++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XS - CRYSTAL STRUCTURE SOLUTION - SHELXTL Ver. 6.12 W95/98/NT/2000/ME + + Copyright(c) 2001 Bruker AXS All Rights Reserved + + shelxs started at 15:43:14 on 05-Mar-2009 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL p21212 in P2(1)2(1)2 CELL 0.71073 9.5368 14.7516 4.5621 90.000 90.000 90.000 ZERR 3.00 0.0002 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 21 21 6 3 3 V = 641.81 At vol = 19.4 F(000) = 318.0 mu = 4.75 mm-1 Max single Patterson vector = 247.9 cell wt = 645.17 rho = 1.669 OMIT 4.00 180.00 ESEL 1.200 5.000 0.005 0.700 0 TREF HKLF 4 h k l F*F Sigma Why Rejected 0.00 3.00 0.00 0.84 0.20 Observed but should be systematically absent 12892 Reflections read, of which 79 rejected Maximum h, k, l and 2-Theta = 12. 19. 5. 54.99 889 Unique reflections, of which 872 observed R(int) = 0.0445 R(sigma) = 0.0219 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. 10. 18. 33. 35. 38. 32. 37. 46. 75. 107. 137. 227. N(measured) 1. 10. 18. 33. 35. 38. 32. 37. 46. 76. 107. 138. 232. N(theory) 3. 11. 18. 33. 35. 38. 32. 37. 46. 76. 107. 138. 232. 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 = 1711 / 4445 Observed E .GT. 1.200 1.300 1.400 1.500 1.600 1.700 1.800 1.900 2.000 2.100 Number 268 222 174 135 109 91 71 53 44 33 Centric Acentric 0kl h0l hk0 Rest Mean Abs(E*E-1) 0.968 0.736 0.937 0.911 1.021 0.677 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 1144. unique TPR for phase annealing 120 Phases refined using 2266. unique TPR 129 Reflections and 2563. unique TPR for R(alpha) 0.0 seconds elapsed time 167 Unique negative quartets found, 167 used for phase refinement 0.0 seconds elapsed time Highest memory used to derive phase relations = 2141 / 8582 ONE-PHASE SEMINVARIANTS h k l E P+ Phi 0 6 0 1.388 0.00 0 0 2 1.365 1.00 0 14 0 2.062 1.00 4 6 0 1.703 0.88 0 12 2 1.992 1.00 4 12 0 1.927 0.02 0 6 2 1.666 0.00 0 12 0 1.423 1.00 6 0 0 1.238 1.00 4 8 0 1.246 0.63 Expected value of Sigma-1 = 0.986 Following phases held constant with unit weights for the initial 4 weighted tangent cycles (before phase annealing): h k l E Phase/Comment 0 6 0 1.388 180 sigma-1 = 0.000 0 0 2 1.365 0 sigma-1 = 1.000 0 14 0 2.062 0 sigma-1 = 0.999 4 6 0 1.703 0 sigma-1 = 0.884 0 12 2 1.992 0 sigma-1 = 1.000 2 1 1 1.789 random phase 4 12 0 1.927 180 sigma-1 = 0.023 0 6 2 1.666 180 sigma-1 = 0.001 0 12 0 1.423 0 sigma-1 = 1.000 2 3 2 1.383 random phase 3 0 2 1.573 90 or 270 at random 5 4 2 1.573 random phase 2 1 0 1.367 0 or 180 at random 1 8 0 1.533 0 or 180 at random 0 6 3 1.512 0 or 180 at random 6 0 0 1.238 0 sigma-1 = 1.000 1 0 2 1.229 90 or 270 at random 5 3 2 1.268 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 24 Unique NQR employed in phase annealing 128 Parallel refinements, highest memory = 1639 / 36889 0.0 seconds elapsed time STRUCTURE SOLUTION for p21212 in P2(1)2(1)2 Phase annealing cycle: 1 Beta = 0.05309 Ralpha 0.030 0.023 0.022 0.037 0.028 0.023 0.029 0.020 0.021 0.023 0.018 0.023 0.027 0.025 0.025 0.023 0.026 0.022 0.022 0.579 Nqual -0.627-0.606-0.604-0.535-0.595-0.798-0.499-0.712-0.634-0.716-0.524-0.648-0.462-0.637-0.605-0.711-0.447-0.709-0.526-0.499 Mabs 1.078 1.149 