++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XS - CRYSTAL STRUCTURE SOLUTION - SHELXTL Ver. 6.12 W95/98/NT/2000/ME + + Copyright(c) 2001 Bruker AXS All Rights Reserved + + shelxs started at 13:55:33 on 18-Nov-2008 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL I2 in I2 CELL 0.71073 6.7095 4.7163 20.0338 90.000 92.902 90.000 ZERR 2.00 0.0003 0.0003 0.0013 0.000 0.004 0.000 LATT -2 SYMM -X, Y, -Z SFAC C H N O UNIT 16 16 4 6 V = 633.14 At vol = 24.4 F(000) = 188.0 mu = 0.07 mm-1 Max single Patterson vector = 54.6 cell wt = 360.33 rho = 0.945 OMIT 4.00 180.00 ESEL 1.200 5.000 0.005 0.700 0 TREF HKLF 4 1 0 0 -1 0 1 0 1 0 1 3631 Reflections read, of which 0 rejected Maximum h, k, l and 2-Theta = 8. 6. 25. 55.09 808 Unique reflections, of which 733 observed R(int) = 0.0414 R(sigma) = 0.0364 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) 3. 8. 17. 27. 26. 41. 21. 35. 43. 67. 88. 122. 174. N(measured) 3. 8. 17. 27. 28. 41. 21. 35. 44. 72. 89. 133. 211. N(theory) 4. 8. 17. 27. 28. 41. 21. 35. 44. 72. 89. 133. 215. 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 = 3220 / 4040 Observed E .GT. 1.200 1.300 1.400 1.500 1.600 1.700 1.800 1.900 2.000 2.100 Number 217 185 152 126 108 88 68 56 44 33 Centric Acentric 0kl h0l hk0 Rest Mean Abs(E*E-1) 0.968 0.736 0.700 1.011 0.825 0.796 0.0 seconds elapsed time SUMMARY OF PARAMETERS FOR I2 in I2 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 0.300 ns 141 mtpr 40 mnqr 10 TREF np 256. nE 186 kapscal 0.800 ntan 3 wn -0.750 FMAP code 8 PLAN npeaks -16 del1 0.500 del2 1.500 MORE verbosity 1 TIME t 9999999. 99 Reflections and 701. unique TPR for phase annealing 99 Phases refined using 701. unique TPR 99 Reflections and 701. unique TPR for R(alpha) 0.0 seconds elapsed time 121 Unique negative quartets found, 121 used for phase refinement 0.0 seconds elapsed time Highest memory used to derive phase relations = 1505 / 6036 ONE-PHASE SEMINVARIANTS h k l E P+ Phi 2 0 16 3.224 0.79 -4 0 8 3.124 1.00 -2 0 4 2.476 0.99 6 0 8 2.271 0.72 2 0 14 2.266 0.69 -4 0 6 1.629 0.73 4 0 12 1.442 0.36 0 0 20 1.617 0.27 2 0 18 1.603 0.32 4 0 10 1.277 0.65 4 0 6 1.398 0.43 -6 0 2 1.263 0.32 Expected value of Sigma-1 = 0.779 Following phases held constant with unit weights for the initial 4 weighted tangent cycles (before phase annealing): h k l E Phase/Comment -4 0 8 3.124 0 sigma-1 = 1.000 -2 0 4 2.476 0 sigma-1 = 0.993 -3 1 6 2.052 random phase -1 1 4 1.743 random phase 5 1 2 2.228 random phase -2 1 11 1.724 random phase -1 0 3 1.419 0 or 180 at random 0 1 9 1.566 random phase 0 3 3 1.806 random phase -3 2 7 1.629 random phase 1 0 3 1.434 0 or 180 at random -3 3 8 1.407 