+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXS-97 - CRYSTAL STRUCTURE SOLUTION - WinGX VERSION + + Copyright(C) George M. Sheldrick 1986-97 Release 97-2 + + s92 started at 15:35:34 on 03 Aug 2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01ESP002 IN P212121 CELL 0.71073 8.4889 11.5350 31.9275 90 90 90 ZERR 4 0.0002 0.0002 0.0006 0 0 0 LATT -1 SYMM 1/2+X, 1/2-Y, -Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2-X, -Y, 1/2+Z SFAC C H N O CL UNIT 104 132 16 48 4 V = 3126.32 At vol = 18.2 F(000) = 1320.0 mu = 0.19 mm-1 Max single Patterson vector = 32.5 cell wt = 2516.06 rho = 1.336 OMIT 4.00 180.00 ESEL 1.200 5.000 0.005 0.700 0 TREF HKLF 4 11451 Reflections read, of which 36 rejected Maximum h, k, l and 2-Theta = 10. 14. 41. 54.93 INCONSISTENT EQUIVALENTS h k l F*F Sigma(F*F) Esd of mean(F*F) 1 1 0 824.49 30.08 263.40 1 1 1 214.83 3.09 55.18 1 1 2 69.42 0.12 134.97 1 2 2 811.74 10.30 86.49 2 4 2 19.98 0.30 3.22 3 7 2 59.05 0.63 11.18 2 4 3 69.32 0.33 15.09 4 6 3 52.70 0.55 23.96 3 7 3 42.82 0.77 6.00 4 7 3 28.72 0.74 6.48 3 8 3 54.74 0.92 12.11 2 2 4 191.29 1.72 25.58 2 4 4 15.92 0.21 2.00 2 2 5 245.97 0.24 293.10 2 3 5 9.79 0.20 1.19 2 3 6 54.73 0.22 9.69 2 4 6 124.09 0.34 20.99 3 3 8 7.18 0.22 1.40 3 3 9 137.71 0.48 106.69 3 4 9 46.91 0.46 11.36 3 4 10 42.22 0.45 10.11 3 5 10 9.79 0.39 1.95 3 6 11 20.68 0.52 4.64 4 5 14 27.98 0.68 9.20 3981 Unique reflections, of which 2782 observed R(int) = 0.0932 R(sigma) = 0.0958 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) 14. 34. 87. 119. 149. 178. 120. 160. 207. 290. 396. 474. 462. N(measured) 15. 35. 89. 121. 153. 187. 125. 170. 226. 321. 465. 665. 1026. N(theory) 22. 36. 89. 121. 153. 187. 126. 170. 226. 323. 466. 669. 1048. 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 = 7081 / 19905 Observed E .GT. 1.200 1.300 1.400 1.500 1.600 1.700 1.800 1.900 2.000 2.100 Number 1098 927 727 577 460 358 270 195 162 114 Centric Acentric 0kl h0l hk0 Rest Mean Abs(E*E-1) 0.968 0.736 0.959 0.878 0.902 0.726 0.1 seconds CPU time SUMMARY OF PARAMETERS FOR 01ESP002 IN P212121 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 13 nf 16 s+ 0.800 s- 0.200 wr 0.200 PHAN steps 10 cool 0.900 Boltz 0.300 ns 193 mtpr 40 mnqr 10 TREF np 256. nE 327 kapscal 0.850 ntan 3 wn -0.384 FMAP code 8 PLAN npeaks -59 del1 0.500 del2 1.500 MORE verbosity 1 TIME t 9999999. 193 Reflections and 2084. unique TPR for phase annealing 327 Phases refined using 10271. unique TPR 470 Reflections and 20596. unique TPR for R(alpha) 0.1 seconds CPU time 4332 Unique negative quartets found, 1512 used for phase refinement 0.1 seconds CPU time Highest memory used to derive phase relations = 6897 / 32097 ONE-PHASE SEMINVARIANTS h k l E P+ Phi 0 0 10 2.397 0.46 2 0 8 2.488 0.22 0 4 14 2.514 0.77 2 2 0 1.752 0.19 4 2 0 1.781 0.50 4 10 0 2.409 0.65 0 6 4 1.789 0.62 0 6 0 1.519 0.08 0 4 10 1.580 0.48 0 8 14 1.873 0.49 0 4 16 1.571 0.61 2 10 0 2.093 0.39 0 6 20 2.046 0.41 0 10 10 1.879 0.34 2 8 0 1.650 0.70 2 0 2 1.278 0.50 4 0 20 2.014 0.32 2 0 18 1.509 0.55 8 0 6 1.614 0.66 0 0 26 1.494 0.08 2 0 10 1.259 0.60 2 0 6 1.251 0.52 2 0 28 1.498 0.61 8 0 10 1.779 0.69 2 0 26 1.613 0.47 4 0 16 1.407 0.88 0 8 6 1.328 0.54 Expected value of Sigma-1 = 0.536 Following phases held constant with unit weights for the initial 4 weighted