 21.64 3. 8 2 8. 3 3 5. 5 1 11.23 6.71  FC  2. 7 9 2.31 5.69 3.73 3. 7 6 0. 2 8 1. 4 0 6. 4 1 4. 5 8 2. 8 3 3. 3 9 5.50 4. 2 2 13. 95 23.79 28.39 3. 0 7 17. 95 15.12 5. 20 5, 3 9 9. 6 8 20. 70 3. 1 8 8. 7 6 5. 3 4 12. 20 5. 9 0 7.13 2. 2 0 * 2. 0 6 2.67* 2. 36 3.39* 2. 1 6 2. 2 7 * 3.79 14. 32 13.91 17. 68 18. 92 16. 7 7 18. 9 3 7. 1 3 8. 3 0 18.83 21.59 12. 98 13. 05 14. 46 13. 85 2.48* 1.38 6. 6 6 6. 6 1 3. 9 4 4. 8 6 15.44 13. 55 5.64 5. 2 9 7. 7 6 8. 2 0 3.63 1.40 7. 4 9 8.99 4. 4 7 2. 6 7 1. 9 0 3.20* 0. O C * 0. 9 8 13. 31 11.15 17. 64 16.44 17.08 1 9 . 51 28. 50 26. 50 16.09 14.45 4. 3 2 3. 9 2 14. 80 13. 30  HEIGHT  H  K  L  FO  FC  HEIGHT  0.11 0.23 3. 0 2 2. 2 7 2. 4 0 0. 14 0. 0 4 3. 7 9 0. 2 6 3. 6 8 0. 2 2 2. 8 0 0.15 5. 1 5 2. 14 1. 9 6 0. 4 0 3. 4 0 4. 4 3 5.71 5. 9 3 7.36 2. 5 7 3. 8 0 6. 0 0 4. 7 7 5. 2 1 5. 0 0 4.75 0. 1 3 0. 2 0 0. 3 4 0. 2 4 5. 1 2 3. 5 8 3.39 8. 1 0 2. 6 7 5. 4 0 4. 9 1 0. 2 1 6. 8 5 2. 7 6 4.94 4. 4 4 7. 5 4 3. 6 5 4. 6 5 4. 9 6 0. 2 8 0. 0 0 5. 5 5 3.74 3. 2 1 1. 6 6 4. 2 1 4.45 4. 3 9  8 9 10 11 12 13 14 15 16 ;-7 18 19 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15  2 2 2 2 2 2 2 2 2 2 2 2 3 3 3 3  -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -5 -c  17.04 3. 1 0 * 2.73* 16.41. 6.67 6.54 1 2 . 12 9.54 5.71 0.79* 3.33* 1. 5 1 * 17.93 7. 2 3 10.90 6. 0 8 8.78 7.97 1 0 . 13 1 3 . 84 7.33 7 . 12 6.46 5.06 6.60 6.52 4. 8 3 3. 3 0 * 3.51 1.79* 5. 2 2 1 2 . 17 12.42 4. 2 2 5.59 3.61* 3. 3 9 * 9. 3 3 12.23 5. 7 9 5.97 7. 08 7.89 5.12 0.66* 2.10* 4.74 7. 19 7.72 18.61 4. 3 8 5.33 5. 8 8 4.97 4.50 3.06* 4.82 3.59*  1 4 . 31 2. 2 5 3. 6 2 16. 60 7. 24 6. 9 1 1 3 . 19 9. 8 0 5. 6 1 1. 8 5 2. 3 5 0. 7 3 1 7 . 18 6. 6 7 10. 52 5. 7.8 7 . 34 8. S 8 9. 6 8 1 5 . 19 6. 9 8 7. 2 4 6. 6 3 4. 8 9 7. 2 5 5. 9 5 4. 9 6 2. 8 2 1.29 1. 10 3. 61 11. 77 1 3 . 36 3. 5 9 6. 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C9 3.23* 3. 20 5.74 4. 39 6. 36 7.03 6. 66 6. 81 3. 15* 0. 77 2. 86* 5. 97 25.21 23.78 8. 45 6.51 3. 11* 1. 33 3.85 2. 59 6. 58 6. 36 4. 66 4.76 7. 69 7.69 6. 71 6.41 14. 41 14.00 3. 16 4.10 4. 73 5.36 11.96 11. 63 10. 89 11.51 6. 77 7.10 4. 57 4.92 1.63* 1. 99 4. 42 4.99 13. 84 14. 75  4. 62 5.50 4.91 4. 66 0. 17 3. 56 3. 83 4. 91 5.62 5. 68 0. 23 0. 15 0. 30 4. 96 3. 25 3.91 4.60 4.69 4.56 2. 40 4. 84 0.01 3. 86 2.26 0. 30 3. 02 0. 05 4. 18 3. 72 4. 32 0. 26 3. 06 4. 12 0. 17 0. 20 5. 19 5. 45 4. 75 0. 26 0. 26 2.03 6.27 0. 40 3. 81 7. 27 4. 48 6.23 6.25 4. 30 3. 43 4. 62 4. 79 5. 26 5. 92 5.67 0. 07 4. 85 4. 93  H 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 0 1 2 3 4 5 6 7 8 9 10 11 12  13  14 15 16 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 0 1 2 3 4 5 6 7 8 9  K 1 1 1 1 1 1 1 1. 