# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _publ_section_title ;Supramolecular assembly under the control of the chelating ligand for the MnII / bridging ligands / 3-sulfobenzoate system and catalytic properties for the disproportionation of hydrogen peroxide ; _publ_contact_author_name 'Zhu, Long-Guan' _publ_contact_author_email chezlg@zju.edu.cn loop_ _publ_author_name 'Long-Guan Zhu' 'Xiao-He Miao' # Attachment '- Final_cifdata.cif' data_comp-1 _database_code_depnum_ccdc_archive 'CCDC 745965' #TrackingRef '- Final_cifdata.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H34 Mn N4 O12 S' _chemical_formula_weight 693.58 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 20.510(2) _cell_length_b 7.0178(8) _cell_length_c 23.495(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.4460(10) _cell_angle_gamma 90.00 _cell_volume 3125.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3317 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 21.7 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1444 _exptl_absorpt_coefficient_mu 0.557 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8162 _exptl_absorpt_correction_T_max 0.9464 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker SMART area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 22010 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 25.20 _reflns_number_total 5629 _reflns_number_gt 3969 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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. The aromatic H atoms were positioned geometrically and were included in the refinement in the riding-model approximation [C-H= 0.93 /%A and U~iso~(H)=1.2 U~eq~(C)]. The water H atoms were also placed in calculated positions (O-H=0.85 /%A) with fixed isotropic displacement parameters. The water molecule, O3w, is disordered. ; _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^)+(0.0754P)^2^+2.8350P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5629 _refine_ls_number_parameters 455 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.0898 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1836 _refine_ls_wR_factor_gt 0.1690 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_restrained_S_all 1.239 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean <0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.0000 0.0000 0.0000 0.0349(3) Uani 1 2 d S . . Mn2 Mn 0.5000 0.0000 0.0000 0.0375(3) Uani 1 2 d S . . S1 S -0.27535(8) 0.0783(3) -0.37323(7) 0.0821(6) Uani 1 1 d . . . O1 O -0.10909(15) -0.1237(4) -0.04450(15) 0.0460(8) Uani 1 1 d D . . O2 O -0.04410(19) 0.2793(4) -0.03367(15) 0.0541(9) Uani 1 1 d D . . O3 O 0.61353(18) -0.1103(6) 0.04799(17) 0.0633(10) Uani 1 1 d D . . O4 O 0.5388(2) 0.2814(5) -0.00282(14) 0.0582(10) Uani 1 1 d D . . O5 O -0.2352(2) 0.0787(6) -0.10264(19) 0.0816(12) Uani 1 1 d D . . O6 O -0.2496(2) 0.3289(5) -0.15990(16) 0.0642(10) Uani 1 1 d . . . O7 O -0.2771(3) 0.2870(7) -0.3683(2) 0.1018(16) Uani 1 1 d D . . O8 O -0.34597(19) 0.0032(6) -0.41746(19) 0.0761(12) Uani 1 1 d . . . O9 O -0.2164(3) 0.0085(12) -0.3828(3) 0.158(3) Uani 1 1 d . . . O1W O -0.1634(2) -0.0148(5) -0.54813(19) 0.0638(10) Uani 1 1 d D . . O2W O 0.2409(4) -0.6631(8) -0.0071(2) 0.1110(18) Uani 1 1 d D . . O3W' O 0.2659(3) -0.0962(12) -0.0035(3) 0.158(4) Uani 0.939(10) 1 d PU A 1 O3W O 0.262(3) 0.079(5) -0.0460(18) 0.07(2) Uani 0.061(10) 1 d PU A 2 N1 N 0.01225(19) -0.0477(5) -0.08668(16) 0.0389(8) Uani 1 1 d . . . N2 N 0.0297(2) -0.0781(6) -0.36834(18) 0.0509(10) Uani 1 1 d . . . N3 N 0.4955(2) -0.0559(5) -0.09269(16) 0.0418(9) Uani 1 1 d . . . N4 N 0.4781(3) -0.0679(6) -0.38747(18) 0.0559(11) Uani 1 1 d . . . C1 C -0.0463(2) -0.0802(7) -0.1408(2) 0.0442(11) Uani 1 1 d . . . H1 H -0.0894 -0.0996 -0.1372 0.053 Uiso 1 1 calc R . . C2 C -0.0456(2) -0.0858(7) -0.1963(2) 0.0433(11) Uani 1 1 d . . . H2 H -0.0858 -0.1067 -0.2315 0.052 Uiso 1 1 calc R . . C3 C 0.0205(2) -0.0576(6) -0.19757(18) 0.0343(9) Uani 1 1 d . . . C4 C 0.0817(3) -0.0258(7) -0.1421(2) 0.0522(13) Uani 1 1 d . . . H4 H 0.1255 -0.0076 -0.1444 0.063 Uiso 1 1 calc R . . C5 C 0.0759(2) -0.0223(7) -0.0884(2) 0.0500(12) Uani 1 1 d . . . H5 H 0.1152 -0.0025 -0.0524 0.060 Uiso 1 1 calc R . . C6 C 0.0242(2) -0.0610(6) -0.25663(19) 0.0357(9) Uani 1 1 d . . . C7 C -0.0380(3) -0.0358(7) -0.3125(2) 0.0467(11) Uani 1 1 d . . . H7 H -0.0815 -0.0121 -0.3102 0.056 Uiso 1 1 calc R . . C8 C -0.0328(3) -0.0464(7) -0.3660(2) 0.0526(12) Uani 1 1 d . . . H8 H -0.0725 -0.0319 -0.4021 0.063 Uiso 1 1 calc R . . C9 C 0.0893(3) -0.1008(7) -0.3142(2) 0.0543(13) Uani 1 1 d . . . H9 H 0.1320 -0.1236 -0.3182 0.065 Uiso 1 1 calc R . . C10 C 0.0898(2) -0.0925(7) -0.2582(2) 0.0479(11) Uani 1 1 d . . . H10 H 0.1306 -0.1065 -0.2230 0.058 Uiso 1 1 calc R . . C11 C 0.4334(2) -0.0982(6) -0.1433(2) 0.0453(11) Uani 1 1 d . . . H11 H 0.3928 -0.1224 -0.1357 0.054 Uiso 1 1 calc R . . C12 C 0.4286(2) -0.1060(6) -0.20097(19) 0.0434(11) Uani 1 1 d . . . H12 H 0.3866 -0.1343 -0.2337 0.052 Uiso 1 1 calc R . . C13 C 0.4899(2) -0.0693(6) -0.20881(18) 0.0360(9) Uani 1 1 d . . . C14 C 0.5554(2) -0.0311(6) -0.1559(2) 0.0434(11) Uani 1 1 d . . . H14 H 0.5972 -0.0116 -0.1620 0.052 Uiso 1 1 calc R . . C15 C 0.5556(2) -0.0243(6) -0.0998(2) 0.0449(11) Uani 1 1 d . . . H15 H 0.5968 0.0020 -0.0661 0.054 Uiso 1 1 calc R . . C16 C 0.4857(2) -0.0675(6) -0.27044(19) 0.0380(10) Uani 1 1 d . . . C17 C 0.4195(3) -0.0313(6) -0.3235(2) 0.0477(12) Uani 1 1 d . . . H17 H 0.3782 -0.0072 -0.3172 0.057 Uiso 1 1 calc R . . C18 C 0.4187(3) -0.0330(7) -0.3797(2) 0.0571(13) Uani 1 1 d . . . H18 H 0.3771 -0.0100 -0.4134 0.068 Uiso 1 1 calc R . . C19 C 0.5409(3) -0.1004(7) -0.3365(2) 0.0531(13) Uani 1 1 d . . . H19 H 0.5815 -0.1232 -0.3442 0.064 Uiso 1 1 calc R . . C20 C 0.5469(2) -0.1013(6) -0.2785(2) 0.0428(10) Uani 1 1 d . . . H20 H 0.5896 -0.1231 -0.2459 0.051 Uiso 1 1 calc R . . C21 C -0.2461(2) 0.1547(7) -0.1513(2) 0.0509(12) Uani 1 1 d . . . C22 C -0.2517(2) 0.0252(7) -0.2020(3) 0.0542(13) Uani 1 1 d . . . C23 C -0.2580(2) 0.1004(7) -0.2563(2) 0.0485(12) Uani 1 1 d . . . H23 H -0.2597 0.2318 -0.2619 0.058 Uiso 1 1 calc R . . C24 C -0.2619(2) -0.0172(8) -0.3022(3) 0.0632(15) Uani 1 1 d . . . C25 C -0.2590(3) -0.2140(10) -0.2942(3) 0.089(2) Uani 1 1 d . . . H25 H -0.2612 -0.2933 -0.3266 0.107 Uiso 1 1 calc R . . C26 C -0.2531(3) -0.2878(8) -0.2415(4) 0.097(3) Uani 1 1 d . . . H26 H -0.2510 -0.4193 -0.2362 0.116 Uiso 1 1 calc R . . C27 C -0.2502(3) -0.1720(8) -0.1950(3) 0.0731(17) Uani 1 1 d . . . H27 H -0.2472 -0.2241 -0.1577 0.088 Uiso 1 1 calc R . . H1C H -0.190(2) 0.059(7) -0.5760(18) 0.076 Uiso 1 1 d D . . H1D H -0.185(2) -0.047(7) -0.5255(19) 0.076 Uiso 1 1 d D . . H2B H -0.075(2) 0.334(6) -0.0245(19) 0.065 Uiso 1 1 d D . . H2A H -0.041(2) 0.330(6) -0.0652(14) 0.065 Uiso 1 1 d D . . H2C H 0.252(4) -0.779(4) -0.001(3) 0.135 Uiso 1 1 d D . . H2D H 0.223(4) -0.642(9) -0.0454(9) 0.135 Uiso 1 1 d D . . H4B H 0.530(2) 0.346(6) -0.0352(12) 0.070 Uiso 1 1 d D . . H4A H 0.5782(15) 0.316(7) 0.0237(15) 0.070 Uiso 1 1 d D . . H1A H -0.1180(19) -0.2426(17) -0.046(2) 0.055 Uiso 1 1 d D . . H1B H -0.1475(12) -0.063(5) -0.062(2) 0.055 Uiso 1 1 d D . . H3B H 0.620(2) -0.2299(17) 0.049(3) 0.076 Uiso 1 1 d D . . H3A H 0.6523(15) -0.057(6) 0.052(3) 0.076 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 Mn1 0.0414(5) 0.0368(5) 0.0311(5) 0.0026(4) 0.0190(4) 0.0003(4) Mn2 0.0493(6) 0.0388(5) 0.0260(5) 0.0015(4) 0.0161(4) 0.0011(4) S1 0.0424(8) 0.1308(16) 0.0717(10) -0.0382(10) 0.0202(7) -0.0063(9) O1 0.0459(18) 0.0449(19) 0.0496(19) 0.0039(15) 0.0208(16) -0.0030(14) O2 0.082(3) 0.0448(19) 0.057(2) 0.0188(15) 0.0500(19) 0.0209(17) O3 0.057(2) 0.076(3) 0.055(2) 0.010(2) 0.0203(19) 0.0165(19) O4 0.096(3) 0.048(2) 0.0322(17) 0.0009(15) 0.0262(18) -0.0199(19) O5 0.090(3) 0.080(3) 0.088(3) 0.028(2) 0.049(3) 0.021(2) O6 0.085(3) 0.052(2) 0.060(2) 0.0006(18) 0.032(2) 0.0087(19) O7 0.127(4) 0.111(4) 0.087(3) -0.028(3) 0.061(3) -0.055(3) O8 0.050(2) 0.086(3) 0.073(3) -0.015(2) 0.0027(19) 0.0017(19) O9 0.065(3) 0.310(9) 0.102(4) -0.056(5) 0.037(3) 0.038(4) O1W 0.067(2) 0.057(2) 0.078(3) 0.0098(18) 0.040(2) 0.0025(18) O2W 0.155(5) 0.111(4) 0.110(4) -0.008(3) 0.098(4) -0.003(4) O3W' 0.084(4) 0.165(6) 0.203(7) -0.077(5) 0.031(4) 0.006(4) O3W 