#------------------------------------------------------------------------------ #$Date: 2011-09-28 17:24:46 +0300 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/23/04/2230443.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_2230443_Fobs loop_ _publ_author_name 'Ellis, Trevor K.' 'Clayton, Jr, Stephen M.' 'Powell, Douglas R.' 'Taylor, Richard W.' _publ_section_title ; 21-(4-Methylphenylsulfonyl)-4,7,13,16-tetraoxa-1,10,21-triazabicyclo[8.8.5]tricosane-19,23-dione: an N-tosylated macrobicyclic dilactam ; _journal_coeditor_code PK2323 _journal_issue 6 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o1533 _journal_volume 67 _journal_year 2011 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _cell_angle_alpha 90.000 _cell_angle_beta 112.949 _cell_angle_gamma 90.000 _cell_length_a 12.8071 _cell_length_b 20.0958 _cell_length_c 10.3305 _exptl_crystal_F_000 1096.00 _reflns_d_resolution_high 0.7833 _[local]_cod_data_source_file pk2323Isup2.hkl _[local]_cod_data_source_block I #BEGIN Tags that were not found in dictionaries: _shelx_title ' 08112a in P2(1)/c' _shelx_refln_list_code 4 _shelx_f_calc_maximum 197.56 _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+1/2' '-x, -y, -z' 'x, -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 2 0 0 0.20 0.74 5.75 o 3 0 0 24138.49 21038.33 2613.56 o 4 0 0 392.18 286.15 40.44 o 5 0 0 1.09 19.11 11.23 o 6 0 0 3073.01 2624.95 140.46 o 7 0 0 1962.47 1460.57 62.43 o 8 0 0 209.37 249.73 25.47 o 9 0 0 951.58 856.36 103.06 o 10 0 0 15.63 3.42 20.96 o 11 0 0 39.67 15.16 24.43 o 12 0 0 313.64 368.92 54.64 o 13 0 0 14.09 6.67 30.21 o 14 0 0 103.52 101.30 35.74 o 15 0 0 92.72 127.06 41.24 o 1 1 0 394.20 228.94 9.90 o 2 1 0 1522.99 971.06 60.45 o 3 1 0 1532.56 909.23 91.45 o 4 1 0 8315.04 7058.09 382.80 o 5 1 0 3.20 0.70 4.48 o 6 1 0 1166.52 924.12 25.10 o 7 1 0 9516.67 8071.99 197.03 o 8 1 0 2897.00 2400.60 70.59 o 9 1 0 2.19 -8.16 12.57 o 10 1 0 1587.52 1608.87 117.28 o 11 1 0 905.44 862.79 71.49 o 12 1 0 321.52 307.21 27.08 o 13 1 0 522.82 590.93 36.19 o 14 1 0 60.72 105.86 25.71 o 15 1 0 153.75 190.69 50.42 o 0 2 0 15216.22 17135.66 548.32 o 1 2 0 394.32 404.24 16.34 o 2 2 0 2853.04 1823.24 128.55 o 3 2 0 4910.99 2875.64 235.43 o 4 2 0 19.48 10.93 5.25 o 5 2 0 700.04 509.21 28.56 o 6 2 0 6856.95 5671.28 126.92 o 7 2 0 2632.34 2380.73 65.54 o 8 2 0 699.55 563.40 