#------------------------------------------------------------------------------ #$Date: 2012-09-11 12:26:43 +0300 (Tue, 11 Sep 2012) $ #$Revision: 66590 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/10/51/2105176.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_2105176_Fobs loop_ _publ_author_name 'Siegler, Maxime A.' 'Parkin, Sean' 'Brock, Carolyn Pratt' _publ_section_title ; [Ni(MeCN)(H~2~O)~2~(NO~3~)~2~]·(15-crown-5)·MeCN: detailed study of a four-phase sequence that includes an intermediate modulated phase ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 389 _journal_page_last 400 _journal_volume 68 _journal_year 2012 _space_group_IT_number 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 90.050 _cell_angle_beta 105.460 _cell_angle_gamma 90.030 _cell_length_a 12.1500 _cell_length_b 12.1520 _cell_length_c 16.0520 _exptl_crystal_F_000 1096.00 _reflns_d_resolution_high 0.7697 _[local]_cod_data_source_file hw5021110K_IV_1sup6.hkl _[local]_cod_data_source_block 110K_IV_1 #BEGIN Tags that were not found in dictionaries: _shelx_title ' k06085 in P-1' _shelx_refln_list_code 4 _shelx_f_calc_maximum 286.95 _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' 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 5673.19 5370.04 81.60 o 2 0 0 24094.53 23961.50 406.57 o 3 0 0 601.77 713.01 11.61 o 4 0 0 1385.21 1311.61 20.74 o 5 0 0 48719.53 51239.99 770.39 o 6 0 0 1393.39 1335.97 23.43 o 7 0 0 11661.12 11651.48 177.81 o 8 0 0 7295.23 7510.33 129.61 o 9 0 0 841.69 942.01 32.99 o 10 0 0 373.27 419.21 14.45 o 11 0 0 1743.37 1622.40 46.68 o 12 0 0 2962.54 3093.35 85.26 o 13 0 0 1995.11 2115.22 78.28 o 14 0 0 52.56 77.84 47.72 o 15 0 0 415.50 326.37 53.79 o -15 1 0 21.23 2.70 28.82 o -14 1 0 339.86 293.10 57.26 o -13 1 0 476.04 483.41 39.19 o -12 1 0 2080.62 2021.88 155.26 o -11 1 0 4927.70 5172.10 124.93 o -10 1 0 513.06 525.07 44.25 o -9 1 0 914.68 976.12 31.86 o -8 1 0 119.90 96.07 14.24 o -7 1 0 2908.60 2788.05 95.48 o -6 1 0 15095.69 15059.49 295.87 o -5 1 0 1924.56 2216.11 36.06 o -4 1 0 18142.54 17363.61 319.95 o -3 1 0 10214.79 9675.71 134.84 o -2 1 0 1101.25 1146.38 20.86 o 0 1 0 54.65 54.87 1.74 o 2 1 0 1013.04 1050.37 15.31 o 3 1 0 10105.15 9617.12 139.25 o 4 1 0 17762.74 17394.79 266.33 o 5 1 0 2075.10 2319.48 69.39 o 6 1 0 14848.81 15083.53 196.24 o 7 1 0 2715.50 2588.36 41.52 o 8 