# Electronic Supplementary Material (ESI) for RSC Advances. # This journal is © The Royal Society of Chemistry 2022 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_dr _audit_block_doi 10.5517/ccdc.csd.cc2d8llw _database_code_depnum_ccdc_archive 'CCDC 2212798' loop_ _audit_author_name _audit_author_address 'Weiming Chen' ;Gannan Medical University China ; _audit_update_record ; 2022-10-13 deposited with the CCDC. 2022-12-06 downloaded from the CCDC. ; _audit_creation_date 2022-05-09 _audit_creation_method ; Olex2 1.5-beta (compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439) ; _shelx_SHELXL_version_number 2017/1 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C16 H15 F3 N6 O2 S' _chemical_formula_sum 'C16 H15 F3 N6 O2 S' _chemical_formula_weight 412.40 _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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 11.715(6) _cell_length_b 7.738(4) _cell_length_c 19.834(9) _cell_angle_alpha 90 _cell_angle_beta 95.723(10) _cell_angle_gamma 90 _cell_volume 1788.9(15) _cell_formula_units_Z 4 _cell_measurement_reflns_used 4037 _cell_measurement_temperature 296.15 _cell_measurement_theta_max 20.27 _cell_measurement_theta_min 2.83 _shelx_estimated_absorpt_T_max 0.977 _shelx_estimated_absorpt_T_min 0.968 _exptl_absorpt_coefficient_mu 0.238 _exptl_absorpt_correction_T_max 0.977 _exptl_absorpt_correction_T_min 0.968 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_absorpt_special_details ? _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_meas . _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 848 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.1091 _diffrn_reflns_av_unetI/netI 0.0843 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 38273 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 25.104 _diffrn_reflns_theta_max 25.104 _diffrn_reflns_theta_min 2.064 _diffrn_ambient_temperature 296.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _diffrn_source_current 30.0 _diffrn_source_power 1.5 _diffrn_source_voltage 50.0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1585 _reflns_number_total 3161 _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 ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics 'Olex2 1.5-beta (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5-beta (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2017/1 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _refine_diff_density_max 0.222 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.061 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 255 _refine_ls_number_reflns 3161 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1600 _refine_ls_R_factor_gt 0.0593 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.9059P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1132 _refine_ls_wR_factor_ref 0.1501 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C4(H4A,H4B), C8(H8A,H8B), C15(H15A,H15B) 2.b Aromatic/amide H refined with riding coordinates: C6(H6), C10(H10), C13(H13) 2.c Idealised Me refined as rotating group: C7(H7A,H7B,H7C), C16(H16A,H16B,H16C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _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 S1 S 0.17022(9) 0.52068(14) 0.59579(5) 0.0590(4) Uani 1 1 d . . . . . F1 F 0.2161(2) 0.1076(3) 0.52904(12) 0.0788(8) Uani 1 1 d . . . . . F2 F 0.6478(2) 0.3476(4) 0.52338(13) 0.0994(10) Uani 1 1 d . . . . . F3 F 0.5372(2) 0.2100(4) 0.41156(12) 0.1024(10) Uani 1 1 d . . . . . O1 O 0.4164(2) 0.8779(4) 0.75414(14) 0.0654(8) Uani 1 1 d . . . . . O2 O 0.4739(2) 0.2988(4) 0.76233(13) 0.0581(8) Uani 1 1 d . . . . . N1 N 0.2946(3) 0.7088(4) 0.68611(16) 0.0487(8) Uani 1 1 d . . . . . N2 N 0.4387(3) 0.5877(4) 0.76452(15) 0.0474(8) Uani 1 1 d . . . . . N3 N 0.3354(3) 0.4095(4) 0.68547(15) 0.0439(8) Uani 1 1 d . . . . . N4 N 0.6589(3) 0.5939(4) 0.72209(17) 0.0570(9) Uani 1 1 d . . . . . N5 N 0.7741(3) 0.5697(4) 0.71995(17) 0.0566(9) Uani 1 1 d . . . . . N6 N 0.7476(3) 0.5611(5) 0.82722(18) 0.0689(11) Uani 1 1 d . . . . . C1 C 0.3845(3) 0.7346(6) 0.7348(2) 0.0491(10) Uani 1 1 d . . . . . C2 C 0.2757(3) 0.5552(6) 