#------------------------------------------------------------------------------ #$Date: 2012-02-24 10:01:01 +0200 (Fri, 24 Feb 2012) $ #$Revision: 34320 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/4/02/58/4025898.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_4025898 loop_ _publ_author_name 'Myron M. Johnson' 'Jeremy M. Naidoo' 'Manuel A. Fernandes' 'Edwin M. Mmutlane' 'Willem A. L. van Otterlo' 'Charles B. de Koning' _publ_section_title ; CAN-Mediated Oxidations for the Synthesis of Xanthones and Related Products ; _journal_name_full 'Journal of Organic Chemistry' _journal_page_first 8701 _journal_page_last 8704 _journal_volume 75 _journal_year 2010 _chemical_formula_moiety 'C15 H11 Cl O5' _chemical_formula_sum 'C15 H11 Cl O5' _chemical_formula_weight 306.69 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 94.569(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 5.2102(3) _cell_length_b 30.1686(16) _cell_length_c 8.4028(5) _cell_measurement_reflns_used 840 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 19.82 _cell_measurement_theta_min 2.52 _cell_volume 1316.59(13) _shelx_F_squared_multiplier 1.000 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 19807.11 18990.93 508.22 o 2 0 0 4895.15 4843.79 121.67 o 3 0 0 60.51 59.27 10.99 o 4 0 0 2.34 0.04 10.33 o 5 0 0 41.37 47.99 17.02 o 6 0 0 0.57 99.94 49.97 o 1 1 0 4587.22 4525.80 88.90 o 2 1 0 634.52 613.51 19.19 o 3 1 0 189.21 210.67 12.00 o 4 1 0 184.23 191.64 13.06 o 5 1 0 296.15 266.02 22.86 o 6 1 0 122.10 92.41 52.62 o 0 2 0 3.00 -2.20 2.26 o 1 2 0 222.71 243.48 9.92 o 2 2 0 1442.88 1459.27 33.48 o 3 2 0 105.63 65.55 11.85 o 4 2 0 111.52 96.58 11.03 o 5 2 0 197.55 206.06 22.72 o 6 2 0 0.49 -5.35 29.21 o 1 3 0 4642.62 4593.85 90.38 o 2 3 0 13.74 10.29 6.78 o 3 3 0 32.24 35.05 7.85 o 4 3 0 535.49 566.60 23.89 o 5 3 0 263.52 240.31 22.15 o 6 3 0 3.06 58.71 41.85 o 0 4 0 209.33 199.05 9.32 o 1 4 0 895.82 921.99 20.78 o 2 4 0 1317.93 1323.71 33.60 o 3 4 0 375.48 393.01 20.79 o 4 4 0 130.65 119.53 13.13 o 5 4 0 421.83 401.00 27.18 o 6 4 0 2.21 -29.75 29.75 o 1 5 0 65.57 53.51 5.93 o 2 5 0 501.78 536.98 19.14 o 3 5 0 1051.29 1146.38 33.94 o 4 5 0 287.12 241.33 15.74 o 5 5 0 1.61 4.22 14.88 o 6 5 0 2.27 -2.43 25.25 o 0 6 0 282.56 286.84 15.50 o 1 6 0 7.77 6.38 5.49 o 2 6 0 1778.83 1816.18 43.59 o 3 6 0 0.60 -0.02 