tangent cycles (before phase annealing): h k l E Phase/Comment 0 0 10 2.397 0 or 180 at random 1 2 3 2.424 random phase 2 2 3 2.440 random phase 2 0 8 2.488 0 or 180 at random 1 0 8 2.347 0 or 180 at random 0 4 14 2.514 0 or 180 at random 1 1 4 1.908 random phase 3 1 8 1.893 random phase 0 2 7 1.968 0 or 180 at random 1 2 2 1.791 random phase 2 2 0 1.752 180 sigma-1 = 0.190 0 1 9 1.642 90 or 270 at random 0 6 0 1.519 180 sigma-1 = 0.082 0 3 3 1.703 90 or 270 at random 5 2 3 1.827 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 311 Unique NQR employed in phase annealing 128 Parallel refinements, highest memory = 9610 / 96152 0.0 seconds CPU time STRUCTURE SOLUTION for 01ESP002 IN P212121 Phase annealing cycle: 1 Beta = 0.18529 Ralpha 0.166 0.317 0.405 0.403 0.198 0.269 0.216 0.381 0.417 0.309 0.367 0.249 0.443 0.422 0.247 0.435 0.228 0.242 0.140 0.284 Nqual 0.370-0.176-0.176-0.085 0.059-0.213 0.204-0.107-0.159-0.028-0.016-0.146-0.251-0.170-0.063-0.172-0.038-0.262 0.336 0.052 Mabs 0.856 0.726 0.655 0.650 0.812 0.722 0.824 0.672 0.648 0.713 0.676 0.765 0.644 0.660 0.754 0.648 0.798 0.766 0.947 0.742 Phase annealing cycle: 2 Beta = 0.20588 Ralpha 0.188 0.425 0.570 0.420 0.199 0.303 0.247 0.461 0.481 0.403 0.422 0.291 0.499 0.495 0.275 0.444 0.285 0.274 0.143 0.377 Nqual -0.001-0.383-0.496-0.527-0.274-0.483-0.108-0.437-0.484-0.460-0.412-0.457-0.493-0.508-0.401-0.245-0.361-0.499-0.189-0.404 Mabs 0.817 0.662 0.595 0.643 0.806 0.701 0.763 0.635 0.616 0.659 0.649 0.717 0.625 0.624 0.739 0.648 0.735 0.729 0.865 0.669 Phase annealing cycle: 3 Beta = 0.22876 Ralpha 0.184 0.463 0.566 0.500 0.194 0.309 0.195 0.486 0.425 0.430 0.372 0.282 0.590 0.505 0.295 0.429 0.258 0.260 0.166 0.436 Nqual 0.084-0.412-0.598-0.597-0.274-0.522-0.207-0.485-0.446-0.562-0.405-0.426-0.474-0.439-0.446-0.363-0.374-0.520-0.252-0.465 Mabs 0.820 0.641 0.600 0.608 0.825 0.697 0.806 0.625 0.636 0.646 0.680 0.722 0.596 0.619 0.728 0.649 0.749 0.735 0.853 0.643 Phase annealing cycle: 4 Beta = 0.25417 Ralpha 0.211 0.326 0.491 0.384 0.189 0.349 0.190 0.423 0.392 0.380 0.359 0.239 0.379 0.316 0.248 0.319 0.202 0.263 0.141 0.320 Nqual -0.111-0.358-0.522-0.565-0.231-0.560-0.200-0.476-0.476-0.503-0.350-0.429-0.431-0.414-0.461-0.302-0.299-0.563-0.215-0.405 Mabs 0.802 0.705 0.624 0.656 0.834 0.679 0.831 0.646 0.655 0.668 0.694 0.753 0.677 0.700 0.759 0.701 0.817 0.739 0.881 0.700 Phase annealing cycle: 5 Beta = 0.28242 Ralpha 0.192 0.298 0.382 0.356 0.154 0.301 0.187 0.411 0.397 0.315 0.337 0.217 0.411 0.279 0.209 0.261 0.150 0.246 0.148 0.232 Nqual -0.182-0.397-0.505-0.591-0.125-0.504-0.246-0.515-0.492-0.477-0.425-0.444-0.567-0.498-0.379-0.309-0.302-0.498-0.213-0.440 Mabs 0.813 0.724 0.668 0.679 0.883 0.711 0.816 0.656 0.655 0.688 0.702 0.774 0.656 0.722 0.793 0.743 0.876 0.764 0.875 0.750 Phase annealing cycle: 6 Beta = 0.31380 Ralpha 0.181 0.303 0.386 0.330 0.150 0.210 0.171 0.366 0.337 0.273 0.243 0.178 0.355 0.280 0.194 0.201 0.145 0.235 0.135 0.243 Nqual -0.185-0.416-0.530-0.586-0.153-0.487-0.258-0.540-0.453-0.465-0.340-0.506-0.544-0.518-0.374-0.316-0.300-0.421-0.214-0.553 Mabs 0.826 0.729 0.670 0.704 0.890 0.771 0.829 0.670 0.681 0.716 0.766 0.809 0.686 0.723 0.807 0.791 0.893 0.767 0.896 0.743 Phase annealing cycle: 7 Beta = 0.34866 Ralpha 0.176 0.300 0.331 0.318 0.128 0.196 0.175 0.271 