#------------------------------------------------------------------------------ #$Date: 2022-09-07 04:48:42 +0300 (Wed, 07 Sep 2022) $ #$Revision: 277702 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/41/2244158.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_2244158 loop_ _publ_author_name 'Schinke, Jascha' 'Gelbrich, Thomas' 'Griesser, Ulrich J.' _publ_section_title ; Crystal structure, PIXEL calculations of intermolecular interaction energies and solid-state characterization of the herbicide isoxaflutole ; _journal_coeditor_code WM5659 _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first ; ; _journal_paper_doi 10.1107/S2056989022008647 _journal_volume 78 _journal_year 2022 _chemical_formula_iupac 'C15 H12 F3 N O4 S' _chemical_formula_moiety 'C15 H12 F3 N O4 S' _chemical_formula_sum 'C15 H12 F3 N O4 S' _chemical_formula_weight 359.32 _chemical_name_common isoxaflutole _chemical_name_systematic ; (5-Cyclopropyl-1,2-oxazol-4-yl)[2-(methylsulfonyl)-4-(trifluoromethyl)\ phenyl]methanone ; _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 geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/6 _cell_angle_alpha 90 _cell_angle_beta 118.530(15) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.5689(16) _cell_length_b 9.2906(8) _cell_length_c 13.4358(15) _cell_measurement_reflns_used 2902 _cell_measurement_temperature 193(2) _cell_measurement_theta_max 29.8150 _cell_measurement_theta_min 5.0110 _cell_volume 1488.1(3) _computing_cell_refinement ; CrysAlisPro (Rigaku OD, 2020) ; _computing_data_collection ; CrysAlisPro (Rigaku OD, 2020) ; _computing_data_reduction ; CrysAlisPro (Rigaku OD, 2020) ; _computing_molecular_graphics ; XP (Bruker, 1998) and Mercury (Macrae et al., 2020) ; _computing_publication_material ; PLATON (Spek, 2020) and publCIF Westrip (2010) ; _computing_structure_refinement ; SHELXL (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 193(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.3575 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_unetI/netI 0.0385 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 9962 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.103 _diffrn_reflns_theta_min 2.780 _diffrn_source 'fine-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.273 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.92448 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2020) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.604 _exptl_crystal_description prism _exptl_crystal_F_000 736 _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.080 _refine_diff_density_max 0.309 _refine_diff_density_min -0.354 _refine_ls_extinction_coef 0.0203(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_hydrogen_treatment refU _refine_ls_matrix_type full _refine_ls_number_parameters 231 _refine_ls_number_reflns 3275 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.016 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0381 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+0.6729P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0890 _refine_ls_wR_factor_ref 0.0973 _reflns_number_gt 2667 _reflns_number_total 3275 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file wm5659sup1.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2244158 _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 0.935 _shelx_estimated_absorpt_t_max 0.978 _shelx_hkl_file ; -2 0 0 1002.90 24.83 -3 0 0 3742.67 83.70 -4 0 0 2865.71 67.72 -5 0 0 46.41 5.91 -6 0 0 158.34 10.21 -6 0 0 135.11 6.79 -7 0 0 544.96 22.51 -7 0 0 539.13 17.05 8 0 0 193.86 13.01 -8 0 0 191.90 12.99 -8 0 0 162.68 8.58 -9 0 0 114.40 10.73 9 0 0 131.23 11.18 -9 0 0 104.92 6.91 -10 0 0 374.23 21.57 -10 0 0 414.20 15.79 -11 0 0 1296.71 48.17 -11 0 0 1419.33 38.29 -12 0 0 66.30 9.77 -13 0 0 5.04 4.41 -14 0 0 116.75 14.16 -15 0 0 401.93 27.58 1 1 0 