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 103 Unique NQR employed in phase annealing 128 Parallel refinements, highest memory = 2684 / 29806 0.0 seconds elapsed time STRUCTURE SOLUTION for I2 in I2 Phase annealing cycle: 1 Beta = 0.10151 Ralpha 0.051 0.081 0.069 0.048 0.072 0.083 0.078 0.085 0.069 0.069 0.053 0.065 0.043 0.051 0.059 0.364 0.063 0.056 0.057 0.082 Nqual 0.518-0.449-0.112 0.680-0.424-0.585-0.085 0.172-0.051-0.024 0.792-0.410 0.480 0.136-0.072 0.080 0.216 0.187-0.099 0.050 Mabs 1.165 0.977 1.004 1.235 0.984 0.977 0.982 1.029 0.997 1.054 1.267 1.137 1.129 1.131 1.131 0.671 1.026 1.083 1.101 1.023 Phase annealing cycle: 2 Beta = 0.11279 Ralpha 0.053 0.058 0.070 0.025 0.089 0.059 0.059 0.087 0.056 0.061 0.025 0.052 0.037 0.041 0.038 0.195 0.057 0.052 0.049 0.065 Nqual -0.241-0.593-0.393 0.044-0.676-0.726-0.672-0.341-0.597-0.313 0.210-0.325-0.209-0.210-0.346-0.423-0.552-0.404-0.413-0.504 Mabs 1.032 0.976 0.998 1.108 0.900 0.954 0.969 0.916 0.942 0.996 1.095 1.023 1.040 1.024 1.038 0.767 0.967 1.006 1.029 0.958 Phase annealing cycle: 3 Beta = 0.12532 Ralpha 0.042 0.048 0.084 0.027 0.087 0.059 0.058 0.074 0.056 0.058 0.029 0.050 0.034 0.044 0.045 0.157 0.056 0.044 0.047 0.056 Nqual -0.188-0.684-0.373 0.068-0.672-0.777-0.711-0.302-0.600-0.270 0.431-0.439-0.038-0.232-0.324-0.430-0.604-0.302-0.312-0.474 Mabs 1.045 0.966 0.978 1.113 0.927 0.956 0.984 0.977 0.977 1.027 1.127 1.070 1.067 1.056 1.086 0.796 0.984 1.033 1.060 1.003 Phase annealing cycle: 4 Beta = 0.13925 Ralpha 0.037 0.060 0.084 0.027 0.079 0.048 0.063 0.090 0.051 0.071 0.024 0.050 0.039 0.054 0.041 0.143 0.054 0.046 0.044 0.044 Nqual -0.321-0.642-0.395-0.073-0.669-0.780-0.742-0.333-0.643-0.378 0.273-0.645-0.109-0.514-0.350-0.392-0.605-0.291-0.400-0.535 Mabs 1.074 0.962 0.971 1.113 0.946 0.957 0.966 0.942 0.981 1.007 1.104 1.035 1.056 1.005 1.083 0.832 0.995 1.054 1.049 1.003 Phase annealing cycle: 5 Beta = 0.15472 Ralpha 0.033 0.050 0.077 0.028 0.082 0.044 0.057 0.082 0.050 0.070 0.027 0.052 0.046 0.054 0.038 0.132 0.047 0.039 0.042 0.039 Nqual -0.334-0.744-0.318-0.098-0.631-0.779-0.706-0.393-0.551-0.364 0.140-0.512-0.129-0.430-0.345-0.480-0.546-0.129-0.425-0.519 Mabs 1.071 0.992 0.991 1.106 0.946 0.979 0.997 0.959 0.999 1.006 1.085 1.021 1.047 1.008 1.081 0.831 0.989 1.072 1.060 1.007 Phase annealing cycle: 6 Beta = 0.17191 Ralpha 0.033 0.043 0.070 0.024 0.071 0.055 0.049 0.064 0.050 0.070 0.026 0.051 0.034 0.051 0.042 0.092 0.040 0.034 0.039 0.046 Nqual -0.279-0.712-0.375-0.053-0.641-0.795-0.752-0.267-0.496-0.413-0.019-0.566 0.000-0.317-0.360-0.501-0.396-0.122-0.286-0.449 Mabs 1.084 0.995 1.001 1.111 0.962 0.984 1.000 0.987 1.007 1.021 1.076 1.038 1.101 