19.66 o 9 2 0 629.90 582.24 27.49 o 10 2 0 1459.40 1357.26 82.64 o 11 2 0 1961.80 2008.78 143.49 o 12 2 0 813.30 899.66 82.08 o 13 2 0 14.66 15.61 20.52 o 14 2 0 0.15 -21.34 21.34 o 15 2 0 85.21 92.16 72.94 o 1 3 0 1192.29 1210.30 48.59 o 2 3 0 7961.48 6202.83 200.54 o 3 3 0 3492.65 2884.55 132.09 o 4 3 0 3607.96 2183.30 157.36 o 5 3 0 172.60 144.37 17.09 o 6 3 0 7289.27 6245.76 145.76 o 7 3 0 2145.52 1849.71 45.99 o 8 3 0 1163.66 917.57 33.62 o 9 3 0 734.98 675.89 42.88 o 10 3 0 617.56 581.11 33.33 o 11 3 0 203.50 227.01 22.96 o 12 3 0 130.30 138.40 26.96 o 13 3 0 205.50 283.07 41.04 o 14 3 0 267.39 306.03 40.62 o 0 4 0 132.14 250.61 37.06 o 1 4 0 39030.95 42936.40 1180.18 o 2 4 0 4644.08 3876.01 133.68 o 3 4 0 4642.18 3732.35 136.28 o 4 4 0 2635.12 1770.48 86.31 o 5 4 0 1985.61 1435.27 57.54 o 6 4 0 505.23 354.69 20.11 o 7 4 0 554.26 397.46 16.79 o 8 4 0 164.17 147.46 12.06 o 9 4 0 1211.27 1136.85 93.31 o 10 4 0 2119.28 1921.97 146.40 o 11 4 0 357.65 350.09 29.45 o 12 4 0 22.43 38.25 19.93 o 13 4 0 76.68 54.50 23.20 o 14 4 0 1.56 -21.41 23.33 o 1 5 0 410.03 348.70 18.34 o 2 5 0 20941.04 19572.16 751.35 o 3 5 0 6978.07 5342.06 148.06 o 4 5 0 3293.52 2919.69 75.84 o 5 5 0 4449.37 3507.30 86.61 o 6 5 0 10.61 -1.14 6.34 o 7 5 0 469.57 385.34 17.19 o 8 5 0 922.83 750.31 34.01 o 9 5 0 1597.94 1344.60 98.54 o 10 5 0 46.14 41.15 16.29 o 11 5 0 64.63 50.60 18.91 o 12 5 0 189.60 212.23 25.34 o 13 5 0 16.96 19.16 21.98 o 14 5 0 595.36 750.91 53.68 o 0 6 0 3681.89 3891.25 133.43 o 1 6 0 1811.38 2148.75 55.58 o 2 6 0 485.52 371.98 14.02 o 3 6 0 516.19 480.61 14.36 o 4 6 0 134.63 117.14 8.49 o 5 6 0 1639.77 1362.76 34.82 o 6 6 0 7.54 3.11 6.62 o 7 6 0 510.00 409.50 18.10 o 8 6 0 59.50 49.49 11.20 o 9 6 0 295.59 248.40 25.05 o 10 6 0 1143.05 993.81 64.31 o 11 6 0 2.67 -5.92 17.31 o 12 6 0 71.80 71.16 21.59 o 13 6 0 65.92 60.18 23.72 o 14 6 0 111.89 120.53 27.72 o 1 7 0 2965.37 3609.30 89.38 o 2 7 0 2550.53 2526.47 75.80 o 3 7 0 12629.96 12255.68 266.03 o 4 7 0 2942.46 2368.02 50.29 o 5 7 0 517.91 404.61 34.90 o 6 7 0 240.24 188.38 11.71 o 7 7 0 59.70 40.05 9.06 o 8 7 0 16.45 -1.45 10.28 o 9 7 0 336.35 269.61 24.33 o 10 7 0 270.91 244.45 22.27 o 11 7 0 16.79 -1.13 17.87 o 12 7 0 47.13 52.07 22.08 o 13 7 0 171.16 135.00 26.12 o 14 7 0 149.18 152.77 29.66 o 0 8 0 4569.46 5854.26 198.85 o 1 8 0 3628.31 4799.25 117.31 o 2 8 0 