++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XS - CRYSTAL STRUCTURE SOLUTION - SHELXTL Ver. 6.12 W95/98/NT/2000/ME + + Copyright(c) 2001 Bruker AXS All Rights Reserved + + shelxs started at 12:08:26 on 06-Mar-2009 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL p21212 in P2(1)2(1)2 CELL 0.71073 11.5691 11.5772 4.6662 90.000 90.000 90.000 ZERR 3.00 0.0004 0.0004 0.0001 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, Z SYMM 0.5-X, 0.5+Y, -Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O BR UNIT 24 24 3 6 3 V = 624.98 At vol = 17.4 F(000) = 342.0 mu = 4.89 mm-1 Max single Patterson vector = 240.3 cell wt = 690.19 rho = 1.834 OMIT 4.00 180.00 ESEL 1.200 5.000 0.005 0.700 0 TREF HKLF 4 7284 Reflections read, of which 34 rejected Maximum h, k, l and 2-Theta = 15. 15. 6. 54.95 866 Unique reflections, of which 840 observed R(int) = 0.0445 R(sigma) = 0.0268 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. 9. 18. 29. 36. 38. 29. 36. 51. 73. 90. 142. 209. N(measured) 4. 9. 18. 29. 36. 39. 29. 36. 51. 73. 91. 144. 224. N(theory) 5. 9. 18. 29. 36. 39. 29. 36. 51. 73. 91. 144. 224. 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 = 1943 / 4330 Observed E .GT. 1.200 1.300 1.400 1.500 1.600 1.700 1.800 1.900 2.000 2.100 Number 275 213 173 149 110 79 64 40 27 16 Centric Acentric 0kl h0l hk0 Rest Mean Abs(E*E-1) 0.968 0.736 0.725 0.873 0.857 0.678 0.0 seconds elapsed time SUMMARY OF PARAMETERS FOR p21212 in P2(1)2(1)2 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 9 nf 16 s+ 0.800 s- 0.200 wr 0.200 PHAN steps 10 cool 0.900 Boltz 0.300 ns 89 mtpr 40 mnqr 10 TREF np 256. nE 118 kapscal 0.850 ntan 3 wn -0.750 FMAP code 8 PLAN npeaks -15 del1 0.500 del2 1.500 MORE verbosity 1 TIME t 9999999. 89 Reflections and 1175. unique TPR for phase annealing 118 Phases refined using 2053. unique TPR 118 Reflections and 2053. unique TPR for R(alpha) 0.0 seconds elapsed time 165 Unique negative quartets found, 165 used for phase refinement 0.0 seconds elapsed time Highest memory used to derive phase relations = 2161 / 8492 ONE-PHASE SEMINVARIANTS h k l E P+ Phi 2 6 0 1.894 0.04 4 0 0 1.628 1.00 2 10 0 2.134 0.93 0 6 0 1.227 1.00 2 4 0 1.609 0.87 4 6 0 1.676 0.95 4 10 0 1.592 0.20 6 6 0 1.370 0.29 6 4 0 1.296 0.64 0 10 2 1.207 0.00 Expected value of Sigma-1 = 0.935 Following phases held constant with unit weights for the initial 4 weighted tangent cycles (before phase annealing): h k l E Phase/Comment 2 6 0 1.894 180 sigma-1 = 0.038 1 4 0 1.620 0 or 180 at random 4 0 0 1.628 0 sigma-1 = 1.000 2 10 0 2.134 0 sigma-1 = 0.930 0 6 0 1.227 0 sigma-1 = 1.000 2 4 0 1.609 0 sigma-1 = 0.866 4 6 0 1.676 0 sigma-1 = 0.947 1 1 3 1.719 random phase 4 1 0 1.461 0 or 180 at random 1 4 1 1.230 random phase 4 10 0 1.592 180 sigma-1 = 0.198 3 1 0 1.400 0 or 180 at random 4 4 1 1.395 random phase 4 3 4 1.687 random phase 9 1 1 1.518 random phase 3 3 1 1.311 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 31 Unique NQR employed in phase annealing 128 Parallel refinements, highest memory = 1791 / 36554 0.0 seconds elapsed time STRUCTURE SOLUTION for p21212 in P2(1)2(1)2 Phase annealing cycle: 1 Beta = 0.05734 Ralpha 0.024 0.022 0.024 0.022 0.021 