#------------------------------------------------------------------------------ #$Date: 2011-02-15 17:23:33 +0200 (Tue, 15 Feb 2011) $ #$Revision: 11387 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/2228557.hkl $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2228557_Fobs loop_ _publ_author_name 'Li, Zhengyi' 'Chen, Liang' 'Tang, Qiuzheng' 'Sun, Xiaoqiang' _publ_section_title ; 3,9-Di-tert-butyl-2,4,8,10-tetraoxaspiro[5.5]undecane ; _journal_coeditor_code SI2313 _journal_issue 12 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o3368 _journal_volume 66 _journal_year 2010 _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 113.846 _cell_angle_gamma 90.000 _cell_length_a 26.7260 _cell_length_b 5.7894 _cell_length_c 11.2635 _exptl_crystal_F_000 600.00 _reflns_d_resolution_high 0.8172 _[local]_cod_data_source_file si2313Isup2.hkl _[local]_cod_data_source_block I #BEGIN Tags that were not found in dictionaries: _shelx_title ' 100927A in Cc New: C2/c' _shelx_refln_list_code 4 _shelx_f_calc_maximum 140.02 _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 7256.81 6490.39 123.46 o 6 0 0 0.14 0.65 0.11 o 8 0 0 6735.90 6802.36 129.98 o 10 0 0 259.01 264.47 5.23 o 12 0 0 133.12 131.47 4.23 o 14 0 0 0.19 1.17 0.27 o 16 0 0 328.61 323.46 6.52 o 18 0 0 427.69 428.83 8.62 o 20 0 0 261.98 292.85 6.11 o 22 0 0 6.64 7.83 0.68 o 24 0 0 4.63 3.33 0.60 o 26 0 0 1068.27 1058.70 30.61 o 28 0 0 604.61 624.83 18.67 o 1 1 0 5296.75 4696.68 110.64 o 3 1 0 9038.18 7761.93 105.62 o 5 1 0 508.40 518.18 8.48 o 7 1 0 1104.32 1157.60 15.72 o 9 1 0 280.66 257.82 4.51 o 11 1 0 12.92 25.93 0.51 o 13 1 0 14.33 12.98 0.45 o 15 1 0 0.01 -0.04 0.26 o 17 1 0 0.39 1.03 0.25 o 19 1 0 20.85 24.87 0.68 o 21 1 0 1.01 0.59 0.36 o 23 1 0 6.93 8.10 0.62 o 25 1 0 9.88 7.79 0.67 o 27 1 0 80.28 80.68 2.03 o 29 1 0 155.77 165.70 4.33 o 0 2 0 727.00 796.45 15.23 o 2 2 0 299.06 262.20 2.96 o 4 2 0 2.77 0.57 0.22 o 6 2 0 76.97 88.38 1.55 o 8 2 0 133.93 144.98 2.21 o 10 2 0 613.56 722.44 11.92 o 12 2 0 80.44 116.29 1.87 o 14 2 0 14.83 16.38 0.43 o 16 2 0 1157.97 1176.73 18.97 o 18 2 0 21.69 27.26 1.30 o 20 2 0 292.38 300.26 5.25 o 22 2 0 1.77 0.66 0.47 o 24 2 0 0.00 -0.38 0.54 o 26 2 0 20.27 20.56 1.44 o 28 2 0 0.03 