++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XS - CRYSTAL STRUCTURE SOLUTION - SHELXTL Ver. 6.12 W95/98/NT/2000/ME + + Copyright(c) 2001 Bruker AXS All Rights Reserved + + shelxs started at 10:52:42 on 23-Nov-2010 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL Cc in Cc CELL 0.71073 3.8456 22.1895 9.4477 90.000 90.048 90.000 ZERR 4.00 0.0010 0.0045 0.0024 0.000 0.015 0.000 LATT -7 SYMM X, -Y, 0.5+Z SFAC C H N O UNIT 36 32 8 4 V = 806.19 At vol = 16.8 F(000) = 336.0 mu = 0.09 mm-1 Max single Patterson vector = 32.4 cell wt = 640.70 rho = 1.320 OMIT 4.00 180.00 ESEL 1.200 5.000 0.005 0.700 0 TREF HKLF 4 4221 Reflections read, of which 58 rejected Maximum h, k, l and 2-Theta = 5. 28. 12. 55.36 923 Unique reflections, of which 649 observed R(int) = 0.0889 R(sigma) = 0.0819 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. 8. 16. 27. 33. 38. 27. 36. 54. 71. 88. 104. 119. N(measured) 1. 8. 16. 27. 33. 41. 28. 38. 54. 77. 105. 157. 245. N(theory) 3. 8. 16. 27. 33. 41. 28. 38. 54. 77. 105. 157. 247. 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 = 3896 / 4615 Observed E .GT. 1.200 1.300 1.400 1.500 1.600 1.700 1.800 1.900 2.000 2.100 Number 234 189 149 124 100 72 51 41 38 32 Centric Acentric 0kl h0l hk0 Rest Mean Abs(E*E-1) 0.968 0.736 1.004 0.737 0.841 0.795 0.0 seconds elapsed time SUMMARY OF PARAMETERS FOR Cc in Cc 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 11 nf 16 s+ 0.800 s- 0.200 wr 0.200 PHAN steps 10 cool 0.900 Boltz 0.300 ns 150 mtpr 40 mnqr 10 TREF np 256. nE 200 kapscal 0.800 ntan 3 wn -0.750 FMAP code 8 PLAN npeaks -19 del1 0.500 del2 1.500 MORE verbosity 1 TIME t 9999999. 105 Reflections and 878. unique TPR for phase annealing 105 Phases refined using 878. unique TPR 105 Reflections and 878. unique TPR for R(alpha) 0.0 seconds elapsed time 67 Unique negative quartets found, 67 used for phase refinement 0.0 seconds elapsed time Highest memory used to derive phase relations = 1682 / 6392 ONE-PHASE SEMINVARIANTS h k l E P+ Phi 0 22 0 3.458 1.00 0 16 0 2.385 1.00 0 10 0 1.323 0.77 Expected value of Sigma-1 = 0.977 Following phases held constant with unit weights for the initial 4 weighted tangent cycles (before phase annealing): h k l E Phase/Comment 0 22 0 3.458 0 sigma-1 = 1.000 1 3 1 2.070 random phase 0 16 0 2.385 0 sigma-1 = 1.000 2 4 0 2.372 random phase 0 0 2 1.669 random phase 1 1 0 1.365 random phase 0 4 3 1.243 random phase 1 9 0 1.324 random phase 0 2 3 1.274 random phase -2 10 3 1.335 random phase 2 8 4 1.600 random phase -2 8 4 1.570 random phase 0 8 2 1.266 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 62 Unique NQR employed in phase annealing 128 Parallel refinements, highest memory = 2069 / 32400 0.0 seconds elapsed time STRUCTURE