0.026 0.023 0.028 0.029 0.021 0.022 0.026 0.022 0.021 0.023 0.023 0.029 0.020 0.025 0.032 Nqual -0.014-0.439-0.649-0.545-0.393-0.186-0.584-0.122-0.209-0.542-0.192-0.531-0.694-0.667-0.593-0.333-0.644-0.479-0.571-0.167 Mabs 1.095 1.053 1.159 1.100 1.078 1.160 1.117 1.060 1.019 1.113 1.109 1.141 1.121 1.088 1.107 1.161 1.118 1.077 1.135 1.030 Phase annealing cycle: 2 Beta = 0.06372 Ralpha 0.019 0.023 0.021 0.020 0.021 0.020 0.021 0.019 0.020 0.020 0.020 0.019 0.020 0.019 0.018 0.020 0.020 0.022 0.019 0.019 Nqual -0.832-0.876-0.834-0.873-0.839-0.841-0.841-0.869-0.863-0.845-0.874-0.842-0.837-0.808-0.864-0.854-0.864-0.856-0.815-0.838 Mabs 1.140 1.159 1.145 1.142 1.147 1.142 1.137 1.145 1.150 1.143 1.137 1.136 1.151 1.135 1.131 1.138 1.140 1.155 1.133 1.141 Phase annealing cycle: 3 Beta = 0.07079 Ralpha 0.018 0.021 0.019 0.020 0.022 0.020 0.019 0.023 0.019 0.021 0.022 0.020 0.021 0.020 0.019 0.019 0.019 0.021 0.022 0.021 Nqual -0.866-0.867-0.856-0.851-0.856-0.869-0.846-0.872-0.888-0.883-0.889-0.871-0.890-0.861-0.871-0.842-0.862-0.893-0.864-0.893 Mabs 1.134 1.142 1.141 1.145 1.152 1.137 1.138 1.161 1.136 1.146 1.152 1.149 1.149 1.149 1.136 1.137 1.131 1.142 1.149 1.149 Phase annealing cycle: 4 Beta = 0.07866 Ralpha 0.020 0.020 0.020 0.019 0.021 0.017 0.019 0.018 0.018 0.020 0.021 0.018 0.022 0.021 0.019 0.020 0.020 0.020 0.019 0.018 Nqual -0.876-0.866-0.846-0.877-0.860-0.862-0.840-0.874-0.888-0.846-0.866-0.866-0.889-0.874-0.879-0.859-0.874-0.869-0.845-0.870 Mabs 1.144 1.146 1.146 1.139 1.151 1.128 1.143 1.131 1.127 1.144 1.149 1.133 1.152 1.146 1.139 1.150 1.144 1.142 1.140 1.131 Phase annealing cycle: 5 Beta = 0.08740 Ralpha 0.019 0.019 0.019 0.021 0.018 0.018 0.019 0.019 0.020 0.021 0.022 0.019 0.022 0.019 0.020 0.021 0.021 0.020 0.020 0.020 Nqual -0.863-0.862-0.847-0.876-0.867-0.866-0.860-0.872-0.883-0.854-0.852-0.871-0.885-0.879-0.869-0.882-0.869-0.879-0.874-0.865 Mabs 1.135 1.134 1.138 1.150 1.127 1.130 1.138 1.141 1.143 1.143 1.152 1.142 1.148 1.138 1.143 1.146 1.147 1.144 1.139 1.142 Phase annealing cycle: 6 Beta = 0.09711 Ralpha 0.020 0.022 0.020 0.020 0.021 0.020 0.020 0.022 0.021 0.021 0.020 0.019 0.020 0.020 0.021 0.021 0.019 0.021 0.021 0.020 Nqual -0.875-0.884-0.856-0.882-0.867-0.870-0.871-0.867-0.881-0.870-0.866-0.875-0.892-0.882-0.885-0.871-0.881-0.884-0.890-0.870 Mabs 1.144 1.155 1.147 1.145 1.147 1.146 1.147 1.154 1.147 1.150 1.144 1.141 1.145 1.140 1.149 1.151 1.141 1.151 1.148 1.146 Phase annealing cycle: 7 Beta = 0.10790 Ralpha 0.019 0.021 0.020 0.018 0.021 0.021 0.021 0.020 0.021 0.020 0.023 0.021 0.022 0.019 0.021 0.021 0.021 0.019 0.021 0.021 Nqual -0.878-0.864-0.870-0.870-0.882-0.866-0.870-0.865-0.878-0.866-0.876-0.871-0.887-0.867-0.878-0.866-0.869-0.870-0.886-0.883 Mabs 1.136 1.151 1.147 1.133 1.150 1.151 1.148 1.142 1.148 1.138 1.160 1.147 1.156 1.139 1.147 1.149 1.147 1.140 1.143 1.147 Phase annealing cycle: 8 Beta = 0.11989 Ralpha 0.021 0.021 0.020 0.019 0.019 0.021 0.020 0.020 0.019 0.021 0.020 0.019 0.020 0.019 0.019 0.021 0.020 0.021 0.020 0.021 Nqual -0.874-0.889-0.858-0.877-0.867-0.869-0.870-0.879-0.863-0.870-0.879-0.873-0.854-0.857-0.863-0.850-0.871-0.861-0.865-0.867 Mabs 1.149 1.150 1.148 1.141 1.140 1.146 1.143 