# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Dong-Sheng Li' _publ_contact_author_email LIDONGSHENG1@126.COM _publ_section_title ; A versatile V-shaped tetracarboxylate building block for con-structing mixed-ligand Co(II) and Mn(II) complexes incorporating with various N-donor co-ligands ; loop_ _publ_author_name 'Dong-Sheng Li' 'Miao Du' 'Feng Fu' 'Xiao-Ming Gao' 'Cai-Xia Meng' ; Long Tang ; 'Ya-Pan Wu' 'Xiao-Ning Zhang' # Attachment '1.cif' data_b _database_code_depnum_ccdc_archive 'CCDC 737213' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H21 Co N3 O11 S' _chemical_formula_weight 702.50 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' Co Co 0.3494 0.9721 '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 10.383(4) _cell_length_b 10.589(4) _cell_length_c 13.430(5) _cell_angle_alpha 97.769(4) _cell_angle_beta 91.815(4) _cell_angle_gamma 92.824(4) _cell_volume 1460.1(9) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 2704 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 26.51 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 718 _exptl_absorpt_coefficient_mu 0.730 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8027 _exptl_absorpt_correction_T_max 0.8990 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10005 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.0654 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5242 _reflns_number_gt 4182 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1008P)^2^+9.3062P] 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 CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5242 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0952 _refine_ls_R_factor_gt 0.0815 _refine_ls_wR_factor_ref 0.2512 _refine_ls_wR_factor_gt 0.2411 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.138 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.76100(8) 0.75885(8) 0.52585(6) 0.0248(3) Uani 1 1 d . . . S1 S 0.79764(19) 0.56705(17) 1.01090(14) 0.0371(5) Uani 1 1 d . . . O1 O 0.8873(5) 0.7601(4) 0.6523(3) 0.0321(11) Uani 1 1 d . . . O2 O 0.8536(5) 0.9537(5) 0.7315(4) 0.0387(12) Uani 1 1 d . . . O3 O 1.1488(5) 0.9294(6) 0.7407(4) 0.0490(14) Uani 1 1 d . . . H3 H 1.2111 0.9697 0.7225 0.074 Uiso 1 1 d R . . O4 O 1.2221(10) 1.0170(11) 0.8913(6) 0.129(5) Uani 1 1 d . . . O5 O 0.8718(6) 0.5154(6) 1.0864(4) 0.0520(15) Uani 1 1 d . . . O6 O 0.7370(6) 0.4837(5) 0.9272(4) 0.0529(16) Uani 1 1 d . . . O7 O 0.3136(5) 0.9276(6) 1.1612(4) 0.0500(15) Uani 1 1 d . . . H7 H 0.2401 0.8952 1.1607 0.075 Uiso 1 1 d R . . O8 O 0.3773(5) 0.8822(5) 1.3123(4) 0.0391(12) Uani 1 1 d . . . O9 O 0.6343(4) 0.7543(4) 1.3947(3) 0.0284(10) Uani 1 1 d . . . O10 O 0.6694(5) 0.9493(4) 1.3490(3) 0.0300(10) Uani 1 1 d . . . O11 O 0.7704(6) 0.9528(4) 0.5334(4) 0.0419(13) Uani 1 1 d . . . H1W H 0.7145 1.0053 0.5477 0.063 Uiso 1 1 d R . . H2W H 0.8371 0.9705 0.5693 0.063 Uiso 1 1 d R . . N1 N 0.9069(5) 0.7082(5) 0.4209(4) 0.0289(12) Uani 1 1 d . . . N2 N 0.7506(5) 0.5617(5) 0.5084(4) 0.0251(11) Uani 1 1 d . . . N3 N 0.6053(5) 0.7109(5) 0.6206(4) 0.0300(12) Uani 1 1 d . . . C1 C 0.9801(7) 0.7898(7) 0.3757(5) 0.0358(16) Uani 1 1 d . . . H1 H 0.9733 0.8771 0.3937 0.043 Uiso 1 1 calc R . . C2 C 1.0658(7) 0.7474(8) 0.3029(6) 0.0418(18) Uani 1 1 d . . . H2 H 1.1144 0.8057 0.2717 0.050 Uiso 1 1 calc R . . C3 C 1.0781(8) 0.6202(8) 0.2776(6) 0.0448(19) Uani 1 1 d . . . H3A H 1.1372 0.5910 0.2304 0.054 Uiso 1 1 calc R . . C4 C 1.0026(7) 0.5346(7) 0.3222(6) 0.0382(17) Uani 1 1 d . . . H4 H 1.0084 0.4472 0.3043 0.046 Uiso 1 1 calc R . . C5 C 0.9177(6) 0.5815(6) 0.3944(5) 0.0275(14) Uani 1 1 d . . . C6 C 0.8311(6) 0.4978(6) 0.4457(5) 0.0291(14) Uani 1 1 d . . . C7 C 0.8280(7) 0.3651(7) 0.4330(6) 0.0390(17) Uani 1 1 d . . . H7A H 0.8841 0.3205 0.3903 0.047 Uiso 1 1 calc R . . C8 C 0.7399(8) 0.3016(7) 0.4852(7) 0.045(2) Uani 1 1 d . . . H8 H 0.7358 0.2129 0.4771 0.054 Uiso 1 1 calc R . . C9 C 0.6573(7) 0.3672(7) 0.5495(6) 0.0387(17) Uani 1 1 d . . . H9 H 0.5979 0.3237 0.5846 0.046 Uiso 1 1 calc R . . C10 C 0.6650(7) 0.4996(6) 0.5605(5) 0.0295(14) Uani 1 1 d . . . C11 C 0.5859(6) 0.5862(6) 0.6257(5) 0.0309(15) Uani 1 1 d . . . C12 C 0.4962(8) 0.5409(8) 0.6901(6) 0.0415(18) Uani 1 1 d . . . H12 H 0.4831 0.4539 0.6924 0.050 Uiso 1 1 calc R . . C13 C 0.4272(8) 0.6287(9) 0.7503(6) 0.047(2) Uani 1 1 d . . . H13 H 0.3678 0.6015 0.7943 0.056 Uiso 1 1 calc R . . C14 C 0.4480(8) 0.7559(9) 0.7440(6) 0.049(2) Uani 1 1 d . . . H14 H 0.4030 0.8160 0.7839 0.059 Uiso 1 1 calc R . . C15 C 0.5365(7) 0.7947(7) 0.6777(6) 0.0404(17) Uani 1 1 d . . . H15 H 0.5485 0.8812 0.6726 0.048 Uiso 1 1 calc R . . C16 C 0.8920(6) 0.8436(6) 0.7289(5) 0.0261(14) Uani 1 1 d . . . C17 C 0.9392(6) 0.8049(6) 0.8261(5) 0.0258(13) Uani 1 1 d . . . C18 C 0.8623(6) 0.7161(6) 0.8674(5) 0.0295(14) Uani 1 1 d . . . H18 H 0.7885 0.6786 0.8321 0.035 Uiso 1 1 calc R . . C19 C 0.8950(7) 0.6827(7) 0.9617(5) 0.0305(15) Uani 1 1 d . . . C20 C 1.0023(7) 0.7407(8) 1.0169(6) 0.0424(18) Uani 1 1 d . . . H20 H 1.0213 0.7212 1.0810 0.051 Uiso 1 1 calc R . . C21 C 1.0806(7) 0.8275(8) 0.9758(6) 0.0429(19) Uani 1 1 d . . . H21 H 1.1537 0.8654 1.0118 0.051 Uiso 1 1 calc R . . C22 C 1.0509(6) 0.8588(7) 0.8806(5) 0.0320(15) Uani 1 1 d . . . C23 C 1.1480(8) 0.9459(8) 0.8395(6) 0.0447(19) Uani 1 1 d . . . C24 C 0.6359(6) 0.8297(7) 1.3307(5) 0.0279(15) Uani 1 1 d . . . C25 C 0.6034(6) 0.7762(6) 1.2231(5) 0.0263(14) Uani 1 1 d . . . C26 C 0.6947(6) 0.7030(6) 1.1739(5) 0.0289(14) Uani 1 1 d . . . H26 H 0.7689 0.6853 1.2088 0.035 Uiso 1 1 calc R . . C27 C 0.6761(7) 0.6558(6) 1.0726(5) 0.0314(15) Uani 1 1 d . . . C28 C 0.5672(8) 0.6813(8) 1.0192(6) 0.0441(19) Uani 1 1 d . . . H28 H 0.5554 0.6497 0.9513 0.053 Uiso 1 1 calc R . . C29 C 0.4762(8) 0.7544(8) 1.0679(6) 0.0456(19) Uani 1 1 d . . . H29 H 0.4026 0.7728 1.0326 0.055 Uiso 1 1 calc R . . C30 C 0.4936(7) 0.8009(7) 1.1697(5) 0.0318(15) Uani 1 1 d . . . C31 C 0.3894(7) 0.8738(7) 1.2220(5) 0.0312(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0285(5) 0.0216(5) 0.0246(5) 0.0049(3) -0.0003(3) 0.0006(3) S1 0.0494(11) 0.0309(9) 0.0330(10) 0.0058(7) 0.0165(8) 0.0082(8) O1 0.040(3) 0.031(2) 0.025(2) 0.004(2) -0.007(2) 0.007(2) O2 0.051(3) 0.031(3) 0.037(3) 0.004(2) 0.001(2) 0.019(2) O3 0.047(3) 0.060(4) 0.039(3) 0.005(3) 0.009(2) -0.018(3) O4 0.144(8) 0.172(10) 0.056(5) 0.014(5) -0.018(5) -0.126(8) O5 0.065(4) 0.052(3) 0.048(3) 0.026(3) 0.022(3) 0.031(3) O6 0.071(4) 0.037(3) 0.047(3) -0.011(3) 0.025(3) -0.011(3) O7 0.048(3) 0.069(4) 0.034(3) 0.004(3) -0.004(2) 0.030(3) O8 0.037(3) 0.050(3) 0.032(3) 0.008(2) 0.006(2) 0.012(2) O9 0.031(2) 0.029(2) 0.025(2) 0.0067(19) -0.0035(18) -0.0032(19) O10 0.043(3) 0.019(2) 0.028(2) 0.0038(18) 0.001(2) -0.0008(19) O11 0.064(4) 0.021(2) 0.039(3) 0.003(2) -0.007(3) 0.004(2) N1 0.028(3) 0.030(3) 0.028(3) 0.004(2) -0.001(2) 0.000(2) N2 0.030(3) 0.022(3) 0.023(3) 0.004(2) -0.005(2) -0.001(2) N3 0.031(3) 0.028(3) 0.031(3) 0.006(2) -0.002(2) -0.002(2) C1 0.034(4) 0.036(4) 0.038(4) 0.008(3) 0.002(3) 0.000(3) C2 0.033(4) 0.053(5) 0.042(4) 0.013(4) 0.008(3) 0.001(3) C3 0.039(4) 0.057(5) 0.040(4) 0.006(4) 0.012(3) 0.011(4) C4 0.042(4) 0.035(4) 0.037(4) -0.001(3) 0.007(3) 0.007(3) C5 0.031(3) 0.022(3) 0.029(3) 0.001(3) -0.007(3) 0.004(3) C6 0.030(3) 0.029(3) 0.029(3) 0.005(3) -0.005(3) 0.002(3) C7 0.045(4) 0.026(3) 0.046(4) 0.001(3) -0.005(3) 0.005(3) C8 0.052(5) 0.023(4) 0.061(5) 0.008(3) -0.008(4) 0.001(3) C9 0.039(4) 0.029(4) 0.049(5) 0.013(3) -0.003(3) -0.005(3) C10 0.033(3) 0.027(3) 0.031(3) 0.012(3) -0.004(3) 0.000(3) C11 0.030(3) 0.030(3) 0.033(4) 0.010(3) -0.005(3) -0.006(3) C12 0.044(4) 0.039(4) 0.044(4) 0.012(3) 0.009(3) -0.006(3) C13 0.038(4) 0.066(6) 0.037(4) 0.010(4) 0.010(3) -0.005(4) C14 0.044(5) 0.055(5) 0.046(5) -0.003(4) 0.012(4) 0.005(4) C15 0.039(4) 0.037(4) 0.044(4) -0.001(3) 0.005(3) 0.005(3) C16 0.018(3) 0.035(4) 0.024(3) 0.001(3) -0.002(2) 0.000(3) C17 0.028(3) 0.027(3) 0.022(3) -0.002(3) 0.000(2) 0.005(3) C18 0.028(3) 0.030(3) 0.028(3) -0.004(3) 0.000(3) 0.001(3) C19 0.035(4) 0.034(4) 0.024(3) 0.007(3) 0.006(3) 0.008(3) C20 0.039(4) 0.057(5) 0.033(4) 0.007(4) 0.000(3) 0.008(4) C21 0.035(4) 0.063(5) 0.030(4) 0.007(4) -0.003(3) -0.004(4) C22 0.026(3) 0.039(4) 0.031(4) 0.002(3) 0.001(3) 0.003(3) C23 0.040(4) 0.054(5) 0.038(4) 0.006(4) -0.002(3) -0.012(4) C24 0.013(3) 0.052(4) 0.021(3) 0.013(3) 0.001(2) 0.000(3) C25 0.025(3) 0.029(3) 0.027(3) 0.011(3) 0.004(3) 0.001(3) C26 0.028(3) 0.034(4) 0.026(3) 0.007(3) 0.000(3) 0.004(3) C27 0.036(4) 0.032(3) 0.027(3) 0.005(3) 0.009(3) 0.004(3) C28 0.042(4) 0.060(5) 0.027(4) -0.005(4) -0.002(3) 0.008(4) C29 0.046(5) 0.058(5) 0.032(4) 0.002(4) 0.002(3) 0.012(4) C30 0.030(3) 0.039(4) 0.026(3) 0.001(3) 0.001(3) 0.000(3) C31 0.031(4) 0.033(4) 0.028(4) -0.002(3) -0.004(3) 0.002(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 Co1 O11 2.040(5) . ? Co1 N2 2.067(5) . ? Co1 O1 2.111(5) . ? Co1 N1 2.140(6) . ? Co1 O9 2.159(4) 1_554 ? Co1 N3 2.171(6) . ? S1 O5 1.436(6) . ? S1 O6 1.439(6) . ? S1 C19 1.760(7) . ? S1 C27 1.771(7) . ? O1 C16 1.261(8) . ? O2 C16 1.247(8) . ? O3 C23 1.315(9) . ? O3 H3 0.8200 . ? O4 C23 1.187(10) . ? O7 C31 1.319(8) . ? O7 H7 0.8200 . ? O8 C31 1.214(8) . ? O9 C24 1.250(8) . ? O9 Co1 2.158(4) 1_556 ? O10 C24 1.286(8) . ? O11 H1W 0.8328 . ? O11 H2W 0.8306 . ? N1 C1 1.341(9) . ? N1 C5 1.351(8) . ? N2 C6 1.346(9) . ? N2 C10 1.348(8) . ? N3 C11 1.337(9) . ? N3 C15 1.341(9) . ? C1 C2 1.387(10) . ? C1 H1 0.9300 . ? C2 C3 1.357(12) . ? C2 H2 0.9300 . ? C3 C4 1.379(11) . ? C3 H3A 0.9300 . ? C4 C5 1.390(10) . ? C4 H4 0.9300 . ? C5 C6 1.481(9) . ? C6 C7 1.391(9) . ? C7 C8 1.374(11) . ? C7 H7A 0.9300 . ? C8 C9 1.381(11) . ? C8 H8 0.9300 . ? C9 C10 1.388(9) . ? C9 H9 0.9300 . ? C10 C11 1.478(10) . ? C11 C12 1.401(10) . ? C12 C13 1.389(11) . ? C12 H12 0.9300 . ? C13 C14 1.368(12) . ? C13 H13 0.9300 . ? C14 C15 1.385(11) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.495(9) . ? C17 C18 1.388(9) . ? C17 C22 1.405(9) . ? C18 C19 1.397(10) . ? C18 H18 0.9300 . ? C19 C20 1.387(10) . ? C20 C21 1.380(11) . ? C20 H20 0.9300 . ? C21 C22 1.393(10) . ? C21 H21 0.9300 . ? C22 C23 1.501(10) . ? C24 C25 1.501(9) . ? C25 C26 1.382(9) . ? C25 C30 1.383(9) . ? C26 C27 1.389(9) . ? C26 H26 0.9300 . ? C27 C28 1.377(10) . ? C28 C29 1.377(11) . ? C28 H28 0.9300 . ? C29 C30 1.391(10) . ? C29 H29 0.9300 . ? C30 C31 1.498(9) . ? 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 O11 Co1 N2 176.4(2) . . ? O11 Co1 O1 93.8(2) . . ? N2 Co1 O1 89.16(19) . . ? O11 Co1 N1 101.2(2) . . ? N2 Co1 N1 76.5(2) . . ? O1 Co1 N1 93.5(2) . . ? O11 Co1 O9 87.05(19) . 1_554 ? N2 Co1 O9 89.92(18) . 1_554 ? O1 Co1 O9 178.69(18) . 1_554 ? N1 Co1 O9 85.34(19) . 1_554 ? O11 Co1 N3 106.4(2) . . ? N2 Co1 N3 75.8(2) . . ? O1 Co1 N3 87.3(2) . . ? N1 Co1 N3 152.2(2) . . ? O9 Co1 N3 93.38(19) 1_554 . ? O5 S1 O6 120.2(4) . . ? O5 S1 C19 108.8(4) . . ? O6 S1 C19 107.5(3) . . ? O5 S1 C27 107.4(3) . . ? O6 S1 C27 107.8(4) . . ? C19 S1 C27 103.9(3) . . ? C16 O1 Co1 124.7(4) . . ? C23 O3 H3 109.5 . . ? C31 O7 H7 109.5 . . ? C24 O9 Co1 127.8(4) . 1_556 ? Co1 O11 H1W 130.4 . . ? Co1 O11 H2W 99.9 . . ? H1W O11 H2W 111.7 . . ? C1 N1 C5 118.7(6) . . ? C1 N1 Co1 125.9(5) . . ? C5 N1 Co1 115.3(4) . . ? C6 N2 C10 121.3(6) . . ? C6 N2 Co1 118.9(4) . . ? C10 N2 Co1 119.7(4) . . ? C11 N3 C15 119.3(6) . . ? C11 N3 Co1 114.8(5) . . ? C15 N3 Co1 125.7(5) . . ? N1 C1 C2 121.7(7) . . ? N1 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? C3 C2 C1 119.5(7) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 119.7(7) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? C3 C4 C5 118.7(7) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 121.6(6) . . ? N1 C5 C6 115.4(6) . . ? C4 C5 C6 123.0(6) . . ? N2 C6 C7 120.5(6) . . ? N2 C6 C5 113.8(6) . . ? C7 C6 C5 125.6(6) . . ? C8 C7 C6 118.2(7) . . ? C8 C7 H7A 120.9 . . ? C6 C7 H7A 120.9 . . ? C7 C8 C9 121.2(7) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C8 C9 C10 118.5(7) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.8 . . ? N2 C10 C9 120.2(7) . . ? N2 C10 C11 113.3(6) . . ? C9 C10 C11 126.5(6) . . ? N3 C11 C12 121.6(7) . . ? N3 C11 C10 116.2(6) . . ? C12 C11 C10 122.2(6) . . ? C13 C12 C11 118.7(7) . . ? C13 C12 H12 120.7 . . ? C11 C12 H12 120.7 . . ? C14 C13 C12 119.0(7) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? C13 C14 C15 119.7(8) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? N3 C15 C14 121.8(7) . . ? N3 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? O2 C16 O1 125.3(6) . . ? O2 C16 C17 117.1(6) . . ? O1 C16 C17 117.4(6) . . ? C18 C17 C22 118.6(6) . . ? C18 C17 C16 117.1(6) . . ? C22 C17 C16 124.2(6) . . ? C17 C18 C19 120.3(6) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C20 C19 C18 120.6(7) . . ? C20 C19 S1 120.1(6) . . ? C18 C19 S1 119.3(5) . . ? C21 C20 C19 119.4(7) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C20 C21 C22 120.4(7) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C21 C22 C17 120.6(7) . . ? C21 C22 C23 116.0(6) . . ? C17 C22 C23 123.3(6) . . ? O4 C23 O3 123.4(8) . . ? O4 C23 C22 123.2(8) . . ? O3 C23 C22 113.3(6) . . ? O9 C24 O10 125.0(6) . . ? O9 C24 C25 117.9(6) . . ? O10 C24 C25 116.9(6) . . ? C26 C25 C30 118.7(6) . . ? C26 C25 C24 116.4(6) . . ? C30 C25 C24 124.7(6) . . ? C25 C26 C27 120.4(6) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C28 C27 C26 120.9(6) . . ? C28 C27 S1 119.9(5) . . ? C26 C27 S1 119.1(5) . . ? C29 C28 C27 118.9(7) . . ? C29 C28 H28 120.6 . . ? C27 C28 H28 120.6 . . ? C28 C29 C30 120.5(7) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C25 C30 C29 120.6(7) . . ? C25 C30 C31 120.1(6) . . ? C29 C30 C31 119.3(6) . . ? O8 C31 O7 123.8(6) . . ? O8 C31 C30 122.4(6) . . ? O7 C31 C30 113.8(6) . . ? 