#------------------------------------------------------------------------------ #$Date: 2016-04-02 23:02:54 +0300 (Sat, 02 Apr 2016) $ #$Revision: 180910 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/10/51/2105177.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_2105177_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 90.040 _cell_angle_beta 105.460 _cell_angle_gamma 90.030 _cell_length_a 12.1540 _cell_length_b 12.1620 _cell_length_c 16.0610 _exptl_crystal_F_000 1096.00 _reflns_d_resolution_high 0.7697 _cod_data_source_file hw5021120K_IV_1sup7.hkl _cod_data_source_block 120K_IV_1 #BEGIN Tags that were not found in dictionaries: _shelx_title ' k06086 in P-1' _shelx_refln_list_code 4 _shelx_f_calc_maximum 293.52 _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 5673.15 5439.49 84.12 o 2 0 0 24106.45 24272.64 377.74 o 3 0 0 612.90 736.67 18.52 o 4 0 0 1413.89 1354.70 20.55 o 5 0 0 47816.00 50863.28 784.87 o 6 0 0 1326.08 1284.69 19.84 o 7 0 0 11404.24 11610.62 172.29 o 8 0 0 7084.27 7502.53 127.24 o 9 0 0 755.14 874.01 40.57 o 10 0 0 368.05 413.81 56.44 o 11 0 0 1568.06 1543.19 46.94 o 12 0 0 2724.87 3001.66 153.45 o 13 0 0 1851.91 1941.01 109.35 o 14 0 0 54.87 61.79 36.53 o 15 0 0 391.75 272.70 46.72 o -15 1 0 31.30 46.55 27.96 o -14 1 0 319.40 336.96 140.22 o -13 1 0 421.51 434.82 55.56 o -12 1 0 1913.80 1931.93 60.16 o -11 1 0 4645.81 5109.61 196.66 o -10 1 0 525.28 523.46 27.67 o -9 1 0 842.26 888.68 29.64 o -8 1 0 126.40 108.24 14.03 o -7 1 0 2814.10 2606.32 60.85 o -6 1 0 14822.57 15124.08 498.26 o -5 1 0 1966.53 2175.32 39.68 o -4 1 0 17732.02 17512.20 302.03 o -3 1 0 10280.14 9728.15 135.10 o -2 1 0 1046.60 1114.25 31.75 o 0 1 0 41.19 41.62 2.65 o 2 1 0 988.51 1057.37 14.97 o 3 1 0 10172.73 9682.06 134.26 o 4 1 0 17482.78 17570.86 254.86 o 5 1 0 2109.04 2311.97 51.15 o 6 1 0 14593.80 15110.64 305.13 o 7 1 0 2629.08 2565.18 43.53 o 8 1 0 136.94 128.56 10.42 o 9 1 0 884.21 913.91 24.69 o 10 1 0 573.96 567.63 25.57 o 11 1 0 4882.58 5057.36 119.05 o 12 1 0 1829.76 1782.34 62.75 o 13 1 0 472.32 422.92 34.65 o 14 1 0 307.10 269.35 38.12 o 15 1 0 37.18 129.66 95.24 o -15 2 0 988.85 1006.26 64.38 o -14 2 0 84.15 122.06 29.63 o -13 2 0 625.38 618.70 44.46 o -12 2 0 1392.28 1541.35 62.06 o -11 2 0 46.18 65.15 22.05 o -10 