++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XS - CRYSTAL STRUCTURE SOLUTION - SHELXTL Ver. 6.12 W95/98/NT/2000/ME + + Copyright(c) 2001 Bruker AXS All Rights Reserved + + shelxs started at 18:01:54 on 27-Nov-2008 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL p21212 in P2(1)2(1)2 CELL 0.71073 9.5899 14.5337 4.6028 90.000 90.000 90.000 ZERR 4.00 0.0010 0.0014 0.0003 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 UNIT 40 52 4 8 V = 641.52 At vol = 12.3 F(000) = 384.0 mu = 0.13 mm-1 Max single Patterson vector = 29.1 cell wt = 716.86 rho = 1.856 OMIT 4.00 180.00 ESEL 1.200 5.000 0.005 0.700 0 TREF HKLF 4 6289 Reflections read, of which 39 rejected Maximum h, k, l and 2-Theta = 12. 18. 5. 55.10 894 Unique reflections, of which 809 observed R(int) = 0.0549 R(sigma) = 0.0414 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) 1. 11. 17. 32. 32. 42. 28. 37. 44. 75. 102. 134. 190. N(measured) 1. 11. 17. 34. 33. 42. 29. 39. 45. 76. 104. 140. 227. N(theory) 3. 11. 17. 34. 33. 42. 29. 39. 45. 76. 104. 140. 227. 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 = 1628 / 4470 Observed E .GT. 1.200 1.300 1.400 1.500 1.600 1.700 1.800 1.900 2.000 2.100 Number 243 201 167 139 111 93 74 59 44 35 Centric Acentric 0kl h0l hk0 Rest Mean Abs(E*E-1) 0.968 0.736 0.984 1.161 0.997 0.784 0.1 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 90 mtpr 40 mnqr 10 TREF np 256. nE 120 kapscal 0.850 ntan 3 wn -0.750 FMAP code 8 PLAN npeaks -16 del1 0.500 del2 1.500 MORE verbosity 1 TIME t 9999999. 90 Reflections and 901. unique TPR for phase annealing 116 Phases refined using 1619. unique TPR 116 Reflections and 1619. unique TPR for R(alpha) 0.0 seconds elapsed time 394 Unique negative quartets found, 394 used for phase refinement 0.0 seconds elapsed time Highest memory used to derive phase relations = 2030 / 10520 ONE-PHASE SEMINVARIANTS h k l E P+ Phi 8 8 0 3.240 0.75 2 2 0 2.101 0.76 2 12 0 2.503 1.00 0 0 2 1.346 0.71 6 6 0 1.899 0.27 0 6 2 1.517 0.19 6 10 0 1.990 0.91 0 14 0 1.835 1.00 2 0 4 1.544 0.33 2 4 0 1.256 0.37 0 10 0 1.324 0.60 0 4 4 1.314 0.40 Expected value of Sigma-1 = 0.785 Following phases held constant with unit weights for the initial 4 weighted tangent cycles (before phase annealing): h k l E Phase/Comment 2 1 1 2.468 random phase 2 12 0 2.503 0 sigma-1 = 0.997 0 6 1 2.277 0 or 180 at random 1 1 1 1.976 random phase 3 1 2 2.013 random phase 4 5 0 1.786 0 or 180 at random 1 1 3 1.916 random phase 4 4 3 1.941 random phase 2 5 1 1.631 random phase 0 6 2 1.517 180 sigma-1 = 0.186 6 10 0 1.990 0 sigma-1 = 0.909 0 14 0 1.835 0 sigma-1 = 0.998 4 3 1 1.386 