#------------------------------------------------------------------------------ #$Date: 2012-09-11 12:26:43 +0300 (Tue, 11 Sep 2012) $ #$Revision: 66590 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/10/51/2105183.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_2105183_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 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 105.450 _cell_angle_gamma 90.000 _cell_length_a 12.1690 _cell_length_b 12.2140 _cell_length_c 16.1330 _exptl_crystal_F_000 1096.00 _reflns_d_resolution_high 0.7697 _[local]_cod_data_source_file hw5021180K_III_1sup13.hkl _[local]_cod_data_source_block 180K_III_1 #BEGIN Tags that were not found in dictionaries: _shelx_title ' k06092 in P2(1)/c' _shelx_refln_list_code 4 _shelx_f_calc_maximum 338.05 _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 5906.73 5580.38 91.81 o 2 0 0 24688.47 24397.21 399.17 o 3 0 0 700.74 794.35 19.96 o 4 0 0 1346.66 1229.44 23.95 o 5 0 0 42178.36 46375.46 702.54 o 6 0 0 1333.98 1349.19 31.93 o 7 0 0 9485.45 10178.81 171.64 o 8 0 0 6469.50 6961.51 143.70 o 9 0 0 486.87 538.88 31.93 o 10 0 0 366.69 375.22 27.94 o 11 0 0 966.10 930.06 55.88 o 12 0 0 1750.72 1784.29 95.80 o 13 0 0 1054.54 1069.77 95.80 o 14 0 0 31.90 35.93 63.87 o 15 0 0 201.42 199.58 99.79 o 1 1 0 45310.26 44447.76 645.18 o 2 1 0 1051.50 1078.29 23.95 o 3 1 0 9849.09 9190.93 122.75 o 4 1 0 16936.60 17123.30 200.16 o 5 1 0 1773.67 1764.33 23.87 o 6 1 0 13089.17 13612.17 157.99 o 7 1 0 2321.53 2331.60 71.85 o 8 1 0 115.65 103.78 12.47 o 9 1 0 732.92 687.91 24.94 o 10 1 0 320.02 309.37 19.76 o 11 1 0 3072.28 3490.74 93.02 o 12 1 0 1166.79 1174.56 69.10 o 13 1 0 243.19 204.45 50.57 o 14 1 0 190.34 197.59 59.27 o 15 1 0 2.73 67.78 67.57 o 0 2 0 11755.51 11154.20 203.92 o 1 2 0 1051.93 1022.09 23.95 o 2 2 0 2777.20 2979.34 39.21 o 3 2 0 9111.96 8344.99 107.33 o 4 2 0 785.74 824.68 17.96 o 5 2 0 18253.27 18797.11 207.44 o 6 2 0 87.04 82.27 8.47 o 7 2 0 5074.18 5359.78 87.36 o 8 2 0 3622.51 3981.65 73.22 o 9 2 0 1246.95 1269.98 32.48 o 10 2 0 2877.14 3382.25 73.85 o 11 2 0 2.82 7.69 37.92 o 12 2 0 842.85 858.59 61.94 o 13 2 0 340.19 337.90 56.35 o 14 2 0 37.73 14.64 53.70 o 15 2 0 448.52 518.41 81.97 o 1 3 0 4834.33 5047.98 72.74 o 2 3 0 5243.30 5192.41 65.93 o 3 3 0 