+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2005src1384 started at 12:49:27 on 30-Nov-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2005src1384 in P2(1) CELL 0.71073 12.3194 10.9269 15.3899 90.000 94.958 90.000 ZERR 2.00 0.0004 0.0003 0.0005 0.000 0.002 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H P FE NI BR UNIT 88 72 4 4 2 8 V = 2063.93 F(000) = 1100.0 Mu = 5.13 mm-1 Cell Wt = 2233.44 Rho = 1.797 MERG 2 OMIT -3.00 55.00 OMIT -1 0 2 OMIT 0 1 2 OMIT 1 0 4 FMAP 2 PLAN 20 SIZE 0.01 0.04 0.30 ACTA BOND WGHT 0.06370 6.29600 L.S. 20 TEMP -153.00 FVAR 0.41418 C13 1 0.977606 0.106643 0.848520 11.00000 0.04153 0.10625 = 0.06465 -0.00411 0.01322 -0.01949 AFIX 43 H13 2 1.020523 0.053037 0.816987 11.00000 -1.20000 AFIX 0 C14 1 1.015239 0.154026 0.926219 11.00000 0.03290 0.20118 = 0.07200 -0.02222 -0.00300 0.01393 AFIX 43 H14 2 1.081735 0.123510 0.953814 11.00000 -1.20000 AFIX 0 C15 1 0.958214 0.250095 0.969675 11.00000 0.04361 0.32949 = 0.07774 -0.09065 -0.01409 0.04368 AFIX 43 H15 2 0.991775 0.290334 1.019723 11.00000 -1.20000 AFIX 0 C16 1 0.852653 0.281675 0.935830 11.00000 0.04140 0.17056 = 0.06085 -0.03434 -0.00424 0.01059 AFIX 43 H16 2 0.811604 0.340090 0.964908 11.00000 -1.20000 AFIX 0 C18 1 0.637227 0.015359 0.794451 11.00000 0.03497 0.07887 = 0.03700 -0.01468 0.00833 0.00124 AFIX 43 H18 2 0.686025 0.005442 0.845223 11.00000 -1.20000 AFIX 0 C19 1 0.590847 -0.090213 0.752178 11.00000 0.05517 0.05609 = 0.04358 0.01233 0.00776 0.00801 AFIX 43 H19 2 0.607311 -0.170070 0.773891 11.00000 -1.20000 AFIX 0 C36 1 0.763935 0.078113 0.513176 11.00000 0.17012 0.04998 = 0.08291 -0.03913 0.08030 -0.06462 AFIX 43 H36 2 0.754876 -0.001128 0.488200 11.00000 -1.20000 AFIX 0 C42 1 0.735557 0.735935 0.421221 11.00000 0.06695 0.05897 = 0.07036 0.03163 -0.03792 -0.03878 AFIX 43 H42 2 0.723245 0.795442 0.376450 11.00000 -1.20000 AFIX 0 C43 1 0.689604 0.751106 0.497369 11.00000 0.04990 0.04238 = 0.07267 0.01481 -0.01442 -0.01820 AFIX 43 H43 2 0.645260 0.820655 0.505322 11.00000 -1.20000 AFIX 0 MOLE 1 C1 1 0.602441 0.278231 0.918805 11.00000 0.02624 0.04590 = 0.03126 -0.00548 0.00169 -0.01101 C2 1 0.599802 0.379668 0.973205 11.00000 0.02908 0.04030 = 0.03388 0.00485 0.00264 -0.00552 AFIX 43 H2 2 0.629190 0.457876 0.961902 11.00000 -1.20000 AFIX 0 C3 1 0.546919 0.348526 1.047487 11.00000 0.03027 0.03360 = 0.02872 0.00374 0.00011 0.00375 AFIX 43 H3 2 0.535809 0.401778 1.094702 11.00000 -1.20000 AFIX 0 C4 1 0.513049 0.225416 1.040524 11.00000 0.02489 0.02555 = 0.03389 0.00724 0.00484 -0.00329 AFIX 43 H4 2 0.475178 0.180818 1.081444 11.00000 -1.20000 AFIX 0 C5 1 0.546573 0.181271 0.960531 11.00000 0.03028 0.02306 = 0.05648 -0.00523 -0.00340 -0.00166 AFIX 43 H5 2 0.534309 0.101029 0.938028 11.00000 -1.20000 AFIX 0 C6 1 0.362134 0.337271 0.815324 11.00000 0.03128 0.05028 = 0.03609 0.00038 -0.00719 -0.00824 AFIX 43 H6 2 0.390077 0.319393 0.761108 11.00000 -1.20000 AFIX 0 C7 1 0.363451 0.455371 0.860422 11.00000 0.03266 0.05061 = 0.04287 0.00345 -0.01166 -0.00574 AFIX 43 H7 2 0.391492 0.529870 0.839722 11.00000 -1.20000 AFIX 0 C8 1 0.316062 0.439603 0.939681 11.00000 0.03299 0.03826 = 0.04395 0.00552 -0.00880 0.00089 AFIX 43 H8 2 0.307971 0.501015 0.982337 11.00000 -1.20000 AFIX 0 C9 1 0.282330 0.315067 0.944615 11.00000 0.02440 0.06425 = 0.02964 0.00712 -0.00132 0.00082 AFIX 43 H9 2 0.246985 0.278684 0.990632 11.00000 -1.20000 AFIX 0 C10 1 0.310975 0.256581 0.869139 11.00000 0.03309 0.03391 = 0.04497 -0.00104 -0.00764 -0.00900 C11 1 0.808990 0.227147 0.859948 11.00000 0.03321 0.07017 = 0.04628 -0.01123 0.00346 -0.01236 C12 1 0.872342 0.140430 0.816825 11.00000 0.03319 0.07799 = 0.04693 -0.01885 0.01121 -0.01890 AFIX 43 H12 2 0.841506 0.104149 0.764271 11.00000 -1.20000 AFIX 0 C17 1 0.613550 0.131800 0.764007 11.00000 0.02633 0.05381 = 0.03363 -0.00155 0.01050 -0.00237 C20 1 0.519898 -0.071955 0.677236 11.00000 0.03494 0.03752 = 0.04926 -0.00087 -0.00109 -0.00319 AFIX 43 H20 2 0.485375 -0.140512 0.648712 11.00000 -1.20000 AFIX 0 C21 1 0.499746 0.040837 0.644914 11.00000 0.03678 0.03892 = 0.04298 0.00127 -0.01113 -0.00179 AFIX 43 H21 2 0.452749 0.051248 0.593175 11.00000 -1.20000 AFIX 0 C22 1 0.548065 0.143178 0.687530 11.00000 0.03497 0.04724 = 0.03811 -0.00928 0.00330 -0.00842 AFIX 43 H22 2 0.535216 0.222153 0.662950 11.00000 -1.20000 AFIX 0 C23 1 0.936208 0.471242 0.680525 11.00000 0.01875 0.02088 = 0.04182 -0.00620 -0.00281 0.00689 C24 1 1.027526 0.472609 0.630528 11.00000 0.03659 0.03169 = 0.02952 0.00060 0.00452 0.00433 AFIX 43 H24 2 1.025459 0.467827 0.568772 11.00000 -1.20000 AFIX 0 C25 1 1.122869 0.482416 0.689244 11.00000 0.03182 0.03714 = 0.05647 0.00974 0.00773 0.00740 AFIX 43 H25 2 1.195462 0.486804 0.673071 11.00000 -1.20000 AFIX 0 C26 1 1.092199 0.484550 0.774895 11.00000 0.02131 0.04859 = 0.04400 0.01138 -0.00234 0.00368 AFIX 43 H26 2 1.140332 0.488418 0.826490 11.00000 -1.20000 AFIX 0 C27 1 0.975171 0.479863 0.771039 11.00000 0.03551 0.03790 = 0.02819 -0.00074 0.00220 -0.00389 AFIX 43 H27 2 0.931883 0.482053 0.819194 11.00000 -1.20000 AFIX 0 C28 1 0.922911 0.780959 0.693894 11.00000 0.03617 0.03301 = 0.05521 -0.00209 -0.00212 0.00032 AFIX 43 H28 2 0.845574 0.781025 0.691112 11.00000 -1.20000 AFIX 0 C29 1 0.986442 0.775798 0.621710 11.00000 0.04259 0.02997 = 0.04818 -0.00983 -0.00915 0.00397 AFIX 43 H29 2 0.958825 0.773535 0.562156 11.00000 -1.20000 AFIX 0 C30 1 1.094966 0.774593 0.652004 11.00000 0.03759 0.03055 = 0.05504 0.00267 0.00778 -0.00212 AFIX 43 H30 2 1.154486 0.771336 0.616725 11.00000 -1.20000 AFIX 0 C31 1 1.103285 0.778959 0.743421 11.00000 0.04346 0.03715 = 0.06323 -0.01361 -0.01757 -0.01104 C32 1 0.993954 0.785987 0.770648 11.00000 0.04513 0.04259 = 0.03541 -0.01276 0.00094 -0.00117 AFIX 43 H32 2 0.974021 0.792665 0.828727 11.00000 -1.20000 AFIX 0 C33 1 0.790176 0.307825 0.587879 11.00000 0.05708 0.02777 = 0.03111 -0.01606 0.02371 -0.01129 C34 1 0.869652 0.221380 0.604625 11.00000 0.08353 0.01903 = 0.04764 -0.01139 0.02643 -0.01417 AFIX 43 H34 2 0.933336 0.240078 0.641508 11.00000 -1.20000 AFIX 0 C35 1 0.856142 0.104156 0.566589 11.00000 0.17118 0.02794 = 0.08757 -0.01083 0.07647 -0.00675 AFIX 43 H35 2 0.910727 0.043442 0.577930 11.00000 -1.20000 AFIX 0 