2 0 4120.30 4312.59 101.69 o -9 2 0 1921.71 1952.57 46.05 o -8 2 0 4901.94 5150.63 141.10 o -7 2 0 5844.14 5983.25 136.69 o -6 2 0 534.75 468.19 30.87 o -5 2 0 18682.19 18660.42 272.50 o -4 2 0 1327.56 1284.20 68.79 o -3 2 0 9285.33 8600.04 160.08 o -2 2 0 2939.83 3130.91 67.73 o -1 2 0 1137.74 1043.87 17.80 o 0 2 0 10867.03 10276.71 142.76 o 1 2 0 1062.22 987.07 15.26 o 2 2 0 2832.81 2991.91 41.43 o 3 2 0 9647.38 8876.34 101.90 o 4 2 0 1572.12 1490.28 34.39 o 5 2 0 19190.71 19412.50 286.61 o 6 2 0 599.76 555.63 12.47 o 7 2 0 5992.16 6101.98 104.94 o 8 2 0 4648.11 4909.25 87.31 o 9 2 0 1981.52 2005.32 38.34 o 10 2 0 4245.24 4543.56 94.36 o 11 2 0 54.60 50.91 15.61 o 12 2 0 1439.14 1462.92 94.36 o 13 2 0 603.91 559.27 76.72 o 14 2 0 92.66 94.56 56.44 o 15 2 0 998.41 934.13 57.50 o -14 3 0 623.00 683.78 45.01 o -13 3 0 27.03 6.85 29.64 o -12 3 0 53.49 97.82 23.81 o -11 3 0 3584.41 3522.27 195.78 o -10 3 0 838.46 806.32 30.65 o -9 3 0 5340.77 5554.50 110.27 o -8 3 0 1557.78 1651.55 49.39 o -7 3 0 1086.25 1130.79 27.87 o -6 3 0 1206.28 1007.41 24.85 o -5 3 0 2175.87 2193.83 37.35 o -4 3 0 18990.92 19420.98 400.37 o -3 3 0 9720.32 9541.23 220.47 o -2 3 0 5669.13 5395.22 99.70 o -1 3 0 4669.67 4835.01 107.59 o 0 3 0 0.12 14.79 2.94 o 1 3 0 4613.42 4764.34 72.30 o 2 3 0 5520.59 5218.43 80.09 o 3 3 0 10575.52 10188.40 196.66 o 4 3 0 19519.92 20074.54 377.44 o 5 3 0 1913.00 2015.43 34.14 o 6 3 0 1255.23 1029.24 22.05 o 7 3 0 949.27 1033.95 25.84 o 8 3 0 1529.30 1662.28 69.67 o 9 3 0 5125.43 5332.12 117.26 o 10 3 0 822.52 836.93 41.45 o 11 3 0 3410.43 3357.03 127.87 o 12 3 0 51.13 14.30 25.87 o 13 3 0 23.06 18.52 21.53 o 14 3 0 600.85 602.55 46.17 o -14 4 0 40.54 -0.78 27.55 o -13 4 0 120.69 148.83 31.22 o -12 4 0 293.55 164.90 39.68 o -11 4 0 155.21 124.80 37.04 o -10 4 0 3788.24 3597.12 104.11 o -9 4 0 265.41 238.96 29.10 o -8 4 0 4125.66 4191.05 112.88 o -7 4 0 4651.78 4858.25 92.90 o -6 4 0 700.53 759.35 19.30 o -5 4 0 11483.69 11690.88 278.67 o -4 4 0 1648.41 1852.37 42.80 o -3 4 0 8837.91 9223.47 211.65 o -2 4 0 13845.34 13851.59 305.13 o -1 4 0 2446.95 2520.15 52.91 o 0 4 0 46295.84 46260.38 1601.49 o 1 4 0 2187.72 2185.44 46.46 o 2 4 0 14918.65 14191.98 215.20 o 3 4 0 8279.14 8499.24 127.25 o 4 4 0 1426.86 1675.15 38.80 o 5 4 0 11106.14 