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Crystal structures and solid state reactions of maleic anhydride and of a cyclohexenone and its photoproduct Hwang, Christine 1988

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CRYSTAL S T R U C T U R E S AND SOLID STATE REACTIONS OF MALEIC ANHYDRIDE AND O F A C Y C L O H E X E N O N E AND ITS P H O T O P R O D U C T By Christine Hwang B.Sc. (Honours), University of British Columbia, 1986 A THES I S S U B M I T T E D IN P A R T I A L F U L F I L L M E N T O F T H E R E Q U I R E M E N T S F O R T H E D E G R E E O F M A S T E R O F S C I E N C E in T H E F A C U L T Y O F G R A D U A T E S T U D I E S D E P A R T M E N T O F C H E M I S T R Y We accept this thesis as conforming to the required standard T H E U N I V E R S I T Y O F BRITISH C O L U M B I A September 1988 © Christine Hwang, 1988 In present ing this thesis i n pa r t i a l fu l f i lment of the requirements for an advanced degree at the Un ive r s i t y of B r i t i s h C o l u m b i a , I agree tha t the L i b r a r y sha l l make it freely avai lable for reference and study. I further agree that permiss ion for extensive copy ing of this thesis for scholarly purposes may be granted by the head of m y depar tment or by his or her representatives. It is unders tood that copy ing or pub l i c a t i on of this thesis for f i nanc i a l ga in shal l not be a l lowed w i thou t m y wr i t ten permiss ion. Depa r tment of Chemi s t r y T h e Un ive r s i t y of B r i t i s h C o l u m b i a 2075 Wesbrook P lace Vancouver , C a n a d a V 6 T 1 W 5 Date: Abstract Two sets of structures were determined by X-ray crystallographic techniques, one of maleic anhydride (2,5-furandione) and the other of 4-phenyl-4-p-bromophenylcyclohex-2-en-l-one and its photoproduct, r.rans-5-phenyl-6-p-bromophenylbicyclo[3.1.0]hexan-2-one. Analysis of maleic anhydride included a room temperature redetermination of the crystal structure. This was done to improve parameters and simplify comparison of the room temperature and low temperature data. The structure determination at 104A resulted in the location of bonding electrons in the double bond. Thermal motions of both sets of data showed that translational motion was greatest along an axis parallel to the carbonyl bonds. Libration was found to be greatest about this axis also. The second set of structures was done to examine the migration pattern of aryl groups upon irradiation of a diarylcyclohexenone. The major photoproduct was formed by migration of the p-bromophenyl group. The resulting bicyclohexanone had the aryl groups trans to each other. n Table of Contents Abstract ii Acknowledgments xii I A Crystallographic Analysis of Maleic Anhydride xiii 1 Introduction 1 2 General Experimental Methods 4 2.1 Choosing a Crystal 4 2.2 F inding the Orientation Mat r ix and Cel l Type 5 2.3 Determining the Space Group 5 2.4 Collecting Data 5 2.5 Correcting Data For Absorption 6 2.6 Processing Data 7 2.7 Determining the Structure 7 2.8 Refining the Structure 8 3 Experimental Details of Maleic Anhydride 9 i i i 3.1 Room Temperature Study 9 3.2 Low Temperature Study 10 3.3 Brominat ion 13 4 Theory 18 4.1 Low Temperature X-ray Diffraction 18 4.2 Librat ion Corrections 19 5 Results and Discussion 22 5.1 Room Temperature Study 22 5.2 Absolute Configuration Analyses 29 5.3 Low Temperature Study 30 5.4 Finding Bonding Electrons 33 5.5 Mean Plane Calculations 35 5.6 Rig id Body Calculations 35 5.7 Librat ion Corrections 35 II The Structure Determination of 4-phenyl-4-p-bromophenylcyclohex-2-en-l-one and rra?i5-5-phenyl-6-p-bromophenylbicyclo[3.1.0]hexan-2-one 39 6 Introduction 40 7 Experimental Details of the Cyclohexenone and its Photoproduct 43 iv 7.1 Cyclohexenone Analysis 43 7.2 Photoproduct Analysis 46 8 Results and Discussion 47 8.1 Structure Determination of the Cyclohexenone 47 8.2 Structure Determination of the Photoproduct 58 8.3 Chemical Implications 59 Bibliography 66 Appendices 68 A Torsion Angles 68 B Structure Factors for Maleic Anhydride at 2 9 5 A ' 77 C Structure Factors for Maleic Anhydride at. 104/\' 83 D Structure Factors for the Cyclohexenone 88 E Structure Factors for the Photoproduct 107 v List of Tables 3.1 Crystallographic data from maleic anhydride at 295K 10 3.2 Data collection conditions for maleic anhydride at 295K 10 3.3 Crystallographic. data from maleic anhydride at 104A' 11 3.4 Data collection conditions for maleic anhydride at 104A' 11 3.5 Elemental analysis results of bromination product 17 5.6 Averaged bond distances and angles from recent and former structure determinations and from electron diffraction 24 5.7 Final positional and isotropic thermal parameters with estimated standard deviations in parentheses for maleic anhydride at room temperature . . . 25 5.8 Final anisotropic thermal parameters for maleic anhydride at room tem-perature and their estimated standard deviations 25 5.9 Final positional and isotropic thermal parameters with estimated standard deviations in parentheses for maleic anhydride at low temperature . . . . 26 5.10 Final anisotropic thermal parameters for maleic anhydride at low temper-ature and their estimated standard deviations 26 v i 5.11 Bond lengths for maleic anhydride at room temperature with estimated standard deviations in parentheses 27 5.12 Bond lengths for maleic anhydride at low temperature with estimated standard deviations in parentheses 27 5.13 Bond angles (°) for maleic anhydride at room temperature with estimated standard deviations in parentheses 27 5.14 Bond angles (°) for maleic anhydride at low temperature with estimated standard deviations in parentheses 28 5.15 Bijvoet calculated and observed values for enantiomorph shown 31 5.16 Bijvoet calculated and observed values for enantiomorph not shown . . . 32 5.17 Principal axes of translation and libration 36 5.18 Principal values of translational and librational tensors 38 7.19 Crystallographic data from the cyclohexenone 44 7.20 Data collection conditions for the cyclohexenone 44 7.21 Crystallographic data from the photoproduct 45 7.22 Data collection conditions for product 45 8.23 Final positional and isotropic thermal parameters for cyclohexenone . . . 51 8.24 Final anisotropic thermal parameters for cyclohexenone 52 8.25 Bond lengths for cyclohexenone with estimated standard deviations in parentheses 53 vii 8.26 B o n d angles (°) for cyc lohexenone 53 8.27 F i n a l po s i t i ona l and i sot rop ic t h e r m a l parameters for cyc lohexenone w i t h spl i t a toms 54 8.28 F i n a l an i so t rop ic t he rma l parameters for the cyc lohexenone w i t h sp l i t atoms 55 8.29 B o n d lengths for cyc lohexenone w i t h spl i t atoms w i t h e s t imated s t anda rd dev ia t ions i n parentheses 56 8.30 B o n d angles (°) for cyc lohexenone w i t h spl it atoms 57 8.31 Per t inent to r s i on angles for analys is 61 . 8.32 F i n a l po s i t i ona l and i sotrop ic t h e r m a l parameters for the p r o d u c t . . . . 62 8.33 F i n a l an i so t rop ic t he rma l parameters for the pho top roduc t 63 8.34 B o n d lengths for the pho top roduc t w i t h e s t imated s tandard dev ia t ions in parentheses 64 8.35 B o n d angles for the pho top roduc t (°) w i t h es t imated s t anda rd dev ia t ions i n parentheses 65 A.36 Tors ion angles (°) w i t h e s t imated s tanda rd dev iat ions in parentheses for male ic anhyd r i de at r oom tempe ra tu re 69 A.37 Tor s ion angles (°) w i t h e s t imated s tanda rd dev iat ions in parentheses for male ic anhyd r i de at low tempera tu re 70 A.38 Tors ion angles (°) w i t h e s t imated s t anda rd dev iat ions in parentheses for the cyc lohexenone 71 viii A.39 Torsion angles (°) with estimated standard deviations in parentheses for the cyclohexenone with split atoms 73 A.40 Torsion angles (°) with estimated standard deviations in parentheses for the photoproduct 75 i x List of Figures 1.1 R e a c t i o n of c o m p o u n d 1 to f o r m compound 2 1 1.2 S t r u c tu re of male ic anhyd r i de 2 3.3 L o w tempera tu re set-up 12 3.4 T h e set-up for b r om ina t i on of maleic. anhyd r i de 14 3.5 T h e n.m.r. s pec t r um of b r om ina t i on p roduc t 15 3.6 T h e i.r. s pec t rum of b r om ina t i on product 16 4.7 D i a g r a m related to the theory of l i b r a t i ona l mot ions 20 5.8 Stereo d i a g r am of male ic anhyd r i de 28 5.9 Stereo pack i ng d i a g r am of ma le i c anhyd r i de 29 5.10 E l e c t r o n dens ity contour m a p f r o m difference Four ier . 34 5.11 M o l e c u l a r axes for reference to Tab le 5.17 36 6.12 R e a c t i o n of d i s ub s t i t u ted cy lohexenones 41 6.13 A r y l - pheny l - d i s ub s t i t u t ed cyc lohexenone react ion 41 6.14 P r o p o s e d mechan i sm of react ion 42 8.15 Stereo d i a g r am of the cyc lohexenone w i t h d isorder 48 x 8.16 Stereo diagram of cyclohexenone with split atoms 49 8.17 Stereo packing diagram of the cyclohexenone 50 8.18 Stereo diagram of a molecule of the photoproduct 59 8.19 Packing diagram of the photoproduct 60 x i Acknowledgments W i t h the help and suppor t of many, I have been able to reach th i s stage in my educat ion. To these people I wou l d l ike to show m y apprec ia t i on . F i r s t , I t h ank m y parents and my b ro the r for the i r constant suppo r t and love through-out the years. I app rec i a ted the f reedom and gentle gu idance they gave me. T h e y have taught me much . I am grate fu l to the teachers th roughout m y school years who have had a posit ive inf luence in my life. T h e y have shown me the way to the fa sc i na t i ng wor ld of Chemis t ry . I g reat ly apprec ia ted the help and suppor t of those w i t h w h o m I have been work ing: M i g u e l G a r c i a - G a r i b a y , Steve R e t t i g , F red W i r e k o , V i v i e n Yee, S tephen Evans , Phan i R a j P o k k u l u r i , and Sara A r i e l . 1 have benef i ted f r om the i r counsel and f r iendsh ip. - F i n a l l y , but ce r ta i n l y not the least, I wou ld l ike to thank Professor James Trotter for hav i ng me as his student. Few students are as p r i v i l eged as I am to have such an at tent i ve and knowledgeab le superv i sor to gu ide t hem th rough the i r research project. x n Part I A Crystallographic Analysis of Maleic Anhydride xni Chapter 1 Introduction Solid state reactions have been of great interest since Schmidt's work on topochemistry in 1964[l]. Experimental work showed that a single enantiomer can be produced when a chiral product is formed from an achiral reactant. This can occur if the achiral starting material crystallizes in a chiral space group, i.e. one with no mirror, glide planes, or centres of inversion. This type of reaction was given the term "absolute asymmetric synthesis". Recently at this university, several people have been experimenting with asymmetric synthesis with success using both photolysis [2, 3] and bromination [4]. In one case, compound I (Fig. 1.1) was photolyzed to produce the chiral compound 2. Compound 1 Figure 1.1: Reaction of compound 1 to form compound 2 1 Chapter 1. Introduction 2 0 H C c o H 0 F i gu r e 1.2: S t r u c tu re of male ic anhydr ide showed the i m p o r t a n c e of the ch i ra l i t y of the space group [3]. T h e diester was f ound to c ry s ta l l i ze in two forms, Pbca and P2\2\2\. The former group conta ins gl ide planes and therefore, is not a ch i ra l space group. T h e latter is ch i ra l s ince it contains on ly screw axes. A l t h o u g h i r r ad i a t i on of bo th crysta l s gave the same p r o d u c t , 2, on ly the p r oduc t f r o m the P2{2i2\ c rysta l s showed op t i c a l act iv i ty . T h i s showed the impo r t ance of the reactant c r y s t a l l i z i n g in a ch i r a l space group. T h e present interest in the c r y s ta l s t ruc tu re of male ic anhyd r i de (F i g . 1.2), also k n o w n as 2,5-furandione, developed w i t h the discovery that i t was an ach i r a l c o m p o u n d c r y s ta l -l i z i ng in a ch i r a l space group. T h i s phenomenon was found d u r i n g the c ry s ta l s t ruc tu re de te rm ina t i on done by R.E. M a r s h , E . U b e l l , and H.E. Wi lcox[5 ] . T h e molecu le of male ic a n h y d r i d e has no ch i ra l a toms but crysta l l i zes i n the ch i ra l space group P 2 ] 2 i 2 i . W o r k was p roposed to p roduce a ch i r a l p roduc t f r o m chemica l react ion of crystals of maleic. an -hyd r i de . To o b t a i n more deta i l ed s t r u c t u r a l i n f o rmat i on , the c r y s t a l s t ructure of ma le i c Chapter 1. Introduction 3 anhydride was redetermined, with a low temperature study to determine the location of bonding electrons. Room- and low-temperature sets were combined to give informa-tion regarding librational and translational motions. Bromination of maleic anhydride followed by the structure determination of the reaction product was planned; however, difficulties arose and this part of the study was not continued further. Chapter 2 General Exper imenta l Methods C r y s t a l l o g r aph i c methods have been wel l deve loped i n recent years such tha t most crys-ta l lographers fo l low a s im i la r procedure. A general i n t r oduc t i on to X - r a y c ry s ta l l og raph ic techniques may be f ound in many texts. A select ion of these has been l i s ted as pa r t of the b i b l i o g r aph i ca l d a t a [6, 7, 8]. T h e fo l l ow ing pages descr ibe a general e xpe r imen ta l p rocedure used in a l l studies i nc l uded i n this thesis. Dev ia t ions f r om th i s p rocedure and deta i l s of each case may be found in the e xpe r imen ta l detai ls section cor respond ing to that p a r t i c u l a r study. 2.1 Choosing a C ry s ta l C a r e was taken in choos ing a su i tab le c r y s ta l for d i f f ract ion . T h e d imens ions of most crysta l s used were between 0.1 m m and 0.3 m m such that the c ry s ta l s were not larger t h a n the beam. La r ge r crystals were cut to the proper d imens ions. Imperfect ions i n crysta l s such as t w i n n i n g and sate l l i te a t tachment s were usua l ly detected us ing e i ther a set of po la r i zed lenses or precession photographs. 4 Chapter 2. General Experimental Methods 5 2.2 Finding the Orientation Matrix and Cell Type T h e c r y s t a l was moun ted on a fibre in a r a n d o m pos i t i on . U s i n g an En ra f -Non iu s C A D 4 d i f f rac tometer , ref lect ions were found us ing S E A R C H , a p r o g r a m designed to search s y s temat i ca l l y t h r ough the rec ip roca l space for up to 25 ref lect ions. These were then cent red by us ing S E T A N G , a p r o g r am used to locate peak centres by scann ing the peak w i t h var ious speeds and apertures. T h e ref lect ions are used to ob ta i n a p r im i t i ve un i t cel l and its o r i en ta t i on m a t r i x . H i gher s y m m e t r y l a t t i ce types may be found upon the app l i c a t i on of cell r educ t i on programs. 2.3 Determining the Space Group T h e space group of a g iven c ry s ta l was de te rmined by check ing absence condit ions. In-d i v i d u a l ref lect ions were scanned to dete rmine whethe r or not they were present. These were checked against, the cond i t ions for different space groups. T h i s m e t h o d at t imes m a y give more t han one poss ib le space group. 2.4 Collecting Data D a t a were co l lected us ing a z ig-zag m o d e in the un ique r ec i p roca l space (except for male ic anhyd r i de at r o o m tempera tu re where more than un ique d a t a were col lected). I nd i ca ted absences were not co l lected. T h r e e ref lect ions f r o m those used to determine the o r i en ta t i on m a t r i x were chosen such t h a t they were s t rong, we l l -determined reflections Chapter 2. General Experimental Methods 6 with their scattering vectors approximately normal to each other. These were used as intensity and orientation checks. Intensity checks were used to measure the amount of decay, if any. The orientations checks determined shifts in the position of the crystal. If the shift in any one of the three reflections was greater than a specified amount, the crystal would be re-oriented. At the end of data collection, the amount of decay was measured by analyzing the intensity checks. If decay was found to be significant, the data would be corrected during data processing. A better set of cell parameters was obtained after data collection using higher angle data. A new set of 25 reflections was obtained by choosing relatively strong reflections at relatively high angles. These new reflections were repeatedly centred. Their positions were improved further using D E T T H , which scans the reflection at positive and negative 6 values to ensure that there were no zeroing errors in 0. New, and hopefully better, cell parameters were obtained. 2.5 Correcting Data For Absorption To correct data for absorption, the absorption coefficient, the dimensions of the crystal, and the indices of faces of the crystal are needed. The former is calculated using C M P L X , which utilizes the cell volume, approximate density, and composition. Absorption cor-rection is done either during data processing or by using BICABS at any time after processing. Often it is done after structure determination so that one can see whether or Chapter 2. General Experimental Methods not cor rect ion d i d improve the da ta . De lay ing correct ion is also useful if the cel l contents were not known at the t ime of d a t a processing.t 2.6 Processing Data A l o ca l l y developed p rog ram, ENPROC [ 9 ] , was used for process ing da ta . T h i s p r og r am wr i tes a d a t a fi le w i t h correct ions as specif ied. For ma le i c anhydr ide , L p ( Lo ren t z and po l a r i z a t i on ) , decay and absorpt ion correct ions were made. In the others, on ly L p cor-rect ions were made us ing the d a t a process ing p rogram. 2.7 Determining the Structure T h e s t ructures presented in th is thesis were solved w i t h one of two methods . W i t h male ic anhydr ide , the s t ruc tu re w-as dete rmined us ing direct methods . Mos t of the non-hydrogen atoms i n male ic anhydr ide were located us ing this m e t h o d . A difference Fou r i e r l ocated the rest of the atoms in the s t ructure. T h e other two structures were solved us ing a heavy a t o m (Pat te r son ) m e t h o d . B y Pa t t e r s on , the b rom ine a t o m was easi ly l ocated. A least-squares refinement, of the one a t o m fo l lowed by a difference Four ie r l ocated the other non-hydrogen atoms. T h i s pro-cedure was repeated but w i t h a l l non-hydrogen atoms i n the refinement process. A l l hydrogen atoms were found in th i s manner. tAU programs used up to this point have been made available by Enraf-Nonius as part of the structure determination package for the CAD4 diffractometer. Minor changes may have been made to the programs to fit the needs and preferences of this particular group of crystallographers. Chapter 2. General Experimental Methods 8 2.8 R e f i n i n g t h e S t r u c t u r e Refinement of structures was done using B U C I L S , a least-squares fitting program, unti l the shifts in atomic positions and thermal parameters were negligible. Difference Fourier maps were done after refinement to ensure that there are no large peaks unaccounted for. . Note: A l l torsion angles and structure factors are presented in the appendix. Chapter 3 Experimental Details of Maleic Anhydride Maleic anhydride samples used in both the room temperature and the low temperature data collections were crystals formed by sublimation during a period of approximately two years. The compound itself was supplied by Kodak. Because of their volatility, the crystals were mounted in 0.5 mm glass capillary tubes distributed by the Charles Supper Company. 3.1 Room Temperature Study Normally, only the unique data set is collected, but since the room temperature analysis wras a redetermination of the structure, data were collected of more than the unique set. In order to improve results and determine the absolute configuration, four octants were collected instead of just one. The four were those with indices ±h,±k, —I. Four reflections were searched for and quickly found. These were used to determine the cell. The cell was then transformed to the same one appearing in Marsh's paper[5]. Additional reflections were chosen from the paper and added to the four. All reflections were then centred several times before obtaining a final set of cell parameters before data 9 Chapter 3. Experimental Details of Maleic Anhydride 10 Tab le 3.1: C r y s t a l l o g r aph i c d a t a f r om male ic an L a t t i c e O r t h o r h o m b i c Space g roup a b P 2 1 2 1 2 1 7.1751 (7) A 11.2165 (10) A c 5.3792 (5) A V 432.91 (7) A 3 D x Z 1.505 g/ml 4 molecules hyd r i de at 295A ' Tab l e 3.2: D a t a co l lec t ion cond i t i on s for male ic anhyd r i de at 295A* Reg ion co l lected ± h , ± k , - l 0 range 0< 0 < 75.0° to scan angle 0.65 + O.14tan0° Ho r i z on t a l ape r tu re w i d t h 2.00 + l.OOtanfl m m Ve r t i c a l ape r tu re w i d t h 4 m m R a d i a t i o n used C u A=1.54A Absence cond i t i ons hOO: h o d d OkO: k o d d 001: 1 o d d Frequency of in tens i ty checks every 3600 s Frequency of o r i en ta t i on checks every 150 ref lect ions co l lect ion (Tab le 3.1). C o n d i t i o n s used d u r i n g da ta co l lect ion may be found i n Tab le 3.2. 3.2 Low Temperature Study T h e e xpe r imen ta l methods for the low tempera tu re d a t a co l lect ion were s im i l a r to the r o o m t empe ra tu r e co l lect ion except tha t on ly one un ique d a t a set,-|-/i4-fc-fI, was col lected, Chapter 3. Experimental Details of Maleic Anhydride 11 Table 3.3: Crystallographic data from maleic anhydride at 104A" Lattice Orthorhombic Space group a P212121 7.0206 (17) A b 10.9957 (66) A c V 5.3209 (26) A 410.76 A 3 Z 4 molecules Table 3.4: Data collection conditions for maleic anhydride at 104K Region collected h,k,l id scan angle 0.65 + 0.35tan(?° Horizontal aperture width 2.00 + l.OOtantf mm Vertical aperture width 4 mm Scan speed range 1.44 to 10.06 Radiation used Mo A=0.71073A Absence conditions hOO: h odd OkO: k odd 001: 1 odd Frequency of intensity checks every 3600 s Frequency of orientation checks every 100 reflections Chapter 3. Experimental Details of Maleic Anhydride 12 Figure 3.3: Low temperature set-up and the crystal was cooled with an Enraf-Nonius Universal Low Temperature Device placed by the diffractometer (Fig. 3.3)[10]. A controlled cold N ; gas stream was directed at the crystal. A warmed nitrogen gas stream surrounded the cold gas to help minimize icing. Also to reduce icing, a plastic sheet, jar of Drier i te™, and litre of liquid nitrogen were used. The plastic, sheet was used to cover the diffractometer. Although there were still openings around the instrumentation for tubes, wires and access, the plastic sheet minimized air turbulences near the gas stream. It also helped in creating a positive pressure in the "box" along with the litre of liquid N 2 in the Dewar placed by the diffractometer and the steady stream of gas from the low temperature device. The positive pressure inhibited moist air in the room from reaching the crystal. Although the Drierite seems to be a primitive idea, its presence did seem to help keep the humidity lower. A dehumidifier may have been better if it were available. Chapter 3. Experimental Details of Maleic Anhydride 13 To measure the t empera tu re , a coppe r -Con s tan tan t he rmocoup le was inserted into the cold s t ream t u b e w i t h its end at the end of the t u b e about 6 m m away f r o m the c ry s ta l . A vo l tage read ing was recorded about every 15 minutes . These readings were ca l i b ra ted at a later t i m e by c o m p a r i n g values w i t h those presented i n the C R C H a n d b o o k of C h e m i s t r y and Phys i c s C a l i b r a t i o n Tab le for The rmocoup le s [ l l ] to give the a c t u a l tempera tu re . T h e 25 ref lect ions used to determine the ce l l were co l lected wh i l e coo l ing . T h e y were centred after at least one ha l f hour of coo l ing had elapsed. O r i e n t a t i o n checks occur red after every 100 ref lect ions and intens i ty was checked every 3600 seconds. Snow and poss ib ly C 0 2 snow were removed app rox ima te l y every 15 minutes. T h e d a t a were co l lected in shells: first w i t h 0 < $ < 27.5°, then 27.5 < 9 < 32.5°, and finally 32.5 < 6 < 37.5°. Other cond i t ions for d a t a co l lect ion are l i s ted in Tab le 3.4. Ice bu i l d -up caused in tens i ty to be lower and u l t i m a t e l y the loss of the c ry s ta l after co l l ec t ing 464 ref lect ions. To finish d a t a co l l ec t ion , another c r y s ta l was used. A second scale factor was added in the appropr i a te places for ref inement. 3.3 Bromination T h e procedure used for b r om ina t i on of ma le i c anhyd r i de is descr ibed below. T h i s proce-dure w i t h some m i n o r var ia t ions was a t t e m p t e d several t imes w i t h no success. Be fore the b r o m i n a t i o n react ion , a l l s t a r t i ng mater ia l s were pu r i f i ed : the male ic an-hyd r i de by s ub l ima t i on and the b rom ine by d i s t i l l a t i on . T h e reagents a long w i t h some d r y i n g agent were set up as shown i n F i g . 3.4. I n i t i a l e xpe r imen ta t i on was done us ing Chapter 3. Experimental Details of Maleic Anhydride 14 Maleic Anhydride • B r 2 i It F i gu re 3.4: T h e set-up for b r om ina t i on of maleic. anhyd r i de powdered ma le i c anhydr ide . It was hoped that after d i scover ing the o p t i m a l cond i t ions tha t the react ion can occu r under s imi la r cond i t i ons w i t h a single c r y s ta l . Sa tu ra ted b r o m i n e vapour in the conta iner wou ld react w i t h the maleic. anhydr ide. T h e react ion was f ound to requi re about four weeks of react ion t i m e for a reasonable amount of p roduc t to be f o rmed . P r o b l e m s d i d arise. A t f i r s t , the unreacted m a t e r i a l and p roduc t s were found to f o r m an o i l d u r i n g the course of the react ion. U p o n charac te r i z ing the p roduct us ing so lut ion n.m.r. spect ra , i.r. d a t a , a n d e lementa l analys is (F igures 3.5 and 3.6, and Tab le 3.5), the r i n g was found to have opened to f o r m d,/-2,3-dibromosuccinic ac id , not the trans anhydr ide . T h e r ing open i ng was a t t r i b u t e d to the long length of t i m e requi red for the reac t i on to take place. W a t e r may have entered t he react ion vessel du r i n g tha t t ime. S ince each expe r iment requ i red four to five weeks, i t was dec ided tha t th is par t of the s tudy shou ld not be pur sued fu r ther at th is t ime. •1 fl) co H f t 3 m n p: 3 c r n O g . P> • o p HI o n S A M P L E L D VARIAN XL-300 STANDARD IH OBSERVE EXP2 PULSE SEQUENCE: DATE 13-10-87 SOLVENT CDCL3 r u e H I D M A - B R ACQUISITION TN SW AT NP PW PI DI D2 TO NT CT PN*0 SS IL IN DP HS I. 7S0 4000. 0 i. 128 23024 35.0 0 0 0 300 256 109 49. 0 DEC. DN 0) DM DLP STD1H A VT 1.750 330. 3 NNN 10 PROCESSING SE 3. 103 LB 0.100 FN 85536 MATH F DISPLAY 0 SP -130.0 N w? 2999.4 r VS 240 Y SC 100 NN wc 400 IS 78 RFL 349.1 RFP 0 TH 20 INS 1.00" DC I I I I I 9 8 CO 8. 