863.22 19.65 -2 -1 0 53.47 4.02 -3 -1 0 172.79 8.51 -3 1 0 162.13 7.91 -4 1 0 354.38 14.00 -4 -1 0 381.94 15.00 -5 -1 0 109.13 8.68 -5 1 0 113.45 8.23 -6 1 0 174.91 10.95 -6 -1 0 180.02 11.48 -7 1 0 2093.52 57.34 -7 -1 0 2144.31 58.72 -8 1 0 467.22 22.02 8 1 0 504.10 22.71 -8 -1 0 480.27 22.57 8 -1 0 563.11 23.76 9 -1 0 894.88 33.52 -9 1 0 785.06 31.86 -9 -1 0 820.54 32.86 -9 -1 0 843.62 27.24 -10 -1 0 54.52 8.53 -10 1 0 37.02 6.84 -10 -1 0 45.78 5.39 -11 1 0 510.23 25.78 -11 -1 0 544.82 27.22 -12 -1 0 15.69 5.91 -12 1 0 18.62 5.30 -13 -1 0 99.67 12.42 -13 1 0 84.70 11.30 -14 -1 0 171.76 17.18 -14 1 0 162.91 16.52 -15 -1 0 12.47 4.50 -15 1 0 21.10 7.20 0 -2 0 858.65 22.24 -1 -2 0 1378.53 33.90 -2 -2 0 6022.04 117.74 2 -2 0 6067.01 116.67 2 2 0 5891.74 113.88 3 -2 0 1268.85 33.86 -3 -2 0 1347.26 35.34 -3 -2 0 1311.08 31.62 -4 -2 0 56.25 6.25 -5 -2 0 316.91 15.02 -6 -2 0 126.84 9.90 7 -2 0 1485.08 43.78 -7 -2 0 1414.94 45.10 -8 2 0 1289.17 43.51 -8 -2 0 1382.46 45.96 8 2 0 1476.10 46.01 8 -2 0 1577.25 46.10 9 -2 0 756.75 30.14 -9 2 0 657.24 28.63 -9 -2 0 732.85 30.93 -10 -2 0 825.52 35.15 -10 2 0 798.30 33.45 -10 -2 0 877.91 30.40 -11 2 0 232.46 17.03 -11 -2 0 242.50 18.42 -11 -2 0 258.34 14.91 -12 -2 0 51.27 9.15 -12 -2 0 55.85 6.95 -13 -2 0 122.58 14.12 -14 -2 0 3.91 3.62 -15 -2 0 31.10 8.25 0 -3 0 2.86 2.69 -1 -3 0 528.18 17.70 -2 -3 0 10.36 3.35 -2 3 0 8.48 2.49 2 3 0 9.84 2.02 -3 -3 0 11.45 3.46 3 3 0 11.07 2.06 -3 -3 0 12.75 2.11 3 -3 0 9.13 3.66 4 -3 0 368.28 15.66 -4 -3 0 400.32 16.78 -4 -3 0 388.21 13.31 -5 -3 0 220.60 13.32 5 -3 0 243.39 12.37 5 -3 0 213.61 11.81 -5 -3 0 239.08 10.39 -6 -3 0 247.92 14.50 -6 -3 0 245.11 11.45 -7 -3 0 645.16 26.83 7 -3 0 674.88 25.68 -7 -3 0 598.92 21.79 8 -3 0 64.88 7.76 -8 -3 0 68.72 8.62 -9 -3 0 14.70 5.08 -10 -3 0 362.67 22.28 -11 -3 0 373.61 23.79 -12 -3 0 31.35 7.64 -13 -3 0 5.02 5.41 -14 -3 0 58.60 10.50 -15 -3 0 41.71 9.60 -15 -3 0 53.15 8.48 0 -4 0 3699.96 86.42 -1 -4 0 185.29 10.41 -2 -4 0 564.02 20.81 -2 4 0 581.28 19.88 2 4 0 532.88 16.85 -3 -4 0 2223.55 57.46 -3 4 0 2284.29 56.44 3 4 0 2132.10 51.81 4 -4 0 198.31 11.62 -4 -4 0 210.21 12.64 -5 -4 0 700.05 26.53 5 -4 0 695.25 24.99 -5 -4 0 676.33 21.22 6 -4 0 223.29 13.55 6 -4 0 241.22 13.94 -6 -4 0 250.61 15.09 -6 -4 0 235.90 11.17 7 4 0 107.92 10.07 7 -4 0 87.09 8.63 -7 -4 0 90.68 9.65 7 -4 0 113.15 9.81 -7 -4 0 89.70 7.17 8 -4 0 7.84 4.17 8 -4 0 6.94 3.20 -8 -4 0 -2.76 3.83 -9 -4 0 86.15 10.69 9 -4 0 96.38 10.19 -10 -4 0 168.60 15.51 10 -4 0 156.16 13.55 -10 -4 0 190.00 12.54 -11 -4 0 69.89 10.72 -11 -4 0 82.02 8.63 -12 -4 0 1.06 3.82 -12 -4 0 1.37 2.19 -13 -4 0 -3.73 5.17 -13 -4 0 -4.15 3.12 -14 -4 0 114.88 15.11 14 -4 0 105.56 13.20 -14 -4 0 112.40 11.58 15 -4 0 -7.08 5.66 0 -5 0 -2.89 2.66 -1 -5 0 17.42 4.43 -1 5 0 19.63 3.86 -2 5 0 444.37 18.06 -2 -5 0 407.56 18.34 2 5 0 390.37 14.53 -3 5 0 29.65 4.81 -3 -5 0 23.73 4.64 3 5 0 24.00 3.23 -4 -5 0 491.65 21.59 4 5 0 473.39 16.59 -5 -5 0 106.27 10.12 5 -5 0 117.69 9.70 5 5 0 120.49 10.48 -6 -5 0 62.64 8.25 6 -5 0 63.11 7.33 -6 -5 0 55.67 5.32 6 -5 0 53.69 7.02 -7 -5 0 29.37 6.50 7 -5 0 25.29 4.90 -7 -5 0 26.49 3.90 7 -5 0 26.63 5.25 8 -5 0 109.08 10.74 -8 -5 0 100.63 11.53 9 -5 0 248.35 17.20 -9 -5 0 249.36 18.57 10 -5 0 0.94 4.16 -10 -5 0 4.00 4.80 -10 -5 0 0.95 2.17 11 -5 0 -2.20 3.91 -11 -5 0 3.89 3.81 -11 -5 0 -4.81 3.66 12 -5 0 185.05 16.65 -12 -5 0 203.83 19.14 -12 -5 0 167.84 12.79 13 -5 0 3.89 4.41 -13 -5 0 12.07 5.69 -13 -5 0 4.63 2.90 14 -5 0 248.12 21.02 -14 -5 0 219.74 21.21 0 -6 0 14.25 4.16 -1 -6 0 56.91 7.10 1 -6 0 58.70 6.90 -1 6 0 61.33 6.99 -2 6 0 72.17 7.63 -2 -6 0 66.49 7.83 2 6 0 62.94 5.61 -3 6 0 211.60 13.15 -3 -6 0 186.05 13.03 3 6 0 188.32 13.04 3 6 0 182.19 9.87 4 6 0 12.70 3.77 -4 6 0 5.19 2.52 -4 -6 0 10.64 4.78 4 6 0 11.57 2.57 -5 -6 0 702.09 29.60 -6 -6 0 346.58 19.98 6 -6 0 314.87 18.35 -7 -6 0 5.30 4.20 7 -6 0 -0.12 3.70 7 -6 0 0.54 0.89 -8 -6 0 68.15 9.84 8 -6 0 58.03 8.37 -9 -6 0 10.87 4.62 9 -6 0 6.51 3.67 -10 -6 0 5.99 3.95 10 -6 0 7.62 3.80 -10 -6 0 9.43 3.24 -11 -6 0 123.58 14.68 11 -6 0 100.73 12.31 -11 -6 0 113.19 9.82 -12 -6 0 23.73 7.73 12 -6 0 22.27 6.88 -13 -6 0 203.40 20.15 13 -6 0 163.12 16.56 14 -6 0 61.87 10.66 0 -7 0 -2.55 2.97 1 -7 0 153.19 12.08 -1 -7 0 152.61 12.23 -1 7 0 177.55 12.57 -2 -7 0 20.75 5.00 2 -7 0 18.58 4.91 -2 7 0 25.78 4.93 2 7 0 16.58 3.33 -3 -7 0 39.43 6.71 -3 7 0 43.96 2.67 -3 7 0 39.60 6.19 3 7 0 35.93 4.61 -3 7 0 41.62 2.60 -3 -7 0 41.49 2.68 -3 -7 0 41.40 2.70 -4 -7 0 671.22 29.30 4 7 0 697.63 23.70 -5 -7 0 18.55 5.28 -6 -7 0 483.68 25.86 -7 -7 0 337.00 21.39 7 -7 0 324.28 12.87 -8 -7 0 110.05 12.87 8 -7 0 122.58 5.19 -9 -7 0 46.17 9.29 9 -7 0 48.63 8.43 -10 -7 0 23.35 6.55 10 -7 0 22.93 6.14 -11 -7 0 282.10 23.08 11 -7 0 264.69 20.31 -12 -7 0 132.50 16.47 12 -7 0 120.16 14.14 13 -7 0 4.02 3.35 0 -8 0 345.81 20.12 -1 -8 0 62.98 8.69 1 -8 0 52.34 7.57 -2 -8 0 660.28 29.91 2 -8 0 643.09 28.40 2 8 0 662.40 24.25 -3 -8 0 681.23 30.62 3 8 0 670.75 24.47 -4 -8 0 215.35 16.63 -4 8 0 250.73 8.49 4 8 0 182.60 11.60 -4 -8 0 255.68 8.71 -4 -8 0 248.86 8.75 -4 8 0 248.48 8.46 -5 -8 0 311.69 20.49 5 8 0 253.81 13.34 -6 -8 0 23.73 6.14 -7 -8 0 2.63 3.78 -8 -8 0 86.71 11.80 -9 -8 0 18.62 6.20 -10 -8 0 3.82 4.68 -11 -8 0 16.03 6.82 12 -8 0 1.65 3.87 0 -9 0 0.63 2.98 -1 -9 0 31.16 6.85 1 -9 0 22.56 5.54 2 -9 0 32.79 6.49 -2 -9 0 35.27 7.40 2 9 0 39.63 5.68 3 -9 0 244.13 17.87 -3 -9 0 263.43 19.31 3 9 0 302.44 15.58 -4 -9 0 196.75 16.74 -5 -9 0 80.22 11.24 -6 -9 0 294.78 21.80 -7 -9 0 43.02 8.63 -8 -9 0 13.00 6.72 -9 -9 0 257.68 21.83 -10 -9 0 -1.81 4.56 0 -10 0 84.17 11.18 -1 -10 0 24.32 6.29 1 -10 0 27.10 6.58 2 -10 0 485.49 27.25 -2 -10 0 479.43 27.90 -3 -10 0 33.08 8.37 3 -10 0 26.19 6.43 4 -10 0 -1.08 3.02 -4 -10 0 10.70 5.74 -5 -10 0 112.01 13.81 5 -10 0 120.08 13.15 -6 -10 0 60.44 10.47 -7 -10 0 36.21 8.55 -8 -10 0 234.11 21.02 0 -11 0 -4.79 4.06 1 -11 0 210.32 18.35 -1 -11 0 198.16 18.39 -2 -11 0 9.87 5.66 2 -11 0 0.95 4.01 -3 -11 0 9.50 5.52 3 -11 0 14.59 5.73 4 -11 0 2.08 3.61 -4 -11 0 1.58 3.65 5 -11 0 7.24 4.90 -5 -11 0 -3.10 6.04 6 -11 0 10.41 5.13 -6 -11 0 12.77 6.31 0 -12 0 375.35 26.68 -1 -12 0 60.37 10.97 1 -12 0 59.92 10.57 -2 -12 0 104.55 14.00 2 -12 0 123.49 14.72 3 -12 0 101.40 13.50 4 -12 0 2.61 3.75 -16 0 1 0.56 3.62 -15 0 1 -4.01 4.69 -14 0 1 0.07 3.82 -13 0 1 -3.18 3.95 -12 0 1 -1.85 3.45 -11 0 1 0.47 3.47 -10 0 1 5.37 4.51 -10 0 1 -0.05 1.54 -9 0 1 2.39 3.38 9 0 -1 -0.42 2.20 -9 0 1 0.53 1.36 -8 0 1 0.33 3.16 -8 0 1 -0.61 1.31 -7 0 1 -3.18 3.30 -7 0 1 0.60 1.25 -6 0 1 -4.04 4.19 -6 0 1 -0.94 1.58 -5 0 1 -2.46 3.71 -5 0 1 0.69 1.56 -4 0 1 1.13 2.88 -4 0 1 1.92 1.48 -3 0 1 1.20 2.34 -3 0 1 -0.92 1.33 -2 0 1 -0.39 1.05 -1 0 -1 7.25 1.47 -2 0 -1 0.81 1.98 -3 0 -1 -2.03 2.80 -4 0 -1 -0.34 2.76 5 0 1 0.56 1.71 -5 0 -1 -0.52 2.89 -6 0 -1 0.98 3.03 7 0 1 1.52 2.39 -7 0 -1 -2.86 3.28 8 0 1 -1.08 1.73 -8 0 -1 -1.44 2.85 -9 0 -1 3.49 3.48 -9 0 -1 -0.18 1.49 -10 0 -1 -0.92 3.11 -10 0 -1 -1.22 1.61 -11 0 -1 3.64 3.91 -11 0 -1 -0.74 1.26 -12 0 -1 2.51 3.35 -13 0 -1 -0.76 3.77 -14 0 -1 10.28 5.55 -15 0 -1 -6.88 4.97 -16 -1 1 16.95 6.15 -16 1 1 13.15 4.64 -15 -1 1 293.72 23.71 -15 1 1 254.01 21.59 -14 -1 1 19.58 6.46 -14 1 1 18.82 6.67 -13 1 1 26.90 6.65 -13 -1 1 34.29 8.28 -12 -1 1 25.70 6.56 -12 1 1 10.49 4.18 -12 -1 1 13.82 3.24 -11 -1 1 22.62 6.24 -11 1 1 16.53 4.62 -11 -1 1 26.47 4.37 -10 1 1 178.40 13.90 -10 -1 1 184.97 14.45 -10 -1 1 183.88 10.90 9 1 -1 88.43 9.20 -9 -1 1 69.01 8.59 -9 1 1 64.10 8.30 9 -1 -1 92.05 9.44 -9 -1 1 76.66 6.63 -8 -1 1 78.90 8.26 -8 1 1 74.36 7.90 8 -1 -1 97.15 9.03 -8 -1 1 81.03 6.51 -7 -1 1 78.71 8.08 -7 1 1 75.34 8.11 -7 -1 1 85.46 6.46 -6 -1 1 6409.28 144.75 -6 1 1 6310.47 143.67 -6 -1 