#------------------------------------------------------------------------------ #$Date: 2012-01-03 14:54:16 +0200 (Tue, 03 Jan 2012) $ #$Revision: 31968 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/10/50/2105020.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_2105020_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 12 _symmetry_space_group_name_Hall '-I 2y' _symmetry_space_group_name_H-M 'I 1 2/m 1' _cell_angle_alpha 90.000 _cell_angle_beta 101.480 _cell_angle_gamma 90.000 _cell_length_a 12.3700 _cell_length_b 12.5700 _cell_length_c 8.1140 _exptl_crystal_F_000 580.00 _reflns_d_resolution_high 0.7709 _[local]_cod_data_source_file hw5018295K_Isup28.hkl _[local]_cod_data_source_block 295K_I #BEGIN Tags that were not found in dictionaries: _shelx_title ' k06204 in I2/m' _shelx_refln_list_code 4 _shelx_f_calc_maximum 179.82 _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' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, -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 2 0 0 5039.71 4518.03 90.71 o 4 0 0 923.64 832.90 19.24 o 6 0 0 9594.41 10394.01 200.12 o 8 0 0 1679.57 1663.07 38.49 o 10 0 0 222.35 223.21 12.64 o 12 0 0 60.56 97.86 13.74 o 14 0 0 7.86 -2.75 19.24 o 1 1 0 7677.35 7119.23 106.13 o 3 1 0 1095.18 919.58 13.59 o 5 1 0 641.34 587.96 29.69 o 7 1 0 983.25 814.68 24.19 o 9 1 0 878.22 965.59 22.00 o 11 1 0 131.42 131.08 9.13 o 13 1 0 84.71 76.91 11.75 o 15 1 0 25.21 67.67 23.64 o 0 2 0 12889.90 12158.06 377.42 o 2 2 0 54.90 43.79 3.02 o 4 2 0 2370.23 2258.82 56.89 o 6 2 0 2028.66 1869.17 37.65 o 8 2 0 773.37 833.11 18.54 o 10 2 0 265.89 290.58 13.19 o 12 2 0 106.26 105.00 11.48 o 14 2 0 17.72 30.22 16.57 o 1 3 0 59.22 99.15 5.77 o 3 3 0 10860.62 10588.03 197.50 o 5 3 0 5019.75 5112.80 165.21 o 7 3 0 354.98 357.78 9.31 o 9 3 0 294.31 300.10 10.64 o 11 3 0 416.10 472.12 25.01 o 13 3 0 122.71 126.78 26.66 o 15 3 0 25.83 34.12 20.44 o 0 4 0 853.62 731.76 16.75 o 2 4 0 9173.45 8721.89 157.40 o 4 4 0 7012.59 7070.08 94.48 o 6 4 0 1061.93 1035.52 18.09 o 8 4 0 591.01 566.26 14.96 o 10 4 0 131.94 144.43 10.72 o 12 4 0 104.17 113.93 13.92 o 14 4 0 39.85 50.02 14.85 o 1 5 0 352.28 348.06 6.72 o 3 5 0 505.22 613.92 17.88 o 5 5 0 2390.68 2302.69 32.10 o 7 5 0 238.60 297.99 9.72 o 9 5 0 4.83 0.73 4.85 o 11 5 0 294.50 318.91 