+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXS-97 - CRYSTAL STRUCTURE SOLUTION - WinGX VERSION + + Copyright(C) George M. Sheldrick 1986-97 Release 97-2 + + 2009src1087 started at 10:13:49 on 07 Oct 2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src1087 in P2(1)2(1)2(1) CELL 0.71073 14.3298 14.4760 23.9774 90.000 90.000 90.000 ZERR 4.00 0.0005 0.0005 0.0009 0.000 0.000 0.000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O P ND UNIT 144 324 12 48 12 4 V = 4973.83 At vol = 22.6 F(000) = 2076.0 mu = 1.19 mm-1 Max single Patterson vector = 136.9 cell wt = 3940.75 rho = 1.316 OMIT 4.00 180.00 ESEL 1.200 5.000 0.005 0.700 0 PATT HKLF 4 h k l F*F Sigma Why Rejected -3.00 0.00 0.00 7.29 1.15 Observed but should be systematically absent -3.00 0.00 0.00 10.11 2.12 Observed but should be systematically absent 3.00 0.00 0.00 9.10 1.92 Observed but should be systematically absent -3.00 0.00 0.00 7.41 1.73 Observed but should be systematically absent 7.00 0.00 0.00 202.93 25.46 Observed but should be systematically absent -7.00 0.00 0.00 240.51 34.42 Observed but should be systematically absent 11.00 0.00 0.00 106.09 11.66 Observed but should be systematically absent 13.00 0.00 0.00 173.19 14.94 Observed but should be systematically absent 0.00 9.00 0.00 33.01 7.70 Observed but should be systematically absent 0.00 -11.00 0.00 105.88 17.03 Observed but should be systematically absent 0.00 -13.00 0.00 188.97 25.05 Observed but should be systematically absent 31606 Reflections read, of which 57 rejected Maximum h, k, l and 2-Theta = 18. 18. 31. 55.02 INCONSISTENT EQUIVALENTS h k l F*F Sigma(F*F) Esd of mean(F*F) 2 16 10 63.32 8.22 54.65 8 10 11 121.50 13.41 67.41 6190 Unique reflections, of which 6126 observed R(int) = 0.0615 R(sigma) = 0.0471 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) 22. 48. 132. 186. 245. 273. 198. 262. 351. 501. 707. 1023. 1565. N(measured) 22. 48. 132. 186. 245. 275. 199. 262. 351. 502. 711. 1032. 1588. N(theory) 32. 50. 133. 186. 245. 275. 199. 262. 351. 502. 711. 1042. 1625. 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 = 11708 / 30950 Observed E .GT. 1.200 1.300 1.400 1.500 1.600 1.700 1.800 1.900 2.000 2.100 Number 1891 1510 1196 957 729 529 386 277 186 115 Centric Acentric 0kl h0l hk0 Rest Mean Abs(E*E-1) 0.968 0.736 0.869 0.884 0.820 0.650 0.3 seconds CPU time SUMMARY OF PARAMETERS FOR 2009src1087 in P2(1)2(1)2(1) ESEL Emin 1.200 Emax 5.000 DelU 0.005 renorm 0.700 axis 0 OMIT s 4.00 2theta(lim) 180.0 PATT nv 1 dmin 1.80 resl 0.77 Nsup 230 Zmin 7.00 maxat 9 FMAP code 6 PLAN npeaks 80 del1 0.500 del2 1.500 MORE verbosity 1 TIME t 9999999. FMAP and GRID set by program FMAP 6 1 32 GRID -1.724 -1 -1 1.724 1 1 Super-sharp Patterson for 2009src1087 in P2(1)2(1)2(1) Maximum = 999.10, minimum = -122.00 highest memory used = 9240 / 59476 0.1 seconds CPU time Rms Patterson density excluding points close to the origin or an equivalent lattice point is 4.56 X Y Z Weight Peak Sigma Length 1 0.0000 0.0000 0.0000 8. 