0.06(2) 0.07(2) 0.06(2) 0.048(10) 0.021(12) -0.014(10) N1 0.045(2) 0.042(2) 0.036(2) -0.0001(15) 0.0232(17) 0.0023(16) N2 0.072(3) 0.049(2) 0.045(2) -0.0105(19) 0.037(2) -0.005(2) N3 0.059(2) 0.038(2) 0.035(2) -0.0030(16) 0.0239(19) -0.0036(17) N4 0.088(3) 0.050(2) 0.043(2) -0.0061(19) 0.040(2) -0.004(2) C1 0.038(2) 0.058(3) 0.043(3) -0.001(2) 0.023(2) -0.002(2) C2 0.039(2) 0.056(3) 0.036(2) -0.006(2) 0.016(2) -0.002(2) C3 0.041(2) 0.031(2) 0.035(2) -0.0022(17) 0.0193(19) 0.0036(17) C4 0.041(3) 0.081(4) 0.042(3) -0.008(2) 0.024(2) -0.007(2) C5 0.042(3) 0.075(4) 0.034(2) -0.005(2) 0.016(2) -0.002(2) C6 0.044(2) 0.032(2) 0.036(2) -0.0054(18) 0.021(2) 0.0002(18) C7 0.046(3) 0.059(3) 0.041(3) -0.007(2) 0.023(2) 0.000(2) C8 0.060(3) 0.062(3) 0.034(3) -0.008(2) 0.016(2) -0.008(2) C9 0.062(3) 0.059(3) 0.058(3) -0.005(2) 0.041(3) 0.004(3) C10 0.050(3) 0.059(3) 0.038(3) -0.002(2) 0.021(2) 0.010(2) C11 0.055(3) 0.049(3) 0.039(3) -0.004(2) 0.026(2) -0.010(2) C12 0.052(3) 0.045(3) 0.034(2) -0.0092(19) 0.017(2) -0.013(2) C13 0.049(3) 0.028(2) 0.035(2) -0.0037(17) 0.021(2) -0.0014(19) C14 0.044(3) 0.046(3) 0.045(3) -0.006(2) 0.022(2) 0.001(2) C15 0.047(3) 0.053(3) 0.032(2) -0.006(2) 0.012(2) -0.001(2) C16 0.054(3) 0.028(2) 0.037(2) -0.0065(18) 0.023(2) -0.0054(19) C17 0.057(3) 0.051(3) 0.041(3) -0.002(2) 0.025(2) 0.004(2) C18 0.076(4) 0.060(3) 0.038(3) -0.002(2) 0.025(3) 0.005(3) C19 0.072(4) 0.050(3) 0.056(3) -0.010(2) 0.045(3) -0.010(3) C20 0.050(3) 0.042(3) 0.042(3) -0.003(2) 0.023(2) -0.004(2) C21 0.041(3) 0.055(3) 0.057(3) 0.017(3) 0.019(2) 0.011(2) C22 0.032(2) 0.039(3) 0.078(4) 0.001(3) 0.006(2) 0.002(2) C23 0.036(3) 0.044(3) 0.061(3) -0.008(2) 0.013(2) 0.003(2) C24 0.033(3) 0.064(4) 0.079(4) -0.031(3) 0.006(2) 0.001(2) C25 0.062(4) 0.077(5) 0.089(5) -0.039(4) -0.015(4) 0.021(3) C26 0.080(5) 0.037(3) 0.117(6) -0.017(4) -0.026(4) 0.007(3) C27 0.050(3) 0.047(3) 0.089(4) 0.006(3) -0.010(3) 0.000(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 Mn1 N1 2.171(3) 3 ? Mn1 N1 2.171(3) . ? Mn1 O2 2.177(3) . ? Mn1 O2 2.177(3) 3 ? Mn1 O1 2.251(3) 3 ? Mn1 O1 2.251(3) . ? Mn2 O4 2.139(3) . ? Mn2 O4 2.139(3) 3_655 ? Mn2 N3 2.180(3) . ? Mn2 N3 2.180(3) 3_655 ? Mn2 O3 2.299(3) . ? Mn2 O3 2.299(3) 3_655 ? S1 O9 1.400(5) . ? S1 O7 1.470(5) . ? S1 O8 1.519(4) . ? S1 C24 1.720(7) . ? O1 H1A 0.851(11) . ? O1 H1B 0.85(3) . ? O2 H2B 0.84(4) . ? O2 H2A 0.85(4) . ? O3 H3B 0.848(11) . ? O3 H3A 0.85(4) . ? O4 H4B 0.84(3) . ? O4 H4A 0.85(4) . ? O5 C21 1.202(6) . ? O6 C21 1.237(6) . ? O1W H1C 0.85(4) . ? O1W H1D 0.85(4) . ? O2W H2C 0.84(4) . ? O2W H2D 0.846(11) . ? N1 C5 1.334(6) . ? N1 C1 1.394(6) . ? N2 C8 1.322(6) . ? N2 C9 1.396(6) . ? N3 C15 1.324(6) . ? N3 C11 1.403(6) . ? N4 C18 1.320(7) . ? N4 C19 1.403(7) . ? C1 C2 1.310(6) . ? C1 H1 0.9300 . ? C2 C3 1.380(6) . ? C2 H2 0.9300 . ? C3 C6 1.419(5) . ? C3 C4 1.440(6) . ? C4 C5 1.312(6) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C10 1.379(6) . ? C6 C7 1.450(6) . ? C7 C8 1.304(6) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C10 1.312(6) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.322(6) . ? C11 H11 0.9300 . ? C12 C13 1.364(6) . ? C12 H12 0.9300 . ? C13 C16 1.417(5) . ? C13 C14 1.465(6) . ? C14 C15 1.317(6) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C20 1.362(6) . ? C16 C17 1.472(6) . ? C17 C18 1.315(6) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.319(6) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.469(7) . ? C22 C23 1.339(7) . ? C22 C27 1.392(7) . ? C23 C24 1.337(7) . ? C23 H23 0.9300 . ? C24 C25 1.392(9) . ? C25 C26 1.304(10) . ? C25 H25 0.9300 . ? C26 C27 1.345(9) . ? C26 H26 0.9300 . ? C27 H27 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 N1 Mn1 N1 180.00 3 . ? N1 Mn1 O2 91.22(12) 3 . ? N1 Mn1 O2 88.78(12) . . ? N1 Mn1 O2 88.78(12) 3 3 ? N1 Mn1 O2 91.22(12) . 3 ? O2 Mn1 O2 180.0 . 3 ? N1 Mn1 O1 87.44(12) 3 3 ? N1 Mn1 O1 92.56(12) . 3 ? O2 Mn1 O1 91.31(13) . 3 ? O2 Mn1 O1 88.69(13) 3 3 ? N1 Mn1 O1 92.56(12) 3 . ? N1 Mn1 O1 87.44(12) . . ? O2 Mn1 O1 88.69(13) . . ? O2 Mn1 O1 91.31(13) 3 . ? O1 Mn1 O1 180.00 3 . ? O4 Mn2 O4 180.0 . 3_655 ? O4 Mn2 N3 90.55(12) . . ? O4 Mn2 N3 89.45(12) 3_655 . ? O4 Mn2 N3 89.45(12) . 3_655 ? O4 Mn2 N3 90.55(12) 3_655 3_655 ? N3 Mn2 N3 180.00 . 3_655 ? O4 Mn2 O3 90.42(15) . . ? O4 Mn2 O3 89.58(15) 3_655 . ? N3 Mn2 O3 94.46(14) . . ? N3 Mn2 O3 85.54(14) 3_655 . ? O4 Mn2 O3 89.58(15) . 3_655 ? O4 Mn2 O3 90.42(15) 3_655 3_655 ? N3 Mn2 O3 85.54(14) . 3_655 ? N3 Mn2 O3 94.46(14) 3_655 3_655 ? O3 Mn2 O3 180.0 . 3_655 ? O9 S1 O7 114.2(4) . . ? O9 S1 O8 115.2(3) . . ? O7 S1 O8 110.8(3) . . ? O9 S1 C24 101.0(3) . . ? O7 S1 C24 108.1(3) . . ? O8 S1 C24 106.7(3) . . ? Mn1 O1 H1A 124(3) . . ? Mn1 O1 H1B 127(3) . . ? H1A O1 H1B 109(4) . . ? Mn1 O2 H2B 125(3) . . ? Mn1 O2 H2A 122(3) . . ? H2B O2 H2A 111(4) . . ? Mn2 O3 H3B 118(3) . . ? Mn2 O3 H3A 129(3) . . ? H3B O3 H3A 108(4) . . ? Mn2 O4 H4B 125(3) . . ? Mn2 O4 H4A 120(3) . . ? H4B O4 H4A 109(4) . . ? H1C O1W H1D 108(4) . . ? H2C O2W H2D 109(6) . . ? C5 N1 C1 120.4(4) . . ? C5 N1 Mn1 118.3(3) . . ? C1 N1 Mn1 120.8(3) . . ? C8 N2 C9 120.5(4) . . ? C15 N3 C11 121.1(4) . . ? C15 N3 Mn2 114.2(3) . . ? C11 N3 Mn2 124.2(3) . . ? C18 N4 C19 120.5(4) . . ? C2 C1 N1 125.4(4) . . ? C2 C1 H1 117.3 . . ? N1 C1 H1 117.3 . . ? C1 C2 C3 113.7(4) . . ? C1 C2 H2 123.1 . . ? C3 C2 H2 123.1 . . ? C2 C3 C6 116.0(4) . . ? C2 C3 C4 121.7(4) . . ? C6 C3 C4 122.3(4) . . ? C5 C4 C3 120.4(4) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 N1 118.4(4) . . ? C4 C5 H5 120.8 . . ? N1 C5 H5 120.8 . . ? C10 C6 C3 116.6(4) . . ? C10 C6 C7 121.7(4) . . ? C3 C6 C7 121.8(4) . . ? C8 C7 C6 119.9(4) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 N2 119.1(5) . . ? C7 C8 H8 120.4 . . ? N2 C8 H8 120.4 . . ? C10 C9 N2 125.3(4) . . ? C10 C9 H9 117.4 . . ? N2 C9 H9 117.4 . . ? C9 C10 C6 113.6(4) . . ? C9 C10 H10 123.2 . . ? C6 C10 H10 123.2 . . ? C12 C11 N3 124.4(4) . . ? C12 C11 H11 117.8 . . ? N3 C11 H11 117.8 . . ? C11 C12 C13 114.8(4) . . ? C11 C12 H12 122.6 . . ? C13 C12 H12 122.6 . . ? C12 C13 C16 116.1(4) . . ? C12 C13 C14 121.0(4) . . ? C16 C13 C14 122.9(4) . . ? C15 C14 C13 120.4(4) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 N3 118.3(4) . . ? C14 C15 H15 120.8 . . ? N3 C15 H15 120.8 . . ? C20 C16 C13 116.2(4) . . ? C20 C16 C17 120.8(4) . . ? C13 C16 C17 123.0(4) . . ? C18 C17 C16 120.2(5) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 N4 118.8(5) . . ? C17 C18 H18 120.6 . . ? N4 C18 H18 120.6 . . ? C20 C19 N4 125.1(4) . . ? C20 C19 H19 117.4 . . ? N4 C19 H19 117.4 . . ? C19 C20 C16 114.6(5) . . ? C19 C20 H20 122.7 . . ? C16 C20 H20 122.7 . . ? O5 C21 O6 125.0(5) . . ? O5 C21 C22 115.2(5) . . ? O6 C21 C22 119.8(5) . . ? C23 C22 C27 119.7(5) . . ? C23 C22 C21 118.5(4) . . ? C27 C22 C21 121.8(6) . . ? C24 C23 C22 118.6(5) . . ? C24 C23 H23 120.7 . . ? C22 C23 H23 120.7 . . ? C23 C24 C25 121.1(6) . . ? C23 C24 S1 118.7(5) . . ? C25 C24 S1 120.1(5) . . ? C26 C25 C24 120.4(6) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C27 119.3(6) . . ? C25 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? C26 C27 C22 120.8(6) . . ? C26 C27 H27 119.6 . . ? C22 C27 H27 119.6 . . ? 