+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2010src0036 started at 13:07:19 on 02-Feb-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2010src0036 in P2(1)/c CELL 0.71073 8.5959 13.7519 15.1599 90.000 92.572 90.000 ZERR 4.00 0.0002 0.0004 0.0005 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O BR RE CL UNIT 68 60 8 12 4 4 4 V = 1790.25 F(000) = 1128.0 Mu = 9.19 mm-1 Cell Wt = 2387.48 Rho = 2.215 MERG 2 OMIT -3.00 55.00 OMIT 0 1 2 OMIT 1 1 1 OMIT -1 1 1 EXTI 0.00109 shel 7 0.77 sadi re1 c21 re1 c31 re1 c41 re1 c51 sadi re1 cl41 re1 cl51 delu 0.005 C41 > cl51 simu 0.005 C41 > cl51 FMAP 2 PLAN 5 SIZE 0.09 0.13 0.26 ACTA BOND $H WGHT 0.02510 8.95380 L.S. 15 TEMP -153.00 FVAR 0.29977 0.73499 RE1 6 0.839000 0.536010 0.188629 11.00000 0.02140 0.01796 = 0.03488 -0.00222 -0.00024 -0.00062 MOLE 1 C1 1 0.591095 0.703372 0.190124 11.00000 0.03404 0.02041 = 0.04222 0.00015 0.01197 0.00343 AFIX 43 H1 2 0.675723 0.741047 0.213749 11.00000 -1.20000 AFIX 0 C2 1 0.446156 0.747303 0.178328 11.00000 0.04784 0.02707 = 0.04463 0.00857 0.01856 0.01424 AFIX 43 H2 2 0.431377 0.813337 0.194345 11.00000 -1.20000 AFIX 0 C3 1 0.323839 0.692525 0.142678 11.00000 0.03541 0.04068 = 0.04320 0.01521 0.00905 0.01701 AFIX 43 H3 2 0.223999 0.721069 0.132512 11.00000 -1.20000 AFIX 0 C4 1 0.347814 0.596473 0.122066 11.00000 0.02476 0.03954 = 0.03691 0.00796 0.00320 0.00607 AFIX 43 H4 2 0.264128 0.558079 0.098330 11.00000 -1.20000 AFIX 0 C5 1 0.494600 0.555761 0.136030 11.00000 0.02725 0.02840 = 0.03009 0.00766 0.00521 0.00608 C6 1 0.531802 0.453740 0.114523 11.00000 0.02453 0.02855 = 0.02319 0.00287 0.00317 0.00054 C7 1 0.422491 0.386549 0.083465 11.00000 0.02075 0.04249 = 0.03746 -0.00426 -0.00031 -0.00617 AFIX 43 H7 2 0.316316 0.405022 0.075370 11.00000 -1.20000 AFIX 0 C8 1 0.467197 0.293274 0.064337 11.00000 0.02602 0.03982 = 0.03928 -0.00576 0.00121 -0.00802 AFIX 43 H8 2 0.391625 0.246877 0.044440 11.00000 -1.20000 AFIX 0 C9 1 0.623311 0.266794 0.074132 11.00000 0.03952 0.02527 = 0.02879 -0.00212 0.00331 -0.00446 C10 1 0.727090 0.337240 0.105733 11.00000 0.02634 0.02404 = 0.02883 -0.00065 -0.00301 -0.00070 AFIX 43 H10 2 0.834030 0.320396 0.113364 11.00000 -1.20000 AFIX 0 C11 1 0.678083 0.166510 0.051630 11.00000 0.04242 0.02640 = 0.03735 0.00078 0.00435 -0.00457 AFIX 23 H11A 2 0.791533 0.168422 0.043035 11.00000 -1.20000 H11B 2 0.625778 0.145741 -0.004762 11.00000 -1.20000 AFIX 0 C12 1 0.645218 0.092096 0.122771 11.00000 0.04033 0.03154 = 0.04606 0.00346 0.00548 -0.00095 AFIX 23 H12A 2 0.534045 0.096719 0.136715 11.00000 -1.20000 H12B 2 0.707894 0.108938 0.177003 11.00000 -1.20000 AFIX 0 C13 1 0.680941 -0.013321 0.097670 11.00000 0.04086 0.02790 = 0.05402 0.00320 -0.00509 -0.00453 AFIX 23 H13A 2 0.662994 -0.056073 0.148762 11.00000 -1.20000 H13B 2 0.608446 -0.033637 0.048510 11.00000 -1.20000 AFIX 0 C14 1 0.842469 -0.026035 0.070810 11.00000 0.03990 0.02226 = 0.05239 0.00308 -0.00211 -0.00112 AFIX 23 H14A 2 0.915202 -0.000118 0.117545 11.00000 -1.20000 H14B 2 0.857775 0.011391 0.016092 11.00000 -1.20000 AFIX 0 N1 3 0.616817 0.609567 0.169484 11.00000 0.02425 0.02210 = 0.03163 0.00205 0.00329 0.00040 N2 3 0.683609 0.428452 0.126149 11.00000 0.02247 0.01930 = 0.02707 0.00111 0.00213 -0.00085 BR1 5 0.889743 -0.163545 0.050278 11.00000 0.04084 0.02938 = 0.06318 -0.00116 -0.00137 -0.00205 MOLE 2 C21 1 1.021997 0.456184 0.202357 11.00000 0.02737 0.02539 = 0.03585 -0.00055 -0.00026 -0.00795 O21 4 1.131577 0.407747 0.209499 11.00000 0.02456 0.03083 = 0.05367 0.00255 0.00032 0.00603 MOLE 3 C31 1 0.950496 0.639669 0.248488 11.00000 0.03046 0.02752 = 0.03923 0.00193 -0.00059 0.00340 O31 4 1.015321 0.701433 0.285760 11.00000 0.04740 0.03036 = 0.06326 -0.01135 -0.01101 -0.00628 MOLE 4 PART 1 C41 1 0.907058 0.584394 0.076966 21.00000 0.01820 0.02125 = 0.03516 -0.00036 0.01011 0.00136 O41 4 0.958030 0.613144 0.014135 21.00000 0.03054 0.03191 = 0.03696 0.00463 0.00324 0.00091 PART 2 CL41 7 0.918479 0.589465 0.045572 -21.00000 0.01869 0.02276 = 0.02059 0.00578 0.01007 -0.00153 MOLE 5 C51 1 0.770096 0.486662 0.300908 -21.00000 0.01751 0.01805 = 0.01537 -0.00161 0.00962 0.00253 O51 4 0.733528 0.468459 0.364662 -21.00000 0.01130 0.01619 = 0.02189 -0.00249 0.01275 -0.00539 PART 1 CL51 7 0.736032 0.478786 0.327596 21.00000 0.02587 0.02562 = 0.02070 0.00450 0.00489 -0.00219 HKLF 4 Covalent radii and connectivity table for 2010src0036 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 BR 1.140 RE 1.370 CL 0.990 Re1 - C21 C31 C41_a C51_b N1 N2 Cl41_b Cl51_a C1 - N1 C2 C2 - C3 C1 C3 - C4 C2 C4 - C3 C5 C5 - N1 C4 C6 C6 - N2 C7 C5 C7 - C8 C6 C8 - C7 C9 C9 - C10 C8 C11 C10 - N2 C9 C11 - C9 C12 C12 - C11 C13 C13 - C14 C12 C14 - C13 Br1 N1 - C1 C5 Re1 N2 - C10 C6 Re1 Br1 - C14 C21 - O21 Re1 O21 - C21 C31 - O31 Re1 O31 - C31 C41_a - O41_a Re1 O41_a - C41_a Cl41_b - Re1 C51_b - O51_b Re1 O51_b - C51_b Cl51_a - Re1 21109 Reflections read, of which 544 rejected -11 =< h =< 9, -17 =< k =< 17, -18 =< l =< 19, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 4090 Unique reflections, of which 0 suppressed R(int) = 0.0449 R(sigma) = 0.0378 Friedel opposites merged Maximum memory for data reduction = 2369 / 40691 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 = 3041 / 319821 wR2 = 0.0774 before cycle 1 for 4090 data and 255 / 255 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 7. 0. 0. 0. 2. 36. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.005 0.010 0.000 0.000 rms deviation 0.000 0.000 0.000 0.021 0.000 0.000 0.000 0.005 0.007 0.000 0.000 GooF = S = 1.073; Restrained GooF = 1.071 for 45 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0251 * P )^2 + 8.95 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29978 0.00050 0.027 OSF 2 0.73480 0.01250 -0.015 FVAR 2 3 0.00109 0.00015 0.002 EXTI Mean shift/esd = 0.005 Maximum = 0.039 for U11 Re1 Max. shift = 0.000 A for O51_b Max. dU = 0.000 for C51_b Least-squares cycle 2 Maximum vector length = 511 Memory required = 3041 / 319821 wR2 = 0.0774 before cycle 2 for 4090 data and 255 / 255 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 7. 0. 0. 0. 2. 36. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.005 0.010 0.000 0.000 rms deviation 0.000 0.000 0.000 0.021 0.000 0.000 0.000 0.005 0.007 0.000 0.000 GooF = S = 1.073; Restrained GooF = 1.071 for 45 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0251 * P )^2 + 8.95 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29979 0.00050 0.015 OSF 2 0.73472 0.01251 -0.006 FVAR 2 3 0.00109 0.00015 0.004 EXTI Mean shift/esd = 0.002 Maximum = 0.015 for U11 Re1 Max. shift = 0.000 A for O51_b Max. dU = 0.000 for Cl41_b Least-squares cycle 3 Maximum vector length = 511 Memory required = 3041 / 319821 wR2 = 0.0774 before cycle 3 for 4090 data and 255 / 255 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 7. 0. 0. 0. 2. 36. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.005 0.010 0.000 0.000 rms deviation 0.000 0.000 0.000 0.021 0.000 0.000 0.000 0.005 0.007 0.000 0.000 GooF = S = 1.074; Restrained GooF = 1.071 for 45 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0251 * P )^2 + 8.95 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29979 0.00050 0.000 OSF 2 0.73471 0.01251 -0.001 FVAR 2 3 0.00109 0.00015 0.001 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for y C51_b Max. shift = 0.000 A for C51_b Max. dU = 0.000 for Cl41_b Least-squares cycle 4 Maximum vector length = 511 Memory required = 3041 / 319821 wR2 = 0.0774 before cycle 4 for 4090 data and 255 / 255 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 7. 0. 0. 0. 2. 36. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.005 0.010 0.000 0.000 rms deviation 0.000 0.000 0.000 0.021 0.000 0.000 0.000 0.005 0.007 0.000 0.000 GooF = S = 1.074; Restrained GooF = 1.071 for 45 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0251 * P )^2 + 8.95 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29979 0.00050 -0.001 OSF 2 0.73471 0.01251 0.000 FVAR 2 3 0.00109 0.00015 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for x Re1 Max. shift = 0.000 A for O51_b Max. dU = 0.000 for O51_b Least-squares cycle 5 Maximum vector length = 511 Memory required = 3041 / 319821 wR2 = 0.0774 before cycle 5 for 4090 data and 255 / 255 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 7. 0. 0. 0. 2. 36. