#------------------------------------------------------------------------------ #$Date: 2016-04-02 23:02:37 +0300 (Sat, 02 Apr 2016) $ #$Revision: 180909 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/10/50/2105002.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_2105002_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 101.520 _cell_angle_gamma 90.000 _cell_length_a 11.9950 _cell_length_b 12.6850 _cell_length_c 16.0050 _exptl_crystal_F_000 1160.00 _reflns_d_resolution_high 0.7702 _cod_data_source_file hw5018130K_IVsup10.hkl _cod_data_source_block 130K_IV #BEGIN Tags that were not found in dictionaries: _shelx_title ' k06181 in P2(1)/c' _shelx_refln_list_code 4 _shelx_f_calc_maximum 353.88 _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 0 760.38 754.02 10.65 o 2 0 0 18888.59 17853.63 261.99 o 3 0 0 26.18 17.04 4.26 o 4 0 0 6074.75 6245.15 91.59 o 5 0 0 963.37 1118.25 23.43 o 6 0 0 55796.18 57407.66 892.47 o 7 0 0 3.80 12.78 8.52 o 8 0 0 7403.82 7638.17 151.23 o 9 0 0 1334.89 1399.41 48.99 o 10 0 0 2960.45 3316.40 108.63 o 11 0 0 14.46 -8.52 19.17 o 12 0 0 359.70 381.27 36.21 o 13 0 0 64.89 115.02 34.08 o 14 0 0 545.12 517.59 80.94 o 15 0 0 989.68 1028.79 117.15 o 1 1 0 26755.43 24000.54 280.82 o 2 1 0 23.41 19.17 1.51 o 3 1 0 4620.19 4420.85 46.40 o 4 1 0 355.17 334.42 7.53 o 5 1 0 6156.12 5878.90 60.98 o 6 1 0 3301.80 3115.96 39.07 o 7 1 0 4370.49 4261.03 59.48 o 8 1 0 5480.76 5740.94 82.07 o 9 1 0 3677.91 3637.70 65.81 o 10 1 0 211.89 136.67 15.06 o 11 1 0 1084.39 1139.57 38.21 o 12 1 0 737.60 812.05 39.34 o 13 1 0 31.51 27.80 29.67 o 14 1 0 8.43 28.12 34.50 o 15 1 0 166.88 184.73 83.07 o 0 2 0 55584.50 51982.57 1833.93 o 1 2 0 62.28 66.10 3.01 o 2 2 0 486.89 434.04 15.97 o 3 2 0 322.08 309.68 6.65 o 4 2 0 6996.42 7095.85 77.78 o 5 2 0 983.38 932.09 14.84 o 6 2 0 7355.96 7372.73 108.63 o 7 2 0 2.52 -1.66 6.65 o 8 2 0 2040.02 2187.23 40.91 o 9 2 0 1153.70 1180.80 30.67 o 10 2 0 1817.20 1859.11 48.10 o 11 2 0 730.91 724.66 35.78 o 12 2 0 444.92 391.64 33.01 o 13 2 0 222.94 136.32 38.38 o 14 2 0 353.24 387.31 124.60 o 15 2 0 398.33 372.75 65.50 o 1 3 0 323.54 350.16 6.65 o 2 3 0 171.77 156.26 5.11 o 3 3 0 51674.95 48841.67 504.82 o 4 3 0 13055.86 13896.23 149.81 o 5 3 0 16461.57 16169.48 177.41 o 6 3 0 