+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - MSDOS 32-BIT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-1 + + s92 started at 13:35:42 on 15-Nov-1999 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P-1 CELL 0.71073 6.050 7.855 12.195 92.78 103.54 111.46 ZERR 2.00 0.001 0.002 0.002 0.03 0.03 0.03 LATT 1 SFAC C H N O S UNIT 20 18 6 4 2 V = 518.58 F(000) = 244.0 Mu = 0.30 mm-1 Cell Wt = 470.52 Rho = 1.507 PLAN 5 ACTA FMAP 2 L.S. 4 BOND WGHT 0.0297 0.2258 FVAR 0.48141 S1 5 0.37872 0.69940 0.76750 11.00000 0.02086 0.02853 = 0.02390 0.00667 0.00652 0.01212 O1 4 0.61268 0.68189 0.79516 11.00000 0.02206 0.04191 = 0.02858 0.00815 0.00508 0.01929 O2 4 0.17810 0.57258 0.80232 11.00000 0.02428 0.02764 = 0.02938 0.00958 0.00932 0.00754 N1 3 0.30296 0.68695 0.62894 11.00000 0.01854 0.03400 = 0.02025 0.00395 0.00591 0.01271 N2 3 0.11509 0.76064 0.46150 11.00000 0.02201 0.02938 = 0.02366 0.00416 0.00682 0.00986 N3 3 -0.29554 0.72627 0.53872 11.00000 0.02210 0.03353 = 0.02362 0.00297 0.00408 0.01368 C1 1 0.50438 1.28187 0.90304 11.00000 0.05794 0.03068 = 0.02583 0.00339 -0.00114 0.02089 C2 1 0.66945 1.24966 0.85244 11.00000 0.04645 0.03156 = 0.03216 0.01036 0.00647 0.00533 C3 1 0.63005 1.07147 0.81084 11.00000 0.02999 0.03393 = 0.03027 0.00840 0.00976 0.00843 C4 1 0.42305 0.92502 0.82061 11.00000 0.02014 0.02657 = 0.01909 0.00762 0.00204 0.00966 C5 1 0.25619 0.95612 0.87147 11.00000 0.02471 0.03552 = 0.02418 0.00507 0.00389 0.01357 C6 1 0.29885 1.13616 0.91258 11.00000 0.04129 0.04395 = 0.02515 0.00117 0.00099 0.02760 C7 1 0.09962 0.71557 0.56425 11.00000 0.01707 0.02265 = 0.02278 0.00067 0.00318 0.00891 C8 1 -0.07932 0.78566 0.39730 11.00000 0.02749 0.03462 = 0.02316 0.00635 0.00572 0.01305 C9 1 -0.28203 0.77204 0.43601 11.00000 0.02450 0.03281 = 0.02765 0.00303 0.00146 0.01405 C10 1 -0.10778 0.69452 0.60272 11.00000 0.02223 0.02964 = 0.02339 0.00317 0.00505 0.01103 H1A 2 0.42881 0.70975 0.59845 11.00000 0.05112 H1 2 0.52800 1.40931 0.93028 11.00000 0.05025 H2 2 0.80620 1.34593 0.84102 11.00000 0.07082 H3 2 0.74052 1.04357 0.77224 11.00000 0.03295 H5 2 0.12303 0.85869 0.87955 11.00000 0.03115 H6 2 0.18561 1.16266 0.94892 11.00000 0.04155 H8 2 -0.07551 0.81522 0.32192 11.00000 0.03208 H9 2 -0.41602 0.79070 0.38762 11.00000 0.03872 H10 2 -0.12761 0.65324 0.67085 11.00000 0.02506 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 N1 C4 O1 - S1 O2 - S1 N1 - C7 S1 N2 - C7 C8 N3 - C10 C9 C1 - C2 C6 C2 - C1 C3 C3 - C2 C4 C4 - C5 C3 S1 C5 - C6 C4 C6 - C1 C5 C7 - N2 N1 C10 C8 - N2 C9 C9 - N3 C8 C10 - N3 C7 4818 Reflections read, of which 0 rejected -7 =< h =< 7, -9 =< k =< 9, -13 =< l =< 14, Max. 2-theta = 49.