+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 11:18:24 on 23-May-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 02SRC310 in P2(1)/c CELL 0.71073 13.9569 14.6122 20.0025 90.000 98.683 90.000 ZERR 4.00 0.0002 0.0002 0.0004 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H P CL FE RU UNIT 172 152 8 24 4 4 V = 4032.58 F(000) = 1992.0 Mu = 1.24 mm-1 Cell Wt = 3945.18 Rho = 1.625 MERG 2 OMIT -3.00 55.00 OMIT 4 4 5 FMAP 2 PLAN 10 SIZE 0.06 0.14 0.18 ACTA BOND $H WGHT 0.04320 2.97470 L.S. 4 TEMP -153.00 FVAR 0.11388 C1 1 0.906463 0.479571 0.095197 11.00000 0.02009 0.01938 = 0.01939 -0.00061 0.00857 0.00323 C2 1 0.858827 0.507640 0.029355 11.00000 0.03120 0.02414 = 0.01901 -0.00026 0.00684 0.00529 AFIX 43 H2 2 0.808642 0.475274 0.001743 11.00000 -1.20000 AFIX 0 C3 1 0.900066 0.592211 0.012965 11.00000 0.04301 0.02709 = 0.02560 0.00812 0.02043 0.01082 AFIX 43 H3 2 0.882084 0.625967 -0.027579 11.00000 -1.20000 AFIX 0 C4 1 0.971670 0.617381 0.066658 11.00000 0.02687 0.02466 = 0.03719 0.00340 0.01904 0.00192 AFIX 43 H4 2 1.010412 0.671048 0.068603 11.00000 -1.20000 AFIX 0 C5 1 0.976622 0.549321 0.117615 11.00000 0.01666 0.02152 = 0.03057 0.00025 0.00920 0.00196 AFIX 43 H5 2 1.019103 0.549757 0.159466 11.00000 -1.20000 AFIX 0 C6 1 0.743675 0.591673 0.164167 11.00000 0.01735 0.01775 = 0.01984 0.00105 0.00494 0.00397 C7 1 0.698248 0.629895 0.101103 11.00000 0.01731 0.02187 = 0.02223 0.00370 0.00180 0.00531 AFIX 43 H7 2 0.644634 0.604419 0.072179 11.00000 -1.20000 AFIX 0 C9 1 0.820544 0.727595 0.144846 11.00000 0.02683 0.01515 = 0.02842 0.00029 0.00888 0.00155 AFIX 43 H9 2 0.863546 0.778365 0.149986 11.00000 -1.20000 AFIX 0 C10 1 0.819384 0.654648 0.191582 11.00000 0.02144 0.01869 = 0.01723 -0.00109 0.00425 0.00372 AFIX 43 H10 2 0.861041 0.648331 0.233504 11.00000 -1.20000 AFIX 0 C11 1 0.815242 0.299155 0.084125 11.00000 0.01574 0.01972 = 0.01953 -0.00237 -0.00027 0.00496 C12 1 0.747068 0.244221 0.108792 11.00000 0.02198 0.02188 = 0.02163 -0.00207 0.00062 0.00098 AFIX 43 H12 2 0.740447 0.246603 0.155336 11.00000 -1.20000 AFIX 0 C13 1 0.688687 0.185915 0.065469 11.00000 0.02052 0.02478 = 0.04423 -0.00526 -0.00001 0.00236 AFIX 43 H13 2 0.641920 0.148848 0.082494 11.00000 -1.20000 AFIX 0 C14 1 0.698031 0.181451 -0.001632 11.00000 0.03183 0.03078 = 0.04105 -0.01311 -0.01386 0.00795 AFIX 43 H14 2 0.657563 0.141557 -0.030939 11.00000 -1.20000 AFIX 0 C15 1 0.766464 0.235045 -0.026984 11.00000 0.04022 0.03369 = 0.02190 -0.00925 -0.00599 0.01115 AFIX 43 H15 2 0.772856 0.231814 -0.073541 11.00000 -1.20000 AFIX 0 C16 1 0.825447 0.293298 0.015864 11.00000 0.02770 0.02516 = 0.01944 -0.00277 -0.00054 0.00580 AFIX 43 H16 2 0.872935 0.329325 -0.001273 11.00000 -1.20000 AFIX 0 C17 1 1.012419 0.324990 0.148435 11.00000 0.01623 0.01977 = 0.01598 0.00075 0.00455 0.00092 C18 1 1.090477 0.368281 0.187788 11.00000 0.01927 0.02020 = 0.02581 -0.00279 0.00198 0.00156 AFIX 43 H18 2 1.079848 0.422297 0.212062 11.00000 -1.20000 AFIX 0 C19 1 1.183268 0.333139 0.191733 11.00000 0.01891 0.02212 = 0.03067 0.00175 -0.00020 -0.00286 AFIX 43 H19 2 1.236116 0.363952 0.217799 11.00000 -1.20000 AFIX 0 C20 1 1.199400 0.253385 0.157906 11.00000 0.01794 0.02662 = 0.02554 0.00451 0.00408 0.00575 AFIX 43 H20 2 1.263201 0.229676 0.160259 11.00000 -1.20000 AFIX 0 C21 1 1.122240 0.208554 0.120757 11.00000 0.02705 0.02179 = 0.02532 -0.00283 0.00526 0.00542 AFIX 43 H21 2 1.132912 0.153044 0.098279 11.00000 -1.20000 AFIX 0 C22 1 1.028954 0.243812 0.115879 11.00000 0.02138 0.01989 = 0.02072 -0.00016 0.00186 0.00150 AFIX 43 H22 2 0.976301 0.212278 0.090183 11.00000 -1.20000 AFIX 0 C23 1 0.611982 0.439486 0.148267 11.00000 0.01821 0.01500 = 0.02304 0.00154 -0.00232 0.00210 C24 1 0.616930 0.428647 0.079545 11.00000 0.02389 0.02188 = 0.02332 0.00055 -0.00165 0.00439 AFIX 43 H24 2 0.671810 0.450942 0.061715 11.00000 -1.20000 AFIX 0 C25 1 0.543135 0.385961 0.037144 11.00000 0.04101 0.02555 = 0.02529 0.00245 -0.01088 0.00088 AFIX 43 H25 2 0.546836 0.379935 -0.009687 11.00000 -1.20000 AFIX 0 C26 1 0.464394 0.352242 0.062797 11.00000 0.03843 0.02601 = 0.03746 0.00622 -0.01651 -0.01016 AFIX 43 H26 2 0.413739 0.322650 0.033637 11.00000 -1.20000 AFIX 0 C27 1 0.458450 0.361100 0.130660 11.00000 0.02555 0.03342 = 0.03897 0.01000 -0.00501 -0.01205 AFIX 43 H27 2 0.403826 0.337350 0.148038 11.00000 -1.20000 AFIX 0 C28 1 0.531771 0.404499 0.173748 11.00000 0.02663 0.02308 = 0.02631 0.00415 -0.00014 -0.00232 AFIX 43 H28 2 0.527360 0.410371 0.220485 11.00000 -1.20000 AFIX 0 C29 1 0.657264 0.539010 0.274170 11.00000 0.01483 0.01480 = 0.02790 0.00057 0.00940 -0.00319 C30 1 0.575834 0.594318 0.257992 11.00000 0.01870 0.02134 = 0.02569 0.00223 0.00613 -0.00044 AFIX 43 H30 2 0.548895 0.603464 0.211960 11.00000 -1.20000 AFIX 0 C31 1 0.533581 0.636353 0.308874 11.00000 0.01934 0.02141 = 0.04114 -0.00037 0.01149 0.00242 AFIX 43 H31 2 0.478307 0.674382 0.297545 11.00000 -1.20000 AFIX 0 C32 1 0.572516 0.622483 0.376182 11.00000 0.02516 0.02259 = 0.03211 -0.00657 0.01387 -0.00458 AFIX 43 H32 