#------------------------------------------------------------------------------ #$Date: 2016-04-02 23:02:54 +0300 (Sat, 02 Apr 2016) $ #$Revision: 180910 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/10/51/2105175.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_2105175_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 12.1460 _cell_length_b 12.1440 _cell_length_c 16.0430 _exptl_crystal_F_000 1096.00 _reflns_d_resolution_high 0.7696 _cod_data_source_file hw5021100K_IV_1sup5.hkl _cod_data_source_block 100K_IV_1 #BEGIN Tags that were not found in dictionaries: _shelx_title ' k06084 in P-1' _shelx_refln_list_code 4 _shelx_f_calc_maximum 295.06 _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 5647.61 5325.75 81.22 o 2 0 0 23848.55 23612.69 407.97 o 3 0 0 561.30 688.55 10.91 o 4 0 0 1354.12 1262.08 19.98 o 5 0 0 49617.07 51602.28 784.08 o 6 0 0 1370.19 1330.83 32.58 o 7 0 0 11578.32 11820.49 183.13 o 8 0 0 7410.79 7526.35 129.92 o 9 0 0 959.74 1010.65 22.78 o 10 0 0 373.63 409.67 14.29 o 11 0 0 1890.59 1750.55 49.34 o 12 0 0 3043.80 3206.02 90.34 o 13 0 0 2082.30 2249.72 79.92 o 14 0 0 40.10 6.07 35.52 o 15 0 0 469.67 416.09 55.74 o -15 1 0 17.78 4.23 36.32 o -14 1 0 361.80 288.61 80.60 o -13 1 0 508.60 521.11 65.17 o -12 1 0 2244.68 2304.46 67.62 o -11 1 0 5201.53 5389.68 120.66 o -10 1 0 503.08 527.84 28.44 o -9 1 0 940.29 948.89 32.50 o -8 1 0 111.37 76.66 13.80 o -7 1 0 3041.69 2767.42 108.04 o -6 1 0 15229.37 15087.33 329.27 o -5 1 0 1904.06 2198.56 42.32 o -4 1 0 18287.24 17357.68 359.28 o -3 1 0 10268.12 9586.42 157.24 o -2 1 0 1107.95 1136.06 18.53 o 0 1 0 60.71 63.45 1.53 o 1 1 0 44128.36 43252.10 1783.52 o 2 1 0 1000.54 1067.79 16.29 o 3 1 0 10165.47 9555.24 139.44 o 4 1 0 17792.40 17401.49 245.23 o 5 1 0 2077.55 2260.43 73.74 o 6 1 0 14944.02 15231.78 238.37 o 7 1 0 2810.82 2704.00 40.78 o 8 1 0 127.39 124.17 11.19 o 9 1 0 1008.24 1001.33 24.21 o 10 1 0 556.48 544.56 42.02 o 11 1 0 5588.42 5564.00 120.87 o 12 1 0 2106.33 2064.83 65.18 o 13 1 0 596.70 614.60 71.17 o 14 1 0 340.04 348.62 77.17 o 15 1 0 21.60 24.40 39.06 o -15 2 0 1147.88 1238.83 186.93 o -14 2 0 102.33 93.03 33.69 o -13 2 0 751.27 755.44 47.85 o -12 2 0 1553.06 1567.40 61.10 o -11 2 0 61.92 72.03 27.44 o -10 2 0 4523.77 4763.62 