1 0 132.66 119.64 21.69 o 9 1 0 973.24 1015.22 35.61 o 10 1 0 562.09 575.37 23.43 o 11 1 0 5237.59 5332.84 113.62 o 12 1 0 1967.35 2013.49 66.95 o 13 1 0 547.09 500.25 43.61 o 14 1 0 321.64 294.51 70.28 o 15 1 0 25.38 90.69 48.59 o -15 2 0 1064.02 1010.84 64.41 o -14 2 0 83.27 126.08 35.33 o -13 2 0 706.07 674.03 50.68 o -12 2 0 1478.53 1650.23 67.78 o -11 2 0 54.60 42.08 23.43 o -10 2 0 4335.09 4596.71 141.40 o -9 2 0 1997.21 2114.46 53.47 o -8 2 0 5133.27 5309.50 117.19 o -7 2 0 5903.21 6025.25 98.66 o -6 2 0 655.37 572.50 17.05 o -5 2 0 18779.74 18534.35 468.49 o -4 2 0 1444.20 1366.13 34.34 o -3 2 0 9294.57 8514.81 254.24 o -2 2 0 2967.33 3078.40 70.89 o -1 2 0 1140.89 1044.13 19.19 o 0 2 0 10831.82 9966.53 142.31 o 1 2 0 1055.44 986.70 15.02 o 2 2 0 2828.09 2977.80 42.00 o 3 2 0 9657.96 8878.98 101.63 o 4 2 0 1731.96 1633.92 32.11 o 5 2 0 19269.55 19222.25 307.16 o 6 2 0 728.23 683.85 14.72 o 7 2 0 6074.15 6168.50 88.78 o 8 2 0 4844.42 5133.07 126.66 o 9 2 0 2062.68 2157.38 41.99 o 10 2 0 4450.26 4740.73 128.43 o 11 2 0 64.86 56.12 15.17 o 12 2 0 1544.67 1600.78 58.77 o 13 2 0 670.03 625.43 40.44 o 14 2 0 88.53 107.99 49.46 o 15 2 0 1081.18 1134.15 180.46 o -14 3 0 709.93 630.48 43.76 o -13 3 0 26.84 -21.03 36.44 o -12 3 0 63.92 75.84 32.10 o -11 3 0 3760.34 3597.89 127.54 o -10 3 0 855.25 834.28 38.19 o -9 3 0 5645.58 5731.56 116.84 o -8 3 0 1530.27 1575.70 79.80 o -7 3 0 1176.54 1226.94 37.10 o -6 3 0 1155.85 1035.31 22.43 o -5 3 0 2298.93 2366.74 41.26 o -4 3 0 18931.06 19420.39 445.99 o -3 3 0 9719.43 9479.65 145.20 o -2 3 0 5751.79 5479.37 95.42 o -1 3 0 4662.43 4705.22 84.31 o 0 3 0 0.42 16.36 2.89 o 1 3 0 4609.74 4656.33 71.91 o 2 3 0 5555.53 5270.35 87.06 o 3 3 0 10664.17 10225.91 289.80 o 4 3 0 19500.52 20121.70 317.57 o 5 3 0 1993.78 2164.94 39.04 o 6 3 0 1192.90 988.89 17.51 o 7 3 0 1008.67 1128.77 31.23 o 8 3 0 1489.64 1621.07 82.41 o 9 3 0 5329.56 5505.02 171.83 o 10 3 0 838.85 839.58 30.35 o 11 3 0 3518.93 3496.14 96.32 o 12 3 0 59.77 45.03 32.97 o 13 3 0 22.98 -0.61 24.03 o 14 3 0 684.55 661.74 48.67 o -14 4 0 40.09 33.90 36.57 o -13 4 0 122.97 87.32 61.60 o -12 4 0 311.95 225.24 36.44 o -11 4 0 157.15 119.24 27.01 o -10 4 0 3920.25 3702.87 106.16 o -9 4 0 288.51 256.85 20.75 o -8 4 0 4200.87 4362.12 111.91 o -7 4 0 4707.05 4884.74 92.11 o -6 4 0 726.29 770.71 21.68 o -5 4 0 11633.33 11957.81 