#------------------------------------------------------------------------------ #$Date: 2011-09-28 17:24:46 +0300 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/22/23/2222335.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_2222335_Fobs loop_ _publ_author_name 'Neelakantan, Sundar' 'Parkin, Sean' 'Crooks, Peter A.' _publ_section_title ; (11R)-13-Dimethylammonio-11,13-dihydro-4,5-epoxycostunolide semifumarate ; _journal_coeditor_code HG2516 _journal_issue 7 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o1569 _journal_volume 65 _journal_year 2009 _space_group_IT_number 19 _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_length_a 6.3164 _cell_length_b 15.1650 _cell_length_c 22.0028 _exptl_crystal_F_000 880.00 _reflns_d_resolution_high 0.8313 _[local]_cod_data_source_file hg2516Isup2.hkl _[local]_cod_data_source_block I #BEGIN Tags that were not found in dictionaries: _shelx_title ' x04054_0m in P2(1)2(1)2(1)' _shelx_refln_list_code 4 _shelx_f_calc_maximum 145.26 _shelx_f_squared_multiplier 1.000 #END Tags that were not found in dictionaries loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -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 6330.16 6624.06 241.27 o 4 0 0 1317.92 1250.51 27.31 o 6 0 0 7.83 4.43 2.75 o 1 1 0 1867.27 1701.04 48.11 o 2 1 0 2447.27 2736.80 69.94 o 3 1 0 1493.92 1470.87 38.46 o 4 1 0 568.39 491.22 8.46 o 5 1 0 156.45 155.90 3.94 o 6 1 0 466.45 412.89 11.76 o 7 1 0 70.93 63.70 3.92 o 0 2 0 14792.01 11994.57 741.04 o 1 2 0 3768.28 3433.85 89.48 o 2 2 0 2114.86 2328.46 60.34 o 3 2 0 270.84 286.24 8.03 o 4 2 0 3775.36 3877.82 67.25 o 5 2 0 17.76 15.06 1.30 o 6 2 0 308.69 317.59 7.57 o 7 2 0 42.87 44.16 6.31 o 1 3 0 795.51 766.62 20.05 o 2 3 0 49.05 53.31 2.03 o 3 3 0 278.02 319.31 9.72 o 4 3 0 947.51 949.03 16.73 o 5 3 0 40.98 47.14 1.75 o 6 3 0 172.17 158.73 5.23 o 7 3 0 265.99 274.64 11.31 o 0 4 0 14687.49 14373.96 645.01 o 1 4 0 5420.32 5347.74 140.13 o 2 4 0 1091.58 1083.76 28.39 o 3 4 0 1685.90 1836.47 48.00 o 4 4 0 737.39 729.31 14.64 o 5 4 0 63.91 61.52 2.32 o 6 4 0 41.32 38.43 2.22 o 7 4 0 15.43 13.36 2.50 o 1 5 0 106.32 106.96 3.06 o 2 5 0 3097.31 3183.39 90.77 o 3 5 0 489.52 490.43 14.28 o 4 5 0 1842.00 1797.23 37.06 o 5 5 0 373.77 340.57 8.37 o 6 5 0 36.46 37.32 2.43 o 7 5 0 17.83 