#------------------------------------------------------------------------------ #$Date: 2012-01-03 14:54:16 +0200 (Tue, 03 Jan 2012) $ #$Revision: 31968 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/10/49/2104999.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_2104999_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 101.550 _cell_angle_gamma 90.000 _cell_length_a 11.9550 _cell_length_b 12.6920 _cell_length_c 15.9880 _exptl_crystal_F_000 1160.00 _reflns_d_resolution_high 0.7702 _[local]_cod_data_source_file hw5018100K_IVsup7.hkl _[local]_cod_data_source_block 100K_IV #BEGIN Tags that were not found in dictionaries: _shelx_title ' k06178 in P2(1)/c' _shelx_refln_list_code 4 _shelx_f_calc_maximum 353.37 _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 0 776.55 771.64 10.57 o 2 0 0 18925.06 17709.55 262.14 o 3 0 0 59.36 40.17 4.23 o 4 0 0 6247.49 6450.02 101.48 o 5 0 0 905.38 1042.24 23.25 o 6 0 0 57234.74 59210.85 909.05 o 7 0 0 3.77 10.57 10.57 o 8 0 0 7686.48 7669.84 147.98 o 9 0 0 1372.58 1462.94 54.97 o 10 0 0 3257.48 3718.65 112.05 o 11 0 0 17.33 -12.68 23.25 o 12 0 0 314.80 315.00 38.05 o 13 0 0 47.39 54.97 31.71 o 14 0 0 726.61 860.43 101.48 o 15 0 0 1335.73 1367.80 133.19 o 1 1 0 26335.58 23816.88 301.08 o 2 1 0 19.47 16.49 3.17 o 3 1 0 4649.95 4410.79 45.43 o 4 1 0 354.25 345.23 14.80 o 5 1 0 6685.22 6321.30 77.16 o 6 1 0 3722.21 3652.65 71.88 o 7 1 0 4427.66 4267.59 61.31 o 8 1 0 6153.33 6651.47 94.18 o 9 1 0 3937.27 3819.69 70.43 o 10 1 0 242.86 167.97 16.44 o 11 1 0 1150.52 1236.25 39.09 o 12 1 0 922.97 1003.67 46.09 o 13 1 0 28.98 -28.01 29.45 o 14 1 0 14.00 20.30 38.70 o 15 1 0 197.43 108.96 57.78 o 0 2 0 55693.59 51325.37 1976.65 o 1 2 0 77.17 84.62 2.99 o 2 2 0 514.95 473.94 8.12 o 3 2 0 343.54 316.14 7.47 o 4 2 0 6781.12 6803.83 74.03 o 5 2 0 927.77 883.61 19.03 o 6 2 0 7113.57 7146.34 77.18 o 7 2 0 2.38 2.11 6.60 o 8 2 0 1830.54 1868.17 37.01 o 9 2 0 1219.35 1252.22 33.61 o 10 2 0 1760.10 1766.38 45.69 o 11 2 0 816.57 866.77 36.76 o 12 2 0 391.92 338.19 28.14 o 13 2 0 227.86 225.24 45.58 o 14 2 0 364.08 312.38 50.74 o 15 2 0 493.15 354.37 70.36 o 1 3 0 335.45 366.44 7.40 o 2 3 0 223.55 219.94 5.98 o 3 3 0 52488.82 49518.54 528.87 o 4 3 0 14045.41 15230.14 157.58 o 5 3 0 16845.03 16150.94 