++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XS - CRYSTAL STRUCTURE SOLUTION - SHELXTL Ver. 6.12 W95/98/NT/2000/ME + + Copyright(c) 2001 Bruker AXS All Rights Reserved + + shelxs started at 21:40:58 on 14-Nov-2010 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL p-1 in P1 CELL 0.71073 8.9722 6.8630 15.3273 90.000 90.092 90.000 ZERR 5.00 0.0006 0.0005 0.0008 0.000 0.004 0.000 LATT -1 SFAC C H N O UNIT 40 50 10 5 V = 943.80 At vol = 17.2 F(000) = 400.0 mu = 0.09 mm-1 Max single Patterson vector = 27.8 cell wt = 750.90 rho = 1.321 OMIT 4.00 180.00 ESEL 1.200 5.000 0.005 0.700 0 TREF HKLF 4 14056 Reflections read, of which 0 rejected Maximum h, k, l and 2-Theta = 11. 8. 19. 55.14 INCONSISTENT EQUIVALENTS h k l F*F Sigma(F*F) Esd of mean(F*F) 1 5 1 0.87 0.21 1.45 -1 5 2 1.70 0.29 1.53 0 -3 8 0.16 0.02 0.15 -8 -1 8 0.74 0.46 4.34 3 3 8 0.57 0.19 1.52 3 0 9 0.04 0.01 0.21 6 -2 15 0.64 0.15 0.99 4248 Unique reflections, of which 2393 observed R(int) = 0.0848 R(sigma) = 0.1102 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. 23. 61. 98. 112. 147. 99. 126. 192. 252. 333. 434. 394. N(measured) 9. 25. 84. 125. 144. 185. 133. 180. 250. 348. 475. 733. 1122. N(theory) 19. 26. 84. 125. 144. 185. 133. 180. 250. 348. 475. 736. 1151. 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 = 7930 / 21240 Observed E .GT. 1.200 1.300 1.400 1.500 1.600 1.700 1.800 1.900 2.000 2.100 Number 888 781 679 600 524 457 385 339 295 238 Centric Acentric 0kl h0l hk0 Rest Mean Abs(E*E-1) 0.968 0.736 1.073 1.453 1.237 1.059 0.1 seconds elapsed time SUMMARY OF PARAMETERS FOR p-1 in P1 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 18 nf 8 s+ 0.800 s- 0.200 wr 0.200 PHAN steps 10 cool 0.900 Boltz 0.300 ns 419 mtpr 40 mnqr 10 TREF np 256. nE 556 kapscal -0.750 ntan 3 wn -0.750 FMAP code 8 PLAN npeaks -71 del1 0.500 del2 1.500 MORE verbosity 1 TIME t 9999999. 400 Reflections and 6912. unique TPR for phase annealing 400 Phases refined using 7414. unique TPR 400 Reflections and 7414. unique TPR for R(alpha) 0.1 seconds elapsed time 3661 Unique negative quartets found, 3661 used for phase refinement 0.1 seconds elapsed time Highest memory used to derive phase relations = 5131 / 79165 Following phases held constant with unit weights for the initial 4 weighted tangent cycles (before phase annealing): h k l E Phase/Comment 1 0 4 2.982 random phase -2 2 4 3.237 random phase -1 -2 8 3.132 random phase -3 -1 6 2.640 random phase 2 0 4 2.377 random phase 3 1 6 2.346 random phase 3 -1 6 2.343 random phase -1 1 2 2.306 random phase -1 -1 2 2.272 random phase 4 1 2 2.306 random phase 4 -1 2 2.299 random phase 1 2 0 1.832 random phase -1 2 0 1.822 random phase 2 0 0 1.491 random phase 1 1 3 1.785 random phase 1 -1 3 1.760 random phase 2 4 0 1.462 random phase -2 4 0 1.453 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 952 