3 3 CD tn O oT fc) a . T T T -b I i " i i | i 7 i I i i i i | i i i i | i i | i i i i 5 i i | i i 4 T T T I | I I I I | I 3 T - r T T -2 ' I ' ' i i | 1 i i | l l i | ' ' i l | 0 P P M Cn Chapter 3. Experimental Details of Maleic Anhydride 16 Figure 3.6: The i.r. spectrum of bromination product Chapter 3. Experimental Details of Maleic Anhydride 17 Table 3.5: Elemental analysis results of bromination product Element C H 0 B r Found (% by wt.) 17.53 1.46 — Expected for anhydride 18.63 0.78 18 .61 61.97 Error 1.10 0.68 — — % Error 6.3% 46.6% - — Expected for acid 17.41 1.46 23.20 57.93 Error 0.12 ~o — — % Error 0.7% ~ 0 % — — Chapter 4 Theory 4.1 Low Temperature X-ray Diffraction T h e m o t i o n of e lectrons is s t rong ly re lated to the the rma l pa rameter s and thus the " q u a l i t y " of the s t r uc tu re de te rm ina t i on . B y lower ing the t e m p e r a t u r e and thus s lowing down the v i b ra t i on s , one can obta in bet te r a tom ic pos i t ions wh i ch in t u r n gives better ca l cu la ted b o n d lengths and to a lesser extent , angles. T h e t h e r m a l mot ion s of atoms are reduced; thus, the peak intens i ty to backg round rat io is improved at a lower temperature. T h e lower tempera tu re s not on ly improve d a t a but also a l low for the co l lec t ion of higher angle da ta . A l t h o u g h lower temperatu res shou ld theore t i ca l l y improve a l l d a t a there are several concerns to deal w i t h when set t ing up equ ipment and co l lect ing d a t a so that on ly when one benefits g reat ly does one venture to co l lect a set of low tempe ra tu r e data . W h e n set t ing up low tempe ra tu r e apparatus one shou ld cons ider the po s i t i on so that i t "will not l i m i t the angles t h a t can be co l lected. T h e equipment shou ld also not d i s tu rb the inc ident or d i f f racted beams. B y us ing a gas s t ream th i s p r o b l e m can be m in im i zed . La rge r concerns d i d arise du r i n g d a t a co l l ec t ion . One must ensure that the alignment. 18 Chapter 4. Theory 19 of c r y s t a l does no t change u p o n coo l ing a n d tha t the adhesive used to at tach the c r y s ta l to the arcs is effective even upon coo l ing. T h e adhesive must not shr ink more t han the c ry s ta l . O t h e r deta i l s encountered du r i ng low tempera tu re studies i nvo lved ob ta in i ng an ac-cura te measurement of tempera tu re . A c oppe r -Con s t an tan the rmocoup le inserted i n to the gas s t ream d i spens ing t ube w i t h its t i p at the end of the t ube near the crys ta l is one of the bet te r so lut ions to th i s p r ob l em as it m in im i ze s large changes i n tempera tu re i n the t he rmocoup le . One of the o the r p rob lems to overcome was tha t of frost f o rmat i on . W i t h a large bu i l d - up of ice o r snow, the reflections may be masked. M i n i m i z i n g frost f o rmat i on was carefu l ly cons idered in the set-up. Ideal ly, the equipment shou ld be in an air-t ight refr igerated r o o m or conta iner w i t h cont ro l led humid i t y . However, this is expensive and also l i m i t i n g in t e m p e r a t u r e range ava i lab le. A closed r o o m or conta iner was not avai lable for use so the d a t a were col lected in an open area w i t h several o ther precaut ions taken in s tead. These p recaut ions are descr ibed i n the exper imenta l deta i l s section. 4.2 Libration Corrections M o l e c u l a r mo t i on s can be d i v i ded into two types: t r an s l a t i ona l , wh ich descr ibe mot ions i n a s t ra ight p a t h , and l i b r a t i ona l , wh i ch refer to mot ions a long an arc. L i b ra t i on s often cause e xpe r imen ta l bond distances to be shorter t h a n the ac tua l lengths [12, 13, 14]. T h i s is because the c i rcu la r pa th of the a t o m is inadequate ly descr ibed by an e l l ipso id Chapter 4. Theory 20 / D' Figure 4.7: Diagram related to the theory of librational motions (Fig. 4.7). If OA is the true bond distance between atoms A and O, and A moves along an arc D D ' , then the atomic position of A would be experimentally determined as B. To correct for this, one must add the length of AB to the experimental bond length, OB to give the true value. Although not always done, libration corrections can be calculated and applied to a set of bond lengths without too much problem. Given the thermal parameters that describe the molecular motions, one can easily calculate the librational corrections which are then added to the bond distances. To calculate a libration correction, the molecule, or at least, portions of it, must be nearly rigid. Angles are seldom affected by librations and thus, are not corrected. Lower temperatures cause less motion within the molecule and, because of this, should give truer experimental bond lengths without libration corrections. Since the bonds should not have been appreciably shortened at the lower temperature, one can Chapter 4. Theory compare the corrected values from the two sets of dat Chapter 5 Results and Discussion 5.1 Room Temperature Study A total of 1951 pieces of data was collected over the four octants, ± / i , ±fc, — / . During data processing, absorption corrections were applied with the assumption that the crystal was spherical. Equivalent reflections were merged (i.e. hkl with hkl) by taking the average of the two equivalent reflections. Ordinarily, all the octants in P2i2i'2i are treated as equivalent. However, in order to find the absolute configuration, the minute differences due to anomalous dispersion were not ignored. For this set of data, 'hkl and hkl were treated as equivalent to each other but not to hkl and hkl. Thus, the hkl data were merged with the corresponding hkl data. This was repeated for hkl and hkl. (See later for absolute configuration analysis.) The number of unique reflections measured was 977 with 753 of them observed (I> 3<T(I)). All of the merged data were involved in a direct methods calculation us-ing MULTAN80[16]. All non-hydrogen atoms were located from the resulting E-map. y" Refinement of these atoms isotropically at first, followed by anisotropic refinement gave 22 Chapter 5. Results and Discussion 23 R = 0.061 and Rw — 0.078. Locations of the two hydrogen atoms were determined by us-ing a difference Fourier map. Adding the hydrogens and refining all atoms dropped R to 0.034 and Rw to 0.043, the final values. The largest difference peak after all least-squares refinement was 0.214 eA-3; the lowest trough was —0.185 eA-3. To show that the merged data did improve the structure, half of the merged data, which is equivalent to one octant, was used to refine the newly obtained atomic positions and thermal parameters. Refinement using the smaller set of data gave a poorer least-squares fit as shown by the R values: R = 0.035 and Rw — 0.046. This shows that the collection of more than unique data did indeed improve data but the improvement was not large enough to be feasible to do the same in future structure analyses. Both sets showed better least-squares fits than those of the earlier study done by Marsh. The R value obtained then was 0.055. The new results did agree with those obtained by Marsh, et al. Upon comparison, the C-C bond lengths differ by, at the most, 0.012A. The bonds were generally shorter than those reported from an electron diffraction study [15]. All bond lengths were reasonably close to theoretical values. Carbonyl bonds were found to be 1.200A. Single bonds be-tween carbon and oxygen atoms were longer at 1.396A. The carbon-carbon single bonds were 1.476A whereas the double bond was considerably shorter at 1.317A. All angles within the ring were between 107.8 and 108.5°. External angles involving O — C — O were 120.7° while C — C — O angles were 131.4°. The newer bond distances and angles are listed in Tables 5.11 and 5.13. The averaged values along with the older ones and those Chapter 5. Results and Discussion 24 Tab le 5.6: Ave r aged b o n d distances and angles f r o m recent and fo rmer s t ructure deter-m ina t i on s and f r o m e lectron d i f f ract ion A . B o n d D i s tances ( A ) b o n d Unco r rec ted Co r r e c ted M a r s h E l e c t r o n Diff. Cl - Ol 1.379(3) 1.396 1.388 1.394 Cl - C2 1.457(4) 1.476 1.469 1.500 C2 - C3 1.302(3) 1.317 1.303 1.330 Cl - 02 1.192(3) 1.200 1.189 1.195 C2-E2 0.97(4) — 1.08 1.091 B. B o n d Ang les (°) C2-C1- Ol 107.8(2) — 107.7 108.8 C2-C1- 02 131.4(2) — 131.6 129.3 Ol - Cl - 02 120.7(2) — 120.7 121.9 C1-C2- C3 108.5(2) — 108.5 107.7 f r o m electron d i f f r ac t i on are l i s ted in Tab le 5.6. B o n d lengths were corrected for l i b r a t i on (see la ter ) . These corrected values are also found in Tab le 5.11. A t o m i c pos it ions and t h e r m a l parameter s cor respond ing to th i s s t ruc tu re analys is are f ound in Tables 5.1 and 5.8. A s i n the prev ious stud) ', the new s tudy d i d also show that the ca rbony l oxygen atoms were s l i ght ly ou t of p lane of the f ive-membered r ing . T h e d i s tance f rom the plane was found to be 0.007A i n the new study. T h i s is smal ler t h a n Ma r sh ' s va lue of 0.029 A . T h e hydrogen atoms were found to be out of t he p lane also by 0.04 to 0.05A. There are no prev ious da ta g iven about the hydrogen pos i t ions w i t h respect to the p lane of the r ing. T h e cel l f ound was comparab le w i t h that f r om the ear l ier s tudy (Tab le 3.1). A stereo d i a g r a m of t he molecu le and a p a c k i n g d i a g r am is shown i n F i g . 5.8 and F i g . 5.9 respect ively. 0 Chapter 5. Results and Discussion 25 Table 5.7: Final positional and isotropic thermal parameters with estimated standard deviations in parentheses for maleic anhydride at room temperature (fractional x lO 4 , H x l O 3 and U x l Q 3 A 2 ) Atom X y z C l 8174( 3) 7968( 2) 6606( 5) 67 C2 9342( 3) 8331( 2) 8678( 5) 70 . C3 10136( 3) 9338( 2) 8106( 5) 71 C4 9517( 3) 9690( 2) 5626( 5) 69 01 8294( 2) 8840( 1) 4789( 3) 71 02 7224( 3) 7110( 2) 6316( 4) 103 03 9891( 3) 10535( 2) 4365( 5) 102 H2 938( 5) 785( 3) 1009( 8) 109(10) H3 1099( 5) 987( 2) 912( 7) 94( 9) Table 5.8: Final anisotropic, thermal parameters for maleic anhydride at room tempera-ture and their estimated standard deviations (Uij x 10 3A 2)t fThe anisotropic therma Atom U22 ^33 U12 t/l3 u23 C l 61( 1) 74( 1) 65( 1) -3( 1) -2( 1) -9( 1) C2 73( 1) 77( 1) 60( 1) 5( 1) -7( 1) -2( 1) C3 60( 1) 78( 1) 75( 1) -1( 1) -12( 1) -17( 1) CA 60( 1) 68( 1) 78( 1) 5( 1) 3( 1) 0( 1) OI 63( 1) 90( 1) 60( 1) 3( 1) -10( 1) -3( 1) 02 105( 1) 98( 1) 105( 2) -35( 1) -7( 1) -15( 1) 03 108( 1) 85( 1) H4( 1) -4( 1) 8( 1) 23( 1) parameters employed in the refinement are U,.. in the expression: / = f°exp(—27r2H'£U,.jh,hja, * a.j*) Chapter 5. Results and Discussion 26 Table 5.9: Final positional and isotropic thermal parameters with estimated standard deviations in parentheses for maleic anhydride at low temperature (fractional x lO 4 , H x l O 3 and U x l 0 3 A 2 ) Atom X y z C l 8169( 9) 7959( 7) 6619(15) 19 C2 9377( 9) 8327( 7) 8691(18) 21 C3 10166( 8) 9417( 6) 8078(17) 21 C4 9504( 9) 9741( 7) 5555(20) 20 01 8267( 7) 8820( 6) 4719(13) 22 02 7256(10) 7032( 7) 6378(21) 30 03 9>346( 9) 10570( 7) 4216(17) 31 H2 954 790 1007 10 H3 1102 987 900 29 Table 5.10: Final anisotropic thermal parameters for maleic anhydride at low temperature and their estimated standard deviations (UV x 10 3A 2)t Atom U22 ^33 U12 UH U23 C l 20( 3) 24( 4) 13( 3) 1( 2) -2( 2) -4( 3) C2 22( 3) 21( 3) 20( 4) 5( 2) -8( 2) -5( 3) C3 18( 3) 20( 3) 24( 4) 0( 2) -4( 2) -4( 3) C4 16( 3) 23( 3) 21( 4) 4( 2) 1( 3) 2( 3) O l 17( 2) 37( 3) 13( 3) 0( 2) -2(2) 4( 2) 02 28( 3) 34( 3) 28( 4) -9( 2) 1( 3) -8( 4) 03 30( 3) 34( 4) 29( 4) K 2) 1( 2) 12( 3) fThe anisotropic thermal parameters employed in the refinement are Uij in the expression: / = /°exp(-27r 2SS^,jfe 1-fe ja,- * a,-*) Chapter 5. Results and Discussion 27 Table 5.11: Bond lengths for maleic. anhydride at room temperature with estimated standard deviations in parentheses B o n d Uncorr. (A) Corr . (A) Bond (A) Uncorr. (A) C o r r . (A) C1-C2 1.453(3) 1.472 C l - O l 1.386(3) 1.402 01 - 02 1.189(2) 1.197 0 2 - C 3 1.302(3) 1.317 C2 - H2 0.93(4) C3 - 04 1.461(4) 1.480 04 - 01 1.372(3) 1.389 04 - 03 1.196(3) 1.203 0 3 - 7 / 3 1.01(4) Table 5.12: Bond lengths for maleic anhydride at low temperature with estimated stan-dard deviations in parentheses Bond (A) Uncorr. (A) Corr . (A) Bond (A) Uncorr. (A) Corr . (A) 01 - C2 1.449(10) 1.455 C l - O l 1.387(10) 1.393 01 - 02 1.211(11) 1.215 02 - C3 1.360(11) 1.364 C2-H2 0.880(9) C 3 - C 4 1.464(14) 1.471 C4 - O l 1.406(9) 1.411 04 - 03 1.182(12) 1.183 C3 - 773 0.920(6) Table 5.13: Bond angles (°) for maleic anhydride at room temperature with estimated standard deviations in parentheses Bonds Angle (°) Bonds Angle (°) C2 - 01 - O l 107.9(2) 03 - 04 - 01 107.8(2) 02 - 01 - 02 131.2(3) C3 - 04 - 03 131.6(2) O l - 01 - 02 120.9(2) 01 - C4 - 03 120.6(2) C l - 02 - C3 108.4(2) C l - O l - C4 107.4(2) 02 - C3 - 04 108.5(2) C l - 02 - H2 119(2) 02 - 03 - HZ 130(2) 03 - 02 - H2 133(2) 04 - 03 - H3 121(2) Chapter 5. Results and Discussion 28 Table 5.14: Bond angles (°) for maleic. anhydride at low temperature with estimated standard deviations in parentheses Bonds Angle (°) Bonds Angle (°) C2 - C l - 0 1 109.6(7) C 3 - C 4 - OI 108.2(7) C2 - C l - 0 2 128.7(9) C 3 - C 4 - 0 3 132.5(8) OI - C l - 0 2 121.6(8) 0 1 - 0 4 - 0 3 119.3(10) C l - C 2 - C 3 107.6(8) C l - 0 1 - 0 4 106.9(7) C 2 - C 3 - C 4 107.7(7) C l - C 2 - H2 124.0(8) C 2 - C 3 - H3 127.8(9) C 3 - C 2 - H2 128.4(8) C 4 - C 3 - H3 124.3(8) Figure 5.8: Stereo diagram of maleic anhydride Chapter 5. Results and Discussion 29 Figure 5.9: Stereo packing diagram of maleic anhydride An attempt to locate bonding electrons using high angle room temperature data proved unsuccessful. There were not enough high angle data to refine the structure. 5.2 Absolute Configuration Analyses Two independent analyses were performed on the data to determine the absolute config-uration of this particular crystal structure. First, an independent refinement of the first set of atomic coordinates gave the value, /?! =0.033920. For the enantiomorphic structure, R2 =0.034397. The ratio between the two, R = ^ = 1.0141. Application of Hamilton's test[l7] showed that this R value is significant to the 99.5% confidence level. This shows that the crystal structure was most likely the one presented in the packing diagram (Fig. 5.9). Chapter 5. Results and Discussion 30 T h e second test compares the signs between Bc. and Bc where: o _ I0{hM)-I0(hki)_  0 0.S\Io(hkl) + Io(hkl)) D _ ic(hu)-ic{hki)_ c 0.5[Ic(hkl)+Ic(hkl)] Fo r the f irst set of da ta , 24 out of the 31 w i t h \R\ >1 were of the same sign (Tab le 5.2). T h e result for the second set was on ly 7 out of 31 (Tab le 5.16). Th i s conf i rms the results of the prev ious test. 5.3 Low Temperature Study T h e s t ruc tu re of male ic anhydr ide at 104 K was solved by ref in ing the a tom ic pos i t ions f r o m the r o o m tempera tu re s t ructure us ing the low tempera tu re data. T h e st ructure ref ined we l l , g i v i n g final R = 0.050 and Ru, = 0.063. In order to use low tempera tu re d a t a to find bond i n g electrons and compare results w i t h those f r o m room tempera tu re , one must ensure that a phase t rans i t i on d i d not occur between 104 and 295A '. T h e d i f f ract ion pa t te rn i nd i ca ted that the c ry s ta l at 104A ' was i n t he same phase as at 295A ' . T h e pa t te rn d i d not change upon coo l ing. Th i s was apparent du r i n g center ing of the reflections wh i ch was done concur rent l y w i t h cool ing. T h e ref lect ions d i d not have large shifts du r i ng this t ime. T h e cel l obta ined after coo l ing h a d s im i l a r d imens ions , bu t the cell d i d shr ink u p o n cool ing (Tables 3.1 and 3.3). T h e axes were a l l shorter t h a n those at r o o m tempera tu re . Chapter 5. Results and Discussion Table 5.15: Bijvoet. calculated and observed values for enantiomorph shown h k 1 B 0 B c Agreement 2 9 -4 0.38981 0.03426 v 7 1 5 - 5 -0.11172 0.03023 2 11 -2 0.13577 0.02785 V 2 7 - 5 0.11259 0.02683 V 2 7 -2 -0.00192 0.02600 2 2 - 5 -0.18435 0.02229 2 10 -3 0.20609 0.02031 v 7 2 10 -2 0.07626 0.01996 V 1 1 -6 -0.02844 0.01971 2 8 -1 0.07728 0.01832 v 7 1 9 -2 -0.03617 0.01566 1 10 -1 0.06551 0.01336 v 7 1 1 -4 -0.09163 0.01327 2 8 -3 0.04939 0.01317 V 1 8 -2 0.02378 0.01284 v 7 1 2 -4 -0.05933 0.01047 2 8 -4 0.00886 0.01043 v 7 1 8 - 5 0.24752 0.01022 V 1 9 -1 -0.01499 -0.01090 3 1 -3 -0.02072 -0.01261 V 2 7 -4 -0.09486 -0.01459 V 2 3 -2 -0.15218 -0.01464 V 1 3 -4 -0.06823 -0.01510 V 2 8 -2 -0.02099 -0.01626 2 4 -1 -0.09527 -0.01681 V 1 2 - 5 -0.11903 -0.01840 V 2 6 -4 -0.22946 -0.01858 V 2 10 -1 -0.21144 -0.01873 v 7 3 2 -3 -0.27527 -0.02040 v 7 2 1 -4 -0.05632 -0.02175 v 7 3 • 1 -2 -0.05278 -0.02530 v 7 Chapter 5. Results and Discussion Table 5.16: Bijvoet calculated and observed values h k 1 B 0 B c Agreement 3 1 -2 -0.05232 0.02529 2 1 -4 -0.05608 0.02174 3 2 -3 -0.27511 0.02043 2 10 -1 -0.21142 0.01871 2 6 -4 -0.22945 0.01854 1 2 -5 -0.11885 0.01839 2 4 -1 -0.09407 0.01678 2 8 -2 -0.02083 0.01629 1 3 -4 -0.06778 0.01510 2 3 -2 -0.15101 0.01465 2 7 -4 -0.09474 0.01459 3 1 -3 -0.02063 0.01260 1 9 -1 -0.01492 0.01088 1 8 -5 0.24749 -0.01018 2 8 -4 0.00881 -0.01044 1 2 -4 -0.05941 -0.01049 1 8 -2 0.02369 -0.01290 2 8 -3 0.04930 -0.01315 1 1 -4 -0.09173 -0.01328 V 1 10 -1 0.06547 -0.01341 1 9 -2 -0.03626 -0.01565 V 2 8 -1 0.07715 -0.01830 1 1 -6 -0.02846 -0.01968 2 10 _o 0.07620 -0.02005 2 10 -3 0.20605 -0.02036 2 2 -5 -0.18438 -0.02226 2 7 -2 -0.00208 -0.02597 2 7 -5 0.11259 -0.02689 2 11 _2 0.13575 -0.02792 1 . 5 -5 -0.11176 -0.03026 2 9 -4 0.38980. -0.03430 or enantiomorph not shown Chapter 5. Results and Discussion 33 Another indication that no phase change occurred was the least-squares fit. Refine-ment of room temperature atomic positions and other parameters gave reasonably low R values. If there were a phase transition, the atomic positions would most likely have changed by a large amount such that refinement of room temperature atomic positions would have given a poor least-squares fit. Comparison of bonds and angles between the room temperature and low tempera-ture structures showed that the values agreed with each other within experimental error (Tables 5.11, 5.12, 5.13, and 5.14). The atomic positions and thermal parameters for the low temperature analysis are presented in Tables 5.1 and 5.10. 5 .4 F i n d i n g Bonding Electrons Bonding electrons were found using the low temperature data. Reflections with 20< 0 < 32° were separated from the main set of data to be used for high angle refinement. Least-squares refinement of the atomic positions and thermal parameters of all non-hydrogen atoms gave the values, R = 0.066 and Rw = 0.06S. After refining the structure using high angle data and calculating a difference map with all data, electron density was found near the bonds. This was most apparent in the double bond. An electron density contour map is presented in Fig. 5.10 with the molecule sketched in. Chapter 5. Results and Discussion Figure 5.10: Electron density contour map from difference Fourier Chapter 5. Results and Discussion 35 5.5 Mean Plane Calculations A mean plane calculation showed that maleic anhydride is essentially planar. Its plane equation is: 0.77a: - 0.50y - 0.40z = 0.85 The carbonyl oxygen atoms are slightly displaced from the plane by 0.007A. The dis-placement of the ring oxygen was quite large. It was found to be 0.027A from the plane. The plane equation along with calculated bond vectors were utilized in direction cosine calculations to determine the magnitude of different types of motions in the molecule. 5.6 Rigid Body Calculations Calculations were done to analyze the rigidity of the molecule. A comparison of the ( T ( U ; J ) , 0.0010 A2, and 6(11^), 0.0020 A2, values showed that the maleic anhydride molecule is a reasonably good rigid body. With such rigidity in the molecule, trans-lational and librational motions can be analyzed and libration corrections applied. 5.7 Libration Corrections Among the principal molecular translation axes (Tz, T2,T3), the greatest translation is found to be nearly in the direction of axis 2 in both the room- and low-temperature cases, being only 4° from the molecular axis. For libration, the principal axis is 19° from axis 2 (Fig. 5.11). Chapter 5. Results and Discussion 36 axis 2 0 O Figure 5.11: Molecular axes for reference to Table 5.17 Table 5.17: Principal axes of translation and libration Principal Axes of Translation normalized vector angle to axis 1 axis 2 axis 3 -0.3503 -0.9020 0.2524 76° 176° 88° T2 -0.1668 0.3254 0.9307 132 91 42 -0.9217 0.2840 -0.2643 138 94 132 Principal Axes of Libration normalized vector angle to axis 1 axis 2 axis 3 -0.6864 -0.6796 0.2588 107 161 97 U>2 0.1512 0.4820 0.8630 135 82 46 U>3 -0.7114 0.5535 -0.4330 131 73 135 Chapter 5. Results and Discussion 37 In b o t h the room- and low- tempera tu re cases, the t rans la t ions are near ly i sot rop ic for the other two direct ions. For instance, at 295A ' , the r.m.s. amp l i t udes were 0.27, 0.23, and 0.21 A a long the T i , T 2 , and T3 axes, respect ive ly (Tab le 5.18). T h e values were on ly 0.19, 0.14, and 0.13 A for the 104A^ data . A t h i gh angle, the d a t a were s imi lar : 0.18, 0.15, and 0.14 A . T h e t r an s l a t i on for the r o o m tempera tu re s tudy was about 1.5 t imes the magn i tude of the low tempera tu re study. T h i s was expected since at lower temperatures the atoms, and thus the molecule, move less. A s the Tab le 5.18 shows, the r.m.s. a m p l i t u d e a long the T i axis was 0.27/1 at 295A ' . T h e corresponding va lue at low tempera tu re was only 0 . 1 9 A T h e l i b r a t i on tensor i nd i ca ted tha t most of the l i b r a t i o n was present about axis 2 and is essent ia l ly i so t rop ic in the other d i rect ions pe rpend i cu la r to i t . T h e r.m.s. amp l i tudes for l i b r a t i o n at 295/\ were 7.9, 6.4, and 5.8° a long the three axes (Tab le 5.18). A s w i t h those for t r an s l a t i on , a d rop in r.m.s. amp l i tudes was found for the lower temperature . A t 104A ' , the values were on ly 5.7, 3.5, and 3.3°. B o n d lengths were corrected for l i b r a t i on accordingly. C o m p a r i n g the two sets of da ta after l i b r a t i on correct ions showed tha t the bond lengths d i d agree w i t h each other. Co r rec t i on s were m i n i m a l for bonds in the r ing but re la t i ve ly large for c a rbony l bonds (Tab le 5.11). T h e correct ions w i t h the r o o m tempera tu re s t ructure were m u c h larger t h a n those made w i t h the low tempera tu re s t ructure because of the increase in molecu la r m o t i o n at higher temperatures . T h e low tempera tu re correct ions were - to \ of t h ose at Chapter 5. Results and Discussion iable 5.18: Pr incipal values of translational and librational tensors T - R . M . S . Amplitudes (A) direction Room Temp. Low Temp. Low Temp. High Angle T i 0.271 0.188 0.182 T2 0.228 0.143 0.150 T3 0.211 0.131 0.140 UJ- R . M . S . Amplitudes (°) ^ i 7.89 5.65 4.99 6.42 3.55 3.49 U)3 5.79 3.27 2.71 room temperature. Part II The Structure Determination of 4-phenyl-4-p-bromophenylcyclohex-2-en-l-one and frc?z5-5-phenyl-6-p-bromophenylbicyclo[3.1.0]hexan-2-one 39 Chapter 6 Introduct ion Photochemical studies of cyclohexenones were started in 1964 as a natural evolution of studies of conjugated cyclohexadienones [IS]. Since then, several experiments regard-ing group migrations in the disubstituted cyclohexenones have been done [19]. Earlier papers showed that in solution, the disubstituted compounds formed the correspond-ing bicyclo[3.1.0]hexanone upon radiation (Fig. 6.12). This led to the question regard-ing which group migrates during the reaction. In an earlier study, H.E. Zimmerman, R.D. Rieke, and J.R. Scheffer, analyzed the different migration patterns in several com-pounds containing phenyl and para-substituted phenyl groups [20]. Although product ratios differed, the p-cyanopheny] and p-methoxyphenyl compounds had a similar reac-tion pattern (Fig. 6.13). For reactions that took place in solution, the ratios between the para-substituted phenyl(zlr) migration product and phenyl(PZi) migration product were found to be 14±2 .5 to 1 for the p-cyanophenyl compound, and 12 .5±2 .5 to 1 for the p-methoxyphenyl compound. A possible mechanism was proposed (Fig. 6.14). Recently, Jianxin Chen and John R. Scheffer have been studying these compounds in the solid state. First, the ratio for the cyano complex in solution was remeasured under 40 Chapter 6. Introduction 41 Figure 6.12: Reaction of disubstituted cylohexenones Major Product Minor Product Figure 6.13: Aryl-phenyl-disubstituted cyclohexenone reaction Chapter 6. Introduction 42 Figure 6.14: Proposed mechanism of reaction different conditions from before. The reaction was repeated in the same manner for a crystal. The ratio for the solution was similar to the published value but the ratio for the solid state reaction was only 2 to 1. For the p-bromo substituted aromatic group, the migration ratios' were 2:1 and 1.3:1 for the solution and solid state reactions respectively. Assuming that it was significant, they proposed to rationalize the difference between the solution and solid state. An X-ray crystal structure was done to supply more information about these compounds. With the newly obtained chemical and structural information, it was believed that the correct mechanism may be identified. Chapter 7 Experimental Details of the Cyclohexenone and its Photoproduct 7.1 Cyclohexenone Analysis Crystals of the cyclohexenone made by Jianxin Chen were submitted for crystal structure analysis. A colourless crystal was mounted onto a glass fibre. The crystals shattered easily upon cutting. For this reason, a larger-than-normal crystal was chosen. Twenty reflections were located with 6 between 10 and 15°. The space group was determined to be P1\fc. Data were collected for ±/i,-f-fc,-M with 0< 9 <27.5° . Intensity checks were done every hour and orientation checks were done after every 150 reflections. Other conditions for data collection may be found in Table 7.20. Out of 3361 reflections measured, 1807 (53.8%) were considered observed. Final parameters and pertinent data are listed in Tables 7.19 and 7.20. 