29.41 o 13 5 0 84.74 83.93 15.46 o 0 6 0 1733.54 1657.01 51.41 o 2 6 0 5938.41 6025.48 118.75 o 4 6 0 1713.76 1765.07 30.51 o 6 6 0 585.32 510.57 12.91 o 8 6 0 378.01 384.17 13.42 o 10 6 0 119.12 138.00 15.71 o 12 6 0 47.14 64.24 21.72 o 14 6 0 22.52 26.24 17.19 o 1 7 0 1700.35 1557.23 26.46 o 3 7 0 353.89 365.33 9.93 o 5 7 0 1084.97 1016.92 24.92 o 7 7 0 266.03 292.31 37.39 o 9 7 0 76.65 63.38 10.95 o 11 7 0 202.44 203.49 19.83 o 13 7 0 20.02 24.61 17.68 o 0 8 0 1234.56 1179.72 36.72 o 2 8 0 661.49 613.99 46.18 o 4 8 0 53.90 60.92 10.17 o 6 8 0 158.20 153.42 12.37 o 8 8 0 296.97 243.16 19.52 o 10 8 0 183.47 196.06 28.86 o 12 8 0 2.95 0.69 17.06 o 1 9 0 671.95 721.69 18.20 o 3 9 0 54.72 58.87 9.90 o 5 9 0 102.59 103.97 12.37 o 7 9 0 239.36 212.84 14.16 o 9 9 0 190.76 185.30 16.27 o 11 9 0 28.47 9.66 36.29 o 13 9 0 9.78 1.39 20.56 o 0 10 0 1286.27 1531.86 49.20 o 2 10 0 164.76 162.36 22.27 o 4 10 0 22.47 17.24 6.68 o 6 10 0 301.87 331.36 14.92 o 8 10 0 155.77 116.49 18.75 o 10 10 0 36.27 23.54 17.59 o 12 10 0 6.40 3.08 21.48 o 1 11 0 58.03 63.82 9.21 o 3 11 0 82.04 79.93 16.22 o 5 11 0 102.96 115.77 11.27 o 7 11 0 52.14 51.35 10.21 o 9 11 0 17.06 18.23 17.04 o 11 11 0 8.41 43.56 21.26 o 0 12 0 174.78 176.48 15.94 o 2 12 0 94.49 100.18 22.54 o 4 12 0 161.73 152.48 17.59 o 6 12 0 105.86 93.74 26.66 o 8 12 0 3.43 -24.19 24.19 o 10 12 0 7.95 -2.81 19.29 o 1 13 0 31.49 40.31 8.44 o 3 13 0 204.00 261.05 16.49 o 5 13 0 96.21 93.62 13.32 o 7 13 0 5.49 9.55 18.14 o 9 13 0 8.49 4.03 20.51 o 0 14 0 2.26 8.80 12.64 o 2 14 0 16.69 12.29 10.01 o 4 14 0 28.09 32.46 10.52 o 6 14 0 10.40 21.99 22.27 o 8 14 0 7.01 12.64 25.29 o 1 15 0 4.13 28.04 25.29 o 3 15 0 10.12 14.37 23.92 o 5 15 0 7.09 5.05 22.47 o 0 16 0 26.10 14.84 42.88 o 2 16 0 18.25 18.14 24.19 o -15 0 1 49.84 37.39 18.69 o -13 0 1 50.50 53.33 17.04 o -11 0 1 527.62 570.10 23.65 o -9 0 1 2765.54 3052.89 67.62 o -7 0 1 3126.00 3472.36 67.09 o -5 0 1 560.20 456.86 10.43 o -3 0 1 20045.18 18960.03 643.24 o -1 0 1 1766.78 1379.92 34.62 o 1 0 1 316.87 280.39 6.05 o 3 0 1 1851.69 1609.18 31.32 o 5 0 1 46.61 39.03 3.85 o 7 0 1 171.56 187.47 9.35 o 9 0 1 987.54 1035.23 25.84 o 11 0 1 19.53 19.24 8.80 o 13 0 1 0.63 7.70 23.64 o 15 0 1 48.18 90.71 28.59 o -14 1 1 44.74 39.32 13.37 o -12 1 1 62.59 42.69 8.48 o -10 1 1 