#------------------------------------------------------------------------------ #$Date: 2016-04-02 22:14:57 +0300 (Sat, 02 Apr 2016) $ #$Revision: 180837 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/01/68/2016862.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_2016862_Fobs loop_ _publ_author_name 'Cruz, Silvia' 'Trilleras, Jorge' 'Cobo, Justo' 'Low, John N.' 'Glidewell, Christopher' _publ_section_title ; Four N^7^-benzyl-substituted 4,5,6,7-tetrahydro-1H-pyrazolo[3,4-b]pyridine-5-spiro-1'-cyclohexane-2',6'-diones as ethanol hemisolvates: similar molecular constitutions but different crystal structures ; _journal_coeditor_code GA3109 _journal_issue 12 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first o637 _journal_page_last o642 _journal_volume 64 _journal_year 2008 _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 122.082 _cell_angle_gamma 90.000 _cell_length_a 27.2810 _cell_length_b 10.6438 _cell_length_c 21.5670 _exptl_crystal_F_000 2184.00 _reflns_d_resolution_high 0.7696 _cod_data_source_file ga3109IIIsup4.hkl _cod_data_source_block III #BEGIN Tags that were not found in dictionaries: _shelx_title ' JT_S10' _shelx_refln_list_code 4 _shelx_f_calc_maximum 548.17 _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+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 6 0 0 17346.56 15275.50 162.89 o 8 0 0 10663.03 9376.09 121.95 o 10 0 0 3048.31 2934.11 70.04 o 12 0 0 1140.73 1001.45 52.48 o 14 0 0 11467.76 11877.32 184.57 o 16 0 0 127.30 190.91 54.27 o 18 0 0 1531.46 1584.35 92.09 o 20 0 0 5851.42 6123.28 148.73 o 22 0 0 132.73 66.71 69.22 o 24 0 0 526.04 878.96 111.91 o 26 0 0 1647.51 1858.04 182.69 o 28 0 0 948.89 884.36 183.78 o 30 0 0 50.63 -321.03 248.13 o 3 1 0 300.57 390.73 18.71 o 5 1 0 1318.49 1183.86 25.83 o 7 1 0 4533.56 3942.98 51.98 o 9 1 0 4.99 -12.11 22.74 o 11 1 0 2735.96 2800.46 50.26 o 13 1 0 46.18 56.49 29.96 o 15 1 0 8.79 29.12 35.00 o 17 1 0 21.80 -10.72 38.40 o 19 1 0 3667.30 3702.81 86.30 o 21 1 0 1154.49 966.31 63.96 o 23 1 0 505.51 507.41 61.57 o 25 1 0 59.64 -13.67 71.10 o 27 1 0 25.43 154.20 103.17 o 29 1 0 247.09 54.29 160.13 o 0 2 0 300488.91 331538.94 5382.90 o 2 2 0 57016.85 53093.59 546.82 o 4 2 0 2492.63 2058.55 32.68 o 6 2 0 5110.28 4438.22 57.43 o 8 2 0 1184.14 1074.29 33.46 o 10 2 0 7641.13 8275.42 101.24 o 12 2 0 345.43 326.78 