+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2005src1385 started at 15:56:20 on 10-Nov-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2005src1385 in P-1 CELL 0.71073 10.6212 11.6023 16.3071 69.778 81.378 73.082 ZERR 2.00 0.0003 0.0003 0.0004 0.001 0.001 0.001 LATT 1 SFAC C H FE BR CL PD P UNIT 70 54 2 4 10 2 4 V = 1801.33 F(000) = 988.0 Mu = 3.61 mm-1 Cell Wt = 2017.65 Rho = 1.860 MERG 2 OMIT -3.00 55.00 OMIT 1 0 2 OMIT 1 1 2 shel 7 0.77 DELU C41 > CL53 SIMU C41 > CL53 FMAP 2 PLAN 5 ACTA SIZE 0.24 0.20 0.08 BOND $H WGHT 0.03570 4.64570 L.S. 20 TEMP -153.00 FVAR 0.41701 0.68377 MOLE 1 C1 1 0.347373 0.083371 0.173975 11.00000 0.02179 0.02718 = 0.03197 -0.01015 -0.00324 -0.01171 C2 1 0.438595 0.082701 0.231293 11.00000 0.03163 0.03928 = 0.03792 -0.01780 0.00081 -0.01701 C3 1 0.566820 0.068035 0.189436 11.00000 0.02293 0.04802 = 0.05692 -0.02021 0.00177 -0.02004 AFIX 43 H3 2 0.644971 0.064277 0.213060 11.00000 -1.20000 AFIX 0 C4 1 0.556940 0.060078 0.106486 11.00000 0.02953 0.04767 = 0.04947 -0.01961 0.01070 -0.01976 AFIX 43 H4 2 0.628085 0.049815 0.064516 11.00000 -1.20000 AFIX 0 C5 1 0.424647 0.069773 0.095691 11.00000 0.02749 0.03873 = 0.04011 -0.01641 0.00642 -0.01443 AFIX 43 H5 2 0.391882 0.067694 0.045257 11.00000 -1.20000 AFIX 0 C6 1 0.410002 -0.216734 0.288486 11.00000 0.02300 0.02793 = 0.03803 -0.01193 0.00020 -0.00557 C7 1 0.444342 -0.236865 0.205277 11.00000 0.02789 0.03388 = 0.03903 -0.01720 0.00393 -0.00924 C8 1 0.582926 -0.252959 0.186726 11.00000 0.02919 0.04449 = 0.05056 -0.02219 0.01065 -0.00524 AFIX 43 H8 2 0.630935 -0.267385 0.135598 11.00000 -1.20000 AFIX 0 C9 1 0.635683 -0.243664 0.257565 11.00000 0.02086 0.04606 = 0.05921 -0.01558 -0.00274 -0.00232 AFIX 43 H9 2 0.725753 -0.250317 0.262355 11.00000 -1.20000 AFIX 0 C10 1 0.531259 -0.222561 0.321066 11.00000 0.02511 0.03817 = 0.04546 -0.01326 -0.00792 -0.00507 AFIX 43 H10 2 0.540175 -0.213834 0.375579 11.00000 -1.20000 AFIX 0 C11 1 0.123500 0.161648 0.074633 11.00000 0.02148 0.02984 = 0.02387 -0.01019 0.00134 -0.01133 C12 1 0.131649 0.076589 0.030523 11.00000 0.03811 0.03034 = 0.03637 -0.01610 -0.00521 -0.00740 AFIX 43 H12 2 0.162347 -0.011968 0.059799 11.00000 -1.20000 AFIX 0 C13 1 0.096357 0.117359 -0.054576 11.00000 0.03256 0.04491 = 0.03259 -0.02305 -0.00070 -0.01035 AFIX 43 H13 2 0.104846 0.057182 -0.083769 11.00000 -1.20000 AFIX 0 C14 1 0.049332 0.243508 -0.097163 11.00000 0.04609 0.05270 = 0.02557 -0.01423 -0.00803 -0.01260 AFIX 43 H14 2 0.024360 0.271968 -0.155870 11.00000 -1.20000 AFIX 0 C15 1 0.038372 0.329903 -0.053695 11.00000 0.10494 0.03344 = 0.03839 -0.00903 -0.03094 -0.00084 AFIX 43 H15 2 0.004386 0.418084 -0.082706 11.00000 -1.20000 AFIX 0 C16 1 0.076327 0.289446 0.031584 11.00000 0.07223 0.03359 = 0.03206 -0.01273 -0.01474 -0.00917 AFIX 43 H16 2 0.069789 0.349821 0.060256 11.00000 -1.20000 AFIX 0 C17 1 0.115563 0.240639 0.227173 11.00000 0.02883 0.02454 = 0.02378 -0.01036 -0.00498 -0.00830 C18 1 0.185540 0.333678 0.198801 11.00000 0.03392 0.02790 = 0.03093 -0.00874 -0.00841 -0.01243 AFIX 43 H18 2 0.260585 0.324886 0.159427 11.00000 -1.20000 AFIX 0 C19 1 0.146566 0.438422 0.227502 11.00000 0.05273 0.02450 = 0.04283 -0.00890 -0.01836 -0.01389 AFIX 43 H19 2 0.195233 0.500855 0.208225 11.00000 -1.20000 AFIX 0 C20 1 0.037505 0.452371 0.283891 11.00000 0.07009 0.03010 = 0.03509 -0.01768 -0.00989 -0.00689 AFIX 43 H20 2 0.011321 0.523988 0.304036 11.00000 -1.20000 AFIX 0 C21 1 -0.034157 0.362158 0.311326 11.00000 0.06634 0.03542 = 0.03496 -0.02048 0.01187 -0.01272 AFIX 43 H21 2 -0.110232 0.372566 0.349678 11.00000 -1.20000 AFIX 0 C22 1 0.004753 0.256277 0.282971 11.00000 0.04298 0.02825 = 0.02904 -0.01245 0.00038 -0.01059 AFIX 43 H22 2 -0.044812 0.194589 0.301933 11.00000 -1.20000 AFIX 0 C23 1 0.245348 -0.367853 0.394644 11.00000 0.02085 0.02692 = 0.02460 -0.00526 -0.00533 -0.00654 C24 1 0.327566 -0.463460 0.363823 11.00000 0.02800 0.03282 = 0.03378 -0.01418 -0.00324 -0.00537 AFIX 43 H24 2 0.385758 -0.442709 0.313923 11.00000 -1.20000 AFIX 0 C25 1 0.324637 -0.588751 0.405800 11.00000 0.03621 0.02798 = 0.05638 -0.01714 -0.00994 -0.00412 AFIX 43 H25 2 0.379371 -0.653133 0.383348 11.00000 -1.20000 AFIX 0 C26 1 0.243665 -0.621637 0.479600 11.00000 0.04478 0.02924 = 0.03959 -0.00174 -0.01389 -0.01422 AFIX 43 H26 2 0.243771 -0.708170 0.508506 11.00000 -1.20000 AFIX 0 C27 1 0.162704 -0.528124 0.511046 11.00000 0.04287 0.04030 = 0.02845 -0.00418 -0.00164 -0.01587 AFIX 43 H27 2 0.107458 -0.550242 0.562368 11.00000 -1.20000 AFIX 0 C28 1 0.161266 -0.401593 0.468208 11.00000 0.03363 0.03159 = 0.03318 -0.00980 -0.00181 -0.00954 AFIX 43 H28 2 0.102531 -0.337354 0.489134 11.00000 -1.20000 AFIX 0 C29 1 0.252467 -0.152851 0.437972 11.00000 0.02194 0.03654 = 0.02814 -0.01367 0.00005 -0.01238 C30 1 0.167301 -0.039626 0.444348 11.00000 0.03026 0.04041 = 0.02875 -0.01568 -0.00260 -0.01209 AFIX 43 H30 2 0.107782 0.011341 0.399685 11.00000 -1.20000 AFIX 0 C31 1 0.168538 -0.000306 0.515707 11.00000 0.03036 0.05383 = 0.04359 -0.03215 0.00350 -0.01590 AFIX 43 H31 2 0.111460 0.078117 0.519134 11.00000 -1.20000 AFIX 0 C32 1 0.253044 -0.075759 0.581433 11.00000 0.03194 0.07753 = 0.03777 -0.03277 0.00494 -0.02530 AFIX 43 H32 2 0.255145 -0.048758 0.629855 11.00000 -1.20000 AFIX 0 C33 1 0.334426 -0.190311 0.576857 11.00000 0.03527 0.07232 = 0.03272 -0.01787 -0.00984 -0.01781 AFIX 43 H33 2 0.390653 -0.242942 0.623094 11.00000 -1.20000 AFIX 0 C34 1 0.335151 -0.229508 0.505687 11.00000 0.02719 0.04775 = 0.03580 -0.01439 -0.00902 -0.00829 AFIX 43 H34 2 0.391874 -0.308465 0.503024 11.00000 -1.20000 AFIX 0 FE1 3 0.490611 -0.081382 0.204500 11.00000 0.01805 0.03719 = 0.03828 -0.01610 0.00331 -0.01033 BR1 4 0.403748 0.103203 0.342234 11.00000 0.03446 0.04663 = 0.04112 -0.02110 -0.00416 -0.01699 BR2 4 0.328992 -0.255089 0.136136 11.00000 0.04368 0.03856 = 0.03643 -0.01733 -0.00384 -0.01152 CL1 5 -0.114610 0.082201 0.195893 11.00000 0.01758 0.02993 = 0.03154 -0.01103 -0.00465 -0.00552 CL2 5 -0.048515 -0.209753 0.326502 11.00000 0.02469 0.02939 = 0.03337 -0.00659 -0.00268 -0.01445 PD1 6 0.075570 -0.061476 0.262830 11.00000 0.01564 0.02256 = 0.02176 -0.01011 -0.00103 -0.00739 P1 7 0.169602 0.103158 0.188316 11.00000 0.01936 0.02506 = 0.02476 -0.01117 -0.00076 -0.00944 P2 7 0.247461 -0.200929 0.343345 11.00000 0.01797 0.02516 = 0.02636 -0.01027 -0.00274 -0.00609 MOLE 2 PART 1 C41 1 0.683086 -0.618947 0.121674 21.00000 0.09701 0.02974 = 0.05329 -0.01762 -0.01384 0.00735 AFIX 13 H41 2 0.748997 -0.696672 0.154400 21.00000 -1.20000 AFIX 0 CL41 5 0.547516 -0.597732 0.189568 21.00000 0.16675 0.05442 = 0.04380 -0.00602 0.03108 0.00262 CL42 5 0.650170 -0.644320 0.029553 21.00000 0.11869 0.08969 = 0.04903 -0.03106 -0.00465 -0.02167 CL43 5 0.757031 -0.491011 0.088762 21.00000 0.10361 0.05892 = 0.14042 -0.05572 0.02091 -0.01842 PART 2 same c41 > cl43 C51 1 0.676170 -0.616500 0.123984 -21.00000 0.04395 0.04372 = 0.09964 0.02256 -0.00472 -0.02175 AFIX 13 H51 2 0.728836 -0.704488 0.126816 -21.00000 -1.20000 AFIX 0 CL51 5 0.676859 -0.515355 0.020611 -21.00000 0.12846 0.21012 = 0.09183 0.04831 0.02526 -0.03402 CL52 5 0.742321 -0.556234 0.185506 -21.00000 0.13373 0.08851 = 0.20120 -0.03122 -0.06282 -0.03138 CL53 5 0.521230 -0.617089 0.176729 -21.00000 0.04959 0.06067 = 0.15735 0.00671 0.02390 -0.01546 HKLF 4 Covalent radii and connectivity table for 2005src1385 in P-1 C 0.770 H 0.320 FE 1.240 BR 1.140 CL 0.990 PD 1.380 P 1.100 C1 - C2 C5 P1 Fe1 C2 - C3 C1 Br1 Fe1 C3 - C4 C2 Fe1 C4 - C3 C5 Fe1 C5 - C4 C1 Fe1 C6 - C7 C10 P2 Fe1 C7 - C8 C6 Br2 Fe1 C8 - C9 C7 Fe1 C9 - C8 C10 Fe1 C10 - C9 C6 Fe1 C11 - C16 C12 P1 C12 - C13 C11 C13 - C14 C12 C14 - C13 C15 C15 - C14 C16 C16 - C11 C15 C17 - C22 C18 P1 C18 - C19 C17 C19 - C20 C18 C20 - C19 C21 C21 - C20 C22 C22 - C17 C21 C23 - C24 C28 P2 C24 - C25 C23 C25 - C26 C24 C26 - C27 C25 C27 - C26 C28 C28 - C27 C23 C29 - C30 C34 P2 C30 - C29 C31 C31 - C32 C30 C32 - C33 C31 C33 - C32 C34 C34 - C33 C29 Fe1 - C7 C2 C6 C1 C10 C3 C8 C5 C9 C4 Br1 - C2 Br2 - C7 Cl1 - Pd1 Cl2 - Pd1 Pd1 - P2 P1 Cl2 Cl1 P1 - C1 C17 C11 Pd1 P2 - C6 C29 C23 Pd1 C41_a - Cl41_a Cl42_a Cl43_a Cl41_a - C41_a Cl42_a - C41_a Cl43_a - C41_a C51_b - Cl51_b Cl52_b Cl53_b Cl51_b - C51_b Cl52_b - C51_b Cl53_b - C51_b 34794 Reflections read, of which 23 rejected -13 =< h =< 13, -15 =< k =< 14, -21 =< l =< 20, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 8237 Unique reflections, of which 0 suppressed R(int) = 0.0426 R(sigma) = 0.0457 Friedel opposites merged Maximum memory for data reduction = 4150 / 82869 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 = 5364 / 591287 wR2 = 0.0972 before cycle 1 for 8237 data and 452 / 452 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 0.1642 0.0400 SAME/SADI Cl42_a Cl43_a Cl52_b Cl53_b -0.0302 0.0100 DELU Cl41_a Cl43_a 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. 6. 0. 0. 0. 12. 54. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.010 0.077 0.000 0.000 rms deviation 0.000 0.000 0.000 0.083 0.000 0.000 0.000 0.011 0.063 0.000 0.000 GooF = S = 1.034; Restrained GooF = 1.035 for 72 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0357 * P )^2 + 4.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41699 0.00045 -0.044 OSF 2 0.68377 0.00513 0.000 FVAR 2 Mean shift/esd = 0.007 Maximum = -0.048 for U11 Pd1 Max. shift = 0.000 A for Cl52_b Max. dU = 0.000 for Cl51_b Least-squares cycle 2 Maximum vector length = 511 Memory required = 5364 / 591287 wR2 = 0.0972 before cycle 2 for 8237 data and 452 / 452 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 0.1642 0.0400 SAME/SADI Cl42_a Cl43_a Cl52_b Cl53_b -0.0302 0.0100 DELU Cl41_a Cl43_a 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. 6. 0. 0. 0. 12. 54. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.010 0.077 0.000 0.000 rms deviation 0.000 0.000 0.000 0.083 0.000 0.000 0.000 0.011 0.063 0.000 0.000 GooF = S = 1.034; Restrained GooF = 1.035 for 72 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0357 * P )^2 + 4.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41698 0.00045 -0.026 OSF 2 0.68376 0.00513 -0.001 FVAR 2 Mean shift/esd = 0.002 Maximum = -0.026 for OSF Max. shift = 0.000 A for C51_b Max. dU = 0.000 for C51_b Least-squares cycle 3 Maximum vector length = 511 Memory required = 5364 / 591287 wR2 = 0.0972 before cycle 3 for 8237 data and 452 / 452 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 0.1643 0.0400 SAME/SADI Cl42_a Cl43_a Cl52_b Cl53_b -0.0302 0.0100 DELU Cl41_a Cl43_a 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. 6. 0. 0. 0. 12. 54. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.010 0.077 0.000 0.000 rms deviation 0.000 0.000 0.000 0.083 0.000 0.000 0.000 0.011 0.063 0.000 0.000 GooF = S = 1.034; Restrained GooF = 1.035 for 72 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0357 * P )^2 + 4.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41698 0.00045 0.002 OSF 2 0.68376 0.00513 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.003 for x Cl51_b Max. shift = 0.000 A for C51_b Max. dU = 0.000 for Cl53_b Least-squares cycle 4 Maximum vector length = 511 Memory required = 5364 / 591287 wR2 = 0.0972 before cycle 4 for 8237 data and 452 / 452 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 0.1643 0.0400 SAME/SADI Cl42_a Cl43_a Cl52_b Cl53_b -0.0302 0.0100 DELU Cl41_a Cl43_a 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. 6. 0. 0. 0. 12. 54. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.010 0.077 0.000 0.000 rms deviation 0.000 0.000 0.000 0.083 0.000 0.000 0.000 0.011 0.063 0.000 0.000 GooF = S = 1.034; Restrained GooF = 1.035 for 72 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0357 * P )^2 + 4.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41698 0.00045 0.001 OSF 2 0.68376 0.00513 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for C51_b Max. dU = 0.000 for Cl41_a Least-squares cycle 5 Maximum vector length = 511 Memory required = 5364 / 591287 wR2 = 0.0972 before cycle 5 for 8237 data and 452 / 452 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 0.1643 0.0400 SAME/SADI Cl42_a Cl43_a Cl52_b Cl53_b -0.0302 0.0100 DELU Cl41_a Cl43_a 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. 6. 0. 0. 0. 12. 54. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.010 0.077 0.000 0.000 rms deviation 0.000 0.000 0.000 0.083 0.000 0.000 0.000 0.011 0.063 0.000 0.000 GooF = S = 1.034; Restrained GooF = 1.035 for 72 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0357 * P )^2 + 4.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41698 0.00045 0.001 OSF 2 0.68376 0.00513 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for Cl53_b Max. dU = 0.000 for Cl51_b Least-squares cycle 6 Maximum vector length = 511 Memory required = 5364 / 591287 wR2 = 0.0972 before cycle 6 for 8237 data and 452 / 452 parameters Disagreeable restraints before cycle 6 Observed Target Error Sigma Restraint 0.1643 0.0400 SAME/SADI Cl42_a Cl43_a Cl52_b Cl53_b -0.0302 0.0100 DELU Cl41_a Cl43_a 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. 6. 0. 0. 0. 12. 54. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.010 0.077 0.000 0.000 rms deviation 0.000 0.000 0.000 0.083 0.000 0.000 0.000 0.011 0.063 0.000 0.000 GooF = S = 1.034; Restrained GooF = 1.035 for 72 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0357 * P )^2 + 4.