#------------------------------------------------------------------------------ #$Date: 2011-09-28 17:24:46 +0300 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/01/25/2012523.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_2012523_Fobs loop_ _publ_author_name 'Low, John Nicolson' 'Cobo, Justo' 'Insuasty, Braulio' 'Insuasty, Henry' 'Nogueras, Manuel' 'S\'anchez, Adolfo' _publ_section_title ; Supramolecular hydrogen-bonded hexamers in two 5-aryl-3-methyl-1-phenyl-1,6,7,8-tetrahydropyrazolo[3,4-b][1,4]diazepines ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first o103 _journal_page_last o105 _journal_volume 58 _journal_year 2002 _space_group_IT_number 148 _symmetry_space_group_name_Hall '-R 3' _symmetry_space_group_name_H-M 'R -3 :H' _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 120.000 _cell_length_a 30.5212 _cell_length_b 30.5212 _cell_length_c 8.8689 _exptl_crystal_F_000 2880.00 _reflns_d_resolution_high 0.7804 _[local]_cod_data_source_file sk1526Isup2.hkl _[local]_cod_data_source_block I #BEGIN Tags that were not found in dictionaries: _shelx_title ' 378 - SHELXL' _shelx_refln_list_code 4 _shelx_f_calc_maximum 383.55 _shelx_f_squared_multiplier 1.000 #END Tags that were not found in dictionaries loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' 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 5 0 32.20 3.39 4.15 o -1 5 0 12268.36 9866.64 228.16 o -3 6 0 53036.95 45267.66 794.36 o 0 6 0 12167.85 10812.48 180.08 o -2 7 0 50757.46 44903.51 701.31 o -7 8 0 1961.58 1724.84 49.92 o -4 8 0 20084.43 17828.05 290.46 o -1 8 0 726.22 836.01 16.79 o -6 9 0 3070.74 2634.56 44.90 o -3 9 0 127898.22 109886.07 1735.41 o 0 9 0 646.17 721.50 15.75 o -8 10 0 30.98 72.75 12.86 o -5 10 0 13426.73 13839.80 208.11 o -2 10 0 12145.55 12437.78 174.58 o -10 11 0 10984.53 10491.86 158.80 o -7 11 0 2.65 8.58 7.88 o -4 11 0 57725.90 52549.11 810.50 o -1 11 0 117.43 88.22 6.95 o -9 12 0 4571.68 4326.18 72.45 o -6 12 0 34601.30 33149.54 536.15 o -3 12 0 165.71 47.99 12.48 o 0 12 0 3735.07 3815.09 62.76 o -11 13 0 1662.26 1509.25 41.57 o -8 13 0 6725.55 6224.13 103.60 o -5 13 0 162.11 160.95 12.57 o -2 13 0 15728.76 14669.52 217.79 o -13 14 0 16445.81 16464.30 355.01 o -10 14 0 57.23 30.04 11.65 o -7 14 0 10887.41 10919.46 181.13 o -4 14 0 32580.90 32081.64 772.99 o -1 14 0 40521.37 42367.22 918.51 o -12 15 0 3816.96 3899.22 76.13 o -9 15 0 10890.01 11222.29 186.30 o -6 15 0 3187.98 4258.55 71.56 o -3 15 0 13581.76 14771.51 398.88 o 0 15 0 412.60 510.08 23.22 o -14 16 0 2341.96 3143.72 87.04 o -11 16 0 1383.87 1370.97 33.43 o -8 16 0 3098.71 3325.63 63.81 o -5 16 0 2742.27 1982.62 43.41 o -2 16 0 1217.54 1530.25 46.46 o -16 17 0 566.48 750.13 