#============================================================================= data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 15 _journal_issue 2 _journal_year 2024 _journal_page_first 155 _journal_page_last 165 #============================================================================= data_shelx _audit_creation_date 2024-03-18 _audit_creation_method ; Olex2 1.3-beta (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C14 H9 Br3 N2 O S' _chemical_formula_sum 'C14 H9 Br3 N2 O S' _chemical_formula_weight 493.02 _chemical_melting_point ? 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' _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. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.0437(13) _cell_length_b 37.021(6) _cell_length_c 10.7842(15) _cell_angle_alpha 90 _cell_angle_beta 90.936(5) _cell_angle_gamma 90 _cell_volume 3210.9(8) _cell_formula_units_Z 8 _cell_measurement_reflns_used 9874 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.03 _cell_measurement_theta_min 3.14 _exptl_absorpt_coefficient_mu 7.666 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.3407 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 2.040 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description prism _exptl_crystal_F_000 1888 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.1432 _diffrn_reflns_av_unetI/netI 0.1346 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_k_min -45 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 36579 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.997 _diffrn_reflns_theta_min 2.900 _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3337 _reflns_number_total 6301 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Olex2 1.3-beta (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-beta (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _refine_diff_density_max 1.158 _refine_diff_density_min -0.915 _refine_diff_density_rms 0.180 _refine_ls_extinction_coef 0.0019(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 1.108 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 380 _refine_ls_number_reflns 6301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1940 _refine_ls_R_factor_gt 0.0989 _refine_ls_restrained_S_all 1.108 _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^)+86.5914P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1802 _refine_ls_wR_factor_ref 0.2171 _refine_special_details ? _olex2_refinement_description ; 1.a Aromatic/amide H refined with riding coordinates: C2(H2), C4(H4), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C18(H18), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), N1(H1), N2(H22), N3(H33), N4(H44) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7045(17) 0.5616(3) 0.0469(13) 0.026(3) Uani 1 1 d . . . . . C2 C 0.736(2) 0.5258(3) 0.0779(15) 0.040(4) Uani 1 1 d . . . . . H2 H 0.6560 0.5082 0.0624 0.048 Uiso 1 1 calc R U . . . C3 C 0.8854(18) 0.5166(4) 0.1314(15) 0.035(4) Uani 1 1 d . . . . . C4 C 1.0090(16) 0.5431(3) 0.1574(14) 0.030(3) Uani 1 1 d . . . . . H4 H 1.1106 0.5368 0.1938 0.036 Uiso 1 1 calc R U . . . C5 C 0.9722(17) 0.5795(3) 0.1261(14) 0.030(3) Uani 1 1 d . . . . . C6 C 0.827(2) 0.5879(3) 0.0706(14) 0.035(4) Uani 