+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXS-97 - CRYSTAL STRUCTURE SOLUTION - WinGX VERSION + + Copyright(C) George M. Sheldrick 1986-97 Release 97-2 + + p21n started at 10:20:51 on 23 Mar 2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL p21n in P2(1)/n CELL 0.71073 6.9836 13.2116 12.0495 90.000 91.532 90.000 ZERR 1.00 0.0001 0.0002 0.0002 0.000 0.001 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O F SI UNIT 56 52 1 12 73 8 V = 1111.34 At vol = 7.4 F(000) = 1260.0 mu = 0.66 mm-1 Max single Patterson vector = 18.9 cell wt = 2542.71 rho = 3.799 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 0.00 0.23 0.05 Observed but should be systematically absent 1.00 0.00 0.00 0.16 0.03 Observed but should be systematically absent -1.00 0.00 2.00 0.35 0.08 Observed but should be systematically absent 1.00 0.00 4.00 0.93 0.18 Observed but should be systematically absent 1.00 0.00 4.00 0.64 0.12 Observed but should be systematically absent -1.00 0.00 -4.00 1.05 0.14 Observed but should be systematically absent -1.00 0.00 4.00 0.40 0.09 Observed but should be systematically absent 0.00 -3.00 0.00 0.68 0.15 Observed but should be systematically absent 0.00 -3.00 0.00 0.67 0.14 Observed but should be systematically absent 0.00 3.00 0.00 0.84 0.08 Observed but should be systematically absent 0.00 3.00 0.00 0.66 0.15 Observed but should be systematically absent 26099 Reflections read, of which 818 rejected Maximum h, k, l and 2-Theta = 9. 17. 15. 55.26 INCONSISTENT EQUIVALENTS h k l F*F Sigma(F*F) Esd of mean(F*F) 1 3 0 127.38 5.16 98.13 -1 2 1 199.62 2.64 136.88 1 4 1 253.51 13.32 103.24 2564 Unique reflections, of which 2446 observed R(int) = 0.0519 R(sigma) = 0.0307 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) 8. 11. 47. 75. 87. 104. 79. 115. 133. 206. 277. 428. 620. N(measured) 8. 13. 47. 75. 87. 104. 79. 115. 133. 208. 280. 448. 672. N(theory) 10. 15. 47. 75. 88. 105. 79. 115. 133. 208. 280. 448. 672. 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 = 5608 / 12820 Observed E .GT. 1.200 1.300 1.400 1.500 1.600 1.700 1.800 1.900 2.000 2.100 Number 725 619 532 457 383 320 273 226 174 134 Centric Acentric 0kl h0l hk0 Rest Mean Abs(E*E-1) 0.968 0.736 1.056 0.917 0.801 0.941 0.7 seconds CPU time SUMMARY OF PARAMETERS FOR p21n in P2(1)/n 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 0.400 ns 142 mtpr 40 mnqr 10 TREF np 256. nE 225 kapscal 0.900 ntan 2 wn -0.950 FMAP code 8 PLAN npeaks -24 del1 0.500 del2 1.500 MORE verbosity 1 TIME t 9999999. 142 Reflections and 1077. unique TPR for phase annealing 225 Phases refined using 3701. unique TPR 306 Reflections and 6535. unique TPR for R(alpha) 0.0 seconds CPU time 2801 Unique negative quartets found, 1472 used for phase refinement 0.0 seconds CPU time Highest memory used to derive phase relations = 4265 / 26028 ONE-PHASE SEMINVARIANTS h k l E P+ Phi 2 10 0 2.841 0.47 2 8 2 2.476 0.51 4 4 2 2.506 0.46 6 4 2 2.454 0.55 -2 2 6 2.166 0.51 -4 4 6 2.435 0.64 4 4 8 2.556 0.63 2 6 0 2.082 0.49 4 2 2 2.116 0.46 4 4 0 1.971 0.47 2 8 6 2.306 0.64 2 0 8 1.733 0.45 2 6 8 2.150 0.48 -6 2 6 2.025 0.46 -2 8 2 1.922 0.46 2 2 4 1.831 0 8 6 1.716 0.47 2 10 4 1.858 0.46 0 8 8 1.566 0.47 4 0 4 