Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'ProfD Manuel R. Bermejo' _publ_contact_author_address ; Departamento de Química Inorgánica Universidade de Santiago de Compostela Facultade de Química, Avda. das Cie Santiago de Compostela 15782 SPAIN ; _publ_contact_author_email QIMB45@USC.ES _publ_section_title ; Syntheses and X-ray characterisation of metal complexes with the pentadentate thiosemicarbazone ligand bis(4-N-methylthiosemicarbazone)-2,6-diacetylpyridine. The first pentacoordinate lead(II) complex with a pentagonal pyramidal geometry ; loop_ _publ_author_name 'Manuel R. Bermejo' 'M Isabel Fernandez' 'Ana M. Gonzalez-Noya' 'Marcelino Maneiro' ; R.Pedrido ; 'M. Jesus Rodriguez' 'M. Jose Romero' 'Miguel Vazquez' data_ropb _database_code_depnum_ccdc_archive 'CCDC 220760' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H17 N7 Pb S2' _chemical_formula_weight 542.65 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' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.267(2) _cell_length_b 22.017(5) _cell_length_c 7.4514(17) _cell_angle_alpha 90.00 _cell_angle_beta 92.432(4) _cell_angle_gamma 90.00 _cell_volume 1682.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 883 _cell_measurement_theta_min 2.89 _cell_measurement_theta_max 26.34 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.142 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 10.283 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.482516 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart-CCD-1000 BRUKER' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'not significant' _diffrn_reflns_number 9344 _diffrn_reflns_av_R_equivalents 0.0663 _diffrn_reflns_av_sigmaI/netI 0.0916 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 26.39 _reflns_number_total 3434 _reflns_number_gt 2157 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0321P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3434 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0817 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.0884 _refine_ls_wR_factor_gt 0.0752 _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_restrained_S_all 0.930 _refine_ls_shift/su_max 0.001 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb Pb 0.39307(3) 0.398040(16) 0.98293(4) 0.03210(12) Uani 1 1 d . . . S1 S 0.1606(2) 0.43579(12) 1.1170(3) 0.0425(6) Uani 1 1 d . . . S2 S 0.4593(2) 0.47968(12) 1.2571(3) 0.0400(6) Uani 1 1 d . . . N3 N 0.2029(7) 0.3170(3) 0.9674(9) 0.0353(18) Uani 1 1 d . . . N4 N 0.4439(7) 0.2834(3) 1.0632(10) 0.0343(18) Uani 1 1 d . . . N5 N 0.6086(7) 0.3715(4) 1.1686(10) 0.0352(19) Uani 1 1 d . . . C1 C -0.1532(9) 0.3884(5) 0.8041(14) 0.052(3) Uani 1 1 d . . . H1A H -0.1204 0.3872 0.6854 0.078 Uiso 1 1 calc R . . H1B H -0.2332 0.4110 0.8021 0.078 Uiso 1 1 calc R . . H1C H -0.1689 0.3477 0.8444 0.078 Uiso 1 1 calc R . . N1 N -0.0591(7) 0.4172(3) 0.9245(10) 0.041(2) Uani 1 1 d . . . H1 H -0.0781 0.4524 0.9661 0.049 Uiso 1 1 calc R . . C2 C 0.0553(8) 0.3931(4) 0.9759(12) 0.036(2) Uani 1 1 d . . . N2 N 0.0787(7) 0.3370(3) 0.9176(10) 0.0366(19) Uani 1 1 d . . . C3 C 0.2210(8) 0.2588(4) 0.9678(11) 0.032(2) Uani 1 1 d . . . C30 C 0.1162(9) 0.2132(4) 0.9302(14) 0.047(3) Uani 1 1 d . . . H30A H 0.0937 0.1941 1.0404 0.071 Uiso 1 1 calc R . . H30B H 0.1465 0.1831 0.8487 0.071 Uiso 1 1 calc R . . H30C H 0.0407 0.2331 0.8772 0.071 Uiso 1 1 calc R . . C4 C 0.3559(8) 0.2401(4) 1.0141(11) 0.032(2) Uani 1 1 d . . . C5 C 0.3924(9) 0.1787(4) 1.0126(12) 0.039(2) Uani 1 1 d . . . H5 H 0.3317 0.1489 0.9796 0.047 Uiso 1 1 calc R . . C6 C 0.5183(10) 0.1629(4) 1.0601(13) 0.045(3) Uani 1 1 d . . . H6 H 0.5444 0.1225 1.0599 0.054 Uiso 1 1 calc R . . C7 C 0.6064(10) 0.2086(5) 1.1085(12) 0.042(3) Uani 1 1 d . . . H7 H 0.6921 0.1987 1.1420 0.050 Uiso 1 1 calc R . . C8 C 0.5669(9) 0.2692(4) 1.1072(11) 0.035(2) Uani 1 1 d . . . C9 C 0.6562(9) 0.3173(5) 1.1615(11) 0.036(2) Uani 1 1 d . . . C90 C 0.7957(9) 0.3030(5) 1.2197(13) 0.051(3) Uani 1 1 d . . . H90A H 0.8489 0.3032 1.1167 0.077 Uiso 1 1 calc R . . H90B H 0.7997 0.2636 1.2752 0.077 Uiso 1 1 calc R . . H90C H 0.8273 0.3331 1.3041 0.077 Uiso 1 1 calc R . . N6 N 0.6898(7) 0.4159(4) 1.2334(10) 0.038(2) Uani 1 1 d . . . C10 C 0.6273(8) 0.4652(5) 1.2778(12) 0.036(2) Uani 1 1 d . . . N7 N 0.7017(7) 0.5118(4) 1.3465(10) 0.044(2) Uani 1 1 d . . . H7A H 0.6650 0.5461 1.3666 0.053 Uiso 1 1 calc R . . C11 C 0.8400(9) 0.5055(5) 1.3864(14) 0.052(3) Uani 1 1 d . . . H11A H 0.8614 0.4632 1.4002 0.078 Uiso 1 1 calc R . . H11B H 0.8631 0.5267 1.4957 0.078 Uiso 1 1 calc R . . H11C H 0.8874 0.5223 1.2899 0.078 Uiso 1 1 calc R . . 