#------------------------------------------------------------------------------ #$Date: 2020-08-01 08:20:32 +0300 (Sat, 01 Aug 2020) $ #$Revision: 254734 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/87/1558724.cif $ #------------------------------------------------------------------------------ # # 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_1558724 loop_ _publ_author_name 'Wu, Mei-Fang' 'Chen, Ling-Yan' 'Li, Ya' _publ_section_title ; 3-(2,2-Dioxo-3,4-dihydrobenzo[e][1,2,3]oxathiazin-4-yl)-3-fluoro-1-phenylindolin-2-one ; _journal_coeditor_code BT4093 _journal_issue 7 _journal_name_full IUCrData _journal_page_first x201028 _journal_paper_doi 10.1107/S2414314620010287 _journal_volume 5 _journal_year 2020 _chemical_formula_sum 'C21 H15 F N2 O4 S' _chemical_formula_weight 410.41 _chemical_name_systematic 3-(2,2-Dioxo-3,4-dihydrobenzo[e][1,2,3]oxathiazin-4-yl)-3-fluoro-1-phenylindolin-2-one _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens difmap _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 94.6790(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.8726(4) _cell_length_b 15.8054(7) _cell_length_c 11.8345(4) _cell_measurement_reflns_used 3064 _cell_measurement_temperature 292(2) _cell_measurement_theta_max 54.376 _cell_measurement_theta_min 4.876 _cell_volume 1840.51(13) _computing_cell_refinement ; SAINT (Bruker, 2014) ; _computing_data_collection ; APEX2 (Bruker, 2014) ; _computing_data_reduction ; SAINT (Bruker, 2014) ; _computing_molecular_graphics ; SHELXTL (Sheldrick 2008) ; _computing_publication_material ; SHELXTL (Sheldrick 2008) ; _computing_structure_refinement ; SHELXL2014/7 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS97 (Sheldrick 2008) ; _diffrn_ambient_temperature 292(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_unetI/netI 0.0443 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 9057 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.000 _diffrn_reflns_theta_min 2.889 _exptl_absorpt_coefficient_mu 0.218 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6714 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2014) ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.481 _exptl_crystal_description prismatic _exptl_crystal_F_000 848 _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.205 _refine_diff_density_min -0.229 _refine_ls_extinction_coef 0.022(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL-2014/7 (Sheldrick 2014 ; _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 351 _refine_ls_number_reflns 3596 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.077 _refine_ls_R_factor_all 0.0711 _refine_ls_R_factor_gt 0.0439 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+0.4204P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0928 _refine_ls_wR_factor_ref 0.1098 _reflns_number_gt 2580 _reflns_number_total 3596 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file bt4093sup1.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 1558724 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.962 _shelx_estimated_absorpt_t_max 0.979 _shelx_hkl_file ; 2 0 0 2982.60 52.79 -2 0 0 2953.50 52.69 3 0 0 22.90 4.50 -3 0 0 21.80 4.30 4 0 0 9999.00 161.18 -4 0 0 9934.21 161.38 -5 0 0 1977.20 52.79 5 0 0 1906.51 51.59 6 0 0 2.30 3.60 -6 0 0 8.20 4.70 7 0 0 17.60 6.00 -7 0 0 16.10 5.80 8 0 0 3721.33 89.19 -8 0 0 3713.63 95.89 -9 0 0 2.70 4.50 9 0 0 3.80 4.60 -10 0 0 30.80 11.00 10 0 0 29.70 9.10 11 0 0 64.99 13.50 -11 0 0 56.09 14.40 -12 0 0 57.39 16.00 12 0 0 71.59 14.90 -1 1 0 2180.48 34.40 2 -1 0 922.61 22.60 -2 -1 0 906.41 23.50 2 -1 0 873.01 19.90 -2 1 0 811.32 21.30 2 1 0 770.82 26.20 -3 -1 0 266.07 13.80 3 -1 0 277.27 12.10 3 -1 0 263.87 13.10 3 1 0 270.77 13.70 -3 1 0 263.37 13.20 -4 -1 0 509.95 22.50 4 -1 0 467.25 18.70 4 -1 0 476.65 21.00 4 1 0 491.15 21.50 -4 1 0 473.65 20.70 5 -1 0 345.07 17.50 -5 -1 0 316.97 19.10 5 -1 0 335.07 19.00 5 1 0 312.67 18.80 -5 1 0 335.97 19.20 6 -1 0 9.00 4.00 6 -1 0 10.20 4.50 -6 -1 0 7.60 4.20 6 1 0 6.50 3.40 -6 1 0 14.70 5.10 7 -1 0 365.26 21.60 -7 -1 0 344.17 23.80 -7 1 0 342.07 23.30 8 -1 0 12.90 6.40 8 1 0 17.20 6.80 -8 1 0 7.10 4.70 9 -1 0 259.07 21.00 -9 -1 0 255.77 23.70 9 1 0 247.78 21.20 -9 1 0 238.88 22.40 -10 -1 0 17.90 9.50 10 -1 0 14.60 7.20 10 1 0 1.20 6.80 -10 1 0 17.40 7.50 -11 -1 0 9.40 7.50 11 -1 0 22.70 8.30 -11 1 0 16.40 6.20 11 1 0 21.20 8.60 12 -1 0 22.60 8.40 -12 -1 0 -5.20 6.30 12 1 0 0.40 5.00 -1 -2 0 16.60 2.90 1 -2 0 12.80 1.70 -1 2 0 12.40 1.90 1 2 0 13.70 2.90 -2 -2 0 1476.35 33.50 2 -2 0 1535.25 32.50 2 -2 0 