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 0 0 1 6.55 0.10 2 32.67 -2 8 5 5.36 1.66 2 14.30 2 Inconsistent equivalents 1807 Unique reflections, of which 0 suppressed R(int) = 0.0577 R(sigma) = 0.0699 Friedel opposites merged Maximum memory for data reduction = 1362 / 18327 Least-squares cycle 1 Maximum vector length = 511 Memory required = 1789 / 225832 wR2 = 0.1060 before cycle 1 for 1807 data and 181 / 181 parameters GooF = S = 1.073; Restrained GooF = 1.073 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0297 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.48141 0.00134 0.003 OSF Mean shift/esd = 0.003 Maximum = -0.061 for z S1 Max. shift = 0.000 A for C2 Max. dU = 0.000 for H1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1789 / 225832 wR2 = 0.1060 before cycle 2 for 1807 data and 181 / 181 parameters GooF = S = 1.073; Restrained GooF = 1.073 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0297 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.48141 0.00134 -0.002 OSF Mean shift/esd = 0.001 Maximum = -0.019 for z S1 Max. shift = 0.000 A for H10 Max. dU = 0.000 for H6 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1789 / 225832 wR2 = 0.1060 before cycle 3 for 1807 data and 181 / 181 parameters GooF = S = 1.073; Restrained GooF = 1.073 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0297 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.48141 0.00134 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for U11 H5 Max. shift = 0.000 A for H6 Max. dU = 0.000 for H5 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1789 / 225832 wR2 = 0.1060 before cycle 4 for 1807 data and 181 / 181 parameters GooF = S = 1.073; Restrained GooF = 1.073 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0297 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.48141 0.00134 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z S1 Max. shift = 0.000 A for H6 Max. dU = 0.000 for H10 Largest correlation matrix elements 0.564 U12 C6 / U11 C6 0.524 U12 O1 / U11 O1 0.501 U12 N1 / U11 N1 0.535 U12 S1 / U11 S1 0.509 U12 C5 / U11 C5 0.530 U12 C6 / U22 C6 0.504 U12 C1 / U11 C1 s92 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq S1 0.37872 0.69940 0.76750 1.00000 0.02086 0.02853 0.02390 0.00667 0.00652 0.01212 0.02349 0.00148 0.00011 0.00009 0.00006 0.00000 0.00036 0.00040 0.00039 0.00028 0.00025 0.00026 0.00022 O1 0.61268 0.68189 0.79516 1.00000 0.02206 0.04191 0.02858 0.00815 0.00508 0.01929 0.02904 0.00407 0.00029 0.00026 0.00015 0.00000 0.00095 0.00116 0.00109 0.00088 0.00075 0.00081 0.00047 O2 0.17810 0.57258 0.80232 1.00000 0.02428 0.02764 0.02938 0.00958 0.00932 0.00754 0.02729 0.00399 0.00030 0.00024 0.00016 0.00000 0.00095 0.00103 0.00108 0.00083 0.00076 0.00075 0.00046 N1 0.30296 0.68695 0.62894 1.00000 0.01854 0.03400 0.02025 0.00395 0.00591 0.01271 0.02341 0.00479 0.00038 0.00030 0.00018 0.00000 0.00114 0.00133 0.00125 0.00099 0.00091 0.00094 0.00052 N2 0.11509 0.76064 0.46150 1.00000 0.02201 0.02938 0.02366 0.00416 0.00682 0.00986 0.02492 0.00473 0.00036 0.00029 0.00018 0.00000 0.00113 0.00126 0.00128 0.00099 0.00089 0.00091 0.00052 N3 -0.29554 0.72627 0.53872 1.00000 0.02210 0.03353 0.02362 0.00297 0.00408 0.01368 0.02600 0.00471 0.00035 0.00030 0.00018 0.00000 0.00116 0.00134 0.00131 0.00103 0.00091 0.00096 0.00054 C1 0.50438 1.28187 0.90304 1.00000 0.05794 0.03068 0.02583 0.00339 -0.00114 