1.028 1.084 0.883 1.030 1.102 1.080 1.032 Phase annealing cycle: 7 Beta = 0.19101 Ralpha 0.038 0.036 0.076 0.024 0.064 0.041 0.050 0.069 0.047 0.062 0.027 0.045 0.033 0.050 0.041 0.076 0.056 0.038 0.039 0.046 Nqual -0.344-0.769-0.287-0.034-0.632-0.804-0.753-0.417-0.514-0.348 0.094-0.386-0.119-0.327-0.291-0.422-0.366-0.094-0.266-0.428 Mabs 1.095 1.011 1.002 1.120 0.982 1.011 1.007 0.988 1.021 1.030 1.103 1.083 1.101 1.056 1.086 0.923 1.041 1.109 1.096 1.028 Phase annealing cycle: 8 Beta = 0.21224 Ralpha 0.036 0.038 0.064 0.026 0.062 0.041 0.044 0.072 0.047 0.061 0.028 0.045 0.037 0.042 0.044 0.090 0.058 0.034 0.041 0.039 Nqual -0.346-0.730-0.350 0.012-0.616-0.744-0.778-0.458-0.467-0.376 0.006-0.382-0.102-0.235-0.326-0.490-0.402-0.196-0.312-0.454 Mabs 1.094 1.012 1.020 1.121 0.987 0.989 0.997 0.969 1.031 1.008 1.094 1.055 1.079 1.045 1.090 0.915 1.035 1.093 1.087 1.045 Phase annealing cycle: 9 Beta = 0.23582 Ralpha 0.035 0.034 0.066 0.029 0.065 0.038 0.041 0.069 0.045 0.053 0.028 0.048 0.033 0.049 0.049 0.081 0.056 0.035 0.043 0.039 Nqual -0.282-0.743-0.299 0.066-0.630-0.769-0.780-0.409-0.381-0.345 0.013-0.473-0.029-0.269-0.369-0.506-0.495-0.258-0.359-0.434 Mabs 1.109 1.011 1.022 1.135 0.993 1.016 0.998 0.988 1.042 1.036 1.092 1.060 1.100 1.056 1.070 0.949 1.050 1.096 1.094 1.056 Phase annealing cycle: 10 Beta = 0.26202 Ralpha 0.036 0.039 0.078 0.028 0.072 0.037 0.038 0.081 0.041 0.059 0.032 0.052 0.036 0.049 0.053 0.074 0.058 0.029 0.039 0.039 Nqual -0.263-0.733-0.288 0.107-0.717-0.752-0.789-0.380-0.348-0.408-0.157-0.384-0.038-0.346-0.469-0.548-0.465-0.318-0.356-0.453 Mabs 1.101 1.023 1.022 1.124 0.986 1.009 1.014 0.973 1.064 1.015 1.091 1.050 1.095 1.036 1.059 0.941 1.031 1.098 1.085 1.048 Phase refinement cycle: 1 Ralpha 0.036 0.041 0.071 0.030 0.067 0.047 0.037 0.073 0.041 0.057 0.036 0.044 0.035 0.045 0.053 0.074 0.054 0.032 0.039 0.035 Nqual -0.262-0.775-0.385 0.223-0.711-0.842-0.814-0.442-0.336-0.434-0.162-0.351-0.002-0.335-0.333-0.544-0.251-0.313-0.310-0.388 Mabs 1.115 1.020 1.031 1.133 1.010 1.015 1.028 0.973 1.069 1.028 1.074 1.098 1.112 1.039 1.081 0.976 1.058 1.100 1.100 1.070 Phase refinement cycle: 2 Ralpha 0.035 0.039 0.073 0.029 0.074 0.034 0.036 0.066 0.046 0.061 0.041 0.047 0.039 0.045 0.049 0.072 0.045 0.032 0.039 0.032 Nqual -0.204-0.779-0.367 0.073-0.779-0.799-0.839-0.414-0.248-0.395-0.203-0.516-0.052-0.298-0.481-0.512-0.272-0.287-0.179-0.366 Mabs 1.114 1.042 1.032 1.120 1.019 1.043 1.039 0.980 1.077 1.033 1.059 1.085 1.108 1.054 1.071 0.981 1.063 1.106 1.117 1.086 Try Ralpha Nqual Sigma-1 M(abs) CFOM Seminvariants 1420309. 0.032 -0.225 0.762 1.109 0.308 +++++ +++++ +- 810089. 0.032 -0.746 0.759 1.039 0.032* +++++ +++-+ ++ 1953293. 