#------------------------------------------------------------------------------ #$Date: 2016-04-03 06:35:56 +0300 (Sun, 03 Apr 2016) $ #$Revision: 181259 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/23/37/2233790.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_2233790_Fobs loop_ _publ_author_name 'Hirotsu, Masakazu' 'Kuwamura, Naoto' 'Kinoshita, Isamu' 'Kojima, Masaaki' 'Yoshikawa, Yuzo' _publ_section_title ; Bis(\m~2~-4,7-dimethyl-4,7-diazadecane-1,10-dithiolato)trinickel(II) bis(perchlorate) ; _journal_coeditor_code FJ2508 _journal_issue 3 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m307 _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 105.033 _cell_angle_gamma 90.000 _cell_length_a 8.0253 _cell_length_b 16.2080 _cell_length_c 12.8070 _exptl_crystal_F_000 876.00 _reflns_d_resolution_high 0.7702 _cod_data_source_file fj2508Isup2.hkl _cod_data_source_block I #BEGIN Tags that were not found in dictionaries: _shelx_title ' mh091217_Ni3 in P 21/c' _shelx_refln_list_code 4 _shelx_f_calc_maximum 231.06 _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 2 0 0 1739.13 1386.48 36.94 o 3 0 0 22.74 78.27 5.36 o 4 0 0 1903.63 2108.32 32.48 o 5 0 0 2253.22 2617.82 46.07 o 6 0 0 1843.83 1890.31 34.88 o 7 0 0 2529.76 2764.52 94.72 o 8 0 0 8.85 7.71 6.56 o 10 0 0 736.09 681.34 49.80 o 2 1 0 2014.21 2167.08 27.07 o 3 1 0 2318.48 2256.12 24.55 o 4 1 0 833.38 755.28 16.84 o 5 1 0 1826.27 1950.24 26.23 o 6 1 0 2089.49 2261.47 23.75 o 7 1 0 58.04 66.21 7.39 o 8 1 0 2.76 4.85 2.43 o 9 1 0 1056.85 1058.01 56.89 o 10 1 0 249.83 275.60 26.80 o 2 2 0 98.85 66.16 2.38 o 3 2 0 3447.93 3260.36 53.18 o 4 2 0 49.86 19.39 2.59 o 5 2 0 673.68 606.09 11.20 o 6 2 0 3484.34 3444.22 48.54 o 7 2 0 891.56 889.44 26.93 o 8 2 0 303.38 284.45 14.42 o 9 2 0 10.89 18.30 15.62 o 10 2 0 81.93 65.12 12.94 o 1 3 0 11257.20 11133.01 96.49 o 2 3 0 493.63 480.40 18.62 o 3 3 0 12392.10 12490.54 84.66 o 4 3 0 426.08 444.52 9.60 o 5 3 0 124.97 132.12 5.99 o 6 3 0 1556.28 1539.54 24.67 o 7 3 0 324.69 316.23 9.89 o 8 3 0 25.36 28.45 4.78 o 9 3 0 817.19 758.05 39.55 o 0 4 0 26091.91 24300.49 417.87 o 1 4 0 2298.50 2083.25 27.80 o 2 4 0 5193.14 5037.11 46.53 o 3 4 0 106.65 117.44 5.59 o 4 4 0 1539.88 1721.83 23.21 o 5 4 0 2806.29 2875.77 28.52 o 6 4 0 446.10 