#------------------------------------------------------------------------------ #$Date: 2011-09-28 17:24:46 +0300 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/01/38/2013863.hkl $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2013863_Fobs loop_ _publ_author_name 'Blake, Alexander J.' 'Lippolis, Vito' 'Schr\"oder, Martin' _publ_section_title ; Intramolecular cyclization of 4,7-bis(2-bromoacetyl)-1-thia-4,7-diazacyclononane ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first o100 _journal_page_last o102 _journal_volume 60 _journal_year 2004 _space_group_IT_number 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 86.665 _cell_angle_beta 75.553 _cell_angle_gamma 83.068 _cell_length_a 7.2655 _cell_length_b 9.5032 _cell_length_c 10.0740 _exptl_crystal_F_000 384.00 _reflns_d_resolution_high 0.8380 _[local]_cod_data_source_file sk1685Isup2.hkl _[local]_cod_data_source_block I #BEGIN Tags that were not found in dictionaries: _shelx_title ' BRCONS #393 for VL/MS in P-1.' _shelx_refln_list_code 4 _shelx_f_calc_maximum 166.17 _shelx_f_squared_multiplier 1.000 #END Tags that were not found in dictionaries loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_calc _refln_F_squared_meas _refln_F_squared_sigma _refln_observed_status 1 0 0 68.94 57.09 2.12 o 2 0 0 1988.66 2232.14 14.04 o 3 0 0 1601.89 1723.05 15.26 o 4 0 0 181.92 187.83 6.90 o 5 0 0 12.39 6.16 4.41 o 6 0 0 517.41 447.65 13.22 o 7 0 0 476.73 465.03 15.50 o 8 0 0 369.98 356.45 15.63 o -8 1 0 23.47 16.09 6.18 o -7 1 0 1019.53 1072.41 23.73 o -6 1 0 3642.49 3720.16 36.18 o -5 1 0 35.49 31.13 5.81 o -4 1 0 2281.04 2449.70 22.43 o -3 1 0 5689.28 5857.76 29.30 o -2 1 0 1563.82 1756.65 12.71 o -1 1 0 3079.26 3208.10 12.61 o 0 1 0 94.61 106.94 2.52 o 1 1 0 19.12 11.04 2.76 o 2 1 0 127.21 90.85 4.38 o 3 1 0 2545.39 2594.06 20.12 o 4 1 0 8856.09 9751.75 45.57 o 5 1 0 236.91 196.86 8.71 o 6 1 0 602.77 531.49 14.92 o 7 1 0 338.57 346.34 14.09 o 8 1 0 61.38 48.49 9.40 o -8 2 0 17.85 18.44 6.87 o -7 2 0 154.35 103.19 10.83 o -6 2 0 409.45 387.82 13.56 o -5 2 0 847.68 916.88 16.83 o -4 2 0 2632.21 2782.61 23.65 o -3 2 0 3576.54 3715.25 22.93 o -2 2 0 5130.10 5436.21 23.17 o -1 2 0 1078.90 1123.10 9.32 o 0 2 0 12984.37 13270.41 39.87 o 1 2 0 6390.32 6052.05 25.08 o 2 2 0 24.82 18.66 4.14 o 3 2 0 130.86 87.27 5.92 o 4 2 0 228.18 183.30 8.15 o 5 2 0 319.86 303.79 11.01 o 6 2 0 20.93 13.01 6.16 o 7 2 0 3099.52 3346.46 38.46 o 8 2 0 483.69 452.40 18.18 o -7 3 0 437.46 409.89 11.09 o -6 3 0 1692.95 1684.16 26.20 o -5 3 0 2198.94 