+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXS-97 - CRYSTAL STRUCTURE SOLUTION - MSDOS 32-BIT VERSION + + Copyright(C) George M. Sheldrick 1986-97 Release 97-1 + + zhu3 started at 17:15:20 on 01-May-1998 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL Zhu3 P21/m Z=2 OVERLAP delta 2theta = 0.03 CELL 1.5406 7.662 9.626 7.072 90. 106.20 90. ZERR 2 0.001 0.001 0.001 0 0.01 0 LATT 1 SYMM -X,0.5+Y,-Z SFAC CO 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 = 71.1692 1.0118 -2.3653 3.61443 0.0 0.6 58.93 SFAC O 4.758 7.831 3.637 30.05 0. 0. 0. 0. 1.594 = 0.047 0.032 0.0 1.35 15.9994 SFAC N C H UNIT 2 14 12 2 30 V = 500.88 At vol = 16.7 F(000) = 320.0 mu = 0.45 mm-1 Max single Patterson vector = 205.3 cell wt = 564.23 rho = 1.871 TREF 500 HKLF 3 ** WARNING - IT WOULD BE BETTER TO INPUT F-SQUARED THAN F SO ** THAT ZERO AND NEGATIVE INTENSITIES ARE TREATED CORRECTLY 434 Reflections read, of which 0 rejected Maximum h, k, l and 2-Theta = 8. 10. 7. 119.17 434 Unique reflections, of which 434 observed R(int) = 0.0000 R(sigma) = 0.0478 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. 8. 19. 33. 25. 32. 22. 31. 46. 46. 61. 99. 6. N(measured) 6. 8. 19. 33. 25. 32. 22. 31. 46. 46. 61. 99. 6. N(theory) 6. 8. 23. 39. 44. 51. 43. 48. 66. 100. 131. 212. 317. Two-theta 0.0 17.7 25.4 35.9 45.3 53.9 61.8 66.8 72.7 79.9 88.9 100.8 117.7 148.7 Highest memory for sort/merge = 1627 / 2170 Observed E .GT. 1.200 1.300 1.400 1.500 1.600 1.700 1.800 1.900 2.000 2.100 Number 127 88 65 56 40 28 20 9 3 3 Centric Acentric 0kl h0l hk0 Rest Mean Abs(E*E-1) 0.968 0.736 0.497 0.580 0.707 0.648 0.2 seconds elapsed time SUMMARY OF PARAMETERS FOR Zhu3 P21/m Z=2 OVERLAP delta 2theta = 0.03 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 10 nf 16 s+ 0.800 s- 0.200 wr 0.200 PHAN steps 10 cool 0.900 Boltz 0.400 ns 117 mtpr 40 mnqr 10 TREF np 500. nE 175 kapscal 0.900 ntan 2 wn -0.950 FMAP code 8 PLAN npeaks -13 del1 0.500 del2 1.500 MORE verbosity 1 TIME t 9999999. 90 Reflections and 484. unique TPR for phase annealing 90 Phases refined using 484. unique TPR 90 Reflections and 484. unique TPR for R(alpha) 0.1 seconds elapsed time 8 Unique negative quartets found, 8 used for phase refinement 0.0 seconds elapsed time Highest memory used to derive phase relations = 1092 / 3531 ONE-PHASE SEMINVARIANTS h k l E P+ Phi 0 2 0 1.683 0.01 2 4 2 1.810 0.43 0 2 2 1.989 0.40 0 4 0 1.316 1.00 6 4 0 1.870 0.77 4 4 2 1.931 0.47 2 6 2 1.582 0.47 0 8 0 1.250 1.00 2 0 0 1.288 0.28 2 2 2 1.322 0.61 0 0 2 1.345 0.86 -2 6 2 1.323 2 2 4 1.326 0.49 -2 2 6 1.613 0.39 4 2 4 1.270 0.46 0 2 6 1.509 0.42 -4 4 6 1.263 0.47 Expected value of Sigma-1 = 0.840 Following phases held constant with unit weights for the initial 4 weighted tangent cycles (before phase annealing): h k l E Phase/Comment 0 2 0 1.683 180 sigma-1 = 0.012 1 5 2 1.931 random phase 0 4 0 1.316 0 sigma-1 = 0.999 -2 1 2 1.270 random phase 4 4 2 1.931 random phase -3 2 2 1.558 random phase -5 1 3 1.594 random phase 0 8 0 1.250 0 sigma-1 = 0.996 2 0 0 1.288 random phase 0 0 2 1.345 0 sigma-1 = 0.857 3 4 1 1.343 random phase 2 1 6 1.509 random phase -2 6 2 1.323 random phase -4 4 6 1.263 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 