#------------------------------------------------------------------------------ #$Date: 2012-01-03 14:54:16 +0200 (Tue, 03 Jan 2012) $ #$Revision: 31968 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/10/49/2104998.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_2104998_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 101.560 _cell_angle_gamma 90.000 _cell_length_a 11.9430 _cell_length_b 12.6930 _cell_length_c 15.9820 _exptl_crystal_F_000 1160.00 _reflns_d_resolution_high 0.7702 _[local]_cod_data_source_file hw501890K_IVsup6.hkl _[local]_cod_data_source_block 90K_IV #BEGIN Tags that were not found in dictionaries: _shelx_title ' k06177 in P2(1)/c' _shelx_refln_list_code 4 _shelx_f_calc_maximum 353.15 _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 0 792.23 781.98 12.61 o 2 0 0 18991.90 17600.79 285.88 o 3 0 0 67.20 50.45 4.20 o 4 0 0 6291.08 6434.49 115.61 o 5 0 0 910.24 1038.43 23.12 o 6 0 0 57420.20 59259.99 929.12 o 7 0 0 3.51 8.41 10.51 o 8 0 0 7656.09 7725.18 159.76 o 9 0 0 1396.54 1370.56 54.65 o 10 0 0 3269.97 3714.39 115.61 o 11 0 0 24.15 -10.51 23.12 o 12 0 0 320.17 340.54 54.65 o 13 0 0 33.33 46.25 42.04 o 14 0 0 730.44 695.79 90.39 o 15 0 0 1459.06 1706.90 149.25 o 1 1 0 26204.06 23703.58 296.07 o 2 1 0 16.81 13.74 1.49 o 3 1 0 4654.47 4417.00 66.22 o 4 1 0 364.43 354.73 13.66 o 5 1 0 6738.10 6432.48 73.74 o 6 1 0 3948.26 3845.10 48.78 o 7 1 0 4459.65 4239.35 58.02 o 8 1 0 6377.99 6856.20 101.04 o 9 1 0 3939.10 3872.19 87.24 o 10 1 0 259.00 201.69 18.65 o 11 1 0 1197.70 1278.71 83.03 o 12 1 0 967.28 1013.38 64.11 o 13 1 0 28.99 19.92 50.45 o 14 1 0 17.05 -18.71 43.38 o 15 1 0 194.99 200.00 64.11 o 0 2 0 55675.63 51124.91 1399.99 o 1 2 0 85.16 92.54 2.97 o 2 2 0 529.69 470.10 11.56 o 3 2 0 353.47 322.09 6.57 o 4 2 0 6672.10 6757.41 69.81 o 5 2 0 944.86 863.54 14.06 o 6 2 0 7015.21 7119.63 78.79 o 7 2 0 2.50 -0.84 7.00 o 8 2 0 1742.18 1808.80 36.36 o 9 2 0 1286.32 1272.46 74.62 o 10 2 0 1698.76 1761.25 49.32 o 11 2 0 877.52 876.10 40.70 o 12 2 0 359.84 224.33 30.43 o 13 2 0 233.78 173.02 50.16 o 14 2 0 330.50 236.88 60.27 o 15 2 0 526.60 399.62 70.31 o 1 3 0 332.16 350.23 6.57 o 2 3 0 240.43 243.86 5.95 o 3 3 0 52687.38 49937.52 517.62 o 4 3 0 14530.70 15627.85 153.71 o 5 3 0 16821.76 16342.03 