#------------------------------------------------------------------------------ #$Date: 2012-09-11 12:26:43 +0300 (Tue, 11 Sep 2012) $ #$Revision: 66590 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/10/51/2105181.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_2105181_Fobs loop_ _publ_author_name 'Siegler, Maxime A.' 'Parkin, Sean' 'Brock, Carolyn Pratt' _publ_section_title ; [Ni(MeCN)(H~2~O)~2~(NO~3~)~2~]·(15-crown-5)·MeCN: detailed study of a four-phase sequence that includes an intermediate modulated phase ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 389 _journal_page_last 400 _journal_volume 68 _journal_year 2012 _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 105.460 _cell_angle_gamma 90.000 _cell_length_a 12.1660 _cell_length_b 12.1970 _cell_length_c 16.1040 _exptl_crystal_F_000 1096.00 _reflns_d_resolution_high 0.7699 _[local]_cod_data_source_file hw5021160K_III_1sup11.hkl _[local]_cod_data_source_block 160K_III_1 #BEGIN Tags that were not found in dictionaries: _shelx_title ' k06090 in P2(1)/c' _shelx_refln_list_code 4 _shelx_f_calc_maximum 293.90 _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 1 0 0 5854.11 5442.22 83.67 o 2 0 0 24656.64 23867.92 374.70 o 3 0 0 663.98 753.03 14.55 o 4 0 0 1345.71 1276.88 25.46 o 5 0 0 44100.36 46266.16 720.29 o 6 0 0 1313.87 1244.14 29.10 o 7 0 0 10043.75 10546.12 203.72 o 8 0 0 6752.48 6955.57 156.43 o 9 0 0 574.28 647.54 21.83 o 10 0 0 389.13 396.53 18.19 o 11 0 0 1080.16 1084.08 54.57 o 12 0 0 2078.59 2422.81 127.32 o 13 0 0 1235.23 1313.26 101.86 o 14 0 0 42.77 18.19 54.57 o 15 0 0 242.65 174.62 80.03 o 1 1 0 45240.18 40947.90 1027.69 o 2 1 0 1008.19 1053.16 15.43 o 3 1 0 10014.47 9272.90 110.52 o 4 1 0 17124.03 16939.94 182.64 o 5 1 0 1819.56 1916.30 34.56 o 6 1 0 13782.15 13886.05 158.18 o 7 1 0 2381.99 2331.86 36.01 o 8 1 0 120.21 101.66 12.86 o 9 1 0 770.65 764.02 28.30 o 10 1 0 385.82 401.58 29.50 o 11 1 0 3655.09 3839.44 102.51 o 12 1 0 1313.71 1374.95 69.12 o 13 1 0 289.11 264.95 46.09 o 14 1 0 208.74 204.01 44.52 o 15 1 0 8.32 -25.08 48.67 o 0 2 0 11452.58 10770.31 192.81 o 1 2 0 1030.08 961.08 18.19 o 2 2 0 2855.66 2959.64 38.59 o 3 2 0 9141.63 8359.83 102.51 o 4 2 0 819.61 846.08 16.57 o 5 2 0 18669.50 18785.87 208.36 o 6 2 0 91.14 94.58 8.73 o 7 2 0 5374.24 5536.19 79.54 o 8 2 0 3918.46 4063.56 