+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXS-97 - CRYSTAL STRUCTURE SOLUTION - WinGX VERSION + + Copyright(C) George M. Sheldrick 1986-97 Release 97-2 + + 2005src1629hklf4 started at 15:12:20 on 02 Feb 2006 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2005src1629hklf4 in P-1 CELL 0.71073 12.6047 12.9795 16.0115 89.829 86.600 64.693 ZERR 2.00 0.0025 0.0026 0.0032 0.030 0.030 0.030 LATT 1 SFAC C H N CL FE NI BR UNIT 86 70 8 18 4 2 4 V = 2363.24 At vol = 19.4 F(000) = 1248.0 mu = 3.24 mm-1 Max single Patterson vector = 68.3 cell wt = 2514.06 rho = 1.766 OMIT 4.00 180.00 ESEL 1.200 5.000 0.005 0.700 0 PATT HKLF 4 6517 Reflections read, of which 0 rejected Maximum h, k, l and 2-Theta = 16. 16. 20. 89.93 6517 Unique reflections, of which 3297 observed R(int) = 0.0000 R(sigma) = 0.2536 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) 4. 33. 105. 151. 156. 208. 142. 193. 256. 331. 414. 470. 430. N(measured) 4. 33. 107. 156. 176. 229. 161. 233. 316. 440. 633. 949. 1481. N(theory) 41. 75. 204. 300. 386. 463. 331. 450. 617. 865. 1214. 1829. 2878. 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 = 11553 / 32585 Observed E .GT. 1.200 1.300 1.400 1.500 1.600 1.700 1.800 1.900 2.000 2.100 Number 1475 1282 1114 937 805 691 570 479 395 320 Centric Acentric 0kl h0l hk0 Rest Mean Abs(E*E-1) 0.968 0.736 0.756 0.808 0.892 0.853 0.2 seconds CPU time SUMMARY OF PARAMETERS FOR 2005src1629hklf4 in P-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 0.50 Nsup 188 Zmin 7.00 maxat 19 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 3 125 GRID -0.820 -2 -1 0.820 2 1 Super-sharp Patterson for 2005src1629hklf4 in P-1 Maximum = 999.10, minimum = -481.07 highest memory used = 9213 /119728 0.3 seconds CPU time Rms Patterson density excluding points close to the origin or an equivalent lattice point is 9.77 X Y Z Weight Peak Sigma Length 1 0.0000 0.0000 0.0000 2. 999. 102.28 0.00 2 0.9960 0.0236 0.9341 1. 141. 14.48 1.10 3 0.2836 0.4995 0.3863 1. 141. 14.39 10.76 4 0.9991 0.0888 0.9844 1. 135. 13.78 1.17 5 0.0063 0.4223 0.0004 1. 114. 11.69 5.52 6 0.9393 0.0301 0.0349 1. 113. 11.57 0.86 7 0.9576 0.0371 0.0489 1. 112. 11.42 0.93 8 0.0590 0.0313 0.0279 1. 110. 11.26 1.10 9 0.9850 0.0600 0.0493 1. 105. 10.72 1.06 10 0.6387 0.0445 0.5112 1. 103. 10.54 9.18 11 0.3406 0.0640 0.4861 1. 89. 9.08 9.31 12 0.1384 0.2631 0.5678 1. 