+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 14:59:50 on 09-Oct-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 03src0043r in P-1 CELL 0.71073 8.8931 9.0266 13.6881 72.225 77.234 77.122 ZERR 2.00 0.0003 0.0002 0.0006 0.002 0.002 0.002 LATT 1 SFAC C H BR N O UNIT 38 66 2 4 2 V = 1006.10 F(000) = 408.0 Mu = 2.05 mm-1 Cell Wt = 770.77 Rho = 1.272 MERG 2 OMIT -3.00 55.00 EXTI 0.00677 DFIX 0.84 H51 O1 H50 O1 DANG 1.37 H51 H50 FMAP 2 PLAN 10 SIZE 0.01 0.20 0.24 ACTA BOND $H WGHT 0.03750 0.64940 L.S. 10 TEMP -153.00 FVAR 0.47999 BR1 3 0.165567 0.125600 0.577753 11.00000 0.02865 0.02842 = 0.06107 -0.01628 -0.00912 -0.00507 N1 4 0.389700 0.760293 0.363325 11.00000 0.02432 0.02220 = 0.02736 -0.00784 -0.00385 -0.00413 N2 4 0.249005 0.593142 0.359251 11.00000 0.02301 0.02429 = 0.02977 -0.00793 -0.00441 -0.00502 C1 1 0.417187 1.356463 -0.097785 11.00000 0.06457 0.04762 = 0.03595 -0.00491 -0.00475 0.00390 AFIX 137 H1A 2 0.445603 1.442904 -0.080177 11.00000 -1.50000 H1B 2 0.340674 1.399594 -0.145297 11.00000 -1.50000 H1C 2 0.510859 1.298877 -0.131478 11.00000 -1.50000 AFIX 0 C2 1 0.346691 1.245111 0.000589 11.00000 0.04613 0.03316 = 0.03760 -0.00780 -0.01092 -0.00032 AFIX 23 H2A 2 0.251710 1.303855 0.033881 11.00000 -1.20000 H2B 2 0.314624 1.160377 -0.018060 11.00000 -1.20000 AFIX 0 C3 1 0.458244 1.171458 0.077553 11.00000 0.03685 0.02934 = 0.03951 -0.00598 -0.00605 -0.00810 AFIX 23 H3A 2 0.493664 1.256770 0.093434 11.00000 -1.20000 H3B 2 0.551352 1.109895 0.044654 11.00000 -1.20000 AFIX 0 C4 1 0.390133 1.064428 0.178478 11.00000 0.03360 0.02844 = 0.03891 -0.00572 -0.00803 -0.00746 AFIX 23 H4A 2 0.356770 0.977412 0.163214 11.00000 -1.20000 H4B 2 0.296194 1.125051 0.211336 11.00000 -1.20000 AFIX 0 C5 1 0.505247 0.994728 0.254725 11.00000 0.02869 0.02297 = 0.03803 -0.00726 -0.00606 -0.00678 AFIX 23 H5A 2 0.591133 0.921210 0.225907 11.00000 -1.20000 H5B 2 0.551503 1.081155 0.260583 11.00000 -1.20000 AFIX 0 C6 1 0.435331 0.907530 0.362433 11.00000 0.03302 0.02203 = 0.03733 -0.01056 -0.00961 -0.00412 AFIX 23 H6A 2 0.512549 0.882892 0.409702 11.00000 -1.20000 H6B 2 0.342239 0.976529 0.388917 11.00000 -1.20000 AFIX 0 C7 1 0.248496 0.740398 0.359269 11.00000 0.02610 0.02480 = 0.02895 -0.00782 -0.00571 -0.00240 AFIX 43 H7 2 0.158740 0.820676 0.356710 11.00000 -1.20000 AFIX 0 C8 1 0.490338 0.617529 0.366309 11.00000 0.02474 0.02239 = 0.02339 -0.00628 -0.00046 -0.00420 C9 1 0.648512 0.572917 0.373041 11.00000 0.02611 0.02755 = 0.02846 -0.00688 -0.00537 -0.00422 AFIX 43 H9 2 0.709838 0.645379 0.375036 11.00000 -1.20000 AFIX 0 C10 1 0.711160 0.418348 0.376645 11.00000 0.02499 0.03143 = 0.02941 -0.00772 -0.00220 -0.00117 AFIX 43 H10 2 0.819036 0.383010 0.380912 11.00000 -1.20000 AFIX 0 C11 1 0.620554 0.310864 0.374213 11.00000 0.03462 0.02131 = 0.03126 -0.00870 -0.00034 -0.00038 AFIX 43 H11 2 0.668747 0.204857 0.377088 11.00000 -1.20000 AFIX 0 C12 1 0.464305 0.354769 0.367796 11.00000 0.03384 0.02508 = 0.02752 -0.00928 -0.00156 -0.00797 AFIX 43 H12 2 0.402961 0.282091 0.366147 11.00000 -1.20000 AFIX 0 C13 1 0.400872 0.510934 0.363851 11.00000 0.02507 0.02596 = 0.02131 -0.00551 -0.00281 -0.00526 C14 1 0.117551 0.528293 0.349634 11.00000 0.02602 0.03128 = 0.03661 -0.00921 -0.00277 -0.01062 AFIX 23 H14A 2 0.018317 0.596606 0.368562 11.00000 -1.20000 H14B 2 0.116493 0.422087 0.398871 11.00000 -1.20000 AFIX 0 C15 1 0.128023 0.516549 0.240193 11.00000 0.03216 0.03231 = 0.03576 -0.01226 -0.00576 -0.01147 AFIX 23 H15A 2 0.049996 0.453165 0.240837 11.00000 -1.20000 H15B 2 0.232888 0.459170 0.218833 11.00000 -1.20000 AFIX 0 C16 1 0.100947 0.673767 0.159711 11.00000 0.03422 0.03208 = 0.03793 -0.01433 -0.00505 -0.00804 AFIX 23 H16A 2 