#------------------------------------------------------------------------------ #$Date: 2011-09-28 17:24:46 +0300 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/10/34/2103460.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_2103460_Fobs loop_ _publ_author_name 'Schmidt, Thorsten' 'Schmitt, Heike' 'Zimmermann, Herbert' 'Haeberlen, Ulrich' 'Lalowicz, Zdzis\/law T.' 'Olejniczak, Zbigniew' 'Oeser, Thomas' _publ_section_title ; Location of the H atoms in ammonium persulphate by deuteron NMR. Verification by X-ray diffraction ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 760 _journal_page_last 769 _journal_volume 58 _journal_year 2002 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _cell_angle_alpha 90.000 _cell_angle_beta 94.966 _cell_angle_gamma 90.000 _cell_length_a 6.1340 _cell_length_b 7.9324 _cell_length_c 7.7541 _exptl_crystal_F_000 236.00 _reflns_d_resolution_high 0.7604 _[local]_cod_data_source_file sn0024Isup2.hkl _[local]_cod_data_source_block I #BEGIN Tags that were not found in dictionaries: _shelx_title ' haeb1 Prof. Haeberlen in P 21/n (Kappa CCD)' _shelx_refln_list_code 4 _shelx_F_calc_maximum 27.67 _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+1/2, -z+1/2' '-x, -y, -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 30.70 20.77 0.45 o 6 0 0 327.19 302.52 7.35 o 8 0 0 45.27 44.10 2.88 o 5 1 0 53.71 53.92 0.85 o 6 1 0 503.31 525.21 12.62 o 7 1 0 79.10 83.83 1.69 o 8 1 0 244.22 230.68 8.32 o 0 2 0 17.99 20.91 0.88 o 2 2 0 615.78 609.80 36.70 o 3 2 0 122.97 99.33 3.82 o 4 2 0 201.29 210.21 5.24 o 6 2 0 28.45 26.50 0.54 o 7 2 0 13.39 10.74 0.41 o 1 3 0 25.75 24.23 0.52 o 2 3 0 231.32 256.69 5.02 o 3 3 0 29.32 31.31 2.95 o 4 3 0 200.60 191.14 3.00 o 5 3 0 397.35 406.94 14.86 o 6 3 0 43.45 41.69 0.91 o 1 4 0 36.83 32.29 1.97 o 2 4 0 469.17 452.04 9.22 o 3 4 0 15.88 17.43 0.32 o 5 4 0 2.95 2.27 0.67 o 6 4 0 221.55 205.57 4.20 o 7 4 0 38.69 36.81 1.82 o 1 5 0 176.79 179.92 3.60 o 3 5 0 104.15 101.26 1.62 o 4 5 0 63.12 66.17 1.28 o 5 5 0 303.24 287.51 7.63 o 6 5 0 282.42 289.61 6.83 o 7 5 0 12.90 9.52 0.48 o 0 6 0 444.58 418.96 15.65 o 2 6 0 225.40 228.09 15.27 o 3 6 0 147.67 153.91 5.35 o 4 6 0 0.21 0.45 0.08 o 5 6 0 66.38 68.26 3.60 