1211.56 1208.08 19.96 o 7 3 0 3122.18 3165.98 63.90 o 8 3 0 3179.23 3395.88 50.94 o 9 3 0 2053.44 2087.32 42.91 o 10 3 0 2204.33 2169.54 53.22 o 11 3 0 2739.90 2881.59 73.39 o 12 3 0 281.36 233.12 26.76 o 13 3 0 854.90 879.53 54.22 o 14 3 0 235.81 188.17 50.44 o 15 3 0 141.08 128.65 55.75 o 0 4 0 2477.38 2299.13 40.42 o 1 4 0 9.88 6.39 3.01 o 2 4 0 45536.78 45339.48 492.87 o 3 4 0 1198.56 1215.57 22.36 o 4 4 0 28118.56 29075.57 287.76 o 5 4 0 9657.63 10601.00 114.35 o 6 4 0 3156.09 2999.65 43.50 o 7 4 0 46.92 36.21 6.65 o 8 4 0 1819.37 2021.67 38.34 o 9 4 0 23.17 25.56 10.54 o 10 4 0 754.70 814.82 53.25 o 11 4 0 2393.97 2536.06 69.33 o 12 4 0 1589.24 1727.15 108.63 o 13 4 0 465.24 434.05 68.16 o 14 4 0 549.69 412.37 144.84 o 1 5 0 1636.81 1674.35 39.40 o 2 5 0 42.52 39.70 5.11 o 3 5 0 4070.56 3833.20 44.26 o 4 5 0 6984.54 7362.14 77.78 o 5 5 0 5736.69 5656.18 68.84 o 6 5 0 34.60 22.25 6.65 o 7 5 0 1916.12 2082.32 34.80 o 8 5 0 603.60 608.92 24.49 o 9 5 0 295.91 260.49 15.06 o 10 5 0 2574.59 2723.15 61.26 o 11 5 0 1181.46 1096.38 68.16 o 12 5 0 33.22 39.29 26.61 o 13 5 0 541.22 509.53 83.07 o 14 5 0 716.56 738.39 92.65 o 0 6 0 6352.16 6468.02 168.27 o 1 6 0 902.39 894.66 20.23 o 2 6 0 28967.52 30111.22 326.95 o 3 6 0 1190.26 1264.92 20.92 o 4 6 0 9697.06 9858.76 141.64 o 5 6 0 810.01 836.34 24.49 o 6 6 0 5092.80 5335.98 85.20 o 7 6 0 62.06 52.28 9.31 o 8 6 0 1089.86 1150.28 30.31 o 9 6 0 192.07 148.66 17.33 o 10 6 0 757.14 821.12 51.12 o 11 6 0 1434.33 1505.49 53.32 o 12 6 0 755.48 752.45 68.16 o 13 6 0 410.67 342.23 46.88 o 14 6 0 78.91 58.60 141.64 o 1 7 0 13633.34 14570.88 282.22 o 2 7 0 11.82 17.04 9.58 o 3 7 0 4477.57 4453.30 63.90 o 4 7 0 329.54 297.81 11.43 o 5 7 0 8356.00 8829.95 160.81 o 6 7 0 42.76 36.25 9.53 o 7 7 0 4804.55 5019.50 87.80 o 8 7 0 318.12 328.39 29.82 o 9 7 0 793.96 760.24 30.67 o 10 7 0 1157.72 1237.97 49.63 o 11 7 0 1431.37 1623.13 94.78 o 12 7 0 5.25 -2.51 36.64 o 13 7 0 84.30 10.65 59.88 o 0 8 0 6800.53 7091.42 129.24 o 1 8 0 108.07 86.65 11.71 o 2 8 0 1896.71 1858.96 29.59 o 3 8 0 908.86 977.85 20.75 o 4 8 0 86.45 83.46 8.14 o 5 8 0 490.20 501.55 16.71 o 6 8 0 1396.49 1441.43 50.05 o 7 8 0 1864.79 2017.91 48.01 o 8 8 0 521.74 441.99 41.53 o 9 8 0 1145.95 1108.39 52.67 o 10 8 0 913.73 1003.67 