Unique NQR employed in phase annealing 128 Parallel refinements, highest memory = 18908 / 133971 0.0 seconds elapsed time STRUCTURE SOLUTION for p-1 in P1 Phase annealing cycle: 1 Beta = 0.10221 Ralpha 0.049 0.063 0.051 0.067 0.069 0.066 0.068 0.062 0.067 0.071 0.069 0.069 0.049 0.072 0.063 0.057 0.066 0.072 0.068 0.058 Nqual -0.728 0.080-0.686 0.450 0.288 0.348 0.414 0.232 0.585-0.115 0.620 0.490-0.664 0.617 0.609-0.523 0.528 0.695 0.493-0.344 Mabs 1.127 1.274 1.102 1.303 1.301 1.302 1.294 1.284 1.304 1.133 1.317 1.318 1.143 1.326 1.260 1.074 1.306 1.336 1.286 1.093 Phase annealing cycle: 2 Beta = 0.11357 Ralpha 0.035 0.054 0.038 0.048 0.054 0.050 0.048 0.043 0.049 0.059 0.047 0.044 0.037 0.050 0.044 0.039 0.044 0.050 0.047 0.047 Nqual -0.797-0.550-0.808-0.329-0.318-0.368-0.299-0.396 0.240-0.532 0.012-0.204-0.793 0.291 0.296-0.806-0.112 0.431 0.145-0.725 Mabs 1.088 1.098 1.066 1.142 1.127 1.155 1.112 1.141 1.190 1.051 1.157 1.171 1.080 1.180 1.133 1.047 1.155 1.202 1.175 1.052 Phase annealing cycle: 3 Beta = 0.12619 Ralpha 0.035 0.055 0.039 0.052 0.055 0.046 0.048 0.045 0.041 0.040 0.045 0.044 0.039 0.047 0.044 0.039 0.043 0.045 0.045 0.054 Nqual -0.815-0.486-0.806-0.404-0.387-0.508-0.362-0.494 0.038-0.748-0.430-0.337-0.811 0.031 0.194-0.817-0.408 0.178-0.010-0.789 Mabs 1.085 1.128 1.079 1.147 1.136 1.146 1.124 1.140 1.162 1.067 1.155 1.174 1.077 1.181 1.157 1.088 1.145 1.181 1.175 1.043 Phase annealing cycle: 4 Beta = 0.14021 Ralpha 0.038 0.051 0.040 0.051 0.056 0.047 0.048 0.046 0.041 0.035 0.044 0.042 0.040 0.047 0.045 0.036 0.042 0.043 0.045 0.055 Nqual -0.812-0.496-0.801-0.479-0.373-0.406-0.365-0.505-0.019-0.804-0.502-0.432-0.822-0.328 0.093-0.818-0.315 0.002-0.033-0.799 Mabs 1.100 1.132 1.091 1.128 1.150 1.164 1.133 1.149 1.163 1.104 1.132 1.150 1.079 1.150 1.164 1.081 1.162 1.168 1.168 1.047 Phase annealing cycle: 5 Beta = 0.15579 Ralpha 0.038 0.052 0.041 0.050 0.055 0.046 0.045 0.048 0.042 0.038 0.046 0.045 0.039 0.050 0.048 0.038 0.044 0.042 0.046 0.056 Nqual -0.818-0.486-0.803-0.422-0.306-0.440-0.267-0.458-0.012-0.815-0.520-0.473-0.818-0.377 0.105-0.812-0.434-0.065-0.119-0.766 Mabs 1.109 1.145 1.092 1.154 1.162 1.161 1.158 1.158 1.165 1.102 1.135 1.158 1.080 1.123 1.185 1.087 1.154 1.151 1.166 1.057 Phase annealing cycle: 6 Beta = 0.17310 Ralpha 0.037 0.055 0.040 0.052 0.054 0.048 0.044 0.052 0.041 0.038 0.048 0.048 0.039 0.058 0.046 0.038 0.044 0.045 0.046 0.044 Nqual -0.809-0.477-0.798-0.463-0.396-0.388-0.279-0.556-0.020-0.824-0.481-0.417-0.795-0.514 0.031-0.820-0.519-0.258-0.118-0.779 Mabs 1.113 1.153 1.089 1.152 1.151 1.157 1.167 1.130 1.172 1.100 1.139 1.166 1.089 1.080 1.174 1.093 1.142 1.135 1.162 1.079 Phase annealing cycle: 7 Beta = 0.19233 Ralpha 0.037 0.053 0.039 0.053 0.054 0.049 0.042 0.052 0.039 0.039 0.053 0.045 0.038 0.056 0.048 0.036 0.048 0.050 0.047 0.038 Nqual -0.811-0.429-0.800-0.474-0.406-0.421-0.259-0.626-0.038-0.813-0.504-0.453-0.800-0.554 0.076-0.802-0.543-0.383-0.260-0.817 Mabs 1.110 1.155 1.092 1.149 1.144 1.157 1.173 1.104 1.154 1.095 1.140 1.152 1.088 1.102 1.181 1.098 1.145 1.134 1.128 1.099 Phase annealing cycle: 8 Beta = 0.21370 Ralpha 0.039 0.054 0.041 0.052 0.054 0.048 0.042 0.053 0.039 0.040 0.051 0.043 0.042 0.054 0.046 0.041 0.047 0.054 0.050 0.035 Nqual -0.806-0.402-0.813-0.492-0.401-0.424-0.305-0.637-0.116-0.813-0.402-0.520-0.801-0.518 0.100-0.825-0.448-0.389-0.371-0.806 Mabs 1.113 1.160 1.095 1.136 1.149 1.154 1.173 1.106 1.146 1.103 1.164 1.140 1.094 1.112 1.185 1.100 1.165 1.137 1.136 1.106 Phase annealing cycle: 9 Beta = 0.23745 Ralpha 0.041 0.056 0.039 0.052 0.055 0.049 0.045 0.054 0.039 0.040 0.051 0.044 0.040 0.060 0.047 0.038 0.047 0.051 0.054 0.038 Nqual -0.816-0.511-0.811-0.440-0.292-0.321-0.269-0.689-0.129-0.814-0.411-0.497-0.818-0.628 0.132-0.809-0.413-0.382-0.329-0.805 Mabs 1.109 1.146 1.100 1.146 1.170 1.174 1.183 1.092 1.139 1.097 1.158 1.142 1.094 1.093 1.197 1.103 1.168 1.158 1.147 1.111 Phase annealing cycle: 10 Beta = 0.26383 Ralpha 0.041 0.053 0.038 0.053 0.055 0.048 0.045 0.054 0.040 0.041 0.054 0.045 0.041 0.057 0.047 0.040 0.047 0.051 0.058 0.038 Nqual -0.811-0.395-0.812-0.400-0.366-0.358-0.259-0.740-0.140-0.825-0.342-0.455-0.815-0.627 0.126-0.813-0.460-0.350-0.310-0.813 Mabs 1.102 1.163 1.104 1.152 1.166 1.171 1.180 1.075 1.136 1.105 1.179 1.151 1.098 1.094 1.191 1.106 1.172 1.163 1.162 1.113 Phase refinement cycle: 1 Ralpha 0.042 0.059 0.038 0.058 0.062 0.056 0.052 0.058 0.041 0.040 0.056 0.054 0.041 0.059 0.047 0.039 0.052 0.052 0.061 0.037 Nqual -0.883-0.252-0.886-0.259-0.292-0.320-0.021-0.666-0.138-0.891-0.111-0.281-0.888-0.658 0.276-0.888-0.286-0.271-0.230-0.882 Mabs 1.093 1.194 1.093 1.183 1.189 1.185 1.211 1.094 1.149 1.091 1.201 1.185 1.087 1.094 1.207 1.090 1.189 1.176 1.185 1.102 Phase refinement cycle: 2 Ralpha 0.042 0.058 0.036 0.059 0.063 0.058 0.055 0.059 0.043 0.041 0.058 0.052 0.042 0.058 0.049 0.041 0.052 0.054 0.061 0.038 Nqual -0.885-0.285-0.905-0.182-0.226-0.287-0.096-0.707-0.167-0.898-0.196-0.200-0.883-0.764 0.049-0.899-0.290-0.216-0.229-0.875 Mabs 1.099 1.186 1.105 1.198 1.201 1.195 1.211 1.090 1.165 1.100 1.192 1.198 1.097 1.086 1.202 1.101 1.192 1.202 1.198 1.105 Try Ralpha Nqual Sigma-1 M(abs) CFOM Seminvariants 892565. 0.039 -0.887 0.000 1.101 0.039 268521. 0.056 -0.341 0.000 1.188 0.223 1342605. 0.037 -0.904 0.000 1.102 0.037 421569. 0.056 -0.225 0.000 1.195 0.331 10693. 0.060 -0.191 0.000 1.206 0.372 53465. 0.058 -0.294 0.000 1.195 0.266 267325. 0.054 -0.183 0.000 1.207 0.375 1336625. 0.055 -0.735 0.000 1.095 0.056 391669. 0.041 -0.193 0.000 1.174 0.352 1958345. 0.040 -0.897 0.000 1.101 0.040 1403117. 0.055 -0.296 0.000 1.187 0.261 724129. 0.051 -0.210 0.000 1.195 0.343 1523493. 0.043 -0.887 0.000 1.092 0.043 1326009. 