+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXS-97 - CRYSTAL STRUCTURE SOLUTION - WinGX VERSION + + Copyright(C) George M. Sheldrick 1986-97 Release 97-2 + + 2007src0011 started at 15:26:18 on 30 Jan 2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0011 in P4(1) CELL 0.71073 11.4912 11.4912 16.7890 90.000 90.000 90.000 ZERR 4.00 0.0001 0.0001 0.0002 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM -Y, X, 0.25+Z SYMM Y, -X, 0.75+Z SFAC C H N O P S UNIT 72 96 20 8 12 8 V = 2216.95 At vol = 18.5 F(000) = 1040.0 mu = 0.48 mm-1 Max single Patterson vector = 28.6 cell wt = 1997.81 rho = 1.496 OMIT 4.00 180.00 ESEL 1.200 5.000 0.005 0.700 0 INIT 12 16 0.80 0.20 0.20 PHAN 10 0.90 0.30 155 40 10 TREF 256 251 0.80 3 -0.60 HKLF 4 h k l F*F Sigma Why Rejected 0.00 0.00 -6.00 10.19 2.00 Observed but should be systematically absent 41685 Reflections read, of which 52 rejected Maximum h, k, l and 2-Theta = 14. 14. 21. 55.01 2622 Unique reflections, of which 2614 observed R(int) = 0.0320 R(sigma) = 0.0127 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. 20. 51. 75. 94. 117. 84. 106. 149. 212. 301. 437. 691. N(measured) 7. 20. 51. 75. 94. 117. 84. 106. 149. 212. 301. 437. 695. N(theory) 11. 21. 51. 75. 94. 117. 84. 106. 149. 212. 301. 437. 695. 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 = 7086 / 13110 Observed E .GT. 1.200 1.300 1.400 1.500 1.600 1.700 1.800 1.900 2.000 2.100 Number 798 663 538 422 333 263 210 161 111 79 Centric Acentric 0kl h0l hk0 Rest Mean Abs(E*E-1) 0.968 0.736 0.803 0.803 1.031 0.753 0.8 seconds CPU time SUMMARY OF PARAMETERS FOR 2007src0011 in P4(1) ESEL Emin 1.200 Emax 5.000 DelU 0.005 renorm 0.700 axis 0 OMIT s 4.00 2theta(lim) 180.0 INIT nn 12 nf 16 s+ 0.800 s- 0.200 wr 0.200 PHAN steps 10 cool 0.900 Boltz 0.300 ns 155 mtpr 40 mnqr 10 TREF np 256. nE 251 kapscal 0.800 ntan 3 wn -0.600 FMAP code 8 PLAN npeaks -43 del1 0.500 del2 1.500 MORE verbosity 1 TIME t 9999999. 155 Reflections and 2173. unique TPR for phase annealing 251 Phases refined using 8923. unique TPR 329 Reflections and 14772. unique TPR for R(alpha) 0.2 seconds CPU time 3682 Unique negative quartets found, 1208 used for phase refinement 0.4 seconds CPU time Highest memory used to derive phase relations = 5498 / 27377 ONE-PHASE SEMINVARIANTS h k l E P+ Phi 6 6 0 1.883 0.86 -2 6 0 2.136 0.02 2 2 0 1.780 0.74 2 6 0 1.542 0.07 -2 8 0 1.510 0.99 -2 10 0 1.414 0.00 Expected value of Sigma-1 = 0.920 Following phases held constant with unit weights for the initial 4 weighted tangent cycles (before phase annealing): h k l E Phase/Comment 1 8 5 2.490 random phase 0 1 5 2.165 random phase 3 6 8 2.658 random phase 0 3 1 1.837 random phase 3 9 2 2.658 random phase 2 3 7 2.117 random phase -1 4 0 2.099 0 or 180 at random 0 2 1 1.812 random phase 0 3 11 1.871 random phase 6 6 0 1.883 0 sigma-1 = 0.858 -2 6 0 2.136 180 sigma-1 = 0.024 1 1 4 1.768 random phase 2 4 14 2.356 random phase 2 4 15 2.214 random phase 2 6 0 1.542 180 sigma-1 = 0.067 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 314 Unique NQR employed in phase annealing 128 Parallel refinements, highest memory = 8396 / 75928 0.0 seconds CPU time STRUCTURE SOLUTION for 2007src0011 in P4(1) Phase annealing cycle: 1 Beta = 0.15476 Ralpha 0.128 0.206 0.122 0.158 0.074 0.117 0.179 0.072 0.306 0.132 0.200 0.129 0.151 0.228 0.160 0.074 0.075 0.153 0.189 0.182 Nqual -0.036-0.014-0.201-0.245-0.505-0.025-0.363-0.538 0.018 0.144-0.220 0.105-0.030-0.099-0.184-0.354-0.509-0.287 0.079 0.059 Mabs 0.951 0.783 0.940 0.830 1.176 1.022 0.806 1.174 0.704 1.009 0.783 1.027 0.948 0.768 0.950 1.081 1.141 0.963 0.840 0.802 Phase annealing cycle: 2 Beta = 0.17196 Ralpha 0.128 0.250 0.125 0.142 0.064 0.119 0.103 