111.10 o -9 2 0 2125.60 2179.81 85.75 o -8 2 0 5400.28 5375.55 103.99 o -7 2 0 6017.25 6080.41 99.28 o -6 2 0 732.72 671.21 18.53 o -5 2 0 18575.85 18437.71 439.02 o -4 2 0 1553.89 1484.11 48.02 o -3 2 0 9375.50 8562.46 194.64 o -2 2 0 2975.65 3039.43 69.97 o -1 2 0 1144.52 1039.16 23.15 o 0 2 0 10679.49 9714.71 142.45 o 1 2 0 1049.74 963.27 15.21 o 2 2 0 2807.02 2926.63 43.65 o 3 2 0 9769.04 8891.94 104.47 o 4 2 0 1889.00 1739.11 26.35 o 5 2 0 19094.91 19040.58 460.46 o 6 2 0 811.26 761.47 15.12 o 7 2 0 6191.89 6152.12 87.76 o 8 2 0 5063.78 5205.24 96.04 o 9 2 0 2222.97 2283.13 42.07 o 10 2 0 4644.98 4971.66 89.41 o 11 2 0 73.53 69.27 18.86 o 12 2 0 1630.02 1656.05 59.27 o 13 2 0 702.99 699.97 49.73 o 14 2 0 105.81 172.21 35.39 o 15 2 0 1176.03 1187.22 110.61 o -14 3 0 777.51 666.78 81.46 o -13 3 0 31.82 2.03 29.78 o -12 3 0 76.28 42.94 25.56 o -11 3 0 3895.40 3675.51 121.56 o -10 3 0 876.26 877.32 31.22 o -9 3 0 5932.25 5957.65 137.19 o -8 3 0 1583.82 1651.16 38.16 o -7 3 0 1251.36 1293.37 38.66 o -6 3 0 1151.83 995.25 21.43 o -5 3 0 2450.93 2507.65 50.10 o -4 3 0 18965.13 19393.81 414.15 o -3 3 0 9791.16 9554.56 236.66 o -2 3 0 5793.01 5514.27 100.40 o -1 3 0 4554.97 4593.53 87.46 o 0 3 0 6.53 12.35 2.85 o 1 3 0 4510.99 4577.16 71.05 o 2 3 0 5579.73 5287.31 90.55 o 3 3 0 10811.72 10288.66 339.55 o 4 3 0 19590.19 20249.23 354.13 o 5 3 0 2095.78 2261.86 46.11 o 6 3 0 1187.12 1015.10 26.58 o 7 3 0 1057.55 1140.29 33.74 o 8 3 0 1535.85 1578.40 36.49 o 9 3 0 5513.45 5580.90 132.42 o 10 3 0 861.72 894.31 26.90 o 11 3 0 3578.85 3653.85 94.21 o 12 3 0 68.50 37.10 36.87 o 13 3 0 27.21 0.31 33.44 o 14 3 0 742.35 687.80 51.01 o -14 4 0 39.96 24.77 32.67 o -13 4 0 122.61 86.22 49.73 o -12 4 0 294.36 234.93 33.24 o -11 4 0 167.01 136.24 28.64 o -10 4 0 3983.70 3989.49 110.44 o -9 4 0 319.05 309.28 20.74 o -8 4 0 4361.37 4529.43 97.16 o -7 4 0 4741.31 4992.41 93.58 o -6 4 0 744.71 767.37 18.77 o -5 4 0 11666.94 12052.18 234.09 o -4 4 0 1851.98 2143.09 55.21 o -3 4 0 9229.28 9225.81 210.23 o -2 4 0 13825.49 13687.03 274.39 o -1 4 0 2671.18 2653.67 60.88 o 0 4 0 46688.15 44518.61 1902.71 o 1 4 0 2278.16 2187.31 64.66 o 2 4 0 15167.83 14182.19 273.91 o 3 4 0 8394.59 8636.81 173.81 o 4 4 0 1553.31 1961.32 40.92 o 5 4 0 11186.84 11725.06 153.78 