#------------------------------------------------------------------------------ #$Date: 2024-06-01 05:14:25 +0300 (Sat, 01 Jun 2024) $ #$Revision: 292158 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023147.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_2023147 loop_ _publ_author_name 'Madhan, S.' 'NizamMohideen, M.' 'Harikrishnan, K.' 'MohanaKrishnan, Arasambattu K.' _publ_section_title ; The crystal structures and Hirshfeld surface analysis of three new bromo-substituted 3-methyl-1-(phenylsulfonyl)-1H-indole derivatives ; _journal_coeditor_code NU2005 _journal_issue 6 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_page_first 682 _journal_page_last 690 _journal_paper_doi 10.1107/S2056989024004985 _journal_volume 80 _journal_year 2024 _chemical_formula_iupac 'C24 H20 Br N O3 S' _chemical_formula_moiety 'C24 H20 Br N O3 S' _chemical_formula_sum 'C24 H20 Br N O3 S' _chemical_formula_weight 482.38 _chemical_name_systematic 2-[(E)-2-(2-Bromo-5-methoxyphenyl)ethenyl]-3-methyl-1-(phenylsulfonyl)-1H-indole _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-2019/3 _cell_angle_alpha 90 _cell_angle_beta 95.445(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.4252(9) _cell_length_b 28.669(3) _cell_length_c 8.9462(11) _cell_measurement_reflns_used 52480 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 24.996 _cell_measurement_theta_min 1.403 _cell_volume 2151.1(4) _computing_cell_refinement ; SAINT (Bruker, 2016) ; _computing_data_collection ; APEX2 (Bruker, 2016) ; _computing_data_reduction ; SAINT (Bruker, 2016) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) and Mercury (Macrae et al., 2020) ; _computing_publication_material ; WinGX (Farrugia, 2012), publCIF (Westrip, 2010) and PLATON (Spek, 2020) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS2018/3 (Sheldrick, 2008) ; _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker D8 Venture Diffractometer' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0772 _diffrn_reflns_av_unetI/netI 0.0363 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 52479 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.273 _diffrn_reflns_theta_min 3.253 _diffrn_source 'micro focus sealed tube' _exptl_absorpt_coefficient_mu 2.034 _exptl_absorpt_correction_T_max 0.745 _exptl_absorpt_correction_T_min 0.555 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour Yellow _exptl_crystal_density_diffrn 1.489 _exptl_crystal_description Solid _exptl_crystal_F_000 984 _exptl_crystal_size_max 0.245 _exptl_crystal_size_mid 0.196 _exptl_crystal_size_min 0.125 _refine_diff_density_max 0.390 _refine_diff_density_min -0.678 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 272 _refine_ls_number_reflns 5296 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.029 _refine_ls_R_factor_all 0.0622 _refine_ls_R_factor_gt 0.0391 _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^)+(0.0367P)^2^+1.0393P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0880 _refine_ls_wR_factor_ref 0.0985 _reflns_number_gt 3905 _reflns_number_total 5296 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file nu2005.cif _cod_data_source_block II _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2023147 _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 0.636 _shelx_estimated_absorpt_t_max 0.785 _shelx_hkl_file ; -2 0 0 1046.60 73.19 -2 0 0 1097.99 73.19 -2 0 0 1137.39 73.49 2 0 0 937.21 73.29 2 0 0 1064.09 73.29 2 0 0 991.90 73.49 -3 0 0 1425.76 96.29 -3 0 0 1347.07 96.19 -3 0 0 1412.76 96.59 3 0 0 1367.56 96.39 3 0 0 1365.46 96.39 3 0 0 1328.67 96.69 -4 0 0 192.28 14.50 4 0 0 198.38 14.40 4 0 0 173.48 14.60 4 0 0 198.28 14.20 -5 0 0 1688.73 116.59 5 0 0 1743.13 116.39 5 0 0 1528.15 116.69 -6 0 0 9.40 4.90 6 0 0 13.00 6.80 6 0 0 2.00 5.60 6 0 0 20.40 5.60 6 0 0 9.50 5.60 -7 0 0 105.69 10.00 7 0 0 108.19 11.60 7 0 0 112.99 11.90 7 0 0 108.99 10.70 7 0 0 92.29 10.30 8 0 0 60.19 8.90 8 0 0 64.79 10.20 8 0 0 46.20 8.70 8 0 0 32.20 8.80 -9 0 0 185.28 14.90 9 0 0 149.59 16.10 9 0 0 158.58 17.70 9 0 0 145.89 15.60 9 0 0 218.78 17.70 10 0 0 94.19 17.70 10 0 0 97.79 12.60 10 0 0 105.19 14.20 10 0 0 118.69 16.10 11 0 0 101.39 14.60 11 0 0 97.79 14.40 11 0 0 87.09 15.80 11 0 -1 -13.70 12.80 11 0 -1 -4.70 19.20 11 0 -1 -22.20 8.90 11 0 -1 0.20 10.80 11 0 -1 -3.70 12.20 10 0 -1 1.20 10.10 10 0 -1 -2.00 9.70 10 0 -1 -18.90 9.40 10 0 -1 -17.10 7.40 9 0 -1 10.40 9.50 9 0 -1 1.10 7.10 9 0 -1 -8.90 9.20 9 0 -1 -1.40 8.10 -9 0 1 -4.50 6.50 8 0 -1 -3.60 6.80 8 0 -1 5.30 7.50 8 0 -1 -4.20 6.80 8 0 -1 6.30 8.20 -8 0 1 2.80 6.30 7 0 -1 15.40 7.30 7 0 -1 0.20 6.20 7 0 -1 -3.00 5.40 -7 0 1 0.10 5.70 6 0 -1 -8.90 4.90 6 0 -1 -9.80 4.20 6 0 -1 -6.00 4.50 6 0 -1 5.70 5.60 -6 0 1 3.20 5.10 5 0 -1 -2.00 3.20 5 0 -1 -2.90 4.00 5 0 -1 4.20 4.80 5 0 -1 -1.40 3.30 -5 0 1 1.80 4.30 4 0 -1 3.60 2.60 4 0 -1 1.90 2.50 4 0 -1 -2.60 3.80 -4 0 1 -0.30 3.70 3 0 -1 1.70 2.00 3 0 -1 -2.90 3.00 3 0 -1 4.10 2.00 -3 0 1 3.90 3.10 2 0 -1 10.50 1.60 2 0 -1 7.70 1.60 2 0 -1 1.60 2.20 -2 0 1 13.30 1.20 -2 0 1 4.70 2.40 -2 0 1 11.00 1.10 1 0 -1 1.50 0.60 1 0 -1 2.60 1.70 -1 0 1 1.10 0.60 -1 0 1 -0.10 0.50 -1 0 1 1.40 0.90 -1 0 -1 -0.40 0.70 -1 0 -1 0.10 1.10 -1 0 -1 2.00 1.20 1 0 1 -0.20 1.00 1 0 1 4.70 1.40 1 0 1 1.20 1.50 -2 0 -1 3.60 1.70 -2 0 -1 1.60 1.30 -2 0 -1 4.00 1.70 2 0 1 4.50 2.00 2 0 1 -0.40 1.30 2 0 1 2.70 1.80 -3 0 -1 4.00 2.00 -3 0 -1 0.10 1.90 -3 0 -1 -0.90 2.20 3 0 1 2.70 2.70 3 0 1 -1.50 1.70 3 0 1 -0.30 2.60 -4 0 -1 0.60 2.60 -4 0 -1 -2.10 2.20 -4 0 -1 0.70 2.30 4 0 1 -2.70 3.20 4 0 1 -2.80 2.60 4 0 1 -2.30 3.30 -5 0 -1 -0.60 2.00 -5 0 -1 0.70 2.90 -5 0 -1 1.00 2.00 5 0 1 -1.10 3.20 5 0 1 -1.50 4.30 5 0 1 -0.20 3.90 -6 0 -1 9.20 3.80 6 0 1 1.50 4.40 6 0 1 0.60 5.80 6 0 1 9.10 5.50 -7 0 -1 7.20 4.90 7 0 1 9.10 6.80 7 0 1 -4.00 7.60 7 0 1 -23.20 7.80 -8 0 -1 -4.00 5.30 8 0 1 -3.30 7.90 8 0 1 2.90 7.20 8 0 1 -27.70 9.00 -9 0 -1 7.40 6.00 9 0 1 10.20 9.00 9 0 1 14.30 10.90 9 0 1 -13.60 11.20 9 0 1 -2.40 8.30 9 0 1 -0.90 8.60 10 0 1 -6.70 14.30 10 0 1 -11.00 9.80 10 0 1 -6.90 8.60 10 0 1 0.00 14.60 11 0 1 -0.10 10.10 11 0 1 0.30 13.00 11 0 1 -28.80 17.40 11 0 -2 116.09 14.80 11 0 -2 90.89 13.20 11 0 -2 111.09 12.80 11 0 -2 73.89 15.70 10 0 -2 9.50 9.40 10 0 -2 2.50 12.80 10 0 -2 -4.30 8.10 10 0 -2 -7.60 9.00 9 0 -2 17.00 8.80 9 0 -2 34.20 10.90 9 0 -2 13.80 7.70 9 0 -2 25.70 8.50 -9 0 2 23.60 8.30 8 0 -2 4.70 6.40 8 0 -2 1.10 9.00 8 0 -2 4.40 6.70 -8 0 2 8.90 7.30 7 0 -2 565.64 40.00 7 0 -2 509.85 41.00 7 0 -2 618.04 40.40 7 0 -2 476.55 40.70 -7 0 2 563.74 40.60 6 0 -2 197.58 14.30 6 0 -2 168.08 14.40 6 0 -2 186.58 15.20 6 0 -2 159.28 13.90 -6 0 2 172.58 14.50 5 0 -2 1340.47 91.89 5 0 -2 1435.26 91.99 5 0 -2 1231.58 92.69 5 0 -2 1189.08 91.79 -5 0 2 1322.97 92.49 4 0 -2 6315.27 448.56 4 0 -2 6041.90 448.56 4 0 -2 6131.69 449.36 -4 0 2 7170.68 449.26 3 0 -2 722.43 54.69 3 0 -2 765.42 53.99 3 0 -2 787.92 54.09 -3 0 2 728.03 53.69 -3 0 2 835.82 54.69 1 0 -2 792.02 59.39 1 0 -2 776.42 59.59 1 0 -2 906.11 59.49 1 0 -2 858.11 59.89 -1 0 2 902.51 59.59 -1 0 2 921.81 59.79 -1 0 2 760.42 59.29 -1 0 2 816.12 59.39 -1 0 2 887.61 59.49 -2 0 -2 133.99 10.00 -2 0 -2 126.69 9.40 -2 0 -2 138.59 10.00 2 0 2 102.49 10.00 2 0 2 146.69 10.00 2 0 2 111.89 10.10 -3 0 -2 205.88 14.40 -3 0 -2 190.28 14.20 -3 0 -2 178.88 13.80 3 0 2 202.68 14.70 3 0 2 210.18 15.10 3 0 2 170.18 14.40 -4 0 -2 1911.81 133.29 -4 0 -2 1995.30 133.19 -4 0 -2 1945.51 133.19 4 0 2 1785.62 133.49 4 0 2 1844.02 134.29 -5 0 -2 94.89 7.90 -5 0 -2 104.49 8.30 -5 0 -2 95.99 8.30 5 0 2 117.89 10.20 5 0 2 86.49 8.20 5 0 2 86.69 12.00 5 0 2 90.59 10.60 -6 0 -2 1792.32 120.89 -6 0 -2 1616.64 120.49 -6 0 -2 1657.83 120.49 6 0 2 1606.04 121.39 6 0 2 1802.32 122.69 6 0 2 1660.73 121.09 6 0 2 1938.01 122.59 -7 0 -2 220.78 16.90 7 0 2 244.18 19.10 7 0 2 262.87 21.10 7 0 2 204.68 17.50 7 0 2 185.58 18.20 7 0 2 211.98 20.30 -8 0 -2 137.79 12.30 8 0 2 167.68 16.70 8 0 2 156.48 15.90 8 0 2 175.58 15.60 8 0 2 135.79 