1.365 0.60 0 10 4 1.675 0.47 -4 6 4 1.552 0.48 -4 8 6 1.614 0.47 0 2 6 1.299 0.52 6 6 2 1.563 0.73 4 8 4 1.463 0.47 2 12 2 1.541 0.47 2 10 6 1.507 0.49 Expected value of Sigma-1 = 0.208 Following phases held constant with unit weights for the initial 4 weighted tangent cycles (before phase annealing): h k l E Phase/Comment 3 2 2 2.428 random phase -2 1 2 2.361 random phase -1 5 1 2.322 random phase -1 1 4 2.024 random phase 2 1 3 2.141 random phase 1 1 3 1.965 random phase 2 2 5 2.039 random phase 1 4 3 1.970 random phase -1 2 2 1.653 random phase 2 2 3 1.759 random phase -2 3 5 1.929 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 298 Unique NQR employed in phase annealing 128 Parallel refinements, highest memory = 7894 / 64491 0.0 seconds CPU time STRUCTURE SOLUTION for p21n in P2(1)/n Phase annealing cycle: 1 Beta = 0.13436 Ralpha 0.167 0.541 0.621 0.744 1.090 0.337 0.330 0.359 0.455 0.282 0.859 0.240 0.332 0.281 0.511 0.319 0.827 0.434 0.777 0.620 Nqual 0.610 0.435-0.047 0.256-0.074-0.050-0.431-0.245 0.035-0.154-0.129-0.464 0.080 0.313 0.147 0.087 0.122-0.389 0.135-0.111 Mabs 0.943 0.610 0.584 0.550 0.488 0.715 0.714 0.675 0.640 0.718 0.529 0.781 0.706 0.750 0.623 0.727 0.532 0.666 0.542 0.584 Phase annealing cycle: 2 Beta = 0.14929 Ralpha 0.138 0.342 0.557 0.418 0.681 0.293 0.228 0.321 0.361 0.206 0.554 0.181 0.269 0.216 0.500 0.251 0.612 0.310 0.561 0.438 Nqual 0.232 0.379-0.148 0.133 0.013-0.013-0.730-0.492-0.039-0.362-0.136-0.614 0.096 0.282 0.126-0.031 0.118-0.496-0.342-0.266 Mabs 1.070 0.702 0.605 0.671 0.566 0.752 0.796 0.711 0.689 0.799 0.607 0.899 0.746 0.853 0.628 0.805 0.589 0.734 0.610 0.654 Phase annealing cycle: 3 Beta = 0.16588 Ralpha 0.129 0.280 0.543 0.351 0.530 0.256 0.216 0.327 0.364 0.212 0.516 0.174 0.234 0.211 0.436 0.248 0.557 0.317 0.470 0.394 Nqual 0.067 0.474-0.170 0.129-0.277 0.019-0.729-0.586 0.035-0.403-0.161-0.767-0.051 0.339-0.290 0.031-0.049-0.632-0.600-0.454 Mabs 1.092 0.743 0.606 0.708 0.617 0.786 0.819 0.711 0.691 0.790 0.625 0.927 0.786 0.870 0.649 0.804 0.601 0.744 0.647 0.669 Phase annealing cycle: 4 Beta = 0.18431 Ralpha 0.137 0.254 0.550 0.264 0.518 0.251 0.204 0.311 0.326 0.211 0.464 0.079 0.239 0.210 0.413 0.254 0.601 0.309 0.362 0.376 Nqual 0.007 0.379-0.310 0.098-0.543 0.286-0.742-0.404 0.131-0.344-0.315-0.977-0.257 0.364-0.416 0.028-0.380-0.582-0.460-0.331 Mabs 1.081 0.751 0.608 0.762 0.625 0.791 0.828 0.713 0.710 0.792 0.641 1.147 0.794 0.866 0.653 0.797 0.589 0.748 0.696 0.680 Phase annealing cycle: 5 Beta = 0.20479 Ralpha 0.134 0.265 0.525 0.221 0.481 0.243 0.202 0.323 0.320 0.206 0.448 0.082 0.224 0.197 0.394 0.269 0.554 0.303 0.232 0.353 Nqual 0.081 0.336-0.295 0.025-0.608 0.227-0.663-0.477 0.299-0.368-0.225-0.986-0.190 0.425-0.372-0.066-0.520-0.519-0.529-0.476 Mabs 1.095 0.741 0.616 0.812 0.639 0.807 0.831 0.714 0.729 0.789 0.648 1.320 0.815 0.913 0.665 0.786 0.608 0.759 0.782 0.694 Phase annealing cycle: 6 Beta = 0.22754 Ralpha 0.136 0.249 0.491 0.185 0.450 0.233 0.195 0.310 0.272 0.203 0.422 0.082 0.201 0.187 0.367 0.253 0.613 0.258 0.223 0.356 Nqual 0.090 0.388-0.259 0.220-0.673 0.219-0.703-0.490 0.470-0.391-0.350-0.986-0.256 0.485-0.359-0.133-0.734-0.697-0.519-0.465 Mabs 1.089 0.757 0.623 0.852 