7.45 o 4 6 0 10.92 12.88 9.02 o 5 6 0 269.86 342.53 47.93 o 6 6 0 44.11 19.00 26.34 o 1 7 0 1360.96 1286.67 30.51 o 2 7 0 2907.62 2908.47 64.37 o 3 7 0 251.44 244.54 16.06 o 4 7 0 3.77 2.27 9.54 o 5 7 0 0.14 17.09 17.70 o 6 7 0 35.17 37.93 39.97 o 0 8 0 370.46 308.41 18.35 o 1 8 0 391.90 411.88 14.51 o 2 8 0 10.96 13.50 7.58 o 3 8 0 456.61 523.03 29.96 o 4 8 0 0.04 7.73 10.53 o 5 8 0 0.16 3.86 16.64 o 6 8 0 19.60 15.04 43.10 o 1 9 0 1.10 -5.89 5.89 o 2 9 0 545.06 580.03 22.78 o 3 9 0 8.53 4.81 14.85 o 4 9 0 308.13 320.67 27.19 o 5 9 0 56.50 75.96 24.43 o 0 10 0 596.00 510.81 38.25 o 1 10 0 35.85 36.65 7.47 o 2 10 0 181.86 183.74 13.93 o 3 10 0 247.51 253.01 17.79 o 4 10 0 368.28 377.35 30.04 o 5 10 0 64.23 90.46 34.26 o 1 11 0 0.46 0.41 6.77 o 2 11 0 212.69 182.89 11.12 o 3 11 0 100.61 113.12 13.61 o 4 11 0 1171.69 1302.16 61.23 o 5 11 0 479.89 413.89 37.85 o 0 12 0 1721.16 1574.33 55.57 o 1 12 0 1.82 0.24 6.75 o 2 12 0 636.75 686.91 22.83 o 3 12 0 54.15 64.37 16.24 o 4 12 0 960.85 982.25 48.86 o 5 12 0 311.62 306.35 34.14 o 1 13 0 107.98 107.96 10.11 o 2 13 0 1027.80 1045.01 29.77 o 3 13 0 73.18 50.60 12.99 o 4 13 0 153.84 168.08 24.05 o 5 13 0 76.43 94.93 24.50 o 0 14 0 7542.70 7522.97 214.16 o 1 14 0 4570.43 4485.02 87.87 o 2 14 0 58.05 65.60 15.85 o 3 14 0 835.30 816.76 33.42 o 4 14 0 265.91 301.08 29.56 o 5 14 0 145.68 132.73 37.32 o 1 15 0 1656.69 1670.81 40.91 o 2 15 0 1.11 -6.54 6.54 o 3 15 0 68.41 72.35 14.04 o 4 15 0 444.60 453.86 35.17 o 5 15 0 10.67 -11.13 28.74 o 0 16 0 1.56 7.06 9.03 o 1 16 0 42.30 36.68 12.32 o 2 16 0 1.48 -0.52 7.40 o 3 16 0 430.41 482.15 32.07 o 4 16 0 876.94 821.20 46.21 o 5 16 0 287.18 163.89 63.55 o 1 17 0 1391.90 1455.26 37.23 o 2 17 0 15.44 21.39 13.69 o 3 17 0 21.26 34.02 16.39 o 4 17 0 31.77 19.95 18.13 o 5 17 0 11.11 24.13 33.67 o 0 18 0 318.50 246.29 24.22 o 1 18 0 75.78 64.24 10.38 o 2 18 0 507.44 530.93 22.49 o 3 18 0 71.28 110.86 20.99 o 4 18 0 26.54 13.13 18.44 o 5 18 0 2.98 36.78 31.70 o 1 19 0 517.14 537.27 24.25 o 2 19 0 559.33 630.30 30.30 o 3 19 0 44.70 37.65 18.73 o 4 19 0 12.11 -17.05 17.05 o 5 19 0 62.00 36.82 39.97 o 0 20 0 76.28 78.56 17.26 o 1 20 0 538.82 508.45 22.44 o 2 20 0 70.81 67.29 14.86 o 3 20 0 1072.36 1148.91 68.70 o 4 20 0 92.50 88.11 34.00 o 5 20 0 0.27 21.35 41.38 o 1 21 0 2217.07 2322.25 62.69 o 2 21 0 1167.35 1162.22 