++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XS - CRYSTAL STRUCTURE SOLUTION - SHELXTL Ver. 6.12 W95/98/NT/2000/ME + + Copyright(c) 2001 Bruker AXS All Rights Reserved + + shelxs started at 20:50:03 on 22-Nov-2010 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL p-1 in P2(1) CELL 0.71073 7.5138 9.3146 12.8999 90.000 90.000 90.000 ZERR 4.00 0.0005 0.0007 0.0011 0.000 0.000 0.000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H N O UNIT 40 44 4 12 V = 902.84 At vol = 16.1 F(000) = 408.0 mu = 0.11 mm-1 Max single Patterson vector = 26.1 cell wt = 772.79 rho = 1.421 OMIT 4.00 180.00 ESEL 1.200 5.000 0.005 0.700 0 TREF HKLF 4 7477 Reflections read, of which 7 rejected Maximum h, k, l and 2-Theta = 9. 12. 16. 55.25 INCONSISTENT EQUIVALENTS h k l F*F Sigma(F*F) Esd of mean(F*F) 2 3 8 6.22 1.19 8.25 1964 Unique reflections, of which 1504 observed R(int) = 0.0618 R(sigma) = 0.0641 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) 4. 14. 35. 58. 76. 85. 77. 75. 113. 148. 221. 270. 242. N(measured) 4. 15. 37. 62. 81. 88. 83. 83. 125. 161. 246. 355. 452. N(theory) 10. 17. 42. 65. 84. 90. 85. 84. 127. 161. 253. 383. 563. 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 = 4321 / 9820 Observed E .GT. 1.200 1.300 1.400 1.500 1.600 1.700 1.800 1.900 2.000 2.100 Number 434 384 324 271 231 204 168 144 107 85 Centric Acentric 0kl h0l hk0 Rest Mean Abs(E*E-1) 0.968 0.736 1.103 1.021 1.120 0.908 0.1 seconds elapsed time SUMMARY OF PARAMETERS FOR p-1 in P2(1) 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 12 nf 16 s+ 0.800 s- 0.200 wr 0.200 PHAN steps 10 cool 0.900 Boltz 0.300 ns 199 mtpr 40 mnqr 10 TREF np 256. nE 283 kapscal 0.800 ntan 3 wn -0.750 FMAP code 8 PLAN npeaks -36 del1 0.500 del2 1.500 MORE verbosity 1 TIME t 9999999. 199 Reflections and 2526. unique TPR for phase annealing 203 Phases refined using 2640. unique TPR 203 Reflections and 2640. unique TPR for R(alpha) 0.0 seconds elapsed time 2066 Unique negative quartets found, 2032 used for phase refinement 0.0 seconds elapsed time Highest memory used to derive phase relations = 3066 / 40589 ONE-PHASE SEMINVARIANTS h k l E P+ Phi 0 0 6 1.977 0.15 -4 0 6 2.010 0.39 6 0 0 1.999 0.23 4 0 4 1.839 0.03 -4 0 4 1.817 0.02 -6 0 2 1.913 0.17 -4 0 10 1.682 0.52 6 0 2 1.887 0.17 4 0 10 1.576 0.52 -2 0 4 1.220 0.87 Expected value of Sigma-1 = 0.781 Following phases held constant with unit weights for the initial 4 weighted tangent cycles (before phase annealing): h k l E Phase/Comment -1 1 1 2.176 random phase 1 1 1 2.154 random phase -3 3 1 2.456 random phase 3 4 0 2.935 random phase 1 3 0 2.002 random phase 0 2 4 2.568 random phase 0 0 6 1.977 180 sigma-1 = 0.153 -2 1 6 2.191 random phase 2 1 4 1.947 random phase -2 1 4 1.893 random phase 4 0 4 1.839 180 