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.005 0.010 0.000 0.000 rms deviation 0.000 0.000 0.000 0.021 0.000 0.000 0.000 0.005 0.007 0.000 0.000 GooF = S = 1.074; Restrained GooF = 1.071 for 45 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0251 * P )^2 + 8.95 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29979 0.00050 0.000 OSF 2 0.73471 0.01251 0.000 FVAR 2 3 0.00109 0.00015 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for x Re1 Max. shift = 0.000 A for C51_b Max. dU = 0.000 for O41_a Least-squares cycle 6 Maximum vector length = 511 Memory required = 3041 / 319821 wR2 = 0.0774 before cycle 6 for 4090 data and 255 / 255 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 7. 0. 0. 0. 2. 36. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.005 0.010 0.000 0.000 rms deviation 0.000 0.000 0.000 0.021 0.000 0.000 0.000 0.005 0.007 0.000 0.000 GooF = S = 1.074; Restrained GooF = 1.071 for 45 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0251 * P )^2 + 8.95 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29979 0.00050 0.000 OSF 2 0.73471 0.01251 0.000 FVAR 2 3 0.00109 0.00015 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for x Re1 Max. shift = 0.000 A for C51_b Max. dU = 0.000 for O51_b Least-squares cycle 7 Maximum vector length = 511 Memory required = 3041 / 319821 wR2 = 0.0774 before cycle 7 for 4090 data and 255 / 255 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 7. 0. 0. 0. 2. 36. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.005 0.010 0.000 0.000 rms deviation 0.000 0.000 0.000 0.021 0.000 0.000 0.000 0.005 0.007 0.000 0.000 GooF = S = 1.074; Restrained GooF = 1.071 for 45 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0251 * P )^2 + 8.95 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29979 0.00050 0.000 OSF 2 0.73471 0.01251 0.000 FVAR 2 3 0.00109 0.00015 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for x Re1 Max. shift = 0.000 A for O51_b Max. dU = 0.000 for C3 Least-squares cycle 8 Maximum vector length = 511 Memory required = 3041 / 319821 wR2 = 0.0774 before cycle 8 for 4090 data and 255 / 255 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 7. 0. 0. 0. 2. 36. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.005 0.010 0.000 0.000 rms deviation 0.000 0.000 0.000 0.021 0.000 0.000 0.000 0.005 0.007 0.000 0.000 GooF = S = 1.074; Restrained GooF = 1.071 for 45 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0251 * P )^2 + 8.95 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29979 0.00050 0.000 OSF 2 0.73471 0.01251 0.000 FVAR 2 3 0.00109 0.00015 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for x Re1 Max. shift = 0.000 A for O51_b Max. dU = 0.000 for Cl41_b Least-squares cycle 9 Maximum vector length = 511 Memory required = 3041 / 319821 wR2 = 0.0774 before cycle 9 for 4090 data and 255 / 255 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 7. 0. 0. 0. 2. 36. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.005 0.010 0.000 0.000 rms deviation 0.000 0.000 0.000 0.021 0.000 0.000 0.000 0.005 0.007 0.000 0.000 GooF = S = 1.074; Restrained GooF = 1.071 for 45 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0251 * P )^2 + 8.95 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29979 0.00050 0.000 OSF 2 0.73471 0.01251 0.000 FVAR 2 3 0.00109 0.00015 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for x Re1 Max. shift = 0.000 A for O51_b Max. dU = 0.000 for O51_b Least-squares cycle 10 Maximum vector length = 511 Memory required = 3041 / 319821 wR2 = 0.0774 before cycle 10 for 4090 data and 255 / 255 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 7. 0. 0. 0. 2. 36. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.005 0.010 0.000 0.000 rms deviation 0.000 0.000 0.000 0.021 0.000 0.000 0.000 0.005 0.007 0.000 0.000 GooF = S = 1.074; Restrained GooF = 1.071 for 45 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0251 * P )^2 + 8.95 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29979 0.00050 0.000 OSF 2 0.73471 0.01251 0.000 FVAR 2 3 0.00109 0.00015 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for x Re1 Max. shift = 0.000 A for O51_b Max. dU = 0.000 for Cl41_b Least-squares cycle 11 Maximum vector length = 511 Memory required = 3041 / 319821 wR2 = 0.0774 before cycle 11 for 4090 data and 255 / 255 parameters Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 7. 