+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 17:23:40 on 04-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01SOT001 in C2/c CELL 0.71073 37.5570 7.0816 22.4980 90.000 124.860 90.000 ZERR 8.00 0.0070 0.0014 0.0040 0.000 0.030 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H O UNIT 232 216 64 V = 4909.89 F(000) = 2120.0 Mu = 0.10 mm-1 Cell Wt = 4028.05 Rho = 1.362 MERG 2 OMIT -3.00 55.00 EXTI 0.00185 SIZE 0.01 0.07 0.48 WGHT 0.06270 L.S. 4 TEMP -123.00 FVAR 0.11056 C1 1 0.338499 0.841428 0.131469 11.00000 0.04610 0.05512 = 0.03351 -0.00405 0.02709 -0.00035 C2 1 0.343350 0.953250 0.234848 11.00000 0.02944 0.03554 = 0.02534 0.00496 0.01342 0.00128 C3 1 0.319253 0.992712 0.267614 11.00000 0.02762 0.02714 = 0.02470 -0.00011 0.01434 -0.00210 C4 1 0.343018 1.038930 0.341031 11.00000 0.02163 0.03128 = 0.02390 0.00371 0.00923 0.00117 C5 1 0.321526 1.080197 0.372700 11.00000 0.02914 0.02429 = 0.02474 0.00118 0.01415 -0.00175 C6 1 0.344883 1.137721 0.450502 11.00000 0.02700 0.03345 = 0.02399 0.00225 0.01269 -0.00397 C7 1 0.413021 1.170363 0.562481 11.00000 0.03770 0.06338 = 0.02017 -0.00440 0.00965 -0.00886 C8 1 0.276414 1.075437 0.331959 11.00000 0.02956 0.02897 = 0.02672 0.00162 0.01679 0.00031 C9 1 0.251904 1.027587 0.258026 11.00000 0.02567 0.02759 = 0.02227 -0.00010 0.01128 -0.00117 C10 1 0.274310 0.989390 0.227152 11.00000 0.02987 0.02628 = 0.02283 -0.00019 0.01137 -0.00255 C11 1 0.203669 1.024363 0.215189 11.00000 0.02616 0.02850 = 0.02426 -0.00343 0.01303 -0.00086 C12 1 0.182150 0.977928 0.246878 11.00000 0.02870 0.02867 = 0.02213 -0.00501 0.01088 -0.00082 C13 1 0.136823 0.977914 0.206601 11.00000 0.02651 0.03170 = 0.02418 -0.00291 0.01255 0.00116 C14 1 0.112927 0.932257 0.239353 11.00000 0.03088 0.03613 = 0.02768 -0.00294 0.01438 -0.00108 C15 1 0.118669 0.851410 0.346324 11.00000 0.04543 0.06678 = 0.03377 0.00107 0.02629 -0.00744 C16 1 0.112607 1.023630 0.133417 11.00000 0.02643 0.03427 = 0.02638 -0.00382 0.01310 0.00015 C17 1 0.133717 1.069592 0.100973 11.00000 0.02739 0.02981 = 0.02438 -0.00060 0.01270 0.00017 C18 1 0.109313 1.126995 0.023433 11.00000 0.02834 0.03502 = 0.02842 0.00100 0.01445 0.00393 C19 1 0.039668 1.157887 -0.086554 11.00000 0.03092 0.07566 = 0.02151 0.00725 0.00871 0.00764 C20 1 0.178598 1.070831 0.141437 11.00000 0.02897 0.03061 = 0.02692 -0.00188 0.01629 -0.00125 C41 1 0.024422 0.490275 0.233151 11.00000 0.04017 0.12897 = 0.02928 -0.00768 0.01655 -0.02429 C42 1 0.024290 0.299896 0.233529 11.00000 0.07661 0.12150 = 0.02882 -0.00032 0.01332 0.05957 C43 1 0.000000 0.205633 0.250000 10.50000 0.15955 0.04683 = 0.02396 0.00000 0.00893 0.00000 AFIX 43 H43 2 0.000000 0.071483 0.250000 10.50000 -1.20000 AFIX 0 C46 1 0.000000 0.585571 0.250000 10.50000 0.08917 0.04273 = 0.02701 0.00000 0.01243 0.00000 C47 1 0.025317 0.407120 0.065633 11.00000 0.04957 0.06763 = 0.04107 0.00062 0.02328 0.01376 C48 1 -0.007928 0.313724 0.004893 11.00000 0.05667 0.05083 = 0.06738 -0.00511 0.03961 -0.00483 