1.138 1.136 1.153 1.146 1.139 1.142 1.141 1.145 1.150 1.142 1.148 1.149 1.149 Phase annealing cycle: 9 Beta = 0.13321 Ralpha 0.021 0.019 0.021 0.020 0.020 0.019 0.020 0.019 0.020 0.020 0.022 0.020 0.021 0.020 0.019 0.020 0.019 0.022 0.020 0.020 Nqual -0.867-0.872-0.874-0.873-0.876-0.870-0.872-0.878-0.895-0.871-0.870-0.883-0.886-0.865-0.879-0.881-0.873-0.872-0.869-0.864 Mabs 1.149 1.140 1.147 1.142 1.142 1.142 1.140 1.140 1.145 1.144 1.154 1.145 1.144 1.143 1.137 1.143 1.134 1.152 1.150 1.142 Phase annealing cycle: 10 Beta = 0.14801 Ralpha 0.019 0.020 0.021 0.022 0.020 0.019 0.020 0.020 0.020 0.021 0.020 0.021 0.020 0.019 0.021 0.019 0.021 0.019 0.019 0.019 Nqual -0.871-0.867-0.849-0.886-0.870-0.870-0.862-0.874-0.876-0.880-0.880-0.887-0.874-0.876-0.876-0.869-0.880-0.870-0.867-0.875 Mabs 1.140 1.145 1.144 1.152 1.142 1.137 1.146 1.147 1.143 1.155 1.140 1.150 1.147 1.137 1.146 1.138 1.150 1.140 1.141 1.141 Phase refinement cycle: 1 Ralpha 0.016 0.017 0.016 0.017 0.016 0.016 0.016 0.017 0.016 0.017 0.017 0.016 0.016 0.017 0.016 0.017 0.017 0.016 0.016 0.017 Nqual -0.889-0.903-0.889-0.900-0.895-0.887-0.878-0.902-0.904-0.888-0.895-0.895-0.902-0.897-0.904-0.878-0.889-0.899-0.894-0.903 Mabs 0.990 0.987 0.989 0.989 0.992 0.991 0.993 0.987 0.992 0.986 0.986 0.988 0.989 0.989 0.991 0.985 0.985 0.990 0.992 0.990 Phase refinement cycle: 2 Ralpha 0.033 0.034 0.034 0.033 0.034 0.033 0.033 0.034 0.033 0.034 0.034 0.033 0.033 0.033 0.033 0.033 0.033 0.034 0.033 0.034 Nqual -0.950-0.946-0.944-0.956-0.947-0.948-0.947-0.942-0.948-0.949-0.949-0.950-0.959-0.948-0.947-0.952-0.948-0.947-0.947-0.943 Mabs 1.202 1.202 1.205 1.203 1.204 1.202 1.201 1.205 1.201 1.205 1.206 1.202 1.199 1.202 1.202 1.201 1.204 1.206 1.203 1.204 Try Ralpha Nqual Sigma-1 M(abs) CFOM Seminvariants 1420309. 0.022 -0.950 1.000 1.154 0.022 -++++ +--+- 810089. 0.024 -0.938 1.000 1.159 0.024 -++++ +--+- 1953293. 0.024 -0.934 1.000 1.157 0.024 -++++ +--+- 1377857. 0.023 -0.945 1.000 1.155 0.023 -++++ +--+- 597829. 0.023 -0.935 1.000 1.157 0.023 -++++ +--+- 891993. 0.023 -0.948 1.000 1.152 0.023 -++++ +--+- 265661. 0.023 -0.940 1.000 1.155 0.023 -++++ +--+- 1328305. 0.024 -0.931 1.000 1.157 0.024 -++++ +--+- 350069. 0.023 -0.949 1.000 1.159 0.023 -++++ +--+- 1750345. 0.024 -0.937 1.000 1.158 0.024 -++++ +--+- 363117. 0.023 -0.935 1.000 1.155 0.023 -++++ +--+- 1815585. 0.025 -0.937 1.000 1.163 0.025 -++++ +--+- 689317. 0.023 -0.941 1.000 1.160 0.023 -++++ +--+- 1349433. 0.024 -0.933 1.000 1.156 0.024 -++++ +--+- 455709. 0.024 -0.941 1.000 1.158 0.024 -++++ +--+- 181393. 0.025 -0.928 1.000 1.159 0.025 -++++ +--+- 906965. 0.023 -0.931 1.000 1.158 0.023 -++++ +--+- 340521. 0.024 -0.928 1.000 1.156 0.024 -++++ +--+- 1702605. 0.023 -0.931 1.000 1.156 0.023 -++++ +--+- 124417. 0.023 -0.930 1.000 1.157 0.023 -++++ +--+- 622085. 0.022 -0.940 1.000 1.153 0.022 -++++ +--+- 1013273. 0.023 -0.940 1.000 1.157 0.023 -++++ +--+- 872061. 0.024 -0.936 1.000 1.153 0.024 -++++ +--+- 166001. 0.024 -0.941 1.000 1.158 0.024 -++++ +--+- 830005. 0.023 -0.934 1.000 1.155 0.023 -++++ +--+- 2052873. 0.023 -0.942 1.000 1.156 0.023 -++++ +--+- 1875757. 0.023 -0.948 1.000 1.152 0.023 -++++ +--+- 990177. 