0.651 0.819 0.835 0.720 0.778 0.791 0.667 1.320 0.825 0.951 0.673 0.790 0.589 0.809 0.787 0.691 Phase annealing cycle: 7 Beta = 0.25283 Ralpha 0.133 0.275 0.491 0.195 0.372 0.231 0.190 0.335 0.208 0.211 0.406 0.082 0.190 0.171 0.374 0.253 0.627 0.205 0.218 0.361 Nqual 0.107 0.241-0.443 0.168-0.503 0.258-0.673-0.507 0.633-0.372-0.397-0.986-0.187 0.380-0.393-0.081-0.715-0.584-0.463-0.438 Mabs 1.093 0.740 0.626 0.844 0.693 0.816 0.845 0.714 0.856 0.793 0.675 1.320 0.832 0.989 0.671 0.792 0.588 0.881 0.793 0.689 Phase annealing cycle: 8 Beta = 0.28092 Ralpha 0.133 0.262 0.478 0.192 0.341 0.229 0.179 0.355 0.180 0.212 0.381 0.082 0.192 0.148 0.338 0.254 0.609 0.206 0.227 0.326 Nqual 0.107 0.284-0.454 0.192-0.542 0.232-0.664-0.578 0.485-0.379-0.335-0.986-0.040 0.241-0.383-0.076-0.638-0.573-0.343-0.383 Mabs 1.093 0.749 0.633 0.847 0.711 0.809 0.843 0.708 0.921 0.787 0.686 1.320 0.857 1.052 0.694 0.790 0.594 0.882 0.804 0.713 Phase annealing cycle: 9 Beta = 0.31213 Ralpha 0.133 0.251 0.481 0.189 0.340 0.219 0.188 0.346 0.170 0.201 0.334 0.082 0.194 0.134 0.345 0.255 0.525 0.193 0.218 0.331 Nqual 0.107 0.421-0.466 0.240-0.420 0.426-0.686-0.653 0.540-0.404-0.438-0.986-0.139 0.042-0.245-0.211-0.574-0.545-0.229-0.393 Mabs 1.093 0.754 0.633 0.860 0.713 0.822 0.856 0.706 0.942 0.795 0.713 1.320 0.840 1.086 0.695 0.780 0.622 0.895 0.814 0.709 Phase annealing cycle: 10 Beta = 0.34681 Ralpha 0.134 0.244 0.465 0.196 0.322 0.231 0.190 0.353 0.165 0.209 0.316 0.082 0.191 0.137 0.346 0.248 0.408 0.205 0.192 0.358 Nqual 0.081 0.389-0.326 0.199-0.600 0.229-0.649-0.709 0.549-0.461-0.370-0.986-0.125 0.064-0.248-0.143-0.462-0.535-0.225-0.401 Mabs 1.095 0.755 0.636 0.850 0.735 0.816 0.855 0.701 0.948 0.788 0.720 1.320 0.852 1.091 0.694 0.798 0.678 0.885 0.851 0.696 Phase refinement cycle: 1 Ralpha 0.392 1.190 2.072 0.838 1.233 1.007 0.728 1.569 0.587 1.256 1.659 0.105 0.888 0.392 1.820 1.102 1.151 0.713 0.810 1.732 Nqual 0.116 0.391-0.283 0.098-0.520 0.313-0.621-0.607 0.561-0.351-0.237-0.983-0.234 0.116-0.226 0.050-0.285-0.526-0.197-0.381 Mabs 0.669 0.473 0.390 0.530 0.467 0.499 0.556 0.428 0.596 0.464 0.422 0.858 0.520 0.669 0.410 0.485 0.479 0.562 0.535 0.412 Try Ralpha Nqual Sigma-1 M(abs) CFOM Seminvariants 1420309. 0.167 0.040 0.513 1.006 1.146 ---++ ++--- ++--- --+-- ++--+ +++ 810089. 0.347 0.224 -0.270 0.727 1.726 -+--- --+-- -++++ ++++- -++++ --- 1953293. 0.636 -0.375 -0.012 0.579 0.966 --+-+ +--+- +---- +--+- --+-- --+ 1377857. 0.267 -0.384 0.016 0.783 0.587 -+-+- +---+ -++-+ ++++- --+++ -+- 597829. 0.370 -0.758 0.092 0.712 0.407 ---+- +---+ --++- ++-+- +++++ --- 891993. 0.314 0.066 -0.083 0.749 1.347 +---- -++-+ +-+-- ---+- ++--- --+ 265661. 0.201 -0.711 -0.158 0.898 0.258 +---- +++-- --+++ +---- -++-- +-- 1328305. 0.371 -0.861 -0.176 0.709 0.379 +---+ +++-+ -+++- --+-- +-++- --- 350069. 0.204 0.642 0.006 0.934 2.739 ++--- ++--- --+++ --+-+ -+--- +-- 1750345. 0.413 -0.638 0.506 0.664 0.510 -+--+ +++-- ----- --+-+ -+--+ ++- 363117. 0.472 -0.277 0.087 0.644 0.925 ++--- +++-- +-+++ +-+-+ +-+-- +++ 1815585. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 689317. 0.278 -0.556 -0.063 0.768 0.433 -+--- +---- -++++ +++-- +-+++ -+- 1349433. 