C49 1 0.032936 0.592625 0.060309 11.00000 0.03563 0.07314 = 0.04827 -0.01986 0.01729 -0.00153 C53 1 0.227951 0.287776 0.030849 11.00000 0.04665 0.05202 = 0.04121 -0.00328 0.02779 0.00048 C54 1 0.229070 0.105035 0.009725 11.00000 0.03980 0.04692 = 0.04056 -0.00053 0.02125 -0.00490 C55 1 0.249012 0.431079 0.021398 11.00000 0.04181 0.04324 = 0.04221 -0.00592 0.02198 -0.00247 O1 3 0.318123 0.877222 0.168536 11.00000 0.03699 0.05022 = 0.02626 -0.00592 0.01874 -0.00279 O2 3 0.381568 0.983805 0.264437 11.00000 0.03144 0.07620 = 0.03060 -0.00720 0.01657 -0.00519 O3 3 0.326990 1.188404 0.478048 11.00000 0.03573 0.06021 = 0.02908 -0.00712 0.01904 -0.00258 O4 3 0.387861 1.126269 0.485258 11.00000 0.02891 0.05324 = 0.02204 -0.00206 0.00964 -0.00114 O5 3 0.073844 0.932705 0.206711 11.00000 0.03128 0.05607 = 0.03492 -0.00081 0.01877 -0.00141 O6 3 0.139713 0.891536 0.310149 11.00000 0.03305 0.06035 = 0.02550 -0.00154 0.01741 -0.00727 O7 3 0.125729 1.190696 -0.005028 11.00000 0.03636 0.06851 = 0.03069 0.00889 0.01847 0.00209 O8 3 0.066653 1.095901 -0.011364 11.00000 0.02800 0.05705 = 0.02191 0.00363 0.00860 0.00279 H1A 2 0.340894 0.957821 0.110284 11.00000 0.07204 H1B 2 0.318633 0.754066 0.091905 11.00000 0.07005 H1C 2 0.367638 0.784993 0.163035 11.00000 0.07791 H4 2 0.374079 1.034608 0.368675 11.00000 0.02492 H7A 2 0.402627 1.304812 0.569568 11.00000 0.08951 H7B 2 0.445271 1.175098 0.577512 11.00000 0.07464 H7C 2 0.406673 1.071628 0.585146 11.00000 0.05981 H8 2 0.261057 1.100321 0.356284 11.00000 0.03445 H10 2 0.258210 0.963833 0.176085 11.00000 0.04154 H12 2 0.197889 0.947291 0.296483 11.00000 0.02073 H15A 2 0.097597 0.960206 0.338103 11.00000 0.07646 H15B 2 0.144457 0.826730 0.400619 11.00000 0.06712 H15C 2 0.099591 0.733435 0.322649 11.00000 0.06564 H16 2 0.083167 1.028103 0.109395 11.00000 0.03106 H19A 2 0.038949 1.308037 -0.085352 11.00000 0.10223 H19B 2 0.009275 1.114459 -0.107659 11.00000 0.06400 H19C 2 0.050648 1.106444 -0.112580 11.00000 0.05553 H20 2 0.194133 1.102150 0.119305 11.00000 0.02475 H41 2 0.040989 0.551943 0.219546 11.00000 0.10921 H42 2 0.040301 0.233107 0.215693 11.00000 0.12633 H46 2 0.000000 0.714609 0.250000 10.50000 0.06560 H47 2 0.044312 0.337480 0.115179 11.00000 0.07407 H48 2 -0.013518 0.184561 0.011969 11.00000 0.08046 H49 2 0.056516 0.658559 0.105857 11.00000 0.10189 H53 2 0.210800 0.314619 0.051981 11.00000 0.04825 H54 2 0.214965 0.010177 0.017247 11.00000 0.06233 H55 2 0.247804 0.560858 0.036259 11.00000 0.05923 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 Covalent radii and connectivity table for 01SOT001 in C2/c C 0.770 H 0.320 O 0.660 C1 - O1 C2 - O2 O1 C3 C3 - C10 C4 C2 C4 - C5 C3 C5 - C4 C8 C6 C6 - O3 O4 C5 C7 - O4 C8 - C5 C9 C9 - C10 C8 C11 C10 - C3 C9 C11 - C12 C20 C9 C12 - C11 C13 C13 - C16 C12 C14 C14 - O5 O6 C13 C15 - O6 C16 - C17 C13 C17 - C20 C16 C18 C18 - O7 O8 C17 C19 - O8 C20 - C17 C11 C41 - C42 C46 C42 - C43 C41 C43 - C42_$1 C42 C46 - C41_$1 C41 C47 - C49 C48 C48 - C49_$2 C47 C49 - C47 C48_$2 C53 - C55 C54 C54 - C55_$3 C53 C55 - C54_$3 C53 O1 - C2 C1 O2 - C2 O3 - C6 O4 - C6 C7 O5 - C14 O6 - C14 C15 O7 - C18 O8 - C18 C19 Operators for generating equivalent atoms: $1 -x, y, -z+1/2 $2 -x, -y+1, -z $3 -x+1/2, -y+1/2, -z 19060 Reflections read, of which 947 rejected -42 =< h =< 42, -7 =< k =< 7, -25 =< l =< 25, Max. 2-theta = 47.21 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -13 5 2 27.17 0.76 4 7.95 1 Inconsistent equivalents 3642 Unique reflections, of which 0 suppressed R(int) = 0.1666 R(sigma) = 0.0997 Friedel opposites merged Maximum memory for data reduction = 2687 / 44635 Special position constraints for C43 x = 0.0000 z = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for C46 x = 0.0000 z = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for H46 x = 0.0000 z = 0.2500 sof = 0.50000 Input constraints retained (at least in part) for sof 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 = 3753 / 572484 wR2 = 0.1481 before cycle 1 for 3642 data and 442 / 442 parameters GooF = S = 1.010; Restrained GooF = 1.010 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.11055 0.00036 -0.039 OSF 2 0.00186 0.00032 0.025 EXTI Mean shift/esd = 0.009 Maximum = -0.039 for OSF Max. shift = 0.002 A for H1B Max. dU = 0.000 for H15B Least-squares cycle 2 Maximum vector length = 511 Memory required = 3753 / 572484 wR2 = 0.1481 before cycle 2 for 3642 data and 442 / 442 parameters GooF = S = 1.011; Restrained GooF = 1.011 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.11054 0.00036 -0.013 OSF 2 0.00186 0.00032 0.009 EXTI Mean shift/esd = 0.003 Maximum = -0.015 for x H19A Max. shift = 0.001 A for H19A Max. dU = 0.000 for H41 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3753 / 572484 wR2 = 0.1481 before cycle 3 for 3642 data and 442 / 442 parameters GooF = S = 1.011; Restrained GooF = 1.011 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.11054 0.00036 0.001 OSF 2 0.00186 0.00032 0.001 EXTI Mean shift/esd = 0.001 Maximum = 0.005 for y H7A Max. shift = 0.000 A for H19A Max. dU = 0.000 for H41 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3753 / 572484 wR2 = 0.1481 before cycle 4 for 3642 data and 442 / 442 parameters GooF = S = 1.011; Restrained GooF = 1.011 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.11054 0.00036 0.001 OSF 2 0.00186 0.00032 0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for U11 H41 Max. shift = 0.000 A for H19A Max. dU = 0.000 for H41 Largest correlation matrix elements 0.763 U13 C48 / U33 C48 0.702 U13 C47 / U33 C47 0.680 U13 C13 / U33 C13 0.732 U13 C15 / U33 C15 0.697 U13 C3 / U33 C3 0.678 U13 C55 / U33 C55 0.728 U13 C1 / U33 C1 0.697 U13 C15 / U11 C15 0.677 U13 O6 / U11 O6 0.723 U13 C1 / U11 C1 0.695 z C1 / x C1 0.675 U13 O1 / U11 O1 0.714 U13 C48 / U11 C48 0.689 U13 O3 / U33 O3 0.674 U13 C8 / U33 C8 0.713 U13 C53 / U33 C53 0.687 z C15 / x C15 0.673 U13 C11 / U33 C11 0.712 U13 O6 / U33 O6 0.683 U13 O5 / U11 O5 0.672 