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 126 Unique NQR employed in phase annealing 128 Parallel refinements, highest memory = 3176 / 35093 0.0 seconds elapsed time STRUCTURE SOLUTION for p21212 in P2(1)2(1)2 Phase annealing cycle: 1 Beta = 0.13827 Ralpha 0.136 0.114 0.165 0.055 0.197 0.105 0.099 0.228 0.240 0.190 0.129 0.123 0.133 0.128 0.044 0.306 0.107 0.087 0.181 0.094 Nqual 0.027 0.015-0.263-0.536-0.089-0.083-0.169-0.231 0.016 0.455-0.018-0.254-0.246-0.389-0.751-0.032 0.066 0.149-0.017-0.011 Mabs 0.901 1.001 0.883 1.108 0.772 0.921 1.009 0.807 0.773 0.796 0.958 0.899 0.884 0.933 1.083 0.694 1.022 1.079 0.828 1.063 Phase annealing cycle: 2 Beta = 0.15364 Ralpha 0.122 0.138 0.102 0.043 0.215 0.107 0.080 0.161 0.332 0.193 0.150 0.165 0.145 0.113 0.038 0.486 0.111 0.073 0.198 0.085 Nqual -0.311-0.510-0.562-0.661-0.290-0.445-0.297-0.561-0.387 0.041-0.491-0.474-0.352-0.600-0.765-0.517-0.419-0.274-0.394-0.356 Mabs 0.953 0.911 0.922 1.046 0.758 0.881 0.949 0.823 0.702 0.787 0.880 0.818 0.884 0.913 1.058 0.621 0.926 1.033 0.800 1.023 Phase annealing cycle: 3 Beta = 0.17071 Ralpha 0.118 0.132 0.041 0.039 0.236 0.105 0.073 0.134 0.300 0.181 0.106 0.088 0.108 0.134 0.036 0.576 0.100 0.079 0.186 0.082 Nqual -0.284-0.530-0.750-0.697-0.485-0.563-0.259-0.615-0.486-0.185-0.458-0.421-0.457-0.561-0.775-0.572-0.457-0.312-0.448-0.326 Mabs 0.979 0.920 1.045 1.042 0.759 0.917 0.966 0.875 0.715 0.806 0.944 0.914 0.928 0.898 1.082 0.588 0.949 1.028 0.810 1.058 Phase annealing cycle: 4 Beta = 0.18968 Ralpha 0.109 0.152 0.032 0.037 0.208 0.109 0.096 0.119 0.277 0.180 0.123 0.101 0.119 0.115 0.038 0.426 0.092 0.074 0.219 0.080 Nqual -0.251-0.659-0.784-0.761-0.406-0.533-0.378-0.493-0.480-0.392-0.342-0.482-0.463-0.625-0.775-0.592-0.507-0.347-0.347-0.404 Mabs 0.978 0.873 1.062 1.077 0.781 0.902 0.920 0.902 0.718 0.804 0.948 0.911 0.905 0.917 1.067 0.629 0.955 1.026 0.797 1.036 Phase annealing cycle: 5 Beta = 0.21075 Ralpha 0.118 0.105 0.036 0.040 0.231 0.147 0.092 0.106 0.307 0.189 0.127 0.101 0.096 0.143 0.042 0.479 0.096 0.075 0.218 0.086 Nqual -0.303-0.615-0.776-0.747-0.421-0.414-0.317-0.594-0.548-0.446-0.250-0.462-0.371-0.479-0.731-0.607-0.507-0.285-0.404-0.373 Mabs 0.964 0.918 1.074 1.067 0.768 0.879 0.933 0.901 0.716 0.821 0.935 0.920 0.945 0.904 1.066 0.617 0.943 1.032 0.806 1.028 Phase annealing cycle: 6 Beta = 0.23417 Ralpha 0.105 0.052 0.035 0.039 0.179 0.136 0.067 0.092 0.202 0.102 0.120 0.106 0.102 0.109 0.038 0.335 0.089 0.077 0.144 0.072 Nqual -0.271-0.761-0.785-0.746-0.354-0.479-0.222-0.504-0.594-0.449-0.493-0.491-0.408-0.599-0.732-0.539-0.438-0.350-0.257-0.382 Mabs 0.977 1.047 1.114 1.094 0.808 