#------------------------------------------------------------------------------ #$Date: 2012-01-03 14:54:16 +0200 (Tue, 03 Jan 2012) $ #$Revision: 31968 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/10/50/2105000.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_2105000_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 11.9670 _cell_length_b 12.6900 _cell_length_c 15.9930 _exptl_crystal_F_000 1160.00 _reflns_d_resolution_high 0.7703 _[local]_cod_data_source_file hw5018110K_IVsup8.hkl _[local]_cod_data_source_block 110K_IV #BEGIN Tags that were not found in dictionaries: _shelx_title ' k06179 in P2(1)/c' _shelx_refln_list_code 4 _shelx_f_calc_maximum 353.39 _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 0 766.78 751.06 12.73 o 2 0 0 18971.94 17594.67 284.30 o 3 0 0 45.47 29.70 4.24 o 4 0 0 6205.24 6269.41 116.69 o 5 0 0 934.59 1067.18 25.46 o 6 0 0 56260.95 58166.59 1045.96 o 7 0 0 4.02 19.09 10.61 o 8 0 0 7583.50 7784.26 161.24 o 9 0 0 1354.48 1423.61 50.92 o 10 0 0 3114.42 3337.32 118.81 o 11 0 0 18.61 29.70 27.58 o 12 0 0 345.69 324.61 57.28 o 13 0 0 41.45 25.46 38.19 o 14 0 0 649.06 714.99 97.59 o 15 0 0 1163.24 1287.83 120.93 o 1 1 0 26447.38 23802.60 318.05 o 2 1 0 20.76 18.60 3.18 o 3 1 0 4598.94 4395.81 50.96 o 4 1 0 349.88 349.21 8.15 o 5 1 0 6373.17 6166.04 71.87 o 6 1 0 3599.30 3479.03 44.86 o 7 1 0 4357.89 4237.06 58.90 o 8 1 0 5870.68 6372.32 97.51 o 9 1 0 3723.92 3718.26 69.32 o 10 1 0 245.58 155.42 36.07 o 11 1 0 1116.43 1154.98 65.77 o 12 1 0 868.27 928.91 52.94 o 13 1 0 27.70 16.30 44.31 o 14 1 0 10.93 58.12 41.93 o 15 1 0 175.86 133.63 52.49 o 1 2 0 71.21 74.80 6.36 o 2 2 0 516.68 456.16 7.50 o 3 2 0 337.50 307.04 6.63 o 4 2 0 6903.64 6873.56 74.25 o 5 2 0 958.62 893.91 26.52 o 6 2 0 7117.65 7229.28 81.01 o 7 2 0 2.43 3.82 7.43 o 8 2 0 1879.18 1981.72 38.73 o 9 2 0 1187.07 1185.05 32.60 o 10 2 0 1763.62 1846.53 50.92 o 11 2 0 780.23 826.68 38.47 o 12 2 0 414.90 300.68 35.31 o 13 2 0 210.95 137.64 47.37 o 14 2 0 346.93 339.72 131.54 o 15 2 0 440.63 343.47 127.30 o 1 3 0 319.87 340.55 6.00 o 2 3 0 207.18 206.86 6.00 o 3 3 0 52071.38 49333.01 530.82 o 4 3 0 13682.23 14606.52 149.93 o 5 3 0 16668.96 16195.58 178.83 o 6 3 0 1272.85 1269.50 20.80 o 7 3 0 3336.38 3301.93 57.30 o 8 3 