+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXS-97 - CRYSTAL STRUCTURE SOLUTION - WinGX VERSION + + Copyright(C) George M. Sheldrick 1986-97 Release 97-2 + + 2007may0002 started at 17:19:18 on 08 Jun 2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007may0002 in I4(1)/a CELL 0.71073 22.5496 22.5496 6.3581 90.000 90.000 90.000 ZERR 14.00 0.0004 0.0004 0.0002 0.000 0.000 0.000 LATT 2 SYMM 0.5-X, -Y, 0.5+Z SYMM 0.75-Y, 0.25+X, 0.25+Z SYMM 0.75+Y, 0.75-X, 0.75+Z SFAC C H O UNIT 126 140 42 V = 3233.00 At vol = 19.2 F(000) = 1232.0 mu = 0.09 mm-1 Max single Patterson vector = 8.7 cell wt = 2326.38 rho = 1.195 OMIT 4.00 180.00 ESEL 1.200 5.000 0.005 0.700 0 TREF HKLF 4 13907 Reflections read, of which 725 rejected Maximum h, k, l and 2-Theta = 29. 29. 8. 54.97 1859 Unique reflections, of which 1549 observed R(int) = 0.0655 R(sigma) = 0.0515 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) 6. 12. 36. 49. 65. 77. 64. 70. 107. 139. 210. 247. 338. N(measured) 6. 12. 36. 49. 65. 79. 64. 72. 109. 143. 217. 298. 494. N(theory) 8. 12. 36. 49. 65. 79. 64. 72. 109. 143. 217. 298. 494. 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 = 11223 / 9295 Observed E .GT. 1.200 1.300 1.400 1.500 1.600 1.700 1.800 1.900 2.000 2.100 Number 474 401 351 300 257 214 179 150 127 96 Centric Acentric 0kl h0l hk0 Rest Mean Abs(E*E-1) 0.968 0.736 0.800 0.800 1.031 0.955 0.4 seconds CPU time SUMMARY OF PARAMETERS FOR 2007may0002 in I4(1)/a 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 97 mtpr 40 mnqr 10 TREF np 256. nE 134 kapscal 0.900 ntan 2 wn -0.950 FMAP code 8 PLAN npeaks -19 del1 0.500 del2 1.500 MORE verbosity 1 TIME t 9999999. 97 Reflections and 743. unique TPR for phase annealing 134 Phases refined using 1876. unique TPR 194 Reflections and 3758. unique TPR for R(alpha) 0.0 seconds CPU time 386 Unique negative quartets found, 386 used for phase refinement 0.0 seconds CPU time Highest memory used to derive phase relations = 3257 / 9769 ONE-PHASE SEMINVARIANTS h k l E P+ Phi 4 4 0 2.529 0.23 -4 6 0 2.466 0.39 -4 14 4 3.492 0.73 -2 6 0 2.446 0.19 -8 10 4 2.462 0.54 0 16 4 2.673 0.47 -4 18 2 2.496 0.46 0 8 4 2.446 0.58 -4 16 2 2.636 -4 8 2 2.164 -12 16 2 2.846 0 10 0 2.020 0.38 6 14 0 2.036 0.25 10 18 0 2.377 0.00 8 14 4 2.332 0.44 -6 12 0 1.999 0.48 -8 12 4 2.336 0.55 2 20 2 1.988 0.45 -6 8 2 1.822 0.52 -8 12 2 1.685 4 4 4 1.787 0.49 -8 14 2 1.792 0.50 2 8 4 1.985 0.48 2 14 0 1.655 0.77 -6 14 4 1.907 0.55 12 12 4 1.745 0.49 8 14 2 1.550 0.46 -6 12 4 1.680 0.46 0 4 2 1.491 2 2 2 1.402 -8 12 0 1.478 0.86 -2 16 4 1.632 0.47 4 6 2 1.340 0.47 -8 14 0 1.529 0.45 -6 10 2 1.506 14 14 0 1.458 0.45 -6 10 0 1.281 0.43 12 16 0 1.516 0.39 8 16 0 1.226 0.36 Expected value of Sigma-1 = 0.583 Following phases held constant with unit weights for the initial 4 weighted tangent cycles (before phase annealing): h k l E Phase/Comment 4 4 0 2.529 random phase -4 6 0 2.466 random phase -2 5 1 2.723 