#============================================================================= 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) ; _shelx_SHELXL_version_number '2014/7' _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 H8 Br3 N3 O3 S' _chemical_formula_sum 'C14 H8 Br3 N3 O3 S' _chemical_formula_weight 538.02 _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' 'Br' 'Br' -0.2901 2.4595 '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' _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 'orthorhombic' _space_group_IT_number 61 _space_group_name_H-M_alt 'P b c a' _space_group_name_Hall '-P 2ac 2ab' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.5477(12) _cell_length_b 7.4257(6) _cell_length_c 28.378(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3487.1(5) _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 7.079 _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_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 2.050 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description prism _exptl_crystal_F_000 2064 _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 0.1111 _diffrn_reflns_av_unetI/netI 0.0740 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_number 27641 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25.050 _diffrn_reflns_theta_max 25.050 _diffrn_reflns_theta_min 2.850 _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _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 2281 _reflns_number_total 3061 _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 1.338 _refine_diff_density_min -1.649 _refine_diff_density_rms 0.233 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.311 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 181 _refine_ls_number_reflns 3061 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1938 _refine_ls_R_factor_gt 0.1606 _refine_ls_restrained_S_all 1.311 _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^)+(0.0001P)^2^+286.1742P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3009 _refine_ls_wR_factor_ref 0.3158 _refine_special_details ? _olex2_refinement_description ; 1. Uiso/Uaniso restraints and constraints Uanis(C1) = Uanis(C4) = Uanis(C8) = Uanis(O1) Uanis(C10) = Uanis(C11) = Uanis(C12) = Uanis(C13) 2.a Aromatic/amide H refined with riding coordinates: C13(H13), C11(H11), C2(H2), C1(H1), C5(H5), C4(H4), N3(H3), N2(H2A) ; _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 