+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s94 started at 11:15:59 on 06-Oct-2003 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s94 in Pc CELL 0.71073 15.9575 8.8522 13.7492 90.000 101.905 90.000 ZERR 4.00 0.0004 0.0002 0.0003 0.000 0.001 0.000 LATT -1 SYMM X, - Y, 1/2 + Z SFAC C H O FE BR UNIT 96 56 8 4 8 V = 1900.42 F(000) = 1080.0 Mu = 5.02 mm-1 Cell Wt = 2200.09 Rho = 1.922 MERG 2 OMIT -3.00 55.00 EXTI 0.00173 SHEL 7 0.77 FMAP 2 PLAN 5 SIZE 0.01 0.12 0.26 ACTA BOND $H WGHT 0.03690 3.54100 L.S. 9 TEMP -153.00 FVAR 0.26905 MOLE 1 C1 1 0.999334 0.086362 0.043370 11.00000 0.02690 0.01568 = 0.02457 0.00628 0.00141 -0.00304 C2 1 1.058419 -0.004201 0.000388 11.00000 0.02385 0.01751 = 0.02090 0.00484 0.01036 0.00346 AFIX 43 H2 2 1.119182 0.001215 0.015395 11.00000 -1.20000 AFIX 0 C3 1 1.006174 -0.103434 -0.069337 11.00000 0.03591 0.02174 = 0.01659 0.00597 0.01243 0.00723 AFIX 43 H3 2 1.026679 -0.175313 -0.110147 11.00000 -1.20000 AFIX 0 C4 1 0.918219 -0.076560 -0.067420 11.00000 0.02861 0.02631 = 0.01936 0.00410 -0.00159 -0.00322 AFIX 43 H4 2 0.870557 -0.128402 -0.105856 11.00000 -1.20000 AFIX 0 C5 1 0.914278 0.041993 0.002424 11.00000 0.02276 0.02036 = 0.02285 0.00513 0.00541 0.00253 AFIX 43 H5 2 0.863788 0.083209 0.018302 11.00000 -1.20000 AFIX 0 C6 1 0.910290 -0.243082 0.155758 11.00000 0.02024 0.01747 = 0.01427 0.00180 0.00469 0.00010 C7 1 0.976743 -0.153576 0.217633 11.00000 0.02398 0.02038 = 0.01599 -0.00138 0.00336 -0.00363 AFIX 43 H7 2 0.968056 -0.073616 0.260569 11.00000 -1.20000 AFIX 0 C8 1 1.055984 -0.205949 0.202847 11.00000 0.01748 0.02291 = 0.02558 0.00588 0.00298 -0.00512 AFIX 43 H8 2 1.110320 -0.166464 0.233750 11.00000 -1.20000 AFIX 0 C9 1 1.042054 -0.326296 0.134922 11.00000 0.02694 0.02757 = 0.01446 0.00818 0.01139 0.00361 AFIX 43 H9 2 1.085528 -0.381726 0.112727 11.00000 -1.20000 AFIX 0 C10 1 0.953713 -0.351649 0.105051 11.00000 0.03229 0.01580 = 0.01404 -0.00102 0.00909 0.00100 AFIX 43 H10 2 0.927166 -0.426750 0.059616 11.00000 -1.20000 AFIX 0 C11 1 0.817308 -0.223601 0.141524 11.00000 0.02350 0.01533 = 0.01423 0.00302 0.00737 -0.00062 C12 1 0.780535 -0.130524 0.204570 11.00000 0.02166 0.01957 = 0.02104 0.00380 0.00223 0.00289 AFIX 43 H12 2 0.816733 -0.077213 0.256895 11.00000 -1.20000 AFIX 0 C13 1 0.693666 -0.115555 0.191783 11.00000 0.02194 0.01729 = 0.01697 -0.00117 0.00509 -0.00104 C14 1 0.656850 -0.017189 0.261127 11.00000 0.01509 0.02261 = 0.02262 -0.00515 0.00182 -0.00093 C15 1 0.562237 -0.006521 0.248059 11.00000 0.02443 0.02116 = 0.01219 -0.00024 0.00235 0.00177 C16 1 0.526842 0.083046 0.312037 11.00000 0.02508 0.02541 = 0.01825 -0.00576 0.00521 -0.00096 AFIX 43 H16 2 0.563081 0.136368 0.364323 11.00000 -1.20000 AFIX 0 C17 1 0.438135 0.094817 0.299622 11.00000 0.02465 0.02136 = 0.02141 -0.00219 0.00754 0.00426 AFIX 43 H17 2 0.413833 0.157156 0.342809 11.00000 -1.20000 AFIX 0 C18 1 0.384978 0.014356 0.223215 11.00000 0.01287 0.02481 = 0.01969 0.00506 0.00343 0.00105 C19 1 0.419914 -0.076682 0.159240 11.00000 0.03459 0.01853 = 0.01473 0.00033 0.00347 -0.00259 AFIX 43 H19 2 0.383611 -0.130968 0.107504 11.00000 -1.20000 AFIX 0 C20 1 0.507687 -0.087417 0.171592 11.00000 0.02035 0.01944 = 0.01423 -0.00174 0.00245 -0.00295 C21 1 0.544728 -0.181161 0.099942 11.00000 0.01653 0.02441 = 0.02097 0.00456 0.00137 -0.00216 C22 1 0.637708 -0.194456 0.114490 11.00000 0.02207 0.01999 = 0.01425 0.00461 0.00293 0.00400 C23 1 0.673866 -0.287284 0.051751 11.00000 0.02713 0.01335 = 0.01634 0.00307 0.00237 -0.00418 AFIX 43 H23 2 0.637868 -0.342519 0.000257 11.00000 -1.20000 AFIX 0 C24 1 0.761784 -0.298795 0.064517 11.00000 0.01827 0.01911 = 0.01516 0.00218 0.00109 0.00147 AFIX 43 H24 2 0.785275 -0.359465 0.019776 11.00000 -1.20000 AFIX 0 O1 3 0.704276 0.055283 0.326617 11.00000 0.02764 0.04955 = 0.04305 -0.02673 0.00584 -0.00661 O2 3 0.496292 -0.240803 0.028974 11.00000 0.02449 0.03755 = 0.02551 -0.00918 0.00149 -0.00001 FE1 4 0.983756 -0.135282 0.071722 11.00000 0.01901 0.01634 = 0.01472 0.00133 0.00431 0.00091 BR1 5 1.035306 0.236092 0.140404 11.00000 0.04115 0.02185 = 0.03468 -0.00620 0.01689 -0.00597 BR2 5 0.265103 0.034414 0.205920 11.00000 0.02036 0.03143 = 0.02418 0.00622 0.00625 0.00255 MOLE 2 C31 1 0.280233 -0.409677 -0.132356 11.00000 0.02677 0.02252 = 0.02311 0.00245 0.00606 0.00446 C32 1 0.223743 -0.500752 -0.203837 11.00000 0.01176 0.02705 = 0.01743 0.00518 -0.00248 -0.00205 AFIX 43 H32 2 0.163046 -0.494470 -0.220879 11.00000 -1.20000 AFIX 0 C33 1 0.277158 -0.602828 -0.244244 11.00000 0.03742 0.02091 = 0.01692 0.00315 0.00682 -0.00217 AFIX 43 H33 2 0.257811 -0.678141 -0.292923 11.00000 -1.20000 AFIX 0 C34 1 0.364004 -0.572690 -0.199365 11.00000 0.02870 0.02817 = 0.02358 -0.00162 0.00855 -0.00145 AFIX 43 H34 2 0.412446 -0.622934 -0.214247 11.00000 -1.20000 AFIX 0 C35 1 0.366448 -0.453827 -0.127854 11.00000 0.02115 0.02217 = 0.02924 0.00490 0.00508 0.00074 AFIX 43 H35 2 0.415989 -0.412802 -0.085808 11.00000 -1.20000 AFIX 0 C36 1 0.370983 -0.738877 0.026131 11.00000 0.01346 0.01690 = 0.01786 0.00154 0.00478 -0.00327 C37 1 0.305177 -0.648110 0.056800 11.00000 0.02660 0.02864 = 0.01558 0.00243 0.00951 -0.00103 AFIX 43 H37 2 0.314928 -0.567345 0.103265 11.00000 -1.20000 AFIX 0 C38 1 0.224884 -0.699612 0.006374 11.00000 0.02084 0.02959 = 0.01461 0.00963 0.00532 0.00065 AFIX 43 H38 2 0.171053 -0.660097 0.013224 11.00000 -1.20000 AFIX 0 C39 1 0.237371 -0.819068 -0.055776 11.00000 0.01976 0.03679 = 0.00919 0.00411 -0.00421 -0.00206 AFIX 43 H39 2 0.193228 -0.872804 -0.098965 11.00000 -1.20000 AFIX 0 C40 1 0.326938 -0.847340 -0.043975 11.00000 0.02489 0.01798 = 0.01556 -0.00023 0.00120 -0.00164 AFIX 43 H40 2 0.352708 -0.923782 -0.076475 11.00000 -1.20000 AFIX 0 C41 1 0.463455 -0.720339 0.055957 11.00000 0.02124 0.01565 = 0.01694 -0.00067 0.00306 0.00076 C42 1 0.500375 -0.629367 0.137004 11.00000 0.01829 0.02041 = 0.01568 -0.00133 0.00730 -0.00292 AFIX 43 H42 2 0.464034 -0.576694 0.172129 11.00000 -1.20000 AFIX 0 C43 1 0.588141 -0.614084 0.167297 11.00000 0.02717 0.01680 = 0.01445 -0.00061 0.00371 -0.00127 C44 1 0.624831 -0.514548 0.253081 11.00000 0.02518 0.02041 = 0.01589 -0.00480 -0.00223 -0.00252 C45 1 0.718715 -0.506699 0.285473 11.00000 0.02002 0.02435 = 0.01293 0.00440 0.00315 0.00221 C46 1 0.755551 -0.416323 0.366482 11.00000 0.02296 0.02490 = 0.01861 -0.00485 0.00291 0.00259 AFIX 43 H46 2 0.719478 -0.361394 0.400801 11.00000 -1.20000 AFIX 0 C47 1 0.844163 -0.405258 0.397862 11.00000 0.02696 0.01785 = 0.01654 -0.00246 0.00673 -0.00287 AFIX 43 H47 2 0.868694 -0.343199 0.452741 11.00000 -1.20000 AFIX 0 C48 1 0.896445 -0.488259 0.346278 11.00000 0.01516 0.02019 = 0.02621 0.00342 0.00656 -0.00538 C49 1 0.861296 -0.576970 0.266338 11.00000 0.02275 0.02392 = 0.01698 0.00304 0.00826 -0.00057 AFIX 43 H49 2 0.897571 -0.631777 0.232223 11.00000 -1.20000 AFIX 0 C50 1 0.773016 -0.586988 0.235106 11.00000 0.01864 0.01605 = 0.01729 0.00287 0.00033 -0.00219 C51 1 0.736416 -0.682076 0.145861 11.00000 0.02960 0.02237 = 0.01914 0.00179 0.00648 0.00246 C52 1 0.642864 -0.693366 0.116661 11.00000 0.02449 0.01614 = 0.01589 0.00053 0.00568 0.00015 C53 1 0.607068 -0.785341 0.036136 11.00000 0.02603 0.01880 = 0.01603 -0.00525 0.00043 -0.00340 AFIX 43 H53 2 0.643658 -0.839385 0.002041 11.00000 -1.20000 AFIX 0 C54 1 0.518758 -0.799027 0.005117 11.00000 0.02531 0.02118 = 0.02204 0.00243 0.00265 -0.00108 AFIX 43 H54 2 0.495506 -0.861184 -0.050203 11.00000 -1.20000 AFIX 0 O31 3 0.577666 -0.441447 0.294824 11.00000 0.01956 0.05581 = 0.03898 -0.02679 0.00708 0.00002 O32 3 0.784306 -0.743548 0.098881 11.00000 0.02180 0.04120 = 0.02939 -0.01540 0.00940 0.00086 FE31 4 0.296601 -0.630785 -0.093220 11.00000 0.01920 0.01817 = 0.01508 0.00147 0.00371 -0.00288 BR31 5 0.240969 -0.259495 -0.054994 11.00000 0.04144 0.02326 = 0.03229 -0.00457 0.00531 0.00440 BR32 5 1.016072 -0.471058 0.386385 11.00000 0.01789 0.03150 = 0.02121 0.00333 0.00139 -0.00389 HKLF 4 Covalent radii and connectivity table for s94 in Pc C 0.770 H 0.320 O 0.660 FE 1.240 BR 1.140 C1 - C5 C2 Br1 Fe1 C2 - C3 C1 Fe1 C3 - C4 C2 Fe1 C4 - C3 C5 Fe1 C5 - C1 C4 Fe1 C6 - C10 C7 C11 Fe1 C7 - C8 C6 Fe1 C8 - C7 C9 Fe1 C9 - C10 C8 Fe1 C10 - C9 C6 Fe1 C11 - C24 C12 C6 C12 - C13 C11 C13 - C12 C22 C14 C14 - O1 C15 C13 C15 - C16 C20 C14 C16 - C15 C17 C17 - C16 C18 C18 - C19 C17 Br2 C19 - C20 C18 C20 - C19 C15 C21 C21 - O2 C22 C20 C22 - C23 C13 C21 C23 - C24 C22 C24 - C23 C11 O1 - C14 O2 - C21 Fe1 - C1 C8 C9 C7 C5 C6 C4 C10 C2 C3 Br1 - C1 Br2 - C18 C31 - C35 C32 Br31 Fe31 C32 - C33 C31 Fe31 C33 - C34 C32 Fe31 C34 - C33 C35 Fe31 C35 - C31 C34 Fe31 C36 - C40 C37 C41 Fe31 C37 - C38 C36 Fe31 C38 - C39 C37 Fe31 C39 - C38 C40 Fe31 C40 - C39 C36 Fe31 C41 - C42 C54 C36 C42 - C43 C41 C43 - C42 C52 C44 C44 - O31 C45 C43 C45 - C46 C50 C44 C46 - C47 C45 C47 - C46 C48 C48 - C49 C47 Br32 C49 - C48 C50 C50 - C49 C45 C51 C51 - O32 C52 C50 C52 - C53 C43 C51 C53 - C54 C52 C54 - C53 C41 O31 - C44 O32 - C51 Fe31 - C31 C39 C35 C37 C34 C38 C33 C36 C40 C32 Br31 - C31 Br32 - C48 Floating origin restraints generated h k l Fo^2 Sigma Why rejected -5 0 -7 10.96 2.74 observed but should be systematically absent 24982 Reflections read, of which 862 rejected -20 =< h =< 19, -11 =< k =< 11, -17 =< l =< 16, Max. 2-theta = 54.96 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -5 2 -2 753.54 31.20 2 160.65 12 4 -2 428.39 20.04 2 100.93 -1 8 -2 192.62 2.53 4 138.68 -1 1 -1 175.62 6.75 3 69.90 1 7 -1 216.97 2.41 4 114.20 -1 5 0 193.55 8.94 2 49.40 -8 9 0 20.62 2.49 2 20.08 1 1 1 162.74 6.35 3 52.75 -17 2 1 2.66 3.96 4 26.30 12 2 1 62.07 5.07 2 27.74 -8 8 2 26.89 2.46 2 16.20 -3 4 3 131.22 6.14 2 30.77 1 6 6 98.07 2.62 3 84.95 2 7 8 15.36 2.50 2 24.35 1 7 9 31.49 2.64 2 80.58 15 Inconsistent equivalents 7305 Unique reflections, of which 0 suppressed R(int) = 0.0935 R(sigma) = 0.0774 Friedel opposites not merged Maximum memory for data reduction = 4613 / 74378 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 = 6001 / 698143 wR2 = 0.1056 before cycle 1 for 7305 data and 524 / 524 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0369 * P )^2 + 3.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26904 0.00042 -0.031 OSF 2 0.00173 0.00025 -0.015 EXTI Mean shift/esd = 0.004 Maximum = -0.031 for OSF Max. shift = 0.000 A for C31 Max. dU = 0.000 for C5 Least-squares cycle 2 Maximum vector length = 511 Memory required = 6001 / 698143 wR2 = 0.1057 before cycle 2 for 7305 data and 524 / 524 parameters GooF = S = 1.034; Restrained GooF = 1.033 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0369 * P )^2 + 3.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26903 0.00042 -0.010 OSF 2 0.00172 0.00025 -0.005 EXTI Mean shift/esd = 0.001 Maximum = -0.010 for OSF Max. shift = 0.000 A for C31 Max. dU = 0.000 for C5 Least-squares cycle 3 Maximum vector length = 511 Memory required = 6001 / 698143 wR2 = 0.1057 before cycle 3 for 7305 data and 524 / 524 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0369 * P )^2 + 3.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26903 0.00042 -0.004 OSF 2 0.00172 0.00025 -0.002 EXTI Mean shift/esd = 0.000 Maximum = -0.004 for OSF Max. shift = 0.000 A for C2 Max. dU = 0.000 for C35 Least-squares cycle 4 Maximum vector length = 511 Memory required = 6001 / 698143 wR2 = 0.1057 before cycle 4 for 7305 data and 524 / 524 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0369 * P )^2 + 3.