+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007may0012 started at 15:39:33 on 01-Oct-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007may0012 in P2(1)/c CELL 0.71073 8.1628 7.9648 11.0496 90.000 95.230 90.000 ZERR 4.00 0.0003 0.0003 0.0004 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 32 20 4 12 V = 715.40 F(000) = 336.0 Mu = 0.12 mm-1 Cell Wt = 652.52 Rho = 1.515 MERG 2 OMIT -3.00 55.00 FMAP 2 PLAN 10 ACTA BOND $H SIZE 0.1 0.1 0.08 L.S. 6 TEMP -153.00 WGHT 0.0387 0.3578 FVAR 1.83703 C1 1 0.559721 0.424812 1.182306 11.00000 0.02534 0.02378 = 0.02359 -0.00363 0.00148 0.00189 AFIX 43 H1 2 0.560210 0.544029 1.179672 11.00000 -1.20000 AFIX 0 C2 1 0.644667 0.330153 1.091536 11.00000 0.02282 0.02152 = 0.02035 -0.00095 0.00219 -0.00014 C3 1 0.751133 0.138164 0.982965 11.00000 0.02196 0.01929 = 0.02027 0.00109 0.00212 -0.00221 C4 1 0.660334 0.154743 1.079240 11.00000 0.02263 0.02064 = 0.02119 0.00072 0.00357 -0.00105 AFIX 43 H4 2 0.617551 0.068755 1.126951 11.00000 -1.20000 AFIX 0 C5 1 0.810573 -0.007975 0.924217 11.00000 0.02003 0.02351 = 0.01973 -0.00087 0.00402 -0.00145 C6 1 0.930674 -0.143675 0.784631 11.00000 0.02615 0.02601 = 0.02811 -0.00558 0.00690 0.00250 AFIX 43 H6 2 0.988045 -0.167197 0.715536 11.00000 -1.20000 AFIX 0 C7 1 0.876257 -0.261008 0.859135 11.00000 0.02502 0.02284 = 0.03477 -0.00305 0.00666 0.00029 AFIX 43 H7 2 0.887949 -0.379198 0.852186 11.00000 -1.20000 AFIX 0 C8 1 0.797906 -0.173654 0.950216 11.00000 0.02431 0.02368 = 0.02755 0.00168 0.00631 -0.00108 AFIX 43 H8 2 0.746973 -0.221669 1.015996 11.00000 -1.20000 AFIX 0 N1 3 0.719050 0.414750 1.009926 11.00000 0.03279 0.02077 = 0.02707 -0.00088 0.00811 0.00110 O1 4 0.489434 0.354721 1.260029 11.00000 0.02969 0.03018 = 0.02418 -0.00328 0.00622 0.00056 O2 4 0.788094 0.292283 0.939195 11.00000 0.03148 0.01941 = 0.02461 0.00142 0.00990 -0.00079 O3 4 0.891859 0.014585 0.822239 11.00000 0.02956 0.02272 = 0.02307 -0.00015 0.00989 0.00035 HKLF 4 Covalent radii and connectivity table for 2007may0012 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1 C2 C2 - N1 C4 C1 C3 - C4 O2 C5 C4 - C3 C2 C5 - C8 O3 C3 C6 - C7 O3 C7 - C6 C8 C8 - C5 C7 N1 - C2 O2 O1 - C1 O2 - C3 N1 O3 - C5 C6 9918 Reflections read, of which 419 rejected -10 =< h =< 10, -10 =< k =< 10, -14 =< l =< 14, Max. 2-theta = 54.99 0 Systematic absence violations 0 Inconsistent equivalents 1637 Unique reflections, of which 0 suppressed R(int) = 0.0258 R(sigma) = 0.0210 Friedel opposites merged Maximum memory for data reduction = 1077 / 16383 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 = 1360 / 140606 wR2 = 0.0983 before cycle 1 for 1637 data and 109 / 109 parameters GooF = S = 1.090; Restrained GooF = 1.090 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0387 * P )^2 + 0.