+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0079 started at 13:17:59 on 05-Mar-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0079 in P2(1)/n CELL 0.71073 15.8005 5.1763 16.9786 90.000 99.723 90.000 ZERR 4.00 0.0006 0.0001 0.0006 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O S UNIT 52 52 4 20 4 V = 1368.70 F(000) = 616.0 Mu = 0.25 mm-1 Cell Wt = 1181.22 Rho = 1.433 MERG 2 OMIT -3.00 55.00 size 0.41 0.06 0.02 SHEL 7 0.77 FMAP 2 PLAN 5 ACTA BOND $H WGHT 0.005000 2.70740 L.S. 15 TEMP -153.00 FVAR 0.52556 C1 1 0.971359 -0.093246 0.255979 11.00000 0.01957 0.01914 = 0.02317 -0.00146 0.00255 0.00134 C2 1 0.982421 -0.028732 0.176485 11.00000 0.01860 0.01880 = 0.02196 -0.00147 0.00168 -0.00052 C3 1 1.042839 -0.138701 0.139836 11.00000 0.01985 0.02040 = 0.02103 0.00207 0.00206 -0.00119 AFIX 43 H3 2 1.048007 -0.087500 0.087126 11.00000 -1.20000 AFIX 0 C4 1 1.165629 -0.386777 0.138649 11.00000 0.02099 0.02221 = 0.02195 -0.00272 0.00559 0.00470 AFIX 23 H4A 2 1.145875 -0.402285 0.080324 11.00000 -1.20000 H4B 2 1.188807 -0.556305 0.158925 11.00000 -1.20000 AFIX 0 C5 1 1.235122 -0.184675 0.154904 11.00000 0.02321 0.01862 = 0.01814 0.00184 0.00205 0.00485 C6 1 1.377401 -0.087550 0.134291 11.00000 0.02250 0.03317 = 0.03271 -0.00510 0.00449 -0.00777 AFIX 23 H6A 2 1.413904 -0.105560 0.187449 11.00000 -1.20000 H6B 2 1.357217 0.093485 0.127813 11.00000 -1.20000 AFIX 0 C7 1 1.427547 -0.157385 0.069556 11.00000 0.02582 0.03694 = 0.03203 0.00139 0.00547 -0.00156 AFIX 137 H7A 2 1.446122 -0.337916 0.075941 11.00000 -1.50000 H7B 2 1.478002 -0.045079 0.073298 11.00000 -1.50000 H7C 2 1.391204 -0.134677 0.017236 11.00000 -1.50000 AFIX 0 C8 1 0.813751 0.011813 0.104676 11.00000 0.02095 0.01914 = 0.01931 0.00095 0.00072 0.00156 C9 1 0.752764 0.038574 0.154390 11.00000 0.02509 0.02439 = 0.01715 -0.00126 0.00203 0.00215 AFIX 43 H9 2 0.759951 0.164388 0.195718 11.00000 -1.20000 AFIX 0 C10 1 0.681392 -0.121096 0.142690 11.00000 0.02293 0.03305 = 0.02297 0.00265 0.00685 0.00212 AFIX 43 H10 2 0.639325 -0.105840 0.176331 11.00000 -1.20000 AFIX 0 C11 1 0.671276 -0.303348 0.081867 11.00000 0.02175 0.02534 = 0.02703 0.00073 0.00042 -0.00313 AFIX 43 H11 2 0.622807 -0.414771 0.074740 11.00000 -1.20000 AFIX 0 C12 1 0.731597 -0.323996 0.031284 11.00000 0.02525 0.02585 = 0.02608 -0.00528 0.00314 0.00010 AFIX 43 H12 2 0.723427 -0.446108 -0.011093 11.00000 -1.20000 AFIX 0 C13 1 0.803626 -0.166679 0.042601 11.00000 0.02121 0.02467 = 0.02260 -0.00214 0.00551 0.00104 AFIX 43 H13 2 0.845334 -0.180574 0.008545 11.00000 -1.20000 AFIX 0 N1 3 0.962030 -0.141420 0.319643 11.00000 0.03400 0.03033 = 0.02472 0.00069 0.00766 0.00399 O1 4 1.094967 -0.317510 0.176865 11.00000 0.02234 0.02465 = 0.02263 0.00288 0.00626 0.00331 O2 4 1.226681 0.021517 0.186107 11.00000 0.02984 0.02221 = 0.03169 -0.00456 0.00595 0.00054 O3 4 1.304031 -0.264189 0.127319 11.00000 0.02271 0.02682 = 0.03037 -0.00503 0.00734 -0.00151 O4 4 0.898110 0.399470 0.177660 11.00000 0.02979 0.01742 = 0.02725 -0.00394 0.00518 0.00092 O5 4 0.938649 0.246545 0.049945 11.00000 0.02828 0.02820 = 0.02152 0.00461 0.00688 -0.00034 S1 5 0.909271 0.192041 0.124229 11.00000 0.02177 