0.300 0.283 0.229 0.183 0.318 0.249 0.167 0.181 0.137 0.230 0.142 0.218 Nqual -0.258-0.452-0.513-0.575-0.238-0.448-0.266-0.533-0.458-0.482-0.322-0.551-0.525-0.484-0.344-0.338-0.250-0.420-0.214-0.536 Mabs 0.827 0.727 0.699 0.710 0.912 0.785 0.847 0.721 0.699 0.716 0.783 0.812 0.698 0.750 0.838 0.816 0.908 0.776 0.911 0.765 Phase annealing cycle: 8 Beta = 0.38740 Ralpha 0.165 0.226 0.326 0.292 0.132 0.180 0.170 0.260 0.272 0.283 0.224 0.174 0.271 0.240 0.167 0.148 0.140 0.220 0.149 0.240 Nqual -0.155-0.375-0.519-0.557-0.221-0.468-0.275-0.477-0.456-0.481-0.275-0.555-0.528-0.495-0.424-0.369-0.149-0.408-0.226-0.546 Mabs 0.852 0.770 0.697 0.721 0.930 0.798 0.837 0.732 0.714 0.724 0.784 0.824 0.731 0.761 0.843 0.839 0.899 0.783 0.895 0.749 Phase annealing cycle: 9 Beta = 0.43045 Ralpha 0.155 0.230 0.339 0.315 0.135 0.182 0.148 0.228 0.260 0.257 0.212 0.157 0.242 0.228 0.188 0.149 0.131 0.226 0.145 0.231 Nqual -0.220-0.418-0.458-0.528-0.261-0.525-0.230-0.485-0.518-0.483-0.284-0.546-0.490-0.393-0.406-0.413-0.224-0.412-0.151-0.561 Mabs 0.862 0.776 0.696 0.708 0.919 0.804 0.852 0.755 0.726 0.750 0.800 0.822 0.756 0.770 0.821 0.840 0.916 0.776 0.901 0.759 Phase annealing cycle: 10 Beta = 0.47827 Ralpha 0.144 0.221 0.340 0.285 0.127 0.196 0.156 0.221 0.284 0.272 0.212 0.161 0.236 0.213 0.184 0.143 0.128 0.237 0.144 0.228 Nqual -0.204-0.379-0.505-0.537-0.285-0.555-0.233-0.522-0.569-0.291-0.292-0.589-0.512-0.436-0.498-0.451-0.221-0.335-0.236-0.556 Mabs 0.869 0.784 0.695 0.736 0.929 0.794 0.848 0.751 0.711 0.741 0.797 0.823 0.761 0.781 0.836 0.829 0.920 0.770 0.889 0.758 Phase refinement cycle: 1 Ralpha 0.577 1.084 1.644 0.982 0.548 1.357 0.613 1.796 2.110 1.410 0.742 0.806 1.321 1.222 0.942 0.935 0.517 1.232 0.604 1.311 Nqual 0.294 0.066-0.316-0.076 0.224-0.387 0.244-0.251-0.283-0.020 0.295-0.006-0.250-0.179-0.046-0.037 0.191-0.050 0.366-0.170 Mabs 0.612 0.492 0.427 0.510 0.616 0.457 0.601 0.415 0.395 0.451 0.563 0.541 0.461 0.473 0.515 0.515 0.633 0.471 0.601 0.461 Phase refinement cycle: 2 Ralpha 0.159 0.211 0.234 0.176 0.165 0.179 0.164 0.275 0.317 0.229 0.167 0.173 0.203 0.200 0.173 0.183 0.160 0.225 0.164 0.206 Nqual 0.441 0.266-0.137 0.456 0.366-0.257 0.438-0.041-0.123 0.291 0.458 0.297 0.001-0.092 0.386 0.207 0.244 0.122 0.597 0.034 Mabs 1.049 0.870 0.829 1.019 1.029 0.850 1.049 0.737 0.701 0.862 1.038 0.956 0.855 0.884 0.966 0.902 1.067 0.830 1.025 0.857 Try Ralpha Nqual Sigma-1 M(abs) CFOM Seminvariants 1420309. 0.181 0.276 0.549 0.996 0.617 --+-- +---- ++--- +++-- ---+- ++ 810089. 0.223 0.123 -0.214 0.843 0.481 --++- --+-+ ++-+- -+++- +---+ -+ 1953293. 0.227 0.001 0.245 0.895 0.376 ++-++ ---+- +-+-- +-++- ++-+- +- 1377857. 0.187 0.342 0.287 0.992 0.713 +-+-+ ++--- +--+- -+-+- -+--+ -- 597829. 0.182 0.198 0.239 0.991 0.520 -+--+ +--++ ----- -+--- +++-+ +- 891993. 0.212 -0.180 0.318 0.865 0.254 +---+ ---++ -+-+- --+-- --++- +- 265661. 0.190 0.246 0.622 0.985 0.587 --+-- +---- ++--- ++++- ---+- ++ 1328305. 0.301 -0.129 -0.101 0.736 0.366 --++- -+--+ -+++- +++-+ +---+ ++ 350069. 0.344 -0.251 -0.550 0.688 0.362 ++-+- +-+++ +-++- +++-+ --+-+ +- 1750345. 0.221 0.329 0.552 0.916 0.729 +++-- ++--+ +--++ +--+- -+--+ ++ 363117. 0.173 0.269 0.504 1.003 0.599 +-+-+ ++--- +--+- -+-+- -+--+ +- 1815585. 0.188 0.160 0.270 0.926 0.484 -+--+ +--+- ----- ---+- +++++ -- 689317. 