#------------------------------------------------------------------------------ #$Date: 2016-04-02 23:02:37 +0300 (Sat, 02 Apr 2016) $ #$Revision: 180909 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/10/50/2105004.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_2105004_Fobs loop_ _publ_author_name 'Siegler, Maxime A.' 'Hao, Xiang' 'Parkin, Sean' 'Brock, Carolyn Pratt' _publ_section_title ; [Ni(H~2~O)~6~](NO~3~)~2~·(15-crown-5)·2H~2~O: three phase transitions and an intermediate modulated phase stable over a range of ca 40K ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 486 _journal_page_last 498 _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 101.470 _cell_angle_gamma 90.000 _cell_length_a 12.0240 _cell_length_b 12.6780 _cell_length_c 16.0160 _exptl_crystal_F_000 1160.00 _reflns_d_resolution_high 0.7698 _cod_data_source_file hw5018150K_IVsup12.hkl _cod_data_source_block 150K_IV #BEGIN Tags that were not found in dictionaries: _shelx_title ' k06183 in P2(1)/c' _shelx_refln_list_code 4 _shelx_f_calc_maximum 353.65 _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 0 726.32 731.96 11.37 o 2 0 0 18785.16 18033.10 286.42 o 3 0 0 19.98 9.09 4.55 o 4 0 0 5753.32 6119.39 88.65 o 5 0 0 1001.55 1113.86 22.73 o 6 0 0 54089.30 57534.07 809.25 o 7 0 0 8.33 29.55 11.37 o 8 0 0 7362.51 7651.51 147.76 o 9 0 0 1281.29 1307.08 50.01 o 10 0 0 2748.11 3146.07 95.47 o 11 0 0 13.01 9.09 20.46 o 12 0 0 327.22 270.51 36.37 o 13 0 0 97.44 138.66 36.37 o 14 0 0 448.30 443.27 63.65 o 15 0 0 681.36 797.88 122.75 o 1 1 0 27133.20 24326.55 347.46 o 2 1 0 27.15 23.92 1.61 o 3 1 0 4558.12 4474.21 49.75 o 4 1 0 372.62 368.12 8.73 o 5 1 0 5894.68 5688.59 62.63 o 6 1 0 2835.53 2727.90 32.92 o 7 1 0 4424.26 4262.34 54.58 o 8 1 0 4810.84 5259.32 73.89 o 9 1 0 3490.55 3619.82 64.73 o 10 1 0 181.67 128.19 34.10 o 11 1 0 971.29 1044.23 38.18 o 12 1 0 575.93 604.02 32.92 o 13 1 0 32.38 33.51 21.65 o 14 1 0 3.21 0.76 26.49 o 15 1 0 165.32 142.07 53.04 o 0 2 0 55448.40 49755.27 1550.31 o 1 2 0 52.20 52.75 2.03 o 2 2 0 473.75 421.14 15.91 o 3 2 0 302.30 302.35 6.43 o 4 2 0 7185.67 7372.09 76.95 o 5 2 0 980.75 963.96 16.07 o 6 2 0 7395.08 7546.46 86.75 o 7 2 0 2.43 6.82 8.04 o 8 2 0 2195.38 2364.59 40.18 o 9 2 0 1069.08 1100.02 47.74 o 10 2 0 1862.58 1990.22 51.14 o 11 2 0 644.75 621.67 