#============================================================================= data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 13 _journal_issue 1 _journal_year 2022 _journal_page_first 91 _journal_page_last 98 #============================================================================= data_STE_ZnTHCA_09052019_0m_a _audit_creation_method 'SHELXL-2018/3' _shelx_SHELXL_version_number '2018/3' _chemical_name_systematic ? _chemical_name_common Inorganic _chemical_melting_point ? _chemical_formula_moiety 'C21 H18 Cl N3 S4 Zn' _chemical_formula_sum 'C21 H18 Cl N3 S4 Zn' _chemical_formula_weight 541.44 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7603(4) _cell_length_b 10.7488(6) _cell_length_c 13.0262(7) _cell_angle_alpha 103.965(2) _cell_angle_beta 91.913(2) _cell_angle_gamma 104.944(2) _cell_volume 1144.07(10) _cell_formula_units_Z 2 _cell_measurement_temperature 302(2) _cell_measurement_reflns_used 8661 _cell_measurement_theta_min 2.4189 _cell_measurement_theta_max 29.9119 _exptl_crystal_description block _exptl_crystal_colour 'clear' _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.572 _exptl_crystal_F_000 552 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.330 _exptl_crystal_size_mid 0.270 _exptl_crystal_size_min 0.250 _exptl_absorpt_coefficient_mu 1.569 _shelx_estimated_absorpt_T_min 0.607 _shelx_estimated_absorpt_T_max 0.676 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5995 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 302(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker D8 Quest XRD' _diffrn_measurement_method 'Omega and Phi Scans' _diffrn_detector_area_resol_mean 7.3910 _diffrn_reflns_number 14892 _diffrn_reflns_av_unetI/netI 0.0230 _diffrn_reflns_av_R_equivalents 0.0188 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.419 _diffrn_reflns_theta_max 28.260 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measured_fraction_theta_full 0.982 _diffrn_reflns_Laue_measured_fraction_max 0.981 _diffrn_reflns_Laue_measured_fraction_full 0.982 _diffrn_reflns_point_group_measured_fraction_max 0.981 _diffrn_reflns_point_group_measured_fraction_full 0.982 _reflns_number_total 5570 _reflns_number_gt 4720 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _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. ; _computing_data_collection ? _computing_cell_refinement 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_data_reduction 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 924)' _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1835P)^2^+2.0288P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 5570 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0891 _refine_ls_R_factor_gt 0.0810 _refine_ls_wR_factor_ref 0.2788 _refine_ls_wR_factor_gt 0.2681 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Zn1 Zn 0.24934(6) 0.32709(6) 