+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 11:34:41 on 03-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 99SOT048 in P2(1)/c CELL 0.71073 15.521 6.827 13.574 90.00 100.06 90.00 ZERR 4.00 0.003 0.001 0.003 0.00 0.03 0.00 LATT 1 SYMM -X, .5+Y, .5-Z SFAC C H N O S UNIT 48 56 8 12 8 V = 1416.21 F(000) = 624.0 Mu = 0.38 mm-1 Cell Wt = 1193.49 Rho = 1.399 L.S. 4 BOND FMAP 2 PLAN 10 REM OMIT -3 51 OMIT 1 0 0 OMIT 1 1 2 OMIT -8 0 4 OMIT -4 0 16 WGHT 0.100000 FVAR 0.34517 S1 5 0.179742 0.164644 0.381328 11.00000 0.02083 0.03800 = 0.02350 -0.00090 0.00487 0.00160 S2 5 0.267792 0.216947 0.597046 11.00000 0.02229 0.03841 = 0.03011 -0.00200 -0.00351 0.00117 O1 4 -0.104117 0.236937 0.333302 11.00000 0.01615 0.03805 = 0.01855 -0.00210 0.00072 -0.00126 O2 4 -0.208558 0.131536 0.163293 11.00000 0.02065 0.05115 = 0.02708 -0.00838 0.00592 -0.00492 O3 4 -0.325507 0.260753 0.218125 11.00000 0.01756 0.04396 = 0.03474 -0.00868 -0.00309 0.00365 N1 3 0.094429 0.227598 0.515877 11.00000 0.01767 0.02036 = 0.01821 -0.00036 0.00099 -0.00130 N2 3 0.072416 0.184711 0.344905 11.00000 0.02126 0.03192 = 0.01868 -0.00037 0.00382 0.00040 C1 1 0.065872 0.256495 0.605979 11.00000 0.02723 0.02414 = 0.01682 0.00037 0.00143 -0.00117 AFIX 43 H1 2 0.105449 0.256722 0.665929 11.00000 -1.20000 AFIX 0 C2 1 -0.019779 0.284126 0.605292 11.00000 0.02901 0.02485 = 0.01583 -0.00140 0.00567 -0.00203 AFIX 43 H2A 2 -0.039526 0.304709 0.665322 11.00000 -1.20000 AFIX 0 C3 1 -0.081320 0.282369 0.513280 11.00000 0.01921 0.02495 = 0.02429 0.00037 0.00459 -0.00145 AFIX 43 H3 2 -0.140306 0.304979 0.513926 11.00000 -1.20000 AFIX 0 C4 1 -0.053996 0.247971 0.425495 11.00000 0.02160 0.02024 = 0.01901 0.00186 0.00051 -0.00220 C5 1 0.037455 0.217510 0.424499 11.00000 0.02133 0.01828 = 0.01774 0.00121 0.00061 -0.00121 C6 1 -0.195612 0.266717 0.328635 11.00000 0.01919 0.03027 = 0.02395 -0.00037 0.00362 0.00024 AFIX 23 H6A 2 -0.207088 0.403027 0.341822 11.00000 -1.20000 H6B 2 -0.216589 0.186846 0.378622 11.00000 -1.20000 AFIX 0 C7 1 -0.241979 0.210481 0.225477 11.00000 0.01836 0.02637 = 0.02716 0.00317 0.00165 -0.00428 C8 1 -0.391516 0.201576 0.130921 11.00000 0.01470 0.04892 = 0.03446 -0.00144 -0.00460 -0.00340 C9 1 -0.394228 -0.018110 0.124122 11.00000 0.02532 0.05299 = 0.05216 -0.00570 -0.00369 -0.00669 AFIX 137 H9A 2 -0.341167 -0.065025 0.105118 11.00000 -1.50000 H9B 2 -0.443325 -0.057603 0.074922 11.00000 -1.50000 H9C 2 -0.399925 -0.072043 0.187984 11.00000 -1.50000 AFIX 0 C10 1 -0.475512 0.280616 0.157770 11.00000 0.02481 0.08547 = 0.07736 -0.02028 -0.00892 0.01407 AFIX 137 H10A 2 -0.485152 0.222303 0.219278 11.00000 -1.50000 H10B 2 -0.523566 0.249499 0.105395 11.00000 -1.50000 H10C 2 -0.471106 0.420191 0.165671 11.00000 -1.50000 AFIX 0 C11 1 -0.371508 0.296926 0.037139 11.00000 0.04401 0.10572 = 0.04972 0.03665 -0.01817 -0.02717 AFIX 137 H11A 2 -0.362966 0.434964 0.048298 11.00000 -1.50000 H11B 2 -0.419507 0.276082 -0.016852 11.00000 -1.50000 H11C 2 -0.319329 0.240368 0.020331 11.00000 -1.50000 AFIX 0 C12 1 0.181866 0.204596 0.506227 11.00000 0.02085 0.02171 = 0.02604 0.00164 0.00400 0.00052 HKLF 4 1 0.0000 0.0000 1.0000 0.0000-1.0000 0.0000 1.0000 0.0000 0.0000 Covalent radii and connectivity table for 99SOT048 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 S1 - N2 C12 S2 - C12 O1 - C4 C6 O2 - C7 O3 - C7 C8 N1 - C1 C5 C12 N2 - C5 S1 C1 - C2 N1 C2 - C1 C3 C3 - C4 C2 C4 - C3 O1 C5 C5 - N2 N1 C4 C6 - O1 C7 C7 - O2 O3 C6 C8 - O3 C9 C11 C10 C9 - C8 C10 - C8 C11 - C8 C12 - N1 S2 S1 h k l Fo^2 Sigma Why rejected -14 0 9 21.79 5.24 observed but should be systematically absent 0 1 0 2.13 0.53 observed but should be systematically absent 0 1 0 2.93 0.33 observed but should be systematically absent 0 1 0 3.92 0.54 observed but should be systematically absent 0 1 0 4.36 0.53 observed but should be systematically absent 1 0 3 2.70 0.65 observed but should be systematically absent 13523 Reflections read, of which 560 rejected -19 =< h =< 19, -8 =< k =< 8, -17 =< l =< 17, Max. 2-theta = 54.87 6 Systematic absence violations 0 Inconsistent equivalents 3159 Unique reflections, of which 0 suppressed R(int) = 0.0583 R(sigma) = 0.0587 Friedel opposites merged Maximum memory for data reduction = 1692 / 31332 Default effective X-H distances for T = 20.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 0.98 0.97 0.96 0.93 0.86 0.89 1.10 0.82 0.93 0.86 0.93 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 = 2167 / 218617 wR2 = 0.1221 before cycle 1 for 3159 data and 175 / 175 parameters GooF = S = 0.808; Restrained GooF = 0.808 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34517 0.00085 0.001 OSF Mean shift/esd = 0.162 Maximum = -0.643 for U13 C10 Max. shift = 0.008 A for H9B Max. dU = 0.000 for C11 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2167 / 218617 wR2 = 0.1218 before cycle 2 for 3159 data and 175 / 175 parameters GooF = S = 0.807; Restrained GooF = 0.807 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34514 0.00085 -0.041 OSF Mean shift/esd = 0.054 Maximum = 0.202 for U11 C10 Max. shift = 0.003 A for H9B Max. dU = 0.000 for C11 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2167 / 218617 wR2 = 0.1218 before cycle 3 for 3159 data and 175 / 175 parameters