0.01746 = 0.01898 0.00100 0.00395 0.00036 HKLF 4 Covalent radii and connectivity table for 2007src0079 in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 C1 - N1 C2 C2 - C3 C1 S1 C3 - O1 C2 C4 - O1 C5 C5 - O2 O3 C4 C6 - O3 C7 C7 - C6 C8 - C13 C9 S1 C9 - C10 C8 C10 - C9 C11 C11 - C10 C12 C12 - C13 C11 C13 - C12 C8 N1 - C1 O1 - C3 C4 O2 - C5 O3 - C5 C6 O4 - S1 O5 - S1 S1 - O4 O5 C2 C8 h k l Fo^2 Sigma Why rejected 0 0 13 41.13 9.31 observed but should be systematically absent 14519 Reflections read, of which 867 rejected -20 =< h =< 20, -6 =< k =< 6, -22 =< l =< 22, Max. 2-theta = 54.96 1 Systematic absence violations 0 Inconsistent equivalents 3138 Unique reflections, of which 0 suppressed R(int) = 0.0522 R(sigma) = 0.0480 Friedel opposites merged Maximum memory for data reduction = 1771 / 31435 Default effective X-H distances for T = -153.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 2271 / 227038 wR2 = 0.1169 before cycle 1 for 3138 data and 182 / 182 parameters GooF = S = 1.095; Restrained GooF = 1.095 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 2.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52623 0.00100 0.674 OSF Mean shift/esd = 0.115 Maximum = 0.674 for OSF Max. shift = 0.002 A for H7A Max. dU = 0.000 for C2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2271 / 227038 wR2 = 0.1168 before cycle 2 for 3138 data and 182 / 182 parameters GooF = S = 1.095; Restrained GooF = 1.095 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 2.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52637 0.00100 0.138 OSF Mean shift/esd = 0.041 Maximum = 0.217 for U33 S1 Max. shift = 0.001 A for H7A Max. dU = 0.000 for C2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2271 / 227038 wR2 = 0.1168 before cycle 3 for 3138 data and 182 / 182 parameters GooF = S = 1.095; Restrained GooF = 1.095 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 2.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52638 0.00100 0.011 OSF Mean shift/esd = 0.002 Maximum = 0.014 for U33 S1 Max. shift = 0.000 A for H7B Max. dU = 0.000 for C3 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2271 / 227038 wR2 = 0.1168 before cycle 4 for 3138 data and 182 / 182 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 2.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52638 0.00100 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.003 for U12 C7 Max. shift = 0.000 A for H7B Max. dU = 0.000 for N1 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2271 / 227038 wR2 = 0.1168 before cycle 5 for 3138 data and 182 / 182 parameters GooF = S = 1.095; Restrained GooF = 1.095 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 2.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52639 0.00100 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H7A Max. dU = 0.000 for C3 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2271 / 227038 wR2 = 0.1168 before cycle 6 for 3138 data and 182 / 182 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 2.