0.02089 0.03936 0.00710 0.00058 0.00044 0.00026 0.00000 0.00209 0.00181 0.00173 0.00140 0.00142 0.00153 0.00078 C2 0.66945 1.24966 0.85244 1.00000 0.04645 0.03156 0.03216 0.01036 0.00647 0.00533 0.04018 0.00707 0.00059 0.00043 0.00027 0.00000 0.00193 0.00182 0.00183 0.00145 0.00144 0.00141 0.00080 C3 0.63005 1.07147 0.81084 1.00000 0.02999 0.03393 0.03027 0.00840 0.00976 0.00843 0.03215 0.00655 0.00050 0.00040 0.00025 0.00000 0.00155 0.00175 0.00168 0.00133 0.00123 0.00122 0.00068 C4 0.42305 0.92502 0.82061 1.00000 0.02014 0.02657 0.01909 0.00762 0.00204 0.00966 0.02220 0.00559 0.00042 0.00035 0.00021 0.00000 0.00127 0.00145 0.00142 0.00112 0.00099 0.00103 0.00059 C5 0.25619 0.95612 0.87147 1.00000 0.02471 0.03552 0.02418 0.00507 0.00389 0.01357 0.02806 0.00634 0.00048 0.00040 0.00023 0.00000 0.00151 0.00171 0.00157 0.00129 0.00114 0.00125 0.00065 C6 0.29885 1.13616 0.91258 1.00000 0.04129 0.04395 0.02515 0.00117 0.00099 0.02760 0.03512 0.00687 0.00056 0.00043 0.00025 0.00000 0.00176 0.00193 0.00165 0.00138 0.00129 0.00147 0.00072 C7 0.09962 0.71557 0.56425 1.00000 0.01707 0.02265 0.02278 0.00067 0.00318 0.00891 0.02098 0.00546 0.00041 0.00034 0.00022 0.00000 0.00125 0.00137 0.00147 0.00111 0.00099 0.00099 0.00057 C8 -0.07932 0.78566 0.39730 1.00000 0.02749 0.03462 0.02316 0.00635 0.00572 0.01305 0.02826 0.00615 0.00046 0.00038 0.00025 0.00000 0.00148 0.00166 0.00159 0.00129 0.00116 0.00118 0.00065 C9 -0.28203 0.77204 0.43601 1.00000 0.02451 0.03281 0.02765 0.00303 0.00146 0.01405 0.02852 0.00618 0.00048 0.00038 0.00024 0.00000 0.00146 0.00160 0.00165 0.00127 0.00115 0.00117 0.00065 C10 -0.10778 0.69452 0.60272 1.00000 0.02223 0.02964 0.02339 0.00317 0.00505 0.01103 0.02504 0.00592 0.00044 0.00037 0.00024 0.00000 0.00136 0.00152 0.00157 0.00124 0.00110 0.00108 0.00061 H1A 0.42881 0.70975 0.59845 1.00000 0.05112 0.07322 0.00583 0.00433 0.00289 0.00000 0.00973 H1 0.52800 1.40931 0.93028 1.00000 0.05024 0.07193 0.00521 0.00457 0.00278 0.00000 0.00936 H2 0.80620 1.34593 0.84102 1.00000 0.07082 0.08333 0.00643 0.00518 0.00313 0.00000 0.01143 H3 0.74052 1.04357 0.77224 1.00000 0.03295 0.06150 0.00472 0.00377 0.00250 0.00000 0.00770 H5 0.12303 0.85869 0.87955 1.00000 0.03115 0.06412 0.00504 0.00389 0.00239 0.00000 0.00757 H6 0.18561 1.16266 0.94892 1.00000 0.04155 0.06641 0.00515 0.00407 0.00266 0.00000 0.00853 H8 -0.07551 0.81522 0.32192 1.00000 0.03208 0.06006 0.00454 0.00368 0.00249 0.00000 0.00766 H9 -0.41602 0.79069 0.38762 1.00000 0.03872 0.06601 0.00522 0.00383 0.00254 0.00000 0.00806 H10 -0.12761 0.65324 0.67085 1.00000 0.02506 0.05845 0.00441 0.00358 0.00249 0.00000 0.00713 Final Structure Factor Calculation for s92 in P-1 Total number of l.s. parameters = 181 Maximum vector length = 511 Memory required = 1608 / 24017 wR2 = 0.1060 before cycle 5 for 1807 data and 0 / 181 parameters GooF = S = 1.073; Restrained GooF = 1.073 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0297 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0433 for 1411 Fo > 4sig(Fo) and 0.0648 