1.128 1.044 1.068 1.162 1.092 1.094 1.122 1.142 1.105 1.144 1.044 1.102 1.107 1.109 1.127 1.142 1.072 0.591 Phase annealing cycle: 2 Beta = 0.05899 Ralpha 0.016 0.017 0.015 0.017 0.016 0.017 0.014 0.014 0.017 0.016 0.017 0.017 0.018 0.018 0.015 0.016 0.017 0.017 0.016 0.367 Nqual -0.850-0.837-0.862-0.873-0.870-0.836-0.865-0.831-0.842-0.843-0.857-0.832-0.875-0.841-0.859-0.865-0.854-0.866-0.863-0.713 Mabs 1.114 1.120 1.115 1.117 1.119 1.117 1.101 1.105 1.119 1.114 1.116 1.119 1.133 1.123 1.110 1.119 1.115 1.128 1.123 0.675 Phase annealing cycle: 3 Beta = 0.06554 Ralpha 0.017 0.017 0.018 0.017 0.018 0.018 0.019 0.019 0.020 0.017 0.017 0.018 0.018 0.017 0.018 0.018 0.018 0.017 0.018 0.245 Nqual -0.869-0.862-0.895-0.893-0.870-0.867-0.893-0.873-0.861-0.851-0.881-0.869-0.868-0.887-0.864-0.871-0.878-0.876-0.873-0.833 Mabs 1.129 1.129 1.127 1.129 1.134 1.129 1.131 1.136 1.133 1.124 1.122 1.123 1.122 1.117 1.128 1.127 1.135 1.120 1.132 0.765 Phase annealing cycle: 4 Beta = 0.07283 Ralpha 0.017 0.017 0.019 0.018 0.017 0.017 0.018 0.017 0.018 0.016 0.017 0.015 0.016 0.018 0.019 0.018 0.018 0.017 0.017 0.083 Nqual -0.882-0.866-0.874-0.864-0.872-0.863-0.871-0.879-0.850-0.866-0.877-0.869-0.901-0.902-0.879-0.890-0.889-0.870-0.891-0.378 Mabs 1.122 1.134 1.129 1.127 1.132 1.128 1.118 1.123 1.122 1.123 1.119 1.121 1.121 1.135 1.136 1.130 1.121 1.131 1.130 0.944 Phase annealing cycle: 5 Beta = 0.08092 Ralpha 0.017 0.018 0.016 0.018 0.017 0.019 0.017 0.019 0.017 0.018 0.017 0.017 0.017 0.015 0.017 0.016 0.016 0.019 0.018 0.018 Nqual -0.872-0.864-0.883-0.852-0.873-0.859-0.901-0.863-0.860-0.848-0.886-0.853-0.885-0.895-0.875-0.876-0.896-0.865-0.890-0.874 Mabs 1.126 1.125 1.119 1.131 1.120 1.132 1.118 1.125 1.125 1.132 1.123 1.118 1.120 1.113 1.125 1.118 1.120 1.135 1.129 1.126 Phase annealing cycle: 6 Beta = 0.08991 Ralpha 0.017 0.018 0.019 0.017 0.018 0.017 0.018 0.019 0.018 0.019 0.017 0.019 0.017 0.018 0.018 0.019 0.018 0.017 0.020 0.016 Nqual -0.890-0.872-0.897-0.883-0.861-0.866-0.901-0.878-0.878-0.869-0.872-0.878-0.884-0.884-0.877-0.885-0.878-0.867-0.899-0.881 Mabs 1.133 1.134 1.134 1.124 1.124 1.127 1.133 1.136 1.131 1.138 1.124 1.129 1.126 1.129 1.127 1.133 1.131 1.126 1.135 1.121 Phase annealing cycle: 7 Beta = 0.09990 Ralpha 0.017 0.019 0.020 0.017 0.018 0.019 0.019 0.018 0.018 0.016 0.018 0.018 0.019 0.020 0.019 0.017 0.019 0.018 0.019 0.018 Nqual -0.883-0.881-0.884-0.901-0.875-0.862-0.885-0.870-0.891-0.877-0.889-0.885-0.888-0.881-0.870-0.898-0.883-0.874-0.875-0.860 Mabs 1.127 1.132 1.139 1.129 1.129 1.135 1.132 1.129 1.130 1.125 1.132 1.128 1.133 1.134 1.136 1.127 1.125 1.130 1.129 1.129 Phase annealing cycle: 8 Beta = 0.11100 Ralpha 0.018 0.017 0.017 0.019 0.020 0.018 0.017 0.019 0.019 0.018 0.016 0.019 0.019 0.017 0.020 0.019 0.018 0.019 0.017 0.018 Nqual -0.851-0.876-0.871-0.895-0.872-0.863-0.884-0.881-0.876-0.865-0.888-0.867-0.879-0.898-0.877-0.883-0.899-0.874-0.890-0.874 Mabs 1.132 1.124 1.125 1.133 1.138 1.127 1.128 1.130 1.135 1.134 1.118 1.133 1.135 1.129 1.137 1.134 1.133 1.137 1.128 1.126 Phase annealing cycle: 9 Beta = 0.12333 Ralpha 0.019 0.016 0.019 0.018 0.020 0.019 0.019 0.018 0.019 0.018 0.018 0.018 0.018 0.018 0.020 0.019 0.017 0.019 0.019 