#------------------------------------------------------------------------------ #$Date: 2011-09-28 14:24:46 +0000 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://cod.ibt.lt/cod/hkl/2/01/25/2012524.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_2012524_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 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 115.728 _cell_angle_beta 101.021 _cell_angle_gamma 98.830 _cell_length_a 9.0066 _cell_length_b 17.9695 _cell_length_c 18.0069 _exptl_crystal_F_000 1056.00 _reflns_d_resolution_high 0.7661 _[local]_cod_data_source_file sk1526IIsup3.hkl _[local]_cod_data_source_block II #BEGIN Tags that were not found in dictionaries: _shelx_title ' 01SRC377 in P-1' _shelx_refln_list_code 4 _shelx_f_calc_maximum 229.37 _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 2 0 0 43.02 70.06 3.35 o 3 0 0 4227.71 4383.70 189.20 o 4 0 0 163.83 142.52 5.63 o 5 0 0 1.47 25.52 7.10 o 6 0 0 1755.64 1851.18 92.60 o 7 0 0 381.12 665.61 133.83 o 8 0 0 68.34 124.04 11.87 o 9 0 0 0.36 24.23 28.45 o -9 1 0 166.65 179.07 39.08 o -8 1 0 331.72 351.36 71.44 o -7 1 0 194.37 200.48 23.55 o -6 1 0 2689.20 2573.06 131.59 o -5 1 0 5.13 18.41 4.23 o -4 1 0 164.88 212.56 12.09 o -3 1 0 2505.12 2616.60 86.30 o -2 1 0 1939.91 1951.65 106.45 o 1 1 0 5805.28 5972.65 266.60 o 2 1 0 323.75 292.36 14.89 o 3 1 0 37.44 46.47 5.63 o 4 1 0 16.27 130.50 32.59 o 5 1 0 14.84 38.82 4.33 o 6 1 0 10.58 12.63 6.33 o 7 1 0 907.22 800.92 82.02 o 8 1 0 90.81 121.17 12.98 o 9 1 0 10.65 7.93 4.58 o -10 2 0 29.72 12.42 40.13 o -9 2 0 618.56 660.03 92.50 o -8 2 0 952.02 967.14 116.54 o -7 2 0 355.57 435.28 43.42 o -6 2 0 272.40 293.64 30.25 o -5 2 0 809.44 819.18 50.92 o -4 2 0 2.36 130.00 36.47 o -3 2 0 617.08 661.54 15.73 o -2 2 0 2.35 21.21 2.54 o -1 2 0 3732.60 3601.16 139.41 o 1 2 0 7316.60 7377.87 252.16 o 2 2 0 0.13 7.89 3.71 o 3 2 0 349.44 472.04 17.35 o 4 2 0 4163.41 4631.11 155.30 o 5 2 0 776.48 686.60 29.40 o 6 2 0 2501.73 3066.00 108.16 o 7 2 0 1432.36 1481.33 77.91 o 8 2 0 1.33 6.70 5.49 o 9 2 0 144.51 119.26 12.04 o -11 3 0 161.17 185.13 53.92 o -10 3 0 0.56 19.38 38.64 o -9 3 0 298.02 366.40 48.33 o -8 3 0 338.96 407.31 39.94 o -7 3 0 155.53 142.01 20.23 o -6 3 0 28.33 