GooF = S = 0.807; Restrained GooF = 0.807 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34513 0.00085 -0.003 OSF Mean shift/esd = 0.003 Maximum = -0.011 for U33 C10 Max. shift = 0.000 A for H11C Max. dU = 0.000 for C10 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2167 / 218617 wR2 = 0.1218 before cycle 4 for 3159 data and 175 / 175 parameters GooF = S = 0.807; Restrained GooF = 0.807 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34513 0.00085 -0.001 OSF Mean shift/esd = 0.001 Maximum = -0.005 for x C5 Max. shift = 0.000 A for H11A Max. dU = 0.000 for C1 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.1054 0.2567 0.6660 43 0.930 0.000 C1 C2 N1 H2A -0.0396 0.3048 0.6653 43 0.930 0.000 C2 C1 C3 H3 -0.1404 0.3049 0.5139 43 0.930 0.000 C3 C4 C2 H6A -0.2071 0.4030 0.3419 23 0.970 0.000 C6 O1 C7 H6B -0.2165 0.1868 0.3787 23 0.970 0.000 C6 O1 C7 H9A -0.3415 -0.0649 0.1046 137 0.960 0.000 C9 C8 H9A H9B -0.4438 -0.0576 0.0755 137 0.960 0.000 C9 C8 H9A H9C -0.3994 -0.0718 0.1883 137 0.960 0.000 C9 C8 H9A H10A -0.4851 0.2225 0.2192 137 0.960 0.000 C10 C8 H10A H10B -0.5236 0.2492 0.1053 137 0.960 0.000 C10 C8 H10A H10C -0.4711 0.4202 0.1654 137 0.960 0.000 C10 C8 H10A H11A -0.3626 0.4348 0.0483 137 0.960 0.000 C11 C8 H11A H11B -0.4194 0.2764 -0.0169 137 0.960 0.000 C11 C8 H11A H11C -0.3193 0.2397 0.0203 137 0.960 0.000 C11 C8 H11A 99SOT048 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq S1 0.17975 0.16465 0.38132 1.00000 0.02074 0.03805 0.02340 -0.00091 0.00493 0.00159 0.02727 0.00093 0.00003 0.00007 0.00004 0.00000 0.00029 0.00031 0.00029 0.00021 0.00020 0.00021 0.00017 S2 0.26781 0.21694 0.59705 1.00000 0.02233 0.03842 0.02996 -0.00199 -0.00349 0.00116 0.03121 0.00095 0.00003 0.00008 0.00004 0.00000 0.00031 0.00031 0.00032 0.00022 0.00023 0.00021 0.00018 O1 -0.10406 0.23694 0.33327 1.00000 0.01605 0.03812 0.01849 -0.00207 0.00079 -0.00130 0.02449 0.00241 0.00009 0.00019 0.00010 0.00000 0.00074 0.00078 0.00073 0.00058 0.00056 0.00056 0.00033 O2 -0.20851 0.13155 0.16325 1.00000 0.02091 0.05119 0.02686 -0.00821 0.00577 -0.00505 0.03279 0.00250 0.00009 0.00021 0.00011 0.00000 0.00077 0.00091 0.00081 0.00070 0.00062 0.00067 0.00036 O3 -0.32551 0.26077 0.21808 1.00000 0.01801 0.04371 0.03483 -0.00873 -0.00345 0.00366 0.03315 0.00261 0.00009 0.00021 0.00012 0.00000 0.00079 0.00087 0.00090 0.00067 0.00065 0.00062 0.00038 N1 0.09447 0.22759 0.51582 1.00000 0.01782 0.02027 0.01836 -0.00036 0.00096 -0.00130 0.01908 0.00274 0.00010 0.00021 0.00012 0.00000 0.00086 0.00074 0.00084 0.00061 0.00065 0.00061 0.00035 N2 0.07236 0.18471 0.34494 1.00000 0.02101 