0.890 0.980 0.937 0.789 0.936 0.967 0.920 0.964 0.943 1.062 0.678 0.984 1.042 0.925 1.053 Phase annealing cycle: 7 Beta = 0.26019 Ralpha 0.118 0.039 0.036 0.040 0.193 0.138 0.071 0.087 0.167 0.069 0.110 0.114 0.104 0.115 0.040 0.224 0.103 0.079 0.097 0.078 Nqual -0.393-0.745-0.769-0.795-0.380-0.469-0.257-0.470-0.628-0.513-0.446-0.458-0.413-0.536-0.781-0.536-0.352-0.341-0.056-0.397 Mabs 0.955 1.093 1.097 1.084 0.784 0.892 0.969 0.957 0.818 1.001 0.957 0.946 0.956 0.956 1.072 0.749 1.005 1.037 1.032 1.044 Phase annealing cycle: 8 Beta = 0.28910 Ralpha 0.110 0.036 0.035 0.036 0.161 0.133 0.079 0.080 0.159 0.066 0.122 0.118 0.108 0.120 0.037 0.125 0.117 0.080 0.086 0.079 Nqual -0.443-0.793-0.788-0.792-0.427-0.531-0.348-0.365-0.681-0.611-0.466-0.460-0.476-0.578-0.792-0.659-0.442-0.286-0.381-0.314 Mabs 0.966 1.099 1.086 1.088 0.799 0.888 0.981 0.991 0.833 1.002 0.957 0.944 0.954 0.939 1.079 0.891 0.987 1.039 1.037 1.057 Phase annealing cycle: 9 Beta = 0.32122 Ralpha 0.122 0.033 0.036 0.037 0.168 0.132 0.078 0.087 0.170 0.066 0.137 0.124 0.109 0.129 0.038 0.089 0.110 0.077 0.101 0.081 Nqual -0.430-0.791-0.786-0.804-0.469-0.563-0.285-0.523-0.680-0.589-0.480-0.483-0.465-0.560-0.789-0.545-0.327-0.262-0.502-0.384 Mabs 0.960 1.091 1.080 1.080 0.819 0.883 0.970 0.960 0.814 0.986 0.957 0.930 0.950 0.935 1.079 0.941 0.992 1.044 0.981 1.020 Phase annealing cycle: 10 Beta = 0.35691 Ralpha 0.111 0.034 0.036 0.038 0.181 0.131 0.078 0.079 0.167 0.067 0.124 0.100 0.105 0.122 0.035 0.072 0.109 0.072 0.109 0.088 Nqual -0.316-0.789-0.791-0.790-0.444-0.562-0.246-0.350-0.702-0.616-0.274-0.501-0.474-0.557-0.797-0.592-0.350-0.265-0.496-0.479 Mabs 0.983 1.101 1.089 1.091 0.814 0.895 0.975 0.989 0.816 0.992 1.007 0.950 0.953 0.954 1.077 0.983 0.989 1.043 0.965 1.001 Phase refinement cycle: 1 Ralpha 0.166 0.045 0.045 0.048 0.311 0.218 0.159 0.128 0.326 0.105 0.160 0.167 0.190 0.181 0.052 0.116 0.149 0.095 0.165 0.142 Nqual -0.113-0.766-0.755-0.789-0.286-0.549-0.087-0.262-0.558-0.604 0.028-0.298-0.338-0.365-0.794-0.564 0.036-0.009-0.291-0.235 Mabs 0.851 0.950 0.952 0.952 0.698 0.759 0.809 0.833 0.681 0.850 0.867 0.811 0.794 0.823 0.936 0.838 0.877 0.922 0.839 0.858 Phase refinement cycle: 2 Ralpha 0.104 0.044 0.043 0.041 0.139 0.108 0.089 0.082 0.163 0.072 0.125 0.114 0.130 0.116 0.044 0.067 0.114 0.090 0.112 0.104 Nqual -0.064-0.868-0.861-0.890-0.233-0.589-0.249-0.417-0.507-0.609 0.130-0.221-0.237-0.285-0.877-0.570 0.187-0.162-0.285-0.277 Mabs 1.069 1.139 1.137 1.133 0.916 0.961 1.018 1.020 0.850 1.025 1.061 0.979 0.956 1.038 1.139 1.032 1.085 1.100 1.060 1.076 Try Ralpha Nqual Sigma-1 M(abs) CFOM Seminvariants 1420309. 