#------------------------------------------------------------------------------ #$Date: 2016-04-02 23:00:40 +0300 (Sat, 02 Apr 2016) $ #$Revision: 180898 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/10/38/2103886.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_2103886_Fobs loop_ _publ_author_name 'Hashizume, Daisuke' 'Miki, Naoko' 'Yamazaki, Toshiyuki' 'Aoyagi, Yosuke' 'Arisato, Tomokuni' 'Uchiyama, Hiroki' 'Endo, Tadashi' 'Yasui, Masanori' 'Iwasaki, Fujiko' _publ_section_title ; Mechanism of the first-order phase transition of an acylurea derivative: observation of intermediate stages of transformation with a detailed temperature-resolved single-crystal diffraction method ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 404 _journal_page_last 415 _journal_volume 59 _journal_year 2003 _space_group_IT_number 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 93.021 _cell_angle_beta 90.616 _cell_angle_gamma 90.319 _cell_length_a 8.7038 _cell_length_b 12.2040 _cell_length_c 4.9747 _exptl_crystal_F_000 204.00 _reflns_d_resolution_high 0.7701 _cod_data_source_file lc0061ethyl98Ksup2.hkl _cod_data_source_block ethyl98K #BEGIN Tags that were not found in dictionaries: _shelx_title ' ethyl98K' _shelx_refln_list_code 4 _shelx_f_calc_maximum 72.38 _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 7.30 4.28 0.33 o 2 0 0 1863.21 1441.14 0.40 o 3 0 0 47.44 49.52 0.48 o 4 0 0 84.91 99.40 0.13 o 5 0 0 182.40 201.55 0.24 o 6 0 0 6.24 5.34 0.16 o 7 0 0 0.56 0.88 0.05 o 8 0 0 29.12 28.72 0.49 o 9 0 0 83.44 89.02 3.50 o 10 0 0 29.15 30.44 0.60 o 11 0 0 1.33 1.92 0.08 o -11 1 0 0.24 0.64 0.02 o -10 1 0 66.52 70.68 1.43 o -9 1 0 11.13 9.99 0.09 o -8 1 0 57.01 50.90 0.11 o -7 1 0 0.52 0.71 0.09 o -6 1 0 7.27 6.46 0.43 o -5 1 0 28.44 30.91 0.32 o -4 1 0 128.42 152.28 1.82 o -2 1 0 733.52 623.67 0.22 o -1 1 0 264.60 255.10 0.11 o 1 1 0 62.36 64.45 0.27 o 2 1 0 918.66 846.80 0.30 o 3 1 0 1208.41 1105.04 5.22 o 4 1 0 14.33 16.23 0.35 o 5 1 0 682.62 748.09 0.83 o 6 1 0 152.35 154.95 2.74 o 7 1 0 6.71 4.33 0.08 o 8 1 0 0.18 0.37 0.16 o 9 1 0 58.63 58.21 2.62 o 10 1 0 6.84 6.65 0.08 o 11 1 0 2.25 2.86 0.32 o -11 2 0 30.13 28.64 0.93 o -10 2 0 3.34 3.99 0.08 o -9 2 0 11.96 12.80 0.10 o -8 2 0 268.32 263.96 2.54 o -7 2 0 317.44 303.65 7.63 o -6 2 0 51.66 54.49 0.15 o -5 2 0 76.83 81.45 0.42 o -4 2 0 58.67 54.46 0.12 o -3 