+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - MSDOS 32-BIT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-1 + + S92 started at 11:52:34 on 20-Oct-1999 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P-1 CELL 0.71073 8.451 11.797 14.488 104.81 103.71 98.48 ZERR 4.00 0.002 0.002 0.003 0.03 0.03 0.03 LATT 1 SFAC C H N O S UNIT 48 48 16 12 4 V = 1322.93 F(000) = 608.0 Mu = 0.26 mm-1 Cell Wt = 1169.26 Rho = 1.468 FMAP 2 OMIT 0 0 1 OMIT 0 -1 1 PLAN 20 L.S. 4 BOND WGHT 0.0631 0.0000 FVAR 0.31800 S1 5 0.23896 0.90913 0.12174 11.00000 0.03533 0.06087 = 0.05066 0.02699 0.01328 0.01043 O1 4 0.16600 0.79140 0.12068 11.00000 0.04390 0.06152 = 0.06064 0.02699 0.01444 -0.00304 O2 4 0.13517 0.98698 0.09408 11.00000 0.04230 0.08447 = 0.06745 0.04245 0.01785 0.02730 O3 4 0.71235 1.35565 0.54343 11.00000 0.18059 0.05372 = 0.08995 0.01961 -0.01887 0.03338 N1 3 0.72425 1.16079 0.51793 11.00000 0.05990 0.04178 = 0.05016 0.01686 0.01057 0.01064 N2 3 0.35060 0.89503 0.04203 11.00000 0.04055 0.05755 = 0.04957 0.03115 0.01610 0.01332 N3 3 0.60090 0.87514 0.00968 11.00000 0.03962 0.04995 = 0.04277 0.01729 0.01255 0.00929 N4 3 0.60556 0.67477 0.07730 11.00000 0.05211 0.04575 = 0.04172 0.01402 0.01262 0.01234 C1 1 0.88927 1.31018 0.67493 11.00000 0.07361 0.05687 = 0.06104 0.00731 0.01595 0.01024 C2 1 0.76866 1.27962 0.57320 11.00000 0.07070 0.04665 = 0.06189 0.01895 0.01802 0.00882 C3 1 0.60886 1.10620 0.42483 11.00000 0.05213 0.04211 = 0.04587 0.01827 0.01870 0.01107 C4 1 0.56238 0.98063 0.39243 11.00000 0.05234 0.04512 = 0.04369 0.02072 0.01447 0.01632 C5 1 0.44884 0.91983 0.30090 11.00000 0.05479 0.03919 = 0.05060 0.02011 0.01806 0.00931 C6 1 0.38047 0.98367 0.23960 11.00000 0.04049 0.04827 = 0.04503 0.02134 0.01556 0.01201 C7 1 0.42480 1.10841 0.27222 11.00000 0.06600 0.04778 = 0.05879 0.02786 0.01069 0.01862 C8 1 0.53566 1.16835 0.36251 11.00000 0.07249 0.03957 = 0.06136 0.02013 0.01240 0.01324 C9 1 0.47920 0.83230 0.04375 11.00000 0.03722 0.04216 = 0.03066 0.01357 0.00588 0.00664 C10 1 0.72475 0.81558 0.00988 11.00000 0.04298 0.05426 = 0.04976 0.01817 0.01633 0.00825 C11 1 0.72794 0.71877 0.04416 11.00000 0.05170 0.05061 = 0.04936 0.01477 0.01631 0.01638 C12 1 0.48012 0.73078 0.07565 11.00000 0.04684 0.04825 = 0.04058 0.01772 0.01201 0.00792 H1A 2 0.77266 1.11501 0.54944 11.00000 0.06444 H1B 2 0.92377 1.24306 0.69107 11.00000 0.07894 H1C 2 0.83487 1.34437 0.73000 11.00000 0.12442 H1D 2 0.97849 1.37700 0.68067 11.00000 0.12688 H2A 2 0.37051 0.95801 0.02327 11.00000 0.05371 H4 2 0.60575 0.93562 0.43463 11.00000 0.04689 H5 2 0.41663 0.83994 0.28143 11.00000 0.04772 H7 2 0.38046 1.14831 0.23445 11.00000 0.06122 H8 2 0.55521 1.25295 0.38405 11.00000 0.06914 H10 2 0.80041 0.84973 -0.01445 11.00000 0.05594 H11 2 0.82380 0.68265 0.05055 11.00000 0.06222 H12 2 0.39420 0.69827 0.09284 11.00000 0.05676 S21 5 0.50845 0.50786 -0.23770 11.00000 0.04011 0.04086 = 0.04700 0.01551 0.00988 0.00869 O21 4 0.56288 0.62168 -0.25085 11.00000 0.05169 0.04036 = 0.06105 0.01955 0.01257 0.00287 O22 4 0.62869 0.44615 -0.19839 11.00000 0.04461 0.05760 = 0.06111 0.02543 0.01322 0.02165 O23 4 0.08025 -0.00078 -0.60246 11.00000 0.10347 0.04341 = 0.06272 0.01800 0.01499 0.01885 N21 3 0.05063 0.18077 -0.62031 11.00000 0.05677 0.04040 = 0.04521 0.01168 0.00286 0.01068 N22 3 0.39700 0.52566 -0.15949 11.00000 0.04479 0.04539 = 0.04429 0.01800 0.01276 0.01609 N23 3 0.16010 0.54641 -0.11254 11.00000 0.04463 0.06092 = 0.04607 0.01368 0.01217 0.01143 N24 3 0.08141 0.69389 -0.23119 11.00000 0.05959 0.06664 = 0.06682 0.02161 0.00655 0.02951 C21 1 -0.11222 0.00292 -0.74968 11.00000 0.07027 