8 Unique NQR employed in phase annealing 125 Parallel refinements, highest memory = 820 / 25677 0.1 seconds elapsed time STRUCTURE SOLUTION for Zhu3 P21/m Z=2 OVERLAP delta 2theta = 0.03 Phase annealing cycle: 1 Beta = 0.12197 Ralpha 0.137 0.252 0.086 0.081 0.118 0.569 0.069 0.081 0.061 0.120 0.085 0.064 0.063 0.099 0.463 0.061 0.055 0.089 0.083 0.069 Nqual -0.481 0.088 0.061-0.082 0.207-0.305 0.102-0.378-0.106-0.649-0.164-0.291 0.217 0.147 0.106-0.453-0.160 0.026-0.322 0.191 Mabs 0.928 0.793 1.089 1.015 1.038 0.609 1.232 1.034 1.208 0.938 1.024 1.181 1.205 1.028 0.648 1.189 1.067 1.063 1.050 1.194 Phase annealing cycle: 2 Beta = 0.13552 Ralpha 0.112 0.163 0.078 0.079 0.105 0.474 0.080 0.086 0.077 0.120 0.086 0.080 0.080 0.107 0.194 0.080 0.081 0.096 0.097 0.079 Nqual -0.487-0.161-0.599 0.299-0.090-0.673 0.292-0.022-0.219-0.724-0.066 0.284 0.167-0.180-0.121 0.284 0.291-0.064-0.923 0.299 Mabs 1.018 0.911 1.173 1.316 1.152 0.659 1.323 1.166 1.310 0.974 1.180 1.322 1.318 1.171 0.870 1.316 1.329 1.199 1.151 1.315 Phase annealing cycle: 3 Beta = 0.15057 Ralpha 0.111 0.132 0.089 0.080 0.104 0.390 0.080 0.091 0.079 0.129 0.086 0.078 0.081 0.090 0.168 0.079 0.080 0.104 0.088 0.079 Nqual 0.133-0.641-0.331 0.292-0.409-0.751 0.293-0.616 0.293-0.868-0.255-0.219 0.291-0.378-0.412 0.300 0.293 0.207-0.822 0.299 Mabs 1.018 0.965 1.196 1.323 1.176 0.687 1.334 1.187 1.328 0.984 1.150 1.317 1.329 1.228 0.893 1.321 1.334 1.180 1.176 1.321 Phase annealing cycle: 4 Beta = 0.16730 Ralpha 0.115 0.113 0.088 0.080 0.095 0.349 0.080 0.082 0.080 0.126 0.088 0.080 0.080 0.080 0.155 0.080 0.079 0.086 0.083 0.079 Nqual -0.119-0.530-0.430 0.293-0.540-0.869 0.293-0.439 0.293-0.717-0.581 0.293 0.293 0.293-0.394 0.293 0.293-0.340-0.334 0.293 Mabs 1.014 1.014 1.196 1.334 1.200 0.708 1.334 1.183 1.334 0.981 1.199 1.334 1.334 1.334 0.923 1.334 1.328 1.204 1.191 1.328 Phase annealing cycle: 5 Beta = 0.18589 Ralpha 0.108 0.110 0.085 0.080 0.095 0.352 0.080 0.086 0.080 0.131 0.082 0.081 0.079 0.080 0.156 0.080 0.081 0.095 0.083 0.080 Nqual 0.117-0.480-0.300 0.293-0.540-0.935 0.293-0.727 0.293 0.120-0.407 0.291 0.293 0.293-0.376 0.293 0.291-0.439-0.422 0.293 Mabs 1.023 1.028 1.193 1.334 1.200 0.715 1.334 1.177 1.334 0.984 1.194 1.329 1.328 1.334 0.921 1.334 1.329 1.198 1.192 1.334 Phase annealing cycle: 6 Beta = 0.20655 Ralpha 0.112 0.112 0.088 0.081 0.095 0.349 0.080 0.088 0.080 0.125 0.089 0.080 0.080 0.081 0.160 0.080 0.080 0.102 0.088 0.080 Nqual -0.494-0.494-0.430 0.291-0.540-0.934 0.293-0.629 0.293 0.131-0.328 0.293 0.293 0.291-0.369 0.293 0.293-0.515-0.432 0.293 Mabs 1.028 1.028 1.194 1.329 1.200 0.713 1.334 1.185 1.334 0.986 1.197 1.334 1.334 1.329 0.915 1.334 1.334 1.179 1.196 1.334 Phase annealing cycle: 7 Beta = 0.22950 Ralpha 0.111 0.109 0.090 0.080 0.098 0.351 0.080 0.090 0.080 0.125 0.077 0.081 0.080 0.081 0.146 0.080 0.080 0.089 0.081 0.080 Nqual -0.477-0.468-0.306 0.293-0.526-0.902 0.293-0.739 0.293 0.094-0.576 0.291 0.293 0.291-0.386 0.293 0.293-0.318-0.417 0.293 Mabs 1.030 1.029 1.197 1.334 1.189 0.712 1.334 1.172 1.334 0.988 1.186 1.329 1.334 1.329 0.926 1.334 1.334 1.196 1.195 1.334 Phase annealing cycle: 8 Beta = 0.25500 Ralpha 