0.112 -0.264 0.776 1.003 0.348 +++-+ -++-+ +- 810089. 0.040 -0.867 0.757 1.112 0.040 +++++ -++++ ++ 1953293. 0.039 -0.852 0.757 1.098 0.039 +++++ -++++ ++ 1377857. 0.042 -0.852 0.757 1.115 0.042 +++++ -++++ ++ 597829. 0.143 -0.252 0.839 0.871 0.392 -+++- -+++- +- 891993. 0.114 -0.566 0.744 0.926 0.148 -++-- -++-- -+ 265661. 0.073 -0.309 0.640 0.996 0.268 +++-+ +++-+ +- 1328305. 0.077 -0.365 0.640 0.999 0.226 +++-+ +++-+ +- 350069. 0.170 -0.635 0.035 0.822 0.183 ----+ -++-+ +- 1750345. 0.071 -0.632 0.703 1.006 0.085 -+++- ++++- +- 363117. 0.109 -0.140 0.776 1.016 0.481 +++-+ -++-+ +- 1815585. 0.127 -0.411 0.782 0.945 0.242 -++-- -++-- ++ 689317. 0.130 -0.322 0.782 0.933 0.314 -++-- -++-- ++ 1349433. 0.130 -0.313 0.640 0.982 0.321 +++-+ +++-+ +- 455709. 0.043 -0.851 0.757 1.112 0.043 +++++ -++++ ++ 181393. 0.069 -0.609 0.703 0.995 0.089 -+++- ++++- +- 906965. 0.102 0.110 0.776 1.048 0.841 +++-+ -++-+ +- 340521. 0.098 -0.324 0.640 1.036 0.279 +++-+ +++-+ +- 1702605. 0.124 -0.334 0.640 0.983 0.297 +++-+ +++-+ +- 124417. 0.111 -0.320 0.640 1.023 0.296 +++-+ +++-+ +- 622085. 0.065 -0.651 0.703 1.021 0.075 -+++- ++++- +- 1013273. 0.071 -0.384 0.640 1.003 0.205 +++-+ +++-+ +- 872061. 0.130 -0.411 0.782 0.917 0.245 -++-- -++-- ++ 166001. 0.042 -0.863 0.757 1.109 0.042 +++++ -++++ ++ 830005. 0.129 -0.506 0.858 0.930 0.188 +++++ -++-+ +- 2052873. 0.123 -0.494 0.782 0.918 0.189 -++-- -++-- ++ 1875757. 0.040 -0.851 0.757 1.115 0.040 +++++ -++++ ++ 990177. 0.173 -0.502 0.035 0.828 0.235 ----+ -++-+ +- 756581. 0.040 -0.865 0.757 1.113 0.040 +++++ -++++ ++ 1685753. 0.147 -0.293 0.691 0.900 0.355 -+++- +++-- -+ 40157. 0.041 -0.861 0.757 1.114 0.041 +++++ -++++ ++ 200785. 0.039 -0.861 0.757 1.110 0.039 +++++ -++++ ++ 852921. 0.113 -0.120 0.776 1.013 0.509 +++-+ -++-+ +- 60721. 0.097 -0.365 0.640 0.991 0.245 +++-+ +++-+ +- 1757525. 0.118 -0.083 0.776 1.006 0.563 +++-+ -++-+ +- 252273. 0.125 -0.312 0.776 0.991 0.317 +++-+ -++-+ +- 2017025. 0.127 -0.509 0.722 0.936 0.185 +++++ +++-+ +- 170201. 0.074 -0.247 0.640 0.999 0.327 +++-+ +++-+ +- 1995085. 0.099 0.000 0.776 1.048 0.662 +++-+ -++-+ +- 303605. 0.123 -0.347 0.640 0.996 0.285 +++-+ +++-+ +- 351505. 0.117 -0.175 0.776 1.017 0.448 +++-+ -++-+ +- 1586817. 0.122 -0.316 0.640 0.997 0.310 +++-+ +++-+ +- 1466601. 0.129 -0.395 0.722 0.964 0.256 +++++ +++-+ +- 1135797. 0.114 -0.291 0.640 1.011 0.325 +++-+ +++-+ +- 1132181. 0.121 -0.329 0.640 0.997 0.298 +++-+ +++-+ +- 872901. 0.041 -0.856 0.757 1.111 0.041 +++++ -++++ ++ 76845. 0.113 -0.329 0.640 1.020 0.290 +++-+ +++-+ +- 201889. 0.041 -0.856 0.757 1.114 0.041 +++++ -++++ ++ 644529. 