C6 C 0.2740(11) 0.895(2) 0.5567(6) 0.015(4) Uani 1 1 d . . . . . C13 C 0.3817(12) 0.610(3) 0.2986(7) 0.025(2) Uani 1 1 d . . . . . H13 H 0.3688 0.6689 0.2706 0.030 Uiso 1 1 calc R U . . . C8 C 0.4088(14) 0.783(4) 0.4545(8) 0.039(3) Uani 1 1 d . . . . . C11 C 0.4392(12) 0.356(3) 0.3399(7) 0.025(2) Uani 1 1 d . . . . . H11 H 0.4643 0.2441 0.3390 0.030 Uiso 1 1 calc R U . . . C14 C 0.3649(11) 0.685(3) 0.3419(8) 0.027(5) Uani 1 1 d . . . . . C12 C 0.4188(12) 0.444(3) 0.2990(7) 0.025(2) Uani 1 1 d . . . . . C2 C 0.1658(13) 0.980(3) 0.6100(8) 0.030(5) Uani 1 1 d . . . . . H2 H 0.1111 0.9962 0.6160 0.037 Uiso 1 1 calc R U . . . C1 C 0.1916(14) 0.917(4) 0.5659(8) 0.039(3) Uani 1 1 d . . . . . H1 H 0.1538 0.8901 0.5427 0.047 Uiso 1 1 calc R U . . . C3 C 0.2215(12) 1.017(3) 0.6442(7) 0.023(5) Uani 1 1 d . . . . . C5 C 0.3287(12) 0.933(3) 0.5931(7) 0.025(5) Uani 1 1 d . . . . . H5 H 0.3837 0.9170 0.5880 0.030 Uiso 1 1 calc R U . . . C4 C 0.3031(14) 0.994(4) 0.6354(8) 0.039(3) Uani 1 1 d . . . . . H4 H 0.3406 1.0213 0.6587 0.047 Uiso 1 1 calc R U . . . C7 C 0.2962(12) 0.824(3) 0.5105(7) 0.022(4) Uani 1 1 d . . . . . C10 C 0.4216(12) 0.438(3) 0.3824(7) 0.025(2) Uani 1 1 d . . . . . C9 C 0.3849(11) 0.606(3) 0.3845(6) 0.018(4) Uani 1 1 d . . . . . Br1 Br 0.44850(17) 0.3230(4) 0.43952(9) 0.0471(8) Uani 1 1 d . . . . . Br3 Br 0.31305(19) 0.9132(4) 0.34090(10) 0.0564(9) Uani 1 1 d . . . . . Br2 Br 0.44454(18) 0.3266(5) 0.24110(10) 0.0654(11) Uani 1 1 d . . . . . N1 N 0.1937(12) 1.088(3) 0.6870(7) 0.039(5) Uani 1 1 d . . . . . N3 N 0.3600(10) 0.688(2) 0.4269(6) 0.024(4) Uani 1 1 d . . . . . H3 H 0.3104 0.6765 0.4353 0.028 Uiso 1 1 calc R U . . . N2 N 0.3744(9) 0.848(2) 0.4950(5) 0.017(4) Uani 1 1 d . . . . . H2A H 0.4052 0.9119 0.5129 0.020 Uiso 1 1 calc R U . . . O2 O 0.2416(15) 1.117(5) 0.7187(7) 0.108(11) Uani 1 1 d . . . . . O1 O 0.1241(10) 1.120(2) 0.6935(5) 0.039(3) Uani 1 1 d . . . . . O3 O 0.2463(9) 0.742(2) 0.4871(5) 0.037(4) Uani 1 1 d . . . . . S1 S 0.5055(3) 0.8233(8) 0.44215(19) 0.0293(13) 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 C6 0.016(9) 0.013(9) 0.017(10) 0.004(8) 0.003(8) -0.003(8) C13 0.021(5) 0.038(6) 0.017(5) -0.007(5) -0.001(5) -0.001(5) C8 0.032(6) 0.055(7) 0.030(6) -0.005(5) 0.011(5) 0.004(5) C11 0.021(5) 0.038(6) 0.017(5) -0.007(5) -0.001(5) -0.001(5) C14 0.011(9) 0.037(12) 