0.167 0.040 0.513 1.006 1.146 ---++ ++--- ++--- --+-- ++--+ +++ 455709. 0.584 -0.474 0.099 0.594 0.811 +-+-- +++-+ ++--- +-+-+ +-+-- +-+ 181393. 0.354 0.024 -0.210 0.720 1.303 -++-- ++++- -+-++ +++++ -+++- +-- 906965. 0.347 -0.547 0.096 0.705 0.510 --+-- ++-++ +---+ ++-++ +++-- --+ 340521. 0.219 -0.528 0.021 0.881 0.396 +---+ +-+-+ +--++ -++-+ --++- --+ 1702605. 0.288 -0.358 -0.399 0.766 0.638 --+-+ ---++ -+++- ----+ -+-+- +-- 124417. 0.610 -0.356 0.155 0.587 0.963 ++--- ++-+- +-+-- ----- +--+- +++ 622085. 0.533 -0.539 0.009 0.608 0.702 +---- +++-+ -+--- +-+-+ ++-+- +-- 1013273. 0.379 -0.552 0.091 0.701 0.538 ++--- ++--- ++++- +-+-+ +-+-- +++ 872061. 0.154 -0.700 -0.061 1.039 0.216 ++++- --+++ ----+ --+-+ ----+ ++- 166001. 0.238 -0.655 0.229 0.825 0.325 +++++ +++++ -+++- ++-++ -++++ +-- 830005. 0.644 -0.186 -0.540 0.576 1.228 +-+-- --+-+ -++-+ +---+ ++--- ++- 2052873. 0.444 -0.736 -0.201 0.649 0.490 +++-+ -+-+- -++++ -++-- +-+-+ --- 1875757. 0.323 -0.534 -0.356 0.720 0.496 ++--+ ----- ----- -++++ -++-- -+- 990177. 0.326 -0.549 -0.356 0.718 0.487 ++--+ ----- ----- -++++ -++-- -+- 756581. 0.354 -0.204 -0.313 0.710 0.910 +---+ --+-- ----- +++++ ---+- ++- 1685753. 0.154 -0.700 -0.061 1.039 0.216 ++++- --+++ ----+ --+-+ ----+ ++- 40157. 0.280 -0.533 0.303 0.780 0.454 +++++ +++++ -++-- ++-++ -+--+ +-- 200785. 0.573 -0.186 0.544 0.596 1.158 ----- ++-++ +-+-- -+--+ +++-+ +-- 1642629. 0.966 -0.698 0.011 0.502 1.030 ----- --+-+ -++-+ +---+ --+++ -+- 80681. 0.629 -0.433 0.243 0.580 0.896 +-+-+ +++-+ +-+++ -+-+- +++-+ --- 1135797. 0.503 -0.249 0.336 0.618 0.995 +---+ +-+-+ +--++ -+-++ +-+++ --+ 1586817. 0.403 -0.535 -0.138 0.665 0.575 +---- -++-+ +++-+ +---- ---+- +++ 93977. 0.266 0.299 0.623 0.808 1.827 ----+ +++-- +---+ ++-++ +-+++ -++ 872901. 0.264 -0.834 -0.273 0.791 0.278 --+-- ++-++ ----+ -+++- -+++- +-- 1904881. 0.221 0.575 0.152 0.886 2.545 -+--- ++--- --+++ +---+ -+--- --- 1518025. 0.305 -0.820 -0.012 0.751 0.321 --+-- ++-++ ----- ++-++ ++++- --- 60721. 0.242 -0.456 -0.138 0.790 0.487 ----- --+-- -++-- -++++ ++--+ ++- 1041549. 0.255 -0.375 -0.454 0.791 0.585 --+-+ ---++ -++++ +---+ ++-+- --- 851005. 0.246 -0.418 -0.138 0.792 0.529 ----- --+-- -++-- -++++ ++--+ ++- 1921689. 0.269 0.097 0.671 0.817 1.366 ----+ +++-- +---+ -+--+ +-+++ -++ 1696517. 0.245 -0.776 0.035 0.820 0.275 +++++ +++++ -+++- ++-+- --+-+ ++- 1465441. 0.154 -0.700 -0.061 1.039 0.216 ++++- --+++ ----+ --+-+ ----+ ++- 351505. 0.145 -0.708 -0.016 1.012 0.203 ++++- --+++ ----+ --+-+ ----+ -+- 252273. 0.245 -0.776 0.035 0.820 0.275 +++++ +++++ -+++- ++-+- --+-+ ++- 807597. 0.167 0.040 0.513 1.006 1.146 ---++ ++--- ++--- --+-- ++--+ +++ 1773469. 0.167 0.040 0.513 1.006 1.146 ---++ ++--- ++--- --+-- ++--+ +++ 1001477. 0.207 -0.481 0.273 0.937 0.427 +++++ +++++ +++++ +++++ +++++ -++ 1121869. 0.332 -0.799 -0.465 0.747 0.354 +---- --+-+ -+--- --+++ ++--- +-- 410665. 0.167 0.040 0.513 1.006 1.146 ---++ ++--- ++--- --+-- ++--+ +++ 697705. 0.312 -0.370 -0.419 0.725 0.649 +---+ +-+-+ ---++ ++--- +++-- -+- 600553. 0.373 -0.563 0.181 0.690 0.523 --+-- ++-++ +---- ++-++ --+-- +-+ 971829. 0.135 -0.867 0.110 1.003 0.141 ++++- --+++ +---- +---- ++-++ +-+ 718581. 0.264 -0.397 -0.454 0.782 0.569 --+-+ ---++ -++++ +---+ ++-+- --- 1208605. 