43 Chapter 7. Experimental Details of the Cyclohexenone and its Photoproduct 44 Table 7.19: Crystallographic. data from the cyclohexenone Lattice Monoclinic Space group P2 1 /c a 16.1567 (15) A b 9.1886 (28) A c 9.9959 (30) A 13 95.80 (2)° V 1476.4 (7)A 3 DT 1.472 g/ml D m 1.46 g/ml Z 4 molecules Table 7.20: Data collection conditions for the cyclohexenone Region collected ±h,k, l 0 range 0< 9 < 27.50° <jj scan angle 0.65 + O.35tan0° Horizontal aperture width 2.00 + l.OOtantf mm Vertical aperture width 4 mm Scan speed range 1.06 to 20.12 Radiation used Mo A=0.71073A Absence conditions OkO: k odd hOl: 1 odd No. reflections measured 3361 No. reflections observed 1807 (53.8%) Frequency of intensity checks every 3600 s Frequency of orientation checks every 150 reflections Chapter 7. Experimental Details of the Cyclohexenone and its Photoproduct 45 Table 7.21: Crystallographic. data from the photoproduct Lattice Monoclinic Space group I2/a a 17.6073 (39) A b 8.2133 (20) A c 19.9763 (50) A 13 93.09 (3)° V 2884.6 (12) A 3 L \ 1.5068 g/ml Z 8 molecules Table 7.22: Data collection conditions for product Region collected ±h,k, l 0 range 0< 0 < 27.50° ui scan angle 0.65 + O.35tan0° Horizontal aperture width 2.00 + l.OOtanfl mm Vertical aperture width 4 mm Scan speed range 1.06 to 20.12 Radiation used Mo A = 0.71073A Absence conditions hkl: h+k+1 odd hOl: h and 1 odd No. reflections measured 3290 No. reflections observed 1651 (50.2%) with \/<T(I) >3.00 Frequency of intensity checks every 3600 s Frequency of orientation checks every 150 reflections Chapter 7. Experimental Details of the Cyclohexenone and its Photoproduct 46 7.2 Photoproduct Analysis A colourless crystal of the photoproduct synthesized by Jianxin Chen with dimensions 0.20 mmx0.12 mmx0.57 mm was mounted on a glass fibre. The unit cell and orien-tation matrix was determined using 20 reflections collected with 6 between 10 and 15°. The space group was determined to be 72/a. Data collection conditions are listed in Table 7.22. A total of 3290 reflections was collected, out of which 1651 (50.2%) were considered observed. The cell parameters and other results are in Table 7.21. Chapter 8 Results and Discussion 8.1 Structure Determination of the Cyclohexenone The structure analysis of the cyclohexenone began with the location of the bromine atom using a Patterson function. Three cycles of least-squares refinement with only the bromine atom gave an R factor of 0.489 and a weighted R factor of 0.526. The other non-hydrogen atoms were easily located with a difference Fourier. Anisotropic refinement reduced the R value to 0.066 and Rw to 0.094 without the hydrogens. All hydrogen atoms were located in the difference map although it was apparent that there was some possible disorder in the non-aromatic ring. Least-squares refinement of all atoms until they were settled gave R — 0.048 and Ru, = 0.060. The mean and maximum shifts for the last refinement cycle were 0.010 and 0.110 a respectively. The large shifts were found only in the hydrogens believed to be disordered. The largest shift in the other atoms was only 0.05 for the disordered carbons and 0.02 for the rest of the structure, which are quite acceptable shifts. The residua] electron density from a difference Fourier was between -0.238 and 0.763 eA~ 3 . 47 Chapter 8. Results and Discussion 48 Figure 8.15: Stereo diagram of the cyclohexenone with disorder Absorption correction was attempted at this point but it did not improve the least-squares fit. This may have been due to the irregular shape of the crystal chosen for the study. Not all of the faces could be properly assigned and measured. AU thermal parameters, bond distances, and angles were reasonable at this point of the analysis (Tables 8.23, 8.24, 8.25 and 8.26). However, there was some disorder found near the C = C double bond. The distance between C2 and C3 was 1.339 A, indicating that it does have 7r character in the bond. The distance between 05 and C6 was 1.455 A which is slightly shorter that expected for a single bond. An ORTEP diagram (a thermal ellipsoid plot) and a meanplane calculation both gave some indication of the extent of the disorder. The thermal ellipsoids representing 02 and 06 were elongated in the direction normal to the plane (Fig. 8.15), indicating that not only the 05 — 06 bond but also the 02 — 03 bond may have some single bond character. Chapter S. Results and Discussion 49 Figure 8.16: Stereo diagram of cyclohexenone with split atoms Efforts were made to split the atomic positions using chemical reasoning such that, the bond distances, angles, and thermal parameters may agree with expected values. Atoms C l , C 2 , and C6 were split to account for the disorder. A 75% to 25% splitting gave acceptable thermal parameters and chemically sensible bond distances and angles. The new data are found in Tables 8.27, 8.28, 8.29 and 8.30. The corresponding stereo diagram is in Fig. 8.16. This diagram displays the structure with all split atoms and hydrogens not corresponding to these carbons isotropically refined. The hydrogens attached to dis-ordered carbons had fixed parameters. All other atoms were anisotropically refined. The dotted lines in the stereo diagram indicate the secondary positions where the disordered atoms are located in approximately 25% of the time. The hydrogens that should appear 25% of the time were located but did not refine well. They were omitted in the final refinement. A packing diagram is presented in Fig. 8.17 to show the relative positions of Chapter S. Results and Discussion 50 Figure 8.17: Stereo packing diagram of the cyclohexenone the molecules in the cell. The final R values after splitting the atoms were R =0.051 and Rw =0.064. The mean and maximum shifts were 0.014 and 0.191a respectively. Large shifts were found only in some of the disordered atoms. The difference Fourier showed that the largest peak unaccounted for was 0.775eA~3; the lowest trough was -0.571eA~3. Chapter 8. Results and Discussion Table 8.23: Final positional and isotropic thermal parameters for cycloh (fractional x lO 4 , H x l O 3 and Uxl0 3 A 2 ) Atom X y z u e g/u, s o Br -193 -7588( 1) 1748( 1) 76 0 4797( 2) -7232( 4) 757( 6) 97 C l 770( 2) -6461( 4) 1528( 4) 47 C2 1295( 3) -6058( 5) 2638( 4) 55 C3 2005( 3) -5284( 5) 2459( 4) 51 C4 2206( 2) -4900( 4) 1186( 4) 36 C5 1652( 3) -5287( 5) 90( 4) 48 C6 934( 2) -6066( 5) 266( 4) 49 C7 2987( 2) -4015( 4) 997( 4) 40 C8 3333( 3) -4402( 5) -333( 5) 50 C9 3730( 4) -5819( 7) -374( 7) 84 CIO 4290( 3) -6254( 5) 809( 6) 67 C l l 4188( 4) -5461( 8) 2028( 8) 103 C12 3672( 3) -4339( 5) 2122( 5) 52 C13 2810( 2) -2362( 4) 1010( 4) 39 C14 2029( 3) -1789( 5) 1137( 4) 48 C15 1899( 3) -288( 5) 1183( 5) 59 C16 2549( 3) 647( 6) 1095( 5) 61 C17 3329( 4) 106( 5) 958( 5) 64 C18 3459( 3) -1389( 5) 914( 5) 54 H2 117( 2) -631( 5) 348( 5) 58(13) H3 238( 3) -482( 6) 331( 6) 94(17) H5 177( 3) -509( 5) -85( 5) 70(14) H6 63( 2) -643( 4) -47( 4) 42(11) H8a 296( 3). -418( 5) -122( 5) 66(14) H8b 374( 4) -379( 7) -62( 7) 116(21) H9a 399( 3) -601( 5) -106( 5) 56(13) H9b 324( 5) -713( 9) -46( 8) 171(29) H l l 454( 4) -571( 7) 271( 6) 101(20) H12 359( 2) -396( 4) 295( 5) 53(13) H14 . 160( 3) -244( 4) 121( 4) 49(12) H15 135( 3) 9( 4) 147( 4) 48(11) H16 251( 2) 165( 5) 113( 4) 39(10) H17 379( 2) 66( 4) 98( 4) 43(11) HIS 393( 3) -180( 5) 78( 4) 47(12) Chapter S. Results and Discussion 52 Table 8.24: Final anisotropic thermal parameters for cyclohexenone (Uij x 10 3A2)t Atom Un u22 ^33 f/23 Br 49 87 91 -22 1 20 0 54( 2) 59( 2) 180( 5) 18( 2) 24( 2) 12( 2) C l 38( 2) 41( 2) 60( 3) -2( 2) 1( 2) 8( 2) C2 60( 3) 71( 3) 35( 2) -17( 2) 3( 2) 10( 2) C3 58( 3) 60( 3) 35( 3) -15( 2) -2( 2) 2( 2) C4 41( 2) 31( 2) 35( 2) 2( 2) 0( 2) -2( 2) C5 50( 2) 64( 3) 30( 2) -2( 2) 5( 2) 3( 2) C6 44( 2) 55( 3) 46( 3) -3( 2) -4( 2) -13( 2) C7 40( 2) 41( 2) 40( 2) -1( 2) 6( 2) 4( 2) C8 49( 2) 49( 3) 56( 3) -6( 2) 16( 2) -3( 2) C9 102( 5) 80( 4) 77( 4) 40( 4) 41( 4) 7( 3) CIO 39( 2) 47( 3) 115( 4) -5( 2) 13( 3) 9( 3) C l l 81( 4) 124( 6) 94( 5) 42( 4) -35( 4) -11( 4) C12 47( 2) 55( 3) 54( 3) -2( 2) -2( 2) 10( 2) C13 46( 2) 41( 2) 30( 2) -2( 2) 2( 2) 2( 2) C14 50( 2) 40( 2) 54( 3) 4( 2) 10( 2) 3( 2) C15 70( 3) 50( 3) 58( 3) 12( 2) 8( 3) 3( 2) C16 87( 4) 39( 3) 54( 3) 7( 3) 2( 2) -4( 2) C17 74( 4) 48( 3) 70( 3) -20( 3) 4( 3) 3( 2) C18 49( 3) 46( 3) 68( 3) -4( 2) 10( 2) -3( 2) tThe anisotropic thermal parameters employed in the refinement are Uij in the expression: / = / ° e x p ( - 2 7 r 2 S E t / u / i I / j . ; , a 1 * a,-*) Chapter S. Results and Discussion 53 Table 8.25: Bond lengths for cyclohexenone with estimated standard deviations in paren-theses B o n d L e n g t h (A) B o n d L e n g t h (A) Br -- CIO 1.901(4) C7 • - C12 1.525(6) 0 - C l 1.220(5) C8 - C9 1.453(7) Cl - C2 1.377(6) C9 -- CIO 1.471(8) Cl - C6 1.364(6) CIO - C l l 1.444(8) C2 - C3 1.378(6) C l l - C12 1.335(7) C3 - CA 1.391(5) C13 - C14 1.385(6) CA - Cb 1.390(5) C13 - C18 1.388(6) CA - C7 1.528(5) C14 - C15 1.397(6) CA -- C13 1.544(5) C15 - C16 1.367(7) Cb - C6 1.389(6) C16 - C17 1.375(7) Cl - C8 1.535(6) C17 - C18 1.391(7) Table 8.26: Bond angles (°) for cyclohexenone B o n d s A n g l e (°) B o n d s A n g l e (°) 0 - C l - Cl 122.6(3) C7 - C8 - C9 115.6(4) 0 - C l - C6 122.1(2) C8 - C9 - C10 117.3(6) C2 - C l - C6 120.8(4) Br - C10 -- C9 119.8(3) C l - C2 - C3 119.1(4) Br -- C10 - C l l 119.3(3) C2 - C3 - C4 121.7(4) C9 -- C10 - C l l 115.3(5) C3 - C4 - C5 117.7(4) C10 - C l l -- C12 125.1(6) C3 - C4 - C7 121.4(3) C7 -- C12 - C l l 120.7(5) C3 - C4 - C13 115.0(3) C4 -- C13 - C14 89.0(3) C5 - C4 - C7 120.9(3) C4 -- C13 - CIS 153.3(3) C5 - C4 - C13 113.7(3) C14 - C13 -- CIS 117.6(4) C7 - CA - C13 111.6(2) C13 - C14 -- C15 121.3(4) C4 -Cb- C6 120.8(4) C14 - C15 -- C16 120.0(5) C l -C6- C5 119.8(4) C15 - C16 -• C17 119.8(5) C4 -Cl - C8 111.2(3) C16 - C17 -- C18 120.2(5) C4 -Cl - C12 110.6(3) C13 - C18 -- C17 121.1(5) C8 -Cl - C12 107.0(3) Chapter S. Results and Discussion 54 Table 8.27: Final positional and isotropic thermal parameters for cyclohexenone with split atoms (fractional x lO 4 , H x l O 3 and U x l 0 3 A 2 ) A t o m x y z ue9/u„0 Br -192 -7588( 1) 1748( 1) 76 0 4800( 3) -7234( 4) 767( 6) 99 Cl 4272( 5) -6260(10) 666(10) 81 cr 4309 -6247 962 10 C2 4239( 6) -5388(10) 1949(10) 71 C2' 4011(16) -5939(29) 2258(31) 77 CZ 3670( 3) -4339( 5) 2120( 6) 51 CA 2986( 2) -4011( 5) 995( 4) 40 Cb 3336( 3) —4401( 5) -333( 5) 50 C6 3684( 5) -5895( 9) -435( 8) 59 C& 3965(14) -5509(23) -169(22) 49 Cl 2206( 3) -4896( 4) 1187( 4) 36 CS 2006( 3) -5283( 5) 2459( 5) 52 C9 1292( 3) -6062( 6) 2632( 5) • 55 CIO 772( 2) -6465( 5) 1533( 5) 47 cn 932( 3) -6068( 5) 265( 5) 49 C12 1656( 3) -5286( 5) 88( 5) 47 C13 2810( 3) -2365( 4) 1010( 4) 40 cu 2027( 3) -1788( 5) 1136( 4) 48 C15 1898( 3) -289( 5) 1187( 5) 59 C16 2548( 4) 646( 6) 1097( 5) 61 C17 3327( 4) 105( 6) 951 ( 6) 66 CIS 3461( 3) -1390( 5) 918( 5) 53 H2 436( 5) -545( 8) 280( 8) 123(27) HZ 360( 2) -392( 4) 293( 4) 41(12) Hba 299( 3) -427( 5) -114( 5) 72(16) Hbb 380( 4) -362( 8) -67( 7) 84(21) H6a 406( 3) -594( 6) -112( 5) 75(15) H6b 326( 4) -683( 9) -39( 6) 77(20) HS 236( 3) -488( 6) 321( 6) 87(18) H9 118( 3) -627( 5) 342( 5) 62(15) HU 59( 2) -649( 4) -48( 4) 38(11) H12 181( 3) -510( 6) -79( 6) 90(18) HU 156( 3) -244( 4) 116( 5) 55(14) Hlb 133( 2) 10( 4) 150( 4) 39(10) H16 249( 2) 172( 6) 117( 4) 47(11) Hll 375( 2) 67( 4) 99( 4) 27(10) HIS 397( 3) -181( 5) 83( 4) 46(12) Chapter 8. Results and Discussion 55 Table 8.28: Final anisotropic thermal parameters for the cyclohexenone with split atoms (Uij x 10 3A 2)t Atom U22 #33 17,2 UH U23 Br 49 87( 1) 91( 1) - 2 2 1 20 0 56( 2) 58( 3) 185( 5) 18( 2) 24( 3) 16( 3) C3 47( 3) 53( 3) 53( 3) - 2 ( 2) - 2 ( 2) 8( 3) C4 39( 2) 40( 2) 41( 2) - 1 ( 2) 4( 2) 2( 2) C 5 50( 3) 47( 3) 55( 3) - 4 ( 2) 14( 2) - 3 ( 2) C 7 42( 2) 31( 2) 36( 2) 2( 2) 2( 2) - 1 ( 2) CS 60.( 3) 61( 3) 33( 3) -19( 2) - 3 ( 2) 2( 2) C9 58( 3) 71( 3) 36( 3) -15( 3) 2( 2) 12( 2) CIO 38( 2) 43( 3) 60( 3) - 3 ( 2) 3( 2) 8( 2) c n 45( 2) 54( 3) 48( 3) - 3 ( 2) - 4 ( 2) -11( 2) C12 46( 2) 64( 3) 31( 3) - 1 ( 2 ) 3( 2) 4( 2) C13 46( 2) 42( 2) 31 ( 2) - 2 ( 2) 3( 2) 1( 2) C14 51( 3) 42( 3) 52 ( 3) 3( 2) 9( 2) 4( 2) C15 69( 3) 47( 3) 59( 3) 13( 3) 6( 3) 3( 2) C16 87( 4) 4K 3) 53( 3) 9( 3) - 2 ( 3) - 4 ( 2) C17 76( 4) 47( 3) 75( 4) -20( 3) 6( 3) 3( 3) C I S 49( 3) 46( 3) 64( 3) - 5 ( 2) 10( 2) - 4 ( 2) fThe anisotropic thermal parameters employed in the refinement are 17,^  in the expression: / = / ° e x p ( - 2 7 r 2 S S ^ u / i I ^ , a 1 * a_,*) Chapter 8. Results and Discussion 56 Table 8.29: Bond lengths for cyclohexenone with split atoms with estimated standard deviations in parentheses B o n d Length (A) B o n d Length (A) Br -- CIO 1.898(4) Cb - C6' 1.44(2) 0 - Cl 1.233(9) Cl - C8 1.389(6) O -- Cl' 1.233(4) Cl -- C12 1.389(6) Cl - C2 1.517(12) c s - C9 1.384(6) Cl - C'6 1.420(13) C9 - CIO 1.366(6) c r - Cl' 1.45(3) CIO - C l l 1.369(6) Cl' - C6' 1.39(2) Cll - C12 1.399(6) C2 - C3 1.354(9) C13 - C14 1.388(6) C2' - C'3 1.57(3) 013 - CIS 1.393(6) C3 - CA 1.525(6) C14 - C15 1.394(7) CA - Cb 1.536(6) C'15 - C16 1.367(7) CA - Cl 1.528(5) C'16 - C17 1.374(7) CA -- C13 1.540(5) cn - CIS 1.391(7) Cb - C6 1.491(9) Chapter 8. Results and Discussion bl Table 8.30: Bond angles (°) for cyclohexenone with split atoms B o n d s A n g l e (°) B o n d s A n g l e (°) Cl - 06 - 05 113.1(7) 09 - O10 - O i l 120.9(4) 0 - 01 - 02 113.4(9) OI' - 06' - 05 131(2) 0 - 01 - 06 129.6(9) 04 - 07 - 08 121.5(4) C2 - 01 - 06 116.9(8) 04 - 07 - 012 120.5(4) 0 -- 01' - 02' 124.1(11) 08 - 07 - 012 117.9(4) 0 -- 01' - 06' 116.2(9) 07 - 08 - 09 121.4(4) C2' - Cl' -- 06' 119.4(13) 08 - 09 - 010 119.6(4) Cl - 02 - 03 124.4(8) Br - 010 - C9 120.1(3) Cl' - 02' -- 03 104(2) Br - 010 - O i l 119.0(3) C2 - 03 - 04 119.9(6) 010 - O i l - 012 119.6(4) C2' - 03 -- 04 118.1(11) 07 - 012 - O i l 120.6(4) 03 - 04 - 05 106.8(4) 04 - 013 - 014 123.2(4) 03 - 04 - 07 110.3(3) 04 - 013 - 018 119.3(4) 03 - 04 - 013 108.0(4) C14-C13-C18 117.5(4) Cb - 04 - 07 111.4(3) C13-C14-C15 121.5(5) Cb - 04 - 013 108.8(3) C14-C15-C16 119.9(5) Cl - (74 - 013 111.4(3) C15-C16-C17 119.8(5) CA - 05 - 06 116.6(5) C16-C17-C18 120.4(5) CA - 05 - 06' 112.6(9) C13-C18-C17 120.9(5) Chapter 8. Results and Discussion 58 8.2 Structure Determination of the Photoproduct The structure determination of the photoproduct began with the location of the bromine atom using Patterson methods. Refinement, of the one atom gave R = 0.447 and Rw = 0.496. All carbon and oxygen atoms were found in a difference Fourier following the refinement. Least-squares refinement of all these atoms followed by difference Fourier calculations located all remaining atoms. An anisotropic refinement of all non-hydrogen atoms and isotropic refinement of hydrogen atoms until the refinement settled yielded the values, R = 0.038 and Rw = 0.045. Absorption correction was applied but, as in the case of the starting material, it did not improve the structure. With the correction made to the data and least-squares re-finement until the parameters settled, the final R - 0.040 and Rw = 0.046 were obtained. Again, the poor results from absorption correction may have been due to the irregular shape of the crystal. The mean and maximum shifts in the last cycle of least-squares refinement were less than 0.001 and 0.003 a, respectively. No disorder was found in this case. Experimentally, the crystal contained only the trans compound, the expected predominant product[20]. All bond lengths and angles are'found in Tables 8.34 and 8.35 respectively. The final set of thermal parameters are listed in Tables 8.32 and 8.33. The five-membered ring is planar. Its plane forms a 107.9° angle to the three-membered ring. The bromophenyl ring is 57.1° from the larger ring and 51.5° from Chapter S. Results and Discussion 59 Figure 8.18: Stereo diagram of a molecule of the photoproduct the smaller ring such that steric interactions are relatively small in this pseudo-axial po-sition. The phenyl ring is in an pseudo-equatorial position trans to the other aromatic ring. The stereo diagram of the molecule is found in Fig. 8.18. Figure 8.19 is the packing diagram of the photoproduct. 8.3 Chemical Implications The planarity of parts of a molecule and the relative positions of the phenyl and bro-mophenyl groups are shown by torsion angles. These angles show that C?l, C2, C3, C4, and C'6 form a plane when the double bond is located between C2 and C3 (Table 8.31). Carbon 5 is displaced from the plane in this conformation. When the double bond is located between C'5 and C'6, C73 is the atom displaced from the plane of the other five ring atoms. Chapter 8. Results and Discussion 60 Figure 8.19: Packing diagram of the photoproduct The expected value for the torsion angles (C6 - Ch -CA- X and C2' -C3-CA- X) related to a pseudo-axial group is 60°; for the pseudo-equatorial group, the value is 180°. Experimental angles show that in both conformations, the Ar group occupies a pseudo-axial position (with C6 - Cb - CA - Cl and C2' - CZ - CA - Cl torsion angles of about 65°). The phenyl groups are in pseudo-equatorial positions (with C6 — Cb — CA-C13 and C2' — C3 — CA — C13 torsion angles of about 170°). The torsion angle in the photoproduct, C6 — Cb — CA — C13 = 151°, shows that the orientation of the Ph group is relatively unchanged. The Ar group migrated during the reaction but it is still in a pseudo-axial position in the product. The small changes in the orientation of the two groups between reactant. and product favours the formation of the major product, but does not explain the fact that the product ratio is only 1.3 : 1 in favour of the major product in the solid state reaction. Chapter S. Results and Discussion 61 Table 8.31: Pertinent torsion angles for analysis Cyclohexenone Photoproduct Bonds 75% • 25% C6 - Cb - CA - Cl -67 -C6 - Cb - CA - C13 170 - -151 C2' --C3-CA - Cl — 62 C2' - C3 - CA - C13 — -176 Chapter S. Results and Discussion 62 Table 8.32: Final positional and isotropic thermal parameters for the product (fractional x lO 4 , H x l O 3 and U x l 0 3 A 2 ) Atom X y z Br 3962 -785( 1) 662 60 0 177( 2) 2961( 4) 33( 2) 65 C l 661 ( 2) 3634( 5) 383( 2) 47 C2 628( 2) 3904( 5) 1116( 2) 46 C3 1332( 3) 3508( 5) 1566( 2) 46 C4 1220( 2) 5211( 5) 1316( 2) 39 C5 .1615( 3) 5657( 6) 681( 2) 43 C6 1357( 3) 4444( 6) 139( 2) 49 C7 1965( 2) 2429( 5) 1372( 2) 43 C8 2716( 3) 2842( 6) 1522( 2) 55 C9 3310( 3) 1903( 5) 1332( 2) 53 CIO 3156( 3) 482( 5) 983( 2) 47 C l l 2422( 3) -1( 6) 857( 3) 56 C12 1825( 3) 942( 5) 1041( 2) 55 C13 1065( 2) 6564( 5) 1788( 2) 41 014 1486( 3) 6746( 6) 2388( 2) 52 C15 1373( 3) 8073( 6) 2801( 2) 60 016 837( 3) 9205( 7) 2623( 2) 59 C17 402( 3) 9052( 6) 2030( 3) 57 CIS 521( 3) 7740( 6) 1611( 2) 51 H2 18( 2) 382( 4) 131( 2) 35(11) H3 120( 2) 339( 4) 203( 2) 28( 9) H5a 219( 3) 566( 5) . 77( 2) 51(12) H5b 145( 2) 665( 5) 55( 2) 40(11) H6a 175( 2) 369( 5) 9( 2) 36(11) H6b 127( 3) 489( 7) -32( 3) 89(17) HS 283( 2) 383( 5) 175( 2) 55(13) H9 380( 2) 222( 6) 140( 2) 61(14) H l l 236( 3) -80( 6) 66(3) 63(16) H12 129( 2) 66( 5) 94( 2) 44(11) H14 185( 2) 603( 5) 248( 2) 43(12) HIS 166( 3) 809( 6) 320( 3) 71(15) H16 72( 2) 1018( 6) 283( 2) 51(13) H17 6( 3) 980( 7) 189( 3) 75(17) H18 24( 2) 761( 5) 121( 2) 42(11) Chapter S. Results and Discussion 63 Table 8.33: Final anisotropic thermal parameters for the photoproduct (Uij x 103A2)t Atom U u C72  ^33 U 1 2 ^13 u23 Br 66 50 63 11 - 8 - 5 0 60( 2) 63( 2) 69( 2) -8( 2) -18( 2) -19( 2) C l 47( 3) 41( 2) 52( 3) 5( 2) -3( 2) -7( 2) C2 40( 2) 49( 3) 50( 3) -9( 2) 10( 2) -11( 2) C3 56( 3) 47( 2) 34( 2) -10( 2) 7( 2) -4( 2) C4 41( 2) 38( 2) 39( 2) -7( 2) 4( 2) -4( 2) C5 46( 3) 41( 3) 42( 2) -3( 2) 4( 2) 1( 2) C6 54( 3) 52( 3) 41( 3) -1( 2) 6( 2) -6( 2) C7 55( 3) 37( 2) 37( 2) -3( 2) 0( 2) 3(2) C8 64( 3) 39( 2) 59( 3) -3( 2) -20( 2) -6( 2) C9 47( 3) 42( 3) 70( 3) 3( 2) -12( 2) -6( 2) CIO 54( 3) 36( 2) 49( 2) 2( 2) -4( 2) 2( 2) C l l 71( 4) 33( 3) 64( 3) -7( 3) 5( 3) -13( 3) C12 57( 3) 45( 3) 64( 3) -14( 2) 4( 2) -9( 2) C13 42( 2) 41( 2) 40( 2) -8( 2) 6( 2) -6(2) C14 61( 3) 50( 3) 44( 3) -1( 2) -4( 2) 0(2) C15 76( 3) 59( 3) 43( 3) -7( 3) -6( 3) -13( 2) C16 65( 3) 55( 3) 58( 3) -15( 3) 22( 3) -20( 3) C17 53( 3) 54( 3) 65 ( 3) 3( 3) 5( 2) -14( 3) C18 46( 3) 58( 3) 50( 3) -2( 2) 0( 2) -13( 2) jThe anisotropic thermal parameters employed in the refinement are UU in the expression: / = / 0exp(-27r 2SSC,,/i 1^a, * a,*) Chapter S. Results and Discussion 64 Table 8.34: Bond lengths for the photoproduct with estimated standard deviations in parentheses Bond Length (A) Bond Length (A) Br -- CIO 1.900(4) C7 -- C12 1.405(6) 0 - C l 1.207(5) CS - C9 1.369(7) Cl - C2 1.484(6) C9 - CIO 1.378(6) Cl - C6 1.499(7) CIO - C l l 1.363(6) C2 - C3 1.527(6) C l l - C12 1.372(7) C2 - C4 1.533(6) C13 - C14 1.384(6) C3 - C4 1.495(6) C13 - CIS 1.392(6) C3 - Cl 1.491(6) C14 - C15 1.387(6) CA - Cb 1.524(6) C15 - C16 1.358(8) CA - C13 1.493(6) C16 - C17 1.382(7) Cb - C6 1.522(6) C17 - CIS 1.388(6) Cl - C8 1.381(6) Chapter S. Results and Discussion 65 Table 8.35: Bond angles for the photoproduct (°) with estimated standard deviations in parentheses Bonds Angle (°) Bonds Angle ( ° ) 0 - C l - C2 125.1(4) C3 - C 7 - C12 121.6( 4) o - C l - C6 125.4(4). CS - C 7 - C12 117.2( 4) C2 - C l - C6 109.3(4) Cl - C 8 - C9 122.5( 4) Cl - C2 - C3 118.4(4) CS - C9 - C10 119.0( 4) Cl - C2 - CA 107.4(4) Br - C10 -- C9 120.3( 3) C3 - C2 - CA 58.5(3) Br- - C10 - C l l 119.8( 3) C2 - C3 - CA 61.0(3) C9 -- C 1 0 - C l l 120.0( 4) C2 - C3 - Cl 124.6(4) C10 - C l l -- C12 121.2( 5) CA - C3 - Cl 123.8(4) C 7 -- C12 - C l l 120.0( 4) 02 - CA - C3 60.6(3) C4 -- C13 - C14 121.4( 4) C2 -CA- Cb 106.6(3) C4 -- C13 - C18 120.1( 4) C2 - CA- C13 122.8(3) C14 - C13 - CIS 11S.4( 4) C3 - CA - Cb 116.4(4) C13 - C14 -- C15 120.8( 5) C3 - CA- C13 120.7(3) C14 - C15 - C16 120.2( 5) C5 -CA- C13 117.0(4) C15 - C16 -- C17 120.4( 5) CA - Cb - C6 107.6(4) C16 - Cll -- CIS 119.6( 5) Cl - C6 - C5 106.1(3) C13 - CIS -- C17 120.6( 4) C3 - C7 - CS 121.2(4) Bibliography [1] M.D. Cohen, G.M.J . Schmidt. J. Chem. Soc. 1996 (1964). [2] M . Garcia-Garibay, J.R. Scheffer, J. Trotter, F. Wireko, Tet. Lett.. 28, 4789 (1987). [3] S.V. Evans, M. Garcia-Garibay, N. Omkaram, J.R. Scheffer, J. Trotter, F. Wireko, J. Am. Chem. Soc... 108. 5648 (1986). [4] M. Garcia-Garibay, J.R. Scheffer, J. Trotter, F. Wireko, Tet. Lett.. 29, 1485 (1988). [5] R.E. Marsh. E. Ubell, H.E, Wilcox, Acta Cryst., 15, 35 (1962). [6] G.H. Stout, L .H. Jensen, X-ray Structure Determination: A Practical Guide MacMillan Co., New York, 1968. [7] R. Rudman, Low-temperature X-ray Diffraction, Plenum Press, New York, 1976. [8] J.P. Glusker, K.N. Trueblood, Crystal Structure Analysis: A Primer, Oxford Uni-versity Press, New York, 1985. [9] S.J. Rettig, E N P R O C , a data reduction program written in F O R T R A N IV for in-tensities measured on an Enraf-Nonius CAD4 diffractometer, University of British Columbia, Vancouver, 1978 (unpublished). 66 Bibliography 67 10 11 12 13 14 15 16 17 18 Instruction Manual for Universal Low Temperature Device, Enraf Nonius, Delft. CRC Handbook of Chemistry and Physics, 57th ed., R.C. Weast, Ed., C R C Press, Ohio, 1976. D.W.J. Cruickshank, Acta Cryst., 9, 754 (1956). D.W.J. Cruickshank, Acta Cryst., 9, 757 (1956). D.W.J. Cruickshank, Acta Cryst., 9, 1005 (1956). R.L. Hilderbrandt, E .M.A. Peixoto, J. Molec. Struct.. 12, 31 (1972). P. Main, S.J. Fiske, S.E. Hull, L. Lessinger, G. Germain, J.-P. Declercq, M.M. Woolfson, MULTANSO, University of York, England, and Louvain, Belgium (1980). W . C . Hamilton, Acta Cryst., 18, 502 (1965). H.E. Zimmerman, J.W. Wilson, J. Am. Chem. Soc. 86, 4036 (1964). 19] D.I. Schuster, Photochemical Rearrangements of Enones, Rearrangements in Ground and Excited States, Vol. 3, P. de Mayo, Ed., Academic Press, pp. 187-193,'1980. [20] H.E . Zimmerman, R.D. Rieke, J.R. Scheffer, J. Am. Chem. Soc. 89, 2033 (1967). Appendix A Torsion Angles 68 Appendix A. Torsion Angles 69 Tab le A.36: Torsion angles ( c ) w i t h est imated standard deviat ions in parentheses for maleic anhydr ide at room temperature  A t oms Value ( c ) 0 1 - C l -C2 -C3 -1.3(3) 0 2 - C l -C2 -C3 179.0(3) C 2 - C l -01 -C4 1.8(2) 0 2 - C l -01 -C4 -178.5(2) C l - C2 -C3 -C4 0.3(3) C 2 -C3 -C4 -01 0.8(2) C 2 -C3 -C4 - 0 3 -179.5(2) C 3 -C4 -01 - C l -1.6(2) 0 3 -C4 -01 - C l 178.6(2) 0 1 - C l -C2 -H2 177(2) 0 2 - C l -C2 -H2 -2(2) C l -C2 -C3 -H3 177(2) H2 -C2 -C3 -C4 -178(3) H2 -C2 -C3 -H3 -1(4) H3 -C3 -C4 -01 ' -176(2) H 3 - C 3 -C4 - 0 3 4(2) Appendix A. Torsion Angles 70 Table A.37: Torsion angles (°) with estimated standard deviations in parentheses for maleic anhydride at low temperature Atoms Yalue(°) 01 - C l -C2 -C3 -1.4(8) 02 - C l -C2 -C3 -177.5(9) C2 - C l -01 -C4 0.6(8) 02 - C l -01 -C4 177.1(7) C l -C2 -C3 -C4 1.6(7) C2 -C3 -C4 -01 -1.3(8) C2 -C3 -C4 -03 177.3(9) C3 -C4 -01 - C l 0.4(8) 03 -C4 -01 - C l -178.4(7) 01 - C l -C2 -H2 178.4(7) 02 - C l -C2 -H2 2.3(13) C l -C2 -C3 -H3 178.0(8) H2 -C2 -C3 -C4 -178.3(7) H2 -C2 -C3 -H3 -1.9(14) H3 -C3 -C4 -01 -177.8(7) H3 -C3 -C4 -03 0.8(13) Appendix A. Torsion Angles 71 Table A.38: Torsion angles (°) with estimated standard deviations in parentheses for the cyclohexenone Atoms Value (°) 0 - C l -C2 -C3 41.4(4) C 6 - C l - C 2 - C 3 -1.9(7) 0 - C l - C 6 - C 5 -40.3(3) C2 - C l -C6 -C5 2.0(7) C l - C 2 - C 3 - C 4 -0.0(7) C2 -C3 -C4 -Co 1.8(7) C 2 - C 3 - C 4 -C7 178.7(4) C 2 - C 3 -C4 -C13 140.1(4) C 3 - C 4 - C 5 - C 6 -1.7(6) C 7 - C 4 - C 5 -C6 -178.6(4) C13 -C4 -C5 -C6 -140.5(4) C 3 - C 4 -C7 -C8 149.3(4) C 3 - C 4 -C7 -C12 30.7(5) C 5 - C 4 - C 7 -C8 -33.9(5) C 5 - C 4 -C7 -C12 -152.5(4) C13 -C4 -C7 -C8 -121.4(4) C13 -C4 -C7 -C12 120.0(5) C3 -C4 -C13 -C14 -72.0(4) C3 -C4 -C13 -C18 103.7(7) C5 -C4 -C13 -C14 67.9(4) C5 -C4 -C13 -C18 -116.4(7) C7 -C4 -C13 -C14 178.4(4) C7 -C4 -C13 -C18 -5.9(7) C4 -C5 -C6 - C l -0.2(7) C4 -C7 -C8 -C9 -72.1(5) C12 -C7 -C8 -C9 48.7(5) C4 -C7 -C12 - C l l 86.2(6) C8 -C7 -C12 - C l l -35.0(6) C 7 - C 8 -C9 -CIO -43.4(7) C8 -C9 -CIO -Br 81.8(5) cont'd next page... Appendix A. Torsion Angles 72 ...cont'd A t o m s Value(°) C8-C9 - C I O - C l l 18.8(8) B r - C I O -C l l -C12 -62.0(7) C 9 -CIO -C l l -C12 -4.4(10) C IO - C l l -C12 -C7 14.7(10) C4 -C13 -C14 -C15 177.1(4) C18 -C13 -C14 -C15 -0.8(6) C 4 - C 1 3 -C18 - C17 -174.6(5) C14 -C13 -C18 -C17 0.6(7) C 1 3 -C14 -C15 -C16 0.4(7) C14 -C15 -C16 -C17 0.1(7) C 1 5 -C16 -C17 -C18 -0.3(8) C16 -C17 -C18 -C13 -0.1(8) Appendix A. Torsion Angles 73 Table A.39: Torsion angles (°) with estimated standard deviations in parentheses for the cyclohexenone with split atoms Atoms Value (°) 0 - C l -C2 -C3 -174.7(7) C 6 - C l - C 2 - C 3 2.7(13) 0 - C l - C 6 - C 5 -162.3(8) C2 - C l -C6 -C5 20.8(11) 0 - C l ' -C2 ' -C3 161.4(7) C6' - C l ' -C2 ' -C3 -26(2) 0 - C l ' -C6 ' -C5 175(2) C2 ' - C l ' -C6 ' -C5 1(3) C l -C2 -C3 -C4 2.3(11) C l ' -C2 ' -C3 -C4 58(2) C2 -C3 -C4 -C5 -28.1(7) C2 -C3 -C4 -C7 93.1(6) C2 -C3 -C4 -C13 -145.0(6) C2' -C3 -C4 -C5 -59.0(12) C2' -C3 -C4 -C7 62.2(13) C2' -C3 -C4 -C13 -175.9(12) C3 -C4 -C5 -C6 53.3(6) C3 -C4 -C5 -C6 ' 27.1(11) C 7 - C 4 - C 5 - C 6 -67.2(6) C7 -C4 -C5 -C6 ' -93.4(11) C13 -C4 -C5 -C6 169.6(5) C13 -C4 -C5 -C6 ' 143.4(10) C3 - C 4 - C 7 - C 8 30.6(6) C3 -C4 -C7 -C12 -152.2(4) C5 -C4 -C7 -C8 149.0(4) C5 -C4 -C7 -C12 -33.8(5) C13 -C4 -C7 -C8 -89.3(5) C13 -C4 -C7 -C12 87.9(5) C3 -C4 -C13 -C14 -123.4(4) C3 -C4 -C13 -C18 55.4(5) cont'd next page... Appendix A. Torsion Angles 74 ...cont'd Atoms Value (°) C5 -C4 -C13 -C14 121.1(4) C5 -C4-C13-C18 -60.2(5) C 7 - C 4 -C13-C14 -2.1(5) C 7 - C 4 - C 1 3 - C 1 8 176.7(4) C4 -C5 -C6 - C l -51.3(8) C4 -C5 -C6' - C l ' -1(2) C4 -C7 -C8 -C9 178.8(4) C12 -C7 -C8 -C9 1.6(7) C4 -C7 -C12 - C l l -178.6(4) C8 -C7 -C12 - C l l -1.3(7) C 7 - C 8 - C 9 -CIO 0.2(8) C8 -C9 -CIO -Br 178.0(4) C8 -C9 -CIO - C l l -2.2(8) Br -CIO - C l l -C12 -177.7(3) C9 -CIO - C l l -C12 2.4(7) CIO - C l l -C12 -C7 -0.7(7) C4 -C13 -C14 -C15 178.0(4) C18 -C13 -C14 -C15 -0.8(7) C4 -C13 -C18 -C17 -178.9(4) C14 -C13 -C18 -C17 -0.0(7) C13 -C14 -C15 -C16 0.7(8) C14 -C15 -C16 -C17 0.3(8) C15 -C16 -C17 -C18 -1.1(8) C16 -C17 -C18 -C13 