0.033(12) -0.008(12) 0.010(10) 0.012(9) C12 0.021(5) 0.038(6) 0.017(5) -0.007(5) -0.001(5) -0.001(5) C2 0.023(11) 0.032(13) 0.037(13) -0.012(11) 0.018(10) -0.006(10) C1 0.032(6) 0.055(7) 0.030(6) -0.005(5) 0.011(5) 0.004(5) C3 0.031(12) 0.024(11) 0.014(10) -0.011(9) 0.003(9) -0.003(10) C5 0.020(11) 0.033(12) 0.021(11) -0.001(10) 0.008(9) 0.000(10) C4 0.032(6) 0.055(7) 0.030(6) -0.005(5) 0.011(5) 0.004(5) C7 0.029(12) 0.015(9) 0.021(10) -0.004(9) -0.008(9) -0.002(9) C10 0.021(5) 0.038(6) 0.017(5) -0.007(5) -0.001(5) -0.001(5) C9 0.019(10) 0.024(11) 0.010(10) 0.004(8) -0.004(8) 0.000(9) Br1 0.0521(16) 0.0436(14) 0.0455(15) 0.0213(13) 0.0041(13) 0.0154(13) Br3 0.077(2) 0.0437(15) 0.0482(16) 0.0042(14) -0.0064(16) 0.0366(15) Br2 0.0547(17) 0.103(3) 0.0390(16) -0.0449(17) -0.0070(14) 0.0265(18) N1 0.035(12) 0.059(14) 0.023(11) -0.014(10) 0.016(10) 0.006(11) N3 0.020(9) 0.030(10) 0.021(9) -0.010(8) 0.003(7) 0.006(8) N2 0.019(8) 0.029(10) 0.002(7) 0.004(7) 0.004(6) 0.001(7) O2 0.063(14) 0.22(3) 0.043(12) -0.055(18) 0.008(12) 0.022(19) O1 0.032(6) 0.055(7) 0.030(6) -0.005(5) 0.011(5) 0.004(5) O3 0.018(7) 0.052(10) 0.041(9) -0.020(8) 0.011(8) -0.008(8) S1 0.019(3) 0.039(3) 0.029(3) -0.008(3) 0.008(2) -0.003(3) _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 C6 C1 1.40(3) . ? C6 C5 1.40(3) . ? C6 C7 1.46(3) . ? C13 H13 0.9300 . ? C13 C14 1.38(3) . ? C13 C12 1.38(3) . ? C8 N3 1.33(3) . ? C8 N2 1.37(3) . ? C8 S1 1.66(2) . ? C11 H11 0.9300 . ? C11 C12 1.37(3) . ? C11 C10 1.38(3) . ? C14 C9 1.38(3) . ? C14 Br3 1.90(2) . ? C12 Br2 1.91(2) . ? C2 H2 0.9300 . ? C2 C1 1.40(3) . ? C2 C3 1.36(3) . ? C1 H1 0.9300 . ? C3 C4 1.38(3) . ? C3 N1 1.41(3) . ? C5 H5 0.9300 . ? C5 C4 1.35(3) . ? C4 H4 0.9300 . ? C7 N2 1.38(2) . ? C7 O3 1.22(2) 1 ? C7 O3 1.22(2) . ? C10 C9 1.39(3) . ? C10 Br1 1.89(2) . ? C9 N3 1.41(2) . ? N1 O2 1.22(3) . ? N1 O1 1.19(2) . ? N3 H3 0.8600 . ? N2 H2A 0.8600 . ? O3 O3 0.00(5) 1 ? 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 C1 C6 C5 117.9(19) . . ? C1 C6 C7 117.1(18) . . ? C5 C6 C7 125.0(17) . . ? C14 C13 H13 121.9 . . ? C14 C13 C12 116(2) . . ? C12 C13 H13 121.9 . . ? N3 C8 N2 115.4(19) . . ? N3 C8 S1 123.7(17) . . ? N2 C8 S1 120.9(18) . . ? C12 C11 H11 120.8 . . ? C12 C11 C10 118(2) . . ? C10 C11 H11 120.8 . . ? C13 C14 C9 124.3(19) . . ? C13 C14 Br3 115.9(17) . . ? C9 C14 Br3 119.8(15) . . ? C13 C12 Br2 120.0(16) . . ? C11 