14.30 -9 0 -2 336.57 26.70 9 0 2 341.87 31.70 9 0 2 355.56 29.60 9 0 2 373.46 27.80 9 0 2 430.86 36.30 9 0 2 359.46 29.20 10 0 2 35.90 13.30 10 0 2 49.60 14.00 10 0 2 18.80 12.30 11 0 -3 -11.80 10.20 11 0 -3 -28.60 13.00 10 0 -3 -15.20 12.30 10 0 -3 0.80 8.10 10 0 -3 12.10 9.20 9 0 -3 1.30 7.80 9 0 -3 3.70 7.10 9 0 -3 13.60 11.20 9 0 -3 1.20 6.50 -9 0 3 9.70 6.10 8 0 -3 -2.70 5.00 8 0 -3 5.00 6.40 8 0 -3 23.50 10.60 8 0 -3 -0.40 6.70 -8 0 3 -0.70 7.70 7 0 -3 2.60 5.80 7 0 -3 5.80 5.80 7 0 -3 -6.10 4.20 7 0 -3 6.50 6.90 -7 0 3 -10.20 5.60 6 0 -3 4.20 4.40 6 0 -3 1.30 4.50 6 0 -3 -0.70 7.40 6 0 -3 -7.70 3.30 -6 0 3 5.00 5.20 5 0 -3 4.20 4.10 5 0 -3 -2.40 4.50 5 0 -3 -0.50 6.20 5 0 -3 -0.20 2.40 -5 0 3 -7.30 4.60 4 0 -3 5.40 3.40 4 0 -3 -3.00 5.10 4 0 -3 -1.80 4.00 -4 0 3 3.30 5.20 3 0 -3 1.70 3.40 3 0 -3 -0.30 4.10 3 0 -3 3.10 3.70 3 0 -3 0.50 3.10 -3 0 3 0.10 2.50 -3 0 3 0.20 3.90 -3 0 3 4.60 2.30 2 0 -3 0.00 4.00 2 0 -3 1.70 3.20 2 0 -3 -3.00 2.90 2 0 -3 2.40 2.80 -2 0 3 -1.00 0.80 -2 0 3 3.70 4.00 -2 0 3 2.30 2.40 -2 0 3 -4.20 2.70 1 0 -3 3.70 2.70 1 0 -3 2.80 2.50 1 0 -3 -3.40 2.60 1 0 -3 -1.60 3.30 -1 0 3 -4.60 2.40 -1 0 3 0.90 2.80 -1 0 3 0.00 2.50 -1 0 3 0.60 1.80 0 0 -3 -0.90 2.40 0 0 -3 3.80 2.80 0 0 -3 -3.60 2.60 0 0 -3 -3.20 3.10 0 0 3 -1.20 2.90 0 0 3 5.10 2.30 0 0 3 1.00 2.90 -1 0 -3 5.50 2.70 -1 0 -3 -5.30 3.40 -1 0 -3 -5.70 2.80 1 0 3 2.00 3.30 1 0 3 -0.20 3.40 1 0 3 -3.80 3.20 -2 0 -3 4.80 3.30 -2 0 -3 -0.30 3.50 -2 0 -3 -0.60 3.70 2 0 3 -5.40 3.60 2 0 3 -0.40 3.50 2 0 3 5.40 3.50 -3 0 -3 1.30 3.50 -3 0 -3 -1.60 2.50 -3 0 -3 -5.50 3.50 3 0 3 -6.40 3.80 3 0 3 -2.50 4.80 3 0 3 1.00 4.10 -4 0 -3 -0.70 2.60 -4 0 -3 11.30 4.20 -4 0 -3 5.60 4.10 4 0 3 7.10 5.30 4 0 3 -2.10 4.90 4 0 3 2.10 5.10 -5 0 -3 0.00 2.80 -5 0 -3 -3.10 4.50 -5 0 -3 -4.50 4.00 5 0 3 4.70 6.50 5 0 3 4.60 7.60 5 0 3 1.40 5.30 -6 0 -3 -1.60 4.00 -6 0 -3 2.10 3.70 -6 0 -3 -2.40 4.40 6 0 3 -3.30 6.30 6 0 3 2.50 7.90 6 0 3 -19.60 8.80 6 0 3 -1.70 7.30 -7 0 -3 2.60 3.80 -7 0 -3 -1.70 3.60 -7 0 -3 0.70 3.90 7 0 3 0.80 8.60 7 0 3 -1.60 11.00 7 0 3 0.70 8.70 7 0 3 0.20 7.80 -8 0 -3 -4.90 4.10 8 0 3 11.20 8.60 8 0 3 -2.20 10.00 8 0 3 -3.20 9.80 8 0 3 2.40 9.80 -9 0 -3 8.40 4.70 9 0 3 -7.70 13.60 9 0 3 6.60 11.00 10 0 3 8.70 14.50 10 0 3 -7.60 11.90 10 0 -4 42.30 10.10 10 0 -4 43.10 12.40 10 0 -4 35.70 9.60 9 0 -4 199.88 20.10 9 0 -4 241.78 23.30 9 0 -4 234.78 19.80 9 0 -4 234.78 17.20 8 0 -4 182.38 16.40 8 0 -4 181.58 16.60 8 0 -4 176.08 13.60 8 0 -4 221.48 19.70 -8 0 4 175.68 16.50 7 0 -4 673.13 48.40 7 0 -4 630.94 46.80 -7 0 4 638.44 47.90 6 0 -4 275.37 23.80 6 0 -4 278.77 21.70 6 0 -4 325.67 23.60 6 0 -4 279.37 22.20 -6 0 4 268.17 22.40 5 0 -4 2208.58 176.78 5 0 -4 2708.83 177.88 5 0 -4 2718.43 176.98 -5 0 4 2448.66 177.58 4 0 -4 704.53 47.50 4 0 -4 606.74 46.80 4 0 -4 639.04 47.90 4 0 -4 707.83 47.00 -4 0 4 648.84 46.20 -4 0 4 664.13 47.80 -4 0 4 627.84 46.20 3 0 -4 589.44 46.10 3 0 -4 661.03 47.10 3 0 -4 735.63 46.40 -3 0 4 617.14 46.90 -3 0 4 652.13 46.00 -3 0 4 630.74 45.80 2 0 -4 36.70 5.00 2 0 -4 13.80 5.20 2 0 -4 19.40 4.20 -2 0 4 19.90 4.90 -2 0 4 29.90 2.90 -2 0 4 32.60 4.40 -2 0 4 28.40 4.40 1 0 -4 5.30 3.70 1 0 -4 6.90 4.20 1 0 -4 10.70 4.50 1 0 -4 1.10 4.40 -1 0 4 -0.30 3.60 -1 0 4 1.90 2.80 -1 0 4 4.50 3.80 -1 0 4 -0.20 3.60 0 0 -4 138.79 11.30 0 0 -4 148.79 11.00 0 0 -4 121.49 10.90 0 0 -4 119.39 10.90 0 0 4 138.69 11.00 0 0 4 138.19 11.00 0 0 4 111.19 11.10 -1 0 -4 6.70 4.10 -1 0 -4 11.70 3.70 -1 0 -4 12.70 4.70 1 0 4 5.00 4.80 1 0 4 7.00 4.30 1 0 4 5.40 4.40 -2 0 -4 2879.11 223.18 -2 0 -4 3402.36 223.68 -2 0 -4 3180.08 223.28 2 0 4 3283.87 223.88 2 0 4 3175.08 223.38 -3 0 -4 488.95 35.10 -3 0 -4 507.95 35.00 3 0 4 435.76 35.50 -4 0 -4 841.92 57.19 -4 0 -4 816.52 57.69 4 0 4 754.92 58.49 -5 0 -4 57.19 6.90 -5 0 -4 45.10 6.70 -5 0 -4 49.00 5.00 5 0 4 42.30 8.60 5 0 4 32.80 9.70 5 0 4 53.99 8.20 -6 0 -4 2010.30 146.89 -6 0 -4 2032.10 146.79 -6 0 -4 2067.89 146.49 6 0 4 1967.20 147.79 6 0 4 2288.57 149.09 