1 1 1 1 1 1 2 2 2 2 2 2 2 2 o c 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 4  I  FO  '  7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7  1.32* 17. 91 6. 22 3. 80 7. 05 0. 00* 14. 78 3.81* 7. 57 3. 07* 2.49* 8. 46 2. 13* 6. 31 2.81* 11. 37 9. 45 6.18 7. 79 21. 06 7. 83 10. 71 12. 23 1.51* 6. 70 8. 56 6. 31 5. 49 10. / 2 2. 70* 4. 22 5.54 12. 23 13. 27 16. 57 6. 87 12. 82 14. 38 10, 59 5. 82 12. 08 4. 13 7. 20 9. 6 8 8.75 9. 72 5.78 5. 97 11.91 19. 52 7.87 5. 06 6.86 9. 39 9. 14 9. 37 8.68 4. 34  FC  WEIGHT  H  K  L  1. 53 16. 90 5. 76 5. 19 7. 50 1. 55 14. 45 3. 94 7.98 2. 11 0. 88 8.66 0. 15 6. 03 2.54 10. 78 9.44 5, 22 6. 66 20. 68 8. 61 10. 59 11.59 0.77 5. 58 8. 57 7.42 6.61  0.06 3. 42 5. 49 2. 86 6. 19 0. 00 4. 37 0. 24 5. 37 0. 18 0. 15 4. 83 0. 12 4. 97 0. 16 5. 82 6. 77 5. 24 5. 33 2.73 5. 01 5. 08 4. 74 0.05 5. 78 5. 48 4. 50 3. 31  10 11 12 13 0 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 0 1 2 3 4 5  7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 8 8 8 8 8 8  10. 1"5  5.11  4 4 4 4 5 5 5 5 5 5 5 5 5 5 5 6 6 6 6 6 6 6 0 0 0 0 0 0 G 0 0 0 0 0 0 0 0 0 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 2 2 2 2 2  2. 70 4. 25 5. 10 11. 05 12. 53 16. 22 5. 87 12. 26 1 5. 27 10. 42 5.68 12. 19 3. 94 6.57 9.76 9. 34 9.21 6. 04 6.08 11. 17 20. 25 7. 58 4.95 5.44 9. 60 8. 31 9. 21 8.85 2. 81  0.13 3.31 4. 58 4. 64 4. 66 3. 76 6. 53 5. 24 4. 44 5. 70 4. 40 5. 22 3. 32 5.92 4. 64 6.49 5. 98 4.34 5. 02 5. 34 2. 91 5. 52 5. 64 4. 37 5. 06 5. 57 6. 24 5. 55 3. 61  6  7 8 9 10 11 12 13 14 15 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 0 1 2 3 4  8  8 8  8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8  FO  FC  2.65* 3. 63 8.05 7. 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C9 10. 39 10. 60 5.32 5. 87 7. 38 7. 16 4. 04 3. 35 2. 33 3. 95 4. 56 4. 36 2. 99 1 . 78* 3.45 4.88 1. 64* 2. 51 8.57 8. 37 12. 23 12.85 6.51 7.36 4. 11 . 4.96  WEIGHT 0. 12 5. 86 .3. 76 0. 29 5. 02 4. 80 5. 52 3. 23 0.17 0. 12 0. 06 2. 97 5. 53 5. 71 0. 23 6. 14 2. 88 0.22 2. 43 5.18 0. 31 5. 23 6. 26 4. 45 0. 17 5. 47 6. 76 5. 92 0.13  2. 76 2. 83 0. 26 0. 15 2. 62 0. 24 0. 19 0. 29 0. 27 5. 45 5. 47 5. 20 5. 98 4. 85 4. 71 5. 19 5. 58 3. 82 5. 12 3. 16 4. 03 2.55 0. 06 5. 08 0. 05 5. 86 4. 82 4.79 4. 45  H  K  I  5  2  8  6  2  8  7  2  8  8  2  8  HEIGHT  FC  FO  H  K  L  WEIGHT  FC  FO  8.  17  5 . 4 5  3  9  3 . 0 2 *  1.  17  0.  17  10.  48  4.  31  4  1  9  4.  3.  32  3.  71  6 . 7 5  6.  33  5.  67  5  1  5.  17  4.  0 3  31  8 . 5 9  5.  43  6  1  9 9  5 . 7 2  8.  5 . 2 9  5.  18  3 . 7 0  7 . 8 1 10.  33  60  9  2  8  2.  61*  3.  83  0 . 