1385.23 1557.09 41.88 o 3 8 0 46.85 62.36 9.38 o 4 8 0 5770.12 5073.00 142.62 o 5 8 0 584.97 458.47 15.91 o 6 8 0 1260.13 991.17 32.29 o 7 8 0 12.20 4.46 8.12 o 8 8 0 166.46 176.87 14.97 o 9 8 0 314.50 253.38 21.17 o 10 8 0 658.74 537.38 44.55 o 11 8 0 643.62 684.94 35.57 o 12 8 0 433.11 481.44 32.94 o 13 8 0 16.55 9.46 22.68 o 14 8 0 112.64 86.90 28.74 o 1 9 0 3425.51 3973.30 100.02 o 2 9 0 251.91 291.30 14.84 o 3 9 0 1428.52 1381.01 39.55 o 4 9 0 1058.73 998.24 36.74 o 5 9 0 4.85 19.11 7.71 o 6 9 0 50.50 51.38 9.57 o 7 9 0 400.50 297.37 22.15 o 8 9 0 1255.59 978.85 31.62 o 9 9 0 0.27 5.95 14.66 o 10 9 0 11.03 -8.16 16.12 o 11 9 0 1.00 0.56 18.30 o 12 9 0 12.80 14.01 21.48 o 13 9 0 303.98 311.93 32.64 o 14 9 0 37.44 55.41 29.38 o 0 10 0 707.86 763.79 40.44 o 1 10 0 201.37 187.07 15.74 o 2 10 0 1271.15 1340.35 47.95 o 3 10 0 4732.65 5014.39 121.23 o 4 10 0 2555.20 2348.05 57.58 o 5 10 0 45.17 40.24 9.13 o 6 10 0 62.12 46.45 10.04 o 7 10 0 45.48 43.43 10.67 o 8 10 0 9.11 -2.58 10.99 o 9 10 0 29.93 26.63 13.27 o 10 10 0 80.32 83.08 19.60 o 11 10 0 282.13 259.79 28.16 o 12 10 0 53.77 38.54 23.01 o 13 10 0 50.48 38.62 26.96 o 1 11 0 716.42 885.81 36.82 o 2 11 0 359.73 491.42 23.94 o 3 11 0 1539.57 1702.75 74.14 o 4 11 0 2746.58 2525.22 81.65 o 5 11 0 1.79 -1.30 8.68 o 6 11 0 0.38 16.49 9.68 o 7 11 0 43.79 36.18 11.13 o 8 11 0 92.41 88.92 14.77 o 9 11 0 45.98 26.38 13.71 o 10 11 0 1.62 -16.39 16.39 o 11 11 0 47.07 37.13 20.85 o 12 11 0 224.32 270.39 30.72 o 13 11 0 501.86 502.59 46.39 o 0 12 0 134.00 242.55 26.34 o 1 12 0 11.94 18.77 11.43 o 2 12 0 1669.97 1971.50 68.67 o 3 12 0 225.98 267.85 17.08 o 4 12 0 611.83 643.74 25.22 o 5 12 0 1666.41 1556.69 44.48 o 6 12 0 1329.83 1193.45 33.11 o 7 12 0 1443.43 1212.24 33.71 o 8 12 0 13.67 0.14 12.95 o 9 12 0 1.04 -12.86 12.86 o 10 12 0 37.36 26.81 19.49 o 11 12 0 84.20 103.88 28.82 o 12 12 0 104.11 84.84 30.95 o 13 12 0 10.29 17.23 32.73 o 1 13 0 1.05 16.57 11.59 o 2 13 0 425.58 603.94 30.78 o 3 13 0 199.13 196.61 16.82 o 4 13 0 231.98 205.28 16.92 o 5 13 0 1443.40 1403.45 41.75 o 6 13 0 1400.62 1259.58 45.53 o 7 13 0 0.19 5.97 13.07 o 8 13 0 155.99 103.38 18.61 o 9 13 0 20.36 -0.10 19.14 o 10 13 0 167.78 162.55 29.18 o 11 13 0 4.69 -24.94 24.94 o 12 13 0 256.38 244.68 38.09 o 0 14 0 1332.80 1534.94 71.41 o 1 14 0 136.55 151.36 20.33 o 2 14 0 287.15 332.99 23.26 o 3 14 0 