0.052 0.371 0.136 0.272 0.120 0.147 0.307 0.121 0.064 0.066 0.159 0.174 0.260 Nqual -0.261-0.260-0.271-0.424-0.462-0.028-0.439-0.467-0.260-0.071-0.373-0.196-0.056-0.289-0.356-0.504-0.530-0.295-0.023-0.112 Mabs 0.916 0.734 0.902 0.881 1.087 0.967 0.960 1.090 0.661 0.936 0.739 0.954 0.906 0.717 0.968 1.077 1.056 0.907 0.838 0.737 Phase annealing cycle: 3 Beta = 0.19106 Ralpha 0.134 0.260 0.141 0.123 0.066 0.110 0.061 0.058 0.273 0.157 0.279 0.098 0.106 0.287 0.070 0.062 0.064 0.097 0.121 0.214 Nqual -0.288-0.256-0.474-0.301-0.490-0.172-0.502-0.530-0.281-0.118-0.283-0.250-0.107-0.354-0.494-0.595-0.512-0.244 0.001-0.227 Mabs 0.898 0.738 0.890 0.935 1.086 0.974 1.083 1.104 0.715 0.918 0.739 0.970 0.967 0.729 1.054 1.073 1.092 1.002 0.926 0.792 Phase annealing cycle: 4 Beta = 0.21229 Ralpha 0.135 0.257 0.117 0.115 0.062 0.110 0.057 0.059 0.224 0.138 0.175 0.111 0.108 0.290 0.065 0.058 0.054 0.085 0.112 0.181 Nqual -0.335-0.336-0.518-0.270-0.558-0.154-0.492-0.538-0.370-0.188-0.329-0.112-0.109-0.327-0.557-0.525-0.633-0.473-0.165-0.319 Mabs 0.906 0.731 0.913 0.965 1.109 0.982 1.096 1.110 0.765 0.942 0.823 0.968 0.983 0.718 1.096 1.098 1.112 1.090 0.969 0.828 Phase annealing cycle: 5 Beta = 0.23588 Ralpha 0.122 0.237 0.123 0.109 0.069 0.118 0.063 0.055 0.192 0.128 0.151 0.103 0.108 0.309 0.065 0.062 0.062 0.066 0.113 0.124 Nqual -0.355-0.336-0.492-0.267-0.557-0.164-0.530-0.515-0.189-0.168-0.239-0.208-0.127-0.330-0.496-0.505-0.613-0.507-0.139-0.386 Mabs 0.904 0.741 0.916 0.960 1.095 0.957 1.104 1.096 0.800 0.960 0.851 0.958 0.975 0.704 1.076 1.066 1.104 1.073 0.971 0.892 Phase annealing cycle: 6 Beta = 0.26209 Ralpha 0.123 0.248 0.121 0.096 0.056 0.124 0.057 0.052 0.192 0.126 0.125 0.113 0.103 0.285 0.064 0.056 0.057 0.070 0.112 0.069 Nqual -0.325-0.377-0.442-0.286-0.560-0.189-0.487-0.514-0.148-0.091-0.089-0.152-0.235-0.437-0.504-0.543-0.524-0.504-0.158-0.470 Mabs 0.935 0.733 0.937 0.992 1.102 0.955 1.092 1.089 0.797 0.950 0.895 0.982 0.995 0.716 1.093 1.094 1.100 1.093 0.973 1.074 Phase annealing cycle: 7 Beta = 0.29121 Ralpha 0.129 0.219 0.122 0.096 0.058 0.119 0.063 0.056 0.175 0.097 0.098 0.118 0.106 0.245 0.064 0.059 0.059 0.058 0.116 0.063 Nqual -0.341-0.421-0.372-0.232-0.568-0.161-0.589-0.531-0.141-0.148-0.257-0.238-0.147-0.394-0.535-0.514-0.560-0.478-0.220-0.470 Mabs 0.940 0.747 0.931 0.998 1.120 0.968 1.096 1.130 0.822 1.001 0.997 0.928 0.983 0.746 1.098 1.128 1.105 1.099 0.988 1.104 Phase annealing cycle: 8 Beta = 0.32357 Ralpha 0.123 0.187 0.127 0.095 0.052 0.108 0.058 0.058 0.146 0.101 0.085 0.098 0.100 0.217 0.054 0.057 0.059 0.063 0.115 0.064 Nqual -0.259-0.459-0.307-0.182-0.523-0.049-0.540-0.559-0.234-0.238-0.389-0.207-0.201-0.432-0.488-0.512-0.559-0.576-0.195-0.540 Mabs 0.955 0.784 0.931 1.001 1.106 0.982 1.085 1.102 0.834 0.993 1.032 0.966 0.997 0.768 1.107 1.123 1.121 1.124 0.991 1.120 Phase annealing cycle: 9 Beta = 0.35952 Ralpha 0.118 0.166 0.120 0.093 0.059 0.102 0.058 0.059 0.139 0.113 0.057 0.100 0.101 0.187 0.059 0.054 0.059 0.071 0.111 0.064 Nqual -0.193-0.336-0.370-0.210-0.533-0.167-0.527-0.558-0.191-0.276-0.472-0.152-0.179-0.467-0.524-0.536-0.555-0.560-0.214-0.530 Mabs 0.953 0.823 0.937 1.009 1.130 0.985 1.106 1.110 0.848 0.980 1.086 0.973 0.997 0.801 1.121 1.124 1.108 1.128 0.994 1.100 Phase annealing cycle: 10 Beta = 0.39946 Ralpha 0.126 0.163 0.113 0.099 0.056 0.112 0.065 0.064 0.150 0.102 0.056 0.097 0.108 0.186 0.057 0.064 0.059 0.065 0.114 0.064 Nqual -0.186-0.308-0.350-0.182-0.587-0.087-0.512-0.529-0.236-0.183-0.515-0.158-0.191-0.384-0.549-0.538-0.526-0.586-0.205-0.583 Mabs 0.960 0.831 0.955 0.991 1.129 0.982 1.108 1.102 0.842 1.010 1.124 0.985 0.975 0.812 1.124 1.129 1.124 1.119 0.988 1.125 Phase refinement cycle: 1 Ralpha 