+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXS-97 - CRYSTAL STRUCTURE SOLUTION - WinGX VERSION + + Copyright(C) George M. Sheldrick 1986-97 Release 97-2 + + 2009src1247 started at 10:41:19 on 24 Nov 2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src1247 in P4(1)2(1)2 CELL 0.71073 15.2959 15.2959 43.2172 90.000 90.000 90.000 ZERR 8.00 0.0006 0.0006 0.0020 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5-Y, 0.5+X, 0.25+Z SYMM 0.5+Y, 0.5-X, 0.75+Z SYMM 0.5-X, 0.5+Y, 0.25-Z SYMM 0.5+X, 0.5-Y, 0.75-Z SYMM Y, X, -Z SYMM -Y, -X, 0.5-Z SFAC C H N O P HO UNIT 288 648 24 96 24 8 V = 10111.29 At vol = 23.0 F(000) = 4208.0 mu = 1.71 mm-1 Max single Patterson vector = 75.2 cell wt = 8047.02 rho = 1.322 OMIT 4.00 180.00 ESEL 1.200 5.000 0.005 0.700 0 PATT 1 1.800 0.770 314 7.0 9 HKLF 4 h k l F*F Sigma Why Rejected 0.00 0.00 -9.00 4.19 0.94 Observed but should be systematically absent 52099 Reflections read, of which 126 rejected Maximum h, k, l and 2-Theta = 19. 19. 56. 55.04 INCONSISTENT EQUIVALENTS h k l F*F Sigma(F*F) Esd of mean(F*F) 2 6 0 593.81 20.87 156.72 1 9 0 79.92 3.71 19.21 3 10 0 244.68 10.35 63.42 3 17 0 16.54 5.98 33.72 2 7 3 394.69 9.44 84.39 9 12 5 23.43 4.93 27.62 6 16 9 30.56 5.04 33.19 1 7 38 140.90 6.79 35.04 7 11 38 27.95 13.29 72.46 1 5 40 215.65 8.11 45.18 2 7 44 37.85 9.56 78.17 5 7 45 146.33 11.42 73.70 6588 Unique reflections, of which 5781 observed R(int) = 0.0731 R(sigma) = 0.0487 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) 21. 60. 144. 204. 246. 293. 217. 276. 356. 493. 704. 971. 1392. N(measured) 21. 60. 145. 204. 246. 294. 218. 283. 368. 509. 750. 1074. 1714. N(theory) 36. 60. 145. 205. 246. 295. 218. 283. 368. 510. 750. 1075. 1718. 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 = 17304 / 32940 Observed E .GT. 1.200 1.300 1.400 1.500 1.600 1.700 1.800 1.900 2.000 2.100 Number 1732 1415 1155 922 740 576 456 371 299 249 Centric Acentric 0kl h0l hk0 Rest Mean Abs(E*E-1) 0.968 0.736 0.957 0.957 0.789 0.786 0.6 seconds CPU time SUMMARY OF PARAMETERS FOR 2009src1247 in P4(1)2(1)2 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 314 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 3 91 GRID -0.568 -1 -1 0.568 1 1 Super-sharp Patterson for 2009src1247 in P4(1)2(1)2 Maximum = 999.10, minimum = -117.10 highest memory used = 9288 /113278 0.3 seconds CPU time Rms Patterson density excluding points close to the origin or an equivalent lattice point is 4.04 X Y Z Weight Peak Sigma Length 1 0.0000 0.0000 0.0000 16. 999. 