9205.35 9149.51 161.66 o 4 3 0 17809.28 18352.47 223.91 o 5 3 0 1426.83 1321.30 25.40 o 6 3 0 1026.00 958.35 21.03 o 7 3 0 759.71 746.11 22.06 o 8 3 0 1341.53 1420.35 39.92 o 9 3 0 3726.48 3982.79 75.75 o 10 3 0 634.95 635.06 32.37 o 11 3 0 2172.44 2372.48 87.54 o 12 3 0 32.23 29.69 43.91 o 13 3 0 5.75 -34.81 75.84 o 14 3 0 324.37 324.04 86.35 o 0 4 0 44762.35 44704.23 1512.85 o 1 4 0 2194.64 2170.43 65.86 o 2 4 0 13188.55 13139.50 395.18 o 3 4 0 8136.87 8359.25 175.63 o 4 4 0 1041.54 980.81 16.24 o 5 4 0 9930.46 10435.02 237.51 o 6 4 0 736.68 729.38 37.92 o 7 4 0 3818.66 4125.96 78.88 o 8 4 0 3161.53 3356.96 83.83 o 9 4 0 117.24 91.52 15.33 o 10 4 0 2566.83 2799.07 139.71 o 11 4 0 82.48 83.83 35.70 o 12 4 0 126.68 124.82 43.18 o 13 4 0 67.65 -24.39 40.19 o 14 4 0 22.45 -56.06 56.06 o 1 5 0 12208.17 12234.72 552.85 o 2 5 0 10279.20 11010.41 329.31 o 3 5 0 9010.31 9070.89 297.38 o 4 5 0 6701.69 6944.89 121.75 o 5 5 0 8.85 9.58 5.99 o 6 5 0 4184.09 4195.08 70.39 o 7 5 0 6.08 -7.98 13.29 o 8 5 0 53.82 41.73 15.33 o 9 5 0 1465.40 1410.56 87.82 o 10 5 0 298.88 187.49 33.21 o 11 5 0 1154.88 1248.68 87.82 o 12 5 0 2.31 -29.31 65.86 o 13 5 0 37.55 -33.64 54.39 o 14 5 0 532.46 528.91 81.54 o 0 6 0 17143.90 18071.85 814.30 o 1 6 0 15.40 26.23 7.41 o 2 6 0 9449.32 9882.28 309.36 o 3 6 0 195.90 186.07 19.96 o 4 6 0 412.57 415.56 15.33 o 5 6 0 5213.92 5298.52 81.83 o 6 6 0 79.59 81.74 18.18 o 7 6 0 2595.25 2663.74 68.08 o 8 6 0 130.31 127.86 19.76 o 9 6 0 22.62 8.60 18.18 o 10 6 0 1573.63 1590.68 139.71 o 11 6 0 63.70 46.94 34.53 o 12 6 0 286.81 188.18 63.87 o 13 6 0 219.51 137.41 68.51 o 14 6 0 11.03 -31.68 107.78 o 1 7 0 1647.42 1669.91 29.18 o 2 7 0 394.40 430.70 23.95 o 3 7 0 901.44 881.02 23.57 o 4 7 0 1101.27 1062.07 24.94 o 5 7 0 0.02 1.50 10.27 o 6 7 0 2718.66 2912.76 43.49 o 7 7 0 369.67 345.70 29.54 o 8 7 0 43.63 0.92 18.18 o 9 7 0 306.44 202.18 41.91 o 10 7 0 90.34 110.77 33.52 o 11 7 0 787.65 752.04 58.47 o 12 7 0 140.78 170.70 61.94 o 13 7 0 14.14 -5.94 58.00 o 0 8 0 2774.78 2827.94 89.81 o 1 8 0 417.58 359.25 15.43 o 2 8 0 151.23 171.24 19.96 o 3 8 0 873.32 857.73 39.92 o 4 8 0 80.05 89.99 17.96 o 5 8 0 4302.64 4483.54 83.37 o 6 8 0 585.77 719.82 51.89 o 7 8 0 79.56 98.97 25.83 o 8 8 0 311.05 275.19 33.87 o 9 8 0 11.23 -11.98 27.94 o 