0.053 -0.816 0.000 1.086 0.053 338589. 0.049 0.031 0.000 1.206 0.659 1692945. 0.040 -0.892 0.000 1.101 0.040 76117. 0.053 -0.308 0.000 1.191 0.249 380585. 0.054 -0.217 0.000 1.205 0.338 1902925. 0.057 -0.228 0.000 1.197 0.329 1126017. 0.038 -0.882 0.000 1.110 0.038 1435781. 0.038 -0.895 0.000 1.109 0.038 887449. 0.059 -0.205 0.000 1.206 0.356 242941. 0.048 -0.129 0.000 1.190 0.434 1214705. 0.046 0.033 0.000 1.185 0.658 1879221. 0.038 -0.898 0.000 1.101 0.038 1007497. 0.057 -0.168 0.000 1.205 0.395 843181. 0.050 -0.245 0.000 1.193 0.305 21601. 0.049 -0.264 0.000 1.191 0.285 108005. 0.055 -0.276 0.000 1.195 0.279 540025. 0.040 -0.903 0.000 1.104 0.040 602973. 0.049 -0.019 0.000 1.197 0.583 917713. 0.048 -0.244 0.000 1.183 0.305 455133. 0.040 -0.900 0.000 1.108 0.040 1999989. 0.038 -0.897 0.000 1.103 0.038 1611337. 0.037 -0.905 0.000 1.104 0.037 1589949. 0.058 -0.241 0.000 1.194 0.317 1154117. 0.056 -0.220 0.000 1.196 0.337 1960677. 0.040 -0.893 0.000 1.101 0.040 2091693. 0.036 -0.894 0.000 1.104 0.036* 178949. 0.056 -0.254 0.000 1.195 0.302 2073201. 0.039 -0.891 0.000 1.105 0.039 91813. 0.049 -0.751 0.000 1.100 0.049 1411785. 0.059 -0.170 0.000 1.206 0.395 1498377. 0.039 -0.879 0.000 1.104 0.039 198173. 0.051 -0.267 0.000 1.190 0.285 437793. 0.048 -0.206 0.000 1.181 0.344 187989. 0.054 -0.329 0.000 1.195 0.231 1089561. 0.040 -0.895 0.000 1.106 0.040 402589. 0.061 -0.255 0.000 1.201 0.305 581165. 0.058 -0.310 0.000 1.193 0.252 1338809. 0.040 -0.897 0.000 1.109 0.040 825625. 0.052 -0.240 0.000 1.194 0.312 1526053. 0.039 -0.897 0.000 1.113 0.039 765277. 0.054 -0.167 0.000 1.202 0.394 1148721. 0.057 -0.086 0.000 1.208 0.497 1830777. 0.061 -0.246 0.000 1.197 0.315 1277785. 0.059 -0.225 0.000 1.205 0.334 654297. 0.054 -0.270 0.000 1.185 0.284 266317. 0.046 -0.151 0.000 1.181 0.405 1730985. 0.057 -0.167 0.000 1.201 0.397 102937. 0.056 -0.313 0.000 1.185 0.247 2061289. 0.058 -0.270 0.000 1.195 0.288 1200577. 0.040 -0.889 0.000 1.098 0.040 657081. 0.045 -0.042 0.000 1.190 0.546 2084081. 0.058 -0.253 0.000 1.199 0.305 1192761. 0.048 -0.174 0.000 1.198 0.381 1346373. 0.056 -0.265 0.000 1.192 0.291 226253. 0.042 -0.898 0.000 1.101 0.042 464681. 0.055 -0.154 0.000 1.206 0.411 1962665. 0.060 -0.293 0.000 1.198 0.269 2087029. 0.052 -0.763 0.000 1.105 0.052 1131265. 0.061 -0.158 0.000 1.209 0.411 269709. 0.056 -0.228 0.000 1.198 0.328 362253. 0.054 -0.272 0.000 1.193 0.282 937237. 0.060 -0.092 0.000 1.209 0.494 1507685. 0.053 -0.244 0.000 1.198 0.310 1312233. 0.055 -0.320 0.000 1.191 0.240 795965. 0.052 -0.301 0.000 1.185 0.253 453101. 0.055 -0.289 0.000 1.189 0.267 1815125. 0.057 -0.262 0.000 1.191 0.296 53689. 0.039 -0.892 0.000 1.103 0.039 1338385. 0.059 -0.308 0.000 1.192 0.255 1270029. 0.039 -0.901 0.000 1.110 0.039 745625. 0.058 -0.311 0.000 1.187 0.251 1505269. 0.060 -0.275 0.000 1.191 0.286 90077. 