0.117 -0.160 0.776 0.997 0.465 +++-+ -++-+ +- 1415041. 0.122 -0.343 0.858 0.968 0.288 +++++ -++-+ +- 410665. 0.041 -0.864 0.757 1.117 0.041 +++++ -++++ ++ 286329. 0.117 -0.125 0.776 1.006 0.507 +++-+ -++-+ +- 1773469. 0.128 -0.330 0.640 0.975 0.304 +++-+ +++-+ +- 1316197. 0.102 -0.005 0.776 1.045 0.657 +++-+ -++-+ +- 1315557. 0.113 -0.283 0.640 1.012 0.331 +++-+ +++-+ +- 289529. 0.132 -0.356 0.640 0.978 0.287 +++-+ +++-+ +- 1121869. 0.125 -0.327 0.640 0.982 0.304 +++-+ +++-+ +- 719357. 0.100 -0.089 0.776 1.045 0.537 +++-+ -++-+ +- 1187309. 0.096 -0.216 0.776 1.045 0.381 +++-+ -++-+ +- 478737. 0.043 -0.845 0.757 1.118 0.043 +++++ -++++ ++ 1206709. 0.113 -0.255 0.640 1.013 0.357 +++-+ +++-+ +- 241721. 0.041 -0.851 0.757 1.118 0.041 +++++ -++++ ++ 697705. 0.043 -0.846 0.757 1.120 0.043 +++++ -++++ ++ 1742241. 0.129 -0.474 0.722 0.942 0.205 +++++ +++-+ +- 2058549. 0.113 -0.326 0.640 1.022 0.292 +++-+ +++-+ +- 1330473. 0.132 -0.327 0.776 0.988 0.311 +++-+ -++-+ +- 726285. 0.129 -0.341 0.640 0.984 0.296 +++-+ +++-+ +- 603709. 0.132 -0.391 0.722 0.971 0.261 +++++ +++-+ +- 1923045. 0.129 -0.383 0.722 0.965 0.264 +++++ +++-+ +- 1058985. 0.135 -0.365 0.640 0.978 0.283 +++-+ +++-+ +- 137105. 0.137 -0.427 0.722 0.936 0.242 +++++ +++-+ +- 235029. 0.115 -0.298 0.640 1.017 0.319 +++-+ +++-+ +- 608089. 0.072 -0.392 0.640 0.999 0.200 +++-+ +++-+ +- 634117. 0.040 -0.855 0.757 1.116 0.040 +++++ -++++ ++ 1942353. 0.108 -0.275 0.640 1.024 0.334 +++-+ +++-+ +- 435857. 0.042 -0.848 0.757 1.118 0.042 +++++ -++++ ++ 1670001. 0.040 -0.858 0.757 1.112 0.040 +++++ -++++ ++ 462425. 0.041 -0.869 0.757 1.114 0.041 +++++ -++++ ++ 1180021. 0.122 -0.316 0.751 1.002 0.310 +++-+ -++-+ +- 360909. 0.132 -0.472 0.858 0.930 0.210 +++++ -++-+ +- 1770733. 0.039 -0.862 0.757 1.114 0.039* +++++ -++++ ++ 1947681. 0.114 0.100 0.776 1.021 0.836 +++-+ -++-+ +- 49349. 0.117 -0.278 0.640 1.015 0.340 +++-+ +++-+ +- 1268097. 0.108 -0.164 0.776 1.005 0.452 +++-+ -++-+ +- 785089. 0.129 -0.392 0.722 0.964 0.257 +++++ +++-+ +- 2029093. 0.102 -0.009 0.776 1.045 0.650 +++-+ -++-+ +- 1541353. 0.133 -0.289 0.776 0.992 0.346 +++-+ -++-+ +- 991073. 0.132 -0.354 0.640 0.982 0.289 +++-+ +++-+ +- 952465. 0.104 0.009 0.776 1.049 0.679 +++-+ -++-+ +- 2044209. 0.123 -0.324 0.640 0.993 0.305 +++-+ +++-+ +- 1978385. 0.126 -0.339 0.858 0.980 0.295 +++++ -++-+ +- 1423341. 0.152 -0.376 0.858 0.928 0.292 +++++ -++-+ +- 1516877. 0.042 -0.851 0.757 1.115 0.042 +++++ -++++ ++ 123529. 0.116 -0.322 0.640 1.020 0.299 +++-+ +++-+ +- 568021. 0.121 -0.306 0.640 1.004 0.318 +++-+ +++-+ +- 245145. 0.041 -0.861 0.757 1.114 0.041 +++++ -++++ ++ 1517285. 0.114 -0.285 0.640 1.010 0.330 +++-+ +++-+ +- 1229737. 