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52639 0.00100 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for O2 Max. dU = 0.000 for C6 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2271 / 227038 wR2 = 0.1168 before cycle 7 for 3138 data and 182 / 182 parameters GooF = S = 1.095; Restrained GooF = 1.095 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 2.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52638 0.00100 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H7C Max. dU = 0.000 for C7 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2271 / 227038 wR2 = 0.1168 before cycle 8 for 3138 data and 182 / 182 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 2.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52638 0.00100 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H7C Max. dU = 0.000 for O4 Least-squares cycle 9 Maximum vector length = 511 Memory required = 2271 / 227038 wR2 = 0.1168 before cycle 9 for 3138 data and 182 / 182 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 2.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52639 0.00100 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H7C Max. dU = 0.000 for O3 Least-squares cycle 10 Maximum vector length = 511 Memory required = 2271 / 227038 wR2 = 0.1168 before cycle 10 for 3138 data and 182 / 182 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 2.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52638 0.00100 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H7B Max. dU = 0.000 for O2 Least-squares cycle 11 Maximum vector length = 511 Memory required = 2271 / 227038 wR2 = 0.1168 before cycle 11 for 3138 data and 182 / 182 parameters GooF = S = 1.095; Restrained GooF = 1.095 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 2.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52638 0.00100 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H7C Max. dU = 0.000 for C1 Least-squares cycle 12 Maximum vector length = 511 Memory required = 2271 / 227038 wR2 = 0.1168 before cycle 12 for 3138 data and 182 / 182 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 2.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52639 0.00100 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H7C Max. dU = 0.000 for O5 Least-squares cycle 13 Maximum vector length = 511 Memory required = 2271 / 227038 wR2 = 0.1168 before cycle 13 for 3138 data and 182 / 182 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 2.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52639 0.00100 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H7C Max. dU = 0.000 for C3 Least-squares cycle 14 Maximum vector length = 511 Memory required = 2271 / 227038 wR2 = 0.1168 before cycle 14 for 3138 data and 182 / 182 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 2.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52638 0.00100 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H7C Max. dU = 0.000 for N1 Least-squares cycle 15 Maximum vector length = 511 Memory required = 2271 / 227038 wR2 = 0.1168 before cycle 15 for 3138 data and 182 / 182 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 2.