sigma-1 = 0.025 3 2 1 1.656 random phase -4 0 4 1.817 180 sigma-1 = 0.021 1 2 1 1.517 random phase -1 2 1 1.504 random phase -6 0 2 1.913 180 sigma-1 = 0.175 6 0 2 1.887 180 sigma-1 = 0.175 -2 0 4 1.220 0 sigma-1 = 0.873 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 526 Unique NQR employed in phase annealing 128 Parallel refinements, highest memory = 10318 / 66140 0.0 seconds elapsed time STRUCTURE SOLUTION for p-1 in P2(1) Phase annealing cycle: 1 Beta = 0.13152 Ralpha 0.134 0.120 0.112 0.121 0.122 0.104 0.212 0.207 0.143 0.122 0.165 0.101 0.110 0.131 0.155 0.124 0.171 0.136 0.147 0.181 Nqual -0.085 0.426 0.330-0.170-0.198 0.228-0.313-0.112 0.164 0.233-0.154-0.046 0.117 0.285 0.052-0.349-0.138 0.251-0.244-0.149 Mabs 0.872 0.926 1.016 0.957 0.925 0.952 0.753 0.771 0.882 1.041 0.844 0.920 0.931 0.911 0.918 0.925 0.805 0.961 0.864 0.790 Phase annealing cycle: 2 Beta = 0.14613 Ralpha 0.153 0.149 0.117 0.169 0.162 0.129 0.346 0.255 0.147 0.111 0.174 0.134 0.140 0.152 0.163 0.106 0.247 0.177 0.148 0.247 Nqual -0.364-0.069 0.027-0.504-0.541-0.116-0.507-0.353-0.062-0.166-0.464-0.318-0.129-0.187-0.399-0.612-0.434-0.163-0.410-0.374 Mabs 0.829 0.836 0.916 0.834 0.835 0.876 0.671 0.733 0.847 0.959 0.804 0.835 0.864 0.839 0.825 0.884 0.721 0.841 0.825 0.740 Phase annealing cycle: 3 Beta = 0.16237 Ralpha 0.143 0.161 0.110 0.138 0.157 0.137 0.244 0.255 0.123 0.084 0.164 0.148 0.131 0.138 0.124 0.076 0.259 0.137 0.154 0.200 Nqual -0.382-0.239-0.265-0.511-0.600-0.300-0.468-0.385-0.182-0.251-0.483-0.456-0.117-0.292-0.415-0.691-0.354-0.257-0.333-0.245 Mabs 0.838 0.824 0.907 0.857 0.829 0.852 0.718 0.730 0.869 0.990 0.805 0.818 0.884 0.858 0.858 0.942 0.715 0.870 0.829 0.766 Phase annealing cycle: 4 Beta = 0.18041 Ralpha 0.140 0.156 0.114 0.139 0.138 0.124 0.184 0.227 0.112 0.085 0.152 0.139 0.140 0.123 0.128 0.071 0.213 0.128 0.144 0.185 Nqual -0.447-0.250-0.348-0.572-0.610-0.216-0.522-0.304-0.200-0.330-0.540-0.465-0.166-0.181-0.532-0.724-0.374-0.253-0.409-0.310 Mabs 0.837 0.834 0.913 0.859 0.862 0.872 0.763 0.750 0.905 1.007 0.814 0.823 0.884 0.898 0.894 0.940 0.753 0.878 0.838 0.797 Phase annealing cycle: 5 Beta = 0.20045 Ralpha 0.133 0.173 0.115 0.139 0.126 0.134 0.166 0.227 0.113 0.085 0.156 0.134 0.146 0.142 0.123 0.069 0.179 0.141 0.140 0.209 Nqual -0.446-0.229-0.301-0.542-0.586-0.268-0.535-0.308-0.270-0.346-0.567-0.397-0.117-0.288-0.582-0.741-0.368-0.215-0.514-0.389 Mabs 0.847 0.819 0.913 0.866 0.873 0.867 0.798 0.748 0.910 0.997 0.803 0.840 0.879 0.873 0.917 0.954 0.798 0.877 0.854 0.785 Phase annealing cycle: 6 Beta = 0.22273 Ralpha 0.112 0.143 0.113 0.122 0.132 0.131 0.156 0.186 0.122 0.077 0.138 0.131 0.138 0.140 0.105 0.074 0.122 0.144 0.131 0.157 Nqual -0.384-0.180-0.309-0.520-0.618-0.326-0.364-0.341-0.288-0.439-0.492-0.422-0.128-0.322-0.611-0.755-0.268-0.267-0.495-0.347 