C37 1 0.685976 0.163607 0.495675 11.00000 0.11182 0.09930 = 0.07328 -0.05651 0.05312 -0.08194 AFIX 43 H37 2 0.623211 0.143349 0.458196 11.00000 -1.20000 AFIX 0 C38 1 0.695154 0.279228 0.530734 11.00000 0.06205 0.06497 = 0.05311 -0.01868 0.01723 -0.03690 AFIX 43 H38 2 0.640003 0.338770 0.517494 11.00000 -1.20000 AFIX 0 C39 1 0.771383 0.565843 0.551402 11.00000 0.03513 0.03897 = 0.03156 -0.00111 -0.00218 -0.01253 C40 1 0.816894 0.548562 0.473898 11.00000 0.05101 0.04018 = 0.03870 -0.00470 -0.00581 -0.01765 AFIX 43 H40 2 0.859493 0.477585 0.466036 11.00000 -1.20000 AFIX 0 C41 1 0.801425 0.633240 0.407227 11.00000 0.07183 0.09773 = 0.02856 -0.00003 -0.01030 -0.04037 AFIX 43 H41 2 0.833919 0.622725 0.353949 11.00000 -1.20000 AFIX 0 C44 1 0.706665 0.667035 0.562703 11.00000 0.03846 0.02919 = 0.06201 0.00766 -0.01450 -0.01124 AFIX 43 H44 2 0.674106 0.678019 0.615907 11.00000 -1.20000 AFIX 0 P1 3 0.671059 0.270167 0.818402 11.00000 0.02810 0.06648 = 0.04137 -0.01680 0.00590 -0.00912 P2 3 0.795102 0.455381 0.641315 11.00000 0.03185 0.02819 = 0.02986 -0.00551 -0.00216 -0.00093 FE1 4 0.445873 0.323339 0.935168 11.00000 0.02502 0.04030 = 0.02828 0.00381 0.00059 -0.00243 FE2 4 1.021975 0.629104 0.702913 11.00000 0.02615 0.02841 = 0.02941 -0.00018 -0.00117 -0.00017 NI1 5 0.666425 0.467088 0.742737 11.00000 0.02840 0.03915 = 0.03062 -0.00381 -0.00157 0.00938 BR1 6 0.734274 0.614434 0.845358 11.00000 0.03712 0.03595 = 0.03483 -0.00558 0.01038 -0.00033 BR2 6 0.503044 0.483909 0.651806 11.00000 0.03085 0.04325 = 0.05053 0.01685 -0.00850 -0.00119 BR3 6 0.284441 0.090984 0.839558 11.00000 0.04060 0.04519 = 0.05292 0.00236 -0.00535 -0.00900 BR4 6 1.231687 0.784798 0.819044 11.00000 0.05453 0.06300 = 0.10048 -0.01234 -0.03503 -0.01261 HKLF 4 Covalent radii and connectivity table for 2005src1384 in P2(1) C 0.770 H 0.320 P 1.100 FE 1.240 NI 1.250 BR 1.140 C13 - C14 C12 C14 - C13 C15 C15 - C16 C14 C16 - C11 C15 C18 - C17 C19 C19 - C20 C18 C36 - C37 C35 C42 - C43 C41 C43 - C42 C44 C1 - C2 C5 P1 Fe1 C2 - C1 C3 Fe1 C3 - C2 C4 Fe1 C4 - C3 C5 Fe1 C5 - C4 C1 Fe1 C6 - C10 C7 Fe1 C7 - C8 C6 Fe1 C8 - C7 C9 Fe1 C9 - C10 C8 Fe1 C10 - C6 C9 Br3 Fe1 C11 - C16 C12 P1 C12 - C13 C11 C17 - C22 C18 P1 C20 - C21 C19 C21 - C20 C22 C22 - C17 C21 C23 - C24 C27 P2 Fe2 C24 - C23 C25 Fe2 C25 - C26 C24 Fe2 C26 - C25 C27 Fe2 C27 - C23 C26 Fe2 C28 - C32 C29 Fe2 C29 - C30 C28 Fe2 C30 - C29 C31 Fe2 C31 - C30 C32 Br4 Fe2 C32 - C28 C31 Fe2 C33 - C34 C38 P2 C34 - C33 C35 C35 - C36 C34 C37 - C36 C38 C38 - C37 C33 C39 - C40 C44 P2 C40 - C39 C41 C41 - C40 C42 C44 - C43 C39 P1 - C11 C1 C17 Ni1 P2 - C23 C33 C39 Ni1 Fe1 - C5 C10 C1 C2 C9 C6 C8 C4 C7 C3 Fe2 - C31 C30 C23 C24 C27 C25 C32 C29 C28 C26 Ni1 - P2 Br2 Br1 P1 Br1 - Ni1 Br2 - Ni1 Br3 - C10 Br4 - C31 Floating origin restraints generated 24584 Reflections read, of which 32 rejected -15 =< h =< 13, -13 =< k =< 14, -19 =< l =< 19, Max. 2-theta = 55.00 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) -12 0 5 112.19 5.93 2 36.79 -8 -9 6 0.94 0.93 2 6.28 -8 2 9 21.53 2.06 2 11.72 3 Inconsistent equivalents 9182 Unique reflections, of which 0 suppressed R(int) = 0.0500 R(sigma) = 0.0724 Friedel opposites not merged Maximum memory for data reduction = 4431 / 90491 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 = 5752 / 628992 wR2 = 0.1436 before cycle 1 for 9182 data and 478 / 478 parameters GooF = S = 1.026; Restrained GooF = 1.026 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0637 * P )^2 + 6.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.41419 0.00067 0.009 OSF Mean shift/su = 0.013 Maximum = 0.118 for U22 C16 Max. shift = 0.002 A for C16 Max. dU = 0.001 for C15 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5752 / 628992 wR2 = 0.1436 before cycle 2 for 9182 data and 478 / 478 parameters GooF = S = 1.026; Restrained GooF = 1.026 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0637 * P )^2 + 6.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.41419 0.00067 0.008 OSF Mean shift/su = 0.008 Maximum = 0.152 for U22 C16 Max. shift = 0.002 A for C15 Max. dU = 0.001 for C15 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5752 / 628992 wR2 = 0.1436 before cycle 3 for 9182 data and 478 / 478 parameters GooF = S = 1.027; Restrained GooF = 1.027 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0637 * P )^2 + 6.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.41421 0.00067 0.023 OSF Mean shift/su = 0.005 Maximum = 0.137 for U22 C16 Max. shift = 0.002 A for C16 Max. dU = 0.001 for C15 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5752 / 628992 wR2 = 0.1436 before cycle 4 for 9182 data and 478 / 478 parameters GooF = S = 1.027; Restrained GooF = 1.026 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0637 * P )^2 + 6.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.41421 0.00067 0.011 OSF Mean shift/su = 0.004 Maximum = 0.123 for U22 C16 Max. shift = 0.001 A for C16 Max. dU = 0.001 for C16 Least-squares cycle 5 Maximum vector length = 511 Memory required = 5752 / 628992 wR2 = 0.1436 before cycle 5 for 9182 data and 478 / 478 parameters GooF = S = 1.026; Restrained GooF = 1.026 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0637 * P )^2 + 6.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.41422 0.00067 0.008 OSF Mean shift/su = 0.003 Maximum = 0.110 for U22 C16 Max. shift = 0.001 A for C16 Max. dU = 0.001 for C16 Least-squares cycle 6 Maximum vector length = 511 Memory required = 5752 / 628992 wR2 = 0.1436 before cycle 6 for 9182 data and 478 / 478 parameters GooF = S = 1.027; Restrained GooF = 1.027 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0637 * P )^2 + 6.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.41422 0.00067 0.008 OSF Mean shift/su = 0.003 Maximum = 0.099 for U22 C16 Max. shift = 0.001 A for C16 Max. dU = 0.001 for C16 Least-squares cycle 7 Maximum vector length = 511 Memory required = 5752 / 628992 wR2 = 0.1436 before cycle 7 for 9182 data and 478 / 478 parameters GooF = S = 1.026; Restrained GooF = 1.026 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0637 * P )^2 + 6.