U13 C49 / U33 C49 0.704 U13 O1 / U33 O1 0.682 U13 C53 / U11 C53 0.672 U13 O7 / U33 O7 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H43 0.0000 0.0714 0.2500 43 0.950 0.000 C43 C42_$1 C42 01SOT001 in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.33850 0.84143 0.13147 1.00000 0.04612 0.05505 0.03352 -0.00402 0.02711 -0.00032 0.04243 0.00933 0.00013 0.00055 0.00020 0.00000 0.00251 0.00232 0.00196 0.00170 0.00196 0.00190 0.00088 C2 0.34335 0.95326 0.23485 1.00000 0.02949 0.03550 0.02531 0.00495 0.01342 0.00128 0.03137 0.00715 0.00010 0.00038 0.00015 0.00000 0.00196 0.00168 0.00165 0.00128 0.00155 0.00139 0.00071 C3 0.31925 0.99271 0.26761 1.00000 0.02757 0.02715 0.02467 -0.00011 0.01431 -0.00209 0.02682 0.00633 0.00009 0.00036 0.00014 0.00000 0.00176 0.00151 0.00160 0.00114 0.00144 0.00126 0.00068 C4 0.34302 1.03894 0.34103 1.00000 0.02162 0.03126 0.02389 0.00371 0.00922 0.00117 0.02773 0.00697 0.00010 0.00037 0.00015 0.00000 0.00177 0.00164 0.00157 0.00122 0.00144 0.00128 0.00069 C5 0.32153 1.08020 0.37270 1.00000 0.02910 0.02431 0.02468 0.00117 0.01412 -0.00175 0.02674 0.00638 0.00009 0.00036 0.00014 0.00000 0.00183 0.00144 0.00151 0.00114 0.00143 0.00122 0.00067 C6 0.34488 1.13772 0.45050 1.00000 0.02698 0.03343 0.02395 0.00225 0.01266 -0.00397 0.02920 0.00658 0.00010 0.00038 0.00014 0.00000 0.00190 0.00162 0.00160 0.00119 0.00155 0.00128 0.00070 C7 0.41302 1.17036 0.56249 1.00000 0.03769 0.06335 0.02015 -0.00439 0.00964 -0.00885 0.04430 0.00789 0.00013 0.00057 0.00016 0.00000 0.00236 0.00249 0.00168 0.00152 0.00169 0.00183 0.00090 C8 0.27641 1.07543 0.33196 1.00000 0.02957 0.02898 0.02669 0.00160 0.01680 0.00029 0.02800 0.00664 0.00010 0.00038 0.00015 0.00000 0.00190 0.00153 0.00158 0.00118 0.00152 0.00126 0.00069 C9 0.25190 1.02759 0.25802 1.00000 0.02566 0.02758 0.02226 -0.00010 0.01127 -0.00117 0.02653 0.00631 0.00009 0.00037 0.00014 0.00000 0.00173 0.00158 0.00153 0.00113 0.00138 0.00125 0.00067 C10 0.27431 0.98940 0.22715 1.00000 0.02984 0.02631 0.02277 -0.00017 0.01133 -0.00253 0.02840 0.00666 0.00009 0.00037 0.00015 0.00000 0.00192 0.00150 0.00165 0.00120 0.00154 0.00127 0.00070 C11 0.20367 1.02436 0.21519 1.00000 0.02614 0.02850 0.02424 -0.00343 0.01302 -0.00087 0.02707 0.00619 0.00009 0.00037 0.00014 0.00000 0.00176 0.00155 0.00157 0.00114 0.00142 0.00123 0.00068 C12 0.18215 0.97793 0.24687 1.00000 0.02866 0.02866 0.02210 -0.00499 0.01085 -0.00081 0.02855 0.00652 0.00009 0.00037 0.00015 0.00000 0.00185 0.00158 0.00164 0.00120 0.00151 0.00128 0.00070 C13 0.13682 0.97791 0.20660 1.00000 0.02650 0.03169 0.02414 -0.00292 0.01252 0.00116 0.02855 0.00639 0.00009 0.00037 0.00014 0.00000 0.00177 0.00155 0.00157 0.00118 0.00145 0.00126 0.00069 C14 0.11293 0.93226 0.23935 1.00000 0.03093 0.03612 0.02766 -0.00294 0.01441 -0.00108 0.03289 0.00698 0.00010 0.00039 0.00015 0.00000 0.00202 0.00167 0.00171 0.00127 0.00158 0.00139 0.00073 C15 0.11867 0.85141 0.34632 1.00000 0.04540 0.06674 0.03378 0.00106 