#------------------------------------------------------------------------------ #$Date: 2012-09-11 12:26:43 +0300 (Tue, 11 Sep 2012) $ #$Revision: 66590 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/10/51/2105178.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_2105178_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 90.030 _cell_angle_beta 105.460 _cell_angle_gamma 90.010 _cell_length_a 12.1560 _cell_length_b 12.1710 _cell_length_c 16.0710 _exptl_crystal_F_000 1096.00 _reflns_d_resolution_high 0.7696 _[local]_cod_data_source_file hw5021130K_IV_1sup8.hkl _[local]_cod_data_source_block 130K_IV_1 #BEGIN Tags that were not found in dictionaries: _shelx_title ' k06087 in P-1' _shelx_refln_list_code 4 _shelx_f_calc_maximum 293.78 _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 5781.91 5520.42 78.64 o 2 0 0 24263.39 24524.67 381.47 o 3 0 0 609.05 758.83 13.95 o 4 0 0 1446.54 1321.36 20.36 o 5 0 0 46683.40 50400.11 901.45 o 6 0 0 1297.00 1290.51 32.56 o 7 0 0 11198.27 11373.62 175.22 o 8 0 0 6987.82 7223.50 121.48 o 9 0 0 657.14 831.12 40.93 o 10 0 0 371.08 419.48 13.82 o 11 0 0 1423.04 1401.40 43.30 o 12 0 0 2631.82 2959.72 85.03 o 13 0 0 1759.69 1741.70 77.33 o 14 0 0 65.88 24.30 33.07 o 15 0 0 346.03 283.94 43.72 o -15 1 0 28.49 -24.19 27.63 o -14 1 0 291.94 278.38 55.82 o -13 1 0 389.19 359.65 34.13 o -12 1 0 1750.43 1793.48 51.97 o -11 1 0 4378.87 4630.96 113.49 o -10 1 0 536.98 520.97 70.70 o -9 1 0 807.15 903.68 36.28 o -8 1 0 147.54 120.95 26.05 o -7 1 0 2732.76 2573.58 74.42 o -6 1 0 14487.48 14974.37 503.28 o -5 1 0 1980.94 2228.07 34.21 o -4 1 0 17316.62 17691.12 273.07 o -3 1 0 10383.38 9774.17 241.87 o -2 1 0 1015.75 1097.68 18.61 o 0 1 0 26.02 29.77 1.32 o 2 1 0 989.72 1051.49 15.09 o 3 1 0 10249.59 9767.86 135.93 o 4 1 0 17356.96 17495.62 276.30 o 5 1 0 2094.59 2275.44 36.28 o 6 1 0 14385.86 14951.68 277.23 o 7 1 0 2575.40 2499.99 40.68 o 8 1 0 154.72 102.77 9.57 o 9 1 0 832.60 916.76 22.73 o 10 1 0 565.48 541.84 46.51 o 11 1 0 4522.60 4809.45 102.38 o 12 1 0 1709.86 1792.32 146.05 o 13 1 0 421.04 495.80 95.82 o 14 1 0 287.12 271.60 37.85 o 15 1 0 32.36 0.45 32.81 o -15 2 0 899.10 821.60 67.01 o -14 2 0 69.88 108.63 34.42 o -13 2 0 536.33 581.40 45.05 o -12 2 0 1282.66 1399.35 104.19 o -11 