999. 219.22 0.00 2 0.5000 0.3856 0.1692 2. 185. 40.55 9.95 3 0.1370 0.1147 0.5000 2. 178. 39.12 12.26 4 0.3626 0.5000 0.3311 2. 176. 38.51 11.93 5 0.1149 0.1953 0.5000 2. 47. 10.27 12.43 6 0.2501 0.0797 0.0000 2. 46. 10.09 3.76 7 0.0150 0.0311 0.0415 1. 45. 9.79 1.11 8 0.5000 0.4469 0.3204 2. 35. 7.78 12.34 9 0.2478 0.3071 0.1783 1. 35. 7.67 7.12 10 0.3845 0.4195 0.3220 1. 33. 7.29 11.26 11 0.0000 0.0000 0.0488 4. 32. 6.98 1.17 12 0.1678 0.1864 0.0518 1. 31. 6.89 3.82 13 0.0000 0.0505 0.1531 2. 31. 6.80 3.74 14 0.3322 0.4293 0.1178 1. 31. 6.76 8.32 15 0.1939 0.3133 0.3804 1. 30. 6.59 10.56 16 0.3049 0.0714 0.4488 1. 29. 6.43 11.66 17 0.1527 0.0506 0.3493 1. 27. 6.00 8.69 18 0.5000 0.0000 0.4437 4. 25. 5.54 12.83 19 0.0135 0.0807 0.0000 2. 24. 5.17 1.18 20 0.2564 0.0000 0.4763 2. 22. 4.84 12.00 21 0.0754 0.0796 0.0901 1. 21. 4.65 2.68 22 0.0000 0.1064 0.4191 2. 20. 4.46 10.17 23 0.3764 0.5000 0.1450 2. 20. 4.33 9.67 24 0.3495 0.4377 0.1781 1. 19. 4.11 9.14 25 0.0267 0.1487 0.0601 1. 19. 4.06 2.62 26 0.0000 0.0386 0.0798 2. 18. 4.05 1.99 27 0.0893 0.1568 0.0000 2. 18. 4.02 2.61 28 0.0415 0.0416 0.5000 2. 18. 4.01 12.02 29 0.5000 0.4427 0.2639 2. 18. 4.00 11.51 30 0.5000 0.2480 0.0707 2. 18. 3.93 8.19 31 0.0873 0.0000 0.0603 2. 17. 3.73 1.91 32 0.5000 0.2301 0.1883 2. 16. 3.57 9.10 33 0.0000 0.1511 0.4792 2. 16. 3.48 11.70 34 0.0000 0.0616 0.1015 2. 16. 3.43 2.59 35 0.1468 0.5000 0.1127 2. 16. 3.42 8.01 36 0.0976 0.1382 0.0643 1. 16. 3.42 2.89 37 0.0997 0.3181 0.5000 2. 15. 3.26 12.92 38 0.0691 0.5000 0.1296 2. 15. 3.23 7.94 39 0.3464 0.3535 0.2718 1. 15. 3.19 9.66 40 0.0000 0.3905 0.3882 2. 14. 2.99 10.89 41 0.5000 0.2802 0.4105 2. 14. 2.96 12.83 42 0.3200 0.0000 0.0424 2. 13. 2.94 4.70 43 0.3438 0.5000 0.3790 2. 13. 2.81 12.62 44 0.4148 0.3222 0.0817 1. 13. 2.80 7.81 45 0.3292 0.4776 0.3728 1. 13. 2.80 12.25 46 0.5000 0.2349 0.2277 2. 13. 2.79 9.63 47 0.3317 0.2867 0.0000 2. 13. 2.78 6.31 48 0.2417 0.1808 0.4658 1. 13. 2.76 11.98 49 0.2406 0.2034 0.0000 2. 12. 2.68 4.53 50 0.3979 0.2470 0.2392 1. 12. 2.61 8.84 51 0.0469 0.0000 0.4358 2. 12. 2.56 10.47 52 0.4659 0.1902 0.0383 1. 12. 2.55 7.28 53 0.5000 0.1610 0.3084 2. 12. 2.54 10.56 54 0.2585 0.3602 0.2636 1. 12. 2.54 8.99 55 0.1368 0.2072 0.0907 1. 11. 2.52 4.19 56 0.2779 0.0781 0.1105 1. 11. 2.51 4.92 57 0.1922 0.1764 0.5000 2. 11. 2.49 12.56 58 0.0347 0.1981 0.1307 1. 