Mabs 0.892 0.847 0.933 0.915 0.881 0.867 0.823 0.780 0.910 1.012 0.831 0.834 0.901 0.879 0.923 0.946 0.875 0.872 0.854 0.814 Phase annealing cycle: 7 Beta = 0.24747 Ralpha 0.117 0.128 0.108 0.120 0.125 0.119 0.134 0.164 0.111 0.074 0.108 0.122 0.130 0.135 0.085 0.072 0.100 0.133 0.113 0.143 Nqual -0.411-0.176-0.310-0.497-0.654-0.347-0.234-0.332-0.278-0.375-0.559-0.454-0.062-0.276-0.691-0.748-0.189-0.195-0.538-0.338 Mabs 0.909 0.888 0.929 0.914 0.905 0.892 0.881 0.793 0.924 1.027 0.869 0.864 0.911 0.880 0.951 0.955 0.918 0.892 0.876 0.828 Phase annealing cycle: 8 Beta = 0.27497 Ralpha 0.117 0.127 0.114 0.111 0.086 0.119 0.122 0.152 0.116 0.077 0.109 0.124 0.133 0.136 0.072 0.076 0.108 0.131 0.108 0.142 Nqual -0.375-0.075-0.278-0.515-0.694-0.335-0.262-0.347-0.212-0.427-0.559-0.366-0.163-0.333-0.697-0.726-0.089-0.192-0.506-0.277 Mabs 0.920 0.902 0.923 0.923 0.946 0.889 0.922 0.816 0.920 1.010 0.878 0.862 0.907 0.890 0.966 0.959 0.920 0.884 0.887 0.842 Phase annealing cycle: 9 Beta = 0.30552 Ralpha 0.102 0.125 0.115 0.107 0.069 0.120 0.104 0.128 0.112 0.070 0.099 0.121 0.117 0.135 0.074 0.075 0.097 0.120 0.110 0.144 Nqual -0.199-0.038-0.241-0.518-0.727-0.331-0.144-0.363-0.203-0.368-0.541-0.403-0.220-0.267-0.708-0.720-0.144-0.250-0.502-0.379 Mabs 0.991 0.912 0.931 0.918 0.979 0.910 0.972 0.839 0.935 1.028 0.902 0.867 0.926 0.885 0.971 0.970 0.932 0.901 0.884 0.846 Phase annealing cycle: 10 Beta = 0.33947 Ralpha 0.076 0.121 0.113 0.120 0.067 0.117 0.097 0.125 0.110 0.075 0.102 0.122 0.116 0.121 0.072 0.077 0.107 0.126 0.106 0.140 Nqual -0.246-0.072-0.219-0.483-0.730-0.261-0.037-0.352-0.301-0.413-0.584-0.416-0.324-0.304-0.711-0.739-0.175-0.261-0.537-0.427 Mabs 1.025 0.912 0.929 0.906 0.979 0.919 0.987 0.848 0.930 1.022 0.913 0.860 0.923 0.902 0.966 0.960 0.919 0.892 0.888 0.845 Phase refinement cycle: 1 Ralpha 0.079 0.119 0.094 0.113 0.069 0.110 0.087 0.113 0.109 0.088 0.094 0.114 0.117 0.119 0.079 0.071 0.107 0.112 0.116 0.144 Nqual -0.406-0.099-0.048-0.528-0.810-0.231 0.106-0.342-0.314-0.441-0.670-0.490-0.241-0.207-0.796-0.805-0.136-0.350-0.589-0.395 Mabs 1.019 0.925 0.950 0.936 0.985 0.920 1.025 0.887 0.940 1.015 0.936 0.870 0.927 0.919 0.963 0.963 0.918 0.917 0.895 0.849 Phase refinement cycle: 2 Ralpha 0.077 0.122 0.094 0.124 0.066 0.107 0.085 0.101 0.104 0.085 0.084 0.104 0.118 0.108 0.071 0.067 0.101 0.113 0.117 0.134 Nqual -0.453-0.392-0.242-0.676-0.836-0.406-0.058-0.373-0.511-0.502-0.648-0.561-0.484-0.392-0.798-0.851-0.252-0.514-0.640-0.513 Mabs 1.031 0.919 0.959 0.918 0.991 0.919 1.032 0.926 0.948 1.023 0.969 0.896 0.928 0.939 0.978 0.993 0.935 0.918 0.905 0.866 Try Ralpha Nqual Sigma-1 M(abs) CFOM Seminvariants 1420309. 0.079 -0.470 0.556 1.028 0.157 -+--- +++++ 810089. 