518.05 12.55 o 7 4 0 101.64 99.14 6.50 o 8 4 0 1916.78 1880.08 48.36 o 9 4 0 3720.19 3697.12 182.55 o 1 5 0 1974.85 1931.33 28.69 o 2 5 0 6273.87 6152.71 74.28 o 3 5 0 5026.87 4878.43 50.86 o 4 5 0 656.06 584.34 14.48 o 5 5 0 4.94 11.89 4.73 o 6 5 0 430.13 418.00 9.09 o 7 5 0 1345.18 1377.81 35.47 o 8 5 0 787.40 788.95 34.07 o 9 5 0 467.02 410.96 30.92 o 0 6 0 1781.50 1951.79 51.52 o 1 6 0 520.62 470.77 8.55 o 2 6 0 10593.33 10092.08 106.51 o 3 6 0 1332.63 1252.02 23.54 o 4 6 0 1951.85 2155.25 33.92 o 5 6 0 1572.56 1670.97 28.02 o 6 6 0 10.69 16.10 4.81 o 7 6 0 112.04 127.95 10.79 o 8 6 0 205.51 226.35 15.75 o 9 6 0 1003.03 1087.71 56.19 o 1 7 0 2036.18 1924.99 150.48 o 2 7 0 6259.28 6067.72 60.06 o 3 7 0 6332.76 6183.37 51.87 o 4 7 0 324.99 294.01 8.85 o 5 7 0 762.67 746.78 19.00 o 6 7 0 762.10 655.63 65.80 o 7 7 0 1536.00 1513.03 46.09 o 8 7 0 649.22 535.87 104.69 o 9 7 0 1098.07 1063.81 59.03 o 0 8 0 13334.98 12432.77 135.36 o 1 8 0 14537.91 13816.54 147.30 o 2 8 0 11044.72 11340.64 207.09 o 3 8 0 8703.91 8559.89 95.97 o 4 8 0 5516.79 5393.02 58.13 o 5 8 0 9.19 31.72 6.26 o 6 8 0 146.30 109.29 12.27 o 7 8 0 881.36 802.35 37.41 o 8 8 0 10.68 24.14 22.29 o 9 8 0 139.78 107.14 15.68 o 1 9 0 143.78 64.75 10.90 o 2 9 0 1444.98 1317.72 24.90 o 3 9 0 583.55 516.54 10.50 o 4 9 0 217.66 192.53 6.76 o 5 9 0 1527.08 1507.57 23.91 o 6 9 0 576.57 526.97 23.13 o 7 9 0 743.61 750.29 27.07 o 8 9 0 257.09 248.94 22.55 o 9 9 0 2.07 4.17 6.12 o 0 10 0 187.55 192.70 9.34 o 1 10 0 599.08 553.92 10.74 o 2 10 0 422.89 368.86 12.08 o 3 10 0 2506.83 2558.79 45.74 o 4 10 0 4319.97 4395.83 73.85 o 5 10 0 33.95 47.69 2.30 o 6 10 0 47.94 59.72 10.25 o 7 10 0 732.41 737.47 37.74 o 8 10 0 852.82 722.81 38.95 o 1 11 0 1203.98 1145.28 15.23 o 2 11 0 7153.77 7169.25 95.12 o 3 11 0 1258.56 1372.45 26.91 o 4 11 0 1009.37 899.47 19.16 o 5 11 0 13.74 13.12 5.84 o 6 11 0 620.60 571.27 26.73 o 7 11 0 585.61 497.95 111.60 o 8 11 0 239.68 196.65 23.82 o 0 12 0 5912.95 5696.46 75.72 o 1 12 0 3290.05 3291.68 24.59 o 2 12 0 22.28 10.91 3.97 o 3 12 0 202.59 162.32 7.82 o 4 12 0 128.44 116.03 6.26 o 5 12 0 756.25 717.29 23.81 o 6 12 0 5.09 20.17 7.46 o 7 12 0 281.75 283.72 38.20 o 8 12 0 805.62 764.53 65.02 o 1 13 0 17.43 16.43 2.00 o 2 13 0 474.32 428.41 12.98 o 3 13 0 