#------------------------------------------------------------------------------ #$Date: 2016-04-02 23:02:54 +0300 (Sat, 02 Apr 2016) $ #$Revision: 180910 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/10/51/2105174.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_2105174_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 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 90.060 _cell_angle_beta 105.460 _cell_angle_gamma 90.040 _cell_length_a 12.1420 _cell_length_b 12.1360 _cell_length_c 16.0350 _exptl_crystal_F_000 1096.00 _reflns_d_resolution_high 0.7696 _cod_data_source_file hw5021090K_IV_1sup4.hkl _cod_data_source_block 090K_IV_1 #BEGIN Tags that were not found in dictionaries: _shelx_title ' k06083 in P-1' _shelx_refln_list_code 4 _shelx_f_calc_maximum 344.20 _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' 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 5623.08 5269.45 77.26 o 2 0 0 23789.41 23338.79 386.03 o 3 0 0 559.39 657.38 10.78 o 4 0 0 1353.38 1228.28 20.26 o 5 0 0 50668.28 52768.24 1187.62 o 6 0 0 1393.01 1377.33 23.72 o 7 0 0 11929.90 12006.66 182.29 o 8 0 0 7569.57 7547.61 127.05 o 9 0 0 1004.64 1054.48 67.77 o 10 0 0 384.19 409.99 14.01 o 11 0 0 1992.50 1855.27 50.85 o 12 0 0 3241.58 3347.69 88.95 o 13 0 0 2259.18 2383.03 78.78 o 14 0 0 37.48 52.45 36.83 o 15 0 0 516.20 416.70 142.31 o -15 1 0 17.09 -4.98 39.89 o -14 1 0 353.60 357.55 45.92 o -13 1 0 551.30 533.66 37.72 o -12 1 0 2371.98 2407.84 73.08 o -11 1 0 5524.89 5824.45 138.23 o -10 1 0 524.74 533.86 26.95 o -9 1 0 960.75 982.62 35.58 o -8 1 0 95.31 78.74 13.48 o -7 1 0 3091.13 2909.60 50.03 o -6 1 0 15539.62 15274.98 284.76 o -5 1 0 1913.72 2099.52 66.07 o -4 1 0 18437.28 17539.66 327.25 o -3 1 0 10168.72 9530.05 155.38 o -2 1 0 1101.55 1141.55 18.31 o 0 1 0 65.78 65.85 3.39 o 1 1 0 44059.26 41692.58 903.95 o 2 1 0 994.19 1059.71 15.57 o 3 1 0 10077.46 9481.72 140.81 o 4 1 0 17920.96 17511.80 221.70 o 5 1 0 2084.03 2229.14 51.67 o 6 1 0 15239.29 15491.18 271.07 o 7 1 0 2876.46 2793.04 41.68 o 8 1 0 108.69 97.84 13.55 o 9 1 0 1051.12 1048.84 33.88 o 10 1 0 573.97 584.62 24.57 o 11 1 0 5948.29 6081.69 118.25 o 12 1 0 2235.06 2240.52 74.54 o 13 1 0 645.57 585.87 46.59 o 14 1 0 336.54 284.99 44.38 o 15 1 0 20.64 37.89 39.04 o -15 2 0 1241.25 1312.25 79.38 o -14 2 0 109.71 174.39 58.45 o -13 2 0 844.56 840.09 50.31 o -12 2 0 1658.10 1701.09 79.63 o -11 2 0 60.00 50.83 27.11 o -10 2 0 4812.54 5187.56 127.06 o -9 2 0 2227.75 2322.57 66.92 o -8 2 0 5574.82 5694.96 102.25 o -7 2 0 6037.24 6240.16 101.30 o -6 2 0 752.79 751.73 21.18 o -5 2 0 18551.62 18334.89 398.13 o -4 2 0 1612.02 1527.29 40.26 o -3 2 0 9362.68 8677.17 152.65 o -2 2 0 2967.76 3064.40 61.31 o -1 2 0 1135.74 1039.53 18.73 o 0 2 0 10690.62 9594.03 143.90 o 1 2 0 1046.11 963.37 14.65 o 2 2 0 2790.53 2958.27 43.13 o 3 2 0 9743.86 8958.01 102.69 o 4 2 0 1955.25 1831.40 54.21 o 5 2 0 19061.61 18983.59 474.37 o 6 2 0 828.34 797.96 16.77 o 7 2 0 6198.36 6291.09 89.54 o 8 2 0 5229.22 5458.62 95.07 o 9 2 0 2334.59 2310.13 55.06 o 10 2 0 4949.72 5083.06 96.48 o 11 2 0 70.99 75.81 16.13 o 12 2 0 1718.74 1734.36 61.27 o 13 2 0 793.69 806.97 51.67 o 14 2 0 113.53 159.12 58.45 o 15 2 0 1284.65 1289.95 148.24 o -14 3 0 850.54 793.83 52.09 o -13 3 0 33.76 57.94 33.83 o -12 3 0 88.13 70.73 26.15 o -11 3 0 4102.33 3925.29 125.68 o -10 3 0 879.64 845.77 65.23 o -9 3 0 6249.74 6237.94 149.09 o -8 3 0 1568.52 1575.25 36.59 o -7 3 0 1308.38 1315.57 37.83 o -6 3 0 1144.12 995.90 21.94 o -5 3 0 2526.45 2636.72 76.24 o -4 3 0 19151.82 19573.09 324.77 o -3 3 0 9936.13 9594.69 297.33 o -2 3 0 5855.11 5529.49 97.06 o -1 3 0 4523.30 4555.07 112.66 o 0 3 0 13.52 17.14 2.82 o 1 3 0 4493.16 4556.00 104.19 o 2 3 0 5621.66 5359.35 91.19 o 3 3 0 10990.73 10426.80 286.32 o 4 3 0 19786.83 20391.30 464.20 o 5 3 0 2163.34 2399.21 67.77 o 6 3 0 1178.18 996.88 20.33 o 7 3 0 1102.94 1252.57 34.47 o 8 3 0 1509.26 1618.32 45.74 o 9 3 0 5761.66 5878.33 136.27 o 10 3 0 879.01 863.06 38.12 o 11 3 0 3754.73 3769.70 95.50 o 12 3 0 80.01 116.99 25.07 o 13 3 0 29.81 -26.77 26.77 o 14 3 0 809.00 833.34 50.48 o -14 4 0 45.04 35.58 49.13 o -13 4 0 136.04 106.53 31.50 o -12 4 0 298.48 232.45 38.12 o -11 4 0 183.05 175.16 63.53 o -10 4 0 4225.94 4172.75 169.42 o -9 4 0 346.15 317.58 21.79 o -8 4 0 4549.26 4574.79 92.28 o -7 4 0 4902.32 4947.76 95.27 o -6 4 0 746.61 756.29 20.33 o -5 4 0 11873.10 12279.58 233.80 o -4 4 0 1940.38 2263.93 52.01 o -3 4 0 9390.66 9363.53 203.30 o -2 4 0 13982.08 13832.83 304.95 o -1 4 0 2749.43 2663.26 44.13 o 0 4 0 47044.49 44456.14 2233.77 o 1 4 0 2335.54 2139.34 59.07 o 2 