0.286 0.533 0.307 0.267 0.165 0.272 0.157 0.158 0.558 0.261 0.151 0.275 0.274 0.727 0.164 0.160 0.160 0.164 0.263 0.170 Nqual 0.048-0.113-0.037 0.053-0.438 0.089-0.441-0.420-0.051 0.026-0.417 0.044 0.082-0.307-0.414-0.415-0.430-0.440 0.065-0.427 Mabs 0.770 0.609 0.749 0.785 0.856 0.778 0.864 0.863 0.601 0.790 0.863 0.772 0.773 0.556 0.851 0.857 0.852 0.854 0.789 0.849 Phase refinement cycle: 2 Ralpha 0.158 0.158 0.167 0.158 0.084 0.156 0.083 0.083 0.167 0.154 0.085 0.151 0.162 0.175 0.083 0.084 0.083 0.083 0.160 0.083 Nqual 0.058-0.043 0.100 0.028-0.620 0.133-0.638-0.645-0.042 0.054-0.644 0.079 0.180-0.410-0.687-0.634-0.628-0.642 0.075-0.638 Mabs 1.076 0.956 1.076 1.083 1.198 1.086 1.201 1.203 0.953 1.086 1.208 1.098 1.093 0.896 1.206 1.205 1.203 1.205 1.093 1.202 Try Ralpha Nqual Sigma-1 M(abs) CFOM Seminvariants 1720229. 0.150 -0.049 0.289 1.047 0.454 ++-++ - 212537. 0.172 -0.065 0.727 0.910 0.458 ----+ - 1062685. 0.159 0.083 0.289 1.046 0.625 ++-++ - 1119121. 0.149 -0.049 0.289 1.056 0.452 ++-++ - 1401301. 0.088 -0.633 0.900 1.163 0.088 +---+ - 715049. 0.144 0.044 0.289 1.055 0.558 ++-++ - 1478093. 0.082 -0.622 0.900 1.163 0.082 +---+ - 1099009. 0.083 -0.615 0.900 1.156 0.083 +---+ - 1300741. 0.154 -0.196 0.727 0.951 0.317 ----+ - 212249. 0.140 0.002 0.289 1.050 0.503 ++-++ - 1061245. 0.088 -0.610 0.900 1.171 0.088 +---+ - 1111921. 0.151 -0.002 0.289 1.054 0.509 ++-++ - 1365301. 0.151 0.059 0.289 1.057 0.586 ++-++ - 535049. 0.204 -0.392 0.747 0.844 0.248 +-+++ - 578093. 0.082 -0.628 0.900 1.173 0.082 +---+ - 793313. 0.091 -0.605 0.900 1.176 0.091 +---+ - 1869413. 0.090 -0.621 0.900 1.171 0.090 +---+ - 958457. 0.085 -0.612 0.900 1.163 0.085 +---+ - 597981. 0.155 0.022 0.647 1.057 0.543 +--++ - 892753. 0.087 -0.589 0.900 1.172 0.087 +---+ - 269461. 0.151 0.100 0.289 1.052 0.640 ++-++ - 1347305. 0.089 -0.611 0.900 1.167 0.089 +---+ - 445069. 0.153 0.096 0.289 1.049 0.638 ++-++ - 128193. 0.088 -0.625 0.900 1.169 0.088 +---+ - 640965. 0.151 -0.014 0.289 1.051 0.494 ++-++ - 1107673. 0.088 -0.629 0.900 1.173 0.088 +---+ - 1344061. 0.090 -0.606 0.900 1.183 0.090 +---+ - 428849. 0.087 -0.611 0.900 1.170 0.087 +---+ - 47093. 0.234 -0.129 -0.048 0.794 0.456 --+++ + 235465. 0.183 -0.167 0.333 0.923 0.371 --+-- - 1177325. 0.160 0.025 0.647 1.050 0.550 +--++ - 1692321. 0.091 -0.640 0.900 1.168 0.091 +---+ - 781509. 0.086 -0.634 0.900 1.166 0.086 +---+ - 936165. 0.080 -0.596 0.900 1.159 0.080 +---+ - 670277. 0.081 -0.610 0.900 1.181 0.081 +---+ - 431489. 0.080 -0.637 0.900 1.163 0.080 +---+ - 2040077. 0.148 0.052 0.289 1.056 0.573 ++-++ - 1130697. 0.087 -0.630 0.900 1.170 0.087 +---+ - 1810393. 0.081 -0.631 0.900 1.165 0.081 +---+ - 1414593. 0.088 -0.613 0.900 1.169 0.088 +---+ - 60293. 0.085 -0.600 0.900 1.180 0.085 +---+ - 2031541. 0.089 -0.624 0.900 1.170 0.089 +---+ - 702349. 0.081 -0.624 0.900 1.173 0.081 +---+ - 948473. 0.078 -0.626 0.900 1.163 0.078 +---+ - 1677265. 0.085 -0.644 0.900 1.168 0.085 +---+ - 1507325. 0.081 -0.653 0.900 1.167 0.081 +---+ - 643153. 0.092 -0.608 0.900 1.169 0.092 +---+ - 2076861. 0.080 -0.607 0.900 1.168 0.080 +---+ - 2047493. 0.146 0.061 0.647 1.053 0.584 +--++ - 1822961. 0.160 -0.035 0.289 1.049 0.479 ++-++ - 1424077. 0.091 -0.641 0.900 1.166 0.091 +---+ - 1626781. 0.083 -0.615 0.900 1.172 0.083 +---+ - 1811597. 0.084 -0.611 0.900 1.165 0.084 +---+ - 626189. 0.158 -0.028 0.289 1.041 0.486 ++-++ - 420405. 0.088 -0.618 0.900 1.168 0.088 +---+ - 750921. 0.078 -0.591 0.900 1.151 0.078 +---+ - 942581. 0.095 -0.613 0.900 1.164 0.095 +---+ - 855677. 0.083 -0.619 0.900 1.176 0.083 +---+ - 597089. 0.087 -0.628 0.900 1.171 0.087 +---+ - 4873. 0.086 -0.642 0.900 1.168 0.086 +---+ - 1848857. 0.084 -0.608 0.900 1.172 0.084 +---+ - 1164217. 