0.264 -0.397 -0.454 0.782 0.569 --+-+ ---++ -++++ +---+ ++-+- --- 1940833. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 177441. 0.154 -0.700 -0.061 1.039 0.216 ++++- --+++ ----+ --+-+ ----+ ++- 333761. 0.131 -0.880 0.074 1.002 0.136 ++++- --+++ +---- ++--- ++-++ +-+ 1482665. 0.154 -0.700 -0.061 1.039 0.216 ++++- --+++ ----+ --+-+ ----+ ++- 2052569. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 286329. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 608089. 0.343 -0.535 -0.278 0.717 0.516 -++-- -+--- -++++ ++--+ +-++- -+- 603709. 0.511 -0.318 0.012 0.621 0.910 +---- -++-+ ++--- +--++ -+-+- +++ 522161. 0.224 0.235 0.198 0.843 1.629 -+--+ ++--- ---++ +---+ -+--- --- 1073433. 0.402 -0.315 -0.030 0.682 0.805 --+-+ +--+- ++--+ --+++ ----- -+- 1534273. 0.136 -0.866 0.110 1.003 0.143 ++++- --+++ +---- +---- ++-++ +-+ 1927917. 0.536 -0.121 0.111 0.607 1.223 +-+-- --+-+ ++--- +-+-+ ++-++ +-+ 726285. 0.262 -0.857 -0.216 0.780 0.271 --+-- ++-++ ----- -+++- -+++- +-- 1058985. 0.270 -0.639 -0.077 0.781 0.367 --+-- ++-++ -+--- ++-++ ++++- --- 360909. 0.359 -0.729 -0.782 0.711 0.408 --+-+ ---++ -++++ +++-- ++-+- ++- 1466081. 0.302 -0.825 -0.397 0.752 0.317 +---- --+-+ -++-- --+-+ ++--- --- 1305297. 0.198 -0.522 0.228 0.889 0.382 ---+- --+-- +-+++ +-+++ -++++ --+ 1904137. 0.323 -0.352 -0.599 0.733 0.680 --+-+ ---++ -++++ --+-+ ++-+- ++- 772409. 0.302 -0.825 -0.397 0.752 0.317 +---- --+-+ -++-- --+-+ ++--- --- 18497. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 1412773. 0.154 -0.700 -0.061 1.039 0.216 ++++- --+++ ----+ --+-+ ----+ ++- 1923045. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 1423341. 0.145 -0.708 -0.016 1.012 0.203 ++++- --+++ ----+ --+-+ ----+ -+- 1931341. 0.309 -0.876 -0.238 0.746 0.314 -+--+ --+-- ----- --+++ -+--- -+- 1092493. 0.167 0.040 0.513 1.006 1.146 ---++ ++--- ++--- --+-- ++--+ +++ 594437. 0.466 -0.296 0.178 0.644 0.893 ++--+ +--+- +---- --+-+ -+--- --- 1225725. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 617645. 0.581 -0.535 -0.384 0.594 0.753 +---+ --+-+ +--++ -+-+- ++++- --- 952465. 0.363 -0.461 -0.570 0.708 0.602 --+-+ ---++ --+++ +++-+ ++-+- ++- 1140665. 0.249 -0.852 0.035 0.816 0.259 +++++ +++++ -+++- ++-+- --+-+ ++- 1934321. 0.206 0.637 0.006 0.920 2.726 ++--- ++--- --+++ --+-+ -+--- +-- 180861. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 1233725. 0.335 -0.788 -0.465 0.742 0.361 +---- --+-+ -+--- --+++ ++--- +-- 904305. 0.287 -0.407 -0.397 0.760 0.582 --+-+ ---++ -+++- +---+ ++-+- --- 1385877. 0.179 -0.511 0.570 0.912 0.371 -+-++ ++--- ++--- --+-- -+--+ +++ 742953. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 785089. 0.262 -0.857 -0.216 0.780 0.271 --+-- ++-++ ----- -+++- -+++- +-- 246745. 0.198 -0.522 0.228 0.889 0.382 ---+- --+-- +-+++ +-+++ -++++ --+ 1252721. 0.283 -0.365 -0.782 0.770 0.625 --+-+ ---++ -++++ +++-- ++-+- ++- 1337385. 0.268 -0.786 -0.021 0.778 0.295 --+-- ++-++ ----- ++-++ ++++- --+ 568129. 0.295 -0.820 -0.397 0.756 0.312 +---- --+-+ -++-- --+-+ ++--- --- 712929. 0.154 -0.700 -0.061 1.039 0.216 ++++- --+++ ----+ --+-+ ----+ ++- 1212533. 0.289 -0.477 0.229 0.769 0.513 +++++ +++++ -+++- ++-++ -++++ +-- 1505009. 0.242 -0.456 -0.138 0.790 0.487 ----- --+-- -++-- -++++ ++--+ ++- 305993. 