#------------------------------------------------------------------------------ #$Date: 2011-09-16 18:46:08 +0300 (Fri, 16 Sep 2011) $ #$Revision: 26025 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/2013252.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_2013252_Fobs loop_ _publ_author_name 'Fonari, Marina S.' 'Simonov, Yurii A.' 'Chumakov, Yurii M.' 'Bocelli, Gabriele' 'Ganin, Eduard V.' 'Gelmboldt, Vladimir O.' _publ_section_title ; The monoclinic polymorph of rac-5,7,7,12,12,14-hexamethyl-1,4,8,11-tetraazoniacyclotetradecane bis(hexafluorogermanate) tetrahydrate ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m168 _journal_page_last m170 _journal_volume 59 _journal_year 2003 _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 96.280 _cell_angle_gamma 90.000 _cell_length_a 9.5650 _cell_length_b 16.5220 _cell_length_c 9.0210 _exptl_crystal_F_000 752.00 _reflns_d_resolution_high 0.7106 _[local]_cod_data_source_file dn1019Isup2.hkl _[local]_cod_data_source_block I #BEGIN Tags that were not found in dictionaries: _shelx_title ' h in P2(1)/c' _shelx_refln_list_code 4 _shelx_f_calc_maximum 179.15 _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 20393.39 17238.37 186.37 o 3 0 0 19017.22 16340.35 222.47 o 4 0 0 2794.71 2760.93 28.72 o 5 0 0 10788.78 10082.02 62.56 o 6 0 0 9029.33 8873.39 66.58 o 7 0 0 264.39 244.77 13.59 o 8 0 0 719.85 769.34 25.06 o 9 0 0 797.93 741.06 27.40 o 10 0 0 691.74 753.50 30.13 o 11 0 0 989.37 1035.49 40.11 o 12 0 0 84.32 74.31 20.07 o 13 0 0 197.71 212.45 24.69 o 2 1 0 4106.19 4148.13 24.55 o 3 1 0 1025.38 909.42 14.57 o 4 1 0 8423.21 8063.51 49.02 o 5 1 0 7.74 -0.74 6.92 o 6 1 0 949.50 914.02 22.28 o 7 1 0 1802.69 1779.68 33.57 o 8 1 0 578.29 577.80 22.09 o 9 1 0 645.37 667.72 26.23 o 10 1 0 395.84 393.87 23.01 o 11 1 0 182.25 156.38 17.81 o 12 1 0 667.36 726.33 36.61 o 13 1 0 53.78 50.90 20.54 o 1 2 0 2459.91 2460.18 16.11 o 2 2 0 4238.70 4278.91 26.36 o 3 2 0 2.01 6.09 5.43 o 4 2 0 542.97 506.98 13.25 o 5 2 0 272.53 294.31 11.63 o 6 2 0 3.60 0.60 7.90 o 7 2 0 398.14 366.52 16.27 o 8 2 0 24.00 18.47 10.17 o 9 2 0 18.13 24.88 10.61 o 10 2 0 88.84 89.24 13.76 o 11 2 0 34.56 52.05 15.07 o 12 2 0 0.10 -19.68 19.68 o 13 2 0 13.58 19.26 20.20 o 1 3 0 4545.37 5112.16 26.63 o 2 3 0 3067.71 3201.28 24.57 o 3 3 0 461.18 506.92 11.90 o 4 3 0 2868.56 2814.85 