787.94 833.01 19.54 o -8 1 1 714.93 662.52 19.80 o -6 1 1 430.63 566.13 11.81 o -4 1 1 435.42 423.71 6.99 o -2 1 1 147.76 156.64 5.77 o 0 1 1 145.84 199.57 2.50 o 2 1 1 16506.41 15531.28 287.35 o 4 1 1 1700.36 2294.25 30.61 o 6 1 1 654.84 660.19 26.66 o 8 1 1 1965.00 1939.34 47.00 o 10 1 1 326.92 370.25 17.60 o 12 1 1 47.29 58.07 10.08 o 14 1 1 27.78 29.09 16.98 o -15 2 1 50.75 35.24 18.98 o -13 2 1 90.65 100.93 14.02 o -11 2 1 231.24 212.97 10.28 o -9 2 1 925.35 1001.91 19.23 o -7 2 1 2621.12 2440.31 73.40 o -5 2 1 328.54 304.57 6.01 o -3 2 1 8905.61 9783.51 135.64 o -1 2 1 10381.48 9225.41 161.10 o 1 2 1 1752.34 1665.57 27.98 o 3 2 1 53.70 87.16 4.67 o 5 2 1 677.20 434.71 15.12 o 7 2 1 68.39 67.14 3.82 o 9 2 1 48.09 53.51 7.00 o 11 2 1 4.81 7.02 7.97 o 13 2 1 24.10 19.59 16.22 o 15 2 1 26.54 15.83 19.30 o -14 3 1 129.63 127.70 18.30 o -12 3 1 137.27 134.39 14.91 o -10 3 1 55.68 57.37 5.41 o -8 3 1 449.69 430.07 9.89 o -6 3 1 3936.41 3883.35 138.82 o -4 3 1 2393.29 2619.31 37.24 o -2 3 1 4561.96 4373.84 69.52 o 0 3 1 6459.81 6570.47 91.76 o 2 3 1 5459.83 5408.80 98.95 o 4 3 1 3185.81 3231.70 43.86 o 6 3 1 1047.07 1107.58 19.28 o 8 3 1 207.42 215.73 10.68 o 10 3 1 174.11 162.01 9.64 o 12 3 1 118.12 103.95 13.31 o 14 3 1 47.61 66.52 16.20 o -15 4 1 34.47 20.10 18.73 o -13 4 1 158.38 174.91 18.23 o -11 4 1 287.27 304.45 23.64 o -9 4 1 270.08 248.36 22.54 o -7 4 1 414.14 394.79 11.59 o -5 4 1 4220.80 4289.23 92.64 o -3 4 1 5770.98 5104.19 149.26 o -1 4 1 209.93 178.29 4.16 o 1 4 1 4.71 1.65 1.72 o 3 4 1 1345.20 1194.51 18.23 o 5 4 1 1818.52 1809.02 28.66 o 7 4 1 73.17 74.55 8.52 o 9 4 1 22.23 24.45 6.32 o 11 4 1 39.43 48.72 8.45 o 13 4 1 115.28 114.97 34.91 o -14 5 1 103.71 132.26 21.43 o -12 5 1 157.94 119.28 16.24 o -10 5 1 56.15 52.11 11.82 o -8 5 1 162.91 176.97 9.51 o -6 5 1 557.53 618.81 22.81 o -4 5 1 585.98 566.80 11.82 o -2 5 1 317.92 344.38 7.52 o 0 5 1 1720.51 1735.73 24.00 o 2 5 1 49.73 100.93 6.87 o 4 5 1 5424.69 5387.55 78.20 o 6 5 1 4.14 5.75 4.22 o 8 5 1 61.92 64.68 5.99 o 10 5 1 307.62 297.73 16.26 o 12 5 1 89.10 118.90 25.84 o 14 5 1 26.19 -13.02 17.25 o -13 6 1 64.33 71.96 19.04 o -11 6 1 258.88 280.88 23.08 o -9 6 1 578.16 625.23 24.63 o -7 6 1 132.77 128.70 9.05 o -5 6 1 2360.37 2370.76 71.19 o -3 6 1 2858.92 2978.89 53.39 o -1 6 1 