0.02629 -0.00742 0.04657 0.00944 0.00013 0.00059 0.00019 0.00000 0.00243 0.00255 0.00203 0.00175 0.00194 0.00206 0.00091 C16 0.11261 1.02363 0.13341 1.00000 0.02640 0.03425 0.02636 -0.00382 0.01309 0.00014 0.03013 0.00719 0.00011 0.00039 0.00015 0.00000 0.00192 0.00171 0.00168 0.00124 0.00154 0.00138 0.00073 C17 0.13372 1.06958 0.10097 1.00000 0.02733 0.02981 0.02433 -0.00061 0.01265 0.00018 0.02835 0.00650 0.00009 0.00037 0.00014 0.00000 0.00183 0.00155 0.00153 0.00119 0.00142 0.00126 0.00068 C18 0.10931 1.12700 0.02343 1.00000 0.02835 0.03502 0.02838 0.00100 0.01444 0.00391 0.03158 0.00687 0.00010 0.00039 0.00015 0.00000 0.00200 0.00170 0.00169 0.00127 0.00163 0.00129 0.00074 C19 0.03967 1.15789 -0.08656 1.00000 0.03091 0.07565 0.02148 0.00728 0.00868 0.00764 0.04624 0.00899 0.00012 0.00060 0.00017 0.00000 0.00229 0.00277 0.00178 0.00161 0.00172 0.00189 0.00093 C20 0.17860 1.07083 0.14144 1.00000 0.02899 0.03060 0.02690 -0.00189 0.01630 -0.00125 0.02864 0.00664 0.00010 0.00038 0.00015 0.00000 0.00188 0.00158 0.00160 0.00121 0.00152 0.00129 0.00069 C41 0.02442 0.49026 0.23315 1.00000 0.04014 0.12909 0.02922 -0.00767 0.01650 -0.02437 0.06803 0.00917 0.00013 0.00081 0.00020 0.00000 0.00258 0.00462 0.00211 0.00237 0.00191 0.00281 0.00139 C42 0.02429 0.29986 0.23353 1.00000 0.07667 0.12131 0.02886 -0.00036 0.01333 0.05952 0.08514 0.01265 0.00017 0.00088 0.00021 0.00000 0.00383 0.00501 0.00231 0.00267 0.00235 0.00358 0.00182 C43 0.00000 0.20560 0.25000 0.50000 0.15949 0.04679 0.02399 0.00000 0.00891 0.00000 0.10138 0.00615 0.00000 0.00087 0.00000 0.00000 0.00882 0.00359 0.00325 0.00000 0.00440 0.00000 0.00329 H43 0.00000 0.07145 0.25000 0.50000 0.12166 0.00000 0.00000 C46 0.00000 0.58559 0.25000 0.50000 0.08908 0.04277 0.02697 0.00000 0.01246 0.00000 0.06466 0.00569 0.00000 0.00080 0.00000 0.00000 0.00512 0.00334 0.00274 0.00000 0.00314 0.00000 0.00191 C47 0.02532 0.40713 0.06563 1.00000 0.04951 0.06761 0.04105 0.00062 0.02324 0.01373 0.05422 0.00926 0.00013 0.00056 0.00019 0.00000 0.00253 0.00263 0.00223 0.00195 0.00204 0.00204 0.00099 C48 -0.00793 0.31371 0.00489 1.00000 0.05665 0.05083 0.06736 -0.00510 0.03959 -0.00483 0.05593 0.00953 0.00013 0.00053 0.00022 0.00000 0.00277 0.00229 0.00282 0.00202 0.00248 0.00197 0.00102 C49 0.03294 0.59261 0.06031 1.00000 0.03564 0.07316 0.04818 -0.01985 0.01723 -0.00151 0.05613 0.00883 0.00012 0.00060 0.00021 0.00000 0.00234 0.00278 0.00243 0.00208 0.00201 0.00197 0.00103 C53 0.22795 0.28777 0.03085 1.00000 0.04658 0.05201 0.04119 -0.00327 0.02776 0.00050 0.04507 0.00803 0.00012 0.00049 0.00017 0.00000 0.00238 0.00214 0.00200 0.00155 0.00195 0.00170 0.00088 C54 0.22907 0.10504 0.00972 1.00000 0.03981 0.04693 0.04051 -0.00052 0.02124 -0.00490 0.04339 0.00782 0.00011 0.00048 0.00017 0.00000 0.00226 0.00219 0.00193 0.00154 0.00182 0.00166 0.00088 C55 0.24901 0.43107 0.02140 1.00000 0.04177 0.04319 0.04220 -0.00590 0.02196 -0.00244 0.04355 0.00771 0.00011 0.00048 0.00017 0.00000 0.00220 