31.95 14.23 o -5 3 0 666.20 600.40 23.40 o -4 3 0 3.96 261.32 119.87 o -3 3 0 2479.79 2442.31 404.05 o -2 3 0 7550.47 7917.27 691.11 o -1 3 0 1171.47 1265.27 66.12 o 0 3 0 344.69 274.43 13.38 o 1 3 0 52610.63 53759.20 3473.15 o 2 3 0 592.09 811.04 76.71 o 3 3 0 1995.80 4330.96 1268.60 o 4 3 0 34.34 6.34 4.20 o 5 3 0 0.76 25.40 9.78 o 6 3 0 2.27 -4.64 4.64 o 7 3 0 575.27 663.15 23.99 o 8 3 0 42.52 67.34 9.50 o 9 3 0 8.20 23.16 11.02 o -11 4 0 117.84 211.09 73.18 o -10 4 0 479.43 637.50 81.38 o -9 4 0 54.91 92.02 43.67 o -8 4 0 1693.53 1854.73 118.78 o -7 4 0 356.09 357.20 33.92 o -6 4 0 1588.16 1815.33 89.21 o -5 4 0 220.83 437.30 91.47 o -4 4 0 1111.49 907.73 97.30 o -3 4 0 1069.70 1077.64 78.08 o -2 4 0 2596.45 2252.71 57.02 o -1 4 0 2279.97 2985.08 909.13 o 1 4 0 5490.68 7018.47 332.12 o 3 4 0 140.78 181.19 7.80 o 4 4 0 3067.18 3235.21 170.66 o 5 4 0 326.53 317.38 12.30 o 6 4 0 1251.20 1503.24 46.48 o 7 4 0 205.30 227.97 18.33 o 8 4 0 408.41 406.61 37.60 o 9 4 0 15.03 21.02 15.76 o -11 5 0 308.45 325.27 67.59 o -10 5 0 133.79 186.12 45.47 o -9 5 0 464.45 553.17 44.94 o -8 5 0 27.09 48.51 21.46 o -7 5 0 684.99 780.73 42.01 o -6 5 0 1358.32 1556.24 39.79 o -5 5 0 186.41 163.37 7.14 o -4 5 0 514.32 859.08 264.64 o -3 5 0 453.26 523.87 22.84 o -2 5 0 15.46 250.98 149.02 o -1 5 0 115.12 309.14 174.54 o 1 5 0 114.84 120.53 8.78 o 3 5 0 32.86 93.38 20.75 o 4 5 0 122.93 264.55 79.92 o 5 5 0 54.99 59.06 7.72 o 6 5 0 817.00 874.67 27.85 o 7 5 0 208.51 230.92 14.14 o 8 5 0 67.63 111.70 22.01 o 9 5 0 3.96 12.80 24.10 o -11 6 0 318.23 462.44 79.89 o -10 6 0 46.65 53.67 41.37 o -9 6 0 48.02 6.67 22.78 o -8 6 0 784.62 923.29 100.33 o -7 6 0 1858.76 1675.38 158.69 o -6 6 0 27.02 338.29 160.40 o -5 6 0 271.81 263.91 18.51 o -4 6 0 601.46 588.43 19.42 o -3 6 0 1568.27 1496.50 35.07 o -2 6 0 212.50 226.68 9.48 o -1 6 0 3773.44 3160.92 89.26 o 0 6 0 2621.73 2766.63 73.48 o 2 6 0 275.63 274.10 10.70 o 3 6 0 189.17 218.88 10.66 o 4 6 0 198.14 229.86 10.40 o 5 6 0 271.14 421.83 18.92 o 6 6 0 18.68 73.56 19.17 o 7 6 0 118.36 152.41 18.65 o 8 6 0 496.04 392.52 32.08 o 9 6 0 145.25 140.02 35.41 o -11 7 0 368.14 489.53 90.70 o -10 7 0 135.89 156.92 46.84 o -9 7 0 90.63 91.61 24.68 o -8 7 0 9.62 12.45 16.66 o -7 7 0 1248.68 1285.66 58.06 o -6 7 0 238.17 301.38 16.04 o -5 7 0 1857.63 2122.23 58.60 o -4 7 0 1307.00 1218.20 35.92 o -3 7 0 335.91 303.76 9.36 o -2 7 0 294.82 302.07 11.33 o -1 7 0 1737.27 1913.67 82.79 o 0 7 0 4077.55 5014.99 180.95 o 2 7 0 1920.74 1901.32 49.94 o 3 7 0 286.67 244.70 18.56 o 4 7 0 274.08 253.76 18.60 o 5 7 0 223.27 226.22 14.61 o 6 7 0 1.83 23.94 12.99 o 7 7 0 544.95 505.48 29.63 o 8 7 0 18.99 27.95 21.94 o 9 7 0 9.31 66.35 32.43 o -11 8 0 87.97 151.08 57.65 o -10 8 0 519.18 792.19 92.19 o -9 8 0 48.78 97.91 38.64 o -8 8 0 32.27 37.15 5.48 o -7 8 0 277.50 547.25 176.92 o -6 8 0 473.56 466.51 15.16 o -5 8 0 373.57 643.19 29.61 o -4 8 0 118.84 204.53 20.85 o -3 8 0 84.64 648.10 211.88 o -2 8 0 374.28 418.78 13.87 o -1 8 0 775.67 802.51 98.40 o 1 8 0 348.49 382.34 23.57 o 2 8 0 2.79 46.63 10.93 o 3 8 0 853.53 855.14 33.24 o 4 8 0 14.92 12.41 12.79 o 5 8 0 67.90 113.39 15.63 o 6 8 0 6.52 18.75 13.87 o 7 8 0 154.60 222.98 26.38 o 8 8 0 126.76 116.33 20.79 o 9 8 0 18.50 77.65 42.37 o -11 9 0 15.99 31.56 45.23 o -10 9 0 155.07 180.03 61.87 o -9 9 0 282.17 407.65 48.21 o -8 9 0 106.22 234.18 26.32 o -7 9 0 71.23 72.88 8.87 o -6 9 0 52.64 76.54 7.49 o -5 9 0 892.05 1208.37 45.51 o -4 9 0 2659.67 2595.27 54.91 o -3 9 0 905.59 1046.38 33.87 o -2 9 0 506.08 603.93 20.44 o -1 9 0 1431.48 1716.28 91.42 o 0 9 0 302.43 288.67 11.44 o 1 9 0 137.61 112.75 11.50 o 2 9 0 5821.23 5882.20 205.84 o 3 9 0 59.53 64.94 10.46 o 4 9 0 37.81 96.57 19.55 o 5 9 0 87.76 68.81 14.13 o 6 9 0 1477.07 1422.29 77.30 o 7 9 0 176.27 130.95 25.69 o 8 9 0 177.02 224.76 49.20 o -10 10 0 0.06 -35.66 35.66 o -9 10 0 151.21 176.06 52.31 o -8 10 0 87.01 88.32 9.26 o -7 10 0 11.93 101.58 11.37 o -6 10 0 85.91 115.77 13.50 o -4 10 0 95.70 135.20 14.20 o -2 10 0 1.37 11.46 6.73 o -1 10 0 458.15 595.21 27.62 o 1 10 0 10.01 67.57 20.16 o 2 10 0 107.29 140.63 16.62 o 3 10 0 350.43 405.67 41.64 o 4 10 0 2758.98 2597.26 137.51 o 5 10 0 314.63 326.29 29.41 o 6 10 0 6.87 2.26 17.06 o 7 10 0 192.50 227.65 32.92 o 8 10 0 14.12 28.08 29.57 o -10 11 0 46.27 98.77 45.23 o -9 11 0 9.34 6.32 8.37 o -8 11 0 12.88 -1.45 12.09 o -7 11 0 1413.30 1194.84 44.74 o -5 11 0 0.22 18.96 7.78 o -4 11 0 2253.85 1852.36 56.56 o -3 11 0 