1437.86 28.30 2 2 0 1462.05 33.00 -2 2 0 1461.95 29.40 -3 -2 0 2420.16 52.59 3 -2 0 2358.16 45.90 3 -2 0 2479.05 50.99 -3 2 0 2403.26 47.10 3 2 0 2493.55 52.19 -4 -2 0 788.02 29.30 4 -2 0 853.81 25.40 4 -2 0 815.02 28.20 -4 2 0 834.32 28.30 4 2 0 864.51 29.60 5 -2 0 68.39 8.40 5 -2 0 62.09 7.50 -5 -2 0 72.89 9.20 -5 2 0 67.49 8.40 5 2 0 68.09 10.70 6 -2 0 16.90 5.80 6 -2 0 17.10 5.30 -6 -2 0 17.90 5.80 6 2 0 11.50 5.90 -6 2 0 13.40 5.30 -7 -2 0 253.87 20.80 7 -2 0 244.48 17.60 -7 2 0 273.97 20.40 -8 -2 0 1176.98 50.09 8 -2 0 1151.48 42.50 -8 2 0 1186.98 48.50 -9 -2 0 17.60 6.90 9 -2 0 5.70 5.40 9 2 0 4.50 4.00 -9 2 0 8.10 5.30 -10 -2 0 53.59 12.70 10 -2 0 41.60 10.10 10 2 0 31.10 8.80 11 -2 0 -6.40 4.70 -11 -2 0 -1.90 4.60 11 2 0 -6.80 4.30 12 -2 0 79.09 15.50 -12 -2 0 53.09 14.50 12 2 0 76.09 16.00 0 -3 0 2.50 2.10 0 3 0 -0.10 1.60 -2 -3 0 1298.27 32.20 2 -3 0 1260.37 26.00 2 3 0 1327.67 31.90 -2 3 0 1265.07 26.60 3 -3 0 532.25 19.80 3 -3 0 520.75 16.60 -3 -3 0 532.95 21.40 3 3 0 497.35 20.40 -3 3 0 542.45 17.70 4 -3 0 21.30 4.90 4 -3 0 12.70 3.40 -4 -3 0 22.20 5.30 4 3 0 16.10 4.80 -4 3 0 10.40 3.40 5 -3 0 248.98 16.40 5 -3 0 248.18 14.20 -5 -3 0 215.78 17.00 5 3 0 241.58 16.90 -6 -3 0 274.37 20.30 6 -3 0 322.67 20.70 6 -3 0 296.47 18.70 6 3 0 287.57 21.70 7 -3 0 1177.68 39.70 -7 -3 0 1217.68 48.10 8 -3 0 7.20 4.20 -8 -3 0 1.20 3.90 -9 -3 0 299.47 26.00 9 -3 0 288.27 21.90 10 -3 0 -1.70 5.40 -10 -3 0 5.50 6.50 10 3 0 4.90 5.40 -11 -3 0 64.19 15.60 11 -3 0 57.89 12.50 11 3 0 39.60 10.00 12 -3 0 16.50 7.80 -12 -3 0 37.20 12.00 12 3 0 20.80 9.30 0 -4 0 1096.99 25.70 0 4 0 1141.19 24.90 1 -4 0 843.12 19.60 -1 -4 0 869.31 24.10 1 4 0 827.02 23.30 -1 4 0 848.62 19.30 -2 -4 0 129.19 9.60 2 -4 0 120.09 6.80 2 4 0 127.59 9.70 -2 4 0 120.59 6.90 3 -4 0 892.81 23.50 -3 -4 0 940.21 30.50 -3 4 0 971.30 25.50 3 4 0 935.71 29.80 4 -4 0 595.94 20.20 4 -4 0 601.54 24.20 -4 -4 0 601.74 26.60 4 4 0 572.44 25.00 -4 4 0 586.24 21.30 5 -4 0 1206.98 39.80 -5 -4 0 1200.18 42.30 5 -4 0 1226.08 33.90 5 4 0 1156.88 40.20 -5 4 0 1182.28 35.60 6 -4 0 25.60 9.70 -6 -4 0 17.80 6.60 6 -4 0 28.50 7.10 7 -4 0 179.58 14.40 -7 -4 0 186.98 18.50 -8 -4 0 5.20 4.40 8 -4 0 -3.80 2.20 -9 -4 0 111.89 18.20 9 -4 0 106.89 13.00 10 -4 0 1.40 4.50 -10 -4 0 -9.30 5.10 11 -4 0 51.89 11.70 -11 -4 0 46.80 13.80 11 4 0 39.30 12.00 -12 -4 0 -15.70 7.50 12 -4 0 -7.60 4.60 12 4 0 -2.60 5.20 0 -5 0 -0.70 3.30 0 5 0 5.10 3.20 1 -5 0 2455.25 45.50 -1 -5 0 2568.74 51.69 1 5 0 2567.94 50.79 -1 5 0 2520.05 44.90 2 -5 0 2226.58 41.80 -2 -5 0 2262.77 50.29 2 5 0 2242.58 49.70 -2 5 0 2193.78 42.00 3 -5 0 1911.71 39.30 -3 -5 0 1916.81 48.90 3 5 0 1961.00 48.50 -3 5 0 1915.31 40.70 4 -5 0 446.36 21.10 -4 -5 0 425.66 22.50 4 -5 0 473.65 17.90 -4 5 0 460.85 18.80 4 5 0 454.85 22.70 -5 -5 0 1152.98 42.70 5 -5 0 1157.58 32.80 5 -5 0 1108.49 38.80 -5 5 0 1110.49 36.20 5 5 0 1104.49 39.80 6 -5 0 1181.08 36.20 -6 -5 0 1207.98 46.70 6 -5 0 1256.37 44.10 -7 -5 0 1069.39 46.60 7 -5 0 1071.09 36.60 8 -5 0 69.89 11.40 -8 -5 0 111.99 18.40 -9 -5 0 35.30 11.80 9 -5 0 26.20 7.90 -10 -5 0 247.88 26.30 10 -5 0 263.97 21.10 11 -5 0 49.20 10.60 -11 -5 0 49.90 13.30 12 -5 0 42.00 12.10 -12 -5 0 46.90 14.00 12 5 0 43.40 12.40 0 -6 0 225.28 12.70 0 6 0 239.88 11.80 1 -6 0 2711.63 51.89 -1 -6 0 2837.12 57.99 -1 6 0 2767.12 50.49 1 6 0 2799.62 56.19 2 -6 0 147.39 8.90 -2 -6 0 163.18 12.30 2 6 0 153.88 12.10 -2 6 0 155.78 8.80 -3 -6 0 403.86 21.10 3 -6 0 421.46 15.80 3 6 0 418.66 20.90 -3 6 0 410.16 16.30 4 -6 0 341.17 15.40 -4 -6 0 336.47 20.60 -4 6 0 317.67 15.90 4 6 0 339.77 20.30 -5 -6 0 647.84 31.50 5 -6 0 659.83 23.60 5 -6 0 641.84 28.60 -5 6 0 647.74 25.40 5 6 0 638.14 37.60 6 -6 0 -3.90 3.20 -6 -6 0 3.50 3.80 6 -6 0 2.30 2.90 -6 6 0 4.00 3.30 -7 -6 0 32.00 9.80 7 -6 0 38.90 8.50 -8 -6 0 1106.69 51.09 8 -6 0 1007.40 38.30 -9 -6 0 103.89 19.60 9 -6 0 117.19 13.40 10 -6 0 9.80 4.30 -10 -6 0 4.50 6.20 11 -6 0 -10.80 5.20 -11 -6 0 7.80 8.50 12 -6 0 34.90 10.20 -12 -6 0 29.80 11.70 12 6 0 17.00 8.70 0 -7 0 0.00 3.50 0 7 0 0.60 2.80 1 -7 0 2719.83 54.29 -1 -7 0 2758.32 59.99 1 7 0 2772.22 57.59 -1 7 0 2767.92 52.19 -2 -7 0 2600.74 60.19 2 -7 0 2601.84 50.99 -2 7 0 2553.74 50.09 2 7 0 2627.64 59.09 3 -7 0 304.47 14.00 -3 -7 0 315.17 19.10 -3 7 0 291.37 14.00 4 -7 0 582.44 21.20 -4 -7 0 566.14 30.30 4 7 0 589.74 28.00 -4 7 0 573.44 22.20 -5 -7 0 654.93 32.60 5 -7 0 612.64 28.60 5 -7 0 620.74 23.40 -5 7 0 607.94 24.90 -6 -7 0 182.98 18.50 6 -7 0 175.98 13.10 -7 -7 0 65.79 14.00 7 -7 0 77.89 9.80 8 -7 0 274.07 19.20 -8 -7 0 255.87 24.20 9 -7 0 107.49 12.70 -9 -7 0 125.19 20.50 10 -7 0 132.39 15.00 -10 -7 0 97.49 18.70 -11 -7 0 -5.50 5.80 11 -7 0 -6.50 4.50 12 -7 0 24.60 8.50 -12 -7 0 53.39 14.50 0 -8 0 7961.20 132.49 0 8 0 7767.32 125.69 1 -8 0 929.01 28.40 -1 -8 0 894.31 31.40 1 8 0 847.02 28.50 -1 8 0 869.71 25.30 -2 -8 0 182.98 14.90 2 -8 0 191.48 11.90 2 8 0 195.48 15.10 -2 8 0 199.28 11.30 -3 -8 0 205.48 16.30 3 -8 0 225.58 13.00 3 8 0 204.78 17.00 -3 8 0 207.58 12.10 4 -8 0 441.26 18.80 -4 -8 0 453.15 25.60 -4 8 0 399.56 18.70 -5 -8 0 187.58 17.60 5 -8 0 178.68 12.60 -5 8 0 192.88 13.90 -6 -8 0 135.99 15.80 6 -8 0 133.29 11.80 -7 -8 0 13.80 6.40 7 -8 0 15.00 5.20 8 -8 0 39.70 8.80 -8 -8 0 4.00 10.50 -9 -8 0 33.40 10.40 9 -8 0 21.00 6.80 10 -8 0 83.99 13.20 -10 -8 0 74.99 17.60 11 -8 0 28.10 9.10 -11 -8 0 21.30 10.40 0 9 0 36.60 6.50 1 -9 0 1740.83 45.00 -1 -9 0 1721.93 48.50 -1 9 0 1753.92 40.90 -2 -9 0 312.47 20.00 2 -9 0 312.47 16.50 2 9 0 315.47 19.60 -2 9 0 282.17 14.30 -3 -9 0 167.48 15.20 3 -9 0 158.88 11.60 -3 9 0 131.29 10.30 3 9 0 118.19 14.10 4 -9 0 18.10 6.30 -4 -9 0 14.50 6.00 -4 9 0 12.70 4.30 -5 -9 0 663.43 34.70 5 -9 0 648.54 25.20 -6 -9 0 323.47 25.10 6 -9 0 281.97 17.60 -7 -9 0 17.50 7.20 7 -9 0 14.90 5.50 -8 -9 0 25.70 8.80 8 -9 0 16.70 6.30 -9 -9 0 0.10 4.50 10 -9 0 40.00 10.20 -10 -9 0 58.79 14.00 11 -9 0 -2.10 5.40 -11 -9 0 16.90 9.50 0 -10 0 61.79 11.50 0 10 0 54.29 8.60 -1 -10 0 371.46 28.80 1 -10 0 420.16 22.40 -1 10 0 408.16 18.40 1 10 0 417.06 20.80 2 -10 0 66.49 10.60 -2 -10 0 68.49 11.90 2 10 0 72.19 12.00 -2 10 0 61.59 7.30 -3 -10 0 324.17 22.20 -3 10 0 297.47 15.90 -4 -10 0 394.46 25.70 4 -10 0 383.96 19.60 -4 10 0 408.66 20.20 5 -10 0 164.28 13.60 -5 -10 0 171.78 18.20 6 -10 0 60.49 10.30 -6 -10 0 71.79 14.90 7 -10 0 130.49 12.70 -7 -10 0 149.88 26.90 -8 -10 0 -1.10 5.40 8 -10 0 -3.50 3.80 -9 -10 0 5.90 5.40 9 -10 0 12.00 6.00 -10 -10 0 63.39 14.50 10 -10 0 53.49 10.80 11 -10 0 14.50 6.50 -11 -10 0 20.80 8.40 0 -11 0 0.20 6.10 0 11 0 -1.00 3.60 -1 -11 0 165.28 16.30 1 -11 0 182.28 17.30 -1 11 0 175.28 12.80 -2 -11 0 55.49 11.20 2 -11 0 76.39 12.30 -2 11 0 65.59 9.30 3 -11 0 67.29 10.80 -3 -11 0 64.39 13.00 -4 -11 0 152.68 16.60 4 -11 0 136.29 13.20 -5 -11 0 44.90 11.20 5 -11 0 38.80 8.40 -6 -11 0 -0.90 4.70 6 -11 0 -4.30 3.60 -7 -11 0 165.08 19.70 7 -11 0 131.79 13.80 8 -11 0 2.70 3.90 -8 -11 0 -0.60 4.20 9 -11 0 98.89 15.30 -9 -11 0 107.69 20.40 10 -11 0 7.10 5.60 -10 -11 0 24.70 9.90 0 -12 0 415.96 26.40 -1 -12 0 74.79 13.30 1 -12 0 80.89 14.60 -2 -12 0 145.79 16.40 2 -12 0 134.19 15.40 -3 -12 0 886.61 40.50 3 -12 0 876.91 33.80 4 -12 0 9.40 6.20 -4 -12 0 -0.70 3.70 -5 -12 0 58.19 12.90 5 -12 0 51.99 9.70 -6 -12 0 92.69 21.40 6 -12 0 93.79 11.90 -7 -12 0 60.19 14.10 7 -12 0 91.99 11.80 -8 -12 0 276.47 27.10 8 -12 0 294.57 21.00 9 -12 0 -4.90 4.90 -9 -12 0 4.80 5.70 -10 -12 0 -5.40 7.90 10 -12 0 12.50 8.00 0 -13 0 -3.10 7.30 -1 -13 0 7.60 7.70 1 -13 0 3.00 7.70 2 -13 0 161.28 18.40 -2 -13 0 155.68 17.40 -3 -13 0 15.00 7.70 3 -13 0 9.00 7.80 4 -13 0 95.29 14.00 -4 -13 0 102.19 16.90 5 -13 0 14.70 6.30 -5 -13 0 1.10 5.20 -6 -13 0 29.20 9.10 6 -13 0 27.00 9.10 7 -13 0 81.39 13.50 -7 -13 0 98.59 18.50 -8 -13 0 21.90 7.90 9 -13 0 61.99 11.50 -9 -13 0 37.10 12.50 0 -14 0 3008.70 81.59 1 -14 0 130.29 19.00 -1 -14 0 114.89 18.10 2 -14 0 12.50 8.10 -2 -14 0 -6.50 4.60 3 -14 0 19.90 8.80 -3 -14 0 45.50 11.30 4 -14 0 209.38 18.80 -4 -14 0 217.68 21.90 5 -14 0 468.25 27.30 -5 -14 0 491.25 34.70 6 -14 0 -2.40 4.30 7 -14 0 10.00 6.50 -7 -14 0 -2.30 6.00 8 -14 0 62.99 12.50 -8 -14 0 32.70 15.30 9 -14 0 -7.20 6.60 -9 -14 0 22.60 10.40 0 -15 0 -1.10 6.70 1 -15 0 83.99 15.70 -1 -15 0 97.19 17.60 2 -15 0 17.40 9.70 -2 -15 0 27.20 9.80 3 -15 0 52.09 13.10 -3 -15 0 54.49 12.50 4 -15 0 57.89 13.00 -4 -15 0 70.29 15.30 -5 -15 0 41.60 12.20 5 -15 0 36.70 10.40 6 -15 0 2.90 7.00 -6 -15 0 2.30 6.70 -7 -15 0 97.99 19.70 7 -15 0 129.49 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14.70 8.10 6 -15 -3 14.90 8.80 5 -15 -3 11.30 8.10 -5 -15 3 -6.00 5.70 -4 -15 3 159.88 24.00 4 -15 -3 178.28 17.40 -3 -15 3 2.40 7.20 3 -15 -3 17.00 8.20 2 -15 -3 2.80 6.60 -2 -15 3 1.70 7.70 1 -15 -3 9.60 6.80 -1 -15 3 11.00 10.10 0 -15 -3 289.47 21.90 -1 -15 -3 11.90 7.00 -2 -15 -3 3.90 5.50 2 -15 3 5.00 8.00 -3 -15 -3 23.40 9.30 3 -15 3 25.60 10.90 4 -15 3 73.59 15.20 5 -15 3 39.10 10.80 -5 -15 -3 42.80 11.10 6 -15 3 -5.40 6.50 -6 -15 -3 -15.60 6.50 7 -15 3 -6.20 4.70 -7 -15 -3 4.10 6.50 -8 -15 -3 13.30 10.30 8 -15 3 24.20 8.30 -7 -16 3 32.50 13.20 7 -16 -3 59.09 13.00 -6 -16 3 13.90 9.80 6 -16 -3 44.80 11.80 5 -16 -3 7.20 