#------------------------------------------------------------------------------ #$Date: 2016-04-02 23:02:37 +0300 (Sat, 02 Apr 2016) $ #$Revision: 180909 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/10/50/2105003.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_2105003_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 101.500 _cell_angle_gamma 90.000 _cell_length_a 12.0080 _cell_length_b 12.6810 _cell_length_c 16.0100 _exptl_crystal_F_000 1160.00 _reflns_d_resolution_high 0.7705 _cod_data_source_file hw5018140K_IVsup11.hkl _cod_data_source_block 140K_IV #BEGIN Tags that were not found in dictionaries: _shelx_title ' k06182 in P2(1)/c' _shelx_refln_list_code 4 _shelx_f_calc_maximum 353.84 _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 0 743.89 735.14 11.38 o 2 0 0 18770.40 18146.24 286.77 o 3 0 0 21.00 13.66 4.55 o 4 0 0 5966.17 6247.51 91.04 o 5 0 0 970.58 1117.50 22.76 o 6 0 0 54707.07 58321.52 842.11 o 7 0 0 7.19 9.10 11.38 o 8 0 0 7475.50 7722.34 147.94 o 9 0 0 1301.74 1381.51 52.35 o 10 0 0 2866.58 3220.49 97.87 o 11 0 0 9.57 -2.28 20.48 o 12 0 0 326.86 355.05 38.69 o 13 0 0 82.15 70.55 36.42 o 14 0 0 500.61 457.47 63.73 o 15 0 0 795.54 965.01 113.80 o 1 1 0 26922.38 24386.99 320.42 o 2 1 0 27.02 19.95 3.41 o 3 1 0 4711.03 4489.69 49.07 o 4 1 0 364.85 357.34 8.05 o 5 1 0 6099.49 5836.07 64.13 o 6 1 0 3078.05 2952.81 34.57 o 7 1 0 4369.37 4295.89 54.72 o 8 1 0 5072.04 5630.33 79.65 o 9 1 0 3644.74 3553.59 127.45 o 10 1 0 183.24 129.50 18.46 o 11 1 0 1007.99 1064.23 39.83 o 12 1 0 640.39 677.84 32.96 o 13 1 0 32.10 10.28 34.14 o 14 1 0 4.63 26.39 29.74 o 15 1 0 169.57 120.63 56.33 o 0 2 0 55262.39 51373.88 1396.30 o 1 2 0 56.46 60.60 2.28 o 2 2 0 488.43 434.89 7.11 o 3 2 0 317.06 310.59 7.11 o 4 2 0 7049.68 7286.18 77.74 o 5 2 0 983.50 943.92 16.84 o 6 2 0 7302.72 7598.75 84.48 o 7 2 0 2.11 0.00 8.05 o 8 2 0 2119.88 2287.37 63.73 o 9 2 0 1130.98 1152.04 42.11 o 10 2 0 1836.28 1931.52 51.95 o 11 2 0 721.56 627.82 31.71 o 12 2 0 478.54 457.60 33.34 o 13 2 0 236.97 206.90 30.45 o 14 2 0 345.70 271.62 43.36 o 15 2 0 351.54 214.62 61.57 o 1 3 0 322.86 335.68 12.52 o 2 3 0 143.48 150.21 4.83 o 3 3 0 51610.26 49008.14 510.28 o 4 3 0 12597.22 13501.02 135.19 o 5 3 0 16412.27 16430.33 170.50 o 6 3 0 