++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XS - CRYSTAL STRUCTURE SOLUTION - SHELXTL Ver. 6.12 W95/98/NT/2000/ME + + Copyright(c) 2001 Bruker AXS All Rights Reserved + + shelxs started at 23:31:01 on 12-Nov-2010 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL Pbca in Pbca CELL 0.71073 12.1766 9.5024 12.9638 90.000 90.000 90.000 ZERR 8.00 0.0004 0.0003 0.0003 0.000 0.000 0.000 LATT 1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O F UNIT 64 64 8 8 8 V = 1500.00 At vol = 17.0 F(000) = 640.0 mu = 0.11 mm-1 Max single Patterson vector = 20.6 cell wt = 1225.23 rho = 1.356 OMIT 4.00 180.00 ESEL 1.200 5.000 0.005 0.700 0 TREF HKLF 4 h k l F*F Sigma Why Rejected 1.00 0.00 3.00 0.24 0.02 Observed but should be systematically absent -2.00 0.00 -3.00 0.12 0.02 Observed but should be systematically absent 2.00 0.00 3.00 0.19 0.04 Observed but should be systematically absent 10311 Reflections read, of which 798 rejected Maximum h, k, l and 2-Theta = 15. 12. 16. 54.98 1704 Unique reflections, of which 1500 observed R(int) = 0.0313 R(sigma) = 0.0291 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) 5. 10. 30. 46. 62. 76. 50. 66. 89. 139. 183. 262. 357. N(measured) 5. 11. 31. 46. 63. 77. 51. 69. 93. 144. 188. 295. 448. N(theory) 5. 13. 32. 46. 63. 77. 51. 69. 93. 144. 188. 295. 451. 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 = 3691 / 8520 Observed E .GT. 1.200 1.300 1.400 1.500 1.600 1.700 1.800 1.900 2.000 2.100 Number 468 394 344 291 246 197 164 137 115 90 Centric Acentric 0kl h0l hk0 Rest Mean Abs(E*E-1) 0.968 0.736 1.284 1.031 0.935 0.967 0.1 seconds elapsed time SUMMARY OF PARAMETERS FOR Pbca in Pbca ESEL Emin 1.200 Emax 5.000 DelU 0.005 renorm 0.700 axis 0 OMIT s 4.00 2theta(lim) 180.0 INIT nn 9 nf 16 s+ 0.800 s- 0.200 wr 0.200 PHAN steps 10 cool 0.900 Boltz 0.400 ns 94 mtpr 40 mnqr 10 TREF np 256. nE 129 kapscal 0.900 ntan 2 wn -0.950 FMAP code 8 PLAN npeaks -18 del1 0.500 del2 1.500 MORE verbosity 1 TIME t 9999999. 94 Reflections and 640. unique TPR for phase annealing 129 Phases refined using 1711. unique TPR 194 Reflections and 3458. unique TPR for R(alpha) 0.0 seconds elapsed time 382 Unique negative quartets found, 382 used for phase refinement 0.0 seconds elapsed time Highest memory used to derive phase relations = 3144 / 9127 ONE-PHASE SEMINVARIANTS h k l E P+ Phi 0 8 4 2.714 0.23 12 0 0 2.470 1.00 0 8 0 2.066 0.00 2 2 8 2.575 0.54 10 4 0 2.253 0.85 2 0 6 2.042 0.59 0 6 8 1.919 0.22 4 0 6 1.891 0.53 6 6 6 2.405 0.46 2 6 4 1.559 0.46 6 2 10 1.648 0.46 Expected value of Sigma-1 = 0.939 Following phases held constant with unit weights for the initial 4 weighted tangent cycles (before phase annealing): h k l E Phase/Comment 12 0 0 2.470 0 sigma-1 = 1.000 1 1 1 2.067 random phase 2 1 7 2.852 random phase 0 8 0 2.066 180 sigma-1 = 0.000 10 4 0 2.253 0 sigma-1 = 0.853 2 4 1 2.149 random phase 1 2 2 1.662 random phase 5 2 1 1.962 random phase 5 4 3 2.043 random phase 5 0 6 1.891 random phase 1 2 7 1.764 random phase 1 7 2 1.862 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 92 Unique NQR employed in phase annealing 128 Parallel refinements, highest memory = 3538 / 37147 0.0 seconds elapsed time STRUCTURE SOLUTION for Pbca in Pbca Phase annealing cycle: 1 Beta = 0.10132 Ralpha 0.688 0.540 0.292 0.416 0.723 0.257 0.332 0.234 0.261 0.121 0.292 0.317 0.591 0.219 0.282 0.302 0.061 0.038 0.325 0.398 Nqual -0.468 0.129-0.596 0.171-0.032-0.168-0.263 0.359-0.296-0.137-0.486-0.411-0.270-0.304 0.185 0.138-0.604-0.473-0.346-0.214 Mabs 0.563 0.606 0.750 0.650 0.556 0.770 0.713 0.749 0.753 0.887 0.723 0.704 0.597 0.767 0.742 0.718 0.982 1.044 0.700 0.668 Phase annealing cycle: 2 Beta = 0.11258 Ralpha 0.438 0.378 0.178 0.373 0.456 0.196 0.243 0.262 0.217 0.057 0.227 0.159 0.439 0.154 0.292 0.269 0.061 0.039 0.215 0.347 