2 0 37.85 26.20 14.59 o -10 2 0 3813.25 4301.72 104.26 o -9 2 0 1787.49 1843.27 44.72 o -8 2 0 4567.18 4842.02 93.11 o -7 2 0 5828.60 5917.86 186.06 o -6 2 0 380.11 316.76 15.81 o -5 2 0 18747.20 19002.20 341.42 o -4 2 0 1151.80 1105.74 35.35 o -3 2 0 9143.11 8588.00 210.24 o -2 2 0 2847.55 3126.06 58.61 o -1 2 0 1091.38 1013.30 18.58 o 0 2 0 11111.19 10590.25 146.02 o 1 2 0 1028.43 974.86 14.29 o 2 2 0 2810.11 3026.44 42.74 o 3 2 0 9515.82 8869.49 111.31 o 4 2 0 1320.05 1259.48 19.04 o 5 2 0 19211.42 19648.13 356.30 o 6 2 0 428.58 383.12 10.23 o 7 2 0 5983.40 6007.30 139.54 o 8 2 0 4409.55 4790.44 125.59 o 9 2 0 1809.43 1857.03 37.32 o 10 2 0 3906.66 4321.28 125.59 o 11 2 0 43.11 67.49 14.98 o 12 2 0 1325.28 1433.31 51.62 o 13 2 0 533.03 548.81 32.67 o 14 2 0 76.02 58.05 27.04 o 15 2 0 903.31 900.20 61.17 o -14 3 0 550.80 486.21 72.56 o -13 3 0 16.35 12.65 25.65 o -12 3 0 45.04 98.32 33.49 o -11 3 0 3381.74 3092.20 145.12 o -10 3 0 793.98 830.20 41.86 o -9 3 0 4964.44 5123.96 100.71 o -8 3 0 1505.95 1670.02 40.56 o -7 3 0 976.38 991.85 24.08 o -6 3 0 1228.52 1004.98 26.98 o -5 3 0 1977.13 1984.34 28.59 o -4 3 0 19148.67 19502.96 637.25 o -3 3 0 9568.56 9440.58 280.02 o -2 3 0 5485.29 5391.79 91.06 o -1 3 0 4705.81 4920.11 76.79 o 0 3 0 3.31 10.27 1.86 o 1 3 0 4639.55 4875.37 88.38 o 2 3 0 5381.63 5251.24 88.06 o 3 3 0 10238.42 10047.79 123.33 o 4 3 0 19648.73 20130.83 413.05 o 5 3 0 1779.57 1861.71 27.63 o 6 3 0 1279.71 1024.32 16.41 o 7 3 0 876.27 953.83 22.71 o 8 3 0 1500.62 1653.95 34.37 o 9 3 0 4899.97 5052.45 98.09 o 10 3 0 775.90 821.07 27.04 o 11 3 0 3291.68 3237.17 87.68 o 12 3 0 41.92 70.12 23.00 o 13 3 0 15.29 22.33 21.67 o 14 3 0 536.70 569.12 75.35 o -14 4 0 39.44 43.49 28.72 o -13 4 0 108.51 70.07 26.42 o -12 4 0 276.75 151.27 22.33 o -11 4 0 147.34 115.79 27.52 o -10 4 0 3737.37 3473.18 114.43 o -9 4 0 248.61 165.93 15.13 o -8 4 0 3900.86 3957.57 166.52 o -7 4 0 4512.27 4768.90 86.71 o -6 4 0 692.09 746.99 15.62 o -5 4 0 11492.88 11761.86 198.15 o -4 4 0 1548.50 1666.80 35.45 o -3 4 0 8444.86 9043.66 198.15 o -2 4 0 13534.49 13324.38 580.50 o -1 4 0 2179.44 2411.22 46.51 o 0 4 0 46340.25 46613.84 840.98 o 1 4 0 2053.48 2185.75 55.82 o 2 4 0 14333.16 14135.09 210.47 o 3 4 0 8154.72 8708.60 122.45 o 4 4 0 