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 Pb 0.03441(18) 0.02746(19) 0.0343(2) 0.0015(2) -0.00064(13) 0.0020(2) S1 0.0369(13) 0.0340(15) 0.0562(16) -0.0142(13) -0.0039(12) 0.0036(12) S2 0.0327(12) 0.0415(16) 0.0456(15) -0.0084(12) -0.0002(11) 0.0041(12) N3 0.039(4) 0.026(5) 0.040(5) -0.006(4) -0.001(4) 0.001(4) N4 0.035(4) 0.025(4) 0.043(5) 0.003(4) 0.003(4) 0.005(4) N5 0.032(4) 0.028(5) 0.045(5) 0.002(4) 0.000(4) 0.003(4) C1 0.044(6) 0.041(7) 0.067(7) 0.008(6) -0.024(5) -0.004(5) N1 0.032(4) 0.021(4) 0.069(6) -0.008(4) -0.004(4) 0.006(3) C2 0.037(5) 0.028(6) 0.043(5) -0.002(5) 0.011(4) -0.001(5) N2 0.035(4) 0.022(4) 0.053(5) -0.006(4) 0.000(4) 0.003(4) C3 0.038(5) 0.024(5) 0.033(5) -0.004(4) 0.002(4) 0.000(4) C30 0.037(5) 0.033(6) 0.071(7) -0.008(5) -0.003(5) 0.001(5) C4 0.038(5) 0.028(5) 0.029(5) 0.004(4) 0.009(4) -0.002(4) C5 0.047(6) 0.026(5) 0.046(6) -0.003(5) 0.008(5) -0.001(5) C6 0.056(6) 0.016(5) 0.063(7) 0.002(5) 0.005(5) 0.007(5) C7 0.045(6) 0.043(7) 0.039(6) -0.008(5) 0.001(5) 0.012(5) C8 0.045(6) 0.026(6) 0.033(5) 0.001(4) 0.000(4) 0.005(5) C9 0.040(5) 0.040(6) 0.028(5) -0.005(4) 0.003(4) 0.002(5) C90 0.045(6) 0.049(7) 0.058(7) 0.011(6) -0.011(5) 0.002(6) N6 0.034(4) 0.035(5) 0.047(5) 0.005(4) 0.002(4) 0.003(4) C10 0.031(5) 0.041(6) 0.036(5) 0.005(5) 0.000(4) -0.007(5) N7 0.041(5) 0.041(5) 0.051(5) -0.007(4) -0.002(4) -0.008(4) C11 0.042(6) 0.047(7) 0.066(7) 0.002(6) -0.007(5) -0.009(5) _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 Pb N5 2.625(7) . ? Pb N4 2.641(7) . ? Pb N3 2.644(7) . ? Pb S1 2.755(2) . ? Pb S2 2.784(2) . ? S1 C2 1.749(9) . ? S2 C10 1.754(9) . ? N3 C3 1.293(11) . ? N3 N2 1.385(9) . ? N4 C8 1.329(11) . ? N4 C4 1.354(11) . ? N5 C9 1.292(11) . ? N5 N6 1.360(10) . ? C1 N1 1.438(10) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? N1 C2 1.330(11) . ? N1 H1 0.8600 . ? C2 N2 1.336(11) . ? C3 C4 1.472(11) . ? C3 C30 1.490(12) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C4 C5 1.402(12) . ? C5 C6 1.371(12) . ? C5 H5 0.9300 . ? C6 C7 1.390(13) . ? C6 H6 0.9300 . ? C7 C8 1.395(13) . ? C7 H7 0.9300 . ? C8 C9 1.446(12) . ? C9 C90 1.512(12) . ? C90 H90A 0.9600 . ? C90 H90B 0.9600 . ? C90 H90C 0.9600 . ? N6 C10 1.310(11) . ? C10 N7 1.366(11) . ? N7 C11 1.445(10) . ? N7 H7A 0.8600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 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 N5 Pb N4 60.9(2) . . ? N5 Pb N3 118.5(2) . . ? N4 Pb N3 60.2(2) . . ? N5 Pb S1 126.87(17) . . ? N4 Pb S1 111.84(16) . . ? N3 Pb S1 64.54(17) . . ? N5 Pb S2 65.35(18) . . ? N4 Pb S2 114.27(17) . . ? N3 Pb S2 128.67(16) . . ? S1 Pb S2 74.19(7) . . ? C2 S1 Pb 98.2(3) . . ? C10 S2 Pb 98.9(3) . . ? C3 N3 N2 116.5(8) . . ? C3 N3 Pb 124.2(6) . . ? N2 N3 Pb 117.8(5) . . ? C8 N4 C4 121.1(8) . . ? C8 N4 Pb 117.2(6) . . ? C4 N4 Pb 119.3(5) . . ? C9 N5 N6 116.8(7) . . ? C9 N5 Pb 119.8(6) . . ? N6 N5 Pb 121.1(5) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 N1 C1 124.5(8) . . ? C2 N1 H1 117.8 . . ? C1 N1 H1 117.8 . . ? N1 C2 N2 116.3(8) . . ? N1 C2 S1 118.3(7) . . ? N2 C2 S1 125.3(7) . . ? C2 N2 N3 112.5(7) . . ? N3 C3 C4 114.3(8) . . ? N3 C3 C30 124.3(8) . . ? C4 C3 C30 121.3(8) . . ? C3 C30 H30A 109.5 . . ? C3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N4 C4 C5 120.4(8) . . ? N4 C4 C3 118.4(8) . . ? C5 C4 C3 121.2(9) . . ? C6 C5 C4 119.4(9) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C5 C6 C7 118.7(9) . . ? C5 C6 H6 120.6 . . ? C7 C6 H6 120.6 . . ? C6 C7 C8 120.3(9) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? N4 C8 C7 120.0(9) . . ? N4 C8 C9 118.8(8) . . ? C7 C8 C9 121.1(8) . . ? N5 C9 C8 116.8(8) . . ? N5 C9 C90 122.4(9) . . ? C8 C9 C90 120.6(9) . . ? C9 C90 H90A 109.5 . . ? C9 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C9 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? C10 N6 N5 112.7(7) . . ? N6 C10 N7 116.4(8) . . ? N6 C10 S2 128.3(7) . . ? N7 C10 S2 115.4(8) . . ? C10 N7 C11 122.3(9) . . ? C10 N7 H7A 118.9 . . ? C11 N7 H7A 118.9 . . ? N7 C11 H11A 109.5 . . ? N7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 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 N5 Pb S1 C2 -138.9(4) . . . . ? N4 Pb S1 C2 -69.7(4) . . . . ? N3 Pb S1 C2 -31.3(4) . . . . ? S2 Pb S1 C2 -179.9(3) . . . . ? N5 Pb S2 C10 23.1(4) . . . . ? N4 Pb S2 C10 60.6(4) . . . . ? N3 Pb S2 C10 130.9(4) . . . . ? S1 Pb S2 C10 167.9(3) . . . . ? N5 Pb N3 C3 -33.3(8) . . . . ? N4 Pb N3 C3 -14.8(6) . . . . ? S1 Pb N3 C3 -153.2(7) . . . . ? S2 Pb N3 C3 -113.3(7) . . . . ? N5 Pb N3 N2 161.1(5) . . . . ? N4 Pb N3 N2 179.6(6) . . . . ? S1 Pb N3 N2 