0.177148 0.738741 0.159681 11.00000 -1.20000 H16B 2 -0.005258 0.730204 0.179231 11.00000 -1.20000 AFIX 0 C17 1 0.117134 0.655977 0.051014 11.00000 0.04011 0.03569 = 0.03626 -0.01330 -0.00507 -0.00857 AFIX 23 H17A 2 0.223499 0.599336 0.032116 11.00000 -1.20000 H17B 2 0.041639 0.589679 0.051900 11.00000 -1.20000 AFIX 0 C18 1 0.090248 0.809559 -0.032204 11.00000 0.04285 0.03755 = 0.04254 -0.00996 -0.00988 -0.01075 AFIX 23 H18A 2 -0.017406 0.864889 -0.015085 11.00000 -1.20000 H18B 2 0.163615 0.877513 -0.032233 11.00000 -1.20000 AFIX 0 C19 1 0.112249 0.787244 -0.139596 11.00000 0.07107 0.06196 = 0.03711 -0.00776 -0.00962 -0.01971 AFIX 137 H19A 2 0.218754 0.732895 -0.157273 11.00000 -1.50000 H19B 2 0.095416 0.890455 -0.190249 11.00000 -1.50000 H19C 2 0.036869 0.723887 -0.141031 11.00000 -1.50000 AFIX 0 O1 5 1.055623 0.151795 0.361936 11.00000 0.05706 0.05755 = 0.06258 -0.00966 -0.01316 -0.02050 H50 2 0.987812 0.084603 0.375728 11.00000 -1.50000 H51 2 1.077065 0.144163 0.425762 11.00000 -1.50000 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 Covalent radii and connectivity table for 03src0043r in P-1 C 0.770 H 0.320 BR 1.140 N 0.700 O 0.660 Br1 - no bonds found N1 - C7 C8 C6 N2 - C7 C13 C14 C1 - C2 C2 - C3 C1 C3 - C2 C4 C4 - C3 C5 C5 - C6 C4 C6 - N1 C5 C7 - N1 N2 C8 - C9 C13 N1 C9 - C10 C8 C10 - C9 C11 C11 - C12 C10 C12 - C11 C13 C13 - C12 C8 N2 C14 - N2 C15 C15 - C14 C16 C16 - C15 C17 C17 - C18 C16 C18 - C19 C17 C19 - C18 O1 - no bonds found 20601 Reflections read, of which 18 rejected -11 =< h =< 11, -11 =< k =< 11, -17 =< l =< 17, Max. 2-theta = 55.00 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 1 10 4 16.85 4.73 2 28.71 6 -5 5 10.03 1.32 5 10.54 6 -4 6 32.79 1.69 7 8.68 -5 5 6 3.16 0.79 7 4.52 -6 3 10 6.18 1.48 5 11.77 -2 7 10 4.44 0.97 6 8.53 -3 8 11 11.98 2.76 2 13.90 7 Inconsistent equivalents 4615 Unique reflections, of which 0 suppressed R(int) = 0.0727 R(sigma) = 0.0500 Friedel opposites merged Maximum memory for data reduction = 2702 / 45906 Default effective X-H distances for T = -153.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 3393 / 269878 wR2 = 0.0940 before cycle 1 for 4615 data and 217 / 217 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 0.9140 0.8400 0.0740 0.0200 DFIX H51 O1 Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.067 0.059 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.025; Restrained GooF = 1.027 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0375 * P )^2 + 0.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.47916 0.00082 -1.011 OSF 2 0.00640 0.00132 -0.280 EXTI Mean shift/su = 0.282 Maximum = -2.612 for z Br1 Max. shift = 0.014 A for H19A Max. dU = 0.001 for O1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3393 / 269878 wR2 = 0.0935 before cycle 2 for 4615 data and 217 / 217 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 0.9103 0.8400 0.0703 0.0200 DFIX H51 O1 Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.065 0.056 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.019; Restrained GooF = 1.022 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0375 * P )^2 + 0.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.47890 0.00082 -0.318 OSF 2 0.00625 0.00130 -0.115 EXTI Mean shift/su = 0.096 Maximum = -0.956 for z Br1 Max. shift = 0.005 A for H19B Max. dU = 0.000 for O1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3393 / 269878 wR2 = 0.0935 before cycle 3 for 4615 data and 217 / 217 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 0.9093 0.8400 0.0693 0.0200 DFIX H51 O1 Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.064 0.055 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.019; Restrained GooF = 1.022 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0375 * P )^2 + 0.