#------------------------------------------------------------------------------ #$Date: 2011-09-16 18:46:08 +0300 (Fri, 16 Sep 2011) $ #$Revision: 26025 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/2011115.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_2011115_Fobs loop_ _publ_author_name 'Bats, Jan W.' 'Rivas Nass, Andreas' 'Hashmi, A. Stephen K.' _publ_section_title ; Tetraallyl (2,2'-bipyridyl)-rac-3,3,7,7-tetramethyl-trans-5-palladatricyclo[4.1.0.0^2,^^4^]heptane-1,2,4,6-tetracarboxylate above and below the phase-transition temperature of 194K ; _journal_issue 7 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 814 _journal_page_last 817 _journal_volume 56 _journal_year 2000 _space_group_IT_number 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 83.438 _cell_angle_beta 88.482 _cell_angle_gamma 72.118 _cell_length_a 8.9583 _cell_length_b 11.3245 _cell_length_c 17.9063 _exptl_crystal_F_000 760.00 _reflns_d_resolution_high 0.6641 _[local]_cod_data_source_file fg1601I205Ksup3.hkl _[local]_cod_data_source_block I205K #BEGIN Tags that were not found in dictionaries: _shelx_title ' test in P-1' _shelx_refln_list_code 4 _shelx_f_calc_maximum 191.74 _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 12290.29 12472.14 221.36 o 2 0 0 2000.98 2329.45 155.69 o 3 0 0 5341.13 5304.96 199.35 o 4 0 0 293.61 306.21 17.28 o 5 0 0 340.33 322.55 6.54 o 6 0 0 3480.86 3273.86 77.85 o 7 0 0 96.40 97.33 6.54 o 8 0 0 1204.09 1199.48 66.16 o 9 0 0 168.41 160.17 15.21 o 10 0 0 0.70 5.89 11.53 o 11 0 0 280.49 232.70 31.44 o 12 0 0 104.09 73.23 25.72 o -12 1 0 58.66 87.30 48.82 o -11 1 0 101.56 90.26 25.72 o -10 1 0 55.85 31.74 13.58 o -9 1 0 453.67 452.45 18.81 o -8 1 0 212.58 224.32 8.81 o -7 1 0 2135.38 1949.20 47.71 o -6 1 0 1282.56 1288.14 39.85 o -5 1 0 293.73 332.17 9.94 o -4 1 0 458.92 369.46 18.80 o -3 1 0 7130.87 7275.58 165.16 o -2 1 0 32453.88 27703.54 1277.69 o -1 1 0 4247.16 4349.54 133.26 o 0 1 0 18559.85 17973.08 2256.61 o 1 1 0 8526.78 9518.53 566.03 o 2 1 0 3982.92 3964.93 169.85 o 3 1 0 860.77 961.54 25.18 o 4 1 0 834.40 912.01 44.04 o 5 1 0 4720.04 4606.58 198.95 o 6 1 0 1055.51 937.04 37.71 o 7 1 0 1215.17 1232.71 42.86 o 8 1 0 1002.55 1085.65 40.43 o 9 1 0 239.75 222.28 9.57 o 10 1 0 104.82 105.94 14.69 o 11 1 0 196.41 226.14 27.39 o 12 1 0 5.53 -13.34 21.67 o -11 2 0 62.52 45.72 21.20 o -10 2 0 136.31 177.75 14.89 o -9 2 0 216.61 226.01 12.04 o -8 2 0 31.33 42.01 7.18 o -7 2 0 944.86 955.17 28.44 o -6 2 0 1684.22 1645.67 32.98 o -5 2 0 500.51 547.38 22.57 o -4 2 0 375.33 377.16 17.39 o -3 2 0 1567.84 1527.00 65.13 o -2 2 0 1284.93 1397.32 39.74 o -1 2 0 7489.96 8231.03 155.89 o 0 2 0 1634.56 1359.66 336.41 o 1 2 0 804.31 749.87 14.50 o 2 2 0 5477.77 4549.20 434.98 o 3 2 0 104.77 185.11 11.75 o 4 2 0 968.46 979.87 66.82 o 5 2 0 5307.46 5065.75 164.14 o 6 2 0 25.50 25.83 4.20 o 7 2 0 704.35 636.54 28.90 o 8 2 0 111.06 114.00 7.27 o 9 2 0 83.43 81.60 11.54 o 10 2 0 526.73 508.99 12.92 o 11 2 0 127.46 109.79 21.32 o 12 2 0 13.24 -7.38 19.89 o -11 3 0 5.14 3.57 24.05 o 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0 341.32 287.27 10.30 o 1 4 0 3727.60 3650.65 145.36 o 2 4 0 12509.95 12296.36 582.70 o 3 4 0 2684.39 2848.25 62.76 o 4 4 0 5656.18 5913.02 268.20 o 5 4 0 1013.21 978.46 45.55 o 6 4 0 229.23 207.00 10.74 o 7 4 0 477.00 460.75 28.36 o 8 4 0 163.56 142.71 11.05 o 9 4 0 297.02 281.26 24.24 o 10 4 0 300.00 291.45 21.40 o 11 4 0 17.74 16.07 18.58 o 12 4 0 77.66 58.23 20.96 o 13 4 0 21.32 -22.74 22.74 o -10 5 0 110.36 165.04 36.68 o -9 5 0 19.19 10.55 15.98 o -8 5 0 367.13 344.09 12.23 o -7 5 0 230.78 269.78 9.86 o -6 5 0 2.38 5.23 5.53 o -5 5 0 2531.84 2401.18 70.00 o -4 5 0 2059.19 2185.32 74.92 o -3 5 0 193.09 239.27 14.14 o -2 5 0 2656.89 2556.97 192.75 o -1 5 0 763.99 787.94 29.76 o 0 5 0 279.61 294.93 12.88 o 1 5 0 7400.78 7098.22 320.66 o 2 5 0 1963.18 2134.82 75.57 o 3 5 0 2387.81 2655.15 90.52 o 4 5 0 1873.26 1701.52 77.79 o 5 5 0 27.48 35.21 4.65 o 6 5 0 656.60 702.46 25.20 o 7 5 0 759.85 774.10 14.57 o 8 5 0 18.18 36.14 7.59 o 9 5 0 1568.57 1663.93 33.86 o 10 5 0 85.33 91.89 10.82 o 11 5 0 78.16 78.64 15.12 o 12 5 0 228.40 235.55 29.77 o 13 5 0 19.61 -4.76 23.34 o -10 6 0 21.63 18.70 17.15 o -9 6 0 97.67 108.36 18.49 o -8 6 0 251.06 217.51 21.74 o -7 6 0 170.57 165.01 13.69 o -6 6 0 118.96 114.12 8.21 o -5 6 0 937.73 972.27 19.29 o -4 6 0 32.17 36.19 6.37 o -3 6 0 4476.26 4541.16 157.90 o -2 6 0 2531.96 2446.52 102.48 o -1 6 0 758.73 780.00 30.57 o 0 6 0 1279.84 1391.84 46.21 o 1 6 0 3046.94 2947.09 55.84 o 2 6 0 576.21 705.22 39.36 o 3 6 0 2888.61 2641.83 91.10 o 4 6 0 1711.36 1689.06 56.45 o 5 6 0 220.65 230.60 9.95 o 6 6 0 2041.47 2011.01 99.74 o 7 6 0 1409.74 1353.87 63.32 o 8 6 0 334.30 336.88 12.93 o 9 6 0 1302.47 1255.69 26.14 o 10 6 0 99.33 91.96 18.17 o 11 6 0 22.38 13.20 11.39 o 12 6 0 136.61 134.13 17.56 o 13 6 0 0.65 -19.53 19.53 o -9 