0 3460.51 3728.50 67.89 o 9 3 0 2141.55 2214.98 47.38 o 10 3 0 2498.05 2560.27 63.55 o 11 3 0 2894.64 3125.50 86.70 o 12 3 0 330.95 281.99 29.25 o 13 3 0 914.46 911.20 59.44 o 14 3 0 273.59 367.36 58.43 o 0 4 0 2538.77 2256.81 66.83 o 1 4 0 13.07 13.34 4.24 o 2 4 0 46473.86 46061.37 519.69 o 3 4 0 1290.71 1268.96 18.00 o 4 4 0 28303.57 29103.22 288.82 o 5 4 0 9952.84 10875.52 118.23 o 6 4 0 3153.51 3022.04 42.81 o 7 4 0 41.71 44.29 8.15 o 8 4 0 1772.07 1876.55 38.73 o 9 4 0 18.36 22.28 11.67 o 10 4 0 778.25 741.29 42.43 o 11 4 0 2460.45 2636.37 227.01 o 12 4 0 1709.46 1842.28 213.22 o 13 4 0 524.29 417.96 46.83 o 14 4 0 531.87 507.44 66.32 o 1 5 0 1661.25 1681.93 44.55 o 2 5 0 43.82 42.63 5.30 o 3 5 0 4048.96 3855.87 40.75 o 4 5 0 7510.77 7907.16 82.54 o 5 5 0 5580.64 5547.23 67.26 o 6 5 0 32.64 19.09 7.06 o 7 5 0 1966.73 2071.18 34.93 o 8 5 0 656.63 657.36 19.88 o 9 5 0 312.13 303.02 16.30 o 10 5 0 2910.99 3166.31 83.68 o 11 5 0 1174.36 1155.45 92.29 o 12 5 0 34.05 61.53 49.86 o 13 5 0 524.09 446.03 53.32 o 14 5 0 853.01 881.69 104.50 o 0 6 0 6399.67 6305.29 149.57 o 1 6 0 900.02 876.63 26.52 o 2 6 0 29267.31 30142.23 323.15 o 3 6 0 1231.36 1330.23 20.37 o 4 6 0 9899.32 10037.28 223.83 o 5 6 0 863.37 902.43 18.29 o 6 6 0 5278.31 5523.38 74.14 o 7 6 0 37.19 33.49 9.27 o 8 6 0 1007.68 1061.23 41.37 o 9 6 0 205.87 183.90 19.80 o 10 6 0 779.75 805.97 39.70 o 11 6 0 1450.40 1589.07 138.97 o 12 6 0 800.83 751.30 64.71 o 13 6 0 489.19 406.09 53.95 o 14 6 0 61.42 42.43 65.77 o 1 7 0 14221.63 15113.60 264.14 o 2 7 0 7.72 3.45 9.55 o 3 7 0 4676.36 4634.94 59.56 o 4 7 0 363.55 344.65 11.18 o 5 7 0 8792.59 9421.80 239.74 o 6 7 0 46.28 45.46 9.79 o 7 7 0 5074.37 5507.11 85.09 o 8 7 0 336.15 304.77 20.16 o 9 7 0 902.71 926.67 33.63 o 10 7 0 1346.21 1473.42 56.12 o 11 7 0 1527.87 1683.42 79.51 o 12 7 0 6.78 -44.21 60.47 o 13 7 0 89.47 56.67 44.09 o 0 8 0 7155.16 7384.79 130.95 o 1 8 0 119.00 102.42 8.15 o 2 8 0 1891.94 1853.88 29.83 o 3 8 0 922.77 1005.44 21.18 o 4 8 0 86.12 77.47 7.98 o 5 8 0 485.67 495.02 23.34 o 6 8 0 1489.84 1557.38 62.59 o 7 8 0 2024.19 2250.77 49.81 o 8 8 0 464.37 413.81 23.91 o 9 8 0 1271.31 1194.08 54.37 o 10 8 0 891.05 963.23 54.37 o 11 8 0 214.06 157.16 83.80 o 12 8 0 3.67 6.07 43.49 o 13 8 0 372.53 