50.01 o 12 2 0 494.00 411.72 32.22 o 13 2 0 231.12 202.31 28.40 o 14 2 0 340.52 248.15 40.18 o 15 2 0 306.37 222.33 61.87 o 1 3 0 326.06 346.58 7.10 o 2 3 0 138.51 131.88 4.82 o 3 3 0 51301.35 48680.57 519.33 o 4 3 0 12107.11 12901.43 131.80 o 5 3 0 16418.05 16279.43 169.30 o 6 3 0 1160.83 1102.57 19.29 o 7 3 0 2807.62 2913.47 42.39 o 8 3 0 2780.75 3012.51 53.04 o 9 3 0 1803.01 1853.75 50.01 o 10 3 0 1793.87 1696.05 50.16 o 11 3 0 2528.73 2741.91 113.66 o 12 3 0 216.58 158.26 29.41 o 13 3 0 774.36 704.86 47.74 o 14 3 0 168.15 190.57 42.03 o 15 3 0 122.41 141.66 110.25 o 0 4 0 2444.45 2268.45 36.86 o 1 4 0 9.03 10.46 3.78 o 2 4 0 44717.39 44708.20 551.25 o 3 4 0 1093.61 1145.68 16.82 o 4 4 0 27653.63 28726.50 290.31 o 5 4 0 9320.41 10227.40 106.05 o 6 4 0 3035.37 3059.74 41.79 o 7 4 0 41.98 30.14 7.57 o 8 4 0 1857.44 2112.12 78.42 o 9 4 0 22.42 12.02 9.94 o 10 4 0 712.58 683.95 33.30 o 11 4 0 2173.70 2409.05 127.30 o 12 4 0 1479.81 1479.16 69.33 o 13 4 0 368.81 311.85 33.64 o 14 4 0 484.39 449.87 88.65 o 1 5 0 1641.83 1637.70 21.65 o 2 5 0 38.43 37.54 4.82 o 3 5 0 4006.73 3806.49 41.79 o 4 5 0 6373.51 6810.03 70.51 o 5 5 0 5916.46 6026.68 68.30 o 6 5 0 45.82 13.39 7.96 o 7 5 0 1880.53 2107.18 80.70 o 8 5 0 546.52 490.60 29.55 o 9 5 0 268.79 239.07 15.49 o 10 5 0 2153.73 2155.25 81.83 o 11 5 0 1106.45 1048.88 47.91 o 12 5 0 23.32 28.19 22.70 o 13 5 0 531.38 428.57 59.10 o 14 5 0 560.21 558.72 97.75 o 0 6 0 6475.36 6491.99 159.12 o 1 6 0 898.94 931.86 36.37 o 2 6 0 28507.41 29616.29 394.40 o 3 6 0 1165.93 1245.70 30.69 o 4 6 0 9364.44 9763.26 116.46 o 5 6 0 770.27 753.25 25.00 o 6 6 0 4847.55 5097.53 69.91 o 7 6 0 75.61 59.89 9.25 o 8 6 0 1154.56 1209.02 35.23 o 9 6 0 173.33 91.03 31.82 o 10 6 0 692.77 714.41 106.84 o 11 6 0 1292.38 1390.66 97.75 o 12 6 0 692.12 634.00 44.12 o 13 6 0 312.75 235.97 81.83 o 14 6 0 84.82 40.92 41.99 o 1 7 0 12978.92 13854.11 279.60 o 2 7 0 14.04 11.04 5.68 o 3 7 0 4141.83 4160.18 53.53 o 4 7 0 277.88 244.72 18.19 o 5 7 0 7864.28 8431.27 122.64 o 6 7 0 33.64 25.18 12.50 o 7 7 0 4342.32 4781.27 83.83 o 8 7 0 261.02 203.12 20.16 o 9 7 0 682.84 609.70 92.06 o 10 7 0 989.58 996.16 51.03 o 11 7 0 1236.17 1366.16 57.61 o 12 7 0 4.96 -13.53 33.21 o 13 7 0 70.46 89.47 40.09 o 0 8 0 6621.51 6792.12 167.08 o 1 8 0 97.81 82.15 10.91 o 2 8 0 1900.03 1807.70 28.56 o 