85. 8.72 8.13 13 0.1423 0.2305 0.8250 1. 83. 8.52 4.89 14 0.9965 0.1511 0.9862 1. 83. 8.46 1.96 15 0.8424 0.2773 0.4337 1. 80. 8.19 7.58 16 0.8565 0.2368 0.1789 1. 80. 8.17 3.95 17 0.8565 0.1632 0.4296 1. 74. 7.60 7.10 18 0.9912 0.0245 0.8825 1. 74. 7.55 1.91 19 0.7009 0.0798 0.6055 1. 70. 7.15 7.39 20 0.8037 0.1019 0.0935 1. 67. 6.87 2.62 21 0.1955 0.1043 0.9048 1. 66. 6.76 3.55 22 0.0617 0.4512 0.1008 1. 65. 6.61 6.45 23 0.3060 0.0876 0.3987 1. 64. 6.60 7.98 24 0.1800 0.1314 0.5760 1. 63. 6.42 7.45 25 0.9673 0.1492 0.9232 1. 62. 6.30 2.19 26 0.7946 0.3214 0.0778 1. 59. 6.04 4.01 27 0.9973 0.2173 0.9901 1. 58. 5.94 2.81 28 0.9180 0.1131 0.9114 1. 58. 5.90 2.02 29 0.2813 0.0725 0.3933 1. 56. 5.72 7.66 30 0.9442 0.4357 0.9015 1. 56. 5.70 5.63 31 0.1202 0.4177 0.4818 1. 56. 5.68 9.99 32 0.1114 0.9995 0.4917 1. 55. 5.63 8.08 33 0.6427 0.4568 0.8754 1. 54. 5.57 6.13 34 0.0617 0.1328 0.0900 1. 54. 5.54 2.64 35 0.1389 0.1664 0.5802 1. 54. 5.52 7.39 36 0.9941 0.2601 0.9888 1. 49. 5.06 3.35 37 0.9942 0.0260 0.8337 1. 49. 5.04 2.68 38 0.5020 0.1913 0.3037 1. 47. 4.84 7.23 39 0.3775 0.4504 0.1261 1. 47. 4.78 9.27 40 0.0189 0.4111 0.1002 1. 46. 4.69 5.68 41 0.8930 0.4156 0.5158 1. 46. 4.68 9.26 42 0.9828 0.0219 0.7858 1. 45. 4.59 3.45 43 0.9017 0.4911 0.6802 1. 43. 4.41 7.89 44 0.0018 0.3364 0.9942 1. 43. 4.37 4.38 45 0.4796 0.2117 0.0528 1. 42. 4.33 7.72 46 0.9537 0.0648 0.0030 1. 42. 4.28 0.79 47 0.7999 0.1993 0.4579 1. 42. 4.28 7.69 48 0.5819 0.2346 0.0502 1. 42. 4.28 4.85 49 0.4256 0.2381 0.9484 1. 41. 4.18 7.26 50 0.2658 0.4926 0.7900 1. 39. 4.04 8.96 51 0.5181 0.2121 0.9457 1. 39. 4.03 5.62 52 0.4020 0.4094 0.7292 1. 39. 3.96 9.64 53 0.1769 0.3345 0.9269 1. 38. 3.94 5.76 54 0.3192 0.3610 0.4705 1. 38. 3.93 10.72 55 0.8790 0.0227 0.0695 1. 38. 3.87 1.75 56 0.2185 0.3153 0.8992 1. 38. 3.86 6.00 57 0.7804 0.2899 0.3299 1. 37. 3.84 6.26 58 0.4368 0.3605 0.9690 1. 37. 3.75 8.61 59 0.5696 0.3629 0.0360 1. 37. 3.74 5.45 60 0.6773 0.3583 0.5237 1. 36. 3.71 9.15 61 0.9956 0.0974 0.8774 1. 36. 3.71 2.32 62 0.0564 0.0214 0.1039 1. 36. 3.70 1.91 63 0.4200 0.3444 0.9709 1. 36. 3.64 8.26 64 0.9560 0.0273 0.1141 1. 35. 3.62 1.87 65 0.2038 0.2910 0.6705 1. 35. 3.60 7.43 66 0.9892 0.0608 0.1087 1. 35. 3.59 1.89 67 0.2083 0.5045 0.8147 1. 35. 3.58 6.47 68 0.9832 0.0227 0.6828 1. 35. 3.57 5.10 69 0.1669 0.1515 0.2320 1. 35. 3.57 5.16 70 0.4764 0.2796 0.4468 1. 