SOLUTION for Cc in Cc Phase annealing cycle: 1 Beta = 0.13144 Ralpha 0.068 0.073 0.056 0.109 0.064 0.076 0.079 0.068 0.090 0.069 0.060 0.064 0.079 0.071 0.064 0.086 0.071 0.076 0.076 0.055 Nqual -0.316-0.120-0.055-0.369-0.213-0.321 0.021-0.156-0.285-0.195-0.251-0.519-0.458-0.406 0.202-0.202 0.276-0.466-0.314-0.113 Mabs 1.045 1.017 1.067 0.946 1.024 0.975 1.042 1.006 0.930 0.985 1.020 1.001 1.017 1.012 1.022 0.952 1.027 0.993 1.053 1.047 Phase annealing cycle: 2 Beta = 0.14604 Ralpha 0.040 0.086 0.053 0.110 0.078 0.063 0.073 0.068 0.086 0.055 0.081 0.079 0.082 0.073 0.092 0.095 0.085 0.100 0.115 0.072 Nqual -0.535-0.327-0.475-0.606-0.389-0.363-0.332-0.396-0.408-0.562-0.323-0.549-0.481-0.562-0.376-0.469-0.282-0.640-0.448-0.531 Mabs 1.021 0.933 0.962 0.903 0.923 0.951 0.951 0.950 0.904 1.006 0.956 0.912 0.942 0.911 0.910 0.895 0.929 0.881 0.929 0.968 Phase annealing cycle: 3 Beta = 0.16227 Ralpha 0.046 0.106 0.046 0.080 0.065 0.052 0.072 0.064 0.075 0.050 0.057 0.077 0.052 0.077 0.080 0.089 0.064 0.100 0.093 0.051 Nqual -0.701-0.519-0.610-0.586-0.574-0.515-0.406-0.590-0.577-0.683-0.448-0.717-0.640-0.644-0.506-0.587-0.243-0.634-0.487-0.615 Mabs 1.054 0.948 1.024 0.957 0.940 1.044 0.961 0.995 0.969 1.039 1.003 0.939 1.025 0.964 0.989 0.922 0.964 0.910 0.987 1.017 Phase annealing cycle: 4 Beta = 0.18030 Ralpha 0.047 0.069 0.035 0.096 0.064 0.077 0.080 0.059 0.068 0.052 0.055 0.084 0.036 0.086 0.085 0.079 0.052 0.089 0.088 0.061 Nqual -0.640-0.596-0.662-0.600-0.478-0.555-0.544-0.643-0.676-0.737-0.504-0.662-0.651-0.597-0.499-0.360-0.566-0.712-0.558-0.637 Mabs 1.028 0.961 1.035 0.923 0.966 0.973 0.939 0.963 0.908 1.021 1.005 0.908 1.047 0.955 0.953 0.918 0.972 0.919 0.951 0.990 Phase annealing cycle: 5 Beta = 0.20033 Ralpha 0.056 0.091 0.036 0.068 0.062 0.072 0.069 0.065 0.065 0.058 0.049 0.072 0.043 0.078 0.069 0.083 0.065 0.072 0.075 0.045 Nqual -0.614-0.561-0.649-0.687-0.494-0.621-0.545-0.637-0.632-0.643-0.620-0.639-0.629-0.661-0.692-0.468-0.471-0.739-0.640-0.577 Mabs 1.058 0.977 1.089 0.978 1.002 0.993 0.991 0.984 0.961 1.057 1.011 0.950 1.063 0.960 0.962 0.941 0.977 0.963 1.019 1.069 Phase annealing cycle: 6 Beta = 0.22259 Ralpha 0.052 0.078 0.044 0.066 0.045 0.061 0.071 0.085 0.065 0.047 0.047 0.064 0.045 0.068 0.092 0.098 0.059 0.082 0.087 0.048 Nqual -0.692-0.496-0.601-0.753-0.548-0.657-0.472-0.669-0.633-0.650-0.726-0.563-0.630-0.658-0.589-0.624-0.346-0.696-0.664-0.642 Mabs 1.047 0.985 1.070 0.991 1.003 0.997 0.993 0.978 0.957 1.066 1.062 0.968 1.054 0.986 0.966 0.938 0.994 0.956 0.976 1.059 Phase annealing cycle: 7 Beta = 0.24732 Ralpha 0.058 0.071 0.044 0.065 0.045 0.054 0.069 0.068 0.072 0.045 0.042 0.068 0.041 0.086 0.086 0.069 0.062 0.084 0.096 0.042 Nqual -0.643-0.572-0.626-0.580-0.655-0.684-0.416-0.665-0.706-0.683-0.744-0.556-0.579-0.642-0.564-0.597-0.292-0.557-0.604-0.516 Mabs 1.053 1.009 1.062 0.985 1.059 1.025 0.995 1.001 0.950 1.047 1.049 0.988 1.050 0.983 0.952 0.958 1.010 0.987 0.956 1.076 Phase annealing cycle: 8 Beta = 0.27480 Ralpha 0.047 0.064 0.035 0.074 0.053 0.049 0.058 0.050 0.065 0.050 0.047 0.083 0.043 0.058 0.082 0.079 0.057 0.072 0.085 0.052 Nqual -0.589-0.621-0.671-0.575-0.614-0.603-0.534-0.625-0.696-0.622-0.680-0.561-0.647-0.633-0.653-0.593-0.332-0.579-0.649-0.677 Mabs 1.041 0.989 1.089 0.988 1.057 1.022 1.018 1.026 0.952 1.059 1.054 0.957 1.061 0.988 0.952 0.964 1.000 0.976 0.960 1.089 Phase annealing cycle: 9 Beta = 0.30534 Ralpha 0.044 0.069 0.036 0.067 0.049 0.053 0.072 0.056 0.065 0.053 0.044 0.077 0.038 0.080 0.070 0.070 0.067 0.072 0.077 0.050 Nqual -0.532-0.725-0.709-0.611-0.660-0.577-0.539-0.617-0.613-0.659-0.762-0.689-0.646-0.585-0.626-0.464-0.324-0.606-0.709-0.751 Mabs 1.067 0.991 1.072 1.010 1.063 1.055 0.984 1.045 0.956 1.074 1.056 0.966 1.084 1.008 1.000 1.038 0.982 0.978 1.006 1.073 Phase annealing cycle: 10 Beta = 0.33926 Ralpha 0.037 0.075 0.042 0.060 0.044 0.053 0.063 0.060 0.058 0.046 0.042 0.064 0.034 0.073 0.066 0.077 0.057 0.071 0.071 0.050 Nqual -0.500-0.738-0.659-0.600-0.691-0.670-0.441-0.679-0.602-0.631-0.723-0.629-0.603-0.638-0.582-0.462-0.549-0.663-0.652-0.720 Mabs 1.072 0.989 1.088 1.023 1.068 1.028 0.996 1.045 0.962 1.075 1.082 0.980 1.089 1.002 0.992 1.038 0.991 1.009 0.989 1.048 Phase refinement cycle: 1 Ralpha 0.036 0.072 0.042 0.067 0.054 0.058 0.053 0.055 0.056 0.047 0.043 0.053 0.039 0.063 0.059 0.071 0.051 0.082 0.073 0.047 Nqual -0.580-0.657-0.728-0.690-0.739-0.695-0.549-0.764-0.656-0.677-0.707-0.637-0.680-0.602-0.592-0.474-0.495-0.612-0.640-0.757 Mabs 1.108 0.997 1.090 1.049 1.083 1.016 1.042 1.072 1.021 1.083 1.092 1.012 1.112 1.021 1.003 1.056 1.038 1.017 1.008 1.073 Phase refinement cycle: 2 Ralpha 0.041 0.071 0.034 0.064 0.048 0.053 0.044 0.059 0.052 0.043 0.041 0.059 0.038 0.078 0.067 0.067 0.061 0.068 0.066 0.038 Nqual -0.595-0.671-0.689-0.693-0.661-0.580-0.509-0.702-0.693-0.588-0.688-0.578-0.676-0.660-0.681-0.557-0.642-0.605-0.680-0.718 Mabs 1.094 1.007 1.089 1.061 1.087 1.050 1.106 1.082 1.056 1.109 1.080 1.023 1.093 1.019 1.025 1.054 1.024 1.027 1.030 1.103 Try Ralpha Nqual Sigma-1 M(abs) CFOM Seminvariants 1420309. 0.038 -0.536 1.000 1.110 0.084 +++ 810089. 0.073 -0.633 0.900 1.008 0.087 ++- 1953293. 0.037 -0.737 1.000 1.087 0.037 +++ 1377857. 0.071 -0.728 1.000 1.059 0.071 +++ 597829. 0.043 -0.671 1.000 1.089 0.049 +++ 891993. 0.055 -0.595 1.000 1.061 0.079 +++ 265661. 0.035 -0.510 1.000 1.095 0.092 +++ 1328305. 0.058 -0.759 1.000 1.079 0.058 +++ 350069. 0.062 -0.656 1.000 1.062 0.071 +++ 1750345. 