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 O11 Co1 O1 C16 35.7(5) . . . . ? N2 Co1 O1 C16 -146.4(5) . . . . ? N1 Co1 O1 C16 137.2(5) . . . . ? O9 Co1 O1 C16 168(8) 1_554 . . . ? N3 Co1 O1 C16 -70.6(5) . . . . ? O11 Co1 N1 C1 -0.1(6) . . . . ? N2 Co1 N1 C1 177.0(6) . . . . ? O1 Co1 N1 C1 -94.7(6) . . . . ? O9 Co1 N1 C1 86.0(6) 1_554 . . . ? N3 Co1 N1 C1 174.4(5) . . . . ? O11 Co1 N1 C5 -175.5(4) . . . . ? N2 Co1 N1 C5 1.6(4) . . . . ? O1 Co1 N1 C5 89.9(5) . . . . ? O9 Co1 N1 C5 -89.5(5) 1_554 . . . ? N3 Co1 N1 C5 -1.1(7) . . . . ? O11 Co1 N2 C6 51(4) . . . . ? O1 Co1 N2 C6 -94.0(5) . . . . ? N1 Co1 N2 C6 -0.2(5) . . . . ? O9 Co1 N2 C6 85.0(5) 1_554 . . . ? N3 Co1 N2 C6 178.6(5) . . . . ? O11 Co1 N2 C10 -130(3) . . . . ? O1 Co1 N2 C10 85.2(5) . . . . ? N1 Co1 N2 C10 179.1(5) . . . . ? O9 Co1 N2 C10 -95.7(5) 1_554 . . . ? N3 Co1 N2 C10 -2.2(5) . . . . ? O11 Co1 N3 C11 -179.3(4) . . . . ? N2 Co1 N3 C11 3.8(5) . . . . ? O1 Co1 N3 C11 -86.1(5) . . . . ? N1 Co1 N3 C11 6.4(8) . . . . ? O9 Co1 N3 C11 92.8(5) 1_554 . . . ? O11 Co1 N3 C15 -4.3(6) . . . . ? N2 Co1 N3 C15 178.7(6) . . . . ? O1 Co1 N3 C15 88.9(6) . . . . ? N1 Co1 N3 C15 -178.6(5) . . . . ? O9 Co1 N3 C15 -92.2(6) 1_554 . . . ? C5 N1 C1 C2 0.2(10) . . . . ? Co1 N1 C1 C2 -175.1(5) . . . . ? N1 C1 C2 C3 -1.2(12) . . . . ? C1 C2 C3 C4 2.0(12) . . . . ? C2 C3 C4 C5 -1.7(12) . . . . ? C1 N1 C5 C4 0.1(10) . . . . ? Co1 N1 C5 C4 175.9(5) . . . . ? C1 N1 C5 C6 -178.4(6) . . . . ? Co1 N1 C5 C6 -2.6(7) . . . . ? C3 C4 C5 N1 0.7(11) . . . . ? C3 C4 C5 C6 179.1(7) . . . . ? C10 N2 C6 C7 -0.1(10) . . . . ? Co1 N2 C6 C7 179.2(5) . . . . ? C10 N2 C6 C5 179.6(6) . . . . ? Co1 N2 C6 C5 -1.1(7) . . . . ? N1 C5 C6 N2 2.5(8) . . . . ? C4 C5 C6 N2 -176.0(6) . . . . ? N1 C5 C6 C7 -177.8(6) . . . . ? C4 C5 C6 C7 3.7(11) . . . . ? N2 C6 C7 C8 0.7(10) . . . . ? C5 C6 C7 C8 -178.9(7) . . . . ? C6 C7 C8 C9 -0.7(12) . . . . ? C7 C8 C9 C10 0.0(12) . . . . ? C6 N2 C10 C9 -0.6(10) . . . . ? Co1 N2 C10 C9 -179.9(5) . . . . ? C6 N2 C10 C11 179.6(6) . . . . ? Co1 N2 C10 C11 0.4(7) . . . . ? C8 C9 C10 N2 0.7(10) . . . . ? C8 C9 C10 C11 -179.7(7) . . . . ? C15 N3 C11 C12 -0.6(10) . . . . ? Co1 N3 C11 C12 174.7(6) . . . . ? C15 N3 C11 C10 179.9(6) . . . . ? Co1 N3 C11 C10 -4.8(7) . . . . ? N2 C10 C11 N3 3.0(9) . . . . ? C9 C10 C11 N3 -176.7(7) . . . . ? N2 C10 C11 C12 -176.4(6) . . . . ? C9 C10 C11 C12 3.9(11) . . . . ? N3 C11 C12 C13 -0.6(11) . . . . ? C10 C11 C12 C13 178.8(7) . . . . ? C11 C12 C13 C14 0.7(12) . . . . ? C12 C13 C14 C15 0.3(13) . . . . ? C11 N3 C15 C14 1.7(11) . . . . ? Co1 N3 C15 C14 -173.0(6) . . . . ? C13 C14 C15 N3 -1.6(13) . . . . ? Co1 O1 C16 O2 -21.9(9) . . . . ? Co1 O1 C16 C17 153.7(4) . . . . ? O2 C16 C17 C18 109.0(7) . . . . ? O1 C16 C17 C18 -67.0(8) . . . . ? O2 C16 C17 C22 -66.6(9) . . . . ? O1 C16 C17 C22 117.4(7) . . . . ? C22 C17 C18 C19 0.8(10) . . . . ? C16 C17 C18 C19 -175.1(6) . . . . ? C17 C18 C19 C20 2.1(10) . . . . ? C17 C18 C19 S1 -178.6(5) . . . . ? O5 S1 C19 C20 -21.6(7) . . . . ? O6 S1 C19 C20 -153.3(6) . . . . ? C27 S1 C19 C20 92.6(6) . . . . ? O5 S1 C19 C18 159.1(5) . . . . ? O6 S1 C19 C18 27.4(7) . . . . ? C27 S1 C19 C18 -86.7(6) . . . . ? C18 C19 C20 C21 -3.2(11) . . . . ? S1 C19 C20 C21 177.5(6) . . . . ? C19 C20 C21 C22 1.3(12) . . . . ? C20 C21 C22 C17 1.6(12) . . . . ? C20 C21 C22 C23 -175.2(7) . . . . ? C18 C17 C22 C21 -2.6(10) . . . . ? C16 C17 C22 C21 172.9(6) . . . . ? C18 C17 C22 C23 173.9(7) . . . . ? C16 C17 C22 C23 -10.6(11) . . . . ? C21 C22 C23 O4 -23.8(14) . . . . ? C17 C22 C23 O4 159.5(11) . . . . ? C21 C22 C23 O3 151.8(7) . . . . ? C17 C22 C23 O3 -24.8(11) . . . . ? Co1 O9 C24 O10 -32.5(9) 1_556 . . . ? Co1 O9 C24 C25 143.9(4) 1_556 . . . ? O9 C24 C25 C26 -71.9(8) . . . . ? O10 C24 C25 C26 104.8(7) . . . . ? O9 C24 C25 C30 111.8(8) . . . . ? O10 C24 C25 C30 -71.5(8) . . . . ? C30 C25 C26 C27 0.2(10) . . . . ? C24 C25 C26 C27 -176.3(6) . . . . ? C25 C26 C27 C28 0.4(11) . . . . ? C25 C26 C27 S1 177.8(5) . . . . ? O5 S1 C27 C28 -159.1(6) . . . . ? O6 S1 C27 C28 -28.2(7) . . . . ? C19 S1 C27 C28 85.8(7) . . . . ? O5 S1 C27 C26 23.5(7) . . . . ? O6 S1 C27 C26 154.4(6) . . . . ? C19 S1 C27 C26 -91.7(6) . . . . ? C26 C27 C28 C29 -0.3(12) . . . . ? S1 C27 C28 C29 -177.7(6) . . . . ? C27 C28 C29 C30 -0.4(13) . . . . ? C26 C25 C30 C29 -0.9(11) . . . . ? C24 C25 C30 C29 175.3(7) . . . . ? C26 C25 C30 C31 176.6(6) . . . . ? C24 C25 C30 C31 -7.2(10) . . . . ? C28 C29 C30 C25 1.0(12) . . . . ? C28 C29 C30 C31 -176.5(8) . . . . ? C25 C30 C31 O8 -21.4(11) . . . . ? C29 C30 C31 O8 156.2(7) . . . . ? C25 C30 C31 O7 158.3(7) . . . . ? C29 C30 C31 O7 -24.1(10) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O11 H2W O2 0.83 2.21 2.771(7) 124.8 . O11 H1W O8 0.83 2.34 3.031(7) 140.5 2_677 O3 H3 O10 0.82 1.84 2.644(7) 165.9 2_777 _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 2.094 _refine_diff_density_min -0.608 _refine_diff_density_rms 0.143 # Attachment '2.cif' data_xb1617 _database_code_depnum_ccdc_archive 'CCDC 737214' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H34 Co2 N4 O16 S' _chemical_formula_weight 976.63 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' Co Co 0.3494 0.9721 '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' _cell_length_a 7.7399(9) _cell_length_b 14.1982(17) _cell_length_c 18.887(2) _cell_angle_alpha 92.863(2) _cell_angle_beta 100.801(2) _cell_angle_gamma 93.957(2) _cell_volume 2029.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 0.949 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7215 _exptl_absorpt_correction_T_max 0.9069 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 10333 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0756 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.05 _reflns_number_total 7064 _reflns_number_gt 4517 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _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^)+(0.0543P)^2^+0.1061P] 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 SHELXL _refine_ls_extinction_coef 0.0010(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7064 _refine_ls_number_parameters 605 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0878 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1342 _refine_ls_wR_factor_gt 0.1097 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.038 _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 Co1 Co 0.20689(7) -0.27710(4) 0.95253(3) 0.03409(19) Uani 1 1 d . . . Co2 Co 0.41330(7) 0.40769(4) 0.70234(3) 0.03356(19) Uani 1 1 d . . . S1 S 0.37032(16) -0.07888(8) 0.63931(6) 0.0406(3) Uani 1 1 d . . . N1 N 0.2392(5) -0.1273(3) 0.9770(2) 0.0447(10) Uani 1 1 d . . . N2 N 0.0869(5) -0.2628(3) 1.0429(2) 0.0411(10) Uani 1 1 d . . . N3 N 0.2602(5) 0.3177(3) 0.6130(2) 0.0384(9) Uani 1 1 d . . . N4 N 0.3825(5) 0.4997(3) 0.61556(19) 0.0376(9) Uani 1 1 d . . . O1 O 0.3417(4) -0.2744(2) 0.86741(16) 0.0445(8) Uani 1 1 d . . . O2 O 0.6194(4) -0.2960(2) 0.91842(16) 0.0473(9) Uani 1 1 d . . . O3 O 0.9822(4) -0.2511(2) 0.88013(16) 0.0388(8) Uani 1 1 d . . . O4 O 0.8614(4) -0.3920(2) 0.82883(17) 0.0467(8) Uani 1 1 d . . . O5 O 0.2047(4) -0.0788(2) 0.66396(18) 0.0509(9) Uani 1 1 d . . . O6 O 0.3703(5) -0.1091(2) 0.56539(16) 0.0543(9) Uani 1 1 d . . . O7 O 0.4444(4) 0.3180(2) 0.78497(16) 0.0439(8) Uani 1 1 d . . . O8 O 0.5201(4) 0.1985(2) 0.85203(16) 0.0435(8) Uani 1 1 d . . . O9 O 0.6638(4) 0.3883(2) 0.69129(17) 0.0437(8) Uani 1 1 d . . . O10 O 0.9010(4) 0.3137(2) 0.68198(19) 0.0538(9) Uani 1 1 d . . . O11 O 0.4386(4) -0.3083(2) 1.02510(17) 0.0448(8) Uani 1 1 d D . . O12 O 0.1418(5) -0.4257(2) 0.93349(19) 0.0464(8) Uani 1 1 d D . . O13 O 0.1750(4) 0.4391(2) 0.7296(2) 0.0484(9) Uani 1 1 d D . . O14 O 0.5192(4) 0.5237(2) 0.77826(17) 0.0435(8) Uani 1 1 d D . . O15 O 0.1282(5) 0.6251(3) 0.7420(2) 0.0631(10) Uani 1 1 d D . . O16 O 0.4500(10) 0.4856(4) 0.9131(4) 0.128(2) Uani 1 1 d D . . C1 C 0.5063(6) -0.2729(3) 0.8680(2) 0.0344(10) Uani 1 1 d . . . C2 C 0.5667(5) -0.2377(3) 0.8018(2) 0.0316(10) Uani 1 1 d . . . C3 C 0.4544(6) -0.1856(3) 0.7550(2) 0.0350(11) Uani 1 1 d . . . H3 H 0.3423 -0.1759 0.7635 0.042 Uiso 1 1 calc R . . C4 C 0.5089(6) -0.1486(3) 0.6963(2) 0.0343(10) Uani 1 1 d . . . C5 C 0.6759(6) -0.1632(3) 0.6824(2) 0.0428(12) Uani 1 1 d . . . H5 H 0.7123 -0.1386 0.6424 0.051 Uiso 1 1 calc R . . C6 C 0.7861(6) -0.2146(3) 0.7288(2) 0.0403(11) Uani 1 1 d . . . H6 H 0.8977 -0.2246 0.7197 0.048 Uiso 1 1 calc R . . C7 C 0.7342(5) -0.2518(3) 0.7887(2) 0.0314(10) Uani 1 1 d . . . C8 C 0.8677(6) -0.3037(3) 0.8382(2) 0.0345(11) Uani 1 1 d . . . C9 C 0.5028(5) 0.2380(3) 0.7946(2) 0.0332(10) Uani 1 1 d . . . C10 C 0.5436(5) 0.1822(3) 0.7295(2) 0.0309(10) Uani 1 1 d . . . C11 C 0.4674(5) 0.0889(3) 0.7171(2) 0.0351(11) Uani 1 1 d . . . H11 H 0.4081 0.0627 0.7508 0.042 Uiso 1 1 calc R . . C12 C 0.4798(6) 0.0358(3) 0.6555(2) 0.0380(11) Uani 1 1 d . . . C13 C 0.5732(6) 0.0713(3) 0.6070(3) 0.0468(13) Uani 1 1 d . . . H13 H 0.5791 0.0354 0.5651 0.056 Uiso 1 1 calc R . . C14 C 0.6584(6) 0.1602(3) 0.6203(2) 0.0407(11) Uani 1 1 d . . . H14 H 0.7277 0.1825 0.5885 0.049 Uiso 1 1 calc R . . C15 C 0.6434(5) 0.2174(3) 0.6802(2) 0.0323(10) Uani 1 1 d . . . C16 C 0.7436(6) 0.3149(3) 0.6868(2) 0.0346(11) Uani 1 1 d . . . C17 C 0.2991(6) -0.0604(4) 0.9395(3) 0.0602(16) Uani 1 1 d . . . H17 H 0.3383 -0.0777 0.8974 0.072 Uiso 1 1 calc R . . C18 C 0.3053(8) 0.0364(4) 0.9613(5) 0.081(2) Uani 1 1 d . . . H18 H 0.3463 0.0821 0.9336 0.097 Uiso 1 1 calc R . . C19 C 0.2512(8) 0.0621(5) 1.0231(5) 0.087(3) Uani 1 1 d . . . H19 H 0.2551 0.1258 1.0379 0.104 Uiso 1 1 calc R . . C20 C 0.1895(8) -0.0067(4) 1.0647(4) 0.0699(19) Uani 1 1 d . . . C21 C 0.1284(8) 0.0133(5) 1.1303(5) 0.088(3) Uani 1 1 d . . . H21 H 0.1370 0.0755 1.1492 0.106 Uiso 1 1 calc R . . C22 C 0.0592(9) -0.0551(6) 1.1654(4) 0.088(2) Uani 1 1 d . . . H22 H 0.0229 -0.0399 1.2085 0.105 Uiso 1 1 calc R . . C23 C 0.0407(7) -0.1511(5) 1.1369(3) 0.0617(16) Uani 1 1 d . . . C24 C -0.0403(9) -0.2257(6) 1.1680(3) 0.083(2) Uani 1 1 d . . . H24 H -0.0836 -0.2142 1.2101 0.100 Uiso 1 1 calc R . . C25 C -0.0552(10) -0.3132(6) 1.1371(4) 0.089(2) Uani 1 1 d . . . H25 H -0.1093 -0.3626 1.1577 0.107 Uiso 1 1 calc R . . C26 C 0.0099(7) -0.3310(4) 1.0743(3) 0.0594(15) Uani 1 1 d . . . H26 H -0.0010 -0.3926 1.0538 0.071 Uiso 1 1 calc R . . C27 C 0.1021(6) -0.1740(4) 1.0736(3) 0.0440(12) Uani 1 1 d . . . C28 C 0.1800(6) -0.1022(3) 1.0375(3) 0.0476(13) Uani 1 1 d . . . C29 C 0.1928(6) 0.2291(3) 0.6119(3) 0.0475(13) Uani 1 1 d . . . H29 H 0.2141 0.1980 0.6545 0.057 Uiso 1 1 calc R . . C30 C 0.0922(7) 0.1798(4) 0.5509(3) 0.0582(15) Uani 1 1 d . . . H30 H 0.0491 0.1174 0.5530 0.070 Uiso 1 1 calc R . . C31 C 0.0572(7) 0.2242(4) 0.4875(3) 0.0614(15) Uani 1 1 d . . . H31 H -0.0073 0.1921 0.4458 0.074 Uiso 1 1 calc R . . C32 C 0.1206(6) 0.3193(4) 0.4869(3) 0.0478(13) Uani 1 1 d . . . C33 C 0.0850(7) 0.3724(5) 0.4237(3) 0.0608(15) Uani 1 1 d . . . H33 H 0.0181 0.3434 0.3812 0.073 Uiso 1 1 calc R . . C34 C 0.1469(7) 0.4631(4) 0.4253(3) 0.0586(15) Uani 1 1 d . . . H34 H 0.1217 0.4961 0.3837 0.070 Uiso 1 1 calc R . . C35 C 0.2503(6) 0.5102(4) 0.4892(3) 0.0466(13) Uani 1 1 d . . . C36 C 0.3152(7) 0.6054(4) 0.4950(3) 0.0589(15) Uani 1 1 d . . . H36 H 0.2932 0.6417 0.4551 0.071 Uiso 1 1 calc R . . C37 C 0.4093(7) 0.6447(4) 0.5583(3) 0.0566(15) Uani 1 1 d . . . H37 H 0.4533 0.7078 0.5621 0.068 Uiso 1 1 calc R . . C38 C 0.4399(7) 0.5899(3) 0.6178(3) 0.0481(13) Uani 1 1 d . . . H38 H 0.5037 0.6181 0.6612 0.058 Uiso 1 1 calc R . . C39 C 0.2876(6) 0.4599(3) 0.5524(2) 0.0379(11) Uani 1 1 d . . . C40 C 0.2227(6) 0.3628(3) 0.5504(2) 0.0377(11) Uani 1 1 d . . . H11A H 0.466(7) -0.272(3) 1.0636(17) 0.080 Uiso 1 1 d D . . H11B H 0.519(5) -0.302(4) 1.000(3) 0.080 Uiso 1 1 d D . . H12B H 0.208(6) -0.466(3) 0.922(3) 0.080 Uiso 1 1 d D . . H12A H 0.063(5) -0.430(4) 0.8953(18) 0.080 Uiso 1 1 d D . . H13A H 0.166(7) 0.4981(10) 0.734(3) 0.080 Uiso 1 1 d D . . H13B H 0.080(4) 0.405(3) 0.712(3) 0.080 Uiso 1 1 d D . . H14B H 0.6292(19) 0.539(4) 0.787(3) 0.080 Uiso 1 1 d D . . H14A H 0.506(7) 0.507(4) 0.8195(14) 0.080 Uiso 1 1 d D . . H15A H 0.208(6) 0.655(3) 0.775(2) 0.080 Uiso 1 1 d D . . H15B H 0.044(5) 0.623(4) 0.766(3) 0.080 Uiso 1 1 d D . . H16A H 0.519(6) 0.461(4) 0.946(2) 0.080 Uiso 1 1 d D . . H16B H 0.400(9) 0.434(3) 0.892(4) 0.080 Uiso 1 1 d 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 Co1 0.0324(4) 0.0326(4) 0.0367(4) 0.0034(3) 0.0054(3) 0.0015(3) Co2 0.0352(4) 0.0309(4) 0.0333(4) 0.0028(3) 0.0042(3) -0.0001(3) S1 0.0478(7) 0.0310(7) 0.0386(7) 0.0040(5) -0.0014(5) -0.0021(5) N1 0.037(2) 0.036(2) 0.054(3) 0.008(2) -0.007(2) -0.0029(19) N2 0.046(2) 0.039(2) 0.039(2) 0.0035(19) 0.0077(18) 0.0078(19) N3 0.034(2) 0.039(2) 0.041(2) 0.0003(18) 0.0030(17) 0.0012(18) N4 