172.77 o 6 3 0 1295.93 1267.47 19.81 o 7 3 0 3440.24 3409.17 50.27 o 8 3 0 3718.58 4037.45 58.90 o 9 3 0 2266.82 2295.40 61.31 o 10 3 0 2685.86 2684.38 64.96 o 11 3 0 3089.38 3252.11 77.03 o 12 3 0 333.03 304.41 27.77 o 13 3 0 1025.17 952.97 182.87 o 14 3 0 309.59 245.34 47.56 o 0 4 0 2536.74 2316.93 38.59 o 1 4 0 11.09 12.85 2.99 o 2 4 0 46918.36 46568.62 545.70 o 3 4 0 1312.46 1324.22 18.64 o 4 4 0 28748.12 29519.44 289.72 o 5 4 0 9994.56 10941.76 114.38 o 6 4 0 3164.58 3011.74 42.13 o 7 4 0 42.72 39.84 8.12 o 8 4 0 1801.63 1923.58 35.50 o 9 4 0 19.30 30.65 11.68 o 10 4 0 842.44 852.96 73.99 o 11 4 0 2643.23 2769.76 84.78 o 12 4 0 1827.00 2022.52 103.59 o 13 4 0 600.77 573.64 48.72 o 14 4 0 556.21 453.98 104.65 o 1 5 0 1662.13 1691.56 21.11 o 2 5 0 50.04 50.23 5.07 o 3 5 0 4186.18 3890.10 45.43 o 4 5 0 7779.28 8129.11 87.86 o 5 5 0 5643.88 5470.97 65.57 o 6 5 0 26.52 12.68 7.47 o 7 5 0 1953.05 2055.76 47.57 o 8 5 0 673.64 691.79 46.51 o 9 5 0 327.41 304.25 15.64 o 10 5 0 3179.08 3412.20 86.68 o 11 5 0 1261.49 1182.50 116.27 o 12 5 0 34.38 13.68 24.25 o 13 5 0 543.85 450.98 101.48 o 14 5 0 948.60 1006.83 98.30 o 0 6 0 6435.76 6397.63 176.52 o 1 6 0 877.46 891.30 13.68 o 2 6 0 29474.11 30377.99 342.69 o 3 6 0 1238.17 1333.65 27.48 o 4 6 0 10060.08 10200.99 156.44 o 5 6 0 881.78 910.56 21.45 o 6 6 0 5328.73 5592.94 79.78 o 7 6 0 31.94 20.69 20.08 o 8 6 0 1000.42 1051.36 30.08 o 9 6 0 223.03 161.11 21.14 o 10 6 0 829.13 900.03 48.62 o 11 6 0 1576.10 1669.42 61.29 o 12 6 0 831.33 775.99 46.05 o 13 6 0 554.39 463.76 100.42 o 14 6 0 61.12 26.36 46.74 o 1 7 0 14514.06 15511.19 243.12 o 2 7 0 9.31 11.98 5.67 o 3 7 0 4839.99 4838.03 88.79 o 4 7 0 387.30 365.62 28.54 o 5 7 0 9135.74 9808.61 235.72 o 6 7 0 46.10 34.09 10.57 o 7 7 0 5385.70 5553.40 96.58 o 8 7 0 350.57 331.38 20.73 o 9 7 0 955.11 930.30 35.04 o 10 7 0 1449.45 1551.41 115.22 o 11 7 0 1652.91 1801.25 67.55 o 12 7 0 9.26 6.02 40.17 o 13 7 0 106.31 55.45 48.15 o 0 8 0 7308.15 7573.88 145.29 o 1 8 0 120.86 97.25 8.60 o 2 8 0 1892.21 1898.33 31.27 o 3 8 0 940.88 987.73 20.60 o 4 8 0 81.83 71.64 17.97 o 5 8 0 473.27 465.60 19.03 o 6 8 0 1598.32 1608.78 35.53 o 7 8 0 2177.27 2319.92 64.48 o 8 8 0 489.18 428.49 23.66 o 9 8 0 1358.99 1299.51 54.77 o 10 8 0 906.22 920.20 88.79 o 