0.059 -0.256 0.000 1.197 0.303 1972485. 0.056 -0.185 0.000 1.190 0.375 1774901. 0.056 -0.288 0.000 1.188 0.270 2017025. 0.038 -0.904 0.000 1.107 0.038 1132181. 0.056 -0.218 0.000 1.199 0.339 403405. 0.050 -0.233 0.000 1.189 0.317 689317. 0.040 -0.890 0.000 1.107 0.040 1391373. 0.041 -0.903 0.000 1.101 0.041 455709. 0.054 -0.745 0.000 1.103 0.054 906965. 0.038 -0.900 0.000 1.099 0.038 756581. 0.048 0.032 0.000 1.192 0.659 1742241. 0.041 -0.891 0.000 1.096 0.041 1323157. 0.060 -0.214 0.000 1.197 0.347 1821593. 0.037 -0.906 0.000 1.104 0.037 1874237. 0.056 -0.331 0.000 1.190 0.232 1180021. 0.046 -0.149 0.000 1.177 0.407 719357. 0.039 -0.907 0.000 1.110 0.039 2058549. 0.039 -0.876 0.000 1.103 0.039 412661. 0.040 -0.899 0.000 1.097 0.040 513653. 0.059 -0.192 0.000 1.204 0.370 49029. 0.051 -0.810 0.000 1.086 0.051 360469. 0.057 -0.318 0.000 1.193 0.243 1981097. 0.057 -0.314 0.000 1.183 0.248 1349797. 0.056 -0.284 0.000 1.191 0.273 180861. 0.042 -0.894 0.000 1.098 0.042 1140665. 0.057 -0.285 0.000 1.187 0.273 228133. 0.054 -0.329 0.000 1.183 0.231 572853. 0.039 -0.903 0.000 1.097 0.039 395469. 0.058 -0.174 0.000 1.205 0.389 1828293. 0.057 -0.244 0.000 1.190 0.313 1977345. 0.059 -0.433 0.000 1.114 0.160 1358369. 0.059 -0.235 0.000 1.196 0.324 183389. 0.058 -0.676 0.000 1.102 0.064 328605. 0.060 -0.306 0.000 1.186 0.257 937449. 0.056 -0.313 0.000 1.187 0.247 477149. 0.048 -0.064 0.000 1.201 0.520 96809. 0.052 -0.196 0.000 1.173 0.359 344325. 0.054 -0.316 0.000 1.188 0.242 1165513. 0.053 -0.135 0.000 1.203 0.432 1143929. 0.055 -0.219 0.000 1.192 0.337 1787709. 0.055 -0.326 0.000 1.183 0.234 1420717. 0.042 -0.890 0.000 1.099 0.042 1417797. 0.055 -0.292 0.000 1.184 0.265 907605. 0.038 -0.897 0.000 1.109 0.038 1718605. 0.041 -0.892 0.000 1.100 0.041 204417. 0.036 -0.898 0.000 1.098 0.036 1022085. 0.041 -0.879 0.000 1.104 0.041 916121. 0.039 -0.888 0.000 1.107 0.039 386301. 0.039 -0.880 0.000 1.102 0.039 1931505. 0.038 -0.900 0.000 1.106 0.038 1268917. 0.037 -0.887 0.000 1.107 0.037 265645. 0.040 -0.896 0.000 1.099 0.040 1328225. 0.038 -0.904 0.000 1.106 0.038 349669. 0.042 -0.898 0.000 1.099 0.042 1765585. 0.042 -0.905 0.000 1.095 0.042 99433. 0.059 -0.665 0.000 1.107 0.066 497165. 0.039 -0.882 0.000 1.105 0.039 388673. 0.042 -0.887 0.000 1.104 0.042 349629. 0.040 -0.882 0.000 1.114 0.040 1760585. 0.039 -0.893 0.000 1.101 0.039 1457977. 0.037 -0.901 0.000 1.106 0.037 998429. 0.037 -0.886 0.000 1.107 0.037 797841. 0.041 -0.896 0.000 1.101 0.041 957729. 0.036 -0.893 0.000 1.105 0.036* 1642521. 0.041 -0.901 0.000 1.094 0.041 238537. 0.042 -0.901 0.000 1.101 0.042 1717361. 0.040 -0.892 0.000 1.104 0.040 44265. 0.041 -0.910 0.000 1.108 0.041 796717. 0.042 -0.891 0.000 1.107 0.042 421201. 0.049 -0.783 0.000 1.096 0.049 2031777. 0.050 -0.802 0.000 1.085 0.050 1351969. 0.040 -0.865 0.000 1.105 0.040 532589. 0.038 -0.884 0.000 1.104 0.038 346849. 