332.85 375.63 24.48 o 4 14 0 254.51 315.39 28.70 o 5 14 0 81.87 84.27 15.37 o 6 14 0 1110.76 1117.53 47.04 o 7 14 0 899.00 778.43 42.66 o 8 14 0 53.35 42.51 17.34 o 9 14 0 16.21 4.13 17.47 o 10 14 0 1.27 -14.78 23.71 o 11 14 0 13.53 -23.84 28.72 o 12 14 0 10.58 -11.99 29.40 o 1 15 0 26.55 82.49 41.71 o 2 15 0 386.06 473.40 27.29 o 3 15 0 5.21 28.71 15.24 o 4 15 0 91.33 111.32 16.77 o 5 15 0 8.30 17.02 14.14 o 6 15 0 633.24 603.79 28.36 o 7 15 0 72.01 72.29 16.71 o 8 15 0 72.90 72.77 19.89 o 9 15 0 93.12 76.72 21.62 o 10 15 0 6.70 -24.49 24.49 o 11 15 0 3.95 -27.45 27.45 o 12 15 0 102.04 65.25 34.07 o 0 16 0 49.94 87.10 29.19 o 1 16 0 1395.88 1634.62 70.77 o 2 16 0 8.05 21.91 15.49 o 3 16 0 20.86 13.38 15.67 o 4 16 0 172.78 181.95 30.08 o 5 16 0 43.43 27.68 15.61 o 6 16 0 327.66 292.73 34.98 o 7 16 0 165.05 156.35 20.09 o 8 16 0 12.34 4.35 18.77 o 9 16 0 155.77 123.04 23.92 o 10 16 0 630.17 557.51 45.07 o 11 16 0 26.37 14.98 32.11 o 1 17 0 13.32 23.35 15.59 o 2 17 0 40.21 57.50 18.18 o 3 17 0 2549.64 2631.51 116.60 o 4 17 0 1119.67 1129.40 79.87 o 5 17 0 50.05 51.91 19.53 o 6 17 0 242.01 241.50 25.40 o 7 17 0 3.19 5.20 18.73 o 8 17 0 171.83 143.92 28.97 o 9 17 0 262.07 212.04 27.98 o 10 17 0 54.11 30.10 30.28 o 11 17 0 395.67 311.29 42.95 o 0 18 0 158.74 259.69 35.33 o 1 18 0 1338.44 1531.94 96.49 o 2 18 0 354.94 367.19 27.99 o 3 18 0 1.80 -10.09 16.07 o 4 18 0 191.40 197.22 24.66 o 5 18 0 5.86 -1.70 16.95 o 6 18 0 0.55 -10.76 18.02 o 7 18 0 380.54 346.57 28.20 o 8 18 0 18.44 22.79 25.08 o 9 18 0 0.14 -23.98 23.98 o 10 18 0 151.18 69.50 46.24 o 1 19 0 107.35 132.67 21.81 o 2 19 0 314.49 367.84 28.00 o 3 19 0 234.47 204.31 27.15 o 4 19 0 34.07 31.89 18.58 o 5 19 0 208.31 217.93 26.14 o 6 19 0 0.23 13.42 18.92 o 7 19 0 369.94 372.76 70.09 o 8 19 0 419.30 369.85 37.70 o 9 19 0 820.48 848.16 73.32 o 10 19 0 15.75 18.21 47.42 o 0 20 0 1151.66 1286.12 80.05 o 1 20 0 570.41 564.60 33.33 o 2 20 0 207.16 231.46 26.68 o 3 20 0 111.58 119.53 22.90 o 4 20 0 81.20 109.73 22.62 o 5 20 0 335.21 306.40 29.01 o 6 20 0 6.87 4.49 20.29 o 7 20 0 16.82 -3.04 26.34 o 8 20 0 67.54 48.71 29.56 o 9 20 0 456.64 449.80 43.08 o 1 21 0 129.10 157.03 24.45 o 2 21 0 958.13 1052.04 46.86 o 3 21 0 478.43 489.97 33.33 o 4 21 0 379.62 416.27 31.59 o 5 21 0 108.12 115.86 24.72 o 6 21 0 159.34 143.66 26.44 o 7 21 0 708.47 573.67 52.98 o 8 21 0 484.76 