#------------------------------------------------------------------------------ #$Date: 2011-09-28 17:24:46 +0300 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/20/18/2201843.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_2201843_Fobs loop_ _publ_author_name 'Gravestock, David' 'McKenzie, Jean M.' _publ_section_title ; (5S*,6R*,7R*,9R*)-1-Benzyl-7,9-dimethyl-8-oxo-1-azaspiro[4.4]nonane-6-carbonitrile ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o63 _journal_page_last o65 _journal_volume 59 _journal_year 2003 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _cell_angle_alpha 90.000 _cell_angle_beta 93.680 _cell_angle_gamma 90.000 _cell_length_a 10.5435 _cell_length_b 10.6143 _cell_length_c 14.5703 _exptl_crystal_F_000 608.00 _reflns_d_resolution_high 0.8412 _[local]_cod_data_source_file cf62253sup2.hkl _[local]_cod_data_source_block 3 #BEGIN Tags that were not found in dictionaries: _shelx_title ' JM24; SPIROCYCLE; MONOCLINIC P2(1)/n' _shelx_refln_list_code 4 _shelx_f_calc_maximum 122.44 _shelx_f_squared_multiplier 1.000 #END Tags that were not found in dictionaries loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -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 1192.75 1575.15 6.39 o 4 0 0 1324.30 880.42 6.89 o 6 0 0 67.89 72.33 0.79 o 8 0 0 0.41 0.52 0.33 o 10 0 0 340.28 354.06 2.19 o 12 0 0 5.39 3.43 0.60 o 1 1 0 1541.43 1697.32 64.85 o 2 1 0 246.44 307.62 21.11 o 3 1 0 42.08 20.81 6.47 o 4 1 0 1.25 1.41 0.18 o 5 1 0 361.02 312.96 8.86 o 6 1 0 0.82 1.45 0.21 o 7 1 0 2.20 1.17 0.21 o 8 1 0 25.39 44.68 1.32 o 9 1 0 12.97 13.90 0.37 o 10 1 0 1.55 1.42 0.38 o 11 1 0 0.91 2.36 0.41 o 12 1 0 0.46 -0.26 0.63 o 0 2 0 686.62 361.79 3.84 o 1 2 0 508.83 511.15 12.34 o 2 2 0 180.30 111.25 8.96 o 3 2 0 2186.71 2559.55 200.70 o 4 2 0 14.02 14.80 0.72 o 5 2 0 212.32 176.56 9.93 o 6 2 0 2.11 7.35 0.21 o 7 2 0 46.24 51.62 2.93 o 8 2 0 88.69 93.01 3.37 o 9 2 0 40.56 29.49 0.56 o 10 2 0 13.43 9.50 0.51 o 11 2 0 0.72 1.81 0.39 o 12 2 0 1.18 0.50 0.41 o 1 3 0 2872.36 2752.85 20.72 o 2 3 0 2288.84 2028.46 139.98 o 3 3 0 557.62 504.11 41.05 o 4 3 0 50.99 54.71 5.12 o 5 3 0 378.77 