0.29 0.68 o 1 3 0 237.29 275.03 3.50 o 3 3 0 110.99 97.23 3.77 o 5 3 0 638.26 680.29 8.41 o 7 3 0 809.68 798.46 11.19 o 9 3 0 546.46 535.66 7.64 o 11 3 0 271.38 275.49 4.08 o 13 3 0 3992.90 3975.99 64.69 o 15 3 0 1059.66 1108.79 18.04 o 17 3 0 116.87 118.26 2.44 o 19 3 0 159.51 152.47 3.03 o 21 3 0 144.12 135.84 3.39 o 23 3 0 6.55 7.10 0.88 o 25 3 0 50.98 53.90 1.97 o 27 3 0 5.09 5.92 0.88 o 0 4 0 3.93 2.12 0.38 o 2 4 0 6.27 7.52 0.38 o 4 4 0 25.16 24.27 0.52 o 6 4 0 8.98 13.08 0.56 o 8 4 0 0.47 -0.16 0.36 o 10 4 0 257.67 274.20 4.80 o 12 4 0 69.45 71.96 2.44 o 14 4 0 449.54 459.61 7.88 o 16 4 0 0.00 -0.47 0.47 o 18 4 0 0.91 0.37 0.47 o 20 4 0 0.16 -0.51 0.51 o 22 4 0 0.64 0.19 0.56 o 24 4 0 17.09 18.80 1.29 o 1 5 0 51.11 44.92 1.03 o 3 5 0 26.80 22.45 0.77 o 5 5 0 32.06 37.51 1.22 o 7 5 0 15.57 15.98 0.81 o 9 5 0 49.85 51.69 1.44 o 11 5 0 10.18 8.92 0.67 o 13 5 0 82.54 77.54 2.03 o 15 5 0 0.22 0.24 0.51 o 17 5 0 74.22 72.76 1.88 o 19 5 0 30.49 35.82 1.37 o 21 5 0 0.50 -0.45 0.56 o 0 6 0 3.56 2.50 0.96 o 2 6 0 12.44 9.15 0.95 o 4 6 0 68.48 72.52 1.87 o 6 6 0 271.63 282.56 6.30 o 8 6 0 8.19 6.38 1.15 o 10 6 0 13.31 11.12 1.64 o 12 6 0 52.65 54.02 1.66 o 14 6 0 34.53 43.80 1.52 o 1 7 0 0.53 0.78 0.88 o 3 7 0 129.19 128.29 3.74 o -29 1 1 214.72 226.55 4.29 o -27 1 1 79.07 78.77 1.96 o -25 1 1 12.66 11.01 0.73 o -23 1 1 72.23 78.28 1.77 o -21 1 1 12.08 11.56 0.58 o -19 1 1 4.93 3.20 0.33 o -17 1 1 60.91 62.40 1.58 o -15 1 1 46.21 54.92 1.02 o -13 1 1 288.76 237.19 3.38 o -11 1 1 52.37 56.74 0.96 o -9 1 1 2418.76 2360.27 37.72 o -7 1 1 4827.93 4514.16 168.27 o -5 1 1 10665.89 2777.67 54.32 o -3 1 1 10335.72 9020.93 261.02 o 1 1 1 1922.04 1937.98 24.46 o 3 1 1 19.50 27.22 0.43 o 5 1 1 94.80 86.01 1.22 o 7 1 1 132.51 143.17 2.03 o 9 1 1 832.02 854.96 10.55 o 11 1 1 403.51 511.83 7.08 o 13 1 1 191.95 216.92 3.73 o 15 1 1 6.57 6.01 0.35 o 17 1 1 188.39 196.19 2.97 o 19 1 1 14.08 14.90 0.62 o 21 1 1 164.73 151.09 2.95 o 23 1 1 5.17 4.72 0.59 o 25 1 1 512.11 535.19 9.06 o 27 1 1 27.62 25.60 1.54 o -28 2 1 21.99 23.11 1.36 o -26 2 1 28.51 27.24 1.42 o -24 2 1 20.42 19.61 0.92 o -22 2 1 92.63 88.19 1.96 o -20 2 1 800.00 840.62 13.65 o -18 2 1 587.80 558.95 11.09 o -16 2 1 59.27 62.67 1.07 o -14 2 1 