0.06436 = 0.05223 -0.00029 0.01504 -0.00294 C22 1 0.01526 0.05870 -0.65155 11.00000 0.05598 0.04701 = 0.04655 0.00939 0.01801 0.00810 C23 1 0.16113 0.25653 -0.52905 11.00000 0.04664 0.03994 = 0.04424 0.01178 0.01050 0.01397 C24 1 0.23815 0.37097 -0.52446 11.00000 0.07901 0.04640 = 0.04270 0.02109 0.00577 0.00961 C25 1 0.34338 0.44819 -0.43575 11.00000 0.07016 0.03858 = 0.05343 0.02084 0.00969 0.00403 C26 1 0.37237 0.41248 -0.35133 11.00000 0.04155 0.03535 = 0.04397 0.01380 0.01326 0.00894 C27 1 0.29503 0.29865 -0.35554 11.00000 0.05426 0.04343 = 0.04140 0.02046 0.01010 0.00880 C28 1 0.18814 0.22146 -0.44349 11.00000 0.05679 0.03554 = 0.04971 0.01593 0.01203 0.00515 C29 1 0.25688 0.57510 -0.16757 11.00000 0.03979 0.03904 = 0.03746 0.00398 0.00320 0.00618 C210 1 0.02640 0.59446 -0.11747 11.00000 0.04649 0.08482 = 0.06279 0.01648 0.01900 0.01839 C211 1 -0.01449 0.66461 -0.17575 11.00000 0.05383 0.08146 = 0.06848 0.01124 0.01342 0.02913 C212 1 0.21727 0.64823 -0.22641 11.00000 0.05361 0.05991 = 0.05880 0.02319 0.01098 0.02029 H21A 2 0.00941 0.21436 -0.66617 11.00000 0.06326 H21B 2 -0.12843 -0.07151 -0.76694 11.00000 0.11402 H21C 2 -0.09304 0.02798 -0.80145 11.00000 0.13544 H21D 2 -0.21811 0.01943 -0.74861 11.00000 0.15131 H22A 2 0.39178 0.46945 -0.13612 11.00000 0.06763 H24 2 0.21533 0.39141 -0.58748 11.00000 0.06124 H25 2 0.38998 0.52510 -0.43372 11.00000 0.07445 H27 2 0.30992 0.27516 -0.29743 11.00000 0.05551 H28 2 0.13578 0.14648 -0.44273 11.00000 0.06356 H210 2 -0.03486 0.57113 -0.08543 11.00000 0.08845 H211 2 -0.09969 0.70101 -0.17714 11.00000 0.07815 H212 2 0.27537 0.66905 -0.26803 11.00000 0.08099 HKLF 4 Covalent radii and connectivity table for s92 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 S1 - O2 O1 N2 C6 O1 - S1 O2 - S1 O3 - C2 N1 - C2 C3 N2 - C9 S1 N3 - C9 C10 N4 - C12 C11 C1 - C2 C2 - O3 N1 C1 C3 - N1 C8 C4 C4 - C5 C3 C5 - C4 C6 C6 - C5 C7 S1 C7 - C8 C6 C8 - C7 C3 C9 - N3 C12 N2 C10 - N3 C11 C11 - N4 C10 C12 - N4 C9 S21 - O21 O22 N22 C26 O21 - S21 O22 - S21 O23 - C22 N21 - C22 C23 N22 - C29 S21 N23 - C210 C29 N24 - C212 C211 C21 - C22 C22 - O23 N21 C21 C23 - C28 C24 N21 C24 - C25 C23 C25 - C26 C24 C26 - C25 C27 S21 C27 - C28 C26 C28 - C27 C23 C29 - N23 C212 N22 C210 - N23 C211 C211 - N24 C210 C212 - N24 C29 11386 Reflections read, of which 4 rejected -9 =< h =< 9, -13 =< k =< 13, -17 =< l =< 17, Max. 2-theta = 50.05 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 4 0 0 4.24 0.28 3 1.70 0 1 0 2.61 0.10 3 2.14 8 0 4 2.60 1.13 2 6.54 -8 0 12 1.08 0.82 2 9.86 3 -7 14 2.38 1.52 2 10.80 5 Inconsistent equivalents 4612 Unique reflections, of which 0 suppressed R(int) = 0.0551 R(sigma) = 0.0740 Friedel opposites merged Maximum memory for data reduction = 2973 / 45834 Least-squares cycle 1 Maximum vector length = 511 Memory required = 4048 / 596638 wR2 = 0.1256 before cycle 1 for 4612 data and 457 / 457 parameters GooF = S = 0.970; Restrained GooF = 0.970 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0631 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31800 0.00068 -0.006 OSF Mean shift/esd = 0.004 Maximum = -0.046 for y S21 Max. shift = 0.000 A for H21D Max. dU = 0.000 for H21D Least-squares cycle 2 Maximum vector length = 511 Memory required = 4048 / 596638 wR2 = 0.1256 before cycle 2 for 4612 data and 457 / 457 parameters GooF = S = 0.970; Restrained GooF = 0.970 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0631 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31799 0.00068 -0.002 OSF Mean shift/esd = 0.001 Maximum = -0.016 for y S21 Max. shift = 0.000 A for H21C Max. dU = 0.000 for H21D Least-squares