0. 0. 0. 2. 36. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.005 0.010 0.000 0.000 rms deviation 0.000 0.000 0.000 0.021 0.000 0.000 0.000 0.005 0.007 0.000 0.000 GooF = S = 1.074; Restrained GooF = 1.071 for 45 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0251 * P )^2 + 8.95 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29979 0.00050 0.000 OSF 2 0.73471 0.01251 0.000 FVAR 2 3 0.00109 0.00015 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for x Re1 Max. shift = 0.000 A for O51_b Max. dU = 0.000 for O41_a Least-squares cycle 12 Maximum vector length = 511 Memory required = 3041 / 319821 wR2 = 0.0774 before cycle 12 for 4090 data and 255 / 255 parameters Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 7. 0. 0. 0. 2. 36. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.005 0.010 0.000 0.000 rms deviation 0.000 0.000 0.000 0.021 0.000 0.000 0.000 0.005 0.007 0.000 0.000 GooF = S = 1.074; Restrained GooF = 1.071 for 45 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0251 * P )^2 + 8.95 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29979 0.00050 0.000 OSF 2 0.73471 0.01251 0.000 FVAR 2 3 0.00109 0.00015 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for x Re1 Max. shift = 0.000 A for C51_b Max. dU = 0.000 for Cl41_b Least-squares cycle 13 Maximum vector length = 511 Memory required = 3041 / 319821 wR2 = 0.0774 before cycle 13 for 4090 data and 255 / 255 parameters Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 7. 0. 0. 0. 2. 36. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.005 0.010 0.000 0.000 rms deviation 0.000 0.000 0.000 0.021 0.000 0.000 0.000 0.005 0.007 0.000 0.000 GooF = S = 1.074; Restrained GooF = 1.071 for 45 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0251 * P )^2 + 8.95 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29979 0.00050 0.001 OSF 2 0.73471 0.01251 0.000 FVAR 2 3 0.00109 0.00015 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for x Re1 Max. shift = 0.000 A for O51_b Max. dU = 0.000 for O41_a Least-squares cycle 14 Maximum vector length = 511 Memory required = 3041 / 319821 wR2 = 0.0774 before cycle 14 for 4090 data and 255 / 255 parameters Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 7. 0. 0. 0. 2. 36. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.005 0.010 0.000 0.000 rms deviation 0.000 0.000 0.000 0.021 0.000 0.000 0.000 0.005 0.007 0.000 0.000 GooF = S = 1.074; Restrained GooF = 1.071 for 45 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0251 * P )^2 + 8.95 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29979 0.00050 0.000 OSF 2 0.73471 0.01251 0.000 FVAR 2 3 0.00109 0.00015 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for x Re1 Max. shift = 0.000 A for O51_b Max. dU = 0.000 for Cl41_b Least-squares cycle 15 Maximum vector length = 511 Memory required = 3041 / 319821 wR2 = 0.0774 before cycle 15 for 4090 data and 255 / 255 parameters Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 7. 0. 0. 0. 2. 36. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.005 0.010 0.000 0.000 rms deviation 0.000 0.000 0.000 0.021 0.000 0.000 0.000 0.005 0.007 0.000 0.000 GooF = S = 1.074; Restrained GooF = 1.071 for 45 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0251 * P )^2 + 8.95 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29979 0.00050 0.000 OSF 2 0.73471 0.01251 0.000 FVAR 2 3 0.00109 0.00015 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for x Re1 Max. shift = 0.000 A for C51_b Max. dU = 0.000 for O51_b Largest correlation matrix elements -0.836 U23 Cl41_b / y C41_a -0.761 U13 Cl51_a / x O51_b 0.679 z O51_b / FVAR 2 -0.833 U13 Cl41_b / x C41_a 0.735 U23 Cl41_b / U23 C41_a 0.655 U13 Cl51_a / U13 O51_b -0.805 U13 C41_a / x C41_a 0.727 U13 Cl41_b / U13 C41_a 0.631 U11 Re1 / OSF 0.801 x Cl41_b / U13 C41_a 0.725 U33 Cl41_b / U33 C41_a 0.631 U33 Cl51_a / U33 O51_b 0.795 y Cl41_b / U23 C41_a 0.711 