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.41423 0.00067 0.004 OSF Mean shift/su = 0.002 Maximum = 0.090 for U22 C16 Max. shift = 0.001 A for C16 Max. dU = 0.001 for C16 Least-squares cycle 8 Maximum vector length = 511 Memory required = 5752 / 628992 wR2 = 0.1436 before cycle 8 for 9182 data and 478 / 478 parameters GooF = S = 1.026; Restrained GooF = 1.026 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0637 * P )^2 + 6.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.41423 0.00067 0.002 OSF Mean shift/su = 0.002 Maximum = 0.081 for U22 C16 Max. shift = 0.001 A for C16 Max. dU = 0.000 for C16 Least-squares cycle 9 Maximum vector length = 511 Memory required = 5752 / 628992 wR2 = 0.1436 before cycle 9 for 9182 data and 478 / 478 parameters GooF = S = 1.026; Restrained GooF = 1.026 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0637 * P )^2 + 6.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.41423 0.00067 0.004 OSF Mean shift/su = 0.002 Maximum = 0.074 for U22 C16 Max. shift = 0.001 A for C16 Max. dU = 0.000 for C16 Least-squares cycle 10 Maximum vector length = 511 Memory required = 5752 / 628992 wR2 = 0.1436 before cycle 10 for 9182 data and 478 / 478 parameters GooF = S = 1.026; Restrained GooF = 1.026 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0637 * P )^2 + 6.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.41423 0.00067 0.005 OSF Mean shift/su = 0.002 Maximum = 0.067 for U22 C16 Max. shift = 0.001 A for C16 Max. dU = 0.000 for C16 Least-squares cycle 11 Maximum vector length = 511 Memory required = 5752 / 628992 wR2 = 0.1436 before cycle 11 for 9182 data and 478 / 478 parameters GooF = S = 1.026; Restrained GooF = 1.026 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0637 * P )^2 + 6.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.41424 0.00067 0.003 OSF Mean shift/su = 0.002 Maximum = 0.061 for U22 C16 Max. shift = 0.001 A for C16 Max. dU = 0.000 for C16 Least-squares cycle 12 Maximum vector length = 511 Memory required = 5752 / 628992 wR2 = 0.1436 before cycle 12 for 9182 data and 478 / 478 parameters GooF = S = 1.026; Restrained GooF = 1.026 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0637 * P )^2 + 6.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.41424 0.00067 0.002 OSF Mean shift/su = 0.001 Maximum = 0.056 for U22 C16 Max. shift = 0.001 A for C16 Max. dU = 0.000 for C16 Least-squares cycle 13 Maximum vector length = 511 Memory required = 5752 / 628992 wR2 = 0.1436 before cycle 13 for 9182 data and 478 / 478 parameters GooF = S = 1.027; Restrained GooF = 1.026 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0637 * P )^2 + 6.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.41424 0.00067 0.002 OSF Mean shift/su = 0.001 Maximum = 0.052 for U22 C16 Max. shift = 0.001 A for C16 Max. dU = 0.000 for C16 Least-squares cycle 14 Maximum vector length = 511 Memory required = 5752 / 628992 wR2 = 0.1436 before cycle 14 for 9182 data and 478 / 478 parameters GooF = S = 1.027; Restrained GooF = 1.026 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0637 * P )^2 + 6.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.41424 0.00067 0.002 OSF Mean shift/su = 0.001 Maximum = 0.047 for U22 C16 Max. shift = 0.001 A for C16 Max. dU = 0.000 for C16 Least-squares cycle 15 Maximum vector length = 511 Memory required = 5752 / 628992 wR2 = 0.1436 before cycle 15 for 9182 data and 478 / 478 parameters GooF = S = 1.027; Restrained GooF = 1.026 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0637 * P )^2 + 6.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.41424 0.00067 0.001 OSF Mean shift/su = 0.001 Maximum = 0.043 for U22 C16 Max. shift = 0.001 A for C16 Max. dU = 0.000 for C16 Least-squares cycle 16 Maximum vector length = 511 Memory required = 5752 / 628992 wR2 = 0.1436 before cycle 16 for 9182 data and 478 / 478 parameters GooF = S = 1.027; Restrained GooF = 1.027 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0637 * P )^2 + 6.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.41424 0.00067 0.001 OSF Mean shift/su = 0.001 Maximum = 0.040 for U22 C16 Max. shift = 0.000 A for C16 Max. dU = 0.000 for C16 Least-squares cycle 17 Maximum vector length = 511 Memory required = 5752 / 628992 wR2 = 0.1436 before cycle 17 for 9182 data and 478 / 478 parameters GooF = S = 1.027; Restrained GooF = 1.026 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0637 * P )^2 + 6.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.41424 0.00067 0.001 OSF Mean shift/su = 0.001 Maximum = 0.037 for U22 C16 Max. shift = 0.000 A for C16 Max. dU = 0.000 for C16 Least-squares cycle 18 Maximum vector length = 511 Memory required = 5752 / 628992 wR2 = 0.1436 before cycle 18 for 9182 data and 478 / 478 parameters GooF = S = 1.027; Restrained GooF = 1.026 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0637 * P )^2 + 6.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.41424 0.00067 0.001 OSF Mean shift/su = 0.001 Maximum = 0.034 for U22 C16 Max. shift = 0.000 A for C16 Max. dU = 0.000 for C16 Least-squares cycle 19 Maximum vector length = 511 Memory required = 5752 / 628992 wR2 = 0.1436 before cycle 19 for 9182 data and 478 / 478 parameters GooF = S = 1.027; Restrained GooF = 1.027 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0637 * P )^2 + 6.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.41424 0.00067 0.001 OSF Mean shift/su = 0.001 Maximum = 0.031 for U22 C16 Max. shift = 0.000 A for C16 Max. dU = 0.000 for C16 Least-squares cycle 20 Maximum vector length = 511 Memory required = 5752 / 628992 wR2 = 0.1436 before cycle 20 for 9182 data and 478 / 478 parameters GooF = S = 1.027; Restrained GooF = 1.027 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0637 * P )^2 + 6.