0.042 -0.580 1.000 1.096 0.071 +++ 363117. 0.037 -0.658 1.000 1.101 0.045 +++ 1815585. 0.055 -0.650 1.000 1.063 0.066 +++ 689317. 0.034 -0.717 1.000 1.098 0.035 +++ 1349433. 0.067 -0.685 0.900 1.016 0.071 ++- 455709. 0.068 -0.643 1.000 1.029 0.079 +++ 181393. 0.062 -0.578 -0.136 1.054 0.092 -+- 906965. 0.063 -0.645 1.000 1.041 0.074 +++ 340521. 0.075 -0.640 0.900 1.009 0.087 ++- 1702605. 0.066 -0.667 -0.036 1.028 0.073 -++ 124417. 0.037 -0.719 1.000 1.106 0.038 +++ 622085. 0.037 -0.461 1.000 1.076 0.120 +++ 1013273. 0.073 -0.463 1.000 1.022 0.156 +++ 872061. 0.034 -0.679 1.000 1.105 0.040 +++ 166001. 0.060 -0.659 1.000 1.076 0.069 +++ 830005. 0.042 -0.731 1.000 1.104 0.042 +++ 2052873. 0.036 -0.681 1.000 1.105 0.041 +++ 1875757. 0.051 -0.596 1.000 1.070 0.075 +++ 990177. 0.035 -0.757 1.000 1.090 0.035 +++ 756581. 0.036 -0.695 1.000 1.105 0.039 +++ 1685753. 0.047 -0.707 1.000 1.096 0.049 +++ 40157. 0.042 -0.658 1.000 1.100 0.050 +++ 200785. 0.066 -0.679 1.000 1.040 0.071 +++ 851005. 0.037 -0.636 1.000 1.109 0.050 +++ 76845. 0.052 -0.647 1.000 1.098 0.063 +++ 93977. 0.065 -0.717 0.900 1.016 0.066 ++- 1035749. 0.038 -0.661 1.000 1.096 0.046 +++ 1298669. 0.037 -0.718 1.000 1.104 0.038 +++ 399017. 0.038 -0.690 1.000 1.095 0.042 +++ 1890781. 0.033 -0.678 1.000 1.109 0.038 +++ 1131949. 0.032 -0.659 1.000 1.121 0.041 +++ 1465441. 0.040 -0.658 1.000 1.120 0.049 +++ 852921. 0.037 -0.691 1.000 1.108 0.040 +++ 1217017. 0.049 -0.692 1.000 1.100 0.052 +++ 80681. 0.040 -0.610 1.000 1.101 0.060 +++ 872901. 0.037 -0.688 1.000 1.100 0.041 +++ 1921125. 0.074 -0.619 0.900 1.025 0.091 ++- 252273. 0.047 -0.569 1.000 1.091 0.079 +++ 1642629. 0.056 -0.721 1.000 1.072 0.056 +++ 600553. 0.044 -0.653 1.000 1.092 0.053 +++ 874349. 0.038 -0.647 1.000 1.107 0.049 +++ 644529. 0.036 -0.714 1.000 1.101 0.037 +++ 539541. 0.048 -0.715 1.000 1.093 0.049 +++ 1482665. 0.040 -0.622 1.000 1.100 0.057 +++ 1499633. 0.036 -0.587 1.000 1.087 0.062 +++ 1433161. 0.047 -0.423 1.000 1.062 0.155 +++ 1878017. 0.043 -0.661 1.000 1.116 0.051 +++ 410665. 0.043 -0.643 1.000 1.091 0.055 +++ 2052569. 0.043 -0.680 1.000 1.098 0.048 +++ 1452657. 0.043 -0.617 1.000 1.109 0.061 +++ 697705. 0.037 -0.479 1.000 1.094 0.110 +++ 946769. 0.057 -0.598 1.000 1.051 0.080 +++ 1415041. 0.044 -0.393 1.000 1.082 0.171 +++ 1955161. 0.047 -0.664 1.000 1.094 0.054 +++ 971829. 0.058 -0.673 1.000 1.071 0.064 +++ 22269. 0.057 -0.634 1.000 1.049 0.071 +++ 844345. 0.036 -0.585 1.000 1.110 0.063 +++ 1379909. 0.030 -0.650 1.000 1.107 0.040 +++ 384609. 0.030 -0.711 1.000 1.108 0.032* +++ 1172861. 0.038 -0.657 1.000 1.105 0.046 +++ 1412773. 0.062 -0.667 1.000 1.045 0.069 +++ 556725. 0.042 -0.651 1.000 1.075 0.051 +++ 513653. 0.038 -0.621 1.000 1.104 0.055 +++ 2060581. 0.034 -0.649 1.000 1.109 0.044 +++ 1100621. 