829.18 802.91 32.61 o -2 11 0 209.27 412.05 192.16 o -1 11 0 0.32 13.82 11.08 o 0 11 0 160.95 180.41 14.18 o 1 11 0 957.02 923.14 42.69 o 2 11 0 23.22 188.02 30.79 o 3 11 0 6483.59 6148.02 266.73 o 4 11 0 811.09 1000.26 100.73 o 5 11 0 64.72 58.75 22.56 o 6 11 0 1.96 -19.73 19.73 o 7 11 0 22.43 51.03 37.89 o -10 12 0 114.11 138.41 45.23 o -9 12 0 89.02 88.76 13.37 o -7 12 0 162.56 201.89 15.50 o -6 12 0 4.63 10.77 8.56 o -5 12 0 43.04 107.87 12.43 o -4 12 0 42.42 175.55 23.37 o -3 12 0 680.96 580.26 25.32 o -2 12 0 1.93 18.93 9.26 o -1 12 0 89.68 132.50 17.61 o 0 12 0 197.53 187.06 19.39 o 1 12 0 665.15 570.78 29.32 o 2 12 0 2.10 10.41 13.53 o 3 12 0 676.69 638.95 40.98 o 4 12 0 1250.21 1116.91 85.47 o 5 12 0 1.51 -14.41 28.17 o 6 12 0 107.70 111.17 28.95 o 7 12 0 224.75 314.19 53.36 o -10 13 0 233.87 310.86 69.83 o -9 13 0 369.64 290.80 39.94 o -8 13 0 290.82 276.16 17.69 o -7 13 0 300.16 394.34 22.93 o -6 13 0 762.43 735.16 32.78 o -5 13 0 39.45 131.78 14.92 o -4 13 0 707.26 680.58 41.17 o -3 13 0 357.06 442.66 31.71 o -2 13 0 287.56 262.18 17.71 o -1 13 0 185.68 151.26 14.31 o 0 13 0 344.26 393.50 22.90 o 1 13 0 13.50 87.13 22.00 o 2 13 0 20.39 83.12 16.40 o 3 13 0 53.75 131.92 31.63 o 4 13 0 592.90 609.46 78.76 o 5 13 0 567.97 522.04 45.73 o 6 13 0 15.10 48.04 28.32 o -10 14 0 90.28 87.59 46.47 o -9 14 0 153.02 226.29 65.97 o -8 14 0 334.90 425.05 34.55 o -7 14 0 69.73 346.33 46.93 o -6 14 0 6.81 71.12 16.69 o -5 14 0 25.91 29.59 12.79 o -4 14 0 897.02 1121.14 46.30 o -3 14 0 114.57 111.03 17.79 o -2 14 0 88.89 175.15 23.85 o -1 14 0 374.62 394.28 28.29 o 0 14 0 139.52 148.35 19.42 o 1 14 0 1.65 530.66 109.25 o 2 14 0 613.00 535.39 37.97 o 3 14 0 11.28 11.30 22.29 o 4 14 0 3.99 82.17 38.75 o 5 14 0 85.96 39.52 30.41 o 6 14 0 342.15 256.75 49.81 o -9 15 0 209.30 143.50 36.65 o -8 15 0 11.88 26.77 22.35 o -7 15 0 510.99 568.90 65.22 o -6 15 0 4.36 0.68 11.31 o -5 15 0 50.06 274.89 51.52 o -4 15 0 1294.05 1341.89 65.80 o -3 15 0 308.74 307.12 23.83 o -2 15 0 166.65 169.08 21.09 o -1 15 0 350.47 315.41 28.09 o 0 15 0 405.76 333.81 30.44 o 1 15 0 580.40 583.29 53.61 o 2 15 0 62.40 62.00 23.90 o 3 15 0 30.66 36.03 29.58 o 4 15 0 8.01 38.19 30.97 o 5 15 0 4.55 20.21 36.70 o -9 16 0 9.19 