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.47890 0.00082 0.000 OSF 2 0.00624 0.00130 -0.006 EXTI Mean shift/su = 0.004 Maximum = 0.042 for U33 Br1 Max. shift = 0.001 A for H51 Max. dU = 0.000 for O1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3393 / 269878 wR2 = 0.0935 before cycle 4 for 4615 data and 217 / 217 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 0.9092 0.8400 0.0692 0.0200 DFIX H51 O1 Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.064 0.055 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.020; Restrained GooF = 1.022 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0375 * P )^2 + 0.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.47891 0.00082 0.010 OSF 2 0.00624 0.00130 -0.002 EXTI Mean shift/su = 0.001 Maximum = 0.010 for OSF Max. shift = 0.000 A for H51 Max. dU = 0.000 for O1 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3393 / 269878 wR2 = 0.0935 before cycle 5 for 4615 data and 217 / 217 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 0.9091 0.8400 0.0691 0.0200 DFIX H51 O1 Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.064 0.055 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.020; Restrained GooF = 1.022 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0375 * P )^2 + 0.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.47891 0.00082 0.001 OSF 2 0.00624 0.00130 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H51 Max. dU = 0.000 for O1 Least-squares cycle 6 Maximum vector length = 511 Memory required = 3393 / 269878 wR2 = 0.0935 before cycle 6 for 4615 data and 217 / 217 parameters Disagreeable restraints before cycle 6 Observed Target Error Sigma Restraint 0.9091 0.8400 0.0691 0.0200 DFIX H51 O1 Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.064 0.055 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.020; Restrained GooF = 1.022 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0375 * P )^2 + 0.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.47891 0.00082 0.001 OSF 2 0.00624 0.00130 0.001 EXTI Mean shift/su = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H51 Max. dU = 0.000 for O1 Least-squares cycle 7 Maximum vector length = 511 Memory required = 3393 / 269878 wR2 = 0.0935 before cycle 7 for 4615 data and 217 / 217 parameters Disagreeable restraints before cycle 7 Observed Target Error Sigma Restraint 0.9091 0.8400 0.0691 0.0200 DFIX H51 O1 Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.064 0.054 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.020; Restrained GooF = 1.022 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0375 * P )^2 + 0.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.47891 0.00082 0.000 OSF 2 0.00624 0.00130 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H51 Max. dU = 0.000 for O1 Least-squares cycle 8 Maximum vector length = 511 Memory required = 3393 / 269878 wR2 = 0.0935 before cycle 8 for 4615 data and 217 / 217 parameters Disagreeable restraints before cycle 8 Observed Target Error Sigma Restraint 0.9091 0.8400 0.0691 0.0200 DFIX H51 O1 Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.064 0.054 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.020; Restrained GooF = 1.022 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0375 * P )^2 + 0.