0.042(2) 0.032(2) 0.038(2) 0.0018(17) 0.0037(18) 0.0023(18) O1 0.0319(18) 0.064(2) 0.0395(19) 0.0120(16) 0.0095(14) 0.0030(16) O2 0.0351(18) 0.070(2) 0.0377(19) 0.0140(17) 0.0048(15) 0.0107(17) O3 0.0324(17) 0.0324(18) 0.048(2) -0.0026(15) 0.0004(15) 0.0022(14) O4 0.045(2) 0.033(2) 0.057(2) -0.0033(16) 0.0010(16) 0.0027(15) O5 0.0396(19) 0.043(2) 0.067(2) 0.0105(17) 0.0022(17) -0.0025(16) O6 0.086(3) 0.036(2) 0.0325(19) -0.0047(15) -0.0042(17) -0.0026(18) O7 0.061(2) 0.034(2) 0.0400(19) 0.0075(15) 0.0144(16) 0.0119(16) O8 0.059(2) 0.042(2) 0.0308(18) 0.0098(15) 0.0099(15) 0.0096(16) O9 0.0399(19) 0.0309(19) 0.062(2) 0.0041(16) 0.0144(16) 0.0030(15) O10 0.0313(19) 0.050(2) 0.082(3) 0.0024(19) 0.0170(18) 0.0000(16) O11 0.046(2) 0.054(2) 0.034(2) 0.0010(16) 0.0091(16) 0.0006(17) O12 0.053(2) 0.036(2) 0.049(2) 0.0043(17) 0.0056(17) 0.0070(17) O13 0.038(2) 0.038(2) 0.068(2) 0.0048(19) 0.0104(17) -0.0032(17) O14 0.0436(19) 0.044(2) 0.0389(19) -0.0023(16) 0.0025(16) -0.0076(16) O15 0.062(3) 0.066(3) 0.056(3) -0.015(2) 0.0037(19) 0.009(2) O16 0.170(6) 0.142(5) 0.115(5) 0.080(4) 0.084(5) 0.107(5) C1 0.033(3) 0.029(3) 0.040(3) 0.002(2) 0.007(2) 0.000(2) C2 0.034(2) 0.025(2) 0.034(2) 0.0023(19) 0.0033(19) -0.0059(19) C3 0.032(2) 0.029(3) 0.044(3) 0.002(2) 0.008(2) 0.000(2) C4 0.040(3) 0.030(3) 0.032(3) 0.000(2) 0.004(2) 0.001(2) C5 0.046(3) 0.047(3) 0.036(3) 0.006(2) 0.011(2) -0.001(2) C6 0.036(3) 0.046(3) 0.043(3) 0.003(2) 0.017(2) 0.006(2) C7 0.032(2) 0.027(2) 0.033(2) -0.0026(19) 0.0045(19) -0.0012(19) C8 0.033(3) 0.035(3) 0.037(3) -0.002(2) 0.010(2) 0.002(2) C9 0.031(2) 0.032(3) 0.035(3) 0.001(2) 0.0049(19) -0.003(2) C10 0.032(2) 0.035(3) 0.024(2) 0.0070(19) -0.0003(18) 0.005(2) C11 0.034(3) 0.038(3) 0.033(3) 0.011(2) 0.006(2) 0.000(2) C12 0.045(3) 0.031(3) 0.036(3) 0.006(2) 0.003(2) 0.003(2) C13 0.061(3) 0.042(3) 0.038(3) 0.001(2) 0.013(2) 0.002(3) C14 0.053(3) 0.038(3) 0.035(3) -0.002(2) 0.019(2) 0.001(2) C15 0.036(3) 0.028(3) 0.032(2) 0.0038(19) 0.0052(19) 0.004(2) C16 0.037(3) 0.035(3) 0.030(2) 0.003(2) 0.007(2) -0.005(2) C17 0.044(3) 0.046(4) 0.083(4) 0.016(3) -0.008(3) -0.005(3) C18 0.055(4) 0.040(4) 0.132(7) 0.029(4) -0.025(4) -0.009(3) C19 0.055(4) 0.038(4) 0.143(7) -0.013(5) -0.039(4) 0.005(3) C20 0.054(4) 0.045(4) 0.095(5) -0.023(4) -0.022(3) 0.012(3) C21 0.054(4) 0.065(5) 0.123(7) -0.053(5) -0.030(4) 0.019(4) C22 0.074(5) 0.102(6) 0.074(5) -0.045(4) -0.013(4) 0.022(4) C23 0.055(4) 0.076(4) 0.048(3) -0.014(3) -0.006(3) 0.025(3) C24 0.099(5) 0.107(6) 0.051(4) -0.002(4) 0.023(4) 0.040(5) C25 0.117(6) 0.100(6) 0.068(5) 0.027(4) 0.051(4) 0.021(5) C26 0.079(4) 0.055(4) 0.048(3) 0.009(3) 0.022(3) 0.006(3) C27 0.040(3) 0.048(3) 0.041(3) -0.004(2) -0.002(2) 0.013(2) C28 0.039(3) 0.040(3) 0.055(3) -0.013(3) -0.011(2) 0.011(2) C29 0.036(3) 0.036(3) 0.065(4) 0.006(3) -0.004(2) -0.003(2) C30 0.051(3) 0.048(3) 0.070(4) -0.011(3) 0.008(3) -0.013(3) C31 0.048(3) 0.070(4) 0.060(4) -0.019(3) 0.004(3) -0.003(3) C32 0.038(3) 0.057(4) 0.045(3) -0.006(3) 0.004(2) -0.003(3) C33 0.052(3) 0.090(5) 0.036(3) -0.009(3) 0.003(2) 0.002(3) C34 0.061(4) 0.077(4) 0.036(3) 0.011(3) 0.001(3) 0.008(3) C35 0.050(3) 0.055(4) 0.036(3) 0.007(2) 0.007(2) 0.013(3) C36 0.072(4) 0.059(4) 0.052(4) 0.023(3) 0.018(3) 0.019(3) C37 0.083(4) 0.035(3) 0.058(4) 0.012(3) 0.028(3) 0.007(3) C38 0.068(4) 0.037(3) 0.040(3) -0.001(2) 0.013(2) 0.000(3) C39 0.035(3) 0.046(3) 0.032(3) 0.005(2) 0.003(2) 0.007(2) C40 0.031(2) 0.041(3) 0.040(3) 0.003(2) 0.004(2) 0.002(2) _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 Co1 O3 2.068(3) 1_455 ? Co1 O1 2.075(3) . ? Co1 N2 2.098(4) . ? Co1 O11 2.130(3) . ? Co1 O12 2.131(3) . ? Co1 N1 2.142(4) . ? Co2 O9 2.024(3) . ? Co2 O7 2.053(3) . ? Co2 O13 2.076(4) . ? Co2 N4 2.135(3) . ? Co2 O14 2.140(3) . ? Co2 N3 2.170(4) . ? S1 O6 1.440(3) . ? S1 O5 1.444(3) . ? S1 C4 1.764(4) . ? S1 C12 1.768(5) . ? N1 C17 1.322(6) . ? N1 C28 1.350(6) . ? N2 C26 1.326(6) . ? N2 C27 1.349(6) . ? N3 C29 1.326(5) . ? N3 C40 1.366(5) . ? N4 C38 1.323(5) . ? N4 C39 1.352(5) . ? O1 C1 1.270(5) . ? O2 C1 1.241(5) . ? O3 C8 1.247(5) . ? O3 Co1 2.068(3) 1_655 ? O4 C8 1.253(5) . ? O7 C9 1.260(5) . ? O8 C9 1.235(5) . ? O9 C16 1.255(5) . ? O10 C16 1.240(5) . ? O11 H11A 0.851(10) . ? O11 H11B 0.848(10) . ? O12 H12B 0.848(10) . ? O12 H12A 0.850(10) . ? O13 H13A 0.847(10) . ? O13 H13B 0.851(10) . ? O14 H14B 0.847(10) . ? O14 H14A 0.846(10) . ? O15 H15A 0.861(10) . ? O15 H15B 0.857(10) . ? O16 H16A 0.844(10) . ? O16 H16B 0.851(10) . ? C1 C2 1.509(6) . ? C2 C7 1.390(6) . ? C2 C3 1.398(6) . ? C3 C4 1.372(6) . ? C3 H3 0.9300 . ? C4 C5 1.393(6) . ? C5 C6 1.378(6) . ? C5 H5 0.9300 . ? C6 C7 1.387(6) . ? C6 H6 0.9300 . ? C7 C8 1.515(6) . ? C9 C10 1.525(6) . ? C10 C11 1.402(6) . ? C10 C15 1.406(6) . ? C11 C12 1.378(6) . ? C11 H11 0.9300 . ? C12 C13 1.363(6) . ? C13 C14 1.371(6) . ? C13 H13 0.9300 . ? C14 C15 1.388(6) . ? C14 H14 0.9300 . ? C15 C16 1.527(6) . ? C17 C18 1.410(8) . ? C17 H17 0.9300 . ? C18 C19 1.353(9) . ? C18 H18 0.9300 . ? C19 C20 1.397(9) . ? C19 H19 0.9300 . ? C20 C28 1.418(7) . ? C20 C21 1.430(9) . ? C21 C22 1.338(9) . ? C21 H21 0.9300 . ? C22 C23 1.428(8) . ? C22 H22 0.9300 . ? C23 C27 1.398(7) . ? C23 C24 1.403(8) . ? C24 C25 1.334(9) . ? C24 H24 0.9300 . ? C25 C26 1.391(8) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.417(7) . ? C29 C30 1.389(7) . ? C29 H29 0.9300 . ? C30 C31 1.372(7) . ? C30 H30 0.9300 . ? C31 C32 1.405(7) . ? C31 H31 0.9300 . ? C32 C40 1.395(6) . ? C32 C33 1.437(7) . ? C33 C34 1.340(7) . ? C33 H33 0.9300 . ? C34 C35 1.424(7) . ? C34 H34 0.9300 . ? C35 C36 1.402(7) . ? C35 C39 1.416(6) . ? C36 C37 1.349(7) . ? C36 H36 0.9300 . ? C37 C38 1.392(6) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C40 1.430(6) . ? 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 O3 Co1 O1 87.98(12) 1_455 . ? O3 Co1 N2 93.90(13) 1_455 . ? O1 Co1 N2 172.72(14) . . ? O3 Co1 O11 178.06(13) 1_455 . ? O1 Co1 O11 91.14(12) . . ? N2 Co1 O11 87.19(13) . . ? O3 Co1 O12 90.44(12) 1_455 . ? O1 Co1 O12 91.60(14) . . ? N2 Co1 O12 95.41(15) . . ? O11 Co1 O12 87.86(13) . . ? O3 Co1 N1 85.88(13) 1_455 . ? O1 Co1 N1 95.15(15) . . ? N2 Co1 N1 77.99(16) . . ? O11 Co1 N1 95.92(14) . . ? O12 Co1 N1 172.18(15) . . ? O9 Co2 O7 88.38(12) . . ? O9 Co2 O13 170.71(14) . . ? O7 Co2 O13 88.17(13) . . ? O9 Co2 N4 91.09(13) . . ? O7 Co2 N4 179.23(13) . . ? O13 Co2 N4 92.43(14) . . ? O9 Co2 O14 87.63(13) . . ? O7 Co2 O14 89.48(12) . . ? O13 Co2 O14 83.71(13) . . ? N4 Co2 O14 91.05(13) . . ? O9 Co2 N3 102.03(13) . . ? O7 Co2 N3 102.42(13) . . ? O13 Co2 N3 87.15(14) . . ? N4 Co2 N3 77.15(14) . . ? O14 Co2 N3 164.76(13) . . ? O6 S1 O5 119.2(2) . . ? O6 S1 C4 108.7(2) . . ? O5 S1 C4 107.7(2) . . ? O6 S1 C12 107.3(2) . . ? O5 S1 C12 109.1(2) . . ? C4 S1 C12 103.7(2) . . ? C17 N1 C28 119.1(5) . . ? C17 N1 Co1 128.7(4) . . ? C28 N1 Co1 112.1(3) . . ? C26 N2 C27 118.1(5) . . ? C26 N2 Co1 127.3(4) . . ? C27 N2 Co1 114.4(3) . . ? C29 N3 C40 117.0(4) . . ? C29 N3 Co2 129.7(3) . . ? C40 N3 Co2 113.3(3) . . ? C38 N4 C39 117.9(4) . . ? C38 N4 Co2 127.5(3) . . ? C39 N4 Co2 114.6(3) . . ? C1 O1 Co1 129.9(3) . . ? C8 O3 Co1 133.1(3) . 1_655 ? C9 O7 Co2 135.9(3) . . ? C16 O9 Co2 131.9(3) . . ? Co1 O11 H11A 115(4) . . ? Co1 O11 H11B 104(4) . . ? H11A O11 H11B 110(5) . . ? Co1 O12 H12B 126(4) . . ? Co1 O12 H12A 103(4) . . ? H12B O12 H12A 100(5) . . ? Co2 O13 H13A 112(4) . . ? Co2 O13 H13B 121(4) . . ? H13A O13 H13B 116(5) . . ? Co2 O14 H14B 120(4) . . ? Co2 O14 H14A 107(4) . . ? H14B O14 H14A 100(5) . . ? H15A O15 H15B 98(5) . . ? H16A O16 H16B 96(6) . . ? O2 C1 O1 125.5(4) . . ? O2 C1 C2 118.3(4) . . ? O1 C1 C2 116.2(4) . . ? C7 C2 C3 119.5(4) . . ? C7 C2 C1 121.5(4) . . ? C3 C2 C1 118.9(4) . . ? C4 C3 C2 120.3(4) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 120.5(4) . . ? C3 C4 S1 120.2(3) . . ? C5 C4 S1 119.3(3) . . ? C6 C5 C4 119.0(4) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C5 C6 C7 121.3(4) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C6 C7 C2 119.3(4) . . ? C6 C7 C8 117.4(4) . . ? C2 C7 C8 123.3(4) . . ? O3 C8 O4 127.2(4) . . ? O3 C8 C7 114.5(4) . . ? O4 C8 C7 118.0(4) . . ? O8 C9 O7 125.1(4) . . ? O8 C9 C10 116.9(4) . . ? O7 C9 C10 117.9(4) . . ? C11 C10 C15 118.3(4) . . ? C11 C10 C9 115.9(4) . . ? C15 C10 C9 125.7(4) . . ? C12 C11 C10 120.6(4) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C13 C12 C11 120.7(4) . . ? C13 C12 S1 120.3(4) . . ? C11 C12 S1 119.1(3) . . ? C12 C13 C14 119.8(5) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C13 C14 C15 121.3(4) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C14 C15 C10 119.1(4) . . ? C14 C15 C16 115.1(4) . . ? C10 C15 C16 125.8(4) . . ? O10 C16 O9 125.0(4) . . ? O10 C16 C15 114.5(4) . . ? O9 C16 C15 120.3(4) . . ? N1 C17 C18 122.0(6) . . ? N1 C17 H17 119.0 . . ? C18 C17 H17 119.0 . . ? C19 C18 C17 119.4(6) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 120.3(6) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C19 C20 C28 117.0(7) . . ? C19 C20 C21 124.5(7) . . ? C28 C20 C21 118.5(7) . . ? C22 C21 C20 121.9(7) . . ? C22 C21 H21 119.1 . . ? C20 C21 H21 119.1 . . ? C21 C22 C23 120.4(7) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C27 C23 C24 116.6(6) . . ? C27 C23 C22 119.6(6) . . ? C24 C23 C22 123.8(7) . . ? C25 C24 C23 119.9(6) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 120.3(6) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? N2 C26 C25 121.9(6) . . ? N2 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? N2 C27 C23 123.0(5) . . ? N2 C27 C28 116.8(5) . . ? C23 C27 C28 120.2(5) . . ? N1 C28 C27 118.4(4) . . ? N1 C28 C20 122.2(6) . . ? C27 C28 C20 119.4(6) . . ? N3 C29 C30 124.0(5) . . ? N3 C29 H29 118.0 . . ? C30 C29 H29 118.0 . . ? C31 C30 C29 119.2(5) . . ? C31 C30 H30 120.4 . . ? C29 C30 H30 120.4 . . ? C30 C31 C32 118.8(5) . . ? C30 C31 H31 120.6 . . ? C32 C31 H31 120.6 . . ? C40 C32 C31 118.1(5) . . ? C40 C32 C33 119.3(5) . . ? C31 C32 C33 122.6(5) . . ? C34 C33 C32 120.9(5) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C33 C34 C35 121.4(5) . . ? C33 C34 H34 119.3 . . ? C35 C34 H34 119.3 . . ? C36 C35 C39 116.5(5) . . ? C36 C35 C34 124.3(5) . . ? C39 C35 C34 119.1(5) . . ? C37 C36 C35 120.3(5) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C36 C37 C38 119.3(5) . . ? C36 C37 H37 120.3 . . ? C38 C37 H37 120.3 . . ? N4 C38 C37 123.2(5) . . ? N4 C38 H38 118.4 . . ? C37 C38 H38 118.4 . . ? N4 C39 C35 122.8(4) . . ? N4 C39 C40 117.9(4) . . ? C35 C39 C40 119.3(4) . . ? N3 C40 C32 122.9(4) . . ? N3 C40 C39 117.1(4) . . ? C32 C40 C39 120.0(4) . . ? 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 O3 Co1 N1 C17 -77.6(4) 1_455 . . . ? O1 Co1 N1 C17 10.0(4) . . . . ? N2 Co1 N1 C17 -172.5(4) . . . . ? O11 Co1 N1 C17 101.7(4) . . . . ? O12 Co1 N1 C17 -139.7(9) . . . . ? O3 Co1 N1 C28 98.9(3) 1_455 . . . ? O1 Co1 N1 C28 -173.6(3) . . . . ? N2 Co1 N1 C28 4.0(3) . . . . ? O11 Co1 N1 C28 -81.9(3) . . . . ? O12 Co1 N1 C28 36.7(11) . . . . ? O3 Co1 N2 C26 94.1(4) 1_455 . . . ? O1 Co1 N2 C26 -161.1(9) . . . . ? O11 Co1 N2 C26 -84.2(4) . . . . ? O12 Co1 N2 C26 3.3(4) . . . . ? N1 Co1 N2 C26 179.1(4) . . . . ? O3 Co1 N2 C27 -90.3(3) 1_455 . . . ? O1 Co1 N2 C27 14.5(12) . . . . ? O11 Co1 N2 C27 91.3(3) . . . . ? O12 Co1 N2 C27 178.9(3) . . . . ? N1 Co1 N2 C27 -5.3(3) . . . . ? O9 Co2 N3 C29 94.9(4) . . . . ? O7 Co2 N3 C29 3.9(4) . . . . ? O13 Co2 N3 C29 -83.6(4) . . . . ? N4 Co2 N3 C29 -176.8(4) . . . . ? O14 Co2 N3 C29 -136.8(5) . . . . ? O9 Co2 N3 C40 -88.8(3) . . . . ? O7 Co2 N3 C40 -179.8(3) . . . . ? O13 Co2 N3 C40 92.7(3) . . . . ? N4 Co2 N3 C40 -0.4(3) . . . . ? O14 Co2 N3 C40 39.6(7) . . . . ? O9 Co2 N4 C38 -79.6(4) . . . . ? O7 Co2 N4 C38 -126(10) . . . . ? O13 Co2 N4 C38 91.8(4) . . . . ? O14 Co2 N4 C38 8.1(4) . . . . ? N3 Co2 N4 C38 178.3(4) . . . . ? O9 Co2 N4 C39 102.9(3) . . . . ? O7 Co2 N4 C39 57(10) . . . . ? O13 Co2 N4 C39 -85.7(3) . . . . ? O14 Co2 N4 C39 -169.5(3) . . . . ? N3 Co2 N4 C39 0.8(3) . . . . ? O3 Co1 O1 C1 169.4(4) 1_455 . . . ? N2 Co1 O1 C1 64.2(12) . . . . ? O11 Co1 O1 C1 -12.4(4) . . . . ? O12 Co1 O1 C1 -100.3(4) . . . . ? N1 Co1 O1 C1 83.7(4) . . . . ? O9 Co2 O7 C9 -47.3(4) . . . . ? O13 Co2 O7 C9 141.3(4) . . . . ? N4 Co2 O7 C9 -1(11) . . . . ? O14 Co2 O7 C9 -135.0(4) . . . . ? N3 Co2 O7 C9 54.6(4) . . . . ? O7 Co2 O9 C16 48.7(4) . . . . ? O13 Co2 O9 C16 116.9(8) . . . . ? N4 Co2 O9 C16 -130.8(4) . . . . ? O14 Co2 O9 C16 138.2(4) . . . . ? N3 Co2 O9 C16 -53.7(4) . . . . ? Co1 O1 C1 O2 19.2(7) . . . . ? Co1 O1 C1 C2 -159.5(3) . . . . ? O2 C1 C2 C7 15.6(6) . . . . ? O1 C1 C2 C7 -165.7(4) . . . . ? O2 C1 C2 C3 -161.0(4) . . . . ? O1 C1 C2 C3 17.8(6) . . . . ? C7 C2 C3 C4 0.1(6) . . . . ? C1 C2 C3 C4 176.7(4) . . . . ? C2 C3 C4 C5 0.6(7) . . . . ? C2 C3 C4 S1 -177.5(3) . . . . ? O6 S1 C4 C3 -134.7(4) . . . . ? O5 S1 C4 C3 -4.3(4) . . . . ? C12 S1 C4 C3 111.3(4) . . . . ? O6 S1 C4 C5 47.2(4) . . . . ? O5 S1 C4 C5 177.6(3) . . . . ? C12 S1 C4 C5 -66.8(4) . . . . ? C3 C4 C5 C6 -0.6(7) . . . . ? S1 C4 C5 C6 177.5(4) . . . . ? C4 C5 C6 C7 -0.1(7) . . . . ? C5 C6 C7 C2 0.7(7) . . . . ? C5 C6 C7 C8 -177.4(4) . . . . ? C3 C2 C7 C6 -0.7(6) . . . . ? C1 C2 C7 C6 -177.3(4) . . . . ? C3 C2 C7 C8 177.3(4) . . . . ? C1 C2 C7 C8 0.8(6) . . . . ? Co1 O3 C8 O4 -0.5(7) 1_655 . . . ? Co1 O3 C8 C7 -173.9(3) 1_655 . . . ? C6 C7 C8 O3 78.5(5) . . . . ? C2 C7 C8 O3 -99.6(5) . . . . ? C6 C7 C8 O4 -95.6(5) . . . . ? C2 C7 C8 O4 86.3(5) . . . . ? Co2 O7 C9 O8 174.9(3) . . . . ? Co2 O7 C9 C10 -9.5(6) . . . . ? O8 C9 C10 C11 47.7(5) . . . . ? O7 C9 C10 C11 -128.1(4) . . . . ? O8 C9 C10 C15 -135.0(4) . . . . ? O7 C9 C10 C15 49.1(6) . . . . ? C15 C10 C11 C12 -4.6(6) . . . . ? C9 C10 C11 C12 172.9(4) . . . . ? C10 C11 C12 C13 3.1(7) . . . . ? C10 C11 C12 S1 -176.1(3) . . . . ? O6 S1 C12 C13 -12.2(4) . . . . ? O5 S1 C12 C13 -142.7(4) . . . . ? C4 S1 C12 C13 102.7(4) . . . . ? O6 S1 C12 C11 167.0(3) . . . . ? O5 S1 C12 C11 36.5(4) . . . . ? C4 S1 C12 C11 -78.1(4) . . . . ? C11 C12 C13 C14 1.2(7) . . . . ? S1 C12 C13 C14 -179.7(4) . . . . ? C12 C13 C14 C15 -3.8(7) . . . . ? C13 C14 C15 C10 2.2(7) . . . . ? C13 C14 C15 C16 -179.0(4) . . . . ? C11 C10 C15 C14 2.0(6) . . . . ? C9 C10 C15 C14 -175.2(4) . . . . ? C11 C10 C15 C16 -176.6(4) . . . . ? C9 C10 C15 C16 6.2(7) . . . . ? Co2 O9 C16 O10 -178.0(3) . . . . ? Co2 O9 C16 C15 7.5(6) . . . . ? C14 C15 C16 O10 -51.3(5) . . . . ? C10 C15 C16 O10 127.4(5) . . . . ? C14 C15 C16 O9 123.7(5) . . . . ? C10 C15 C16 O9 -57.6(6) . . . . ? C28 N1 C17 C18 0.9(7) . . . . ? Co1 N1 C17 C18 177.1(4) . . . . ? N1 C17 C18 C19 1.0(8) . . . . ? C17 C18 C19 C20 -0.1(9) . . . . ? C18 C19 C20 C28 -2.6(8) . . . . ? C18 C19 C20 C21 -179.6(6) . . . . ? C19 C20 C21 C22 175.2(6) . . . . ? C28 C20 C21 C22 -1.7(9) . . . . ? C20 C21 C22 C23 -1.4(10) . . . . ? C21 C22 C23 C27 2.6(9) . . . . ? C21 C22 C23 C24 -175.9(6) . . . . ? C27 C23 C24 C25 0.1(9) . . . . ? C22 C23 C24 C25 178.7(6) . . . . ? C23 C24 C25 C26 0.3(11) . . . . ? C27 N2 C26 C25 0.3(8) . . . . ? Co1 N2 C26 C25 175.7(4) . . . . ? C24 C25 C26 N2 -0.5(10) . . . . ? C26 N2 C27 C23 0.1(7) . . . . ? Co1 N2 C27 C23 -175.9(4) . . . . ? C26 N2 C27 C28 -178.1(4) . . . . ? Co1 N2 C27 C28 5.9(5) . . . . ? C24 C23 C27 N2 -0.3(7) . . . . ? C22 C23 C27 N2 -179.0(5) . . . . ? C24 C23 C27 C28 177.8(5) . . . . ? C22 C23 C27 C28 -0.9(7) . . . . ? C17 N1 C28 C27 174.6(4) . . . . ? Co1 N1 C28 C27 -2.2(5) . . . . ? C17 N1 C28 C20 -3.9(7) . . . . ? Co1 N1 C28 C20 179.3(4) . . . . ? N2 C27 C28 N1 -2.4(6) . . . . ? C23 C27 C28 N1 179.4(4) . . . . ? N2 C27 C28 C20 176.1(4) . . . . ? C23 C27 C28 C20 -2.1(7) . . . . ? C19 C20 C28 N1 4.7(7) . . . . ? C21 C20 C28 N1 -178.2(5) . . . . ? C19 C20 C28 C27 -173.8(5) . . . . ? C21 C20 C28 C27 3.4(7) . . . . ? C40 N3 C29 C30 1.9(7) . . . . ? Co2 N3 C29 C30 178.2(4) . . . . ? N3 C29 C30 C31 -0.7(8) . . . . ? C29 C30 C31 C32 -1.7(8) . . . . ? C30 C31 C32 C40 2.6(8) . . . . ? C30 C31 C32 C33 -177.8(5) . . . . ? C40 C32 C33 C34 -0.7(8) . . . . ? C31 C32 C33 C34 179.6(5) . . . . ? C32 C33 C34 C35 0.2(8) . . . . ? C33 C34 C35 C36 -178.3(5) . . . . ? C33 C34 C35 C39 -0.3(8) . . . . ? C39 C35 C36 C37 0.6(8) . . . . ? C34 C35 C36 C37 178.7(5) . . . . ? C35 C36 C37 C38 -0.6(8) . . . . ? C39 N4 C38 C37 -1.0(7) . . . . ? Co2 N4 C38 C37 -178.4(4) . . . . ? C36 C37 C38 N4 0.8(8) . . . . ? C38 N4 C39 C35 1.0(7) . . . . ? Co2 N4 C39 C35 178.8(4) . . . . ? C38 N4 C39 C40 -178.8(4) . . . . ? Co2 N4 C39 C40 -1.0(5) . . . . ? C36 C35 C39 N4 -0.8(7) . . . . ? C34 C35 C39 N4 -179.0(4) . . . . ? C36 C35 C39 C40 179.0(4) . . . . ? C34 C35 C39 C40 0.8(7) . . . . ? C29 N3 C40 C32 -0.8(7) . . . . ? Co2 N3 C40 C32 -177.7(4) . . . . ? C29 N3 C40 C39 176.9(4) . . . . ? Co2 N3 C40 C39 0.0(5) . . . . ? C31 C32 C40 N3 -1.4(7) . . . . ? C33 C32 C40 N3 179.0(4) . . . . ? C31 C32 C40 C39 -179.1(4) . . . . ? C33 C32 C40 C39 1.3(7) . . . . ? N4 C39 C40 N3 0.7(6) . . . . ? C35 C39 C40 N3 -179.2(4) . . . . ? N4 C39 C40 C32 178.5(4) . . . . ? C35 C39 C40 C32 -1.3(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O11 H11A O8 0.851(10) 1.844(15) 2.684(5) 169(6) 2_657 O12 H12A O4 0.850(10) 1.94(3) 2.735(4) 156(6) 1_455 O12 H12B O16 0.848(10) 2.07(3) 2.852(7) 154(5) 1_545 O13 H13B O10 0.851(10) 1.821(15) 2.660(4) 169(5) 1_455 O14 H14B O4 0.847(10) 1.99(2) 2.804(4) 161(6) 1_565 O15 H15A O1 0.861(10) 2.03(2) 2.871(5) 164(6) 1_565 O15 H15B O4 0.857(10) 2.019(13) 2.872(5) 174(6) 1_465 O16 H16A O11 0.844(10) 2.30(5) 2.944(6) 134(5) 2_657 O11 H11B O2 0.848(10) 1.86(2) 2.666(4) 158(5) . O13 H13A O15 0.847(10) 1.850(12) 2.695(5) 176(6) . O14 H14A O16 0.846(10) 1.931(15) 2.769(7) 171(6) . _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.406 _refine_diff_density_min -0.512 _refine_diff_density_rms 0.081 # Attachment '3.cif' data_aa _database_code_depnum_ccdc_archive 'CCDC 737215' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H32 Mn2 N4 O15 S' _chemical_formula_weight 950.64 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' Mn Mn 0.3368 0.7283 '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 7.3235(6) _cell_length_b 23.2694(18) _cell_length_c 23.6456(18) _cell_angle_alpha 90.00 _cell_angle_beta 98.4420(10) _cell_angle_gamma 90.00 _cell_volume 3985.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 6022 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 24.89 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 0.764 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7709 _exptl_absorpt_correction_T_max 0.9112 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29562 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7415 _reflns_number_gt 5766 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0543P)^2^+2.4262P] 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 CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7415 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.1129 _refine_ls_wR_factor_gt 0.1019 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 Mn1 Mn 1.01267(6) 0.380996(17) 0.031707(16) 0.02399(12) Uani 1 1 d . . . Mn2 Mn 0.68808(6) 0.730587(17) 0.290544(17) 0.02425(12) Uani 1 1 d . . . S1 S 1.05629(18) 0.45664(4) 0.36862(4) 0.0608(3) Uani 1 1 d . . . O1 O 1.2453(3) 0.32932(9) 0.04426(9) 0.0398(5) Uani 1 1 d . . . H1W H 1.3226 0.3373 0.0731 0.060 Uiso 1 1 d R . . H2W H 1.2234 0.2938 0.0443 0.060 Uiso 1 1 d R . . O2 O 0.7987(3) 0.44409(10) 0.01849(10) 0.0504(6) Uani 1 1 d . . . H3W H 0.7258 0.4460 0.0425 0.076 Uiso 1 1 d R . . H4W H 0.7920 0.4745 -0.0009 0.076 Uiso 1 1 d R . . O3 O 1.2119(3) 0.45360(9) 0.04439(9) 0.0403(5) Uani 1 1 d . . . H5W H 1.3237 0.4444 0.0515 0.060 Uiso 1 1 d R . . H6W H 1.1762 0.4634 0.0755 0.060 Uiso 1 1 d R . . O4 O 0.7707(3) 0.81968(9) 0.30393(9) 0.0449(6) Uani 1 1 d . . . H7W H 0.8773 0.8172 0.3222 0.067 Uiso 1 1 d R . . H8W H 0.6970 0.8303 0.3262 0.067 Uiso 1 1 d R . . O5 O 0.4134(3) 0.75951(9) 0.28673(9) 0.0417(5) Uani 1 1 d . . . H9W H 0.3420 0.7353 0.2987 0.063 Uiso 1 1 d R . . H10W H 0.4162 0.7886 0.3083 0.063 Uiso 1 1 d R . . O6 O 1.1002(3) 0.46890(10) 0.14277(10) 0.0521(6) Uani 1 1 d . . . O7 O 0.9641(3) 0.38507(8) 0.11584(8) 0.0336(5) Uani 1 1 d . . . O8 O 0.5032(3) 0.35432(10) 0.13730(10) 0.0483(6) Uani 1 1 d . . . O9 O 0.5790(3) 0.43916(9) 0.10323(9) 0.0427(5) Uani 1 1 d . . . O10 O 1.2487(4) 0.45828(12) 0.35873(12) 0.0736(9) Uani 1 1 d . . . O11 O 1.0009(6) 0.41924(11) 0.41115(11) 0.0906(12) Uani 1 1 d . . . O12 O 0.9650(3) 0.71541(10) 0.30585(11) 0.0481(6) Uani 1 1 d . . . O13 O 1.2310(3) 0.67024(10) 0.32282(11) 0.0519(6) Uani 1 1 d . . . O14 O 0.8242(3) 0.71504(10) 0.46465(9) 0.0465(6) Uani 1 1 d . . . O15 O 0.6848(4) 0.72036(11) 0.37575(9) 0.0524(6) Uani 1 1 d . . . N1 N 0.8494(4) 0.30514(11) 0.01872(11) 0.0368(6) Uani 1 1 d . . . N2 N 0.9802(4) 0.37242(11) -0.05846(11) 0.0367(6) Uani 1 1 d . . . N3 N 0.5918(3) 0.64883(11) 0.25858(11) 0.0343(6) Uani 1 1 d . . . N4 N 0.6914(3) 0.74053(11) 0.20131(11) 0.0363(6) Uani 1 1 d . . . C1 C 0.7804(5) 0.27341(15) 0.05724(15) 0.0444(8) Uani 1 1 d . . . H1A H 0.7857 0.2875 0.0942 0.053 Uiso 1 1 calc R . . C2 C 0.7001(5) 0.21958(16) 0.04428(18) 0.0563(10) Uani 1 1 d . . . H2A H 0.6499 0.1989 0.0720 0.068 Uiso 1 1 calc R . . C3 C 0.6960(5) 0.19762(16) -0.00963(18) 0.0582(10) Uani 1 1 d . . . H3A H 0.6478 0.1612 -0.0184 0.070 Uiso 1 1 calc R . . C4 C 0.7650(5) 0.23051(15) -0.05150(16) 0.0478(9) Uani 1 1 d . . . C5 C 0.7530(5) 0.21326(18) -0.10992(17) 0.0583(11) Uani 1 1 d . . . H5A H 0.7096 0.1767 -0.1206 0.070 Uiso 1 1 calc R . . C6 C 0.8035(5) 0.24904(19) -0.15000(17) 0.0575(10) Uani 1 1 d . . . H6 H 0.7900 0.2373 -0.1880 0.069 Uiso 1 1 calc R . . C7 C 0.8775(5) 0.30482(16) -0.13454(14) 0.0456(9) Uani 1 1 d . . . C8 C 0.9275(5) 0.34463(19) -0.17428(15) 0.0561(10) Uani 1 1 d . . . H8 H 0.9126 0.3355 -0.2130 0.067 Uiso 1 1 calc R . . C9 C 0.9976(5) 0.39642(18) -0.15580(15) 0.0532(10) Uani 1 1 d . . . H9 H 1.0271 0.4235 -0.1819 0.064 Uiso 1 1 calc R . . C10 C 1.0253(5) 0.40879(15) -0.09729(14) 0.0448(8) Uani 1 1 d . . . H10 H 1.0775 0.4439 -0.0851 0.054 Uiso 1 1 calc R . . C11 C 0.9029(4) 0.32123(14) -0.07728(13) 0.0367(7) Uani 1 1 d . . . C12 C 0.8395(4) 0.28442(13) -0.03546(13) 0.0372(7) Uani 1 1 d . . . C13 C 0.5398(4) 0.60414(14) 0.28741(15) 0.0404(8) Uani 1 1 d . . . H13 H 0.5480 0.6069 0.3269 0.048 Uiso 1 1 calc R . . C14 C 0.4736(5) 0.55350(14) 0.26087(16) 0.0473(8) Uani 1 1 d . . . H14 H 0.4392 0.5231 0.2825 0.057 Uiso 1 1 calc R . . C15 C 0.4595(5) 0.54865(14) 0.20305(16) 0.0480(9) Uani 1 1 d . . . H15 H 0.4155 0.5148 0.1850 0.058 Uiso 1 1 calc R . . C16 C 0.5116(4) 0.59492(14) 0.17058(14) 0.0405(8) Uani 1 1 d . . . C17 C 0.4989(5) 0.59440(17) 0.10957(15) 0.0491(9) Uani 1 1 d . . . H17 H 0.4538 0.5619 0.0893 0.059 Uiso 1 1 calc R . . C18 C 0.5513(5) 0.64022(16) 0.08095(15) 0.0494(9) Uani 1 1 d . . . H18 H 0.5422 0.6387 0.0413 0.059 Uiso 1 1 calc R . . C19 C 0.6206(4) 0.69127(15) 0.11048(13) 0.0411(8) Uani 1 1 d . . . C20 C 0.6783(5) 0.73987(16) 0.08304(15) 0.0487(9) Uani 1 1 d . . . H20 H 0.6741 0.7401 0.0435 0.058 Uiso 1 1 calc R . . C21 C 0.7405(5) 0.78687(16) 0.11453(15) 0.0500(9) Uani 1 1 d . . . H21 H 0.7805 0.8192 0.0968 0.060 Uiso 1 1 calc R . . C22 C 0.7435(5) 0.78586(15) 0.17339(15) 0.0457(8) Uani 1 1 d . . . H22 H 0.7839 0.8185 0.1943 0.055 Uiso 1 1 calc R . . C23 C 0.6312(4) 0.69357(13) 0.16997(13) 0.0329(7) Uani 1 1 d . . . C24 C 0.5775(4) 0.64450(13) 0.20059(13) 0.0333(7) Uani 1 1 d . . . C25 C 0.9945(4) 0.42826(13) 0.14906(12) 0.0328(7) Uani 1 1 d . . . C26 C 0.8965(4) 0.42871(12) 0.20024(12) 0.0339(7) Uani 1 1 d . . . C27 C 0.7115(4) 0.41286(12) 0.19738(13) 0.0352(7) Uani 1 1 d . . . C28 C 0.6329(5) 0.41015(14) 0.24769(14) 0.0458(8) Uani 1 1 d . . . H28 H 0.5103 0.3990 0.2461 0.055 Uiso 1 1 calc R . . C29 C 0.7356(6) 0.42397(14) 0.30005(14) 0.0520(10) Uani 1 1 d . . . H29 H 0.6822 0.4225 0.3334 0.062 Uiso 1 1 calc R . . C30 C 0.9194(6) 0.44005(14) 0.30205(14) 0.0451(8) Uani 1 1 d . . . C31 C 0.9994(5) 0.44274(13) 0.25302(13) 0.0407(8) Uani 1 1 d . . . H31 H 1.1221 0.4539 0.2550 0.049 Uiso 1 1 calc R . . C32 C 0.5907(4) 0.40107(13) 0.14119(13) 0.0355(7) Uani 1 1 d . . . C33 C 0.9857(6) 0.52726(14) 0.38339(14) 0.0483(9) Uani 1 1 d . . . C34 C 0.8744(6) 0.53662(15) 0.42530(16) 0.0589(11) Uani 1 1 d . . . H34 H 0.8361 0.5060 0.4459 0.071 Uiso 1 1 calc R . . C35 C 0.8216(6) 0.59213(15) 0.43582(15) 0.0521(9) Uani 1 1 d . . . H35 H 0.7522 0.5989 0.4651 0.062 Uiso 1 1 calc R . . C36 C 0.8706(4) 0.63819(13) 0.40336(12) 0.0358(7) Uani 1 1 d . . . C37 C 0.9860(4) 0.62845(13) 0.36198(12) 0.0338(7) Uani 1 1 d . . . C38 C 1.0450(5) 0.57255(13) 0.35330(13) 0.0410(8) Uani 1 1 d . . . H38 H 1.1252 0.5658 0.3269 0.049 Uiso 1 1 calc R . . C39 C 1.0650(4) 0.67513(13) 0.32795(13) 0.0350(7) Uani 1 1 d . . . C40 C 0.7907(4) 0.69607(13) 0.41556(13) 0.0345(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0305(2) 0.0222(2) 0.0188(2) 0.00002(16) 0.00206(17) 0.00180(17) Mn2 0.0271(2) 0.0219(2) 0.0237(2) -0.00385(17) 0.00339(17) -0.00208(17) S1 0.1151(9) 0.0319(5) 0.0301(5) -0.0042(4) -0.0076(5) 0.0128(5) O1 0.0466(13) 0.0326(12) 0.0383(12) 0.0004(9) 0.0004(10) 0.0020(10) O2 0.0578(15) 0.0503(14) 0.0461(14) 0.0164(11) 0.0178(12) 0.0195(12) O3 0.0415(13) 0.0369(12) 0.0432(13) 0.0043(10) 0.0090(10) 0.0008(10) O4 0.0443(13) 0.0404(13) 0.0486(14) -0.0079(11) 0.0020(11) -0.0033(10) O5 0.0399(13) 0.0424(13) 0.0422(13) -0.0044(10) 0.0042(10) -0.0044(10) O6 0.0611(16) 0.0492(14) 0.0480(14) -0.0119(11) 0.0148(12) -0.0234(12) O7 0.0430(12) 0.0287(11) 0.0288(11) -0.0030(9) 0.0041(9) -0.0010(9) O8 0.0531(15) 0.0428(14) 0.0471(14) 0.0062(11) 0.0013(11) -0.0130(11) O9 0.0421(13) 0.0423(13) 0.0440(13) 0.0111(11) 0.0075(10) 0.0026(10) O10 0.077(2) 0.0706(19) 0.0657(19) -0.0195(15) -0.0150(15) 0.0301(16) O11 0.197(4) 0.0355(15) 0.0346(15) 0.0057(12) 0.0013(18) 0.0086(19) O12 0.0382(13) 0.0437(14) 0.0628(16) 0.0146(12) 0.0086(11) 0.0021(11) O13 0.0380(14) 0.0538(15) 0.0665(17) 0.0070(12) 0.0157(12) 0.0055(11) O14 0.0642(16) 0.0423(13) 0.0317(12) -0.0081(10) 0.0029(11) 0.0036(11) O15 0.0641(16) 0.0600(16) 0.0324(13) -0.0050(11) 0.0050(11) 0.0222(13) N1 0.0389(15) 0.0386(15) 0.0312(14) -0.0010(12) -0.0006(11) 0.0035(12) N2 0.0389(15) 0.0401(15) 0.0307(14) 0.0008(12) 0.0038(11) 0.0097(12) N3 0.0344(14) 0.0329(14) 0.0363(14) -0.0022(11) 0.0070(11) -0.0007(11) N4 0.0368(15) 0.0359(15) 0.0365(15) -0.0013(12) 0.0059(12) -0.0011(11) C1 0.046(2) 0.045(2) 0.0421(19) 0.0048(16) 0.0050(15) -0.0050(16) C2 0.051(2) 0.052(2) 0.063(3) 0.0128(19) -0.0020(19) -0.0106(18) C3 