0.113 0.115 0.084 0.080 0.087 0.299 0.080 0.091 0.080 0.126 0.087 0.080 0.080 0.080 0.148 0.080 0.080 0.084 0.083 0.080 Nqual -0.272-0.302-0.529 0.293-0.452-0.565 0.293-0.501 0.293-0.421-0.344 0.293 0.293 0.293-0.400 0.293 0.293-0.300-0.412 0.293 Mabs 1.027 1.026 1.189 1.334 1.206 0.739 1.334 1.193 1.334 0.991 1.209 1.334 1.334 1.334 0.924 1.334 1.334 1.194 1.191 1.334 Phase annealing cycle: 9 Beta = 0.28333 Ralpha 0.114 0.109 0.083 0.080 0.093 0.314 0.080 0.090 0.080 0.132 0.100 0.080 0.080 0.080 0.152 0.080 0.080 0.083 0.089 0.080 Nqual -0.287-0.468-0.414 0.293-0.538-0.711 0.293-0.309 0.293-0.556-0.530 0.293 0.293 0.293-0.444 0.293 0.293-0.414-0.322 0.293 Mabs 1.026 1.029 1.192 1.334 1.196 0.733 1.334 1.195 1.334 0.977 1.194 1.334 1.334 1.334 0.915 1.334 1.334 1.194 1.198 1.334 Phase annealing cycle: 10 Beta = 0.31481 Ralpha 0.112 0.113 0.088 0.080 0.096 0.313 0.080 0.089 0.080 0.128 0.094 0.080 0.080 0.080 0.142 0.080 0.080 0.083 0.085 0.080 Nqual -0.494-0.272-0.433 0.293-0.538-0.600 0.293-0.331 0.293-0.733-0.443 0.293 0.293 0.293-0.539 0.293 0.293-0.404-0.447 0.293 Mabs 1.028 1.027 1.198 1.334 1.198 0.734 1.334 1.197 1.334 0.984 1.199 1.334 1.334 1.334 0.917 1.334 1.334 1.191 1.204 1.334 Phase refinement cycle: 1 Ralpha 0.110 0.115 0.076 0.080 0.095 0.299 0.080 0.083 0.080 0.132 0.095 0.080 0.080 0.080 0.159 0.080 0.080 0.089 0.095 0.080 Nqual -0.480-0.302-0.590 0.293-0.540-0.483 0.293-0.422 0.293-0.651-0.450 0.293 0.293 0.293-0.414 0.293 0.293-0.327-0.450 0.293 Mabs 1.028 1.026 1.186 1.334 1.200 0.738 1.334 1.192 1.334 0.986 1.200 1.334 1.334 1.334 0.919 1.334 1.334 1.194 1.200 1.334 Try Ralpha Nqual Sigma-1 M(abs) CFOM Seminvariants 1913623. 0.112 -0.494 0.613 1.028 0.319 --++- +++++ -+--- -- 1179507. 0.112 -0.494 0.613 1.028 0.319 --++- +++++ -+--- -- 1703231. 0.088 -0.440 0.976 1.195 0.348 ---++ -++-+ +-+-- -+ 127547. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 637735. 0.095 -0.540 0.950 1.200 0.263 ---++ -++-+ +-+-- ++ 1091523. 0.302 -0.506 0.812 0.738 0.500 -+-+- +-+-- +++-- -+ 1263311. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 25099. 0.088 -0.440 0.976 1.195 0.348 ---++ -++-+ +-+-- -+ 125495. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 627475. 0.128 -0.882 0.967 0.984 0.133* ---++ +++-+ +++-- -+ 1040223. 0.095 -0.540 0.950 1.200 0.263 ---++ -++-+ +-+-- ++ 1006811. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 839751. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 4451. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 22255. 0.159 -0.414 0.620 0.919 0.446 -+++- --+-- --+-- +- 111275. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 556375. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 684723. 0.088 -0.440 0.976 1.195 0.348 ---++ -++-+ +-+-- -+ 1326463. 0.095 -0.540 0.950 1.200 0.263 ---++ -++-+ +-+-- ++ 340859. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1704295. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 132867. 0.095 -0.540 0.950 1.200 0.263 ---++ -++-+ +-+-- ++ 664335. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1224523. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1928311. 0.089 0.276 0.937 1.148 1.593 ---++ -++-+ +-+++ -- 1252947. 