31.44 o 14 2 0 918.70 951.40 47.28 o 16 2 0 679.38 726.48 67.51 o 18 2 0 387.41 307.35 54.63 o 20 2 0 3.26 25.64 62.20 o 22 2 0 1086.70 877.61 64.69 o 24 2 0 23.17 48.48 66.01 o 26 2 0 3177.09 3513.81 152.07 o 28 2 0 225.15 370.07 120.92 o 1 3 0 38064.31 36137.68 314.98 o 3 3 0 803.38 849.07 27.43 o 5 3 0 4218.23 3637.75 52.23 o 7 3 0 5504.69 5021.20 66.61 o 9 3 0 272.32 262.05 25.96 o 11 3 0 320.80 366.53 32.78 o 13 3 0 542.57 521.87 38.89 o 15 3 0 272.46 199.98 50.11 o 17 3 0 1432.24 1399.42 63.65 o 19 3 0 0.12 47.68 47.26 o 21 3 0 2696.13 2878.52 86.67 o 23 3 0 23.25 -34.86 64.96 o 25 3 0 1.11 70.52 76.95 o 27 3 0 86.77 -89.16 119.06 o 29 3 0 161.64 601.66 165.61 o 0 4 0 60865.13 65439.70 1288.80 o 2 4 0 21258.57 21693.47 223.79 o 4 4 0 4008.97 3845.61 59.68 o 6 4 0 66.73 93.10 29.98 o 8 4 0 1833.78 1890.53 47.36 o 10 4 0 413.28 376.86 28.76 o 12 4 0 406.94 332.62 32.05 o 14 4 0 2.24 35.25 36.51 o 16 4 0 459.57 336.26 43.74 o 18 4 0 13.00 19.92 45.39 o 20 4 0 41.27 -5.02 54.55 o 22 4 0 1236.23 1168.95 99.60 o 24 4 0 17.18 103.72 74.96 o 26 4 0 35.26 151.18 102.60 o 28 4 0 62.82 73.31 151.95 o 1 5 0 417.28 366.18 23.63 o 3 5 0 4314.71 4213.97 73.13 o 5 5 0 582.33 570.44 29.64 o 7 5 0 917.91 761.37 37.24 o 9 5 0 0.44 -11.40 27.81 o 11 5 0 63.64 110.36 32.89 o 13 5 0 659.78 670.34 50.81 o 15 5 0 592.85 578.91 45.14 o 17 5 0 83.59 221.49 45.40 o 19 5 0 2296.24 2070.81 75.25 o 21 5 0 6.98 -1.43 61.23 o 23 5 0 94.84 135.75 74.36 o 25 5 0 296.75 326.71 105.11 o 27 5 0 23.39 -171.50 157.41 o 0 6 0 21911.30 24879.30 572.18 o 2 6 0 321.95 341.70 26.03 o 4 6 0 159.37 178.77 29.47 o 6 6 0 7.82 22.43 26.86 o 8 6 0 1783.92 1755.54 56.00 o 10 6 0 219.67 191.68 39.98 o 12 6 0 21.16 27.03 40.93 o 14 6 0 1856.53 2002.02 75.55 o 16 6 0 786.82 830.56 56.38 o 18 6 0 3613.59 3699.78 94.39 o 20 6 0 0.95 -21.23 58.16 o 22 6 0 1507.75 1721.62 94.72 o 24 6 0 3.34 202.78 115.06 o 26 6 0 303.40 32.94 184.49 o 1 7 0 370.29 315.03 30.64 o 3 7 0 423.26 352.11 33.53 o 5 7 0 409.51 358.10 43.19 o 7 7 0 8.08 5.80 31.04 o 9 7 0 50.73 53.20 39.42 o 11 7 0 59.70 53.95 43.21 o 13 7 0 187.68 133.49 48.89 o 15 7 0 55.56 72.54 60.68 o 17 7 0 98.45 197.23 58.83 o 19 7 0 2129.72 2304.66 103.18 o 21 7 0 230.57 31.16 107.63 o 23 7 0 13.17 317.49 164.70 o 25 7 0 99.20 215.27 181.90 o 0 8 0 367.14 461.57 63.69 o 2 8 0 7.83 -7.63 27.10 o 