o 6 6 0 3.27 3.51 0.37 o 1 7 0 521.84 490.49 15.38 o 2 7 0 3.61 4.19 0.23 o 3 7 0 440.57 436.26 15.67 o 4 7 0 16.57 15.34 0.46 o 5 7 0 157.07 171.08 12.25 o 0 8 0 281.47 277.32 12.15 o 1 8 0 292.99 297.04 9.17 o 2 8 0 164.10 162.19 4.88 o 3 8 0 226.27 230.12 7.27 o 4 8 0 33.55 34.01 2.57 o 5 8 0 4.55 4.30 0.50 o 1 9 0 23.93 23.23 2.64 o 2 9 0 60.35 54.75 2.67 o 3 9 0 11.07 10.55 1.15 o 4 9 0 20.67 18.57 1.16 o 0 10 0 81.67 69.90 4.50 o 1 10 0 4.59 3.89 0.47 o 2 10 0 83.06 78.68 9.09 o -7 0 1 13.17 10.79 0.56 o -3 0 1 360.77 329.07 6.88 o 5 0 1 0.40 0.41 0.05 o 7 0 1 33.57 41.33 1.32 o -8 1 1 27.20 28.29 2.18 o -7 1 1 295.44 297.01 7.17 o -6 1 1 2.34 2.17 0.10 o -5 1 1 54.77 57.69 0.94 o -4 1 1 347.31 368.25 5.09 o -3 1 1 0.14 0.92 0.08 o -2 1 1 107.62 109.68 1.45 o 2 1 1 7.34 6.00 0.12 o 4 1 1 8.02 6.05 0.12 o 5 1 1 110.51 111.74 1.69 o 6 1 1 54.12 47.31 0.83 o 7 1 1 12.81 12.78 0.84 o -7 2 1 58.67 60.24 1.64 o -6 2 1 395.99 386.24 9.01 o -5 2 1 320.56 328.17 6.24 o -4 2 1 268.53 254.67 3.54 o -3 2 1 211.89 217.01 3.08 o -2 2 1 449.68 480.60 13.35 o -1 2 1 77.17 70.79 1.16 o 1 2 1 248.29 234.85 4.88 o 2 2 1 19.86 15.16 0.24 o 3 2 1 9.42 11.82 0.25 o 4 2 1 129.06 141.85 2.02 o 5 2 1 265.01 273.08 4.36 o 6 2 1 2.60 2.02 0.13 o 7 2 1 55.53 54.40 1.59 o -7 3 1 0.40 0.44 0.17 o -6 3 1 119.58 124.84 2.60 o -5 3 1 3.98 5.34 1.39 o -4 3 1 186.99 187.76 3.64 o -3 3 1 80.98 86.15 1.28 o -2 3 1 98.93 105.87 1.79 o -1 3 1 6.70 8.15 0.14 o 0 3 1 323.30 337.27 7.31 o 3 3 1 13.60 10.45 0.21 o 4 3 1 583.28 611.53 17.27 o 5 3 1 152.45 142.43 3.35 o 6 3 1 195.57 199.33 7.85 o 7 3 1 3.13 3.83 0.29 o -7 4 1 37.50 33.94 2.52 o -6 4 1 33.12 34.58 0.84 o -5 4 1 541.17 533.28 22.90 o -4 4 1 0.36 0.44 0.13 o -3 4 1 58.66 66.40 1.12 o -2 4 1 344.01 322.92 5.92 o -1 4 1 16.95 16.61 0.29 o 0 4 1 210.55 204.10 14.79 o 2 4 1 74.97 74.16 1.24 o 3 4 1 5.38 5.49 0.22 o 4 4 1 44.87 43.80 0.85 o 5 4 1 18.56 19.62 0.49 o 6 4 1 0.15 0.55 0.15 o 7 4 1 75.46 75.05 2.59 o -7 5 1 147.89 139.84 8.31 o -6 5 1 0.48 0.95 0.41 o -5 5 1 18.83 19.79 1.32 o -4 5 1 15.44 16.31 0.70 o -3 5 1 4.92 5.18 0.34 o -2 5 1 66.07 68.77 1.28 o -1 5 1 21.50 23.87 0.56 o 0 5 1 17.45 18.13 0.36 o 2 5 1 22.03 22.62 1.37 o 3 5 1 401.85 