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.83404 0.00484 -0.618 OSF Mean shift/esd = 0.226 Maximum = -0.730 for U33 C5 Max. shift = 0.001 A for C8 Max. dU = 0.000 for C5 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1360 / 140606 wR2 = 0.0978 before cycle 2 for 1637 data and 109 / 109 parameters GooF = S = 1.086; Restrained GooF = 1.086 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0387 * P )^2 + 0.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.83313 0.00481 -0.188 OSF Mean shift/esd = 0.078 Maximum = -0.245 for U33 C5 Max. shift = 0.000 A for H8 Max. dU = 0.000 for C5 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1360 / 140606 wR2 = 0.0978 before cycle 3 for 1637 data and 109 / 109 parameters GooF = S = 1.086; Restrained GooF = 1.086 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0387 * P )^2 + 0.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.83314 0.00481 0.002 OSF Mean shift/esd = 0.004 Maximum = 0.013 for U22 C8 Max. shift = 0.000 A for C5 Max. dU = 0.000 for C8 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1360 / 140606 wR2 = 0.0978 before cycle 4 for 1637 data and 109 / 109 parameters GooF = S = 1.086; Restrained GooF = 1.086 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0387 * P )^2 + 0.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.83318 0.00481 0.008 OSF Mean shift/esd = 0.001 Maximum = 0.008 for OSF Max. shift = 0.000 A for C2 Max. dU = 0.000 for O2 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1360 / 140606 wR2 = 0.0978 before cycle 5 for 1637 data and 109 / 109 parameters GooF = S = 1.086; Restrained GooF = 1.086 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0387 * P )^2 + 0.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.83318 0.00481 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z O2 Max. shift = 0.000 A for O2 Max. dU = 0.000 for C8 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1360 / 140606 wR2 = 0.0978 before cycle 6 for 1637 data and 109 / 109 parameters GooF = S = 1.086; Restrained GooF = 1.086 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0387 * P )^2 + 0.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.83319 0.00481 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C2 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C8 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.5602 0.5440 1.1796 43 0.950 0.000 C1 O1 C2 H4 0.6175 0.0688 1.1269 43 0.950 0.000 C4 C3 C2 H6 0.9880 -0.1673 0.7156 43 0.950 0.000 C6 C7 O3 H7 0.8879 -0.3791 0.8522 43 0.950 0.000 C7 C6 C8 H8 0.7469 -0.2216 1.0159 43 0.950 0.000 C8 C5 C7 2007may0012 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.55974 0.42477 1.18226 1.00000 0.02518 0.02361 0.02366 -0.00339 0.00107 0.00165 0.02422 0.00228 0.00015 0.00017 0.00012 0.00000 0.00061 0.00062 0.00061 0.00050 0.00048 0.00050 0.00028 H1 0.56024 0.54398 1.17961 1.00000 0.02906 0.00000 0.00000 C2 0.64465 0.33016 1.09152 1.00000 0.02247 0.02167 0.02005 -0.00094 0.00186 -0.00028 0.02140 0.00217 0.00015 0.00016 0.00011 0.00000 0.00059 0.00061 0.00059 0.00046 0.00046 