1.0(8) Appendix A. Torsion Angles Table A.40: Torsion angles (°) with estimated standard deviations in parentheses for the photoproduct Atoms Value (°) 0 -C l - C2 -C3 133.5(4) 0 -C l - C2 -C4 -163.4(4) C6 - C l -C2 -C3 -50.9(5) C6 - C l -C2 -C4 12.1(5) 0 -C l - C6 -C5 157.8(4) C2 - C l - C 6 - C o -17.7(5) C l -C2 -C3 -C4 93.9(4) C l -C2 - C 3 - C 7 -19.1(6) C4 -C2 -C3 -C7 -113.0(5) C l -C2 - C 4 - C 3 -113.1(4) C l -C2 -C4 -C5 -1.7(5) C l -C2 -C4 -C13 137.4(4) C3 -C2 - C 4 - C 5 111.4(4) C3 -C2 -C4 -C13 -109.4(4) C2 -C3 - C 4 - C 5 -94.9(4) C2 -C3 -C4 -C13 112.9(4) C7 -C3 - C 4 - C 2 114.2(5) C7 -C3 - C 4 - C 5 19.2(5) C7 -C3 - C 4 - C 1 3 -133.0(4) C2 -C3 -C7-C8 137.3(4) C2 -C3 -C7 -C12 -43.7(6) C4 -C3 -C7-C8 61.7(6) C4 -C3 -C7 -C12 -119.4(5) C2 -C4 -C5 -C6 -9.1(5) C3 -C4 -C5 -C6 55.8(5) C13 -C4 -C5 -C6 -150.9(4) C2 -C4 -C13 -C14 118.7(5) C2 -C4 -C13 -C18 -65.7(6) C3 -C4 -C13 -C14 46.0(5) cont'd next page... Appendix A. Torsion Angles 76 ...cont'd Atoms Va lue (°) C 3 -C4 -C13 -C18 -138.3(4) C 5 -C4 -C13 -C14 -106.0(5) C 5 -C4 -C13 -C18 69.6(5) C 4 - C 5 - C 6 - C l 16.3(5) C 3 - C 7 - C 8 - C 9 -177.9(4) C12 -C7 -C8 - C9 3.1(7) C 3 -C7 -C12 - C l l 178.5(4) C8 -C7 -C12 - C l l -2.5(7) C 7 - C 8 - C 9 -C IO -0.6(7) C 8 - C 9 - C I O - B r 176.1(4) C 8 - C 9 - C I O - C l l -2.6(7) B r -CIO - C l l -C12 -175.5(4) C9 -CIO - C l l -C12 3.2(7) C IO - C l l -C12 - C 7 -0.6(8) C4 -C13 -C14 -C15 175.4(4) C18 -C13 -C14 -C15 -0.3(7) C 4 -C13 -C18 -C17 -176.4(4) C14 -C13 -C18 -C17 -0.7(7) C13 -C14 -C15 -C16 0.8(7) C14 -C15 -C16 -C17 -0.3(8) C 1 5 -C16 -C17 -C18 -0.7(7) C16 -C17 -C18 -C13 1.2(7) Appendix B Structure Factors for Maleic Anhydride at 295K 77 h k 1 FO Fc weight h k 1 0 -1 14 86 15 73 0 41 0 8 -5 0 1 -2 15 09 16 09 10 65 0 9 -1 0 1 -3 0 26* 0 12 6 32 0 9 -2 O 1 -4 0 56* 0 12 94 32 0 9 -3 0 1 -5 1 62 1 51 368 73 0 9 -4 0 1 -6 0 44* 0 48 10 24 0 9 -5 0 2 0 4 12 4 05 128 58 0 10 0 0 2 -.1 16 81 18 22 0 32 0 10 -1 0 2 -2 10 68 1 1 27 20 62 0 10 -2 O 2 -3 1 95 1 97 835 59 0 10 -3 0 2 -4 5 01 5 18 93 07 0 10 -4 0 2 -5 2 39 2 40 455 99 0 1 1 - 1 0 2 -6 1 23 1 26 328 86 0 1 1 -2 0 3 -1 7 94 7 55 36 82 0 1 1 -3 0 3 -2 7 48 7 62 39 60 0 1 1 -4 0 3 -3 13 08 13 08 13 73 0 12 0 o 3 -4 2 59 2 69 467 45 0 12 -1 0 3 -5 0 45* 0 39 43 98 0 12 -2 0 3 -6 0 28* 0 40 24 88 0 12 -3 0 4 0 3 85 3 72 121 56 0 13 -1 0 4 -1 9 09 9 22 28 20 0 13 -2 0 4 -2 4 73 5 05 80 78 0 14 0 0 4 -3 3 65 3 60 187 78 1 0 -1 0 4 -4 3 44 3 45 214 73 1 0 -2 0 4 -5 2 13 2 29 452 31 1 O -3 o 4 -6 1 02 1 13 313 78 1 0 -4 o 5 -1 4 79 4 60 81 52 1 0 -5 0 5 -2 1 00 0 74 442 88 1 0 -6 0 5 -3 3 73 3 45 170 01 1 1 0 0 5 -4 0 65 0 61 95 69 1 1 -1 0 5 -5 1 97 2 17 440 40 1 1 -2 0 5 -6 1 36 1 48 476 57 1 1 -3 0 6 0 2 25 2 19 712 24 1 1 -4 0 6 -1 7 13 6 98 41 65 1 1 -5 0 6 -2 1 87 1 78 673 99 1 1 -6 0 6 -3 3 80 3 63 160 49 1 2 O o 6 -4 2 67 2 72 469 94 1 2 -1 0 6 -5 1 61 1 61 405 43 1 2 -2 0 6 -6 0 24* 0 30 6 91 1 2 -3 0 7 -1 6 oo 5 63 52 94 1 2 -4 0 7 -2 2 85 3 06 363 09 1 2 -5 0 7 -3 1 7 1 1 51 420 20 1 2 -6 0 7 -4 0 37* 0 52 4 99 1 3 0 0 7 -5 0 35* 0 45 38 22 1 3 -1 o 8 O 7 90 7 39 33 50 1 3 -2 o 8 - 1 4 42 4 23 1 10 97 1 3 -3 0 8 -2 3 28 3 26 318 56 1 3 -4 0 8 -3 4 44 4 41 110 93 1 3 -5 0 8 -4 2 34 2 25 503 68 1 3 -6 Fo Fc weight h k 1 Fo Fc 0 65* 0 83 37 57 1 4 0 8 33 8 43 1 21 1 32 314 52 1 4 - 1 7 89 7 77 2 16 2 20 462 47 1 4 -2 10 04 10 16 2 31 2 31 476 53 1 4 -3 0 51* 0 64 1 24 1 30 296 56 1 4 -4 2 82 2 93 0 26* 0 21 12 94 1 4 -5 1 97 2 00 0 45* 0 17 7 58 1 4 -6 0 28* 0 40 1 81 1 81 395 21 1 5 0 8 07 7 91 0 37* 0 51 5 21 1 5 - 1 2 25 2 16 0 43* 0 42 8 27 1 5 -2 9 12 9 27 0 29* 0 31 10 56 1 5 -3 4 37 4 32 4 81 4 87 93 64 1 5 -4 4 45 4 59 0 38* 0 20 6 92 1 5 -5 O 76 0 76 1 13 1 04 345 82 1 5 -6 0 49* 0 24 0 27* 0 1 1 17 28 1 6 0 1 10 1 12 2 39 2 41 537 95 1 6 -1 6 94 7 04 0 37* 0 35 1 1 13 1 6 -2 4 96 4 84 0 47* 0 75 21 83 1 6 -3 4 91 5 01 0 46* O 57 32 25 1 6 -4 0 96 0 97 0 39* 0 12 12 66 1 6 -5 0 26* 0 33 0 76 0 84 286 84 1 6 -6 0 31* 0 34 0 21* 0 10 12 78 1 7 0 4 28 4 17 17 83 19 16 0 29 1 7 - 1 4 35 4 45 12 82 13 19 14 53 1 7 -2 3 42 3 28 2 21 2 31 626 00 1 7 -3 2 20 2 09 3 80 3 81 162 81 1 7 -4 2 73 2 66 2 72 2 82 417 24 1 7 -5 0 62* 0 82 0 62 0 79 108 21 1 8 0 0 31* 0 30 15 25 18 22 0 40 1 8 - 1 3 07 2 88 25 82 31 67 0 14 1 8 -2 2 23 2 19 10 95 1 1 21 19 67 1 8 -3 0 71* 0 85 1 1 17 1 1 10 18 44 1 8 -4 0 50* 0 4 1 2 40 2 36 586 37 1 8 -5 0 95 1 00 3 59 3 54 223 49 1 9 0 O 40* 0 19 0 75 0 80 159 86 1 9 -1 2 30 2 19 22 27 25 87 0 19 1 9 -2 2 01 1 97 9 90 10 34 24 31 1 9 -3 2 13 2 17 10 52 1 1 08 21 18 1 9 -4 1 63 1 60 7 32 7 45 38 92 1 9 -5 0 78 0 89 2 29 2 32 559 69 1 10 0 0 54* 0 88 2 50 2 63 463 93 1 10 - 1 1 46 1 45 1 19 1 15 333 69 1 10 -2 2 89 3 04 7 63 7 92 40 24 1 10 -3 0 80* 0 98 15 63 16 93 0 64 1 10 -4 1 39 1 35 3 15 3 38 227 74 1 11 0 0 49* 0 26 3 17 3 21 237 95 1 1 1 - 1 2 40 2 43 4 55 4 57 100 51 1 1 1 -2 1 88 1 88 2 38 2 39 427 17 1 1 1 -3 0 22* 0 08 0 98 1 08 260 75 1 1 1 -4 0 73 0 72 weight h k 1 Fo Fc weight 33 51 1 12 0 0 88 0 83 197 97 36 50 1 12 - 1 1 07 1 06 288 95 3 22 85 1 12 -2 1 92 1 93 591 07 o_ 25 20 1 12 -3 0 44* 0 45 36 68 H 436 76 1 13 0 0 91 0 91 306 82 (3D 439 78 1 13 - 1 1 21 1 32 461 18 5 20 1 13 -2 0 38* 0 54 25 92 34 70 2 0 0 12 96 13 86 14 56 584 34 2 0 -1 14 23 15 54 0 78 26 84 2 0 -2 2 13 2 14 883 OO 1 10 18 2 0 -3 6 36 6 23 48 84 97 96 2 0 -4 0 41* 0 55 12 49 135 38 2 0 -5 2 46 2 39 476 94 32 85 2 0 -6 1 10 1 12 300 31 555 98 2 1 0 16 73 19 33 0 33 43 30 2 1 - 1 22 74 25 23 0 18 79 48 2 1 -2 8 18 8 50 33 55 93 81 2 1 -3 6 16 6 26 51 30 162 35 2 1 -4 2 74 2 72 421 55 3 59 2 1 -5 1 41 1 43 321 13 18 94 2 1 -6 0 98 1 04 280 43 123 23 2 2 0 30 41 36 65 0 10 1 18 81 2 2 -1 16 85 18 30 0 54 244 12 2 2 -2 2 14 2 12 681 94 528 46 2 2 -3 5 34 5 79 62 51 485 53 2 2 -4 2 83 2 81 439 37 34 53 2 2 -5 0 89 0 86 169 85 4 60 2 2 -6 0 34* 0 13 8 52 321 49 2 3 0 7 44 7 42 41 24 533 30 2 3 - 1 9 40 9 85 26 34 30 77 2 3 -2 7 26 7 65 40 74 67 45 2 3 -3 3 46 3 63 186 58 327 47 2 3 -4 1 70 1 83 438 73 1 1 33 2 3 -5 3 10 3 21 298 55 530 31 2 3 -6 0 42* 0 60 1 1 88 421 57 2 4 O 3 32 3 21 197 42 453 31 2 4 - 1 6 89 7 2 1 45 38 434 39 2 4 -2 7 18 7 00 40 81 303 59 2 4 -3 4 54 4 32 108 07 18 29 2 4 -4 3 43 3 35 234 94 337 78 2 4 -5 1 68 1 84 386 83 328 4 1 2 4 -6 O 34* 0 33 8 73 39 26 2 5 0 7 51 7 29 38 92 482 48 2 5 - 1 7 50 7 78 38 31 14 91 2 5 -2 2 80 2 86 373 39 513 50 2 5 -3 3 17 3 4 1 289 44 482 00 2 5 -4 0 84 0 72 155 1 1 3 83 2 5 -5 0 60* 0 65 94 80 325 60 2 5 -6 0 27* 0 37 12 61 oo h k 1 Fo Fc weight h k 1 Fo Fc we\ght h k 1 Fo Fc weight h k 1 Fo Fc weight It. 2 6 0 0 51* 0 88 36 03 3 1 -4 4 18 4 40 1 19 18 3 9 - 1 3 93 3 96 159 64 4 4 -5 0 36* 0 08 7 92 ts 2 6 -1 6 57 6 61 46 48 3 1 -5 2 50 2 51 501 69 3 9 -2 2 6 1 2 57 503 07 4 5 0 1 66 1 69 527 41 a 2 6 -2 6 06 5 97 50 12 3 1 -6 0 75 0 79 225 07 3 9 -3 1 61 1 59 427 83 4 5 -1 2 95 3 01 303 20 a . s-». 2 6 -3 3 26 3 35 246 31 3 2 0 12 51 13 18 15 35 3 9 -4 0 39* 0 45 18 07 4 5 -2 3 74 3 82 171 85 H 2 6 -4 0 85 0 90 148 96 3 2 -1 3 30 3 39 190 53 3 10 0 2 12 2 27 477 90 4 5 -3 1 43 1 38 325 69 to 2 6 -5 0 65* 0 77 31 09 3 2 -2 13 36 13 96 13 28 3 10 - 1 2 1 1 2 05 479 19 4 5 -4 1 37 1 19 330 67 2 7 0 1 65 1 53 587 06 3 2 -3 2 43 2 31 471 67 3 10 -2 O 95 0 92 212 35 4 5 -5 O 65 0 63 153 13 2 7 -1 1 59 1 56 524 96 3 2 -4 2 36 2 46 479 19 3 10 -3 0 76 0 67 181 21 4 6 0 1 91 1 73 527 08 2 7 -2 1 98 1 99 533 74 3 2 -5 0 35* 0 42 9 73 3 10 -4 0 24* 0 20 13 28 4 6 -1 1 27 1 26 332 35 2 7 -3 3 67 3 64 185 48 3 2 -6 0 52* O 66 34 75 3 1 1 O O 37* 0 32 13 63 4 6 -2 1 70 1 7 1 436 91 2 7 -4 2 25 2 39 483 46 3 3 0 5 92 5 62 58 48 3 1 1 - 1 1 07 0 96 299 02 4 6 -3 2 45 2 66 475 49 2 7 -5 o 65 0 52 136 10 3 3 -1 14 73 15 44 1 1 07 3 1 1 -2 0 72 0 79 171 12 4 6 -4 1 37 1 30 399 29 2 8 0 4 96 4 92 94 50 3 3 -2 3 38 3 53 177 00 3 1 1 -3 0 32* 0 33 9 55 4 6 -5 0 51* 0 59 38 08 2 8 -1 2 25 2 21 563 10 3 3 -3 2 98 3 10 362 50 3 12 0 0 40* 0 1 1 18 17 4 7 0 4 04 3 90 146 94 2 8 -2 2 47 2 60 549 08 3 3 -4 4 20 4 34 1 17 26 3 12 -1 0 61 0 69 140 77 4 7 - 1 4 21 4 29 140 20 2 8 -3 2 02 1 99 446 44 3 3 -5 0 36* 0 14 1 1 05 3 12 -2 0 55 0 63 142 10 4 7 -2 4 42 4 30 1 12 92 2 8 -4 1 88 1 90 498 11 3 3 -6 0 48* 0 61 34 24 3 13 0 0 35* 0 31 15 21 4 7 -3 0 96 1 00 182 62 2 8 -5 0 32* 0 35 8 08 3 4 0 3 52 3 70 166 07 3 13 - 1 0 68 0 70 286 87 4 7 -4 0 52* 0 60 83 84 2 9 0 0 32* 0 41 4 21 3 4 -1 2 65 2 62 412 99 4 0 0 12 39 12 79 15 42 4 7 -5 0 63 0 59 256 32 2 9 -1 2 71 2 70 473 49 3 4 -2 7 33 7 22 38 37 4 0 -1 4 23 4 46 104 35 4 8 0 4 33 4 27 1 16 27 2 9 -2 3 59 3 60 203 95 3 4 -3 0 98 1 06 219 12 4 0 -2 1 49 1 37 513 98 4 8 -1 1 42 1 29 312 66 2 9 -3 1 80 1 74 425 92 3 4 -4 1 74 1 75 367 14 4 0 -3 0 42* 0 18 14 08 4 8 -2 1 42 1 43 338 35 2 9 -4 0 93 0 74 269 50 3 4 -5 0 38* 0 09 6 87 4 0 -4 1 54 1 38 331 04 4 8 -3 1 94 1 95 505 76 2 10 0 5 77 5 57 50 08 3 4 -6 0 80 0 67 362 21 4 0 -5 0 96 1 20 220 04 4 8 -4 0 38* 0 21 1 1 28 2 10 -1 1 19 1 .18 241 85 3 5 0 8 17 7 78 32 62 4 0 -6 0 19* 0 03 8 41 4 9 0 2 14 2 22 457 77 2 10 -2 1 46 1 45 341 44 3 5 -1 4 04 3 78 132 87 4 1 0 1 58 1 60 77 1 OO 4 9 - 1 1 46 1 51 355 77 2 10 -3 1 16 1 14 300 40 3 5 -2 3 47 3 45 200 06 4 1 - 1 1 27 1 23 563 77 4 9 -2 0 72 0 72 137 82 2 10 -4 0 37* 0 47 21 04 3 5 -3 4 62 4 47 98 16 4 1 -2 3 82 4 02 130 54 4 9 -3 0 40* 0 62 15 99 2 11 0 1 85 1 76 454 54 3 5 -4 2 58 2 66 483 77 4 1 -3 3 52 3 60 252 18 4 9 -4 0 38* 0 47 24 20 2 11 -1 0 37* 0 58 5 67 3 5 -5 1 41 1 26 405 78 4 1 -4 3 15 3 06 301 00 4 10 0 1 09 1 05 273 34 2 11 -2 o 87 0 88 216 63 3 6 0 0 34* 0 51 6 72 4 1 -5 1 40 1 38 374 75 4 10 - 1 1 28 1 26 352 28 2 11 -3 0 41* 0 10 12 21 3 6 -1 4 46 4 27 1 1 1 35 4 1 -6 0 65* 0 81 85 62 4 10 -2 0 70 0 63 142 77 2 12 0 1 14 1 06 322 80 3 6 -2 3 60 3 51 225 56 4 2 0 5 07 5 14 70 07 4 10 -3 0 37* 0 35 12 54 2 12 -1 1 42 1 43 420 54 3 6 -3 0 45* O 44 7 65 4 2 - 1 6 08 6 09 52 68 4 11 0 0 84 0 66 2 18 47 2 12 -2 0 48* 0 47 25 00 3 6 -4 3 21 3 1 1 290 81 4 2 -2 2 37 2 30 492 66 4 11 - 1 0 99 0 93 304 10 2 12 -3 0 26* 0 24 14 47 3 6 -5 0 38* 0 48 15 17 4 2 -3 1 77 1 85 463 15 4 11 -2 0 28* 0 32 6 55 2 13 0 0 39* 0 46 23 56 3 7 0 1 15 1 01 326 18 4 2 -4 2 46 2 38 491 36 4 12 0 0 32* 0 49 9 50 2 13 -1 0 97 1 04 346 94 3 7 - 1 1 29 1 20 337 82 4 2 -5 0 50* 0 86 19 04 4 12 - 1 0 67 0 58 260 60 2 13 -2 0 23* 0 41 12 95 3 7 -2 1 15 1 28 261 94 4 3 0 5 84 6 01 56 18 5 0 -1 0 78 0 79 180 35 3 0 -1 5 59 5 25 65 52 3 7 -3 4 74 4 70 93 74 4 3 - 1 7 59 7 78 36 49 5 0 -2 0 96 1 06 225 07 3 0 -2 8 86 9 03 28 50 3 7 -4 0 79 0 95 154 68 4 3 -2 2 84 2 94 379 88 5 0 -3 3 09 3 17 258 36 3 0 -3 0 38* 0 63 6 83 3 7 -5 0 35* 0 46 9 55 4 3 -3 0 75 0 72 135 09 5 0 -4 1 89 2 16 454 63 3 0 -4 1 65 1 59 407 24 3 8 0 4 29 4 45 105 92 4 3 -4 1 60 1 55 377 34 5 0 -5 1 01 0 97 298 84 3 0 -5 0 87 1 1 1 154 87 3 8 -1 0 62* 0 49 25 67 4 3 -5 0 66 0 64 128 48 5 1 0 0 30* 0 00 9 63 3 o -6 1 55 1 43 601 35 3 8 -2 2 16 2 06 448 07 4 4 0 5 10 4 73 65 9 1 5 1 -1 5 47 5 54 57 64 3 1 0 9 31 9 65 26 95 3 B -3 2 78 2 73 443 96 4 4 - 1 1 1 09 1 1 12 1B 56 5 1 -2 1 10 1 03 271 01 3 1 - 1 3 43 3 49 189 06 3 8 -4 0 36* 0 13 7 62 4 4 -2 8 58 8 55 28 75 5 1 -3 3 30 3 40 277 58 3 1 -2 3 45 3 43 189 57 3 8 -5 0 75 0 59 318 53 4 4 -3 3 15 3 28 299 19 5 1 -4 1 50 1 44 383 16 -1 3 1 -3 2 18 2 27 637 62 3 9 O 0 97 1 07 186 73 4 4 -4 0 62* O 60 88 77 5 1 -5 0 4 1 • 0 42 20 23 CD h k 1 Fo Fc weight 5 2 0 4 43 4 36 1 1 1 6 5 2 - 1 5 68 5 66 54 00 5 2 -2 2 41 2 34 568 64 5 2 -3 0 63* 0 54 23 42 5 2 -4 0 58* 0 78 80 56 5 2 -5 O 34* 0 23 8 60 5 3 0 5 26 4 92 59 55 5 3 -1 2 76 2 75 485 56 5 3 -2 2 79 2 87 477 27 5 3 -3 2 88 2 71 355 65 5 3 -4 1 71 1 71 462 89 5 3 -5 0 86 0 89 278 15 5 4 0 1 89 1 92 514 86 5 4 -1 3 52 3 43 225 44 5 4 -2 1 16 1 30 267 65 5 4 -3 2 44 2 59 464 00 5 4 -4 0 56* 0 48 92 83 5 4 -5 0 29* 0 28 7 65 5 5 0 1 99 2 02 496 00 5 5 -1 1 71 1 77 422 51 5 5 -2 2 44 2 55 485 93 5 5 -3 3 69 3 75 171 97 5 5 -4 1 40 1 53 390 43 5 5 -5 0 79 0 71 334 37 5 6 0 0 67* o 88 26 91 5 6 -1 1 86 1 84 398 66 5 6 -2 3 37 3 37 197 85 5 6 -3 2 26 2 21 515 84 5 6 -4 1 33 1 22 435 78 5 7 0 2 38 2 22 449 94 5 7 -1 1 61 1 55 354 25 5 7 -2 2 19 2 23 474 47 5 7 -3 1 36 1 20 359 68 5 7 -4 1 05 0 94 395 60 5 8 O 2 85 3 01 418 28 5 8 -1 2 10 2 07 475 27 5 8 -2 0 41* 0 43 7 92 5 8 -3 0 92 O 93 243 75 5 8 -4 1 02 0 90 535 69 5 9 0 2 26 2 22 542 12 5 9 - 1 0 52* 0 87 22 33 5 9 -2 0 93 1 02 239 27 5 9 -3 0 54* O 71 43 24 5 10 0 1 08 1 00 332 35 5 10 - 1 O 43* 0 52 20 28 5 10 -2 0 87 0 77 310 79 5 1 1 0 0 34* 0 32 12 93 5 1 1 - 1 0 21* 0 46 24 09 6 0 0 5 52 5 63 53 84 h k 1 Fo Fc weight 6 0 -1 2 20 2 09 519 77 6 0 -2 1 27 1 21 281 76 6 O -3 O 93 0 83 187 92 6 0 -4 1 33 1 40 394 36 6 0 -5 0 66 0 64 271 81 6 1 0 0 61* 0 8 1 23 38 6 1 -1 2 53 2 47 525 93 6 1 -2 1 42 1 31 323 83 6 1 -3 1 70 1 73 404 51 6 1 -4 0 55* 0 56 89 77 6 2 0 2 24 2 27 514 79 6 2 - 1 3 31 3 26 235 32 6 2 -2 1 47 1 35 326 25 6 2 -3 0 93 0 93 183 00 6 2 -4 0 34* 0 10 9 99 6 3 0 0 48* 0 41 8 70 6 3 -1 2 03 1 90 423 78 6 3 -2 3 36 3 42 230 02 6 3 -3 2 46 2 44 540 91 6 3 -4 0 41* 0 72 17 36 6 4 O 1 51 1 43 325 52 6 4 -1 0 85 0 79 146 35 6 4 -2 2 38 2 42 490 17 6 4 -3 0 35* 0 23 1 1 38 6 4 -4 1 48 1 32 54 1 62 6 5 0 1 35 1 35 298 09 6 5 - 1 3 81 3 74 187 87 6 5 -2 2 91 2 94 391 22 6 5 -3 O 69 0 65 134 50 6 5 -4 0 36* 0 40 18 24 6 6 0 3 23 3 09 264 63 6 6 -1 2 37 2 23 513 99 6 6 -2 2 22 2 19 54 1 01 6 6 -3 0 87 0 80 237 72 6 6 -4 0 54 0 30 195 26 6 7 0 1 63 1 73 421 14 6 7 -1 1 57 1 50 430 37 6 7 -2 O 55* 0 53 95 15 6 7 -3 0 89 1 05 289 24 6 8 0 0 38* 0 14 8 42 6 8 -1 0 82 0 89 196 89 6 8 -2 1 25 1 16 443 79 6 8 -3 0 36* 0 52 . 15 90 6 9 0 1 04 0 94 373 50 6 9 - 1 o 65 0 59 185 45 6 9 -2 0 53* 0 53 54 28 6 10 0 0 30* 0 09 10 85 6 10 - 1 0 29* 0 19 1 1 74 7 0 -1 o 35* 0 15 4 94 h k 1 Fo Fc weight 7 0 -2 1 11 1 15 275 24 7 0 -3 1 73 1 59 520 21 7 0 -4 0 73 0 72 279 37 7 1 0 3 12 3 16 324 95 7 1 - 1 0 77 0 90 127 89 7 1 -2 2 46 2 47 500 09 7 1 -3 0 78 0 70 200 98 7 1 -4 0 26* 0 08 7 92 7 2 0 0 82 0 75 147 72 7 2 - 1 2 51 2 55 477 70 7 2 -2 0 28* O 24 7 50 7 2 -3 1 06 0 96 340 92 7 2 -4 0 77 0 78 355 24 7 3 O 1 76 1 69 4 17 99 7 3 - 1 1 53 1 45 400 01 7 3 -2 1 35 1 40 396 18 7 3 -3 0 57 0 61 120 13 7 4 0 1 80 1 70 445 94 7 4 - 1 0 37* O 47 IO 03 7 4 -2 1 79 1 68 521 01 7 4 -3 0 67 0 75 185 43 7 5 0 1 33 1 27 378 39 7 5 - 1 0 53* O 60 20 36 7 5 -2 1 43 1 34 466 14 7 5 -3 1 05 1 03 422 06 7 6 0 1 57 1 58 474 1 1 7 6 - 1 1 15 1 20 360 37 7 6 -2 0 82 0 91 247 83 7 6 -3 1 20 1 28 602 01 7 7 0 0 33* 0 13 8 64 7 7 - 1 0 73 0 73 215 52 7 7 -2 0 42* 0 36 28 66 7 8 0 0 6 1 0 69 182 76 7 8 - 1 0 30* 0 23 10 84 8 0 0 2 22 2 15 564 90 8 0 - 1 2 4 1 2 34 539 32 8 0 -2 0 88 0 92 287 00 8 0 -3 0 16* 0 OO 6 82 8 1 0 0 94 O 95 246 14 8 1 - 1 1 12 1 05 338 89 8 1 -2 1 07 1 12 384 50 8 1 -3 0 25* O 26 1 1 26 8 2 0 1 07 1 15 295 94 8 2 - 1 0 68 0 65 163 99 8 2 -2 o 93 0 95 340 48 8 3 0 0 36* 0 15 9 66 8 3 - 1 1 17 1 19 402 36 8 3 -2 1 21 1 16 478 85 8 4 0 0 13* 0 08 1 52 h k 1 Fo Fc we 1ght 8 4 -1 1 51 1 53 611 80 pen 8 4 -2 0 72 O 63 285 52 pen 8 5 O 0 32* O 14 20 96 a . ^ . 8 5 -1 1 00 1 03 432 65 H 8 6 0 0 78 0 88 348 44 tn 8 6 - 1 0 44* 0 43 157 70 1 - 1 0 15 60 18 22 0 38 1 - 1 -1 28 1 1 31 67 0 12 1 - 1 -2 1 1 48 1 1 21 18 17 1 - 1 -3 11 37 1 1 10 18 02 1 -1 -4 2 51 2 36 595 79 1 - 1 -5 3 72 3 54 206 29 1 - 1 -6 0 76 0 80 163 64 1 -2 O 22 64 25 87 0 18 1 -2 -1 10 61 10 34 21 46 1 -2 -2 10 97 1 1 08 19 68 1 -2 -3 7 45 7 45 38 29 1 -2 -4 2 36 2 32 560 4 1 1 -2 -5 2 66 2 63 44 1 97 1 -2 -6 1 16 1 15 322 41 1 -3 0 7 61 7 92 40 50 1 -3 -1 16 64 16 93 0 69 1 -3 -2 3 27 3 38 198 61 1 -3 -3 3 17 3 21 269 27 1 -3 -4 4 71 4 57 96 65 1 -3 -5 2 47 2 39 496 83 1 -3 -6 1 04 1 08 295 63 1 -4 0 8 25 8 43 34 14 1 -4 -1 8 10 7 77 34 82 1 -4 -2 10 29 10 16 21 91 1 -4 -3 0 61* 0 64 36 51 1 -4 -4 2 87 2 93 370 51 1 -4 -5 1 99 2 OO 442 95 1 -4 -6 0 40* 0 40 10 82 1 -5 0 8 02 7 91 35 1 1 1 -5 - 1 2 24 2 16 607 73 1 -5 -2 9 26 9 27 26 22 1 -5 -3 4 45 4 32 1 10 07 1 -5 -4 4 63 4 59 97 14 1 -5 -5 0 81 0 76 144 90 1 -5 -6 0 4 1 * O 24 20 62 1 -6 0 1 19 1 12 654 80 1 -6 - 1 7 01 7 04 42 60 1 -6 -2 5 03 4 84 66 09 1 -6 -3 4 91 5 01 93 38 1 -6 -4 0 94 O 97 158 85 1 -6 -5 0 39* O 33 1 1 1 1 1 -6 -6 0 34* 0 34 25 48 1 -7 0 4 29 4 17 124 26 —' h k 1 Fo Fc weight 1 - 7 -1 4 41 4 45 118 75 1 -7 -2 3 47 3 28 194 60 1 -7 -3 2 18 2 09 498 47 1 -7 -4 2 73 2 66 485 87 1 -7 -5 0 89 0 82 216 18 1 -8 0 O 53* 0 30 25 89 1 -8 - 1 3 10 2 88 336 71 1 -8 -2 2 21 2 19 493 29 1 -8 -3 0 61* 0 85 19 20 1 -8 -4 O 39* 0 41 6 57 1 -8 -5 0 84 1 00 244 74 1 -9 0 0 38* 0 19 11 01 1 - 9 -1 2 32 2 19 532 55 1 -9 -2 2 05 1 97 436 69 1 -9 -3 2 13 2 17 453 82 1 -9 -4 1 60 1 60 417 82 1 - 9 -5 0 80 0 89 320 70 1- 10 0 0 36* 0 88 8 32 1- 10 -1 1 41 1 45 299 32 1- 10 -2 2 88 3 04 377 35 1- 10 -3 0 99 0 98 249 94 1- 10 -4 1 37 1 35 481 09 1- 1 1 0 0 39* 0 26 10 29 1- 1 1 -1 2 36 2 43 490 56 1- 1 1 -2 1 89 1 88 499 92 1- 1 1 -3 0 35* 0 08 7 97 1- 1 1 -4 0 63 0 72 240 10 1- 12 0 0 88 0 83 201 62 1- 12 -1 1 01 1 06 251 94 1- 12 -2 1 89 1 93 568 34 1- 12 -3 0 52* 0 45 42 27 1- 13 0 0 96 0 91 322 94 1- 13 -1 1 21 1 32 454 49 1- 13 -2 0 44* O 54 34 14 2 -1 0 16 65 19 33 0 33 2 -1 -1 23 85 25 23 0 16 2 -1 -2 8 41 8 50 31 89 2 - 1 -3 6 21 6 26 50 30 2 -1 -4 2 82 2 72 374 98 2 -1 -5 1 43 1 43 319 36 2 -1 -6 1 00 1 04 279 13 2 -2 O 31 17 36 65 0 10 2 -2 - 1 17 79 18 30 0 51 2 -2 -2 2 28 2 12 689 83 2 -2 -3 5 70 5 79 56 84 2 -2 -4 2 89 2 81 382 88 2 -2 -5 0 97 0 86 196 43 2 -2 -6 0 40* 0 13 1 1 23 2 -3 0 7 30 7 42 42 63 h k 1 Fo Fc we 1ght 2 -3 -1 9 60 9 85 25 46 2 -3 -2 7 84 7 65 35 91 2 -3 -3 3 57 3 63 157 21 2 -3 -4 1 91 1 83 477 04 2 -3 -5 3 28 3 21 284 67 2 -3 -6 0 50* 0 60 27 98 2 -4 0 3 35 3 21 198 49 2 -4 -1 7 23 7 21 41 97 2 -4 -2 7 81 7 00 35 24 2 -4 -3 4 80 4 32 99 27 2 -4 -4 3 51 3 35 247 00 2 -4 -5 1 83 1 84 442 16 2 -4 -6 0 33* 0 33 9 01 2 -5 0 7 40 7 29 39 73 2 -5 - 1 7 64 7 78 37 27 2 -5 -2 2 92 2 86 383 91 2 -5 -3 3 43 3 41 234 00 2 -5 -4 0 67* 0 72 23 30 2 -5 -5 0 40* 0 65 12 62 2 -5 -6 0 30* 0 37 50 14 2 -6 0 0 93 0 88 354 96 2 -6 -1 6 64 6 61 45 77 2 -6 -2 6 22 5 97 48 48 2 -6 -3 3 49 3 35 244 34 2 -6 -4 0 96 0 90 181 58 2 -6 -5 0 61* 0 77 30 4 1 2 -7 0 1 68 1 53 570 40 2 -7 -1 1 59 1 56 523 1 1 2 -7 -2 1 98 1 99 546 70 2 -7 -3 3 66 3 64 187 05 2 -7 -4 2 36 2 39 501 26 2 -7 -5 0 62 0 52 128 7 1 2 -8 0 4 93 4 92 95 46 2 -8 -1 2 17 2 21 562 07 2 -8 -2 2 50 2 60 485 46 2 -8 -3 1 97 1 99 425 64 2 -8 -4 1 87 1 90 480 54 2 -8 -5 0 33* 0 35 9 07 2 -9 0 0 33* 0 41 4 02 2 -9 -1 2 72 2 70 453 37 2 -9 -2 3 57 3 60 207 55 2 -9 -3 1 85 1 74 450 18 2 -9 -4 0 76 0 74 •172 86 2- 10 0 5 66 5 57 60 83 2- 10 -1 1 32 1 18 304 82 2- 10 -2 1 41 1 45 329 08 2- 10 -3 1 04 1 14 250 4 1 2- 10 -4 0 48* 0 47 31 21 2- 1 1 0 1 79 1 76 454 67 h k l Fo Fc weight 2- 1 1 - 1 0 35* 0 58 5 30 2- 1 1 -2 0 82 0 88 182 84 2- 1 1 -3 0 29* 0 10 9 56 2- 12 0 1 1 1 1 06 299 64 2- 12 - 1 1 40 1 43 435 7 1 2- 12 -2 0 36* 0 47 53 48 2- 12 -3 o 26* 0 24 15 13 2- 13 0 0 32* 0 46 9 59 2- 13 - 1 0 93 1 04 340 94 2- 13 -2 0 32* 0 4 1 26 07 3 - 1 0 9 17 9 65 27 78 3 - 1 - 1 3 50 3 49 185 22 3 - 1 -2 3 55 3 43 159 95 3 - 1 -3 2 20 2 27 540 68 3 - 1 -4 4 47 4 40 1 15 28 3 - 1 -5 2 51 2 51 516 28 3 - 1 -6 0 76 0 79 230 70 3 -2 0 12 58 13 18 15 19 3 -2 - 1 3 30 3 39 189 83 3 -2 -2 13 85 13 96 12 44 3 -2 -3 2 80 2 31 387 97 3 -2 -4 2 45 2 46 476 08 3 -2 -5 O 36* O 42 9 00 3 -2 -6 O 40* 0 66 19 89 3 -3 0 5 86 5 62 59 27 3 -3 - 1 15 07 15 44 10 64 3 -3 -2 3 59 3 53 172 91 3 -3 -3 3 16 3 10 312 64 3 -3 -4 4 43 4 34 ioo 25 3 -3 -5 O 39* O 14 6 44 3 -3 -6 0 53 0 61 130 54 3 -4 0 3 60 3 70 163 72 3 -4 - 1 2 67 2 62 402 35 3 -4 -2 7 56 7 22 36 49 3 -4 -3 1 01 1 06 214 19 3 -4 -4 1 89 1 75 420 74 3 -4 -5 0 30* 0 09 7 08 3 -4 -6 0 69 0 67 280 54 3 -5 0 8 03 7 78 33 65 3 -5 - 1 4 03 3 78 132 51 3 -5 -2 3 58 3 45 198 44 3 -5 -3 4 75 4 47 95 42 3 -5 -4 2 73 2 66 439 44 3 -5 -5 1 36 1 26 380 95 3 -6 0 0 42* 0 51 18 46 3 -6 - 1 4 4 1 4 27 1 12 81 3 -6 -2 3 69 3 51 183 38 3 -6 -3 0 38* 0 44 9 34 3 -6 -4 3 34 3 1 1 267 07 h k 1 Fo Fc weight ts 3 -6 -5 0 26* 0 48 24 36 ts n> 3 -7 0 1 17 1 01 340 13 3 3 -7 - 1 1 31 1 20 365 52 a , . 3 -7 -2 1 19 1 28 291 74 H 3 -7 -3 4 71 4 70 92 85 to 3 -7 -4 0 91 0 95 201 17 3 -7 -5 0 45* 0 46 25 34 3 -8 0 4 35 4 45 1 19 41 3 -8 - 1 0 46* 0 49 7 56 3 -8 -2 2 17 2 06 463 88 3 -8 -3 2 77 2 73 456 55 3 -8 -4 O 20* O 13 12 77 3 -8 -5 0 69 O 59 281 76 3 -9 0 0 96 1 07 173 68 3 -9 - 1 3 86 3 96 185 12 3 -9 -2 2 58 2 57 495 79 3 -9 -3 1 58 1 59 436 31 3 -9 -4 0 60 0 45 156 95 3- 10 0 2 01 2 27 448 00 3- 10 - 1 2 03 2 05 451 50 3- 10 -2 0 83 0 92 166 19 3- 10 -3 0 71 0 67 170 65 3- 10 -4 O 37* O 20 91 23 3- 1 1 0 0 38* 0 32 7 09 3- 1 1 - 1 1 01 0 96 280 71 3- 1 1 -2 0 69 0 79 163 47 3- 1 1 -3 0 36* 0 33 22 33 3- 12 0 0 31* 0 1 1 6 92 3- 12 -1 0 56* 0 69 33 82 3- 12 -2 O 65 0 63 200 57 3- 13 0 0 29* 0 31 1 1 56 3- 13 - 1 0 66 0 70 282 70 4 - 1 0 1 72 1 60 805 22 4 - 1 -1 1 33 1 23 616 61 4 -1 -2 3 94 4 02 129 97 4 - 1 -3 3 61 3 60 204 04 4 - 1 -4 3 1 1 3 06 314 59 4 - 1 -5 1 39 1 38 371 85 4 - 1 -6 0 69 0 81 269 33 4 -2 0 5 09 5 14 69 75 4 -2 - 1 6 01 6 09 53 71 4 -2 -2 2 48 2 30 624 10 4 -2 -3 1 76 1 85 457 85 4 -2 -4 2 45 2 38 473 91 4 -2 -5 O 74 0 86 146 08 4 -3 0 5 80 6 01 56 86 4 -3 - 1 7 58 7 78 36 68 4 -3 -2 3 06 2 94 279 61 OO 4 -3 -3 0 79 0 72 152 77 1 h k 1 Fo Fc weIght h k 1 Fo Fc weight h k 1 Fo Fc weIght h k 1 Fo Fc weight 4 -3 -4 1 65 1 55 401 02 5 -1 -4 1 51 1 44 375 64 5- 1 1 - 1 0 30* 0 46 19 1 1 7 -2 0 0 75 0 75 1 19 14 "tJ nj 4 -3 -5 0 74 0 64 155 53 5 -1 -5 0 38* 0 42 17 56 6 -1 0 O 63 O 81 96 16 7 -2 - 1 2 53 2 55 512 15 3 4 -4 0 4 87 4 73 69 57 5 -2 0 4 36 4 36 111 82 6 -1 - 1 2 50 2 47 538 58 7 -2 -2 0 30* 0 24 8 12 ft. r* -4 -4 -1 1 1 08 11 12 18 62 5 -2 -1 5 72 5 66 53 63 6 -1 -2 1 36 1 31 285 64 7 -2 -3 1 00 0 96 305 58 H 4 -4 -2 8 71 8 55 27 94 5 -2 -2 2 35 2 34 501 01 6 -1 -3 1 64 1 73 396 50 7 -2 -4 0 80 0 78 385 10 ba 4 -4 -3 3 20 3 28 298 33 5 -2 -3 0 64 0 54 89 79 6 -1 -4 O 56* 0 56 100 63 7 -3 0 1 71 1 69 409 62 4 -4 -4 0 57* 0 60 19 93 5 -2 -4 0 77 0 78 139 84 6 -2 0 2 22 2 27 506 23 7 -3 - 1 1 44 1 45 361 23 4 -4 -5 O 35* O 08 7 37 5 -2 -5 0 35* 0 23 16 60 6 -2 - 1 3 44 3 26 238 59 7 -3 -2 1 30 1 40 393 27 4 -5 0 1 70 1 69 553 05 5 -3 0 5 07 4 92 62 49 6 -2 -2 1 50 1 35 349 83 7 -3 -3 0 28* 0 61 5 49 4 -5 -1 2 93 3 01 324 11 5 -3 -1 2 68 2 75 513 35 6 -2 -3 1 00 0 93 221 33 7 -4 0 1 80 1 70 461 21 4 -5 -2 3 89 3 82 154 22 5 -3 -2 2 81 2 87 415 27 6 -2 -4 0 23* 0 10 3 92 7 -4 - 1 0 38* 0 47 6 07 4 -5 -3 1 48 1 38 332 49 5 -3 -3 2 96 2 71 369 38 6 -3 0 0 43* O 4 1 12 31 7 -4 -2 1 68 1 68 444 99 4 -5 -4 1 37 1 19 328 38 5 -3 -4 1 72 1 71 449 14 6 -3 - 1 1 98 1 90 4 18 52 7 -4 -3 0 65 0 75 168 26 4 -5 -5 0 59 O 63 129 75 5 -3 -5 0 83 0 89 267 95 6 -3 -2 3 37 3 42 231 89 7 -5 0 1 23 1 27 337 48 4 -6 0 1 69 1 73 489 00 5 -4 0 1 95 1 92 528 36 6 -3 -3 2 45 2 44 499 59 7 -5 - 1 0 69* 0 60 37 16 4 -6 -1 1 17 1 26 304 62 5 -4 -1 3 48 3 43 200 28 6 -3 -4 0 72 0 72 178 80 7 -5 -2 1 27 1 34 383 50 4 -6 -2 1 62 1 71 393 63 5 -4 -2 1 25 1 30 301 80 6 -4 0 1 42 1 43 316 29 7 -5 -3 0 95 1 03 359 37 4 -6 -3 2 45 2 66 462 81 5 -4 -3 2 49 2 59 458 71 6 -4 - 1 0 82 0 79 125 86 7 -6 0 1 50 1 58 436 35 4 -6 -4 1 36 1 SO 377 17 5 -4 -4 0 74 O 48 164 04 6 -4 -2 2 32 2 42 484 34 7 -6 -1 1 13 1 20 345 37 4 -6 -5 0 58* O 59 49 02 5 -4 -5 0 37* 0 28 14 39 6 -4 -3 O 42* 0 23 9 29 7 -6 -2 0 77 0 91 228 40 4 -7 0 4 08 3 90 145 78 5 -5 0 1 91 2 02 463 21 6 -4 -4 1 45 1 32 539 34 7 -6 -3 1 16 1 28 587 52 4 -7 -1 4 18 4 29 159 39 5 -5 -1 1 69 1 77 424 98 6 -5 0 1 33 1 35 305 10 7 -7 0 O 34* 0 13 8 45 4 -7 -2 4 26 4 30 115 73 5 -5 -2 2 40 2 55 466 91 6 -5 - 1 3 67 3 74 169 81 7 -7 - 1 O 73 0 73 224 63 4 -7 -3 1 00 1 00 198 95 5 -5 -3 3 70 3 75 165 69 6 -5 -2 2 83 2 94 408 71 7 -7 -2 0 46* 0 36 120 51 4 -7 -4 0 64 0 60 130 43 5 -5 -4 1 39 1 53 392 17 6 -5 -3 0 59* 0 65 97 04 7 -8 0 0 57* 0 69 56 32 4 -7 -5 0 61 0 59 239 71 5 -5 -5 0 60* 0 71 71 97 6 -5 -4 0 24* 0 40 5 67 7 -8 - 1 0 33* 0 23 13 30 4 -8 0 4 23 4 27 1 17 93 5 -6 0 0 68* 0 88 24 47 6 -6 0 3 16 3 09 290 00 8 - 1 0 0 89 0 95 219 59 4 -8 -1 1 30 i 29 269 60 5 -6 - 1 1 85 1 84 422 45 6 -6 - 1 2 32 2 23 500 41 8 - 1 -1 1 13 1 05 357 19 4 -8 -2 1 33 1 43 280 98 5 -6 -2 3 38 3 37 316 15 6 -6 -2 2 12 2 19 519 73 8 -1 -2 1 01 1 12 364 22 4 -8 -3 1 82 1 95 474 44 5 -6 -3 2 27 2 21 515 82 6 -6 -3 0 85 0 80 234 75 8 - 1 -3 0 20* o 26 1 1 79 4 -8 -4 0 31* 0 21 7 OO 5 -6 -4 1 34 1 22 440 46 6 -6 -4 0 47* 0 30 52 23 8 -2 O 1 05 1 15 293 12 4 -9 O 2 07 2 22 473 86 5 -7 0 2 47 2 22 470 91 6 -7 0 1 6 1 1 73 4 36 74 8 -2 - 1 o 62* o 65 37 81 4 -9 -1 1 36 1 51 316 57 5 -7 -1 1 58 1 55 362 58 6 -7 -1 1 47 1 50 392 13 8 -2 -2 0 94 0 95 345 22 4 -9 -2 0 51* 0 72 17 82 5 -7 -2 2 18 2 23 478 12 6 -7 -2 0 42* 0 53 15 44 8 -3 0 o 31* 0 15 6 74 4 -9 -3 0 50* 0 62 83 50 5 -7 -3 1 36 1 20 360 55 6 -7 -3 0 88 1 05 290 66 8 -3 - 1 1 15 1 19 399 27 4 -9 -4 0 26* 0 47 13 22 5 -7 -4 0 97 0 94 348 03 6 -8 0 0 41* 0 14 1 1 00 8 -3 -2 1 15 1 16 458 38 4- 10 0 1 01 1 05 241 89 5 -8 0 2 74 3 01 373 75 6 -8 - 1 0 75 0 89 159 29 8 -4 0 0 39* 0 08 13 07 4- 10 -1 1 23 1 26 333 44 5 -8 -1 1 99 2 07 463 40 6 -8 -2 1 19 1 16 423 32 8 -4 -1 1 51 1 53 600 31 4- 10 -2 0 72 o 63 161 38 5 -8 -2 0 35* 0 43 5 98 6 -8 -3 0 40* 0 52 30 55 8 -4 -2 0 76 0 63 311 26 4- 10 -3 0 35* 0 35 59 92 5 -8 -3 0 85 0 93 210 86 6 -9 0 0 92 0 94 284 70 8 -5 0 0 30* 0 14 15 00 4- 1 1 0 0 65* 0 66 33 95 5 -8 -4 0 95 0 90 485 16 6 -9 - 1 0 30* 0 59 1 1 77 8 -5 - 1 0 96 1 03 396 49 4 - 1 1 -1 o 93 0 93 260 83 5 -9 0 2 16 2 22 526 51 6 -9 -2 0 33* 0 53 19 08 8 -6 O 0 70 0 88 304 30 4 - 1 1 -2 0 32* 0 32 8 84 5 -9 -1 O 74 0 87 163 28 6- 10 0 0 31* 0 09 10 71 8 -6 - 1 0 43* 0 43 142 83 4 - 12 O 0 45* 0 49 32 00 5 -9 -2 0 95 1 02 27 1 19 6- 10 - 1 0 23* 0 19 7 53 0 0 -2 15 51 17 34 10 19 4 - 12 -1 0 55 0 58 169 56 5 -9 -3 0 57 0 71 163 02 7 - 1 0 3 08 3 16 304 28 O 0 -4 3 39 3 40 267 31 5 -1 O 0 18* o OO 2 72 5- 10 O 1 04 1 00 303 43 7 - 1 - 1 O 84 O 90 153 34 0 0 -6 1 95 1 92 519 19 5 -1 -1 5 38 5 54 58 49 5- 10 - 1 0 48* 0 52 24 21 7 - 1 -2 2 51 2 47 522 09 5 -1 -2 1 07 1 03 256 16 5- 10 -2 0 77 0 77 257 47 7 - 1 -3 0 56* 0 70 29 20 977 r e f 1 e c t i ons OO 5 -1 -3 3 27 3 40 280 81 5- 1 1 0 0 31* 0 32 10 12 7 - 1 -4 0 31* 0 08 12 57 Appendix C Structure Factors for Maleic Anhydride at 104K 83 h k 1 Fc weight h k 1 Fo Fc weight h k 1 Fo Fc we 1ght h k 1 Fo Fc weight 2 0 0 2 4 9 9 2 0 6 9 3 2 8 5 6 0 1 9 7 * 2 8 0 0 3 6 2 1 0 1 4 5 3 3 9 6 9 6 9 2 3 1 2 1 5 5 18 2 3 3 5 6 4 0 0 3 2 1 9 2 9 5 9 1 8 5 6 6 0 1 0 6 6 1 0 2 8 2 0 2 2 1 1 0 1 6 9 1 6 8 9 1 5 18 3 3 1 3 4 9 9 3 0 2 8 1 6 4 6 0 0 14 7 3 1 3 2 5 17 12 7 6 0 7 4 7 7 6 5 12 6 3 0 1 0 1 5 8 6 5 0 1 1 3 7 4 4 3 1 1 7 6 1 16 3 2 8 4 3 8 O o 8 1 8 7 9 5 1 2 9 0 7 7 o 2 1 8 * 0 4 6 0 4 5 0 9 1 2 3 2 * 2 8 5 0 4 3 5 3 1 8 4 0 7 7 7 2 4 6 0 8 1 0 3 1 5 * 5 2 3 0 3 9 6 7 0 2 3 9 * 1 9 3 0 4 3 1 9 1 9 12 8 8 3 2 2 7 0 6 3 1 7 5 3 7 8 8 17 1 0 7 1 0 1 2 2 8 12 14 2 0 8 7 5 7 0 7 8 6 7 2 5 17 0 2 2 9 1 9 7 8 8 9 1 2 1 5 7 7 3 1 4 0 1 3 6 9 7 4 3 6 1 0 1 5 7 * 1 0 5 0 2 8 4 7 0 12 9 8 1 1 8 6 16 9 5 3 9 1 1 3 17 1 0 8 9 18 3 4 8 3 1 5 8 5 6 4 1 9 2 3 5 1 0 1 6 8 * 2 0 1 0 3 5 3 7 0 1 7 9 * 2 12 0 3 0 4 9 1 3 9 1 3 19 7 5 6 8 2 1 2 0 4 * 3 0 3 0 2 4 4 1 0 4 3 4 3 18 2 4 1 7 2 7 0 1 6 1 * 0 0 6 0 3 9 5 9 1 2 9 9 * 2 6 7 3 18 7 2 1 7 0 6 7 2 8 1 5 4 0 3 1 0 2 0 8 4 1 7 8 2 3 6 9 1 7 0 9 0 4 9 4 3 2 7 9 3 6 8 1 4 14 3 3 3 5 9 1 6 2 1 12 3 9 12 0 4 2 0 6 1 2 1 0 3 3 6 4 2 8 8 7 1 9 5 0 8 0 1 5 5 4 1 9 8 1 1 1 9 6 5 8 1 5 9 4 5 4 0 12 2 4 5 2 1 1 5 4 7 14 6 2 1 1 9 7 1 1 o 3 0 8 7 2 5 3 5 2 4 4 1 8 o 4 4 4 5 2 2 14 5 5 4 8 1 7 0 2 6 2 9 16 9 5 4 2 1 1 5 6 6 14 2 1 9 5 9 0 2 o 8 9 0 7 8 3 2 9 0 0 2 8 0 1 0 8 9 1 0 6 8 2 7 7 8 3 8 1 1 9 3 * 0 7 8 0 4 6 3 2 1 6 8 3 5 3 7 3 9 0 5 1 2 o 4 3 4 2 3 6 6 3 1 2 6 3 8 0 1 1 7 1 1 3 0 8 19 9 0 2 8 1 7 9 4 8 3 4 2 0 6 2 2 2 1 3 9 5 1 3 3 4 5 1 4 3 2 2 o 6 6 5 5 5 8 9 4 0 5 4 4 8 0 12 3 8 14 5 8 2 0 5 9 1 8 1 5 4 5 4 8 9 17 0 7 1 2 1 18 0 0 14 2 1 5 3 0 3 2 0 2 9 6 6 2 5 8 8 2 2 3 5 8 o 7 7 9 8 5 4 17 3 7 0 8 1 1 1 7 4 IO 4 0 2 3 9 7 O 2 1 3 2 0 6 2 5 0 6 2 1 8 4 2 0 9 5 6 8 0 9 3 5 3 7 6 8 0 2 3 0 * 0 4 4 0 3 8 0 7 1 12 12 1 0 3 5 2 0 17 0 1 1 2 9 4 2 2 2 7 6 2 6 2 5 2 0 1 0 9 1 1 0 0 9 2 6 5 0 6 9 0 3 9 1 4 8 5 4 6 6 1 7 1 12 1 5 1 1 0 8 2 3 1 9 1 1 1 5 5 9 7 4 8 3 5 0 7 7 6 2 0 7 7 8 8 3 4 2 0 8 3 5 9 0 7 3 5 7 8 1 14 2 8 2 7 1 4 18 4 4 5 14 0 5 2 1 1 4 9 8 1 4 2 1 0 0 9 4 7 2 0 5 6 4 6 0 8 1 1 9 0 4 9 0 4 12 3 7 5 9 5 9 3 7 1 2 2 3 * 1 6 3 0 4 3 3 1 1 8 4 9 7 7 1 4 4 6 6 8 2 0 4 5 0 4 6 0 7 1 9 3 9 0 2 6 5 * 3 7 1 4 1 9 4 7 1 14 0 8 12 8 2 16 6 7 4 1 1 2 8 3 2 5 4 1 1 3 2 8 3 0 4 12 3 8 5 6 5 4 2 9 0 1 1 1* 2 8 3 0 1 0 5 7 1 5 7 5 5 5 2 12 7 3 5 1 1 16 1 1 1 5 3 8 1 1 8 2 7 3 0 7 2 6 7 1 1 1 5 6 4 1 9 0 2 4 3 * 2 7 0 4 17 6 7 1 6 4 3 6 16 1 1 0 9 6 1 1 5 17 4 7 3 1 3 2 5 6 3 0 1 7 3 * 0 4 7 0 3 4 0 1 0 0 1 8 4 * 0 9 2 0 3 0 7 6 1 3 9 6 3 3 4 5 6 5 7 1 1 O 8 8 * 2 1 0 0 0 6 5 3 0 1 3 4 8 12 5 7 1 6 5 6 1 1 0 0 5 0 9 4 2 1 1 3 0 7 6 6 1 1 0 1 3 9 8 7 1 9 1 1 8 1 1 5 2 2 4 8 7 8 5 9 4 3 0 14 9 5 1 3 7 8 1 2 2 4 2 1 0 0 19 7 0 1 9 7 3 6 2 4 5 6 1 4 4 7 3 5 5 1 1 8 0 8 0 1 1 1 1 5 1 1 5 6 1 5 5 2 3 3 0 1 2 8 4 11 3 8 1 9 9 8 3 1 0 0 4 7 8 5 16 9 9 3 4 6 1 2 1 4 * 1 9 2 0 4 6 7 0 1 1 8 4 * 0 0 2 0 3 0 2 3 0 1 0 6 5 7 8 0 2 4 2 6 4 1 0 0 2 8 9 * 4 4 3 3 6 6 3 6 1 1 0 0 1 8 0 5 2 6 5 1 6 0 1 6 9 1 6 3 6 1 9 0 7 1. 