+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 17:44:27 on 04-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL SHELXL INS file, from DIRDIF output for S92 CELL 0.71073 12.6771 16.0582 16.0851 110.325 93.158 96.365 ZERR 2.00 0.0025 0.0032 0.0032 0.030 0.030 0.030 LATT 1 SFAC C H SI P RU UNIT 132 132 4 8 2 V = 3036.23 F(000) = 1188.0 Mu = 0.44 mm-1 Cell Wt = 2280.64 Rho = 1.247 MERG 2 FMAP 2 PLAN 10 OMIT -3 55 OMIT 2 2 2 OMIT 2 5 3 OMIT -4 4 0 EXTI ISOR 0.001 C58 C57 C59 SIZE 0.2 0.075 0.05 TEMP -123 BOND WGHT 0.05650 L.S. 4 FVAR 0.18554 C1 1 0.453534 0.311477 0.454214 11.00000 0.02715 0.01897 = 0.02629 0.00807 -0.00119 0.00201 C2 1 0.402673 0.283874 0.516005 11.00000 0.02908 0.04443 = 0.03825 0.02363 -0.00280 -0.00263 AFIX 43 H2 2 0.328581 0.276776 0.512944 11.00000 -1.20000 AFIX 0 C3 1 0.460503 0.266678 0.582301 11.00000 0.04560 0.06325 = 0.05250 0.04174 -0.00606 -0.00356 AFIX 43 H3 2 0.425211 0.248754 0.623741 11.00000 -1.20000 AFIX 0 C4 1 0.570538 0.276071 0.587080 11.00000 0.04485 0.04958 = 0.04705 0.02927 -0.01433 -0.00108 AFIX 43 H4 2 0.609379 0.264748 0.631811 11.00000 -1.20000 AFIX 0 C5 1 0.622605 0.302292 0.525312 11.00000 0.02753 0.03849 = 0.04940 0.01763 -0.00936 0.00250 AFIX 43 H5 2 0.696654 0.308148 0.528103 11.00000 -1.20000 AFIX 0 C6 1 0.564680 0.320000 0.458862 11.00000 0.02993 0.02994 = 0.03192 0.01186 -0.00062 -0.00002 AFIX 43 H6 2 0.600162 0.337605 0.417320 11.00000 -1.20000 AFIX 0 C7 1 0.474517 0.380391 0.313113 11.00000 0.01830 0.02883 = 0.02620 0.01412 -0.00075 0.00089 C8 1 0.509288 0.471912 0.335758 11.00000 0.02787 0.03114 = 0.03072 0.01236 0.00110 0.00059 AFIX 43 H8 2 0.480594 0.513579 0.381623 11.00000 -1.20000 AFIX 0 C9 1 0.586489 0.500977 0.290117 11.00000 0.03563 0.03049 = 0.04837 0.02138 0.00397 -0.00490 AFIX 43 H9 2 0.608683 0.562013 0.305177 11.00000 -1.20000 AFIX 0 C10 1 0.630365 0.439733 0.222577 11.00000 0.03644 0.04971 = 0.05054 0.02782 0.01584 -0.00498 AFIX 43 H10 2 0.682032 0.459493 0.192221 11.00000 -1.20000 AFIX 0 C11 1 0.597597 0.349214 0.200091 11.00000 0.03253 0.04690 = 0.03705 0.01338 0.01466 0.00509 AFIX 43 H11 2 0.627341 0.307975 0.154623 11.00000 -1.20000 AFIX 0 C12 1 0.520262 0.319406 0.245151 11.00000 0.02469 0.02905 = 0.03330 0.00972 0.00540 0.00171 AFIX 43 H12 2 0.498841 0.258227 0.229825 11.00000 -1.20000 AFIX 0 C13 1 0.318523 0.437102 0.438890 11.00000 0.02823 0.02160 = 0.01945 0.00439 0.00335 0.00161 AFIX 23 H13A 2 0.279421 0.423562 0.483852 11.00000 -1.20000 H13B 2 0.376583 0.484792 0.469005 11.00000 -1.20000 AFIX 0 C14 1 0.244746 0.467788 0.380934 11.00000 0.02777 0.01829 = 0.02648 0.00602 0.00409 0.00276 AFIX 23 H14A 2 0.287275 0.500351 0.350822 11.00000 -1.20000 H14B 2 0.201102 0.508469 0.418512 11.00000 -1.20000 AFIX 0 C15 1 0.155491 0.407609 0.199786 11.00000 0.03438 0.01795 = 0.02129 0.00800 0.00494 0.00537 C16 1 0.252742 0.428258 0.169642 11.00000 0.03374 0.02888 = 0.03076 0.01561 0.00881 0.00660 AFIX 43 H16 2 0.316122 0.424138 0.199019 11.00000 -1.20000 AFIX 0 C17 1 0.255748 0.454764 0.096567 11.00000 0.05406 0.03784 = 0.03752 0.01990 0.01937 0.00531 AFIX 43 H17 2 0.321030 0.469967 0.078138 11.00000 -1.20000 AFIX 0 C18 1 0.161831 0.458719 0.050791 11.00000 0.07165 0.03738 = 0.02662 0.01682 0.00622 0.00747 AFIX 43 H18 2 0.163954 0.476363 0.001549 11.00000 -1.20000 AFIX 0 C19 1 0.065855 0.436597 0.078190 11.00000 0.05447 0.04026 = 0.03130 0.01526 -0.00622 0.00695 AFIX 43 H19 2 0.002888 0.439171 0.047218 11.00000 -1.20000 AFIX 0 C20 1 0.061434 0.410289 0.151895 11.00000 0.03672 0.02527 = 0.02975 0.01055 0.00100 0.00397 AFIX 43 H20 2 -0.004280 0.394466 0.169283 11.00000 -1.20000 AFIX 0 C21 1 0.023889 0.390299 0.332813 11.00000 0.02381 0.02229 = 0.02137 0.00724 0.00534 0.00719 C22 1 -0.007931 0.475301 0.356754 11.00000 0.02816 0.02671 = 0.04188 0.01171 0.01000 0.00406 AFIX 43 H22 2 0.039686 0.523496 0.356233 11.00000 -1.20000 AFIX 0 C23 1 -0.108747 0.488730 0.381100 11.00000 0.03104 0.02393 = 0.05882 0.00841 0.01742 0.01087 AFIX 43 H23 2 -0.128536 0.545865 0.397199 11.00000 -1.20000 AFIX 0 C24 1 -0.181451 0.417277 0.381803 11.00000 0.02649 0.03219 = 0.04277 0.00707 0.01429 0.00754 AFIX 43 H24 2 -0.249869 0.426328 0.397645 11.00000 -1.20000 AFIX 0 C25 1 -0.150904 0.332954 0.358756 11.00000 0.02729 0.02774 = 0.03886 0.00658 0.00999 -0.00110 AFIX 43 H25 2 -0.198692 0.285003 0.359606 11.00000 -1.20000 AFIX 0 C26 1 -0.049128 0.319494 0.334324 11.00000 0.02622 0.02339 = 0.02727 0.00753 0.00704 0.00517 AFIX 43 H26 2 -0.029394 0.262370 0.318735 11.00000 -1.20000 AFIX 0 C27 1 0.008757 0.169730 0.103547 11.00000 0.02671 0.01828 = 0.02003 0.00386 0.00013 0.00144 C28 1 0.056823 0.177612 0.030626 11.00000 0.02852 0.02468 = 0.02261 0.00683 0.00287 0.00157 AFIX 43 H28 2 0.126832 0.166421 0.023644 11.00000 -1.20000 AFIX 0 C29 1 0.000982 0.202081 -0.031840 11.00000 0.04284 0.03225 = 0.02383 0.01211 0.00523 0.00486 AFIX 43 H29 2 0.033645 0.206611 -0.080759 11.00000 -1.20000 AFIX 0 C30 1 -0.102700 0.219789 -0.022084 11.00000 0.04248 0.04100 = 0.02925 0.01592 -0.00189 0.00993 AFIX 43 H30 2 -0.140080 0.235819 -0.064298 11.00000 -1.20000 AFIX 0 C31 1 -0.150205 0.213406 0.051115 11.00000 0.03351 0.04125 = 0.03447 0.01230 0.00054 0.01341 AFIX 43 H31 2 -0.219747 0.225824 0.058422 11.00000 -1.20000 AFIX 0 C32 1 -0.095255 0.188673 0.113801 11.00000 0.02841 0.03134 = 0.02676 0.00892 0.00420 0.00542 AFIX 43 H32 2 -0.128023 0.184727 0.162883 11.00000 -1.20000 AFIX 0 C33 1 -0.023975 0.073388 0.221855 11.00000 0.02314 0.02109 = 0.02798 0.01083 0.00738 0.00437 C34 1 -0.097813 0.006822 0.158956 11.00000 0.02704 0.02687 = 0.02969 0.00926 0.00350 0.00043 AFIX 43 H34 2 -0.095470 -0.002851 0.098670 11.00000 -1.20000 AFIX 0 C35 1 -0.174162 -0.044687 0.185458 11.00000 0.02863 0.03111 = 0.04562 0.01134 0.00531 -0.00477 AFIX 43 H35 2 -0.222685 -0.088763 0.143173 11.00000 -1.20000 AFIX 0 C36 1 -0.177991 -0.030460 0.274428 11.00000 0.03138 0.03835 = 0.05685 0.02545 0.01499 -0.00284 AFIX 43 H36 2 -0.228912 -0.065465 0.292139 11.00000 -1.20000 AFIX 0 C37 1 -0.107315 0.034993 0.337535 11.00000 0.04475 0.04470 = 0.03786 0.02085 0.01422 -0.00147 AFIX 43 H37 2 -0.111406 0.045016 0.397720 11.00000 -1.20000 AFIX 0 C38 1 -0.029557 0.086282 0.311173 11.00000 0.03341 0.02620 = 0.03097 0.01087 0.00528 -0.00210 AFIX 43 H38 2 0.019150 0.129653 0.353966 11.00000 -1.20000 AFIX 0 C39 1 0.146906 0.041691 0.117129 11.00000 0.02274 0.02153 = 0.02038 0.00375 0.00467 0.00086 AFIX 23 H39A 2 0.093372 -0.006130 0.078694 11.00000 -1.20000 H39B 2 0.194695 0.060906 0.080187 11.00000 -1.20000 AFIX 0 C40 1 0.208995 0.009201 0.181130 11.00000 0.02659 0.01947 = 0.03061 0.00907 0.00493 0.00275 AFIX 23 H40A 2 0.254230 -0.032990 0.147996 11.00000 -1.20000 H40B 2 0.159158 -0.022137 0.207563 11.00000 -1.20000 AFIX 0 C41 1 0.299084 0.054149 0.358992 11.00000 0.03127 0.02272 = 0.03353 0.01343 0.00069 0.00175 C42 1 0.240189 0.081899 0.430676 11.00000 0.04976 0.03706 = 0.03809 0.02196 0.01227 0.01323 AFIX 43 H42 2 