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 O2 Mn1 N1 C5 100.1(3) . . . . ? O2 Mn1 N1 C5 -79.9(3) 3 . . . ? O1 Mn1 N1 C5 8.8(3) 3 . . . ? O1 Mn1 N1 C5 -171.2(3) . . . . ? O2 Mn1 N1 C1 -71.9(3) . . . . ? O2 Mn1 N1 C1 108.1(3) 3 . . . ? O1 Mn1 N1 C1 -163.2(3) 3 . . . ? O1 Mn1 N1 C1 16.8(3) . . . . ? O4 Mn2 N3 C15 53.9(3) . . . . ? O4 Mn2 N3 C15 -126.1(3) 3_655 . . . ? O3 Mn2 N3 C15 -36.6(3) . . . . ? O3 Mn2 N3 C15 143.4(3) 3_655 . . . ? O4 Mn2 N3 C11 -118.3(4) . . . . ? O4 Mn2 N3 C11 61.7(4) 3_655 . . . ? O3 Mn2 N3 C11 151.3(3) . . . . ? O3 Mn2 N3 C11 -28.7(3) 3_655 . . . ? C5 N1 C1 C2 -1.2(7) . . . . ? Mn1 N1 C1 C2 170.6(4) . . . . ? N1 C1 C2 C3 0.6(7) . . . . ? C1 C2 C3 C6 -179.6(4) . . . . ? C1 C2 C3 C4 0.1(7) . . . . ? C2 C3 C4 C5 -0.2(7) . . . . ? C6 C3 C4 C5 179.5(5) . . . . ? C3 C4 C5 N1 -0.4(7) . . . . ? C1 N1 C5 C4 1.0(7) . . . . ? Mn1 N1 C5 C4 -171.0(4) . . . . ? C2 C3 C6 C10 -160.5(4) . . . . ? C4 C3 C6 C10 19.8(6) . . . . ? C2 C3 C6 C7 18.5(6) . . . . ? C4 C3 C6 C7 -161.2(4) . . . . ? C10 C6 C7 C8 1.3(7) . . . . ? C3 C6 C7 C8 -177.6(4) . . . . ? C6 C7 C8 N2 -0.7(7) . . . . ? C9 N2 C8 C7 0.3(7) . . . . ? C8 N2 C9 C10 -0.4(8) . . . . ? N2 C9 C10 C6 0.9(7) . . . . ? C3 C6 C10 C9 177.7(4) . . . . ? C7 C6 C10 C9 -1.3(7) . . . . ? C15 N3 C11 C12 -1.6(7) . . . . ? Mn2 N3 C11 C12 170.1(4) . . . . ? N3 C11 C12 C13 0.1(7) . . . . ? C11 C12 C13 C16 -177.0(4) . . . . ? C11 C12 C13 C14 1.9(6) . . . . ? C12 C13 C14 C15 -2.7(7) . . . . ? C16 C13 C14 C15 176.2(4) . . . . ? C13 C14 C15 N3 1.1(7) . . . . ? C11 N3 C15 C14 0.9(6) . . . . ? Mn2 N3 C15 C14 -171.6(3) . . . . ? C12 C13 C16 C20 -156.7(4) . . . . ? C14 C13 C16 C20 24.4(6) . . . . ? C12 C13 C16 C17 23.4(6) . . . . ? C14 C13 C16 C17 -155.5(4) . . . . ? C20 C16 C17 C18 0.6(7) . . . . ? C13 C16 C17 C18 -179.4(4) . . . . ? C16 C17 C18 N4 0.1(7) . . . . ? C19 N4 C18 C17 -0.7(7) . . . . ? C18 N4 C19 C20 0.6(8) . . . . ? N4 C19 C20 C16 0.1(7) . . . . ? C13 C16 C20 C19 179.3(4) . . . . ? C17 C16 C20 C19 -0.7(6) . . . . ? O5 C21 C22 C23 -174.6(4) . . . . ? O6 C21 C22 C23 2.3(7) . . . . ? O5 C21 C22 C27 5.0(7) . . . . ? O6 C21 C22 C27 -178.0(5) . . . . ? C27 C22 C23 C24 -0.8(7) . . . . ? C21 C22 C23 C24 178.8(4) . . . . ? C22 C23 C24 C25 -0.4(7) . . . . ? C22 C23 C24 S1 176.1(4) . . . . ? O9 S1 C24 C23 122.7(5) . . . . ? O7 S1 C24 C23 2.6(5) . . . . ? O8 S1 C24 C23 -116.6(4) . . . . ? O9 S1 C24 C25 -60.7(6) . . . . ? O7 S1 C24 C25 179.2(5) . . . . ? O8 S1 C24 C25 60.0(5) . . . . ? C23 C24 C25 C26 0.7(9) . . . . ? S1 C24 C25 C26 -175.8(5) . . . . ? C24 C25 C26 C27 0.3(10) . . . . ? C25 C26 C27 C22 -1.5(10) . . . . ? C23 C22 C27 C26 1.8(8) . . . . ? C21 C22 C27 C26 -177.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.438 _refine_diff_density_min -0.755 _refine_diff_density_rms 0.073 data_comp-2 _database_code_depnum_ccdc_archive 'CCDC 745966' #TrackingRef '- Final_cifdata.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H30 Mn N4 O8 S' _chemical_formula_weight 673.59 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7416(10) _cell_length_b 11.9663(10) _cell_length_c 12.9264(11) _cell_angle_alpha 69.0420(10) _cell_angle_beta 89.5550(10) _cell_angle_gamma 67.9040(10) _cell_volume 1554.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 4486 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 26.8 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 698 _exptl_absorpt_coefficient_mu 0.549 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.841 _exptl_absorpt_correction_T_max 0.875 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker SMART area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 11460 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.20 _reflns_number_total 5549 _reflns_number_gt 5153 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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. The aromatic H atoms were positioned geometrically and were included in the refinement in the riding-model approximation [C-H= 0.93 /%A and U~iso~(H)=1.2 U~eq~(C)]. The water H atoms were also placed in calculated positions (O-H=0.85 /%A) with fixed isotropic displacement parameters. ; _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^)+(0.0426P)^2^+2.2165P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5549 _refine_ls_number_parameters 424 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0610 _refine_ls_wR_factor_ref 0.1324 _refine_ls_wR_factor_gt 0.1294 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.138 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean <0.001 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 0.69708(4) 0.94493(4) 0.47305(4) 0.02740(15) Uani 1 1 d . . . S1 S 0.84388(8) 1.30961(9) 0.62560(10) 0.0485(3) Uani 1 1 d . . . O1 O 0.5818(2) 1.0619(2) 0.5528(2) 0.0409(6) Uani 1 1 d . . . O2 O 0.3866(2) 1.1669(2) 0.5683(2) 0.0428(6) Uani 1 1 d . . . O3 O 0.9161(2) 1.1906(3) 0.6132(3) 0.0783(11) Uani 1 1 d . . . O4 O 0.8419(3) 1.4220(4) 0.5399(5) 0.137(2) Uani 1 1 d . . . O5 O 0.8781(3) 1.3076(5) 0.7321(4) 0.1193(17) Uani 1 1 d . . . O6 O 0.8525(2) 1.0001(2) 0.5088(2) 0.0386(6) Uani 1 1 d D . . O7 O 0.8373(2) 0.8432(3) 0.3896(3) 0.0490(7) Uani 1 1 d D . . N1 N 0.6105(3) 1.1181(3) 0.3064(2) 0.0380(7) Uani 1 1 d . . . N2 N 0.0715(3) 1.8254(4) -0.3200(3) 0.0620(10) Uani 1 1 d . . . N3 N 0.7692(3) 0.7895(3) 0.6469(2) 0.0376(6) Uani 1 1 d . . . N4 N 0.6576(4) 0.8822(4) 1.0282(3) 0.0701(11) Uani 1 1 d . . . C1 C 0.5953(4) 1.0931(4) 0.2164(3) 0.0526(10) Uani 1 1 d . . . H1 H 0.6359 1.0078 0.2208 0.063 Uiso 1 1 calc R . . C2 C 0.5228(4) 1.1863(4) 0.1171(3) 0.0533(10) Uani 1 1 d . . . H2 H 0.5159 1.1631 0.0567 0.064 Uiso 1 1 calc R . . C3 C 0.4601(3) 1.3141(4) 0.1069(3) 0.0440(9) Uani 1 1 d . . . C4 C 0.4795(4) 1.3403(4) 0.1990(3) 0.0544(11) Uani 1 1 d . . . H4 H 0.4420 1.4253 0.1960 0.065 Uiso 1 1 calc R . . C5 C 0.5538(4) 1.2421(4) 0.2954(3) 0.0498(10) Uani 1 1 d . . . H5 H 0.5649 1.2635 0.3559 0.060 Uiso 1 1 calc R . . C6 C 0.3779(4) 1.4109(4) 0.0021(3) 0.0558(10) Uani 1 1 d . . . H6 H 0.3734 1.3814 -0.0546 0.067 Uiso 1 1 calc R . . C7 C 0.3115(4) 1.5324(4) -0.0194(3) 0.0575(11) Uani 1 1 d . . . H7 H 0.3173 1.5619 0.0371 0.069 Uiso 1 1 calc R . . C8 C 0.2275(3) 1.6297(4) -0.1229(3) 0.0518(10) Uani 1 1 d . . . C9 C 0.2004(4) 1.6013(4) -0.2127(4) 0.0581(11) Uani 1 1 d . . . H9 H 0.2338 1.5157 -0.2087 0.070 Uiso 1 1 calc R . . C10 C 0.1232(4) 1.7012(4) -0.3084(3) 0.0607(11) Uani 1 1 d . . . H10 H 0.1068 1.6800 -0.3676 0.073 Uiso 1 1 calc R . . C11 C 0.1722(4) 1.7582(4) -0.1348(4) 0.0622(12) Uani 1 1 d . . . H11 H 0.1863 1.7825 -0.0770 0.075 Uiso 1 1 calc R . . C12 C 0.0960(4) 1.8508(4) -0.2326(4) 0.0651(12) Uani 1 1 d . . . H12 H 0.0593 1.9367 -0.2378 0.078 Uiso 1 1 calc R . . C13 C 0.8116(4) 0.6620(3) 0.6658(3) 0.0455(9) Uani 1 1 d . . . H13 H 0.7970 0.6383 0.6077 0.055 Uiso 1 1 calc R . . C14 C 0.8753(4) 0.5650(3) 0.7663(3) 0.0472(9) Uani 1 1 d . . . H14 H 0.9017 0.4780 0.7753 0.057 Uiso 1 1 calc R . . C15 C 0.9005(3) 0.5960(3) 0.8546(3) 0.0412(8) Uani 1 1 d . . . C16 C 0.8517(4) 0.7278(3) 0.8371(3) 0.0444(9) Uani 1 1 d . . . H16 H 0.8622 0.7539 0.8947 0.053 Uiso 1 1 calc R . . C17 C 0.7877(3) 0.8192(3) 0.7339(3) 0.0429(8) Uani 1 1 d . . . H17 H 0.7555 0.9068 0.7242 0.051 Uiso 1 1 calc R . . C18 C 0.9767(3) 0.4921(4) 0.9587(3) 0.0456(9) Uani 1 1 d . . . H18 H 0.9936 0.4067 0.9669 0.055 Uiso 1 1 calc R . . C19 C 0.7615(5) 0.8254(5) 1.1007(4) 0.0662(12) Uani 1 1 d . . . H19 H 0.7693 0.7542 1.1652 0.079 Uiso 1 1 calc R . . C20 C 0.8581(4) 0.8651(5) 1.0864(4) 0.0634(12) Uani 1 1 d . . . H20 H 0.9287 0.8211 1.1401 0.076 Uiso 1 1 calc R . . C21 C 0.8497(4) 0.9715(4) 0.9911(4) 0.0572(11) Uani 1 1 d . . . C22 C 0.7412(4) 1.0308(5) 0.9165(4) 0.0667(12) Uani 1 1 d . . . H22 H 0.7299 1.1030 0.8516 0.080 Uiso 1 1 calc R . . C23 C 0.6502(4) 0.9837(5) 0.9379(4) 0.0711(13) Uani 1 1 d . . . H23 H 0.5786 1.0256 0.8856 0.085 Uiso 1 1 calc R . . C24 C 0.9470(4) 1.0221(5) 0.9678(4) 0.0647(12) Uani 1 1 d . . . H24 H 0.9322 1.0928 0.9007 0.078 Uiso 1 1 calc R . . C25 C 0.4985(3) 1.1500(3) 0.5721(2) 0.0291(7) Uani 1 1 d . . . C26 C 0.5344(3) 1.2444(3) 0.6020(3) 0.0317(7) Uani 1 1 d . . . C27 C 0.6565(3) 1.2346(3) 0.6007(3) 0.0294(7) Uani 1 1 d . . . H27 H 0.7157 1.1689 0.5833 0.035 Uiso 1 1 calc R . . C28 C 0.6891(3) 1.3223(3) 0.6252(3) 0.0346(7) Uani 1 1 d . . . C29 C 0.6012(4) 1.4214(4) 0.6493(4) 0.0582(11) Uani 1 1 d . . . H29 H 0.6234 1.4816 0.6642 0.070 Uiso 1 1 calc R . . C30 C 0.4808(4) 1.4309(5) 0.6513(5) 0.0730(15) Uani 1 1 d . . . H30 H 0.4220 1.4969 0.6685 0.088 Uiso 1 1 calc R . . C31 C 0.4467(3) 1.3425(4) 0.6278(4) 0.0540(11) Uani 1 1 d . . . H31 H 0.3653 1.3491 0.6293 0.065 Uiso 1 1 calc R . . O1W O 0.8885(3) 1.6046(3) 0.3670(3) 0.0640(8) Uani 1 1 d D . . H7B H 0.9107(15) 0.840(3) 0.391(3) 0.050 Uiso 1 1 d D . . H6B H 0.870(3) 1.059(3) 0.463(2) 0.050 Uiso 1 1 d D . . H6A H 0.912(2) 0.951(3) 0.562(2) 0.050 Uiso 1 1 d D . . H7A H 0.839(3) 0.771(2) 0.391(3) 0.050 Uiso 1 1 d D . . H1WA H 0.877(4) 1.542(3) 0.416(3) 0.090 Uiso 1 1 d D . . H1WB H 0.9660(13) 1.584(4) 0.368(4) 0.090 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 Mn1 0.0220(2) 0.0260(3) 0.0315(3) -0.0092(2) -0.00057(18) -0.00824(19) S1 0.0278(4) 0.0389(5) 0.0842(7) -0.0251(5) 0.0033(4) -0.0176(4) O1 0.0330(12) 0.0394(13) 0.0581(15) -0.0291(12) 0.0065(11) -0.0127(11) O2 0.0274(12) 