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.41425 0.00067 0.002 OSF Mean shift/su = 0.001 Maximum = 0.029 for U22 C16 Max. shift = 0.000 A for C16 Max. dU = 0.000 for C16 Largest correlation matrix elements -0.649 U12 C37 / U22 C37 -0.592 y C37 / x C37 0.522 U12 C35 / U23 C35 -0.637 U12 C37 / U11 C37 0.582 z C36 / x C36 -0.516 U23 C15 / U33 C15 -0.636 U13 C37 / U23 C37 0.582 U13 C35 / U33 C35 -0.516 y C36 / x C36 0.635 U13 C36 / U33 C36 0.569 z C35 / x C35 0.508 U13 C37 / U11 C37 0.627 U12 C36 / U23 C36 -0.555 U23 C15 / U22 C15 0.508 U12 C37 / U23 C37 0.610 U13 C36 / U11 C36 -0.541 U12 C36 / U22 C36 0.598 U13 C35 / U11 C35 -0.541 U13 C36 / U23 C36 Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H13 1.0206 0.0530 0.8170 43 0.950 0.000 C13 C14 C12 H14 1.0819 0.1235 0.9538 43 0.950 0.000 C14 C13 C15 H15 0.9917 0.2898 1.0198 43 0.950 0.000 C15 C16 C14 H16 0.8110 0.3374 0.9660 43 0.950 0.000 C16 C11 C15 H18 0.6859 0.0055 0.8452 43 0.950 0.000 C18 C17 C19 H19 0.6073 -0.1700 0.7739 43 0.950 0.000 C19 C20 C18 H36 0.7547 -0.0012 0.4884 43 0.950 0.000 C36 C37 C35 H42 0.7232 0.7955 0.3765 43 0.950 0.000 C42 C43 C41 H43 0.6453 0.8207 0.5053 43 0.950 0.000 C43 C42 C44 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C2 ** H2 0.6292 0.4578 0.9618 43 0.950 0.000 C2 C1 C3 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C3 ** H3 0.5357 0.4019 1.0947 43 0.950 0.000 C3 C2 C4 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C4 ** H4 0.4752 0.1808 1.0814 43 0.950 0.000 C4 C3 C5 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C5 ** H5 0.5344 0.1010 0.9380 43 0.950 0.000 C5 C4 C1 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C6 ** H6 0.3900 0.3195 0.7611 43 0.950 0.000 C6 C10 C7 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C7 ** H7 0.3916 0.5298 0.8398 43 0.950 0.000 C7 C8 C6 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C8 ** H8 0.3079 0.5009 0.9823 43 0.950 0.000 C8 C7 C9 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C9 ** H9 0.2471 0.2786 0.9907 43 0.950 0.000 C9 C10 C8 H12 0.8415 0.1041 0.7643 43 0.950 0.000 C12 C13 C11 H20 0.4854 -0.1405 0.6487 43 0.950 0.000 C20 C21 C19 H21 0.4528 0.0512 0.5932 43 0.950 0.000 C21 C20 C22 H22 0.5352 0.2221 0.6629 43 0.950 0.000 C22 C17 C21 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C24 ** H24 1.0255 0.4679 0.5687 43 0.950 0.000 C24 C23 C25 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C25 ** H25 1.1955 0.4868 0.6731 43 0.950 0.000 C25 C26 C24 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C26 ** H26 1.1403 0.4884 0.8265 43 0.950 0.000 C26 C25 C27 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C27 ** H27 0.9319 0.4821 0.8192 43 0.950 0.000 C27 C23 C26 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C28 ** H28 0.8456 0.7810 0.6911 43 0.950 0.000 C28 C32 C29 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C29 ** H29 0.9588 0.7734 0.5622 43 0.950 0.000 C29 C30 C28 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C30 ** H30 1.1545 0.7713 0.6167 43 0.950 0.000 C30 C29 C31 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C32 ** H32 0.9740 0.7927 0.8287 43 0.950 0.000 C32 C28 C31 H34 0.9334 0.2400 0.6415 43 0.950 0.000 C34 C33 C35 H35 0.9108 0.0434 0.5780 43 0.950 0.000 C35 C36 C34 H37 0.6231 0.1439 0.4580 43 0.950 0.000 C37 C36 C38 H38 0.6401 0.3387 0.5175 43 0.950 0.000 C38 C37 C33 H40 0.8596 0.4777 0.4660 43 0.950 0.000 C40 C39 C41 H41 0.8339 0.6228 0.3539 43 0.950 0.000 C41 C40 C42 H44 0.6740 0.6781 0.6159 43 0.950 0.000 C44 C43 C39 2005src1384 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C13 0.97765 0.10652 0.84856 1.00000 0.04135 0.10691 0.06458 -0.00433 0.01312 -0.01958 0.07045 0.02098 0.00083 0.00144 0.00071 0.00000 0.00525 0.00994 0.00659 0.00712 0.00477 0.00631 0.00330 H13 1.02056 0.05295 0.81700 1.00000 0.08454 0.00000 0.00000 C14 1.01528 0.15380 0.92630 1.00000 0.03272 0.20294 0.07176 -0.02288 -0.00307 0.01361 0.10291 0.02687 0.00091 0.00194 0.00087 0.00000 0.00548 0.01911 0.00803 0.01022 0.00541 0.00843 0.00602 H14 1.08190 0.12348 0.95379 1.00000 0.12350 0.00000 0.00000 C15 0.95810 0.24932 0.96982 1.00000 0.04318 0.34556 0.07892 -0.09537 -0.01433 0.04570 0.15702 0.03263 0.00108 0.00264 0.00099 0.00000 0.00700 0.03339 0.00960 0.01545 0.00663 0.01260 0.01144 H15 0.99166 0.28976 1.01978 1.00000 0.18843 0.00000 0.00000 C16 0.85245 0.28016 0.93631 1.00000 0.03897 0.19654 0.06328 -0.04801 -0.00556 0.01216 0.10018 0.02479 0.00093 0.00194 0.00078 0.00000 0.00579 0.01876 0.00737 0.01015 0.00521 0.00865 0.00610 H16 0.81097 0.33743 0.96603 1.00000 0.12021 0.00000 0.00000 C18 0.63718 0.01544 0.79444 1.00000 0.03473 0.07936 0.03674 -0.01481 0.00823 0.00088 0.04998 0.01758 0.00077 0.00104 0.00061 0.00000 0.00471 0.00749 0.00465 0.00456 0.00374 0.00455 0.00250 H18 0.68594 0.00555 0.84524 1.00000 0.05998 0.00000 0.00000 C19 0.59085 -0.09015 0.75217 1.00000 0.05520 0.05614 0.04351 0.01244 0.00781 0.00801 0.05141 0.01931 0.00086 0.00100 0.00061 0.00000 0.00612 0.00634 0.00530 0.00467 0.00454 0.00491 0.00245 H19 0.60734 -0.17000 0.77388 1.00000 0.06170 0.00000 0.00000 C36 0.76391 0.07805 0.51324 1.00000 0.17023 0.05062 0.08233 -0.03887 0.07963 -0.06552 0.09707 0.02802 0.00172 0.00130 0.00096 0.00000 0.01679 0.00789 0.00933 0.00728 0.01118 0.00985 0.00642 H36 0.75474 -0.00124 0.48836 1.00000 0.11648 0.00000 0.00000 C42 0.73557 0.73598 0.42122 1.00000 0.06687 0.05925 0.07048 0.03186 -0.03781 -0.03865 0.06807 0.01789 0.00099 0.00112 0.00081 0.00000 0.00711 0.00718 0.00745 0.00597 0.00609 0.00604 0.00372 H42 0.72324 0.79549 0.37645 1.00000 0.08169 0.00000 0.00000 C43 0.68965 0.75110 0.49733 1.00000 0.04975 0.04281 0.07289 0.01473 -0.01450 -0.01800 0.05630 0.01747 0.00086 0.00098 0.00074 0.00000 0.00573 0.00546 0.00728 0.00509 0.00521 0.00453 0.00274 H43 0.64533 0.82068 0.50525 1.00000 0.06756 0.00000 0.00000 C1 0.60243 0.27823 0.91882 1.00000 0.02621 0.04593 0.03126 -0.00544 0.00161 -0.01095 0.03452 0.01296 0.00059 0.00079 0.00049 0.00000 0.00370 0.00472 0.00378 0.00349 0.00301 0.00343 0.00173 C2 0.59981 0.37966 0.97318 1.00000 0.02899 0.04046 0.03376 0.00478 0.00256 -0.00543 0.03441 0.01454 0.00065 0.00080 0.00051 0.00000 0.00399 0.00446 0.00404 0.00344 0.00325 0.00330 0.00173 H2 0.62921 0.45785 0.96185 1.00000 0.04130 0.00000 0.00000 C3 0.54688 0.34860 1.04753 1.00000 0.03029 0.03357 0.02871 0.00394 0.00007 0.00383 0.03100 0.01437 0.00064 0.00073 0.00050 0.00000 0.00404 0.00425 0.00386 0.00312 0.00310 0.00313 0.00167 H3 0.53575 0.40186 1.09473 1.00000 0.03720 0.00000 0.00000 C4 0.51306 0.22540 1.04051 1.00000 0.02495 0.02551 0.03369 0.00700 0.00467 -0.00367 0.02792 0.01354 0.00060 0.00067 0.00050 0.00000 0.00364 0.00375 0.00381 0.00304 0.00300 0.00294 0.00155 H4 0.47518 0.18077 1.08141 