0.217 -0.117 -0.017 0.829 0.288 -+--+ ---++ +---+ --+++ +---- -+ 1349433. 0.203 -0.084 -0.259 0.917 0.294 ++-++ -+-++ +---- +++-+ +-+++ -+ 455709. 0.182 0.264 0.390 0.937 0.602 +-+-+ ++--- +--+- -+-+- -+-+- -- 181393. 0.207 0.144 -0.016 0.886 0.486 -+++- +++-- +--++ -+--- ++++- -+ 906965. 0.171 0.063 0.241 1.020 0.371 ---++ ++-++ -+--+ +++-- ----- +- 340521. 0.234 0.117 0.130 0.825 0.485 ++--+ ----- --+++ +-++- -+-+- -+ 1702605. 0.181 0.404 0.003 0.967 0.802 +---- +++++ ++-+- ----+ ++++- +- 124417. 0.219 0.142 0.405 0.872 0.495 -++-- ++--- -++-- -+--- -+++- +- 622085. 0.227 0.028 -0.175 0.844 0.397 -++-- +-+-+ +--+- -+--- ++--+ -- 1013273. 0.178 0.077 0.278 1.006 0.391 ---++ +--++ -+--+ +++-- ---+- +- 872061. 0.279 0.071 -0.072 0.754 0.487 +-+-+ +-+++ -+--- -+-++ -+--- ++ 166001. 0.189 -0.008 0.455 0.942 0.330 --+-+ ---++ ----+ ++++- ++-++ -+ 830005. 0.218 0.190 0.197 0.869 0.548 ----+ ----+ -++-+ +-+++ --+-- +- 2052873. 0.271 -0.161 -0.444 0.750 0.321 +++-- --+-+ -++-+ ++-++ -+--+ -+ 1875757. 0.307 -0.306 0.111 0.726 0.313 --++- +---+ --+-+ --+-+ +-+++ -- 990177. 0.180 -0.033 -0.153 0.979 0.303 ---+- -++-- -++-+ +-+++ -++-+ ++ 756581. 0.330 -0.332 0.043 0.699 0.332 +++++ ----- --+-- +-+-+ +-+++ ++ 1685753. 0.226 -0.071 0.009 0.837 0.324 +++-+ +---+ ---+- +++-+ --+-- +- 40157. 0.212 0.143 0.235 0.883 0.490 -++++ -+--- +--+- -+-+- --+-- ++ 200785. 0.205 0.112 0.164 0.891 0.451 ----+ +---- --++- +-+++ -++-- +- 351505. 0.221 0.030 -0.042 0.898 0.392 ++--- +--++ -+-+- +++-+ +-+++ ++ 1135797. 0.250 0.019 0.284 0.798 0.412 --+-+ +---- +-+-- -++-- +---+ -+ 170201. 0.227 0.064 -0.420 0.884 0.428 ++-+- --+-- +--++ ++-+- -+--+ -- 1518025. 0.210 0.278 0.220 0.902 0.649 -+--+ ----- ++-++ -+--- +++-+ ++ 1041549. 0.164 -0.321 0.562 1.025 0.168 --+-+ ---++ ----+ +-+++ ++++- ++ 1757525. 0.215 -0.159 0.151 0.851 0.265 +-+-- -+--+ --+-+ +--++ +---+ -- 60721. 0.205 0.256 0.060 0.928 0.616 +-+-+ ++--- +--+- -+--+ -+-+- -- 399017. 0.180 0.216 0.291 0.967 0.541 -+--+ ++-++ ----- -+--- +++-+ +- 252273. 0.189 0.439 0.281 0.977 0.867 +---- +-+++ ++-+- ---+- ++++- +- 851005. 0.228 0.279 0.455 0.848 0.668 +---+ ----- +++++ ++++- +-+++ +- 854997. 0.213 -0.004 -0.254 0.891 0.357 ++--- +-+++ ++-+- +++-+ +-+++ ++ 76845. 0.171 -0.018 -0.078 0.986 0.305 ----- +++-- -+++- +-+++ -++-- ++ 852921. 0.191 0.273 0.291 0.979 0.622 -+--+ ++-++ ----- -+--- +++-+ +- 1890781. 0.203 0.325 0.647 0.964 0.706 --+-+ ----- ++-++ +-+-- +-+++ +- 1904881. 0.181 0.278 0.577 0.974 0.619 --+-- +---- +++-- +-++- ----- ++ 1217017. 0.177 0.214 0.479 0.993 0.535 +-++- ++--- +--+- ---+- -++-+ +- 322597. 0.197 0.288 -0.071 0.895 0.649 +---+ -+-++ +++-+ -+-++ -+--- -+ 971829. 0.179 -0.022 0.529 0.982 0.310 ----- ++-+- --+-+ +++-- +--++ +- 1848721. 0.200 0.172 -0.012 0.959 0.510 -+--+ -+-+- +---+ ++--+ +-++- -- 1668805. 0.221 -0.005 -0.004 0.890 0.365 +--++ ++-+- +-+-- +++++ +-++- -+ 1482665. 0.238 -0.343 0.532 0.800 0.240 ----+ ++-+- ----- +-+-- +++-+ +- 905613. 0.195 -0.032 0.179 0.881 0.318 ---++ ----- +-++- +-+-- --+-- ++ 807597. 0.223 0.166 -0.226 0.862 0.526 ++-++ ++-+- +-+-- +++-+ +-+++ -+ 1227053. 0.184 0.360 0.212 0.978 0.738 +---- +--++ ++-+- ----+ ++++- +- 1499633. 0.233 0.122 -0.402 0.870 0.489 -+-++ --+++ -+++- -+--- +++-+ +- 289529. 0.185 0.274 0.273 0.976 0.618 --+-- +-+-- ++--- ++++- ----- ++ 2052569. 