0.12712(4) 0.0448(2) Uani 1 1 d . . . . . Cl1 Cl 0.33194(15) 0.27393(15) -0.04014(9) 0.0492(3) Uani 1 1 d . . . . . S1 S 0.28440(16) 0.14492(14) 0.21759(11) 0.0527(4) Uani 1 1 d . . . . . S2 S 0.45211(18) 0.43016(13) 0.27186(11) 0.0516(4) Uani 1 1 d . . . . . S3 S 0.9134(3) 0.29464(19) 0.36328(13) 0.0701(5) Uani 1 1 d . . . . . N3 N 0.5246(5) 0.2608(4) 0.3711(3) 0.0460(9) Uani 1 1 d . . . . . N4 N -0.0006(5) 0.2644(5) 0.1108(3) 0.0464(9) Uani 1 1 d . . . . . S4 S 0.4545(4) 0.2053(3) 0.6125(3) 0.1133(9) Uani 1 1 d . . . . . N5 N 0.1831(6) 0.5093(5) 0.1361(3) 0.0483(10) Uani 1 1 d . . . . . C1 C 0.4303(6) 0.2756(5) 0.2954(4) 0.0415(9) Uani 1 1 d . . . . . C2 C 0.5012(7) 0.1332(5) 0.3990(4) 0.0480(11) Uani 1 1 d . . . . . H2A H 0.603986 0.123020 0.419046 0.058 Uiso 1 1 calc R U . . . H2AB H 0.452773 0.061308 0.336694 0.058 Uiso 1 1 calc R U . . . C3 C 0.3988(7) 0.1208(5) 0.4883(5) 0.0509(12) Uani 1 1 d . . . . . C4 C 0.2259(4) 0.0144(3) 0.4712(3) 0.0242(7) Uani 1 1 d . . . . . H4 H 0.166475 -0.045566 0.410516 0.029 Uiso 1 1 calc R U . . . C5 C 0.1918(9) 0.0449(8) 0.5887(7) 0.0752(19) Uani 1 1 d . . . . . H5 H 0.098284 -0.000426 0.610465 0.090 Uiso 1 1 calc R U . . . C6 C 0.3030(11) 0.1394(9) 0.6576(8) 0.084(2) Uani 1 1 d . . . . . H6 H 0.289726 0.164412 0.729511 0.101 Uiso 1 1 calc R U . . . C7 C 0.6494(7) 0.3758(5) 0.4400(5) 0.0537(13) Uani 1 1 d . . . . . H7A H 0.608850 0.405405 0.507352 0.064 Uiso 1 1 calc R U . . . H7AB H 0.669904 0.448818 0.406288 0.064 Uiso 1 1 calc R U . . . C8 C 0.8026(6) 0.3452(5) 0.4614(4) 0.0461(10) Uani 1 1 d . . . . . C9 C 0.8747(6) 0.3559(5) 0.5643(4) 0.0465(11) Uani 1 1 d . . . . . H9 H 0.833160 0.379622 0.628614 0.056 Uiso 1 1 calc R U . . . C10 C 1.0227(7) 0.3235(7) 0.5504(6) 0.0629(15) Uani 1 1 d . . . . . H10 H 1.090876 0.326153 0.607668 0.075 Uiso 1 1 calc R U . . . C11 C 1.0560(8) 0.2894(7) 0.4506(7) 0.0673(17) Uani 1 1 d . . . . . H11 H 1.147733 0.265422 0.431176 0.081 Uiso 1 1 calc R U . . . C12 C 0.2828(8) 0.6291(7) 0.1518(5) 0.0604(14) Uani 1 1 d . . . . . H12 H 0.391037 0.636839 0.151795 0.072 Uiso 1 1 calc R U . . . C13 C 0.2318(12) 0.7448(7) 0.1685(6) 0.077(2) Uani 1 1 d . . . . . H13 H 0.304490 0.828204 0.180360 0.092 Uiso 1 1 calc R U . . . C14 C 0.0708(11) 0.7321(8) 0.1668(6) 0.076(2) Uani 1 1 d . . . . . H14 H 0.033176 0.807051 0.176588 0.091 Uiso 1 1 calc R U . . . C15 C -0.0325(9) 0.6085(8) 0.1507(5) 0.0676(18) Uani 1 1 d . . . . . H15 H -0.141162 0.598793 0.150560 0.081 Uiso 1 1 calc R U . . . C16 C 0.0254(7) 0.4972(6) 0.1345(4) 0.0495(12) Uani 1 1 d . . . . . C17 C -0.0771(6) 0.3585(6) 0.1162(4) 0.0476(11) Uani 1 1 d . . . . . C18 C -0.2424(7) 0.3253(8) 0.1033(5) 0.0621(15) Uani 1 1 d . . . . . H18 H -0.293775 0.391583 0.106259 0.074 Uiso 1 1 calc R U . . . C19 C -0.3287(8) 0.1963(10) 0.0866(6) 0.078(2) Uani 1 1 d . . . . . H19 H -0.439107 0.173858 0.079205 0.093 