1388.84 1503.94 25.92 o 5 4 0 11168.68 11700.43 158.15 o 6 4 0 674.92 735.87 15.79 o 7 4 0 4480.75 4844.77 90.24 o 8 4 0 3778.69 3798.73 63.38 o 9 4 0 255.09 157.19 13.40 o 10 4 0 3662.52 3444.48 80.26 o 11 4 0 147.97 137.74 20.63 o 12 4 0 252.39 133.73 48.37 o 13 4 0 102.44 33.49 35.52 o 14 4 0 39.86 -30.70 38.15 o -14 5 0 984.50 980.98 110.70 o -13 5 0 74.28 65.12 29.77 o -12 5 0 18.98 38.48 30.86 o -11 5 0 1750.33 1847.55 91.17 o -10 5 0 517.08 414.17 26.63 o -9 5 0 1996.65 1911.89 96.75 o -8 5 0 80.01 75.63 16.75 o -7 5 0 6.22 5.21 5.13 o -6 5 0 4960.45 5066.07 109.77 o -5 5 0 43.73 28.03 5.26 o -4 5 0 7099.41 7339.51 132.10 o -3 5 0 9374.33 9675.41 213.04 o -2 5 0 10398.79 11420.76 351.65 o -1 5 0 12525.56 12656.88 349.79 o 0 5 0 396.79 275.15 12.09 o 1 5 0 12506.33 12748.17 213.97 o 2 5 0 10103.74 10581.16 155.74 o 3 5 0 9510.94 9938.28 138.02 o 4 5 0 6609.05 6972.87 107.04 o 5 5 0 38.38 17.16 5.81 o 6 5 0 4638.12 5008.34 163.73 o 7 5 0 5.85 7.30 13.95 o 8 5 0 84.89 104.12 13.02 o 9 5 0 1920.32 1810.34 66.98 o 10 5 0 458.67 368.00 25.92 o 11 5 0 1658.06 1700.25 59.59 o 12 5 0 19.48 42.22 24.44 o 13 5 0 70.45 54.03 43.72 o 14 5 0 944.09 835.73 61.67 o -14 6 0 15.68 34.87 43.32 o -13 6 0 315.53 388.44 41.96 o -12 6 0 391.53 438.04 38.10 o -11 6 0 91.05 182.09 77.21 o -10 6 0 1788.31 1904.49 70.72 o -9 6 0 120.50 77.52 26.98 o -8 6 0 88.41 105.56 17.68 o -7 6 0 3092.49 3379.82 72.36 o -6 6 0 108.88 150.27 22.33 o -5 6 0 5380.43 5581.55 189.78 o -4 6 0 517.60 423.53 12.04 o -3 6 0 212.36 164.44 10.28 o -2 6 0 9542.18 10368.21 189.78 o -1 6 0 93.11 112.17 6.19 o 0 6 0 16469.99 17592.46 385.14 o 1 6 0 89.61 145.48 8.48 o 2 6 0 9285.20 10022.25 143.46 o 3 6 0 184.42 132.32 22.33 o 4 6 0 471.94 434.72 12.68 o 5 6 0 5166.66 5701.88 98.34 o 6 6 0 98.37 161.33 11.16 o 7 6 0 3070.69 3355.07 72.41 o 8 6 0 85.76 98.80 22.33 o 9 6 0 117.37 76.27 17.43 o 10 6 0 1784.61 2018.11 66.05 o 11 6 0 78.57 71.82 29.77 o 12 6 0 374.95 399.83 88.38 o 13 6 0 308.91 322.79 44.06 o 14 6 0 14.13 -5.61 43.72 o -13 7 0 54.10 30.95 32.31 o -12 7 0 157.65 268.05 45.58 o -11 7 0 933.11 1042.97 43.35 o -10 7 0 221.03 114.36 30.70 o -9 7 0 242.73 314.44 27.91 o -8 7 0 43.75 53.36 25.12 o -7 7 0 467.86 478.04 36.28 o -6 7 0 2800.87 3090.11 63.80 o -5 7 0 