3 0 1 0 9 9 9 4 2 2 4 5 9 5 1 0 0 5 0 4 5 2 1 8 0 5 2 6 1 17 5 2 1 5 7 6 8 8 8 5 0 1 1 0 7 * 1 7 9 1 2 1 0 4 0 4 2 4 5 2 9 3 8 9 5 4 11 0 2 1 4 * 2 0 5 0 2 2 1 6 1 1 9 12 1 5 6 8 7 16 4 0 1 6 6 8 6 OO 3 1 0 5 1 4 0 2 0 6 9 17 3 8 3 9 1 3 11 0 0 9 2 * 1 7 7 0 0 7 0 6 1 1 5 9 6 1 5 0 9 1 0 6 2 3 0 1 9 7 3 7 6 1 3 5 2 6 2 4 o 7 0 8 8 9 7 4 1 4 5 2 11 0 5 7 4 5 9 8 12 1 1 0 5 1 12 5 4 12 0 3 16 0 4 2 0 1 3 0 9 4 2 6 9 1 2 2 2 3 4 0 6 9 8 5 8 5 3 3 4 1 1 11 0 1 9 2 * 1 0 6 0 2 7 1 5 1 5 7 2 4 3 0 3 5 7 5 1 0 1 3 1 2 5 2 6 2 0 2 3 1 4 4 0 1 1 14 1 0 2 8 3 0 6 8 0 1 2 0 1 0 2 2 1 0 4 8 1 5 5 9 2 5 1 1 6 7 5 14 6 5 7 8 2 0 0 2 3 0 7 0 2 5 3 9 2 2 1 5 4 o 9 6 0 8 8 7 2 5 5 8 1 12 0 4 0 9 4 5 4 6 3 1 3 5 1 7 2 1 5 4 7 2 8 9 4 1 0 2 2 6 16 2 2 4 2 2 8 1 6 4 0 5 1 0 4 9 7 12 5 8 2 1 2 0 5 6 5 5 8 9 9 3 6 4 5 1 8 9 5 8 5 2 2 6 0 5 2 0 2 5 2 5 5 3 3 3 4 4 9 7 4 0 6 3 1 6 14 1 5 9 9 3 1 2 0 1 5 9 * 1 4 0 1 0 6 5 5 4 0 0 4 3 0 9 0 2 3 0 2 2 1 2 6 18 9 6 4 8 4 7 5 0 5 2 9 5 2 6 9 7 5 3 12 1 2 5 8 * 3 2 3 0 2 6 6 5 14 5 2 14 0 7 1 3 3 8 4 0 2 1 7 2 * 3 1 6 0 3 4 6 5 o 6 0 7 6 4 7 12 7 4 2 12 1 5 2 8 6 3 8 8 5 5 7 5 3 9 8 3 9 4 5 9 9 5 0 2 1 9 9 * 2 9 6 0 4 8 5 5 0 4 0 8 4 0 8 1 0 6 8 1 1 2 1 2 9 1 * 2 9 1 3 7 7 7 4 1 2 0 5 * 2 14 0 2 4 6 0 2 4 2 1 4 17 9 9 5 4 5 0 1 5 9 * 1 5 1 0 4 0 0 12 1 3 3 5 4 2 0 4 12 6 4 2 0 9 * 2 9 1 2 9 6 7 0 2 1 1 4 * 0 3 2 O 7 7 3 5 0 2 0 3 3 1 8 4 1 4 8 7 0 1 1 1 16 0 1 19 5 0 12 8 9 5 4 1 9 3 6 8 7 8 2 2 7 1 7 1 2 1 1 2 6 11 1 1 18 0 4 2 5 o 1 5 7 4 1 3 5 7 8 9 0 1 1 1 1 5 9 9 7 19 12 0 4 4 4 2 8 9 7 2 5 6 4 2 0 5 6 1 2 6 OI 5 3 1 1 6 2 5 1 5 0 1 9 6 8 1 5 4 9 5 7 0 2 1 1 1 2 3 8 * 2 9 7 0 3 8 3 4 5 12 3 9 2 2 3 6 0 5 1 2 4 9 3 4 4 2 14 2 4 0 6 0 0 8 2 * 2 9 1 1 1 6 3 1 1 1 4 0 7 4 2 3 6 9 8 2 4 1 2 5 3 1 0 3 2 1 5 4 1 4 1 2 1 2 6 3 12 0 8 1 9 5 2 1 6 0 3 6 7 4 6 2 18 7 7 4 1 1 1 5 8 6 5 2 9 1 0 0 3 1 4 16 17 13 4 8 7 2 1 3 1 2 8 4 4 7 7 0 3 5 7 6 2 6 0 1 6 0 * 3 0 5 0 3 9 5 1 0 1 2 6 8 * 2 8 2 2 9 3 0 4 1 2 3 1 0 1 9 7 6 3 2 9 2 1 2 18 5 0 1 5 5 1 6 2 8 3 6 0 0 6 9 * 0 11 0 0 7 4 1 0 1 2 9 0 * 3 5 3 0 3 8 0 3 1 5 19 1 1 2 6 8 8 6 1 1 2 2 2 1 0 18 6 6 3 5 3 4 6 o 6 1 9 4 12 1 9 7 0 3 1 0 1 6 8 0 6 8 7 14 19 1 3 3 1 7 1 2 6 6 6 2 0 9 0 1 2 3 8 8 5 3 2 9 6 1 4 7 h k 1 FO Fc weight 0 2 2 21 86 18 26 3 61 1 2 2 23 56 19 38 3 15 2 2 2 1 39* 1 03 3 13 3 2 2 31 30 27 34 1 91 4 2 2 5 63 4 59 22 02 5 2 2 3 86 3 33 9 55 6 2 2 4 43 4 30 10 29 7 2 2 2 07* 1 80 0 23 7 3 2 3 76 4 29 5 61 6 3 2 1 1 95 11 53 20 64 5 3 2 7 76 7 81 18 74 4 3 2 8 28 7 64 25 76 3 3 2 12 71 11 96 21 01 2 3 2 16 85 14 41 8 1 1 1 3 2 7 88 7 71 41 12 0 3 2 18 50 15 27 6 26 0 4 2 1 1 71 9 97 19 85 1 4 2 23 50 19 32 2 94 2 4 2 16 21 13 88 9 67 3 4 2 17 04 14 98 8 31 4 4 2 24 29 22 58 3 47 5 4 2 5 97 4 58 16 47 6 4 2 8 00 7 87 17 34 7 4 2 7 41 7 66 12 79 7 5 2 5 56 5 44 8 44 6 5 2 10 70 10 74 18 88 5 5 2 7 80 8 07 18 26 4 5 2 9 96 9 73 23 08 3 5 2 7 81 6 64 25 19 2 5 2 9 74 7 75 29 80 1 5 2 22 67 19 09 4 30 0 5 2 2 40 0 61 7 85 0 6 2 2 71 2 55 7 46 1 6 2 11 89 9 79 30 32 2 e 2 17 51 15 18 8 27 3 6 2 9 20 8 66 24 57 4 6 2 5 25 5 36 12 36 5 6 2 1 1 37 1 1 10 20 82 6 6 2 1 1 43 1 1 16 16 29 6 7 2 1 91* 1 84 0 27 5 7 2 6 34 6 14 12 44 4 7 2 15 93 14 79. 11 44 3 7 2 2 84 2 53 5 54 2 7 2 6 17 6 21 17 44 1 7 2 6 71 4 95 20 26 0 7 2 9 70 8 91 25 86 0 8 2 1 1 30 10 46 25 04 1 8 2 9 08 8 63 24 23 2 8 2 7 19 6 48 17 40 h k 1 Fo Fc •weight 3 8 2 7 71 8 79 17 68 4 8 2 5 10 4 70 10 17 5 8 2 3 1 1 2 93 3 80 6 8 2 5 50 5 27 7 72 5 9 2 3 67 3 96 4 29 4 9 2 4 94 5 31 9 65 3 9 2 5 05 4 88 10 44 2 9 2 14 86 14 25 15 06 1 9 2 4 06 3 71 8 80 0 9 2 10 36 1 1 34 21 57 0 10 2 1 89* 0 61 0 28 1 10 2 12 98 12 15 20 62 2 10 2 2 64* 4 53 0 42 3 10 2 3 85 3 25 7 24 4 10 2 4 18 4 25 6 13 3 11 2 2 55* 3 26 2 20 2 11 2 2 87* 4 19 2 83 1 11 2 5 35 5 71 8 78 0 11 2 2 01* 2 01 2 09 0 12 2 2 70* 1 57 0 36 1 12 2 10 1 1 9 72 13 40 2 12 2 2 27* 0 66 0 19 0 11 3 5 87 6 29 8 94 1 1 1 3 1 29* 1 08 0 60 2 1 1 3 2 08* 1 64 0 23 3 10 3 6 06 5 22 10 46 2 10 3 2 46* 2 57 0 36 1 10 3 2 41* 4 75 0 25 0 10 3 3 79 3 31 6 57 0 9 3 12 21 12 34 20 88 1 9 3 7 20 7 48 15 15 2 9 3 5 53 5 31 9 90 3 9 3 7 14 7 03 13 OO 4 9 3 0 95* 2 79 0 05 5 8 3 5 10 5 13 8 69 4 8 3 5 61 5 59 9 61 3 8 3 1 1 27 11 18 19 62 2 8 3 6 20 5 90 13 52 1 8 3 6 42 5 92 14 75 0 8 3 13 32 1 1 19 19 88 0 7 3 3 19 2 37 6 24 1 7 3 8 50 7 93 19 90 2 7 3 13 08 14 76 14 69 3 7 3 13 84 12 64 21 51 4 7 3 7 22 6 87 15 13 5 7 3 6 72 6 55 12 35 6 6 3 5 34 5 46 7 38 5 6 3 8 58 B 55 16 1 1 4 6 3 7 83 7 48 17 40 h k 1 Fo Fc weight 3 6 3 6 36 6 22 15 51 2 6 3 9 54 8 83 21 73 1 6 3 15 64 14 01 11 56 0 6 3 9 69 10 16 23 91 0 5 3 7 08 3 36 23 42 1 5 3 9 48 8 05 26 23 2 5 3 1 1 05 10 67 25 98 3 5 3 14 56 13 97 16 97 4 5 3 3 97 4 82 8 27 5 5 3 12 94 12 62 20 58 6 5 3 4 86 5 47 7 05 6 4 3 1 59* 1 73 0 19 5 4 3 9 74 9 75 19 27 4 4 3 10 49 IO 38 23 21 3 4 3 2 48* 3 53 0 53 2 4 3 1 1 50 10 03 19 81 1 4 3 3 75 4 25 10 70 0 4 3 12 77 1 1 29 21 54 0 3 3 33 30 29 47 1 7 1 1 3 3 8 18 7 19 31 45 2 3 3 8 26 7 03 27 06 3 3 3 9 83 8 38 25 91 4 3 3 4 64 4 63 1 1 88 5 3 3 8 57 8 86 18 03 6 3 3 6 95 6 93 14 78 7 3 3 2 74* 2 89 0 35 7 2 3 2 54* 5 45 O 29 6 2 3 1 54* 2 86 0 24 5 2 3 3 26 3 36 5 85 4 2 3 4 75 4 43 12 44 3 2 3 8 25 7 99 25 73 2 2 3 17 51 16 21 8 91 1 2 3 18 58 16 40 7 17 0 2 3 4 03 2 82 17 21 0 1 3 1 51* 3 86 0 44 1 1 3 23 29 19 35 4 22 2 1 3 16 12 15 78 1 1 69 3 1 3 4 99 5 03 16 27 4 1 3 7 92 9 06 23 31 10 0 0 2 61* 1 28 0 55 10 1 0 8 7 1 9 42 13 14 9 1 0 1 91* 1 98 0 27 9 2 0 6 29 6 55 1 1 75 10 2 0 2 04* 1 10 0 24 10 3 0 2 96* 3 25 0 37 9 3 0 4 7 1 5 19 8 7 1 8 4 0 1 78* 1 84 0 32 9 4 0 1 76* 0 78 0 32 10 4 0 2 05* 0 09 0 24 h k 1 Fo Fc weight T3 10 5 0 2 62* 1 33 3 17 "a 9 5 0 1 33* 1 10 0 21 3 8 5 0 4 34 4 27 9 73 8 6 0 5 72 5 75 10 70 H 9 6 0 2 02* 1 51 0 25 9 7 0 1 29* 2 57 0 60 8 7 0 1 81* 1 52 0 26 7 8 0 O 87* 1 92 O OS 8 8 0 3 93 4 01 5 05 9 8 0 3 07* 3 76 3 19 8 9 0 2 00* 0 81 0 25 7 9 0 4 1 1 4 37 7 13 6 10 0 1 94* 1 46 0 27 7 10 0 1 20* 0 13 0 70 8 10 O 1 97* 3 28 0 17 7 1 1 0 1 88* 0 35 1 89 6 1 1 0 3 23 3 49 4 47 5 1 1 O 1 84* 0 61 0 30 4 12 O 1 87* 3 07 0 28 5 12 0 2 02* O 92 0 30 6 12 0 5 52 5 23 8 1 1 7 12 o O 99* 2 08 0 06 6 13 0 5 98 5 92 8 04 5 13 0 3 37 3 29 4 26 4 13 0 8 22 8 06 16 47 3 13 0 2 15* 1 26 0 58 2 13 0 1 99* 3 36 0 25 1 13 0 2 82 2 32 5 31 0 14 0 1 96* 0 37 0 26 1 14 0 2 18* 2 07 0 50 2 14 0 2 39* 2 OO 0 35 3 14 0 6 92 5 89 1 1 1 1 4 14 o 3 39 2 47 4 86 5 14 o 2 33* 4 02 0 18 4 15 0 3 50 3 67 3 35 3 15 0 2 16* 3 06 0 28 2 15 0 1 85* 0 09 0 29 1 15 0 2 16* 1 44 0 22 0 16 0 2 06* 1 50 0 24 1 16 0 2 14* 0 29 O 22 2 16 0 2 14* 0 56 0 22 2 16 1 1 30* 2 20 0 59 1 16 1 O 67* 0 05 0 19 0 16 1 2 41* 1 95 2 16 0 15 1 0 82* 2 61 0 28 1 15 1 1 74* 1 78 1 1 1 2 15 1 2 10* 3 31 0 23 3 15 1 2 38* 1 57 0 53 oo 4 15 1 6 18 5 53 8 87 Ol h k 1 Fo Fc weight h k 1 Fo Fc we 1ght h k 1 Fo Fc we 1ght h k 1 Fo Fc weight 5 14 1 0 99* 3 39 0 06 9 0 2 1 77* 0 51 0 32 3 14 2 5 02 3 93 8 46 7 6 3 8 51 8 16 16 48 4 14 1 2 37* 1 44 2 68 10 O 2 2 31* 2 86 2 31 4 14 2 1 96* O 51 0 24 7 5 3 5 27 5 69 9 84 3 14 1 2 01* 0 52 0 25 10 1 2 2 06* 2 19 0 24 5 14 2 2 14* 2 08 0 22 8 5 3 4 42 4 62 6 23 2 14 1 3 23 2 28 4 68 9 1 2 2 75* 3 03 0 38 3 15 2 1 85* 0 49 0 29 9 5 3 3 03* 3 16 0 41 1 14 1 1 56* 1 31 0 IB 8 1 2 4 47 4 48 9 43 2 15 2 2 19* 1 48 0 24 9 4 3 4 89 5 19 7 14 0 14 1 1 77* 0 92 0 32 8 2 2 4 03 3 96 8 07 1 15 2 1 67* 1 22 0 33 8 4 3 3 33 3 71 4 61 0 13 1 1 71* 1 02 0 34 9 2 2 5 24 5 36 8 51 0 15 2 1 36* 0 67 0 09 7 4 3 1 98* 3 28 0 26 1 13 1 5 48 4 81 1 1 68 10 2 2 2 86* 4 43 0 28 0 16 2 1 32* 0 81 0 57 8 3 3 4 82 4 75 8 12 2 13 1 7 20 6 96 14 45 10 3 2 4 53 5 40 4 50 1 16 2 2 04* 1 12 0 24 9 3 3 3 10* 4 45 2 74 3 13 1 5 60 5 37 11 69 9 3 2 3 15 3 32 3 81 0 15 3 2 63* 3 31 0 29 9 2 3 2 27* 2 1 1 0 19 4 13 1 1 83* 3 85 0 18 8 3 2 5 48 5 48 12 35 1 15 3 2 82* 1 74 0 43 8 2 3 2 04* 2 29 0 24 5 13 1 2 76* 3 77 2 69 8 4 2 5 98 5 94 1 1 59 2 15 3 2 85* 1 81 0 37 8 1 3 1 57* 1 40 0 21 6 13 1 1 65* 2 09 1 08 9 4 2 4 23 4 46 5 39 4 14 3 2 05* 0 43 0 24 9 1 3 3 44 3 01 4 18 7 12 1 5 15 4 68 7 53 9 5 2 4 65 4 87 6 46 3 14 3 4 42 3 87 5 54 9 0 3 4 76 5 23 8 19 6 12 1 3 33 3 07 3 94 8 5 2 2 69* 3 48 2 86 2 14 3 2 94* 2 92 2 92 8 0 3 1 68* 1 38 O 30 5 12 1 2 03* 1 57 0 24 7 6 2 4 07 4 35 7 36 1 14 3 2 65* 3 01 2 46 7 0 4 5 08 5 32 12 32 4 12 1 4 43 4 82 8 43 8 6 2 2 06* 2 63 0 23 0 14 3 2 15* 3 39 0 22 8 0 4 1 98* 0 07 0 54 5 1 1 1 1 95* 0 81 0 44 9 6 2 1 71* 1 46 0 27 0 13 3 4 47 4 30 7 32 9 0 4 1 95* 0 26 0 26 6 1 1 1 4 08 3 56 7 08 9 7 2 3 65 3 39 4 42 1 13 3 1 83* 1 25 0 30 9 1 4 1 76* 3 14 0 13 7 1 1 1 1 97* 2 19 1 61 8 7 2 6 33 6 10 10 08 2 13 3 O 93* 2 4 1 0 05 8 1 4 2 36* 1 20 0 43 8 10 1 1 28* O 93 0 61 7 7 2 3 IO 3 17 5 60 3 13 3 3 94 3 06 6 41 7 1 4 1 87* 0 44 0 29 7 10 1 6 13 5 21 10 50 7 8 2 3 33 2 60 6 30 4 13 3 2 07* 1 29 0 23 7 2 4 5 14 4 98 9 81 6 10 1 1 13* 1 49 0 78 8 8 2 1 36* 3 78 0 07 5 13 3 1 42* 1 28 0 14 8 2 4 2 80* 3 43 2 21 6 9 1 3 39 3 32 6 60 8 9 2 2 19* 2 21 0 2 1 6 12 3 1 36* 1 66 0 54 9 2 4 2 33* 3 08 0 21 7 9 1 1 57* 3 07 0 18 7 9 2 2 28* 2 59 2 08 5 12 3 2 10* 3 40 0 23 9 3 4 2 09* 2 59 0 28 8 9 1 2 83* 2 69 3 05 6 9 2 3 78 3 64 6 39 4 12 3 2 64* 2 46 0 43 a 3 4 4 96 5 46 7 06 9 8 1 2 26* 2 62 0 20 5 10 2 4 97 4 70 10 99 3 12 3 1 61* 0 86 1 77 7 3 4 1 84* 2 62 0 16 8 8 1 2 03* 0 91 0 24 6 10 2 4 26 4 01 9 10 2 12 3 1 85* 1 81 O 29 6 4 4 6 15 6 16 1 1 88 7 8 1 1 75* 1 91 0 33 7 10 2 2 12* 1 77 0 22 1 12 3 3 91 4 49 7 92 7 4 4 5 57 4 98 1 1 84 7 7 1 0 85* 2 70 0 05 8 10 2 1 99* 1 36 0 25 0 12 3 1 79* 1 33 0 31 8 4 4 1 71* 1 16 0 18 8 7 1 3 81 4 26 6 53 7 1 1 2 2 24* 2 51 0 20 3 1 1 3 0 87* 1 79 0 06 8 5 4 0 99* 0 87 0 06 9 7 1 2 41* 2 67 0 28 6 1 1 2 2 98* 5 31 0 35 4 1 1 3 3 20 3 67 5 15 7 5 4 6 06 6 62 9 58 9 6 1 3 32 3 41 4 17 5 1 1 2 1 92* 1 16 0 27 5 1 1 3 1 62* 2 37 0 24 6 5 4 1 88* 2 95 0 28 8 6 1 2 32* 2 04 3 21 4 1 1 2 2 13* 2 76 2 63 6 1 1 3 1 38* 0 50 0 12 6 6 4 1 79* 1 77 0 38 8 5 1 5 48 5 36 1 1 69 2 12 2 1 89* 0 66 0 31 7 10 3 4 80 4 51 6 93 7 6 4 4 85 5 12 7 02 9 5 1 1 39* 2 64 0 74 3 12 2 3 60 4 29 5 51 6 io 3 0 83* 1 19 0 29 8 6 4 4 29 3 54 6 05 10 5 1 4 05 3 42 5 21 4 12 2 1 80* 1 21 0 31 5 10 3 2 48* 2 99 3 1 1 8 7 4 2 44* 2 76 1 89 10 4 1 1 98* 2 17 0 25 5 12 2 5 42 4 96 9 36 4 10 3 1 79* 0 79 0 31 7 7 4 2 16* 3 08 0 22 9 4 1 1 87* 1 69 0 22 6 12 2 1 24* 0 54 0 65 5 9 3 3 05 3 65 4 52 6 7 4 2 52* 1 66 3 34 8 4 1 7 54 8 39 15 13 6 13 2 2 05* 1 03 0 24 6 9 3 1 92* 1 18 O 27 5 7 4 6 60 6 36 14 82 9 3 1 2 46* 2 45 0 59 5 13 2 2 05* 1 42 0 24 7 9 3 1 30* 2 32 0 59 4 8 4 2 09* 1 48 0 46 10 3 1 2 77* 3 34 2 32 4 13 2 2 01* 1 02 0 25 8 8 3 5 53 5 45 7 98 5 8 4 6 76 6 58 14 74 10 2 1 2 15* 2 96 0 22 3 13 2 1 58* 0 90 0 18 7 8 3 3 02* 4 29 2 91 6 8 4 5 33 4 88 8 85 9 2 1 4 43 4 31 8 25 2 13 2 3 42 2 93 5 16 6 8 3 1 99* 2 78 0 28 7 8 4 2 66* 2 31 2 67 9 1 1 4 25 4 79 8 59 1 13 2 3 30 3 05 5 05 6 7 3 3 62 3 73 6 69 7 9 4 2 15* 3 49 0 22 10 1 1 1 36* 2 90 0 10 0 13 2 1 92* 1 39 0 27 7 7 3 7 13 7 67 1 1 96 6 9 4 2 73* 2 75 0 46 10 0 1 1 54* 2 44 1 05 O 14 2 3 94 3 28 6 21 8 7 3 2 07* 1 55 1 78 5 9 4 2 90* 2 96 3 92 9 0 1 4 81 5 06 10 69 1 14 2 4 73 4 97 6 67 9 6 3 1 02* 2 42 0 05 4 9 4 1 53* 0 70 0 18 8 0 2 3 75 4 77 9 15 2 14 2 2 91* 2 65 3 38 8 6 3 1 92* 2 94 0 18 3 9 4 2 09* 2 54 0 37 h k 1 Fo Fc weight h k 1 2 10 4 5 80 5 45 12 77 3 8 5 3 10 4 2 17* 2 62 0 42 2 8 5 4 10 4 5 27 5 26 8 79 1 8 5 5 10 4 2 33* 2 28 0 32 0 8 5 6 10 4 2 70* 1 76 2 81 3 7 5 5 1 1 4 5 61 5 14 7 97 4 7 5 4 1 1 4 1 64* 1 33 0 16 5 7 5 3 1 1 4 2 06* 1 48 2 41 6 7 5 2 1 1 4 3 86 3 99 6 19 7 7 5 1 1 1 4 4 76 4 35 9 27 7 6 5 0 1 1 4 1 91* 0 58 2 31 6 6 5 0 12 4 1 87* 0 57 0 29 5 6 5 1 12 4 3 83 3 80 6 15 4 6 5 2 12 4 4 65 3 70 8 16 4 5 5 3 12 4 1 91 * 1 44 0 27 5 5 5 4 12 4 1 39* 3 84 0 06 6 5 5 5 12 . 4 2 58* 1 41 2 24 7 5 5 3 13 4 1 99* 4 24 0 14 7 4 5 2 13 4 2 24* 1 81 0 20 6 4 5 1 13 4 2 72* 2 42 0 37 5 4 5 0 13 4 2 11* 0 79 0 22 5 3 5 0 14 4 2 28* 1 34 0 19 6 3 5 1 14 4 2 00* 2 91 0 23 7 3 5 2 14 4 3 97 4 1 1 4 44 8 3 5 0 13 5 1 01 * 1 65 0 09 8 2 5 3 12 5 4 37 4 21 5 34 7 2 5 2 12 5 1 29* 1 35 0 60 6 2 5 1 12 5 2 14* 1 68 0 22 5 2 5 0 12 5 1 97* 0 80 0 26 6 1 5 0 1 1 5 1 64* 1 23 0 17 7 1 5 1 1 1 5 7 21 6 41 12 02 8 1 5 2 11 5 2 15* 1 13 O 41 8 0 5 3 1 1 5 6 04 6 35 8 81 7 0 5 4 1 1 5 2 05* 1 76 0 24 6 0 5 5 10 5 3 46 2 91 3 43 3 0 6 4 10 5 1 38* 3 14 0 09 4 0 6 3 10 5 5 16 5 57 6 20 5 0 6 2 10 5 4 34 4 62 7 09 6 0 6 1 10 5 0 92* 2 33 0 05 7 0 6 0 10 5 1 96* 1 39 0 26 7 1 6 O 9 5 2 65* 0 36 0 53 6 1 6 1 9 5 6 26 6 57 13 18 5 1 6 2 9 5 1 56* 1 54 0 16 4 1 6 3 9 5 1 93* 1 81 0 27 3 1 6 4 9 5 7 25 6 99 1 1 32 3 2 6 5 9 5 6 77 6 21 10 86 4 2 6 6 8 5 2 24* 2 93 0 20 5 2 6 5 8 5 2 35* 2 12 0 39 6 2 6 4 8 5 1 31* 3 23 0 08 6 3 6 Fo Fc weight h k 1 Fo Fc 6 62 6 15 13 18 5 3 6 4 76 3 78 1 78* 0 36 0 32 4 3 6 2 00* 2 83 4 82 5 27 10 24 3 3 6 4 06 4 07 1 99* 1 97 2 29 2 3 6 1 87* 1 20 4 00 4 34 7 52 1 4 G 2 40* 3 38 3 23 2 54 5 32 2 4 6 2 08* 2 09 3 51 3 28 4 41 3 4 6 6 57 6 54 4 06 4 19 5 48 4 4 6 1 79* 1 36 2 72* 2 74 0 36 5 4 6 2 09* 2 OO 2 21* 2 26 0 2 1 6 4 6 2 65* 2 66 1 93* 1 37 0 27 6 5 6 2 17 + 1 00 4 93 4 69 8 94 5 5 6 1 39* 1 85 4 35 3 88 8 61 4 5 6 2 17* 2 53 3 36 3 63 5 82 3 5 6 3 80 4 29 4 95 4 51 10 82 2 5 6 1 88* 0 91 1 94* 1 80 1 45 1 5 6 2 66* 1 28 3 64 4 26 3 92 0 5 6 10 12 10 83 1 99* 3 07 0 35 0 6 6 1 26* 0 44 1 98* 2 30 0 26 1 6 6 2 73* 3 59 1 99* 2 04 0 25 2 6 6 2 23* 3 6 1 5 77 5 88 13 08 3 6 6 3 51 3 88 7 1 1 7 80 1 1 16 4 6 6 2 06* 1 96 1 72* 0 98 0 16 5 6 6 4 16 5 08 2 14* 2 02 0 22 5 7 6 2 19* 2 44 4 39 4 92 4 86 4 7 6 2 04* 1 48 4 97 5 22 5 96 3 7 6 2 06* 2 02 5 06 4 94 9 72 2 7 6 7 16 7 16 2 57* 1 95 3 53 1 7 6 4 68 4 25 1 23* 1 70 0 66 0 7 6 2 60* 1 42 5 14 5 20 6 51 0 8 6 1 24* 1 54 3 13* 3 58 0 38 1 8 6 2 30* 1 81 0 97* 0 30 0 45 2 8 6 5 42 4 7 1 4 40 3 99 8 65 3 8 6 3 86 4 48 3 47 3 54 6 69 4 8 6 2 05* 2 32 9 54 9 68 19 76 4 9 6 2 71* 3 63 2 46* 0 7 1 0 62 3 9 6 2 66* 1 57 7 81 8 01 15 80 2 9 6 2 04* 1 78 3 58 3 46 5 10 1 9 6 2 13* 3 02 1 86* 0 97 0 29 0 9 6 1 89* 1 24 4 60 4 40 4 47 0 10 6 3 64 4 70 6 31 6 74 6 82 1 IO 6 4 31 4 18 5 47 4 85 7 15 2 10 6 3 39 3 86 3 13* 3 63 0 38 3 10 6 4 02 3 90 4 73 4 04 7 62 0 1 1 6 r 13* 1 90 2 00* 1 65 0 25 1 8 7 3 66 3 04 9 66 9 70 14 90 0 8 7 2 04* 1 61 7 06 7 01 10 46 0 7 7 1 33* 0 52 2 31* 2 13 0 24 1 7 7 2 92* 3 51 2 04* 3 90 1 12 2 7 7 2 16* 2 79 we 1ght h k 1 Fo Fc weight *w 8 14 3 6 7 2 04* 1 28 0 24 "T3 ns 1 66 2 6 7 1 .41* 3 02 0 12 3 9 00 1 6 7 1 . 10* 1 90 0 39 a . 8-0 29 0 6 7 7 .77 7 63 10 57 3 12 0 5 7 3 .71 3 90 4 93 O 0 23 1 5 7 2 . 12* 2 69 0 22 13 21 2 5 7 5 29 5 45 8 18 O 31 3 5 7 2 25* 2 89 0 24 0 23 4 5 7 3 35 4 44 3 22 2 10 4 4 7 2 15* 1 22 0 22 O 21 4 4 7 2 24* 1 22 0 20 O 09 3 4 7 2 18* 3 42 1 38 1 89 2 4 7 5 31 5 12 6 51 6 31 1 4 7 5 12 4 77 7 81 0 28 0 4 7 2 14* O 58 O 28 4 31 0 3 7 2 02* 0 71 0 24 17 79 1 3 7 3 95 3 86 5 58 0 12 2 3 7 4 82 4 84 7 43 3 15 3 3 7 3 06* 2 90 3 00 0 34 4 3 7 2 77* 2 35 2 40 4 58 5 2 7 4 18 4 46 3 57 0 24 4 2 7 2 27* 3 07 O 19 5 16 3 2 7 6 44 5 86 9 07 0 21 2 2 7 1 16* 2 6 1 0 47 0 24 1 2 7 3 88 3 44 4 69 0 23 0 2 7 2 03* 2 15 0 24 13 30 0 1 7 3 48 4 61 3 97 7 79 1 1 7 2 87* 3 58 2 85 3 97 2 1 7 5 10 5 27 6 15 0 65 3 1 7 4 25 4 75 3 75 0 32 4 1 7 2 94* 3 12 2 10 8 07 5 1 7 2 32* 1 18 0 19 4 38 5 0 7 1 39* 2 98 0 71 0 24 4 0 7 7 39 7 64 1 1 69 0 34 3 0 7 3 87 4 67 5 77 2 83 2 0 7 1 96* 1 59 O 26 0 24 1 0 7 2 37* 2 42 2 80 0 22 0 0 8 2 01* 1 63 O 25 0 28 1 0 8 2 03* 0 65 0 24 3 51 0 1 8 2 03* 0 19 0 24 5 20 3 54 775 r e f 1 e c t i o n s 4 21 0 43 4 08 0 27 0 56 2 O 84 2 1 O O —i Appendix D Structure Factors for the Cyclohexenone 88 h k 1 Fo Fc weight h k 1 Fo Fc weight h k 1 Fo Fc weight h k 1 Fo Fc weight 1 0 0 65. 09 71 , 10 O. .03 9 0 2 42 . 37 40 .28 1 . 15 17 0 4 10 . 53 9 .57 4 . 7 1 -8 O 8 21 .31 21 .55 6. .54 2 0 0 21 . 34 20. .05 4. 78 10 0 2 34 .59 38 .23 1 .49 18 0 4 10 .08 8 . 36 3 .37 -7 0 8 30 .63 31 .02 2. .67 3 0 o 102. 81 109 68 0. OI 1 1 0 2 34 .84 35 .90 1 .40 19 0 4 4 .87* 2 . 46 0 .04 -6 0 8 27 . 77 23 .89 3 .00 4 0 0 50. 46 51 56 0 94 12 0 2 43 .73 46 .26 1 .02 - 19 0 6 6 . 23* 8 .64 0 .07 -5 0 8 12 .09 12 .41 14 .50 5 0 0 92 . 79 95, . 16 0 02 13 0 2 39 . 74 39 .30 1 . 12 - 18 0 6 8 . 72 8 .56 2 . 48 -4 0 8 24 . 15 22 . 22 4 .66 6 0 o 84 18 87 47 0 02 14 0 2 26 . 13 25 .86 4 . 10 - 17 0 6 8 . 36 9 .03 2 .94 -3 0 8 29 .64 29 88 3. 05 7 0 0 16 48 17 .45 10. 07 15 0 2 8 .38 9 . 14 5 . 15 - 16 0 6 16 . 89 15 .94 1 1 . 13 -2 0 8 17 . 44 15 .65 13 76 8 0 0 25 .65 29 .33 4 .88 16 0 2 17 .59 16 . 12 10 .82 - 15 0 6 13 .82 13 .72 9 . 33 -1 0 8 33 . 79 31 .57 2. 69 9 0 0 41 . 62 41 , .34 1 , , 22 17 0 2 17 .35 18 .02 12 . , 17 - 14 0 6 8 .83 7 .70 4 . 91 0 O 8 2 . 44* 5 . 20 0. 04 10 0 0 33 .85 34 .66 1 , . 57 18 0 2 25 .54 24 .60 5 . 45 -13 0 6 1 1 .59 1 1 .94 9 .07 1 0 8 19 .23 21 . 74 7 . 17 1 1 0 0 23 . 11 24 .92 3 .96 19 0 2 14 .23 14 .92 6 . 15 - 12 0 6 10 . 10 1 1 . 46 8. .07 2 0 8 66 .70 69 .23 0. .50 12 0 o 8 .49 7 .95 11 28 20 0 2 15 .72 15 .47 6 .23 - 1 1 0 6 3 . 56* 1 . 42 0. .08 3 0 8 45 .63 43 .39 0. .93 13 0 o 9 .78 8 .81 12 . 12 -20 0 4 5 ;46* 6 .20 0 .06 -10 0 6 9 .81 8 . 46 10. 82 4 0 8 3 .58* 1 . 43 0 .08 14 0 0 10 .61 10 .56 1 1 , .37 -19 0 4 14; .30 13 .89 6 .36 -9 0 6 3 . 37* 0 . 7 1 O. .09 5 0 8 6 .20 3 .68 4 . 02 15 0 o 7 .57 6 .45 4 82 - 18 0 4 14 .47 15 . 44 8 . 10 -8 0 6 18 .83 18 . 39 1 1 92 6 0 8 1 .84* 3 .91 O. . 30 16 0 0 15 .07 14 .71 13 . 15 -17 0 4 13 .35 13 . 19 8 .36 -7 0 6 4 . 25 5 .59 3 20 7 0 8 3 .86* 1 . 12 0 .07 17 0 0 12 . 20 12 .31 7 82 -16 0 4 16 .96 17 .67 9 .31 -6 0 6 3 .06* 4 .70 0. . 1 1 8 0 8 3 .98* 2 .52 1. 21 18 0 0 16 .27 15 .30 10 .76 -15 0 4 26 .55 26 .51 3 . 74 -5 O 6 27 .91 28 . 32 3 . 67 9 0 8 3 .95* 4 .85 0. 06 19 0 0 10 . 37 1 1 . 13 4 .30 -14 0 4 12 .84 13 . 18 1 1 .97 -4 0 6 13 . 27 13 .97 23. .30 10 0 8 10 .45 1 1 .73 6. 19 20 0 0 14 .70 13 .95 6 .08 -13 0 4 36 .68 35 .80 2 . 38 -3 0 6 62 .62 59 .00 0. .59 1 1 0 8 8 .01 7 .45 3. 46 20 0 2 4 .68* 3 .52 0 .05 - 12 0 4 35 .74 38 OI 1 , . 28 -2 O 6 69 . 46 64 . 73 0. .49 12 0 8 5 .96* 6 .43 0. 1 1 19 0 2 4 .39* 2 . 1 1 0 .05 - 11 0 4 44 .30 42 .72 1 . .02 - 1 O 6 26 . 17 26 . 29 4 . 19 13 0 8 2 .32* 0. .97 O. 22 18 0 2 4 . 28* 1 . 15 0 .05 -10 0 4 31 .29 29 .35 3 .20 0 0 6 7 . 80 8 .87 14 . 32 14 0 8 1 .04* 3 .96 0. OO 17 0 2 4 .22* 5 .79 0 .06 -9 0 4 34 .80 34 .95 1 .52 1 0 6 108 . 23 107 .43 0. .01 15 0 a 8 .82 9 .38 2 . 28 16 o 2 27 .57 26 .90 4 .90 -8 0 4 48 . 32 44 . 34 0 . 93 2 o 6 73 . 33 7 1 . 73 0. . 44 - 14 0 10 10 .07 1 1 .03 2 . 95 15 0 2 10 .26 10 .04 8 .21 -7 0 4 47 . 72 47 .50 0 .96 3 0 6 13 . 39 13 .59 24 . 30 - 13 0 10 4 . 74* 3 .67 0. 04 14 0 2 37 .97 38 .62 1 , . 15 -6 0 4 7 .70 8 . 14 22 40 4 0 6 37 .84 38 .00 1 31 - 12 0 10 8 .62 7 56 2 .61 13 0 2 32 .67 34 .01 2 .82 -5 0 4 44 .99 42 .03 1 . .09 5 0 6 39 .31 38 .49 1 . .23 - 1 1 0 10 13 .24 13 .47 6 .79 12 0 2 18 .05 18 .50 10 . 12 -4 0 4 53 . 28 47 , 12 0 .82 6 0 6 31 . 7 1 34 . 74 3 .07 -10 0 10 4 32* 2 . 33 O. .05 1 1 0 2 39 .55 38 .82 1 .23 -3 0 4 31 .24 27 .48 2 .00 7 o 6 36 . 15 35 .20 1 . .31 -9 0 10 2 . 84* 1 .68 0. .42 10 0 2 66 .50 70 .05 0 .53 -2 0 4 50 .07 43 . 28 0 92 8 0 6 19 .64 20 . 13 12 . 33 -8 0 10 4 . 27* 2 .06 O 05 -9 0 2 89 .78 88 .07 0. .30 -1 0 4 22 .00 21 .69 6. .24 9 0 6 14 .99 14 .62 13. .02 -7 0 10 13 .85 13 .24 9 . 13 -8 0 2 104 ,43 106 .61 O, .01 0 0 4 66 .96 63 . 49 0. .53 10 0 6 17 .02 17 . 56 12 . 14 -6 o 10 17 . 79 16 . 1 1 13 . 72 -7 0 2 69 . 16 71 .97 0 .50 1 0 4 51 . 12 47 .02 0. .89 11 0 6 18 . 35 18 .59 17 .21 -5 0 10 1 1 .86 io .52 7 .87 -6 0 2 61 .89 60 ,80 0 62 2 0 4 10 .47 10 .99 25. . 4 1 12 0 6 18 .83 19 . 32 1 1 .91 -4 0 10 4 .03* 2 .67 0. .06 -5 0 2 86 .60 86 .33 0. .02 3 0 4 38 .95 41 .48 1 . 4 1 13 0 6 9 .58 10 . 32 5. .25 -3 o 10 , .54* ; 1 .09 b. 01 -4 0 2 109 .73 104 .21 0 ,01 4 0 4 95 .67 97 . 33 0. .02 14 0 6 4 .57* 8 .47 0 .07 -2 0 IO 4 .95* 1 .65 0. .09 -3 0 2 92 .21 88 .62 0 .02 5 0 4 54 .06 58 .80 0. 78 15 0 6 4 . 35* 2 .01 0 .05 - 1 0 10 1 .78* 0 .67 0. .01 -2 0 2 1 18 .55 111, . 19 0 .01 6 0 4 14 .21 16 . 74 17 . 70 16 0 6 0 .72* 0 .90 0 .02 0 0 10 12 .31 1 1 .95 8 69 - 1 0 2 59. .25 48 .27 0 .04 7 0 4 52 ,30 55 .65 0. .81 17 o 6 5 .01* 3 .46 0 .80 1 0 10 12 .91 16 .01 9 33 0 0 2 14 . 35 12 ,09 13. 27 8 0 4 31 .91 37 .85 1 . .65 -17 0 8 4 . 74* 1 .07 0 .04 2 0 10 18 .62 2 1 . 19 10. 51 1 0 2 217. 23 237. .57 0. 00 9 0 4 46 .26 46 .97 O .96 -16 0 8 4 88* 1 . 76 0 .05 3 0 10 2 . 74* 7 .81 0. 03 2 0 2 36. ,93 35 92 1 . 68 10 0 4 47 .43 51 .22' 0. .91 -15 0 8 5 . 33* 2 .69 0 .07 4 0 10 6 . 28 5 . 19 2 22 3 0 2 16. 10 17 . 70 9. 66 1 1 0 4 40 .97 41 .61 1 .08 - 14 o 8 5 . 10* 1 . 18 0 .08 5 0 10 4 .20* 9 . 39 0 .06 4 o 2 2. 03* 1 . .71 0. .24 12 o 4 30 .91 33 . 18 2 . 75 - 13 0 8 1 . 47* 1 .67 0 . 12 6 0 10 10 .05 12 .01 4 .96 5 0 2 63 96 63 .67 0. 58 13 0 4 29 .93 30 .67 2 .62 -12 o 8 18 . 26 18 .73 10 .78 7 0 10 2 .57* 1 . 19 0 .02 6 0 2 28 .92 28 . 12 2 . 26 14 0 4 28 .49 28 .36 3 .68 -11 0 8 13 .00 13 .49 9 .49 8 0 10 3 . 70* 5 . 1 1 0 .04 7 0 2 1 .54* 1 .96 0 .06 15 0 4 24 .73 25 . 25 6 .56 -10 0 8 8 . 94 9 .09 5 .58 9 0 10 4 . 52* 7 .51 0 .05 8 0 2 30 . 29 31 .83 1 .92 16 o 4 1 1 .81 10 . 77 6 .59 -9 0 8 18 . 37 17 . 63 12 .80 10 o 10 2 . 52* 4 05 0 .02 h k 1 Fo Fc weight 11 0 10 4 76* 6 55 0 04 -9 0 12 4 51* 4 27 0 58 -8 0 12 3 14* 0 41 0 02 -7 0 12 2 61* 6 20 0 22 -6 0 12 3 24* 2 19 0 02 -5 0 12 4 67* 0 51 0 05 -4 0 12 4 63* 0 64 0 05 -3 0 12 5 90* 3 66 0 08 -2 0 12 4 07* 5 78 0 58 - 1 0 12 14 36 15 79 6 23 0 0 12 4 69* 4 59 0 05 1 0 12 0 44* 4 33 0 01 2 0 12 1 45* 2 63 0 00 3 o 12 5 10* 4 40 0 87 4 0 12 4 74* 2 88 0 04 5 0 12 4 70* 1 65 0 05 5 1 12 5 99* 0 28 0 07 4 1 12 4 79* 5 26 0 04 3 1 12 4 86* 0 47 0 05 2 1 12 7 27 6 97 1 71 1 1 12 4 75* 4 31 0 04 0 1 12 4 67* 0 50 0 05 -1 1 12 e 41* 2 75 0 09 -2 1 12 5 99* 4 84 0 08 -3 1 12 1 95* 0 75 0 13 -4 1 12 2 33* 3 41 0 18 -5 1 12 4 04* 5 59 0 54 -6 1 12 4 69* 2 93 0 05 -7 1 12 2 38* 2 55 0 18 -8 1 12 7 00 6 66 1 43 -9 1 12 4 91* 6 84 0 67 -12 1 1 1 4 82* 2 91 0 04 -11 1 1 1 2 07* 2 00 0 01 -10 1 1 1 1 44* 0 28 0 OO -9 1 11 4 65* 3 12 0 05 -8 1 1 1 5 70* 1 67 0 09 -7 1 1 1 6 04* 6 56 0 09 -G 1 1 1 2 15* 1 91 0 22 -5 1 1 1 2 14* 0 82 0 22 -4 1 1 1 0 96* 0 35 0 OO -3 1 1 1 4 31* 4 85 0 94 -2 1 1 1 4 33* 0 45 0 05 -1 1 1 1 4 28* 0 46 0 05 0 1 1 1 0 87* 0 21 0 04 1 1 1 1 4 35* 4 93 0 94 2 1 1 1 4 31* 2 52 0 05 3 1 1 1 3 24* 8 28 o 03 4 1 1 1 2 17* 1 67 0 21 5 1 1 1 5 OO* O 35 0 06 h k 1 Fo Fc weight 6 1 1 1 4 06* 2 04 0 04 7 1 11 9 23 9 33 2 82 8 1 1 1 0 83* 2 08 0 02 9 1 1 1 4 72* 3 15 0 04 1 1 1 10 4 75* 3 92 0 04 10 1 10 4 65* 0 92 0 05 9 1 10 2 68* 1 52 0 02 8 1 10 4 54* 4 44 0 06 7 1 10 5 15* 6 21 O 07 6 1 10 8 61 6 43 3 73 5 1 10 12 42 10 36 7 34 4 1 10 14 39 14 00 9 68 3 1 10 7 38 6 31 3 06 2 1 10 1 1 98 10 84 7 83 1 1 10 20 45 19 74 9 66 0 1 10 13 4 1 13 62 9 63 -1 1 10 4 06* 2 23 0 06 -2 1 10 1 1 75 10 63 8 15 -3 1 10 9 29 9 00 5 24 -4 1 10 3 36* 4 44 0 04 -5 1 10 1 1 34 12 65 7 12 -6 1 10 5 17* 9 01 O 09 -7 1 10 6 27 7 31 2 20 -8 1 10 4 40* 5 05 0 06 -9 1 10 5 87* 5 16 0 11 -10 1 10 5 27* 7 44 1 28 -11 1 10 4 51* 3 49 0 05 -12 1 10 6 55 3 95 1 53 -13 1 10 4 83* 4 31 0 04 -14 1 10 6 30* 2 28 o 07 -16 1 9 4 87* 0 40 0 04 -15 1 9 4 70* 4 44 0 05 -14 1 9 4 63* 2 09 0 05 -13 1 9 7 48 7 51 2 35 -12 1 9 3 59* 0 93 0 04 -11 1 9 4 23* 0 33 0 06 -10 1 9 4 53* 2 77 1 2 1 -9 1 9 1 77* 1 29 0 20 -8 1 9 4 OO* 4 81 1 08 -7 1 9 3 92* 3 30 0 07 -6 1 9 3 89* 4 49 0 07 -5 1 9 3 79* 4 48 0 07 -4 1 9 3 79* 1 44 0 07 -3 1 9 4 80* 2 69 0 12 -2 1 9 14 02 15 37 13 28 -1 1 9 6 85 5 27 3 98 0 1 9 3 74* 0 78 0 07 1 1 9 3 79* 4 29 0 07 2 1 9 13 29 14 34 1 1 84 h k 1 Fo Fc weight 3 1 9 3 43* 0 60 0 06 4 1 9 .4 17* 2 84 O 08 5 1 9 2 82* 5 46 0 55 6 1 9 4 20* 0 52 1 21 7 1 9 4 85* 2 02 0 09 8 1 9 2 10* 3 80 0 02 9 1 9 1 66* 0 14 0 01 10 1 9 1 80* 2 68 0 16 1 1 9 4 47* 1 92 0 05 12 9 4 61* 1 53 0 05 13 9 3 17* 2 87 0 02 14 8 1 1 4 1 9 76 4 12 13 8 9 91 10 1 1 3 56 12 8 1 96* 7 51 0 01 1 1 8 14 55 14 19 9 4 1 10 8 17 27 18 38 13 02 9 8 17 75 18 02 7 88 8 8 14 51 14 84 12 52 7 8 14 74 14 28 13 52 6 8 18 04 19 14 18 28 5 8 7 89 8 23 5 91 4 8 19 4 1 19 51 1 1 58 3 8 26 4 1 27 69 2 89 2 8 15 37 14 89 20 08 1 8 19 87 20 54 8 76 0 8 31 52 30 94 2 82 -1 8 17 46 19 19 12 18 -2 8 3 63* 2 65 O 09 -3 8 6 84 8 77 5 72 -4 8 4 42 2 25 2 40 -5 8 6 26 5 29 4 44 -6 8 3 55* O 37 0 08 -7 8 3 70* 1 82 0 07 -8 8 1 1 52 9 72 9 83 -9 8 13 88 12 77 12 32 -10 8 8 32 6 64 4 81 -11 8 4 46* 1 91 0 07 -12 8 10 65 9 54 6 16 -13 8 12 92 1 1 74 7 89 -14 8 4 45* 5 90 0 05 -15 8 5 35* 4 66 1 23 - 16 8 12 4 1 1 1 81 4 81 -17 8 4 43* 5 85 0 59 -18 7 4 68* 4 38 0 67 -17 7 2 88* 1 28 0 02 - IG 7 4 74* 4 09 0 99 -15 7 4 29* 2 32 0 05 - 14 7 4 10* 1 49 0 06 -13 7 13 GO 13 28 9 81 h k 1 Fo Fc weight -12 1 7 14 10 13 76 1 1 78 pen -11 1 7 1 1 90 1 1 12 9 73 pen -10 1 7 12 02 12 82 12 07 a . -9 1 7 3 60* 0 09 0 08 H' -8 1 7 2 94* 0 90 0 06 <3 -7 1 7 3 42* 5 63 0 09 -6 1 7 3 27* 2 51 0 09 -5 1 7 7 08 5 86 7 50 -4 1 7 5 79 5 02 5 50 -3 1 7 3 17* 2 24 O IO -2 1 7 2 86* 1 85 0 08 -1 1 7 8 44 8 42 1 1 37 0 1 7 1 81* 0 84 0 59 1 1 7 9 63 10 6 1 13 99 2 1 7 8 28 8 04 10 17 3 1 7 10 81 10 66 15 52 4 1 7 5 89 6 84 5 02 5 1 7 1 1 19 1 1 99 14 27 6 1 7 1 94* 2 87 0 03 7 1 7 3 48* 0 49 0 08 8 1 7 1 44* 2 96 O 01 9 1 7 3 74* O 30 0 07 10 1 7 3 95* 4 65 0 07 1 1 1 7 5 95 5 4 1 2 4 1 12 1 7 1 33* 0 77 0 01 13 1 7 4 21* 5 62 0 06 14 1 7 4 38* 2 77 0 05 15 1 7 2 29* 1 35 0 19 16 1 7 4 81 * 5 43 0 04 17 1 6 13 02 12 92 4 7 1 16 1 6 16 19 16 05 7 55 15 1 6 10 15 9 59 4 50 14 1 6 12 01 13 03 6 60 13 1 6 22 09 2 1 66 8 14 12 1 6 16 35 17 55 13 69 1 1 1 6 17 76 18 73 9 17 10 1 6 18 92 2 