2 0.543226 0.650277 0.410982 11.00000 -1.20000 AFIX 0 C33 1 0.653909 0.568241 0.392634 11.00000 0.02574 0.02449 = 0.02245 -0.00582 0.00815 -0.00767 AFIX 43 H33 2 0.680469 0.559126 0.438742 11.00000 -1.20000 AFIX 0 C34 1 0.697050 0.526993 0.342049 11.00000 0.01749 0.01767 = 0.02193 -0.00058 0.00418 -0.00258 AFIX 43 H34 2 0.753558 0.490646 0.353610 11.00000 -1.20000 AFIX 0 C35 1 0.916064 0.462515 0.273550 11.00000 0.01881 0.01622 = 0.01679 0.00098 0.00467 0.00395 C36 1 0.977832 0.457426 0.339225 11.00000 0.01744 0.01827 = 0.01716 -0.00231 0.00253 0.00006 C37 1 1.056162 0.518077 0.352143 11.00000 0.02956 0.02628 = 0.02371 0.00139 0.00270 -0.00850 AFIX 43 H37 2 1.065864 0.562877 0.319403 11.00000 -1.20000 AFIX 0 C38 1 1.119488 0.513089 0.412338 11.00000 0.03419 0.05030 = 0.03020 0.00157 -0.00876 -0.02316 AFIX 43 H38 2 1.173664 0.553095 0.420323 11.00000 -1.20000 AFIX 0 C39 1 1.103839 0.450345 0.460341 11.00000 0.03932 0.04892 = 0.02567 0.00424 -0.01309 -0.01515 AFIX 43 H39 2 1.147255 0.447566 0.501722 11.00000 -1.20000 AFIX 0 C40 1 1.025950 0.390963 0.449634 11.00000 0.04079 0.03227 = 0.01819 0.00547 -0.00098 -0.00716 AFIX 43 H40 2 1.015640 0.348215 0.483618 11.00000 -1.20000 AFIX 0 C41 1 0.963281 0.394075 0.389381 11.00000 0.02650 0.02643 = 0.01757 0.00013 0.00153 -0.00707 AFIX 43 H41 2 0.909933 0.353057 0.381805 11.00000 -1.20000 AFIX 0 C42 1 0.248089 0.582018 0.176883 11.00000 0.02935 0.02853 = 0.06490 0.00327 0.00636 0.00635 AFIX 23 H42A 2 0.191421 0.545567 0.156327 11.00000 -1.20000 H42B 2 0.228681 0.647244 0.174864 11.00000 -1.20000 AFIX 0 C43 1 0.526620 0.900693 0.144842 11.00000 0.03731 0.03824 = 0.03898 0.00499 0.00924 0.00731 AFIX 23 H43A 2 0.541873 0.955278 0.173815 11.00000 -1.20000 H43B 2 0.455572 0.891394 0.138740 11.00000 -1.20000 AFIX 0 C78 1 0.746902 0.711873 0.089404 11.00000 0.02699 0.01990 = 0.02400 0.00611 0.00778 0.00609 AFIX 43 H78 2 0.732478 0.750002 0.050725 11.00000 -1.20000 AFIX 0 P1 3 0.890952 0.375355 0.142123 11.00000 0.01481 0.01648 = 0.01407 -0.00066 0.00218 0.00116 P2 3 0.713431 0.487917 0.205854 11.00000 0.01476 0.01664 = 0.01476 0.00029 0.00227 -0.00001 CL1 4 0.913549 0.235305 0.268197 11.00000 0.02272 0.01835 = 0.02429 0.00388 0.00376 0.00411 CL2 4 0.702381 0.314928 0.297976 11.00000 0.02180 0.02326 = 0.02276 0.00644 0.00783 0.00088 CL3 4 0.279596 0.549468 0.262852 11.00000 0.05493 0.03650 = 0.05838 -0.00586 -0.00277 -0.00014 CL4 4 0.341316 0.566903 0.129726 11.00000 0.04554 0.13928 = 0.06160 -0.02260 0.00298 0.04336 CL5 4 0.583662 0.805399 0.185742 11.00000 0.04889 0.03792 = 0.04767 0.00681 0.01437 0.01758 CL6 4 0.562223 0.921269 0.065338 11.00000 0.07464 0.06321 = 0.04703 0.01526 0.02918 0.01794 FE1 5 0.841995 0.603988 0.100552 11.00000 0.01918 0.01802 = 0.01728 0.00290 0.00615 0.00242 RU1 6 0.825959 0.374962 0.239271 11.00000 0.01463 0.01546 = 0.01307 0.00099 0.00196 0.00065 H35 2 0.924996 0.512960 0.252224 11.00000 0.01841 HKLF 4 Covalent radii and connectivity table for 02SRC310 in P2(1)/c C 0.770 H 0.320 P 1.100 CL 0.990 FE 1.240 RU 1.330 C1 - C5 C2 P1 Fe1 C2 - C3 C1 Fe1 C3 - C4 C2 Fe1 C4 - C3 C5 Fe1 C5 - C4 C1 Fe1 C6 - C7 C10 P2 Fe1 C7 - C78 C6 Fe1 C9 - C78 C10 Fe1 C10 - C9 C6 Fe1 C11 - C12 C16 P1 C12 - C13 C11 C13 - C14 C12 C14 - C13 C15 C15 - C16 C14 C16 - C15 C11 C17 - C22 C18 P1 C18 - C19 C17 C19 - C20 C18 C20 - C21 C19 C21 - C20 C22 C22 - C17 C21 C23 - C28 C24 P2 C24 - C25 C23 C25 - C26 C24 C26 - C25 C27 C27 - C26 C28 C28 - C27 C23 C29 - C30 C34 P2 C30 - C29 C31 C31 - C32 C30 C32 - C33 C31 C33 - C32 C34 C34 - C33 C29 C35 - C36 Ru1 C36 - C37 C41 C35 C37 - C38 C36 C38 - C39 C37 C39 - C38 C40 C40 - C41 C39 C41 - C40 C36 C42 - Cl4 Cl3 C43 - Cl5 Cl6 C78 - C9 C7 Fe1 P1 - C1 C11 C17 Ru1 P2 - C6 C23 C29 Ru1 Cl1 - Ru1 Cl2 - Ru1 Cl3 - C42 Cl4 - C42 Cl5 - C43 Cl6 - C43 Fe1 - C6 C5 C10 C4 C1 C2 C7 C3 C78 C9 Ru1 - C35 P1 P2 Cl2 Cl1 34507 Reflections read, of which 624 rejected -16 =< h =< 18, -17 =< k =< 18, -25 =< l =< 23, Max. 2-theta = 54.98 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 0 2 1 260.27 1.04 8 42.30 0 7 5 79.37 1.30 6 7.17 1 9 5 36.40 0.77 6 4.04 2 12 6 99.67 1.06 5 30.33 0 8 7 60.26 0.97 5 11.46 3 14 7 33.83 0.99 5 8.14 0 9 9 112.18 1.03 6 17.81 2 12 9 38.57 0.93 6 5.36 1 11 10 27.30 0.91 6 4.90 2 12 10 80.14 1.07 4 27.27 1 11 11 104.52 1.06 6 24.99 -5 9 15 25.42 0.94 4 6.08 -6 9 16 37.99 0.97 4 10.35 -5 9 16 105.30 1.07 4 55.32 14 Inconsistent equivalents 9187 Unique reflections, of which 0 suppressed R(int) = 0.0525 R(sigma) = 0.0570 Friedel opposites merged Maximum memory for data reduction = 4569 / 90793 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 = 5912 / 635010 wR2 = 0.0947 before cycle 1 for 9187 data and 482 / 482 parameters GooF = S = 1.015; Restrained GooF = 1.015 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0432 * P )^2 + 2.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.11393 0.00012 0.390 OSF Mean shift/esd = 0.018 Maximum = 0.390 for OSF Max. shift = 0.000 A for H35 Max. dU = 0.000 for H35 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5912 / 635010 wR2 = 0.0947 before cycle 2 for 9187 data and 482 / 482 parameters GooF = S = 1.016; Restrained GooF = 1.016 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0432 * P )^2 + 2.