4 8 0 387.33 349.32 34.74 o 6 8 0 267.07 304.45 49.21 o 8 8 0 3.34 2.38 43.56 o 10 8 0 1264.27 1166.49 63.82 o 12 8 0 4181.19 4736.81 122.44 o 14 8 0 7268.90 8692.23 187.56 o 16 8 0 1566.99 1915.07 114.73 o 18 8 0 93.29 141.72 86.63 o 20 8 0 271.68 275.35 113.99 o 22 8 0 0.24 -68.31 169.72 o 24 8 0 1.00 -188.37 214.34 o 1 9 0 1201.22 1347.85 60.87 o 3 9 0 121.59 125.29 41.80 o 5 9 0 683.79 608.84 54.50 o 7 9 0 42.04 26.62 43.75 o 9 9 0 818.97 857.05 64.17 o 11 9 0 35.59 -13.88 54.95 o 13 9 0 396.63 458.87 73.29 o 15 9 0 45.16 -37.81 84.59 o 17 9 0 642.13 575.10 105.72 o 19 9 0 53.38 114.93 150.96 o 21 9 0 67.65 514.21 247.90 o 0 10 0 690.15 711.78 64.76 o 2 10 0 231.02 175.15 43.11 o 4 10 0 234.70 150.98 38.85 o 6 10 0 42.43 41.25 48.64 o 8 10 0 243.98 79.00 76.67 o 10 10 0 239.39 152.50 59.50 o 12 10 0 421.70 322.25 79.12 o 14 10 0 2179.09 2507.82 134.09 o 16 10 0 430.83 238.61 158.90 o 18 10 0 113.02 224.52 175.38 o 20 10 0 94.48 167.22 201.05 o 1 11 0 405.98 395.24 49.08 o 3 11 0 97.45 -9.56 47.60 o 5 11 0 992.00 872.56 79.45 o 7 11 0 699.02 414.35 67.74 o 9 11 0 420.06 424.95 102.11 o 11 11 0 804.84 891.35 122.75 o 13 11 0 386.93 192.64 153.26 o 15 11 0 103.96 285.13 158.30 o 17 11 0 129.35 245.90 193.39 o 0 12 0 141.66 169.48 72.74 o 2 12 0 484.36 593.85 74.62 o 4 12 0 48.88 103.00 76.65 o 6 12 0 0.25 -108.82 91.40 o 8 12 0 426.81 205.04 124.77 o 10 12 0 90.14 260.19 140.57 o 12 12 0 1.15 -115.72 186.95 o 14 12 0 53.70 187.33 171.05 o 1 13 0 193.03 278.40 165.21 o 3 13 0 0.62 -90.64 224.93 o 5 13 0 3.11 11.23 161.32 o 7 13 0 7.34 138.33 187.87 o 9 13 0 3.59 -28.31 174.13 o -29 1 1 36.69 141.43 137.60 o -27 1 1 1342.89 1511.12 115.21 o -25 1 1 2.08 46.33 64.55 o -23 1 1 55.85 16.48 55.14 o -21 1 1 1472.87 1579.86 72.44 o -19 1 1 105.90 98.01 45.00 o -17 1 1 1383.55 1357.38 53.31 o -15 1 1 1151.03 1151.78 44.17 o -13 1 1 119.20 123.27 33.12 o -11 1 1 532.63 458.18 29.30 o -9 1 1 472.15 424.47 26.63 o -7 1 1 7488.61 7374.00 70.86 o -5 1 1 1566.97 1696.71 34.56 o -3 1 1 1373.03 656.89 54.70 o 3 1 1 753.28 1038.40 35.92 o 5 1 1 394.60 441.45 26.90 o 7 1 1 2444.51 2560.45 46.47 o 9 1 1 12.38 50.62 30.27 o 11 1 1 2052.75 2054.29 50.41 o 13 1 1 984.68 942.48 44.37 o 15 1 1 835.46 853.81 47.53 o 17 1 1 1553.89 1413.96 58.21 o 19 1 1 21.63 98.59 48.52 o 21 1 1 52.17 21.66 56.47 o 23 1 1 355.28 185.03 