0.196729 0.125885 0.434743 11.00000 -1.20000 AFIX 0 C43 1 0.244826 0.045106 0.496908 11.00000 0.07846 0.04846 = 0.04135 0.02814 0.01696 0.01441 AFIX 43 H43 2 0.204202 0.064634 0.544629 11.00000 -1.20000 AFIX 0 C44 1 0.308183 -0.019381 0.493057 11.00000 0.07312 0.05952 = 0.05752 0.04532 0.00635 0.01314 AFIX 43 H44 2 0.312164 -0.042647 0.538451 11.00000 -1.20000 AFIX 0 C45 1 0.365428 -0.049139 0.421867 11.00000 0.07219 0.06265 = 0.08256 0.05419 0.01737 0.03344 AFIX 43 H45 2 0.407571 -0.093882 0.418319 11.00000 -1.20000 AFIX 0 C46 1 0.361859 -0.013658 0.354351 11.00000 0.05859 0.04725 = 0.05962 0.03457 0.02350 0.02663 AFIX 43 H46 2 0.401181 -0.034953 0.306053 11.00000 -1.20000 AFIX 0 C47 1 0.426979 0.095827 0.235566 11.00000 0.02376 0.02034 = 0.04555 0.01129 0.00905 0.00777 C48 1 0.516259 0.117383 0.298609 11.00000 0.02718 0.02756 = 0.06019 0.01223 -0.00005 0.00592 AFIX 43 H48 2 0.506832 0.132017 0.358699 11.00000 -1.20000 AFIX 0 C49 1 0.618363 0.116990 0.271852 11.00000 0.02597 0.03554 = 0.09872 0.01962 -0.00128 0.00388 AFIX 43 H49 2 0.677008 0.130739 0.313985 11.00000 -1.20000 AFIX 0 C50 1 0.633261 0.096414 0.183517 11.00000 0.03029 0.04851 = 0.11556 0.02437 0.03189 0.01220 AFIX 43 H50 2 0.701992 0.096414 0.166069 11.00000 -1.20000 AFIX 0 C51 1 0.546778 0.075695 0.120336 11.00000 0.04452 0.04345 = 0.07371 0.01551 0.03341 0.01070 AFIX 43 H51 2 0.557289 0.062546 0.060603 11.00000 -1.20000 AFIX 0 C52 1 0.444324 0.074546 0.146152 11.00000 0.03033 0.03102 = 0.04725 0.00846 0.01603 0.00542 AFIX 43 H52 2 0.386284 0.059363 0.103223 11.00000 -1.20000 AFIX 0 C53 1 0.285544 0.230857 0.168987 11.00000 0.02020 0.01630 = 0.03428 0.00778 -0.00006 0.00176 C54 1 0.322200 0.230382 0.103012 11.00000 0.02208 0.02379 = 0.03365 0.00823 0.00413 0.00276 C55 1 0.370986 0.237050 0.029549 11.00000 0.03565 0.03768 = 0.02833 0.01344 0.01316 0.00638 C56 1 0.415411 0.244953 -0.032931 11.00000 0.04200 0.05277 = 0.03771 0.01969 0.01102 0.00560 C57 1 0.456363 0.172399 -0.224076 11.00000 0.21200 0.08286 = 0.07748 0.03559 0.09517 0.03177 AFIX 137 H57A 2 0.463274 0.117312 -0.214682 11.00000 -1.50000 H57B 2 0.503857 0.179310 -0.266420 11.00000 -1.50000 H57C 2 0.384234 0.171161 -0.246537 11.00000 -1.50000 AFIX 0 C58 1 0.453385 0.368573 -0.133989 11.00000 0.17706 0.08623 = 0.09451 0.06119 0.04493 0.01391 AFIX 137 H58A 2 0.379745 0.357895 -0.157160 11.00000 -1.50000 H58B 2 0.497106 0.382895 -0.175359 11.00000 -1.50000 H58C 2 0.463978 0.417740 -0.078004 11.00000 -1.50000 AFIX 0 C59 1 0.632237 0.287376 -0.079094 11.00000 0.03113 0.67849 = 0.25199 0.37061 0.01679 0.01172 AFIX 137 H59A 2 0.643947 0.330512 -0.019472 11.00000 -1.50000 H59B 2 0.672012 0.309948 -0.117701 11.00000 -1.50000 H59C 2 0.655360 0.232199 -0.079856 11.00000 -1.50000 AFIX 0 C60 1 0.157797 0.258055 0.406168 11.00000 0.01713 0.01949 = 0.04462 0.01895 -0.00562 -0.00300 C61 1 0.121482 0.271865 0.469577 11.00000 0.02757 0.01303 = 0.02927 0.00067 -0.00882 0.00425 C62 1 0.069378 0.274053 0.547701 11.00000 0.03591 0.02757 = 0.02415 0.00863 0.00805 0.00251 C63 1 0.026484 0.275270 0.614065 11.00000 0.04631 0.03692 = 0.03028 0.01160 0.01289 0.00510 C64 1 0.066447 0.344392 0.811448 11.00000 0.07487 0.07184 = 0.03990 0.01788 -0.00463 -0.00690 AFIX 137 H64A 2 0.128426 0.314721 0.809801 11.00000 -1.50000 H64B 2 0.035222 0.350988 0.866026 11.00000 -1.50000 H64C 2 0.086643 0.402489 0.808153 11.00000 -1.50000 AFIX 0 C65 1 -0.156277 0.329287 0.724088 11.00000 0.05405 0.07274 = 0.06388 0.03421 0.02102 0.02062 AFIX 137 H65A 2 -0.140003 0.389757 0.725899 11.00000 -1.50000 H65B 2 -0.186818 0.329605 0.777483 11.00000 -1.50000 H65C 2 -0.206243 0.295635 0.673270 11.00000 -1.50000 AFIX 0 C66 1 -0.063891 0.160706 0.712914 11.00000 0.08018 0.04308 = 0.04689 0.02345 0.01399 -0.00024 AFIX 137 H66A 2 -0.113292 0.126748 0.661802 11.00000 -1.50000 H66B 2 -0.095270 0.161493 0.766107 11.00000 -1.50000 H66C 2 0.000293 0.133580 0.709441 11.00000 -1.50000 AFIX 0 SI1 3 0.490425 0.267360 -0.117591 11.00000 0.04057 0.08971 = 0.04680 0.04645 0.01784 0.00952 SI2 3 -0.031947 0.276759 0.715593 11.00000 0.03969 0.03492 = 0.02383 0.01237 0.00977 0.00280 P1 4 0.372544 0.337032 0.370217 11.00000 0.02058 0.01961 = 0.01999 0.00697 0.00230 0.00170 P2 4 0.156306 0.371857 0.296247 11.00000 0.02074 0.01834 = 0.01961 0.00727 0.00472 0.00330 P3 4 0.082704 0.136877 0.186267 11.00000 0.02033 0.01873 = 0.01886 0.00661 0.00444 0.00197 P4 4 0.292863 0.102620 0.271124 11.00000 0.02081 0.01962 = 0.02479 0.00911 0.00468 0.00388 RU1 5 0.223205 0.237616 0.285141 11.00000 0.01847 0.01745 = 0.01718 0.00669 0.00482 0.00245 HKLF 4 Covalent radii and connectivity table for SHELXL INS file, from DIRDIF output for S92 C 0.770 H 0.320 SI 1.170 P 1.100 RU 1.330 C1 - C2 C6 P1 C2 - C1 C3 C3 - C4 C2 C4 - C5 C3 C5 - C4 C6 C6 - C5 C1 C7 - C12 C8 P1 C8 - C9 C7 C9 - C10 C8 C10 - C11 C9 C11 - C10 C12 C12 - C11 C7 C13 - C14 P1 C14 - C13 P2 C15 - C20 C16 P2 C16 - C17 C15 C17 - C16 C18 C18 - C19 C17 C19 - C18 C20 C20 - C19 C15 C21 - C26 C22 P2 C22 - C23 C21 C23 - C22 C24 C24 - C25 C23 C25 - C24 C26 C26 - C25 C21 C27 - C28 C32 P3 C28 - C29 C27 C29 - C30 C28 C30 - C29 C31 C31 - C30 C32 C32 - C31 C27 C33 - C38 C34 P3 C34 - C35 C33 C35 - C36 C34 C36 - C35 C37 C37 - C36 C38 C38 - C33 C37 C39 - C40 P3 C40 - C39 P4 C41 - C42 C46 P4 C42 - C41 C43 C43 - C44 C42 C44 - C45 C43 C45 - C44 C46 C46 - C45 C41 C47 - C52 C48 P4 C48 - C49 C47 C49 - C50 C48 C50 - C49 C51 C51 - C50 C52 C52 - C51 C47 C53 - C54 Ru1 C54 - C53 C55 C55 - C56 C54 C56 - C55 Si1 C57 - Si1 C58 - Si1 C59 - Si1 C60 - C61 Ru1 C61 - C60 C62 C62 - C63 C61 C63 - C62 Si2 C64 - Si2 C65 - Si2 C66 - Si2 Si1 - C56 C59 C58 C57 Si2 - C63 C66 C64 C65 P1 - C13 C1 C7 Ru1 P2 - C21 C15 C14 Ru1 P3 - C33 C27 C39 Ru1 P4 - C47 C41 C40 Ru1 Ru1 - C53 C60 P1 P2 P3 P4 42694 Reflections read, of which 9 rejected -16 =< h =< 16, -20 =< k =< 20, -20 =< l =< 20, Max. 2-theta = 54.92 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 3 3 2 984.04 10.03 3 403.04 1 2 3 68.15 0.24 3 236.51 1 3 3 53.63 0.48 3 26.67 2 4 3 80.39 0.35 3 85.19 5 4 3 124.77 0.49 3 78.75 1 0 4 98.36 0.46 6 23.34 1 2 4 24.12 0.35 4 5.73 1 3 4 24.14 0.34 4 6.16 7 3 4 57.48 0.37 3 86.71 8 4 4 37.56 0.62 3 50.10 2 5 4 14.94 0.33 3 5.61 4 7 4 17.71 0.52 3 6.97 6 9 4 30.52 0.59 4 12.42 1 3 5 27.25 0.24 4 9.06 9 3 5 43.68 1.07 3 19.87 10 3 5 14.90 0.70 3 8.60 1 4 5 10.70 0.23 3 4.31 2 5 5 83.66 2.51 3 12.64 2 6 5 3.65 0.36 3 1.91 2 0 6 205.45 3.85 6 20.33 1 1 6 9.38 0.28 5 1.83 1 2 6 96.40 0.37 4 66.71 1 3 6 21.47 0.34 4 5.22 1 4 6 9.97 0.39 4 2.51 9 4 6 0.36 0.23 4 1.49 0 -7 7 133.76 4.10 2 23.63 2 0 7 142.02 0.48 6 39.60 1 1 7 86.26 1.55 6 8.94 1 2 7 50.52 0.36 4 18.79 1 3 7 39.87 0.36 4 13.26 1 5 7 26.83 0.46 4 8.37 2 8 7 29.31 0.57 4 10.87 2 9 7 81.26 0.82 4 53.55 2 0 8 56.62 0.45 6 8.96 1 2 8 112.28 0.50 4 91.01 1 4 8 11.46 0.33 4 3.48 1 6 8 40.15 0.69 4 11.99 6 -2 9 4.89 0.43 3 2.95 9 -2 9 20.24 0.91 4 5.41 9 0 9 2.06 0.24 3 1.23 1 2 9 10.42 0.42 4 2.93 1 3 9 