random phase -2 6 0 2.446 180 sigma-1 = 0.187 2 5 5 2.266 random phase 5 7 2 2.172 random phase 10 18 0 2.377 180 sigma-1 = 0.005 4 5 5 2.223 random phase -1 4 1 1.837 random phase 5 9 2 1.892 random phase 5 18 3 2.036 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 94 Unique NQR employed in phase annealing 128 Parallel refinements, highest memory = 3684 / 39054 0.0 seconds CPU time STRUCTURE SOLUTION for 2007may0002 in I4(1)/a Phase annealing cycle: 1 Beta = 0.09336 Ralpha 1.317 0.722 0.580 0.517 0.778 0.619 0.714 0.483 0.873 1.459 0.610 0.650 0.635 0.979 0.407 0.876 1.716 0.769 0.594 0.728 Nqual -0.269 0.266 0.351 0.046-0.465 0.232-0.234-0.274 0.325-0.631-0.228-0.036 0.327-0.563-0.298 0.640-0.091-0.420-0.147-0.347 Mabs 0.458 0.554 0.590 0.611 0.538 0.576 0.556 0.621 0.521 0.442 0.581 0.566 0.577 0.503 0.651 0.519 0.416 0.543 0.585 0.551 Phase annealing cycle: 2 Beta = 0.10374 Ralpha 1.262 0.421 0.447 0.410 0.773 0.527 0.601 0.437 0.599 1.237 0.614 0.645 0.373 0.975 0.343 0.766 0.990 0.736 0.523 0.682 Nqual -0.504 0.425-0.221 0.077-0.643-0.075-0.273-0.327 0.141-0.624-0.353-0.173-0.033-0.605-0.309 0.147-0.348-0.547 0.070-0.737 Mabs 0.463 0.649 0.632 0.659 0.539 0.608 0.587 0.639 0.584 0.465 0.579 0.569 0.687 0.504 0.691 0.543 0.501 0.551 0.613 0.564 Phase annealing cycle: 3 Beta = 0.11527 Ralpha 0.990 0.430 0.419 0.391 0.714 0.497 0.666 0.472 0.579 1.122 0.613 0.683 0.322 0.883 0.327 0.783 1.041 0.717 0.463 0.690 Nqual -0.555 0.405-0.198-0.188-0.306-0.182-0.526-0.361-0.040-0.757-0.259-0.152 0.182-0.590-0.459 0.123-0.646-0.520 0.603-0.826 Mabs 0.502 0.648 0.644 0.671 0.556 0.615 0.568 0.624 0.585 0.480 0.582 0.559 0.700 0.522 0.699 0.538 0.493 0.554 0.636 0.558 Phase annealing cycle: 4 Beta = 0.12807 Ralpha 1.027 0.377 0.369 0.331 0.711 0.461 0.594 0.394 0.518 1.039 0.586 0.626 0.296 0.932 0.279 0.783 0.988 0.710 0.496 0.673 Nqual -0.579 0.356-0.281 0.165-0.264-0.299-0.525 0.120 0.062-0.845 0.121 0.026 0.037-0.549-0.282-0.030-0.527-0.610 0.491-0.800 Mabs 0.496 0.664 0.666 0.702 0.554 0.627 0.587 0.656 0.607 0.495 0.590 0.573 0.714 0.512 0.726 0.539 0.502 0.555 0.625 0.565 Phase annealing cycle: 5 Beta = 0.14230 Ralpha 0.935 0.329 0.418 0.355 0.702 0.526 0.626 0.386 0.545 0.801 0.550 0.549 0.292 0.823 0.264 0.846 1.153 0.718 0.482 0.656 Nqual -0.666 0.460-0.246 0.202-0.334-0.316-0.518 0.210-0.123-0.796 0.066 0.209-0.241-0.562-0.240-0.034-0.654-0.541 0.404-0.806 Mabs 0.512 0.695 0.645 0.693 0.557 0.606 0.580 0.660 0.596 0.538 0.602 0.594 0.718 0.533 0.741 0.526 0.475 0.557 0.626 0.568 Phase annealing cycle: 6 Beta = 0.15811 Ralpha 0.772 0.321 0.416 0.350 0.636 0.477 0.589 0.369 0.531 0.534 0.469 0.562 0.319 0.788 0.264 0.730 1.038 0.585 0.425 0.656 Nqual -0.614 0.503-0.194 0.235-0.129-0.133-0.319 0.268-0.067-0.776-0.002-0.052-0.367-0.666-0.238-0.063-0.707-0.543 0.586-0.806 Mabs 0.544 0.700 0.643 0.697 0.575 0.621 0.590 0.674 0.600 0.605 0.628 0.590 0.707 0.539 0.741 0.549 0.493 