1 6367.22 140.08 -5 1 1 69.71 6.49 -5 -1 1 73.46 6.78 -4 -1 1 3142.63 73.43 -4 1 1 3048.38 72.39 4 -1 -1 3127.09 67.07 -3 -1 1 992.27 26.83 -1 -1 -1 238.03 8.18 1 1 1 224.85 7.95 -2 1 -1 336.95 11.05 -2 -1 -1 359.47 12.01 -3 -1 -1 380.80 14.09 -3 1 -1 384.94 13.39 -4 -1 -1 36.97 5.01 -4 1 -1 36.92 4.58 4 -1 1 34.37 3.99 -5 1 -1 20.54 4.03 5 -1 1 19.52 3.42 -5 -1 -1 24.77 4.65 -6 1 -1 125.52 9.29 -6 -1 -1 130.17 9.96 -6 1 -1 130.39 4.93 -7 1 -1 31.13 5.46 7 -1 1 35.31 5.10 7 1 1 30.02 4.90 -7 -1 -1 32.73 5.68 -7 1 -1 28.38 2.30 -8 1 -1 381.16 19.15 8 1 1 369.98 19.11 8 -1 1 410.68 19.92 -8 -1 -1 374.16 19.83 -8 1 -1 381.44 11.43 -9 1 -1 154.20 12.76 -9 -1 -1 151.73 13.08 -10 -1 -1 353.24 20.97 -10 1 -1 315.10 19.44 -10 -1 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1 -8 70.71 8.20 -2 1 -8 138.68 6.40 -2 -1 -8 140.75 8.84 2 -1 8 135.90 6.20 2 1 8 126.60 8.14 -2 -1 -8 128.39 11.85 -3 1 -8 63.33 5.02 -3 -1 -8 74.36 6.99 3 1 8 49.47 5.34 3 -1 8 58.14 4.65 -3 -1 -8 51.40 7.55 -4 1 -8 68.45 5.93 -4 -1 -8 60.55 6.84 4 -1 8 61.32 5.50 -4 -1 -8 64.08 8.83 -5 1 -8 341.47 15.50 -5 -1 -8 341.73 17.56 5 1 8 323.35 16.74 -5 -1 -8 327.43 21.44 -6 1 -8 147.08 10.40 -6 -1 -8 131.38 11.28 6 1 8 153.99 11.68 6 -1 8 150.98 10.41 -6 -1 -8 141.10 14.13 -7 1 -8 46.24 6.31 -7 -1 -8 43.43 6.84 -7 -1 -8 36.75 8.23 -8 1 -8 175.09 13.12 -8 -1 -8 177.82 14.16 -8 -1 -8 162.48 16.62 -9 -1 -8 0.44 2.49 -9 -1 -8 3.85 3.88 -17 -2 8 214.29 20.75 -17 2 8 225.92 21.09 -17 -2 8 211.71 20.25 -16 -2 8 -0.39 3.73 -16 2 8 1.72 4.63 -16 -2 8 0.60 4.76 -15 -2 8 230.89 19.72 -15 2 8 215.71 18.97 -15 -2 8 218.63 19.23 -14 -2 8 -0.83 3.59 -14 2 8 -2.97 4.31 -14 -2 8 3.17 4.23 14 -2 -8 1.67 2.22 -13 -2 8 355.84 22.75 -13 2 8 340.02 22.01 -13 -2 8 392.62 23.59 13 -2 -8 346.62 18.71 -12 -2 8 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56.13 -5 2 8 2079.97 56.00 -5 -2 8 1957.23 55.40 -5 2 8 1948.26 55.35 4 2 -8 1.10 1.07 -4 -2 8 0.35 3.13 -4 2 8 -3.89 3.20 4 2 -8 2.38 2.76 -4 2 8 0.28 1.92 4 2 -8 0.02 1.54 4 2 -8 -3.13 2.53 4 -2 -8 1.02 2.25 -3 2 8 11.97 2.47 -3 -2 8 4.96 3.28 -3 2 8 10.58 3.37 3 2 -8 12.13 3.33 3 2 -8 11.58 2.76 -3 2 8 13.81 4.02 -2 2 8 1897.12 49.30 2 -2 -8 1891.58 49.09 -2 -2 8 1938.82 54.35 2 2 -8 1904.88 52.03 -2 2 8 1947.19 54.26 2 -2 -8 1823.92 53.99 -2 2 8 2142.00 56.34 1 -2 -8 29.74 4.08 1 2 -8 39.30 5.70 1 -2 -8 31.09 5.32 -1 2 8 35.46 5.65 1 -2 -8 30.12 5.16 -1 2 8 28.00 5.38 -1 -2 8 31.17 5.24 -1 2 8 32.62 3.99 1 2 -8 31.91 4.69 0 -2 -8 141.62 9.01 0 2 -8 135.43 10.87 0 -2 -8 141.62 11.24 0 -2 -8 123.13 10.83 -1 -2 -8 333.30 15.21 -1 2 -8 380.67 19.57 -1 -2 -8 361.77 19.33 -1 -2 -8 337.34 18.99 2 -2 8 101.27 4.16 2 -2 8 100.95 4.15 -2 -2 -8 101.21 8.15 -2 -2 -8 88.82 9.90 -3 -2 -8 512.97 21.66 3 -2 8 527.01 16.00 3 2 8 497.36 20.79 3 -2 8 546.02 16.25 -3 -2 -8 502.26 25.51 4 -2 8 7.25 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1 16 16.27 6.12 13 -1 -16 31.36 8.49 12 1 -16 90.18 13.36 -12 -1 16 69.31 11.52 -12 1 16 92.99 13.15 12 -1 -16 88.68 13.43 11 1 -16 0.97 3.44 -11 -1 16 4.55 4.66 -10 -1 16 191.62 18.24 -10 1 16 181.45 18.47 10 1 -16 168.06 18.07 9 1 -16 20.34 7.51 -9 -1 16 12.00 3.94 -9 1 16 17.26 6.88 -8 -1 16 249.93 20.94 -8 1 16 246.90 21.23 8 1 -16 250.69 21.39 7 1 -16 123.33 15.33 -7 -1 16 127.16 15.23 -7 1 16 111.16 13.99 6 1 -16 1.37 4.17 -6 1 16 -1.76 4.91 -5 -1 16 61.12 10.76 -5 1 16 54.91 9.63 4 1 -16 35.89 8.30 3 -1 -16 55.71 10.20 3 1 -16 49.81 9.74 2 -1 -16 105.01 13.79 2 1 -16 85.88 12.60 1 1 -16 4.34 4.68 16 -2 -16 111.02 13.98 15 -2 -16 1.98 4.41 14 -2 -16 177.52 16.38 13 -2 -16 108.48 12.40 -13 -2 16 142.14 16.30 -13 2 16 119.91 15.11 13 -2 -16 114.24 14.96 12 2 -16 23.99 7.95 -12 -2 16 16.18 6.74 -12 2 16 3.31 4.02 -11 -2 16 232.77 20.71 -11 2 16 204.69 19.37 11 2 -16 218.24 20.56 10 2 -16 51.06 10.44 -10 -2 16 51.15 9.69 -10 2 16 45.08 9.19 