14.65 0.42 4 3.39 1 7 9 50.07 0.70 4 18.88 1 8 9 25.45 0.77 4 7.85 1 9 9 23.41 0.67 4 8.42 1 2 10 41.35 0.48 4 12.05 1 3 10 27.56 0.66 4 6.07 7 -3 11 28.18 0.68 4 14.37 3 -1 11 111.45 0.83 5 32.00 2 0 11 135.58 0.73 5 67.86 ** etc. ** 51 Inconsistent equivalents 13576 Unique reflections, of which 0 suppressed R(int) = 0.0959 R(sigma) = 0.0867 Friedel opposites merged Maximum memory for data reduction = 5982 / 135619 Default effective X-H distances for T = -123.0 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 = 7910 / 926422 wR2 = 0.1203 before cycle 1 for 13576 data and 665 / 665 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint -0.0664 0.0010 ISOR U11 C58 0.0244 0.0010 ISOR U22 C58 0.0161 0.0010 ISOR U33 C58 -0.0218 0.0010 ISOR U23 C58 -0.0338 0.0010 ISOR U13 C58 -0.0939 0.0010 ISOR U11 C57 0.0353 0.0010 ISOR U22 C57 0.0406 0.0010 ISOR U33 C57 0.0065 0.0010 ISOR U23 C57 -0.0833 0.0010 ISOR U13 C57 -0.0154 0.0010 ISOR U12 C57 0.2376 0.0010 ISOR U11 C59 -0.4098 0.0010 ISOR U22 C59 0.0167 0.0010 ISOR U33 C59 -0.2749 0.0010 ISOR U23 C59 0.0102 0.0010 ISOR U13 C59 0.0256 0.0010 ISOR U12 C59 Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.135 0.000 GooF = S = 1.022; Restrained GooF = 5.112 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0565 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.18518 0.00117 -0.307 OSF 2 0.00000 0.00181 -0.102 EXTI Mean shift/esd = 0.086 Maximum = -1.579 for U22 C59 Max. shift = 0.036 A for H59C Max. dU =-0.005 for C59 Least-squares cycle 2 Maximum vector length = 511 Memory required = 7910 / 926422 wR2 = 0.1197 before cycle 2 for 13576 data and 665 / 665 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint -0.0560 0.0010 ISOR U11 C58 0.0210 0.0010 ISOR U22 C58 0.0131 0.0010 ISOR U33 C58 -0.0182 0.0010 ISOR U23 C58 -0.0274 0.0010 ISOR U13 C58 -0.0844 0.0010 ISOR U11 C57 0.0300 0.0010 ISOR U22 C57 0.0356 0.0010 ISOR U33 C57 -0.0764 0.0010 ISOR U13 C57 -0.0092 0.0010 ISOR U12 C57 0.2325 0.0010 ISOR U11 C59 -0.3995 0.0010 ISOR U22 C59 0.0122 0.0010 ISOR U33 C59 -0.2695 0.0010 ISOR U23 C59 0.0176 0.0010 ISOR U12 C59 Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.131 0.000 GooF = S = 1.016; Restrained GooF = 4.932 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0565 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.18504 0.00113 -0.119 OSF 2 0.00000 0.00175 -0.150 EXTI Mean shift/esd = 0.049 Maximum = -2.099 for U22 C59 Max. shift = 0.011 A for H57B Max. dU =-0.006 for C59 Least-squares cycle 3 Maximum vector length = 511 Memory required = 7910 / 926422 wR2 = 0.1201 before cycle 3 for 13576 data and 665 / 665 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint -0.0428 0.0010 ISOR U11 C58 0.0168 0.0010 ISOR U22 C58 0.0093 0.0010 ISOR U33 C58 -0.0141 0.0010 ISOR U23 C58 -0.0193 0.0010 ISOR U13 C58 -0.0710 0.0010 ISOR U11 C57 0.0242 0.0010 ISOR U22 C57 0.0302 0.0010 ISOR U33 C57 -0.0676 0.0010 ISOR U13 C57 0.2258 0.0010 ISOR U11 C59 -0.3857 0.0010 ISOR U22 C59 0.0065 0.0010 ISOR U33 C59 -0.2627 0.0010 ISOR U23 C59 0.0075 0.0010 ISOR U12 C59 Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.125 0.000 GooF = S = 1.020; Restrained GooF = 4.760 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0565 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.18498 0.00109 -0.061 OSF 2 0.00000 0.00169 -0.173 EXTI Mean shift/esd = 0.032 Maximum = -2.042 for U11 C57 Max. shift = 0.006 A for H57B Max. dU =-0.006 for C59 Least-squares cycle 4 Maximum vector length = 511 Memory required = 7910 / 926422 wR2 = 0.1209 before cycle 4 for 13576 data and 665 / 665 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint -0.0308 0.0010 ISOR U11 C58 0.0125 0.0010 ISOR U22 C58 0.0063 0.0010 ISOR U33 C58 -0.0106 0.0010 ISOR U23 C58 -0.0120 0.0010 ISOR U13 C58 -0.0583 0.0010 ISOR U11 C57 0.0181 0.0010 ISOR U22 C57 0.0252 0.0010 ISOR U33 C57 -0.0595 0.0010 ISOR U13 C57 0.2188 0.0010 ISOR U11 C59 -0.3726 0.0010 ISOR U22 C59 0.0032 0.0010 ISOR U33 C59 -0.2554 0.0010 ISOR U23 C59 Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.120 0.000 GooF = S = 1.026; Restrained GooF = 4.612 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0565 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.18491 0.00106 -0.060 OSF 2 0.00000 0.00163 -0.197 EXTI 510 0.14802 0.00804 -1.959 U11 C57 514 0.06228 0.00451 -1.730 U13 C57 520 0.12131 0.00844 -1.232 U11 C58 524 0.01526 0.00442 -1.547 U13 C58 531 0.60599 0.00913 -1.940 U22 C59 533 0.33522 0.00516 -1.860 U23 C59 Mean shift/esd = 0.033 Maximum = -1.959 for U11 C57 Max. shift = 0.008 A for H59A Max. dU =-0.005 for C59 Largest correlation matrix elements 0.734 U33 C59 / U22 C59 0.665 U33 C57 / U11 C57 0.598 U23 C45 / U33 C45 0.733 z C59 / y C59 0.657 U33 C57 / U22 C57 0.590 U23 C3 / U33 C3 0.728 U22 C59 / U11 C59 0.642 U23 C59 / U33 C59 0.584 U23 C45 / U22 C45 0.714 U33 C59 / U11 C59 0.632 U23 C59 / U22 C59 0.582 U23 Si1 / U33 Si1 0.708 U22 C58 / U11 C58 0.607 U23 C58 / U33 C58 0.577 U23 C44 / U22 C44 0.707 U33 C58 / U11 C58 0.607 U23 C58 / U22 C58 0.575 U23 C57 / U22 C57 0.697 U33 C58 / U22 C58 0.600 U23 C59 / U11 C59 0.574 U23 C57 / U33 C57 0.679 U22 C57 / U11 C57 0.599 U23 C44 / U33 C44 0.574 U23 C58 / U11 C58 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.3270 0.2767 0.5129 43 0.950 0.000 C2 C1 C3 H3 0.4244 0.2481 0.6243 43 0.950 0.000 C3 C4 C2 H4 0.6104 0.2650 0.6329 43 0.950 0.000 C4 C5 C3 H5 0.6984 0.3086 0.5282 43 0.950 0.000 C5 C4 C6 H6 0.6009 0.3379 0.4162 43 0.950 0.000 C6 C5 C1 H8 0.4798 0.5146 0.3824 43 0.950 0.000 C8 C9 C7 H9 0.6089 0.5633 0.3054 43 0.950 0.001 C9 C10 C8 H10 0.6833 0.4597 0.1916 43 0.950 0.000 C10 C11 C9 H11 0.6280 0.3072 0.1537 43 0.950 0.000 C11 C10 C12 H12 0.4986 0.2569 0.2295 43 0.950 0.000 C12 C11 C7 H13A 0.2783 0.4231 0.4847 23 0.990 0.000 C13 C14 P1 H13B 0.3776 0.4857 0.4698 23 0.990 0.000 C13 C14 P1 H14A 0.2883 0.5011 0.3502 23 0.990 0.000 C14 C13 P2 H14B 0.2003 0.5095 0.4193 23 0.990 0.000 C14 C13 P2 H16 0.3174 0.4245 0.1999 43 0.950 0.000 C16 C17 C15 H17 0.3226 0.4704 0.0778 43 0.950 0.000 C17 C16 C18 H18 0.1636 0.4763 0.0002 43 0.950 0.000 C18 C19 C17 H19 0.0016 0.4397 0.0468 43 0.950 0.000 C19 C18 C20 H20 -0.0058 0.3939 0.1695 43 0.950 0.000 C20 C19 C15 H22 0.0407 0.5245 0.3563 43 0.950 0.001 C22 C23 C21 H23 -0.1290 0.5470 0.3974 43 0.950 0.001 C23 C22 C24 H24 -0.2512 0.4264 0.3981 43 0.950 0.001 C24 C25 C23 H25 -0.1996 0.2842 0.3597 43 0.950 0.000 C25 C24 C26 H26 -0.0291 0.2611 0.3183 43 0.950 0.000 C26 C25 C21 H28 0.1283 0.1666 0.0236 43 0.950 0.000 C28 C29 C27 H29 0.0342 0.2063 -0.0821 43 0.950 0.000 C29 C30 C28 H30 -0.1410 0.2363 -0.0650 43 0.950 0.000 C30 C29 C31 H31 -0.2212 0.2260 0.0585 43 0.950 0.000 C31 C30 C32 H32 -0.1285 0.1848 0.1640 43 0.950 0.000 C32 C31 C27 H34 -0.0957 -0.0031 0.0972 43 0.950 0.000 C34 C35 C33 H35 -0.2234 -0.0896 0.1422 43 0.950 0.001 C35 C36 C34 H36 -0.2299 -0.0663 0.2924 43 0.950 0.000 C36 C35 C37 H37 -0.1115 0.0452 0.3989 43 0.950 0.000 