173.59 o 6 3 0 1355.95 1293.02 20.99 o 7 3 0 3509.82 3506.11 57.91 o 8 3 0 3788.88 4081.89 149.25 o 9 3 0 2329.08 2348.76 48.45 o 10 3 0 2876.49 2955.48 72.90 o 11 3 0 3133.71 3296.50 84.79 o 12 3 0 380.45 373.18 110.36 o 13 3 0 1023.04 1053.15 64.78 o 14 3 0 326.95 204.22 63.37 o 0 4 0 2544.87 2321.86 54.65 o 1 4 0 11.73 13.74 2.97 o 2 4 0 47206.82 47271.45 500.26 o 3 4 0 1346.67 1332.84 17.84 o 4 4 0 28802.00 29679.44 287.28 o 5 4 0 10203.53 11132.97 119.41 o 6 4 0 3165.28 3039.27 43.38 o 7 4 0 35.46 19.97 9.46 o 8 4 0 1703.99 1887.19 35.75 o 9 4 0 19.51 8.69 11.07 o 10 4 0 817.89 881.03 38.12 o 11 4 0 2669.77 2829.80 88.00 o 12 4 0 1867.48 2049.16 74.09 o 13 4 0 657.72 590.06 115.61 o 14 4 0 555.20 451.22 150.30 o 1 5 0 1669.46 1718.75 28.38 o 2 5 0 43.97 36.52 5.05 o 3 5 0 4144.55 3924.16 41.88 o 4 5 0 7991.61 8422.52 86.87 o 5 5 0 5598.48 5488.77 76.73 o 6 5 0 25.70 7.01 6.57 o 7 5 0 1930.88 2094.18 66.22 o 8 5 0 689.43 721.16 21.02 o 9 5 0 332.36 347.51 17.05 o 10 5 0 3350.07 3628.99 97.29 o 11 5 0 1258.27 1161.90 60.86 o 12 5 0 37.19 24.51 32.58 o 13 5 0 526.38 450.41 55.59 o 14 5 0 991.99 980.74 105.49 o 0 6 0 6440.35 6391.89 162.91 o 1 6 0 871.33 873.87 14.06 o 2 6 0 29665.77 30666.04 318.86 o 3 6 0 1244.43 1324.66 29.43 o 4 6 0 10174.85 10320.64 176.58 o 5 6 0 883.98 931.40 20.99 o 6 6 0 5458.96 5725.73 95.65 o 7 6 0 22.72 4.37 8.91 o 8 6 0 975.05 1022.72 46.25 o 9 6 0 211.80 177.47 19.52 o 10 6 0 817.47 847.49 42.59 o 11 6 0 1589.26 1708.00 245.94 o 12 6 0 830.84 706.30 46.94 o 13 6 0 596.05 507.20 54.94 o 14 6 0 55.75 11.16 69.37 o 1 7 0 14860.13 15803.19 182.88 o 2 7 0 5.90 4.20 5.41 o 3 7 0 4938.19 4932.07 187.09 o 4 7 0 423.30 389.45 11.28 o 5 7 0 9418.90 10092.33 126.55 o 6 7 0 49.67 66.95 11.56 o 7 7 0 5509.67 5789.04 92.34 o 8 7 0 368.42 358.92 30.48 o 9 7 0 1038.02 1029.39 38.89 o 10 7 0 1561.11 1591.81 57.54 o 11 7 0 1726.35 1818.04 112.46 o 12 7 0 10.08 36.27 43.83 o 13 7 0 101.06 118.48 44.88 o 0 8 0 7416.72 7549.98 133.38 o 1 8 0 128.72 105.26 8.07 o 2 8 0 1910.06 1858.05 29.55 o 3 8 0 966.03 1009.99 21.33 o 4 8 0 79.84 81.43 7.81 o 5 8 0 486.82 484.33 15.04 o 6 8 0 1618.44 1599.09 33.74 o 7 8 0 2300.01 2468.71 49.77 o 8 8 0 486.95 400.67 24.11 o 9 8 0 1449.08 1327.98 55.50 o 10 8 0 867.87 1008.67 74.62 