1.00000 0.03351 0.00000 0.00000 C5 0.54664 0.18128 0.96054 1.00000 0.03021 0.02304 0.05642 -0.00515 -0.00347 -0.00162 0.03698 0.01453 0.00066 0.00073 0.00059 0.00000 0.00409 0.00382 0.00525 0.00365 0.00369 0.00310 0.00187 H5 0.53444 0.10102 0.93804 1.00000 0.04437 0.00000 0.00000 C6 0.36212 0.33733 0.81533 1.00000 0.03131 0.05014 0.03613 0.00036 -0.00723 -0.00821 0.03978 0.01444 0.00067 0.00087 0.00055 0.00000 0.00417 0.00511 0.00426 0.00385 0.00335 0.00376 0.00192 H6 0.39002 0.31950 0.76110 1.00000 0.04774 0.00000 0.00000 C7 0.36349 0.45529 0.86044 1.00000 0.03247 0.05074 0.04280 0.00349 -0.01148 -0.00578 0.04286 0.01547 0.00068 0.00094 0.00056 0.00000 0.00425 0.00545 0.00452 0.00415 0.00351 0.00387 0.00205 H7 0.39160 0.52978 0.83978 1.00000 0.05143 0.00000 0.00000 C8 0.31606 0.43951 0.93963 1.00000 0.03293 0.03844 0.04368 0.00530 -0.00868 0.00089 0.03905 0.01525 0.00067 0.00080 0.00056 0.00000 0.00427 0.00462 0.00466 0.00370 0.00358 0.00338 0.00193 H8 0.30790 0.50095 0.98226 1.00000 0.04686 0.00000 0.00000 C9 0.28239 0.31504 0.94462 1.00000 0.02442 0.06440 0.02956 0.00727 -0.00124 0.00077 0.03967 0.01547 0.00063 0.00094 0.00051 0.00000 0.00366 0.00587 0.00390 0.00405 0.00308 0.00391 0.00196 H9 0.24711 0.27864 0.99067 1.00000 0.04760 0.00000 0.00000 C10 0.31098 0.25660 0.86913 1.00000 0.03313 0.03376 0.04503 -0.00101 -0.00765 -0.00904 0.03795 0.01408 0.00066 0.00081 0.00056 0.00000 0.00428 0.00429 0.00469 0.00371 0.00357 0.00342 0.00187 C11 0.80899 0.22696 0.85995 1.00000 0.03330 0.07093 0.04649 -0.01150 0.00350 -0.01248 0.05024 0.01672 0.00075 0.00104 0.00064 0.00000 0.00472 0.00684 0.00521 0.00483 0.00398 0.00454 0.00244 C12 0.87234 0.14036 0.81687 1.00000 0.03316 0.07825 0.04703 -0.01893 0.01125 -0.01902 0.05236 0.01630 0.00070 0.00105 0.00062 0.00000 0.00443 0.00733 0.00495 0.00489 0.00379 0.00472 0.00256 H12 0.84152 0.10412 0.76429 1.00000 0.06283 0.00000 0.00000 C17 0.61356 0.13177 0.76399 1.00000 0.02633 0.05380 0.03371 -0.00142 0.01044 -0.00205 0.03749 0.01505 0.00061 0.00089 0.00051 0.00000 0.00374 0.00528 0.00391 0.00396 0.00308 0.00381 0.00182 C20 0.51991 -0.07190 0.67724 1.00000 0.03487 0.03764 0.04907 -0.00089 -0.00117 -0.00305 0.04080 0.01620 0.00073 0.00083 0.00060 0.00000 0.00456 0.00477 0.00505 0.00393 0.00388 0.00355 0.00201 H20 0.48537 -0.14047 0.64874 1.00000 0.04896 0.00000 0.00000 C21 0.49977 0.04082 0.64491 1.00000 0.03672 0.03894 0.04293 0.00123 -0.01123 -0.00174 0.04038 0.01551 0.00072 0.00083 0.00059 0.00000 0.00473 0.00470 0.00472 0.00374 0.00379 0.00354 0.00200 H21 0.45280 0.05122 0.59315 1.00000 0.04846 0.00000 0.00000 C22 0.54804 0.14312 0.68750 1.00000 0.03482 0.04738 0.03814 -0.00940 0.00329 -0.00856 0.04010 0.01442 0.00067 0.00088 0.00054 0.00000 0.00427 0.00534 0.00440 0.00386 0.00348 0.00384 0.00199 H22 0.53517 0.22210 0.66292 1.00000 0.04812 0.00000 0.00000 C23 0.93617 0.47124 0.68052 1.00000 0.01871 0.02113 0.04162 -0.00633 -0.00278 0.00693 0.02747 0.01252 0.00054 0.00068 0.00048 0.00000 0.00314 0.00343 0.00394 0.00330 0.00279 0.00292 0.00148 C24 1.02757 0.47267 0.63050 1.00000 0.03663 0.03161 0.02954 0.00071 0.00456 0.00416 0.03250 0.01430 0.00063 0.00076 0.00048 0.00000 0.00410 0.00409 0.00364 0.00347 0.00305 0.00363 0.00161 H24 1.02553 0.46794 0.56874 1.00000 0.03899 0.00000 0.00000 C25 1.12288 0.48243 0.68926 1.00000 0.03166 0.03724 0.05644 0.00980 0.00756 0.00718 0.04156 0.01647 0.00067 0.00084 0.00058 0.00000 0.00404 0.00453 0.00518 0.00432 0.00363 0.00381 0.00192 H25 1.19548 0.48680 0.67311 1.00000 0.04988 0.00000 0.00000 C26 1.09220 0.48453 0.77491 1.00000 0.02123 0.04874 0.04398 0.01145 -0.00233 0.00389 0.03828 0.01579 0.00060 0.00087 0.00055 0.00000 0.00353 0.00496 0.00436 0.00420 0.00311 0.00365 0.00184 H26 1.14033 0.48836 0.82651 1.00000 0.04594 0.00000 0.00000 C27 0.97518 0.47989 0.77103 1.00000 0.03538 0.03790 0.02808 -0.00081 0.00222 -0.00390 0.03382 0.01367 0.00063 0.00079 0.00047 0.00000 0.00399 0.00431 0.00354 0.00357 0.00298 0.00366 0.00163 H27 0.93190 0.48212 0.81919 1.00000 0.04058 0.00000 0.00000 C28 0.92294 0.78093 0.69390 1.00000 0.03614 0.03281 0.05543 -0.00215 -0.00211 0.00013 0.04181 0.01533 0.00072 0.00079 0.00059 0.00000 0.00449 0.00445 0.00533 0.00396 0.00393 0.00357 0.00201 H28 0.84560 0.78102 0.69112 1.00000 0.05018 0.00000 0.00000 C29 0.98642 0.77573 0.62171 1.00000 0.04278 0.03004 0.04819 -0.00976 -0.00917 0.00396 0.04110 0.01489 0.00072 0.00078 0.00060 0.00000 0.00472 0.00432 0.00496 0.00381 0.00388 0.00358 0.00201 H29 0.95880 0.77342 0.56216 1.00000 0.04932 0.00000 0.00000 C30 1.09497 0.77457 0.65202 1.00000 0.03739 0.03072 0.05507 0.00262 0.00753 -0.00192 0.04085 0.01577 0.00071 0.00078 0.00061 0.00000 0.00449 0.00433 0.00535 0.00390 0.00389 0.00351 0.00195 H30 1.15450 0.77134 0.61674 1.00000 0.04903 0.00000 0.00000 C31 1.10326 0.77892 0.74344 1.00000 0.04336 0.03718 0.06352 -0.01389 -0.01734 -0.01104 0.04930 0.01413 0.00078 0.00087 0.00065 0.00000 0.00496 0.00501 0.00616 0.00452 0.00442 0.00394 0.00238 C32 0.99396 0.78597 0.77063 1.00000 0.04503 0.04258 0.03526 -0.01278 0.00097 -0.00111 0.04110 0.01451 0.00071 0.00082 0.00054 0.00000 0.00486 0.00495 0.00436 0.00378 0.00367 0.00390 0.00200 H32 0.97401 0.79267 0.82871 1.00000 0.04932 0.00000 0.00000 C33 0.79016 0.30783 0.58789 1.00000 0.05702 0.02789 0.03128 -0.01616 0.02369 -0.01125 0.03758 0.01440 0.00073 0.00074 0.00050 0.00000 0.00520 0.00410 0.00394 0.00337 0.00371 0.00380 0.00193 C34 0.86970 0.22133 0.60464 1.00000 0.08327 0.01924 0.04755 -0.01129 0.02634 -0.01410 0.04882 0.01772 0.00094 0.00073 0.00061 0.00000 0.00738 0.00406 0.00521 0.00365 0.00495 0.00430 0.00251 H34 0.93340 0.24004 0.64150 1.00000 0.05858 0.00000 0.00000 C35 0.85619 0.10414 0.56664 1.00000 0.16987 0.02798 0.08712 -0.01039 0.07562 -0.00638 0.09125 0.03115 0.00154 0.00105 0.00091 0.00000 0.01526 0.00550 0.00870 0.00596 0.01002 0.00745 0.00518 H35 0.91079 0.04343 0.57796 1.00000 0.10950 0.00000 0.00000 C37 0.68581 0.16396 0.49561 1.00000 0.11119 0.09848 0.07299 -0.05548 0.05197 -0.08125 0.09167 0.02099 0.00137 0.00156 0.00089 0.00000 0.01147 0.01111 0.00829 0.00832 0.00827 0.01023 0.00578 H37 0.62308 0.14390 0.45803 1.00000 0.11000 0.00000 0.00000 C38 0.69519 0.27916 0.53073 