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26903 0.00042 0.000 OSF 2 0.00172 0.00025 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for x Br32 Max. shift = 0.000 A for C39 Max. dU = 0.000 for C8 Least-squares cycle 5 Maximum vector length = 511 Memory required = 6001 / 698143 wR2 = 0.1057 before cycle 5 for 7305 data and 524 / 524 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0369 * P )^2 + 3.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26903 0.00042 0.000 OSF 2 0.00172 0.00025 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for x Br32 Max. shift = 0.000 A for C42 Max. dU = 0.000 for C2 Least-squares cycle 6 Maximum vector length = 511 Memory required = 6001 / 698143 wR2 = 0.1057 before cycle 6 for 7305 data and 524 / 524 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0369 * P )^2 + 3.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26903 0.00042 0.000 OSF 2 0.00172 0.00025 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for x Br32 Max. shift = 0.000 A for H33 Max. dU = 0.000 for C47 Least-squares cycle 7 Maximum vector length = 511 Memory required = 6001 / 698143 wR2 = 0.1057 before cycle 7 for 7305 data and 524 / 524 parameters GooF = S = 1.034; Restrained GooF = 1.033 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0369 * P )^2 + 3.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26903 0.00042 0.000 OSF 2 0.00172 0.00025 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for x Br32 Max. shift = 0.000 A for C46 Max. dU = 0.000 for C48 Least-squares cycle 8 Maximum vector length = 511 Memory required = 6001 / 698143 wR2 = 0.1057 before cycle 8 for 7305 data and 524 / 524 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0369 * P )^2 + 3.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26903 0.00042 0.000 OSF 2 0.00172 0.00025 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for x Br32 Max. shift = 0.000 A for Fe1 Max. dU = 0.000 for C37 Least-squares cycle 9 Maximum vector length = 511 Memory required = 6001 / 698143 wR2 = 0.1057 before cycle 9 for 7305 data and 524 / 524 parameters GooF = S = 1.034; Restrained GooF = 1.033 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0369 * P )^2 + 3.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26903 0.00042 0.000 OSF 2 0.00172 0.00025 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for x Br32 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C10 Largest correlation matrix elements 0.547 EXTI / OSF Idealized hydrogen atom generation before cycle 10 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 C2 ** H2 1.1192 0.0012 0.0154 43 0.950 0.000 C2 C3 C1 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C3 ** H3 1.0267 -0.1753 -0.1101 43 0.950 0.000 C3 C4 C2 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C4 ** H4 0.8706 -0.1284 -0.1059 43 0.950 0.000 C4 C3 C5 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C5 ** H5 0.8638 0.0832 0.0183 43 0.950 0.000 C5 C1 C4 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C7 ** H7 0.9681 -0.0736 0.2606 43 0.950 0.000 C7 C8 C6 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C8 ** H8 1.1103 -0.1665 0.2337 43 0.950 0.000 C8 C7 C9 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C9 ** H9 1.0855 -0.3817 0.1127 43 0.950 0.000 C9 C10 C8 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C10 ** H10 0.9272 -0.4268 0.0596 43 0.950 0.000 C10 C9 C6 H12 0.8167 -0.0772 0.2569 43 0.950 0.000 C12 C13 C11 H16 0.5631 0.1364 0.3643 43 0.950 0.000 C16 C15 C17 H17 0.4138 0.1572 0.3428 43 0.950 0.000 C17 C16 C18 H19 0.3836 -0.1310 0.1075 43 0.950 0.000 C19 C20 C18 H23 0.6379 -0.3425 0.0002 43 0.950 0.000 C23 C24 C22 H24 0.7853 -0.3595 0.0198 43 0.950 0.000 C24 C23 C11 ** Bond(s) to Fe31 ignored in idealizing H-atoms attached to C32 ** H32 0.1630 -0.4945 -0.2209 43 0.950 0.000 C32 C33 C31 ** Bond(s) to Fe31 ignored in idealizing H-atoms attached to C33 ** H33 0.2578 -0.6781 -0.2929 43 0.950 0.000 C33 C34 C32 ** Bond(s) to Fe31 ignored in idealizing H-atoms attached to C34 ** H34 0.4124 -0.6229 -0.2142 43 0.950 0.000 C34 C33 C35 ** Bond(s) to Fe31 ignored in idealizing H-atoms attached to C35 ** H35 0.4160 -0.4128 -0.0858 43 0.950 0.000 C35 C31 C34 ** Bond(s) to Fe31 ignored in idealizing H-atoms attached to C37 ** H37 0.3149 -0.5673 0.1033 43 0.950 0.000 C37 C38 C36 ** Bond(s) to Fe31 ignored in idealizing H-atoms attached to C38 ** H38 0.1710 -0.6601 0.0132 43 0.950 0.000 C38 C39 C37 ** Bond(s) to Fe31 ignored in idealizing H-atoms attached to C39 ** H39 0.1932 -0.8728 -0.0990 43 0.950 0.000 C39 C38 C40 ** Bond(s) to Fe31 ignored in idealizing H-atoms attached to C40 ** H40 0.3527 -0.9238 -0.0765 43 0.950 0.000 C40 C39 C36 H42 0.4640 -0.5767 0.1721 43 0.950 0.000 C42 C43 C41 H46 0.7195 -0.3614 0.4008 43 0.950 0.000 C46 C47 C45 H47 0.8687 -0.3432 0.4527 43 0.950 0.000 C47 C46 C48 H49 0.8976 -0.6318 0.2322 43 0.950 0.000 C49 C48 C50 H53 0.6437 -0.8394 0.0020 43 0.950 0.000 C53 C54 C52 H54 0.4955 -0.8612 -0.0502 43 0.950 0.000 C54 C53 C41 s94 in Pc ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.99933 0.08636 0.04337 1.00000 0.02687 0.01570 0.02455 0.00627 0.00138 -0.00305 0.02294 0.01313 0.00046 0.00075 0.00050 0.00000 0.00388 0.00314 0.00344 0.00259 0.00289 0.00268 0.00145 C2 1.05842 -0.00420 0.00039 1.00000 0.02380 0.01753 0.02089 0.00486 0.01036 0.00346 0.01991 0.01298 0.00045 0.00070 0.00046 0.00000 0.00374 0.00306 