43.42 o 3 21 0 185.67 226.66 27.79 o 4 21 0 0.44 -10.39 22.32 o 5 21 0 43.19 82.50 40.19 o 0 22 0 560.45 499.28 59.75 o 1 22 0 14.47 25.89 10.65 o 2 22 0 1647.20 1632.60 54.20 o 3 22 0 120.99 113.29 23.00 o 4 22 0 118.89 123.29 30.30 o 1 23 0 430.64 393.33 21.37 o 2 23 0 249.08 263.91 23.36 o 3 23 0 424.77 448.41 52.60 o 4 23 0 19.47 -0.13 22.56 o 0 24 0 985.09 970.89 83.17 o 1 24 0 83.60 67.20 12.37 o 2 24 0 40.18 35.08 15.48 o 3 24 0 30.22 33.38 19.39 o 4 24 0 16.94 7.82 23.05 o 1 25 0 824.18 833.48 29.96 o 2 25 0 20.42 55.34 28.29 o 3 25 0 3.99 8.63 19.08 o 4 25 0 246.44 297.13 61.57 o 0 26 0 225.52 243.09 29.84 o 1 26 0 1.24 19.89 12.67 o 2 26 0 41.93 11.40 23.44 o 3 26 0 153.07 127.53 29.57 o 4 26 0 20.26 20.78 27.27 o 1 27 0 989.06 971.52 39.68 o 2 27 0 24.59 48.18 18.32 o 3 27 0 26.29 34.81 26.47 o 4 27 0 0.63 15.84 30.20 o 0 28 0 5.29 11.93 15.73 o 1 28 0 26.66 10.74 13.74 o 2 28 0 46.12 39.79 18.08 o 3 28 0 125.51 120.42 31.99 o 1 29 0 21.31 45.21 14.98 o 2 29 0 58.57 60.33 19.79 o 3 29 0 2.70 -1.90 21.38 o 0 30 0 5.90 7.30 17.49 o 1 30 0 5.43 31.16 15.34 o 2 30 0 10.87 23.49 17.80 o 3 30 0 24.19 61.61 26.66 o 1 31 0 410.96 445.30 36.68 o 2 31 0 25.38 12.11 18.40 o 3 31 0 92.36 71.07 40.38 o 0 32 0 20.11 36.67 19.62 o 1 32 0 38.55 27.25 16.50 o 2 32 0 11.36 24.33 24.10 o 1 33 0 270.13 311.56 30.30 o 2 33 0 288.16 256.96 50.68 o 0 34 0 1278.39 1418.00 78.10 o 1 34 0 383.24 378.93 35.82 o 1 35 0 72.52 101.56 24.80 o -6 1 1 20.00 22.97 33.19 o -5 1 1 10.23 6.92 24.49 o -4 1 1 46.48 36.65 10.24 o -3 1 1 789.66 804.30 22.58 o -2 1 1 3340.81 3452.22 73.32 o -1 1 1 104.43 101.38 5.50 o 0 1 1 4552.55 4549.00 81.50 o 1 1 1 835.20 777.20 18.81 o 2 1 1 845.36 901.15 28.72 o 3 1 1 1125.89 1171.01 66.44 o 4 1 1 116.25 97.11 10.61 o 5 1 1 1.75 3.85 10.62 o 6 1 1 0.02 -33.42 38.72 o -6 2 1 124.63 150.01 42.13 o -5 2 1 364.98 360.43 52.00 o -4 2 1 257.47 280.98 17.36 o -3 2 1 6.35 4.18 6.77 o -2 2 1 1032.29 992.97 27.29 o -1 2 1 65.86 64.81 5.07 o 0 2 1 122.41 144.55 5.53 o 1 2 1 6093.94 5811.94 113.42 o 2 2 1 4869.12 4627.98 105.44 o 3 2 1 851.71 861.76 34.35 o 4 2 1 244.19 259.51 16.94 o 5 2 1 726.48 674.93 28.07 o 6 2 1 42.72 104.93 53.09 o -6 3 1 295.99 345.01 58.29 o -5 3 1 7.38 13.22 17.66 o -4 3 1 1190.88 1242.15 35.99 o -3 3 1 2234.75 2338.97 51.50 o -2 3 1 123.51 131.74 10.86 o -1 3 1 207.51 