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.11393 0.00012 -0.003 OSF Mean shift/esd = 0.006 Maximum = -0.024 for y C43 Max. shift = 0.000 A for H35 Max. dU = 0.000 for H35 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5912 / 635010 wR2 = 0.0947 before cycle 3 for 9187 data and 482 / 482 parameters GooF = S = 1.016; Restrained GooF = 1.016 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0432 * P )^2 + 2.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.11393 0.00012 -0.003 OSF Mean shift/esd = 0.000 Maximum = -0.003 for OSF Max. shift = 0.000 A for H35 Max. dU = 0.000 for H35 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5912 / 635010 wR2 = 0.0947 before cycle 4 for 9187 data and 482 / 482 parameters GooF = S = 1.016; Restrained GooF = 1.016 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0432 * P )^2 + 2.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.11393 0.00012 0.002 OSF Mean shift/esd = 0.000 Maximum = 0.002 for OSF Max. shift = 0.000 A for H35 Max. dU = 0.000 for H35 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 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 0.8086 0.4753 0.0017 43 0.950 0.000 C2 C3 C1 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C3 ** H3 0.8821 0.6260 -0.0276 43 0.950 0.000 C3 C4 C2 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C4 ** H4 1.0104 0.6710 0.0686 43 0.950 0.000 C4 C3 C5 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C5 ** H5 1.0191 0.5498 0.1595 43 0.950 0.000 C5 C4 C1 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C7 ** H7 0.6447 0.6044 0.0722 43 0.950 0.000 C7 C78 C6 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C9 ** H9 0.8635 0.7784 0.1500 43 0.950 0.000 C9 C78 C10 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C10 ** H10 0.8610 0.6483 0.2335 43 0.950 0.000 C10 C9 C6 H12 0.7404 0.2466 0.1553 43 0.950 0.000 C12 C13 C11 H13 0.6419 0.1488 0.0825 43 0.950 0.000 C13 C14 C12 H14 0.6576 0.1416 -0.0309 43 0.950 0.000 C14 C13 C15 H15 0.7729 0.2318 -0.0735 43 0.950 0.000 C15 C16 C14 H16 0.8729 0.3293 -0.0013 43 0.950 0.000 C16 C15 C11 H18 1.0798 0.4223 0.2121 43 0.950 0.000 C18 C19 C17 H19 1.2361 0.3640 0.2178 43 0.950 0.000 C19 C20 C18 H20 1.2632 0.2297 0.1603 43 0.950 0.000 C20 C21 C19 H21 1.1329 0.1530 0.0983 43 0.950 0.000 C21 C20 C22 H22 0.9763 0.2123 0.0902 43 0.950 0.000 C22 C17 C21 H24 0.6718 0.4510 0.0617 43 0.950 0.000 C24 C25 C23 H25 0.5469 0.3799 -0.0097 43 0.950 0.000 C25 C26 C24 H26 0.4137 0.3227 0.0336 43 0.950 0.000 C26 C25 C27 H27 0.4038 0.3374 0.1480 43 0.950 0.000 C27 C26 C28 H28 0.5274 0.4103 0.2205 43 0.950 0.000 C28 C27 C23 H30 0.5489 0.6035 0.2120 43 0.950 0.000 C30 C29 C31 H31 0.4783 0.6744 0.2976 43 0.950 0.000 C31 C32 C30 H32 0.5432 0.6503 0.4110 43 0.950 0.000 C32 C33 C31 H33 0.6805 0.5591 0.4387 43 0.950 0.000 C33 C32 C34 H34 0.7536 0.4907 0.3536 43 0.950 0.000 C34 C33 C29 H37 1.0658 0.5629 0.3194 43 0.950 0.000 C37 C38 C36 H38 1.1737 0.5531 0.4203 43 0.950 0.000 C38 C39 C37 H39 1.1472 0.4476 0.5017 43 0.950 0.000 C39 C38 C40 H40 1.0156 0.3482 0.4836 43 0.950 0.000 C40 C41 C39 H41 0.9099 0.3531 0.3818 43 0.950 0.000 C41 C40 C36 H42A 0.1914 0.5456 0.1563 23 0.990 0.000 C42 Cl4 Cl3 H42B 0.2287 0.6472 0.1748 23 0.990 0.000 C42 Cl4 Cl3 H43A 0.5419 0.9553 0.1738 23 0.990 0.000 C43 Cl5 Cl6 H43B 0.4556 0.8914 0.1387 23 0.990 0.000 C43 Cl5 Cl6 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C78 ** H78 0.7325 0.7500 0.0507 43 0.950 0.000 C78 C9 C7 02SRC310 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.90646 0.47957 0.09520 1.00000 0.02009 0.01936 0.01945 -0.00060 0.00856 0.00320 0.01906 0.00526 0.00020 0.00019 0.00015 0.00000 0.00140 0.00138 0.00152 0.00116 0.00118 0.00111 0.00059 C2 0.85881 0.50765 0.02935 1.00000 0.03123 0.02415 0.01898 -0.00023 0.00681 0.00532 0.02448 0.00587 0.00023 0.00020 0.00015 0.00000 0.00164 0.00152 0.00156 0.00122 0.00130 0.00127 0.00065 H2 0.80862 0.47528 0.00175 1.00000 0.02937 0.00000 0.00000 C3 0.90005 0.59221 0.01295 1.00000 0.04297 0.02711 0.02555 0.00812 0.02038 0.01085 0.03031 0.00665 0.00025 0.00022 0.00017 0.00000 0.00196 0.00162 0.00178 0.00137 0.00155 0.00144 0.00075 H3 0.88206 0.62597 -0.02759 1.00000 0.03637 0.00000 0.00000 C4 0.97168 0.61738 0.06666 1.00000 0.02690 0.02470 0.03716 0.00342 0.01907 0.00193 0.02812 0.00636 0.00023 0.00021 0.00017 0.00000 0.00163 0.00160 0.00200 0.00137 0.00149 0.00126 0.00073 H4 1.01044 0.67104 0.06860 1.00000 0.03375 0.00000 0.00000 C5 0.97662 0.54932 0.11762 1.00000 0.01667 0.02148 0.03059 0.00027 0.00918 0.00199 0.02233 0.00566 0.00020 0.00019 0.00016 0.00000 0.00139 0.00144 0.00173 0.00127 0.00124 0.00113 0.00063 H5 1.01909 0.54977 0.15947 1.00000 0.02680 0.00000 0.00000 C6 0.74368 0.59167 0.16418 1.00000 0.01738 0.01772 0.01985 0.00101 0.00493 0.00402 0.01810 0.00519 0.00020 