o 11 8 0 227.37 217.21 56.76 o 12 8 0 3.88 -5.55 39.94 o 13 8 0 480.53 512.11 196.55 o 1 9 0 5734.78 6031.42 113.51 o 2 9 0 1174.12 1229.03 57.81 o 3 9 0 61.59 34.73 7.68 o 4 9 0 908.46 939.86 34.68 o 5 9 0 358.67 365.97 21.02 o 6 9 0 1010.45 963.55 38.89 o 7 9 0 1658.50 1783.59 52.38 o 8 9 0 2072.37 2180.04 70.93 o 9 9 0 1489.00 1412.10 59.09 o 10 9 0 916.17 866.32 48.98 o 11 9 0 176.88 150.40 39.37 o 12 9 0 6.46 -10.88 48.22 o 0 10 0 10281.36 10520.83 261.71 o 1 10 0 158.86 146.45 11.62 o 2 10 0 389.83 374.29 16.49 o 3 10 0 70.35 52.90 15.14 o 4 10 0 195.17 188.18 28.38 o 5 10 0 138.11 126.46 18.65 o 6 10 0 2281.52 2376.35 57.16 o 7 10 0 1055.18 1081.87 38.11 o 8 10 0 666.32 644.35 42.42 o 9 10 0 713.90 608.07 46.38 o 10 10 0 816.89 747.15 54.65 o 11 10 0 39.16 8.69 44.30 o 12 10 0 32.60 89.32 48.29 o 1 11 0 3119.06 3294.60 64.95 o 2 11 0 222.56 176.30 19.70 o 3 11 0 207.08 175.77 34.68 o 4 11 0 50.88 13.38 16.15 o 5 11 0 1915.47 1963.30 53.51 o 6 11 0 213.91 198.84 39.94 o 7 11 0 350.76 282.14 34.72 o 8 11 0 34.58 5.41 30.27 o 9 11 0 287.87 235.89 41.88 o 10 11 0 273.57 214.11 41.41 o 11 11 0 105.43 98.31 56.87 o 0 12 0 422.91 412.31 42.04 o 1 12 0 204.90 146.16 27.33 o 2 12 0 455.42 395.19 24.75 o 3 12 0 31.91 26.84 43.09 o 4 12 0 2777.18 2723.30 80.22 o 5 12 0 747.60 678.10 38.56 o 6 12 0 311.27 278.65 63.06 o 7 12 0 145.79 127.81 32.70 o 8 12 0 65.98 74.12 42.04 o 9 12 0 215.47 245.75 69.37 o 10 12 0 61.51 83.71 41.88 o 1 13 0 2009.80 2315.89 75.03 o 2 13 0 392.45 393.16 75.68 o 3 13 0 2827.18 2979.98 83.50 o 4 13 0 404.18 337.49 35.30 o 5 13 0 2372.17 2423.12 80.27 o 6 13 0 52.53 6.70 27.47 o 7 13 0 214.04 156.68 43.03 o 8 13 0 1.81 -31.66 34.85 o 9 13 0 127.36 125.47 45.17 o 0 14 0 211.49 67.34 60.66 o 1 14 0 46.88 40.20 35.30 o 2 14 0 282.37 245.91 54.12 o 3 14 0 312.80 234.26 65.16 o 4 14 0 1018.37 873.06 56.06 o 5 14 0 143.50 67.27 33.22 o 6 14 0 65.49 81.52 40.86 o 7 14 0 6.10 -2.97 40.99 o 8 14 0 175.30 87.82 43.83 o 1 15 0 17.42 -7.81 47.81 o 2 15 0 28.12 -3.02 42.34 o 3 15 0 59.91 20.28 48.22 o 4 15 0 237.22 226.71 58.02 o 5 15 0 14.67 66.01 58.57 o 6 15 0 37.37 50.36 69.43 o 0 16 0 424.07 315.31 86.06 o 1 16 0 66.00 37.23 57.58 o 2 16 0 65.92 36.45 48.15 o 3 16 0 25.48 53.23 54.94 o -15 1 1 22.66 -26.05 66.22 