30.63 o 5 3 0 1405.20 1398.28 24.60 o 6 3 0 4705.44 4644.59 49.74 o 7 3 0 29.30 22.41 9.21 o 8 3 0 501.80 505.40 21.56 o 9 3 0 867.82 877.20 30.28 o 10 3 0 25.87 23.06 13.08 o 11 3 0 315.13 337.53 24.88 o 12 3 0 903.01 935.82 43.03 o 13 3 0 13.27 1.38 22.41 o 0 4 0 21129.13 20933.54 220.54 o 1 4 0 12017.32 12264.38 174.17 o 2 4 0 2784.88 2697.81 24.43 o 3 4 0 43.58 52.21 5.24 o 4 4 0 40.06 55.89 6.23 o 5 4 0 6566.33 6604.01 53.85 o 6 4 0 3552.10 3519.29 44.87 o 7 4 0 575.21 577.95 20.73 o 8 4 0 627.73 655.69 24.18 o 9 4 0 2.42 3.90 11.36 o 10 4 0 553.79 558.48 27.75 o 11 4 0 775.55 818.93 36.72 o 12 4 0 3.25 24.76 18.47 o 13 4 0 485.81 494.66 35.69 o 1 5 0 2350.47 2413.47 23.24 o 2 5 0 15.72 16.93 5.39 o 3 5 0 8995.41 9675.09 54.58 o 4 5 0 37.13 60.44 6.37 o 5 5 0 6.53 8.84 6.95 o 6 5 0 963.40 928.88 23.75 o 7 5 0 760.26 745.65 23.85 o 8 5 0 29.20 24.69 10.84 o 9 5 0 769.98 798.10 29.50 o 10 5 0 586.05 595.07 28.48 o 11 5 0 29.36 15.00 18.23 o 12 5 0 497.83 512.66 33.38 o 13 5 0 22.28 30.67 19.82 o 0 6 0 2330.93 2544.13 25.49 o 1 6 0 165.88 177.14 7.92 o 2 6 0 652.55 678.33 14.80 o 3 6 0 836.98 938.59 18.62 o 4 6 0 1187.51 1197.01 22.91 o 5 6 0 636.02 611.89 18.40 o 6 6 0 630.44 549.22 19.13 o 7 6 0 0.93 13.87 10.42 o 8 6 0 32.49 38.71 12.48 o 9 6 0 95.63 84.48 12.66 o 10 6 0 0.36 11.15 15.65 o 11 6 0 23.54 23.79 18.70 o 12 6 0 16.83 -0.74 20.27 o 1 7 0 4473.91 4434.54 37.01 o 2 7 0 44.72 38.40 5.25 o 3 7 0 10.24 3.31 6.85 o 4 7 0 1373.05 1271.14 24.79 o 5 7 0 293.78 271.47 13.54 o 6 7 0 975.84 989.61 26.38 o 7 7 0 1007.65 1050.11 29.27 o 8 7 0 360.48 329.12 19.13 o 9 7 0 499.18 531.84 25.89 o 10 7 0 929.51 992.35 37.74 o 11 7 0 840.57 875.80 39.26 o 12 7 0 1026.88 1064.89 47.10 o 0 8 0 13354.20 13914.05 69.71 o 1 8 0 1389.40 1280.69 22.08 o 2 8 0 1447.94 1393.68 23.87 o 3 8 0 3877.33 4057.52 42.41 o 4 8 0 1871.45 1819.37 31.10 o 5 8 0 6801.70 6868.13 64.57 o 6 8 0 4557.97 4828.38 59.20 o 7 8 0 649.79 649.29 24.77 o 8 8 0 2309.20 2357.44 49.01 o 9 8 0 52.43 62.33 13.78 o 10 8 0 358.04 315.00 24.06 o 11 8 0 695.31 742.32 37.92 o 12 8 0 0.11 15.74 21.55 o 1 9 0 7095.41 7241.12 54.96 o 2 9 0 229.83 212.93 11.02 o 3 9 0 71.55 74.80 7.98 o 4 9 0 6274.83 6485.47 60.90 o 5 9 0 629.55 639.05 21.48 o 6 9 0 1179.70 1130.23 30.45 o 7 9 0 1383.83 1402.30 36.45 o 8 9 0 57.67 42.93 13.18 o 9 9 0 121.24 109.10 