20.82 21.96 0.48 o -12 2 1 78.99 87.96 1.46 o -10 2 1 128.53 128.07 2.33 o -8 2 1 291.36 341.06 4.85 o -6 2 1 298.01 265.29 3.58 o -4 2 1 340.63 354.33 4.33 o -2 2 1 36.62 43.45 0.72 o 0 2 1 431.04 463.09 6.32 o 2 2 1 276.89 329.81 4.58 o 4 2 1 289.32 314.15 5.05 o 6 2 1 352.77 380.71 5.32 o 8 2 1 4953.63 5217.08 72.11 o 10 2 1 42.16 33.88 0.51 o 12 2 1 415.57 430.53 5.09 o 14 2 1 8.92 8.71 0.38 o 16 2 1 80.99 90.16 2.50 o 18 2 1 316.42 329.82 5.66 o 20 2 1 8.65 5.87 0.59 o 22 2 1 55.23 47.28 1.70 o 24 2 1 0.85 0.67 0.68 o 26 2 1 1.24 0.59 0.74 o -27 3 1 11.03 8.75 1.25 o -25 3 1 24.01 25.85 1.42 o -23 3 1 0.05 0.00 0.68 o -21 3 1 1.43 1.55 0.47 o -19 3 1 698.71 686.45 11.43 o -17 3 1 579.40 543.06 9.13 o -15 3 1 47.67 54.00 1.30 o -13 3 1 768.58 760.81 12.66 o -11 3 1 235.68 237.46 3.55 o -9 3 1 477.37 492.39 7.04 o -7 3 1 57.18 67.08 1.00 o -5 3 1 17.09 4.53 0.28 o -3 3 1 51.98 57.84 0.94 o -1 3 1 0.10 0.10 0.18 o 1 3 1 2022.44 1996.71 27.20 o 3 3 1 10.21 7.43 0.44 o 5 3 1 8.58 13.77 0.40 o 7 3 1 84.74 93.51 1.28 o 9 3 1 1689.52 1773.82 28.45 o 11 3 1 15.35 20.94 3.85 o 13 3 1 588.66 569.00 11.91 o 15 3 1 1053.04 1039.61 16.93 o 17 3 1 95.64 92.97 2.07 o 19 3 1 2.81 1.72 0.47 o 21 3 1 55.23 56.72 1.97 o 23 3 1 41.68 39.99 1.70 o 25 3 1 7.61 4.71 0.88 o -24 4 1 0.73 -0.56 0.56 o -22 4 1 26.26 27.92 1.22 o -20 4 1 56.57 55.87 1.59 o -16 4 1 1222.93 1239.72 20.22 o -14 4 1 1476.82 1445.25 23.39 o -12 4 1 65.98 70.44 2.04 o -10 4 1 120.68 122.03 2.41 o -8 4 1 6.36 4.19 0.77 o -6 4 1 40.95 39.43 0.75 o -4 4 1 63.30 60.91 1.05 o -2 4 1 245.12 228.07 4.56 o 0 4 1 92.73 90.87 1.35 o 2 4 1 1.23 1.64 0.25 o 4 4 1 431.09 446.39 6.35 o 6 4 1 476.32 500.33 7.07 o 8 4 1 3.56 1.88 0.44 o 10 4 1 1233.90 1226.19 19.88 o 12 4 1 2047.98 2058.07 33.11 o 14 4 1 185.14 186.94 3.59 o 16 4 1 13.72 17.30 0.96 o 18 4 1 0.01 -0.51 0.51 o 20 4 1 42.74 45.24 1.44 o 22 4 1 0.27 0.72 0.59 o -21 5 1 1.31 1.28 0.67 o -19 5 1 35.68 38.00 1.40 o -17 5 1 123.64 120.34 2.63 o -15 5 1 11.37 9.55 0.89 o -13 5 1 24.16 22.96 1.03 o -11 5 1 44.71 40.34 1.21 o -9 5 1 0.01 -0.58 0.59 o -7 5 1 134.54 122.93 2.47 o -5 5 1 156.57 157.58 2.95 o -3 5 1 109.70 97.31 1.73 o -1 5 1 8.48 5.60 0.43 o 1 5 1 100.56 93.11 1.46 o 3 5 1 20.52 