0.114 -0.454 0.351 0.924 0.201 ---+- ++-++ 1953293. 0.097 -0.329 0.089 0.954 0.274 ----+ -+++- 1377857. 0.125 -0.716 0.375 0.921 0.126 --++- ----+ 597829. 0.065 -0.825 0.617 0.992 0.065 +-+-- ----+ 891993. 0.106 -0.506 0.089 0.917 0.165 ----+ -+++- 265661. 0.079 -0.149 0.553 1.031 0.440 -++-- -+-+- 1328305. 0.104 -0.405 0.806 0.930 0.223 ----- ++-++ 350069. 0.101 -0.547 0.351 0.945 0.142 ---+- ++-++ 1750345. 0.084 -0.533 0.943 1.014 0.131 -+--- -+-++ 363117. 0.083 -0.601 0.556 0.979 0.105 -+--- +++++ 1815585. 0.101 -0.541 0.397 0.896 0.145 --+-- --+-- 689317. 0.117 -0.504 0.351 0.925 0.177 ---+- ++-++ 1349433. 0.105 -0.383 0.351 0.943 0.240 ---+- ++-++ 455709. 0.069 -0.783 0.376 0.978 0.069 +-+-- ----- 181393. 0.067 -0.855 0.617 0.987 0.067 +-+-- ----+ 906965. 0.101 -0.215 0.330 0.942 0.387 ----+ -++++ 340521. 0.112 -0.481 0.274 0.921 0.184 -+-+- +---+ 1702605. 0.121 -0.648 -0.203 0.898 0.131 -+-++ +---+ 124417. 0.132 -0.545 0.254 0.869 0.174 ++-+- ----+ 622085. 0.102 -0.572 0.351 0.940 0.134 ---+- ++-++ 1013273. 0.085 -0.393 0.192 0.959 0.213 --++- ++--+ 872061. 0.113 -0.648 0.806 0.874 0.123 ----- ++-++ 166001. 0.060 -0.830 0.617 0.994 0.060 +-+-- ----+ 830005. 0.095 -0.262 -0.367 0.939 0.333 ---++ -+++- 2052873. 0.067 -0.830 0.617 0.985 0.067 +-+-- ----+ 1875757. 0.062 -0.834 0.617 1.001 0.062 +-+-- ----+ 990177. 0.056 -0.837 0.617 0.996 0.056* +-+-- ----+ 756581. 0.102 -0.434 0.089 0.949 0.201 ----+ -+++- 1685753. 0.106 -0.586 -0.340 0.915 0.133 ---++ +-+-+ 40157. 0.098 -0.341 0.351 0.950 0.265 ---+- ++-++ 200785. 0.083 -0.436 0.556 1.017 0.181 -+--- +++++ 15369. 0.090 -0.597 -0.340 0.932 0.113 ---++ +-+-+ 1035749. 0.076 -0.490 0.556 1.034 0.143 -+--- +++++ 1696517. 0.069 -0.514 0.556 1.028 0.125 -+--- +++++ 351505. 0.061 -0.853 0.376 0.993 0.061 +-+-- ----- 60721. 0.066 -0.832 0.617 0.990 0.066 +-+-- ----+ 1921689. 0.094 -0.350 0.351 0.966 0.254 ---+- ++-++ 399017. 0.100 -0.614 0.603 0.923 0.119 ----- +++-+ 1465441. 0.077 -0.403 0.556 1.027 0.197 -+--- +++++ 854997. 0.099 -0.079 0.089 0.962 0.549 ----+ -+++- 201889. 0.067 -0.847 0.617 0.986 0.067 +-+-- ----+ 1904881. 0.100 -0.514 0.806 0.918 0.156 ----- ++-++ 303605. 0.064 -0.853 0.617 0.994 0.064 +-+-- ----+ 984441. 0.105 -0.410 0.351 0.935 0.220 ---+- ++-++ 1041549. 0.106 -0.514 0.125 0.926 0.161 ----+ +-+++ 727901. 0.071 -0.795 0.617 0.994 0.071 +-+-- ----+ 70301. 0.077 -0.474 0.556 1.018 0.153 -+--- +++++ 664841. 0.096 -0.287 0.556 1.013 0.310 -+--- +++++ 1187309. 0.096 -0.325 0.091 0.988 0.277 -+-+- +++-+ 333761. 0.090 -0.174 0.556 1.013 0.421 -+--- +++++ 1955161. 0.080 -0.450 0.556 1.031 0.170 -+--- +++++ 1452657. 0.067 -0.829 0.617 0.985 0.067 +-+-- ----+ 1001477. 0.068 -0.843 0.617 0.988 0.068 +-+-- ----+ 1316197. 0.104 -0.594 -0.396 0.916 0.128 -+-++ +-+-+ 1742241. 