11 8 0 221.10 137.54 39.62 o 12 8 0 3.80 35.45 48.15 o 13 8 0 436.39 571.44 246.29 o 1 9 0 5637.59 5988.38 84.20 o 2 9 0 1148.00 1182.84 26.06 o 3 9 0 52.74 22.35 9.51 o 4 9 0 861.26 912.62 57.08 o 5 9 0 345.61 354.59 12.24 o 6 9 0 982.16 920.01 68.71 o 7 9 0 1674.90 1676.80 105.70 o 8 9 0 1997.12 1949.23 81.39 o 9 9 0 1467.55 1359.29 76.11 o 10 9 0 855.90 793.38 114.16 o 11 9 0 173.40 165.27 85.62 o 12 9 0 5.87 -31.38 66.27 o 0 10 0 10043.52 10304.45 227.36 o 1 10 0 152.14 127.22 38.05 o 2 10 0 380.88 367.55 17.61 o 3 10 0 65.93 55.78 17.93 o 4 10 0 186.71 193.65 21.45 o 5 10 0 113.56 99.52 20.73 o 6 10 0 2237.50 2237.78 67.65 o 7 10 0 1002.41 979.79 43.51 o 8 10 0 625.33 685.03 139.53 o 9 10 0 644.29 592.92 83.51 o 10 10 0 826.92 849.68 57.78 o 11 10 0 32.69 143.34 65.70 o 12 10 0 32.31 -26.53 51.80 o 1 11 0 2934.70 3100.16 66.21 o 2 11 0 225.03 194.10 23.25 o 3 11 0 194.61 208.63 46.51 o 4 11 0 46.86 43.30 19.16 o 5 11 0 1826.33 1805.25 58.14 o 6 11 0 211.17 184.26 40.17 o 7 11 0 339.73 310.98 40.12 o 8 11 0 32.70 17.57 32.43 o 9 11 0 267.64 161.65 40.93 o 10 11 0 254.15 284.56 136.36 o 11 11 0 98.85 -11.38 57.78 o 0 12 0 439.54 418.55 32.48 o 1 12 0 184.56 134.42 31.71 o 2 12 0 473.71 399.59 27.19 o 3 12 0 31.24 39.84 20.60 o 4 12 0 2687.46 2729.87 82.85 o 5 12 0 661.61 539.58 39.62 o 6 12 0 326.34 255.26 48.62 o 7 12 0 142.38 119.20 36.76 o 8 12 0 55.83 70.77 53.91 o 9 12 0 196.22 131.11 43.93 o 10 12 0 61.85 99.66 47.11 o 1 13 0 1918.02 1987.73 78.10 o 2 13 0 353.44 322.03 31.29 o 3 13 0 2710.92 2724.23 109.93 o 4 13 0 412.35 385.63 124.73 o 5 13 0 2246.46 2258.36 81.77 o 6 13 0 50.16 21.85 33.02 o 7 13 0 195.57 230.35 42.58 o 8 13 0 0.93 9.84 39.69 o 9 13 0 129.48 24.09 56.02 o 0 14 0 210.08 223.68 103.59 o 1 14 0 53.40 6.16 48.01 o 2 14 0 270.96 288.80 60.62 o 3 14 0 290.09 298.13 58.69 o 4 14 0 915.92 814.93 63.42 o 5 14 0 113.22 116.99 37.12 o 6 14 0 55.91 99.81 87.73 o 7 14 0 5.66 -24.28 84.56 o 8 14 0 163.80 199.12 47.56 o 1 15 0 12.63 -24.22 50.74 o 2 15 0 20.33 22.12 50.06 o 3 15 0 51.27 85.59 59.74 o 4 15 0 231.62 315.80 77.64 o 5 15 0 13.75 39.92 63.20 o 6 15 0 32.75 80.96 68.72 o 0 16 0 394.93 448.70 110.10 o 1 16 0 57.05 -41.66 52.67 o 2 16 0 71.36 39.36 62.54 o 3 16 0 17.68 -68.23 68.23 o -15 1 1 24.10 16.34 