0.018 Nqual -0.863-0.871-0.867-0.871-0.862-0.870-0.873-0.882-0.895-0.889-0.898-0.868-0.894-0.886-0.886-0.868-0.879-0.869-0.882-0.865 Mabs 1.137 1.118 1.132 1.131 1.137 1.138 1.131 1.132 1.139 1.129 1.132 1.129 1.132 1.127 1.136 1.129 1.126 1.132 1.136 1.132 Phase annealing cycle: 10 Beta = 0.13704 Ralpha 0.017 0.018 0.019 0.018 0.017 0.017 0.020 0.019 0.018 0.021 0.019 0.017 0.018 0.018 0.019 0.019 0.018 0.018 0.018 0.018 Nqual -0.872-0.859-0.889-0.886-0.862-0.863-0.872-0.876-0.884-0.879-0.870-0.888-0.906-0.877-0.865-0.883-0.883-0.864-0.899-0.859 Mabs 1.128 1.131 1.139 1.128 1.132 1.127 1.140 1.140 1.128 1.140 1.133 1.124 1.134 1.130 1.126 1.137 1.134 1.133 1.129 1.131 Phase refinement cycle: 1 Ralpha 0.027 0.027 0.028 0.027 0.027 0.027 0.027 0.028 0.028 0.027 0.028 0.027 0.028 0.027 0.027 0.028 0.028 0.026 0.029 0.027 Nqual -0.856-0.857-0.857-0.852-0.856-0.859-0.853-0.850-0.842-0.853-0.853-0.844-0.854-0.858-0.851-0.857-0.860-0.859-0.861-0.865 Mabs 0.936 0.938 0.934 0.936 0.938 0.937 0.938 0.936 0.934 0.939 0.934 0.936 0.934 0.936 0.940 0.937 0.936 0.939 0.933 0.938 Phase refinement cycle: 2 Ralpha 0.033 0.033 0.033 0.034 0.033 0.033 0.034 0.033 0.033 0.033 0.033 0.034 0.033 0.034 0.033 0.033 0.033 0.034 0.032 0.034 Nqual -0.896-0.904-0.897-0.898-0.904-0.902-0.907-0.907-0.897-0.903-0.897-0.897-0.905-0.901-0.905-0.904-0.898-0.900-0.899-0.903 Mabs 1.200 1.200 1.199 1.200 1.201 1.199 1.202 1.199 1.200 1.202 1.202 1.202 1.201 1.202 1.200 1.202 1.200 1.201 1.198 1.202 Try Ralpha Nqual Sigma-1 M(abs) CFOM Seminvariants 1420309. 0.021 -0.896 1.000 1.132 0.021 -++++ --+++ 810089. 0.021 -0.898 1.000 1.131 0.021 -++++ --+++ 1953293. 0.021 -0.891 1.000 1.136 0.021 -++++ --+++ 1377857. 0.022 -0.895 1.000 1.136 0.022 -++++ --+++ 597829. 0.021 -0.896 1.000 1.132 0.021 -++++ --+++ 891993. 0.021 -0.897 1.000 1.132 0.021 -++++ --+++ 265661. 0.021 -0.911 1.000 1.132 0.021 -++++ --+++ 1328305. 0.021 -0.899 1.000 1.131 0.021 -++++ --+++ 350069. 0.021 -0.892 1.000 1.134 0.021 -++++ --+++ 1750345. 0.021 -0.896 1.000 1.132 0.021 -++++ --+++ 363117. 0.021 -0.899 1.000 1.132 0.021 -++++ --+++ 1815585. 0.021 -0.895 1.000 1.135 0.021 -++++ --+++ 689317. 0.021 -0.897 1.000 1.133 0.021 -++++ --+++ 1349433. 0.022 -0.906 1.000 1.138 0.022 -++++ --+++ 455709. 0.021 -0.899 1.000 1.132 0.021 -++++ --+++ 181393. 0.021 -0.898 1.000 1.134 0.021 -++++ --+++ 906965. 0.021 -0.890 1.000 1.133 0.021 -++++ --+++ 340521. 0.021 -0.897 1.000 1.133 0.021 -++++ --+++ 1702605. 0.020 -0.897 1.000 1.131 0.020* -++++ --+++ 124417. 0.021 -0.912 1.000 1.132 0.021 -++++ --+++ 622085. 0.022 -0.911 1.000 1.135 0.022 -++++ --+++ 1013273. 0.021 -0.907 1.000 1.137 0.021 -++++ --+++ 872061. 0.021 -0.889 1.000 1.133 0.021 -++++ --+++ 166001. 0.021 -0.898 1.000 1.131 0.021 -++++ --+++ 830005. 0.021 -0.899 1.000 1.133 0.021 -++++ --+++ 2052873. 0.022 -0.909 1.000 1.139 0.022 -++++ --+++ 1875757. 0.021 -0.909 1.000 1.130 0.021 -++++ --+++ 990177. 0.021 -0.891 1.000 1.133 0.021 -++++ --+++ 756581. 0.022 -0.894 1.000 1.138 0.022 -++++ --+++ 1685753. 0.021 -0.890 1.000 1.136 0.021 -++++ --+++ 40157. 0.022 -0.895 1.000 1.138 0.022 -++++ --+++ 200785. 0.022 -0.907 1.000 1.136 0.022 -++++ --+++ 15369. 