#------------------------------------------------------------------------------ #$Date: 2010-02-13 12:42:52 +0200 (Sat, 13 Feb 2010) $ #$Revision: 986 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/2224658.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_2224658_Fobs loop_ _publ_author_name 'Robinson, Tony V.' 'Taylor, Dennis K.' 'Tiekink, Edward R. T.' _publ_section_title ; 5-Bromospiro[1,2-dioxane-4,4'-tricyclo[4.3.1.1^3,8^]undecane]-3'-ol ; _journal_coeditor_code HB5281 _journal_issue 1 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o247 _journal_volume 66 _journal_year 2010 _space_group_IT_number 4 _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _cell_angle_alpha 90.000 _cell_angle_beta 105.426 _cell_angle_gamma 90.000 _cell_length_a 8.6199 _cell_length_b 6.6370 _cell_length_c 11.7171 _exptl_crystal_F_000 328.00 _reflns_d_resolution_high 0.7696 _[local]_cod_data_source_file hb5281Isup2.hkl _[local]_cod_data_source_block I #BEGIN Tags that were not found in dictionaries: _shelx_title ' 0485' _shelx_refln_list_code 4 _shelx_f_calc_maximum 90.61 _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+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 1 0 0 2143.32 2032.17 49.91 o 2 0 0 8209.66 7992.83 137.59 o 3 0 0 315.61 254.18 5.09 o 4 0 0 844.90 804.37 14.78 o 5 0 0 412.89 383.40 7.91 o 6 0 0 405.90 350.39 7.64 o 7 0 0 236.24 208.55 5.71 o 8 0 0 70.28 61.14 10.74 o 9 0 0 20.62 19.23 2.80 o 10 0 0 44.39 35.60 3.79 o 1 1 0 655.18 702.08 10.16 o 2 1 0 271.62 279.63 3.80 o 3 1 0 204.23 224.41 11.13 o 4 1 0 577.60 575.27 7.66 o 5 1 0 1386.35 1382.65 17.55 o 6 1 0 1003.29 950.18 12.58 o 7 1 0 361.84 357.49 5.79 o 8 1 0 669.28 624.16 9.25 o 9 1 0 272.53 255.02 5.16 o 10 1 0 142.55 138.40 4.18 o 0 2 0 4579.08 5160.17 89.02 o 1 2 0 2828.64 3204.81 45.39 o 2 2 0 1335.91 1397.74 20.19 o 3 2 0 505.63 469.80 7.32 o 4 2 0 253.48 253.39 5.85 o 5 2 0 128.45 116.80 5.00 o 6 2 0 122.47 118.87 3.09 o 7 2 0 9.08 12.82 1.52 o 8 2 0 119.18 105.56 3.61 o 9 2 0 3.55 4.41 2.16 o 10 2 0 111.76 115.52 4.71 o 1 3 0 290.71 302.34 4.30 o 2 3 0 391.16 402.59 8.82 o 3 3 0 115.91 118.72 3.22 o 4 3 0 327.05 335.82 14.60 o 5 3 0 861.53 783.41 84.91 o 6 3 0 217.82 