+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007sot0277 started at 08:01:40 on 27-Feb-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007sot0277 in C2/c CELL 0.71073 11.0540 11.9883 11.2576 90.000 96.475 90.000 ZERR 4.00 0.0003 0.0004 0.0004 0.000 0.002 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H F N SI UNIT 40 72 24 16 4 V = 1482.33 F(000) = 696.0 Mu = 0.22 mm-1 Cell Wt = 1345.50 Rho = 1.507 shel 7 0.77 OMIT 2 0 0 TEMP -153 ACTA 55 SIZE 0.2 0.2 0.1 FMAP 2 PLAN 10 L.S. 4 WGHT 0.031400 3.520500 FVAR 0.45450 SI1 5 0.250000 0.250000 0.500000 10.50000 0.01596 0.01602 = 0.01428 -0.00072 0.00094 0.00244 F1 3 0.331021 0.158919 0.426716 11.00000 0.02185 0.02068 = 0.01997 -0.00090 0.00422 0.00339 F2 3 0.285586 0.178090 0.628034 11.00000 0.03122 0.02568 = 0.01763 0.00309 0.00231 0.00835 F3 3 0.124620 0.169144 0.468461 11.00000 0.01943 0.02524 = 0.03142 -0.00501 0.00303 -0.00182 N1 4 0.367008 0.114752 0.988020 11.00000 0.01809 0.01992 = 0.01758 0.00126 0.00341 0.00258 N2 4 0.241782 0.106915 1.121585 11.00000 0.01900 0.02148 = 0.01881 0.00135 0.00413 0.00184 C1 1 0.426806 0.090344 0.880961 11.00000 0.02187 0.02849 = 0.01806 0.00079 0.00707 0.00123 C2 1 0.398109 0.199852 1.068521 11.00000 0.01731 0.02123 = 0.02103 -0.00026 -0.00024 0.00045 C3 1 0.319669 0.194996 1.152108 11.00000 0.02128 0.02326 = 0.01792 -0.00251 0.00136 0.00058 C4 1 0.272066 0.060318 1.022117 11.00000 0.02035 0.01711 = 0.01893 0.00107 0.00364 0.00162 C5 1 0.139847 0.071575 1.185432 11.00000 0.02251 0.03440 = 0.02494 0.00249 0.00923 -0.00199 H1 2 0.508394 0.112018 0.894153 11.00000 0.02880 H2 2 0.387616 0.128589 0.815647 11.00000 0.02506 H4 2 0.461687 0.245894 1.058070 11.00000 0.04016 H7 2 0.065627 0.099239 1.140934 11.00000 0.03495 H3 2 0.421002 0.014576 0.868154 11.00000 0.03825 H5 2 0.314298 0.234872 1.219382 11.00000 0.03261 H9 2 0.152022 0.096625 1.264232 11.00000 0.04236 H8 2 0.136544 -0.008035 1.183756 11.00000 0.05054 H6 2 0.235966 0.002475 0.986604 11.00000 0.02609 HKLF 4 1.0 -1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 -1.00 Covalent radii and connectivity table for 2007sot0277 in C2/c C 0.770 H 0.320 F 0.640 N 0.700 SI 1.170 Si1 - F1 F1_$1 F2_$1 F2 F3_$1 F3 F1 - Si1 F2 - Si1 F3 - Si1 N1 - C4 C2 C1 N2 - C4 C3 C5 C1 - N1 C2 - C3 N1 C3 - C2 N2 C4 - N2 N1 C5 - N2 Operators for generating equivalent atoms: $1 -x+1/2, -y+1/2, -z+1 h k l Fo^2 Sigma Why rejected -5 0 0 3.48 0.85 observed but should be systematically absent -5 0 0 5.46 1.33 observed but should be systematically absent -7 0 0 20.77 4.75 observed but should be systematically absent 1 2 0 45.74 3.11 observed but should be systematically absent -1 2 0 54.74 7.83 observed but should be systematically absent 1 -2 0 45.73 3.66 observed but should be systematically absent 1 2 0 56.15 4.31 observed but should be systematically absent -1 -2 0 62.20 8.11 observed but should be systematically