0.66224(18) 0.0452(10) Uani 1 1 d . . . . . C3 C 0.4200(3) 0.4235(6) 0.73948(19) 0.0468(10) Uani 1 1 d . . . . . C4 C 0.5364(3) 0.6077(6) 0.8162(2) 0.0587(12) Uani 1 1 d . . . . . H4A H 0.531039 0.522062 0.851406 0.070 Uiso 1 1 calc R U . . . H4B H 0.533180 0.721136 0.836723 0.070 Uiso 1 1 calc R U . . . C5 C 0.6486(3) 0.5876(5) 0.7872(2) 0.0504(11) Uani 1 1 d . . . . . C6 C 0.8233(4) 0.5504(6) 0.7820(2) 0.0694(13) Uani 1 1 d . . . . . H6 H 0.901358 0.531471 0.792790 0.083 Uiso 1 1 calc R U . . . C7 C 0.8242(4) 0.5680(6) 0.6563(2) 0.0766(14) Uani 1 1 d . . . . . H7A H 0.790081 0.477133 0.628174 0.115 Uiso 1 1 calc R U . . . H7B H 0.905331 0.548697 0.664631 0.115 Uiso 1 1 calc R U . . . H7C H 0.810483 0.677048 0.633890 0.115 Uiso 1 1 calc R U . . . C8 C 0.3201(3) 0.2405(5) 0.65146(19) 0.0505(10) Uani 1 1 d . . . . . H8A H 0.238861 0.218189 0.640851 0.061 Uiso 1 1 calc R U . . . H8B H 0.351271 0.150626 0.682045 0.061 Uiso 1 1 calc R U . . . C9 C 0.3783(3) 0.2336(5) 0.58751(18) 0.0431(10) Uani 1 1 d . . . . . C10 C 0.4890(4) 0.2943(5) 0.5850(2) 0.0561(11) Uani 1 1 d . . . . . H10 H 0.529027 0.341200 0.623515 0.067 Uiso 1 1 calc R U . . . C11 C 0.5393(4) 0.2855(6) 0.5261(2) 0.0627(12) Uani 1 1 d . . . . . C12 C 0.4841(5) 0.2175(6) 0.4687(2) 0.0662(13) Uani 1 1 d . . . . . C13 C 0.3748(4) 0.1548(6) 0.4687(2) 0.0646(13) Uani 1 1 d . . . . . H13 H 0.335658 0.106831 0.430073 0.078 Uiso 1 1 calc R U . . . C14 C 0.3261(4) 0.1665(5) 0.5286(2) 0.0533(11) Uani 1 1 d . . . . . C15 C 0.1283(4) 0.7397(6) 0.5753(2) 0.0735(13) Uani 1 1 d . . . . . H15A H 0.085262 0.786435 0.610420 0.088 Uiso 1 1 calc R U . . . H15B H 0.196039 0.810612 0.572765 0.088 Uiso 1 1 calc R U . . . C16 C 0.0564(5) 0.7435(7) 0.5091(3) 0.112(2) Uani 1 1 d . . . . . H16A H 0.098019 0.692442 0.474804 0.169 Uiso 1 1 calc R U . . . H16B H 0.037640 0.861005 0.497005 0.169 Uiso 1 1 calc R U . . . H16C H -0.012957 0.679453 0.512630 0.169 Uiso 1 1 calc R U . . . 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 S1 0.0602(8) 0.0566(8) 0.0573(7) 0.0010(5) -0.0085(6) -0.0005(6) F1 0.0688(18) 0.0822(19) 0.0825(18) -0.0171(14) -0.0070(14) -0.0151(15) F2 0.074(2) 0.139(3) 0.090(2) -0.0065(18) 0.0324(16) -0.0179(18) F3 0.118(2) 0.133(3) 0.0608(18) -0.0010(16) 0.0335(17) 0.0209(19) O1 0.070(2) 0.051(2) 0.074(2) -0.0149(16) 0.0029(16) -0.0022(17) O2 0.0581(19) 0.056(2) 0.0576(18) 0.0047(14) -0.0061(14) 0.0052(16) N1 0.045(2) 0.051(2) 0.050(2) -0.0060(17) 0.0024(18) 0.0004(17) N2 0.044(2) 0.047(2) 0.050(2) -0.0084(17) -0.0009(16) -0.0008(18) N3 0.044(2) 0.044(2) 0.0438(19) 0.0031(16) 0.0039(16) 0.0006(17) N4 0.044(2) 0.072(3) 0.054(2) 0.0001(18) -0.0035(17) 0.0023(18) N5 0.051(2) 0.062(3) 0.056(2) 0.0011(18) 0.0008(19) -0.0043(18) N6 0.052(2) 0.098(3) 0.054(2) 0.009(2) -0.006(2) 0.000(2) C1 0.048(3) 0.053(3) 0.048(3) -0.006(2) 0.016(2) -0.001(2) C2 0.038(2) 0.058(3) 0.040(2) 0.001(2) 0.0063(18) -0.002(2) C3 0.039(3) 0.058(3) 0.043(2) 0.006(2) 0.005(2) 0.003(2) C4 0.058(3) 0.064(3) 0.052(3) -0.008(2) -0.007(2) -0.001(2) C5 0.051(3) 0.051(3) 0.048(3) 0.001(2) -0.006(2) -0.006(2) C6 0.052(3) 0.084(4) 0.069(3) 0.008(3) -0.012(3) -0.002(3) C7 0.068(3) 0.098(4) 0.065(3) -0.003(3) 0.013(3) 0.003(3) C8 0.050(3) 0.044(3) 0.057(3) 0.002(2) 0.003(2) -0.003(2) C9 0.046(3) 0.038(2) 0.045(2) -0.0008(19) 0.003(2) 0.005(2) C10 0.055(3) 0.066(3) 0.047(3) -0.003(2) 0.007(2) 0.001(2) C11 0.054(3) 0.069(3) 0.067(3) 0.002(3) 0.012(3) 0.002(2) C12 0.078(4) 0.076(3) 0.047(3) 0.005(2) 0.016(3) 0.020(3) C13 0.080(4) 0.063(3) 0.048(3) -0.011(2) -0.006(3) 0.013(3) C14 0.046(3) 0.050(3) 0.062(3) -0.003(2) -0.002(2) 0.001(2) C15 0.085(3) 0.064(3) 0.068(3) 0.002(2) -0.010(3) 0.016(3) C16 0.132(5) 0.077(4) 0.112(4) 0.000(3) -0.062(4) 0.022(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 S1 C2 1.735(4) . ? S1 C15 1.800(4) . ? F1 C14 1.367(4) . ? F2 C11 1.364(5) . ? F3 C12 1.348(5) . ? O1 C1 1.219(5) . ? O2 C3 1.216(4) . ? N1 C1 1.371(5) . ? N1 C2 1.291(5) . ? N2 C1 1.403(5) . ? N2 C3 1.374(5) . ? N2 C4 1.467(4) . ? N3 C2 1.382(5) . ? N3 C3 1.389(5) . ? N3 C8 1.474(5) . ? N4 N5 1.368(4) . ? N4 C5 1.310(5) . ? N5 C6 1.314(5) . ? N5 C7 1.444(5) . ? N6 C5 1.353(5) . ? N6 C6 1.325(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 C5 1.494(5) . ? C6 H6 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 C9 1.499(5) . ? C9 C10 1.385(5) . ? C9 C14 1.365(5) . ? C10 H10 0.9300 . ? C10 C11 1.362(5) . ? C11 C12 1.357(6) . ? C12 C13 1.369(6) . ? C13 H13 0.9300 . ? C13 C14 1.372(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 C16 1.488(6) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? 