516.39 36.76 o 6 3 0 174.78 154.19 9.78 o 7 3 0 58.08 74.21 4.81 o 8 3 0 186.77 150.46 5.40 o 9 3 0 359.32 354.50 15.31 o 10 3 0 2.17 0.75 0.50 o 11 3 0 2.73 1.41 0.85 o 12 3 0 6.56 9.73 0.46 o 0 4 0 279.67 151.82 1.54 o 1 4 0 222.76 157.99 1.85 o 2 4 0 1.07 1.13 0.61 o 3 4 0 106.91 85.94 6.86 o 4 4 0 0.09 4.22 0.28 o 5 4 0 123.73 170.65 16.18 o 6 4 0 20.80 17.77 1.17 o 7 4 0 0.39 2.26 0.30 o 8 4 0 0.06 3.76 1.78 o 9 4 0 146.40 145.81 10.54 o 10 4 0 9.38 12.36 0.43 o 11 4 0 1.30 1.46 0.55 o 1 5 0 870.04 744.93 5.06 o 2 5 0 180.46 218.57 10.19 o 3 5 0 438.37 472.88 32.91 o 4 5 0 49.38 52.15 2.79 o 5 5 0 170.46 156.15 11.86 o 6 5 0 33.08 35.62 2.31 o 7 5 0 257.79 308.96 26.33 o 8 5 0 19.80 20.49 1.32 o 9 5 0 1.55 0.20 0.67 o 10 5 0 6.88 7.67 0.92 o 11 5 0 7.31 8.50 0.45 o 0 6 0 24.14 12.46 0.27 o 1 6 0 24.47 26.15 0.39 o 2 6 0 3.69 3.08 0.73 o 3 6 0 4.89 8.33 0.24 o 4 6 0 0.09 -0.15 0.36 o 5 6 0 28.96 44.85 3.81 o 6 6 0 4.26 -0.46 0.46 o 7 6 0 41.81 65.42 5.06 o 8 6 0 178.22 201.38 18.87 o 9 6 0 8.29 12.83 0.97 o 10 6 0 8.04 7.59 0.44 o 11 6 0 0.12 -0.09 1.00 o 1 7 0 103.02 103.12 0.79 o 2 7 0 10.35 15.22 0.67 o 3 7 0 17.70 22.75 0.66 o 4 7 0 142.93 126.77 7.59 o 5 7 0 167.12 162.21 11.87 o 6 7 0 97.87 125.02 11.30 o 7 7 0 5.43 4.98 0.38 o 8 7 0 6.01 13.89 1.63 o 9 7 0 2.67 3.36 0.40 o 10 7 0 0.03 0.50 0.43 o 0 8 0 131.81 103.59 2.64 o 1 8 0 31.61 25.75 0.44 o 2 8 0 120.42 114.47 3.12 o 3 8 0 87.27 109.42 5.18 o 4 8 0 42.99 50.28 2.91 o 5 8 0 10.96 10.63 0.89 o 6 8 0 11.66 11.94 1.36 o 7 8 0 34.99 29.18 4.35 o 8 8 0 4.95 6.82 1.06 o 9 8 0 1.62 2.35 0.43 o 1 9 0 110.34 101.07 0.93 o 2 9 0 75.50 58.00 0.74 o 3 9 0 90.08 90.79 2.83 o 4 9 0 1.03 3.19 0.36 o 5 9 0 42.19 46.74 3.83 o 6 9 0 10.92 14.10 1.42 o 7 9 0 18.97 21.06 1.84 o 8 9 0 0.63 1.88 0.43 o 0 10 0 27.20 23.97 0.52 o 1 10 0 33.90 21.33 0.47 o 2 10 0 22.42 20.24 0.44 o 3 10 0 0.15 0.40 0.37 o 4 10 0 31.72 30.53 1.19 o 5 10 0 1.85 0.91 1.03 o 6 10 0 2.64 3.15 0.40 o 7 10 0 9.18 7.09 0.73 o 1 11 0 0.07 0.34 0.30 o 2 11 0 28.16 18.31 0.70 o 3 11 0 3.31 1.83 0.55 o 4 11 0 1.07 0.97 1.46 o 5 11 0 16.34 13.96 0.60 o 6 11 0 5.54 5.47 0.45 o 0 