0.089 -0.643 0.900 1.169 0.089 +---+ - 974661. 0.081 -0.634 0.900 1.167 0.081 +---+ - 1984721. 0.088 -0.609 0.900 1.178 0.088 +---+ - 1053357. 0.083 -0.604 0.900 1.167 0.083 +---+ - 496329. 0.154 0.118 0.289 1.050 0.669 ++-++ - 1774797. 0.139 0.004 0.289 1.052 0.503 ++-++ - 1888393. 0.150 0.012 0.289 1.046 0.525 ++-++ - 1417713. 0.146 0.072 0.289 1.053 0.597 ++-++ - 1926801. 0.083 -0.601 0.900 1.171 0.083 +---+ - 1271145. 0.147 -0.081 0.647 1.054 0.416 +--++ - 702973. 0.080 -0.612 0.900 1.172 0.080 +---+ - 1357557. 0.089 -0.618 0.900 1.171 0.089 +---+ - 1606725. 0.080 -0.581 0.900 1.154 0.081 +---+ - 1611185. 0.088 -0.609 0.900 1.172 0.088 +---+ - 1951869. 0.088 -0.607 0.900 1.173 0.088 +---+ - 1788325. 0.082 -0.579 0.900 1.164 0.082 +---+ - 1648665. 0.077 -0.650 0.900 1.172 0.077 +---+ - 1924281. 0.088 -0.610 0.900 1.179 0.088 +---+ - 2086849. 0.087 -0.586 0.900 1.173 0.087 +---+ - 1635901. 0.086 -0.610 0.900 1.171 0.086 +---+ - 864549. 0.080 -0.606 0.900 1.155 0.080 +---+ - 147125. 0.088 -0.592 0.900 1.163 0.088 +---+ - 822093. 0.083 -0.619 0.900 1.179 0.083 +---+ - 1166041. 0.089 -0.592 0.900 1.182 0.089 +---+ - 1434733. 0.078 -0.614 0.900 1.168 0.078 +---+ - 1648949. 0.152 0.070 0.289 1.042 0.601 ++-++ - 597729. 0.081 -0.634 0.900 1.173 0.081 +---+ - 5885. 0.076 -0.647 0.900 1.168 0.076* +---+ - 2059525. 0.080 -0.584 0.900 1.163 0.080 +---+ - 1909017. 0.083 -0.585 0.900 1.180 0.084 +---+ - 1580973. 0.085 -0.606 0.900 1.171 0.085 +---+ - 1156477. 0.091 -0.603 0.900 1.181 0.091 +---+ - 660061. 0.089 -0.556 0.900 1.172 0.091 +---+ - 1652813. 0.092 -0.625 0.900 1.168 0.092 +---+ - 706377. 0.091 -0.603 0.900 1.169 0.091 +---+ - 270121. 0.085 -0.604 0.900 1.171 0.085 +---+ - 461569. 0.082 -0.634 0.900 1.165 0.082 +---+ - 1731285. 0.084 -0.592 0.900 1.174 0.084 +---+ - 124105. 0.092 -0.598 0.900 1.173 0.092 +---+ - 842389. 0.085 -0.619 0.900 1.170 0.085 +---+ - 1997441. 0.078 -0.618 0.900 1.172 0.078 +---+ - 751905. 0.084 -0.623 0.900 1.166 0.084 +---+ - 168765. 0.161 -0.056 0.289 1.041 0.457 ++-++ - 1628593. 0.087 -0.589 0.900 1.170 0.087 +---+ - 1543645. 0.080 -0.629 0.900 1.154 0.080 +---+ - 997805. 0.090 -0.599 0.900 1.183 0.090 +---+ - 267817. 0.090 -0.589 0.900 1.175 0.090 +---+ - 346257. 0.088 -0.609 0.900 1.168 0.088 +---+ - 745149. 0.083 -0.634 0.900 1.175 0.083 +---+ - 1451961. 0.081 -0.640 0.900 1.170 0.081 +---+ - 1598597. 0.086 -0.613 0.900 1.174 0.086 +---+ - 2025829. 0.076 -0.634 0.900 1.170 0.076 +---+ - 2059985. 0.146 -0.002 0.289 1.056 0.503 ++-++ - 838973. 0.089 -0.599 0.900 1.178 0.089 +---+ - 2050437. 0.086 -0.623 0.900 1.165 0.086 +---+ - 1885085. 0.086 -0.583 0.900 1.169 0.086 +---+ - 1036817. 0.079 -0.587 0.900 1.162 0.079 +---+ - 176729. 0.086 -0.618 0.900 1.173 0.086 +---+ - 1763957. 0.082 -0.610 0.900 1.162 0.082 +---+ - 2044201. 0.078 -0.625 0.900 1.167 0.078 +---+ - 727149. 0.083 -0.578 0.900 1.177 0.084 +---+ - 1911317. 0.078 -0.616 0.900 1.155 0.078 +---+ - 884021. 0.087 -0.613 0.900 1.162 0.087 +---+ - 350625. 0.087 -0.592 0.900 1.169 0.088 +---+ - 1532257. 0.087 -0.629 0.900 1.159 0.087 +---+ - 587225. 0.082 -0.627 0.900 1.164 0.082 +---+ - 1496809. 0.086 -0.618 0.900 1.164 0.086 +---+ - 1432549. 0.083 -0.622 0.900 1.166 0.083 +---+ - 871289. 0.089 -0.579 0.900 1.188 0.089 +---+ - 810705. 0.083 -0.645 0.900 1.165 0.083 +---+ - 1956373. 0.087 -0.599 0.900 1.178 0.087 +---+ - 1393257. 0.088 -0.624 0.900 1.176 0.088 +---+ - 674829. 0.088 -0.637 0.900 1.175 0.088 +---+ - 93509. 0.084 -0.617 0.900 1.166 0.084 +---+ - 240573. 0.093 -0.555 0.900 1.167 0.095 +---+ - 1202865. 0.089 -0.613 0.900 1.169 0.089 +---+ - 1820021. 0.087 -0.596 0.900 1.167 0.087 +---+ - 689365. 0.089 -0.617 0.900 1.178 0.089 +---+ - 1349673. 