+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 15:08:49 on 19-Oct-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 03src0863 in C2/c CELL 0.71073 24.1967 10.5977 7.5551 90.000 95.146 90.000 ZERR 4.00 0.0016 0.0007 0.0004 0.000 0.003 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O S UNIT 68 48 8 16 20 V = 1929.54 F(000) = 960.0 Mu = 0.63 mm-1 Cell Wt = 1874.34 Rho = 1.613 MERG 2 OMIT -3.00 55.00 OMIT 3 3 0 FMAP 2 PLAN 10 SIZE 0.01 0.04 0.10 ACTA BOND $H CONF WGHT 0.04590 1.05080 L.S. 10 TEMP -153.00 FVAR 0.19896 C1 1 0.000000 0.108469 0.250000 10.50000 0.01667 0.02587 = 0.01890 0.00000 0.00490 0.00000 C2 1 -0.026024 -0.130587 0.209325 11.00000 0.02093 0.01802 = 0.02242 0.00130 0.00410 -0.00072 C3 1 -0.110930 -0.283074 0.314165 11.00000 0.02634 0.02532 = 0.02738 -0.00492 0.00492 -0.00736 AFIX 23 H3A 2 -0.089482 -0.292601 0.431283 11.00000 -1.20000 H3B 2 -0.135428 -0.208508 0.318279 11.00000 -1.20000 AFIX 0 C4 1 -0.144520 -0.399748 0.268421 11.00000 0.02384 0.02255 = 0.01914 -0.00300 0.00624 -0.00437 C5 1 -0.121925 -0.518932 0.304988 11.00000 0.02430 0.02863 = 0.01751 0.00210 0.00118 0.00014 AFIX 43 H5 2 -0.085661 -0.525591 0.363811 11.00000 -1.20000 AFIX 0 C6 1 -0.151310 -0.628155 0.257240 11.00000 0.02692 0.01965 = 0.02471 0.00420 0.00054 0.00202 AFIX 43 H6 2 -0.135191 -0.708379 0.284320 11.00000 -1.20000 AFIX 0 C7 1 -0.203950 -0.620325 0.170417 11.00000 0.02636 0.01639 = 0.02393 0.00010 0.00316 -0.00419 AFIX 43 H7 2 -0.224434 -0.694230 0.136332 11.00000 -1.20000 AFIX 0 C8 1 -0.225978 -0.501130 0.134539 11.00000 0.01730 0.02448 = 0.02021 -0.00038 0.00417 -0.00065 C9 1 -0.197137 -0.391324 0.180673 11.00000 0.02502 0.01741 = 0.02614 0.00015 0.00620 -0.00046 AFIX 43 H9 2 -0.213256 -0.311264 0.152464 11.00000 -1.20000 AFIX 0 N1 3 -0.281105 -0.491974 0.036395 11.00000 0.02139 0.02255 = 0.03276 0.00395 0.00250 0.00009 O1 4 -0.304479 -0.589316 -0.016676 11.00000 0.02546 0.02936 = 0.05487 -0.00339 -0.00792 -0.00624 O2 4 -0.301605 -0.387103 0.010265 11.00000 0.02769 0.02886 = 0.06862 0.01031 -0.00772 0.00492 S1 5 0.000000 0.263866 0.250000 10.50000 0.02932 0.01779 = 0.03027 0.00000 0.00708 0.00000 S2 5 -0.055896 0.017478 0.164914 11.00000 0.01805 0.02007 = 0.02640 0.00164 -0.00079 0.00132 S3 5 -0.064159 -0.265213 0.138136 11.00000 0.02275 0.02223 = 0.02612 -0.00445 0.00385 -0.00590 HKLF 4 Covalent radii and connectivity table for 03src0863 in C2/c C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 C1 - S1 S2 S2_$1 C2 - C2_$1 S2 S3 C3 - C4 S3 C4 - C9 C5 C3 C5 - C6 C4 C6 - C7 C5 C7 - C6 C8 C8 - C9 C7 N1 C9 - C4 C8 N1 - O2 O1 C8 O1 - N1 O2 - N1 S1 - C1 S2 - C1 C2 S3 - C2 C3 Operators for generating equivalent atoms: $1 -x, y, -z+1/2 10330 Reflections read, of which 337 rejected -31 =< h =< 31, -13 =< k =< 13, -9 =< l =< 9, Max. 2-theta = 55.00 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) -1 1 1 189.94 2.09 5 24.33 1 3 1 62.56 0.67 12 3.48 0 0 2 1649.40 18.79 6 166.54 3 3 2 562.59 4.85 12 26.36 3 7 3 287.70 1.01 9 28.55 -3 1 4 84.08 0.90 8 7.85 6 Inconsistent equivalents 2200 Unique reflections, of which 0 suppressed R(int) = 0.0832 R(sigma) = 0.0566 Friedel opposites merged Maximum memory for data reduction = 1486 / 25886 Special position constraints for C1 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 S1 x = 0.0000 z = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof 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 = 1827 / 163345 wR2 = 0.1014 before cycle 1 for 2200 data and 128 / 128 parameters GooF = S = 1.054; Restrained GooF = 1.054 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0459 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19934 0.00045 0.846 OSF Mean shift/su = 0.048 Maximum = 0.846 for OSF Max. shift = 0.000 A for C1 Max. dU = 0.000 for C1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1827 / 163345 wR2 = 0.1015 before cycle 2 for 2200 data and 128 / 128 parameters GooF = S = 1.055; Restrained GooF = 1.055 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0459 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19942 0.00045 0.163 OSF Mean shift/su = 0.016 Maximum = 0.163 for OSF Max. shift = 0.000 A for C1 Max. dU = 0.000 for C1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1827 / 163345 wR2 = 0.1015 before cycle 3 for 2200 data and 128 / 128 parameters GooF = S = 1.055; Restrained GooF = 1.055 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0459 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19942 0.00045 0.003 OSF Mean shift/su = 0.000 Maximum = 0.003 for OSF Max. shift = 0.000 A for C1 Max. dU = 0.000 for C3 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1827 / 163345 wR2 = 0.1015 before cycle 4 for 2200 data and 128 / 128 parameters GooF = S = 1.055; Restrained GooF = 1.055 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0459 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19942 0.00045 -0.001 OSF Mean shift/su = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for C5 Max. dU = 0.000 for C7 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1827 / 163345 wR2 = 0.1015 before cycle 5 for 2200 data and 128 / 128 parameters GooF = S = 1.055; Restrained GooF = 1.055 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0459 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19942 0.00045 -0.001 OSF Mean shift/su = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for C8 Max. dU = 0.000 for O1 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1827 / 163345 wR2 = 0.1015 