247.46 0.00 2 0.5000 0.5000 0.4467 8. 220. 54.37 22.13 3 0.0336 0.0336 0.2496 2. 140. 34.66 10.81 4 0.0000 0.0704 0.5000 4. 121. 29.99 21.64 5 0.5000 0.5000 0.3633 8. 111. 27.58 19.07 6 0.5000 0.5000 0.1980 8. 101. 24.99 13.79 7 0.5000 0.4349 0.0531 2. 87. 21.47 10.39 8 0.4582 0.4582 0.3031 2. 83. 20.66 16.43 9 0.0156 0.0156 0.0236 2. 55. 13.53 1.08 10 0.0000 0.0000 0.0830 8. 43. 10.65 3.59 11 0.1916 0.1916 0.5000 4. 38. 9.29 22.00 12 0.4583 0.5000 0.3865 2. 31. 7.71 19.66 13 0.1234 0.2020 0.0000 2. 31. 7.61 3.62 14 0.0477 0.0477 0.3343 2. 30. 7.36 14.49 15 0.0000 0.0000 0.1679 8. 30. 7.34 7.26 16 0.0702 0.0000 0.4155 2. 29. 7.26 17.99 17 0.3358 0.3358 0.3026 2. 29. 7.11 14.96 18 0.1346 0.1346 0.5000 4. 28. 6.99 21.80 19 0.0370 0.0370 0.0178 2. 28. 6.85 1.11 20 0.1628 0.1628 0.2495 2. 27. 6.75 11.34 21 0.1195 0.1195 0.0000 4. 25. 6.30 2.59 22 0.5000 0.5000 0.4719 8. 25. 6.24 23.08 23 0.4603 0.4603 0.1129 2. 24. 5.83 11.09 24 0.0000 0.0000 0.2279 8. 23. 5.73 9.85 25 0.2985 0.2985 0.0502 2. 22. 5.37 6.81 26 0.0480 0.0000 0.0412 2. 20. 4.91 1.93 27 0.4044 0.4044 0.0000 4. 18. 4.57 8.75 28 0.4732 0.4344 0.1373 1. 18. 4.45 11.48 29 0.0000 0.0000 0.0435 8. 17. 4.19 1.88 30 0.0000 0.0727 0.0000 4. 17. 4.12 1.11 31 0.4373 0.4373 0.0688 2. 17. 4.11 9.92 32 0.5000 0.5000 0.4218 8. 16. 3.89 21.20 33 0.4876 0.4876 0.4033 2. 16. 3.88 20.37 34 0.0000 0.0000 0.2714 8. 15. 3.74 11.73 35 0.0000 0.0000 0.2081 8. 14. 3.54 8.99 36 0.1721 0.1721 0.0405 2. 14. 3.53 4.11 37 0.3658 0.3077 0.4471 1. 14. 3.43 20.66 38 0.3751 0.3751 0.0574 2. 14. 3.41 8.48 39 0.0281 0.0281 0.4585 2. 14. 3.35 19.82 40 0.1150 0.1150 0.0268 2. 13. 3.33 2.74 41 0.0124 0.0124 0.0614 2. 13. 3.25 2.67 42 0.3942 0.3942 0.4490 2. 13. 3.20 21.20 43 0.4526 0.4321 0.5000 2. 13. 3.16 23.63 44 0.1070 0.0558 0.0102 1. 12. 2.98 1.90 45 0.4047 0.4047 0.3187 2. 12. 2.92 16.32 46 0.5000 0.5000 0.3195 8. 11. 2.82 17.54 47 0.3444 0.2711 0.1999 1. 11. 2.80 10.94 48 0.0876 0.0388 0.0517 1. 11. 2.79 2.67 49 0.4768 0.3529 0.0000 2. 11. 2.77 9.07 50 0.4300 0.4300 0.2435 2. 11. 2.72 14.05 51 0.5000 0.4457 0.2585 2. 11. 2.68 15.16 52 0.5000 0.5000 0.1739 8. 11. 2.67 13.17 53 0.1621 0.2197 0.2444 1. 11. 2.67 11.36 54 0.5000 0.4383 0.3485 2. 11. 2.65 18.17 55 0.4565 0.4565 0.0106 2. 10. 2.59 9.89 56 0.5000 0.5000 0.2213 8. 10. 2.55 14.44 57 0.0649 0.0000 0.2913 2. 10. 2.55 12.63 58 0.0915 0.0915 0.1244 2. 10. 2.46 5.73 59 0.0995 0.0000 0.0279 2. 10. 2.42 1.94 60 0.0000 0.1576 0.3557 2. 9. 2.33 15.56 61 0.5000 0.3663 0.0934 2. 9. 