10 8 0 534.71 527.79 67.86 o 11 8 0 18.95 -41.22 41.22 o 12 8 0 31.13 19.19 51.89 o 13 8 0 65.19 188.06 153.68 o 1 9 0 840.86 786.49 47.90 o 2 9 0 1304.23 1334.51 71.85 o 3 9 0 225.50 207.54 83.83 o 4 9 0 66.78 44.36 14.82 o 5 9 0 399.10 378.84 28.89 o 6 9 0 495.59 474.97 71.85 o 7 9 0 1224.70 1147.33 55.88 o 8 9 0 213.34 185.92 35.20 o 9 9 0 127.82 83.83 31.93 o 10 9 0 27.90 6.65 38.03 o 11 9 0 91.64 7.98 93.80 o 12 9 0 78.83 31.93 67.86 o 0 10 0 6680.77 7193.03 171.64 o 1 10 0 166.89 203.58 15.97 o 2 10 0 31.21 12.47 19.96 o 3 10 0 876.23 981.37 36.85 o 4 10 0 0.03 -33.93 67.86 o 5 10 0 210.74 155.68 25.84 o 6 10 0 27.55 28.90 35.93 o 7 10 0 14.82 57.36 34.41 o 8 10 0 112.42 47.90 35.70 o 9 10 0 0.02 29.03 41.59 o 10 10 0 40.95 47.90 55.88 o 11 10 0 31.37 19.96 63.87 o 1 11 0 428.87 407.15 23.95 o 2 11 0 90.31 106.39 63.87 o 3 11 0 51.57 55.16 25.32 o 4 11 0 46.31 17.56 24.60 o 5 11 0 49.49 47.90 25.84 o 6 11 0 255.50 257.95 43.91 o 7 11 0 93.82 15.17 39.86 o 8 11 0 0.10 -6.65 41.91 o 9 11 0 3.05 11.98 63.87 o 10 11 0 3.06 -75.84 87.82 o 0 12 0 1.85 15.97 47.90 o 1 12 0 55.57 63.87 35.93 o 2 12 0 0.03 11.98 35.70 o 3 12 0 449.63 374.66 48.72 o 4 12 0 51.87 168.26 43.51 o 5 12 0 509.46 445.51 76.21 o 6 12 0 1.72 -16.38 53.70 o 7 12 0 9.67 54.55 54.99 o 8 12 0 10.41 23.95 83.83 o 9 12 0 11.50 39.92 127.73 o 1 13 0 49.48 9.12 36.86 o 2 13 0 132.60 4.10 107.78 o 3 13 0 10.88 16.48 43.14 o 4 13 0 127.45 56.83 56.11 o 5 13 0 3.34 -28.97 52.43 o 6 13 0 106.21 0.00 79.83 o 7 13 0 0.94 -79.83 79.83 o 8 13 0 3.60 123.74 87.82 o 0 14 0 22.30 87.82 127.73 o 1 14 0 17.74 -6.84 47.90 o 2 14 0 8.88 -6.12 55.92 o 3 14 0 52.00 22.29 67.04 o 4 14 0 58.07 48.55 68.08 o 5 14 0 34.45 79.83 123.74 o 6 14 0 7.32 47.90 115.76 o 7 14 0 0.36 -11.98 139.71 o 1 15 0 31.26 28.44 77.79 o 2 15 0 6.12 -15.24 79.83 o 3 15 0 7.53 83.63 139.71 o 4 15 0 32.92 0.00 83.83 o -15 1 1 0.49 55.36 64.73 o -14 1 1 52.86 -37.39 41.22 o -13 1 1 2.99 24.84 49.87 o -12 1 1 60.86 31.93 30.81 o -11 1 1 145.45 114.05 19.16 o -10 1 1 28.15 35.93 10.71 o -9 1 1 1214.08 1314.99 73.85 o -8 1 1 347.43 375.45 16.24 o -7 1 1 1388.46 1441.10 31.05 o -6 1 1 0.10 -0.80 6.64 o -5 1 1 984.43 973.38 18.18 o -4 1 1 46.75 40.78 3.57 o -3 1 1 16.50 19.96 2.82 o -2 1 1 4.60 7.98 2.82 o -1 1 1 17.39 9.98 