+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXS-97 - CRYSTAL STRUCTURE SOLUTION - WinGX VERSION + + Copyright(C) George M. Sheldrick 1986-97 Release 97-2 + + s92 started at 16:17:45 on 03 Aug 2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01SOT013 in Cc CELL 0.71073 25.5294 18.9718 9.7130 90 103.111 90 ZERR 8 0.0005 0.0005 0.0002 0 0.002 0 LATT -7 SYMM X, -Y, 1/2+Z SFAC C H N O UNIT 208 248 24 16 V = 4581.75 At vol = 18.5 F(000) = 1792.0 mu = 0.08 mm-1 Max single Patterson vector = 6.4 cell wt = 3340.30 rho = 1.211 OMIT 4.00 180.00 ESEL 1.200 5.000 0.005 0.700 0 TREF HKLF 4 h k l F*F Sigma Why Rejected -2.00 0.00 -1.00 1.02 0.23 Observed but should be systematically absent -2.00 0.00 -1.00 2.82 0.40 Observed but should be systematically absent 24093 Reflections read, of which 311 rejected Maximum h, k, l and 2-Theta = 33. 24. 12. 54.96 INCONSISTENT EQUIVALENTS h k l F*F Sigma(F*F) Esd of mean(F*F) -3 1 2 406.08 7.95 55.74 -1 1 2 706.82 16.44 98.39 -5 1 3 145.41 3.22 18.04 -7 1 4 49.07 0.36 25.05 -6 2 4 20.20 0.35 2.46 -9 1 5 97.09 0.51 100.66 -5 3 5 48.57 0.44 140.01 -3 3 5 77.81 0.43 17.04 -11 3 6 127.86 2.45 17.27 -2 4 6 76.54 0.43 11.53 -4 6 6 23.35 0.37 2.58 0 6 7 58.74 0.78 6.47 -16 2 8 102.97 0.73 39.46 -14 4 8 56.13 0.68 9.40 -15 5 8 190.53 1.67 66.03 -2 8 8 31.05 0.62 3.11 1 9 9 45.94 1.06 5.99 5193 Unique reflections, of which 3986 observed R(int) = 0.0914 R(sigma) = 0.0701 Friedel opposites merged NUMBER OF UNIQUE DATA AS A FUNCTION OF RESOLUTION IN ANGSTROMS Resolution Inf 5.00 3.50 2.50 2.00 1.70 1.50 1.40 1.30 1.20 1.10 1.00 0.90 0.80 N(observed) 11. 37. 93. 151. 180. 228. 154. 212. 281. 404. 535. 729. 791. N(measured) 11. 37. 93. 153. 182. 231. 158. 219. 291. 430. 581. 899. 1386. N(theory) 18. 39. 94. 154. 182. 231. 158. 219. 291. 430. 581. 899. 1390. Two-theta 0.0 8.2 11.7 16.3 20.5 24.1 27.4 29.4 31.7 34.5 37.7 41.6 46.5 52.7 Highest memory for sort/merge = 21576 / 25965 Observed E .GT. 1.200 1.300 1.400 1.500 1.600 1.700 1.800 1.900 2.000 2.100 Number 1347 1151 957 804 675 537 455 372 304 251 Centric Acentric 0kl h0l hk0 Rest Mean Abs(E*E-1) 0.968 0.736 0.874 0.933 0.895 0.909 0.2 seconds CPU time SUMMARY OF PARAMETERS FOR 01SOT013 in Cc ESEL Emin 1.200 Emax 5.000 DelU 0.005 renorm 0.700 axis 0 OMIT s 4.00 2theta(lim) 180.0 INIT nn 17 nf 16 s+ 0.800 s- 0.200 wr 0.200 PHAN steps 10 cool 0.900 Boltz 0.300 ns 336 mtpr 40 mnqr 10 TREF np 256. nE 510 kapscal 0.800 ntan 3 wn -0.470 FMAP code 8 PLAN npeaks -85 del1 0.500 del2 1.500 MORE verbosity 1 TIME t 9999999. 336 Reflections and 5398. unique TPR for phase annealing 510 Phases refined using 18467. unique TPR 606 Reflections and 25845. unique TPR for R(alpha) 0.2 seconds CPU time 36591 Unique negative quartets found, 4488 used for phase refinement 0.3 seconds CPU time Highest memory used to derive phase relations = 8148 / 85476 ONE-PHASE SEMINVARIANTS h k l E P+ Phi 0 14 0 2.280 0.00 0 8 0 1.853 0.44 Expected value of Sigma-1 = 0.956 Following phases held constant with unit weights for the initial 4 weighted tangent cycles (before phase annealing): h k l E Phase/Comment 6 2 0 3.409 random phase -4 2 2 2.602 random phase -1 1 3 2.650 random phase 3 3 2 2.241 random phase 0 4 1 2.405 random phase 5 1 7 3.139 random phase 3 1 5 2.473 random phase -6 6 2 2.269 random phase 5 1 5 2.401 random phase -9 7 2 2.635 random phase 9 1 0 2.099 random phase 0 14 0 2.280 180 sigma-1 = 0.004 -7 7 3 2.144 random phase 5 3 0 1.968 random phase -5 3 1 2.057 random phase -3 7 5 2.042 random phase -3 3 2 1.855 random phase -9 3 5 2.100 random phase All other phases random with initial weights of 0.200 replaced by 0.2*alpha (or 1 if