219.72 o -4 4 0 1799.05 2041.77 49.61 o -3 4 0 8968.57 9229.50 204.03 o -2 4 0 13886.90 13762.22 266.97 o -1 4 0 2584.06 2573.15 41.50 o 0 4 0 46331.32 45234.26 1707.49 o 1 4 0 2250.95 2188.48 56.57 o 2 4 0 15097.29 14143.04 260.27 o 3 4 0 8260.82 8287.70 208.23 o 4 4 0 1533.53 1805.22 45.97 o 5 4 0 11175.19 11725.99 154.93 o 6 4 0 699.09 733.70 17.76 o 7 4 0 4642.10 4841.81 84.67 o 8 4 0 3942.01 4002.58 91.27 o 9 4 0 278.15 240.83 20.82 o 10 4 0 3739.95 3737.92 107.51 o 11 4 0 162.95 131.27 22.64 o 12 4 0 265.78 240.55 39.81 o 13 4 0 112.88 52.11 39.93 o 14 4 0 42.60 39.99 42.21 o -14 5 0 1216.93 1119.61 80.15 o -13 5 0 86.51 43.86 41.64 o -12 5 0 49.15 41.07 59.00 o -11 5 0 1985.72 2070.52 85.74 o -10 5 0 781.97 673.32 41.58 o -9 5 0 2146.82 2084.99 64.17 o -8 5 0 97.71 98.68 16.26 o -7 5 0 14.32 18.77 6.03 o -6 5 0 5438.86 5453.58 104.21 o -5 5 0 57.02 49.17 10.41 o -4 5 0 7239.85 7684.74 164.21 o -3 5 0 9237.04 9606.96 147.76 o -2 5 0 10394.81 11274.01 320.14 o -1 5 0 12568.57 12256.54 186.75 o 0 5 0 707.38 628.57 13.33 o 1 5 0 12613.85 12440.04 217.58 o 2 5 0 9741.40 10307.39 209.11 o 3 5 0 9601.27 9650.15 157.37 o 4 5 0 6482.40 6529.81 343.56 o 5 5 0 50.56 28.08 6.14 o 6 5 0 5011.79 5258.84 103.96 o 7 5 0 14.75 17.82 9.14 o 8 5 0 116.47 101.33 14.71 o 9 5 0 1967.14 1930.31 66.74 o 10 5 0 656.30 634.15 56.40 o 11 5 0 1791.03 1907.92 77.93 o 12 5 0 52.04 25.68 39.04 o 13 5 0 78.26 64.12 44.25 o 14 5 0 1123.23 1045.94 82.27 o -14 6 0 24.05 9.92 45.25 o -13 6 0 502.07 512.89 75.48 o -12 6 0 495.84 550.39 98.04 o -11 6 0 253.76 275.40 33.06 o -10 6 0 1910.03 1917.44 75.03 o -9 6 0 225.51 154.18 26.03 o -8 6 0 127.16 162.55 30.37 o -7 6 0 3308.16 3633.27 72.83 o -6 6 0 113.55 140.11 14.07 o -5 6 0 5603.79 5945.39 189.20 o -4 6 0 456.43 414.69 12.84 o -3 6 0 280.63 270.84 18.22 o -2 6 0 9478.41 9982.63 255.08 o -1 6 0 227.07 237.74 9.81 o 0 6 0 16019.01 17108.47 505.82 o 1 6 0 228.27 271.70 11.04 o 2 6 0 9232.61 9493.51 403.44 o 3 6 0 236.23 231.71 10.25 o 4 6 0 418.16 420.81 17.36 o 5 6 0 5315.81 5785.02 119.07 o 6 6 0 128.67 177.96 11.61 o 7 6 0 3299.55 3597.12 83.37 o 8 6 0 106.18 119.42 18.75 o 9 6 0 218.14 188.40 29.50 o 10 6 0 1905.21 2124.59 74.87 o 11 6 0 213.68 182.65 28.76 o 12 6 0 451.64 423.03 37.51 o 13 6 0 444.89 436.07 57.67 o 14 6 0 22.12 50.82 50.38 o -13 7 0 77.66 22.53 34.30 o -12 7 0 