for all 1807 data wR2 = 0.1060, GooF = S = 1.073, Restrained GooF = 1.073 for all data Occupancy sum of asymmetric unit = 16.00 for non-hydrogen and 9.00 for hydrogen atoms Principal mean square atomic displacements U 0.0295 0.0226 0.0184 S1 0.0424 0.0297 0.0150 O1 0.0348 0.0272 0.0199 O2 0.0341 0.0202 0.0159 N1 0.0297 0.0237 0.0214 N2 0.0342 0.0247 0.0191 N3 0.0671 0.0283 0.0227 C1 0.0621 0.0337 0.0248 C2 0.0401 0.0314 0.0250 C3 0.0297 0.0229 0.0139 C4 0.0355 0.0279 0.0207 C5 0.0559 0.0277 0.0217 C6 0.0265 0.0205 0.0159 C7 0.0349 0.0280 0.0220 C8 0.0357 0.0304 0.0195 C9 0.0299 0.0241 0.0211 C10 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.013 0.028 0.042 0.059 0.077 0.095 0.118 0.151 0.210 1.000 Number in group 183. 188. 173. 184. 179. 184. 173. 181. 182. 180. GooF 0.861 1.049 1.205 1.038 1.173 1.191 1.038 0.929 1.046 1.155 K 2.561 0.979 0.955 0.974 0.946 0.983 0.992 1.008 1.027 1.002 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.15 1.26 1.45 1.83 inf Number in group 189. 182. 173. 185. 174. 186. 178. 179. 181. 180. GooF 1.041 0.979 0.846 1.049 0.936 1.035 1.042 0.992 1.193 1.482 K 0.954 1.010 1.016 1.037 1.010 1.035 1.026 1.026 1.043 0.966 R1 0.165 0.116 0.075 0.092 0.059 0.056 0.044 0.037 0.040 0.042 Recommended weighting scheme: WGHT 0.0297 0.2258 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 5 5 33.25 55.19 3.77 0.080 1.26 2 -1 3 80.77 59.61 3.65 0.083 2.12 -1 0 1 5240.34 6157.98 3.59 0.848 5.52 2 0 1 -0.28 2.37 3.49 0.017 2.50 -6 4 10 21.57 61.55 3.32 0.085 0.84 0 1 0 6.54 1.64 3.17 0.014 7.23 -1 0 9 24.17 38.68 3.03 0.067 1.35 -1 1 11 23.60 7.04 3.02 0.029 1.08 -1 6 2 47.55 65.12 3.00 0.087 1.23 0 -2 2 53.46 39.45 2.99 0.068 3.30 -1 4 4 1.48 9.54 2.93 0.033 1.58 0 -1 1 2664.56 3081.30 2.91 0.600 6.61 -2 1 0 69.49 86.40 2.91 0.100 2.94 0 6 3 32.82 48.10 2.88 0.075 1.11 1 -7 7 111.03 76.01 2.87 0.094 0.96 -1 -1 2 525.23 604.16 2.87 0.266 3.58 3 -3 1 1187.44 1046.52 2.84 0.350 1.76 3 -3 2 107.45 129.16 2.83 0.123 1.67 -3 -6 6 -2.08 11.89 2.82 0.037 0.87 -3 -2 3 5.61 0.52 2.82 0.008 1.46 1 -3 1 58.13 73.71 2.82 0.093 2.56 2 -4 10 -3.30 6.51 2.80 0.028 0.98 2 2 0 19.41 11.48 2.79 0.037 1.85 -1 1 0 561.88 642.05 2.68 0.274 5.48 -1 -3 5 246.14 196.45 2.64 0.151 1.68 -6 3 10 122.45 157.14 2.64 0.135 0.86 -4 4 12 110.59 56.73 2.63 0.081 0.86 -4 -3 3 20.80 31.13 2.59 0.060 1.06 -2 2 5 2.71 7.91 2.57 0.030 1.94 0 3 6 19.60 10.60 2.55 0.035 1.42 5 1 3 90.44 122.88 2.54 0.120 0.92 0 -2 1 3.36 0.17 2.51 0.005 3.61 -2 -2 2 413.20 363.62 2.50 0.206 1.91 1 5 8 8.36 22.38 2.50 0.051 0.88 0 -2 10 23.79 38.06 2.49 0.067 1.17 2 1 7 22.93 33.33 2.49 0.062 1.20 -5 6 9 -0.82 13.06 2.45 0.039 0.86 -1 -2 12 51.46 28.86 2.44 0.058 0.99 0 -3 7 4.54 11.86 2.41 0.037 1.48 -4 -3 9 42.36 59.36 2.41 0.083 0.94 -1 0 2 1374.24 1547.99 2.41 0.425 4.66 0 3 12 29.02 49.87 2.39 0.076 0.86 -2 8 1 15.03 0.80 2.38 0.010 0.97 -1 0 5 55.66 68.90 2.37 0.090 2.40 -5 0 6 91.70 111.14 2.35 0.114 1.08 2 -2 4 8.85 2.92 2.32 0.018 1.86 1 1 6 5.47 10.77 2.31 0.035 1.57 -1 0 12 5.90 16.96 2.31 