0.588 0.651 0.568 Phase annealing cycle: 7 Beta = 0.17568 Ralpha 0.762 0.304 0.388 0.348 0.608 0.455 0.593 0.371 0.509 0.414 0.484 0.579 0.335 0.725 0.269 0.752 0.979 0.569 0.398 0.657 Nqual -0.572 0.476-0.201 0.218-0.007-0.267-0.372 0.293-0.128-0.681 0.042 0.060-0.010-0.656-0.213-0.246-0.720-0.584 0.507-0.802 Mabs 0.547 0.707 0.657 0.701 0.580 0.627 0.587 0.674 0.608 0.654 0.623 0.587 0.704 0.554 0.737 0.544 0.503 0.591 0.670 0.567 Phase annealing cycle: 8 Beta = 0.19520 Ralpha 0.704 0.300 0.385 0.350 0.597 0.457 0.588 0.374 0.558 0.289 0.499 0.551 0.305 0.699 0.280 0.816 0.960 0.516 0.328 0.639 Nqual -0.630 0.414-0.111 0.054-0.150-0.272-0.553 0.166-0.241-0.556 0.148 0.120-0.013-0.733-0.320-0.212-0.680-0.600 0.679-0.793 Mabs 0.560 0.711 0.659 0.697 0.584 0.627 0.589 0.671 0.595 0.704 0.617 0.595 0.717 0.562 0.736 0.530 0.506 0.610 0.715 0.573 Phase annealing cycle: 9 Beta = 0.21689 Ralpha 0.696 0.281 0.377 0.350 0.610 0.484 0.566 0.369 0.529 0.289 0.488 0.542 0.304 0.694 0.274 0.711 0.960 0.477 0.165 0.639 Nqual -0.649 0.639-0.291 0.054-0.284-0.290-0.430 0.372-0.211-0.556 0.144 0.065-0.207-0.666-0.202 0.268-0.681-0.590 0.900-0.793 Mabs 0.563 0.728 0.661 0.697 0.582 0.620 0.595 0.671 0.604 0.704 0.622 0.596 0.710 0.563 0.733 0.555 0.506 0.621 0.864 0.573 Phase annealing cycle: 10 Beta = 0.24099 Ralpha 0.662 0.274 0.395 0.361 0.632 0.456 0.537 0.376 0.534 0.297 0.490 0.554 0.289 0.689 0.245 0.716 0.955 0.462 0.113 0.639 Nqual -0.697 0.652-0.407-0.011-0.388-0.256-0.424 0.241-0.208-0.565-0.126 0.067-0.190-0.676-0.015 0.035-0.724-0.590 0.972-0.793 Mabs 0.571 0.732 0.655 0.693 0.576 0.628 0.604 0.670 0.603 0.705 0.621 0.594 0.717 0.565 0.753 0.552 0.507 0.625 1.004 0.573 Phase refinement cycle: 1 Ralpha 2.115 1.063 1.411 1.320 2.242 1.723 1.903 1.286 1.988 1.262 1.712 2.018 1.081 2.350 0.889 2.566 3.292 1.997 0.246 2.328 Nqual -0.576 0.679-0.415-0.121-0.517-0.182-0.507 0.330-0.011-0.433-0.267 0.071-0.187-0.491 0.065-0.016-0.564-0.478 0.972-0.659 Mabs 0.390 0.490 0.447 0.455 0.378 0.416 0.404 0.461 0.395 0.464 0.420 0.396 0.486 0.375 0.517 0.362 0.329 0.395 0.743 0.375 Try Ralpha Nqual Sigma-1 M(abs) CFOM Seminvariants 1420309. 0.966 -0.509 -0.308 0.502 1.160 -+-++ -++-- -+++- +-+-+ --++- -++-+ +--++ ---+ 810089. 0.447 0.825 0.345 0.647 3.598 +---- ++++- +---- +++-+ +++-- +++-- ++--- --++ 1953293. 0.576 -0.305 0.449 0.593 0.993 --+-- ---++ -++-- +++++ +---+ -+-++ +++++ -+-+ 1377857. 0.590 -0.196 0.179 0.594 1.159 ----+ +-+++ +++-+ +-+-- -+--- +-+++ --+-- ++-- 597829. 1.174 -0.658 0.549 0.471 1.260 -++-- --+-+ --+-- --+++ -+--+ +++-+ +++-+ -+-- 891993. 0.864 -0.033 0.203 0.522 1.705 +--+- +++++ +---- +++++ +++-+ +++-+ +++-- --++ 265661. 0.803 -0.652 0.089 0.535 0.892 -+-++ +--+- --+-- ++--+ +-+-+ +---+ --++- +--- 1328305. 0.576 0.167 -0.542 0.592 1.823 +++-+ +++-- -++++ +-++- ++--- +++-- -+--- +--+ 350069. 0.938 -0.073 0.487 0.506 1.706 -++-- +-+-- --+-- -++++ -++-- +--++ +-+-+ --++ 1750345. 