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41698 0.00045 0.001 OSF 2 0.68376 0.00513 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for C51_b Max. dU = 0.000 for Cl51_b Least-squares cycle 7 Maximum vector length = 511 Memory required = 5364 / 591287 wR2 = 0.0972 before cycle 7 for 8237 data and 452 / 452 parameters Disagreeable restraints before cycle 7 Observed Target Error Sigma Restraint 0.1643 0.0400 SAME/SADI Cl42_a Cl43_a Cl52_b Cl53_b -0.0302 0.0100 DELU Cl41_a Cl43_a 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. 6. 0. 0. 0. 12. 54. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.010 0.077 0.000 0.000 rms deviation 0.000 0.000 0.000 0.083 0.000 0.000 0.000 0.011 0.063 0.000 0.000 GooF = S = 1.034; Restrained GooF = 1.035 for 72 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0357 * P )^2 + 4.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41698 0.00045 0.000 OSF 2 0.68376 0.00513 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for z Pd1 Max. shift = 0.000 A for C51_b Max. dU = 0.000 for Cl51_b Least-squares cycle 8 Maximum vector length = 511 Memory required = 5364 / 591287 wR2 = 0.0972 before cycle 8 for 8237 data and 452 / 452 parameters Disagreeable restraints before cycle 8 Observed Target Error Sigma Restraint 0.1643 0.0400 SAME/SADI Cl42_a Cl43_a Cl52_b Cl53_b -0.0302 0.0100 DELU Cl41_a Cl43_a 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. 6. 0. 0. 0. 12. 54. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.010 0.077 0.000 0.000 rms deviation 0.000 0.000 0.000 0.083 0.000 0.000 0.000 0.011 0.063 0.000 0.000 GooF = S = 1.034; Restrained GooF = 1.035 for 72 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0357 * P )^2 + 4.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41698 0.00045 0.000 OSF 2 0.68376 0.00513 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for z Pd1 Max. shift = 0.000 A for Cl53_b Max. dU = 0.000 for Cl51_b Least-squares cycle 9 Maximum vector length = 511 Memory required = 5364 / 591287 wR2 = 0.0972 before cycle 9 for 8237 data and 452 / 452 parameters Disagreeable restraints before cycle 9 Observed Target Error Sigma Restraint 0.1643 0.0400 SAME/SADI Cl42_a Cl43_a Cl52_b Cl53_b -0.0302 0.0100 DELU Cl41_a Cl43_a 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. 6. 0. 0. 0. 12. 54. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.010 0.077 0.000 0.000 rms deviation 0.000 0.000 0.000 0.083 0.000 0.000 0.000 0.011 0.063 0.000 0.000 GooF = S = 1.034; Restrained GooF = 1.035 for 72 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0357 * P )^2 + 4.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41698 0.00045 0.001 OSF 2 0.68376 0.00513 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for Cl53_b Max. dU = 0.000 for Cl41_a Least-squares cycle 10 Maximum vector length = 511 Memory required = 5364 / 591287 wR2 = 0.0972 before cycle 10 for 8237 data and 452 / 452 parameters Disagreeable restraints before cycle 10 Observed Target Error Sigma Restraint 0.1643 0.0400 SAME/SADI Cl42_a Cl43_a Cl52_b Cl53_b -0.0302 0.0100 DELU Cl41_a Cl43_a 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. 6. 0. 0. 0. 12. 54. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.010 0.077 0.000 0.000 rms deviation 0.000 0.000 0.000 0.083 0.000 0.000 0.000 0.011 0.063 0.000 0.000 GooF = S = 1.034; Restrained GooF = 1.035 for 72 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0357 * P )^2 + 4.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41698 0.00045 -0.001 OSF 2 0.68376 0.00513 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for Cl53_b Max. dU = 0.000 for Cl53_b Least-squares cycle 11 Maximum vector length = 511 Memory required = 5364 / 591287 wR2 = 0.0972 before cycle 11 for 8237 data and 452 / 452 parameters Disagreeable restraints before cycle 11 Observed Target Error Sigma Restraint 0.1643 0.0400 SAME/SADI Cl42_a Cl43_a Cl52_b Cl53_b -0.0302 0.0100 DELU Cl41_a Cl43_a 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. 6. 0. 0. 0. 12. 54. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.010 0.077 0.000 0.000 rms deviation 0.000 0.000 0.000 0.083 0.000 0.000 0.000 0.011 0.063 0.000 0.000 GooF = S = 1.034; Restrained GooF = 1.035 for 72 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0357 * P )^2 + 4.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41698 0.00045 0.001 OSF 2 0.68376 0.00513 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for Cl53_b Max. dU = 0.000 for Cl41_a Least-squares cycle 12 Maximum vector length = 511 Memory required = 5364 / 591287 wR2 = 0.0972 before cycle 12 for 8237 data and 452 / 452 parameters Disagreeable restraints before cycle 12 Observed Target Error Sigma Restraint 0.1643 0.0400 SAME/SADI Cl42_a Cl43_a Cl52_b Cl53_b -0.0302 0.0100 DELU Cl41_a Cl43_a 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. 6. 0. 0. 0. 12. 54. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.010 0.077 0.000 0.000 rms deviation 0.000 0.000 0.000 0.083 0.000 0.000 0.000 0.011 0.063 0.000 0.000 GooF = S = 1.034; Restrained GooF = 1.035 for 72 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0357 * P )^2 + 4.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41698 0.00045 -0.001 OSF 2 0.68376 0.00513 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for Cl53_b Max. dU = 0.000 for Cl53_b Least-squares cycle 13 Maximum vector length = 511 Memory required = 5364 / 591287 wR2 = 0.0972 before cycle 13 for 8237 data and 452 / 452 parameters Disagreeable restraints before cycle 13 Observed Target Error Sigma Restraint 0.1643 0.0400 SAME/SADI Cl42_a Cl43_a Cl52_b Cl53_b -0.0302 0.0100 DELU Cl41_a Cl43_a 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. 6. 0. 0. 0. 12. 54. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.010 0.077 0.000 0.000 rms deviation 0.000 0.000 0.000 0.083 0.000 0.000 0.000 0.011 0.063 0.000 0.000 GooF = S = 1.034; Restrained GooF = 1.035 for 72 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0357 * P )^2 + 4.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41698 0.00045 0.000 OSF 2 0.68376 0.00513 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for z Pd1 Max. shift = 0.000 A for Cl53_b Max. dU = 0.000 for Cl51_b Least-squares cycle 14 Maximum vector length = 511 Memory required = 5364 / 591287 wR2 = 0.0972 before cycle 14 for 8237 data and 452 / 452 parameters Disagreeable restraints before cycle 14 Observed Target Error Sigma Restraint 0.1643 0.0400 SAME/SADI Cl42_a Cl43_a Cl52_b Cl53_b -0.0302 0.0100 DELU Cl41_a Cl43_a 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. 6. 0. 0. 0. 12. 54. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.010 0.077 0.000 0.000 rms deviation 0.000 0.000 0.000 0.083 0.000 0.000 0.000 0.011 0.063 0.000 0.000 GooF = S = 1.034; Restrained GooF = 1.035 for 72 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0357 * P )^2 + 4.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41698 0.00045 0.000 OSF 2 0.68376 0.00513 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for z Pd1 Max. shift = 0.000 A for Cl53_b Max. dU = 0.000 for Cl53_b Least-squares cycle 15 Maximum vector length = 511 Memory required = 5364 / 591287 wR2 = 0.0972 before cycle 15 for 8237 data and 452 / 452 parameters Disagreeable restraints before cycle 15 Observed Target Error Sigma Restraint 0.1643 0.0400 SAME/SADI Cl42_a Cl43_a Cl52_b Cl53_b -0.0302 0.0100 DELU Cl41_a Cl43_a 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. 6. 0. 0. 0. 12. 54. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.010 0.077 0.000 0.000 rms deviation 0.000 0.000 0.000 0.083 0.000 0.000 0.000 0.011 0.063 0.000 0.000 GooF = S = 1.034; Restrained GooF = 1.035 for 72 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0357 * P )^2 + 4.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41698 0.00045 0.000 OSF 2 0.68376 0.00513 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for z Pd1 Max. shift = 0.000 A for Cl53_b Max. dU = 0.000 for Cl51_b Least-squares cycle 16 Maximum vector length = 511 Memory required = 5364 / 591287 wR2 = 0.0972 before cycle 16 for 8237 data and 452 / 452 parameters Disagreeable restraints before cycle 16 Observed Target Error Sigma Restraint 0.1643 0.0400 SAME/SADI Cl42_a Cl43_a Cl52_b Cl53_b -0.0302 0.0100 DELU Cl41_a Cl43_a 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. 6. 0. 0. 0. 12. 54. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.010 0.077 0.000 0.000 rms deviation 0.000 0.000 0.000 0.083 0.000 0.000 0.000 0.011 0.063 0.000 0.000 GooF = S = 1.034; Restrained GooF = 1.035 for 72 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0357 * P )^2 + 4.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41698 0.00045 0.000 OSF 2 0.68376 0.00513 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for z Pd1 Max. shift = 0.000 A for C51_b Max. dU = 0.000 for Cl53_b Least-squares cycle 17 Maximum vector length = 511 Memory required = 5364 / 591287 wR2 = 0.0972 before cycle 17 for 8237 data and 452 / 452 parameters Disagreeable restraints before cycle 17 Observed Target Error Sigma Restraint 0.1643 0.0400 SAME/SADI Cl42_a Cl43_a Cl52_b Cl53_b -0.0302 0.0100 DELU Cl41_a Cl43_a Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 12. 54. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.010 0.077 0.000 0.000 rms deviation 0.000 0.000 0.000 0.083 0.000 0.000 0.000 0.011 0.063 0.000 0.000 GooF = S = 1.034; Restrained GooF = 1.035 for 72 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0357 * P )^2 + 4.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41698 0.00045 0.000 OSF 2 0.68376 0.00513 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for z Pd1 Max. shift = 0.000 A for Cl53_b Max. dU = 0.000 for Cl51_b Least-squares cycle 18 Maximum vector length = 511 Memory required = 5364 / 591287 wR2 = 0.0972 before cycle 18 for 8237 data and 452 / 452 parameters Disagreeable restraints before cycle 18 Observed Target Error Sigma Restraint 0.1643 0.0400 SAME/SADI Cl42_a Cl43_a Cl52_b Cl53_b -0.0302 0.0100 DELU Cl41_a Cl43_a Summary of restraints applied in cycle 18 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 12. 54. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.010 0.077 0.000 0.000 rms deviation 0.000 0.000 0.000 0.083 0.000 0.000 0.000 0.011 0.063 0.000 0.000 GooF = S = 1.034; Restrained GooF = 1.035 for 72 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0357 * P )^2 + 4.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41698 0.00045 0.000 OSF 2 0.68376 0.00513 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for z Pd1 Max. shift = 0.000 A for C51_b Max. dU = 0.000 for Cl53_b Least-squares cycle 19 Maximum vector length = 511 Memory required = 5364 / 591287 wR2 = 0.0972 before cycle 19 for 8237 data and 452 / 452 parameters Disagreeable restraints before cycle 19 Observed Target Error Sigma Restraint 0.1643 0.0400 SAME/SADI Cl42_a Cl43_a Cl52_b Cl53_b -0.0302 0.0100 DELU Cl41_a Cl43_a Summary of restraints applied in cycle 19 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 12. 54. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.010 0.077 0.000 0.000 rms deviation 0.000 0.000 0.000 0.083 0.000 0.000 0.000 0.011 0.063 0.000 0.000 GooF = S = 1.034; Restrained GooF = 1.035 for 72 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0357 * P )^2 + 4.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41698 0.00045 0.000 OSF 2 0.68376 0.00513 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for z Pd1 Max. shift = 0.000 A for Cl53_b Max. dU = 0.000 for Cl51_b Least-squares cycle 20 Maximum vector length = 511 Memory required = 5364 / 591287 wR2 = 0.0972 before cycle 20 for 8237 data and 452 / 452 parameters Disagreeable restraints before cycle 20 Observed Target Error Sigma Restraint 0.1643 0.0400 SAME/SADI Cl42_a Cl43_a Cl52_b Cl53_b -0.0302 0.0100 DELU Cl41_a Cl43_a Summary of restraints applied in cycle 20 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 12. 54. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.010 0.077 0.000 0.000 rms deviation 0.000 0.000 0.000 0.083 0.000 0.000 0.000 0.011 0.063 0.000 0.000 GooF = S = 1.034; Restrained GooF = 1.035 for 72 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0357 * P )^2 + 4.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41698 0.00045 0.000 OSF 2 0.68376 0.00513 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for z Pd1 Max. shift = 0.000 A for Cl53_b Max. dU = 0.000 for C51_b Largest correlation matrix elements -0.824 z C51_b / z C41_a -0.699 z Cl53_b / z Cl41_a -0.640 U12 Cl41_a / y Cl41_a -0.803 y Cl53_b / y Cl41_a -0.692 U22 Cl53_b / y Cl41_a -0.629 x Cl53_b / x Cl41_a -0.782 U22 C51_b / U22 C41_a -0.691 U23 Cl43_a / U22 Cl43_a 0.627 y Cl53_b / U22 Cl41_a -0.773 x C51_b / x C41_a -0.651 U11 C51_b / U11 C41_a 0.625 y Cl53_b / U12 Cl41_a 0.740 x Cl53_b / U11 Cl41_a -0.646 U33 Cl53_b / z Cl41_a -0.600 U12 C51_b / U22 C51_b -0.737 y C51_b / y C41_a -0.646 U13 C51_b / U23 C51_b -0.599 U23 Cl42_a / U22 Cl42_a -0.725 U12 C51_b / U12 C41_a -0.644 U13 C51_b / U13 C41_a 0.595 z Cl53_b / U13 Cl41_a -0.718 U23 Cl43_a / U33 Cl43_a 0.642 U22 Cl53_b / U12 Cl41_a -0.592 z Cl43_a / y Cl43_a Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C3 ** H3 0.6450 0.0643 0.2131 43 0.950 0.000 C3 C4 C2 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C4 ** H4 0.6281 0.0498 0.0645 43 0.950 