412.63 127.30 o 1 9 0 5509.90 5733.16 171.85 o 2 9 0 1082.25 1144.57 24.33 o 3 9 0 51.63 34.93 7.88 o 4 9 0 831.73 867.95 25.90 o 5 9 0 361.19 371.16 11.92 o 6 9 0 918.19 918.29 25.37 o 7 9 0 1600.93 1564.28 48.60 o 8 9 0 1850.02 1784.67 61.60 o 9 9 0 1430.37 1415.37 80.62 o 10 9 0 800.26 710.73 48.80 o 11 9 0 181.86 169.53 41.93 o 12 9 0 5.23 14.39 50.96 o 0 10 0 9824.51 10059.86 276.87 o 1 10 0 141.03 128.62 10.18 o 2 10 0 397.62 394.73 24.40 o 3 10 0 60.48 56.07 15.91 o 4 10 0 185.96 225.43 30.76 o 5 10 0 92.46 112.47 18.55 o 6 10 0 2143.88 2085.62 54.01 o 7 10 0 900.73 904.59 37.19 o 8 10 0 591.44 588.01 40.17 o 9 10 0 592.03 525.82 41.69 o 10 10 0 744.54 713.65 50.94 o 11 10 0 25.87 -2.79 52.44 o 12 10 0 35.55 70.50 57.08 o 1 11 0 2726.01 2937.43 79.56 o 2 11 0 231.61 176.30 19.88 o 3 11 0 169.96 164.05 19.23 o 4 11 0 51.52 27.58 14.12 o 5 11 0 1739.26 1726.76 48.43 o 6 11 0 192.57 163.88 22.93 o 7 11 0 319.58 275.56 33.53 o 8 11 0 34.56 -19.89 29.89 o 9 11 0 232.98 235.35 40.26 o 10 11 0 231.50 203.36 49.37 o 11 11 0 91.09 31.95 48.91 o 0 12 0 423.54 404.39 31.82 o 1 12 0 177.36 150.68 22.28 o 2 12 0 463.39 383.30 24.45 o 3 12 0 33.68 25.81 17.26 o 4 12 0 2543.64 2497.98 70.85 o 5 12 0 612.35 536.12 35.64 o 6 12 0 311.03 275.67 35.04 o 7 12 0 119.97 64.30 29.23 o 8 12 0 47.25 80.62 36.01 o 9 12 0 177.13 150.57 88.05 o 10 12 0 56.21 40.24 41.60 o 1 13 0 1772.94 1990.69 71.87 o 2 13 0 301.98 263.99 30.73 o 3 13 0 2554.24 2656.69 83.56 o 4 13 0 370.88 337.94 34.66 o 5 13 0 2128.08 2156.07 78.75 o 6 13 0 42.96 58.74 28.39 o 7 13 0 189.00 168.21 40.51 o 8 13 0 0.70 2.68 33.63 o 9 13 0 125.32 166.01 46.43 o 0 14 0 175.08 174.27 53.12 o 1 14 0 45.04 52.16 39.73 o 2 14 0 246.76 122.18 39.83 o 3 14 0 265.19 221.73 52.86 o 4 14 0 829.63 668.21 51.93 o 5 14 0 103.35 33.43 36.07 o 6 14 0 53.06 67.11 36.55 o 7 14 0 6.70 5.32 44.55 o 8 14 0 146.53 115.54 42.26 o 1 15 0 11.28 0.92 50.96 o 2 15 0 23.22 79.95 75.32 o 3 15 0 39.88 65.74 79.56 o 4 15 0 192.26 230.46 60.08 o 5 15 0 11.30 -53.20 57.99 o 6 15 0 36.35 39.64 106.08 o 0 16 0 404.50 286.46 78.46 o 1 16 0 50.17 -18.76 52.25 o 2 16 0 74.58 15.48 45.59 o 3 16 0 17.66 -35.14 74.26 o -15 1 1 19.30 94.60 49.96 o -14 1 1 1.41 10.09 30.51 o -13 1 1 231.03 241.86 42.01 o -12 1 1 