22.58 2.56 o 0 6 0 2262.97 2165.68 80.14 o 1 6 0 3877.34 4033.59 115.15 o 2 6 0 28.88 29.00 1.75 o 3 6 0 263.64 272.04 7.39 o 4 6 0 1683.22 1585.56 32.87 o 5 6 0 1.66 3.06 1.48 o 6 6 0 3.60 1.19 1.66 o 7 6 0 18.93 14.32 2.39 o 1 7 0 0.22 2.86 1.00 o 2 7 0 217.88 235.66 8.20 o 3 7 0 470.29 476.76 11.33 o 4 7 0 913.74 914.60 18.37 o 5 7 0 0.01 -0.30 1.53 o 6 7 0 199.34 214.04 7.25 o 7 7 0 0.30 -1.34 4.16 o 0 8 0 945.44 986.39 44.90 o 1 8 0 24.66 24.06 1.66 o 2 8 0 1585.16 1509.89 43.73 o 3 8 0 712.78 657.29 15.40 o 4 8 0 793.99 745.05 17.45 o 5 8 0 580.91 608.45 15.64 o 6 8 0 542.22 577.98 16.00 o 1 9 0 15.35 28.36 3.19 o 2 9 0 650.46 656.34 19.61 o 3 9 0 260.20 237.55 6.66 o 4 9 0 13.89 13.11 1.52 o 5 9 0 0.16 0.77 1.61 o 6 9 0 205.43 201.71 6.14 o 0 10 0 1014.38 1040.58 39.23 o 1 10 0 17.40 15.95 2.07 o 2 10 0 3.85 3.46 1.75 o 3 10 0 0.24 1.36 1.67 o 4 10 0 324.01 343.14 12.15 o 5 10 0 654.28 656.09 18.78 o 6 10 0 354.97 342.34 9.68 o 1 11 0 188.29 198.44 7.81 o 2 11 0 105.42 101.83 5.00 o 3 11 0 1263.50 1238.54 33.67 o 4 11 0 147.60 143.43 6.02 o 5 11 0 28.72 28.77 2.58 o 6 11 0 20.08 23.92 2.57 o 0 12 0 885.54 759.39 47.09 o 1 12 0 65.94 63.69 6.16 o 2 12 0 299.13 285.83 12.46 o 3 12 0 57.73 59.31 6.48 o 4 12 0 24.99 28.77 2.52 o 5 12 0 39.07 39.45 3.17 o 1 13 0 1204.30 1260.63 49.15 o 2 13 0 272.73 314.23 23.06 o 3 13 0 74.90 85.60 9.27 o 4 13 0 390.86 371.38 13.00 o 5 13 0 68.10 71.34 3.80 o 0 14 0 218.54 235.93 18.20 o 1 14 0 0.67 4.26 3.52 o 2 14 0 30.28 27.30 5.71 o 3 14 0 210.62 199.84 16.07 o 4 14 0 367.13 332.91 11.73 o 1 15 0 2.61 3.04 4.54 o 2 15 0 62.02 75.34 7.94 o 3 15 0 14.76 15.13 4.69 o 4 15 0 10.50 9.38 5.36 o 0 16 0 265.27 268.62 19.83 o 1 16 0 654.35 667.40 45.65 o 2 16 0 71.60 73.41 7.42 o 3 16 0 16.00 19.76 5.19 o 1 17 0 1.32 5.84 4.86 o 2 17 0 122.30 122.80 10.55 o 1 0 1 14659.32 13848.06 355.32 o 2 0 1 1972.61 2008.25 51.59 o 3 0 1 624.64 620.50 18.05 o 4 0 1 344.87 364.95 6.10 o 5 0 1 267.89 240.03 5.04 o 6 0 1 225.16 240.16 7.74 o 7 0 1 0.95 -1.04 1.80 o -7 1 1 176.90 169.32 7.51 o -6 1 1 1241.25 1255.39 34.04 o -5 1 1 41.48 41.32 1.66 o -4 1 1 3587.41 3495.73 61.14 o -3 1 1 202.12 201.16 5.87 o -2 1 1 10523.33 10609.56 253.21 o -1 1 1 6800.43 6290.55 162.69 o 0 1 1 804.96 739.83 15.87 o 1 1 1 6784.61 6241.71 177.25 o 2 1 