736.54 723.09 33.80 o 1 6 1 974.76 931.11 16.40 o 3 6 1 1146.15 1239.74 21.52 o 5 6 1 359.60 327.35 24.74 o 7 6 1 379.10 366.72 25.84 o 9 6 1 42.30 62.87 9.07 o 11 6 1 26.53 25.00 9.64 o 13 6 1 60.46 66.72 22.68 o -14 7 1 34.37 49.11 19.84 o -12 7 1 43.19 44.42 20.64 o -10 7 1 92.89 94.55 12.50 o -8 7 1 665.39 749.00 60.75 o -6 7 1 248.14 246.21 11.82 o -4 7 1 138.25 128.11 7.21 o -2 7 1 1275.46 1315.73 29.14 o 0 7 1 1136.40 1126.26 29.42 o 2 7 1 716.06 791.36 15.03 o 4 7 1 666.94 691.74 14.39 o 6 7 1 42.67 46.04 6.20 o 8 7 1 423.25 452.13 24.19 o 10 7 1 160.07 168.93 29.96 o 12 7 1 25.55 34.71 20.07 o -13 8 1 15.59 18.57 22.54 o -11 8 1 62.73 59.98 17.77 o -9 8 1 262.60 255.27 23.91 o -7 8 1 200.47 210.33 14.90 o -5 8 1 85.07 73.46 11.00 o -3 8 1 103.84 107.19 9.97 o -1 8 1 776.39 801.04 34.37 o 1 8 1 616.04 665.04 18.00 o 3 8 1 4.76 4.40 3.93 o 5 8 1 4.95 -2.47 12.37 o 7 8 1 324.97 358.95 15.99 o 9 8 1 45.92 30.46 11.89 o 11 8 1 8.76 0.98 14.34 o 13 8 1 10.18 -4.89 14.07 o -12 9 1 16.66 -4.61 30.12 o -10 9 1 55.72 72.80 17.54 o -8 9 1 240.56 206.03 15.34 o -6 9 1 138.32 125.94 12.74 o -4 9 1 192.01 166.42 19.52 o -2 9 1 337.93 321.19 15.39 o 0 9 1 985.50 918.67 22.37 o 2 9 1 707.55 725.14 19.56 o 4 9 1 33.53 28.45 7.64 o 6 9 1 82.55 75.73 9.61 o 8 9 1 194.33 202.15 16.06 o 10 9 1 60.11 51.55 19.79 o 12 9 1 11.00 -2.71 20.22 o -11 10 1 36.90 57.66 23.80 o -9 10 1 111.91 108.70 16.65 o -7 10 1 164.50 170.19 45.63 o -5 10 1 158.83 148.77 12.19 o -3 10 1 551.83 655.41 25.84 o -1 10 1 722.41 702.60 26.11 o 1 10 1 392.74 393.07 16.56 o 3 10 1 310.12 371.04 13.98 o 5 10 1 102.59 103.59 10.68 o 7 10 1 85.64 62.06 12.01 o 9 10 1 52.18 36.02 28.04 o 11 10 1 12.82 1.65 19.67 o -10 11 1 27.26 0.31 32.98 o -8 11 1 47.27 51.68 15.90 o -6 11 1 41.81 42.38 24.19 o -4 11 1 139.77 164.31 12.51 o -2 11 1 14.12 21.44 6.78 o 0 11 1 38.06 25.84 7.70 o 2 11 1 199.50 227.38 12.85 o 4 11 1 31.73 27.55 26.39 o 6 11 1 46.83 42.56 11.82 o 8 11 1 52.21 40.04 15.70 o 10 11 1 18.44 1.55 16.38 o -9 12 1 22.35 42.46 19.15 o -7 12 1 56.23 57.57 12.92 o -5 12 1 25.88 31.83 14.57 o -3 12 1 82.63 70.14 14.30 o -1 12 1 22.79 21.44 19.24 o 1 12 1 0.52 0.61 8.72 o 3 12 1 67.58 43.83 10.71 o 5 12 1 77.13 68.76 12.37 o 7 12 1 24.48 28.21 12.06 o 9 12 1 10.02 -12.02 14.03 o -8 13 1 12.94 -22.54 