3 8 0 889.42 943.01 34.10 o 4 8 0 87.45 101.95 9.64 o 5 8 0 496.57 513.41 16.82 o 6 8 0 1311.01 1406.95 33.64 o 7 8 0 1663.43 1708.93 44.01 o 8 8 0 526.80 476.99 32.34 o 9 8 0 997.93 916.79 46.91 o 10 8 0 932.28 869.64 62.51 o 11 8 0 200.33 170.59 44.33 o 12 8 0 3.61 -32.92 40.09 o 13 8 0 237.39 276.57 54.05 o 1 9 0 4977.29 5238.67 147.76 o 2 9 0 932.70 938.97 21.34 o 3 9 0 28.50 17.43 8.13 o 4 9 0 714.23 779.12 19.59 o 5 9 0 356.67 432.49 17.54 o 6 9 0 799.60 788.50 31.31 o 7 9 0 1504.23 1509.43 61.38 o 8 9 0 1553.01 1505.50 53.70 o 9 9 0 1258.00 1212.88 72.74 o 10 9 0 594.30 441.62 51.22 o 11 9 0 181.79 117.61 67.06 o 12 9 0 3.56 -42.57 42.57 o 0 10 0 9135.10 9394.79 209.97 o 1 10 0 104.14 78.90 14.23 o 2 10 0 458.23 464.98 30.69 o 3 10 0 48.13 51.11 8.44 o 4 10 0 156.62 159.18 44.33 o 5 10 0 32.13 3.46 16.82 o 6 10 0 1986.51 1919.51 61.74 o 7 10 0 714.08 698.37 34.87 o 8 10 0 520.48 472.03 40.33 o 9 10 0 408.27 378.96 52.07 o 10 10 0 612.69 634.03 122.75 o 11 10 0 11.24 -18.82 47.44 o 12 10 0 38.53 -17.05 48.22 o 1 11 0 2045.05 2179.98 61.38 o 2 11 0 215.88 152.29 23.87 o 3 11 0 142.27 132.46 32.96 o 4 11 0 44.26 27.28 22.73 o 5 11 0 1404.83 1493.74 51.36 o 6 11 0 161.57 126.20 23.95 o 7 11 0 278.71 275.25 44.18 o 8 11 0 31.41 27.23 34.53 o 9 11 0 154.01 218.44 95.47 o 10 11 0 160.16 91.87 60.63 o 11 11 0 65.10 14.47 52.97 o 0 12 0 461.94 456.27 46.24 o 1 12 0 128.83 72.29 22.70 o 2 12 0 512.71 430.26 38.64 o 3 12 0 36.96 58.03 26.76 o 4 12 0 2173.61 2163.60 79.94 o 5 12 0 431.81 421.96 37.00 o 6 12 0 338.24 326.81 78.42 o 7 12 0 81.32 77.43 49.75 o 8 12 0 22.33 16.75 59.10 o 9 12 0 105.78 103.81 50.46 o 10 12 0 50.76 53.37 67.77 o 1 13 0 1358.29 1517.31 142.07 o 2 13 0 202.35 187.77 32.34 o 3 13 0 2182.58 2241.75 248.91 o 4 13 0 305.20 245.42 86.38 o 5 13 0 1707.32 1845.59 365.98 o 6 13 0 23.58 -40.93 40.93 o 7 13 0 137.36 80.56 56.83 o 8 13 0 0.68 49.47 47.40 o 9 13 0 111.79 127.30 59.88 o 0 14 0 111.98 79.24 38.19 o 1 14 0 42.70 44.04 35.09 o 2 14 0 221.43 149.82 34.05 o 3 14 0 199.61 204.67 42.89 o 4 14 0 612.80 501.08 51.40 o 5 14 0 59.94 71.61 57.97 o 6 14 0 36.39 13.09 62.61 o 7 14 0 6.44 9.49 50.16 o 8 14 0 114.60 55.69 55.98 o 1 15 0 4.58 20.38 42.34 o 2 15 0 23.61 -43.64 43.64 o 3 15 0 19.88 39.92 38.66 o 4 15 0 132.82 159.62 85.24 o 5 15 0 8.85 -26.19 59.54 o 6 