Uiso 1 1 calc R U . . . C20 C -0.2494(8) 0.0976(8) 0.0805(6) 0.0715(18) Uani 1 1 d . . . . . H20 H -0.305258 0.008339 0.068213 0.086 Uiso 1 1 calc R U . . . C21 C -0.0822(7) 0.1381(7) 0.0936(5) 0.0591(14) Uani 1 1 d . . . . . H21 H -0.027488 0.073887 0.090080 0.071 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 Zn1 0.0418(4) 0.0608(4) 0.0388(4) 0.0133(3) 0.0035(2) 0.0259(3) Cl1 0.0537(7) 0.0791(8) 0.0303(5) 0.0171(5) 0.0127(4) 0.0412(6) S1 0.0471(7) 0.0585(8) 0.0521(7) 0.0163(6) -0.0084(5) 0.0135(6) S2 0.0649(8) 0.0491(7) 0.0478(7) 0.0141(5) -0.0056(6) 0.0277(6) S3 0.0874(12) 0.0737(10) 0.0493(8) 0.0148(7) 0.0132(7) 0.0224(9) N3 0.053(2) 0.0413(19) 0.045(2) 0.0103(16) -0.0098(17) 0.0187(17) N4 0.040(2) 0.064(3) 0.039(2) 0.0100(18) 0.0035(15) 0.0242(18) S4 0.126(2) 0.0982(18) 0.103(2) 0.0183(15) 0.0053(16) 0.0159(16) N5 0.053(2) 0.061(3) 0.038(2) 0.0135(18) 0.0015(17) 0.030(2) C1 0.043(2) 0.049(2) 0.038(2) 0.0123(18) 0.0043(17) 0.0228(19) C2 0.055(3) 0.042(2) 0.049(3) 0.011(2) -0.009(2) 0.020(2) C3 0.055(3) 0.041(2) 0.057(3) 0.013(2) -0.009(2) 0.015(2) C4 0.0168(13) 0.0183(13) 0.0387(18) 0.0159(13) -0.0089(12) 0.0003(10) C5 0.064(4) 0.081(4) 0.098(6) 0.044(4) 0.014(4) 0.030(3) C6 0.094(6) 0.090(5) 0.079(5) 0.024(4) 0.012(4) 0.041(5) C7 0.061(3) 0.044(2) 0.055(3) 0.004(2) -0.015(2) 0.022(2) C8 0.052(3) 0.046(2) 0.040(2) 0.0094(19) -0.0038(19) 0.014(2) C9 0.037(2) 0.047(2) 0.052(3) 0.007(2) -0.0070(19) 0.0119(18) C10 0.048(3) 0.069(4) 0.071(4) 0.023(3) -0.011(3) 0.014(3) C11 0.055(3) 0.060(3) 0.093(5) 0.024(3) 0.020(3) 0.021(3) C12 0.067(4) 0.067(3) 0.051(3) 0.019(3) 0.004(3) 0.023(3) C13 0.118(6) 0.061(4) 0.053(3) 0.014(3) -0.004(4) 0.030(4) C14 0.114(6) 0.071(4) 0.059(4) 0.019(3) 0.002(4) 0.055(4) C15 0.079(4) 0.092(5) 0.050(3) 0.019(3) 0.005(3) 0.057(4) C16 0.058(3) 0.072(3) 0.029(2) 0.011(2) 0.0028(19) 0.038(3) C17 0.046(2) 0.076(3) 0.030(2) 0.015(2) 0.0039(17) 0.033(2) C18 0.050(3) 0.094(5) 0.052(3) 0.018(3) 0.004(2) 0.038(3) C19 0.044(3) 0.128(7) 0.061(4) 0.015(4) 0.003(3) 0.031(4) C20 0.051(3) 0.082(4) 0.068(4) 0.007(3) -0.005(3) 0.007(3) C21 0.056(3) 0.070(4) 0.050(3) 0.007(3) 0.002(2) 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 Zn1 N4 2.105(4) . ? Zn1 N5 2.161(4) . ? Zn1 Cl1 2.3053(12) . ? Zn1 S2 2.3856(15) . ? Zn1 S1 2.5917(15) . ? S1 C1 1.713(5) . ? S2 C1 1.725(5) . ? S3 C11 1.682(8) . ? S3 C8 1.700(6) . ? N3 C1 1.330(6) . ? N3 C2 1.468(6) . ? N3 C7 1.494(7) . ? N4 C21 1.322(8) . ? N4 C17 1.340(7) . ? S4 C6 1.542(10) . ? S4 C3 1.640(7) . ? N5 C12 1.321(8) . ? N5 C16 1.352(7) . ? C2 C3 1.503(9) . ? C2 H2A 0.9700 . ? C2 H2AB 0.9700 . ? C3 C4 1.617(6) . ? C4 C5 1.542(10) . ? C4 H4 0.9300 . ? C5 C6 1.333(13) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.495(7) . ? C7 H7A 0.9700 . ? C7 H7AB 0.9700 . ? C8 C9 1.428(7) . ? C9 C10 1.432(8) . ? C9 H9 0.9300 . ? C10 C11 1.327(11) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.399(10) . ? C12 H12 0.9300 . ? C13 C14 1.380(13) . ? C13 H13 0.9300 . ? C14 C15 1.364(12) . ? C14 H14 0.9300 . ? C15 C16 1.391(8) . ? C15 H15 0.9300 . ? C16 C17 1.486(9) . ? C17 C18 1.394(8) . ? C18 C19 1.358(12) . ? C18 H18 0.9300 . ? C19 C20 1.399(12) . ? C19 H19 0.9300 . ? C20 C21 1.408(9) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? 