2151.80 25.48 o -4 3 0 388.87 397.35 10.51 o -3 3 0 884.21 872.87 12.50 o -2 3 0 4154.85 4492.12 23.65 o -1 3 0 3395.34 3742.06 20.70 o 0 3 0 5873.07 6383.10 26.28 o 1 3 0 6301.07 7068.75 29.83 o 2 3 0 2505.51 2220.83 18.79 o 3 3 0 381.27 280.25 9.87 o 4 3 0 7266.05 8167.19 49.02 o 5 3 0 569.79 524.81 14.70 o 6 3 0 565.27 546.20 16.91 o 7 3 0 341.29 325.69 15.26 o 8 3 0 79.04 68.90 11.12 o -7 4 0 127.56 122.57 10.15 o -6 4 0 520.99 465.43 15.08 o -5 4 0 184.34 160.50 9.10 o -4 4 0 13.99 8.81 4.49 o -3 4 0 5337.87 5552.67 31.98 o -2 4 0 6492.42 6836.83 33.31 o -1 4 0 846.48 924.65 12.50 o 0 4 0 629.86 657.06 10.48 o 1 4 0 4645.49 5425.64 28.51 o 2 4 0 2.71 3.48 3.85 o 3 4 0 316.16 212.09 8.55 o 4 4 0 1225.93 1271.15 21.66 o 5 4 0 1629.92 1767.35 27.02 o 6 4 0 32.85 35.72 8.36 o 7 4 0 604.32 569.53 19.80 o 8 4 0 1647.17 1836.65 35.19 o -7 5 0 54.91 40.06 8.97 o -6 5 0 3000.81 3017.58 35.80 o -5 5 0 681.95 657.11 16.06 o -4 5 0 163.27 168.94 8.71 o -3 5 0 42.55 44.93 5.57 o -2 5 0 3.23 5.31 4.41 o -1 5 0 448.10 484.30 10.88 o 0 5 0 720.24 737.54 12.90 o 1 5 0 3529.79 3859.67 28.27 o 2 5 0 7679.98 8551.49 44.88 o 3 5 0 51.66 36.10 5.73 o 4 5 0 399.40 332.51 12.69 o 5 5 0 2681.38 2795.06 36.36 o 6 5 0 2.21 -13.56 7.48 o 7 5 0 19.00 18.00 9.42 o -6 6 0 11.00 19.11 7.99 o -5 6 0 1318.44 1208.89 21.98 o -4 6 0 272.31 241.69 10.99 o -3 6 0 1282.38 1329.41 20.84 o -2 6 0 3579.95 3651.82 32.12 o -1 6 0 771.34 821.94 15.23 o 0 6 0 61.73 34.98 5.36 o 1 6 0 33.57 16.48 4.86 o 2 6 0 12.96 3.74 4.86 o 3 6 0 1019.93 1033.45 18.87 o 4 6 0 2985.99 2662.14 32.04 o 5 6 0 957.44 729.92 20.68 o 6 6 0 1146.05 1053.64 26.17 o 7 6 0 66.82 47.72 10.96 o -5 7 0 840.74 863.05 20.89 o -4 7 0 76.42 96.98 9.40 o -3 7 0 390.44 415.48 14.44 o -2 7 0 883.98 926.38 18.66 o -1 7 0 1234.99 1340.98 20.78 o 0 7 0 1682.84 1834.81 23.57 o 1 7 0 4559.00 4917.98 37.95 o 2 7 0 2809.87 3383.09 33.07 o 3 7 0 859.01 847.76 19.08 o 4 7 0 16.85 14.09 7.22 o 5 7 0 194.25 115.40 11.49 o 6 7 0 6.23 -3.03 8.81 o 7 7 0 0.72 0.56 9.98 o -5 8 0 1250.22 1190.07 27.23 o -4 8 0 402.11 387.59 16.35 o -3 8 0 51.35 24.50 8.17 o -2 8 0 675.74 675.77 18.21 o -1 8 0 82.25 89.74 8.73 o 0 8 0 1709.17 1769.97 25.93 o 1 8 0 4.28 -7.22 5.92 o 2 8 0 819.13 908.62 20.07 o 3 8 0 222.09 245.51 12.69 o 4 8 0 0.95 6.87 7.88 o 5 8 0 1493.23 1312.58 28.53 o 6 8 0 1254.82 1099.32 29.25 o -4 9 0 111.83 98.68 12.18 o -3 9 0 7.75 -5.60 8.28 o -2 9 0 213.84 192.88 12.63 o -1 9 0 2951.46 3085.93 36.95 o 0 9 0 892.01 773.82 19.64 o 1 9 0 170.56 116.57 10.30 o 2 9 0 2459.98 