0.03199 0.01872 -0.00034 0.00384 0.00043 0.02386 0.00296 0.00011 0.00023 0.00012 0.00000 0.00091 0.00087 0.00084 0.00068 0.00068 0.00067 0.00038 C1 0.06582 0.25649 0.60604 1.00000 0.02679 0.02436 0.01662 0.00033 0.00180 -0.00116 0.02283 0.00354 0.00013 0.00026 0.00015 0.00000 0.00117 0.00095 0.00099 0.00077 0.00080 0.00081 0.00044 H1 0.10536 0.25666 0.66602 1.00000 0.02740 0.00000 0.00000 C2 -0.01982 0.28415 0.60526 1.00000 0.02966 0.02462 0.01587 -0.00134 0.00545 -0.00203 0.02320 0.00352 0.00013 0.00026 0.00014 0.00000 0.00118 0.00093 0.00097 0.00074 0.00083 0.00079 0.00044 H2A -0.03958 0.30478 0.66528 1.00000 0.02785 0.00000 0.00000 C3 -0.08142 0.28238 0.51326 1.00000 0.01936 0.02499 0.02397 0.00038 0.00454 -0.00146 0.02268 0.00355 0.00013 0.00026 0.00015 0.00000 0.00105 0.00093 0.00105 0.00079 0.00080 0.00077 0.00043 H3 -0.14041 0.30494 0.51387 1.00000 0.02722 0.00000 0.00000 C4 -0.05394 0.24797 0.42546 1.00000 0.02119 0.02022 0.01933 0.00190 0.00059 -0.00215 0.02060 0.00342 0.00013 0.00025 0.00014 0.00000 0.00104 0.00089 0.00101 0.00073 0.00079 0.00074 0.00042 C5 0.03748 0.21752 0.42444 1.00000 0.02183 0.01821 0.01741 0.00118 0.00045 -0.00119 0.01951 0.00339 0.00013 0.00024 0.00014 0.00000 0.00104 0.00084 0.00096 0.00072 0.00076 0.00072 0.00041 C6 -0.19561 0.26671 0.32871 1.00000 0.01863 0.03032 0.02441 -0.00041 0.00375 0.00024 0.02445 0.00361 0.00013 0.00028 0.00015 0.00000 0.00107 0.00101 0.00109 0.00082 0.00083 0.00080 0.00044 H6A -0.20709 0.40301 0.34193 1.00000 0.02935 0.00000 0.00000 H6B -0.21654 0.18680 0.37872 1.00000 0.02935 0.00000 0.00000 C7 -0.24207 0.21047 0.22550 1.00000 0.01816 0.02660 0.02689 0.00317 0.00199 -0.00429 0.02411 0.00363 0.00013 0.00028 0.00015 0.00000 0.00105 0.00098 0.00113 0.00081 0.00085 0.00076 0.00045 C8 -0.39160 0.20161 0.13089 1.00000 0.01513 0.04877 0.03406 -0.00150 -0.00488 -0.00345 0.03376 0.00388 0.00014 0.00033 0.00017 0.00000 0.00109 0.00128 0.00129 0.00099 0.00090 0.00089 0.00053 C9 -0.39432 -0.01799 0.12423 1.00000 0.02604 0.05289 0.05185 -0.00581 -0.00412 -0.00672 0.04490 0.00391 0.00014 0.00034 0.00019 0.00000 0.00124 0.00146 0.00155 0.00121 0.00108 0.00106 0.00062 H9A -0.34151 -0.06490 0.10459 1.00000 0.06735 0.00000 0.00000 H9B -0.44376 -0.05761 0.07554 1.00000 0.06735 0.00000 0.00000 H9C -0.39942 -0.07180 0.18830 1.00000 0.06735 0.00000 0.00000 C10 -0.47550 0.28057 0.15765 1.00000 0.02593 0.08471 0.07728 -0.02050 -0.01009 0.01441 0.06494 0.00537 0.00017 0.00046 0.00026 0.00000 0.00149 0.00206 0.00228 0.00170 0.00140 0.00133 0.00090 H10A -0.48512 0.22246 0.21921 1.00000 0.09740 0.00000 0.00000 H10B -0.52355 0.24925 0.10531 