2 0 7.29 6.52 0.04 o -2 2 0 635.96 595.30 0.23 o -1 2 0 216.24 199.41 0.12 o 0 2 0 141.03 153.85 0.75 o 1 2 0 893.50 825.51 0.26 o 2 2 0 1067.44 1108.55 7.15 o 3 2 0 165.98 182.72 0.56 o 4 2 0 114.70 135.47 1.83 o 5 2 0 87.83 108.09 3.14 o 6 2 0 137.45 134.31 7.48 o 7 2 0 1.60 1.17 0.06 o 8 2 0 0.12 0.32 0.05 o 9 2 0 56.20 46.99 0.17 o 10 2 0 0.08 0.45 0.09 o 11 2 0 39.19 46.40 0.18 o -11 3 0 1.13 1.54 0.02 o -10 3 0 13.26 14.25 0.11 o -9 3 0 154.51 149.13 0.36 o -7 3 0 73.10 80.13 3.27 o -6 3 0 247.13 250.05 0.28 o -5 3 0 3.03 4.69 0.07 o -4 3 0 84.24 88.35 0.13 o -3 3 0 295.44 288.01 0.19 o -2 3 0 229.59 244.95 1.82 o -1 3 0 641.40 556.40 10.30 o 0 3 0 385.35 340.90 0.19 o 1 3 0 27.42 30.95 0.84 o 2 3 0 70.74 72.12 0.86 o 3 3 0 400.78 435.37 6.01 o 4 3 0 36.29 37.34 0.83 o 5 3 0 9.69 10.19 0.07 o 6 3 0 0.21 0.71 0.04 o 7 3 0 0.67 0.30 0.16 o 8 3 0 204.90 187.06 7.39 o 9 3 0 30.86 24.88 1.38 o 10 3 0 3.45 3.21 0.35 o 11 3 0 10.31 13.03 0.10 o -10 4 0 9.57 9.87 0.10 o -9 4 0 268.73 268.57 0.51 o -8 4 0 112.26 107.05 0.29 o -7 4 0 8.05 8.29 0.35 o -6 4 0 8.07 7.11 0.08 o -5 4 0 57.14 68.67 0.15 o -4 4 0 478.90 555.43 0.36 o -3 4 0 2.29 1.75 0.05 o -2 4 0 146.60 157.97 1.61 o -1 4 0 62.23 64.52 1.34 o 0 4 0 336.99 349.67 5.85 o 1 4 0 54.45 66.18 0.46 o 2 4 0 32.69 39.63 0.10 o 3 4 0 416.00 439.71 0.47 o 4 4 0 157.00 163.51 4.46 o 5 4 0 0.03 0.07 0.05 o 6 4 0 1.28 1.70 0.06 o 7 4 0 8.26 6.58 0.05 o 8 4 0 16.24 13.77 0.12 o 9 4 0 20.10 18.02 0.13 o 10 4 0 7.15 7.37 0.10 o -10 5 0 38.58 38.23 0.16 o -9 5 0 114.04 121.85 4.27 o -8 5 0 72.44 75.82 0.20 o -7 5 0 8.28 8.30 0.10 o -6 5 0 70.64 75.95 0.18 o -5 5 0 1.61 1.05 0.06 o -4 5 0 388.22 337.23 0.35 o -3 5 0 179.94 184.39 0.28 o -2 5 0 172.69 176.30 3.38 o -1 5 0 34.04 34.62 0.11 o 0 5 0 1168.45 1185.27 7.33 o 1 5 0 83.20 97.42 0.16 o 2 5 0 20.98 20.47 0.14 o 3 5 0 206.09 241.17 1.81 o 4 5 0 0.46 0.66 0.15 o 5 5 0 40.48 44.20 0.22 o 6 5 0 0.83 1.55 0.11 o 7 5 0 224.65 223.01 0.32 o 8 5 0 4.04 4.73 0.10 o 9 5 0 92.14 92.97 1.42 o 10 5 0 19.34 19.49 0.14 o -10 6 0 44.96 51.92 1.71 o -9 6 0 1.66 1.63 0.16 o -8 6 0 5.93 5.49 0.11 o -7 6 0 99.10 105.43 5.81 o -6 6 0 0.73 0.51 0.17 o -5 6 0 48.77 49.51 0.16 o -4 6 0 84.05 90.55 1.60 o -3 6 0 123.25 117.37 0.23 o -2 6 0 19.71 21.49 0.10 o -1 6 0 10.46 10.41 0.09 o 1 6 0 0.39 0.40 0.07 o 2 6 0 622.13 637.12 0.40 o 3 6 0 11.72 12.03 