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.47891 0.00082 0.000 OSF 2 0.00624 0.00130 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H51 Max. dU = 0.000 for O1 Least-squares cycle 9 Maximum vector length = 511 Memory required = 3393 / 269878 wR2 = 0.0935 before cycle 9 for 4615 data and 217 / 217 parameters Disagreeable restraints before cycle 9 Observed Target Error Sigma Restraint 0.9091 0.8400 0.0691 0.0200 DFIX H51 O1 Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.064 0.055 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.020; Restrained GooF = 1.022 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0375 * P )^2 + 0.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.47891 0.00082 0.000 OSF 2 0.00624 0.00130 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for y Br1 Max. shift = 0.000 A for H51 Max. dU = 0.000 for C17 Least-squares cycle 10 Maximum vector length = 511 Memory required = 3393 / 269878 wR2 = 0.0935 before cycle 10 for 4615 data and 217 / 217 parameters Disagreeable restraints before cycle 10 Observed Target Error Sigma Restraint 0.9091 0.8400 0.0691 0.0200 DFIX H51 O1 Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.064 0.054 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.020; Restrained GooF = 1.022 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0375 * P )^2 + 0.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.47891 0.00082 0.000 OSF 2 0.00624 0.00130 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for x Br1 Max. shift = 0.000 A for H51 Max. dU = 0.000 for O1 Largest correlation matrix elements -0.718 y H50 / x H50 0.607 U11 Br1 / OSF 0.543 U33 Br1 / OSF 0.612 U22 Br1 / OSF -0.547 z H51 / x H51 0.541 EXTI / OSF Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.4470 1.4420 -0.0802 137 0.980 0.000 C1 C2 H1A H1B 0.3402 1.4006 -0.1449 137 0.980 0.000 C1 C2 H1A H1C 0.5101 1.2984 -0.1320 137 0.980 0.000 C1 C2 H1A H2A 0.2517 1.3038 0.0339 23 0.990 0.000 C2 C3 C1 H2B 0.3146 1.1603 -0.0180 23 0.990 0.000 C2 C3 C1 H3A 0.4938 1.2568 0.0933 23 0.990 0.000 C3 C2 C4 H3B 0.5514 1.1098 0.0446 23 0.990 0.000 C3 C2 C4 H4A 0.3565 0.9776 0.1633 23 0.990 0.000 C4 C3 C5 H4B 0.2963 1.1253 0.2114 23 0.990 0.000 C4 C3 C5 H5A 0.5911 0.9210 0.2258 23 0.990 0.000 C5 C6 C4 H5B 0.5519 1.0810 0.2604 23 0.990 0.000 C5 C6 C4 H6A 0.5126 0.8829 0.4097 23 0.990 0.000 C6 N1 C5 H6B 0.3423 0.9767 0.3889 23 0.990 0.000 C6 N1 C5 H7 0.1588 0.8208 0.3566 43 0.950 0.000 C7 N1 N2 H9 0.7098 0.6455 0.3752 43 0.950 0.000 C9 C10 C8 H10 0.8192 0.3831 0.3807 43 0.950 0.000 C10 C9 C11 H11 0.6688 0.2048 0.3771 43 0.950 0.000 C11 C12 C10 H12 0.4028 0.2822 0.3661 43 0.950 0.000 C12 C11 C13 H14A 0.0183 0.5968 0.3685 23 0.990 0.000 C14 N2 C15 H14B 0.1163 0.4221 0.3990 23 0.990 0.000 C14 N2 C15 H15A 0.0501 0.4531 0.2408 23 0.990 0.000 C15 C14 C16 H15B 0.2330 0.4592 0.2188 23 0.990 0.000 C15 C14 C16 H16A 0.1771 0.7389 0.1597 23 0.990 0.000 C16 C15 C17 H16B -0.0053 0.7302 0.1792 23 0.990 0.000 C16 C15 C17 H17A 0.2237 0.5994 0.0321 23 0.990 0.000 C17 C18 C16 H17B 0.0418 0.5896 0.0518 23 0.990 0.000 C17 C18 C16 H18A -0.0175 0.8650 -0.0152 23 0.990 0.000 C18 C19 C17 H18B 0.1635 0.8777 -0.0324 23 0.990 0.000 C18 C19 C17 H19A 0.2181 0.7308 -0.1566 137 0.980 0.000 C19 C18 H19A H19B 0.0977 0.8904 -0.1905 137 0.980 0.000 C19 C18 H19A H19C 0.0355 0.7257 -0.1414 137 0.980 0.000 C19 C18 H19A 03src0043r in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Br1 0.16555 0.12565 0.57767 1.00000 0.02841 0.02836 0.06104 -0.01632 -0.00899 -0.00506 0.03797 0.00035 0.00003 0.00003 0.00002 0.00000 0.00015 0.00015 0.00021 0.00011 0.00011 0.00009 0.00011 N1 0.38962 0.76030 0.36325 1.00000 0.02412 0.02100 0.02677 -0.00766 -0.00384 -0.00362 0.02376 0.00257 0.00021 0.00020 0.00015 0.00000 0.00093 0.00089 0.00106 0.00074 0.00078 0.00069 0.00040 N2 0.24911 0.59304 0.35935 1.00000 0.02280 0.02381 0.02937 -0.00781 -0.00401 -0.00533 0.02499 0.00262 0.00021 0.00021 0.00015 0.00000 0.00092 0.00094 0.00111 0.00077 0.00079 