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 S1 C15 100.6(2) . . ? C2 N1 C1 119.0(3) . . ? C1 N2 C4 119.8(3) . . ? C3 N2 C1 123.3(3) . . ? C3 N2 C4 115.8(3) . . ? C2 N3 C3 119.5(3) . . ? C2 N3 C8 122.5(3) . . ? C3 N3 C8 117.8(3) . . ? C5 N4 N5 102.3(3) . . ? N4 N5 C7 121.1(3) . . ? C6 N5 N4 109.2(3) . . ? C6 N5 C7 129.7(4) . . ? C6 N6 C5 101.8(3) . . ? O1 C1 N1 122.9(4) . . ? O1 C1 N2 119.6(4) . . ? N1 C1 N2 117.5(4) . . ? N1 C2 S1 120.2(3) . . ? N1 C2 N3 124.5(3) . . ? N3 C2 S1 115.2(3) . . ? O2 C3 N2 122.8(4) . . ? O2 C3 N3 122.0(4) . . ? N2 C3 N3 115.2(4) . . ? N2 C4 H4A 109.2 . . ? N2 C4 H4B 109.2 . . ? N2 C4 C5 112.1(3) . . ? H4A C4 H4B 107.9 . . ? C5 C4 H4A 109.2 . . ? C5 C4 H4B 109.2 . . ? N4 C5 N6 115.2(4) . . ? N4 C5 C4 123.0(4) . . ? N6 C5 C4 121.7(4) . . ? N5 C6 N6 111.5(4) . . ? N5 C6 H6 124.3 . . ? N6 C6 H6 124.3 . . ? N5 C7 H7A 109.5 . . ? N5 C7 H7B 109.5 . . ? N5 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 H8A 109.2 . . ? N3 C8 H8B 109.2 . . ? N3 C8 C9 112.0(3) . . ? H8A C8 H8B 107.9 . . ? C9 C8 H8A 109.2 . . ? C9 C8 H8B 109.2 . . ? C10 C9 C8 121.7(4) . . ? C14 C9 C8 122.3(4) . . ? C14 C9 C10 116.0(4) . . ? C9 C10 H10 120.0 . . ? C11 C10 C9 120.1(4) . . ? C11 C10 H10 120.0 . . ? C10 C11 F2 120.0(4) . . ? C12 C11 F2 118.2(4) . . ? C12 C11 C10 121.8(4) . . ? F3 C12 C11 120.0(5) . . ? F3 C12 C13 119.6(5) . . ? C11 C12 C13 120.4(4) . . ? C12 C13 H13 121.8 . . ? C12 C13 C14 116.5(4) . . ? C14 C13 H13 121.8 . . ? F1 C14 C13 117.2(4) . . ? C9 C14 F1 117.6(4) . . ? C9 C14 C13 125.2(4) . . ? S1 C15 H15A 109.7 . . ? S1 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? C16 C15 S1 109.6(3) . . ? C16 C15 H15A 109.7 . . ? C16 C15 H15B 109.7 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? 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 F2 C11 C12 F3 1.1(6) . . . . ? F2 C11 C12 C13 -179.5(4) . . . . ? F3 C12 C13 C14 179.9(4) . . . . ? N2 C4 C5 N4 15.5(6) . . . . ? N2 C4 C5 N6 -164.4(4) . . . . ? N3 C8 C9 C10 45.6(5) . . . . ? N3 C8 C9 C14 -134.8(4) . . . . ? N4 N5 C6 N6 -0.4(5) . . . . ? N5 N4 C5 N6 -0.1(4) . . . . ? N5 N4 C5 C4 180.0(3) . . . . ? C1 N1 C2 S1 -174.7(3) . . . . ? C1 N1 C2 N3 4.6(5) . . . . ? C1 N2 C3 O2 174.0(3) . . . . ? C1 N2 C3 N3 -5.4(5) . . . . ? C1 N2 C4 C5 -98.2(4) . . . . ? C2 S1 C15 C16 167.3(4) . . . . ? C2 N1 C1 O1 171.1(3) . . . . ? C2 N1 C1 N2 -10.9(5) . . . . ? C2 N3 C3 O2 179.1(3) . . . . ? C2 N3 C3 N2 -1.5(5) . . . . ? C2 N3 C8 C9 75.5(4) . . . . ? C3 N2 C1 O1 -170.2(3) . . . . ? C3 N2 C1 N1 11.8(5) . . . . ? C3 N2 C4 C5 70.0(4) . . . . ? C3 N3 C2 S1 -178.7(2) . . . . ? C3 N3 C2 N1 2.0(5) . . . . ? C3 N3 C8 C9 -99.2(4) . . . . ? C4 N2 C1 O1 -2.9(5) . . . . ? C4 N2 C1 N1 179.1(3) . . . . ? C4 N2 C3 O2 6.3(5) . . . . ? C4 N2 C3 N3 -173.2(3) . . . . ? C5 N4 N5 C6 0.3(4) . . . . ? C5 N4 N5 C7 -179.8(4) . . . . ? C5 N6 C6 N5 0.3(5) . . . . ? C6 N6 C5 N4 -0.1(5) . . . . ? C6 N6 C5 C4 179.8(4) . . . . ? C7 N5 C6 N6 179.7(4) . . . . ? C8 N3 C2 S1 6.7(4) . . . . ? C8 N3 C2 N1 -172.6(3) . . . . ? C8 N3 C3 O2 -6.1(5) . . . . ? C8 N3 C3 N2 173.3(3) . . . . ? C8 C9 C10 C11 179.8(4) . . . . ? C8 C9 C14 F1 1.3(5) . . . . ? C8 C9 C14 C13 -179.4(4) . . . . ? C9 C10 C11 F2 179.1(4) . . . . ? C9 C10 C11 C12 -0.2(7) . . . . ? C10 C9 C14 F1 -179.1(3) . . . . ? C10 C9 C14 C13 0.3(6) . . . . ? C10 C11 C12 F3 -179.5(4) . . . . ? C10 C11 C12 C13 -0.1(7) . . . . ? C11 C12 C13 C14 0.5(6) . . . . ? C12 C13 C14 F1 178.7(4) . . . . ? C12 C13 C14 C9 -0.6(6) . . . . ? C14 C9 C10 C11 0.2(6) . . . . ? C15 S1 C2 N1 6.1(4) . . . . ? C15 S1 C2 N3 -173.3(3) . . . . ? _shelx_res_file ; TITL dr_a.res in P2(1)/n dr.res created by SHELXL-2017/1 at 