22.54 o -6 13 1 69.34 66.69 15.83 o -4 13 1 83.44 82.94 15.09 o -2 13 1 25.73 32.66 16.77 o 0 13 1 30.03 46.73 12.10 o 2 13 1 60.90 58.40 9.61 o 4 13 1 66.82 62.18 21.99 o 6 13 1 51.96 43.43 16.72 o 8 13 1 8.50 11.94 14.42 o -7 14 1 10.62 -6.96 24.04 o -5 14 1 36.44 55.30 15.96 o -3 14 1 53.24 65.30 19.52 o -1 14 1 30.59 25.29 13.74 o 1 14 1 11.62 19.79 21.99 o 3 14 1 35.76 51.77 16.77 o 5 14 1 40.06 16.71 13.51 o 7 14 1 3.41 -2.99 18.24 o -6 15 1 9.90 -8.95 23.75 o -4 15 1 20.35 0.98 15.09 o -2 15 1 19.64 14.84 15.39 o 0 15 1 19.04 21.44 14.84 o 2 15 1 17.69 21.99 15.94 o 4 15 1 17.68 10.52 17.17 o -1 16 1 15.35 -7.70 16.49 o 1 16 1 14.76 18.69 30.24 o -16 0 2 24.30 28.59 28.04 o -14 0 2 78.61 58.28 20.89 o -12 0 2 26.00 36.29 14.84 o -10 0 2 489.78 463.45 23.65 o -8 0 2 1754.97 1335.41 30.78 o -6 0 2 1072.85 1039.07 24.73 o -4 0 2 280.77 295.23 7.70 o -2 0 2 8823.59 7285.58 151.74 o 0 0 2 11715.75 15499.74 285.34 o 2 0 2 574.04 597.59 12.65 o 4 0 2 75.01 66.52 3.85 o 6 0 2 3.98 4.40 4.95 o 8 0 2 702.58 755.38 19.24 o 10 0 2 92.98 76.97 14.30 o 12 0 2 57.40 58.28 17.04 o 14 0 2 26.72 3.30 28.04 o -15 1 2 28.92 12.92 15.16 o -13 1 2 46.46 55.86 11.23 o -11 1 2 46.08 43.92 6.08 o -9 1 2 479.88 537.03 10.96 o -7 1 2 1480.54 1502.73 22.53 o -5 1 2 8.50 15.94 2.33 o -3 1 2 3532.27 2846.34 40.78 o -1 1 2 32334.68 29793.64 882.89 o 1 1 2 418.67 342.62 6.04 o 3 1 2 379.67 265.42 5.01 o 5 1 2 1363.56 1384.65 21.45 o 7 1 2 786.97 818.95 17.44 o 9 1 2 354.49 334.37 12.10 o 11 1 2 119.18 103.26 12.42 o 13 1 2 9.48 2.12 15.31 o -14 2 2 68.13 40.84 12.42 o -12 2 2 165.70 152.44 16.49 o -10 2 2 317.22 311.55 24.75 o -8 2 2 59.77 56.63 6.32 o -6 2 2 71.84 83.76 5.22 o -4 2 2 325.37 292.67 6.60 o -2 2 2 2431.31 2037.57 30.52 o 0 2 2 5332.23 5335.36 108.86 o 2 2 2 31.31 45.46 5.50 o 4 2 2 118.29 108.23 4.12 o 6 2 2 8.09 -0.55 5.50 o 8 2 2 180.76 220.44 9.24 o 10 2 2 148.72 140.54 9.64 o 12 2 2 101.71 73.13 11.88 o 14 2 2 29.87 -1.70 38.76 o -15 3 2 23.47 -0.83 16.86 o -13 3 2 111.53 90.30 12.98 o -11 3 2 195.09 183.20 12.81 o -9 3 2 227.51 322.48 11.66 o -7 3 2 156.57 183.26 11.55 o -5 3 2 2104.06 2023.83 34.67 o -3 3 2 996.93 984.93 31.88 o -1 3 2 39.65 42.48 2.47 o 1 3 2 972.42 941.37 13.94 o 3 3 2 3135.90 3531.16 75.87 o 5 3 2 1666.04 1744.32 27.70 o 7 3 2 820.52 