before cycle 6 for 2200 data and 128 / 128 parameters GooF = S = 1.055; Restrained GooF = 1.055 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0459 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19942 0.00045 0.001 OSF Mean shift/su = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for C6 Max. dU = 0.000 for O1 Least-squares cycle 7 Maximum vector length = 511 Memory required = 1827 / 163345 wR2 = 0.1015 before cycle 7 for 2200 data and 128 / 128 parameters GooF = S = 1.055; Restrained GooF = 1.055 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0459 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19942 0.00045 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y S1 Max. shift = 0.000 A for O1 Max. dU = 0.000 for C2 Least-squares cycle 8 Maximum vector length = 511 Memory required = 1827 / 163345 wR2 = 0.1015 before cycle 8 for 2200 data and 128 / 128 parameters GooF = S = 1.055; Restrained GooF = 1.055 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0459 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19942 0.00045 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y S1 Max. shift = 0.000 A for C5 Max. dU = 0.000 for O2 Least-squares cycle 9 Maximum vector length = 511 Memory required = 1827 / 163345 wR2 = 0.1015 before cycle 9 for 2200 data and 128 / 128 parameters GooF = S = 1.055; Restrained GooF = 1.055 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0459 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19942 0.00045 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y S1 Max. shift = 0.000 A for C5 Max. dU = 0.000 for C1 Least-squares cycle 10 Maximum vector length = 511 Memory required = 1827 / 163345 wR2 = 0.1015 before cycle 10 for 2200 data and 128 / 128 parameters GooF = S = 1.055; Restrained GooF = 1.055 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0459 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19942 0.00045 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y S1 Max. shift = 0.000 A for C5 Max. dU = 0.000 for O2 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3A -0.0895 -0.2926 0.4313 23 0.990 0.000 C3 C4 S3 H3B -0.1354 -0.2085 0.3183 23 0.990 0.000 C3 C4 S3 H5 -0.0857 -0.5256 0.3638 43 0.950 0.000 C5 C6 C4 H6 -0.1352 -0.7084 0.2843 43 0.950 0.000 C6 C7 C5 H7 -0.2244 -0.6942 0.1363 43 0.950 0.000 C7 C6 C8 H9 -0.2133 -0.3113 0.1524 43 0.950 0.000 C9 C4 C8 03src0863 in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.00000 0.10850 0.25000 0.50000 0.01682 0.02598 0.01899 0.00000 0.00500 0.00000 0.02039 0.00320 0.00000 0.00030 0.00000 0.00000 0.00162 0.00170 0.00160 0.00000 0.00132 0.00000 0.00069 C2 -0.02603 -0.13059 0.20932 1.00000 0.02104 0.01810 0.02250 0.00130 0.00412 -0.00072 0.02042 0.00398 0.00010 