6 0 4 2212.98 147.89 6 0 4 2063.89 148.89 -7 0 -4 202.88 14.30 -7 0 -4 190.98 15.30 7 0 4 184.88 19.30 7 0 4 172.98 20.50 7 0 4 178.68 18.60 7 0 4 176.48 18.80 -8 0 -4 237.88 17.30 -8 0 -4 225.48 17.20 -8 0 -4 221.78 17.20 8 0 4 283.17 23.10 8 0 4 254.17 22.00 8 0 4 249.97 24.40 9 0 4 18.70 15.20 9 0 4 23.00 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14.30 11.90 8 -12 4 10.00 10.10 9 -12 4 2.90 11.20 9 -12 4 -11.70 11.20 9 -12 4 4.30 13.60 9 12 -5 -8.30 11.10 9 12 -5 22.30 13.50 8 12 -5 315.27 28.60 8 12 -5 335.77 28.70 -8 -12 5 309.37 24.10 7 12 -5 111.09 16.80 7 12 -5 141.19 14.40 -7 -12 5 107.89 11.50 -7 -12 5 113.19 11.90 6 12 -5 466.95 38.50 6 12 -5 570.14 40.30 -6 -12 5 485.25 37.50 -6 -12 5 509.65 37.20 5 12 -5 43.90 10.10 5 12 -5 28.70 9.20 5 12 -5 34.20 10.00 5 12 -5 45.30 9.60 -5 -12 5 28.10 5.10 -5 -12 5 34.00 8.80 4 12 -5 11.60 9.70 4 12 -5 8.20 7.80 4 12 -5 -9.90 8.10 4 12 -5 13.90 9.70 -4 -12 5 9.00 5.40 -4 -12 5 10.00 7.60 -4 -12 5 -0.20 7.60 -4 -12 5 9.10 8.50 3 12 -5 507.15 41.10 3 12 -5 566.04 41.40 3 12 -5 604.14 41.90 3 12 -5 575.24 41.60 -3 -12 5 539.65 41.50 -3 -12 5 559.64 40.90 -3 -12 5 563.64 40.50 -3 -12 5 567.54 41.30 -3 -12 5 527.75 41.50 2 12 -5 187.18 16.60 2 12 -5 181.88 16.30 2 12 -5 203.28 16.70 2 12 -5 178.08 17.30 -2 -12 5 193.18 16.20 -2 -12 5 180.08 15.50 -2 -12 5 172.08 16.40 -2 -12 5 202.38 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8.10 2 -37 -1 -10.60 12.30 2 -37 -1 9.10 16.50 2 37 0 11.20 12.40 -2 -37 0 7.40 16.60 -2 -37 0 -3.60 18.60 1 37 0 -22.60 10.50 -1 -37 0 -3.60 23.90 -1 -37 0 8.30 20.90 0 37 0 -0.40 9.80 0 -37 0 17.50 17.60 0 -37 0 14.20 16.20 -1 37 0 0.60 7.40 -1 37 0 13.40 6.40 1 -37 0 -31.80 18.90 1 -37 0 -21.30 13.60 2 -37 0 -31.70 15.70 2 -37 0 9.30 15.00 -2 -37 1 7.60 15.90 -2 -37 1 9.20 15.70 1 37 -1 6.10 11.00 -1 -37 1 -15.00 24.50 0 37 -1 -1.70 15.90 0 -37 1 -6.30 17.10 0 -37 1 8.30 14.30 -1 37 -1 -6.40 6.80 -1 37 -1 3.10 7.70 1 -37 1 35.70 19.80 1 -37 1 -14.20 13.50 2 -37 1 0.60 15.70 2 -37 1 -3.70 12.90 2 -37 1 -4.20 14.40 2 37 -2 18.10 11.80 -2 -37 2 -2.80 16.00 -2 -37 2 -14.70 15.20 -1 -37 2 10.20 20.50 -1 -37 2 32.70 20.00 0 -37 2 8.10 19.90 -1 37 -2 7.90 7.30 -1 37 -2 16.50 8.60 1 -37 2 5.10 13.80 1 -37 2 -1.50 19.20 1 -37 2 24.60 14.70 0 38 1 10.20 9.00 0 -38 -1 27.40 16.70 1 38 0 31.90 11.10 -1 -38 0 7.80 16.30 -1 -38 0 5.30 19.70 0 38 0 13.20 9.60 0 -38 0 -29.40 18.70 -1 38 0 27.50 7.10 -1 38 0 22.00 7.80 1 -38 0 27.60 20.20 1 -38 0 22.40 16.60 0 -38 1 21.20 16.50 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 55221 _shelx_res_file ; TITL SM16_a.res in P2(1)/c ii.res created by SHELXL-2019/3 at 11:32:26 on 15-May-2024 CELL 0.71073 8.4252 28.6687 8.9462 90.000 95.445 90.000 ZERR 4.00 0.0009 0.0034 0.0011 0.000 0.004 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O S BR UNIT 96 80 4 12 4 4 MERG 2 OMIT 0 3 1 OMIT 0 2 1 OMIT 1 3 0 EQIV $1 1-X, 1-Y, -Z EQIV $2 X-1, -Y+1/2, Z+1/2 EQIV $3 2-X, 1-Y, 1-Z EQIV $4 x, 0.5-Y, 0.5+Z HTAB C2 O2 HTAB C3 O2_$1 HTAB C24 Br1_$2 RTAB D2CG C5 C9_$3 C10_$3 C11_$3 C12_$3 C13_$3 C14_$3 RTAB D2CG H5 C9_$3 C10_$3 C11_$3 C12_$3 C13_$3 C14_$3 RTAB D2CG C20 C17_$4 C18_$4 C19_$4 C20_$4 C21_$4 C22_$4 RTAB D2CG H20 C17_$4 C18_$4 C19_$4 C20_$4 C21_$4 C22_$4 RTAB D2CG C23 C1_$3 C2_$3 C3_$3 C4_$3 C5_$3 C6_$3 RTAB D2CG H23C C1_$3 C2_$3 C3_$3 C4_$3 C5_$3 C6_$3 FMAP 2 PLAN 20 SIZE 0.13 0.20 0.25 ACTA BOND $H CONF L.S. 6 TEMP 25.00 WGHT 0.036700 1.039300 FVAR 0.68436 C1 1 0.656141 0.485498 0.347048 11.00000 0.04520 0.05094 = 0.04539 0.00732 0.00920 0.01211 C2 1 0.628123 0.508289 0.209281 11.00000 0.06527 0.06998 = 0.04930 0.01390 0.00760 0.01683 AFIX 43 H2 2 0.568729 0.494387 0.128332 11.00000 -1.20000 AFIX 0 C3 1 0.692258 0.552364 0.198075 11.00000 0.07839 0.07313 = 0.06604 0.03113 0.01936 0.02334 AFIX 43 H3 2 0.676266 0.568262 0.107279 11.00000 -1.20000 AFIX 0 C4 1 0.779089 0.573368 0.317502 11.00000 0.07776 0.05259 = 0.09568 0.02748 0.02622 0.00884 AFIX 43 H4 2 0.820363 