220.73 9.24 o 0 3 1 1973.10 1925.65 34.38 o 1 3 1 38.98 11.69 4.74 o 2 3 1 641.35 662.88 24.28 o 3 3 1 755.45 758.52 25.13 o 4 3 1 73.66 81.03 13.04 o 5 3 1 366.43 316.52 31.63 o 6 3 1 117.14 72.91 38.63 o -6 4 1 129.75 134.79 44.38 o -5 4 1 222.56 217.52 27.29 o -4 4 1 3.46 17.24 8.74 o -3 4 1 139.79 164.75 11.39 o -2 4 1 2536.48 2473.28 46.59 o -1 4 1 13.65 14.87 5.17 o 0 4 1 318.71 309.08 9.83 o 1 4 1 1404.54 1535.31 29.81 o 2 4 1 0.81 18.60 8.07 o 3 4 1 594.07 590.65 23.99 o 4 4 1 88.77 66.09 12.12 o 5 4 1 1363.32 1499.75 46.66 o 6 4 1 4.58 18.25 31.98 o -6 5 1 206.80 191.55 109.15 o -5 5 1 16.40 2.05 17.24 o -4 5 1 292.90 297.32 25.51 o -3 5 1 904.00 886.99 25.41 o -2 5 1 109.15 122.26 7.25 o -1 5 1 867.41 855.38 23.16 o 0 5 1 1700.29 1685.92 36.67 o 1 5 1 19364.62 19143.33 313.76 o 2 5 1 10.05 15.75 7.18 o 3 5 1 1290.53 1295.99 37.71 o 4 5 1 517.04 523.90 27.47 o 5 5 1 209.35 177.22 18.55 o 6 5 1 49.27 6.58 34.19 o -6 6 1 12.02 -3.59 27.16 o -5 6 1 6.09 -4.93 16.38 o -4 6 1 0.81 11.47 11.98 o -3 6 1 276.84 292.19 14.14 o -2 6 1 398.84 374.72 15.33 o -1 6 1 326.57 341.05 14.29 o 0 6 1 3250.20 3169.30 64.87 o 1 6 1 15873.87 15657.72 276.23 o 2 6 1 443.52 502.05 17.65 o 3 6 1 719.60 757.43 27.66 o 4 6 1 17.82 10.47 10.32 o 5 6 1 84.99 78.59 19.34 o 6 6 1 70.29 7.72 33.23 o -6 7 1 77.46 74.84 30.69 o -5 7 1 111.40 66.85 21.03 o -4 7 1 937.29 976.70 39.97 o -3 7 1 86.63 89.28 8.00 o -2 7 1 2315.87 2373.17 51.62 o -1 7 1 2994.03 2902.09 56.75 o 0 7 1 447.06 430.50 15.13 o 1 7 1 8137.19 8071.42 158.20 o 2 7 1 1422.07 1501.47 35.49 o 3 7 1 654.22 617.86 25.04 o 4 7 1 142.18 118.17 18.65 o 5 7 1 32.84 23.88 14.94 o -6 8 1 8.50 38.45 29.69 o -5 8 1 89.61 49.58 20.17 o -4 8 1 246.63 283.96 23.92 o -3 8 1 195.04 217.65 12.02 o -2 8 1 568.31 537.79 21.11 o -1 8 1 1715.67 1646.18 35.73 o 0 8 1 8269.34 7825.63 141.31 o 1 8 1 3897.19 3629.18 76.20 o 2 8 1 213.65 214.10 13.56 o 3 8 1 566.89 625.68 25.64 o 4 8 1 2.06 11.55 10.70 o 5 8 1 29.99 13.79 14.14 o -5 9 1 214.23 224.98 29.26 o -4 9 1 10.33 29.30 16.17 o -3 9 1 135.05 111.38 13.41 o -2 9 1 155.89 157.95 10.68 o -1 9 1 111.56 118.93 8.92 o 0 9 1 2801.49 2536.88 57.58 o 1 9 1 3090.66 3018.44 65.37 o 2 9 1 1485.31 1632.86 38.25 o 3 9 1 19.52 8.45 9.21 o 4 9 1 118.88 127.58 16.43 o 5 9 1 200.18 166.55 24.15 o -5 10 1 4.04 -17.22 17.22 o -4 10 1 12.93 