203.03 13.97 o 7 3 0 658.42 621.90 29.58 o 8 3 0 368.35 349.00 13.94 o 9 3 0 222.08 213.75 11.25 o 10 3 0 149.92 146.53 10.39 o 0 4 0 866.73 937.64 17.21 o 1 4 0 1191.70 1208.73 27.13 o 2 4 0 950.71 978.87 20.78 o 3 4 0 1619.07 1774.20 31.32 o 4 4 0 942.37 992.93 22.87 o 5 4 0 141.61 139.69 3.64 o 6 4 0 68.69 61.73 4.68 o 7 4 0 34.74 35.52 2.45 o 8 4 0 4.57 2.87 2.22 o 9 4 0 25.34 30.37 3.00 o 1 5 0 262.05 254.76 4.18 o 2 5 0 72.78 69.92 2.15 o 3 5 0 228.06 211.72 4.79 o 4 5 0 47.62 48.12 2.26 o 5 5 0 196.32 193.49 8.13 o 6 5 0 195.85 186.25 9.21 o 7 5 0 220.75 218.73 10.31 o 8 5 0 141.50 141.85 10.52 o 0 6 0 252.73 273.69 24.95 o 1 6 0 121.54 118.35 3.53 o 2 6 0 674.18 674.90 38.94 o 3 6 0 322.13 317.19 9.48 o 4 6 0 319.32 315.88 7.65 o 5 6 0 121.96 130.14 4.07 o 6 6 0 15.74 17.22 2.43 o 7 6 0 19.97 21.19 2.71 o 1 7 0 98.24 93.12 2.88 o 2 7 0 19.80 17.55 1.81 o 3 7 0 14.72 12.63 1.78 o 4 7 0 80.90 76.64 6.96 o 5 7 0 175.96 148.06 10.94 o 6 7 0 45.21 43.72 11.78 o 0 8 0 126.22 137.32 7.97 o 1 8 0 97.81 109.63 5.04 o 2 8 0 14.92 18.29 3.07 o 3 8 0 19.15 15.94 4.48 o 4 8 0 55.29 59.55 5.94 o -6 -1 1 636.18 588.98 16.62 o -5 -1 1 819.62 735.23 19.65 o -4 -1 1 3251.58 3229.22 79.84 o -3 -1 1 1444.01 1305.59 22.88 o -2 -1 1 5393.00 5245.09 127.83 o -1 -1 1 3293.06 3260.00 79.56 o 3 -1 1 1152.74 1236.87 31.29 o 4 -1 1 642.05 617.92 16.78 o 5 -1 1 88.69 90.01 4.46 o 6 -1 1 718.65 709.72 19.97 o 9 -1 1 57.30 55.07 3.79 o 10 -1 1 197.84 189.98 6.81 o -10 0 1 134.67 127.36 5.39 o -9 0 1 117.50 117.35 7.06 o -8 0 1 345.68 347.54 11.84 o -7 0 1 17.82 30.17 3.39 o -6 0 1 14.87 26.23 3.25 o -5 0 1 360.32 327.79 6.89 o -4 0 1 1.89 3.52 0.93 o -3 0 1 2729.56 2713.31 47.21 o -2 0 1 131.51 117.96 2.51 o -1 0 1 202.72 194.16 5.10 o 0 0 1 794.52 788.65 15.23 o 1 0 1 5622.30 5778.15 276.91 o 2 0 1 2694.64 2457.46 63.98 o 3 0 1 1187.11 1131.77 20.20 o 4 0 1 595.85 533.88 10.24 o 5 0 1 1385.37 1304.96 30.37 o 6 0 1 279.37 257.26 9.45 o 7 0 1 285.92 280.52 5.69 o 8 0 1 95.72 88.34 3.99 o 9 0 1 6.78 2.78 2.35 o 10 0 1 0.59 2.32 3.07 o -10 1 1 20.07 20.69 2.39 o -9 1 1 291.84 261.34 7.86 o -8 1 1 273.38 268.82 4.95 o -7 1 1 839.29 780.08 10.75 o -6 1 1 663.23 642.05 12.57 o -5 1 