15.36 o 10 9 0 400.98 400.37 26.60 o 11 9 0 31.75 24.39 22.43 o 12 9 0 5.55 16.23 21.71 o 0 10 0 4159.57 4805.55 47.38 o 1 10 0 1182.19 1270.43 25.20 o 2 10 0 735.05 772.62 20.50 o 3 10 0 1048.19 1124.94 25.75 o 4 10 0 2626.47 2661.03 41.54 o 5 10 0 596.74 600.41 22.09 o 6 10 0 1423.53 1333.04 34.23 o 7 10 0 15.29 18.24 14.46 o 8 10 0 19.10 18.63 14.60 o 9 10 0 2.97 3.73 14.60 o 10 10 0 34.97 37.41 18.09 o 11 10 0 11.00 9.38 18.42 o 12 10 0 0.25 8.58 21.36 o 1 11 0 2980.29 3242.65 42.48 o 2 11 0 1612.55 1631.98 31.40 o 3 11 0 830.14 814.86 23.55 o 4 11 0 4924.16 5337.21 61.10 o 5 11 0 906.61 942.80 28.16 o 6 11 0 3367.21 3317.68 55.53 o 7 11 0 1353.01 1378.48 38.79 o 8 11 0 10.07 -13.25 15.25 o 9 11 0 1104.76 1132.34 41.16 o 10 11 0 242.77 221.79 23.24 o 11 11 0 23.58 2.87 20.24 o 0 12 0 4210.99 4408.29 52.78 o 1 12 0 607.52 601.66 20.29 o 2 12 0 1544.86 1527.42 32.10 o 3 12 0 468.42 460.40 19.13 o 4 12 0 219.80 209.79 14.50 o 5 12 0 5198.21 5435.95 68.94 o 6 12 0 1145.54 1177.69 35.19 o 7 12 0 261.19 195.76 18.05 o 8 12 0 1638.29 1719.43 48.30 o 9 12 0 360.61 378.55 26.65 o 10 12 0 780.53 811.95 40.36 o 11 12 0 715.19 816.19 43.74 o 1 13 0 787.36 811.53 24.88 o 2 13 0 702.46 722.88 24.14 o 3 13 0 33.34 33.46 11.28 o 4 13 0 476.85 486.71 21.88 o 5 13 0 981.25 989.31 31.74 o 6 13 0 53.81 23.01 15.67 o 7 13 0 468.42 415.94 24.54 o 8 13 0 140.94 109.94 17.07 o 9 13 0 275.18 278.08 24.22 o 10 13 0 137.68 146.19 24.29 o 11 13 0 8.16 23.83 21.88 o 0 14 0 1110.10 1094.78 30.69 o 1 14 0 230.80 204.33 14.64 o 2 14 0 125.88 96.64 11.87 o 3 14 0 11.79 -4.01 12.54 o 4 14 0 0.77 -0.09 12.38 o 5 14 0 225.41 203.06 17.42 o 6 14 0 64.26 50.84 14.41 o 7 14 0 28.97 35.61 14.43 o 8 14 0 105.40 101.18 18.19 o 9 14 0 21.79 10.59 21.17 o 10 14 0 73.14 55.45 21.26 o 1 15 0 182.28 185.58 15.13 o 2 15 0 28.10 17.75 13.20 o 3 15 0 252.14 268.51 18.35 o 4 15 0 1011.96 1029.51 34.33 o 5 15 0 22.20 23.34 15.77 o 6 15 0 926.83 891.29 35.69 o 7 15 0 1034.66 1035.86 40.07 o 8 15 0 234.37 219.11 22.90 o 9 15 0 598.16 584.12 36.19 o 10 15 0 197.46 211.98 26.81 o 0 16 0 1175.20 1174.68 35.11 o 1 16 0 190.76 184.44 16.37 o 2 16 0 47.33 55.38 13.66 o 3 16 0 553.40 543.47 26.17 o 4 16 0 71.38 59.11 15.09 o 5 16 0 1362.55 1393.96 43.00 o 6 16 0 415.50 434.62 26.97 o 7 16 0 376.03 332.38 25.94 o 8 16 0 313.29 267.83 26.20 o 9 16 0 26.43 