2757.03 35.75 o 3 9 0 68.25 65.27 9.90 o 4 9 0 133.91 99.66 11.60 o 5 9 0 41.35 46.74 10.38 o -3 10 0 10.92 23.54 10.75 o -2 10 0 44.60 49.00 10.40 o -1 10 0 458.43 435.84 17.60 o 0 10 0 0.20 2.68 7.67 o 1 10 0 13.78 10.17 8.15 o 2 10 0 460.27 448.13 17.73 o 3 10 0 550.26 485.05 18.92 o 4 10 0 390.53 333.33 18.42 o -1 11 0 363.69 280.68 17.04 o 0 11 0 613.34 476.98 20.07 o 1 11 0 145.22 82.41 12.08 o 2 11 0 84.26 58.87 11.55 o -2 -11 1 1.45 7.99 9.79 o -1 -11 1 61.07 78.24 11.25 o 0 -11 1 304.45 326.41 16.80 o -4 -10 1 175.50 163.63 15.10 o -3 -10 1 1459.08 1683.66 31.85 o -2 -10 1 65.58 49.26 10.25 o -1 -10 1 98.35 113.60 11.23 o 0 -10 1 1949.05 2180.84 33.81 o 1 -10 1 111.71 144.17 12.10 o 2 -10 1 13.97 7.94 9.08 o 3 -10 1 0.11 8.47 8.20 o -5 -9 1 36.10 36.26 11.31 o -4 -9 1 59.75 77.77 11.07 o -3 -9 1 619.19 732.20 20.86 o -2 -9 1 92.44 84.38 9.90 o -1 -9 1 495.25 512.57 16.64 o 0 -9 1 187.82 170.93 11.41 o 1 -9 1 1091.89 1143.62 23.78 o 2 -9 1 100.71 76.78 9.24 o 3 -9 1 522.47 444.54 16.08 o 4 -9 1 340.23 301.78 14.81 o -6 -8 1 59.45 71.53 12.53 o -5 -8 1 87.38 107.44 11.92 o -4 -8 1 309.95 316.80 15.39 o -3 -8 1 2158.39 2630.87 34.00 o -2 -8 1 898.87 1042.42 21.42 o -1 -8 1 271.08 246.57 11.01 o 0 -8 1 745.08 759.91 17.97 o 1 -8 1 285.24 319.93 13.08 o 2 -8 1 531.95 562.97 15.26 o 3 -8 1 264.99 273.83 12.37 o 4 -8 1 1813.43 1762.81 28.61 o 5 -8 1 102.76 99.27 10.51 o -6 -7 1 474.70 469.20 20.46 o -5 -7 1 285.39 307.64 15.95 o -4 -7 1 661.21 697.54 19.53 o -3 -7 1 654.91 799.54 19.24 o -2 -7 1 5.02 10.38 5.81 o -1 -7 1 7.51 16.83 5.39 o 0 -7 1 669.43 719.67 15.42 o 1 -7 1 3798.52 4045.27 33.79 o 2 -7 1 513.30 461.82 12.50 o 3 -7 1 27.96 24.58 5.81 o 4 -7 1 2267.99 2135.24 28.27 o 5 -7 1 33.12 34.50 7.99 o 6 -7 1 39.13 18.39 8.63 o -7 -6 1 0.96 5.73 10.11 o -6 -6 1 732.04 732.89 21.90 o -5 -6 1 219.42 216.39 13.88 o -4 -6 1 95.49 82.54 9.16 o -3 -6 1 4617.26 4894.60 39.94 o -2 -6 1 1653.50 1956.64 23.38 o -1 -6 1 29.40 22.72 5.10 o 0 -6 1 10.21 9.82 4.33 o 1 -6 1 2.08 -5.31 3.53 o 2 -6 1 355.88 328.03 9.98 o 3 -6 1 308.25 296.34 10.40 o 4 -6 1 1544.09 1514.46 22.56 o 5 -6 1 2437.45 2358.11 30.15 o 6 -6 1 185.47 172.57 11.60 o -7 -5 1 1.57 5.18 9.63 o -6 -5 1 877.04 863.50 23.52 o -5 -5 1 572.87 545.19 17.60 o -4 -5 1 16.80 16.61 7.27 o -3 -5 1 117.59 88.30 7.33 o -2 -5 1 890.90 971.34 16.06 o -1 -5 1 4136.21 4639.48 29.89 o 0 -5 1 1851.59 1920.65 19.51 o 1 -5 1 7436.82 7838.50 37.58 o 2 -5 1 1825.63 1759.41 19.14 o 3 -5 1 180.63 170.37 7.75 o 4 -5 1 8.37 3.08 4.75 o 5 -5 1 318.07 