U33 O51_b / U33 C51_b 0.628 U22 Re1 / OSF -0.790 U23 C41_a / y C41_a 0.694 U33 Cl51_a / FVAR 2 0.628 U13 Cl41_b / x Cl41_b -0.767 x Cl41_b / x C41_a 0.691 U23 Cl51_a / y C51_b 0.628 U23 Cl51_a / U23 O51_b -0.762 y Cl41_b / y C41_a 0.684 EXTI / OSF -0.626 U23 Cl51_a / y O51_b Idealized hydrogen atom generation before cycle 16 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.6757 0.7410 0.2137 43 0.950 0.000 C1 N1 C2 H2 0.4314 0.8133 0.1943 43 0.950 0.000 C2 C3 C1 H3 0.2240 0.7211 0.1325 43 0.950 0.000 C3 C4 C2 H4 0.2641 0.5581 0.0983 43 0.950 0.000 C4 C3 C5 H7 0.3163 0.4050 0.0754 43 0.950 0.000 C7 C8 C6 H8 0.3916 0.2469 0.0444 43 0.950 0.000 C8 C7 C9 H10 0.8340 0.3204 0.1134 43 0.950 0.000 C10 N2 C9 H11A 0.7915 0.1684 0.0430 23 0.990 0.000 C11 C9 C12 H11B 0.6258 0.1457 -0.0048 23 0.990 0.000 C11 C9 C12 H12A 0.5340 0.0967 0.1367 23 0.990 0.000 C12 C11 C13 H12B 0.7079 0.1089 0.1770 23 0.990 0.000 C12 C11 C13 H13A 0.6630 -0.0561 0.1488 23 0.990 0.000 C13 C14 C12 H13B 0.6085 -0.0336 0.0485 23 0.990 0.000 C13 C14 C12 H14A 0.9152 -0.0001 0.1176 23 0.990 0.000 C14 C13 Br1 H14B 0.8578 0.0114 0.0161 23 0.990 0.000 C14 C13 Br1 2010src0036 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Re1 0.83900 0.53601 0.18863 1.00000 0.02141 0.01796 0.03489 -0.00222 -0.00024 -0.00062 0.02480 0.00036 0.00002 0.00001 0.00002 0.00000 0.00013 0.00013 0.00016 0.00009 0.00008 0.00008 0.00010 C1 0.59110 0.70337 0.19012 1.00000 0.03404 0.02040 0.04225 0.00014 0.01200 0.00344 0.03192 0.01108 0.00068 0.00039 0.00041 0.00000 0.00309 0.00266 0.00363 0.00240 0.00258 0.00225 0.00130 H1 0.67573 0.74104 0.21375 1.00000 0.03831 0.00000 0.00000 C2 0.44616 0.74731 0.17833 1.00000 0.04786 0.02709 0.04468 0.00857 0.01856 0.01424 0.03938 0.01277 0.00075 0.00044 0.00043 0.00000 0.00376 0.00299 0.00386 0.00271 0.00300 0.00274 0.00152 H2 0.43138 0.81334 0.19435 1.00000 0.04726 0.00000 0.00000 C3 0.32383 0.69253 0.14267 1.00000 0.03545 0.04070 0.04323 0.01521 0.00904 0.01702 0.03957 0.01292 0.00074 0.00047 0.00044 0.00000 0.00329 0.00353 0.00392 0.00293 0.00275 0.00280 0.00152 H3 0.22399 0.72107 0.13251 1.00000 0.04749 0.00000 0.00000 C4 0.34781 0.59647 0.12206 1.00000 0.02477 0.03956 0.03694 0.00796 0.00320 0.00608 0.03370 0.01145 0.00065 0.00046 0.00040 0.00000 0.00279 0.00332 0.00347 0.00271 0.00237 0.00245 0.00132 H4 0.26413 0.55807 0.09833 1.00000 0.04044 0.00000 0.00000 C5 0.49461 0.55576 0.13603 1.00000 0.02728 0.02839 0.03012 0.00765 0.00521 0.00609 0.02848 0.01065 0.00064 0.00041 0.00039 0.00000 0.00284 0.00283 0.00316 0.00230 0.00229 0.00221 0.00121 C6 0.53180 0.45374 0.11452 1.00000 0.02456 0.02855 0.02321 0.00288 0.00319 0.00055 0.02538 0.00967 0.00062 0.00039 0.00036 0.00000 0.00266 0.00279 0.00287 0.00220 0.00209 0.00213 0.00112 C7 0.42249 0.38655 0.08346 1.00000 0.02077 0.04250 0.03747 -0.00427 -0.00030 -0.00617 0.03363 0.00996 0.00064 0.00046 0.00040 0.00000 0.00264 0.00344 0.00347 0.00272 0.00230 0.00246 0.00132 H7 0.31632 0.40502 0.07537 1.00000 0.04035 0.00000 0.00000 C8 0.46719 0.29327 0.06434 1.00000 0.02601 0.03982 0.03935 -0.00576 0.00120 -0.00800 0.03507 0.01031 0.00066 0.00046 0.00041 0.00000 0.00292 0.00342 0.00371 0.00272 0.00250 0.00247 0.00138 H8 0.39161 0.24688 0.04444 1.00000 0.04208 0.00000 0.00000 C9 0.62332 0.26679 0.07414 1.00000 0.03954 0.02528 0.02882 -0.00212 0.00332 -0.00446 0.03116 0.00990 0.00069 0.00041 0.00038 0.00000 0.00321 0.00277 0.00321 0.00233 0.00243 0.00239 0.00125 C10 0.72709 0.33724 0.10574 1.00000 0.02635 0.02406 0.02884 -0.00066 -0.00303 -0.00070 0.02654 0.00930 0.00064 0.00038 0.00037 0.00000 0.00271 0.00268 0.00307 0.00220 0.00221 0.00213 0.00116 H10 0.83403 0.32040 0.11337 1.00000 0.03185 0.00000 0.00000 C11 0.67808 0.16651 0.05163 1.00000 0.04243 0.02641 0.03736 0.00077 0.00435 -0.00455 0.03532 0.01101 0.00074 0.00041 0.00042 0.00000 0.00345 0.00297 0.00359 0.00250 0.00271 0.00254 0.00136 H11A 0.79153 0.16841 0.04303 1.00000 0.04239 0.00000 0.00000 H11B 0.62577 0.14574 -0.00476 1.00000 0.04239 0.00000 0.00000 C12 0.64522 0.09210 0.12277 1.00000 0.04036 0.03151 0.04609 0.00346 0.00548 -0.00094 0.03921 0.01169 0.00075 0.00044 0.00045 0.00000 0.00345 0.00320 