0.103 0.007 0.776 1.052 0.676 +++-+ -++-+ +- 76133. 0.113 -0.060 0.776 1.017 0.588 +++-+ -++-+ +- 1128017. 0.040 -0.855 0.757 1.117 0.040 +++++ -++++ ++ 712929. 0.133 -0.300 0.776 0.988 0.336 +++-+ -++-+ +- 303457. 0.108 -0.289 0.640 1.019 0.320 +++-+ +++-+ +- 1977345. 0.106 0.015 0.776 1.052 0.691 +++-+ -++-+ +- 1035741. 0.040 -0.856 0.757 1.116 0.040 +++++ -++++ ++ 731289. 0.127 -0.352 0.640 0.993 0.286 +++-+ +++-+ +- 767113. 0.040 -0.870 0.757 1.119 0.040 +++++ -++++ ++ 500389. 0.128 -0.327 0.640 0.976 0.307 +++-+ +++-+ +- 1131057. 0.122 -0.326 0.640 0.992 0.302 +++-+ +++-+ +- 1559293. 0.131 -0.324 0.640 0.991 0.312 +++-+ +++-+ +- 1212533. 0.135 -0.338 0.640 0.980 0.304 +++-+ +++-+ +- 1068201. 0.042 -0.853 0.757 1.112 0.042 +++++ -++++ ++ 156957. 0.133 -0.294 0.776 0.990 0.341 +++-+ -++-+ +- 858777. 0.136 -0.339 0.858 0.985 0.304 +++++ -++-+ +- 2038433. 0.132 -0.443 0.722 0.931 0.226 +++++ +++-+ +- 1190989. 0.114 0.062 0.776 1.037 0.773 +++-+ -++-+ +- 344325. 0.117 -0.339 0.640 1.011 0.285 +++-+ +++-+ +- 1785369. 0.102 -0.005 0.776 1.045 0.657 +++-+ -++-+ +- 1975137. 0.130 -0.389 0.722 0.964 0.260 +++++ +++-+ +- 288593. 0.127 -0.355 0.722 0.969 0.283 +++++ +++-+ +- 1944125. 0.126 -0.439 0.722 0.944 0.223 +++++ +++-+ +- 84437. 0.120 -0.294 0.640 1.002 0.328 +++-+ +++-+ +- 923369. 0.121 -0.323 0.640 0.994 0.303 +++-+ +++-+ +- 1428857. 0.112 -0.322 0.640 1.021 0.295 +++-+ +++-+ +- 1417797. 0.040 -0.855 0.757 1.116 0.040 +++++ -++++ ++ 594033. 0.041 -0.856 0.757 1.112 0.041 +++++ -++++ ++ 1887409. 0.041 -0.844 0.757 1.116 0.041 +++++ -++++ ++ 13773. 0.043 -0.846 0.757 1.118 0.043 +++++ -++++ ++ 1803557. 0.131 -0.293 0.776 0.993 0.340 +++-+ -++-+ +- 411049. 0.067 -0.635 0.703 1.013 0.080 -+++- ++++- +- 2055245. 0.041 -0.862 0.757 1.115 0.041 +++++ -++++ ++ 1049477. 0.040 -0.850 0.757 1.116 0.040 +++++ -++++ ++ 1303673. 0.040 -0.856 0.757 1.114 0.040 +++++ -++++ ++ 226909. 0.070 -0.620 0.703 1.010 0.087 -+++- ++++- +- 253249. 0.040 -0.851 0.757 1.105 0.040 +++++ -++++ ++ 39769. 0.040 -0.855 0.757 1.116 0.040 +++++ -++++ ++ 198845. 0.041 -0.850 0.757 1.112 0.041 +++++ -++++ ++ 1609501. 0.042 -0.855 0.757 1.114 0.042 +++++ -++++ ++ 2053169. 0.044 -0.846 0.757 1.121 0.044 +++++ -++++ ++ 793581. 0.044 -0.865 0.757 1.123 0.044 +++++ -++++ ++ 1971305. 0.040 -0.868 0.757 1.113 0.040 +++++ -++++ ++ 824013. 0.042 -0.848 0.757 1.117 0.042 +++++ -++++ ++ 769201. 0.042 -0.852 0.757 1.118 0.042 +++++ -++++ ++ 1835121. 0.041 -0.856 0.757 1.111 0.041 +++++ -++++ ++ 241177. 0.042 -0.847 0.757 1.117 0.042 +++++ -++++ ++ 1048129. 0.042 -0.858 0.757 1.118 0.042 +++++ -++++ ++ 338589. 