C37 C36 C38 H38 0.0202 0.1304 0.3548 43 0.950 0.000 C38 C33 C37 H39A 0.0923 -0.0071 0.0779 23 0.990 0.000 C39 C40 P3 H39B 0.1958 0.0614 0.0795 23 0.990 0.000 C39 C40 P3 H40A 0.2553 -0.0339 0.1473 23 0.990 0.000 C40 C39 P4 H40B 0.1583 -0.0230 0.2081 23 0.990 0.000 C40 C39 P4 H42 0.1960 0.1268 0.4351 43 0.950 0.000 C42 C41 C43 H43 0.2035 0.0650 0.5455 43 0.950 0.001 C43 C44 C42 H44 0.3128 -0.0427 0.5395 43 0.950 0.000 C44 C45 C43 H45 0.4077 -0.0957 0.4175 43 0.950 0.000 C45 C44 C46 H46 0.4026 -0.0349 0.3055 43 0.950 0.000 C46 C45 C41 H48 0.5070 0.1325 0.3600 43 0.950 0.000 C48 C49 C47 H49 0.6782 0.1306 0.3147 43 0.950 0.001 C49 C50 C48 H50 0.7032 0.0970 0.1658 43 0.950 0.001 C50 C49 C51 H51 0.5576 0.0617 0.0591 43 0.950 0.000 C51 C50 C52 H52 0.3850 0.0591 0.1022 43 0.950 0.000 C52 C51 C47 H57A 0.4654 0.1166 -0.2146 137 0.980 0.002 C57 Si1 H57A H57B 0.5035 0.1807 -0.2675 137 0.980 0.001 C57 Si1 H57A H57C 0.3821 0.1706 -0.2458 137 0.980 0.002 C57 Si1 H57A H58A 0.3793 0.3580 -0.1594 137 0.980 0.000 C58 Si1 H58A H58B 0.5003 0.3856 -0.1738 137 0.980 0.000 C58 Si1 H58A H58C 0.4618 0.4188 -0.0759 137 0.980 0.000 C58 Si1 H58A H59A 0.6437 0.3302 -0.0179 137 0.980 0.000 C59 Si1 H59A H59B 0.6724 0.3117 -0.1178 137 0.980 0.000 C59 Si1 H59A H59C 0.6560 0.2307 -0.0814 137 0.980 0.000 C59 Si1 H59A H64A 0.1306 0.3139 0.8086 137 0.980 0.000 C64 Si2 H64A H64B 0.0359 0.3505 0.8669 137 0.980 0.000 C64 Si2 H64A H64C 0.0873 0.4035 0.8078 137 0.980 0.000 C64 Si2 H64A H65A -0.1396 0.3914 0.7278 137 0.980 0.000 C65 Si2 H65A H65B -0.1889 0.3276 0.7775 137 0.980 0.000 C65 Si2 H65A H65C -0.2065 0.2958 0.6712 137 0.980 0.000 C65 Si2 H65A H66A -0.1163 0.1270 0.6615 137 0.980 0.000 C66 Si2 H66A H66B -0.0940 0.1618 0.7678 137 0.980 0.000 C66 Si2 H66A H66C 0.0010 0.1325 0.7070 137 0.980 0.000 C66 Si2 H66A SHELXL INS file, from DIRDIF output for S92 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.45345 0.31140 0.45425 1.00000 0.02720 0.01889 0.02468 0.00774 -0.00103 0.00184 0.02385 0.02344 0.00092 0.00076 0.00075 0.00000 0.00635 0.00595 0.00606 0.00494 0.00508 0.00498 0.00261 C2 0.40270 0.28388 0.51596 1.00000 0.02849 0.04327 0.03898 0.02404 -0.00184 -0.00188 0.03516 0.02767 0.00103 0.00093 0.00085 0.00000 0.00685 0.00820 0.00745 0.00651 0.00588 0.00602 0.00315 H2 0.32702 0.27671 0.51289 1.00000 0.04219 0.00000 0.00000 C3 0.46048 0.26664 0.58210 1.00000 0.04471 0.06345 0.05197 0.04202 -0.00541 -0.00404 0.04898 0.03173 0.00115 0.00109 0.00100 0.00000 0.00884 0.01069 0.00920 0.00844 0.00733 0.00771 0.00402 H3 0.42442 0.24810 0.62429 1.00000 0.05878 0.00000 0.00000 C4 0.57074 0.27632 0.58706 1.00000 0.04445 0.05035 0.04664 0.02981 -0.01298 -0.00046 0.04506 0.03004 0.00114 0.00101 0.00096 0.00000 0.00864 0.00938 0.00859 0.00756 0.00711 0.00718 0.00378 H4 0.61043 0.26495 0.63288 1.00000 0.05407 0.00000 0.00000 C5 0.62273 0.30248 0.52533 1.00000 0.02696 0.03860 0.04922 0.01699 -0.00901 0.00287 0.03855 0.02774 0.00105 0.00093 0.00093 0.00000 0.00691 0.00808 0.00842 0.00684 0.00634 0.00606 0.00339 H5 0.69838 0.30855 0.52823 1.00000 0.04626 0.00000 0.00000 C6 0.56474 0.32002 0.45875 1.00000 0.02954 0.02915 0.03235 0.01179 -0.00017 -0.00013 0.03059 0.02500 0.00096 0.00084 0.00083 0.00000 0.00676 0.00695 0.00685 0.00570 0.00559 0.00553 0.00292 H6 0.60090 0.33792 0.41623 1.00000 0.03671 0.00000 0.00000 C7 0.47424 0.38035 0.31309 1.00000 0.01807 0.02901 0.02484 0.01385 -0.00104 0.00120 0.02313 0.02385 0.00087 0.00080 0.00074 0.00000 0.00567 0.00661 0.00609 0.00524 0.00484 0.00498 0.00258 C8 0.50913 0.47197 0.33559 1.00000 0.02738 0.03032 0.02939 0.01166 0.00058 0.00024 0.02915 0.02468 0.00093 0.00084 0.00080 0.00000 0.00656 0.00705 0.00661 0.00559 0.00543 0.00552 0.00286 H8 0.47977 0.51458 0.38236 1.00000 0.03498 0.00000 0.00000 C9 0.58626 0.50097 0.29009 1.00000 0.03480 0.02942 0.04696 0.02084 0.00385 -0.00502 0.03589 0.02806 0.00103 0.00092 0.00090 0.00000 0.00739 0.00722 0.00821 0.00636 0.00636 0.00592 0.00318 H9 0.60886 0.56332 0.30541 1.00000 0.04307 0.00000 0.00000 C10 0.63040 0.43955 0.22252 1.00000 0.03396 0.05062 0.05084 0.02753 0.01492 -0.00581 0.04313 0.03046 0.00107 0.00101 0.00096 0.00000 0.00773 0.00946 0.00889 0.00752 0.00679 0.00688 0.00363 H10 0.68331 0.45968 0.19158 1.00000 0.05175 0.00000 0.00000 C11 0.59762 0.34933 0.20019 1.00000 0.03197 0.04606 0.03700 0.01375 0.01463 0.00540 0.03818 0.02888 0.00102 0.00098 0.00088 0.00000 0.00724 0.00865 0.00753 0.00653 0.00606 0.00640 0.00330 H11 0.62801 0.30721 0.15375 1.00000 0.04581 0.00000 0.00000 C12 0.52031 0.31939 0.24513 1.00000 0.02484 0.02926 0.03416 0.01046 0.00641 0.00228 0.02963 0.02562 0.00092 0.00087 0.00079 0.00000 0.00635 0.00695 0.00691 0.00568 0.00548 0.00540 0.00286 H12 0.49860 0.25687 0.22947 1.00000 0.03555 0.00000 0.00000 C13 0.31841 0.43706 0.43892 1.00000 0.02808 0.02128 0.01896 0.00407 0.00351 0.00158 0.02371 0.02327 0.00091 0.00076 0.00071 0.00000 0.00633 0.00609 0.00574 0.00482 0.00499 0.00508 0.00261 H13A 0.27834 0.42313 0.48467 1.00000 0.02845 0.00000 0.00000 H13B 0.37763 0.48571 0.46983 1.00000 0.02845 0.00000 0.00000 C14 0.24482 0.46791 0.38096 1.00000 0.02770 0.01769 0.02669 0.00646 0.00459 0.00267 0.02437 0.02331 0.00092 0.00076 0.00076 0.00000 0.00631 0.00590 0.00616 0.00493 0.00513 0.00494 0.00261 H14A 0.28833 0.50106 0.35021 1.00000 0.02925 0.00000 0.00000 H14B 0.20032 0.50950 0.41928 1.00000 0.02925 0.00000 0.00000 C15 0.15556 0.40767 0.19997 1.00000 0.03424 0.01720 0.02048 0.00777 0.00548 0.00540 0.02343 0.02392 0.00095 0.00075 0.00072 0.00000 0.00676 0.00586 0.00579 0.00478 0.00517 0.00514 0.00259 C16 0.25266 0.42851 0.16978 1.00000 0.03310 0.02891 0.03001 0.01542 0.00883 0.00708 0.02891 0.02676 0.00101 0.00084 0.00079 0.00000 0.00695 0.00683 0.00655 0.00553 0.00555 0.00562 0.00281 H16 0.31741 0.42454 0.19994 1.00000 0.03469 0.00000 0.00000 C17 0.25596 0.45485 0.09662 1.00000 0.05357 0.03748 0.03683 0.01969 0.01887 0.00593 0.04036 0.03033 0.00121 0.00094 0.00087 0.00000 0.00898 0.00808 0.00757 0.00647 0.00687 0.00693 0.00342 H17 0.32265 0.47037 0.07779 1.00000 0.04844 0.00000 0.00000 C18 0.16156 0.45857 0.05072 1.00000 0.07119 0.03613 0.02567 0.01628 0.00579 0.00738 0.04289 0.03028 0.00127 0.00096 0.00087 0.00000 0.01080 0.00802 0.00696 0.00610 0.00718 0.00752 0.00366 H18 0.16359 0.47628 0.00023 1.00000 0.05147 0.00000 0.00000 C19 0.06593 0.43675 0.07825 1.00000 0.05438 0.03761 0.03131 0.01422 -0.00638 0.00653 0.04099 0.02869 0.00121 0.00093 0.00087 0.00000 0.00924 0.00820 0.00723 0.00640 0.00681 0.00709 0.00353 H19 0.00163 0.43966 0.04677 1.00000 0.04919 0.00000 0.00000 C20 0.06134 0.41027 0.15186 1.00000 0.03547 0.02430 0.02914 0.00934 0.00004 0.00362 0.02985 0.02519 0.00103 0.00081 0.00079 0.00000 0.00713 0.00662 0.00656 0.00543 0.00566 0.00559 0.00289 H20 -0.00583 0.39395 0.16946 1.00000 0.03582 0.00000 0.00000 C21 0.02406 0.39038 0.33289 1.00000 0.02365 0.02268 0.02080 0.00805 0.00453 0.00712 0.02189 0.02361 0.00089 0.00077 0.00072 0.00000 