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 N4 Zn1 N5 76.58(18) . . ? N4 Zn1 Cl1 107.63(12) . . ? N5 Zn1 Cl1 104.45(12) . . ? N4 Zn1 S2 135.62(12) . . ? N5 Zn1 S2 92.96(12) . . ? Cl1 Zn1 S2 116.74(5) . . ? N4 Zn1 S1 95.01(13) . . ? N5 Zn1 S1 149.10(12) . . ? Cl1 Zn1 S1 106.42(5) . . ? S2 Zn1 S1 72.16(4) . . ? C1 S1 Zn1 82.08(16) . . ? C1 S2 Zn1 88.34(17) . . ? C11 S3 C8 92.5(3) . . ? C1 N3 C2 121.8(4) . . ? C1 N3 C7 122.0(4) . . ? C2 N3 C7 115.9(4) . . ? C21 N4 C17 120.0(5) . . ? C21 N4 Zn1 122.9(4) . . ? C17 N4 Zn1 117.2(4) . . ? C6 S4 C3 96.1(5) . . ? C12 N5 C16 119.1(5) . . ? C12 N5 Zn1 125.5(4) . . ? C16 N5 Zn1 115.1(4) . . ? N3 C1 S1 122.3(4) . . ? N3 C1 S2 120.4(4) . . ? S1 C1 S2 117.3(3) . . ? N3 C2 C3 113.6(4) . . ? N3 C2 H2A 108.9 . . ? C3 C2 H2A 108.9 . . ? N3 C2 H2AB 108.9 . . ? C3 C2 H2AB 108.9 . . ? H2A C2 H2AB 107.7 . . ? C2 C3 C4 122.4(4) . . ? C2 C3 S4 124.0(4) . . ? C4 C3 S4 113.5(4) . . ? C5 C4 C3 96.7(4) . . ? C5 C4 H4 131.6 . . ? C3 C4 H4 131.6 . . ? C6 C5 C4 116.7(7) . . ? C6 C5 H5 121.6 . . ? C4 C5 H5 121.6 . . ? C5 C6 S4 116.9(7) . . ? C5 C6 H6 121.5 . . ? S4 C6 H6 121.5 . . ? N3 C7 C8 114.1(4) . . ? N3 C7 H7A 108.7 . . ? C8 C7 H7A 108.7 . . ? N3 C7 H7AB 108.7 . . ? C8 C7 H7AB 108.7 . . ? H7A C7 H7AB 107.6 . . ? C9 C8 C7 125.2(5) . . ? C9 C8 S3 111.9(4) . . ? C7 C8 S3 122.9(4) . . ? C8 C9 C10 107.6(5) . . ? C8 C9 H9 126.2 . . ? C10 C9 H9 126.2 . . ? C11 C10 C9 115.6(6) . . ? C11 C10 H10 122.2 . . ? C9 C10 H10 122.2 . . ? C10 C11 S3 112.2(5) . . ? C10 C11 H11 123.9 . . ? S3 C11 H11 123.9 . . ? N5 C12 C13 122.4(7) . . ? N5 C12 H12 118.8 . . ? C13 C12 H12 118.8 . . ? C14 C13 C12 118.3(7) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C15 C14 C13 119.4(6) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 119.6(7) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? N5 C16 C15 121.1(6) . . ? N5 C16 C17 115.1(5) . . ? C15 C16 C17 123.8(6) . . ? N4 C17 C18 120.9(6) . . ? N4 C17 C16 115.8(5) . . ? C18 C17 C16 123.3(5) . . ? C19 C18 C17 120.1(6) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 119.1(6) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? C19 C20 C21 117.8(7) . . ? C19 C20 H20 121.1 . . ? C21 C20 H20 121.1 . . ? N4 C21 C20 122.1(6) . . ? N4 C21 H21 119.0 . . ? C20 C21 H21 119.0 . . ? _refine_diff_density_max 2.323 _refine_diff_density_min -1.307 _refine_diff_density_rms 0.154 _shelx_res_file ; TITL STE_ZnTHCA_09052019_0m_a.res in P-1 STE_ZnTHCA_09052019_0m_a.res