2.82 o 0 1 1 35.26 34.05 2.82 o 1 1 1 3.82 3.99 2.82 o 2 1 1 127.58 119.75 3.57 o 3 1 1 197.58 185.64 5.65 o 4 1 1 818.91 819.25 15.33 o 5 1 1 180.10 171.74 8.47 o 6 1 1 2136.78 2276.13 32.37 o 7 1 1 168.95 159.77 11.29 o 8 1 1 438.66 421.13 16.94 o 9 1 1 1.33 -3.99 14.11 o 10 1 1 17.38 19.23 15.33 o 11 1 1 30.91 35.93 19.93 o 12 1 1 25.90 49.07 39.61 o 13 1 1 44.82 132.67 67.07 o 14 1 1 1.85 57.25 56.58 o -15 2 1 43.81 91.24 67.06 o -14 2 1 0.19 29.39 60.38 o -13 2 1 54.66 29.70 47.90 o -12 2 1 35.49 39.92 29.43 o -11 2 1 114.36 104.58 28.89 o -10 2 1 570.58 579.66 26.70 o -9 2 1 32.75 30.60 12.47 o -8 2 1 606.40 651.85 17.45 o -7 2 1 4.26 1.33 7.98 o -6 2 1 1488.03 1486.47 24.94 o -5 2 1 98.47 112.25 11.98 o -4 2 1 242.13 221.56 9.58 o -3 2 1 245.86 244.54 15.97 o -2 2 1 3.46 7.98 2.82 o -1 2 1 628.18 549.04 9.98 o 0 2 1 272.51 269.45 5.65 o 1 2 1 1041.45 962.15 16.94 o 2 2 1 341.20 317.45 8.47 o 3 2 1 240.25 196.90 15.97 o 4 2 1 406.93 431.97 21.95 o 5 2 1 29.24 19.16 6.64 o 6 2 1 246.82 193.62 11.29 o 7 2 1 786.12 842.83 23.87 o 8 2 1 10.65 1.14 9.58 o 9 2 1 40.00 29.94 11.29 o 10 2 1 5.51 3.99 16.24 o 11 2 1 3.21 11.98 25.60 o 12 2 1 205.74 154.19 44.68 o 13 2 1 3.49 19.77 41.52 o 14 2 1 27.60 57.69 72.86 o -15 3 1 20.50 21.41 93.80 o -14 3 1 91.60 28.47 46.04 o -13 3 1 5.50 -16.48 40.87 o -12 3 1 0.76 -38.30 40.44 o -11 3 1 12.51 5.08 25.32 o -10 3 1 98.72 53.27 26.22 o -9 3 1 135.12 104.42 11.01 o -8 3 1 87.62 93.04 17.96 o -7 3 1 1168.59 1243.62 61.87 o -6 3 1 275.56 287.76 15.97 o -5 3 1 946.29 967.78 53.89 o -4 3 1 1511.30 1513.90 39.92 o -3 3 1 12.22 13.79 3.99 o -2 3 1 4911.36 4951.12 91.81 o -1 3 1 221.06 246.28 13.97 o 0 3 1 2124.20 1969.47 39.92 o 1 3 1 2733.86 2597.55 101.79 o 2 3 1 35.81 31.14 5.99 o 3 3 1 1034.50 939.74 18.18 o 4 3 1 783.40 782.81 23.95 o 5 3 1 1.65 5.99 5.65 o 6 3 1 90.79 93.37 11.98 o 7 3 1 53.72 50.69 9.58 o 8 3 1 90.94 75.84 11.29 o 9 3 1 7.52 3.63 15.97 o 10 3 1 24.79 22.62 16.24 o 11 3 1 110.62 118.19 30.41 o 12 3 1 25.18 75.48 47.90 o 13 3 1 25.27 -32.52 75.84 o 14 3 1 14.06 43.11 73.07 o -14 4 1 15.79 36.06 107.78 o -13 4 1 197.52 175.85 54.39 o -12 4 1 0.36 -8.86 49.61 o -11 4 1 57.15 69.46 28.89 o -10 4 1 17.02 11.98 22.06 o -9 4 1 167.53 170.21 15.97 o -8 4 1 8.41 3.99 13.29 o -7 4 1 1109.64 