0.00316 0.00248 0.00277 0.00253 0.00135 H2 1.11918 0.00122 0.01540 1.00000 0.02390 0.00000 0.00000 C3 1.00617 -0.10343 -0.06933 1.00000 0.03589 0.02174 0.01659 0.00595 0.01244 0.00723 0.02373 0.01372 0.00047 0.00075 0.00047 0.00000 0.00424 0.00350 0.00307 0.00262 0.00293 0.00286 0.00149 H3 1.02668 -0.17531 -0.11014 1.00000 0.02848 0.00000 0.00000 C4 0.91822 -0.07656 -0.06742 1.00000 0.02861 0.02632 0.01936 0.00411 -0.00156 -0.00322 0.02570 0.01334 0.00047 0.00079 0.00048 0.00000 0.00394 0.00354 0.00317 0.00273 0.00287 0.00293 0.00146 H4 0.87056 -0.12840 -0.10586 1.00000 0.03084 0.00000 0.00000 C5 0.91428 0.04200 0.00242 1.00000 0.02273 0.02033 0.02285 0.00513 0.00541 0.00253 0.02187 0.01272 0.00044 0.00071 0.00048 0.00000 0.00373 0.00331 0.00329 0.00261 0.00274 0.00263 0.00138 H5 0.86379 0.08321 0.01830 1.00000 0.02624 0.00000 0.00000 C6 0.91029 -0.24309 0.15575 1.00000 0.02020 0.01747 0.01427 0.00179 0.00467 0.00010 0.01715 0.01190 0.00042 0.00068 0.00045 0.00000 0.00338 0.00309 0.00287 0.00229 0.00253 0.00241 0.00127 C7 0.97674 -0.15358 0.21764 1.00000 0.02397 0.02038 0.01600 -0.00138 0.00336 -0.00362 0.02022 0.01240 0.00044 0.00074 0.00046 0.00000 0.00379 0.00342 0.00306 0.00251 0.00268 0.00260 0.00139 H7 0.96806 -0.07363 0.26058 1.00000 0.02427 0.00000 0.00000 C8 1.05599 -0.20595 0.20284 1.00000 0.01745 0.02291 0.02556 0.00590 0.00299 -0.00510 0.02218 0.01313 0.00044 0.00075 0.00049 0.00000 0.00350 0.00339 0.00348 0.00272 0.00278 0.00267 0.00139 H8 1.11032 -0.16646 0.23373 1.00000 0.02662 0.00000 0.00000 C9 1.04205 -0.32629 0.13492 1.00000 0.02691 0.02761 0.01442 0.00817 0.01139 0.00360 0.02196 0.01401 0.00047 0.00076 0.00049 0.00000 0.00408 0.00350 0.00296 0.00272 0.00278 0.00299 0.00143 H9 1.08552 -0.38173 0.11273 1.00000 0.02635 0.00000 0.00000 C10 0.95371 -0.35165 0.10506 1.00000 0.03230 0.01580 0.01405 -0.00102 0.00909 0.00099 0.02010 0.01301 0.00047 0.00072 0.00046 0.00000 0.00408 0.00317 0.00297 0.00239 0.00277 0.00266 0.00139 H10 0.92717 -0.42676 0.05962 1.00000 0.02412 0.00000 0.00000 C11 0.81731 -0.22360 0.14153 1.00000 0.02349 0.01533 0.01421 0.00301 0.00738 -0.00062 0.01717 0.01219 0.00043 0.00068 0.00044 0.00000 0.00356 0.00294 0.00292 0.00228 0.00258 0.00245 0.00128 C12 0.78053 -0.13053 0.20457 1.00000 0.02167 0.01957 0.02103 0.00381 0.00224 0.00287 0.02107 0.01315 0.00044 0.00071 0.00049 0.00000 0.00371 0.00325 0.00313 0.00260 0.00269 0.00258 0.00137 H12 0.81673 -0.07722 0.25690 1.00000 0.02528 0.00000 0.00000 C13 0.69367 -0.11556 0.19178 1.00000 0.02195 0.01727 0.01698 -0.00118 0.00509 -0.00104 0.01858 0.01218 0.00043 0.00070 0.00046 0.00000 0.00356 0.00314 0.00303 0.00242 0.00265 0.00247 0.00132 C14 0.65685 -0.01719 0.26113 1.00000 0.01510 0.02260 0.02259 -0.00515 0.00182 -0.00091 0.02039 0.01239 0.00044 0.00074 0.00050 0.00000 0.00351 0.00334 0.00329 0.00271 0.00269 0.00260 0.00135 C15 0.56223 -0.00653 0.24806 1.00000 0.02443 0.02115 0.01217 -0.00024 0.00234 0.00176 0.01946 0.01259 0.00045 0.00074 0.00046 0.00000 0.00380 0.00332 0.00298 0.00243 0.00273 0.00265 0.00138 C16 0.52684 0.08305 0.31204 1.00000 0.02509 0.02540 0.01824 -0.00576 0.00520 -0.00095 0.02280 0.01302 0.00045 0.00079 0.00049 0.00000 0.00380 0.00351 0.00321 0.00269 0.00276 0.00282 0.00141 H16 0.56308 0.13638 0.36432 1.00000 0.02736 0.00000 0.00000 C17 0.43814 0.09481 0.29962 1.00000 0.02463 0.02135 0.02141 -0.00220 0.00754 0.00426 0.02206 0.01288 0.00043 0.00074 0.00048 0.00000 0.00378 0.00337 0.00329 0.00262 0.00285 0.00267 0.00141 H17 0.41383 0.15715 0.34281 1.00000 0.02647 0.00000 0.00000 C18 0.38498 0.01436 0.22322 1.00000 0.01285 0.02481 0.01965 0.00506 0.00341 0.00105 0.01910 0.01364 0.00047 0.00074 0.00051 0.00000 0.00349 0.00345 0.00320 0.00257 0.00263 0.00249 0.00138 C19 0.41992 -0.07668 0.15924 1.00000 0.03460 0.01851 0.01473 0.00034 0.00348 -0.00259 0.02284 0.01297 0.00047 0.00075 0.00047 0.00000 0.00417 0.00319 0.00300 0.00248 0.00282 0.00285 0.00144 H19 0.38361 -0.13096 0.10751 1.00000 0.02741 0.00000 0.00000 C20 0.50768 -0.08742 0.17159 1.00000 0.02034 0.01943 0.01422 -0.00172 0.00245 -0.00294 0.01816 0.01177 0.00042 0.00071 0.00045 0.00000 0.00349 0.00313 0.00296 0.00247 0.00258 0.00259 0.00131 C21 0.54473 -0.18116 0.09994 1.00000 0.01652 0.02441 0.02100 0.00456 0.00138 -0.00216 0.02100 0.01250 0.00042 0.00077 0.00047 0.00000 0.00352 0.00351 0.00324 0.00266 0.00270 0.00262 0.00138 C22 0.63771 -0.19446 0.11449 1.00000 0.02206 0.01999 0.01423 0.00460 0.00291 0.00399 0.01888 0.01259 0.00042 0.00074 0.00045 0.00000 0.00359 0.00324 0.00291 0.00242 0.00256 0.00257 0.00132 C23 0.67387 -0.28728 0.05175 1.00000 0.02714 0.01334 0.01634 0.00306 0.00239 -0.00417 0.01924 0.01257 0.00045 0.00072 0.00046 0.00000 0.00396 0.00293 0.00315 0.00237 0.00272 0.00254 0.00136 H23 0.63787 -0.34251 0.00025 1.00000 0.02309 0.00000 0.00000 C24 0.76178 -0.29880 0.06452 1.00000 0.01827 0.01910 0.01515 0.00218 0.00107 0.00147 0.01785 0.01214 0.00041 0.00074 0.00046 0.00000 0.00374 0.00318 0.00300 0.00245 0.00261 0.00259 0.00135 H24 0.78527 -0.35947 0.01978 1.00000 0.02142 0.00000 0.00000 O1 0.70428 0.05528 0.32661 1.00000 0.02763 0.04955 0.04302 -0.02673 0.00584 -0.00660 0.04028 0.01001 0.00036 0.00067 0.00043 0.00000 0.00314 0.00352 0.00333 0.00277 0.00260 0.00261 0.00145 O2 0.49629 -0.24081 0.02898 1.00000 0.02445 0.03756 0.02550 -0.00920 0.00147 -0.00001 0.02970 0.00933 0.00034 0.00057 0.00037 0.00000 0.00289 0.00304 0.00260 0.00216 0.00222 0.00220 0.00118 Fe1 0.98376 -0.13528 0.07172 1.00000 0.01900 0.01633 0.01471 0.00132 0.00432 0.00091 0.01656 0.00169 0.00006 0.00010 0.00006 0.00000 0.00051 0.00044 