0.00046 0.00028 C3 0.75119 0.13815 0.98297 1.00000 0.02152 0.01927 0.02010 0.00126 0.00174 -0.00228 0.02031 0.00216 0.00015 0.00015 0.00011 0.00000 0.00056 0.00059 0.00057 0.00045 0.00044 0.00045 0.00027 C4 0.66034 0.15483 1.07918 1.00000 0.02241 0.02060 0.02092 0.00100 0.00346 -0.00119 0.02122 0.00218 0.00015 0.00016 0.00011 0.00000 0.00058 0.00060 0.00058 0.00046 0.00046 0.00045 0.00027 H4 0.61751 0.06885 1.12687 1.00000 0.02546 0.00000 0.00000 C5 0.81050 -0.00798 0.92428 1.00000 0.01956 0.02369 0.01917 -0.00067 0.00386 -0.00157 0.02068 0.00218 0.00015 0.00016 0.00011 0.00000 0.00053 0.00061 0.00057 0.00047 0.00043 0.00047 0.00027 C6 0.93061 -0.14377 0.78467 1.00000 0.02604 0.02607 0.02783 -0.00568 0.00684 0.00247 0.02638 0.00244 0.00016 0.00017 0.00013 0.00000 0.00062 0.00065 0.00066 0.00052 0.00050 0.00051 0.00029 H6 0.98795 -0.16733 0.71556 1.00000 0.03165 0.00000 0.00000 C7 0.87625 -0.26095 0.85908 1.00000 0.02488 0.02263 0.03458 -0.00310 0.00643 0.00039 0.02714 0.00245 0.00016 0.00017 0.00013 0.00000 0.00063 0.00063 0.00073 0.00054 0.00053 0.00050 0.00030 H7 0.88793 -0.37914 0.85215 1.00000 0.03256 0.00000 0.00000 C8 0.79790 -0.17353 0.95015 1.00000 0.02431 0.02367 0.02709 0.00160 0.00612 -0.00132 0.02479 0.00239 0.00016 0.00017 0.00012 0.00000 0.00060 0.00062 0.00065 0.00051 0.00049 0.00049 0.00028 H8 0.74695 -0.22158 1.01591 1.00000 0.02975 0.00000 0.00000 N1 0.71901 0.41481 1.00998 1.00000 0.03279 0.02062 0.02672 -0.00104 0.00810 0.00121 0.02638 0.00208 0.00014 0.00014 0.00010 0.00000 0.00060 0.00054 0.00058 0.00043 0.00046 0.00045 0.00027 O1 0.48943 0.35473 1.26000 1.00000 0.02926 0.03006 0.02402 -0.00329 0.00614 0.00055 0.02755 0.00172 0.00012 0.00012 0.00008 0.00000 0.00049 0.00051 0.00047 0.00038 0.00037 0.00039 0.00024 O2 0.78812 0.29225 0.93918 1.00000 0.03146 0.01928 0.02450 0.00124 0.00995 -0.00070 0.02463 0.00168 0.00011 0.00011 0.00008 0.00000 0.00049 0.00045 0.00047 0.00035 0.00037 0.00036 0.00024 O3 0.89187 0.01457 0.82225 1.00000 0.02946 0.02273 0.02303 -0.00011 0.01000 0.00028 0.02461 0.00168 0.00011 0.00012 0.00008 0.00000 0.00047 0.00047 0.00046 0.00035 0.00036 0.00036 0.00023 Final Structure Factor Calculation for 2007may0012 in P2(1)/c Total number of l.s. parameters = 109 Maximum vector length = 511 Memory required = 1251 / 22995 wR2 = 0.0978 before cycle 7 for 1637 data and 0 / 109 parameters GooF = S = 1.085; Restrained GooF = 1.085 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0387 * P )^2 + 0.36 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0377 for 1487 Fo > 4sig(Fo) and 0.0430 for all 1637 data wR2 = 0.0978, GooF = S = 1.085, Restrained GooF = 1.085 for all data Occupancy sum of asymmetric unit = 12.00 for non-hydrogen and 5.00 for hydrogen atoms Principal mean square atomic displacements U 0.0285 0.0240 0.0202 C1 0.0226 0.0220 0.0196 C2 0.0233 0.0203 0.0174 C3 0.0233 0.0217 0.0186 C4 0.0245 0.0206 0.0170 C5 0.0330 0.0284 0.0177 C6 0.0361 0.0242 0.0211 C7 0.0295 0.0248 0.0201 C8 0.0355 0.0238 0.0198 N1 0.0319 0.0302 0.0206 O1 0.0355 0.0207 0.0177 O2 0.0339 0.0227 0.0172 O3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.019 0.037 0.056 0.076 0.099 0.125 0.163 0.217 0.317 1.000 Number in group 169. 