1 849.66 799.60 16.26 o -4 1 1 3266.54 3430.76 59.75 o -3 1 1 1414.51 1412.01 24.92 o -2 1 1 5354.79 5780.31 69.81 o -1 1 1 2959.10 3303.78 46.69 o 0 1 1 7594.19 8429.59 303.76 o 1 1 1 1620.83 1805.37 27.42 o 2 1 1 55.18 50.32 1.83 o 3 1 1 1146.50 1239.31 15.49 o 4 1 1 633.64 645.81 8.62 o 5 1 1 92.78 90.49 2.18 o 6 1 1 713.83 678.04 9.38 o 7 1 1 11.39 27.27 3.56 o 8 1 1 215.83 203.43 4.90 o 9 1 1 82.75 82.86 3.88 o 10 1 1 184.75 174.21 6.38 o -10 2 1 91.38 91.74 3.98 o -9 2 1 117.80 108.62 3.34 o -8 2 1 115.50 104.95 3.10 o -7 2 1 76.14 76.41 3.06 o -6 2 1 90.72 92.18 3.61 o -5 2 1 139.34 138.58 2.76 o -4 2 1 421.57 413.04 5.76 o -3 2 1 520.55 489.84 17.47 o -2 2 1 1824.76 1942.17 41.15 o -1 2 1 1219.93 1250.15 15.55 o 0 2 1 872.46 945.10 25.04 o 1 2 1 3671.52 4208.62 59.49 o 2 2 1 2949.94 3305.41 46.95 o 3 2 1 1976.61 2103.30 30.27 o 4 2 1 1684.17 1701.04 51.87 o 5 2 1 604.22 572.17 16.87 o 6 2 1 1210.02 1179.82 29.70 o 7 2 1 216.19 198.34 8.62 o 8 2 1 121.24 107.43 4.43 o 9 2 1 41.76 46.69 3.82 o 10 2 1 57.78 58.06 3.58 o -10 3 1 7.89 6.40 3.96 o -9 3 1 32.57 35.61 3.08 o -8 3 1 169.31 165.21 10.26 o -7 3 1 317.86 317.25 18.69 o -6 3 1 499.49 490.16 27.75 o -5 3 1 601.91 584.28 23.38 o -4 3 1 1228.27 1264.26 33.40 o -3 3 1 1028.60 1086.39 16.09 o -2 3 1 1310.74 1401.02 28.32 o -1 3 1 251.45 228.14 7.68 o 0 3 1 793.11 850.14 19.97 o 1 3 1 111.68 117.74 2.42 o 2 3 1 164.58 180.21 3.41 o 3 3 1 135.32 136.05 5.23 o 4 3 1 258.20 275.15 5.11 o 5 3 1 358.55 356.94 6.60 o 6 3 1 333.89 309.16 7.57 o 7 3 1 431.39 410.33 14.50 o 8 3 1 133.10 131.38 6.10 o 9 3 1 147.48 136.15 6.93 o -9 4 1 98.23 101.22 4.01 o -8 4 1 38.68 38.25 2.84 o -7 4 1 35.21 40.31 2.46 o -6 4 1 120.93 128.61 3.63 o -5 4 1 62.69 54.62 3.45 o -4 4 1 225.77 219.39 7.51 o -3 4 1 379.39 392.41 19.48 o -2 4 1 707.74 728.25 18.83 o -1 4 1 582.70 598.38 15.19 o 0 4 1 393.73 409.15 5.79 o 1 4 1 951.44 985.31 27.64 o 2 4 1 354.51 355.62 13.24 o 3 4 1 628.58 629.46 10.74 o 4 4 1 464.52 449.34 9.82 o 5 4 1 748.90 702.67 23.55 o 6 4 1 247.61 236.10 5.75 o 7 4 1 39.01 39.27 2.60 o 8 4 1 111.47 118.76 4.29 o 9 4 1 4.05 6.26 2.66 o -8 5 1 91.82 100.33 7.84 o -7 5 1 120.45 123.93 10.78 o -6 5 1 446.66 436.08 