11744.33 146.91 o 6 4 0 674.36 769.82 18.05 o 7 4 0 4579.56 4837.34 85.87 o 8 4 0 3916.59 3926.34 71.24 o 9 4 0 263.94 249.52 17.00 o 10 4 0 3652.55 3576.61 95.54 o 11 4 0 157.82 120.43 35.28 o 12 4 0 254.60 133.89 29.62 o 13 4 0 109.04 80.97 38.73 o 14 4 0 42.22 76.17 51.15 o -14 5 0 1109.55 1020.13 112.00 o -13 5 0 84.73 41.95 27.49 o -12 5 0 40.60 -22.65 29.64 o -11 5 0 1883.90 2017.73 97.01 o -10 5 0 693.01 576.69 35.17 o -9 5 0 2085.98 1926.72 57.32 o -8 5 0 86.52 113.69 15.87 o -7 5 0 8.79 3.00 9.70 o -6 5 0 5195.98 5359.13 100.44 o -5 5 0 53.39 28.66 7.18 o -4 5 0 7113.81 7523.91 135.73 o -3 5 0 9322.13 9550.08 287.49 o -2 5 0 10299.68 11295.58 463.87 o -1 5 0 12645.52 12440.77 331.59 o 0 5 0 597.09 473.42 11.46 o 1 5 0 12664.07 12436.97 251.33 o 2 5 0 9813.57 10390.13 179.12 o 3 5 0 9559.41 9746.60 145.76 o 4 5 0 6462.56 6745.97 191.37 o 5 5 0 46.67 31.75 6.24 o 6 5 0 4819.62 5108.22 92.61 o 7 5 0 9.02 15.87 8.73 o 8 5 0 100.69 91.15 37.04 o 9 5 0 1937.66 1913.92 63.64 o 10 5 0 591.09 517.25 35.28 o 11 5 0 1723.11 1812.27 135.81 o 12 5 0 42.16 53.62 24.85 o 13 5 0 79.20 37.24 33.03 o 14 5 0 1033.87 895.99 104.06 o -14 6 0 19.81 -9.92 46.00 o -13 6 0 403.32 447.21 49.21 o -12 6 0 452.01 475.50 39.88 o -11 6 0 177.39 177.76 31.51 o -10 6 0 1845.50 1957.41 88.19 o -9 6 0 189.57 146.09 24.71 o -8 6 0 107.27 109.08 29.10 o -7 6 0 3191.35 3533.29 72.21 o -6 6 0 107.81 143.25 24.69 o -5 6 0 5436.49 5857.69 124.59 o -4 6 0 476.82 422.12 12.29 o -3 6 0 240.69 218.70 12.70 o -2 6 0 9472.90 10069.32 253.10 o -1 6 0 176.75 185.21 7.48 o 0 6 0 16126.16 17319.86 547.65 o 1 6 0 175.65 218.21 9.29 o 2 6 0 9194.46 9755.63 305.13 o 3 6 0 203.27 192.59 9.29 o 4 6 0 429.62 449.45 16.76 o 5 6 0 5191.42 5611.72 123.46 o 6 6 0 116.43 168.17 11.46 o 7 6 0 3186.48 3427.63 74.55 o 8 6 0 92.37 131.68 17.61 o 9 6 0 182.61 172.74 24.69 o 10 6 0 1830.01 1975.12 65.04 o 11 6 0 150.34 169.96 25.36 o 12 6 0 423.63 451.15 37.92 o 13 6 0 367.70 395.70 56.36 o 14 6 0 17.44 40.57 44.09 o -13 7 0 68.62 85.25 36.28 o -12 7 0 192.85 201.62 35.01 o -11 7 0 1000.55 1071.10 54.45 o -10 7 0 232.90 135.90 44.09 o -9 7 0 258.41 303.37 38.80 o -8 7 0 61.09 55.93 16.06 o -7 7 0 447.35 522.39 21.59 o -6 7 0 2888.18 3079.79 67.96 o -5 7 0 69.90 90.81 7.71 o -4 7 0 1021.56 1004.61 