0.040 -0.900 0.000 1.095 0.040 792273. 0.038 -0.898 0.000 1.101 0.038 1213765. 0.038 -0.900 0.000 1.107 0.038 1245637. 0.037 -0.888 0.000 1.113 0.037 757677. 0.040 -0.894 0.000 1.099 0.040 2053809. 0.038 -0.897 0.000 1.106 0.038 1197401. 0.039 -0.906 0.000 1.105 0.039 1418629. 0.040 -0.898 0.000 1.103 0.040 885813. 0.037 -0.908 0.000 1.105 0.037 827465. 0.041 -0.899 0.000 1.100 0.041 1266233. 0.038 -0.901 0.000 1.104 0.038 821153. 0.038 -0.898 0.000 1.104 0.038 1256229. 0.041 -0.886 0.000 1.101 0.041 CFOM Range Frequency 0.000 - 0.020 0 0.020 - 0.040 49 0.040 - 0.060 34 0.060 - 0.080 2 0.080 - 0.100 0 0.100 - 0.120 0 0.120 - 0.140 0 0.140 - 0.160 1 0.160 - 0.180 1 0.180 - 0.200 1 0.200 - 0.220 1 0.220 - 0.240 7 0.240 - 0.260 19 0.260 - 0.280 19 0.280 - 0.300 25 0.300 - 0.320 22 0.320 - 0.340 18 0.340 - 0.360 16 0.360 - 0.380 6 0.380 - 0.400 8 0.400 - 0.420 10 0.420 - 0.440 4 0.440 - 0.460 0 0.460 - 0.480 2 0.480 - 0.500 2 0.500 - 0.520 1 0.520 - 0.540 0 0.540 - 0.560 1 0.560 - 0.580 0 0.580 - 0.600 1 0.600 - 9.999 6 256. Phase sets refined - best is code 957729. with CFOM = 0.0356 6.4 seconds elapsed time Tangent expanded to 888 out of 888 E greater than 1.200 Highest memory used = 3662 / 2665 0.0 seconds elapsed time FMAP and GRID set by program FMAP 8 2 31 GRID -3.571 -2 -2 3.571 2 2 E-Fourier for p-1 in P1 Maximum = 363.87, minimum = -99.71 highest memory used = 9114 / 17452 0.0 seconds elapsed time Peak list optimization RE = 0.183 for 43 surviving atoms and 888 E-values Highest memory used = 1929 / 7992 0.0 seconds elapsed time E-Fourier for p-1 in P1 Maximum = 342.49, minimum = -91.11 highest memory used = 9114 / 17452 0.0 seconds elapsed time Peak list optimization RE = 0.174 for 41 surviving atoms and 888 E-values Highest memory used = 1929 / 7992 0.0 seconds elapsed time E-Fourier for p-1 in P1 Maximum = 335.92, minimum = -80.00 highest memory used = 9114 / 17452 0.0 seconds elapsed time Molecule 1 scale 0.872 inches = 2.214 cm per Angstrom 36 52 41 65 12 24 18 14 55 19 21 1 60 27 60 61 25 61 22 68 Atom Peak x y z SOF Height Distances and Angles 1 336. 0.1798 0.5053 0.0371 1.000 2.15 0 25 1.245 0 61 1.155 56.8 12 288. -0.3730 0.5347 0.0374 1.000 0.00 0 52 1.192 14 286. -0.1020 0.2789 0.0337 1.000 0.91 0 19 1.434 0 24 1.347 123.0 18 273. -0.1982 -0.0208 0.0866 1.000 1.02 0 24 1.399 0 55 1.318 119.2 0 65 1.919 134.9 104.9 19 272. 0.0137 0.1828 -0.0143 1.000 0.77 0 14 1.434 0 21 1.424 114.0 0 27 1.396 122.9 122.9 21 266. 0.0175 -0.0229 -0.0024 1.000 0.84 0 19 1.424 0 55 1.383 120.3 0 60 1.896 136.3 103.4 22 262. 0.3070 0.5182 -0.0997 1.000 1.08 0 25 1.512 0 61 1.639 42.3 0 68 1.214 130.5 163.5 24 255. -0.2072 0.1819 0.0788 1.000 0.98 0 14 1.347 0 18 1.399 119.7 0 41 1.417 121.3 118.5 25 254. 0.1916 0.4370 -0.0378 1.000 1.31 0 1 1.245 0 22 1.512 119.9 0 27 1.302 123.1 116.6 0 61 1.144 57.6 74.8 149.5 27 243. 