1 25 9 34 9 1 6 24 63 26 02 5 88 8 1 6 24 73 27 88 4 82 7 1 6 14 87 15 29 19 50 6 1 6 10 61 1 1 59 15 86 5 1 6 12 17 14 40 21 05 4 1 6 12 29 1 1 94 23 38 3 1 6 9 44 10 26 16 64 2 1 6 6 51 5 66 9 12 1 1 6 23 14 19 63 4 25 0 1 6 30 74 27 47 1 75 - 1 1 6 6 19 5 98 9 00 <o -2 1 6 17 45 16 59 10 34 h k 1 Fo Fc weight h k 1 Fo Fc we i ght h k 1 Fo Fc we 1ght h k 1 Fo Fc weight -3 1 6 30 90 29 96 1 75 13 1 5 1 54* 4 25 0 01 -17 1 3 3 96* 3 31 0 06 8 1 2 58 4 1 61 42 O 67 -4 1 6 21 84 20 66 6 49 14 1 5 5 12* 2 34 0 10 -16 1 3 8 37 8 42 4 48 7 1 2 63 89 66 33 0 58 -5 1 6 36 46 35 14 1 39 15 1 5 5 22* 5 02 0 09 -15 1 3 10 61 10 72 8 08 6 1 2 65 89 69 85 0 55 -G 1 6 36 32 34 81 1 36 16 1 5 4 41* 0 34 0 05 -14 1 3 5 16* 8 16 0 14 5 1 2 84 35 85 30 0 02 -7 1 6 37 61 36 61 1 28 17 1 5 5 78* 4 65 0 08 -13 1 3 1 64* 2 13 0 34 4 1 2 95 62 98 28 0 02 -8 1 6 24 OO 22 66 5 23 18 1 5 5 20* 1 84 0 87 -12 1 3 3 32* 0 47 0 09 3 1 2 89 81 94 99 O 02 -9 1 6 43 37 43 20 1 02 19 1 4 10 86 10 21 3 30 - 1 1 1 3 13 35 13 92 16 08 2 1 2 144 29 153 80 0 01 10 1 6 46 22 46 04 0 91 18 1 4 10 91 1 1 47 3 73 -10 1 3 3 25* 0 60 2 37 1 1 2 83 10 80 38 O 02 1 1 1 6 27 25 27 36 2 88 17 1 4 5 98 6 51 1 52 -9 1 3 10 31 8 58 22 87 0 1 2 82 26 79 27 0 02 12 1 6 17 78 17 71 9 58 16 1 4 13 75 13 36 8 42 -8 1 3 20 96 19 88 5 16 -1 1 2 89 55 84 22 0 02 13 1 6 18 08 18 07 8 83 15 1 4 12 23 12 44 8 05 -7 1 3 1 44* 0 59 0 91 -2 1 2 150 47 148 81 0 01 14 1 6 13 07 14 07 9 40 14 1 4 3 97* 4 57 0 06 -6 1 3 2 40* 0 79 0 17 -3 1 2 13 1 1 13 00 15 42 15 1 6 9 78 10 80 5 01 13 1 4 3 20* 2 74 0 05 -5 1 3 48 13 46 49 0 99 -4 1 2 67 12 66 00 0 54 16 1 6 4 69* 4 40 0 06 12 1 4 14 13 14 07 1 1 34 -4 1 3 8 70 8 84 46 99 -5 1 2 5 17 3 B9 23 04 17 1 6 10 59 1 1 16 4 66 11 1 4 10 72 10 87 12 75 -3 1 3 10 61 9 85 27 98 -6 1 2 5 52 4 90 20 40 18 1 6 2 89* 3 83 0 02 10 1 4 1 07* 2 55 0 01 -2 1 3 9 70 9 09 39 10 -7 1 2 2 54* 1 46 0 20 19 1 6 4 21* 5 65 0 52 9 1 4 8 69 8 66 12 62 -1 1 3 58 49 53 18 0 70 -8 1 2 12 55 12 27 23 84 19 1 5 4 72* 4 31 0 04 8 1 4 3 19* 3 37 0 13 0 1 3 49 07 48 54 0 98 -9 1 2 13 37 14 58 21 14 18 1 5 4 54* 3 33 0 05 7 1 4 17 21 18 09 13 03 1 1 3 98 03 91 37 0 01 -10 1 2 9 28 8 70 18 53 17 1 5 2 12* 1 01 0 22 6 1 4 30 39 32 15 1 87 2 1 3 46 73 42 17 1 06 - 1 1 1 2 25 93 26 54 3 80 16 1 5 3 96* 5 16 0 05 5 1 4 52 07 53 35 0 83 3 1 3 2 73 4 98 6 09 -12 1 2 3 27* 5 36 O 09 15 1 5 4 OO* 1 53 0 06 4 1 4 46 99 48 28 1 01 4 1 3 19 53 18 90 6 75 -13 1 2 22 15 22 76 6 37 14 1 5 12 19 12 19 9 72 3 1 4 93 29 88 70 0 02 5 1 3 39 89 37 81 1 35 -14 1 2 33 05 34 18 2 62 13 1 5 12 49 12 66 11 39 2 1 4 35 87 35 17 1 62 6 1 3 52 24 52 56 0 83 -15 1 2 24 59 24 05 6 52 12 1 5 17 44 17 42 9 94 1 1 4 49 89 48 81 0 92 7 1 3 9 03 9 28 26 50 -16 1 2 13 63 12 92 1 1 14 11 1 5 19 46 18 75 10 38 0 1 4 81 91 77 81 0 02 8 1 3 3 02* 6 16 0 13 -17 1 2 24 09 23 79 6 33 10 1 5 12 97 13 79 19 30 -1 1 4 129 50 122 03 0 01 9 1 3 13 2 1 13 94 23 56 -18 1 2 15 12 14 72 9 65 -9 1 5 11 34 1 1 74 18 47 -2 1 4 67 14 64 88 0 53 10 1 3 3 17* 2 45 0 10 -19 1 2 13 54 13 52 6 84 -8 1 5 2 45* 3 39 1 18 -3 1 4 90 03 86 16 0 02 1 1 1 3 5 93 6 12 5 22 -20 1 2 18 87 18 17 7 90 -7 1 5 19 32 18 49 10 46 -4 1 4 66 74 63 79 0 53 12 1 3 19 7 1 21 54 8 59 -20 1 1 2 33* 0 31 0 18 -6 1 5 4 88 4 13 6 13 -5 1 4 56 80 57 32 0 72 13 1 3 2 19* 2 79 0 03 -19 1 1 4 51* 4 42 O 05 -5 1 5 1 1 35 1 1 21 31 72 -6 1 4 52 29 52 38 0 83 14 1 3 23 25 22 47 5 02 -18 1 1 4 23* 2 47 0 06 -4 1 5 54 67 50 50 0 76 -7 1 4 55 78 54 29 0 73 15 1 3 2 20* 2 25 0 02 -17 1 1 4 70* 6 65 0 08 -3 1 5 4 97 5 26 9 52 -8 1 4 41 86 41 53 1 18 16 1 3 4 04* 6 20 0 93 -16 1 1 7 31 7 40 3 78 -2 1 5 12 96 10 74 20 90 -9 1 4 21 82 21 09 6 22 17 1 3 4 35* 2 85 0 05 -15 1 1 3 69* 5 68 1 12 -1 1 5 4 54 4 30 8 33 -10 1 4 30 08 30 22 3 32 18 1 3 4 52* 3 58 0 05 -14 1 1 12 00 12 46 13 85 0 1 5 45 54 4 1 54 1 06 -11 1 4 37 76 37 32 1 26 19 1 3 4 75* 1 45 0 04 - 13 1 1 3 35* 0 24 0 09 1 1 5 15 62 15 91 21 03 -12 1 4 15 97 16 77 16 49 20 1 2 5 65* 5 47 0 94 -12 1 1 3 22* 0 49 0 10 2 1 5 35 06 34 67 1 59 -13 1 4 2 33* 2 53 O 62 19 1 2 4 62* 0 80 0 05 - 1 1 1 1 7 06 7 46 9 88 3 1 5 8 29 7 76 22 05 -14 1 4 7 13 8 05 4 22 18 1 2 1 71* 6 46 0 01 -10 1 1 12 93 13 1 1 31 14 4 1 5 0 21* 0 24 0 01 -15 1 4 5 87 6 09 2 49 17 1 2 4 84* 1 63 0 08 -9 1 1 16 09 15 32 15 53 5 1 5 12 60 1 1 27 29 57 -16 1 4 3 41* 2 45 0 05 16 1 2 3 02* 4 61 0 04 -8 1 1 16 97 16 68 1 1 65 6 1 5 15 22 15 99 16 49 -17 1 4 5 68* 5 73 0 1 1 15 1 2 9 73 10 18 6 51 -7 1 1 14 97 14 78 16 33 7 1 5 9 33 1 1 20 14 97 -18 1 4 2 15* 2 21 0 22 14 1 2 17 72 17 13 14 17 -6 1 1 13 61 13 21 15 17 8 1 5 3 19* 5 12 0 10 -19 1 4 10 92 1 1 18 3 86 13 1 2 3 1 95 33 61 2 71 -5 1 1 8 53 8 39 44 81 9 1 5 3 28* 0 37 0 09 -20 1 4 2 41* 3 90 0 18 12 1 2 45 51 46 59 0 95 -4 1 1 59 55 58 99 0 68 10 1 5 3 47* 5 70 1 55 -20 1 3 4 47* 2 83 0 65 1 1 1 2 33 61 34 90 1 43 -3 1 1 37 95 36 76 1 61 1 1 1 5 1 85* 5 46 0 02 -19 1 3 2 27* 2 12 0 19 10 1 2 29 54 30 36 3 51 -2 1 1 30 13 31 89 2 49 12 1 5 4 .92* 5 48 0 12 - 18 1 3 5 39* 3 32 O 09 9 1 2 6 1 70 63 67 O 60 -1 1 1 19 79 17 31 5 18 CD h k 1 Fo Fc weight 0 ! 65 14 67 82 0 03 1 1 1 44 30 44 46 1 23 2 1 1 9 00 7 97 48 25 3 1 1 45 76 44 13 1 13 4 1 1 8 06 8 72 65 78 5 1 1 24 58 23 OO 2 99 6 1 1 13 19 14 02 20 99 7 1 1 14 73 13 31 15 18 8 1 1 12 98 12 55 19 30 9 1 1 2 82* 0 45 0 13 10 1 1 1 75* 0 56 0 75 1 1 1 1 12 50 12 98 23 04 12 1 1 3 97* 4 43 0 13 13 1 1 21 80 21 89 6 25 14 1 1 2 85* 3 67 0 05 15 1 1 21 13 21 15 9 21 16 1 1 0 90* 3 71 0 00 17 1 1 4 58* 7 65 0 07 18 1 1 3 55* 1 34 0 62 19 1 1 5 44* 0 37 0 07 20 1 1 5 74* 5 75 0 06 20 1 0 9 82 9 75 2 96 19 1 0 9 43 9 83 3 22 18 1 0 20 33 20 44 9 69 17 1 0 1 1 96 12 40 7 56 16 1 o 26 61 26 54 3 64 15 1 0 28 60 30 74 2 52 14 1 0 35 01 35 43 2 51 13 1 0 28 90 29 19 3 00 12 1 0 59 20 60 98 0 63 1 1 1 0 59 12 59 61 0 64 10 1 o 61 89 63 17 0 60 9 1 0 51 48 53 90 0 85 8 1 0 77 75 78 21 0 40 7 1 0 79 93 81 41 0 02 6 1 0 86 19 86 32 0 02 5 1 0 18 86 18 80 8 19 4 1 0 80 30 78 18 0 02 3 1 0 45 72 44 33 1 14 2 1 0 13 68 12 52 15 65 1 1 0 38 68 35 69 0 19 0 2 0 10 40 9 7-7 26 7 1 1 2 0 107 46 109 24 0 01 2 2 0 175 72 183 90 0 OO 3 2 0 94 95 92 10 0 02 4 2 0 140 79 136 26 O 01 5 2 0 20 66 21 60 6 88 6 2 0 54 1 1 53 29 0 BO 7 2 0 67 61 64 34 0 52 h k 1 Fo Fc we 1ght 8 2 0 55 05 53 66 0 75 9 2 0 8 90 9 44 18 94 10 2 0 23 74 24 27 4 03 1 1 2 0 15 58 15 21 15 63 12 2 0 3 33* 1 12 0 09 13 2 O 3 42* 0 22 0 09 14 2 0 2 98* 1 61 0 05 15 2 0 3 83* 3 15 0 07 16 2 0 12 47 12 83 8 82 17 2 0 10 10 9 22 5 42 18 2 0 13 47 12 87 7 61 19 2 0 13 16 12 07 5 55 20 2 O 9 78 9 68 2 81 20 2 1 3 50* 2 51 0 02 19 2 1 4 78* 2 92 0 05 18 2 1 4 60* 3 59 0 06 17 2 1 2 07* 1 66 0 23 16 2 1 3 96* 2 35 0 06 15 2 1 15 31 15 89 13 62 14 2 1 2 05* 2 82 0 02 13 2 1 8 33 8 13 7 73 12 2 1 12 36 1 1 58 17 35 1 1 2 1 13 63 13 76 23 85 10 2 1 8 99 9 18 15 19 9 2 1 3 84* 4 81 0 21 8 2 1 36 14 34 98 1 50 7 2 1 10 66 10 61 38 51 6 2 1 7 16 6 30 25 95 5 2 1 6 38 6 20 27 64 4 2 1 53 92 52 03 O 81 3 2 1 1 1 98 12 38 17 74 2 2 1 28 36 25 13 2 60 1 2 1 38 20 38 00 1 58 O 2 1 42 54 40 56 1 30 - 1 2 1 13 28 13 45 1 1 91 -2 2 1 4 70 4 56 32 60 -3 2 1 109 84 1 15 59 0 01 -4 2 1 4 37 4 46 20 28 -5 2 1 14 18 14 85 15 99 -6 2 1 36 70 37 68 1 58 -7 2 1 9 62 9 97 34 22 -8 2 1 8 99 9 98 28 64 -9 2 1 14 20 12 71 27 67 10 2 1 6 20 7 25 8 79 1 1 2 1 7 51 8 85 10 32 12 2 1 12 53 12 61 19 62 13 2 1 16 57 17 12 13 27 14 2 1 1 43* 1 1 1 0 01 15 2 1 4 63* 5 17 0 10 h k 1 Fo Fc weight 16 2 1 4 04* 6 52 0 06 17 2 1 9 92 8 63 5 55 18 2 1 4 30* 1 18 0 05 19 2 1 2 66* 6 55 O 02 20 2 1 4 78* 2 85 0 04 20 2 2 4 66* 2 91 0 05 19 2 2 2 27* 0 53 0 19 18 2 2 10 92 10 86 5 37 17 2 2 7 20 7 91 2 89 16 2 2 7 45 8 36 3 54 15 2 2 9 98 9 62 7 30 14 2 2 21 77 23 35 8 15 13 2 2 33 89 34 95 2 65 12 2 2 50 14 51 37 0 83 1 1 2 2 33 49 35 14 1 47 10 2 2 59 78 60 74 0 63 -9 2 2 47 46 51 44 0 96 -8 2 2 53 73 55 65 0 78 -7 2 2 69 68 71 92 0 49 -6 2 2 108 15 1 1 1 94 0 01 -5 2 2 59 47 62 26 0 67 -4 2 2 48 51 52 73 0 99 -3 2 2 83 14 86 14 0 02 -2 2 2 60 14 62 85 0 66 - 1 2 2 105 79 1 1 1 62 0 01 0 2 2 46 87 47 88 1 07 1 2 2 44 57 45 79 1 17 2 2 2 19 13 20 37 7 95 3 2 2 56 29 53 48 0 75 4 2 2 3 6 1 3 83 9 24 5 2 2 1 14* 2 59 0 78 6 2 2 17 35 16 75 9 05 7 2 2 8 09 7 67 22 61 8 2 2 21 75 22 17 6 87 9 2 2 20 76 22 05 6 29 10 2 2 54 55 52 42 0 74 1 1 2 2 23 75 24 33 3 43 12 2 2 19 26 17 82 10 51 13 2 2 22 90 22 66 7 23 14 2 2 39 12 38 64 1 07 15 2 2 23 60 23 20 4 58 16 2 2 24 34 24 27 7 46 17 2 2 20 46 20 17 9 84 18 2 2 10 82 1 1 78 4 67 19 2 2 16 46 14 78 7 42 19 2 3 4 84* 3 47 O 04 18 2 3 4 62* 3 90 0 05 17 2 3 4 45* 6 50 0 05 16 2 3 10 48 12 38 5 44 h k 1 Fo Fc weight ^ 15 2 3 3 97* 6 09 0 98 •a (7) 14 2 3 7 40 7 30 3 88 3 13 2 3 8 81 10 25 6 26 R. . 12 2 3 9 87 9 24 10 44 H 1 1 2 3 13 45 13 03 19 02 fa 10 2 3 9 70 9 13 13 70 9 2 3 14 82 14 10 12 74 8 2 3 8 56 8 28 15 47 7 2 3 35 48 36 81 1 50 6 2 3 3 32* 2 67 0 20 5 2 3 2 52* 1 1 1 O 16 4 2 3 1 1 77 1 1 49 26 68 3 2 3 2 29* 2 96 0 19 2 2 3 17 30 15 43 7 53 1 2 3 9 24 9 35 44 04 0 2 3 9 08 9 75 46 57 - 1 2 3 31 09 30 63 2 12 -2 2 3 14 48 15 68 1 1 40 -3 2 3 3 35 3 81 8 20 -4 2 3 17 09 14 64 10 62 -5 2 3 15 90 16 23 9 40 -6 2 3 19 20 19 90 8 80 -7 2 3 9 13 9 22 26 81 -8 2 3 17 37 15 35 9 14 -9 2 3 2 93* 0 51 0 12 10 2 3 3 94* 4 49 0 17 1 1 2 3 7 46 8 26 8 67 12 2 3 14 86 14 38 17 18 13 2 3 5 59 4 37 3 65 14 2 3 4 52* 1 13 0 1 1 15 2 3 6 40 7 92 3 07 16 2 3 6 98 6 57 3 08 17 2 3 4 20* 2 50 0 06 18 2 3 6 93 7 97 2 15 19 2 3 4 62* 6 37 0 05 20 2 3 4 20* 0 95 0 04 20 2 4 6 54* 7 56 0 08 19 2 4 10 98 1 1 13 3 82 18 2 4 1 1 23 10 95 5 27 17 2 4 19 81 19 03 1 1 44 16 2 4 18 59 19 88 10 92 15 2 4 23 73 24 86 4 43 14 2 4 18 19 17 68 14 67 13 2 4 29 46 30 50 2 75 12 2 4 31 36 31 75 2 82 1 1 2 4 27 58 28 18 3 18 10 2 4 21 92 23 39 5 40 -9 2 4 51 67 51 14 0 81 CO -8 2 4 30 76 32 35 1 73 to h k 1 Fo Fc weight h k 1 Fo Fc we i ght h k 1 Fo Fc we 1ght h k 1 Fo Fc weight -7 2 4 28 .32 27 .50 3 .96 -5 2 5 10 .32 10 .45 23 . 16 15 2 6 6 . 47 5 .42 1 .82 -6 2 8 16 .64 16 . 32 19 .98 -6 2 4 13 .89 14 .23 15 .33 -6 2 5 23 .65 20 . 77 4 . 20 16 2 6 4 .80* 2 . 13 0 .04 -5 2 8 33 . 28 32 . 7 1 2 .61 -5 2 4 21 . 41 21 .07 5 .30 -7 2 5 28 . 33 27 .82 3 .61 17 2 6 4 .81* 1 .99 0 .04 -4 2 8 24 . 72 22 . 36 4 .58 -4 2 4 19 . 16 17 .72 5 . 74 -8 2 5 3 . 16* 1 .35 O . 10 16 2 7 4 .87* 1 . 37 0 .04 -3 2 8 9 . 36 7 .75 9 .36 -3 2 4 25 .02 23 .85 2 .58 -9 2 5 24 .08 24 .40 3 .57 15 2 7 5 . 48* 3 .57 0 .06 -2 2 8 24 . 18 21 .65 4 .48 -2 2 4 37 .86 32 .76 1 .47 -10 2 5 9 . 54 9 .51 11 . 39 14 2 7 4 . 45* 0 .26 0 .05 - 1 2 8 23 . 13 22 .59 4 .52 -1 2 4 5 .33 4 .05 14 .40 -11 2 5 7 . 4 1 6 .88 6 . 55 13 2 7 2 . 93 + 5 . 14 0 .02 0 2 8 32 .95 32 .02 2 .66 0 2 4 48 .36 45 .01 0 .97 -12 2 5 13 .98 13 .82 16 . 12 12 2 7 2 .71* 4 .84 0 .40 1 2 8 30 . 12 28 .03 2 . 79 1 2 4 38 .53 37 .47 1 .42 -13 2 5 8 .61 9 .07 5 , 70 1 1 2 7 4 .04* 3 . 44 0 .06 2 2 8 1 .96* 4 .84 0 .03 2 2 4 23 . 14 22 .76 5 .31 -14 2 5 1 1 .35 12 .04 8 . 23 10 2 7 5 .43* 3 .67 0 . 13 3 2 8 3 . 64* 2 . 18 0 .08 3 2 4 47 .21 45 .23 1 .OO -15 2 5 3 .97* 4 .49 0. 06 9 2 7 3 . 85* 3 .07 0 .07 4 2 8 15 .87 14 .93 18 .08 4 2 4 22 .50 23 .74 5 .07 -16 2 5 5 .81* 0 .52 0. . 1 1 8 2 7 2 .67* 5 .03 0 .04 5 2 8 1 1 .83 10 .91 10 .32 5 2 4 46 .77 48 .66 0 .99 -17 2 5 4 .38* 0 . 74 0. ,05 7 2 7 2 . 48* 0 . 38 0 .68 6 2 8 15 .57 14 .92 14. .80 6 2 4 52 .28 54 .86 0 .81 -18 2 5 4 .28* 0 .74 0, .04 6 2 7 9 . 77 8 .65 10 .20 7 2 8 5 . 17* 2 .45 0. . 13 7 2 4 50 .08 51 .20 0 .86 -19 2 5 4 .66* 1 . 10 0, ,05 5 2 7 17 .64 18 .61 10 . 59 8 2 8 8 .54 9 . 77 4 .95 8 2 4 43 .50 43 .38 1 .06 -19 2 6 6 . 15 6 . 33 1, .09 4 2 7 7 . 23 9 .46 6 .51 9 2 8 4 .05* 0 .61 0. .06 9 2 4 33 .55 35 .87 1 .45 -18 2 6 9 .56 9 . 16 2 , 90 3 2 7 10 . 27 8 .71 13. . 1 1 10 2 8 5 . 48* 2 . 13 0, . 1 1 10 2 4 35 .86 36 .33 1 .27 -17 2 6 1 1 . 70 1 1 . 28 5, 26 2 2 7 9 . 4 1 9 .95 12 .02 1 1 2 8 4 .38* 7 . 34 0. ,05 1 1 2 4 45 .55 48 .34 0 .93 -16 2 6 2 . 13* 2 68 0, , 22 1 2 7 2 .75* 4 . 82 0 .06 12 2 8 4 .98* 6 .65 1 . , 13 12 2 4 30 .95 31 .94 2 .56 -15 2 6 8 .68 8 . 14 4 . ,03 0 2 7 4 .00* 3 . 29 0. . 15 13 2 8 1 .69* 4 .04 0. 1 1 13 2 4 19 .33 19 .88 9 .67 -14 2 6 1 1 .50 9 .79 7. 55 - 1 2 7 7 . 72 6 .50 9 . 15 14 2 8 4 . 32* 6 . 44 0. 04 14 2 4 20 .28 20 .36 6 .97 -13 2 6 4 . 39* 3 .45 1 . 37 -2 2 7 15 . 99 16 .99 14 . 91 13 2 9 6 . 39* 4 .03 0. 08 15 2 4 22 .48 21 .29 7 .81 -12 2 6 13 .93 13 . 18 12. 64 -3 2 7 3 . 27* 2 . 39 0. .09 12 2 9 4 . 70* 0 .52 0. ,05 16 2 4 9 .58 10 .03 4 . 24 -11 2 6 5 .51 5 .23 3. 06 -4 2 7 1 . 48* 4 .23 0 .02 1 1 2 9 3 .93* 0 .39 0. .04 17 2 4 1 1 .09 9 .95 4 .37 -10 2 6 1 1 .52 12 .29 13. 37 -5 2 7 17 .51 16 . 25 1 1 . 99 10 2 9 1 . 94* 4 .54 0. 18 18 2 4 5 . 19* 6 .04 0 .05 -9 2 6 17 .81 18 . 34 11 . ,06 -6 2 7 13 .93 13 . 33 14 92 9 2 9 5 .21* 3 . 55 0. ,08 18 2 5 4 .52* 3 .68 0 .04 -8 2 6 6 .94 5 .65 6. 61 -7 2 7 3 .52* 0 .68 0, .08 8 2 9 3 .67* 2 . 15 0 ,04 17 2 5 4 .69* O .75 0 .05 -7 2 6 7 .89 6 .89 9. 45 -8 2 7 9 . 72 9 . 55 9 .91 7 2 9 2 .90* 1 . 32 0 ,51 16 2 5 2 . 18* 1 .82 0 .21 -6 2 6 21 .84 21 .50 5 , 66 -9 2 7 3 .59* 4 . 43 1 35 6 2 9 2 .23* 1 .89 0 .02 15 2 5 4 .34* 1 .98 O .05 -5 2 6 28 . 97 27 .02 3 . 51 -10 2 7 3 . 76* 4 .OO 0 .07 5 2 9 4 . 38* 9 . 72 0 .07 14 2 5 7 .25 7 .67 3 .02 -4 2 6 27 .59 28 .30 3. 66 -1 1 2 7 9 . 1 1 8 . 37 6 .09 4 2 9 1 1 . 30 1 1 .69 7, .95 13 2 5 3 .93* 3 .39 0 .06 -3 2 6 28 .57 28 .75 3 . 65 -12 2 7 6 . 16 6 . 28 2, .49 3 2 9 3 .96* 6 .08 O .06 12 2 5 3 . 13* 0 .87 0. .04 -2 2 6 31 .00 30 . 10 1 . 72 - 13 2 7 4 . 13* 3 . 95 0, ,06 2 2 9 3 .86* 3 . 15 0 .07 1 1 2 5 1 .67* 0 .67 0. .27 -1 2 6 54 . 12 51 . 83 O. 76 - 14 2 7 1 1 . 18 1 1 .95 6 07 1 2 9 2 . 55* 3 . 96 0. .03 10 2 5 3 .47* 0 67 0. 08 0 2 6 43. .73 39. .44 1 . 07 - 15 2 7 5 .85 6 . 23 1 .63 0 2 9 3 .59* 6 . 94 O, .05 9 2 5 6 .22 7. 33 5. 25 1 2 6 41 86 39, . 35 1 . 15 -16 2 7 6 .52 6 .99 1 , . 77 - 1 2 9 10 . 23 1 1 . 24 7 , 69 8 2 5 15 .32 15. 26 •20. 91 2 2 6 37 .30 35. .30 1 . 34 -17 2 7 4 . 76* 3 . 73 0 .04 -2 2 9 3 .87* 6 .54 0. 07 7 2 5 5. 68 7. 73 5. 71 3 2 6 55 . 16 54, .29 0. 72 -18 2 7 4 . 72* 2 . 4 1 0 .04 -3 2 9 3 .83* O . 72 0. 07 6 2 5 3. .11* 4. 87 0. 10 4 2 6 39 . 19 40, 92 1 . 22 -17 2 8 2 .80* 0 . 16 0 .01 -4 2 9 5 . 32* 4 . 34 0. 13 5 2 5 1 1 . ,43 12. 14 23. 86 5 2 6 41 .44 40, .73 1 . 12 -16 2 8 4 . 75* 0 .82 0, .04 -5 2 9 4 .03* 5 .96 0. 07 4 2 5 14. 01 14. 52 20. 07 6 2 6 27 .28 27, . 1 1 3. 28 -15 2 8 6 . 26* 4 .62 0, 09 -6 2 9 4 .17* 3 . 32 O. 07 3 2 5 9. .86 9. 94 21 . 47 7 2 6 15. .60 16, .62 16 . 42 -14 2 8 3 . 70* 1 .87 0 .64 -7 2 9 4 .01* 6 .90 0. 06 2 2 5 1 1 . 45 1 i . 48 32. 15 8 2 6 29 .34 29 .55 2 . 96 - 13 2 8 5 .97 6 . 42 1 .83 -8 2 9 4 .05* 1 .04 0 06 1 2 5 7. .33 5. 90 16. 89 9 2 6 23 .54 25. .82 5. 74 -12 2 8 9 .95 10 .56 5 25 -9 2 9 4 . 13* 5 . 44 0. 06 0 2 5 20. . 18 19. 79 5 . 16 10 2 6 1 1 . 48 10 . 44 10. 26 - 1 1 2 8 1 1 . 75 12 . 32 7 . 67 -10 2 9 5 . 29 4 .42 1 . . 53 -1 2 5 4 . 86 4. 59 8 52 1 1 2 6 8 .65 8 .69 5. 35 -10 2 8 10 .04 9 . 76 6 39 - 1 1 2 9 4 . 19* 2 . 82 o 06 -2 2 5 1 .95* 1 . .77 0 .07 12 2 6 9 .85 9 .00 6 02 -9 2 8 15 . 30 15 . 29 13. 62 - 12 2 9 4 . 40* 2 . 39 0 05 -3 2 5 9 .02 8 .74 24 .07 13 2 6 4 . 29* 1 .88 0. 06 -8 2 8 22 .60 22 .04 4 . 99 -13 2 9 5 .95* 2 .09 0 . 10 -4 2 5 9 .02 7 . 40 22. . 23 14 2 6 4 . 33* 3 .82 0. 05 -7 2 8 13 . 22 12 . 55 14 . 14 - 14 2 9 4 . 84* 4 . 09 0 . 83 h k l Fo Fc weight 15 2 9 4 72* 2 49 0 04 16 2 9 4 79* 0 35 0 04 14 2 10 4 86* 3 74 0 04 13 2 10 4 69* 1 69 0 05 12 2 10 1 44* 1 72 0 00 1 1 2 10 4 45* 7 45 0 05 10 2 10 13 44 12 29 7 03 -9 2 10 7 91 7 52 2 84 -8 2 10 5 91* 8 01 0 10 -7 2 10 8 54 6 76 3 67 -6 2 10 4 62* 1 90 0 08 -5 2 10 4 25* 2 43 0 06 -4 2 10 14 77 14 03 10 52 -3 2 10 9 32 8 17 4 85 -2 2 10 4 13* 4 20 0 06 - 1 2 10 5 42* 2 96 0 1 1 0 2 10 4 34* 1 88 0 07 1 2 10 4 99* 3 85 0 09 2 2 10 1 59* 0 37 0 01 3 2 10 3 93* 6 58 0 06 4 2 10 4 28* 5.88 0 05 5 2 10 3 29* 4 77 0 03 6 2 10 4 01* 2 49 0 80 7 2 10 5 95 6 16 1 64 8 2 10 4 48* 8 15 0 05 9 2 10 6 79 6 16 1 64 10 2 10 4 68* 3 96 0 05 11 2 10 4 77* 3 84 o 04 8 2 11 4 75* 1 64 0 04 7 2 11 6 23* 0 54 0 08 6 2 11 0 57* 0 91 0 01 5 2 11 4 59* 1 34 o 05 4 2 11 4 42* 1 68 0 05 3 2 11 4 41* 2 17 0 05 2 2 11 2 58* 2 43 0 02 1 2 11 4 12* 3 54 0 05 0 2 11 4 39* 1 31 0 05 -1 2 11 4 37* 0 96 0 05 -2 2 11 2 14* 2 49 0 22 -3 2 11 4 82* 2 87 0 06 -4 2 11 1 39* 4 54 0 09 -5 2 11 5 49 5 88 1 36 -6 2 11 1 39* 4 16 0 01 -7 2 11 4 57* 0 70 0 05 -8 2 11 4 59* 1 66 0 05 -9 2 11 3 51* 0 63 0 03 10 2 11 4 79* 1 62 0 04 1 1 2 11 5 06* 5 57 0 78 12 2 11 3 08* 0 67 0 28 h k 1 Fo Fc we ight -8 2 12 4 82* 3 10 0 04 -7 2 12 4 79* 1 77 0 04 -6 2 12 5 48* 2 08 0 97 -5 2 12 1 00* 1 57 0 03 -4 2 12 4 70* 4 59 0 05 -3 2 12 6 47* 3 98 0 09 -2 2 12 3 96* 0 65 0 03 -1 2 12 2 57* 0 50 0 22 0 2 12 6 40* 4 40 0 09 1 2 12 5 45* 2 33 0 06 2 2 12 3 74* 6 32 0 03 3 2 12 4 88* 8 59 0 04 4 2 12 5 78* 2 98 0 06 5 2 12 4 82* 2 33 0 04 3 3 12 4 93* 1 66 0 04 2 3 12 4 87* 1 44 0 04 1 3 12 4 78* 2 45 0 04 0 3 12 6 33* 3 08 0 08 -1 3 12 6 23 5 05 1 24 -2 3 12 5 58* 5 74 0 06 -3 3 12 4 64* 4 40 0 04 -4 3 12 2 36* 2 66 , o 17 -5 3 12 6 87 4 18 1 46 -6 3 12 5 46* 5 7 1 0 06 -7 3 12 4 89* 2 66 0 04 - 1 1 3 1 1 3 00* 4 12 0 02 -10 3 1 1 5 00* 1 67 0 05 -9 3 11 4 72* 0 79 0 04 -8 3 11 1 02* 1 34 0 OO -7 3 1 1 4 53* 0 29 0 05 -6 3 1 1 4 57* 2 82 0 05 -5 3 1 1 6 09* 2 22 0 09 -4 3 1 1 5 64* 2 80 0 09 -3 3 1 1 4 36* 0 47 0 05 -2 3 1 1 4 82* 3 55 1 06 - 1 3 1 1 4 49* 4 30 0 05 0 3 1 1 4 41* 0 99 0 05 1 3 1 1 2 19* 0 56 0 21 2 3 1 1 4 52* 1 58 0 05 3 3 1 1 4 53* 1 86 0 05 4 3 1 1 4 62* 0 95 0 05 5 3 1 1 2 89* 1 25 0 02 6 3 1 1 4 72* 0 27 0 04 7 3 1 1 4 82* 0 65 0 04 10 3 10 4 65* 2 14 0 05 9 3 10 6 38* 3 46 0 09 8 3 10 5 92* 6 24 0 07 7 3 10 4 51* 3 26 0 05 6 3 10 4 51* 2 21 0 05 h k l Fo Fc weight 5 3 10 8 81 8 14 3 55 4 3 10 9 24 8 65 3 98 3 3 10 7 99 6 52 3 26 2 3 10 8 49 6 65 3 68 1 3 10 1 1 04 10 4 1 6 27 0 3 10 12 22 10 24 7 46 - 1 3 10 1 1 90 1 1 14 7 26 -2 3 10 7 39 8 42 2 99 -3 3 10 14 45 13 79 9 94 -4 3 10 1 1 26 12 07 6 60 -5 3 10 2 07* 1 56 0 23 -6 3 10 9 68 10 47 4 66 -7 3 10 5 54* 3 40 0 09 -8 3 10 2 14* 2 96 0 22 -9 3 10 6 18* 4 54 0 10 -10 3 10 4 66* 2 88 0 06 - 1 1 3 10 4 65* 6 53 0 05 -12 3 10 4 74* 2 36 0 04 -13 3 10 5 94* 3 95 0 07 -15 3 9 4 88* 1 99 0 04 -14 3 9 4 30* 3 13 0 60 -13 3 9 6 37* 1 20 O 09 -12 3 9 3 44* 4 91 0 51 - 1 1 3 9 2 73* 0 94 0 02 -10 3 9 2 10* 1 84 0 23 -9 3 9 6 10 5 88 2 10 -8 3 9 4 66* 3 90 1 31 -7 3 9 5 36 5 08 1 81 -6 3 9 4 65* 2 91 1 41 -5 3 9 4 12* 1 90 0 07 -4 3 9 1 1 87 12 39 8 83 -3 3 9 17 12 17 22 9 74 -2 3 9 3 98* 6 75 0 06 - 1 3 9 3 89* 1 32 0 07 0 3 9 5 60 6 33 2 31 1 3 9 5 22* 0 63 O 1 1 2 3 9 8 29 7 75 4 62 3 3 9 4 02* 0 78 0 06 4 3 9 4 07* 4 03 0 06 5 3 9 2 00* 0 99 0 25 6 3 9 5 24* 4 80 0 09 7 3 9 9 04 9 76 4 24 8 3 9 4 24* 1 96 0 06 9 3 9 4 35* 1 20 O 05 10 3 9 3 48* 1 79 0 03 1 1 3 9 2 9 1 * 2 16 0 02 12 3 9 5 77* 1 13 0 07 14 3 8 6 42 7 22 1 22 13 3 8 2 07* 3 44 0 01 h k 1 Fo Fc we 1ght l u *« 12 3 8 6 63 6 84 1 63 "a n> 1 1 3 8 9 00 9 25 3 77 3 10 3 8 12 21 1 1 45 7 02 ft. s-9 3 8 7 12 5 72 2 93 8 3 8 15 62 15 48 12 OO fa 7 3 8 21 61 23 10 7 35 6 3 8 12 04 1 1 66 8 85 5 3 8 25 21 25 63 5 00 4 3 8 26 43 26 17 2 47 3 3 8 15 53 16 28 15 25 2 3 8 7 74 7 81 5 74 1 3 8 1 75* 2 1 1 0 33 0 3 8 3 62* 5 44 0 08 - 1 3 8 13 28 12 52 15 31 -2 3 8 10 20 1 1 32 9 90 -3 3 8 5 06* 1 55 0 15 -4 3 8 1 1 80 1 1 98 12 46 -5 3 8 3 71* 5 58 0 07 -6 3 8 13 22 12 78 12 03 -7 3 8 5 37* 0 59 6 13 -8 3 8 4 14* 3 99 1 28 -9 3 8 .0 62 9 28 7 10 -10 3 8 1 1 63 10 42 7 70 - 1 1 3 8 2 25* 6 43 0 02 -12 3 8 12 62 10 79 7 46 -13 3 8 3 74* 10 51 0 04 -14 3 8 9 21 9 17 3 40 -15 3 8 6 51* 6 41 0 09 -16 3 8 4 77* 4 48 0 04 -17 3 7 4 72* 1 32 0 04 -16 3 7 6 07* 8 06 0 08 -15 3 7 IO 24 9 78 4 51 -14 3 7 4 26* 1 42 O 05 -13 3 7 3 47* 2 64 O 04 -12 3 7 4 10* 1 35 0 06 - 1 1 3 7 9 27 9 24 5 53 - 10 3 7 3 90* 0 91 0 07 -9 3 7 7 29 6 61 4 45 -8 3 7 12 92 13 27 14 12 -7 3 7 5 06* 8 72 0 15 -6 3 7 3 86* 3 59 1 78 -5 3 7 3 46* 4 62 0 08 -4 3 7 1 1 50 10 48 15 16 -3 3 7 3 40* 6 07 0 09 -2 3 7 4 33* 2 90 0 16 - 1 3 7 3 45* 3 99 O 08 0 3 7 6 06 7 37 5 15 1 3 7 1 1 06 9 62 14 83 2 3 7 5 49 7 01 3 86 h k 1 Fo Fc weight h k 1 Fo Fc weight h k 1 Fo Fc we 1ght h k 1 Fo Fc weight 3 3 7 3 51* 4 .90 0. 08 -18 3 5 7 .60 6 .45 2 .00 5 3 4 17 . 29 19 .06 12 . 29 4 3 3 19 .88 19 . 79 5 . 13 4 3 7 8 . 1 1 7 .01 7. ,37 -17 3 5 9 .21 9 .54 3 .58 4 3 4 20 .23 20 . 35 6 .94 5 3 3 13 . 17 13 .03 15 .66 5 3 7 11 . 95 12 .21 13 62 -16 3 5 13 .40 13 .02 7 .98 3 3 4 56 .64 61 . 54 0 . 7 1 6 3 3 7 .60 7 .33 14 .09 6 3 7 17. 44 17 .52 11 . 45 -15 3 5 1 .60* 2 . 1 1 O .01 2 3 4 57 .97 60 .53 0, .69 7 3 3 4 .42 4 .66 4 . 34 7 3 7 4. 98 5 .89 2 11 -14 3 5 4 .00* 3 . 78 O .06 1 3 4 70 .71 71 . 20 0 .48 8 3 3 14 .52 15 . 29 17 .04 8 3 7 7 . 44 8 .55 4. 31 -13 3 5 5 .34* 7 .07 0 . 13 0 3 4 63 . 34 64 .81 0 .58 9 3 3 28 .85 28 . 35 3 .33 9 3 7 1 . .25* 1 .32 0 01 -12 3 5 18 .76 19 .06 9 .07 - 1 3 4 61 .34 63 . 73 0 .62 10 3 3 14 .49 14 .51 20 .44 10 3 7 2 .98* 2 .95 0. 60 -1 1 3 5 6 . 28 6 .81 4 .31 -2 3 4 25 .99 27 .49 4 .62 11 3 3 3 .52* 4 .45 O .08 1 1 3 7 4 .86* 3 .59 0. 08 -10 3 5 3 .04* 6 .68 0 .06 -3 3 4 51 .83 53 .45 0 84 12 3 3 8 .43 7 .82 6 .87 12 3 7 3 .97* 3 .36 0. 05 -9 3 5 5 .76 4 .81 4 .64 -4 3 4 58 .62 60 .40 0 67 13 3 3 6 .24 5 .73 3 .08 13 3 7 4 .40* 0 .71 0 05 -8 3 5 2 . 15* 4 .00 0 . 74 -5 3 4 62 .03 60 . 25 0 60 14 3 3 9 . 34 8 .82 5 .56 14 3 7 2 .50* 0 .92 O. 01 -7 3 5 24 .92 24 . 36 3 . 7 1 -6 3 4 4 1 . 27 42 .84 1 20 15 3 3 4 . 16* 4 .83 0 06 15 3 7 2 .77* 3 .08 0 24 -6 3 5 23 .91 23 . 38 5 89 -7 3 4 42 . 26 42 .45 1 14 16 3 3 3 .46* 2 .02 0 03 16 3 6 3 .46* 3 .52 0. ,02 -5 3 5 2 .96* 1 .69 O . 1 1 -8 3 4 39 . 17 38 .60 1 . 25 17 3 3 4 . 36* 3. .94 0 05 15 3 6 12 48 12 .41 5 13 -4 3 5 1 . 15* 2 . 13 o 02 -9 3 4 40 .95 41 . 22 1 . 15 18 3 3 4 .81* 3 .97 0 .04 14 3 6 16 .85 16 .33 10 .29 -3 3 5 5 . 32 4 .55 7 . 1 1 -10 3 4 16 . 72 16 .44 1 1 . 89 19 3 3 4 .90* 4 .52 0 .04 13 3 6 18 . 19 19 .78 9 .35 -2 3 5 18 .00 18 .70 9 . 15 - 1 1 3 4 8 . 32 8 .93 8 75 19 3 2 1 .05* 0 .79 0 OO 12 3 6 20 .08 19 .34 8 .24 - 1 3 5 6 .26 6 .56 10. 09 -12 3 4 18 . 74 18 . 25 9. 24 18 3 2 6 .47* 0 .50 0 .09 11 3 6 11 .81 12 .05 8 .29 0 3 5 12 .67 12 .90 28 .09 -13 3 4 1 . 46* 2 .09 0. .01 17 3 2 7 .57 8 . 23 2 56 10 3 6 17 .81 17 .77 13 .80 1 3 5 11 .05 1 1 . 34 25 OO - 14 3 4 3 .38* 0 .63 0. .05 16 3 2 9 . 78 10 .02 4 .85 9 3 6 19 .51 20 .89 9 . 34 2 3 5 1 .62* 2 . 25 0 .04 -15 3 4 4 .OO* 0 . 57 0. 06 15 3 2 4 . 70* 4 .71 1 .40 8 3 6 3 .54* 2 .53 0 .08 3 3 5 3 .75* 2 . 22 0 . 19 - 16 3 4 4 . 18* 2 . 22 0. 06 14 3 2 3 . 25* 2 .02 0 .05 7 3 6 17 .51 19 .71 8 .99 4 3 5 12 .20 1 1 .84 23 .67 - 17 3 4 8 .64 8 . 39 3 .54 13 3 2 23 .85 23 .00 5 .28 6 3 6 15 .39 15 .89 20 .99 5 3 5 3 .03* 0 . 16 0. . 1 1 - 18 3 4 3 .76* 3 . 16 0. .04 12 3 2 2 .86* 5 .70 0 .92 5 3 6 4 .84 4 .09 3 .34 6 3 5 3 . 17* 1 .43 0 . 10 - 19 3 4 4 . 75* 1 .51 0 .04 1 1 3 2 31 .51 31 .28 2. .88 4 3 6 8 .31 9 .61 10, .04 7 3 5 7 .25 6 . 73 7. 83 -20 3 3 4 .83* 0. .63 0. .04 10 3 2 56 .81 57 .86 0 .68 3 3 6 3 .23* 5 .04 0 . 10 8 3 5 7 .01 6 . 24 6 . 47 -19 3 3 4 . 70* 5 . 14 0 .05 9 3 2 43 .30 42 .43 1 .07 2 3 6 3 . 16* 0 .71 0 . 10 9 3 5 3 .64* 2 .86 1 .65 - 18 3 3 3 .97* 0 .89 0. .04 8 3 2 53 . 15 51 . 20 0 .78 1 3 6 7 .22 8 .44 9 .22 10 3 5 3 .60* 5 . 32 O .08 -17 3 3 8 .95 8 .91 3 89 7 3 2 60 . 33 60 .20 0 .63 0 3 6 16 .23 15 .26 13 68 11 3 5 3 .80* 1 . 33 0 .07 -16 3 3 4 . 12* 2 .08 0. .06 6 3 2 82 .03 76 .81 0 .36 -1 3 6 9 .22 9 .53 14 .60 12 3 5 1 . 29* 3 .55 o . . 12 - 15 3 3 4 .02* 0 .8 1 0. .06 5 3 2 77 .37 74 .60 0 .40 -2 3 6 19 . 75 19 .00 7 .79 13 3 5 4 .08* 1 .69 o .06 - 14 3 3 10 . 10 9 . 54 7 . 73 4 3 2 64 . 44 63 . 18 0 .57 -3 3 6 35 .67 34 . 19 1 .40 14 3 5 5 .83 4 .33 1 89 - 13 3 3 10 .70 11 . 72 10. 78 3 3 2 63 .52 59 . 19 0 .59 -4 3 6 35 .42 33 .22 1 .40 15 3 5 5 . 13* 2 . 77 1. .25 -12 3 3 1 . 12* 2 .49 0. .01 2 3 2 95 .07 95 63 0. 02 -5 3 6 26 .73 26 .53 3 .48 16 3 5 4 . 29* 1 . 38 o .04 - 1 1 3 3 2 . 95* 4 .84 0. 07 1 3 2 57 .83 59 .91 0. . 7 1 - 6 3 6 26 .74 27 . 18 3 .43 17 3 5 3 .91* 3 . 49 0 .03 - 10 3 3 12 .59 12 . 72 21 . 71 0 3 2 60 .94 61 89 0. .64 -7 3 6 35 .78 35 .73 1 .29 18 3 4 4 .58* 5 .82 0 .04 -9 3 3 13 .66 13 . 27 27. .67 -1 3 2 47 . 76 50 .73 1. .01 -8 3 6 38 .56 39 . 16 1 . 18 17 3 4 13 .83 13 . 34 5 .96 -8 3 3 21 . 10 20 .45 6 60 -2 3 2 62 . 16 62 . 18 0. 62 -9 3 6 15 .31 14 .98 14 .47 16 3 4 12 .77 12 .94 6 .56 -7 3 3 22 .93 23 . 15 4 . 61 -3 3 2 44 .61 43 . 18 1. . 13 10 3 6 10 .83 1 1 .27 11 .06 15 3 4 10 .48 10 . 12 5 . 33 -6 3 3 5 .80 5 .61 12 . 12 -4 3 2 31 .64 31 . 15 1. 98 1 1 3 6 27 .49 27 .39 3 93 14 3 4 8 .64 7 . 24 4 . 36 -5 3 3 29 .04 29 .51 2 .08 -5 3 2 18 .88 19 .75 6 . 01 12 3 6 7 .97 7 .06 4 , .62 13 3 4 9 .41 10 . 72 5. . 76 -4 3 3 19 .83 19 . 76 5 89 -6 3 2 62 .46 61 .04 0. .60 13 3 6 22 .31 22 .30 6 50 12 3 4 8 . 19 7 . 47 5 . 10 -3 3 3 28 . 17 29 .04 2 25 -7 3 2 31 .59 30 .68 1. 81 14 3 6 23 .94 23 .51 6 28 1 1 3 4 10 . 20 9 .45 9 .87 -2 3 3 6 .05 5 . 15 20. .60 -8 3 2 1 1 . 29 10 . 33 28 39 15 3 6 12 20 13 . 39 6 55 10 3 4 3 .07* 0 .61 O .06 - 1 3 3 9 .95 9 .66 42 . .73 -9 3 2 7 . 77 9 .61 12 88 16 3 6 8 40 8 .27 3 .07 9 3 4 2 . 18* 2 .54 0 67 0 3 3 7 . 49 8 . 75 30 56 -10 3 2 24 . 18 26 .33 3 .81 17 3 6 7 . 92 6 .61 2 . 23 8 3 4 1 1 .38 10 . 57 17 26 1 3 3 7 . 10 6 . 93 26 . 92 - 1 1 3 2 21 .61 23 . 50 7 OO 18 3 6 3 .62* 4 .90 0 03 7 3 4 26 .75 27 . 34 3 .55 2 3 3 18 . 78 20 .55 9 43 - 12 3 2 20 .06 20 .67 6 .27 19 3 5 4 .80* 3 .35 0. 04 6 3 4 17 .63 17 . 26 1 1 . .56 3 3 3 4 .81 1 . 79 10. 50 - 13 3 2 17 . 35 17 . 89 14 .84 h k 1 Fo Fc weight 14 3 2 10 11 8 92 8 15 15 3 2 23 49 24 79 4 84 16 3 2 22 34 21 67 7 43 17 3 2 1 1 10 1 1 70 5 97 18 3 2 22 01 23 12 4 78 19 3 2 14 08 14 25 6 02 20 3 2 4 23* 6 92 0 03 20 3 1 4 76* 0 86 0 04 19 3 1 4 08* 3 30 0 04 18 3 1 2 87* 0 76 0 39 17 3 1 2 51* 5 99 O 02 16 3 1 10 26 1 1 10 6 29 15 3 1 3 82* 0 .46 0 07 14 3 1 3 76* 1 40 1 28 13 3 1 8 67 9 22 8 23 12 3 1 4 24* 0 56 0 16 1 1 3 1 7 13 5 .67 8 04 10 3 1 2 55* 3 02 0 08 -9 3 1 3 63 3 96 3 37 -8 3 1 3 47 2 71 3 79 -7 3 1 1 37* 2 58 0 05 -6 3 1 44 59 44 56 1 1 1 -5 3 1 41 93 41 83 1 25 -4 3 1 22 29 22 65 6 23 -3 3 1 24 95 22 70 2 89 -2 3 1 35 20 38 07 1 75 -1 3 1 27 42 26 63 2 61 0 3 1 7 32 6 79 45 41 1 3 1 4 51 3 00 18 85 2 3 1 16 10 13 42 12 07 3 3 1 29 74 26 86 2 22 4 3 1 33 99 32 74 1 76 5 3 1 34 76 32 58 1 68 6 3 1 5 00 4 45 10 06 7 3 1 8 94 9 01 23 66 8 3 1 18 75 17 39 8 80 9 3 1 12 84 13 48 15 62 10 3 1 3 20* 2 40 0 10 1 1 3 1 3 31* 1 09 0 09 12 3 1 3 45* 1 31 0 08 13 3 1 14 43 15 04 16 49 14 3 1 10 80 10 62 8 36 15 3 1 5 40 5 90 1 93 16 3 1 4 08* 1 72 O 06 17 3 1 10 34 11 56 4 95 18 3 1 13 38 12 64 6 67 19 3 1 7 59 6 95 1 88 20 3 0 7 7 1 7 26 1 75 19 3 0 10 78 1 1 34 3 59 h k 1 Fo Fc weight 18 3 0 11 .23 10 1 1 5 17 17 3 O 16 .46 16 07 10 67 16 3 0 27 . 