+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXS-97 - CRYSTAL STRUCTURE SOLUTION - WinGX VERSION + + Copyright(C) George M. Sheldrick 1986-97 Release 97-2 + + shelxs started at 11:54:22 on 12 Aug 2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0893b in Pna2(1) CELL 0.71073 19.3041 10.1462 13.1353 90.000 90.000 90.000 ZERR 4.00 0.0007 0.0003 0.0005 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5+X, 0.5-Y, Z SYMM 0.5-X, 0.5+Y, 0.5+Z SFAC C H B N O UNIT 128 136 4 4 4 V = 2572.72 At vol = 18.4 F(000) = 984.0 mu = 0.07 mm-1 Max single Patterson vector = 12.1 cell wt = 1837.65 rho = 1.186 OMIT 4.00 180.00 ESEL 1.200 5.000 0.005 0.700 0 INIT 10 16 0.80 0.20 0.20 PHAN 10 0.90 0.40 116 40 10 TREF 256 173 0.90 2 -0.83 HKLF 4 h k l F*F Sigma Why Rejected 0.00 -2.00 1.00 2.08 0.35 Observed but should be systematically absent 0.00 2.00 -1.00 1.65 0.18 Observed but should be systematically absent 0.00 -2.00 -1.00 2.09 0.22 Observed but should be systematically absent 0.00 -2.00 1.00 1.70 0.20 Observed but should be systematically absent 0.00 2.00 1.00 1.98 0.24 Observed but should be systematically absent 0.00 2.00 1.00 1.56 0.24 Observed but should be systematically absent 0.00 2.00 -1.00 2.15 0.28 Observed but should be systematically absent 0.00 5.00 -2.00 1.76 0.29 Observed but should be systematically absent 0.00 5.00 -2.00 1.21 0.30 Observed but should be systematically absent 0.00 -5.00 -2.00 1.72 0.31 Observed but should be systematically absent 0.00 -5.00 2.00 1.38 0.30 Observed but should be systematically absent 0.00 -5.00 2.00 1.99 0.44 Observed but should be systematically absent 0.00 -5.00 -2.00 1.90 0.34 Observed but should be systematically absent 0.00 5.00 2.00 1.96 0.30 Observed but should be systematically absent 0.00 5.00 2.00 1.83 0.27 Observed but should be systematically absent 0.00 6.00 3.00 0.90 0.20 Observed but should be systematically absent 0.00 7.00 6.00 0.95 0.23 Observed but should be systematically absent 0.00 7.00 6.00 1.35 0.29 Observed but should be systematically absent 0.00 6.00 7.00 1.68 0.31 Observed but should be systematically absent 0.00 -1.00 8.00 1.88 0.45 Observed but should be systematically absent -1.00 0.00 8.00 2.79 0.67 Observed but should be systematically absent -3.00 0.00 0.00 0.75 0.08 Observed but should be systematically absent -3.00 0.00 0.00 0.71 0.09 Observed but should be systematically absent 3.00 0.00 0.00 0.89 0.09 Observed but should be systematically absent 3.00 0.00 0.00 0.83 0.10 Observed but should be systematically absent 3.00 0.00 0.00 0.64 0.11 Observed but should be systematically absent 3.00 0.00 -2.00 1.04 0.26 Observed but should be systematically absent 5.00 0.00 0.00 1.54 0.18 Observed but should be systematically absent -5.00 0.00 0.00 1.32 0.16 Observed but should be systematically absent 5.00 0.00 0.00 1.39 0.15 Observed but should be systematically absent 5.00 0.00 0.00 1.43 0.15 Observed but should be systematically absent -5.00 0.00 0.00 1.45 0.17 Observed but should be systematically absent 23246 Reflections read, of which 1177 rejected Maximum h, k, l and 2-Theta = 25. 