23.85 19.91 o 1 17 0 468.13 479.88 25.19 o 2 17 0 535.30 546.45 27.40 o 3 17 0 49.83 45.54 16.13 o 4 17 0 330.52 329.11 23.26 o 5 17 0 119.02 93.53 16.95 o 6 17 0 62.27 74.76 17.86 o 7 17 0 250.56 213.09 23.90 o 8 17 0 14.05 -13.74 21.74 o 9 17 0 44.47 71.91 22.46 o 0 18 0 62.12 58.60 16.23 o 1 18 0 53.43 50.27 15.99 o 2 18 0 341.79 333.85 23.45 o 3 18 0 95.67 90.63 15.48 o 4 18 0 58.71 47.24 17.14 o 5 18 0 194.78 184.98 21.12 o 6 18 0 52.24 53.21 19.01 o 7 18 0 101.14 82.57 22.32 o 8 18 0 138.45 120.74 23.25 o 1 19 0 2679.89 2854.29 64.85 o 2 19 0 1274.36 1351.23 45.62 o 3 19 0 297.01 278.49 24.01 o 4 19 0 1612.29 1673.01 53.20 o 5 19 0 719.51 750.18 39.33 o 6 19 0 408.05 396.20 30.79 o 7 19 0 736.21 729.20 42.71 o 0 20 0 989.78 995.71 41.88 o 1 20 0 324.89 303.57 27.88 o 2 20 0 264.78 260.62 24.88 o 3 20 0 547.77 609.09 34.78 o 4 20 0 13.86 26.70 18.56 o 5 20 0 1009.85 979.36 45.68 o 6 20 0 161.33 157.50 24.34 o 1 21 0 37.16 45.33 20.87 o 2 21 0 29.20 19.00 20.61 o 3 21 0 3.20 -4.39 19.77 o 4 21 0 62.94 34.49 23.79 o 5 21 0 41.03 29.05 22.69 o 0 22 0 143.60 152.93 23.50 o 1 22 0 0.43 16.35 20.27 o 2 22 0 123.08 98.61 24.25 o 3 22 0 77.22 54.33 22.69 o 4 22 0 82.50 65.55 23.79 o 1 23 0 883.03 830.44 46.21 o -13 1 1 2.48 -2.12 20.10 o -12 1 1 782.21 877.47 40.03 o -11 1 1 285.28 266.49 21.99 o -10 1 1 1.08 3.38 11.92 o -9 1 1 39.98 50.07 12.22 o -8 1 1 1671.51 1718.03 36.90 o -7 1 1 589.19 515.36 18.71 o -6 1 1 8095.29 7930.34 62.38 o -5 1 1 699.73 625.23 16.20 o -4 1 1 393.63 315.06 10.29 o -3 1 1 158.49 130.12 6.24 o -2 1 1 2710.06 2829.81 21.06 o -1 1 1 4225.81 4801.17 82.52 o 1 1 1 3825.89 4105.83 21.57 o 2 1 1 9473.46 8505.30 142.89 o 3 1 1 231.05 244.07 8.60 o 4 1 1 14197.18 13504.50 65.89 o 5 1 1 6623.34 6167.98 50.87 o 6 1 1 3528.25 3660.57 44.53 o 7 1 1 3644.46 3845.89 50.45 o 8 1 1 13.86 12.97 11.68 o 9 1 1 208.63 238.83 17.44 o 10 1 1 985.21 1001.36 35.90 o 11 1 1 4.73 9.10 17.19 o 12 1 1 457.39 485.74 31.63 o 13 1 1 109.47 113.42 21.47 o -13 2 1 491.03 553.28 36.43 o -12 2 1 158.78 119.78 19.31 o -11 2 1 1144.78 1187.88 42.55 o -10 2 1 1763.07 1896.73 47.70 o -9 2 1 1.99 -1.77 12.05 o -8 2 1 4999.88 5105.63 64.05 o -7 2 1 3303.43 3193.15 44.88 o -6 2 1 1174.01 1046.45 23.43 o -5 2 1 3261.53 2900.99 34.34 o -4 2 1 4043.40 4027.48 35.42 o -3 2 1 410.50 389.32 10.13 o -2 2 1 32094.66 32003.90 