o 6 4 0 706.73 721.49 18.19 o 7 4 0 4674.25 4838.59 86.19 o 8 4 0 4025.62 4132.61 100.74 o 9 4 0 304.74 276.37 16.10 o 10 4 0 3744.40 3839.85 108.44 o 11 4 0 177.50 139.50 21.76 o 12 4 0 246.61 198.24 50.59 o 13 4 0 110.52 43.21 41.23 o 14 4 0 44.60 72.08 42.93 o -14 5 0 1315.50 1125.13 78.03 o -13 5 0 89.48 89.71 31.32 o -12 5 0 62.74 26.83 29.98 o -11 5 0 2102.40 2249.09 92.89 o -10 5 0 887.00 817.30 46.17 o -9 5 0 2217.02 2087.29 73.74 o -8 5 0 108.33 130.10 26.58 o -7 5 0 18.53 19.77 10.25 o -6 5 0 5634.53 5606.07 109.44 o -5 5 0 51.11 41.01 7.81 o -4 5 0 7427.63 7727.91 184.22 o -3 5 0 9094.19 9562.82 160.46 o -2 5 0 10366.78 11050.85 510.19 o -1 5 0 12655.13 12378.24 246.09 o 0 5 0 794.43 733.06 15.12 o 1 5 0 12784.75 12668.87 465.60 o 2 5 0 9570.57 10111.17 213.50 o 3 5 0 9539.89 9584.85 163.67 o 4 5 0 6522.04 6368.48 493.04 o 5 5 0 45.47 30.62 6.06 o 6 5 0 5145.97 5354.05 107.95 o 7 5 0 20.11 14.58 9.43 o 8 5 0 131.15 140.84 27.44 o 9 5 0 2002.85 2001.26 68.38 o 10 5 0 734.10 698.57 46.30 o 11 5 0 1866.14 1977.67 92.83 o 12 5 0 66.39 49.22 28.64 o 13 5 0 82.77 8.99 36.87 o 14 5 0 1198.37 1119.28 83.74 o -14 6 0 29.29 16.81 39.95 o -13 6 0 579.26 662.70 135.48 o -12 6 0 547.86 512.04 59.16 o -11 6 0 321.86 334.73 89.18 o -10 6 0 1967.82 2015.58 69.47 o -9 6 0 293.47 276.07 26.69 o -8 6 0 138.76 174.00 20.99 o -7 6 0 3363.30 3728.33 74.39 o -6 6 0 119.92 152.37 16.85 o -5 6 0 5669.55 5995.19 200.63 o -4 6 0 450.85 415.34 17.15 o -3 6 0 317.37 319.50 42.87 o -2 6 0 9365.08 9880.95 333.55 o -1 6 0 289.49 306.97 10.25 o 0 6 0 15878.13 16849.32 428.73 o 1 6 0 294.23 299.90 11.95 o 2 6 0 9152.74 9436.13 435.59 o 3 6 0 265.08 259.66 17.15 o 4 6 0 416.20 387.50 19.72 o 5 6 0 5317.75 5676.49 122.28 o 6 6 0 139.65 160.35 11.10 o 7 6 0 3344.15 3718.13 82.74 o 8 6 0 114.17 103.17 18.95 o 9 6 0 284.61 272.35 23.62 o 10 6 0 1974.74 2044.91 66.08 o 11 6 0 268.00 268.99 61.74 o 12 6 0 488.18 436.42 46.74 o 13 6 0 501.98 524.91 54.69 o 14 6 0 25.96 54.94 51.01 o -13 7 0 83.23 86.36 37.48 o -12 7 0 278.41 365.96 39.44 o -11 7 0 1086.29 1132.56 65.17 o -10 7 0 245.54 170.63 32.36 o -9 7 0 313.33 301.83 36.01 o -8 7 0 106.21 120.04 20.58 o -7 7 0 516.85 571.06 21.25 o -6 7 0 3004.47 3248.45 91.88 o -5 7 0 117.54 175.20 15.54 o -4 7 0 