0.021 -0.898 1.000 1.133 0.021 -++++ --+++ 872901. 0.022 -0.910 1.000 1.135 0.022 -++++ --+++ 1484681. 0.021 -0.897 1.000 1.131 0.021 -++++ --+++ 170201. 0.021 -0.898 1.000 1.134 0.021 -++++ --+++ 1035749. 0.021 -0.897 1.000 1.133 0.021 -++++ --+++ 80681. 0.021 -0.892 1.000 1.133 0.021 -++++ --+++ 1132181. 0.021 -0.898 1.000 1.131 0.021 -++++ --+++ 1642629. 0.021 -0.892 1.000 1.134 0.021 -++++ --+++ 399017. 0.021 -0.896 1.000 1.135 0.021 -++++ --+++ 469885. 0.021 -0.890 1.000 1.133 0.021 -++++ --+++ 70301. 0.021 -0.895 1.000 1.134 0.021 -++++ --+++ 1466601. 0.022 -0.893 1.000 1.137 0.022 -++++ --+++ 852921. 0.021 -0.907 1.000 1.135 0.021 -++++ --+++ 1217017. 0.021 -0.895 1.000 1.134 0.021 -++++ --+++ 76845. 0.021 -0.895 1.000 1.136 0.021 -++++ --+++ 384225. 0.022 -0.895 1.000 1.137 0.022 -++++ --+++ 982577. 0.022 -0.912 1.000 1.135 0.022 -++++ --+++ 1742241. 0.021 -0.892 1.000 1.138 0.021 -++++ --+++ 2053325. 0.021 -0.898 1.000 1.129 0.021 -++++ --+++ 322597. 0.021 -0.897 1.000 1.132 0.021 -++++ --+++ 1447645. 0.021 -0.891 1.000 1.136 0.021 -++++ --+++ 1495753. 0.021 -0.903 1.000 1.133 0.021 -++++ --+++ 719357. 0.022 -0.894 1.000 1.137 0.022 -++++ --+++ 866769. 0.021 -0.895 1.000 1.133 0.021 -++++ --+++ 1940833. 0.021 -0.896 1.000 1.134 0.021 -++++ --+++ 874349. 0.021 -0.899 1.000 1.132 0.021 -++++ --+++ 1940961. 0.022 -0.909 1.000 1.137 0.022 -++++ --+++ 289529. 0.021 -0.896 1.000 1.135 0.021 -++++ --+++ 1955161. 0.021 -0.897 1.000 1.129 0.021 -++++ --+++ 1125493. 0.021 -0.896 1.000 1.133 0.021 -++++ --+++ 139541. 0.021 -0.897 1.000 1.134 0.021 -++++ --+++ 1839241. 0.021 -0.894 1.000 1.134 0.021 -++++ --+++ 1226617. 0.021 -0.897 1.000 1.131 0.021 -++++ --+++ 943293. 0.022 -0.894 1.000 1.137 0.022 -++++ --+++ 1175145. 0.021 -0.894 1.000 1.136 0.021 -++++ --+++ 1923045. 0.021 -0.909 1.000 1.136 0.021 -++++ --+++ 360909. 0.021 -0.906 1.000 1.133 0.021 -++++ --+++ 1534273. 0.022 -0.895 1.000 1.136 0.022 -++++ --+++ 2058549. 0.021 -0.902 1.000 1.134 0.021 -++++ --+++ 686473. 0.022 -0.894 1.000 1.137 0.022 -++++ --+++ 435857. 0.022 -0.908 1.000 1.139 0.022 -++++ --+++ 634117. 0.021 -0.909 1.000 1.137 0.021 -++++ --+++ 1621645. 0.022 -0.891 1.000 1.140 0.022 -++++ --+++ 1330473. 0.021 -0.897 1.000 1.131 0.021 -++++ --+++ 556725. 0.021 -0.901 1.000 1.131 0.021 -++++ --+++ 22269. 0.021 -0.899 1.000 1.133 0.021 -++++ --+++ 1804545. 0.021 -0.911 1.000 1.133 0.021 -++++ --+++ 1412773. 0.021 -0.892 1.000 1.134 0.021 -++++ --+++ 1423341. 0.021 -0.909 1.000 1.135 0.021 -++++ --+++ 1482997. 0.021 -0.897 1.000 1.131 0.021 -++++ --+++ 617645. 0.021 -0.895 1.000 1.134 0.021 -++++ --+++ 327221. 0.021 -0.892 1.000 1.133 0.021 -++++ --+++ 49029. 0.021 -0.897 1.000 1.132 0.021 -++++ --+++ 295001. 0.021 -0.892 1.000 1.134 0.021 -++++ --+++ 1503317. 0.021 -0.896 1.000 1.132 0.021 -++++ --+++ 1140665. 0.021 -0.907 1.000 1.136 0.021 -++++ --+++ 1268161. 0.021 -0.897 1.000 1.134 0.021 -++++ --+++ 568021. 0.022 -0.909 1.000 1.136 0.022 -++++ --+++ 1667133. 0.021 -0.897 1.000 1.135 0.021 -++++ --+++ 2023909. 0.021 -0.904 1.000 1.134 0.021 -++++ --+++ 1981097. 0.021 -0.890 1.000 1.134 0.021 -++++ --+++ 465057. 0.021 -0.895 1.000 1.135 0.021 -++++ --+++ 1832437. 0.021 -0.890 1.000 1.133 0.021 -++++ --+++ 1092493. 