41.2(5) . . . . ? S2 Pb N3 N2 81.1(6) . . . . ? N5 Pb N4 C8 -19.8(6) . . . . ? N3 Pb N4 C8 178.9(7) . . . . ? S1 Pb N4 C8 -140.9(6) . . . . ? S2 Pb N4 C8 -59.0(6) . . . . ? N5 Pb N4 C4 177.3(7) . . . . ? N3 Pb N4 C4 16.0(6) . . . . ? S1 Pb N4 C4 56.2(6) . . . . ? S2 Pb N4 C4 138.1(6) . . . . ? N4 Pb N5 C9 21.9(6) . . . . ? N3 Pb N5 C9 40.3(7) . . . . ? S1 Pb N5 C9 118.5(6) . . . . ? S2 Pb N5 C9 162.5(7) . . . . ? N4 Pb N5 N6 -175.8(7) . . . . ? N3 Pb N5 N6 -157.4(6) . . . . ? S1 Pb N5 N6 -79.2(6) . . . . ? S2 Pb N5 N6 -35.1(6) . . . . ? C1 N1 C2 N2 -3.8(14) . . . . ? C1 N1 C2 S1 177.7(7) . . . . ? Pb S1 C2 N1 -145.3(7) . . . . ? Pb S1 C2 N2 36.4(8) . . . . ? N1 C2 N2 N3 176.0(7) . . . . ? S1 C2 N2 N3 -5.6(11) . . . . ? C3 N3 N2 C2 159.1(8) . . . . ? Pb N3 N2 C2 -34.2(9) . . . . ? N2 N3 C3 C4 177.5(7) . . . . ? Pb N3 C3 C4 11.8(10) . . . . ? N2 N3 C3 C30 -4.1(13) . . . . ? Pb N3 C3 C30 -169.9(6) . . . . ? C8 N4 C4 C5 1.4(13) . . . . ? Pb N4 C4 C5 163.6(6) . . . . ? C8 N4 C4 C3 179.8(7) . . . . ? Pb N4 C4 C3 -18.1(10) . . . . ? N3 C3 C4 N4 4.5(11) . . . . ? C30 C3 C4 N4 -173.9(8) . . . . ? N3 C3 C4 C5 -177.2(8) . . . . ? C30 C3 C4 C5 4.4(13) . . . . ? N4 C4 C5 C6 -0.4(13) . . . . ? C3 C4 C5 C6 -178.7(8) . . . . ? C4 C5 C6 C7 0.0(14) . . . . ? C5 C6 C7 C8 -0.5(14) . . . . ? C4 N4 C8 C7 -1.9(13) . . . . ? Pb N4 C8 C7 -164.5(7) . . . . ? C4 N4 C8 C9 -179.0(8) . . . . ? Pb N4 C8 C9 18.5(10) . . . . ? C6 C7 C8 N4 1.5(14) . . . . ? C6 C7 C8 C9 178.4(8) . . . . ? N6 N5 C9 C8 174.9(7) . . . . ? Pb N5 C9 C8 -22.0(10) . . . . ? N6 N5 C9 C90 -0.7(13) . . . . ? Pb N5 C9 C90 162.4(6) . . . . ? N4 C8 C9 N5 1.9(12) . . . . ? C7 C8 C9 N5 -175.1(9) . . . . ? N4 C8 C9 C90 177.6(8) . . . . ? C7 C8 C9 C90 0.6(13) . . . . ? C9 N5 N6 C10 -164.1(8) . . . . ? Pb N5 N6 C10 33.1(9) . . . . ? N5 N6 C10 N7 179.2(7) . . . . ? N5 N6 C10 S2 -1.9(12) . . . . ? Pb S2 C10 N6 -23.9(9) . . . . ? Pb S2 C10 N7 155.0(6) . . . . ? N6 C10 N7 C11 -6.4(13) . . . . ? S2 C10 N7 C11 174.6(7) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.294 _refine_diff_density_min -1.561 _refine_diff_density_rms 0.219 data_zndapt _database_code_depnum_ccdc_archive 'CCDC 240031' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H44 N14 O3 S4 Zn2' _chemical_formula_weight 883.76 _chemical_melting_point ? _chemical_compound_source ? 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.008(4) _cell_length_b 11.763(4) _cell_length_c 15.946(6) _cell_angle_alpha 92.21(3) _cell_angle_beta 107.08(3) _cell_angle_gamma 90.75(4) _cell_volume 1971.6(11) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Blocklike _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method ? _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 1.478 _exptl_absorpt_correction_type Sadabs _exptl_absorpt_correction_T_min 0.699924 _exptl_absorpt_correction_T_max 0.963581 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens CCD' _diffrn_measurement_method 'omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8315 _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_sigmaI/netI 0.1644 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 25.05 _reflns_number_total 6793 _reflns_number_observed 3359 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w==1/[\s^2^(Fo^2^)+(0.0715P)^2^+9.7371P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding mode' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6793 _refine_ls_number_parameters 469 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1912 _refine_ls_R_factor_obs 0.0874 _refine_ls_wR_factor_all 0.2329 _refine_ls_wR_factor_obs 0.1720 _refine_ls_goodness_of_fit_all 1.047 _refine_ls_goodness_of_fit_obs 1.128 _refine_ls_restrained_S_all 1.048 _refine_ls_restrained_S_obs 1.130 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zn1 Zn 0.10567(12) 0.63969(11) 0.27451(8) 0.0402(4) Uani 1 d . . Zn2 Zn -0.13271(12) 0.88680(11) 0.26348(8) 0.0413(4) Uani 1 d . . S3 S 0.0922(3) 0.5296(3) 0.1432(2) 0.0460(8) Uani 1 d . . S1 S -0.2966(3) 0.8574(3) 0.3240(2) 0.0497(8) Uani 1 d . . S4 S -0.1432(3) 1.0535(3) 0.1860(2) 0.0528(8) Uani 1 d . . S2 S 0.2492(3) 0.5576(3) 0.3997(2) 0.0555(9) Uani 1 d . . N3 N -0.2184(8) 0.7562(7) 0.1752(5) 0.038(2) Uani 1 d . . N10 N -0.0606(8) 0.5507(7) 0.2682(6) 0.038(2) Uani 1 d . . N9 N -0.1141(9) 0.4721(7) 0.2004(6) 0.042(2) Uani 1 d . . N2 N -0.3306(8) 0.7067(8) 0.1817(6) 0.044(2) Uani 1 d . . N5 N 0.2475(8) 0.7642(7) 0.3002(6) 0.036(2) Uani 1 d . . N14 N 0.0513(9) 1.1961(8) 0.2198(6) 0.056(3) Uani 1 d . . H14N H 0.0024(9) 1.2282(8) 0.1753(6) 0.067 Uiso 1 calc R . N13 N 0.0876(8) 1.0549(7) 0.3157(6) 