34.00 o -3 7 0 674.52 699.05 24.69 o -2 7 0 1134.65 1082.63 35.59 o -1 7 0 1337.34 1386.94 27.45 o 0 7 0 439.79 318.18 12.02 o 1 7 0 1211.33 1198.14 38.12 o 2 7 0 954.69 899.55 38.99 o 3 7 0 684.28 689.35 20.92 o 4 7 0 988.98 1000.62 25.20 o 5 7 0 68.07 97.50 19.40 o 6 7 0 2847.81 3150.07 76.61 o 7 7 0 463.28 426.68 34.19 o 8 7 0 52.33 57.53 16.07 o 9 7 0 259.16 274.04 26.68 o 10 7 0 273.89 168.49 24.30 o 11 7 0 998.86 1096.88 58.20 o 12 7 0 183.04 139.91 59.97 o 13 7 0 62.25 61.14 39.15 o -13 8 0 115.64 85.57 43.67 o -12 8 0 26.50 12.68 29.98 o -11 8 0 23.47 39.55 44.98 o -10 8 0 698.13 830.23 47.45 o -9 8 0 17.93 -28.22 28.22 o -8 8 0 405.96 455.05 37.04 o -7 8 0 13.38 17.25 13.35 o -6 8 0 1068.88 1182.45 51.01 o -5 8 0 4457.01 4836.90 130.22 o -4 8 0 367.55 317.58 26.68 o -3 8 0 890.93 855.79 33.47 o -2 8 0 564.10 589.19 59.97 o -1 8 0 898.82 835.81 25.42 o 0 8 0 2398.24 2567.41 62.62 o 1 8 0 756.43 667.84 29.04 o 2 8 0 482.36 470.83 26.46 o 3 8 0 911.28 851.45 44.98 o 4 8 0 315.71 241.08 16.67 o 5 8 0 4451.48 4677.68 103.29 o 6 8 0 932.60 1039.96 77.61 o 7 8 0 13.49 25.87 30.87 o 8 8 0 404.00 424.52 33.35 o 9 8 0 15.46 57.42 31.75 o 10 8 0 714.24 758.00 54.45 o 11 8 0 22.46 -6.32 25.36 o 12 8 0 25.46 -26.85 44.09 o 13 8 0 99.41 56.44 44.09 o -12 9 0 174.03 131.20 34.75 o -11 9 0 178.03 172.91 39.28 o -10 9 0 38.38 -1.76 28.22 o -9 9 0 313.48 275.15 31.22 o -8 9 0 441.52 342.17 45.86 o -7 9 0 1712.99 1878.93 68.65 o -6 9 0 488.87 430.19 34.65 o -5 9 0 758.90 741.75 46.95 o -4 9 0 12.77 23.37 9.07 o -3 9 0 463.03 427.23 30.97 o -2 9 0 1364.78 1474.21 53.82 o -1 9 0 765.27 810.71 36.16 o 0 9 0 52.15 30.74 13.23 o 1 9 0 735.40 782.96 76.72 o 2 9 0 1299.35 1433.12 64.38 o 3 9 0 421.95 401.82 53.79 o 4 9 0 14.29 9.07 17.64 o 5 9 0 862.71 812.87 49.30 o 6 9 0 512.99 367.33 29.56 o 7 9 0 1594.21 1647.07 165.79 o 8 9 0 435.09 434.54 71.43 o 9 9 0 263.78 265.28 60.85 o 10 9 0 45.46 2.65 30.84 o 11 9 0 156.07 198.45 84.66 o 12 9 0 154.48 165.13 43.27 o -11 10 0 73.04 26.15 30.34 o -10 10 0 56.40 12.35 44.09 o -9 10 0 1.36 -24.69 35.28 o -8 10 0 251.29 164.03 37.04 o -7 10 0 7.50 -3.28 17.33 o -6 10 0 153.08 80.41 28.22 o -5 10 0 265.70 210.58 26.42 o -4 10 0 127.11 105.44 17.35 o -3 10 0 1255.64 1320.23 62.69 o -2 10 0 177.72 174.75 22.05 o -1 10 