12 0 1.25 -0.26 0.62 o 1 12 0 1.06 -0.16 0.44 o 2 12 0 0.22 0.08 0.49 o 3 12 0 12.85 12.31 0.47 o -9 0 1 0.79 1.20 0.40 o -7 0 1 6.38 5.32 0.31 o -5 0 1 171.08 245.23 1.18 o -3 0 1 13.36 2.57 0.15 o -1 0 1 14.95 63.01 1.04 o 1 0 1 2842.89 3085.92 32.40 o 3 0 1 3924.60 3566.93 12.09 o 5 0 1 543.60 942.64 2.24 o 7 0 1 146.80 165.32 1.23 o 9 0 1 5.42 6.35 0.44 o 11 0 1 1.55 -0.34 0.84 o -12 1 1 5.25 5.95 0.76 o -11 1 1 76.87 72.15 0.94 o -10 1 1 20.95 14.01 1.09 o -9 1 1 0.64 0.12 0.29 o -8 1 1 26.37 37.68 0.57 o -7 1 1 14.64 15.48 0.32 o -6 1 1 1.52 4.08 0.50 o -5 1 1 0.32 3.14 0.41 o -4 1 1 538.96 493.24 23.23 o -3 1 1 41.19 16.26 1.38 o -2 1 1 5806.77 5445.25 500.54 o -1 1 1 14991.43 10179.05 576.96 o 0 1 1 478.58 337.29 25.22 o 1 1 1 3052.83 2858.42 27.72 o 2 1 1 908.27 897.70 48.68 o 3 1 1 248.07 439.03 14.94 o 4 1 1 27.88 94.23 2.64 o 5 1 1 220.50 160.58 3.99 o 6 1 1 452.24 581.07 14.90 o 7 1 1 1.06 1.40 0.61 o 8 1 1 5.29 6.61 0.51 o 9 1 1 30.79 30.47 1.43 o 10 1 1 0.41 2.20 0.42 o 11 1 1 8.30 9.92 0.44 o 12 1 1 7.50 7.02 0.43 o -12 2 1 1.52 1.10 0.66 o -11 2 1 28.37 32.19 1.27 o -10 2 1 49.56 47.15 1.77 o -9 2 1 44.37 38.12 1.29 o -8 2 1 0.60 -0.28 0.43 o -7 2 1 39.47 38.26 1.20 o -6 2 1 0.08 1.48 0.86 o -5 2 1 32.85 43.14 3.13 o -4 2 1 3.64 1.49 0.15 o -3 2 1 82.23 114.13 10.88 o -2 2 1 2358.82 2560.32 245.96 o -1 2 1 13417.54 12769.18 495.10 o 0 2 1 87.66 12.65 0.78 o 1 2 1 2362.25 1948.30 29.43 o 2 2 1 2758.77 2573.77 91.10 o 3 2 1 1972.12 2523.00 156.26 o 4 2 1 1052.09 1432.68 47.78 o 5 2 1 305.21 336.49 15.54 o 6 2 1 40.18 41.35 1.29 o 7 2 1 29.89 35.85 1.85 o 8 2 1 23.44 11.59 0.30 o 9 2 1 7.82 9.42 0.34 o 10 2 1 10.62 9.18 0.40 o 11 2 1 0.02 -0.65 1.01 o 12 2 1 0.21 2.66 0.48 o -12 3 1 0.50 0.88 0.43 o -11 3 1 1.75 1.08 1.13 o -10 3 1 0.03 -0.58 0.58 o -9 3 1 33.42 39.40 4.48 o -8 3 1 36.45 38.90 1.96 o -7 3 1 29.51 28.41 2.24 o -6 3 1 13.74 15.71 0.92 o -5 3 1 93.14 124.64 13.01 o -4 3 1 944.22 1206.36 110.01 o -3 3 1 397.46 278.22 32.39 o -2 3 1 99.86 183.65 18.82 o -1 3 1 2116.13 1813.11 37.55 o 0 3 1 617.59 645.28 14.43 o 1 3 1 2311.42 2109.81 29.11 o 2 3 1 19.03 24.55 1.33 o 3 