+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 15:15:45 on 19-Jul-2001 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01SRC618 in P-1 CELL 0.71073 10.6895 13.4060 13.6885 93.628 93.588 113.060 ZERR 4 0.0002 0.0002 0.0002 0.003 0.003 0.003 LATT 1 SFAC C H B O F FE UNIT 76 20 4 8 40 4 V = 1793.08 F(000) = 1024.0 Mu = 0.96 mm-1 Cell Wt = 2087.56 Rho = 1.933 SHEL 7 0.84 ACTA TEMP -153 SIZE 0.2 0.2 0.1 FMAP 2 PLAN 20 L.S. 4 WGHT 0.0000 0.0000 FVAR 0.14268 FE1 6 0.567693 0.245898 0.459209 11.00000 0.01781 0.01835 = 0.01606 0.00124 0.00237 0.00774 FE2 6 0.321340 -0.253849 1.031795 11.00000 0.01812 0.02105 = 0.01550 0.00315 0.00351 0.00868 F16 5 0.123816 -0.106058 1.214271 11.00000 0.03239 0.01932 = 0.02504 0.00567 0.00578 0.01196 F17 5 0.013774 -0.151961 1.387342 11.00000 0.04173 0.02914 = 0.02247 -0.00395 0.00833 0.01847 F6 5 0.368406 0.407363 0.640373 11.00000 0.03348 0.01841 = 0.02834 0.00161 0.00421 0.01250 F20 5 0.029181 -0.478301 1.138366 11.00000 0.03236 0.02006 = 0.02202 -0.00065 0.00845 0.01182 F14 5 -0.300215 -0.356809 0.872135 11.00000 0.01980 0.03869 = 0.02910 -0.00290 -0.00217 0.01109 F15 5 -0.124827 -0.403599 0.991424 11.00000 0.02329 0.02300 = 0.02479 0.00332 0.00319 0.00646 F5 5 0.150722 0.062008 0.469796 11.00000 0.02811 0.02061 = 0.02627 0.00785 -0.00048 0.00603 F19 5 -0.079807 -0.522708 1.310974 11.00000 0.03070 0.01986 = 0.02940 0.00806 0.01107 0.00699 F9 5 0.296329 0.033405 0.805634 11.00000 0.02931 0.03300 = 0.02167 0.01467 0.00725 0.01313 F18 5 -0.084914 -0.360131 1.436710 11.00000 0.02711 0.03456 = 0.01783 0.00504 0.00974 0.01066 F10 5 0.363500 0.052872 0.620117 11.00000 0.02574 0.02101 = 0.02148 0.00342 0.00453 0.01126 F11 5 0.199149 -0.041357 0.997606 11.00000 0.02724 0.02192 = 0.02581 0.00446 0.00043 0.00877 F2 5 0.155394 0.418675 0.301009 11.00000 0.03941 0.02979 = 0.02983 0.00667 -0.00045 0.02218 F1 5 0.375523 0.431726 0.416831 11.00000 0.02875 0.01862 = 0.02919 0.00373 0.00142 0.00772 F12 5 0.024492 0.004013 0.877820 11.00000 0.03700 0.03066 = 0.02632 0.01007 0.00490 0.02047 F3 5 -0.068565 0.227980 0.269897 11.00000 0.02424 0.05013 = 0.02017 0.00139 -0.00311 0.02255 F7 5 0.306848 0.388515 0.828931 11.00000 0.04228 0.03592 = 0.02832 -0.00947 0.00798 0.01930 F4 5 -0.070539 0.050093 0.354303 11.00000 0.02052 0.03672 = 0.03124 0.00329 -0.00632 0.00144 F8 5 0.269096 0.201411 0.911917 11.00000 0.02856 0.04746 = 0.01622 0.00125 0.00754 0.01176 F13 5 -0.228195 -0.151571 0.816010 11.00000 0.03025 0.04864 = 0.02479 0.00524 -0.00171 0.02800 O1 4 0.519803 0.341574 0.282853 11.00000 0.04106 0.03949 = 0.01794 0.01013 0.00769 0.01942 O4 4 0.336379 -0.394370 1.181249 11.00000 0.03464 0.03651 = 0.02418 0.01262 0.00516 0.01917 O3 4 0.416562 -0.056031 1.165348 11.00000 0.02918 0.03145 = 0.03418 -0.01103 -0.00090 0.00910 C31 1 -0.176848 -0.279356 0.901593 11.00000 0.01757 0.03001 = 0.01710 -0.00836 0.00485 0.00786 C12 1 0.040735 0.143454 0.369815 11.00000 0.01731 0.02468 = 0.01457 0.00132 0.00159 0.00314 C20 1 0.244093 -0.299492 0.882356 11.00000 0.02009 0.02549 = 0.01411 -0.00182 0.00241 0.00927 AFIX 43 H20 2 0.150934 -0.322972 0.857856 11.00000 -1.20000 AFIX 0 C13 1 0.154754 0.151998 0.427400 11.00000 0.02162 0.02300 = 0.01247 0.00227 0.00360 0.01154 C33 1 0.083463 -0.289268 1.171018 11.00000 0.01118 0.01826 = 0.01379 0.00254 0.00139 0.00631 C5 1 0.684720 0.338431 0.587318 11.00000 0.01279 0.02103 = 0.02323 0.00005 0.00038 0.00508 AFIX 43 H5 2 0.654550 0.377543 0.633963 11.00000 -1.20000 AFIX 0 C9 1 0.266975 0.335160 0.400669 11.00000 0.01787 0.01697 = 0.01827 -0.00188 0.00334 0.00669 C29 1 -0.012093 -0.097258 0.905912 11.00000 0.02034 0.02008 = 0.01715 0.00137 0.00734 0.00799 C28 1 0.077541 -0.122938 0.965927 11.00000 0.02418 0.02681 = 0.01506 -0.00189 -0.00001 0.01280 C32 1 -0.083992 -0.301374 0.963812 11.00000 0.02256 0.02247 = 0.01538 0.00231 0.00551 0.01309 C30 1 -0.138326 -0.174732 0.874308 11.00000 0.02808 0.03997 = 0.01533 0.00298 0.00357 0.02497 C8 1 0.271762 0.245161 0.444705 11.00000 0.01681 0.01643 = 0.01575 0.00042 0.00425 0.00577 C11 1 0.042404 0.234405 0.327226 11.00000 0.02237 0.03450 = 0.01172 0.00188 0.00175 0.01812 C38 1 0.029403 -0.394860 1.199390 11.00000 0.01602 0.02255 = 0.01483 -0.00179 0.00145 0.00943 C34 1 0.074954 -0.210573 1.237386 11.00000 0.01545 0.01817 = 0.02021 0.00385 0.00025 0.00596 O2 4 0.387485 0.024801 0.383226 11.00000 0.03026 0.02346 = 0.03923 -0.00719 -0.00172 0.01000 C15 1 0.352145 0.313449 0.680416 11.00000 0.01820 0.01735 = 0.02049 0.00099 0.00001 0.00568 C26 1 0.327014 -0.338404 1.123146 11.00000 0.01550 0.03090 = 0.02009 0.00081 0.00544 0.01109 C25 1 0.379261 -0.133567 1.112455 11.00000 0.01963 0.03279 = 0.02160 0.01053 0.00489 0.01249 C35 1 0.018923 -0.231514 1.325445 11.00000 0.01605 0.02268 = 0.01754 -0.00571 0.00047 0.00999 C24 1 0.310364 -0.366563 0.914719 11.00000 0.02936 0.02206 = 0.01630 0.00218 0.00595 0.01103 AFIX 43 H24 2 0.268602 -0.443190 0.917124 11.00000 -1.20000 AFIX 0 C19 1 0.351326 0.138848 0.669664 11.00000 0.01142 0.02267 = 0.01682 0.00001 