0.00398 0.00282 0.00283 0.00271 0.00145 H12A 0.53404 0.09672 0.13671 1.00000 0.04705 0.00000 0.00000 H12B 0.70789 0.10894 0.17700 1.00000 0.04705 0.00000 0.00000 C13 0.68095 -0.01332 0.09767 1.00000 0.04089 0.02787 0.05405 0.00318 -0.00508 -0.00453 0.04116 0.01153 0.00076 0.00044 0.00049 0.00000 0.00359 0.00313 0.00439 0.00286 0.00299 0.00263 0.00154 H13A 0.66300 -0.05607 0.14877 1.00000 0.04939 0.00000 0.00000 H13B 0.60846 -0.03364 0.04851 1.00000 0.04939 0.00000 0.00000 C14 0.84246 -0.02603 0.07082 1.00000 0.03989 0.02224 0.05245 0.00308 -0.00212 -0.00111 0.03832 0.01139 0.00074 0.00041 0.00048 0.00000 0.00344 0.00284 0.00418 0.00266 0.00291 0.00246 0.00146 H14A 0.91519 -0.00012 0.11755 1.00000 0.04598 0.00000 0.00000 H14B 0.85777 0.01140 0.01610 1.00000 0.04598 0.00000 0.00000 N1 0.61681 0.60956 0.16948 1.00000 0.02425 0.02211 0.03166 0.00207 0.00328 0.00039 0.02595 0.00793 0.00050 0.00032 0.00031 0.00000 0.00222 0.00220 0.00264 0.00191 0.00184 0.00179 0.00096 N2 0.68361 0.42845 0.12615 1.00000 0.02249 0.01930 0.02709 0.00109 0.00213 -0.00085 0.02293 0.00763 0.00049 0.00031 0.00030 0.00000 0.00220 0.00210 0.00250 0.00178 0.00177 0.00169 0.00092 Br1 0.88974 -0.16355 0.05028 1.00000 0.04084 0.02938 0.06317 -0.00115 -0.00137 -0.00205 0.04458 0.00117 0.00008 0.00005 0.00005 0.00000 0.00036 0.00032 0.00047 0.00029 0.00031 0.00026 0.00018 C21 1.02200 0.45618 0.20236 1.00000 0.02738 0.02540 0.03588 -0.00055 -0.00026 -0.00794 0.02960 0.00965 0.00064 0.00039 0.00040 0.00000 0.00290 0.00279 0.00339 0.00236 0.00235 0.00233 0.00124 O21 1.13158 0.40775 0.20950 1.00000 0.02456 0.03084 0.05369 0.00254 0.00031 0.00603 0.03641 0.00739 0.00044 0.00029 0.00030 0.00000 0.00203 0.00215 0.00282 0.00196 0.00180 0.00176 0.00097 C31 0.95049 0.63967 0.24849 1.00000 0.03049 0.02752 0.03923 0.00193 -0.00058 0.00339 0.03248 0.01014 0.00065 0.00041 0.00041 0.00000 0.00301 0.00293 0.00356 0.00254 0.00256 0.00237 0.00130 O31 1.01533 0.70143 0.28577 1.00000 0.04741 0.03037 0.06328 -0.01133 -0.01103 -0.00628 0.04742 0.00752 0.00054 0.00031 0.00034 0.00000 0.00268 0.00230 0.00326 0.00220 0.00228 0.00204 0.00117 C41_a 0.90707 0.58440 0.07697 0.73471 0.01821 0.02128 0.03520 -0.00037 0.01011 0.00135 0.02463 0.03079 0.00211 0.00129 0.00085 0.01251 0.00390 0.00396 0.00706 0.00576 0.00575 0.00297 0.00260 O41_a 0.95804 0.61315 0.01412 0.73471 0.03057 0.03191 0.03700 0.00464 0.00325 0.00089 0.03311 0.01302 0.00097 0.00060 0.00062 0.01251 0.00380 0.00370 0.00477 0.00314 0.00314 0.00281 0.00165 Cl41_b 0.91848 0.58947 0.04557 0.26529 0.01873 0.02279 0.02067 0.00575 0.01003 -0.00151 0.02046 0.01845 0.00123 0.00079 0.00050 0.01251 0.00370 0.00337 0.00599 0.00414 0.00421 0.00236 0.00233 C51_b 0.77009 0.48666 0.30090 0.26529 0.01758 0.01812 0.01544 -0.00161 0.00961 0.00254 0.01678 0.05741 0.00338 0.00229 0.00138 0.01251 0.00680 0.00659 0.00802 0.00668 0.00621 0.00611 0.00382 O51_b 0.73353 0.46847 0.36463 0.26529 0.01135 0.01622 0.02197 -0.00252 0.01275 -0.00541 0.01615 0.03834 0.00226 0.00154 0.00162 0.01251 0.00496 0.00570 0.00766 0.00660 0.00634 0.00443 0.00321 Cl51_a 0.73603 0.47879 0.32759 0.73471 0.02588 0.02563 0.02069 0.00450 0.00489 -0.00218 0.02395 0.00477 0.00031 0.00018 0.00019 0.01251 0.00133 0.00118 0.00254 0.00150 0.00139 0.00095 0.00101 Final Structure Factor Calculation for 2010src0036 in P2(1)/c Total number of l.s. parameters = 255 Maximum vector length = 511 Memory required = 2786 / 26061 wR2 = 0.0774 before cycle 16 for 4090 data and 0 / 255 parameters Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 7. 0. 0. 0. 2. 36. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.005 0.010 0.000 0.000 rms deviation 0.000 0.000 0.000 0.021 0.000 0.000 0.000 0.005 0.007 0.000 0.000 GooF = S = 1.074; Restrained GooF = 1.071 for 45 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0251 * P )^2 + 8.95 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0334 for 3471 Fo > 4sig(Fo) and 0.0441 for all 4090 data wR2 = 0.0774, GooF = S = 1.074, Restrained GooF = 1.071 for all data Occupancy sum of asymmetric unit = 25.00 for non-hydrogen and 15.00 for hydrogen atoms Principal mean square atomic displacements U 0.0354 0.0215 0.0175 Re1 0.0489 0.0276 0.0192 C1 0.0683 0.0300 0.0198 C2 0.0661 0.0327 0.0199 C3 0.0476 0.0310 0.0226 C4 0.0404 0.0244 0.0207 C5 0.0301 0.0251 0.0210 C6 0.0457 0.0363 0.0189 C7 0.0468 0.0363 0.0220 C8 0.0411 0.0287 0.0236 C9 0.0322 0.0247 0.0227 C10 0.0443 0.0367 0.0250 C11 0.0481 0.0392 0.0304 C12 0.0584 0.0387 0.0264 C13 0.0543 0.0388 0.0219 C14 0.0325 0.0237 0.0217 N1 0.0274 0.0226 0.0188 N2 0.0640 0.0408 0.0289 Br1 0.0366 0.0339 0.0183 C21 0.0540 0.0344 0.0208 O21 0.0399 0.0327 0.0249 C31 0.0728 0.0467 0.0228 O31 0.0386 0.0215 0.0137 C41_a 0.0401 0.0302 0.0291 O41_a 0.0302 0.0230 0.0082 Cl41_b 0.0252 0.0188 0.0064 C51_b 0.0310 0.0153 0.0022 O51_b 0.0283 0.0277 0.0158 Cl51_a Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.023 0.044 0.068 0.095 0.123 0.154 0.191 0.243 0.326 1.000 Number in group 427. 398. 412. 406. 412. 402. 407. 409. 406. 411. GooF 1.048 0.963 1.153 1.092 1.121 1.173 1.041 0.934 1.019 1.158 K 2.365 1.029 1.038 0.963 0.964 0.973 0.995 1.008 1.017 1.008 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.65 inf Number in group 416. 413. 402. 405. 415. 413. 404. 401. 411. 410. GooF 1.044 0.982 0.987 1.007 0.916 1.026 0.907 0.840 1.001 1.745 K 0.990 0.992 1.005 1.012 1.013 1.016 1.024 1.021 1.012 0.992 R1 0.114 0.084 0.076 0.062 0.045 0.037 0.029 0.024 0.021 0.028 Recommended weighting scheme: WGHT 0.0252 8.9246 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)/esd Fc/Fc(max) Resolution(A) -1 10 10 946.67 2117.37 7.81 0.134 1.01 2 3 3 1203.42 566.72 6.48 0.069 2.62 -8 10 3 1628.95 2944.89 6.12 0.158 0.84 -1 2 1 736.19 310.44 5.70 0.051 5.10 -2 2 1 1906.10 2908.87 5.70 0.157 3.57 0 2 1 7314.45 12469.83 5.32 0.325 6.26 0 3 1 8923.28 11211.40 5.13 0.308 4.39 0 1 4 2953.41 2043.65 5.07 0.132 3.65 3 2 1 1062.62 601.09 4.72 0.071 2.59 4 2 3 2002.27 1383.73 4.38 0.108 1.87 3 5 2 3388.20 2641.00 3.77 0.150 1.90 -1 3 1 7342.76 6080.75 3.76 0.227 3.93 1 2 7 634.56 339.98 3.73 0.054 1.99 0 0 4 6989.67 5611.15 3.65 0.218 3.79 3 2 3 14609.71 16847.65 3.55 0.378 2.30 -3 5 1 801.36 505.45 3.51 0.065 1.97 1 6 2 3781.75 4634.02 3.51 0.198 2.12 -3 3 3 6672.46 5622.41 3.43 0.218 2.22 0 4 1 14944.57 17097.21 3.40 0.381 3.35 3 1 2 14433.13 16456.72 3.38 0.374 2.59 -2 6 4 800.51 492.38 3.37 0.065 1.80 -3 0 4 3047.40 3819.67 3.37 0.180 2.33 0 7 3 229.24 82.95 3.35 0.027 1.83 2 2 1 671.90 1005.52 3.32 0.092 3.51 1 0 2 31265.36 36701.52 3.32 0.558 5.56 -3 2 1 1464.92 1939.71 3.24 0.128 2.62 -1 5 4 12440.31 14204.04 3.21 0.347 2.17 0 2 7 3479.43 2819.87 3.19 0.155 2.06 2 8 4 443.43 238.58 3.18 0.045 1.46 9 5 8 -205.28 264.50 3.17 0.047 0.80 -3 8 2 111.80 8.14 3.14 0.008 1.45 -5 1 2 636.21 403.12 3.09 0.058 1.68 5 5 16 1367.54 2076.63 3.09 0.133 0.78 0 6 0 9900.15 11684.88 3.08 0.315 2.29 -10 1 9 679.58 1192.48 3.01 0.101 0.78 -2 1 3 15575.39 17560.99 2.98 0.386 3.25 10 7 0 678.49 1181.24 2.98 0.100 0.79 -1 2 5 18610.23 16539.95 2.97 0.375 2.67 2 7 12 1259.27 1742.14 2.92 0.122 1.02 -10 5 4 1260.38 1899.10 2.89 0.127 0.81 -2 1 2 2189.72 2695.81 2.89 0.151 3.67 -4 1 4 508.46 307.76 2.87 0.051 1.89 9 10 1 2419.40 3297.83 2.85 0.167 0.78 -7 12 4 776.68 1148.20 2.85 0.099 0.82 2 2 16 -15.38 295.31 2.84 0.050 0.91 -2 4 3 514.81 324.94 2.84 0.053 2.40 -1 5 2 11036.71 12446.53 2.81 0.325 2.49 -1 6 6 5585.67 6457.33 2.80 0.234 1.67 -1 2 3 29958.89 33193.31 2.80 0.531 3.73 2 13 6 170.55 13.10 2.79 0.011 0.95 Bond lengths and angles Re1 - Distance Angles C21 1.9219 (0.0056) C31 1.9225 (0.0058) 89.09 (0.23) C41_a 1.9337 (0.0112) 90.74 (0.60) 89.66 (0.56) C51_b 1.9491 (0.0150) 89.19 (0.91) 90.60 (1.00) 179.73 (1.14) N1 2.1692 (0.0043) 172.90 (0.19) 97.74 (0.20) 91.24 (0.58) 88.80 (0.90) N2 2.1808 (0.0043) 98.16 (0.20) 172.14 (0.20) 93.25 (0.54) 86.50 (0.98) 74.91 (0.16) Cl41_b 2.4174 (0.0077) 90.46 (0.31) 92.47 (0.32) 2.83 (0.73) 176.90 (1.01) 91.19 (0.28) 90.51 (0.28) Cl51_a 2.4511 (0.0028) 92.80 (0.19) 91.37 (0.19) 176.32 (0.57) 3.68 (0.91) 85.12 (0.13) 85.28 (0.13) 175.00 (0.26) Re1 - C21 C31 C41_a C51_b N1 N2 Cl41_b C1 - Distance Angles N1 1.3481 (0.0069) C2 1.3890 (0.0082) 122.81 (0.58) H1 0.9500 118.59 118.59 C1 - N1 C2 C2 - Distance Angles C3 1.3836 (0.0097) C1 1.3890 (0.0082) 