C12 C13 122.7(19) . . ? C11 C12 Br2 117.3(16) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C3 C2 C1 120(2) . . ? C6 C1 C2 120(2) . . ? C6 C1 H1 120.0 . . ? C2 C1 H1 120.0 . . ? C2 C3 C4 120.5(19) . . ? C2 C3 N1 118.0(19) . . ? C4 C3 N1 121(2) . . ? C6 C5 H5 119.3 . . ? C4 C5 C6 121(2) . . ? C4 C5 H5 119.3 . . ? C3 C4 H4 119.8 . . ? C5 C4 C3 120(2) . . ? C5 C4 H4 119.8 . . ? N2 C7 C6 118.4(17) . . ? O3 C7 C6 119.8(18) . . ? O3 C7 C6 119.8(18) 1 . ? O3 C7 N2 121.8(18) 1 . ? O3 C7 N2 121.8(18) . . ? O3 C7 O3 0(2) 1 . ? C11 C10 C9 122(2) . . ? C11 C10 Br1 120.0(17) . . ? C9 C10 Br1 118.3(15) . . ? C14 C9 C10 116.5(18) . . ? C14 C9 N3 119.6(17) . . ? C10 C9 N3 123.6(17) . . ? O2 N1 C3 120(2) . . ? O1 N1 C3 122(2) . . ? O1 N1 O2 118.8(19) . . ? C8 N3 C9 123.8(17) . . ? C8 N3 H3 118.1 . . ? C9 N3 H3 118.1 . . ? C8 N2 C7 127.7(18) . . ? C8 N2 H2A 116.1 . . ? C7 N2 H2A 116.1 . . ? O3 O3 C7 0(10) 1 . ? 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 N3 H3 O3 0.86 1.88 2.57(2) 137.0 1 N2 H2A S1 0.86 2.77 3.616(17) 167.7 5_676 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 C6 C5 C4 C3 1(4) . . . . ? C6 C7 N2 C8 175(2) . . . . ? C6 C7 O3 O3 0(3) . . . 1 ? C13 C14 C9 C10 -2(3) . . . . ? C13 C14 C9 N3 -176(2) . . . . ? C11 C10 C9 C14 2(3) . . . . ? C11 C10 C9 N3 174.8(19) . . . . ? C14 C13 C12 C11 -1(3) . . . . ? C14 C13 C12 Br2 179.7(15) . . . . ? C14 C9 N3 C8 -103(2) . . . . ? C12 C13 C14 C9 2(3) . . . . ? C12 C13 C14 Br3 -179.5(15) . . . . ? C12 C11 C10 C9 -1(3) . . . . ? C12 C11 C10 Br1 180.0(16) . . . . ? C2 C3 C4 C5 -1(4) . . . . ? C2 C3 N1 O2 178(3) . . . . ? C2 C3 N1 O1 -2(3) . . . . ? C1 C6 C5 C4 -1(3) . . . . ? C1 C6 C7 N2 161.6(19) . . . . ? C1 C6 C7 O3 -20(3) . . . 1 ? C1 C6 C7 O3 -20(3) . . . . ? C1 C2 C3 C4 1(4) . . . . ? C1 C2 C3 N1 177(2) . . . . ? C3 C2 C1 C6 -1(4) . . . . ? C5 C6 C1 C2 1(3) . . . . ? C5 C6 C7 N2 -22(3) . . . . ? C5 C6 C7 O3 157(2) . . . . ? C5 C6 C7 O3 157(2) . . . 1 ? C4 C3 N1 O2 -6(4) . . . . ? C4 C3 N1 O1 174(2) . . . . ? C7 C6 C1 C2 178(2) . . . . ? C7 C6 C5 C4 -178(2) . . . . ? C10 C11 C12 C13 0(3) . . . . ? C10 C11 C12 Br2 179.7(15) . . . . ? C10 C9 N3 C8 84(3) . . . . ? Br1 C10 C9 C14 -178.9(15) . . . . ? Br1 C10 C9 N3 -6(3) . . . . ? Br3 C14 C9 C10 179.2(14) . . . . ? Br3 C14 C9 N3 6(3) . . . . ? N1 C3 C4 C5 -177(2) . . . . ? N3 C8 N2 C7 1(3) . . . . ? N2 C8 N3 C9 -178.1(18) . . . . ? N2 C7 O3 O3 0(4) . . . 