0.040(2) Uani 1 d . . N12 N 0.0395(8) 0.9559(7) 0.3412(6) 0.036(2) Uani 1 d . . C15 C -0.0498(11) 0.4603(9) 0.1423(8) 0.045(3) Uani 1 d . . N11 N -0.0018(8) 0.7345(7) 0.3795(5) 0.032(2) Uani 1 d . . N4 N 0.0266(9) 0.7948(7) 0.1716(6) 0.038(2) Uani 1 d . . N8 N -0.1030(10) 0.3868(8) 0.0726(6) 0.057(3) Uani 1 d . . H8N H -0.0596(10) 0.3688(8) 0.0374(6) 0.068 Uiso 1 calc R . N1 N -0.4730(8) 0.6991(9) 0.2571(6) 0.054(3) Uani 1 d . . H1N H -0.4980(8) 0.7215(9) 0.3012(6) 0.065 Uiso 1 calc R . C10 C 0.2449(10) 0.8483(9) 0.2494(7) 0.039(3) Uani 1 d . . C25 C 0.0079(10) 1.1014(9) 0.2456(7) 0.040(3) Uani 1 d . . C2 C -0.3659(10) 0.7480(9) 0.2484(7) 0.040(3) Uani 1 d . . C9 C 0.1369(11) 0.8478(9) 0.1702(8) 0.042(3) Uani 1 d . . C11 C 0.3468(11) 0.9395(10) 0.2676(9) 0.061(4) Uani 1 d . . H11A H 0.4100(11) 0.9264(10) 0.3222(9) 0.091 Uiso 1 calc R . H11B H 0.3101(11) 1.0124(10) 0.2713(9) 0.091 Uiso 1 calc R . H11C H 0.3857(11) 0.9380(10) 0.2210(9) 0.091 Uiso 1 calc R . N6 N 0.3565(8) 0.7594(8) 0.3712(6) 0.046(2) Uani 1 d . . C5 C -0.0686(10) 0.7811(9) 0.0981(7) 0.034(3) Uani 1 d . . C23 C 0.1039(10) 0.9196(9) 0.4165(7) 0.038(3) Uani 1 d . . C18 C -0.0624(10) 0.6456(9) 0.4010(7) 0.037(3) Uani 1 d . . C3 C -0.1859(10) 0.7304(9) 0.1042(7) 0.037(3) Uani 1 d . . C12 C 0.3600(11) 0.6655(11) 0.4188(7) 0.051(3) Uani 1 d . . C22 C 0.0517(10) 0.8165(9) 0.4430(7) 0.036(3) Uani 1 d . . C17 C -0.2279(10) 0.4865(10) 0.3307(8) 0.050(3) Uani 1 d . . H17A H -0.2509(10) 0.4348(10) 0.2801(8) 0.075 Uiso 1 calc R . H17B H -0.2981(10) 0.5343(10) 0.3299(8) 0.075 Uiso 1 calc R . H17C H -0.2065(10) 0.4440(10) 0.3830(8) 0.075 Uiso 1 calc R . C21 C 0.0493(12) 0.8052(11) 0.5296(8) 0.054(3) Uani 1 d . . H21A H 0.0898(12) 0.8597(11) 0.5730(8) 0.065 Uiso 1 calc R . C6 C -0.0591(12) 0.8192(10) 0.0189(7) 0.053(3) Uani 1 d . . H6A H -0.1253(12) 0.8061(10) -0.0325(7) 0.064 Uiso 1 calc R . C16 C -0.1165(10) 0.5581(9) 0.3290(7) 0.037(3) Uani 1 d . . C7 C 0.0496(14) 0.8767(11) 0.0178(8) 0.059(4) Uani 1 d . . H7A H 0.0571(14) 0.9044(11) -0.0344(8) 0.071 Uiso 1 calc R . C4 C -0.2674(11) 0.6536(11) 0.0318(8) 0.059(4) Uani 1 d . . H4A H -0.3408(11) 0.6283(11) 0.0474(8) 0.089 Uiso 1 calc R . H4B H -0.2197(11) 0.5890(11) 0.0228(8) 0.089 Uiso 1 calc R . H4C H -0.2941(11) 0.6943(11) -0.0213(8) 0.089 Uiso 1 calc R . C20 C -0.0120(13) 0.7148(11) 0.5499(8) 0.061(4) Uani 1 d . . H20A H -0.0142(13) 0.7068(11) 0.6073(8) 0.073 Uiso 1 calc R . C26 C 0.1754(12) 1.2490(12) 0.2617(9) 0.072(4) Uani 1 d . . H26A H 0.1852(12) 1.3160(12) 0.2316(9) 0.108 Uiso 1 calc R . H26B H 0.2404(12) 1.1964(12) 0.2592(9) 0.108 Uiso 1 calc R . H26C H 0.1828(12) 1.2694(12) 0.3218(9) 0.108 Uiso 1 calc R . C1 C -0.5493(12) 0.6108(13) 0.1967(9) 0.084(5) Uani 1 d . . H1A H -0.6206(12) 0.5892(13) 0.2163(9) 0.127 Uiso 1 calc R . H1B H -0.4981(12) 0.5456(13) 0.1954(9) 0.127 Uiso 1 calc R . H1C H -0.5792(12) 0.6395(13) 0.1389(9) 0.127 Uiso 1 calc R . C14 C -0.2304(12) 0.3376(11) 0.0552(8) 0.066(4) Uani 1 d . . H14A H -0.2495(12) 0.2885(11) 0.0032(8) 0.099 Uiso 1 calc R . H14B H -0.2908(12) 0.3974(11) 0.0466(8) 0.099 Uiso 1 calc R . H14C H -0.2348(12) 0.2945(11) 0.1041(8) 0.099 Uiso 1 calc R . C13 C 0.5723(14) 0.7452(17) 0.5089(10) 0.124(8) Uani 1 d . . H13A H 0.6378(14) 0.7222(17) 0.5594(10) 0.186 Uiso 1 calc R . H13B H 0.5412(14) 0.8176(17) 0.5219(10) 0.186 Uiso 1 calc R . H13C H 0.6063(14) 0.7514(17) 0.4603(10) 0.186 Uiso 1 calc R . N7 N 0.4659(10) 0.6589(11) 0.4859(7) 0.084(4) Uani 1 d . . H7N H 0.4733(10) 0.6009(11) 0.5180(7) 0.101 Uiso 1 calc R . C8 C 0.1469(12) 0.8929(10) 0.0939(8) 0.053(3) Uani 1 d . . H8A H 0.2196(12) 0.9342(10) 0.0942(8) 0.063 Uiso 1 calc R . C24 C 0.2190(11) 0.9772(10) 0.4732(7) 0.056(3) Uani 1 d . . H24A H 0.2384(11) 1.0427(10) 0.4450(7) 0.084 Uiso 1 calc R . H24B H 0.2885(11) 0.9260(10) 0.4838(7) 0.084 Uiso 1 calc R . H24C H 0.2055(11) 1.0007(10) 0.5280(7) 0.084 Uiso 1 calc R . C19 C -0.0713(13) 0.6346(11) 0.4852(8) 0.058(4) Uani 1 d . . H19A H -0.1167(13) 0.5737(11) 0.4978(8) 0.070 Uiso 1 calc R . O1S O 0.4026(10) 0.7856(10) 0.6560(7) 0.097(4) Uani 1 d D . H1SA H 0.4686(10) 0.7999(10) 0.6441(7) 0.146 Uiso 1 calc R 1 O3S O 0.4999(16) 1.0896(12) 0.9487(10) 0.162(6) Uani 1 d . . O2S O 0.5976(29) 0.9643(27) 0.9753(23) 0.425(27) Uani 1 d . . C1S C 0.4210(28) 0.8146(23) 0.7517(15) 0.199(22) Uani 0.75(3) d PD 1 H1SB H 0.4355(28) 0.8965(23) 0.7574(15) 0.239 Uiso 0.75(3) calc PR 1 H1SC H 0.3375(28) 0.8020(23) 0.7591(15) 0.239 Uiso 0.75(3) calc PR 1 C2S C 0.5102(23) 0.7719(27) 0.8327(11) 0.127(14) Uani 0.75(3) d PD 1 H2SA H 0.4948(23) 0.8088(27) 0.8833(11) 0.191 Uiso 0.75(3) calc