less) during first 4 cycles - unit weights for all phases thereafter 875 Unique NQR employed in phase annealing 128 Parallel refinements, highest memory = 19530 / 157691 0.0 seconds CPU time STRUCTURE SOLUTION for 01SOT013 in Cc Phase annealing cycle: 1 Beta = 0.15633 Ralpha 0.091 0.127 0.102 0.175 0.167 0.141 0.180 0.136 0.107 0.200 0.095 0.086 0.136 0.194 0.156 0.116 0.106 0.088 0.068 0.099 Nqual 0.158 0.038 0.119-0.019-0.067 0.131-0.211 0.212 0.266-0.127 0.216-0.375-0.216-0.261-0.035 0.145-0.129-0.243-0.468 0.006 Mabs 1.018 0.986 0.956 0.804 0.815 0.875 0.817 0.979 1.030 0.761 1.061 1.065 0.882 0.782 0.903 0.983 0.969 1.045 1.109 1.087 Phase annealing cycle: 2 Beta = 0.17370 Ralpha 0.099 0.148 0.129 0.288 0.236 0.188 0.242 0.148 0.111 0.309 0.086 0.065 0.158 0.280 0.195 0.120 0.122 0.071 0.058 0.098 Nqual -0.294-0.253-0.076-0.370-0.206-0.037-0.384-0.151-0.062-0.327-0.087-0.594-0.449-0.450-0.222-0.140-0.355-0.464-0.605-0.263 Mabs 0.918 0.861 0.877 0.704 0.747 0.797 0.736 0.862 0.915 0.692 0.969 1.031 0.813 0.709 0.814 0.905 0.875 1.005 1.044 0.958 Phase annealing cycle: 3 Beta = 0.19299 Ralpha 0.091 0.123 0.113 0.232 0.182 0.168 0.220 0.145 0.111 0.253 0.080 0.055 0.147 0.251 0.159 0.108 0.113 0.052 0.054 0.099 Nqual -0.362-0.254-0.068-0.346-0.139-0.039-0.430-0.231-0.088-0.363-0.161-0.633-0.431-0.414-0.315-0.182-0.473-0.565-0.641-0.363 Mabs 0.941 0.898 0.918 0.748 0.805 0.824 0.752 0.870 0.946 0.723 1.001 1.043 0.837 0.734 0.841 0.910 0.905 1.057 1.067 0.965 Phase annealing cycle: 4 Beta = 0.21444 Ralpha 0.092 0.117 0.101 0.163 0.149 0.120 0.193 0.137 0.096 0.240 0.073 0.059 0.133 0.205 0.141 0.099 0.112 0.052 0.053 0.093 Nqual -0.329-0.237-0.008-0.240-0.120-0.106-0.347-0.155-0.089-0.359-0.200-0.621-0.454-0.430-0.297-0.220-0.422-0.640-0.634-0.382 Mabs 0.953 0.927 0.959 0.834 0.882 0.911 0.787 0.895 0.973 0.734 1.011 1.080 0.862 0.783 0.869 0.932 0.917 1.067 1.068 0.986 Phase annealing cycle: 5 Beta = 0.23827 Ralpha 0.089 0.124 0.101 0.113 0.124 0.087 0.182 0.128 0.093 0.204 0.061 0.057 0.127 0.142 0.135 0.090 0.101 0.049 0.051 0.091 Nqual -0.399-0.337-0.057-0.152-0.191-0.499-0.240-0.108-0.182-0.438-0.227-0.612-0.399-0.436-0.352-0.325-0.456-0.665-0.626-0.444 Mabs 0.974 0.898 0.965 0.927 0.919 0.976 0.797 0.894 0.979 0.766 1.023 1.085 0.873 0.861 0.888 0.941 0.948 1.063 1.077 0.982 Phase annealing cycle: 6 Beta = 0.26474 Ralpha 0.087 0.125 0.103 0.105 0.116 0.054 0.175 0.129 0.088 0.189 0.064 0.057 0.120 0.083 0.133 0.090 0.107 0.055 0.054 0.092 Nqual -0.454-0.366-0.101-0.104-0.218-0.597-0.322-0.230-0.208-0.386-0.306-0.613-0.362-0.545-0.304-0.370-0.480-0.637-0.665-0.491 Mabs 0.980 0.895 0.971 0.974 0.942 1.086 0.798 0.904 1.002 0.785 1.039 1.092 0.903 1.003 0.893 0.937 0.955 1.088 1.084 1.005 Phase annealing cycle: 7 Beta = 0.29415 Ralpha 0.088 0.116 0.098 0.100 0.120 0.056 0.156 0.127 0.081 0.161 0.060 0.057 0.114 0.054 0.119 0.088 0.091 0.053 0.055 0.083 Nqual -0.430-0.346-0.097-0.065-0.241-0.626-0.323-0.222-0.318-0.380-0.388-0.628-0.354-0.628-0.298-0.404-0.471-0.651-0.646-0.536 Mabs 0.991 0.901 0.989 0.980 0.961 1.106 0.829 0.908 1.022 0.814 1.062 1.096 0.912 1.085 0.910 0.963 0.982 1.079 1.097 1.026 Phase annealing cycle: 8 Beta = 0.32684 Ralpha 0.074 0.107 0.097 0.099 0.114 0.058 0.153 0.118 0.069 0.158 0.055 0.053 0.099 0.055 0.112 0.074 0.065 0.053 0.052 0.077 Nqual -0.498-0.346-0.102-0.147-0.300-0.644-0.224-0.253-0.410-0.334-0.534-0.620-0.291-0.623-0.301-0.459-0.599-0.646-0.667-0.539 Mabs 0.997 0.936 0.988 0.996 0.965 1.103 0.843 0.912 1.048 0.831 1.087 1.079 0.935 1.094 0.918 1.003 1.054 1.087 1.090 1.047 Phase annealing cycle: 9 Beta = 0.36315 Ralpha 0.076 0.106 0.101 0.093 0.112 