9 2 -16 83.94 12.32 -9 -2 16 67.95 10.72 -9 2 16 76.94 12.37 8 2 -16 85.83 12.36 -8 -2 16 96.31 12.95 -8 2 16 92.39 12.71 7 2 -16 7.09 5.96 -7 -2 16 -13.48 6.94 -7 2 16 -15.10 7.27 6 2 -16 89.88 12.50 -6 -2 16 60.21 10.75 -6 2 16 79.68 11.52 5 2 -16 21.81 5.68 5 2 -16 18.31 6.17 4 2 -16 46.46 8.49 4 2 -16 36.68 7.64 3 2 -16 8.55 3.47 3 2 -16 19.27 6.69 2 2 -16 8.79 4.24 2 2 -16 14.37 5.74 1 2 -16 44.77 8.40 1 2 -16 43.44 9.89 15 -3 -16 31.59 7.36 14 -3 -16 5.11 4.47 -12 -3 16 35.76 8.70 -12 3 16 66.82 11.16 11 3 -16 32.36 7.68 -11 -3 16 35.26 8.91 -11 3 16 35.40 8.58 -10 -3 16 225.22 20.22 -10 3 16 223.93 20.11 10 3 -16 266.08 22.57 9 3 -16 126.97 15.33 -9 -3 16 108.58 13.99 -9 3 16 114.81 14.20 8 3 -16 9.68 4.87 -8 -3 16 1.98 5.23 -8 3 16 13.81 5.53 -7 -3 16 256.92 21.88 -7 3 16 282.22 22.36 7 3 -16 295.82 23.45 6 3 -16 0.97 4.33 -6 -3 16 -0.59 4.66 -6 3 16 11.90 5.39 5 3 -16 152.38 14.33 5 3 -16 235.63 20.26 4 3 -16 147.12 14.75 4 3 -16 162.27 16.88 3 3 -16 104.83 13.02 3 3 -16 80.09 11.13 2 3 -16 53.35 9.56 2 3 -16 63.09 10.98 1 3 -16 10.84 5.74 1 3 -16 5.24 5.19 -12 -4 16 62.41 10.91 -12 4 16 60.08 11.03 -11 4 16 136.15 15.95 -11 -4 16 129.68 15.47 -10 -4 16 28.70 7.56 -10 4 16 10.88 5.98 10 4 -16 11.16 5.51 -9 -4 16 52.75 9.74 -9 4 16 54.17 10.14 9 4 -16 63.00 11.21 -8 -4 16 104.85 13.65 -8 4 16 77.36 11.71 8 4 -16 93.71 12.94 7 4 -16 18.72 6.98 -7 -4 16 34.89 8.03 -7 4 16 27.11 7.52 6 4 -16 74.21 12.01 -6 -4 16 72.16 11.56 -6 4 16 75.01 11.67 5 4 -16 199.95 16.12 5 4 -16 195.11 18.70 4 4 -16 46.06 9.10 4 4 -16 36.59 7.43 3 4 -16 33.77 8.29 3 4 -16 34.87 7.56 2 4 -16 57.28 9.60 2 4 -16 61.53 10.13 1 4 -16 6.77 3.33 -11 -5 16 5.07 5.24 -11 5 16 1.98 3.66 -10 -5 16 52.46 9.48 -10 5 16 44.65 9.52 -9 -5 16 111.62 14.29 -9 5 16 124.90 14.95 -8 -5 16 22.05 6.47 -8 5 16 8.71 4.58 8 5 -16 18.77 7.01 -7 -5 16 85.84 12.62 -7 5 16 75.26 11.47 7 5 -16 99.47 13.71 6 5 -16 17.13 6.63 5 5 -16 217.18 20.04 4 5 -16 20.90 5.76 3 5 -16 107.91 13.69 -11 6 16 -4.32 3.45 -10 6 16 155.96 16.78 -10 -6 16 144.80 16.10 9 -6 -16 9.89 4.69 -9 -6 16 1.32 3.64 -9 6 16 8.18 3.44 -8 -6 16 27.16 7.98 -8 6 16 23.77 6.93 -7 -6 16 5.35 4.63 -7 6 16 10.56 5.72 5 6 -16 26.93 8.54 4 6 -16 5.54 3.82 -10 7 16 9.19 5.17 9 -7 -16 -2.55 3.33 -9 7 16 -5.99 5.01 -8 -7 16 16.68 6.45 -8 7 16 23.24 7.20 -10 0 17 4.35 4.02 10 0 -17 2.59 5.70 -9 0 17 1.90 5.51 9 0 -17 -7.57 5.86 -8 0 17 -4.46 6.11 -7 0 17 1.32 4.37 -6 0 17 1.52 3.83 3 0 -17 0.65 3.82 10 1 -17 2.18 3.58 -10 -1 17 5.87 4.54 -10 1 17 7.55 5.79 9 1 -17 -6.16 5.23 -9 -1 17 0.87 4.30 -9 1 17 6.39 6.32 8 1 -17 4.11 5.49 -8 -1 17 8.63 5.99 -8 1 17 13.62 6.53 7 1 -17 5.89 5.55 -7 -1 17 4.64 5.16 -7 1 17 -10.96 6.59 6 1 -17 -6.90 4.93 -6 -1 17 -8.55 6.20 -6 1 17 -7.78 4.90 5 1 -17 5.58 4.65 4 1 -17 -3.03 3.63 3 1 -17 -3.69 4.28 -10 -2 17 63.74 11.52 -10 2 17 55.57 10.96 9 2 -17 11.37 5.93 -9 -2 17 1.73 4.09 -9 2 17 6.86 4.98 8 2 -17 -6.86 5.13 -8 -2 17 -1.42 3.84 -8 2 17 -4.69 4.45 7 2 -17 4.52 5.95 -7 -2 17 2.81 4.40 6 2 -17 1.86 4.03 5 2 -17 47.64 8.83 5 2 -17 37.23 8.42 4 2 -17 39.25 8.73 4 2 -17 33.80 7.45 3 2 -17 9.85 3.57 3 2 -17 18.44 6.88 2 2 -17 22.03 6.23 -9 3 17 2.83 5.60 -8 -3 17 8.62 6.17 -8 3 17 -2.16 3.71 7 3 -17 13.04 6.31 6 3 -17 11.26 5.55 5 3 -17 5.82 3.81 5 3 -17 6.41 3.32 4 3 -17 8.97 3.74 4 3 -17 7.21 3.36 3 3 -17 5.63 2.24 3 3 -17 3.09 2.99 2 3 -17 -2.03 2.67 5 4 -17 14.87 6.21 4 4 -17 35.26 8.03 3 4 -17 15.06 5.33 TITL exp_4135 in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 0.71073 13.568938 9.290623 13.435787 90.0000 118.5299 90.0000 ZERR 6.00 0.001581 0.000794 0.001512 0.0000 0.0147 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O UNIT 66.00 60.00 6.00 6.