0.00019 0.00029 0.00000 0.00117 0.00107 0.00120 0.00091 0.00096 0.00093 0.00049 C3 -0.11093 -0.28306 0.31416 1.00000 0.02642 0.02544 0.02747 -0.00493 0.00493 -0.00736 0.02630 0.00421 0.00010 0.00022 0.00032 0.00000 0.00135 0.00126 0.00133 0.00102 0.00106 0.00104 0.00056 H3A -0.08948 -0.29258 0.43128 1.00000 0.03155 0.00000 0.00000 H3B -0.13543 -0.20849 0.31827 1.00000 0.03155 0.00000 0.00000 C4 -0.14452 -0.39974 0.26842 1.00000 0.02390 0.02266 0.01925 -0.00301 0.00628 -0.00440 0.02168 0.00402 0.00010 0.00021 0.00029 0.00000 0.00124 0.00116 0.00114 0.00094 0.00097 0.00096 0.00050 C5 -0.12193 -0.51892 0.30499 1.00000 0.02437 0.02875 0.01759 0.00211 0.00120 0.00014 0.02361 0.00428 0.00011 0.00022 0.00030 0.00000 0.00123 0.00122 0.00117 0.00096 0.00095 0.00104 0.00051 H5 -0.08567 -0.52558 0.36383 1.00000 0.02834 0.00000 0.00000 C6 -0.15131 -0.62815 0.25724 1.00000 0.02702 0.01973 0.02481 0.00421 0.00060 0.00205 0.02396 0.00423 0.00010 0.00021 0.00030 0.00000 0.00133 0.00114 0.00125 0.00095 0.00103 0.00101 0.00053 H6 -0.13519 -0.70837 0.28432 1.00000 0.02875 0.00000 0.00000 C7 -0.20394 -0.62032 0.17041 1.00000 0.02645 0.01648 0.02398 0.00008 0.00318 -0.00421 0.02225 0.00412 0.00010 0.00020 0.00030 0.00000 0.00128 0.00109 0.00122 0.00090 0.00102 0.00096 0.00051 H7 -0.22442 -0.69423 0.13631 1.00000 0.02670 0.00000 0.00000 C8 -0.22598 -0.50113 0.13454 1.00000 0.01740 0.02456 0.02026 -0.00039 0.00420 -0.00065 0.02059 0.00401 0.00009 0.00021 0.00030 0.00000 0.00113 0.00120 0.00118 0.00093 0.00093 0.00097 0.00049 C9 -0.19713 -0.39132 0.18066 1.00000 0.02511 0.01750 0.02620 0.00016 0.00623 -0.00046 0.02270 0.00417 0.00010 0.00021 0.00031 0.00000 0.00129 0.00110 0.00123 0.00093 0.00101 0.00096 0.00051 H9 -0.21325 -0.31126 0.15244 1.00000 0.02724 0.00000 0.00000 N1 -0.28111 -0.49198 0.03639 1.00000 0.02148 0.02264 0.03288 0.00395 0.00250 0.00009 0.02566 0.00365 0.00008 0.00018 0.00027 0.00000 0.00104 0.00106 0.00120 0.00087 0.00089 0.00087 0.00047 O1 -0.30448 -0.58932 -0.01668 1.00000 0.02553 0.02950 0.05498 -0.00339 -0.00794 -0.00625 0.03737 0.00309 0.00007 0.00017 0.00025 0.00000 0.00101 0.00097 0.00122 0.00089 0.00090 0.00082 0.00047 O2 -0.30160 -0.38710 0.01025 1.00000 0.02778 0.02896 0.06872 0.01033 -0.00770 0.00491 0.04254 0.00349 0.00008 0.00017 0.00028 0.00000 0.00107 0.00100 0.00138 0.00091 0.00099 0.00083 0.00052 S1 0.00000 0.26386 0.25000 0.50000 0.02942 0.01790 0.03036 0.00000 0.00708 0.00000 0.02563 0.00080 0.00000 0.00008 0.00000 0.00000 0.00049 0.00041 0.00049 0.00000 0.00038 0.00000 0.00022 S2 -0.05590 0.01747 0.16491 1.00000 0.01815 0.02017 0.02651 0.00164 -0.00078 0.00132 0.02177 0.00102 0.00002 0.00005 0.00008 0.00000 0.00029 0.00029 0.00034 0.00023 0.00023 0.00023 0.00017 S3 -0.06416 -0.26521 