0.214 0.494 0.152 0.890 2.298 -+--- ++--- --+++ +---+ -+--- --- 882437. 0.145 -0.708 -0.016 1.012 0.203 ++++- --+++ ----+ --+-+ ----+ -+- 916945. 0.278 -0.757 0.210 0.765 0.316 +--+- +---- +++++ +--+- -++-+ --+ 1854209. 0.162 -0.047 0.556 1.002 0.978 ---++ ++--- ++--- --+-- -+--+ +++ 618097. 0.271 -0.563 0.211 0.749 0.421 -+--- +-+-- -++++ ++--+ ---++ -++ 400249. 0.145 -0.708 -0.016 1.012 0.203 ++++- --+++ ----+ --+-+ ----+ -+- 1467493. 0.154 -0.700 -0.061 1.039 0.216 ++++- --+++ ----+ --+-+ ----+ ++- 480629. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 1027993. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 65721. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 1944125. 0.197 -0.050 -0.145 0.932 1.007 ++--- +++-- --+++ +---- -++-- +-- 1031201. 0.154 -0.700 -0.061 1.039 0.216 ++++- --+++ ----+ --+-+ ----+ ++- 1826241. 0.136 -0.866 0.110 1.003 0.143 ++++- --+++ +---- +---- ++-++ +-+ 2072985. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 1615365. 0.423 -0.579 -0.137 0.667 0.560 -++-- ++-+- -+-+- -+-+- -+-+- --- 69841. 0.248 -0.426 -0.138 0.788 0.523 ----- --+-- -++-- -++++ ++--+ ++- 1063857. 0.197 -0.587 0.228 0.882 0.329 ---+- --+-- +-+++ +-+++ -++++ --+ 1597213. 0.201 -0.711 -0.158 0.898 0.258 +---- +++-- --+++ +---- -++-- +-- 629177. 0.245 -0.776 0.035 0.820 0.275 +++++ +++++ -+++- ++-+- --+-+ ++- 1353721. 0.249 -0.852 0.035 0.816 0.259 +++++ +++++ -+++- ++-+- --+-+ ++- 797529. 0.332 -0.799 -0.465 0.747 0.354 +---- --+-+ -+--- --+++ ++--- +-- 873013. 0.145 -0.626 -0.016 1.019 0.250 ++++- --+++ ----+ --+-+ ----+ -+- 74721. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 674961. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 973853. 0.154 -0.700 -0.061 1.039 0.216 ++++- --+++ ----+ --+-+ ----+ ++- 1047881. 0.106 -0.996 0.273 1.346 0.106* +++++ +++++ +++++ -++++ +++++ -++ 198845. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 1071013. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 421569. 0.131 -0.880 0.074 1.002 0.136 ++++- --+++ +---- ++--- ++-++ +-+ 1879221. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 894745. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 887449. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 1089561. 0.135 -0.867 0.110 1.003 0.141 ++++- --+++ +---- +---- ++-++ +-+ 760021. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 52613. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 100717. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 1331585. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 1070329. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 343273. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 193217. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 1096165. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 1018649. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 831777. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 898941. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 2063493. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 945365. 0.136 -0.866 0.110 1.003 0.143 ++++- --+++ +---- +---- ++-++ +-+ 343989. 0.106 -0.996 0.273 1.346 0.106 +++++ +++++ +++++ -++++ +++++ -++ 1190185. 