1 ? O3 C7 N2 C8 -3(3) 1 . . . ? O3 C7 N2 C8 -3(3) . . . . ? S1 C8 N3 C9 2(3) . . . . ? S1 C8 N2 C7 -178.7(17) . . . . ? _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL fatma8_a.res in Pbca CELL 0.71073 16.5477 7.4257 28.3783 90.000 90.000 90.000 ZERR 8.00 0.0012 0.0006 0.0023 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H BR N O S UNIT 112 64 24 24 24 8 MERG 2 OMIT -4.00 50.10 EADP C1 C4 C8 O1 EADP C10 C11 C12 C13 EQIV $1 -x+1,-y+2,-z+1 EQIV $3 x,y,z HTAB N2 S1_$1 HTAB N3 O3_$3 FMAP 2 PLAN 20 ACTA BOND BOND $H CONF L.S. 10 WGHT 0.000100 286.174194 FVAR 0.16076 C6 1 0.274041 0.894707 0.556716 11.00000 0.01568 0.01338 = 0.01712 0.00361 0.00317 -0.00346 C13 1 0.381693 0.610318 0.298575 11.00000 0.02107 0.03792 = 0.01716 -0.00670 -0.00127 -0.00056 AFIX 43 H13 2 0.368818 0.668908 0.270600 11.00000 -1.20000 AFIX 0 C8 1 0.408836 0.783267 0.454521 11.00000 0.03243 0.05529 = 0.02985 -0.00479 0.01087 0.00413 C11 1 0.439189 0.356089 0.339879 11.00000 0.02107 0.03792 = 0.01716 -0.00670 -0.00127 -0.00056 AFIX 43 H11 2 0.464266 0.244052 0.339035 11.00000 -1.20000 AFIX 0 C14 1 0.364869 0.684732 0.341882 11.00000 0.01083 0.03729 = 0.03274 -0.00819 0.01036 0.01191 C12 1 0.418808 0.443574 0.298994 11.00000 0.02107 0.03792 = 0.01716 -0.00670 -0.00127 -0.00056 C2 1 0.165847 0.979774 0.610032 11.00000 0.02279 0.03156 = 0.03701 -0.01214 0.01835 -0.00610 AFIX 43 H2 2 0.111081 0.996222 0.616002 11.00000 -1.20000 AFIX 0 C1 1 0.191579 0.916966 0.565886 11.00000 0.03243 0.05529 = 0.02985 -0.00479 0.01087 0.00413 AFIX 43 H1 2 0.153762 0.890092 0.542685 11.00000 -1.20000 AFIX 0 C3 1 0.221479 1.016609 0.644156 11.00000 0.03124 0.02408 = 0.01359 -0.01075 0.00340 -0.00251 C5 1 0.328693 0.933471 0.593084 11.00000 0.02021 0.03336 = 0.02059 -0.00063 0.00845 0.00008 AFIX 43 H5 2 0.383709 0.916955 0.587972 11.00000 -1.20000 AFIX 0 C4 1 0.303127 0.994269 0.635369 11.00000 0.03243 0.05529 = 0.02985 -0.00479 0.01087 0.00413 AFIX 43 H4 2 0.340617 1.021305 0.658736 11.00000 -1.20000 AFIX 0 C7 1 0.296235 0.824118 0.510480 11.00000 0.02904 0.01469 = 0.02096 -0.00400 -0.00755 -0.00209 C10 1 0.421592 0.438308 0.382358 11.00000 0.02107 0.03792 = 0.01716 -0.00670 -0.00127 -0.00056 C9 1 0.384860 0.606124 0.384474 11.00000 0.01868 0.02412 = 0.00972 0.00424 -0.00394 0.00042 BR1 3 0.448503 0.322979 0.439521 11.00000 0.05209 0.04358 = 0.04549 0.02128 0.00411 