0.038 -0.626 1.000 1.109 0.054 +++ 608089. 0.048 -0.696 1.000 1.107 0.051 +++ 522161. 0.033 -0.627 1.000 1.097 0.048 +++ 1132077. 0.036 -0.621 1.000 1.118 0.053 +++ 686473. 0.062 -0.708 1.000 1.066 0.063 +++ 1764893. 0.039 -0.704 1.000 1.107 0.041 +++ 1292065. 0.041 -0.454 1.000 1.078 0.128 +++ 360469. 0.061 -0.684 1.000 1.080 0.066 +++ 266077. 0.056 -0.693 1.000 1.093 0.059 +++ 1018433. 0.041 -0.722 1.000 1.105 0.042 +++ 1225129. 0.034 -0.685 1.000 1.098 0.038 +++ 457529. 0.063 -0.711 1.000 1.005 0.065 +++ 991073. 0.038 -0.679 1.000 1.111 0.043 +++ 1233725. 0.043 -0.612 1.000 1.093 0.063 +++ 1092493. 0.074 -0.528 0.900 1.017 0.123 ++- 245145. 0.033 -0.611 1.000 1.081 0.052 +++ 1663073. 0.050 -0.652 1.000 1.097 0.059 +++ 677105. 0.034 -0.628 1.000 1.101 0.049 +++ 2044209. 0.067 -0.508 -0.136 1.053 0.126 -+- 897861. 0.052 -0.665 1.000 1.089 0.060 +++ 2068701. 0.043 -0.440 1.000 1.090 0.139 +++ 1330385. 0.054 -0.668 1.000 1.096 0.061 +++ 1349797. 0.049 -0.630 1.000 1.081 0.063 +++ 1035741. 0.048 -0.371 1.000 1.072 0.191 +++ 772361. 0.041 -0.675 1.000 1.105 0.047 +++ 1810109. 0.037 -0.661 1.000 1.113 0.045 +++ 434657. 0.046 -0.532 1.000 1.053 0.093 +++ 767113. 0.037 -0.654 1.000 1.094 0.046 +++ 404793. 0.045 -0.663 1.000 1.074 0.053 +++ 1338341. 0.052 -0.631 1.000 1.102 0.066 +++ 937449. 0.039 -0.689 1.000 1.109 0.043 +++ 1371917. 0.041 -0.666 1.000 1.120 0.048 +++ 1479597. 0.038 -0.667 1.000 1.103 0.045 +++ 156957. 0.053 -0.485 1.000 1.076 0.124 +++ 993333. 0.043 -0.619 1.000 1.092 0.060 +++ 500389. 0.047 -0.711 1.000 1.086 0.049 +++ 800217. 0.033 -0.685 1.000 1.108 0.037 +++ 1620313. 0.052 -0.678 1.000 1.083 0.058 +++ 1233589. 0.039 -0.649 1.000 1.108 0.049 +++ 1557589. 0.042 -0.613 1.000 1.091 0.061 +++ 113441. 0.059 -0.673 1.000 1.090 0.064 +++ 1975137. 0.044 -0.611 1.000 1.099 0.063 +++ 594033. 0.046 -0.585 1.000 1.064 0.073 +++ 288593. 0.050 -0.467 1.000 1.088 0.130 +++ 77765. 0.040 -0.613 1.000 1.100 0.058 +++ 13773. 0.043 -0.671 1.000 1.107 0.050 +++ 614201. 0.050 -0.692 1.000 1.085 0.053 +++ 1615833. 0.049 -0.699 1.000 1.095 0.051 +++ 221921. 0.041 -0.681 1.000 1.102 0.046 +++ 368629. 0.051 -0.679 1.000 1.089 0.056 +++ 1293621. 0.034 -0.677 1.000 1.096 0.039 +++ 861549. 0.037 -0.700 1.000 1.097 0.039 +++ 1124981. 0.044 -0.660 1.000 1.101 0.052 +++ 1572253. 0.036 -0.705 1.000 1.106 0.038 +++ 1760641. 0.033 -0.713 1.000 1.104 0.035 +++ 1340501. 0.046 -0.640 1.000 1.095 0.058 +++ 411049. 0.035 -0.653 1.000 1.098 0.044 +++ 1887617. 0.072 -0.686 -0.136 1.043 0.077 -+- 1049477. 0.037 -0.709 1.000 1.091 0.039 +++ 1053081. 0.070 -0.651 0.900 1.019 0.080 ++- 1161201. 0.036 -0.675 1.000 1.105 0.041 +++ 1611701. 0.037 -0.602 1.000 1.118 0.059 +++ 1767049. 0.036 -0.661 1.000 1.100 0.044 +++ 136033. 