0.071 -0.369 0.529 1.027 0.216 -++-+ ---++ ++ 1377857. 0.033 0.014 0.691 1.126 0.616 +++++ +++++ ++ 597829. 0.064 -0.771 0.759 0.998 0.064 +++++ +++-+ ++ 891993. 0.032 -0.797 0.759 1.038 0.032 +++++ +++-+ ++ 265661. 0.041 -0.832 0.759 1.033 0.041 +++++ +++-+ ++ 1328305. 0.068 -0.472 0.601 0.996 0.145 -++-+ ---++ +- 350069. 0.045 -0.211 0.715 1.069 0.336 +++++ +++++ -+ 1750345. 0.060 -0.409 0.529 1.046 0.176 -++-+ ---++ ++ 363117. 0.034 -0.172 0.691 1.067 0.368 +++++ +++++ ++ 1815585. 0.048 -0.480 0.787 1.084 0.121 +++++ +++++ -- 689317. 0.036 -0.054 0.691 1.110 0.521 +++++ +++++ ++ 1349433. 0.046 -0.283 0.715 1.055 0.264 +++++ +++++ -+ 455709. 0.046 -0.427 0.787 1.094 0.151 +++++ +++++ -- 181393. 0.067 -0.519 0.565 0.992 0.120 -++-+ +--+- ++ 906965. 0.053 -0.316 0.715 1.034 0.241 +++++ +++++ -+ 340521. 0.034 -0.317 0.762 1.099 0.221 +++++ +++++ +- 1702605. 0.034 -0.194 0.762 1.116 0.343 +++++ +++++ +- 124417. 0.032 -0.376 0.691 1.085 0.172 +++++ +++++ ++ 622085. 0.033 -0.338 0.762 1.116 0.203 +++++ +++++ +- 1013273. 0.031 0.055 0.691 1.115 0.679 +++++ +++++ ++ 872061. 0.034 -0.407 0.691 1.091 0.152 +++++ +++++ ++ 166001. 0.035 -0.807 0.588 1.049 0.035 -++-- +--+- -- 830005. 0.035 -0.154 0.715 1.072 0.390 +++++ +++++ -+ 2052873. 0.041 -0.290 0.787 1.064 0.252 +++++ +++++ -- 1875757. 0.047 -0.491 0.787 1.087 0.114 +++++ +++++ -- 990177. 0.062 -0.543 0.529 1.029 0.104 -++-+ ---++ ++ 756581. 0.031 0.300 0.691 1.167 1.135 +++++ +++++ ++ 1685753. 0.044 -0.510 0.787 1.052 0.101 +++++ +++++ -- 40157. 0.037 -0.262 0.762 1.100 0.275 +++++ +++++ +- 200785. 0.035 0.232 0.762 1.138 1.000 +++++ +++++ +- 384225. 0.031 -0.383 0.691 1.097 0.166 +++++ +++++ ++ 1298669. 0.030 0.204 0.691 1.147 0.941 +++++ +++++ ++ 872901. 0.034 0.208 0.691 1.168 0.952 +++++ +++++ ++ 1217017. 0.041 -0.265 0.691 1.137 0.275 +++++ +++++ ++ 1642629. 0.040 -0.266 0.762 1.112 0.275 +++++ +++++ +- 1995085. 0.037 -0.347 0.691 1.073 0.199 +++++ +++++ ++ 252273. 0.046 -0.359 0.787 1.063 0.199 +++++ +++++ -- 1013441. 0.032 -0.336 0.762 1.114 0.203 +++++ +++++ +- 1542353. 0.045 -0.451 0.787 1.090 0.135 +++++ +++++ -- 399017. 0.027 -0.234 0.691 1.103 0.294 +++++ +++++ ++ 1035749. 0.034 0.223 0.691 1.173 0.980 +++++ +++++ ++ 854997. 0.033 0.139 0.691 1.141 0.824 +++++ +++++ ++ 70301. 0.042 -0.324 0.762 1.095 0.223 +++++ +++++ +- 1132181. 0.031 0.113 0.691 1.138 0.776 +++++ +++++ ++ 851005. 0.047 -0.406 0.787 1.074 0.165 +++++ +++++ -- 201889. 0.064 -0.615 0.691 0.993 0.082 +++++ +++++ ++ 296533. 0.043 -0.579 0.540 1.060 0.072 ++++- -+++- +- 1612985. 0.035 -0.302 0.691 1.119 0.236 +++++ +++++ ++ 1125493. 0.056 -0.428 0.787 1.040 0.160 +++++ +++++ -- 1208605. 