o -14 1 1 4.37 -10.51 31.21 o -13 1 1 271.18 268.11 46.25 o -12 1 1 15.91 -0.06 24.75 o -11 1 1 0.21 -22.30 22.30 o -10 1 1 610.19 564.55 28.12 o -9 1 1 20.84 28.26 13.13 o -8 1 1 6.69 7.76 8.91 o -7 1 1 80.23 64.05 8.55 o -6 1 1 2649.50 2940.82 37.71 o -5 1 1 108.71 105.77 6.31 o -4 1 1 773.11 811.96 18.92 o -3 1 1 50.71 32.62 2.97 o -2 1 1 1.73 4.20 1.49 o -1 1 1 124.94 124.34 6.31 o 0 1 1 219.04 199.72 2.97 o 1 1 1 124.29 129.36 3.15 o 2 1 1 47.69 40.94 3.15 o 3 1 1 743.23 745.44 13.66 o 4 1 1 194.04 186.15 14.71 o 5 1 1 204.94 242.64 14.71 o 6 1 1 41.89 44.14 6.57 o 7 1 1 0.15 -1.26 11.56 o 8 1 1 201.78 160.25 12.57 o 9 1 1 3259.01 3548.74 62.53 o 10 1 1 60.03 38.07 16.82 o 11 1 1 300.71 285.70 33.63 o 12 1 1 16.96 -12.05 21.71 o 13 1 1 99.69 114.91 49.35 o 14 1 1 0.65 24.43 42.33 o -15 2 1 207.46 207.68 54.04 o -14 2 1 39.03 6.27 39.66 o -13 2 1 176.11 67.62 35.74 o -12 2 1 45.05 41.74 30.27 o -11 2 1 161.55 127.90 30.48 o -10 2 1 470.84 474.07 23.23 o -9 2 1 1217.18 1290.46 43.09 o -8 2 1 128.14 130.33 10.82 o -7 2 1 1020.82 1050.68 19.41 o -6 2 1 1915.92 2150.45 28.64 o -5 2 1 63.55 56.88 5.41 o -4 2 1 7.08 5.05 4.20 o -3 2 1 1095.09 1005.75 14.06 o -2 2 1 44.92 37.06 3.15 o -1 2 1 113.25 107.21 2.97 o 0 2 1 845.50 792.49 8.92 o 1 2 1 68.33 62.03 1.49 o 2 2 1 1076.65 1053.21 11.89 o 3 2 1 112.62 92.68 4.20 o 4 2 1 63.02 71.43 5.05 o 5 2 1 332.28 379.00 9.58 o 6 2 1 12.82 9.46 5.95 o 7 2 1 704.63 718.06 20.03 o 8 2 1 555.33 559.87 20.03 o 9 2 1 17.05 18.92 12.61 o 10 2 1 919.62 850.10 34.34 o 11 2 1 136.23 81.03 20.26 o 12 2 1 5.44 11.67 25.52 o 13 2 1 79.35 50.70 67.27 o 14 2 1 29.38 -26.29 71.47 o -15 3 1 160.91 85.95 59.86 o -14 3 1 46.09 23.44 45.19 o -13 3 1 567.37 515.00 43.90 o -12 3 1 186.68 120.35 31.96 o -11 3 1 315.02 299.28 32.76 o -10 3 1 293.00 252.27 32.58 o -9 3 1 283.93 278.40 17.87 o -8 3 1 205.72 186.60 19.97 o -7 3 1 587.73 580.76 43.09 o -6 3 1 163.12 182.38 8.55 o -5 3 1 332.61 324.69 11.56 o -4 3 1 1074.72 1024.78 15.77 o -3 3 1 90.18 63.13 4.46 o -2 3 1 428.34 422.06 15.77 o -1 3 1 342.42 370.35 6.57 o 0 3 1 650.53 610.39 8.07 o 1 3 1 581.95 507.71 8.92 o 2 3 1 3485.30 3408.87 40.99 o 3 3 1 6.97 19.22 3.50 o 4 3 1 824.06 815.47 12.57 o 5 3 1 1029.41 1012.64 22.07 o 6 3 1 90.38 87.34 6.57 o 7 3 