1 10525.30 10577.58 299.57 o 3 1 1 199.99 200.85 6.38 o 4 1 1 3584.06 3544.82 58.96 o 5 1 1 40.73 37.94 1.84 o 6 1 1 1242.74 1254.30 34.05 o 7 1 1 175.97 166.94 7.45 o -7 2 1 92.01 92.11 5.43 o -6 2 1 141.43 135.20 3.88 o -5 2 1 23.68 26.87 1.48 o -4 2 1 457.94 460.63 8.25 o -3 2 1 1254.26 1488.89 38.98 o -2 2 1 3006.60 3289.85 83.66 o -1 2 1 4714.27 4650.99 111.43 o 0 2 1 606.42 570.84 13.80 o 1 2 1 4716.90 4551.75 119.76 o 2 2 1 3004.80 3196.27 83.78 o 3 2 1 1257.55 1493.82 39.00 o 4 2 1 456.19 448.08 8.25 o 5 2 1 23.47 28.10 1.92 o 6 2 1 144.96 136.23 3.87 o 7 2 1 94.15 92.75 4.74 o -7 3 1 290.71 258.39 15.44 o -6 3 1 47.20 49.42 2.53 o -5 3 1 140.00 127.66 3.31 o -4 3 1 307.49 315.31 6.33 o -3 3 1 14.25 12.41 1.51 o -2 3 1 1149.28 1215.98 31.38 o -1 3 1 3077.47 2820.42 68.07 o 0 3 1 656.81 658.98 16.09 o 1 3 1 3092.46 2812.48 80.10 o 2 3 1 1138.52 1183.52 34.37 o 3 3 1 16.17 12.68 1.55 o 4 3 1 310.19 320.28 6.30 o 5 3 1 136.45 124.89 3.23 o 6 3 1 47.74 50.35 2.53 o 7 3 1 287.75 279.47 10.92 o -7 4 1 204.11 220.90 8.86 o -6 4 1 181.08 187.84 5.79 o -5 4 1 230.79 231.59 6.23 o -4 4 1 373.15 356.03 7.40 o -3 4 1 133.84 128.46 4.18 o -2 4 1 1784.39 1831.98 47.69 o -1 4 1 141.73 137.69 3.39 o 0 4 1 8547.33 8243.62 186.34 o 1 4 1 138.94 134.43 3.95 o 2 4 1 1791.03 1819.84 47.68 o 3 4 1 133.66 130.32 4.20 o 4 4 1 369.36 346.96 7.72 o 5 4 1 233.77 233.57 6.56 o 6 4 1 180.17 178.79 5.94 o 7 4 1 199.24 194.16 8.78 o -7 5 1 17.99 14.25 2.70 o -6 5 1 294.73 314.13 9.01 o -5 5 1 1054.66 1014.07 29.75 o -4 5 1 140.73 146.11 3.67 o -3 5 1 115.22 118.72 4.39 o -2 5 1 921.43 1002.78 28.82 o -1 5 1 132.96 135.39 3.81 o 0 5 1 1405.72 1437.54 37.41 o 1 5 1 132.75 125.14 3.51 o 2 5 1 917.42 988.37 32.04 o 3 5 1 113.93 120.49 3.65 o 4 5 1 137.01 137.29 3.62 o 5 5 1 1053.24 1035.69 35.78 o 6 5 1 297.40 306.86 8.37 o 7 5 1 17.14 18.80 2.62 o -7 6 1 369.90 355.53 13.91 o -6 6 1 56.00 59.91 3.26 o -5 6 1 937.12 991.00 29.91 o -4 6 1 63.93 63.02 2.11 o -3 6 1 325.45 308.02 12.17 o -2 6 1 289.47 327.33 9.94 o -1 6 1 992.11 1060.03 27.59 o 0 6 1 279.35 302.67 7.59 o 1 6 1 999.37 1059.92 32.04 o 2 6 1 290.55 331.50 11.08 o 3 6 1 323.52 312.31 14.15 o 4 6 1 63.76 62.87 2.09 o 5 6 1 937.87 930.63 32.74 o 6 6 1 55.83 60.13 2.53 o 7 6 1 369.22 341.31 13.86 o -7 7 1 451.56 436.50 