#------------------------------------------------------------------------------ #$Date: 2016-04-02 22:21:09 +0300 (Sat, 02 Apr 2016) $ #$Revision: 180853 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/01/84/2018429.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_2018429_Fobs loop_ _publ_author_name 'Blanco, Maria C.' 'Palma, Alirio' 'Cobo, Justo' 'Glidewell, Christopher' _publ_section_title ; Nine closely related tetrahydro-1,4-epoxy-1-benzazepines carrying pendant heterocyclic substituents: hydrogen-bonded supramolecular assembly in zero, one and two dimensions ; _journal_coeditor_code SK3430 _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first o131 _journal_page_last o140 _journal_volume 68 _journal_year 2012 _space_group_IT_number 15 _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _cell_angle_alpha 90.000 _cell_angle_beta 103.275 _cell_angle_gamma 90.000 _cell_length_a 27.1405 _cell_length_b 5.4082 _cell_length_c 17.2849 _exptl_crystal_F_000 1088.00 _reflns_d_resolution_high 0.7696 _cod_data_source_file sk3430IIsup3.hkl _cod_data_source_block II #BEGIN Tags that were not found in dictionaries: _shelx_title ' CAB139' _shelx_refln_list_code 4 _shelx_f_calc_maximum 293.01 _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+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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 4 0 0 43557.94 39763.51 658.58 o 6 0 0 30140.65 29411.41 418.80 o 8 0 0 4847.87 4765.19 88.53 o 10 0 0 942.71 902.05 29.21 o 12 0 0 12234.00 12762.44 200.45 o 14 0 0 8.98 6.52 16.94 o 16 0 0 5534.93 6234.24 139.98 o 18 0 0 5266.22 6102.14 156.90 o 20 0 0 200.05 171.47 39.57 o 22 0 0 81.17 71.57 40.58 o 24 0 0 1760.80 2088.64 108.34 o 26 0 0 6.41 145.29 55.01 o 28 0 0 230.88 118.93 70.03 o 30 0 0 158.33 120.30 69.11 o 32 0 0 13.95 98.65 95.46 o 34 0 0 17.09 -114.13 118.00 o 1 1 0 6709.00 6116.18 84.64 o 3 1 0 1002.66 989.83 14.86 o 5 1 0 4129.17 3756.43 44.56 o 7 1 0 758.19 692.65 15.42 o 9 1 0 777.75 757.36 17.56 o 11 1 0 843.08 855.62 19.99 o 13 1 0 1992.42 2029.82 35.40 o 15 1 0 3861.68 4154.44 71.78 o 17 1 0 2.18 21.36 20.04 o 19 1 0 1.67 19.68 23.55 o 21 1 0 4.20 -11.18 29.57 o 23 1 0 886.66 837.22 46.09 o 25 1 0 663.32 754.61 58.71 o 27 1 0 1223.46 1148.50 65.95 o 29 1 0 163.40 73.07 46.57 o 31 1 0 111.31 124.52 52.82 o 33 1 0 63.17 67.82 59.56 o 0 