0.01543 BR3 3 0.313050 0.913165 0.340904 11.00000 0.07740 0.04366 = 0.04819 0.00417 -0.00639 0.03661 BR2 3 0.444537 0.326624 0.241102 11.00000 0.05467 0.10263 = 0.03899 -0.04490 -0.00704 0.02654 N1 4 0.193704 1.088082 0.687042 11.00000 0.03451 0.05923 = 0.02333 -0.01395 0.01550 0.00586 N3 4 0.360030 0.688451 0.426895 11.00000 0.02027 0.02954 = 0.02107 -0.00973 0.00296 0.00552 AFIX 43 H3 2 0.310406 0.676506 0.435339 11.00000 -1.20000 AFIX 0 N2 4 0.374379 0.848356 0.495004 11.00000 0.01854 0.02926 = 0.00219 0.00370 0.00445 0.00117 AFIX 43 H2A 2 0.405208 0.911872 0.512865 11.00000 -1.20000 AFIX 0 O2 5 0.241569 1.116567 0.718726 11.00000 0.06313 0.21824 = 0.04319 -0.05503 0.00834 0.02183 O1 5 0.124117 1.120112 0.693481 11.00000 0.03243 0.05529 = 0.02985 -0.00479 0.01087 0.00413 O3 5 0.246297 0.742293 0.487080 11.00000 0.01789 0.05246 = 0.04089 -0.02009 0.01076 -0.00819 S1 6 0.505518 0.823302 0.442149 11.00000 0.01939 0.03931 = 0.02930 -0.00834 0.00813 -0.00310 HKLF 4 REM fatma8_a.res in Pbca REM R1 = 0.1606 for 2281 Fo > 4sig(Fo) and 0.1938 for all 3061 data REM 181 parameters refined using 0 restraints END WGHT 0.0001 280.9907 REM Highest difference peak 1.338, deepest hole -1.649, 1-sigma level 0.233 Q1 1 0.4508 0.3114 0.2125 11.00000 0.05 1.34 Q2 1 0.4420 0.3678 0.2712 11.00000 0.05 1.33 Q3 1 0.4533 0.2754 0.2714 11.00000 0.05 1.28 Q4 1 0.4439 0.3642 0.3109 11.00000 0.05 1.08 Q5 1 0.4442 0.3196 0.3687 11.00000 0.05 1.03 Q6 1 0.4464 0.3652 0.3696 11.00000 0.05 1.01 Q7 1 0.4528 0.2966 0.4673 11.00000 0.05 1.00 Q8 1 0.3183 0.9557 0.3121 11.00000 0.05 0.99 Q9 1 0.3183 0.8803 0.3730 11.00000 0.05 0.97 Q10 1 0.4523 0.3755 0.4103 11.00000 0.05 0.96 Q11 1 0.4550 0.2911 0.4089 11.00000 0.05 0.93 Q12 1 0.3086 0.9905 0.3713 11.00000 0.05 0.90 Q13 1 0.5064 0.6241 0.3096 11.00000 0.05 0.85 Q14 1 0.4423 0.5143 0.1986 11.00000 0.05 0.84 Q15 1 0.1437 1.0268 0.7097 11.00000 0.05 0.81 Q16 1 0.1159 1.0120 0.7028 11.00000 0.05 0.79 Q17 1 0.5046 0.8760 0.5094 11.00000 0.05 0.78 Q18 1 0.4485 0.1564 0.4012 11.00000 0.05 0.77 Q19 1 0.4391 0.9964 0.4995 11.00000 0.05 0.75 Q20 1 0.4104 0.5339 0.2835 11.00000 0.05 0.73 ; _shelx_res_checksum 19968 _shelx_hkl_file ; 0 2 0 622.64 38.60 0 2 0 595.64 38.60 0 -2 0 668.63 38.70 0 -2 0 638.34 38.70 0 3 0 0.80 4.00 0 3 0 4.00 5.30 0 -3 0 2.00 5.10 0 -3 0 3.30 4.50 0 -4 0 1549.54 92.19 0 4 0 1501.45 92.19 0 4 0 1481.65 92.29 