0.0455(14) 0.0659(17) -0.0287(13) 0.0043(11) -0.0183(11) O3 0.0322(14) 0.0646(19) 0.165(3) -0.070(2) 0.0230(18) -0.0231(14) O4 0.053(2) 0.072(2) 0.215(5) 0.024(3) 0.037(3) -0.0262(19) O5 0.065(2) 0.160(4) 0.165(4) -0.111(4) -0.020(2) -0.031(3) O6 0.0292(12) 0.0372(13) 0.0440(14) -0.0059(11) -0.0039(10) -0.0164(11) O7 0.0302(13) 0.0532(16) 0.0791(19) -0.0386(15) 0.0169(13) -0.0205(12) N1 0.0374(15) 0.0339(15) 0.0369(16) -0.0110(13) -0.0022(12) -0.0104(13) N2 0.056(2) 0.052(2) 0.047(2) 0.0073(17) -0.0072(16) -0.0134(18) N3 0.0409(16) 0.0322(15) 0.0358(15) -0.0093(12) 0.0017(12) -0.0140(13) N4 0.063(2) 0.090(3) 0.068(3) -0.032(2) 0.011(2) -0.040(2) C1 0.060(3) 0.037(2) 0.050(2) -0.0172(18) -0.0040(19) -0.0080(18) C2 0.063(3) 0.049(2) 0.039(2) -0.0146(18) -0.0095(19) -0.016(2) C3 0.0366(19) 0.046(2) 0.0362(19) -0.0061(16) -0.0016(15) -0.0117(16) C4 0.067(3) 0.0279(19) 0.046(2) -0.0073(17) 0.0041(19) -0.0012(18) C5 0.067(3) 0.039(2) 0.039(2) -0.0167(17) 0.0015(18) -0.0148(19) C6 0.051(2) 0.055(3) 0.046(2) -0.0088(19) -0.0003(19) -0.015(2) C7 0.055(2) 0.054(3) 0.049(2) -0.009(2) 0.0008(19) -0.017(2) C8 0.039(2) 0.054(2) 0.042(2) 0.0005(18) -0.0001(17) -0.0151(18) C9 0.047(2) 0.049(2) 0.059(3) -0.006(2) 0.008(2) -0.0125(19) C10 0.058(3) 0.065(3) 0.043(2) -0.007(2) 0.0011(19) -0.021(2) C11 0.058(3) 0.054(3) 0.055(3) -0.006(2) -0.005(2) -0.017(2) C12 0.060(3) 0.045(2) 0.063(3) 0.002(2) -0.005(2) -0.013(2) C13 0.054(2) 0.040(2) 0.042(2) -0.0167(17) -0.0001(17) -0.0168(18) C14 0.055(2) 0.0285(18) 0.048(2) -0.0085(16) -0.0012(18) -0.0116(17) C15 0.0380(19) 0.040(2) 0.0373(19) -0.0083(16) 0.0063(15) -0.0137(16) C16 0.053(2) 0.040(2) 0.0348(19) -0.0137(16) 0.0027(16) -0.0139(17) C17 0.051(2) 0.0303(18) 0.042(2) -0.0127(16) 0.0012(17) -0.0107(16) C18 0.048(2) 0.0343(18) 0.041(2) -0.0061(16) 0.0032(17) -0.0110(16) C19 0.074(3) 0.078(3) 0.053(3) -0.023(2) 0.007(2) -0.039(3) C20 0.059(3) 0.075(3) 0.060(3) -0.029(2) 0.000(2) -0.028(2) C21 0.059(3) 0.067(3) 0.060(3) -0.037(2) 0.016(2) -0.029(2) C22 0.068(3) 0.068(3) 0.061(3) -0.022(2) 0.009(2) -0.027(2) C23 0.056(3) 0.087(4) 0.067(3) -0.029(3) 0.001(2) -0.026(3) C24 0.070(3) 0.071(3) 0.063(3) -0.032(2) 0.015(2) -0.032(3) C25 0.0277(16) 0.0301(16) 0.0278(16) -0.0070(13) -0.0015(13) -0.0134(14) C26 0.0269(16) 0.0296(16) 0.0382(18) -0.0125(14) 0.0024(13) -0.0111(13) C27 0.0235(15) 0.0283(16) 0.0360(17) -0.0127(14) 0.0026(13) -0.0095(13) C28 0.0279(16) 0.0373(18) 0.0453(19) -0.0197(16) 0.0066(14) -0.0164(14) C29 0.048(2) 0.065(3) 0.097(3) -0.060(3) 0.027(2) -0.033(2) C30 0.044(2) 0.080(3) 0.139(5) -0.086(3) 0.044(3) -0.030(2) C31 0.0314(19) 0.061(3) 0.091(3) -0.049(2) 0.023(2) -0.0228(18) O1W 0.0545(17) 0.0513(17) 0.080(2) -0.0182(16) 0.0138(16) -0.0216(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 2.106(2) . ? Mn1 O2 2.133(2) 2_676 ? Mn1 O7 2.181(2) . ? Mn1 N3 2.254(3) . ? Mn1 O6 2.262(2) . ? Mn1 N1 2.286(3) . ? S1 O4 1.396(4) . ? S1 O3 1.423(3) . ? S1 O5 1.427(4) . ? S1 C28 1.766(3) . ? O1 C25 1.242(4) . ? O2 C25 1.250(4) . ? O2 Mn1 2.133(2) 2_676 ? O6 H6B 0.84(3) . ? O6 H6A 0.85(3) . ? O7 H7B 0.847(10) . ? O7 H7A 0.85(3) . ? N1 C1 1.329(5) . ? N1 C5 1.332(4) . ? N2 C10 1.328(6) . ? N2 C12 1.330(6) . ? N3 C17 1.337(4) . ? N3 C13 1.341(4) . ? N4 C23 1.324(6) . ? N4 C19 1.329(6) . ? C1 C2 1.377(5) . ? C1 H1 0.9300 . ? C2 C3 1.382(5) . ? C2 H2 0.9300 . ? C3 C4 1.376(5) . ? C3 C6 1.472(5) . ? C4 C5 1.376(5) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.288(6) . ? C6 H6 0.9300 . ? C7 C8 1.470(5) . ? C7 H7 0.9300 . ? C8 C11 1.375(6) . ? C8 C9 1.391(6) . ? C9 C10 1.387(6) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.376(6) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.371(5) . ? C13 H13 0.9300 . ? C14 C15 1.385(5) . ? C14 H14 0.9300 . ? C15 C16 1.390(5) . ? C15 C18 1.464(5) . ? C16 C17 1.376(5) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C18 1.305(7) 2_767 ? C18 H18 0.9300 . ? C19 C20 1.373(6) . ? C19 H19 0.9300 . ? C20 C21 1.390(6) . ? C20 H20 0.9300 . ? C21 C22 1.381(6) . ? C21 C24 1.466(6) . ? C22 C23 1.369(7) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C24 1.314(9) 2_777 ? C24 H24 0.9300 . ? C25 C26 1.508(4) . ? C26 C31 1.383(5) . ? C26 C27 1.394(4) . ? C27 C28 1.375(4) . ? C27 H27 0.9300 . ? C28 C29 1.382(5) . ? C29 C30 1.376(5) . ? C29 H29 0.9300 . ? C30 C31 1.386(5) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? O1W H1WA 0.85(4) . ? O1W H1WB 0.85(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O2 112.14(9) . 2_676 ? O1 Mn1 O7 169.65(9) . . ? O2 Mn1 O7 78.10(9) 2_676 . ? O1 Mn1 N3 85.39(10) . . ? O2 Mn1 N3 90.26(10) 2_676 . ? O7 Mn1 N3 96.36(11) . . ? O1 Mn1 O6 89.51(9) . . ? O2 Mn1 O6 157.08(9) 2_676 . ? O7 Mn1 O6 80.56(9) . . ? N3 Mn1 O6 83.84(9) . . ? O1 Mn1 N1 88.04(10) . . ? O2 Mn1 N1 92.61(10) 2_676 . ? O7 Mn1 N1 90.03(11) . . ? N3 Mn1 N1 173.41(10) . . ? O6 Mn1 N1 95.70(9) . . ? O4 S1 O3 114.9(3) . . ? O4 S1 O5 110.4(3) . . ? O3 S1 O5 112.0(2) . . ? O4 S1 C28 106.9(2) . . ? O3 S1 C28 107.08(16) . . ? O5 S1 C28 104.9(2) . . ? C25 O1 Mn1 163.7(2) . . ? C25 O2 Mn1 127.5(2) . 2_676 ? Mn1 O6 H6B 125(2) . . ? Mn1 O6 H6A 123(2) . . ? H6B O6 H6A 109.9(17) . . ? Mn1 O7 H7B 124(2) . . ? Mn1 O7 H7A 117(2) . . ? H7B O7 H7A 108.8(16) . . ? C1 N1 C5 116.2(3) . . ? C1 N1 Mn1 117.9(2) . . ? C5 N1 Mn1 124.8(2) . . ? C10 N2 C12 116.1(4) . . ? C17 N3 C13 116.3(3) . . ? C17 N3 Mn1 121.2(2) . . ? C13 N3 Mn1 121.9(2) . . ? C23 N4 C19 115.8(4) . . ? N1 C1 C2 123.7(4) . . ? N1 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C1 C2 C3 120.1(4) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C4 C3 C2 115.9(3) . . ? C4 C3 C6 124.7(4) . . ? C2 C3 C6 119.4(4) . . ? C5 C4 C3 120.7(3) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? N1 C5 C4 123.3(3) . . ? N1 C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? C7 C6 C3 126.8(4) . . ? C7 C6 H6 116.6 . . ? C3 C6 H6 116.6 . . ? C6 C7 C8 127.4(4) . . ? C6 C7 H7 116.3 . . ? C8 C7 H7 116.3 . . ? C11 C8 C9 116.5(4) . . ? C11 C8 C7 119.3(4) . . ? C9 C8 C7 124.2(4) . . ? C10 C9 C8 119.7(4) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? N2 C10 C9 123.6(4) . . ? N2 C10 H10 118.2 . . ? C9 C10 H10 118.2 . . ? C8 C11 C12 119.8(5) . . ? C8 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? N2 C12 C11 124.3(4) . . ? N2 C12 H12 117.8 . . ? C11 C12 H12 117.8 . . ? N3 C13 C14 123.3(3) . . ? N3 C13 H13 118.3 . . ? C14 C13 H13 118.3 . . ? C13 C14 C15 120.3(3) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C16 116.6(3) . . ? C14 C15 C18 119.8(3) . . ? C16 C15 C18 123.6(3) . . ? C17 C16 C15 119.5(3) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? N3 C17 C16 123.8(3) . . ? N3 C17 H17 118.1 . . ? C16 C17 H17 118.1 . . ? C18 C18 C15 126.2(5) 2_767 . ? C18 C18 H18 116.9 2_767 . ? C15 C18 H18 116.9 . . ? N4 C19 C20 124.3(5) . . ? N4 C19 H19 117.9 . . ? C20 C19 H19 117.9 . . ? C19 C20 C21 119.6(4) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C22 C21 C20 116.0(4) . . ? C22 C21 C24 120.0(4) . . ? C20 C21 C24 124.0(4) . . ? C23 C22 C21 120.1(5) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? N4 C23 C22 124.2(5) . . ? N4 C23 H23 117.9 . . ? C22 C23 H23 117.9 . . ? C24 C24 C21 126.6(6) 2_777 . ? C24 C24 H24 116.7 2_777 . ? C21 C24 H24 116.7 . . ? O1 C25 O2 124.9(3) . . ? O1 C25 C26 117.7(3) . . ? O2 C25 C26 117.4(3) . . ? C31 C26 C27 119.8(3) . . ? C31 C26 C25 120.7(3) . . ? C27 C26 C25 119.5(3) . . ? C28 C27 C26 119.8(3) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C27 C28 C29 120.4(3) . . ? C27 C28 S1 120.3(2) . . ? C29 C28 S1 119.3(3) . . ? C30 C29 C28 119.8(3) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C29 C30 C31 120.4(4) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C26 C31 C30 119.7(3) . . ? C26 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? H1WA O1W H1WB 109(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Mn1 O1 C25 -76.8(8) 2_676 . . . ? O7 Mn1 O1 C25 94.5(9) . . . . ? N3 Mn1 O1 C25 -165.3(8) . . . . ? O6 Mn1 O1 C25 110.9(8) . . . . ? N1 Mn1 O1 C25 15.2(8) . . . . ? O1 Mn1 N1 C1 -145.8(3) . . . . ? O2 Mn1 N1 C1 -33.7(3) 2_676 . . . ? O7 Mn1 N1 C1 44.4(3) . . . . ? O6 Mn1 N1 C1 124.9(3) . . . . ? O1 Mn1 N1 C5 21.5(3) . . . . ? O2 Mn1 N1 C5 133.6(3) 2_676 . . . ? O7 Mn1 N1 C5 -148.3(3) . . . . ? O6 Mn1 N1 C5 -67.8(3) . . . . ? O1 Mn1 N3 C17 -39.1(3) . . . . ? O2 Mn1 N3 C17 -151.3(3) 2_676 . . . ? O7 Mn1 N3 C17 130.6(3) . . . . ? O6 Mn1 N3 C17 50.9(3) . . . . ? O1 Mn1 N3 C13 150.3(3) . . . . ? O2 Mn1 N3 C13 38.1(3) 2_676 . . . ? O7 Mn1 N3 C13 -40.0(3) . . . . ? O6 Mn1 N3 C13 -119.7(3) . . . . ? C5 N1 C1 C2 -2.0(6) . . . . ? Mn1 N1 C1 C2 166.4(3) . . . . ? N1 C1 C2 C3 -0.4(7) . . . . ? C1 C2 C3 C4 2.4(6) . . . . ? C1 C2 C3 C6 -176.8(4) . . . . ? C2 C3 C4 C5 -2.2(6) . . . . ? C6 C3 C4 C5 177.0(4) . . . . ? C1 N1 C5 C4 2.2(6) . . . . ? Mn1 N1 C5 C4 -165.2(3) . . . . ? C3 C4 C5 N1 -0.1(7) . . . . ? C4 C3 C6 C7 -0.8(7) . . . . ? C2 C3 C6 C7 178.4(4) . . . . ? C3 C6 C7 C8 -179.0(4) . . . . ? C6 C7 C8 C11 -174.2(5) . . . . ? C6 C7 C8 C9 4.8(7) . . . . ? C11 C8 C9 C10 1.3(6) . . . . ? C7 C8 C9 C10 -177.8(4) . . . . ? C12 N2 C10 C9 -1.0(7) . . . . ? C8 C9 C10 N2 -0.4(7) . . . . ? C9 C8 C11 C12 -0.8(6) . . . . ? C7 C8 C11 C12 178.3(4) . . . . ? C10 N2 C12 C11 1.6(7) . . . . ? C8 C11 C12 N2 -0.7(7) . . . . ? C17 N3 C13 C14 -2.6(6) . . . . ? Mn1 N3 C13 C14 168.4(3) . . . . ? N3 C13 C14 C15 -0.9(6) . . . . ? C13 C14 C15 C16 3.8(6) . . . . ? C13 C14 C15 C18 -175.3(4) . . . . ? C14 C15 C16 C17 -3.2(5) . . . . ? C18 C15 C16 C17 175.9(4) . . . . ? C13 N3 C17 C16 3.2(5) . . . . ? Mn1 N3 C17 C16 -167.9(3) . . . . ? C15 C16 C17 N3 -0.3(6) . . . . ? C14 C15 C18 C18 168.9(5) . . . 2_767 ? C16 C15 C18 C18 -10.2(7) . . . 2_767 ? C23 N4 C19 C20 -0.4(7) . . . . ? N4 C19 C20 C21 0.2(7) . . . . ? C19 C20 C21 C22 0.3(6) . . . . ? C19 C20 C21 C24 179.8(4) . . . . ? C20 C21 C22 C23 -0.6(7) . . . . ? C24 C21 C22 C23 179.9(4) . . . . ? C19 N4 C23 C22 0.0(7) . . . . ? C21 C22 C23 N4 0.5(8) . . . . ? C22 C21 C24 C24 178.2(6) . . . 2_777 ? C20 C21 C24 C24 -1.3(9) . . . 2_777 ? Mn1 O1 C25 O2 71.7(9) . . . . ? Mn1 O1 C25 C26 -108.0(7) . . . . ? Mn1 O2 C25 O1 -0.7(5) 2_676 . . . ? Mn1 O2 C25 C26 179.0(2) 2_676 . . . ? O1 C25 C26 C31 -178.0(3) . . . . ? O2 C25 C26 C31 2.2(5) . . . . ? O1 C25 C26 C27 3.6(4) . . . . ? O2 C25 C26 C27 -176.1(3) . . . . ? C31 C26 C27 C28 0.1(5) . . . . ? C25 C26 C27 C28 178.4(3) . . . . ? C26 C27 C28 C29 -1.0(5) . . . . ? C26 C27 C28 S1 179.2(2) . . . . ? O4 S1 C28 C27 115.7(4) . . . . ? O3 S1 C28 C27 -7.9(4) . . . . ? O5 S1 C28 C27 -127.0(3) . . . . ? O4 S1 C28 C29 -64.1(4) . . . . ? O3 S1 C28 C29 172.4(4) . . . . ? O5 S1 C28 C29 53.2(4) . . . . ? C27 C28 C29 C30 1.4(7) . . . . ? S1 C28 C29 C30 -178.8(4) . . . . ? C28 C29 C30 C31 -0.8(8) . . . . ? C27 C26 C31 C30 0.5(6) . . . . ? C25 C26 C31 C30 -177.8(4) . . . . ? C29 C30 C31 C26 -0.1(8) . . . . ? 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 O7 H7B O3 0.847(10) 1.930(12) 2.771(3) 171(3) 2_776 O7 H7B S1 0.847(10) 2.82(2) 3.535(2) 144(3) 2_776 O6 H6B N2 0.84(3) 2.154(15) 2.972(4) 164(4) 2_685 O6 H6A N2 0.85(3) 2.09(3) 2.935(4) 173(4) 1_646 O7 H7A O1W 0.85(3) 1.994(16) 2.811(4) 162(3) 1_545 O1W H1WA O4 0.85(4) 1.89(4) 2.730(5) 170(5) . O1W H1WB O4 0.85(4) 2.53(3) 3.255(6) 145(5) 2_786 O1W H1WB S1 0.85(4) 2.97(3) 3.666(3) 140(4) 2_786 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.658 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.062 data_comp-3 _database_code_depnum_ccdc_archive 'CCDC 745967' #TrackingRef '- Final_cifdata.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H28 Mn N4 O9 S' _chemical_formula_weight 663.55 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 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.4415(8) _cell_length_b 20.268(2) _cell_length_c 10.2404(11) _cell_angle_alpha 90.00 _cell_angle_beta 107.6090(10) _cell_angle_gamma 90.00 _cell_volume 1472.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 4290 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 27.05 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 686 _exptl_absorpt_coefficient_mu 0.581 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.809 _exptl_absorpt_correction_T_max 0.907 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker SMART area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 9285 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.19 _reflns_number_total 5193 _reflns_number_gt 4907 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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. The aromatic H atoms were positioned geometrically and were included in the refinement in the riding-model approximation [C-H= 0.93 /%A and U~iso~(H)=1.2 U~eq~(C)]. The water H atoms were also placed in calculated positions (O-H=0.85 /%A) with fixed isotropic displacement parameters. ; _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^)+(0.0292P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.003(13) _refine_ls_number_reflns 5193 _refine_ls_number_parameters 421 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0352 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0739 _refine_ls_wR_factor_gt 0.0726 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean <0.001 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 H6B H 0.217(5) 0.4214(17) 0.707(2) 0.090 Uiso 1 1 d D . . H6A H 0.105(3) 0.4382(18) 0.579(2) 0.090 Uiso 1 1 d D . . H7A H 0.486(4) 0.3393(12) 0.611(4) 0.080 Uiso 1 1 d D . . H7B H 0.6626(17) 0.3603(16) 0.616(4) 0.080 Uiso 1 1 d D . . H8A H 0.705(4) 0.4614(17) 0.410(3) 0.090 Uiso 1 1 d D . . H8B H 0.569(5) 0.5048(18) 0.337(3) 0.090 Uiso 1 1 d D . . Mn1 Mn 0.41103(5) 0.46388(2) 0.52423(3) 0.03105(10) Uani 1 1 d . . . S1 S 0.05918(9) 0.33190(3) -0.15067(6) 0.03320(15) Uani 1 1 d . . . O1 O 0.1990(2) 0.42831(11) 0.34805(18) 0.0456(5) Uani 1 1 d . . . O2 O -0.0642(3) 0.42478(14) 0.40717(19) 0.0629(7) Uani 1 1 d . . . O3 O 0.2063(3) 0.38136(10) -0.12218(18) 0.0440(5) Uani 1 1 d . . . O4 O 0.1347(3) 0.26620(11) -0.1284(2) 0.0599(6) Uani 1 1 d . . . O5 O -0.0776(3) 0.34057(11) -0.28367(17) 0.0477(5) Uani 1 1 d . . . O6 O 0.2101(3) 0.44569(10) 0.63873(18) 0.0450(5) Uani 1 1 d D . . O7 O 0.5480(3) 0.37119(11) 0.5916(2) 0.0523(5) Uani 1 1 d D . . O8 O 0.6073(3) 0.48244(11) 0.4096(2) 0.0474(6) Uani 1 1 d D . . O1W O 0.3741(3) 0.26506(12) 0.6678(2) 0.0591(6) Uani 1 1 d D . . N1 N 0.5719(3) 0.52547(10) 0.7106(2) 0.0335(5) Uani 1 1 d . . . N2 N 0.3160(3) 0.56993(12) 0.4791(2) 0.0366(5) Uani 1 1 d . . . N3 N -0.1629(4) 0.68762(13) 0.5567(2) 0.0477(6) Uani 1 1 d . . . N4 N 0.4672(4) 0.55368(13) 1.1654(3) 0.0523(7) Uani 1 1 d . . . C1 C 0.6890(4) 0.50372(15) 0.8267(3) 0.0446(7) Uani 1 1 d . . . H1 H 0.7178 0.4590 0.8341 0.054 Uiso 1 1 calc R . . C2 C 0.7719(5) 0.54410(18) 0.9391(3) 0.0547(9) Uani 1 1 d . . . H2 H 0.8532 0.5265 1.0192 0.066 Uiso 1 1 calc R . . C3 C 0.7316(5) 0.60945(19) 0.9292(3) 0.0533(9) Uani 1 1 d . . . H3 H 0.7863 0.6373 1.0026 0.064 Uiso 1 1 calc R . . C4 C 0.6081(4) 0.63493(15) 0.8088(3) 0.0431(7) Uani 1 1 d . . . C5 C 0.5606(5) 0.70357(17) 0.7913(4) 0.0606(9) Uani 1 1 d . . . H5 H 0.6149 0.7331 0.8616 0.073 Uiso 1 1 calc R . . C6 C 0.4380(5) 0.72571(16) 0.6738(4) 0.0614(10) Uani 1 1 d . . . H6 H 0.4092 0.7704 0.6642 0.074 Uiso 1 1 calc R . . C7 C 0.3527(4) 0.68216(15) 0.5653(3) 0.0475(8) Uani 1 1 d . . . C8 C 0.2207(5) 0.70257(17) 0.4426(4) 0.0613(10) Uani 1 1 d . . . H8 H 0.1876 0.7469 0.4290 0.074 Uiso 1 1 calc R . . C9 C 0.1418(5) 0.65775(19) 0.3443(4) 0.0621(10) Uani 1 1 d . . . H9 H 0.0550 0.6712 0.2626 0.074 Uiso 1 1 calc R . . C10 C 0.1903(4) 0.59196(17) 0.3656(3) 0.0492(8) Uani 1 1 d . . . H10 H 0.1325 0.5617 0.2974 0.059 Uiso 1 1 calc R . . C11 C 0.3964(4) 0.61433(13) 0.5781(3) 0.0346(6) Uani 1 1 d . . . C12 C 0.5287(4) 0.59065(13) 0.7019(3) 0.0340(6) Uani 1 1 d . . . C13 C 0.0088(4) 0.59635(15) 0.6827(3) 0.0441(7) Uani 1 1 d . . . H13 H 0.0378 0.5517 0.6839 0.053 Uiso 1 1 calc R . . C14 C -0.1163(4) 0.62427(16) 0.5678(3) 0.0472(7) Uani 1 1 d . . . H14 H -0.1713 0.5969 0.4936 0.057 Uiso 1 1 calc R . . C15 C -0.0827(5) 0.72483(16) 0.6659(3) 0.0523(8) Uani 1 1 d . . . H15 H -0.1126 0.7695 0.6611 0.063 Uiso 1 1 calc R . . C16 C 0.0415(4) 0.70160(15) 0.7853(3) 0.0471(7) Uani 1 1 d . . . H16 H 0.0923 0.7301 0.8583 0.056 Uiso 1 1 calc R . . C17 C 0.0906(4) 0.63549(14) 0.7962(3) 0.0366(6) Uani 1 1 d . . . C18 C 0.2230(4) 0.60761(14) 0.9240(3) 0.0382(6) Uani 1 1 d . . . C19 C 0.3246(5) 0.64605(15) 1.0315(3) 0.0514(8) Uani 1 1 d . . . H19 H 0.3132 0.6917 1.0248 0.062 Uiso 1 1 calc R . . C20 C 0.4420(5) 0.61857(17) 1.1483(3) 0.0558(9) Uani 1 1 d . . . H20 H 0.5072 0.6464 1.2189 0.067 Uiso 1 1 calc R . . C21 C 0.3705(5) 0.51605(17) 1.0610(3) 0.0539(8) Uani 1 1 d . . . H21 H 0.3859 0.4706 1.0696 0.065 Uiso 1 1 calc R . . C22 C 0.2501(4) 0.54026(15) 0.9422(3) 0.0492(8) Uani 1 1 d . . . H22 H 0.1860 0.5114 0.8732 0.059 Uiso 1 1 calc R . . C23 C 0.0277(4) 0.41584(15) 0.3258(3) 0.0364(6) Uani 1 1 d . . . C24 C -0.0736(3) 0.38650(13) 0.1877(2) 0.0317(6) Uani 1 1 d . . . C25 C 0.0250(4) 0.37428(13) 0.0949(2) 0.0311(6) Uani 1 1 d . . . H25 H 0.1519 0.3854 0.1169 0.037 Uiso 1 1 calc R . . C26 C -0.0652(3) 0.34548(12) -0.0304(2) 0.0298(6) Uani 1 1 d . . . C27 C -0.2539(4) 0.32796(15) -0.0622(3) 0.0358(6) Uani 1 1 d . . . H27 H -0.3135 0.3073 -0.1452 0.043 Uiso 1 1 calc R . . C28 C -0.3527(4) 0.34104(15) 0.0287(3) 0.0414(7) Uani 1 1 d . . . H28 H -0.4800 0.3304 0.0063 0.050 Uiso 1 1 calc R . . C29 C -0.2621(4) 0.37009(15) 0.1536(3) 0.0391(6) Uani 1 1 d . . . H29 H -0.3289 0.3786 0.2151 0.047 Uiso 1 1 calc R . . H1WB H 0.293(4) 0.272(2) 0.710(3) 0.090 Uiso 1 1 d D . . H1WA H 0.316(4) 0.2448(19) 0.594(2) 0.090 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 Mn1 0.0328(2) 0.0312(2) 0.02777(18) -0.00092(18) 0.00701(14) 0.00321(19) S1 0.0333(3) 0.0349(4) 0.0276(3) -0.0036(3) 0.0035(3) -0.0019(3) O1 0.0339(11) 0.0669(14) 0.0338(10) -0.0140(9) 0.0069(8) -0.0065(10) O2 0.0360(11) 0.117(2) 0.0345(11) -0.0108(12) 0.0098(9) 0.0169(13) O3 0.0391(11) 0.0563(13) 0.0369(10) -0.0034(10) 0.0120(9) -0.0120(10) O4 0.0727(15) 0.0442(14) 0.0618(14) -0.0025(11) 0.0189(12) 0.0147(12) O5 0.0411(11) 0.0700(15) 0.0260(9) -0.0059(9) 0.0010(8) -0.0032(11) O6 0.0431(11) 0.0594(16) 0.0325(10) 0.0007(9) 0.0117(8) -0.0092(10) O7 0.0422(11) 0.0392(12) 0.0680(14) 0.0122(11) 0.0054(11) 0.0074(10) O8 0.0400(11) 0.0614(16) 0.0453(11) 0.0086(10) 0.0198(9) 0.0123(10) O1W 0.0596(14) 0.0535(15) 0.0637(15) -0.0091(12) 0.0179(12) -0.0071(12) N1 0.0355(12) 0.0316(13) 0.0345(12) 0.0025(10) 0.0121(10) 0.0000(10) N2 0.0375(13) 0.0389(13) 0.0353(12) 0.0085(10) 0.0139(10) 0.0109(11) N3 0.0466(15) 0.0488(17) 0.0490(14) 0.0014(12) 0.0161(12) -0.0026(13) N4 0.0585(17) 0.0534(18) 0.0486(15) 0.0067(13) 0.0216(13) 0.0009(14) C1 0.0464(17) 0.0443(18) 0.0382(15) 0.0083(13) 0.0054(13) -0.0026(14) C2 0.0488(19) 0.076(3) 0.0352(16) 0.0021(16) 0.0065(14) -0.0107(18) C3 0.0472(19) 0.069(2) 0.0457(18) -0.0200(17) 0.0164(15) -0.0222(18) C4 0.0392(16) 0.0474(18) 0.0503(17) -0.0111(14) 0.0247(14) -0.0116(13) C5 0.063(2) 0.0419(19) 0.087(3) -0.0276(19) 0.038(2) -0.0114(17) C6 0.061(2) 0.0267(17) 0.107(3) -0.0075(18) 0.042(2) 0.0009(16) C7 0.0485(18) 0.0335(16) 0.070(2) 0.0100(16) 0.0327(16) 0.0092(14) C8 0.064(2) 0.0376(19) 0.096(3) 0.027(2) 0.044(2) 0.0188(17) C9 0.060(2) 0.067(3) 0.059(2) 0.034(2) 0.0185(18) 0.0283(19) C10 0.0494(18) 0.059(2) 0.0383(15) 0.0131(14) 0.0121(13) 0.0154(16) C11 0.0352(14) 0.0329(15) 0.0430(14) 0.0064(12) 0.0229(12) 0.0057(12) C12 0.0374(14) 0.0328(15) 0.0375(14) -0.0015(12) 0.0202(12) -0.0047(12) C13 0.0500(18) 0.0358(16) 0.0504(17) -0.0041(14) 0.0210(14) -0.0017(14) C14 0.0514(18) 0.048(2) 0.0459(16) -0.0074(14) 0.0195(14) -0.0081(15) C15 0.0530(19) 0.0369(18) 0.065(2) 0.0017(15) 0.0157(17) -0.0003(15) C16 0.0481(18) 0.0355(17) 0.0531(18) -0.0063(14) 0.0086(15) -0.0032(14) C17 0.0368(15) 0.0326(15) 0.0456(16) -0.0022(12) 0.0203(13) -0.0041(12) C18 0.0385(15) 0.0359(16) 0.0441(15) -0.0023(13) 0.0183(12) -0.0031(13) C19 0.070(2) 0.0364(18) 0.0480(17) -0.0029(14) 0.0174(16) 0.0006(16) C20 0.076(2) 0.047(2) 0.0439(17) -0.0052(15) 0.0166(16) -0.0046(17) C21 0.058(2) 0.0382(17) 0.063(2) 0.0043(16) 0.0137(17) 0.0020(15) C22 0.0496(19) 0.0354(17) 0.059(2) -0.0052(15) 0.0117(16) -0.0023(15) C23 0.0323(15) 0.0446(16) 0.0305(13) 0.0017(12) 0.0068(11) 0.0085(12) C24 0.0296(13) 0.0323(14) 0.0297(13) 0.0050(11) 0.0036(10) 0.0025(11) C25 0.0267(13) 0.0320(14) 0.0314(13) 0.0016(11) 0.0041(11) -0.0032(11) C26 0.0316(13) 0.0244(14) 0.0282(12) 0.0045(10) 0.0014(10) -0.0028(11) C27 0.0351(14) 0.0382(16) 0.0262(12) 0.0055(12) -0.0024(11) -0.0083(13) C28 0.0252(13) 0.0473(18) 0.0448(15) 0.0126(14) 0.0004(12) -0.0063(13) C29 0.0322(15) 0.0465(17) 0.0380(14) 0.0071(13) 0.0098(12) 0.0068(13) _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 2.1311(18) . ? Mn1 O7 2.149(2) . ? Mn1 O8 2.1661(19) . ? Mn1 O6 2.1924(18) . ? Mn1 N2 2.266(2) . ? Mn1 N1 2.291(2) . ? S1 O4 1.436(2) . ? S1 O5 1.4433(18) . ? S1 O3 1.448(2) . ? S1 C26 1.772(3) . ? O1 C23 1.251(3) . ? O2 C23 1.241(3) . ? O6 H6B 0.84(3) . ? O6 H6A 0.848(10) . ? O7 H7A 0.85(3) . ? O7 H7B 0.842(10) . ? O8 H8A 0.84(3) . ? O8 H8B 0.84(3) . ? O1W H1WB 0.85(3) . ? O1W H1WA 0.85(3) . ? N1 C1 1.320(3) . ? N1 C12 1.356(3) . ? N2 C10 1.330(4) . ? N2 C11 1.352(4) . ? N3 C14 1.326(4) . ? N3 C15 1.331(4) . ? N4 C20 1.333(4) . ? N4 C21 1.333(4) . ? C1 C2 1.395(4) . ? C1 H1 0.9300 . ? C2 C3 1.355(5) . ? C2 H2 0.9300 . ? C3 C4 1.395(5) . ? C3 H3 0.9300 . ? C4 C12 1.400(4) . ? C4 C5 1.433(5) . ? C5 C6 1.348(5) . ? C5 H5 0.9300 . ? C6 C7 1.411(5) . ? C6 H6 0.9300 . ? C7 C8 1.403(5) . ? C7 C11 1.410(4) . ? C8 C9 1.351(5) . ? C8 H8 0.9300 . ? C9 C10 1.381(5) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.433(4) . ? C13 C14 1.382(4) . ? C13 C17 1.386(4) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.373(4) . ? C15 H15 0.9300 . ? C16 C17 1.385(4) . ? C16 H16 0.9300 . ? C17 C18 1.491(4) . ? C18 C19 1.374(4) . ? C18 C22 1.384(4) . ? C19 C20 1.368(4) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.365(4) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.508(4) . ? C24 C29 1.379(4) . ? C24 C25 1.388(3) . ? C25 C26 1.384(3) . ? C25 H25 0.9300 . ? C26 C27 1.388(4) . ? C27 C28 1.376(4) . ? C27 H27 0.9300 . ? C28 C29 1.384(4) . ? C28 H28 0.9300 . ? C29 H29 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 97.69(9) . . ? O1 Mn1 O8 92.73(8) . . ? O7 Mn1 O8 89.65(8) . . ? O1 Mn1 O6 86.90(7) . . ? O7 Mn1 O6 90.86(9) . . ? O8 Mn1 O6 179.41(8) . . ? O1 Mn1 N2 92.45(8) . . ? O7 Mn1 N2 169.41(9) . . ? O8 Mn1 N2 86.83(8) . . ? O6 Mn1 N2 92.72(8) . . ? O1 Mn1 N1 162.91(8) . . ? O7 Mn1 N1 97.54(8) . . ? O8 Mn1 N1 95.08(8) . . ? O6 Mn1 N1 85.15(7) . . ? N2 Mn1 N1 72.87(8) . . ? O4 S1 O5 113.14(13) . . ? O4 S1 O3 111.98(14) . . ? O5 S1 O3 112.35(12) . . ? O4 S1 C26 107.17(12) . . ? O5 S1 C26 105.63(11) . . ? O3 S1 C26 105.95(11) . . ? C23 O1 Mn1 132.47(16) . . ? Mn1 O6 H6B 132(3) . . ? Mn1 O6 H6A 106(2) . . ? H6B O6 H6A 107.4(16) . . ? Mn1 O7 H7A 120(2) . . ? Mn1 O7 H7B 131(2) . . ? H7A O7 H7B 107.9(16) . . ? Mn1 O8 H8A 129(2) . . ? Mn1 O8 H8B 118(2) . . ? H8A O8 H8B 109.9(17) . . ? H1WB O1W H1WA 106.0(16) . . ? C1 N1 C12 117.6(2) . . ? C1 N1 Mn1 127.22(19) . . ? C12 N1 Mn1 114.99(16) . . ? C10 N2 C11 117.8(3) . . ? C10 N2 Mn1 126.2(2) . . ? C11 N2 Mn1 115.99(16) . . ? C14 N3 C15 115.9(3) . . ? C20 N4 C21 116.0(3) . . ? N1 C1 C2 123.7(3) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C3 C2 C1 118.6(3) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 120.0(3) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C12 117.6(3) . . ? C3 C4 C5 122.8(3) . . ? C12 C4 C5 119.6(3) . . ? C6 C5 C4 120.6(3) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C7 121.1(3) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C8 C7 C11 116.7(3) . . ? C8 C7 C6 123.2(3) . . ? C11 C7 C6 120.1(3) . . ? C9 C8 C7 119.9(3) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 119.9(3) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? N2 C10 C9 122.9(3) . . ? N2 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? N2 C11 C7 122.8(3) . . ? N2 C11 C12 118.1(2) . . ? C7 C11 C12 119.1(3) . . ? N1 C12 C4 122.5(2) . . ? N1 C12 C11 118.0(2) . . ? C4 C12 C11 119.5(3) . . ? C14 C13 C17 119.4(3) . . ? C14 C13 H13 120.3 . . ? C17 C13 H13 120.3 . . ? N3 C14 C13 124.1(3) . . ? N3 C14 H14 117.9 . . ? C13 C14 H14 117.9 . . ? N3 C15 C16 124.3(3) . . ? N3 C15 H15 117.9 . . ? C16 C15 H15 117.9 . . ? C15 C16 C17 119.6(3) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C16 C17 C13 116.6(3) . . ? C16 C17 C18 121.7(3) . . ? C13 C17 C18 121.7(3) . . ? C19 C18 C22 115.4(3) . . ? C19 C18 C17 123.1(3) . . ? C22 C18 C17 121.5(3) . . ? C20 C19 C18 121.4(3) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? N4 C20 C19 123.0(3) . . ? N4 C20 H20 118.5 . . ? C19 C20 H20 118.5 . . ? N4 C21 C22 124.0(3) . . ? N4 C21 H21 118.0 . . ? C22 C21 H21 118.0 . . ? C21 C22 C18 120.3(3) . . ? C21 C22 H22 119.9 . . ? C18 C22 H22 119.9 . . ? O2 C23 O1 125.9(2) . . ? O2 C23 C24 117.8(2) . . ? O1 C23 C24 116.3(2) . . ? C29 C24 C25 119.4(2) . . ? C29 C24 C23 120.9(2) . . ? C25 C24 C23 119.6(2) . . ? C26 C25 C24 120.1(2) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C27 119.9(2) . . ? C25 C26 S1 120.04(19) . . ? C27 C26 S1 120.05(19) . . ? C28 C27 C26 120.1(2) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C29 119.8(2) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C24 C29 C28 120.7(2) . . ? C24 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? 