0.034 -0.206 0.762 1.117 0.330 +++++ +++++ +- 982577. 0.040 -0.230 0.762 1.112 0.310 +++++ +++++ +- 241721. 0.033 -0.212 0.762 1.116 0.323 +++++ +++++ +- 1206709. 0.040 -0.249 0.762 1.099 0.291 +++++ +++++ +- 1968253. 0.042 -0.400 0.691 1.092 0.165 +++++ +++++ ++ 478737. 0.034 0.072 0.691 1.136 0.710 +++++ +++++ ++ 1848721. 0.046 -0.428 0.787 1.080 0.150 +++++ +++++ -- 1447645. 0.034 0.105 0.691 1.159 0.766 +++++ +++++ ++ 971829. 0.041 -0.352 0.691 1.076 0.200 +++++ +++++ ++ 874349. 0.053 -0.377 0.787 1.045 0.192 +++++ +++++ -- 783749. 0.039 -0.066 0.691 1.124 0.507 +++++ +++++ ++ 807597. 0.045 -0.273 0.715 1.051 0.273 +++++ +++++ -+ 697705. 0.046 -0.365 0.787 1.093 0.194 +++++ +++++ -- 258413. 0.033 -0.211 0.762 1.114 0.324 +++++ +++++ +- 1923045. 0.031 -0.329 0.762 1.114 0.209 +++++ +++++ +- 1804545. 0.031 -0.159 0.691 1.130 0.380 +++++ +++++ ++ 1379909. 0.031 -0.332 0.762 1.113 0.206 +++++ +++++ +- 943293. 0.040 -0.242 0.787 1.088 0.298 +++++ +++++ -- 1720081. 0.032 -0.385 0.691 1.117 0.166 +++++ +++++ ++ 27421. 0.039 -0.438 0.787 1.080 0.136 +++++ +++++ -- 1705801. 0.037 -0.049 0.695 1.123 0.529 +++++ +++++ ++ 1764893. 0.035 -0.255 0.762 1.114 0.279 +++++ +++++ +- 1942353. 0.035 -0.086 0.691 1.100 0.476 +++++ +++++ ++ 1927917. 0.035 -0.302 0.691 1.090 0.236 +++++ +++++ ++ 2063305. 0.033 -0.206 0.762 1.114 0.328 +++++ +++++ +- 92485. 0.048 -0.283 0.691 1.121 0.267 +++++ +++++ ++ 1706773. 0.047 -0.026 0.691 1.096 0.572 +++++ +++++ ++ 384609. 0.032 0.205 0.691 1.159 0.944 +++++ +++++ ++ 22269. 0.031 0.198 0.691 1.146 0.929 +++++ +++++ ++ 465057. 0.038 -0.204 0.787 1.109 0.337 +++++ +++++ -- 1981097. 0.038 -0.277 0.762 1.111 0.262 +++++ +++++ +- 135421. 0.034 -0.220 0.762 1.112 0.315 +++++ +++++ +- 1268097. 0.032 0.030 0.691 1.092 0.640 +++++ +++++ ++ 246745. 0.036 -0.334 0.691 1.112 0.209 +++++ +++++ ++ 617645. 0.043 -0.314 0.691 1.081 0.233 +++++ +++++ ++ 1947681. 0.039 -0.266 0.787 1.097 0.273 +++++ +++++ -- 1233725. 0.045 -0.173 0.762 1.110 0.378 +++++ +++++ +- 360469. 0.035 -0.199 0.762 1.121 0.338 +++++ +++++ +- 1482997. 0.034 -0.144 0.762 1.117 0.401 +++++ +++++ +- 637929. 0.035 0.206 0.691 1.166 0.949 +++++ +++++ ++ 1934321. 0.034 -0.110 0.691 1.127 0.443 +++++ +++++ ++ 760785. 0.034 -0.007 0.691 1.143 0.586 +++++ +++++ ++ 1349797. 0.030 0.161 0.691 1.141 0.860 +++++ +++++ ++ 1475005. 0.042 0.050 0.691 1.138 0.682 +++++ +++++ ++ 1889069. 0.031 0.427 0.691 1.165 1.415 +++++ +++++ ++ 1027993. 0.041 -0.344 0.787 1.075 0.205 +++++ +++++ -- 1358369. 0.036 -0.245 0.691 1.125 0.291 +++++ +++++ ++ 1106529. 0.040 -0.386 0.691 1.093 0.173 +++++ +++++ ++ 1068201. 0.030 -0.183 0.762 1.108 0.351 +++++ +++++ +- 800217. 