cycle 3 Maximum vector length = 511 Memory required = 4048 / 596638 wR2 = 0.1256 before cycle 3 for 4612 data and 457 / 457 parameters GooF = S = 0.970; Restrained GooF = 0.970 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0631 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31800 0.00068 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H21C Max. dU = 0.000 for H21C Least-squares cycle 4 Maximum vector length = 511 Memory required = 4048 / 596638 wR2 = 0.1256 before cycle 4 for 4612 data and 457 / 457 parameters GooF = S = 0.970; Restrained GooF = 0.970 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0631 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31800 0.00068 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y S1 Max. shift = 0.000 A for H21D Max. dU = 0.000 for H210 Largest correlation matrix elements 0.545 U23 O2 / U33 O2 0.534 U23 N2 / U33 N2 0.502 U23 C25 / U33 C25 0.538 U11 H21B / U22 C21 0.519 y H5 / y C5 0.537 U23 C7 / U33 C7 0.510 U23 S1 / U33 S1 s92 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq S1 0.23896 0.90913 0.12174 1.00000 0.03533 0.06087 0.05066 0.02699 0.01328 0.01043 0.04683 0.00170 0.00009 0.00006 0.00006 0.00000 0.00042 0.00045 0.00051 0.00036 0.00036 0.00031 0.00023 O1 0.16600 0.79140 0.12068 1.00000 0.04389 0.06152 0.06063 0.02699 0.01444 -0.00304 0.05541 0.00432 0.00023 0.00016 0.00015 0.00000 0.00118 0.00116 0.00146 0.00101 0.00105 0.00090 0.00054 O2 0.13517 0.98698 0.09408 1.00000 0.04229 0.08446 0.06746 0.04244 0.01785 0.02730 0.05910 0.00483 0.00023 0.00018 0.00016 0.00000 0.00123 0.00136 0.00154 0.00117 0.00112 0.00103 0.00057 O3 0.71236 1.35565 0.54343 1.00000 0.18059 0.05372 0.08996 0.01962 -0.01887 0.03338 0.11808 0.00618 0.00043 0.00020 0.00021 0.00000 0.00302 0.00148 0.00219 0.00138 0.00206 0.00163 0.00115 N1 0.72425 1.16079 0.51793 1.00000 0.05990 0.04178 0.05016 0.01686 0.01056 0.01064 0.05105 0.00567 0.00033 0.00020 0.00019 0.00000 0.00169 0.00142 0.00176 0.00124 0.00140 0.00116 0.00065 N2 0.35060 0.89503 0.04203 1.00000 0.04055 0.05756 0.04957 0.03115 0.01610 0.01332 0.04547 0.00550 0.00028 0.00022 0.00018 0.00000 0.00140 0.00148 0.00163 0.00122 0.00119 0.00110 0.00060 N3 0.60090 0.87514 0.00968 1.00000 0.03961 0.04995 0.04277 0.01729 0.01255 0.00929 0.04341 0.00503 0.00027 0.00018 0.00017 0.00000 0.00137 0.00125 0.00151 0.00106 0.00115 0.00103 0.00056 N4 0.60556 0.67477 0.07730 1.00000 0.05210 0.04575 0.04172 0.01402 0.01262 0.01235 0.04636 0.00503 0.00029 0.00018 0.00017 0.00000 0.00154 0.00127 0.00153 0.00108 0.00124 0.00110 0.00059 C1 0.88927 1.31018 0.67493 1.00000 0.07361 0.05687 0.06104 0.00731 0.01594 0.01024 0.06697 0.00851 0.00052 0.00035 0.00030 0.00000 0.00265 0.00216 0.00267 0.00180 0.00215 0.00186 0.00098 C2 0.76866 1.27962 0.57320 1.00000 0.07069 0.04666 0.06190 0.01896 0.01802 0.00882 0.05990 0.00731 0.00041 0.00026 0.00025 0.00000 0.00230 0.00187 0.00240 0.00164 0.00192 0.00154 0.00087 C3 0.60886 1.10620 0.42483 1.00000 0.05213 0.04211 0.04587 0.01827 0.01870 0.01107 0.04483 0.00656 0.00036 0.00022 0.00022 0.00000 0.00182 0.00157 0.00196 0.00132 0.00158 0.00126 0.00070 C4 0.56238 0.98063 0.39243 1.00000 0.05234 0.04512 0.04369 0.02072 0.01446 0.01632 0.04489 0.00670 0.00036 0.00023 0.00022 0.00000 0.00188 0.00164 0.00195 0.00140 0.00157 0.00133 0.00072 C5 0.44884 0.91983 0.30090 1.00000 0.05478 0.03918 0.05060 0.02011 0.01806 0.00931 0.04651 0.00713 0.00036 0.00026 0.00023 0.00000 0.00192 0.00163 0.00207 0.00139 0.00162 0.00131 0.00073 C6 0.38047 0.98367 0.23960 1.00000 0.04049 0.04827 0.04502 0.02134 0.01557 0.01201 0.04235 0.00622 0.00033 0.00022 