13. 17. 55.04 3073 Unique reflections, of which 2745 observed R(int) = 0.0440 R(sigma) = 0.0320 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) 7. 21. 63. 84. 114. 133. 97. 132. 169. 241. 339. 472. 652. N(measured) 7. 21. 64. 84. 114. 133. 97. 132. 170. 241. 350. 526. 810. N(theory) 13. 22. 64. 84. 114. 133. 97. 132. 170. 241. 350. 526. 811. 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 = 6703 / 15365 Observed E .GT. 1.200 1.300 1.400 1.500 1.600 1.700 1.800 1.900 2.000 2.100 Number 835 717 606 507 407 343 279 250 209 167 Centric Acentric 0kl h0l hk0 Rest Mean Abs(E*E-1) 0.968 0.736 0.682 0.985 0.885 0.969 0.1 seconds CPU time SUMMARY OF PARAMETERS FOR 2009src0893b in Pna2(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 10 nf 16 s+ 0.800 s- 0.200 wr 0.200 PHAN steps 10 cool 0.900 Boltz 0.400 ns 116 mtpr 40 mnqr 10 TREF np 256. nE 173 kapscal 0.900 ntan 2 wn -0.830 FMAP code 8 PLAN npeaks -50 del1 0.500 del2 1.500 MORE verbosity 1 TIME t 9999999. 116 Reflections and 672. unique TPR for phase annealing 173 Phases refined using 2069. unique TPR 265 Reflections and 4160. unique TPR for R(alpha) 0.1 seconds CPU time 534 Unique negative quartets found, 534 used for phase refinement 0.0 seconds CPU time Highest memory used to derive phase relations = 4841 / 12747 ONE-PHASE SEMINVARIANTS h k l E P+ Phi 10 0 0 3.085 1.00 12 0 0 2.657 0.00 8 0 0 2.017 0.37 2 6 0 1.910 0.57 14 0 0 1.734 0.00 6 0 0 1.536 0.00 0 6 0 1.657 0.00 4 4 0 1.525 0.56 6 4 0 1.470 0.55 8 6 0 1.548 0.52 16 4 0 1.596 0.88 10 4 0 1.404 0.35 Expected value of Sigma-1 = 0.953 Following phases held constant with unit weights for the initial 4 weighted tangent cycles (before phase annealing): h k l E Phase/Comment 10 0 0 3.085 0 sigma-1 = 0.999 12 0 0 2.657 180 sigma-1 = 0.000 7 4 4 2.905 random phase 1 1 2 1.976 random phase 2 6 1 2.453 random phase 3 2 1 2.051 random phase 3 1 3 2.189 random phase 11 2 4 2.026 random phase 3 1 11 2.016 random phase 3 2 2 1.826 random phase 2 1 8 2.177 random phase 6 2 6 1.836 random phase 14 0 0 1.734 180 sigma-1 = 0.002 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 114 Unique NQR employed in phase annealing 128 Parallel refinements, highest memory = 5361 / 48715 0.0 seconds CPU time STRUCTURE SOLUTION for 2009src0893b in Pna2(1) Phase annealing cycle: 1 Beta = 0.10928 Ralpha 0.093 0.210 0.142 0.077 0.080 0.066 0.255 0.308 0.242 0.119 0.075 0.097 0.312 0.162 0.345 0.075 0.084 0.072 0.090 0.102 Nqual -0.048-0.213-0.116 0.223 0.055-0.201-0.267-0.129-0.161-0.275 0.242 0.001-0.209-0.288-0.309-0.125 0.117 0.104-0.370-0.176 Mabs 0.913 0.740 0.830 0.918 0.898 0.915 0.712 0.687 0.725 0.845 0.921 0.874 0.683 0.782 0.669 0.966 0.898 0.937 0.882 0.877 Phase annealing cycle: 2 Beta = 0.12142 Ralpha 0.133 0.354 0.184 0.125 0.094 0.157 0.297 0.417 0.233 0.184 0.122 0.161 0.614 0.314 0.504 0.125 0.169 0.137 0.117 0.108 Nqual -0.482-0.317-0.270-0.025-0.436-0.483-0.493-0.104-0.173-0.566-0.222-0.544-0.470-0.417-0.527-0.581-0.406-0.448-0.437-0.400 Mabs 0.819 0.656 0.774 0.835 0.865 0.789 0.682 0.642 0.733 