0.095 -0.540 0.950 1.200 0.263 ---++ -++-+ +-+-- ++ 2070431. 0.152 -0.077 0.733 0.896 0.914 -+-+- +-++- +++-- -+ 1963547. 0.095 -0.540 0.950 1.200 0.263 ---++ -++-+ +-+-- ++ 1429127. 0.114 -0.583 0.835 1.038 0.249 --+++ -++++ +-+-- ++ 1925867. 0.091 0.160 0.831 1.145 1.323 ---++ -++++ +-+++ +- 1240727. 0.091 0.160 0.831 1.145 1.323 ---++ -++++ +-+++ +- 9159. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 228975. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1209243. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 134291. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 418043. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1144875. 0.089 0.276 0.937 1.148 1.593 ---++ -++-+ +-+++ -- 1839443. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 808607. 0.095 -0.540 0.950 1.200 0.263 ---++ -++-+ +-+-- ++ 1230027. 0.095 -0.540 0.950 1.200 0.263 ---++ -++-+ +-+-- ++ 160431. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 503039. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 865719. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 661279. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 895491. 0.087 -0.455 0.950 1.208 0.332 ---++ -++-+ +-+-- ++ 1690939. 0.088 -0.440 0.976 1.195 0.348 ---++ -++-+ +-+-- -+ 1656939. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 2068275. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 214439. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 783447. 0.095 -0.540 0.950 1.200 0.263 ---++ -++-+ +-+-- ++ 1072195. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1639051. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1518527. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 330435. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1848803. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1166671. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1458487. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1577587. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 996699. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1576227. 0.095 -0.540 0.950 1.200 0.263 ---++ -++-+ +-+-- ++ 1834411. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 479963. 0.095 -0.540 0.950 1.200 0.263 ---++ -++-+ +-+-- ++ 465507. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 372751. 0.095 -0.450 0.950 1.200 0.345 ---++ -++-+ +-+-- ++ 1239807. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1274515. 0.088 -0.440 0.976 1.195 0.348 ---++ -++-+ +-+-- -+ 913411. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 405595. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1379495. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 84139. 0.095 -0.540 0.950 1.200 0.263 ---++ -++-+ +-+-- ++ 367727. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1863107. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 440331. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 81119. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1863755. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 456531. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1383039. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 917735. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1381151. 0.088 -0.440 0.976 1.195 0.348 ---++ -++-+ +-+-- -+ 1731207. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 566675. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 299047. 0.088 -0.440 0.976 1.195 0.348 ---++ -++-+ +-+-- -+ 761723. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 114355. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1600583. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1918519. 0.087 -0.455 0.950 1.208 0.332 ---++ -++-+ +-+-- ++ 1914071. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1184719. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 22667. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1687495. 0.088 -0.440 0.976 1.195 0.348 ---++ -++-+ +-+-- -+ 1711459. 0.095 -0.540 0.950 1.200 0.263 ---++ -++-+ +-+-- ++ 1554183. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1047015. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1785563. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1532939. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 359855. 0.095 -0.540 0.950 1.200 0.263 ---++ -++-+ +-+-- ++ 980211. 0.089 0.276 0.937 1.148 1.593 ---++ -++-+ +-+++ -- 1460055. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 539207. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1799275. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1991975. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 2036147. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 387139. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1574191. 0.095 -0.540 0.950 1.200 0.263 ---++ -++-+ +-+-- ++ 1479095. 0.095 -0.540 0.950 1.200 0.263 ---++ -++-+ +-+-- ++ 1335719. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1056867. 0.095 -0.540 0.950 1.200 0.263 ---++ -++-+ +-+-- ++ 178443. 0.095 -0.540 0.950 1.200 0.263 ---++ -++-+ +-+-- ++ 810871. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1224243. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 2071311. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 49067. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 250015. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1439823. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1757215. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1156331. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1955951. 0.088 -0.440 0.976 1.195 0.348 ---++ -++-+ +-+-- -+ 886271. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1798547. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1587351. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 299295. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 59859. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 134011. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1016115. 0.087 -0.455 0.950 1.208 0.332 ---++ -++-+ +-+-- ++ 2092859. 0.080 0.293 0.952 1.334 1.625 ---++ +++-+ +++-- +- 1049799. 0.128 -0.733 0.967 0.984 0.175 ---++ +++-+ +++-- -+ 486475. 0.095 -0.540 0.950 1.200 0.263 ---++ -++-+ +-+-- ++ 1136791. 0.128 -0.882 0.967 0.984 0.133 ---++ +++-+ +++-- -+ 1993539. 