1 1 d . . . . . C7 C 0.819(2) 0.6393(4) -0.0686(14) 0.037(4) Uani 1 1 d . . . . . C8 C 0.749(2) 0.7011(4) 0.0126(17) 0.039(4) Uani 1 1 d . . . . . C9 C 0.724(2) 0.7387(3) -0.0293(15) 0.038(4) Uani 1 1 d . . . . . C10 C 0.638(2) 0.7467(4) -0.1409(19) 0.063(5) Uani 1 1 d . . . . . H10 H 0.5993 0.7284 -0.1931 0.075 Uiso 1 1 calc R U . . . C11 C 0.611(3) 0.7837(5) -0.171(2) 0.094(8) Uani 1 1 d . . . . . H11 H 0.5503 0.7905 -0.2414 0.112 Uiso 1 1 calc R U . . . C12 C 0.681(4) 0.8101(5) -0.090(2) 0.116(12) Uani 1 1 d . . . . . H12 H 0.6864 0.8341 -0.1152 0.140 Uiso 1 1 calc R U . . . C13 C 0.735(4) 0.8020(5) 0.013(2) 0.095(8) Uani 1 1 d . . . . . H13 H 0.7576 0.8203 0.0703 0.114 Uiso 1 1 calc R U . . . C14 C 0.765(3) 0.7657(4) 0.0490(19) 0.085(8) Uani 1 1 d . . . . . H14 H 0.8131 0.7606 0.1261 0.102 Uiso 1 1 calc R U . . . C15 C 0.514(2) 0.5768(4) 0.6266(14) 0.037(4) Uani 1 1 d . . . . . C16 C 0.492(2) 0.5429(4) 0.6570(14) 0.039(4) Uani 1 1 d . . . . . H16 H 0.3949 0.5362 0.6959 0.047 Uiso 1 1 calc R U . . . C17 C 0.6106(19) 0.5170(4) 0.6328(14) 0.036(4) Uani 1 1 d . . . . . C18 C 0.754(2) 0.5265(3) 0.5750(15) 0.040(4) Uani 1 1 d . . . . . H18 H 0.8336 0.5092 0.5570 0.048 Uiso 1 1 calc R U . . . C19 C 0.7784(19) 0.5632(4) 0.5430(14) 0.037(4) Uani 1 1 d . . . . . C20 C 0.661(2) 0.5890(3) 0.5682(14) 0.034(4) Uani 1 1 d . . . . . C21 C 0.657(2) 0.6406(3) 0.4313(14) 0.035(4) Uani 1 1 d . . . . . C22 C 0.7302(19) 0.7018(4) 0.5157(16) 0.037(4) Uani 1 1 d . . . . . C23 C 0.737(2) 0.7411(4) 0.4808(15) 0.044(4) Uani 1 1 d . . . . . C24 C 0.651(2) 0.7547(4) 0.3767(18) 0.059(5) Uani 1 1 d . . . . . H24 H 0.5886 0.7393 0.3256 0.071 Uiso 1 1 calc R U . . . C25 C 0.659(3) 0.7917(4) 0.351(2) 0.081(7) Uani 1 1 d . . . . . H25 H 0.6070 0.8012 0.2809 0.098 Uiso 1 1 calc R U . . . C26 C 0.745(3) 0.8139(5) 0.431(2) 0.081(7) Uani 1 1 d . . . . . H26 H 0.7558 0.8382 0.4111 0.097 Uiso 1 1 calc R U . . . C27 C 0.814(3) 0.8017(4) 0.534(2) 0.078(7) Uani 1 1 d . . . . . H27 H 0.8665 0.8176 0.5893 0.094 Uiso 1 1 calc R U . . . C28 C 0.809(3) 0.7651(4) 0.5606(18) 0.062(6) Uani 1 1 d . . . . . H28 H 0.8550 0.7568 0.6348 0.074 Uiso 1 1 calc R U . . . N1 N 0.7923(17) 0.6247(3) 0.0426(11) 0.042(3) Uani 1 1 d . . . . . H1 H 0.7521 0.6381 0.0999 0.050 Uiso 1 1 calc R U . . . N2 N 0.7786(17) 0.6764(3) -0.0786(12) 0.043(3) Uani 1 1 d . . . . . H22 H 0.7721 0.6847 -0.1531 0.051 Uiso 1 1 calc R U . . . N3 N 0.6930(17) 0.6266(3) 0.5399(11) 0.041(3) Uani 1 1 d . . . . . H33 H 0.7373 0.6401 0.5962 0.049 Uiso 1 1 calc R U . . . N4 N 0.6948(16) 0.6783(3) 0.4242(12) 0.041(3) Uani 1 1 d . . . . . H44 H 0.6947 0.6872 0.3506 0.050 Uiso 1 1 calc R U . . . O1 O 0.7453(15) 0.6924(3) 0.1216(11) 0.049(3) Uani 1 1 d . . . . . O2 O 0.7534(16) 0.6924(3) 0.6232(10) 0.053(3) Uani 1 1 d . . . . . S1 S 0.8966(6) 0.61797(10) -0.1879(4) 0.0520(12) Uani 1 1 d . . . . . S2 S 0.5698(7) 0.62064(10) 0.3108(4) 0.0543(13) Uani 1 1 d . . . . . Br1 Br 0.4973(2) 0.57327(5) -0.02085(19) 0.0599(6) Uani 1 1 d . . . . . Br2 Br 0.9343(2) 0.46818(4) 0.17331(17) 0.0483(5) Uani 1 1 d . . . . . Br3 Br 1.1352(2) 0.61346(4) 0.16190(19) 0.0569(6) Uani 1 1 d . . . . . Br4 Br 0.3532(3) 0.61185(5) 0.6681(2) 0.0650(6) Uani 1 1 d . . . . . Br5 Br 