0.603085 0.305664 11.00000 -1.20000 AFIX 0 C5 1 0.806160 0.551319 0.454165 11.00000 0.07016 0.04946 = 0.07403 0.00524 0.01147 -0.00183 AFIX 43 H5 2 0.863821 0.565906 0.534811 11.00000 -1.20000 AFIX 0 C6 1 0.744586 0.506317 0.468647 11.00000 0.05073 0.04354 = 0.04872 0.00472 0.00992 0.00663 C7 1 0.751342 0.474580 0.593527 11.00000 0.04943 0.04698 = 0.04192 0.00127 0.00437 0.00263 C8 1 0.671596 0.435165 0.547528 11.00000 0.04230 0.04772 = 0.03671 0.00319 0.00596 0.00552 C9 1 0.783654 0.382925 0.242423 11.00000 0.04811 0.05260 = 0.04587 -0.01268 0.00364 -0.00510 C10 1 0.868408 0.351085 0.333730 11.00000 0.06145 0.06976 = 0.07136 -0.00063 0.00996 0.01123 AFIX 43 H10 2 0.820424 0.335580 0.408902 11.00000 -1.20000 AFIX 0 C11 1 1.026093 0.342599 0.311589 11.00000 0.06662 0.09001 = 0.10000 -0.01262 0.00040 0.02393 AFIX 43 H11 2 1.084868 0.321232 0.372357 11.00000 -1.20000 AFIX 0 C12 1 1.096406 0.365608 0.200131 11.00000 0.05180 0.09621 = 0.11239 -0.04836 0.01945 -0.00749 AFIX 43 H12 2 1.202336 0.359691 0.185423 11.00000 -1.20000 AFIX 0 C13 1 1.010345 0.397239 0.110810 11.00000 0.08162 0.07993 = 0.08605 -0.02660 0.03997 -0.01907 AFIX 43 H13 2 1.058787 0.412993 0.036429 11.00000 -1.20000 AFIX 0 C14 1 0.853894 0.405885 0.129910 11.00000 0.07379 0.06727 = 0.05391 -0.00909 0.01671 -0.00362 AFIX 43 H14 2 0.795426 0.426986 0.067855 11.00000 -1.20000 AFIX 0 C15 1 0.638275 0.393871 0.634579 11.00000 0.04401 0.04737 = 0.04247 0.00134 0.00719 -0.00095 AFIX 43 H15 2 0.536056 0.381323 0.623013 11.00000 -1.20000 AFIX 0 C16 1 0.747767 0.373319 0.729952 11.00000 0.04080 0.04346 = 0.04769 -0.00078 0.00687 0.00080 AFIX 43 H16 2 0.851979 0.384173 0.732095 11.00000 -1.20000 AFIX 0 C17 1 0.717003 0.334902 0.831932 11.00000 0.04243 0.03661 = 0.03986 -0.00266 -0.00196 0.00027 C18 1 0.568302 0.329175 0.884384 11.00000 0.04308 0.04309 = 0.04407 0.00382 -0.00211 0.00172 AFIX 43 H18 2 0.486448 0.349562 0.851587 11.00000 -1.20000 AFIX 0 C19 1 0.538085 0.293878 0.984466 11.00000 0.04688 0.05144 = 0.04714 0.00762 -0.00281 -0.00593 C20 1 0.658739 0.263803 1.036600 11.00000 0.06142 0.05308 = 0.06307 0.02011 -0.00602 -0.00301 AFIX 43 H20 2 0.639903 0.240384 1.104648 11.00000 -1.20000 AFIX 0 C21 1 0.807424 0.268908 0.986578 11.00000 0.05587 0.04722 = 0.06827 0.01146 -0.00811 0.00975 AFIX 43 H21 2 0.889518 0.248965 1.022176 11.00000 -1.20000 AFIX 0 C22 1 0.836106 0.303065 0.884796 11.00000 0.04217 0.04248 = 0.05049 -0.00573 -0.00218 0.00358 C23 1 0.822302 0.486722 0.748509 11.00000 0.09296 0.05775 = 0.05101 -0.00381 -0.00601 -0.00493 AFIX 137 H23A 2 0.791508 0.463736 0.818252 11.00000 -1.50000 H23B 2 0.784469 0.516817 0.776049 11.00000 -1.50000 H23C 2 0.936409 0.487396 0.750554 11.00000 -1.50000 AFIX 0 C24 1 0.348855 0.258005 1.129517 11.00000 0.07886 0.10950 = 0.10580 0.05289 0.02348 -0.01237 AFIX 33 H24A 2 0.238662 0.260695 1.147390 11.00000 -1.50000 H24B 2 0.368142 0.227541 1.090527 11.00000 -1.50000 H24C 2 0.414581 0.262561 1.222022 11.00000 -1.50000 AFIX 0 N1 3 0.604368 0.441080 0.394838 11.00000 0.04543 0.04903 = 0.03993 0.00236 0.00177 0.00467 O1 4 0.520540 0.358181 0.352524 11.00000 0.05811 0.06597 = 0.06661 -0.00489 0.00663 -0.01935 O2 4 0.502017 0.413581 0.140934 11.00000 0.06652 0.09391 = 0.05124 -0.00416 -0.01950 0.00618 O3 4 0.386122 0.292369 1.023855 11.00000 0.05095 0.08448 = 0.07604 0.03371 0.00770 -0.00576 S1 5 0.585890 0.395953 0.275181 11.00000 0.04408 0.06195 = 0.04435 -0.00533 -0.00327 -0.00217 BR1 6 1.042539 0.306077 0.817297 11.00000 0.04735 0.06198 = 0.08971 -0.00450 0.01150 0.01104 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 REM SM16_a.res in P2(1)/c REM wR2 = 0.0985, GooF = S = 1.029, Restrained GooF = 1.029 for all data REM R1 = 0.0391 for 3905 Fo > 4sig(Fo) and 0.0622 for all 5296 data REM 272 parameters refined using 0 restraints END WGHT 0.0367 1.0395 REM Highest difference peak 0.390, deepest hole -0.678, 1-sigma level 0.085 Q1 1 1.0735 0.3125 0.7366 11.00000 0.05 0.39 Q2 1 0.9995 0.2822 