0.021 -0.906 1.000 1.132 0.021 -++++ --+++ 1052501. 0.021 -0.897 1.000 1.133 0.021 -++++ --+++ 305993. 0.021 -0.901 1.000 1.131 0.021 -++++ --+++ 1973641. 0.021 -0.906 1.000 1.131 0.021 -++++ --+++ 772361. 0.021 -0.897 1.000 1.134 0.021 -++++ --+++ 65721. 0.021 -0.898 1.000 1.131 0.021 -++++ --+++ 1854209. 0.022 -0.893 1.000 1.137 0.022 -++++ --+++ 852005. 0.021 -0.894 1.000 1.130 0.021 -++++ --+++ 480629. 0.021 -0.912 1.000 1.134 0.021 -++++ --+++ 1128017. 0.021 -0.896 1.000 1.137 0.021 -++++ --+++ 571681. 0.021 -0.897 1.000 1.135 0.021 -++++ --+++ 1952105. 0.021 -0.890 1.000 1.133 0.021 -++++ --+++ 945661. 0.022 -0.892 1.000 1.139 0.022 -++++ --+++ 1810109. 0.021 -0.898 1.000 1.135 0.021 -++++ --+++ 767113. 0.021 -0.908 1.000 1.137 0.021 -++++ --+++ 1709113. 0.021 -0.896 1.000 1.130 0.021 -++++ --+++ 434657. 0.021 -0.894 1.000 1.136 0.021 -++++ --+++ 1124981. 0.021 -0.890 1.000 1.133 0.021 -++++ --+++ 13773. 0.021 -0.896 1.000 1.132 0.021 -++++ --+++ 219517. 0.021 -0.892 1.000 1.134 0.021 -++++ --+++ 1165513. 0.021 -0.890 1.000 1.132 0.021 -++++ --+++ 373605. 0.021 -0.891 1.000 1.135 0.021 -++++ --+++ 858777. 0.020 -0.893 1.000 1.131 0.020 -++++ --+++ 1890493. 0.021 -0.897 1.000 1.134 0.021 -++++ --+++ 1976317. 0.021 -0.891 1.000 1.132 0.021 -++++ --+++ 973853. 0.021 -0.890 1.000 1.132 0.021 -++++ --+++ 1097585. 0.021 -0.890 1.000 1.134 0.021 -++++ --+++ 1332017. 0.021 -0.890 1.000 1.134 0.021 -++++ --+++ 1143929. 0.021 -0.899 1.000 1.134 0.021 -++++ --+++ 417449. 0.021 -0.894 1.000 1.130 0.021 -++++ --+++ 170761. 0.021 -0.896 1.000 1.135 0.021 -++++ --+++ 861549. 0.021 -0.896 1.000 1.134 0.021 -++++ --+++ 349205. 0.021 -0.911 1.000 1.131 0.021 -++++ --+++ 1340501. 0.021 -0.891 1.000 1.132 0.021 -++++ --+++ 411049. 0.021 -0.897 1.000 1.131 0.021 -++++ --+++ 2055245. 0.021 -0.892 1.000 1.134 0.021 -++++ --+++ 1887617. 0.021 -0.899 1.000 1.135 0.021 -++++ --+++ 1049477. 0.021 -0.899 1.000 1.133 0.021 -++++ --+++ 1053081. 0.021 -0.896 1.000 1.135 0.021 -++++ --+++ 1071101. 0.021 -0.898 1.000 1.132 0.021 -++++ --+++ 1161201. 0.022 -0.908 1.000 1.139 0.022 -++++ --+++ 1611701. 0.021 -0.896 1.000 1.133 0.021 -++++ --+++ 1767049. 0.021 -0.892 1.000 1.134 0.021 -++++ --+++ 446637. 0.021 -0.910 1.000 1.133 0.021 -++++ --+++ 136033. 0.022 -0.912 1.000 1.132 0.022 -++++ --+++ 680165. 0.021 -0.899 1.000 1.133 0.021 -++++ --+++ 1303673. 0.021 -0.891 1.000 1.134 0.021 -++++ --+++ 226909. 0.021 -0.900 1.000 1.132 0.021 -++++ --+++ 1134545. 0.021 -0.898 1.000 1.133 0.021 -++++ --+++ 1478421. 0.021 -0.905 1.000 1.134 0.021 -++++ --+++ 1100649. 0.021 -0.898 1.000 1.133 0.021 -++++ --+++ 1308941. 0.021 -0.905 1.000 1.136 0.021 -++++ --+++ 253249. 0.021 -0.917 1.000 1.133 0.021 -++++ --+++ 1266245. 0.021 -0.897 1.000 1.130 0.021 -++++ --+++ 39769. 0.021 -0.899 1.000 1.131 0.021 -++++ --+++ 198845. 0.021 -0.890 1.000 1.133 0.021 -++++ --+++ 994225. 0.021 -0.899 1.000 1.131 0.021 -++++ --+++ 776821. 0.021 -0.893 1.000 1.133 0.021 -++++ --+++ 1786953. 0.021 -0.897 1.000 1.133 0.021 -++++ --+++ 546157. 0.021 -0.907 1.000 1.135 0.021 -++++ --+++ 633633. 0.021 -0.893 1.000 1.137 0.021 -++++ --+++ 1071013. 0.021 -0.893 1.000 1.134 0.021 -++++ --+++ 1160761. 