1178.85 1165.33 19.31 o 7 3 0 2957.51 3045.28 43.71 o 8 3 0 2917.78 3270.19 84.21 o 9 3 0 1908.38 1935.72 43.45 o 10 3 0 1992.47 1924.92 88.76 o 11 3 0 2629.29 2870.55 71.57 o 12 3 0 248.05 203.39 32.77 o 13 3 0 804.54 763.24 53.49 o 14 3 0 205.86 190.61 42.08 o 15 3 0 127.18 180.88 56.28 o 0 4 0 2456.54 2281.05 72.83 o 1 4 0 12.21 11.38 3.79 o 2 4 0 45373.17 45081.21 504.13 o 3 4 0 1156.79 1154.02 16.09 o 4 4 0 27742.78 29037.31 290.94 o 5 4 0 9423.38 10467.85 118.35 o 6 4 0 3172.26 3084.71 42.62 o 7 4 0 47.00 41.62 7.57 o 8 4 0 1849.93 2082.42 39.83 o 9 4 0 30.54 13.33 9.95 o 10 4 0 706.80 735.96 32.77 o 11 4 0 2287.42 2352.80 67.25 o 12 4 0 1572.84 1644.16 64.86 o 13 4 0 431.34 363.06 44.38 o 14 4 0 495.92 433.27 52.82 o 1 5 0 1702.30 1688.11 28.45 o 2 5 0 38.44 30.29 4.83 o 3 5 0 4028.78 3802.07 42.62 o 4 5 0 6676.05 7141.75 73.11 o 5 5 0 5863.12 5929.23 66.77 o 6 5 0 42.66 25.95 7.57 o 7 5 0 1954.84 2081.84 39.37 o 8 5 0 572.19 517.74 42.11 o 9 5 0 283.12 253.45 23.90 o 10 5 0 2344.79 2463.40 66.85 o 11 5 0 1132.18 1113.91 85.35 o 12 5 0 23.90 38.49 25.16 o 13 5 0 530.72 484.66 45.06 o 14 5 0 646.11 669.96 125.18 o 0 6 0 6522.13 6517.39 126.32 o 1 6 0 882.07 901.28 15.23 o 2 6 0 28621.34 29683.15 391.47 o 3 6 0 1167.34 1277.02 36.42 o 4 6 0 9554.96 9857.38 117.35 o 5 6 0 767.37 814.49 26.17 o 6 6 0 5063.99 5255.71 73.21 o 7 6 0 55.12 26.17 9.26 o 8 6 0 1096.71 1163.74 34.43 o 9 6 0 167.19 114.96 24.80 o 10 6 0 731.36 676.77 89.90 o 11 6 0 1329.88 1406.39 142.25 o 12 6 0 758.94 679.07 45.35 o 13 6 0 374.09 359.40 55.09 o 14 6 0 81.42 54.25 42.51 o 1 7 0 13451.96 14306.19 261.74 o 2 7 0 11.66 9.10 9.10 o 3 7 0 4310.28 4279.36 54.67 o 4 7 0 288.26 283.52 10.92 o 5 7 0 8223.14 8757.17 123.14 o 6 7 0 38.68 54.03 15.93 o 7 7 0 4627.28 4870.48 85.19 o 8 7 0 287.04 241.45 18.94 o 9 7 0 774.36 686.51 41.01 o 10 7 0 1070.67 1065.50 110.38 o 11 7 0 1323.79 1437.04 143.39 o 12 7 0 6.50 -13.91 34.91 o 13 7 0 81.15 40.97 43.45 o 0 8 0 6801.63 7011.48 131.36 o 1 8 0 101.23 84.96 10.37 o 2 8 0 1869.15 1829.77 29.89 o 3 8 0 899.46 948.84 23.90 o 4 8 0 95.78 112.89 11.38 o 5 8 0 489.06 509.90 16.84 o 6 8 0 1380.42 1461.47 35.28 o 7 8 0 1805.72 1912.08 88.76 o 8 8 0 509.47 498.46 30.67 o 9 8 0 1079.49 945.04 50.82 o 10 8 0 948.59 982.92 