0.128 -0.882 0.967 0.984 0.133 ---++ +++-+ +++-- -+ 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 3 0.140 - 0.160 0 0.160 - 0.180 1 0.180 - 0.200 0 0.200 - 0.220 0 0.220 - 0.240 0 0.240 - 0.260 2 0.260 - 0.280 68 0.280 - 0.300 0 0.300 - 0.320 2 0.320 - 0.340 7 0.340 - 0.360 66 0.360 - 0.380 0 0.380 - 0.400 0 0.400 - 0.420 0 0.420 - 0.440 4 0.440 - 0.460 1 0.460 - 0.480 0 0.480 - 0.500 1 0.500 - 0.520 0 0.520 - 0.540 0 0.540 - 0.560 0 0.560 - 0.580 2 0.580 - 0.600 0 0.600 - 9.999 343 500. Phase sets refined - best is code 627475. with CFOM = 0.1326 2.8 seconds elapsed time Tangent expanded to 127 out of 127 E greater than 1.200 Highest memory used = 639 / 739 0.1 seconds elapsed time FMAP and GRID set by program FMAP 8 2 12 GRID -2.778 -2 -2 2.778 2 2 E-Fourier for Zhu3 P21/m Z=2 OVERLAP delta 2theta = 0.03 Maximum = 490.09, minimum = -176.07 highest memory used = 8671 / 1701 0.1 seconds elapsed time Heavy-atom assignments: x y z s.o.f. Height CO1 0.0105 0.2500 0.3410 0.5000 490.1 CO2 0.6666 0.2500 0.5661 0.5000 461.8 CO3 0.4001 0.2500 0.8038 0.5000 348.3 CO4 0.7357 0.2500 0.4552 0.5000 256.0 O5 0.7333 0.2500 0.0134 0.5000 181.4 O6 0.6583 0.2500 0.7410 0.5000 176.9 O7 0.4350 0.1750 0.4838 1.0000 161.0 O8 0.0839 0.0998 0.1748 1.0000 147.9 O9 0.1420 0.2500 0.9781 0.5000 142.4 O10 0.3538 0.1076 0.0340 1.0000 137.8 Peak list optimization RE = 0.484 for 12 surviving atoms and 127 E-values Highest memory used = 1486 / 1143 0.0 seconds elapsed time E-Fourier for Zhu3 P21/m Z=2 OVERLAP delta 2theta = 0.03 Maximum = 450.75, minimum = -203.80 highest memory used = 8751 / 1701 0.1 seconds elapsed time Peak list optimization RE = 0.481 for 17 surviving atoms and 127 E-values Highest memory used = 1566 / 1143 0.1 seconds elapsed time E-Fourier for Zhu3 P21/m Z=2 OVERLAP delta 2theta = 0.03 Maximum = 422.37, minimum = -183.36 highest memory used = 8751 / 1701 0.1 seconds elapsed time Molecule 1 scale 0.721 inches = 1.831 cm per Angstrom O9 O8 O10 O10 10 8 13 O7 O7 1 CO4 CO2 7 7 3 O9 5 CO3 6 6 4 4 12 O6 O8 O10 O10 9 2 O10 O8 4 O5 12 12 8 11 11 O7 O9 O8 O8 CO4 O10 O10 CO1 3 3 5 6 6 10 10 8 9 13 O7 O7 1 Atom Peak x y z SOF Height Distances and Angles CO1 0. 0.0105 0.2500 0.3410 0.500 1.55 0 O8 2.039 0 3 1.457 73.5 0 5 1.512 132.1 59.6 0 10 1.296 64.9 71.7 105.8 0 13 1.625 104.3 92.3 87.7 40.8 9 O8 2.039 90.3 159.3 132.1 113.4 104.3 20 3 1.457 159.3 118.7 59.6 133.1 92.3 73.5 32 10 1.296 113.4 133.1 105.8 70.8 40.8 64.9 71.7 CO2 0. -0.3334 0.2500 -0.4339 0.500 1.88 0 CO4 1.061 0 O6 1.257 154.2 0 O7 1.853 113.5 90.1 4 O7 1.853 113.5 90.1 45.9 CO3 0. -0.5999 0.2500 -0.1962 0.500 1.25 0 O6 2.145 0 O10 2.231 119.6 0 1 1.149 71.7 137.6 0 2 1.256 79.1 59.3 150.8 0 7 1.527 70.1 76.2 70.1 100.2 15 O10 2.231 119.6 75.8 137.6 59.3 151.3 27 7 1.527 70.1 151.3 70.1 100.2 130.3 76.2 CO4 0. -0.2643 0.2500 -0.5448 0.500 2.09 0 CO2 1.061 0 O6 2.259 14.0 0 6 1.614 108.8 97.7 23 5 1.073 131.7 117.6 40.0 25 6 1.614 108.8 97.7 72.6 40.0 O5 0. -0.2667 0.2500 0.0134 0.500 1.50 0 O6 1.850 0 O8 2.983 112.5 0 2 1.682 79.9 147.3 0 11 1.534 144.5 56.4 95.4 0 12 1.992 101.5 79.0 68.7 45.7 9 O8 2.983 112.5 58.0 147.3 90.4 132.4 33 11 1.534 144.5 90.4 95.4 70.7 109.6 56.4 35 12 1.992 101.5 132.4 68.7 109.6 126.5 79.0 45.7 O6 0. -0.3417 0.2500 -0.2590 0.500 1.68 0 CO2 1.257 0 CO3 2.145 120.5 