0.771 0.824 0.773 0.575 0.688 0.599 0.837 0.777 0.804 0.834 0.836 Phase annealing cycle: 3 Beta = 0.13491 Ralpha 0.165 0.331 0.149 0.115 0.096 0.157 0.255 0.205 0.173 0.149 0.128 0.151 0.600 0.322 0.819 0.130 0.170 0.119 0.125 0.127 Nqual -0.387-0.387-0.416-0.157-0.493-0.531-0.498-0.397-0.289-0.568-0.475-0.543-0.394-0.529-0.625-0.428-0.418-0.389-0.537-0.389 Mabs 0.787 0.670 0.798 0.845 0.849 0.802 0.713 0.746 0.761 0.801 0.821 0.795 0.581 0.682 0.531 0.810 0.775 0.837 0.836 0.820 Phase annealing cycle: 4 Beta = 0.14990 Ralpha 0.151 0.271 0.139 0.114 0.153 0.210 0.217 0.184 0.152 0.110 0.145 0.189 0.324 0.310 0.611 0.108 0.117 0.120 0.099 0.130 Nqual -0.490-0.538-0.498-0.215-0.451-0.608-0.608-0.405-0.488-0.482-0.454-0.554-0.447-0.527-0.511-0.460-0.461-0.359-0.542-0.443 Mabs 0.797 0.708 0.806 0.841 0.794 0.746 0.738 0.764 0.785 0.850 0.823 0.762 0.685 0.691 0.572 0.846 0.835 0.841 0.881 0.815 Phase annealing cycle: 5 Beta = 0.16656 Ralpha 0.116 0.207 0.116 0.103 0.138 0.170 0.146 0.113 0.113 0.096 0.145 0.157 0.193 0.176 0.375 0.099 0.114 0.137 0.085 0.134 Nqual -0.532-0.579-0.462-0.237-0.543-0.606-0.536-0.485-0.309-0.504-0.486-0.402-0.615-0.379-0.482-0.413-0.522-0.486-0.605-0.559 Mabs 0.840 0.742 0.860 0.892 0.815 0.788 0.807 0.833 0.819 0.866 0.824 0.795 0.780 0.768 0.648 0.876 0.873 0.816 0.895 0.829 Phase annealing cycle: 6 Beta = 0.18506 Ralpha 0.120 0.208 0.119 0.103 0.117 0.139 0.128 0.115 0.115 0.090 0.144 0.165 0.163 0.170 0.275 0.103 0.110 0.174 0.107 0.125 Nqual -0.648-0.503-0.632-0.424-0.557-0.353-0.470-0.582-0.501-0.406-0.566-0.352-0.511-0.490-0.338-0.489-0.511-0.532-0.633-0.373 Mabs 0.841 0.754 0.835 0.871 0.824 0.820 0.833 0.842 0.828 0.881 0.825 0.786 0.816 0.780 0.700 0.870 0.864 0.786 0.860 0.849 Phase annealing cycle: 7 Beta = 0.20563 Ralpha 0.150 0.245 0.125 0.103 0.172 0.166 0.157 0.120 0.124 0.087 0.164 0.170 0.191 0.202 0.269 0.087 0.127 0.132 0.085 0.124 Nqual -0.684-0.575-0.453-0.317-0.629-0.425-0.525-0.521-0.413-0.498-0.521-0.363-0.426-0.455-0.294-0.610-0.538-0.487-0.534-0.424 Mabs 0.817 0.722 0.829 0.866 0.789 0.793 0.789 0.836 0.833 0.888 0.798 0.779 0.793 0.756 0.702 0.873 0.835 0.816 0.875 0.830 Phase annealing cycle: 8 Beta = 0.22847 Ralpha 0.117 0.257 0.097 0.084 0.094 0.152 0.149 0.109 0.105 0.072 0.122 0.146 0.164 0.150 0.188 0.090 0.108 0.131 0.060 0.096 Nqual -0.658-0.698-0.556-0.354-0.592-0.337-0.536-0.544-0.489-0.584-0.615-0.447-0.509-0.507-0.351-0.561-0.591-0.558-0.601-0.447 Mabs 0.855 0.716 0.871 0.910 0.876 0.820 0.795 0.842 0.838 0.922 0.833 0.814 0.804 0.787 0.765 0.884 0.854 0.831 0.927 0.880 Phase annealing cycle: 9 Beta = 0.25386 Ralpha 0.090 0.191 0.073 0.083 0.067 0.104 0.154 0.100 0.079 0.071 0.115 0.154 0.156 0.143 0.144 0.064 0.086 0.103 0.064 0.083 Nqual -0.582-0.502-0.457-0.302-0.578-0.186-0.609-0.631-0.498-0.559-0.506-0.441-0.475-0.571-0.451-0.609-0.570-0.663-0.626-0.332 Mabs 0.886 0.763 0.928 0.917 0.919 0.867 0.808 0.864 0.867 0.935 0.858 0.809 0.829 0.822 0.799 0.926 0.887 0.864 0.934 0.901 Phase annealing cycle: 10 Beta = 0.28207 Ralpha 0.075 0.143 0.064 0.068 0.066 0.096 