1 11.89 9.55 8.07 o 8 3 1 251.71 223.44 14.06 o 9 3 1 119.13 111.77 13.38 o 10 3 1 740.53 741.01 34.65 o 11 3 1 745.36 694.83 38.68 o 12 3 1 86.42 38.11 26.96 o 13 3 1 121.93 110.89 47.30 o 14 3 1 18.31 111.55 74.62 o -14 4 1 78.53 13.86 44.93 o -13 4 1 364.82 318.53 51.50 o -12 4 1 185.57 92.75 35.30 o -11 4 1 1826.47 1819.82 76.73 o -10 4 1 552.13 522.73 24.11 o -9 4 1 323.42 299.73 15.14 o -8 4 1 289.49 287.42 14.71 o -7 4 1 92.78 93.04 8.91 o -6 4 1 4.53 4.20 5.41 o -5 4 1 1659.13 1634.65 43.09 o -4 4 1 34.47 24.17 5.95 o -3 4 1 1855.73 1704.14 23.12 o -2 4 1 2086.25 2014.35 24.49 o -1 4 1 34.81 29.58 2.97 o 0 4 1 6.28 11.56 2.97 o 1 4 1 918.83 925.70 12.57 o 2 4 1 3990.11 4078.50 43.42 o 3 4 1 1116.53 1094.41 17.87 o 4 4 1 3373.88 3486.12 38.87 o 5 4 1 244.17 191.17 9.46 o 6 4 1 1984.38 2065.25 36.16 o 7 4 1 1180.25 1288.52 28.12 o 8 4 1 25.02 11.50 12.57 o 9 4 1 430.04 419.67 26.67 o 10 4 1 71.27 62.53 24.17 o 11 4 1 209.76 176.70 26.67 o 12 4 1 479.86 391.61 39.67 o 13 4 1 6.56 39.41 40.99 o 14 4 1 0.62 34.85 101.95 o -14 5 1 584.26 513.04 60.29 o -13 5 1 32.11 0.09 33.32 o -12 5 1 19.85 14.18 27.52 o -11 5 1 1.62 13.23 23.24 o -10 5 1 874.16 862.91 58.86 o -9 5 1 448.07 373.95 19.41 o -8 5 1 2392.20 2614.42 49.24 o -7 5 1 153.10 154.77 10.49 o -6 5 1 37.37 12.19 8.41 o -5 5 1 9.07 7.01 6.57 o -4 5 1 2989.46 3172.64 36.84 o -3 5 1 62.03 46.25 5.95 o -2 5 1 3027.17 3067.32 34.09 o -1 5 1 293.62 260.66 6.57 o 0 5 1 503.73 427.60 15.77 o 1 5 1 303.30 247.60 6.57 o 2 5 1 5141.68 5255.93 63.06 o 3 5 1 1598.25 1699.36 20.99 o 4 5 1 5102.09 5654.62 64.59 o 5 5 1 2.03 -7.30 7.30 o 6 5 1 138.14 127.81 9.40 o 7 5 1 171.49 129.23 12.05 o 8 5 1 1100.97 1112.49 66.22 o 9 5 1 1019.04 940.22 48.35 o 10 5 1 160.01 130.89 23.71 o 11 5 1 7.99 -2.10 33.63 o 12 5 1 10.20 -37.35 37.84 o 13 5 1 521.34 484.40 46.93 o 14 5 1 24.45 39.74 58.82 o -14 6 1 65.55 77.70 76.22 o -13 6 1 129.45 38.36 52.96 o -12 6 1 1180.53 1257.58 183.93 o -11 6 1 672.47 573.90 113.51 o -10 6 1 169.59 142.66 22.74 o -9 6 1 13.55 15.77 10.40 o -8 6 1 6.52 7.11 8.91 o -7 6 1 134.01 116.63 10.82 o -6 6 1 299.35 277.00 12.71 o -5 6 1 8087.56 8729.86 141.89 o -4 6 1 441.64 463.73 12.57 o -3 6 1 150.54 97.08 8.07 o -2 6 1 3340.97 3440.13 46.25 o -1 6 1 721.14 679.06 27.33 