25.54 33.29 10.81 o 4 13 0 2225.42 2326.40 64.13 o 5 13 0 3750.44 3854.47 77.95 o 6 13 0 245.10 251.64 21.39 o 7 13 0 73.09 63.69 17.30 o 0 14 0 131.28 98.33 6.75 o 1 14 0 725.22 746.17 12.52 o 2 14 0 2577.28 2772.07 55.47 o 3 14 0 481.08 466.53 17.18 o 4 14 0 960.12 866.45 21.90 o 5 14 0 1125.39 1110.08 32.93 o 6 14 0 17.14 19.47 6.98 o 7 14 0 122.39 121.94 13.95 o 1 15 0 327.86 324.26 8.43 o 2 15 0 739.65 652.18 22.28 o 3 15 0 850.90 782.23 18.18 o 4 15 0 244.55 212.38 11.49 o 5 15 0 121.56 101.23 14.48 o 6 15 0 93.24 109.00 12.74 o 7 15 0 103.29 116.04 21.94 o 0 16 0 5459.54 5404.40 78.62 o 1 16 0 6345.25 6620.72 65.89 o 2 16 0 2442.86 2626.50 58.14 o 3 16 0 645.28 691.64 23.06 o 4 16 0 427.23 411.47 22.53 o 5 16 0 322.70 323.37 18.95 o 6 16 0 691.54 710.06 34.98 o 1 17 0 302.77 266.13 8.76 o 2 17 0 3.90 6.64 4.05 o 3 17 0 232.72 225.76 13.93 o 4 17 0 781.51 950.52 55.30 o 5 17 0 395.30 467.84 31.72 o 0 18 0 2922.36 3062.95 83.84 o 1 18 0 599.65 605.01 19.08 o 2 18 0 136.75 171.09 13.01 o 3 18 0 59.60 97.69 15.20 o 4 18 0 28.31 11.64 8.05 o 5 18 0 51.45 66.00 14.37 o 1 19 0 119.01 156.57 15.96 o 2 19 0 566.33 636.30 24.59 o 3 19 0 353.30 279.23 42.08 o 4 19 0 70.59 35.13 7.44 o 0 20 0 1.59 23.32 13.95 o 1 20 0 83.84 70.29 13.48 o 2 20 0 259.07 205.68 18.22 o 3 20 0 225.30 213.79 16.12 o -10 1 1 407.07 417.74 33.41 o -9 1 1 95.27 80.79 9.94 o -8 1 1 8.51 3.89 1.91 o -7 1 1 378.32 392.15 13.94 o -6 1 1 2313.98 2171.31 26.92 o -5 1 1 3.32 5.90 3.13 o -4 1 1 2819.90 2872.96 38.55 o -3 1 1 682.43 743.99 15.88 o -2 1 1 18912.02 19129.64 163.86 o 2 1 1 458.32 430.97 8.46 o 3 1 1 981.45 1003.70 20.47 o 4 1 1 7324.67 7072.79 79.26 o 5 1 1 12930.10 13151.00 112.62 o 6 1 1 4065.79 4056.26 55.73 o 7 1 1 2012.26 2056.43 35.87 o 8 1 1 1065.41 981.13 29.41 o 9 1 1 11.90 13.38 6.16 o -10 2 1 777.23 757.62 37.80 o -9 2 1 26.91 29.94 11.44 o -8 2 1 49.83 72.07 8.36 o -7 2 1 328.50 325.12 11.32 o -6 2 1 13.10 26.48 4.54 o -5 2 1 1734.86 1765.85 20.97 o -4 2 1 915.66 1105.80 19.93 o -3 2 1 6643.23 7600.85 70.45 o -2 2 1 28558.86 27442.49 233.59 o 1 2 1 3555.19 3356.23 23.00 o 2 2 1 9111.71 8907.67 79.26 o 3 2 1 2821.72 2861.05 30.42 o 4 2 1 381.02 273.89 7.08 o 5 2 1 955.39 1013.53 21.74 o 6 2 1 4.73 12.29 3.15 o 7 2 1 3030.38 2901.38 46.21 o 8 2 1 