0.125 0.084 0.075 0.072 0.119 0.182 0.129 0.114 0.130 0.059 0.063 0.120 0.068 0.087 Nqual -0.502-0.492-0.414-0.237-0.608-0.301-0.674-0.527-0.396-0.554-0.468-0.412-0.603-0.659-0.508-0.628-0.580-0.600-0.565-0.325 Mabs 0.899 0.813 0.942 0.934 0.927 0.880 0.830 0.882 0.885 0.929 0.860 0.799 0.845 0.828 0.825 0.931 0.921 0.858 0.937 0.893 Phase refinement cycle: 1 Ralpha 0.305 0.411 0.263 0.275 0.321 0.384 0.576 0.342 0.374 0.262 0.384 0.472 0.451 0.515 0.408 0.303 0.277 0.481 0.306 0.332 Nqual -0.098-0.019-0.076 0.215-0.559 0.033-0.494-0.165 0.059-0.422-0.032-0.023-0.335-0.352-0.140-0.477-0.535-0.425-0.333 0.093 Mabs 0.694 0.648 0.717 0.711 0.683 0.659 0.588 0.677 0.659 0.714 0.659 0.625 0.630 0.601 0.647 0.692 0.705 0.613 0.692 0.683 Try Ralpha Nqual Sigma-1 M(abs) CFOM Seminvariants 1720229. 0.123 -0.223 0.961 0.920 0.491 +-+-- --++- +- 212537. 0.129 -0.004 0.870 0.934 0.811 +-+-- --++- -- 1062685. 0.100 -0.216 0.961 0.967 0.477 +-+-- --++- +- 1119121. 0.121 0.061 0.961 0.957 0.914 +-+-- --++- +- 1401301. 0.081 -0.608 0.924 0.975 0.130 +-+-- ---++ ++ 715049. 0.130 -0.067 0.961 0.940 0.713 +-+-- --++- +- 1478093. 0.159 -0.350 0.870 0.840 0.389 +-+-- --++- -- 1099009. 0.110 -0.198 0.961 0.939 0.509 +-+-- --++- +- 1300741. 0.117 0.032 0.961 0.936 0.860 +-+-- --++- +- 212249. 0.078 -0.554 0.921 0.980 0.154 +-+-- ---+- ++ 1061245. 0.149 -0.101 0.961 0.885 0.681 +-+-- --++- +- 1111921. 0.134 -0.038 0.870 0.901 0.761 +-+-- --++- -- 1365301. 0.117 -0.387 0.870 0.910 0.314 +-+-- --++- -- 535049. 0.144 -0.412 0.870 0.854 0.319 +-+-- --++- -- 578093. 0.121 -0.029 0.870 0.925 0.762 +-+-- --++- -- 793313. 0.106 -0.516 0.842 0.942 0.205 +-+-- --++- -+ 1869413. 0.076 -0.632 0.921 0.979 0.115* +-+-- ---+- ++ 958457. 0.142 -0.400 0.870 0.861 0.327 +-+-- --++- -- 597981. 0.095 -0.445 0.961 0.964 0.243 +-+-- --++- +- 892753. 0.115 0.078 0.961 0.957 0.939 +-+-- --++- +- 269461. 0.105 -0.363 0.932 0.942 0.324 +-+-- --++- ++ 1347305. 0.131 -0.243 0.961 0.919 0.476 +-+-- --++- +- 445069. 0.114 0.124 0.870 0.959 1.024 +-+-- --++- -- 128193. 0.114 0.113 0.870 0.938 1.004 +-+-- --++- -- 640965. 0.126 -0.142 0.961 0.914 0.600 +-+-- --++- +- 1107673. 0.116 -0.225 0.961 0.940 0.482 +-+-- --++- +- 1344061. 0.119 0.065 0.870 0.927 0.920 +-+-- --++- -- 428849. 0.105 -0.219 0.961 0.948 0.479 +-+-- --++- +- 47093. 0.113 -0.204 0.961 0.953 0.505 +-+-- --++- +- 235465. 0.105 -0.319 0.961 0.942 0.366 +-+-- --++- +- 1177325. 0.112 -0.078 0.961 0.949 0.678 +-+-- --++- +- 1692321. 0.097 -0.440 0.961 0.956 0.249 +-+-- --++- +- 609125. 0.134 -0.118 0.870 0.888 0.640 +-+-- --++- -- 1527209. 0.078 -0.588 0.924 0.982 0.136 +-+-- ---++ ++ 2076861. 0.086 -0.333 0.961 0.973 0.333 +-+-- --++- +- 1254233. 0.107 -0.157 0.961 0.948 0.560 +-+-- --++- +- 948473. 0.103 -0.253 0.961 0.956 0.436 +-+-- --++- +- 1602337. 0.084 -0.523 0.921 0.968 0.178 +-+-- ---+- ++ 1903861. 0.099 -0.518 0.842 0.961 0.196 +-+-- --++- -+ 670277. 0.126 0.115 0.961 0.935 1.020 +-+-- --++- +- 936165. 0.133 -0.400 0.961 0.899 0.318 +-+-- --++- +- 187233. 0.152 -0.374 0.596 0.851 0.360 +-++- -++++ +- 548061. 