32 27 42 4 36 15 3 0 26 .87 26 19 4 66 14 3 0 33 55 32 1 1 2 48 13 3 0 32 .81 32 31 2 64 12 3 0 50 .75 49 75 0 80 11 3 0 36 .38 36 41 1 30 10 3 0 51 .81 50 75 0 80 9 3 0 38 .49 37 13 1 31 8 3 0 79 16 76 33 0 38 7 3 0 10 .65 1 1 03 32 31 6 3 0 45 1 1 43 55 1 08 5 3 0 74 80 68 95 0 43 4 3 0 20 .95 19 47 6 43 3 3 0 59 .44 57 32 0 67 2 3 0 66 .62 65 61 0 06 1 3 0 47 17 45 19 1 05 0 4 0 76 63 80 32 0 41 1 4 0 65 86 63 54 0 55 2 4 0 40 02 4 1 14 1 35 3 4 0 27 01 28 39 2 32 4 4 0 109 24 103 28 0 01 5 4 0 74 77 73 06 0 43 6 4 0 73 94 70 54 O 43 7 4 0 32 20 31 26 1 66 8 4 0 23 45 22 37 3 98 9 4 0 13 13 13 98 16 58 10 4 0 16 20 16 01 15 61 1 1 4 0 3 38* 3 42 0 09 12 4 0 1 98* 0 91 0 45 13 4 0 1 68* 4 27 O 01 14 4 0 10 81 10 96 7 59 15 4 0 1 81* 2 1 1 0 01 16 4 0 15 86 14 37 10 59 17 4 0 7 85 8 45 2 68 18 4 0 4 69* 2 94 0 05 19 4 0 5 69* 5 93 0 97 19 4 1 5 87* 2 55 O 07 18 4 1 4 64* 1 87 0 05 17 4 1 4 61* 0 70 0 06 16 4 1 4 26* 2 06 O 05 15 4 1 2 01* 1 97 O 25 14 4 1 5 13* 6 01 0 10 13 4 1 3 79* 0 54 0 07 12 4 1 1 1 94 1 1 58 12 85 1 1 4 1 3 47* 2 61 O 08 10 4 1 5 02 4 79 3 6 1 9 4 1 1 1 94 12 74 19 69 h k 1 Fo Fc weight 8 4 1 1 1 36 1 1 05 21 02 7 4 1 15 69 15 21 18 80 6 4 1 16 66 16 31 9 14 5 4 1 10 77 10 30 31 81 4 4 1 13 50 13 34 16 76 3 4 1 13 10 13 69 23 72 2 4 1 43 34 39 95 1 18 1 4 1 3 84 2 59 8 39 O 4 1 9 16 8 48 39 12 -1 4 1 51 43 51 90 0 87 -2 4 1 2 38* 2 68 0 18 -3 4 1 23 06 21 05 5 48 -4 4 1 28 40 32 05 2 14 -5 4 1 31 60 31 18 1 86 -6 4 1 4 32 7 55 6 89 -7 4 1 37 25 39 75 1 40 -8 4 1 9 98 9 95 20 45 -9 4 1 23 67 25 44 3 89 - 10 4 1 2 1 55 21 92 5 26 - 1 1 4 1 9 37 10 12 1 1 63 -12 4 1 10 77 1 1 03 12 44 -13 4 1 3 13* 5 81 0 05 -14 4 1 3 79* 1 74 0 07 -15 4 1 15 61 16 12 12 77 -16 4 1 10 61 10 88 6 00 -17 4 1 9 24 8 79 4 08 - 18 4 1 5 95* 7 68 0 08 - 19 4 1 6 62 4 49 1 47 -19 4 2 2 33* 1 64 0 01 -18 4 2 2 47* 2 70 0 01 -17 4 2 8 39 7 92 3 29 -16 4 2 10 70 10 07 6 10 -15 4 2 6 36 8 08 2 54 -14 4 2 25 94 24 83 5 09 -13 4 2 16 87 16 95 10 69 -12 4 2 30 44 31 16 2 82 - 1 1 4 2 24 21 26 49 4 78 -10 4 2 45 32 45 46 0 98 -9 4 2 38 34 40 57 1 27 -8 4 2 39 72 4 1 57 1 24 -7 4 2 36 31 39 70 1 44 -6 4 2 36 62 37 94 1 45 -5 4 2 64 80 68 52 0 56 -4 4 2 67 98 73 59 0 51 -3 4 2 83 90 85 95 0 34 -2 4 2 45 09 48 82 1 09 - 1 4 2 24 59 27 28 5 19 0 4 2 37 10 39 76 1 51 1 4 2 42 69 44 51 1 20 h k 1 Fo Fc weight "a 2 4 2 28 04 28 28 2 23 "13 ni 3 4 2 7 39 9 1 1 20 OO 3 4 4 2 10 06 9 34 29 16 ft. H 5 4 2 7 82 8 08 16 96 6 4 2 21 57 18 32 4 35 t ) 7 4 2 14 27 12 78 13 80 8 4 2 29 05 26 81 3 34 9 4 2 3 28* 2 84 0 09 10 4 2 16 38 15 06 13 03 1 1 4 2 9 36 8 51 9 18 12 4 2 27 85 26 66 2 73 13 4 2 27 63 26 79 2 46 14 4 2 25 50 25 09 5 65 15 4 2 24 09 23 15 5 08 16 4 2 16 75 16 27 10 56 17 4 2 23 03 22 19 4 72 18 4 2 18 12 16 62 8 37 19 4 2 5 64* 5 94 0 05 18 4 3 4 76* 4 20 0 04 17 4 3 4 65* 5 75 0 05 16 4 3 5 37* 3 93 0 08 15 4 3 3 79* 3 24 0 05 14 4 3 5 86* 7 16 0 1 1 13 4 3 4 32* 3 34 0 08 12 4 3 9 24 9 75 6 25 1 1 4 3 12 25 1 1 52 12 71 10 4 3 15 07 14 63 19 59 9 4 3 8 25 7 05 8 56 8 4 3 4 54* 1 48 0 18 7 4 3 4 15* 4 71 0 16 6 4 3 18 67 16 66 7 67 5 4 3 4 72 3 13 4 90 4 4 3 8 21 8 29 15 59 3 4 3 17 14 16 96 10 05 2 4 3 26 03 24 87 4 54 1 4 3 32 02 30 75 1 81 0 4 3 33 74 33 67 1 71 - 1 4 3 4 62 5 17 8 97 -2 4 3 2 64* 4 19 O 14 -3 4 3 10 12 9 63 24 75 -4 4 3 16 43 15 86 10 15 -5 4 3 2 85* 1 55 0 12 -6 4 3 1 33* 0 81 O 03 -7 4 3 9 16 7 99 16 71 -8 4 3 5 4 1 5 60 5 64 -9 4 3 5 60 6 05 5 21 - 10 4 3 4 1 1 * 3 19 0 14 - 1 1 4 3 5 80 5 78 4 30 C O -12 4 3 3 58* 1 19 0 08 h k 1 Fo Fc w e i g h t h k 1 Fo Fc w e 1 g h t h k 1 Fo Fc w e t g h t h k 1 Fo Fc w e 1 g h t 13 4 3 5 . 18* 1 .83 0 . 14 12 4 5 1 . 29* 3 .76 0. ,01 0 4 6 28 .88 30 .85 3. .33 -16 4 8 2 . 13* 7 .42 0 .01 14 4 3 17 .59 19 .33 12 . 12 1 1 4 5 6 . 24 6 . 12 2 .63 1 4 6 32 .05 30 .69 3 .04 -15 4 8 5 .08* 5 .04 0 .05 15 4 3 1 1 .63 12. .06 7 .61 10 4 5 4 . 36* 4 .03 0. .08 2 4 6 36 . 35 37 .03 1 .32 -14 4 8 4 .58* O .59 0 .05 16 4 3 4 .51* 6 .29 1 .07 9 4 5 4 .31* 5 .02 0 .09 3 4 6 24 . 68 24 OO 5 .09 -13 4 8 3 .95* 6 . 14 0 .04 17 4 3 7. .84 8 .23 2 .79 8 4 5 8 .09 8 . 77 6 .68 4 4 6 18 .08 16 . 24 8 .71 -12 4 8 3 .98* 5 .31 0 .04 18 4 3 3 .80* 3 .51 0, .03 7 4 5 10 .75 10 .40 12 . 15 5 4 6 34 . 76 34 .91 2 . 56 - 1 1 4 8 2 .50* 7 .41 O .02 19 4 3 5 . 16* 5 .02 0 .84 6 4 5 15 . 16 14 . 19 17 .91 6 4 6 29 . 77 30 . 25 2. 86 -10 4 8 4 .80* 6 . 25 0 .08 19 4 4 6 .54* 10 .97 0 .07 5 4 5 3 .33* 1 .59 0 .09 7 4 6 26 . 98 29 OO 4 , 27 -9 4 8 8 .97 9 .45 4 .86 18 4 4 9 .74 8 .47 3 . 18 4 4 5 10 .94 10 ,65 18 .48 8 4 6 14 .85 15 .63 13 . 13 -8 4 8 14 .74 13 .93 1 1 , .65 17 4 4 12 . 10 13 . 37 5 .82 3 4 5 21 .74 21 .31 5. .90 9 4 6 1 1 .73 1 1 .35 8 99 -7 4 8 14 . 35 15 .43 1 1 .92 16 4 4 21 .34 20. .80 6 .89 2 4 5 16 .78 16 .96 21 .22 10 4 6 6 . 1 1 6 .48 2. ,49 -6 4 8 1 1 .04 1 1 .47 8 .20 15 4 4 17 .08 16 .47 12 .70 1 4 5 18 .58 19 .27 9 .90 1 1 4 6 7 .02 6 .03 2. 86 -5 4 8 12 . 49 1 1 .20 10 .52 14 4 4 18 .79 19 .45 15 .90 0 4 5 0 .54* 1 .50 0. .07 12 4 6 2 . 32* 7 . 24 0. ,02 -4 4 8 18 .06 18 . 1 1 13 .82 13 4 4 25 .95 25 83 3 .79 -1 4 5 20 . 15 20 . 36 6 . 38 13 4 6 4 .87* 4 .45 0. 07 -3 4 8 23 .63 21 ,95 5 . 13 12 4 4 23 . 17 24 .08 6 .49 -2 4 5 21 .70 20 .21 6 . 14 14 4 6 4 . 59* 2 .57 0. .05 -2 4 8 33 .89 33 .78 2 .45 1 1 4 4 30 .76 32 .71 2 .77 -3 4 5 7 .67 7 . 57 1 1 . .50 15 4 6 4 . 75* 1 . 94 0. .04 - 1 4 8 20 . 50 18 .68 7, . 20 10 4 4 1 1 .63 12 .60 14 .61 -4 4 5 7 .48 7 . 10 10. . 34 16 4 6 4 .88* 2 .31 0. .04 0 4 8 9 OO 6 . 24 6 53 -9 4 4 25 .86 26 .49 3 .33 -5 4 5 26 .88 27 .42 3 .56 14 4 7 5 . 70* 1 .92 0. 07 1 4 8 8 .90 8 .87 6 .08 -8 4 4 6 .51 8 .86 6 .78 -6 4 5 9 .40 9 . 39 13, .38 13 4 7 3 .28* 0 .32 0. ,41 2 4 8 13 . 10 1 1 .71 1 1 .56 -7 4 4 28 . 14 29 .75 3 .50 -7 4 5 12 .43 13 .82 18 .75 12 4 7 3 . 12* 5 .01 0. 45 3 4 8 12 .81 13 . 13 10 .81 -6 4 4 23 .29 26 .90 3 .93 -8 4 5 19 .76 20 . 32 7 .71 1 1 4 7 4 . 25* 0 .64 0. 06 4 4 8 3 .86* 1 .28 1 , . 1 1 -5 4 4 22 .20 23 .47 4 .27 -9 4 5 5 .32 6 .98 3 .49 10 4 7 4 . 23* 3 .81 0. 06 5 4 8 7 42 7 .69 3 ,58 -4 4 4 11 .94 12 .90 28 .26 -10 4 5 1 .82* 3 .59 0, .02 9 4 7 0 .91* 6 .04 0. 00 6 4 8 4 .07* 2 .80 0 .06 -3 4 4 2 .82* 1 .42 0 . 13 -11 4 5 12 .54 1 1 .61 1 1 , .93 8 4 7 3 .93* 0 . 40 0. ,06 7 4 8 10 .24 10 . 23 5 .92 -2 4 4 3 .82* 6 .55 0 .20 -12 4 5 4 .89* 1 .32 0, . 12 7 4 7 4 .52* 3 .64 1 . ,60 8 4 8 7 . 1 1 7 .79 2 .84 -1 4 4 12 .54 12 .36 21 .47 -13 4 5 4 .86 5 .56 1 . 60 6 4 7 3 .80* 0 .60 0 .07 9 4 8 4 . 19* 1 .42 0 .06 0 4 4 24 .99 24 .25 4 .44 - 14 4 5 5 .37* 1 .98 0, . 10 5 4 7 12 .45 12 .03 11. 33 10 4 8 3 .20* 1 ,97 0 .52 1 4 4 24 .49 23 .62 4 .38 -15 4 5 4 . 32* O . 35 0. .05 4 4 7 7 . 54 7 . 28 5. 67 1 1 4 8 5 .67* 6 .57 0 .08 2 4 4 21 .24 20 .72 4 .60 -16 4 5 2 . 15* 1 .22 0 22 3 4 7 10 .66 10 .95 1 1 , 06 12 4 8 5 . 20* 3 .60 0 .97 3 4 4 18 .25 17 .82 13 . 13 -17 4 5 6 .24* O . 74 0 .09 2 4 7 4 . 36* 6 . 13 0. . 12 13 4 8 5 . 34* 5 . 29 0 .89 4 4 4 39 . 15 37 .36 1 .26 -18 4 5 4 .81*' 3 .77 0, .04 1 4 7 7 . 47 5 .64 6. 58 1 1 4 9 5 .03* 0 .35 0 .05 5 4 4 35 .09 31 .69 1 .42 -18 4 6 5 .43* 6 . 32 0, .05 0 4 7 17 .06 17 . 26 14 , 30 10 4 9 2 . 30* 1 .87 0 .01 6 4 4 38 .00 35 .49 1 .26 -17 4 6 2 .74* 1 . 30 0. .02 - 1 4 7 2 . 74* 4 .36 0. ,94 9 4 9 4 . 50* 0 .64 0 .05 7 4 4 37 .09 36 .01 1 .26 -16 4 6 6 . 19* 6 .50 0, ,09 -2 4 7 3 .04* 1 , .90 0. 07 8 4 9 2 . 14* 2 .09 0 , 22 8 4 4 44 .55 42 . 32 0 98 -15 4 6 14 .78 14 .53 8. 68 -3 4 7 10 .48 10 .71 1 1 . ,48 7 4 9 4 . 33* 4 .07 0 .05 9 4 4 42 .58 41 .94 1 . .01 -14 4 6 4 .73* 5 .86 0. 07 -4 4 7 14 .05 12, .69 17 . ,55 6 4 9 5 .79 6 . 18 1 , ,67 10 4 4 22 . 15 20 .43 5 .32 - 13 4 6 8 .41 9 . 2 1 3. 98 -5 4 7 9 .09 8 .91 8 .52 5 4 9 4 .25* 1 .03 0, .06 1 1 4 4 26 .48 24 .70 5. .25 -12 4 6 6, .22 6. .03 2 . ,60 -6 4 7 1 1 . .57 10, .28 12. .52 4 4 9 4 . 19* 1 . .63 0. .06 12 4 4 12 .28 1 1 .71 9 29 -11 4 6 10 .76 11 .06 7 . 87 -7 4 7 8 . 7 1 8 .56 7 . 09 3 4 9 7 .90 7 .86 3. 69 13 4 4 20 .09 18. .98 9 .25 -10 4 6 10 .75 10 .64 8 . 68 -8 4 7 4 . 55* 2 .49 0, . 10 2 4 9 4 .11* 1 .63 0. 06 14 4 4 13 .85 14 , .57 8 .53 -9 4 6 8 . 24 7 .53 6 .68 -9 4 7 7 . 42 7 .75 4 05 1 4 9 4 .08* 4 . 1 1 0. 06 15 4 4 14 .31 14 . 36 8 .09 -8 4 6 12 .23 12 .41 14 . , 43 -10 4 7 10 . 54 1 1 .29 7. .21 0 4 9 10 .99 10 .51 7 , .31 16 4 4 10 .27 9. 12 3 . 69 -7 4 6 24 .59 24 .95 4 . 70 - 1 1 4 7 4 . 10* 4 . 16 0, .06 - 1 4 9 6 .83 8 . 17 2 .91 17 4 4 5. 78* 5. 65 0. .07 -6 4 6 14 .85 13 .91 17 . 33 -12 4 7 10 . 4 1 10 .51 5. ,65 -2 4 9 9 .39 9 .06 5 .51 17 4 5 6. 39* 6. .50 0. .07 -5 4 6 16 .57 16 .72 10. 98 - 13 4 7 2 . 52* 4 .59 0, ,02 -3 4 9 4 .11* 1 .62 0 .06 16 4 5 5. 46* 4. 94 0. .06 -4 4 6 12, .96 1 1 .93 15. ,35 - 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14 8 3 7 2 1 5 65 1 75 -7 8 5 6 8 1 6 01 2 65 8 8 0 1 98* 0 88 0 26 -5 8 2 16 22 17 27 13 43 -15 8 3 6 07 5 37 1 12 -8 8 5 1 64* 6 48 0 01 9 8 0 7 98 8 53 3 55 -4 8 2 11 19 10 98 10 02 - 14 8 4 2 10* 3 7 1 O 01 -9 8 5 7 42 7 70 2 75 10 8 0 4 21* 2 54 0 06 -3 8 2 10 20 1 1 42 8 84 - 13 8 4 2 29* 8 48 0 01 - 10 8 5 8 26 7 33 3 22 11 8 0 1 58* 0 10 0 12 -2 8 2 17 66 17 86 14 12 - 12 8 4 1 1 90 12 74 4 99 - 1 1 8 5 4 69* 1 36 0 06 12 8 0 4 58* 1 26 0 06 -1 8 2 8 41 9 52 7 01 -11 8 4 10 22 9 94 4 68 - 12 8 5 5 69* 1 84 0 08 13 8 0 3 75* 1 98 O 03 0 8 2 7 74 8 65 6 1 1 -10 8 4 13 30 14 5 1 7 79 - 13 8 5 3 78* 3 39 0 47 14 8 0 4 72* 1 42 0 04 1 8 2 18 61 20 23 12 04 -9 8 4 7 05 7 70 2 71 - 14 8 5 4 81* O 60 0 04 15 8 0 4 26* 4 82 0 50 2 8 2 3 65* 1 64 0 08 -8 8 4 8 76 9 46 4 47 - 13 8 6 3 59* 4 24 0 39 15 8 1 3 68* 0 53 0 02 3 8 2 6 61 6 66 3 56 -7 8 4 13 52 15 08 10 06 - 12 8 6 4 68* 3 01 0 05 14 8 1 6 44 4 64 1 28 4 8 2 8 17 8 42 5 15 -6 8 4 3 99* 4 89 0 06 - 1 1 8 6 4 56* 3 30 0 05 13 8 1 4 63* 0 53 0 05 5 8 2 1 92* 1 21 0 02 -5 8 4 1 25* 3 06 0 01 - 10 8 6 4 52* 0 83 0 05 12 8 1 3 72* 4 14 0 58 6 8 2 2 98* 3 52 0 61 -4 8 4 9 56 10 75 6 52 -9 8 6 4 33* 4 88 0 86 1 1 8 1 5 22* 5 45 1 30 7 8 2 2 81* 1 24 0 03 -3 8 4 4 60* 1 65 0 10 -8 8 6 1 08* 0 90 0 06 10 8 1 5 51 5 81 1 58 8 8 2 13 02 10 83 8 76 -2 8 4 8 68 7 16 5 76 -7 8 6 4 26* 1 43 0 06 9 8 1 4 15* 2 28 0 06 9 8 2 10 69 10 90 5 51 -1 8 4 12 68 14 48 10 82 -6 8 6 4 65* 2 23 0 07 8 8 1 2 19* 3 00 0 02 10 8 2 5 11* 3 72 1 25 0 8 4 9 92 9 53 6 98 -5 8 6 2 82* 4 96 0 03 7 8 1 6 07 5 75 2 42 11 8 2 14 65 13 88 7 91 1 8 4 6 82 6 74 3 38 -4 8 6 7 99 8 2 1 3 77 6 8 1 8 22 8 52 4 66 12 8 2 5 54* 7 31 0 06 2 8 4 3 14* 5 76 0 04 - 3 8 6 4 13* 3 36 0 06 5 8 1 4 87* 8 41 0 1 1 13 8 2 9 59 9 24 2 77 3 8 4 22 08 20 86 6 74 -2 8 6 10 4 1 1 1 13 6 09 4 8 1 3 73* 1 56 0 07 14 8 2 9 72 9 18 2 58 4 8 4 10 32 9 06 6 56 - 1 8 6 1 1 4 1 12 7 1 7 19 3 8 1 7 56 6 15 5 38 14 8 3 6 81* 3 28 0 08 5 8 4 4 89* 4 5 1 1 47 0 8 6 4 12* 3 07 0 06 2 8 1 8 80 7 68 7 62 13 8 3 5 29* 3 72 0 05 6 8 4 1 1 87 10 19 7 20 1 8 6 13 99 14 55 9 77 1 8 1 13 13 12 37 14 93 12 8 3 3 20* 0 89 0 35 7 8 4 4 36* 9 32 0 05 2 8 6 8 30 8 08 3 77 O 8 1 14 35 14 26 17 01 11 8 3 5 01* 3 75 1 03 8 8 4 4 1 1 * 4 26 0 81 3 8 6 4 84* 5 12 1 31 - 1 8 1 6 81 5 31 4 90 10 8 3 4 93* 3 97 1 10 9 8 4 13 96 13 56 7 49 4 8 6 10 10 10 07 4 87 h k 1 Fo Fc weight 5 8 6 7. 91 8 .35 2. 94 6 8 6 4. .77* 5 .64 0. 06 7 8 6 3 .70* 2 .54 0. 03 8 8 6 4. 73* 7. .50 0. ,04 9 8 6 3. .83* 2 . 95 0 .03 10 8 6 4. .91* 4 .86 0. 04 11 8 6 6 87 4 , 52 1 . 25 9 8 7 5. .30* 0 .92 0. 05 8 8 7 2 .55* 5 .34 0. .01 7 8 7 4 .72* 4 99 0. 04 6 8 7 5 . 15* O . 57 o. 06 5 8 7 4 .52* 0 .31 0. .05 4 8 7 4 .38* 0 .79 0. ,05 3 8 7 2 . 12* 2 .86 0. 22 2 8 7 5 . 89* 6 .00 0. . 10 1 8 7 4 .86* 1 .62 1 .28 0 8 7 2 . 15* 1 .62 0 .01 - 1 8 7 2 .08* 1 . 77 0 23 -2 8 7 3 .88* 4 .28 o 81 -3 8 7 5 .43 5 .03 1. .55 -4 8 7 5 .27 5 .79 1 .41 -5 8 7 2 .73* 3 .90 0, .37 -6 8 7 2 .60* 2 .42 0 .02 -7 8 7 6 . 13 5 .63 1 .70 -8 8 7 8 . 18 8 .65 2 .51 -9 8 7 7 .29 6 .89 1, .90 10 8 7 6 .40 5 .92 1 .40 11 8 7 5 .87* 4 .59 0 .07 -9 8 8 4 . 78* 2 .25 o. 04 -8 8 8 4 .78* 6 .35 0 04 -7 8 8 8 .01 6 .58 2 . 21 -6 8 8 4 .54* 1 .48 0 05 -5 8 8 7 .20 7 .49 1. 89 -4 8 8 7 . 13 6 .88 1. 89 -3 8 8 4 .57* 4 .66 o. .05 -2 8 8 5 .31* 4 .77 1. ,27 -1 8 8 4 . 49* 4 .08 0. 90 0 8 8 1 .03* 3 .82 0. .04 1 8 8 4 .01* 5 .68 0, .04 2 8 8 2 .85* 8 08 0. 02 3 8 8 3 .05* 6 .01 0. 02 4 8 8 4 .63* 3 .94 0. 05 5 8 8 4. .65* 0 .34 0. 05 6 8 8 4 .77* 3 . 18 0. .04 7 8 8 4 .29* 1 . .20 0. 55 3 8 9 5 .80* 0 .30 0. ,07 2 8 9 2 .35* 0 .59 0. . 18 1 8 9 4 .77* 4 .86 0, .04 0 8 9 3 .01* 2 . 13 0. .31 h k 1 Fo Fc we 1ght -1 8 9 4 .42* 1 . 29 0 .04 -2 8 9 3 .29* 1 . 34 0 . 37 -3 8 9 6 . 34* 1 . 44 0 .09 -4 8 9 4 .62* 3 .54 0 .05 -5 8 9 4 .77* 6 .38 0, .71 -6 8 9 4 .83* 0 .71 0 .04 3 9 8 4 .08* 2 .74 0 52 2 9 8 3 .04* 1 .71 0 . 29 1 9 8 6 .41* 2 .97 0, ,09 0 9 8 1 .87* 2 .48 0. . 12 -1 9 8 3 .92* 2 . 3 1 O 03 -2 9 8 4 .70* 1 .27 0. .05 -3 9 8 4 .46* 0 .05 0. .04 -4 9 8 3 . 16* 0 68 0. .02 -5 9 8 4 . 80* 0 .77 0. .04 -8 9 7 1 . 49* 0 . 16 0. .00 -7 9 7 4 .71* 1 .84 0 .05 -6 9 7 3 . 73* 2 .43 0. .03 -5 9 7 4 .57* 3 . 24 0. .05 -4 9 7 4 .44* 2 .84 0. 05 -3 9 7 1 .43* 0 .57 0 .01 -2 9 7 7 .52 7 . 35 2 . 09 -1 9 7 4 .86* 5 . 36 0. .90 0 9 7 4 .52* 0 .95 0 .05 1 9 7 4 .87* O .99 0 .05 2 9 7 3 .06* 4 . 17 0. . 34 3 9 7 6 .57 5 .04 1 .49 4 9 7 5 . 18* 7 .96 0. .06 5 9 7 4 . 75* 1 12 0. .04 6 9 7 5 .80* 0 .40 0 07 8 9 6 1 .83* 1 . 27 o. 10 7 9 6 4 .82* 4 .47 0. 04 6 9 6 6 .07* 1 . . 38 0. .07 5 9 6 4 .30* 1 . .38 0. .04 4 9 6 4 .61* 1 .88 0. ,05 3 9 6 4 .52* 0. .26 0. .05 2 9 6 4 . 39* o .43 0 .05 1 9 6 5 .00* 2 .77 0 .07 O 9 6 6 .96 8 .68 2 . 26 -1 9 6 4 . 35* 1 .68 0 .05 -2 9 6 4 .35* 0 .95 0. .05 -3 9 6 4 .35* 3. .41 0. .05 -4 9 6 4 . 37* 3 .95 0 05 -5 9 6 9 . 13 10 .42 3. .55 -6 9 6 5 .99 6 .93 1. . 39 -7 9 6 8 .02 7 .46 2 . 36 -8 9 6 8 .80 8 . 78 2 . 7 1 -9 9 6 4 .71* 2 .69 0 .05 -IO 9 6 6 .50 7 .69 1 .28 h k 1 Fo Fc weight - 1 1 9 5 4 .74* 4 . 12 0 .04 -10 9 5 6 . 19* 6 .30 0 .08 -9 9 5 5 .37* 7 .59 0 06 -8 9 5 6 .33 5 . 15 1 .55 -7 9 5 5 .41* 2 .31 0 08 -6 9 5 4 . 78* 7 .92 0 .06 -5 9 5 9 . 20 10 .03 4 , . 19 -4 9 5 4 .87* 2 . 14 1 . 30 -3 9 5 1 . 35* 6 .34 0 .01 -2 9 5 3 .55* 3 .26 0, .04 - 1 9 5 4 . 25* 2 .91 0, .06 0 9 5 7 .66 10 . 18 3. .04 1 9 5 4 . 25* 2 .45 0. 06 2 9 5 2 .09* 2 . 12 0. 23 3 9 5 2 .95* 4 .04 o .43 4 9 5 4 .40* 4 .97 0. .05 5 9 5 4 . 47* 3 .33 0. .05 6 9 5 4 . 55* 4 .88 o 86 7 9 5 4 70* 1 . 26 0. .05 8 9 5 3 .40* 0. . 17 0 .02 9 9 5 1 .33* 0 . 33 0 .05 10 9 5 6 .11* 1 .00 o. .07 1 1 9 4 4 .96* 0 . 18 0. .04 10 9 4 4 .79* 0 .31 0. ,04 9 9 4 4 . 73* 2 ,67 0 .04 8 9 4 2 . 49* 1 .99 0 .22 7 9 4 4 .40* 2 . 14 0. .05 6 9 4 4 .41* 1 .76 0. .05 5 9 4 4 . 37* 5 . IO o. .05 4 9 4 10 . 40 1 1 . 13 5 . 14 3 9 4 13 . 22 14 .53 7 . 98 2 9 4 5 .93 6 . 24 1 .94 1 9 4 4 . 23* 4 .31 1 .06 0 9 4 10 . 29 12 . 19 5. .65 - 1 9 4 17 .08 17 . 73 13 , .04 -2 9 4 8 . 7 1 9 .65 4 . 19 -3 9 4 4 . 12* 4 . 46 0. 06 -4 9 4 2 .64* 2 .75 0, .02 -5 9 4 3 58* 4 . 42 0 . 73 -6 9 4 9 . 57 9 .90 4 64 -7 9 4 4 .09* 5 . 1 1 0 .05 -8 9 4 6 . 17 6 . 89 1 .80 -9 9 4 4 . 43* 6 .45 0 .05 - 10 9 4 4 .96* 0 . 77 0 .06 - 1 1 9 4 4 . 74* 2 .49 O .04 - 12 9 4 3 . 16* 4 . 19 0 .02 -13 9 3 2 . 40* 4 .66 O . 17 -12 9 3 3 . 28* 3 . 49 0 .02 - 1 1 9 3 12 . 32 1 1 . 74 4 .99 h k l Fo Fc weight -10 9 3 4 , 57* 7 . 26 0 .05 -9 9 3 1 . 38* 2 , 92 0 .01 -8 9 3 4 .70* 4 . 24 1 . 14 -7 9 3 5 . 19* 8 . 10 0 .08 -6 9 3 8 60 7 . 44 4 .24 -5 9 3 10 .65 9 .43 6 .51 -4 9 3 5 .01* 2 . 45 O. .09 -3 9 3 4 .54* 5. .02 0. .08 -2 9 3 10 . 37 10. .34 6. ,53 -1 9 3 15 . 18 15, . 10 1 1 . .67 0 9 3 4 . 51* 5 , 15 0. ,07 1 9 3 2 ,39* O, .79 0. .02 2 9 3 13 .89 13. , 35 9. 84 3 9 3 8 , 25 7 , . 33 3. ,84 4 9 3 4 . 73* 4 . 56 1 . 24 5 9 3 2 09* 4 , 79 0. ,01 6 9 3 1 , .64* 0, . 76 0. 01 7 9 3 4 . 34* 4 . ,04 0. 05 8 9 3 10, . 27 9 . 25 4 . 26 9 9 3 2 .64* 3. . 38 0. 02 10 9 3 6 44* 2. 86 0. 09 1 1 9 3 6 , . 57* 4 93 0. 09 12 9 3 2 . 12* 4 . , 36 0. 01 12 9 2 5, .01* 0. .97 0. .05 1 1 9 2 4 69* 2 . 54 0. 05 10 9 2 9 64 9. . 17 3 . 12 9 9 2 5 . 97* 7 , .04 0 .09 8 9 2 4 .48* 6 .58 0, .05 7 9 2 12 36 12 .81 6 88 6 9 2 3 .61* 2 . 28 0 .04 5 9 2 8 .07 8 , 18 3 .56 4 9 2 4 . 58* 4 .68 1 . 24 3 9 2 1 1 .41 1 1 . .13 7 . 23 2 9 2 18 . 54 18 . 19 10 .83 1 9 2 7 . 25 6 . 73 3 , . 42 0 9 2 9, .98 8 . 86 6, .36 - 1 9 2 8 . 95 10. .02 5, . 20 -2 9 2 10 96 1 1 . . 16 7 , . 47 -3 9 2 1 55* 6 28 0 01 -4 9 2 5 .41* 0. . 53 0 12 -5 9 2 4 . 47* 0 28 0, 08 -6 9 2 0 . 39* 2 . 47 0 01 -7 9 2 4 . 77* 2 . 7 1 0. ,08 -8 9 2 1 1 .41 1 1 . 34 6 . 44 -9 9 2 4 .31* 2 .88 0. .05 - 10 9 2 5 . 30 5 .60 1 .31 - 1 1 9 2 4 .51* 5 .86 0 .05 -12 9 2 4 . 49* 3 . 46 0 .04 -13 9 2 6 . 66* 5 .51 0 .09 h k 1 Fo Fc weight h k 1 Fo Fc weight h k 1 Fo Fc weight h k 1 Fo Fc weight -13 9 ! 5 11* 3 45 0 87 9 10 0 6 05* 1 72 0 07 8 10 3 6 39* 1 68 0 08 -4 10 5 6 IO* 4 19 0 09 -12 9 1 1 45* 3 81 0 00 10 10 0 2 95* 4 70 0 02 7 10 3 4 57* 4 95 0 04 -5 10 5 5 02* 9 10 0 05 -11 9 1 2 85* 2 90 0 32 1 1 10 0 4 63* 3 05 0 04 6 10 3 4 83* 4 06 0 05 -6 10 5 4 65* 0 83 0 05 -10 9 1 5 15* 6 95 1 23 1 1 10 1 4 87* 0 94 O 04 5 10 3 7 62 6 39 2 28 -7 10 5 2 34* 0 66 0 18 -9 9 1 3 61* 0 95 0 04 10 10 1 7 12 6 36 1 46 4 10 3 5 31* 0 66 0 07 -8 10 5 6 48 6 79 1 30 -8 9 1 4 17* 1 27 0 06 9 10 1 4 84* 4 09 0 04 3 10 3 4 37 + 1 83 O 05 -6 10 6 4 72* 3 14 0 04 -7 9 1 2 02* 2 96 O 24 8 10 1 4 52* 0 47 0 04 2 10 3 4 50* 4 18 0 05 -5 10 6 2 .35* 0 36 0 18 -6 9 1 10 03 9 34 6 03 7 10 1 4 56* 0 46 0 05 1 10 3 5 38 4 01 1 38 -4 10 6 6 34* 2 83 0 09 -5 9 1 4 05* 1 64 0 06 6 10 1 9 69 8 18 3 91 0 10 3 4 28* 1 46 0 05 -3 10 6 4 69* 1 47 0 05 -4 9 1 2 19* 1 07 0 02 5 10 1 3 63* 1 86 0 04 - 1 10 3 5 54* 4 66 O 10 -2 10 6 6 04* 2 05 0 08 -3 9 1 14 88 16 70 12 1 1 4 10 1 5 02* 4 29 1 19 -2 10 3 4 29* 0 32 0 05 - 1 10 6 5 85* 4 00 0 07 -2 9 1 4 83* 1 04 0 1 1 3 10 1 4 38* 1 64 0 05 -3 10 3 4 29* 1 10 0 05 O 10 6 3 73* 6 30 0 03 -1 9 1 3 12* 1 83 0 73 2 10 1 5 65 5 31 1 61 -4 10 3 4 41* 3 04 0 05 1 10 6 2 08* 2 98 0 01 O 9 1 1 59* 2 89 0 18 1 10 1 1 86* 1 08 o 18 -5 10 3 4 32* 2 27 O 05 2 10 6 4 78* 4 97 0 05 1 9 1 9 60 8 36 6 03 0 10 1 2 08* 3 85 0 23 -6 10 3 3 86* 1 62 0 04 3 10 6 4 76* 5 33 0 04 2 9 1 8 02 8 03 4 16 -1 10 1 13 31 1 1 47 8 25 -7 10 3 5 68 3 52 1 27 4 10 6 2 59* 4 80 0 01 3 9 1 11 58 9 67 7 94 -2 10 1 2 61* 2 03 0 37 -8 10 3 2 04* 4 87 0 01 0 10 7 4 80* 3 76 0 04 4 9 1 4 98 7 47 1 54 -3 10 1 4 32* 7 01 0 05 -9 10 3 4 64* 0 76 0 05 -1 10 7 4 79* 1 36 0 04 5 9 1 7 06 5 61 2 83 -4 10 1 4 07* 5 60 0 05 -10 10 3 2 09* 1 77 0 14 -2 10 7 4 82* 3 13 0 04 6 9 1 9 OO 7 72 4 30 -5 IO 1 5 77 5 73 1 61 - 10 10 4 2 39* 5 84 O 01 4 11 4 3 . 20* O 86 0 02 7 9 1 8 OO 6 60 3 25 -6 10 1 4 27* 0 84 0 05 -9 10 4 1 1 38 10 86 3 91 3 11 4 6 53* 0 54 0 08 8 9 1 3 56* 2 72 0 04 -7 10 1 6 05 5 88 1 68 -8 10 4 4 60* 4 98 0 05 2 11 4 2 98* 9 01 0 02 9 9 1 4 45* 3 99 0 05 -8 10 1 6 36* 6 19 0 09 -7 10 4 4 67* 2 83 0 05 1 11 4 10 47 10 81 3 16 10 9 1 4 85* 3 47 0 06 -9 10 1 8 53 8 69 2 49 -6 10 4 8 68 8 22 2 74 0 11 4 4 77* 3 53 0 04 11 9 1 4 72* 6 80 0 04 -10 10 1 4 46* 2 56 0 67 -5 10 4 4 55* 7 39 0 05 - 1 11 4 3 89* 1 60 0 48 12 9 1 6 78* 4 97 0 08 -1 1 10 1 3 18* 2 12 O 02 -4 10 4 4 87* 2 8 1 0 07 -2 11 4 2 10* 1 67 0 01 13 9 1 4 91* 3 19 0 04 -1 1 10 2 8 56 9 25 2 13 -3 10 4 4 39* 0 4 1 0 05 -3 11 4 6 22* 3 60 0 08 13 9 0 5 86* 6 53 0 97 -10 10 2 12 01 12 30 4 34 -2 10 4 3 40* 2 35 0 54 -4 11 4 6 .25* 4 OO 0 08 12 9 0 10 69 10 68 3 39 -9 10 2 4 57* 2 97 0 05 -1 10 4 5 30* 6 56 0 08 -5 11 4 4 81* 1 76 0 04 1 1 9 o 6 36* 9 75 0 08 -8 10 2 5 19* 3 8 1 1 04 0 10 4 3 81* 0 53 0 04 -6 11 3 4 86* 5 83 0 04 10 9 0 5 57* 7 94 0 07 -7 10 2 6 43 6 92 1 78 1 10 4 3 42* 2 18 0 03 -5 11 3 4 77* 3 68 0 04 9 9 o 17 06 16 59 10 34 -6 10 2 5 39* 4 25 0 08 2 10 4 4 60* 4 7 1 0 05 -4 11 3 1 75* 2 25 0 10 8 9 0 9 51 8 49 4 21 -5 10 2 4 13* 5 60 0 05 3 10 4 1 99* 0 47 0 01 -3 11 3 8 67 8 07 2 38 7 9 0 5 10* 3 24 0 08 -4 10 2 4 43* 6 22 0 05 4 10 4 4 55* 1 73 0 05 -2 11 3 4 80* O 99 0 04 6 9 o 11 16 10 64 6 48 -3 10 2 4 24* 3 34 0 06 5 10 4 4 65* 0 96 0 05 - 1 11 3 4 60* 2 00 0 05 5 9 o 7 15 6 52 3 03 -2 10 2 5 25 6 80 1 41 6 10 4 4 78* 0 76 0 04 O 11 3 4 70* 2 83 0 05 4 9 0 9 23 8 62 5 13 -1 10 2 5 38 6 87 1 46 7 10 4 1 71* 4 59 0 09 1 11 3 4 68* 4 40 0 05 3 9 0 1 97* 1 27 0 26 0 10 2 4 27* 5 74 0 05 8 10 4 6 51* 7 51 0 07 2 11 3 4 75* 1 10 0 04 2 9 0 4 03* 2 12 0 07 1 10 2 4 35* 4 16 0 05 7 10 5 4 98* 1 31 0 04 3 11 3 4 81* 2 16 0 04 1 9 0 4 55* 1 10 0 09 2 10 2 5 82* 4 52 o 10 6 10 5 4 07* 6 39 0 03 4 11 3 4 91* 7 40 0 04 0 10 0 4 25* 8 30 0 06 3 10 2- 2 15* 5 78 0 01 5 10 5 4 80* 1 22 0 04 5 11 3 4 86* 2 79 0 04 1 10 o 4 92* 6 15 1 27 4 10 2 4 38* 1 57 0 05 4 10 5 4 64* 1 17 0 05 6 11 2 5 87* 3 68 0 07 2 10 0 9 03 8 48 4 12 5 10 2 2 18* 0 42 0 2 1 3 10 5 4 65* 1 18 o 05 5 11 2 4 77* 4 67 0 04 3 10 o 8 92 9 60 3 86 6 10 2 4 53* 4 01 0 05 2 10 5 5 45 + 5 2 1 1 04 4 11 2 4 77* 4 28 0 04 4 10 0 2 71* 5 12 0 02 7 10 2 7 57 7 55 1 94 1 10 5 6 23* 3 48 0 09 3 11 2 4 69* 1 28 0 05 5 10 0 5 89 5 91 1 59 8 10 2 6 13* 1 53 0 08 0 10 5 8 55 7 65 2 70 2 11 2 4 68* 1 02 0 05 6 10 0 4 45* 2 50 0 05 9 10 2 4 76* 0 96 0 04 - 1 10 5 1 74* 2 91 0 01 1 11 2 6 23 6 55 1 31 7 10 0 5 13* 2 92 1 15 10 10 2 5 49* 6 23 0 05 -2 10 5 3 9 1 + 0 85 0 03 0 11 2 4 66* 5 04 0 05 8 10 0 4 69* 1 41 0 05 9 10 3 7 86 5 43 1 69 -3 10 5 2 02* 0 92 0 01 - 1 11 2 3 67* 5 74 0 03 Fo Fc weight Fo Fc weight Fo Fc weight Fo 2 1 1 2 5 49* 1 58 0 07 3 1 1 2 4 67* 1 00 0 05 4 1 1 2 5 40* 5 99 0 98 5 1 1 2 4 70* 0 98 0 05 6 1 1 2 2 36* 4 23 0 18 7 1 1 2 4 86* 2 02 0 04 8 1 1 1 4 81* 3 86 0 04 7 1 1 1 4 73* 1 12 0 04 6 1 1 1 4 62* 1 34 0 05 5 1 1 1 5 05* 1 29 0 06 4 1 1 1 4 89* 4 36 0 84 3 11 1 4 55* 0 70 0 05 2 1 1 1 4 96* 3 56 0 05 1 11 1 5 65 4 49 1 16 0 1 1 1 4 63* 1 92 0 05 1 1 1 1 4 61* 1 63 0 05 2 1 1 1 3 21* 2 49 0 02 3 1 1 1 10 43 8 44 3 45 4 1 1 1 2 36* 1 13 0 18 5 1 1 1 4 79* 1 80 0 04 6 11 1 2 45* 2 61 0 18 7 1 1 1 4 89* 3 59 0 04 7 1 1 0 2 90* 6 04 o 24 6 1 1 0 4 80* 1 44 0 04 5 1 1 0 4 79* 2 58 0 04 4 1 1 0 2 95* 3 47 0 29 3 11 o 3 52* 6 94 o 03 2 1 1 0 3 59* 1 72 0 46 1 1 1 0 3 54* 2 51 0 45 Fc weight ^ O) 3 ft. e-> . H fa 3361 r e f l e c t i o n s Appendix E Structure Factors for the Photoproduct 107 h k 1 Fo Fc weight 2 0 0 36 51 34 84 1 28 4 0 0 315 06 332 81 0 02 6 0 0 73 05 74 86 0 30 8 0 o 73 03 74 34 0 34 10 O 0 69 77 71 05 0 32 12 0 0 8 49* 5 29 0 01 14 0 0 69 66 70 59 0 35 16 0 0 8 27* 3 85 O 01 18 0 0 28 83 26 81 0 65 20 0 0 14 16* 15 93 0 01 22 0 0 13 26* 3 35 0 01 22 0 2 13 41* 12 62 0 01 20 0 2 1 1 90* 4 34 O 01 18 0 2 43 36 40 05 0 71 16 0 2 25 12 26 05 0 75 14 0 2 92 03 94 29 0 19 12 0 2 51 89 55 33 0 54 10 0 2 76 70 83 39 0 29 -8 0 2 159 61 172 53 0 09 -6 0 2 63 06 64 03 0 45 -4 0 2 35 27 38 30 1 22 -2 0 2 52 24 55 28 0 61 0 0 2 148 50 142 08 0 11 2 0 2 25 34 24 35 2 58 4 0 2 51 11 51 18 0 65 6 0 2 154 85 157 46 0 09 8 0 2 67 37 69 62 0 36 10 0 2 85 87 86 22 0 25 12 0 2 103 27 103 78 0 18 14 0 2 10 97* 11 33 0 28 16 0 2 39 92 37 80 0 82 18 0 2 5 52* 6 67 0 03 20 0 2 15 81* 8 71 0 01 22 0 2 12 67* 4 76 0 01 22 0 4 19 17 14 28 0 19 20 0 4 14 76* 3 34 0 01 18 0 4 18 48 16 30 o 34 16 0 4 24 38 23 12 o 70 14 0 4 45 02 47 57 0 87 12 0 4 1 1 1 70 1 14 14 0 13 10 0 4 76 57 76 60 0 28 -8 0 4 154 41 165 96 0 09 -6 0 4 150 73 156 26 0 10 -4 0 4 164 98 177 18 0 09 -2 0 4 50 76 54 71 0 68 0 0 4 137 12 128 04 0 12 2 0 4 364 07 354 02 0 02 4 0 4 173 82 164 90 0 08 6 0 4 121 56 1 14 71 0 14 h k l Fo Fc weight 8 O 4 71 98 78 16 0 32 10 0 4 26 34 28 32 1 46 12 0 4 141 32 143 32 0 09 14 O 4 31 23 29 70 1 02 16 0 4 73 89 73 48 0 29 18 0 4 63 43 59 85 0 39 20 0 4 1 1 83* 8 28 0 01 22 0 4 12 83* 17 83 0 01 22 0 6 13 15* 4 14 0 01 20 0 6 12 83* 16 16 0 01 18 0 6 1 1 20* 6 81 0 01 16 0 6 29 18 25 74 0 74 14 0 6 61 65 61 72 O 4 1 12 0 6 106 30 105 4 1 0 17 10 0 6 85 22 86 68 0 24 -8 0 6 102 70 103 76 0 17 -6 0 6 169 OO 179 59 0 08 -4 0 6 81 83 80 43 0 26 -2 0 6 69 20 68 34 0 40 0 0 6 134 63 131 12 0 12 2 0 6 189 69 174 55 0 07 4 o 6 226 01 2 19 47 0 05 6 0 6 6 97* 6 06 0 02 8 0 6 106 72 104 39 0 15 10 0 6 41 88 42 03 0 94 12 0 6 12 07* 16 51 0 02 14 0 6 38 25 36 25 0 91 16 0 6 14 38 12 84 0 26 18 0 6 7 59* 19 47 0 00 20 0 6 14 08* 16 12 0 01 22 0 8 13 95* 7 33 0 01 20 0 8 28 04 27 23 0 43 18 0 8 31 04 29 27 0 62 16 0 8 52 35 50 01 0 53 14 0 8 41 39 40 21 0 76 12 0 8 14 27 12 88 0 50 10 o 8 65 59 65 81 0 36 -8 o 8 73 53 77 69 0 29 -6 0 8 83 08 86 61 o 27 -4 0 8 161 09 163 07 0 08 -2 0 8 72 36 67 17 0 35 O 0 8 67 56 67 92 0 38 2 0 8 156 70 142 38 ' 0 09 4 0 8 69 60 68 75 0 35 6 0 8 223 16 210 90 o 05 8 0 8 45 82 44 2 1 0 80 10 0 8 83 08 83 79 o 23 12 0 8 21 54 22 13 0 81 14 0 8 97 06 96 07 0 17 h k l Fo Fc weight 16 0 8 24 70 24 61 0 53 18 0 8 29 14 3 1 67 O 52 20 0 8 26 75 28 7 1 0 33 20 0 10 12 79* 2 50 0 01 18 0 10 20 38 12 52 0 34 16 0 10 14 95* 9 09 0 01 14 0 10 10 30* 14 00 0 01 12 0 10 48 89 47 24 0 67 10 0 10 8 88* 5 7 1 o 01 -8 0 10 91 95 89 72 o 21 -6 0 10 24 49 26 24 1 45 -4 0 10 158 85 160 92 o 08 -2 O 10 121 97 1 14 12 o 13 0 0 10 8 1 37 78 26 0 28 2 0 10 97 44 93 89 0 18 4 0 10 45 52 40 40 0 77 6 o 10 129 14 124 64 o 1 1 8 0 10 54 56 55 19 0 53 10 0 10 54 47 53 52 0 55 12 0 10 58 99 58 55 0 48 14 0 10 10 79* 11 76 0 14 16 o 10 30 36 30 01 o 59 18 0 10 7 99* 10 06 0 00 20 0 10 14 73* 16 47 0 01 20 0 12 9 44* 12 99 0 00 18 0 12 12 70* 7 63 0 01 16 0 12 36 09 35 32 0 67 14 0 12 5 24* 4 56 0 04 12 0 12 56 48 57 49 0 49 10 0 12 26 92 27 74 0 97 -8 0 12 46 50 47 07 0 83 -6 0 12 75 64 75 53 0 26 -4 0 12 82 89 81 84 0 25 -2 0 12 1 19 53 1 16 98 0 13 0 0 12 69 89 66 57 0 31 2 0 12 137 28 133 63 0 10 4 0 12 107 82 102 72 0 14 6 0 12 51 13 49 94 o 56 8 0 12 134 52 131 55 0 10 10 0 12 9 14* 5 20 o 01 12 0 12 44 58 41 69 0 62 14 o 12 35 75 34 63 o 72 16 0 12 2 1 39 19 29 0 35 18 0 12 13 68* 1 1 84 0 01 18 0 14 12 78* 2 82 o 01 16 0 14 28 17 23 75 0 50 14 0 14 18 88 20 56 0 35 12 0 14 10 86* 9 05 0 01 10 0 14 48 79 47 30 o 75 h k 1 Fo Fc weight 0^-ppe -8 0 14 57 10 59 13 O 50 ppe -6 0 14 56 39 56 95 0 51 ndix -4 0 14 46 68 47 55 0 69 ndix -2 0 14 43 33 44 82 0 86 ndix 0 0 14 1 10 66 108 09 0 13 2 0 14 34 96 33 75 1 1 1 4 0 14 72 21 69 77 0 30 6 0 14 19 98 19 46 0 69 8 0 14 69 55 69 31 0 31 10 0 14 37 23 37 15 0 80 12 0 14 14 80 17 82 0 22 14 0 14 39 16 38 34 0 64 16 0 14 12 61* 13 95 0 01 18 0 14 20 37 18 68 0 20 18 0 16 16 30* 13 90 0 14 16 0 16 10 67* 5 18 0 01 14 0 16 31 04 26 48 O 60 12 0 16 5 53* 6 06 0 03 10 0 16 63 06 60 75 0 43 -8 0 16 43 50 42 52 0 82 -6 0 16 10 23* 1 1 31 0 01 -4 0 16 84 76 82 39 0 24 -2 0 16 8 58* 10 79 0 15 0 0 16 68 99 66 06 O 33 2 0 16 56 82 55 96 0 46 4 0 16 38 55 38 19 0 89 6 0 16 40 28 40 97 0 84 8 0 16 10 75* 14 31 0 01 10 0 16 47 03 47 81 0 66 12 0 16 15 50 13 23 0 21 14 0 16 28 07 26 85 0 44 16 0 16 36 41 36 1 1 0 46 16 0 18 12 59* 5 94 0 01 14 0 18 12 10* 2 10 0 01 12 0 18 17 54 15 76 0 25 10 0 18 15 21* 8 16 0 01 -8 0 18 38 36 36 20 0 73 -6 0 18 12 49* 3 28 0 01 -4 0 18 69 39 68 63 o 33 -2 0 18 10 74* 10 22 0 OI 0 0 18 24 50 24 12 0 68 2 o 18 59 39 59 31 0 46 4 0 18 31 57 31 1 1 0 72 6 0 18 29 05 26 76 0 64 8 0 18 27 63 28 32 0 55 10 0 18 5 83* 3 91 0 03 12 0 18 22 38 25 12 0 31 14 0 18 10 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1—1 - 7 1 1 4 6 4 2 * 6 4 0 0 1 0 c5 h k 1 Fo Fc weight h k 1 Fo Fc weight h k 1 Fo Fc we 1ght h k 1 Fo Fc weight -9 1 14 16 72 13 77 0 51 -14 1 1 1 22 26 20 48 0 57 2 1 9 124 45 1 15 7 1 0 13 12 1 7 37 94 36 26 1 02 1 1 1 14 10 76* 8 20 0 01 -12 1 1 1 61 90 59 22 0 35 4 1 9 66 82 63 57 0 34 14 1 7 69 73 68 10 0 36 13 1 14 10 99* 4 65 0 01 -10 1 1 1 9 07* 3 75 0 01 6 1 9 129 03 125 34 0 11 16 1 7 10 97* 3 68 0 01 15 1 14 1 1 37* 5 44 0 01 -8 1 1 1 45 18 46 14 0 79 8 1 9 10 83* 8 83 0 03 18 1 7 17 04 14 80 0 26 17 1 14 12 53* 9 62 0 01 -6 1 1 1 67 61 67 74 0 35 10 1 9 45 43 46 02 0 67 20 1 7 15 96* 12 64 0 01 19 1 14 4 49* 5 15 0 01 -4 1 11 27 99 29 29 1 49 12 1 9 45 31 45 32 0 78 21 1 6 13 04* 1 51 0 01 20 1 13 19 41 13 68 0 19 -2 1 1 1 89 13 87 07 0 24 14 1 9 5 17* 4 00 0 04 19 1 6 5 90* 4 23 0 03 18 1 13 6 26* 9 98 0 03 0 1 1 1 39 96 37 84 0 98 16 1 9 33 47 32 95 0 67 17 1 6 1 1 33* 7 99 0 01 16 1 13 3 83* 12 82 0 00 2 1 1 1 138 21 131 31 0 10 18 1 9 1 1 76* 7 32 0 01 15 1 6 10 42* 5 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weight h k 1 Fo Fc weight h k 1 Fo Fc we 1ght h k 1 Fo Fc weight 22 1 5 13 44* 1 1 38 0 01 15 1 2 34 73 33 30 0 98 7 1 0 131 69 130 86 0 12 0 2 2 176 72 171 45 0 08 21 1 4 12 52* 10 53 0 01 13 1 2 39 99 42 52 0 88 5 1 0 42 52 42 63 0 83 2 2 2 38 52 35 42 1 18 19 1 4 25 86 26 26 0 46 1 1 1 2 3 89* 7 91 0 00 3 1 0 197 64 197 92 0 06 4 2 2 64 31 62 6 1 0 43 17 1 4 15 53 14 59 0 28 9 1 2 84 65 88 70 0 26 1 1 0 12 84 12 40 5 35 6 2 2 43 96 45 74 0 76 15 1 4 32 51 33 72 0 88 7 1 2 88 37 89 85 0 22 0 2 0 96 93 95 52 0 22 8 2 2 15 22 17 06 1 29 13 1 4 13 12 13 89 0 40 5 1 2 51 80 55 55 0 57 2 2 0 9 00 8 75 1 48 10 2 2 13 7 1 10 91 0 75 1 1 1 4 46 80 48 1 1 0 73 3 1 2 28 58 27 79 1 7 1 4 2 0 136 01 131 20 0 12 12 2 2 53 52 53 20 O 58 9 1 4 71 82 71 19 0 31 1 1 2 97 09 89 14 0 23 6 2 0 1 15 79 113 10 0 15 14 2 2 28 44 28 4 1 0 96 7 1 4 79 62 77 21 0 30 -1 1 2 17 24 17 44 4 40 8 2 0 40 16 40 45 0 92 16 2 2 9 01* 9 91 0 1 1 5 1 4 18 16 18 02 2 36 -3 1 2 1 12 67 113 83 O 17 10 2 0 59 60 60 16 O 46 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97 60 90 0 41 20 1 1 38 48 36 50 0 58 -18 2 2 28 77 28 50 0 62 - 10 2 4 20 76 21 46 1 23 14 1 3 9 38* 4 86 0 01 22 1 1 1 1 83* 1 1 70 o 08 - 16 2 2 8 46* 5 88 0 01 -8 2 4 19 17 20 12 1 56 16 1 3 39 36 37 81 0 81 21 1 0 15 92 12 51 0 16 -14 2 2 1 1 05* 10 56 0 02 -6 2 4 31 19 34 33 1 53 18 1 3 14 39* 7 83 0 01 19 1 0 18 98 19 02 0 31 - 12 2 2 58 74 59 95 0 46 -4 2 4 39 78 42 87 1 02 20 1 3 22 OO 19 13 0 34 17 1 0 48 74 46 76 0 68 - 10 2 2 24 19 25 61 1 43 -2 2 4 102 21 102 59 0 19 22 1 3 13 52* 4 36 0 01 15 1 o 12 62* 14 4 1 0 02 -8 2 2 92 37 95 56 0 19 0 2 4 15 08 13 92 2 4 1 21 1 2 12 55* 1 94 o 01 13 1 o 21 79 22 48 0 96 -6 2 2 32 29 31 40 1 67 2 2 4 58 27 56 69 0 49 19 1 2 1 1 48* 1 73 0 01 1 1 1 0 28 91 28 39 1 38 -4 2 2 212 91 219 03 0 05 4 2 4 45 46 46 84 0 76 17 1 2 10 85* 15 13 0 01 9 1 0 7 31* 3 82 0 02 -2 2. 