#------------------------------------------------------------------------------ #$Date: 2016-04-02 22:14:57 +0300 (Sat, 02 Apr 2016) $ #$Revision: 180837 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/01/68/2016860.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_2016860_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 122.625 _cell_angle_gamma 90.000 _cell_length_a 27.4190 _cell_length_b 10.5860 _cell_length_c 21.5800 _exptl_crystal_F_000 2248.00 _reflns_d_resolution_high 0.7689 _cod_data_source_file ga3109Isup2.hkl _cod_data_source_block I #BEGIN Tags that were not found in dictionaries: _shelx_title ' JTS5' _shelx_refln_list_code 4 _shelx_f_calc_maximum 395.51 _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 31954.59 29524.08 807.45 o 6 0 0 8799.07 8144.03 185.04 o 8 0 0 9369.12 9349.87 212.69 o 10 0 0 12011.85 10136.70 254.00 o 12 0 0 144.55 127.72 19.93 o 14 0 0 24406.58 24093.81 603.01 o 16 0 0 981.24 920.40 38.21 o 18 0 0 2952.96 2690.53 78.97 o 20 0 0 16845.68 17290.22 438.82 o 22 0 0 3.25 -13.61 31.23 o 24 0 0 2291.10 2575.41 89.63 o 26 0 0 2451.81 2858.11 98.41 o 28 0 0 926.84 1045.49 80.54 o 30 0 0 1011.42 1364.93 106.40 o 3 1 0 584.31 719.16 17.82 o 5 1 0 185.35 220.91 10.67 o 7 1 0 5968.76 5412.35 102.12 o 9 1 0 767.58 612.35 17.60 o 11 1 0 4773.69 5010.65 91.78 o 13 1 0 14.19 -8.46 14.12 o 15 1 0 723.80 570.60 22.32 o 17 1 0 211.50 146.55 23.66 o 19 1 0 7247.84 7254.37 133.11 o 21 1 0 3025.15 2835.08 63.11 o 23 1 0 994.81 1041.03 35.18 o 25 1 0 59.33 96.93 26.06 o 27 1 0 183.27 208.26 27.02 o 29 1 0 461.89 581.76 34.39 o 2 2 0 64346.54 57856.90 1821.61 o 4 2 0 878.40 900.26 31.08 o 6 2 0 1133.34 1042.19 23.80 o 8 2 0 496.98 463.49 15.17 o 10 2 0 16274.93 16465.33 288.32 o 12 2 0 84.50 105.16 13.75 o 14 2 0 1882.00 1819.40 40.43 o 16 2 0 141.58 110.36 19.73 o 18 2 0 164.05 116.55 19.29 o 20 2 0 286.35 280.60 23.93 o 22 2 0 1170.61 971.44 35.63 o 24 2 0 10.11 -16.73 24.37 o 26 2 0 2117.24 2202.23 58.02 o 28 2 0 30.24 25.45 29.87 o 1 3 0 70371.52 65626.91 3030.22 o 3 3 0 2382.62 2455.00 60.27 o 5 3 0 298.90 306.88 14.15 o 7 3 0 3446.12 3218.50 67.70 o 9 3 0 3609.35 3101.18 58.16 o 11 3 0 1759.32 1321.46 43.08 o 13 3 0 191.13 191.35 17.85 o 15 3 0 4443.45 4244.65 80.37 o 17 3 0 741.60 622.34 26.20 o 19 3 0 559.00 540.48 29.16 o 21 3 0 865.44 785.65 28.03 o 23 3 0 19.36 32.44 23.09 o 25 3 0 677.26 810.66 37.71 o 27 3 0 56.09 4.20 24.79 o 29 3 0 19.08 -5.83 37.16 o 0 4 0 35884.00 35808.36 3260.14 o 2 4 0 22524.29 24617.56 485.66 o 4 4 0 8733.65 9218.30 200.00 o 6 4 0 1647.37 1449.84 34.72 o 8 4 0 2263.80 2277.32 52.95 o 10 4 0 4125.63 4205.96 91.71 o 12 4 0 503.07 393.56 20.72 o 14 4 0 503.14 558.56 22.61 o 16 