1128.44 29.54 o -6 4 1 2275.44 2229.61 40.85 o -5 4 1 1840.45 1890.67 33.93 o -4 4 1 1505.89 1489.74 20.54 o -3 4 1 188.18 183.62 8.47 o -2 4 1 149.94 131.85 5.65 o -1 4 1 1863.03 1795.03 71.85 o 0 4 1 1594.86 1484.53 43.91 o 1 4 1 532.35 496.11 29.94 o 2 4 1 90.91 99.95 8.47 o 3 4 1 68.92 57.17 6.64 o 4 4 1 656.24 671.92 16.24 o 5 4 1 1359.59 1256.51 22.89 o 6 4 1 267.13 223.28 23.95 o 7 4 1 789.71 822.84 37.92 o 8 4 1 138.99 99.79 18.18 o 9 4 1 72.67 45.44 19.96 o 10 4 1 29.64 32.20 21.03 o 11 4 1 83.10 61.87 35.93 o 12 4 1 261.05 226.88 50.64 o 13 4 1 0.18 -19.19 51.45 o 14 4 1 39.69 -61.07 89.33 o -14 5 1 258.55 250.53 77.84 o -13 5 1 11.79 -23.57 123.74 o -12 5 1 260.78 268.05 51.45 o -11 5 1 80.97 43.18 30.67 o -10 5 1 835.77 848.30 44.99 o -9 5 1 789.97 744.67 69.85 o -8 5 1 65.70 47.10 13.97 o -7 5 1 853.32 827.18 29.54 o -6 5 1 1289.80 1285.79 32.37 o -5 5 1 217.92 187.35 17.96 o -4 5 1 1143.77 1034.65 31.93 o -3 5 1 53.16 63.01 19.96 o -2 5 1 4759.68 4885.66 61.90 o -1 5 1 3009.36 3080.63 129.73 o 0 5 1 1232.08 1289.61 53.89 o 1 5 1 3936.54 3794.63 177.63 o 2 5 1 53.95 46.74 6.64 o 3 5 1 3014.81 2974.76 43.68 o 4 5 1 1476.34 1481.75 27.80 o 5 5 1 1068.16 1037.02 53.89 o 6 5 1 2216.89 2262.03 57.88 o 7 5 1 213.41 165.68 22.58 o 8 5 1 783.16 884.19 65.86 o 9 5 1 149.63 193.45 53.89 o 10 5 1 156.27 163.82 36.85 o 11 5 1 386.39 442.95 87.82 o 12 5 1 5.76 26.94 41.66 o 13 5 1 46.47 43.91 53.55 o 14 5 1 1.00 54.74 59.93 o -14 6 1 32.27 59.03 121.75 o -13 6 1 363.11 414.97 76.95 o -12 6 1 156.00 134.36 95.80 o -11 6 1 623.47 636.49 50.15 o -10 6 1 2023.17 2000.98 73.07 o -9 6 1 547.09 537.67 33.52 o -8 6 1 786.25 732.01 31.64 o -7 6 1 172.44 142.87 31.93 o -6 6 1 427.98 378.45 22.06 o -5 6 1 1852.18 1888.09 31.75 o -4 6 1 63.66 50.61 8.47 o -3 6 1 3244.75 3392.71 46.51 o -2 6 1 913.31 962.00 19.93 o -1 6 1 2307.59 2331.42 53.89 o 0 6 1 3373.35 3210.40 187.61 o 1 6 1 554.19 562.86 16.94 o 2 6 1 7737.09 8103.20 213.56 o 3 6 1 140.53 111.47 19.96 o 4 6 1 5373.77 5560.21 76.04 o 5 6 1 156.66 134.20 10.71 o 6 6 1 244.27 257.58 29.94 o 7 6 1 2410.54 2482.47 61.90 o 8 6 1 351.95 344.52 29.54 o 9 6 1 1047.77 1125.74 67.86 o 10 6 1 319.15 266.52 36.18 o 11 6 1 375.00 455.64 46.41 o 12 6 1 261.97 211.08 53.89 o 13 6 1 7.00 26.55 56.35 o -13 