0.166 -0.364 0.561 1.023 0.166* --+-- ---++ ----+ +-+++ ++++- ++ 719357. 0.187 0.020 0.612 1.008 0.350 ----+ ++-+- --+-+ +-+-- +--++ +- 1001477. 0.182 0.268 0.511 0.984 0.608 --+-- +---- +++-- +++-- ---+- ++ 139541. 0.187 0.036 -0.190 0.982 0.363 ---+- +++-- -++++ +--++ --+-- +- 1940833. 0.167 -0.273 0.769 1.029 0.180 --+-+ ---++ ----+ +-++- ++-+- ++ 539541. 0.161 -0.311 0.512 1.028 0.166 --+-+ ---++ ----+ +-+++ ++-+- ++ 1330473. 0.225 -0.293 0.083 0.846 0.234 +++++ +--+- -+--+ +++-+ +-+++ +- 522161. 0.219 -0.008 0.433 0.834 0.361 +-+-+ ----+ -+-++ +-+++ ++++- ++ 1927917. 0.189 0.119 0.069 0.972 0.442 -+--+ -+-+- +---+ +---+ +-++- -- 1412773. 0.236 -0.063 0.374 0.815 0.340 -+--+ +--+- +--+- +--+- ---++ ++ 603709. 0.236 -0.166 0.184 0.808 0.284 -++++ +--+- +---- +---+ +-++- +- 211797. 0.208 -0.145 0.109 0.897 0.265 -++-+ ---++ +---+ -+-++ ++-+- -+ 258413. 0.186 0.363 0.285 0.979 0.744 +---- +--++ ++-+- ---++ ++++- +- 1379033. 0.186 0.033 0.522 1.006 0.360 ----+ ++-+- --+-- +-+-- +--++ +- 686473. 0.187 -0.073 0.723 0.953 0.284 --+-+ -+-+- --+-+ +-+-- +-+++ +- 92485. 0.220 0.205 0.341 0.878 0.567 ++++- -+--- ++-++ +-++- +---- +- 943293. 0.192 0.149 0.282 0.982 0.476 +---+ ++--- +--+- -+++- -++-+ -+ 726285. 0.202 0.144 0.069 0.951 0.481 -+--- ++-+- +---+ ++--+ +-++- -+ 1074865. 0.185 -0.030 -0.184 0.963 0.310 ---+- +++-+ -++++ +--++ -++-+ ++ 27421. 0.208 0.053 0.161 0.896 0.399 +--++ -+-+- +-+-- -+-+- +++++ -+ 1172861. 0.219 -0.082 -0.180 0.878 0.310 +--++ ----+ +-++- ---++ -+++- -- 1720081. 0.174 0.315 0.472 1.012 0.663 +-+-+ -+--+ +--++ --++- -++-+ -+ 360469. 0.262 -0.032 0.264 0.829 0.386 +---+ +---- --++- --++- --+++ -+ 228133. 0.211 0.333 0.375 0.933 0.725 +---+ +---+ --++- -+-+- --+++ ++ 1018433. 0.205 -0.018 0.109 0.908 0.340 -++-+ ---++ +---+ -+-++ ++-+- -+ 1252601. 0.234 -0.009 0.427 0.832 0.374 +-+-+ --+++ -+--+ ---+- -+++- ++ 1268161. 0.209 0.005 -0.435 0.886 0.361 +--++ --+-+ +++++ -+-++ ++++- -- 180861. 0.212 0.279 0.540 0.910 0.651 ----+ -+-++ ----+ ++++- ---+- +- 1292929. 0.175 0.358 0.370 1.006 0.726 +-+-- -+--+ +--++ -+-+- -++-+ -+ 1828293. 0.191 0.077 0.053 0.914 0.404 -++-- +-+-+ +++-- -+--- --+-- ++ 1475005. 0.191 -0.132 0.118 0.885 0.254 -++-+ ---++ +---+ -++++ +--+- -+ 1225725. 0.176 0.386 0.390 1.009 0.769 +-+-+ -+--+ +--++ -+++- -++-+ -+ 1092493. 0.172 -0.307 0.562 1.022 0.178 --+-+ ---++ ----+ +-+++ ++++- ++ 742953. 0.223 0.043 -0.136 0.883 0.405 +--++ ----+ ++-++ -+-++ ++++- -- 1516877. 0.184 0.010 0.612 1.003 0.339 ----+ ++-+- --+-+ +-+-- +--++ +- 266077. 0.194 0.312 0.542 0.979 0.678 --+-- +---- ++--- +-+-- ----- ++ 1423341. 0.203 0.093 -0.205 0.950 0.431 +-+-- ++++- -+-+- +--++ +---+ -+ 1330385. 0.184 0.361 0.356 0.998 0.739 +-+-+ ++--- +--+- -+++- -++-+ -- 761253. 0.223 0.003 -0.568 0.871 0.373 ++-+- +-+++ ++-++ ++-++ -+-++ -+ 389721. 0.218 0.066 -0.288 0.892 0.421 +--++ ----+ +--+- -+-++ -+-++ -- 492941. 0.198 0.318 0.278 0.932 0.691 +-+-+ ++--- +--+- -+--+ -+-+- +- 1954381. 0.176 0.407 0.285 0.989 0.802 +---- +--++ ++-+- ---++ ++++- +- 984401. 0.187 0.075 0.364 0.974 0.398 --+-+ +-+++ ++-+- --+-- +-+++ ++ 1404549. 0.174 0.007 0.241 1.010 0.327 ---++ ++-++ -+--+ +++-- ----- +- 875533. 0.204 0.166 0.144 0.943 0.507 +++-- +--+- -+-+- ++-+- ++-+- -- 852005. 0.216 0.049 0.007 0.887 0.404 ++--- +--++ ++-+- +++-+ +-+++ ++ 1801341. 