52.50 o 11 8 0 226.32 211.82 34.91 o 12 8 0 3.93 13.34 46.66 o 13 8 0 282.25 206.94 57.11 o 1 9 0 5105.47 5412.79 88.76 o 2 9 0 941.22 979.85 38.69 o 3 9 0 33.25 33.30 9.95 o 4 9 0 777.89 823.41 25.04 o 5 9 0 363.80 373.03 17.23 o 6 9 0 851.93 858.54 36.18 o 7 9 0 1554.00 1529.39 45.34 o 8 9 0 1639.93 1679.37 57.55 o 9 9 0 1291.35 1214.55 84.21 o 10 9 0 657.14 527.85 54.31 o 11 9 0 177.02 156.81 42.72 o 12 9 0 2.93 35.11 54.62 o 0 10 0 9319.08 9494.12 232.23 o 1 10 0 115.02 109.06 14.25 o 2 10 0 444.12 447.45 28.45 o 3 10 0 53.23 50.50 18.21 o 4 10 0 171.00 192.37 20.74 o 5 10 0 49.96 35.28 17.70 o 6 10 0 2023.15 2051.71 62.52 o 7 10 0 775.23 777.42 40.38 o 8 10 0 523.04 479.04 42.51 o 9 10 0 438.45 367.06 53.75 o 10 10 0 656.74 633.50 70.52 o 11 10 0 22.15 20.99 46.48 o 12 10 0 42.49 33.10 47.46 o 1 11 0 2258.00 2402.08 58.04 o 2 11 0 224.69 198.32 25.04 o 3 11 0 161.66 136.43 23.29 o 4 11 0 46.38 35.73 15.85 o 5 11 0 1512.09 1613.88 54.65 o 6 11 0 169.46 170.12 70.55 o 7 11 0 295.41 204.88 41.01 o 8 11 0 30.31 5.69 30.58 o 9 11 0 174.82 192.24 42.62 o 10 11 0 174.27 130.88 53.40 o 11 11 0 81.95 13.24 57.11 o 0 12 0 452.38 407.26 43.36 o 1 12 0 133.53 83.07 23.42 o 2 12 0 497.04 419.71 63.73 o 3 12 0 35.39 19.66 26.23 o 4 12 0 2245.02 2174.58 82.59 o 5 12 0 487.55 339.23 50.07 o 6 12 0 323.13 255.85 72.83 o 7 12 0 92.34 58.76 48.91 o 8 12 0 25.86 -41.75 41.75 o 9 12 0 127.28 128.87 54.67 o 10 12 0 60.76 109.25 100.14 o 1 13 0 1475.66 1530.39 127.45 o 2 13 0 233.27 191.05 42.11 o 3 13 0 2283.07 2503.69 267.43 o 4 13 0 317.35 290.89 69.42 o 5 13 0 1807.52 1968.85 99.98 o 6 13 0 26.64 -31.64 37.48 o 7 13 0 157.72 201.00 50.30 o 8 13 0 0.50 -0.40 50.22 o 9 13 0 123.56 96.08 59.48 o 0 14 0 116.50 19.37 38.25 o 1 14 0 40.37 65.51 35.28 o 2 14 0 231.88 162.95 35.13 o 3 14 0 216.28 193.53 41.66 o 4 14 0 654.36 570.84 85.35 o 5 14 0 80.96 75.11 58.59 o 6 14 0 43.82 17.39 59.69 o 7 14 0 8.02 -37.59 48.20 o 8 14 0 127.69 31.80 56.41 o 1 15 0 6.02 -9.85 38.24 o 2 15 0 23.59 -23.21 44.46 o 3 15 0 25.39 30.52 42.95 o 4 15 0 151.07 120.31 57.39 o 5 15 0 10.46 18.96 53.49 o 6 15 0 32.85 -25.04 67.59 o 0 16 0 371.52 292.68 76.11 o 1 16 0 40.12 -21.88 52.14 o 2 16 0 83.27 84.69 55.10 o 3 16 0 9.87 17.18 73.72 o -15 1 1 18.42 -41.94 49.16 