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 O7 Mn1 O1 C23 101.8(3) . . . . ? O8 Mn1 O1 C23 -168.2(3) . . . . ? O6 Mn1 O1 C23 11.4(3) . . . . ? N2 Mn1 O1 C23 -81.2(3) . . . . ? N1 Mn1 O1 C23 -51.0(4) . . . . ? O1 Mn1 N1 C1 144.1(3) . . . . ? O7 Mn1 N1 C1 -8.7(2) . . . . ? O8 Mn1 N1 C1 -99.0(2) . . . . ? O6 Mn1 N1 C1 81.6(2) . . . . ? N2 Mn1 N1 C1 175.9(2) . . . . ? O1 Mn1 N1 C12 -30.4(4) . . . . ? O7 Mn1 N1 C12 176.76(17) . . . . ? O8 Mn1 N1 C12 86.45(17) . . . . ? O6 Mn1 N1 C12 -93.01(17) . . . . ? N2 Mn1 N1 C12 1.35(16) . . . . ? O1 Mn1 N2 C10 -8.9(2) . . . . ? O7 Mn1 N2 C10 154.4(4) . . . . ? O8 Mn1 N2 C10 83.7(2) . . . . ? O6 Mn1 N2 C10 -95.9(2) . . . . ? N1 Mn1 N2 C10 -180.0(2) . . . . ? O1 Mn1 N2 C11 171.18(18) . . . . ? O7 Mn1 N2 C11 -25.5(6) . . . . ? O8 Mn1 N2 C11 -96.21(18) . . . . ? O6 Mn1 N2 C11 84.17(18) . . . . ? N1 Mn1 N2 C11 0.10(17) . . . . ? C12 N1 C1 C2 -1.1(4) . . . . ? Mn1 N1 C1 C2 -175.5(2) . . . . ? N1 C1 C2 C3 -0.3(5) . . . . ? C1 C2 C3 C4 0.6(5) . . . . ? C2 C3 C4 C12 0.5(4) . . . . ? C2 C3 C4 C5 -179.5(3) . . . . ? C3 C4 C5 C6 -178.9(3) . . . . ? C12 C4 C5 C6 1.1(4) . . . . ? C4 C5 C6 C7 0.2(5) . . . . ? C5 C6 C7 C8 178.3(3) . . . . ? C5 C6 C7 C11 -0.6(5) . . . . ? C11 C7 C8 C9 0.4(4) . . . . ? C6 C7 C8 C9 -178.6(3) . . . . ? C7 C8 C9 C10 0.5(5) . . . . ? C11 N2 C10 C9 1.1(4) . . . . ? Mn1 N2 C10 C9 -178.8(2) . . . . ? C8 C9 C10 N2 -1.3(5) . . . . ? C10 N2 C11 C7 -0.1(4) . . . . ? Mn1 N2 C11 C7 179.81(19) . . . . ? C10 N2 C11 C12 178.6(2) . . . . ? Mn1 N2 C11 C12 -1.5(3) . . . . ? C8 C7 C11 N2 -0.6(4) . . . . ? C6 C7 C11 N2 178.4(3) . . . . ? C8 C7 C11 C12 -179.3(2) . . . . ? C6 C7 C11 C12 -0.3(4) . . . . ? C1 N1 C12 C4 2.3(4) . . . . ? Mn1 N1 C12 C4 177.38(19) . . . . ? C1 N1 C12 C11 -177.8(2) . . . . ? Mn1 N1 C12 C11 -2.6(3) . . . . ? C3 C4 C12 N1 -2.0(4) . . . . ? C5 C4 C12 N1 178.0(2) . . . . ? C3 C4 C12 C11 178.0(2) . . . . ? C5 C4 C12 C11 -1.9(4) . . . . ? N2 C11 C12 N1 2.8(3) . . . . ? C7 C11 C12 N1 -178.4(2) . . . . ? N2 C11 C12 C4 -177.2(2) . . . . ? C7 C11 C12 C4 1.5(4) . . . . ? C15 N3 C14 C13 -0.8(4) . . . . ? C17 C13 C14 N3 1.2(5) . . . . ? C14 N3 C15 C16 0.0(5) . . . . ? N3 C15 C16 C17 0.4(5) . . . . ? C15 C16 C17 C13 0.0(4) . . . . ? C15 C16 C17 C18 -179.3(3) . . . . ? C14 C13 C17 C16 -0.8(4) . . . . ? C14 C13 C17 C18 178.6(2) . . . . ? C16 C17 C18 C19 -9.1(4) . . . . ? C13 C17 C18 C19 171.6(3) . . . . ? C16 C17 C18 C22 170.2(3) . . . . ? C13 C17 C18 C22 -9.1(4) . . . . ? C22 C18 C19 C20 -0.7(4) . . . . ? C17 C18 C19 C20 178.7(3) . . . . ? C21 N4 C20 C19 0.0(5) . . . . ? C18 C19 C20 N4 0.6(5) . . . . ? C20 N4 C21 C22 -0.5(5) . . . . ? N4 C21 C22 C18 0.4(5) . . . . ? C19 C18 C22 C21 0.2(4) . . . . ? C17 C18 C22 C21 -179.2(3) . . . . ? Mn1 O1 C23 O2 3.2(5) . . . . ? Mn1 O1 C23 C24 -175.93(18) . . . . ? O2 C23 C24 C29 -0.1(4) . . . . ? O1 C23 C24 C29 179.1(3) . . . . ? O2 C23 C24 C25 -178.5(3) . . . . ? O1 C23 C24 C25 0.7(4) . . . . ? C29 C24 C25 C26 -0.4(4) . . . . ? C23 C24 C25 C26 178.0(2) . . . . ? C24 C25 C26 C27 -0.9(4) . . . . ? C24 C25 C26 S1 178.32(19) . . . . ? O4 S1 C26 C25 92.7(2) . . . . ? O5 S1 C26 C25 -146.4(2) . . . . ? O3 S1 C26 C25 -27.0(2) . . . . ? O4 S1 C26 C27 -88.0(2) . . . . ? O5 S1 C26 C27 32.9(2) . . . . ? O3 S1 C26 C27 152.3(2) . . . . ? C25 C26 C27 C28 2.0(4) . . . . ? S1 C26 C27 C28 -177.2(2) . . . . ? C26 C27 C28 C29 -1.8(4) . . . . ? C25 C24 C29 C28 0.7(4) . . . . ? C23 C24 C29 C28 -177.7(3) . . . . ? C27 C28 C29 C24 0.4(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 O6 H6A O2 0.848(10) 1.850(15) 2.653(3) 157(3) . O7 H7A O1W 0.85(3) 1.89(3) 2.742(3) 173(3) . O7 H7B O5 0.842(10) 1.94(3) 2.761(3) 166(4) 1_656 O8 H8A O2 0.84(3) 1.88(3) 2.716(3) 173(4) 1_655 O1W H1WB O4 0.85(3) 2.309(16) 3.128(3) 161(4) 1_556 O1W H1WA N3 0.85(3) 1.99(3) 2.834(3) 170(4) 2_546 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.19 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.225 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.062 data_comp-4 _database_code_depnum_ccdc_archive 'CCDC 745968' #TrackingRef '- Final_cifdata.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H40 Mn2 N6 O14 S2' _chemical_formula_weight 1098.86 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 13.7428(15) _cell_length_b 13.7074(15) _cell_length_c 14.2123(15) _cell_angle_alpha 90.00 _cell_angle_beta 118.3340(10) _cell_angle_gamma 90.00 _cell_volume 2356.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3828 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 29.72 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.700 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8174 _exptl_absorpt_correction_T_max 0.9207 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker SMART area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 13083 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.20 _reflns_number_total 4204 _reflns_number_gt 3516 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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. The aromatic H atoms were positioned geometrically and were included in the refinement in the riding-model approximation [C-H= 0.93 /%A and U~iso~(H)=1.2 U~eq~(C)]. The water H atoms were also placed in calculated positions (O-H=0.85 /%A) with fixed isotropic displacement parameters. ; _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^)+(0.0455P)^2^+0.9632P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4204 _refine_ls_number_parameters 341 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0949 _refine_ls_wR_factor_gt 0.0896 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean <0.001 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 0.24320(3) 0.29038(3) 0.32354(3) 0.03141(12) Uani 1 1 d . . . S1 S -0.31739(5) 0.11168(5) 0.05063(6) 0.04114(18) Uani 1 1 d . . . O1 O 0.09138(13) 0.25406(13) 0.18899(13) 0.0413(4) Uani 1 1 d . . . O2 O 0.07135(16) 0.36579(16) 0.06762(15) 0.0614(6) Uani 1 1 d . . . O3 O -0.24321(16) 0.08261(15) 0.15905(16) 0.0586(5) Uani 1 1 d . . . O4 O -0.39315(16) 0.18744(14) 0.04569(19) 0.0628(6) Uani 1 1 d . . . O5 O -0.37366(17) 0.03127(14) -0.02009(16) 0.0581(5) Uani 1 1 d . . . O6 O 0.38575(14) 0.34412(14) 0.46572(15) 0.0445(4) Uani 1 1 d D . . O7 O 0.25779(16) 0.41734(14) 0.23635(16) 0.0451(4) Uani 1 1 d D . . N1 N 0.24343(17) 0.13600(14) 0.38356(16) 0.0369(5) Uani 1 1 d . . . N2 N 0.36196(16) 0.20088(14) 0.28961(16) 0.0361(5) Uani 1 1 d . . . N3 N 0.14439(16) 0.36338(15) 0.39406(16) 0.0393(5) Uani 1 1 d . . . C1 C 0.1803(2) 0.1023(2) 0.4234(2) 0.0513(7) Uani 1 1 d . . . H1 H 0.1309 0.1450 0.4292 0.062 Uiso 1 1 calc R . . C2 C 0.1838(3) 0.0064(2) 0.4569(3) 0.0633(9) Uani 1 1 d . . . H2 H 0.1376 -0.0141 0.4841 0.076 Uiso 1 1 calc R . . C3 C 0.2552(3) -0.0560(2) 0.4495(2) 0.0604(9) Uani 1 1 d . . . H3 H 0.2592 -0.1200 0.4725 0.072 Uiso 1 1 calc R . . C4 C 0.3237(2) -0.02540(19) 0.4073(2) 0.0487(7) Uani 1 1 d . . . C5 C 0.4030(3) -0.0860(2) 0.3986(3) 0.0639(9) Uani 1 1 d . . . H5 H 0.4116 -0.1501 0.4225 0.077 Uiso 1 1 calc R . . C6 C 0.4650(3) -0.0524(2) 0.3568(3) 0.0668(9) Uani 1 1 d . . . H6 H 0.5177 -0.0934 0.3543 0.080 Uiso 1 1 calc R . . C7 C 0.4531(2) 0.0450(2) 0.3154(2) 0.0496(7) Uani 1 1 d . . . C8 C 0.5119(3) 0.0820(3) 0.2659(3) 0.0613(9) Uani 1 1 d . . . H8 H 0.5626 0.0426 0.2577 0.074 Uiso 1 1 calc R . . C9 C 0.4954(2) 0.1749(3) 0.2297(2) 0.0616(9) Uani 1 1 d . . . H9 H 0.5336 0.1999 0.1958 0.074 Uiso 1 1 calc R . . C10 C 0.4201(2) 0.2325(2) 0.2441(2) 0.0500(7) Uani 1 1 d . . . H10 H 0.4103 0.2968 0.2203 