19.90 0.78 o 5 5 1 235.74 235.56 4.24 o 7 5 1 4.67 3.86 0.56 o 9 5 1 0.04 -0.14 0.47 o 11 5 1 107.86 105.52 2.33 o 13 5 1 55.56 46.73 1.40 o 15 5 1 1.26 0.36 0.59 o 17 5 1 50.87 52.87 1.59 o 19 5 1 0.07 0.43 0.62 o -16 6 1 7.14 8.50 0.81 o -14 6 1 14.75 10.64 1.01 o -12 6 1 71.85 77.49 2.44 o -10 6 1 28.02 22.61 1.73 o -8 6 1 5.16 4.93 0.88 o -6 6 1 216.36 223.90 6.26 o -4 6 1 250.93 256.22 4.75 o -2 6 1 0.10 -0.60 0.60 o 0 6 1 147.91 151.98 4.08 o 2 6 1 130.48 141.52 2.94 o 4 6 1 31.80 30.83 1.26 o 6 6 1 2.12 1.15 0.68 o 8 6 1 29.11 27.58 1.48 o 10 6 1 0.11 -0.56 0.56 o 12 6 1 8.23 5.22 0.78 o 14 6 1 13.18 17.03 1.16 o -5 7 1 31.42 29.22 2.12 o -3 7 1 215.91 215.01 5.44 o -1 7 1 250.35 262.66 6.40 o 1 7 1 32.00 30.21 1.83 o 3 7 1 47.41 47.88 2.11 o -30 0 2 276.72 268.91 8.85 o -28 0 2 26.98 26.95 1.92 o -26 0 2 29.74 31.12 1.92 o -24 0 2 128.95 126.91 2.99 o -22 0 2 2.50 4.06 0.67 o -20 0 2 50.40 53.32 1.48 o -18 0 2 47.99 41.46 1.20 o -16 0 2 4.89 3.46 0.41 o -14 0 2 444.78 402.01 7.88 o -12 0 2 702.53 642.15 18.29 o -10 0 2 2389.03 2307.70 44.31 o -8 0 2 432.15 400.96 11.36 o -6 0 2 1572.23 1466.02 41.19 o -2 0 2 5933.70 5352.32 102.06 o 0 0 2 3575.11 3452.82 53.38 o 2 0 2 4933.65 4666.37 89.21 o 4 0 2 1110.64 1287.90 24.60 o 6 0 2 395.52 378.56 7.41 o 8 0 2 2116.80 2330.88 64.87 o 10 0 2 206.07 254.46 5.09 o 12 0 2 36.31 49.11 1.34 o 14 0 2 783.23 852.12 16.58 o 16 0 2 476.83 501.59 9.99 o 18 0 2 2.58 2.26 0.46 o 20 0 2 7.55 7.63 0.68 o 22 0 2 592.56 584.58 11.74 o 24 0 2 1052.90 1085.65 31.38 o 26 0 2 43.85 40.23 2.69 o -31 1 2 19.30 20.17 1.36 o -29 1 2 47.53 49.11 1.52 o -27 1 2 4.02 3.89 0.56 o -25 1 2 33.40 28.24 1.07 o -23 1 2 3.17 3.79 0.47 o -21 1 2 696.80 674.86 9.41 o -19 1 2 147.20 150.01 2.35 o -17 1 2 2.34 0.10 0.15 o -15 1 2 282.35 274.42 3.94 o -13 1 2 1858.47 1895.13 29.27 o -11 1 2 1601.52 1511.24 96.35 o -9 1 2 4220.44 4271.58 119.73 o -7 1 2 134.83 161.94 2.35 o -5 1 2 10852.91 10104.85 292.20 o -3 1 2 1732.70 1729.24 21.23 o -1 1 2 122.55 102.03 1.49 o 1 1 2 232.57 237.07 2.97 o 3 1 2 8549.16 8207.15 156.09 o 5 1 2 5236.16 5464.03 87.01 o 7 1 2 6161.00 6506.74 79.73 o 9 1 2 1165.36 1327.93 17.99 o 11 1 2 389.02 489.68 7.99 o 13 1 2 473.70 433.33 7.30 o 15 1 2 