7 0 34.25 13.24 16.50 o -8 7 0 187.53 174.23 19.30 o -7 7 0 82.32 61.14 9.21 o -6 7 0 330.73 364.83 14.42 o -5 7 0 818.22 806.54 26.26 o -4 7 0 30.45 29.21 6.13 o -3 7 0 902.63 955.94 29.23 o -2 7 0 37.51 38.47 8.82 o 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24.65 o 13 8 0 63.59 78.83 28.82 o -8 9 0 115.70 117.33 21.05 o -7 9 0 3.57 -0.50 12.97 o -6 9 0 285.57 284.13 24.25 o -5 9 0 23.49 21.41 14.21 o -4 9 0 208.42 199.65 22.63 o -3 9 0 573.96 528.38 21.35 o -2 9 0 59.97 74.77 7.17 o -1 9 0 430.85 437.16 15.72 o 0 9 0 724.90 720.15 17.56 o 1 9 0 104.48 91.79 6.95 o 2 9 0 153.22 154.01 10.25 o 3 9 0 365.35 387.68 9.96 o 4 9 0 5.54 -2.22 4.36 o 5 9 0 172.49 200.30 12.66 o 6 9 0 77.27 89.77 8.67 o 7 9 0 464.06 503.50 15.85 o 8 9 0 250.42 321.30 24.95 o 9 9 0 0.45 7.88 12.92 o 10 9 0 50.12 68.06 20.48 o 11 9 0 22.39 0.19 18.58 o 12 9 0 68.00 52.39 29.05 o -7 10 0 85.43 99.04 20.26 o -6 10 0 179.51 171.60 16.13 o -5 10 0 8.59 17.28 10.72 o -4 10 0 318.34 310.42 23.96 o -3 10 0 394.04 415.21 16.90 o -2 10 0 50.73 63.82 9.45 o -1 10 0 1323.75 1450.45 58.30 o 0 10 0 1.56 -4.24 9.83 o 1 10 0 219.42 243.99 15.98 o 2 10 0 27.81 43.01 10.49 o 3 10 0 1.24 -8.21 8.21 o 4 10 0 363.58 411.62 14.42 o 5 10 0 562.65 534.18 24.70 o 6 10 0 0.70 -2.96 8.87 o 7 10 0 1039.20 936.30 24.21 o 8 10 0 527.78 543.72 29.40 o 9 10 0 11.49 8.03 10.63 o 10 10 0 173.12 212.95 18.51 o 11 10 0 78.58 27.86 21.31 o 12 10 0 24.62 37.75 27.27 o -6 11 0 100.85 90.63 21.43 o -5 11 0 7.19 23.62 13.57 o -4 11 0 762.37 722.92 25.40 o -3 11 0 169.78 185.16 13.57 o -2 11 0 423.44 459.96 28.11 o -1 11 0 692.77 685.66 42.55 o 0 11 0 755.34 775.50 37.39 o 1 11 0 2428.98 2340.29 101.31 o 2 11 0 705.53 677.37 17.46 o 3 11 0 14.74 27.30 11.09 o 4 11 0 625.39 570.74 14.08 o 5 11 0 382.79 418.72 14.52 o 6 11 0 114.21 115.38 11.34 o 7 11 0 598.18 662.25 19.71 o 8 11 0 106.91 126.14 14.41 o 9 11 0 148.27 133.47 16.58 o 10 11 0 331.14 374.09 22.54 o 11 11 0 23.03 -19.77 19.77 o 12 11 0 69.87 95.14 35.37 o -5 12 0 106.43 93.05 38.46 o -4 12 0 274.64 247.65 20.97 o -3 12 0 53.54 64.25 18.85 o -2 12 0 805.66 749.13 42.48 o -1 12 0 461.93 467.72 17.96 o 0 12 0 446.99 443.67 20.37 o 1 12 0 1170.52 1223.71 57.65 o 2 12 0 130.91 127.02 11.05 o 3 12 0 183.86 179.10 11.83 o 4 12 0 872.84 866.55 27.10 o 5 12 0 15.24 24.86 20.97 o 6 12 0 545.96 518.45 19.12 o 7 12 0 450.72 486.89 33.30 o 8 12 0 0.10 7.86 15.96 o 9 12 0 146.43 138.04 17.20 o 10 12 0 146.99 