284.72 o -1 2 1 6272.67 6067.20 102.08 o 0 2 1 19749.99 20697.75 400.23 o 1 2 1 17651.73 16685.07 179.07 o 2 2 1 2242.71 2333.85 21.14 o 3 2 1 8077.40 7613.70 43.88 o 4 2 1 2255.37 1984.12 26.23 o 5 2 1 2620.67 2349.38 31.87 o 6 2 1 6896.93 6776.29 60.04 o 7 2 1 26.35 30.83 9.87 o 8 2 1 760.90 840.44 26.95 o 9 2 1 178.29 149.17 14.69 o 10 2 1 174.07 176.73 17.23 o 11 2 1 1296.73 1403.88 46.27 o 12 2 1 18.72 27.38 17.42 o 13 2 1 256.14 291.49 29.56 o -13 3 1 25.56 22.38 20.38 o -12 3 1 246.73 257.27 24.90 o -11 3 1 565.35 546.18 29.99 o -10 3 1 114.56 96.53 14.04 o -9 3 1 298.60 276.72 18.18 o -8 3 1 268.58 243.83 15.53 o -7 3 1 1322.73 1253.38 29.28 o -6 3 1 1779.42 1553.13 28.99 o -5 3 1 581.38 619.01 16.51 o -4 3 1 24.15 20.29 5.48 o -3 3 1 1986.11 2091.77 23.41 o -2 3 1 308.93 379.57 9.29 o -1 3 1 20324.09 20333.38 212.01 o 0 3 1 374.11 381.05 5.62 o 1 3 1 14264.37 13801.63 177.53 o 2 3 1 756.04 716.94 12.93 o 3 3 1 203.75 211.26 8.53 o 4 3 1 9456.77 9323.06 56.95 o 5 3 1 1279.53 1180.78 23.44 o 6 3 1 1551.20 1498.91 29.26 o 7 3 1 1252.66 1316.46 30.67 o 8 3 1 1094.50 1042.89 30.20 o 9 3 1 257.18 273.41 18.65 o 10 3 1 1162.75 1181.37 39.13 o 11 3 1 0.56 7.60 17.19 o 12 3 1 251.25 210.64 23.55 o 13 3 1 99.17 90.57 24.51 o -13 4 1 0.85 -7.28 21.31 o -12 4 1 135.30 127.66 21.50 o -11 4 1 115.98 115.70 17.51 o -10 4 1 296.02 304.55 21.29 o -9 4 1 56.70 50.35 12.66 o -8 4 1 74.64 71.42 10.26 o -7 4 1 1069.07 1005.34 26.73 o -6 4 1 143.86 144.12 10.54 o -5 4 1 91.80 105.10 8.07 o -4 4 1 631.90 695.85 16.37 o -3 4 1 4406.14 4671.10 36.20 o -2 4 1 180.65 207.44 7.65 o -1 4 1 306.74 298.95 8.41 o 0 4 1 714.22 769.69 8.80 o 1 4 1 1535.42 1682.01 18.70 o 2 4 1 207.64 226.21 8.32 o 3 4 1 1765.49 1905.91 24.21 o 4 4 1 110.72 89.39 7.63 o 5 4 1 30.80 27.30 8.16 o 6 4 1 0.51 4.85 8.95 o 7 4 1 2.77 11.99 9.59 o 8 4 1 97.72 91.68 11.56 o 9 4 1 13.55 11.52 12.34 o 10 4 1 1.52 -1.47 15.74 o 11 4 1 62.87 57.66 18.05 o 12 4 1 96.32 91.06 21.76 o 13 4 1 12.61 4.17 21.10 o -13 5 1 47.07 28.91 22.18 o -12 5 1 224.32 220.18 23.99 o -11 5 1 245.69 238.69 22.06 o -10 5 1 6.97 17.39 12.05 o -9 5 1 205.51 206.94 16.71 o -8 5 1 76.79 100.31 11.29 o -7 5 1 1211.95 1185.51 29.56 o -6 5 1 1966.92 1855.11 32.86 o -5 5 1 24.37 28.17 7.35 o -4 5 1 380.59 336.57 12.21 o -3 5 1 196.17 233.49 9.35 o -2 5 1 5798.68 6077.49 39.74 