81.37 93.40 1.58 o 17 1 2 237.12 219.25 3.33 o 19 1 2 1.39 2.10 0.37 o 21 1 2 229.21 222.46 4.10 o 23 1 2 297.63 294.56 5.25 o 25 1 2 2.92 1.28 0.62 o 27 1 2 13.45 11.93 1.73 o -30 2 2 2.55 2.02 0.68 o -28 2 2 36.97 32.99 1.48 o -26 2 2 65.07 66.35 1.70 o -24 2 2 53.29 52.93 1.48 o -22 2 2 11.43 10.43 0.70 o -20 2 2 392.24 398.29 6.73 o -18 2 2 5.06 4.00 0.46 o -16 2 2 110.01 121.61 2.14 o -14 2 2 86.10 100.87 1.35 o -12 2 2 106.37 115.17 2.95 o -10 2 2 48.54 54.71 2.47 o -8 2 2 10740.77 10719.38 148.41 o -6 2 2 5573.65 5613.49 66.53 o -4 2 2 7.50 12.51 0.35 o -2 2 2 2586.29 2665.95 44.66 o 0 2 2 3179.39 3139.40 50.24 o 2 2 2 32.84 35.61 0.95 o 4 2 2 43.68 44.98 0.80 o 6 2 2 695.96 950.14 11.68 o 8 2 2 674.65 733.25 9.03 o 10 2 2 5.50 11.86 0.72 o 12 2 2 63.94 62.36 1.07 o 14 2 2 4.48 6.72 0.89 o 16 2 2 125.68 105.12 2.14 o 18 2 2 476.41 454.44 7.62 o 20 2 2 588.99 567.47 11.55 o 22 2 2 5.98 6.65 1.06 o 24 2 2 14.98 13.13 1.09 o 26 2 2 1.58 1.05 0.74 o -27 3 2 16.50 19.28 2.31 o -25 3 2 5.95 5.20 0.82 o -23 3 2 61.41 51.29 1.83 o -21 3 2 222.18 226.78 4.18 o -19 3 2 45.20 47.62 1.37 o -17 3 2 1275.16 1289.91 18.09 o -15 3 2 19.71 19.73 0.92 o -13 3 2 293.72 269.67 5.71 o -11 3 2 2.49 4.33 0.47 o -9 3 2 0.08 0.21 0.21 o -7 3 2 111.39 141.98 1.90 o -5 3 2 242.04 279.53 3.98 o -3 3 2 147.62 181.87 2.66 o -1 3 2 27.22 24.30 0.55 o 1 3 2 387.64 384.45 4.84 o 3 3 2 490.29 456.84 6.40 o 5 3 2 623.87 715.38 11.68 o 7 3 2 13.51 17.75 0.53 o 9 3 2 2232.27 2285.72 36.55 o 11 3 2 1446.90 1506.09 30.55 o 13 3 2 32.04 35.18 1.35 o 15 3 2 59.83 64.58 1.59 o 17 3 2 95.85 91.45 2.07 o 19 3 2 2.26 3.09 0.68 o 21 3 2 125.55 117.12 3.18 o 23 3 2 73.16 76.33 2.44 o -26 4 2 1.42 -0.10 0.82 o -24 4 2 34.12 35.00 1.29 o -22 4 2 36.97 40.45 1.37 o -20 4 2 53.48 57.43 1.63 o -18 4 2 268.13 274.58 4.99 o -16 4 2 0.08 0.80 0.47 o -14 4 2 394.80 382.74 6.62 o -12 4 2 124.93 112.10 2.26 o -10 4 2 65.81 63.25 1.77 o -8 4 2 5.96 5.21 0.39 o -6 4 2 56.81 57.01 1.01 o -4 4 2 16.28 16.36 0.56 o -2 4 2 62.56 53.04 0.84 o 0 4 2 151.08 143.21 2.05 o 2 4 2 32.02 26.75 0.81 o 4 4 2 325.79 312.21 4.55 o 6 4 2 5.34 5.34 0.53 o 8 4 2 292.53 293.36 5.14 o 10 4 2 459.55 433.53 7.43 o 12 4 2 59.74 55.43 1.48 o 14 4 2 47.22 44.19 