73.28 o 9 2 0 1445.82 1470.32 44.52 o 10 2 0 3196.99 3407.52 81.24 o 11 2 0 10.11 0.00 30.92 o 12 2 0 1018.47 1014.57 55.26 o 13 2 0 413.96 405.88 70.94 o 14 2 0 47.76 7.90 54.57 o 15 2 0 557.89 506.54 125.51 o 1 3 0 4820.26 4963.97 62.98 o 2 3 0 5317.63 5089.35 62.67 o 3 3 0 9222.83 9031.95 107.95 o 4 3 0 18172.25 18603.63 201.92 o 5 3 0 1497.10 1485.56 22.73 o 6 3 0 1067.21 948.97 20.10 o 7 3 0 732.34 760.27 20.10 o 8 3 0 1436.33 1533.51 36.70 o 9 3 0 4022.02 4321.18 89.92 o 10 3 0 733.92 652.16 34.66 o 11 3 0 2454.95 2556.90 88.49 o 12 3 0 26.83 90.14 34.09 o 13 3 0 6.00 -0.61 69.12 o 14 3 0 365.97 348.88 59.89 o 0 4 0 44964.77 44921.97 911.28 o 1 4 0 2206.75 2094.14 41.84 o 2 4 0 13265.45 13300.14 156.34 o 3 4 0 8357.94 8324.64 105.47 o 4 4 0 1070.02 1132.19 25.46 o 5 4 0 10168.17 10729.87 137.60 o 6 4 0 714.16 703.18 18.19 o 7 4 0 4039.18 4278.05 69.85 o 8 4 0 3380.03 3440.56 94.58 o 9 4 0 145.47 120.12 21.83 o 10 4 0 2718.95 2985.40 87.31 o 11 4 0 80.47 41.12 28.83 o 12 4 0 129.68 54.57 36.01 o 13 4 0 62.30 61.53 44.96 o 14 4 0 27.94 -55.89 55.89 o 1 5 0 12377.14 12275.63 165.52 o 2 5 0 10065.22 10834.69 126.05 o 3 5 0 9107.05 9390.31 109.81 o 4 5 0 6525.92 6718.65 84.77 o 5 5 0 11.25 9.09 7.72 o 6 5 0 4370.73 4488.26 73.01 o 7 5 0 2.55 9.35 6.76 o 8 5 0 70.17 64.35 21.83 o 9 5 0 1591.16 1580.01 41.17 o 10 5 0 338.32 232.96 81.85 o 11 5 0 1282.50 1406.48 90.95 o 12 5 0 1.28 32.22 35.74 o 13 5 0 47.26 24.80 41.92 o 14 5 0 633.20 503.70 110.95 o 0 6 0 16665.01 17568.90 270.05 o 1 6 0 5.29 -1.46 6.05 o 2 6 0 9453.80 10021.83 138.97 o 3 6 0 130.51 99.13 11.36 o 4 6 0 444.47 476.91 16.37 o 5 6 0 5207.00 5325.81 85.91 o 6 6 0 98.69 89.02 12.11 o 7 6 0 2768.63 2961.42 100.04 o 8 6 0 99.02 113.99 16.79 o 9 6 0 21.12 31.96 15.90 o 10 6 0 1657.25 1706.02 70.70 o 11 6 0 63.62 33.47 32.08 o 12 6 0 354.13 314.52 42.83 o 13 6 0 268.22 227.73 48.87 o 14 6 0 15.21 -23.44 68.18 o 1 7 0 1540.43 1515.01 28.54 o 2 7 0 355.71 385.25 23.65 o 3 7 0 826.16 838.06 28.83 o 4 7 0 1011.17 1024.58 32.98 o 5 7 0 0.09 -3.64 12.73 o 6 7 0 2726.91 2899.73 63.69 o 7 7 0 353.92 388.08 38.20 o 8 7 0 33.29 23.28 18.16 o 9 7 0 289.93 267.45 40.20 o 10 7 0 99.54 48.28 27.95 o 11 7 0 910.87 836.88 57.83 o 12 7 0 160.30 123.88 47.12 o 13 7 0 21.60 -48.67 48.67 o 0 8 0 2630.01 2762.24 87.31 o 1 8 0 443.01 377.94 38.20 o 2 8 0 