o -1 5 1 4396.63 4394.31 31.73 o 0 5 1 125.42 114.17 4.46 o 1 5 1 5458.09 5457.76 35.89 o 2 5 1 3089.34 2894.32 28.29 o 3 5 1 990.08 1025.90 18.98 o 4 5 1 4502.73 4662.42 43.51 o 5 5 1 2297.95 2153.13 32.81 o 6 5 1 198.47 211.47 12.78 o 7 5 1 2455.61 2489.22 43.27 o 8 5 1 826.43 759.75 26.72 o 9 5 1 232.12 232.39 18.14 o 10 5 1 933.42 986.45 37.34 o 11 5 1 28.02 21.92 18.70 o 12 5 1 386.48 370.66 29.54 o -13 6 1 408.47 427.52 33.97 o -12 6 1 45.89 10.82 21.06 o -11 6 1 394.48 421.35 27.69 o -10 6 1 798.97 818.31 33.80 o -9 6 1 0.91 0.82 12.40 o -8 6 1 1036.49 972.32 30.23 o -7 6 1 3665.19 3572.62 51.52 o -6 6 1 374.96 373.10 16.11 o -5 6 1 8229.53 8758.14 66.35 o -4 6 1 54.25 51.09 6.48 o -3 6 1 213.52 235.62 10.09 o -2 6 1 4575.19 4672.35 37.54 o -1 6 1 1676.35 1698.17 21.84 o 0 6 1 5958.44 5803.43 27.70 o 1 6 1 442.58 587.34 13.76 o 2 6 1 86.07 101.77 7.07 o 3 6 1 890.51 837.06 18.24 o 4 6 1 2532.11 2739.64 35.35 o 5 6 1 6209.81 6151.42 57.13 o 6 6 1 2618.72 2531.04 41.12 o 7 6 1 149.83 139.09 12.66 o 8 6 1 996.91 1022.51 31.83 o 9 6 1 302.66 299.32 20.31 o 10 6 1 285.94 282.29 22.20 o 11 6 1 643.43 648.32 34.84 o 12 6 1 154.72 172.59 23.94 o -12 7 1 360.98 365.11 30.54 o -11 7 1 513.10 543.20 32.05 o -10 7 1 7.25 17.98 14.58 o -9 7 1 731.20 728.66 29.63 o -8 7 1 101.58 77.97 11.73 o -7 7 1 1075.82 1081.55 30.01 o -6 7 1 2564.37 2596.34 41.32 o -5 7 1 1112.75 1182.69 26.11 o -4 7 1 127.24 115.50 8.69 o -3 7 1 5173.55 5402.19 46.30 o -2 7 1 1226.08 1344.97 21.97 o -1 7 1 3067.79 3136.06 31.76 o 0 7 1 12115.96 12994.23 65.06 o 1 7 1 656.79 674.05 15.74 o 2 7 1 935.26 911.88 18.73 o 3 7 1 31.57 36.63 6.15 o 4 7 1 307.17 286.74 12.98 o 5 7 1 11.47 8.42 9.07 o 6 7 1 601.45 572.27 21.01 o 7 7 1 266.84 293.42 17.06 o 8 7 1 39.12 33.93 12.48 o 9 7 1 182.43 183.86 17.63 o 10 7 1 94.84 100.29 15.97 o 11 7 1 36.27 33.37 17.82 o 12 7 1 373.46 375.20 31.10 o -12 8 1 80.13 90.06 23.09 o -11 8 1 16.21 20.94 17.16 o -10 8 1 22.35 22.39 15.35 o -9 8 1 10.98 -5.16 14.37 o -8 8 1 320.70 293.76 18.67 o -7 8 1 335.22 305.49 17.92 o -6 8 1 144.00 132.97 12.22 o -5 8 1 1956.90 1999.46 35.24 o -4 8 1 78.79 62.95 7.62 o -3 8 1 1018.86 1027.55 21.97 o -2 8 1 333.87 356.60 12.77 o -1 8 1 565.98 568.86 15.30 o 0 8 1 1035.69 1033.50 28.35 o 1 8 1 1104.80 1144.11 21.82 o 2 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