PR 1 H2SB H 0.5961(23) 0.7880(27) 0.8331(11) 0.191 Uiso 0.75(3) calc PR 1 H2SC H 0.4974(23) 0.6912(27) 0.8342(11) 0.191 Uiso 0.75(3) calc PR 1 C1S' C 0.4819(60) 0.7032(46) 0.7112(27) 0.103(28) Uiso 0.25(3) d PD 2 H1SD H 0.5611(60) 0.7016(46) 0.6962(27) 0.124 Uiso 0.25(3) calc PR 2 H1SE H 0.4404(60) 0.6292(46) 0.6931(27) 0.124 Uiso 0.25(3) calc PR 2 C2S' C 0.5168(42) 0.7122(38) 0.8102(25) 0.024(11) Uiso 0.25(3) d PD 2 H2SD H 0.5684(42) 0.6493(38) 0.8342(25) 0.037 Uiso 0.25(3) calc PR 2 H2SE H 0.4408(42) 0.7108(38) 0.8281(25) 0.037 Uiso 0.25(3) calc PR 2 H2SF H 0.5635(42) 0.7822(38) 0.8313(25) 0.037 Uiso 0.25(3) calc PR 2 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 0.0389(8) 0.0449(8) 0.0386(8) 0.0056(6) 0.0140(6) -0.0077(6) Zn2 0.0412(8) 0.0463(9) 0.0359(8) 0.0002(6) 0.0109(6) -0.0077(6) S3 0.051(2) 0.045(2) 0.045(2) -0.0016(14) 0.0192(15) -0.0001(15) S1 0.044(2) 0.058(2) 0.051(2) -0.006(2) 0.0227(15) -0.008(2) S4 0.047(2) 0.052(2) 0.055(2) 0.018(2) 0.006(2) -0.004(2) S2 0.052(2) 0.058(2) 0.053(2) 0.021(2) 0.009(2) -0.005(2) N3 0.039(6) 0.041(6) 0.036(5) 0.006(4) 0.014(4) 0.008(4) N10 0.042(6) 0.032(5) 0.040(6) -0.001(4) 0.014(5) 0.000(4) N9 0.047(6) 0.037(6) 0.040(6) 0.002(4) 0.009(5) -0.004(5) N2 0.032(5) 0.044(6) 0.055(6) -0.006(5) 0.015(5) -0.005(5) N5 0.027(5) 0.036(5) 0.047(6) 0.007(4) 0.012(4) -0.001(4) N14 0.049(6) 0.043(6) 0.069(7) 0.024(5) 0.004(5) -0.016(5) N13 0.043(6) 0.039(6) 0.040(6) 0.007(5) 0.013(5) 0.005(5) N12 0.041(5) 0.030(5) 0.041(6) -0.003(4) 0.021(5) 0.002(4) C15 0.057(8) 0.022(6) 0.048(7) 0.004(5) 0.003(6) 0.003(6) N11 0.037(5) 0.033(5) 0.031(5) 0.007(4) 0.017(4) 0.000(4) N4 0.051(6) 0.032(5) 0.041(6) 0.004(4) 0.028(5) 0.015(5) N8 0.070(7) 0.044(6) 0.054(7) -0.011(5) 0.016(6) -0.006(6) N1 0.029(5) 0.070(7) 0.065(7) -0.005(5) 0.018(5) -0.012(5) C10 0.043(7) 0.037(7) 0.047(7) 0.003(6) 0.026(6) 0.003(6) C25 0.041(7) 0.040(7) 0.041(7) 0.005(5) 0.016(6) 0.003(6) C2 0.033(7) 0.034(7) 0.048(7) 0.001(5) 0.005(5) -0.003(5) C9 0.050(8) 0.032(7) 0.054(8) 0.006(5) 0.033(6) 0.001(6) C11 0.053(8) 0.056(8) 0.080(10) 0.019(7) 0.030(7) -0.002(7) N6 0.035(6) 0.068(7) 0.037(6) 0.008(5) 0.012(5) -0.001(5) C5 0.042(7) 0.037(6) 0.027(6) 0.007(5) 0.014(5) 0.013(5) C23 0.047(7) 0.037(7) 0.032(6) 0.005(5) 0.012(5) 0.003(6) C18 0.037(6) 0.040(7) 0.037(6) 0.001(5) 0.016(5) -0.003(5) C3 0.034(6) 0.038(7) 0.034(6) 0.005(5) 0.003(5) 0.016(5) C12 0.044(7) 0.076(9) 0.033(7) 0.015(6) 0.010(6) -0.006(7) C22 0.040(7) 0.032(6) 0.034(6) 0.002(5) 0.006(5) 0.014(5) C17 0.044(7) 0.052(8) 0.058(8) 0.008(6) 0.023(6) -0.015(6) C21 0.069(9) 0.059(9) 0.038(7) 0.003(6) 0.023(6) 0.014(7) C6 0.065(9) 0.056(8) 0.036(7) 0.002(6) 0.011(6) 0.012(7) C16 0.031(6) 0.037(7) 0.042(7) 0.009(5) 0.010(5) 0.003(5) C7 0.078(10) 0.064(9) 0.044(8) 0.029(7) 0.026(8) 0.016(8) C4 0.057(8) 0.069(9) 0.047(8) -0.003(7) 0.009(6) 0.007(7) C20 0.091(10) 0.065(9) 0.040(8) 0.014(7) 0.038(7) 0.008(8) C26 0.071(10) 0.064(10) 0.082(10) 0.023(8) 0.021(8) -0.009(8) C1 0.049(9) 0.105(13) 0.095(11) -0.040(10) 0.022(8) -0.040(8) C14 0.061(9) 0.052(8) 0.069(9) -0.012(7) -0.004(7) -0.018(7) C13 0.069(11) 0.199(21) 0.079(12) 0.040(13) -0.017(9) -0.067(13) N7 0.055(8) 0.129(12) 0.051(7) 0.032(7) -0.016(6) -0.007(7) C8 0.067(9) 0.046(8) 0.063(9) 0.022(7) 0.043(8) 0.007(7) C24 0.053(8) 0.056(8) 0.047(8) -0.001(6) -0.003(6) -0.012(6) C19 0.078(10) 0.062(9) 0.046(8) 0.012(7) 0.033(7) 0.012(8) O1S 0.083(8) 0.123(10) 0.076(7) 0.044(7) 0.007(6) -0.013(7) O3S 0.200(16) 0.119(12) 0.193(15) 0.075(11) 0.087(13) 0.024(12) O2S 0.444(49) 0.288(37) 0.424(46) 0.188(34) -0.067(41) -0.192(39) C1S 0.265(45) 0.093(23) 0.319(56) -0.066(29) 0.224(45) -0.073(26) C2S 0.155(23) 0.213(31) 0.012(9) 0.036(14) 0.013(11) 0.160(23) _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 N5 2.067(9) . ? Zn1 N10 2.071(9) . ? Zn1 S3 2.385(3) . ? Zn1 S2 2.398(3) . ? Zn1 N4 2.493(8) . ? Zn1 N11 2.549(9) . ? Zn2 N3 2.061(9) . ? Zn2 N12 2.072(9) . ? Zn2 S1 2.310(3) . ? Zn2 S4 2.344(3) . ? S3 C15 1.750(13) . ? S1 C2 1.734(11) . ? S4 C25 1.730(11) . ? S2 C12 1.704(13) . ? N3 C3 1.309(12) . ? N3 N2 1.392(11) . ? N10 C16 1.293(12) . ? N10 N9 1.380(11) . ? N9 C15 1.325(14) . ? N2 C2 1.314(13) . ? N5 C10 1.297(12) . ? N5 N6 1.391(11) . ? N14 C25 1.332(13) . ? N14 C26 1.452(15) . ? N13 C25 1.343(12) . ? N13 N12 1.397(11) . ? N12 C23 1.294(12) . ? C15 N8 1.363(13) . ? N11 C18 1.342(12) . ? N11 C22 1.364(12) . ? N4 C5 1.326(13) . ? N4 C9 1.364(13) . ? N8 C14 1.454(15) . ? N1 C2 1.350(13) . ? N1 C1 1.462(14) . ? C10 C9 1.46(2) . ? C10 C11 1.50(2) . ? C9 C8 1.378(14) . ? N6 C12 1.358(14) . ? C5 C6 1.388(14) . ? C5 C3 1.446(15) . ? C23 C24 1.462(15) . ? C23 C22 1.465(14) . ? C18 C19 1.384(14) . ? C18 C16 1.491(14) . ? C3 C4 1.499(15) . ? C12 N7 1.336(14) . ? C22 C21 1.399(14) . ? C17 C16 1.486(14) . ? C21 C20 1.35(2) . ? C6 C7 1.37(2) . ? C7 C8 1.37(2) . ? C20 C19 1.38(2) . ? C13 N7 1.49(2) . ? O1S C1S' 1.45(3) . ? O1S C1S 1.50(2) . ? C1S C2S 1.48(2) . ? C1S' C2S' 1.51(3) . ? 