15 0 33.45 33.17 72.81 o 0 16 0 369.93 125.78 65.06 o 1 16 0 32.41 11.57 52.39 o 2 16 0 95.69 88.15 78.42 o 3 16 0 6.62 134.20 78.66 o -15 1 1 18.36 52.99 50.24 o -14 1 1 0.06 44.58 32.22 o -13 1 1 161.66 158.69 37.51 o -12 1 1 7.44 -7.27 20.04 o -11 1 1 4.47 1.25 21.60 o -10 1 1 340.79 354.31 20.04 o -9 1 1 4.92 -6.82 9.64 o -8 1 1 1.08 -1.14 11.25 o -7 1 1 124.59 111.64 12.50 o -6 1 1 2287.69 2527.42 67.06 o -5 1 1 64.83 66.83 7.10 o -4 1 1 837.47 832.78 13.04 o -3 1 1 50.62 35.62 3.78 o -2 1 1 0.42 0.00 3.41 o -1 1 1 150.75 145.63 4.55 o 0 1 1 249.76 230.73 3.21 o 1 1 1 95.04 93.42 5.68 o 2 1 1 47.23 41.39 2.03 o 3 1 1 798.88 838.96 11.98 o 4 1 1 163.27 156.76 6.82 o 5 1 1 124.34 131.84 6.43 o 6 1 1 24.84 25.00 10.23 o 7 1 1 0.10 -1.52 7.10 o 8 1 1 242.10 205.60 13.59 o 9 1 1 2265.87 2440.68 50.76 o 10 1 1 22.56 56.26 18.50 o 11 1 1 180.56 135.18 21.65 o 12 1 1 26.20 18.19 40.92 o 13 1 1 49.66 52.83 26.49 o 14 1 1 0.46 -0.58 40.40 o 15 1 1 191.27 221.29 69.06 o -15 2 1 79.87 83.18 48.78 o -14 2 1 8.56 -13.24 31.82 o -13 2 1 160.82 159.82 30.04 o -12 2 1 21.98 13.23 15.79 o -11 2 1 79.45 40.16 16.82 o -10 2 1 365.07 315.69 25.00 o -9 2 1 772.49 833.65 34.10 o -8 2 1 123.73 99.65 13.64 o -7 2 1 844.72 880.24 22.73 o -6 2 1 1589.35 1718.24 25.57 o -5 2 1 44.37 35.64 5.46 o -4 2 1 2.31 -0.91 4.55 o -3 2 1 1024.45 949.07 11.98 o -2 2 1 46.57 37.37 2.27 o -1 2 1 106.82 102.29 3.21 o 0 2 1 769.94 721.53 8.73 o 1 2 1 51.95 51.07 3.41 o 2 2 1 945.47 910.45 12.56 o 3 2 1 129.52 109.82 3.78 o 4 2 1 39.42 40.99 3.78 o 5 2 1 301.90 367.53 9.25 o 6 2 1 1.58 1.95 5.46 o 7 2 1 465.21 453.31 17.05 o 8 2 1 370.50 356.34 18.02 o 9 2 1 2.30 3.21 13.04 o 10 2 1 746.71 782.53 32.73 o 11 2 1 40.27 14.64 19.66 o 12 2 1 4.45 7.65 35.23 o 13 2 1 49.82 50.07 29.86 o 14 2 1 13.52 31.65 40.33 o 15 2 1 6.66 107.56 60.51 o -15 3 1 95.28 138.46 49.55 o -14 3 1 28.11 20.16 28.56 o -13 3 1 380.53 299.32 71.61 o -12 3 1 109.89 62.94 32.96 o -11 3 1 245.67 185.34 37.51 o -10 3 1 140.41 104.04 17.21 o -9 3 1 129.95 139.69 15.21 o -8 3 1 119.72 96.65 14.78 o -7 3 1 515.96 549.32 16.82 o -6 3 1 139.84 154.84 14.78 o -5 3 1 302.64 329.72 10.36 o -4 3 1 1090.74 1030.92 16.07 o -3 3 1 168.53 118.93 14.78 o -2 3 1 360.48 361.93 9.09 o -1 3 1 410.74 442.80 7.96 o 0 3 1 644.18 619.09 17.05 o 1 3 1 468.18 420.51 21.60 o 