4 0 15369.91 14231.73 269.38 o 3 4 0 8502.39 8747.39 162.82 o 4 4 0 1625.12 2060.69 48.28 o 5 4 0 11403.34 11880.22 149.73 o 6 4 0 709.10 750.44 44.05 o 7 4 0 4837.93 4997.49 85.50 o 8 4 0 4160.24 4305.35 135.53 o 9 4 0 323.90 315.06 17.65 o 10 4 0 3967.18 3943.30 111.86 o 11 4 0 197.41 194.54 23.36 o 12 4 0 249.94 177.35 32.80 o 13 4 0 121.15 56.81 42.05 o 14 4 0 52.59 96.53 81.32 o -14 5 0 1417.55 1346.15 162.64 o -13 5 0 98.47 93.53 36.62 o -12 5 0 68.23 63.66 46.59 o -11 5 0 2225.63 2170.38 91.41 o -10 5 0 964.46 872.12 43.11 o -9 5 0 2291.33 2206.51 71.04 o -8 5 0 109.54 74.07 27.11 o -7 5 0 22.46 29.32 17.79 o -6 5 0 5835.78 5811.94 112.88 o -5 5 0 44.78 28.80 6.89 o -4 5 0 7570.89 7770.71 168.67 o -3 5 0 9156.10 9593.92 189.10 o -2 5 0 10451.31 11181.66 300.72 o -1 5 0 12685.52 12359.73 365.94 o 0 5 0 860.72 854.36 22.02 o 1 5 0 12802.80 12811.59 384.58 o 2 5 0 9623.60 10199.90 215.30 o 3 5 0 9633.85 9522.85 166.29 o 4 5 0 6649.96 6712.63 422.70 o 5 5 0 40.81 35.66 7.19 o 6 5 0 5344.68 5529.00 107.85 o 7 5 0 24.72 38.12 9.58 o 8 5 0 132.14 132.15 16.61 o 9 5 0 2056.77 2070.80 77.09 o 10 5 0 799.12 743.39 39.43 o 11 5 0 1972.72 2131.78 93.98 o 12 5 0 74.49 79.82 63.53 o 13 5 0 91.84 70.77 38.12 o 14 5 0 1283.46 1374.84 96.42 o -14 6 0 34.07 -33.24 45.39 o -13 6 0 667.68 548.91 121.98 o -12 6 0 602.32 672.42 51.57 o -11 6 0 359.73 424.16 38.99 o -10 6 0 2062.55 2040.38 79.51 o -9 6 0 332.23 276.68 27.44 o -8 6 0 140.58 145.13 20.68 o -7 6 0 3507.52 3855.39 75.22 o -6 6 0 121.15 152.93 30.50 o -5 6 0 5785.00 6070.86 197.22 o -4 6 0 433.87 404.66 21.18 o -3 6 0 337.30 318.04 15.44 o -2 6 0 9295.35 10029.05 333.75 o -1 6 0 338.04 332.14 10.78 o 0 6 0 15931.51 16834.42 521.81 o 1 6 0 343.53 357.76 11.98 o 2 6 0 9079.18 9553.73 184.57 o 3 6 0 284.09 271.89 13.29 o 4 6 0 403.08 410.52 17.79 o 5 6 0 5420.09 5868.20 123.35 o 6 6 0 142.94 168.46 11.80 o 7 6 0 3484.82 3726.43 94.03 o 8 6 0 116.44 146.54 18.72 o 9 6 0 328.13 305.14 25.07 o 10 6 0 2072.48 1993.16 67.49 o 11 6 0 300.22 345.86 33.29 o 12 6 0 528.88 419.57 47.84 o 13 6 0 572.47 605.94 63.36 o 14 6 0 31.02 40.66 66.07 o -13 7 0 111.98 70.66 39.55 o -12 7 0 310.67 307.17 44.05 o -11 7 0 1160.18 1114.85 56.00 o -10 7 0 276.12 207.89 35.09 o -9 7 0 318.54 213.47 33.88 o -8 7 0 128.92 138.92 25.41 o -7 7 