0.037 -0.219 0.787 1.094 0.320 +++++ +++++ -- 305993. 0.038 -0.177 0.762 1.109 0.367 +++++ +++++ +- 2069301. 0.046 -0.312 0.762 1.088 0.239 +++++ +++++ +- 1954381. 0.034 -0.411 0.691 1.097 0.149 +++++ +++++ ++ 1952105. 0.043 -0.365 0.787 1.089 0.191 +++++ +++++ -- 2023965. 0.054 -0.530 0.529 1.013 0.102 -++-+ ---++ ++ 1903325. 0.052 -0.509 0.715 1.065 0.110 +++++ +++++ -+ 661937. 0.035 0.450 0.691 1.163 1.476 +++++ +++++ ++ 1400877. 0.031 -0.036 0.691 1.122 0.541 +++++ +++++ ++ 480629. 0.037 -0.404 0.691 1.106 0.156 +++++ +++++ ++ 303457. 0.041 -0.378 0.762 1.092 0.179 +++++ +++++ +- 1796629. 0.030 -0.065 0.691 1.117 0.500 +++++ +++++ ++ 170761. 0.063 -0.477 0.529 1.031 0.138 -++-+ ---++ ++ 873013. 0.040 0.002 0.691 1.142 0.605 +++++ +++++ ++ 827117. 0.046 -0.357 0.762 1.088 0.200 +++++ +++++ +- 1097585. 0.041 -0.291 0.787 1.102 0.252 +++++ +++++ -- 1293621. 0.034 -0.261 0.762 1.121 0.273 +++++ +++++ +- 384789. 0.040 -0.276 0.787 1.087 0.265 +++++ +++++ -- 1231117. 0.040 -0.233 0.762 1.107 0.308 +++++ +++++ +- 883245. 0.047 -0.401 0.691 1.058 0.169 +++++ +++++ ++ 417449. 0.037 -0.249 0.691 1.105 0.288 +++++ +++++ ++ 1492977. 0.034 -0.478 0.691 1.091 0.108 +++++ +++++ ++ 567205. 0.035 -0.152 0.762 1.114 0.392 +++++ +++++ +- 484045. 0.037 -0.235 0.762 1.109 0.302 +++++ +++++ +- 1428857. 0.051 -0.397 0.787 1.027 0.176 +++++ +++++ -- 1335249. 0.045 -0.401 0.730 1.081 0.167 +++++ +++++ +- 674961. 0.036 -0.254 0.691 1.125 0.282 +++++ +++++ ++ 1787709. 0.033 0.277 0.691 1.163 1.088 +++++ +++++ ++ 1767049. 0.048 -0.648 0.787 1.004 0.059 +++++ +++++ -- 136033. 0.046 -0.774 0.588 1.028 0.046 -++-- +--+- -- 680165. 0.058 -0.660 0.622 0.994 0.066 -++-+ +--++ ++ 1478421. 0.045 -0.766 0.759 1.033 0.045 +++++ +++-+ ++ 1308941. 0.065 -0.729 0.475 0.971 0.065 -++-+ ---+- ++ 1503481. 0.051 -0.638 0.529 1.022 0.063 -++-+ ---++ ++ 437537. 0.033 -0.804 0.759 1.038 0.033 +++++ +++-+ ++ CFOM Range Frequency 0.000 - 0.020 0 0.020 - 0.040 4 0.040 - 0.060 4 0.060 - 0.080 5 0.080 - 0.100 2 0.100 - 0.120 10 0.120 - 0.140 7 0.140 - 0.160 16 0.160 - 0.180 15 0.180 - 0.200 13 0.200 - 0.220 16 0.220 - 0.240 9 0.240 - 0.260 10 0.260 - 0.280 16 0.280 - 0.300 11 0.300 - 0.320 12 0.320 - 0.340 11 0.340 - 0.360 5 0.360 - 0.380 9 0.380 - 0.400 7 0.400 - 0.420 2 0.420 - 0.440 2 0.440 - 0.460 2 0.460 - 0.480 3 0.480 - 0.500 3 0.500 - 0.520 2 0.520 - 0.540 9 0.540 - 0.560 6 0.560 - 0.580 2 0.580 - 0.600 5 0.600 - 9.999 38 256. Phase sets refined - best is code 810089. with CFOM = 0.0321 0.7 seconds elapsed time Tangent expanded to 217 out of 217 E greater than 1.200 Highest memory used = 994 / 1168 0.0 seconds elapsed time FMAP and GRID set by program FMAP 8 2 13 