absent 3 2 0 45.94 10.01 observed but should be systematically absent -3 -2 0 39.24 8.74 observed but should be systematically absent -3 -4 0 33.47 7.23 observed but should be systematically absent 3 -4 0 29.38 4.77 observed but should be systematically absent 2 -1 1 109.73 8.20 observed but should be systematically absent -2 1 -1 123.87 14.27 observed but should be systematically absent 4 1 1 60.41 11.63 observed but should be systematically absent 4 1 1 40.57 7.96 observed but should be systematically absent -2 3 1 17.28 3.98 observed but should be systematically absent 2 3 -1 21.10 4.73 observed but should be systematically absent 2 3 -1 30.41 7.23 observed but should be systematically absent 2 -3 -1 32.96 7.48 observed but should be systematically absent 0 -3 -1 29.34 2.93 observed but should be systematically absent 0 -3 1 39.52 6.79 observed but should be systematically absent 0 3 -1 26.64 3.39 observed but should be systematically absent 0 3 1 36.18 5.21 observed but should be systematically absent -2 3 -1 18.83 3.67 observed but should be systematically absent -2 3 -1 22.95 3.82 observed but should be systematically absent 2 -3 1 17.76 1.91 observed but should be systematically absent -2 3 -1 19.02 2.83 observed but should be systematically absent 4 -3 1 83.53 12.57 observed but should be systematically absent 4 3 1 110.23 25.65 observed but should be systematically absent -2 5 1 17.41 3.45 observed but should be systematically absent 2 -5 -1 22.97 4.30 observed but should be systematically absent 4 -5 1 13.25 2.53 observed but should be systematically absent 4 5 1 14.44 2.90 observed but should be systematically absent -2 7 -1 36.75 7.04 observed but should be systematically absent 2 7 1 21.52 3.37 observed but should be systematically absent 2 -7 1 32.91 4.24 observed but should be systematically absent -2 7 -1 34.21 6.12 observed but should be systematically absent -2 -7 -1 22.86 5.12 observed but should be systematically absent 2 9 1 19.06 4.05 observed but should be systematically absent -1 -2 2 14.24 3.37 observed but should be systematically absent -1 2 -2 268.48 40.50 observed but should be systematically absent 1 2 2 277.84 26.63 observed but should be systematically absent -1 2 -2 276.07 21.88 observed but should be systematically absent 1 -2 2 223.16 24.18 observed but should be systematically absent -1 2 -2 238.40 19.94 observed but should be systematically absent 1 -2 2 235.16 19.76 observed but should be systematically absent -3 2 -2 192.02 31.15 observed but should be systematically absent 3 2 2 256.41 28.56 observed but should be systematically absent 3 -2 2 255.13 23.29 observed but should be systematically absent ** etc. ** 18233 Reflections read, of which 9031 rejected -13 =< h =< 14, -15 =< k =< 13, -14 =< l =< 14, Max. 2-theta = 54.96 154 Systematic absence violations 0 Inconsistent equivalents 1703 Unique reflections, of