34. 3.52 11.15 71 0.7353 0.3545 0.0996 1. 34. 3.50 4.60 72 0.9157 0.0273 0.9632 1. 34. 3.47 1.16 73 0.9719 0.0219 0.4685 1. 34. 3.47 7.49 74 0.4564 0.0172 0.8187 1. 33. 3.40 6.38 75 0.4464 0.2226 0.6094 1. 33. 3.40 9.42 76 0.8356 0.0611 0.0908 1. 33. 3.33 2.30 77 0.3376 0.0579 0.8834 1. 32. 3.30 4.89 78 0.8304 0.3622 0.4228 1. 32. 3.28 7.90 79 0.4630 0.2626 0.4527 1. 32. 3.24 10.97 80 0.9827 0.0205 0.7176 1. 32. 3.23 4.54 Vectors selected for Patterson superposition: Vector X Y Z Weight Peak Length 1 0.2836 0.4995 0.3863 1. 141. 10.76 FMAP and GRID set by program FMAP 6 3 125 GRID -0.820 -2 -1 0.820 2 1 Patterson vector superposition minimum function for 2005src1629hklf4 in P-1 Patt. sup. on vector 1 0.2836 0.4995 0.3863 Height 141. Length 10.76 Maximum = 140.86, minimum = -493.36 highest memory used = 12878 /238978 0.4 seconds CPU time 188 Superposition peaks employed, maximum height 43.9 and minimum height 4.6 on atomic number scale Heavy-Atom Location for 2005src1629hklf4 in P-1 3297 reflections used for structure factor sums Solution 1 CFOM = 14.58 PATFOM = 74.2 Corr. Coeff. = 44.3 SYMFOM = 36.0 Shift to be added to superposition coordinates: 0.5719 0.6307 0.2835 Name At.No. x y z s.o.f. Minimum distances / PATSMF (self first) BR1 37.4 0.4297 0.3850 0.0882 1.0000 4.89 120.4 FE2 24.5 0.2891 0.1216 0.5227 1.0000 4.90 8.17 63.5 134.4 CL3 17.9 0.3877 0.5270 0.0064 1.0000 2.61 2.15 9.81 0.0 68.5 55.3 CL4 14.9 0.0709 0.4235 0.6021 1.0000 3.93 9.14 3.86 8.10 20.2 59.0 79.9 6.3 CL5 13.4 -0.2256 0.3263 0.5768 1.0000 8.88 6.30 6.42 6.89 4.46 0.0 44.8 56.7 0.0 0.0 CL6 12.9 0.3858 0.7107 0.0015 1.0000 4.97 2.48 9.17 2.38 8.98 7.01 0.0 30.7 32.7 0.0 8.1 0.0 CL7 12.6 0.4137 0.9570 0.0822 1.0000 3.78 4.79 7.26 5.82 9.78 7.40 3.61 0.0 42.0 82.5 12.3 22.9 10.9 0.0 CL8 12.3 0.4281 0.8520 0.0935 1.0000 5.68 3.98 7.36 4.69 9.57 6.57 2.60 1.31 6.6 21.0 11.1 0.0 0.0 0.0 28.3 0.0 CL9 11.3 -0.2836 0.4578 0.4827 1.0000 5.08 7.08 5.43 8.00 3.81 2.18 8.38 8.90 8.05 0.2 88.0 29.0 76.0 24.7 40.6 15.2 31.9 0.0 CL10 10.0 0.0706 0.8404 -0.0335 1.0000 3.87 5.71 8.80 4.39 7.97 7.74 3.67 5.57 5.11 7.93 0.0 54.2 13.3 0.0 0.0 0.0 0.0 0.0 11.0 17.8 N11 9.7 0.0539 0.9321 -0.0378 1.0000 2.05 8.76 8.25 5.22 8.65 7.98 4.02 5.16 4.97 8.36 1.12 0.0 10.7 26.5 10.5 15.8 11.7 22.3 7.0 15.2 0.0 16.2 N12 9.7 -0.1873 0.4171 0.4978 1.0000 5.97 7.13 5.57 