1486.88 1538.98 41.42 o 9 2 1 2226.08 2204.84 90.74 o -10 3 1 755.06 840.92 40.30 o -9 3 1 442.53 429.21 29.12 o -8 3 1 2549.83 2657.70 65.09 o -7 3 1 2050.66 2209.33 43.18 o -6 3 1 2236.33 2599.61 31.78 o -5 3 1 8189.96 8694.88 60.60 o -4 3 1 464.57 426.39 9.19 o -3 3 1 4426.89 4837.64 73.66 o -2 3 1 2398.34 2412.84 52.70 o -1 3 1 39167.74 36370.15 317.35 o 0 3 1 88.98 121.93 2.94 o 1 3 1 3534.32 3353.05 34.75 o 2 3 1 2471.29 2472.02 28.66 o 3 3 1 139.12 97.32 3.72 o 4 3 1 694.69 995.78 22.48 o 5 3 1 143.40 145.47 6.53 o 6 3 1 412.61 364.44 9.43 o 7 3 1 1.21 12.08 3.79 o 8 3 1 341.55 248.45 10.42 o 9 3 1 217.69 237.63 25.59 o -10 4 1 37.28 10.67 11.47 o -9 4 1 45.90 52.58 16.14 o -8 4 1 329.62 365.89 19.25 o -7 4 1 2.32 10.31 3.40 o -6 4 1 275.70 299.34 14.32 o -5 4 1 5.07 16.73 3.62 o -4 4 1 19.86 80.96 4.94 o -3 4 1 473.48 488.52 11.29 o -2 4 1 366.67 360.66 11.18 o -1 4 1 463.47 339.30 6.75 o 0 4 1 2492.38 2401.55 19.28 o 1 4 1 150.20 179.30 4.62 o 2 4 1 5665.85 5806.44 47.90 o 3 4 1 3884.70 4385.12 46.17 o 4 4 1 6133.18 6736.16 77.16 o 5 4 1 229.07 220.45 6.82 o 6 4 1 698.58 635.65 13.14 o 7 4 1 1459.67 1414.63 26.58 o 8 4 1 52.39 60.12 5.79 o 9 4 1 248.52 221.39 22.67 o -9 5 1 997.72 1009.97 62.12 o -8 5 1 1724.13 1828.56 61.13 o -7 5 1 1401.47 1300.02 34.02 o -6 5 1 212.04 161.66 12.18 o -5 5 1 4275.33 3970.26 55.00 o -4 5 1 11987.67 11771.26 128.68 o -3 5 1 2231.21 2012.90 30.22 o -2 5 1 6124.76 5819.91 68.75 o -1 5 1 5108.74 4539.35 53.78 o 0 5 1 5086.06 4921.48 52.63 o 1 5 1 5556.70 5525.30 103.43 o 2 5 1 973.59 1028.83 18.14 o 3 5 1 6532.48 6399.16 69.20 o 4 5 1 3.82 22.86 3.03 o 5 5 1 645.49 635.88 12.64 o 6 5 1 1.73 11.01 4.41 o 7 5 1 14.68 42.08 5.23 o 8 5 1 213.76 238.89 11.23 o 9 5 1 556.09 601.71 27.02 o -9 6 1 428.29 497.06 22.45 o -8 6 1 888.82 985.21 31.19 o -7 6 1 66.04 76.95 9.40 o -6 6 1 368.13 359.29 15.13 o -5 6 1 533.58 455.98 12.83 o -4 6 1 294.21 230.90 6.67 o -3 6 1 12546.25 13333.44 116.24 o -2 6 1 36530.59 36005.41 380.47 o -1 6 1 12127.11 12232.31 81.06 o 0 6 1 604.03 636.50 11.16 o 1 6 1 21.88 13.58 3.85 o 2 6 1 1893.44 1687.22 19.17 o 3 6 1 2179.05 1988.46 24.66 o 4 6 1 420.42 378.70 9.51 o 5 6 1 194.21 153.21 7.44 o 6 6 1 297.06 378.29 28.35 o 7 6 1 5888.11 6505.53 165.15 o 8 6 1 2482.63 2589.36 106.95 