1 3  7  1  9  7.  46  7.  28  5.  10  2  8  3.  3 9 *  2.  65  0.  27  8  0.  0 0 *  1.  99  0 . 0 0  11  2  8  5 . 6 8  5 . 4 7  4.  20  9  i1  9 9-  10.  43  10.  20  5.  12  2  8  4 . 5 0  3.  55  3.  31  10  1  9  4.  48  2.  73  5 . 1 9  13  2  8  3.  1.  88  0.  31  11  1  9  3.  83  4 . 2 0  2.  84  11  2  8  1.56*  1.  29  0 . 0 7  12  1  9  3.  66  3.  97  2.  92  0  3  8  5.  36  4 . 5 6  4.  66  0  2  9  5 . 0 0  4.  77  •3.  42  1  3  8  8.  02  7 . 5 8  4.  28  1  2  9  4 . 4 0  4.  89  2.  39  2  3  8  5.  24  4 . 4 4  3.  17  2  2  9  4.  4.  08  5.  11  3  3  8  16.  16  16.  3.  67  3  2  9  5 . 2 3  6.  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S3  2.  52  5  8  2 . 8 6 *  2 . 4 9  0.  15  6  4  9  5.  5.  43  3.  98  5  5  8  4 . 3 3  3.  4.  14  7  4  9  3 . 4 3  1.  56  3.  35  6  5  8  7.  30  7 . 5 2  5.  33  0  0  10  6 . 5 1  4.  46  5.  63  7  5  8  2.  9 2 *  3.  29  0.  22  1  0  10  5.  89  0  0  9  3.  27*  0.  25  0 . 2 6  2  0  10  12.  80  a  16*  50  0 2 * 25  4. 11.  57  5.  14  97  4.  45  4 . 9 6  3  0  10  0 . 0 0 *  0.  31  0.  00  0.  86  0.  4  0  10  1.  8 6 *  0.  63  0.  08  1 . 9 8 *  1.  10  0 . 0 8  5  0  10  2.  6 6 *  2.  39  0.  19  9  0 . 0 0 *  2 . 3 1  0.  00  6  0  10  4 . 0 2  2.  44  2.  85  1 1 . 0 0  1  0  9  2  0  9  0.  3  0  9  0  0 0 *  1 0 . 6 8  00  5  0  9  6.  32  6.  67  5.  30  7  0  10  2.  0 3 *  0.  45  0.  10  6  0  9  3.  74  3.  12  2.  75  8  0  10  4.  49  5.  46  2.  70  7  0  9  3 . 0 3 *  3.  38  0.  17  9  1.  2 2 *  0.  18  0.  04  0  9  5.  5 . 2 1  5.  06  0  0 1  10  8  10  6 . 2 2  5.  80  4 . 6 1  8.  39  5.  65  5.  13  98  5.  74  86  12  9  0  9  3.  59*  1.  0.  30  1  1  10  9 . 3 5  10  0  9  5.  94  5 . 6 5  5.  51  2  1  10  1 2 . 6 7  11  0  9  0 . 0 0 *  0 . 5 7  0.  00  3  1  10  9 . 8 9  8.  12  0  9  2.  97*  0.  0.  28  4  1  10  0 . 0 0 *  0.  78  0.  00  1  9  4.  66  3 . 6 1  3.  83  5  1  10  6.  6.  24  5.  29  4.  72  6  1  10  4 . 1 4  5.  29  2 . 5 5  6.  16  7  1  10  4.  1.  93  5 . 2 6  0 1  1  9  2  1  9  12.  45  9 . 4 6  10.  72  71 3 3  8 . 8 9  83 24  11.  H  K  L  8  1 2 2 2 2 2 2 2  10 10 10 10 10 10 10 10  0 1 2 3 4 5 6  FO  FC  2. 50* 4. 17 4. 85 3. 83 4. 41 4.58 5. 89 6. 28 6.48 5.68 5. 86 5. 53 13. 86 12.79 6. 54 5. 74  WEIGHT  H  K  L  0.12 4. 39 3. 19 3. 96 4. 44 3..56 4. 73 5. 65  7 0 1 2 3 4 0 1  2 3 3 3 3 3 0 0  10 10 10 10 10 10 11 11  * DENOTES AN UNOBSERVED REFLECTION  FO 4. 17 7.76 3.56 5. 38 2.01* 6. 08 1. 80* 10.38  FC 3. 6. 3. 4. 1. 5. 1. 9.  64 31 53 87 19 45 72 45  WEIGHT 3. 7. 3. 5. 0. 6. 0. 5.  55 00 20 62 11 58 10 50  

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