190.17 201.23 41.84 o 3 8 0 899.23 842.15 33.60 o 4 8 0 81.55 86.24 20.86 o 5 8 0 4360.15 4555.25 130.96 o 6 8 0 673.43 644.69 37.57 o 7 8 0 43.82 10.91 20.58 o 8 8 0 334.31 260.87 54.57 o 9 8 0 6.61 49.06 37.25 o 10 8 0 579.72 571.49 58.50 o 11 8 0 19.58 14.34 44.96 o 12 8 0 25.97 -28.72 47.07 o 13 8 0 67.44 43.91 67.76 o 1 9 0 840.01 813.93 23.55 o 2 9 0 1361.59 1396.95 52.75 o 3 9 0 279.08 277.39 32.74 o 4 9 0 49.66 41.73 20.86 o 5 9 0 472.60 421.00 33.14 o 6 9 0 501.13 448.00 35.74 o 7 9 0 1359.31 1403.61 66.40 o 8 9 0 271.70 201.82 44.40 o 9 9 0 145.12 75.81 35.06 o 10 9 0 25.71 7.03 96.40 o 11 9 0 96.55 71.54 58.21 o 12 9 0 91.02 69.93 55.81 o 0 10 0 6735.09 7055.66 217.00 o 1 10 0 213.44 253.47 30.92 o 2 10 0 17.98 23.65 23.15 o 3 10 0 1031.09 1044.31 140.06 o 4 10 0 0.33 12.20 21.83 o 5 10 0 201.90 202.87 40.02 o 6 10 0 21.96 49.28 27.95 o 7 10 0 9.42 5.46 28.30 o 8 10 0 94.98 47.29 35.79 o 9 10 0 0.14 -50.93 50.93 o 10 10 0 34.63 30.26 53.84 o 11 10 0 33.56 -33.18 51.57 o 1 11 0 405.75 297.56 50.93 o 2 11 0 147.05 150.37 39.81 o 3 11 0 95.91 114.59 38.59 o 4 11 0 31.65 17.32 26.92 o 5 11 0 48.11 10.44 28.83 o 6 11 0 243.68 228.26 43.65 o 7 11 0 79.17 26.28 49.11 o 8 11 0 1.45 -35.79 35.79 o 9 11 0 0.22 0.39 43.50 o 10 11 0 3.56 12.69 50.96 o 0 12 0 16.54 -32.74 36.01 o 1 12 0 88.73 91.28 41.00 o 2 12 0 1.13 -40.02 43.65 o 3 12 0 442.28 409.34 47.29 o 4 12 0 86.72 114.15 36.70 o 5 12 0 482.22 402.80 56.39 o 6 12 0 2.29 -2.91 36.32 o 7 12 0 23.86 -46.79 46.79 o 8 12 0 23.02 12.10 61.13 o 9 12 0 17.43 55.04 60.75 o 1 13 0 82.98 117.18 61.84 o 2 13 0 117.94 78.75 42.83 o 3 13 0 5.13 -35.06 35.06 o 4 13 0 118.17 73.57 42.97 o 5 13 0 6.04 -30.87 45.09 o 6 13 0 157.58 58.14 107.32 o 7 13 0 4.18 10.16 54.23 o 8 13 0 5.65 -29.10 52.39 o 0 14 0 62.37 47.29 87.31 o 1 14 0 22.28 37.87 48.94 o 2 14 0 20.05 -48.43 48.43 o 3 14 0 71.59 89.13 46.30 o 4 14 0 80.15 114.78 48.07 o 5 14 0 62.06 83.28 89.13 o 6 14 0 13.60 29.16 79.88 o 7 14 0 0.17 76.97 121.87 o 1 15 0 50.60 90.95 94.58 o 2 15 0 10.97 -25.68 65.26 o 3 15 0 15.63 -6.18 83.67 o 4 15 0 48.40 -51.35 87.31 o -15 1 1 3.32 -47.29 76.39 o -14 1 1 79.14 38.70 74.58 o -13 1 1 7.78 -5.46 33.44 o -12 1 1 68.33 10.91 26.92 o -11 1 1 205.97 193.69 40.02 o -10 1 1 24.69 13.43 15.42 o -9 1 1 1452.06 1553.36 34.09 o -8 1 1 437.25 421.31 30.92 o -7 1 1 