1002.73 998.11 33.24 o -3 7 0 610.38 584.40 39.44 o -2 7 0 1436.01 1500.79 53.51 o -1 7 0 1300.98 1292.18 40.30 o 0 7 0 595.02 482.68 16.81 o 1 7 0 1140.65 1089.19 48.88 o 2 7 0 1182.70 1178.84 55.82 o 3 7 0 615.53 551.85 18.68 o 4 7 0 953.44 974.88 63.45 o 5 7 0 115.51 143.64 34.30 o 6 7 0 2908.88 3098.29 93.90 o 7 7 0 499.02 501.35 83.17 o 8 7 0 88.63 69.06 24.01 o 9 7 0 302.30 304.96 42.87 o 10 7 0 296.85 256.12 27.19 o 11 7 0 1066.31 1142.70 78.03 o 12 7 0 242.81 220.93 64.31 o 13 7 0 76.93 99.14 47.38 o -13 8 0 127.21 79.58 39.26 o -12 8 0 40.08 109.66 41.52 o -11 8 0 27.18 21.80 34.80 o -10 8 0 802.96 861.38 52.31 o -9 8 0 30.79 -10.29 29.15 o -8 8 0 498.16 589.93 44.59 o -7 8 0 5.20 5.21 14.83 o -6 8 0 1358.70 1416.97 74.60 o -5 8 0 4377.93 5009.71 178.83 o -4 8 0 465.72 429.79 29.50 o -3 8 0 868.47 857.95 49.73 o -2 8 0 697.30 774.11 45.66 o -1 8 0 1059.40 1048.80 32.74 o 0 8 0 2212.67 2538.64 85.63 o 1 8 0 873.42 844.83 40.92 o 2 8 0 578.23 636.40 40.31 o 3 8 0 892.69 868.01 29.69 o 4 8 0 396.19 339.03 59.16 o 5 8 0 4310.46 4691.01 240.09 o 6 8 0 1134.55 1231.42 114.90 o 7 8 0 4.44 21.01 21.44 o 8 8 0 465.93 405.27 54.02 o 9 8 0 25.35 -21.89 42.02 o 10 8 0 817.84 953.84 58.02 o 11 8 0 23.95 57.07 29.67 o 12 8 0 35.05 108.64 47.23 o 13 8 0 104.87 39.44 39.44 o -12 9 0 193.31 168.25 64.31 o -11 9 0 231.18 255.27 50.54 o -10 9 0 58.51 41.16 25.72 o -9 9 0 392.28 377.51 34.78 o -8 9 0 572.59 670.54 48.02 o -7 9 0 1867.70 2037.71 76.94 o -6 9 0 429.55 365.59 55.74 o -5 9 0 894.51 872.91 86.40 o -4 9 0 2.11 5.49 11.42 o -3 9 0 499.36 453.43 42.87 o -2 9 0 1374.40 1577.67 61.36 o -1 9 0 768.30 805.98 58.31 o 0 9 0 74.13 60.99 10.37 o 1 9 0 726.99 766.80 34.16 o 2 9 0 1288.89 1456.24 54.08 o 3 9 0 448.30 420.69 24.87 o 4 9 0 2.10 -9.15 18.41 o 5 9 0 1054.25 1031.81 62.07 o 6 9 0 453.26 348.41 48.02 o 7 9 0 1692.12 1743.76 106.93 o 8 9 0 553.54 479.19 54.02 o 9 9 0 324.92 343.84 41.48 o 10 9 0 69.05 83.50 56.59 o 11 9 0 190.71 146.99 47.16 o 12 9 0 163.98 105.21 47.23 o -11 10 0 100.85 63.60 34.17 o -10 10 0 64.70 80.60 46.30 o -9 10 0 3.34 -1.71 37.73 o -8 10 0 262.77 252.09 44.59 o -7 10 0 12.97 10.92 23.15 o -6 10 0 195.07 145.45 22.41 o -5 10 0 267.46 221.08 27.25 o -4 10 0 187.45 158.89 23.15 o -3 10 0 1297.66 1336.04 64.92 