o -14 1 1 0.09 -9.43 32.77 o -13 1 1 174.45 158.25 45.52 o -12 1 1 6.75 21.62 20.92 o -11 1 1 4.15 24.35 15.93 o -10 1 1 385.59 354.13 20.74 o -9 1 1 6.44 7.97 12.52 o -8 1 1 0.06 9.10 10.37 o -7 1 1 119.42 101.50 8.74 o -6 1 1 2343.33 2610.58 58.04 o -5 1 1 74.28 75.64 7.11 o -4 1 1 815.56 848.92 13.05 o -3 1 1 49.89 32.35 3.79 o -2 1 1 0.07 3.03 2.04 o -1 1 1 143.75 138.98 4.55 o 0 1 1 242.03 225.34 3.22 o 1 1 1 103.09 100.14 2.04 o 2 1 1 46.95 42.41 2.28 o 3 1 1 804.21 803.44 21.62 o 4 1 1 171.77 158.19 6.44 o 5 1 1 141.04 141.15 6.44 o 6 1 1 29.57 20.48 6.44 o 7 1 1 0.07 3.41 8.05 o 8 1 1 223.79 183.36 13.61 o 9 1 1 2425.12 2712.66 51.20 o 10 1 1 30.32 33.38 18.52 o 11 1 1 188.23 160.53 25.75 o 12 1 1 26.54 17.66 20.07 o 13 1 1 59.27 20.41 24.91 o 14 1 1 0.40 37.55 38.62 o 15 1 1 233.96 196.03 66.66 o -15 2 1 99.30 113.20 50.09 o -14 2 1 10.12 -11.70 28.13 o -13 2 1 168.19 125.71 58.04 o -12 2 1 26.80 23.71 18.52 o -11 2 1 89.86 51.59 16.84 o -10 2 1 403.91 362.01 52.35 o -9 2 1 887.52 934.81 38.69 o -8 2 1 122.15 110.49 11.27 o -7 2 1 903.87 959.41 33.00 o -6 2 1 1638.04 1795.77 43.24 o -5 2 1 45.88 38.79 5.46 o -4 2 1 2.18 5.92 4.55 o -3 2 1 1027.44 947.97 12.87 o -2 2 1 46.60 40.97 3.22 o -1 2 1 105.84 103.57 3.22 o 0 2 1 792.51 744.35 9.66 o 1 2 1 59.16 53.40 3.41 o 2 2 1 963.40 944.91 14.79 o 3 2 1 121.36 106.89 3.79 o 4 2 1 50.95 58.32 4.07 o 5 2 1 329.21 366.78 10.24 o 6 2 1 3.09 -4.55 5.46 o 7 2 1 512.60 500.62 14.73 o 8 2 1 405.75 391.92 17.48 o 9 2 1 5.82 -1.85 12.58 o 10 2 1 789.62 860.77 32.96 o 11 2 1 48.22 18.94 22.36 o 12 2 1 5.16 12.92 23.09 o 13 2 1 51.62 34.94 28.21 o 14 2 1 13.93 -6.52 44.11 o -15 3 1 111.82 114.19 49.47 o -14 3 1 33.08 -5.19 35.28 o -13 3 1 416.34 376.98 34.14 o -12 3 1 103.99 29.37 24.60 o -11 3 1 242.88 233.03 26.23 o -10 3 1 171.58 150.68 31.86 o -9 3 1 146.07 133.03 15.23 o -8 3 1 135.06 96.11 12.87 o -7 3 1 536.27 535.05 16.39 o -6 3 1 136.84 165.47 25.04 o -5 3 1 307.06 321.29 13.66 o -4 3 1 1099.83 1031.56 15.85 o -3 3 1 140.46 110.40 4.83 o -2 3 1 375.91 385.18 11.38 o -1 3 1 401.37 431.77 15.93 o 0 3 1 639.25 619.83 9.10 o 1 3 1 482.15 448.87 11.38 o 2 3 1 3362.90 3409.39 41.54 o 3 3 1 0.52 4.55 3.22 o 4 3 1 823.21 839.84 14.48 o 5 3 1 840.70 833.15 14.22 o 6 3 1 56.57 