which 0 suppressed R(int) = 0.0436 R(sigma) = 0.0357 Friedel opposites merged Maximum memory for data reduction = 1228 / 20251 Special position constraints for Si1 x = 0.2500 y = 0.2500 z = 0.5000 sof = 0.50000 Input constraints retained (at least in part) for sof Least-squares cycle 1 Maximum vector length = 511 Memory required = 1544 / 169120 wR2 = 0.1000 before cycle 1 for 1703 data and 133 / 133 parameters GooF = S = 1.051; Restrained GooF = 1.051 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0314 * P )^2 + 3.52 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45450 0.00115 0.003 OSF Mean shift/esd = 0.002 Maximum = 0.011 for U23 Si1 Max. shift = 0.000 A for H8 Max. dU = 0.000 for H5 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1544 / 169120 wR2 = 0.1000 before cycle 2 for 1703 data and 133 / 133 parameters GooF = S = 1.051; Restrained GooF = 1.051 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0314 * P )^2 + 3.52 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45450 0.00115 0.001 OSF Mean shift/esd = 0.001 Maximum = 0.004 for U23 Si1 Max. shift = 0.000 A for H8 Max. dU = 0.000 for H5 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1544 / 169120 wR2 = 0.1000 before cycle 3 for 1703 data and 133 / 133 parameters GooF = S = 1.051; Restrained GooF = 1.051 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0314 * P )^2 + 3.52 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45450 0.00115 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C4 Max. shift = 0.000 A for H8 Max. dU = 0.000 for H8 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1544 / 169120 wR2 = 0.1000 before cycle 4 for 1703 data and 133 / 133 parameters GooF = S = 1.051; Restrained GooF = 1.051 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0314 * P )^2 + 3.52 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.45450 0.00115 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for H8 Max. dU = 0.000 for H9 No correlation matrix elements larger than 0.500 2007sot0277 in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Si1 0.25000 0.25000 0.50000 0.50000 0.01596 0.01602 0.01428 -0.00072 0.00094 0.00244 0.01548 0.00000 0.00000 0.00000 0.00000 0.00000 0.00035 0.00036 0.00034 0.00026 0.00025 0.00025 0.00019 F1 0.33102 0.15892 0.42672 1.00000 0.02185 0.02068 0.01997 -0.00090 0.00422 0.00339 0.02069 0.00197 0.00010 0.00009 0.00010 0.00000 0.00057 0.00058 0.00057 0.00043 0.00042 0.00043 0.00027 F2 0.28559 0.17809 0.62803 1.00000 0.03122 0.02568 0.01763 0.00309 0.00231 0.00835 0.02488 0.00214 0.00011 0.00010 0.00010 0.00000 0.00064 0.00063 0.00057 0.00045 0.00045 0.00048 0.00029 F3 0.12462 0.16914 0.46846 1.00000 0.01943 0.02524 0.03142 -0.00501 0.00303 -0.00182 0.02535 0.00204 0.00010 0.00010 0.00011 0.00000 0.00057 0.00062 0.00065 0.00048 0.00046 0.00045 0.00029 N1 0.36701 0.11475 0.98802 1.00000 0.01809 0.01992 0.01758 