76.11 o -14 1 1 2.44 19.03 31.39 o -13 1 1 265.98 247.89 32.79 o -12 1 1 20.80 -3.76 19.81 o -11 1 1 1.01 13.26 16.91 o -10 1 1 568.08 569.38 24.89 o -9 1 1 17.21 19.42 11.68 o -8 1 1 4.64 15.86 8.97 o -7 1 1 87.91 75.48 8.12 o -6 1 1 2651.43 2917.51 35.11 o -5 1 1 102.08 96.70 5.07 o -4 1 1 791.78 807.69 14.80 o -3 1 1 54.19 35.68 5.29 o -2 1 1 0.41 1.06 1.49 o -1 1 1 129.45 126.99 4.23 o 0 1 1 224.82 200.84 2.99 o 1 1 1 125.35 121.57 2.99 o 2 1 1 52.84 35.28 3.17 o 3 1 1 776.67 779.05 11.96 o 4 1 1 195.13 187.06 6.60 o 5 1 1 188.55 206.82 8.12 o 6 1 1 40.39 32.82 7.40 o 7 1 1 0.36 -8.12 8.12 o 8 1 1 217.35 172.26 24.31 o 9 1 1 3101.92 3421.80 87.73 o 10 1 1 51.27 21.14 14.14 o 11 1 1 269.53 221.90 20.77 o 12 1 1 20.86 2.84 21.33 o 13 1 1 84.51 59.73 34.54 o 14 1 1 0.37 -18.69 41.65 o 15 1 1 412.36 358.08 67.27 o -15 2 1 191.75 186.78 56.38 o -14 2 1 30.14 57.04 40.12 o -13 2 1 199.69 189.14 64.48 o -12 2 1 44.17 30.69 21.33 o -11 2 1 148.58 114.75 17.75 o -10 2 1 467.15 454.84 23.13 o -9 2 1 1165.61 1199.68 31.91 o -8 2 1 123.59 113.04 11.14 o -7 2 1 996.36 1042.41 18.29 o -6 2 1 1818.92 2086.64 27.77 o -5 2 1 63.00 56.15 5.44 o -4 2 1 7.46 2.54 3.52 o -3 2 1 1091.60 1015.09 14.14 o -2 2 1 45.44 32.80 2.99 o -1 2 1 109.32 102.63 3.17 o 0 2 1 837.73 771.32 9.63 o 1 2 1 66.09 53.76 6.34 o 2 2 1 1058.29 1065.49 14.14 o 3 2 1 115.89 97.66 6.34 o 4 2 1 62.02 78.29 10.57 o 5 2 1 355.08 394.44 9.63 o 6 2 1 11.12 11.63 5.98 o 7 2 1 682.96 675.82 19.43 o 8 2 1 521.12 519.02 17.94 o 9 2 1 13.44 15.58 21.14 o 10 2 1 889.84 897.75 31.29 o 11 2 1 112.91 93.72 19.16 o 12 2 1 3.87 -11.98 20.80 o 13 2 1 77.60 34.91 30.40 o 14 2 1 27.11 21.88 44.18 o -15 3 1 163.88 131.82 63.20 o -14 3 1 37.27 43.05 53.91 o -13 3 1 576.34 462.07 48.62 o -12 3 1 176.46 129.36 42.28 o -11 3 1 308.21 303.12 24.31 o -10 3 1 261.17 204.45 16.44 o -9 3 1 258.00 259.31 15.64 o -8 3 1 181.01 148.99 10.55 o -7 3 1 570.99 568.07 14.07 o -6 3 1 156.69 178.86 11.63 o -5 3 1 315.59 322.04 8.96 o -4 3 1 1044.11 972.25 14.14 o -3 3 1 94.48 71.58 7.40 o -2 3 1 410.24 434.72 11.63 o -1 3 1 351.66 364.01 6.60 o 0 3 1 657.78 597.23 8.97 o 1 3 1 555.78 499.50 9.63 o 2 3 1 3437.21 3392.04 41.86 o 3 3 1 5.04 13.11 3.52 o 4 3 1 831.40 811.00 20.08 o 5 3 1 996.54 1002.94 29.60 o 