0.1190 0.2832 -0.0639 1.000 0.66 0 19 1.396 0 25 1.302 124.8 36 218. -0.5012 0.5243 0.1696 1.000 1.02 0 52 1.547 41 202. -0.3166 0.2822 0.1280 1.000 1.16 0 24 1.417 0 52 1.333 125.5 52 162. -0.3882 0.4428 0.1027 1.000 0.65 0 12 1.192 0 36 1.547 116.2 0 41 1.333 128.7 115.0 55 128. -0.0823 -0.1125 0.0534 1.000 1.05 0 18 1.318 0 21 1.383 122.6 60 76. 0.1323 -0.2334 -0.0458 1.000 0.70 0 21 1.896 2 61 1.307 143.6 61 74. 0.1941 0.6009 -0.0244 1.000 1.54 0 1 1.155 0 22 1.639 116.6 0 25 1.144 65.6 62.9 1 60 1.307 130.6 112.7 143.3 65 66. -0.2999 -0.2138 0.1548 1.000 1.32 0 18 1.919 68 62. 0.4090 0.4382 -0.1374 1.000 1.02 0 22 1.214 Atom Code x y z Height Symmetry transformation 60 1 0.1323 0.7666 -0.0458 1.12 0.0000+X 1.0000+Y 0.0000+Z 61 2 0.1941 -0.3991 -0.0244 1.12 0.0000+X -1.0000+Y 0.0000+Z Molecule 2 scale 0.599 inches = 1.523 cm per Angstrom 38 63 58 23 10 15 63 5 58 53 40 51 4 37 69 66 31 34 54 47 71 33 20 6 48 62 8 59 45 44 42 13 32 29 39 11 35 49 57 26 43 17 7 16 9 28 67 56 46 3 30 50 64 2 70 Atom Peak x y z SOF Height Distances and Angles 2 329. 0.4993 0.0235 0.9209 1.000 2.22 0 50 1.515 0 64 1.050 94.8 0 70 1.303 125.9 61.7 3 328. 0.6250 0.0026 0.7859 1.000 2.65 0 50 1.244 0 67 2.023 124.6 4 309. 0.6237 -0.9415 0.2849 1.000 2.63 0 54 1.286 5 302. 1.0137 -0.6143 0.2428 1.000 3.03 0 15 1.388 0 40 1.454 121.1 0 53 1.381 121.1 117.7 6 301. 1.1827 -0.4461 0.5372 1.000 1.57 0 34 1.238 0 69 1.994 78.2 7 299. 1.1788 0.0443 0.7850 1.000 1.66 0 35 1.211 8 298. 1.0123 -0.1170 0.4857 1.000 3.16 0 20 1.379 0 44 1.418 122.1 0 45 1.415 122.0 115.8 9 297. 0.9030 -0.2230 0.7948 1.000 1.38 0 26 1.444 0 46 1.321 122.6 10 294. 1.1758 -0.9851 0.2824 1.000 1.40 0 23 1.194 0 58 1.361 60.9 11 291. 0.7915 -0.1136 0.5789 1.000 3.10 0 17 1.392 0 43 1.360 118.2 0 44 1.387 120.0 121.6 13 287. 0.6287 -0.4765 0.5373 1.000 2.60 0 49 1.221 0 62 1.994 160.0 15 281. 1.1218 -0.7171 0.1973 1.000 2.76 0 5 1.388 0 23 1.390 130.2 16 281. 0.4996 -0.4661 0.6760 1.000 2.13 0 49 1.559 17 275. 0.6831 -0.2143 0.6256 1.000 2.77 0 11 1.392 0 49 1.398 129.9 0 67 1.342 128.8 94.6 20 271. 1.1182 -0.2155 0.4378 1.000 2.92 0 8 1.379 0 34 1.380 127.1 23 261. 1.1957 -0.8887 0.2187 1.000 1.99 0 10 1.194 0 15 1.390 126.1 0 38 1.584 117.3 116.2 0 58 1.304 65.9 139.6 63.5 26 247. 1.0141 -0.3203 0.7425 1.000 1.16 0 9 1.444 0 29 1.410 115.2 0 32 1.405 121.9 122.7 28 243. 0.7841 -0.5191 0.8269 1.000 0.58 0 46 1.392 0 56 1.768 140.3 0 57 1.401 118.1 101.5 29 234. 0.9989 -0.5245 0.7370 1.000 0.62 0 26 1.410 0 57 1.313 121.1 0 59 1.941 131.1 107.5 30 231. 0.6855 -0.2190 0.8876 1.000 1.32 0 46 1.441 0 50 1.296 122.8 31 231. 0.7949 -0.6084 0.3368 1.000 2.98 0 33 1.442 0 40 1.371 117.1 0 47 1.387 121.6 121.0 32 225. 1.1236 -0.2166 0.6964 1.000 1.49 0 26 1.405 0 35 1.353 129.0 33 224. 0.6856 -0.7154 0.3863 1.000 2.61 0 31 1.442 0 54 1.279 126.9 0 62 1.229 128.2 97.4 34 223. 