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 95879 _shelx_res_file ; REM colourless prism watch glass ACN TITL s92_a.res in P2(1)/c REM Old TITL exp_4135 in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.156, Rweak 0.217, Alpha 0.029, Orientation as input REM Formula found by SHELXT: C16 N O3 F3 S CELL 0.71073 13.5689 9.2906 13.4358 90.000 118.530 90.000 ZERR 4.000 0.0016 0.0008 0.0015 0.000 0.015 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N O F S UNIT 60 48 4 16 12 4 SHEL 999 .78 OMIT 1 0 2 OMIT 2 0 2 ACTA TEMP -80 SIZE .25 .1 .08 HTAB L.S. 10 BOND $H LIST 4 FMAP 2 PLAN 20 WGHT 0.042800 0.672900 EXTI 0.020263 FVAR 0.74859 O1 4 0.248201 0.731411 0.029683 11.00000 0.02106 0.04004 = 0.02486 0.00671 0.00927 0.00340 N2 3 0.326927 0.757719 -0.010320 11.00000 0.02955 0.03866 = 0.02570 0.00414 0.01500 -0.00102 C3 1 0.421440 0.710702 0.069256 11.00000 0.02323 0.03016 = 0.02605 0.00039 0.01333 -0.00309 AFIX 43 H3 2 0.489849 0.715795 0.066157 11.00000 0.03313 AFIX 0 C4 1 0.412529 0.650389 0.162199 11.00000 0.01847 0.02462 = 0.02291 -0.00073 0.01062 -0.00391 C5 1 0.301376 0.667710 0.131499 11.00000 0.01984 0.02433 = 0.02136 0.00019 0.00813 -0.00089 C6 1 0.498241 0.582256 0.264999 11.00000 0.01879 0.02954 = 0.02486 0.00160 0.01101 -0.00232 O7 4 0.477729 0.524421 0.334177 11.00000 0.02450 0.06004 = 0.03685 0.02065 0.01620 0.00133 C8 1 0.233893 0.631103 0.185622 11.00000 0.01913 0.03739 = 0.02989 0.00320 0.01289 -0.00011 AFIX 13 H8 2 0.276345 0.612066 0.268928 11.00000 0.05077 AFIX 0 C9 1 0.119285 0.695576 0.142810 11.00000 0.02698 0.03782 = 0.05278 0.00058 0.02592 0.00474 AFIX 23 H9A 2 0.094108 0.718258 0.199107 11.00000 0.04691 H9B 2 0.093029 0.763680 0.078485 11.00000 0.06080 AFIX 0 C10 1 0.129278 0.542596 0.119895 11.00000 0.02964 0.03756 = 0.05471 -0.00720 0.02632 -0.00765 AFIX 23 H10A 2 0.109430 0.515201 0.041326 11.00000 0.04986 H10B 2 0.110509 0.469765 0.161986 11.00000 0.05892 AFIX 0 C11 1 0.616436 0.582083 0.281077 11.00000 0.01758 0.02431 = 0.02299 0.00541 0.00986 0.00032 C12 1 0.706542 0.651486 0.371096 11.00000 0.01807 0.02017 = 0.02067 0.00196 0.00996 0.00155 C13 1 0.812860 0.649647 0.380422 11.00000 0.01714 0.02132 = 0.02075 0.00044 0.00762 -0.00032 AFIX 43 H13 2 0.872920 0.699182 0.440800 11.00000 0.02354 AFIX 0 C14 1 0.831088 0.575240 0.301286 11.00000 0.01926 0.02101 = 0.02348 0.00419 0.01180 0.00236 C15 1 0.744231 0.502313 0.213884 11.00000 0.02625 0.02310 = 0.02351 -0.00077 0.01400 0.00005 AFIX 43 H15 2 0.757377 0.449063 0.161001 11.00000 0.03481 AFIX 0 C16 1 0.637621 0.507227 0.203712 11.00000 0.02274 0.02811 = 0.02398 -0.00437 0.00970 -0.00608 AFIX 43 H16 2 0.577816 0.458389 0.142565 11.00000 0.03137 AFIX 0 S17 6 0.692369 0.747776 0.478051 11.00000 0.02548 0.02439 = 0.02444 0.00053 0.01593 0.00307 O18 4 0.788777 0.838332 0.533215 11.00000 0.04501 0.04211 = 0.03883 -0.01738 0.02798 -0.01535 C19 1 0.945976 0.580198 0.310811 11.00000 0.02378 0.02843 = 0.02961 0.00295 0.01638 0.00238 F20 5 1.025310 0.536418 0.412373 11.00000 0.01927 0.08886 = 0.03625 0.01434 0.01116 0.01013 O21 4 0.583324 0.812580 0.428680 11.00000 0.03781 0.04112 = 0.04140 0.01092 0.02517 0.02007 C22 1 0.699822 0.614533 0.573699 11.00000 0.04111 0.03703 = 0.02633 0.00819 0.01906 0.00689 AFIX 137 H22A 2 0.771362 0.563214 0.602573 11.00000 0.04802 H22B 2 0.637801 0.546456 0.535065 11.00000 0.05715 H22C 2 0.694471 0.659405 0.636958 11.00000 0.04582 AFIX 0 F23 5 0.955590 0.497643 0.235364 11.00000 0.03576 0.04548 = 0.04970 -0.00833 0.03060 0.00459 F24 5 0.973897 0.713181 0.297201 11.00000 0.04363 0.03266 = 0.08444 -0.00001 0.04714 -0.00679 HKLF 4 REM s92_a.res in P2(1)/c REM R1 = 0.0381 for 2667 Fo > 4sig(Fo) and 0.0502 for all 3275 data REM 231 parameters refined using 0 restraints END WGHT 0.0424 0.6814 REM Instructions for potential hydrogen bonds HTAB C8 O7 HTAB C22 O7 REM Highest difference peak 0.309, deepest hole -0.354, 1-sigma level 0.067 Q1 1 0.4249 0.7129 0.1373 11.00000 0.05 0.31 Q2 1 0.6973 0.6857 0.4186 11.00000 0.05 0.30 Q3 1 0.3642 