0.17 o 4 6 0 7.78 8.07 0.19 o 5 6 0 120.29 130.38 4.73 o 6 6 0 13.50 10.75 0.12 o 7 6 0 78.04 68.98 0.19 o 8 6 0 25.84 23.83 0.48 o 9 6 0 1.46 2.12 0.13 o 10 6 0 8.42 8.12 0.13 o -10 7 0 5.39 3.95 0.11 o -9 7 0 13.67 12.88 0.96 o -8 7 0 4.86 3.17 0.11 o -7 7 0 40.65 41.84 3.20 o -6 7 0 30.12 28.03 0.16 o -5 7 0 54.42 56.52 0.98 o -4 7 0 2.29 1.79 0.15 o -3 7 0 0.10 0.16 0.14 o -2 7 0 73.16 76.59 0.89 o -1 7 0 8.96 8.24 0.10 o 0 7 0 266.42 261.65 2.92 o 1 7 0 204.83 234.44 0.26 o 2 7 0 0.72 0.87 0.10 o 3 7 0 47.83 51.77 0.47 o 4 7 0 63.20 63.40 2.40 o 5 7 0 6.33 8.60 0.28 o 6 7 0 17.37 15.93 0.50 o 7 7 0 42.88 45.86 1.10 o 8 7 0 0.92 1.09 0.08 o 9 7 0 67.84 65.01 1.24 o 10 7 0 34.22 34.92 0.21 o -9 8 0 0.61 0.39 0.09 o -8 8 0 17.62 21.23 1.49 o -7 8 0 4.38 3.36 0.11 o -6 8 0 110.80 140.23 0.29 o -5 8 0 16.56 13.85 0.95 o -4 8 0 5.94 4.50 0.10 o -3 8 0 7.07 6.88 0.25 o -2 8 0 102.47 107.32 0.65 o -1 8 0 2.34 2.21 0.04 o 0 8 0 636.34 588.40 0.43 o 1 8 0 171.96 170.72 2.25 o 2 8 0 46.15 39.90 0.66 o 3 8 0 2.29 1.83 0.06 o 4 8 0 0.41 0.28 0.11 o 5 8 0 30.05 30.58 0.25 o 6 8 0 134.03 133.96 6.02 o 7 8 0 2.19 2.16 0.08 o 9 8 0 12.47 10.26 0.10 o -9 9 0 0.86 0.72 0.09 o -8 9 0 0.00 -0.07 0.13 o -7 9 0 1.07 1.27 0.08 o -5 9 0 2.86 2.38 0.08 o -4 9 0 30.85 30.86 0.16 o -3 9 0 10.97 10.90 0.49 o -2 9 0 306.08 308.53 2.10 o -1 9 0 151.18 129.30 5.09 o 1 9 0 28.43 30.07 0.61 o 2 9 0 103.44 106.84 3.69 o 3 9 0 408.30 417.82 7.85 o 4 9 0 19.83 21.26 0.67 o 5 9 0 218.73 221.86 4.22 o 6 9 0 13.43 10.92 0.30 o 7 9 0 46.86 45.01 1.75 o 8 9 0 1.00 0.80 0.06 o 9 9 0 1.97 1.25 0.10 o -8 10 0 16.56 15.50 0.78 o -7 10 0 34.30 32.50 0.22 o -6 10 0 20.73 20.09 0.47 o -5 10 0 155.46 158.78 0.42 o -4 10 0 2.83 2.58 0.16 o -3 10 0 25.92 25.45 0.15 o -2 10 0 243.00 238.24 0.29 o -1 10 0 10.89 9.40 0.15 o 0 10 0 0.00 0.24 0.14 o 1 10 0 46.75 44.53 0.34 o 2 10 0 38.12 34.55 1.44 o 3 10 0 557.49 627.61 0.67 o 4 10 0 55.14 60.27 1.40 o 5 10 0 3.38 3.17 0.30 o 6 10 0 27.65 29.18 0.93 o 7 10 0 0.08 0.16 0.06 o 8 10 0 3.91 3.75 0.12 o -8 11 0 22.78 21.49 0.21 o -7 11 0 3.41 3.72 0.43 o -6 11 0 7.59 7.61 0.16 o -4 11 0 3.61 3.69 0.15 o -3 11 0 98.52 103.60 2.50 o -2 11 0 0.16 0.47 0.13 o -1 11 0 15.34 13.18 0.14 o 0 11 0 296.03 290.08 9.68 o 1 11 0 0.39 0.43 0.17 o 2 11 0 26.37 25.42 0.16 o 3 11 0 135.49 127.09 0.35 o 4 11 0 36.87 38.77 0.79 o 5 11 0 18.38 