0.021 -0.906 1.000 1.132 0.021 -++++ --+++ 1609501. 0.021 -0.911 1.000 1.131 0.021 -++++ --+++ 1756049. 0.021 -0.916 1.000 1.134 0.021 -++++ --+++ 2022913. 0.021 -0.890 1.000 1.133 0.021 -++++ --+++ 2053169. 0.021 -0.899 1.000 1.133 0.021 -++++ --+++ 333785. 0.021 -0.896 1.000 1.135 0.021 -++++ --+++ 66757. 0.021 -0.891 1.000 1.134 0.021 -++++ --+++ 631481. 0.022 -0.909 1.000 1.136 0.022 -++++ --+++ 1668925. 0.021 -0.909 1.000 1.128 0.021 -++++ --+++ 1048129. 0.021 -0.902 1.000 1.129 0.021 -++++ --+++ 1784977. 0.021 -0.898 1.000 1.131 0.021 -++++ --+++ 997577. 0.021 -0.897 1.000 1.135 0.021 -++++ --+++ 1837833. 0.020 -0.892 1.000 1.132 0.020 -++++ --+++ 824013. 0.021 -0.897 1.000 1.135 0.021 -++++ --+++ 1748853. 0.021 -0.898 1.000 1.133 0.021 -++++ --+++ 1778285. 0.020 -0.894 1.000 1.131 0.020 -++++ --+++ 2084665. 0.021 -0.908 1.000 1.137 0.021 -++++ --+++ 1106961. 0.021 -0.898 1.000 1.133 0.021 -++++ --+++ 1725957. 0.021 -0.894 1.000 1.132 0.021 -++++ --+++ 540025. 0.022 -0.895 1.000 1.137 0.022 -++++ --+++ 1999989. 0.021 -0.896 1.000 1.133 0.021 -++++ --+++ 602973. 0.021 -0.893 1.000 1.132 0.021 -++++ --+++ 1908545. 0.021 -0.898 1.000 1.131 0.021 -++++ --+++ 1902925. 0.021 -0.896 1.000 1.133 0.021 -++++ --+++ 1692945. 0.021 -0.896 1.000 1.133 0.021 -++++ --+++ 380585. 0.022 -0.893 1.000 1.139 0.022 -++++ --+++ 76117. 0.021 -0.898 1.000 1.133 0.021 -++++ --+++ 574509. 0.021 -0.904 1.000 1.134 0.021 -++++ --+++ 381709. 0.021 -0.910 1.000 1.134 0.021 -++++ --+++ 178949. 0.021 -0.897 1.000 1.131 0.021 -++++ --+++ 1779813. 0.021 -0.897 1.000 1.133 0.021 -++++ --+++ 421569. 0.021 -0.910 1.000 1.136 0.021 -++++ --+++ 452665. 0.021 -0.906 1.000 1.133 0.021 -++++ --+++ 455133. 0.021 -0.898 1.000 1.133 0.021 -++++ --+++ 830865. 0.021 -0.894 1.000 1.130 0.021 -++++ --+++ 437793. 0.021 -0.912 1.000 1.132 0.021 -++++ --+++ 2095021. 0.021 -0.890 1.000 1.132 0.021 -++++ --+++ 1155833. 0.021 -0.889 1.000 1.132 0.021 -++++ --+++ 1740193. 0.021 -0.896 1.000 1.132 0.021 -++++ --+++ 91813. 0.021 -0.897 1.000 1.130 0.021 -++++ --+++ 2086497. 0.021 -0.891 1.000 1.132 0.021 -++++ --+++ 630785. 0.020 -0.897 1.000 1.130 0.020* -++++ --+++ 198173. 0.021 -0.891 1.000 1.135 0.021 -++++ --+++ 1814993. 0.021 -0.898 1.000 1.132 0.021 -++++ --+++ 767469. 0.021 -0.902 1.000 1.134 0.021 -++++ --+++ 2057037. 0.021 -0.894 1.000 1.137 0.021 -++++ --+++ 1676117. 0.021 -0.893 1.000 1.133 0.021 -++++ --+++ 2069857. 0.021 -0.894 1.000 1.137 0.021 -++++ --+++ 1315325. 0.021 -0.895 1.000 1.133 0.021 -++++ --+++ 1411785. 0.021 -0.899 1.000 1.132 0.021 -++++ --+++ 469745. 0.021 -0.891 1.000 1.132 0.021 -++++ --+++ 100717. 0.022 -0.910 1.000 1.136 0.022 -++++ --+++ 874125. 0.021 -0.896 1.000 1.135 0.021 -++++ --+++ 213721. 0.021 -0.899 1.000 1.133 0.021 -++++ --+++ 983789. 0.021 -0.897 1.000 1.132 0.021 -++++ --+++ 402589. 0.021 -0.909 1.000 1.136 0.021 -++++ --+++ 357605. 0.022 -0.909 1.000 1.138 0.022 -++++ --+++ 1746961. 0.021 -0.896 1.000 1.132 0.021 -++++ --+++ 1768433. 0.022 -0.911 1.000 1.135 0.022 -++++ --+++ 773117. 0.021 -0.896 1.000 1.133 0.021 -++++ --+++ 551517. 0.022 -0.909 1.000 1.138 0.022 -++++ --+++ 167825. 0.021 -0.902 1.000 1.135 0.021 -++++ --+++ 739021. 