4 0 1465.52 1385.76 39.17 o 18 4 0 66.97 54.32 18.90 o 20 4 0 1397.26 1231.65 35.32 o 22 4 0 1547.94 1392.10 39.51 o 24 4 0 385.01 336.54 30.06 o 26 4 0 185.06 162.34 30.69 o 28 4 0 184.32 238.15 41.86 o 1 5 0 804.41 831.37 27.85 o 3 5 0 5269.59 5129.61 118.62 o 5 5 0 627.74 683.64 25.87 o 7 5 0 202.20 145.70 19.83 o 9 5 0 250.61 214.56 16.38 o 11 5 0 17.10 -14.69 16.39 o 13 5 0 1027.19 1069.10 33.42 o 15 5 0 863.36 762.36 39.75 o 17 5 0 2.25 -31.70 26.60 o 19 5 0 4432.34 4014.92 110.17 o 21 5 0 134.38 118.91 20.01 o 23 5 0 21.86 20.85 20.74 o 25 5 0 335.67 382.09 29.30 o 27 5 0 89.36 78.73 50.44 o 0 6 0 42388.36 46407.93 1852.97 o 2 6 0 13.75 -13.77 16.84 o 4 6 0 475.76 382.74 18.93 o 6 6 0 982.70 1048.22 31.72 o 8 6 0 2638.41 2433.64 55.41 o 10 6 0 674.56 647.94 23.53 o 12 6 0 174.68 150.72 18.96 o 14 6 0 202.31 241.19 24.94 o 16 6 0 3613.22 3703.31 88.17 o 18 6 0 5911.95 5698.17 149.76 o 20 6 0 451.89 432.13 28.50 o 22 6 0 1198.05 1200.42 43.91 o 24 6 0 65.77 -10.22 31.74 o 26 6 0 1037.49 1101.70 52.54 o 1 7 0 5.40 10.64 16.69 o 3 7 0 788.82 868.62 44.33 o 5 7 0 52.59 60.38 21.70 o 7 7 0 437.36 369.70 24.30 o 9 7 0 781.98 821.99 35.39 o 11 7 0 121.33 107.74 20.28 o 13 7 0 735.35 711.74 30.95 o 15 7 0 26.27 26.58 19.52 o 17 7 0 938.67 928.37 45.54 o 19 7 0 4555.88 4705.69 132.44 o 21 7 0 65.23 92.14 30.31 o 23 7 0 2.76 -43.27 32.05 o 25 7 0 237.34 288.95 36.60 o 0 8 0 151.99 280.27 32.88 o 2 8 0 34.14 100.59 20.57 o 4 8 0 449.91 427.82 22.33 o 6 8 0 299.16 381.20 25.29 o 8 8 0 74.81 43.57 21.19 o 10 8 0 2012.92 1971.42 57.99 o 12 8 0 4391.23 4236.35 131.73 o 14 8 0 8134.43 7845.99 205.00 o 16 8 0 1634.27 1530.80 54.75 o 18 8 0 45.48 23.95 25.68 o 20 8 0 88.16 133.19 30.44 o 22 8 0 15.97 -50.24 33.50 o 24 8 0 38.76 37.55 48.31 o 1 9 0 3422.84 3969.02 92.36 o 3 9 0 111.12 125.46 20.20 o 5 9 0 46.92 85.50 18.54 o 7 9 0 199.99 200.20 51.56 o 9 9 0 242.11 242.15 28.92 o 11 9 0 66.73 64.42 24.88 o 13 9 0 1120.16 1033.60 43.00 o 15 9 0 1126.56 896.64 60.93 o 17 9 0 767.82 703.58 40.13 o 19 9 0 1.08 24.32 28.68 o 21 9 0 490.12 553.96 62.51 o 0 10 0 2295.15 2677.78 88.57 o 2 10 0 199.20 221.51 21.40 o 4 10 0 53.53 143.07 29.66 o 6 10 0 4.23 28.12 24.60 o 8 10 0 313.15 258.18 31.45 o 10 10 0 825.74 806.02 34.98 o 12 10 0 519.94 486.14 28.86 o 14 10 0 4095.65 3731.25 108.24 o 16 10 0 272.55 367.52 54.92 o 18 10 0 308.14 430.84 100.16 o 20 10 0 529.56 775.40 111.92 o 1 11 0 1017.28 1193.75 36.92 o 3 11 0 192.24 205.40 23.43 o 5 11 0 1913.04 2063.81 59.88 o 7 11 0 841.65 906.95 38.41 o 9 11 0 731.92 803.67 39.57 o 11 11 0 2347.13 2273.90 74.47 o 13 11 0 864.77 587.34 47.55 o 15 11 0 515.54 679.74 99.96 o 17 11 0 152.16 28.05 64.24 o 0 12 0 1516.89 1727.33 