0.48 13.13 o -3 10 1 186.46 200.10 14.68 o -2 10 1 807.22 749.77 26.21 o -1 10 1 873.82 854.48 23.12 o 0 10 1 34.89 27.42 12.74 o 1 10 1 225.19 217.35 16.12 o 2 10 1 54.34 36.13 7.79 o 3 10 1 26.00 34.97 10.09 o 4 10 1 2.23 -11.38 11.38 o 5 10 1 9.73 3.85 16.70 o -5 11 1 39.20 49.07 27.23 o -4 11 1 41.88 46.27 16.45 o -3 11 1 0.11 -0.05 8.22 o -2 11 1 6.48 19.84 7.45 o -1 11 1 237.86 203.77 16.64 o 0 11 1 240.66 216.86 11.86 o 1 11 1 9.98 10.07 6.70 o 2 11 1 383.30 391.24 19.31 o 3 11 1 91.49 89.81 13.15 o 4 11 1 105.60 105.51 15.30 o 5 11 1 283.75 284.66 29.26 o -5 12 1 152.44 170.20 28.63 o -4 12 1 39.61 15.93 15.78 o -3 12 1 203.97 180.02 20.67 o -2 12 1 114.09 135.81 12.57 o -1 12 1 109.45 123.24 10.59 o 0 12 1 871.65 909.22 26.78 o 1 12 1 0.15 -0.32 8.89 o 2 12 1 451.91 424.32 17.87 o 3 12 1 9.57 11.85 10.16 o 4 12 1 85.81 57.84 16.50 o 5 12 1 122.99 200.62 56.34 o -5 13 1 159.41 126.53 26.42 o -4 13 1 75.86 66.97 18.46 o -3 13 1 76.45 58.33 15.77 o -2 13 1 12.20 21.70 8.60 o -1 13 1 1051.18 988.78 27.45 o 0 13 1 73.65 121.95 12.63 o 1 13 1 1383.86 1452.69 41.69 o 2 13 1 20.88 13.18 10.15 o 3 13 1 13.59 18.03 10.36 o 4 13 1 678.58 751.82 38.54 o 5 13 1 324.88 314.75 40.92 o -5 14 1 13.50 10.87 21.01 o -4 14 1 262.03 262.38 27.29 o -3 14 1 1332.07 1375.58 72.39 o -2 14 1 1917.46 1961.77 54.72 o -1 14 1 1159.23 1233.47 32.24 o 0 14 1 983.00 1012.97 27.87 o 1 14 1 894.86 860.63 35.68 o 2 14 1 264.49 293.30 16.01 o 3 14 1 106.83 101.71 14.44 o 4 14 1 21.43 15.56 17.20 o 5 14 1 31.18 31.78 25.40 o -5 15 1 0.06 -8.13 19.57 o -4 15 1 61.66 30.69 21.41 o -3 15 1 8.56 4.48 12.92 o -2 15 1 92.54 102.78 17.09 o -1 15 1 1137.29 1129.82 28.33 o 0 15 1 2760.18 2588.75 56.17 o 1 15 1 363.42 382.33 18.40 o 2 15 1 241.31 268.26 16.65 o 3 15 1 78.88 94.62 15.42 o 4 15 1 0.27 34.16 20.83 o 5 15 1 0.54 17.34 23.69 o -5 16 1 13.51 -21.36 21.36 o -4 16 1 600.58 632.30 40.43 o -3 16 1 438.55 425.51 50.58 o -2 16 1 226.53 237.68 17.70 o -1 16 1 4659.25 4396.26 82.65 o 0 16 1 320.52 318.81 16.28 o 1 16 1 2502.01 2517.88 60.03 o 2 16 1 917.21 950.29 31.21 o 3 16 1 65.57 55.46 20.57 o 4 16 1 10.43 -18.16 18.16 o 5 16 1 0.03 -10.94 27.01 o -5 17 1 2.09 6.84 21.44 o -4 17 1 1900.27 1863.07 71.97 o -3 17 1 1478.21 1584.95 61.10 o -2 17 1 110.03 128.44 14.59 o -1 17 1 17.94 17.05 7.46 o 0 17 1 985.27 919.98 27.98 o 1 17 