0.00021 0.00000 0.00164 0.00158 0.00183 0.00130 0.00140 0.00120 0.00067 C7 0.42480 1.10841 0.27222 1.00000 0.06600 0.04778 0.05879 0.02786 0.01069 0.01862 0.05587 0.00777 0.00043 0.00026 0.00026 0.00000 0.00220 0.00185 0.00238 0.00169 0.00186 0.00154 0.00087 C8 0.53566 1.16835 0.36251 1.00000 0.07248 0.03957 0.06136 0.02013 0.01239 0.01324 0.05799 0.00795 0.00042 0.00027 0.00026 0.00000 0.00233 0.00172 0.00238 0.00155 0.00193 0.00148 0.00088 C9 0.47920 0.83230 0.04375 1.00000 0.03722 0.04216 0.03066 0.01357 0.00588 0.00664 0.03711 0.00562 0.00032 0.00021 0.00019 0.00000 0.00155 0.00141 0.00159 0.00115 0.00125 0.00113 0.00061 C10 0.72475 0.81558 0.00988 1.00000 0.04298 0.05425 0.04977 0.01817 0.01634 0.00825 0.04826 0.00679 0.00038 0.00026 0.00023 0.00000 0.00182 0.00174 0.00206 0.00145 0.00152 0.00140 0.00074 C11 0.72794 0.71877 0.04416 1.00000 0.05170 0.05060 0.04936 0.01477 0.01631 0.01638 0.04974 0.00682 0.00040 0.00025 0.00023 0.00000 0.00199 0.00167 0.00201 0.00140 0.00161 0.00145 0.00075 C12 0.48012 0.73078 0.07565 1.00000 0.04684 0.04825 0.04058 0.01772 0.01202 0.00792 0.04477 0.00654 0.00039 0.00024 0.00021 0.00000 0.00187 0.00163 0.00186 0.00133 0.00149 0.00136 0.00071 H1A 0.77267 1.11502 0.54943 1.00000 0.06442 0.06904 0.00379 0.00255 0.00231 0.00000 0.00975 H1B 0.92380 1.24307 0.69108 1.00000 0.07895 0.07332 0.00401 0.00300 0.00243 0.00000 0.01101 H1C 0.83485 1.34438 0.72998 1.00000 0.12446 0.09411 0.00525 0.00341 0.00327 0.00000 0.01524 H1D 0.97848 1.37701 0.68067 1.00000 0.12689 0.10134 0.00559 0.00386 0.00319 0.00000 0.01591 H2A 0.37050 0.95800 0.02327 1.00000 0.05371 0.06291 0.00346 0.00235 0.00211 0.00000 0.00873 H4 0.60575 0.93562 0.43462 1.00000 0.04688 0.05943 0.00321 0.00212 0.00205 0.00000 0.00745 H5 0.41663 0.83994 0.28143 1.00000 0.04771 0.06122 0.00322 0.00230 0.00198 0.00000 0.00787 H7 0.38046 1.14831 0.23445 1.00000 0.06122 0.06826 0.00372 0.00246 0.00231 0.00000 0.00914 H8 0.55520 1.25296 0.38406 1.00000 0.06914 0.06798 0.00361 0.00261 0.00225 0.00000 0.00943 H10 0.80041 0.84973 -0.01445 1.00000 0.05595 0.06265 0.00357 0.00224 0.00217 0.00000 0.00881 H11 0.82380 0.68265 0.05055 1.00000 0.06220 0.06393 0.00365 0.00235 0.00215 0.00000 0.00881 H12 0.39421 0.69827 0.09284 1.00000 0.05674 0.06389 0.00363 0.00231 0.00218 0.00000 0.00885 S21 0.50845 0.50786 -0.23770 1.00000 0.04011 0.04086 0.04700 0.01551 0.00988 0.00869 0.04273 0.00155 0.00008 0.00005 0.00005 0.00000 0.00042 0.00038 0.00049 0.00031 0.00035 0.00029 0.00022 O21 0.56288 0.62168 -0.25085 1.00000 0.05169 0.04036 0.06105 0.01955 0.01257 0.00286 0.05167 0.00414 0.00023 0.00014 0.00015 0.00000 0.00122 0.00098 0.00142 0.00091 0.00106 0.00083 0.00052 O22 0.62869 0.44614 -0.19839 1.00000 0.04461 0.05759 0.06111 0.02543 0.01322 0.02166 0.05219 0.00439 0.00023 0.00015 0.00015 0.00000 0.00115 0.00110 0.00143 0.00099 0.00104 0.00089 0.00052 O23 0.08025 -0.00078 -0.60246 1.00000 0.10347 0.04341 0.06272 0.01800 0.01499 0.01885 0.07080 0.00501 0.00031 0.00017 0.00017 0.00000 0.00190 0.00117 0.00160 0.00107 0.00141 0.00112 0.00068 N21 0.05063 0.18077 -0.62031 1.00000 0.05678 0.04040 0.04521 0.01168 0.00286 0.01068 0.04984 0.00544 0.00031 0.00020 0.00019 0.00000 0.00163 0.00139 0.00168 0.00118 0.00134 0.00110 0.00065 N22 0.39700 0.52566 -0.15949 1.00000 0.04479 0.04539 0.04429 0.01800 0.01277 0.01610 0.04329 0.00531 0.00029 0.00021 0.00018 0.00000 0.00147 0.00138 0.00157 0.00113 0.00117 0.00108 0.00059 N23 0.16010 0.54641 -0.11254 1.00000 0.04463 0.06092 0.04607 0.01368 0.01217 0.01143 0.05121 0.00533 0.00030 0.00020 0.00018 0.00000 0.00151 0.00144 0.00164 0.00118 0.00128 