282.27 11.52 o 6 -5 1 112.93 129.95 9.77 o 7 -5 1 2.05 -6.66 7.17 o -7 -4 1 9.99 8.55 9.53 o -6 -4 1 901.09 1041.65 23.62 o -5 -4 1 3046.24 3386.11 37.45 o -4 -4 1 16.61 19.69 6.16 o -3 -4 1 955.75 831.81 16.96 o -2 -4 1 926.27 904.40 14.17 o -1 -4 1 1424.46 1484.71 15.74 o 0 -4 1 153.21 112.70 5.12 o 1 -4 1 1427.97 1445.56 14.76 o 2 -4 1 34.26 19.06 3.64 o 3 -4 1 3846.02 4046.09 27.66 o 4 -4 1 4137.75 4202.50 30.87 o 5 -4 1 2479.65 2500.79 27.68 o 6 -4 1 144.15 126.18 9.24 o 7 -4 1 4.59 8.28 7.03 o -8 -3 1 434.36 353.21 12.67 o -7 -3 1 16.16 24.87 9.10 o -6 -3 1 123.61 120.21 10.25 o -5 -3 1 121.46 91.25 8.60 o -4 -3 1 306.40 317.04 10.91 o -3 -3 1 134.77 175.94 7.83 o -2 -3 1 9726.42 8571.08 41.46 o -1 -3 1 4696.79 4938.74 24.76 o 0 -3 1 376.35 314.60 6.32 o 1 -3 1 4597.82 4912.62 23.81 o 2 -3 1 3927.46 4070.17 23.01 o 3 -3 1 773.36 773.07 11.86 o 4 -3 1 620.70 644.93 12.39 o 5 -3 1 431.91 441.07 11.81 o 6 -3 1 565.37 549.91 14.97 o 7 -3 1 42.24 22.53 7.17 o -8 -2 1 170.33 174.76 20.97 o -7 -2 1 251.81 254.08 14.39 o -6 -2 1 195.66 207.32 11.60 o -5 -2 1 4883.82 5469.01 41.30 o -4 -2 1 1100.30 1085.28 17.09 o -3 -2 1 972.80 1020.36 14.57 o -2 -2 1 6593.42 7209.92 32.33 o -1 -2 1 1095.41 1210.24 11.47 o 0 -2 1 0.41 3.48 2.36 o 1 -2 1 4762.37 5317.03 21.23 o 2 -2 1 4895.45 4973.64 22.64 o 3 -2 1 1390.93 1455.64 14.97 o 4 -2 1 452.31 446.80 10.09 o 5 -2 1 1837.77 1808.51 21.55 o 6 -2 1 1025.60 1073.76 19.53 o 7 -2 1 0.18 13.80 6.56 o 8 -2 1 3.43 -6.77 7.72 o -8 -1 1 509.96 519.91 37.73 o -7 -1 1 1.80 0.19 7.88 o -6 -1 1 140.10 129.84 9.82 o -5 -1 1 67.35 60.33 6.87 o -4 -1 1 1065.17 1079.28 16.22 o -3 -1 1 74.26 61.20 4.94 o -2 -1 1 4558.15 5179.04 24.58 o -1 -1 1 27612.26 26538.85 86.58 o 0 -1 1 116.28 85.68 3.42 o 1 -1 1 37.13 47.19 2.79 o 2 -1 1 13681.39 14291.70 41.46 o 3 -1 1 133.48 146.16 5.26 o 4 -1 1 799.02 858.91 13.24 o 5 -1 1 1632.46 1682.20 20.46 o 6 -1 1 854.57 842.69 17.52 o 7 -1 1 1154.83 1174.36 22.37 o 8 -1 1 547.54 497.97 17.97 o -8 0 1 674.13 650.20 46.91 o -7 0 1 1976.90 2031.04 32.51 o -6 0 1 463.50 468.30 14.84 o -5 0 1 1829.81 2082.53 25.19 o -4 0 1 3890.81 4046.07 29.46 o -3 0 1 16.62 18.90 3.90 o -2 0 1 87.30 42.84 3.72 o -1 0 1 342.58 360.65 5.23 o 0 0 1 48.04 27.31 1.38 o 1 0 1 175.16 150.22 3.61 o 2 0 1 3588.72 3714.83 18.26 o 3 0 1 4729.41 4899.51 25.85 o 4 0 1 1325.52 1380.34 16.32 o 5 0 1 1064.98 1059.51 17.12 o 6 0 1 523.80 458.82 13.51 o 7 0 1 6.61 14.60 6.58 o 8 0 1 44.49 43.77 9.26 o -8 1 1 74.44 68.00 7.48 o -7 1 1 409.59 452.67 17.12 o -6 1 1 217.05 213.26 