390.91 14.19 o 4 5 1 155.90 159.07 3.54 o 5 5 1 79.95 84.78 3.36 o 6 5 1 31.01 34.69 3.77 o -6 6 1 57.71 60.42 5.40 o -5 6 1 53.00 53.18 1.34 o -4 6 1 175.92 175.49 5.85 o -3 6 1 413.65 401.74 8.23 o -2 6 1 383.59 382.60 9.09 o -1 6 1 765.90 742.55 32.51 o 0 6 1 368.83 385.24 12.74 o 1 6 1 59.48 57.60 1.17 o 2 6 1 77.48 74.09 4.02 o 3 6 1 4.69 5.31 0.34 o 4 6 1 119.07 113.28 2.76 o 5 6 1 2.99 3.32 0.20 o 6 6 1 5.51 6.42 0.35 o -5 7 1 0.04 0.17 0.50 o -4 7 1 0.80 0.83 0.14 o -3 7 1 82.96 84.51 6.21 o -2 7 1 3.22 3.90 0.38 o -1 7 1 28.82 29.10 0.82 o 0 7 1 508.38 497.30 19.83 o 1 7 1 69.16 70.06 2.84 o 3 7 1 122.23 128.80 4.34 o 4 7 1 58.76 63.97 1.90 o 5 7 1 12.79 12.97 0.43 o -5 8 1 0.60 0.24 0.40 o -4 8 1 340.27 352.45 16.68 o -3 8 1 31.12 29.70 1.65 o -2 8 1 412.40 425.81 19.54 o -1 8 1 51.48 52.49 1.58 o 0 8 1 255.02 261.48 8.99 o 1 8 1 1.72 1.89 0.26 o 2 8 1 92.06 97.11 3.32 o 3 8 1 0.26 0.13 0.16 o 4 8 1 16.42 14.70 1.26 o 5 8 1 0.11 0.64 0.38 o -4 9 1 12.34 12.23 1.85 o -3 9 1 43.54 45.31 1.64 o -2 9 1 6.25 6.82 0.43 o -1 9 1 16.13 18.01 0.85 o 0 9 1 48.32 44.22 1.91 o 1 9 1 148.12 145.11 6.08 o 2 9 1 231.43 227.50 13.59 o 3 9 1 265.36 254.31 10.57 o -2 10 1 0.85 0.29 0.32 o -1 10 1 187.86 215.24 12.86 o 0 10 1 5.66 5.51 0.51 o 1 10 1 139.95 138.38 7.36 o 2 10 1 30.29 30.38 1.21 o -8 0 2 111.94 104.17 4.90 o 0 0 2 57.53 52.78 1.33 o 6 0 2 59.09 57.99 1.74 o -7 1 2 9.13 10.74 0.34 o -6 1 2 39.03 38.38 0.76 o -5 1 2 12.98 13.00 0.22 o -3 1 2 209.52 201.05 2.81 o 3 1 2 160.91 136.93 2.69 o 4 1 2 124.73 118.94 2.00 o 5 1 2 546.16 536.15 9.90 o 6 1 2 7.91 6.15 0.19 o 7 1 2 45.57 40.59 1.01 o -7 2 2 279.11 283.71 10.43 o -6 2 2 223.55 229.39 4.93 o -4 2 2 15.11 14.01 0.80 o -3 2 2 121.72 109.99 1.68 o -2 2 2 30.74 29.39 1.04 o 0 2 2 11.99 9.77 0.47 o 2 2 2 195.02 206.21 4.73 o 4 2 2 255.69 273.41 4.27 o 5 2 2 515.15 524.27 10.20 o 6 2 2 13.62 16.33 0.87 o 7 2 2 180.67 183.76 5.68 o -7 3 2 24.23 23.82 0.91 o -6 3 2 68.60 66.18 1.46 o -5 3 2 277.39 271.12 6.00 o -4 3 2 4.14 3.32 0.29 o -3 3 2 243.77 236.54 3.52 o -2 3 2 4.81 2.69 0.16 o -1 3 2 5.68 1.67 0.09 o 2 3 2 494.17 503.73 16.87 o 4 3 2 559.81 584.44 14.50 o 5 3 2 77.38 77.94 1.67 o 6 3 2 57.73 52.25 1.23 o 7 3 2 