0.00126 0.00341 0.00258 0.01843 0.00286 0.00014 0.00013 0.00014 0.00000 0.00076 0.00081 0.00076 0.00061 0.00058 0.00061 0.00034 N2 0.24178 0.10692 1.12159 1.00000 0.01900 0.02148 0.01881 0.00135 0.00413 0.00184 0.01961 0.00292 0.00014 0.00014 0.00014 0.00000 0.00079 0.00084 0.00079 0.00063 0.00060 0.00061 0.00035 C1 0.42681 0.09034 0.88096 1.00000 0.02187 0.02849 0.01806 0.00079 0.00707 0.00123 0.02244 0.00397 0.00019 0.00019 0.00018 0.00000 0.00101 0.00112 0.00095 0.00079 0.00075 0.00081 0.00042 C2 0.39811 0.19985 1.06852 1.00000 0.01731 0.02123 0.02103 -0.00026 -0.00024 0.00045 0.02004 0.00343 0.00017 0.00016 0.00017 0.00000 0.00090 0.00095 0.00093 0.00075 0.00069 0.00074 0.00039 C3 0.31967 0.19500 1.15211 1.00000 0.02128 0.02326 0.01792 -0.00251 0.00136 0.00058 0.02089 0.00350 0.00017 0.00017 0.00017 0.00000 0.00093 0.00099 0.00093 0.00075 0.00070 0.00074 0.00040 C4 0.27207 0.06032 1.02212 1.00000 0.02035 0.01711 0.01893 0.00107 0.00364 0.00162 0.01869 0.00360 0.00017 0.00016 0.00017 0.00000 0.00091 0.00094 0.00091 0.00072 0.00068 0.00073 0.00038 C5 0.13985 0.07157 1.18543 1.00000 0.02251 0.03440 0.02494 0.00249 0.00923 -0.00199 0.02678 0.00430 0.00019 0.00021 0.00020 0.00000 0.00101 0.00125 0.00107 0.00090 0.00081 0.00086 0.00045 H1 0.50839 0.11202 0.89415 1.00000 0.02880 0.04610 0.00237 0.00204 0.00215 0.00000 0.00624 H2 0.38762 0.12859 0.81565 1.00000 0.02506 0.04271 0.00216 0.00207 0.00220 0.00000 0.00585 H4 0.46169 0.24589 1.05807 1.00000 0.04016 0.05033 0.00258 0.00231 0.00239 0.00000 0.00734 H7 0.06563 0.09924 1.14093 1.00000 0.03495 0.04709 0.00246 0.00216 0.00236 0.00000 0.00680 H3 0.42100 0.01458 0.86815 1.00000 0.03825 0.05050 0.00241 0.00253 0.00237 0.00000 0.00719 H5 0.31430 0.23487 1.21938 1.00000 0.03261 0.04719 0.00231 0.00217 0.00237 0.00000 0.00657 H9 0.15202 0.09662 1.26423 1.00000 0.04236 0.05283 0.00248 0.00233 0.00268 0.00000 0.00760 H8 0.13655 -0.00804 1.18376 1.00000 0.05054 0.05608 0.00270 0.00282 0.00262 0.00000 0.00836 H6 0.23596 0.00247 0.98660 1.00000 0.02609 0.04652 0.00215 0.00219 0.00210 0.00000 0.00612 Final Structure Factor Calculation for 2007sot0277 in C2/c Total number of l.s. parameters = 133 Maximum vector length = 511 Memory required = 1411 / 24017 wR2 = 0.1000 before cycle 5 for 1703 data and 0 / 133 parameters GooF = S = 1.051; Restrained GooF = 1.051 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0314 * P )^2 + 3.52 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0435 for 1485 Fo > 4sig(Fo) and 0.0523 for all 1703 data wR2 = 0.1000, GooF = S = 1.051, Restrained GooF = 1.051 for all data Occupancy sum of asymmetric unit = 10.50 for non-hydrogen and 9.00 for hydrogen atoms Principal mean square atomic displacements U 0.0188 0.0141 0.0135 Si1 0.0248 0.0209 0.0164 F1 0.0373 0.0213 0.0160 F2 0.0342 0.0230 0.0189 F3 0.0223 0.0171 0.0159 N1 0.0233 0.0189 0.0166 N2 0.0289 0.0242 0.0142 C1 0.0227 0.0211 0.0164 C2 0.0246 0.0211 0.0169 C3 0.0218 0.0179 0.0164 C4 0.0351 0.0296 0.0156 C5 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.014 0.027 0.041 0.057 0.071 0.089 0.113 0.146 0.217 1.000 Number in group 178. 