0.00114 0.00062 N24 0.08141 0.69389 -0.23119 1.00000 0.05959 0.06664 0.06682 0.02161 0.00655 0.02951 0.06445 0.00610 0.00035 0.00022 0.00022 0.00000 0.00184 0.00163 0.00203 0.00141 0.00159 0.00138 0.00075 C21 -0.11222 0.00292 -0.74968 1.00000 0.07027 0.06436 0.05221 -0.00029 0.01504 -0.00294 0.06820 0.00850 0.00057 0.00039 0.00032 0.00000 0.00281 0.00247 0.00262 0.00189 0.00208 0.00188 0.00104 C22 0.01526 0.05870 -0.65155 1.00000 0.05597 0.04701 0.04655 0.00939 0.01801 0.00810 0.05055 0.00677 0.00038 0.00024 0.00023 0.00000 0.00196 0.00177 0.00202 0.00145 0.00160 0.00138 0.00075 C23 0.16113 0.25653 -0.52905 1.00000 0.04664 0.03994 0.04423 0.01178 0.01050 0.01397 0.04377 0.00621 0.00034 0.00022 0.00021 0.00000 0.00172 0.00146 0.00189 0.00131 0.00147 0.00122 0.00069 C24 0.23815 0.37097 -0.52446 1.00000 0.07901 0.04640 0.04270 0.02109 0.00577 0.00962 0.05713 0.00733 0.00043 0.00025 0.00025 0.00000 0.00233 0.00171 0.00205 0.00149 0.00179 0.00150 0.00085 C25 0.34338 0.44819 -0.43575 1.00000 0.07016 0.03858 0.05342 0.02083 0.00969 0.00402 0.05504 0.00727 0.00041 0.00026 0.00024 0.00000 0.00218 0.00164 0.00222 0.00149 0.00174 0.00142 0.00084 C26 0.37238 0.41248 -0.35133 1.00000 0.04155 0.03535 0.04396 0.01380 0.01326 0.00893 0.03971 0.00590 0.00032 0.00021 0.00020 0.00000 0.00160 0.00137 0.00180 0.00119 0.00137 0.00110 0.00065 C27 0.29503 0.29865 -0.35554 1.00000 0.05425 0.04343 0.04140 0.02046 0.01010 0.00880 0.04575 0.00670 0.00037 0.00023 0.00023 0.00000 0.00188 0.00157 0.00194 0.00140 0.00155 0.00129 0.00072 C28 0.18815 0.22146 -0.44349 1.00000 0.05679 0.03554 0.04971 0.01593 0.01203 0.00516 0.04790 0.00683 0.00038 0.00025 0.00023 0.00000 0.00191 0.00152 0.00205 0.00135 0.00157 0.00127 0.00075 C29 0.25688 0.57510 -0.16757 1.00000 0.03978 0.03904 0.03746 0.00398 0.00320 0.00618 0.04194 0.00577 0.00034 0.00021 0.00021 0.00000 0.00165 0.00141 0.00175 0.00119 0.00135 0.00116 0.00067 C210 0.02640 0.59446 -0.11747 1.00000 0.04649 0.08481 0.06278 0.01648 0.01900 0.01839 0.06481 0.00809 0.00045 0.00034 0.00029 0.00000 0.00216 0.00249 0.00264 0.00197 0.00193 0.00183 0.00096 C211 -0.01449 0.66461 -0.17575 1.00000 0.05383 0.08147 0.06848 0.01124 0.01342 0.02913 0.06935 0.00807 0.00048 0.00033 0.00030 0.00000 0.00234 0.00244 0.00273 0.00198 0.00203 0.00195 0.00102 C212 0.21727 0.64823 -0.22641 1.00000 0.05361 0.05991 0.05880 0.02319 0.01099 0.02029 0.05650 0.00743 0.00042 0.00027 0.00026 0.00000 0.00211 0.00193 0.00235 0.00165 0.00179 0.00155 0.00084 H21A 0.00941 0.21436 -0.66616 1.00000 0.06327 0.06885 0.00374 0.00253 0.00235 0.00000 0.00964 H21B -0.12841 -0.07151 -0.76695 1.00000 0.11408 0.09668 0.00514 0.00362 0.00321 0.00000 0.01664 H21C -0.09305 0.02800 -0.80144 1.00000 0.13543 0.10359 0.00578 0.00384 0.00367 0.00000 0.01946 H21D -0.21809 0.01943 -0.74862 1.00000 0.15139 0.11101 0.00672 0.00397 0.00381 0.00000 0.02115 H22A 0.39178 0.46945 -0.13611 1.00000 0.06761 0.07106 0.00391 0.00258 0.00245 0.00000 0.01068 H24 0.21534 0.39141 -0.58747 1.00000 0.06122 0.06605 0.00353 0.00231 0.00232 0.00000 0.00859 H25 0.38998 0.52511 -0.43372 1.00000 0.07446 0.07093 0.00379 0.00266 0.00234 0.00000 0.00985 H27 0.30992 0.27516 -0.29743 1.00000 0.05552 0.06211 0.00334 0.00220 0.00216 0.00000 0.00829 H28 0.13578 0.14647 -0.44273 1.00000 0.06357 0.06416 0.00347 0.00244 0.00209 0.00000 0.00885 H210 -0.03486 0.57113 -0.08541 1.00000 0.08848 0.08509 0.00468 0.00300 0.00290 0.00000 0.01363 H211 -0.09970 0.70101 -0.17714 1.00000 0.07816 0.07452 0.00434 0.00271 0.00250 0.00000 0.01087 H212 0.27537 0.66905 -0.26804 1.00000 0.08099 0.07479 0.00418 0.00271 0.00260 0.00000 0.01170 Final