0.131 -0.880 0.074 1.002 0.136 ++++- --+++ +---- ++--- ++-++ +-+ 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 34 0.120 - 0.140 3 0.140 - 0.160 5 0.160 - 0.180 0 0.180 - 0.200 0 0.200 - 0.220 32 0.220 - 0.240 0 0.240 - 0.260 8 0.260 - 0.280 15 0.280 - 0.300 3 0.300 - 0.320 7 0.320 - 0.340 9 0.340 - 0.360 5 0.360 - 0.380 4 0.380 - 0.400 8 0.400 - 0.420 3 0.420 - 0.440 4 0.440 - 0.460 3 0.460 - 0.480 2 0.480 - 0.500 7 0.500 - 0.520 5 0.520 - 0.540 6 0.540 - 0.560 5 0.560 - 0.580 4 0.580 - 0.600 5 0.600 - 9.999 79 256. Phase sets refined - best is code 1047881. with CFOM = 0.1062 0.7 seconds CPU time Tangent expanded to 725 out of 725 E greater than 1.200 Highest memory used = 3036 / 3697 0.0 seconds CPU time FMAP and GRID set by program FMAP 8 1 10 GRID -3.571 -2 -2 3.571 2 2 E-Fourier for p21n in P2(1)/n Maximum = 546.30, minimum = -93.71 highest memory used = 8764 / 8422 0.0 seconds CPU time Heavy-atom assignments: x y z s.o.f. Height SI1 0.0000 0.5000 0.5000 0.5000 546.3 Peak list optimization RE = 0.269 for 14 surviving atoms and 725 E-values Highest memory used = 1579 / 6525 0.0 seconds CPU time E-Fourier for p21n in P2(1)/n Maximum = 506.17, minimum = -97.43 highest memory used = 8772 / 8422 0.0 seconds CPU time Peak list optimization RE = 0.265 for 14 surviving atoms and 725 E-values Highest memory used = 1587 / 6525 0.0 seconds CPU time E-Fourier for p21n in P2(1)/n Maximum = 461.23, minimum = -78.10 highest memory used = 8772 / 8422 0.0 seconds CPU time Molecule 1 scale 0.790 inches = 2.006 cm per Angstrom 21 13 9 12 24 22 4 8 7 19 20 SI1 10 6 11 5 16 14 23 22 17 3 18 15 5 2 1 19 20 SI1 20 19 2 1 15 18 3 17 22 14 21 Atom Peak x y z SOF Height Distances and Angles SI1 0. 0.0000 0.5000 0.5000 0.500 3.09 0 1 1.712 0 2 1.706 90.4 0 3 1.694 89.9 90.8 0 14 2.516 80.0 52.1 40.5 0 15 2.819 5.5 85.5 92.5 78.9 0 17 2.637 80.1 105.4 17.7 53.4 83.8 0 18 1.975 64.3 71.6 33.0 23.2 65.0 37.8 0 20 2.288 26.1 64.8 85.6 61.0 22.0 83.2 53.4 0 22 2.429 20.7 110.9 92.5 95.3 25.4 78.1 75.4 46.8 2 1 1.712 180.0 89.6 90.1 100.0 174.5 99.9 115.7 153.9 159.3 3 2 1.706 89.6 180.0 89.2 127.9 94.5 74.6 108.4 115.2 69.1 90.4 4 3 1.694 90.1 89.2 180.0 139.5 87.5 162.3 147.0 94.4 87.5 89.9 90.8 6 14 2.516 100.0 127.9 139.5 180.0 101.1 126.6 156.8 119.0 84.7 80.0 52.1 7 15 2.819 174.5 94.5 87.5 101.1 180.0 96.2 115.0 158.0 154.6 5.5 85.5 8 17 2.637 99.9 74.6 162.3 126.6 96.2 180.0 142.2 96.8 101.9 80.1 105.4 9 18 1.975 115.7 108.4 147.0 156.8 115.0 142.2 180.0 126.6 104.6 64.3 71.6 10 19 3.236 144.8 72.1 119.7 109.4 140.1 133.3 132.2 130.1 147.8 35.2 107.9 11 19 3.236 35.2 107.9 60.3 70.6 39.9 46.7 47.8 49.9 32.2 144.8 72.1 12 20 2.288 153.9 115.2 94.4 119.0 158.0 96.8 126.6 180.0 133.2 26.1 64.8 15 22 2.429 159.3 69.1 87.5 84.7 154.6 101.9 104.6 133.2 180.0 20.7 110.9 1 315. 0.1042 0.3829 0.4942 1.000 2.56 0 SI1 1.712 0 15 1.126 166.2 0 18 1.974 64.3 116.4 0 20 1.062 108.9 60.5 72.3 0 22 1.025 123.1 68.5 126.9 128.0 2 289. 0.0409 0.5183 0.3625 1.000 1.94 0 SI1 1.706 0 14 1.992 85.4 3 282. 0.2153 0.5516 0.5351 1.000 3.55 0 SI1 1.694 0 14 1.649 97.6 0 17 1.145 135.7 110.7 0 18 1.076 88.0 38.4 93.6 4 201. 0.5137 0.6908 0.2465 1.000 1.47 0 6 1.542 0 7 1.527 111.4 0 8 1.495 108.1 110.2 0 9 1.549 108.9 107.0 111.3 5 194. 