0.225 -0.047 0.288 0.834 0.339 -++++ -+--- +-++- ----- -+++- +- 571681. 0.172 0.052 0.241 1.014 0.363 ---++ ++-++ -+--+ +++-- ----- +- 1903933. 0.188 0.332 0.243 0.962 0.700 --+-- +-+-- +++-- +-+-- ----- ++ 1643025. 0.205 0.349 -0.078 0.925 0.742 +---+ --+++ +++-+ -+-++ -+-+- ++ 328605. 0.193 0.169 0.359 0.911 0.498 +-+-+ +--+- +-++- --+-- --+++ -+ 1952105. 0.185 0.048 0.087 0.907 0.372 ----+ ----- --++- +-+++ --+-+ ++ 390421. 0.216 -0.074 -0.063 0.896 0.313 +++++ ---+- +---- +-+++ ++-+- -- 712929. 0.185 0.129 0.617 0.965 0.449 ----+ ++-+- +---+ +++-- +--++ +- 951517. 0.186 0.240 0.164 0.921 0.575 ----+ +---- --++- +-+++ -++-- +- 2072985. 0.190 0.373 0.239 0.988 0.762 -+--+ +--++ ----- -+--- +++-+ +- 74721. 0.244 -0.053 0.352 0.856 0.353 +-+-+ -+--- --++- -++-- --+-+ ++ 113441. 0.243 0.045 -0.091 0.761 0.428 -++-+ ----- +-+-- --+-+ +---+ -+ 1231117. 0.200 0.357 0.375 0.946 0.749 +-+-+ ++--- +--+- -+-+- -+-++ -- 797529. 0.212 0.063 -0.245 0.908 0.412 ++--- +--++ -+-+- +++-+ +-++- -+ 1672841. 0.204 0.196 0.740 0.924 0.540 +---- -+-+- +-+-+ --++- ++++- ++ 742597. 0.205 -0.017 -0.003 0.914 0.340 ++--- +--++ -+-+- +++-- +-+++ -+ 923369. 0.193 0.269 0.631 0.985 0.620 --+-- +---- ++--- +-+-- ---+- ++ 1569809. 0.191 0.180 0.061 0.911 0.509 ---++ +---- ---+- +-+++ -++-- ++ 417449. 0.193 0.210 0.266 0.959 0.546 +---+ -+--+ +---+ -+-+- -+--+ -+ 853805. 0.245 0.136 0.506 0.847 0.515 +---+ +---+ +-++- ---+- --+++ ++ 1923945. 0.190 0.238 0.422 0.975 0.577 --+-- +---- +++-- +++-- ----- ++ 373605. 0.182 0.391 0.285 0.979 0.783 +---- +--++ ++-+- ---++ ++++- +- 1746025. 0.213 0.193 0.182 0.943 0.547 +++-- +--+- ++-+- +-+-+ ++-+- +- 388825. 0.167 0.239 0.390 1.003 0.556 +-+-- -+--+ +--++ -+++- -++-+ -+ 76117. 0.136 -0.639 0.361 0.982 0.136* +++-- ---++ ----+ +-+++ ++-+- ++ 263065. 0.167 -0.301 0.562 1.031 0.173 --+-+ ---++ ----+ +-+++ ++++- ++ 285169. 0.161 -0.284 0.562 1.029 0.171 --+-+ ---++ ----+ +-+++ ++++- ++ 1421065. 0.146 -0.406 0.561 1.000 0.146 --+-- ---++ ----+ +-+++ ++++- ++ 72605. 0.174 -0.296 0.361 0.914 0.182 +++-- ---++ ----+ +-+++ ++-+- ++ 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 1 0.140 - 0.160 1 0.160 - 0.180 7 0.180 - 0.200 1 0.200 - 0.220 0 0.220 - 0.240 3 0.240 - 0.260 5 0.260 - 0.280 5 0.280 - 0.300 10 0.300 - 0.320 11 0.320 - 0.340 14 0.340 - 0.360 10 0.360 - 0.380 21 0.380 - 0.400 12 0.400 - 0.420 12 0.420 - 0.440 12 0.440 - 0.460 8 0.460 - 0.480 5 0.480 - 0.500 16 0.500 - 0.520 14 0.520 - 0.540 11 0.540 - 0.560 6 0.560 - 0.580 4 0.580 - 0.600 6 0.600 - 9.999 61 256. Phase sets refined - best is code 76117. with CFOM = 0.1357 3.2 seconds CPU time Tangent expanded to 1098 out of 1098 E greater than 1.200 Highest memory used = 4543 / 11035 0.1 seconds CPU time FMAP and GRID set by program FMAP 8 3 35 GRID -0.781 -2 -2 0.781 2 2 E-Fourier for 01ESP002 IN P212121 Maximum = 390.31, minimum = -77.46 highest memory used = 9059 / 17964 0.1 seconds CPU time Heavy-atom assignments: x y z s.o.f. Height CL1 0.8047 0.5861 0.2398 1.0000 390.3 Peak list optimization RE = 0.185 for 43 surviving atoms and 1098 E-values Highest memory used = 1874 / 9882 0.1 seconds CPU time E-Fourier for 01ESP002 IN P212121 Maximum = 302.90, minimum = -60.97 highest memory used = 9067 / 17964 0.1 seconds CPU time Peak list optimization RE = 0.171 