1.1961 -0.3798 0.4625 1.000 2.15 0 6 1.238 0 20 1.380 120.3 0 51 1.472 123.4 116.1 35 219. 1.1948 -0.0502 0.7190 1.000 1.71 0 7 1.211 0 32 1.353 127.5 0 42 1.520 117.2 115.3 37 214. 0.8868 -0.3180 0.2746 1.000 3.98 0 47 1.354 0 53 1.367 123.1 0 66 0.883 119.0 117.3 0 71 1.194 48.2 171.2 71.5 38 213. 1.3045 -0.9734 0.1468 1.000 1.92 0 23 1.584 0 58 1.538 49.3 39 208. 0.9109 0.1815 0.5482 1.000 3.89 0 43 1.360 0 45 1.395 122.2 40 205. 0.9036 -0.7145 0.2958 1.000 2.67 0 5 1.454 0 31 1.371 119.3 42 195. 1.3064 0.0252 0.6526 1.000 2.07 0 35 1.520 43 195. 0.7979 0.0835 0.5878 1.000 3.62 0 11 1.360 0 39 1.360 118.6 44 192. 0.8982 -0.2155 0.5320 1.000 2.85 0 8 1.418 0 11 1.387 121.2 45 192. 1.0161 0.0879 0.4960 1.000 3.69 0 8 1.415 0 39 1.395 120.3 46 188. 0.7953 -0.3178 0.8353 1.000 1.10 0 9 1.321 0 28 1.392 119.9 0 30 1.441 122.1 118.0 47 185. 0.7832 -0.4087 0.3243 1.000 3.65 0 31 1.387 0 37 1.354 118.7 0 66 1.942 141.8 23.4 0 71 1.050 175.6 57.9 35.0 48 183. 0.5011 -0.9570 0.4259 1.000 2.07 0 54 1.545 49 182. 0.6078 -0.3866 0.6050 1.000 2.54 0 13 1.221 0 16 1.559 120.8 0 17 1.398 123.1 116.0 0 67 2.014 153.9 79.6 41.6 50 178. 0.6142 -0.0662 0.8607 1.000 2.06 0 2 1.515 0 3 1.244 117.5 0 30 1.296 118.1 124.1 0 64 1.914 33.1 102.5 121.1 51 174. 1.3035 -0.4561 0.3986 1.000 2.06 0 34 1.472 53 160. 1.0010 -0.4145 0.2345 1.000 3.69 0 5 1.381 0 37 1.367 120.1 0 63 1.464 121.1 118.7 0 66 1.938 143.5 23.9 95.0 54 151. 0.6148 -0.8677 0.3618 1.000 2.45 0 4 1.286 0 33 1.279 124.0 0 48 1.545 118.0 117.8 0 62 1.883 150.5 40.3 81.5 56 105. 0.6776 -0.7168 0.8666 1.000 0.00 0 28 1.768 57 105. 0.8828 -0.6138 0.7703 1.000 0.41 0 28 1.401 0 29 1.313 121.8 58 92. 1.1869 -1.0753 0.2036 1.000 1.55 0 10 1.361 0 23 1.304 53.2 0 38 1.538 110.3 67.2 2 63 1.774 123.7 158.5 124.9 59 92. 1.1174 -0.7186 0.6765 1.000 0.15 0 29 1.941 62 67. 0.5900 -0.6510 0.4358 1.000 2.73 0 13 1.994 0 33 1.229 125.2 0 54 1.883 157.4 42.3 63 67. 1.1038 -0.3036 0.1795 1.000 4.10 0 53 1.464 1 58 1.774 127.2 64 67. 0.4072 -0.0306 0.8862 1.000 2.44 0 2 1.050 0 50 1.914 52.1 0 70 1.227 69.3 104.1 66 65. 0.8739 -0.1942 0.2611 1.000 4.44 0 37 0.883 0 47 1.942 37.6 0 53 1.938 38.8 76.1 0 71 1.239 66.0 29.1 104.8 67 64. 0.5728 -0.1430 0.6752 1.000 2.93 0 3 2.023 0 17 1.342 119.0 0 49 2.014 145.3 43.8 69 62. 1.1563 -0.6846 0.4645 1.000 1.33 0 6 1.994 70 62. 0.3970 -0.0709 0.9639 1.000 1.92 0 2 1.303 0 64 1.227 48.9 71 61. 0.7834 -0.2571 0.3152 1.000 4.14 0 37 1.194 0 47 1.050 73.9 0 66 1.239 42.5 115.8 Atom Code x y z Height Symmetry transformation 58 1 1.1869 -0.0753 0.2036 4.47 0.0000+X 1.0000+Y 0.0000+Z 63 2 1.1038 -1.3036 0.1795 1.18 0.0000+X -1.0000+Y 0.0000+Z 0.0 seconds elapsed time +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + shelxs finished at 21:41:05 Total elapsed time: 6.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++