0.056 0.135 0.114 0.068 0.151 0.053 0.053 0.093 0.056 0.114 0.059 0.058 0.056 0.054 0.056 Nqual -0.540-0.326-0.068-0.262-0.296-0.626-0.282-0.301-0.464-0.326-0.639-0.640-0.366-0.606-0.329-0.598-0.696-0.612-0.654-0.575 Mabs 1.022 0.939 0.994 0.997 0.973 1.104 0.857 0.917 1.057 0.861 1.092 1.095 0.941 1.105 0.927 1.038 1.085 1.098 1.102 1.080 Phase annealing cycle: 10 Beta = 0.40350 Ralpha 0.067 0.110 0.092 0.098 0.113 0.058 0.143 0.107 0.060 0.125 0.056 0.054 0.079 0.056 0.110 0.055 0.057 0.059 0.051 0.056 Nqual -0.565-0.324-0.033-0.317-0.263-0.621-0.221-0.299-0.554-0.204-0.646-0.609-0.375-0.602-0.318-0.620-0.649-0.621-0.634-0.642 Mabs 1.061 0.964 1.009 1.006 0.965 1.102 0.864 0.941 1.084 0.932 1.091 1.098 0.975 1.107 0.942 1.075 1.099 1.104 1.107 1.103 Phase refinement cycle: 1 Ralpha 0.118 0.271 0.205 0.210 0.200 0.109 0.358 0.289 0.104 0.234 0.107 0.107 0.199 0.110 0.274 0.107 0.107 0.109 0.109 0.103 Nqual -0.726 0.030 0.369-0.092 0.013-0.771 0.024-0.191-0.742 0.120-0.790-0.785-0.352-0.770-0.213-0.753-0.749-0.776-0.741-0.774 Mabs 0.870 0.755 0.850 0.814 0.832 0.875 0.690 0.724 0.885 0.817 0.878 0.882 0.786 0.876 0.736 0.879 0.883 0.882 0.875 0.887 Phase refinement cycle: 2 Ralpha 0.062 0.150 0.129 0.109 0.136 0.061 0.166 0.127 0.061 0.150 0.062 0.063 0.090 0.061 0.136 0.063 0.061 0.064 0.061 0.061 Nqual -0.838-0.070-0.021-0.486-0.196-0.812-0.086-0.422-0.827-0.098-0.835-0.829-0.619-0.829-0.349-0.834-0.820-0.829-0.828-0.832 Mabs 1.157 1.022 1.094 1.086 1.101 1.146 0.992 1.000 1.157 1.086 1.153 1.148 1.111 1.154 1.002 1.147 1.156 1.151 1.158 1.148 Try Ralpha Nqual Sigma-1 M(abs) CFOM Seminvariants 1420309. 0.063 -0.776 0.917 1.129 0.063 -+ 810089. 0.152 -0.205 -1.000 0.986 0.222 ++ 1953293. 0.126 -0.230 1.000 1.049 0.183 -- 1377857. 0.093 -0.655 1.000 1.063 0.093 -- 597829. 0.132 -0.348 1.000 1.061 0.147 -- 891993. 0.058 -0.790 0.917 1.123 0.058 -+ 265661. 0.191 -0.051 0.917 0.952 0.366 -+ 1328305. 0.101 -0.586 0.917 1.002 0.101 -+ 350069. 0.057 -0.778 0.917 1.131 0.057 -+ 1750345. 0.142 -0.297 1.000 1.072 0.171 -- 363117. 0.059 -0.794 0.917 1.132 0.059 -+ 1815585. 0.057 -0.801 0.917 1.127 0.057 -+ 689317. 0.068 -0.753 0.917 1.112 0.068 -+ 1349433. 0.056 -0.776 0.917 1.131 0.056 -+ 455709. 0.135 -0.345 0.917 0.984 0.151 -+ 181393. 0.058 -0.786 0.917 1.128 0.058 -+ 906965. 0.057 -0.780 0.917 1.130 0.057 -+ 340521. 0.059 -0.785 0.917 1.131 0.059 -+ 1702605. 0.056 -0.792 0.917 1.134 0.056 -+ 124417. 0.055 -0.786 0.917 1.126 0.055 -+ 622085. 0.174 -0.031 1.000 1.029 0.367 -- 1013273. 0.057 -0.788 0.917 1.129 0.057 -+ 872061. 0.057 -0.796 0.917 1.126 0.057 -+ 166001. 0.114 -0.361 1.000 1.046 0.126 -- 830005. 0.056 -0.783 0.917 1.127 0.056 -+ 2052873. 0.108 -0.404 1.000 1.046 0.112 -- 1875757. 0.120 -0.429 1.000 1.079 0.122 -- 990177. 0.061 -0.794 0.917 1.135 0.061 -+ 756581. 0.128 -0.385 0.917 0.994 0.135 -+ 1685753. 0.055 -0.794 0.917 1.129 0.055 -+ 40157. 0.152 0.030 1.000 1.049 0.402 -- 200785. 0.057 -0.792 0.917 1.133 0.057 -+ 1135797. 0.059 -0.795 0.917 1.130 0.059 -+ 93977. 0.057 -0.797 0.917 1.129 0.057 -+ 1921125. 0.056 -0.787 0.917 1.128 0.056 -+ 399017. 0.100 -0.555 0.917 1.082 0.100 -+ 15369. 0.059 -0.791 0.917 1.132 0.059 -+ 384225. 0.143 -0.352 -1.000 0.979 0.157 ++ 80681. 0.059 -0.765 0.917 1.132 0.059 -+ 1035749. 0.057 -0.801 0.917 1.125 0.057 -+ 1131949. 0.055 -0.801 0.917 1.130 0.055 -+ 984441. 0.058 -0.780 0.917 1.141 0.058 -+ 76845. 0.056 -0.816 0.917 1.129 0.056 -+ 1586817. 0.055 -0.792 0.917 1.126 0.055 -+ 854997. 0.055 -0.788 0.917 1.132 0.055 -+ 403405. 0.056 -0.795 0.917 1.123 0.056 -+ 252273. 0.057 -0.786 0.917 1.131 0.057 -+ 1995085. 0.060 -0.791 0.917 1.131 0.060 -+ 1206709. 