11.33 o 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2948.95 3052.27 23.22 o -2 3 1 50.84 57.86 3.90 o -1 3 1 1109.27 1250.29 12.93 o 0 3 1 8732.78 9522.70 32.86 o 1 3 1 186.82 177.16 5.47 o 2 3 1 1201.79 1112.81 13.40 o 3 3 1 292.18 207.87 8.02 o 4 3 1 3428.36 3433.86 31.32 o 5 3 1 2.67 2.15 5.20 o 6 3 1 2251.05 2553.21 32.25 o 7 3 1 994.76 1031.30 24.07 o 8 3 1 95.50 120.31 12.26 o -7 4 1 1499.71 1456.15 54.36 o -6 4 1 883.49 902.46 21.60 o -5 4 1 30.73 15.55 6.42 o -4 4 1 709.20 710.17 14.20 o -3 4 1 29.25 43.61 4.80 o -2 4 1 1949.46 2125.68 20.15 o -1 4 1 2198.25 2257.65 19.16 o 0 4 1 4880.19 5203.68 27.66 o 1 4 1 8360.69 9109.34 37.87 o 2 4 1 1906.97 1922.37 18.63 o 3 4 1 874.95 666.06 13.08 o 4 4 1 2404.41 2264.95 26.62 o 5 4 1 1.86 -2.44 5.71 o 6 4 1 27.97 13.80 7.19 o 7 4 1 163.67 185.29 12.66 o 8 4 1 234.01 224.14 14.57 o -6 5 1 890.57 670.76 19.14 o -5 5 1 66.24 53.08 7.59 o -4 5 1 1956.22 1951.65 23.83 o -3 5 1 1669.90 1772.79 21.31 o -2 5 1 2272.91 2426.13 24.18 o -1 5 1 295.72 289.44 9.02 o 1 5 1 245.85 248.14 8.04 o 2 5 1 10.92 7.56 4.11 o 3 5 1 2367.54 2164.35 24.29 o 4 5 1 2246.14 1968.82 26.33 o 5 5 1 1707.10 1676.04 28.08 o 6 5 1 641.07 573.56 18.92 o 7 5 1 605.62 514.08 19.59 o 8 5 1 74.95 75.96 12.10 o -6 6 1 247.02 206.15 13.27 o -5 6 1 27.46 17.36 6.87 o -4 6 1 61.21 67.84 7.80 o -3 6 1 1463.54 1453.12 22.59 o -2 6 1 826.24 893.92 16.99 o -1 6 1 599.29 653.56 13.85 o 0 6 1 6844.59 7612.02 42.31 o 1 6 1 3270.28 3811.68 29.83 o 2 6 1 2434.18 2690.30 26.86 o 3 6 1 489.70 398.04 12.29 o 4 6 1 1201.92 934.26 19.51 o 5 6 1 329.85 259.84 13.03 o 6 6 1 125.73 71.77 10.72 o 7 6 1 264.15 255.06 15.79 o -5 7 1 241.70 227.67 12.82 o -4 7 1 127.09 112.96 10.27 o -3 7 1 1973.30 2090.38 29.35 o -2 7 1 759.60 840.62 18.58 o -1 7 1 525.24 542.83 14.25 o 0 7 1 4.10 10.59 5.28 o 1 7 1 1871.43 2166.21 26.38 o 2 7 1 9.12 7.67 5.39 o 3 7 1 555.27 551.11 15.23 o 4 7 1 1070.16 851.37 19.77 o 5 7 1 1836.56 1600.96 28.69 o 6 7 1 1.12 3.88 8.84 o 7 7 1 88.39 60.89 11.52 o -5 8 1 166.28 130.98 12.55 o -4 8 1 155.63 148.10 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350.67 392.71 15.85 o 2 2 11 842.86 935.32 23.68 o 3 2 11 97.88 108.66 10.17 o 4 2 11 851.30 881.52 23.46 o 5 2 11 1443.54 1760.60 35.62 o 0 3 11 2.07 -10.46 6.82 o 1 3 11 486.13 437.43 16.96 o 2 3 11 253.64 136.42 11.39 o 3 3 11 1.73 -1.83 6.79 o 4 3 11 122.33 93.93 10.48 o 1 4 11 356.58 330.36 15.13 o 2 4 11 667.60 711.66 20.73 o 3 4 11 726.81 724.21 20.86 o 4 4 11 174.11 205.11 12.98 o 2 5 11 0.17 9.66 7.59 o