17.67 o -5 5 1 358.11 362.06 13.58 o -4 5 1 783.35 725.98 18.19 o -3 5 1 929.22 916.89 21.51 o -2 5 1 735.51 748.77 10.17 o -1 5 1 242.02 227.26 3.85 o 0 5 1 401.16 437.81 6.41 o 1 5 1 24.23 27.98 1.78 o 2 5 1 260.40 248.61 7.05 o 3 5 1 2.18 4.24 2.12 o 4 5 1 53.60 56.76 3.19 o 5 5 1 74.50 64.09 3.62 o 6 5 1 108.16 98.09 5.22 o 7 5 1 95.26 92.58 5.16 o 8 5 1 90.52 89.91 3.94 o -7 6 1 18.49 18.16 3.19 o -6 6 1 4.71 6.69 2.15 o -5 6 1 16.26 15.44 2.08 o -4 6 1 8.67 8.68 1.54 o -3 6 1 81.12 82.11 2.81 o -2 6 1 147.69 155.17 4.14 o -1 6 1 371.24 378.01 6.62 o 0 6 1 147.34 157.87 3.78 o 1 6 1 78.54 84.05 2.55 o 2 6 1 230.02 227.69 4.26 o 3 6 1 331.93 315.72 16.20 o 4 6 1 68.28 71.78 2.88 o 5 6 1 398.51 405.80 16.28 o 6 6 1 82.72 84.73 4.51 o 7 6 1 52.41 54.49 4.29 o -6 7 1 17.54 21.74 2.65 o -5 7 1 66.56 63.29 3.13 o -4 7 1 130.40 123.50 7.24 o -3 7 1 218.33 211.71 4.37 o -2 7 1 79.23 73.47 2.78 o -1 7 1 46.08 48.29 2.62 o 0 7 1 30.21 37.30 3.10 o 1 7 1 3.63 5.88 1.95 o 2 7 1 67.25 66.74 2.95 o 3 7 1 26.97 30.05 4.02 o 4 7 1 36.26 34.27 2.63 o 5 7 1 5.89 1.68 2.31 o 6 7 1 111.39 106.82 5.25 o -4 8 1 17.69 19.17 5.02 o -3 8 1 35.50 44.56 5.54 o -2 8 1 55.42 67.68 4.12 o -1 8 1 51.74 57.28 3.89 o 0 8 1 36.09 45.28 3.81 o 1 8 1 125.64 124.80 5.68 o 2 8 1 58.90 61.77 3.27 o 3 8 1 31.61 33.69 2.92 o 10 -2 2 51.92 50.23 6.30 o -8 -1 2 124.32 124.09 6.54 o -7 -1 2 397.55 375.05 11.80 o -6 -1 2 692.30 669.26 18.58 o -5 -1 2 1030.86 967.58 64.00 o -4 -1 2 2601.14 2519.09 136.78 o -3 -1 2 3064.31 3016.69 231.17 o -2 -1 2 3163.91 3167.18 148.12 o -1 -1 2 1063.77 1046.05 26.45 o 0 -1 2 331.56 313.86 8.21 o 1 -1 2 265.38 244.20 4.88 o 2 -1 2 3127.33 3131.33 76.77 o 3 -1 2 1393.59 1327.40 33.60 o 4 -1 2 412.70 391.11 11.44 o 5 -1 2 83.33 72.03 4.46 o 6 -1 2 115.71 113.76 5.94 o 7 -1 2 507.88 497.74 15.71 o 8 -1 2 103.52 104.81 4.46 o 9 -1 2 75.90 74.92 9.85 o 10 -1 2 60.00 59.25 4.63 o -11 0 2 186.68 181.04 28.12 o -10 0 2 87.43 81.59 6.46 o -9 0 2 171.63 183.32 8.49 o -8 0 2 867.90 849.27 23.88 o -7 0 2 471.88 483.83 14.51 o -6 0 2 973.19 928.61 69.70 o -5 0 2 16.45 20.25 1.56 o -4 0 2 292.61 318.45 9.13 o -3 0 2 8.86 8.25 1.20 o -2 0 2 1392.85 1420.95 35.32 o -1 0 2 498.34 