0.00238 0.00694 B2 3 0.143823 -0.259024 1.067762 11.00000 0.02274 0.00892 = 0.01805 -0.00148 0.00054 0.00421 C27 1 0.045528 -0.225464 0.997102 11.00000 0.02376 0.02052 = 0.01447 0.00237 0.00673 0.01272 C18 1 0.317158 0.127584 0.765307 11.00000 0.01856 0.02377 = 0.01767 0.00662 -0.00034 0.00668 C22 1 0.470380 -0.191813 0.930441 11.00000 0.02614 0.03154 = 0.02118 0.00147 0.00832 0.00726 AFIX 43 H22 2 0.554182 -0.129962 0.944109 11.00000 -1.20000 AFIX 0 C1 1 0.751715 0.378698 0.503641 11.00000 0.01825 0.01810 = 0.02900 0.00242 0.00290 0.00454 AFIX 43 H1 2 0.773745 0.449719 0.483622 11.00000 -1.20000 AFIX 0 C17 1 0.301366 0.210913 0.817902 11.00000 0.02030 0.03507 = 0.01017 0.00118 0.00503 0.00979 C7 1 0.459202 0.112911 0.413512 11.00000 0.03171 0.02824 = 0.01929 0.00475 0.00392 0.02007 C37 1 -0.026928 -0.419250 1.286905 11.00000 0.01591 0.01724 = 0.02295 0.00108 0.00247 0.00495 C10 1 0.155386 0.329984 0.342704 11.00000 0.02878 0.02778 = 0.01555 0.00513 0.00377 0.02016 C36 1 -0.031667 -0.337779 1.350113 11.00000 0.01816 0.02918 = 0.01275 0.00147 0.00430 0.00726 C4 1 0.670748 0.229051 0.588958 11.00000 0.01563 0.02430 = 0.01920 0.00497 0.00073 0.00534 AFIX 43 H4 2 0.628411 0.181429 0.636678 11.00000 -1.20000 AFIX 0 C14 1 0.369760 0.231997 0.623058 11.00000 0.01628 0.02224 = 0.01512 0.00042 -0.00039 0.00756 C2 1 0.780409 0.294700 0.454663 11.00000 0.01462 0.03083 = 0.02342 0.00188 0.00406 0.00680 AFIX 43 H2 2 0.825469 0.299925 0.396364 11.00000 -1.20000 AFIX 0 C6 1 0.537189 0.303584 0.352971 11.00000 0.02216 0.02778 = 0.02185 -0.00296 0.00548 0.01175 C23 1 0.449623 -0.299366 0.942813 11.00000 0.02657 0.03278 = 0.01762 0.00424 0.00819 0.01783 AFIX 43 H23 2 0.517467 -0.323604 0.966173 11.00000 -1.20000 AFIX 0 C16 1 0.320726 0.305922 0.775773 11.00000 0.02025 0.02722 = 0.02186 -0.00885 0.00328 0.01066 C3 1 0.730987 0.202909 0.506920 11.00000 0.01877 0.02831 = 0.02443 -0.00183 -0.00400 0.01199 AFIX 43 H3 2 0.736702 0.135008 0.490444 11.00000 -1.20000 AFIX 0 C21 1 0.342566 -0.191622 0.893446 11.00000 0.03611 0.02737 = 0.01706 0.00766 0.00994 0.01812 AFIX 43 H21 2 0.326623 -0.129040 0.878747 11.00000 -1.20000 AFIX 0 B1 3 0.399592 0.244820 0.510431 11.00000 0.02308 0.00645 = 0.01707 0.00076 0.00414 0.00325 HKLF 4 Covalent radii and connectivity table for 01SRC618 in P-1 C 0.770 H 0.320 B 0.820 O 0.660 F 0.640 FE 1.240 Fe1 - C7 C6 B1 C1 C5 C4 C2 C3 Fe2 - C26 C25 B2 C24 C21 C20 C23 C22 F16 - C34 F17 - C35 F6 - C15 F20 - C38 F14 - C31 F15 - C32 F5 - C13 F19 - C37 F9 - C18 F18 - C36 F10 - C19 F11 - C28 F2 - C10 F1 - C9 F12 - C29 F3 - C11 F7 - C16 F4 - C12 F8 - C17 F13 - C30 O1 - C6 O4 - C26 O3 - C25 C31 - F14 C30 C32 C12 - F4 C13 C11 C20 - C21 C24 Fe2 C13 - F5 C12 C8 C33 - C34 C38 B2 C5 - C1 C4 Fe1 C9 - F1 C10 C8 C29 - F12 C30 C28 C28 - F11 C29 C27 C32 - F15 C27 C31 C30 - F13 C29 C31 C8 - C13 C9 B1 C11 - F3 C10 C12 C38 - F20 C37 C33 C34 - F16 C35 C33 O2 - C7 C15 - F6 C16 C14 C26 - O4 Fe2 C25 - O3 Fe2 C35 - F17 C34 C36 C24 - C23 C20 Fe2 C19 - F10 C18 C14 B2 - C27 C33 Fe2 C27 - C28 C32 B2 C18 - F9 C17 C19 C22 - C23 C21 Fe2 C1 - C5 C2 Fe1 C17 - F8 C18 C16 C7 - O2 Fe1 C37 - F19 C36 C38 C10 - F2 C11 C9 C36 - F18 C37 C35 C4 - C5 C3 Fe1 C14 - C15 C19 B1 C2 - C3 C1 Fe1 C6 - O1 Fe1 C23 - C22 C24 Fe2 C16 - F7 C15 C17 C3 - C2 C4 Fe1 C21 - C20 C22 Fe2 B1 - C8 C14 Fe1 13192 Reflections read, of which 734 rejected -12 =< h =< 12, -15 =< k =< 15, -16 =< l =< 16, Max. 2-theta = 50.05 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 0 0 2 97.59 2.30 3 45.61 1 Inconsistent equivalents 6094 Unique reflections, of which 0 suppressed R(int) = 0.0589 R(sigma) = 0.1042 Friedel opposites merged Maximum memory for data reduction = 3939 / 61588 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 = 5386 / 811629 wR2 = 0.0867 before cycle 1 for 6094 data and 595 / 595 parameters GooF = S = 0.952; Restrained GooF = 0.952 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.14238 0.00016 -1.873 OSF Mean shift/esd = 0.245 Maximum = -1.873 for OSF Max. shift = 0.004 A for C25 Max. dU =-0.001 for C14 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5386 / 811629 wR2 = 0.0859 before cycle 2 for 6094 data and 595 / 595 parameters GooF = S = 0.943; Restrained GooF = 0.943 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.14230 0.00016 -0.512 OSF Mean shift/esd = 0.073 Maximum = -0.512 for OSF Max. shift = 0.001 A for C34 Max. dU = 0.000 for C14 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5386 / 811629 wR2 = 0.0858 before cycle 3 for 6094 data and 595 / 595 parameters GooF = S = 0.942; Restrained GooF = 0.942 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.14230 0.00016 0.020 OSF Mean shift/esd = 0.003 Maximum = 0.027 for U13 C4 Max. shift = 0.000 A for C19 Max. dU = 0.000 for C16 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5386 / 811629 wR2 = 0.0858 before cycle 4 for 6094 data and 595 / 595 parameters GooF = S = 0.942; Restrained GooF = 0.942 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.14230 0.00016 0.023 OSF Mean shift/esd = 0.001 Maximum = 0.023 for OSF Max. shift = 0.000 A for C10 Max. dU = 0.000 for C18 Largest correlation matrix elements 0.681 U12 C30 / U11 C30 0.660 U12 F2 / U11 F2 0.646 U12 F2 / U22 F2 0.679 U12 C10 / U11 C10 0.660 U12 C10 / U22 C10 0.645 U12 C27 / U11 C27 0.676 U12 F13 / U11 F13 0.660 U12 F3 / U11 F3 0.645 U12 F3 / U22 F3 0.669 U12 C7 / U22 C7 0.657 U12 F12 / U11 F12 0.644 U12 F12 / U22 F12 0.667 U12 C11 / U11 C11 0.655 U12 C11 / U22 C11 0.643 U12 C7 / U11 C7 0.665 U12 F13 / U22 F13 0.654 U12 C21 / U22 C21 0.638 U12 C21 / U11 C21 0.662 U12 C30 / U22 C30 0.649 U12 C32 / U11 C32 0.637 U12 F11 / U11 F11 0.661 U12 C23 / U11 C23 0.649 U12 O4 / U11 O4 0.633 U12 C32 / U22 C32 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C20 ** H20 0.1511 -0.3229 0.8581 43 0.950 0.000 C20 C21 C24 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C5 ** H5 0.6551 0.3776 0.6341 43 0.950 0.000 C5 C1 C4 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C24 ** H24 0.2686 -0.4431 0.9171 43 0.950 0.000 C24 C23 C20 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C22 ** H22 0.5542 -0.1300 0.9441 43 0.950 0.000 C22 C23 C21 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C1 ** H1 0.7733 0.4497 0.4836 43 0.950 0.000 C1 C5 C2 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C4 ** H4 0.6277 0.1814 0.6364 43 0.950 0.000 C4 C5 C3 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C2 ** H2 0.8259 0.3002 0.3964 43 0.950 0.000 C2 C3 C1 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C23 ** H23 0.5172 -0.3238 0.9659 43 0.950 0.000 C23 C22 C24 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C3 ** H3 0.7373 0.1352 0.4905 43 0.950 0.000 C3 C2 C4 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C21 ** H21 0.3265 -0.1291 0.8788 43 0.950 0.000 C21 C20 C22 01SRC618 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Fe1 0.56769 0.24589 0.45921 1.00000 0.01765 0.01826 0.01605 0.00117 0.00231 0.00779 0.01710 0.00119 0.00006 0.00004 0.00003 0.00000 0.00036 0.00031 0.00028 0.00022 0.00023 0.00028 0.00015 Fe2 0.32135 -0.25383 1.03181 1.00000 0.01799 0.02095 0.01531 0.00301 0.00347 0.00876 0.01762 0.00120 0.00006 0.00004 0.00003 0.00000 0.00037 0.00032 0.00028 0.00023 0.00023 0.00029 0.00015 F16 0.12374 -0.10609 1.21431 1.00000 0.03212 0.01798 0.02493 0.00534 0.00564 0.01144 0.02426 0.00467 0.00023 0.00016 0.00013 0.00000 0.00159 0.00120 0.00112 0.00092 0.00101 0.00117 0.00053 F17 0.01390 -0.15195 1.38736 1.00000 0.04047 0.02811 0.02211 -0.00347 0.00851 0.01763 0.02900 0.00484 0.00024 0.00017 0.00013 0.00000 0.00173 0.00132 0.00113 0.00099 0.00105 0.00129 0.00057 F6 0.36847 0.40745 0.64039 1.00000 0.03247 0.01899 0.02816 0.00166 0.00411 0.01268 0.02575 0.00465 0.00023 0.00016 0.00013 0.00000 0.00160 0.00121 0.00114 0.00095 0.00103 0.00120 0.00054 F20 0.02920 -0.47830 1.13829 1.00000 0.03239 0.01958 0.02160 -0.00025 0.00862 0.01158 0.02396 0.00464 0.00023 0.00016 0.00013 0.00000 0.00159 0.00119 0.00109 0.00092 0.00100 0.00117 0.00053 F14 -0.30015 -0.35687 0.87205 1.00000 0.01986 0.03797 0.02935 -0.00234 -0.00164 0.01130 0.02955 0.00487 0.00024 0.00018 0.00014 0.00000 0.00156 0.00144 0.00121 0.00106 0.00104 0.00131 0.00056 F15 -0.12497 -0.40356 0.99138 1.00000 0.02329 0.02172 0.02441 0.00349 0.00331 0.00600 0.02395 0.00451 0.00022 0.00016 0.00013 0.00000 0.00150 0.00125 0.00113 0.00095 0.00099 0.00115 0.00052 F5 0.15073 0.06197 0.46982 1.00000 0.02790 0.02015 0.02545 0.00788 -0.00014 0.00603 0.02545 0.00457 0.00023 0.00016 0.00013 0.00000 0.00154 0.00122 0.00113 0.00094 0.00100 0.00116 0.00054 F19 -0.07988 -0.52283 1.31085 1.00000 0.03061 0.01977 0.02881 0.00816 0.01120 0.00700 0.02668 0.00472 0.00023 0.00016 0.00013 0.00000 0.00161 0.00125 0.00118 0.00097 0.00105 0.00119 0.00055 F9 0.29634 0.03337 0.80561 1.00000 0.02889 0.03232 0.02126 0.01454 0.00718 0.01291 0.02648 0.00474 0.00023 0.00016 0.00013 0.00000 0.00158 0.00135 0.00111 0.00098 0.00100 0.00125 0.00055 F18 -0.08491 -0.36001 1.43668 1.00000 0.02706 0.03519 0.01774 0.00549 0.00990 0.01119 0.02653 0.00474 0.00023 0.00017 0.00013 0.00000 0.00157 0.00136 0.00109 0.00097 0.00099 0.00124 0.00055 F10 0.36369 0.05302 0.62008 1.00000 0.02524 0.02117 0.02121 0.00345 0.00463 0.01165 0.02161 0.00453 0.00022 0.00015 0.00013 0.00000 0.00149 0.00120 0.00109 0.00091 0.00096 0.00115 0.00051 F11 0.19917 -0.04133 0.99767 1.00000 0.02695 0.02165 0.02509 0.00455 0.00088 0.00933 0.02463 0.00473 0.00023 0.00016 0.00013 0.00000 0.00158 0.00125 0.00115 0.00097 0.00103 0.00123 0.00053 F2 0.15531 0.41861 0.30087 1.00000 0.03894 0.02922 0.02989 0.00663 0.00005 0.02225 0.02995 0.00491 0.00024 0.00017 0.00014 0.00000 0.00173 0.00132 0.00120 0.00101 0.00108 0.00131 0.00058 F1 0.37546 0.43170 0.41684 1.00000 0.02869 0.01883 0.02870 0.00436 0.00221 0.00838 0.02566 0.00474 0.00024 0.00016 0.00013 0.00000 0.00159 0.00124 0.00117 0.00096 0.00104 0.00122 0.00054 F12 0.02449 0.00409 0.87780 1.00000 0.03689 0.03009 0.02596 0.01015 0.00527 0.02017 0.02839 0.00483 0.00023 0.00017 0.00013 0.00000 0.00171 0.00137 