0 CO4 2.259 11.8 132.3 0 O5 1.850 159.9 79.7 148.1 0 O7 2.241 55.8 68.2 66.8 142.2 0 1 2.092 89.0 31.5 100.8 111.1 39.5 0 2 2.272 153.3 32.9 165.1 46.8 99.3 64.3 0 4 2.263 108.8 61.3 113.0 79.8 67.7 68.8 63.0 0 7 2.169 103.3 41.5 112.1 92.1 50.6 43.1 57.6 25.7 4 O7 2.241 55.8 68.2 66.8 142.2 37.6 39.5 99.3 100.6 77.1 22 4 2.263 108.8 61.3 113.0 79.8 100.6 68.8 63.0 121.5 102.3 67.7 27 7 2.169 103.3 41.5 112.1 92.1 77.1 43.1 57.6 102.3 79.4 50.6 25.7 O7 0. -0.5650 0.1750 -0.5162 1.000 2.14 0 CO2 1.853 0 O6 2.241 34.1 0 1 1.472 92.8 64.8 0 7 1.884 94.6 62.7 54.0 0 8 1.536 93.8 121.7 113.4 165.3 4 O7 1.444 67.1 71.2 60.6 110.6 62.0 6 O8 3.042 153.6 169.0 104.3 111.8 61.1 103.8 12 O10 3.134 107.5 141.3 145.9 145.9 40.1 101.9 48.4 31 10 2.153 155.7 131.0 66.7 83.8 83.6 90.8 38.2 85.9 36 13 2.286 129.2 104.8 40.0 73.5 91.8 71.6 64.2 108.9 27.6 O8 0. 0.0839 0.0998 0.1748 1.000 2.83 0 CO1 2.039 0 O5 2.983 60.9 0 O9 2.138 92.1 75.6 0 3 2.142 40.7 68.4 130.4 0 10 1.896 38.2 98.3 110.1 46.8 2 O7 3.042 75.4 132.9 90.2 90.2 44.6 8 O8 3.112 140.9 82.4 90.9 115.9 158.6 143.5 9 O8 2.891 44.8 61.0 47.4 84.9 68.5 76.2 128.1 13 O10 2.534 126.3 125.6 51.9 157.9 111.3 67.7 84.7 88.3 O9 0. 0.1420 0.2500 -0.0219 0.500 2.12 0 O8 2.138 0 9 2.435 117.5 9 O8 2.138 85.1 117.5 13 O10 2.076 73.9 114.4 128.0 16 O10 2.076 128.0 114.4 73.9 82.6 28 8 2.441 70.8 167.7 70.8 57.5 57.5 O10 0. -0.6462 0.1076 0.0340 1.000 1.89 0 CO3 2.231 0 2 1.922 34.2 0 7 2.385 38.5 58.5 0 12 2.207 81.2 60.3 66.1 3 O7 3.134 125.9 96.5 151.3 90.0 7 O8 2.534 128.2 136.0 143.5 148.3 63.9 10 O9 2.076 74.4 88.8 103.2 148.8 88.9 54.1 14 O10 3.185 91.6 86.3 58.9 34.0 109.8 136.5 161.1 15 O10 2.741 52.1 44.5 90.4 100.7 78.1 91.7 48.7 130.6 21 4 1.902 142.1 120.1 111.0 62.4 67.3 89.7 143.4 52.5 140.5 29 8 2.196 101.4 77.8 136.1 97.2 26.8 68.1 69.6 126.7 51.4 93.4 34 12 1.832 103.5 118.8 65.7 76.3 126.1 103.7 127.9 42.3 155.2 60.1 152.9 1 222. -0.6253 0.2500 -0.3642 0.500 1.39 0 CO3 1.149 0 O6 2.092 76.8 0 O7 1.472 139.2 75.7 0 7 1.568 66.3 71.1 76.5 4 O7 1.472 139.2 75.7 58.8 129.4 27 7 1.568 66.3 71.1 129.4 124.3 76.5 36 13 1.497 107.3 175.9 100.7 110.4 100.7 110.4 2 160. -0.4935 0.2500 -0.0251 0.500 1.22 0 CO3 1.256 0 O5 1.682 121.3 0 O6 2.272 68.0 53.3 0 O10 1.922 86.5 128.9 128.6 15 O10 1.922 86.5 128.9 128.6 91.0 3 156. -0.0635 0.1198 0.3900 1.000 2.26 0 CO1 1.457 0 O8 2.142 65.8 0 5 1.476 62.0 127.0 0 10 1.618 49.5 58.6 92.8 0 11 1.609 82.2 81.7 82.3 125.6 24 6 1.064 98.6 157.2 45.3 98.7 113.9 4 141. -0.4592 0.0449 -0.1970 1.000 2.81 0 O6 2.263 0 7 0.989 71.8 14 O10 1.902 131.8 154.1 5 136. -0.1223 0.2500 0.4639 0.500 1.23 0 CO1 1.512 0 3 1.476 58.3 1 CO4 1.073 143.3 112.6 20 3 1.476 58.3 116.2 112.6 24 6 1.050 96.0 46.1 99.0 148.4 26 6 1.050 96.0 148.4 99.0 46.1 130.9 30 9 1.211 113.7 105.5 103.0 105.5 65.8 65.8 6 133. -0.0882 0.1507 -0.4753 1.000 2.93 0 CO4 1.614 0 9 1.236 76.5 19 3 1.064 103.6 137.5 23 5 1.050 41.0 63.4 88.6 7 121. -0.5610 0.1060 -0.2656 1.000 2.34 0 CO3 1.527 0 O6 2.169 68.4 0 O7 1.884 91.7 66.7 0 O10 2.385 65.3 112.3 153.7 0 1 1.568 43.6 65.8 49.4 105.0 0 4 0.989 125.4 82.5 118.3 86.6 148.3 8 116. -0.6125 0.2500 -0.7157 0.500 1.78 0 O7 1.536 4 O7 1.536 56.1 11 O9 2.441 137.9 137.9 12 O10 2.196 113.0 168.1 52.9 17 O10 2.196 168.1 113.0 52.9 77.2 9 116. -0.0501 0.2500 -0.3603 0.500 2.20 0 O9 2.435 0 6 1.236 127.9 23 5 1.211 170.5 50.8 25 6 1.236 127.9 101.3 50.8 10 114. 