167. 155. 167. 165. 163. 160. 168. 159. 164. GooF 1.218 1.128 1.332 0.976 1.105 1.065 0.927 1.017 0.975 1.058 K 1.692 1.014 0.937 0.960 1.004 0.997 0.996 1.006 1.013 1.003 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.14 1.31 1.62 inf Number in group 165. 163. 166. 164. 163. 164. 163. 162. 165. 162. GooF 1.182 0.988 0.988 1.075 0.910 0.905 0.769 0.964 1.263 1.587 K 1.026 1.014 1.008 1.008 1.017 0.999 0.993 1.006 1.029 0.991 R1 0.090 0.089 0.059 0.062 0.040 0.038 0.025 0.031 0.034 0.033 Recommended weighting scheme: WGHT 0.0351 0.3685 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 3 15.31 3.90 5.70 0.037 1.73 -1 2 4 66.83 93.99 4.00 0.184 2.22 -1 4 3 2.78 0.13 3.97 0.007 1.73 -2 2 2 46.68 65.82 3.51 0.154 2.60 -5 8 2 -0.15 4.84 3.50 0.042 0.85 -2 1 2 0.44 4.22 3.45 0.039 3.14 0 5 3 55.49 39.53 3.43 0.119 1.46 3 3 6 6.09 1.68 3.40 0.025 1.28 7 5 5 -0.87 4.51 3.29 0.040 0.84 -1 1 3 270.39 325.06 3.24 0.341 3.18 -3 3 6 60.05 44.46 3.14 0.126 1.36 0 1 4 10.64 18.85 3.12 0.082 2.60 -3 2 2 184.23 223.83 3.12 0.283 2.13 0 8 9 0.13 4.22 3.00 0.039 0.77 -1 7 5 20.29 30.71 2.94 0.105 1.01 -2 1 7 116.50 94.19 2.92 0.184 1.49 -3 7 3 2.48 6.77 2.89 0.049 1.02 -2 5 4 30.07 20.59 2.89 0.086 1.32 1 2 0 4.35 1.42 2.87 0.023 3.58 -1 4 2 517.43 447.84 2.87 0.401 1.84 -4 1 5 149.02 123.03 2.86 0.210 1.54 -4 3 4 27.60 18.67 2.85 0.082 1.44 -3 7 10 4.88 11.50 2.84 0.064 0.77 -2 3 2 203.71 171.10 2.82 0.248 2.10 9 1 6 3.30 0.42 2.71 0.012 0.78 -2 5 1 70.84 55.75 2.71 0.141 1.48 10 3 1 -1.24 1.69 2.68 0.025 0.77 1 7 7 24.14 34.25 2.61 0.111 0.91 -4 5 2 3.08 0.86 2.61 0.018 1.24 -1 5 3 39.81 29.52 2.59 0.103 1.45 -4 5 4 36.57 48.43 2.58 0.132 1.17 -2 5 6 94.79 115.49 2.57 0.204 1.17 -4 8 2 2.87 7.02 2.56 0.050 0.89 -3 6 9 1.95 0.11 2.53 0.006 0.87 -1 3 3 6.47 11.59 2.52 0.064 2.11 -2 5 11 -0.31 1.89 2.50 0.026 0.84 -8 1 7 8.52 14.41 2.50 0.072 0.89 4 2 0 68.95 85.57 2.49 0.175 1.81 0 3 2 73.56 90.24 2.46 0.180 2.39 -7 6 7 -0.44 2.08 2.45 0.027 0.79 -3 1 6 25.65 34.94 2.44 0.112 1.56 0 3 1 51.52 64.83 2.42 0.152 2.58 -2 0 6 412.86 363.35 2.41 0.361 1.73 -6 0 8 1.26 0.01 2.38 0.002 1.01 1 9 2 11.75 18.68 2.38 0.082 0.87 4 1 1 32.02 42.12 2.38 0.123 1.91 -1 7 8 3.28 0.82 2.34 0.017 0.88 -7 6 4 -0.56 0.93 2.31 0.018 0.85 -2 1 5 263.08 230.73 2.30 0.288 1.95 3 1 13 6.96 12.61 2.30 0.067 0.78 Bond lengths and angles C1 - Distance Angles O1 1.2117 (0.0016) C2 1.4766 (0.0017) 121.90 (0.12) H1 0.9500 119.05 119.05 C1 - O1 C2 C2 - Distance Angles N1 1.3170 (0.0016) C4 1.4101 (0.0017) 112.91 (0.11) C1 1.4766 (0.0017) 118.52 (0.12) 128.57 (0.12) C2 - N1 C4 C3 - Distance Angles C4 1.3571 (0.0017) O2 1.3631 (0.0015) 