0.5502 0.6259 0.6300 1.000 4.59 0 16 2.018 0 17 1.945 99.9 0 23 1.253 71.5 28.7 13 20 2.030 71.2 135.0 118.4 6 147. 0.3957 0.6774 0.3519 1.000 2.38 0 4 1.542 0 10 1.490 114.5 0 14 1.983 124.8 106.8 0 19 1.978 75.3 148.1 88.7 7 146. 0.3956 0.6643 0.1420 1.000 0.47 0 4 1.527 0 11 1.456 114.6 8 144. 0.6857 0.6237 0.2566 1.000 1.25 0 4 1.495 0 12 1.552 113.8 0 19 1.747 84.0 147.1 9 142. 0.5722 0.8034 0.2363 1.000 1.80 0 4 1.549 0 13 1.475 112.3 10 123. 0.2306 0.7482 0.3601 1.000 2.76 0 6 1.490 11 121. 0.3394 0.5584 0.1337 1.000 0.00 0 7 1.456 12 117. 0.8187 0.6294 0.1556 1.000 0.35 0 8 1.552 13 109. 0.6854 0.8390 0.3337 1.000 2.77 0 9 1.475 0 21 1.891 127.6 0 24 1.921 113.2 92.6 14 53. 0.3107 0.5454 0.4116 1.000 2.41 0 SI1 2.516 0 2 1.992 42.5 0 3 1.649 41.9 82.8 0 6 1.983 129.3 109.9 114.6 0 18 1.046 48.0 84.8 39.7 150.3 15 49. 0.1610 0.3067 0.4689 1.000 2.03 0 SI1 2.819 0 1 1.126 8.3 0 20 1.104 50.8 56.9 0 22 1.213 59.1 51.8 108.0 16 49. 0.7043 0.5387 0.7368 1.000 5.16 0 5 2.018 0 23 2.009 36.2 17 44. 0.3294 0.5386 0.6036 1.000 4.08 0 SI1 2.637 0 3 1.145 26.7 0 5 1.945 150.4 124.2 0 18 1.620 48.3 41.5 119.6 0 23 1.039 171.2 155.4 35.4 125.7 18 43. 0.2795 0.4989 0.4790 1.000 2.83 0 SI1 1.975 0 1 1.974 51.4 0 3 1.076 59.0 100.0 0 14 1.046 108.8 132.2 101.9 0 17 1.620 93.9 106.5 44.9 119.0 0 20 1.936 71.6 31.5 128.7 106.4 134.5 19 42. 0.6610 0.6424 0.3990 1.000 2.59 0 6 1.978 0 8 1.747 82.4 16 22 1.753 155.3 101.3 20 40. 0.1729 0.3753 0.4171 1.000 1.83 0 SI1 2.288 0 1 1.062 45.1 0 15 1.104 107.2 62.6 0 18 1.936 55.0 76.2 120.6 0 22 1.876 70.6 25.5 37.9 90.9 5 5 2.030 130.2 134.6 103.8 75.8 121.9 21 40. 0.9302 0.7940 0.3829 1.000 2.97 0 13 1.891 16 22 1.824 106.8 22 39. 0.1019 0.3320 0.5585 1.000 2.93 0 SI1 2.429 0 1 1.025 36.2 0 15 1.213 95.6 59.7 0 20 1.876 62.7 26.5 34.0 11 19 1.753 100.1 93.5 88.4 86.3 14 21 1.824 155.2 153.4 98.1 131.9 100.8 23 38. 0.4655 0.5430 0.6402 1.000 4.38 0 5 1.253 0 16 2.009 72.3 0 17 1.039 115.8 168.7 24 38. 0.5718 0.8055 0.4724 1.000 3.89 0 13 1.921 Atom Code x y z Height Symmetry transformation SI1 1 1.0000 0.5000 0.5000 2.84 1.0000+X 0.0000+Y 0.0000+Z 1 2 -0.1042 0.6171 0.5058 3.63 0.0000-X 1.0000-Y 1.0000-Z 2 3 -0.0409 0.4817 0.6375 4.25 0.0000-X 1.0000-Y 1.0000-Z 3 4 -0.2153 0.4484 0.4649 2.64 0.0000-X 1.0000-Y 1.0000-Z 5 5 0.4498 0.3741 0.3700 1.34 1.0000-X 1.0000-Y 1.0000-Z 14 6 -0.3107 0.4546 0.5884 3.78 0.0000-X 1.0000-Y 1.0000-Z 15 7 -0.1610 0.6933 0.5311 4.16 0.0000-X 1.0000-Y 1.0000-Z 17 8 -0.3294 0.4614 0.3964 2.11 0.0000-X 1.0000-Y 1.0000-Z 18 9 -0.2795 0.5011 0.5210 3.35 0.0000-X 1.0000-Y 1.0000-Z 19 10 -0.3390 0.6424 0.3990 2.84 -1.0000+X 0.0000+Y 0.0000+Z 19 11 0.3390 0.3576 0.6010 3.35 1.0000-X 1.0000-Y 1.0000-Z 20 12 -0.1729 0.6247 0.5829 4.35 0.0000-X 1.0000-Y 1.0000-Z 20 13 0.8271 0.6247 0.5829 4.10 1.0000-X 1.0000-Y 1.0000-Z 21 14 0.0698 0.2060 0.6171 2.97 1.0000-X 1.0000-Y 1.0000-Z 22 15 -0.1019 0.6680 0.4415 3.25 0.0000-X 1.0000-Y 1.0000-Z 22 16 0.8981 0.6680 0.4415 3.00 1.0000-X 1.0000-Y 1.0000-Z 0.0 seconds CPU time +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + p21n finished at 10:20:52 Total CPU time: 1.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++