0 536.09 572.47 21.00 o -6 7 0 3096.81 3179.26 80.09 o -5 7 0 143.68 161.82 16.61 o -4 7 0 1045.81 976.51 33.78 o -3 7 0 598.64 590.09 36.42 o -2 7 0 1575.22 1610.00 56.17 o -1 7 0 1297.29 1285.96 55.06 o 0 7 0 634.90 576.71 18.47 o 1 7 0 1126.57 1089.36 43.42 o 2 7 0 1302.49 1241.24 58.29 o 3 7 0 609.58 567.31 26.26 o 4 7 0 994.67 994.87 26.26 o 5 7 0 139.13 199.52 34.73 o 6 7 0 2987.88 3265.89 85.24 o 7 7 0 521.44 556.60 38.53 o 8 7 0 109.47 44.71 28.80 o 9 7 0 306.41 285.90 26.77 o 10 7 0 334.14 267.68 37.27 o 11 7 0 1140.45 1170.92 60.65 o 12 7 0 268.40 261.72 37.83 o 13 7 0 105.33 110.32 39.89 o -13 8 0 134.46 57.96 38.68 o -12 8 0 45.92 90.47 42.71 o -11 8 0 28.19 -20.69 35.09 o -10 8 0 901.59 955.96 51.61 o -9 8 0 33.08 35.58 30.50 o -8 8 0 547.40 586.18 45.74 o -7 8 0 5.17 -7.62 23.72 o -6 8 0 1419.11 1514.40 70.19 o -5 8 0 4424.75 4996.68 160.60 o -4 8 0 508.52 495.88 53.37 o -3 8 0 902.10 889.29 41.02 o -2 8 0 771.74 799.88 44.43 o -1 8 0 1093.64 1105.84 34.12 o 0 8 0 2231.16 2500.60 92.33 o 1 8 0 904.15 881.31 38.53 o 2 8 0 638.76 682.69 45.74 o 3 8 0 921.70 912.47 30.72 o 4 8 0 438.21 400.05 52.52 o 5 8 0 4344.00 4649.17 119.08 o 6 8 0 1187.53 1205.71 83.34 o 7 8 0 4.78 4.79 19.84 o 8 8 0 508.61 519.49 113.51 o 9 8 0 27.54 39.80 31.34 o 10 8 0 921.17 1020.37 64.30 o 11 8 0 25.05 58.50 29.15 o 12 8 0 40.11 10.92 42.33 o 13 8 0 110.76 52.52 47.44 o -12 9 0 198.97 238.79 88.10 o -11 9 0 255.94 246.33 39.55 o -10 9 0 65.25 42.35 35.58 o -9 9 0 459.16 432.37 39.22 o -8 9 0 641.29 665.81 45.74 o -7 9 0 1979.81 2044.39 157.56 o -6 9 0 413.12 360.98 49.13 o -5 9 0 951.80 869.87 94.87 o -4 9 0 1.87 6.53 12.20 o -3 9 0 495.13 462.31 37.83 o -2 9 0 1408.36 1595.01 60.79 o -1 9 0 784.69 828.38 70.31 o 0 9 0 63.04 37.53 10.44 o 1 9 0 738.08 704.93 31.32 o 2 9 0 1324.45 1398.26 51.59 o 3 9 0 444.67 387.91 60.99 o 4 9 0 1.80 22.45 22.87 o 5 9 0 1119.72 1075.60 67.13 o 6 9 0 437.42 387.92 45.74 o 7 9 0 1804.07 1849.51 97.15 o 8 9 0 624.62 585.31 40.08 o 9 9 0 382.54 316.36 63.53 o 10 9 0 76.50 11.65 47.44 o 11 9 0 211.02 146.53 46.02 o 12 9 0 170.41 155.53 50.75 o -11 10 0 110.65 83.92 46.64 o -10 10 0 60.59 54.21 45.74 o -9 10 0 2.06 -15.25 32.19 o -8 10 0 310.84 306.65 44.05 o -7 10 0 14.32 -44.90 44.90 o -6 10 0 228.97 192.46 27.89 o -5 10 0 266.54 270.24 27.89 