0.057(2) 0.041(2) 0.071(3) -0.0012(19) -0.009(2) -0.0108(18) C4 0.043(2) 0.044(2) 0.051(2) -0.0117(17) -0.0099(16) 0.0038(16) C5 0.053(2) 0.054(2) 0.061(3) -0.024(2) -0.010(2) 0.0050(19) C6 0.052(2) 0.073(3) 0.044(2) -0.027(2) -0.0053(18) 0.014(2) C7 0.0408(19) 0.062(2) 0.0322(18) -0.0099(16) -0.0015(14) 0.0157(17) C8 0.053(2) 0.086(3) 0.0283(18) -0.0049(19) 0.0019(16) 0.025(2) C9 0.054(2) 0.070(3) 0.0366(19) 0.0135(18) 0.0115(17) 0.018(2) C10 0.048(2) 0.048(2) 0.0387(19) 0.0099(16) 0.0096(16) 0.0130(16) C11 0.0344(17) 0.0418(18) 0.0317(16) -0.0058(14) -0.0024(13) 0.0115(14) C12 0.0347(17) 0.0383(18) 0.0360(17) -0.0032(14) -0.0033(14) 0.0077(14) C13 0.0410(19) 0.0360(18) 0.0452(19) -0.0008(15) 0.0097(15) -0.0017(14) C14 0.047(2) 0.0340(18) 0.059(2) -0.0001(16) 0.0026(17) -0.0030(15) C15 0.0402(19) 0.0340(18) 0.067(3) -0.0132(17) -0.0013(17) -0.0033(15) C16 0.0346(17) 0.0375(18) 0.048(2) -0.0112(15) 0.0004(15) 0.0024(14) C17 0.045(2) 0.056(2) 0.043(2) -0.0196(18) -0.0036(16) 0.0048(17) C18 0.047(2) 0.063(2) 0.0358(18) -0.0143(18) -0.0016(16) 0.0112(18) C19 0.0364(18) 0.054(2) 0.0324(17) -0.0044(15) 0.0041(14) 0.0095(15) C20 0.046(2) 0.067(2) 0.0352(18) 0.0068(18) 0.0106(16) 0.0141(18) C21 0.052(2) 0.052(2) 0.048(2) 0.0136(18) 0.0140(17) 0.0023(18) C22 0.053(2) 0.043(2) 0.0428(19) 0.0045(16) 0.0099(16) -0.0019(16) C23 0.0296(16) 0.0345(17) 0.0342(16) -0.0044(13) 0.0036(13) 0.0041(13) C24 0.0278(15) 0.0360(17) 0.0354(17) -0.0079(13) 0.0020(13) 0.0039(13) C25 0.0346(17) 0.0313(16) 0.0313(16) -0.0020(13) 0.0004(13) -0.0006(13) C26 0.0476(19) 0.0238(15) 0.0308(16) -0.0023(12) 0.0067(14) 0.0000(13) C27 0.0466(19) 0.0262(16) 0.0340(17) 0.0003(13) 0.0094(14) 0.0013(13) C28 0.058(2) 0.0393(19) 0.044(2) -0.0021(15) 0.0196(17) -0.0024(16) C29 0.089(3) 0.0381(19) 0.0330(18) 0.0002(15) 0.0230(19) 0.0026(19) C30 0.075(3) 0.0268(16) 0.0324(18) -0.0031(14) 0.0040(17) 0.0027(16) C31 0.055(2) 0.0324(17) 0.0333(17) -0.0070(14) 0.0009(15) -0.0003(15) C32 0.0360(17) 0.0331(17) 0.0386(18) 0.0011(14) 0.0099(14) 0.0011(14) C33 0.084(3) 0.0303(17) 0.0285(17) -0.0058(14) 0.0003(17) 0.0011(17) C34 0.103(3) 0.0340(19) 0.042(2) 0.0004(16) 0.018(2) -0.010(2) C35 0.080(3) 0.041(2) 0.0390(19) -0.0011(16) 0.0206(18) -0.0039(18) C36 0.0487(19) 0.0308(16) 0.0274(16) -0.0029(13) 0.0035(14) -0.0028(14) C37 0.0402(17) 0.0322(16) 0.0285(16) -0.0034(13) 0.0031(13) -0.0009(13) C38 0.057(2) 0.0368(18) 0.0298(16) -0.0028(14) 0.0075(15) 0.0042(15) C39 0.0365(18) 0.0351(17) 0.0335(17) -0.0089(14) 0.0055(14) 0.0000(14) C40 0.0372(17) 0.0379(17) 0.0293(16) -0.0012(14) 0.0079(14) -0.0046(14) _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 O1 2.071(2) . ? Mn1 O7 2.074(2) . ? Mn1 N2 2.120(3) . ? Mn1 N1 2.129(3) . ? Mn1 O2 2.137(2) . ? Mn1 O3 2.224(2) . ? Mn2 O15 2.032(2) . ? Mn2 O12 2.038(2) . ? Mn2 O5 2.110(2) . ? Mn2 N4 2.126(3) . ? Mn2 N3 2.129(2) . ? Mn2 O4 2.170(2) . ? S1 O11 1.433(3) . ? S1 O10 1.462(3) . ? S1 C33 1.773(3) . ? S1 C30 1.780(3) . ? O1 H1W 0.8409 . ? O1 H2W 0.8411 . ? O2 H3W 0.8354 . ? O2 H4W 0.8412 . ? O3 H5W 0.8392 . ? O3 H6W 0.8484 . ? O4 H7W 0.8366 . ? O4 H8W 0.8455 . ? O5 H9W 0.8453 . ? O5 H10W 0.8470 . ? O6 C25 1.245(4) . ? O7 C25 1.275(3) . ? O8 C32 1.259(4) . ? O9 C32 1.255(4) . ? O12 C39 1.255(4) . ? O13 C39 1.244(4) . ? O14 C40 1.232(3) . ? O15 C40 1.262(4) . ? N1 C1 1.329(4) . ? N1 C12 1.361(4) . ? N2 C10 1.326(4) . ? N2 C11 1.365(4) . ? N3 C13 1.329(4) . ? N3 C24 1.363(4) . ? N4 C22 1.330(4) . ? N4 C23 1.357(4) . ? C1 C2 1.399(5) . ? C1 H1A 0.9300 . ? C2 C3 1.370(5) . ? C2 H2A 0.9300 . ? C3 C4 1.403(5) . ? C3 H3A 0.9300 . ? C4 C12 1.398(5) . ? C4 C5 1.429(5) . ? C5 C6 1.353(6) . ? C5 H5A 0.9300 . ? C6 C7 1.433(5) . ? C6 H6 0.9300 . ? C7 C11 1.393(4) . ? C7 C8 1.406(5) . ? C8 C9 1.357(5) . ? C8 H8 0.9300 . ? C9 C10 1.398(5) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.436(5) . ? C13 C14 1.388(5) . ? C13 H13 0.9300 . ? C14 C15 1.361(5) . ? C14 H14 0.9300 . ? C15 C16 1.407(5) . ? C15 H15 0.9300 . ? C16 C24 1.402(4) . ? C16 C17 1.432(5) . ? C17 C18 1.348(5) . ? C17 H17 0.9300 . ? C18 C19 1.433(5) . ? C18 H18 0.9300 . ? C19 C23 1.398(4) . ? C19 C20 1.400(5) . ? C20 C21 1.363(5) . ? C20 H20 0.9300 . ? C21 C22 1.389(5) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.437(4) . ? C25 C26 1.495(4) . ? C26 C27 1.397(4) . ? C26 C31 1.398(4) . ? C27 C28 1.397(4) . ? C27 C32 1.509(4) . ? C28 C29 1.389(5) . ? C28 H28 0.9300 . ? C29 C30 1.391(5) . ? C29 H29 0.9300 . ? C30 C31 1.375(5) . ? C31 H31 0.9300 . ? C33 C38 1.377(5) . ? C33 C34 1.390(5) . ? C34 C35 1.381(5) . ? C34 H34 0.9300 . ? C35 C36 1.396(4) . ? C35 H35 0.9300 . ? C36 C37 1.402(4) . ? C36 C40 1.513(4) . ? C37 C38 1.395(4) . ? C37 C39 1.516(4) . ? C38 H38 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 O1 Mn1 O7 98.19(8) . . ? O1 Mn1 N2 93.32(9) . . ? O7 Mn1 N2 163.62(9) . . ? O1 Mn1 N1 88.39(9) . . ? O7 Mn1 N1 90.25(9) . . ? N2 Mn1 N1 78.42(10) . . ? O1 Mn1 O2 172.02(9) . . ? O7 Mn1 O2 83.30(8) . . ? N2 Mn1 O2 86.91(9) . . ? N1 Mn1 O2 99.46(10) . . ? O1 Mn1 O3 84.96(8) . . ? O7 Mn1 O3 92.15(8) . . ? N2 Mn1 O3 100.47(9) . . ? N1 Mn1 O3 173.19(9) . . ? O2 Mn1 O3 87.15(9) . . ? O15 Mn2 O12 87.70(10) . . ? O15 Mn2 O5 85.98(9) . . ? O12 Mn2 O5 168.60(9) . . ? O15 Mn2 N4 179.52(10) . . ? O12 Mn2 N4 92.23(10) . . ? O5 Mn2 N4 94.17(9) . . ? O15 Mn2 N3 101.30(10) . . ? O12 Mn2 N3 100.21(10) . . ? O5 Mn2 N3 90.34(9) . . ? N4 Mn2 N3 78.25(10) . . ? O15 Mn2 O4 90.62(10) . . ? O12 Mn2 O4 83.72(9) . . ? O5 Mn2 O4 86.86(9) . . ? N4 Mn2 O4 89.84(9) . . ? N3 Mn2 O4 167.55(9) . . ? O11 S1 O10 120.4(2) . . ? O11 S1 C33 107.71(17) . . ? O10 S1 C33 108.84(18) . . ? O11 S1 C30 107.96(19) . . ? O10 S1 C30 107.15(17) . . ? C33 S1 C30 103.45(16) . . ? Mn1 O1 H1W 115.4 . . ? Mn1 O1 H2W 114.7 . . ? H1W O1 H2W 108.8 . . ? Mn1 O2 H3W 117.7 . . ? Mn1 O2 H4W 129.9 . . ? H3W O2 H4W 109.5 . . ? Mn1 O3 H5W 115.7 . . ? Mn1 O3 H6W 92.4 . . ? H5W O3 H6W 108.2 . . ? Mn2 O4 H7W 103.2 . . ? Mn2 O4 H8W 100.4 . . ? H7W O4 H8W 109.3 . . ? Mn2 O5 H9W 114.0 . . ? Mn2 O5 H10W 106.9 . . ? H9W O5 H10W 106.9 . . ? C25 O7 Mn1 126.01(19) . . ? C39 O12 Mn2 135.0(2) . . ? C40 O15 Mn2 134.1(2) . . ? C1 N1 C12 118.4(3) . . ? C1 N1 Mn1 128.6(2) . . ? C12 N1 Mn1 112.4(2) . . ? C10 N2 C11 117.7(3) . . ? C10 N2 Mn1 129.3(2) . . ? C11 N2 Mn1 112.9(2) . . ? C13 N3 C24 118.2(3) . . ? C13 N3 Mn2 128.5(2) . . ? C24 N3 Mn2 113.31(19) . . ? C22 N4 C23 117.5(3) . . ? C22 N4 Mn2 128.7(2) . . ? C23 N4 Mn2 113.8(2) . . ? N1 C1 C2 122.5(3) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C3 C2 C1 119.3(4) . . ? C3 C2 H2A 120.4 . . ? C1 C2 H2A 120.4 . . ? C2 C3 C4 119.5(3) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C12 C4 C3 117.7(3) . . ? C12 C4 C5 118.7(4) . . ? C3 C4 C5 123.5(4) . . ? C6 C5 C4 121.3(4) . . ? C6 C5 H5A 119.3 . . ? C4 C5 H5A 119.3 . . ? C5 C6 C7 120.7(3) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C11 C7 C8 117.3(3) . . ? C11 C7 C6 119.2(3) . . ? C8 C7 C6 123.5(3) . . ? C9 C8 C7 119.6(3) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 119.6(4) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? N2 C10 C9 122.6(4) . . ? N2 C10 H10 118.7 . . ? C9 C10 H10 118.7 . . ? N2 C11 C7 123.1(3) . . ? N2 C11 C12 117.2(3) . . ? C7 C11 C12 119.7(3) . . ? N1 C12 C4 122.6(3) . . ? N1 C12 C11 117.3(3) . . ? C4 C12 C11 120.1(3) . . ? N3 C13 C14 122.6(3) . . ? N3 C13 H13 118.7 . . ? C14 C13 H13 118.7 . . ? C15 C14 C13 119.6(3) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 119.9(3) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C24 C16 C15 117.0(3) . . ? C24 C16 C17 118.9(3) . . ? C15 C16 C17 124.1(3) . . ? C18 C17 C16 121.2(3) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C19 121.2(3) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C23 C19 C20 117.4(3) . . ? C23 C19 C18 119.0(3) . . ? C20 C19 C18 123.6(3) . . ? C21 C20 C19 119.6(3) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 C22 119.2(3) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? N4 C22 C21 123.2(3) . . ? N4 C22 H22 118.4 . . ? C21 C22 H22 118.4 . . ? N4 C23 C19 123.1(3) . . ? N4 C23 C24 117.1(3) . . ? C19 C23 C24 119.8(3) . . ? N3 C24 C16 122.7(3) . . ? N3 C24 C23 117.5(3) . . ? C16 C24 C23 119.9(3) . . ? O6 C25 O7 125.5(3) . . ? O6 C25 C26 118.2(3) . . ? O7 C25 C26 116.3(3) . . ? C27 C26 C31 119.8(3) . . ? C27 C26 C25 122.4(3) . . ? C31 C26 C25 117.7(3) . . ? C26 C27 C28 119.3(3) . . ? C26 C27 C32 122.0(3) . . ? C28 C27 C32 118.7(3) . . ? C29 C28 C27 120.8(3) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C30 119.2(3) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? C31 C30 C29 120.9(3) . . ? C31 C30 S1 118.8(3) . . ? C29 C30 S1 120.3(3) . . ? C30 C31 C26 120.1(3) . . ? C30 C31 H31 119.9 . . ? C26 C31 H31 119.9 . . ? O9 C32 O8 125.3(3) . . ? O9 C32 C27 118.1(3) . . ? O8 C32 C27 116.6(3) . . ? C38 C33 C34 120.7(3) . . ? C38 C33 S1 119.0(3) . . ? C34 C33 S1 120.3(3) . . ? C35 C34 C33 119.0(3) . . ? C35 C34 H34 120.5 . . ? C33 C34 H34 120.5 . . ? C34 C35 C36 121.2(3) . . ? C34 C35 H35 119.4 . . ? C36 C35 H35 119.4 . . ? C35 C36 C37 119.3(3) . . ? C35 C36 C40 116.2(3) . . ? C37 C36 C40 124.5(3) . . ? C38 C37 C36 119.0(3) . . ? C38 C37 C39 116.1(3) . . ? C36 C37 C39 124.8(3) . . ? C33 C38 C37 120.6(3) . . ? C33 C38 H38 119.7 . . ? C37 C38 H38 119.7 . . ? O13 C39 O12 123.1(3) . . ? O13 C39 C37 116.1(3) . . ? O12 C39 C37 120.8(3) . . ? O14 C40 O15 123.9(3) . . ? O14 C40 C36 118.0(3) . . ? O15 C40 C36 118.0(3) . . ? 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 O1 Mn1 O7 C25 106.0(2) . . . . ? N2 Mn1 O7 C25 -119.8(4) . . . . ? N1 Mn1 O7 C25 -165.6(2) . . . . ? O2 Mn1 O7 C25 -66.1(2) . . . . ? O3 Mn1 O7 C25 20.7(2) . . . . ? O15 Mn2 O12 C39 57.4(3) . . . . ? O5 Mn2 O12 C39 113.7(5) . . . . ? N4 Mn2 O12 C39 -122.2(3) . . . . ? N3 Mn2 O12 C39 -43.7(3) . . . . ? O4 Mn2 O12 C39 148.2(3) . . . . ? O12 Mn2 O15 C40 -21.2(3) . . . . ? O5 Mn2 O15 C40 168.3(3) . . . . ? N4 Mn2 O15 C40 60(12) . . . . ? N3 Mn2 O15 C40 78.8(3) . . . . ? O4 Mn2 O15 C40 -104.8(3) . . . . ? O1 Mn1 N1 C1 88.9(3) . . . . ? O7 Mn1 N1 C1 -9.3(3) . . . . ? N2 Mn1 N1 C1 -177.4(3) . . . . ? O2 Mn1 N1 C1 -92.6(3) . . . . ? O3 Mn1 N1 C1 101.3(8) . . . . ? O1 Mn1 N1 C12 -81.9(2) . . . . ? O7 Mn1 N1 C12 180.0(2) . . . . ? N2 Mn1 N1 C12 11.9(2) . . . . ? O2 Mn1 N1 C12 96.7(2) . . . . ? O3 Mn1 N1 C12 -69.4(8) . . . . ? O1 Mn1 N2 C10 -101.2(3) . . . . ? O7 Mn1 N2 C10 124.1(3) . . . . ? N1 Mn1 N2 C10 171.1(3) . . . . ? O2 Mn1 N2 C10 70.8(3) . . . . ? O3 Mn1 N2 C10 -15.7(3) . . . . ? O1 Mn1 N2 C11 78.1(2) . . . . ? O7 Mn1 N2 C11 -56.6(4) . . . . ? N1 Mn1 N2 C11 -9.6(2) . . . . ? O2 Mn1 N2 C11 -109.9(2) . . . . ? O3 Mn1 N2 C11 163.6(2) . . . . ? O15 Mn2 N3 C13 1.5(3) . . . . ? O12 Mn2 N3 C13 91.2(3) . . . . ? O5 Mn2 N3 C13 -84.5(3) . . . . ? N4 Mn2 N3 C13 -178.6(3) . . . . ? O4 Mn2 N3 C13 -161.3(4) . . . . ? O15 Mn2 N3 C24 178.84(19) . . . . ? O12 Mn2 N3 C24 -91.5(2) . . . . ? O5 Mn2 N3 C24 92.9(2) . . . . ? N4 Mn2 N3 C24 -1.32(19) . . . . ? O4 Mn2 N3 C24 16.0(5) . . . . ? O15 Mn2 N4 C22 -160(12) . . . . ? O12 Mn2 N4 C22 -79.0(3) . . . . ? O5 Mn2 N4 C22 91.6(3) . . . . ? N3 Mn2 N4 C22 -179.0(3) . . . . ? O4 Mn2 N4 C22 4.7(3) . . . . ? O15 Mn2 N4 C23 20(12) . . . . ? O12 Mn2 N4 C23 101.2(2) . . . . ? O5 Mn2 N4 C23 -88.3(2) . . . . ? N3 Mn2 N4 C23 1.2(2) . . . . ? O4 Mn2 N4 C23 -175.1(2) . . . . ? C12 N1 C1 C2 0.6(5) . . . . ? Mn1 N1 C1 C2 -169.6(3) . . . . ? N1 C1 C2 C3 1.8(6) . . . . ? C1 C2 C3 C4 -2.8(6) . . . . ? C2 C3 C4 C12 1.4(5) . . . . ? C2 C3 C4 C5 -174.7(3) . . . . ? C12 C4 C5 C6 -3.3(5) . . . . ? C3 C4 C5 C6 172.8(4) . . . . ? C4 C5 C6 C7 2.4(6) . . . . ? C5 C6 C7 C11 2.1(5) . . . . ? C5 C6 C7 C8 -178.1(3) . . . . ? C11 C7 C8 C9 0.2(5) . . . . ? C6 C7 C8 C9 -179.6(3) . . . . ? C7 C8 C9 C10 2.2(5) . . . . ? C11 N2 C10 C9 -0.4(5) . . . . ? Mn1 N2 C10 C9 178.9(2) . . . . ? C8 C9 C10 N2 -2.2(5) . . . . ? C10 N2 C11 C7 3.0(4) . . . . ? Mn1 N2 C11 C7 -176.4(2) . . . . ? C10 N2 C11 C12 -174.6(3) . . . . ? Mn1 N2 C11 C12 6.0(3) . . . . ? C8 C7 C11 N2 -2.9(5) . . . . ? C6 C7 C11 N2 176.9(3) . . . . ? C8 C7 C11 C12 174.6(3) . . . . ? C6 C7 C11 C12 -5.6(5) . . . . ? C1 N1 C12 C4 -2.1(5) . . . . ? Mn1 N1 C12 C4 169.7(2) . . . . ? C1 N1 C12 C11 175.6(3) . . . . ? Mn1 N1 C12 C11 -12.6(3) . . . . ? C3 C4 C12 N1 1.0(5) . . . . ? C5 C4 C12 N1 177.4(3) . . . . ? C3 C4 C12 C11 -176.6(3) . . . . ? C5 C4 C12 C11 -0.3(5) . . . . ? N2 C11 C12 N1 4.5(4) . . . . ? C7 C11 C12 N1 -173.1(3) . . . . ? N2 C11 C12 C4 -177.7(3) . . . . ? C7 C11 C12 C4 4.7(5) . . . . ? C24 N3 C13 C14 0.6(5) . . . . ? Mn2 N3 C13 C14 177.9(2) . . . . ? N3 C13 C14 C15 -0.4(5) . . . . ? C13 C14 C15 C16 -0.1(5) . . . . ? C14 C15 C16 C24 0.3(5) . . . . ? C14 C15 C16 C17 -178.9(3) . . . . ? C24 C16 C17 C18 0.8(5) . . . . ? C15 C16 C17 C18 -180.0(3) . . . . ? C16 C17 C18 C19 -0.3(5) . . . . ? C17 C18 C19 C23 -0.9(5) . . . . ? C17 C18 C19 C20 179.4(3) . . . . ? C23 C19 C20 C21 -0.3(5) . . . . ? C18 C19 C20 C21 179.3(3) . . . . ? C19 C20 C21 C22 -0.7(5) . . . . ? C23 N4 C22 C21 -0.7(5) . . . . ? Mn2 N4 C22 C21 179.5(2) . . . . ? C20 C21 C22 N4 1.3(5) . . . . ? C22 N4 C23 C19 -0.5(4) . . . . ? Mn2 N4 C23 C19 179.3(2) . . . . ? C22 N4 C23 C24 179.2(3) . . . . ? Mn2 N4 C23 C24 -0.9(3) . . . . ? C20 C19 C23 N4 