39.09 o -13 17 0 9236.90 9382.61 191.25 o -10 17 0 8652.38 8977.35 156.30 o -7 17 0 1698.09 1767.41 46.92 o -4 17 0 1687.80 1655.50 44.22 o -1 17 0 191.72 183.37 21.12 o -15 18 0 2962.40 2929.06 127.20 o -12 18 0 5071.45 4816.27 100.81 o -9 18 0 259.75 221.43 24.69 o -6 18 0 1773.16 2353.03 46.78 o -3 18 0 414.77 536.19 36.84 o 0 18 0 3441.38 3140.78 92.65 o -17 19 0 10.38 23.80 10.69 o -14 19 0 285.42 297.33 36.20 o -11 19 0 60.02 6.64 28.49 o -8 19 0 16799.53 17058.95 352.23 o -5 19 0 2776.97 2517.78 77.50 o -2 19 0 2680.30 2498.04 128.55 o -19 20 0 796.71 991.97 55.14 o -16 20 0 6852.14 7805.20 204.80 o -13 20 0 395.41 380.81 27.75 o -10 20 0 14.90 9.54 19.60 o -7 20 0 946.88 728.34 54.07 o -4 20 0 4712.32 4660.36 130.65 o -1 20 0 4509.25 4574.70 166.31 o -18 21 0 4257.73 4359.36 655.81 o -15 21 0 305.74 325.83 29.90 o -12 21 0 1418.51 1396.25 43.82 o -9 21 0 928.14 1202.13 46.18 o -6 21 0 2815.14 3004.36 80.94 o -3 21 0 2610.60 2407.51 89.59 o 0 21 0 842.21 680.92 42.35 o -20 22 0 110.21 114.82 44.90 o -17 22 0 0.80 5.05 6.24 o -14 22 0 181.36 224.36 36.61 o -11 22 0 2702.77 2971.32 102.46 o -8 22 0 4158.85 5080.02 135.67 o -5 22 0 2954.53 3359.89 106.82 o -2 22 0 183.30 127.59 38.61 o -22 23 0 1600.04 1573.74 91.27 o -19 23 0 1456.89 1460.98 99.00 o -16 23 0 359.30 318.55 31.74 o -13 23 0 2216.58 2422.20 113.10 o -10 23 0 112.50 88.29 13.51 o -7 23 0 3991.62 4036.37 121.21 o -4 23 0 1509.48 1355.98 77.37 o -21 24 0 3622.12 3818.58 185.09 o -18 24 0 641.92 567.02 53.43 o -15 24 0 2743.80 2610.95 103.72 o -12 24 0 618.51 751.62 33.85 o -9 24 0 37.29 -24.76 24.76 o -6 24 0 5805.48 5934.77 161.75 o -3 24 0 2107.82 1929.00 102.19 o 0 24 0 6.83 7.89 32.68 o -23 25 0 365.95 312.32 41.61 o -20 25 0 1215.32 1100.10 55.60 o -17 25 0 258.54 294.69 43.57 o -14 25 0 575.62 472.50 31.05 o -11 25 0 2714.34 2689.87 87.91 o -8 25 0 2596.56 2868.73 122.15 o -5 25 0 2710.01 2608.20 105.05 o -2 25 0 139.29 207.42 38.94 o -22 26 0 14.19 -6.84 30.30 o -19 26 0 51.50 32.24 18.80 o -16 26 0 3706.87 4054.48 117.52 o -13 26 0 1361.46 1454.09 55.87 o -10 26 0 1362.45 1319.72 67.19 o -7 26 0 2167.05 2534.94 97.97 o -4 26 0 22.96 33.67 34.74 o -24 27 0 481.96 389.85 69.53 o -21 27 0 408.35 380.26 43.21 o -18 27 0 469.31 374.31 50.71 o -15 27 0 860.43 902.20 69.49 o -12 27 0 457.30 446.92 41.89 o -9 27 0 6701.92 6626.74 450.67 o -6 27 0 250.12 164.54 35.93 o 0 27 0 7724.54 7360.05 440.63 o -26 28 0 240.37 272.77 67.49 o -23 28 0 7975.84 7707.03 308.80 o -20 28 0 3834.15 3817.73 179.65 o -17 28 0 18.45 50.45 27.84 o -14 28 0 2.14 5.55 16.63 o -11 28 0 242.87 349.00 58.53 o -8 28 0 1306.70 1073.94 68.61 o -2 28 0 46.75 40.73 35.96 o -28 29 0 109.96 97.75 47.71 o -25 29 0 597.79 609.48 