0.00019 0.00015 0.00000 0.00137 0.00132 0.00152 0.00115 0.00116 0.00110 0.00058 C7 0.69826 0.62990 0.10110 1.00000 0.01738 0.02184 0.02218 0.00371 0.00180 0.00531 0.02059 0.00554 0.00021 0.00019 0.00015 0.00000 0.00139 0.00144 0.00159 0.00119 0.00119 0.00113 0.00061 H7 0.64465 0.60442 0.07217 1.00000 0.02471 0.00000 0.00000 C9 0.82052 0.72760 0.14484 1.00000 0.02681 0.01522 0.02841 0.00028 0.00891 0.00161 0.02299 0.00557 0.00022 0.00019 0.00016 0.00000 0.00157 0.00136 0.00172 0.00121 0.00132 0.00117 0.00064 H9 0.86352 0.77837 0.14997 1.00000 0.02759 0.00000 0.00000 C10 0.81938 0.65465 0.19158 1.00000 0.02147 0.01871 0.01724 -0.00112 0.00426 0.00372 0.01900 0.00531 0.00020 0.00019 0.00015 0.00000 0.00145 0.00135 0.00148 0.00113 0.00118 0.00114 0.00059 H10 0.86104 0.64834 0.23350 1.00000 0.02280 0.00000 0.00000 C11 0.81525 0.29917 0.08412 1.00000 0.01574 0.01967 0.01951 -0.00237 -0.00027 0.00497 0.01861 0.00506 0.00019 0.00019 0.00015 0.00000 0.00135 0.00139 0.00150 0.00114 0.00115 0.00109 0.00059 C12 0.74706 0.24423 0.10879 1.00000 0.02194 0.02189 0.02164 -0.00212 0.00062 0.00093 0.02210 0.00524 0.00021 0.00019 0.00016 0.00000 0.00148 0.00143 0.00158 0.00121 0.00121 0.00118 0.00062 H12 0.74044 0.24662 0.15533 1.00000 0.02652 0.00000 0.00000 C13 0.68868 0.18591 0.06548 1.00000 0.02053 0.02475 0.04426 -0.00530 0.00002 0.00238 0.03035 0.00582 0.00022 0.00021 0.00018 0.00000 0.00157 0.00157 0.00215 0.00146 0.00144 0.00125 0.00075 H13 0.64192 0.14883 0.08251 1.00000 0.03642 0.00000 0.00000 C14 0.69802 0.18145 -0.00163 1.00000 0.03185 0.03073 0.04105 -0.01317 -0.01387 0.00795 0.03654 0.00607 0.00025 0.00023 0.00019 0.00000 0.00186 0.00175 0.00217 0.00157 0.00161 0.00145 0.00086 H14 0.65755 0.14156 -0.03094 1.00000 0.04385 0.00000 0.00000 C15 0.76647 0.23505 -0.02698 1.00000 0.04018 0.03370 0.02192 -0.00921 -0.00597 0.01124 0.03303 0.00594 0.00025 0.00022 0.00017 0.00000 0.00195 0.00178 0.00172 0.00140 0.00146 0.00152 0.00078 H15 0.77286 0.23182 -0.07353 1.00000 0.03963 0.00000 0.00000 C16 0.82544 0.29330 0.01586 1.00000 0.02767 0.02524 0.01943 -0.00274 -0.00048 0.00576 0.02453 0.00548 0.00022 0.00020 0.00015 0.00000 0.00161 0.00152 0.00160 0.00124 0.00128 0.00127 0.00066 H16 0.87293 0.32932 -0.00128 1.00000 0.02943 0.00000 0.00000 C17 1.01241 0.32499 0.14843 1.00000 0.01623 0.01978 0.01601 0.00079 0.00457 0.00092 0.01712 0.00506 0.00019 0.00018 0.00014 0.00000 0.00135 0.00136 0.00143 0.00111 0.00112 0.00108 0.00057 C18 1.09048 0.36828 0.18778 1.00000 0.01931 0.02018 0.02580 -0.00281 0.00197 0.00159 0.02192 0.00535 0.00021 0.00019 0.00016 0.00000 0.00145 0.00142 0.00168 0.00121 0.00125 0.00114 0.00063 H18 1.07985 0.42229 0.21205 1.00000 0.02630 0.00000 0.00000 C19 1.18325 0.33316 0.19173 1.00000 0.01889 0.02212 0.03068 0.00170 -0.00020 -0.00283 0.02430 0.00557 0.00021 0.00020 0.00016 0.00000 0.00148 0.00148 0.00176 0.00130 0.00128 0.00117 0.00065 H19 1.23610 0.36398 0.21780 1.00000 0.02916 0.00000 0.00000 C20 1.19941 0.25338 0.15790 1.00000 0.01795 0.02656 0.02552 0.00446 0.00408 0.00574 0.02326 0.00556 0.00021 0.00020 0.00015 0.00000 0.00144 0.00155 0.00165 0.00128 0.00123 0.00119 0.00064 H20 1.26321 0.22967 0.16026 1.00000 0.02792 0.00000 0.00000 C21 1.12224 0.20855 0.12076 1.00000 0.02703 0.02181 0.02532 -0.00286 0.00527 0.00543 0.02459 0.00566 0.00022 0.00020 0.00016 0.00000 0.00160 0.00146 0.00167 0.00125 0.00131 0.00125 0.00065 H21 1.13291 0.15304 0.09828 1.00000 0.02950 0.00000 0.00000 C22 1.02896 0.24381 0.11588 1.00000 0.02138 0.01987 0.02075 -0.00017 0.00186 0.00154 0.02080 0.00540 0.00021 0.00019 0.00015 0.00000 0.00145 0.00140 0.00155 0.00117 0.00120 0.00114 0.00061 H22 0.97631 0.21226 0.09019 1.00000 0.02496 0.00000 0.00000 C23 0.61199 0.43949 0.14826 1.00000 0.01819 0.01502 0.02303 0.00156 -0.00232 0.00214 0.01931 0.00509 0.00020 0.00018 0.00015 0.00000 0.00140 0.00130 0.00158 0.00114 0.00118 0.00108 0.00060 C24 0.61694 0.42865 0.07955 1.00000 0.02387 0.02189 0.02332 0.00055 -0.00168 0.00437 0.02357 0.00542 0.00022 0.00020 0.00015 0.00000 0.00154 0.00148 0.00165 0.00121 0.00126 0.00120 0.00065 H24 0.67181 0.45096 0.06172 1.00000 0.02828 0.00000 0.00000 C25 0.54315 0.38595 0.03715 1.00000 0.04095 0.02546 0.02533 0.00244 -0.01083 0.00080 0.03221 0.00585 0.00025 0.00021 0.00018 0.00000 0.00200 0.00163 0.00179 0.00133 0.00151 0.00141 0.00078 H25 0.54687 0.37989 -0.00968 1.00000 0.03865 0.00000 0.00000 C26 0.46438 0.35226 0.06280 1.00000 0.03843 0.02601 0.03739 0.00616 -0.01648 -0.01013 0.03623 0.00607 0.00026 0.00023 0.00019 0.00000 0.00196 0.00165 0.00211 0.00147 0.00161 0.00146 0.00085 H26 0.41371 0.32269 0.03364 1.00000 0.04348 0.00000 0.00000 C27 0.45845 0.36112 0.13066 1.00000 0.02562 0.03339 0.03896 0.00997 -0.00499 -0.01206 0.03367 0.00599 0.00024 0.00023 0.00019 0.00000 0.00171 0.00177 0.00212 0.00152 0.00150 0.00139 0.00080 H27 0.40383 0.33737 0.14805 1.00000 0.04041 0.00000 0.00000 C28 0.53178 0.40449 0.17374 1.00000 0.02661 0.02309 0.02631 0.00416 -0.00013 -0.00236 0.02576 0.00564 0.00022 0.00020 0.00017 