8.20 -5 -16 3 8.20 6.80 4 -16 -3 6.90 8.90 -4 -16 3 0.40 6.90 -3 -16 3 21.20 11.20 3 -16 -3 20.90 10.30 -2 -16 3 43.50 13.20 2 -16 -3 31.60 10.10 -1 -16 3 42.40 12.60 1 -16 -3 28.50 10.10 0 -16 -3 42.30 11.10 0 -16 3 57.99 15.30 -1 -16 -3 5.10 4.40 1 -16 3 -4.90 7.10 -2 -16 -3 18.30 6.80 2 -16 3 24.90 11.30 -3 -16 -3 4.70 9.60 3 -16 3 25.10 10.90 -4 -16 -3 198.18 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13 -0.80 4.10 -2 0 13 0.70 6.30 -2 0 13 3.00 4.90 2 0 -13 1.60 4.00 -1 0 13 -7.70 5.00 -1 0 13 7.30 6.40 1 0 -13 2.90 4.90 0 0 13 -7.30 4.30 1 0 13 -1.30 4.60 2 0 13 3.30 5.00 3 0 13 -3.10 3.80 4 0 13 6.90 4.80 5 0 13 1.10 4.90 -7 -1 13 6.40 6.20 -5 -1 13 67.49 10.30 -5 1 13 67.39 6.80 -4 -1 13 43.00 8.40 -4 1 13 31.60 7.00 -4 1 13 46.50 6.50 -3 1 13 82.69 8.40 -3 1 13 70.89 9.50 3 1 -13 84.99 15.40 2 -1 -13 19.70 4.80 -2 -1 13 25.10 7.90 -2 1 13 19.30 6.30 2 1 -13 21.00 6.00 -2 1 13 19.20 6.80 -1 -1 13 10.20 7.10 1 -1 -13 15.30 7.40 -1 1 13 15.60 6.40 -1 1 13 9.90 6.10 0 -1 13 -5.70 4.70 0 1 13 -7.40 9.70 0 1 13 8.60 5.00 1 -1 13 9.00 5.90 1 1 13 9.60 5.30 2 -1 13 18.20 6.50 2 1 13 11.20 5.90 3 -1 13 -1.10 4.70 3 1 13 0.80 4.40 4 -1 13 9.70 5.80 4 1 13 3.20 4.40 5 -1 13 67.89 12.80 5 1 13 50.59 11.50 -7 -2 13 -10.90 6.80 -6 -2 13 2.40 5.90 -5 -2 13 10.10 5.70 -4 -2 13 29.20 7.80 -3 -2 13 45.60 10.10 -2 -2 13 21.60 8.70 -2 2 13 21.70 5.90 -2 2 13 13.00 4.70 -1 -2 13 -10.80 5.90 -1 2 13 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3 4 13 -0.10 4.20 4 -4 13 49.20 11.50 4 4 13 56.99 9.40 5 -4 13 15.40 8.50 5 4 13 6.60 5.30 -6 -5 13 -11.20 6.70 -5 -5 13 8.60 9.20 -4 -5 13 -8.90 6.30 -3 -5 13 20.60 8.60 -2 -5 13 6.40 8.80 -1 -5 13 71.29 14.60 0 -5 13 2.40 7.50 0 5 13 5.10 5.30 0 5 13 7.10 3.90 1 -5 13 28.40 9.20 1 5 13 25.30 5.30 2 -5 13 8.60 7.40 2 5 13 6.40 3.90 3 -5 13 11.90 6.60 3 5 13 12.80 5.20 4 -5 13 35.10 10.70 4 5 13 30.90 7.60 5 -5 13 13.10 7.30 5 5 13 -3.30 3.90 -6 -6 13 1.20 6.30 -5 -6 13 16.30 12.10 -4 -6 13 32.80 11.80 -3 -6 13 12.20 9.20 -2 -6 13 32.00 12.40 -1 -6 13 9.90 11.30 0 -6 13 70.89 14.10 1 -6 13 120.29 17.80 1 6 13 148.89 9.90 2 -6 13 39.90 11.80 2 6 13 79.69 8.70 3 -6 13 32.40 9.10 3 6 13 26.20 6.40 4 -6 13 26.00 9.70 4 6 13 1.80 4.40 -6 -7 13 14.30 8.40 -5 -7 13 5.90 8.50 -4 -7 13 17.60 9.40 -3 -7 13 5.50 8.90 -2 -7 13 21.60 11.60 -1 -7 13 -0.30 9.60 0 -7 13 0.70 7.70 1 -7 13 -5.80 7.00 1 7 13 -0.20 2.90 2 -7 13 7.10 8.10 3 -7 13 -2.00 6.80 3 7 13 -4.20 4.20 4 -7 13 11.80 7.50 4 7 13 0.10 4.70 -5 -8 13 16.70 10.80 -4 -8 13 143.49 22.00 -3 -8 13 92.59 17.20 -2 -8 13 2.30 7.70 -1 -8 13 15.40 11.70 0 -8 13 41.90 13.30 1 -8 13 74.39 16.30 2 -8 13 16.60 10.30 2 8 13 22.10 5.60 3 -8 13 47.80 12.10 3 8 13 7.90 5.10 -4 -9 13 11.50 10.60 -3 -9 13 8.90 10.80 -2 -9 13 -13.60 7.50 -1 -9 13 -1.20 9.90 0 -9 13 26.10 12.10 1 -9 13 15.90 11.10 2 -9 13 15.30 9.30 -3 -10 13 -9.20 8.80 -2 -10 13 20.10 12.10 -1 -10 13 72.09 18.50 0 -10 13 15.30 11.10 1 -10 13 12.70 10.60 -4 0 14 43.60 7.80 -3 0 14 2.90 5.00 -2 0 14 20.50 10.40 -1 0 14 204.08 16.50 0 0 14 31.10 8.80 1 0 14 2.40 5.80 2 0 14 20.70 7.60 3 0 14 205.68 18.20 4 0 14 231.78 20.00 -5 -1 14 -0.90 5.70 -3 -1 14 6.10 6.00 -3 1 14 8.20 4.40 -2 -1 14 3.00 6.40 -2 1 14 5.60 5.70 -1 -1 14 -0.10 7.00 -1 1 14 0.70 5.50 0 -1 14 11.30 7.50 0 1 14 7.20 6.70 1 -1 14 0.40 6.80 1 1 14 0.50 4.70 2 -1 14 5.30 5.00 2 1 14 17.70 6.90 3 -1 14 4.80 7.20 3 1 14 10.70 6.20 4 -1 14 -3.70 5.40 4 1 14 4.10 6.40 -6 -2 14 9.30 8.20 -5 -2 14 67.09 11.90 -4 -2 14 62.49 10.70 -3 -2 14 8.00 6.80 -2 -2 14 14.60 7.80 -2 2 14 5.60 4.30 -1 -2 14 72.39 13.30 -1 2 14 52.39 9.00 0 -2 14 -13.70 6.40 1 -2 14 4.10 6.80 1 2 14 9.00 5.50 2 -2 14 -4.20 4.90 2 2 14 1.70 4.80 3 -2 14 25.90 8.70 3 2 14 5.00 5.50 4 -2 14 49.00 11.20 4 2 14 54.59 10.50 -5 -3 14 12.90 8.00 -4 -3 14 -2.00 6.10 -3 -3 14 48.70 10.90 -2 -3 14 96.29 15.80 -1 -3 14 14.40 10.80 -1 3 14 25.60 5.80 0 -3 14 149.29 17.10 0 3 14 152.18 12.60 1 -3 14 -3.60 11.20 1 3 14 3.70 4.70 2 -3 14 56.59 12.00 2 3 14 29.00 7.50 3 -3 14 35.70 9.90 3 3 14 40.80 8.70 -5 -4 14 -8.30 7.00 -4 -4 14 11.10 8.40 -2 -4 14 47.80 13.50 -1 -4 14 -7.00 7.90 0 -4 14 -6.80 11.00 0 4 14 -3.10 4.90 1 -4 14 11.50 8.10 2 -4 14 71.39 13.80 2 4 14 78.69 10.70 3 -4 14 19.10 8.00 3 4 14 0.00 5.70 -5 -5 14 -0.80 7.10 -4 -5 14 19.70 8.10 -3 -5 14 177.48 20.10 -2 -5 14 99.49 18.50 -1 -5 14 -7.00 7.70 0 -5 14 27.30 11.50 1 -5 14 86.99 15.80 1 5 14 85.79 9.30 2 -5 14 110.89 17.30 2 5 14 103.59 11.20 3 -5 14 5.40 7.20 3 5 14 0.80 5.50 -4 -6 14 18.80 10.70 -3 -6 14 19.70 10.00 -2 -6 14 14.60 11.00 -1 -6 14 9.90 