73.91 o 25 1 1 89.52 240.09 89.54 o 27 1 1 828.71 561.33 120.51 o 29 1 1 40.33 -52.83 155.46 o -30 2 1 36.52 151.95 123.58 o -28 2 1 68.12 263.14 110.96 o -26 2 1 826.94 1039.97 131.19 o -24 2 1 105.54 -7.81 66.97 o -22 2 1 382.98 378.92 63.20 o -20 2 1 979.50 970.76 59.94 o -18 2 1 210.87 138.35 44.78 o -16 2 1 230.80 327.47 42.13 o -14 2 1 204.96 214.99 34.08 o -12 2 1 411.84 513.06 31.19 o -10 2 1 636.53 637.25 30.21 o -8 2 1 16595.92 16192.00 135.80 o -6 2 1 5369.62 4831.90 55.76 o -4 2 1 13016.70 13207.47 108.15 o -2 2 1 60630.31 63443.22 763.95 o 0 2 1 11760.96 8202.47 145.59 o 2 2 1 7090.08 5434.98 70.63 o 4 2 1 346.77 374.28 29.67 o 6 2 1 1591.21 1314.46 35.12 o 8 2 1 1108.82 1155.16 35.86 o 10 2 1 268.44 408.48 30.08 o 12 2 1 0.66 21.96 32.38 o 14 2 1 44.96 39.18 34.66 o 16 2 1 3146.47 3227.61 76.82 o 18 2 1 52.92 70.45 45.32 o 20 2 1 19.49 -8.07 47.95 o 22 2 1 55.81 16.25 56.22 o 24 2 1 14.89 88.66 67.99 o 26 2 1 8.35 -45.29 94.39 o 28 2 1 185.32 194.60 125.48 o -29 3 1 0.63 -114.53 120.67 o -27 3 1 0.87 -16.81 95.93 o -25 3 1 35.95 54.85 74.03 o -23 3 1 21.26 -20.28 60.68 o -21 3 1 67.85 43.33 49.73 o -19 3 1 527.90 440.60 55.83 o -17 3 1 3433.69 3503.12 78.79 o -15 3 1 937.96 892.45 47.79 o -13 3 1 399.95 420.04 37.69 o -11 3 1 384.76 397.65 30.47 o -9 3 1 73.17 112.94 27.60 o -7 3 1 379.44 329.33 20.64 o -5 3 1 1381.03 1472.63 36.10 o -3 3 1 47150.18 45175.63 535.80 o -1 3 1 15309.32 13690.14 129.23 o 1 3 1 12960.76 13196.92 151.16 o 3 3 1 7276.80 6436.14 85.07 o 5 3 1 140.96 167.75 18.64 o 7 3 1 45.78 91.00 20.43 o 9 3 1 1488.62 1421.11 42.46 o 11 3 1 19782.04 22152.46 201.02 o 13 3 1 77.20 48.92 32.26 o 15 3 1 4814.43 4999.71 90.03 o 17 3 1 840.76 960.46 57.43 o 19 3 1 2841.84 2791.37 80.18 o 21 3 1 268.86 141.64 62.21 o 23 3 1 539.69 518.68 81.56 o 25 3 1 1052.85 1418.61 106.65 o 27 3 1 5.34 -16.65 112.88 o -28 4 1 175.27 213.05 182.78 o -26 4 1 337.70 495.72 92.20 o -24 4 1 101.33 85.58 78.03 o -22 4 1 2432.32 2646.87 101.53 o -20 4 1 25.82 22.84 50.17 o -18 4 1 929.21 1055.41 63.91 o -16 4 1 145.08 191.72 44.72 o -14 4 1 2274.07 2308.64 59.29 o -12 4 1 2827.24 2956.65 57.49 o -10 4 1 2360.87 2294.37 48.14 o -8 4 1 3179.13 3131.81 55.61 o -6 4 1 1328.77 988.96 34.08 o -4 4 1 143.05 243.42 25.99 o -2 4 1 10745.36 9786.61 101.47 o 0 4 1 2692.97 2480.68 42.22 o 2 4 1 1342.75 1251.29 