o -4 10 0 229.81 224.90 46.59 o -3 10 0 1381.60 1512.30 68.61 o -2 10 0 328.67 315.32 33.88 o -1 10 0 683.04 699.83 52.52 o 0 10 0 6667.78 7283.35 228.91 o 1 10 0 828.39 878.63 68.61 o 2 10 0 319.51 266.12 42.35 o 3 10 0 1290.46 1256.15 66.82 o 4 10 0 227.13 161.52 24.65 o 5 10 0 230.90 184.95 28.80 o 6 10 0 227.32 155.38 73.70 o 7 10 0 12.67 31.47 26.95 o 8 10 0 282.12 239.64 50.83 o 9 10 0 1.79 -11.34 35.64 o 10 10 0 49.80 47.48 38.14 o 11 10 0 96.90 114.12 55.47 o -10 11 0 12.60 -20.33 45.74 o -9 11 0 62.25 6.78 44.05 o -8 11 0 39.18 20.33 35.58 o -7 11 0 56.27 30.50 44.05 o -6 11 0 289.20 389.66 76.24 o -5 11 0 77.63 67.19 24.37 o -4 11 0 9.37 2.48 18.79 o -3 11 0 261.10 241.54 30.27 o -2 11 0 254.84 226.01 44.05 o -1 11 0 532.25 572.89 49.24 o 0 11 0 5.45 -5.31 35.58 o 1 11 0 439.31 346.09 57.60 o 2 11 0 290.16 247.43 27.81 o 3 11 0 263.40 183.75 26.77 o 4 11 0 10.86 17.77 20.40 o 5 11 0 89.68 89.64 29.42 o 6 11 0 255.37 173.84 40.66 o 7 11 0 49.93 77.45 50.83 o 8 11 0 46.97 28.75 38.54 o 9 11 0 68.99 85.09 67.77 o 10 11 0 11.85 1.71 44.50 o -9 12 0 25.22 6.78 55.91 o -8 12 0 71.89 59.30 96.57 o -7 12 0 152.67 99.96 81.32 o -6 12 0 29.35 43.42 29.69 o -5 12 0 453.34 475.13 89.79 o -4 12 0 354.14 375.15 42.35 o -3 12 0 289.71 262.17 34.49 o -2 12 0 95.08 61.95 28.98 o -1 12 0 493.42 486.91 60.22 o 0 12 0 66.91 39.14 23.36 o 1 12 0 407.13 319.53 45.74 o 2 12 0 85.43 47.93 44.90 o 3 12 0 323.28 274.41 35.52 o 4 12 0 300.05 260.84 86.40 o 5 12 0 412.82 388.52 43.28 o 6 12 0 25.43 -0.09 34.22 o 7 12 0 184.81 238.28 89.79 o 8 12 0 78.98 121.98 50.83 o 9 12 0 30.20 24.31 61.84 o -8 13 0 41.75 12.99 59.30 o -7 13 0 102.04 135.53 50.83 o -6 13 0 333.64 232.10 52.52 o -5 13 0 44.33 16.49 33.98 o -4 13 0 22.25 35.55 27.92 o -3 13 0 83.34 69.15 29.08 o -2 13 0 84.72 108.69 44.77 o -1 13 0 200.73 194.15 45.99 o 0 13 0 275.57 338.67 59.30 o 1 13 0 234.34 259.72 39.08 o 2 13 0 70.47 100.52 89.79 o 3 13 0 80.13 115.71 62.68 o 4 13 0 25.08 50.75 41.51 o 5 13 0 52.73 61.91 52.52 o 6 13 0 374.70 386.41 48.02 o 7 13 0 84.22 113.91 44.87 o 8 13 0 50.46 116.37 88.10 o -7 14 0 139.58 191.44 113.51 o -6 14 0 92.95 150.78 64.38 o -5 14 0 99.94 36.74 45.33 o -4 14 0 225.87 67.77 44.05 o -3 14 0 125.17 61.67 69.46 o -2 14 0 112.71 -48.79 48.79 o -1 14 0 58.31 59.03 52.67 o 0 