0.050 -0.587 1.000 1.052 0.077 +++ 680165. 0.047 -0.681 1.000 1.091 0.052 +++ 1303673. 0.031 -0.666 1.000 1.088 0.038 +++ 226909. 0.049 -0.587 1.000 1.097 0.076 +++ 1134545. 0.032 -0.651 1.000 1.114 0.042 +++ 1478421. 0.043 -0.643 1.000 1.098 0.054 +++ 1100649. 0.042 -0.721 1.000 1.092 0.043 +++ 1308941. 0.062 -0.701 1.000 1.025 0.064 +++ 1266245. 0.059 -0.698 1.000 1.076 0.062 +++ 39769. 0.060 -0.685 0.900 1.044 0.064 ++- 198845. 0.040 -0.670 1.000 1.080 0.046 +++ 994225. 0.063 -0.626 0.900 1.041 0.078 ++- 1786953. 0.070 -0.649 1.000 1.080 0.081 +++ 546157. 0.044 -0.719 1.000 1.100 0.045 +++ 1071013. 0.052 -0.609 1.000 1.053 0.072 +++ 1160761. 0.037 -0.661 1.000 1.113 0.045 +++ 1756049. 0.047 -0.612 1.000 1.055 0.066 +++ 1467917. 0.065 -0.641 -0.136 1.045 0.076 -+- 1935441. 0.047 -0.644 1.000 1.074 0.059 +++ 241177. 0.034 -0.666 1.000 1.089 0.041 +++ 355657. 0.038 -0.717 1.000 1.108 0.040 +++ 584233. 0.039 -0.679 1.000 1.105 0.044 +++ 536277. 0.065 -0.634 0.900 1.027 0.078 ++- 824013. 0.042 -0.697 1.000 1.100 0.045 +++ 1905633. 0.037 -0.633 1.000 1.105 0.051 +++ 151529. 0.037 -0.683 1.000 1.108 0.041 +++ 1748853. 0.032 -0.630 1.000 1.108 0.047 +++ 1971305. 0.041 -0.708 1.000 1.104 0.043 +++ 1503481. 0.058 -0.598 1.000 1.038 0.081 +++ 394261. 0.036 -0.676 1.000 1.112 0.041 +++ 333785. 0.041 -0.617 1.000 1.095 0.059 +++ 1326009. 0.035 -0.688 1.000 1.091 0.039 +++ 1611337. 0.039 -0.714 1.000 1.107 0.040 +++ 2057173. 0.054 -0.703 1.000 1.081 0.057 +++ 887449. 0.040 -0.717 1.000 1.089 0.041 +++ 686357. 0.042 -0.656 1.000 1.105 0.051 +++ 1576281. 0.032 -0.715 1.000 1.092 0.033 +++ 76117. 0.057 -0.656 1.000 1.094 0.066 +++ 1336625. 0.067 -0.652 0.900 1.037 0.077 ++- 1334633. 0.037 -0.680 1.000 1.108 0.042 +++ 917713. 0.057 -0.695 1.000 1.079 0.060 +++ 268521. 0.034 -0.658 1.000 1.105 0.042 +++ 452665. 0.031 -0.582 1.000 1.095 0.060 +++ 108005. 0.040 -0.698 1.000 1.097 0.043 +++ 843181. 0.040 -0.715 1.000 1.101 0.041 +++ 939945. 0.040 -0.669 1.000 1.101 0.047 +++ 1740193. 0.045 -0.683 1.000 1.090 0.050 +++ 2057037. 0.040 -0.660 1.000 1.114 0.048 +++ 2086497. 0.039 -0.722 1.000 1.099 0.040 +++ 187989. 0.047 -0.654 1.000 1.080 0.056 +++ 1734193. 0.059 -0.694 1.000 1.084 0.062 +++ 1584861. 0.071 -0.675 1.000 1.044 0.076 +++ 1896577. 0.036 -0.617 1.000 1.114 0.054 +++ 91813. 0.036 -0.686 1.000 1.098 0.040 +++ 1729233. 0.039 -0.553 1.000 1.089 0.077 +++ 52613. 0.038 -0.600 1.000 1.099 0.061 +++ 2073201. 0.057 -0.757 1.000 1.086 0.057 +++ 506989. 0.046 -0.651 1.000 1.087 0.056 +++ 1632849. 0.038 -0.643 1.000 1.105 0.049 +++ 339573. 0.048 -0.675 1.000 1.080 0.054 +++ 514685. 0.052 -0.706 1.000 1.093 0.054 +++ 1331585. 0.039 -0.628 1.000 1.092 0.054 +++ 1766257. 0.035 -0.641 1.000 1.092 0.047 +++ 1697865. 