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 N5 Zn1 N10 162.8(3) . . ? N5 Zn1 S3 111.9(3) . . ? N10 Zn1 S3 83.2(3) . . ? N5 Zn1 S2 82.4(3) . . ? N10 Zn1 S2 100.3(2) . . ? S3 Zn1 S2 111.08(12) . . ? N5 Zn1 N4 72.6(3) . . ? N10 Zn1 N4 102.2(3) . . ? N4 Zn1 N11 88.48(3) . . ? N10 Zn1 N11 70.33(3) . . ? S3 Zn1 N4 83.7(2) . . ? S2 Zn1 N4 154.4(2) . . ? N3 Zn2 N12 144.8(3) . . ? N3 Zn2 S1 85.3(3) . . ? N12 Zn2 S1 119.7(2) . . ? N3 Zn2 S4 108.1(2) . . ? N12 Zn2 S4 84.4(3) . . ? S1 Zn2 S4 115.47(13) . . ? C15 S3 Zn1 93.6(4) . . ? C2 S1 Zn2 93.3(4) . . ? C25 S4 Zn2 94.1(4) . . ? C12 S2 Zn1 95.0(4) . . ? C3 N3 N2 117.1(9) . . ? C3 N3 Zn2 123.2(8) . . ? N2 N3 Zn2 118.7(6) . . ? C16 N10 N9 115.3(9) . . ? C16 N10 Zn1 123.4(7) . . ? N9 N10 Zn1 121.2(7) . . ? C15 N9 N10 114.1(9) . . ? C2 N2 N3 113.6(9) . . ? C10 N5 N6 115.4(9) . . ? C10 N5 Zn1 122.9(8) . . ? N6 N5 Zn1 121.6(6) . . ? C25 N14 C26 124.7(10) . . ? C25 N13 N12 114.1(9) . . ? C23 N12 N13 115.6(9) . . ? C23 N12 Zn2 125.2(8) . . ? N13 N12 Zn2 119.0(6) . . ? N9 C15 N8 115.5(11) . . ? N9 C15 S3 128.0(9) . . ? N8 C15 S3 116.5(10) . . ? C18 N11 C22 118.4(9) . . ? C5 N4 C9 119.7(9) . . ? C5 N4 Zn1 123.7(7) . . ? C9 N4 Zn1 102.2(7) . . ? C15 N8 C14 122.7(11) . . ? C2 N1 C1 124.4(10) . . ? N5 C10 C9 115.7(10) . . ? N5 C10 C11 123.4(10) . . ? C9 C10 C11 120.8(10) . . ? N14 C25 N13 115.4(10) . . ? N14 C25 S4 116.9(8) . . ? N13 C25 S4 127.8(9) . . ? N2 C2 N1 114.5(10) . . ? N2 C2 S1 129.1(9) . . ? N1 C2 S1 116.3(9) . . ? N4 C9 C8 120.2(11) . . ? N4 C9 C10 118.1(10) . . ? C8 C9 C10 121.6(11) . . ? C12 N6 N5 113.6(9) . . ? N4 C5 C6 121.6(11) . . ? N4 C5 C3 117.4(9) . . ? C6 C5 C3 120.9(10) . . ? N12 C23 C24 123.5(10) . . ? N12 C23 C22 115.1(10) . . ? C24 C23 C22 121.4(10) . . ? N11 C18 C19 122.1(10) . . ? N11 C18 C16 115.6(9) . . ? C19 C18 C16 122.3(11) . . ? N3 C3 C5 117.0(10) . . ? N3 C3 C4 121.7(10) . . ? C5 C3 C4 121.3(10) . . ? N7 C12 N6 113.9(11) . . ? N7 C12 S2 118.6(10) . . ? N6 C12 S2 127.4(9) . . ? N11 C22 C21 120.8(10) . . ? N11 C22 C23 117.9(9) . . ? C21 C22 C23 121.2(10) . . ? C20 C21 C22 119.8(12) . . ? C7 C6 C5 119.0(11) . . ? N10 C16 C17 124.5(10) . . ? N10 C16 C18 115.8(9) . . ? C17 C16 C18 119.7(10) . . ? C8 C7 C6 119.5(11) . . ? C21 C20 C19 119.5(12) . . ? C12 N7 C13 124.6(12) . . ? C7 C8 C9 119.9(12) . . ? C20 C19 C18 119.3(12) . . ? C2S C1S O1S 131.9(21) . . ? O1S C1S' C2S' 122.4(37) . . ? 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 N5 Zn1 S3 C15 -170.5(4) . . . . ? N10 Zn1 S3 C15 0.9(4) . . . . ? S2 Zn1 S3 C15 99.3(4) . . . . ? N4 Zn1 S3 C15 -102.2(4) . . . . ? N3 Zn2 S1 C2 0.0(4) . . . . ? N12 Zn2 S1 C2 -153.8(4) . . . . ? S4 Zn2 S1 C2 107.7(4) . . . . ? N3 Zn2 S4 C25 -140.7(4) . . . . ? N12 Zn2 S4 C25 5.6(4) . . . . ? S1 Zn2 S4 C25 125.9(4) . . . . ? N5 Zn1 S2 C12 1.7(5) . . . . ? N10 Zn1 S2 C12 -161.1(5) . . . . ? S3 Zn1 S2 C12 112.3(4) . . . . ? N4 Zn1 S2 C12 -10.1(7) . . . . ? N12 Zn2 N3 C3 -52.6(10) . . . . ? S1 Zn2 N3 C3 169.3(8) . . . . ? S4 Zn2 N3 C3 54.0(8) . . . . ? N12 Zn2 N3 N2 139.7(7) . . . . ? S1 Zn2 N3 N2 1.5(7) . . . . ? S4 Zn2 N3 N2 -113.7(7) . . . . ? N5 Zn1 N10 C16 -33.5(16) . . . . ? S3 Zn1 N10 C16 174.3(8) . . . . ? S2 Zn1 N10 C16 64.1(8) . . . . ? N4 Zn1 N10 C16 -103.6(8) . . . . ? N5 Zn1 N10 N9 151.4(10) . . . . ? S3 Zn1 N10 N9 -0.8(7) . . . . ? S2 Zn1 N10 N9 -111.0(7) . . . . ? N4 Zn1 N10 N9 81.3(7) . . . . ? C16 N10 N9 C15 -175.3(9) . . . . ? Zn1 N10 N9 C15 0.2(11) . . . . ? C3 N3 N2 C2 -171.3(9) . . . . ? Zn2 N3 N2 C2 -2.9(11) . . . . ? N10 Zn1 N5 C10 -85.4(14) . . . . ? S3 Zn1 N5 C10 64.6(8) . . . . ? S2 Zn1 N5 C10 174.3(8) . . . . ? N4 Zn1 N5 C10 -11.0(8) . . . . ? N10 Zn1 N5 N6 98.3(12) . . . . ? S3 Zn1 N5 N6 -111.7(7) . . . . ? S2 Zn1 N5 N6 -2.0(7) . . . . ? N4 Zn1 N5 N6 172.8(8) . . . . ? C25 N13 N12 C23 -168.8(9) . . . . ? C25 N13 N12 Zn2 6.3(11) . . . . ? N3 Zn2 N12 C23 -79.2(10) . . . . ? S1 Zn2 N12 C23 50.8(9) . . . . ? S4 Zn2 N12 C23 167.1(8) . . . . ? N3 Zn2 N12 N13 106.2(8) . . . . ? S1 Zn2 N12 N13 -123.8(6) . . . . ? S4 Zn2 N12 N13 -7.6(6) . . . . ? N10 N9 C15 N8 -177.3(8) . . . . ? N10 N9 C15 S3 1.0(14) . . . . ? Zn1 S3 C15 N9 -1.4(10) . . . . ? Zn1 S3 C15 N8 176.9(8) . . . . ? N5 Zn1 N4 C5 160.5(8) . . . . ? N10 