781.02 16.46 o 9 3 2 226.85 251.62 11.47 o 11 3 2 122.92 121.30 11.88 o 13 3 2 44.71 68.51 14.98 o -14 4 2 44.61 57.62 19.21 o -12 4 2 321.78 351.19 30.52 o -10 4 2 95.30 67.51 9.11 o -8 4 2 3.44 13.39 5.40 o -6 4 2 1699.51 1808.01 50.58 o -4 4 2 2669.58 2301.95 36.82 o -2 4 2 141.69 125.72 3.75 o 0 4 2 37.80 44.30 2.33 o 2 4 2 162.17 179.91 14.84 o 4 4 2 1148.01 1192.33 27.77 o 6 4 2 518.27 578.83 16.20 o 8 4 2 26.98 26.03 6.31 o 10 4 2 120.62 104.12 13.47 o 12 4 2 149.26 145.53 16.55 o 14 4 2 31.26 14.39 14.79 o -15 5 2 17.23 33.49 19.23 o -13 5 2 62.39 63.44 20.63 o -11 5 2 78.93 65.34 12.24 o -9 5 2 70.49 64.54 12.37 o -7 5 2 77.16 74.85 7.42 o -5 5 2 722.29 793.76 15.74 o -3 5 2 1065.72 1063.32 18.81 o -1 5 2 44.89 56.56 3.15 o 1 5 2 1487.43 1419.28 40.96 o 3 5 2 321.91 367.97 16.76 o 5 5 2 325.76 367.59 19.80 o 7 5 2 404.60 428.69 14.39 o 9 5 2 37.32 31.59 7.26 o 11 5 2 55.23 41.63 10.56 o 13 5 2 53.74 40.19 48.93 o -14 6 2 17.08 27.89 24.11 o -12 6 2 192.85 203.62 22.05 o -10 6 2 46.79 34.85 9.86 o -8 6 2 54.61 62.32 8.52 o -6 6 2 1176.83 1089.11 23.21 o -4 6 2 684.57 720.62 17.89 o -2 6 2 417.45 429.34 17.04 o 0 6 2 1187.80 1154.35 18.96 o 2 6 2 9.40 14.90 3.04 o 4 6 2 630.13 656.13 27.76 o 6 6 2 444.73 444.55 15.66 o 8 6 2 24.25 15.67 7.00 o 10 6 2 152.15 155.01 11.23 o 12 6 2 77.42 98.21 26.66 o -13 7 2 9.66 38.72 15.85 o -11 7 2 119.64 145.65 26.66 o -9 7 2 200.50 193.33 13.70 o -7 7 2 109.89 89.54 5.77 o -5 7 2 242.89 214.94 9.59 o -3 7 2 1035.62 1017.96 23.24 o -1 7 2 571.09 536.67 16.08 o 1 7 2 1551.10 1385.29 41.23 o 3 7 2 401.26 455.56 32.43 o 5 7 2 218.07 258.88 10.43 o 7 7 2 250.78 249.31 31.61 o 9 7 2 206.39 239.98 26.39 o 11 7 2 28.73 22.48 13.30 o 13 7 2 11.67 -15.01 29.41 o -12 8 2 31.42 118.10 32.70 o -10 8 2 136.21 157.23 20.34 o -8 8 2 143.67 135.88 14.84 o -6 8 2 56.57 50.61 16.22 o -4 8 2 5.59 12.99 7.70 o -2 8 2 260.79 236.78 11.55 o 0 8 2 236.83 214.27 23.09 o 2 8 2 17.31 4.73 6.87 o 4 8 2 137.39 145.04 7.66 o 6 8 2 38.16 33.51 7.91 o 8 8 2 84.44 64.35 11.47 o 10 8 2 105.72 105.81 15.71 o 12 8 2 8.12 21.16 15.46 o -13 9 2 1.63 3.43 25.36 o -11 9 2 34.85 16.84 20.62 o -9 9 2 206.30 169.06 24.46 o -7 9 2 183.61 186.58 14.16 o -5 9 2 2.02 6.45 4.25 o -3 9 2 45.82 30.88 7.72 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