49.63 o 11 8 0 214.95 181.92 40.42 o 12 8 0 4.04 7.40 40.58 o 13 8 0 303.86 410.55 64.88 o 1 9 0 5241.84 5604.10 110.76 o 2 9 0 993.30 1034.72 23.22 o 3 9 0 37.69 31.41 11.71 o 4 9 0 763.52 787.28 54.31 o 5 9 0 363.70 367.18 12.29 o 6 9 0 887.76 846.58 27.02 o 7 9 0 1580.71 1554.88 54.16 o 8 9 0 1743.43 1702.60 51.95 o 9 9 0 1347.57 1473.08 84.13 o 10 9 0 676.27 542.48 39.72 o 11 9 0 197.50 160.40 37.03 o 12 9 0 4.92 -17.63 58.91 o 0 10 0 9500.93 9778.95 223.81 o 1 10 0 112.85 88.00 10.63 o 2 10 0 424.94 417.16 27.69 o 3 10 0 53.88 34.51 17.72 o 4 10 0 180.93 166.05 38.34 o 5 10 0 57.51 46.86 17.72 o 6 10 0 2049.19 2041.70 63.46 o 7 10 0 828.73 861.53 44.73 o 8 10 0 569.45 487.97 80.94 o 9 10 0 500.25 450.62 92.65 o 10 10 0 690.19 648.03 88.39 o 11 10 0 23.36 37.42 70.11 o 12 10 0 42.39 -13.50 56.81 o 1 11 0 2431.04 2544.99 60.98 o 2 11 0 213.53 178.37 19.67 o 3 11 0 152.90 142.71 20.28 o 4 11 0 45.31 49.33 16.71 o 5 11 0 1561.12 1564.63 52.25 o 6 11 0 186.67 129.04 25.16 o 7 11 0 299.18 212.30 37.86 o 8 11 0 33.75 28.32 33.49 o 9 11 0 194.84 92.65 43.68 o 10 11 0 201.65 206.03 57.27 o 11 11 0 75.07 100.86 79.87 o 0 12 0 460.03 387.20 60.70 o 1 12 0 145.70 111.79 35.14 o 2 12 0 470.05 419.23 26.76 o 3 12 0 36.06 10.50 19.67 o 4 12 0 2344.44 2215.55 78.15 o 5 12 0 505.82 495.70 40.33 o 6 12 0 323.65 335.14 55.38 o 7 12 0 99.39 52.18 34.66 o 8 12 0 30.68 48.48 66.03 o 9 12 0 143.98 166.70 57.51 o 10 12 0 52.22 32.92 96.91 o 1 13 0 1576.84 1716.17 76.39 o 2 13 0 256.23 251.74 34.80 o 3 13 0 2376.12 2449.33 87.50 o 4 13 0 335.88 251.44 36.85 o 5 13 0 1925.15 1962.47 81.37 o 6 13 0 28.83 -19.37 32.15 o 7 13 0 173.45 130.94 44.41 o 8 13 0 0.55 28.69 42.20 o 9 13 0 126.95 149.53 67.09 o 0 14 0 145.22 4.12 56.44 o 1 14 0 41.35 180.75 58.64 o 2 14 0 235.80 260.60 63.93 o 3 14 0 242.06 322.39 63.36 o 4 14 0 734.90 589.80 130.99 o 5 14 0 84.94 50.78 39.67 o 6 14 0 45.29 -14.91 43.83 o 7 14 0 7.25 52.15 48.99 o 8 14 0 127.82 110.95 50.05 o 1 15 0 6.06 2.13 79.87 o 2 15 0 25.42 38.74 51.69 o 3 15 0 32.86 39.24 57.00 o 4 15 0 162.01 109.06 70.89 o 5 15 0 10.79 33.90 61.79 o 6 15 0 38.66 85.87 200.22 o 0 16 0 369.98 262.89 123.54 o 1 16 0 41.80 3.19 88.39 o 2 16 0 86.68 137.20 72.42 o 3 16 0 12.57 37.36 62.94 o -15 1 1 17.08 23.31 54.16 o -14 1 1 0.42 -8.52 25.56 o -13 1 1 206.03 250.47 34.25 o -12 1 1 11.18 5.54 17.72 o -11 1 1 3.25 -3.19 18.10 o -10 1 1 444.75 454.08 22.00 o -9 1 1 9.98 3.11 9.70 o -8 1 1 0.07 9.58 11.71 o -7 1 1 106.30 99.15 9.04 o -6 1 1 2485.78 2621.19 32.36 o -5 1 1 71.78 68.82 5.11 o -4 1 1 821.57 825.67 15.97 o -3 1 1 54.10 37.31 3.01 o -2 1 1 0.13 0.00 1.51 o -1 1 1 141.54 143.85 3.19 o 0 1 1 243.65 225.07 8.52 o 1 1 1 107.97 109.71 3.01 o 2 1 1 47.46 39.07 4.26 o 3 1 1 797.18 815.79 12.05 o 4 1 1 191.81 171.28 7.45 o 5 1 1 144.71 150.17 7.53 o 6 1 1 31.51 24.62 6.02 o 7 1 1 0.22 6.82 8.52 o 8 1 1 235.53 184.76 17.04 o 9 1 1 2622.69 2935.35 61.77 o 10 1 1 34.43 30.25 19.17 o 11 1 1 226.78 186.30 20.29 o 12 1 1 22.96 6.56 18.42 o 13 1 1 69.30 12.58 46.86 o 14 1 1 0.02 -20.19 46.86 o 15 1 1 273.62 225.70 63.89 o -15 2 1 120.20 122.97 50.04 o -14 2 1 13.23 -22.77 36.12 o -13 2 1 174.61 151.83 29.67 o -12 2 1 31.27 12.00 22.00 o -11 2 1 110.05 96.79 16.36 o -10 2 1 427.25 435.17 20.92 o -9 2 1 963.51 1012.01 29.11 o -8 2 1 125.23 126.59 11.71 o -7 2 1 906.80 956.93 17.89 o -6 2 1 1704.18 1852.35 23.54 o -5 2 1 49.50 44.17 5.11 o -4 2 1 4.75 6.82 3.54 o -3 2 1 1051.07 971.20 13.31 o -2 2 1 49.50 38.77 7.45 o -1 2 1 105.65 96.28 6.39 o 0 2 1 790.28 745.50 9.04 o 1 2 1 54.30 52.21 1.51 o 2 2 1 1019.33 969.40 12.74 o 3 2 1 123.74 104.54 4.26 o 4 2 1 48.83 54.84 5.32 o 5 2 1 329.31 396.18 11.22 o 6 2 1 5.14 2.13 6.02 o 7 2 1 562.33 521.06 16.36 o 8 2 1 443.00 452.22 17.27 o 9 2 1 4.78 -9.80 11.22 o 10 2 1 816.77 824.99 29.34 o 11 2 1 64.55 22.32 18.78 o 12 2 1 6.68 -15.41 23.54 o 13 2 1 57.85 101.58 31.20 o 14 2 1 20.02 8.18 40.58 o -15 3 1 115.27 48.04 46.57 o -14 3 1 31.57 17.61 32.68 o -13 3 1 466.39 405.37 53.25 o -12 3 1 132.61 95.85 28.65 o -11 3 1 269.65 251.96 25.16 o -10 3 1 183.71 137.14 15.97 o -9 3 1 180.20 174.39 15.06 o -8 3 1 133.83 102.61 9.70 o -7 3 1 563.17 572.97 14.18 o -6 3 1 155.54 165.27 8.18 o -5 3 1 295.66 308.64 11.71 o -4 3 1 1062.35 1036.03 14.84 o -3 3 1 120.20 85.41 6.02 o -2 3 1 380.13 389.76 8.18 o -1 3 1 374.76 410.78 11.71 o 0 3 1 653.68 621.25 9.70 o 1 3 1 507.61 457.96 9.04 o 2 3 1 3469.82 3322.35 40.58 o 3 3 1 1.80 2.98 3.54 o 4 3 1 829.81 846.67 13.56 o 5 3 1 885.94 871.17 15.76 o 6 3 1 58.11 57.53 10.65 o 