0.041 -0.851 0.757 1.112 0.041 +++++ -++++ ++ 843181. 0.042 -0.865 0.757 1.108 0.042 +++++ -++++ ++ 421569. 0.041 -0.862 0.757 1.114 0.041 +++++ -++++ ++ 602973. 0.041 -0.866 0.757 1.115 0.041 +++++ -++++ ++ 574509. 0.042 -0.854 0.757 1.113 0.042 +++++ -++++ ++ 1676117. 0.040 -0.849 0.757 1.114 0.040 +++++ -++++ ++ 187989. 0.040 -0.849 0.757 1.112 0.040 +++++ -++++ ++ 630785. 0.042 -0.858 0.757 1.119 0.042 +++++ -++++ ++ 654297. 0.042 -0.862 0.757 1.112 0.042 +++++ -++++ ++ 660433. 0.040 -0.855 0.757 1.116 0.040 +++++ -++++ ++ 983789. 0.041 -0.864 0.757 1.108 0.041 +++++ -++++ ++ 102937. 0.041 -0.857 0.757 1.112 0.041 +++++ -++++ ++ 6713. 0.038 -0.858 0.757 1.104 0.038* +++++ -++++ ++ 2061289. 0.041 -0.857 0.757 1.112 0.041 +++++ -++++ ++ 6605. 0.042 -0.852 0.757 1.115 0.042 +++++ -++++ ++ 420773. 0.041 -0.851 0.757 1.113 0.041 +++++ -++++ ++ 1211677. 0.040 -0.865 0.757 1.113 0.040 +++++ -++++ ++ 1431573. 0.045 -0.853 0.757 1.107 0.045 +++++ -++++ ++ 226253. 0.039 -0.860 0.757 1.110 0.039 +++++ -++++ ++ 404677. 0.040 -0.868 0.757 1.111 0.040 +++++ -++++ ++ 2029453. 0.040 -0.872 0.757 1.114 0.040 +++++ -++++ ++ 419669. 0.042 -0.851 0.757 1.117 0.042 +++++ -++++ ++ 1475609. 0.041 -0.862 0.757 1.112 0.041 +++++ -++++ ++ CFOM Range Frequency 0.000 - 0.020 0 0.020 - 0.040 17 0.040 - 0.060 51 0.060 - 0.080 1 0.080 - 0.100 4 0.100 - 0.120 0 0.120 - 0.140 0 0.140 - 0.160 2 0.160 - 0.180 3 0.180 - 0.200 7 0.200 - 0.220 8 0.220 - 0.240 12 0.240 - 0.260 11 0.260 - 0.280 6 0.280 - 0.300 30 0.300 - 0.320 32 0.320 - 0.340 26 0.340 - 0.360 8 0.360 - 0.380 1 0.380 - 0.400 4 0.400 - 0.420 2 0.420 - 0.440 1 0.440 - 0.460 2 0.460 - 0.480 1 0.480 - 0.500 1 0.500 - 0.520 2 0.520 - 0.540 1 0.540 - 0.560 0 0.560 - 0.580 1 0.580 - 0.600 1 0.600 - 9.999 21 256. Phase sets refined - best is code 6713. with CFOM = 0.0378 1.0 seconds elapsed time Tangent expanded to 243 out of 243 E greater than 1.200 Highest memory used = 1118 / 2443 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 = 343.07, minimum = -82.76 highest memory used = 8710 / 6376 0.0 seconds elapsed time Peak list optimization RE = 0.140 for 10 surviving atoms and 243 E-values Highest memory used = 1525 / 2187 0.0 seconds elapsed time E-Fourier for p21212 in P2(1)2(1)2 Maximum = 329.15, minimum = -92.31 highest memory used = 8710 / 6376 0.0 seconds elapsed time Peak list optimization RE = 0.138 for 10 surviving atoms and 243 E-values Highest memory used = 1525 / 2187 0.0 seconds elapsed time E-Fourier for p21212 in P2(1)2(1)2 Maximum = 331.92, minimum = -77.11 highest memory used = 8710 / 6376 0.0 seconds elapsed time Molecule 1 scale 0.876 inches = 2.226 cm per Angstrom 12 11 13 15 1 2 4 13 15 1 6 5 12 9 3 8 12 14 7 11 15 13 10 16 16 Atom Peak x y z SOF Height Distances and Angles 1 332. 