1.00000 0.09740 0.00000 0.00000 H10C -0.47113 0.42018 0.16542 1.00000 0.09740 0.00000 0.00000 C11 -0.37139 0.29679 0.03711 1.00000 0.04301 0.10590 0.04971 0.03646 -0.01759 -0.02679 0.06929 0.00542 0.00018 0.00048 0.00022 0.00000 0.00175 0.00244 0.00183 0.00167 0.00142 0.00158 0.00100 H11A -0.36259 0.43475 0.04831 1.00000 0.10393 0.00000 0.00000 H11B -0.41942 0.27639 -0.01690 1.00000 0.10393 0.00000 0.00000 H11C -0.31931 0.23974 0.02030 1.00000 0.10393 0.00000 0.00000 C12 0.18184 0.20460 0.50625 1.00000 0.02151 0.02155 0.02575 0.00160 0.00369 0.00052 0.02299 0.00360 0.00013 0.00026 0.00015 0.00000 0.00108 0.00091 0.00108 0.00077 0.00084 0.00074 0.00044 Final Structure Factor Calculation for 99SOT048 in P2(1)/c Total number of l.s. parameters = 175 Maximum vector length = 511 Memory required = 1992 / 24017 wR2 = 0.1218 before cycle 5 for 3159 data and 0 / 175 parameters GooF = S = 0.807; Restrained GooF = 0.807 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0393 for 2304 Fo > 4sig(Fo) and 0.0679 for all 3159 data wR2 = 0.1218, GooF = S = 0.807, Restrained GooF = 0.807 for all data Occupancy sum of asymmetric unit = 19.00 for non-hydrogen and 14.00 for hydrogen atoms Principal mean square atomic displacements U 0.0383 0.0236 0.0199 S1 0.0402 0.0349 0.0184 S2 0.0384 0.0202 0.0149 O1 0.0541 0.0243 0.0199 O2 0.0521 0.0314 0.0159 O3 0.0213 0.0200 0.0159 N1 0.0320 0.0210 0.0186 N2 0.0281 0.0239 0.0165 C1 0.0304 0.0240 0.0152 C2 0.0254 0.0240 0.0187 C3 0.0258 0.0185 0.0175 C4 0.0245 0.0179 0.0162 C5 0.0304 0.0244 0.0186 C6 0.0322 0.0238 0.0163 C7 0.0491 0.0397 0.0124 C8 0.0597 0.0533 0.0217 C9 0.1127 0.0611 0.0210 C10 0.1434 0.0405 0.0240 C11 0.0264 0.0219 0.0207 C12 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.022 0.033 0.044 0.057 0.071 0.090 0.114 0.168 1.000 Number in group 343. 313. 321. 312. 306. 309. 312. 313. 316. 314. GooF 0.829 0.885 0.954 0.955 0.834 0.821 0.790 0.676 0.652 0.582 K 2.325 1.133 1.001 1.045 1.021 1.008 0.996 0.994 1.009 1.028 Resolution(A) 0.77 0.81 0.84 0.87 0.92 0.98 1.05 1.16 1.33 1.66 inf Number in group 324. 316. 307. 321. 312. 317. 313. 316. 315. 318. GooF 0.803 0.814 0.836 0.720 0.828 0.794 0.748 0.739 0.853 0.917 K 1.038 1.027 1.041 1.010 1.010 1.001 1.021 1.023 1.023 1.022 R1 0.204 0.175 0.137 0.087 0.075 0.055 0.040 0.034 0.033 0.030 Recommended weighting scheme: WGHT 0.0533 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) -8 0 2 107.53 62.53 4.84 0.044 1.93 -6 0 10 22.15 62.03 4.10 0.044 1.28 -8 2 2 14.12 3.89 4.00 0.011 1.68 7 1 6 114.93 83.02 3.59 0.051 1.41 -6 6 1 2.60 25.00 3.59 0.028 1.04 -3 0 16 329.34 514.13 3.56 