0.089 -0.553 0.545 0.949 0.128 -+--- +-+++ 296533. 0.071 -0.852 0.376 0.985 0.071 +-+-- ----- 1668805. 0.092 -0.354 0.089 0.954 0.249 ----+ -+++- 1874237. 0.075 -0.227 0.089 0.954 0.348 ----+ -+++- 410665. 0.077 -0.300 0.089 0.951 0.280 ----+ -+++- 241721. 0.081 -0.474 0.360 1.037 0.157 -++-- -+++- 874349. 0.086 -0.339 0.089 0.953 0.255 ----+ -+++- 2052569. 0.122 -0.487 0.351 0.928 0.191 ---+- ++-++ 1821593. 0.103 -0.303 0.089 0.931 0.303 ----+ -+++- 1705801. 0.095 -0.221 0.330 0.950 0.375 ----+ -++++ 1927917. 0.070 -0.835 0.376 0.994 0.070 +-+-- ----- 360909. 0.089 -0.554 0.553 1.000 0.127 -++-- -+-+- 844345. 0.093 -0.389 0.089 0.955 0.224 ----+ -+++- 324329. 0.085 -0.322 0.089 0.952 0.268 ----+ -+++- 1038949. 0.069 -0.848 0.617 0.970 0.069 +-+-- ----+ 513653. 0.076 -0.469 0.556 1.041 0.155 -+--- +++++ 1923045. 0.081 -0.405 0.553 1.035 0.200 -++-- -+-+- 22269. 0.069 -0.843 0.617 0.980 0.069 +-+-- ----+ 412661. 0.095 -0.421 0.330 0.926 0.203 ----+ -++++ 1226617. 0.092 -0.269 0.351 0.950 0.324 ---+- ++-++ 772409. 0.114 -0.592 0.806 0.911 0.139 ----- ++-++ 140397. 0.107 -0.428 0.351 0.952 0.210 ---+- ++-++ 695237. 0.097 -0.552 0.116 0.933 0.136 +---+ -++++ 137105. 0.065 -0.837 0.617 0.985 0.065 +-+-- ----+ 1720081. 0.105 -0.508 0.351 0.930 0.163 ---+- ++-++ 1931341. 0.111 -0.574 0.444 0.896 0.142 --+-- +-+-+ 1330385. 0.101 -0.481 0.806 0.934 0.173 ----- ++-++ 1288373. 0.089 -0.455 0.553 1.026 0.176 -++-- -+-+- 49349. 0.113 -0.370 0.351 0.923 0.258 ---+- ++-++ 1503317. 0.108 -0.478 0.566 0.908 0.182 ----- -+++- 1828293. 0.080 -0.353 0.089 0.952 0.238 ----+ -+++- 1802345. 0.073 -0.468 0.556 1.027 0.153 -+--- +++++ 677105. 0.089 -0.425 0.553 1.046 0.195 -++-- -+-+- 1225129. 0.093 -0.441 0.351 0.960 0.189 ---+- ++-++ 1123529. 0.068 -0.850 0.617 0.991 0.068 +-+-- ----+ 245145. 0.120 -0.479 0.351 0.923 0.193 ---+- ++-++ 752045. 0.063 -0.839 0.617 0.990 0.063 +-+-- ----+ 228133. 0.082 -0.438 0.553 1.042 0.179 -++-- -+-+- 1636105. 0.080 -0.479 0.556 1.013 0.153 -+--- +++++ 1708153. 0.078 -0.405 0.556 1.018 0.197 -+--- +++++ 1541353. 0.066 -0.855 0.617 0.989 0.066 +-+-- ----+ 404793. 0.104 -0.469 0.351 0.936 0.183 ---+- ++-++ 170401. 0.072 -0.854 0.617 0.984 0.072 +-+-- ----+ 183361. 0.113 -0.410 0.089 0.919 0.229 ----+ -+++- 1643025. 0.064 -0.843 0.617 0.985 0.064 +-+-- ----+ 852005. 0.082 -0.450 0.556 1.029 0.172 -+--- +++++ 1199129. 0.103 -0.448 0.351 0.942 0.194 ---+- ++-++ 389721. 0.131 -0.465 0.351 0.916 0.212 ---+- ++-++ 500389. 0.066 -0.796 0.617 0.994 0.066 +-+-- ----+ 183389. 0.102 -0.596 0.806 0.908 0.126 ----- ++-++ 594537. 0.097 -0.508 -0.125 0.932 0.155 +---+ -+++- 1948605. 0.089 -0.289 0.556 1.001 0.301 -+--- +++++ 916945. 0.108 -0.517 0.351 0.936 0.162 ---+- ++-++ 1620313. 0.103 -0.511 0.351 0.936 0.160 ---+- ++-++ 1371917. 