0.5727(2) 0.46827(4) 0.67290(16) 0.0468(5) Uani 1 1 d . . . . . Br6 Br 0.9836(3) 0.57606(5) 0.4702(2) 0.0656(6) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.025(8) 0.024(7) 0.031(9) -0.001(6) -0.009(6) 0.013(6) C2 0.047(10) 0.023(7) 0.049(10) -0.003(7) -0.005(8) -0.008(7) C3 0.029(9) 0.033(8) 0.045(10) 0.008(7) 0.001(7) 0.002(7) C4 0.017(8) 0.027(7) 0.045(10) 0.008(6) -0.010(7) 0.002(6) C5 0.029(8) 0.018(6) 0.043(9) 0.010(6) 0.001(7) 0.005(6) C6 0.051(10) 0.020(7) 0.035(9) 0.003(6) 0.005(8) -0.006(6) C7 0.051(10) 0.027(7) 0.033(10) -0.001(7) -0.008(8) 0.006(7) C8 0.046(10) 0.020(7) 0.052(12) -0.005(7) -0.003(8) 0.008(7) C9 0.054(11) 0.019(7) 0.041(10) 0.004(6) 0.007(8) 0.003(6) C10 0.085(15) 0.027(8) 0.076(15) 0.007(9) 0.005(12) 0.004(9) C11 0.15(2) 0.040(11) 0.088(18) 0.012(11) 0.010(16) 0.036(13) C12 0.26(4) 0.023(10) 0.067(18) 0.011(11) 0.03(2) 0.017(15) C13 0.17(3) 0.031(10) 0.084(19) -0.004(11) 0.027(18) -0.019(13) C14 0.18(2) 0.027(9) 0.052(13) -0.016(8) -0.012(14) 0.021(12) C15 0.062(11) 0.023(7) 0.026(9) -0.003(6) -0.013(8) 0.004(7) C16 0.044(10) 0.037(8) 0.035(10) 0.006(7) 0.010(8) -0.011(7) C17 0.042(10) 0.029(7) 0.036(10) 0.009(7) -0.002(8) 0.002(7) C18 0.048(10) 0.023(7) 0.050(10) -0.001(7) 0.000(8) 0.000(7) C19 0.038(10) 0.035(8) 0.038(10) 0.007(7) 0.016(7) -0.005(7) C20 0.058(11) 0.009(6) 0.036(9) 0.002(6) 0.005(8) -0.003(6) C21 0.057(11) 0.014(6) 0.032(9) 0.000(6) 0.001(8) -0.008(6) C22 0.044(10) 0.023(7) 0.045(11) 0.003(7) -0.002(8) 0.002(7) C23 0.056(11) 0.028(8) 0.046(11) 0.013(7) -0.012(9) -0.019(7) C24 0.078(14) 0.037(9) 0.062(13) -0.003(9) 0.011(11) 0.002(9) C25 0.16(2) 0.021(9) 0.066(15) 0.005(9) -0.005(14) 0.029(11) C26 0.15(2) 0.026(9) 0.069(16) 0.008(10) 0.009(14) 0.009(12) C27 0.15(2) 0.015(8) 0.073(16) -0.012(9) 0.018(14) -0.020(10) C28 0.109(17) 0.022(8) 0.054(13) -0.002(8) 0.011(11) 0.008(9) N1 0.077(10) 0.021(6) 0.027(8) 0.003(5) -0.008(7) 0.014(6) N2 0.073(10) 0.020(6) 0.035(8) -0.002(6) -0.006(7) 0.011(6) N3 0.076(10) 0.017(6) 0.030(8) 0.003(5) -0.011(7) -0.015(6) N4 0.064(10) 0.026(6) 0.034(8) 0.005(6) 0.005(7) -0.013(6) O1 0.084(9) 0.028(5) 0.036(7) -0.003(5) 0.004(6) 0.001(5) O2 0.100(10) 0.026(5) 0.033(7) 0.001(5) -0.007(7) -0.010(6) S1 0.091(4) 0.030(2) 0.035(3) -0.0004(17) 0.000(2) 0.015(2) S2 0.092(4) 0.032(2) 0.038(3) 0.0021(18) -0.012(2) -0.021(2) Br1 0.0560(12) 0.0469(10) 0.0760(14) 0.0048(9) -0.0230(10) 0.0107(8) Br2 0.0597(12) 0.0244(7) 0.0607(12) 0.0125(7) -0.0022(9) 0.0067(7) Br3 0.0603(12) 0.0375(9) 0.0726(14) -0.0010(8) -0.0036(10) -0.0175(8) Br4 0.0722(14) 0.0384(9) 0.0846(16) 0.0101(9) 0.0086(11) 0.0215(9) Br5 0.0585(12) 0.0266(7) 0.0551(12) 0.0125(7) -0.0048(9) -0.0049(7) Br6 0.0636(13) 0.0575(11) 0.0763(15) 0.0048(10) 0.0216(11) -0.0173(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.392(18) . ? C1 C6 1.409(19) . ? C1 Br1 1.859(13) . ? C2 H2 0.9300 . ? C2 C3 1.37(2) . ? C3 C4 1.423(19) . ? C3 Br2 1.887(14) . ? C4 H4 0.9300 . ? C4 C5 1.418(17) . ? C5 C6 1.34(2) . ? C5 Br3 1.854(14) . ? C6 N1 1.421(17) . ? C7 N1 1.336(19) . ? C7 N2 1.414(17) . ? C7 S1 1.643(16) . ? C8 C9 1.478(19) . ? C8 N2 1.367(19) . ? C8 O1 1.219(18) . ? C9 C10 1.41(2) . ? C9 C14 1.35(2) . ? C10 H10 0.9300 . ? C10 C11 1.42(2) . ? C11 