10.20 0 -6 14 14.10 9.80 1 -6 14 6.30 8.00 2 -6 14 13.40 8.50 2 6 14 7.60 5.00 -3 -7 14 8.90 10.10 -1 -7 14 7.10 10.50 0 -7 14 4.40 9.80 1 -7 14 26.10 10.80 2 -7 14 -17.00 6.80 -2 -8 14 -8.20 9.10 -1 -8 14 10.60 11.10 0 -8 14 -7.20 9.90 -2 0 15 -0.40 10.60 -1 0 15 3.50 6.80 0 0 15 0.30 8.30 1 0 15 5.80 7.10 -3 -1 15 38.40 11.60 -2 -1 15 70.89 13.10 -1 -1 15 67.89 13.50 0 -1 15 20.30 8.80 0 1 15 -6.20 7.20 1 -1 15 42.80 10.90 1 1 15 77.59 12.00 -3 -2 15 -8.10 6.80 -2 -2 15 -3.70 7.70 -1 -2 15 35.70 10.90 0 -2 15 36.00 11.20 0 2 15 39.00 10.20 1 -2 15 24.70 10.20 1 2 15 3.10 7.10 -3 -3 15 25.40 10.60 -2 -3 15 24.70 9.80 -1 -3 15 16.50 10.50 0 -3 15 34.90 14.20 1 -3 15 -2.10 6.80 -2 -4 15 -15.00 7.60 -1 -4 15 27.60 13.20 0 -4 15 30.80 11.80 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 3518 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL mo_dd18258_0m_a.res in P2(1)/c CELL 0.71073 9.8726 15.8054 11.8345 90 94.679 90 ZERR 4 0.0004 0.0007 0.0004 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H F N O S UNIT 84 60 4 8 16 4 OMIT 0 1 1 OMIT 1 1 0 OMIT -3.00 52.00 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 LIST 4 DeLu 0.002 S1' O3 HTAB N2 O1_$1 HTAB N2 O1_$1 EQIV $1 -x+1, -y+1, -z+1 conf htab mpla n1 c1 > c8 mpla c9 > c14 mpla c16 > c21 wpdb -1 size 0.18 0.15 0.10 HTAB N2 O1_$1 TEMP 19 WGHT 0.041900 0.420400 EXTI 0.022431 FVAR 0.91744 0.93264 PART 1 S1 6 0.375463 0.458782 0.175605 21.00000 0.05339 0.07919 = 0.04027 -0.01331 0.00847 -0.02605 O2 5 0.261727 0.391735 0.137066 21.00000 0.05255 0.07123 = 0.05212 -0.02748 0.00624 -0.01686 O4 5 0.335580 0.538766 0.127612 21.00000 0.09941 0.08478 = 0.05462 0.02319 -0.00749 -0.03964 PART 0 O3 5 0.501419 0.425922 0.151295 11.00000 0.05653 0.14816 = 0.07744 -0.04275 0.02526 -0.02428 PART 2 S1' 6 0.379247 0.408712 0.188733 -21.00000 0.09022 0.06508 = 0.08665 -0.01438 0.04217 -0.04492 O2' 5 0.250823 0.452462 0.118040 -21.00000 0.07706 0.09324 = 0.05195 0.01377 -0.00620 0.02861 O4' 5 0.372820 0.327051 0.191293 -21.00000 0.10688 0.04632 = 0.07747 0.00017 0.02541 -0.01525 PART 0 F1 3 0.130325 0.395705 0.515311 11.00000 0.03238 0.05732 = 0.04622 -0.00562 0.00954 0.00192 O1 5 0.402530 0.457846 0.584193 11.00000 0.04400 0.04434 = 0.04492 -0.01360 -0.00323 -0.00354 N1 4 0.450475 0.325721 0.514484 11.00000 0.02844 0.04092 = 0.03871 -0.00555 -0.00170 0.00140 N2 4 0.365003 0.455572 0.310469 11.00000 0.04160 0.04962 = 0.03978 -0.00449 0.00230 -0.01528 C1 1 0.378228 0.265078 0.443514 11.00000 0.03189 0.03790 = 0.03194 -0.00285 0.00272 -0.00370 C2 1 0.420785 0.185200 0.416212 11.00000 0.03703 0.03989 = 0.04576 -0.00133 0.00225 0.00333 C3 1 0.329461 0.136204 0.349561 11.00000 0.05465 0.03434 = 0.05599 -0.00796 -0.00010 0.00235 C4 1 0.201878 0.165958 0.312048 11.00000 0.05229 0.03650 = 0.05854 -0.00911 -0.00935 -0.00450 C5 1 0.161111 0.246757 0.340489 11.00000 0.03577 0.03876 = 0.04736 -0.00375 -0.00611 -0.00270 C6 1 0.251005 0.296457 0.406781 11.00000 0.03096 0.03580 = 0.03625 0.00062 0.00162 -0.00055 C7 1 0.240621 0.384831 0.450118 11.00000 0.02737 0.03677 = 0.03557 -0.00630 0.00389 -0.00014 C8 1 0.372843 0.395412 0.527301 11.00000 0.03151 0.04247 = 0.03023 -0.00342 0.00275 -0.00352 C9 1 0.592301 0.319519 0.550889 11.00000 0.02852 0.04081 = 0.04047 -0.00020 -0.00123 -0.00067 C10 1 0.634566 0.314176 0.663674 11.00000 0.04275 0.07349 = 0.03989 0.00756 -0.00021 0.00078 C11 1 0.772917 0.310518 0.695772 11.00000 0.05279 0.08274 = 0.05110 0.01251 -0.01568 0.00107 C12 1 0.864826 0.310178 0.616462 11.00000 0.03487 0.05438 = 0.07768 0.00567 -0.00868 0.00012 C13 1 0.822018 0.315874 0.503917 11.00000 0.03601 0.07090 = 0.07041 0.00015 0.00944 -0.00163 C14 1 0.684888 0.320879 0.470232 11.00000 0.03845 0.07247 = 0.04256 -0.00093 0.00248 -0.00395 C15 1 0.233245 0.455608 0.360264 11.00000 0.03770 0.03176 = 0.03842 -0.00674 0.00053 -0.00009 C16 1 0.113461 0.444114 0.273488 11.00000 0.03985 0.02890 = 0.04461 0.00121 -0.00579 -0.00127 C17 1 -0.017729 0.459938 0.300550 11.00000 0.04746 0.04196 = 0.06048 0.00081 -0.00465 0.00919 C18 1 -0.128014 0.444037 0.223711 11.00000 0.04410 0.05487 = 0.08696 0.01029 -0.01485 0.00622 C19 1 -0.108190 0.414529 0.117272 11.00000 0.05982 0.06628 = 0.07670 0.01282 -0.03032 -0.01139 C20 1 0.021481 0.399404 0.087066 11.00000 0.07201 0.07206 = 0.05183 -0.00367 -0.01512 -0.01890 C21 1 0.129834 0.413522 0.166275 11.00000 0.04801 0.05236 = 0.04577 -0.00283 -0.00229 -0.01066 H1 2 0.219657 0.506559 0.398669 11.00000 0.03715 H2 2 0.650920 0.324871 0.392996 11.00000 0.05965 H3 2 0.070965 0.266209 0.316089 11.00000 0.04045 