0.061 -0.836 0.617 0.990 0.061 +-+-- ----+ 390421. 0.066 -0.791 0.617 0.997 0.066 +-+-- ----+ 395469. 0.082 -0.318 0.556 1.021 0.269 -+--- +++++ 1442965. 0.068 -0.850 0.617 0.987 0.068 +-+-- ----+ 549937. 0.076 -0.832 0.617 0.988 0.076 +-+-- ----+ 1277653. 0.065 -0.832 0.617 0.977 0.065 +-+-- ----+ 13773. 0.080 -0.484 0.556 1.026 0.150 -+--- +++++ 349205. 0.084 -0.439 0.556 1.027 0.181 -+--- +++++ 629177. 0.095 -0.439 0.330 0.927 0.192 ----+ -++++ 961701. 0.108 -0.438 0.351 0.941 0.205 ---+- ++-++ 77765. 0.062 -0.850 0.617 0.988 0.062 +-+-- ----+ 742597. 0.089 -0.385 0.351 0.954 0.222 ---+- ++-++ 1672841. 0.092 -0.555 0.943 0.997 0.131 -+--- -+-++ 414597. 0.104 -0.581 0.553 0.977 0.133 -++-- -+-+- 951517. 0.101 -0.416 0.089 0.950 0.212 ----+ -+++- 538237. 0.064 -0.855 0.617 0.993 0.064 +-+-- ----+ 2072749. 0.084 -0.513 0.703 1.021 0.140 -+--- -+-+- 1975137. 0.099 -0.478 0.351 0.946 0.173 ---+- ++-++ 219517. 0.085 -0.246 0.089 0.962 0.339 ----+ -+++- 1478421. 0.075 -0.803 0.376 0.969 0.075 +-+-- ----- 1266245. 0.063 -0.842 0.617 0.976 0.063 +-+-- ----+ 546157. 0.062 -0.848 0.617 0.986 0.062 +-+-- ----+ 1071013. 0.062 -0.812 0.617 0.984 0.062 +-+-- ----+ 2034717. 0.066 -0.848 0.617 0.991 0.066 +-+-- ----+ 1294081. 0.071 -0.825 0.617 0.986 0.071 +-+-- ----+ 917713. 0.067 -0.838 0.617 0.988 0.067 +-+-- ----+ 775393. 0.094 -0.817 0.376 0.956 0.094 +-+-- ----- 2057173. 0.067 -0.840 0.617 0.989 0.067 +-+-- ----+ 1425845. 0.105 -0.754 0.590 0.948 0.105 --+-- ----- 650597. 0.101 -0.737 0.590 0.948 0.101 --+-- ----- 1729233. 0.084 -0.618 0.943 0.993 0.101 -+--- -+-++ 282357. 0.059 -0.836 0.617 0.994 0.059 +-+-- ----+ 1584861. 0.069 -0.816 0.617 0.978 0.069 +-+-- ----+ 505421. 0.069 -0.827 0.617 0.986 0.069 +-+-- ----+ 1808581. 0.061 -0.818 0.617 0.996 0.061 +-+-- ----+ 1677361. 0.062 -0.834 0.617 1.000 0.062 +-+-- ----+ 813869. 0.065 -0.848 0.617 0.979 0.065 +-+-- ----+ 1326181. 0.070 -0.831 0.617 0.987 0.070 +-+-- ----+ 362253. 0.064 -0.854 0.617 0.995 0.064 +-+-- ----+ 141149. 0.065 -0.813 0.617 0.987 0.065 +-+-- ----+ 300401. 0.060 -0.835 0.617 0.998 0.060 +-+-- ----+ 1286521. 0.066 -0.842 0.617 0.990 0.066 +-+-- ----+ 332333. 0.064 -0.827 0.617 0.984 0.064 +-+-- ----+ 1972485. 0.066 -0.816 0.376 0.988 0.066 +-+-- ----- 400469. 0.083 -0.601 0.553 0.995 0.106 -++-- -+-+- 2041553. 0.067 -0.846 0.617 0.990 0.067 +-+-- ----+ 1824129. 