1494.73 1577.58 26.92 o -6 1 1 0.10 2.43 3.25 o -5 1 1 1059.29 1079.90 16.57 o -4 1 1 45.20 44.43 3.25 o -3 1 1 15.47 20.17 2.57 o -2 1 1 5.17 7.28 2.57 o -1 1 1 19.59 16.57 2.57 o 0 1 1 39.29 33.14 3.64 o 1 1 1 3.51 5.46 2.57 o 2 1 1 146.67 143.90 5.46 o 3 1 1 221.06 209.32 5.46 o 4 1 1 899.60 916.95 21.83 o 5 1 1 233.67 216.98 8.73 o 6 1 1 2456.11 2467.80 34.09 o 7 1 1 215.48 208.51 21.83 o 8 1 1 540.71 480.31 20.58 o 9 1 1 1.63 3.97 12.63 o 10 1 1 12.65 7.00 16.57 o 11 1 1 46.28 20.76 21.75 o 12 1 1 27.09 -8.42 41.84 o 13 1 1 47.85 32.20 36.38 o 14 1 1 2.25 -42.39 42.39 o -15 2 1 64.34 -39.52 56.42 o -14 2 1 0.04 38.74 67.30 o -13 2 1 75.04 29.10 81.85 o -12 2 1 50.36 20.01 38.20 o -11 2 1 109.94 85.69 22.73 o -10 2 1 708.90 702.08 70.94 o -9 2 1 42.76 40.93 14.80 o -8 2 1 705.55 744.90 25.46 o -7 2 1 2.46 2.60 8.73 o -6 2 1 1649.23 1647.95 26.92 o -5 2 1 121.46 126.76 9.36 o -4 2 1 247.60 257.57 6.51 o -3 2 1 285.30 261.74 6.05 o -2 2 1 4.74 9.09 2.57 o -1 2 1 683.25 597.65 8.73 o 0 2 1 288.34 289.49 9.09 o 1 2 1 1124.80 1026.74 13.97 o 2 2 1 355.40 316.66 7.72 o 3 2 1 254.68 229.18 7.72 o 4 2 1 458.90 485.98 11.36 o 5 2 1 30.69 9.46 7.28 o 6 2 1 300.35 255.95 18.19 o 7 2 1 913.97 900.74 27.28 o 8 2 1 7.61 -6.87 11.36 o 9 2 1 58.67 53.00 27.28 o 10 2 1 8.74 3.92 16.57 o 11 2 1 9.58 5.46 20.58 o 12 2 1 243.08 218.33 36.01 o 13 2 1 1.98 22.96 39.03 o 14 2 1 32.41 88.09 47.12 o -15 3 1 24.55 9.84 65.56 o -14 3 1 125.58 109.86 48.43 o -13 3 1 5.17 1.04 34.92 o -12 3 1 0.72 25.46 32.08 o -11 3 1 19.49 -25.72 25.72 o -10 3 1 124.01 90.95 21.75 o -9 3 1 168.92 122.69 15.42 o -8 3 1 112.77 130.58 27.28 o -7 3 1 1336.54 1416.23 26.92 o -6 3 1 340.35 346.57 12.11 o -5 3 1 1042.20 1069.83 18.16 o -4 3 1 1703.02 1662.92 26.92 o -3 3 1 15.92 12.13 3.25 o -2 3 1 5456.37 5406.96 69.31 o -1 3 1 224.43 252.12 12.73 o 0 3 1 2247.47 2127.72 30.92 o 1 3 1 2908.09 2742.30 32.74 o 2 3 1 37.28 33.14 5.14 o 3 3 1 1106.89 1015.72 21.83 o 4 3 1 881.07 862.42 15.43 o 5 3 1 1.15 1.46 6.05 o 6 3 1 103.38 93.09 10.29 o 7 3 1 58.14 52.81 10.29 o 8 3 1 89.34 89.90 14.80 o 9 3 1 15.91 3.64 15.43 o 10 3 1 33.33 65.48 30.92 o 11 3 1 148.75 133.41 30.92 o 12 3 1 27.65 -18.19 25.72 o 13 3 1 29.08 -37.85 50.93 o 14 3 1 24.91 7.28 53.84 o -14 4 1 18.93 -18.89 58.46 o -13 4 1 273.69 354.86 54.57 o -12 4 1 0.58 -15.34 27.54 