38.00 o 4 4 1 915.75 990.63 38.73 o 6 4 1 31.97 8.03 29.97 o 8 4 1 5512.50 5665.55 80.12 o 10 4 1 519.07 496.28 33.41 o 12 4 1 17.48 38.78 42.79 o 14 4 1 2015.21 1961.76 69.70 o 16 4 1 46.84 19.10 49.24 o 18 4 1 2092.42 2391.73 76.86 o 20 4 1 16.53 -3.65 55.84 o 22 4 1 1069.62 1183.09 83.49 o 24 4 1 346.58 306.46 100.94 o 26 4 1 14.99 118.22 113.76 o 28 4 1 50.53 207.91 273.02 o -27 5 1 26.45 51.20 151.27 o -25 5 1 571.04 624.49 103.34 o -23 5 1 61.69 -4.87 67.75 o -21 5 1 2.94 40.25 57.86 o -19 5 1 1654.83 1506.57 64.31 o -17 5 1 1368.08 1504.76 58.60 o -15 5 1 2925.63 2903.40 66.27 o -13 5 1 345.19 309.58 31.69 o -11 5 1 541.54 563.03 37.41 o -9 5 1 1441.35 1556.92 60.85 o -7 5 1 9981.13 10336.96 124.51 o -5 5 1 356.25 347.01 26.18 o -3 5 1 22239.63 23422.06 221.69 o -1 5 1 6175.07 6548.40 98.28 o 1 5 1 6.53 -12.39 25.00 o 3 5 1 95.50 162.10 31.62 o 5 5 1 2489.60 2261.90 57.29 o 7 5 1 593.74 547.80 38.38 o 9 5 1 206.69 183.37 35.23 o 11 5 1 49.09 63.04 29.75 o 13 5 1 2117.43 2252.76 69.17 o 15 5 1 3971.03 3751.95 86.33 o 17 5 1 0.79 16.26 45.26 o 19 5 1 232.91 216.10 57.06 o 21 5 1 995.03 890.30 75.41 o 23 5 1 246.32 261.13 92.50 o 25 5 1 2211.08 2725.97 188.82 o 27 5 1 139.62 15.21 173.68 o -26 6 1 605.55 763.30 172.22 o -24 6 1 514.68 393.21 103.58 o -22 6 1 2583.35 2727.50 98.70 o -20 6 1 4387.16 5227.00 152.85 o -18 6 1 939.04 763.52 75.85 o -16 6 1 164.68 210.88 57.99 o -14 6 1 438.90 313.20 47.14 o -12 6 1 12.13 39.38 40.63 o -10 6 1 136.61 150.17 47.59 o -8 6 1 2814.78 2998.02 65.63 o -6 6 1 132.07 91.86 24.08 o -4 6 1 73.55 125.32 26.45 o -2 6 1 526.35 584.87 28.62 o 0 6 1 719.59 549.19 30.37 o 2 6 1 186.45 163.51 23.49 o 4 6 1 336.03 318.33 30.24 o 6 6 1 179.10 172.14 30.91 o 8 6 1 558.56 480.01 42.60 o 10 6 1 6.17 11.15 35.44 o 12 6 1 443.75 598.07 56.70 o 14 6 1 451.99 447.97 67.59 o 16 6 1 125.80 79.04 41.46 o 18 6 1 82.98 25.98 53.31 o 20 6 1 610.85 621.43 68.10 o 22 6 1 0.13 104.46 91.24 o 24 6 1 87.24 37.75 125.67 o 26 6 1 0.04 75.99 294.73 o -25 7 1 31.47 -83.10 171.45 o -23 7 1 5.81 -19.52 103.97 o -21 7 1 4064.08 4863.01 140.74 o -19 7 1 41.95 41.17 70.65 o -17 7 1 221.32 197.63 57.08 o -15 7 1 1634.91 1539.96 74.37 o -13 7 1 11.93 -14.95 47.90 o -11 7 1 2971.22 3258.30 84.01 o -9 7 1 81.20 88.44 38.84 o -7 7 1 306.44 394.10 35.82 o -5 7 1 45.44 75.80 26.63 o -3 7 1 54.30 106.90 