0.605 -0.414 -0.734 0.581 0.892 ++-+- ---+- -+++- +---- +--+- +++-+ -++++ ++-+ 363117. 0.643 -0.045 0.259 0.575 1.462 +-+-+ +---+ ----- +++-- ----- +--++ --+-+ -+++ 1815585. 0.975 -0.050 0.220 0.501 1.785 -++-- +-+-- --+-- +-+-+ -+--- +++-- --+-- ++-+ 689317. 0.466 -0.077 0.444 0.638 1.228 -+++- +-+++ +-+-- +--+- -++++ -++-- ++--- --++ 1349433. 1.126 -0.469 -0.187 0.477 1.357 +++++ --+-+ -+-+- +-+-+ ++++- +-+-- ++-++ ++-- 455709. 0.342 0.116 0.429 0.691 1.478 +-+++ +---+ +---- -+--+ --+-+ ++++- ++--- -+-- 181393. 1.162 -0.048 0.281 0.473 1.975 -++-- +-+-+ --+-- --+-+ -+--- ++--- --+-+ -++- 906965. 1.829 -0.743 0.319 0.404 1.872 ++--- ----- ++--- --+-- --+++ -++-+ +++++ -+++ 340521. 1.044 -0.531 0.221 0.489 1.219 ++--- ----+ ++--- --+-+ -++-+ -++-+ ++++- --++ 1702605. 0.134 0.990 0.453 1.086 3.898 +-+-+ -+-++ ----+ +-+-- ----+ -+-++ +-+-- --++ 124417. 1.015 -0.541 0.213 0.495 1.183 ----+ +++++ -++-+ ++-+- --++- --+-- -++++ -+++ 622085. 0.494 -0.389 0.200 0.619 0.808 ----- +++++ -++-- ++--- ----+ --+-- ---+- +--+ 1013273. 1.328 -0.395 0.697 0.451 1.636 -++-- --+-+ --+-- -++++ -+++- +-+-+ +-+-- -+-- 872061. 0.569 -0.329 -0.229 0.602 0.954 +++-+ -++++ -++++ -+--+ ++--+ --+++ +-+-+ +-+- 166001. 0.324 -0.692 0.652 0.687 0.390 -++-- -+++- +-+-- ----- ---++ --+++ +++++ ++-- 830005. 0.689 -0.326 -0.471 0.559 1.078 +++++ +++-- -+-+- +-++- ++--+ ++++- -+--- +--- 2052873. 0.703 -0.365 0.450 0.556 1.045 +---- -++-- ----- ----- +++++ ----- --+-- +--- 1875757. 0.949 -0.068 0.044 0.506 1.727 -+--+ +---+ +-+-- --+-- ++--- ++++- --+-+ ++++ 990177. 1.584 -0.232 0.429 0.427 2.099 -+--+ --+-- +++-+ -++-+ -++++ -++-- +---+ -+++ 756581. 0.676 -0.387 0.341 0.560 0.993 ++--- +---- ++--+ -++++ ----+ ----- +--++ --+- 1685753. 0.925 -0.194 -0.520 0.510 1.496 ++--- ++-+- -+-+- ++--- -++-+ -+-+- ----- +-++ 40157. 0.869 0.033 0.450 0.519 1.835 +-+-+ ++--- +---- ++-+- ---+- +-++- -++-- +-+- 200785. 1.579 -0.602 0.610 0.426 1.700 --+-- ++--- +++-- -+--+ ++-+- -++++ +-+-- ++-- 170201. 0.568 -0.651 0.334 0.600 0.657 -+--+ ++-+- --+-+ -+-++ +-++- +---- --+++ +--- 303605. 0.732 0.610 0.399 0.548 3.166 --++- +--+- -++-+ ----+ +++++ ++--+ +---- --++ 1035749. 0.511 -0.029 0.380 0.610 1.359 --++- ++--+ +++-+ ---+- +--+- +-+++ +-++- +-+- 1261365. 0.810 -0.550 0.414 0.534 0.970 +-+++ --+++ +---- ++-++ +-+-- ++++- +++++ -+-- 1298669. 0.586 -0.009 0.256 0.591 1.472 +-+-+ -+-+- +---- ++-++ ----- +--++ -++-+ ++++ 727901. 0.626 -0.187 0.122 0.578 1.208 --++- -+--+ +++-- ----+ +-++- ++-+- ---++ ++++ 1995085. 1.196 -0.744 0.297 0.469 1.239 ++--- +---- ++--- --+-+ -++-- ++-++ +-+-- --+- 1466601. 0.538 0.048 0.570 0.612 1.533 -++-- +++-- --+-- --+-+ ---++ ---+- +++++ ++-+ 851005. 1.165 -0.656 0.092 0.472 1.251 +++++ +-+++ ++--- ++-++ +++-- -+--- --+-+ -+-+ 1009445. 0.036 -0.803 0.504 1.026 0.057 -+--+ ++-+- --+-+ -+-++ +-++- +---- +-+++ ++-- 403405. 0.958 -0.221 -0.897 0.504 1.491 ++-+- ++-++ -++++ +---- -++-+ -+++- ----- ++++ 1041549. 