0.044 1.01 -1 2 1 301.87 346.66 2.31 0.201 3.61 1 -1 10 2.55 10.23 2.31 0.035 1.11 Bond lengths and angles S1 - Distance Angles O2 1.4296 (0.0018) O1 1.4351 (0.0017) 119.45 (0.11) N1 1.6319 (0.0023) 109.76 (0.12) 104.62 (0.12) C4 1.7584 (0.0027) 108.05 (0.12) 108.73 (0.12) 105.36 (0.12) S1 - O2 O1 N1 O1 - Distance Angles S1 1.4351 (0.0017) O1 - O2 - Distance Angles S1 1.4296 (0.0018) O2 - N1 - Distance Angles C7 1.3969 (0.0031) S1 1.6319 (0.0023) 125.13 (0.19) N1 - C7 N2 - Distance Angles C7 1.3334 (0.0033) C8 1.3371 (0.0032) 116.08 (0.22) N2 - C7 N3 - Distance Angles C10 1.3315 (0.0032) C9 1.3322 (0.0035) 117.78 (0.23) N3 - C10 C1 - Distance Angles C2 1.3785 (0.0046) C6 1.3816 (0.0044) 120.29 (0.30) C1 - C2 C2 - Distance Angles C1 1.3785 (0.0046) C3 1.3798 (0.0044) 120.12 (0.29) C2 - C1 C3 - Distance Angles C2 1.3798 (0.0044) C4 1.3910 (0.0036) 119.47 (0.29) C3 - C2 C4 - Distance Angles C5 1.3865 (0.0037) C3 1.3910 (0.0037) 120.80 (0.26) S1 1.7584 (0.0027) 120.78 (0.20) 118.42 (0.21) C4 - C5 C3 C5 - Distance Angles C6 1.3862 (0.0041) C4 1.3865 (0.0037) 118.86 (0.27) C5 - C6 C6 - Distance Angles C1 1.3816 (0.0044) C5 1.3862 (0.0041) 120.46 (0.30) C6 - C1 C7 - Distance Angles N2 1.3334 (0.0033) N1 1.3969 (0.0031) 115.03 (0.21) C10 1.3975 (0.0036) 122.16 (0.22) 122.78 (0.25) C7 - N2 N1 C8 - Distance Angles N2 1.3371 (0.0032) C9 1.3850 (0.0039) 122.34 (0.27) C8 - N2 C9 - Distance Angles N3 1.3322 (0.0035) C8 1.3850 (0.0039) 120.95 (0.24) C9 - N3 C10 - Distance Angles N3 1.3315 (0.0031) C7 1.3975 (0.0036) 120.61 (0.26) C10 - N3 FMAP and GRID set by program FMAP 2 1 17 GRID -3.571 -2 -2 3.571 2 2 R1 = 0.0644 for 1807 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.25 at 0.0443 0.6827 0.9851 [ 1.94 A from H5 ] Deepest hole -0.43 at 0.3265 0.5893 0.7422 [ 0.82 A from S1 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 1672 / 15608 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0443 0.6827 0.9851 1.00000 0.05 0.25 1.94 H5 2.16 H2 2.20 C2 2.39 H6 Q2 1 0.1011 1.0580 0.9843 1.00000 0.05 0.22 0.98 H6 1.61 C6 2.03 H5 2.11 C5 Q3 1 0.4588 1.1789 0.9475 1.00000 0.05 0.21 0.89 C6 0.99 C1 1.62 H6 1.74 H1 Q4 1 0.0566 0.7886 0.9007 1.00000 0.05 0.19 0.66 H5 1.55 C5 2.45 O2 2.49 O1 Q5 1 0.3134 0.4821 0.7175 1.00000 0.05 0.19 1.65 S1 1.73 O2 1.90 O1 1.99 N1 Shortest distances between peaks (including symmetry equivalents) 1 4 1.35 2 2 1.38 2 3 2.19 2 4 2.20 2 4 2.37 1 2 2.54 1 3 2.69 1 1 2.78 1 2 2.84 3 4 2.99 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. 0.44: 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 1.64: Structure factors and derivatives 3.58: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.06: Apply other restraints 0.44: Solve l.s. equations 0.00: Generate HTAB table 0.19: Other dependent quantities, CIF, tables 0.20: Analysis of variance 0.11: Merge reflections for Fourier and .fcf 0.16: Fourier summations 0.06: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 13:35:49 Total elapsed time: 7.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++