30.02 o -1 7 1 1189.77 1310.84 44.04 o 1 7 1 194.67 103.65 27.97 o 3 7 1 3147.19 3470.51 79.64 o 5 7 1 126.40 80.35 32.00 o 7 7 1 303.27 242.62 39.35 o 9 7 1 1725.42 1863.06 69.39 o 11 7 1 251.30 204.57 76.93 o 13 7 1 2512.51 2774.62 89.48 o 15 7 1 0.31 65.87 65.67 o 17 7 1 1440.38 1638.51 82.30 o 19 7 1 659.88 643.09 85.32 o 21 7 1 781.47 808.17 114.87 o 23 7 1 7.48 150.55 175.74 o 25 7 1 1091.81 1107.73 257.30 o -24 8 1 1.58 96.74 180.51 o -22 8 1 128.19 484.83 169.72 o -20 8 1 3245.78 3822.70 268.03 o -18 8 1 1246.89 1266.23 117.36 o -16 8 1 13.32 149.88 66.88 o -14 8 1 1109.57 1356.41 108.18 o -12 8 1 3.51 71.22 59.90 o -10 8 1 722.39 693.09 58.23 o -8 8 1 641.24 513.15 60.66 o -6 8 1 376.60 420.75 40.16 o -4 8 1 419.64 453.37 41.95 o -2 8 1 3058.47 3194.64 68.89 o 0 8 1 56.89 95.66 30.46 o 2 8 1 215.03 201.88 29.45 o 4 8 1 171.82 74.33 35.67 o 6 8 1 506.05 562.04 45.99 o 8 8 1 0.08 23.89 35.83 o 10 8 1 3.56 15.31 58.45 o 12 8 1 34.89 -58.39 55.66 o 14 8 1 30.93 -36.72 59.77 o 16 8 1 257.45 268.08 73.30 o 18 8 1 2.16 55.43 93.53 o 20 8 1 228.97 19.24 150.86 o 22 8 1 266.08 208.20 176.61 o -23 9 1 568.55 735.79 245.56 o -21 9 1 217.99 506.43 179.85 o -19 9 1 1256.75 1661.54 194.30 o -17 9 1 383.92 456.18 91.98 o -15 9 1 330.62 314.24 72.66 o -13 9 1 322.87 337.93 82.41 o -11 9 1 2552.91 2443.37 103.17 o -9 9 1 2477.70 2836.24 101.09 o -7 9 1 5403.24 6382.88 126.24 o -5 9 1 257.68 153.50 38.20 o -3 9 1 165.80 103.16 31.72 o -1 9 1 45.86 -14.92 33.26 o 1 9 1 744.01 840.99 41.24 o 3 9 1 211.78 214.00 37.11 o 5 9 1 1211.72 1374.02 71.50 o 7 9 1 752.92 746.31 70.12 o 9 9 1 18.12 52.11 56.14 o 11 9 1 137.85 214.75 54.57 o 13 9 1 1710.72 1940.52 120.11 o 15 9 1 37.07 73.34 89.95 o 17 9 1 492.58 400.03 120.64 o 19 9 1 81.12 58.37 158.57 o 21 9 1 420.23 469.93 194.22 o -20 10 1 5.48 84.40 180.10 o -18 10 1 159.22 -197.30 193.79 o -16 10 1 26.87 -8.20 126.78 o -14 10 1 590.59 489.34 106.49 o -12 10 1 2.05 -58.19 97.82 o -10 10 1 227.36 156.75 57.75 o -8 10 1 322.37 211.41 60.23 o -6 10 1 74.80 107.52 48.72 o -4 10 1 4.54 13.85 40.95 o -2 10 1 445.74 373.10 56.06 o 0 10 1 2.81 22.93 33.99 o 2 10 1 16.50 45.38 35.25 o 4 10 1 515.70 444.49 61.82 o 6 10 1 8.02 -21.57 67.28 o 8 10 1 377.02 296.97 83.78 o 10 10 1 64.18 -17.57 79.72 o 12 10 1 0.24 -93.64 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