0.6706 0.1672 11.00000 0.05 0.26 Q4 1 0.8792 0.5796 0.3078 11.00000 0.05 0.25 Q5 1 0.7324 0.8482 0.4801 11.00000 0.05 0.24 Q6 1 0.4538 0.6394 0.2075 11.00000 0.05 0.22 Q7 1 0.2629 0.6435 0.1541 11.00000 0.05 0.22 Q8 1 0.6922 0.6794 0.5290 11.00000 0.05 0.22 Q9 1 0.6554 0.6422 0.3240 11.00000 0.05 0.22 Q10 1 0.7603 0.6154 0.3881 11.00000 0.05 0.21 Q11 1 0.5585 0.6061 0.2669 11.00000 0.05 0.20 Q12 1 1.0328 0.5258 0.4600 11.00000 0.05 0.20 Q13 1 0.9071 0.8077 0.2133 11.00000 0.05 0.20 Q14 1 0.1194 0.4967 -0.0041 11.00000 0.05 0.19 Q15 1 0.6265 0.7943 0.4348 11.00000 0.05 0.19 Q16 1 0.1012 0.3397 0.2126 11.00000 0.05 0.18 Q17 1 1.0285 0.6364 0.4060 11.00000 0.05 0.18 Q18 1 0.5981 0.7610 0.3078 11.00000 0.05 0.18 Q19 1 0.8141 0.6431 0.3159 11.00000 0.05 0.18 Q20 1 0.1545 0.2971 0.1900 11.00000 0.05 0.18 ; _shelx_res_checksum 15822 _shelxl_version_number 2014/6 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 O O1 0.24820(10) 0.73141(14) 0.02968(10) 0.0294(3) Uani d 1 . . N N2 0.32693(13) 0.75772(18) -0.01032(12) 0.0306(4) Uani d 1 . . C C3 0.42144(15) 0.7107(2) 0.06926(14) 0.0258(4) Uani d 1 . . H H3 0.4898 0.7158 0.0662 0.033(5) Uiso calc 1 . . C C4 0.41253(14) 0.65039(18) 0.16220(13) 0.0217(4) Uani d 1 . . C C5 0.30138(14) 0.66771(19) 0.13150(13) 0.0225(4) Uani d 1 . . C C6 0.49824(14) 0.58226(19) 0.26500(14) 0.0242(4) Uani d 1 . . O O7 0.47773(11) 0.52442(17) 0.33418(11) 0.0398(4) Uani d 1 . . C C8 0.23389(15) 0.6311(2) 0.18562(15) 0.0283(4) Uani d 1 . . H H8 0.2763 0.6121 0.2689 0.051(6) Uiso calc 1 . . C C9 0.11929(16) 0.6956(2) 0.14281(18) 0.0364(5) Uani d 1 . . H H9A 0.0941 0.7183 0.1991 0.047(6) Uiso calc 1 . . H H9B 0.0930 0.7637 0.0785 0.061(8) Uiso calc 1 . . C C10 0.12928(17) 0.5426(2) 0.11990(19) 0.0381(5) Uani d 1 . . H H10A 0.1094 0.5152 0.0413 0.050(7) Uiso calc 1 . . H H10B 0.1105 0.4698 0.1620 0.059(7) Uiso calc 1 . . C C11 0.61644(14) 0.58208(18) 0.28108(13) 0.0216(4) Uani d 1 . . C C12 0.70654(13) 0.65149(18) 0.37110(13) 0.0193(3) Uani d 1 . . C C13 0.81286(13) 0.64965(18) 0.38042(13) 0.0203(3) Uani d 1 . . H H13 0.8729 0.6992 0.4408 0.024(5) Uiso calc 1 . . C C14 0.83109(14) 0.57524(18) 0.30129(13) 0.0206(3) Uani d 1 . . C C15 0.74423(14) 0.50231(18) 0.21388(14) 0.0234(4) Uani d 1 . . H H15 0.7574 0.4491 0.1610 0.035(5) Uiso calc 1 . . C C16 0.63762(14) 0.50723(19) 0.20371(14) 0.0255(4) Uani d 1 . . H H16 0.5778 0.4584 0.1426 0.031(5) Uiso calc 1 . . S S17 0.69237(4) 0.74778(5) 0.47805(3) 0.02312(14) Uani d 1 . . O O18 0.78878(12) 0.83833(16) 0.53321(11) 0.0387(4) Uani d 1 . . C C19 0.94598(15) 0.5802(2) 0.31081(14) 0.0258(4) Uani d 1 . . F F20 1.02531(9) 0.53642(16) 0.41237(10) 0.0490(4) Uani d 1 . . O O21 0.58332(12) 0.81258(15) 0.42868(11) 0.0375(4) Uani d 1 . . C C22 0.69982(18) 0.6145(2) 0.57370(15) 0.0336(4) Uani d 1 . . H H22A 0.7714 0.5632 0.6026 0.048(7) Uiso calc 1 . . H H22B 0.6378 0.5465 0.5351 0.057(7) Uiso calc 1 . . H H22C 0.6945 0.6594 0.6370 0.046(6) Uiso calc 1 . . F F23 0.95559(9) 0.49764(13) 0.23536(10) 0.0394(3) Uani d 1 . . F F24 0.97390(10) 0.71318(13) 0.29720(12) 0.0467(3) Uani 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 O1 0.0211(7) 0.0400(8) 0.0249(6) 0.0034(5) 0.0093(5) 0.0067(5) N2 0.0295(9) 0.0387(10) 0.0257(7) -0.0010(7) 0.0150(7) 0.0041(6) C3 0.0232(9) 0.0302(10) 0.0261(8) -0.0031(7) 0.0133(7) 0.0004(7) C4 0.0185(8) 0.0246(9) 0.0229(8) -0.0039(7) 0.0106(7) -0.0007(7) C5 0.0198(8) 0.0243(9) 0.0214(8) -0.0009(7) 0.0081(7) 0.0002(7) C6 0.0188(8) 0.0295(10) 0.0249(8) -0.0023(7) 0.0110(7) 0.0016(7) O7 0.0245(7) 0.0600(10) 0.0369(7) 0.0013(7) 0.0162(6) 0.0207(7) C8 0.0191(9) 0.0374(11) 0.0299(9) -0.0001(8) 0.0129(7) 0.0032(8) C9 0.0270(10) 0.0378(11) 0.0528(12) 0.0047(9) 0.0259(9) 0.0006(9) C10 0.0296(11) 0.0376(11) 0.0547(12) -0.0076(9) 0.0263(10) -0.0072(9) C11 0.0176(8) 0.0243(9) 0.0230(8) 0.0003(7) 0.0099(7) 