15.44 53.15 29.70 o -11 1 1 1.41 -13.34 20.37 o -10 1 1 507.72 499.86 29.89 o -9 1 1 15.10 13.44 13.25 o -8 1 1 2.39 1.06 9.00 o -7 1 1 94.68 84.28 9.00 o -6 1 1 2574.76 2846.81 39.19 o -5 1 1 93.33 80.62 5.46 o -4 1 1 787.06 820.52 24.40 o -3 1 1 53.15 33.74 5.30 o -2 1 1 0.35 3.18 1.50 o -1 1 1 131.67 135.82 3.00 o 0 1 1 228.58 201.55 3.00 o 1 1 1 120.55 119.88 3.00 o 2 1 1 48.50 39.54 2.12 o 3 1 1 780.38 776.99 19.09 o 4 1 1 184.40 178.63 6.63 o 5 1 1 176.16 191.54 10.61 o 6 1 1 36.28 31.50 6.63 o 7 1 1 0.15 -4.24 7.50 o 8 1 1 214.32 172.13 12.69 o 9 1 1 2913.75 3165.98 56.24 o 10 1 1 40.68 29.14 16.97 o 11 1 1 251.76 276.48 22.76 o 12 1 1 20.53 19.70 23.64 o 13 1 1 77.68 88.06 46.81 o 14 1 1 0.25 -7.21 43.20 o 15 1 1 333.56 260.79 64.22 o -15 2 1 151.41 189.76 55.25 o -14 2 1 20.64 22.65 45.86 o -13 2 1 176.16 205.27 35.66 o -12 2 1 35.73 7.64 29.00 o -11 2 1 129.30 63.88 19.88 o -10 2 1 439.35 386.34 23.45 o -9 2 1 1094.06 1175.84 40.31 o -8 2 1 118.91 102.69 10.59 o -7 2 1 978.80 1020.97 18.29 o -6 2 1 1799.39 2002.18 32.89 o -5 2 1 56.67 46.69 7.43 o -4 2 1 5.50 -0.42 3.53 o -3 2 1 1079.67 997.14 14.19 o -2 2 1 45.40 36.19 3.00 o -1 2 1 107.45 98.94 5.30 o 0 2 1 818.79 779.77 9.00 o 1 2 1 65.12 57.36 2.12 o 2 2 1 1040.24 998.48 15.91 o 3 2 1 114.46 96.64 3.18 o 4 2 1 56.14 65.09 5.09 o 5 2 1 326.68 374.49 11.67 o 6 2 1 9.14 5.30 6.00 o 7 2 1 610.74 607.93 18.71 o 8 2 1 502.99 512.51 37.13 o 9 2 1 9.92 11.46 10.59 o 10 2 1 837.53 845.10 45.62 o 11 2 1 104.25 52.79 29.70 o 12 2 1 7.12 47.85 60.47 o 13 2 1 64.37 42.26 37.15 o 14 2 1 22.82 18.39 47.24 o -15 3 1 126.62 164.46 68.15 o -14 3 1 35.87 77.03 40.26 o -13 3 1 531.72 446.57 41.55 o -12 3 1 162.94 142.07 51.98 o -11 3 1 290.06 224.85 34.93 o -10 3 1 242.62 215.19 19.23 o -9 3 1 225.80 192.19 15.91 o -8 3 1 166.62 139.73 10.92 o -7 3 1 538.18 563.04 14.46 o -6 3 1 149.21 180.87 20.16 o -5 3 1 306.96 298.78 8.15 o -4 3 1 1044.18 1005.05 16.97 o -3 3 1 103.11 76.38 5.09 o -2 3 1 410.85 410.35 8.15 o -1 3 1 361.29 377.95 10.61 o 0 3 1 647.95 605.54 8.15 o 1 3 1 552.47 491.49 8.15 o 2 3 1 3445.79 3383.90 39.23 o 3 3 1 3.76 4.24 3.00 o 4 3 1 825.38 814.23 12.69 o 5 3 1 949.22 938.88 15.00 o 6 3 1 69.86 77.57 7.50 o 7 3 1 10.20 13.89 8.15 o 8 3 1 262.41 247.56 14.85 