1 132.83 131.27 15.22 o 2 17 1 205.44 216.99 16.09 o 3 17 1 1624.91 1667.93 54.60 o 4 17 1 161.24 215.75 34.58 o 5 17 1 2.52 24.59 25.53 o -5 18 1 409.71 441.92 44.02 o -4 18 1 141.15 131.12 29.30 o -3 18 1 260.43 255.16 36.83 o -2 18 1 23.24 11.01 10.63 o -1 18 1 28.27 23.46 8.34 o 0 18 1 321.13 336.33 17.58 o 1 18 1 231.91 272.00 17.58 o 2 18 1 705.08 666.57 30.54 o 3 18 1 249.61 259.10 26.28 o 4 18 1 353.41 270.32 37.40 o 5 18 1 59.26 60.04 30.31 o -5 19 1 22.37 16.89 28.06 o -4 19 1 23.59 17.67 19.55 o -3 19 1 14.53 22.85 17.45 o -2 19 1 106.23 109.30 21.74 o -1 19 1 386.28 402.31 18.23 o 0 19 1 585.90 550.70 25.27 o 1 19 1 3.96 19.97 9.87 o 2 19 1 324.88 352.33 21.87 o 3 19 1 349.53 376.50 26.38 o 4 19 1 854.25 972.77 64.29 o 5 19 1 7.56 10.49 27.26 o -5 20 1 138.23 159.89 38.11 o -4 20 1 0.32 -18.54 18.54 o -3 20 1 1078.31 1160.59 57.18 o -2 20 1 1.25 -10.06 10.06 o -1 20 1 391.22 404.25 18.68 o 0 20 1 30.28 29.68 9.65 o 1 20 1 18.49 16.09 10.13 o 2 20 1 137.97 153.40 15.76 o 3 20 1 25.78 18.29 16.87 o 4 20 1 168.34 222.42 36.59 o 5 20 1 51.03 55.32 30.47 o -5 21 1 2.59 20.71 29.31 o -4 21 1 7.39 -15.83 15.83 o -3 21 1 93.89 77.73 19.36 o -2 21 1 0.12 -10.66 10.66 o -1 21 1 318.44 345.82 18.21 o 0 21 1 515.84 561.53 24.29 o 1 21 1 543.26 540.79 25.54 o 2 21 1 1.47 -9.60 11.70 o 3 21 1 3.92 -7.84 17.92 o 4 21 1 8.02 -10.18 23.41 o -4 22 1 28.01 22.63 19.46 o -3 22 1 910.72 984.69 46.59 o -2 22 1 841.41 835.82 40.46 o -1 22 1 6.55 14.09 10.18 o 0 22 1 8.76 2.71 9.79 o 1 22 1 157.67 157.75 16.39 o 2 22 1 492.89 538.60 38.59 o 3 22 1 13.02 0.97 20.27 o 4 22 1 56.90 42.60 28.06 o -4 23 1 8.48 -12.67 18.66 o -3 23 1 1.77 -9.54 15.66 o -2 23 1 163.70 194.45 22.97 o -1 23 1 360.22 356.82 25.17 o 0 23 1 473.44 434.21 23.00 o 1 23 1 791.43 829.02 32.67 o 2 23 1 285.37 315.43 27.79 o 3 23 1 24.91 73.51 25.09 o 4 23 1 48.90 93.08 30.56 o -4 24 1 1.31 -6.77 18.76 o -3 24 1 381.73 439.71 33.95 o -2 24 1 36.29 27.56 15.41 o -1 24 1 2.15 14.08 10.07 o 0 24 1 317.25 311.93 20.86 o 1 24 1 0.75 -4.71 10.85 o 2 24 1 598.10 601.97 33.78 o 3 24 1 6.07 12.12 22.53 o 4 24 1 30.47 -2.76 26.22 o -4 25 1 13.37 24.30 24.58 o -3 25 1 0.60 -16.33 16.33 o -2 25 1 183.78 221.95 29.96 o -1 25 1 1028.06 925.29 41.03 o 0 25 1 683.55 694.56 44.09 o 1 25 1 120.57 81.41 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