0.00071 0.00040 C1 0.41721 1.35635 -0.09783 1.00000 0.06496 0.04750 0.03563 -0.00521 -0.00505 0.00338 0.05338 0.00521 0.00041 0.00036 0.00024 0.00000 0.00207 0.00173 0.00173 0.00130 0.00147 0.00142 0.00080 H1A 0.44695 1.44203 -0.08016 1.00000 0.08007 0.00000 0.00000 H1B 0.34020 1.40057 -0.14495 1.00000 0.08007 0.00000 0.00000 H1C 0.51005 1.29841 -0.13201 1.00000 0.08007 0.00000 0.00000 C2 0.34668 1.24502 0.00060 1.00000 0.04596 0.03277 0.03757 -0.00776 -0.01073 -0.00027 0.03957 0.00404 0.00033 0.00030 0.00022 0.00000 0.00154 0.00134 0.00158 0.00111 0.00123 0.00110 0.00062 H2A 0.25173 1.30379 0.03391 1.00000 0.04749 0.00000 0.00000 H2B 0.31459 1.16026 -0.01800 1.00000 0.04749 0.00000 0.00000 C3 0.45832 1.17147 0.07748 1.00000 0.03669 0.02951 0.03840 -0.00562 -0.00544 -0.00795 0.03540 0.00375 0.00030 0.00029 0.00021 0.00000 0.00136 0.00125 0.00155 0.00105 0.00114 0.00100 0.00057 H3A 0.49382 1.25680 0.09329 1.00000 0.04248 0.00000 0.00000 H3B 0.55137 1.10982 0.04460 1.00000 0.04248 0.00000 0.00000 C4 0.39012 1.06452 0.17851 1.00000 0.03292 0.02783 0.03867 -0.00590 -0.00804 -0.00726 0.03314 0.00355 0.00029 0.00028 0.00021 0.00000 0.00128 0.00120 0.00153 0.00102 0.00110 0.00096 0.00055 H4A 0.35651 0.97759 0.16331 1.00000 0.03977 0.00000 0.00000 H4B 0.29634 1.12528 0.21141 1.00000 0.03977 0.00000 0.00000 C5 0.50538 0.99465 0.25465 1.00000 0.02912 0.02250 0.03757 -0.00698 -0.00607 -0.00734 0.02940 0.00330 0.00027 0.00026 0.00020 0.00000 0.00119 0.00110 0.00146 0.00096 0.00104 0.00088 0.00051 H5A 0.59108 0.92098 0.22582 1.00000 0.03528 0.00000 0.00000 H5B 0.55189 1.08096 0.26043 1.00000 0.03528 0.00000 0.00000 C6 0.43536 0.90760 0.36244 1.00000 0.03300 0.02080 0.03764 -0.01059 -0.00909 -0.00452 0.02931 0.00324 0.00028 0.00025 0.00020 0.00000 0.00123 0.00109 0.00146 0.00095 0.00107 0.00089 0.00052 H6A 0.51257 0.88291 0.40973 1.00000 0.03518 0.00000 0.00000 H6B 0.34230 0.97668 0.38889 1.00000 0.03518 0.00000 0.00000 C7 0.24853 0.74047 0.35922 1.00000 0.02611 0.02389 0.02764 -0.00737 -0.00536 -0.00242 0.02592 0.00318 0.00026 0.00025 0.00019 0.00000 0.00112 0.00110 0.00129 0.00089 0.00094 0.00084 0.00048 H7 0.15878 0.82076 0.35659 1.00000 0.03110 0.00000 0.00000 C8 0.49034 0.61762 0.36627 1.00000 0.02452 0.02110 0.02283 -0.00549 -0.00139 -0.00328 0.02341 0.00314 0.00025 0.00024 0.00018 0.00000 0.00108 0.00104 0.00122 0.00085 0.00089 0.00081 0.00046 C9 0.64856 0.57304 0.37308 1.00000 0.02580 0.02781 0.02794 -0.00703 -0.00488 -0.00499 0.02714 0.00331 0.00026 0.00026 0.00019 0.00000 0.00113 0.00115 0.00132 0.00093 0.00096 0.00087 0.00049 H9 0.70982 0.64547 0.37520 1.00000 0.03257 0.00000 0.00000 C10 0.71129 0.41839 0.37657 1.00000 0.02487 0.03084 0.02829 -0.00732 -0.00199 -0.00105 0.02913 0.00348 0.00027 0.00027 0.00019 0.00000 0.00114 0.00121 0.00134 0.00096 0.00097 0.00090 0.00051 H10 0.81920 0.38311 0.38071 1.00000 0.03496 0.00000 0.00000 C11 0.62063 0.31079 0.37419 1.00000 0.03455 0.02086 0.02970 -0.00820 0.00020 0.00001 0.02971 0.00354 0.00028 0.00026 0.00019 0.00000 0.00127 0.00110 0.00137 0.00093 0.00103 0.00089 0.00052 H11 0.66880 0.20476 0.37712 1.00000 0.03565 0.00000 0.00000 C12 0.46420 0.35479 0.36775 1.00000 0.03278 0.02457 0.02690 -0.00899 -0.00147 -0.00756 0.02772 0.00330 0.00027 0.00026 0.00019 0.00000 0.00123 0.00113 0.00131 0.00093 0.00099 0.00091 0.00050 H12 0.40279 0.28216 0.36611 1.00000 0.03326 0.00000 0.00000 C13 0.40093 0.51095 0.36377 1.00000 0.02427 0.02491 0.02054 -0.00527 -0.00233 -0.00509 0.02349 0.00312 0.00025 0.00025 0.00017 0.00000 0.00107 0.00108 0.00119 0.00085 0.00088 0.00082 0.00045 C14 0.11752 0.52832 0.34968 1.00000 0.02554 0.03036 0.03634 -0.00877 -0.00297 -0.01042 0.03020 0.00328 0.00027 