o 9 3 1 104.48 75.82 12.69 o 10 3 1 647.53 641.90 60.47 o 11 3 1 670.24 612.76 38.31 o 12 3 1 80.20 7.88 27.58 o 13 3 1 117.55 3.16 39.23 o 14 3 1 22.73 -0.47 45.73 o -14 4 1 68.95 151.17 85.93 o -13 4 1 341.36 257.27 46.83 o -12 4 1 182.57 126.83 30.52 o -11 4 1 1702.15 1811.01 61.59 o -10 4 1 535.57 464.25 22.76 o -9 4 1 317.07 312.28 16.30 o -8 4 1 240.83 246.29 24.40 o -7 4 1 104.57 121.51 26.52 o -6 4 1 3.98 -2.92 5.46 o -5 4 1 1740.05 1740.82 23.45 o -4 4 1 37.59 25.99 5.09 o -3 4 1 1860.56 1770.72 23.34 o -2 4 1 1941.75 1907.80 24.40 o -1 4 1 31.34 28.68 3.00 o 0 4 1 7.85 15.15 3.00 o 1 4 1 886.54 861.26 25.46 o 2 4 1 3922.48 3981.42 44.28 o 3 4 1 1075.46 1042.92 15.28 o 4 4 1 3330.64 3437.87 38.23 o 5 4 1 264.73 229.98 15.91 o 6 4 1 1974.39 2072.60 37.71 o 7 4 1 1091.70 1169.03 25.50 o 8 4 1 38.61 12.98 12.69 o 9 4 1 413.57 369.34 25.46 o 10 4 1 93.96 97.79 35.01 o 11 4 1 173.50 139.42 45.62 o 12 4 1 422.62 322.88 60.47 o 13 4 1 1.59 -14.76 31.12 o 14 4 1 2.66 -41.98 96.53 o -14 5 1 489.34 352.91 93.35 o -13 5 1 24.53 16.12 38.19 o -12 5 1 19.98 37.51 25.76 o -11 5 1 0.59 -7.78 27.58 o -10 5 1 737.03 677.89 31.41 o -9 5 1 412.78 401.19 18.55 o -8 5 1 2263.74 2487.66 65.77 o -7 5 1 148.87 138.68 10.18 o -6 5 1 46.67 22.95 8.15 o -5 5 1 2.98 4.51 5.46 o -4 5 1 2849.26 3093.54 36.70 o -3 5 1 73.17 55.49 6.00 o -2 5 1 2956.35 2998.39 33.53 o -1 5 1 294.79 256.73 8.49 o 0 5 1 490.29 416.01 8.15 o 1 5 1 281.59 233.55 6.36 o 2 5 1 5154.18 5170.75 68.95 o 3 5 1 1469.10 1562.31 20.37 o 4 5 1 5025.87 5506.30 102.90 o 5 5 1 1.50 0.00 9.55 o 6 5 1 141.80 133.64 9.27 o 7 5 1 148.11 104.67 12.17 o 8 5 1 1013.29 1002.60 35.98 o 9 5 1 981.37 1025.69 44.93 o 10 5 1 113.63 102.50 21.82 o 11 5 1 5.65 26.11 21.36 o 12 5 1 15.82 0.00 59.41 o 13 5 1 457.90 458.61 115.63 o 14 5 1 22.59 -16.85 53.67 o -14 6 1 67.97 79.34 71.74 o -13 6 1 124.51 49.46 45.62 o -12 6 1 973.22 1035.77 62.02 o -11 6 1 620.87 649.62 118.81 o -10 6 1 144.83 125.30 23.27 o -9 6 1 3.28 10.61 10.50 o -8 6 1 15.51 -5.06 9.00 o -7 6 1 120.54 107.36 25.46 o -6 6 1 281.02 274.96 12.53 o -5 6 1 7659.08 8338.89 141.09 o -4 6 1 428.38 440.84 12.69 o -3 6 1 176.38 128.18 8.15 o -2 6 1 3250.66 3334.66 36.73 o -1 6 1 712.82 667.52 11.72 o 0 6 1 311.70 375.83 10.61 o 1 