145.12 49.33 o -8 16 0 32.91 91.82 33.92 o -7 16 0 10.56 30.91 23.76 o -6 16 0 6.09 -8.34 42.73 o -5 16 0 71.29 71.76 18.32 o -4 16 0 29.18 33.01 16.13 o -3 16 0 188.75 196.17 23.90 o -2 16 0 3.75 80.84 66.85 o -1 16 0 4.11 27.49 19.11 o 0 16 0 303.71 321.37 69.95 o 1 16 0 5.39 7.08 23.44 o 2 16 0 28.11 3.86 34.75 o 3 16 0 53.58 26.11 28.75 o 4 16 0 3.50 16.90 41.00 o -9 17 0 2.92 0.00 36.65 o -8 17 0 10.83 42.37 26.84 o -7 17 0 365.09 324.48 41.34 o -6 17 0 601.33 577.35 37.03 o -5 17 0 168.83 160.69 22.27 o -4 17 0 222.70 265.97 35.91 o -3 17 0 716.90 639.98 43.23 o -2 17 0 48.13 42.57 21.76 o -1 17 0 177.83 349.31 50.03 o 0 17 0 1205.72 1153.61 117.54 o 1 17 0 135.13 152.51 33.99 o 2 17 0 121.03 177.39 39.63 o 3 17 0 25.64 13.00 41.47 o 4 17 0 21.65 58.02 46.04 o -8 18 0 79.96 -29.69 46.72 o -7 18 0 4.60 146.13 79.39 o -6 18 0 416.24 544.21 55.23 o -5 18 0 70.20 94.34 31.32 o -4 18 0 28.36 110.49 43.66 o -3 18 0 218.92 187.25 33.65 o -2 18 0 351.61 310.60 53.92 o -1 18 0 0.35 -34.67 34.67 o 0 18 0 97.67 206.55 52.49 o 1 18 0 4.44 -7.48 38.52 o 2 18 0 27.33 57.78 30.46 o 3 18 0 210.16 129.46 40.51 o -7 19 0 16.13 41.13 51.06 o -6 19 0 4.36 4.45 25.53 o -5 19 0 19.00 15.59 37.58 o -4 19 0 6.09 9.18 22.21 o -3 19 0 3.86 -12.05 37.25 o -2 19 0 69.22 68.00 42.95 o -1 19 0 6.42 50.74 41.65 o 0 19 0 0.56 5.43 34.11 o 1 19 0 94.93 168.87 46.90 o 2 19 0 55.14 152.08 89.58 o -6 20 0 137.43 133.70 43.74 o -5 20 0 238.66 206.93 37.90 o -4 20 0 9.95 62.82 29.78 o -3 20 0 4.26 -13.52 31.18 o -2 20 0 331.93 341.61 51.41 o -1 20 0 15.61 12.65 27.38 o 0 20 0 7.34 18.17 38.70 o -4 21 0 270.96 209.85 87.10 o -3 21 0 22.56 45.76 31.86 o 1 -21 1 81.07 103.09 37.81 o 2 -21 1 64.29 93.48 52.19 o 3 -21 1 77.28 68.02 33.21 o 4 -21 1 0.55 24.75 32.67 o 5 -21 1 0.32 9.12 33.21 o -1 -20 1 213.96 282.56 69.02 o 0 -20 1 0.21 8.06 32.15 o 1 -20 1 55.30 82.27 44.73 o 2 -20 1 68.51 53.95 33.82 o 3 -20 1 198.22 334.01 50.50 o 4 -20 1 76.02 100.04 33.45 o 5 -20 1 0.06 37.83 36.63 o 6 -20 1 38.05 84.24 38.73 o -2 -19 1 2.56 25.59 38.13 o -1 -19 1 0.18 -41.02 41.02 o 0 -19 1 25.37 32.83 39.94 o 1 -19 1 119.42 228.71 50.44 o 2 -19 1 5.32 -15.38 25.60 o 3 -19 1 350.84 336.77 61.54 o 4 -19 1 20.76 -17.94 31.22 o 5 -19 1 