0.00000 0.00163 0.00148 0.00172 0.00130 0.00133 0.00125 0.00067 H28 0.52737 0.41035 0.22048 1.00000 0.03092 0.00000 0.00000 C29 0.65727 0.53900 0.27417 1.00000 0.01479 0.01479 0.02790 0.00060 0.00936 -0.00316 0.01853 0.00515 0.00019 0.00018 0.00015 0.00000 0.00133 0.00130 0.00163 0.00115 0.00118 0.00104 0.00059 C30 0.57584 0.59432 0.25800 1.00000 0.01868 0.02134 0.02567 0.00222 0.00610 -0.00045 0.02161 0.00548 0.00020 0.00019 0.00016 0.00000 0.00144 0.00141 0.00167 0.00125 0.00124 0.00115 0.00062 H30 0.54890 0.60348 0.21197 1.00000 0.02593 0.00000 0.00000 C31 0.53359 0.63635 0.30889 1.00000 0.01928 0.02140 0.04112 -0.00036 0.01145 0.00239 0.02656 0.00590 0.00022 0.00020 0.00018 0.00000 0.00151 0.00150 0.00203 0.00135 0.00141 0.00118 0.00070 H31 0.47831 0.67438 0.29756 1.00000 0.03187 0.00000 0.00000 C32 0.57251 0.62248 0.37618 1.00000 0.02519 0.02260 0.03217 -0.00652 0.01392 -0.00462 0.02567 0.00566 0.00022 0.00020 0.00017 0.00000 0.00159 0.00150 0.00185 0.00130 0.00138 0.00123 0.00068 H32 0.54322 0.65027 0.41097 1.00000 0.03080 0.00000 0.00000 C33 0.65391 0.56824 0.39264 1.00000 0.02573 0.02447 0.02245 -0.00584 0.00814 -0.00765 0.02375 0.00537 0.00021 0.00020 0.00016 0.00000 0.00158 0.00150 0.00162 0.00124 0.00127 0.00123 0.00065 H33 0.68047 0.55913 0.43874 1.00000 0.02850 0.00000 0.00000 C34 0.69705 0.52700 0.34205 1.00000 0.01748 0.01770 0.02187 -0.00060 0.00419 -0.00263 0.01889 0.00501 0.00020 0.00019 0.00015 0.00000 0.00138 0.00135 0.00155 0.00115 0.00117 0.00108 0.00059 H34 0.75356 0.49066 0.35361 1.00000 0.02267 0.00000 0.00000 C35 0.91607 0.46251 0.27355 1.00000 0.01882 0.01627 0.01675 0.00092 0.00463 0.00396 0.01708 0.00519 0.00020 0.00020 0.00015 0.00000 0.00139 0.00136 0.00145 0.00115 0.00114 0.00110 0.00057 C36 0.97784 0.45742 0.33923 1.00000 0.01744 0.01826 0.01718 -0.00227 0.00250 0.00005 0.01764 0.00495 0.00019 0.00018 0.00014 0.00000 0.00137 0.00134 0.00146 0.00111 0.00112 0.00108 0.00057 C37 1.05616 0.51808 0.35215 1.00000 0.02953 0.02627 0.02364 0.00148 0.00266 -0.00852 0.02662 0.00546 0.00022 0.00021 0.00016 0.00000 0.00166 0.00156 0.00167 0.00129 0.00134 0.00130 0.00068 H37 1.06585 0.56288 0.31941 1.00000 0.03194 0.00000 0.00000 C38 1.11950 0.51310 0.41234 1.00000 0.03416 0.05034 0.03030 0.00158 -0.00874 -0.02303 0.03967 0.00594 0.00026 0.00026 0.00018 0.00000 0.00191 0.00217 0.00196 0.00166 0.00153 0.00167 0.00089 H38 1.17368 0.55310 0.42032 1.00000 0.04760 0.00000 0.00000 C39 1.10384 0.45034 0.46035 1.00000 0.03932 0.04897 0.02570 0.00429 -0.01306 -0.01515 0.03984 0.00609 0.00026 0.00026 0.00018 0.00000 0.00201 0.00214 0.00189 0.00163 0.00156 0.00169 0.00089 H39 1.14725 0.44756 0.50173 1.00000 0.04781 0.00000 0.00000 C40 1.02595 0.39096 0.44964 1.00000 0.04072 0.03225 0.01815 0.00550 -0.00099 -0.00715 0.03094 0.00590 0.00025 0.00022 0.00017 0.00000 0.00195 0.00177 0.00164 0.00135 0.00143 0.00145 0.00075 H40 1.01564 0.34821 0.48362 1.00000 0.03712 0.00000 0.00000 C41 0.96328 0.39407 0.38938 1.00000 0.02650 0.02645 0.01759 0.00015 0.00155 -0.00704 0.02370 0.00540 0.00022 0.00020 0.00015 0.00000 0.00161 0.00155 0.00157 0.00122 0.00126 0.00124 0.00065 H41 0.90993 0.35305 0.38180 1.00000 0.02844 0.00000 0.00000 C42 0.24809 0.58201 0.17687 1.00000 0.02931 0.02855 0.06485 0.00331 0.00636 0.00631 0.04098 0.00714 0.00025 0.00024 0.00021 0.00000 0.00184 0.00176 0.00270 0.00175 0.00176 0.00146 0.00091 H42A 0.19143 0.54556 0.15632 1.00000 0.04918 0.00000 0.00000 H42B 0.22868 0.64724 0.17485 1.00000 0.04918 0.00000 0.00000 C43 0.52662 0.90067 0.14484 1.00000 0.03720 0.03833 0.03897 0.00498 0.00917 0.00728 0.03782 0.00727 0.00027 0.00025 0.00019 0.00000 0.00200 0.00192 0.00216 0.00163 0.00165 0.00156 0.00083 H43A 0.54185 0.95525 0.17381 1.00000 0.04538 0.00000 0.00000 H43B 0.45557 0.89135 0.13873 1.00000 0.04538 0.00000 0.00000 C78 0.74691 0.71187 0.08941 1.00000 0.02691 0.01990 0.02404 0.00610 0.00776 0.00609 0.02321 0.00570 0.00021 0.00020 0.00016 0.00000 0.00157 0.00142 0.00163 0.00122 0.00129 0.00121 0.00064 H78 0.73248 0.75001 0.05073 1.00000 0.02785 0.00000 0.00000 P1 0.89095 0.37536 0.14212 1.00000 0.01481 0.01647 0.01406 -0.00066 0.00220 0.00116 0.01511 0.00128 0.00005 0.00005 0.00004 0.00000 0.00034 0.00033 0.00036 0.00027 0.00028 0.00026 0.00015 P2 0.71343 0.48792 0.20585 1.00000 0.01476 0.01663 0.01477 0.00031 0.00227 0.00000 0.01538 0.00127 0.00005 0.00005 0.00004 0.00000 0.00034 0.00034 0.00036 0.00027 0.00028 0.00027 0.00015 Cl1 0.91355 0.23531 0.26820 1.00000 0.02270 0.01836 0.02431 0.00388 0.00377 0.00412 0.02177 0.00131 0.00005 0.00005 0.00004 0.00000 0.00035 0.00033 0.00038 0.00027 0.00029 0.00026 0.00015 Cl2 0.70238 0.31493 0.29798 1.00000 0.02179 0.02327 0.02275 0.00645 0.00784 0.00088 0.02214 0.00133 0.00005 0.00005 0.00004 0.00000 0.00035 0.00035 0.00038 0.00028 0.00029 0.00027 0.00016 Cl3 0.27960 0.54947 0.26285 1.00000 0.05494 0.03648 0.05839 -0.00584 -0.00277 -0.00012 0.05110 0.00180 0.00008 0.00006 0.00006 0.00000 0.00060 0.00048 0.00066 0.00045 0.00050 0.00042 0.00026 Cl4 0.34131 