0.00601 0.00616 0.00571 0.00486 0.00481 0.00496 0.00251 C22 -0.00789 0.47526 0.35679 1.00000 0.02811 0.02637 0.04024 0.01137 0.00987 0.00360 0.03146 0.02627 0.00097 0.00085 0.00082 0.00000 0.00670 0.00682 0.00747 0.00580 0.00575 0.00547 0.00297 H22 0.04073 0.52453 0.35630 1.00000 0.03776 0.00000 0.00000 C23 -0.10873 0.48869 0.38106 1.00000 0.03108 0.02339 0.05711 0.00747 0.01688 0.01010 0.03802 0.02773 0.00099 0.00087 0.00093 0.00000 0.00721 0.00692 0.00891 0.00634 0.00652 0.00574 0.00337 H23 -0.12902 0.54703 0.39740 1.00000 0.04563 0.00000 0.00000 C24 -0.18131 0.41720 0.38182 1.00000 0.02560 0.03177 0.04243 0.00736 0.01322 0.00735 0.03417 0.02690 0.00101 0.00087 0.00086 0.00000 0.00662 0.00739 0.00769 0.00608 0.00582 0.00568 0.00314 H24 -0.25119 0.42639 0.39806 1.00000 0.04101 0.00000 0.00000 C25 -0.15074 0.33313 0.35880 1.00000 0.02630 0.02616 0.03920 0.00611 0.00977 -0.00093 0.03214 0.02547 0.00096 0.00084 0.00082 0.00000 0.00658 0.00689 0.00733 0.00573 0.00575 0.00545 0.00303 H25 -0.19956 0.28417 0.35970 1.00000 0.03857 0.00000 0.00000 C26 -0.04917 0.31953 0.33432 1.00000 0.02695 0.02225 0.02622 0.00681 0.00753 0.00443 0.02535 0.02421 0.00091 0.00080 0.00074 0.00000 0.00635 0.00629 0.00623 0.00511 0.00514 0.00511 0.00266 H26 -0.02915 0.26112 0.31829 1.00000 0.03042 0.00000 0.00000 C27 0.00881 0.16985 0.10358 1.00000 0.02687 0.01779 0.01897 0.00378 0.00084 0.00185 0.02211 0.02275 0.00090 0.00075 0.00072 0.00000 0.00622 0.00581 0.00564 0.00467 0.00489 0.00489 0.00253 C28 0.05673 0.17779 0.03064 1.00000 0.02756 0.02468 0.02305 0.00694 0.00276 0.00212 0.02563 0.02389 0.00096 0.00079 0.00074 0.00000 0.00635 0.00641 0.00599 0.00508 0.00511 0.00520 0.00267 H28 0.12832 0.16656 0.02361 1.00000 0.03075 0.00000 0.00000 C29 0.00094 0.20197 -0.03197 1.00000 0.04298 0.03232 0.02298 0.01233 0.00569 0.00497 0.03203 0.02627 0.00105 0.00086 0.00080 0.00000 0.00781 0.00729 0.00625 0.00554 0.00572 0.00609 0.00299 H29 0.03419 0.20631 -0.08210 1.00000 0.03843 0.00000 0.00000 C30 -0.10279 0.21984 -0.02202 1.00000 0.04136 0.04025 0.02791 0.01550 -0.00266 0.00906 0.03558 0.02789 0.00108 0.00092 0.00084 0.00000 0.00799 0.00800 0.00676 0.00605 0.00602 0.00647 0.00320 H30 -0.14098 0.23634 -0.06504 1.00000 0.04269 0.00000 0.00000 C31 -0.15015 0.21343 0.05105 1.00000 0.03282 0.04133 0.03459 0.01189 0.00067 0.01353 0.03611 0.02772 0.00106 0.00092 0.00084 0.00000 0.00723 0.00819 0.00726 0.00629 0.00598 0.00627 0.00325 H31 -0.22122 0.22603 0.05851 1.00000 0.04334 0.00000 0.00000 C32 -0.09504 0.18875 0.11384 1.00000 0.02746 0.03184 0.02624 0.00880 0.00390 0.00566 0.02875 0.02488 0.00094 0.00084 0.00079 0.00000 0.00657 0.00707 0.00637 0.00552 0.00529 0.00551 0.00285 H32 -0.12846 0.18476 0.16402 1.00000 0.03450 0.00000 0.00000 C33 -0.02407 0.07335 0.22169 1.00000 0.02202 0.02086 0.02744 0.01042 0.00734 0.00410 0.02267 0.02395 0.00089 0.00077 0.00075 0.00000 0.00593 0.00602 0.00624 0.00507 0.00499 0.00487 0.00254 C34 -0.09792 0.00678 0.15885 1.00000 0.02671 0.02635 0.03006 0.00901 0.00405 0.00147 0.02811 0.02448 0.00091 0.00081 0.00081 0.00000 0.00649 0.00662 0.00665 0.00547 0.00542 0.00535 0.00281 H34 -0.09566 -0.00312 0.09725 1.00000 0.03374 0.00000 0.00000 C35 -0.17391 -0.04457 0.18544 1.00000 0.02719 0.03111 0.04606 0.01117 0.00512 -0.00464 0.03612 0.02786 0.00100 0.00089 0.00092 0.00000 0.00681 0.00739 0.00823 0.00632 0.00615 0.00577 0.00323 H35 -0.22344 -0.08963 0.14224 1.00000 0.04334 0.00000 0.00000 C36 -0.17787 -0.03049 0.27438 1.00000 0.03171 0.03713 0.05524 0.02378 0.01381 -0.00414 0.03974 0.02946 0.00104 0.00093 0.00096 0.00000 0.00737 0.00803 0.00908 0.00706 0.00671 0.00624 0.00341 H36 -0.22986 -0.06633 0.29241 1.00000 0.04769 0.00000 0.00000 C37 -0.10731 0.03494 0.33740 1.00000 0.04405 0.04580 0.03710 0.02098 0.01359 -0.00181 0.04092 0.02986 0.00109 0.00097 0.00092 0.00000 0.00827 0.00878 0.00773 0.00671 0.00657 0.00696 0.00346 H37 -0.11154 0.04522 0.39888 1.00000 0.04911 0.00000 0.00000 C38 -0.02964 0.08614 0.31111 1.00000 0.03359 0.02507 0.02963 0.01036 0.00468 -0.00250 0.02973 0.02624 0.00098 0.00084 0.00081 0.00000 0.00696 0.00660 0.00661 0.00542 0.00558 0.00549 0.00286 H38 0.02016 0.13038 0.35484 1.00000 0.03568 0.00000 0.00000 C39 0.14696 0.04171 0.11714 1.00000 0.02222 0.02208 0.01959 0.00389 0.00475 0.00170 0.02224 0.02322 0.00089 0.00076 0.00072 0.00000 0.00591 0.00607 0.00559 0.00475 0.00473 0.00486 0.00253 H39A 0.09234 -0.00707 0.07786 1.00000 0.02669 0.00000 0.00000 H39B 0.19576 0.06137 0.07949 1.00000 0.02669 0.00000 0.00000 C40 0.20911 0.00905 0.18114 1.00000 0.02604 0.01913 0.02964 0.00869 0.00523 0.00299 0.02485 0.02341 0.00092 0.00076 0.00076 0.00000 0.00621 0.00604 0.00641 0.00509 0.00520 0.00498 0.00263 H40A 0.25534 -0.03394 0.14732 1.00000 0.02982 0.00000 0.00000 H40B 0.15827 -0.02298 0.20809 1.00000 0.02982 0.00000 0.00000 C41 0.29931 0.05414 0.35898 1.00000 0.03067 0.02189 0.03216 0.01186 0.00052 0.00193 0.02789 0.02508 0.00097 0.00081 0.00080 0.00000 0.00672 0.00638 0.00673 0.00539 0.00560 0.00534 0.00280 C42 0.24042 0.08183 0.43087 1.00000 0.04799 0.03549 0.03792 0.02101 0.01086 0.01253 0.03755 0.02959 0.00112 0.00093 0.00086 0.00000 0.00842 0.00784 0.00755 0.00637 0.00656 0.00662 0.00327 H42 0.19604 0.12679 0.43512 1.00000 0.04505 0.00000 0.00000 C43 0.24504 0.04514 0.49679 1.00000 0.07900 0.04630 0.04185 0.02774 0.01810 0.01461 0.05154 0.03457 0.00137 0.00107 0.00098 0.00000 0.01165 0.00945 0.00838 0.00737 0.00806 0.00865 0.00410 H43 0.20350 0.06501 0.54552 1.00000 0.06185 0.00000 0.00000 C44 0.30844 -0.01924 0.49288 1.00000 0.07255 0.05985 0.05798 0.04607 0.00597 0.01263 0.05650 0.03609 0.00136 0.00113 0.00111 0.00000 0.01145 0.01119 0.01004 0.00893 0.00900 0.00930 0.00443 H44 0.31283 -0.04271 0.53946 1.00000 0.06780 0.00000 0.00000 C45 0.36535 -0.04949 0.42152 1.00000 0.06988 0.05949 0.08169 0.05270 0.01697 0.03144 0.06081 0.03991 0.00139 0.00118 0.00119 0.00000 0.01150 0.01123 0.01236 0.01003 0.00991 0.00928 0.00472 H45 0.40774 -0.09570 0.41749 1.00000 0.07297 0.00000 0.00000 C46 0.36201 -0.01347 0.35463 1.00000 0.05691 0.04633 0.05703 0.03314 0.02177 0.02525 0.04739 0.03381 0.00122 0.00100 0.00101 0.00000 0.00950 0.00933 0.00947 0.00787 0.00773 0.00774 0.00385 H46 0.40259 -0.03486 0.30550 1.00000 0.05687 0.00000 0.00000 C47 0.42673 0.09566 0.23552 1.00000 0.02294 0.02008 0.04492 0.01082 0.00856 0.00786 0.02892 0.02608 0.00093 0.00080 0.00086 0.00000 0.00627 0.00623 0.00765 0.00560 0.00569 0.00508 0.00287 C48 0.51642 0.11738 0.29857 1.00000 0.02792 0.02656 0.05876 0.01217 -0.00054 0.00611 0.03856 0.02753 0.00099 0.00086 0.00100 0.00000 0.00702 0.00714 0.00917 0.00659 0.00649 0.00572 0.00341 H48 0.50695 0.13250 0.35999 1.00000 0.04628 0.00000 0.00000 C49 0.61825 0.11686 0.27172 1.00000 0.02589 0.03433 0.09516 0.01833 -0.00051 0.00461 0.05329 0.03380 0.00112 0.00099 0.00130 0.00000 0.00760 0.00842 0.01368 0.00877 0.00830 0.00634 0.00447 H49 0.67822 0.13064 0.31465 1.00000 0.06394 0.00000 