0 454.24 490.95 28.03 o 0 10 0 6689.78 7247.19 176.47 o 1 10 0 532.22 603.95 33.15 o 2 10 0 171.67 160.33 16.54 o 3 10 0 1189.17 1227.74 58.36 o 4 10 0 128.81 84.77 21.14 o 5 10 0 239.35 192.35 112.00 o 6 10 0 145.76 122.62 62.61 o 7 10 0 8.17 22.93 25.24 o 8 10 0 219.79 131.47 50.27 o 9 10 0 1.20 -26.82 26.82 o 10 10 0 48.42 -0.91 38.16 o 11 10 0 67.68 116.45 46.05 o -10 11 0 11.64 29.98 37.04 o -9 11 0 32.07 10.58 31.75 o -8 11 0 17.49 12.97 33.51 o -7 11 0 74.51 125.23 44.09 o -6 11 0 254.07 204.61 34.39 o -5 11 0 60.39 34.57 16.79 o -4 11 0 14.91 25.57 22.05 o -3 11 0 192.59 172.43 33.67 o -2 11 0 192.92 201.80 34.39 o -1 11 0 452.43 433.48 35.17 o 0 11 0 17.35 -11.22 13.55 o 1 11 0 389.94 327.24 27.70 o 2 11 0 206.43 216.83 53.79 o 3 11 0 192.76 193.63 21.04 o 4 11 0 15.40 4.30 19.56 o 5 11 0 65.98 94.99 25.67 o 6 11 0 232.34 136.26 28.55 o 7 11 0 67.48 68.79 66.14 o 8 11 0 20.68 26.08 33.51 o 9 11 0 34.39 8.21 37.04 o 10 11 0 10.12 -26.30 51.15 o -9 12 0 23.36 4.82 39.47 o -8 12 0 40.72 40.57 54.68 o -7 12 0 90.82 62.44 32.29 o -6 12 0 12.34 13.79 26.68 o -5 12 0 439.62 453.80 41.45 o -4 12 0 220.08 266.08 40.57 o -3 12 0 359.39 315.34 35.28 o -2 12 0 49.98 50.01 21.09 o -1 12 0 288.33 255.11 42.18 o 0 12 0 57.36 87.41 21.86 o 1 12 0 244.54 190.39 30.87 o 2 12 0 44.89 37.39 23.48 o 3 12 0 391.20 318.76 52.91 o 4 12 0 193.49 179.24 35.14 o 5 12 0 412.57 385.95 107.59 o 6 12 0 10.76 23.29 44.98 o 7 12 0 106.29 158.69 42.33 o 8 12 0 40.50 79.76 38.93 o 9 12 0 27.16 36.74 41.59 o -8 13 0 33.83 65.50 43.61 o -7 13 0 64.89 107.59 47.62 o -6 13 0 294.34 190.49 47.62 o -5 13 0 21.03 15.43 29.24 o -4 13 0 35.13 54.68 27.87 o -3 13 0 56.19 32.34 23.66 o -2 13 0 100.06 40.74 33.51 o -1 13 0 168.83 184.83 34.00 o 0 13 0 125.24 144.40 26.62 o 1 13 0 186.81 135.69 41.45 o 2 13 0 87.29 65.99 29.98 o 3 13 0 57.45 54.80 27.79 o 4 13 0 37.40 54.09 31.55 o 5 13 0 24.67 27.21 31.98 o 6 13 0 313.10 273.09 43.29 o 7 13 0 55.05 100.87 41.17 o 8 13 0 40.00 30.19 41.43 o -7 14 0 54.32 56.44 54.68 o -6 14 0 56.26 74.08 51.15 o -5 14 0 113.23 18.01 80.25 o -4 14 0 143.26 88.32 32.23 o -3 14 0 133.37 106.76 26.42 o -2 14 0 61.01 40.47 46.95 o -1 14 0 38.26 26.29 33.40 o 0 14 0 154.10 137.46 38.56 o 1 14 0 34.33 41.89 29.62 o 2 14 0 72.43 57.25 33.08 o 3 14 0 