77.82 o -22 29 0 3230.12 2852.21 124.74 o -19 29 0 331.89 355.34 39.51 o -16 29 0 8.71 3.46 20.97 o -13 29 0 1351.15 1205.20 85.58 o -10 29 0 250.02 272.77 84.43 o -4 29 0 4028.85 3616.53 168.88 o -27 30 0 1775.24 1588.06 90.80 o -24 30 0 18.77 -28.56 41.39 o -21 30 0 100.84 116.34 71.16 o -18 30 0 3002.06 2923.22 107.83 o -15 30 0 21.47 56.73 38.29 o -6 30 0 70.76 90.56 53.26 o 0 30 0 328.74 328.12 96.29 o -29 31 0 334.25 182.07 50.80 o -26 31 0 1010.62 697.18 121.14 o -23 31 0 5.30 109.12 56.41 o -20 31 0 110.61 125.85 43.31 o -17 31 0 772.15 578.60 54.55 o -8 31 0 21.80 -6.06 52.04 o -2 31 0 592.84 621.88 85.43 o -31 32 0 41.84 120.03 62.10 o -28 32 0 332.15 145.07 51.35 o -25 32 0 22.82 -45.36 45.36 o -22 32 0 1543.54 1396.00 90.06 o -19 32 0 1649.84 1719.32 104.41 o -16 32 0 0.08 -48.29 68.90 o -13 32 0 4050.92 4601.84 383.75 o -10 32 0 1098.74 913.76 136.10 o -7 32 0 12.44 72.01 53.15 o -4 32 0 79.19 62.12 88.38 o -1 32 0 1560.33 1859.15 206.13 o -30 33 0 15.89 40.54 51.08 o -27 33 0 1812.35 1761.51 148.89 o -24 33 0 1693.77 1253.17 173.38 o -21 33 0 118.04 129.33 78.22 o -18 33 0 555.25 579.98 63.97 o -15 33 0 166.90 55.06 79.06 o -9 33 0 3423.45 3555.75 187.52 o 0 33 0 29.99 90.81 61.11 o -32 34 0 0.79 70.68 58.61 o -29 34 0 493.78 556.25 109.56 o -26 34 0 561.76 432.18 76.62 o -23 34 0 368.74 234.26 58.83 o -20 34 0 26.66 72.75 50.69 o -17 34 0 382.02 281.29 60.82 o -14 34 0 358.70 249.62 112.95 o -11 34 0 632.81 481.45 129.04 o -5 34 0 1261.15 1311.99 113.64 o -2 34 0 725.85 977.30 102.70 o -31 35 0 45.28 147.82 64.89 o -28 35 0 31.28 -8.56 94.26 o -25 35 0 2036.88 2423.78 154.70 o -22 35 0 130.31 153.17 58.56 o -19 35 0 63.54 43.64 62.59 o -16 35 0 2378.08 2409.41 143.17 o -10 35 0 79.00 25.71 53.05 o -30 36 0 2647.32 3245.32 333.77 o -24 36 0 6.85 112.67 90.08 o -21 36 0 145.86 66.07 80.10 o -18 36 0 20.55 49.64 56.82 o -15 36 0 989.81 937.76 151.92 o -12 36 0 12.41 -91.21 91.21 o -29 37 0 5.83 -5.86 64.91 o -26 37 0 477.62 438.17 97.70 o -20 37 0 89.16 -42.64 98.27 o -17 37 0 2634.78 2581.25 151.96 o -11 37 0 308.58 424.10 102.56 o -8 37 0 0.00 47.04 83.08 o -25 38 0 19.13 97.39 68.62 o -22 38 0 222.71 375.56 144.86 o -16 38 0 1347.49 1557.83 123.07 o -18 39 0 948.54 819.54 123.27 o -3 2 1 1833.80 1743.64 26.86 o -5 3 1 46479.92 39272.17 639.85 o -2 3 1 20825.85 17991.60 257.61 o 1 3 1 13256.92 11934.29 170.36 o -7 4 1 5137.29 5089.58 70.96 o -4 4 1 24875.43 22640.75 321.52 o 2 4 1 38021.98 33438.78 568.43 o -9 5 1 16428.04 15194.62 233.08 o -6 5 1 38257.56 34466.70 544.95 o -3 5 1 17275.73 15360.81 284.69 o 0 5 1 22049.35 18561.85 283.32 o 3 5 1 20475.77 19453.21 322.35 o -11 6 1 27546.27 25890.76 397.95 o -8 6 1 8341.31 8151.61 184.49 o -5 