o -2 10 0 280.09 297.33 25.55 o -1 10 0 607.27 678.73 42.56 o 0 10 0 6543.04 7096.03 216.70 o 1 10 0 736.96 790.90 43.35 o 2 10 0 267.36 226.55 19.11 o 3 10 0 1211.79 1285.02 76.31 o 4 10 0 185.96 147.75 32.58 o 5 10 0 233.88 174.80 26.83 o 6 10 0 193.07 159.02 36.01 o 7 10 0 12.06 15.56 27.90 o 8 10 0 234.84 208.78 33.98 o 9 10 0 2.82 -12.98 33.24 o 10 10 0 53.21 60.34 51.45 o 11 10 0 88.72 23.50 90.89 o -10 11 0 8.87 -25.72 32.58 o -9 11 0 52.72 68.60 44.59 o -8 11 0 26.94 15.29 27.81 o -7 11 0 63.14 39.44 61.74 o -6 11 0 269.45 232.35 70.31 o -5 11 0 70.92 40.78 21.43 o -4 11 0 10.80 0.13 18.81 o -3 11 0 223.26 212.46 27.78 o -2 11 0 213.23 173.81 27.10 o -1 11 0 474.28 514.83 40.24 o 0 11 0 10.46 23.68 49.73 o 1 11 0 392.60 328.75 34.04 o 2 11 0 239.66 287.39 56.59 o 3 11 0 225.97 199.89 27.90 o 4 11 0 11.92 29.78 30.87 o 5 11 0 79.29 38.54 30.64 o 6 11 0 238.81 188.98 80.60 o 7 11 0 56.98 100.27 34.04 o 8 11 0 32.41 28.81 45.66 o 9 11 0 57.58 47.45 39.88 o 10 11 0 8.53 91.22 50.59 o -9 12 0 25.42 21.84 42.73 o -8 12 0 52.40 58.31 82.32 o -7 12 0 126.00 159.49 42.87 o -6 12 0 20.55 -1.20 43.73 o -5 12 0 436.45 425.20 39.01 o -4 12 0 300.93 301.21 28.81 o -3 12 0 302.60 233.31 33.33 o -2 12 0 82.36 72.71 24.16 o -1 12 0 430.94 480.23 52.14 o 0 12 0 71.18 93.34 30.01 o 1 12 0 354.98 352.98 41.26 o 2 12 0 73.47 81.30 22.38 o 3 12 0 336.58 312.99 33.89 o 4 12 0 256.08 239.98 66.88 o 5 12 0 396.67 371.32 40.55 o 6 12 0 17.82 4.78 33.20 o 7 12 0 153.08 190.17 38.03 o 8 12 0 56.43 7.93 74.60 o 9 12 0 30.67 38.65 40.91 o -8 13 0 38.66 1.19 44.38 o -7 13 0 64.83 30.87 46.30 o -6 13 0 319.35 262.38 51.45 o -5 13 0 27.80 14.45 35.05 o -4 13 0 16.74 -25.64 25.64 o -3 13 0 73.04 56.34 31.09 o -2 13 0 93.56 124.12 37.85 o -1 13 0 183.82 197.53 37.73 o 0 13 0 186.24 239.46 35.12 o 1 13 0 210.34 235.78 32.88 o 2 13 0 77.77 57.16 27.91 o 3 13 0 70.00 35.05 39.02 o 4 13 0 17.78 46.30 35.28 o 5 13 0 33.23 7.38 37.73 o 6 13 0 354.88 318.02 43.64 o 7 13 0 53.41 -19.49 40.44 o 8 13 0 46.96 115.58 114.04 o -7 14 0 108.48 229.80 73.74 o -6 14 0 77.48 198.93 48.02 o -5 14 0 99.35 51.52 45.65 o -4 14 0 193.59 126.90 44.59 o -3 14 0 119.24 106.79 33.33 o -2 14 0 96.58 37.73 77.17 o -1 14 0 45.40 -4.48 87.46 o 0 14 0 147.15 165.24 52.20 o 1 14 0 