0.8206 11.00000 0.05 0.33 Q3 1 0.7564 0.3133 0.8312 11.00000 0.05 0.31 Q4 1 0.6507 0.3315 0.8312 11.00000 0.05 0.30 Q5 1 1.0557 0.3619 0.2963 11.00000 0.05 0.28 Q6 1 0.9381 0.4110 0.1580 11.00000 0.05 0.26 Q7 1 0.5441 0.3401 0.8833 11.00000 0.05 0.26 Q8 1 0.9485 0.5830 0.6573 11.00000 0.05 0.26 Q9 1 0.9446 0.3437 0.2796 11.00000 0.05 0.25 Q10 1 0.5458 0.3030 0.9021 11.00000 0.05 0.25 Q11 1 0.5393 0.3310 0.8430 11.00000 0.05 0.25 Q12 1 0.5081 0.3893 0.6950 11.00000 0.05 0.24 Q13 1 0.7611 0.5284 0.4540 11.00000 0.05 0.23 Q14 1 0.9498 0.3324 0.2177 11.00000 0.05 0.23 Q15 1 1.0394 0.3272 0.3063 11.00000 0.05 0.23 Q16 1 1.1511 0.3583 0.4181 11.00000 0.05 0.23 Q17 1 0.4886 0.3591 0.7420 11.00000 0.05 0.23 Q18 1 0.5835 0.4301 0.0991 11.00000 0.05 0.22 Q19 1 0.5363 0.3791 0.8470 11.00000 0.05 0.22 Q20 1 0.5569 0.4054 0.8872 11.00000 0.05 0.22 ; _shelx_res_checksum 99769 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 C C1 0.6561(3) 0.48550(8) 0.3470(2) 0.0469(5) Uani d 1 . . C C2 0.6281(3) 0.50829(10) 0.2093(3) 0.0614(6) Uani d 1 . . H H2 0.568729 0.494387 0.128332 0.074 Uiso calc 1 . . C C3 0.6923(4) 0.55236(11) 0.1981(3) 0.0717(8) Uani d 1 . . H H3 0.676266 0.568262 0.107279 0.086 Uiso calc 1 . . C C4 0.7791(4) 0.57337(10) 0.3175(4) 0.0742(8) Uani d 1 . . H H4 0.820363 0.603085 0.305664 0.089 Uiso calc 1 . . C C5 0.8062(3) 0.55132(9) 0.4542(3) 0.0643(7) Uani d 1 . . H H5 0.863821 0.565906 0.534811 0.077 Uiso calc 1 . . C C6 0.7446(3) 0.50632(8) 0.4686(2) 0.0473(5) Uani d 1 . . C C7 0.7513(3) 0.47458(8) 0.5935(2) 0.0461(5) Uani d 1 . . C C8 0.6716(2) 0.43516(7) 0.5475(2) 0.0421(4) Uani d 1 . . C C9 0.7837(3) 0.38292(8) 0.2424(3) 0.0489(5) Uani d 1 . . C C10 0.8684(3) 0.35109(10) 0.3337(3) 0.0673(7) Uani d 1 . . H H10 0.820424 0.335580 0.408902 0.081 Uiso calc 1 . . C C11 1.0261(4) 0.34260(13) 0.3116(4) 0.0860(10) Uani d 1 . . H H11 1.084868 0.321232 0.372357 0.103 Uiso calc 1 . . C C12 1.0964(4) 0.36561(13) 0.2001(5) 0.0861(10) Uani d 1 . . H H12 1.202336 0.359691 0.185423 0.103 Uiso calc 1 . . C C13 1.0103(4) 0.39724(12) 0.1108(4) 0.0805(9) Uani d 1 . . H H13 1.058787 0.412993 0.036429 0.097 Uiso calc 1 . . C C14 0.8539(4) 0.40589(10) 0.1299(3) 0.0643(7) Uani d 1 . . H H14 0.795426 0.426986 0.067855 0.077 Uiso calc 1 . . C C15 0.6383(3) 0.39387(8) 0.6346(2) 0.0444(5) Uani d 1 . . H H15 0.536056 0.381323 0.623013 0.053 Uiso calc 1 . . C C16 0.7478(3) 0.37332(7) 0.7300(2) 0.0438(5) Uani d 1 . . H H16 0.851979 0.384173 0.732095 0.053 Uiso calc 1 . . C C17 0.7170(2) 0.33490(7) 0.8319(2) 0.0400(4) Uani d 1 . . C C18 0.5683(3) 0.32918(7) 0.8844(2) 0.0438(5) Uani d 1 . . H H18 0.486448 0.349562 0.851587 0.053 Uiso calc 1 . . C C19 0.5381(3) 0.29388(8) 0.9845(3) 0.0490(5) Uani d 1 . . C C20 0.6587(3) 0.26380(9) 1.0366(3) 0.0599(6) Uani d 1 . . H H20 0.639903 0.240384 1.104648 0.072 Uiso calc 1 . . C C21 0.8074(3) 0.26891(8) 0.9866(3) 0.0580(6) Uani d 1 . . H H21 0.889518 0.248965 1.022176 0.070 Uiso calc 1 . . C C22 0.8361(3) 0.30307(7) 0.8848(3) 0.0455(5) Uani d 1 . . C C23 0.8223(4) 0.48672(10) 0.7485(3) 0.0681(7) Uani d 1 . . H H23A 0.791508 0.463736 0.818252 0.102 Uiso calc 1 . . H H23B 0.784469 0.516817 0.776049 0.102 Uiso calc 1 . . H H23C 0.936409 0.487396 0.750554 0.102 Uiso calc 1 . . C C24 0.3489(4) 0.25800(13) 1.1295(4) 0.0971(12) Uani d 1 . . H H24A 0.238662 0.260695 1.147390 0.146 Uiso calc 1 . . H H24B 0.368142 0.227541 1.090527 0.146 Uiso calc 1 . . H H24C 0.414581 0.262561 1.222022 0.146 Uiso calc 1 . . N N1 0.6044(2) 0.44108(6) 0.39484(19) 0.0449(4) Uani d 1 . . O O1 0.5205(2) 0.35818(6) 0.3525(2) 0.0635(5) Uani d 1 . . O O2 0.5020(2) 0.41358(7) 0.1409(2) 0.0722(5) Uani d 1 . . O O3 0.3861(2) 0.29237(7) 1.0239(2) 0.0704(5) Uani d 1 . . S S1 0.58589(7) 0.39595(2) 0.27518(6) 0.05060(15) Uani d 1 . . Br Br1 1.04254(3) 0.30608(2) 0.81730(3) 0.06603(11) 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 C1 0.0452(11) 0.0509(12) 0.0454(12) 0.0121(9) 0.0092(9) 0.0073(10) C2 