55.77 5.85 o 7 3 1 7.37 16.69 6.11 o 8 3 1 266.04 251.18 19.35 o 9 3 1 88.35 79.65 11.99 o 10 3 1 544.19 545.86 28.44 o 11 3 1 548.44 505.04 63.73 o 12 3 1 72.60 49.74 35.28 o 13 3 1 119.97 39.56 33.68 o 14 3 1 20.57 7.90 38.82 o -14 4 1 62.70 35.59 45.52 o -13 4 1 331.12 240.31 33.34 o -12 4 1 174.16 102.00 26.10 o -11 4 1 1609.99 1677.66 52.96 o -10 4 1 472.00 443.33 25.75 o -9 4 1 309.19 290.25 15.81 o -8 4 1 166.57 146.94 13.66 o -7 4 1 122.07 136.52 12.58 o -6 4 1 8.80 6.83 8.05 o -5 4 1 1899.86 1977.35 39.83 o -4 4 1 50.47 35.46 5.69 o -3 4 1 1901.30 1821.68 21.68 o -2 4 1 1830.87 1789.83 20.74 o -1 4 1 21.04 17.15 3.22 o 0 4 1 9.91 10.24 3.22 o 1 4 1 836.91 827.09 15.93 o 2 4 1 3821.31 3856.96 85.35 o 3 4 1 1028.14 1036.33 19.35 o 4 4 1 3207.29 3401.84 39.89 o 5 4 1 318.05 272.21 9.66 o 6 4 1 1910.43 2017.42 31.10 o 7 4 1 944.44 980.99 46.66 o 8 4 1 52.36 28.25 22.76 o 9 4 1 380.90 322.20 23.98 o 10 4 1 121.79 108.23 20.19 o 11 4 1 125.76 122.15 24.42 o 12 4 1 319.50 284.19 33.34 o 13 4 1 0.00 42.02 32.73 o 14 4 1 3.90 -37.59 37.59 o -14 5 1 380.57 307.08 96.73 o -13 5 1 12.89 11.26 30.07 o -12 5 1 21.58 0.14 26.52 o -11 5 1 1.23 -22.96 22.96 o -10 5 1 557.61 508.47 35.71 o -9 5 1 360.81 358.92 34.14 o -8 5 1 1972.27 2082.32 66.00 o -7 5 1 111.67 116.09 19.35 o -6 5 1 64.42 48.01 9.26 o -5 5 1 1.59 -3.25 5.46 o -4 5 1 2703.90 2941.37 33.68 o -3 5 1 122.85 114.63 5.46 o -2 5 1 2759.65 2901.16 31.10 o -1 5 1 271.94 253.48 7.97 o 0 5 1 464.18 414.22 15.93 o 1 5 1 252.54 213.37 7.11 o 2 5 1 5020.65 5198.65 102.42 o 3 5 1 1209.58 1284.06 23.90 o 4 5 1 4883.38 5364.85 100.14 o 5 5 1 5.37 -2.28 7.97 o 6 5 1 135.73 125.23 9.26 o 7 5 1 118.41 96.45 25.04 o 8 5 1 860.93 928.40 60.31 o 9 5 1 958.34 920.75 35.97 o 10 5 1 54.39 44.54 21.02 o 11 5 1 2.81 -13.33 27.31 o 12 5 1 29.63 53.51 28.29 o 13 5 1 424.76 425.13 48.20 o 14 5 1 18.49 30.82 46.97 o -14 6 1 50.47 -6.83 38.82 o -13 6 1 112.94 123.81 37.87 o -12 6 1 762.83 672.58 96.73 o -11 6 1 651.50 647.18 146.80 o -10 6 1 137.60 119.01 52.35 o -9 6 1 3.57 -13.20 15.15 o -8 6 1 34.94 38.69 23.90 o -7 6 1 107.57 93.55 11.36 o -6 6 1 258.77 228.79 12.52 o -5 6 1 7055.86 7836.13 96.20 o -4 6 1 427.82 441.23 11.99 o -3 6 1 220.59 161.62 10.24 o -2 6 1 3184.70 3331.42 35.97 o -1 6 1 