0.622 -0.202 0.274 0.578 1.181 ----+ -++-+ -++-+ +---- --+++ --+-+ ---+- ++-+ 1542353. 0.036 -0.803 0.504 1.026 0.057 -+--+ ++-+- --+-+ -+-++ +-++- +---- +-+++ ++-- 872901. 0.546 -0.008 -0.330 0.608 1.432 +---- -++-- --+++ +---- +++++ --+-+ ----+ ++-- 984441. 0.454 -0.231 0.390 0.631 0.971 --++- -+-++ -++-- -++-+ +--+- -+-+- ++++- +--+ 1013441. 0.491 -0.210 0.439 0.626 1.039 -++-- +-+++ +-+-- ---+- -+++- -++-- -+--- ---+ 813081. 0.924 -0.487 0.305 0.510 1.138 +---- +++-- ----- +---- ++--+ ----- --+-- +--- 1391373. 0.622 -0.202 0.274 0.578 1.181 ----+ -++-+ -++-+ +---- --+++ --+-+ ---+- ++-+ 289529. 0.639 0.254 -0.270 0.582 2.088 ----+ +++-+ -++++ ----+ --+-- +-+-- +-++- -+-+ 1495753. 0.712 -0.517 0.345 0.553 0.899 -++-- --+++ +-+-- ---+- -++-+ -++-- -+--- ---+ 664841. 0.324 -0.692 0.652 0.687 0.390 -++-- -+++- +-+-- ----- ---++ --+++ +++++ ++-- 1612985. 1.027 -0.453 0.281 0.491 1.274 +++-+ +-++- ++--+ ++-++ +-+-- -++-- --++- ---- 1316197. 0.700 -0.602 0.394 0.561 0.821 +---- -++-- ----+ +---- +++++ ----- --+++ +--- 665409. 1.016 -0.357 0.458 0.492 1.368 -++-- +-+-- --+-- -++-+ -++-- +--++ +-+-- +-++ 1229893. 0.134 0.994 0.467 1.088 3.914 +-+-+ -+--+ ----+ +-+-- ----+ -+-++ +---- --++ 1125493. 0.590 -0.196 0.179 0.594 1.159 ----+ +-+++ +++-+ +-+-- -+--- +-+++ --+-- ++-- 1001477. 0.699 -0.320 0.449 0.559 1.096 --+-- ---+- -++-- +++++ +---+ -+-++ +++++ -+-+ 1742241. 0.816 -0.168 -0.360 0.530 1.427 +++-+ --+-- -+-+- --++- +-+-+ -+--- -+++- +--+ 1387197. 0.546 0.051 0.193 0.602 1.548 ----+ --++- +++-+ +-+-- -+--- +-+++ --+-- ++-- 1121869. 0.810 -0.395 -0.027 0.531 1.118 --+-- ---+- -+-+- +++++ +---+ -++++ ++-++ -+-+ 241721. 1.101 -0.094 0.328 0.481 1.835 -++-- +-+-- --+-- -++-+ -++-- +--++ --+-- ---+ 1433161. 0.036 -0.803 0.504 1.026 0.057 -+--+ ++-+- --+-+ -+-++ +-++- +---- +-+++ ++-- 1412773. 1.256 -0.454 0.620 0.461 1.502 -++-- ----+ --+-+ -++-+ ++-+- +-+-- +---+ ++-- 1720081. 1.118 -0.290 0.599 0.477 1.553 +-+-+ +---+ +---- -+--+ -++-- +++++ ++--- ---- 522161. 1.165 0.110 0.424 0.472 2.289 ++--- ++-++ -+--- ---+- --++- +---+ +++-+ +-+- 1175145. 0.133 0.989 0.484 1.091 3.894 +-+-+ -+-+- ----+ +-+-- -+--+ ---++ +---- --++ 471113. 0.675 0.195 -0.175 0.566 1.985 +---- -++-- ---++ +---- +++++ ----- --+-+ +--- 844345. 1.148 -0.561 0.374 0.474 1.299 ++--- +---- ++--- -++++ ----+ ---++ +---- ---+ 1904137. 0.925 -0.115 0.201 0.509 1.622 --+-- ---++ +++-- -+-+- +-+-- -+--+ ---++ ++++ 1534273. 0.700 -0.265 0.365 0.558 1.169 ---++ +-+-- -++-- ++-++ -+-++ -+-++ ++--+ -+++ 603709. 0.324 -0.692 0.652 0.687 0.390 -++-- -+++- +-+-- ----- ---++ --+++ +++++ ++-- 1335213. 0.338 -0.298 0.420 0.696 0.763 +-+++ ----+ +---- -+--+ --+-+ ++++- ++-++ -+-- 608089. 1.044 -0.022 0.278 0.488 1.904 -++-- +-+-- --+-- -++-+ -++-- +--++ --+-+ --++ 1058985. 0.599 -0.106 -0.301 0.589 1.311 ----+ +++++ +++++ +-+-- --+-- +-+-- +-+++ -+-+ 1379033. 0.480 -0.119 0.551 0.618 1.172 --+-- ++--+ +++-+ +--+- +--+- +-+++ +-++- ++-- 1670001. 