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52638 0.00100 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H7B Max. dU = 0.000 for C3 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 16 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 1.0479 -0.0871 0.0872 43 0.950 0.000 C3 O1 C2 H4A 1.1459 -0.4022 0.0803 23 0.990 0.000 C4 O1 C5 H4B 1.1888 -0.5562 0.1589 23 0.990 0.000 C4 O1 C5 H6A 1.4139 -0.1056 0.1875 23 0.990 0.000 C6 O3 C7 H6B 1.3572 0.0936 0.1279 23 0.990 0.000 C6 O3 C7 H7A 1.4459 -0.3381 0.0758 137 0.980 0.000 C7 C6 H7A H7B 1.4781 -0.0455 0.0734 137 0.980 0.000 C7 C6 H7A H7C 1.3912 -0.1341 0.0173 137 0.980 0.000 C7 C6 H7A H9 0.7600 0.1642 0.1957 43 0.950 0.000 C9 C10 C8 H10 0.6393 -0.1057 0.1762 43 0.950 0.000 C10 C9 C11 H11 0.6229 -0.4146 0.0747 43 0.950 0.000 C11 C10 C12 H12 0.7234 -0.4458 -0.0111 43 0.950 0.000 C12 C13 C11 H13 0.8453 -0.1808 0.0086 43 0.950 0.000 C13 C12 C8 2007src0079 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.97137 -0.09324 0.25600 1.00000 0.01934 0.01903 0.02337 -0.00168 0.00245 0.00145 0.02071 0.00455 0.00016 0.00047 0.00015 0.00000 0.00127 0.00118 0.00125 0.00098 0.00099 0.00097 0.00051 C2 0.98241 -0.02879 0.17646 1.00000 0.01858 0.01865 0.02144 -0.00141 0.00140 -0.00047 0.01979 0.00440 0.00016 0.00047 0.00014 0.00000 0.00124 0.00118 0.00119 0.00094 0.00098 0.00095 0.00050 C3 1.04277 -0.13850 0.13991 1.00000 0.02004 0.02057 0.02092 0.00214 0.00173 -0.00123 0.02071 0.00448 0.00016 0.00047 0.00015 0.00000 0.00127 0.00122 0.00115 0.00095 0.00096 0.00096 0.00051 H3 1.04794 -0.08711 0.08721 1.00000 0.02485 0.00000 0.00000 C4 1.16564 -0.38670 0.13866 1.00000 0.02099 0.02238 0.02182 -0.00265 0.00541 0.00469 0.02152 0.00468 0.00016 0.00049 0.00015 0.00000 0.00131 0.00123 0.00118 0.00098 0.00100 0.00100 0.00052 H4A 1.14588 -0.40224 0.08033 1.00000 0.02583 0.00000 0.00000 H4B 1.18883 -0.55621 0.15894 1.00000 0.02583 0.00000 0.00000 C5 1.23510 -0.18462 0.15489 1.00000 0.02332 0.01885 0.01782 0.00197 0.00186 0.00468 0.02018 0.00458 0.00016 0.00048 0.00014 0.00000 0.00130 0.00117 0.00111 0.00095 0.00095 0.00098 0.00050 C6 1.37741 -0.08747 0.13434 1.00000 0.02244 0.03314 0.03281 -0.00488 0.00420 -0.00772 0.02952 0.00494 0.00018 0.00057 0.00017 0.00000 0.00142 0.00149 0.00145 0.00120 0.00115 0.00116 0.00061 H6A 1.41392 -0.10558 0.18749 1.00000 0.03542 0.00000 0.00000 H6B 1.35724 0.09358 0.12788 1.00000 0.03542 0.00000 0.00000 C7 1.42751 -0.15736 0.06956 1.00000 0.02588 0.03696 0.03241 0.00172 0.00567 -0.00169 0.03166 0.00535 0.00018 0.00058 0.00017 0.00000 0.00149 0.00162 0.00145 0.00124 0.00118 0.00122 0.00063 H7A 1.44591 -0.33808 0.07583 1.00000 0.04750 0.00000 0.00000 H7B 1.47808 -0.04548 0.07339 1.00000 0.04750 0.00000 0.00000 H7C 1.39120 -0.13407 0.01725 1.00000 0.04750 0.00000 0.00000 C8 0.81373 0.01188 0.10469 1.00000 0.02070 0.01891 0.01957 0.00091 0.00062 0.00164 0.02005 0.00453 0.00016 0.00047 0.00014 0.00000 0.00126 0.00117 0.00114 0.00093 0.00096 0.00096 0.00050 C9 0.75279 0.03850 0.15434 1.00000 0.02512 0.02433 0.01695 -0.00135 0.00185 0.00247 0.02233 0.00469 0.00017 0.00050 0.00014 0.00000 0.00137 0.00128 0.00113 0.00097 0.00100 0.00103 0.00053 H9 0.75999 0.16423 0.19570 1.00000 0.02680 0.00000 0.00000 C10 0.68139 -0.12100 0.14263 1.00000 0.02249 0.03320 0.02296 