0.057 -0.845 0.617 0.998 0.057 +-+-- ----+ CFOM Range Frequency 0.000 - 0.020 0 0.020 - 0.040 0 0.040 - 0.060 4 0.060 - 0.080 51 0.080 - 0.100 1 0.100 - 0.120 7 0.120 - 0.140 23 0.140 - 0.160 39 0.160 - 0.180 30 0.180 - 0.200 24 0.200 - 0.220 20 0.220 - 0.240 9 0.240 - 0.260 16 0.260 - 0.280 8 0.280 - 0.300 3 0.300 - 0.320 5 0.320 - 0.340 5 0.340 - 0.360 2 0.360 - 0.380 3 0.380 - 0.400 2 0.400 - 0.420 0 0.420 - 0.440 3 0.440 - 0.460 0 0.460 - 0.480 0 0.480 - 0.500 0 0.500 - 0.520 0 0.520 - 0.540 0 0.540 - 0.560 1 0.560 - 0.580 0 0.580 - 0.600 0 0.600 - 9.999 0 256. Phase sets refined - best is code 990177. with CFOM = 0.0560 2.2 seconds elapsed time Tangent expanded to 434 out of 434 E greater than 1.200 Highest memory used = 1858 / 2485 0.0 seconds elapsed time FMAP and GRID set by program FMAP 8 1 18 GRID -3.333 -2 -2 3.333 2 2 E-Fourier for p-1 in P2(1) Maximum = 343.00, minimum = -118.42 highest memory used = 8846 / 9362 0.0 seconds elapsed time Peak list optimization RE = 0.283 for 27 surviving atoms and 434 E-values Highest memory used = 1661 / 3906 0.0 seconds elapsed time E-Fourier for p-1 in P2(1) Maximum = 268.66, minimum = -116.91 highest memory used = 8846 / 9362 0.0 seconds elapsed time Peak list optimization RE = 0.245 for 25 surviving atoms and 434 E-values Highest memory used = 1661 / 3906 0.0 seconds elapsed time E-Fourier for p-1 in P2(1) Maximum = 265.66, minimum = -83.91 highest memory used = 8846 / 9362 0.0 seconds elapsed time Molecule 1 scale 1.000 inches = 2.540 cm per Angstrom 24 10 5 30 18 12 1 2 33 6 20 29 36 32 27 21 9 31 Atom Peak x y z SOF Height Distances and Angles 1 266. 0.1600 0.5046 0.1901 1.000 0.89 0 6 1.389 0 18 1.449 129.5 2 257. -0.0199 0.7277 0.2558 1.000 0.02 0 12 1.166 0 20 1.544 127.2 0 29 1.247 170.8 44.8 0 33 1.106 96.9 81.0 86.4 5 247. 0.1003 0.5647 -0.0035 1.000 0.58 0 10 1.139 0 18 1.589 114.0 0 24 1.478 132.0 113.9 0 30 1.311 152.0 38.9 75.1 6 245. 0.1583 0.5089 0.2977 1.000 0.88 0 1 1.389 0 20 1.371 112.3 0 32 1.753 151.5 39.4 0 36 2.002 116.5 45.5 50.9 9 217. 0.1262 0.4370 0.5124 1.000 0.49 0 21 1.229 0 32 1.874 43.5 10 216. 0.1962 0.4729 -0.0201 1.000 1.09 0 5 1.139 12 193. -0.0178 0.7174 0.1657 1.000 0.02 0 2 1.166 0 18 1.450 120.5 0 30 1.527 159.6 39.2 0 33 1.700 40.2 106.8 131.1 18 176. 0.0810 0.6028 0.1161 1.000 0.51 0 1 1.449 0 5 1.589 117.5 0 12 1.450 112.5 129.8 0 30 1.001 172.8 55.4 74.5 20 173. 0.0646 0.6240 0.3352 1.000 0.43 0 2 1.544 0 6 1.371 117.8 0 27 1.357 115.7 126.5 0 29 1.098 53.1 170.5 62.7 0 32 1.112 152.8 89.2 37.4 99.8 0 33 1.753 38.6 111.0 110.6 64.3 137.8 0 36 1.429 103.0 91.2 77.6 93.8 78.6 64.9 21 173. 0.0763 0.5626 0.5145 1.000 0.38 0 9 1.229 0 27 1.368 131.2 0 31 1.725 108.9 118.8 0 32 1.297 95.8 36.0 154.8 24 152. -0.0007 0.6613 -0.0728 1.000 0.04 0 5 1.478 0 30 1.706 48.0 27 112. 0.0359 0.6563 0.4364 1.000 0.28 0 20 1.357 0 21 1.368 122.1 0 29 1.295 48.8 165.8 0 32 0.825 55.0 67.3 103.4 0 36 1.746 53.1 110.5 73.7 68.0 29 96. -0.0198 0.7173 0.3522 1.000 0.00 0 2 1.247 0 20 1.098 82.1 0 27 1.295 150.5 68.5 0 32 1.690 122.5 40.4 28.4 0 33 1.614 43.1 78.0 123.4 108.6 0 36 1.859 95.0 50.1 64.4 54.4 59.2 30 93. 