0.0653(16) 0.0700(16) 0.0493(13) 0.0168(13) 0.0076(11) 0.0139(12) C3 0.0784(19) 0.0731(18) 0.0660(17) 0.0233(15) 0.0194(15) 0.0311(15) C4 0.0778(19) 0.0526(15) 0.096(2) 0.0088(14) 0.0262(17) 0.0275(15) C5 0.0702(17) 0.0495(14) 0.0740(17) -0.0018(12) 0.0115(14) 0.0052(13) C6 0.0507(12) 0.0435(11) 0.0487(12) 0.0066(9) 0.0099(10) 0.0047(10) C7 0.0494(12) 0.0470(12) 0.0419(11) 0.0026(9) 0.0044(9) 0.0013(9) C8 0.0423(11) 0.0477(11) 0.0367(10) 0.0055(9) 0.0060(8) 0.0032(9) C9 0.0481(12) 0.0526(13) 0.0459(12) -0.0051(10) 0.0036(10) -0.0127(10) C10 0.0614(16) 0.0698(17) 0.0714(17) 0.0112(13) 0.0100(13) -0.0006(14) C11 0.0666(19) 0.090(2) 0.100(2) 0.0239(17) 0.0004(18) -0.0126(19) C12 0.0518(16) 0.096(2) 0.112(3) -0.0075(16) 0.0195(18) -0.048(2) C13 0.082(2) 0.080(2) 0.086(2) -0.0191(17) 0.0400(18) -0.0266(18) C14 0.0738(17) 0.0673(16) 0.0539(14) -0.0036(13) 0.0167(13) -0.0091(12) C15 0.0440(11) 0.0474(12) 0.0425(11) -0.0010(9) 0.0072(9) 0.0013(9) C16 0.0408(11) 0.0435(11) 0.0477(12) 0.0008(9) 0.0069(9) -0.0008(9) C17 0.0424(10) 0.0366(10) 0.0399(10) 0.0003(8) -0.0020(8) -0.0027(8) C18 0.0431(11) 0.0431(11) 0.0441(11) 0.0017(9) -0.0021(9) 0.0038(9) C19 0.0469(12) 0.0514(12) 0.0471(12) -0.0059(10) -0.0028(10) 0.0076(10) C20 0.0614(15) 0.0531(14) 0.0631(15) -0.0030(11) -0.0060(12) 0.0201(12) C21 0.0559(14) 0.0472(13) 0.0683(16) 0.0097(11) -0.0081(12) 0.0115(12) C22 0.0422(11) 0.0425(11) 0.0505(12) 0.0036(9) -0.0022(9) -0.0057(9) C23 0.093(2) 0.0577(15) 0.0510(14) -0.0049(14) -0.0060(14) -0.0038(12) C24 0.079(2) 0.110(3) 0.106(3) -0.0124(19) 0.0235(19) 0.053(2) N1 0.0454(9) 0.0490(10) 0.0399(9) 0.0047(8) 0.0018(7) 0.0024(8) O1 0.0581(10) 0.0660(11) 0.0666(11) -0.0193(8) 0.0066(8) -0.0049(9) O2 0.0665(11) 0.0939(14) 0.0512(10) 0.0062(10) -0.0195(8) -0.0042(9) O3 0.0510(10) 0.0845(13) 0.0760(12) -0.0058(9) 0.0077(9) 0.0337(10) S1 0.0441(3) 0.0620(4) 0.0443(3) -0.0022(3) -0.0033(2) -0.0053(3) Br1 0.04735(15) 0.06198(17) 0.0897(2) 0.01104(11) 0.01150(13) -0.00450(14) 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 C6 C1 C2 . . 121.5(2) ? C6 C1 N1 . . 107.75(18) ? C2 C1 N1 . . 130.7(2) ? C3 C2 C1 . . 117.2(3) ? C3 C2 H2 . . 121.4 ? C1 C2 H2 . . 121.4 ? C4 C3 C2 . . 121.8(2) ? C4 C3 H3 . . 119.1 ? C2 C3 H3 . . 119.1 ? C3 C4 C5 . . 121.4(3) ? C3 C4 H4 . . 119.3 ? C5 C4 H4 . . 119.3 ? C4 C5 C6 . . 118.3(3) ? C4 C5 H5 . . 120.9 ? C6 C5 H5 . . 120.9 ? C1 C6 C5 . . 119.8(2) ? C1 C6 C7 . . 108.3(2) ? C5 C6 C7 . . 131.8(2) ? C8 C7 C6 . . 108.00(19) ? C8 C7 C23 . . 128.0(2) ? C6 C7 C23 . . 123.7(2) ? C7 C8 N1 . . 109.18(18) ? C7 C8 C15 . . 128.9(2) ? N1 C8 C15 . . 121.62(19) ? C10 C9 C14 . . 120.9(2) ? C10 C9 S1 . . 119.18(19) ? C14 C9 S1 . . 119.9(2) ? C9 C10 C11 . . 118.8(3) ? C9 C10 H10 . . 120.6 ? C11 C10 H10 . . 120.6 ? C12 C11 C10 . . 120.3(3) ? C12 C11 H11 . . 119.8 ? C10 C11 H11 . . 119.8 ? C13 C12 C11 . . 120.0(3) ? C13 C12 H12 . . 120.0 ? C11 C12 H12 . . 120.0 ? C14 C13 C12 . . 120.7(3) ? C14 C13 H13 . . 119.7 ? C12 C13 H13 . . 119.7 ? C13 C14 C9 . . 119.3(3) ? C13 C14 H14 . . 120.4 ? C9 C14 H14 . . 120.4 ? C16 C15 C8 . . 122.9(2) ? C16 C15 H15 . . 118.5 ? C8 C15 H15 . . 118.5 ? C15 C16 C17 . . 125.2(2) ? C15 C16 H16 . . 117.4 ? C17 C16 H16 . . 117.4 ? C18 C17 C22 . . 116.61(19) ? C18 C17 C16 . . 121.10(18) ? C22 C17 C16 . . 122.26(19) ? C17 C18 C19 . . 122.0(2) ? C17 C18 H18 . . 119.0 ? C19 C18 H18 . . 119.0 ? O3 C19 C20 . . 125.0(2) ? O3 C19 C18 . . 115.1(2) ? C20 C19 C18 . . 119.9(2) ? C21 C20 C19 . . 119.2(2) ? C21 C20 H20 . . 120.4 ? C19 C20 H20 . . 120.4 ? C22 C21 C20 . . 120.9(2) ? C22 C21 H21 . . 119.5 ? C20 C21 H21 . . 119.5 ? C21 C22 C17 . . 121.4(2) ? C21 C22 Br1 . . 117.89(17) ? C17 C22 Br1 . . 120.70(17) ? C7 C23 H23A . . 109.5 ? C7 C23 H23B . . 109.5 ? H23A C23 H23B . . 109.5 ? C7 C23 H23C . . 109.5 ? H23A C23 H23C . . 109.5 ? H23B C23 H23C . . 109.5 ? O3 C24 H24A . . 109.5 ? O3 C24 H24B . . 109.5 ? H24A C24 H24B . . 109.5 ? O3 C24 H24C . . 109.5 ? H24A C24 H24C . . 109.5 ? H24B C24 H24C . . 