1.37 o 16 4 2 29.97 27.48 1.11 o 18 4 2 26.72 24.65 1.11 o 20 4 2 28.71 33.98 1.52 o 22 4 2 0.84 -0.05 0.74 o -21 5 2 200.73 202.16 4.03 o -19 5 2 104.72 95.91 2.26 o -17 5 2 15.12 12.75 1.01 o -15 5 2 126.63 116.03 2.52 o -13 5 2 27.95 24.21 1.30 o -11 5 2 304.07 291.02 5.21 o -9 5 2 77.58 82.64 2.46 o -7 5 2 112.80 105.42 2.71 o -5 5 2 87.59 87.57 2.36 o -3 5 2 140.78 145.01 2.38 o -1 5 2 0.71 1.23 0.28 o 1 5 2 46.28 42.93 0.92 o 3 5 2 98.53 108.48 1.99 o 5 5 2 495.48 505.12 8.57 o 7 5 2 212.22 206.01 3.85 o 9 5 2 5.66 4.97 0.62 o 11 5 2 80.94 76.16 2.52 o 13 5 2 8.06 6.30 0.67 o 15 5 2 18.12 16.62 1.07 o 17 5 2 45.25 54.00 1.70 o -16 6 2 1.83 0.42 0.74 o -14 6 2 1.35 1.31 2.02 o -12 6 2 0.01 -0.60 0.60 o -10 6 2 103.49 103.68 2.85 o -8 6 2 250.94 265.58 5.95 o -6 6 2 45.26 48.99 1.47 o -4 6 2 6.97 3.58 0.82 o -2 6 2 69.12 70.42 2.38 o 0 6 2 1.09 1.44 0.82 o 2 6 2 190.82 194.41 3.75 o 4 6 2 6.06 6.73 0.77 o 6 6 2 61.23 61.79 1.81 o 8 6 2 32.57 35.36 1.56 o 10 6 2 15.88 17.56 1.26 o 12 6 2 0.04 -0.38 0.56 o -3 7 2 1.39 1.21 1.73 o -1 7 2 82.84 84.35 2.86 o -31 1 3 7.93 6.54 0.88 o -29 1 3 3.15 4.18 0.59 o -27 1 3 82.87 85.81 1.99 o -25 1 3 212.47 205.51 5.06 o -23 1 3 5.64 6.46 0.56 o -21 1 3 0.68 0.73 0.38 o -19 1 3 91.36 89.83 1.69 o -17 1 3 142.12 127.72 5.38 o -15 1 3 100.19 77.83 1.83 o -13 1 3 32.46 57.17 3.67 o -11 1 3 2246.90 2303.11 37.55 o -9 1 3 10727.45 10330.88 203.62 o -7 1 3 385.36 384.78 6.24 o -5 1 3 1438.83 1515.69 21.04 o -3 1 3 215.64 253.50 3.60 o -1 1 3 1537.96 1526.76 24.30 o 1 1 3 1536.22 1588.47 24.38 o 3 1 3 115.51 130.68 2.18 o 5 1 3 926.53 969.33 11.92 o 7 1 3 2944.50 3513.22 48.62 o 9 1 3 452.58 508.10 8.21 o 11 1 3 38.15 34.03 0.76 o 13 1 3 3.28 1.32 0.31 o 15 1 3 39.40 49.56 1.07 o 17 1 3 851.81 813.60 11.31 o 19 1 3 260.02 276.92 4.92 o 21 1 3 151.71 149.32 3.00 o 23 1 3 86.64 84.25 2.24 o 25 1 3 10.00 9.65 1.01 o -30 2 3 27.05 31.61 1.56 o -28 2 3 1.73 1.70 0.51 o -26 2 3 0.49 0.29 0.47 o -24 2 3 500.53 496.01 8.36 o -22 2 3 1282.09 1235.93 19.83 o -20 2 3 11.21 12.03 0.84 o -18 2 3 136.24 132.53 2.51 o -16 2 3 98.81 100.01 1.62 o -14 2 3 273.65 254.69 3.80 o -12 2 3 432.04 450.80 7.59 o -10 2 3 99.55 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