197.31 32.27 o 11 12 0 2.15 30.48 23.81 o -4 13 0 90.02 63.68 20.42 o -3 13 0 21.69 40.97 20.24 o -2 13 0 244.35 239.48 20.63 o -1 13 0 29.78 19.40 13.31 o 0 13 0 159.96 159.79 17.16 o 1 13 0 266.85 267.58 18.86 o 2 13 0 0.79 -0.45 12.40 o 3 13 0 472.73 454.31 44.28 o 4 13 0 337.64 309.02 18.03 o 5 13 0 88.97 87.38 15.36 o 6 13 0 694.03 703.26 69.65 o 7 13 0 85.22 69.76 49.65 o 8 13 0 23.70 -11.64 11.64 o 9 13 0 118.39 86.81 24.17 o 10 13 0 34.36 -9.88 24.05 o 11 13 0 75.33 35.37 26.91 o -2 14 0 71.24 119.79 28.34 o -1 14 0 17.33 8.93 18.22 o 0 14 0 158.38 165.87 18.90 o 1 14 0 184.66 231.87 20.79 o 2 14 0 1.73 19.12 11.21 o 3 14 0 197.81 196.38 15.00 o 4 14 0 5.12 7.53 12.32 o 5 14 0 48.36 123.60 24.05 o 6 14 0 64.78 87.76 28.34 o 7 14 0 38.28 81.16 28.28 o 8 14 0 174.36 144.82 41.68 o 9 14 0 201.13 275.56 34.18 o 10 14 0 2.93 -14.41 27.03 o -1 15 0 66.21 62.63 26.32 o 0 15 0 226.16 241.98 32.27 o 1 15 0 28.59 48.82 25.24 o 2 15 0 146.99 153.38 20.26 o 3 15 0 155.96 172.94 32.51 o 4 15 0 0.45 49.18 23.93 o 5 15 0 147.34 140.04 27.39 o 6 15 0 227.12 269.96 34.89 o 7 15 0 4.00 -4.52 25.48 o 8 15 0 144.06 173.62 35.25 o 9 15 0 17.72 -28.34 28.34 o 2 16 0 344.67 363.58 39.42 o 3 16 0 152.89 158.73 29.17 o 4 16 0 20.97 35.25 30.24 o 6 16 0 46.72 39.06 28.70 o 7 16 0 153.49 172.19 34.65 o -7 -16 1 91.96 118.96 32.15 o -6 -16 1 315.00 347.02 38.35 o -5 -16 1 51.75 38.10 27.51 o -4 -16 1 83.35 159.20 38.82 o -3 -16 1 222.57 251.38 36.20 o -2 -16 1 46.24 78.35 27.27 o -9 -15 1 164.64 150.99 36.08 o -8 -15 1 16.35 -12.15 24.17 o -7 -15 1 159.63 209.70 30.37 o -6 -15 1 160.27 259.95 35.72 o -5 -15 1 3.88 13.69 22.39 o -4 -15 1 36.12 101.21 28.70 o -3 -15 1 127.78 158.79 28.88 o -2 -15 1 41.08 38.58 16.75 o -1 -15 1 451.66 344.06 33.47 o 0 -15 1 184.83 129.20 29.53 o 1 -15 1 17.04 17.50 24.89 o -10 -14 1 111.41 93.24 34.65 o -9 -14 1 147.43 107.05 28.58 o -8 -14 1 0.83 -12.61 12.61 o -7 -14 1 99.05 93.36 25.24 o -6 -14 1 18.29 34.53 23.22 o -5 -14 1 9.11 37.15 21.79 o -4 -14 1 165.83 187.43 28.46 o -3 -14 1 127.96 142.19 13.92 o -2 -14 1 187.94 201.56 16.83 o -1 -14 1 174.80 158.58 18.94 o 0 -14 1 55.79 65.08 17.49 o 1 -14 1 46.43 80.61 24.05 o 2 -14 1 149.25 229.94 30.84 o -11 -13 1 3.54 16.43 27.03 o -10 -13 1 188.79 249.71 35.25 o -9 -13 1 10.26 68.11 24.29 o -8 -13 1 183.29 198.88 19.02 o -7 -13 1 859.61 898.68 37.05 o -6 -13 1 315.62 298.47 17.42 o -5 -13 1 61.60 111.23 40.25 o -4 -13 1 453.18 474.88 