0.0054(6) C12 0.0181(8) 0.0202(8) 0.0207(7) 0.0016(6) 0.0100(6) 0.0020(6) C13 0.0171(8) 0.0213(8) 0.0207(8) -0.0003(6) 0.0076(6) 0.0004(6) C14 0.0193(8) 0.0210(8) 0.0235(8) 0.0024(6) 0.0118(7) 0.0042(6) C15 0.0263(9) 0.0231(9) 0.0235(8) 0.0000(7) 0.0140(7) -0.0008(7) C16 0.0227(9) 0.0281(10) 0.0240(8) -0.0061(7) 0.0097(7) -0.0044(7) S17 0.0255(3) 0.0244(2) 0.0244(2) 0.00307(17) 0.01593(19) 0.00053(16) O18 0.0450(9) 0.0421(8) 0.0388(7) -0.0153(7) 0.0280(7) -0.0174(6) C19 0.0238(9) 0.0284(10) 0.0296(9) 0.0024(7) 0.0164(7) 0.0029(7) F20 0.0193(6) 0.0889(10) 0.0363(6) 0.0101(6) 0.0112(5) 0.0143(6) O21 0.0378(8) 0.0411(8) 0.0414(8) 0.0201(6) 0.0252(7) 0.0109(6) C22 0.0411(12) 0.0370(11) 0.0263(9) 0.0069(9) 0.0191(9) 0.0082(8) F23 0.0358(7) 0.0455(7) 0.0497(7) 0.0046(5) 0.0306(6) -0.0083(5) F24 0.0436(7) 0.0327(7) 0.0844(9) -0.0068(6) 0.0471(7) 0.0000(6) 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' 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' F F 0.0171 0.0103 '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 C5 O1 N2 . . 108.95(12) ? C3 N2 O1 . . 104.84(13) ? N2 C3 C4 . . 113.07(16) ? N2 C3 H3 . . 123.5 ? C4 C3 H3 . . 123.5 ? C5 C4 C3 . . 103.41(14) ? C5 C4 C6 . . 126.98(15) ? C3 C4 C6 . . 129.59(15) ? O1 C5 C4 . . 109.72(14) ? O1 C5 C8 . . 116.89(15) ? C4 C5 C8 . . 133.39(15) ? O7 C6 C4 . . 123.08(16) ? O7 C6 C11 . . 120.32(15) ? C4 C6 C11 . . 116.57(13) ? C5 C8 C9 . . 119.94(16) ? C5 C8 C10 . . 118.40(16) ? C9 C8 C10 . . 58.67(13) ? C5 C8 H8 . . 115.9 ? C9 C8 H8 . . 115.9 ? C10 C8 H8 . . 115.9 ? C10 C9 C8 . . 60.89(13) ? C10 C9 H9A . . 117.7 ? C8 C9 H9A . . 117.7 ? C10 C9 H9B . . 117.7 ? C8 C9 H9B . . 117.7 ? H9A C9 H9B . . 114.8 ? C9 C10 C8 . . 60.44(13) ? C9 C10 H10A . . 117.7 ? C8 C10 H10A . . 117.7 ? C9 C10 H10B . . 117.7 ? C8 C10 H10B . . 117.7 ? H10A C10 H10B . . 114.8 ? C16 C11 C12 . . 117.98(15) ? C16 C11 C6 . . 118.53(15) ? C12 C11 C6 . . 123.48(15) ? C13 C12 C11 . . 120.91(14) ? C13 C12 S17 . . 116.24(12) ? C11 C12 S17 . . 122.85(12) ? C14 C13 C12 . . 119.72(15) ? C14 C13 H13 . . 120.1 ? C12 C13 H13 . . 120.1 ? C15 C14 C13 . . 120.32(15) ? C15 C14 C19 . . 121.13(15) ? C13 C14 C19 . . 118.51(15) ? C14 C15 C16 . . 119.61(15) ? C14 C15 H15 . . 120.2 ? C16 C15 H15 . . 120.2 ? C15 C16 C11 . . 121.41(15) ? C15 C16 H16 . . 119.3 ? C11 C16 H16 . . 119.3 ? O18 S17 O21 . . 118.66(9) ? O18 S17 C22 . . 108.52(10) ? O21 S17 C22 . . 108.75(9) ? O18 S17 C12 . . 106.83(8) ? O21 S17 C12 . . 108.86(8) ? C22 S17 C12 . . 104.27(9) ? F23 C19 F24 . . 107.07(14) ? F23 C19 F20 . . 106.22(14) ? F24 C19 F20 . . 106.25(16) ? F23 C19 C14 . . 113.20(15) ? F24 C19 C14 . . 111.64(14) ? F20 C19 C14 . . 112.02(13) ? S17 C22 H22A . . 109.5 ? S17 C22 H22B . . 109.5 ? H22A C22 H22B . . 109.5 ? S17 C22 H22C . . 109.5 ? H22A C22 H22C . . 109.5 ? H22B C22 H22C . . 109.5 ? 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 O1 C5 . 1.341(2) ? O1 N2 . 1.4276(19) ? N2 C3 . 1.292(2) ? C3 C4 . 1.426(2) ? C3 H3 . 0.9500 ? C4 C5 . 1.370(2) ? C4 C6 . 1.458(2) ? C5 C8 . 1.456(2) ? C6 O7 . 1.215(2) ? C6 C11 . 1.513(2) ? C8 C9 . 1.501(3) ? C8 C10 . 1.508(3) ? C8 H8 . 1.0000 ? C9 C10 . 1.474(3) ? C9 H9A . 0.9900 ? C9 H9B . 0.9900 ? C10 H10A . 0.9900 ? C10 H10B . 0.9900 ? C11 C16 . 1.390(2) ? C11 C12 . 1.400(2) ? C12 C13 . 1.387(2) ? C12 S17 . 1.7794(16) ? C13 C14 . 1.386(2) ? C13 H13 . 0.9500 ? C14 C15 . 1.380(2) ? C14 C19 . 1.503(2) ? C15 C16 . 1.387(2) ? C15 H15 . 0.9500 ? C16 H16 . 0.9500 ? S17 O18 . 1.4291(14) ? S17 O21 . 1.4333(14) ? S17 C22 . 1.7521(18) ? C19 F23 . 1.326(2) ? C19 F24 . 1.330(2) ? C19 F20 . 1.335(2) ? C22 H22A . 0.9800 ? C22 H22B . 0.9800 ? C22 H22C . 0.9800 ? 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 C16 H16 O21 2_645 0.95 2.35 3.214(2) 150.6 C10 H10A O18 2_645 0.99 2.63 3.355(2) 129.9 C3 H3 O21 4_575 0.95 2.71 3.522(2) 144.2 _cod_database_fobs_code 2244158