0.129 -0.297 0.870 0.899 0.413 +-+-- --++- -- 1219633. 0.105 -0.155 0.961 0.954 0.560 +-+-- --++- +- 1004449. 0.106 -0.501 0.870 0.950 0.213 +-+-- --++- -- 2031541. 0.099 -0.547 0.842 0.962 0.179 +-+-- --++- -+ 431489. 0.081 -0.548 0.921 0.973 0.161 +-+-- ---+- ++ 2040077. 0.110 -0.390 0.961 0.939 0.304 +-+-- --++- +- 1811597. 0.160 -0.381 0.465 0.838 0.362 +-+-- -++++ -+ 1246869. 0.105 -0.498 0.842 0.944 0.216 +-+-- --++- -+ 1962537. 0.084 -0.516 0.921 0.975 0.183 +-+-- ---+- ++ 84081. 0.148 -0.279 0.870 0.875 0.452 +-+-- --++- -- 1883197. 0.126 -0.110 0.870 0.906 0.644 +-+-- --++- -- 1507665. 0.103 -0.114 0.961 0.951 0.616 +-+-- --++- +- 495853. 0.100 -0.443 0.961 0.935 0.249 +-+-- --++- +- 197809. 0.097 -0.436 0.961 0.956 0.252 +-+-- --++- +- 626189. 0.121 0.281 0.870 0.955 1.356 +-+-- --++- -- 1822961. 0.149 -0.524 0.870 0.875 0.242 +-+-- --++- -- 1660729. 0.087 -0.448 0.921 0.966 0.233 +-+-- ---+- ++ 247161. 0.097 -0.411 0.961 0.955 0.272 +-+-- --++- +- 1590437. 0.114 -0.207 0.870 0.921 0.502 +-+-- --++- -- 2070229. 0.092 -0.445 0.921 0.955 0.241 +-+-- ---+- ++ 2012189. 0.119 -0.181 0.973 0.935 0.541 +-++- --++- +- 1424077. 0.087 -0.523 0.921 0.963 0.181 +-+-- ---+- ++ 322237. 0.088 -0.531 0.921 0.964 0.177 +-+-- ---+- ++ 1839577. 0.080 -0.561 0.921 0.963 0.153 +-+-- ---+- ++ 562229. 0.110 -0.109 0.961 0.949 0.629 +-+-- --++- +- 384493. 0.099 -0.602 0.842 0.933 0.151 +-+-- --++- -+ 170353. 0.077 -0.581 0.924 0.979 0.139 +-+-- ---++ ++ 1648665. 0.120 -0.068 0.961 0.937 0.701 +-+-- --++- +- 624385. 0.099 -0.589 0.830 0.949 0.157 +-+-- ---+- -+ 322605. 0.080 -0.417 0.961 0.970 0.251 +-+-- --++- +- 2086849. 0.109 0.010 0.961 0.940 0.815 +-+-- --++- +- 1951869. 0.123 -0.290 0.961 0.909 0.415 +-+-- --++- +- 851765. 0.110 -0.434 0.960 0.945 0.267 +-+-- --++- +- 124877. 0.096 -0.604 0.830 0.949 0.147 +-+-- ---+- -+ 1764469. 0.106 -0.480 0.842 0.951 0.229 +-+-- --++- -+ 329733. 0.077 -0.621 0.924 0.984 0.121 +-+-- ---++ ++ 1788325. 0.122 -0.038 0.961 0.941 0.750 +-+-- --++- +- 254229. 0.124 -0.107 0.961 0.923 0.646 +-+-- --++- +- 1583901. 0.096 -0.451 0.961 0.959 0.239 +-+-- --++- +- 2059525. 0.084 -0.558 0.924 0.979 0.158 +-+-- ---++ ++ 1437845. 0.078 -0.608 0.921 0.976 0.127 +-+-- ---+- ++ 1635901. 0.113 -0.014 0.961 0.949 0.779 +-+-- --++- +- 2013313. 0.124 -0.203 0.870 0.894 0.517 +-+-- --++- -- 1771585. 0.135 -0.205 0.870 0.908 0.526 +-+-- --++- -- 1069989. 0.083 -0.588 0.924 0.977 0.141 +-+-- ---++ ++ 749993. 0.110 -0.206 0.973 0.950 0.500 +-++- --++- +- 1888049. 0.128 -0.310 0.961 0.903 0.399 +-+-- --++- +- 891493. 0.119 0.010 0.961 0.938 0.824 +-+-- --++- +- 863405. 0.094 -0.568 0.932 0.956 0.163 +-+-- --++- ++ 147125. 0.115 -0.220 0.961 0.940 0.488 +-+-- --++- +- 1628049. 0.123 0.141 0.870 0.931 1.065 +-+-- --++- -- 1975485. 0.083 -0.558 0.921 0.974 0.157 +-+-- ---+- ++ 1177. 0.164 -0.180 0.961 0.833 0.587 +-+-- --++- +- 613605. 0.078 -0.569 0.921 0.977 0.146 +-+-- ---+- ++ 794721. 0.083 -0.573 0.921 0.988 0.149 +-+-- ---+- ++ 300113. 0.107 -0.209 0.961 0.962 0.493 +-+-- --++- +- 539865. 0.119 -0.191 0.961 0.924 0.528 +-+-- --++- +- 153765. 