0.116 -0.351 0.917 1.081 0.130 -+ 664841. 0.059 -0.774 0.917 1.131 0.059 -+ 1773469. 0.055 -0.790 0.917 1.129 0.055 -+ 971829. 0.058 -0.781 0.917 1.136 0.058 -+ 600553. 0.055 -0.804 0.917 1.124 0.055 -+ 177441. 0.136 -0.242 1.000 1.060 0.188 -- 322597. 0.144 -0.274 -1.000 0.968 0.183 ++ 1940833. 0.149 -0.049 0.917 1.053 0.326 -+ 1499633. 0.149 -0.066 1.000 1.048 0.312 -- 887205. 0.060 -0.777 0.917 1.137 0.060 -+ 139541. 0.058 -0.785 0.917 1.135 0.058 -+ 1387197. 0.057 -0.782 0.917 1.126 0.057 -+ 644529. 0.155 -0.034 1.000 1.058 0.345 -- 539541. 0.150 -0.098 -1.000 0.981 0.288 ++ 874349. 0.057 -0.778 0.917 1.125 0.057 -+ 1482665. 0.055 -0.795 0.917 1.130 0.055 -+ 1262745. 0.059 -0.807 0.917 1.136 0.059 -+ 27421. 0.141 -0.051 1.000 1.062 0.316 -- 1335213. 0.054 -0.791 0.917 1.130 0.054* -+ 1764893. 0.059 -0.797 0.917 1.136 0.059 -+ 1816769. 0.058 -0.785 0.917 1.132 0.058 -+ 772409. 0.057 -0.770 0.917 1.128 0.057 -+ 1534273. 0.058 -0.786 0.917 1.129 0.058 -+ 695237. 0.059 -0.781 0.917 1.134 0.059 -+ 1038949. 0.059 -0.789 0.917 1.141 0.059 -+ 608089. 0.056 -0.785 0.917 1.131 0.056 -+ 844345. 0.156 -0.228 -1.000 0.980 0.215 ++ 1938781. 0.156 0.097 1.000 1.047 0.477 -- 1681421. 0.059 -0.790 0.917 1.129 0.059 -+ 634117. 0.057 -0.788 0.917 1.134 0.057 -+ 1621645. 0.144 -0.064 1.000 1.059 0.309 -- 1323157. 0.058 -0.781 0.917 1.127 0.058 -+ 1092493. 0.058 -0.787 0.917 1.134 0.058 -+ 1140665. 0.056 -0.788 0.917 1.130 0.056 -+ 1225725. 0.058 -0.788 0.917 1.132 0.058 -+ 295001. 0.055 -0.799 0.917 1.127 0.055 -+ 1123529. 0.088 -0.647 1.000 1.070 0.088 -- 1934321. 0.056 -0.786 0.917 1.133 0.056 -+ 1503317. 0.154 -0.283 -1.000 0.970 0.189 ++ 991073. 0.060 -0.786 0.917 1.128 0.060 -+ 395677. 0.058 -0.796 0.917 1.133 0.058 -+ 1233725. 0.136 -0.199 1.000 1.063 0.210 -- 785089. 0.058 -0.786 0.917 1.129 0.058 -+ 1889069. 0.059 -0.785 0.917 1.131 0.059 -+ 2073941. 0.059 -0.790 0.917 1.130 0.059 -+ 327221. 0.135 -0.038 1.000 1.065 0.321 -- 465057. 0.055 -0.779 0.917 1.130 0.055 -+ 135421. 0.059 -0.783 0.917 1.139 0.059 -+ 156957. 0.059 -0.770 0.917 1.139 0.059 -+ 1233589. 0.061 -0.778 0.917 1.137 0.061 -+ 1128017. 0.055 -0.775 0.917 1.131 0.055 -+ 1106529. 0.056 -0.799 0.917 1.128 0.056 -+ 2069301. 0.058 -0.777 0.917 1.128 0.058 -+ 328605. 0.076 -0.742 1.000 1.092 0.076 -- 400249. 0.058 -0.774 0.917 1.128 0.058 -+ 1923669. 0.056 -0.783 0.917 1.132 0.056 -+ 1620313. 0.055 -0.788 0.917 1.129 0.055 -+ 1868361. 0.141 -0.061 0.917 1.065 0.308 -+ 1957897. 0.059 -0.789 0.917 1.133 0.059 -+ 303457. 0.154 0.032 1.000 1.049 0.407 -- 1354417. 0.057 -0.786 0.917 1.131 0.057 -+ 661937. 0.060 -0.785 0.917 1.130 0.060 -+ 1400877. 0.056 -0.794 0.917 1.132 0.056 -+ 1294969. 0.058 -0.774 0.917 1.132 0.058 -+ 2072985. 0.056 -0.798 0.917 1.127 0.056 -+ 1173429. 0.054 -0.784 0.917 1.129 0.054 -+ 1803557. 0.059 -0.803 0.917 1.128 0.059 -+ 1572253. 0.153 0.106 1.000 1.055 0.485 -- 1746025. 0.121 -0.289 1.000 1.061 0.154 -- 629177. 0.057 -0.790 0.917 1.129 0.057 -+ 96809. 0.084 -0.718 1.000 1.083 0.084 -- 1868025. 0.056 -0.782 0.917 1.128 0.056 -+ 1190989. 0.142 -0.027 1.000 1.041 0.339 -- 77765. 0.058 -0.793 0.917 1.130 0.058 -+ 1963493. 0.127 -0.139 1.000 1.078 0.237 -- 341517. 0.058 -0.779 0.917 1.135 0.058 -+ 812129. 0.058 -0.787 0.917 1.132 0.058 -+ 1165513. 0.059 -0.789 0.917 1.128 0.059 -+ 1707585. 0.149 0.080 1.000 1.066 0.451 -- 719253. 0.060 -0.791 0.917 1.137 0.060 -+ 1340501. 0.057 -0.792 0.917 1.133 0.057 -+ 411049. 0.056 -0.793 0.917 1.133 0.056 -+ 1049477. 0.057 -0.790 0.917 1.131 0.057 -+ 1053081. 0.057 -0.787 0.917 1.134 0.057 -+ 1071101. 0.089 -0.637 0.917 1.091 0.089 -+ 1161201. 0.057 -0.801 0.917 1.134 0.057 -+ 1611701. 