2.29 10.31 62 0.0560 0.0560 0.0341 2. 9. 2.27 1.91 63 0.5000 0.3491 0.4796 2. 9. 2.25 22.73 64 0.5000 0.5000 0.4910 8. 9. 2.24 23.82 65 0.0604 0.0293 0.0569 1. 9. 2.24 2.66 66 0.0000 0.0000 0.2913 8. 9. 2.24 12.59 67 0.1246 0.0000 0.1974 2. 9. 2.23 8.74 68 0.5000 0.3865 0.2483 2. 9. 2.23 14.44 69 0.1345 0.1345 0.4639 2. 9. 2.18 20.26 70 0.1399 0.0000 0.0346 2. 9. 2.17 2.61 71 0.0546 0.0546 0.2740 2. 9. 2.13 11.90 72 0.5000 0.3911 0.2286 2. 8. 2.09 13.85 73 0.4361 0.3759 0.0208 1. 8. 2.08 8.85 74 0.0836 0.1632 0.2513 1. 8. 2.07 11.22 75 0.4288 0.4288 0.2789 2. 8. 2.05 15.21 76 0.0714 0.0000 0.4755 2. 8. 2.04 20.58 77 0.0652 0.0652 0.3057 2. 8. 2.04 13.29 78 0.4076 0.3276 0.1953 1. 8. 1.97 11.63 79 0.0000 0.0000 0.1099 8. 8. 1.92 4.75 80 0.0000 0.1225 0.1082 2. 8. 1.90 5.04 Vectors selected for Patterson superposition: Vector X Y Z Weight Peak Length 1 0.0336 0.0336 0.2496 2. 140. 10.81 FMAP and GRID set by program FMAP 6 3 91 GRID -0.568 -2 -2 0.568 2 2 Patterson vector superposition minimum function for 2009src1247 in P4(1)2(1)2 Patt. sup. on vector 1 0.0336 0.0336 0.2496 Height 140. Length 10.81 Maximum = 140.17, minimum = -119.82 highest memory used = 13961 /225936 0.5 seconds CPU time 155 Superposition peaks employed, maximum height 72.9 and minimum height 2.8 on atomic number scale Heavy-Atom Location for 2009src1247 in P4(1)2(1)2 5781 reflections used for structure factor sums Solution 1 CFOM = 44.49 PATFOM = 98.4 Corr. Coeff. = 67.3 SYMFOM = 99.9 Shift to be added to superposition coordinates: 0.5196 0.9850 0.9735 Name At.No. x y z s.o.f. Minimum distances / PATSMF (self first) HO1 71.6 0.5343 0.0018 0.0985 1.0000 10.36 91.0 P2 15.4 0.6633 -0.1970 0.0991 1.0000 8.40 3.63 0.5 11.2 P3 13.8 0.5391 -0.0111 0.0144 1.0000 9.81 3.64 5.01 2.1 22.8 1.8 P4 13.4 0.3372 0.1292 0.0971 1.0000 8.45 3.59 7.06 5.19 1.1 10.4 0.6 0.9 Solution 2 CFOM = 40.42 PATFOM = 99.9 Corr. Coeff. = 67.7 SYMFOM = 88.2 Shift to be added to superposition coordinates: 0.5150 0.9791 0.0265 Name At.No. x y z s.o.f. Minimum distances / PATSMF (self first) HO1 71.6 0.5341 0.9978 0.1515 1.0000 10.36 91.7 P2 15.6 0.6637 1.1974 0.1510 1.0000 8.40 3.64 0.5 11.2 P3 14.2 0.3349 0.8736 0.1530 1.0000 8.43 3.59 7.06 1.1 10.3 0.5 P4 13.6 0.5376 1.0127 0.2356 1.0000 9.81 3.64 5.01 5.19 2.2 23.5 1.7 1.0 Maximum memory for Patterson interpretation = 4829 / 790 0.6 seconds CPU time +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src1247 finished at 10:41:21 Total CPU time: 2.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++