110.13 (0.11) C5 1.4376 (0.0017) 131.55 (0.12) 118.32 (0.10) C3 - C4 O2 C4 - Distance Angles C3 1.3571 (0.0017) C2 1.4101 (0.0017) 103.51 (0.11) H4 0.9500 128.25 128.25 C4 - C3 C2 C5 - Distance Angles C8 1.3552 (0.0018) O3 1.3714 (0.0014) 110.65 (0.11) C3 1.4376 (0.0017) 131.10 (0.12) 118.23 (0.11) C5 - C8 O3 C6 - Distance Angles C7 1.3456 (0.0019) O3 1.3737 (0.0016) 110.74 (0.11) H6 0.9500 124.63 124.63 C6 - C7 O3 C7 - Distance Angles C6 1.3456 (0.0019) C8 1.4225 (0.0018) 106.70 (0.12) H7 0.9500 126.65 126.65 C7 - C6 C8 C8 - Distance Angles C5 1.3552 (0.0018) C7 1.4225 (0.0018) 106.22 (0.12) H8 0.9500 126.89 126.89 C8 - C5 C7 N1 - Distance Angles C2 1.3170 (0.0016) O2 1.4012 (0.0014) 105.03 (0.10) N1 - C2 O1 - Distance Angles C1 1.2117 (0.0016) O1 - O2 - Distance Angles C3 1.3631 (0.0015) N1 1.4012 (0.0014) 108.41 (0.09) O2 - C3 O3 - Distance Angles C5 1.3714 (0.0014) C6 1.3737 (0.0016) 105.69 (0.10) O3 - C5 FMAP and GRID set by program FMAP 2 2 12 GRID -2.778 -2 -2 2.778 2 2 R1 = 0.0430 for 1637 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.24 at 0.6130 0.1210 0.6383 [ 0.71 A from C2 ] Deepest hole -0.22 at 0.0143 0.2129 0.2891 [ 0.37 A from H6 ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 1416 / 14190 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6130 0.3790 1.1383 1.00000 0.05 0.24 0.71 C2 0.77 C1 1.47 H1 1.75 N1 Q2 1 0.8000 0.0583 0.9623 1.00000 0.05 0.23 0.69 C5 0.79 C3 1.81 O3 1.85 C8 Q3 1 0.9945 -0.1063 0.6990 1.00000 0.05 0.23 0.52 H6 1.16 C6 1.92 O3 2.15 H7 Q4 1 0.6635 0.2482 1.0961 1.00000 0.05 0.23 0.67 C2 0.77 C4 1.52 H4 1.72 N1 Q5 1 0.7537 -0.0841 0.9241 1.00000 0.05 0.22 0.76 C5 0.84 C8 1.50 H8 1.84 O3 Q6 1 0.7258 0.1311 1.0431 1.00000 0.05 0.21 0.72 C3 0.72 C4 1.43 H4 1.82 C2 Q7 1 0.8543 -0.2042 0.7998 1.00000 0.05 0.20 0.80 C7 0.82 C6 1.52 H7 1.53 H6 Q8 1 0.9419 -0.2012 0.8461 1.00000 0.05 0.20 0.74 C7 0.82 C6 1.49 H7 1.55 H6 Q9 1 0.6837 0.1324 1.0211 1.00000 0.05 0.19 0.71 C4 0.72 C3 1.42 H4 1.80 C2 Q10 1 0.8795 -0.2211 0.9310 1.00000 0.05 0.19 0.81 C8 0.85 C7 1.50 H8 1.54 H7 Shortest distances between peaks (including symmetry equivalents) 6 9 0.40 7 8 0.84 8 10 1.12 1 4 1.23 4 6 1.23 2 5 1.26 4 9 1.26 2 6 1.26 2 9 1.33 7 10 1.45 5 10 1.50 3 7 1.84 3 8 1.88 5 7 1.92 5 8 2.05 5 9 2.13 5 6 2.18 2 10 2.35 1 9 2.45 2 4 2.45 1 6 2.46 2 8 2.74 2 7 2.82 6 8 2.93 3 10 2.95 Time profile in seconds ----------------------- 0.12: 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 0.01: Analyse other restraints etc. 1.25: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.44: Structure factors and derivatives 0.71: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.15: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.04: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.01: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007may0012 finished at 15:39:50 Total CPU time: 2.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++