created by SHELXL-2018/3 at 06:40:06 on 18-Jul-2020 REM Old TITL STE_ZnTHCA_09052019_0m in P-1 REM SHELXT solution in P-1 REM R1 0.180, Rweak 0.010, Alpha 0.052, Orientation as input REM Formula found by SHELXT: C20 N5 S4 Zn CELL 0.71073 8.7603 10.7488 13.0262 103.965 91.913 104.944 ZERR 2.000 0.0004 0.0006 0.0007 0.002 0.002 0.002 LATT 1 SFAC C H N S ZN Cl O UNIT 42 36 6 8 2 2 0 ACTA TEMP 28.610 L.S. 10 BOND $H LIST 6 FMAP 2 PLAN 20 WGHT 0.183500 2.028800 FVAR 1.13880 ZN1 5 0.249341 0.327090 0.127116 11.00000 0.04185 0.06079 = 0.03882 0.01327 0.00349 0.02589 CL1 6 0.331936 0.273927 -0.040137 11.00000 0.05372 0.07906 = 0.03029 0.01709 0.01268 0.04125 S1 4 0.284397 0.144921 0.217588 11.00000 0.04714 0.05848 = 0.05206 0.01627 -0.00837 0.01351 S2 4 0.452112 0.430165 0.271862 11.00000 0.06489 0.04907 = 0.04782 0.01415 -0.00560 0.02768 S3 4 0.913437 0.294642 0.363282 11.00000 0.08743 0.07369 = 0.04933 0.01481 0.01324 0.02236 N3 3 0.524626 0.260777 0.371050 11.00000 0.05330 0.04133 = 0.04523 0.01030 -0.00978 0.01874 N4 3 -0.000618 0.264395 0.110762 11.00000 0.03993 0.06398 = 0.03919 0.01000 0.00347 0.02422 S4 4 0.454500 0.205332 0.612520 11.00000 0.12599 0.09815 = 0.10280 0.01834 0.00533 0.01594 N5 3 0.183053 0.509326 0.136053 11.00000 0.05337 0.06130 = 0.03842 0.01347 0.00153 0.02964 C1 1 0.430326 0.275633 0.295358 11.00000 0.04331 0.04919 = 0.03832 0.01233 0.00430 0.02284 C2 1 0.501160 0.133232 0.398979 11.00000 0.05518 0.04236 = 0.04865 0.01056 -0.00913 0.02011 AFIX 23 H2A 2 0.603986 0.123020 0.419046 11.00000 -1.20000 H2AB 2 0.452773 0.061308 0.336694 11.00000 -1.20000 AFIX 0 C3 1 0.398831 0.120802 0.488300 11.00000 0.05462 0.04139 = 0.05697 0.01309 -0.00855 0.01532 C4 1 0.225870 0.014358 0.471230 11.00000 0.01677 0.01832 = 0.03869 0.01585 -0.00895 0.00033 AFIX 43 H4 2 0.166475 -0.045566 0.410516 11.00000 -1.20000 AFIX 0 C5 1 0.191805 0.044885 0.588723 11.00000 0.06446 0.08087 = 0.09769 0.04425 0.01442 0.02981 AFIX 43 H5 2 0.098284 -0.000426 0.610465 11.00000 -1.20000 AFIX 0 C6 1 0.302965 0.139402 0.657603 11.00000 0.09397 0.09033 = 0.07872 0.02368 0.01204 0.04144 AFIX 43 H6 2 0.289726 0.164412 0.729511 11.00000 -1.20000 AFIX 0 C7 1 0.649381 0.375776 0.440028 11.00000 0.06050 0.04364 = 0.05534 0.00409 -0.01462 0.02212 AFIX 23 H7A 2 0.608850 0.405405 0.507352 11.00000 -1.20000 H7AB 2 0.669904 0.448818 0.406288 11.00000 -1.20000 AFIX 0 C8 1 0.802602 0.345186 0.461399 11.00000 0.05169 0.04560 = 0.03983 0.00943 -0.00380 0.01386 C9 1 0.874724 0.355901 0.564285 11.00000 0.03718 0.04693 = 0.05199 0.00728 -0.00699 0.01195 AFIX 43 H9 2 0.833160 0.379622 0.628614 11.00000 -1.20000 AFIX 0 C10 1 1.022658 0.323494 0.550436 11.00000 0.04838 0.06935 = 0.07105 0.02342 -0.01083 0.01368 AFIX 43 H10 2 1.090876 0.326153 0.607668 11.00000 -1.20000 AFIX 0 C11 1 1.056037 0.289425 0.450615 11.00000 0.05513 0.06021 = 0.09252 0.02416 0.02041 