0.057 -0.779 0.917 1.130 0.057 -+ 1767049. 0.057 -0.794 0.917 1.131 0.057 -+ 446637. 0.057 -0.789 0.917 1.129 0.057 -+ 136033. 0.059 -0.777 0.917 1.134 0.059 -+ 1303673. 0.060 -0.780 0.917 1.131 0.060 -+ 226909. 0.057 -0.781 0.917 1.137 0.057 -+ 1134545. 0.055 -0.784 0.917 1.124 0.055 -+ 1478421. 0.055 -0.801 0.917 1.131 0.055 -+ 1100649. 0.057 -0.792 0.917 1.129 0.057 -+ 253249. 0.058 -0.785 0.917 1.131 0.058 -+ 39769. 0.058 -0.777 0.917 1.129 0.058 -+ 198845. 0.096 -0.578 1.000 1.068 0.096 -- 776821. 0.058 -0.801 0.917 1.132 0.058 -+ 1786953. 0.059 -0.787 0.917 1.126 0.059 -+ 546157. 0.057 -0.786 0.917 1.134 0.057 -+ 633633. 0.059 -0.794 0.917 1.139 0.059 -+ 1071013. 0.057 -0.785 0.917 1.128 0.057 -+ 1160761. 0.060 -0.782 0.917 1.131 0.060 -+ 1609501. 0.057 -0.775 0.917 1.133 0.057 -+ 1756049. 0.057 -0.785 0.917 1.132 0.057 -+ 2034717. 0.057 -0.782 0.917 1.131 0.057 -+ 1668925. 0.059 -0.787 0.917 1.132 0.059 -+ 1225949. 0.055 -0.805 0.917 1.127 0.055 -+ 355657. 0.058 -0.786 0.917 1.126 0.058 -+ 66757. 0.058 -0.796 0.917 1.125 0.058 -+ 824013. 0.057 -0.794 0.917 1.135 0.057 -+ 1748853. 0.066 -0.766 0.917 1.120 0.066 -+ 1106961. 0.057 -0.799 0.917 1.135 0.057 -+ 793581. 0.059 -0.781 0.917 1.132 0.059 -+ 1288597. 0.057 -0.794 0.917 1.130 0.057 -+ 992701. 0.055 -0.796 0.917 1.116 0.055 -+ 1037401. 0.059 -0.803 0.917 1.136 0.059 -+ 2084665. 0.065 -0.738 0.917 1.122 0.065 -+ 602973. 0.057 -0.792 0.917 1.128 0.057 -+ 1214705. 0.056 -0.766 0.917 1.128 0.056 -+ 380585. 0.058 -0.782 0.917 1.132 0.058 -+ 694069. 0.101 -0.453 1.000 1.049 0.101 -- 1336625. 0.059 -0.790 0.917 1.133 0.059 -+ 437537. 0.076 -0.739 0.917 1.105 0.076 -+ 917713. 0.063 -0.782 0.917 1.133 0.063 -+ 1902925. 0.059 -0.793 0.917 1.137 0.059 -+ 76117. 0.058 -0.786 0.917 1.132 0.058 -+ 381709. 0.056 -0.785 0.917 1.130 0.056 -+ 1576281. 0.101 -0.470 1.000 1.050 0.101 -- 894745. 0.059 -0.780 0.917 1.135 0.059 -+ 10693. 0.056 -0.786 0.917 1.124 0.056 -+ 2089129. 0.057 -0.786 0.917 1.136 0.057 -+ 263065. 0.055 -0.801 0.917 1.130 0.055 -+ 767469. 0.058 -0.784 0.917 1.131 0.058 -+ 282309. 0.057 -0.791 0.917 1.130 0.057 -+ 2091693. 0.057 -0.794 0.917 1.135 0.057 -+ 1089561. 0.056 -0.795 0.917 1.128 0.056 -+ 1656409. 0.058 -0.767 0.917 1.133 0.058 -+ 282357. 0.059 -0.793 0.917 1.131 0.059 -+ 1729233. 0.070 -0.737 0.917 1.105 0.070 -+ 630785. 0.056 -0.791 0.917 1.132 0.056 -+ 1584861. 0.057 -0.778 0.917 1.136 0.057 -+ 970277. 0.056 -0.788 0.917 1.131 0.056 -+ 1338809. 0.065 -0.759 0.917 1.105 0.065 -+ 100717. 0.057 -0.779 0.917 1.129 0.057 -+ 839125. 0.058 -0.800 0.917 1.129 0.058 -+ 420829. 0.056 -0.780 0.917 1.126 0.056 -+ 881605. 0.094 -0.576 1.000 1.075 0.094 -- 825625. 0.058 -0.782 0.917 1.138 0.058 -+ 116233. 0.059 -0.796 0.917 1.132 0.059 -+ 1830761. 0.058 -0.806 0.917 1.127 0.058 -+ 167825. 0.057 -0.783 0.917 1.134 0.057 -+ 1549301. 0.057 -0.800 0.917 1.135 0.057 -+ 1592401. 0.060 -0.784 0.917 1.137 0.060 -+ 1697865. 0.056 -0.793 0.917 1.126 0.056 -+ 2030973. 0.057 -0.788 0.917 1.131 0.057 -+ 705745. 0.056 -0.780 0.917 1.129 0.056 -+ 219233. 0.057 -0.789 0.917 1.127 0.057 -+ 1312233. 0.059 -0.793 0.917 1.133 0.059 -+ 1770377. 0.058 -0.786 0.917 1.130 0.058 -+ 1697245. 0.058 -0.784 0.917 1.131 0.058 -+ 1882673. 0.057 -0.776 0.917 1.128 0.057 -+ 524465. 0.057 -0.796 0.917 1.128 0.057 -+ 300401. 0.056 -0.794 0.917 1.134 0.056 -+ 398209. 0.063 -0.765 0.917 1.114 0.063 -+ 929481. 0.057 -0.784 0.917 1.133 0.057 -+ 634913. 0.057 -0.772 0.917 1.140 0.057 -+ 1096165. 0.055 -0.786 0.917 1.129 0.055 -+ 149125. 0.056 -0.789 0.917 1.128 0.056 -+ 1980181. 0.059 -0.778 0.917 1.132 0.059 -+ 1342225. 0.057 -0.794 0.917 1.126 0.057 -+ 1563033. 