11.07 11.07 0.56 o -7 4 2 26.92 26.75 0.80 o -6 4 2 601.04 652.77 25.89 o -5 4 2 23.19 25.79 0.54 o -4 4 2 361.14 349.85 7.82 o -3 4 2 114.07 119.80 1.91 o -2 4 2 9.11 9.48 0.35 o -1 4 2 320.31 347.76 13.26 o 1 4 2 0.02 0.15 0.07 o 2 4 2 0.94 2.35 0.09 o 3 4 2 4.46 4.63 0.13 o 5 4 2 51.08 53.69 1.23 o 6 4 2 160.50 165.45 4.91 o 7 4 2 134.16 141.06 5.59 o -7 5 2 12.50 8.84 0.73 o -6 5 2 20.09 21.44 1.23 o -5 5 2 215.62 224.75 6.69 o -4 5 2 307.07 305.34 12.95 o -3 5 2 25.17 26.75 0.95 o -2 5 2 528.52 508.52 19.62 o -1 5 2 455.98 437.18 9.62 o 0 5 2 738.73 708.65 30.26 o 1 5 2 175.25 180.45 3.37 o 3 5 2 20.03 21.74 1.00 o 4 5 2 247.59 261.70 6.65 o 5 5 2 15.94 15.77 2.46 o 6 5 2 92.47 93.07 3.44 o -6 6 2 140.26 138.60 4.99 o -5 6 2 532.74 567.28 24.12 o -4 6 2 131.01 138.24 3.35 o -3 6 2 258.49 262.20 5.44 o -2 6 2 195.26 198.61 4.86 o -1 6 2 0.03 0.22 0.16 o 0 6 2 4.60 2.54 0.21 o 1 6 2 70.89 64.49 1.32 o 2 6 2 75.01 69.47 1.70 o 3 6 2 206.40 205.70 6.46 o 4 6 2 16.28 17.94 0.47 o 5 6 2 81.24 78.93 5.10 o 6 6 2 125.55 123.79 4.19 o -5 7 2 41.11 44.39 2.38 o -4 7 2 18.02 17.27 1.92 o -2 7 2 45.53 44.88 2.29 o -1 7 2 439.87 434.87 13.07 o 0 7 2 81.45 83.62 2.16 o 2 7 2 74.80 71.55 2.06 o 3 7 2 269.24 296.17 12.25 o 4 7 2 36.63 36.61 1.06 o 5 7 2 4.42 5.14 0.42 o -5 8 2 147.87 144.20 8.52 o -4 8 2 111.26 103.26 3.83 o -3 8 2 15.24 14.94 0.57 o -2 8 2 78.28 77.57 2.49 o -1 8 2 41.46 44.36 2.76 o 0 8 2 2.35 2.95 0.48 o 1 8 2 17.13 13.33 0.86 o 2 8 2 1.97 1.28 0.25 o 3 8 2 151.14 151.01 6.27 o 4 8 2 10.95 10.14 0.70 o -3 9 2 20.85 19.79 2.02 o -2 9 2 48.07 45.43 1.81 o -1 9 2 2.57 3.80 0.43 o 0 9 2 99.90 102.24 4.30 o 1 9 2 22.49 23.20 1.19 o 3 9 2 3.08 2.02 0.58 o -1 10 2 45.37 41.88 2.09 o 0 10 2 45.84 45.21 2.06 o 1 10 2 6.18 5.70 0.58 o -7 0 3 77.21 78.42 3.93 o -3 0 3 484.91 512.80 20.69 o 3 0 3 340.45 331.28 15.24 o 5 0 3 392.38 392.08 11.49 o 7 0 3 18.79 18.81 0.91 o -7 1 3 24.65 23.52 1.04 o -6 1 3 7.66 7.76 0.78 o -5 1 3 610.28 637.90 18.86 o -4 1 3 497.47 507.59 11.68 o -3 1 3 355.59 350.97 6.71 o -2 1 3 72.43 66.33 1.08 o -1 1 3 15.20 25.30 0.44 o 0 1 3 8.03 8.90 0.34 o 1 1 3 25.61 24.48 0.94 o 2 1 3 0.03 0.17 0.05 o 3 1 3 27.10 28.27 0.49 o 4 1 3 86.18 87.75 2.64 o 