17.59 o -6 7 1 69.62 72.46 3.26 o -5 7 1 1448.08 1470.26 41.72 o -4 7 1 393.66 393.99 8.18 o -3 7 1 140.71 144.12 3.94 o -2 7 1 1257.64 1315.38 38.74 o -1 7 1 188.79 193.10 5.51 o 0 7 1 852.77 943.79 27.37 o 1 7 1 187.64 192.14 7.74 o 2 7 1 1252.72 1370.08 42.71 o 3 7 1 139.05 135.63 4.27 o 4 7 1 391.73 385.12 8.19 o 5 7 1 1446.17 1495.75 42.17 o 6 7 1 69.68 66.88 2.72 o 7 7 1 451.52 461.26 17.60 o -6 8 1 55.25 59.64 2.43 o -5 8 1 74.97 73.38 2.68 o -4 8 1 400.96 379.61 8.49 o -3 8 1 36.82 41.73 2.00 o -2 8 1 177.10 206.67 6.89 o -1 8 1 35.45 45.79 2.87 o 0 8 1 48.85 52.05 2.45 o 1 8 1 36.14 47.78 3.85 o 2 8 1 177.91 213.76 6.90 o 3 8 1 36.65 39.84 1.91 o 4 8 1 399.46 381.72 8.06 o 5 8 1 73.58 65.99 3.80 o 6 8 1 54.02 60.04 2.97 o -6 9 1 92.57 95.91 5.18 o -5 9 1 365.12 381.52 10.13 o -4 9 1 329.56 333.26 7.81 o -3 9 1 276.16 271.55 7.44 o -2 9 1 129.49 133.69 5.02 o -1 9 1 1744.99 1797.56 48.11 o 0 9 1 81.35 82.82 3.05 o 1 9 1 1744.14 1835.90 58.69 o 2 9 1 131.32 142.36 5.08 o 3 9 1 276.45 272.23 7.45 o 4 9 1 320.08 315.31 8.51 o 5 9 1 370.77 386.99 10.15 o 6 9 1 96.42 102.01 3.56 o -6 10 1 58.54 58.06 3.39 o -5 10 1 43.27 41.44 2.60 o -4 10 1 69.70 73.76 3.85 o -3 10 1 82.35 81.71 3.18 o -2 10 1 381.90 381.39 11.88 o -1 10 1 513.02 484.74 16.77 o 0 10 1 79.93 88.88 3.38 o 1 10 1 508.02 492.86 16.79 o 2 10 1 382.87 391.93 13.50 o 3 10 1 84.75 80.46 3.12 o 4 10 1 69.58 77.32 3.97 o 5 10 1 42.20 38.96 2.14 o 6 10 1 60.19 64.31 2.53 o -6 11 1 82.65 75.49 4.11 o -5 11 1 11.50 12.89 2.35 o -4 11 1 407.34 415.94 14.34 o -3 11 1 268.15 250.56 10.65 o -2 11 1 146.51 146.00 6.35 o -1 11 1 35.13 33.22 2.94 o 0 11 1 43.38 50.58 3.35 o 1 11 1 34.74 37.72 3.02 o 2 11 1 145.35 142.84 6.36 o 3 11 1 268.84 255.02 7.84 o 4 11 1 408.48 403.04 14.36 o 5 11 1 11.50 16.52 2.34 o 6 11 1 84.08 81.74 4.23 o -5 12 1 82.48 83.79 5.06 o -4 12 1 96.31 98.50 4.57 o -3 12 1 309.08 281.41 20.91 o -2 12 1 94.27 93.53 5.78 o -1 12 1 343.61 323.81 12.10 o 0 12 1 4.13 7.36 2.58 o 1 12 1 344.86 331.22 12.77 o 2 12 1 95.68 86.66 4.81 o 3 12 1 308.89 292.97 10.54 o 4 12 1 94.25 98.25 4.46 o 5 12 1 79.06 82.45 7.71 o -5 13 1 41.59 35.71 3.24 o -4 13 1 192.22 195.90 7.41 o -3 13 1 158.27 135.99 12.61 o -2 13 1 181.70 193.91 15.11 o -1 13 1 340.68 339.58 20.83 o 0 13 1 1073.99 1115.90 