0.095 -0.358 0.961 0.953 0.318 +-+-- --++- +- 1359313. 0.121 -0.362 0.870 0.910 0.340 +-+-- --++- -- 168765. 0.104 -0.072 0.961 0.957 0.678 +-+-- --++- +- 1339085. 0.085 -0.516 0.921 0.975 0.183 +-+-- ---+- ++ 1407321. 0.104 -0.113 0.961 0.963 0.618 +-+-- --++- +- 923977. 0.147 -0.335 0.961 0.855 0.392 +-+-- --++- +- 1073021. 0.083 -0.498 0.921 0.975 0.193 +-+-- ---+- ++ 842389. 0.116 -0.243 0.961 0.930 0.460 +-+-- --++- +- 119037. 0.087 -0.552 0.921 0.964 0.164 +-+-- ---+- ++ 1129253. 0.099 -0.161 0.961 0.957 0.546 +-+-- --++- +- 968349. 0.105 -0.210 0.961 0.961 0.489 +-+-- --++- +- 1997441. 0.078 -0.637 0.921 0.976 0.116 +-+-- ---+- ++ 2007049. 0.124 0.117 0.870 0.937 1.022 +-+-- --++- -- 2001165. 0.085 -0.564 0.924 0.978 0.156 +-+-- ---++ ++ 2034713. 0.094 -0.544 0.924 0.965 0.176 +-+-- ---++ ++ 225801. 0.124 -0.245 0.961 0.930 0.466 +-+-- --++- +- 1760121. 0.100 -0.380 0.932 0.959 0.303 +-+-- --++- ++ 1832397. 0.089 -0.473 0.921 0.970 0.216 +-+-- ---+- ++ 1532257. 0.103 -0.184 0.961 0.953 0.520 +-+-- --++- +- 460057. 0.122 -0.047 0.870 0.902 0.736 +-+-- --++- -- 1768641. 0.110 -0.340 0.961 0.947 0.350 +-+-- --++- +- 732805. 0.112 -0.210 0.961 0.949 0.496 +-+-- --++- +- 1570385. 0.128 -0.180 0.961 0.931 0.550 +-+-- --++- +- 816265. 0.099 -0.138 0.961 0.963 0.577 +-+-- --++- +- 2050437. 0.115 -0.353 0.973 0.915 0.343 +-++- --++- +- 431177. 0.082 -0.560 0.924 0.969 0.155 +-+-- ---++ ++ 1262989. 0.114 -0.158 0.961 0.947 0.566 +-+-- --++- +- 536177. 0.143 -0.521 0.973 0.869 0.238 +-++- --++- +- 1763957. 0.113 -0.030 0.870 0.937 0.752 +-+-- --++- -- 674829. 0.079 -0.539 0.921 0.982 0.164 +-+-- ---+- ++ 93509. 0.080 -0.549 0.921 0.973 0.159 +-+-- ---+- ++ 447005. 0.081 -0.582 0.924 0.981 0.142 +-+-- ---++ ++ 689365. 0.079 -0.605 0.924 0.978 0.129 +-+-- ---++ ++ 950101. 0.092 -0.572 0.924 0.966 0.159 +-+-- ---++ ++ 1197801. 0.080 -0.576 0.924 0.978 0.145 +-+-- ---++ ++ 1544801. 0.099 -0.577 0.842 0.957 0.164 +-+-- --++- -+ 406613. 0.098 -0.583 0.842 0.943 0.159 +-+-- --++- -+ 377397. 0.078 -0.569 0.921 0.977 0.146 +-+-- ---+- ++ 975469. 0.081 -0.555 0.921 0.980 0.157 +-+-- ---+- ++ 970689. 0.094 -0.603 0.830 0.953 0.146 +-+-- ---+- -+ 1237117. 0.080 -0.551 0.924 0.975 0.158 +-+-- ---++ ++ 1026565. 0.096 -0.600 0.842 0.953 0.149 +-+-- --++- -+ 736017. 0.090 -0.590 0.842 0.961 0.147 +-+-- --++- -+ CFOM Range Frequency 0.000 - 0.020 0 0.020 - 0.040 0 0.040 - 0.060 0 0.060 - 0.080 0 0.080 - 0.100 0 0.100 - 0.120 2 0.120 - 0.140 6 0.140 - 0.160 23 0.160 - 0.180 10 0.180 - 0.200 10 0.200 - 0.220 9 0.220 - 0.240 6 0.240 - 0.260 10 0.260 - 0.280 6 0.280 - 0.300 5 0.300 - 0.320 8 0.320 - 0.340 4 0.340 - 0.360 5 0.360 - 0.380 7 0.380 - 0.400 6 0.400 - 0.420 6 0.420 - 0.440 4 0.440 - 0.460 5 0.460 - 0.480 9 0.480 - 0.500 11 0.500 - 0.520 8 0.520 - 0.540 5 0.540 - 0.560 4 0.560 - 0.580 9 0.580 - 0.600 3 0.600 - 9.999 75 256. Phase sets refined - best is code 1869413. with CFOM = 0.1153 1.0 seconds CPU time Tangent expanded to 835 out of 835 E greater than 1.200 Highest memory used = 3491 / 8242 0.1 seconds CPU time FMAP and GRID set by program