0.057 -0.779 0.917 1.125 0.057 -+ 5965. 0.057 -0.798 0.917 1.128 0.057 -+ 264133. 0.059 -0.772 0.917 1.138 0.059 -+ 1725329. 0.058 -0.791 0.917 1.129 0.058 -+ 1758657. 0.056 -0.773 0.917 1.135 0.056 -+ 1605897. 0.058 -0.792 0.917 1.129 0.058 -+ 902209. 0.057 -0.788 0.917 1.131 0.057 -+ 825321. 0.061 -0.770 0.917 1.130 0.061 -+ 1320665. 0.058 -0.792 0.917 1.132 0.058 -+ 404677. 0.056 -0.797 0.917 1.126 0.056 -+ 1246969. 0.057 -0.785 0.917 1.130 0.057 -+ CFOM Range Frequency 0.000 - 0.020 0 0.020 - 0.040 0 0.040 - 0.060 169 0.060 - 0.080 18 0.080 - 0.100 6 0.100 - 0.120 7 0.120 - 0.140 6 0.140 - 0.160 7 0.160 - 0.180 1 0.180 - 0.200 5 0.200 - 0.220 4 0.220 - 0.240 3 0.240 - 0.260 1 0.260 - 0.280 1 0.280 - 0.300 4 0.300 - 0.320 6 0.320 - 0.340 3 0.340 - 0.360 1 0.360 - 0.380 6 0.380 - 0.400 0 0.400 - 0.420 3 0.420 - 0.440 1 0.440 - 0.460 2 0.460 - 0.480 1 0.480 - 0.500 1 0.500 - 0.520 0 0.520 - 0.540 0 0.540 - 0.560 0 0.560 - 0.580 0 0.580 - 0.600 0 0.600 - 9.999 0 256. Phase sets refined - best is code 1335213. with CFOM = 0.0540 6.9 seconds CPU time Tangent expanded to 1347 out of 1347 E greater than 1.200 Highest memory used = 5514 / 7747 0.1 seconds CPU time FMAP and GRID set by program FMAP 8 2 44 GRID -1.220 -2 -1 1.220 2 1 E-Fourier for 01SOT013 in Cc Maximum = 226.93, minimum = -63.84 highest memory used = 9242 / 47260 0.1 seconds CPU time Peak list optimization RE = 0.187 for 57 surviving atoms and 1347 E-values Highest memory used = 2057 / 12123 0.1 seconds CPU time E-Fourier for 01SOT013 in Cc Maximum = 248.84, minimum = -73.99 highest memory used = 9242 / 47260 0.1 seconds CPU time Peak list optimization RE = 0.171 for 59 surviving atoms and 1347 E-values Highest memory used = 2057 / 12123 0.1 seconds CPU time E-Fourier for 01SOT013 in Cc Maximum = 247.57, minimum = -54.50 highest memory used = 9242 / 47260 0.1 seconds CPU time Molecule 1 scale 0.476 inches = 1.210 cm per Angstrom 55 65 60 59 49 78 67 33 44 84 45 74 43 10 68 31 26 51 1 82 85 18 69 15 35 23 6 2 22 17 11 16 77 79 8 75 85 7 82 12 14 42 24 9 72 19 32 20 15 80 39 37 38 29 5 4 40 25 73 13 3 57 48 27 70 46 71 21 34 41 5*2 54 58 28 81 64 76 62 30 36 56 47 61 63 66 Atom Peak x y z SOF Height Distances and Angles 1 248. 0.0072 0.4665 0.7033 1.000 1.48 0 18 1.194 2 244. -0.1070 0.4663 0.1795 1.000 3.60 0 17 1.279 0 79 1.653 45.8 0 82 1.884 165.8 134.5 3 211. -0.0699 0.7286 0.7013 1.000 1.23 0 25 1.163 4 209. -0.0299 0.7271 0.1816 1.000 3.74 0 27 1.193 5 188. -0.0990 0.6829 0.2817 1.000 3.10 0 13 1.338 0 14 1.364 108.6 0 27 1.502 132.7 118.4 0 80 1.201 54.7 53.9 170.2 6 185. -0.1210 0.4561 0.4040 1.000 2.53 0 17 1.317 0 31 1.473 122.0 7 184. -0.1201 0.5720 0.3001 1.000 2.98 0 14 1.309 0 15 1.365 108.5 0 17 1.511 120.6 130.8 0 79 1.085 119.2 106.8 51.6 0 80 1.134 56.8 51.8 177.2 128.0 0 85 1.031 77.1 87.1 100.7 151.7 80.0 8 183. -0.0142 0.6160 0.6191 1.000 1.78 0 9 1.339 0 11 1.310 110.1 0 77 1.185 55.7 55.3 9 182. -0.0003 0.6829 0.6014 1.000 1.88 0 8 1.339 0 12 1.362 109.3 0 25 1.528 117.0 133.1 0 77 1.187 55.5 54.1 166.2 10 181. 0.0206 0.4564 0.4803 1.000 2.55 0 18 1.353 0 33 1.473 120.6 11 180. 0.0201 0.5728 0.5813 1.000 2.05 0 8 1.310 0 16 1.371 109.4 0 18 1.556 121.1 129.2 0 77 1.163 56.9 53.1 168.5 12 178. 0.0472 0.6839 0.5597 1.000 2.20 0 9 1.362 0 16 1.440 105.2 0 19 1.452 129.4 125.4 0 77 1.170 55.3 50.9 169.5 13 174. -0.1459 0.6834 0.3213 1.000 2.79 0 5 1.338 0 15 1.423 106.2 0 21 1.482 130.0 123.8 0 80 1.172 56.7 49.6 172.1 14 172. -0.0840 0.6146 0.2695 1.000 3.21 0 5 1.364 0 7 1.309 110.0 0 80 1.172 55.9 54.1 0 85 1.475 100.9 43.0 62.3 15 170. -0.1591 0.6116 0.3383 1.000 2.70 0 7 1.365 0 13 1.423 106.7 0 20 1.515 127.7 125.4 0 79 1.974 31.8 123.0 104.1 0 80 1.112 53.3 53.4 175.1 74.8 0 85 1.668 38.1 96.2 128.3 68.0 56.0 2 82 1.913 76.6 101.9 95.4 99.4 89.5 41.7 16 165. 