461.58 44.41 o 0 22 0 1091.27 1066.15 138.33 o 1 22 0 41.30 60.74 20.79 o 2 22 0 293.68 315.38 30.83 o 3 22 0 2.14 10.02 19.71 o 4 22 0 56.29 62.32 21.80 o 5 22 0 40.23 21.38 20.69 o 6 22 0 82.66 85.36 26.59 o 7 22 0 10.32 -28.78 28.78 o 1 23 0 724.43 757.38 40.88 o 2 23 0 353.49 375.63 31.88 o 3 23 0 225.72 230.91 29.47 o 4 23 0 626.81 627.41 40.19 o 5 23 0 512.89 517.41 37.34 o 6 23 0 183.67 144.91 31.08 o 0 24 0 2483.44 2127.77 107.40 o 1 24 0 190.94 237.53 29.83 o 2 24 0 91.52 71.01 25.92 o 3 24 0 27.88 12.47 21.95 o 4 24 0 178.48 183.29 30.03 o 5 24 0 156.03 181.06 30.02 o 1 25 0 88.20 116.05 25.94 o 2 25 0 394.74 355.45 34.79 o 3 25 0 713.04 695.83 44.07 o -15 1 1 0.92 -13.81 22.01 o -14 1 1 53.14 43.93 22.00 o -13 1 1 53.91 49.10 20.84 o -12 1 1 1.14 -7.08 16.85 o -11 1 1 46.75 39.41 17.40 o -10 1 1 95.68 110.48 18.09 o -9 1 1 1378.98 1298.31 47.15 o -8 1 1 15.51 16.63 7.39 o -7 1 1 64.36 79.75 7.28 o -6 1 1 975.04 881.60 21.65 o -5 1 1 1021.58 1060.65 24.35 o -4 1 1 2220.45 2168.68 61.72 o -3 1 1 141.65 157.03 7.03 o -2 1 1 515.10 339.70 8.99 o -1 1 1 5609.11 5295.53 100.80 o 0 1 1 8.37 -2.54 2.54 o 1 1 1 3359.28 3134.47 65.56 o 2 1 1 8421.40 6766.34 252.31 o 3 1 1 2016.82 1796.51 78.34 o 4 1 1 371.08 264.65 13.64 o 5 1 1 2045.66 1697.01 62.96 o 6 1 1 1359.44 1217.68 37.53 o 7 1 1 180.10 167.04 15.78 o 8 1 1 13.38 5.87 12.09 o 9 1 1 373.01 322.52 22.40 o 10 1 1 154.63 188.27 20.88 o 11 1 1 244.55 254.31 24.28 o 12 1 1 244.78 279.00 26.63 o 13 1 1 166.84 190.24 32.82 o 14 1 1 1.04 -23.37 23.37 o -15 2 1 49.69 40.96 24.20 o -14 2 1 0.98 -16.29 22.79 o -13 2 1 304.30 383.72 32.64 o -12 2 1 124.20 120.13 21.40 o -11 2 1 1073.54 1074.00 69.55 o -10 2 1 0.40 0.21 14.51 o -9 2 1 25.80 15.75 13.09 o -8 2 1 30.63 45.53 9.64 o -7 2 1 1656.31 1557.93 35.11 o -6 2 1 83.68 79.33 7.17 o -5 2 1 187.85 186.96 8.51 o -4 2 1 5998.98 5287.81 115.49 o -3 2 1 7669.52 6881.07 131.13 o -2 2 1 853.30 756.58 16.86 o -1 2 1 4189.94 4200.11 87.63 o 0 2 1 6177.14 6401.67 121.79 o 1 2 1 1.16 -0.21 3.36 o 2 2 1 20760.91 18510.29 545.33 o 3 2 1 1697.08 1519.00 49.32 o 4 2 1 11.99 11.70 5.56 o 5 2 1 33.63 32.97 7.07 o 6 2 1 147.46 158.81 14.15 o 7 2 1 1523.85 1382.91 43.53 o 8 2 1 1484.48 1425.43 46.08 o 9 2 1 25.17 27.06 14.27 o 10 2 1 1595.46 1506.50 100.01 o 11 2 1 175.51 192.34 23.04 o 12 2 1 152.70 155.23 44.22 o 13 2 1 38.15 