0.797 -0.530 0.522 0.533 0.973 ++--- +---- ++--+ -++++ ---++ ---+- +--++ ---- 211797. 0.324 -0.692 0.652 0.687 0.390 -++-- -+++- +-+-- ----- ---++ --+++ +++++ ++-- 1074865. 0.957 -0.181 0.077 0.504 1.548 -+-++ -+--- +-+-- +++-+ +-++- -++-+ --+++ +--+ 49029. 0.377 0.003 0.292 0.666 1.285 +--+- --+++ ----+ ---++ +---- -+-+- +-+++ -+-- 952465. 0.619 -0.094 0.390 0.580 1.351 --++- -+-++ -++-- -++-+ +--+- -+-+- ++++- +--+ 1415309. 0.036 -0.803 0.504 1.026 0.057 -+--+ ++-+- --+-+ -+-++ +-++- +---- +-+++ ++-- 1832437. 0.725 -0.362 0.062 0.550 1.070 -+++- --+++ +-+-+ +--+- -++-- -++-- -++-- --++ 465057. 0.639 -0.575 0.344 0.576 0.779 +---- -++-- ----+ +---- +++++ ----- --+++ +-+- 246745. 0.036 -0.803 0.504 1.026 0.057 -+--+ ++-+- --+-+ -+-++ +-++- +---- +-+++ ++-- 594437. 0.524 -0.252 0.476 0.612 1.011 -++-- +-+++ +-+-- ---+- -++-- -+--+ ++--- ++-+ 395677. 0.736 -0.649 0.363 0.550 0.826 +---- -++-- ----+ +---- +++++ ----- --+++ ++-- 173189. 0.957 -0.181 0.077 0.504 1.548 -+-++ -+--- +-+-- +++-+ +-++- -++-+ --+++ +--+ 752857. 1.002 -0.137 0.201 0.496 1.663 ++-+- -+--+ ++--+ +++-+ ---+- --+-+ +-++- +--+ 180861. 0.395 0.495 0.450 0.675 2.482 -+++- +-+++ +-+-- ---+- -++++ -+--- ++--- +-++ 2023909. 0.676 -0.387 0.341 0.560 0.993 ++--- +---- ++--+ -++++ ----+ ----- +--++ --+- 2068701. 0.575 -0.100 0.316 0.592 1.298 +---- -++-- ----+ +---- +++++ --+-- --+-+ +++- 2044209. 0.335 -0.442 0.429 0.701 0.593 +-+++ +---+ +---- -+--+ --+-+ ++++- ++--+ -+-- 150409. 0.036 -0.803 0.504 1.026 0.057 -+--+ ++-+- --+-+ -+-++ +-++- +---- +-+++ ++-- 1089381. 0.036 -0.803 0.504 1.026 0.057 -+--+ ++-+- --+-+ -+-++ +-++- +---- +-+++ ++-- 1826773. 0.743 -0.270 0.162 0.549 1.206 -+--+ +--++ --+-+ -+-+- ++--+ ++-+- --+-+ ++-+ 1046009. 0.674 -0.267 0.115 0.567 1.141 ----+ +-+++ +++-+ +-+-- -+--- +-+++ --+-- ++-+ 2001245. 0.860 -0.432 0.107 0.525 1.129 +++++ --+++ ++--- +--++ +-+-- +-++- -++++ -+-- 1068201. 0.627 0.161 -0.017 0.580 1.862 ---++ +++++ +++-- +++-- ----+ --+-+ ---+- +-++ 1505009. 0.590 -0.196 0.179 0.594 1.159 ----+ +-+++ +++-+ +-+-- -+--- +-+++ --+-- ++-- 1460981. 0.690 0.018 0.178 0.560 1.626 --+-- +--++ +++-- +-++- +-+-+ --+-+ ----+ ++++ 1954381. 0.482 -0.202 0.583 0.619 1.041 --+-- ++--+ +++-+ +--+- +--+- +-+++ +-++- +--- 367553. 1.314 -0.236 0.580 0.455 1.824 +---- ---+- -+--- +++-- -+-++ +--++ ++-+- ---- 305993. 0.547 -0.282 0.449 0.601 0.993 --+-- ---++ -++-- +++++ +---+ -+-++ +++++ -+-+ 1810109. 0.791 -0.135 0.194 0.537 1.455 --+-- ----- +++-- +---- +++-+ --+-- --+-+ ++++ 1952105. 0.626 -0.148 0.332 0.576 1.270 --++- -+-++ -++-- -++-+ +-++- -+-+- ++++- +-++ 1338341. 0.576 0.167 -0.542 0.592 1.823 +++-+ +++-- -++++ +-++- ++--- +++-- -+--- +--+ 1796629. 0.627 0.161 -0.017 0.580 1.862 ---++ +++++ +++-- +++-- ----+ --+-+ ---+- +-++ 267477. 0.036 -0.803 0.504 1.026 0.057* -+--+ ++-+- --+-+ -+-++ +-++- +---- +-+++ ++-- 594537. 0.324 -0.692 0.652 0.687 0.390 -++-- -+++- +-+-- ----- ---++ --+++ +++++ ++-- 872941. 