78.02 o 2 12 0 632.73 899.69 32.74 o 4 12 0 272.88 315.07 31.32 o 6 12 0 77.75 32.52 26.42 o 8 12 0 605.25 628.37 34.26 o 10 12 0 739.84 774.21 47.50 o 12 12 0 0.47 28.85 69.85 o 14 12 0 0.24 12.82 59.70 o 1 13 0 611.05 713.66 68.77 o 3 13 0 22.61 54.03 30.87 o 5 13 0 0.69 0.13 32.03 o 7 13 0 20.22 135.55 49.20 o -29 1 1 265.15 274.62 33.39 o -27 1 1 1953.05 2056.86 58.21 o -25 1 1 281.60 288.88 25.61 o -23 1 1 148.85 117.54 24.56 o -21 1 1 813.24 757.00 29.13 o -19 1 1 526.49 487.75 24.46 o -17 1 1 869.29 942.46 29.84 o -15 1 1 37.11 10.50 15.56 o -13 1 1 416.75 382.33 20.25 o -11 1 1 0.19 -13.75 13.26 o -9 1 1 557.98 397.38 14.83 o -7 1 1 5643.54 6003.48 114.61 o -5 1 1 7632.76 7117.59 125.12 o -3 1 1 6445.92 6691.69 151.86 o 3 1 1 596.85 724.79 22.63 o 5 1 1 399.83 418.00 15.00 o 7 1 1 122.60 167.22 14.01 o 9 1 1 65.35 -23.47 15.65 o 11 1 1 1.11 18.64 16.97 o 13 1 1 495.24 443.08 19.78 o 15 1 1 4320.61 4167.63 80.26 o 17 1 1 4397.87 4273.09 93.41 o 19 1 1 92.75 56.52 25.46 o 21 1 1 608.78 570.04 30.67 o 23 1 1 270.07 285.48 26.65 o 25 1 1 884.97 880.86 35.15 o 27 1 1 266.63 301.89 32.98 o 29 1 1 180.62 201.80 35.66 o -30 2 1 414.63 424.25 39.97 o -28 2 1 72.30 114.34 37.03 o -26 2 1 1647.28 1840.80 51.58 o -24 2 1 865.84 874.47 31.51 o -22 2 1 1078.40 997.08 31.85 o -20 2 1 11.59 -10.58 17.87 o -18 2 1 1659.63 1632.60 37.39 o -16 2 1 47.93 19.54 20.47 o -14 2 1 735.65 558.66 19.87 o -12 2 1 384.13 467.22 20.74 o -10 2 1 158.33 39.62 18.60 o -8 2 1 8533.32 9272.88 172.57 o -6 2 1 1722.00 1743.46 36.10 o -4 2 1 25613.26 25997.63 520.60 o -2 2 1 58260.35 57981.63 2215.18 o 0 2 1 19380.89 17068.94 482.16 o 2 2 1 16918.32 15527.51 366.21 o 4 2 1 9.42 59.40 20.60 o 6 2 1 9114.67 8595.53 158.84 o 8 2 1 307.87 270.34 15.35 o 10 2 1 3412.44 3648.44 74.21 o 12 2 1 507.59 517.62 19.73 o 14 2 1 70.27 59.86 18.95 o 16 2 1 8966.88 8777.83 159.50 o 18 2 1 660.48 522.70 26.50 o 20 2 1 649.90 565.90 26.56 o 22 2 1 38.77 -22.61 21.39 o 24 2 1 128.47 156.68 35.55 o 26 2 1 356.59 457.25 31.75 o 28 2 1 103.38 138.31 49.87 o -29 3 1 1.82 1.66 32.07 o -27 3 1 101.15 132.81 46.33 o -25 3 1 10.49 1.58 28.73 o -23 3 1 91.94 28.09 20.64 o -21 3 1 10.02 -23.92 20.33 o -19 3 1 473.64 506.39 22.13 o -17 3 1 3911.92 3893.00 72.06 o -15 3 1 550.22 539.74 20.97 o -13 3 1 337.32 372.82 17.11 o -11 3 1 304.11 320.40 14.11 o -9 3 1 43.01 97.17 15.89 o -7 3 1 384.09 334.11 19.11 o -5 3 1 1152.29 1351.72 33.29 o -3 3 1 44880.32 43707.73 925.63 o -1 3 1 19634.76 21095.36 747.24 o 1 3 1 12111.03 13154.35 317.02 o 3 3 1 8379.37 7946.07 157.07 o 5 3 1 82.09 90.38 11.93 o 7 3 1 1.28 -23.80 16.61 o 9 3 1 1440.14 1578.67 37.69 o 11 3 1 19049.78 20482.26 380.99 o 13 3 1 216.74 