7 3 1 9.69 3.41 9.58 o 8 3 1 282.28 259.14 19.17 o 9 3 1 98.86 74.68 12.78 o 10 3 1 582.76 552.11 28.36 o 11 3 1 601.26 515.51 70.29 o 12 3 1 71.13 75.13 25.47 o 13 3 1 118.67 168.22 38.88 o 14 3 1 23.72 -35.14 35.14 o -14 4 1 70.08 54.59 38.61 o -13 4 1 338.14 326.61 44.26 o -12 4 1 177.56 124.62 29.34 o -11 4 1 1675.46 1764.55 53.07 o -10 4 1 481.44 474.45 21.80 o -9 4 1 314.78 339.74 17.27 o -8 4 1 199.13 190.12 11.77 o -7 4 1 109.02 111.15 8.67 o -6 4 1 5.77 -1.06 5.48 o -5 4 1 1873.15 1857.42 23.02 o -4 4 1 46.05 35.44 6.02 o -3 4 1 1887.40 1783.88 22.59 o -2 4 1 1845.67 1833.70 45.79 o -1 4 1 23.21 20.29 3.01 o 0 4 1 9.30 10.65 3.01 o 1 4 1 846.98 855.26 12.05 o 2 4 1 3924.71 3921.80 44.88 o 3 4 1 1043.95 1008.87 16.36 o 4 4 1 3259.75 3422.94 40.33 o 5 4 1 295.23 259.94 8.67 o 6 4 1 1948.15 2035.14 38.34 o 7 4 1 976.60 1065.61 24.49 o 8 4 1 52.06 33.61 13.31 o 9 4 1 401.84 425.17 21.49 o 10 4 1 112.29 87.33 16.88 o 11 4 1 143.76 116.38 30.88 o 12 4 1 364.35 317.73 48.99 o 13 4 1 0.11 -29.40 63.90 o 14 4 1 5.05 18.86 45.92 o -14 5 1 408.30 365.30 54.31 o -13 5 1 19.63 56.33 46.86 o -12 5 1 21.02 -12.34 20.88 o -11 5 1 0.17 24.49 22.36 o -10 5 1 624.23 600.71 27.98 o -9 5 1 394.39 401.65 17.89 o -8 5 1 2068.73 2244.27 37.79 o -7 5 1 125.11 117.39 18.10 o -6 5 1 54.46 39.56 7.09 o -5 5 1 0.57 0.00 6.02 o -4 5 1 2732.33 2920.73 34.80 o -3 5 1 106.27 101.06 8.52 o -2 5 1 2874.65 2914.05 32.22 o -1 5 1 270.07 249.08 7.09 o 0 5 1 477.41 414.87 8.67 o 1 5 1 266.43 218.45 6.02 o 2 5 1 5083.59 5137.32 57.97 o 3 5 1 1279.78 1366.64 44.73 o 4 5 1 4972.72 5495.34 68.16 o 5 5 1 2.85 5.54 5.87 o 6 5 1 150.82 147.46 10.65 o 7 5 1 130.97 90.46 13.78 o 8 5 1 960.51 999.20 31.20 o 9 5 1 937.97 1008.60 33.66 o 10 5 1 75.21 84.61 17.72 o 11 5 1 4.52 -14.91 18.07 o 12 5 1 23.69 35.53 31.52 o 13 5 1 456.51 390.91 110.76 o 14 5 1 18.02 -4.45 47.87 o -14 6 1 59.74 40.04 56.10 o -13 6 1 107.09 96.42 39.07 o -12 6 1 850.22 935.63 56.44 o -11 6 1 636.21 642.47 33.86 o -10 6 1 127.77 96.45 19.31 o -9 6 1 1.44 14.91 10.54 o -8 6 1 25.02 16.55 21.30 o -7 6 1 113.27 103.82 22.36 o -6 6 1 263.64 236.18 15.97 o -5 6 1 7177.48 7894.26 199.15 o -4 6 1 438.11 412.57 12.74 o -3 6 1 191.42 140.71 7.62 o -2 6 1 3200.99 3317.58 36.85 o -1 6 1 756.27 701.12 