0.00042 0.00034 0.00036 0.00036 0.00020 Br1 1.03531 0.23609 0.14040 1.00000 0.04115 0.02184 0.03467 -0.00620 0.01689 -0.00597 0.03125 0.00140 0.00005 0.00008 0.00005 0.00000 0.00048 0.00036 0.00040 0.00030 0.00035 0.00032 0.00019 Br2 0.26510 0.03441 0.20592 1.00000 0.02036 0.03142 0.02418 0.00622 0.00625 0.00254 0.02508 0.00131 0.00004 0.00008 0.00005 0.00000 0.00037 0.00037 0.00034 0.00029 0.00027 0.00030 0.00017 C31 0.28024 -0.40967 -0.13235 1.00000 0.02675 0.02251 0.02313 0.00246 0.00609 0.00448 0.02399 0.01390 0.00047 0.00080 0.00051 0.00000 0.00393 0.00351 0.00331 0.00269 0.00290 0.00279 0.00147 C32 0.22374 -0.50076 -0.20384 1.00000 0.01173 0.02705 0.01742 0.00519 -0.00249 -0.00205 0.01952 0.01215 0.00042 0.00075 0.00045 0.00000 0.00326 0.00335 0.00302 0.00252 0.00248 0.00249 0.00132 H32 0.16305 -0.49447 -0.22088 1.00000 0.02343 0.00000 0.00000 C33 0.27716 -0.60283 -0.24424 1.00000 0.03745 0.02088 0.01690 0.00316 0.00681 -0.00218 0.02490 0.01347 0.00048 0.00076 0.00048 0.00000 0.00431 0.00350 0.00316 0.00261 0.00296 0.00289 0.00150 H33 0.25781 -0.67814 -0.29292 1.00000 0.02988 0.00000 0.00000 C34 0.36400 -0.57269 -0.19936 1.00000 0.02868 0.02817 0.02356 -0.00162 0.00855 -0.00144 0.02635 0.01344 0.00047 0.00080 0.00050 0.00000 0.00396 0.00359 0.00340 0.00288 0.00293 0.00300 0.00148 H34 0.41245 -0.62294 -0.21423 1.00000 0.03162 0.00000 0.00000 C35 0.36645 -0.45383 -0.12785 1.00000 0.02112 0.02218 0.02924 0.00490 0.00507 0.00075 0.02419 0.01373 0.00045 0.00074 0.00052 0.00000 0.00378 0.00347 0.00360 0.00275 0.00294 0.00268 0.00145 H35 0.41599 -0.41281 -0.08581 1.00000 0.02903 0.00000 0.00000 C36 0.37099 -0.73887 0.02613 1.00000 0.01341 0.01692 0.01785 0.00155 0.00476 -0.00327 0.01584 0.01166 0.00040 0.00067 0.00045 0.00000 0.00313 0.00301 0.00301 0.00231 0.00247 0.00230 0.00124 C37 0.30518 -0.64811 0.05680 1.00000 0.02660 0.02864 0.01558 0.00244 0.00952 -0.00103 0.02286 0.01359 0.00046 0.00078 0.00048 0.00000 0.00394 0.00361 0.00301 0.00269 0.00279 0.00285 0.00145 H37 0.31493 -0.56734 0.10326 1.00000 0.02744 0.00000 0.00000 C38 0.22488 -0.69962 0.00637 1.00000 0.02079 0.02962 0.01461 0.00961 0.00531 0.00062 0.02144 0.01294 0.00044 0.00077 0.00046 0.00000 0.00360 0.00359 0.00300 0.00266 0.00259 0.00275 0.00138 H38 0.17105 -0.66011 0.01322 1.00000 0.02572 0.00000 0.00000 C39 0.23737 -0.81906 -0.05578 1.00000 0.01976 0.03675 0.00918 0.00410 -0.00420 -0.00205 0.02293 0.01341 0.00047 0.00080 0.00048 0.00000 0.00372 0.00388 0.00280 0.00281 0.00245 0.00316 0.00141 H39 0.19323 -0.87279 -0.09897 1.00000 0.02752 0.00000 0.00000 C40 0.32693 -0.84733 -0.04398 1.00000 0.02491 0.01797 0.01554 -0.00023 0.00121 -0.00163 0.01990 0.01224 0.00044 0.00072 0.00046 0.00000 0.00388 0.00321 0.00302 0.00244 0.00268 0.00258 0.00137 H40 0.35270 -0.92378 -0.07648 1.00000 0.02388 0.00000 0.00000 C41 0.46346 -0.72034 0.05596 1.00000 0.02124 0.01564 0.01692 -0.00067 0.00306 0.00074 0.01806 0.01178 0.00042 0.00068 0.00045 0.00000 0.00355 0.00296 0.00302 0.00238 0.00256 0.00248 0.00129 C42 0.50038 -0.62937 0.13700 1.00000 0.01829 0.02041 0.01568 -0.00134 0.00730 -0.00293 0.01758 0.01200 0.00042 0.00072 0.00044 0.00000 0.00339 0.00337 0.00292 0.00237 0.00256 0.00250 0.00131 H42 0.46403 -0.57669 0.17213 1.00000 0.02110 0.00000 0.00000 C43 0.58814 -0.61408 0.16730 1.00000 0.02716 0.01678 0.01447 -0.00062 0.00371 -0.00126 0.01956 0.01195 0.00044 0.00069 0.00045 0.00000 0.00380 0.00311 0.00300 0.00239 0.00270 0.00255 0.00135 C44 0.62483 -0.51455 0.25308 1.00000 0.02517 0.02042 0.01589 -0.00479 -0.00221 -0.00252 0.02142 0.01206 0.00046 0.00073 0.00047 0.00000 0.00388 0.00327 0.00306 0.00259 0.00278 0.00272 0.00140 C45 0.71872 -0.50671 0.28547 1.00000 0.02002 0.02434 0.01291 0.00440 0.00314 0.00222 0.01913 0.01286 0.00044 0.00076 0.00046 0.00000 0.00357 0.00341 0.00302 0.00243 0.00268 0.00259 0.00136 C46 0.75555 -0.41632 0.36648 1.00000 0.02295 0.02489 0.01862 -0.00485 0.00291 0.00258 0.02235 0.01265 0.00044 0.00079 0.00049 0.00000 0.00373 0.00347 0.00318 0.00270 0.00274 0.00280 0.00140 H46 0.71948 -0.36138 0.40079 1.00000 0.02682 0.00000 0.00000 C47 0.84417 -0.40526 0.39786 1.00000 0.02695 0.01786 0.01656 -0.00243 0.00672 -0.00286 0.02013 0.01234 0.00044 0.00071 0.00046 0.00000 0.00381 0.00320 0.00307 0.00244 0.00275 0.00260 0.00137 H47 0.86870 -0.34320 0.45274 1.00000 0.02416 0.00000 0.00000 C48 0.89644 -0.48826 0.34628 1.00000 0.01515 0.02016 0.02622 0.00341 0.00656 -0.00540 0.02018 0.01321 0.00047 0.00073 0.00052 0.00000 0.00375 0.00335 0.00366 0.00263 0.00290 0.00253 0.00147 C49 0.86130 -0.57698 0.26634 1.00000 0.02277 0.02392 0.01697 0.00304 0.00826 -0.00057 0.02062 0.01249 0.00043 0.00076 0.00046 0.00000 0.00369 0.00331 0.00312 0.00257 0.00273 0.00270 0.00137 H49 0.89757 -0.63179 0.23223 1.00000 0.02475 0.00000 0.00000 C50 0.77302 -0.58699 0.23511 1.00000 0.01862 0.01605 0.01728 0.00288 0.00032 -0.00220 0.01780 0.01169 0.00041 0.00071 0.00045 0.00000 0.00341 0.00296 0.00309 0.00236 0.00264 0.00244 0.00129 C51 0.73641 -0.68208 0.14586 1.00000 0.02963 0.02236 0.01912 0.00179 0.00650 0.00247 0.02349 0.01336 0.00046 0.00077 0.00048 0.00000 0.00400 0.00348 0.00319 0.00262 0.00282 0.00280 0.00144 C52 0.64287 -0.69337 0.11666 1.00000 0.02449 0.01613 0.01588 0.00053 0.00567 0.00013 0.01862 0.01231 0.00042 0.00071 0.00045 0.00000 0.00369 0.00310 0.00293 0.00237 0.00256 0.00253 0.00131 C53 0.60707 -0.78533 0.03614 1.00000 0.02603 0.01879 0.01603 -0.00525 0.00044 -0.00340 0.02085 0.01228 0.00046 0.00076 0.00047 0.00000 0.00392 0.00324 0.00318 0.00249 0.00276 0.00264 0.00140 H53 0.64365 -0.83938 0.00204 1.00000 0.02502 