498.11 15.91 o 0 0 2 1842.19 1884.15 26.75 o 1 0 2 2875.48 3062.89 99.51 o 2 0 2 7485.33 8020.34 265.96 o 3 0 2 3328.46 3511.57 76.57 o 4 0 2 1446.48 1467.47 56.43 o 5 0 2 260.48 240.90 7.84 o 6 0 2 146.93 139.96 6.12 o 7 0 2 77.46 84.59 3.07 o 8 0 2 224.11 226.65 5.41 o 9 0 2 57.42 52.24 3.89 o 10 0 2 67.89 67.88 3.87 o -11 1 2 15.73 15.90 3.04 o -10 1 2 36.90 40.88 3.14 o -9 1 2 155.28 140.21 7.55 o -8 1 2 97.03 96.27 4.23 o -7 1 2 425.40 411.42 21.62 o -6 1 2 643.35 608.49 11.92 o -5 1 2 1172.99 1165.04 21.14 o -4 1 2 2292.10 2356.70 41.29 o -3 1 2 3204.74 3256.47 56.47 o -2 1 2 2715.58 2917.45 50.58 o -1 1 2 849.92 899.34 35.94 o 0 1 2 553.99 599.60 33.02 o 1 1 2 343.39 334.93 5.16 o 2 1 2 3069.38 3295.68 112.26 o 3 1 2 1352.45 1336.39 16.75 o 4 1 2 378.93 381.15 6.34 o 5 1 2 83.95 79.36 2.98 o 6 1 2 134.58 131.63 2.99 o 7 1 2 458.32 435.91 6.83 o 8 1 2 101.47 101.69 7.99 o 9 1 2 76.37 82.83 4.49 o 10 1 2 81.68 84.63 5.16 o -10 2 2 60.27 61.25 2.94 o -9 2 2 241.71 234.31 9.24 o -8 2 2 165.11 166.16 3.95 o -7 2 2 394.49 349.72 9.37 o -6 2 2 587.55 534.33 33.75 o -5 2 2 270.49 259.37 4.13 o -4 2 2 437.03 479.79 6.54 o -3 2 2 37.34 38.35 1.16 o -2 2 2 1345.76 1572.66 58.89 o -1 2 2 2204.12 2518.25 89.61 o 0 2 2 2483.60 2821.35 104.11 o 1 2 2 2319.44 2599.24 36.97 o 2 2 2 3210.13 3633.79 51.61 o 3 2 2 3333.97 3616.90 51.53 o 4 2 2 2270.07 2377.36 29.60 o 5 2 2 428.49 391.20 16.00 o 6 2 2 649.02 589.81 28.25 o 7 2 2 354.16 326.79 11.79 o 8 2 2 204.03 200.61 8.81 o 9 2 2 35.66 33.13 2.95 o 10 2 2 52.63 49.78 4.37 o -10 3 2 6.40 8.78 2.55 o -9 3 2 21.04 21.79 2.48 o -8 3 2 193.22 176.76 9.84 o -7 3 2 273.32 258.24 11.10 o -6 3 2 1405.72 1389.72 66.40 o -5 3 2 963.90 940.14 47.67 o -4 3 2 915.29 934.20 31.47 o -3 3 2 1580.69 1671.09 36.88 o -2 3 2 1101.29 1122.50 32.28 o -1 3 2 2325.32 2619.48 73.88 o 0 3 2 1014.52 1098.55 32.47 o 1 3 2 1933.42 2126.19 39.43 o 2 3 2 787.76 839.89 12.65 o 3 3 2 299.40 303.85 9.19 o 4 3 2 171.45 182.64 4.80 o 5 3 2 49.64 49.48 2.16 o 6 3 2 64.68 67.28 3.83 o 7 3 2 112.30 113.86 3.82 o 8 3 2 27.77 30.49 2.67 o 9 3 2 120.82 119.67 5.70 o -9 4 2 76.61 68.48 6.44 o -8 4 2 77.64 79.54 3.72 o -7 4 2 259.31 241.25 6.92 o -6 4 2 92.18 