0.56690 0.12973 1.00000 0.04557 0.13929 0.06157 -0.02256 0.00303 0.04338 0.08266 0.00266 0.00008 0.00012 0.00007 0.00000 0.00064 0.00127 0.00079 0.00080 0.00056 0.00073 0.00046 Cl5 0.58366 0.80540 0.18574 1.00000 0.04887 0.03792 0.04768 0.00681 0.01437 0.01758 0.04409 0.00192 0.00007 0.00006 0.00005 0.00000 0.00054 0.00047 0.00057 0.00041 0.00045 0.00040 0.00023 Cl6 0.56222 0.92127 0.06534 1.00000 0.07463 0.06323 0.04704 0.01528 0.02919 0.01794 0.05957 0.00246 0.00009 0.00008 0.00006 0.00000 0.00075 0.00067 0.00063 0.00052 0.00056 0.00057 0.00030 Fe1 0.84199 0.60399 0.10055 1.00000 0.01917 0.01801 0.01729 0.00290 0.00616 0.00242 0.01781 0.00076 0.00003 0.00003 0.00002 0.00000 0.00021 0.00020 0.00022 0.00016 0.00017 0.00016 0.00010 Ru1 0.82596 0.37496 0.23927 1.00000 0.01462 0.01546 0.01307 0.00099 0.00196 0.00065 0.01440 0.00039 0.00002 0.00001 0.00001 0.00000 0.00012 0.00012 0.00012 0.00008 0.00009 0.00008 0.00007 H35 0.92503 0.51298 0.25223 1.00000 0.01827 0.05552 0.00216 0.00221 0.00158 0.00000 0.00785 Final Structure Factor Calculation for 02SRC310 in P2(1)/c Total number of l.s. parameters = 482 Maximum vector length = 511 Memory required = 5430 / 25039 wR2 = 0.0947 before cycle 5 for 9187 data and 0 / 482 parameters GooF = S = 1.016; Restrained GooF = 1.016 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0432 * P )^2 + 2.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0385 for 7133 Fo > 4sig(Fo) and 0.0595 for all 9187 data wR2 = 0.0947, GooF = S = 1.016, Restrained GooF = 1.016 for all data Occupancy sum of asymmetric unit = 53.00 for non-hydrogen and 38.00 for hydrogen atoms Principal mean square atomic displacements U 0.0252 0.0199 0.0120 C1 0.0342 0.0222 0.0171 C2 0.0554 0.0216 0.0139 C3 0.0459 0.0241 0.0143 C4 0.0319 0.0218 0.0133 C5 0.0227 0.0184 0.0132 C6 0.0265 0.0220 0.0132 C7 0.0319 0.0221 0.0150 C9 0.0241 0.0185 0.0145 C10 0.0261 0.0174 0.0123 C11 0.0262 0.0210 0.0191 C12 0.0477 0.0239 0.0194 C13 0.0673 0.0237 0.0186 C14 0.0571 0.0254 0.0166 C15 0.0348 0.0206 0.0182 C16 0.0203 0.0174 0.0136 C17 0.0278 0.0201 0.0179 C18 0.0333 0.0226 0.0170 C19 0.0317 0.0230 0.0151 C20 0.0306 0.0265 0.0166 C21 0.0233 0.0203 0.0188 C22 0.0275 0.0177 0.0127 C23 0.0309 0.0230 0.0168 C24 0.0536 0.0261 0.0169 C25 0.0678 0.0234 0.0174 C26 0.0570 0.0272 0.0168 C27 0.0337 0.0234 0.0202 C28 0.0295 0.0168 0.0093 C29 0.0270 0.0211 0.0168 C30 0.0422 0.0224 0.0151 C31 0.0407 0.0195 0.0168 C32 0.0356 0.0185 0.0172 C33 0.0223 0.0195 0.0148 C34 0.0222 0.0159 0.0131 C35 0.0201 0.0174 0.0154 C36 0.0373 0.0235 0.0190 C37 0.0710 0.0342 0.0138 C38 0.0683 0.0363 0.0150 C39 0.0481 0.0285 0.0162 C40 0.0340 0.0198 0.0173 C41 0.0654 0.0349 0.0226 C42 0.0479 0.0351 0.0305 C43 0.0337 0.0208 0.0151 C78 0.0173 0.0144 0.0137 P1 0.0167 0.0148 0.0147 P2 0.0270 0.0232 0.0151 Cl1 0.0304 0.0215 0.0145 Cl2 0.0708 0.0477 0.0348 Cl3 0.1645 0.0566 0.0269 Cl4 0.0652 0.0421 0.0249 Cl5 0.0966 0.0501 0.0320 Cl6 0.0235 0.0161 0.0138 Fe1 0.0160 0.0145 0.0127 Ru1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.018 0.037 0.056 0.075 0.097 0.122 0.151 0.189 0.259 1.000 Number in group 920. 972. 906. 892. 911. 910. 933. 911. 906. 926. GooF 0.861 0.976 1.079 1.028 1.082 1.062 1.033 0.993 0.986 1.045 K 1.286 0.908 0.964 0.977 0.972 0.978 0.985 1.003 1.022 1.016 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.64 inf Number in group 935. 922. 913. 920. 910. 911. 922. 920. 918. 916. GooF 0.942 0.888 0.937 0.961 0.943 1.002 1.019 1.017 1.000 1.371 K 0.986 1.018 1.016 1.001 1.019 1.021 1.033 1.029 1.015 0.993 R1 0.147 0.119 0.101 0.078 0.060 0.050 0.043 0.037 0.029 0.030 Recommended weighting scheme: WGHT 0.0427 3.0480 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) 0 4 8 3502.44 4624.03 4.68 0.205 2.05 4 2 0 3369.32 2620.62 4.48 0.155 3.12 4 3 6 1706.20 1282.69 4.36 0.108 2.02 2 3 3 2907.42 2244.55 4.16 0.143 3.28 4 4 3 5707.48 7051.47 4.07 0.254 2.26 -2 10 15 134.45 439.42 4.05 0.063 0.98 3 1 1 5063.92 4073.53 4.04 0.193 4.16 4 4 4 2869.11 2268.70 4.00 0.144 2.14 -7 3 6 270.70 99.61 3.96 0.030 1.70 -1 4 7 1016.10 731.34 3.88 0.082 2.25 -4 4 1 907.39 1223.09 3.87 0.106 2.52 -5 0 2 3747.65 3002.35 3.84 0.166 2.77 -2 16 6 504.66 890.29 3.82 0.090 0.88 1 3 2 6825.62 8292.07 3.82 0.275 4.09 3 0 4 2146.58 2867.15 3.81 0.162 3.14 4 4 6 444.97 255.34 3.80 0.048 1.90 -7 2 6 2588.07 3313.76 3.69 0.174 1.76 5 5 3 711.08 974.56 3.67 0.094 1.86 3 1 3 194.24 11.40 3.66 0.010 3.43 6 2 0 900.99 1190.71 3.64 0.104 2.19 4 4 1 5104.14 4235.19 3.57 0.197 2.45 -8 8 6 799.13 1107.31 3.55 0.101 1.22 -5 6 7 432.15 227.71 3.54 0.046 1.61 -2 6 6 1777.01 2251.86 3.51 0.143 1.93 1 1 9 3226.79 2579.74 3.49 0.153 2.10 -1 3 6 1311.39 1016.07 3.47 0.096 2.74 -3 9 11 -42.18 111.55 3.47 0.032 1.20 9 13 3 490.92 791.76 3.47 0.085 0.89 2 2 4 1317.27 1668.79 3.47 0.123 3.34 5 2 4 408.73 242.61 3.40 0.047 2.17 2 6 2 780.41 580.29 3.38 0.073 2.21 -16 1 8 1769.81 2336.81 3.38 0.146 0.85 3 1 7 2457.74 1967.36 3.35 0.134 2.23 -4 8 17 60.14 231.79 3.31 0.046 0.98 2 12 11 0.00 169.07 