5 1 3 42.69 45.30 0.79 o 6 1 3 8.13 9.54 0.67 o 7 1 3 23.85 25.42 0.71 o -7 2 3 39.43 39.08 1.70 o -6 2 3 186.28 187.77 7.34 o -5 2 3 48.07 45.87 1.59 o -4 2 3 397.07 390.01 11.75 o -3 2 3 128.49 138.32 2.65 o -2 2 3 295.91 335.05 5.59 o -1 2 3 40.59 37.38 0.60 o 0 2 3 88.47 107.11 2.62 o 1 2 3 294.20 292.36 5.87 o 2 2 3 254.96 242.92 7.74 o 3 2 3 160.59 176.37 5.13 o 5 2 3 16.52 13.42 0.30 o 6 2 3 36.89 36.66 1.03 o 7 2 3 3.04 2.10 0.19 o -7 3 3 4.42 4.78 0.28 o -6 3 3 51.58 47.80 2.27 o -5 3 3 41.07 40.68 1.06 o -4 3 3 274.76 277.98 4.58 o -3 3 3 91.66 86.93 2.35 o -2 3 3 186.34 166.28 2.62 o -1 3 3 190.78 204.26 3.49 o 1 3 3 459.10 449.58 16.21 o 3 3 3 18.68 19.13 0.33 o 4 3 3 81.96 85.03 1.45 o 5 3 3 0.10 0.41 0.11 o 6 3 3 129.67 134.90 4.94 o 7 3 3 43.66 43.84 1.73 o -7 4 3 36.43 34.60 2.62 o -6 4 3 182.98 182.10 5.88 o -5 4 3 148.51 149.79 3.90 o -4 4 3 51.31 52.07 1.13 o -3 4 3 39.06 37.39 0.55 o -2 4 3 19.98 20.65 0.32 o -1 4 3 4.41 5.43 0.23 o 0 4 3 3.89 3.47 0.31 o 1 4 3 10.54 8.41 0.20 o 2 4 3 249.60 255.94 4.61 o 4 4 3 208.74 218.97 4.81 o 5 4 3 237.80 230.77 7.06 o 6 4 3 242.89 255.75 7.25 o -6 5 3 72.07 64.28 2.48 o -5 5 3 175.02 174.53 4.78 o -4 5 3 26.63 26.95 1.58 o -2 5 3 167.70 160.66 3.32 o -1 5 3 187.83 191.40 3.43 o 0 5 3 34.56 40.40 0.76 o 1 5 3 344.77 368.18 14.11 o 2 5 3 236.34 229.78 4.66 o 3 5 3 242.73 256.44 5.11 o 4 5 3 84.15 84.56 2.11 o 5 5 3 60.20 60.31 1.73 o 6 5 3 2.00 1.90 0.36 o -6 6 3 74.47 72.14 2.97 o -5 6 3 166.35 166.86 4.39 o -4 6 3 15.86 17.25 0.53 o -3 6 3 19.68 20.39 1.14 o -2 6 3 255.15 257.53 6.81 o -1 6 3 32.84 29.46 0.86 o 0 6 3 102.05 98.39 5.64 o 1 6 3 160.10 156.75 3.39 o 2 6 3 9.89 10.60 0.41 o 3 6 3 177.71 190.24 4.91 o 4 6 3 83.02 88.41 2.22 o 5 6 3 220.97 219.88 6.10 o -5 7 3 15.38 15.91 1.66 o -3 7 3 80.39 80.45 2.30 o -2 7 3 372.49 363.83 12.95 o -1 7 3 13.05 11.52 0.48 o 0 7 3 0.15 0.09 0.17 o 1 7 3 92.53 91.78 4.69 o 2 7 3 157.89 182.14 6.32 o 3 7 3 32.08 28.23 1.35 o 4 7 3 1.06 1.95 0.33 o 5 7 3 37.57 34.89 1.19 o -4 8 3 10.61 11.03 0.55 o -3 8 3 0.00 -0.03 0.28 o -2 8 3 11.20 10.87 0.42 o -1 8 3 4.36 3.78 0.26 o 0 8 3 36.68 33.57 1.26 o 1 8 3 7.56 6.51 0.44 o 2 8 3 346.35 359.25 21.02 o 3 8 3 18.65 18.73 0.93 