14 0 170.81 122.00 49.65 o 1 14 0 48.31 75.52 32.88 o 2 14 0 133.88 218.79 117.75 o 3 14 0 124.66 43.12 38.91 o 4 14 0 273.95 213.96 47.10 o 5 14 0 114.82 98.26 45.46 o 6 14 0 76.47 -12.90 60.14 o -4 15 0 139.03 33.46 57.65 o -3 15 0 49.30 90.82 54.48 o -2 15 0 34.43 45.52 53.36 o -1 15 0 131.11 121.33 49.00 o 0 15 0 63.80 147.24 59.22 o 1 15 0 145.67 143.93 65.40 o 2 15 0 33.84 -6.08 60.14 o 3 15 0 56.12 13.05 48.02 o 4 15 0 135.59 189.03 53.35 o -4 -15 1 287.52 279.01 86.55 o -3 -15 1 211.24 174.91 51.52 o -2 -15 1 670.31 471.30 63.64 o -1 -15 1 315.85 196.52 91.49 o 0 -15 1 141.60 32.92 55.67 o 1 -15 1 93.17 204.15 64.69 o 2 -15 1 48.80 30.07 55.14 o 3 -15 1 157.58 151.88 106.73 o 4 -15 1 64.85 -44.05 79.63 o -7 -14 1 335.01 331.99 88.95 o -6 -14 1 260.24 244.43 72.85 o -5 -14 1 476.28 428.91 63.80 o -4 -14 1 461.84 381.07 71.16 o -3 -14 1 510.83 495.17 50.53 o -2 -14 1 100.26 111.28 36.05 o -1 -14 1 432.35 337.85 56.66 o 0 -14 1 114.87 138.92 54.21 o 1 -14 1 110.41 98.03 67.77 o 2 -14 1 298.30 302.03 89.79 o 3 -14 1 230.99 210.06 44.81 o 4 -14 1 248.05 208.34 61.84 o 5 -14 1 179.68 271.07 57.60 o 6 -14 1 164.05 154.17 57.60 o -8 -13 1 220.99 273.11 57.60 o -7 -13 1 900.64 682.68 117.75 o -6 -13 1 252.36 253.84 72.85 o -5 -13 1 300.57 243.45 55.06 o -4 -13 1 977.55 986.13 78.04 o -3 -13 1 580.26 542.96 54.73 o -2 -13 1 1317.12 1321.28 85.56 o -1 -13 1 616.17 684.64 51.43 o 0 -13 1 966.36 1041.91 93.72 o 1 -13 1 1287.49 1369.68 107.58 o 2 -13 1 441.98 394.57 43.28 o 3 -13 1 448.51 505.17 76.24 o 4 -13 1 466.67 568.29 57.28 o 5 -13 1 354.57 410.43 49.48 o 6 -13 1 625.78 711.55 83.01 o 7 -13 1 138.58 135.53 67.77 o 8 -13 1 219.50 125.37 62.68 o -10 -12 1 460.43 484.53 93.18 o -9 -12 1 219.98 153.71 49.91 o -8 -12 1 623.74 552.64 147.39 o -7 -12 1 438.71 427.21 99.96 o -6 -12 1 1270.55 1268.25 134.69 o -5 -12 1 2143.05 2312.68 148.74 o -4 -12 1 308.67 247.58 44.90 o -3 -12 1 1637.11 1709.81 108.43 o -2 -12 1 729.93 755.60 44.87 o -1 -12 1 874.24 901.99 72.53 o 0 -12 1 3365.53 3976.24 220.63 o 1 -12 1 919.24 793.31 201.61 o 2 -12 1 3968.81 4286.69 250.74 o 3 -12 1 1018.41 1155.76 93.18 o 4 -12 1 1038.82 1004.51 134.29 o 5 -12 1 914.78 918.20 114.36 o 6 -12 1 385.49 389.66 110.12 o 7 -12 1 823.77 943.65 94.87 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