3.26 0.039 0.99 1 0 18 -112.66 165.19 3.24 0.039 1.08 2 3 0 167.15 37.50 3.23 0.019 3.98 -3 6 6 2399.70 1956.82 3.21 0.134 1.86 3 3 11 280.16 461.36 3.20 0.065 1.52 6 1 1 2395.76 2880.16 3.19 0.162 2.22 -9 4 9 1049.79 1348.06 3.17 0.111 1.27 -9 13 7 -83.99 97.21 3.17 0.030 0.89 5 2 2 3681.96 4398.65 3.16 0.200 2.42 -6 1 23 1844.87 2519.86 3.16 0.152 0.85 5 1 2 2326.31 2796.50 3.16 0.160 2.52 -11 15 1 -339.78 458.25 3.15 0.065 0.77 -4 3 9 1300.77 1020.85 3.15 0.097 1.85 8 11 5 482.18 723.47 3.11 0.081 0.99 -5 3 2 521.33 361.22 3.11 0.057 2.41 3 5 5 497.11 333.04 3.10 0.055 2.02 Bond lengths and angles C1 - Distance Angles C5 1.4374 (0.0041) C2 1.4425 (0.0041) 106.36 (0.25) P1 1.8188 (0.0029) 124.14 (0.22) 129.41 (0.22) Fe1 2.0384 (0.0027) 68.69 (0.15) 69.39 (0.16) 129.18 (0.15) C1 - C5 C2 P1 C2 - Distance Angles C3 1.4222 (0.0045) C1 1.4425 (0.0041) 108.11 (0.28) Fe1 2.0410 (0.0030) 69.81 (0.18) 69.19 (0.16) H2 0.9500 125.94 125.94 126.62 C2 - C3 C1 Fe1 C3 - Distance Angles C4 1.4016 (0.0049) C2 1.4222 (0.0045) 108.53 (0.28) Fe1 2.0458 (0.0031) 69.53 (0.18) 69.46 (0.17) H3 0.9500 125.74 125.74 126.85 C3 - C4 C2 Fe1 C4 - Distance Angles C3 1.4016 (0.0049) C5 1.4183 (0.0044) 108.58 (0.27) Fe1 2.0358 (0.0030) 70.30 (0.18) 69.05 (0.17) H4 0.9500 125.71 125.71 126.52 C4 - C3 C5 Fe1 C5 - Distance Angles C4 1.4183 (0.0044) C1 1.4374 (0.0041) 108.43 (0.28) Fe1 2.0227 (0.0028) 70.04 (0.17) 69.86 (0.16) H5 0.9500 125.79 125.79 125.89 C5 - C4 C1 Fe1 C6 - Distance Angles C7 1.4367 (0.0040) C10 1.4452 (0.0040) 106.62 (0.24) P2 1.8105 (0.0028) 128.85 (0.22) 124.50 (0.21) Fe1 2.0155 (0.0028) 70.31 (0.16) 69.77 (0.16) 126.43 (0.15) C6 - C7 C10 P2 C7 - Distance Angles C78 1.4137 (0.0041) C6 1.4367 (0.0040) 108.38 (0.26) Fe1 2.0432 (0.0028) 70.10 (0.16) 68.24 (0.15) H7 0.9500 125.81 125.81 127.42 C7 - C78 C6 Fe1 C9 - Distance Angles C78 1.4119 (0.0043) C10 1.4196 (0.0041) 108.40 (0.26) Fe1 2.0535 (0.0029) 69.78 (0.17) 68.93 (0.16) H9 0.9500 125.80 125.80 127.06 C9 - C78 C10 Fe1 C10 - Distance Angles C9 1.4196 (0.0041) C6 1.4452 (0.0040) 107.98 (0.25) Fe1 2.0338 (0.0029) 70.42 (0.17) 68.41 (0.16) H10 0.9500 126.01 126.01 126.71 C10 - C9 C6 Fe1 C11 - Distance Angles C12 1.3912 (0.0041) C16 1.3966 (0.0042) 119.17 (0.27) P1 1.8253 (0.0029) 119.20 (0.22) 121.62 (0.23) C11 - C12 C16 C12 - Distance Angles C13 1.3884 (0.0042) C11 1.3912 (0.0042) 120.09 (0.30) H12 0.9500 119.96 119.96 C12 - C13 C11 C13 - Distance Angles C14 1.3696 (0.0051) C12 1.3884 (0.0042) 120.47 (0.32) H13 0.9500 119.77 119.77 C13 - C14 C12 C14 - Distance Angles C13 1.3696 (0.0051) C15 1.3890 (0.0053) 120.22 (0.30) H14 0.9500 119.89 119.89 C14 - C13 C15 C15 - Distance Angles C16 1.3868 (0.0044) C14 1.3890 (0.0053) 119.82 (0.32) H15 0.9500 120.09 120.09 C15 - C16 C14 C16 - Distance Angles C15 1.3868 (0.0044) C11 1.3966 (0.0042) 120.21 (0.31) H16 0.9500 119.89 119.89 C16 - C15 C11 C17 - Distance Angles C22 1.3892 (0.0040) C18 1.3956 (0.0040) 118.71 (0.25) P1 1.8349 (0.0027) 121.84 (0.21) 119.44 (0.21) C17 - C22 C18 C18 - Distance Angles C19 1.3840 (0.0041) C17 1.3956 (0.0040) 120.54 (0.27) H18 0.9500 119.73 119.73 C18 - C19 C17 C19 - Distance Angles C20 1.3833 (0.0043) C18 1.3840 (0.0041) 120.31 (0.28) H19 0.9500 119.84 119.84 C19 - C20 C18 C20 - Distance Angles C21 1.3782 (0.0043) C19 1.3833 (0.0043) 119.50 (0.27) H20 0.9500 120.25 120.25 C20 - C21 C19 C21 - Distance Angles C20 1.3782 (0.0043) C22 1.3897 (0.0041) 120.61 (0.28) H21 0.9500 119.70 119.70 C21 - C20 C22 C22 - Distance Angles C17 1.3892 (0.0040) C21 1.3897 (0.0041) 120.26 (0.27) H22 0.9500 119.87 119.87 C22 - C17 C21 C23 - Distance Angles C28 1.3953 (0.0042) C24 1.3956 (0.0043) 118.68 (0.27) P2 1.8275 (0.0028) 119.98 (0.23) 121.06 (0.22) C23 - C28 C24 C24 - Distance Angles C25 1.3804 (0.0044) C23 1.3956 (0.0043) 120.87 (0.30) H24 0.9500 119.57 119.57 C24 - C25 C23 C25 - Distance Angles C26 1.3728 (0.0052) C24 1.3804 (0.0044) 119.86 (0.33) H25 0.9500 120.07 120.07 C25 - C26 C24 C26 - Distance Angles C25 1.3728 (0.0052) C27 1.3785 (0.0053) 120.32 (0.31) H26 0.9500 119.84 119.84 C26 - C25 C27 C27 - Distance Angles C26 1.3785 (0.0053) C28 1.3875 (0.0045) 120.41 (0.32) H27 0.9500 119.80 119.80 C27 - C26 C28 C28 - Distance Angles C27 1.3875 (0.0045) C23 1.3953 (0.0042) 119.85 (0.31) H28 0.9500 120.07 120.07 C28 - C27 C23 C29 - Distance Angles C30 1.3924 (0.0040) C34 1.3981 (0.0041) 119.28 (0.27) P2 1.8338 (0.0029) 119.27 (0.23) 121.39 (0.21) C29 - C30 C34 C30 - Distance Angles C29 1.3924 (0.0040) C31 1.3936 (0.0043) 120.44 (0.29) H30 0.9500 119.78 119.78 C30 - C29 C31 C31 - Distance Angles C32 1.3882 (0.0047) C30 1.3936 (0.0043) 119.80 (0.28) H31 0.9500 120.10 120.10 C31 - C32 C30 C32 - Distance Angles C33 1.3835 (0.0044) C31 1.3882 (0.0047) 120.10 (0.29) H32 0.9500 119.95 119.95 C32 - C33 C31 C33 - Distance Angles C32 1.3835 (0.0044) C34 1.3905 (0.0041) 120.35 (0.30) H33 0.9500 119.82 119.82 C33 - C32 C34 C34 - Distance Angles C33 1.3905 (0.0041) C29 1.3981 (0.0041) 120.01 (0.27) H34 0.9500 119.99 119.99 C34 - C33 C29 