0.13814 1.00000 0.02285 0.02233 0.02623 -0.00445 0.00386 -0.00590 0.02370 0.00103 0.00003 0.00005 0.00008 0.00000 0.00032 0.00031 0.00034 0.00023 0.00025 0.00024 0.00017 Final Structure Factor Calculation for 03src0863 in C2/c Total number of l.s. parameters = 128 Maximum vector length = 511 Memory required = 1699 / 24017 wR2 = 0.1015 before cycle 11 for 2200 data and 0 / 128 parameters GooF = S = 1.055; Restrained GooF = 1.055 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0459 * P )^2 + 1.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0415 for 1714 Fo > 4sig(Fo) and 0.0629 for all 2200 data wR2 = 0.1015, GooF = S = 1.055, Restrained GooF = 1.055 for all data Occupancy sum of asymmetric unit = 14.00 for non-hydrogen and 6.00 for hydrogen atoms Principal mean square atomic displacements U 0.0260 0.0212 0.0140 C1 0.0240 0.0202 0.0171 C2 0.0359 0.0247 0.0183 C3 0.0298 0.0190 0.0162 C4 0.0291 0.0245 0.0172 C5 0.0282 0.0268 0.0169 C6 0.0281 0.0238 0.0149 C7 0.0247 0.0214 0.0157 C8 0.0293 0.0214 0.0174 C9 0.0342 0.0215 0.0212 N1 0.0602 0.0336 0.0183 O1 0.0748 0.0333 0.0195 O2 0.0340 0.0250 0.0179 S1 0.0278 0.0208 0.0167 S2 0.0315 0.0232 0.0164 S3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.024 0.037 0.051 0.066 0.085 0.106 0.135 0.187 1.000 Number in group 236. 213. 229. 207. 218. 220. 225. 213. 218. 221. GooF 1.055 0.987 1.059 1.183 1.061 0.970 0.990 1.159 0.982 1.087 K 3.825 1.240 1.055 1.000 1.001 0.984 0.994 1.010 1.004 1.015 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.31 1.66 inf Number in group 226. 218. 220. 220. 216. 229. 210. 222. 218. 221. GooF 1.106 0.906 0.965 0.980 1.003 0.989 1.092 0.959 1.042 1.417 K 0.920 1.031 1.035 1.039 1.025 1.018 1.030 1.009 1.000 1.010 R1 0.167 0.120 0.096 0.082 0.069 0.069 0.048 0.038 0.027 0.032 Recommended weighting scheme: WGHT 0.0458 1.0308 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)/su Fc/Fc(max) Resolution(A) 10 0 2 92.22 0.63 5.76 0.002 1.95 -9 3 6 2106.74 1326.83 5.63 0.110 1.12 -18 0 6 3145.57 2249.97 4.30 0.143 0.96 -26 0 6 2500.26 3916.56 4.09 0.189 0.78 12 0 0 17318.46 13887.29 3.98 0.355 2.01 5 5 2 1730.86 1375.44 3.77 0.112 1.70 10 8 2 395.72 243.86 3.69 0.047 1.10 -7 5 2 697.98 919.69 3.53 0.091 1.66 -12 0 4 611.03 815.13 3.48 0.086 1.44 11 1 2 2095.81 1731.31 3.31 0.125 1.80 -23 1 5 283.12 128.09 3.28 0.034 0.90 -20 0 8 -130.99 160.10 3.23 0.038 0.78 3 5 0 179.23 119.48 3.14 0.033 2.05 -4 4 8 685.36 413.99 3.05 0.061 0.89 -8 8 6 5793.87 4813.07 3.05 0.209 0.89 7 11 5 206.20 389.51 2.88 0.060 0.78 2 4 1 179.90 122.57 2.86 0.033 2.43 10 8 7 901.97 1347.28 2.84 0.111 0.77 4 4 0 357.83 452.37 2.82 0.064 2.43 -13 1 8 152.11 333.52 2.80 0.055 0.87 6 0 4 73.79 29.07 2.64 0.016 1.65 -10 4 1 326.17 241.39 2.62 