28.54 45.07 6.66 o -4 7 0 978.79 1041.99 28.60 o -3 7 0 759.88 734.03 22.77 o -2 7 0 885.06 813.00 28.54 o -1 7 0 1361.39 1410.71 28.72 o 0 7 0 299.04 171.25 8.32 o 1 7 0 1261.87 1311.20 35.31 o 2 7 0 766.32 694.65 25.27 o 3 7 0 770.12 744.93 26.05 o 4 7 0 991.35 1017.23 22.41 o 5 7 0 27.64 55.82 10.59 o 6 7 0 2828.74 3091.39 85.04 o 7 7 0 506.49 468.34 50.24 o 8 7 0 42.52 39.64 15.09 o 9 7 0 255.19 280.04 25.12 o 10 7 0 253.80 152.29 23.00 o 11 7 0 944.50 1071.25 51.17 o 12 7 0 159.96 200.42 33.38 o 13 7 0 50.23 26.93 37.48 o -13 8 0 93.81 114.90 35.26 o -12 8 0 32.74 54.42 51.17 o -11 8 0 23.53 -9.83 31.26 o -10 8 0 632.43 751.90 43.18 o -9 8 0 9.13 20.47 26.05 o -8 8 0 347.89 385.14 33.49 o -7 8 0 34.30 16.95 11.62 o -6 8 0 855.34 1023.08 47.44 o -5 8 0 4467.22 4669.65 112.04 o -4 8 0 278.70 234.80 23.26 o 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558.08 389.69 26.98 o 7 9 0 1473.70 1552.88 65.33 o 8 9 0 375.17 351.31 31.93 o 9 9 0 184.01 146.25 31.27 o 10 9 0 28.80 14.37 32.56 o 11 9 0 149.24 148.52 36.44 o 12 9 0 144.75 149.13 45.00 o -11 10 0 62.01 -19.72 27.87 o -10 10 0 66.91 78.37 39.07 o -9 10 0 0.99 7.44 35.35 o -8 10 0 199.40 120.94 27.91 o -7 10 0 4.75 -4.39 16.41 o -6 10 0 97.52 63.84 14.29 o -5 10 0 292.14 183.53 23.06 o -4 10 0 74.20 62.68 13.77 o -3 10 0 1167.48 1438.73 54.94 o -2 10 0 116.42 130.39 19.04 o -1 10 0 359.83 392.37 21.98 o 0 10 0 6910.44 7500.26 157.23 o 1 10 0 401.40 484.34 26.35 o 2 10 0 110.39 90.29 46.51 o 3 10 0 1126.22 1214.89 50.05 o 4 10 0 76.54 40.11 16.09 o 5 10 0 265.77 169.12 42.79 o 6 10 0 91.38 44.77 19.96 o 7 10 0 4.81 31.63 21.63 o 8 10 0 173.74 99.50 25.12 o 9 10 0 1.12 -11.96 27.52 o 10 10 0 59.22 50.38 37.73 o 11 10 0 61.46 53.49 43.08 o -10 11 0 7.78 18.61 33.49 o -9 11 0 13.25 -27.91 27.91 o -8 11 0 13.31 42.17 23.30 o -7 11 0 83.16 80.00 37.21 o -6 11 0 255.87 207.04 27.18 o -5 11 0 52.85 13.02 25.12 o -4 11 0 23.76 0.00 15.14 o -3 11 0 144.19 152.42 39.07 o -2 11 0 182.55 146.84 24.79 o -1 11 0 437.59 437.16 29.92 o 0 11 0 19.06 -6.27 12.04 o 1 11 0 399.43 356.25 25.86 o 2 11 0 185.22 176.60 23.93 o 3 11 0 148.24 145.51 19.35 o 4 11 0 23.64 1.92 17.68 o 5 11 0 56.46 83.23 24.96 o 6 11 0 242.03 158.82 28.05 o 7 11 0 77.33 55.08 51.17 o 8 11 0 15.10 29.53 30.12 