2 0 13.61 24.76 10.30 o 2 2 0 14.73 10.39 8.39 o 4 2 0 10.92 11.12 8.99 o 6 2 0 1512.80 1433.91 23.90 o 8 2 0 49.58 -2.64 10.03 o 10 2 0 316.66 273.45 18.48 o 12 2 0 445.94 465.25 18.75 o 14 2 0 97.02 72.51 18.89 o 16 2 0 688.39 646.88 36.97 o 18 2 0 440.63 433.86 30.98 o 20 2 0 880.71 838.75 40.11 o 22 2 0 48.99 -23.78 29.81 o 24 2 0 2203.22 2257.27 74.95 o 26 2 0 0.04 60.59 44.34 o 28 2 0 366.70 454.05 54.21 o 30 2 0 10.68 -5.95 46.65 o 32 2 0 14.58 11.38 54.82 o 1 3 0 594.43 640.59 18.20 o 3 3 0 2668.11 2906.45 42.78 o 5 3 0 1078.98 1291.36 32.66 o 7 3 0 261.46 221.79 14.14 o 9 3 0 2983.57 3029.27 51.95 o 11 3 0 1010.25 928.81 28.28 o 13 3 0 313.82 312.34 22.97 o 15 3 0 1887.14 1888.61 51.73 o 17 3 0 190.88 229.62 31.27 o 19 3 0 444.43 465.97 38.24 o 21 3 0 1007.39 967.65 56.73 o 23 3 0 0.35 2.63 38.51 o 25 3 0 234.56 183.37 45.08 o 27 3 0 93.54 48.76 46.19 o 29 3 0 50.80 82.24 50.97 o 31 3 0 0.32 -32.59 58.53 o 0 4 0 669.24 756.50 35.23 o 2 4 0 821.28 858.13 26.84 o 4 4 0 29.19 10.88 17.35 o 6 4 0 159.65 132.78 24.59 o 8 4 0 793.56 827.92 36.07 o 10 4 0 63.43 25.59 21.39 o 12 4 0 2565.39 2775.78 72.01 o 14 4 0 68.69 61.66 30.90 o 16 4 0 2422.18 2766.78 80.64 o 18 4 0 2.03 24.92 36.71 o 20 4 0 114.92 110.68 41.14 o 22 4 0 152.82 136.40 44.89 o 24 4 0 358.52 352.37 52.79 o 26 4 0 569.35 588.37 73.16 o 28 4 0 665.25 700.14 133.08 o 1 5 0 480.06 491.07 31.02 o 3 5 0 1274.59 1383.24 66.64 o 5 5 0 366.74 401.13 36.32 o 7 5 0 11.57 17.86 42.63 o 9 5 0 161.91 86.12 38.39 o 11 5 0 607.52 603.71 49.73 o 13 5 0 0.75 96.50 54.31 o 15 5 0 122.15 34.11 52.74 o 17 5 0 21.50 95.13 53.42 o 19 5 0 261.05 242.09 57.96 o 21 5 0 72.79 66.50 60.94 o 23 5 0 22.44 42.63 64.82 o 0 6 0 685.81 802.66 112.39 o 2 6 0 0.45 22.28 46.91 o 4 6 0 192.49 69.85 57.20 o 6 6 0 1.19 36.46 67.13 o 8 6 0 494.64 519.69 80.90 o 10 6 0 57.21 97.66 102.02 o 12 6 0 1131.96 1115.55 93.60 o 14 6 0 6.77 -34.58 65.76 o 16 6 0 38.44 107.48 68.14 o 1 7 0 343.74 304.19 96.60 o 3 7 0 93.01 106.06 93.16 o -33 1 1 0.33 8.21 56.92 o -31 1 1 43.80 54.79 50.24 o -29 1 1 321.01 369.63 52.38 o -27 1 1 392.40 336.65 48.25 o -25 1 1 1194.51 1284.71 81.00 o -23 1 1 34.78 -35.94 35.94 o -21 1 1 467.89 417.08 34.89 o -19 1 1 1782.60 1791.36 62.34 o -17 1 1 149.98 111.32 29.39 o -15 1 1 398.63 382.13 18.92 o -13 1 1 7691.31 7969.61 91.16 o -11 1 1 1939.27 1869.76 30.61 