o -11 4 1 73.29 45.47 30.55 o -10 4 1 28.48 -9.42 21.75 o -9 4 1 173.14 192.39 27.28 o -8 4 1 6.94 3.64 6.90 o -7 4 1 1325.04 1383.41 28.54 o -6 4 1 2548.95 2514.46 42.83 o -5 4 1 2119.84 2151.02 38.33 o -4 4 1 1694.46 1643.34 26.92 o -3 4 1 228.18 207.42 7.72 o -2 4 1 164.75 153.14 7.72 o -1 4 1 2108.55 1955.11 60.02 o 0 4 1 1738.33 1634.32 41.84 o 1 4 1 562.75 499.21 11.36 o 2 4 1 108.40 112.77 5.14 o 3 4 1 86.17 78.59 7.72 o 4 4 1 720.59 714.95 15.43 o 5 4 1 1548.48 1425.76 24.34 o 6 4 1 279.79 244.87 12.11 o 7 4 1 891.26 903.79 47.29 o 8 4 1 135.79 133.40 15.43 o 9 4 1 62.31 44.87 19.16 o 10 4 1 26.82 41.71 19.16 o 11 4 1 99.19 61.48 40.02 o 12 4 1 358.68 368.27 39.31 o 13 4 1 0.89 -33.51 41.00 o 14 4 1 58.94 50.14 47.54 o -14 5 1 330.84 346.75 72.76 o -13 5 1 19.61 36.61 40.20 o -12 5 1 329.13 301.67 42.39 o -11 5 1 106.02 76.13 34.66 o -10 5 1 1019.96 1040.14 74.58 o -9 5 1 934.04 885.78 56.39 o -8 5 1 84.87 64.18 16.37 o -7 5 1 924.76 933.53 67.30 o -6 5 1 1444.05 1376.69 34.66 o -5 5 1 250.34 229.30 29.10 o -4 5 1 1256.05 1192.49 24.34 o -3 5 1 63.35 67.35 7.72 o -2 5 1 5334.87 5433.68 70.42 o -1 5 1 3306.07 3402.45 40.92 o 0 5 1 1332.75 1411.07 21.75 o 1 5 1 4391.90 4172.00 70.94 o 2 5 1 61.14 55.74 6.05 o 3 5 1 3334.53 3259.55 43.73 o 4 5 1 1652.36 1635.04 65.48 o 5 5 1 1211.89 1156.96 30.92 o 6 5 1 2564.37 2455.02 56.39 o 7 5 1 233.77 215.54 12.63 o 8 5 1 908.22 933.07 50.93 o 9 5 1 217.15 226.09 20.10 o 10 5 1 178.90 219.94 28.83 o 11 5 1 531.92 534.46 44.52 o 12 5 1 5.55 10.91 35.74 o 13 5 1 60.99 52.65 47.07 o 14 5 1 0.66 0.00 45.55 o -14 6 1 40.33 99.29 52.69 o -13 6 1 470.19 420.82 58.50 o -12 6 1 206.37 169.26 39.81 o -11 6 1 723.69 620.90 46.30 o -10 6 1 2472.73 2390.53 88.49 o -9 6 1 624.86 636.15 56.39 o -8 6 1 922.86 907.30 30.92 o -7 6 1 218.88 178.99 16.27 o -6 6 1 500.06 449.07 21.75 o -5 6 1 2097.79 2117.23 44.96 o -4 6 1 74.62 54.66 14.55 o -3 6 1 3595.08 3633.08 57.49 o -2 6 1 994.75 1027.72 25.72 o -1 6 1 2548.21 2491.80 49.11 o 0 6 1 3626.55 3680.72 48.07 o 1 6 1 598.14 579.10 13.97 o 2 6 1 8633.37 8903.68 110.06 o 3 6 1 152.48 151.51 8.73 o 4 6 1 5990.20 6193.94 95.07 o 5 6 1 156.39 121.04 12.86 o 6 6 1 304.59 255.17 14.80 o 7 6 1 2861.22 2808.54 54.19 o 8 6 1 418.15 373.10 23.15 o 9 6 1 1302.59 1338.87 45.47 o 10 6 1 384.03 379.33 52.75 o 11 6 1 492.34 451.30 