3 1 1.65 0.04 0.17 o 4 3 1 1.57 0.16 0.41 o 5 3 1 134.57 139.16 7.54 o 6 3 1 102.43 104.38 5.79 o 7 3 1 0.45 -0.19 0.38 o 8 3 1 1.46 0.06 0.36 o 9 3 1 10.10 11.77 0.37 o 10 3 1 18.03 16.11 0.91 o 11 3 1 3.65 6.00 0.87 o 12 3 1 2.03 2.76 0.50 o -11 4 1 7.53 4.93 0.74 o -10 4 1 23.88 19.81 0.67 o -9 4 1 82.70 91.31 6.33 o -8 4 1 0.44 0.92 0.46 o -7 4 1 56.00 58.82 4.64 o -6 4 1 92.60 72.57 7.43 o -5 4 1 423.88 420.65 41.80 o -4 4 1 89.04 71.91 8.15 o -3 4 1 114.31 199.74 19.65 o -2 4 1 1833.98 1703.76 85.02 o -1 4 1 370.85 406.39 7.82 o 0 4 1 137.54 188.43 4.26 o 1 4 1 206.00 131.79 1.30 o 2 4 1 16.25 26.58 0.48 o 3 4 1 646.15 724.23 25.98 o 4 4 1 303.71 416.72 24.01 o 5 4 1 416.63 409.93 21.31 o 6 4 1 415.79 515.27 30.55 o 7 4 1 15.00 8.99 0.55 o 8 4 1 146.20 148.77 8.24 o 10 4 1 0.13 -0.57 0.57 o 11 4 1 0.31 -0.49 0.86 o -11 5 1 0.29 0.60 0.50 o -10 5 1 10.01 8.85 0.83 o -9 5 1 33.40 37.90 2.58 o -8 5 1 8.94 11.89 0.67 o -7 5 1 175.36 212.07 17.98 o -6 5 1 128.74 176.19 11.68 o -5 5 1 124.54 125.84 13.85 o -4 5 1 37.58 26.33 2.78 o -3 5 1 1354.38 1328.05 104.66 o -2 5 1 587.28 753.69 41.73 o -1 5 1 29.06 31.70 0.55 o 0 5 1 138.05 207.69 1.20 o 1 5 1 160.27 97.89 0.86 o 2 5 1 106.65 67.95 1.87 o 3 5 1 96.13 78.17 4.18 o 4 5 1 86.33 96.90 4.72 o 5 5 1 30.81 34.20 2.62 o 6 5 1 68.42 82.14 6.91 o 7 5 1 400.43 424.54 28.91 o 8 5 1 167.92 144.32 8.45 o 9 5 1 36.09 30.65 3.13 o 10 5 1 0.28 0.33 0.62 o 11 5 1 6.71 4.99 0.72 o -11 6 1 3.23 2.05 0.45 o -10 6 1 0.00 -0.94 0.94 o -9 6 1 0.78 0.63 0.47 o -8 6 1 36.72 44.93 4.28 o -7 6 1 138.31 148.39 12.54 o -6 6 1 52.87 45.87 4.35 o -5 6 1 69.54 58.99 6.45 o -4 6 1 1.37 3.91 0.23 o -3 6 1 4.85 3.86 0.42 o -2 6 1 176.66 204.97 5.67 o -1 6 1 16.40 30.45 1.11 o 0 6 1 101.42 84.96 1.47 o 1 6 1 114.00 119.47 0.69 o 2 6 1 7.72 4.18 0.20 o 3 6 1 0.20 2.16 0.21 o 4 6 1 124.62 123.68 5.46 o 5 6 1 31.11 24.42 1.86 o 6 6 1 7.36 14.66 1.17 o 7 6 1 18.65 25.37 3.05 o 8 6 1 9.63 13.55 1.97 o 9 6 1 6.12 9.56 0.42 o 10 6 1 0.00 -0.04 0.61 o -10 7 1 4.36 6.64 0.71 o -9 7 1 6.62 4.49 0.60 o -8 7 1 4.57 1.51 0.83 o -7 7 1 4.54 1.22 0.36 o -6 7 1 194.31 211.60 20.63 o -5 7 1 