o -9 1 1 4195.88 4140.17 50.57 o -7 1 1 1325.54 1282.69 21.79 o -5 1 1 30.64 39.40 7.38 o -3 1 1 517.89 454.80 8.94 o -1 1 1 26601.37 26077.85 237.30 o 1 1 1 5233.44 5013.05 54.28 o 3 1 1 8833.21 8404.20 90.12 o 5 1 1 4711.05 4470.68 53.11 o 7 1 1 85.88 96.01 9.43 o 9 1 1 11.83 -8.59 8.59 o 11 1 1 67.22 78.28 11.04 o 13 1 1 3600.98 3644.46 53.45 o 15 1 1 146.41 100.62 17.90 o 17 1 1 1916.97 1956.51 52.18 o 19 1 1 1299.44 1366.56 49.99 o 21 1 1 32.56 -1.50 27.85 o 23 1 1 287.07 359.96 37.66 o 25 1 1 575.29 461.20 48.45 o 27 1 1 134.03 184.28 46.34 o 29 1 1 1.17 -4.50 46.65 o 31 1 1 24.84 31.23 48.14 o 33 1 1 43.37 -34.08 57.04 o -32 2 1 7.90 115.02 56.13 o -30 2 1 0.75 23.73 47.33 o -28 2 1 29.43 67.38 43.75 o -26 2 1 684.54 744.96 55.76 o -24 2 1 1745.17 1959.89 73.06 o -22 2 1 1.27 -22.43 28.90 o -20 2 1 29.73 19.30 30.23 o -18 2 1 898.11 889.20 36.95 o -16 2 1 9.50 31.86 18.44 o -14 2 1 190.48 203.69 23.00 o -12 2 1 1.40 -11.73 11.73 o -10 2 1 1412.11 1427.39 26.65 o -8 2 1 60.02 39.25 9.90 o -6 2 1 1535.88 1555.90 24.15 o -4 2 1 2299.69 2393.77 30.55 o -2 2 1 81.25 76.01 9.81 o 0 2 1 8565.23 8529.35 87.29 o 2 2 1 11971.99 12146.77 128.13 o 4 2 1 4084.28 4343.28 54.51 o 6 2 1 1333.81 1372.45 23.89 o 8 2 1 2166.36 2171.30 36.19 o 10 2 1 1634.25 1708.39 32.59 o 12 2 1 1322.88 1406.62 32.81 o 14 2 1 416.50 336.63 25.02 o 16 2 1 5.90 23.00 27.81 o 18 2 1 0.39 -3.87 25.78 o 20 2 1 233.91 226.43 29.36 o 22 2 1 430.85 463.42 40.00 o 24 2 1 1.61 13.48 36.81 o 26 2 1 115.83 108.81 47.56 o 28 2 1 35.14 35.67 44.29 o 30 2 1 153.37 212.06 51.90 o 32 2 1 65.25 57.70 57.29 o -31 3 1 6.67 12.30 62.87 o -29 3 1 3.68 56.61 53.56 o -27 3 1 101.84 110.76 49.13 o -25 3 1 53.57 -12.37 40.02 o -23 3 1 38.92 63.41 38.16 o -21 3 1 17.70 -28.90 31.20 o -19 3 1 81.21 62.10 30.46 o -17 3 1 93.06 79.55 23.19 o -15 3 1 137.94 88.77 24.35 o -13 3 1 1497.07 1540.13 42.37 o -11 3 1 78.74 63.31 15.40 o -9 3 1 2606.96 2876.13 47.22 o -7 3 1 1930.96 2211.91 36.61 o -5 3 1 230.02 194.38 12.36 o -3 3 1 98.96 49.83 11.42 o -1 3 1 4516.05 4764.98 58.20 o 1 3 1 10756.99 11809.44 131.49 o 3 3 1 3321.52 3650.46 50.75 o 5 3 1 129.45 127.24 16.05 o 7 3 1 2862.41 2967.46 55.09 o 9 3 1 0.00 -11.03 13.86 o 11 3 1 22.54 19.29 20.05 o 13 3 1 392.58 402.46 31.70 o 15 3 1 830.09 800.52 45.81 o 17 3 1 802.38 840.70 45.13 o 19 3 1 18.65 35.84 31.39 o 21 