0 -4 0 1516.25 92.39 0 5 0 6.90 9.70 0 -5 0 2.70 7.20 0 -5 0 -6.80 7.50 0 -6 0 130.29 15.60 0 -6 0 112.19 13.80 0 6 0 158.28 18.30 0 6 0 111.79 14.60 0 7 0 19.30 14.60 0 7 0 21.10 15.90 0 -8 0 172.18 24.90 0 8 0 221.88 23.90 0 -9 0 -28.10 20.50 0 9 0 -23.60 31.40 1 -1 0 1.70 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52.99 29.80 -8 3 30 105.49 36.10 -9 0 -30 85.79 31.90 9 0 30 29.00 38.90 9 -1 -30 174.48 34.50 -9 1 -30 112.39 36.80 9 1 30 281.67 47.60 -9 1 30 191.08 34.70 9 -2 -30 261.27 47.80 9 2 30 158.98 44.20 10 0 -30 -26.60 35.00 10 0 30 -19.10 50.09 10 -1 -30 312.87 49.40 -10 1 30 287.77 41.90 10 1 -30 284.97 41.20 10 -2 -30 137.69 41.60 10 2 -30 187.08 33.30 0 0 -31 59.49 34.70 0 1 -31 13.00 28.00 0 -1 31 62.79 28.30 0 -1 -31 39.90 30.10 0 1 31 87.19 40.20 0 -2 -31 109.49 31.10 0 2 -31 101.69 35.70 0 3 31 93.19 38.00 0 4 -31 -0.50 47.90 0 -4 -31 84.49 33.50 0 -4 31 131.39 39.40 -1 0 -31 47.60 30.50 -1 0 31 81.59 27.70 1 0 -31 8.60 33.10 -1 1 -31 38.90 27.00 1 -1 -31 23.30 25.60 1 1 31 78.19 32.80 -1 -1 -31 81.49 30.80 1 1 -31 41.90 29.10 -1 -2 31 126.39 34.30 -1 2 -31 100.09 31.60 1 -2 -31 139.99 30.60 -1 -2 -31 97.59 29.00 1 2 -31 83.09 25.60 1 2 -31 119.99 32.60 -1 2 31 143.59 30.00 1 -3 -31 253.37 37.50 -1 -3 31 254.97 48.20 1 3 31 267.37 37.70 -1 -3 -31 219.48 37.50 1 -3 31 292.27 43.80 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29.50 2 0 33 35.60 32.50 2 0 -33 44.80 35.10 2 -1 -33 136.19 33.00 -2 1 -33 97.49 31.00 2 1 33 153.38 33.40 -2 -1 -33 106.89 34.30 2 1 -33 137.49 34.20 -2 1 33 184.68 35.30 2 2 33 109.99 41.00 2 -2 -33 207.28 40.70 -2 -2 33 238.38 42.20 -2 2 -33 154.98 38.20 2 2 -33 262.67 49.70 -2 3 -33 9.00 34.40 -2 -3 33 65.39 32.10 2 -3 -33 56.09 34.50 2 3 -33 28.30 36.20 -2 3 33 -10.10 35.70 2 -3 33 30.00 37.40 3 0 33 62.99 35.90 3 0 -33 59.39 33.90 3 -1 -33 53.89 35.00 -3 1 -33 66.09 29.40 -3 -1 33 93.29 32.80 -3 -1 -33 13.50 32.80 -3 1 33 63.39 34.20 3 1 -33 54.09 31.60 3 -2 -33 136.29 36.00 -3 2 -33 100.49 34.90 3 2 33 102.29 36.10 -3 2 33 33.50 34.60 3 2 -33 131.79 37.10 3 -3 -33 124.99 30.40 3 3 33 140.59 43.20 -3 3 -33 29.40 43.00 3 3 -33 51.19 36.20 -3 3 33 98.99 36.60 -3 -3 -33 86.89 39.40 4 0 -33 90.19 37.80 4 1 33 -16.80 33.10 4 -1 -33 153.08 40.00 -4 1 -33 52.69 28.60 4 -1 33 60.39 36.40 -4 -1 -33 40.40 34.80 4 1 -33 113.89 41.10 -4 1 33 74.79 40.80 4 -2 -33 84.49 42.40 -4 2 -33 60.19 