4.95 3.48 0.63 o -4 7 1 285.87 302.44 22.49 o -3 7 1 16.03 4.51 0.24 o -2 7 1 12.10 11.84 0.52 o -1 7 1 21.28 23.29 0.53 o 0 7 1 11.45 13.04 0.20 o 1 7 1 16.47 12.81 0.19 o 2 7 1 0.05 -0.44 0.52 o 3 7 1 8.58 7.62 0.46 o 4 7 1 6.18 5.33 0.32 o 5 7 1 66.20 51.47 1.19 o 6 7 1 161.36 166.96 12.10 o 7 7 1 30.90 41.63 3.36 o 8 7 1 2.09 1.19 0.82 o 9 7 1 1.14 2.89 0.41 o 10 7 1 0.72 -0.66 0.66 o -9 8 1 5.69 7.18 0.74 o -8 8 1 7.60 4.74 0.40 o -7 8 1 0.04 -0.54 1.14 o -6 8 1 109.94 111.90 10.69 o -5 8 1 2.05 0.23 0.37 o -4 8 1 20.08 19.26 1.40 o -3 8 1 167.44 164.08 8.53 o -2 8 1 18.90 8.29 0.28 o -1 8 1 2.52 6.35 0.24 o 0 8 1 226.49 204.41 1.47 o 1 8 1 37.85 35.87 0.40 o 2 8 1 27.09 29.92 1.04 o 3 8 1 16.01 14.51 0.69 o 4 8 1 145.16 163.07 8.15 o 5 8 1 3.62 3.96 0.43 o 6 8 1 1.75 1.60 0.74 o 7 8 1 6.07 3.24 0.39 o 8 8 1 3.21 2.38 0.45 o 9 8 1 1.82 6.74 1.47 o -8 9 1 4.19 3.63 0.70 o -7 9 1 0.00 0.52 0.46 o -6 9 1 2.61 1.19 0.38 o -5 9 1 23.22 24.15 2.54 o -4 9 1 115.42 109.76 7.19 o -3 9 1 11.06 7.22 0.45 o -2 9 1 0.07 0.12 0.51 o -1 9 1 20.82 19.42 0.30 o 0 9 1 11.06 7.61 0.32 o 1 9 1 29.39 27.44 0.38 o 2 9 1 3.54 2.66 0.31 o 3 9 1 0.16 0.27 0.37 o 4 9 1 40.42 39.89 2.51 o 5 9 1 16.36 14.76 1.14 o 6 9 1 3.93 2.73 0.38 o 7 9 1 0.02 -0.60 0.60 o 8 9 1 11.73 9.53 1.29 o -7 10 1 0.88 3.64 1.37 o -6 10 1 2.91 1.30 0.75 o -5 10 1 1.50 0.16 0.46 o -4 10 1 1.04 1.75 0.40 o -3 10 1 80.04 75.22 3.98 o -2 10 1 8.92 10.21 0.99 o -1 10 1 19.52 19.76 0.36 o 0 10 1 74.14 78.67 1.15 o 1 10 1 3.52 4.87 0.28 o 2 10 1 57.83 61.93 0.82 o 3 10 1 3.29 3.94 0.38 o 4 10 1 35.02 34.32 1.60 o 5 10 1 5.06 6.87 1.12 o 6 10 1 4.99 3.51 0.42 o 7 10 1 11.64 17.87 0.61 o -6 11 1 1.85 0.04 0.66 o -5 11 1 1.00 1.20 0.67 o -4 11 1 10.32 12.53 0.44 o -3 11 1 0.06 -0.61 0.61 o -2 11 1 5.46 7.74 1.08 o -1 11 1 69.79 67.36 0.87 o 0 11 1 7.82 5.61 0.30 o 1 11 1 11.20 11.93 0.40 o 2 11 1 0.20 -0.46 0.46 o 3 11 1 13.75 13.43 0.49 o 4 11 1 3.38 2.54 0.42 o 5 11 1 0.19 0.08 0.48 o 6 11 1 8.74 7.21 0.46 o -3 12 1 0.90 -0.12 0.66 o -2 12 1 6.24 7.65 0.45 o -1 12 1 2.75 1.03 0.30 o 0 12 1 0.63 2.69 0.29 o 1 12 1 0.86 -0.22 0.53 o 2 12 1 0.03 -0.02 