Zn1 N4 C5 -36.4(8) . . . . ? S3 Zn1 N4 C5 45.2(7) . . . . ? S2 Zn1 N4 C5 172.7(6) . . . . ? N5 Zn1 N4 C9 21.7(6) . . . . ? N10 Zn1 N4 C9 -175.2(6) . . . . ? S3 Zn1 N4 C9 -93.6(6) . . . . ? S2 Zn1 N4 C9 33.9(9) . . . . ? N9 C15 N8 C14 9.0(15) . . . . ? S3 C15 N8 C14 -169.6(9) . . . . ? N6 N5 C10 C9 174.3(8) . . . . ? Zn1 N5 C10 C9 -2.2(12) . . . . ? N6 N5 C10 C11 -3.9(14) . . . . ? Zn1 N5 C10 C11 179.6(8) . . . . ? C26 N14 C25 N13 0.3(17) . . . . ? C26 N14 C25 S4 180.0(10) . . . . ? N12 N13 C25 N14 179.9(9) . . . . ? N12 N13 C25 S4 0.2(14) . . . . ? Zn2 S4 C25 N14 175.2(8) . . . . ? Zn2 S4 C25 N13 -5.2(10) . . . . ? N3 N2 C2 N1 -178.5(9) . . . . ? N3 N2 C2 S1 3.2(14) . . . . ? C1 N1 C2 N2 -2.5(17) . . . . ? C1 N1 C2 S1 176.0(10) . . . . ? Zn2 S1 C2 N2 -1.8(10) . . . . ? Zn2 S1 C2 N1 180.0(8) . . . . ? C5 N4 C9 C8 3.8(15) . . . . ? Zn1 N4 C9 C8 144.7(9) . . . . ? C5 N4 C9 C10 -172.2(9) . . . . ? Zn1 N4 C9 C10 -31.3(10) . . . . ? N5 C10 C9 N4 26.8(14) . . . . ? C11 C10 C9 N4 -154.9(10) . . . . ? N5 C10 C9 C8 -149.0(10) . . . . ? C11 C10 C9 C8 29.2(16) . . . . ? C10 N5 N6 C12 -175.2(9) . . . . ? Zn1 N5 N6 C12 1.3(12) . . . . ? C9 N4 C5 C6 0.2(15) . . . . ? Zn1 N4 C5 C6 -132.0(9) . . . . ? C9 N4 C5 C3 -176.4(9) . . . . ? Zn1 N4 C5 C3 51.4(11) . . . . ? N13 N12 C23 C24 0.8(15) . . . . ? Zn2 N12 C23 C24 -174.0(8) . . . . ? N13 N12 C23 C22 179.3(8) . . . . ? Zn2 N12 C23 C22 4.6(13) . . . . ? C22 N11 C18 C19 -0.5(15) . . . . ? C22 N11 C18 C16 -178.9(8) . . . . ? N2 N3 C3 C5 -179.3(8) . . . . ? Zn2 N3 C3 C5 12.7(12) . . . . ? N2 N3 C3 C4 1.8(14) . . . . ? Zn2 N3 C3 C4 -166.2(8) . . . . ? N4 C5 C3 N3 35.8(13) . . . . ? C6 C5 C3 N3 -140.8(10) . . . . ? N4 C5 C3 C4 -145.3(10) . . . . ? C6 C5 C3 C4 38.1(15) . . . . ? N5 N6 C12 N7 178.4(10) . . . . ? N5 N6 C12 S2 0.7(15) . . . . ? Zn1 S2 C12 N7 -179.5(10) . . . . ? Zn1 S2 C12 N6 -1.9(11) . . . . ? C18 N11 C22 C21 3.4(14) . . . . ? C18 N11 C22 C23 -172.7(9) . . . . ? N12 C23 C22 N11 37.7(13) . . . . ? C24 C23 C22 N11 -143.7(10) . . . . ? N12 C23 C22 C21 -138.4(10) . . . . ? C24 C23 C22 C21 40.2(15) . . . . ? N11 C22 C21 C20 -3.3(16) . . . . ? C23 C22 C21 C20 172.7(11) . . . . ? N4 C5 C6 C7 -2.8(17) . . . . ? C3 C5 C6 C7 173.7(11) . . . . ? N9 N10 C16 C17 2.1(15) . . . . ? Zn1 N10 C16 C17 -173.3(8) . . . . ? N9 N10 C16 C18 -177.9(8) . . . . ? Zn1 N10 C16 C18 6.7(13) . . . . ? N11 C18 C16 N10 26.4(13) . . . . ? C19 C18 C16 N10 -152.0(11) . . . . ? N11 C18 C16 C17 -153.6(9) . . . . ? C19 C18 C16 C17 27.9(15) . . . . ? C5 C6 C7 C8 1.4(18) . . . . ? C22 C21 C20 C19 0.2(18) . . . . ? N6 C12 N7 C13 0.4(20) . . . . ? S2 C12 N7 C13 178.3(12) . . . . ? C6 C7 C8 C9 2.5(18) . . . . ? N4 C9 C8 C7 -5.1(17) . . . . ? C10 C9 C8 C7 170.7(11) . . . . ? C21 C20 C19 C18 2.7(19) . . . . ? N11 C18 C19 C20 -2.6(17) . . . . ? C16 C18 C19 C20 175.8(11) . . . . ? C1S' O1S C1S C2S 13.0(42) . . . . ? C1S O1S C1S' C2S' -0.6(46) . . . . ? _refine_diff_density_max 1.169 _refine_diff_density_min -0.501 _refine_diff_density_rms 0.123 data_mndaptszme _database_code_depnum_ccdc_archive 'CCDC 240032' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H29 Mn N7 O2 S2' _chemical_formula_weight 482.52 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' Mn Mn 0.3368 0.7283 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.981(6) _cell_length_b 10.466(4) _cell_length_c 14.281(4) _cell_angle_alpha 90.000(4) _cell_angle_beta 100.32(2) _cell_angle_gamma 90.00(2) _cell_volume 2202.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 0.817 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5038 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0091 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 27.44 _reflns_number_total 2519 _reflns_number_gt 2450 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2519 _refine_ls_number_parameters 187 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0011 _refine_ls_R_factor_gt 0.0008 _refine_ls_wR_factor_ref 0.0033 _refine_ls_wR_factor_gt 0.0022 _refine_ls_goodness_of_fit_ref 0.246 _refine_ls_restrained_S_all 0.246 _refine_ls_shift/su_max 0.061 _refine_ls_shift/su_mean 0.010 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.0000 0.476570(2) 0.2500 0.03154(1) Uani 1 2 d S . . S1 S -0.079872(2) 0.286829(2) 0.152843(2) 0.04578(1) Uani 1 1 d . . . N4 N 0.0000 0.692800(9) 0.2500 0.03133(2) Uani 1 2 d S . . N3 N -0.071205(5) 0.555992(7) 0.099544(5) 0.03156(2) Uani 1 1 d . . . N2 N -0.104903(6) 0.481205(7) 0.021958(5) 0.03368(2) Uani 1 1 d . . . N1 N -0.133912(7) 0.281004(8) -0.033707(6) 0.04447(2) Uani 1 1 d . . . C5 C -0.037689(6) 0.757091(8) 