31.98 o -3 -13 1 40.24 63.08 11.03 o -2 -13 1 90.08 100.20 11.39 o -1 -13 1 61.99 78.72 11.89 o 0 -13 1 0.20 29.73 11.06 o 1 -13 1 241.99 276.38 20.76 o 2 -13 1 195.76 182.60 19.83 o 3 -13 1 91.78 79.43 19.24 o 4 -13 1 339.89 341.23 25.72 o -11 -12 1 84.21 72.04 25.13 o -10 -12 1 244.67 209.35 33.82 o -9 -12 1 39.11 25.21 31.32 o -8 -12 1 260.68 301.39 63.77 o -7 -12 1 337.58 306.26 41.28 o -6 -12 1 22.08 14.07 16.02 o -5 -12 1 819.98 820.09 21.13 o -4 -12 1 196.95 157.96 19.35 o -3 -12 1 206.98 203.20 12.18 o -2 -12 1 963.48 1020.54 58.90 o -1 -12 1 429.75 447.91 16.13 o 0 -12 1 94.77 105.77 17.07 o 1 -12 1 977.41 915.89 23.50 o 2 -12 1 238.87 209.54 20.16 o 3 -12 1 135.45 139.28 13.98 o 4 -12 1 107.86 131.80 19.41 o 5 -12 1 0.27 -21.43 21.43 o -12 -11 1 0.67 -23.10 23.10 o -11 -11 1 141.10 190.88 32.87 o -10 -11 1 190.40 213.20 19.19 o -9 -11 1 16.61 16.07 18.28 o -8 -11 1 403.00 416.77 16.69 o -7 -11 1 201.94 190.75 13.10 o -6 -11 1 139.53 161.25 10.83 o -5 -11 1 551.36 536.60 26.34 o -4 -11 1 54.76 33.67 7.15 o -3 -11 1 439.58 437.91 25.40 o -2 -11 1 631.54 740.29 30.46 o -1 -11 1 831.68 818.67 20.54 o 0 -11 1 502.68 498.34 15.98 o 1 -11 1 1220.03 1202.51 22.38 o 2 -11 1 3.76 0.53 7.41 o 3 -11 1 455.01 417.05 13.39 o 4 -11 1 61.22 92.60 16.34 o 5 -11 1 34.53 89.41 18.69 o 6 -11 1 128.29 171.41 34.18 o -12 -10 1 0.07 -20.24 20.24 o -11 -10 1 123.19 155.75 30.48 o -10 -10 1 5.00 -11.10 11.10 o -9 -10 1 116.63 127.04 12.33 o -8 -10 1 621.54 630.02 31.12 o -7 -10 1 0.20 0.01 11.78 o -6 -10 1 639.60 629.05 40.42 o -5 -10 1 644.74 663.93 25.18 o -4 -10 1 26.33 33.17 6.58 o -3 -10 1 17.74 18.93 10.91 o -2 -10 1 3.50 8.53 7.73 o -1 -10 1 228.64 249.16 11.21 o 0 -10 1 1268.80 1244.16 21.60 o 1 -10 1 336.10 326.10 10.11 o 2 -10 1 237.49 214.33 13.24 o 3 -10 1 371.77 392.72 24.98 o 4 -10 1 0.87 -8.37 8.37 o 5 -10 1 92.01 124.86 14.45 o 6 -10 1 92.87 123.78 15.02 o 7 -10 1 10.21 1.10 18.35 o -12 -9 1 10.74 22.39 24.41 o -11 -9 1 127.20 144.01 40.78 o -10 -9 1 20.24 -3.15 12.15 o -9 -9 1 140.54 154.45 28.32 o -8 -9 1 447.93 448.46 15.12 o -7 -9 1 99.94 95.56 9.31 o -6 -9 1 504.39 598.00 15.78 o -5 -9 1 70.60 62.14 7.38 o -4 -9 1 377.51 445.63 19.74 o -3 -9 1 21.28 22.77 5.32 o -2 -9 1 295.92 311.55 9.52 o -1 -9 1 3.26 -1.12 4.76 o 0 -9 1 369.79 379.33 12.82 o 1 -9 1 5.02 12.20 5.19 o 2 -9 1 532.34 509.33 26.42 o 3 -9 1 173.81 196.05 9.58 o 4 -9 1 35.18 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