179.21 19.86 o 15 3 1 5409.24 5400.83 101.36 o 17 3 1 941.09 1073.24 32.42 o 19 3 1 2873.32 2861.04 63.36 o 21 3 1 217.13 123.67 22.75 o 23 3 1 819.50 740.29 30.41 o 25 3 1 1222.78 1339.52 43.77 o 27 3 1 2.44 -9.36 32.78 o -28 4 1 131.43 263.26 48.61 o -26 4 1 435.77 535.97 31.87 o -24 4 1 812.93 794.24 29.20 o -22 4 1 3944.55 4096.81 92.40 o -20 4 1 458.56 337.36 23.17 o -18 4 1 309.17 297.64 23.30 o -16 4 1 15.67 -10.86 16.44 o -14 4 1 5594.59 5917.23 108.40 o -12 4 1 4423.49 4832.23 94.48 o -10 4 1 8299.48 7807.90 168.23 o -8 4 1 7265.85 7085.65 142.28 o -6 4 1 455.30 367.93 15.66 o -4 4 1 2185.69 2231.86 52.77 o -2 4 1 13779.13 13647.80 290.79 o 0 4 1 12895.20 12603.54 278.70 o 2 4 1 3695.85 3433.95 86.73 o 4 4 1 137.05 123.09 20.02 o 6 4 1 1778.20 1794.79 45.84 o 8 4 1 8549.21 9145.40 183.66 o 10 4 1 2653.83 2527.73 53.98 o 12 4 1 1196.80 1235.60 41.85 o 14 4 1 3615.21 3563.84 73.48 o 16 4 1 1565.38 1406.10 39.36 o 18 4 1 3354.50 3410.00 72.75 o 20 4 1 100.64 87.89 22.70 o 22 4 1 2370.36 2487.00 58.16 o 24 4 1 716.80 735.79 30.36 o 26 4 1 302.54 360.65 37.34 o 28 4 1 0.10 7.48 64.91 o -27 5 1 60.13 72.00 40.20 o -25 5 1 1734.14 1995.88 55.62 o -23 5 1 21.32 38.77 20.40 o -21 5 1 113.46 111.46 21.63 o -19 5 1 435.91 281.53 26.34 o -17 5 1 1783.90 1943.79 50.04 o -15 5 1 8480.92 8489.79 172.60 o -13 5 1 1177.93 1138.58 32.90 o -11 5 1 2529.55 2517.88 58.22 o -9 5 1 111.59 224.43 16.30 o -7 5 1 12727.21 13063.55 258.63 o -5 5 1 3952.81 3903.17 91.21 o -3 5 1 27705.74 30865.57 611.79 o -1 5 1 9099.65 9385.22 212.52 o 1 5 1 2179.79 1993.16 50.77 o 3 5 1 96.00 83.91 12.16 o 5 5 1 8954.62 8388.22 194.13 o 7 5 1 3301.85 3076.96 70.59 o 9 5 1 1079.19 1131.98 30.77 o 11 5 1 1459.20 1555.19 43.27 o 13 5 1 3282.75 3356.07 80.04 o 15 5 1 8697.81 8318.74 181.56 o 17 5 1 899.05 788.14 33.31 o 19 5 1 1094.92 1055.09 39.44 o 21 5 1 1756.65 1696.22 51.32 o 23 5 1 313.60 289.17 22.25 o 25 5 1 3588.45 3729.12 157.11 o 27 5 1 33.07 47.17 45.96 o -26 6 1 1264.71 1114.93 55.81 o -24 6 1 822.25 781.43 43.87 o -22 6 1 2603.44 2556.70 71.77 o -20 6 1 4757.05 4875.85 106.66 o -18 6 1 1871.33 1702.07 49.09 o -16 6 1 135.46 159.36 22.03 o -14 6 1 600.22 471.76 23.53 o -12 6 1 1.31 20.91 21.32 o -10 6 1 210.39 219.66 19.12 o -8 6 1 2035.98 2162.83 53.74 o -6 6 1 132.22 81.73 16.81 o -4 6 1 12.75 38.82 15.73 o -2 6 1 584.66 677.56 25.41 o 0 6 1 394.68 364.33 34.74 o 2 6 1 38.40 33.01 14.08 o 4 6 1 415.28 455.12 18.89 o 6 6 1 182.44 167.16 18.64 o 8 6 1 672.98 605.12 23.48 o 10 6 1 9.42 24.77 16.27 o 12 6 1 796.53 675.86 32.10 o 14 6 1 567.63 571.83 28.37 o 16 6 1 184.50 187.69 26.30 o 18 6 1 166.76 151.52 25.60 o 20 6 1 625.48 566.62 30.92 o 22 6 1 8.02 -9.34 26.80 o 24 