1.0(5) . . . . ? C18 C19 C23 N4 -178.6(3) . . . . ? C20 C19 C23 C24 -178.7(3) . . . . ? C18 C19 C23 C24 1.6(4) . . . . ? C13 N3 C24 C16 -0.4(4) . . . . ? Mn2 N3 C24 C16 -178.1(2) . . . . ? C13 N3 C24 C23 178.9(3) . . . . ? Mn2 N3 C24 C23 1.3(3) . . . . ? C15 C16 C24 N3 0.0(5) . . . . ? C17 C16 C24 N3 179.2(3) . . . . ? C15 C16 C24 C23 -179.3(3) . . . . ? C17 C16 C24 C23 -0.1(4) . . . . ? N4 C23 C24 N3 -0.2(4) . . . . ? C19 C23 C24 N3 179.5(3) . . . . ? N4 C23 C24 C16 179.1(3) . . . . ? C19 C23 C24 C16 -1.1(4) . . . . ? Mn1 O7 C25 O6 -20.0(4) . . . . ? Mn1 O7 C25 C26 161.3(2) . . . . ? O6 C25 C26 C27 138.6(3) . . . . ? O7 C25 C26 C27 -42.7(4) . . . . ? O6 C25 C26 C31 -44.9(4) . . . . ? O7 C25 C26 C31 133.9(3) . . . . ? C31 C26 C27 C28 -1.3(4) . . . . ? C25 C26 C27 C28 175.2(3) . . . . ? C31 C26 C27 C32 175.9(3) . . . . ? C25 C26 C27 C32 -7.6(4) . . . . ? C26 C27 C28 C29 1.1(5) . . . . ? C32 C27 C28 C29 -176.2(3) . . . . ? C27 C28 C29 C30 -0.7(5) . . . . ? C28 C29 C30 C31 0.4(5) . . . . ? C28 C29 C30 S1 -178.7(3) . . . . ? O11 S1 C30 C31 -143.5(3) . . . . ? O10 S1 C30 C31 -12.4(3) . . . . ? C33 S1 C30 C31 102.5(3) . . . . ? O11 S1 C30 C29 35.7(3) . . . . ? O10 S1 C30 C29 166.8(3) . . . . ? C33 S1 C30 C29 -78.3(3) . . . . ? C29 C30 C31 C26 -0.6(5) . . . . ? S1 C30 C31 C26 178.6(2) . . . . ? C27 C26 C31 C30 1.0(5) . . . . ? C25 C26 C31 C30 -175.6(3) . . . . ? C26 C27 C32 O9 -54.2(4) . . . . ? C28 C27 C32 O9 123.0(3) . . . . ? C26 C27 C32 O8 128.7(3) . . . . ? C28 C27 C32 O8 -54.1(4) . . . . ? O11 S1 C33 C38 171.1(3) . . . . ? O10 S1 C33 C38 39.0(3) . . . . ? C30 S1 C33 C38 -74.7(3) . . . . ? O11 S1 C33 C34 -8.0(4) . . . . ? O10 S1 C33 C34 -140.1(3) . . . . ? C30 S1 C33 C34 106.2(3) . . . . ? C38 C33 C34 C35 0.9(6) . . . . ? S1 C33 C34 C35 -180.0(3) . . . . ? C33 C34 C35 C36 3.1(6) . . . . ? C34 C35 C36 C37 -4.4(6) . . . . ? C34 C35 C36 C40 174.8(3) . . . . ? C35 C36 C37 C38 1.7(5) . . . . ? C40 C36 C37 C38 -177.5(3) . . . . ? C35 C36 C37 C39 -173.7(3) . . . . ? C40 C36 C37 C39 7.1(5) . . . . ? C34 C33 C38 C37 -3.7(5) . . . . ? S1 C33 C38 C37 177.2(3) . . . . ? C36 C37 C38 C33 2.3(5) . . . . ? C39 C37 C38 C33 178.1(3) . . . . ? Mn2 O12 C39 O13 165.5(2) . . . . ? Mn2 O12 C39 C37 -13.3(5) . . . . ? C38 C37 C39 O13 -39.6(4) . . . . ? C36 C37 C39 O13 135.8(3) . . . . ? C38 C37 C39 O12 139.2(3) . . . . ? C36 C37 C39 O12 -45.3(5) . . . . ? Mn2 O15 C40 O14 142.7(3) . . . . ? Mn2 O15 C40 C36 -41.8(4) . . . . ? C35 C36 C40 O14 58.1(4) . . . . ? C37 C36 C40 O14 -122.7(3) . . . . ? C35 C36 C40 O15 -117.7(3) . . . . ? C37 C36 C40 O15 61.6(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H10W O8 0.85 2.03 2.854(3) 164.6 2_655 O5 H9W O13 0.85 1.85 2.676(3) 166.2 1_455 O4 H8W O8 0.85 1.89 2.725(3) 168.5 2_655 O4 H7W O7 0.84 2.34 2.933(3) 128.0 2_755 O3 H6W O6 0.85 1.76 2.601(3) 168.6 . O3 H5W O9 0.84 2.08 2.860(3) 153.8 1_655 O2 H4W O3 0.84 1.96 2.802(3) 177.3 3_765 O2 H3W O9 0.84 1.92 2.750(3) 170.4 . O1 H2W O15 0.84 2.56 3.159(3) 128.8 2_745 O1 H2W O14 0.84 1.87 2.710(3) 173.4 2_745 O1 H1W O8 0.84 1.90 2.743(3) 178.2 1_655 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.618 _refine_diff_density_min -0.532 _refine_diff_density_rms 0.064 # Attachment '4.cif' data_a _database_code_depnum_ccdc_archive 'CCDC 737216' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H30 Mn2 N4 O14 S' _chemical_formula_weight 884.58 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' Mn Mn 0.3368 0.7283 '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 12.826(3) _cell_length_b 38.750(8) _cell_length_c 7.3476(14) _cell_angle_alpha 90.00 _cell_angle_beta 94.165(2) _cell_angle_gamma 90.00 _cell_volume 3642.1(12) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 7659 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 28.00 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 0.828 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7251 _exptl_absorpt_correction_T_max 0.8619 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27247 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0370 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6754 _reflns_number_gt 5482 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0403P)^2^+3.7581P] 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 CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6754 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0527 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1059 _refine_ls_wR_factor_gt 0.0995 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _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 Mn1 Mn 0.26254(4) 0.046826(12) -0.21950(6) 0.02920(13) Uani 1 1 d . . . Mn2 Mn 0.09295(3) 0.149819(11) -0.08389(6) 0.02657(12) Uani 1 1 d . . . S1 S 0.56718(5) 0.187876(19) 0.59364(10) 0.02921(17) Uani 1 1 d . . . O1 O 0.12047(16) 0.15011(5) 0.2093(3) 0.0335(5) Uani 1 1 d . . . H1W H 0.0691 0.1567 0.2627 0.050 Uiso 1 1 d R . . H2W H 0.1424 0.1313 0.2494 0.050 Uiso 1 1 d R . . O2 O 0.12158(16) 0.04848(6) -0.4147(3) 0.0381(5) Uani 1 1 d . . . H3W H 0.0634 0.0529 -0.3753 0.057 Uiso 1 1 d R . . H4W H 0.1380 0.0635 -0.4873 0.057 Uiso 1 1 d R . . O3 O 0.13786(18) 0.04428(6) -0.0285(3) 0.0483(6) Uani 1 1 d . . . H5W H 0.0946 0.0602 -0.0293 0.072 Uiso 1 1 d R . . H6W H 0.1390 0.0334 0.0690 0.072 Uiso 1 1 d R . . O4 O 0.1268(3) 1.00313(7) 0.2757(4) 0.0727(9) Uani 1 1 d . . . H7W H 0.1226 1.0106 0.3816 0.109 Uiso 1 1 d R . . H8W H 0.1080 0.9825 0.2687 0.109 Uiso 1 1 d R . . O5 O 0.23759(15) 0.12279(6) -0.0862(3) 0.0341(5) Uani 1 1 d . . . O6 O 0.34180(17) 0.07867(5) -0.0110(3) 0.0372(5) Uani 1 1 d . . . O7 O 0.20307(15) 0.08919(5) 0.3398(3) 0.0341(5) Uani 1 1 d . . . O8 O 0.32480(16) 0.07808(6) 0.5658(3) 0.0347(5) Uani 1 1 d . . . O9 O 0.60552(16) 0.21847(6) 0.5113(3) 0.0412(6) Uani 1 1 d . . . O10 O 0.51016(16) 0.19064(6) 0.7540(3) 0.0380(5) Uani 1 1 d . . . O11 O 0.95139(17) 0.16572(7) 0.3878(3) 0.0484(6) Uani 1 1 d . . . O12 O 1.04098(15) 0.14461(6) 0.6322(3) 0.0387(5) Uani 1 1 d . . . O13 O 0.99608(16) 0.10294(6) 0.9347(3) 0.0379(5) Uani 1 1 d . . . O14 O 0.93444(18) 0.06574(6) 0.7213(4) 0.0499(6) Uani 1 1 d . . . N1 N 0.4227(2) 0.02096(7) -0.2295(4) 0.0363(6) Uani 1 1 d . . . N2 N 0.2425(2) -0.01228(7) -0.2335(4) 0.0410(7) Uani 1 1 d . . . N3 N 0.15867(18) 0.20293(7) -0.1497(3) 0.0312(6) Uani 1 1 d . . . N4 N -0.03176(18) 0.19047(6) -0.0344(3) 0.0300(6) Uani 1 1 d . . . C1 C 0.5111(3) 0.03889(9) -0.2268(5) 0.0466(9) Uani 1 1 d . . . H1A H 0.5077 0.0627 -0.2104 0.056 Uiso 1 1 calc R . . C2 C 0.6073(3) 0.02432(10) -0.2470(5) 0.0494(9) Uani 1 1 d . . . H2A H 0.6672 0.0379 -0.2443 0.059 Uiso 1 1 calc R . . C3 C 0.6125(3) -0.01058(11) -0.2711(5) 0.0551(10) Uani 1 1 d . . . H3A H 0.6764 -0.0213 -0.2849 0.066 Uiso 1 1 calc R . . C4 C 0.5220(3) -0.02963(10) -0.2746(5) 0.0536(10) Uani 1 1 d . . . H4 H 0.5241 -0.0534 -0.2905 0.064 Uiso 1 1 calc R . . C5 C 0.4277(3) -0.01323(8) -0.2545(4) 0.0353(7) Uani 1 1 d . . . C6 C 0.3264(3) -0.03178(8) -0.2575(4) 0.0380(8) Uani 1 1 d . . . C7 C 0.3170(4) -0.06730(9) -0.2825(5) 0.0553(10) Uani 1 1 d . . . H7 H 0.3757 -0.0807 -0.2992 0.066 Uiso 1 1 calc R . . C8 C 0.2201(4) -0.08241(11) -0.2821(5) 0.0640(12) Uani 1 1 d . . . H8 H 0.2129 -0.1061 -0.2990 0.077 Uiso 1 1 calc R . . C9 C 0.1346(4) -0.06257(11) -0.2570(5) 0.0586(11) Uani 1 1 d . . . H9 H 0.0685 -0.0724 -0.2562 0.070 Uiso 1 1 calc R . . C10 C 0.1485(3) -0.02749(10) -0.2328(5) 0.0536(10) Uani 1 1 d . . . H10 H 0.0905 -0.0138 -0.2152 0.064 Uiso 1 1 calc R . . C11 C 0.2571(2) 0.20869(9) -0.1900(5) 0.0411(8) Uani 1 1 d . . . H11 H 0.3005 0.1898 -0.2035 0.049 Uiso 1 1 calc R . . C12 C 0.2976(3) 0.24121(10) -0.2126(5) 0.0470(9) Uani 1 1 d . . . H12 H 0.3667 0.2441 -0.2402 0.056 Uiso 1 1 calc R . . C13 C 0.2340(3) 0.26920(9) -0.1936(5) 0.0477(9) Uani 1 1 d . . . H13 H 0.2596 0.2915 -0.2065 0.057 Uiso 1 1 calc R . . C14 C 0.1314(3) 0.26395(9) -0.1551(5) 0.0421(8) Uani 1 1 d . . . H14 H 0.0867 0.2826 -0.1435 0.050 Uiso 1 1 calc R . . C15 C 0.0958(2) 0.23046(8) -0.1340(4) 0.0311(7) Uani 1 1 d . . . C16 C -0.0133(2) 0.22295(8) -0.0907(4) 0.0311(7) Uani 1 1 d . . . C17 C -0.0923(3) 0.24728(9) -0.1080(5) 0.0481(9) Uani 1 1 d . . . H17 H -0.0788 0.2695 -0.1487 0.058 Uiso 1 1 calc R . . C18 C -0.1914(3) 0.23825(10) -0.0641(6) 0.0547(10) Uani 1 1 d . . . H18 H -0.2460 0.2540 -0.0798 0.066 Uiso 1 1 calc R . . C19 C -0.2089(3) 0.20589(10) 0.0031(5) 0.0464(9) Uani 1 1 d . . . H19 H -0.2743 0.1997 0.0394 0.056 Uiso 1 1 calc R . . C20 C -0.1273(2) 0.18276(9) 0.0153(4) 0.0359(7) Uani 1 1 d . . . H20 H -0.1391 0.1608 0.0602 0.043 Uiso 1 1 calc R . . C21 C 0.3081(2) 0.10839(8) 0.0142(4) 0.0274(6) Uani 1 1 d . . . C22 C 0.3652(2) 0.12872(7) 0.1665(4) 0.0258(6) Uani 1 1 d . . . C23 C 0.3620(2) 0.12061(7) 0.3513(4) 0.0240(6) Uani 1 1 d . . . C24 C 0.4237(2) 0.13927(7) 0.4798(4) 0.0267(6) Uani 1 1 d . . . H24 H 0.4217 0.1341 0.6031 0.032 Uiso 1 1 calc R . . C25 C 0.4880(2) 0.16542(8) 0.4260(4) 0.0281(6) Uani 1 1 d . . . C26 C 0.4917(2) 0.17372(9) 0.2434(4) 0.0347(7) Uani 1 1 d . . . H26 H 0.5348 0.1914 0.2074 0.042 Uiso 1 1 calc R . . C27 C 0.4302(2) 0.15532(8) 0.1156(4) 0.0342(7) Uani 1 1 d . . . H27 H 0.4322 0.1608 -0.0074 0.041 Uiso 1 1 calc R . . C28 C 0.2908(2) 0.09348(7) 0.4235(4) 0.0257(6) Uani 1 1 d . . . C29 C 0.6739(2) 0.15974(8) 0.6470(4) 0.0281(6) Uani 1 1 d . . . C30 C 0.6623(2) 0.13287(8) 0.7689(4) 0.0353(7) Uani 1 1 d . . . H30 H 0.5986 0.1292 0.8187 0.042 Uiso 1 1 calc R . . C31 C 0.7463(2) 0.11167(8) 0.8153(4) 0.0358(7) Uani 1 1 d . . . H31 H 0.7382 0.0932 0.8938 0.043 Uiso 1 1 calc R . . C32 C 0.8432(2) 0.11753(7) 0.7464(4) 0.0287(6) Uani 1 1 d . . . C33 C 0.8544(2) 0.14458(7) 0.6236(4) 0.0263(6) Uani 1 1 d . . . C34 C 0.7679(2) 0.16519(8) 0.5720(4) 0.0281(6) Uani 1 1 d . . . H34 H 0.7739 0.1827 0.4867 0.034 Uiso 1 1 calc R . . C35 C 0.9327(2) 0.09352(8) 0.8039(4) 0.0331(7) Uani 1 1 d . . . C36 C 0.9574(2) 0.15220(8) 0.5420(4) 0.0292(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0344(3) 0.0273(2) 0.0259(2) 0.00201(18) 0.00169(18) 0.00356(19) Mn2 0.0250(2) 0.0276(2) 0.0268(2) 0.00130(18) -0.00006(17) 0.00466(17) S1 0.0215(3) 0.0312(4) 0.0348(4) 0.0003(3) 0.0011(3) -0.0030(3) O1 0.0350(11) 0.0385(12) 0.0277(11) 0.0059(9) 0.0077(9) 0.0111(9) O2 0.0367(12) 0.0406(13) 0.0373(13) 0.0106(10) 0.0047(10) -0.0021(10) O3 0.0504(15) 0.0503(15) 0.0455(14) 0.0095(11) 0.0128(11) 0.0141(11) O4 0.111(3) 0.0499(17) 0.0593(19) -0.0011(14) 0.0219(17) -0.0188(16) O5 0.0292(11) 0.0453(13) 0.0269(11) -0.0013(9) -0.0042(9) 0.0127(9) O6 0.0429(12) 0.0331(12) 0.0344(12) -0.0070(9) -0.0047(9) 0.0127(10) O7 0.0308(11) 0.0363(12) 0.0343(12) 0.0085(9) -0.0047(9) -0.0056(9) O8 0.0343(11) 0.0395(13) 0.0295(11) 0.0116(9) -0.0027(9) -0.0027(9) O9 0.0305(11) 0.0346(13) 0.0581(15) 0.0078(11) 0.0000(10) -0.0071(9) O10 0.0330(12) 0.0453(13) 0.0364(12) -0.0072(10) 0.0074(9) -0.0023(10) O11 0.0350(12) 0.0789(18) 0.0328(13) 0.0222(12) 0.0117(10) 0.0162(12) O12 0.0248(11) 0.0635(16) 0.0277(12) 0.0023(10) 0.0006(9) 0.0029(10) O13 0.0349(12) 0.0361(12) 0.0410(13) 0.0088(10) -0.0081(10) -0.0013(9) O14 0.0465(14) 0.0330(13) 0.0695(18) -0.0081(12) 0.0000(12) 0.0024(11) N1 0.0417(16) 0.0320(15) 0.0354(15) -0.0004(11) 0.0033(12) 0.0072(12) N2 0.0463(17) 0.0324(15) 0.0441(17) 0.0039(12) 0.0011(13) 0.0000(13) N3 0.0285(13) 0.0339(14) 0.0314(14) 0.0036(11) 0.0034(10) 0.0058(11) N4 0.0285(13) 0.0348(14) 0.0265(13) -0.0002(11) -0.0001(10) 0.0047(11) C1 0.044(2) 0.039(2) 0.057(2) -0.0073(17) 0.0045(17) 0.0045(16) C2 0.040(2) 0.062(3) 0.046(2) -0.0046(18) 0.0008(16) 0.0043(17) C3 0.045(2) 0.062(3) 0.058(3) -0.002(2) 0.0041(18) 0.0214(19) C4 0.062(3) 0.041(2) 0.058(2) 0.0015(18) 0.0040(19) 0.0222(19) C5 0.051(2) 0.0313(17) 0.0228(16) 0.0020(12) -0.0002(13) 0.0117(14) C6 0.056(2) 0.0332(18) 0.0244(16) 0.0029(13) 0.0003(14) 0.0059(15) C7 0.086(3) 0.033(2) 0.047(2) -0.0061(16) 0.005(2) 0.0053(19) C8 0.107(4) 0.038(2) 0.046(2) -0.0053(18) -0.001(2) -0.018(2) C9 0.071(3) 0.053(3) 0.050(2) 0.0045(19) -0.005(2) -0.022(2) C10 0.052(2) 0.049(2) 0.059(2) 0.0095(18) -0.0004(18) -0.0086(18) C11 0.0332(17) 0.043(2) 0.049(2) 0.0074(16) 0.0094(15) 0.0079(14) C12 0.0347(18) 0.053(2) 0.054(2) 0.0095(18) 0.0099(16) -0.0023(16) C13 0.050(2) 0.038(2) 0.055(2) 0.0077(16) 0.0051(17) -0.0072(16) C14 0.0442(19) 0.0338(19) 0.048(2) 0.0025(15) 0.0017(16) 0.0067(15) C15 0.0331(16) 0.0324(17) 0.0276(16) 0.0030(12) -0.0001(12) 0.0055(13) C16 0.0335(16) 0.0321(17) 0.0270(16) -0.0024(12) -0.0019(12) 0.0081(13) C17 0.042(2) 0.038(2) 0.065(2) 0.0015(17) 0.0022(17) 0.0122(15) C18 0.037(2) 0.050(2) 0.076(3) -0.014(2) 0.0007(18) 0.0190(17) C19 0.0279(17) 0.062(2) 0.050(2) -0.0157(18) 0.0077(15) 0.0017(16) C20 0.0324(17) 0.045(2) 0.0301(17) -0.0051(14) 0.0016(13) -0.0033(14) C21 0.0242(14) 0.0357(17) 0.0228(15) -0.0003(12) 0.0054(11) 0.0042(12) C22 0.0231(14) 0.0294(16) 0.0247(15) -0.0013(12) 0.0002(11) 0.0070(11) C23 0.0231(14) 0.0254(15) 0.0235(15) 0.0015(11) 0.0011(11) 0.0025(11) C24 0.0270(15) 0.0310(16) 0.0221(15) 0.0028(12) 0.0010(11) -0.0012(12) C25 0.0199(14) 0.0317(16) 0.0325(16) 0.0019(12) 0.0006(11) -0.0003(12) C26 0.0255(15) 0.0436(19) 0.0353(18) 0.0102(14) 0.0044(13) -0.0059(13) C27 0.0315(16) 0.0451(19) 0.0264(16) 0.0068(14) 0.0040(12) -0.0019(14) C28 