o 9 11 0 13.31 -3.97 60.47 o 10 11 0 7.05 -7.63 46.51 o -9 12 0 19.77 68.91 35.23 o -8 12 0 39.67 0.00 37.21 o -7 12 0 74.40 45.12 33.50 o -6 12 0 12.38 18.61 26.37 o -5 12 0 419.19 461.50 49.31 o -4 12 0 175.45 215.84 22.33 o -3 12 0 387.65 326.20 28.85 o -2 12 0 18.46 49.31 23.68 o -1 12 0 213.46 214.20 30.12 o 0 12 0 37.51 45.62 21.40 o 1 12 0 187.30 198.07 22.19 o 2 12 0 16.24 16.46 15.78 o 3 12 0 419.17 310.08 24.44 o 4 12 0 159.87 94.57 36.28 o 5 12 0 414.11 458.17 52.10 o 6 12 0 11.03 -21.28 46.51 o 7 12 0 81.40 96.85 31.78 o 8 12 0 35.55 34.00 32.33 o 9 12 0 21.38 37.24 37.07 o -8 13 0 26.46 22.46 44.05 o -7 13 0 39.43 42.79 42.79 o -6 13 0 305.49 199.08 44.65 o -5 13 0 15.38 7.59 51.17 o -4 13 0 43.27 53.16 20.73 o -3 13 0 33.60 70.78 22.33 o -2 13 0 91.32 148.98 74.42 o -1 13 0 159.87 155.02 30.64 o 0 13 0 69.91 128.17 26.21 o 1 13 0 167.44 148.54 31.93 o 2 13 0 87.93 55.68 27.25 o 3 13 0 34.88 -8.33 24.79 o 4 13 0 47.64 57.85 32.31 o 5 13 0 17.71 6.90 30.12 o 6 13 0 311.18 178.25 34.00 o 7 13 0 34.15 61.60 42.54 o 8 13 0 30.23 40.74 42.89 o -7 14 0 41.93 78.14 42.79 o -6 14 0 43.22 63.26 53.96 o -5 14 0 110.69 10.41 35.44 o -4 14 0 116.15 84.38 34.40 o -3 14 0 143.49 111.14 36.28 o -2 14 0 55.50 12.77 40.00 o -1 14 0 35.36 95.82 33.50 o 0 14 0 131.24 50.16 33.01 o 1 14 0 32.15 -8.40 24.31 o 2 14 0 63.87 33.18 32.07 o 3 14 0 139.07 111.71 30.70 o 4 14 0 130.36 126.77 30.90 o 5 14 0 116.57 133.77 117.22 o 6 14 0 38.54 55.31 41.43 o 7 14 0 46.40 133.72 78.14 o -4 15 0 94.76 82.56 66.98 o -3 15 0 27.07 31.82 52.58 o -2 15 0 21.57 40.39 47.76 o -1 15 0 92.02 77.03 40.25 o 0 15 0 13.49 -25.90 58.61 o 1 15 0 99.41 57.78 55.82 o 2 15 0 23.27 -8.25 39.40 o 3 15 0 30.43 3.72 39.94 o 4 15 0 97.05 99.47 45.58 o -4 -15 1 252.23 176.77 65.96 o -3 -15 1 102.24 29.54 42.35 o -2 -15 1 698.32 524.99 56.90 o -1 -15 1 161.07 149.45 52.43 o 0 -15 1 94.90 45.86 44.50 o 1 -15 1 104.09 60.62 43.94 o 2 -15 1 7.50 11.16 73.49 o 3 -15 1 175.82 83.48 59.84 o 4 -15 1 16.89 -20.47 78.14 o -7 -14 1 272.53 199.12 60.76 o -6 -14 1 211.87 166.63 42.73 o -5 -14 1 358.18 309.86 45.58 o -4 -14 1 307.19 239.08 38.00 o -3 -14 1 495.49 472.76 83.73 o -2 -14 1 20.64 -8.84 28.15 o -1 -14 1 356.27 403.76 45.00 o 0 -14 1 45.22 24.42 41.85 o 1 -14 1 131.02 