11. 2.46 4.28 59 0.4178 0.4648 0.1605 1. 11. 2.45 9.79 60 0.1518 0.0758 0.0388 1. 11. 2.42 2.61 61 0.2801 0.4398 0.4209 1. 11. 2.42 12.59 62 0.4459 0.3434 0.3377 1. 11. 2.42 11.45 63 0.3328 0.3048 0.4624 1. 11. 2.40 12.85 64 0.2915 0.1839 0.0332 1. 11. 2.40 5.02 65 0.1734 0.0482 0.0225 1. 11. 2.38 2.64 66 0.4634 0.2462 0.1089 1. 11. 2.38 7.98 67 0.1315 0.0196 0.0153 1. 11. 2.33 1.94 68 0.3491 0.4287 0.2291 1. 11. 2.32 9.68 69 0.0476 0.0380 0.0703 1. 10. 2.29 1.90 70 0.1346 0.1069 0.0297 1. 10. 2.29 2.57 71 0.2872 0.1368 0.1400 1. 10. 2.28 5.67 72 0.0760 0.0356 0.1711 1. 10. 2.28 4.27 73 0.3681 0.3958 0.0859 1. 10. 2.27 8.06 74 0.3341 0.3456 0.1894 1. 10. 2.26 8.28 75 0.5000 0.3513 0.2102 2. 10. 2.24 10.13 76 0.0149 0.0984 0.0502 1. 10. 2.24 1.88 77 0.2584 0.1770 0.1609 1. 10. 2.23 5.93 78 0.3589 0.1992 0.2684 1. 10. 2.21 8.73 79 0.2235 0.1819 0.4109 1. 10. 2.21 10.69 80 0.4714 0.4011 0.2114 1. 10. 2.19 10.25 Vectors selected for Patterson superposition: Vector X Y Z Weight Peak Length 1 0.5000 0.3856 0.1692 2. 185. 9.95 FMAP and GRID set by program FMAP 6 2 62 GRID -1.695 -1 -2 1.695 1 2 Patterson vector superposition minimum function for 2009src1087 in P2(1)2(1)2(1) Patt. sup. on vector 1 0.5000 0.3856 0.1692 Height 185. Length 9.95 Maximum = 157.53, minimum = -106.64 highest memory used = 13241 /226591 0.2 seconds CPU time 105 Superposition peaks employed, maximum height 60.0 and minimum height 2.8 on atomic number scale Heavy-Atom Location for 2009src1087 in P2(1)2(1)2(1) 6126 reflections used for structure factor sums Solution 1 CFOM = 63.40 PATFOM = 99.4 Corr. Coeff. = 79.9 SYMFOM = 99.9 Shift to be added to superposition coordinates: 0.5682 0.2500 1.0000 Name At.No. x y z s.o.f. Minimum distances / PATSMF (self first) ND1 64.1 0.1818 0.9423 0.4161 1.0000 9.93 177.3 P2 19.3 0.4330 0.8640 0.4084 1.0000 9.03 3.78 4.7 34.6 P3 17.6 0.0134 1.1279 0.4670 1.0000 8.14 3.81 7.26 5.4 31.1 6.1 P4 11.0 0.1800 0.9976 0.2623 1.0000 8.91 3.77 5.40 5.78 0.6 22.6 1.8 2.6 Solution 2 CFOM = 63.40 PATFOM = 99.4 Corr. Coeff. = 79.9 SYMFOM = 99.9 Shift to be added to superposition coordinates: 0.9318 0.7500 1.0000 Name At.No. x y z s.o.f. Minimum distances / PATSMF (self first) ND1 64.1 0.3182 0.0577 0.5839 1.0000 9.93 177.3 P2 19.3 0.0670 0.1360 0.5916 1.0000 9.03 3.78 4.7 34.6 P3 17.6 0.4866 -0.1279 0.5330 1.0000 8.14 3.81 7.26 5.4 31.1 6.1 P4 11.0 0.3200 0.0024 0.7377 1.0000 8.91 3.77 5.40 5.78 0.6 22.6 1.8 2.6 Solution 3 CFOM = 63.40 PATFOM = 99.4 Corr. Coeff. = 79.9 SYMFOM = 99.9 Shift to be added to superposition coordinates: 0.4318 0.2500 1.0000 Name At.No. x y z s.o.f. Minimum distances / PATSMF (self first) ND1 64.1 0.8182 0.5577 