0.0310 0.6618 0.0581 1.000 0.27 0 5 1.311 0 12 1.527 151.7 0 18 1.001 85.7 66.3 0 24 1.706 56.9 150.2 142.3 31 92. 0.0169 0.6062 0.6398 1.000 0.04 0 21 1.725 32 83. 0.0859 0.5831 0.4153 1.000 0.50 0 6 1.753 0 9 1.874 104.0 0 20 1.112 51.5 153.2 0 21 1.297 144.4 40.7 163.6 0 27 0.825 138.9 116.9 87.6 76.7 0 29 1.690 91.2 159.2 39.8 123.9 48.2 0 36 1.628 72.5 129.7 59.4 122.4 84.0 68.1 33 68. 0.1116 0.7798 0.2641 1.000 1.09 0 2 1.106 0 12 1.700 42.9 0 20 1.753 60.5 89.6 0 29 1.614 50.5 93.0 37.8 0 36 1.728 108.4 133.0 48.5 67.5 36 65. 0.2255 0.6959 0.3635 1.000 1.75 0 6 2.002 0 20 1.429 43.2 0 27 1.746 80.7 49.4 0 29 1.859 79.1 36.1 42.0 0 32 1.628 56.6 42.0 28.0 57.5 0 33 1.728 87.4 66.6 95.2 53.3 106.1 Molecule 2 scale 1.000 inches = 2.540 cm per Angstrom 23 8 11 28 14 34 22 17 25 4 35 3 7 15 16 19 13 26 Atom Peak x y z SOF Height Distances and Angles 3 256. 0.4785 0.1828 0.2441 1.000 1.54 0 15 1.489 0 17 1.143 126.9 0 25 1.460 84.9 42.0 0 35 1.863 92.5 94.8 96.2 4 252. 0.6587 0.4031 0.3057 1.000 3.13 0 7 1.309 0 22 1.443 128.8 0 25 1.408 97.5 31.4 7 230. 0.6574 0.4012 0.2042 1.000 3.11 0 4 1.309 0 15 1.411 110.6 8 223. 0.6950 0.4367 0.5218 1.000 3.46 0 11 1.145 0 28 0.805 77.1 11 202. 0.5979 0.3447 0.5053 1.000 2.63 0 8 1.145 0 14 1.257 148.7 0 22 1.704 114.0 35.3 0 23 1.418 128.5 82.1 117.4 0 28 1.245 39.1 131.3 102.8 126.9 13 191. 0.6217 0.4699 -0.0095 1.000 2.90 0 19 1.156 14 183. 0.5319 0.2577 0.4414 1.000 2.04 0 11 1.257 0 17 1.575 157.6 0 22 0.994 97.7 60.0 0 23 1.762 52.9 149.3 150.4 0 25 1.570 121.4 36.3 23.7 173.2 15 182. 0.5584 0.2831 0.1673 1.000 2.24 0 3 1.489 0 7 1.411 118.5 0 16 1.384 119.4 122.0 0 25 1.991 46.9 71.6 166.4 16 182. 0.5379 0.2561 0.0624 1.000 2.05 0 15 1.384 0 19 1.384 125.4 17 181. 0.4830 0.1928 0.3324 1.000 1.59 0 3 1.143 0 14 1.575 158.2 0 22 1.379 119.6 38.6 0 25 0.979 86.6 71.6 33.0 0 34 1.990 116.3 71.6 90.8 107.3 19 174. 0.5740 0.3523 -0.0165 1.000 2.42 0 13 1.156 0 16 1.384 128.1 0 26 1.616 115.4 115.4 22 172. 0.5759 0.3044 0.3771 1.000 2.41 0 4 1.443 0 11 1.704 116.0 0 14 0.994 163.0 47.0 0 17 1.379 115.5 128.4 81.4 0 25 0.771 71.9 172.1 125.1 43.7 23 158. 0.5052 0.2569 0.5771 1.000 1.85 0 11 1.418 0 14 1.762 45.0 25 140. 0.5567 0.2782 0.3215 1.000 2.23 0 3 1.460 0 4 1.408 128.5 0 14 1.570 123.5 108.0 0 15 1.991 48.1 80.3 171.4 0 17 0.979 51.4 178.5 72.1 99.5 0 22 0.771 154.7 76.8 31.2 157.1 103.3 26 140. 0.5059 0.3048 -0.1302 1.000 1.85 0 19 1.616 28 98. 0.6056 0.4781 0.5050 1.000 2.84 0 8 0.805 0 11 1.245 63.8 34 67. 0.2595 0.2569 0.4010 1.000 0.00 0 17 1.990 35 66. 0.6710 0.0572 0.2360 1.000 2.84 0 3 1.863 0.0 seconds elapsed time +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + shelxs finished at 20:50:05 Total elapsed time: 2.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++