0.021 -0.917 1.000 1.131 0.021 -++++ --+++ 1670549. 0.021 -0.895 1.000 1.134 0.021 -++++ --+++ 453557. 0.021 -0.898 1.000 1.133 0.021 -++++ --+++ 197333. 0.021 -0.895 1.000 1.135 0.021 -++++ --+++ 765197. 0.021 -0.897 1.000 1.132 0.021 -++++ --+++ 72605. 0.022 -0.911 1.000 1.133 0.022 -++++ --+++ 742181. 0.021 -0.896 1.000 1.134 0.021 -++++ --+++ 14521. 0.021 -0.895 1.000 1.135 0.021 -++++ --+++ 688705. 0.021 -0.897 1.000 1.133 0.021 -++++ --+++ 634913. 0.021 -0.894 1.000 1.131 0.021 -++++ --+++ 1326181. 0.021 -0.902 1.000 1.136 0.021 -++++ --+++ 300401. 0.022 -0.895 1.000 1.136 0.022 -++++ --+++ 2063493. 0.021 -0.899 1.000 1.131 0.021 -++++ --+++ 1962665. 0.021 -0.897 1.000 1.132 0.021 -++++ --+++ 339449. 0.021 -0.909 1.000 1.135 0.021 -++++ --+++ 525173. 0.021 -0.892 1.000 1.133 0.021 -++++ --+++ 1882673. 0.021 -0.892 1.000 1.134 0.021 -++++ --+++ 1213897. 0.021 -0.890 1.000 1.133 0.021 -++++ --+++ 681877. 0.021 -0.893 1.000 1.137 0.021 -++++ --+++ 1337933. 0.021 -0.891 1.000 1.134 0.021 -++++ --+++ 363025. 0.021 -0.903 1.000 1.135 0.021 -++++ --+++ 58689. 0.022 -0.890 1.000 1.140 0.022 -++++ --+++ 1505269. 0.021 -0.895 1.000 1.137 0.021 -++++ --+++ 1512297. 0.021 -0.892 1.000 1.139 0.021 -++++ --+++ 1972485. 0.021 -0.912 1.000 1.131 0.021 -++++ --+++ 1738029. 0.021 -0.897 1.000 1.134 0.021 -++++ --+++ 1772173. 0.021 -0.912 1.000 1.134 0.021 -++++ --+++ 394497. 0.021 -0.897 1.000 1.135 0.021 -++++ --+++ 1728317. 0.021 -0.897 1.000 1.132 0.021 -++++ --+++ 1003925. 0.021 -0.899 1.000 1.133 0.021 -++++ --+++ 1269029. 0.021 -0.898 1.000 1.134 0.021 -++++ --+++ 1238641. 0.021 -0.896 1.000 1.132 0.021 -++++ --+++ 91449. 0.022 -0.908 1.000 1.139 0.022 -++++ --+++ 472257. 0.021 -0.897 1.000 1.134 0.021 -++++ --+++ 1193841. 0.021 -0.897 1.000 1.130 0.021 -++++ --+++ 1774901. 0.021 -0.898 1.000 1.132 0.021 -++++ --+++ 928437. 0.022 -0.909 1.000 1.135 0.022 -++++ --+++ 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 630785. with CFOM = 0.0203 0.9 seconds elapsed time Tangent expanded to 268 out of 268 E greater than 1.200 Highest memory used = 1223 / 2116 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 = 614.57, minimum = -159.75 highest memory used = 8715 / 5901 0.0 seconds elapsed time Heavy-atom assignments: x y z s.o.f. Height BR1 0.6498 0.0815 0.4421 1.0000 614.6 Peak list optimization RE = 0.191 for 9 surviving atoms and 268 E-values Highest memory used = 1530 / 2412 0.0 seconds elapsed time E-Fourier for p21212 in P2(1)2(1)2 Maximum = 640.04, minimum = -195.24 highest memory used = 8723 / 5901 0.0 seconds elapsed time Peak list optimization RE = 0.172 for 10 surviving atoms and 268 E-values Highest memory used = 1538 / 2412 0.0 seconds elapsed time E-Fourier for p21212 in P2(1)2(1)2 Maximum = 645.84, minimum = -151.31 highest memory used = 8723 / 5901 0.0 seconds elapsed time Molecule 1 scale 0.812 inches = 2.062 cm per Angstrom BR1 15 13 15 BR1 11 212 7 6 14 16 10 7 3 6 BR1 12 2 11 5 1 9 * 13 15 1 BR1 BR1 Atom Peak x y z SOF Height Distances and Angles BR1 0. 