8.13 3.36 1.90 8.88 9.29 8.41 1.14 7.95 8.36 0.0 23.1 20.2 0.0 0.0 10.2 0.0 5.9 5.2 8.1 0.0 0.0 N13 9.3 0.0900 0.3276 0.6035 1.0000 5.32 9.26 3.00 8.05 1.16 4.03 8.62 7.87 7.56 4.58 7.63 7.81 3.69 0.0 3.4 25.8 0.0 10.8 2.2 0.0 12.7 25.8 4.2 12.6 2.6 0.0 Solution 2 CFOM = 12.76 PATFOM = 99.9 Corr. Coeff. = 35.7 SYMFOM = 44.9 Shift to be added to superposition coordinates: 0.3307 0.4675 0.2590 Name At.No. x y z s.o.f. Minimum distances / PATSMF (self first) BR1 37.4 0.4728 0.7138 0.4525 1.0000 5.51 87.9 FE2 23.2 0.8115 0.7766 0.9354 1.0000 9.24 9.25 75.5 153.1 FE3 23.0 0.6706 1.0134 1.1180 1.0000 6.01 7.50 3.99 7.3 52.9 65.3 CL4 18.6 0.3299 0.9498 0.6350 1.0000 6.43 3.98 7.51 3.98 2.6 54.3 43.4 0.0 CL5 18.0 0.5130 0.8592 0.5421 1.0000 3.78 2.61 7.37 5.74 2.49 14.0 75.9 61.7 0.0 0.0 CL6 13.4 0.8289 0.6782 0.9440 1.0000 5.20 9.20 1.21 4.76 7.82 7.60 0.0 35.7 80.2 38.0 29.1 6.0 CL7 12.9 0.6675 0.5176 0.3721 1.0000 5.87 2.91 8.19 7.62 6.05 4.79 7.57 14.5 32.4 7.5 5.8 2.0 41.0 39.2 CL8 11.1 0.0309 1.0787 0.4900 1.0000 2.49 5.56 7.44 7.34 4.24 5.61 8.03 5.97 0.0 48.8 24.8 29.6 0.0 0.0 6.5 0.0 CL9 10.8 1.0000 1.0000 1.0000 0.5000 12.60 9.37 4.62 4.39 6.83 10.48 5.55 10.56 7.97 999.0 42.5 28.7 11.0 0.0 11.1 15.9 7.3 0.0 CL10 10.6 0.8723 1.2302 1.0350 1.0000 5.52 8.87 4.01 4.67 6.58 8.47 4.44 6.32 7.70 2.76 0.0 14.0 10.3 0.0 0.0 0.0 0.0 17.9 0.0 0.0 CL11 10.4 0.6269 0.8697 1.0272 1.0000 3.67 7.48 2.50 2.62 6.05 7.51 2.94 7.06 9.23 5.63 6.63 0.0 69.1 51.0 0.0 0.0 85.0 19.1 1.2 2.6 0.0 0.0 N12 9.7 1.0000 0.5000 0.5000 0.5000 12.60 7.58 7.62 10.96 8.83 5.91 7.39 4.69 5.32 10.32 8.76 9.34 999.0 13.2 66.9 21.6 0.0 0.0 0.0 0.0 27.4 20.8 18.6 5.0 N13 9.3 0.6169 1.4584 1.0138 1.0000 2.73 7.56 5.74 5.77 7.58 8.63 4.76 5.90 9.60 5.84 3.35 5.40 9.54 0.0 27.1 57.7 1.7 13.7 20.3 2.1 11.5 0.0 9.7 0.0 0.5 58.8 N14 9.2 1.0310 0.4718 0.8535 1.0000 4.72 7.24 3.91 5.83 9.12 8.15 3.09 5.13 7.75 6.71 4.90 5.15 5.70 0.0 45.1 12.0 0.0 0.0 15.5 21.1 19.9 0.0 2.3 10.8 0.0 23.9 Solution 3 CFOM = 12.76 PATFOM = 61.7 Corr. Coeff. = 45.5 SYMFOM = 99.9 Shift to be added to superposition coordinates: 0.4997 0.4995 0.4998 Name At.No. x y z s.o.f. Minimum distances / PATSMF (self first) BR1 37.4 0.6416 0.7463 0.6933 1.0000 10.69 221.8 FE2 23.9 0.5009 0.5165 0.8689 1.0000 4.22 4.88 17.5 120.7 FE3 22.6 0.5007 0.9814 0.8768 1.0000 3.97 3.99 6.03 0.0 131.7 6.2 CL4 20.3 