0.0601 0.6109 0.5427 1.000 2.33 0 11 1.371 0 12 1.440 105.8 0 23 1.462 128.8 125.1 0 77 1.148 54.1 52.3 167.7 17 164. -0.1128 0.4931 0.2960 1.000 3.04 0 2 1.279 0 6 1.317 124.4 0 7 1.511 117.2 117.6 0 79 1.193 83.9 131.4 45.4 0 85 1.981 137.1 96.8 30.8 76.1 18 162. 0.0151 0.4916 0.5972 1.000 1.99 0 1 1.194 0 10 1.353 126.7 0 11 1.556 121.0 112.3 19 159. 0.0801 0.7436 0.5387 1.000 2.37 0 12 1.452 0 32 1.447 116.9 0 38 1.345 126.6 116.5 20 154. -0.2098 0.5858 0.3787 1.000 2.38 0 15 1.515 0 24 1.377 119.9 0 29 1.340 120.8 119.3 0 72 1.710 163.5 45.8 74.3 21 152. -0.1804 0.7435 0.3425 1.000 2.59 0 13 1.482 0 28 1.440 117.9 0 41 1.377 127.0 115.1 22 150. 0.1297 0.6118 0.3948 1.000 3.20 0 23 1.402 0 35 1.314 125.3 0 68 1.818 67.3 58.9 23 150. 0.1094 0.5855 0.5072 1.000 2.63 0 16 1.462 0 22 1.402 123.8 0 26 1.380 121.3 114.8 0 68 1.817 167.2 67.4 48.3 24 149. -0.2412 0.5352 0.2977 1.000 2.68 0 20 1.377 0 42 1.384 122.8 0 72 1.241 81.4 44.0 25 149. -0.0345 0.7405 0.6475 1.000 1.57 0 3 1.163 0 9 1.528 123.1 0 46 1.364 124.8 112.1 26 148. 0.1408 0.5345 0.5874 1.000 2.35 0 23 1.380 0 45 1.426 121.8 0 68 1.367 82.8 40.7 27 144. -0.0656 0.7403 0.2383 1.000 3.38 0 4 1.193 0 5 1.502 121.3 0 34 1.345 123.1 115.6 28 144. -0.2213 0.7666 0.2234 1.000 3.03 0 21 1.440 0 36 1.356 120.0 29 143. -0.2253 0.6129 0.4906 1.000 1.82 0 20 1.340 0 40 1.477 117.9 0 72 1.866 61.9 57.2 30 140. -0.2095 0.8357 0.4765 1.000 1.88 0 41 1.339 0 47 1.428 119.9 31 140. -0.1224 0.3785 0.4024 1.000 2.55 0 6 1.473 0 51 1.548 110.3 32 132. 0.1206 0.7666 0.6597 1.000 1.92 0 19 1.447 0 37 1.401 122.7 33 130. 0.0236 0.3788 0.4804 1.000 2.57 0 10 1.473 0 49 1.509 111.7 0 74 1.821 76.5 125.7 34 129. -0.0802 0.8065 0.2621 1.000 3.22 0 27 1.345 0 53 1.412 121.1 35 126. 0.1752 0.5927 0.3646 1.000 3.46 0 22 1.314 0 43 1.395 120.2 0 68 1.601 76.5 45.1 36 125. -0.2529 0.8224 0.2368 1.000 2.87 0 28 1.356 0 47 1.331 123.9 37 121. 0.1579 0.8197 0.6513 1.000 2.04 0 32 1.401 0 48 1.413 115.2 0 70 2.017 147.2 32.2 0 73 1.014 163.1 48.6 16.4 38 121. 0.0763 0.7803 0.4183 1.000 2.91 0 19 1.345 0 57 1.451 120.9 0 71 1.918 148.6 31.9 39 121. -0.3074 0.5417 0.4349 1.000 1.87 0 40 1.332 0 42 1.381 119.6 0 72 1.262 78.2 43.8 0 75 1.822 78.3 75.8 50.0 40 120. -0.2775 0.5900 0.5163 1.000 1.57 0 29 1.477 0 39 1.332 121.4 0 72 1.637 73.4 49.0 0 75 2.026 85.6 61.7 43.3 41 120. -0.1777 0.7809 0.4654 1.000 2.02 0 21 1.377 0 30 1.339 123.9 42 119. -0.2901 0.5134 0.3220 1.000 2.45 0 24 1.384 0 39 1.381 118.9 0 72 0.992 60.3 61.7 0 75 1.997 85.0 62.2 40.4 43 119. 0.2078 0.5423 0.4469 1.000 3.18 0 35 1.395 0 45 1.380 118.7 0 68 1.165 76.9 44.0 44 118. -0.1779 0.2716 0.3815 1.000 2.52 0 51 1.536 0 67 1.100 155.8 0 84 1.601 106.0 95.4 45 116. 0.1904 0.5118 0.5578 1.000 2.63 0 26 1.426 0 43 1.380 119.2 0 68 0.973 66.4 56.2 46 115. -0.0178 0.8063 0.6211 1.000 1.72 0 25 1.364 0 52 1.512 116.6 0 76 1.690 122.9 35.2 47 112. -0.2493 0.8582 0.3565 1.000 2.32 0 30 1.428 0 36 1.331 117.1 48 112. 0.1492 0.8554 0.5204 1.000 2.62 0 37 1.413 0 57 1.287 124.0 0 70 1.115 105.2 130.7 0 73 1.063 45.7 169.4 59.5 49 110. 0.0798 0.3532 0.4840 1.000 2.71 0 33 1.509 0 59 1.480 132.8 0 60 1.572 105.2 30.0 0 78 1.092 103.3 81.6 100.0 51 108. -0.1798 0.3518 0.4008 1.000 2.41 0 31 1.548 0 44 1.536 105.6 0 69 1.124 98.8 101.2 52 107. -0.0422 0.8673 0.6852 1.000 1.35 0 46 1.512 0 54 1.602 118.0 0 76 0.984 82.3 158.9 53 104. -0.0498 0.8650 0.2346 1.000 3.41 0 34 1.412 0 56 1.595 103.5 0 62 1.957 103.4 64.4 0 81 1.995 77.1 88.9 152.8 54 102. -0.0208 0.8822 0.8507 1.000 0.64 0 52 1.602 0 58 1.459 109.5 55 98. 