22:35:39 on 09-May-2022 REM Old TITL DR in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.236, Rweak 0.066, Alpha 0.052, Orientation as input REM Formula found by SHELXT: C18 N6 O3 S CELL 0.71073 11.7146 7.738 19.8336 90 95.723 90 ZERR 4 0.0061 0.0039 0.0093 0 0.01 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H F N O S UNIT 64 60 12 24 8 4 L.S. 20 0 0 PLAN 5 SIZE 0.1 0.12 0.14 TEMP 23 CONF BOND $H list 4 MORE -1 fmap 2 53 acta REM REM REM WGHT 0.054200 0.905900 FVAR 0.47079 S1 6 0.170217 0.520683 0.595795 11.00000 0.06021 0.05660 = 0.05729 0.00103 -0.00848 -0.00045 F1 3 0.216102 0.107578 0.529043 11.00000 0.06877 0.08225 = 0.08250 -0.01711 -0.00705 -0.01514 F2 3 0.647771 0.347593 0.523383 11.00000 0.07432 0.13868 = 0.08996 -0.00651 0.03242 -0.01788 F3 3 0.537235 0.210032 0.411560 11.00000 0.11795 0.13338 = 0.06078 -0.00099 0.03354 0.02093 O1 5 0.416414 0.877897 0.754141 11.00000 0.07041 0.05150 = 0.07351 -0.01495 0.00289 -0.00217 O2 5 0.473938 0.298757 0.762334 11.00000 0.05810 0.05620 = 0.05757 0.00473 -0.00615 0.00516 N1 4 0.294606 0.708829 0.686112 11.00000 0.04488 0.05064 = 0.05004 -0.00603 0.00245 0.00037 N2 4 0.438652 0.587693 0.764516 11.00000 0.04374 0.04681 = 0.05049 -0.00843 -0.00086 -0.00079 N3 4 0.335403 0.409464 0.685472 11.00000 0.04370 0.04424 = 0.04381 0.00312 0.00391 0.00057 N4 4 0.658867 0.593920 0.722094 11.00000 0.04350 0.07159 = 0.05418 0.00015 -0.00348 0.00231 N5 4 0.774107 0.569731 0.719953 11.00000 0.05090 0.06198 = 0.05608 0.00110 0.00083 -0.00429 N6 4 0.747609 0.561121 0.827221 11.00000 0.05243 0.09781 = 0.05406 0.00865 -0.00611 -0.00049 C1 1 0.384548 0.734639 0.734823 11.00000 0.04849 0.05295 = 0.04789 -0.00618 0.01558 -0.00133 C2 1 0.275703 0.555197 0.662236 11.00000 0.03847 0.05756 = 0.04007 0.00146 0.00629 -0.00155 C3 1 0.419989 0.423452 0.739483 11.00000 0.03856 0.05844 = 0.04348 0.00620 0.00522 0.00328 C4 1 0.536431 0.607732 0.816161 11.00000 0.05765 0.06368 = 0.05204 -0.00758 -0.00738 -0.00145 AFIX 23 H4A 2 0.531039 0.522062 0.851406 11.00000 -1.20000 H4B 2 0.533180 0.721136 0.836723 11.00000 -1.20000 AFIX 0 C5 1 0.648638 0.587633 0.787244 11.00000 0.05058 0.05054 = 0.04774 0.00111 -0.00645 -0.00633 C6 1 0.823274 0.550359 0.781988 11.00000 0.05178 0.08398 = 0.06883 0.00750 -0.01205 -0.00241 AFIX 43 H6 2 0.901358 0.531471 0.792790 11.00000 -1.20000 AFIX 0 C7 1 0.824196 0.568008 0.656333 11.00000 0.06825 0.09823 = 0.06462 -0.00261 0.01285 0.00313 AFIX 137 H7A 2 0.790081 0.477133 0.628174 11.00000 -1.50000 H7B 2 0.905331 0.548697 0.664631 11.00000 -1.50000 H7C 2 0.810483 0.677048 0.633890 11.00000 -1.50000 AFIX 0 C8 1 0.320145 0.240537 0.651459 11.00000 0.05022 0.04418 = 0.05655 0.00166 0.00291 -0.00329 AFIX 23 H8A 2 0.238861 0.218189 0.640851 11.00000 -1.20000 H8B 2 0.351271 0.150626 0.682045 11.00000 -1.20000 AFIX 0 C9 1 0.378289 0.233550 0.587511 11.00000 0.04625 0.03804 = 0.04485 -0.00078 0.00312 0.00460 C10 1 0.489010 0.294307 0.584952 11.00000 0.05515 0.06610 = 0.04737 -0.00254 0.00691 0.00083 AFIX 43 H10 2 0.529027 0.341200 0.623515 11.00000 -1.20000 AFIX 0 C11 1 0.539333 0.285467 0.526056 11.00000 0.05380 0.06882 = 0.06664 0.00211 0.01195 0.00162 C12 1 0.484089 0.217501 0.468733 11.00000 0.07831 0.07570 = 0.04651 0.00490 0.01611 0.02002 C13 1 0.374810 0.154806 0.468696 11.00000 0.07998 0.06292 = 0.04843 -0.01071 -0.00595 0.01342 AFIX 43 H13 2 0.335658 0.106831 0.430073 11.00000 -1.20000 AFIX 0 C14 1 0.326070 0.166467 0.528643 11.00000 0.04594 0.05036 = 0.06211 -0.00317 -0.00201 0.00075 C15 1 0.128296 0.739733 0.575268 11.00000 0.08545 0.06386 = 0.06769 0.00247 -0.00969 0.01620 AFIX 23 H15A 2 0.085262 0.786435 0.610420 11.00000 -1.20000 H15B 2 0.196039 0.810612 0.572765 11.00000 -1.20000 AFIX 0 C16 1 0.056367 0.743492 0.509050 11.00000 0.13222 0.07748 = 0.11230 -0.00015 -0.06239 0.02206 AFIX 137 H16A 2 0.098019 0.692442 0.474804 11.00000 -1.50000 H16B 2 0.037640 0.861005 0.497005 11.00000 -1.50000 H16C 2 -0.012957 0.679453 0.512630 11.00000 -1.50000 AFIX 0 HKLF 4 REM dr_a.res in P2(1)/n REM R1 = 0.0593 for 1585 Fo > 4sig(Fo) and 0.1600 for all 3161 data REM 255 parameters refined using 0 