0.089 -0.597 0.900 1.180 0.089 +---+ - 456909. 0.079 -0.637 0.900 1.167 0.079 +---+ - 936965. 0.082 -0.568 0.900 1.174 0.083 +---+ - 490521. 0.087 -0.631 0.900 1.158 0.087 +---+ - 497717. 0.090 -0.627 0.900 1.177 0.090 +---+ - 1208177. 0.087 -0.607 0.900 1.170 0.087 +---+ - 1595545. 0.084 -0.627 0.900 1.168 0.084 +---+ - 27181. 0.088 -0.614 0.900 1.170 0.088 +---+ - 1322113. 0.088 -0.615 0.900 1.167 0.088 +---+ - 1068425. 0.089 -0.614 0.900 1.177 0.089 +---+ - 2039513. 0.081 -0.620 0.900 1.175 0.081 +---+ - 42737. 0.086 -0.613 0.900 1.165 0.086 +---+ - 683853. 0.085 -0.595 0.900 1.176 0.085 +---+ - 1123789. 0.079 -0.617 0.900 1.167 0.079 +---+ - 1300473. 0.083 -0.608 0.900 1.167 0.083 +---+ - 1972133. 0.078 -0.632 0.900 1.159 0.078 +---+ - 1028881. 0.076 -0.634 0.900 1.166 0.076 +---+ - 135905. 0.087 -0.628 0.900 1.168 0.087 +---+ - 1753201. 0.086 -0.623 0.900 1.166 0.086 +---+ - 1674089. 0.085 -0.604 0.900 1.174 0.085 +---+ - 419061. 0.086 -0.609 0.900 1.178 0.086 +---+ - 1593109. 0.083 -0.632 0.900 1.169 0.083 +---+ - 1037281. 0.082 -0.625 0.900 1.158 0.082 +---+ - 1202101. 0.083 -0.593 0.900 1.160 0.083 +---+ - 2033065. 0.089 -0.622 0.900 1.169 0.089 +---+ - 109097. 0.078 -0.630 0.900 1.159 0.078 +---+ - 1643077. 0.091 -0.624 0.900 1.178 0.091 +---+ - 1347009. 0.088 -0.575 0.900 1.176 0.089 +---+ - 787529. 0.086 -0.598 0.900 1.174 0.086 +---+ - 1178769. 0.084 -0.630 0.900 1.169 0.084 +---+ - 724969. 0.088 -0.612 0.900 1.164 0.088 +---+ - 1494045. 0.083 -0.626 0.900 1.168 0.083 +---+ - 1923929. 0.091 -0.619 0.900 1.182 0.091 +---+ - 1290333. 0.081 -0.616 0.900 1.169 0.081 +---+ - 1870329. 0.088 -0.620 0.900 1.167 0.088 +---+ - 2002601. 0.090 -0.575 0.900 1.183 0.091 +---+ - 1086737. 0.081 -0.627 0.900 1.171 0.081 +---+ - 160209. 0.080 -0.625 0.900 1.172 0.080 +---+ - 224657. 0.089 -0.566 0.900 1.174 0.090 +---+ - 1151757. 0.084 -0.598 0.900 1.174 0.084 +---+ - 1908073. 0.086 -0.613 0.900 1.167 0.086 +---+ - 541813. 0.086 -0.640 0.900 1.159 0.086 +---+ - 824409. 0.085 -0.614 0.900 1.164 0.085 +---+ - 620881. 0.084 -0.615 0.900 1.168 0.084 +---+ - 1299517. 0.093 -0.624 0.900 1.169 0.093 +---+ - 2004193. 0.085 -0.646 0.900 1.166 0.085 +---+ - 975469. 0.075 -0.655 0.900 1.164 0.075 +---+ - 689681. 0.080 -0.607 0.900 1.168 0.080 +---+ - 1873081. 0.087 -0.625 0.900 1.169 0.087 +---+ - 1227817. 0.093 -0.622 0.900 1.166 0.093 +---+ - 618017. 0.077 -0.613 0.900 1.163 0.077 +---+ - 605177. 0.085 -0.614 0.900 1.167 0.085 +---+ - 1801325. 0.085 -0.588 0.900 1.183 0.086 +---+ - 1273181. 0.074 -0.610 0.900 1.160 0.074* +---+ - 1443417. 0.089 -0.617 0.900 1.166 0.089 +---+ - 770361. 0.081 -0.613 0.900 1.164 0.081 +---+ - 603697. 0.088 -0.623 0.900 1.175 0.088 +---+ - 393281. 0.089 -0.631 0.900 1.169 0.089 +---+ - 3645. 0.089 -0.610 0.900 1.169 0.089 +---+ - 240301. 0.080 -0.629 0.900 1.167 0.080 +---+ - 226893. 0.083 -0.625 0.900 1.175 0.083 +---+ - 815137. 0.083 -0.626 0.900 1.168 0.083 +---+ - 344641. 0.084 -0.631 0.900 1.177 0.084 +---+ - 2037473. 0.086 -0.607 0.900 1.170 0.086 +---+ - 907789. 0.089 -0.578 0.900 1.170 0.090 +---+ - 1103841. 0.087 -0.594 0.900 1.163 0.087 +---+ - 1026565. 0.091 -0.595 0.900 1.178 0.091 +---+ - 1470217. 0.090 -0.605 0.900 1.176 0.090 +---+ - 1439849. 0.089 -0.629 0.900 1.172 0.089 +---+ - 978549. 0.090 -0.623 0.900 1.163 0.090 +---+ - 1840749. 0.085 -0.614 0.900 1.177 0.085 +---+ - 1148113. 0.081 -0.624 0.900 1.169 0.081 +---+ - 1129661. 0.079 -0.611 0.900 1.162 0.079 +---+ - 881237. 0.088 -0.604 0.900 1.177 0.088 +---+ - 1525245. 0.085 -0.593 0.900 1.165 0.085 +---+ - 882557. 0.085 -0.604 0.900 1.160 0.085 +---+ - 916713. 0.087 -0.619 0.900 1.167 0.087 +---+ - 402745. 0.089 -0.573 0.900 1.171 0.090 +---+ - 1102721. 