3 1 3.59 -36.72 36.72 o 23 3 1 873.63 1009.28 60.50 o 25 3 1 192.92 191.93 52.11 o 27 3 1 440.36 523.47 61.49 o 29 3 1 51.92 -6.33 52.91 o -28 4 1 16.39 -22.23 67.02 o -26 4 1 137.53 66.75 59.98 o -24 4 1 268.16 266.33 60.13 o -22 4 1 96.24 112.90 42.29 o -20 4 1 37.29 53.95 37.59 o -18 4 1 169.86 181.07 35.58 o -16 4 1 1001.86 1099.27 51.36 o -14 4 1 0.83 -26.77 26.77 o -12 4 1 515.15 546.77 33.73 o -10 4 1 300.18 292.89 27.36 o -8 4 1 289.56 286.48 20.00 o -6 4 1 173.46 156.46 18.94 o -4 4 1 372.59 356.72 18.58 o -2 4 1 4.38 -9.77 15.21 o 0 4 1 1535.52 1634.78 38.84 o 2 4 1 1.75 4.21 18.30 o 4 4 1 59.91 68.24 18.69 o 6 4 1 19.38 7.34 20.50 o 8 4 1 131.24 130.48 25.76 o 10 4 1 133.94 127.89 26.21 o 12 4 1 550.08 568.89 42.98 o 14 4 1 327.27 312.61 35.76 o 16 4 1 1490.61 1527.79 66.64 o 18 4 1 37.02 -16.72 37.12 o 20 4 1 308.32 385.09 54.45 o 22 4 1 848.22 1031.88 90.39 o 24 4 1 0.99 -3.67 48.09 o 26 4 1 237.66 154.54 83.00 o -23 5 1 143.38 146.68 64.21 o -21 5 1 86.17 166.46 60.96 o -19 5 1 0.49 -1.12 54.65 o -17 5 1 31.37 68.02 53.14 o -15 5 1 29.82 33.16 52.01 o -13 5 1 0.41 -46.87 46.87 o -11 5 1 110.86 75.19 49.49 o -9 5 1 261.27 229.29 38.23 o -7 5 1 276.83 234.64 33.37 o -5 5 1 5.45 7.58 25.73 o -3 5 1 69.24 83.19 20.54 o -1 5 1 243.25 251.57 27.99 o 1 5 1 43.09 25.44 24.99 o 3 5 1 365.98 353.39 37.75 o 5 5 1 356.15 351.38 46.28 o 7 5 1 1.00 -16.93 32.32 o 9 5 1 668.99 531.11 43.59 o 11 5 1 378.30 469.14 56.59 o 13 5 1 111.83 90.07 42.36 o 15 5 1 3.71 45.58 56.98 o 17 5 1 0.64 27.54 61.43 o 19 5 1 159.90 97.86 55.49 o 21 5 1 94.20 -5.22 65.91 o 23 5 1 2.64 66.07 67.02 o -18 6 1 0.44 29.81 93.48 o -16 6 1 0.07 -39.72 64.25 o -14 6 1 304.13 175.43 73.01 o -12 6 1 313.46 230.87 86.27 o -10 6 1 41.46 -2.63 64.20 o -8 6 1 734.96 594.43 74.87 o -6 6 1 82.08 60.01 55.52 o -4 6 1 522.92 417.93 66.13 o -2 6 1 126.45 81.28 45.33 o 0 6 1 416.99 466.80 51.56 o 2 6 1 550.64 541.00 95.23 o 4 6 1 3.59 60.46 59.84 o 6 6 1 482.32 455.49 73.27 o 8 6 1 29.20 -57.18 62.09 o 10 6 1 19.58 45.87 67.15 o 12 6 1 491.06 589.24 89.22 o 14 6 1 254.10 113.98 69.13 o 16 6 1 546.82 453.53 79.01 o -1 7 1 139.14 17.24 111.38 o 1 7 1 53.48 97.90 105.05 o -34 0 2 20.89 113.53 86.91 o -32 0 2 446.15 282.43 100.68 o -30 0 2 130.44 27.80 69.88 o -28 0 2 85.10 63.58 58.28 o -26 0 2 777.91 655.86 72.98 o -24 0 2 535.32 401.48 59.35 o -22 