0.1393 0.2449 0.5567 1.000 2.55 0 59 1.111 0 60 1.633 25.7 0 65 2.022 58.3 32.9 56 93. -0.0932 0.9267 0.1999 1.000 3.44 0 53 1.595 0 61 1.372 123.9 0 62 1.916 67.0 161.6 57 89. 0.1114 0.8398 0.4126 1.000 3.02 0 38 1.451 0 48 1.287 120.2 0 71 1.030 99.9 136.4 58 75. 0.0313 0.9174 0.8750 1.000 0.65 0 54 1.459 0 64 1.480 109.9 59 56. 0.1072 0.2850 0.5229 1.000 2.62 0 49 1.480 0 55 1.111 161.5 0 60 0.795 81.5 117.0 0 65 1.721 109.6 88.4 29.3 0 78 1.705 39.3 128.9 105.5 133.5 60 56. 0.0772 0.2709 0.4986 1.000 2.65 0 49 1.572 0 55 1.633 105.8 0 59 0.795 68.5 37.3 0 65 1.099 156.8 93.4 129.9 61 56. -0.1200 0.9535 0.2957 1.000 2.92 0 56 1.372 0 63 1.439 123.5 62 52. -0.0789 0.8837 0.0337 1.000 4.26 0 53 1.957 0 56 1.916 48.6 63 49. -0.1597 1.0085 0.2626 1.000 2.96 0 61 1.439 0 66 1.387 111.9 64 46. 0.0484 0.9390 1.0249 1.000 0.00 0 58 1.480 65 45. 0.0623 0.2171 0.4712 1.000 2.75 0 55 2.022 0 59 1.721 33.3 0 60 1.099 53.7 20.8 66 44. -0.1477 1.0650 0.3549 1.000 2.55 0 63 1.387 67 44. -0.1613 0.2181 0.4027 1.000 2.48 0 44 1.100 0 84 2.026 51.9 68 39. 0.1667 0.5355 0.4787 1.000 2.92 0 22 1.818 0 23 1.817 45.4 0 26 1.367 93.7 48.9 0 35 1.601 44.6 89.6 135.2 0 43 1.165 101.7 141.9 145.9 58.0 0 45 0.973 152.7 119.9 72.9 134.6 79.9 69 38. -0.2005 0.3691 0.2912 1.000 2.86 0 51 1.124 70 38. 0.1793 0.8990 0.5370 1.000 2.61 0 37 2.017 0 48 1.115 42.5 0 73 1.082 15.3 57.8 71 36. 0.0886 0.8665 0.3276 1.000 3.35 0 38 1.918 0 57 1.030 48.2 72 36. -0.2630 0.5355 0.3996 1.000 2.16 0 20 1.710 0 24 1.241 52.8 0 29 1.866 43.8 96.0 0 39 1.262 140.1 144.1 101.4 0 40 1.637 92.3 140.1 49.3 52.8 0 42 0.992 125.5 75.7 152.6 74.5 124.4 0 75 1.399 110.8 123.7 94.3 86.2 83.3 112.2 73 36. 0.1764 0.8621 0.6200 1.000 2.23 0 37 1.014 0 48 1.063 85.7 0 70 1.082 148.3 62.6 74 36. -0.0277 0.3986 0.3215 1.000 3.17 0 33 1.821 75 35. -0.2479 0.4908 0.5166 1.000 1.66 0 39 1.822 0 40 2.026 40.0 0 42 1.997 42.1 71.3 0 72 1.399 43.7 53.4 27.4 76 35. -0.0600 0.8760 0.5857 1.000 1.76 0 46 1.690 0 52 0.984 62.5 0 81 1.508 87.2 141.7 77 35. 0.0272 0.6332 0.5938 1.000 2.00 0 8 1.185 0 9 1.187 68.7 0 11 1.163 67.9 135.0 0 12 1.170 138.7 70.6 148.0 0 16 1.148 139.6 145.1 72.8 76.8 78 34. 0.1019 0.3669 0.5906 1.000 2.27 0 49 1.092 0 59 1.705 59.1 79 34. -0.1404 0.5349 0.2210 1.000 3.31 0 2 1.653 0 7 1.085 119.6 0 15 1.974 157.9 41.5 0 17 1.193 50.3 83.0 108.9 0 80 1.995 138.0 26.6 32.5 109.6 80 34. -0.1241 0.6316 0.2996 1.000 2.96 0 5 1.201 0 7 1.134 139.2 0 13 1.172 68.6 151.8 0 14 1.172 70.2 69.1 138.7 0 15 1.112 145.3 74.8 77.0 143.7 0 79 1.995 139.7 25.4 140.8 76.7 72.7 0 85 1.394 114.9 46.7 127.9 69.5 82.7 72.1 81 34. -0.0492 0.8762 0.4393 1.000 2.46 0 53 1.995 0 76 1.508 167.6 82 33. -0.1119 0.4115 0.0153 1.000 4.36 0 2 1.884 1 15 1.913 142.6 3 85 1.296 137.0 59.0 84 33. -0.2390 0.2467 0.3282 1.000 2.61 0 44 1.601 0 67 2.026 32.7 85 32. -0.0961 0.5836 0.3980 1.000 2.59 0 7 1.031 0 14 1.475 59.9 0 15 1.668 54.8 87.1 0 17 1.981 48.6 89.1 91.2 0 80 1.394 53.3 48.1 41.4 101.8 2 82 1.296 126.0 152.0 79.3 115.2 110.1 Atom Code x y z Height Symmetry transformation 15 1 -0.1591 0.3884 -0.1617 5.06 0.0000+X 1.0000-Y -0.5000+Z 82 2 -0.1119 0.5885 0.5153 2.01 0.0000+X 1.0000-Y 0.5000+Z 85 3 -0.0961 0.4164 -0.1020 4.94 0.0000+X 1.0000-Y -0.5000+Z Molecule 2 Atom Peak x y z SOF Height Distances and Angles 50 109. 0.0208 0.0476 0.0823 1.000 Molecule 3 Atom Peak x y z SOF Height Distances and Angles 83 33. 0.2081 0.1783 0.8965 1.000 0.0 seconds CPU time +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 16:17:53 Total CPU time: 8.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++