+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXS-97 - CRYSTAL STRUCTURE SOLUTION - WinGX VERSION + + Copyright(C) George M. Sheldrick 1986-97 Release 97-2 + + 00skl038 started at 15:05:18 on 06 Aug 2000 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 00skl038 in P 21/c CELL 0.71073 13.1826 12.8268 16.4122 90.000 105.964 90.000 ZERR 4 0.0002 0.0002 0.0003 0.000 0.001 0.000 LATT 1 SYMM -X,1/2+Y,1/2-Z SFAC C H Br Cu N UNIT 72 76 4 4 12 V = 2668.12 At vol = 29.0 F(000) = 848.0 mu = 2.32 mm-1 Max single Patterson vector = 106.2 cell wt = 1683.25 rho = 1.048 TEMP -123 SIZE 0.05 0.05 0.05 PATT HKLF 4 27502 Reflections read, of which 785 rejected Maximum h, k, l and 2-Theta = 18. 17. 23. 61.02 INCONSISTENT EQUIVALENTS h k l F*F Sigma(F*F) Esd of mean(F*F) 1 0 0 1.25 0.07 3.56 1 1 0 7.96 0.06 2.25 1 5 0 10.67 0.09 1.28 1 6 0 10.40 0.17 1.32 -2 1 3 9.51 0.09 1.18 -1 2 3 33.48 0.10 9.53 -1 3 4 41.07 0.10 16.11 -1 5 5 10.70 0.10 1.60 -1 6 6 13.27 0.10 2.24 -4 4 7 19.20 0.35 2.21 -5 7 10 16.50 0.40 3.00 7647 Unique reflections, of which 3690 observed R(int) = 0.0812 R(sigma) = 0.1574 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) 19. 44. 115. 163. 202. 246. 178. 223. 295. 392. 502. 595. 513. N(measured) 21. 44. 116. 170. 213. 263. 193. 249. 344. 482. 702. 1035. 1607. N(theory) 21. 44. 116. 170. 213. 263. 193. 249. 344. 482. 702. 1035. 1613. 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 = 16115 / 38235 Observed E .GT. 1.200 1.300 1.400 1.500 1.600 1.700 1.800 1.900 2.000 2.100 Number 1578 1372 1161 975 809 655 534 428 333 259 Centric Acentric 0kl h0l hk0 Rest Mean Abs(E*E-1) 0.968 0.736 0.803 0.959 0.796 0.869 3.9 seconds CPU time SUMMARY OF PARAMETERS FOR 00skl038 in P 21/c 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 0.70 Nsup 182 Zmin 7.00 maxat 8 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 2 34 GRID -1.613 -1 -2 1.613 1 2 Super-sharp Patterson for 00skl038 in P 21/c Maximum = 999.10, minimum = -87.42 highest memory used = 9215 / 44989 3.2 seconds CPU time Rms Patterson density excluding points close to the origin or an equivalent lattice point is 6.56 X Y Z Weight Peak Sigma Length 1 0.0000 0.0000 0.0000 4. 999. 152.36 0.00 2 0.0000 0.0452 0.5000 2. 163. 24.80 8.23 3 0.1796 0.0000 0.0801 2. 151. 22.96 2.37 4 0.1504 0.5000 0.2026 2. 136. 20.73 7.25 5 0.3274 0.5000 0.2814 2. 124. 18.87 8.37 6 0.8204 0.0393 0.4209 1. 105. 16.06 7.91 7 0.9693 0.5000 0.1191 2. 103. 15.64 6.75 8 0.8515 0.4600 0.2989 1. 101. 15.44 8.25 9 0.0291 0.5000 0.3757 2. 68. 10.41 8.83 10 0.6724 0.4426 0.2196 1. 56. 8.57 8.51 11 0.3743 0.0000 0.1280 2. 50. 7.70 4.80 12 0.7012 0.5000 0.4056 2. 50. 7.68 10.74 13 0.0000 0.0839 0.0000 2. 49. 7.50 1.08 14 0.5000 0.2784 0.0000 2. 49. 7.46 7.50 15 0.2125 0.4253 0.0012 1. 47. 7.15 6.13 16 0.0634 0.0345 0.0442 1. 43. 6.62 1.04 17 0.5000 0.3365 0.5000 2. 41. 6.20 9.98 18 0.9805 0.0317 0.0514 1. 40. 6.06 1.03 19 0.2892 0.2924 0.4758 1. 36. 5.55 8.56 20 0.3252 0.3152 0.4110 1. 35. 5.35 8.02 21 0.2551 0.1647 0.1733 1. 35. 5.27 4.31 22 0.7932 0.4421 0.4986 1. 34. 5.19 10.90 23 0.4142 0.1287 0.2479 1. 34. 5.12 6.07 24 0.1073 0.2755 0.3958 1. 33. 5.02 7.19 25 0.0993 0.3062 0.4611 1. 32. 4.95 8.30 26 0.9449 0.0936 0.2016 1. 32. 4.87 3.77 27 0.9582 0.2152 0.1956 1. 32. 4.86 4.38 28 0.6220 0.4621 0.4190 1. 32. 4.85 11.23 29 0.0000 0.5000 0.5000 4. 31. 4.79 10.41 30 0.2288 0.0515 0.3764 1. 31. 4.74 6.12 31 0.0811 0.0000 0.0017 2. 30. 4.65 1.06 32 0.3792 0.4065 0.0813 1. 