0.00028 0.00020 0.00000 0.00115 0.00120 0.00145 0.00100 0.00101 0.00091 0.00052 H14A 0.01833 0.59675 0.36854 1.00000 0.03624 0.00000 0.00000 H14B 0.11631 0.42215 0.39895 1.00000 0.03624 0.00000 0.00000 C15 0.12808 0.51651 0.24019 1.00000 0.03175 0.03200 0.03589 -0.01219 -0.00571 -0.01105 0.03154 0.00330 0.00029 0.00028 0.00020 0.00000 0.00125 0.00123 0.00149 0.00103 0.00107 0.00097 0.00054 H15A 0.05011 0.45308 0.24082 1.00000 0.03785 0.00000 0.00000 H15B 0.23298 0.45918 0.21885 1.00000 0.03785 0.00000 0.00000 C16 0.10094 0.67383 0.15970 1.00000 0.03325 0.03234 0.03855 -0.01476 -0.00540 -0.00718 0.03331 0.00346 0.00030 0.00028 0.00021 0.00000 0.00128 0.00126 0.00154 0.00108 0.00111 0.00098 0.00055 H16A 0.17708 0.73886 0.15968 1.00000 0.03998 0.00000 0.00000 H16B -0.00530 0.73022 0.17920 1.00000 0.03998 0.00000 0.00000 C17 0.11724 0.65592 0.05095 1.00000 0.03939 0.03565 0.03646 -0.01381 -0.00474 -0.00893 0.03603 0.00364 0.00032 0.00029 0.00021 0.00000 0.00139 0.00135 0.00154 0.00110 0.00116 0.00106 0.00058 H17A 0.22365 0.59937 0.03206 1.00000 0.04324 0.00000 0.00000 H17B 0.04182 0.58956 0.05182 1.00000 0.04324 0.00000 0.00000 C18 0.09022 0.80972 -0.03230 1.00000 0.04156 0.03772 0.04243 -0.01024 -0.00951 -0.01034 0.03966 0.00384 0.00033 0.00031 0.00022 0.00000 0.00147 0.00141 0.00168 0.00117 0.00125 0.00112 0.00061 H18A -0.01747 0.86499 -0.01519 1.00000 0.04759 0.00000 0.00000 H18B 0.16354 0.87773 -0.03235 1.00000 0.04759 0.00000 0.00000 C19 0.11229 0.78717 -0.13960 1.00000 0.07128 0.06114 0.03613 -0.00732 -0.01016 -0.01947 0.05592 0.00475 0.00043 0.00040 0.00025 0.00000 0.00222 0.00198 0.00178 0.00143 0.00158 0.00165 0.00082 H19A 0.21809 0.73081 -0.15662 1.00000 0.08388 0.00000 0.00000 H19B 0.09767 0.89039 -0.19052 1.00000 0.08388 0.00000 0.00000 H19C 0.03547 0.72565 -0.14138 1.00000 0.08388 0.00000 0.00000 O1 1.05561 0.15187 0.36187 1.00000 0.05836 0.05991 0.06323 -0.00994 -0.01301 -0.02166 0.05961 0.00340 0.00029 0.00028 0.00020 0.00000 0.00144 0.00142 0.00163 0.00117 0.00123 0.00109 0.00060 H50 0.98738 0.08528 0.37547 1.00000 0.08941 0.03793 0.00398 0.00407 0.00312 0.00000 0.00000 H51 1.07790 0.14279 0.42535 1.00000 0.08941 0.03902 0.00482 0.00474 0.00201 0.00000 0.00000 Final Structure Factor Calculation for 03src0043r in P-1 Total number of l.s. parameters = 217 Maximum vector length = 511 Memory required = 3176 / 24017 wR2 = 0.0935 before cycle 11 for 4615 data and 0 / 217 parameters Disagreeable restraints before cycle 11 Observed Target Error Sigma Restraint 0.9091 0.8400 0.0691 0.0200 DFIX H51 O1 Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.040 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.064 0.054 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.020; Restrained GooF = 1.022 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0375 * P )^2 + 0.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0397 for 3747 Fo > 4sig(Fo) and 0.0563 for all 4615 data wR2 = 0.0935, GooF = S = 1.020, Restrained GooF = 1.022 for all data Occupancy sum of asymmetric unit = 23.00 for non-hydrogen and 33.00 for hydrogen atoms Principal mean square atomic displacements U 0.0611 0.0286 0.0242 Br1 0.0269 0.0242 0.0202 N1 0.0295 0.0244 0.0211 N2 0.0810 0.0449 0.0342 C1 0.0498 0.0386 0.0304 C2 0.0411 0.0371 0.0280 C3 0.0409 0.0319 0.0266 C4 0.0383 0.0296 0.0203 C5 0.0389 0.0307 0.0183 C6 0.0281 0.0265 0.0231 C7 0.0278 0.0214 0.0211 C8 0.0286 0.0275 0.0253 C9 0.0358 0.0286 0.0229 C10 0.0425 0.0279 0.0188 C11 0.0352 0.0259 0.0220 C12 0.0255 0.0248 0.0202 C13 0.0372 0.0330 0.0204 C14 0.0381 0.0347 0.0219 C15 0.0406 0.0335 0.0258 C16 0.0419 0.0370 0.0292 C17 0.0455 0.0403 0.0332 C18 0.0752 0.0569 0.0356 C19 0.0748 0.0596 0.0445 O1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.015 0.028 0.041 0.056 0.070 0.086 0.106 0.137 0.191 1.000 Number in group 464. 