0.00000 C50 0.63298 0.09657 0.18351 1.00000 0.02853 0.04765 0.11463 0.02363 0.03142 0.01208 0.06350 0.03970 0.00123 0.00110 0.00142 0.00000 0.00839 0.01019 0.01620 0.01039 0.00979 0.00731 0.00526 H50 0.70323 0.09702 0.16578 1.00000 0.07620 0.00000 0.00000 C51 0.54676 0.07548 0.12017 1.00000 0.04411 0.04337 0.07356 0.01624 0.03378 0.01122 0.05338 0.03521 0.00119 0.00103 0.00116 0.00000 0.00929 0.00922 0.01117 0.00821 0.00854 0.00743 0.00432 H51 0.55758 0.06175 0.05913 1.00000 0.06406 0.00000 0.00000 C52 0.44423 0.07445 0.14605 1.00000 0.02971 0.03014 0.04721 0.00873 0.01678 0.00490 0.03646 0.02857 0.00103 0.00087 0.00092 0.00000 0.00698 0.00733 0.00820 0.00629 0.00624 0.00579 0.00325 H52 0.38497 0.05906 0.10220 1.00000 0.04375 0.00000 0.00000 C53 0.28551 0.23078 0.16899 1.00000 0.02000 0.01548 0.03385 0.00725 -0.00071 0.00226 0.02367 0.02344 0.00089 0.00075 0.00082 0.00000 0.00590 0.00583 0.00683 0.00515 0.00528 0.00474 0.00263 C54 0.32219 0.23062 0.10313 1.00000 0.02143 0.02329 0.03281 0.00787 0.00409 0.00302 0.02636 0.02477 0.00091 0.00080 0.00082 0.00000 0.00613 0.00649 0.00692 0.00543 0.00548 0.00507 0.00274 C55 0.37095 0.23689 0.02943 1.00000 0.03557 0.03788 0.02893 0.01379 0.01190 0.00626 0.03318 0.02764 0.00103 0.00091 0.00082 0.00000 0.00735 0.00777 0.00676 0.00590 0.00588 0.00608 0.00305 C56 0.41565 0.24499 -0.03294 1.00000 0.04110 0.05241 0.03738 0.01936 0.01019 0.00532 0.04258 0.03112 0.00113 0.00104 0.00093 0.00000 0.00817 0.00949 0.00778 0.00700 0.00659 0.00707 0.00354 C57 0.45641 0.17275 -0.22376 1.00000 0.14802 0.08954 0.08127 0.03914 0.06228 0.01567 0.10199 0.04897 0.00202 0.00147 0.00130 0.00000 0.00804 0.00776 0.00729 0.00464 0.00451 0.00437 0.00669 H57A 0.46537 0.11662 -0.21459 1.00000 0.15298 0.00000 0.00000 H57B 0.50353 0.18069 -0.26753 1.00000 0.15298 0.00000 0.00000 H57C 0.38213 0.17055 -0.24576 1.00000 0.15298 0.00000 0.00000 C58 0.45365 0.36943 -0.13353 1.00000 0.12131 0.09339 0.09589 0.04282 0.01526 0.01276 0.10109 0.04971 0.00194 0.00152 0.00149 0.00000 0.00844 0.00813 0.00806 0.00486 0.00442 0.00444 0.00724 H58A 0.37930 0.35799 -0.15939 1.00000 0.15164 0.00000 0.00000 H58B 0.50027 0.38558 -0.17377 1.00000 0.15164 0.00000 0.00000 H58C 0.46183 0.41882 -0.07586 1.00000 0.15164 0.00000 0.00000 C59 0.63198 0.28726 -0.07924 1.00000 0.03457 0.60599 0.24329 0.33522 0.02586 0.03367 0.24584 0.09088 0.00156 0.00345 0.00228 0.00000 0.00793 0.00913 0.00853 0.00516 0.00428 0.00452 0.00759 H59A 0.64371 0.33021 -0.01787 1.00000 0.36876 0.00000 0.00000 H59B 0.67240 0.31166 -0.11781 1.00000 0.36876 0.00000 0.00000 H59C 0.65599 0.23067 -0.08138 1.00000 0.36876 0.00000 0.00000 C60 0.15777 0.25814 0.40633 1.00000 0.01630 0.01796 0.04374 0.01801 -0.00609 -0.00229 0.02486 0.02445 0.00089 0.00077 0.00089 0.00000 0.00588 0.00614 0.00793 0.00578 0.00572 0.00485 0.00273 C61 0.12158 0.27176 0.46940 1.00000 0.02561 0.01173 0.02683 -0.00033 -0.00860 0.00411 0.02364 0.02274 0.00095 0.00073 0.00081 0.00000 0.00640 0.00565 0.00652 0.00496 0.00560 0.00482 0.00269 C62 0.06951 0.27405 0.54764 1.00000 0.03515 0.02750 0.02517 0.00899 0.00742 0.00299 0.02932 0.02610 0.00101 0.00084 0.00080 0.00000 0.00711 0.00681 0.00635 0.00535 0.00558 0.00561 0.00284 C63 0.02681 0.27528 0.61416 1.00000 0.04717 0.03603 0.03036 0.01125 0.01388 0.00735 0.03748 0.02886 0.00112 0.00093 0.00085 0.00000 0.00829 0.00790 0.00708 0.00605 0.00636 0.00659 0.00327 C64 0.06716 0.34409 0.81098 1.00000 0.08071 0.07173 0.03897 0.01766 -0.00523 -0.00650 0.06618 0.03273 0.00141 0.00122 0.00099 0.00000 0.01244 0.01265 0.00899 0.00875 0.00872 0.01019 0.00512 H64A 0.13060 0.31389 0.80865 1.00000 0.09926 0.00000 0.00000 H64B 0.03593 0.35048 0.86690 1.00000 0.09926 0.00000 0.00000 H64C 0.08733 0.40355 0.80784 1.00000 0.09926 0.00000 0.00000 C65 -0.15645 0.32907 0.72401 1.00000 0.05287 0.07265 0.06350 0.03361 0.01905 0.01981 0.05909 0.03778 0.00123 0.00124 0.00111 0.00000 0.00994 0.01233 0.01070 0.00943 0.00842 0.00900 0.00454 H65A -0.13962 0.39140 0.72775 1.00000 0.08863 0.00000 0.00000 H65B -0.18885 0.32764 0.77751 1.00000 0.08863 0.00000 0.00000 H65C -0.20653 0.29577 0.67119 1.00000 0.08863 0.00000 0.00000 C66 -0.06408 0.16097 0.71265 1.00000 0.07999 0.04269 0.04682 0.02212 0.01382 -0.00094 0.05531 0.03359 0.00137 0.00102 0.00103 0.00000 0.01186 0.00932 0.00897 0.00745 0.00845 0.00848 0.00432 H66A -0.11634 0.12703 0.66155 1.00000 0.08297 0.00000 0.00000 H66B -0.09400 0.16182 0.76779 1.00000 0.08297 0.00000 0.00000 H66C 0.00095 0.13248 0.70705 1.00000 0.08297 0.00000 0.00000 Si1 0.49054 0.26729 -0.11761 1.00000 0.04030 0.08964 0.04640 0.04607 0.01772 0.00989 0.05234 0.01088 0.00034 0.00037 0.00029 0.00000 0.00239 0.00373 0.00247 0.00253 0.00195 0.00237 0.00126 Si2 -0.03189 0.27669 0.71560 1.00000 0.04042 0.03495 0.02397 0.01273 0.01020 0.00331 0.03239 0.00769 0.00030 0.00025 0.00022 0.00000 0.00212 0.00209 0.00180 0.00156 0.00158 0.00169 0.00089 P1 0.37259 0.33703 0.37021 1.00000 0.02034 0.01939 0.01999 0.00698 0.00243 0.00177 0.01998 0.00602 0.00023 0.00020 0.00019 0.00000 0.00152 0.00154 0.00150 0.00122 0.00121 0.00122 0.00069 P2 0.15628 0.37184 0.29627 1.00000 0.02037 0.01833 0.01958 0.00737 0.00466 0.00315 0.01912 0.00602 0.00023 0.00020 0.00019 0.00000 0.00151 0.00151 0.00145 0.00120 0.00120 0.00120 0.00068 P3 0.08270 0.13686 0.18628 1.00000 0.02019 0.01832 0.01893 0.00661 0.00457 0.00196 0.01911 0.00599 0.00023 0.00020 0.00019 0.00000 0.00150 0.00151 0.00145 0.00119 0.00119 0.00121 0.00068 P4 0.29285 0.10267 0.27116 1.00000 0.02069 0.01932 0.02456 0.00907 0.00477 0.00390 0.02100 0.00621 0.00023 0.00020 0.00020 0.00000 0.00153 0.00156 0.00156 0.00126 0.00125 0.00123 0.00070 Ru1 0.22320 0.23761 0.28515 1.00000 0.01841 0.01725 0.01700 0.00663 0.00486 0.00247 0.01729 0.00176 0.00007 0.00006 0.00005 0.00000 0.00055 0.00054 0.00053 0.00038 0.00037 0.00037 0.00036 Final Structure Factor Calculation for SHELXL INS file, from DIRDIF output for S92 Total number of l.s. parameters = 665 Maximum vector length = 511 Memory required = 7245 / 24017 wR2 = 0.1216 before cycle 5 for 13576 data and 0 / 665 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint -0.0202 0.0010 ISOR U11 C58 0.0077 0.0010 ISOR U22 C58 0.0052 0.0010 ISOR U33 C58 -0.0068 0.0010 ISOR U23 C58 -0.0051 0.0010 ISOR U13 C58 -0.0460 0.0010 ISOR U11 C57 0.0125 0.0010 ISOR U22 C57 0.0207 0.0010 ISOR U33 C57 -0.0520 0.0010 ISOR U13 C57 0.2113 0.0010 ISOR U11 C59 -0.3601 0.0010 ISOR U22 C59 -0.2477 0.0010 ISOR U23 C59 Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.116 0.000 GooF = S = 1.033; Restrained GooF = 4.474 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0565 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0460 for 9761 Fo > 4sig(Fo) and 0.0753 for all 13576 data wR2 = 0.1216, GooF = S = 1.033, Restrained GooF = 4.474 for all data Occupancy sum of asymmetric unit = 73.00 for non-hydrogen and 66.00 for hydrogen atoms Principal mean square atomic displacements U 0.0302 0.0227 