o 4 8 3 143.78 132.22 6.39 o -3 9 3 209.09 202.74 12.58 o -2 9 3 65.20 67.43 2.87 o -1 9 3 115.02 116.33 5.16 o 0 9 3 25.51 25.72 1.33 o 1 9 3 262.75 290.53 20.53 o 2 9 3 51.17 54.49 2.17 o 3 9 3 89.11 80.95 3.70 o -6 0 4 0.37 0.80 0.15 o -4 0 4 148.86 158.87 3.50 o 0 0 4 176.63 152.01 3.93 o 2 0 4 40.42 32.88 1.02 o 6 0 4 138.39 130.38 4.32 o -7 1 4 51.25 52.14 1.68 o -6 1 4 263.00 266.75 7.45 o -4 1 4 617.40 648.70 24.12 o -3 1 4 395.44 382.58 7.50 o -2 1 4 8.03 4.52 0.09 o -1 1 4 0.02 0.35 0.07 o 0 1 4 22.53 17.13 0.36 o 1 1 4 464.58 441.68 32.00 o 2 1 4 51.79 48.55 0.88 o 3 1 4 1.02 1.00 0.10 o 4 1 4 78.10 81.10 2.77 o 5 1 4 198.39 197.35 3.31 o 6 1 4 88.95 96.43 2.24 o 7 1 4 235.15 235.97 7.80 o -7 2 4 0.77 0.62 0.25 o -6 2 4 15.65 16.07 0.58 o -5 2 4 29.02 27.28 0.58 o -4 2 4 8.39 9.31 0.19 o -3 2 4 283.12 296.69 5.46 o -2 2 4 6.30 5.89 0.15 o 0 2 4 4.14 3.01 0.12 o 2 2 4 31.10 31.20 0.56 o 4 2 4 52.51 52.83 1.06 o 5 2 4 612.14 642.70 24.07 o 6 2 4 0.53 0.88 0.16 o -7 3 4 116.27 115.80 5.71 o -6 3 4 147.94 150.60 4.27 o -5 3 4 405.27 417.76 12.18 o -4 3 4 374.56 389.21 10.04 o -2 3 4 185.40 186.93 3.67 o -1 3 4 603.58 583.38 26.21 o 1 3 4 56.87 62.61 2.81 o 2 3 4 41.41 35.82 0.71 o 3 3 4 176.70 179.12 2.75 o 4 3 4 190.53 193.93 5.46 o 5 3 4 384.07 424.52 17.44 o 6 3 4 13.86 14.38 0.40 o -6 4 4 0.07 0.52 0.38 o -5 4 4 56.17 56.88 1.74 o -4 4 4 6.33 6.29 0.32 o -3 4 4 189.23 186.97 3.69 o -1 4 4 64.06 59.08 2.77 o 1 4 4 214.26 206.31 3.74 o 3 4 4 343.58 354.77 8.44 o 5 4 4 42.36 45.80 1.28 o 6 4 4 34.05 30.50 1.83 o -6 5 4 231.73 234.68 12.78 o -5 5 4 30.55 29.86 1.08 o -3 5 4 13.68 14.02 0.89 o -2 5 4 381.10 384.47 10.37 o -1 5 4 40.15 43.39 1.92 o 0 5 4 10.43 6.81 0.19 o 1 5 4 13.50 13.89 0.45 o 2 5 4 62.20 68.70 3.14 o 3 5 4 85.25 81.53 1.82 o 4 5 4 135.76 144.54 3.57 o 5 5 4 53.26 50.76 1.89 o -6 6 4 75.60 65.38 3.01 o -5 6 4 12.70 13.73 0.57 o -4 6 4 101.49 105.77 3.76 o -3 6 4 342.16 353.35 9.32 o -2 6 4 233.53 226.96 6.92 o -1 6 4 351.11 351.48 9.49 o 0 6 4 15.56 14.13 1.54 o 1 6 4 31.86 34.57 1.35 o 2 6 4 253.88 263.21 6.86 o 3 6 4 262.83 282.67 9.77 o 4 6 4 132.64 131.68 3.64 o -5 7 4 237.15 227.58 11.55 o 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