0.000 C4 C3 C5 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C5 ** H5 0.3919 0.0677 0.0453 43 0.950 0.000 C5 C4 C1 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C8 ** H8 0.6309 -0.2674 0.1356 43 0.950 0.000 C8 C9 C7 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C9 ** H9 0.7258 -0.2503 0.2624 43 0.950 0.000 C9 C8 C10 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C10 ** H10 0.5402 -0.2138 0.3756 43 0.950 0.000 C10 C9 C6 H12 0.1624 -0.0120 0.0598 43 0.950 0.000 C12 C13 C11 H13 0.1048 0.0572 -0.0838 43 0.950 0.000 C13 C14 C12 H14 0.0244 0.2720 -0.1559 43 0.950 0.000 C14 C13 C15 H15 0.0044 0.4181 -0.0827 43 0.950 0.000 C15 C14 C16 H16 0.0698 0.3498 0.0603 43 0.950 0.000 C16 C11 C15 H18 0.2606 0.3249 0.1594 43 0.950 0.000 C18 C19 C17 H19 0.1952 0.5009 0.2082 43 0.950 0.000 C19 C20 C18 H20 0.0113 0.5240 0.3040 43 0.950 0.000 C20 C19 C21 H21 -0.1102 0.3726 0.3497 43 0.950 0.000 C21 C20 C22 H22 -0.0448 0.1946 0.3019 43 0.950 0.000 C22 C17 C21 H24 0.3858 -0.4427 0.3139 43 0.950 0.000 C24 C25 C23 H25 0.3794 -0.6531 0.3833 43 0.950 0.000 C25 C26 C24 H26 0.2438 -0.7082 0.5085 43 0.950 0.000 C26 C27 C25 H27 0.1075 -0.5502 0.5624 43 0.950 0.000 C27 C26 C28 H28 0.1025 -0.3374 0.4891 43 0.950 0.000 C28 C27 C23 H30 0.1078 0.0113 0.3997 43 0.950 0.000 C30 C29 C31 H31 0.1115 0.0781 0.5191 43 0.950 0.000 C31 C32 C30 H32 0.2551 -0.0488 0.6299 43 0.950 0.000 C32 C33 C31 H33 0.3907 -0.2429 0.6231 43 0.950 0.000 C33 C32 C34 H34 0.3919 -0.3085 0.5030 43 0.950 0.000 C34 C33 C29 H41 0.7490 -0.6967 0.1544 13 1.000 0.000 C41_a Cl41_a Cl42_a Cl43_a H51 0.7288 -0.7045 0.1268 13 1.000 0.000 C51_b Cl51_b Cl52_b Cl53_b 2005src1385 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.34737 0.08337 0.17398 1.00000 0.02177 0.02718 0.03194 -0.01014 -0.00323 -0.01170 0.02537 0.00517 0.00038 0.00038 0.00027 0.00000 0.00188 0.00217 0.00229 0.00180 0.00164 0.00163 0.00085 C2 0.43860 0.08270 0.23129 1.00000 0.03161 0.03928 0.03786 -0.01775 0.00080 -0.01702 0.03332 0.00573 0.00042 0.00043 0.00030 0.00000 0.00226 0.00262 0.00261 0.00214 0.00191 0.00195 0.00100 C3 0.56682 0.06803 0.18943 1.00000 0.02291 0.04800 0.05691 -0.02022 0.00177 -0.02001 0.03967 0.00633 0.00042 0.00046 0.00034 0.00000 0.00211 0.00292 0.00322 0.00248 0.00204 0.00204 0.00114 H3 0.64498 0.06427 0.21305 1.00000 0.04761 0.00000 0.00000 C4 0.55694 0.06008 0.10649 1.00000 0.02949 0.04770 0.04945 -0.01960 0.01069 -0.01976 0.04034 0.00653 0.00044 0.00046 0.00033 0.00000 0.00232 0.00297 0.00306 0.00245 0.00210 0.00213 0.00114 H4 0.62808 0.04982 0.06452 1.00000 0.04841 0.00000 0.00000 C5 0.42465 0.06977 0.09569 1.00000 0.02748 0.03875 0.04012 -0.01643 0.00643 -0.01444 0.03401 0.00624 0.00041 0.00043 0.00031 0.00000 0.00217 0.00259 0.00266 0.00213 0.00190 0.00191 0.00101 H5 0.39189 0.06769 0.04526 1.00000 0.04081 0.00000 0.00000 C6 0.41000 -0.21674 0.28849 1.00000 0.02300 0.02791 0.03801 -0.01192 0.00021 -0.00556 0.02969 0.00585 0.00039 0.00040 0.00029 0.00000 0.00199 0.00226 0.00253 0.00194 0.00177 0.00168 0.00092 C7 0.44434 -0.23687 0.20527 1.00000 0.02788 0.03383 0.03904 -0.01718 0.00393 -0.00922 0.03244 0.00597 0.00041 0.00042 0.00030 0.00000 0.00215 0.00247 0.00259 0.00206 0.00186 0.00183 0.00097 C8 0.58292 -0.25297 0.18673 1.00000 0.02918 0.04446 0.05055 -0.02219 0.01066 -0.00522 0.04188 0.00708 0.00044 0.00046 0.00035 0.00000 0.00233 0.00291 0.00310 0.00245 0.00213 0.00206 0.00116 H8 0.63093 -0.26741 0.13560 1.00000 0.05026 0.00000 0.00000 C9 0.63568 -0.24366 0.25757 1.00000 0.02081 0.04608 0.05919 -0.01559 -0.00269 -0.00231 0.04371 0.00721 0.00044 0.00047 0.00035 0.00000 0.00213 0.00298 0.00337 0.00255 0.00213 0.00199 0.00120 H9 0.72575 -0.25031 0.26237 1.00000 0.05245 0.00000 0.00000 C10 0.53126 -0.22256 0.32106 1.00000 0.02513 0.03817 0.04543 -0.01326 -0.00792 -0.00507 0.03629 0.00632 0.00041 0.00043 0.00033 0.00000 0.00214 0.00262 0.00285 0.00220 0.00196 0.00188 0.00104 H10 0.54017 -0.21382 0.37557 1.00000 0.04355 0.00000 0.00000 C11 0.12350 0.16166 0.07463 1.00000 0.02147 0.02980 0.02385 -0.01018 0.00134 -0.01132 0.02383 0.00522 0.00037 0.00038 0.00026 0.00000 0.00188 0.00222 0.00208 0.00173 0.00155 0.00163 0.00082 C12 0.13165 0.07658 0.03052 1.00000 0.03810 0.03035 0.03632 -0.01608 -0.00521 -0.00741 0.03341 0.00584 0.00044 0.00043 0.00030 0.00000 0.00242 0.00240 0.00259 0.00202 0.00197 0.00190 0.00099 H12 0.16235 -0.01197 0.05980 1.00000 0.04009 0.00000 0.00000 C13 0.09635 0.11736 -0.05458 1.00000 0.03256 0.04493 0.03260 -0.02307 -0.00070 -0.01038 0.03383 0.00584 0.00042 0.00045 0.00029 0.00000 0.00228 0.00283 0.00249 0.00220 0.00188 0.00202 0.00101 H13 0.10483 0.05718 -0.08377 1.00000 0.04060 0.00000 0.00000 C14 0.04933 0.24351 -0.09716 1.00000 0.04603 0.05265 0.02558 -0.01422 -0.00803 -0.01257 0.04031 0.00638 0.00048 0.00049 0.00030 0.00000 0.00277 0.00316 0.00243 0.00224 0.00205 0.00236 0.00113 H14 0.02437 0.27198 -0.15587 1.00000 0.04837 0.00000 0.00000 C15 0.03837 0.32989 -0.05370 1.00000 0.10492 0.03340 0.03839 -0.00902 -0.03092 -0.00083 0.06036 0.00780 0.00067 0.00051 0.00035 0.00000 0.00495 0.00292 0.00305 0.00239 0.00316 0.00294 0.00168 H15 0.00438 0.41807 -0.08271 1.00000 0.07243 0.00000 0.00000 C16 0.07633 0.28944 0.03158 1.00000 0.07221 0.03358 0.03205 -0.01274 -0.01473 -0.00919 0.04501 0.00678 0.00055 0.00046 0.00031 0.00000 0.00359 0.00271 0.00267 0.00216 0.00246 0.00245 0.00125 H16 0.06978 0.34982 0.06025 1.00000 0.05401 0.00000 0.00000 C17 0.11556 0.24064 0.22717 1.00000 0.02880 0.02453 0.02376 -0.01035 -0.00500 -0.00829 0.02427 0.00512 0.00039 0.00037 0.00026 0.00000 0.00205 0.00211 0.00208 0.00169 0.00164 0.00165 0.00083 C18 0.18554 0.33368 0.19880 1.00000 0.03391 0.02788 0.03091 -0.00872 -0.00841 -0.01241 0.02935 0.00530 0.00042 0.00039 0.00028 0.00000 0.00224 0.00225 0.00235 0.00185 0.00183 0.00182 0.00092 H18 0.26059 0.32489 0.15942 1.00000 0.03522 0.00000 0.00000 C19 0.14656 0.43842 0.22751 1.00000 0.05273 0.02450 0.04281 -0.00890 -0.01835 -0.01389 0.03788 0.00585 0.00049 0.00042 0.00032 0.00000 0.00290 0.00232 0.00283 0.00205 0.00233 0.00206 0.00110 H19 0.19523 0.50085 0.20823 1.00000 0.04545 0.00000 0.00000 C20 0.03750 0.45237 0.28389 1.00000 0.07007 0.03005 0.03506 -0.01766 -0.00988 -0.00687 0.04366 0.00663 0.00055 0.00045 0.00032 0.00000 0.00351 0.00257 0.00272 0.00216 0.00247 0.00237 0.00122 H20 0.01132 0.52399 0.30403 1.00000 0.05239 0.00000 0.00000 C21 -0.03415 0.36216 0.31133 1.00000 0.06631 0.03543 0.03495 -0.02048 0.01186 -0.01271 0.04478 0.00715 0.00055 0.00045 0.00032 0.00000 0.00340 0.00273 0.00272 0.00225 0.00239 0.00243 0.00123 H21 -0.11023 0.37256 0.34968 1.00000 0.05374 0.00000 0.00000 C22 0.00475 0.25628 0.28298 1.00000 0.04296 0.02820 0.02903 -0.01242 