0.5839 1.0000 9.93 177.3 P2 19.3 0.5670 0.6360 0.5916 1.0000 9.03 3.78 4.7 34.6 P3 17.6 0.9866 0.3721 0.5330 1.0000 8.14 3.81 7.26 5.4 31.1 6.1 P4 11.0 0.8200 0.5024 0.7377 1.0000 8.91 3.77 5.40 5.78 0.6 22.6 1.8 2.6 Solution 4 CFOM = 63.40 PATFOM = 99.4 Corr. Coeff. = 79.9 SYMFOM = 99.9 Shift to be added to superposition coordinates: 0.0682 0.7500 0.0000 Name At.No. x y z s.o.f. Minimum distances / PATSMF (self first) ND1 64.1 0.6818 0.4423 0.4161 1.0000 9.93 177.3 P2 19.3 0.9330 0.3640 0.4084 1.0000 9.03 3.78 4.7 34.6 P3 17.6 0.5134 0.6279 0.4670 1.0000 8.14 3.81 7.26 5.4 31.1 6.1 P4 11.0 0.6800 0.4976 0.2623 1.0000 8.91 3.77 5.40 5.78 0.6 22.6 1.8 2.6 Solution 5 CFOM = 61.92 PATFOM = 99.9 Corr. Coeff. = 79.9 SYMFOM = 97.0 Shift to be added to superposition coordinates: 0.5682 0.7493 1.0000 Name At.No. x y z s.o.f. Minimum distances / PATSMF (self first) ND1 64.1 0.1818 0.4423 0.4161 1.0000 9.93 177.3 P2 19.3 0.4330 0.3640 0.4084 1.0000 9.03 3.78 4.7 34.6 P3 17.6 0.0134 0.6279 0.4670 1.0000 8.14 3.81 7.26 5.4 31.1 6.1 P4 11.0 0.1794 0.4981 0.2623 1.0000 8.90 3.77 5.41 5.77 0.4 22.8 1.8 2.7 Solution 6 CFOM = 61.86 PATFOM = 99.9 Corr. Coeff. = 79.9 SYMFOM = 96.9 Shift to be added to superposition coordinates: 0.4318 0.7493 0.5000 Name At.No. x y z s.o.f. Minimum distances / PATSMF (self first) ND1 64.1 0.8182 0.0577 0.0839 1.0000 9.93 177.3 P2 19.3 0.5670 0.1360 0.0916 1.0000 9.03 3.78 4.7 34.6 P3 17.6 0.9866 -0.1279 0.0330 1.0000 8.14 3.81 7.26 5.4 31.1 6.1 P4 11.0 0.8206 0.0019 0.2377 1.0000 8.90 3.77 5.41 5.77 0.4 22.8 1.8 2.7 Solution 7 CFOM = 61.63 PATFOM = 99.5 Corr. Coeff. = 79.9 SYMFOM = 97.0 Shift to be added to superposition coordinates: 0.9318 0.2507 0.0000 Name At.No. x y z s.o.f. Minimum distances / PATSMF (self first) ND1 64.1 0.3182 0.5577 0.5839 1.0000 9.93 177.3 P2 19.3 0.0670 0.6360 0.5916 1.0000 9.03 3.78 4.7 34.6 P3 17.6 0.4866 0.3721 0.5330 1.0000 8.14 3.81 7.26 5.4 31.1 6.1 P4 11.0 0.3201 0.5023 0.7377 1.0000 8.91 3.77 5.40 5.77 0.5 22.6 1.8 2.6 Solution 8 CFOM = 61.57 PATFOM = 99.5 Corr. Coeff. = 79.9 SYMFOM = 96.9 Shift to be added to superposition coordinates: 0.0682 0.2507 0.0000 Name At.No. x y z s.o.f. Minimum distances / PATSMF (self first) ND1 64.1 0.6818 0.9423 0.4161 1.0000 9.93 177.3 P2 19.3 0.9330 0.8640 0.4084 1.0000 9.03 3.78 4.7 34.6 P3 17.6 0.5134 1.1279 0.4670 1.0000 8.14 3.81 7.26 5.4 31.1 6.1 P4 11.0 0.6799 0.9977 0.2623 1.0000 8.91 3.77 5.40 5.77 0.5 22.6 1.8 2.6 Maximum memory for Patterson interpretation = 3866 / 1730 0.4 seconds CPU time +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src1087 finished at 10:13:50 Total CPU time: 1.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++