1.00000 0.06195 0.06564 0.05277 -0.01850 0.01718 -0.03717 0.05941 0.01659 0.00091 0.00108 0.00065 0.00000 0.00637 0.00703 0.00566 0.00528 0.00495 0.00565 0.00296 H38 0.64006 0.33875 0.51755 1.00000 0.07129 0.00000 0.00000 C39 0.77132 0.56584 0.55141 1.00000 0.03510 0.03893 0.03146 -0.00129 -0.00219 -0.01264 0.03546 0.01385 0.00069 0.00079 0.00051 0.00000 0.00431 0.00454 0.00397 0.00347 0.00325 0.00350 0.00181 C40 0.81692 0.54861 0.47389 1.00000 0.05103 0.04032 0.03845 -0.00458 -0.00580 -0.01758 0.04383 0.01453 0.00080 0.00085 0.00057 0.00000 0.00549 0.00492 0.00463 0.00382 0.00398 0.00400 0.00214 H40 0.85958 0.47768 0.46603 1.00000 0.05259 0.00000 0.00000 C41 0.80142 0.63333 0.40723 1.00000 0.07166 0.09711 0.02859 -0.00029 -0.01013 -0.03995 0.06663 0.01714 0.00097 0.00130 0.00059 0.00000 0.00697 0.00962 0.00448 0.00545 0.00437 0.00728 0.00342 H41 0.83392 0.62284 0.35395 1.00000 0.07995 0.00000 0.00000 C44 0.70659 0.66708 0.56274 1.00000 0.03850 0.02915 0.06165 0.00782 -0.01431 -0.01134 0.04418 0.01493 0.00072 0.00078 0.00066 0.00000 0.00469 0.00419 0.00578 0.00404 0.00420 0.00359 0.00217 H44 0.67400 0.67810 0.61593 1.00000 0.05302 0.00000 0.00000 P1 0.67107 0.27014 0.81841 1.00000 0.02804 0.06661 0.04138 -0.01690 0.00588 -0.00916 0.04518 0.00400 0.00018 0.00026 0.00015 0.00000 0.00106 0.00166 0.00122 0.00118 0.00092 0.00108 0.00059 P2 0.79511 0.45539 0.64132 1.00000 0.03187 0.02821 0.02984 -0.00551 -0.00214 -0.00092 0.03025 0.00338 0.00016 0.00018 0.00012 0.00000 0.00097 0.00100 0.00093 0.00079 0.00076 0.00079 0.00041 Fe1 0.44588 0.32333 0.93517 1.00000 0.02503 0.04033 0.02827 0.00383 0.00058 -0.00244 0.03131 0.00199 0.00009 0.00011 0.00007 0.00000 0.00053 0.00064 0.00054 0.00047 0.00043 0.00047 0.00025 Fe2 1.02198 0.62910 0.70291 1.00000 0.02616 0.02842 0.02941 -0.00023 -0.00118 -0.00019 0.02820 0.00182 0.00008 0.00010 0.00007 0.00000 0.00051 0.00055 0.00051 0.00045 0.00040 0.00043 0.00023 Ni1 0.66643 0.46710 0.74274 1.00000 0.02840 0.03912 0.03063 -0.00382 -0.00159 0.00938 0.03296 0.00179 0.00008 0.00010 0.00006 0.00000 0.00049 0.00058 0.00047 0.00044 0.00038 0.00045 0.00023 Br1 0.73428 0.61444 0.84536 1.00000 0.03711 0.03597 0.03482 -0.00559 0.01038 -0.00033 0.03555 0.00142 0.00006 0.00007 0.00005 0.00000 0.00041 0.00043 0.00038 0.00035 0.00031 0.00035 0.00019 Br2 0.50304 0.48391 0.65181 1.00000 0.03085 0.04326 0.05054 0.01684 -0.00852 -0.00121 0.04225 0.00153 0.00007 0.00008 0.00006 0.00000 0.00039 0.00048 0.00048 0.00041 0.00034 0.00037 0.00022 Br3 0.28444 0.09098 0.83955 1.00000 0.04063 0.04523 0.05295 0.00237 -0.00536 -0.00902 0.04682 0.00156 0.00007 0.00008 0.00006 0.00000 0.00048 0.00054 0.00052 0.00041 0.00038 0.00040 0.00024 Br4 1.23169 0.78481 0.81904 1.00000 0.05452 0.06296 0.10053 -0.01232 -0.03504 -0.01261 0.07510 0.00185 0.00010 0.00012 0.00009 0.00000 0.00063 0.00072 0.00091 0.00065 0.00061 0.00053 0.00038 Final Structure Factor Calculation for 2005src1384 in P2(1) Total number of l.s. parameters = 478 Maximum vector length = 511 Memory required = 5276 / 27090 wR2 = 0.1436 before cycle 21 for 9182 data and 2 / 478 parameters GooF = S = 1.027; Restrained GooF = 1.026 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0637 * P )^2 + 6.30 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0573 for 7441 Fo > 4sig(Fo) and 0.0767 for all 9182 data wR2 = 0.1436, GooF = S = 1.027, Restrained GooF = 1.026 for all data Flack x parameter = 0.0776 with su 0.0125 Expected values are 0 (within 3 su's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Occupancy sum of asymmetric unit = 53.00 for non-hydrogen and 36.00 for hydrogen atoms Principal mean square atomic displacements U 0.1128 0.0650 0.0335 C13 0.2085 0.0690 0.0312 C14 may be split into 1.0163 0.1706 0.9241 and 1.0143 0.1370 0.9285 0.3861 0.0494 0.0356 C15 may be split into 0.9608 0.2742 0.9638 and 0.9554 0.2244 0.9758 0.2141 0.0503 0.0361 C16 may be split into 0.8533 0.2977 0.9321 and 0.8516 0.2627 0.9405 0.0840 0.0385 0.0274 C18 0.0685 0.0499 0.0359 C19 0.2322 0.0382 0.0208 C36 may be split into 0.7794 0.0705 0.5192 and 0.7484 0.0856 0.5073 0.1474 0.0333 0.0235 C42 0.0961 0.0448 0.0279 C43 0.0516 0.0312 0.0208 C1 0.0448 0.0322 0.0262 C2 0.0366 0.0323 0.0242 C3 0.0377 0.0279 0.0182 C4 0.0596 0.0298 0.0215 C5 0.0547 0.0420 0.0227 C6 0.0595 0.0461 0.0229 C7 0.0537 0.0383 0.0252 C8 0.0659 0.0306 0.0225 C9 0.0536 0.0385 0.0218 C10 0.0780 0.0436 0.0291 C11 0.0930 0.0382 0.0259 C12 0.0541 0.0378 0.0206 C17 0.0510 0.0394 0.0320 C20 0.0565 0.0387 0.0260 C21 0.0554 0.0364 0.0285 C22 0.0461 0.0235 0.0128 C23 0.0392 0.0296 0.0288 C24 0.0614 0.0366 0.0267 C25 0.0581 0.0375 0.0192 C26 0.0407 0.0327 0.0280 C27 0.0579 0.0349 0.0326 C28 0.0634 0.0341 0.0257 C29 0.0557 0.0373 0.0296 C30 0.0805 0.0498 0.0175 C31 0.0524 0.0454 0.0255 C32 0.0728 0.0283 0.0117 C33 0.0949 0.0368 0.0147 C34 0.2006 0.0475 0.0256 C35 may be split into 0.8710 0.1031 0.5723 and 0.8414 0.1052 0.5610 0.2141 0.0399 0.0209 C37 may be split into 0.6976 0.1519 0.5010 and 0.6740 0.1761 0.4902 0.1076 0.0443 0.0264 C38 0.0504 0.0335 0.0225 C39 0.0658 0.0429 0.0228 C40 0.1279 0.0490 0.0230 C41 0.0773 0.0339 0.0213 C44 0.0764 0.0332 0.0260 P1 0.0374 0.0311 0.0222 P2 0.0421 0.0275 0.0244 Fe1 0.0321 0.0284 0.0241 Fe2 0.0469 0.0292 0.0228 Ni1 0.0446 0.0361 0.0260 Br1 0.0682 0.0350 0.0236 Br2 0.0620 0.0462 0.0323 Br3 0.1294 0.0700 0.0259 Br4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.033 0.049 0.063 0.078 0.094 0.114 0.140 0.181 0.254 1.000 Number in group 944. 908. 909. 946. 917. 907. 910. 902. 919. 920. GooF 0.978 1.003 1.043 1.079 1.062 0.984 1.080 1.038 1.002 0.991 K 1.602 1.171 1.019 1.018 1.003 1.008 0.996 1.009 1.016 1.008 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.66 inf Number in group 955. 880. 929. 922. 913. 915. 918. 913. 932. 