Structure Factor Calculation for s92 in P-1 Total number of l.s. parameters = 457 Maximum vector length = 511 Memory required = 3591 / 24017 wR2 = 0.1256 before cycle 5 for 4612 data and 0 / 457 parameters GooF = S = 0.970; Restrained GooF = 0.970 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0631 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0471 for 2969 Fo > 4sig(Fo) and 0.0862 for all 4612 data wR2 = 0.1256, GooF = S = 0.970, Restrained GooF = 0.970 for all data Occupancy sum of asymmetric unit = 40.00 for non-hydrogen and 24.00 for hydrogen atoms Principal mean square atomic displacements U 0.0658 0.0401 0.0346 S1 0.0779 0.0553 0.0330 O1 0.0927 0.0514 0.0332 O2 0.2330 0.0750 0.0463 O3 may be split into 0.7273 1.3513 0.5350 and 0.6974 1.3600 0.5518 0.0645 0.0494 0.0392 N1 0.0658 0.0394 0.0312 N2 0.0509 0.0406 0.0387 N3 0.0529 0.0450 0.0412 N4 0.0760 0.0742 0.0507 C1 0.0732 0.0619 0.0446 C2 0.0536 0.0453 0.0357 C3 0.0544 0.0470 0.0333 C4 0.0558 0.0509 0.0329 C5 0.0524 0.0394 0.0352 C6 0.0735 0.0619 0.0322 C7 0.0786 0.0598 0.0356 C8 0.0448 0.0383 0.0282 C9 0.0558 0.0495 0.0394 C10 0.0555 0.0497 0.0440 C11 0.0523 0.0455 0.0365 C12 0.0493 0.0401 0.0387 S21 0.0655 0.0543 0.0352 O21 0.0653 0.0570 0.0342 O22 0.1093 0.0625 0.0406 O23 0.0690 0.0406 0.0399 N21 0.0502 0.0445 0.0352 N22 0.0626 0.0467 0.0443 N23 0.0872 0.0678 0.0383 N24 0.0955 0.0663 0.0429 C21 0.0603 0.0491 0.0423 C22 0.0516 0.0433 0.0365 C23 0.0888 0.0497 0.0328 C24 0.0803 0.0523 0.0325 C25 0.0441 0.0409 0.0341 C26 0.0588 0.0471 0.0314 C27 0.0615 0.0492 0.0330 C28 0.0527 0.0427 0.0305 C29 0.0890 0.0626 0.0428 C210 0.0998 0.0646 0.0437 C211 0.0643 0.0634 0.0418 C212 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.014 0.021 0.029 0.039 0.050 0.065 0.087 0.129 1.000 Number in group 476. 479. 445. 459. 472. 480. 433. 451. 455. 462. GooF 0.758 0.858 0.873 0.946 1.024 1.056 1.093 0.989 0.999 1.059 K 3.013 0.971 1.003 0.949 1.008 0.983 0.990 1.002 1.021 1.003 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.15 1.26 1.44 1.82 inf Number in group 465. 469. 455. 469. 446. 473. 449. 465. 458. 463. GooF 0.867 0.864 0.871 0.889 0.929 0.936 0.951 0.969 1.075 1.273 K 1.035 1.047 1.020 1.005 1.016 1.013 1.036 1.027 1.047 0.980 R1 0.278 0.230 0.161 0.120 0.101 0.072 0.058 0.053 0.045 0.037 Recommended weighting scheme: WGHT 0.0630 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 4 0 116.06 86.48 4.51 0.054 2.83 2 2 2 39.89 25.13 4.36 0.029 2.39 -8 -4 11 26.60 61.79 4.04 0.046 0.87 -1 0 3 107.00 77.69 4.00 0.051 4.49 -3 -4 2 608.40 475.17 3.97 0.127 1.87 -4 -9 5 82.83 115.24 3.77 0.062 1.04 -7 -2 7 67.78 110.65 3.60 0.061 1.10 -1 -3 8 6.87 21.84 3.41 0.027 1.77 -8 0 9 52.12 77.13 3.33 0.051 0.97 -6 4 10 42.51 71.68 3.32 0.049 1.02 -2 -9 7 134.72 107.22 3.26 0.060 1.16 0 1 0 25.82 89.99 3.23 0.055 11.12 -2 -6 2 44.70 59.67 3.22 0.045 1.65 -9 3 7 17.77 58.99 3.21 0.045 0.90 -8 1 3 25.63 57.51 3.18 0.044 1.05 -7 7 5 31.94 55.03 3.17 0.043 0.99 1 -1 3 92.80 118.75 3.14 0.063 3.71 0 0 4 -2.90 5.41 3.10 0.014 3.35 0 -4 7 51.04 34.77 3.10 0.034 1.86 0 2 5 1085.86 884.28 3.09 0.173 2.17 -2 4 4 26.41 41.97 3.06 0.038 1.95 -3 -3 2 309.39 244.50 3.04 0.091 2.11 1 -5 2 46.57 36.93 3.01 0.035 2.32 5 -1 11 136.07 53.90 3.00 0.043 0.88 4 0 0 41.92 89.91 2.99 0.055 2.00 0 -1 2 1044.02 1272.92 2.98 0.207 6.71 -7 1 11 36.60 58.79 2.97 0.045 0.98 0 0 14 18.00 50.52 2.96 0.041 0.96 -7 2 2 -4.06 16.43 2.94 0.024 1.20 3 4 7 -3.03 14.78 2.94 0.022 1.10 5 -2 1 48.79 69.98 2.93 0.049 1.59 -3 3 2 139.82 170.10 2.91 0.076 2.34 -1 -7 3 909.70 708.94 2.90 0.155 1.59 0 -10 7 167.45 221.55 2.90 0.086 