231.44 249.48 37.40 o -11 7 0 1054.42 1080.41 58.91 o -10 7 0 231.50 172.29 27.51 o -9 7 0 285.98 293.26 36.44 o -8 7 0 85.14 78.99 16.66 o -7 7 0 472.66 484.35 30.37 o -6 7 0 2930.39 3170.55 112.79 o -5 7 0 89.64 98.73 7.76 o -4 7 0 1014.06 972.67 33.45 o -3 7 0 645.06 636.10 29.43 o -2 7 0 1297.48 1305.61 51.19 o -1 7 0 1292.70 1310.89 29.69 o 0 7 0 529.87 414.17 14.12 o 1 7 0 1154.55 1132.92 42.51 o 2 7 0 1081.55 1036.28 48.38 o 3 7 0 653.06 640.69 19.24 o 4 7 0 970.45 953.22 26.58 o 5 7 0 88.57 102.01 18.22 o 6 7 0 2871.11 3059.00 88.49 o 7 7 0 472.71 489.87 34.95 o 8 7 0 71.21 52.24 17.51 o 9 7 0 281.10 310.07 35.57 o 10 7 0 275.52 209.05 25.13 o 11 7 0 1045.74 1086.82 50.82 o 12 7 0 209.56 272.46 43.38 o 13 7 0 71.31 24.77 40.44 o -13 8 0 105.51 94.64 38.06 o -12 8 0 36.56 84.72 39.80 o -11 8 0 23.11 32.36 41.65 o -10 8 0 781.51 858.04 44.67 o -9 8 0 21.91 53.79 29.50 o -8 8 0 442.88 522.31 45.12 o -7 8 0 7.19 -8.07 13.75 o -6 8 0 1172.96 1354.71 74.84 o -5 8 0 4386.69 4863.28 216.91 o -4 8 0 413.48 365.97 27.89 o -3 8 0 879.62 834.65 36.91 o -2 8 0 651.24 632.19 41.65 o -1 8 0 992.76 937.10 51.21 o 0 8 0 2331.04 2519.48 78.78 o 1 8 0 828.07 733.37 41.65 o 2 8 0 546.78 548.32 36.44 o 3 8 0 893.73 876.39 29.09 o 4 8 0 353.66 292.77 19.42 o 5 8 0 4343.64 4738.91 135.33 o 6 8 0 1001.78 1068.96 74.62 o 7 8 0 6.59 48.72 26.90 o 8 8 0 429.37 450.86 33.98 o 9 8 0 18.65 -1.11 25.66 o 10 8 0 797.03 838.06 128.42 o 11 8 0 21.28 47.43 32.59 o 12 8 0 33.77 65.56 45.25 o 13 8 0 89.06 59.00 64.21 o -12 9 0 160.67 138.25 37.05 o -11 9 0 201.23 228.44 35.57 o -10 9 0 49.27 19.09 27.76 o -9 9 0 365.59 337.07 32.08 o -8 9 0 509.34 532.73 46.85 o -7 9 0 1779.91 1920.13 84.19 o -6 9 0 432.85 365.88 31.27 o -5 9 0 815.94 754.38 53.59 o -4 9 0 6.47 -4.83 16.03 o -3 9 0 469.81 449.72 30.74 o -2 9 0 1359.13 1518.65 74.58 o -1 9 0 745.26 795.61 30.89 o 0 9 0 57.98 34.87 12.84 o 1 9 0 714.03 713.64 29.59 o 2 9 0 1287.57 1382.79 74.62 o 3 9 0 428.60 397.37 23.93 o 4 9 0 6.65 14.82 19.09 o 5 9 0 943.87 975.56 61.36 o 6 9 0 456.86 346.91 35.57 o 7 9 0 1644.40 1656.17 84.86 o 8 9 0 498.90 473.19 36.52 o 9 9 0 305.29 305.15 104.99 o 10 9 0 58.58 50.02 32.57 o 11 9 0 170.31 229.47 72.88 o 12 9 0 142.05 153.75 49.55 o -11 10 0 93.00 55.44 33.68 o -10 10 0 57.98 -6.94 45.12 o -9 10 0 1.75 -20.82 38.17 o -8 10 0 251.88 197.82 39.91 o -7 