0.00038 -0.01057 0.03246 0.00605 0.00045 0.00041 0.00028 0.00000 0.00253 0.00230 0.00236 0.00189 0.00192 0.00193 0.00096 H22 -0.04481 0.19459 0.30195 1.00000 0.03895 0.00000 0.00000 C23 0.24535 -0.36785 0.39464 1.00000 0.02086 0.02687 0.02459 -0.00526 -0.00533 -0.00653 0.02437 0.00530 0.00037 0.00038 0.00026 0.00000 0.00186 0.00214 0.00212 0.00170 0.00157 0.00158 0.00083 C24 0.32757 -0.46346 0.36382 1.00000 0.02800 0.03279 0.03375 -0.01414 -0.00323 -0.00536 0.03095 0.00575 0.00041 0.00041 0.00029 0.00000 0.00212 0.00242 0.00243 0.00197 0.00180 0.00179 0.00094 H24 0.38577 -0.44271 0.31392 1.00000 0.03713 0.00000 0.00000 C25 0.32464 -0.58875 0.40580 1.00000 0.03622 0.02796 0.05637 -0.01713 -0.00996 -0.00411 0.03929 0.00630 0.00046 0.00043 0.00034 0.00000 0.00248 0.00245 0.00323 0.00226 0.00225 0.00194 0.00111 H25 0.37937 -0.65314 0.38335 1.00000 0.04715 0.00000 0.00000 C26 0.24367 -0.62164 0.47960 1.00000 0.04474 0.02921 0.03957 -0.00173 -0.01387 -0.01419 0.03802 0.00618 0.00047 0.00044 0.00031 0.00000 0.00267 0.00246 0.00276 0.00206 0.00219 0.00207 0.00108 H26 0.24377 -0.70817 0.50850 1.00000 0.04562 0.00000 0.00000 C27 0.16270 -0.52812 0.51105 1.00000 0.04287 0.04030 0.02847 -0.00420 -0.00162 -0.01587 0.03794 0.00647 0.00047 0.00045 0.00030 0.00000 0.00262 0.00274 0.00245 0.00206 0.00201 0.00217 0.00106 H27 0.10746 -0.55024 0.56237 1.00000 0.04553 0.00000 0.00000 C28 0.16127 -0.40159 0.46821 1.00000 0.03362 0.03156 0.03317 -0.00979 -0.00180 -0.00953 0.03268 0.00599 0.00043 0.00042 0.00029 0.00000 0.00230 0.00244 0.00248 0.00197 0.00188 0.00188 0.00097 H28 0.10254 -0.33735 0.48914 1.00000 0.03922 0.00000 0.00000 C29 0.25246 -0.15285 0.43797 1.00000 0.02193 0.03651 0.02813 -0.01366 0.00006 -0.01239 0.02702 0.00533 0.00038 0.00041 0.00027 0.00000 0.00192 0.00240 0.00224 0.00189 0.00164 0.00174 0.00088 C30 0.16731 -0.03963 0.44435 1.00000 0.03025 0.04039 0.02873 -0.01566 -0.00260 -0.01208 0.03110 0.00562 0.00042 0.00043 0.00029 0.00000 0.00218 0.00258 0.00232 0.00199 0.00178 0.00190 0.00094 H30 0.10779 0.01134 0.39969 1.00000 0.03731 0.00000 0.00000 C31 0.16853 -0.00031 0.51571 1.00000 0.03036 0.05381 0.04361 -0.03214 0.00350 -0.01592 0.03757 0.00576 0.00044 0.00048 0.00031 0.00000 0.00229 0.00304 0.00282 0.00245 0.00202 0.00212 0.00110 H31 0.11145 0.07811 0.51914 1.00000 0.04509 0.00000 0.00000 C32 0.25305 -0.07576 0.58143 1.00000 0.03195 0.07755 0.03771 -0.03275 0.00493 -0.02532 0.04343 0.00626 0.00045 0.00054 0.00032 0.00000 0.00243 0.00385 0.00277 0.00271 0.00206 0.00253 0.00125 H32 0.25515 -0.04876 0.62986 1.00000 0.05212 0.00000 0.00000 C33 0.33443 -0.19031 0.57686 1.00000 0.03523 0.07228 0.03271 -0.01787 -0.00983 -0.01779 0.04467 0.00644 0.00047 0.00054 0.00032 0.00000 0.00254 0.00374 0.00266 0.00255 0.00206 0.00252 0.00124 H33 0.39066 -0.24294 0.62310 1.00000 0.05360 0.00000 0.00000 C34 0.33515 -0.22950 0.50569 1.00000 0.02718 0.04777 0.03578 -0.01440 -0.00899 -0.00831 0.03611 0.00599 0.00043 0.00047 0.00030 0.00000 0.00218 0.00285 0.00259 0.00220 0.00189 0.00199 0.00104 H34 0.39188 -0.30846 0.50302 1.00000 0.04334 0.00000 0.00000 Fe1 0.49061 -0.08138 0.20450 1.00000 0.01804 0.03718 0.03827 -0.01610 0.00331 -0.01033 0.02989 0.00083 0.00005 0.00006 0.00004 0.00000 0.00028 0.00036 0.00037 0.00029 0.00025 0.00025 0.00015 Br1 0.40375 0.10320 0.34223 1.00000 0.03445 0.04662 0.04111 -0.02110 -0.00415 -0.01699 0.03711 0.00058 0.00004 0.00005 0.00003 0.00000 0.00024 0.00029 0.00028 0.00022 0.00020 0.00021 0.00012 Br2 0.32899 -0.25509 0.13614 1.00000 0.04367 0.03855 0.03643 -0.01732 -0.00384 -0.01152 0.03771 0.00062 0.00005 0.00004 0.00003 0.00000 0.00026 0.00027 0.00026 0.00021 0.00020 0.00021 0.00012 Cl1 -0.11461 0.08220 0.19589 1.00000 0.01757 0.02993 0.03152 -0.01103 -0.00465 -0.00552 0.02578 0.00127 0.00009 0.00009 0.00007 0.00000 0.00042 0.00052 0.00054 0.00043 0.00037 0.00037 0.00021 Cl2 -0.04851 -0.20975 0.32650 1.00000 0.02469 0.02938 0.03336 -0.00659 -0.00268 -0.01445 0.02828 0.00132 0.00009 0.00009 0.00007 0.00000 0.00046 0.00054 0.00056 0.00044 0.00040 0.00040 0.00022 Pd1 0.07557 -0.06148 0.26283 1.00000 0.01563 0.02256 0.02176 -0.01011 -0.00103 -0.00739 0.01861 0.00036 0.00003 0.00003 0.00002 0.00000 0.00014 0.00016 0.00016 0.00012 0.00011 0.00011 0.00008 P1 0.16960 0.10316 0.18832 1.00000 0.01935 0.02505 0.02476 -0.01116 -0.00076 -0.00944 0.02140 0.00130 0.00009 0.00010 0.00007 0.00000 0.00047 0.00053 0.00054 0.00043 0.00039 0.00040 0.00021 P2 0.24746 -0.20093 0.34334 1.00000 0.01795 0.02515 0.02633 -0.01027 -0.00273 -0.00609 0.02230 0.00134 0.00009 0.00010 0.00007 0.00000 0.00046 0.00053 0.00055 0.00044 0.00039 0.00039 0.00021 C41_a 0.68307 -0.61895 0.12168 0.68376 0.09707 0.02972 0.05326 -0.01759 -0.01386 0.00736 0.06306 0.02050 0.00164 0.00119 0.00096 0.00513 0.00904 0.00664 0.00590 0.00503 0.00590 0.00593 0.00326 H41_a 0.74898 -0.69668 0.15441 0.68376 0.07568 0.00513 0.00000 Cl41_a 0.54752 -0.59774 0.18957 0.68376 0.16673 0.05443 0.04381 -0.00603 0.03109 0.00261 0.10203 0.00937 0.00064 0.00059 0.00030 0.00513 0.00537 0.00233 0.00164 0.00152 0.00234 0.00282 0.00201 Cl42_a 0.65017 -0.64432 0.02955 0.68376 0.11868 0.08970 0.04904 -0.03108 -0.00467 -0.02165 0.08455 0.00401 0.00032 0.00030 0.00017 0.00513 0.00239 0.00223 0.00155 0.00146 0.00141 0.00171 0.00110 Cl43_a 0.75703 -0.49101 0.08876 0.68376 0.10361 0.05892 0.14043 -0.05573 0.02090 -0.01843 0.09815 0.00498 0.00033 0.00028 0.00027 0.00513 0.00231 0.00184 0.00363 0.00215 0.00214 0.00155 0.00140 C51_b 0.67619 -0.61652 0.12396 0.31624 0.04399 0.04378 0.09955 0.02240 -0.00467 -0.02175 0.07230 0.03492 0.00241 0.00242 0.00171 0.00513 0.01185 0.01698 0.01233 0.01019 0.01204 0.01267 0.00657 H51_b 0.72885 -0.70450 0.12679 0.31624 0.08677 0.00513 0.00000 Cl51_b 0.67686 -0.51535 0.02061 0.31624 0.12863 0.20991 0.09186 0.04819 0.02524 -0.03429 0.17520 0.02099 0.00099 0.00123 0.00058 0.00513 0.00724 0.01247 0.00547 0.00652 0.00494 0.00735 0.00647 Cl52_b 0.74232 -0.55624 0.18549 0.31624 0.13384 0.08845 0.20127 -0.03129 -0.06294 -0.03135 0.13864 0.01146 0.00094 0.00080 0.00080 0.00513 0.00677 0.00545 0.01051 0.00622 0.00713 0.00487 0.00416 Cl53_b 0.52122 -0.61708 0.17673 0.31624 0.04955 0.06066 0.15737 0.00678 0.02390 -0.01542 0.10351 0.01964 0.00102 0.00135 0.00095 0.00513 0.00335 0.00581 0.01059 0.00575 0.00447 0.00342 0.00479 Final Structure Factor Calculation for 2005src1385 in P-1 Total number of l.s. parameters = 452 Maximum vector length = 511 Memory required = 4912 / 26061 wR2 = 0.0972 before cycle 21 for 8237 data and 0 / 452 parameters Disagreeable restraints before cycle 21 Observed Target Error Sigma Restraint 0.1643 0.0400 SAME/SADI Cl42_a Cl43_a Cl52_b Cl53_b -0.0302 0.0100 DELU Cl41_a Cl43_a Summary of restraints applied in cycle 21 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 12. 54. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.010 0.077 0.000 0.000 rms deviation 0.000 0.000 0.000 0.083 0.000 0.000 0.000 0.011 0.063 0.000 0.000 GooF = S = 1.034; Restrained GooF = 1.035 for 72 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0357 * P )^2 + 4.65 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0398 for 6426 Fo > 4sig(Fo) and 0.0609 for all 8237 data wR2 = 0.0972, GooF = S = 1.034, Restrained GooF = 1.035 for all data Occupancy sum of asymmetric unit = 46.00 for non-hydrogen and 27.00 for hydrogen atoms Principal mean square atomic displacements U 0.0322 0.0294 0.0145 C1 0.0450 0.0334 0.0216 C2 0.0582 0.0465 0.0143 C3 0.0577 0.0426 0.0207 C4 0.0459 0.0339 0.0223 C5 0.0385 0.0279 0.0227 C6 0.0426 0.0292 0.0255 C7 0.0574 0.0468 0.0215 C8 0.0608 0.0499 0.0205 C9 0.0468 0.0390 0.0231 C10 0.0312 0.0227 0.0177 C11 0.0419 0.0349 0.0234 C12 0.0486 0.0323 0.0206 C13 0.0530 0.0473 0.0206 C14 0.1182 0.0361 0.0268 C15 0.0762 0.0342 0.0246 C16 0.0305 0.0260 0.0163 C17 0.0402 0.0287 0.0192 C18 0.0640 0.0313 0.0183 C19 0.0739 0.0370 0.0201 C20 0.0743 0.0391 0.0209 C21 0.0435 0.0305 0.0234 C22 0.0305 0.0248 0.0178 C23 0.0372 0.0282 0.0274 C24 0.0585 0.0340 0.0253 C25 0.0576 0.0307 0.0258 C26 0.0482 0.0391 0.0265 C27 0.0340 0.0334 0.0307 C28 0.0375 0.0257 0.0179 C29 0.0411 0.0306 0.0216 C30 0.0624 0.0287 0.0216 C31 0.0797 0.0281 0.0225 C32 0.0730 0.0415 0.0195 C33 0.0486 0.0388 0.0209 C34 0.0414 0.0320 0.0162 Fe1 0.0502 0.0397 0.0215 Br1 0.0440 0.0416 0.0275 Br2 0.0327 0.0287 0.0160 Cl1 0.0381 0.0306 0.0162 Cl2 0.0246 0.0188 0.0124 Pd1 0.0278 0.0221 0.0143 P1 0.0276 0.0230 0.0164 P2 0.1131 0.0510 0.0251 C41_a 0.2170 0.0539 0.0352 Cl41_a may be split into 0.5609 -0.5937 0.1950 and 0.5342 -0.6018 0.1841 0.1219 0.0898 0.0419 Cl42_a 0.1572 0.0967 0.0405 Cl43_a 0.1482 0.0463 0.0224 C51_b 0.3413 0.1352 0.0491 Cl51_b may be split into 0.6734 -0.5049 0.0305 and 0.6803 -0.5258 0.0107 0.2327 0.1021 0.0812 Cl52_b 0.2139 0.0578 0.0389 Cl53_b may be split into 0.5218 -0.6189 0.1892 and 0.5206 -0.6153 0.1643 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.019 0.036 0.053 0.073 0.094 0.119 0.151 0.194 0.269 1.000 Number in group 845. 844. 786. 840. 820. 834. 805. 810. 826. 827. GooF 0.909 1.070 1.028 1.049 1.091 1.085 0.990 1.069 0.982 1.058 K 1.476 1.032 0.974 0.963 0.977 0.986 0.995 1.005 1.015 1.005 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.64 inf Number in group 839. 815. 828. 829. 807. 840. 806. 822. 828. 823. GooF 0.963 0.910 0.913 0.966 0.926 0.924 0.952 0.886 1.010 1.661 K 0.973 1.011 1.018 1.020 1.018 1.006 1.019 1.014 1.006 0.992 R1 0.155 0.119 0.107 0.086 0.065 0.052 0.043 0.033 0.027 0.032 Recommended weighting scheme: WGHT 0.0355 4.6535 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) -2 0 1 2593.54 1621.25 7.86 0.168 4.74 -3 1 2 3013.62 2079.73 6.48 0.190 2.84 -2 1 2 170.56 34.41 6.44 0.024 3.79 4 2 2 872.50 508.18 5.97 0.094 2.60 -1 3 5 392.02 175.63 5.88 0.055 2.53 0 0 4 1192.57 763.31 5.56 0.115 3.82 1 1 3 867.37 537.75 5.36 0.097 5.10 1 2 1 784.38 482.69 5.20 0.091 5.61 -3 0 1 4251.04 5473.72 4.95 0.308 3.26 6 1 1 121.19 27.07 4.77 0.022 1.75 2 2 1 1150.41 792.39 4.77 0.117 4.45 -1 5 2 281.35 125.96 4.76 0.047 2.05 -1 4 2 581.05 350.47 4.56 0.078 2.50 4 2 3 89.33 22.27 4.41 0.020 2.51 -2 -2 3 1595.60 2122.59 4.34 0.192 2.86 1 3 5 195.47 85.12 4.29 0.038 2.88 4 1 5 5294.67 6474.17 4.16 0.335 2.14 -3 2 1 841.92 578.63 4.14 0.100 2.57 -3 3 2 908.09 641.53 3.92 0.105 2.18 5 4 2 417.40 251.75 3.87 0.066 1.93 3 -1 2 270.57 137.64 3.83 0.049 2.75 0 4 1 299.88 502.11 3.82 0.093 2.74 1 -1 1 685.50 961.67 3.79 0.129 5.67 3 13 3 52.65 265.82 3.73 0.068 0.88 0 4 2 2137.44 2672.59 3.67 0.215 2.77 1 2 3 1621.59 1266.37 3.63 0.148 4.53 0 -1 5 2681.79 2168.87 3.56 0.194 2.71 2 1 8 1403.40 1790.97 3.54 0.176 1.93 6 -3 10 1635.45 40.00 3.53 0.026 0.99 2 2 4 846.15 1135.44 3.52 0.140 3.39 1 -2 1 78.73 21.91 3.51 0.019 3.86 -4 0 3 1274.42 1636.26 3.51 0.168 2.22 8 5 2 149.19 63.04 3.50 0.033 1.27 -4 1 4 3165.34 3821.58 3.47 0.257 2.01 6 -7 10 2.39 256.39 3.45 0.067 0.78 1 0 5 1564.46 1229.80 3.45 0.146 2.97 0 2 1 2180.13 1715.15 3.42 0.172 5.55 -4 -3 1 2426.56 2955.51 3.39 0.226 2.25 10 7 2 140.51 30.14 3.33 0.023 0.99 3 7 1 599.56 423.68 3.32 0.086 1.57 -3 -4 1 1342.31 1049.29 3.32 0.135 2.26 0 -2 1 5896.92 4995.58 3.31 0.294 4.55 -6 1 4 1903.59 1532.91 3.27 0.163 1.48 2 1 1 1443.49 1802.72 3.26 0.177 5.19 -3 -3 2 8963.56 7755.03 3.25 0.366 2.42 -2 -1 4 5766.29 4931.32 3.22 0.292 2.79 5 2 3 1587.51 1960.57 3.21 0.184 2.06 2 4 2 55.96 130.52 3.18 0.048 2.80 6 4 2 305.02 190.80 3.16 0.057 1.68 0 2 4 13730.96 12024.96 3.15 0.456 3.70 Bond lengths and angles C1 - Distance Angles C2 1.4404 (0.0056) C5 1.4416 (0.0059) 105.67 (0.35) P1 1.8234 (0.0039) 130.36 (0.32) 123.92 (0.30) Fe1 2.0231 (0.0041) 68.28 (0.24) 70.47 (0.25) 127.50 (0.21) C1 - C2 C5 P1 C2 - Distance Angles C3 1.4200 (0.0059) C1 1.4404 (0.0056) 109.13 (0.39) Br1 1.8741 (0.0044) 122.31 (0.33) 128.53 (0.32) Fe1 2.0027 (0.0044) 71.08 (0.26) 69.80 (0.23) 126.96 (0.25) C2 - C3 C1 Br1 C3 - Distance Angles C4 1.4083 (0.0068) C2 1.4200 (0.0059) 107.48 (0.39) Fe1 2.0453 (0.0043) 70.74 (0.26) 67.86 (0.24) H3 0.9500 126.26 126.26 126.68 C3 - C4 C2 Fe1 C4 - Distance Angles C3 1.4083 (0.0068) C5 1.4094 (0.0060) 109.13 (0.40) Fe1 2.0655 (0.0047) 69.19 (0.27) 69.58 (0.26) H4 0.9500 125.44 125.44 127.39 C4 - C3 C5 Fe1 C5 - Distance Angles C4 1.4094 (0.0060) C1 1.4416 (0.0059) 108.59 (0.39) Fe1 2.0545 (0.0049) 70.42 (0.28) 68.13 (0.25) H5 0.9500 125.71 125.71 127.32 C5 - C4 C1 Fe1 C6 - Distance Angles C7 1.4320 (0.0061) C10 1.4405 (0.0058) 106.16 (0.37) P2 1.8111 (0.0041) 125.55 (0.32) 128.11 (0.35) Fe1 2.0048 (0.0043) 68.81 (0.24) 70.48 (0.26) 129.11 (0.23) C6 - C7 C10 P2 C7 - Distance Angles C8 1.4277 (0.0059) C6 1.4320 (0.0061) 109.05 (0.39) Br2 1.8832 (0.0043) 125.08 (0.34) 125.64 (0.31) Fe1 1.9986 (0.0042) 71.12 (0.26) 69.27 (0.24) 130.12 (0.25) C7 - C8 C6 Br2 C8 - Distance Angles C9 1.4057 (0.0071) C7 1.4277 (0.0059) 107.84 (0.41) Fe1 2.0461 (0.0047) 70.62 (0.28) 67.56 (0.25) H8 0.9500 126.08 126.08 127.29 C8 - C9 C7 Fe1 C9 - Distance Angles C8 1.4057 (0.0071) C10 1.4265 (0.0066) 108.53 (0.39) Fe1 2.0623 (0.0047) 69.37 (0.28) 68.84 (0.26) H9 0.9500 125.73 125.73 127.64 C9 - C8 C10 Fe1 C10 - Distance Angles C9 1.4265 (0.0066) C6 1.4405 (0.0058) 108.42 (0.42) Fe1 2.0407 (0.0049) 70.47 (0.28) 67.81 (0.25) H10 0.9500 125.79 125.79 127.49 C10 - C9 C6 Fe1 C11 - Distance Angles C16 1.3768 (0.0062) C12 1.3861 (0.0055) 118.30 (0.39) P1 1.8293 (0.0041) 121.57 (0.31) 