0.0281(15) 0.0228(15) 0.0262(15) -0.0009(12) 0.0024(12) 0.0014(11) C29 0.0236(14) 0.0318(16) 0.0282(16) 0.0010(12) -0.0018(11) -0.0016(12) C30 0.0248(15) 0.0419(19) 0.0389(18) 0.0058(14) 0.0014(13) -0.0076(13) C31 0.0322(17) 0.0358(18) 0.0387(18) 0.0096(14) -0.0009(13) -0.0058(13) C32 0.0297(15) 0.0272(15) 0.0284(16) -0.0026(12) -0.0028(12) -0.0017(12) C33 0.0264(15) 0.0294(16) 0.0228(15) -0.0030(12) -0.0002(11) -0.0015(12) C34 0.0256(15) 0.0312(16) 0.0274(16) 0.0004(12) 0.0011(11) -0.0024(12) C35 0.0292(16) 0.0289(17) 0.0413(19) 0.0076(14) 0.0028(13) -0.0021(12) C36 0.0283(16) 0.0314(16) 0.0281(16) -0.0028(13) 0.0042(12) 0.0027(12) _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 O6 2.162(2) . ? Mn1 O8 2.185(2) 1_554 ? Mn1 O3 2.205(2) . ? Mn1 O2 2.225(2) . ? Mn1 N1 2.292(3) . ? Mn1 N2 2.306(3) . ? Mn2 O5 2.132(2) . ? Mn2 O12 2.153(2) 1_454 ? Mn2 O1 2.157(2) . ? Mn2 O13 2.211(2) 1_454 ? Mn2 N3 2.289(3) . ? Mn2 N4 2.293(2) . ? S1 O9 1.434(2) . ? S1 O10 1.435(2) . ? S1 C25 1.767(3) . ? S1 C29 1.772(3) . ? O1 H1W 0.8309 . ? O1 H2W 0.8291 . ? O2 H3W 0.8366 . ? O2 H4W 0.8278 . ? O3 H5W 0.8306 . ? O3 H6W 0.8307 . ? O4 H7W 0.8357 . ? O4 H8W 0.8341 . ? O5 C21 1.255(3) . ? O6 C21 1.249(3) . ? O7 C28 1.253(3) . ? O8 C28 1.254(3) . ? O8 Mn1 2.185(2) 1_556 ? O11 C36 1.245(4) . ? O12 C36 1.254(3) . ? O12 Mn2 2.153(2) 1_656 ? O13 C35 1.267(4) . ? O13 Mn2 2.211(2) 1_656 ? O14 C35 1.237(4) . ? N1 C1 1.329(4) . ? N1 C5 1.340(4) . ? N2 C6 1.337(4) . ? N2 C10 1.342(4) . ? N3 C11 1.337(4) . ? N3 C15 1.347(4) . ? N4 C20 1.338(4) . ? N4 C16 1.351(4) . ? C1 C2 1.374(5) . ? C1 H1A 0.9300 . ? C2 C3 1.366(5) . ? C2 H2A 0.9300 . ? C3 C4 1.375(6) . ? C3 H3A 0.9300 . ? C4 C5 1.384(5) . ? C4 H4 0.9300 . ? C5 C6 1.483(5) . ? C6 C7 1.392(5) . ? C7 C8 1.374(6) . ? C7 H7 0.9300 . ? C8 C9 1.363(6) . ? C8 H8 0.9300 . ? C9 C10 1.381(6) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.378(5) . ? C11 H11 0.9300 . ? C12 C13 1.371(5) . ? C12 H12 0.9300 . ? C13 C14 1.381(5) . ? C13 H13 0.9300 . ? C14 C15 1.388(5) . ? C14 H14 0.9300 . ? C15 C16 1.485(4) . ? C16 C17 1.384(4) . ? C17 C18 1.378(5) . ? C17 H17 0.9300 . ? C18 C19 1.372(5) . ? C18 H18 0.9300 . ? C19 C20 1.376(5) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.513(4) . ? C22 C27 1.394(4) . ? C22 C23 1.397(4) . ? C23 C24 1.390(4) . ? C23 C28 1.514(4) . ? C24 C25 1.382(4) . ? C24 H24 0.9300 . ? C25 C26 1.384(4) . ? C26 C27 1.380(4) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C29 C34 1.378(4) . ? C29 C30 1.389(4) . ? C30 C31 1.377(4) . ? C30 H30 0.9300 . ? C31 C32 1.396(4) . ? C31 H31 0.9300 . ? C32 C33 1.397(4) . ? C32 C35 1.513(4) . ? C33 C34 1.396(4) . ? C33 C36 1.520(4) . ? C34 H34 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 O6 Mn1 O8 91.00(8) . 1_554 ? O6 Mn1 O3 84.27(9) . . ? O8 Mn1 O3 143.52(9) 1_554 . ? O6 Mn1 O2 139.29(8) . . ? O8 Mn1 O2 80.87(8) 1_554 . ? O3 Mn1 O2 79.55(9) . . ? O6 Mn1 N1 84.03(9) . . ? O8 Mn1 N1 81.01(9) 1_554 . ? O3 Mn1 N1 133.95(9) . . ? O2 Mn1 N1 132.85(9) . . ? O6 Mn1 N2 130.05(9) . . ? O8 Mn1 N2 124.30(9) 1_554 . ? O3 Mn1 N2 84.28(10) . . ? O2 Mn1 N2 85.25(9) . . ? N1 Mn1 N2 70.21(10) . . ? O5 Mn2 O12 98.90(8) . 1_454 ? O5 Mn2 O1 86.05(8) . . ? O12 Mn2 O1 169.96(8) 1_454 . ? O5 Mn2 O13 95.17(8) . 1_454 ? O12 Mn2 O13 81.21(8) 1_454 1_454 ? O1 Mn2 O13 89.68(8) . 1_454 ? O5 Mn2 N3 96.09(9) . . ? O12 Mn2 N3 88.43(9) 1_454 . ? O1 Mn2 N3 99.79(9) . . ? O13 Mn2 N3 165.74(8) 1_454 . ? O5 Mn2 N4 163.04(9) . . ? O12 Mn2 N4 92.72(8) 1_454 . ? O1 Mn2 N4 84.46(8) . . ? O13 Mn2 N4 98.80(9) 1_454 . ? N3 Mn2 N4 71.79(9) . . ? O9 S1 O10 119.71(14) . . ? O9 S1 C25 108.07(14) . . ? O10 S1 C25 107.93(13) . . ? O9 S1 C29 108.60(13) . . ? O10 S1 C29 107.22(14) . . ? C25 S1 C29 104.28(14) . . ? Mn2 O1 H1W 113.3 . . ? Mn2 O1 H2W 112.1 . . ? H1W O1 H2W 111.2 . . ? Mn1 O2 H3W 119.1 . . ? Mn1 O2 H4W 101.7 . . ? H3W O2 H4W 110.8 . . ? Mn1 O3 H5W 118.5 . . ? Mn1 O3 H6W 127.1 . . ? H5W O3 H6W 110.7 . . ? H7W O4 H8W 110.6 . . ? C21 O5 Mn2 143.51(19) . . ? C21 O6 Mn1 118.77(19) . . ? C28 O8 Mn1 137.89(19) . 1_556 ? C36 O12 Mn2 133.1(2) . 1_656 ? C35 O13 Mn2 121.49(19) . 1_656 ? C1 N1 C5 118.0(3) . . ? C1 N1 Mn1 122.5(2) . . ? C5 N1 Mn1 119.2(2) . . ? C6 N2 C10 119.0(3) . . ? C6 N2 Mn1 118.6(2) . . ? C10 N2 Mn1 122.2(2) . . ? C11 N3 C15 117.9(3) . . ? C11 N3 Mn2 124.4(2) . . ? C15 N3 Mn2 117.51(19) . . ? C20 N4 C16 118.4(3) . . ? C20 N4 Mn2 123.6(2) . . ? C16 N4 Mn2 116.83(19) . . ? N1 C1 C2 123.7(3) . . ? N1 C1 H1A 118.1 . . ? C2 C1 H1A 118.1 . . ? C3 C2 C1 118.3(4) . . ? C3 C2 H2A 120.9 . . ? C1 C2 H2A 120.9 . . ? C2 C3 C4 119.0(3) . . ? C2 C3 H3A 120.5 . . ? C4 C3 H3A 120.5 . . ? C3 C4 C5 119.7(4) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? N1 C5 C4 121.3(3) . . ? N1 C5 C6 115.5(3) . . ? C4 C5 C6 123.2(3) . . ? N2 C6 C7 120.8(3) . . ? N2 C6 C5 115.9(3) . . ? C7 C6 C5 123.3(3) . . ? C8 C7 C6 119.4(4) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C9 C8 C7 119.8(4) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 118.4(4) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.8 . . ? N2 C10 C9 122.7(4) . . ? N2 C10 H10 118.7 . . ? C9 C10 H10 118.7 . . ? N3 C11 C12 123.4(3) . . ? N3 C11 H11 118.3 . . ? C12 C11 H11 118.3 . . ? C13 C12 C11 118.6(3) . . ? C13 C12 H12 120.7 . . ? C11 C12 H12 120.7 . . ? C12 C13 C14 119.2(3) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C13 C14 C15 119.1(3) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? N3 C15 C14 121.8(3) . . ? N3 C15 C16 116.2(3) . . ? C14 C15 C16 122.0(3) . . ? N4 C16 C17 121.3(3) . . ? N4 C16 C15 115.9(2) . . ? C17 C16 C15 122.8(3) . . ? C18 C17 C16 119.2(3) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C19 C18 C17 119.6(3) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 118.4(3) . . ? C18 C19 H19 120.8 . . ? C20 C19 H19 120.8 . . ? N4 C20 C19 123.0(3) . . ? N4 C20 H20 118.5 . . ? C19 C20 H20 118.5 . . ? O6 C21 O5 124.4(3) . . ? O6 C21 C22 115.8(2) . . ? O5 C21 C22 119.5(3) . . ? C27 C22 C23 119.2(3) . . ? C27 C22 C21 117.0(3) . . ? C23 C22 C21 123.7(3) . . ? C24 C23 C22 119.2(3) . . ? C24 C23 C28 116.8(2) . . ? C22 C23 C28 123.9(2) . . ? C25 C24 C23 120.6(3) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 120.7(3) . . ? C24 C25 S1 119.1(2) . . ? C26 C25 S1 120.2(2) . . ? C27 C26 C25 118.8(3) . . ? C27 C26 H26 120.6 . . ? C25 C26 H26 120.6 . . ? C26 C27 C22 121.5(3) . . ? C26 C27 H27 119.2 . . ? C22 C27 H27 119.2 . . ? O7 C28 O8 126.3(3) . . ? O7 C28 C23 117.6(2) . . ? O8 C28 C23 116.1(2) . . ? C34 C29 C30 120.7(3) . . ? C34 C29 S1 120.1(2) . . ? C30 C29 S1 119.1(2) . . ? C31 C30 C29 119.2(3) . . ? C31 C30 H30 120.4 . . ? C29 C30 H30 120.4 . . ? C30 C31 C32 121.0(3) . . ? C30 C31 H31 119.5 . . ? C32 C31 H31 119.5 . . ? C31 C32 C33 119.5(3) . . ? C31 C32 C35 118.4(3) . . ? C33 C32 C35 122.1(3) . . ? C34 C33 C32 119.2(3) . . ? C34 C33 C36 118.5(3) . . ? C32 C33 C36 122.2(3) . . ? C29 C34 C33 120.3(3) . . ? C29 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? O14 C35 O13 126.1(3) . . ? O14 C35 C32 116.0(3) . . ? O13 C35 C32 117.8(3) . . ? O11 C36 O12 125.0(3) . . ? O11 C36 C33 116.3(3) . . ? O12 C36 C33 118.7(3) . . ? 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 O12 Mn2 O5 C21 -163.1(3) 1_454 . . . ? O1 Mn2 O5 C21 8.1(3) . . . . ? O13 Mn2 O5 C21 -81.3(3) 1_454 . . . ? N3 Mn2 O5 C21 107.5(3) . . . . ? N4 Mn2 O5 C21 64.2(5) . . . . ? O8 Mn1 O6 C21 72.5(2) 1_554 . . . ? O3 Mn1 O6 C21 -71.3(2) . . . . ? O2 Mn1 O6 C21 -4.6(3) . . . . ? N1 Mn1 O6 C21 153.3(2) . . . . ? N2 Mn1 O6 C21 -148.9(2) . . . . ? O6 Mn1 N1 C1 -43.4(3) . . . . ? O8 Mn1 N1 C1 48.6(3) 1_554 . . . ? O3 Mn1 N1 C1 -119.5(3) . . . . ? O2 Mn1 N1 C1 117.1(3) . . . . ? N2 Mn1 N1 C1 -179.9(3) . . . . ? O6 Mn1 N1 C5 142.4(2) . . . . ? O8 Mn1 N1 C5 -125.6(2) 1_554 . . . ? O3 Mn1 N1 C5 66.3(3) . . . . ? O2 Mn1 N1 C5 -57.1(3) . . . . ? N2 Mn1 N1 C5 5.9(2) . . . . ? O6 Mn1 N2 C6 -69.6(3) . . . . ? O8 Mn1 N2 C6 57.3(3) 1_554 . . . ? O3 Mn1 N2 C6 -147.2(2) . . . . ? O2 Mn1 N2 C6 132.9(2) . . . . ? N1 Mn1 N2 C6 -6.2(2) . . . . ? O6 Mn1 N2 C10 115.7(3) . . . . ? O8 Mn1 N2 C10 -117.4(3) 1_554 . . . ? O3 Mn1 N2 C10 38.1(3) . . . . ? O2 Mn1 N2 C10 -41.8(3) . . . . ? N1 Mn1 N2 C10 179.1(3) . . . . ? O5 Mn2 N3 C11 5.5(3) . . . . ? O12 Mn2 N3 C11 -93.3(3) 1_454 . . . ? O1 Mn2 N3 C11 92.5(3) . . . . ? O13 Mn2 N3 C11 -136.5(4) 1_454 . . . ? N4 Mn2 N3 C11 173.3(3) . . . . ? O5 Mn2 N3 C15 -169.6(2) . . . . ? O12 Mn2 N3 C15 91.6(2) 1_454 . . . ? O1 Mn2 N3 C15 -82.6(2) . . . . ? O13 Mn2 N3 C15 48.4(5) 1_454 . . . ? N4 Mn2 N3 C15 -1.8(2) . . . . ? O5 Mn2 N4 C20 -137.2(3) . . . . ? O12 Mn2 N4 C20 89.5(2) 1_454 . . . ? O1 Mn2 N4 C20 -80.9(2) . . . . ? O13 Mn2 N4 C20 7.9(2) 1_454 . . . ? N3 Mn2 N4 C20 176.9(2) . . . . ? O5 Mn2 N4 C16 55.1(4) . . . . ? O12 Mn2 N4 C16 -78.2(2) 1_454 . . . ? O1 Mn2 N4 C16 111.5(2) . . . . ? O13 Mn2 N4 C16 -159.7(2) 1_454 . . . ? N3 Mn2 N4 C16 9.2(2) . . . . ? C5 N1 C1 C2 -0.5(5) . . . . ? Mn1 N1 C1 C2 -174.7(3) . . . . ? N1 C1 C2 C3 0.0(6) . . . . ? C1 C2 C3 C4 0.1(6) . . . . ? C2 C3 C4 C5 0.2(6) . . . . ? C1 N1 C5 C4 0.8(5) . . . . ? Mn1 N1 C5 C4 175.3(2) . . . . ? C1 N1 C5 C6 -179.6(3) . . . . ? Mn1 N1 C5 C6 -5.1(3) . . . . ? C3 C4 C5 N1 -0.7(5) . . . . ? C3 C4 C5 C6 179.7(3) . . . . ? C10 N2 C6 C7 0.3(5) . . . . ? Mn1 N2 C6 C7 -174.5(3) . . . . ? C10 N2 C6 C5 -179.3(3) . . . . ? Mn1 N2 C6 C5 5.9(4) . . . . ? N1 C5 C6 N2 -0.5(4) . . . . ? C4 C5 C6 N2 179.1(3) . . . . ? N1 C5 C6 C7 179.8(3) . . . . ? C4 C5 C6 C7 -0.6(5) . . . . ? N2 C6 C7 C8 -0.1(5) . . . . ? C5 C6 C7 C8 179.5(3) . . . . ? C6 C7 C8 C9 -0.2(6) . . . . ? C7 C8 C9 C10 0.1(6) . . . . ? C6 N2 C10 C9 -0.4(5) . . . . ? Mn1 N2 C10 C9 174.2(3) . . . . ? C8 C9 C10 N2 0.2(6) . . . . ? C15 N3 C11 C12 1.3(5) . . . . ? Mn2 N3 C11 C12 -173.8(3) . . . . ? N3 C11 C12 C13 -0.2(6) . . . . ? C11 C12 C13 C14 -0.9(5) . . . . ? C12 C13 C14 C15 0.9(5) . . . . ? C11 N3 C15 C14 -1.2(5) . . . . ? Mn2 N3 C15 C14 174.2(2) . . . . ? C11 N3 C15 C16 179.4(3) . . . . ? Mn2 N3 C15 C16 -5.1(3) . . . . ? C13 C14 C15 N3 0.1(5) . . . . ? C13 C14 C15 C16 179.4(3) . . . . ? C20 N4 C16 C17 -4.0(4) . . . . ? Mn2 N4 C16 C17 164.4(2) . . . . ? C20 N4 C16 C15 176.6(3) . . . . ? Mn2 N4 C16 C15 -15.0(3) . . . . ? N3 C15 C16 N4 13.4(4) . . . . ? C14 C15 C16 N4 -165.9(3) . . . . ? N3 C15 C16 C17 -166.0(3) . . . . ? C14 C15 C16 C17 14.7(5) . . . . ? N4 C16 C17 C18 1.0(5) . . . . ? C15 C16 C17 C18 -179.7(3) . . . . ? C16 C17 C18 C19 2.8(6) . . . . ? C17 C18 C19 C20 -3.4(6) . . . . ? C16 N4 C20 C19 3.4(4) . . . . ? Mn2 N4 C20 C19 -164.1(2) . . . . ? C18 C19 C20 N4 0.3(5) . . . . ? Mn1 O6 C21 O5 -8.0(4) . . . . ? Mn1 O6 C21 C22 178.01(18) . . . . ? Mn2 O5 C21 O6 129.3(3) . . . . ? Mn2 O5 C21 C22 -56.9(4) . . . . ? O6 C21 C22 C27 106.3(3) . . . . ? O5 C21 C22 C27 -68.0(4) . . . . ? O6 C21 C22 C23 -68.9(4) . . . . ? O5 C21 C22 C23 116.8(3) . . . . ? C27 C22 C23 C24 0.0(4) . . . . ? C21 C22 C23 C24 175.0(2) . . . . ? C27 C22 C23 C28 176.9(3) . . . . ? C21 C22 C23 C28 -8.0(4) . . . . ? C22 C23 C24 C25 -0.4(4) . . . . ? C28 C23 C24 C25 -177.5(3) . . . . ? C23 C24 C25 C26 0.5(4) . . . . ? C23 C24 C25 S1 -178.7(2) . . . . ? O9 S1 C25 C24 -165.9(2) . . . . ? O10 S1 C25 C24 -35.1(3) . . . . ? C29 S1 C25 C24 78.7(3) . . . . ? O9 S1 C25 C26 14.9(3) . . . . ? O10 S1 C25 C26 145.7(2) . . . . ? C29 S1 C25 C26 -100.5(3) . . . . ? C24 C25 C26 C27 -0.2(5) . . . . ? S1 C25 C26 C27 179.0(2) . . . . ? C25 C26 C27 C22 -0.1(5) . . . . ? C23 C22 C27 C26 0.3(4) . . . . ? C21 C22 C27 C26 -175.1(3) . . . . ? Mn1 O8 C28 O7 -15.8(5) 1_556 . . . ? Mn1 O8 C28 C23 162.1(2) 1_556 . . . ? C24 C23 C28 O7 144.0(3) . . . . ? C22 C23 C28 O7 -33.0(4) . . . . ? C24 C23 C28 O8 -34.1(4) . . . . ? C22 C23 C28 O8 148.9(3) . . . . ? O9 S1 C29 C34 -14.9(3) . . . . ? O10 S1 C29 C34 -145.5(2) . . . . ? C25 S1 C29 C34 100.2(3) . . . . ? O9 S1 C29 C30 163.3(2) . . . . ? O10 S1 C29 C30 32.6(3) . . . . ? C25 S1 C29 C30 -81.7(3) . . . . ? C34 C29 C30 C31 0.3(5) . . . . ? S1 C29 C30 C31 -177.8(2) . . . . ? C29 C30 C31 C32 2.1(5) . . . . ? C30 C31 C32 C33 -2.2(5) . . . . ? C30 C31 C32 C35 179.4(3) . . . . ? C31 C32 C33 C34 -0.1(4) . . . . ? C35 C32 C33 C34 178.1(3) . . . . ? C31 C32 C33 C36 -179.4(3) . . . . ? C35 C32 C33 C36 -1.2(4) . . . . ? C30 C29 C34 C33 -2.7(4) . . . . ? S1 C29 C34 C33 175.5(2) . . . . ? C32 C33 C34 C29 2.6(4) . . . . ? C36 C33 C34 C29 -178.1(3) . . . . ? Mn2 O13 C35 O14 120.2(3) 1_656 . . . ? Mn2 O13 C35 C32 -62.5(3) 1_656 . . . ? C31 C32 C35 O14 81.0(4) . . . . ? C33 C32 C35 O14 -97.3(3) . . . . ? C31 C32 C35 O13 -96.6(3) . . . . ? C33 C32 C35 O13 85.1(4) . . . . ? Mn2 O12 C36 O11 138.0(3) 1_656 . . . ? Mn2 O12 C36 C33 -42.1(4) 1_656 . . . ? C34 C33 C36 O11 -28.1(4) . . . . ? C32 C33 C36 O11 151.2(3) . . . . ? C34 C33 C36 O12 151.9(3) . . . . ? C32 C33 C36 O12 -28.8(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H8W O14 0.83 1.95 2.782(4) 174.3 3_666 O4 H7W O2 0.84 2.10 2.880(4) 155.7 1_566 O3 H6W O4 0.83 1.93 2.757(4) 171.1 1_545 O3 H5W O13 0.83 2.09 2.911(3) 171.6 1_454 O2 H4W O8 0.83 2.46 2.861(3) 110.4 1_554 O2 H4W O7 0.83 1.86 2.667(3) 164.9 1_554 O2 H3W O14 0.84 1.91 2.749(3) 176.1 1_454 O1 H2W O7 0.83 1.91 2.733(3) 175.7 . O1 H1W O11 0.83 1.86 2.684(3) 173.1 1_455 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.486 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.067 # Attachment '5.cif' data_c _database_code_depnum_ccdc_archive 'CCDC 737217' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H38 Mn2 N4 O16 S' _chemical_formula_weight 972.68 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Aba2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/2, -y+1, z+1/2' '-x+1/2, y+1, z+1/2' _cell_length_a 17.581(2) _cell_length_b 27.365(3) _cell_length_c 8.8889(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4276.