167. 170. 179. 162. 170. 170. 167. 170. 170. GooF 1.076 1.245 1.040 1.124 1.052 1.049 0.990 0.945 0.982 0.969 K 2.182 1.193 1.036 0.989 0.983 0.998 1.014 1.004 1.009 1.002 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 173. 168. 176. 168. 166. 170. 174. 167. 170. 171. GooF 1.172 1.056 1.118 1.049 0.973 0.981 0.883 0.846 1.152 1.209 K 1.037 1.035 1.057 0.984 1.004 0.999 0.996 1.010 1.018 0.992 R1 0.129 0.093 0.094 0.082 0.062 0.046 0.034 0.031 0.032 0.028 Recommended weighting scheme: WGHT 0.0219 3.7815 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) 7 7 5 34.63 3.71 3.47 0.009 0.99 -5 3 5 71.39 26.09 3.30 0.024 1.54 -6 2 2 509.65 691.28 3.27 0.121 1.72 2 8 0 66.48 25.06 3.15 0.023 1.45 -6 12 6 154.81 256.67 2.89 0.074 0.81 -4 10 9 48.51 0.86 2.87 0.004 0.84 2 4 0 89.07 46.28 2.79 0.031 2.63 -2 14 1 304.46 185.57 2.77 0.063 0.84 0 6 2 194.39 283.75 2.75 0.078 1.88 0 0 12 52.28 5.57 2.71 0.011 0.93 4 12 2 77.66 147.67 2.70 0.056 0.92 3 11 1 52.68 14.34 2.69 0.017 1.04 6 6 11 -8.72 21.81 2.68 0.021 0.78 0 4 7 303.46 411.46 2.64 0.093 1.41 -5 5 3 1174.70 1396.73 2.64 0.172 1.53 6 10 2 22.20 61.09 2.61 0.036 0.98 -2 2 6 660.04 822.07 2.60 0.132 1.75 -1 3 3 50.61 18.71 2.58 0.020 2.70 -1 13 8 49.74 8.33 2.54 0.013 0.77 3 15 0 64.80 15.95 2.51 0.018 0.78 0 14 0 1437.98 1094.90 2.50 0.152 0.86 2 10 6 67.45 122.50 2.49 0.051 0.98 -6 4 9 79.69 133.85 2.41 0.053 1.02 -4 6 12 223.03 146.51 2.39 0.056 0.83 0 12 3 67.56 28.87 2.39 0.025 0.96 3 11 9 240.70 152.68 2.36 0.057 0.79 3 15 2 209.70 129.93 2.35 0.052 0.77 6 4 0 788.29 945.04 2.35 0.141 1.56 9 11 2 -3.80 45.95 2.35 0.031 0.80 -11 5 8 37.53 2.36 2.33 0.007 0.81 2 0 4 1280.88 1073.74 2.32 0.151 2.39 1 1 2 9405.51 10340.23 2.31 0.468 4.43 -6 12 2 52.85 100.41 2.30 0.046 0.87 1 5 8 334.20 252.24 2.29 0.073 1.19 13 1 3 551.98 411.94 2.29 0.093 0.80 0 4 6 611.23 747.96 2.28 0.126 1.58 8 0 2 692.62 562.30 2.28 0.109 1.30 -13 1 1 138.68 214.80 2.27 0.067 0.85 -3 3 6 42.53 17.75 2.26 0.019 1.60 7 3 6 -2.31 10.04 2.25 0.015 1.10 -6 4 13 479.39 362.25 2.24 0.088 0.79 -3 5 5 1039.44 1212.85 2.24 0.160 1.54 5 3 5 547.76 440.96 2.22 0.097 1.39 -13 5 5 702.07 448.57 2.20 0.097 0.78 5 5 6 651.21 779.29 2.19 0.128 1.18 -2 12 3 63.95 24.70 2.18 0.023 0.96 2 2 11 29.21 8.12 2.17 0.013 0.97 8 12 3 239.67 150.92 2.16 0.057 0.78 -4 8 12 166.04 99.46 2.15 0.046 0.78 0 2 8 138.89 196.91 2.13 0.065 1.36 Bond lengths and angles Si1 - Distance Angles F1 1.6857 (0.0011) F1_$1 1.6857 (0.0011) 180.00 (0.06) F2_$1 1.6875 (0.0011) 89.91 (0.05) 90.09 (0.05) F2 1.6875 (0.0011) 90.09 (0.05) 89.91 (0.05) 180.00 F3_$1 1.6957 (0.0011) 90.34 (0.05) 89.66 (0.05) 89.61 (0.06) 90.39 (0.06) F3 1.6957 (0.0011) 