o 9 6 1 481.26 499.10 26.21 o -9 7 1 85.58 66.98 11.90 o -8 7 1 533.85 578.73 38.12 o -7 7 1 331.83 295.17 22.09 o -6 7 1 77.76 98.03 11.39 o -5 7 1 238.06 288.39 9.66 o -4 7 1 1189.91 1323.98 19.28 o -3 7 1 1026.24 954.80 14.07 o -2 7 1 942.02 1136.82 25.31 o -1 7 1 132.20 189.36 4.85 o 0 7 1 3170.29 3165.77 37.88 o 1 7 1 6450.12 6452.67 45.38 o 2 7 1 13761.28 14140.81 159.07 o 3 7 1 13828.80 14125.38 236.80 o 4 7 1 3319.88 3236.02 28.99 o 5 7 1 600.61 648.66 16.83 o 6 7 1 369.82 405.83 20.66 o 7 7 1 2570.77 2660.49 73.52 o 8 7 1 2115.71 2143.51 100.22 o 9 7 1 460.35 340.88 36.97 o -9 8 1 592.82 524.24 47.49 o -8 8 1 197.36 163.18 36.62 o -7 8 1 149.04 155.70 15.31 o -6 8 1 1.44 10.98 3.97 o -5 8 1 5.77 16.40 6.61 o -4 8 1 347.26 323.94 7.40 o -3 8 1 210.15 174.08 7.36 o -2 8 1 943.60 906.06 16.51 o 0 8 1 418.67 418.50 8.51 o 1 8 1 402.10 361.52 14.89 o 2 8 1 125.75 85.34 6.39 o 3 8 1 472.75 434.45 10.50 o 4 8 1 78.92 82.92 5.49 o 5 8 1 2157.15 2282.14 63.28 o 6 8 1 287.55 261.85 20.15 o 7 8 1 370.74 389.89 27.61 o 8 8 1 136.56 139.05 21.87 o 9 8 1 183.95 139.64 18.09 o -9 9 1 326.97 310.01 32.82 o -8 9 1 95.49 90.29 13.47 o -7 9 1 268.07 193.18 16.39 o -6 9 1 597.68 648.58 28.57 o -5 9 1 19.34 17.67 1.98 o -4 9 1 1333.11 1368.28 14.63 o -3 9 1 834.40 774.88 11.34 o -2 9 1 286.72 250.41 8.44 o -1 9 1 1099.19 1121.84 17.57 o 0 9 1 3742.41 3774.18 37.13 o 1 9 1 15282.15 14514.27 153.54 o 2 9 1 11045.23 10773.96 235.22 o 3 9 1 287.23 340.84 8.39 o 4 9 1 1491.29 1557.99 30.43 o 5 9 1 319.54 286.44 11.28 o 6 9 1 1108.20 1015.85 27.55 o 7 9 1 3484.65 3584.88 123.03 o 8 9 1 2774.42 2941.35 106.34 o -8 10 1 40.03 27.44 10.13 o -7 10 1 9.13 15.25 2.93 o -6 10 1 225.68 195.78 12.11 o -5 10 1 549.39 504.26 11.16 o -4 10 1 1212.25 1088.88 14.86 o -3 10 1 4138.02 4124.38 57.76 o -2 10 1 16047.90 16666.06 308.16 o -1 10 1 7066.12 6909.62 57.30 o 0 10 1 1825.63 1595.50 18.13 o 1 10 1 880.40 873.91 15.38 o 2 10 1 859.84 953.16 18.45 o 3 10 1 2.68 10.77 2.97 o 4 10 1 14.00 20.49 3.56 o 5 10 1 177.10 178.15 13.08 o 6 10 1 38.24 43.43 10.79 o 7 10 1 1682.52 1972.80 86.09 o 8 10 1 1393.86 1314.93 93.85 o -8 11 1 777.39 773.12 54.43 o -7 11 1 832.98 726.87 85.51 o -6 11 1 1530.38 1408.44 26.21 o -5 11 1 1994.25 2023.13 29.75 o -4 11 1 2273.31 2359.96 