145.74 37.10 o 2 -14 1 332.66 314.83 35.52 o 3 -14 1 60.89 25.51 34.75 o 4 -14 1 302.96 251.18 30.63 o 5 -14 1 89.40 174.89 35.35 o 6 -14 1 34.35 98.61 35.35 o -8 -13 1 51.77 100.21 70.70 o -7 -13 1 729.44 519.48 51.30 o -6 -13 1 170.14 160.27 34.40 o -5 -13 1 191.12 182.81 33.74 o -4 -13 1 972.19 1011.96 80.93 o -3 -13 1 179.45 236.30 36.07 o -2 -13 1 1179.54 1210.69 52.98 o -1 -13 1 333.88 403.52 47.44 o 0 -13 1 725.76 767.73 56.48 o 1 -13 1 1284.40 1338.94 76.28 o 2 -13 1 97.17 190.10 60.47 o 3 -13 1 519.70 538.98 50.24 o 4 -13 1 217.12 258.75 36.61 o 5 -13 1 318.09 297.34 39.20 o 6 -13 1 457.11 561.89 55.82 o 7 -13 1 62.66 58.80 29.78 o 8 -13 1 195.31 170.91 53.03 o -10 -12 1 333.83 388.07 56.01 o -9 -12 1 170.49 142.87 40.66 o -8 -12 1 540.95 498.79 52.10 o -7 -12 1 120.23 173.06 33.49 o -6 -12 1 1196.34 1269.55 62.24 o -5 -12 1 1325.99 1460.79 75.87 o -4 -12 1 165.65 146.14 24.09 o -3 -12 1 1347.07 1365.40 94.89 o -2 -12 1 657.59 617.53 35.91 o -1 -12 1 641.85 654.92 35.72 o 0 -12 1 2284.82 2599.11 114.97 o 1 -12 1 646.30 576.60 49.53 o 2 -12 1 3191.38 3548.67 140.59 o 3 -12 1 694.01 702.35 54.89 o 4 -12 1 775.80 936.48 83.71 o 5 -12 1 783.01 829.76 46.43 o 6 -12 1 228.99 230.24 27.53 o 7 -12 1 665.36 729.34 53.96 o 8 -12 1 34.29 76.28 35.35 o 9 -12 1 485.07 496.77 50.24 o -11 -11 1 149.23 189.76 82.80 o -10 -11 1 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71.27 37.21 o -2 0 20 918.44 860.92 68.13 o -1 0 20 604.76 501.52 40.21 o 0 0 20 119.06 122.02 78.90 o -8 1 20 190.81 109.77 57.68 o -7 1 20 8.82 -33.98 48.37 o -6 1 20 176.90 135.59 43.59 o -5 1 20 242.94 149.18 51.17 o -4 1 20 44.27 72.15 36.83 o -3 1 20 566.41 709.29 85.24 o -2 1 20 174.24 159.01 49.20 o -1 1 20 109.66 34.32 57.08 o 0 1 20 16.75 -32.95 53.17 o -7 2 20 184.71 171.95 53.53 o -6 2 20 261.69 279.63 50.24 o -5 2 20 175.85 119.39 65.43 o -4 2 20 369.17 134.99 131.17 o -3 2 20 28.60 -40.26 40.26 o -2 2 20 330.94 263.30 68.99 o -1 2 20 83.86 14.88 78.14 o -7 3 20 24.81 37.43 68.26 o -6 3 20 525.03 534.07 70.70 o -5 3 20 353.83 315.45 55.22 o -4 3 20 2.17 -89.31 89.31 o -3 3 20 473.53 334.90 85.59 o -2 3 20 16.06 -93.03 93.03 o -1 3 20 40.95 -24.19 66.98 o -6 4 20 13.27 -27.91 55.82 o -4 4 20 175.84 53.96 91.17 o -3 4 20 59.11 163.73 93.03 o