H11 0.9300 . ? C11 C12 1.42(3) . ? C12 H12 0.9300 . ? C12 C13 1.22(3) . ? C13 H13 0.9300 . ? C13 C14 1.42(3) . ? C14 H14 0.9300 . ? C15 C16 1.309(19) . ? C15 C20 1.42(2) . ? C15 Br4 1.889(15) . ? C16 H16 0.9300 . ? C16 C17 1.38(2) . ? C17 C18 1.36(2) . ? C17 Br5 1.882(14) . ? C18 H18 0.9300 . ? C18 C19 1.416(18) . ? C19 C20 1.38(2) . ? C19 Br6 1.900(14) . ? C20 N3 1.448(16) . ? C21 N3 1.309(18) . ? C21 N4 1.430(16) . ? C21 S2 1.643(15) . ? C22 C23 1.505(19) . ? C22 N4 1.341(19) . ? C22 O2 1.222(18) . ? C23 C24 1.40(2) . ? C23 C28 1.36(2) . ? C24 H24 0.9300 . ? C24 C25 1.40(2) . ? C25 H25 0.9300 . ? C25 C26 1.37(3) . ? C26 H26 0.9300 . ? C26 C27 1.32(3) . ? C27 H27 0.9300 . ? C27 C28 1.39(2) . ? C28 H28 0.9300 . ? N1 H1 0.8600 . ? N2 H22 0.8600 . ? N3 H33 0.8600 . ? N4 H44 0.8600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 119.4(13) . . ? C2 C1 Br1 118.3(11) . . ? C6 C1 Br1 122.2(10) . . ? C1 C2 H2 120.2 . . ? C3 C2 C1 119.7(13) . . ? C3 C2 H2 120.2 . . ? C2 C3 C4 121.2(13) . . ? C2 C3 Br2 121.0(11) . . ? C4 C3 Br2 117.8(10) . . ? C3 C4 H4 121.1 . . ? C5 C4 C3 117.8(12) . . ? C5 C4 H4 121.1 . . ? C4 C5 Br3 116.8(10) . . ? C6 C5 C4 120.4(13) . . ? C6 C5 Br3 122.8(10) . . ? C1 C6 N1 119.1(13) . . ? C5 C6 C1 121.5(12) . . ? C5 C6 N1 119.3(13) . . ? N1 C7 N2 115.0(13) . . ? N1 C7 S1 125.2(11) . . ? N2 C7 S1 119.8(12) . . ? N2 C8 C9 115.7(15) . . ? O1 C8 C9 122.6(14) . . ? O1 C8 N2 121.6(13) . . ? C10 C9 C8 121.4(14) . . ? C14 C9 C8 118.5(16) . . ? C14 C9 C10 119.5(15) . . ? C9 C10 H10 121.1 . . ? C9 C10 C11 117.8(18) . . ? C11 C10 H10 121.1 . . ? C10 C11 H11 121.2 . . ? C10 C11 C12 118(2) . . ? C12 C11 H11 121.2 . . ? C11 C12 H12 119.2 . . ? C13 C12 C11 122(2) . . ? C13 C12 H12 119.2 . . ? C12 C13 H13 118.8 . . ? C12 C13 C14 122(2) . . ? C14 C13 H13 118.8 . . ? C9 C14 C13 120(2) . . ? C9 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C16 C15 C20 122.0(14) . . ? C16 C15 Br4 120.3(13) . . ? C20 C15 Br4 117.6(10) . . ? C15 C16 H16 119.2 . . ? C15 C16 C17 121.7(15) . . ? C17 C16 H16 119.2 . . ? C16 C17 Br5 120.6(12) . . ? C18 C17 C16 119.9(13) . . ? C18 C17 Br5 119.5(11) . . ? C17 C18 H18 120.7 . . ? C17 C18 C19 118.7(14) . . ? C19 C18 H18 120.7 . . ? C18 C19 Br6 117.9(11) . . ? C20 C19 C18 121.3(14) . . ? C20 C19 Br6 120.8(10) . . ? C15 C20 N3 123.5(13) . . ? C19 C20 C15 116.5(12) . . ? C19 C20 N3 119.9(14) . . ? N3 C21 N4 113.1(12) . . ? N3 C21 S2 127.8(10) . . ? N4 C21 S2 119.0(11) . . ? N4 C22 C23 116.8(14) . . ? O2 C22 C23 120.5(14) . . ? O2 C22 N4 122.7(13) . . ? C24 C23 C22 121.7(14) . . ? C28 C23 C22 119.5(15) . . ? C28 C23 C24 118.2(14) . . ? C23 C24 H24 120.7 . . ? C25 C24 C23 118.7(18) . . ? C25 C24 H24 120.7 . . ? C24 C25 H25 120.3 . . ? C26 C25 C24 119.5(19) . . ? C26 C25 H25 120.3 . . ? C25 C26 H26 119.1 . . ? C27 C26 C25 121.9(17) . . ? C27 C26 H26 119.1 . . ? C26 C27 H27 120.2 . . ? C26 C27 C28 119.5(19) . . ? C28 C27 H27 120.2 . . ? C23 C28 C27 121.7(19) . . ? C23 C28 H28 119.1 . . ? C27 C28 H28 119.1 . . ? C6 N1 H1 118.5 . . ? C7 N1 C6 123.0(12) . . ? C7 N1 H1 118.5 . . ? C7 N2 H22 115.2 . . ? C8 N2 C7 129.5(13) . . ? C8 N2 H22 115.2 . . ? C20 N3 H33 118.9 . . ? C21 N3 C20 122.2(12) . . ? C21 N3 H33 118.9 . . ? C21 N4 H44 115.3 . . ? C22 N4 C21 129.4(13) . . ? C22 N4 H44 115.3 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C4 H4 Br5 0.93 2.91 3.827(13) 168.6 3_766 C16 H16 Br2 0.93 3.02 3.937(16) 167.4 3_666 N2 H22 O2 0.86 2.43 3.273(17) 165.9 1_554 N3 H33 S1 0.86 2.76 3.353(13) 127.2 1_556 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 C3 C4 1(2) . . . . ? C1 C2 C3 Br2 -179.3(12) . . . . ? C1 C6 N1 C7 -88.0(19) . . . . ? C2 C1 C6 C5 -2(2) . . . . ? C2 C1 C6 N1 -177.8(14) . . . . ? C2 C3 C4 C5 0(2) . . . . ? C3 C4 C5 C6 -2(2) . . . . ? C3 C4 C5 Br3 179.7(11) . . . . ? C4 C5 C6 C1 3(2) . . . . ? C4 C5 C6 N1 178.7(14) . . . . ? C5 C6 N1 C7 96.2(19) . . . . ? C6 C1 C2 C3 0(2) . . . . ? C8 C9 C10 C11 176.4(18) . . . . ? C8 C9 C14 C13 -177(2) . . . . ? C9 C8 N2 C7 174.9(15) . . . . ? C9 C10 C11 C12 3(3) . . . . ? C10 C9 C14 C13 -6(3) . . . . ? C10 C11 C12 C13 -13(4) . . . . ? C11 C12 C13 C14 14(5) . . . . ? C12 C13 C14 C9 -4(4) . . . . ? C14 C9 C10 C11 6(3) . . . . ? C15 C16 C17 C18 0(2) . . . . ? C15 C16 C17 Br5 -177.9(12) . . . . ? C15 C20 N3 C21 -94.5(19) . . . . ? C16 C15 C20 C19 1(2) . . . . ? C16 C15 C20 N3 -176.2(14) . . . . ? C16 C17 C18 C19 1(2) . . . . ? C17 C18 C19 C20 -1(2) . . . . ? C17 C18 C19 Br6 176.9(12) . . . . ? C18 C19 C20 C15 -1(2) . . . . ? C18 C19 C20 N3 177.0(14) . . . . ? C19 C20 N3 C21 88(2) . . . . ? C20 C15 C16 C17 -1(2) . . . . ? C22 C23 C24 C25 178.5(18) . . . . ? C22 C23 C28 C27 -178.3(18) . . . . ? C23 C22 N4 C21 -170.4(15) . . . . ? C23 C24 C25 C26 -3(3) . . . . ? C24 C23 C28 C27 -8(3) . . . . ? C24 C25 C26 C27 -3(4) . . . . ? C25 C26 C27 C28 4(4) . . . . ? C26 C27 C28 C23 2(3) . . . . ? C28 C23 C24 C25 8(3) . . . . ? N1 C7 N2 C8 14(2) . . . . ? N2 C7 N1 C6 -179.1(14) . . . . ? N2 C8 C9 C10 38(2) . . . . ? N2 C8 C9 C14 -151.5(18) . . . . ? N3 C21 N4 C22 -14(2) . . . . ? N4 C21 N3 C20 178.2(13) . . . . ? N4 C22 C23 C24 25(2) . . . . ? N4 C22 C23 C28 -164.9(17) . . . . ? O1 C8 C9 C10 -143.6(18) . . . . ? O1 C8 C9 C14 27(3) . . . . ? O1 C8 N2 C7 -4(3) . . . . ? O2 C22 C23 C24 -154.2(17) . . . . ? O2 C22 C23 C28 16(3) . . . . ? O2 C22 N4 C21 9(3) . . . . ? S1 C7 N1 C6 -1(2) . . . . ? S1 C7 N2 C8 -163.9(14) . . . . ? S2 C21 N3 C20 1(2) . . . . ? S2 C21 N4 C22 163.5(14) . . . . ? Br1 C1 C2 C3 -178.0(12) . . . . ? Br1 C1 C6 C5 176.0(12) . . . . ? Br1 C1 C6 N1 0(2) . . . . ? Br2 C3 C4 C5 -179.9(11) . . . . ? Br3 C5 C6 C1 -178.7(11) . . . . ? Br3 C5 C6 N1 -3(2) . . . . ? Br4 C15 C16 C17 -177.1(12) . . . . ? Br4 C15 C20 C19 177.7(11) . . . . ? Br4 C15 C20 N3 0(2) . . . . ? Br5 C17 C18 C19 178.6(12) . . . . ? Br6 C19 C20 C15 -177.9(11) . . . . ? Br6 C19 C20 N3 0(2) . . . . ? _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL fatma1_0m_a.res in P2(1)/n CELL 0.71073 8.0437 37.0206 10.7842 90.000 90.936 90.000 ZERR 8.00 0.0013 0.0055 0.0015 0.000 0.005 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O S BR UNIT 112 72 16 8 8 24 MERG 2 OMIT -4.00 52.00 FMAP 2 PLAN 5 ACTA BOND BOND $H HTAB CONF EQIV $1 -x+2, -y+1, -z+1 EQIV $2 x, y, z-1 EQIV $3 -x+1, -y+1, -z+1 EQIV $4 x, y, z+1 HTAB C4 Br5_$1 HTAB C16 Br2_$3 HTAB N2 O2_$2 HTAB N3 S1_$4 L.S. 10 WGHT 0.000000 86.591362 EXTI 0.001908 FVAR 0.17397 C1 1 0.704484 0.561629 0.046851 11.00000 0.02458 0.02407 = 