for 43 surviving atoms and 1098 E-values Highest memory used = 1882 / 9882 0.1 seconds CPU time E-Fourier for 01ESP002 IN P212121 Maximum = 296.88, minimum = -36.90 highest memory used = 9067 / 17964 0.0 seconds CPU time Molecule 1 scale 0.469 inches = 1.191 cm per Angstrom 55 40 37 36 50 3 53 47 29 9 45 30 36 52 58 CL1 22 20 11 51 47 21 26 41 5 44 57 18 54 35 2 24 39 59 4 33 28 23 49 46 25 1*9 1*7 8 13 32 56 7 48 1 31 6 38 16 39 44 14 17 12 42 34 50 53 Atom Peak x y z SOF Height Distances and Angles CL1 0. 0.8047 0.5861 0.2398 1.000 1.41 0 21 2.711 0 22 1.778 25.7 0 30 2.630 52.5 26.9 0 44 2.023 118.5 125.4 124.3 0 47 1.832 133.7 126.4 111.6 106.0 0 51 1.090 137.7 127.3 109.7 33.3 87.3 0 52 1.956 22.6 28.7 49.9 140.9 111.4 155.8 0 53 2.352 91.4 67.5 43.5 126.9 70.2 95.0 78.0 7 58 2.607 139.7 163.9 164.9 62.1 54.1 67.5 135.8 121.3 1 140. 0.7518 -0.0416 0.3177 1.000 0.78 0 16 1.291 0 25 1.286 116.4 0 46 1.628 156.1 80.8 0 56 1.103 73.2 53.5 129.7 2 137. 0.8876 -0.0411 0.4810 1.000 1.96 0 24 1.347 0 27 1.410 120.1 3 134. 1.2221 0.3985 0.3856 1.000 1.25 0 29 1.399 0 37 1.449 115.7 4 128. 0.6024 0.0906 0.4933 1.000 3.12 0 13 1.460 0 28 1.327 118.7 0 49 1.659 125.4 76.7 0 59 1.155 107.3 120.2 45.0 5 128. 0.9994 0.1462 0.3717 1.000 1.10 0 11 1.391 0 18 1.317 116.6 0 57 1.218 103.7 60.9 6 127. 0.5775 -0.0387 0.4058 1.000 2.06 0 19 1.409 0 31 1.330 117.8 7 124. 0.8448 -0.1888 0.3894 1.000 0.86 0 15 1.479 0 32 1.296 118.3 0 56 1.998 61.3 109.4 8 122. 0.5582 0.1423 0.3816 1.000 2.31 0 31 1.211 0 54 1.853 114.5 9 121. 1.2214 0.2282 0.4211 1.000 1.18 0 29 1.201 10 117. 0.4208 0.0933 0.5433 1.000 4.06 0 28 1.184 11 113. 1.0553 0.2583 0.3657 1.000 1.16 0 5 1.391 0 20 1.459 125.5 0 29 1.337 111.9 122.6 12 112. 0.5151 -0.2742 0.2961 1.000 0.63 0 17 1.308 0 42 1.505 115.4 13 109. 0.6162 -0.0356 0.4943 1.000 2.79 0 4 1.460 0 27 1.484 110.3 0 48 1.882 142.6 33.6 14 106. 0.5682 -0.1219 0.2553 1.000 0.48 0 17 1.185 15 106. 0.8519 -0.0608 0.3913 1.000 1.16 0 7 1.479 0 19 1.551 110.0 0 25 1.442 109.9 112.9 0 56 1.828 73.5 129.3 36.5 16 106. 0.6831 -0.1413 0.3192 1.000 0.73 0 1 1.291 0 17 1.401 119.9 0 56 1.436 47.3 154.1 17 101. 0.5824 -0.1756 0.2867 1.000 0.61 0 12 1.308 0 14 1.185 127.2 0 16 1.401 110.0 122.7 18 101. 0.9073 0.1039 0.3423 1.000 0.96 0 5 1.317 0 25 1.503 117.5 0 46 1.603 158.9 75.6 0 57 1.288 55.7 100.2 107.5 19 99. 0.7274 -0.0144 0.4226 1.000 1.89 0 6 1.409 0 15 1.551 107.6 0 27 1.519 108.1 111.4 20 95. 0.9998 0.3390 0.3337 1.000 1.20 0 11 1.459 0 26 1.404 115.9 0 36 1.297 122.9 121.0 0 45 1.152 113.8 106.5 53.6 21 94. 0.7826 0.4429 0.3069 1.000 1.75 0 CL1 2.711 0 22 1.350 34.8 0 26 1.347 154.5 119.7 0 52 1.178 39.7 43.0 127.6 22 94. 0.8787 0.4843 0.2767 1.000 1.32 0 CL1 1.778 0 21 1.350 119.6 0 30 1.318 115.6 124.9 0 52 0.941 86.2 58.7 127.2 23 94. 0.9633 -0.2254 0.4920 1.000 1.42 0 24 1.218 24 94. 0.9929 -0.1221 0.4928 1.000 1.60 0 2 1.347 0 23 1.218 122.4 0 41 1.442 113.4 123.5 25 94. 0.8344 -0.0130 0.3498 1.000 0.94 0 1 1.286 0 15 1.442 133.7 0 18 1.503 109.1 116.6 0 46 1.906 57.5 155.3 54.5 0 56 1.088 54.6 91.5 140.5 108.9 26 93. 0.8389 0.3671 0.3353 1.000 1.69 0 20 1.404 0 21 1.347 118.1 27 92. 0.7401 -0.0748 0.4647 1.000 2.10 0 2 1.410 0 13 1.484 108.2 0 19 1.519 105.2 111.9 0 48 1.046 119.7 94.5 116.8 28 91. 