10 0 5.02 6.51 19.52 o -6 10 0 173.03 143.65 32.97 o -5 10 0 257.86 267.37 83.30 o -4 10 0 161.45 137.71 18.28 o -3 10 0 1273.77 1330.95 59.33 o -2 10 0 239.96 234.45 34.71 o -1 10 0 525.79 586.52 92.83 o 0 10 0 6531.58 7115.75 201.85 o 1 10 0 626.99 703.78 46.59 o 2 10 0 233.12 185.31 27.76 o 3 10 0 1199.48 1240.00 63.67 o 4 10 0 161.29 99.61 39.91 o 5 10 0 230.48 194.70 98.91 o 6 10 0 167.20 93.84 38.17 o 7 10 0 5.12 22.02 26.93 o 8 10 0 222.50 146.19 55.53 o 9 10 0 1.46 -2.94 39.28 o 10 10 0 48.50 61.28 50.32 o 11 10 0 83.90 16.04 43.31 o -10 11 0 9.33 10.41 36.44 o -9 11 0 39.71 17.35 39.91 o -8 11 0 26.34 33.19 23.90 o -7 11 0 62.41 60.73 45.12 o -6 11 0 258.99 165.93 30.04 o -5 11 0 73.21 68.43 47.72 o -4 11 0 13.77 -12.19 17.68 o -3 11 0 197.48 176.61 29.50 o -2 11 0 204.96 194.47 45.99 o -1 11 0 459.27 489.14 38.84 o 0 11 0 12.99 -4.86 15.01 o 1 11 0 387.01 320.55 34.70 o 2 11 0 223.31 218.49 25.37 o 3 11 0 201.29 169.07 50.32 o 4 11 0 14.95 35.40 32.97 o 5 11 0 82.30 45.25 42.51 o 6 11 0 234.74 191.08 66.81 o 7 11 0 57.32 39.85 28.23 o 8 11 0 31.03 -2.89 31.04 o 9 11 0 43.38 67.26 39.85 o 10 11 0 9.00 79.54 54.66 o -9 12 0 23.41 8.46 39.12 o -8 12 0 51.80 29.50 81.56 o -7 12 0 110.73 72.18 34.95 o -6 12 0 16.41 7.57 45.12 o -5 12 0 429.98 451.03 103.25 o -4 12 0 255.73 261.43 31.23 o -3 12 0 318.88 258.31 49.45 o -2 12 0 67.79 14.03 25.16 o -1 12 0 345.61 245.49 41.66 o 0 12 0 54.28 47.44 37.31 o 1 12 0 289.23 314.05 31.71 o 2 12 0 60.84 30.86 59.00 o 3 12 0 351.66 301.98 45.12 o 4 12 0 219.38 173.35 46.85 o 5 12 0 400.04 359.94 42.84 o 6 12 0 14.02 -4.60 34.71 o 7 12 0 132.75 148.24 36.50 o 8 12 0 54.70 61.33 42.96 o 9 12 0 27.78 51.63 80.69 o -8 13 0 33.65 1.16 40.44 o -7 13 0 67.60 98.91 48.59 o -6 13 0 303.12 209.96 46.85 o -5 13 0 30.38 63.79 34.60 o -4 13 0 27.03 48.68 44.25 o -3 13 0 60.85 82.13 26.05 o -2 13 0 90.87 26.95 61.60 o -1 13 0 171.71 103.31 33.82 o 0 13 0 171.54 143.31 35.19 o 1 13 0 193.46 156.43 30.71 o 2 13 0 78.29 16.10 44.25 o 3 13 0 60.30 11.55 60.73 o 4 13 0 28.04 37.44 35.35 o 5 13 0 35.82 60.90 33.79 o 6 13 0 331.29 244.68 47.00 o 7 13 0 56.43 41.26 61.60 o 8 13 0 40.35 -24.90 171.79 o -7 14 0 84.41 126.67 69.41 o -6 14 0 72.59 52.06 48.59 o -5 14 0 100.70 14.57 36.91 o -4 14 0 180.82 124.94 34.70 o -3 14 0 125.74 102.83 33.06 o -2 14 0 81.82 92.28 47.07 o -1 14 0 45.03 