0.03054 -0.00136 -0.00860 0.01272 C2 1 0.736052 0.525769 0.077945 11.00000 0.04741 0.02274 = 0.04947 -0.00324 -0.00504 -0.00802 AFIX 43 H2 2 0.655959 0.508152 0.062419 11.00000 -1.20000 AFIX 0 C3 1 0.885402 0.516564 0.131433 11.00000 0.02879 0.03265 = 0.04498 0.00765 0.00125 0.00239 C4 1 1.009038 0.543113 0.157434 11.00000 0.01700 0.02695 = 0.04518 0.00836 -0.00991 0.00194 AFIX 43 H4 2 1.110611 0.536832 0.193796 11.00000 -1.20000 AFIX 0 C5 1 0.972199 0.579457 0.126056 11.00000 0.02906 0.01847 = 0.04284 0.01012 0.00077 0.00484 C6 1 0.827461 0.587943 0.070626 11.00000 0.05120 0.02050 = 0.03468 0.00311 0.00488 -0.00647 C7 1 0.818762 0.639327 -0.068576 11.00000 0.05060 0.02659 = 0.03256 -0.00106 -0.00802 0.00649 C8 1 0.748508 0.701071 0.012645 11.00000 0.04594 0.01976 = 0.05226 -0.00519 -0.00274 0.00802 C9 1 0.724015 0.738734 -0.029339 11.00000 0.05374 0.01888 = 0.04060 0.00353 0.00716 0.00307 C10 1 0.637645 0.746729 -0.140949 11.00000 0.08550 0.02668 = 0.07571 0.00653 0.00545 0.00421 AFIX 43 H10 2 0.599287 0.728425 -0.193094 11.00000 -1.20000 AFIX 0 C11 1 0.611203 0.783748 -0.171042 11.00000 0.15401 0.03955 = 0.08778 0.01159 0.01026 0.03565 AFIX 43 H11 2 0.550289 0.790471 -0.241357 11.00000 -1.20000 AFIX 0 C12 1 0.681437 0.810104 -0.089541 11.00000 0.26068 0.02272 = 0.06651 0.01100 0.03480 0.01661 AFIX 43 H12 2 0.686408 0.834059 -0.115187 11.00000 -1.20000 AFIX 0 C13 1 0.735362 0.801972 0.013380 11.00000 0.17032 0.03058 = 0.08399 -0.00388 0.02655 -0.01937 AFIX 43 H13 2 0.757563 0.820280 0.070334 11.00000 -1.20000 AFIX 0 C14 1 0.765253 0.765718 0.049049 11.00000 0.17553 0.02726 = 0.05158 -0.01560 -0.01213 0.02139 AFIX 43 H14 2 0.813069 0.760569 0.126136 11.00000 -1.20000 AFIX 0 C15 1 0.513814 0.576831 0.626565 11.00000 0.06165 0.02275 = 0.02571 -0.00337 -0.01285 0.00395 C16 1 0.492366 0.542937 0.656987 11.00000 0.04449 0.03706 = 0.03547 0.00614 0.00954 -0.01059 AFIX 43 H16 2 0.394868 0.536164 0.695914 11.00000 -1.20000 AFIX 0 C17 1 0.610573 0.517027 0.632808 11.00000 0.04236 0.02932 = 0.03584 0.00866 -0.00163 0.00192 C18 1 0.753732 0.526463 0.575006 11.00000 0.04757 0.02280 = 0.04985 -0.00086 -0.00048 0.00006 AFIX 43 H18 2 0.833560 0.509152 0.556983 11.00000 -1.20000 AFIX 0 C19 1 0.778394 0.563153 0.542978 11.00000 0.03783 0.03481 = 0.03846 0.00715 0.01649 -0.00540 C20 1 0.660595 0.589014 0.568224 11.00000 0.05783 0.00875 = 0.03588 0.00170 0.00491 -0.00349 C21 1 0.657252 0.640623 0.431303 11.00000 0.05746 0.01381 = 0.03234 -0.00041 0.00115 -0.00792 C22 1 0.730162 0.701789 0.515670 11.00000 0.04425 0.02279 = 0.04498 0.00255 -0.00197 0.00240 C23 1 0.737187 0.741115 0.480803 11.00000 0.05642 0.02815 = 0.04626 0.01333 -0.01176 -0.01866 C24 1 0.650570 0.754652 0.376695 11.00000 0.07773 0.03747 = 0.06217 -0.00297 0.01051 0.00194 AFIX 43 H24 2 0.588597 0.739325 0.325618 11.00000 -1.20000 AFIX 0 C25 1 0.659372 0.791722 0.351292 11.00000 0.15726 0.02113 = 0.06569 0.00524 -0.00526 0.02947 AFIX 43 H25 2 0.606991 0.801162 0.280935 11.00000 -1.20000 AFIX 0 C26 1 0.745489 0.813889 0.430670 11.00000 0.14891 0.02609 = 0.06851 0.00840 0.00925 0.00876 AFIX 43 H26 2 0.755779 0.838241 0.411066 11.00000 -1.20000 AFIX 0 C27 1 0.814410 0.801730 0.534272 11.00000 0.14619 0.01542 = 0.07330 -0.01204 0.01831 -0.02018 AFIX 43 H27 2 0.866488 0.817606 0.589294 11.00000 -1.20000 AFIX 0 C28 1 0.808677 0.765117 0.560574 11.00000 0.10903 0.02200 = 0.05434 -0.00192 0.01112 0.00776 AFIX 43 H28 2 0.854987 0.756767 0.634775 11.00000 -1.20000 AFIX 0 N1 3 0.792272 0.624677 0.042625 11.00000 0.07732 0.02056 = 0.02710 0.00288 -0.00780 0.01428 AFIX 43 H1 2 0.752064 0.638110 0.099876 11.00000 -1.20000 AFIX 0 N2 3 0.778557 0.676408 -0.078626 11.00000 0.07318 0.01960 = 0.03459 -0.00222 -0.00592 0.01124 AFIX 43 H22 2 0.772057 0.684655 -0.153099 11.00000 -1.20000 AFIX 0 N3 3 0.693028 0.626556 0.539868 11.00000 0.07600 0.01733 = 0.02966 0.00324 -0.01118 -0.01532 AFIX 43 H33 2 0.737286 0.640071 0.596241 11.00000 -1.20000 AFIX 0 N4 3 0.694807 0.678326 0.424213 11.00000 0.06412 0.02637 = 0.03382 0.00455 0.00458 -0.01259 AFIX 43 H44 2 0.694703 0.687249 0.350584 11.00000 -1.20000 AFIX 0 O1 4 0.745333 0.692386 0.121582 11.00000 0.08400 0.02751 = 0.03597 -0.00286 0.00419 0.00118 O2 4 0.753415 0.692368 0.623185 11.00000 0.10009 0.02637 = 0.03311 0.00129 -0.00712 -0.00970 S1 5 0.896616 0.617969 -0.187887 11.00000 0.09055 0.03001 = 0.03543 -0.00037 -0.00044 0.01500 S2 5 0.569781 0.620639 0.310838 11.00000 0.09236 0.03203 = 0.03797 0.00206 -0.01185 -0.02096 BR1 6 0.497254 0.573268 -0.020850 11.00000 0.05604 0.04685 = 0.07598 0.00485 -0.02296 0.01067 BR2 6 0.934267 0.468182 0.173308 11.00000 0.05970 0.02440 = 0.06069 0.01249 -0.00222 0.00665 BR3 6 1.135209 0.613457 0.161895 11.00000 0.06033 0.03754 = 0.07260 -0.00097 -0.00359 -0.01755 BR4 6 0.353199 0.611845 0.668084 11.00000 0.07220 0.03842 = 0.08455 0.01007 0.00861 0.02154 BR5 6 0.572672 0.468270 0.672903 11.00000 0.05848 0.02663 = 0.05510 0.01254 -0.00482 -0.00486 BR6 6 0.983594 0.576064 0.470190 11.00000 0.06358 0.05751 = 0.07629 0.00481 0.02159 -0.01729 HKLF 4 REM fatma1_0m_a.res in P2(1)/n REM R1 = 0.0989 for 3337 Fo > 4sig(Fo) and 0.1940 for all 6301 data REM 380 parameters refined using 0 restraints END WGHT 0.0000 86.5911 REM Instructions for potential hydrogen bonds HTAB C4 Br5_$1 HTAB C16 Br2_$3 HTAB N1 O1 HTAB N1 S2 HTAB N2 O2_$2 HTAB N3 O2 HTAB N3 S1_$4 HTAB N4 O1 REM Highest difference peak 1.158, deepest hole -0.915, 1-sigma level 0.180 Q1 1 1.0437 0.4680 0.1734 11.00000 0.05 1.16 Q2 1 0.5816 0.4718 0.7650 11.00000 0.05 1.07 Q3 1 0.3560 0.6148 0.5821 11.00000 0.05 1.05 Q4 1 1.0366 0.6177 0.1708 11.00000 0.05 0.98 Q5 1 0.5148 0.4324 0.6714 11.00000 0.05 0.96 ; _shelx_res_checksum 71042 _shelx_hkl_file ; -2 0 0 88.19 11.70 -2 0 0 80.29 10.90 2 0 0 92.99 11.50 2 0 0 93.19 11.00 -3 0 0 -8.90 6.20 -3 0 0 -9.30 6.80 3 0 0 -9.80 6.50 3 0 0 0.40 5.80 -4 0 0 52.09 12.90 -4 0 0 59.99 12.20 4 0 0 60.69 11.60 4 0 0 68.69 12.90 5 0 0 -5.00 9.70 -6 0 0 13.40 14.50 -6 0 0 32.20 15.80 6 0 0 10.50 14.70 6 0 0 20.00 14.00 -7 0 0 -14.20 18.10 7 0 0 -17.40 15.50 -8 0 0 77.79 20.80 -8 0 0 51.69 19.60 -8 0 0 -7.20 25.80 8 0 0 36.60 17.90 8 0 0 16.50 16.90 -9 0 0 18.40 22.20 9 0 0 -19.00 21.90 -10 0 0 86.79 27.60 -10 1 0 76.29 25.40 9 -1 0 -23.00 29.50 8 -1 0 -13.80 20.60 8 -1 0 -22.40 15.60 -8 1 0 -35.10 19.70 -8 1 0 32.60 24.50 7 -1 0 -17.60 13.40 7 -1 0 -15.90 15.60 -7 1 0 3.40 18.60 -7 1 0 -9.20 17.60 6 -1 0 4.20 14.70 6 -1 0 12.60 