0.02065 AFIX 43 H11 2 1.147733 0.265422 0.431176 11.00000 -1.20000 AFIX 0 C12 1 0.282829 0.629121 0.151794 11.00000 0.06743 0.06660 = 0.05140 0.01900 0.00375 0.02269 AFIX 43 H12 2 0.391037 0.636839 0.151795 11.00000 -1.20000 AFIX 0 C13 1 0.231800 0.744816 0.168464 11.00000 0.11782 0.06092 = 0.05326 0.01448 -0.00423 0.02964 AFIX 43 H13 2 0.304490 0.828204 0.180360 11.00000 -1.20000 AFIX 0 C14 1 0.070827 0.732072 0.166808 11.00000 0.11405 0.07108 = 0.05938 0.01915 0.00173 0.05505 AFIX 43 H14 2 0.033176 0.807051 0.176588 11.00000 -1.20000 AFIX 0 C15 1 -0.032540 0.608516 0.150699 11.00000 0.07928 0.09229 = 0.05042 0.01895 0.00531 0.05676 AFIX 43 H15 2 -0.141162 0.598793 0.150560 11.00000 -1.20000 AFIX 0 C16 1 0.025445 0.497167 0.134485 11.00000 0.05833 0.07161 = 0.02918 0.01131 0.00276 0.03807 C17 1 -0.077068 0.358549 0.116155 11.00000 0.04611 0.07587 = 0.03028 0.01452 0.00392 0.03271 C18 1 -0.242423 0.325292 0.103328 11.00000 0.04995 0.09392 = 0.05218 0.01802 0.00431 0.03775 AFIX 43 H18 2 -0.293775 0.391583 0.106259 11.00000 -1.20000 AFIX 0 C19 1 -0.328717 0.196314 0.086561 11.00000 0.04373 0.12788 = 0.06103 0.01531 0.00258 0.03088 AFIX 43 H19 2 -0.439107 0.173858 0.079205 11.00000 -1.20000 AFIX 0 C20 1 -0.249416 0.097649 0.080494 11.00000 0.05114 0.08155 = 0.06791 0.00656 -0.00462 0.00741 AFIX 43 H20 2 -0.305258 0.008339 0.068213 11.00000 -1.20000 REM ##### REM ##### AFIX 0 C21 1 -0.082218 0.138081 0.093605 11.00000 0.05554 0.06973 = 0.05041 0.00750 0.00227 0.02220 AFIX 43 H21 2 -0.027488 0.073887 0.090080 11.00000 -1.20000 REM ##### AFIX 0 HKLF 4 REM STE_ZnTHCA_09052019_0m_a.res in P-1 REM wR2 = 0.278756, GooF = S = 1.08319, Restrained GooF = 1.08319 for all data REM R1 = 0.080979 for 4720 Fo > 4sig(Fo) and 0.089084 for all 5570 data REM 271 parameters refined using 0 restraints END WGHT 0.1835 2.0288 REM Highest difference peak 2.323, deepest hole -1.307, 1-sigma level 0.154 Q1 1 0.8424 0.3520 0.5395 11.00000 0.05 0.45 Q2 1 0.1873 0.0674 0.6385 11.00000 0.05 0.39 Q3 1 1.0395 0.3388 0.4184 11.00000 0.05 0.37 Q4 1 0.7657 0.3300 0.4616 11.00000 0.05 0.36 Q5 1 0.5935 0.2538 0.6396 11.00000 0.05 0.33 Q6 1 0.5778 0.2779 0.6555 11.00000 0.05 0.33 Q7 1 0.4246 0.1635 0.5283 11.00000 0.05 0.29 Q8 1 0.4535 0.1390 0.4598 11.00000 0.05 0.28 Q9 1 0.1528 0.1596 0.1794 11.00000 0.05 0.27 Q10 1 0.5703 0.1448 0.6008 11.00000 0.05 0.27 Q11 1 0.3860 0.2641 0.1203 11.00000 0.05 0.27 Q12 1 1.0568 0.4383 0.4579 11.00000 0.05 0.25 Q13 1 0.5551 0.3008 0.3972 11.00000 0.05 0.25 Q14 1 -0.3071 0.1794 0.0624 11.00000 0.05 0.25 Q15 1 0.8871 0.5522 0.6043 11.00000 0.05 0.24 Q16 1 0.4877 0.2643 0.3604 11.00000 0.05 0.24 Q17 1 0.0164 -0.0631 0.7016 11.00000 0.05 0.24 Q18 1 -0.5916 0.2279 0.0963 11.00000 0.05 0.24 Q19 1 0.9266 0.3829 0.4233 11.00000 0.05 0.23 Q20 1 -0.2627 0.4997 0.0937 11.00000 0.05 0.23 ; _shelx_res_checksum 55195 _shelx_hkl_file ; -1 0 0 6.80 0.70 -1 0 0 7.50 0.70 1 0 0 10.80 0.90 1 0 0 6.50 0.80 -3 0 0 833.92 19.20 3 0 0 874.41 20.10 3 0 0 869.71 19.70 3 0 0 862.21 16.80 3 0 0 846.12 16.70 -5 0 0 496.65 14.40 5 0 0 495.25 10.20 5 0 0 497.45 15.60 6 0 0 930.01 25.50 7 0 0 3.00 3.10 8 0 0 36.30 6.40 9 0 0 78.29 9.10 10 0 0 83.59 9.20 11 0 0 9.10 5.80 10 -1 0 229.18 14.00 9 -1 0 60.79 8.30 8 -1 0 48.60 7.00 -7 1 0 0.80 1.90 6 -1 0 49.50 5.50 6 -1 0 51.09 2.30 -6 1 0 47.80 4.50 5 -1 0 606.54 17.40 5 -1 0 610.14 12.70 -5 1 0 556.24 16.70 -5 1 0 614.74 16.40 4 -1 0 36.50 3.50 4 -1 0 55.29 2.30 -4 1 0 42.20 3.30 -4 1 0 42.90 3.60 3 -1 0 2442.96 46.60 3 -1 0 2465.55 49.50 -3 1 0 2454.35 49.40 -3 1 0 2471.75 48.80 -3 1 0 2432.26 46.80 1 -1 0 473.45 10.10 1 -1 0 463.95 9.70 -1 1 0 476.75 9.80 -3 -1 0 2050.09 41.20 3 1 0 1947.31 41.60 3 1 0 2045.50 41.90 -4 -1 0 2.90 1.60 4 1 0 3.10 2.20 4 1 0 3.80 2.00 4 1 0 6.60 1.40 -5 -1 0 1267.37 29.50 5 1 0 1261.57 25.80 5 1 0 1245.18 30.60 5 1 0 1307.27 31.20 -6 -1 0 180.28 8.40 6 1 0 179.28 5.40 6 1 0 161.88 9.10 6 1 0 170.78 9.50 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0 366.76 8.60 4 2 0 372.36 12.30 4 2 0 347.47 12.30 5 2 0 2781.02 53.09 5 2 0 2821.22 55.09 5 2 0 2711.13 59.49 5 2 0 2799.72 59.79 6 2 0 283.37 6.60 6 2 0 288.27 12.60 6 2 0 287.57 8.70 6 2 0 272.97 12.40 7 2 0 19.70 2.60 7 2 0 18.30 4.80 7 2 0 14.90 2.30 7 2 0 13.70 4.70 8 2 0 108.69 4.60 8 2 0 124.49 10.20 8 2 0 106.49 4.60 9 2 0 122.49 11.00 10 2 0 58.89 8.70 11 -3 0 6.20 4.10 10 -3 0 514.75 21.20 9 -3 0 106.29 9.70 8 -3 0 733.13 23.60 8 -3 0 735.13 16.70 7 -3 0 508.15 17.90 7 -3 0 505.95 12.50 -7 3 0 483.75 15.80 6 -3 0 2350.76 51.39 6 -3 0 2355.46 46.40 -6 3 0 2327.17 49.80 -6 3 0 2265.37 51.59 5 -3 0 1829.62 40.30 5 -3 0 1803.82 36.80 -5 3 0 1799.02 35.10 -5 3 0 1802.42 37.30 -5 3 0 1821.82 40.50 4 -3 0 8.60 2.10 4 -3 0 10.80 1.80 -4 3 0 7.60 2.10 -4 3 0 9.30 1.30 -4 3 0 9.10 1.60 3 -3 0 276.07 7.80 3 -3 0 272.87 8.50 -3 3 0 275.77 7.40 -3 3 0 272.67 8.70 -3 3 0 276.77 8.00 2 -3 0 1307.67 26.70 2 -3 0 1255.87 26.40 -2 3 0 1293.57 27.00 -2 3 0 1313.87 26.90 -2 3 0 1277.07 26.40 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1125.29 26.30 8 -5 0 1152.28 31.40 -8 5 0 1142.79 32.00 -8 5 0 1105.29 27.20 7 -5 0 1479.35 37.50 7 -5 0 1376.36 35.40 -7 5 0 1365.36 32.00 -7 5 0 1370.16 28.60 6 -5 0 320.37 12.10 6 -5 0 313.27 10.40 -6 5 0 282.37 10.40 -6 5 0 307.67 9.20 -6 5 0 302.37 12.30 5 -5 0 748.83 20.00 5 -5 0 754.82 18.90 -5 5 0 737.13 19.20 -5 5 0 768.92 18.20 -5 5 0 760.12 21.00 4 -5 0 1018.60 23.60 4 -5 0 1022.50 23.80 -4 5 0 1002.90 24.90 -4 5 0 972.70 22.60 -4 5 0 1026.00 24.10 -4 5 0 1012.60 23.10 3 -5 0 1114.39 24.70 3 -5 0 1134.29 25.50 -3 5 0 1087.89 25.60 -3 5 0 1084.29 23.90 -3 5 0 1092.39 25.70 -3 5 0 1151.88 25.40 2 -5 0 401.26 11.80 -2 5 0 409.56 11.90 -2 5 0 399.26 11.20 -2 5 0 398.06 