0.023 -0.945 1.000 1.154 0.023 -++++ +--+- 756581. 0.024 -0.941 1.000 1.162 0.024 -++++ +--+- 1685753. 0.023 -0.941 1.000 1.150 0.023 -++++ +--+- 40157. 0.023 -0.938 1.000 1.153 0.023 -++++ +--+- 200785. 0.025 -0.933 1.000 1.158 0.025 -++++ +--+- 1131949. 0.023 -0.927 1.000 1.156 0.023 -++++ +--+- 852921. 0.024 -0.944 1.000 1.157 0.024 -++++ +--+- 1035749. 0.024 -0.941 1.000 1.154 0.024 -++++ +--+- 1298669. 0.023 -0.948 1.000 1.157 0.023 -++++ +--+- 1518025. 0.023 -0.941 1.000 1.156 0.023 -++++ +--+- 469885. 0.023 -0.939 1.000 1.158 0.023 -++++ +--+- 1261365. 0.025 -0.938 1.000 1.163 0.025 -++++ +--+- 727901. 0.024 -0.941 1.000 1.155 0.024 -++++ +--+- 1217017. 0.024 -0.943 1.000 1.159 0.024 -++++ +--+- 1465441. 0.024 -0.936 1.000 1.158 0.024 -++++ +--+- 1890781. 0.023 -0.934 1.000 1.153 0.023 -++++ +--+- 1921689. 0.023 -0.951 1.000 1.155 0.023 -++++ +--+- 984441. 0.023 -0.939 1.000 1.155 0.023 -++++ +--+- 1642629. 0.023 -0.947 1.000 1.154 0.023 -++++ +--+- 15369. 0.023 -0.949 1.000 1.154 0.023 -++++ +--+- 1586817. 0.024 -0.925 1.000 1.157 0.024 -++++ +--+- 1955161. 0.024 -0.927 1.000 1.155 0.024 -++++ +--+- 874349. 0.023 -0.945 1.000 1.158 0.023 -++++ +--+- 1206709. 0.023 -0.942 1.000 1.153 0.023 -++++ +--+- 410665. 0.024 -0.926 1.000 1.153 0.024 -++++ +--+- 1391373. 0.023 -0.946 1.000 1.158 0.023 -++++ +--+- 866769. 0.024 -0.940 1.000 1.157 0.024 -++++ +--+- 1447645. 0.025 -0.929 1.000 1.156 0.025 -++++ +--+- 333761. 0.022 -0.949 1.000 1.155 0.022 -++++ +--+- 664841. 0.023 -0.932 1.000 1.152 0.023 -++++ +--+- 905613. 0.023 -0.931 1.000 1.157 0.023 -++++ +--+- 1874237. 0.024 -0.930 1.000 1.158 0.024 -++++ +--+- 1612985. 0.023 -0.934 1.000 1.159 0.023 -++++ +--+- 1187309. 0.024 -0.928 1.000 1.158 0.024 -++++ +--+- 1821593. 0.023 -0.935 1.000 1.159 0.023 -++++ +--+- 1499633. 0.025 -0.939 1.000 1.158 0.025 -++++ +--+- 289529. 0.023 -0.946 1.000 1.155 0.023 -++++ +--+- 726285. 0.022 -0.948 1.000 1.152 0.022 -++++ +--+- 1262745. 0.024 -0.930 1.000 1.158 0.024 -++++ +--+- 608089. 0.024 -0.939 1.000 1.157 0.024 -++++ +--+- 27421. 0.023 -0.936 1.000 1.157 0.023 -++++ +--+- 214973. 0.023 -0.940 1.000 1.154 0.023 -++++ +--+- 522161. 0.023 -0.946 1.000 1.156 0.023 -++++ +--+- 1335213. 0.023 -0.939 1.000 1.153 0.023 -++++ +--+- 943293. 0.024 -0.942 1.000 1.153 0.024 -++++ +--+- 1292065. 0.024 -0.944 1.000 1.160 0.024 -++++ +--+- 1923045. 0.024 -0.923 1.000 1.156 0.024 -++++ +--+- 844345. 0.024 -0.938 1.000 1.159 0.024 -++++ +--+- 1379909. 0.025 -0.928 1.000 1.158 0.025 -++++ +--+- 92485. 0.024 -0.928 1.000 1.152 0.024 -++++ +--+- 1132077. 0.023 -0.949 1.000 1.158 0.023 -++++ +--+- 211797. 0.024 -0.938 1.000 1.160 0.024 -++++ +--+- 471113. 0.024 -0.944 1.000 1.154 0.024 -++++ +--+- 49349. 0.024 -0.942 1.000 1.154 0.024 -++++ +--+- 246745. 0.023 -0.931 1.000 1.160 0.023 -++++ +--+- 637929. 0.023 -0.935 1.000 1.155 0.023 -++++ +--+- 1089381. 0.023 -0.945 1.000 1.154 0.023 -++++ +--+- 1282997. 0.023 -0.935 1.000 1.159 0.023 -++++ +--+- 465057. 0.024 -0.938 1.000 1.158 0.024 -++++ +--+- 1889069. 0.025 -0.936 1.000 1.164 0.025 -++++ +--+- 1708153. 0.023 -0.941 1.000 1.156 0.023 -++++ +--+- 1330385. 0.022 -0.951 1.000 1.152 0.022 -++++ +--+- 1931341. 0.023 -0.940 1.000 1.155 0.023 -++++ +--+- 1663073. 