0.033 -0.665 1.000 1.102 0.040 +++ 2061289. 0.038 -0.636 1.000 1.084 0.051 +++ 1205013. 0.039 -0.588 1.000 1.096 0.065 +++ 476273. 0.038 -0.668 1.000 1.070 0.045 +++ 1174333. 0.048 -0.691 1.000 1.095 0.052 +++ 1157341. 0.039 -0.719 1.000 1.115 0.040 +++ 357605. 0.035 -0.675 1.000 1.099 0.040 +++ 1188253. 0.039 -0.590 1.000 1.086 0.065 +++ 2095349. 0.043 -0.693 1.000 1.098 0.046 +++ 581165. 0.045 -0.643 1.000 1.091 0.056 +++ 841765. 0.053 -0.761 -0.036 1.048 0.053 -++ 1864081. 0.058 -0.632 1.000 1.030 0.072 +++ 269709. 0.047 -0.692 1.000 1.083 0.051 +++ 966085. 0.035 -0.667 1.000 1.106 0.042 +++ 464681. 0.041 -0.704 1.000 1.100 0.043 +++ 1337933. 0.035 -0.692 1.000 1.099 0.038 +++ 72605. 0.051 -0.704 1.000 1.090 0.054 +++ 432481. 0.041 -0.670 1.000 1.092 0.048 +++ 1865169. 0.040 -0.620 1.000 1.122 0.057 +++ 1898541. 0.035 -0.644 1.000 1.111 0.046 +++ 326265. 0.034 -0.694 1.000 1.103 0.037 +++ 1018649. 0.040 -0.641 1.000 1.112 0.052 +++ 1320665. 0.035 -0.661 1.000 1.113 0.043 +++ 1327089. 0.041 -0.644 1.000 1.112 0.052 +++ 819109. 0.035 -0.701 1.000 1.104 0.037 +++ 1998393. 0.034 -0.677 1.000 1.091 0.040 +++ 1238641. 0.044 -0.701 1.000 1.095 0.046 +++ 1467225. 0.035 -0.669 1.000 1.105 0.041 +++ 252977. 0.039 -0.668 1.000 1.086 0.045 +++ 773865. 0.035 -0.663 1.000 1.106 0.043 +++ 1553413. 0.043 -0.675 1.000 1.102 0.049 +++ 1814097. 0.031 -0.640 1.000 1.107 0.043 +++ 1003925. 0.058 -0.674 1.000 1.073 0.064 +++ 1246969. 0.052 -0.608 1.000 1.056 0.072 +++ 1234889. 0.034 -0.688 1.000 1.103 0.038 +++ CFOM Range Frequency 0.000 - 0.020 0 0.020 - 0.040 29 0.040 - 0.060 128 0.060 - 0.080 55 0.080 - 0.100 17 0.100 - 0.120 3 0.120 - 0.140 10 0.140 - 0.160 5 0.160 - 0.180 3 0.180 - 0.200 4 0.200 - 0.220 0 0.220 - 0.240 2 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 384609. with CFOM = 0.0320 0.8 seconds elapsed time Tangent expanded to 234 out of 234 E greater than 1.200 Highest memory used = 1062 / 1369 0.0 seconds elapsed time FMAP and GRID set by program FMAP 8 1 11 GRID -6.250 -1 -2 6.250 1 2 E-Fourier for Cc in Cc Maximum = 384.65, minimum = -108.65 highest memory used = 8714 / 6004 0.0 seconds elapsed time Peak list optimization RE = 0.205 for 13 surviving atoms and 234 E-values Highest memory used = 1529 / 2106 0.0 seconds elapsed time E-Fourier for Cc in Cc Maximum = 383.63, minimum = -113.78 highest memory used = 8714 / 6004 0.0 seconds elapsed time Peak list optimization RE = 0.198 for 13 surviving atoms and 234 E-values Highest memory used = 1529 / 2106 0.0 seconds elapsed time E-Fourier for Cc in Cc Maximum = 375.96, minimum = -98.51 highest memory used = 8714 / 6004 0.0 seconds elapsed time Molecule 1 scale 0.673 inches = 1.709 cm per Angstrom 13 15 16 8 2 8 16 9 17 7 4 1 18 6 7 3 18 19 5 10 11 12 14 11 10 13 15 Atom Peak x y z SOF Height Distances and Angles 1 376. 