0.00320 0.00685 0.00239 0.02587 0.00502 0.00017 0.00054 0.00015 0.00000 0.00137 0.00146 0.00125 0.00107 0.00105 0.00109 0.00057 H10 0.63930 -0.10568 0.17624 1.00000 0.03104 0.00000 0.00000 C11 0.67132 -0.30315 0.08182 1.00000 0.02157 0.02538 0.02730 0.00083 0.00040 -0.00319 0.02519 0.00482 0.00017 0.00052 0.00015 0.00000 0.00131 0.00131 0.00128 0.00109 0.00103 0.00109 0.00055 H11 0.62286 -0.41462 0.07468 1.00000 0.03022 0.00000 0.00000 C12 0.73159 -0.32373 0.03130 1.00000 0.02546 0.02599 0.02595 -0.00534 0.00304 0.00005 0.02595 0.00488 0.00017 0.00052 0.00015 0.00000 0.00138 0.00135 0.00126 0.00108 0.00106 0.00110 0.00056 H12 0.72339 -0.44576 -0.01109 1.00000 0.03114 0.00000 0.00000 C13 0.80360 -0.16672 0.04261 1.00000 0.02127 0.02472 0.02243 -0.00182 0.00539 0.00121 0.02261 0.00467 0.00016 0.00049 0.00015 0.00000 0.00130 0.00131 0.00118 0.00102 0.00099 0.00103 0.00053 H13 0.84532 -0.18077 0.00857 1.00000 0.02713 0.00000 0.00000 N1 0.96202 -0.14146 0.31965 1.00000 0.03434 0.03020 0.02477 0.00047 0.00767 0.00396 0.02946 0.00438 0.00016 0.00045 0.00013 0.00000 0.00139 0.00128 0.00117 0.00096 0.00100 0.00102 0.00053 O1 1.09497 -0.31752 0.17687 1.00000 0.02232 0.02459 0.02271 0.00301 0.00610 0.00327 0.02294 0.00331 0.00011 0.00034 0.00010 0.00000 0.00094 0.00092 0.00085 0.00073 0.00072 0.00074 0.00039 O2 1.22666 0.02146 0.18610 1.00000 0.03023 0.02200 0.03153 -0.00447 0.00584 0.00069 0.02785 0.00340 0.00012 0.00035 0.00011 0.00000 0.00108 0.00094 0.00100 0.00079 0.00083 0.00079 0.00043 O3 1.30402 -0.26416 0.12732 1.00000 0.02245 0.02698 0.03063 -0.00511 0.00754 -0.00156 0.02633 0.00333 0.00012 0.00036 0.00011 0.00000 0.00097 0.00098 0.00096 0.00078 0.00077 0.00076 0.00042 O4 0.89815 0.39941 0.17765 1.00000 0.02981 0.01747 0.02725 -0.00367 0.00507 0.00091 0.02481 0.00327 0.00012 0.00033 0.00010 0.00000 0.00104 0.00086 0.00092 0.00071 0.00078 0.00074 0.00040 O5 0.93863 0.24642 0.04993 1.00000 0.02812 0.02799 0.02179 0.00475 0.00685 -0.00021 0.02566 0.00338 0.00012 0.00035 0.00010 0.00000 0.00101 0.00099 0.00088 0.00075 0.00075 0.00079 0.00041 S1 0.90927 0.19205 0.12425 1.00000 0.02195 0.01756 0.01920 0.00099 0.00403 0.00040 0.01951 0.00113 0.00004 0.00012 0.00003 0.00000 0.00032 0.00029 0.00029 0.00023 0.00023 0.00024 0.00015 Final Structure Factor Calculation for 2007src0079 in P2(1)/n Total number of l.s. parameters = 182 Maximum vector length = 511 Memory required = 2089 / 24017 wR2 = 0.1168 before cycle 16 for 3138 data and 0 / 182 parameters GooF = S = 1.094; Restrained GooF = 1.094 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0050 * P )^2 + 2.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0566 for 2581 Fo > 4sig(Fo) and 0.0722 for all 3138 data wR2 = 0.1168, GooF = S = 1.094, Restrained GooF = 1.094 for all data Occupancy sum of asymmetric unit = 20.00 for non-hydrogen and 13.00 for hydrogen atoms Principal mean square atomic displacements U 0.0248 0.0198 0.0176 C1 0.0231 0.0191 0.0172 C2 0.0245 0.0191 0.0186 C3 0.0269 0.0229 0.0148 C4 0.0264 0.0195 0.0146 C5 0.0391 0.0312 0.0183 C6 0.0378 0.0319 0.0252 C7 0.0237 0.0199 0.0166 C8 0.0281 0.0222 0.0167 C9 0.0347 0.0239 0.0191 C10 0.0311 0.0253 0.0192 C11 0.0318 0.0255 0.0206 C12 0.0258 0.0232 0.0188 C13 0.0369 0.0281 0.0234 N1 0.0286 0.0205 0.0197 O1 0.0333 0.0303 0.0200 O2 0.0347 0.0236 0.0207 O3 0.0299 0.0285 0.0161 O4 0.0307 0.0283 0.0180 O5 0.0220 0.0194 0.0171 S1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.020 0.030 0.042 0.055 0.069 0.087 0.113 0.156 1.000 Number in group 353. 