0.022 -0.946 1.000 1.152 0.022* -++++ +--+- 1123529. 0.023 -0.947 1.000 1.156 0.023 -++++ +--+- 568021. 0.024 -0.929 1.000 1.158 0.024 -++++ +--+- 1268097. 0.025 -0.937 1.000 1.160 0.025 -++++ +--+- 360469. 0.024 -0.937 1.000 1.156 0.024 -++++ +--+- 1056737. 0.023 -0.941 1.000 1.153 0.023 -++++ +--+- 800217. 0.023 -0.947 1.000 1.155 0.023 -++++ +--+- 1199129. 0.023 -0.942 1.000 1.158 0.023 -++++ +--+- 303457. 0.023 -0.946 1.000 1.155 0.023 -++++ +--+- 328605. 0.024 -0.932 1.000 1.160 0.024 -++++ +--+- 1923669. 0.024 -0.937 1.000 1.154 0.024 -++++ +--+- 572853. 0.022 -0.950 1.000 1.152 0.022 -++++ +--+- 1467493. 0.023 -0.948 1.000 1.157 0.023 -++++ +--+- 380665. 0.024 -0.930 1.000 1.154 0.024 -++++ +--+- 761253. 0.023 -0.936 1.000 1.156 0.023 -++++ +--+- 953197. 0.024 -0.938 1.000 1.157 0.024 -++++ +--+- 993333. 0.023 -0.936 1.000 1.150 0.023 -++++ +--+- 1479597. 0.023 -0.946 1.000 1.148 0.023 -++++ +--+- 217881. 0.023 -0.947 1.000 1.153 0.023 -++++ +--+- 1796629. 0.025 -0.924 1.000 1.158 0.025 -++++ +--+- 1709113. 0.024 -0.928 1.000 1.156 0.024 -++++ +--+- 367553. 0.024 -0.929 1.000 1.154 0.024 -++++ +--+- 1048437. 0.023 -0.931 1.000 1.157 0.023 -++++ +--+- 1803557. 0.024 -0.935 1.000 1.160 0.024 -++++ +--+- 852829. 0.024 -0.939 1.000 1.164 0.024 -++++ +--+- 1615833. 0.023 -0.943 1.000 1.154 0.023 -++++ +--+- 219517. 0.023 -0.943 1.000 1.155 0.023 -++++ +--+- 2072985. 0.023 -0.948 1.000 1.157 0.023 -++++ +--+- 349205. 0.023 -0.936 1.000 1.154 0.023 -++++ +--+- 629177. 0.023 -0.941 1.000 1.154 0.023 -++++ +--+- 1097585. 0.023 -0.948 1.000 1.154 0.023 -++++ +--+- 341517. 0.023 -0.948 1.000 1.153 0.023 -++++ +--+- 652533. 0.024 -0.931 1.000 1.159 0.024 -++++ +--+- 1944125. 0.025 -0.928 1.000 1.160 0.025 -++++ +--+- 15553. 0.023 -0.946 1.000 1.153 0.023 -++++ +--+- 827117. 0.024 -0.947 1.000 1.159 0.024 -++++ +--+- 853805. 0.024 -0.933 1.000 1.158 0.024 -++++ +--+- 1353721. 0.023 -0.944 1.000 1.154 0.023 -++++ +--+- 1340501. 0.022 -0.947 1.000 1.153 0.022 -++++ +--+- 411049. 0.024 -0.929 1.000 1.161 0.024 -++++ +--+- 2055245. 0.022 -0.950 1.000 1.153 0.022 -++++ +--+- 1887617. 0.024 -0.934 1.000 1.152 0.024 -++++ +--+- 1049477. 0.023 -0.939 1.000 1.157 0.023 -++++ +--+- 1053081. 0.023 -0.946 1.000 1.157 0.023 -++++ +--+- 1071101. 0.023 -0.948 1.000 1.156 0.023 -++++ +--+- 1161201. 0.024 -0.942 1.000 1.155 0.024 -++++ +--+- 1611701. 0.024 -0.930 1.000 1.158 0.024 -++++ +--+- 1767049. 0.022 -0.942 1.000 1.155 0.022 -++++ +--+- 446637. 0.024 -0.927 1.000 1.155 0.024 -++++ +--+- 136033. 0.024 -0.942 1.000 1.156 0.024 -++++ +--+- 680165. 0.023 -0.948 1.000 1.155 0.023 -++++ +--+- 1303673. 0.022 -0.948 1.000 1.154 0.022 -++++ +--+- 226909. 0.023 -0.941 1.000 1.157 0.023 -++++ +--+- 1134545. 0.023 -0.947 1.000 1.156 0.023 -++++ +--+- 1478421. 0.024 -0.929 1.000 1.162 0.024 -++++ +--+- 1100649. 0.024 -0.927 1.000 1.158 0.024 -++++ +--+- 1308941. 0.024 -0.930 1.000 1.154 0.024 -++++ +--+- 253249. 0.023 -0.941 1.000 1.155 0.023 -++++ +--+- 1266245. 0.024 -0.935 1.000 1.158 0.024 -++++ +--+- 39769. 0.024 -0.926 1.000 1.157 0.024 -++++ +--+- 198845. 0.024 -0.937 1.000 1.157 0.024 -++++ +--+- 994225. 0.023 -0.938 1.000 1.156 0.023 -++++ +--+- 776821. 