40.43 o -3 11 1 4170.58 4089.18 54.01 o -2 11 1 276.05 213.14 9.18 o -1 11 1 6.54 4.34 1.95 o 0 11 1 114.43 94.35 4.24 o 1 11 1 640.67 623.05 9.13 o 2 11 1 74.10 81.12 6.74 o 3 11 1 7.39 7.43 4.69 o 4 11 1 410.84 457.79 13.50 o 5 11 1 83.59 105.00 13.45 o 6 11 1 271.38 219.86 18.71 o 7 11 1 0.97 4.47 3.61 o 8 11 1 613.55 559.48 57.71 o -8 12 1 1299.14 1386.15 73.79 o -7 12 1 71.12 63.95 10.56 o -6 12 1 663.71 669.02 23.30 o -5 12 1 212.59 194.97 16.11 o -4 12 1 256.61 200.76 9.00 o -3 12 1 588.31 577.15 13.02 o -2 12 1 1651.78 1587.59 27.00 o -1 12 1 466.32 492.23 8.12 o 0 12 1 1900.64 1955.21 18.95 o 1 12 1 2039.12 1977.96 17.49 o 2 12 1 227.45 194.14 8.74 o 3 12 1 201.82 184.27 10.71 o 4 12 1 413.74 415.28 10.96 o 5 12 1 823.34 848.81 29.26 o 6 12 1 1.60 2.94 5.90 o 7 12 1 260.29 225.05 15.49 o 8 12 1 0.16 0.00 6.60 o -8 13 1 540.71 549.22 56.61 o -7 13 1 65.84 29.91 11.87 o -6 13 1 185.75 243.55 15.37 o -5 13 1 2600.74 2721.92 59.77 o -4 13 1 6789.46 7087.15 95.51 o -3 13 1 1574.33 1435.85 81.30 o -2 13 1 380.12 348.84 12.56 o -1 13 1 13.10 16.74 2.53 o 0 13 1 43.77 38.26 3.09 o 1 13 1 925.53 937.83 13.98 o 2 13 1 1012.46 1035.45 22.28 o 3 13 1 3459.67 3542.93 51.62 o 4 13 1 510.95 489.28 25.39 o 5 13 1 86.76 66.55 8.53 o 6 13 1 5.56 1.98 7.40 o 7 13 1 42.51 39.37 9.94 o -7 14 1 29.80 20.19 8.36 o -6 14 1 162.90 225.53 21.77 o -5 14 1 1446.12 1417.07 52.87 o -4 14 1 1498.90 1297.82 29.76 o -3 14 1 373.28 349.89 16.17 o -2 14 1 2222.41 2445.76 60.80 o -1 14 1 4874.56 5078.01 52.19 o 0 14 1 6248.38 6343.93 58.24 o 1 14 1 1887.50 1848.09 20.78 o 2 14 1 2.69 4.31 2.81 o 3 14 1 533.31 390.37 12.92 o 4 14 1 88.77 50.87 6.06 o 5 14 1 1.43 2.73 10.51 o 6 14 1 1.82 2.13 6.03 o 7 14 1 153.48 97.26 18.96 o -7 15 1 2.14 2.21 6.42 o -6 15 1 176.33 169.84 20.76 o -5 15 1 145.71 138.78 12.39 o -4 15 1 86.84 54.39 6.78 o -3 15 1 323.46 224.00 15.28 o -2 15 1 92.90 75.68 10.41 o -1 15 1 1749.49 1839.77 24.56 o 0 15 1 2005.60 1980.87 24.19 o 1 15 1 188.65 129.76 6.36 o 2 15 1 2358.97 2280.42 41.89 o 3 15 1 1906.67 2085.53 48.25 o 4 15 1 2251.07 2239.90 65.81 o 5 15 1 1625.55 1576.34 71.23 o 6 15 1 2004.99 1950.80 75.55 o -6 16 1 0.84 9.00 6.44 o -5 16 1 0.06 4.58 8.39 o -4 16 1 409.67 376.44 19.17 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