484. 438. 483. 459. 456. 455. 458. 453. 465. GooF 0.939 1.018 1.083 1.015 1.073 1.051 1.001 1.063 0.965 0.979 K 1.983 1.267 1.037 1.021 1.010 1.002 0.995 1.002 1.004 1.007 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.66 inf Number in group 476. 460. 452. 465. 455. 464. 457. 460. 462. 464. GooF 0.909 0.889 0.954 1.001 0.969 1.004 1.010 0.932 0.942 1.462 K 1.022 1.007 0.999 1.004 1.005 1.016 1.017 1.019 1.008 1.000 R1 0.169 0.132 0.107 0.087 0.063 0.051 0.039 0.029 0.025 0.030 Recommended weighting scheme: WGHT 0.0335 0.7260 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/su Fc/Fc(max) Resolution(A) 2 1 2 145.81 87.78 5.85 0.061 4.03 2 -2 2 250.55 166.90 5.38 0.085 2.49 4 4 3 48.99 91.00 5.11 0.062 1.75 0 0 3 6853.47 8226.61 4.32 0.593 4.29 1 1 2 666.62 524.33 4.31 0.150 5.65 -4 0 1 154.51 216.83 4.22 0.096 2.05 -2 2 2 321.00 410.45 4.05 0.133 2.62 -3 -5 12 122.19 0.29 3.99 0.004 0.77 3 1 2 290.55 374.07 3.86 0.127 2.89 3 -2 3 129.16 177.80 3.82 0.087 1.95 -1 -3 3 809.77 665.48 3.81 0.169 2.07 6 -3 9 63.75 32.03 3.72 0.037 0.93 5 3 1 42.33 17.90 3.67 0.028 1.63 -1 -1 4 341.01 268.44 3.65 0.107 2.57 0 -3 4 293.45 387.26 3.59 0.129 1.88 2 3 0 17.25 34.93 3.50 0.039 2.56 1 0 4 605.23 742.43 3.49 0.178 3.19 2 5 4 433.59 359.18 3.28 0.124 1.74 0 4 5 303.59 374.25 3.28 0.127 1.91 6 1 9 225.77 170.70 3.26 0.085 1.15 3 4 15 39.56 72.11 3.17 0.056 0.91 -2 -4 3 158.01 121.09 3.16 0.072 1.64 1 -7 9 34.10 65.12 3.15 0.053 0.82 0 9 10 67.15 102.42 3.14 0.066 0.88 1 -1 4 233.23 291.52 3.09 0.112 2.70 1 -1 3 134.83 182.67 3.08 0.088 3.29 -4 -3 3 39.72 17.02 3.05 0.027 1.54 4 0 3 232.02 286.25 3.04 0.111 2.05 -1 2 1 2448.98 2785.47 3.02 0.345 3.59 6 -3 8 121.00 162.41 3.02 0.083 0.97 4 -1 11 87.38 56.37 2.95 0.049 1.05 4 3 11 179.88 135.16 2.95 0.076 1.17 -2 -2 12 55.01 24.21 2.92 0.032 0.93 5 3 14 41.30 17.74 2.91 0.028 0.93 -4 6 1 18.77 2.75 2.91 0.011 1.10 4 4 1 331.05 274.90 2.88 0.108 1.71 5 -1 2 222.89 270.93 2.84 0.108 1.62 2 -5 6 35.44 20.77 2.82 0.030 1.13 -1 1 7 1354.04 1554.16 2.82 0.258 1.78 7 -3 8 110.51 80.82 2.78 0.059 0.90 6 -8 2 47.64 92.63 2.77 0.063 0.77 -5 4 3 432.75 367.52 2.76 0.125 1.20 8 4 13 64.08 17.20 2.75 0.027 0.84 1 1 1 32.80 10.90 2.74 0.022 6.89 4 -1 15 -2.15 12.99 2.73 0.024 0.81 6 -4 11 37.04 11.35 2.73 0.022 0.80 -8 3 4 94.61 64.78 2.73 0.053 0.90 5 -1 1 78.61 103.37 2.70 0.067 1.63 7 -2 10 21.67 8.78 2.70 0.019 0.88 0 3 0 1536.66 1751.60 2.69 0.274 2.82 Bond lengths and angles N1 - Distance Angles C7 1.3214 (0.0029) C8 1.3901 (0.0027) 108.21 (0.18) C6 1.4710 (0.0027) 126.63 (0.18) 125.15 (0.18) N1 - C7 C8 N2 - Distance Angles C7 1.3291 (0.0028) C13 1.3923 (0.0028) 107.86 (0.18) C14 1.4659 (0.0029) 126.92 (0.19) 125.11 (0.18) N2 - C7 C13 C1 - Distance Angles C2 1.5165 (0.0041) H1A 0.9800 109.47 H1B 0.9800 109.47 109.47 H1C 0.9800 109.47 109.47 109.47 C1 - C2 H1A H1B C2 - Distance Angles C3 1.5084 (0.0037) C1 1.5165 (0.0041) 112.81 (0.25) H2A 0.9900 109.03 109.03 H2B 0.9900 109.03 109.03 107.80 C2 - C3 C1 H2A C3 - Distance Angles C2 1.5084 (0.0037) C4 1.5124 (0.0036) 114.39 (0.22) H3A 0.9900 108.66 108.66 H3B 0.9900 108.66 108.66 107.60 C3 - C2 C4 H3A C4 - Distance Angles C3 1.5124 (0.0036) C5 1.5223 (0.0034) 112.83 (0.21) H4A 0.9900 109.02 109.02 H4B 0.9900 109.02 109.02 107.80 C4 - C3 C5 H4A C5 - Distance Angles C6 1.5121 (0.0035) C4 1.5223 (0.0034) 114.64 (0.20) H5A 0.9900 108.60 108.60 H5B 0.9900 108.60 108.60 107.57 C5 - C6 C4 H5A C6 - Distance Angles N1 1.4710 (0.0027) C5 1.5121 (0.0035) 112.03 (0.19) H6A 0.9900 109.20 109.20 