0.00000 0.00000 C54 0.51876 -0.79901 0.00512 1.00000 0.02529 0.02119 0.02202 0.00245 0.00264 -0.00107 0.02316 0.01364 0.00046 0.00079 0.00052 0.00000 0.00405 0.00336 0.00340 0.00272 0.00290 0.00276 0.00147 H54 0.49550 -0.86116 -0.05021 1.00000 0.02779 0.00000 0.00000 O31 0.57766 -0.44145 0.29482 1.00000 0.01956 0.05578 0.03897 -0.02675 0.00709 0.00003 0.03795 0.00981 0.00034 0.00068 0.00040 0.00000 0.00289 0.00368 0.00321 0.00280 0.00244 0.00258 0.00142 O32 0.78431 -0.74356 0.09888 1.00000 0.02178 0.04118 0.02938 -0.01539 0.00939 0.00086 0.03019 0.00947 0.00033 0.00058 0.00037 0.00000 0.00281 0.00314 0.00269 0.00224 0.00228 0.00220 0.00122 Fe31 0.29660 -0.63078 -0.09322 1.00000 0.01919 0.01816 0.01508 0.00147 0.00371 -0.00288 0.01745 0.00170 0.00006 0.00010 0.00006 0.00000 0.00051 0.00045 0.00042 0.00035 0.00036 0.00037 0.00020 Br31 0.24097 -0.25949 -0.05499 1.00000 0.04144 0.02326 0.03229 -0.00456 0.00530 0.00440 0.03266 0.00147 0.00005 0.00008 0.00006 0.00000 0.00048 0.00037 0.00040 0.00029 0.00034 0.00033 0.00019 Br32 1.01607 -0.47106 0.38638 1.00000 0.01788 0.03150 0.02120 0.00333 0.00138 -0.00389 0.02391 0.00126 0.00004 0.00008 0.00005 0.00000 0.00036 0.00036 0.00032 0.00030 0.00026 0.00030 0.00016 Final Structure Factor Calculation for s94 in Pc Total number of l.s. parameters = 524 Maximum vector length = 511 Memory required = 5479 / 26068 wR2 = 0.1057 before cycle 10 for 7305 data and 2 / 524 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0369 * P )^2 + 3.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0445 for 6547 Fo > 4sig(Fo) and 0.0538 for all 7305 data wR2 = 0.1057, GooF = S = 1.033, Restrained GooF = 1.033 for all data Flack x parameter = -0.0141 with esd 0.0106 Expected values are 0 (within 3 esd'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 = 58.00 for non-hydrogen and 28.00 for hydrogen atoms Principal mean square atomic displacements U 0.0337 0.0230 0.0121 C1 0.0296 0.0167 0.0135 C2 0.0405 0.0193 0.0114 C3 0.0366 0.0241 0.0165 C4 0.0273 0.0221 0.0162 C5 0.0203 0.0182 0.0130 C6 0.0263 0.0189 0.0155 C7 0.0328 0.0204 0.0134 C8 0.0348 0.0237 0.0074 C9 0.0326 0.0162 0.0115 C10 0.0241 0.0174 0.0101 C11 0.0243 0.0237 0.0152 C12 0.0223 0.0176 0.0158 C13 0.0281 0.0186 0.0144 C14 0.0258 0.0204 0.0122 C15 0.0287 0.0249 0.0148 C16 0.0276 0.0234 0.0152 C17 0.0279 0.0166 0.0127 C18 0.0357 0.0181 0.0147 C19 0.0229 0.0181 0.0135 C20 0.0292 0.0180 0.0158 C21 0.0253 0.0199 0.0115 C22 0.0298 0.0173 0.0106 C23 0.0202 0.0200 0.0133 C24 0.0732 0.0292 0.0184 O1 0.0433 0.0263 0.0195 O2 0.0194 0.0165 0.0138 Fe1 0.0482 0.0262 0.0193 Br1 0.0352 0.0208 0.0193 Br2 0.0298 0.0228 0.0194 C31 0.0312 0.0181 0.0093 C32 0.0378 0.0226 0.0143 C33 0.0309 0.0270 0.0211 C34 0.0318 0.0211 0.0196 C35 0.0195 0.0178 0.0102 C36 0.0292 0.0277 0.0117 C37 0.0343 0.0208 0.0092 C38 0.0384 0.0239 0.0065 C39 0.0268 0.0178 0.0151 C40 0.0218 0.0171 0.0153 C41 0.0233 0.0175 0.0119 C42 0.0276 0.0168 0.0143 C43 0.0302 0.0231 0.0110 C44 0.0262 0.0198 0.0114 C45 0.0297 0.0215 0.0159 C46 0.0280 0.0179 0.0145 C47 0.0280 0.0228 0.0098 C48 0.0253 0.0238 0.0128 C49 0.0242 0.0155 0.0137 C50 0.0304 0.0220 0.0181 C51 0.0245 0.0163 0.0150 C52 0.0286 0.0228 0.0111 C53 0.0279 0.0224 0.0191 C54 0.0759 0.0216 0.0164 O31 0.0518 0.0245 0.0142 O32 0.0220 0.0167 0.0137 Fe31 0.0444 0.0332 0.0204 Br31 0.0344 0.0208 0.0165 Br32 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.035 0.053 0.067 0.083 0.098 0.116 0.138 0.168 0.221 1.000 Number in group 736. 769. 693. 767. 709. 731. 732. 707. 726. 735. GooF 1.056 1.097 1.036 1.023 0.980 1.004 1.023 1.055 0.990 1.058 K 1.136 1.021 0.986 0.991 0.989 1.002 0.998 1.009 1.015 1.005 Resolution(A) 0.77 0.81 0.86 0.91 0.97 1.03 1.11 1.22 1.39 1.74 inf Number in group 742. 748. 713. 720. 737. 726. 741. 718. 728. 732. GooF 1.024 1.036 1.039 1.101 0.978 1.012 1.022 0.966 1.042 1.103 K 0.984 0.999 0.999 1.008 1.016 1.026 1.021 1.014 1.008 0.993 R1 0.130 0.102 0.084 0.071 0.055 0.050 0.041 0.034 0.031 0.031 Recommended weighting scheme: WGHT 0.0367 3.5814 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) -12 0 0 1424.70 593.05 6.67 0.073 1.30 0 3 -6 543.41 138.13 5.90 0.035 1.79 3 6 -9 324.95 100.48 5.40 0.030 1.06 -11 0 0 552.90 150.86 5.12 0.037 1.42 10 0 0 783.97 53.76 4.57 0.022 1.56 -14 1 0 11205.04 8467.52 4.56 0.276 1.11 -13 0 0 560.85 163.64 4.55 0.038 1.20 0 3 6 497.05 164.24 4.24 0.038 1.79 -17 1 0 3105.32 2321.28 4.22 0.145 0.91 15 4 4 216.44 840.35 4.08 0.087 0.87 11 3 3 1945.81 2851.13 4.07 0.160 1.17 10 0 -2 6041.13 8328.21 4.07 0.274 1.60 -14 4 8 127.56 346.66 3.87 0.056 0.94 -17 3 8 1194.91 2006.70 3.80 0.134 0.85 4 1 14 462.76 949.19 3.75 0.092 0.89 14 4 6 -112.13 174.43 3.71 0.040 0.85 -8 1 0 89.31 10.91 3.62 0.010 1.91 4 2 1 6535.31 8278.05 3.61 0.273 2.77 -6 5 8 35.18 179.66 3.60 0.040 1.17 6 6 -6 321.14 158.12 3.60 0.038 1.17 12 0 0 1630.67 629.15 3.59 0.075 1.30 0 6 3 388.94 182.51 3.53 0.041 1.40 0 6 -3 288.71 126.32 3.52 0.034 1.40 3 6 -6 4649.05 3652.77 3.47 0.181 1.23 -4 3 14 1335.03 1938.15 3.39 0.132 0.93 -10 3 -12 121.14 465.87 3.39 0.065 0.80 -15 1 0 6974.41 5612.67 3.39 0.225 1.03 -14 0 12 287.60 685.53 3.38 0.079 0.89 -4 1 -1 14199.49 17895.95 3.32 0.402 3.30 -5 1 -1 5236.69 6857.87 3.32 0.249 2.77 15 5 -7 1922.22 1256.58 3.31 0.106 0.87 0 6 6 5424.29 4306.99 3.28 0.197 1.23 13 5 -9 3190.97 2428.25 3.23 0.148 0.90 15 4 -3 303.49 585.60 3.20 0.073 0.96 -2 5 -15 -81.68 214.08 3.19 0.044 0.78 12 1 -5 2684.68 2112.58 3.18 0.138 1.27 -17 1 10 -90.49 106.53 3.17 0.031 0.84 -7 9 -7 26.47 252.66 3.12 0.048 0.79 1 4 -1 171.39 82.32 3.10 0.027 2.17 -4 