53.06 o 1 13 1 341.77 349.74 22.57 o 2 13 1 180.42 175.50 15.59 o 3 13 1 159.74 148.42 12.30 o 4 13 1 194.28 194.20 7.46 o 5 13 1 41.36 38.33 3.07 o -4 14 1 30.39 31.02 2.70 o -3 14 1 510.62 566.30 37.71 o -2 14 1 178.67 190.72 15.57 o -1 14 1 370.86 420.47 20.89 o 0 14 1 0.37 6.05 3.82 o 1 14 1 372.80 411.42 22.15 o 2 14 1 181.66 199.72 15.59 o 3 14 1 509.47 525.91 37.52 o 4 14 1 30.22 30.18 2.71 o -4 15 1 7.29 1.77 4.48 o -3 15 1 274.20 281.70 20.95 o -2 15 1 53.01 56.48 6.92 o -1 15 1 625.65 630.73 30.96 o 0 15 1 608.15 698.21 33.77 o 1 15 1 623.54 645.46 31.04 o 2 15 1 52.63 52.83 7.50 o 3 15 1 273.35 289.63 20.95 o -3 16 1 185.65 184.50 14.22 o -2 16 1 100.80 107.91 9.69 o -1 16 1 67.58 71.09 7.88 o 0 16 1 22.64 29.39 4.19 o 1 16 1 67.11 88.41 8.15 o 2 16 1 104.04 104.97 9.82 o 3 16 1 186.62 183.29 14.55 o -2 17 1 331.03 342.90 23.34 o -1 17 1 19.28 27.65 5.61 o 0 17 1 172.87 201.69 10.90 o 1 17 1 20.14 23.70 4.75 o 2 17 1 331.55 317.50 23.42 o -1 18 1 55.86 50.96 6.09 o 0 0 2 14695.48 15181.29 680.73 o 1 0 2 1828.35 1782.45 46.27 o 2 0 2 11264.54 12161.41 342.74 o 3 0 2 1484.43 1572.91 40.97 o 4 0 2 0.21 6.08 1.64 o 5 0 2 8.15 3.05 1.20 o 6 0 2 8.13 9.46 2.46 o 7 0 2 0.20 1.46 2.21 o -7 1 2 269.22 233.21 10.10 o -6 1 2 23.30 25.67 2.93 o -5 1 2 223.91 235.17 7.20 o -4 1 2 268.33 278.38 4.99 o -3 1 2 276.56 270.49 7.08 o -2 1 2 361.91 347.69 8.63 o -1 1 2 7468.89 7530.83 191.70 o 0 1 2 427.42 364.39 8.87 o 1 1 2 7441.83 7264.89 208.81 o 2 1 2 365.21 350.47 10.23 o 3 1 2 281.62 282.69 8.43 o 4 1 2 266.74 278.43 5.18 o 5 1 2 221.78 230.01 7.32 o 6 1 2 24.42 22.30 1.97 o 7 1 2 265.25 251.96 11.76 o -7 2 2 277.24 239.48 10.44 o -6 2 2 121.63 130.00 4.07 o -5 2 2 529.99 530.06 10.72 o -4 2 2 637.49 621.79 11.74 o -3 2 2 9.16 11.28 1.28 o -2 2 2 8336.07 8747.50 224.39 o -1 2 2 4021.24 3879.46 93.39 o 0 2 2 373.37 340.63 7.93 o 1 2 2 4045.12 3868.84 109.36 o 2 2 2 8346.82 8548.41 244.63 o 3 2 2 9.74 11.44 1.27 o 4 2 2 643.84 640.31 11.30 o 5 2 2 528.44 506.98 10.43 o 6 2 2 120.97 124.86 5.17 o 7 2 2 281.89 266.99 12.37 o -7 3 2 63.44 75.00 4.06 o -6 3 2 1249.15 1246.87 34.66 o -5 3 2 823.90 766.56 14.95 o -4 3 2 1346.02 1298.96 22.07 o -3 3 2 566.08 537.64 16.02 o -2 3 2 722.09 772.60 18.75 o -1 3 2 796.05 766.52 18.14 o 0 3 2 8.28 28.29 1.57 o 1 3 