C35 - Distance Angles C36 1.4603 (0.0039) Ru1 1.8515 (0.0029) 125.01 (0.21) H35 0.8703 (0.0325) 112.02 (2.04) 122.95 (2.03) C35 - C36 Ru1 C36 - Distance Angles C37 1.4007 (0.0040) C41 1.4021 (0.0041) 118.63 (0.27) C35 1.4603 (0.0039) 118.17 (0.26) 123.20 (0.26) C36 - C37 C41 C37 - Distance Angles C38 1.3839 (0.0045) C36 1.4007 (0.0040) 120.37 (0.29) H37 0.9500 119.82 119.82 C37 - C38 C36 C38 - Distance Angles C39 1.3690 (0.0050) C37 1.3839 (0.0045) 119.79 (0.30) H38 0.9500 120.11 120.11 C38 - C39 C37 C39 - Distance Angles C38 1.3690 (0.0050) C40 1.3821 (0.0047) 121.13 (0.31) H39 0.9500 119.44 119.44 C39 - C38 C40 C40 - Distance Angles C41 1.3791 (0.0044) C39 1.3821 (0.0047) 119.67 (0.30) H40 0.9500 120.16 120.16 C40 - C41 C39 C41 - Distance Angles C40 1.3791 (0.0044) C36 1.4021 (0.0041) 120.38 (0.28) H41 0.9500 119.81 119.81 C41 - C40 C36 C42 - Distance Angles Cl4 1.7324 (0.0039) Cl3 1.7745 (0.0042) 113.38 (0.20) H42A 0.9900 108.90 108.90 H42B 0.9900 108.90 108.90 107.73 C42 - Cl4 Cl3 H42A C43 - Distance Angles Cl5 1.7448 (0.0035) Cl6 1.7620 (0.0038) 112.86 (0.20) H43A 0.9900 109.01 109.01 H43B 0.9900 109.01 109.01 107.79 C43 - Cl5 Cl6 H43A C78 - Distance Angles C9 1.4119 (0.0043) C7 1.4137 (0.0041) 108.59 (0.26) Fe1 2.0510 (0.0028) 69.98 (0.16) 69.50 (0.16) H78 0.9500 125.70 125.70 126.40 C78 - C9 C7 Fe1 P1 - Distance Angles C1 1.8188 (0.0029) C11 1.8253 (0.0029) 106.57 (0.13) C17 1.8349 (0.0028) 100.99 (0.13) 103.84 (0.12) Ru1 2.2652 (0.0008) 122.62 (0.09) 105.98 (0.10) 115.18 (0.09) P1 - C1 C11 C17 P2 - Distance Angles C6 1.8105 (0.0028) C23 1.8275 (0.0028) 104.26 (0.13) C29 1.8338 (0.0029) 99.08 (0.13) 104.46 (0.13) Ru1 2.3066 (0.0007) 122.46 (0.09) 109.54 (0.09) 115.10 (0.10) P2 - C6 C23 C29 Cl1 - Distance Angles Ru1 2.4042 (0.0007) Cl1 - Cl2 - Distance Angles Ru1 2.3948 (0.0007) Cl2 - Cl3 - Distance Angles C42 1.7745 (0.0042) Cl3 - Cl4 - Distance Angles C42 1.7324 (0.0039) Cl4 - Cl5 - Distance Angles C43 1.7448 (0.0035) Cl5 - Cl6 - Distance Angles C43 1.7620 (0.0038) Cl6 - Fe1 - Distance Angles C6 2.0155 (0.0028) C5 2.0227 (0.0028) 124.18 (0.12) C10 2.0338 (0.0029) 41.82 (0.11) 104.98 (0.12) C4 2.0358 (0.0030) 160.59 (0.13) 40.91 (0.12) 121.95 (0.13) C1 2.0384 (0.0027) 107.55 (0.11) 41.45 (0.11) 120.07 (0.11) 69.30 (0.12) C2 2.0410 (0.0030) 122.68 (0.12) 69.12 (0.13) 157.73 (0.12) 68.42 (0.13) 41.42 (0.12) C7 2.0432 (0.0028) 41.46 (0.11) 163.76 (0.12) 69.06 (0.12) 155.10 (0.12) 127.38 (0.11) 110.36 (0.12) C3 2.0458 (0.0031) 158.24 (0.13) 68.50 (0.13) 158.83 (0.13) 40.17 (0.14) 69.21 (0.12) 40.73 (0.13) 122.43 (0.13) C78 2.0510 (0.0028) 69.28 (0.11) 153.02 (0.12) 68.42 (0.12) 118.89 (0.12) 164.43 (0.12) 126.51 (0.12) 40.40 (0.12) C9 2.0535 (0.0029) 69.43 (0.11) 117.83 (0.12) 40.64 (0.12) 104.72 (0.12) 154.34 (0.12) 161.31 (0.12) 68.12 (0.12) Fe1 - C6 C5 C10 C4 C1 C2 C7 Ru1 - Distance Angles C35 1.8515 (0.0029) P1 2.2652 (0.0008) 88.76 (0.09) P2 2.3066 (0.0007) 90.44 (0.09) 95.33 (0.03) Cl2 2.3948 (0.0007) 124.80 (0.09) 146.40 (0.03) 83.97 (0.02) Cl1 2.4042 (0.0007) 101.83 (0.09) 87.34 (0.03) 167.51 (0.03) 87.06 (0.02) Ru1 - C35 P1 P2 Cl2 FMAP and GRID set by program FMAP 2 3 25 GRID -1.136 -2 -2 1.136 2 2 R1 = 0.0586 for 9187 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.13 at 0.2389 0.5393 0.1344 [ 0.85 A from H42A ] Deepest hole -1.26 at 0.3554 0.6214 0.1143 [ 0.89 A from CL4 ] Mean = 0.00, Rms deviation from mean = 0.10 e/A^3, Highest memory used = 5285 / 35750 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2389 0.5393 0.1344 1.00000 0.05 1.13 0.85 H42A 1.05 C42 1.50 CL4 1.79 H42B Q2 1 0.5221 0.7925 0.1439 1.00000 0.05 0.94 1.12 CL5 1.58 C43 1.71 H43B 2.46 H43A Q3 1 0.6237 0.9378 0.0818 1.00000 0.05 0.71 0.90 CL6 2.06 C43 2.32 H43A 2.84 H43B Q4 1 0.7579 0.3766 0.3342 1.00000 0.05 0.56 1.33 CL2 1.71 H34 2.22 H41 2.25 RU1 Q5 1 1.1796 0.3774 0.2613 1.00000 0.05 0.55 1.27 H19 1.54 C19 1.71 H18 1.78 C18 Q6 1 0.3469 0.5866 0.1240 1.00000 0.05 0.53 0.32 CL4 1.86 C42 2.25 H42B 2.43 H42A Q7 1 1.1523 0.6490 0.3990 1.00000 0.05 0.47 1.48 H38 2.00 C12 2.06 H22 2.06 C38 Q8 1 0.1773 0.4967 0.2609 1.00000 0.05 0.46 1.62 CL3 1.89 H18 2.25 H42A 2.30 H37 Q9 1 0.5430 0.9431 0.0621 1.00000 0.05 0.45 0.41 CL6 1.81 C43 2.23 H43B 2.24 H43A Q10 1 0.5518 0.8755 0.0561 1.00000 0.05 0.43 0.70 CL6 1.90 C43 2.29 H43B 2.65 H43A Shortest distances between peaks (including symmetry equivalents) 9 10 1.00 3 9 1.14 3 10 1.39 1 6 1.70 5 8 1.74 2 10 2.22 2 9 2.78 1 8 2.86 2 3 2.93 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. 0.77: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.05: Set up l.s. refinement 0.00: Generate idealized H-atoms 5.55: Structure factors and derivatives 22.45: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 1.94: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.44: Analysis of variance 0.17: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.20: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 11:18:56 Total elapsed time: 31.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++