restraints END WGHT 0.0546 0.8970 REM Highest difference peak 0.222, deepest hole -0.270, 1-sigma level 0.061 Q1 1 -0.1246 0.7148 0.4801 11.00000 0.05 0.22 Q2 1 0.2348 -0.0354 0.4764 11.00000 0.05 0.21 Q3 1 0.0846 0.5348 0.5190 11.00000 0.05 0.20 Q4 1 -0.0248 0.8767 0.5494 11.00000 0.05 0.20 Q5 1 0.1355 0.0213 0.4592 11.00000 0.05 0.20 ; _shelx_res_checksum 69860 _shelx_hkl_file ; -2 0 0 316.87 16.40 -2 0 0 309.17 16.40 -2 0 0 277.57 16.00 -2 0 0 324.27 16.60 -2 0 0 288.67 15.70 -2 0 0 281.87 13.30 2 0 0 285.67 15.50 2 0 0 297.07 13.80 2 0 0 309.37 16.70 2 0 0 308.97 16.10 2 0 0 281.17 15.60 2 0 0 290.47 16.10 -3 0 0 10.70 6.20 -3 0 0 2.60 5.50 -3 0 0 6.90 5.80 -3 0 0 13.00 6.30 -3 0 0 -1.20 3.40 -3 0 0 4.50 5.20 3 0 0 -5.80 3.70 3 0 0 -0.20 3.40 3 0 0 -5.40 3.80 3 0 0 4.30 5.00 3 0 0 -3.70 4.00 3 0 0 2.40 4.40 -4 0 0 25.00 8.10 -4 0 0 14.30 7.40 -4 0 0 24.80 8.60 -4 0 0 31.00 7.40 -4 0 0 21.30 8.10 -4 0 0 33.00 9.00 4 0 0 22.10 7.90 4 0 0 23.60 7.00 4 0 0 27.80 8.80 4 0 0 33.10 9.60 4 0 0 47.60 11.00 4 0 0 29.30 9.00 -5 0 0 4.20 5.90 -5 0 0 -5.60 4.20 -5 0 0 -4.70 5.70 -5 0 0 -3.90 5.10 -5 0 0 6.40 4.90 -5 0 0 -9.60 3.80 5 0 0 1.60 4.90 5 0 0 7.20 6.30 5 0 0 -3.30 5.70 5 0 0 -3.10 4.00 5 0 0 -4.00 4.10 5 0 0 -1.60 4.90 -6 0 0 1059.69 53.09 -6 0 0 974.50 51.99 -6 0 0 1042.40 52.59 -6 0 0 1067.79 54.09 -6 0 0 993.60 51.59 6 0 0 1110.69 54.99 6 0 0 1023.60 52.19 6 0 0 1070.49 53.49 6 0 0 971.70 52.19 6 0 0 1022.90 51.69 6 0 0 957.20 43.40 -7 0 0 -8.10 4.70 -7 0 0 -6.50 5.60 -7 0 0 -2.90 5.30 -7 0 0 -1.90 4.80 -7 0 0 -1.10 8.10 7 0 0 -0.70 8.00 7 0 0 -5.30 5.60 7 0 0 -1.30 6.20 7 0 0 5.10 5.90 7 0 0 0.10 6.00 7 0 0 1.90 7.00 7 0 0 3.70 6.90 -8 0 0 59.89 16.90 -8 0 0 85.89 20.30 -8 0 0 112.59 23.10 -8 0 0 74.69 20.10 -8 0 0 61.19 17.60 8 0 0 69.59 18.10 8 0 0 84.99 19.50 8 0 0 93.99 17.40 8 0 0 82.39 20.80 8 0 0 81.99 17.10 8 0 0 73.99 18.30 8 0 0 106.39 22.80 -9 0 0 9.90 9.80 -9 0 0 -1.30 7.50 9 0 0 -5.10 9.60 9 0 0 21.00 9.40 9 0 0 20.40 11.90 9 0 0 13.40 11.70 9 0 0 12.20 11.00 9 0 0 16.80 11.20 -10 0 0 100.99 24.40 -10 0 0 79.39 20.20 -10 0 0 61.39 20.60 -10 0 0 63.69 21.80 -10 0 0 54.59 21.80 10 0 0 67.59 20.30 10 0 0 35.40 16.20 10 0 0 111.79 26.90 10 0 0 59.29 18.50 10 0 0 55.99 21.10 10 0 0 65.89 17.50 10 0 0 83.39 19.80 -11 0 0 -8.90 12.00 -11 0 0 15.00 17.20 -11 0 0 4.00 10.70 11 0 0 6.60 15.80 11 0 0 24.60 16.60 11 0 0 -5.90 11.60 11 0 0 5.50 11.60 -12 0 0 23.30 17.00 -13 0 0 -14.30 19.30 -13 1 0 9.20 20.50 12 -1 0 -15.10 29.00 12 -1 0 0.50 14.30 -12 1 0 7.80 14.20 11 -1 0 83.09 24.30 11 -1 0 99.79 28.00 11 -1 0 126.99 28.20 11 -1 0 76.49 25.80 11 -1 0 91.89 26.00 -11 1 0 148.79 30.20 -11 1 0 99.19 25.20 -11 1 0 73.29 21.80 10 -1 0 7.00 13.10 10 -1 0 -9.20 10.70 10 -1 0 -9.70 10.50 10 -1 0 9.00 13.20 -10 1 0 -11.10 11.00 -10 1 0 -8.60 12.10 -10 1 0 6.20 9.40 -10 1 0 15.40 13.40 -10 1 0 -0.10 12.20 9 -1 0 24.00 15.40 9 -1 0 11.40 9.50 9 -1 0 7.60 11.40 9 -1 0 30.00 14.00 9 -1 0 5.60 12.90 9 -1 0 31.10 14.70 -9 1 0 34.70 17.10 -9 1 0 37.50 17.10 -9 1 0 21.10 12.10 -9 1 0 -1.10 12.50 -9 1 0 31.40 16.30 -9 1 0 42.10 13.70 8 -1 0 280.77 31.60 8 -1 0 272.27 32.00 8 -1 0 310.17 32.40 8 -1 0 321.37 33.90 8 -1 0 234.78 29.70 8 -1 0 318.97 29.30 -8 1 0 334.17 33.20 -8 1 0 291.17 27.70 -8 1 0 305.67 31.70 -8 1 0 333.77 34.10 -8 1 0 274.07 32.50 -8 1 0 279.47 31.90 7 -1 0 11.80 10.30 7 -1 0 7.90 9.60 7 -1 0 8.40 8.20 7 -1 0 29.40 12.70 7 -1 0 27.50 11.90 -7 1 0 7.30 8.50 -7 1 0 13.40 9.30 -7 1 0 23.40 11.20 -7 1 0 5.30 7.60 -7 1 0 13.50 8.10 -7 1 0 11.00 9.30 6 -1 0 220.18 23.80 6 -1 0 202.28 23.00 6 -1 0 177.08 21.20 6 -1 0 221.48 23.90 6 -1 0 220.98 23.20 6 -1 0 201.98 22.50 -6 1 0 176.38 21.10 -6 1 0 212.18 23.10 -6 1 0 191.28 19.70 -6 1 0 157.18 20.00 -6 1 0 188.78 22.20 -6 1 0 163.38 20.10 5 -1 0 8.20 7.10 5 -1 0 7.80 7.70 5 -1 0 6.20 5.60 5 -1 0 -5.60 4.60 5 -1 0 5.70 6.20 -5 1 0 13.10 6.50 -5 1 0 16.50 8.30 -5 1 0 8.10 6.30 -5 1 0 0.80 5.80 -5 1 0 11.40 7.30 -5 1 0 -2.00 3.90 4 -1 0 12.30 6.50 4 -1 0 4.70 5.10 4 -1 0 0.90 4.30 4 -1 0 -3.20 5.50 4 -1 0 7.40 5.70 -4 1 0 2.30 3.70 -4 1 0 -0.60 3.20 -4 1 0 -3.40 4.00 -4 1 0 4.70 5.10 -4 1 0 