89.66 (0.05) 90.34 (0.05) 90.39 (0.06) 89.61 (0.06) 180.00 (0.08) Si1 - F1 F1_$1 F2_$1 F2 F3_$1 F1 - Distance Angles Si1 1.6857 (0.0011) F1 - F2 - Distance Angles Si1 1.6875 (0.0011) F2 - F3 - Distance Angles Si1 1.6957 (0.0011) F3 - N1 - Distance Angles C4 1.3287 (0.0024) C2 1.3820 (0.0025) 108.62 (0.16) C1 1.4679 (0.0024) 125.65 (0.17) 125.72 (0.17) N1 - C4 C2 N2 - Distance Angles C4 1.3276 (0.0025) C3 1.3812 (0.0026) 108.79 (0.16) C5 1.4657 (0.0024) 124.95 (0.18) 126.23 (0.17) N2 - C4 C3 C1 - Distance Angles N1 1.4679 (0.0024) C1 - C2 - Distance Angles C3 1.3508 (0.0028) N1 1.3820 (0.0025) 107.05 (0.17) C2 - C3 C3 - Distance Angles C2 1.3508 (0.0028) N2 1.3812 (0.0026) 106.90 (0.17) C3 - C2 C4 - Distance Angles N2 1.3276 (0.0025) N1 1.3287 (0.0024) 108.63 (0.17) C4 - N2 C5 - Distance Angles N2 1.4657 (0.0024) C5 - FMAP and GRID set by program FMAP 2 1 15 GRID -2.083 -1 -2 2.083 1 2 R1 = 0.0522 for 1703 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.28 at 0.2206 0.1714 0.3591 [ 1.37 A from F1 ] Deepest hole -0.25 at 0.1868 0.2689 0.4656 [ 0.79 A from SI1 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 1709 / 19077 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2206 0.1714 0.3591 1.00000 0.05 0.28 1.37 F1 1.53 H9 1.71 F3 1.81 F2 Q2 1 0.2038 0.1801 0.5669 1.00000 0.05 0.27 1.07 F2 1.27 SI1 1.34 F3 1.97 F1 Q3 1 0.3783 0.1676 1.1306 1.00000 0.05 0.25 0.79 C3 0.85 C2 1.52 H5 1.60 H4 Q4 1 0.0897 0.1271 1.2002 1.00000 0.05 0.25 0.77 H7 0.89 C5 1.01 H9 1.72 H8 Q5 1 0.3527 0.1779 0.5761 1.00000 0.05 0.24 1.00 F2 1.60 SI1 1.69 F1 1.73 H1 Q6 1 0.2700 0.1551 1.1321 1.00000 0.05 0.24 0.66 N2 0.74 C3 1.42 H5 1.68 C4 Q7 1 0.3850 0.1613 1.0134 1.00000 0.05 0.23 0.65 N1 0.77 C2 1.38 H4 1.75 C4 Q8 1 0.2315 0.0988 1.0537 1.00000 0.05 0.23 0.76 C4 0.77 N2 1.38 H6 1.75 N1 Q9 1 0.4005 0.1429 1.0341 1.00000 0.05 0.23 0.69 N1 0.79 C2 1.42 H4 1.72 C4 Q10 1 0.3304 0.1381 0.7842 1.00000 0.05 0.22 0.70 H2 1.55 C1 1.83 F2 1.97 H3 Shortest distances between peaks (including symmetry equivalents) 7 9 0.35 6 8 1.15 3 9 1.18 3 6 1.21 3 7 1.33 2 5 1.64 6 9 1.92 3 8 1.94 6 7 1.95 7 8 1.95 8 9 1.98 1 2 2.10 1 5 2.14 1 4 2.23 4 6 2.24 1 2 2.37 2 5 2.38 4 4 2.39 4 8 2.42 5 10 2.43 2 2 2.54 7 10 2.60 1 6 2.68 1 5 2.70 2 10 2.72 1 10 2.82 9 10 2.83 6 10 2.91 4 10 2.95 Time profile in seconds ----------------------- 0.50: 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 0.02: 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. 13.77: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.05: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.53: Structure factors and derivatives 0.77: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.64: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.11: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007sot0277 finished at 08:02:09 Total CPU time: 16.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++