13.30 -6 1 0 15.90 15.60 -6 1 0 14.80 14.40 5 -1 0 30.00 10.40 -5 1 0 15.00 11.70 4 -1 0 -12.00 8.30 4 -1 0 0.60 7.70 -4 1 0 -9.20 9.20 -4 1 0 -15.80 8.20 3 -1 0 -2.50 6.50 3 -1 0 -3.60 6.20 -3 1 0 -13.10 6.40 -3 1 0 -4.50 7.00 2 -1 0 90.89 11.10 2 -1 0 103.79 12.00 -2 1 0 93.19 12.20 -2 1 0 98.69 11.90 -2 -1 0 111.19 12.60 -2 -1 0 93.79 12.60 2 1 0 89.89 12.10 2 1 0 93.09 11.70 -3 -1 0 -6.00 6.90 3 1 0 -0.40 5.90 3 1 0 -11.30 7.20 -4 -1 0 -10.60 8.80 4 1 0 -7.70 7.90 -5 -1 0 22.10 12.70 5 1 0 27.50 12.60 -6 -1 0 34.90 16.10 -6 -1 0 24.60 16.40 6 1 0 13.70 13.00 6 1 0 -3.70 12.90 -7 -1 0 1.00 17.60 -7 -1 0 2.80 18.50 7 1 0 -10.90 18.50 -8 -1 0 16.30 18.40 8 1 0 -16.00 19.40 8 1 0 7.10 18.00 -9 -1 0 45.70 31.20 9 1 0 -38.80 22.90 -10 -1 0 -18.50 25.60 10 -2 0 88.29 46.60 -10 2 0 154.88 64.69 9 -2 0 -14.50 23.00 -9 2 0 66.69 24.40 8 -2 0 -34.20 19.60 8 -2 0 -13.40 16.30 -8 2 0 18.40 18.70 7 -2 0 -14.60 13.70 7 -2 0 -0.80 21.20 -7 2 0 -23.40 17.50 -7 2 0 -16.50 19.10 6 -2 0 -12.30 11.60 6 -2 0 -21.90 11.80 -6 2 0 -23.40 12.80 -6 2 0 -17.40 14.90 5 -2 0 440.66 44.30 -5 2 0 450.55 45.00 4 -2 0 24.40 8.60 4 -2 0 18.70 9.30 -4 2 0 15.10 8.90 -4 2 0 21.00 10.10 3 -2 0 639.84 60.29 3 -2 0 667.93 60.69 -3 2 0 661.33 60.39 -3 2 0 626.84 60.19 2 -2 0 5036.90 454.85 2 -2 0 5151.78 454.85 -2 2 0 4921.91 454.75 -2 2 0 5142.19 454.85 -2 -2 0 5349.67 494.35 -2 -2 0 5921.51 494.55 2 2 0 5253.47 494.35 2 2 0 5487.65 494.35 -3 -2 0 669.83 63.39 -3 -2 0 694.73 63.49 3 2 0 647.34 62.79 3 2 0 693.03 63.29 -4 -2 0 19.30 9.80 -4 -2 0 2.30 9.90 4 2 0 11.20 8.90 4 2 0 19.10 9.30 -5 -2 0 452.05 47.40 5 2 0 455.95 45.70 -6 -2 0 -6.00 15.70 -6 -2 0 -1.90 12.50 -6 -2 0 -10.60 14.60 6 2 0 -20.00 11.90 -7 -2 0 -5.30 16.60 -7 -2 0 15.00 17.30 -7 -2 0 15.30 17.30 7 2 0 -8.10 16.40 7 2 0 -16.80 16.80 -8 -2 0 15.60 21.30 -8 -2 0 -31.50 23.70 -8 -2 0 22.40 23.80 8 2 0 -23.60 15.30 8 2 0 -17.00 16.00 -9 -2 0 54.09 22.40 -10 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4 28 -4 25.90 13.50 4 28 -4 27.10 19.40 -4 -28 4 48.50 22.10 -4 -28 4 34.70 16.70 -4 -28 4 41.40 18.00 3 28 -4 18.40 15.10 3 28 -4 12.40 12.60 3 28 -4 21.20 17.10 -3 -28 4 16.00 12.50 2 28 -4 61.19 15.20 2 28 -4 68.79 15.90 2 28 -4 73.89 15.30 -2 -28 4 74.09 15.60 -2 -28 4 97.59 20.50 1 28 -4 17.10 11.50 1 28 -4 0.70 11.80 1 28 -4 1.30 12.30 -1 -28 4 5.50 12.40 -1 -28 4 16.30 12.90 0 28 -4 77.29 15.50 0 28 -4 46.20 14.30 0 28 -4 71.79 16.40 0 -28 4 66.89 15.00 0 -28 4 75.19 17.90 -1 28 -4 18.20 14.10 -1 28 -4 16.30 13.20 -1 28 -4 10.20 12.80 1 -28 4 18.10 15.40 1 -28 4 15.90 11.50 -2 28 -4 57.79 16.20 -2 28 -4 17.50 14.50 -2 28 -4 39.90 13.90 2 -28 4 42.70 14.50 2 -28 4 62.39 15.90 -3 28 -4 62.49 19.00 -3 28 -4 84.29 17.70 3 -28 4 80.59 18.80 -4 28 -4 67.69 21.50 -4 28 -4 100.89 20.30 4 -28 4 84.79 21.00 4 -28 4 83.59 18.80 -5 28 -4 9.60 19.10 5 -28 4 4.10 21.10 5 -28 4 29.40 19.50 -6 28 -4 27.40 32.40 -6 28 -4 20.60 30.50 6 -28 4 17.00 45.60 6 -28 4 -6.20 39.50 6 -28 4 8.90 32.20 6 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14 58.09 61.49 0 6 14 73.59 59.49 -1 9 14 -36.70 38.30 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 75518 _olex2_submission_special_instructions 'No special instructions were received'