1.12 5 2 7 33.41 3.77 2.89 0.011 1.01 -2 -10 3 29.47 68.52 2.89 0.048 1.07 5 -6 1 267.11 212.06 2.89 0.085 1.36 4 -5 1 27.67 38.77 2.89 0.036 1.67 -4 1 7 57.41 38.03 2.87 0.036 1.60 0 1 4 785.87 653.58 2.87 0.149 2.97 0 -1 5 783.89 948.58 2.84 0.179 2.81 2 1 0 358.14 299.48 2.82 0.101 3.53 -5 2 0 -1.97 3.14 2.82 0.010 1.64 9 -7 1 4.71 21.94 2.79 0.027 0.85 0 11 5 37.58 62.50 2.79 0.046 0.86 -5 0 8 8.13 24.67 2.78 0.029 1.37 -2 -4 2 21.33 13.69 2.78 0.022 2.24 0 2 15 58.64 97.82 2.76 0.057 0.84 -2 -3 1 36.60 45.01 2.74 0.039 2.60 -3 -1 7 475.04 395.65 2.74 0.116 1.84 Bond lengths and angles S1 - Distance Angles O2 1.4257 (0.0019) O1 1.4287 (0.0018) 120.22 (0.12) N2 1.6481 (0.0024) 103.87 (0.12) 108.08 (0.12) C6 1.7531 (0.0030) 109.06 (0.13) 108.54 (0.13) 106.18 (0.13) S1 - O2 O1 N2 O1 - Distance Angles S1 1.4287 (0.0018) O1 - O2 - Distance Angles S1 1.4257 (0.0019) O2 - O3 - Distance Angles C2 1.2014 (0.0035) O3 - N1 - Distance Angles C2 1.3696 (0.0037) C3 1.3901 (0.0037) 128.74 (0.26) N1 - C2 N2 - Distance Angles C9 1.4012 (0.0032) S1 1.6481 (0.0024) 124.98 (0.19) N2 - C9 N3 - Distance Angles C9 1.3311 (0.0032) C10 1.3437 (0.0035) 115.90 (0.23) N3 - C9 N4 - Distance Angles C12 1.3280 (0.0034) C11 1.3320 (0.0035) 116.60 (0.25) N4 - C12 C1 - Distance Angles C2 1.4996 (0.0048) C1 - C2 - Distance Angles O3 1.2014 (0.0035) N1 1.3696 (0.0036) 122.40 (0.32) C1 1.4996 (0.0048) 121.25 (0.30) 116.33 (0.29) C2 - O3 N1 C3 - Distance Angles N1 1.3901 (0.0037) C8 1.3938 (0.0039) 124.35 (0.25) C4 1.3980 (0.0036) 117.51 (0.25) 118.13 (0.29) C3 - N1 C8 C4 - Distance Angles C5 1.3789 (0.0040) C3 1.3980 (0.0036) 120.98 (0.27) C4 - C5 C5 - Distance Angles C4 1.3789 (0.0040) C6 1.3845 (0.0036) 119.71 (0.26) C5 - C4 C6 - Distance Angles C5 1.3845 (0.0036) C7 1.3882 (0.0039) 119.37 (0.28) S1 1.7531 (0.0030) 120.90 (0.21) 119.73 (0.22) C6 - C5 C7 C7 - Distance Angles C8 1.3564 (0.0045) C6 1.3882 (0.0039) 120.97 (0.29) C7 - C8 C8 - Distance Angles C7 1.3564 (0.0045) C3 1.3938 (0.0039) 120.82 (0.28) C8 - C7 C9 - Distance Angles N3 1.3311 (0.0032) C12 1.3900 (0.0035) 121.51 (0.25) N2 1.4012 (0.0032) 114.96 (0.22) 123.50 (0.25) C9 - N3 C12 C10 - Distance Angles N3 1.3437 (0.0035) C11 1.3581 (0.0040) 122.41 (0.29) C10 - N3 C11 - Distance Angles N4 1.3320 (0.0035) C10 1.3581 (0.0040) 121.90 (0.29) C11 - N4 C12 - Distance Angles N4 1.3280 (0.0034) C9 1.3900 (0.0035) 121.62 (0.28) C12 - N4 S21 - Distance Angles O21 1.4286 (0.0017) O22 1.4292 (0.0019) 119.89 (0.12) N22 1.6303 (0.0024) 108.51 (0.12) 103.98 (0.12) C26 1.7529 (0.0029) 108.25 (0.13) 109.41 (0.12) 105.92 (0.12) S21 - O21 O22 N22 O21 - Distance Angles S21 1.4286 (0.0017) O21 - O22 - Distance Angles S21 1.4292 (0.0019) O22 - O23 - Distance Angles C22 1.2178 (0.0033) O23 - N21 - Distance Angles C22 1.3579 (0.0034) C23 1.4083 (0.0036) 126.71 (0.26) N21 - C22 N22 - Distance Angles C29 1.3888 (0.0033) S21 1.6303 (0.0024) 126.67 (0.21) N22 - C29 N23 - Distance Angles C210 1.3320 (0.0039) C29 1.3358 (0.0035) 115.47 (0.29) N23 - C210 N24 - Distance Angles C212 1.3330 (0.0038) C211 1.3376 (0.0044) 116.06 (0.31) N24 - C212 C21 - Distance Angles C22 1.4837 (0.0049) C21 - C22 - Distance Angles O23 1.2178 (0.0033) N21 1.3579 (0.0034) 122.97 (0.29) C21 1.4837 (0.0049) 122.39 (0.30) 114.63 (0.31) C22 - O23 N21 C23 - Distance Angles C28 1.3840 (0.0039) C24 1.3875 (0.0037) 119.61 (0.28) N21 1.4083 (0.0036) 121.55 (0.25) 118.77 (0.27) C23 - C28 C24 C24 - Distance Angles C25 1.3759 (0.0043) C23 1.3875 (0.0037) 120.13 (0.30) C24 - C25 C25 - Distance Angles C26 1.3730 (0.0038) C24 1.3759 (0.0043) 120.18 (0.27) C25 - C26 C26 - Distance