H4 2 0.507963 0.165482 0.445315 11.00000 0.04024 H5 2 0.357458 0.080160 0.329344 11.00000 0.04949 H6 2 0.803187 0.307656 0.773555 11.00000 0.07792 H8 2 -0.216871 0.454457 0.244152 11.00000 0.07969 H9 2 0.137342 0.129011 0.266466 11.00000 0.06083 H10 2 0.886630 0.316721 0.446569 11.00000 0.07489 H11 2 0.961810 0.309119 0.642176 11.00000 0.07371 H12 2 0.427222 0.489390 0.346018 11.00000 0.06515 H13 2 -0.183316 0.406580 0.062070 11.00000 0.08957 H14 2 -0.032028 0.481528 0.374474 11.00000 0.06552 H15 2 0.568242 0.315460 0.715891 11.00000 0.06216 H17 2 0.043913 0.377630 0.014711 11.00000 0.07839 HKLF 4 REM mo_dd18258_0m_a.res in P2(1)/c REM R1 = 0.0439 for 2580 Fo > 4sig(Fo) and 0.0711 for all 3596 data REM 351 parameters refined using 1 restraints END WGHT 0.0419 0.4204 REM Instructions for potential hydrogen bonds HTAB N2 O1_$1 REM Highest difference peak 0.205, deepest hole -0.229, 1-sigma level 0.041 Q1 1 0.2365 0.3370 0.4186 11.00000 0.05 0.20 Q2 1 0.4557 0.4662 0.1383 11.00000 0.05 0.16 Q3 1 0.6156 0.3298 0.6060 11.00000 0.05 0.16 Q4 1 0.4768 0.3901 0.1797 11.00000 0.05 0.15 Q5 1 0.1851 0.4032 0.4694 11.00000 0.05 0.15 Q6 1 0.3828 0.1744 0.3670 11.00000 0.05 0.15 Q7 1 0.2228 0.2278 0.2945 11.00000 0.05 0.14 Q8 1 0.1799 0.4191 0.5850 11.00000 0.05 0.14 Q9 1 0.1797 0.4050 0.1551 11.00000 0.05 0.14 Q10 1 0.3883 0.1983 0.4582 11.00000 0.05 0.14 Q11 1 0.3805 0.4669 0.2444 11.00000 0.05 0.14 Q12 1 0.0519 0.4365 0.2931 11.00000 0.05 0.14 Q13 1 0.8436 0.3388 0.5624 11.00000 0.05 0.14 Q14 1 0.4905 0.0965 0.4674 11.00000 0.05 0.14 Q15 1 0.2050 0.2642 0.4172 11.00000 0.05 0.14 Q16 1 0.1290 0.4652 0.1797 11.00000 0.05 0.13 Q17 1 0.2857 0.1703 0.3019 11.00000 0.05 0.13 Q18 1 0.1235 0.4027 0.2406 11.00000 0.05 0.13 Q19 1 0.1574 0.4405 0.3212 11.00000 0.05 0.13 Q20 1 0.1317 0.4689 0.5210 11.00000 0.05 0.13 ; _shelx_res_checksum 11347 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S S1 0.37546(9) 0.45878(11) 0.17560(7) 0.0574(4) Uani d 0.933(4) A 1 O O2 0.2617(2) 0.39173(17) 0.13707(18) 0.0585(7) Uani d 0.933(4) A 1 O O4 0.3356(2) 0.53877(14) 0.12761(16) 0.0804(8) Uani d 0.933(4) A 1 O O3 0.50142(19) 0.42592(16) 0.15129(17) 0.0930(8) Uani d 1 . . S S1' 0.3792(17) 0.4087(16) 0.1887(14) 0.079(5) Uani d 0.067(4) A 2 O O2' 0.251(4) 0.452(3) 0.118(3) 0.075(11) Uani d 0.067(4) A 2 O O4' 0.373(3) 0.3271(18) 0.191(2) 0.076(11) Uani d 0.067(4) A 2 F F1 0.13032(11) 0.39571(8) 0.51531(10) 0.0450(4) Uani d 1 . . O O1 0.40253(15) 0.45785(9) 0.58419(12) 0.0448(4) Uani d 1 . . N N1 0.45048(16) 0.32572(11) 0.51448(13) 0.0363(4) Uani d 1 . . N N2 0.36500(19) 0.45557(12) 0.31047(15) 0.0437(5) Uani d 1 . . C C1 0.37823(19) 0.26508(13) 0.44351(16) 0.0339(5) Uani d 1 . . C C2 0.4208(2) 0.18520(14) 0.41621(18) 0.0410(5) Uani d 1 . . C C3 0.3295(2) 0.13620(15) 0.3496(2) 0.0486(6) Uani d 1 . . C C4 0.2019(3) 0.16596(15) 0.3120(2) 0.0499(6) Uani d 1 . . C C5 0.1611(2) 0.24676(14) 0.34049(18) 0.0412(5) Uani d 1 . . C C6 0.25100(19) 0.29646(13) 0.40678(16) 0.0344(5) Uani d 1 . . C C7 0.24062(19) 0.38483(13) 0.45012(16) 0.0332(5) Uani d 1 . . C C8 0.37284(19) 0.39541(14) 0.52730(16) 0.0347(5) Uani d 1 . . C C9 0.59230(19) 0.31952(13) 0.55089(17) 0.0368(5) Uani d 1 . . C C10 0.6346(2) 0.31418(17) 0.66367(19) 0.0522(6) Uani d 1 . . C C11 0.7729(3) 0.31052(19) 0.6958(2) 0.0633(8) Uani d 1 . . C C12 0.8648(3) 0.31018(17) 0.6165(2) 0.0564(7) Uani d 1 . . C C13 0.8220(2) 0.31587(18) 0.5039(2) 0.0588(7) Uani d 1 . . C C14 0.6849(2) 0.32088(17) 0.4702(2) 0.0512(6) Uani d 1 . . C C15 0.2332(2) 0.45561(14) 0.36026(17) 0.0361(5) Uani d 1 . . C C16 0.1135(2) 0.44411(13) 0.27349(18) 0.0383(5) Uani d 1 . . C C17 -0.0177(2) 0.45994(15) 0.3006(2) 0.0505(6) Uani d 1 . . C C18 -0.1280(3) 0.44404(17) 0.2237(3) 0.0631(8) Uani d 1 . . C C19 -0.1082(3) 0.41453(19) 0.1173(3) 0.0696(8) Uani d 1 . . C C20 0.0215(3) 0.39940(19) 0.0871(2) 0.0664(8) Uani d 1 . . C C21 0.1298(2) 0.41352(15) 0.16628(19) 0.0490(6) Uani d 1 . . H H1 0.2197(19) 0.5066(14) 0.3987(17) 0.037(5) Uiso d 1 . . H H2 0.651(2) 0.3249(15) 0.393(2) 0.060(7) Uiso d 1 . . H H3 0.071(2) 0.2662(13) 0.3161(16) 0.040(6) Uiso d 1 . . H H4 0.508(2) 0.1655(13) 0.4453(16) 0.040(6) Uiso d 1 . . H H5 0.357(2) 0.0802(15) 0.3293(18) 0.049(6) Uiso d 1 . . H H6 0.803(3) 0.3077(17) 0.774(2) 0.078(8) Uiso d 1 . . H H8 -0.217(3) 0.4545(17) 0.244(2) 0.080(9) Uiso d 1 . . H H9 0.137(2) 0.1290(16) 0.266(2) 0.061(7) Uiso d 1 . . H H10 0.887(3) 0.3167(17) 0.447(2) 0.075(8) Uiso d 1 . . H H11 0.962(3) 0.3091(16) 0.642(2) 0.074(8) Uiso d 1 . . H H12 0.427(3) 0.4894(16) 0.346(2) 0.065(8) Uiso