905. GooF 0.990 1.003 0.975 0.987 0.998 0.968 0.902 0.936 0.986 1.431 K 1.009 1.070 1.023 1.023 1.011 1.020 1.025 1.015 1.014 1.000 R1 0.224 0.178 0.141 0.113 0.081 0.063 0.049 0.044 0.038 0.042 Recommended weighting scheme: WGHT 0.0628 6.4623 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/su Fc/Fc(max) Resolution(A) 3 0 1 2198.34 1112.06 7.01 0.138 3.87 4 0 3 681.68 255.98 6.48 0.066 2.54 3 -1 1 184.95 12.87 6.46 0.015 3.65 0 0 3 1884.65 3279.34 5.96 0.236 5.11 -12 9 5 47.96 462.98 5.69 0.089 0.77 6 0 4 509.48 225.22 4.84 0.062 1.74 6 1 2 2117.35 1370.56 4.51 0.153 1.91 4 11 3 195.65 459.50 4.35 0.089 0.92 2 0 1 2818.13 1858.74 4.26 0.178 5.53 -1 0 7 1693.78 1107.29 4.12 0.137 2.19 4 0 1 208.02 65.23 4.09 0.033 2.96 5 -8 10 669.93 1103.78 4.08 0.137 0.92 6 -1 2 1565.48 1030.89 4.01 0.133 1.91 -9 2 11 327.51 601.75 3.98 0.101 1.00 1 0 5 882.63 1355.09 3.90 0.152 2.92 -3 0 2 7785.78 5433.03 3.87 0.304 3.75 -1 0 4 246.38 483.19 3.84 0.091 3.75 0 0 4 4122.92 5632.70 3.79 0.310 3.83 -3 13 1 158.90 394.26 3.73 0.082 0.82 3 11 2 565.34 297.36 3.72 0.071 0.96 2 -1 1 795.03 1210.14 3.72 0.144 4.94 5 0 5 7973.40 5949.17 3.67 0.318 1.84 1 0 2 208.68 441.60 3.66 0.087 6.26 -2 -3 4 818.50 1230.68 3.62 0.145 2.48 -12 2 5 -37.40 217.51 3.58 0.061 0.98 1 10 7 29.79 221.17 3.58 0.061 0.97 -4 1 4 189.02 75.65 3.55 0.036 2.44 -2 -5 6 542.85 858.80 3.49 0.121 1.63 -2 2 5 1851.05 2549.80 3.42 0.208 2.52 -2 5 6 577.25 901.43 3.38 0.124 1.63 5 12 0 392.20 683.49 3.36 0.108 0.85 -2 3 4 936.14 1403.80 3.34 0.155 2.48 1 0 6 495.17 286.43 3.30 0.070 2.46 8 -8 2 504.09 265.67 3.29 0.067 1.00 -2 0 2 1286.17 1841.87 3.28 0.177 5.01 -4 11 6 323.12 584.49 3.27 0.100 0.89 -7 -8 12 12.46 251.85 3.26 0.066 0.85 5 -7 1 448.85 233.11 3.21 0.063 1.31 -3 -1 6 295.59 155.59 3.20 0.051 2.21 4 4 4 1224.21 858.06 3.18 0.121 1.76 1 11 4 2104.43 1455.31 3.17 0.157 0.96 3 3 4 2226.97 2952.16 3.13 0.224 2.16 -1 10 9 267.39 72.87 3.11 0.035 0.92 -2 -2 5 2041.37 2706.76 3.11 0.215 2.52 6 -8 9 296.66 142.67 3.10 0.049 0.92 2 3 1 44.76 186.63 3.08 0.056 3.04 10 6 7 101.30 334.41 3.07 0.075 0.90 -7 2 14 825.43 546.03 3.07 0.096 0.95 -4 0 5 3851.82 5005.37 3.06 0.292 2.27 11 -4 12 -79.25 315.90 3.06 0.073 0.77 Bond lengths and angles C13 - Distance Angles C14 1.3480 (0.0173) C12 1.3958 (0.0147) 116.52 (1.19) C13 - C14 C14 - Distance Angles C13 1.3480 (0.0172) C15 1.4546 (0.0247) 122.73 (1.24) C14 - C13 C15 - Distance Angles C16 1.3991 (0.0177) C14 1.4546 (0.0247) 118.37 (1.35) C15 - C16 C16 - Distance Angles C11 1.3772 (0.0153) C15 1.3991 (0.0178) 119.57 (1.39) C16 - C11 C18 - Distance Angles C17 1.3771 (0.0146) C19 1.4199 (0.0147) 121.96 (0.86) C18 - C17 C19 - Distance Angles C20 1.3996 (0.0131) C18 1.4199 (0.0147) 117.35 (0.93) C19 - C20 C36 - Distance Angles C37 1.3547 (0.0247) C35 1.3739 (0.0239) 120.84 (1.13) C36 - C37 C42 - Distance Angles C43 1.3542 (0.0177) C41 1.4116 (0.0189) 121.16 (0.97) C42 - C43 C43 - Distance Angles C42 1.3542 (0.0177) C44 1.3652 (0.0136) 120.48 (1.15) C43 - C42 C1 - Distance Angles C2 1.3906 (0.0117) C5 1.4433 (0.0116) 106.30 (0.68) P1 1.8267 (0.0079) 125.74 (0.61) 127.87 (0.63) Fe1 2.0273 (0.0077) 70.11 (0.47) 68.19 (0.44) 129.17 (0.42) C1 - C2 C5 P1 C2 - Distance Angles C1 1.3906 (0.0117) C3 1.4066 (0.0110) 109.49 (0.74) Fe1 2.0311 (0.0080) 69.81 (0.45) 70.99 (0.46) C2 - C1 C3 C3 - Distance Angles C2 1.4066 (0.0110) C4 1.4106 (0.0107) 108.82 (0.72) Fe1 2.0599 (0.0077) 68.79 (0.45) 69.80 (0.45) C3 - C2 C4 C4 - Distance Angles C3 1.4106 (0.0107) C5 1.4165 (0.0115) 106.55 (0.66) Fe1 2.0558 (0.0075) 70.11 (0.43) 67.66 (0.45) C4 - C3 C5 C5 - Distance Angles C4 1.4165 (0.0115) C1 1.4433 (0.0116) 108.83 (0.68) Fe1 2.0047 (0.0082) 71.54 (0.45) 69.86 (0.47) C5 - C4 C1 C6 - Distance Angles C10 1.3967 (0.0120) C7 1.4633 (0.0136) 105.22 (0.76) Fe1 2.0397 (0.0080) 68.62 (0.46) 69.69 (0.46) C6 - C10 C7 C7 - Distance Angles C8 1.4070 (0.0125) C6 1.4633 (0.0136) 108.32 (0.82) Fe1 2.0567 (0.0092) 69.61 (0.50) 68.45 (0.50) C7 - C8 C6 C8 - Distance Angles C7 1.4070 (0.0125) C9 1.4259 (0.0132) 107.94 (0.82) Fe1 2.0477 (0.0087) 70.30 (0.53) 69.03 (0.48) C8 - C7 C9 C9 - Distance Angles C10 1.3973 (0.0124) C8 1.4259 (0.0132) 107.20 (0.77) Fe1 2.0338 (0.0079) 68.81 (0.47) 70.08 (0.49) C9 - C10 C8 C10 - Distance Angles C6 1.3967 (0.0120) C9 1.3973 (0.0124) 111.30 (0.81) Br3 1.8877 (0.0087) 122.70 (0.67) 126.00 (0.69) Fe1 2.0085 (0.0078) 71.02 (0.46) 70.75 (0.47) 126.05 (0.46) C10 - C6 C9 Br3 C11 - Distance Angles C16 1.3772 (0.0153) C12 1.4261 (0.0142) 119.26 (1.01) P1 1.8250 (0.0103) 118.12 (0.89) 122.61 (0.71) C11 - C16 C12 C12 - Distance Angles C13 1.3958 (0.0148) C11 1.4261 (0.0142) 122.87 (0.93) C12 - C13 C17 - Distance Angles C22 1.3742 (0.0118) C18 1.3771 (0.0146) 117.78 (0.85) P1 1.8403 (0.0093) 119.35 (0.72) 122.80 (0.66) C17 - C22 C18 C20 - Distance Angles C21 1.3435 (0.0127) C19 1.3996 (0.0131) 121.19 (0.88) C20 - C21 C21 - Distance Angles C20 1.3435 (0.0127) C22 1.4020 (0.0120) 120.04 (0.79) C21 - C20 C22 - Distance Angles C17 1.3742 (0.0118) C21 1.4020 (0.0120) 121.50 (0.88) C22 - C17 C23 - Distance Angles C24 1.4180 (0.0105) C27 1.4369 (0.0102) 108.11 (0.62) P2 1.7980 (0.0069) 127.50 (0.57) 124.35 (0.56) Fe2 2.0368 (0.0075) 69.98 (0.45) 69.82 (0.44) 127.65 (0.39) C23 - C24 C27 P2 C24 - Distance Angles C23 1.4180 (0.0104) C25 1.4228 (0.0115) 107.83 (0.66) Fe2 2.0450 (0.0082) 69.36 (0.43) 69.86 (0.49) C24 - C23 C25 C25 - Distance Angles C26 1.4024 (0.0121) C24 1.4228 (0.0115) 108.91 (0.70) Fe2 2.0501 (0.0086) 71.08 (0.50) 69.48 (0.47) C25 - C26 C24 C26 - Distance Angles C25 1.4024 (0.0121) C27 1.4386 (0.0106) 108.11 (0.70) Fe2 2.0750 (0.0085) 69.17 (0.48) 68.57 (0.45) C26 - C25 C27 C27 - Distance Angles C23 1.4369 (0.0102) C26 1.4386 (0.0106) 107.01 (0.65) Fe2 2.0480 (0.0082) 68.99 (0.44) 70.59 (0.47) C27 - C23 C26 C28 - Distance Angles C32 1.4087 (0.0118) C29 1.4140 (0.0131) 108.34 (0.76) Fe2 2.0570 (0.0087) 69.71 (0.49) 69.84 (0.50) C28 - C32 C29 C29 - Distance Angles C30 1.3777 (0.0121) C28 1.4140 (0.0131) 108.73 (0.80) Fe2 2.0557 (0.0090) 68.74 (0.51) 69.94 (0.52) C29 - C30 C28 C30 - Distance Angles C29 1.3777 (0.0121) C31 1.4027 (0.0134) 108.88 (0.84) Fe2 2.0175 (0.0087) 71.73 (0.53) 68.50 (0.52) C30 - C29 C31 C31 - Distance Angles C30 1.4027 (0.0134) C32 1.4463 (0.0133) 107.65 (0.75) Br4 1.8823 (0.0086) 127.27 (0.77) 124.97 (0.72) Fe2 1.9909 (0.0085) 70.54 (0.49) 71.27 (0.49) 126.50 (0.54) C31 - C30 C32 Br4 C32 - Distance Angles C28 1.4087 (0.0118) C31 1.4463 (0.0133) 106.36 (0.75) Fe2 2.0508 (0.0085) 70.18 (0.48) 66.83 (0.47) C32 - C28 C31 C33 - Distance Angles C34 1.3699 (0.0139) C38 1.4363 (0.0136) 119.76 (0.82) P2 1.8085 (0.0076) 122.29 (0.69) 117.81 (0.77) C33 - C34 C38 C34 - Distance Angles C33 1.3699 (0.0138) C35 1.4116 (0.0142) 119.42 (1.22) C34 - C33 C35 - Distance Angles C36 1.3739 (0.0239) C34 1.4116 (0.0142) 119.86 (1.45) C35 - C36 C37 - Distance Angles C36 1.3547 (0.0247) C38 1.3709 (0.0177) 121.54 (1.41) C37 - C36 C38 - Distance Angles C37 1.3709 (0.0177) C33 1.4363 (0.0136) 118.57 (1.35) C38 - C37 C39 - Distance Angles C40 1.3749 (0.0127) C44 1.3835 (0.0128) 120.14 (0.86) P2 1.8403 (0.0085) 120.81 (0.73) 119.06 (0.65) C39 - C40 C44 C40 - Distance Angles C39 1.3749 (0.0127) C41 1.3828 (0.0146) 120.77 (1.03) C40 - C39 C41 - Distance Angles C40 1.3828 (0.0146) C42 1.4116 (0.0189) 117.59 (1.01) C41 - C40 C44 - Distance Angles C43 1.3652 (0.0136) C39 1.3835 (0.0128) 119.85 (1.01) C44 - C43 P1 - Distance Angles C11 1.8250 (0.0104) C1 1.8267 (0.0079) 101.60 (0.41) C17 1.8403 (0.0094) 104.91 (0.45) 103.68 (0.36) Ni1 2.4453 (0.0031) 112.16 (0.36) 111.52 (0.30) 120.94 (0.30) P1 - C11 C1 C17 P2 - Distance Angles C23 1.7980 (0.0070) C33 1.8085 (0.0077) 103.42 (0.38) C39 1.8403 (0.0085) 106.00 (0.37) 104.23 (0.38) Ni1 2.3223 (0.0022) 117.73 (0.25) 110.89 (0.26) 113.30 (0.29) P2 - C23 C33 C39 Fe1 - Distance Angles C5 2.0047 (0.0082) C10 2.0085 (0.0078) 106.79 (0.35) C1 2.0273 (0.0078) 41.95 (0.34) 127.11 (0.34) C2 2.0311 (0.0081) 68.38 (0.35) 165.19 (0.34) 40.08 (0.32) C9 2.0338 (0.0080) 123.50 (0.38) 40.44 (0.36) 163.07 (0.38) 153.97 (0.35) C6 2.0397 (0.0080) 119.38 (0.38) 40.36 (0.34) 108.57 (0.34) 128.64 (0.33) 68.98 (0.33) C8 2.0477 (0.0087) 161.04 (0.35) 68.14 (0.36) 155.37 (0.35) 120.99 (0.35) 40.89 (0.37) 69.41 (0.37) C4 2.0558 (0.0075) 40.81 (0.33) 117.98 (0.33) 69.44 (0.31) 68.18 (0.31) 104.72 (0.31) 152.85 (0.34) 123.96 (0.33) C7 2.0567 (0.0092) 156.79 (0.37) 67.97 (0.36) 121.99 (0.35) 110.61 (0.35) 68.12 (0.36) 41.86 (0.37) 40.10 (0.35) C3 2.0599 (0.0078) 67.75 (0.33) 152.48 (0.34) 67.95 (0.31) 40.21 (0.31) 118.43 (0.32) 166.09 (0.34) 107.80 (0.33) Fe1 - C5 C10 C1 C2 C9 C6 C8 Fe2 - Distance Angles C31 1.9909 (0.0085) C30 2.0175 (0.0088) 40.96 (0.40) C23 2.0368 (0.0075) 171.49 (0.37) 147.54 (0.34) C24 2.0450 (0.0082) 144.92 (0.38) 114.19 (0.34) 40.66 (0.30) C27 2.0480 (0.0083) 130.58 (0.37) 168.69 (0.33) 41.19 (0.30) 68.76 (0.31) C25 2.0501 (0.0086) 112.45 (0.38) 106.35 (0.35) 68.35 (0.31) 40.66 (0.33) 68.29 (0.34) C32 2.0508 (0.0085) 41.90 (0.39) 68.84 (0.37) 133.32 (0.32) 172.17 (0.33) 109.76 (0.33) 146.69 (0.35) C29 2.0557 (0.0091) 67.95 (0.37) 39.53 (0.35) 118.49 (0.32) 109.61 (0.32) 151.29 (0.34) 130.26 (0.36) 67.74 (0.35) C28 2.0570 (0.0087) 68.73 (0.38) 67.67 (0.36) 112.05 (0.29) 133.25 (0.33) 119.02 (0.35) 170.06 (0.36) 40.11 (0.34) C26 2.0750 (0.0085) 106.47 (0.37) 128.89 (0.34) 68.41 (0.32) 67.82 (0.34) 40.84 (0.30) 39.74 (0.34) 116.46 (0.36) Fe2 - C31 C30 C23 C24 C27 C25 C32 Ni1 - Distance Angles P2 2.3223 (0.0022) Br2 2.3572 (0.0012) 101.70 (0.06) Br1 2.3573 (0.0013) 105.36 (0.06) 125.43 (0.05) P1 2.4453 (0.0031) 106.40 (0.08) 109.57 (0.07) 106.84 (0.07) Ni1 - P2 Br2 Br1 Br1 - Distance Angles Ni1 2.3573 (0.0013) Br1 - Br2 - Distance Angles Ni1 2.3572 (0.0012) Br2 - Br3 - Distance Angles C10 1.8877 (0.0087) Br3 - Br4 - Distance Angles C31 1.8823 (0.0086) Br4 - FMAP and GRID set by program FMAP 2 3 35 GRID -1.563 -2 -2 1.563 2 2 R1 = 0.0692 for 4964 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 2.30 at 0.3120 0.7001 0.1600 [ 0.85 A from P1 ] Deepest hole -1.16 at 0.3488 0.8241 0.2003 [ 0.69 A from P1 ] Mean = 0.00, Rms deviation from mean = 0.14 e/A^3, Highest memory used = 4906 / 33614 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6880 0.2001 0.8400 1.00000 0.05 2.30 0.85 P1 1.52 C11 1.61 C17 1.88 C1 Q2 1 0.7042 0.3417 0.7752 1.00000 0.05 1.46 1.13 P1 1.52 NI1 2.16 C11 2.55 C17 Q3 1 0.4534 0.2481 0.9339 1.00000 0.05 1.23 0.83 FE1 1.39 C5 1.76 C4 1.89 H5 Q4 1 1.2108 0.8684 0.8195 1.00000 0.05 1.08 0.95 BR4 1.95 C31 2.60 BR3 2.86 C32 Q5 1 0.2083 0.4065 1.0048 1.00000 0.05 1.05 1.50 H9 1.66 H8 1.68 C9 1.77 C8 Q6 1 0.6835 0.5224 0.7203 1.00000 0.05 1.02 0.74 NI1 2.05 P2 2.21 BR1 2.34 H44 Q7 1 0.8515 0.1687 0.9710 1.00000 0.05 0.89 1.33 C16 1.58 C15 1.86 C11 1.91 H16 Q8 1 1.2713 0.7843 0.7619 1.00000 0.05 0.80 1.04 BR4 2.07 C31 2.55 H30 2.64 C30 Q9 1 0.8199 0.1524 0.8873 1.00000 0.05 0.76 0.92 C11 1.32 C12 1.62 C16 2.00 H12 Q10 1 0.4997 0.5593 0.6572 1.00000 0.05 0.62 0.83 BR2 2.41 H37 2.55 NI1 2.63 H44 Q11 1 0.9456 0.1204 1.0043 1.00000 0.05 0.61 1.52 C15 1.58 C14 1.91 H14 1.94 H15 Q12 1 0.7467 0.6754 0.8438 1.00000 0.05 0.59 0.68 BR1 2.58 H19 2.78 H9 2.88 NI1 Q13 1 0.9262 0.7252 0.3634 1.00000 0.05 0.56 1.59 H41 1.75 H34 2.00 C41 2.52 C34 Q14 1 1.0169 0.0715 0.9507 1.00000 0.05 0.56 0.97 C14 0.98 H14 1.65 C13 2.07 H13 Q15 1 0.8874 0.5978 0.2561 1.00000 0.05 0.54 1.72 H41 1.74 H13 2.41 C13 2.47 BR3 Q16 1 0.2808 0.2175 0.9232 1.00000 0.05 0.54 1.03 C10 1.12 C9 1.33 H9 1.89 BR3 Q17 1 0.6980 0.0373 0.8451 1.00000 0.05 0.49 0.38 H18 1.06 C18 1.87 C17 2.32 C19 Q18 1 0.5521 0.1229 0.9697 1.00000 0.05 0.48 0.57 H5 0.66 C5 1.66 C4 1.99 C1 Q19 1 0.8219 0.1556 0.5877 1.00000 0.05 0.48 0.79 C35 0.95 C34 1.55 C36 1.66 H35 Q20 1 0.5968 0.0782 0.7833 1.00000 0.05 0.47 0.70 C17 0.86 C18 1.60 H18 1.70 C22 Shortest distances between peaks (including symmetry equivalents) 7 9 1.32 7 11 1.34 11 14 1.36 4 8 1.52 17 20 1.57 1 17 1.79 1 9 1.80 1 2 1.86 3 18 1.88 1 20 1.91 9 17 2.02 3 16 2.14 2 6 2.15 13 15 2.18 9 11 2.30 7 14 2.34 6 10 2.42 6 12 2.60 5 16 2.62 9 14 2.69 1 7 2.74 1 18 2.84 5 17 2.87 17 18 2.90 7 17 2.96 4 15 2.97 2 9 2.98 5 7 2.99 Time profile in seconds ----------------------- 0.03: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 1.23: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 14.42: Structure factors and derivatives 52.83: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.17: Apply other restraints 3.41: Solve l.s. equations 0.00: Generate HTAB table 0.08: Other dependent quantities, CIF, tables 0.14: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.08: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2005src1384 finished at 12:50:40 Total CPU time: 72.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++