3.80 4.30 -4 1 0 -2.30 3.10 3 -1 0 466.75 26.10 3 -1 0 455.65 25.50 3 -1 0 444.46 25.20 3 -1 0 455.75 24.60 3 -1 0 467.85 25.50 3 -1 0 442.66 25.10 -3 1 0 485.55 26.00 -3 1 0 427.66 25.10 -3 1 0 465.55 24.90 -3 1 0 430.06 24.20 -3 1 0 467.75 25.70 -3 1 0 435.46 25.20 2 -1 0 394.96 19.80 2 -1 0 386.46 20.40 2 -1 0 357.26 19.20 2 -1 0 368.16 19.30 2 -1 0 368.56 20.50 2 -1 0 316.67 18.60 -2 1 0 321.37 18.90 -2 1 0 331.37 18.70 -2 1 0 362.56 19.60 -2 1 0 342.37 18.90 -2 1 0 388.46 20.00 1 -1 0 190.08 11.30 1 -1 0 172.68 11.40 1 -1 0 169.68 14.70 1 -1 0 166.38 11.60 1 -1 0 196.08 11.60 -1 1 0 186.68 11.70 -1 1 0 181.18 12.00 -1 1 0 184.38 11.50 0 -1 0 -1.40 1.60 0 -1 0 0.80 2.40 0 -1 0 4.20 2.50 0 1 0 -2.80 1.30 -1 -1 0 138.79 14.40 -1 -1 0 187.58 11.40 -1 -1 0 188.98 12.40 -1 -1 0 190.68 11.30 -1 -1 0 169.78 10.00 -1 -1 0 137.99 15.20 1 1 0 158.08 11.20 1 1 0 179.98 11.80 1 1 0 184.18 9.30 1 1 0 186.18 11.30 -2 -1 0 381.06 19.80 -2 -1 0 351.66 19.10 -2 -1 0 355.96 14.40 -2 -1 0 347.57 20.70 -2 -1 0 320.97 18.90 2 1 0 364.96 19.80 2 1 0 368.46 22.30 2 1 0 361.96 14.40 2 1 0 360.16 19.50 2 1 0 368.56 19.50 2 1 0 336.47 19.90 -3 -1 0 446.66 18.30 -3 -1 0 450.05 25.20 -3 -1 0 462.75 25.40 -3 -1 0 417.46 24.30 -3 -1 0 474.75 27.40 -3 -1 0 442.56 24.90 3 1 0 464.85 25.50 3 1 0 449.26 26.00 3 1 0 473.05 25.60 3 1 0 451.25 24.90 3 1 0 442.66 18.30 3 1 0 388.36 23.70 -4 -1 0 -5.30 4.30 -4 -1 0 0.30 3.60 -4 -1 0 -0.40 4.80 -4 -1 0 5.50 5.10 -4 -1 0 2.60 5.00 4 1 0 4.60 5.40 4 1 0 7.20 3.90 4 1 0 6.30 6.80 4 1 0 -3.60 2.90 4 1 0 2.90 5.00 4 1 0 1.00 3.80 4 1 0 -0.10 3.40 -5 -1 0 -0.20 5.00 -5 -1 0 3.20 4.50 -5 -1 0 -1.80 5.50 -5 -1 0 6.70 6.60 -5 -1 0 6.60 5.90 5 1 0 3.70 4.10 5 1 0 -1.10 3.80 5 1 0 9.30 6.80 5 1 0 22.70 9.60 5 1 0 9.40 6.40 5 1 0 -0.20 3.70 -6 -1 0 179.48 21.70 -6 -1 0 213.78 22.90 -6 -1 0 231.58 24.70 -6 -1 0 191.58 22.00 6 1 0 208.48 16.40 6 1 0 226.58 24.00 6 1 0 209.38 23.40 6 1 0 203.08 22.90 6 1 0 187.28 21.00 6 1 0 174.88 15.50 -7 -1 0 12.90 8.50 -7 -1 0 19.80 10.60 -7 -1 0 30.00 19.70 -7 -1 0 19.40 9.40 -7 -1 0 -1.00 7.60 7 1 0 16.50 10.10 7 1 0 6.40 9.50 7 1 0 14.00 9.20 7 1 0 14.60 10.00 7 1 0 -0.10 5.90 -8 -1 0 319.07 31.80 -8 -1 0 241.88 30.80 -8 -1 0 243.18 40.10 -8 -1 0 288.97 33.00 -8 -1 0 268.27 31.30 8 1 0 258.47 22.20 8 1 0 290.57 30.90 8 1 0 330.77 33.50 8 1 0 273.47 22.70 8 1 0 244.78 30.40 8 1 0 315.47 31.70 8 1 0 311.37 31.70 -9 -1 0 41.80 17.30 -9 -1 0 26.50 16.70 -9 -1 0 15.40 13.90 -9 -1 0 10.50 11.70 -9 -1 0 6.40 10.60 9 1 0 9.10 11.10 9 1 0 25.00 15.70 9 1 0 29.60 15.40 9 1 0 16.10 8.90 9 1 0 20.30 13.10 9 1 0 41.40 16.70 -10 -1 0 -8.50 12.70 -10 -1 0 58.89 20.40 -10 -1 0 -17.40 10.80 -10 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13.20 -9 4 -3 4.60 15.90 -9 4 -3 -16.90 13.70 9 -4 3 6.50 16.40 9 -4 3 10.40 13.10 9 -4 3 22.20 17.80 9 -4 3 16.00 17.80 -10 4 -3 41.80 23.70 10 -4 3 36.10 27.60 10 -4 3 36.70 26.60 10 -4 3 43.10 21.60 -11 4 -3 49.90 32.40 11 -4 3 2.70 21.10 12 -4 3 20.20 27.80 -13 -3 3 -24.80 17.90 -11 -3 3 16.30 17.60 10 3 -3 -8.10 9.40 10 3 -3 1.70 11.60 -10 -3 3 18.30 18.40 -10 -3 3 -5.70 17.80 -10 -3 3 -6.30 16.80 9 3 -3 76.29 22.80 9 3 -3 86.29 23.30 9 3 -3 46.10 17.40 9 3 -3 45.00 13.20 9 3 -3 71.89 24.80 9 3 -3 35.30 19.10 -9 -3 3 99.19 23.80 -9 -3 3 34.60 19.60 -9 -3 3 76.49 25.50 -9 -3 3 78.79 24.20 -9 -3 3 73.19 21.60 8 3 -3 4.20 8.80 8 3 -3 28.60 15.60 8 3 -3 -10.80 9.40 8 3 -3 23.00 13.80 8 3 -3 -6.50 7.90 -8 -3 3 -10.00 7.00 -8 -3 3 22.90 15.30 -8 -3 3 15.10 14.70 -8 -3 3 -4.60 12.80 -8 -3 3 -7.50 9.30 -8 -3 3 -0.80 9.90 7 3 -3 10.40 12.10 7 3 -3 21.60 12.80 7 3 -3 -10.10 7.00 7 3 -3 -1.40 7.30 -7 -3 3 6.60 10.20 -7 -3 3 9.60 10.10 -7 -3 3 15.10 10.50 -7 -3 3 5.30 10.60 -7 -3 3 14.70 11.80 6 3 -3 18.30 8.60 6 3 -3 14.70 10.30 6 3 -3 0.00 9.20 6 3 -3 11.50 10.70 6 3 -3 0.30 6.80 6 3 -3 11.40 10.50 -6 -3 3 16.20 10.70 -6 -3 3 31.60 13.30 -6 -3 3 15.50 8.70 -6 -3 3 -3.10 9.90 -6 -3 3 29.60 14.00 5 3 -3 177.58 21.40 5 3 -3 178.18 19.20 5 3 -3 180.58 22.70 5 3 -3 190.78 24.30 5 3 -3 220.38 24.00 5 3 -3 152.68 24.70 -5 -3 3 163.78 26.80 -5 -3 3 134.69 22.90 -5 -3 3 165.18 18.90 -5 -3 