Nqual -0.493-0.277-0.346-0.141-0.201-0.115-0.012 0.234-0.237-0.355-0.611-0.610-0.414-0.212-0.038 0.059-0.413-0.522-0.459-0.417 Mabs 0.641 0.677 0.850 0.681 0.643 0.827 0.782 0.737 0.822 1.040 0.785 0.816 0.661 0.849 0.748 0.734 1.033 1.087 0.774 0.698 Phase annealing cycle: 3 Beta = 0.12509 Ralpha 0.368 0.279 0.068 0.403 0.330 0.163 0.257 0.263 0.169 0.061 0.220 0.140 0.387 0.150 0.280 0.250 0.059 0.039 0.207 0.350 Nqual -0.163 0.075-0.201-0.296-0.164 0.034-0.280 0.245-0.137-0.420-0.427-0.524-0.417-0.201-0.035-0.193-0.400-0.522-0.508-0.387 Mabs 0.679 0.723 1.024 0.667 0.701 0.876 0.773 0.741 0.868 1.040 0.790 0.841 0.679 0.850 0.746 0.755 1.045 1.087 0.780 0.694 Phase annealing cycle: 4 Beta = 0.13898 Ralpha 0.201 0.270 0.069 0.382 0.254 0.136 0.212 0.228 0.143 0.061 0.227 0.142 0.310 0.150 0.249 0.255 0.061 0.039 0.225 0.350 Nqual -0.038-0.083-0.227-0.536-0.010-0.157-0.487 0.512-0.390-0.417-0.403-0.525-0.401-0.231 0.080-0.325-0.420-0.522-0.600-0.387 Mabs 0.791 0.735 1.046 0.674 0.758 0.900 0.790 0.760 0.877 1.046 0.782 0.847 0.721 0.847 0.766 0.770 1.040 1.087 0.772 0.694 Phase annealing cycle: 5 Beta = 0.15443 Ralpha 0.156 0.294 0.068 0.401 0.262 0.125 0.235 0.224 0.128 0.062 0.234 0.137 0.319 0.162 0.261 0.140 0.061 0.039 0.232 0.352 Nqual -0.274 0.009-0.232-0.634-0.197-0.094-0.380 0.432-0.243-0.407-0.585-0.505-0.291-0.105-0.169-0.556-0.424-0.522-0.668-0.355 Mabs 0.842 0.717 1.035 0.675 0.750 0.900 0.783 0.762 0.898 1.050 0.777 0.854 0.722 0.841 0.765 0.884 1.045 1.087 0.778 0.692 Phase annealing cycle: 6 Beta = 0.17159 Ralpha 0.158 0.281 0.061 0.233 0.126 0.136 0.193 0.249 0.129 0.069 0.222 0.131 0.296 0.155 0.282 0.067 0.061 0.039 0.253 0.332 Nqual -0.225 0.065-0.424-0.366-0.428-0.171-0.374 0.389-0.349-0.227-0.358-0.523-0.317-0.220-0.115-0.558-0.424-0.522-0.779-0.337 Mabs 0.851 0.732 1.045 0.763 0.907 0.904 0.804 0.747 0.900 1.046 0.797 0.858 0.734 0.853 0.756 1.028 1.045 1.087 0.761 0.711 Phase annealing cycle: 7 Beta = 0.19065 Ralpha 0.158 0.284 0.062 0.218 0.078 0.128 0.189 0.275 0.128 0.068 0.225 0.150 0.289 0.155 0.243 0.068 0.061 0.039 0.200 0.271 Nqual -0.193 0.119-0.414-0.367-0.170-0.188-0.257 0.248-0.243-0.232-0.317-0.527-0.388-0.220 0.147-0.245-0.424-0.522-0.625 0.024 Mabs 0.851 0.726 1.056 0.780 1.010 0.900 0.823 0.733 0.898 1.035 0.799 0.849 0.740 0.849 0.776 1.026 1.045 1.087 0.804 0.752 Phase annealing cycle: 8 Beta = 0.21183 Ralpha 0.151 0.276 0.068 0.193 0.061 0.135 0.179 0.233 0.128 0.061 0.200 0.129 0.295 0.157 0.247 0.061 0.061 0.039 0.172 0.168 Nqual -0.271-0.071-0.232-0.058-0.417-0.141-0.299 0.390-0.188-0.424-0.186-0.568-0.478-0.154 0.096-0.424-0.424-0.522-0.494 0.053 Mabs 0.849 0.727 1.035 0.814 1.046 0.903 0.825 0.761 0.900 1.045 0.823 0.873 0.732 0.846 0.780 1.045 1.045 1.087 0.844 0.842 Phase annealing cycle: 9 Beta = 0.23537 Ralpha 0.148 0.283 0.062 0.168 0.061 0.136 0.150 0.247 0.136 0.061 0.190 0.050 0.318 0.151 0.243 0.061 0.061 0.039 0.175 0.142 Nqual -0.302 0.011-0.414 0.140-0.420-0.171-0.198 0.097-0.171-0.424-0.120-0.549-0.398-0.296 0.035-0.424-0.424-0.522-0.112-0.108 Mabs 0.856 0.717 1.056 0.838 1.040 0.904 0.842 0.748 0.904 1.045 0.824 1.007 0.721 0.857 0.787 1.045 1.045 1.087 0.864 0.882 Phase annealing cycle: 10 Beta = 0.26152 Ralpha 0.159 0.267 0.068 0.169 0.061 0.129 0.159 0.256 0.129 0.061 0.189 0.039 0.323 0.151 0.246 0.061 0.061 0.039 0.141 0.142 Nqual -0.213-0.013-0.232 0.131-0.424-0.216-0.242 0.182-0.216-0.424-0.140-0.522-0.442-0.248-0.095-0.424-0.424-0.522-0.181-0.047 Mabs 0.848 0.738 1.035 0.838 1.045 0.901 0.836 0.747 0.901 1.045 0.825 1.087 0.716 0.848 0.789 1.045 1.045 1.087 0.888 0.895 Phase refinement cycle: 1 Ralpha 0.687 1.164 0.269 0.694 0.269 0.470 0.730 1.148 0.470 0.269 0.746 0.180 1.135 0.642 0.819 0.269 0.269 0.180 0.470 0.500 Nqual 0.086 0.053-0.418 0.055-0.418-0.032-0.267 0.190-0.032-0.418-0.239-0.485-0.323-0.017 0.058-0.418-0.418-0.485-0.032 0.125 Mabs 0.558 0.473 0.699 0.558 0.699 0.622 0.549 0.475 0.622 0.699 0.547 0.742 0.478 0.569 0.533 0.699 0.699 0.742 0.622 0.614 Try Ralpha Nqual Sigma-1 M(abs) CFOM Seminvariants 1420309. 