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 5381 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 24.20 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 0.716 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7210 _exptl_absorpt_correction_T_max 0.9102 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15476 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 25.50 _reflns_number_total 3950 _reflns_number_gt 3334 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1084P)^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 CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 3950 _refine_ls_number_parameters 285 _refine_ls_number_restraints 81 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1514 _refine_ls_wR_factor_gt 0.1435 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.156 _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 Mn1 Mn 0.17316(3) 0.33977(2) 0.26758(9) 0.0325(2) Uani 1 1 d . . . S1 S 0.0000 0.5000 -0.2933(3) 0.1070(14) Uani 1 2 d SU . . O1 O 0.5282(3) 0.2007(2) 0.6665(7) 0.096(2) Uani 1 1 d . . . H1W H 0.5194 0.2077 0.7555 0.144 Uiso 1 1 d R . . H2W H 0.5068 0.2201 0.6081 0.144 Uiso 1 1 d R . . O2 O 0.5392(5) 0.3705(4) 0.9384(13) 0.148(3) Uani 1 1 d . . . H3W H 0.5372 0.3437 0.9893 0.223 Uiso 1 1 d R . . H4W H 0.5293 0.3628 0.8489 0.223 Uiso 1 1 d R . . O3 O 0.1389(2) 0.34639(17) 0.4989(4) 0.0575(11) Uani 1 1 d . . . H5W H 0.1028 0.3286 0.5247 0.086 Uiso 1 1 d R . . H6W H 0.1650 0.3536 0.5744 0.086 Uiso 1 1 d R . . O4 O 0.20754(19) 0.36014(11) -0.2108(4) 0.0397(8) Uani 1 1 d . . . O5 O 0.1910(2) 0.33714(11) 0.0242(4) 0.0377(8) Uani 1 1 d . . . O6 O 0.0183(3) 0.28227(19) 0.0098(7) 0.0857(16) Uani 1 1 d . . . O7 O 0.0563(2) 0.32111(15) 0.2185(4) 0.0492(9) Uani 1 1 d . . . O8 O 0.0714(5) 0.5084(2) -0.3731(7) 0.134(3) Uani 1 1 d U . . N1 N 0.2076(2) 0.25873(13) 0.2725(7) 0.0478(10) Uani 1 1 d . . . N2 N 0.3370(2) -0.07480(14) 0.2308(5) 0.0413(10) Uani 1 1 d . . . C1 C 0.1547(5) 0.2258(2) 0.2726(18) 0.110(3) Uani 1 1 d U . . H1 H 0.1052 0.2353 0.2957 0.132 Uiso 1 1 calc R . . C2 C 0.1687(5) 0.1770(3) 0.2396(18) 0.109(3) Uani 1 1 d U . . H2 H 0.1278 0.1565 0.2193 0.131 Uiso 1 1 calc R . . C3 C 0.2380(4) 0.15878(19) 0.2361(10) 0.0710(19) Uani 1 1 d U . . C4 C 0.2902(5) 0.1908(3) 0.2718(16) 0.105(2) Uani 1 1 d U . . H4 H 0.3405 0.1807 0.2798 0.126 Uiso 1 1 calc R . . C5 C 0.2722(4) 0.2404(2) 0.2986(14) 0.099(3) Uani 1 1 d U . . H5 H 0.3100 0.2606 0.3374 0.119 Uiso 1 1 calc R . . C6 C 0.2506(5) 0.1056(2) 0.2113(9) 0.0715(19) Uani 1 1 d . . . H6 H 0.2124 0.0886 0.1612 0.086 Uiso 1 1 calc R . . C7 C 0.3100(4) 0.08054(19) 0.2531(9) 0.0579(14) Uani 1 1 d . . . H7 H 0.3496 0.0974 0.2990 0.069 Uiso 1 1 calc R . . C8 C 0.3191(3) 0.02730(19) 0.2331(6) 0.0493(14) Uani 1 1 d . . . C9 C 0.2712(3) -0.00215(19) 0.1506(8) 0.0516(14) Uani 1 1 d . . . H9 H 0.2319 0.0117 0.0951 0.062 Uiso 1 1 calc R . . C10 C 0.2812(3) -0.05192(18) 0.1499(7) 0.0478(13) Uani 1 1 d . . . H10 H 0.2485 -0.0709 0.0920 0.057 Uiso 1 1 calc R . . C11 C 0.3847(3) -0.04579(19) 0.3030(6) 0.0490(14) Uani 1 1 d . . . H11 H 0.4246 -0.0602 0.3553 0.059 Uiso 1 1 calc R . . C12 C 0.3791(4) 0.00452(19) 0.3060(7) 0.0562(16) Uani 1 1 d . . . H12 H 0.4154 0.0230 0.3566 0.067 Uiso 1 1 calc R . . C13 C 0.0374(3) 0.3186(2) 0.0809(7) 0.0507(13) Uani 1 1 d . . . C14 C 0.0322(3) 0.3665(2) -0.0056(6) 0.0448(12) Uani 1 1 d . . . C15 C -0.0366(4) 0.3917(3) -0.0050(9) 0.079(2) Uani 1 1 d . . . H15 H -0.0770 0.3798 0.0518 0.094 Uiso 1 1 calc R . . C16 C -0.0456(5) 0.4335(3) -0.0868(9) 0.086(3) Uani 1 1 d . . . H16 H -0.0908 0.4511 -0.0821 0.103 Uiso 1 1 calc R . . C17 C 0.0129(4) 0.4490(3) -0.1757(7) 0.070(2) Uani 1 1 d . . . C18 C 0.0830(3) 0.4250(2) -0.1792(6) 0.0471(13) Uani 1 1 d . . . H18 H 0.1225 0.4367 -0.2387 0.056 Uiso 1 1 calc R . . C19 C 0.0923(3) 0.38342(17) -0.0922(5) 0.0363(10) Uani 1 1 d . . . C20 C 0.1688(3) 0.35784(16) -0.0921(5) 0.0293(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0362(4) 0.0252(3) 0.0362(4) 0.0010(3) 0.0012(3) -0.0014(2) S1 0.179(3) 0.105(2) 0.0371(11) 0.000 0.000 0.112(2) O1 0.114(4) 0.092(4) 0.082(4) 0.018(3) 0.018(3) 0.052(3) O2 0.117(6) 0.175(8) 0.153(8) 0.006(7) -0.016(6) -0.019(6) O3 0.048(2) 0.089(3) 0.036(2) 0.0018(19) -0.0045(19) -0.022(2) O4 0.0393(16) 0.0407(17) 0.0391(19) 0.0081(16) 0.0062(17) 0.0081(14) O5 0.0399(17) 0.0368(18) 0.0364(19) 0.0022(14) 0.0050(15) 0.0121(14) O6 0.109(4) 0.068(3) 0.081(3) -0.012(3) -0.010(3) -0.037(3) O7 0.0423(19) 0.057(2) 0.049(2) 0.0027(17) 0.0025(16) -0.0099(17) O8 0.217(6) 0.108(4) 0.078(4) 0.042(3) 0.064(4) 0.109(4) N1 0.046(2) 0.0270(18) 0.070(3) 0.002(3) -0.004(3) 0.0032(16) N2 0.056(2) 0.0243(19) 0.043(3) 0.0013(16) -0.0059(18) 0.0004(16) C1 0.088(4) 0.046(3) 0.197(7) 0.000(5) -0.001(6) 0.000(3) C2 0.100(4) 0.052(3) 0.176(7) -0.007(5) -0.014(5) -0.008(3) C3 0.079(4) 0.029(2) 0.105(5) 0.004(3) 0.001(4) 0.000(2) C4 0.084(4) 0.056(3) 0.175(6) -0.019(5) -0.022(5) 0.017(3) C5 0.080(4) 0.045(3) 0.171(7) -0.022(4) -0.050(5) 0.005(3) C6 0.091(4) 0.033(3) 0.091(5) 0.009(3) 0.001(4) -0.001(3) C7 0.068(3) 0.035(3) 0.070(4) -0.001(3) 0.003(4) 0.002(2) C8 0.065(3) 0.033(3) 0.051(4) 0.000(2) 0.007(3) -0.004(2) C9 0.049(3) 0.040(3) 0.067(4) 0.008(3) -0.002(3) 0.006(2) C10 0.055(3) 0.032(3) 0.057(3) -0.003(2) -0.015(3) 0.005(2) C11 0.059(3) 0.035(2) 0.054(4) 0.000(2) -0.010(3) 0.000(2) C12 0.073(4) 0.036(3) 0.059(4) -0.004(2) -0.009(3) -0.009(3) C13 0.047(3) 0.049(3) 0.056(4) -0.003(3) 0.006(3) -0.012(3) C14 0.036(3) 0.050(3) 0.049(3) -0.002(2) -0.001(2) 0.009(2) C15 0.044(3) 0.115(6) 0.077(5) 0.003(5) 0.012(3) 0.031(4) C16 0.072(5) 0.115(6) 0.070(5) -0.003(4) 0.002(4) 0.057(5) C17 0.088(5) 0.078(5) 0.045(3) -0.004(3) -0.001(3) 0.061(4) C18 0.060(3) 0.045(3) 0.036(3) -0.003(2) 0.002(2) 0.025(3) C19 0.035(2) 0.037(2) 0.036(2) -0.006(2) -0.0022(19) 0.010(2) C20 0.038(3) 0.020(2) 0.030(3) -0.0017(17) 0.000(2) 0.0062(17) _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 O3 2.151(4) . ? Mn1 O7 2.162(4) . ? Mn1 O4 2.179(3) 8_545 ? Mn1 O5 2.187(4) . ? Mn1 N1 2.299(4) . ? Mn1 N2 2.367(4) 4 ? S1 O8 1.460(8) . ? S1 O8 1.460(8) 2_565 ? S1 C17 1.758(7) 2_565 ? S1 C17 1.758(7) . ? O1 H1W 0.8285 . ? O1 H2W 0.8315 . ? O2 H3W 0.8609 . ? O2 H4W 0.8408 . ? O3 H5W 0.8329 . ? O3 H6W 0.8361 . ? O4 C20 1.258(6) . ? O4 Mn1 2.179(3) 8_544 ? O5 C20 1.242(6) . ? O6 C13 1.224(7) . ? O7 C13 1.270(8) . ? N1 C5 1.264(8) . ? N1 C1 1.295(9) . ? N2 C11 1.321(7) . ? N2 C10 1.368(7) . ? N2 Mn1 2.367(4) 4_545 ? C1 C2 1.391(12) . ? C1 H1 0.9300 . ? C2 C3 1.316(11) . ? C2 H2 0.9300 . ? C3 C4 1.308(11) . ? C3 C6 1.488(8) . ? C4 C5 1.414(10) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.304(9) . ? C6 H6 0.9300 . ? C7 C8 1.476(7) . ? C7 H7 0.9300 . ? C8 C9 1.378(8) . ? C8 C12 1.386(9) . ? C9 C10 1.373(8) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.380(7) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.523(9) . ? C14 C19 1.386(7) . ? C14 C15 1.393(8) . ? C15 C16 1.366(11) . ? C15 H15 0.9300 . ? C16 C17 1.365(12) . ? C16 H16 0.9300 . ? C17 C18 1.396(8) . ? C18 C19 1.386(7) . ? C18 H18 0.9300 . ? C19 C20 1.517(6) . ? 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 O3 Mn1 O7 86.94(15) . . ? O3 Mn1 O4 99.43(15) . 8_545 ? O7 Mn1 O4 173.35(15) . 8_545 ? O3 Mn1 O5 171.42(17) . . ? O7 Mn1 O5 85.94(15) . . ? O4 Mn1 O5 87.56(14) 8_545 . ? O3 Mn1 N1 97.9(2) . . ? O7 Mn1 N1 91.51(15) . . ? O4 Mn1 N1 89.52(13) 8_545 . ? O5 Mn1 N1 87.11(18) . . ? O3 Mn1 N2 91.59(16) . 4 ? O7 Mn1 N2 97.67(15) . 4 ? O4 Mn1 N2 80.34(13) 8_545 4 ? O5 Mn1 N2 84.64(13) . 4 ? N1 Mn1 N2 167.16(16) . 4 ? O8 S1 O8 121.9(7) . 2_565 ? O8 S1 C17 106.0(4) . 2_565 ? O8 S1 C17 107.6(3) 2_565 2_565 ? O8 S1 C17 107.6(3) . . ? O8 S1 C17 106.0(4) 2_565 . ? C17 S1 C17 107.0(4) 2_565 . ? H1W O1 H2W 111.5 . . ? H3W O2 H4W 106.1 . . ? Mn1 O3 H5W 115.3 . . ? Mn1 O3 H6W 129.3 . . ? H5W O3 H6W 109.6 . . ? C20 O4 Mn1 125.6(3) . 8_544 ? C20 O5 Mn1 139.8(3) . . ? C13 O7 Mn1 117.1(3) . . ? C5 N1 C1 111.8(6) . . ? C5 N1 Mn1 128.5(4) . . ? C1 N1 Mn1 118.8(4) . . ? C11 N2 C10 115.8(4) . . ? C11 N2 Mn1 125.0(3) . 4_545 ? C10 N2 Mn1 118.1(3) . 4_545 ? N1 C1 C2 122.7(8) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 122.2(8) . . ? C3 C2 H2 118.9 . . ? C1 C2 H2 118.9 . . ? C4 C3 C2 112.9(7) . . ? C4 C3 C6 125.9(7) . . ? C2 C3 C6 120.8(7) . . ? C3 C4 C5 121.9(7) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? N1 C5 C4 123.4(7) . . ? N1 C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? C7 C6 C3 126.3(7) . . ? C7 C6 H6 116.9 . . ? C3 C6 H6 116.9 . . ? C6 C7 C8 124.9(6) . . ? C6 C7 H7 117.6 . . ? C8 C7 H7 117.6 . . ? C9 C8 C12 116.8(5) . . ? C9 C8 C7 125.1(5) . . ? C12 C8 C7 118.0(5) . . ? C10 C9 C8 120.2(5) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? N2 C10 C9 122.9(5) . . ? N2 C10 H10 118.5 . . ? C9 C10 H10 118.5 . . ? N2 C11 C12 124.3(5) . . ? N2 C11 H11 117.8 . . ? C12 C11 H11 117.8 . . ? C11 C12 C8 119.6(5) . . ? C11 C12 H12 120.2 . . ? C8 C12 H12 120.2 . . ? O6 C13 O7 127.8(6) . . ? O6 C13 C14 115.0(6) . . ? O7 C13 C14 117.1(5) . . ? C19 C14 C15 120.0(5) . . ? C19 C14 C13 121.5(4) . . ? C15 C14 C13 118.4(5) . . ? C16 C15 C14 120.9(7) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C17 C16 C15 118.8(6) . . ? C17 C16 H16 120.6 . . ? C15 C16 H16 120.6 . . ? C16 C17 C18 122.1(6) . . ? C16 C17 S1 119.6(5) . . ? C18 C17 S1 118.3(6) . . ? C19 C18 C17 118.6(6) . . ? C19 C18 H18 120.7 . . ? C17 C18 H18 120.7 . . ? C14 C19 C18 119.6(5) . . ? C14 C19 C20 121.4(4) . . ? C18 C19 C20 119.0(5) . . ? O5 C20 O4 123.5(4) . . ? O5 C20 C19 119.3(4) . . ? O4 C20 C19 117.2(4) . . ? 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 O3 Mn1 O5 C20 27.8(13) . . . . ? O7 Mn1 O5 C20 61.8(5) . . . . ? O4 Mn1 O5 C20 -116.9(5) 8_545 . . . ? N1 Mn1 O5 C20 153.5(5) . . . . ? N2 Mn1 O5 C20 -36.4(5) 4 . . . ? O3 Mn1 O7 C13 170.8(4) . . . . ? O4 Mn1 O7 C13 7.4(14) 8_545 . . . ? O5 Mn1 O7 C13 -4.5(4) . . . . ? N1 Mn1 O7 C13 -91.5(4) . . . . ? N2 Mn1 O7 C13 79.6(4) 4 . . . ? O3 Mn1 N1 C5 -91.8(9) . . . . ? O7 Mn1 N1 C5 -179.0(9) . . . . ? O4 Mn1 N1 C5 7.6(9) 8_545 . . . ? O5 Mn1 N1 C5 95.2(9) . . . . ? N2 Mn1 N1 C5 45.2(14) 4 . . . ? O3 Mn1 N1 C1 76.1(9) . . . . ? O7 Mn1 N1 C1 -11.0(9) . . . . ? O4 Mn1 N1 C1 175.5(9) 8_545 . . . ? O5 Mn1 N1 C1 -96.9(9) . . . . ? N2 Mn1 N1 C1 -146.9(10) 4 . . . ? C5 N1 C1 C2 -26.0(19) . . . . ? Mn1 N1 C1 C2 164.2(11) . . . . ? N1 C1 C2 C3 14(2) . . . . ? C1 C2 C3 C4 2(2) . . . . ? C1 C2 C3 C6 175.5(12) . . . . ? C2 C3 C4 C5 -4.8(19) . . . . ? C6 C3 C4 C5 -177.6(11) . . . . ? C1 N1 C5 C4 23.5(17) . . . . ? Mn1 N1 C5 C4 -168.0(9) . . . . ? C3 C4 C5 N1 -9(2) . . . . ? C4 C3 C6 C7 16.6(16) . . . . ? C2 C3 C6 C7 -155.6(11) . . . . ? C3 C6 C7 C8 176.9(7) . . . . ? C6 C7 C8 C9 9.0(11) . . . . ? C6 C7 C8 C12 -169.0(7) . . . . ? C12 C8 C9 C10 3.7(9) . . . . ? C7 C8 C9 C10 -174.4(6) . . . . ? C11 N2 C10 C9 -4.3(8) . . . . ? Mn1 N2 C10 C9 164.4(5) 4_545 . . . ? C8 C9 C10 N2 1.1(10) . . . . ? C10 N2 C11 C12 2.8(8) . . . . ? Mn1 N2 C11 C12 -165.0(5) 4_545 . . . ? N2 C11 C12 C8 1.9(10) . . . . ? C9 C8 C12 C11 -5.1(9) . . . . ? C7 C8 C12 C11 173.1(6) . . . . ? Mn1 O7 C13 O6 113.2(6) . . . . ? Mn1 O7 C13 C14 -71.4(6) . . . . ? O6 C13 C14 C19 -87.9(7) . . . . ? O7 C13 C14 C19 96.1(7) . . . . ? O6 C13 C14 C15 87.4(8) . . . . ? O7 C13 C14 C15 -88.6(7) . . . . ? C19 C14 C15 C16 -1.2(10) . . . . ? C13 C14 C15 C16 -176.6(7) . . . . ? C14 C15 C16 C17 3.3(12) . . . . ? C15 C16 C17 C18 -3.5(12) . . . . ? C15 C16 C17 S1 175.0(6) . . . . ? O8 S1 C17 C16 179.5(7) . . . . ? O8 S1 C17 C16 -48.7(7) 2_565 . . . ? C17 S1 C17 C16 65.9(6) 2_565 . . . ? O8 S1 C17 C18 -2.0(7) . . . . ? O8 S1 C17 C18 129.9(6) 2_565 . . . ? C17 S1 C17 C18 -115.5(7) 2_565 . . . ? C16 C17 C18 C19 1.6(10) . . . . ? S1 C17 C18 C19 -176.9(4) . . . . ? C15 C14 C19 C18 -0.7(8) . . . . ? C13 C14 C19 C18 174.5(5) . . . . ? C15 C14 C19 C20 178.2(6) . . . . ? C13 C14 C19 C20 -6.6(8) . . . . ? C17 C18 C19 C14 0.6(8) . . . . ? C17 C18 C19 C20 -178.4(5) . . . . ? Mn1 O5 C20 O4 154.2(4) . . . . ? Mn1 O5 C20 C19 -23.7(8) . . . . ? Mn1 O4 C20 O5 -10.4(7) 8_544 . . . ? Mn1 O4 C20 C19 167.5(3) 8_544 . . . ? C14 C19 C20 O5 -32.0(7) . . . . ? C18 C19 C20 O5 146.9(5) . . . . ? C14 C19 C20 O4 150.0(5) . . . . ? C18 C19 C20 O4 -31.1(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1W O6 0.83 2.28 3.092(9) 167.8 3_556 O1 H2W O6 0.83 1.96 2.754(7) 158.8 8_545 O2 H3W O1 0.86 2.30 3.052(13) 146.2 6_655 O2 H4W O7 0.84 2.22 2.909(10) 139.8 8_545 O3 H5W O1 0.83 1.99 2.770(7) 156.1 3_455 O3 H6W O4 0.84 2.06 2.873(6) 164.6 1_556 O3 H6W O5 0.84 2.61 3.009(6) 110.8 8_545 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.921 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.073