518.56 457.37 87.16 o 6 -19 1 24.79 8.25 32.68 o 7 -19 1 21.17 55.41 49.70 o -3 -18 1 31.49 74.43 53.86 o -2 -18 1 78.77 140.84 39.85 o -1 -18 1 144.53 191.56 39.70 o 0 -18 1 332.09 366.82 54.60 o 1 -18 1 0.03 26.85 59.51 o 2 -18 1 149.62 164.98 42.31 o 3 -18 1 11.86 28.25 30.60 o 4 -18 1 96.47 76.72 27.81 o 5 -18 1 349.56 352.79 39.25 o 6 -18 1 29.20 56.46 26.49 o 7 -18 1 2.53 18.94 21.40 o 8 -18 1 68.91 52.43 45.35 o -4 -17 1 53.82 15.21 46.40 o -3 -17 1 9.25 27.58 27.94 o -2 -17 1 14.63 -21.08 35.18 o -1 -17 1 78.47 55.59 30.22 o 0 -17 1 90.27 183.10 34.00 o 1 -17 1 0.12 72.10 22.95 o 2 -17 1 445.10 436.45 35.89 o 3 -17 1 166.24 190.76 32.05 o 4 -17 1 83.29 65.06 22.90 o 5 -17 1 0.43 9.59 15.46 o 6 -17 1 401.71 403.79 37.82 o 7 -17 1 177.79 224.52 39.63 o 8 -17 1 30.73 101.88 43.86 o 9 -17 1 95.69 74.80 41.00 o -5 -16 1 275.86 302.99 49.79 o -4 -16 1 260.09 248.10 38.31 o -3 -16 1 41.28 43.35 38.38 o -2 -16 1 126.74 124.97 30.72 o -1 -16 1 239.71 215.86 38.31 o 0 -16 1 69.40 50.17 18.91 o 1 -16 1 1.18 44.17 16.72 o 2 -16 1 122.93 136.62 25.86 o 3 -16 1 245.30 278.73 25.06 o 4 -16 1 367.23 300.19 26.02 o 5 -16 1 189.72 349.69 35.85 o 6 -16 1 1321.62 1267.66 65.70 o 7 -16 1 35.72 63.05 25.04 o 8 -16 1 24.09 72.06 38.14 o 9 -16 1 50.75 39.51 32.43 o -5 -15 1 36.18 38.00 37.25 o -4 -15 1 35.80 33.42 51.31 o -3 -15 1 277.99 305.54 34.24 o -2 -15 1 0.02 -4.66 17.14 o -1 -15 1 39.79 63.00 22.77 o 0 -15 1 458.88 480.67 44.15 o 1 -15 1 74.75 223.41 31.65 o 2 -15 1 63.45 247.54 44.61 o 3 -15 1 1467.22 1456.09 63.77 o 4 -15 1 1031.35 1640.66 82.10 o 5 -15 1 189.84 212.68 18.79 o 6 -15 1 72.87 100.70 21.05 o 7 -15 1 433.14 483.98 26.02 o 8 -15 1 229.32 224.61 21.94 o 9 -15 1 58.52 -1.37 28.20 o -6 -14 1 4.55 -33.77 38.25 o -5 -14 1 527.23 508.66 66.21 o -4 -14 1 1144.61 1032.00 73.45 o -3 -14 1 229.71 220.70 26.32 o -2 -14 1 927.28 902.05 58.32 o -1 -14 1 539.26 884.66 75.15 o 0 -14 1 8.50 172.26 27.13 o 1 -14 1 912.33 875.53 48.37 o 2 -14 1 793.50 947.96 48.92 o 3 -14 1 58.44 67.31 10.91 o 4 -14 1 1110.34 1456.98 82.09 o 5 -14 1 261.47 196.54 18.36 o 6 -14 1 18.80 97.25 21.77 o 7 -14 1 388.71 347.37 20.68 o 8 -14 1 47.07 66.92 16.79 o 9 -14 1 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