6 1 834.97 831.79 16.07 o 4 6 1 71.77 67.15 8.51 o -13 7 1 0.01 17.54 14.01 o -10 7 1 20717.65 19849.04 317.01 o -7 7 1 117115.70 101957.63 2400.71 o -4 7 1 3013.28 2368.17 38.79 o -1 7 1 147108.81 122437.09 5324.43 o 2 7 1 45260.78 43059.11 811.71 o 5 7 1 7284.55 7360.60 115.62 o -15 8 1 1498.13 1942.70 67.20 o -12 8 1 5479.02 5157.83 90.46 o -9 8 1 38500.00 36334.40 623.06 o -6 8 1 10841.33 10012.86 171.01 o -3 8 1 68464.02 62485.15 1064.34 o 0 8 1 107954.44 98023.07 2105.64 o 3 8 1 12972.90 13286.68 211.59 o 6 8 1 355.95 237.73 17.57 o -17 9 1 8208.34 8323.70 148.74 o -14 9 1 2217.02 2250.42 43.87 o -11 9 1 3475.65 3652.76 58.48 o -8 9 1 1222.13 1205.11 25.14 o -5 9 1 1872.57 1823.45 32.58 o -2 9 1 20138.19 18772.52 296.17 o 1 9 1 58995.25 56482.50 1035.49 o 4 9 1 31318.73 31543.10 612.97 o 7 9 1 86.75 112.65 19.59 o -19 10 1 4818.03 5714.07 119.85 o -16 10 1 12983.81 13142.49 226.87 o -13 10 1 8152.86 7169.32 110.98 o -10 10 1 4035.57 3897.94 71.51 o -7 10 1 681.12 691.80 18.46 o -4 10 1 928.07 1052.43 22.63 o -1 10 1 33302.82 32397.25 574.54 o 2 10 1 1706.02 1649.94 31.71 o 5 10 1 1310.10 1132.72 30.72 o 8 10 1 1361.53 1499.49 49.63 o -21 11 1 5447.15 5431.37 166.66 o -18 11 1 5638.51 5468.31 113.86 o -15 11 1 5000.92 5037.81 83.41 o -12 11 1 6101.23 5897.50 131.86 o -9 11 1 9657.88 10225.33 167.21 o -6 11 1 9055.93 8494.17 122.03 o -3 11 1 24792.80 24375.95 303.95 o 0 11 1 13478.08 12954.40 285.60 o 3 11 1 4072.44 4515.99 75.72 o 6 11 1 5642.61 5750.85 106.52 o 9 11 1 10367.49 10298.25 239.66 o -23 12 1 4256.75 4186.71 99.81 o -20 12 1 281.06 227.12 27.94 o -17 12 1 13.36 6.84 12.05 o -14 12 1 148.88 151.26 18.18 o -11 12 1 238.58 340.79 16.15 o -8 12 1 50785.42 53925.16 944.38 o -5 12 1 7811.16 7868.50 119.35 o -2 12 1 382.25 339.70 13.91 o 1 12 1 106.15 69.94 9.58 o 4 12 1 1192.20 1428.88 32.76 o 7 12 1 123.01 142.71 21.32 o 10 12 1 125.04 88.09 24.03 o -25 13 1 754.74 725.76 45.16 o -22 13 1 624.73 737.11 43.56 o -19 13 1 10775.03 11180.68 255.65 o -16 13 1 15329.58 14700.60 263.38 o -13 13 1 6587.27 7081.18 239.47 o -10 13 1 2818.94 2708.67 60.13 o -7 13 1 997.86 939.13 30.27 o -4 13 1 19050.63 18647.51 251.48 o -1 13 1 54983.14 55899.79 1339.78 o 2 13 1 3852.58 3528.75 78.14 o 5 13 1 7984.67 8487.75 149.84 o 8 13 1 154.20 122.47 24.13 o 11 13 1 268.39 301.10 21.82 o -27 14 1 2219.27 2161.59 90.12 o -24 14 1 1095.34 988.37 52.75 o -21 14 1 7969.77 8361.69 202.19 o -18 14 1 56.89 91.82 18.90 o -15 14 1 173.18 237.72 17.66 o -12 14 1 283.75 332.36 12.30 o -9 14 1 943.49 843.18 47.19 o -6 14 1 3277.18 3107.55 62.62 o -3 14 1 1776.72 1649.09 37.77 o 0 14 1 5050.89 4904.29 147.62 o 3 14 1 597.53 558.42 17.42 o 6 14 1 50.25 30.09 13.21 o 9 14 1 3734.44 