0.080 -0.638 0.900 1.166 0.080 +---+ - 1257873. 0.078 -0.625 0.900 1.164 0.078 +---+ - 2014949. 0.085 -0.601 0.900 1.168 0.085 +---+ - 2086697. 0.084 -0.656 0.900 1.166 0.084 +---+ - 558145. 0.081 -0.625 0.900 1.162 0.081 +---+ - 1434625. 0.084 -0.622 0.900 1.176 0.084 +---+ - 1335645. 0.085 -0.617 0.900 1.172 0.085 +---+ - 1686137. 0.083 -0.605 0.900 1.165 0.083 +---+ - 1946305. 0.082 -0.643 0.900 1.169 0.082 +---+ - 1132301. 0.077 -0.652 0.900 1.169 0.077 +---+ - CFOM Range Frequency 0.000 - 0.020 0 0.020 - 0.040 0 0.040 - 0.060 0 0.060 - 0.080 28 0.080 - 0.100 170 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 1 0.260 - 0.280 0 0.280 - 0.300 0 0.300 - 0.320 1 0.320 - 0.340 1 0.340 - 0.360 0 0.360 - 0.380 2 0.380 - 0.400 0 0.400 - 0.420 1 0.420 - 0.440 1 0.440 - 0.460 10 0.460 - 0.480 1 0.480 - 0.500 5 0.500 - 0.520 6 0.520 - 0.540 4 0.540 - 0.560 6 0.560 - 0.580 5 0.580 - 0.600 4 0.600 - 9.999 10 256. Phase sets refined - best is code 1273181. with CFOM = 0.0739 4.1 seconds CPU time Tangent expanded to 798 out of 798 E greater than 1.200 Highest memory used = 3348 / 8758 0.1 seconds CPU time FMAP and GRID set by program FMAP 8 3 20 GRID -1.471 -2 -2 1.471 2 2 E-Fourier for 2007src0011 in P4(1) Maximum = 292.22, minimum = -60.11 highest memory used = 8936 / 13777 0.1 seconds CPU time Heavy-atom assignments: x y z s.o.f. Height S1 0.6567 0.3622 0.1655 1.0000 292.2 S2 0.8919 0.4149 0.1581 1.0000 266.6 S3 0.3426 0.6953 0.2528 1.0000 258.1 S4 0.5824 0.7548 0.1713 1.0000 257.2 P5 0.7439 0.4891 0.0355 1.0000 238.0 Peak list optimization RE = 0.160 for 27 surviving atoms and 798 E-values Highest memory used = 1751 / 7182 0.1 seconds CPU time E-Fourier for 2007src0011 in P4(1) Maximum = 290.60, minimum = -62.87 highest memory used = 8976 / 13777 0.0 seconds CPU time Peak list optimization RE = 0.124 for 30 surviving atoms and 798 E-values Highest memory used = 1791 / 7182 0.1 seconds CPU time E-Fourier for 2007src0011 in P4(1) Maximum = 285.36, minimum = -43.35 highest memory used = 8976 / 13777 0.0 seconds CPU time Molecule 1 scale 0.533 inches = 1.353 cm per Angstrom S3 40 28 30 S4 25 21 14 35 23 17 32 13 6 19 42 40 28 26 24 S3 33 10 1*5 5 1 43 29 31 8 20 30 34 S1 37 36 24 18 12 9 22 S4 35 32 2 34 S2 27 3 15 39 38 41 4 7 11 28 30 S3 S4 Atom Peak x y z SOF Height Distances and Angles S1 0. 0.6567 0.3622 0.1655 1.000 3.94 0 S2 2.773 0 P5 2.810 60.3 0 1 1.507 120.6 120.2 0 2 1.575 28.0 88.3 108.2 0 6 2.633 150.9 118.4 31.6 138.3 0 8 2.696 151.2 123.4 83.7 135.4 56.8 0 9 1.717 125.0 125.8 102.1 110.2 80.9 26.8 0 10 3.044 165.7 133.8 53.1 137.8 28.3 30.6 52.7 0 16 1.720 86.5 26.3 109.0 114.6 96.0 100.5 112.1 107.6 0 18 3.163 28.3 32.0 126.1 56.3 142.6 146.4 131.7 165.6 58.2 0 33 2.694 145.0 137.7 29.0 122.8 19.8 55.2 73.4 25.1 115.8 154.8 0 34 2.958 56.9 107.9 71.0 37.2 101.4 128.7 117.4 110.1 129.4 80.6 88.6 0 36 2.641 24.8 47.2 105.9 47.3 130.3 169.0 148.7 158.2 71.6 22.7 134.8 0 38 3.161 106.1 142.3 97.2 83.8 90.6 51.8 30.4 64.9 139.8 126.7 74.9 0 42 1.917 90.2 56.7 63.6 107.5 69.7 116.0 142.3 96.6 51.1 72.9 84.8 S2 0. 0.8919 0.4149 0.1581 1.000 2.70 0 S1 2.773 0 P5 2.802 60.5 0 2 1.569 28.2 88.7 0 3 1.679 125.6 121.3 112.7 0 4 1.650 120.6 124.3 106.4 102.0 0 7 3.027 172.2 127.0 144.2 54.2 54.6 0 11 2.641 148.6 116.7 137.6 83.9 31.4 29.8 0 15 2.561 155.6 114.1 145.5 33.6 82.8 28.2 55.8 0 16 3.173 32.7 27.8 60.9 129.6 128.3 154.7 137.2 137.9 0 18 1.499 90.5 30.0 118.6 105.7 110.3 97.1 91.2 87.1 57.7 0 28 3.268 146.6 136.4 124.6 74.8 28.3 27.2 19.8 55.1 153.5 110.4 0 31 2.019 87.0 63.6 100.3 59.1 152.1 98.4 121.0 70.5 72.5 61.9 125.5 0 34 2.735 65.0 114.7 44.4 68.4 112.8 110.1 128.6 101.1 92.0 136.8 108.9 0 36 1.171 71.3 47.5 89.7 77.3 162.5 115.0 132.6 87.8 53.9 54.3 142.1 0 37 3.058 94.9 98.6 90.8 32.7 133.3 86.2 115.9 61.5 98.2 97.6 107.2 0 39 2.162 160.5 100.0 171.2 64.0 67.5 27.0 36.1 30.5 127.8 70.0 47.2 0 41 1.895 158.9 133.2 134.5 65.1 40.2 14.7 20.8 42.7 157.5 104.4 12.5 S3 0. 