28.41 22.43 o 14 2 1 0.47 -22.70 22.70 o -15 3 1 0.33 -11.44 22.16 o -14 3 1 53.85 32.16 21.00 o -13 3 1 75.13 70.28 21.08 o -12 3 1 2.00 -16.34 16.34 o -11 3 1 153.77 130.70 20.27 o -10 3 1 0.20 -13.61 13.61 o -9 3 1 64.12 41.43 10.71 o -8 3 1 1068.38 961.00 28.81 o -7 3 1 16.69 8.26 6.03 o -6 3 1 65.39 50.15 7.21 o -5 3 1 6024.31 5344.79 103.96 o -4 3 1 2174.68 2080.87 59.41 o -3 3 1 22410.30 20477.80 384.98 o -2 3 1 13872.87 13453.56 314.45 o -1 3 1 6.14 4.02 5.08 o 0 3 1 6460.94 6988.64 144.56 o 1 3 1 1752.70 1683.24 49.79 o 2 3 1 4754.74 4253.96 152.72 o 3 3 1 2283.11 1787.44 100.09 o 4 3 1 1613.31 1546.90 52.49 o 5 3 1 56.29 64.95 12.80 o 6 3 1 153.73 135.99 13.81 o 7 3 1 703.92 601.88 22.91 o 8 3 1 26.40 12.28 12.54 o 9 3 1 723.89 676.60 44.26 o 10 3 1 19.37 15.69 16.21 o 11 3 1 0.92 -4.92 17.18 o 12 3 1 301.62 366.99 29.40 o 13 3 1 38.46 59.66 23.67 o 14 3 1 1.65 -6.29 24.62 o -15 4 1 121.95 114.87 27.22 o -14 4 1 31.04 41.19 21.71 o -13 4 1 52.59 38.25 20.92 o -12 4 1 295.42 244.75 25.92 o -11 4 1 108.77 63.58 18.48 o -10 4 1 347.79 343.01 34.95 o -9 4 1 288.75 238.71 15.69 o -8 4 1 4.43 -1.48 6.67 o -7 4 1 0.48 -2.00 6.16 o -6 4 1 138.25 154.71 9.24 o -5 4 1 3559.21 3134.18 63.44 o -4 4 1 351.59 321.92 18.18 o -3 4 1 12048.37 11219.93 212.66 o -2 4 1 1011.88 1154.49 31.52 o -1 4 1 1407.99 1522.37 48.42 o 0 4 1 15668.62 16898.08 351.38 o 1 4 1 672.76 637.36 28.56 o 2 4 1 8.55 8.65 4.78 o 3 4 1 0.00 -4.58 4.58 o 4 4 1 6163.67 5288.96 160.09 o 5 4 1 311.83 289.04 12.19 o 6 4 1 480.76 398.56 19.54 o 7 4 1 48.75 42.20 9.36 o 8 4 1 18.70 6.06 12.44 o 9 4 1 265.52 222.24 20.63 o 10 4 1 90.84 89.74 18.47 o 11 4 1 534.25 549.83 48.03 o 12 4 1 3.62 17.45 20.11 o 13 4 1 175.69 184.65 27.99 o 14 4 1 184.53 229.18 32.03 o -15 5 1 25.78 22.60 25.59 o -14 5 1 86.89 66.78 24.17 o -13 5 1 81.66 67.65 26.31 o -12 5 1 281.34 301.29 25.58 o -11 5 1 454.78 420.89 27.57 o -10 5 1 382.39 338.34 23.96 o -9 5 1 19.59 0.89 9.34 o -8 5 1 16.67 25.08 7.94 o -7 5 1 449.10 346.32 14.92 o -6 5 1 517.59 412.15 14.31 o -5 5 1 3023.26 2629.79 54.55 o -4 5 1 3739.63 3349.84 67.42 o -3 5 1 8225.75 7863.19 239.16 o -2 5 1 2217.01 2595.22 72.87 o -1 5 1 3412.23 4004.97 104.56 o 0 5 1 12012.47 13556.40 330.06 o 1 5 1 6663.74 7166.37 233.55 o 2 5 1 7842.86 6864.74 293.57 o 3 5 1 2355.61 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