120.09 (0.32) C11 - C16 C12 C12 - Distance Angles C13 1.3744 (0.0061) C11 1.3861 (0.0055) 121.54 (0.42) H12 0.9500 119.23 119.23 C12 - C13 C11 C13 - Distance Angles C14 1.3601 (0.0067) C12 1.3744 (0.0061) 120.27 (0.41) H13 0.9500 119.87 119.87 C13 - C14 C12 C14 - Distance Angles C13 1.3601 (0.0067) C15 1.3851 (0.0067) 119.04 (0.43) H14 0.9500 120.48 120.48 C14 - C13 C15 C15 - Distance Angles C14 1.3851 (0.0067) C16 1.3870 (0.0067) 120.93 (0.48) H15 0.9500 119.54 119.54 C15 - C14 C16 C16 - Distance Angles C11 1.3768 (0.0062) C15 1.3870 (0.0067) 119.90 (0.43) H16 0.9500 120.05 120.05 C16 - C11 C15 C17 - Distance Angles C22 1.3838 (0.0058) C18 1.3966 (0.0055) 118.99 (0.37) P1 1.8253 (0.0039) 121.41 (0.30) 119.58 (0.31) C17 - C22 C18 C18 - Distance Angles C19 1.3819 (0.0059) C17 1.3966 (0.0055) 120.57 (0.42) H18 0.9500 119.72 119.72 C18 - C19 C17 C19 - Distance Angles C20 1.3740 (0.0071) C18 1.3819 (0.0059) 120.08 (0.42) H19 0.9500 119.96 119.96 C19 - C20 C18 C20 - Distance Angles C19 1.3740 (0.0071) C21 1.3830 (0.0070) 120.00 (0.42) H20 0.9500 120.00 120.00 C20 - C19 C21 C21 - Distance Angles C20 1.3830 (0.0070) C22 1.3904 (0.0059) 120.24 (0.46) H21 0.9500 119.88 119.88 C21 - C20 C22 C22 - Distance Angles C17 1.3838 (0.0058) C21 1.3904 (0.0059) 120.10 (0.42) H22 0.9500 119.95 119.95 C22 - C17 C21 C23 - Distance Angles C24 1.3914 (0.0057) C28 1.3955 (0.0057) 118.53 (0.38) P2 1.8304 (0.0041) 122.02 (0.32) 119.43 (0.31) C23 - C24 C28 C24 - Distance Angles C25 1.3838 (0.0063) C23 1.3914 (0.0057) 120.05 (0.42) H24 0.9500 119.98 119.98 C24 - C25 C23 C25 - Distance Angles C26 1.3772 (0.0068) C24 1.3838 (0.0063) 121.07 (0.44) H25 0.9500 119.46 119.46 C25 - C26 C24 C26 - Distance Angles C27 1.3745 (0.0067) C25 1.3772 (0.0068) 119.40 (0.43) H26 0.9500 120.30 120.30 C26 - C27 C25 C27 - Distance Angles C26 1.3745 (0.0067) C28 1.3873 (0.0063) 120.32 (0.44) H27 0.9500 119.84 119.84 C27 - C26 C28 C28 - Distance Angles C27 1.3873 (0.0063) C23 1.3955 (0.0057) 120.58 (0.42) H28 0.9500 119.71 119.71 C28 - C27 C23 C29 - Distance Angles C30 1.3889 (0.0059) C34 1.3925 (0.0060) 119.23 (0.39) P2 1.8254 (0.0041) 119.05 (0.31) 121.65 (0.33) C29 - C30 C34 C30 - Distance Angles C29 1.3889 (0.0059) C31 1.3919 (0.0058) 120.48 (0.42) H30 0.9500 119.76 119.76 C30 - C29 C31 C31 - Distance Angles C32 1.3796 (0.0070) C30 1.3919 (0.0058) 119.68 (0.45) H31 0.9500 120.16 120.16 C31 - C32 C30 C32 - Distance Angles C33 1.3783 (0.0072) C31 1.3796 (0.0070) 120.01 (0.43) H32 0.9500 119.99 119.99 C32 - C33 C31 C33 - Distance Angles C32 1.3783 (0.0072) C34 1.3835 (0.0064) 120.74 (0.46) H33 0.9500 119.63 119.63 C33 - C32 C34 C34 - Distance Angles C33 1.3835 (0.0064) C29 1.3925 (0.0060) 119.79 (0.45) H34 0.9500 120.11 120.11 C34 - C33 C29 Fe1 - Distance Angles C7 1.9986 (0.0043) C2 2.0027 (0.0044) 149.17 (0.17) C6 2.0048 (0.0043) 41.92 (0.17) 114.19 (0.18) C1 2.0231 (0.0041) 116.89 (0.16) 41.92 (0.16) 107.73 (0.16) C10 2.0407 (0.0049) 69.29 (0.19) 106.34 (0.19) 41.71 (0.17) 130.78 (0.18) C3 2.0453 (0.0043) 169.60 (0.18) 41.06 (0.17) 146.06 (0.19) 69.90 (0.17) 113.02 (0.19) C8 2.0461 (0.0047) 41.32 (0.17) 167.35 (0.19) 70.17 (0.18) 149.92 (0.19) 68.47 (0.20) 129.05 (0.18) C5 2.0545 (0.0049) 111.14 (0.18) 68.94 (0.18) 133.28 (0.17) 41.40 (0.16) 171.92 (0.17) 68.11 (0.19) 117.53 (0.20) C9 2.0623 (0.0047) 68.63 (0.19) 128.78 (0.20) 69.73 (0.18) 169.32 (0.19) 40.69 (0.19) 106.09 (0.19) 40.02 (0.20) C4 2.0655 (0.0047) 132.87 (0.19) 68.17 (0.19) 172.57 (0.18) 68.97 (0.17) 145.44 (0.18) 40.07 (0.19) 109.11 (0.19) Fe1 - C7 C2 C6 C1 C10 C3 C8 Br1 - Distance Angles C2 1.8741 (0.0044) Br1 - Br2 - Distance Angles C7 1.8832 (0.0043) Br2 - Cl1 - Distance Angles Pd1 2.3439 (0.0010) Cl1 - Cl2 - Distance Angles Pd1 2.3343 (0.0010) Cl2 - Pd1 - Distance Angles P2 2.2816 (0.0010) P1 2.2944 (0.0010) 99.98 (0.04) Cl2 2.3343 (0.0010) 88.81 (0.04) 171.20 (0.04) Cl1 2.3439 (0.0010) 173.24 (0.04) 83.18 (0.04) 88.10 (0.03) Pd1 - P2 P1 Cl2 P1 - Distance Angles C1 1.8234 (0.0039) C17 1.8253 (0.0039) 101.49 (0.18) C11 1.8293 (0.0041) 101.35 (0.18) 105.85 (0.18) Pd1 2.2944 (0.0010) 122.98 (0.14) 115.39 (0.13) 107.86 (0.12) P1 - C1 C17 C11 P2 - Distance Angles C6 1.8111 (0.0041) C29 1.8254 (0.0041) 107.45 (0.19) C23 1.8304 (0.0041) 101.10 (0.19) 102.00 (0.19) Pd1 2.2816 (0.0010) 117.00 (0.15) 108.40 (0.14) 119.40 (0.13) P2 - C6 C29 C23 C41_a - Distance Angles Cl41_a 1.6921 (0.0168) Cl42_a 1.7288 (0.0128) 112.27 (0.98) Cl43_a 1.7636 (0.0175) 112.81 (0.62) 108.91 (0.90) H41_a 1.0000 107.54 107.54 107.54 C41_a - Cl41_a Cl42_a Cl43_a Cl41_a - Distance Angles C41_a 1.6921 (0.0168) Cl41_a - Cl42_a - Distance Angles C41_a 1.7288 (0.0128) Cl42_a - Cl43_a - Distance Angles C41_a 1.7636 (0.0175) Cl43_a - C51_b - Distance Angles Cl51_b 1.6888 (0.0254) Cl52_b 1.7237 (0.0240) 105.96 (1.54) Cl53_b 1.7398 (0.0255) 115.44 (1.42) 101.25 (1.46) H51_b 1.0000 111.21 111.21 111.21 C51_b - Cl51_b Cl52_b Cl53_b Cl51_b - Distance Angles C51_b 1.6888 (0.0254) Cl51_b - Cl52_b - Distance Angles C51_b 1.7237 (0.0240) Cl52_b - Cl53_b - Distance Angles C51_b 1.7398 (0.0255) Cl53_b - FMAP and GRID set by program FMAP 2 3 42 GRID -1.282 -2 -2 1.282 2 2 R1 = 0.0588 for 8237 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.68 at 0.4246 0.1425 0.0099 [ 0.99 A from H5 ] Deepest hole -1.31 at 0.3976 0.1363 0.3035 [ 0.62 A from BR1 ] Mean = 0.00, Rms deviation from mean = 0.11 e/A^3, Highest memory used = 4597 / 35037 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4246 0.1425 0.0099 1.00000 0.05 1.68 0.99 H5 1.36 C5 2.05 C4 2.28 H4 Q2 1 0.6125 -0.3274 0.3872 1.00000 0.05 1.18 1.28 H10 1.47 C10 2.01 C9 2.24 H9 Q3 1 0.4996 -0.6014 0.0699 1.00000 0.05 0.95 1.64 CL42 1.73 CL53 2.11 CL41 2.13 C51 Q4 1 0.7645 -0.5979 0.0227 1.00000 0.05 0.62 1.12 CL51 1.44 CL42 1.69 C41 1.75 C51 Q5 1 0.6575 -0.5745 0.1927 1.00000 0.05 0.60 0.97 CL52 1.28 CL41 1.34 C51 1.38 C41 Shortest distances between peaks (including symmetry equivalents) 3 3 2.65 3 4 2.81 4 5 2.91 3 5 2.94 Time profile in seconds ----------------------- 0.06: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.01: 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 0.00: Analyse other restraints etc. 1.27: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.06: Set up l.s. refinement 0.00: Generate idealized H-atoms 10.70: Structure factors and derivatives 49.11: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.07: Apply other restraints 3.38: Solve l.s. equations 0.00: Generate HTAB table 0.11: Other dependent quantities, CIF, tables 0.15: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2005src1385 finished at 15:57:25 Total CPU time: 64.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++