0.126 0.85 7 1 4 11.80 0.36 3.45 0.003 1.65 -16 2 2 110.78 34.39 3.45 0.033 0.93 6 2 1 318.37 242.99 3.32 0.087 1.98 -17 3 4 68.24 19.38 3.31 0.024 0.84 4 4 2 47.00 66.87 3.29 0.045 1.49 11 2 1 39.81 57.44 3.29 0.042 1.26 -15 1 4 76.43 41.03 3.27 0.036 1.01 8 3 10 -7.95 12.34 3.24 0.020 0.93 -4 1 1 -1.32 2.61 3.20 0.009 3.36 6 2 5 11.03 23.63 3.20 0.027 1.52 -7 0 4 34.34 55.17 3.08 0.041 1.99 6 3 7 48.94 31.34 3.05 0.031 1.20 2 3 3 89.25 116.93 3.05 0.060 1.92 5 1 6 354.94 278.41 3.05 0.093 1.62 13 5 3 52.37 10.13 3.03 0.018 0.85 -6 0 4 39.11 58.94 3.02 0.043 2.22 -10 1 1 48.63 34.56 2.99 0.033 1.51 -9 0 2 1179.47 927.15 2.97 0.169 1.72 9 1 8 509.99 656.76 2.96 0.142 1.08 -1 7 1 118.49 87.34 2.94 0.052 0.97 -15 4 7 103.60 50.58 2.94 0.039 0.84 3 2 0 44.24 34.17 2.90 0.032 2.84 -8 0 14 200.92 136.52 2.89 0.065 0.92 -8 4 8 38.44 60.66 2.87 0.043 1.07 1 2 5 -2.93 3.67 2.86 0.011 2.05 -1 8 7 -20.62 25.28 2.83 0.028 0.78 -8 2 4 12.74 23.94 2.82 0.027 1.59 11 2 12 93.67 166.28 2.80 0.072 0.78 12 1 6 26.19 7.03 2.79 0.015 1.02 -9 1 4 99.21 127.36 2.77 0.063 1.59 5 0 6 336.32 427.62 2.77 0.115 1.67 -8 4 14 86.18 155.57 2.75 0.069 0.81 -10 0 10 182.42 131.81 2.73 0.064 1.11 -6 2 13 -13.39 23.14 2.70 0.027 0.97 6 5 8 44.96 66.81 2.69 0.045 0.94 -6 2 8 32.48 49.15 2.69 0.039 1.39 -6 0 16 995.58 750.45 2.68 0.152 0.84 -19 0 4 262.26 160.62 2.67 0.070 0.82 -15 2 2 -11.23 16.15 2.66 0.022 0.99 1 2 11 9.21 23.39 2.65 0.027 1.13 3 2 7 45.31 60.33 2.64 0.043 1.52 -4 5 6 0.35 10.20 2.62 0.018 1.14 8 1 14 11.76 50.24 2.62 0.039 0.79 -8 4 11 22.78 4.76 2.61 0.012 0.93 Bond lengths and angles S1 - Distance Angles N2 1.6593 (0.0017) C12 1.7122 (0.0021) 97.23 (0.09) S1 - N2 S2 - Distance Angles C12 1.6530 (0.0021) S2 - O1 - Distance Angles C4 1.3552 (0.0024) C6 1.4260 (0.0025) 116.05 (0.15) O1 - C4 O2 - Distance Angles C7 1.1957 (0.0024) O2 - O3 - Distance Angles C7 1.3264 (0.0026) C8 1.4805 (0.0026) 121.40 (0.17) O3 - C7 N1 - Distance Angles C1 1.3880 (0.0025) C5 1.3938 (0.0025) 122.74 (0.17) C12 1.3935 (0.0026) 124.42 (0.17) 112.84 (0.16) N1 - C1 C5 N2 - Distance Angles C5 1.3083 (0.0025) S1 1.6593 (0.0017) 107.91 (0.14) N2 - C5 C1 - Distance Angles C2 1.3409 (0.0029) N1 1.3880 (0.0025) 118.88 (0.18) C1 - C2 C2 - Distance Angles C1 1.3409 (0.0029) C3 1.4341 (0.0028) 120.99 (0.19) C2 - C1 C3 - Distance Angles C4 1.3546 (0.0028) C2 1.4341 (0.0028) 120.21 (0.19) C3 - C4 C4 - Distance Angles C3 1.3546 (0.0028) O1 1.3552 (0.0024) 127.14 (0.18) C5 1.4365 (0.0029) 119.79 (0.18) 113.06 (0.17) C4 - C3 O1 C5 - Distance Angles N2 1.3083 (0.0025) N1 1.3938 (0.0025) 116.92 (0.17) C4 1.4365 (0.0029) 