30. 4.63 7.09 33 0.5212 0.4580 0.3218 1. 29. 4.49 10.98 34 0.9378 0.0309 0.0205 1. 29. 4.48 1.05 35 0.0450 0.2580 0.3076 1. 29. 4.48 5.93 36 0.1333 0.2225 0.2736 1. 29. 4.46 5.20 37 0.7660 0.0837 0.3269 1. 29. 4.46 6.97 38 0.8921 0.2469 0.1025 1. 29. 4.43 4.03 39 0.3425 0.1901 0.2820 1. 29. 4.42 6.02 40 0.1630 0.2417 0.1434 1. 29. 4.40 4.12 41 0.0536 0.0375 0.2986 1. 28. 4.32 4.78 42 0.0000 0.1464 0.5000 2. 28. 4.25 8.42 43 0.4806 0.4360 0.1767 1. 28. 4.22 8.35 44 0.8289 0.2244 0.2889 1. 28. 4.22 6.46 45 0.7166 0.2331 0.0218 1. 27. 4.18 4.87 46 0.4524 0.0637 0.2984 1. 27. 4.09 6.64 47 0.2760 0.1397 0.9993 1. 27. 4.05 4.06 48 0.7412 0.0000 0.3956 2. 27. 4.04 8.12 49 0.6278 0.0754 0.3737 1. 26. 4.02 8.90 50 0.8737 0.2343 0.2280 1. 26. 4.01 5.41 51 0.7716 0.0730 0.1211 1. 26. 3.94 4.15 52 0.0222 0.2283 0.4464 1. 26. 3.90 7.82 53 0.1560 0.5000 0.3593 2. 25. 3.87 8.57 54 0.3004 0.4227 0.0967 1. 25. 3.86 6.64 55 0.6790 0.2968 0.0915 1. 25. 3.81 6.18 56 0.5815 0.0000 0.3049 2. 25. 3.81 8.41 57 0.0953 0.5000 0.4193 2. 25. 3.75 9.24 58 0.1726 0.1637 0.2107 1. 24. 3.72 4.15 59 0.5180 0.0000 0.3600 2. 24. 3.61 9.79 60 0.0849 0.1903 0.0997 1. 23. 3.55 2.98 61 0.5952 0.0793 0.2505 1. 23. 3.48 7.65 62 0.0445 0.4382 0.1202 1. 22. 3.43 5.93 63 0.4382 0.3705 0.2120 1. 22. 3.42 7.55 64 0.6493 0.2068 0.2113 1. 22. 3.39 7.02 65 0.3329 0.1087 0.3158 1. 22. 3.34 5.96 66 0.9820 0.2671 0.0598 1. 22. 3.33 3.59 67 0.9212 0.3664 0.0364 1. 22. 3.30 4.88 68 0.7182 0.0878 0.5032 1. 22. 3.28 8.06 69 0.5558 0.0354 0.2051 1. 21. 3.21 7.53 70 0.8945 0.4029 0.2557 1. 21. 3.20 7.03 71 0.9818 0.0954 0.0665 1. 21. 3.19 1.70 72 0.7933 0.1479 0.0991 1. 21. 3.15 4.01 73 0.4140 0.3801 0.1993 1. 20. 3.13 7.38 74 0.2632 0.3525 0.0408 1. 20. 3.09 5.63 75 0.3970 0.4043 0.2069 1. 20. 3.01 7.49 76 0.0000 0.2092 0.5000 2. 20. 3.01 8.63 77 0.5445 0.1028 0.4231 1. 20. 3.00 10.44 78 0.9199 0.4513 0.0798 1. 20. 2.99 6.09 79 0.7207 0.3167 0.4593 1. 19. 2.97 10.11 80 0.5804 0.3719 0.4607 1. 19. 2.93 11.55 Vectors selected for Patterson superposition: Vector X Y Z Weight Peak Length 1 0.8204 0.0393 0.4209 1. 105. 7.91 FMAP and GRID set by program FMAP 6 1 67 GRID -1.563 -2 -1 1.563 2 1 Patterson vector superposition minimum function for 00skl038 in P 21/c Patt. sup. on vector 1 0.8204 0.0393 0.4209 Height 105. Length 7.91 Maximum = 144.19, minimum = -83.40 highest memory used = 12832 /171892 8.4 seconds CPU time 117 Superposition peaks employed, maximum height 39.7 and minimum height 2.8 on atomic number scale Heavy-Atom Location for 00skl038 in P 21/c 3690 reflections used for structure factor sums Solution 1 CFOM = 49.57 PATFOM = 99.9 Corr. Coeff. = 70.4 SYMFOM = 99.9 Shift to be added to superposition coordinates: 0.5745 0.2463 0.6006 Name At.No. x y z s.o.f. Minimum distances / PATSMF (self first) BR1 37.4 0.1641 0.2728 0.8904 1.0000 8.23 84.3 CU2 29.8 -0.0151 0.2677 0.8107 1.0000 6.76 2.37 57.5 182.0 CU3 12.1 0.5350 0.3001 1.0136 1.0000 5.21 4.76 6.62 0.0 43.5 40.9 CU4 12.0 -0.1212 0.5139 0.9137 1.0000 3.66 4.38 4.01 5.90 7.7 48.6 44.9 12.1 CU5 11.9 -0.2159 0.6849 0.8106 1.0000 8.37 3.72 4.21 5.72 2.84 18.1 46.5 43.7 11.9 13.5 N6 10.3 -0.3383 0.5542 0.8987 1.0000 6.24 4.22 6.09 3.79 2.85 2.96 0.0 42.0 37.7 7.0 8.1 16.6 Maximum memory for Patterson interpretation = 2387 / 558 1.1 seconds CPU time +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 00skl038 finished at 15:05:35 Total CPU time: 16.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++