0.1447 0.1720 0.4344 1.000 2.16 0 CO1 1.296 0 O8 1.896 76.9 0 3 1.618 58.8 74.6 0 13 1.065 86.4 156.6 110.5 2 O7 2.153 135.4 97.2 162.5 83.2 32 10 1.502 54.6 111.5 108.1 45.2 89.2 11 113. -0.2260 0.1577 0.1975 1.000 1.98 0 O5 1.534 0 3 1.609 140.8 0 12 1.432 84.3 127.9 12 110. -0.3551 0.0652 0.0741 1.000 2.54 0 O5 1.992 0 O10 2.207 101.5 0 11 1.432 50.0 117.7 14 O10 1.832 132.8 103.7 137.4 13 105. 0.1731 0.2500 0.5457 0.500 1.57 0 CO1 1.625 0 10 1.065 52.7 2 O7 2.286 109.0 69.2 5 O7 2.286 109.0 95.2 36.8 18 1 1.497 145.3 106.8 39.2 39.2 32 10 1.065 52.7 89.7 95.2 69.2 106.8 Atom Code x y z Height Symmetry transformation CO4 1 -0.2643 0.2500 0.4552 1.04 0.0000+X 0.0000+Y 1.0000+Z O7 2 0.4350 0.1750 0.4838 2.50 1.0000+X 0.0000+Y 1.0000+Z O7 3 -0.5650 0.1750 0.4838 1.09 0.0000+X 0.0000+Y 1.0000+Z O7 4 -0.5650 0.3250 -0.5162 1.14 0.0000+X 0.5000-Y 0.0000+Z O7 5 0.4350 0.3250 0.4838 1.50 1.0000+X 0.5000-Y 1.0000+Z O8 6 -0.9161 0.0998 -0.8252 2.46 -1.0000+X 0.0000+Y -1.0000+Z O8 7 -0.9161 0.0998 0.1748 1.41 -1.0000+X 0.0000+Y 0.0000+Z O8 8 -0.0839 -0.0998 -0.1748 4.28 0.0000-X 0.0000-Y 0.0000-Z O8 9 0.0839 0.4002 0.1748 0.83 0.0000+X 0.5000-Y 0.0000+Z O9 10 -0.8580 0.2500 -0.0219 0.70 -1.0000+X 0.0000+Y 0.0000+Z O9 11 -0.8580 0.2500 -1.0219 1.76 -1.0000+X 0.0000+Y -1.0000+Z O10 12 -0.6462 0.1076 -0.9660 2.94 0.0000+X 0.0000+Y -1.0000+Z O10 13 0.3538 0.1076 0.0340 3.30 1.0000+X 0.0000+Y 0.0000+Z O10 14 -0.3538 -0.1076 -0.0340 3.80 -1.0000-X 0.0000-Y 0.0000-Z O10 15 -0.6462 0.3924 0.0340 0.00 0.0000+X 0.5000-Y 0.0000+Z O10 16 0.3538 0.3924 0.0340 1.41 1.0000+X 0.5000-Y 0.0000+Z O10 17 -0.6462 0.3924 -0.9660 1.05 0.0000+X 0.5000-Y -1.0000+Z 1 18 0.3747 0.2500 0.6358 1.76 1.0000+X 0.0000+Y 1.0000+Z 3 19 -0.0635 0.1198 -0.6100 3.31 0.0000+X 0.0000+Y -1.0000+Z 3 20 -0.0635 0.3802 0.3900 0.53 0.0000+X 0.5000-Y 0.0000+Z 4 21 -0.5408 -0.0449 0.1970 2.88 -1.0000-X 0.0000-Y 0.0000-Z 4 22 -0.4592 0.4551 -0.1970 0.09 0.0000+X 0.5000-Y 0.0000+Z 5 23 -0.1223 0.2500 -0.5361 2.28 0.0000+X 0.0000+Y -1.0000+Z 6 24 -0.0882 0.1507 0.5247 1.88 0.0000+X 0.0000+Y 1.0000+Z 6 25 -0.0882 0.3493 -0.4753 1.61 0.0000+X 0.5000-Y 0.0000+Z 6 26 -0.0882 0.3493 0.5247 0.56 0.0000+X 0.5000-Y 1.0000+Z 7 27 -0.5610 0.3940 -0.2656 0.42 0.0000+X 0.5000-Y 0.0000+Z 8 28 0.3875 0.2500 0.2843 2.14 1.0000+X 0.0000+Y 1.0000+Z 8 29 -0.6125 0.2500 0.2843 0.73 0.0000+X 0.0000+Y 1.0000+Z 9 30 -0.0501 0.2500 0.6397 1.15 0.0000+X 0.0000+Y 1.0000+Z 10 31 -0.8553 0.1720 -0.5656 1.80 -1.0000+X 0.0000+Y -1.0000+Z 10 32 0.1447 0.3280 0.4344 1.12 0.0000+X 0.5000-Y 0.0000+Z 11 33 -0.2260 0.3423 0.1975 0.75 0.0000+X 0.5000-Y 0.0000+Z 12 34 -0.6449 -0.0652 -0.0741 3.15 -1.0000-X 0.0000-Y 0.0000-Z 12 35 -0.3551 0.4348 0.0741 0.09 0.0000+X 0.5000-Y 0.0000+Z 13 36 -0.8269 0.2500 -0.4543 1.20 -1.0000+X 0.0000+Y -1.0000+Z 0.0 seconds elapsed time +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + zhu3 finished at 17:15:23 Total elapsed time: 3.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++