2 3 1 3368.03 3343.29 39.84 o 3 3 1 0.54 1.14 3.21 o 4 3 1 825.63 843.74 18.19 o 5 3 1 819.80 813.01 21.60 o 6 3 1 49.50 57.87 6.10 o 7 3 1 9.86 -0.76 6.10 o 8 3 1 281.73 257.00 14.78 o 9 3 1 79.60 45.80 11.97 o 10 3 1 489.46 425.07 24.39 o 11 3 1 492.60 395.79 27.75 o 12 3 1 67.18 65.72 24.78 o 13 3 1 103.39 66.04 30.58 o 14 3 1 16.03 19.67 39.36 o -14 4 1 57.68 32.57 44.18 o -13 4 1 319.74 269.80 35.74 o -12 4 1 181.49 155.08 63.65 o -11 4 1 1521.45 1631.78 52.97 o -10 4 1 441.72 363.67 22.33 o -9 4 1 318.27 309.90 18.50 o -8 4 1 149.79 122.63 11.98 o -7 4 1 119.63 125.87 12.56 o -6 4 1 9.05 12.63 9.09 o -5 4 1 1956.04 2050.97 34.10 o -4 4 1 60.48 48.47 5.46 o -3 4 1 1949.93 1855.62 21.65 o -2 4 1 1785.75 1739.27 20.71 o -1 4 1 19.40 17.73 3.41 o 0 4 1 10.42 7.73 3.78 o 1 4 1 812.96 818.40 20.46 o 2 4 1 3791.28 3808.78 45.01 o 3 4 1 1026.21 1019.78 15.83 o 4 4 1 3129.29 3337.24 39.32 o 5 4 1 348.38 325.43 10.36 o 6 4 1 1902.95 1974.48 30.41 o 7 4 1 871.22 936.49 18.91 o 8 4 1 61.01 36.50 13.59 o 9 4 1 380.47 319.76 23.95 o 10 4 1 129.98 122.32 20.04 o 11 4 1 113.10 80.47 22.70 o 12 4 1 284.13 290.17 34.93 o 13 4 1 1.28 -6.57 29.70 o 14 4 1 8.76 74.10 41.70 o -14 5 1 333.59 258.52 61.38 o -13 5 1 9.39 4.32 32.92 o -12 5 1 22.37 33.43 27.18 o -11 5 1 2.49 -2.91 24.39 o -10 5 1 476.10 418.93 34.35 o -9 5 1 341.29 331.15 30.69 o -8 5 1 1874.12 1984.84 105.70 o -7 5 1 108.72 95.00 11.35 o -6 5 1 72.37 49.56 14.78 o -5 5 1 4.25 1.30 5.46 o -4 5 1 2624.81 2811.32 32.92 o -3 5 1 148.25 136.51 7.10 o -2 5 1 2706.29 2822.15 40.92 o -1 5 1 252.30 237.60 6.43 o 0 5 1 459.85 417.13 11.37 o 1 5 1 233.91 205.96 7.10 o 2 5 1 5019.54 5116.24 103.43 o 3 5 1 1135.21 1187.71 31.82 o 4 5 1 4786.39 5317.41 156.85 o 5 5 1 9.67 6.49 5.46 o 6 5 1 141.73 120.53 9.25 o 7 5 1 107.07 82.22 15.83 o 8 5 1 829.71 865.35 79.56 o 9 5 1 906.74 899.87 36.04 o 10 5 1 38.96 34.70 21.64 o 11 5 1 1.65 -11.23 26.49 o 12 5 1 34.65 -18.19 47.74 o 13 5 1 405.82 351.72 40.96 o 14 5 1 14.18 6.82 41.79 o -14 6 1 52.78 25.52 41.49 o -13 6 1 101.30 62.74 35.93 o -12 6 1 685.47 660.54 44.66 o -11 6 1 615.30 605.88 43.56 o -10 6 1 120.91 121.80 57.97 o -9 6 1 5.83 -4.55 11.70 o -8 6 1 42.30 5.91 11.35 o -7 6 1 96.87 74.38 18.19 o -6 6 1 259.58 231.18 11.25 o -5 6 1 6753.93 7521.78 109.11 o -4 6 1 408.98 458.63 12.56 o -3 6 1 