0.6953 0.6574 0.0028 1.000 2.37 0 P5 2.087 0 5 1.813 98.8 0 12 2.681 95.0 25.3 0 17 2.750 101.6 27.0 52.2 0 40 2.113 82.6 175.9 151.0 156.5 4 S4 3.308 101.2 123.4 100.3 145.6 52.5 7 28 3.274 153.7 106.9 105.7 103.9 71.4 59.8 9 30 2.664 148.7 89.4 79.6 99.3 87.5 50.7 29.9 S4 0. 0.7548 0.4176 -0.0787 1.000 2.16 0 P5 2.090 0 13 2.741 104.0 0 14 1.812 99.0 28.0 0 21 2.858 92.9 53.8 25.8 0 31 3.001 58.9 48.4 41.2 47.6 0 42 2.871 54.6 94.0 69.5 48.4 54.7 2 S3 3.308 156.7 95.7 92.6 88.8 133.3 112.5 6 28 3.282 137.5 75.1 97.2 116.8 119.7 165.0 59.6 8 30 2.622 151.4 54.1 70.0 87.3 102.5 135.3 51.8 29.7 13 40 2.627 124.0 131.7 132.0 121.9 168.9 116.8 39.7 66.4 78.7 P5 0. 0.7439 0.4891 0.0355 1.000 2.64 0 S1 2.810 0 S2 2.802 59.2 0 S3 2.087 126.1 129.6 0 S4 2.090 122.0 121.2 98.0 0 2 3.180 29.7 29.6 135.0 127.0 0 16 1.479 31.0 90.2 107.4 108.3 60.7 0 18 1.680 85.7 26.5 115.3 109.5 56.0 116.7 0 31 2.627 75.8 43.5 153.2 78.1 56.0 98.9 44.9 0 36 2.188 62.3 23.2 149.6 99.2 37.2 90.8 34.7 21.1 0 42 2.378 42.4 80.9 140.9 79.7 59.0 40.5 101.9 65.1 67.3 1 96. 0.6150 0.2389 0.1543 1.000 4.33 0 S1 1.507 0 6 1.564 118.1 0 33 1.559 123.0 34.2 0 42 1.837 69.1 103.0 137.1 2 91. 0.7840 0.3578 0.2000 1.000 3.52 0 S1 1.575 0 S2 1.569 123.8 0 P5 3.180 62.0 61.8 0 34 1.952 113.6 101.4 129.1 0 36 1.954 96.3 36.8 42.6 93.7 3 90. 0.9995 0.3193 0.1409 1.000 2.30 0 S2 1.679 0 15 1.488 107.8 0 31 1.848 69.6 106.4 0 36 1.824 38.8 113.5 31.0 0 37 1.877 118.5 118.7 60.5 84.7 0 41 1.932 62.8 59.4 119.5 96.0 178.1 4 90. 0.9518 0.5024 0.2244 1.000 2.57 0 S2 1.650 0 11 1.504 113.7 0 28 1.977 128.3 36.8 0 41 1.240 80.5 46.1 48.2 5 77. 0.8334 0.7069 -0.0369 1.000 1.43 0 S3 1.813 0 12 1.298 118.1 0 17 1.400 117.1 124.8 6 75. 0.4819 0.2184 0.1409 1.000 4.93 0 S1 2.633 0 1 1.564 30.3 0 10 1.445 91.8 109.3 0 33 0.917 83.8 72.6 61.5 7 75. 1.1498 0.4634 0.1739 1.000 1.47 0 S2 3.027 0 11 1.503 60.7 0 15 1.433 57.5 112.1 0 28 1.500 85.4 46.5 141.2 0 39 1.476 41.8 62.9 53.0 107.4 0 41 1.288 22.0 45.6 79.2 63.4 56.0 8 73. 0.4425 0.3952 0.2271 1.000 5.19 0 S1 2.696 0 9 1.399 33.7 0 10 1.552 87.2 110.4 9 72. 0.5621 0.4137 0.2364 1.000 4.64 0 S1 1.717 0 8 1.399 119.5 0 38 1.890 122.3 102.9 10 71. 0.4179 0.2654 0.2077 1.000 5.47 0 S1 3.044 0 6 1.445 59.8 0 8 1.552 62.2 115.4 0 33 1.291 62.1 38.7 122.6 0 43 1.973 137.3 160.5 84.0 132.5 11 68. 1.0640 0.5563 0.1969 1.000 1.80 0 S2 2.641 0 4 1.504 34.9 0 7 1.503 89.5 110.4 0 28 1.187 111.5 93.9 66.6 0 39 1.556 54.9 89.8 57.7 121.5 0 41 1.100 37.7 54.2 56.8 80.3 55.9 12 67. 0.9106 0.7459 0.0128 1.000 1.23 0 S3 2.681 0 5 1.298 36.6 0 22 1.472 153.0 116.5 0 27 2.029 150.3 133.0 39.8 0 35 1.202 141.4 123.4 39.2 67.7 13 65. 0.9595 0.2951 -0.0767 1.000 1.45 0 S4 2.741 0 14 1.423 36.7 0 24 1.453 151.1 115.0 14 64. 0.8396 0.2889 -0.0557 1.000 2.13 0 S4 1.812 0 13 1.423 115.3 0 21 1.459 121.4 123.3 0 31 2.026 102.7 84.7 83.9 15 64. 1.1037 0.3861 0.1148 1.000 1.54 0 S2 2.561 0 3 1.488 38.6 0 7 1.433 94.3 114.5 0 39 1.299 57.5 96.1 65.2 0 41 1.737 47.7 73.1 46.8 48.4 16 62. 0.6435 0.4357 0.0768 1.000 3.42 0 S1 1.720 0 S2 3.173 60.7 0 P5 1.479 122.7 62.0 0 42 1.579 70.9 83.4 102.0 17 60. 0.8477 0.7023 -0.1196 1.000 0.96 0 S3 2.750 0 5 1.400 36.0 0 19 1.375 153.7 118.1 18 59. 0.8737 0.4780 0.0810 1.000 2.27 0 S1 3.163 0 S2 1.499 61.2 0 P5 1.680 62.3 123.6 0 31 1.863 78.8 72.9 95.6 0 36 1.252 54.5 49.4 95.5 29.2 19 56. 0.9475 0.7489 -0.1516 1.000 0.24 0 17 1.375 0 20 1.413 119.0 20 54. 1.0380 0.7840 -0.0999 1.000 0.00 0 19 1.413 0 22 1.328 120.3 0 35 2.015 107.3 22.2 21 52. 