2 150 73 145 28 0 10 6 2 4 84 72 83 26 0 22 h k 1 Fo Fc weight 8 2 4 108 72 109 76 0 15 10 2 4 9 19* 10 88 0 02 12 2 4 50 27 51 08 0 62 14 2 4 23 90 24 18 0 81 16 2 4 24 36 23 61 0 60 18 2 4 12 06* 7 72 0 01 20 2 4 9 08* 3 34 0 00 21 2 5 1 1 18* 19 75 0 00 19 2 5 13 71* 21 19 0 01 17 2 5 24 60 18 68 0 55 15 2 5 43 84 42 45 O 78 13 2 5 13 51* 17 16 0 02 1 1 2 5 52 43 54 11 0 58 9 2 5 18 15 18 95 1 13 7 2 5 77 57 81 OO 0 29 5 2 5 74 60 79 94 0 33 3 2 5 3 62* 3 85 0 01 1 2 5 1 12 23 105 81 0 16 -1 2 5 114 91 115 82 0 16 -3 2 5 183 19 182 69 0 07 -5 2 5 91 30 92 56 0 21 -7 2 5 164 66 164 99 0 08 -9 2 5 70 92 75 74 0 30 1 1 2 5 8 91* 7 54 0 01 13 2 5 37 05 37 01 1 03 15 2 5 33 43 32 98 0 85 17 2 5 18 48 20 43 0 37 19 2 5 23 59 21 02 0 41 21 2 5 8 32* 11 71 0 04 22 2 6 13 81* O 91 o Ol 20 2 6 21 86 18 03 0 33 18 2 6 1 1 32* 1 1 94 0 01 16 2 6 27 67 26 96 0 66 14 2 6 20 72 23 11 0 67 12 2 6 43 10 44 22 0 79 10 2 6 51 46 53 76 0 54 -8 2 6 56 46 57 49 0 45 -6 2 6 1 13 96 1 17 59 0 15 -4 2 6 62 46 59 48 0 41 -2 2 6 70 82 70 47 0 36 0 2 6 228 26 229 23 0 05 2 2 6 74 23 69 13 0 34 4 2 6 44 04 46 28 0 80 6 2 6 7 15* 4 33 0 02 8 2 6 52 71 54 55 0 57 10 2 6 39 37 40 25 1 08 12 2 6 4 27* 5 1 1 o 05 14 2 6 57 81 57 66 0 52 16 2 6 12 99* 12 50 0 01 h k 1 Fo Fc weight 18 2 6 16 60 13 82 0 25 20 2 6 12 90* 1 13 0 01 21 2 7 13 26* 1 1 91 0 01 19 2 7 1 1 41* 7 60 0 01 17 2 7 32 47 35 46 0 62 15 2 7 48 71 50 54 0 59 13 2 7 42 56 42 1 1 0 79 1 1 2 7 88 65 88 04 0 21 9 2 7 21 00 21 34 1 08 7 2 7 125 93 129 87 0 12 5 2 7 28 06 28 26 1 77 3 2 7 108 62 106 64 0 16 1 2 7 37 39 40 91 0 99 -1 2 7 5 53* 8 56 0 30 -3 2 7 85 99 90 76 0 27 -5 2 7 66 07 68 60 0 36 -7 2 7 62 05 64 90 O 42 -9 2 7 84 90 86 12 0 24 1 1 2 7 27 60 30 03 1 13 13 2 7 48 59 48 77 0 72 15 2 7 10 64* 1 1 25 0 01 17 2 7 40 06 37 71 0 7 1 19 2 7 1 1 98* 12 57 0 1 1 21 2 7 16 29* 1 1 91 0 01 20 2 8 14 23* 13 23 0 01 18 2 8 1 1 79* 4 11 0 01 16 2 8 25 23 24 93 0 58 14 2 8 40 12 38 34 0 84 12 2 8 12 02 10 32 0 35 IO 2 8 42 36 42 74 o 89 -8 2 8 34 70 35 89 1 28 -6 2 8 20 51 18 42 1 69 -4 2 8 14 64 1 1 51 1 31 -2 2 8 7 39* 8 29 0 46 O 2 8 1 18 36 124 24 o 14 2 2 8 12 91 13 48 1 05 4 2 8 29 12 28 81 1 66 6 2 8 30 27 31 37 1 46 8 2 8 7 48* 3 40 0 21 10 2 8 43 37 43 62 0 86 12 2 8 32 21 32 37 1 00 14 2 8 17 14 16 59 o 36 16 2 8 31 50 31 95 o 66 18 2 8 12 03* 10 79 0 01 20 2 8 17 36* 1 1 52 0 01 19 2 9 12 38* 16 95 0 01 17 2 9 23 19 23 24 0 4 1 15 2 9 10 94* 1 36 0 01 13 2 9 34 44 33 27 0 83 h k 1 Fo Fc weight 11 2 9 5 08* 2 45 0 06 9 2 9 65 98 68 91 0 37 7 2 9 70 19 72 05 0 33 5 2 9 46 73 45 83 0 79 3 2 9 128 25 1 19 95 0 12 1 2 9 7 46* 2 73 0 02 - 1 2 9 17 1 97 180 99 0 07 -3 2 9 20 73 25 65 1 64 -5 2 9 12 1 44 122 08 0 13 -7 2 9 79 7 1 83 23 0 26 -9 2 9 8 74* 3 76 O 01 11 2 9 62 51 62 86 0 45 13 2 9 17 91 16 81 0 54 15 2 9 24 16 23 98 0 58 17 2 9 12 50* 2 61 0 01 19 2 9 8 03* 3 10 0 00 21 2 9 9 55* 4 47 0 00 20 2 10 10 62* 3 88 0 07 18 2 10 9 92* 8 87 0 08 16 2 10 9 78* O 77 0 01 14 2 10 9 81* 3 02 0 01 12 2 10 9 84* 12 21 0 01 10 2 10 18 85 19 53 0 73 -8 2 10 58 57 61 42 0 43 -6 2 10 42 07 42 30 0 80 -4 2 10 80 56 80 91 O 27 -2 2 10 24 07 23 59 1 65 0 2 10 2 1 39 19 37 1 54 2 2 10 153 33 145 29 0 09 4 2 10 8 60* 6 46 0 01 6 2 10 88 84 88 21 0 22 8 2 10 9 14* 5 54 0 01 10 2 10 52 1 1 54 70 0 53 12 2 10 35 24 37 28 0 89 14 2 10 16 95 17 55 0 34 16 2 10 31 92 34 40 0 59 18 2 10 14 64* 3 37 0 01 20 2 10 14 93* 4 52 0 01 19 2 1 1 18 00* 19 15 0 01 17 2 1 1 13 26* 9 96 0 01 15 2 1 1 1 1 90* 19 09 0 01 13 2 1 1 20 30 2 1 38 0 43 1 1 2 1 1 13 73* 14 27 0 02 9 2 1 1 74 51 72 43 0 31 7 2 1 1 9 38* 4 96 0 01 5 2 1 1 101 64 98 53 0 18 3 2 1 1 50 58 48 86 0 64 1 2 1 1 1 14 72 1 1 1 56 0 13 - 1 2 1 1 1 13 51 1 14 98 o 14 h k 1 Fo Fc weight t3 -3 2 1 1 35 7 1 35 96 1 26 CS -5 2 1 1 60 89 61 68 0 44 3 -7 2 1 1 20 60 22 38 0 99 n. -9 2 1 1 8 60* 13 72 0 01 H 1 1 2 1 1 23 92 24 26 0 81 13 2 1 1 12 34* 8 40 0 01 15 2 1 1 44 19 39 97 0 69 17 2 1 1 1 1 86* 0 41 0 01 19 2 1 1 27 44 23 14 0 37 20 2 12 12 92* 2 44 0 01 18 2 12 17 46 16 66 O 20 16 2 12 12 03* 2 25 0 01 14 2 12 10 96* 5 90 0 01 12 2 12 36 31 34 84 0 82 10 2 12 4 54* 8 45 O OO -8 2 12 39 55 40 76 0 99 -6 2 12 27 56 28 14 1 17 -4 2 12 24 97 27 58 1 25 -2 2 12 13 36 15 30 0 59 O 2 12 8 49* 12 63 0 01 2 2 12 97 77 92 10 0 20 4 2 12 60 77 60 45 0 41 6 2 12 22 50 20 65 0 93 8 2 12 30 69 31 24 0 99 10 2 12 10 23* 9 86 0 01 12 2 12 1 1 1 1* 10 32 0 01 14 2 12 1 1 62* 2 97 0 01 16 2 12 12 08* 2 76 0 01 18 2 12 12 88* 12 09 0 01 17 2 13 13 72* 9 27 0 Ol 15 2 13 23 44 22 64 0 41 13 2 13 1 1 09* 15 59 0 12 1 1 2 13 65 47 67 74 0 36 9 2 13 38 53 34 99 0 89 7 2 13 62 25 61 50 0 4 1 5 2 13 83 53 77 52 0 22 3 2 13 4 15* 6 43 0 OO 1 2 13 76 98 73 40 0 29 - 1 2 13 9 48* 1 1 75 0 02 -3 2 13 43 41 44 24 0 81 -5 2 13 27 97 29 21 1 16 -7 2 13 35 30 39 22 1 01 -9 2 13 31 59 30 77 0 97 1 1 2 13 28 59 30 89 0 77 13 2 13 28 65 25 56 0 66 15 2 13 1 1 42* 9 . 1 1 0 01 17 2 13 9 77* 9 . 20 0 07 19 2 13 13 15* 6 20 0 01 i—» 18 2 14 2 75* 7 39 0 00 to h k 1 Fo Fc weight 16 2 14 12. .00* 9. 67 0. 01 14 2 14 1 1 . 62* 7. 14 0. 01 12 2 14 11 . OO* 8 76 0. 01 10 2 14 20 ,08 19, 89 0. 49 -8 2 14 10 .03* 1 . 45 0. 01 -6 2 14 47. ,48 48. .50 O. 69 -4 2 14 48 26 50. , 1 1 0. 62 -2 2 14 13. .33* 19, ,05 0. .02 0 2 14 19 . 17 20 80 0, .73 2 2 14 9 .39* 14 .23 0 01 4 2 14 53 .97 51 .05 0 53 6 2 14 28 .92 28 . 18 0, ,91 8 2 14 60 .49 58 .49 0, 49 10 2 14 4 .94* 4 .66 0. 00 12 2 14 11 .75* 2 .28 o .01 14 2 14 26 .39 24 06 0 48 16 2 14 11 .59* 10 37 0 09 17 2 15 22 . 19 18 .05 0. 24 15 2 15 12 .48* 7 .01 0, .01 13 2 15 25 .07 23 .60 0 .44 1 1 2 15 39 .83 40 .29 0. .68 9 2 15 12 .65* 6 .04 0 .01 7 2 15 24 .33 22 .64 0 .64 5 2 15 18 .49 18 .70 0 .51 3 2 15 37 . 15 34 .50 0 .91 1 2 15 61 .21 59 .89 0. .41 -1 2 15 27 .30 27 .64 o. 96 -3 2 15 82 .65 83 .42 0, .22 -5 2 15 9 .88* 1 .61 0 .01 -7 2 15 70 .41 70 .20 0 .31 -9 2 15 28 .60 28 .03 o. . 77 1 1 2 15 43 .68 44 .52 0 72 13 2 15 40 .97 41 .44 0 66 15 2 15 3 .92* 4 .01 0 .00 17 2 15 8 .25* 8 . 52 0. .OO 18 2 16 12 . 17* 8 .64 0. .00 16 2 16 7 .45* 6 .99 0. .03 14 2 16 11 .03* 1 .81 0. .01 12 2 16 14 .88* 22 . 10 o .01 10 2 16 1 1 .82* 12 .42 0 .01 -8 2 16 28 .64 29 .78 0 .71 -6 2 16 36 .31 37 .27 0 .89 -4 2 16 42 . 1 1 44 .04 0 80 -2 2 16 26 .79 28 .27 o .87 0 2 16 44 .41 43 . 12 0. .82 2 2 16 3 .24* 2, . 72 0. OO 4 2 16 41 .73 41 , .74 0. 83 6 2 16 30 , 16 28 26 0. 74 8 2 16 12 . 74* 5 .62 0. 01 h k l Fo Fc weight 10 2 16 11 .50* 6 99 0 ,01 12 2 16 13 .92* 9 .60 0 .01 14 2 16 12 . 82* 6 .76 0 .01 16 2 16 13 . 30* 3 .79 0 01 15 2 17 3 .00* 1 .25 0 oo 13 2 17 23, ,48 25 .24 0. . 33 1 1 2 17 7 , . 74* 13 .98 0. .00 9 2 17 34. .72 34 .83 0. .65 7 2 17 17, 29 16 .84 0. .31 5 2 17 46 .40 47 . 20 0 . 7 1 3 2 17 39 . 44 36 . 4 1 0 .80 1 2 17 41 .28 41 .35 0 .82 - 1 2 17 46 .53 46 .33 0 .67 -3 2 17 4 .93* 8 .81 0 .04 -5 2 17 38 . 19 37 .94 o 8 1 -7 2 17 19, .22 18 .67 0 42 -9 2 17 12 .45* 4 .35 0 .01 11 2 17 16, ,09 14 . 30 0. . 24 13 2 17 11 , 96* 1 . 4 1 0. .01 15 2 17 12 .81* 7 .65 0. .01 17 2 17 13, .73* 3 .31 0 .01 16 2 18 12, .99* 0 .70 0 .01 14 2 18 8 . 14* 13 . 23 0 .00 12 2 18 1 1 .71* 9 .05 0 .01 10 2 18 13 . 55* 12 .97 0 .01 -8 2 18 1 1 .06* 12 .97 0 .01 -6 2 18 14 .60* 7 .62 0 .02 -4 2 18 28 .85 28 , 13 0 .71 -2 2 18 23 . 16 23 . 35 0. . 55 0 2 18 10 .43* 2 . 17 0 01 2 2 18 12 .02* 6 .36 0 .01 4 2 18 12 , .59* 8 . 77 0, . 18 6 2 18 14 .95* 9 .03 o. OI 8 2 18 40 , 44 41 .81 0, ,65 10 2 18 1 1 .67* 25 . 83 0 01 12 2 18 12 .82* 18 .02 0 .01 14 2 18 6 .61* 8 .21 0 .02 13 2 19 1 1 .22* 1 1 .45 0 .06 1 1 2 19 23 . 14 21 .87 0 .29 9 2 19 1 1 .09* 10 .72 0, .01 7 2 19 1 1 , .68* 7 . 77 0 .01 5 2 19 35 .84 35 . 27 0 .66 3 2 19 28 .06 28 . 32 0 .57 1 2 19 1 1 .83* 20 . 12 0 .01 -1 2 19 48, .05 47 . 79 0 .67 -3 2 19 9 , 44* 7 .00 o .01 -5 2 19 29 61 29 . 1 1 0 64 -7 2 19 10, .86* 1 1 .51 0, . 12 -9 2 19 26, 87 24 .85 0 52 h k l Fo Fc weight 11 2 19 7 . 86* 13 17 O oo 13 2 19 12 . 24* 15 34 0. 01 15 2 19 13 .58* 13 . 62 0. 01 14 2 20 12 94* 1 . 88 0 01 12 2 20 12 . 57* 6 . 65 0 ,01 10 2 20 14 . 29* 8 . 25 0 ,01 -8 2 20 1 1 . 72* 1 . . 37 0 .01 -6 2 20 16 .80 15 .68 0 .25 -4 2 20 1 1 .61* 17 . 73 0 .01 -2 2 20 0 .89* 10 . 7 1 0 .00 0 2 20 1 1 .02* 1 1 .26 0 .01 2 2 20 1 1 .58* 7 . 12 0 .01 4 2 20 22 .45 24 60 0 .38 6 2 20 12 .29* 1 . .90 0 OI 8 2 20 26 . 36 26 09 0 . 40 10 2 20 12 .51* 3 . IO 0. OI 12 2 20 14 .11* 13 . 43 0. .01 1 1 2 21 14 . 19* 20. .48 0. OI 9 2 21 6 . 47* 4 . 47 0. 02 7 2 21 23 . 30 22 .58 0 , 32 5 2 21 14 . 13* 12 . 80 0 .01 3 2 21 15 .86* 17 . 76 0, .01 1 2 21 28 . 46 23 . 38 0 .51 - 1 2 21 1 1 . 36* 15 .69 0 .01 -3 2 2 1 28 .84 29 .45 0 .52 -5 2 21 12 . 14* 1 .60 0 .01 -7 2 2 1 7 .17* 9 .86 0 .04 -9 2 21 12 . 38* 10 .87 0 .01 1 1 2 21 6 . 45* 6 .83 0 .02 13 2 2 1 13 . 19* 1 .55 0 .01 12 2 22 18 25* 7 .69 0 01 10 2 22 13 . 29* 1 1 . 15 0, .01 -8 2 22 12 66* 5 . 30 0. .01 -6 2 22 3 .99* 6. .07 0, .00 -4 2 22 1 1 . 14* 13 .55 0 .01 -2 2 22 14 . 94 13 .59 0 . 16 0 2 22 18 .67 18 .65 0 . 24 2 2 22 12 .80* 7 .57 0 .01 4 2 22 12 .78* 1 1 .81 0 .01 6 2 22 12 .62* 6 .69 o .09 8 2 22 4 . 19* 1 .64 o .00 10 2 22 13 . 32* 14 .64 0 .01 7 2 23 32 . 46 27 .93 0 . 39 5 2 23 5 . 19* 4 . 39 0 .01 3 2 23 27 89 27 .69 o . 34 1 2 23 19 . 74 17 69 0 24 - 1 2 23 12 .51* 12 . 24 0 .01 -3 2 23 8 .08* 15 91 0 OO -5 2 23 12 . 68* 1 .89 0 01 h k 1 Fo Fc weight l u ts -7 2 23 13 .63* 16 . 12 0. OI t i -9 2 23 6 .59* 3 . 74 0 .02 -8 2 24 17 . 72* 4 .07 0 .01 ta. -6 2 24 12 .00* 14 . 24 0 .07 H -4 2 24 13 .85* 15 .93 0 .01 -2 2 24 6 .62* 4 . 26 0 .02 O 2 24 13 .56* 12 . 70 0. .01 2 2 24 13 . 87* 18 . 26 0. .01 4 2 24 13 .30* 1 .99 0. .01 6 2 24 13 .64* 16 . 77 0. .01 1 2 25 13 . 40* 10 . 6 1 O. 01 - 1 2 25 17 .09* 4 . 10 0. 01 -3 2 25 13 .83* 7 .90 O. 01 -5 2 25 14 .95* 3 . 56 0. .01 3 3 24 13 .65* 19 . 27 0. 01 1 3 24 13 .65* 6 .68 0. 01 - 1 3 24 16 .90* 23 .54 0. 01 -3 3 24 14 .05* 7 . 12 0. 01 -5 3 24 7 . 40* 7 . 4 1 0 oo -8 3 23 1 1 . 26* 2 .44 0. oo -6 3 23 1 1 .83* 0 .42 0, 00 -4 3 23 9 . 64* 9 .45 0. ,05 -2 3 23 17 .91* 4 . 94 0 .01 0 3 23 10 .07* 2 .88 0, oo 2 3 23 13 . 19* 1 1 . 25 0. .01 4 3 23 4 . 19* 5 .20 0. .00 6 3 23 13 .11* 4 .64 0 01 9 3 22 13 .96* 3 . 53 0 .01 7 3 22 13 . 14* 18 .95 0 .01 5 3 22 18 . 37 16 .88 0 . 18 3 3 22 12 .85* 7 . 23 0 .01 1 3 22 22 . 77 19 .63 0 .31 - 1 3 22 12 . 16* 1 .67 0 .01 -3 3 22 23 . 15 25 .83 0 .31 -5 3 22 16 .66* 7 . 16 0 .01 -7 3 22 17 .66 17 . 55 0. . 17 -9 3 22 15 . 70* 8 .96 0. 01 1 1 3 22 7 .46* 5 .04 0. oo 12 3 21 13 . 30* 2 . 47 o. .01 10 3 21 1 1 .72* 3 . 49 0. 01 -8 3 21 12 .55* 5 . 20 0 01 -6 3 21 12 .61* 3 . 45 0. 01 -4 3 2 1 1 1 . 77* O . 46 0 01 -2 3 2 1 13 . 42* 2 . 70 0. .01 0 3 21 12 .32* 7 .07 0 .01 2 3 21 3 . 28* 1 . 74 0 .01 4 3 21 12 . 12* 8 . 39 0 01 6 3 21 1 1 . 44* 13 .97 0 .01 8 3 21 6 .61* 5 . 84 0 .02 C O h k 1 Fo Fc weight 10 3 21 14 82* 9 37 0 01 11 3 20 13 18* 14 09 0 09 9 3 20 13 OO* 1 1 16 0 01 7 3 20 14 36* 19 73 O 01 5 3 20 42 22 40 08 0 61 3 3 20 1 1 44* 1 37 0 01 1 3 20 44 58 43 59 0 63 -1 3 20 14 05* 1 1 51 0 01 -3 3 20 28 78 30 68 0 54 -5 3 20 8 53* 8 67 0 00 -7 3 20 5 50* 1 39 0 00 -9 3 20 28 60 27 71 0 46 1 1 3 20 13 14* 1 81 0 01 13 3 20 23 34 22 96 0 24 14 3 19 12 71* 1 76 0 01 12 3 19 12 89* 1 96 0 01 10 3 19 12 20* 2 18 0 01 -8 3 19 5 80* 2 00 0 03 -6 3 19 3 51* 13 67 0 01 -4 3 19 1 1 39* 10 48 0 01 -2 3 19 9 65* 12 06 0 01 0 3 19 7 29* 12 23 0 00 2 3 19 9 05* 10 59 O OS 4 3 19 10 68* 3 47 0 11 6 3 19 11 99* 0 96 0 01 8 3 19 9 64* 8 77 0 00 10 3 19 12 59* 3 12 0 01 12 3 19 13 40* 9 39 0 01 13 3 18 29 33 28 59 0 38 1 1 3 18 12 20* 1 1 54 0 01 9 3 18 25 92 25 1 1 0 43 7 3 18 13 59* 20 74 0 01 5 3 18 43 70 42 62 0 66 3 3 18 26 77 25 49 0 54 1 3 18 39 91 40 71 0 71 -1 3 18 27 28 26 55 0 61 -3 3 18 12 28* 5 08 0 01 -5 3 18 46 88 45 85 0 69 -7 3 18 27 18 25 75 0 57 -9 3 18 23 98 25 96 0 42 1 1 3 18 19 42 19 84 0 27 13 3 18 12 33* 2 78 0 01 15 3 18 13 30* 3 56 0 01 16 3 17 18 01 * 11 67 0 01 14 3 17 10 75* 3 55 0 00 12 3 17 12 38* 5 76 0 01 10 3 17 1 1 42* 2 71 0 01 -8 3 17 11 48* 2 22 0 01 -6 3 17 12 21* 1 1 42 0 19 h k l Fo Fc weight -4 3 17 20 04 20 17 0 47 -2 3 17 14 92* 13 05 0 02 0 3 17 8 97* 12 12 0 1 1 2 3 17 15 04* 20 4 1 0 02 4 3 17 1 1 07* 0 45 0 01 6 3 17 11 38* 5 45 0 01 8 3 17 7 45* 5 7 1 0 00 10 3 17 12 70* 12 86 0 13 12 3 17 10 59* 1 37 O 08 14 3 17 13 19* 8 39 0 01 15 3 16 13 52* 1 55 0 01 13 3 16 27 38 27 05 0 4 1 11 3 16 23 42 21 92 O 40 9 3 16 43 90 44 70 0 68 7 3 16 41 04 42 55 0 72 5 3 16 14 64* 9 90 0 02 3 3 16 82 93 83 19 0 23 1 3 16 63 82 63 02 0 41 -1 3 16 49 31 50 20 0 62 -3 3 16 50 80 52 57 0 58 -5 3 16 39 89 39 99 0 82 -7 3 16 10 91* 1 1 13 O 16 -9 3 16 10 84* 10 98 0 01 -11 3 16 22 89 21 1 1 0 45 -13 3 16 15 90 13 97 0 20 -15 3 16 9 97* 17 56 0 00 -17 3 16 15 83* 9 39 0 13 -18 3 15 13 59* 0 92 0 01 -16 3 15 14 76* 7 1 1 0 01 -14 3 15 12 21* 0 09 0 01 -12 3 15 13 42* 1 1 32 0 01 -10 3 15 10 92* 15 02 0 01 -8 3 15 1 86* 6 94 0 01 -6 3 15 10 35* 10 50 0 01 -4 3 15 18 23 20 72 0 52 -2 3 15 4 70* 0 95 0 05 0 3 15 32 89 33 43 0 94 2 3 15 36 15 36 94 0 89 4 3 15 34 50 33 28 0 88 6 3 15 10 75* 8 1 1 0 01 8 3 15 10 63* 0 49 0 01 10 3 15 1 1 64* 13 53 0 01 12 3 15 7 71* 2 59 0 00 14 3 15 12 18* 4 08 0 01 16 3 15 18 03* 8 39 0 01 17 3 14 17 23 16 40 0 15 15 3 14 24 29 25 00 0 33 13 3 14 19 54 23 42 0 30 1 1 3 14 57 24 58 42 0 48 h k l Fo Fc weight 9 3 14 10 83* 9 02 0 01 7 3 14 25 99 27 39 0 70 5 3 14 24 09 2 1 88 0 78 3 3 14 59 86 59 7 1 0 46 1 3 14 81 38 80 27 0 22 - 1 3 14 66 73 70 51 0 38 -3 3 14 59 07 59 15 0 50 -5 3 14 13 85* 17 93 0 02 -7 3 14 6 55* 19 47 0 00 -9 3 14 45 00 44 56 0 68 - 1 1 3 14 10 5 1 * 2 4 1 0 01 -13 3 14 28 66 25 63 0 55 -15 3 14 5 85* 2 96 0 03 - 17 3 14 15 45* 16 02 0 01 - 18 3 13 6 52* 12 09 0 02 -16 3 13 6 44* 6 2 1 0 03 -14 3 13 10 98* 2 35 0 01 -12 3 13 1 1 07* 2 58 0 01 -10 3 13 13 37 12 76 0 26 -8 3 13 14 56 15 23 0 42 -6 3 13 9 37* 8 80 0 01 -4 3 13 17 47 17 46 0 65 -2 3 13 8 67* 1 1 05 0 20 0 3 13 22 04 22 7 1 0 88 2 3 13 43 4 1 43 54 0 91 4 3 13 9 64* 14 4 1 0 01 6 3 13 37 96 36 68 0 95 8 3 13 46 02 45 35 0 78 10 3 13 19 26 20 64 0 4 1 12 3 13 7 20* 1 82 0 06 14 3 13 12 05* 0 63 0 01 16 3 13 9 16* 8 05 0 00 17 3 12 1 1 71* 0 7 1 0 01 15 3 12 29 75 30 17 0 52 13 3 12 12 70* 6 76 0 17 1 1 3 12 36 15 38 09 0 78 9 3 12 63 42 65 55 0 40 7 3 12 47 31 49 39 0 67 5 3 12 78 85 79 02 0 27 3 3 12 16 78 16 30 0 65 1 3 12 79 02 81 93 0 24 - 1 3 12 59 69 61 44 0 47 -3 3 12 35 21 33 07 1 14 -5 3 12 88 51 91 68 0 21 -7 3 12 1 1 13 12 27 0 30 -9 3 12 75 56 77 93 0 27 - 1 1 3 12 3 1 44 30 4 1 0 81 -13 3 12 36 72 35 73 0 74 -15 3 12 45 43 44 44 0 64 h k l Fo Fc weight -17 3 12 12 10* 1 55 O 01 -19 3 12 13 55* 5 25 0 01 -20 3 1 1 3 23* 5 12 0 01 -18 3 1 1 7 04* 2 77 O oo -16 3 1 1 13 83* 2 00 0 01 -14 3 11 8 87* 12 45 0 01 -12 3 1 1 9 74* 4 28 0 15 - 10 3 1 1 9 71* 4 45 0 01 -8 3 1 1 10 02* 7 46 O 25 -6 3 1 1 32 03 33 29 1 18 -4 3 1 1 40 42 4 1 10 O 91 -2 3 1 1 19 38 18 89 1 02 O 3 1 1 25 6 1 26 40 1 28 2 3 11 9 33* 10 24 O 01 4 3 1 1 3 34* 6 4 1 0 03 6 3 1 1 21 40 21 77 O 93 8 3 1 1 25 57 27 22 O 90 10 3 1 1 33 06 35 4 1 O 90 12 3 1 1 10 30* 2 72 O 01 14 3 1 1 30 24 32 50 0 61 16 3 1 1 10 47* 10 96 O 01 18 3 1 1 12 69* 7 43 0 01 19 3 10 14 12* 15 65 0 01 17 3 10 12 56* 1 1 OO 0 01 15 3 10 17 54 16 22 0 29 13 3 10 62 92 64 00 0 45 1 1 3 IO 9 85* 7 48 o 01 9 3 10 1 16 61 122 85 0 14 7 3 10 33 13 34 50 1 13 5 3 10 40 34 42 77 1 05 3 3 10 49 82 53 19 o 56 1 3 10 27 52 27 26 1 4 1 - 1 3 10 151 57 153 73 0 09 -3 3 10 13 25 13 38 0 66 -5 3 10 108 62 112 74 0 14 -7 3 10 51 93 54 14 0 59 -9 3 10 25 92 26 23 1 04 - 1 1 3 10 36 02 37 13 0 95 -13 3 10 14 23 17 95 o 27 -15 3 10 30 01 28 35 o 65 -17 3 10 1 1 64* 1 68 0 01 -19 3 10 13 29* 13 58 o 01 -20 3 9 1 1 16* 0 53 o 00 -18 3 9 16 85* 3 72 0 01 -16 3 9 1 1 58* 1 1 30 0 01 -14 3 9 10 88* 15 04 0 01 - 12 3 9 9 79* 1 75 0 01 - 10 3 9 44 77 47 38 0 84 -8 3 9 18 38 17 13 0 87 h k 1 Fo Fc weight h k 1 Fo Fc weight h k 1 Fo Fc we i ght h k 1 Fo Fc weight -6 3 9 42 45 44 45 0 89 10 3 7 9 20* 2 24 0 01 19 3 4 18 53 18 88 0 24 7 3 2 47 72 46 16 0 72 -4 3 9 20 75 19 85 1 31 12 3 7 20 54 20 90 0 67 17 3 4 5 53* 5 75 0 03 5 3 2 1 14 OO 1 13 37 0 15 -2 3 9 26 65 28 47 1 54 14 3 7 20 89 21 54 0 50 15 3 4 36 93 33 77 0 80 3 3 2 102 42 101 74 0 18 O 3 9 10 31* 8 63 O 03 16 3 7 1 1 46* 1 59 0 01 13 3 4 62 14 64 2 1 0 35 1 3 2 104 34 96 63 O 18 H 2 3 9 7 89* 12 52 0 02 18 3 7 12 08* 5 69 0 01 1 1 3 4 57 26 57 59 0 45 - 1 3 2 192 21 186 29 0 06 fa 4 3 9 41 76 42 05 0 99 20 3 7 10 38* 6 31 0 00 9 3 4 112 23 1 10 30 0 13 -3 3 2 63 69 62 71 0 4 1 6 3 9 24 08 24 93 1 23 19 3 6 12 70* 2 77 0 01 7 3 4 76 74 74 95 0 29 -5 3 2 170 51 170 95 0 08 8 3 9 31 43 33 89 1 10 17 3 6 37 56 37 1 1 0 66 5 3 4 226 17 219 20 O 05 -7 3 2 1 14 42 1 17 34 0 14 10 3 9 10 56* 21 29 0 01 15 3 6 19 24 21 36 0 40 3 3 4 82 36 78 47 0 28 -9 3 2 56 10 57 84 0 52 12 3 9 11 23* 5 49 0 01 13 3 6 10 15* 2 52 0 01 1 3 4 190 53 181 15 O 06 - 1 1 3 2 74 69 75 89 0 29 14 3 9 7 21* 1 80 0 00 1 1 3 6 73 12 73 96 0 30 - 1 3 4 130 10 126 07 0 12 -13 3 2 30 16 29 70 1 03 16 3 9 6 65* 2 92 0 00 9 3 6 46 75 47 50 0 69 -3 3 4 14 37 12 78 1 60 -15 3 2 36 63 34 69 0 84 18 3 9 15 80* 0 85 0 01 7 3 6 134 82 138 65 0 1 1 -5 3 4 ioo 50 100 65 0 17 - 17 3 2 17 37 13 89 0 32 19 3 8 9 29* 8 98 O 00 5 3 6 127 66 125 33 0 12 -7 3 4 32 04 31 39 1 54 - 19 3 2 22 07 17 62 0 38 17 3 8 34 19 33 37 O 60 3 3 6 105 70 99 73 0 16 -9 3 4 81 09 84 53 0 25 -21 3 2 26 75 21 84 0 34 15 3 8 1 1 47* 16 09 O Ol 1 3 6 1 15 66 1 1 1 24 O 14 - 1 1 3 4 36 77 36 58 1 09 -20 3 1 12 68* 10 43 0 01 13 3 8 49 09 50 55 0 71 -1 3 6 28 58 27 34 1 81 - 13 3 4 4 1 99 41 70 0 89 -18 3 1 10 75* 6 41 0 01 11 3 8 6 44* 7 46 O OO -3 3 6 201 61 197 58 0 06 - 15 3 4 39 21 36 44 O 82 -16 3 1 10 42* 1 96 0 01 9 3 8 43 55 47 00 0 80 -5 3 6 73 33 75 63 0 31 - 17 3 4 6 01* 8 09 0 04 - 14 3 1 10 04* 9 92 0 01 7 3 8 83 88 89 04 O 24 -7 3 6 88 22 90 73 0 23 - 19 3 4 23 49 20 88 0 38 - 12 3 1 7 46* 1 1 72 0 01 5 3 8 10 03* 7 64 O 02 -9 3 6 92 99 96 47 0 21 -21 3 4 12 89* 4 8 1 O 01 - 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1 7 14 8 61* 6 63 0 00 7 7 10 19 OO 18 53 0 29 12 6 1S 13 40* 1 14 0 01 -1 6 21 4 29* 1 66 0 00 -3 7 14 24 10 24 80 0 41 5 7 10 18 32 19 43 0 28 10 € 16 14 77* 7 58 0 01 -3 6 21 13 74* 2 03 0 01 -5 7 14 9 2 1 * 7 15 0 07 3 7 10 10 23* 6 13 o 01 -8 6 16 1 1 27* 21 69 0 OO -4 7 19 13 87* 9 07 0 01 -7 7 14 14 38* 13 65 0 01 1 7 10 1 1 10* 4 80 0 01 -6 6 16 5 51* 1 1 29 0 00 -2 7 19 13 51* 23 03 0 01 -9 7 14 12 92* 1 07 c 01 - 1 7 10 7 14* 3 20 o OO -4 6 16 .29 22 32 89 0 50 0 7 19 10 49* 0 76 0 00 - 1 1 7 14 7 44* 6 59 0 03 -3 7 10 14 81* 0 63 0 01 h k 1 Fo Fc weight -5 7 10 1 1 71* 14 97 0 01 -7 7 10 11 19* 2 43 0 01 -9 7 10 13 17* 14 27 0 15 1 1 7 10 8 89* 4 31 0 00 13 7 10 9 85* 6 84 0 06 15 7 10 18 75* 1 1 41 0 01 14 7 9 13 09* 15 34 0 01 12 7 9 12 18* 8 14 0 01 10 7 9 24 06 23 53 0 42 -8 7 9 48 23 48 33 0 64 -6 7 9 28 89 28 65 0 63 -4 7 9 53 35 53 69 0 48 -2 7 9 9 95* 7 20 0 01 O 7 9 57 24 55 60 0 50 2 7 9 73 65 73 07 0 29 4 7 9 30 03 28 40 0 63 6 7 9 45 42 45 24 0 65 8 7 9 1 1 50* 3 43 0 01 10 7 9 25 75 26 05 0 41 12 7. 9 12 73* 2 77 0 01 14 7 9 4 25* 7 79 0 00 15 7 8 12 15* 12 96 0 00 13 7 8 12 87* 9 38 0 01 1 1 7 8 12 13* 8 70 0 01 9 7 8 13 69* 6 89 0 01 7 7 8 13 45* 10 59 0 18 5 7 8 1 1 45* 0 94 0 01 3 7 8 28 68 28 35 0 63 1 7 8 13 85* 1 1 1 1 0 01 -1 7 8 25 99 25 81 0 62 -3 7 8 5 91* 8 28 0 05 -5 7 8 10 88* 4 58 0 01 -7 7 8 11 25* 12 66 0 01 -9 7 8 1 1 30* 2 02 0 01 11 7 8 14 75 16 06 0 18 13 7 8 12 25* 7 62 0 01 15 7 8 17 92* 1 1 09 0 01 16 7 7 12 86* 6 43 0 01 14 7 7 8 93* 14 23 0 05 12 7 7 1 1 74* 9 74 0 01 10 7 7 40 75 41 19 0 66 -8 7 7 11 21* 9 69 0 14 -6 7 7 51 90 51 56 0 63 -4 7 7 27 43 28 06 0 68 -2 7 7 32 35 31 54 0 78 0 7 7 43 82 43 32 0 75 2 7 7 20 24 19 49 0 46 4 7 7 30 55 31 05 0 70 6 7 7 24 42 24 78 0 50 h k 1 Fo Fc we 1ght 8 7 7 27 08 28 39 0 52 10 7 7 45 98 45 55 0 61 12 7 7 12 57* 1 1 37 0 01 14 7 7 12 48* 25 91 0 00 15 7 6 10 33* 15 97 0 00 13 7 6 12 92* 13 38 0 01 1 1 7 6 21 76 24 49 0 34 9 7 6 8 39* 1 41 0 07 7 7 6 19 81 19 23 0 40 5 7 6 18 82 19 02 0 37 3 7 6 19 78 17 51 0 46 1 7 6 13 90* 5 00 0 02 -1 7 6 17 34 17 33 0 39 -3 7 6 12 24* 5 99 0 01 -5 7 6 17 43 18 70 0 36 -7 7 6 28 36 28 38 0 67 -9 7 6 28 04 29 42 0 60 11 7 6 18 85 21 37 0 30 13 7 6 5 95* 3 89 0 03 15 7 6 1 1 02* 3 70 0 00 16 7 5 22 68 19 77 0 25 14 7 5 9 05* 1 43 0 OO 12 7 5 27 47 25 75 0 49 10 7 5 50 46 52 80 0 61 -8 7 5 29 57 27 80 0 66 -6 7 5 36 44 37 00 0 78 -4 7 5 7 57* 14 14 0 00 -2 7 5 79 79 81 64 0 24 0 7 5 37 04 37 26 o 88 2 7 5 61 49 60 15 0 42 4 7 5 47 85 46 37 0 70 6 7 5 34 24 35 14 0 74 8 7 5 48 37 46 55 0 66 10 7 5 1 1 84* 3 48 0 01 12 7 5 26 16 27 16 0 42 14 7 5 1 1 48* 13 18 0 08 16 7 5 12 86* 16 32 0 01 15 7 4 14 41* 2 59 0 01 13 7 4 12 10* 10 75 o 01 11 7 4 8 97* 14 79 0 07 9 7 4 5 15* 9 06 0 OO 7 7 4 1 1 08* 5 39 0 01 5 7 4 24 87 25 02 0 62 3 7 4 10 50* 15 15 0 01 1 7 4 24 57 24 17 0 75 - 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1 9 10 31 65 31 .92 o 42 -3 8 5 15 01* 24. 89 0 01 7 8 9 31 49 33 22 0 49 1 8 13 22 86 23 07 0 31 -3 9 10 13 48* 8 .80 0 01 -5 8 5 30 36 28 85 0 62 5 8 9 12 51* 13 77 0 01 - 1 8 13 12 38* 0 50 o 01 -5 9 10 17 53 16 32 0 16 -7 8 5 21 28 21 21 0 38 3 8 9 26 46 25 63 0 44 -3 8 13 12 79* 4 28 0 01 -7 9 10 17 98* 17 .69 0 01 -9 8 5 18 05 21 33 0 24 1 8 9 6 02* 5 56 0 03 -5 8 13 18 26* 18 63 0 01 -8 9 9 3 35* 9 37 o OI 1 1 8 5 12 59* 3 90 0 01 -1 8 9 34 24 34 37 0 61 -7 8 13 10 59* 2 67 0 07 -6 9 9 13 78* 8 14 0 01 13 8 5 13 39* 16 33 0 01 -3 8 9 5 79* 3 57 0 03 -9 8 13 6 19* 14 48 0 02 -4 9 9 12 95* 6 55 0 01 14 8 6 13 43* 0 91 0 01 -5 8 9 12 26* 19 70 0 01 -8 8 14 17 05* 2 23 0 01 -2 9 9 12 39* 8 95 0 01 12 8 6 14 89* 10 24 0 01 -7 8 9 12 25* 18 45 0 01 -6 8 14 14 48* 17 82 0 01 0 9 9 15 16* 1 65 0 01 h k 1 Fo Fc weight h k 1 Fo Fc weight h k 1 Fo Fc we i ght h k 1 Fo Fc weight 2 9 9 8 33* 2 28 0 04 7 9 4 12 95* 2 04 0 01 5 9 0 8 34* 3 59 0 06 1 10 7 12.78* 20 .94 0.01 4 9 9 1 1 64* 3 81 0 oo 5 9 4 25 37 22 50 0 40 3 9 0 43 57 41 54 0 60 -1 10 7 17.02* 2 .70 0.01 6 9 9 9 36* 5 77 0 oo 3 9 4 10 35* 20 46 0 00 1 9 0 29 79 29 7 1 0 54 -3 10 7 18.15* 16 . 28 0.01 8 9 9 6 06* 2 53 0 00 1 9 4 19 77 18 65 0 28 0 10 0 10 93* 8 15 0 00 -5 10 7 18.34* 17 .46 0.01 9 9 8 6 07* 2 27 0 oo -1 9 4 34 53 33 62 O 59 2 10 0 12 70* 0 49 0 01 -2 10 8 13.39* 4 . 23 0.01 7 9 8 17 01 14 85 0 15 -3 9 4 13 52* 9 39 0 01 4 10 0 8 37* 6 74 0 00 0 10 8 12.14* 1 .81 0.00 5 9 8 13 17* 1 85 0 01 -5 9 4 25 77 25 94 0 4 1 6 10 0 12 01* 4 28 0 oo 2 10 8 13.62* 12 . 72 0.01 3 9 8 39 48 39 39 0 53 -7 9 4 5 54* 2 37 O 02 7 10 1 23 75 24 62 0 24 1 9 8 13 11* 9 42 0 01 -9 9 4 24 54 25 17 0 29 5 10 1 13 28* 4 40 0 01 3290 r e f l e c t Ions 1 9 8 38 22 36 99 0 56 -11 9 4 12 83* 3 75 0 01 3 10 1 4 16* 22 17 0 OO 3 9 8 15 97 16 45 0 16 -10 9 3 13 1 1* 14 63 0 09 1 10 1 8 78* 1 29 0 04 5 9 8 4 78* 8 70 0 01 -8 9 3 7 05* 7 34 0 OO - 1 10 1 16 55* 19 67 0 01 7 9 8 22 46 24 12 0 25 -6 9 3 9 60* 7 62 0 07 -3 10 1 12 49* 19 53 0 00 9 9 8 15 90* 1 38 0 01 -4 9 3 11 78* 4 42 0 01 -5 10 1 17 37* 16 78 0 01 0 9 7 17 09* 15 27 0 01 -2 9 3 15 47* 2 18 0 01 -7 10 1 6 07* 24 69 0 00 8 9 7 14 94* 1 1 50 0 13 0 9 3 3 86* 5 81 0 00 -6 10 2 13 04* 9 40 0 01 6 9 7 6 39* 12 17 0 02 2 9 3 27 09 24 77 0 47 -4 10 2 13 03* 2 82 0 01 4 9 7 8 97* 3 76 0 OO 4 9 3 12 65* 10 96 0 01 -2 10 2 12 81* 1 1 40 0 01 2 9 7 13 64* 18 54 0 13 6 9 3 12 56* 1 63 0 01 O 10 2 5 86* 0 91 0 00 0 9 7 7 70* 2 66 0 05 8 9 3 13 1 1* 12 06 0 01 2 10 2 16 36 10 36 0 15 2 9 7 13 80* 0 04 0 01 10 9 3 13 30* 2 94 0 01 4 10 2 5 93* 1 1 1 0 02 4 9 7 11 40* 27 76 0 00 11 9 2 13 65* 2 92 0 01 6 10 2 10 76* 14 34 0 06 6 9 7 15 89* 1 54 0 01 9 9 2 35 55 36 01 0 45 7 10 3 13 84* 1 23 0 01 8 9 7 6 57* 1 66 0 02 7 9 2 21 37 22 74 0 28 5 10 3 18 96* 26 65 0 01 0 9 7 17 79* 8 05 0 01 5 9 2 31 61 31 45 0 51 3 10 3 13 17* 1 1 25 0 01 9 9 6 13 25* 1 1 67 0 01 3 9 2 30 59 29 18 0 55 1 10 3 15 77* 15 60 0 13 7 9 6 22 31 23 85 0 24 1 9 2 16 32* 7 52 0 01 - 1 10 3 34 93 33 21 0 46 5 9 6 20 16 20 09 0 25 -1 9 2 34 99 35 50 0 61 -3 10 3 13 22* 0 19 0 01 3 9 6 12 60* 14 76 0 01 -3 9 2 12 35* 1 1 36 0 01 -5 10 3 13 82* 21 97 o 01 1 9 6 34 08 34 99 0 54 -5 9 2 34 38 34 99 o 58 -7 10 3 21 17 16 61 0 21 1 9 6 15 73* 8 95 0 01 -7 9 2 20 33 21 92 o 27 -6 10 4 6 7 1 * 10 17 0 02 •3 9 6 43 82 43 18 0 60 -9 9 2 15 90 14 48 o 14 -4 10 4 6 06* 5 12 0 02 5 9 6 16 52* 10 03 0 01 -11 9 2 20 98 19 40 0 22 -2 10 4 13 22* 4 15 0 01 7 9 6 21 52 24 20 0 26 -12 9 1 17 77* 1 89 o 01 0 10 4 13 1 1 * 3 31 0 01 •9 9 6 23 30 20 66 0 26 -10 9 1 12 90* 12 94 0 01 2 10 4 6 56* 1 38 0 02 1 9 6 16 69* 1 71 0 01 -8 9 1 13 17* 6 77 0 01 4 10 4 13 67* 7 51 0 01 0 9 5 13 10* 1 81 0 01 -6 9 1 15 84* 13 81 0 01 6 10 4 13 86* 1 79 0 01 •8 9 5 10 42* 5 40 0 07 -4 9 1 3 89* 5 42 0 00 5 10 5 16 09* 15 32 0 12 -6 9 5 12 50* 12 04 0 01 -2 9 1 5 44* 8 34 0 00 3 10 5 13 46* 2 84 0 01 -4 9 5 12 54* 9 03 0 01 0 9 1 1 1 96* 3 65 0 01 1 10 5 28 00 29 4 1 0 32 -2 9 5 12 18* 18 41 0 01 2 9 1 29 69 29 4 1 0 54 - 1 10 5 13 45* 12 55 0 01 0 9 5 10 70* 10 16 0 09 4 9 1 12 41* 8 13 0 01 -3 10 5 4 22* 30 79 0 00 2 9 5 12 22* 1 39 0 01 6 9 1 13 14* 8 31 0 01 -5 10 5 9 1 1 * 14 56 0 04 4 9 5 17 17 17 16 0 21 8 9 1 13 17* 9 86 0 01 -4 10 6 13 36* 7 40 0 09 6 9 5 6 71* 7 20 0 03 10 9 1 4 18* 14 13 0 00 -2 10 6 13 67* 5 60 0 01 8 9 5 12 85* 4 33 0 01 12 9 1 13 54* 7 57 0 01 0 10 6 1 1 94* 13 24 0 00 0 9 5 13 48* 9 35 0 01 1 1 9 0 16 42* 12 36 0 01 2 10 6 13 4 1 * 1 1 37 0 01 1 9 4 22 20 21 27 0 21 9 9 0 13 4 1 * 13 39 0 01 4 10 6 16 26* 14 05 0 12 9 9 4 22 80 21 77 0 25 7 9 0 28 38 27 61 0 44 3 10 7 19 45 17 10 0 17 to 

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