0.171106(7) 0.03338(2) Uani 1 1 d . . . C6 C -0.038908(8) 0.890729(9) 0.169503(8) 0.04406(2) Uani 1 1 d . . . C7 C 0.0000 0.956100(13) 0.2500 0.04890(4) Uani 1 2 d S . . C4 C -0.076904(6) 0.678904(8) 0.087298(7) 0.03346(2) Uani 1 1 d . . . C3 C -0.120302(10) 0.742115(12) -0.003807(9) 0.05090(3) Uani 1 1 d . . . C2 C -0.106712(6) 0.356097(9) 0.043090(6) 0.03318(2) Uani 1 1 d . . . C1 C -0.146606(10) 0.144600(11) -0.032100(9) 0.05117(3) Uani 1 1 d . . . O1S O 0.122895(5) 0.498897(7) 0.172710(5) 0.04107(2) Uani 1 1 d . . . C1S C 0.218091(8) 0.480685(12) 0.207197(9) 0.04995(3) Uani 1 1 d . . . C2S C 0.256634(10) 0.584503(15) 0.272902(11) 0.05974(3) Uani 1 1 d . . . H1N H -0.14463(8) 0.31796(11) -0.08851(9) 0.0529(3) Uiso 1 1 d . . . H6A H -0.06574(8) 0.93445(11) 0.11491(9) 0.0529(3) Uiso 1 1 d . . . H7A H 0.0000 1.04499(17) 0.2500 0.0589(5) Uiso 1 2 d S . . H3A H -0.14206(10) 0.67793(14) -0.05044(11) 0.0766(5) Uiso 1 1 d . . . H3B H -0.07645(10) 0.79487(14) -0.02694(11) 0.0769(5) Uiso 1 1 d . . . H3C H -0.17025(10) 0.79391(14) 0.00730(10) 0.0764(4) Uiso 1 1 d . . . H1A H -0.16618(10) 0.11412(14) -0.09586(11) 0.0774(4) Uiso 1 1 d . . . H1C H -0.19163(10) 0.12462(14) 0.00563(11) 0.0771(5) Uiso 1 1 d . . . H1B H -0.09020(10) 0.10429(14) -0.00491(11) 0.0759(5) Uiso 1 1 d . . . H1SA H 0.24974(8) 0.47808(12) 0.15373(10) 0.0599(4) Uiso 1 1 d . . . H1SB H 0.22758(8) 0.39945(12) 0.24025(9) 0.0601(4) Uiso 1 1 d . . . H2SA H 0.32022(11) 0.56936(15) 0.29447(11) 0.0891(5) Uiso 1 1 d . . . H2SB H 0.22606(11) 0.58657(15) 0.32634(12) 0.0880(5) Uiso 1 1 d . . . H2SC H 0.24852(10) 0.66503(15) 0.24013(12) 0.0896(5) Uiso 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 Mn1 0.04790(1) 0.02310(1) 0.02240(1) 0.000 0.00300(1) 0.000 S1 0.07963(2) 0.03030(1) 0.02431(1) 0.00210(1) 0.00091(1) -0.00911(1) N4 0.04293(6) 0.02328(5) 0.02799(5) 0.000 0.00692(4) 0.000 N3 0.03893(4) 0.02826(4) 0.02742(4) 0.00078(3) 0.00578(3) 0.00169(3) N2 0.04614(4) 0.03058(4) 0.02290(4) 0.00091(3) 0.00239(3) 0.00119(3) N1 0.07182(6) 0.03355(4) 0.02330(4) -0.00165(3) -0.00424(4) -0.00332(4) C5 0.04119(5) 0.02699(4) 0.03309(5) 0.00277(4) 0.00972(4) 0.00196(4) C6 0.05786(6) 0.02534(5) 0.04800(6) 0.00810(4) 0.00680(5) 0.00519(4) C7 0.06491(10) 0.02015(6) 0.06182(10) 0.000 0.01179(8) 0.000 C4 0.04154(5) 0.02755(4) 0.03143(5) 0.00419(3) 0.00694(4) 0.00450(4) C3 0.07106(8) 0.03902(6) 0.03895(6) 0.01028(5) -0.00008(6) 0.01299(6) C2 0.03918(5) 0.03517(5) 0.02478(4) -0.00086(3) 0.00460(4) 0.00148(4) C1 0.07404(9) 0.03396(5) 0.04200(6) -0.00706(5) 0.00094(6) -0.00546(5) O1S 0.04222(4) 0.04990(4) 0.03039(3) 0.00351(3) 0.00460(3) 0.00460(3) C1S 0.04704(6) 0.05103(7) 0.04999(7) 0.00137(5) 0.00389(5) 0.01018(5) C2S 0.05606(8) 0.06003(8) 0.06008(8) 0.00096(6) 0.00213(7) -0.00694(6) _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 Mn1 N4 2.2631(9) . ? Mn1 O1S 2.3218(7) 2 ? Mn1 O1S 2.3218(7) . ? Mn1 N3 2.3716(6) 2 ? Mn1 N3 2.3716(6) . ? Mn1 S1 2.5895(7) . ? Mn1 S1 2.5895(7) 2 ? S1 C2 1.7083(4) . ? N4 C5 1.3465(4) 2 ? N4 C5 1.3465(4) . ? N3 C4 1.2990(5) . ? N3 N2 1.3765(4) . ? N2 C2 1.3451(5) . ? N1 C2 1.3515(3) . ? N1 C1 1.4409(6) . ? C5 C6 1.3989(5) . ? C5 C4 1.4817(4) . ? C6 C7 1.3745(4) . ? C7 C6 1.3745(4) 2 ? C4 C3 1.5000(4) . ? O1S C1S 1.4357(6) . ? C1S C2S 1.4834(4) . ? 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 Mn1 O1S 84.224(16) . 2 ? N4 Mn1 O1S 84.224(16) . . ? O1S Mn1 O1S 168.447(7) 2 . ? N4 Mn1 N3 69.482(13) . 2 ? O1S Mn1 N3 78.48(3) 2 2 ? O1S Mn1 N3 97.42(2) . 2 ? N4 Mn1 N3 69.482(13) . . ? O1S Mn1 N3 97.42(2) 2 . ? O1S Mn1 N3 78.48(3) . . ? N3 Mn1 N3 138.964(19) 2 . ? N4 Mn1 S1 140.074(15) . . ? O1S Mn1 S1 90.13(2) 2 . ? O1S Mn1 S1 98.75(2) . . ? N3 Mn1 S1 147.555(6) 2 . ? N3 Mn1 S1 72.16(2) . . ? N4 Mn1 S1 140.074(15) . 2 ? O1S Mn1 S1 98.75(2) 2 2 ? O1S Mn1 S1 90.13(2) . 2 ? N3 Mn1 S1 72.16(2) 2 2 ? N3 Mn1 S1 147.555(7) . 2 ? S1 Mn1 S1 79.85(3) . 2 ? C2 S1 Mn1 100.16(2) . . ? C5 N4 C5 120.04(3) 2 . ? C5 N4 Mn1 119.981(15) 2 . ? C5 N4 Mn1 119.981(15) . . ? C4 N3 N2 116.677(19) . . ? C4 N3 Mn1 118.498(12) . . ? N2 N3 Mn1 124.79(2) . . ? C2 N2 N3 113.09(2) . . ? C2 N1 C1 125.781(17) . . ? N4 C5 C6 121.038(17) . . ? N4 C5 C4 116.49(3) . . ? C6 C5 C4 122.469(17) . . ? C7 C6 C5 118.792(18) . . ? C6 C7 C6 120.30(3) . 2 ? N3 C4 C5 115.54(2) . . ? N3 C4 C3 124.150(14) . . ? C5 C4 C3 120.30(3) . . ? N2 C2 N1 113.53(2) . . ? N2 C2 S1 127.452(10) . . ? N1 C2 S1 119.01(2) . . ? C1S O1S Mn1 130.33(2) . . ? O1S C1S C2S 111.71(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.006 _refine_diff_density_min -0.008 _refine_diff_density_rms 0.001