d 1 . . H H13 -0.183(3) 0.4066(19) 0.062(2) 0.090(9) Uiso d 1 . . H H14 -0.032(2) 0.4815(16) 0.374(2) 0.066(8) Uiso d 1 . . H H15 0.568(2) 0.3155(15) 0.716(2) 0.062(7) Uiso d 1 . . H H17 0.044(3) 0.3776(17) 0.015(2) 0.078(9) Uiso d 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S1 0.0534(5) 0.0792(9) 0.0403(4) -0.0260(5) 0.0085(3) -0.0133(5) O2 0.0526(13) 0.0712(17) 0.0521(12) -0.0169(13) 0.0062(10) -0.0275(12) O4 0.0994(17) 0.0848(17) 0.0546(12) -0.0396(13) -0.0075(11) 0.0232(11) O3 0.0565(12) 0.148(2) 0.0774(13) -0.0243(13) 0.0253(10) -0.0428(14) S1' 0.090(8) 0.065(12) 0.087(10) -0.045(9) 0.042(8) -0.014(8) O2' 0.08(2) 0.09(3) 0.052(17) 0.03(2) -0.006(14) 0.014(18) O4' 0.11(3) 0.046(18) 0.08(2) -0.015(16) 0.025(17) 0.000(14) F1 0.0324(7) 0.0573(8) 0.0462(7) 0.0019(6) 0.0095(5) -0.0056(6) O1 0.0440(9) 0.0443(9) 0.0449(8) -0.0035(7) -0.0032(7) -0.0136(7) N1 0.0284(9) 0.0409(10) 0.0387(9) 0.0014(8) -0.0017(7) -0.0056(8) N2 0.0416(11) 0.0496(12) 0.0398(10) -0.0153(9) 0.0023(8) -0.0045(9) C1 0.0319(10) 0.0379(12) 0.0319(10) -0.0037(9) 0.0027(8) -0.0028(9) C2 0.0370(12) 0.0399(13) 0.0458(12) 0.0033(10) 0.0023(9) -0.0013(10) C3 0.0546(15) 0.0343(13) 0.0560(14) 0.0024(11) -0.0001(11) -0.0080(11) C4 0.0523(15) 0.0365(13) 0.0585(14) -0.0045(11) -0.0094(11) -0.0091(11) C5 0.0358(12) 0.0388(13) 0.0474(12) -0.0027(10) -0.0061(10) -0.0038(10) C6 0.0310(10) 0.0358(12) 0.0363(10) -0.0006(9) 0.0016(8) 0.0006(9) C7 0.0274(10) 0.0368(12) 0.0356(10) -0.0001(8) 0.0039(8) -0.0063(9) C8 0.0315(11) 0.0425(13) 0.0302(10) -0.0035(9) 0.0027(8) -0.0034(9) C9 0.0285(10) 0.0408(13) 0.0405(11) -0.0007(9) -0.0012(8) -0.0002(10) C10 0.0428(13) 0.0735(18) 0.0399(12) 0.0008(12) -0.0002(10) 0.0076(12) C11 0.0528(16) 0.083(2) 0.0511(15) 0.0011(14) -0.0157(13) 0.0125(15) C12 0.0349(13) 0.0544(16) 0.0777(18) 0.0001(11) -0.0087(12) 0.0057(13) C13 0.0360(13) 0.0709(19) 0.0704(17) -0.0016(12) 0.0094(12) 0.0001(15) C14 0.0384(13) 0.0725(18) 0.0426(13) -0.0039(12) 0.0025(10) -0.0009(12) C15 0.0377(12) 0.0318(12) 0.0384(11) -0.0001(9) 0.0005(9) -0.0067(9) C16 0.0398(12) 0.0289(12) 0.0446(12) -0.0013(9) -0.0058(9) 0.0012(9) C17 0.0475(14) 0.0420(14) 0.0605(16) 0.0092(11) -0.0047(12) 0.0008(12) C18 0.0441(15) 0.0549(17) 0.087(2) 0.0062(13) -0.0149(14) 0.0103(15) C19 0.0598(19) 0.0663(19) 0.077(2) -0.0114(15) -0.0303(16) 0.0128(16) C20 0.072(2) 0.072(2) 0.0518(15) -0.0189(16) -0.0151(14) -0.0037(14) C21 0.0480(14) 0.0524(15) 0.0458(13) -0.0107(11) -0.0023(10) -0.0028(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O3 S1 O4 . . 117.89(16) ? O3 S1 O2 . . 108.28(17) ? O4 S1 O2 . . 108.17(16) ? O3 S1 N2 . . 108.81(13) ? O4 S1 N2 . . 112.62(14) ? O2 S1 N2 . . 99.39(13) ? C21 O2 S1 . . 114.28(18) ? O4' S1' O3 . . 105(2) ? O4' S1' O2' . . 114(3) ? O3 S1' O2' . . 115(2) ? O4' S1' N2 . . 115.1(18) ? O3 S1' N2 . . 110.0(11) ? O2' S1' N2 . . 98.2(19) ? C21 O2' S1' . . 104(2) ? C8 N1 C1 . . 110.56(16) ? C8 N1 C9 . . 124.62(17) ? C1 N1 C9 . . 124.05(16) ? C15 N2 S1 . . 121.86(15) ? C15 N2 S1' . . 119.7(6) ? C15 N2 H12 . . 114.1(17) ? S1 N2 H12 . . 110.6(17) ? S1' N2 H12 . . 125.5(18) ? C2 C1 C6 . . 122.69(19) ? C2 C1 N1 . . 127.34(18) ? C6 C1 N1 . . 109.93(17) ? C1 C2 C3 . . 116.7(2) ? C1 C2 H4 . . 119.9(12) ? C3 C2 H4 . . 123.3(12) ? C4 C3 C2 . . 121.7(2) ? C4 C3 H5 . . 120.3(13) ? C2 C3 H5 . . 117.9(13) ? C3 C4 C5 . . 120.6(2) ? C3 C4 H9 . . 120.2(14) ? C5 C4 H9 . . 119.2(14) ? C6 C5 C4 . . 118.4(2) ? C6 C5 H3 . . 121.6(12) ? C4 C5 H3 . . 120.0(12) ? C5 C6 C1 . . 119.89(19) ? C5 C6 C7 . . 131.90(19) ? C1 C6 C7 . . 108.20(17) ? F1 C7 C6 . . 112.54(15) ? F1 C7 C8 . . 108.70(14) ? C6 C7 C8 . . 103.09(16) ? F1 C7 C15 . . 107.28(15) ? C6 C7 C15 . . 116.26(16) ? C8 C7 C15 . . 108.69(16) ? O1 C8 N1 . . 127.38(18) ? O1 C8 C7 . . 124.78(18) ? N1 C8 C7 . . 107.73(16) ? C10 C9 C14 . . 120.7(2) ? C10 C9 N1 . . 120.65(18) ? C14 C9 N1 . . 118.59(18) ? C9 C10 C11 . . 119.0(2) ? C9 C10 H15 . . 117.9(15) ? C11 C10 H15 . . 123.1(15) ? C12 C11 C10 . . 120.6(2) ? C12 C11 H6 . . 119.8(16) ? C10 C11 H6 . . 119.6(16) ? C11 C12 C13 . . 120.2(2) ? C11 C12 H11 . . 118.4(15) ? C13 C12 H11 . . 121.3(15) ? C12 C13 C14 . . 120.2(2) ? C12 C13 H10 . . 121.0(16) ? C14 C13 H10 . . 118.9(16) ? C9 C14 C13 . . 119.3(2) ? C9 C14 H2 . . 117.8(14) ? C13 C14 H2 . . 122.8(14) ? N2 C15 C16 . . 113.32(17) ? N2 C15 C7 . . 106.41(16) ? C16 C15 C7 . . 111.82(17) ? N2 C15 H1 . . 111.1(12) ? C16 C15 H1 . . 107.3(12) ? C7 C15 H1 . . 106.8(12) ? C21 C16 C17 . . 117.3(2) ? C21 C16 C15 . . 121.5(2) ? C17 C16 C15 . . 121.1(2) ? C16 C17 C18 . . 121.1(3) ? C16 C17 H14 . . 