6 1 1738.02 1744.13 19.88 o 2 6 1 2628.26 2738.51 36.07 o 3 6 1 820.62 808.54 26.52 o 4 6 1 2633.73 2698.82 35.66 o 5 6 1 1068.01 1120.52 21.83 o 6 6 1 290.90 268.78 13.08 o 7 6 1 51.95 39.10 7.98 o 8 6 1 86.84 68.98 14.85 o 9 6 1 1850.41 1892.97 67.66 o 10 6 1 2282.22 2433.31 70.82 o 11 6 1 242.96 231.55 32.55 o 12 6 1 86.92 58.65 75.32 o 13 6 1 18.58 -13.79 43.82 o 14 6 1 129.80 147.10 72.11 o -13 7 1 70.27 57.02 47.73 o -12 7 1 17.18 -14.52 53.04 o -11 7 1 9.55 -4.29 32.09 o -10 7 1 72.44 64.03 22.11 o -9 7 1 342.62 367.48 24.40 o -8 7 1 3142.49 3429.90 69.65 o -7 7 1 2589.90 2766.60 67.89 o -6 7 1 60.37 43.42 9.67 o -5 7 1 801.54 750.29 22.76 o -4 7 1 18.00 15.56 10.61 o -3 7 1 181.75 170.55 10.92 o -2 7 1 6560.87 6886.65 77.32 o -1 7 1 921.94 926.22 16.30 o 0 7 1 1058.52 924.30 14.78 o 1 7 1 750.13 677.41 11.72 o 2 7 1 874.21 910.46 18.35 o 3 7 1 326.02 344.94 13.25 o 4 7 1 1872.46 1965.12 29.47 o 5 7 1 549.27 563.75 15.51 o 6 7 1 91.75 74.62 9.55 o 7 7 1 1293.05 1404.99 38.19 o 8 7 1 200.09 154.66 16.37 o 9 7 1 16.06 14.85 17.65 o 10 7 1 125.06 112.19 39.04 o 11 7 1 235.86 238.63 38.92 o 12 7 1 54.87 37.15 39.23 o 13 7 1 218.74 136.18 43.78 o -13 8 1 1.99 5.52 44.71 o -12 8 1 296.32 214.86 74.26 o -11 8 1 541.43 537.35 46.81 o -10 8 1 165.15 70.13 28.39 o -9 8 1 668.61 567.07 68.95 o -8 8 1 878.76 837.50 31.40 o -7 8 1 27.93 14.73 11.18 o -6 8 1 166.60 159.51 13.46 o -5 8 1 852.07 887.75 21.83 o -4 8 1 171.36 151.06 12.83 o -3 8 1 218.36 232.35 12.83 o -2 8 1 148.64 124.91 9.00 o -1 8 1 1274.45 1246.58 22.35 o 0 8 1 2114.15 2301.38 32.89 o 1 8 1 282.39 262.26 10.18 o 2 8 1 2469.07 2630.86 42.81 o 3 8 1 153.89 138.72 13.79 o 4 8 1 722.36 724.00 25.46 o 5 8 1 578.16 610.35 23.45 o 6 8 1 1462.74 1449.80 30.17 o 7 8 1 61.69 55.83 12.83 o 8 8 1 2235.61 2346.36 69.65 o 9 8 1 402.81 396.79 30.00 o 10 8 1 1976.82 2166.51 104.72 o 11 8 1 117.48 96.59 39.62 o 12 8 1 190.39 183.21 47.37 o 13 8 1 21.67 -24.40 47.74 o -12 9 1 6.79 34.32 41.93 o -11 9 1 43.32 115.69 42.43 o -10 9 1 298.98 272.43 38.19 o -9 9 1 53.04 26.48 31.82 o -8 9 1 1084.31 1071.30 98.66 o -7 9 1 26.55 30.48 11.56 o -6 9 1 456.70 384.23 24.40 o -5 9 1 382.96 328.64 13.73 o -4 9 1 6.04 2.65 10.92 o -3 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