FMAP 8 1 23 GRID -1.250 -2 -2 1.250 2 2 E-Fourier for 2009src0893b in Pna2(1) Maximum = 207.30, minimum = -52.78 highest memory used = 8987 / 16216 0.0 seconds CPU time Peak list optimization RE = 0.191 for 36 surviving atoms and 835 E-values Highest memory used = 1802 / 7515 0.0 seconds CPU time E-Fourier for 2009src0893b in Pna2(1) Maximum = 200.60, minimum = -61.03 highest memory used = 8987 / 16216 0.0 seconds CPU time Peak list optimization RE = 0.183 for 35 surviving atoms and 835 E-values Highest memory used = 1802 / 7515 0.0 seconds CPU time E-Fourier for 2009src0893b in Pna2(1) Maximum = 188.59, minimum = -50.06 highest memory used = 8987 / 16216 0.0 seconds CPU time Molecule 1 scale 0.800 inches = 2.033 cm per Angstrom 34 30 35 33 44 41 37 18 24 36 39 26 29 38 15 40 ** 16 31 32 50 19 8 13 42 48 5 20 12 2 49 6 1 10 43 7 11 4 17 3 23 25 9 14 22 21 28 47 46 Atom Peak x y z SOF Height Distances and Angles 1 189. 0.0078 0.2386 0.7635 1.000 1.94 0 5 1.422 0 6 1.399 115.8 0 10 1.617 121.2 122.8 0 48 1.116 96.5 55.2 111.7 0 50 1.602 78.6 78.9 107.0 24.8 2 183. 0.1105 0.0744 0.7635 1.000 3.36 0 10 1.617 0 19 1.435 120.9 0 20 1.374 123.9 114.4 3 165. 0.1258 0.3120 0.6631 1.000 3.18 0 9 1.386 0 10 1.705 122.1 0 14 1.367 115.8 121.3 4 163. 0.0975 0.4281 0.9007 1.000 0.69 0 7 1.412 0 23 1.310 124.9 5 160. -0.0309 0.2368 0.8556 1.000 0.99 0 1 1.422 0 8 1.383 121.6 0 42 1.141 128.8 109.4 0 48 1.905 35.6 99.2 141.6 0 50 1.920 54.8 96.8 125.3 22.7 6 160. -0.0311 0.2372 0.6736 1.000 2.36 0 1 1.399 0 12 1.381 122.1 0 43 1.287 124.8 112.8 0 48 1.192 50.2 104.5 122.3 0 50 1.914 55.2 96.5 126.6 8.1 7 157. 0.1271 0.3101 0.8639 1.000 1.68 0 4 1.412 0 10 1.689 120.7 0 11 1.356 115.2 123.6 8 153. -0.1025 0.2401 0.8556 1.000 0.49 0 5 1.383 0 13 1.418 120.9 9 151. 0.1894 0.2784 0.6214 1.000 4.08 0 3 1.386 0 22 1.376 122.7 10 150. 0.0915 0.2296 0.7643 1.000 2.55 0 1 1.617 0 2 1.617 106.4 0 3 1.705 110.8 112.6 0 7 1.689 112.6 112.6 102.0 11 148. 0.1892 0.2778 0.9053 1.000 1.94 0 7 1.356 0 17 1.376 126.4 12 148. -0.1026 0.2397 0.6744 1.000 1.86 0 6 1.381 0 13 1.371 122.3 0 48 2.039 34.5 98.2 0 49 1.294 120.8 116.7 138.9 13 147. -0.1402 0.2429 0.7629 1.000 0.92 0 8 1.418 0 12 1.371 117.2 14 142. 0.0979 0.4282 0.6298 1.000 2.73 0 3 1.367 0 21 1.375 124.3 15 134. -0.1695 -0.0593 0.6606 1.000 2.82 0 24 1.435 0 26 1.861 125.4 0 40 1.405 105.7 52.3 16 133. 0.1221 -0.2101 0.7633 1.000 4.69 0 31 1.500 0 32 1.265 117.5 17 126. 0.2237 0.3460 0.9803 1.000 1.31 0 11 1.376 0 25 1.477 117.2 18 125. -0.1226 -0.1981 0.7809 1.000 2.84 0 26 1.944 0 29 1.330 97.8 0 30 1.579 97.2 107.6 0 33 2.040 124.6 86.7 134.1 0 35 1.304 92.6 132.8 116.6 50.9 0 36 2.016 123.0 42.2 71.3 96.6 143.3 0 40 1.516 49.4 49.9 99.0 121.7 131.8 76.7 0 41 1.561 145.3 60.7 114.6 36.1 85.5 60.4 109.0 19 123. 0.1122 -0.0003 0.8563 1.000 3.00 0 2 1.435 0 31 1.379 124.6 20 121. 0.1153 -0.0002 0.6765 1.000 4.38 0 2 1.374 0 32 1.466 120.9 21 118. 0.1256 0.5042 0.5534 1.000 3.17 0 14 1.375 0 28 1.343 121.9 0 46 2.028 155.1 33.5 0 47 1.038 117.9 118.2 85.1 22 117. 0.2203 0.3505 0.5452 1.000 4.55 0 9 1.376 0 28 1.492 119.1 23 115. 