H6B 0.9900 109.20 109.20 107.90 C6 - N1 C5 H6A C7 - Distance Angles N1 1.3214 (0.0029) N2 1.3291 (0.0028) 110.86 (0.19) H7 0.9500 124.57 124.57 C7 - N1 N2 C8 - Distance Angles C9 1.3904 (0.0031) C13 1.3906 (0.0030) 121.68 (0.20) N1 1.3901 (0.0027) 131.78 (0.20) 106.52 (0.19) C8 - C9 C13 C9 - Distance Angles C10 1.3734 (0.0032) C8 1.3904 (0.0031) 116.23 (0.21) H9 0.9500 121.88 121.88 C9 - C10 C8 C10 - Distance Angles C9 1.3734 (0.0032) C11 1.4052 (0.0034) 121.97 (0.21) H10 0.9500 119.01 119.01 C10 - C9 C11 C11 - Distance Angles C12 1.3738 (0.0034) C10 1.4052 (0.0034) 121.77 (0.21) H11 0.9500 119.12 119.12 C11 - C12 C10 C12 - Distance Angles C11 1.3738 (0.0034) C13 1.3854 (0.0031) 116.31 (0.21) H12 0.9500 121.84 121.84 C12 - C11 C13 C13 - Distance Angles C12 1.3854 (0.0031) C8 1.3906 (0.0030) 122.03 (0.21) N2 1.3923 (0.0028) 131.40 (0.21) 106.55 (0.18) C13 - C12 C8 C14 - Distance Angles N2 1.4659 (0.0029) C15 1.5156 (0.0035) 111.73 (0.20) H14A 0.9900 109.27 109.27 H14B 0.9900 109.27 109.27 107.94 C14 - N2 C15 H14A C15 - Distance Angles C14 1.5156 (0.0035) C16 1.5161 (0.0035) 114.59 (0.20) H15A 0.9900 108.62 108.62 H15B 0.9900 108.62 108.62 107.57 C15 - C14 C16 H15A C16 - Distance Angles C15 1.5161 (0.0035) C17 1.5179 (0.0037) 112.57 (0.20) H16A 0.9900 109.08 109.08 H16B 0.9900 109.08 109.08 107.83 C16 - C15 C17 H16A C17 - Distance Angles C18 1.5133 (0.0037) C16 1.5179 (0.0037) 114.66 (0.21) H17A 0.9900 108.60 108.60 H17B 0.9900 108.60 108.60 107.56 C17 - C18 C16 H17A C18 - Distance Angles C19 1.5081 (0.0043) C17 1.5133 (0.0037) 113.02 (0.23) H18A 0.9900 108.98 108.98 H18B 0.9900 108.98 108.98 107.77 C18 - C19 C17 H18A C19 - Distance Angles C18 1.5081 (0.0043) H19A 0.9800 109.47 H19B 0.9800 109.47 109.47 H19C 0.9800 109.47 109.47 109.47 C19 - C18 H19A H19B O1 - Distance Angles H50 0.8992 (0.0182) H51 0.9091 (0.0183) 103.96 (3.02) O1 - H50 FMAP and GRID set by program FMAP 2 3 35 GRID -1.563 -2 -2 1.563 2 2 R1 = 0.0540 for 4615 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.12 at 0.8628 0.8486 0.4819 [ 0.85 A from BR1 ] Deepest hole -0.71 at 0.8019 0.9266 0.3753 [ 0.75 A from BR1 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 3001 / 23155 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1372 0.1514 0.5181 1.00000 0.05 1.12 0.85 BR1 1.51 H51 2.40 O1 2.48 H14B Q2 1 0.1237 0.0985 0.6122 1.00000 0.05 0.32 0.56 BR1 2.06 H50 2.43 H7 2.58 H51 Q3 1 0.0355 0.2147 0.5748 1.00000 0.05 0.32 1.25 BR1 1.82 H7 2.00 H14A 2.26 H51 Q4 1 0.2052 0.1198 0.5792 1.00000 0.05 0.31 0.35 BR1 2.54 H51 2.54 H6A 2.64 H50 Q5 1 0.1755 0.2586 0.5294 1.00000 0.05 0.28 1.19 BR1 2.03 H14B 2.27 H9 2.38 H14A Q6 1 0.6585 0.3742 0.3707 1.00000 0.05 0.28 0.71 C10 0.71 C11 1.49 H10 1.49 H11 Q7 1 0.2253 0.1124 0.6575 1.00000 0.05 0.28 1.28 BR1 2.27 H9 2.31 H6A 2.44 H5A Q8 1 0.1479 0.5185 0.2961 1.00000 0.05 0.26 0.75 C14 0.83 C15 1.34 H15B 1.42 H14B Q9 1 0.4448 0.6943 0.3576 1.00000 0.05 0.25 0.69 N1 0.71 C8 1.70 C7 1.76 C13 Q10 1 0.1459 -0.0269 0.6575 1.00000 0.05 0.25 1.49 BR1 1.60 H50 1.97 H19B 2.11 H11 Shortest distances between peaks (including symmetry equivalents) 2 4 0.79 1 4 1.07 4 7 1.11 2 10 1.11 1 5 1.16 2 3 1.21 1 3 1.21 1 2 1.22 4 5 1.23 2 7 1.25 3 5 1.35 4 10 1.54 3 4 1.56 7 10 1.57 2 5 1.63 5 7 1.92 1 10 2.09 3 7 2.12 1 7 2.12 3 10 2.24 5 10 2.67 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.02: Analyse other restraints etc. 0.88: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.53: Structure factors and derivatives 2.98: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.30: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 14:59:56 Total CPU time: 5.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++