754.92 718.28 12.87 o 0 6 1 272.73 304.97 8.74 o 1 6 1 1711.73 1737.37 29.59 o 2 6 1 2475.45 2549.01 31.35 o 3 6 1 694.10 679.73 31.86 o 4 6 1 2369.03 2447.72 64.86 o 5 6 1 1104.58 1153.29 24.91 o 6 6 1 242.61 218.76 19.35 o 7 6 1 33.35 15.16 13.66 o 8 6 1 99.84 59.43 21.33 o 9 6 1 1385.24 1357.17 43.71 o 10 6 1 1926.32 2105.11 68.86 o 11 6 1 164.08 139.58 33.00 o 12 6 1 75.17 7.31 37.79 o 13 6 1 12.46 39.04 55.77 o 14 6 1 65.81 138.32 52.82 o -13 7 1 61.25 69.11 43.71 o -12 7 1 15.72 29.71 30.07 o -11 7 1 0.96 -18.70 35.28 o -10 7 1 47.10 55.86 39.83 o -9 7 1 296.40 286.05 28.83 o -8 7 1 2782.08 3102.28 73.82 o -7 7 1 2158.06 2417.42 48.20 o -6 7 1 92.11 81.57 10.92 o -5 7 1 819.85 774.19 37.55 o -4 7 1 21.48 28.22 7.57 o -3 7 1 223.98 214.34 9.65 o -2 7 1 6164.28 6559.24 126.32 o -1 7 1 923.85 944.22 19.35 o 0 7 1 1072.54 981.56 17.48 o 1 7 1 841.64 771.93 14.73 o 2 7 1 873.47 907.85 33.00 o 3 7 1 245.44 271.42 12.58 o 4 7 1 1740.07 1842.82 40.97 o 5 7 1 596.50 586.10 19.35 o 6 7 1 60.96 33.49 10.92 o 7 7 1 1177.28 1275.73 30.58 o 8 7 1 129.19 80.16 23.50 o 9 7 1 11.38 43.34 19.11 o 10 7 1 50.94 46.92 25.16 o 11 7 1 252.66 180.75 40.97 o 12 7 1 58.52 22.33 44.38 o 13 7 1 221.06 234.31 45.85 o -13 8 1 2.90 -41.08 48.91 o -12 8 1 239.42 372.34 51.40 o -11 8 1 543.89 558.72 101.28 o -10 8 1 171.76 147.33 36.43 o -9 8 1 702.51 563.21 44.46 o -8 8 1 872.27 856.15 31.11 o -7 8 1 12.55 28.45 12.58 o -6 8 1 188.73 181.43 13.44 o -5 8 1 794.41 876.16 23.99 o -4 8 1 138.74 119.06 10.92 o -3 8 1 238.17 257.38 11.71 o -2 8 1 168.32 155.74 10.37 o -1 8 1 1277.10 1292.62 26.02 o 0 8 1 2075.34 2197.10 85.35 o 1 8 1 307.56 283.91 15.93 o 2 8 1 2352.06 2473.06 33.07 o 3 8 1 134.59 107.63 10.37 o 4 8 1 633.95 640.01 35.28 o 5 8 1 523.73 519.80 20.07 o 6 8 1 1306.28 1241.04 36.91 o 7 8 1 25.26 -3.41 13.66 o 8 8 1 2242.76 2436.14 69.47 o 9 8 1 350.85 352.56 34.91 o 10 8 1 1714.03 1795.69 66.00 o 11 8 1 82.11 32.64 35.78 o 12 8 1 122.93 147.21 42.08 o 13 8 1 18.52 31.14 80.80 o -12 9 1 6.91 -23.35 43.36 o -11 9 1 31.79 17.54 44.38 o -10 9 1 229.24 97.73 40.83 o -9 9 1 54.68 -3.66 29.19 o -8 9 1 927.41 1048.34 106.97 o -7 9 1 33.05 34.90 14.22 o -6 9 1 444.58 400.54 21.33 o -5 9 1 391.58 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