119.1(15) ? C18 C17 H14 . . 119.8(15) ? C19 C18 C17 . . 120.1(3) ? C19 C18 H8 . . 120.0(18) ? C17 C18 H8 . . 119.9(18) ? C18 C19 C20 . . 120.2(3) ? C18 C19 H13 . . 120.7(18) ? C20 C19 H13 . . 119.0(18) ? C19 C20 C21 . . 118.7(3) ? C19 C20 H17 . . 125.3(16) ? C21 C20 H17 . . 116.0(16) ? C16 C21 C20 . . 122.6(2) ? C16 C21 O2 . . 119.2(2) ? C20 C21 O2 . . 118.1(2) ? C16 C21 O2' . . 111.3(15) ? C20 C21 O2' . . 113.9(12) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S1 O3 . 1.399(2) ? S1 O4 . 1.428(3) ? S1 O2 . 1.584(2) ? S1 N2 . 1.6086(19) ? O2 C21 . 1.417(3) ? O3 S1' . 1.346(14) ? S1' O4' . 1.29(4) ? S1' O2' . 1.62(4) ? S1' N2 . 1.636(16) ? O2' C21 . 1.50(4) ? F1 C7 . 1.396(2) ? O1 C8 . 1.217(2) ? N1 C8 . 1.357(3) ? N1 C1 . 1.427(2) ? N1 C9 . 1.434(2) ? N2 C15 . 1.471(3) ? N2 H12 . 0.89(3) ? C1 C2 . 1.377(3) ? C1 C6 . 1.387(3) ? C2 C3 . 1.385(3) ? C2 H4 . 0.95(2) ? C3 C4 . 1.383(3) ? C3 H5 . 0.96(2) ? C4 C5 . 1.389(3) ? C4 H9 . 0.99(2) ? C5 C6 . 1.381(3) ? C5 H3 . 0.96(2) ? C6 C7 . 1.494(3) ? C7 C8 . 1.540(3) ? C7 C15 . 1.541(3) ? C9 C10 . 1.368(3) ? C9 C14 . 1.375(3) ? C10 C11 . 1.389(3) ? C10 H15 . 0.94(2) ? C11 C12 . 1.358(4) ? C11 H6 . 0.95(3) ? C12 C13 . 1.367(4) ? C12 H11 . 0.98(3) ? C13 C14 . 1.382(3) ? C13 H10 . 0.97(3) ? C14 H2 . 0.95(2) ? C15 C16 . 1.513(3) ? C15 H1 . 0.94(2) ? C16 C21 . 1.380(3) ? C16 C17 . 1.382(3) ? C17 C18 . 1.383(3) ? C17 H14 . 0.96(3) ? C18 C19 . 1.372(4) ? C18 H8 . 0.94(3) ? C19 C20 . 1.378(4) ? C19 H13 . 0.96(3) ? C20 C21 . 1.382(3) ? C20 H17 . 0.97(3) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N2 H12 O1 3_666 0.89(3) 1.99(3) 2.868(2) 166(2) loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag O3 S1 O2 C21 . . . . 174.48(19) ? O4 S1 O2 C21 . . . . -56.7(2) ? N2 S1 O2 C21 . . . . 61.0(3) ? O4' S1' O2' C21 . . . . 51(3) ? O3 S1' O2' C21 . . . . 172.2(14) ? N2 S1' O2' C21 . . . . -71(3) ? O3 S1 N2 C15 . . . . -157.38(18) ? O4 S1 N2 C15 . . . . 70.0(2) ? O2 S1 N2 C15 . . . . -44.3(2) ? O4' S1' N2 C15 . . . . -70(2) ? O3 S1' N2 C15 . . . . 171.6(11) ? O2' S1' N2 C15 . . . . 51(2) ? C8 N1 C1 C2 . . . . -176.2(2) ? C9 N1 C1 C2 . . . . 13.4(3) ? C8 N1 C1 C6 . . . . 1.3(2) ? C9 N1 C1 C6 . . . . -169.02(17) ? C6 C1 C2 C3 . . . . -0.2(3) ? N1 C1 C2 C3 . . . . 177.03(19) ? C1 C2 C3 C4 . . . . 0.1(3) ? C2 C3 C4 C5 . . . . 0.0(4) ? C3 C4 C5 C6 . . . . 0.1(3) ? C4 C5 C6 C1 . . . . -0.2(3) ? C4 C5 C6 C7 . . . . 178.8(2) ? C2 C1 C6 C5 . . . . 0.3(3) ? N1 C1 C6 C5 . . . . -177.37(18) ? C2 C1 C6 C7 . . . . -178.93(18) ? N1 C1 C6 C7 . . . . 3.4(2) ? C5 C6 C7 F1 . . . . 57.8(3) ? C1 C6 C7 F1 . . . . -123.05(17) ? C5 C6 C7 C8 . . . . 174.7(2) ? C1 C6 C7 C8 . . . . -6.1(2) ? C5 C6 C7 C15 . . . . -66.5(3) ? C1 C6 C7 C15 . . . . 112.66(19) ? C1 N1 C8 O1 . . . . 178.27(19) ? C9 N1 C8 O1 . . . . -11.5(3) ? C1 N1 C8 C7 . . . . -5.3(2) ? C9 N1 C8 C7 . . . . 165.00(16) ? F1 C7 C8 O1 . . . . -56.9(2) ? C6 C7 C8 O1 . . . . -176.50(18) ? C15 C7 C8 O1 . . . . 59.6(2) ? F1 C7 C8 N1 . . . . 126.54(17) ? C6 C7 C8 N1 . . . . 6.9(2) ? C15 C7 C8 N1 . . . . -117.00(18) ? C8 N1 C9 C10 . . . . 72.0(3) ? C1 N1 C9 C10 . . . . -119.0(2) ? C8 N1 C9 C14 . . . . -106.6(2) ? C1 N1 C9 C14 . . . . 62.4(3) ? C14 C9 C10 C11 . . . . 0.3(4) ? N1 C9 C10 C11 . . . . -178.3(2) ? C9 C10 C11 C12 . . . . -1.6(4) ? C10 C11 C12 C13 . . . . 1.9(4) ? C11 C12 C13 C14 . . . . -0.9(4) ? C10 C9 C14 C13 . . . . 0.7(4) ? N1 C9 C14 C13 . . . . 179.3(2) ? C12 C13 C14 C9 . . . . -0.4(4) ? S1 N2 C15 C16 . . . . 9.7(3) ? S1' N2 C15 C16 . . . . -23.9(11) ? S1 N2 C15 C7 . . . . 132.95(18) ? S1' N2 C15 C7 . . . . 99.4(11) ? F1 C7 C15 N2 . . . . 167.10(15) ? C6 C7 C15 N2 . . . . -66.0(2) ? C8 C7 C15 N2 . . . . 49.7(2) ? F1 C7 C15 C16 . . . . -68.7(2) ? C6 C7 C15 C16 . . . . 58.3(2) ? C8 C7 C15 C16 . . . . 173.96(16) ? N2 C15 C16 C21 . . . . 16.9(3) ? C7 C15 C16 C21 . . . . -103.4(2) ? N2 C15 C16 C17 . . . . -166.4(2) ? C7 C15 C16 C17 . . . . 73.3(3) ? C21 C16 C17 C18 . . . . 1.3(4) ? C15 C16 C17 C18 . . . . -175.6(2) ? C16 C17 C18 C19 . . . . -2.1(4) ? C17 C18 C19 C20 . . . . 1.0(4) ? C18 C19 C20 C21 . . . . 0.8(4) ? C17 C16 C21 C20 . . . . 0.6(4) ? C15 C16 C21 C20 . . . . 177.4(2) ? C17 C16 C21 O2 . . . . -176.3(2) ? C15 C16 C21 O2 . . . . 0.5(3) ? C17 C16 C21 O2' . . . . 140.5(14) ? C15 C16 C21 O2' . . . . -42.6(14) ? C19 C20 C21 C16 . . . . -1.6(4) ? C19 C20 C21 O2 . . . . 175.3(3) ? C19 C20 C21 O2' . . . . -140.6(17) ? S1 O2 C21 C16 . . . . -44.5(3) ? S1 O2 C21 C20 . . . . 138.4(2) ? S1' O2' C21 C16 . . . . 73(2) ? S1' O2' C21 C20 . . . . -143.7(16) ? _cod_database_fobs_code 1558724