35.70 4 2 33 181.48 41.10 -4 -2 33 105.89 38.10 4 -2 33 58.09 37.80 4 2 -33 122.19 35.80 5 0 33 -13.10 31.80 5 0 -33 114.49 43.50 -5 1 -33 23.30 31.60 5 1 33 85.29 35.80 5 -1 -33 91.49 35.60 -5 1 33 68.99 41.80 -5 -1 -33 28.20 33.30 -5 -2 33 87.89 35.00 5 -2 -33 78.99 34.70 5 2 33 78.29 39.80 -5 2 -33 24.70 38.00 5 2 -33 116.59 38.70 -5 -2 -33 1.40 34.40 -6 0 33 331.87 42.80 6 0 -33 245.68 50.59 -6 -1 33 128.29 38.50 -6 1 -33 122.09 40.50 6 -1 -33 96.49 38.80 6 1 -33 226.58 45.60 6 -1 33 66.69 43.50 -7 0 -33 63.79 29.00 7 0 33 57.69 40.60 7 0 -33 85.09 42.60 7 1 33 96.49 32.40 -7 1 -33 126.39 38.30 7 -1 -33 72.99 29.60 7 -1 33 61.99 49.20 7 1 -33 100.49 43.60 0 0 -34 230.88 44.20 0 0 34 363.26 42.00 0 1 -34 137.39 42.90 0 -1 -34 225.58 41.40 0 -2 -34 88.99 38.10 0 2 -34 52.49 31.80 0 2 34 -7.50 35.40 1 0 -34 162.28 40.00 -1 0 -34 105.39 39.70 -1 -1 34 66.79 30.60 1 1 -34 92.29 36.50 1 -1 34 136.79 40.90 -1 -2 34 85.19 38.60 1 2 34 98.49 33.90 1 -2 -34 53.09 35.50 -1 2 -34 50.29 34.80 1 2 -34 43.00 31.30 2 0 -34 303.57 44.50 -2 0 34 294.87 40.10 2 0 34 285.37 41.50 -2 0 -34 338.77 44.80 -2 -1 34 169.28 49.10 -2 1 -34 158.08 41.40 2 1 34 116.49 35.90 2 1 -34 145.89 38.10 2 -1 34 128.39 36.40 2 -2 -34 76.99 31.10 -2 2 -34 59.19 31.60 -2 -2 34 65.99 41.10 2 2 -34 67.59 33.00 2 -2 34 53.39 34.90 3 0 -34 103.49 45.60 -3 0 34 102.19 39.60 3 0 34 170.98 37.00 3 1 34 69.29 33.20 3 -1 -34 59.89 36.70 -3 1 -34 125.09 42.10 3 -1 34 212.38 39.30 3 1 -34 54.99 36.00 -3 -1 -34 137.59 45.60 3 -2 -34 96.99 47.00 3 -2 34 141.79 42.50 3 2 -34 80.49 37.00 -3 2 34 141.19 40.30 -3 -2 -34 227.08 44.60 4 0 -34 77.09 37.70 -4 0 34 97.69 43.90 4 0 34 102.69 34.10 4 -1 -34 104.89 38.00 -4 1 -34 65.79 36.50 4 1 -34 99.99 37.30 -4 2 -34 50.19 23.10 4 2 34 111.19 39.70 -4 2 34 107.69 35.90 4 2 -34 76.19 37.50 5 0 34 230.48 45.70 -5 0 -34 225.98 45.50 -5 0 34 324.27 43.40 -5 1 -34 45.50 36.70 5 1 34 63.79 41.20 5 1 -34 80.29 32.00 -5 1 34 112.39 32.80 5 -1 34 120.89 43.00 0 0 35 112.59 34.70 0 0 -35 84.49 34.50 0 1 -35 53.49 26.50 0 -1 -35 114.49 32.00 0 1 35 121.19 36.10 1 0 -35 96.09 33.30 -1 0 -35 66.89 31.50 -1 1 35 266.57 41.60 2 0 -35 67.69 30.60 -2 0 -35 79.29 32.20 2 1 35 231.78 42.00 -2 -1 -35 118.29 36.80 -2 1 35 164.58 38.40 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 48401 _olex2_submission_special_instructions 'No special instructions were received'