109.5 ? C1 N1 C8 . . 106.63(17) ? C1 N1 S1 . . 120.69(15) ? C8 N1 S1 . . 121.31(15) ? C19 O3 C24 . . 117.8(2) ? O1 S1 O2 . . 119.67(12) ? O1 S1 N1 . . 107.06(10) ? O2 S1 N1 . . 105.82(11) ? O1 S1 C9 . . 109.61(12) ? O2 S1 C9 . . 109.65(12) ? N1 S1 C9 . . 103.78(10) ? 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 C1 C6 . 1.393(3) ? C1 C2 . 1.395(3) ? C1 N1 . 1.425(3) ? C2 C3 . 1.382(4) ? C2 H2 . 0.9300 ? C3 C4 . 1.375(4) ? C3 H3 . 0.9300 ? C4 C5 . 1.376(4) ? C4 H4 . 0.9300 ? C5 C6 . 1.401(3) ? C5 H5 . 0.9300 ? C6 C7 . 1.438(3) ? C7 C8 . 1.358(3) ? C7 C23 . 1.498(3) ? C8 N1 . 1.438(3) ? C8 C15 . 1.459(3) ? C9 C10 . 1.378(4) ? C9 C14 . 1.382(3) ? C9 S1 . 1.759(2) ? C10 C11 . 1.383(4) ? C10 H10 . 0.9300 ? C11 C12 . 1.376(5) ? C11 H11 . 0.9300 ? C12 C13 . 1.370(5) ? C12 H12 . 0.9300 ? C13 C14 . 1.368(4) ? C13 H13 . 0.9300 ? C14 H14 . 0.9300 ? C15 C16 . 1.333(3) ? C15 H15 . 0.9300 ? C16 C17 . 1.469(3) ? C16 H16 . 0.9300 ? C17 C18 . 1.389(3) ? C17 C22 . 1.405(3) ? C18 C19 . 1.391(3) ? C18 H18 . 0.9300 ? C19 O3 . 1.360(3) ? C19 C20 . 1.380(3) ? C20 C21 . 1.377(4) ? C20 H20 . 0.9300 ? C21 C22 . 1.374(3) ? C21 H21 . 0.9300 ? C22 Br1 . 1.896(2) ? C23 H23A . 0.9600 ? C23 H23B . 0.9600 ? C23 H23C . 0.9600 ? C24 O3 . 1.421(3) ? C24 H24A . 0.9600 ? C24 H24B . 0.9600 ? C24 H24C . 0.9600 ? N1 S1 . 1.6770(19) ? O1 S1 . 1.4237(19) ? O2 S1 . 1.4269(18) ? 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 _geom_hbond_publ_flag C2 H2 O2 . 0.93 2.39 2.958(4) 119 yes C3 H3 O2 3_665 0.93 2.61 3.448(3) 150 yes C24 H24A Br1 4_466 0.96 3.03 3.699(3) 128 yes C5 H5 Cg(C9--C14) 3_766 0.93 3.12 4.047(3) 173 yes C20 H20 Cg(C17--C22) 4_566 0.93 3.15 3.978(2) 149 yes C23 H23C Cg(C1--C6) 3_766 0.96 3.11 4.036(4) 162 yes 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 C6 C1 C2 C3 . . . . 0.2(4) ? N1 C1 C2 C3 . . . . 178.4(2) ? C1 C2 C3 C4 . . . . -0.6(4) ? C2 C3 C4 C5 . . . . 0.0(4) ? C3 C4 C5 C6 . . . . 0.8(4) ? C2 C1 C6 C5 . . . . 0.6(3) ? N1 C1 C6 C5 . . . . -177.9(2) ? C2 C1 C6 C7 . . . . 179.6(2) ? N1 C1 C6 C7 . . . . 1.0(2) ? C4 C5 C6 C1 . . . . -1.1(4) ? C4 C5 C6 C7 . . . . -179.8(2) ? C1 C6 C7 C8 . . . . 1.2(3) ? C5 C6 C7 C8 . . . . 180.0(3) ? C1 C6 C7 C23 . . . . -173.6(2) ? C5 C6 C7 C23 . . . . 5.2(4) ? C6 C7 C8 N1 . . . . -2.9(2) ? C23 C7 C8 N1 . . . . 171.6(2) ? C6 C7 C8 C15 . . . . -176.6(2) ? C23 C7 C8 C15 . . . . -2.1(4) ? C14 C9 C10 C11 . . . . 0.4(4) ? S1 C9 C10 C11 . . . . -177.1(2) ? C9 C10 C11 C12 . . . . -0.1(5) ? C10 C11 C12 C13 . . . . 0.3(5) ? C11 C12 C13 C14 . . . . -0.8(5) ? C12 C13 C14 C9 . . . . 1.1(4) ? C10 C9 C14 C13 . . . . -0.9(4) ? S1 C9 C14 C13 . . . . 176.6(2) ? C7 C8 C15 C16 . . . . -45.2(3) ? N1 C8 C15 C16 . . . . 141.7(2) ? C8 C15 C16 C17 . . . . 173.14(19) ? C15 C16 C17 C18 . . . . -27.4(3) ? C15 C16 C17 C22 . . . . 154.5(2) ? C22 C17 C18 C19 . . . . 0.2(3) ? C16 C17 C18 C19 . . . . -178.1(2) ? C17 C18 C19 O3 . . . . -179.1(2) ? C17 C18 C19 C20 . . . . 1.2(4) ? O3 C19 C20 C21 . . . . 179.4(2) ? C18 C19 C20 C21 . . . . -0.9(4) ? C19 C20 C21 C22 . . . . -0.7(4) ? C20 C21 C22 C17 . . . . 2.1(4) ? C20 C21 C22 Br1 . . . . -177.9(2) ? C18 C17 C22 C21 . . . . -1.8(3) ? C16 C17 C22 C21 . . . . 176.4(2) ? C18 C17 C22 Br1 . . . . 178.23(15) ? C16 C17 C22 Br1 . . . . -3.6(3) ? C6 C1 N1 C8 . . . . -2.7(2) ? C2 C1 N1 C8 . . . . 178.9(2) ? C6 C1 N1 S1 . . . . -146.59(16) ? C2 C1 N1 S1 . . . . 35.0(3) ? C7 C8 N1 C1 . . . . 3.5(2) ? C15 C8 N1 C1 . . . . 177.77(19) ? C7 C8 N1 S1 . . . . 147.12(16) ? C15 C8 N1 S1 . . . . -38.6(3) ? C20 C19 O3 C24 . . . . 1.6(4) ? C18 C19 O3 C24 . . . . -178.1(3) ? C1 N1 S1 O1 . . . . -175.43(16) ? C8 N1 S1 O1 . . . . 45.94(19) ? C1 N1 S1 O2 . . . . -46.74(19) ? C8 N1 S1 O2 . . . . 174.62(17) ? C1 N1 S1 C9 . . . . 68.69(18) ? C8 N1 S1 C9 . . . . -69.95(18) ? C10 C9 S1 O1 . . . . -23.7(2) ? C14 C9 S1 O1 . . . . 158.74(19) ? C10 C9 S1 O2 . . . . -157.0(2) ? C14 C9 S1 O2 . . . . 25.5(2) ? C10 C9 S1 N1 . . . . 90.3(2) ? C14 C9 S1 N1 . . . . -87.2(2) ?