0.5590 0.0662 0.4501 1.000 2.58 0 4 1.324 0 5 1.442 125.4 0 15 1.073 66.9 58.6 2 323. 0.5000 0.0000 0.0253 0.500 0.94 0 4 1.242 0 13 1.496 118.0 0 15 1.574 55.3 125.3 5 13 1.496 118.0 124.0 87.5 7 15 1.574 55.3 87.5 110.5 125.3 3 285. 0.6074 0.2308 0.4432 1.000 2.59 0 5 1.405 0 7 1.425 117.6 4 278. 0.5000 0.0000 0.2951 0.500 1.86 0 1 1.324 0 2 1.242 122.6 0 15 1.338 47.5 75.1 1 1 1.324 114.8 122.6 162.3 7 15 1.338 162.3 75.1 150.1 47.5 5 263. 0.6366 0.1427 0.3335 1.000 2.44 0 1 1.442 0 3 1.405 117.8 0 6 1.383 120.2 122.0 0 15 1.272 46.1 137.6 86.9 6 247. 0.7366 0.1281 0.1222 1.000 2.19 0 5 1.383 0 9 1.392 119.0 0 15 1.828 44.0 148.7 7 236. 0.6825 0.3064 0.3230 1.000 2.43 0 3 1.425 0 8 1.380 120.3 0 10 1.546 115.9 123.9 0 14 1.144 110.7 43.5 114.6 8 226. 0.7819 0.2917 0.1113 1.000 2.17 0 7 1.380 0 9 1.391 120.5 0 11 1.469 121.0 118.5 0 12 1.834 145.2 89.8 33.1 0 14 0.961 55.1 105.8 108.7 137.1 9 221. 0.8096 0.2032 0.0121 1.000 2.06 0 6 1.392 0 8 1.391 120.6 0 14 1.895 102.7 29.2 10 181. 0.6448 0.4024 0.4450 1.000 2.57 0 7 1.546 0 16 1.143 144.8 11 76. 0.8619 0.3686 -0.0119 1.000 2.03 0 8 1.469 0 12 1.003 93.9 0 14 1.997 27.1 117.9 6 13 1.191 124.7 91.4 130.3 12 65. 0.9486 0.3310 -0.0397 1.000 2.37 0 8 1.834 0 11 1.003 53.0 6 13 1.576 87.2 49.0 8 15 1.962 152.8 99.8 72.8 13 63. 0.5762 -0.0757 -0.1272 1.000 0.85 0 2 1.496 2 11 1.191 119.4 3 12 1.576 109.3 39.5 14 61. 0.6845 0.3021 0.0748 1.000 1.60 0 7 1.144 0 8 0.961 81.4 0 9 1.895 101.8 44.9 0 11 1.997 100.8 44.2 78.3 15 57. 0.5695 0.0762 0.2201 1.000 1.83 0 1 1.073 0 2 1.574 115.2 0 4 1.338 65.5 49.7 0 5 1.272 75.3 169.2 140.8 0 6 1.828 112.5 121.4 147.4 49.1 4 12 1.962 117.1 89.5 112.5 87.2 97.5 16 57. 0.5680 0.4623 0.4308 1.000 2.11 0 10 1.143 9 16 1.702 169.7 Atom Code x y z Height Symmetry transformation 1 1 0.4410 -0.0662 0.4501 2.19 1.0000-X 0.0000-Y 0.0000+Z 11 2 0.6381 -0.1314 0.0119 1.67 1.5000-X -0.5000+Y 0.0000-Z 12 3 0.5514 -0.1690 0.0397 1.41 1.5000-X -0.5000+Y 0.0000-Z 12 4 0.4486 0.1690 0.0397 0.57 -0.5000+X 0.5000-Y 0.0000-Z 13 5 0.4238 0.0757 -0.1272 0.00 1.0000-X 0.0000-Y 0.0000+Z 13 6 0.9238 0.4243 0.1272 2.72 1.5000-X 0.5000+Y 0.0000-Z 15 7 0.4305 -0.0762 0.2201 1.38 1.0000-X 0.0000-Y 0.0000+Z 15 8 1.0695 0.4238 -0.2201 2.19 0.5000+X 0.5000-Y 0.0000-Z 16 9 0.4320 0.5377 0.4308 1.41 1.0000-X 1.0000-Y 0.0000+Z 0.0 seconds elapsed time +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + shelxs finished at 18:01:56 Total elapsed time: 1.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++