230.97 171.12 7.57 o -2 6 1 3100.79 3237.43 90.93 o -1 6 1 752.69 713.70 11.98 o 0 6 1 267.21 301.40 8.73 o 1 6 1 1706.42 1742.18 45.46 o 2 6 1 2372.70 2468.55 31.31 o 3 6 1 694.64 662.41 17.05 o 4 6 1 2270.29 2332.40 37.75 o 5 6 1 1111.63 1127.73 22.33 o 6 6 1 232.92 216.79 22.73 o 7 6 1 30.12 26.19 6.27 o 8 6 1 101.24 48.83 20.04 o 9 6 1 1278.29 1249.27 78.42 o 10 6 1 1807.74 1893.71 63.90 o 11 6 1 154.07 118.64 35.23 o 12 6 1 72.37 48.16 30.04 o 13 6 1 8.10 -42.03 42.03 o 14 6 1 45.50 22.67 55.98 o -13 7 1 63.39 77.86 44.33 o -12 7 1 12.80 10.17 30.41 o -11 7 1 0.64 -31.34 31.34 o -10 7 1 47.26 45.51 46.60 o -9 7 1 288.13 307.88 28.09 o -8 7 1 2639.08 2894.41 146.62 o -7 7 1 2039.23 2222.42 48.14 o -6 7 1 93.67 63.65 10.36 o -5 7 1 814.01 775.15 19.66 o -4 7 1 22.91 19.70 6.10 o -3 7 1 223.47 218.59 10.36 o -2 7 1 5996.72 6310.76 115.93 o -1 7 1 914.72 952.28 17.05 o 0 7 1 1052.89 966.10 17.46 o 1 7 1 849.93 812.18 22.73 o 2 7 1 893.46 890.13 14.01 o 3 7 1 216.65 244.87 11.98 o 4 7 1 1671.15 1789.06 33.75 o 5 7 1 613.96 583.07 17.68 o 6 7 1 53.08 20.65 19.32 o 7 7 1 1172.51 1204.49 32.03 o 8 7 1 102.73 98.93 28.41 o 9 7 1 9.81 15.34 20.46 o 10 7 1 29.80 41.22 27.18 o 11 7 1 243.67 159.73 32.22 o 12 7 1 56.41 87.34 40.33 o 13 7 1 207.38 105.00 47.74 o -13 8 1 3.61 -1.77 46.42 o -12 8 1 215.67 266.15 75.01 o -11 8 1 546.86 435.47 44.01 o -10 8 1 157.89 69.65 61.38 o -9 8 1 697.04 615.73 60.24 o -8 8 1 848.68 900.20 33.64 o -7 8 1 10.60 3.64 21.60 o -6 8 1 196.36 175.67 17.05 o -5 8 1 778.90 834.34 21.82 o -4 8 1 108.90 93.98 9.25 o -3 8 1 268.95 285.81 12.56 o -2 8 1 181.43 179.58 9.25 o -1 8 1 1308.79 1309.73 28.41 o 0 8 1 2020.41 2184.36 31.96 o 1 8 1 318.89 298.39 11.70 o 2 8 1 2277.39 2457.36 31.82 o 3 8 1 123.04 92.43 14.78 o 4 8 1 595.35 607.18 20.71 o 5 8 1 494.74 550.18 21.65 o 6 8 1 1206.98 1185.01 34.53 o 7 8 1 16.15 14.40 11.98 o 8 8 1 2196.25 2411.83 65.18 o 9 8 1 323.44 327.68 32.22 o 10 8 1 1593.13 1771.01 153.44 o 11 8 1 78.29 70.86 33.62 o 12 8 1 104.92 79.09 38.18 o 13 8 1 15.19 -26.42 49.01 o -12 9 1 4.59 -7.28 39.36 o -11 9 1 24.59 22.57 38.64 o -10 9 1 231.08 249.92 77.29 o -9 9 1 56.72 74.56 26.48 o -8 9 1 855.96 952.28 39.32 o -7 9 1 30.87 40.11 13.59 o -6 9 1 420.97 373.56 19.32 o -5 9 1 374.97 330.50 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