7 -2 1665.86 1303.59 3.10 0.108 1.17 11 1 -7 3253.77 2693.20 3.06 0.156 1.26 -10 1 7 1290.88 1647.34 3.05 0.122 1.34 14 0 -8 7482.16 5536.99 3.03 0.223 1.03 -5 8 9 163.49 577.73 3.03 0.072 0.88 15 1 2 819.26 1320.02 3.00 0.109 0.99 1 11 -5 86.08 291.08 2.99 0.051 0.77 -2 8 8 549.02 975.55 2.98 0.094 0.93 -15 6 4 449.97 254.49 2.98 0.048 0.86 13 0 0 617.75 44.18 2.95 0.020 1.20 13 1 -1 335.86 566.51 2.94 0.071 1.21 Bond lengths and angles C1 - Distance Angles C5 1.4134 (0.0098) C2 1.4528 (0.0093) 109.58 (0.60) Br1 1.8843 (0.0070) 127.21 (0.53) 123.20 (0.51) Fe1 2.0256 (0.0065) 70.23 (0.38) 70.09 (0.37) 125.22 (0.34) C1 - C5 C2 Br1 C2 - Distance Angles C3 1.4338 (0.0098) C1 1.4528 (0.0093) 105.87 (0.58) Fe1 2.0518 (0.0062) 70.02 (0.36) 68.16 (0.35) H2 0.9500 127.07 127.07 126.30 C2 - C3 C1 Fe1 C3 - Distance Angles C4 1.4291 (0.0101) C2 1.4338 (0.0098) 108.87 (0.57) Fe1 2.0628 (0.0061) 69.14 (0.36) 69.19 (0.34) H3 0.9500 125.56 125.56 127.69 C3 - C4 C2 Fe1 C4 - Distance Angles C3 1.4291 (0.0101) C5 1.4326 (0.0095) 108.26 (0.61) Fe1 2.0490 (0.0067) 70.18 (0.38) 69.18 (0.37) H4 0.9500 125.87 125.87 126.35 C4 - C3 C5 Fe1 C5 - Distance Angles C1 1.4134 (0.0098) C4 1.4326 (0.0095) 107.41 (0.61) Fe1 2.0405 (0.0065) 69.09 (0.38) 69.81 (0.37) H5 0.9500 126.29 126.29 126.37 C5 - C1 C4 Fe1 C6 - Distance Angles C10 1.4453 (0.0087) C7 1.4505 (0.0093) 106.31 (0.57) C11 1.4662 (0.0093) 125.91 (0.58) 127.68 (0.57) Fe1 2.0442 (0.0061) 69.51 (0.35) 68.99 (0.35) 123.52 (0.43) C6 - C10 C7 C11 C7 - Distance Angles C8 1.4005 (0.0097) C6 1.4505 (0.0093) 107.86 (0.58) Fe1 2.0387 (0.0062) 69.44 (0.37) 69.39 (0.35) H7 0.9500 126.07 126.07 126.66 C7 - C8 C6 Fe1 C8 - Distance Angles C7 1.4005 (0.0097) C9 1.4038 (0.0099) 108.90 (0.61) Fe1 2.0279 (0.0067) 70.27 (0.39) 70.11 (0.39) H8 0.9500 125.55 125.55 125.66 C8 - C7 C9 Fe1 C9 - Distance Angles C10 1.4026 (0.0102) C8 1.4038 (0.0099) 109.14 (0.58) Fe1 2.0362 (0.0067) 70.42 (0.38) 69.48 (0.38) H9 0.9500 125.43 125.43 126.26 C9 - C10 C8 Fe1 C10 - Distance Angles C9 1.4026 (0.0102) C6 1.4453 (0.0087) 107.77 (0.57) Fe1 2.0492 (0.0065) 69.42 (0.38) 69.14 (0.35) H10 0.9500 126.11 126.11 126.89 C10 - C9 C6 Fe1 C11 - Distance Angles C24 1.4008 (0.0091) C12 1.4087 (0.0087) 117.66 (0.61) C6 1.4662 (0.0093) 120.66 (0.55) 121.69 (0.59) C11 - C24 C12 C12 - Distance Angles C13 1.3673 (0.0096) C11 1.4087 (0.0087) 121.17 (0.64) H12 0.9500 119.42 119.42 C12 - C13 C11 C13 - Distance Angles C12 1.3673 (0.0096) C22 1.4223 (0.0092) 120.80 (0.58) C14 1.4979 (0.0086) 119.66 (0.59) 119.53 (0.58) C13 - C12 C22 C14 - Distance Angles O1 1.2304 (0.0086) C15 1.4862 (0.0093) 120.77 (0.60) C13 1.4979 (0.0086) 120.41 (0.62) 118.82 (0.56) C14 - O1 C15 C15 - Distance Angles C16 1.3880 (0.0089) C20 1.4136 (0.0090) 119.48 (0.63) C14 1.4862 (0.0093) 119.72 (0.61) 120.80 (0.56) C15 - C16 C20 C16 - Distance Angles C15 1.3880 (0.0089) C17 1.3943 (0.0097) 120.04 (0.63) H16 0.9500 119.98 119.98 C16 - C15 C17 C17 - Distance Angles C16 1.3943 (0.0097) C18 1.4010 (0.0098) 119.75 (0.59) H17 0.9500 120.13 120.13 C17 - C16 C18 C18 - Distance Angles C19 1.3915 (0.0095) C17 1.4010 (0.0098) 120.59 (0.66) Br2 1.8867 (0.0074) 120.19 (0.55) 119.21 (0.50) C18 - C19 C17 C19 - Distance Angles C20 1.3789 (0.0096) C18 1.3915 (0.0095) 119.43 (0.63) H19 0.9500 120.29 120.29 C19 - C20 C18 C20 - Distance Angles C19 1.3789 (0.0096) C15 1.4136 (0.0090) 120.71 (0.58) C21 1.4996 (0.0089) 119.03 (0.57) 120.21 (0.58) C20 - C19 C15 C21 - Distance Angles O2 1.2317 (0.0083) C22 1.4604 (0.0090) 121.85 (0.61) C20 1.4996 (0.0089) 119.31 (0.60) 118.79 (0.57) C21 - O2 C22 C22 - Distance Angles C23 1.3992 (0.0091) C13 1.4223 (0.0092) 118.28 (0.60) C21 1.4604 (0.0090) 119.96 (0.61) 121.75 (0.57) C22 - C23 C13 C23 - Distance Angles C24 1.3812 (0.0093) C22 1.3992 (0.0091) 120.15 (0.62) H23 0.9500 119.93 119.93 C23 - C24 C22 C24 - Distance Angles C23 1.3812 (0.0093) C11 1.4008 (0.0091) 121.91 (0.60) H24 0.9500 119.05 119.05 C24 - C23 C11 O1 - Distance Angles C14 1.2304 (0.0086) O1 - O2 - Distance Angles C21 1.2317 (0.0083) O2 - Fe1 - Distance Angles C1 2.0256 (0.0065) C8 2.0279 (0.0067) 113.58 (0.27) C9 2.0362 (0.0067) 145.40 (0.29) 40.41 (0.28) C7 2.0387 (0.0062) 107.47 (0.27) 40.29 (0.27) 68.10 (0.26) C5 2.0405 (0.0065) 40.68 (0.28) 143.78 (0.27) 173.87 (0.29) 112.69 (0.26) C6 2.0442 (0.0061) 131.94 (0.26) 68.94 (0.26) 68.65 (0.26) 41.62 (0.26) 107.65 (0.26) C4 2.0490 (0.0067) 68.52 (0.28) 174.43 (0.28) 135.18 (0.29) 144.88 (0.28) 41.01 (0.27) 113.85 (0.27) C10 2.0492 (0.0065) 172.76 (0.28) 68.23 (0.27) 40.16 (0.28) 69.07 (0.25) 133.92 (0.28) 41.35 (0.24) 110.37 (0.28) C2 2.0518 (0.0062) 41.74 (0.26) 108.65 (0.27) 114.48 (0.26) 132.10 (0.26) 69.82 (0.26) 172.49 (0.25) 69.21 (0.28) C3 2.0628 (0.0061) 68.58 (0.27) 134.50 (0.27) 111.23 (0.26) 172.50 (0.29) 68.82 (0.26) 145.70 (0.27) 40.68 (0.28) Fe1 - C1 C8 C9 C7 C5 C6 C4 Br1 - Distance Angles C1 1.8843 (0.0070) Br1 - Br2 - Distance Angles C18 1.8867 (0.0074) Br2 - C31 - Distance Angles C35 1.4192 (0.0099) C32 1.4365 (0.0098) 109.94 (0.61) Br31 1.8884 (0.0069) 126.92 (0.57) 123.11 (0.52) Fe31 2.0324 (0.0070) 69.68 (0.39) 70.66 (0.39) 124.63 (0.35) C31 - C35 C32 Br31 C32 - Distance Angles C33 1.4307 (0.0096) C31 1.4365 (0.0098) 106.27 (0.58) Fe31 2.0640 (0.0064) 69.13 (0.37) 68.30 (0.37) H32 0.9500 126.87 126.87 127.23 C32 - C33 C31 Fe31 C33 - Distance Angles C34 1.4212 (0.0104) C32 1.4307 (0.0096) 108.58 (0.59) Fe31 2.0502 (0.0064) 69.67 (0.38) 70.17 (0.36) H33 0.9500 125.71 125.71 126.02 C33 - C34 C32 Fe31 C34 - Distance Angles C33 1.4212 (0.0104) C35 1.4350 (0.0096) 108.75 (0.61) Fe31 