0.00118 0.00101 0.00106 0.00131 0.00058 F3 -0.06865 0.22796 0.26984 1.00000 0.02340 0.04971 0.01949 0.00073 -0.00337 0.02232 0.02881 0.00473 0.00023 0.00017 0.00013 0.00000 0.00154 0.00153 0.00112 0.00102 0.00098 0.00134 0.00057 F7 0.30676 0.38839 0.82890 1.00000 0.04164 0.03554 0.02784 -0.00982 0.00749 0.01948 0.03412 0.00500 0.00025 0.00018 0.00014 0.00000 0.00178 0.00142 0.00120 0.00103 0.00110 0.00137 0.00061 F4 -0.07040 0.05022 0.35433 1.00000 0.02075 0.03615 0.03078 0.00377 -0.00614 0.00124 0.03273 0.00493 0.00024 0.00018 0.00014 0.00000 0.00157 0.00145 0.00124 0.00106 0.00106 0.00129 0.00057 F8 0.26910 0.20151 0.91180 1.00000 0.02868 0.04766 0.01575 0.00167 0.00792 0.01204 0.03146 0.00494 0.00024 0.00018 0.00013 0.00000 0.00163 0.00150 0.00109 0.00100 0.00100 0.00133 0.00058 F13 -0.22824 -0.15165 0.81607 1.00000 0.02992 0.04851 0.02426 0.00502 -0.00190 0.02760 0.03062 0.00489 0.00024 0.00018 0.00013 0.00000 0.00162 0.00151 0.00116 0.00105 0.00104 0.00139 0.00059 O1 0.51996 0.34148 0.28287 1.00000 0.04081 0.04013 0.01747 0.01014 0.00791 0.01986 0.03105 0.00620 0.00030 0.00021 0.00017 0.00000 0.00221 0.00182 0.00139 0.00129 0.00130 0.00169 0.00074 O4 0.33637 -0.39437 1.18132 1.00000 0.03462 0.03675 0.02327 0.01201 0.00503 0.01957 0.02934 0.00603 0.00030 0.00021 0.00017 0.00000 0.00207 0.00176 0.00144 0.00130 0.00130 0.00164 0.00071 O3 0.41647 -0.05606 1.16523 1.00000 0.02876 0.03201 0.03331 -0.01005 -0.00045 0.00888 0.03312 0.00625 0.00030 0.00022 0.00018 0.00000 0.00209 0.00180 0.00160 0.00139 0.00137 0.00164 0.00073 C31 -0.17660 -0.27930 0.90173 1.00000 0.01573 0.02866 0.01621 -0.00877 0.00396 0.00600 0.02147 0.00857 0.00042 0.00032 0.00024 0.00000 0.00263 0.00245 0.00196 0.00175 0.00173 0.00221 0.00092 C12 0.04088 0.14341 0.36997 1.00000 0.01654 0.02331 0.01394 0.00067 0.00054 0.00185 0.01991 0.00846 0.00042 0.00030 0.00024 0.00000 0.00260 0.00231 0.00191 0.00169 0.00169 0.00212 0.00090 C20 0.24430 -0.29944 0.88251 1.00000 0.02000 0.02688 0.01291 -0.00139 0.00270 0.00965 0.01992 0.00849 0.00042 0.00030 0.00022 0.00000 0.00262 0.00238 0.00188 0.00166 0.00166 0.00218 0.00091 H20 0.15110 -0.32294 0.85809 1.00000 0.02391 0.00000 0.00000 C13 0.15499 0.15217 0.42734 1.00000 0.02112 0.02149 0.01153 0.00229 0.00373 0.01096 0.01714 0.00842 0.00041 0.00029 0.00023 0.00000 0.00264 0.00222 0.00183 0.00161 0.00165 0.00212 0.00088 C33 0.08350 -0.28921 1.17086 1.00000 0.01085 0.01695 0.01350 0.00190 0.00158 0.00596 0.01359 0.00795 0.00038 0.00028 0.00023 0.00000 0.00229 0.00204 0.00177 0.00155 0.00155 0.00187 0.00082 C5 0.68495 0.33844 0.58727 1.00000 0.01249 0.02125 0.02220 -0.00045 0.00069 0.00568 0.01912 0.00800 0.00039 0.00029 0.00024 0.00000 0.00242 0.00221 0.00201 0.00168 0.00170 0.00200 0.00089 H5 0.65512 0.37764 0.63408 1.00000 0.02295 0.00000 0.00000 C9 0.26680 0.33506 0.40065 1.00000 0.01671 0.01588 0.01777 -0.00182 0.00335 0.00503 0.01732 0.00830 0.00041 0.00029 0.00023 0.00000 0.00252 0.00214 0.00195 0.00161 0.00167 0.00201 0.00086 C29 -0.01243 -0.09733 0.90602 1.00000 0.02005 0.01982 0.01697 0.00197 0.00728 0.00861 0.01847 0.00870 0.00042 0.00030 0.00024 0.00000 0.00268 0.00223 0.00193 0.00168 0.00174 0.00213 0.00089 C28 0.07750 -0.12300 0.96614 1.00000 0.02187 0.02565 0.01482 -0.00291 0.00063 0.01178 0.02033 0.00868 0.00043 0.00031 0.00024 0.00000 0.00273 0.00238 0.00190 0.00171 0.00173 0.00223 0.00092 C32 -0.08371 -0.30112 0.96374 1.00000 0.02319 0.02168 0.01487 0.00214 0.00543 0.01321 0.01839 0.00868 0.00043 0.00030 0.00024 0.00000 0.00270 0.00226 0.00191 0.00165 0.00172 0.00218 0.00090 C30 -0.13814 -0.17452 0.87434 1.00000 0.02628 0.03779 0.01496 0.00249 0.00341 0.02333 0.02298 0.00928 0.00044 0.00033 0.00024 0.00000 0.00285 0.00266 0.00193 0.00180 0.00177 0.00246 0.00097 C8 0.27186 0.24523 0.44471 1.00000 0.01665 0.01639 0.01395 -0.00013 0.00407 0.00615 0.01574 0.00814 0.00040 0.00029 0.00023 0.00000 0.00249 0.00210 0.00184 0.00156 0.00162 0.00199 0.00085 C11 0.04253 0.23437 0.32724 1.00000 0.02243 0.03455 0.01106 0.00236 0.00188 0.01828 0.02049 0.00894 0.00043 0.00032 0.00023 0.00000 0.00273 0.00256 0.00186 0.00173 0.00168 0.00236 0.00094 C38 0.02933 -0.39478 1.19936 1.00000 0.01589 0.02064 0.01504 -0.00236 0.00134 0.00897 0.01685 0.00806 0.00039 0.00029 0.00023 0.00000 0.00249 0.00220 0.00187 0.00164 0.00164 0.00202 0.00088 C34 0.07463 -0.21064 1.23758 1.00000 0.01438 0.01786 0.02023 0.00403 -0.00026 0.00539 0.01779 0.00819 0.00040 0.00029 0.00024 0.00000 0.00247 0.00216 0.00199 0.00166 0.00168 0.00196 0.00088 O2 0.38757 0.02491 0.38326 1.00000 0.03033 0.02348 0.03795 -0.00640 -0.00095 0.01019 0.03137 0.00631 0.00031 0.00022 0.00018 0.00000 0.00208 0.00173 0.00167 0.00136 0.00141 0.00164 0.00072 C15 0.35208 0.31328 0.68054 1.00000 0.01741 0.01567 0.02107 0.00137 -0.00028 0.00527 0.01857 0.00819 0.00041 0.00029 0.00025 0.00000 0.00254 0.00210 0.00199 0.00163 0.00168 0.00196 0.00089 C26 0.32709 -0.33812 1.12307 1.00000 0.01524 0.02977 0.02091 0.00036 0.00536 0.01108 0.02124 0.00842 0.00040 0.00031 0.00025 