11.70 -2 5 0 390.66 10.30 1 -5 0 1739.33 36.50 1 -5 0 1803.12 37.90 -1 5 0 1793.22 38.20 -1 5 0 1779.72 36.40 -1 5 0 1782.52 37.80 0 -5 0 3132.59 61.39 0 -5 0 3103.99 62.49 0 5 0 3147.89 62.39 0 5 0 3145.49 61.59 0 5 0 3034.70 62.89 -1 -5 0 461.95 12.50 1 5 0 441.36 12.50 1 5 0 458.05 13.50 1 5 0 456.15 12.90 -2 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2249.47 44.60 3 -2 3 2244.18 43.80 -4 2 -3 143.59 5.20 -4 2 -3 125.59 4.00 -4 2 -3 136.89 5.20 4 -2 3 129.79 6.40 4 -2 3 128.59 5.10 4 -2 3 133.39 5.50 -5 2 -3 2007.00 41.50 -5 2 -3 2059.89 40.50 -5 2 -3 1982.80 38.30 5 -2 3 1973.00 40.10 5 -2 3 1974.10 44.10 -6 2 -3 83.29 5.20 6 -2 3 87.79 6.90 6 -2 3 84.69 3.90 -7 2 -3 329.17 11.50 7 -2 3 324.97 8.30 7 -2 3 325.27 14.10 8 -2 3 53.69 7.40 9 -2 3 398.46 18.00 10 -2 3 3.30 4.90 11 -2 3 75.89 9.90 11 1 -3 -1.60 4.40 10 1 -3 55.89 8.60 9 1 -3 3.00 1.80 9 1 -3 2.40 4.10 8 1 -3 323.27 9.90 8 1 -3 309.87 14.80 7 1 -3 803.02 24.40 7 1 -3 824.12 19.70 6 1 -3 305.07 12.30 6 1 -3 275.87 7.70 5 1 -3 1421.26 33.30 5 1 -3 1409.06 29.30 -5 -1 3 1441.06 33.40 -5 -1 3 1431.16 33.10 4 1 -3 1237.18 28.80 4 1 -3 1224.98 26.30 -4 -1 3 1295.27 28.80 -4 -1 3 1271.67 29.20 -4 -1 3 1280.27 25.90 3 1 -3 130.89 4.90 3 1 -3 132.69 5.60 -3 -1 3 139.39 6.00 -3 -1 3 135.99 4.70 2 1 -3 53.79 3.00 2 1 -3 56.19 2.90 -2 -1 3 49.90 2.70 -2 -1 3 54.89 2.90 1 1 -3 1993.30 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4 -8 28.00 4.70 8 -4 8 35.80 6.40 8 -4 8 15.30 3.60 9 -4 8 20.30 5.40 10 -4 8 101.39 10.10 9 3 -8 21.80 3.50 9 3 -8 16.40 4.90 9 3 -8 13.00 4.30 8 3 -8 182.98 8.80 8 3 -8 183.18 11.00 7 3 -8 207.98 11.10 7 3 -8 196.48 9.70 -7 -3 8 203.98 8.80 6 3 -8 378.66 14.00 6 3 -8 372.56 13.90 -6 -3 8 387.76 14.10 -6 -3 8 379.56 12.80 5 3 -8 14.40 3.20 5 3 -8 14.30 3.70 -5 -3 8 16.90 3.30 -5 -3 8 18.90 3.50 4 3 -8 236.38 10.90 4 3 -8 235.88 8.80 -4 -3 8 221.18 10.30 -4 -3 8 220.78 8.80 -4 -3 8 228.18 9.70 3 3 -8 153.48 8.70 3 3 -8 154.88 6.20 -3 -3 8 151.78 6.40 -3 -3 8 146.19 7.80 2 3 -8 126.59 8.00 -2 -3 8 140.49 5.60 -2 -3 8 131.19 7.20 1 3 -8 122.19 7.90 -1 -3 8 130.19 7.20 -1 -3 8 140.99 5.10 0 3 -8 1964.50 45.50 0 -3 8 2008.90 44.90 0 -3 8 1985.00 40.60 0 -3 8 2032.00 39.70 -1 3 -8 20.90 3.90 1 -3 8 25.90 2.40 1 -3 8 26.00 4.30 -2 3 -8 956.10 25.50 2 -3 8 942.01 24.90 2 -3 8 900.01 19.80 -3 3 -8 862.61 23.90 -3 3 -8 861.81 18.90 3 -3 8 831.52 18.60 3 -3 8 858.51 23.50 -4 3 -8 492.15 16.40 -4 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2 -17 21.60 7.20 1 2 -17 31.90 8.10 -1 -2 17 36.40 5.80 0 2 -17 89.79 17.50 0 2 -17 134.49 13.00 0 -2 17 122.29 8.80 -1 2 -17 -5.50 4.40 -1 2 -17 5.70 4.80 1 -2 17 -0.90 3.10 2 1 -17 17.20 6.50 -2 -1 17 14.00 4.60 1 1 -17 59.19 9.00 1 1 -17 49.00 9.40 -1 -1 17 65.19 7.40 0 1 -17 69.69 14.30 0 1 -17 61.99 9.70 0 -1 17 80.49 8.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 32414