0.3666 0.3164 0.7757 1.000 2.77 0 7 1.351 0 9 1.366 122.0 0 18 1.906 73.0 101.0 2 348. 0.6144 0.2307 0.8994 1.000 2.00 0 8 1.164 0 9 1.441 174.7 0 16 1.721 107.0 67.9 3 335. 0.1279 0.4016 0.9031 1.000 1.96 0 5 1.447 0 6 1.390 123.0 0 7 1.457 119.0 117.8 0 19 1.539 68.4 54.9 172.2 4 335. 0.3718 0.3165 1.0245 1.000 1.21 0 6 1.393 0 9 1.354 121.8 0 17 1.123 118.2 119.0 5 334. -0.0413 0.4598 0.8977 1.000 1.98 0 3 1.447 0 10 1.944 108.2 0 11 1.914 110.6 140.5 0 12 1.106 140.1 111.2 29.6 0 14 1.083 145.9 38.0 102.6 73.2 0 19 1.681 58.4 49.9 166.4 159.9 87.6 6 328. 0.1998 0.3717 1.0291 1.000 1.18 0 3 1.390 0 4 1.393 119.1 0 19 1.357 68.1 169.0 7 326. 0.2076 0.3706 0.7710 1.000 2.79 0 1 1.351 0 3 1.457 119.2 0 18 1.987 66.5 99.8 8 18 1.866 120.5 75.3 172.7 8 310. 0.7351 0.1826 0.9018 1.000 2.00 0 2 1.164 0 15 1.284 177.2 7 16 1.886 85.9 91.3 9 305. 0.4353 0.2878 0.9007 1.000 2.00 0 1 1.366 0 2 1.441 119.5 0 4 1.354 119.5 120.5 0 16 1.781 106.1 63.5 105.9 10 231. -0.1021 0.4883 1.0906 1.000 0.77 0 5 1.944 0 14 1.278 31.4 0 19 1.547 56.2 87.4 4 11 1.223 166.7 143.8 123.7 11 228. -0.0776 0.4874 0.7064 1.000 3.16 0 5 1.914 0 12 1.097 29.8 3 10 1.223 172.6 143.3 12 206. -0.1194 0.4945 0.8200 1.000 2.46 0 5 1.106 0 11 1.097 120.6 0 13 1.851 111.4 127.9 0 14 1.305 52.6 171.7 59.4 13 196. -0.3340 0.5592 0.9075 1.000 1.91 0 12 1.851 0 14 1.635 43.4 6 15 1.925 152.3 163.5 14 144. -0.1275 0.4985 0.9578 1.000 1.59 0 5 1.083 0 10 1.278 110.6 0 12 1.305 54.2 164.8 0 13 1.635 130.6 117.9 77.2 0 19 1.961 58.9 52.0 112.9 169.4 15 95. 0.8829 0.1307 0.9044 1.000 1.99 0 8 1.284 5 13 1.925 171.8 16 90. 0.1697 0.2220 0.9023 1.000 2.17 0 2 1.721 0 9 1.781 48.6 2 8 1.886 158.8 152.6 17 90. 0.4105 0.2914 1.1265 1.000 0.59 0 4 1.123 18 83. 0.7234 0.3760 0.7742 1.000 2.56 0 1 1.906 0 7 1.987 40.5 1 7 1.866 132.4 172.7 19 83. 0.0797 0.4284 1.0520 1.000 1.01 0 3 1.539 0 5 1.681 53.2 0 6 1.357 56.9 109.8 0 10 1.547 127.1 73.9 171.4 0 14 1.961 86.6 33.5 143.2 40.6 Atom Code x y z Height Symmetry transformation 7 1 1.2076 0.3706 0.7710 2.40 1.0000+X 0.0000+Y 0.0000+Z 8 2 -0.2649 0.1826 0.9018 2.40 -1.0000+X 0.0000+Y 0.0000+Z 10 3 -0.1021 0.5117 0.5906 3.86 0.0000+X 1.0000-Y -0.5000+Z 11 4 -0.0776 0.5126 1.2064 0.00 0.0000+X 1.0000-Y 0.5000+Z 13 5 1.1660 0.0592 0.9075 1.95 1.5000+X -0.5000+Y 0.0000+Z 15 6 -0.6171 0.6307 0.9044 1.95 -1.5000+X 0.5000+Y 0.0000+Z 16 7 1.1697 0.2220 0.9023 1.78 1.0000+X 0.0000+Y 0.0000+Z 18 8 -0.2766 0.3760 0.7742 2.96 -1.0000+X 0.0000+Y 0.0000+Z 0.0 seconds elapsed time +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + shelxs finished at 10:52:43 Total elapsed time: 0.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++