16.27 0.63 o 6 11 0 43.55 43.27 0.92 o 7 11 0 5.68 6.16 0.14 o 8 11 0 3.88 4.01 0.10 o -6 12 0 10.28 10.23 0.19 o -5 12 0 52.87 55.28 1.35 o -4 12 0 67.39 72.24 1.56 o -3 12 0 29.62 29.73 1.40 o -2 12 0 5.19 5.74 0.15 o -1 12 0 9.46 7.72 0.27 o 1 12 0 37.92 37.51 0.21 o 2 12 0 1.47 1.17 0.16 o 3 12 0 26.76 27.30 0.45 o 4 12 0 5.51 7.09 0.53 o 5 12 0 39.26 42.15 2.42 o 6 12 0 0.47 0.56 0.22 o 7 12 0 0.79 0.67 0.16 o -6 13 0 4.38 3.78 0.16 o -5 13 0 36.60 38.15 1.24 o -4 13 0 2.90 3.01 0.24 o -3 13 0 6.03 5.79 0.29 o -2 13 0 6.29 5.87 0.14 o -1 13 0 16.08 16.11 0.40 o 0 13 0 0.06 0.60 0.07 o 1 13 0 42.30 46.86 1.30 o 2 13 0 22.30 21.97 0.28 o 3 13 0 62.92 67.72 0.32 o 4 13 0 0.39 0.43 0.20 o 5 13 0 14.06 14.11 0.64 o 6 13 0 0.67 0.69 0.15 o -5 14 0 108.06 106.51 0.39 o -4 14 0 0.00 0.33 0.12 o -3 14 0 12.16 15.56 0.19 o -2 14 0 0.23 0.21 0.16 o -1 14 0 1.77 1.79 0.14 o 0 14 0 0.60 0.53 0.17 o 1 14 0 18.13 18.91 0.26 o 2 14 0 43.57 46.61 0.88 o 3 14 0 24.30 26.16 0.29 o 4 14 0 0.18 0.45 0.30 o 5 14 0 38.94 41.37 1.69 o -3 15 0 7.63 8.06 0.22 o -2 15 0 9.08 7.64 0.21 o -1 15 0 0.65 0.50 0.19 o 0 15 0 36.73 41.15 0.18 o 1 15 0 10.05 8.70 0.19 o 2 15 0 0.25 0.16 0.12 o 3 15 0 48.14 50.62 0.34 o -3 -15 1 6.02 7.03 0.43 o -2 -15 1 13.31 14.06 0.30 o -1 -15 1 8.85 10.31 0.29 o 0 -15 1 11.86 11.29 0.21 o 1 -15 1 83.90 93.13 0.38 o 2 -15 1 8.73 10.23 0.23 o -5 -14 1 0.80 0.84 0.18 o -4 -14 1 0.06 0.57 0.25 o -3 -14 1 1.85 1.68 0.16 o -2 -14 1 148.41 156.58 1.46 o -1 -14 1 0.00 0.21 0.21 o 0 -14 1 8.97 8.57 0.21 o 3 -14 1 5.90 6.82 0.20 o 4 -14 1 0.05 -0.18 0.18 o 5 -14 1 4.62 5.00 0.20 o -6 -13 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5 -11 1 1.23 1.40 0.14 o 6 -11 1 5.32 6.49 0.17 o 7 -11 1 31.76 31.88 1.99 o 8 -11 1 2.35 2.04 0.14 o -8 -10 1 38.49 38.84 1.06 o -7 -10 1 15.15 14.04 0.62 o -6 -10 1 0.21 0.26 0.06 o -5 -10 1 2.42 1.73 0.11 o -4 -10 1 44.77 45.39 0.18 o -3 -10 1 25.85 22.24 1.16 o -2 -10 1 10.59 12.21 0.13 o -1 -10 1 11.50 7.74 0.11 o 0 -10 1 15.84 14.05 0.16 o 1 -10 1 531.42 517.58 7.53 o 2 -10 1 72.17 72.27 0.14 o 3 -10 1 19.50 17.51 0.17 o 4 -10 1 19.89 20.00 0.16 o 5 -10 1 8.16 7.26 0.33 o 6 -10 1 8.00 9.65 0.17 o 7 -10 1 31.43 33.45 1.88 o 8 -10 1 20.30 20.28 0.23 o -9 -9 1 58.93 55.02 0.25 o -8 -9 1 0.00 0.33 0.11 o -7 -9 1 1.70 1.19 0.17 o -6 -9 1 61.24 61.06 1.56 o -5 -9 1 38.36 35.68 1.00 o -4 -9 1 13.53 13.63 0.59 o -3 -9 1 37.39 39.92 1.39 o -2 -9 1 59.02 56.46 0.19 o -1 -9 1 44.72 38.77 1.76 o 0 -9 1 5.00 5.19 0.09 o 1 -9 1 10.17 13.73 0.72 o 2 -9 1 6.40 6.52 0.28 o 4 -9 1 35.44 31.40 1.47 o 5 -9 1 25.47 26.85 0.62 o 6 -9 1 23.34 19.02 0.21 o 7 -9 1 7.40 8.63 0.14 o 8 -9 1 13.98 13.98 1.18 o 9 -9 1 3.11 3.47 0.27 o -9 -8 1 7.33 8.74 0.12 o -8 -8 1 9.31 9.50 0.12 o -7 -8 1 24.02 21.43 0.47 o -6 -8 1 278.49 285.01 12.98 o -5 -8 1 10.19 10.39 0.10 o -4 -8 1 0.02 0.34 0.29 o -3 -8 1 0.30 0.19 0.09 o -2 -8 1 35.78 36.75 0.35 o -1 -8 1 36.85 34.11 0.13 o 0 -8 1 31.97 33.38 0.88 o 1 -8 1 128.56 128.42 0.25 o 3 -8 1 28.31 29.84 0.14 o 4 -8 1 83.07 85.13 1.36 o 5 -8 1 115.31 102.21 0.30 o 6 -8 1 96.37 101.31 5.34 o 7 -8 1 5.39 5.34 0.59 o -10 -7 1 4.99 5.49 0.12 o -9 -7 1 0.06 0.27 0.17 o -8 -7 1 31.76 27.63 1.21 o -7 -7 1 11.47 8.31 0.23 o -6 -7 1 4.19 2.98 0.34 o -5 -7 1 54.29 54.72 2.53 o -4 -7 1 135.37 134.07 2.25 o -3 -7 1 60.87 60.64 1.52 o -2 -7 1 0.20 0.14 0.06 o -1 -7 1 141.06 139.09 2.21 o 0 -7 1 124.58 122.22 2.92 o 1 -7 1 209.88 208.27 0.34 o 2 -7 1 171.99 173.49 0.24 o 3 -7 1 22.53 25.43 0.13 o 4 -7 1 153.39 151.72 2.33 o 5 -7 1 51.35 57.61 3.62 o 6 -7 1 36.95 31.33 0.20 o 7 -7 1 0.00 0.13 0.11 o 8 -7 1 2.10 2.81 0.12 o 9 -7 1 117.32 122.18 4.15 o 10 -7 1 79.39 77.09 0.27 o -10 -6 1 2.57 1.69 0.04 o -9 -6 1 9.22 8.76 0.38 o -8 -6 1 71.61 64.27 0.57 o -7 -6 1 56.00 55.59 1.47 o -6 -6 1 0.06 0.19 0.10 o -5 -6 1 15.22 14.06 0.44 o -4 -6 1 1.92 3.97 0.51 o -3 -6 1 162.68 169.48 3.06 o -2 -6 1 1034.62 1112.95 21.99 o -1 -6 1 202.39 220.34 0.23 o 0 -6 1 218.39 231.17 0.24 o 1 -6 1 134.54 134.06 0.21 o 2 -6 1 34.31 30.66 0.12 o 3 -6 1 63.99 76.94 1.76 o 5 -6 1 207.45 205.25 6.39 o 6 -6 1 51.46 50.55 0.18 o 8 -6 1 66.99 71.01 0.23 o 9 -6 1 40.30 42.13 0.22 o 10 -6 1 101.44 115.09 4.19 o -10 -5 1 5.83 7.58 0.07 o -9 -5 1 0.24 0.39 0.08 o -8 -5 1 28.72 28.27 0.69 o -7 -5 1 35.08 34.32 0.13 o -6 -5 1 28.53 31.04 0.14 o -5 -5 1 49.41 47.21 0.84 o -4 -5 1 376.38 406.07 10.89 o -3 -5 1 2.42 2.05 0.06 o -2 -5 1 202.92 232.52 2.13 o -1 -5 1 1075.74 1162.92 20.16 o 0 -5 1 4.75 6.03 0.30 o 1 -5 1 297.90 297.19 0.39 o 2 -5 1 64.36 65.01 0.77 o 3 -5 1 390.71 367.48 7.11 o 4 -5 1 71.97 69.74 0.18 o 5 -5 1 5.78 4.24 0.06 o 6 -5 1 4.56 4.16 0.10 o 9 -5 1 40.28 43.45 1.40 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