38.50 93.34 32.93 o 2 14 0 115.80 146.12 44.59 o 3 14 0 120.33 115.91 37.67 o 4 14 0 234.89 112.53 60.02 o 5 14 0 113.77 37.37 42.76 o 6 14 0 63.79 40.08 53.16 o 7 14 0 115.91 111.22 48.83 o -4 15 0 124.10 89.51 55.60 o -3 15 0 41.76 -8.65 52.33 o -2 15 0 28.37 5.20 52.74 o -1 15 0 111.24 119.68 73.74 o 0 15 0 57.88 25.12 92.61 o 1 15 0 123.26 36.10 102.90 o 2 15 0 27.86 84.79 42.34 o 3 15 0 47.34 74.84 75.46 o 4 15 0 121.19 34.71 48.61 o -4 -15 1 276.47 239.78 80.72 o -3 -15 1 181.36 128.05 44.92 o -2 -15 1 636.34 453.68 62.57 o -1 -15 1 280.70 365.28 89.18 o 0 -15 1 127.02 8.96 53.16 o 1 -15 1 90.44 54.50 65.17 o 2 -15 1 41.00 56.49 49.17 o 3 -15 1 144.95 126.98 86.60 o 4 -15 1 58.78 3.43 80.60 o -7 -14 1 315.16 425.07 89.12 o -6 -14 1 241.77 119.47 63.45 o -5 -14 1 441.67 469.82 58.42 o -4 -14 1 439.02 332.84 102.04 o -3 -14 1 485.80 444.78 49.65 o -2 -14 1 76.38 88.14 34.42 o -1 -14 1 395.28 393.75 48.93 o 0 -14 1 86.08 96.73 46.63 o 1 -14 1 108.64 130.64 50.54 o 2 -14 1 280.84 288.49 41.86 o 3 -14 1 177.03 194.25 42.19 o 4 -14 1 239.81 217.37 40.92 o 5 -14 1 167.26 265.81 53.16 o 6 -14 1 132.43 72.03 48.02 o -8 -13 1 183.19 131.95 47.23 o -7 -13 1 806.51 587.86 61.30 o -6 -13 1 240.78 230.08 41.41 o -5 -13 1 280.91 283.40 96.04 o -4 -13 1 963.26 907.67 84.03 o -3 -13 1 484.00 500.42 48.61 o -2 -13 1 1247.68 1333.05 72.03 o -1 -13 1 548.39 657.18 54.39 o 0 -13 1 885.03 948.75 89.12 o 1 -13 1 1261.62 1360.76 73.30 o 2 -13 1 381.95 407.61 95.18 o 3 -13 1 456.93 475.81 42.85 o 4 -13 1 405.95 538.27 57.60 o 5 -13 1 336.27 289.22 48.29 o 6 -13 1 579.89 703.12 75.46 o 7 -13 1 108.90 41.16 41.16 o 8 -13 1 206.10 125.19 56.59 o -10 -12 1 433.78 397.86 61.74 o -9 -12 1 195.00 125.11 63.45 o -8 -12 1 590.38 475.47 54.02 o -7 -12 1 337.97 296.05 43.51 o -6 -12 1 1178.80 1113.87 205.79 o -5 -12 1 1841.08 2134.84 142.28 o -4 -12 1 244.03 208.53 39.03 o -3 -12 1 1536.99 1628.14 83.30 o -2 -12 1 715.84 718.70 41.98 o -1 -12 1 791.73 819.73 60.16 o 0 -12 1 3066.75 3531.01 209.76 o 1 -12 1 855.34 723.02 132.05 o 2 -12 1 3768.14 4064.13 186.22 o 3 -12 1 921.71 971.99 59.73 o 4 -12 1 938.70 1140.43 139.77 o 5 -12 1 831.17 928.65 63.45 o 6 -12 1 333.28 311.63 43.63 o 7 -12 1 752.12 770.00 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