0.333 -0.451 0.429 0.701 0.583 +-+++ +---+ +---- -+--+ --+-+ ++++- ++--+ -+-- 1597213. 0.581 -0.658 -0.827 0.591 0.666 ++-+- ---+- -++++ +---- ----+ +++-+ -++++ -++- 1487077. 0.690 0.018 0.178 0.560 1.626 --+-- +--++ +++-- +-++- +-+-+ --+-+ ----+ ++++ 1557589. 0.454 -0.231 0.390 0.631 0.971 --++- -+-++ -++-- -++-+ +--+- -+-+- ++++- +--+ 1615365. 1.451 -0.545 0.312 0.441 1.615 +--+- +-+++ +---- -+-++ +-+-+ -+++- +++++ -+-- 1569809. 0.572 -0.248 0.449 0.594 1.064 --+-- ---++ -++-- +++++ +---+ -+-++ +++++ -+-+ 384789. 0.447 0.825 0.345 0.647 3.598 +---- ++++- +---- +++-+ +++-- +++-- ++--- --++ 2072985. 0.630 -0.299 0.391 0.574 1.054 +---- -++-- ----- +---- +++++ ----- --+-- +-+- 797529. 0.642 -0.193 0.571 0.573 1.216 +---- -++-- ----- +---- +++++ ----- +-++- +-+- 1760641. 0.577 -0.146 -0.274 0.590 1.224 +---- -++-- ---++ +---- +++++ --+-- --+-+ +++- 614201. 0.546 0.051 0.193 0.602 1.548 ----+ --++- +++-+ +-+-- -+--- +-+++ --+-- ++-- 341517. 0.771 -0.224 0.220 0.541 1.298 ++--- ----- ++--- --+-+ --+-+ -++-+ ++++- --++ 2047617. 0.644 -0.263 0.366 0.569 1.116 +---- -++-- ----+ +---- +++++ ----- --+-- +-+- 1045101. 0.576 -0.305 0.449 0.593 0.993 --+-- ---++ -++-- +++++ +---+ -+-++ +++++ -+-+ 1961865. 0.720 -0.107 0.358 0.551 1.430 ---++ --+-- -++-- ++-++ -+-++ -+-++ ++--+ ++++ 1417797. 0.524 -0.252 0.476 0.612 1.011 -++-- +-+++ +-+-- ---+- -++-- -+--+ ++--- ++-+ 1963493. 0.635 -0.061 0.390 0.571 1.425 --++- -+-++ -++-- -++-+ +--+- -+-+- ++++- +--+ 151529. 0.036 -0.803 0.504 1.026 0.057 -+--+ ++-+- --+-+ -+-++ +-++- +---- +-+++ ++-- 975337. 0.036 -0.803 0.504 1.026 0.057 -+--+ ++-+- --+-+ -+-++ +-++- +---- +-+++ ++-- 724641. 0.036 -0.803 0.504 1.026 0.057 -+--+ ++-+- --+-+ -+-++ +-++- +---- +-+++ ++-- 266317. 0.036 -0.803 0.504 1.026 0.057 -+--+ ++-+- --+-+ -+-++ +-++- +---- +-+++ ++-- 168353. 0.036 -0.803 0.504 1.026 0.057 -+--+ ++-+- --+-+ -+-++ +-++- +---- +-+++ ++-- 1459173. 0.036 -0.803 0.504 1.026 0.057 -+--+ ++-+- --+-+ -+-++ +-++- +---- +-+++ ++-- 1505269. 0.036 -0.803 0.504 1.026 0.057 -+--+ ++-+- --+-+ -+-++ +-++- +---- +-+++ ++-- CFOM Range Frequency 0.000 - 0.020 0 0.020 - 0.040 0 0.040 - 0.060 15 0.060 - 0.080 0 0.080 - 0.100 0 0.100 - 0.120 0 0.120 - 0.140 0 0.140 - 0.160 0 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 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 9 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 1 0.520 - 0.540 0 0.540 - 0.560 0 0.560 - 0.580 0 0.580 - 0.600 2 0.600 - 9.999 229 256. Phase sets refined - best is code 267477. with CFOM = 0.0572 0.3 seconds CPU time Tangent expanded to 474 out of 474 E greater than 1.200 Highest memory used = 2049 / 5029 0.0 seconds CPU time FMAP and GRID set by program FMAP 8 3 6 GRID -4.167 -2 24 4.167 2 1 E-Fourier for 2007may0002 in I4(1)/a Maximum = 230.00, minimum = -49.46 highest memory used = 8741 / 9582 0.0 seconds CPU time Peak list optimization RE = 0.178 for 12 