0.0187 C1 0.0525 0.0268 0.0262 C2 0.0827 0.0408 0.0235 C3 0.0710 0.0418 0.0224 C4 0.0565 0.0376 0.0215 C5 0.0360 0.0301 0.0256 C6 0.0319 0.0208 0.0167 C7 0.0340 0.0282 0.0253 C8 0.0489 0.0409 0.0179 C9 0.0589 0.0544 0.0160 C10 0.0493 0.0437 0.0216 C11 0.0364 0.0297 0.0228 C12 0.0299 0.0237 0.0175 C13 0.0301 0.0253 0.0177 C14 0.0345 0.0196 0.0161 C15 0.0377 0.0277 0.0213 C16 0.0609 0.0390 0.0212 C17 0.0714 0.0368 0.0205 C18 0.0598 0.0377 0.0254 C19 0.0372 0.0282 0.0242 C20 0.0267 0.0207 0.0183 C21 0.0437 0.0266 0.0241 C22 0.0660 0.0310 0.0171 C23 0.0510 0.0328 0.0187 C24 0.0486 0.0268 0.0210 C25 0.0320 0.0239 0.0201 C26 0.0274 0.0227 0.0162 C27 0.0290 0.0254 0.0225 C28 0.0432 0.0323 0.0205 C29 0.0459 0.0392 0.0216 C30 0.0484 0.0349 0.0251 C31 0.0333 0.0279 0.0251 C32 0.0299 0.0200 0.0182 C33 0.0322 0.0279 0.0243 C34 0.0495 0.0383 0.0205 C35 0.0577 0.0452 0.0163 C36 0.0558 0.0461 0.0209 C37 0.0390 0.0294 0.0208 C38 0.0286 0.0210 0.0171 C39 0.0312 0.0246 0.0187 C40 0.0346 0.0290 0.0201 C41 0.0524 0.0360 0.0242 C42 0.0817 0.0484 0.0246 C43 0.0774 0.0726 0.0194 C44 0.0993 0.0640 0.0191 C45 0.0776 0.0391 0.0254 C46 0.0467 0.0244 0.0156 C47 0.0627 0.0293 0.0237 C48 0.1007 0.0337 0.0255 C49 0.1245 0.0472 0.0187 C50 0.0923 0.0441 0.0238 C51 0.0578 0.0304 0.0213 C52 0.0362 0.0195 0.0153 C53 0.0347 0.0233 0.0211 C54 0.0407 0.0375 0.0213 C55 0.0528 0.0450 0.0299 C56 0.1744 0.0897 0.0419 C57 0.1223 0.1011 0.0799 C58 0.6417 0.0641 0.0318 C59 may be split into 0.6375 0.3125 -0.0734 and 0.6265 0.2620 -0.0851 0.0481 0.0147 0.0118 C60 0.0430 0.0173 0.0107 C61 0.0377 0.0274 0.0229 C62 0.0514 0.0365 0.0246 C63 0.0967 0.0648 0.0370 C64 0.0807 0.0542 0.0424 C65 0.0854 0.0495 0.0310 C66 0.0932 0.0459 0.0180 Si1 0.0437 0.0348 0.0187 Si2 0.0214 0.0199 0.0187 P1 0.0224 0.0182 0.0168 P2 0.0227 0.0184 0.0162 P3 0.0256 0.0192 0.0182 P4 0.0208 0.0173 0.0139 Ru1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.025 0.038 0.052 0.068 0.085 0.109 0.140 0.189 1.000 Number in group 1377. 1398. 1365. 1356. 1349. 1304. 1370. 1357. 1340. 1360. GooF 0.841 0.928 1.021 1.139 1.153 1.127 1.145 1.022 0.961 0.949 K 1.517 0.946 0.975 0.974 0.989 0.992 0.992 1.001 1.025 1.019 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.05 1.16 1.32 1.66 inf Number in group 1361. 1407. 1326. 1354. 1352. 1374. 1346. 1347. 1343. 1366. GooF 0.892 0.856 0.876 0.910 0.948 0.968 0.976 0.963 1.150 1.583 K 0.986 1.017 0.987 1.009 1.019 1.033 1.042 1.039 1.025 0.992 R1 0.180 0.150 0.125 0.100 0.081 0.060 0.051 0.045 0.040 0.039 Recommended weighting scheme: WGHT 0.0519 0.3370 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) -5 4 1 342.63 617.56 7.62 0.090 2.17 4 0 0 141.53 246.83 7.01 0.057 3.13 -3 -2 1 923.34 574.41 6.70 0.087 3.56 5 0 5 237.13 374.55 6.24 0.070 1.84 3 -1 4 537.31 835.44 6.18 0.105 2.79 -2 1 0 418.28 615.26 5.82 0.090 6.09 4 2 0 366.97 558.50 5.79 0.086 2.76 -4 3 2 623.67 982.27 5.70 0.114 2.56 -3 1 1 318.72 473.51 5.68 0.079 4.02 -4 -3 2 233.78 410.36 5.53 0.073 2.58 1 4 2 131.15 79.08 5.51 0.032 2.78 -3 7 0 529.71 854.87 5.30 0.106 2.01 -3 -6 2 68.78 133.97 5.22 0.042 2.14 -4 -4 3 311.74 189.74 5.16 0.050 2.32 2 0 1 193.27 136.69 5.14 0.042 5.59 2 0 2 2616.52 3618.14 5.07 0.218 4.59 -1 -5 7 175.71 283.67 5.03 0.061 2.11 6 -2 1 101.89 185.91 4.99 0.049 2.07 3 5 3 51.64 133.68 4.98 0.042 1.86 -2 7 1 631.75 893.28 4.89 0.108 2.00 -5 3 1 1462.93 1086.20 4.85 0.120 2.32 1 -2 4 199.29 121.66 4.77 0.040 3.75 4 -5 5 92.10 21.24 4.74 0.017 2.05 -5 -3 5 168.60 264.53 4.66 0.059 1.97 0 -5 3 528.86 745.74 4.63 0.099 3.09 -5 9 2 79.68 32.37 4.55 0.021 1.39 8 8 4 187.38 292.21 4.51 0.062 1.00 -1 1 9 87.14 145.64 4.32 0.044 1.61 7 -2 1 93.95 172.24 4.29 0.048 1.78 -2 4 3 152.35 227.45 4.28 0.055 2.52 -1 4 0 507.73 673.60 4.26 0.094 3.72 5 -1 3 334.00 444.34 4.17 0.076 2.22 3 5 2 44.91 86.26 4.11 0.034 2.01 6 0 1 1000.81 1323.84 4.06 0.132 2.04 7 -8 10 383.62 239.30 4.04 0.056 1.13 3 -4 6 1491.56 1083.02 4.01 0.119 2.16 4 -3 6 138.45 89.94 3.98 0.034 1.99 2 1 4 958.35 1326.52 3.96 0.132 2.83 -4 -4 5 1781.91 1225.76 3.95 0.127 2.12 4 -1 8 92.65 142.05 3.92 0.043 1.59 -3 2 7 958.59 742.41 3.91 0.099 1.81 8 1 1 385.93 270.05 3.87 0.060 1.51 6 3 4 146.48 93.84 3.86 0.035 1.52 0 2 3 551.34 706.76 3.86 0.096 3.60 5 0 7 42.19 85.55 3.83 0.034 1.55 -3 8 0 402.88 292.74 3.81 0.062 1.80 6 -2 2 275.16 197.58 3.78 0.051 2.01 5 1 4 1214.91 1551.11 3.78 0.143 1.90 4 -10 2 399.98 261.70 3.77 0.059 1.48 3 5 1 241.06 338.31 3.75 0.067 2.15 Bond lengths and angles C1 - Distance Angles C2 1.3808 (0.0173) C6 1.3976 (0.0163) 118.78 (1.12) P1 1.8371 (0.0117) 118.91 (0.90) 122.30 (0.95) C1 - C2 C6 C2 - Distance Angles C1 1.3808 (0.0174) C3 1.3815 (0.0178) 120.90 (1.24) C2 - C1 C3 - Distance Angles C4 1.3840 (0.0194) C2 1.3815 (0.0178) 120.18 (1.39) C3 - C4 C4 - Distance Angles C5 1.3774 (0.0198) C3 1.3840 (0.0194) 119.76 (1.27) C4 - C5 C5 - Distance Angles C4 1.3774 (0.0198) C6 1.3912 (0.0175) 120.17 (1.24) C5 - C4 C6 - Distance Angles C5 1.3912 (0.0175) C1 1.3976 (0.0163) 120.19 (1.25) C6 - C5 C7 - Distance Angles C12 1.3957 (0.0163) C8 1.3997 (0.0166) 118.36 (1.12) P1 1.8342 (0.0121) 118.71 (0.93) 122.92 (0.92) C7 - C12 C8 C8 - Distance Angles C9 1.3869 (0.0173) C7 1.3997 (0.0166) 120.47 (1.19) C8 - C9 C9 - Distance Angles C10 1.3827 (0.0193) C8 1.3869 (0.0173) 120.30 (1.27) C9 - C10 C10 - Distance Angles C11 1.3745 (0.0197) C9 1.3827 (0.0193) 119.90 (1.27) C10 - C11 C11 - Distance Angles C10 1.3745 (0.0197) C12 1.3889 (0.0176) 120.38 (1.27) C11 - C10 C12 - Distance Angles C11 1.3889 (0.0176) C7 1.3957 (0.0163) 120.58 (1.23) C12 - C11 C13 - Distance Angles C14 1.5206 (0.0156) P1 1.8353 (0.0112) 110.15 (0.75) C13 - C14 C14 - Distance Angles C13 1.5206 (0.0156) P2 1.8664 (0.0112) 111.98 (0.79) C14 - C13 C15 - Distance Angles C20 1.3996 (0.0163) C16 1.3967 (0.0168) 118.22 (1.11) P2 1.8301 (0.0118) 122.73 (0.95) 118.95 (0.90) C15 - C20 C16 C16 - Distance Angles C17 1.3829 (0.0178) C15 1.3967 (0.0167) 120.98 (1.23) C16 - C17 C17 - Distance Angles C16 1.3829 (0.0178) C18 1.3892 (0.0197) 119.87 (1.35) C17 - C16 C18 - Distance Angles C19 1.3642 (0.0201) C17 1.3892 (0.0197) 119.92 (1.29) C18 - C19 C19 - Distance Angles C18 1.3642 (0.0201) C20 1.3921 (0.0182) 120.87 (1.31) C19 - C18 C20 - Distance Angles C19 1.3921 (0.0182) C15 1.3996 (0.0163) 120.08 (1.27) C20 - C19 C21 - Distance Angles C26 1.3940 (0.0162) C22 1.3947 (0.0167) 118.10 (1.06) P2 1.8284 (0.0114) 121.00 (0.86) 120.86 (0.92) C21 - C26 C22 C22 - Distance Angles C23 1.3750 (0.0166) C21 1.3947 (0.0167) 120.97 (1.19) C22 - C23 C23 - Distance Angles C22 1.3750 (0.0166) C24 1.3934 (0.0181) 120.35 (1.20) C23 - C22 C24 - Distance Angles C25 1.3764 (0.0178) C23 1.3934 (0.0181) 119.33 (1.16) C24 - C25 C25 - Distance Angles C24 1.3764 (0.0178) C26 1.3854 (0.0161) 120.36 (1.19) C25 - C24 C26 - Distance Angles C25 1.3854 (0.0161) C21 1.3940 (0.0162) 120.89 (1.12) C26 - C25 C27 - Distance Angles C28 1.3881 (0.0160) C32 1.3893 (0.0158) 118.86 (1.11) P3 1.8412 (0.0116) 120.45 (0.89) 120.67 (0.91) C27 - C28 C32 C28 - Distance Angles C29 1.3854 (0.0167) C27 1.3881 (0.0160) 120.50 (1.15) C28 - C29 C29 - Distance Angles C30 1.3829 (0.0179) C28 1.3854 (0.0167) 120.46 (1.21) C29 - C30 C30 - Distance Angles C29 1.3829 (0.0179) C31 1.3786 (0.0183) 119.25 (1.20) C30 - C29 C31 - Distance Angles C30 1.3786 (0.0183) C32 1.3882 (0.0170) 120.67 (1.22) C31 - C30 C32 - Distance Angles C31 1.3882 (0.0170) C27 1.3893 (0.0158) 120.24 (1.19) C32 - C31 C33 - Distance Angles C38 1.3875 (0.0161) C34 1.4015 (0.0160) 118.17 (1.10) P3 1.8382 (0.0119) 120.81 (0.86) 120.90 (0.89) C33 - C38 C34 C34 - Distance Angles C35 1.3802 (0.0174) C33 1.4015 (0.0160) 120.75 (1.16) C34 - C35 C35 - Distance Angles C36 1.3733 (0.0187) C34 1.3802 (0.0174) 119.96 (1.20) C35 - C36 C36 - Distance Angles C35 1.3733 (0.0187) C37 1.3724 (0.0188) 120.51 (1.25) C36 - C35 C37 - Distance Angles C36 1.3724 (0.0187) C38 1.3901 (0.0176) 119.88 (1.26) C37 - C36 C38 - Distance Angles C33 1.3875 (0.0161) C37 1.3901 (0.0176) 120.71 (1.15) C38 - C33 C39 - Distance Angles C40 1.5274 (0.0158) P3 1.8520 (0.0111) 106.95 (0.75) C39 - C40 C40 - Distance Angles C39 1.5274 (0.0158) P4 1.8569 (0.0112) 112.21 (0.80) C40 - C39 C41 - Distance Angles C42 1.3797 (0.0175) C46 1.4001 (0.0181) 117.52 (1.24) P4 1.8373 (0.0128) 120.99 (0.96) 121.47 (1.01) C41 - C42 C46 C42 - Distance Angles C41 1.3797 (0.0175) C43 1.3817 (0.0190) 120.99 (1.33) C42 - C41 C43 - Distance Angles C44 1.3652 (0.0218) C42 1.3817 (0.0190) 120.94 (1.48) C43 - C44 C44 - Distance Angles C45 1.3622 (0.0223) C43 1.3652 (0.0218) 119.32 (1.45) C44 - C45 C45 - Distance Angles C44 1.3622 (0.0223) C46 1.3882 (0.0206) 120.66 (1.48) C45 - C44 C46 - Distance Angles C45 1.3882 (0.0206) C41 1.4001 (0.0182) 120.52 (1.41) C46 - C45 C47 - Distance Angles C52 1.3955 (0.0178) C48 1.4079 (0.0172) 117.90 (1.19) P4 1.8239 (0.0122) 121.35 (0.95) 120.62 (1.02) C47 - C52 C48 C48 - Distance Angles C49 1.3836 (0.0194) C47 1.4079 (0.0172) 120.48 (1.44) C48 - C49 C49 - Distance Angles C50 1.3695 (0.0240) C48 1.3836 (0.0194) 120.28 (1.47) C49 - C50 C50 - Distance Angles C49 1.3695 (0.0240) C51 1.3794 (0.0231) 120.62 (1.43) C50 - C49 C51 - Distance Angles C50 1.3794 (0.0232) C52 1.3866 (0.0178) 119.66 (1.54) C51 - C50 C52 - Distance Angles C51 1.3866 (0.0178) C47 1.3955 (0.0178) 121.04 (1.34) C52 - C51 C53 - Distance Angles C54 1.1794 (0.0168) Ru1 2.0412 (0.0130) 177.26 (1.06) C53 - C54 C54 - Distance Angles C53 1.1794 (0.0168) C55 1.3955 (0.0176) 175.31 (1.35) C54 - C53 C55 - Distance Angles C56 1.2173 (0.0185) C54 1.3955 (0.0176) 177.78 (1.55) C55 - C56 C56 - Distance Angles C55 1.2173 (0.0185) Si1 1.8138 (0.0148) 174.07 (1.38) C56 - C55 C57 - Distance Angles Si1 1.8384 (0.0211) C57 - C58 - Distance Angles Si1 1.8502 (0.0229) C58 - C59 - Distance Angles Si1 1.8199 (0.0206) C59 - C60 - Distance Angles C61 1.0986 (0.0167) Ru1 2.0948 (0.0141) 177.05 (1.12) C60 - C61 C61 - Distance Angles C60 1.0986 (0.0167) C62 1.4442 (0.0183) 170.69 (1.32) C61 - C60 C62 - Distance Angles C63 1.2206 (0.0174) C61 1.4442 (0.0183) 178.92 (1.47) C62 - C63 C63 - Distance Angles C62 1.2206 (0.0174) Si2 1.8244 (0.0135) 177.70 (1.31) C63 - C62 C64 - Distance Angles Si2 1.8533 (0.0149) C64 - C65 - Distance Angles Si2 1.8597 (0.0155) C65 - C66 - Distance Angles Si2 1.8412 (0.0154) C66 - Si1 - Distance Angles C56 1.8138 (0.0148) C59 1.8199 (0.0206) 108.53 (0.93) C58 1.8502 (0.0229) 109.57 (0.91) 108.38 (1.64) C57 1.8384 (0.0211) 109.25 (0.83) 112.87 (1.76) 108.21 (1.05) Si1 - C56 C59 C58 Si2 - Distance Angles C63 1.8244 (0.0136) C66 1.8412 (0.0155) 109.48 (0.69) C64 1.8533 (0.0150) 107.28 (0.74) 111.37 (0.80) C65 1.8597 (0.0155) 109.95 (0.71) 108.95 (0.84) 109.80 (0.81) Si2 - C63 C66 C64 P1 - Distance Angles C13 1.8353 (0.0113) C1 1.8371 (0.0117) 101.85 (0.51) C7 1.8342 (0.0122) 104.23 (0.56) 102.51 (0.52) Ru1 2.3525 (0.0031) 105.04 (0.38) 121.63 (0.39) 119.08 (0.37) P1 - C13 C1 C7 P2 - Distance Angles C21 1.8284 (0.0115) C15 1.8301 (0.0118) 102.40 (0.53) C14 1.8664 (0.0112) 102.47 (0.51) 100.95 (0.54) Ru1 2.3563 (0.0031) 120.43 (0.40) 118.83 (0.38) 108.98 (0.38) P2 - C21 C15 C14 P3 - Distance Angles C33 1.8382 (0.0119) C27 1.8412 (0.0116) 101.98 (0.53) C39 1.8520 (0.0111) 98.71 (0.53) 103.55 (0.51) Ru1 2.3624 (0.0031) 123.63 (0.38) 120.32 (0.38) 104.93 (0.36) P3 - C33 C27 C39 P4 - Distance Angles C47 1.8239 (0.0122) C41 1.8373 (0.0128) 101.45 (0.58) C40 1.8569 (0.0112) 103.44 (0.54) 100.20 (0.55) Ru1 2.3734 (0.0031) 116.02 (0.42) 124.56 (0.41) 108.36 (0.38) P4 - C47 C41 C40 Ru1 - Distance Angles C53 2.0412 (0.0130) C60 2.0948 (0.0141) 174.21 (0.43) P1 2.3525 (0.0031) 91.54 (0.32) 86.26 (0.31) P2 2.3563 (0.0031) 91.54 (0.33) 82.88 (0.32) 82.76 (0.11) P3 2.3624 (0.0031) 82.41 (0.31) 99.81 (0.31) 173.93 (0.10) 97.77 (0.11) P4 2.3734 (0.0031) 87.14 (0.33) 98.43 (0.32) 97.05 (0.11) 178.66 (0.11) 82.28 (0.11) Ru1 - C53 C60 P1 P2 P3 FMAP and GRID set by program FMAP 2 2 78 GRID -1.333 -1 -2 1.333 1 2 R1 = 0.0742 for 13576 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.76 at 0.3332 0.2892 0.1515 [ 0.98 A from C54 ] Deepest hole -0.81 at 0.2210 0.2418 0.2367 [ 0.80 A from RU1 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 6684 / 92460 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3332 0.2892 0.1515 1.00000 0.05 0.76 0.98 C54 1.18 C53 1.96 C55 2.08 H16 Q2 1 0.5309 0.1785 -0.1891 1.00000 0.05 0.72 1.05 C57 1.16 H57A 1.30 H57B 1.64 SI1 Q3 1 0.1530 0.2917 0.4513 1.00000 0.05 0.66 0.63 C61 0.75 C60 2.01 C62 2.38 H13A Q4 1 0.5419 0.3013 -0.0796 1.00000 0.05 0.56 0.86 SI1 1.19 C59 1.51 H59A 1.81 H59B Q5 1 0.5099 0.3641 -0.1233 1.00000 0.05 0.51 0.74 C58 0.99 H58B 1.20 H58C 1.58 SI1 Q6 1 0.6049 0.3459 -0.0498 1.00000 0.05 0.51 0.81 H59A 1.00 C59 1.42 H59B 1.83 SI1 Q7 1 0.2541 0.3330 0.3266 1.00000 0.05 0.45 1.44 RU1 1.57 P2 1.61 P1 2.04 C13 Q8 1 0.2174 0.2424 0.1998 1.00000 0.05 0.44 1.02 C53 1.40 RU1 2.07 C54 2.21 P3 Q9 1 0.2411 0.1987 0.1965 1.00000 0.05 0.44 0.95 C53 1.39 RU1 2.04 C54 2.11 P3 Q10 1 0.3193 0.3013 0.3144 1.00000 0.05 0.43 1.04 P1 1.44 RU1 2.21 C53 2.22 C7 Shortest distances between peaks (including symmetry equivalents) 8 9 0.78 4 6 0.99 7 10 1.01 4 5 1.49 5 6 1.76 1 8 1.90 7 8 2.04 8 10 2.05 1 9 2.11 2 4 2.12 9 10 2.13 7 9 2.41 1 10 2.58 3 7 2.67 2 5 2.85 2 6 2.86 1 7 2.92 Time profile in seconds ----------------------- 0.20: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: 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. 5.97: 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 11.25: Structure factors and derivatives 39.42: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 3.06: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.20: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.36: Fourier summations 0.16: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 17:45:31 Total CPU time: 60.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++