0.047 1.76 9 1 2 12874.76 11224.13 2.60 0.319 2.05 -6 4 2 2400.51 2783.89 2.58 0.159 1.95 -17 3 8 -60.18 143.07 2.57 0.036 0.80 1 13 1 1292.58 982.28 2.54 0.094 0.81 8 6 0 525.31 400.94 2.54 0.060 1.52 9 3 0 9654.06 8493.69 2.52 0.278 2.13 -25 7 3 -47.24 162.63 2.50 0.038 0.79 13 9 1 103.31 2.95 2.48 0.005 0.98 15 7 2 3578.06 3032.55 2.44 0.166 1.04 6 4 1 1876.70 1636.36 2.41 0.122 2.09 8 4 0 48.05 81.39 2.40 0.027 1.99 10 2 1 1017.55 851.53 2.39 0.088 2.06 -7 5 3 38.61 0.01 2.37 0.000 1.50 -2 6 3 406.21 296.22 2.37 0.052 1.44 -4 0 4 2383.74 2744.54 2.36 0.158 1.84 12 8 0 395.55 527.83 2.36 0.069 1.11 11 9 2 236.51 120.05 2.36 0.033 0.99 -18 10 2 40.03 201.94 2.35 0.043 0.82 12 6 6 227.45 133.12 2.34 0.035 0.89 -3 3 2 3884.46 4408.06 2.34 0.200 2.50 19 7 3 2966.65 2463.49 2.33 0.150 0.89 -11 5 2 238.83 158.61 2.32 0.038 1.44 23 1 3 240.77 90.57 2.32 0.029 0.93 -10 10 1 5325.79 4687.74 2.31 0.206 0.97 13 3 5 965.70 798.51 2.29 0.085 1.07 16 0 6 2616.78 3087.16 2.28 0.168 0.92 -12 6 7 464.75 664.72 2.27 0.078 0.86 22 4 2 2351.80 2000.55 2.26 0.135 0.96 Bond lengths and angles C1 - Distance Angles S1 1.6465 (0.0033) S2 1.7370 (0.0019) 123.74 (0.09) S2_$1 1.7370 (0.0019) 123.74 (0.09) 112.53 (0.18) C1 - S1 S2 C2 - Distance Angles C2_$1 1.3510 (0.0047) S2 1.7474 (0.0022) 116.10 (0.08) S3 1.7570 (0.0022) 125.58 (0.08) 118.27 (0.13) C2 - C2_$1 S2 C3 - Distance Angles C4 1.5029 (0.0030) S3 1.8317 (0.0025) 105.94 (0.15) H3A 0.9900 110.55 110.55 H3B 0.9900 110.55 110.55 108.70 C3 - C4 S3 H3A C4 - Distance Angles C9 1.3845 (0.0034) C5 1.3941 (0.0032) 118.73 (0.21) C3 1.5029 (0.0030) 120.81 (0.21) 120.37 (0.22) C4 - C9 C5 C5 - Distance Angles C6 1.3890 (0.0032) C4 1.3941 (0.0032) 121.40 (0.23) H5 0.9500 119.30 119.30 C5 - C6 C4 C6 - Distance Angles C7 1.3818 (0.0034) C5 1.3890 (0.0032) 120.12 (0.21) H6 0.9500 119.94 119.94 C6 - C7 C5 C7 - Distance Angles C6 1.3818 (0.0034) C8 1.3883 (0.0030) 117.95 (0.21) H7 0.9500 121.02 121.02 C7 - C6 C8 C8 - Distance Angles C9 1.3853 (0.0031) C7 1.3883 (0.0030) 122.63 (0.22) N1 1.4701 (0.0030) 119.03 (0.20) 118.27 (0.20) C8 - C9 C7 C9 - Distance Angles C4 1.3845 (0.0034) C8 1.3853 (0.0031) 119.15 (0.21) H9 0.9500 120.42 120.42 C9 - C4 C8 N1 - Distance Angles O2 1.2259 (0.0025) O1 1.2263 (0.0025) 122.82 (0.21) C8 1.4701 (0.0030) 118.47 (0.20) 118.71 (0.19) N1 - O2 O1 O1 - Distance Angles N1 1.2263 (0.0025) O1 - O2 - Distance Angles N1 1.2259 (0.0025) O2 - S1 - Distance Angles C1 1.6465 (0.0033) S1 - S2 - Distance Angles C1 1.7370 (0.0019) C2 1.7474 (0.0022) 97.63 (0.12) S2 - C1 S3 - Distance Angles C2 1.7570 (0.0022) C3 1.8317 (0.0025) 101.73 (0.11) S3 - C2 Selected torsion angles -97.40 ( 0.23) S3 - C3 - C4 - C9 79.01 ( 0.24) S3 - C3 - C4 - C5 -0.79 ( 0.34) C9 - C4 - C5 - C6 -177.27 ( 0.21) C3 - C4 - C5 - C6 0.48 ( 0.35) C4 - C5 - C6 - C7 -0.39 ( 0.34) C5 - C6 - C7 - C8 0.66 ( 0.35) C6 - C7 - C8 - C9 177.78 ( 0.20) C6 - C7 - C8 - N1 1.01 ( 0.33) C5 - C4 - C9 - C8 177.48 ( 0.20) C3 - C4 - C9 - C8 -0.98 ( 0.36) C7 - C8 - C9 - C4 -178.09 ( 0.20) N1 - C8 - C9 - C4 -5.46 ( 0.33) C9 - C8 - N1 - O2 177.31 ( 0.22) C7 - C8 - N1 - O2 174.13 ( 0.21) C9 - C8 - N1 - O1 -3.10 ( 0.32) C7 - C8 - N1 - O1 179.75 ( 0.07) S1 - C1 - S2 - C2 -0.25 ( 0.07) S2_$1 - C1 - S2 - C2 0.86 ( 0.26) C2_$1 - C2 - S2 - C1 -176.67 ( 0.12) S3 - C2 - S2 - C1 101.80 ( 0.30) C2_$1 - C2 - S3 - C3 -80.93 ( 0.15) S2 - C2 - S3 - C3 -178.15 ( 0.17) C4 - C3 - S3 - C2 FMAP and GRID set by program FMAP 2 3 12 GRID -2.778 -1 -2 2.778 1 2 R1 = 0.0623 for 2200 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.36 at 0.2866 0.9452 0.1701 [ 0.69 A from C8 ] Deepest hole -0.40 at 0.4656 0.5006 0.2502 [ 0.81 A from S2 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2368 / 16650 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.2134 -0.5548 0.1701 1.00000 0.05 0.36 0.69 C8 0.73 C7 1.52 H7 1.77 C6 Q2 1 -0.0471 -0.0166 0.0248 1.00000 0.05 0.33 1.16 S2 1.88 C2 2.37 C1 2.64 C1 Q3 1 -0.0435 -0.0539 0.1681 1.00000 0.05 0.29 0.81 S2 0.96 C2 2.02 C2 2.08 C1 Q4 1 0.0064 0.1765 0.2031 1.00000 0.05 0.28 0.82 C1 1.01 S1 2.25 S2 2.26 S2 Q5 1 -0.0714 -0.1793 0.0596 1.00000 0.05 0.28 1.09 S3 1.59 C2 2.25 S2 2.48 C3 Q6 1 -0.0609 -0.3534 0.0428 1.00000 0.05 0.26 1.19 S3 1.92 H5 2.58 C3 2.60 C5 Q7 1 -0.1321 -0.4539 0.2497 1.00000 0.05 0.26 0.67 C4 0.83 C5 1.55 H5 1.74 C9 Q8 1 -0.0297 0.0843 0.2172 1.00000 0.05 0.26 0.78 C1 1.01 S2 2.04 S1 2.28 C2 Q9 1 -0.2023 -0.4469 0.1318 1.00000 0.05 0.24 0.70 C9 0.81 C8 1.47 H9 1.74 C4 Q10 1 -0.0329 0.0260 0.3412 1.00000 0.05 0.24 1.40 S2 1.40 C1 1.95 C2 2.15 S2 Shortest distances between peaks (including symmetry equivalents) 4 4 0.80 8 10 1.13 2 3 1.15 1 9 1.22 4 8 1.25 4 8 1.32 2 10 1.46 8 8 1.48 3 8 1.54 3 10 1.56 3 5 1.67 8 10 1.73 4 10 1.76 2 8 1.82 7 9 1.85 2 5 1.85 5 6 1.87 3 10 2.04 2 10 2.15 4 10 2.17 10 10 2.20 1 7 2.27 3 3 2.34 2 2 2.37 3 8 2.40 2 10 2.43 2 8 2.50 3 10 2.52 5 10 2.55 4 5 2.64 6 7 2.65 2 4 2.67 2 4 2.71 3 4 2.73 3 4 2.75 2 8 2.78 2 3 2.80 10 10 2.81 2 8 2.81 2 3 2.84 Time profile in seconds ----------------------- 0.00: Read and process instructions 0.00: Fit rigid groups 0.00: 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 0.02: Analyse other restraints etc. 0.39: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.58: Structure factors and derivatives 0.47: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.09: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 15:08:51 Total CPU time: 1.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++