0.023 -0.940 1.000 1.151 0.023 -++++ +--+- 1786953. 0.024 -0.934 1.000 1.158 0.024 -++++ +--+- 546157. 0.024 -0.934 1.000 1.159 0.024 -++++ +--+- 633633. 0.023 -0.941 1.000 1.156 0.023 -++++ +--+- 1071013. 0.023 -0.949 1.000 1.153 0.023 -++++ +--+- 1160761. 0.023 -0.937 1.000 1.156 0.023 -++++ +--+- 1609501. 0.023 -0.948 1.000 1.155 0.023 -++++ +--+- 1756049. 0.022 -0.947 1.000 1.154 0.022 -++++ +--+- 824013. 0.024 -0.935 1.000 1.159 0.024 -++++ +--+- 66757. 0.023 -0.946 1.000 1.159 0.023 -++++ +--+- 2034717. 0.023 -0.924 1.000 1.156 0.023 -++++ +--+- 2053169. 0.023 -0.947 1.000 1.155 0.023 -++++ +--+- 1905633. 0.024 -0.926 1.000 1.159 0.024 -++++ +--+- 1725957. 0.024 -0.929 1.000 1.155 0.024 -++++ +--+- 1870753. 0.023 -0.937 1.000 1.155 0.023 -++++ +--+- 997577. 0.024 -0.935 1.000 1.159 0.024 -++++ +--+- 584233. 0.024 -0.940 1.000 1.162 0.024 -++++ +--+- 769201. 0.024 -0.936 1.000 1.164 0.024 -++++ +--+- 394261. 0.023 -0.938 1.000 1.154 0.023 -++++ +--+- 757645. 0.024 -0.941 1.000 1.160 0.024 -++++ +--+- 965157. 0.024 -0.936 1.000 1.152 0.024 -++++ +--+- 1837833. 0.024 -0.944 1.000 1.157 0.024 -++++ +--+- 355657. 0.023 -0.948 1.000 1.152 0.023 -++++ +--+- 241177. 0.024 -0.941 1.000 1.155 0.024 -++++ +--+- 843181. 0.024 -0.931 1.000 1.157 0.024 -++++ +--+- 391669. 0.023 -0.939 1.000 1.153 0.023 -++++ +--+- 1403117. 0.023 -0.942 1.000 1.152 0.023 -++++ +--+- 1126017. 0.022 -0.930 1.000 1.150 0.022 -++++ +--+- 267325. 0.023 -0.951 1.000 1.157 0.023 -++++ +--+- 1958345. 0.024 -0.938 1.000 1.156 0.024 -++++ +--+- 437537. 0.023 -0.948 1.000 1.155 0.023 -++++ +--+- 1879221. 0.023 -0.946 1.000 1.154 0.023 -++++ +--+- 338589. 0.024 -0.925 1.000 1.159 0.024 -++++ +--+- 1373193. 0.023 -0.933 1.000 1.153 0.023 -++++ +--+- 455133. 0.024 -0.938 1.000 1.157 0.024 -++++ +--+- 1294081. 0.024 -0.931 1.000 1.158 0.024 -++++ +--+- 602973. 0.023 -0.944 1.000 1.155 0.023 -++++ +--+- 76117. 0.023 -0.950 1.000 1.154 0.023 -++++ +--+- 1765229. 0.024 -0.939 1.000 1.161 0.024 -++++ +--+- 887449. 0.023 -0.930 1.000 1.157 0.023 -++++ +--+- 1734193. 0.023 -0.949 1.000 1.155 0.023 -++++ +--+- 1530229. 0.023 -0.944 1.000 1.157 0.023 -++++ +--+- 1315325. 0.023 -0.929 1.000 1.158 0.023 -++++ +--+- 630785. 0.023 -0.934 1.000 1.156 0.023 -++++ +--+- 990865. 0.025 -0.933 1.000 1.158 0.025 -++++ +--+- 2089129. 0.022 -0.948 1.000 1.154 0.022 -++++ +--+- 2057037. 0.024 -0.934 1.000 1.161 0.024 -++++ +--+- 1977397. 0.022 -0.954 1.000 1.154 0.022 -++++ +--+- 2091693. 0.024 -0.936 1.000 1.154 0.024 -++++ +--+- 1314753. 0.023 -0.937 1.000 1.157 0.023 -++++ +--+- 1702953. 0.023 -0.948 1.000 1.158 0.023 -++++ +--+- 1584861. 0.024 -0.945 1.000 1.157 0.024 -++++ +--+- 91813. 0.023 -0.940 1.000 1.155 0.023 -++++ +--+- 837769. 0.023 -0.951 1.000 1.154 0.023 -++++ +--+- 1155833. 0.024 -0.931 1.000 1.158 0.024 -++++ +--+- 1359689. 0.023 -0.949 1.000 1.152 0.023 -++++ +--+- 2052077. 0.024 -0.945 1.000 1.157 0.024 -++++ +--+- 1871777. 0.023 -0.944 1.000 1.156 0.023 -++++ +--+- 1338809. 0.023 -0.939 1.000 1.157 0.023 -++++ +--+- 1342457. 0.023 -0.930 1.000 1.157 0.023 -++++ +--+- 881605. 0.023 -0.950 1.000 1.156 0.023 -++++ +--+- 813869. 0.024 -0.944 1.000 1.157 0.024 -++++ +--+- 255557. 