125.76 (0.18) 117.30 (0.17) C5 - N2 N1 C6 - Distance Angles O1 1.4260 (0.0025) C7 1.5090 (0.0029) 108.36 (0.16) C6 - O1 C7 - Distance Angles O2 1.1957 (0.0024) O3 1.3264 (0.0026) 127.09 (0.19) C6 1.5090 (0.0029) 125.05 (0.19) 107.85 (0.17) C7 - O2 O3 C8 - Distance Angles O3 1.4805 (0.0026) C9 1.5021 (0.0031) 109.19 (0.18) C11 1.5102 (0.0035) 109.85 (0.19) 112.74 (0.23) C10 1.5111 (0.0035) 102.50 (0.19) 110.75 (0.21) 111.33 (0.23) C8 - O3 C9 C11 C9 - Distance Angles C8 1.5021 (0.0031) C9 - C10 - Distance Angles C8 1.5111 (0.0035) C10 - C11 - Distance Angles C8 1.5102 (0.0035) C11 - C12 - Distance Angles N1 1.3935 (0.0026) S2 1.6530 (0.0021) 126.63 (0.16) S1 1.7122 (0.0021) 105.06 (0.14) 128.30 (0.13) C12 - N1 S2 FMAP and GRID set by program FMAP 2 2 11 GRID -3.125 -2 -2 3.125 2 2 R1 = 0.0673 for 3159 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.28 at 0.0665 0.2358 0.4733 [ 0.66 A from N1 ] Deepest hole -0.29 at 0.2250 0.1365 0.4200 [ 0.82 A from S1 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2397 / 20252 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0665 0.2358 0.4733 1.00000 0.05 0.28 0.66 N1 0.74 C5 1.78 C12 1.79 N2 Q2 1 -0.0406 0.2835 0.5568 1.00000 0.05 0.27 0.68 C2 0.79 C3 1.48 H2A 1.56 H3 Q3 1 -0.0030 0.2374 0.4237 1.00000 0.05 0.27 0.64 C5 0.80 C4 1.75 N2 1.79 N1 Q4 1 -0.3258 0.3003 0.2487 1.00000 0.05 0.24 0.50 O3 1.52 C7 1.87 C8 2.13 C6 Q5 1 0.1447 0.2030 0.5139 1.00000 0.05 0.24 0.60 C12 0.80 N1 1.88 C5 1.93 C1 Q6 1 0.1857 0.1649 0.4459 1.00000 0.05 0.23 0.86 S1 0.88 C12 1.89 N1 2.04 N2 Q7 1 0.0573 0.2318 0.3928 1.00000 0.05 0.22 0.58 C5 0.80 N2 1.67 N1 1.86 C4 Q8 1 0.0618 0.1864 0.2985 1.00000 0.05 0.22 0.62 N2 1.83 C5 1.98 S1 2.07 H1 Q9 1 0.1054 0.1819 0.5131 1.00000 0.05 0.21 0.36 N1 1.22 C12 1.47 C5 1.58 C1 Q10 1 -0.2042 0.2182 0.1581 1.00000 0.05 0.21 0.60 O2 1.17 C7 2.20 O3 2.32 C6 Shortest distances between peaks (including symmetry equivalents) 5 9 0.63 1 9 0.82 1 7 1.08 3 7 1.09 1 3 1.17 5 6 1.24 1 5 1.26 7 8 1.33 6 9 1.67 7 9 1.71 3 9 1.93 5 7 1.95 1 6 2.01 2 3 2.02 6 7 2.05 3 8 2.15 1 2 2.19 1 8 2.38 3 5 2.41 4 10 2.49 6 8 2.53 2 9 2.54 8 9 2.87 2 7 2.93 3 6 2.93 5 8 2.98 Time profile in seconds ----------------------- 0.17: 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. 1.91: 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 0.83: Structure factors and derivatives 0.98: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.20: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.08: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 11:34:46 Total CPU time: 4.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++