0.00206 0.00195 0.00156 0.00179 0.00163 0.00084 O1 0.31812 0.87722 0.16853 1.00000 0.03698 0.05021 0.02623 -0.00593 0.01873 -0.00281 0.03743 0.00453 0.00007 0.00028 0.00010 0.00000 0.00137 0.00129 0.00114 0.00090 0.00107 0.00097 0.00055 O2 0.38157 0.98381 0.26444 1.00000 0.03142 0.07620 0.03057 -0.00722 0.01654 -0.00521 0.04673 0.00504 0.00007 0.00033 0.00011 0.00000 0.00145 0.00164 0.00126 0.00107 0.00115 0.00119 0.00061 O3 0.32699 1.18840 0.47805 1.00000 0.03569 0.06020 0.02904 -0.00712 0.01900 -0.00260 0.04136 0.00469 0.00007 0.00030 0.00010 0.00000 0.00141 0.00145 0.00119 0.00097 0.00115 0.00106 0.00059 O4 0.38786 1.12627 0.48526 1.00000 0.02887 0.05324 0.02200 -0.00206 0.00960 -0.00114 0.03750 0.00452 0.00007 0.00027 0.00010 0.00000 0.00138 0.00134 0.00109 0.00090 0.00104 0.00097 0.00055 O5 0.07384 0.93271 0.20671 1.00000 0.03125 0.05606 0.03487 -0.00080 0.01873 -0.00140 0.04082 0.00496 0.00007 0.00028 0.00011 0.00000 0.00148 0.00137 0.00123 0.00101 0.00115 0.00104 0.00056 O6 0.13971 0.89154 0.31015 1.00000 0.03302 0.06032 0.02547 -0.00155 0.01738 -0.00729 0.03923 0.00456 0.00007 0.00029 0.00010 0.00000 0.00137 0.00138 0.00114 0.00095 0.00107 0.00100 0.00056 O7 0.12573 1.19069 -0.00503 1.00000 0.03634 0.06848 0.03066 0.00889 0.01845 0.00211 0.04555 0.00505 0.00007 0.00032 0.00011 0.00000 0.00147 0.00154 0.00122 0.00103 0.00118 0.00112 0.00062 O8 0.06665 1.09589 -0.01136 1.00000 0.02798 0.05703 0.02188 0.00363 0.00858 0.00279 0.03884 0.00467 0.00007 0.00029 0.00010 0.00000 0.00133 0.00135 0.00108 0.00091 0.00099 0.00098 0.00056 H1A 0.34087 0.95772 0.11025 1.00000 0.07205 0.08614 0.00119 0.00531 0.00196 0.00000 0.01193 H1B 0.31866 0.75390 0.09187 1.00000 0.07015 0.09212 0.00122 0.00497 0.00199 0.00000 0.01146 H1C 0.36764 0.78488 0.16303 1.00000 0.07787 0.09406 0.00138 0.00526 0.00210 0.00000 0.01294 H4 0.37408 1.03462 0.36867 1.00000 0.02478 0.06265 0.00092 0.00344 0.00136 0.00000 0.00726 H7A 0.40264 1.30490 0.56950 1.00000 0.08981 0.09642 0.00134 0.00596 0.00213 0.00000 0.01348 H7B 0.44531 1.17510 0.57753 1.00000 0.07473 0.09354 0.00140 0.00495 0.00198 0.00000 0.01193 H7C 0.40666 1.07164 0.58514 1.00000 0.05958 0.07826 0.00111 0.00487 0.00182 0.00000 0.01072 H8 0.26106 1.10033 0.35628 1.00000 0.03423 0.06368 0.00094 0.00357 0.00145 0.00000 0.00772 H10 0.25821 0.96384 0.17607 1.00000 0.04151 0.07191 0.00096 0.00394 0.00161 0.00000 0.00837 H12 0.19788 0.94729 0.29647 1.00000 0.02073 0.06045 0.00084 0.00327 0.00141 0.00000 0.00670 H15A 0.09759 0.96024 0.33813 1.00000 0.07635 0.08678 0.00126 0.00524 0.00196 0.00000 0.01252 H15B 0.14444 0.82672 0.40061 1.00000 0.06743 0.09120 0.00125 0.00468 0.00213 0.00000 0.01083 H15C 0.09959 0.73340 0.32267 1.00000 0.06573 0.08918 0.00119 0.00513 0.00184 0.00000 0.01092 H16 0.08316 1.02805 0.10939 1.00000 0.03100 0.06636 0.00096 0.00372 0.00148 0.00000 0.00819 H19A 0.03888 1.30814 -0.08539 1.00000 0.10234 0.09999 0.00141 0.00654 0.00221 0.00000 0.01525 H19B 0.00926 1.11431 -0.10766 1.00000 0.06388 0.08907 0.00133 0.00470 0.00187 0.00000 0.01107 H19C 0.05066 1.10654 -0.11258 1.00000 0.05555 0.07839 0.00114 0.00451 0.00182 0.00000 0.01035 H20 0.19413 1.10224 0.11928 1.00000 0.02458 0.05954 0.00087 0.00339 0.00135 0.00000 0.00702 H41 0.04096 0.55196 0.21956 1.00000 0.10891 0.11127 0.00163 0.00618 0.00247 0.00000 0.01673 H42 0.04033 0.23289 0.21570 1.00000 0.12653 0.11700 0.00169 0.00680 0.00261 0.00000 0.01806 H46 0.00000 0.71477 0.25000 0.50000 0.06589 0.05529 0.00000 0.00781 0.00000 0.00000 0.01620 H47 0.04434 0.33746 0.11519 1.00000 0.07406 0.08918 0.00125 0.00495 0.00205 0.00000 0.01145 H48 -0.01349 0.18460 0.01200 1.00000 0.08059 0.09203 0.00127 0.00555 0.00208 0.00000 0.01283 H49 0.05650 0.65855 0.10583 1.00000 0.10181 0.10761 0.00148 0.00574 0.00242 0.00000 0.01520 H53 0.21079 0.31467 0.05196 1.00000 0.04821 0.07239 0.00104 0.00420 0.00163 0.00000 0.00888 H54 0.21498 0.01033 0.01724 1.00000 0.06226 0.08179 0.00114 0.00495 0.00185 0.00000 0.01110 H55 0.24778 0.56087 0.03621 1.00000 0.05927 0.08047 0.00109 0.00479 0.00175 0.00000 0.01015 Final Structure Factor Calculation for 01SOT001 in C2/c Total number of l.s. parameters = 442 Maximum vector length = 511 Memory required = 3311 / 21973 wR2 = 0.1481 before cycle 5 for 3642 data and 0 / 442 parameters GooF = S = 1.011; Restrained GooF = 1.011 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0527 for 2251 Fo > 4sig(Fo) and 0.0946 for all 3642 data wR2 = 0.1481, GooF = S = 1.011, Restrained GooF = 1.011 for all data Occupancy sum of asymmetric unit = 37.00 for non-hydrogen and 27.00 for hydrogen atoms Principal mean square atomic displacements U 0.0558 0.0461 0.0254 C1 0.0385 0.0324 0.0233 C2 0.0305 0.0253 0.0246 C3 0.0348 0.0288 0.0196 C4 0.0323 0.0253 0.0226 C5 0.0389 0.0253 0.0234 C6 0.0670 0.0465 0.0194 C7 0.0299 0.0294 0.0247 C8 0.0307 0.0271 0.0218 C9 0.0372 0.0256 0.0224 C10 0.0314 0.0275 0.0223 C11 0.0368 0.0295 0.0194 C12 0.0353 0.0272 0.0231 C13 0.0376 0.0346 0.0265 C14 0.0699 0.0434 0.0264 C15 0.0374 0.0285 0.0245 C16 0.0316 0.0295 0.0240 C17 0.0377 0.0309 0.0262 C18 0.0770 0.0423 0.0194 C19 0.0315 0.0286 0.0257 C20 0.1362 0.0396 0.0283 C41 0.1866 0.0406 0.0282 C42 0.2335 0.0468 0.0238 C43 may be split into 0.0022 0.2056 0.2430 and -0.0022 0.2056 0.2570 0.1244 0.0428 0.0268 C46 0.0785 0.0433 0.0409 C47 0.0690 0.0513 0.0475 C48 0.0905 0.0441 0.0338 C49 0.0531 0.0468 0.0353 C53 0.0509 0.0420 0.0373 C54 0.0501 0.0440 0.0366 C55 0.0516 0.0375 0.0232 O1 0.0773 0.0338 0.0291 O2 0.0618 0.0360 0.0263 O3 0.0534 0.0381 0.0211 O4 0.0561 0.0354 0.0309 O5 0.0625 0.0313 0.0239 O6 0.0708 0.0376 0.0283 O7 0.0574 0.0389 0.0202 O8 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.013 0.019 0.026 0.035 0.046 0.061 0.083 0.126 1.000 Number in group 426. 352. 331. 355. 369. 385. 351. 350. 358. 365. GooF 0.917 0.952 1.000 1.042 1.015 1.038 1.087 0.996 0.980 1.078 K -0.145 0.880 0.964 0.891 0.987 0.952 1.004 1.009 1.025 1.037 Resolution(A) 0.89 0.92 0.96 1.00 1.05 1.12 1.21 1.33 1.52 1.91 inf Number in group 367. 