30.88 o 0 6 1 290.49 337.97 8.67 o 1 6 1 1693.08 1726.25 45.79 o 2 6 1 2475.35 2578.46 33.03 o 3 6 1 754.42 735.60 23.43 o 4 6 1 2498.49 2508.51 36.64 o 5 6 1 1117.12 1122.07 25.56 o 6 6 1 269.69 252.10 13.78 o 7 6 1 41.68 30.56 7.91 o 8 6 1 94.96 64.66 28.75 o 9 6 1 1580.82 1679.62 53.97 o 10 6 1 2088.04 2330.87 73.48 o 11 6 1 200.34 161.22 26.33 o 12 6 1 83.70 25.33 37.27 o 13 6 1 9.71 31.38 44.88 o 14 6 1 87.59 84.61 58.57 o -13 7 1 65.39 59.71 45.48 o -12 7 1 13.35 19.35 35.77 o -11 7 1 2.14 -23.54 23.54 o -10 7 1 57.61 50.82 20.45 o -9 7 1 302.26 318.43 48.99 o -8 7 1 2904.86 3195.68 66.22 o -7 7 1 2332.01 2542.67 42.53 o -6 7 1 74.10 35.60 10.22 o -5 7 1 808.59 755.57 52.18 o -4 7 1 17.70 12.07 8.52 o -3 7 1 197.47 198.12 10.96 o -2 7 1 6315.18 6633.28 107.56 o -1 7 1 932.98 956.97 42.60 o 0 7 1 1046.98 943.63 21.30 o 1 7 1 771.60 716.97 13.78 o 2 7 1 868.31 920.59 29.82 o 3 7 1 265.08 321.36 29.82 o 4 7 1 1817.38 1891.28 56.44 o 5 7 1 569.13 580.77 16.94 o 6 7 1 76.54 52.52 17.04 o 7 7 1 1233.71 1355.06 42.60 o 8 7 1 151.36 112.68 17.04 o 9 7 1 15.30 0.00 16.88 o 10 7 1 72.61 62.20 26.04 o 11 7 1 239.25 188.85 35.78 o 12 7 1 53.29 90.24 42.75 o 13 7 1 230.21 252.43 60.25 o -13 8 1 2.13 10.70 57.00 o -12 8 1 271.65 277.64 94.78 o -11 8 1 565.91 543.03 50.05 o -10 8 1 153.62 86.72 25.56 o -9 8 1 701.65 620.54 32.73 o -8 8 1 898.67 899.36 52.18 o -7 8 1 16.33 13.21 13.13 o -6 8 1 175.02 150.71 33.01 o -5 8 1 834.13 894.99 33.01 o -4 8 1 148.64 115.46 11.75 o -3 8 1 233.18 223.24 11.75 o -2 8 1 167.00 134.14 10.65 o -1 8 1 1278.18 1328.02 23.84 o 0 8 1 2112.98 2273.59 42.60 o 1 8 1 299.25 286.74 10.63 o 2 8 1 2394.13 2559.14 84.13 o 3 8 1 144.04 127.58 12.74 o 4 8 1 654.70 639.53 23.54 o 5 8 1 546.50 586.28 27.69 o 6 8 1 1364.24 1367.37 31.50 o 7 8 1 45.52 28.44 11.22 o 8 8 1 2269.45 2451.76 62.42 o 9 8 1 363.95 386.00 30.01 o 10 8 1 1823.26 2050.21 86.26 o 11 8 1 99.94 80.58 37.74 o 12 8 1 153.91 116.27 50.94 o 13 8 1 20.34 132.94 61.70 o -12 9 1 6.00 52.98 46.62 o -11 9 1 30.72 25.27 33.03 o -10 9 1 263.01 247.51 35.78 o -9 9 1 51.59 48.38 34.08 o -8 9 1 978.53 1007.25 50.15 o -7 9 1 32.02 46.15 13.34 o -6 9 1 467.37 396.55 45.79 o -5 9 1 387.38 383.40 15.82 o -4 9 1 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