3 183.18 23.70 -5 -3 3 168.58 21.30 -5 -3 3 140.79 23.60 4 3 -3 97.49 19.00 4 3 -3 90.99 18.30 4 3 -3 106.09 19.00 4 3 -3 119.39 19.80 4 3 -3 90.59 15.80 -4 -3 3 103.99 20.70 -4 -3 3 91.89 17.10 -4 -3 3 83.09 19.40 -4 -3 3 100.39 16.20 -4 -3 3 70.89 15.60 -4 -3 3 79.39 17.60 3 3 -3 59.09 14.20 3 3 -3 60.09 14.50 3 3 -3 44.60 12.80 3 3 -3 54.19 12.90 3 3 -3 74.69 16.00 3 3 -3 47.40 11.20 -3 -3 3 56.89 12.60 -3 -3 3 59.39 14.10 -3 -3 3 56.69 13.70 -3 -3 3 53.39 14.40 -3 -3 3 44.70 11.20 -3 -3 3 43.20 13.10 2 3 -3 14.50 7.70 2 3 -3 6.30 6.50 2 3 -3 21.30 8.80 2 3 -3 8.10 6.10 2 3 -3 10.70 7.30 2 3 -3 5.80 5.70 -2 -3 3 11.00 7.80 -2 -3 3 12.60 7.90 -2 -3 3 24.50 9.10 -2 -3 3 7.30 7.10 -2 -3 3 18.80 8.50 1 3 -3 247.48 22.20 1 3 -3 239.78 22.00 1 3 -3 274.07 22.30 1 3 -3 224.18 20.50 1 3 -3 250.17 22.10 1 3 -3 274.67 23.30 -1 -3 3 241.28 21.50 -1 -3 3 252.27 21.60 -1 -3 3 205.58 19.80 -1 -3 3 240.28 22.10 -1 -3 3 265.47 23.10 -1 -3 3 202.18 19.20 0 3 -3 4.50 6.30 0 3 -3 9.10 6.50 0 3 -3 7.20 8.00 0 3 -3 7.00 7.20 0 3 -3 7.40 7.10 0 -3 3 -7.60 5.00 0 -3 3 2.90 5.70 0 -3 3 0.50 4.70 0 -3 3 -7.80 6.30 0 -3 3 9.50 7.40 -1 3 -3 6.50 7.50 -1 3 -3 12.30 8.60 -1 3 -3 10.20 6.70 -1 3 -3 -0.80 4.60 -1 3 -3 3.40 5.90 -1 3 -3 5.50 6.00 1 -3 3 1.30 4.60 1 -3 3 10.20 6.50 1 -3 3 8.60 6.40 1 -3 3 6.90 6.10 1 -3 3 2.10 6.40 -2 3 -3 355.96 28.30 -2 3 -3 345.07 27.20 -2 3 -3 349.17 27.50 -2 3 -3 330.77 26.80 -2 3 -3 387.76 29.50 2 -3 3 420.66 30.20 2 -3 3 358.76 27.80 2 -3 3 393.96 29.40 2 -3 3 386.96 25.20 2 -3 3 346.67 24.20 2 -3 3 340.97 29.10 2 -3 3 359.46 28.10 -3 3 -3 400.86 30.00 -3 3 -3 435.36 31.70 -3 3 -3 346.47 37.70 -3 3 -3 378.96 29.90 -3 3 -3 423.96 31.90 3 -3 3 391.76 26.30 3 -3 3 411.46 31.40 3 -3 3 454.85 33.00 3 -3 3 459.05 34.10 3 -3 3 464.05 32.30 3 -3 3 373.06 26.00 3 -3 3 371.16 29.90 -4 3 -3 149.69 23.40 -4 3 -3 184.58 21.50 -4 3 -3 176.38 22.20 -4 3 -3 173.28 21.40 -4 3 -3 166.28 21.60 -4 3 -3 165.68 18.00 4 -3 3 189.48 19.30 4 -3 3 167.88 25.10 4 -3 3 159.48 20.40 4 -3 3 165.78 21.20 4 -3 3 206.58 24.80 -5 3 -3 102.09 20.50 -5 3 -3 100.59 19.70 -5 3 -3 88.99 19.40 -5 3 -3 83.59 16.60 -5 3 -3 75.29 18.30 -5 3 -3 107.09 20.30 5 -3 3 74.89 19.00 5 -3 3 83.89 19.80 5 -3 3 119.19 22.70 5 -3 3 77.79 15.10 5 -3 3 89.79 20.60 5 -3 3 91.79 18.40 -6 3 -3 -14.70 7.30 -6 3 -3 12.20 10.40 -6 3 -3 7.40 8.20 -6 3 -3 1.00 5.30 -6 3 -3 2.30 6.00 -6 3 -3 6.10 9.70 6 -3 3 -15.40 7.20 6 -3 3 9.00 10.10 6 -3 3 -1.30 6.60 6 -3 3 5.90 7.70 -7 3 -3 7.90 10.10 -7 3 -3 15.00 13.30 -7 3 -3 41.60 17.50 -7 3 -3 15.60 12.20 -7 3 -3 24.40 15.80 -7 3 -3 20.40 10.30 7 -3 3 36.90 16.60 7 -3 3 30.90 16.70 7 -3 3 54.99 15.10 7 -3 3 15.00 11.50 7 -3 3 18.40 13.50 7 -3 3 37.10 14.20 -8 3 -3 -7.30 12.00 -8 3 -3 1.70 9.60 -8 3 -3 -7.80 8.00 -8 3 -3 9.00 12.60 -8 3 -3 -16.10 10.70 8 -3 3 20.00 13.00 8 -3 3 0.80 12.50 8 -3 3 11.30 14.80 8 -3 3 -6.10 12.50 8 -3 3 10.40 14.30 -9 3 -3 249.88 41.30 -9 3 -3 204.98 33.40 -9 3 -3 183.08 35.20 -9 3 -3 186.58 33.10 -9 3 -3 177.98 29.90 -9 3 -3 98.39 28.00 9 -3 3 171.28 32.20 9 -3 3 278.27 35.30 9 -3 3 280.67 40.50 9 -3 3 187.48 32.00 9 -3 3 157.48 31.70 -10 3 -3 91.29 29.60 -10 3 -3 82.69 22.50 -10 3 -3 75.89 23.50 10 -3 3 74.99 24.80 10 -3 3 62.09 26.50 10 -3 3 79.69 29.30 -11 3 -3 -18.10 11.40 -11 3 -3 -15.70 19.00 11 -3 3 8.20 18.30 11 -3 3 -39.30 24.30 12 -3 3 -38.50 17.20 -13 -2 3 44.40 23.60 11 2 -3 11.90 21.70 -11 -2 3 11.90 13.50 10 2 -3 7.00 12.20 10 2 -3 -14.40 9.80 10 2 -3 4.00 14.90 10 2 -3 24.00 16.40 10 2 -3 5.20 13.40 -10 -2 3 1.30 10.50 -10 -2 3 -2.90 18.00 -10 -2 3 -16.50 10.60 -10 -2 3 -1.50 11.00 -10 -2 3 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140.09 16.40 5 2 -3 169.08 20.50 5 2 -3 121.89 20.80 -5 -2 3 154.88 19.10 -5 -2 3 144.19 15.70 -5 -2 3 134.89 22.90 -5 -2 3 133.89 21.80 -5 -2 3 173.98 20.40 -5 -2 3 113.99 19.60 4 2 -3 8.70 8.20 4 2 -3 4.90 7.00 4 2 -3 1.00 5.40 4 2 -3 2.70 4.90 4 2 -3 10.20 8.30 -4 -2 3 6.80 7.10 -4 -2 3 11.40 7.70 -4 -2 3 6.20 5.90 -4 -2 3 -2.80 5.40 -4 -2 3 6.30 7.50 -4 -2 3 12.90 8.60 3 2 -3 36.30 10.20 3 2 -3 35.10 9.40 3 2 -3 26.70 9.30 3 2 -3 22.70 8.60 3 2 -3 43.30 9.70 3 2 -3 27.30 9.50 -3 -2 3 26.60 10.10 -3 -2 3 40.60 10.60 -3 -2 3 28.60 8.90 -3 -2 3 29.60 9.50 -3 -2 3 30.50 10.10 -3 -2 3 23.80 9.00 2 2 -3 106.49 13.10 2 2 -3 92.19 14.30 2 2 -3 94.09 12.50 2 2 -3 111.39 13.80 2 2 -3 87.69 14.20 2 2 -3 84.79 14.00 -2 -2 3 79.79 13.50 -2 -2 3 89.69 14.40 -2 -2 3 112.49 13.40 -2 -2 3 87.99 13.70 -2 -2 3 108.89 13.70 -2 -2 3 116.89 14.40 1 2 -3 431.66 25.70 1 2 -3 433.16 24.50 1 2 -3 465.55 26.60 1 2 -3 460.25 26.40 1 2 -3 452.35 27.00 1 2 -3 467.55 26.40 -1 -2 3 418.06 25.60 -1 -2 3 455.35 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38.50 15.50 -9 4 -5 40.10 21.60 9 -4 5 40.00 32.20 10 -4 5 -21.50 15.00 11 -4 5 12.70 24.40 -13 -3 5 41.00 25.40 -12 -3 5 28.60 18.30 -11 -3 5 13.30 17.60 10 3 -5 69.39 28.80 10 3 -5 117.69 30.60 10 3 -5 63.79 18.80 -10 -3 5 54.69 30.70 -10 -3 5 40.20 18.50 -10 -3 5 46.80 22.50 9 3 -5 11.80 14.80 9 3 -5 5.20 16.40 9 3 -5 0.60 10.10 9 3 -5 34.40 17.40 9 3 -5 -4.50 8.30 -9 -3 5 -2.30 13.30 -9 -3 5 15.30 19.60 -9 -3 5 -5.40 9.70 -9 -3 5 -5.30 10.70 -9 -3 5 14.80 15.70 -9 -3 5 2.20 8.40 8 3 -5 13.70 12.10 8 3 -5 18.90 16.00 8 3 -5 67.89 21.20 8 3 -5 53.39 17.10 8 3 -5 47.40 18.50 -8 -3 5 25.10 17.10 -8 -3 5 9.70 15.70 -8 -3 5 51.89 15.60 -8 -3 5 20.70 12.80 -8 -3 5 42.50 17.50 -8 -3 5 44.40 17.70 7 3 -5 -5.00 5.50 7 3 -5 -5.30 10.30 7 3 -5 1.00 7.50 7 3 -5 5.40 8.20 7 3 -5 4.80 9.90 -7 -3 5 -13.70 8.10 -7 -3 5 10.20 8.70 -7 -3 5 31.40 14.10 -7 -3 5 7.40 9.40 -7 -3 5 3.50 13.00 -7 -3 5 3.40 10.10 6 3 -5 9.90 11.20 6 3 -5 17.60 12.40 6 3 -5 22.20 13.80 6 3 -5 26.40 13.50 6 3 -5 19.30 12.20 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21.30 1 3 -22 42.30 20.20 -1 -3 22 2.30 16.50 -1 -3 22 -47.30 20.80 0 3 -22 -6.70 19.30 0 -3 22 13.30 20.80 0 -3 22 14.30 17.80 5 2 -22 9.80 15.30 -5 -2 22 -3.60 12.70 4 2 -22 7.40 13.30 -4 -2 22 30.40 16.80 -4 -2 22 -37.90 17.30 -3 -2 22 11.90 21.30 -3 -2 22 4.60 14.80 -2 -2 22 24.10 34.00 1 2 -22 -33.10 20.00 -1 -2 22 -32.30 12.20 0 2 -22 -9.40 14.00 0 -2 22 -30.50 11.80 -1 2 -22 -26.60 11.10 1 -2 22 -3.80 16.20 1 -2 22 19.80 20.70 -2 2 -22 20.10 17.70 2 -2 22 34.60 18.90 2 -2 22 -29.10 21.10 6 1 -22 -22.10 12.60 -6 -1 22 14.10 17.70 5 1 -22 21.70 13.60 -5 -1 22 -47.00 19.10 -5 -1 22 -33.60 12.80 -4 -1 22 43.30 25.40 -3 -1 22 6.80 15.50 2 1 -22 12.40 15.00 -2 -1 22 25.70 19.40 -1 -1 22 -18.20 15.20 -1 -1 22 12.30 14.20 0 -1 22 -0.30 12.00 0 -1 22 1.70 22.50 -1 1 -22 -9.90 12.50 1 -1 22 -0.60 24.70 -2 1 -22 20.40 17.80 2 -1 22 -5.90 20.20 2 -1 22 33.70 15.90 -3 1 -22 -28.30 15.00 3 -1 22 -23.90 16.80 3 -1 22 33.70 26.00 6 0 -22 11.50 12.30 -6 0 22 -12.80 9.80 -6 0 22 -25.00 18.90 5 0 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-5.30 4.60 -5 2 22 6.90 8.90 4 -2 -22 28.40 29.90 3 -2 -22 -15.30 23.40 -3 2 22 -2.50 7.30 2 -2 -22 -31.30 19.40 -2 2 22 -2.30 6.00 -1 2 22 -0.50 6.40 -1 2 22 -7.60 17.80 0 2 22 35.00 23.00 1 2 22 3.10 7.80 -2 -2 -22 12.60 9.60 2 2 22 9.30 11.10 3 -3 -22 -3.00 22.20 2 -3 -22 1.50 21.70 2 2 -23 36.90 17.50 -2 -2 23 0.30 14.00 1 2 -23 41.60 18.60 -1 -2 23 4.10 17.10 4 1 -23 -20.20 11.60 -4 -1 23 35.30 15.10 3 1 -23 7.20 13.00 -3 -1 23 8.00 12.50 -3 -1 23 -19.50 17.80 2 1 -23 -12.10 10.10 -2 -1 23 14.40 13.00 1 1 -23 -9.40 12.00 -1 -1 23 12.10 12.50 -1 -1 23 -8.20 19.10 0 1 -23 -15.60 12.30 0 -1 23 28.00 23.30 0 -1 23 5.90 10.00 -1 1 -23 16.00 14.80 1 -1 23 32.50 19.70 4 0 -23 9.60 12.40 -4 0 23 26.40 13.10 3 0 -23 15.50 11.70 -3 0 23 -25.40 11.10 2 0 -23 8.70 12.00 -2 0 23 -14.90 11.80 1 0 -23 9.40 11.90 -1 0 23 28.10 24.60 0 0 -23 -2.10 12.00 0 0 23 -6.80 23.70 0 0 23 -12.20 11.40 -1 0 -23 32.50 16.20 1 0 23 37.60 18.00 1 0 23 28.40 23.70 4 -1 -23 4.10 10.70 -4 1 23 -13.20 9.20 3 -1 -23 6.00 15.10 -3 1 23 -37.70 28.90 -3 1 23 -8.80 9.40 -2 1 23 28.60 12.60 -2 1 23 -13.70 21.10 1 -1 -23 11.20 10.90 -1 1 23 -39.50 20.40 -1 1 23 6.00 10.50 0 -1 -23 -1.60 10.10 0 1 23 -4.00 10.90 0 1 23 -11.10 21.00 -1 -1 -23 10.40 12.10 1 1 23 -14.70 9.20 -2 2 23 9.60 8.00 -1 2 23 -1.80 7.40 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 60577 _olex2_submission_special_instructions 'No special instructions were received'