0.277 0.115 -0.084 0.733 1.411 +---- +-++- + 810089. 0.581 0.205 0.914 0.589 1.915 ++-++ --++- + 1953293. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 1377857. 0.168 -0.632 0.835 0.846 0.269 ++-+- +--++ + 597829. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 891993. 0.185 0.037 0.930 0.847 1.159 ++--+ +---- - 265661. 0.344 -0.270 0.855 0.688 0.807 ++-+- +-+-+ - 1328305. 0.581 0.205 0.914 0.589 1.915 ++-++ --++- + 350069. 0.185 0.037 0.930 0.847 1.159 ++--+ +---- - 1750345. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 363117. 0.255 -0.199 0.938 0.774 0.819 ++-++ +---- - 1815585. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 689317. 0.541 -0.302 0.005 0.607 0.961 +---+ +---- - 1349433. 0.267 -0.009 -0.084 0.738 1.153 +---- +-++- + 455709. 0.273 0.180 0.914 0.782 1.550 ++--+ ----- - 181393. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 906965. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 340521. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1702605. 0.185 0.037 0.930 0.847 1.159 ++--+ +---- - 124417. 0.192 0.314 0.930 0.849 1.790 ++--+ +---- - 622085. 0.255 -0.199 0.938 0.774 0.819 ++-++ +---- - 1013273. 0.275 -0.228 0.855 0.745 0.795 ++-+- +-+-+ - 872061. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 166001. 0.423 -0.210 -0.083 0.656 0.971 +---+ -+-++ - 830005. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 2052873. 0.344 -0.270 0.855 0.688 0.807 ++-+- +-+-+ - 1875757. 0.185 0.037 0.930 0.847 1.159 ++--+ +---- - 990177. 0.344 -0.270 0.855 0.688 0.807 ++-+- +-+-+ - 756581. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1685753. 0.577 -0.126 0.914 0.595 1.255 ++-++ --++- + 40157. 0.344 -0.270 0.855 0.688 0.807 ++-+- +-+-+ - 200785. 0.501 -0.144 0.849 0.622 1.150 ++-++ -++++ + 984441. 0.185 0.037 0.930 0.847 1.159 ++--+ +---- - 1542353. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 469885. 0.731 -0.592 0.005 0.550 0.859 +---+ +---- - 384225. 0.344 -0.270 0.855 0.688 0.807 ++-+- +-+-+ - 1298669. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 170201. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 1890781. 0.344 -0.270 0.855 0.688 0.807 ++-+- +-+-+ - 1009445. 0.255 -0.199 0.938 0.774 0.819 ++-++ +---- - 2017025. 0.255 -0.199 0.938 0.774 0.819 ++-++ +---- - 1135797. 0.344 -0.270 0.855 0.688 0.807 ++-+- +-+-+ - 1217017. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 60721. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1757525. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 1642629. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 1065297. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 872901. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1452657. 0.344 -0.270 0.855 0.688 0.807 ++-+- +-+-+ - 1315557. 0.457 -0.235 -0.008 0.637 0.969 +--++ +--++ + 1387197. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 1433161. 0.344 -0.270 0.855 0.688 0.807 ++-+- +-+-+ - 783749. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 1316197. 0.344 -0.270 0.855 0.688 0.807 ++-+- +-+-+ - 600553. 0.302 -0.061 0.930 0.727 1.092 ++-++ +---+ - 1447645. 0.255 -0.199 0.938 0.774 0.819 ++-++ +---- - 664841. 0.344 -0.270 0.855 0.688 0.807 ++-+- +-+-+ - 1955161. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1227053. 0.344 -0.270 0.855 0.688 0.807 ++-+- +-+-+ - 139541. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 1495753. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1208605. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 1125493. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 1839241. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 137105. 0.344 -0.270 0.855 0.688 0.807 ++-+- +-+-+ - 360909. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 1466081. 0.344 -0.270 0.855 0.688 0.807 ++-+- +-+-+ - 1292065. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 726285. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 2063305. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 18497. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 211797. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 435857. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 168869. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 92485. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 1172861. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 22269. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 145257. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 701985. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 695237. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1931341. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 135421. 0.255 -0.199 0.938 0.774 0.819 ++-++ +---- - 173189. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 457529. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 1252601. 0.361 -0.182 0.839 0.675 0.951 ++-+- --+-+ - 1978385. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 2023909. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1415309. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1934321. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 1268161. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 360469. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 1089381. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 180861. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 617645. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 395677. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 150409. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1810109. 0.344 -0.270 0.855 0.688 0.807 ++-+- +-+-+ - 1837765. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 1826773. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 852005. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1383297. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 1358369. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 1046009. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1903933. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 800217. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 984401. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1068201. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 1013449. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 1445781. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1505009. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 661937. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 400249. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 1961865. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 1204109. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 1569809. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1428857. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 567205. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 674961. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 15553. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1048437. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 68865. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 742597. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 1097585. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 417449. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 349205. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 96809. 0.115 -0.558 0.012 0.920 0.268 +--++ +-+-+ - 1332017. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1746025. 0.040 -0.618 0.835 1.041 0.150* ++-+- +--++ + 1053081. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1161201. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1303673. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1308941. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1756049. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1691073. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1048129. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1205885. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 965157. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 887449. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1658289. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1902925. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 574509. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 21601. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 540025. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 510457. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1958345. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1200429. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1990589. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 429953. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 93949. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1498377. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1584861. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 506989. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1257865. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 630785. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 91813. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1315325. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 366469. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1917837. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1342457. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 34965. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 808673. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1832345. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 657081. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1698309. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 2088137. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 432481. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 2031797. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 681877. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 2061733. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 742181. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1920501. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 925357. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 831777. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 339449. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 832129. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1541629. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 269709. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 293445. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 2040541. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1077629. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1338385. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 730113. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 825321. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1276581. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 1605897. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + 2023973. 0.040 -0.618 0.835 1.041 0.150 ++-+- +--++ + CFOM Range Frequency 0.000 - 0.020 0 0.020 - 0.040 0 0.040 - 0.060 0 0.060 - 0.080 0 0.080 - 0.100 0 0.100 - 0.120 0 0.120 - 0.140 0 0.140 - 0.160 103 0.160 - 0.180 0 0.180 - 0.200 0 0.200 - 0.220 0 0.220 - 0.240 0 0.240 - 0.260 0 0.260 - 0.280 79 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 74 256. Phase sets refined - best is code 1746025. with CFOM = 0.1503 0.2 seconds elapsed time Tangent expanded to 468 out of 468 E greater than 1.200 Highest memory used = 2027 / 5254 0.0 seconds elapsed time FMAP and GRID set by program FMAP 8 2 13 GRID -2.500 24 -2 2.500 1 2 E-Fourier for Pbca in Pbca Maximum = 230.40, minimum = -61.40 highest memory used = 8735 / 9505 0.0 seconds elapsed time Peak list optimization RE = 0.191 for 11 surviving atoms and 468 E-values Highest memory used = 1550 / 4212 0.0 seconds elapsed time E-Fourier for Pbca in Pbca Maximum = 241.61, minimum = -68.10 highest memory used = 8735 / 9505 0.0 seconds elapsed time Peak list optimization RE = 0.187 for 11 surviving atoms and 468 E-values Highest memory used = 1550 / 4212 0.0 seconds elapsed time E-Fourier for Pbca in Pbca Maximum = 258.37, minimum = -55.12 highest memory used = 8735 / 9505 0.0 seconds elapsed time Molecule 1 scale 0.917 inches = 2.329 cm per Angstrom 16 18 9 8 3 1 15 7 17 12 10 14 6 5 6 14 10 17 15 3 13 4 2 11 12 17 Atom Peak x y z SOF Height Distances and Angles 1 258. 0.3416 0.2023 0.6351 1.000 0.00 0 7 1.339 0 15 1.870 53.7 2 215. 0.7297 0.1609 0.5927 1.000 1.17 0 4 1.185 3 206. 0.6753 -0.0635 0.5980 1.000 1.94 0 4 1.326 0 6 1.429 126.4 0 13 1.016 59.7 120.1 6 15 1.794 100.0 86.5 152.5 4 172. 0.7475 0.0390 0.5829 1.000 1.79 0 2 1.185 0 3 1.326 125.5 0 11 1.534 121.5 112.8 0 13 1.196 126.5 47.2 95.7 5 168. 0.5098 0.0779 0.6203 1.000 0.90 0 6 1.375 0 7 1.414 117.7 0 14 1.964 118.7 95.7 0 15 1.962 117.3 50.5 49.9 6 167. 0.5646 -0.0474 0.6327 1.000 1.36 0 3 1.429 0 5 1.375 120.9 0 10 1.416 118.3 119.9 5 14 1.906 92.3 101.2 66.7 7 150. 0.3970 0.0815 0.6460 1.000 0.45 0 1 1.339 0 5 1.414 119.0 0 9 1.380 118.8 122.1 0 15 1.524 81.3 83.7 102.2 8 149. 0.3980 -0.1614 0.6882 1.000 0.99 0 9 1.378 0 10 1.360 120.9 0 16 1.164 54.2 164.2 0 17 2.016 144.1 30.7 143.4 0 18 0.968 123.5 115.4 70.4 87.9 9 143. 0.3408 -0.0372 0.6774 1.000 0.52 0 7 1.380 0 8 1.378 118.6 0 16 1.174 165.4 53.6 10 137. 0.5064 -0.1694 0.6635 1.000 1.44 0 6 1.416 0 8 1.360 120.4 0 17 1.094 122.6 110.0 0 18 1.980 146.7 26.2 86.6 5 14 1.871 69.3 104.0 73.7 109.6 11 123. 0.8573 -0.0146 0.5403 1.000 2.61 0 4 1.534 0 12 1.830 85.9 0 13 2.036 35.8 79.0 12 40. 0.9193 0.0672 0.6541 1.000 1.19 0 11 1.830 8 17 1.669 114.9 13 39. 0.7386 -0.0496 0.6479 1.000 1.46 0 3 1.016 0 4 1.196 73.2 0 11 2.036 97.1 48.6 14 39. 0.4917 0.1535 0.4803 1.000 2.03 0 5 1.964 0 15 1.655 65.0 2 6 1.906 123.8 76.9 3 10 1.871 161.6 115.4 44.0 7 17 1.884 163.9 118.4 71.2 33.9 15 37. 0.3809 0.0780 0.5295 1.000 1.66 0 1 1.870 0 5 1.962 76.5 0 7 1.524 45.1 45.7 0 14 1.655 102.5 65.1 105.5 1 3 1.794 128.7 149.1 164.6 89.4 16 37. 0.3029 -0.1503 0.6850 1.000 0.84 0 8 1.164 0 9 1.174 72.2 0 18 1.239 47.4 118.6 17 34. 0.5257 -0.2743 0.6338 1.000 2.20 0 8 2.016 0 10 1.094 39.4 4 12 1.669 137.2 148.5 5 14 1.884 82.2 72.4 135.9 18 34. 0.3642 -0.2494 0.7084 1.000 1.09 0 8 0.968 0 10 1.980 38.4 0 16 1.239 62.2 99.4 Atom Code x y z Height Symmetry transformation 3 1 0.3247 0.0635 0.4020 2.96 1.0000-X 0.0000-Y 1.0000-Z 6 2 0.4354 0.0474 0.3673 3.55 1.0000-X 0.0000-Y 1.0000-Z 10 3 0.4936 0.1694 0.3365 3.47 1.0000-X 0.0000-Y 1.0000-Z 12 4 0.5807 -0.4328 0.6541 2.71 1.5000-X -0.5000+Y 0.0000+Z 14 5 0.5083 -0.1535 0.5197 2.88 1.0000-X 0.0000-Y 1.0000-Z 15 6 0.6191 -0.0780 0.4705 3.25 1.0000-X 0.0000-Y 1.0000-Z 17 7 0.4743 0.2743 0.3662 2.71 1.0000-X 0.0000-Y 1.0000-Z 17 8 0.9743 0.2257 0.6338 0.84 1.5000-X 0.5000+Y 0.0000+Z 0.0 seconds elapsed time +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + shelxs finished at 23:31:01 Total elapsed time: 0.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++