0.00000 0.00253 0.00241 0.00204 0.00184 0.00173 0.00214 0.00092 C25 0.37883 -0.13385 1.11244 1.00000 0.01950 0.03165 0.02036 0.00923 0.00499 0.01237 0.02269 0.00932 0.00042 0.00033 0.00026 0.00000 0.00269 0.00253 0.00207 0.00191 0.00180 0.00227 0.00095 C35 0.01892 -0.23162 1.32552 1.00000 0.01614 0.02205 0.01713 -0.00528 0.00068 0.01060 0.01787 0.00819 0.00040 0.00030 0.00024 0.00000 0.00248 0.00223 0.00190 0.00166 0.00166 0.00202 0.00088 C24 0.31037 -0.36650 0.91473 1.00000 0.02785 0.02151 0.01583 0.00151 0.00542 0.01044 0.02139 0.00880 0.00043 0.00031 0.00023 0.00000 0.00286 0.00222 0.00193 0.00165 0.00178 0.00220 0.00093 H24 0.26857 -0.44313 0.91715 1.00000 0.02566 0.00000 0.00000 C19 0.35130 0.13886 0.66966 1.00000 0.01102 0.02161 0.01676 -0.00139 0.00177 0.00643 0.01660 0.00809 0.00039 0.00029 0.00024 0.00000 0.00233 0.00217 0.00189 0.00163 0.00160 0.00195 0.00085 B2 0.14389 -0.25915 1.06775 1.00000 0.02239 0.00769 0.01827 -0.00269 -0.00014 0.00380 0.01707 0.00947 0.00049 0.00032 0.00028 0.00000 0.00298 0.00220 0.00218 0.00173 0.00196 0.00219 0.00101 C27 0.04547 -0.22551 0.99708 1.00000 0.02290 0.01962 0.01342 0.00199 0.00616 0.01250 0.01716 0.00841 0.00041 0.00029 0.00023 0.00000 0.00267 0.00218 0.00185 0.00160 0.00169 0.00212 0.00088 C18 0.31716 0.12777 0.76521 1.00000 0.01801 0.02307 0.01726 0.00675 -0.00045 0.00672 0.01977 0.00838 0.00041 0.00030 0.00024 0.00000 0.00256 0.00223 0.00196 0.00172 0.00169 0.00204 0.00091 C22 0.47037 -0.19184 0.93038 1.00000 0.02519 0.03128 0.02099 0.00204 0.00997 0.00631 0.02701 0.00927 0.00045 0.00032 0.00024 0.00000 0.00287 0.00254 0.00209 0.00181 0.00185 0.00228 0.00100 H22 0.55423 -0.13004 0.94406 1.00000 0.03241 0.00000 0.00000 C1 0.75159 0.37874 0.50367 1.00000 0.01784 0.01722 0.02867 0.00169 0.00287 0.00357 0.02229 0.00831 0.00041 0.00030 0.00025 0.00000 0.00259 0.00216 0.00215 0.00175 0.00183 0.00203 0.00093 H1 0.77326 0.44971 0.48362 1.00000 0.02675 0.00000 0.00000 C17 0.30145 0.21100 0.81773 1.00000 0.01953 0.03424 0.00917 0.00068 0.00465 0.00935 0.02131 0.00848 0.00041 0.00031 0.00023 0.00000 0.00262 0.00249 0.00186 0.00173 0.00165 0.00218 0.00093 C7 0.45941 0.11297 0.41335 1.00000 0.03072 0.02762 0.01798 0.00368 0.00264 0.01945 0.02291 0.00959 0.00045 0.00034 0.00025 0.00000 0.00291 0.00254 0.00202 0.00185 0.00185 0.00243 0.00097 C37 -0.02682 -0.41898 1.28685 1.00000 0.01578 0.01583 0.02112 0.00165 0.00264 0.00433 0.01815 0.00820 0.00040 0.00029 0.00024 0.00000 0.00249 0.00213 0.00198 0.00166 0.00170 0.00196 0.00088 C10 0.15527 0.32996 0.34275 1.00000 0.02736 0.02735 0.01483 0.00565 0.00439 0.01932 0.02027 0.00901 0.00044 0.00031 0.00024 0.00000 0.00283 0.00242 0.00195 0.00173 0.00177 0.00235 0.00094 C36 -0.03166 -0.33768 1.35006 1.00000 0.01701 0.02800 0.01169 0.00236 0.00473 0.00641 0.01951 0.00842 0.00041 0.00031 0.00024 0.00000 0.00253 0.00236 0.00184 0.00167 0.00165 0.00207 0.00090 C4 0.67054 0.22915 0.58885 1.00000 0.01535 0.02329 0.01888 0.00456 0.00082 0.00467 0.02003 0.00808 0.00040 0.00030 0.00024 0.00000 0.00251 0.00225 0.00195 0.00167 0.00170 0.00203 0.00090 H4 0.62774 0.18144 0.63639 1.00000 0.02404 0.00000 0.00000 C14 0.36966 0.23194 0.62292 1.00000 0.01567 0.02095 0.01399 0.00039 -0.00033 0.00807 0.01676 0.00799 0.00040 0.00028 0.00023 0.00000 0.00247 0.00217 0.00182 0.00160 0.00160 0.00200 0.00087 C2 0.78069 0.29486 0.45463 1.00000 0.01384 0.03099 0.02335 0.00195 0.00421 0.00653 0.02338 0.00838 0.00041 0.00030 0.00025 0.00000 0.00254 0.00243 0.00206 0.00183 0.00175 0.00215 0.00094 H2 0.82590 0.30020 0.39640 1.00000 0.02806 0.00000 0.00000 C6 0.53732 0.30343 0.35292 1.00000 0.02137 0.02693 0.02188 -0.00284 0.00544 0.01170 0.02282 0.00861 0.00042 0.00031 0.00026 0.00000 0.00270 0.00237 0.00212 0.00180 0.00178 0.00218 0.00095 C23 0.44935 -0.29947 0.94265 1.00000 0.02817 0.03168 0.01683 0.00407 0.00879 0.01915 0.02292 0.00894 0.00044 0.00031 0.00024 0.00000 0.00294 0.00248 0.00197 0.00175 0.00183 0.00237 0.00098 H23 0.51716 -0.32379 0.96591 1.00000 0.02750 0.00000 0.00000 C16 0.32080 0.30570 0.77577 1.00000 0.02038 0.02659 0.02033 -0.00940 0.00215 0.01092 0.02247 0.00840 0.00042 0.00031 0.00025 0.00000 0.00268 0.00237 0.00204 0.00177 0.00175 0.00218 0.00095 C3 0.73129 0.20307 0.50687 1.00000 0.01908 0.02716 0.02311 -0.00114 -0.00339 0.01184 0.02270 0.00836 0.00041 0.00031 0.00025 0.00000 0.00262 0.00237 0.00203 0.00178 0.00178 0.00217 0.00094 H3 0.73725 0.13525 0.49050 1.00000 0.02724 0.00000 0.00000 C21 0.34253 -0.19161 0.89346 1.00000 0.03488 0.02702 0.01574 0.00701 0.00952 0.01812 0.02351 0.00904 0.00045 0.00031 0.00023 0.00000 0.00297 0.00242 0.00196 0.00171 0.00182 0.00236 0.00098 H21 0.32652 -0.12906 0.87875 1.00000 0.02821 0.00000 0.00000 B1 0.39967 0.24491 0.51036 1.00000 0.02202 0.00505 0.01783 0.00047 0.00394 0.00273 0.01572 0.00939 0.00047 0.00031 0.00028 0.00000 0.00295 0.00211 0.00215 0.00170 0.00192 0.00216 0.00099 Final Structure Factor Calculation for 01SRC618 in P-1 Total number of l.s. parameters = 595 Maximum vector length = 511 Memory required = 4791 / 25039 wR2 = 0.0858 before cycle 5 for 6094 data and 0 / 595 parameters GooF = S = 0.942; Restrained GooF = 0.942 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0431 for 4084 Fo > 4sig(Fo) and 0.0829 for all 6094 data wR2 = 0.0858, GooF = S = 0.942, Restrained GooF = 0.942 for all data Occupancy sum of asymmetric unit = 66.00 for non-hydrogen and 10.00 for hydrogen atoms Principal mean square atomic displacements U 0.0185 0.0175 0.0153 Fe1 0.0212 0.0175 0.0141 Fe2 0.0330 0.0243 0.0155 F16 0.0416 0.0322 0.0132 F17 0.0327 0.0279 0.0166 F6 0.0354 0.0223 0.0141 F20 0.0415 0.0288 0.0184 F14 0.0275 0.0248 0.0196 F15 0.0359 0.0245 0.0159 F5 0.0380 0.0270 0.0149 F19 0.0390 0.0282 0.0123 F9 0.0363 0.0308 0.0125 F18 0.0265 0.0199 0.0184 F10 0.0292 0.0249 0.0198 F11 0.0420 0.0323 0.0156 F2 0.0307 0.0283 0.0181 F1 0.0402 0.0283 0.0167 F12 0.0507 0.0232 0.0126 F3 0.0468 0.0424 0.0132 F7 0.0503 0.0319 0.0160 F4 0.0513 0.0304 0.0127 F8 0.0512 0.0277 0.0129 F13 0.0444 0.0344 0.0143 O1 0.0418 0.0295 0.0167 O4 0.0481 0.0308 0.0205 O3 0.0395 0.0162 0.0087 C31 0.0309 0.0154 0.0134 C12 0.0283 0.0199 0.0116 C20 0.0232 0.0174 0.0108 C13 0.0171 0.0134 0.0103 C33 0.0248 0.0202 0.0124 C5 0.0231 0.0157 0.0132 C9 0.0240 0.0197 0.0117 C29 0.0283 0.0197 0.0130 C28 0.0259 0.0175 0.0118 C32 0.0412 0.0155 0.0123 C30 0.0197 0.0162 0.0113 C8 0.0359 0.0146 0.0110 C11 0.0232 0.0155 0.0118 C38 0.0232 0.0163 0.0139 C34 0.0437 0.0308 0.0196 O2 0.0225 0.0180 0.0153 C15 0.0307 0.0223 0.0107 C26 0.0342 0.0176 0.0163 C25 0.0280 0.0157 0.0100 C35 0.0286 0.0212 0.0143 C24 0.0241 0.0155 0.0103 C19 0.0246 0.0199 0.0067 B2 0.0251 0.0164 0.0099 C27 0.0280 0.0183 0.0129 C18 0.0395 0.0273 0.0142 C22 0.0289 0.0230 0.0150 C1 0.0361 0.0201 0.0077 C17 0.0350 0.0183 0.0154 C7 0.0215 0.0187 0.0143 C37 0.0337 0.0147 0.0124 C10 0.0305 0.0183 0.0097 C36 0.0275 0.0175 0.0151 C4 0.0213 0.0160 0.0129 C14 0.0336 0.0236 0.0129 C2 0.0311 0.0241 0.0133 C6 0.0359 0.0215 0.0114 C23 0.0371 0.0205 0.0099 C16 0.0307 0.0228 0.0146 C3 0.0380 0.0201 0.0125 C21 0.0253 0.0168 0.0050 B1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.017 0.033 0.049 0.068 0.089 0.112 0.140 0.180 0.244 1.000 Number in group 622. 604. 619. 591. 634. 598. 598. 606. 608. 614. GooF 0.767 0.885 0.893 0.984 0.993 0.978 0.984 0.923 0.957 1.039 K 1.538 0.971 0.991 0.964 0.969 0.978 0.986 0.999 1.014 1.010 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.14 1.25 1.43 1.78 inf Number in group 626. 600. 601. 613. 626. 610. 591. 611. 602. 614. GooF 0.835 0.862 0.909 0.899 0.906 0.895 0.876 0.888 1.090 1.203 K 0.985 1.000 1.014 1.013 1.003 1.003 1.018 1.019 1.021 0.988 R1 0.207 0.173 0.150 0.106 0.093 0.076 0.062 0.043 0.036 0.027 Recommended weighting scheme: WGHT 0.0000 0.0000 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) 6 9 1 0.00 464.06 4.93 0.104 0.88 2 3 0 339.74 488.23 4.48 0.107 2.66 2 1 5 6507.17 7314.71 4.11 0.415 2.15 -5 -3 2 21.23 169.23 3.89 0.063 1.54 1 0 6 151.22 89.21 3.88 0.046 2.16 -3 5 3 309.78 396.57 3.80 0.097 2.16 -2 -1 13 382.08 625.06 3.78 0.121 1.04 1 -6 1 345.58 256.01 3.66 0.078 2.18 0 4 0 1287.45 1088.80 3.59 0.160 3.07 1 -2 6 1556.14 1727.95 3.52 0.202 2.17 0 11 5 302.28 599.57 3.43 0.119 1.00 2 4 2 1546.52 1282.29 3.43 0.174 2.05 -2 -1 1 131.35 34.89 3.41 0.029 3.98 -7 -2 3 1254.78 754.51 3.39 0.133 1.25 7 5 4 980.22 1503.45 3.38 0.188 0.97 -6 6 13 486.59 148.85 3.28 0.059 0.89 1 -6 4 4049.93 3646.90 3.28 0.293 1.91 -2 6 13 266.45 37.14 3.26 0.030 0.93 4 -5 6 1303.54 1116.69 3.24 0.162 1.59 -3 7 1 267.55 363.89 3.23 0.093 1.86 -1 -10 10 582.43 358.32 3.23 0.092 0.93 5 -13 7 128.17 285.91 3.22 0.082 0.93 4 -4 4 1834.10 1577.14 3.17 0.193 1.97 1 3 2 78.77 136.41 3.14 0.057 2.87 1 -7 3 2514.78 2281.35 3.14 0.232 1.77 -1 -1 6 60.89 108.27 3.11 0.050 2.22 -4 -3 12 167.37 314.21 3.10 0.086 1.01 -4 8 2 2482.03 2148.91 3.07 0.225 1.56 2 -8 3 174.80 229.59 3.07 0.073 1.60 5 5 2 37.04 152.11 3.06 0.060 1.25 -2 0 6 143.66 200.70 3.06 0.069 2.14 -1 -7 2 910.19 1072.45 3.05 0.159 1.61 -7 5 3 6861.60 6122.02 3.05 0.379 1.44 1 4 7 1324.09 1122.44 3.05 0.162 1.49 5 1 9 1029.26 787.00 3.04 0.136 1.11 -12 3 4 503.69 967.45 3.02 0.151 0.86 -4 4 11 1165.38 1409.23 2.98 0.182 1.11 -6 5 4 4339.76 3979.78 2.98 0.306 1.55 -4 6 0 9784.55 10894.37 2.97 0.506 2.01 -6 4 0 939.72 771.03 2.96 0.135 1.76 -2 1 2 14600.99 16323.31 2.96 0.620 4.33 -4 7 3 5350.67 4917.57 2.95 0.340 1.66 4 -11 7 501.17 637.88 2.95 0.122 1.06 -6 8 12 84.94 279.23 2.93 0.081 0.89 12 -3 3 158.52 311.10 2.92 0.086 0.84 1 -5 8 1756.84 1932.19 2.91 0.213 1.48 -2 7 2 -13.31 55.03 2.90 0.036 1.81 -10 1 6 410.85 797.55 2.89 0.137 0.95 -2 -6 12 217.89 27.98 2.88 0.026 0.99 -2 -1 6 3.37 87.03 2.84 0.045 2.08 Bond lengths and angles Fe1 - Distance Angles C7 1.7495 (0.0044) C6 1.7596 (0.0037) 93.98 (0.17) B1 1.9638 (0.0044) 82.27 (0.17) 91.48 (0.17) C1 2.0921 (0.0040) 157.88 (0.16) 92.98 (0.17) 118.51 (0.15) C5 2.1012 (0.0035) 142.13 (0.14) 123.54 (0.15) 91.00 (0.16) 39.29 (0.13) C4 2.0995 (0.0033) 105.12 (0.15) 158.78 (0.17) 100.04 (0.15) 65.87 (0.14) 39.33 (0.12) C2 2.1144 (0.0040) 118.68 (0.16) 97.36 (0.17) 156.37 (0.16) 39.46 (0.13) 65.86 (0.14) 65.53 (0.14) C3 2.1223 (0.0036) 94.39 (0.16) 131.47 (0.16) 137.01 (0.15) 65.57 (0.14) 65.85 (0.13) 39.37 (0.13) 38.53 (0.13) Fe1 - C7 C6 B1 C1 C5 C4 C2 Fe2 - Distance Angles C26 1.7506 (0.0037) C25 1.7603 (0.0041) 95.00 (0.16) B2 1.9649 (0.0046) 91.20 (0.16) 80.99 (0.17) C24 2.0965 (0.0034) 94.65 (0.14) 161.25 (0.17) 114.84 (0.17) C21 2.1069 (0.0033) 158.26 (0.14) 101.84 (0.15) 104.85 (0.15) 65.48 (0.14) C20 2.1132 (0.0033) 128.21 (0.16) 136.38 (0.14) 91.16 (0.16) 39.36 (0.12) 38.94 (0.14) C23 2.1229 (0.0035) 94.17 (0.14) 123.93 (0.18) 153.79 (0.17) 39.16 (0.15) 65.02 (0.13) 65.54 (0.14) C22 2.1311 (0.0039) 125.66 (0.16) 96.02 (0.17) 143.09 (0.15) 65.33 (0.15) 39.38 (0.14) 65.71 (0.15) 38.25 (0.13) Fe2 - C26 C25 B2 C24 C21 C20 C23 F16 - Distance Angles C34 1.3575 (0.0038) F16 - F17 - Distance Angles C35 1.3403 (0.0035) F17 - F6 - Distance Angles C15 1.3613 (0.0036) F6 - F20 - Distance Angles C38 1.3537 (0.0035) F20 - F14 - Distance Angles C31 1.3395 (0.0044) F14 - F15 - Distance Angles C32 1.3549 (0.0038) F15 - F5 - Distance Angles C13 1.3608 (0.0036) F5 - F19 - Distance Angles C37 1.3531 (0.0038) F19 - F9 - Distance Angles C18 1.3566 (0.0037) F9 - F18 - Distance Angles C36 1.3474 (0.0036) F18 - F10 - Distance Angles C19 1.3544 (0.0034) F10 - F11 - Distance Angles C28 1.3531 (0.0044) F11 - F2 - Distance Angles C10 1.3516 (0.0036) F2 - F1 - Distance Angles C9 1.3525 (0.0042) F1 - F12 - Distance Angles C29 1.3486 (0.0038) F12 - F3 - Distance Angles C11 1.3535 (0.0039) F3 - F7 - Distance Angles C16 1.3499 (0.0036) F7 - F4 - Distance Angles C12 1.3385 (0.0043) F4 - F8 - Distance Angles C17 1.3550 (0.0036) F8 - F13 - Distance Angles C30 1.3505 (0.0037) F13 - O1 - Distance Angles C6 1.1523 (0.0036) O1 - O4 - Distance Angles C26 1.1572 (0.0036) O4 - O3 - Distance Angles C25 1.1450 (0.0041) O3 - C31 - Distance Angles F14 1.3395 (0.0044) C30 1.3844 (0.0051) 121.41 (0.34) C32 1.3947 (0.0047) 120.75 (0.34) 117.82 (0.38) C31 - F14 C30 C12 - Distance Angles F4 1.3385 (0.0043) C13 1.3691 (0.0049) 122.17 (0.31) C11 1.3799 (0.0046) 119.71 (0.33) 118.12 (0.38) C12 - F4 C13 C20 - Distance Angles C21 1.4066 (0.0053) C24 1.4179 (0.0046) 107.19 (0.36) Fe2 2.1132 (0.0033) 70.29 (0.20) 69.68 (0.19) C20 - C21 C24 C13 - Distance Angles F5 1.3608 (0.0036) C12 1.3691 (0.0049) 117.23 (0.35) C8 1.3704 (0.0052) 118.36 (0.31) 124.41 (0.32) C13 - F5 C12 C33 - Distance Angles C34 1.3856 (0.0044) C38 1.3953 (0.0046) 114.51 (0.30) B2 1.5979 (0.0050) 121.34 (0.30) 124.06 (0.29) C33 - C34 C38 C5 - Distance Angles C1 1.4098 (0.0048) C4 1.4137 (0.0045) 107.63 (0.30) Fe1 2.1012 (0.0035) 70.01 (0.20) 70.27 (0.20) C5 - C1 C4 C9 - Distance Angles F1 1.3525 (0.0042) C10 1.3658 (0.0049) 118.20 (0.30) C8 1.3985 (0.0044) 119.12 (0.32) 122.68 (0.38) C9 - F1 C10 C29 - Distance Angles F12 1.3486 (0.0038) C30 1.3585 (0.0055) 119.56 (0.32) C28 1.3841 (0.0047) 120.28 (0.36) 120.15 (0.35) C29 - F12 C30 C28 - Distance Angles F11 1.3531 (0.0044) C29 1.3841 (0.0047) 117.03 (0.32) C27 1.3815 (0.0047) 120.10 (0.31) 122.82 (0.39) C28 - F11 C29 C32 - Distance Angles F15 1.3549 (0.0038) C27 1.3815 (0.0054) 119.27 (0.30) C31 1.3947 (0.0047) 116.70 (0.36) 124.03 (0.34) C32 - F15 C27 C30 - Distance Angles F13 1.3505 (0.0037) C29 1.3585 (0.0055) 121.44 (0.34) C31 1.3844 (0.0051) 118.44 (0.38) 120.12 (0.34) C30 - F13 C29 C8 - Distance Angles C13 1.3704 (0.0052) C9 1.3985 (0.0044) 114.87 (0.33) B1 1.5892 (0.0053) 119.97 (0.29) 125.16 (0.35) C8 - C13 C9 C11 - Distance Angles F3 1.3535 (0.0039) C10 1.3650 (0.0054) 120.30 (0.30) C12 1.3799 (0.0046) 119.41 (0.37) 120.30 (0.34) C11 - F3 C10 C38 - Distance Angles F20 1.3537 (0.0035) C37 1.3734 (0.0046) 117.69 (0.30) C33 1.3953 (0.0046) 119.40 (0.29) 122.89 (0.30) C38 - F20 C37 C34 - Distance Angles F16 1.3575 (0.0038) C35 1.3726 (0.0046) 117.81 (0.29) C33 1.3856 (0.0044) 117.88 (0.30) 124.31 (0.32) C34 - F16 C35 O2 - Distance Angles C7 1.1583 (0.0044) O2 - C15 - Distance Angles F6 1.3613 (0.0036) C16 1.3660 (0.0047) 117.70 (0.30) C14 1.3845 (0.0044) 118.11 (0.29) 124.18 (0.32) C15 - F6 C16 C26 - Distance Angles O4 1.1572 (0.0036) Fe2 1.7506 (0.0037) 176.57 (0.33) C26 - O4 C25 - Distance Angles O3 1.1450 (0.0041) Fe2 1.7603 (0.0041) 179.65 (0.34) C25 - O3 C35 - Distance Angles F17 1.3403 (0.0035) C34 1.3726 (0.0047) 121.57 (0.32) C36 1.3812 (0.0049) 120.00 (0.31) 118.43 (0.31) C35 - F17 C34 C24 - Distance Angles C23 1.4143 (0.0055) C20 1.4179 (0.0046) 108.11 (0.35) Fe2 2.0965 (0.0033) 71.43 (0.20) 70.95 (0.19) C24 - C23 C20 C19 - Distance Angles F10 1.3544 (0.0034) C18 1.3812 (0.0044) 117.34 (0.29) C14 1.3892 (0.0045) 119.67 (0.28) 122.97 (0.31) C19 - F10 C18 B2 - Distance Angles C27 1.5955 (0.0051) C33 1.5979 (0.0050) 111.42 (0.31) Fe2 1.9649 (0.0046) 122.67 (0.27) 125.80 (0.25) B2 - C27 C33 C27 - Distance Angles C28 1.3815 (0.0047) C32 1.3815 (0.0054) 115.03 (0.32) B2 1.5955 (0.0051) 124.99 (0.36) 119.96 (0.32) C27 - C28 