276. 323. 320. 312. 303. 312. 315. 309. 315. GooF 1.141 1.249 1.185 1.171 1.138 1.113 1.011 0.971 0.910 1.017 K 3.283 1.475 1.143 1.031 0.995 1.000 0.993 1.004 1.007 1.005 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.64 inf Number in group 314. 328. 315. 305. 312. 311. 314. 309. 315. 315. GooF 1.176 1.187 1.204 1.181 1.018 1.053 0.907 0.990 0.923 1.238 K 1.067 1.069 1.025 1.020 1.012 1.003 1.003 0.993 1.000 1.006 R1 0.172 0.148 0.129 0.112 0.083 0.077 0.052 0.042 0.039 0.031 Recommended weighting scheme: WGHT 0.0000 2.6374 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) 3 3 9 110.81 7.26 6.16 0.015 1.20 -3 0 9 83.66 5.26 4.23 0.012 1.85 3 3 18 42.89 1.04 3.38 0.006 0.79 -11 4 8 112.24 203.74 3.36 0.077 0.91 12 1 13 25.57 94.29 3.30 0.052 0.83 7 0 17 207.02 356.63 3.24 0.102 0.85 3 3 16 50.49 5.44 3.20 0.013 0.86 8 2 11 206.37 319.54 3.18 0.096 1.02 7 4 13 -4.16 23.41 3.16 0.026 0.81 -19 1 6 97.51 16.00 3.13 0.022 0.81 -6 1 21 27.31 0.01 3.08 0.001 0.79 5 4 12 1.20 32.96 3.07 0.031 0.88 7 6 5 95.89 3.66 3.04 0.010 0.77 7 4 10 48.39 14.19 2.97 0.020 0.90 -4 1 8 38.66 81.70 2.94 0.049 1.86 3 6 3 27.30 1.52 2.92 0.007 0.84 1 3 1 79.29 135.09 2.90 0.063 1.70 -18 0 6 -0.90 45.13 2.89 0.036 0.87 -2 5 14 21.16 68.81 2.85 0.045 0.79 11 4 3 64.59 21.88 2.84 0.025 0.92 -17 3 8 537.91 379.87 2.83 0.105 0.80 -9 0 19 377.41 250.21 2.83 0.085 0.84 4 4 12 54.46 14.65 2.81 0.021 0.90 10 3 10 42.60 89.30 2.79 0.051 0.90 -5 2 16 103.47 53.91 2.78 0.040 0.97 -18 0 12 5.10 44.19 2.78 0.036 0.80 1 4 10 30.79 7.18 2.76 0.014 1.01 -12 1 17 88.16 42.97 2.74 0.035 0.85 -7 4 16 141.94 77.04 2.71 0.047 0.80 -6 0 2 1099.44 1306.63 2.67 0.195 2.61 18 1 4 45.20 92.75 2.65 0.052 0.81 4 3 13 208.49 140.90 2.64 0.064 0.97 13 4 4 499.48 381.24 2.63 0.105 0.84 -10 1 20 24.21 70.91 2.62 0.045 0.79 -13 1 13 85.93 142.46 2.59 0.064 0.95 2 1 1 796.05 940.02 2.59 0.165 4.08 -14 2 17 111.43 58.54 2.56 0.041 0.77 12 4 9 18.46 57.73 2.56 0.041 0.79 -10 3 18 122.72 65.16 2.55 0.044 0.77 -12 4 12 30.72 0.53 2.54 0.004 0.81 8 3 16 46.41 4.39 2.53 0.011 0.77 -6 1 19 20.23 0.04 2.52 0.001 0.87 8 3 14 32.95 76.26 2.52 0.047 0.83 -12 4 7 -9.33 14.62 2.52 0.021 0.89 9 4 12 122.40 72.71 2.51 0.046 0.79 12 0 8 229.39 140.64 2.50 0.064 1.03 -4 6 9 103.40 43.51 2.49 0.036 0.78 -7 5 10 38.27 10.70 2.49 0.018 0.84 -2 4 2 21.51 1.48 2.46 0.007 1.27 -8 2 19 57.39 106.48 2.46 0.056 0.82 Bond lengths and angles C1 - Distance Angles N1 1.1429 (0.0032) C2 1.4301 (0.0034) 179.04 (0.28) C1 - N1 C2 - Distance Angles C3 1.3479 (0.0034) C1 1.4301 (0.0034) 123.04 (0.23) S1 1.7556 (0.0025) 119.89 (0.19) 116.99 (0.18) C2 - C3 C1 C3 - Distance Angles O1 1.3260 (0.0029) C2 1.3479 (0.0034) 120.56 (0.22) H3 0.9500 119.72 119.72 C3 - O1 C2 C4 - Distance Angles O1 1.4285 (0.0028) C5 1.5075 (0.0035) 