0.7865 0.1868 -0.0191 1.000 2.77 0 S4 2.858 0 14 1.459 32.8 0 23 1.256 152.9 120.3 22 51. 1.0199 0.7894 -0.0219 1.000 0.46 0 12 1.472 0 20 1.328 120.6 0 27 1.301 93.9 116.4 0 35 0.932 54.6 125.2 118.3 23 48. 0.8483 0.1015 0.0011 1.000 2.75 0 21 1.256 0 25 1.474 124.0 0 26 1.490 120.0 111.2 24 46. 1.0303 0.1989 -0.0483 1.000 1.45 0 13 1.453 0 26 1.399 118.6 11 34 2.026 139.3 102.1 25 45. 0.8028 -0.0169 0.0140 1.000 3.26 0 23 1.474 0 32 1.085 116.0 26 42. 0.9743 0.0990 -0.0200 1.000 2.05 0 23 1.490 0 24 1.399 120.8 27 36. 1.0852 0.7232 0.0223 1.000 0.50 0 12 2.029 0 22 1.301 46.4 0 35 1.927 35.3 25.2 28 35. 1.1183 0.5196 0.2515 1.000 1.89 0 S2 3.268 0 4 1.977 23.4 0 7 1.500 67.4 89.4 0 11 1.187 48.8 49.4 66.9 0 30 1.641 125.7 103.8 140.1 93.5 0 41 1.476 16.1 38.8 51.3 47.3 136.2 29 34. 0.5509 0.0812 0.2484 1.000 5.41 0 33 1.704 30 33. 1.1250 0.6466 0.2960 1.000 1.83 0 28 1.641 31 32. 0.8966 0.3216 0.0563 1.000 2.36 0 S2 2.019 0 S4 3.001 115.4 0 P5 2.627 72.9 43.0 0 3 1.848 51.2 158.9 122.7 0 14 2.026 151.1 36.1 78.3 156.5 0 18 1.863 45.2 74.7 39.5 86.2 109.8 0 36 0.982 22.3 96.2 53.4 73.1 130.0 38.4 0 37 1.878 103.3 139.1 161.0 60.5 103.6 146.2 117.9 32 32. 0.8647 -0.0805 0.0360 1.000 3.20 0 25 1.085 12 35 1.594 139.4 33 32. 0.4996 0.1922 0.1911 1.000 5.14 0 S1 2.694 0 1 1.559 28.0 0 6 0.917 76.4 73.2 0 10 1.291 92.8 118.7 79.8 0 29 1.704 113.6 100.8 147.3 128.2 34 31. 0.8408 0.2002 0.2190 1.000 3.66 0 S1 2.958 0 S2 2.735 58.1 0 2 1.952 29.2 34.2 5 24 2.026 113.7 149.8 142.7 35 31. 0.9635 0.8350 0.0030 1.000 0.76 0 12 1.202 0 20 2.015 94.9 0 22 0.932 86.2 32.6 0 27 1.927 77.0 69.0 36.5 10 32 1.594 96.4 141.1 173.6 149.9 36 30. 0.8638 0.3723 0.0977 1.000 2.61 0 S1 2.641 0 S2 1.171 83.9 0 P5 2.188 70.4 109.2 0 2 1.954 36.3 53.4 100.1 0 3 1.824 125.8 63.9 158.8 91.4 0 18 1.252 102.8 76.3 49.8 108.8 109.6 0 31 0.982 128.7 139.1 105.5 138.8 75.9 112.4 37 30. 0.9632 0.1798 0.0882 1.000 2.48 0 S2 3.058 0 3 1.877 28.9 0 31 1.878 40.0 59.0 38 30. 0.5851 0.3877 0.3464 1.000 5.12 0 S1 3.161 0 9 1.890 27.3 39 29. 1.0547 0.4879 0.1172 1.000 1.58 0 S2 2.162 0 7 1.476 111.2 0 11 1.556 89.0 59.4 0 15 1.299 92.0 61.8 116.8 0 41 1.308 60.4 54.7 44.1 83.6 40 29. 0.5360 0.6077 0.0558 1.000 3.48 0 S3 2.113 41 29. 1.0411 0.4635 0.1927 1.000 2.07 0 S2 1.895 0 3 1.932 52.0 0 4 1.240 59.2 107.3 0 7 1.288 143.3 97.4 155.3 0 11 1.100 121.5 156.8 79.7 77.5 0 15 1.737 89.6 47.5 148.3 54.1 116.4 0 28 1.476 151.4 145.6 93.0 65.3 52.4 118.6 0 39 1.308 82.8 77.1 116.0 69.3 80.0 48.0 118.9 42 29. 0.6623 0.3021 0.0591 1.000 3.51 0 S1 1.917 0 S4 2.871 126.7 0 P5 2.378 80.9 45.7 0 1 1.837 47.3 173.2 128.2 0 16 1.579 58.0 75.7 37.5 100.4 43 28. 0.3072 0.2766 0.2972 1.000 6.41 0 10 1.973 Atom Code x y z Height Symmetry transformation S3 1 1.3426 0.6953 0.2528 0.49 2.0000-Y 0.0000+X 0.2500+Z S3 2 0.6574 0.3047 -0.2472 2.01 0.0000+Y 1.0000-X -0.2500+Z S4 3 1.2452 0.5824 0.4213 2.01 2.0000-X 1.0000-Y 0.5000+Z S4 4 0.5824 0.7548 0.1713 3.54 1.0000-Y 0.0000+X 0.2500+Z 24 5 0.8011 0.0303 0.2017 4.10 1.0000-Y -1.0000+X 0.2500+Z 28 6 0.8817 0.4804 -0.2485 0.60 2.0000-X 1.0000-Y -0.5000+Z 28 7 0.5196 0.8817 0.0015 2.74 0.0000+Y 2.0000-X -0.2500+Z 30 8 0.8750 0.3534 -0.2040 1.10 2.0000-X 1.0000-Y -0.5000+Z 30 9 0.6466 0.8750 0.0460 2.38 0.0000+Y 2.0000-X -0.2500+Z 32 10 0.8647 0.9195 0.0360 1.22 0.0000+X 1.0000+Y 0.0000+Z 34 11 1.2002 0.1592 -0.0310 0.82 1.0000+Y 1.0000-X -0.2500+Z 35 12 0.9635 -0.1650 0.0030 2.74 0.0000+X -1.0000+Y 0.0000+Z 40 13 0.6077 0.4640 -0.1942 2.19 0.0000+Y 1.0000-X -0.2500+Z 0.0 seconds CPU time +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src0011 finished at 15:26:24 Total CPU time: 6.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++