2.0490 (0.0066) 69.76 (0.38) 68.91 (0.37) H34 0.9500 125.63 125.63 127.29 C34 - C33 C35 Fe31 C35 - Distance Angles C31 1.4192 (0.0099) C34 1.4350 (0.0096) 106.44 (0.64) Fe31 2.0351 (0.0066) 69.48 (0.40) 69.95 (0.38) H35 0.9500 126.78 126.78 125.38 C35 - C31 C34 Fe31 C36 - Distance Angles C40 1.4372 (0.0088) C37 1.4522 (0.0090) 106.34 (0.56) C41 1.4570 (0.0089) 126.22 (0.54) 127.38 (0.57) Fe31 2.0527 (0.0063) 69.70 (0.36) 68.94 (0.36) 123.89 (0.41) C36 - C40 C37 C41 C37 - Distance Angles C38 1.4014 (0.0098) C36 1.4522 (0.0090) 108.57 (0.59) Fe31 2.0446 (0.0064) 70.19 (0.36) 69.54 (0.35) H37 0.9500 125.72 125.72 126.13 C37 - C38 C36 Fe31 C38 - Distance Angles C39 1.3993 (0.0100) C37 1.4014 (0.0098) 108.49 (0.62) Fe31 2.0500 (0.0060) 69.34 (0.38) 69.78 (0.36) H38 0.9500 125.76 125.76 126.70 C38 - C39 C37 Fe31 C39 - Distance Angles C38 1.3993 (0.0100) C40 1.4268 (0.0100) 109.19 (0.61) Fe31 2.0339 (0.0070) 70.58 (0.39) 70.47 (0.38) H39 0.9500 125.41 125.41 125.13 C39 - C38 C40 Fe31 C40 - Distance Angles C39 1.4268 (0.0100) C36 1.4372 (0.0088) 107.40 (0.56) Fe31 2.0572 (0.0064) 68.71 (0.37) 69.36 (0.35) H40 0.9500 126.30 126.30 127.17 C40 - C39 C36 Fe31 C41 - Distance Angles C42 1.4023 (0.0087) C54 1.4166 (0.0091) 118.17 (0.61) C36 1.4570 (0.0089) 121.56 (0.55) 120.24 (0.57) C41 - C42 C54 C42 - Distance Angles C43 1.3829 (0.0093) C41 1.4023 (0.0087) 121.93 (0.57) H42 0.9500 119.03 119.03 C42 - C43 C41 C43 - Distance Angles C42 1.3829 (0.0093) C52 1.4110 (0.0088) 119.61 (0.57) C44 1.4917 (0.0085) 120.26 (0.57) 120.13 (0.61) C43 - C42 C52 C44 - Distance Angles O31 1.2218 (0.0083) C45 1.4739 (0.0095) 121.29 (0.58) C43 1.4917 (0.0084) 120.32 (0.63) 118.39 (0.57) C44 - O31 C45 C45 - Distance Angles C46 1.3986 (0.0094) C50 1.4082 (0.0090) 118.70 (0.61) C44 1.4739 (0.0095) 120.11 (0.58) 121.19 (0.58) C45 - C46 C50 C46 - Distance Angles C47 1.3942 (0.0096) C45 1.3986 (0.0094) 121.29 (0.60) H46 0.9500 119.35 119.35 C46 - C47 C45 C47 - Distance Angles C46 1.3942 (0.0096) C48 1.4081 (0.0091) 118.42 (0.59) H47 0.9500 120.79 120.79 C47 - C46 C48 C48 - Distance Angles C49 1.3729 (0.0096) C47 1.4081 (0.0091) 121.00 (0.65) Br32 1.8808 (0.0073) 120.22 (0.52) 118.75 (0.50) C48 - C49 C47 C49 - Distance Angles C48 1.3729 (0.0097) C50 1.3882 (0.0092) 120.33 (0.62) H49 0.9500 119.83 119.83 C49 - C48 C50 C50 - Distance Angles C49 1.3882 (0.0092) C45 1.4082 (0.0090) 120.25 (0.59) C51 1.5032 (0.0090) 119.14 (0.58) 120.60 (0.59) C50 - C49 C45 C51 - Distance Angles O32 1.2252 (0.0081) C52 1.4671 (0.0096) 122.38 (0.62) C50 1.5032 (0.0090) 119.96 (0.64) 117.63 (0.56) C51 - O32 C52 C52 - Distance Angles C53 1.3978 (0.0089) C43 1.4110 (0.0088) 119.15 (0.62) C51 1.4671 (0.0096) 118.88 (0.58) 121.97 (0.58) C52 - C53 C43 C53 - Distance Angles C54 1.3909 (0.0102) C52 1.3978 (0.0089) 121.08 (0.63) H53 0.9500 119.46 119.46 C53 - C54 C52 C54 - Distance Angles C53 1.3909 (0.0102) C41 1.4166 (0.0091) 120.05 (0.63) H54 0.9500 119.97 119.97 C54 - C53 C41 O31 - Distance Angles C44 1.2218 (0.0083) O31 - O32 - Distance Angles C51 1.2252 (0.0081) O32 - Fe31 - Distance Angles C31 2.0324 (0.0070) C39 2.0339 (0.0070) 144.60 (0.29) C35 2.0351 (0.0066) 40.84 (0.28) 174.54 (0.29) C37 2.0446 (0.0064) 108.51 (0.28) 67.73 (0.27) 111.58 (0.28) C34 2.0490 (0.0067) 68.13 (0.28) 136.51 (0.29) 41.14 (0.27) 143.28 (0.29) C38 2.0500 (0.0060) 113.83 (0.27) 40.07 (0.28) 142.49 (0.28) 40.03 (0.27) 176.11 (0.29) C33 2.0502 (0.0064) 68.37 (0.27) 111.97 (0.27) 69.26 (0.28) 174.53 (0.30) 40.57 (0.29) 136.36 (0.28) C36 2.0527 (0.0063) 133.00 (0.27) 68.78 (0.26) 106.95 (0.26) 41.52 (0.25) 112.61 (0.27) 68.77 (0.25) 143.87 (0.26) C40 2.0572 (0.0064) 173.29 (0.29) 40.82 (0.28) 133.73 (0.27) 68.64 (0.26) 110.23 (0.28) 68.23 (0.27) 114.96 (0.26) C32 2.0640 (0.0064) 41.05 (0.27) 115.02 (0.27) 69.56 (0.27) 134.07 (0.27) 68.52 (0.27) 110.53 (0.26) 40.70 (0.27) Fe31 - C31 C39 C35 C37 C34 C38 C33 Br31 - Distance Angles C31 1.8884 (0.0069) Br31 - Br32 - Distance Angles C48 1.8808 (0.0073) Br32 - FMAP and GRID set by program FMAP 2 2 23 GRID -2.500 -2 -2 2.500 2 2 R1 = 0.0485 for 4347 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.89 at 0.0412 0.2267 0.6446 [ 0.81 A from C8 ] Deepest hole -0.61 at 0.0363 0.4043 0.8603 [ 0.79 A from BR32 ] Mean = 0.00, Rms deviation from mean = 0.13 e/A^3, Highest memory used = 5365 / 34721 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.0412 -0.2267 0.1446 1.00000 0.05 0.89 0.81 C8 0.89 C9 1.46 FE1 1.56 H8 Q2 1 0.2392 -0.7194 -0.0621 1.00000 0.05 0.83 0.89 C39 1.03 C38 1.34 FE31 1.58 H39 Q3 1 0.3001 -0.2968 -0.0981 1.00000 0.05 0.76 1.12 C31 1.26 BR31 1.84 C35 2.09 H35 Q4 1 0.9829 0.1311 0.0960 1.00000 0.05 0.72 0.91 C1 1.31 BR1 1.70 C5 2.02 H5 Q5 1 0.2672 -0.0495 0.1796 1.00000 0.05 0.66 0.83 BR2 1.94 C18 2.39 H19 2.45 H33 No peaks closer than 4 Angstroms to each other Time profile in seconds ----------------------- 0.08: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.02: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 2.02: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.13: Set up l.s. refinement 0.00: Generate idealized H-atoms 13.72: Structure factors and derivatives 40.03: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.16: Apply other restraints 5.27: Solve l.s. equations 0.00: Generate HTAB table 0.09: Other dependent quantities, CIF, tables 0.19: Analysis of variance 0.09: Merge reflections for Fourier and .fcf 0.13: Fourier summations 0.09: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s94 finished at 11:17:01 Total CPU time: 62.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++