92.57 3.16 o -5 4 2 592.97 546.54 44.95 o -4 4 2 605.99 605.89 15.10 o -3 4 2 149.10 143.61 2.77 o -2 4 2 203.52 216.13 5.23 o -1 4 2 527.52 619.28 15.25 o 0 4 2 726.39 767.07 18.17 o 1 4 2 357.35 372.86 6.22 o 2 4 2 307.22 312.90 5.48 o 3 4 2 346.33 339.25 18.51 o 4 4 2 462.22 466.41 17.62 o 5 4 2 457.27 443.56 9.48 o 6 4 2 578.28 536.76 20.21 o 7 4 2 99.63 96.95 5.86 o 8 4 2 80.11 79.63 6.31 o 9 4 2 35.32 39.19 4.30 o -9 5 2 10.85 9.29 4.80 o -8 5 2 46.96 52.48 3.96 o -7 5 2 110.18 128.02 22.02 o -6 5 2 251.60 251.71 10.29 o -5 5 2 488.69 477.40 20.46 o -4 5 2 176.19 173.85 6.05 o -3 5 2 137.66 131.21 3.81 o -2 5 2 409.18 397.85 5.93 o -1 5 2 683.86 744.78 10.11 o 0 5 2 149.44 158.39 3.88 o 1 5 2 632.83 632.90 19.47 o 2 5 2 13.59 13.31 1.48 o 3 5 2 22.03 25.88 3.29 o 4 5 2 70.27 77.76 2.85 o 5 5 2 11.36 16.24 1.96 o 6 5 2 5.92 8.59 2.67 o 7 5 2 1.89 5.96 2.92 o 8 5 2 117.13 112.10 6.14 o -8 6 2 18.82 17.11 5.58 o -7 6 2 32.25 26.58 3.26 o -6 6 2 40.42 29.86 5.38 o -5 6 2 31.95 27.13 2.26 o -4 6 2 124.67 113.03 5.45 o -3 6 2 25.21 23.91 2.25 o -2 6 2 3.04 3.65 1.26 o -1 6 2 321.43 327.76 12.67 o 0 6 2 438.93 452.28 13.03 o 1 6 2 204.97 195.72 4.53 o 2 6 2 71.86 69.52 5.93 o 3 6 2 247.49 244.20 9.94 o 4 6 2 177.90 178.71 28.46 o 5 6 2 48.89 54.44 3.80 o 6 6 2 241.67 253.97 14.45 o 7 6 2 98.93 108.10 8.61 o -6 7 2 110.34 108.59 8.19 o -5 7 2 32.94 39.24 6.46 o -4 7 2 127.17 133.05 10.12 o -3 7 2 106.11 100.09 4.56 o -2 7 2 342.69 346.44 6.94 o -1 7 2 97.41 93.62 3.38 o 0 7 2 127.04 123.90 6.49 o 1 7 2 200.64 202.10 7.63 o 2 7 2 24.65 25.66 2.33 o 3 7 2 36.07 38.90 2.70 o 4 7 2 39.60 42.88 2.84 o 5 7 2 26.65 28.78 2.83 o -4 8 2 35.23 28.86 3.63 o -3 8 2 30.01 30.21 3.56 o -2 8 2 13.34 11.08 3.07 o -1 8 2 50.56 51.16 3.81 o 0 8 2 20.89 23.57 2.62 o 1 8 2 50.71 56.03 3.21 o 2 8 2 158.37 147.98 5.58 o 3 8 2 45.46 38.50 4.34 o 9 -3 3 7.16 3.87 3.37 o -5 -2 3 1324.32 1242.25 31.05 o -4 -2 3 555.37 532.70 13.91 o -3 -2 3 15.68 12.52 1.36 o -2 -2 3 553.53 537.40 14.03 o -1 -2 3 557.63 601.89 15.63 o 0 -2 3 156.94 174.79 5.38 o 8 -2 3 172.19 188.76 6.13 o 9 -2 3 111.73 124.11 5.49 o -9 -1 3 55.51 59.51 5.30 o -8 -1 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