4268.81 126.15 o 12 14 1 1994.23 2106.74 76.48 o -29 15 1 1898.29 1897.46 82.22 o -26 15 1 0.10 -5.78 29.86 o -23 15 1 2202.39 2151.83 61.79 o -20 15 1 50.15 13.68 27.72 o -17 15 1 313.69 167.84 18.65 o -14 15 1 19005.74 18827.01 339.70 o -11 15 1 2712.41 2858.24 55.13 o -8 15 1 245.27 290.21 14.13 o -5 15 1 14609.92 13639.78 192.80 o -2 15 1 15739.32 16234.50 350.55 o 1 15 1 6774.42 6895.52 211.85 o 4 15 1 117.41 148.90 14.10 o 7 15 1 1662.35 1663.31 54.04 o 10 15 1 53.77 31.40 28.72 o 13 15 1 1101.56 1159.17 60.47 o -31 16 1 9657.34 10430.86 379.43 o -28 16 1 3454.10 3631.73 159.88 o -25 16 1 9389.59 9813.10 275.32 o -22 16 1 1753.06 1927.53 89.54 o -19 16 1 2735.78 2457.29 84.06 o -16 16 1 13069.24 12782.16 1081.88 o -13 16 1 15811.31 17511.29 357.78 o -10 16 1 13749.24 15651.88 265.35 o -7 16 1 1811.29 1615.62 33.38 o -4 16 1 3557.94 3445.71 62.13 o -1 16 1 1412.81 1379.63 44.34 o 2 16 1 6956.56 6995.62 304.25 o 5 16 1 871.05 813.47 38.32 o 8 16 1 336.19 406.44 25.55 o 11 16 1 8898.08 9710.91 271.14 o 14 16 1 114.63 216.09 40.68 o -33 17 1 126.51 103.59 56.67 o -30 17 1 7121.28 7450.52 269.99 o -27 17 1 1277.98 1400.86 73.00 o -24 17 1 141.83 134.21 34.78 o -21 17 1 158.71 147.90 23.57 o -18 17 1 8.41 -3.22 20.21 o -15 17 1 394.81 255.11 22.61 o -12 17 1 31.13 59.50 14.23 o -9 17 1 971.20 816.37 28.37 o -6 17 1 21106.47 23147.68 369.78 o -3 17 1 12560.29 10599.12 205.60 o 0 17 1 3303.35 3268.70 148.50 o 3 17 1 5.39 20.97 19.17 o 6 17 1 1414.42 1571.01 65.86 o 9 17 1 1366.22 1404.86 60.00 o 12 17 1 15.21 2.58 16.86 o 15 17 1 946.02 732.96 97.72 o -35 18 1 1045.87 864.54 109.24 o -32 18 1 295.31 330.12 56.05 o -29 18 1 983.04 859.09 73.37 o -26 18 1 257.08 183.26 51.59 o -23 18 1 280.48 347.60 39.34 o -20 18 1 26.46 43.48 26.10 o -17 18 1 496.76 642.99 55.19 o -14 18 1 7496.89 8597.67 318.75 o -11 18 1 3495.25 3701.70 70.00 o -8 18 1 110.20 140.00 11.89 o -5 18 1 3466.91 3348.85 71.22 o -2 18 1 15542.80 15809.30 545.29 o 1 18 1 404.85 401.22 29.02 o 4 18 1 1596.74 1833.02 63.00 o 7 18 1 445.47 458.52 25.63 o 10 18 1 534.01 611.19 40.05 o 13 18 1 159.05 98.73 53.09 o 16 18 1 4.84 -77.65 77.65 o -37 19 1 3.96 -13.71 67.67 o -34 19 1 736.29 649.18 133.28 o -31 19 1 579.17 520.19 64.01 o -28 19 1 1065.26 884.78 63.32 o -25 19 1 90.78 7.22 27.79 o -22 19 1 323.86 225.81 32.80 o -19 19 1 1.07 -17.95 29.23 o -16 19 1 0.10 7.90 18.04 o -13 19 1 201.72 269.91 25.35 o -10 19 1 1.58 -0.78 11.77 o -7 19 1 0.18 -13.02 13.02 o -4 19 1 2033.72 2003.18 66.25 o -1 19 1 739.70 777.44 48.89 o 2 19 1 813.23 1033.90 130.03 o 5 19 1 111.40 114.86 13.16 o 8 19 1 4151.24 4266.07 159.57 o 11 19 1 269.70 303.42 50.90 o 14 19 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