Angles C25 1.3730 (0.0038) C27 1.3837 (0.0034) 119.83 (0.27) S21 1.7529 (0.0029) 121.26 (0.20) 118.91 (0.22) C26 - C25 C27 C27 - Distance Angles C28 1.3738 (0.0040) C26 1.3837 (0.0034) 120.41 (0.28) C27 - C28 C28 - Distance Angles C27 1.3738 (0.0040) C23 1.3840 (0.0039) 119.81 (0.27) C28 - C27 C29 - Distance Angles N23 1.3358 (0.0035) C212 1.3816 (0.0040) 121.42 (0.28) N22 1.3888 (0.0033) 114.22 (0.25) 124.36 (0.29) C29 - N23 C212 C210 - Distance Angles N23 1.3320 (0.0039) C211 1.3493 (0.0051) 123.50 (0.38) C210 - N23 C211 - Distance Angles N24 1.3376 (0.0044) C210 1.3493 (0.0051) 121.52 (0.35) C211 - N24 C212 - Distance Angles N24 1.3330 (0.0038) C29 1.3816 (0.0040) 122.00 (0.34) C212 - N24 FMAP and GRID set by program FMAP 2 1 21 GRID -2.778 -2 -2 2.778 2 2 R1 = 0.0858 for 4612 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.28 at 0.1928 0.6644 0.5014 [ 1.16 A from O3 ] Deepest hole -0.33 at 0.1501 0.9050 0.1362 [ 0.82 A from S1 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 3474 / 23949 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.8072 1.3356 0.4986 1.00000 0.05 0.28 1.16 O3 1.48 C2 2.19 N1 2.26 H8 Q2 1 0.0205 0.6818 0.0011 1.00000 0.05 0.21 1.48 H210 1.78 C210 1.89 O1 1.96 H11 Q3 1 0.1735 0.7659 0.1382 1.00000 0.05 0.19 0.44 O1 1.79 S1 2.30 H12 2.41 H5 Q4 1 0.5794 1.0590 0.4179 1.00000 0.05 0.19 0.55 C3 0.88 C4 1.57 H4 1.70 N1 Q5 1 0.5817 0.6879 -0.0998 1.00000 0.05 0.18 1.89 C10 2.07 C11 2.09 O21 2.12 N22 Q6 1 0.6356 1.2756 0.3804 1.00000 0.05 0.18 0.71 H8 1.34 C8 2.15 H212 2.20 O3 Q7 1 -0.2520 0.0742 -0.6530 1.00000 0.05 0.18 1.48 H21D 1.83 C3 2.11 C4 2.13 C21 Q8 1 -0.2454 0.6170 -0.1839 1.00000 0.05 0.17 1.43 H211 1.70 O21 1.92 C211 2.07 O22 Q9 1 0.2110 0.8096 -0.0569 1.00000 0.05 0.17 1.60 N2 1.94 H2A 2.32 C9 2.35 C211 Q10 1 0.8640 1.4235 0.6546 1.00000 0.05 0.17 1.21 H1D 1.47 C1 1.65 H1C 1.71 O3 Q11 1 0.3121 0.3861 -0.3428 1.00000 0.05 0.17 0.61 C26 0.98 C27 1.61 H27 1.74 C25 Q12 1 0.3139 1.1210 0.3594 1.00000 0.05 0.17 1.73 C7 1.86 C8 2.10 H7 2.27 H8 Q13 1 0.1147 0.7917 0.0044 1.00000 0.05 0.17 1.64 O1 1.85 S1 2.05 N2 2.30 O2 Q14 1 0.4081 0.5011 -0.1346 1.00000 0.05 0.16 0.37 H22A 0.52 N22 1.70 C29 1.90 S21 Q15 1 0.1115 1.0024 0.0813 1.00000 0.05 0.16 0.34 O2 1.76 S1 2.31 H10 2.60 H2A Q16 1 -0.0283 0.2843 -0.5377 1.00000 0.05 0.16 1.66 C23 1.80 N21 1.95 H21A 2.27 C24 Q17 1 1.0047 1.4596 0.5557 1.00000 0.05 0.16 2.30 H1D 2.53 O3 2.72 C24 2.78 H24 Q18 1 -0.1730 0.0612 -0.7831 1.00000 0.05 0.16 0.89 H21C 0.89 H21D 1.06 C21 1.72 H21B Q19 1 0.6002 0.8162 -0.0189 1.00000 0.05 0.16 0.71 N3 1.04 C10 1.52 C9 1.66 H10 Q20 1 -0.2466 -0.0746 -0.7613 1.00000 0.05 0.16 1.02 H21B 1.06 H21D 1.30 C21 1.93 H21C Shortest distances between peaks (including symmetry equivalents) 9 13 1.37 2 13 1.40 5 19 1.62 1 16 1.73 18 20 1.76 1 6 1.85 1 17 1.90 4 7 1.96 3 13 2.00 2 3 2.00 7 20 2.05 17 17 2.07 16 17 2.10 7 18 2.12 1 10 2.13 10 17 2.15 5 8 2.24 5 14 2.32 13 15 2.46 2 9 2.48 4 12 2.49 15 15 2.63 6 7 2.66 7 16 2.74 4 6 2.74 6 16 2.78 11 14 2.83 2 8 2.90 6 12 2.95 9 15 2.99 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. 0.83: 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 10.02: Structure factors and derivatives 57.68: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 6.66: Solve l.s. equations 0.00: Generate HTAB table 0.19: Other dependent quantities, CIF, tables 0.66: Analysis of variance 0.11: Merge reflections for Fourier and .fcf 0.33: Fourier summations 0.17: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + S92 finished at 11:53:51 Total elapsed time: 76.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++