13.91 59.00 o 0 14 0 151.52 110.98 40.44 o 1 14 0 38.70 30.03 31.62 o 2 14 0 97.51 76.93 42.57 o 3 14 0 125.00 109.05 78.09 o 4 14 0 216.48 166.82 40.64 o 5 14 0 113.54 72.23 41.40 o 6 14 0 60.47 82.46 58.13 o 7 14 0 90.97 171.79 53.80 o -4 15 0 116.68 45.31 59.50 o -3 15 0 36.90 32.43 63.34 o -2 15 0 24.69 152.04 83.29 o -1 15 0 109.86 117.92 47.72 o 0 15 0 44.26 24.36 45.90 o 1 15 0 122.13 79.93 55.16 o 2 15 0 24.46 61.65 43.90 o 3 15 0 42.85 42.33 98.04 o 4 15 0 115.27 101.71 47.26 o -4 -15 1 249.16 116.87 78.50 o -3 -15 1 144.10 147.93 42.96 o -2 -15 1 643.97 526.82 61.76 o -1 -15 1 238.83 239.47 74.62 o 0 -15 1 118.92 7.09 56.67 o 1 -15 1 90.21 43.55 62.00 o 2 -15 1 36.89 4.19 56.40 o 3 -15 1 146.52 126.24 56.81 o 4 -15 1 49.02 83.29 83.29 o -7 -14 1 290.29 411.26 131.88 o -6 -14 1 243.75 132.13 49.96 o -5 -14 1 401.10 367.30 52.74 o -4 -14 1 365.76 340.12 50.62 o -3 -14 1 476.87 534.15 84.16 o -2 -14 1 63.17 99.44 41.65 o -1 -14 1 379.66 393.91 52.46 o 0 -14 1 76.63 75.05 48.35 o 1 -14 1 123.22 89.05 48.36 o 2 -14 1 303.09 207.25 46.85 o 3 -14 1 141.08 134.28 41.09 o 4 -14 1 251.70 183.69 35.02 o 5 -14 1 133.88 119.74 64.20 o 6 -14 1 96.28 112.79 50.33 o -8 -13 1 166.34 156.98 50.55 o -7 -13 1 797.86 568.14 108.45 o -6 -13 1 207.26 163.11 71.14 o -5 -13 1 256.58 225.50 43.46 o -4 -13 1 1001.29 1020.07 60.61 o -3 -13 1 402.12 445.73 46.39 o -2 -13 1 1219.88 1328.90 92.82 o -1 -13 1 487.49 534.96 44.16 o 0 -13 1 868.86 969.73 84.55 o 1 -13 1 1263.77 1385.14 87.09 o 2 -13 1 275.27 307.07 69.41 o 3 -13 1 466.65 476.35 39.53 o 4 -13 1 367.02 377.32 45.11 o 5 -13 1 336.66 398.35 45.72 o 6 -13 1 520.64 635.11 72.88 o 7 -13 1 92.59 78.09 48.59 o 8 -13 1 204.15 105.85 38.17 o -10 -12 1 391.73 423.41 64.20 o -9 -12 1 189.75 239.11 116.27 o -8 -12 1 563.78 531.12 51.17 o -7 -12 1 293.57 249.17 58.13 o -6 -12 1 1216.69 1273.50 137.11 o -5 -12 1 1698.61 1935.94 131.75 o -4 -12 1 245.18 258.46 32.22 o -3 -12 1 1472.16 1605.88 80.93 o -2 -12 1 689.90 714.13 60.74 o -1 -12 1 755.55 740.19 52.95 o 0 -12 1 2840.27 3072.79 182.01 o 1 -12 1 794.95 700.94 67.19 o 2 -12 1 3578.98 3725.59 174.13 o 3 -12 1 862.04 938.63 82.41 o 4 -12 1 897.37 910.17 106.08 o 5 -12 1 837.01 913.77 150.97 o 6 -12 1 333.28 295.07 41.41 o 7 -12 1 717.88 678.49 55.52 o 8 -12 1 87.21 81.56 48.59 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