366. 365. 360. 365. 368. 356. 366. 363. 366. GooF 0.916 0.968 0.991 0.985 1.005 0.992 0.972 1.063 1.019 1.173 K 0.988 0.994 0.995 1.017 1.053 1.073 1.046 1.039 1.054 1.015 R1 0.268 0.183 0.157 0.126 0.102 0.086 0.074 0.078 0.051 0.045 Recommended weighting scheme: WGHT 0.0623 0.0000 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) -1 1 2 77.45 5.42 4.17 0.005 5.90 -9 3 15 -37.66 85.25 4.04 0.019 1.24 -14 4 14 103.87 229.77 3.69 0.031 1.19 -26 4 12 695.78 507.47 3.68 0.046 1.10 -30 0 2 1756.71 3104.57 3.65 0.115 1.09 -24 2 7 185.39 463.27 3.61 0.044 1.42 -19 3 20 434.78 187.19 3.57 0.028 1.02 -19 1 24 680.86 407.11 3.48 0.041 0.92 2 0 2 584.49 454.41 3.43 0.044 6.46 -29 3 20 -53.58 141.24 3.32 0.024 0.97 -4 0 20 1470.78 2015.19 3.28 0.092 0.99 -9 1 3 9014.88 11256.54 3.25 0.218 3.59 -9 1 5 17987.63 22478.50 3.25 0.308 3.37 -1 1 5 698.60 501.86 3.20 0.046 3.44 -32 0 18 823.37 1201.25 3.16 0.071 1.07 -11 1 6 9471.36 12038.76 3.13 0.226 2.88 -6 0 2 15088.60 19052.75 3.11 0.284 6.26 -15 3 3 1124.18 774.32 3.09 0.057 1.68 2 0 4 -76.00 96.98 3.02 0.020 3.86 23 3 1 287.19 133.94 3.02 0.024 1.13 -18 0 20 25578.27 19580.71 3.01 0.288 1.12 6 4 7 47.33 156.89 2.99 0.026 1.31 0 0 4 308143.38 236602.42 2.97 1.000 4.62 1 1 16 560.94 776.66 2.94 0.057 1.12 -4 6 8 1010.24 1279.65 2.92 0.074 1.08 -8 2 8 301.09 200.32 2.87 0.029 2.20 -25 3 21 53.71 247.50 2.86 0.032 0.96 -29 3 15 -61.06 50.43 2.80 0.015 1.08 -24 2 10 473.79 687.68 2.80 0.054 1.42 4 2 9 68.23 195.65 2.78 0.029 1.57 -23 1 18 480.19 297.73 2.78 0.035 1.20 3 5 2 96.99 199.25 2.78 0.029 1.37 -10 6 8 295.84 25.98 2.77 0.010 1.08 3 1 17 209.72 410.85 2.74 0.042 1.01 -28 0 4 -85.92 126.88 2.73 0.023 1.24 13 1 2 2540.38 2000.31 2.73 0.092 1.95 -22 2 2 2395.36 1920.18 2.71 0.090 1.40 -33 3 7 275.71 54.49 2.69 0.015 1.00 -13 5 7 1547.38 1140.30 2.68 0.069 1.25 -19 3 11 5123.35 3958.40 2.66 0.129 1.42 -4 4 6 134.46 72.40 2.65 0.017 1.59 -30 2 18 345.51 532.20 2.63 0.047 1.06 -2 4 10 -44.10 31.93 2.63 0.012 1.32 23 1 8 238.40 482.09 2.62 0.045 0.94 -19 1 14 1812.48 2384.38 2.60 0.100 1.51 -23 3 22 1804.51 1414.04 2.60 0.077 0.94 10 6 4 1102.76 873.46 2.60 0.061 1.03 -21 1 18 1635.58 1287.17 2.59 0.074 1.22 17 3 2 329.74 495.32 2.58 0.046 1.33 -15 3 13 67.08 2.29 2.57 0.003 1.39 Time profile in seconds ----------------------- 0.17: Read and process instructions 0.00: Fit rigid groups 0.02: Interpret restraints etc. 0.00: Generate connectivity array 0.02: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 2.70: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.14: Structure factors and derivatives 4.95: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 1.16: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.00: Merge reflections for Fourier and .fcf 0.00: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 17:23:52 Total CPU time: 11.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++