0 2 1764.25 1924.21 98.59 o -20 0 2 15.54 35.98 33.16 o -18 0 2 32.61 0.09 27.87 o -16 0 2 2.06 2.16 21.56 o -14 0 2 482.68 466.23 29.20 o -12 0 2 9577.12 10088.30 187.53 o -10 0 2 3716.69 3698.85 62.83 o -8 0 2 1225.56 1179.20 28.25 o -6 0 2 20998.90 19321.27 248.08 o -4 0 2 8768.09 8004.84 101.03 o -2 0 2 2806.52 2336.51 54.34 o 2 0 2 1069.93 1015.85 20.27 o 4 0 2 27547.54 26641.48 406.66 o 6 0 2 6230.89 6359.37 154.89 o 8 0 2 2545.06 2263.85 59.13 o 10 0 2 1421.12 1373.91 38.81 o 12 0 2 17196.39 18318.01 278.00 o 14 0 2 3173.66 3008.80 78.20 o 16 0 2 4287.05 4817.02 129.15 o 18 0 2 39.50 3.86 30.49 o 20 0 2 28.17 26.14 36.76 o 22 0 2 383.75 332.04 46.68 o 24 0 2 955.60 863.45 78.36 o 26 0 2 473.75 504.26 87.94 o 28 0 2 442.83 353.47 71.89 o 30 0 2 814.51 799.53 96.85 o 32 0 2 5.20 60.50 85.42 o -33 1 2 11.95 24.34 55.26 o -31 1 2 44.28 16.57 49.71 o -29 1 2 3.96 -13.79 45.51 o -27 1 2 322.20 335.02 49.76 o -25 1 2 652.44 788.28 63.72 o -23 1 2 226.39 214.47 36.32 o -21 1 2 10.91 2.46 26.92 o -19 1 2 0.01 28.29 22.77 o -17 1 2 1052.94 1100.64 37.69 o -15 1 2 570.09 468.65 21.50 o -13 1 2 2215.75 2469.47 39.19 o -11 1 2 3792.04 3870.39 49.22 o -9 1 2 582.52 520.01 14.19 o -7 1 2 14.12 7.53 8.75 o -5 1 2 6092.80 5672.06 56.58 o -3 1 2 3153.10 2936.28 32.66 o -1 1 2 56878.66 54896.90 550.46 o 1 1 2 4.95 6.27 5.64 o 3 1 2 85852.04 83351.29 973.47 o 5 1 2 779.32 660.09 15.25 o 7 1 2 1799.38 1674.05 26.93 o 9 1 2 96.29 65.94 9.50 o 11 1 2 2660.03 2608.50 40.42 o 13 1 2 1123.85 1113.28 26.24 o 15 1 2 2045.29 2135.60 48.88 o 17 1 2 269.84 313.76 33.25 o 19 1 2 137.08 87.00 29.72 o 21 1 2 146.88 69.35 32.85 o 23 1 2 30.42 90.65 35.53 o 25 1 2 528.76 590.24 46.69 o 27 1 2 160.35 169.74 42.88 o 29 1 2 49.89 60.65 44.84 o 31 1 2 229.53 301.09 55.07 o 33 1 2 26.59 -41.82 58.75 o -32 2 2 118.59 144.80 56.24 o -30 2 2 0.11 -46.40 46.40 o -28 2 2 7.05 -41.85 41.85 o -26 2 2 58.45 36.44 36.84 o -24 2 2 1866.55 1940.51 75.16 o -22 2 2 123.56 79.77 33.79 o -20 2 2 103.68 68.75 36.84 o -18 2 2 217.09 234.97 28.61 o -16 2 2 689.49 590.08 26.26 o -14 2 2 115.89 110.69 16.66 o -12 2 2 204.42 164.15 14.14 o -10 2 2 340.76 330.67 14.08 o -8 2 2 1321.71 1331.12 24.30 o -6 2 2 10.34 8.82 10.14 o -4 2 2 153.77 128.57 12.69 o -2 2 2 274.76 236.91 13.21 o 0 2 2 12070.17 12430.49 126.37 o 2 2 2 833.30 959.17 21.14 o 4 2 2 4952.19 