118.36 (0.56) H2 0.9500 120.82 120.82 C2 - C3 C1 C3 - Distance Angles C4 1.3751 (0.0089) C2 1.3836 (0.0097) 119.52 (0.55) H3 0.9500 120.24 120.24 C3 - C4 C2 C4 - Distance Angles C3 1.3751 (0.0089) C5 1.3879 (0.0076) 119.82 (0.60) H4 0.9500 120.09 120.09 C4 - C3 C5 C5 - Distance Angles N1 1.3639 (0.0073) C4 1.3879 (0.0076) 121.18 (0.53) C6 1.4786 (0.0075) 115.22 (0.46) 123.59 (0.55) C5 - N1 C4 C6 - Distance Angles N2 1.3543 (0.0068) C7 1.3852 (0.0077) 120.52 (0.50) C5 1.4786 (0.0075) 115.57 (0.47) 123.90 (0.50) C6 - N2 C7 C7 - Distance Angles C8 1.3737 (0.0087) C6 1.3852 (0.0077) 120.18 (0.52) H7 0.9500 119.91 119.91 C7 - C8 C6 C8 - Distance Angles C7 1.3737 (0.0087) C9 1.3921 (0.0084) 119.95 (0.53) H8 0.9500 120.03 120.03 C8 - C7 C9 C9 - Distance Angles C10 1.3875 (0.0075) C8 1.3921 (0.0083) 117.12 (0.53) C11 1.5014 (0.0081) 121.10 (0.54) 121.78 (0.53) C9 - C10 C8 C10 - Distance Angles N2 1.3488 (0.0067) C9 1.3875 (0.0075) 123.23 (0.51) H10 0.9500 118.38 118.38 C10 - N2 C9 C11 - Distance Angles C9 1.5014 (0.0081) C12 1.5223 (0.0084) 112.73 (0.51) H11A 0.9900 109.04 109.04 H11B 0.9900 109.04 109.04 107.81 C11 - C9 C12 H11A C12 - Distance Angles C11 1.5223 (0.0084) C13 1.5334 (0.0087) 114.47 (0.54) H12A 0.9900 108.64 108.64 H12B 0.9900 108.64 108.64 107.59 C12 - C11 C13 H12A C13 - Distance Angles C14 1.4746 (0.0091) C12 1.5334 (0.0087) 112.47 (0.51) H13A 0.9900 109.11 109.11 H13B 0.9900 109.11 109.11 107.85 C13 - C14 C12 H13A C14 - Distance Angles C13 1.4746 (0.0091) Br1 1.9621 (0.0057) 111.25 (0.41) H14A 0.9900 109.38 109.38 H14B 0.9900 109.38 109.38 108.00 C14 - C13 Br1 H14A N1 - Distance Angles C1 1.3481 (0.0069) C5 1.3639 (0.0073) 118.28 (0.47) Re1 2.1692 (0.0043) 124.59 (0.38) 117.11 (0.35) N1 - C1 C5 N2 - Distance Angles C10 1.3488 (0.0067) C6 1.3543 (0.0068) 118.97 (0.46) Re1 2.1808 (0.0043) 124.04 (0.35) 116.75 (0.34) N2 - C10 C6 Br1 - Distance Angles C14 1.9621 (0.0057) Br1 - C21 - Distance Angles O21 1.1547 (0.0065) Re1 1.9219 (0.0056) 179.10 (0.55) C21 - O21 O21 - Distance Angles C21 1.1547 (0.0065) O21 - C31 - Distance Angles O31 1.1502 (0.0068) Re1 1.9225 (0.0057) 178.60 (0.58) C31 - O31 O31 - Distance Angles C31 1.1502 (0.0068) O31 - C41_a - Distance Angles O41_a 1.1374 (0.0167) Re1 1.9337 (0.0112) 174.88 (1.65) C41_a - O41_a O41_a - Distance Angles C41_a 1.1374 (0.0167) O41_a - Cl41_b - Distance Angles Re1 2.4174 (0.0076) Cl41_b - C51_b - Distance Angles O51_b 1.0593 (0.0284) Re1 1.9491 (0.0150) 173.19 (3.48) C51_b - O51_b O51_b - Distance Angles C51_b 1.0593 (0.0284) O51_b - Cl51_a - Distance Angles Re1 2.4511 (0.0028) Cl51_a - FMAP and GRID set by program FMAP 2 3 19 GRID -1.563 -2 -2 1.563 2 2 R1 = 0.0429 for 4090 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.22 at 0.8418 0.3979 0.1881 [ 1.56 A from H10 ] Deepest hole -1.40 at 0.8598 0.8376 0.0834 [ 0.57 A from BR1 ] Mean = 0.00, Rms deviation from mean = 0.16 e/A^3, Highest memory used = 2797 / 20450 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.8418 0.3979 0.1881 1.00000 0.05 1.22 1.56 H10 1.67 N2 1.75 C21 1.77 C10 Q2 1 0.5184 0.0352 0.0656 1.00000 0.05 1.14 1.26 H13B 1.37 H12A 1.57 C12 1.60 C13 Q3 1 0.8961 0.0949 0.0510 1.00000 0.05 0.98 1.30 H14B 1.35 H11A 1.65 H14A 1.75 C14 Q4 1 1.2166 0.3364 0.1683 1.00000 0.05 0.89 1.39 O21 1.93 H7 2.34 C7 2.37 H1 Q5 1 0.8882 0.2371 0.0478 1.00000 0.05 0.89 1.26 H11A 1.60 H10 2.05 C11 2.17 C10 Shortest distances between peaks (including symmetry equivalents) 3 5 1.96 2 2 2.22 Time profile in seconds ----------------------- 0.13: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.02: 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 0.03: Analyse other restraints etc. 6.29: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.06: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.02: Generate idealized H-atoms 3.53: Structure factors and derivatives 6.50: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.17: Apply other restraints 1.92: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.17: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2010src0036 finished at 13:08:05 Total CPU time: 19.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++