0.1238 0.5012 0.9733 1.000 0.00 0 4 1.310 0 25 1.466 120.4 24 113. -0.2261 -0.0794 0.7298 1.000 2.00 0 15 1.435 0 30 1.463 95.5 0 37 0.810 131.4 70.8 0 44 1.099 154.5 109.3 65.5 25 113. 0.1915 0.4690 1.0173 1.000 0.27 0 17 1.477 0 23 1.466 115.7 26 108. -0.0970 -0.1770 0.6387 1.000 3.99 0 15 1.861 0 18 1.944 74.4 0 27 1.199 101.8 93.4 0 39 1.150 170.0 96.9 83.5 0 40 1.497 47.9 50.2 65.3 129.7 27 108. -0.0475 -0.1104 0.6583 1.000 3.89 0 26 1.199 0 39 1.564 46.9 0 40 1.476 67.1 104.3 0 45 1.999 97.3 129.8 30.1 28 105. 0.1855 0.4724 0.5074 1.000 4.06 0 21 1.343 0 22 1.492 116.0 0 46 1.173 107.2 136.4 29 103. -0.1093 -0.0756 0.8112 1.000 2.16 0 18 1.330 0 36 1.363 96.9 0 38 1.452 96.8 117.0 0 40 1.212 73.0 119.5 123.4 0 41 1.474 67.4 80.9 49.9 137.5 0 45 1.059 125.8 116.1 103.7 53.7 153.6 30 103. -0.2034 -0.2096 0.7641 1.000 2.46 0 18 1.579 0 24 1.463 105.7 0 37 1.421 102.7 32.6 31 103. 0.1134 -0.1361 0.8613 1.000 3.56 0 16 1.500 0 19 1.379 117.4 32 100. 0.1249 -0.1434 0.6820 1.000 5.03 0 16 1.265 0 20 1.466 124.4 33 94. -0.0567 -0.2579 0.8931 1.000 2.70 0 18 2.040 0 35 1.582 39.7 0 38 1.568 69.1 101.8 0 41 1.206 49.7 87.9 50.8 34 93. -0.0843 -0.4255 0.7673 1.000 4.19 0 35 1.225 35 91. -0.0885 -0.3084 0.7891 1.000 3.49 0 18 1.304 0 33 1.582 89.4 0 34 1.225 147.9 119.4 0 41 1.954 52.8 38.1 148.7 36 82. -0.1699 -0.0555 0.8621 1.000 1.28 0 18 2.016 0 29 1.363 40.9 0 37 1.472 82.9 108.1 0 41 1.842 47.5 52.2 124.9 37 60. -0.2274 -0.0820 0.7914 1.000 1.54 0 24 0.810 0 30 1.421 76.6 0 36 1.472 126.9 94.6 0 44 1.061 70.5 114.8 149.7 38 57. -0.0488 -0.1065 0.8721 1.000 2.25 0 29 1.452 0 33 1.568 103.3 0 41 1.235 66.0 49.2 0 45 1.989 31.1 129.0 97.1 39 50. -0.0570 -0.2607 0.6359 1.000 4.65 0 26 1.150 0 27 1.564 49.6 40 45. -0.1091 -0.0747 0.7190 1.000 2.86 0 15 1.405 0 18 1.516 104.0 0 26 1.497 79.7 80.3 0 27 1.476 113.7 103.1 47.6 0 29 1.212 122.9 57.1 134.4 122.8 0 45 1.034 119.1 112.0 151.7 104.1 55.6 41 45. -0.1003 -0.1730 0.8934 1.000 2.03 0 18 1.561 0 29 1.474 51.9 0 33 1.206 94.1 123.9 0 35 1.954 41.7 88.4 54.0 0 36 1.842 72.1 46.9 166.2 112.6 0 38 1.235 95.6 64.1 79.9 97.5 100.6 42 43. -0.0112 0.2398 0.9376 1.000 0.49 0 5 1.141 43 42. -0.0056 0.2477 0.5835 1.000 3.17 0 6 1.287 44 41. -0.2771 -0.0574 0.7627 1.000 1.31 0 24 1.099 0 37 1.061 44.0 45 39. -0.0924 0.0027 0.7639 1.000 2.29 0 27 1.999 0 29 1.059 96.3 0 38 1.989 89.6 45.1 0 40 1.034 45.7 70.7 96.7 0 50 1.643 87.0 131.7 86.9 132.3 46 37. 0.1994 0.5590 0.4520 1.000 4.19 0 21 2.028 0 28 1.173 39.3 47 36. 0.1070 0.5996 0.5448 1.000 2.69 0 21 1.038 48 35. -0.0162 0.1488 0.7293 1.000 2.43 0 1 1.116 0 5 1.905 47.9 0 6 1.192 74.5 98.4 0 12 2.039 96.5 88.5 41.0 0 50 0.753 116.6 79.8 159.0 118.1 49 35. -0.1373 0.2473 0.5903 1.000 2.22 0 12 1.294 50 34. -0.0209 0.0905 0.7640 1.000 2.39 0 1 1.602 0 5 1.920 46.6 0 6 1.914 45.8 77.1 0 45 1.643 143.1 109.6 109.6 0 48 0.753 38.5 77.5 12.9 121.9 0.0 seconds CPU time +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + shelxs finished at 11:54:23 Total CPU time: 1.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++