surviving atoms and 474 E-values Highest memory used = 1556 / 4266 0.0 seconds CPU time E-Fourier for 2007may0002 in I4(1)/a Maximum = 240.97, minimum = -51.35 highest memory used = 8741 / 9582 0.0 seconds CPU time Peak list optimization RE = 0.175 for 12 surviving atoms and 474 E-values Highest memory used = 1556 / 4266 0.0 seconds CPU time E-Fourier for 2007may0002 in I4(1)/a Maximum = 246.49, minimum = -44.85 highest memory used = 8741 / 9582 0.0 seconds CPU time Molecule 1 scale 1.000 inches = 2.540 cm per Angstrom 13 9 16 6 10 14 4 12 8 17 5 2 16 1 11 18 15 7 16 12 3 18 14 19 Atom Peak x y z SOF Height Distances and Angles 1 246. 0.2183 0.3426 0.1264 1.000 2.39 0 5 1.352 0 7 1.443 113.8 0 17 1.960 47.3 139.6 0 18 1.077 121.1 112.3 107.1 2 219. 0.2601 0.3313 0.5475 1.000 0.60 0 8 1.425 0 11 1.413 113.8 3 169. 0.2876 0.4467 0.0156 1.000 2.66 0 12 1.522 0 19 1.506 89.6 4 158. 0.1300 0.2906 0.2221 1.000 3.11 0 5 1.424 0 6 1.372 118.9 0 17 0.962 71.3 135.8 5 143. 0.1865 0.3143 0.2761 1.000 2.29 0 1 1.352 0 4 1.424 118.8 0 8 1.399 124.8 116.4 0 17 1.439 89.1 39.2 138.5 6 140. 0.0984 0.2604 0.3721 1.000 2.98 0 4 1.372 0 9 1.370 121.9 7 140. 0.2802 0.3498 0.1785 1.000 1.28 0 1 1.443 0 11 1.526 107.5 0 12 1.534 112.6 116.8 0 15 1.062 116.0 106.1 97.8 0 16 1.906 170.9 68.2 64.6 73.1 8 137. 0.2045 0.3070 0.4851 1.000 1.43 0 2 1.425 0 5 1.399 118.3 0 10 1.400 120.2 121.4 9 137. 0.1191 0.2533 0.5729 1.000 2.10 0 6 1.370 0 10 1.302 121.0 0 13 1.126 115.7 122.9 10 134. 0.1706 0.2743 0.6284 1.000 1.32 0 8 1.400 0 9 1.302 120.2 0 14 1.958 87.0 104.1 11 132. 0.2835 0.3730 0.4036 1.000 1.00 0 2 1.413 0 7 1.526 111.2 0 16 1.949 129.4 65.2 12 117. 0.3143 0.3848 0.0109 1.000 1.46 0 3 1.522 0 7 1.534 105.0 0 15 1.981 136.8 32.1 0 16 1.864 109.7 67.4 58.9 2 14 1.974 102.1 125.8 104.4 59.4 13 50. 0.0869 0.2335 0.6885 1.000 2.17 0 9 1.126 14 44. 0.1519 0.3498 0.7649 1.000 2.25 0 10 1.958 1 12 1.974 152.8 3 16 1.905 148.8 57.4 15 41. 0.3062 0.3106 0.1751 1.000 0.36 0 7 1.062 0 12 1.981 50.1 0 16 1.894 74.4 57.5 16 36. 0.3588 0.3721 0.2539 1.000 0.00 0 7 1.906 0 11 1.949 46.6 0 12 1.864 48.0 86.2 0 15 1.894 32.4 65.8 63.6 2 14 1.905 110.4 144.4 63.2 110.7 5 18 1.804 114.8 91.9 92.4 147.1 73.0 17 34. 0.1579 0.2802 0.1138 1.000 2.74 0 1 1.960 0 4 0.962 104.5 0 5 1.439 43.6 69.5 18 33. 0.2006 0.3806 0.0454 1.000 3.33 0 1 1.077 4 16 1.804 122.6 19 32. 0.3436 0.4710 -0.0808 1.000 2.17 0 3 1.506 Atom Code x y z Height Symmetry transformation 12 1 0.1348 0.4357 0.7609 3.58 -0.2500+Y 0.7500-X 0.7500+Z 14 2 0.4002 0.4019 0.0149 0.15 0.7500-Y 0.2500+X -0.7500+Z 16 3 0.1221 0.3912 1.0039 2.74 -0.2500+Y 0.7500-X 0.7500+Z 16 4 0.1221 0.3912 0.0039 4.92 -0.2500+Y 0.7500-X -0.2500+Z 18 5 0.3694 0.4506 0.2954 0.66 0.7500-Y 0.2500+X 0.2500+Z 0.0 seconds CPU time +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007may0002 finished at 17:19:19 Total CPU time: 0.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++