0.4914 0.1408 0.5163 1.000 3.74 0 4 1.327 0 10 1.184 124.0 0 35 1.477 116.9 119.0 0 49 1.871 59.7 144.1 72.9 29 88. 1.1691 0.2855 0.3929 1.000 1.19 0 3 1.399 0 9 1.201 121.3 0 11 1.337 110.0 128.7 30 87. 1.0276 0.4548 0.2719 1.000 0.83 0 CL1 2.630 0 22 1.318 37.6 0 36 1.452 152.3 114.9 0 45 2.014 126.5 95.1 32.5 0 52 2.030 47.5 21.7 106.3 79.5 0 53 1.865 60.3 93.3 139.0 121.8 88.8 31 86. 0.5041 0.0456 0.3851 1.000 2.25 0 6 1.330 0 8 1.211 122.8 0 39 1.541 111.4 125.8 32 86. 0.9760 -0.2462 0.3899 1.000 0.39 0 7 1.296 0 33 1.214 123.6 0 38 1.507 108.4 127.1 33 85. 1.1033 -0.2023 0.3969 1.000 0.23 0 32 1.214 34 85. 0.2339 -0.2684 0.2815 1.000 1.24 0 42 1.494 0 50 1.880 115.9 35 82. 0.4647 0.2659 0.5093 1.000 4.04 0 28 1.477 0 49 2.014 62.6 36 82. 1.0888 0.3770 0.3037 1.000 0.78 0 20 1.297 0 30 1.452 121.2 0 45 1.111 56.5 102.8 4 47 2.032 104.6 98.8 156.8 37 78. 1.3646 0.4316 0.4076 1.000 1.17 0 3 1.449 0 40 1.575 108.4 38 75. 0.9381 -0.3738 0.3886 1.000 0.17 0 32 1.507 39 71. 0.3451 0.0039 0.3673 1.000 2.40 0 31 1.541 3 44 1.834 112.1 40 70. 1.4236 0.5507 0.3893 1.000 1.13 0 37 1.575 0 55 0.893 128.5 41 68. 1.1486 -0.0761 0.4998 1.000 1.38 0 24 1.442 42 68. 0.3886 -0.3135 0.2663 1.000 0.59 0 12 1.505 0 34 1.494 108.4 44 33. 0.6811 0.5462 0.1876 1.000 1.15 0 CL1 2.023 0 51 1.263 28.3 2 39 1.834 155.7 128.3 45 32. 1.0672 0.4257 0.3332 1.000 1.23 0 20 1.152 0 30 2.014 94.4 0 36 1.111 69.9 44.7 46 32. 0.7647 0.0974 0.3094 1.000 1.00 0 1 1.628 0 18 1.603 89.5 0 25 1.906 41.7 49.8 47 31. 0.8713 0.7359 0.2329 1.000 1.53 0 CL1 1.832 1 36 2.032 151.2 48 31. 0.7065 -0.1620 0.4658 1.000 1.99 0 13 1.882 0 27 1.046 51.8 49 30. 0.4999 0.1660 0.4584 1.000 3.24 0 4 1.659 0 28 1.871 43.7 0 35 2.014 80.6 44.5 0 59 1.173 44.1 86.9 112.2 50 29. 0.0973 -0.3787 0.3051 1.000 1.54 0 34 1.880 6 53 1.902 76.1 51 29. 0.8056 0.5786 0.2058 1.000 1.07 0 CL1 1.090 0 44 1.263 118.5 52 29. 0.8363 0.5333 0.2974 1.000 1.74 0 CL1 1.956 0 21 1.178 117.7 0 22 0.941 65.1 78.3 0 30 2.030 82.6 91.0 31.2 53 29. 1.0803 0.5951 0.2465 1.000 0.79 0 CL1 2.352 0 30 1.865 76.2 5 50 1.902 99.9 74.2 54 29. 0.7115 0.1790 0.4207 1.000 2.37 0 8 1.853 0 57 1.934 84.9 0 59 1.593 95.1 146.6 55 28. 1.5191 0.5827 0.3912 1.000 0.98 0 40 0.893 56 28. 0.8290 -0.0992 0.3361 1.000 0.62 0 1 1.103 0 7 1.998 143.7 0 15 1.828 115.5 45.2 0 16 1.436 59.4 101.7 122.4 0 25 1.088 71.9 97.2 52.0 119.8 57 28. 0.8573 0.1589 0.3748 1.000 1.52 0 5 1.218 0 18 1.288 63.3 0 54 1.934 135.1 151.8 59 27. 0.6229 0.1196 0.4591 1.000 2.82 0 4 1.155 0 49 1.173 90.9 0 54 1.593 157.4 102.1 Atom Code x y z Height Symmetry transformation 36 1 0.9112 0.8770 0.1963 1.42 2.0000-X 0.5000+Y 0.5000-Z 39 2 0.6549 0.5039 0.1327 0.60 1.0000-X 0.5000+Y 0.5000-Z 44 3 0.3189 0.0462 0.3124 2.05 1.0000-X -0.5000+Y 0.5000-Z 47 4 1.1287 0.2359 0.2671 0.00 2.0000-X -0.5000+Y 0.5000-Z 50 5 1.0973 0.6213 0.3051 1.35 1.0000+X 1.0000+Y 0.0000+Z 53 6 0.0803 -0.4049 0.2465 0.98 -1.0000+X -1.0000+Y 0.0000+Z 58 7 0.6465 0.7517 0.2035 1.87 0.0000+X 0.0000+Y 0.0000+Z Molecule 2 Atom Peak x y z SOF Height Distances and Angles 43 36. 0.1249 0.0765 0.0247 1.000 Molecule 3 Atom Peak x y z SOF Height Distances and Angles 58 27. 0.6465 0.7517 0.2035 1.000 0.0 seconds CPU time +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 15:35:38 Total CPU time: 3.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++