72.76 o 12 6 1 318.77 251.66 42.39 o 13 6 1 8.82 10.91 43.73 o -13 7 1 1.72 -48.67 48.67 o -12 7 1 244.47 239.53 43.50 o -11 7 1 560.77 538.29 46.09 o -10 7 1 465.36 458.69 76.39 o -9 7 1 2697.58 3009.27 103.59 o -8 7 1 484.35 473.67 40.02 o -7 7 1 2763.57 3009.13 76.39 o -6 7 1 207.04 218.71 16.37 o -5 7 1 550.26 553.65 27.54 o -4 7 1 4475.05 4520.36 110.95 o -3 7 1 5.31 10.91 10.29 o -2 7 1 6933.83 6948.12 123.79 o -1 7 1 372.39 404.36 15.42 o 0 7 1 2069.53 2156.78 34.15 o 1 7 1 5452.60 5533.95 98.22 o 2 7 1 1.75 2.73 9.09 o 3 7 1 5255.56 5277.54 93.86 o 4 7 1 965.62 1001.96 32.74 o 5 7 1 324.83 300.13 15.43 o 6 7 1 870.46 868.09 25.72 o 7 7 1 144.98 128.84 16.57 o 8 7 1 1686.71 1569.29 65.48 o 9 7 1 602.85 548.26 39.81 o 10 7 1 300.73 294.89 36.70 o 11 7 1 266.32 253.09 45.47 o 12 7 1 17.74 1.68 33.14 o 13 7 1 94.27 134.28 67.30 o -13 8 1 433.62 429.62 90.95 o -12 8 1 49.46 12.78 65.48 o -11 8 1 73.59 53.78 47.54 o -10 8 1 429.90 498.63 70.94 o -9 8 1 0.48 53.39 40.21 o -8 8 1 696.62 811.46 44.96 o -7 8 1 42.20 30.66 26.19 o -6 8 1 1525.63 1432.67 57.82 o -5 8 1 3221.48 3276.25 91.64 o -4 8 1 847.55 798.19 33.60 o -3 8 1 3336.72 3536.69 92.77 o -2 8 1 2.29 -0.99 13.97 o -1 8 1 1923.26 1829.84 40.21 o 0 8 1 595.78 582.61 22.42 o 1 8 1 720.44 745.76 22.78 o 2 8 1 2473.11 2705.89 63.25 o 3 8 1 93.80 55.41 20.01 o 4 8 1 1263.62 1310.64 54.57 o 5 8 1 194.35 209.20 22.73 o 6 8 1 39.76 38.65 20.10 o 7 8 1 204.39 220.56 24.21 o 8 8 1 0.27 -6.00 41.84 o 9 8 1 415.15 442.16 56.63 o 10 8 1 203.45 171.21 39.81 o 11 8 1 66.38 55.28 85.49 o 12 8 1 157.54 117.65 61.88 o -12 9 1 172.49 201.42 62.04 o -11 9 1 97.15 81.85 46.30 o -10 9 1 137.73 59.42 45.45 o -9 9 1 660.30 724.33 149.15 o -8 9 1 67.07 67.42 34.63 o -7 9 1 1014.87 1147.70 85.49 o -6 9 1 1056.54 1066.51 52.39 o -5 9 1 47.95 75.36 26.19 o -4 9 1 1898.20 2064.21 67.20 o -3 9 1 99.93 102.43 34.56 o -2 9 1 3753.09 4226.73 140.06 o -1 9 1 379.31 382.67 29.10 o 0 9 1 616.99 623.07 26.03 o 1 9 1 1131.01 1236.34 54.57 o 2 9 1 33.26 26.19 18.16 o 3 9 1 898.46 936.71 49.11 o 4 9 1 236.59 263.50 92.77 o 5 9 1 454.36 531.93 72.76 o 6 9 1 427.28 459.78 45.47 o 7 9 1 4.58 -3.64 29.10 o 8 9 1 92.32 63.77 72.76 o 9 9 1 350.53 341.68 51.36 o 10 9 1 177.73 307.31 56.53 o 11 9 1 273.01 147.80 44.96 o 12 9 1 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