0.6498 0.0815 0.4421 1.000 1.79 0 3 2.761 0 6 2.890 50.9 0 7 1.918 24.3 26.6 0 10 3.382 28.3 76.1 50.7 0 14 1.852 12.9 47.5 23.2 28.6 0 16 1.952 16.6 64.4 38.4 27.3 28.5 1 BR1 3.734 122.0 144.1 137.6 94.2 116.2 118.6 6 2 3.277 45.8 42.4 37.2 72.0 54.4 46.2 163.7 10 12 3.289 45.5 21.5 25.9 73.8 48.5 53.6 162.5 20.9 11 13 2.588 157.8 120.7 143.4 160.6 166.4 147.4 77.4 112.8 117.9 12 15 2.690 164.8 138.5 162.8 136.9 156.3 156.8 42.9 148.9 148.7 36.1 13 15 2.541 75.9 113.5 94.3 48.3 71.3 74.3 46.1 120.3 119.8 122.2 89.0 1 182. 0.5561 0.4236 0.5015 1.000 1.79 0 5 1.466 0 8 1.493 112.6 0 13 1.681 52.6 102.6 2 148. 0.3524 0.2430 0.4380 1.000 1.67 0 10 0.981 0 12 1.193 72.4 3 116. 0.6090 0.2668 0.4336 1.000 1.64 0 BR1 2.761 0 5 1.491 153.0 0 7 1.286 38.0 115.1 0 10 1.618 97.7 105.5 129.1 0 14 1.043 23.4 139.0 36.3 92.8 0 16 1.050 32.0 160.2 65.2 86.4 53.4 4 112. 0.5000 0.5000 0.0300 0.500 0.00 0 8 1.331 5 103. 0.6409 0.3602 0.3286 1.000 1.19 0 1 1.466 0 3 1.491 107.7 0 9 1.355 131.1 121.2 0 13 1.407 71.6 132.6 73.5 6 92. 0.7929 0.2179 0.0996 1.000 0.44 0 BR1 2.890 0 7 1.456 36.2 0 11 1.355 151.5 115.3 10 12 1.217 98.0 82.6 71.8 7 87. 0.6846 0.2038 0.3196 1.000 1.26 0 BR1 1.918 0 3 1.286 117.7 0 6 1.456 117.2 125.0 0 14 0.760 73.5 54.2 147.2 0 16 1.274 72.2 48.4 162.6 47.2 10 12 1.772 126.0 101.5 42.9 155.7 119.7 8 87. 0.5000 0.5000 0.3219 0.500 1.08 0 1 1.493 0 4 1.331 123.3 5 1 1.493 113.4 123.3 9 78. 0.7387 0.3751 0.1186 1.000 0.41 0 5 1.355 0 11 1.335 119.0 0 13 1.654 54.7 134.5 10 70. 0.4429 0.2666 0.5060 1.000 1.91 0 BR1 3.382 0 2 0.981 101.5 0 3 1.618 54.0 142.9 0 12 1.295 103.6 61.4 143.5 0 14 1.967 26.8 114.2 32.0 130.3 0 16 1.873 28.5 129.8 34.0 112.3 28.2 11 54. 0.8135 0.3052 0.0180 1.000 0.08 0 6 1.355 0 9 1.335 124.2 10 12 1.512 49.9 101.2 12 52. 0.3507 0.2427 0.6996 1.000 2.64 0 2 1.193 0 10 1.295 46.2 7 6 1.217 139.2 133.7 8 7 1.772 87.8 116.9 54.5 9 11 1.512 148.9 150.2 58.4 92.3 13 51. 0.7293 0.4290 0.4359 1.000 1.55 0 1 1.681 0 5 1.407 55.9 0 9 1.654 100.7 51.8 0 15 1.637 144.9 118.4 97.1 14 49. 0.6066 0.2007 0.3527 1.000 1.39 0 BR1 1.852 0 3 1.043 143.6 0 7 0.760 83.3 89.5 0 10 1.967 124.6 55.2 144.8 0 16 0.941 81.7 63.7 96.5 70.3 15 46. 0.8848 0.4005 0.5570 1.000 2.01 0 13 1.637 16 44. 0.6145 0.2069 0.5573 1.000 2.14 0 BR1 1.952 0 3 1.050 131.4 0 7 1.274 69.4 66.3 0 10 1.873 124.3 59.6 111.6 0 14 0.941 69.8 62.9 36.4 81.5 Atom Code x y z Height Symmetry transformation BR1 1 0.3502 -0.0815 0.4421 1.90 1.0000-X 0.0000-Y 0.0000+Z BR1 2 0.8502 0.5815 0.5579 1.90 1.5000-X 0.5000+Y 1.0000-Z BR1 3 0.1498 0.4185 0.5579 2.00 -0.5000+X 0.5000-Y 1.0000-Z BR1 4 1.1498 0.4185 0.5579 2.00 0.5000+X 0.5000-Y 1.0000-Z 1 5 0.4439 0.5764 0.5015 1.69 1.0000-X 1.0000-Y 0.0000+Z 2 6 0.8524 0.2570 0.5620 2.12 0.5000+X 0.5000-Y 1.0000-Z 6 7 0.2929 0.2821 0.9004 3.36 -0.5000+X 0.5000-Y 1.0000-Z 7 8 0.1846 0.2962 0.6804 2.54 -0.5000+X 0.5000-Y 1.0000-Z 11 9 0.3135 0.1948 0.9820 3.72 -0.5000+X 0.5000-Y 1.0000-Z 12 10 0.8507 0.2573 0.3004 1.16 0.5000+X 0.5000-Y 1.0000-Z 13 11 0.7707 -0.0710 0.5641 2.34 1.5000-X -0.5000+Y 1.0000-Z 15 12 0.6152 -0.0995 0.4430 1.91 1.5000-X -0.5000+Y 1.0000-Z 15 13 0.3848 0.0995 0.4430 1.79 -0.5000+X 0.5000-Y 1.0000-Z 0.0 seconds elapsed time +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + shelxs finished at 15:43:16 Total elapsed time: 1.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++