2 787.23 733.11 19.59 o 2 3 2 726.02 768.69 22.45 o 3 3 2 571.44 550.20 16.06 o 4 3 2 1343.54 1308.00 22.83 o 5 3 2 821.34 777.54 26.80 o 6 3 2 1248.79 1322.57 39.83 o 7 3 2 63.31 69.90 4.00 o -7 4 2 64.18 63.87 5.84 o -6 4 2 222.01 252.87 7.32 o -5 4 2 45.05 48.48 2.52 o -4 4 2 334.24 320.09 6.84 o -3 4 2 428.78 468.11 13.88 o -2 4 2 4436.97 4418.63 123.39 o -1 4 2 4365.72 4127.69 119.06 o 0 4 2 203.38 173.87 4.48 o 1 4 2 4373.07 4178.29 108.01 o 2 4 2 4429.74 4348.76 113.50 o 3 4 2 430.16 467.86 17.63 o 4 4 2 327.33 319.61 7.06 o 5 4 2 43.95 48.45 2.38 o 6 4 2 217.38 229.55 7.29 o 7 4 2 63.82 69.88 5.45 o -7 5 2 39.19 37.01 2.72 o -6 5 2 65.22 62.21 2.97 o -5 5 2 134.75 139.67 4.37 o -4 5 2 427.20 404.60 9.13 o -3 5 2 491.21 486.42 12.62 o -2 5 2 1815.59 1989.69 57.08 o -1 5 2 1132.60 1114.17 31.09 o 0 5 2 2608.66 2589.60 74.63 o 1 5 2 1127.43 1059.02 35.55 o 2 5 2 1813.15 1986.07 63.42 o 3 5 2 495.19 502.93 15.11 o 4 5 2 427.31 404.66 9.55 o 5 5 2 131.35 137.52 4.22 o 6 5 2 63.84 60.92 2.55 o 7 5 2 38.73 49.06 3.11 o -7 6 2 298.63 298.08 12.15 o -6 6 2 430.43 465.60 12.29 o -5 6 2 278.71 287.50 8.41 o -4 6 2 1685.17 1609.57 35.77 o -3 6 2 550.44 552.25 13.04 o -2 6 2 635.53 678.98 19.73 o -1 6 2 1308.34 1417.35 37.64 o 0 6 2 1441.24 1381.53 36.20 o 1 6 2 1315.80 1467.20 45.82 o 2 6 2 625.35 669.40 21.93 o 3 6 2 553.60 568.11 18.14 o 4 6 2 1680.84 1571.31 35.53 o 5 6 2 282.72 286.05 10.17 o 6 6 2 429.90 483.50 13.29 o 7 6 2 297.50 305.94 12.16 o -6 7 2 199.47 214.25 6.07 o -5 7 2 9.21 7.52 1.78 o -4 7 2 46.31 46.21 2.00 o -3 7 2 0.23 0.88 1.08 o -2 7 2 1292.00 1308.04 36.08 o -1 7 2 1214.81 1187.27 31.31 o 0 7 2 1568.00 1648.75 39.64 o 1 7 2 1212.28 1199.20 38.04 o 2 7 2 1286.05 1358.92 42.36 o 3 7 2 0.33 1.09 1.03 o 4 7 2 47.66 48.32 2.05 o 5 7 2 9.06 10.53 1.71 o 6 7 2 203.05 211.92 6.50 o -6 8 2 94.96 103.80 3.84 o -5 8 2 918.88 920.04 26.42 o -4 8 2 78.54 77.54 2.77 o -3 8 2 639.41 606.87 15.46 o -2 8 2 2089.77 2114.15 54.91 o -1 8 2 154.00 154.93 4.78 o 0 8 2 3280.49 3436.37 98.26 o 1 8 2 154.29 159.56 12.87 o 2 8 2 2079.21 2041.51 59.93 o 3 8 2 639.92 609.91 14.42 o 4 8 2 77.21 74.91 2.62 o 5 8 2 923.52 939.46 29.55 o 6 8 2 96.46 111.07 3.92 o -6 9 2 78.71 71.58 4.28 o -5 9 2 59.74 63.45 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