0.023 -0.936 1.000 1.158 0.023 -++++ +--+- 1549301. 0.022 -0.950 1.000 1.154 0.022 -++++ +--+- 102937. 0.023 -0.942 1.000 1.156 0.023 -++++ +--+- 514685. 0.023 -0.945 1.000 1.155 0.023 -++++ +--+- 2095349. 0.024 -0.933 1.000 1.161 0.024 -++++ +--+- 2012945. 0.023 -0.933 1.000 1.154 0.023 -++++ +--+- 1677361. 0.023 -0.939 1.000 1.157 0.023 -++++ +--+- 1768433. 0.024 -0.937 1.000 1.159 0.024 -++++ +--+- 1174333. 0.023 -0.926 1.000 1.158 0.023 -++++ +--+- 284213. 0.023 -0.946 1.000 1.152 0.023 -++++ +--+- 2012861. 0.024 -0.931 1.000 1.157 0.024 -++++ +--+- 1770377. 0.023 -0.945 1.000 1.155 0.023 -++++ +--+- 1864081. 0.023 -0.945 1.000 1.157 0.023 -++++ +--+- 966085. 0.023 -0.941 1.000 1.152 0.023 -++++ +--+- 14521. 0.023 -0.950 1.000 1.153 0.023 -++++ +--+- 440409. 0.023 -0.934 1.000 1.155 0.023 -++++ +--+- 1424717. 0.024 -0.935 1.000 1.158 0.024 -++++ +--+- 104893. 0.024 -0.936 1.000 1.158 0.024 -++++ +--+- 2031797. 0.024 -0.937 1.000 1.157 0.024 -++++ +--+- 1346373. 0.022 -0.948 1.000 1.156 0.022 -++++ +--+- 2061733. 0.023 -0.949 1.000 1.154 0.023 -++++ +--+- 497937. 0.024 -0.940 1.000 1.157 0.024 -++++ +--+- 1928857. 0.023 -0.948 1.000 1.153 0.023 -++++ +--+- 159193. 0.024 -0.935 1.000 1.156 0.024 -++++ +--+- 688705. 0.023 -0.949 1.000 1.155 0.023 -++++ +--+- 2046537. 0.024 -0.924 1.000 1.156 0.024 -++++ +--+- 1276581. 0.023 -0.941 1.000 1.152 0.023 -++++ +--+- 1814097. 0.024 -0.935 1.000 1.156 0.024 -++++ +--+- 1623117. 0.025 -0.930 1.000 1.156 0.025 -++++ +--+- 1094177. 0.023 -0.946 1.000 1.154 0.023 -++++ +--+- 2023973. 0.023 -0.930 1.000 1.158 0.023 -++++ +--+- 565453. 0.023 -0.941 1.000 1.152 0.023 -++++ +--+- 189073. 0.025 -0.937 1.000 1.158 0.025 -++++ +--+- 1270029. 0.023 -0.948 1.000 1.157 0.023 -++++ +--+- 1234897. 0.024 -0.936 1.000 1.157 0.024 -++++ +--+- 1924701. 0.022 -0.946 1.000 1.155 0.022 -++++ +--+- 1044669. 0.024 -0.938 1.000 1.157 0.024 -++++ +--+- 1725329. 0.023 -0.932 1.000 1.153 0.023 -++++ +--+- 1512097. 0.023 -0.935 1.000 1.157 0.023 -++++ +--+- 773865. 0.023 -0.948 1.000 1.153 0.023 -++++ +--+- 827741. 0.023 -0.946 1.000 1.155 0.023 -++++ +--+- 211117. 0.024 -0.937 1.000 1.155 0.024 -++++ +--+- CFOM Range Frequency 0.000 - 0.020 0 0.020 - 0.040 256 0.040 - 0.060 0 0.060 - 0.080 0 0.080 - 0.100 0 0.100 - 0.120 0 0.120 - 0.140 0 0.140 - 0.160 0 0.160 - 0.180 0 0.180 - 0.200 0 0.200 - 0.220 0 0.220 - 0.240 0 0.240 - 0.260 0 0.260 - 0.280 0 0.280 - 0.300 0 0.300 - 0.320 0 0.320 - 0.340 0 0.340 - 0.360 0 0.360 - 0.380 0 0.380 - 0.400 0 0.400 - 0.420 0 0.420 - 0.440 0 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 0 0.560 - 0.580 0 0.580 - 0.600 0 0.600 - 9.999 0 256. Phase sets refined - best is code 1663073. with CFOM = 0.0221 1.0 seconds elapsed time Tangent expanded to 275 out of 275 E greater than 1.200 Highest memory used = 1251 / 2092 0.0 seconds elapsed time FMAP and GRID set by program FMAP 8 3 12 GRID -5.556 -2 -1 5.556 2 1 E-Fourier for p21212 in P2(1)2(1)2 Maximum = 641.80, minimum = -119.91 highest memory used = 8707 / 6226 0.0 seconds elapsed time Heavy-atom assignments: x y z s.o.f. Height BR1 0.2809 0.3385 0.4352 1.0000 641.8 Peak list optimization RE = 0.170 for 8 surviving atoms and 275 