GRID -5.000 -1 -2 5.000 1 2 E-Fourier for I2 in I2 Maximum = 407.84, minimum = -106.29 highest memory used = 8690 / 4861 0.0 seconds elapsed time Peak list optimization RE = 0.171 for 12 surviving atoms and 217 E-values Highest memory used = 1505 / 1953 0.0 seconds elapsed time E-Fourier for I2 in I2 Maximum = 374.60, minimum = -116.24 highest memory used = 8690 / 4861 0.0 seconds elapsed time Peak list optimization RE = 0.140 for 12 surviving atoms and 217 E-values Highest memory used = 1505 / 1953 0.0 seconds elapsed time E-Fourier for I2 in I2 Maximum = 365.21, minimum = -113.32 highest memory used = 8690 / 4861 0.0 seconds elapsed time Molecule 1 scale 0.905 inches = 2.300 cm per Angstrom 15 11 3 6 8 5 10 7 12 2 5 1 16 9 13 4 14 16 7 4 Atom Peak x y z SOF Height Distances and Angles 1 365. 0.8222 0.0000 0.3869 1.000 2.20 0 2 1.217 0 4 1.187 126.8 0 10 1.518 114.7 118.5 2 346. 0.6788 0.0192 0.3474 1.000 2.04 0 1 1.217 3 339. 1.2419 -0.6341 0.3418 1.000 2.28 0 8 1.357 0 11 1.338 123.2 4 338. 0.8548 0.1392 0.4356 1.000 2.33 0 1 1.187 0 14 1.628 126.3 5 336. 1.4148 -0.5770 0.4483 1.000 2.23 0 8 1.373 0 12 1.375 129.4 6 330. 0.9475 -0.3606 0.3114 1.000 2.22 0 10 1.334 0 11 1.438 116.7 0 15 1.245 165.5 51.7 7 326. 1.1242 -0.2824 0.4157 1.000 2.27 0 8 1.447 0 10 1.362 119.2 0 13 2.022 133.1 100.2 0 16 1.212 112.3 128.0 41.9 8 322. 1.2650 -0.5050 0.4023 1.000 2.25 0 3 1.357 0 5 1.373 122.4 0 7 1.447 116.5 121.1 9 320. 1.5000 -0.1661 0.5000 0.500 3.32 0 12 1.194 10 318. 0.9726 -0.2258 0.3698 1.000 2.24 0 1 1.518 0 6 1.334 118.4 0 7 1.362 117.8 123.7 11 288. 1.0937 -0.5718 0.2970 1.000 2.27 0 3 1.338 0 6 1.438 120.6 0 15 1.182 172.4 55.8 12 255. 1.5000 -0.4192 0.5000 0.500 2.59 0 5 1.375 0 9 1.194 122.8 2 5 1.375 114.5 122.8 13 118. 1.0000 -0.1481 0.5000 0.500 1.52 0 7 2.022 0 14 0.950 108.2 0 16 1.381 35.9 90.1 3 7 2.022 143.5 108.2 144.1 4 16 1.381 144.1 90.1 179.9 35.9 14 112. 1.0000 0.0534 0.5000 0.500 2.11 0 4 1.628 0 13 0.950 104.4 0 16 1.677 102.3 55.4 1 4 1.628 151.2 104.4 93.9 4 16 1.677 93.9 55.4 110.8 102.3 15 111. 0.9710 -0.4858 0.2577 1.000 2.38 0 6 1.245 0 11 1.182 72.6 16 106. 1.1731 -0.1485 0.4655 1.000 2.44 0 7 1.212 0 13 1.381 102.3 0 14 1.677 118.1 34.5 Atom Code x y z Height Symmetry transformation 4 1 1.1452 0.1392 0.5644 2.38 2.0000-X 0.0000+Y 1.0000-Z 5 2 1.5852 -0.5770 0.5517 2.04 3.0000-X 0.0000+Y 1.0000-Z 7 3 0.8758 -0.2824 0.5843 0.00 2.0000-X 0.0000+Y 1.0000-Z 16 4 0.8269 -0.1485 0.5345 0.60 2.0000-X 0.0000+Y 1.0000-Z 0.0 seconds elapsed time +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + shelxs finished at 13:55:34 Total elapsed time: 0.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++