0.62 o 3 12 1 0.03 -0.35 0.65 o -12 0 2 0.37 0.58 0.59 o -10 0 2 5.30 8.42 0.56 o -8 0 2 0.09 2.13 0.34 o -6 0 2 1570.14 1498.26 11.42 o -4 0 2 67.30 94.22 0.69 o -2 0 2 858.57 601.94 4.37 o 0 0 2 336.29 614.63 22.87 o 2 0 2 763.08 956.80 5.64 o 4 0 2 279.84 262.01 1.10 o 6 0 2 887.73 873.47 2.45 o 8 0 2 8.28 16.85 0.49 o 10 0 2 136.28 126.06 1.47 o 12 0 2 10.69 10.40 0.64 o -12 1 2 16.56 14.91 0.48 o -11 1 2 8.33 9.50 0.43 o -10 1 2 45.53 38.79 2.04 o -9 1 2 1.36 0.30 0.54 o -8 1 2 30.91 30.09 0.54 o -7 1 2 28.47 29.37 0.59 o -6 1 2 14.32 17.16 0.59 o -5 1 2 1802.71 1871.56 71.50 o -4 1 2 364.67 454.68 21.16 o -3 1 2 67.61 41.54 1.84 o -2 1 2 6925.62 7687.77 325.08 o -1 1 2 2642.72 2663.27 86.26 o 0 1 2 4450.38 4902.17 333.44 o 1 1 2 3551.00 3165.32 85.08 o 2 1 2 1523.17 1232.51 5.55 o 3 1 2 1.67 0.78 0.43 o 4 1 2 0.89 18.01 0.76 o 5 1 2 180.22 240.93 1.91 o 6 1 2 17.63 34.36 1.92 o 7 1 2 3.58 1.13 0.22 o 8 1 2 9.78 3.77 0.30 o 9 1 2 0.31 0.19 0.38 o 10 1 2 15.39 19.32 0.44 o 11 1 2 0.43 -0.59 0.59 o 12 1 2 5.43 3.16 0.43 o -12 2 2 0.14 -0.01 0.65 o -11 2 2 18.79 16.40 0.45 o -10 2 2 9.42 8.88 0.40 o -9 2 2 21.23 17.94 0.76 o -8 2 2 49.58 47.85 2.01 o -7 2 2 6.61 8.60 0.70 o -6 2 2 248.51 235.19 14.26 o -5 2 2 66.00 40.95 2.34 o -4 2 2 4.21 1.50 0.14 o -3 2 2 64.41 85.16 5.22 o -2 2 2 1565.46 1815.08 204.29 o -1 2 2 721.36 657.73 53.85 o 0 2 2 726.14 749.17 51.98 o 1 2 2 666.52 878.99 36.28 o 2 2 2 129.66 145.84 2.95 o 3 2 2 650.45 533.48 14.88 o 4 2 2 824.63 943.14 27.05 o 5 2 2 46.43 146.02 4.18 o 6 2 2 41.49 41.16 0.90 o 7 2 2 2.74 0.16 0.23 o 8 2 2 72.15 81.88 1.65 o 9 2 2 6.90 5.59 0.34 o 10 2 2 12.99 15.39 0.88 o 11 2 2 0.10 0.07 0.58 o 12 2 2 0.00 0.00 0.98 o -12 3 2 12.71 9.12 0.46 o -11 3 2 1.57 2.97 0.41 o -10 3 2 0.14 0.66 0.38 o -9 3 2 0.10 0.26 0.33 o -8 3 2 32.42 39.20 1.29 o -7 3 2 262.94 253.91 17.98 o -6 3 2 4.54 4.49 0.40 o -5 3 2 31.83 84.75 9.00 o -4 3 2 217.59 272.77 26.83 o -3 3 2 6.10 1.14 0.14 o -2 3 2 86.96 131.50 13.19 o -1 3 2 166.64 164.20 6.64 o 0 3 2 246.70 115.13 6.02 o 1 3 2 8.69 14.90 2.76 o 2 3 2 1365.87 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