o 0 6 1 335.46 398.68 11.56 o 1 6 1 1777.40 1809.27 30.48 o 2 6 1 2791.95 2850.05 72.52 o 3 6 1 864.62 864.81 24.17 o 4 6 1 2782.75 2884.96 37.24 o 5 6 1 1079.72 1108.28 22.14 o 6 6 1 341.14 343.47 14.32 o 7 6 1 64.83 64.66 9.57 o 8 6 1 89.05 86.91 14.71 o 9 6 1 2198.14 2249.16 73.57 o 10 6 1 2418.04 2568.40 76.61 o 11 6 1 310.68 277.05 31.53 o 12 6 1 98.90 60.96 31.21 o 13 6 1 22.98 50.22 48.15 o -13 7 1 71.68 55.18 50.47 o -12 7 1 16.98 39.79 39.89 o -11 7 1 10.77 -17.87 29.55 o -10 7 1 85.48 57.92 23.79 o -9 7 1 379.04 375.74 21.90 o -8 7 1 3386.51 3777.58 69.43 o -7 7 1 2956.10 3196.72 51.32 o -6 7 1 57.61 47.48 9.58 o -5 7 1 806.35 774.94 21.63 o -4 7 1 12.55 5.73 7.30 o -3 7 1 167.34 188.49 10.82 o -2 7 1 6908.67 7152.19 81.39 o -1 7 1 956.67 929.49 21.02 o 0 7 1 1090.69 971.87 15.77 o 1 7 1 722.27 648.20 12.05 o 2 7 1 854.71 920.53 18.65 o 3 7 1 362.69 408.87 37.84 o 4 7 1 1957.62 2042.63 43.09 o 5 7 1 525.42 537.67 17.87 o 6 7 1 122.06 105.59 11.07 o 7 7 1 1357.36 1459.06 47.30 o 8 7 1 241.31 239.34 17.83 o 9 7 1 21.33 8.80 18.12 o 10 7 1 186.85 148.89 67.27 o 11 7 1 241.35 149.08 36.36 o 12 7 1 54.62 14.27 45.32 o 13 7 1 250.96 127.85 48.98 o -13 8 1 2.10 23.58 39.89 o -12 8 1 347.27 257.19 64.11 o -11 8 1 564.31 526.64 97.75 o -10 8 1 179.14 152.86 53.60 o -9 8 1 656.50 593.84 33.63 o -8 8 1 916.13 915.75 30.71 o -7 8 1 35.88 20.91 12.71 o -6 8 1 167.06 163.62 18.92 o -5 8 1 889.48 904.24 23.24 o -4 8 1 207.03 174.33 12.96 o -3 8 1 198.59 197.95 11.28 o -2 8 1 137.60 109.69 8.55 o -1 8 1 1270.65 1256.50 21.71 o 0 8 1 2196.48 2283.36 33.63 o 1 8 1 263.63 233.63 9.58 o 2 8 1 2586.64 2697.00 49.40 o 3 8 1 177.38 152.72 26.28 o 4 8 1 766.63 720.46 22.55 o 5 8 1 622.00 642.99 21.02 o 6 8 1 1550.29 1592.94 44.14 o 7 8 1 93.86 92.41 14.32 o 8 8 1 2309.26 2451.78 68.68 o 9 8 1 465.09 411.43 67.27 o 10 8 1 2133.66 2458.07 120.15 o 11 8 1 138.25 132.20 47.50 o 12 8 1 244.02 244.10 47.88 o 13 8 1 24.17 -28.23 46.80 o -12 9 1 5.37 -46.01 46.01 o -11 9 1 50.45 31.30 32.83 o -10 9 1 329.81 267.84 33.42 o -9 9 1 59.02 37.11 21.51 o -8 9 1 1210.90 1293.58 55.37 o -7 9 1 31.86 38.33 18.92 o -6 9 1 485.48 420.99 22.07 o -5 9 1 395.69 348.81 42.04 o -4 9 1 6.84 0.74 11.07 o -3 9 1 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