0.6576 1.1722 0.7007 1.0000 9.77 5.62 4.80 4.63 3.2 111.8 40.9 0.0 CL5 19.4 0.7044 1.1973 0.7935 1.0000 10.72 6.45 3.97 4.69 1.71 0.0 88.8 45.3 7.8 2.0 CL6 17.6 0.6958 1.3188 0.7881 1.0000 8.30 5.51 2.92 6.00 2.59 1.54 0.0 88.1 14.1 51.4 16.6 12.8 CL7 17.6 0.6454 1.3270 0.6974 1.0000 7.88 5.42 3.54 6.16 1.95 2.19 1.61 19.1 87.3 0.0 0.0 77.5 28.8 0.0 CL8 17.0 1.0009 1.2892 0.8169 1.0000 8.03 6.14 5.71 5.98 5.57 4.42 3.75 4.81 0.0 80.4 48.2 29.3 0.0 0.0 11.6 25.6 CL9 16.1 0.4595 0.6589 0.7880 1.0000 7.82 3.27 2.15 4.67 5.85 5.44 4.14 4.14 8.15 0.0 73.2 6.1 0.0 13.6 0.0 5.6 59.6 0.2 CL10 15.5 1.0174 1.1985 0.8200 1.0000 7.84 9.27 8.77 5.64 5.17 4.00 3.74 4.80 1.11 8.06 1.8 75.6 1.4 42.1 6.6 6.7 0.0 0.0 12.9 0.0 CL11 15.3 0.8602 1.4399 0.6117 1.0000 5.55 3.92 5.69 9.73 5.27 5.18 4.10 3.78 3.93 5.26 4.50 12.0 64.2 9.9 0.0 24.4 5.4 1.9 42.5 24.0 0.0 6.5 CL12 15.2 0.4566 0.8400 0.7858 1.0000 8.39 2.51 4.22 2.61 5.98 6.61 7.50 7.75 6.19 2.34 5.50 6.04 0.0 69.2 6.5 0.0 53.7 0.0 0.0 23.3 12.5 0.0 0.0 3.1 CL13 14.0 0.2160 0.5091 0.7447 1.0000 9.86 7.25 4.24 8.54 5.42 5.84 5.56 4.90 4.80 4.36 5.68 5.48 6.28 2.8 59.1 2.0 1.6 18.5 3.8 26.5 13.2 12.0 0.0 0.0 0.0 0.0 CL14 14.0 0.2260 0.9864 0.7378 1.0000 9.69 4.83 6.03 4.20 6.83 7.71 8.46 7.80 3.90 4.12 3.11 6.15 2.86 0.0 66.6 5.8 5.4 15.8 2.7 0.0 0.0 8.9 15.4 19.9 0.0 7.2 CL15 13.3 0.6842 0.6051 0.7749 1.0000 9.36 2.14 3.28 4.67 5.90 5.20 3.66 4.05 4.42 2.61 5.23 3.41 3.17 0.0 51.1 0.0 0.0 17.0 0.0 13.0 4.4 0.5 0.0 3.1 0.0 0.0 CL16 12.9 1.1963 1.3932 0.7242 1.0000 8.72 6.89 5.39 5.72 5.26 7.67 6.10 5.34 3.53 5.84 4.27 4.50 7.88 1.4 47.3 7.3 0.0 0.0 0.0 2.9 7.7 0.0 20.3 0.0 2.6 0.0 CL17 12.7 0.6842 0.8900 0.7859 1.0000 7.86 2.63 6.31 2.48 3.79 4.11 5.63 5.66 7.52 4.93 6.97 5.93 3.20 0.3 60.6 0.0 0.0 15.2 0.0 0.0 22.3 0.7 5.2 0.0 6.2 0.0 CL18 12.7 1.2172 1.4108 0.7219 1.0000 8.92 6.86 5.04 5.82 5.06 5.74 5.79 5.02 3.93 5.44 4.67 4.79 7.48 20.7 46.3 12.3 0.0 18.1 29.6 13.0 9.3 0.2 8.4 5.5 0.0 3.2 CL19 12.5 0.4788 0.6756 0.7927 1.0000 7.96 2.97 2.32 4.32 7.79 5.62 4.25 4.33 8.31 0.40 8.18 5.17 2.03 0.0 58.1 17.8 0.0 24.7 0.0 10.1 45.3 2.8 0.0 0.6 0.0 1.3 Maximum memory for Patterson interpretation = 4313 / 3822 0.9 seconds CPU time +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2005src1629hklf4 finished at 15:12:22 Total CPU time: 1.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++