110.11 (0.20) H4A 0.9900 109.64 109.64 H4B 0.9900 109.64 109.64 108.15 C4 - O1 C5 H4A C5 - Distance Angles O2 1.2085 (0.0030) O3 1.3217 (0.0029) 126.07 (0.24) C4 1.5075 (0.0035) 124.18 (0.23) 109.70 (0.20) C5 - O2 O3 C6 - Distance Angles O3 1.4658 (0.0031) C7 1.5037 (0.0037) 107.30 (0.22) H6A 0.9900 110.25 110.25 H6B 0.9900 110.25 110.25 108.52 C6 - O3 C7 H6A C7 - Distance Angles C6 1.5037 (0.0037) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - C6 H7A H7B C8 - Distance Angles C13 1.3908 (0.0034) C9 1.3896 (0.0034) 121.52 (0.24) S1 1.7577 (0.0026) 118.76 (0.19) 119.59 (0.19) C8 - C13 C9 C9 - Distance Angles C10 1.3850 (0.0037) C8 1.3896 (0.0034) 119.00 (0.23) H9 0.9500 120.50 120.50 C9 - C10 C8 C10 - Distance Angles C9 1.3850 (0.0037) C11 1.3873 (0.0037) 120.02 (0.24) H10 0.9500 119.99 119.99 C10 - C9 C11 C11 - Distance Angles C10 1.3873 (0.0037) C12 1.3891 (0.0036) 120.48 (0.25) H11 0.9500 119.76 119.76 C11 - C10 C12 C12 - Distance Angles C13 1.3850 (0.0036) C11 1.3891 (0.0036) 120.15 (0.24) H12 0.9500 119.93 119.93 C12 - C13 C11 C13 - Distance Angles C12 1.3850 (0.0036) C8 1.3908 (0.0034) 118.80 (0.24) H13 0.9500 120.60 120.60 C13 - C12 C8 N1 - Distance Angles C1 1.1429 (0.0032) N1 - O1 - Distance Angles C3 1.3260 (0.0029) C4 1.4285 (0.0028) 115.58 (0.19) O1 - C3 O2 - Distance Angles C5 1.2085 (0.0030) O2 - O3 - Distance Angles C5 1.3217 (0.0029) C6 1.4658 (0.0031) 117.69 (0.20) O3 - C5 O4 - Distance Angles S1 1.4349 (0.0018) O4 - O5 - Distance Angles S1 1.4438 (0.0017) O5 - S1 - Distance Angles O4 1.4349 (0.0018) O5 1.4438 (0.0017) 119.88 (0.11) C2 1.7556 (0.0025) 107.96 (0.11) 106.67 (0.11) C8 1.7577 (0.0026) 108.87 (0.12) 109.32 (0.11) 102.77 (0.12) S1 - O4 O5 C2 FMAP and GRID set by program FMAP 2 2 9 GRID -4.167 -2 -2 4.167 2 2 R1 = 0.0717 for 3138 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.34 at 0.8549 0.1057 0.1176 [ 0.81 A from C8 ] Deepest hole -0.40 at 0.8785 0.1964 0.1412 [ 0.61 A from S1 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2728 / 21036 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.8549 0.1057 0.1176 1.00000 0.05 0.34 0.81 C8 0.96 S1 1.86 C9 1.89 O4 Q2 1 0.9556 0.0713 0.1570 1.00000 0.05 0.30 0.71 C2 1.05 S1 1.82 C3 1.86 C1 Q3 1 0.7584 0.3005 0.1031 1.00000 0.05 0.27 1.62 C9 1.72 H9 1.73 C8 2.30 C12 Q4 1 0.5806 -0.0714 0.1217 1.00000 0.05 0.24 1.21 H10 1.59 C10 1.69 H7B 2.07 C11 Q5 1 0.6794 -0.2409 0.0427 1.00000 0.05 0.24 0.77 C11 0.98 C12 1.44 H11 1.63 H12 Shortest distances between peaks (including symmetry equivalents) 1 2 1.63 1 3 1.81 4 5 2.39 3 5 2.80 Time profile in seconds ----------------------- 0.07: 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. 0.98: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.01: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.35: Structure factors and derivatives 2.97: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.52: Solve l.s. equations 0.00: Generate HTAB table 0.07: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.01: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src0079 finished at 13:18:15 Total CPU time: 7.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++