E-values Highest memory used = 1522 / 2475 0.0 seconds elapsed time E-Fourier for p21212 in P2(1)2(1)2 Maximum = 667.05, minimum = -132.66 highest memory used = 8715 / 6226 0.0 seconds elapsed time Peak list optimization RE = 0.128 for 10 surviving atoms and 275 E-values Highest memory used = 1530 / 2475 0.0 seconds elapsed time E-Fourier for p21212 in P2(1)2(1)2 Maximum = 673.54, minimum = -109.46 highest memory used = 8715 / 6226 0.0 seconds elapsed time Molecule 1 scale 0.873 inches = 2.217 cm per Angstrom 14 5 BR1 7 15 15 7 1 11 13 2 9 10 12 8 6 4 3 8 Atom Peak x y z SOF Height Distances and Angles BR1 0. 0.2809 0.3385 0.4352 1.000 0.15 0 1 1.932 0 2 1.432 68.0 0 5 1.917 45.0 113.0 0 7 2.783 114.5 77.5 125.5 0 8 3.102 46.2 28.8 89.0 78.0 0 10 2.764 67.8 40.2 102.2 50.7 27.6 0 11 1.858 92.4 60.1 115.2 23.2 55.1 27.6 0 13 1.866 61.5 50.2 91.1 53.6 30.3 12.5 30.9 0 14 1.884 68.2 127.5 33.8 95.8 98.7 96.2 94.6 83.8 0 15 1.960 36.5 70.0 57.4 143.1 65.1 92.6 120.1 91.4 90.6 1 180. 0.2176 0.4840 0.5641 1.000 0.99 0 BR1 1.932 0 2 1.926 43.6 0 5 1.474 66.9 110.5 0 13 1.943 57.6 44.1 103.6 0 15 1.219 73.0 74.8 86.9 118.2 2 162. 0.1572 0.3388 0.4291 1.000 0.00 0 BR1 1.432 0 1 1.926 68.5 0 8 1.972 130.8 70.5 0 10 1.909 110.9 89.9 43.4 0 11 1.689 72.6 98.2 87.8 45.6 0 13 1.452 80.6 68.6 59.7 32.0 35.8 0 15 1.992 67.6 36.2 93.6 124.9 127.9 104.2 3 120. 0.0000 0.5000 1.0785 0.500 2.82 0 4 1.157 4 111. 0.0000 0.5000 0.8306 0.500 1.85 0 3 1.157 0 8 1.320 120.4 2 8 1.320 120.4 119.2 5 94. 0.3450 0.4818 0.5665 1.000 1.13 0 BR1 1.917 0 1 1.474 68.0 0 14 1.106 71.5 111.3 0 15 1.861 62.5 40.9 132.5 6 90. 0.0211 0.2495 1.0142 1.000 1.89 0 10 1.482 0 12 1.339 112.7 7 88. 0.2255 0.1506 0.7807 1.000 0.91 0 BR1 2.783 0 9 1.398 154.7 0 11 1.301 34.3 120.4 3 15 1.998 123.4 80.7 153.5 8 87. 0.0439 0.4120 0.6875 1.000 1.09 0 BR1 3.102 0 2 1.972 20.5 0 4 1.320 138.1 153.8 0 10 1.436 63.0 66.0 128.0 0 13 1.762 32.2 45.4 130.1 35.6 9 71. 0.1617 0.0922 0.9899 1.000 1.49 0 7 1.398 0 12 1.395 117.1 10 71. 0.0953 0.3087 0.8010 1.000 1.30 0 BR1 2.764 0 2 1.909 28.9 0 6 1.482 157.2 155.7 0 8 1.436 89.4 70.6 113.1 0 11 1.410 37.6 58.9 119.6 126.9 0 13 1.025 23.2 48.6 150.0 89.8 44.7 11 68. 0.1985 0.2557 0.7084 1.000 0.90 0 BR1 1.858 0 2 1.689 47.3 0 7 1.301 122.5 143.3 0 10 1.410 114.8 75.4 122.1 0 13 0.992 75.0 59.0 157.1 46.6 12 67. 0.0665 0.1497 1.1056 1.000 2.01 0 6 1.339 0 9 1.395 126.7 13 64. 0.1751 0.3373 0.7371 1.000 1.21 0 BR1 1.866 0 1 1.943 60.9 0 2 1.452 49.2 67.3 0 8 1.762 117.5 74.6 75.0 0 10 1.025 144.4 129.1 99.4 54.6 0 11 0.992 74.1 135.0 85.2 133.2 88.7 14 63. 0.3781 0.4114 0.7040 1.000 1.50 0 BR1 1.884 0 5 1.106 74.7 15 57. 0.2242 0.4890 0.3037 1.000 0.00 0 BR1 1.960 0 1 1.219 70.5 0 2 1.992 42.5 68.9 0 5 1.861 60.2 52.3 93.4 1 7 1.998 142.8 105.0 171.3 87.3 Atom Code x y z Height Symmetry transformation 7 1 0.2745 0.6506 0.2193 0.18 0.5000-X 0.5000+Y 1.0000-Z 8 2 -0.0439 0.5880 0.6875 1.50 0.0000-X 1.0000-Y 0.0000+Z 15 3 0.2758 -0.0110 0.6963 0.18 0.5000-X -0.5000+Y 1.0000-Z 0.0 seconds elapsed time +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + shelxs finished at 12:08:27 Total elapsed time: 1.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++