6 3 1 70.65 82.90 12.68 o 7 3 1 11.45 4.23 7.04 o 8 3 1 259.29 245.03 14.14 o 9 3 1 117.77 85.10 14.80 o 10 3 1 702.38 692.48 46.51 o 11 3 1 716.58 695.41 95.13 o 12 3 1 87.74 85.31 73.99 o 13 3 1 120.35 122.94 46.51 o 14 3 1 23.57 -22.30 83.51 o -14 4 1 74.97 54.06 58.14 o -13 4 1 358.41 282.14 41.09 o -12 4 1 185.69 159.12 39.11 o -11 4 1 1758.40 1915.39 52.67 o -10 4 1 552.66 533.92 21.64 o -9 4 1 336.30 346.07 17.14 o -8 4 1 255.14 262.38 13.68 o -7 4 1 97.62 92.45 8.60 o -6 4 1 2.88 3.44 5.44 o -5 4 1 1697.19 1649.82 21.33 o -4 4 1 43.27 30.69 5.98 o -3 4 1 1881.31 1765.10 21.64 o -2 4 1 2004.33 1939.59 24.36 o -1 4 1 36.97 27.65 2.99 o 0 4 1 6.38 4.23 2.99 o 1 4 1 906.83 902.96 12.64 o 2 4 1 4009.24 3967.74 45.14 o 3 4 1 1089.05 1051.73 17.14 o 4 4 1 3335.05 3511.34 40.60 o 5 4 1 262.30 228.58 8.96 o 6 4 1 1994.18 2063.35 36.06 o 7 4 1 1168.05 1266.84 25.28 o 8 4 1 27.49 3.98 13.74 o 9 4 1 430.72 414.36 23.36 o 10 4 1 83.83 61.61 27.48 o 11 4 1 191.65 164.42 24.17 o 12 4 1 461.89 436.26 40.59 o 13 4 1 2.84 41.01 33.83 o 14 4 1 1.40 38.77 60.83 o -14 5 1 530.18 459.16 49.93 o -13 5 1 30.18 83.62 33.02 o -12 5 1 18.72 -1.15 41.22 o -11 5 1 0.91 -7.10 18.64 o -10 5 1 807.02 854.54 29.72 o -9 5 1 436.79 441.71 18.29 o -8 5 1 2338.89 2483.55 44.97 o -7 5 1 147.36 146.07 10.15 o -6 5 1 41.86 20.30 8.46 o -5 5 1 4.82 7.40 5.98 o -4 5 1 2896.74 3143.12 38.52 o -3 5 1 71.43 52.64 10.57 o -2 5 1 2957.03 3056.01 33.98 o -1 5 1 307.05 285.40 8.60 o 0 5 1 498.69 427.03 8.60 o 1 5 1 291.16 235.66 6.60 o 2 5 1 5092.08 5218.87 60.42 o 3 5 1 1548.34 1638.13 24.31 o 4 5 1 5088.09 5592.89 71.75 o 5 5 1 1.36 1.69 13.74 o 6 5 1 143.88 145.25 10.57 o 7 5 1 163.13 139.19 13.21 o 8 5 1 1019.74 1088.87 33.41 o 9 5 1 1025.74 1035.68 39.59 o 10 5 1 133.22 93.61 18.75 o 11 5 1 6.02 -2.85 17.14 o 12 5 1 15.80 -10.77 29.72 o 13 5 1 509.35 418.85 44.15 o 14 5 1 21.86 12.77 54.74 o -14 6 1 68.04 30.02 60.25 o -13 6 1 129.01 107.82 58.14 o -12 6 1 1132.31 1293.38 56.81 o -11 6 1 646.96 700.78 63.42 o -10 6 1 160.23 167.01 20.30 o -9 6 1 8.36 8.46 11.14 o -8 6 1 10.90 -1.41 8.60 o -7 6 1 125.52 111.78 11.63 o -6 6 1 284.30 266.57 12.64 o -5 6 1 7865.79 8462.84 219.86 o -4 6 1 454.49 448.18 13.45 o -3 6 1 172.77 122.16 10.57 o -2 6 1 3285.59 3448.08 38.59 