6 1 205.25 154.32 35.09 o 26 6 1 1.50 -12.33 49.16 o -25 7 1 415.42 423.42 41.43 o -23 7 1 182.53 223.38 30.27 o -21 7 1 5046.00 5366.20 279.28 o -19 7 1 716.35 725.51 39.35 o -17 7 1 569.06 502.92 25.48 o -15 7 1 3908.17 3691.98 95.84 o -13 7 1 279.99 234.52 21.27 o -11 7 1 4055.98 4070.16 102.18 o -9 7 1 671.42 618.58 28.56 o -7 7 1 21.97 39.51 14.89 o -5 7 1 661.12 734.58 24.39 o -3 7 1 249.36 203.69 18.00 o -1 7 1 201.07 319.77 22.47 o 1 7 1 327.01 425.01 23.69 o 3 7 1 6233.11 6429.52 140.51 o 5 7 1 1896.37 1881.47 53.15 o 7 7 1 2091.55 2136.42 59.03 o 9 7 1 2978.59 3020.99 85.94 o 11 7 1 35.63 129.10 29.70 o 13 7 1 2055.73 2091.47 68.49 o 15 7 1 327.51 302.27 25.71 o 17 7 1 3468.13 3376.11 90.16 o 19 7 1 272.30 265.47 30.85 o 21 7 1 193.80 220.97 31.01 o 23 7 1 32.43 6.48 38.74 o 25 7 1 336.75 231.19 149.91 o -24 8 1 181.68 360.78 57.98 o -22 8 1 123.27 22.57 41.51 o -20 8 1 2139.61 2075.42 81.36 o -18 8 1 2848.68 2739.38 100.77 o -16 8 1 5.41 -42.48 28.77 o -14 8 1 5090.10 4976.92 169.97 o -12 8 1 11.33 31.95 23.72 o -10 8 1 4277.64 4012.74 101.77 o -8 8 1 139.35 174.94 21.67 o -6 8 1 87.72 151.75 17.50 o -4 8 1 2838.15 2775.76 66.77 o -2 8 1 6182.79 6388.53 151.71 o 0 8 1 3060.29 3262.96 76.85 o 2 8 1 2241.46 2488.15 75.57 o 4 8 1 1.10 -13.73 20.08 o 6 8 1 2920.93 3185.31 82.76 o 8 8 1 428.46 474.59 27.08 o 10 8 1 1154.79 1136.83 45.20 o 12 8 1 908.88 780.09 39.71 o 14 8 1 421.74 358.67 26.63 o 16 8 1 1651.04 1668.40 60.05 o 18 8 1 481.54 543.60 37.66 o 20 8 1 1203.91 1134.49 55.82 o 22 8 1 800.06 872.85 88.91 o -23 9 1 578.87 482.39 78.66 o -21 9 1 71.99 24.03 26.49 o -19 9 1 1562.42 1249.13 80.54 o -17 9 1 581.82 514.71 47.96 o -15 9 1 392.88 358.74 28.87 o -13 9 1 424.33 386.64 27.15 o -11 9 1 3519.31 3278.00 86.58 o -9 9 1 3200.61 3175.42 83.90 o -7 9 1 7705.18 7779.31 170.86 o -5 9 1 66.60 64.97 28.55 o -3 9 1 64.92 -0.80 19.28 o -1 9 1 28.96 142.17 26.41 o 1 9 1 796.50 924.17 34.21 o 3 9 1 8.74 114.22 22.90 o 5 9 1 752.87 810.62 30.06 o 7 9 1 652.84 564.50 31.74 o 9 9 1 234.04 219.66 24.16 o 11 9 1 119.66 36.24 23.94 o 13 9 1 1978.21 1899.64 64.18 o 15 9 1 18.90 -39.73 36.25 o 17 9 1 768.99 729.57 47.12 o 19 9 1 10.39 26.16 29.65 o 21 9 1 575.72 573.20 66.18 o -18 10 1 29.78 -16.98 27.25 o -16 10 1 29.01 31.70 29.79 o -14 10 1 1245.77 982.60 38.63 o -12 10 1 19.17 49.09 23.20 o -10 10 1 133.09 198.83 33.51 o -8 10 1 2021.33 1929.13 57.99 o -6 10 1 51.44 25.76 20.51 o -4 10 1 615.81 644.34 29.74 o -2 10 1 801.88 830.57 28.93 o 0 10 1 147.44 257.21 20.73 o 2 10 1 379.28 704.93 40.10 o 4 10 1 612.34 548.52 32.18 o 6 10 1 485.54 459.67 30.75 o 8 10 1 520.24 531.71 38.73 o 10 10 1 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