5333.06 66.63 o 6 2 2 50.42 32.20 12.29 o 8 2 2 165.07 187.48 12.44 o 10 2 2 599.65 506.65 26.12 o 12 2 2 2926.89 3049.18 52.36 o 14 2 2 49.64 36.50 19.76 o 16 2 2 2463.73 2398.45 57.15 o 18 2 2 1395.24 1475.21 48.59 o 20 2 2 216.80 248.97 41.70 o 22 2 2 246.29 210.69 35.28 o 24 2 2 183.78 253.28 43.85 o 26 2 2 753.45 777.98 69.22 o 28 2 2 78.22 136.41 48.78 o 30 2 2 21.26 -1.87 51.03 o 32 2 2 72.94 38.35 59.15 o -31 3 2 233.69 241.03 104.03 o -29 3 2 102.60 31.49 49.24 o -27 3 2 34.28 4.52 44.40 o -25 3 2 952.99 1007.27 60.97 o -23 3 2 18.83 -6.01 33.40 o -21 3 2 517.30 484.03 37.99 o -19 3 2 117.17 94.33 27.54 o -17 3 2 751.75 734.70 37.98 o -15 3 2 143.90 82.27 21.20 o -13 3 2 6964.17 7892.40 109.33 o -11 3 2 143.10 121.98 16.59 o -9 3 2 252.53 231.02 17.82 o -7 3 2 2554.35 2788.50 43.60 o -5 3 2 301.34 323.52 14.35 o -3 3 2 312.07 283.54 13.38 o -1 3 2 971.31 949.84 22.11 o 1 3 2 579.08 447.64 17.25 o 3 3 2 1846.79 1942.95 36.57 o 5 3 2 794.66 809.00 26.07 o 7 3 2 162.68 165.53 18.77 o 9 3 2 1.12 12.49 21.04 o 11 3 2 73.29 70.73 18.30 o 13 3 2 1695.42 1707.56 47.12 o 15 3 2 5879.38 6314.80 109.77 o 17 3 2 83.95 99.18 27.25 o 19 3 2 1166.41 1136.50 57.56 o 21 3 2 176.83 167.88 38.83 o 23 3 2 43.82 86.77 46.86 o 25 3 2 85.50 69.07 45.23 o 27 3 2 677.93 782.27 71.70 o 29 3 2 14.92 -53.94 53.94 o -28 4 2 44.33 43.86 66.67 o -26 4 2 67.73 -6.47 56.97 o -24 4 2 66.21 30.06 53.03 o -22 4 2 17.07 -49.21 49.21 o -20 4 2 115.09 101.24 36.65 o -18 4 2 441.08 477.45 37.39 o -16 4 2 0.82 -8.19 26.65 o -14 4 2 234.31 203.52 29.01 o -12 4 2 1608.80 1632.64 45.01 o -10 4 2 4.48 -4.40 19.54 o -8 4 2 28.50 40.40 18.56 o -6 4 2 124.62 120.65 17.26 o -4 4 2 24.20 26.78 15.02 o -2 4 2 21.51 19.04 14.09 o 0 4 2 745.56 783.99 27.70 o 2 4 2 0.21 21.66 20.49 o 4 4 2 239.14 221.65 24.87 o 6 4 2 196.54 221.59 28.45 o 8 4 2 242.92 201.83 29.59 o 10 4 2 36.91 76.90 25.81 o 12 4 2 640.51 578.42 40.65 o 14 4 2 2369.81 2462.07 79.30 o 16 4 2 3.01 10.65 36.07 o 18 4 2 71.44 60.23 40.75 o 20 4 2 707.18 658.63 55.12 o 22 4 2 1.83 28.11 44.19 o 24 4 2 145.41 114.17 58.57 o 26 4 2 124.57 71.85 56.40 o -23 5 2 694.00 606.08 100.55 o -21 5 2 44.78 18.92 60.91 o -19 5 2 10.15 90.91 56.06 o -17 5 2 29.10 33.81 50.94 o -15 5 2 40.68 62.39 48.13 o -13 5 2 2510.47 2509.05 99.73 o -11 5 2 151.74 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