o -1 6 1 717.99 674.59 12.12 o 0 6 1 320.25 402.36 9.63 o 1 6 1 1750.39 1793.68 21.83 o 2 6 1 2704.17 2776.61 72.94 o 3 6 1 832.38 818.36 17.75 o 4 6 1 2704.17 2760.25 54.97 o 5 6 1 1069.13 1072.99 29.60 o 6 6 1 328.24 300.64 16.91 o 7 6 1 48.95 29.60 7.85 o 8 6 1 82.21 62.01 14.80 o 9 6 1 2045.85 2123.18 61.29 o 10 6 1 2393.32 2483.76 109.93 o 11 6 1 274.35 251.23 29.12 o 12 6 1 91.15 56.02 60.25 o 13 6 1 22.62 13.07 47.65 o -13 7 1 74.29 65.08 64.42 o -12 7 1 18.03 7.93 32.79 o -11 7 1 8.69 45.24 24.63 o -10 7 1 75.11 77.81 22.28 o -9 7 1 378.30 370.21 27.48 o -8 7 1 3296.17 3549.80 63.81 o -7 7 1 2806.80 2979.58 50.83 o -6 7 1 58.96 40.17 9.63 o -5 7 1 815.71 770.20 25.28 o -4 7 1 14.69 8.26 8.46 o -3 7 1 182.25 196.04 10.88 o -2 7 1 6763.70 7003.75 171.24 o -1 7 1 941.87 945.26 16.00 o 0 7 1 1065.48 954.92 16.76 o 1 7 1 744.67 677.54 21.14 o 2 7 1 858.04 844.53 18.29 o 3 7 1 345.66 353.88 14.73 o 4 7 1 1895.69 2043.56 32.01 o 5 7 1 538.18 532.01 15.30 o 6 7 1 107.11 85.82 11.35 o 7 7 1 1323.35 1386.25 34.41 o 8 7 1 222.44 171.36 17.93 o 9 7 1 19.57 19.03 16.00 o 10 7 1 162.37 154.32 35.10 o 11 7 1 238.98 240.94 36.37 o 12 7 1 59.22 94.08 46.34 o 13 7 1 235.97 174.21 54.35 o -13 8 1 1.81 8.00 57.30 o -12 8 1 332.46 311.90 93.02 o -11 8 1 561.94 529.42 47.21 o -10 8 1 170.53 132.75 43.34 o -9 8 1 675.27 555.61 29.79 o -8 8 1 894.90 851.63 31.51 o -7 8 1 28.82 -0.53 13.03 o -6 8 1 172.05 163.92 15.86 o -5 8 1 861.34 906.20 24.58 o -4 8 1 188.49 155.83 11.78 o -3 8 1 199.91 207.16 37.00 o -2 8 1 147.91 129.23 8.96 o -1 8 1 1279.51 1260.93 23.37 o 0 8 1 2196.68 2355.49 32.43 o 1 8 1 265.26 251.39 10.55 o 2 8 1 2515.27 2707.25 46.93 o 3 8 1 173.89 146.16 13.21 o 4 8 1 748.96 742.95 31.71 o 5 8 1 600.75 649.08 20.08 o 6 8 1 1489.39 1449.31 32.01 o 7 8 1 80.43 68.15 13.21 o 8 8 1 2245.95 2518.86 64.23 o 9 8 1 450.13 446.79 30.97 o 10 8 1 2085.11 2277.44 135.30 o 11 8 1 130.23 169.01 82.45 o 12 8 1 212.72 237.59 48.25 o 13 8 1 20.44 12.16 47.77 o -12 9 1 5.68 -60.25 60.25 o -11 9 1 55.27 56.41 35.11 o -10 9 1 317.83 308.28 99.36 o -9 9 1 57.17 20.80 26.20 o -8 9 1 1187.17 1315.86 57.42 o -7 9 1 26.93 18.32 13.24 o -6 9 1 472.10 407.44 38.05 o -5 9 1 376.38 330.00 15.59 o -4 9 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