7 1 1.33 -12.36 56.11 o -12 7 1 196.36 135.93 51.70 o -11 7 1 447.82 405.95 47.73 o -10 7 1 418.23 352.44 49.90 o -9 7 1 2251.71 2507.51 82.37 o -8 7 1 425.81 358.46 29.54 o -7 7 1 2333.41 2489.00 75.84 o -6 7 1 177.86 191.42 27.94 o -5 7 1 493.12 471.71 16.92 o -4 7 1 4053.46 4084.94 68.67 o -3 7 1 3.94 16.96 10.27 o -2 7 1 6289.52 6499.89 167.65 o -1 7 1 375.26 401.25 11.36 o 0 7 1 1860.34 1903.17 115.76 o 1 7 1 5080.90 5215.40 231.52 o 2 7 1 4.63 -2.00 8.47 o 3 7 1 4831.99 4898.75 129.73 o 4 7 1 841.59 820.89 25.83 o 5 7 1 278.48 283.10 16.92 o 6 7 1 793.04 782.17 59.88 o 7 7 1 88.31 130.20 24.94 o 8 7 1 1411.91 1407.10 52.74 o 9 7 1 523.60 423.04 38.03 o 10 7 1 221.53 165.90 39.21 o 11 7 1 236.90 218.29 42.07 o 12 7 1 9.44 55.65 52.27 o 13 7 1 71.94 31.49 63.87 o -13 8 1 322.67 300.99 77.48 o -12 8 1 36.44 3.99 53.55 o -11 8 1 67.16 63.07 53.89 o -10 8 1 360.30 323.54 43.91 o -9 8 1 0.67 -20.40 31.93 o -8 8 1 559.72 627.72 55.88 o -7 8 1 33.08 17.38 22.89 o -6 8 1 1372.68 1489.10 91.81 o -5 8 1 2794.37 2813.45 62.76 o -4 8 1 785.63 693.88 51.89 o -3 8 1 2990.49 3121.44 58.09 o -2 8 1 2.41 10.38 7.75 o -1 8 1 1720.85 1751.97 75.84 o 0 8 1 560.14 509.91 49.90 o 1 8 1 620.03 656.99 41.91 o 2 8 1 2267.30 2407.06 55.45 o 3 8 1 87.60 76.68 13.97 o 4 8 1 1110.93 1139.43 36.04 o 5 8 1 169.83 196.29 27.94 o 6 8 1 36.51 37.26 14.28 o 7 8 1 191.22 174.34 29.54 o 8 8 1 0.50 -7.98 22.58 o 9 8 1 328.44 340.09 57.88 o 10 8 1 181.42 155.95 37.40 o 11 8 1 44.55 -34.16 49.90 o 12 8 1 131.81 141.02 56.53 o -12 9 1 141.87 159.67 71.85 o -11 9 1 79.85 -2.00 50.81 o -10 9 1 125.18 115.76 47.98 o -9 9 1 538.91 559.49 55.88 o -8 9 1 46.23 39.74 77.84 o -7 9 1 849.45 906.07 50.57 o -6 9 1 933.20 920.38 31.31 o -5 9 1 55.34 53.22 17.85 o -4 9 1 1711.24 1887.87 48.76 o -3 9 1 91.38 76.71 41.91 o -2 9 1 3264.84 3531.99 90.26 o -1 9 1 315.83 323.79 31.93 o 0 9 1 561.23 599.14 15.82 o 1 9 1 991.96 1045.82 31.93 o 2 9 1 23.74 27.94 21.95 o 3 9 1 839.65 802.94 43.91 o 4 9 1 205.26 174.98 25.95 o 5 9 1 384.63 444.51 55.88 o 6 9 1 342.38 394.97 45.90 o 7 9 1 1.85 -23.57 23.57 o 8 9 1 79.09 50.00 39.92 o 9 9 1 268.64 212.36 71.85 o 10 9 1 137.67 133.40 41.22 o 11 9 1 224.89 232.01 85.82 o 12 9 1 0.33 -3.99 67.86 o 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