132.45 104.47 32.14 o 4 14 0 168.47 174.53 40.78 o 5 14 0 123.96 128.17 44.17 o 6 14 0 48.25 -13.20 47.77 o 7 14 0 60.03 46.98 76.63 o -4 15 0 119.97 64.37 55.40 o -3 15 0 35.90 -18.17 59.97 o -2 15 0 21.72 18.81 54.64 o -1 15 0 101.47 81.28 42.41 o 0 15 0 33.79 -16.52 36.84 o 1 15 0 112.01 41.74 50.41 o 2 15 0 23.04 81.09 67.02 o 3 15 0 40.45 18.67 39.11 o 4 15 0 117.44 107.21 52.91 o -4 -15 1 256.62 153.95 78.31 o -3 -15 1 127.87 91.06 68.79 o -2 -15 1 663.21 559.02 66.42 o -1 -15 1 196.68 214.29 61.01 o 0 -15 1 105.91 84.77 55.76 o 1 -15 1 101.48 87.58 56.77 o 2 -15 1 18.88 24.34 85.54 o 3 -15 1 155.54 94.91 56.77 o 4 -15 1 41.60 49.39 79.37 o -7 -14 1 267.24 288.30 69.70 o -6 -14 1 243.77 227.44 89.95 o -5 -14 1 374.98 366.58 49.62 o -4 -14 1 344.12 245.99 46.46 o -3 -14 1 496.85 453.67 37.29 o -2 -14 1 36.37 20.44 33.56 o -1 -14 1 387.54 336.51 45.42 o 0 -14 1 52.37 5.90 42.80 o 1 -14 1 120.90 60.02 38.45 o 2 -14 1 311.83 316.57 43.27 o 3 -14 1 100.15 144.18 38.99 o 4 -14 1 269.08 234.13 56.44 o 5 -14 1 120.97 171.08 44.09 o 6 -14 1 76.49 67.02 38.80 o -8 -13 1 97.93 31.12 43.04 o -7 -13 1 771.27 638.71 99.65 o -6 -13 1 189.43 189.55 39.74 o -5 -13 1 227.87 219.10 41.32 o -4 -13 1 989.95 967.64 58.96 o -3 -13 1 273.56 382.96 42.59 o -2 -13 1 1231.62 1257.00 60.40 o -1 -13 1 414.85 473.68 37.80 o 0 -13 1 797.09 835.26 120.82 o 1 -13 1 1305.75 1419.82 77.09 o 2 -13 1 203.87 173.14 39.68 o 3 -13 1 489.66 492.22 40.93 o 4 -13 1 289.42 360.61 40.59 o 5 -13 1 336.74 315.61 72.31 o 6 -13 1 500.49 627.90 75.84 o 7 -13 1 78.32 85.95 35.28 o 8 -13 1 199.72 181.67 42.33 o -10 -12 1 382.87 413.55 119.94 o -9 -12 1 163.03 127.44 42.43 o -8 -12 1 561.72 545.27 49.39 o -7 -12 1 183.25 186.83 56.44 o -6 -12 1 1187.39 1126.63 67.02 o -5 -12 1 1500.18 1660.12 103.15 o -4 -12 1 201.71 174.15 27.49 o -3 -12 1 1426.19 1486.98 68.19 o -2 -12 1 709.41 657.48 69.67 o -1 -12 1 712.95 719.61 46.94 o 0 -12 1 2566.65 2959.94 169.51 o 1 -12 1 747.13 706.11 65.26 o 2 -12 1 3466.46 3778.33 168.64 o 3 -12 1 776.24 783.19 104.94 o 4 -12 1 856.75 962.73 107.06 o 5 -12 1 822.35 914.82 83.78 o 6 -12 1 280.07 303.37 50.41 o 7 -12 1 699.06 640.24 58.20 o 8 -12 1 71.40 35.28 35.28 o 9 -12 1 495.30 391.55 59.97 o -11 -11 1 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