C32 C18 - Distance Angles F9 1.3566 (0.0036) C17 1.3603 (0.0046) 120.22 (0.30) C19 1.3812 (0.0044) 120.10 (0.30) 119.66 (0.31) C18 - F9 C17 C22 - Distance Angles C23 1.3936 (0.0048) C21 1.4282 (0.0052) 107.34 (0.38) Fe2 2.1311 (0.0039) 70.56 (0.22) 69.40 (0.22) C22 - C23 C21 C1 - Distance Angles C5 1.4098 (0.0048) C2 1.4201 (0.0045) 108.16 (0.31) Fe1 2.0921 (0.0040) 70.70 (0.22) 71.12 (0.22) C1 - C5 C2 C17 - Distance Angles F8 1.3550 (0.0036) C18 1.3603 (0.0046) 120.25 (0.31) C16 1.3733 (0.0048) 119.90 (0.31) 119.84 (0.31) C17 - F8 C18 C7 - Distance Angles O2 1.1583 (0.0044) Fe1 1.7495 (0.0044) 179.79 (0.44) C7 - O2 C37 - Distance Angles F19 1.3531 (0.0038) C36 1.3674 (0.0045) 119.27 (0.31) C38 1.3734 (0.0046) 120.86 (0.29) 119.86 (0.32) C37 - F19 C36 C10 - Distance Angles F2 1.3516 (0.0036) C11 1.3650 (0.0054) 119.71 (0.32) C9 1.3658 (0.0049) 120.68 (0.37) 119.61 (0.31) C10 - F2 C11 C36 - Distance Angles F18 1.3474 (0.0036) C37 1.3674 (0.0045) 120.51 (0.32) C35 1.3812 (0.0049) 119.50 (0.30) 119.99 (0.32) C36 - F18 C37 C4 - Distance Angles C5 1.4137 (0.0045) C3 1.4223 (0.0048) 108.09 (0.33) Fe1 2.0995 (0.0033) 70.40 (0.19) 71.18 (0.19) C4 - C5 C3 C14 - Distance Angles C15 1.3845 (0.0044) C19 1.3892 (0.0045) 114.31 (0.30) B1 1.5998 (0.0048) 121.17 (0.28) 124.42 (0.29) C14 - C15 C19 C2 - Distance Angles C3 1.3978 (0.0049) C1 1.4201 (0.0045) 108.18 (0.32) Fe1 2.1144 (0.0040) 71.04 (0.23) 69.43 (0.22) C2 - C3 C1 C6 - Distance Angles O1 1.1523 (0.0037) Fe1 1.7596 (0.0037) 178.67 (0.35) C6 - O1 C23 - Distance Angles C22 1.3936 (0.0048) C24 1.4143 (0.0055) 108.72 (0.33) Fe2 2.1229 (0.0035) 71.19 (0.21) 69.41 (0.21) C23 - C22 C24 C16 - Distance Angles F7 1.3499 (0.0036) C15 1.3660 (0.0047) 121.57 (0.32) C17 1.3733 (0.0048) 119.41 (0.31) 119.01 (0.31) C16 - F7 C15 C3 - Distance Angles C2 1.3978 (0.0049) C4 1.4223 (0.0048) 107.94 (0.32) Fe1 2.1223 (0.0036) 70.43 (0.20) 69.45 (0.20) C3 - C2 C4 C21 - Distance Angles C20 1.4066 (0.0053) C22 1.4282 (0.0052) 108.62 (0.31) Fe2 2.1069 (0.0033) 70.77 (0.19) 71.22 (0.19) C21 - C20 C22 B1 - Distance Angles C8 1.5892 (0.0053) C14 1.5998 (0.0048) 111.60 (0.30) Fe1 1.9638 (0.0044) 124.75 (0.25) 123.40 (0.26) B1 - C8 C14 FMAP and GRID set by program FMAP 2 3 34 GRID -1.613 -2 -2 1.613 2 2 R1 = 0.0807 for 6094 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.36 at 0.3131 0.7772 0.1292 [ 1.17 A from C25 ] Deepest hole -0.43 at 0.6887 0.2181 0.0048 [ 0.75 A from FE2 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 4361 / 28375 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3131 -0.2228 1.1292 1.00000 0.05 0.36 1.17 C25 1.39 FE2 1.61 C26 1.81 B2 Q2 1 -0.0847 -0.2585 1.3988 1.00000 0.05 0.34 1.43 F17 1.49 F18 1.49 C35 1.52 C36 Q3 1 0.1177 0.1585 0.2814 1.00000 0.05 0.33 1.49 C12 1.64 C11 1.86 F13 2.03 C13 Q4 1 0.4216 -0.1044 1.0027 1.00000 0.05 0.32 1.62 C25 1.74 C22 1.78 C21 1.81 H22 Q5 1 0.3591 0.2781 0.8109 1.00000 0.05 0.31 0.81 C16 0.88 C17 1.78 F7 1.86 F8 Q6 1 0.4555 0.2947 0.2186 1.00000 0.05 0.31 1.08 O1 1.96 C6 2.43 F13 2.44 F14 Q7 1 0.4256 0.4973 0.8376 1.00000 0.05 0.31 1.51 F7 2.41 H24 2.43 C16 2.68 H23 Q8 1 0.2582 -0.0770 0.7252 1.00000 0.05 0.30 1.68 F9 2.24 F3 2.31 F10 2.38 F4 Q9 1 0.4436 0.4572 0.7581 1.00000 0.05 0.30 1.72 F6 1.78 F7 1.98 C16 1.98 C15 Q10 1 0.6242 0.3329 0.4334 1.00000 0.05 0.30 1.17 FE1 1.33 C6 1.50 C1 1.80 H1 Q11 1 0.3144 -0.1433 0.8235 1.00000 0.05 0.29 0.76 H21 1.27 C21 2.16 C20 2.45 C22 Q12 1 -0.0954 -0.3518 0.9824 1.00000 0.05 0.29 0.66 F15 0.71 C32 1.76 C27 1.90 C31 Q13 1 0.1579 0.2664 0.2727 1.00000 0.05 0.29 1.25 C10 1.42 C11 1.99 C9 2.06 F2 Q14 1 0.0144 -0.2775 0.9582 1.00000 0.05 0.29 0.79 C27 0.98 C32 1.87 F15 1.90 C28 Q15 1 0.5180 0.4608 0.2719 1.00000 0.05 0.29 1.62 O1 1.98 F6 2.52 C6 2.53 F1 Q16 1 0.3312 -0.3728 1.0059 1.00000 0.05 0.29 1.27 C24 1.44 H24 1.61 C23 1.65 C26 Q17 1 0.2223 -0.4551 1.2062 1.00000 0.05 0.29 1.26 O4 2.00 C26 2.11 F20 2.12 F2 Q18 1 0.1603 0.1401 0.8580 1.00000 0.05 0.29 1.28 F8 1.59 C17 1.88 F12 2.22 C18 Q19 1 0.3574 0.1824 0.8019 1.00000 0.05 0.29 0.81 C18 0.86 C17 1.85 F9 1.86 C19 Q20 1 0.2599 0.3013 0.3278 1.00000 0.05 0.29 1.06 C9 1.34 C10 1.83 C8 1.98 F1 Shortest distances between peaks (including symmetry equivalents) 9 15 1.13 13 20 1.20 7 9 1.24 5 19 1.27 12 14 1.29 3 13 1.35 7 15 1.70 8 11 1.85 3 20 1.95 6 15 2.12 18 19 2.16 5 18 2.37 5 9 2.39 1 4 2.45 4 11 2.57 1 16 2.62 4 4 2.65 6 20 2.67 5 7 2.73 6 7 2.76 15 20 2.94 Time profile in seconds ----------------------- 0.11: 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. 0.32: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 3.17: Structure factors and derivatives 27.30: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 6.39: Solve l.s. equations 0.00: Generate HTAB table 0.09: Other dependent quantities, CIF, tables 0.22: Analysis of variance 0.11: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.11: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 15:16:23 Total elapsed time: 38.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++