0.060 Uiso 1 1 calc R . . C11 C 0.37836(19) 0.10784(18) 0.32547(18) 0.0352(5) Uani 1 1 d . . . C12 C 0.3135(2) 0.07251(17) 0.37324(18) 0.0353(5) Uani 1 1 d . . . C13 C 0.0539(2) 0.4141(3) 0.3318(2) 0.0639(9) Uani 1 1 d . . . H13 H 0.0285 0.4129 0.2584 0.077 Uiso 1 1 calc R . . C14 C -0.0039(2) 0.4679(3) 0.3696(2) 0.0628(9) Uani 1 1 d . . . H14 H -0.0665 0.5023 0.3221 0.075 Uiso 1 1 calc R . . C15 C 0.02993(19) 0.47155(17) 0.47767(19) 0.0337(5) Uani 1 1 d . . . C16 C 0.1240(2) 0.4200(2) 0.5413(2) 0.0446(7) Uani 1 1 d . . . H16 H 0.1516 0.4201 0.6150 0.053 Uiso 1 1 calc R . . C17 C 0.1774(2) 0.3683(2) 0.4973(2) 0.0466(7) Uani 1 1 d . . . H17 H 0.2411 0.3345 0.5432 0.056 Uiso 1 1 calc R . . C18 C 0.0388(2) 0.29522(18) 0.09928(19) 0.0360(6) Uani 1 1 d . . . C19 C -0.07364(19) 0.25471(18) 0.02654(18) 0.0338(5) Uani 1 1 d . . . C20 C -0.13095(19) 0.20202(16) 0.06743(19) 0.0330(5) Uani 1 1 d . . . H20 H -0.0989 0.1899 0.1405 0.040 Uiso 1 1 calc R . . C21 C -0.23544(19) 0.16741(18) 0.0002(2) 0.0368(6) Uani 1 1 d . . . C22 C -0.2806(2) 0.1810(2) -0.1091(2) 0.0545(8) Uani 1 1 d . . . H22 H -0.3498 0.1551 -0.1548 0.065 Uiso 1 1 calc R . . C23 C -0.2240(3) 0.2322(3) -0.1501(2) 0.0649(9) Uani 1 1 d . . . H23 H -0.2544 0.2408 -0.2236 0.078 Uiso 1 1 calc R . . C24 C -0.1215(2) 0.2712(2) -0.0824(2) 0.0499(7) Uani 1 1 d . . . H24 H -0.0846 0.3087 -0.1101 0.060 Uiso 1 1 calc R . . H6B H 0.4520(12) 0.3298(19) 0.482(2) 0.071(10) Uiso 1 1 d D . . H6A H 0.385(2) 0.4043(10) 0.481(3) 0.077(11) Uiso 1 1 d D . . H7A H 0.2003(19) 0.414(2) 0.1762(15) 0.089(13) Uiso 1 1 d D . . H7B H 0.257(2) 0.4714(13) 0.2651(19) 0.061(10) 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 Mn1 0.0271(2) 0.0313(2) 0.0370(2) -0.00209(16) 0.01622(16) 0.00036(15) S1 0.0320(3) 0.0326(3) 0.0567(4) 0.0025(3) 0.0193(3) -0.0023(3) O1 0.0305(9) 0.0459(10) 0.0397(10) -0.0022(8) 0.0104(8) -0.0057(8) O2 0.0559(13) 0.0741(15) 0.0461(11) 0.0045(10) 0.0176(10) -0.0293(11) O3 0.0528(12) 0.0615(13) 0.0570(12) 0.0142(10) 0.0223(10) -0.0068(10) O4 0.0431(11) 0.0437(11) 0.1111(18) 0.0020(11) 0.0445(12) 0.0014(9) O5 0.0583(13) 0.0398(11) 0.0679(13) -0.0034(10) 0.0233(11) -0.0163(9) O6 0.0295(10) 0.0439(12) 0.0517(11) -0.0121(9) 0.0125(9) 0.0009(8) O7 0.0448(12) 0.0400(11) 0.0474(11) -0.0012(9) 0.0195(10) -0.0065(9) N1 0.0379(11) 0.0348(11) 0.0410(11) 0.0003(9) 0.0212(10) -0.0021(9) N2 0.0328(11) 0.0372(12) 0.0416(11) -0.0044(9) 0.0204(10) -0.0041(9) N3 0.0320(11) 0.0466(12) 0.0406(11) -0.0026(10) 0.0183(10) 0.0056(10) C1 0.0580(18) 0.0472(16) 0.0616(18) -0.0045(14) 0.0388(16) -0.0085(14) C2 0.085(2) 0.0546(19) 0.067(2) -0.0056(16) 0.0496(19) -0.0231(18) C3 0.081(2) 0.0373(16) 0.0576(18) 0.0055(14) 0.0291(18) -0.0175(16) C4 0.0552(18) 0.0305(14) 0.0463(15) -0.0038(12) 0.0124(14) -0.0011(13) C5 0.070(2) 0.0339(16) 0.072(2) -0.0070(15) 0.0206(19) 0.0066(15) C6 0.061(2) 0.0457(18) 0.081(2) -0.0226(17) 0.0229(19) 0.0143(16) C7 0.0399(15) 0.0515(17) 0.0537(16) -0.0215(14) 0.0191(14) 0.0005(13) C8 0.0463(18) 0.076(2) 0.068(2) -0.0278(18) 0.0322(16) 0.0001(16) C9 0.0482(18) 0.089(3) 0.0629(19) -0.0211(18) 0.0390(16) -0.0168(18) C10 0.0483(17) 0.0554(17) 0.0558(17) -0.0029(14) 0.0324(15) -0.0098(14) C11 0.0306(13) 0.0351(13) 0.0348(12) -0.0099(11) 0.0113(11) -0.0008(10) C12 0.0361(14) 0.0311(13) 0.0327(12) -0.0048(10) 0.0116(11) -0.0031(11) C13 0.0508(18) 0.097(3) 0.0366(15) -0.0094(16) 0.0146(14) 0.0308(17) C14 0.0465(17) 0.093(2) 0.0393(15) -0.0032(15) 0.0124(14) 0.0345(17) C15 0.0309(13) 0.0319(13) 0.0407(13) -0.0001(11) 0.0190(11) -0.0005(10) C16 0.0468(16) 0.0566(17) 0.0349(13) 0.0067(12) 0.0231(12) 0.0146(13) C17 0.0407(15) 0.0563(17) 0.0435(15) 0.0103(13) 0.0205(13) 0.0191(13) C18 0.0339(13) 0.0399(14) 0.0380(14) -0.0074(12) 0.0202(12) -0.0024(11) C19 0.0306(13) 0.0354(13) 0.0344(12) -0.0021(11) 0.0145(11) 0.0034(10) C20 0.0293(13) 0.0322(13) 0.0344(12) 0.0017(10) 0.0127(11) 0.0046(10) C21 0.0296(13) 0.0313(13) 0.0444(14) 0.0030(11) 0.0134(11) 0.0038(10) C22 0.0324(15) 0.070(2) 0.0441(16) 0.0038(14) 0.0040(13) -0.0084(14) C23 0.0483(18) 0.098(3) 0.0335(14) 0.0092(16) 0.0075(14) -0.0126(18) C24 0.0408(16) 0.0647(19) 0.0414(15) 0.0077(14) 0.0172(13) -0.0056(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 2.1143(16) . ? Mn1 O6 2.1694(18) . ? Mn1 O7 2.2001(19) . ? Mn1 N3 2.267(2) . ? Mn1 N2 2.269(2) . ? Mn1 N1 2.281(2) . ? S1 O3 1.443(2) . ? S1 O5 1.444(2) . ? S1 O4 1.448(2) . ? S1 C21 1.770(3) . ? O1 C18 1.262(3) . ? O2 C18 1.237(3) . ? O6 H6B 0.849(10) . ? O6 H6A 0.853(10) . ? O7 H7A 0.847(10) . ? O7 H7B 0.849(10) . ? N1 C1 1.324(3) . ? N1 C12 1.356(3) . ? N2 C10 1.317(3) . ? N2 C11 1.352(3) . ? N3 C17 1.315(3) . ? N3 C13 1.330(3) . ? C1 C2 1.391(4) . ? C1 H1 0.9300 . ? C2 C3 1.343(4) . ? C2 H2 0.9300 . ? C3 C4 1.398(4) . ? C3 H3 0.9300 . ? C4 C12 1.411(3) . ? C4 C5 1.421(4) . ? C5 C6 1.331(5) . ? C5 H5 0.9300 . ? C6 C7 1.437(5) . ? C6 H6 0.9300 . ? C7 C8 1.394(4) . ? C7 C11 1.399(3) . ? C8 C9 1.353(5) . ? C8 H8 0.9300 . ? C9 C10 1.392(4) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.437(3) . ? C13 C14 1.368(4) . ? C13 H13 0.9300 . ? C14 C15 1.379(4) . ? C14 H14 0.9300 . ? C15 C16 1.371(3) . ? C15 C15 1.478(5) 3_566 ? C16 C17 1.367(4) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.499(3) . ? C19 C20 1.383(3) . ? C19 C24 1.384(3) . ? C20 C21 1.378(3) . ? C20 H20 0.9300 . ? C21 C22 1.385(4) . ? C22 C23 1.368(4) . ? C22 H22 0.9300 . ? C23 C24 1.382(4) . ? C23 H23 0.9300 . ? C24 H24 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 O6 171.74(7) . . ? O1 Mn1 O7 89.51(7) . . ? O6 Mn1 O7 88.43(8) . . ? O1 Mn1 N3 87.87(7) . . ? O6 Mn1 N3 84.49(7) . . ? O7 Mn1 N3 97.68(7) . . ? O1 Mn1 N2 100.43(7) . . ? O6 Mn1 N2 87.65(7) . . ? O7 Mn1 N2 92.35(7) . . ? N3 Mn1 N2 167.06(7) . . ? O1 Mn1 N1 86.87(7) . . ? O6 Mn1 N1 97.26(7) . . ? O7 Mn1 N1 163.77(7) . . ? N3 Mn1 N1 97.99(7) . . ? N2 Mn1 N1 72.81(7) . . ? O3 S1 O5 113.96(12) . . ? O3 S1 O4 112.16(14) . . ? O5 S1 O4 112.23(12) . . ? O3 S1 C21 106.79(11) . . ? O5 S1 C21 106.31(12) . . ? O4 S1 C21 104.59(12) . . ? C18 O1 Mn1 130.92(16) . . ? Mn1 O6 H6B 124(2) . . ? Mn1 O6 H6A 117(2) . . ? H6B O6 H6A 106.9(15) . . ? Mn1 O7 H7A 104(2) . . ? Mn1 O7 H7B 113(2) . . ? H7A O7 H7B 108.2(16) . . ? C1 N1 C12 117.7(2) . . ? C1 N1 Mn1 126.78(18) . . ? C12 N1 Mn1 115.47(15) . . ? C10 N2 C11 117.7(2) . . ? C10 N2 Mn1 126.26(19) . . ? C11 N2 Mn1 115.97(15) . . ? C17 N3 C13 115.7(2) . . ? C17 N3 Mn1 123.62(17) . . ? C13 N3 Mn1 120.24(17) . . ? N1 C1 C2 123.6(3) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C3 C2 C1 118.8(3) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C2 C3 C4 120.6(3) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C3 C4 C12 117.0(3) . . ? C3 C4 C5 124.2(3) . . ? C12 C4 C5 118.8(3) . . ? C6 C5 C4 121.1(3) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C7 122.1(3) . . ? C5 C6 H6 118.9 . . ? C7 C6 H6 118.9 . . ? C8 C7 C11 117.2(3) . . ? C8 C7 C6 124.3(3) . . ? C11 C7 C6 118.4(3) . . ? C9 C8 C7 120.0(3) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 118.8(3) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? N2 C10 C9 123.5(3) . . ? N2 C10 H10 118.2 . . ? C9 C10 H10 118.2 . . ? N2 C11 C7 122.8(2) . . ? N2 C11 C12 117.8(2) . . ? C7 C11 C12 119.4(2) . . ? N1 C12 C4 122.3(2) . . ? N1 C12 C11 117.8(2) . . ? C4 C12 C11 119.9(2) . . ? N3 C13 C14 123.7(3) . . ? N3 C13 H13 118.1 . . ? C14 C13 H13 118.1 . . ? C13 C14 C15 120.3(3) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 115.5(2) . . ? C16 C15 C15 122.1(3) . 3_566 ? C14 C15 C15 122.4(3) . 3_566 ? C17 C16 C15 120.6(2) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? N3 C17 C16 124.2(2) . . ? N3 C17 H17 117.9 . . ? C16 C17 H17 117.9 . . ? O2 C18 O1 125.8(2) . . ? O2 C18 C19 118.1(2) . . ? O1 C18 C19 116.1(2) . . ? C20 C19 C24 119.5(2) . . ? C20 C19 C18 120.6(2) . . ? C24 C19 C18 119.9(2) . . ? C21 C20 C19 120.1(2) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 119.8(2) . . ? C20 C21 S1 121.44(19) . . ? C22 C21 S1 118.66(19) . . ? C23 C22 C21 120.3(3) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 120.0(3) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C19 120.1(3) . . ? C23 C24 H24 119.9 . . ? C19 C24 H24 119.9 . . ? 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 O7 Mn1 O1 C18 -0.3(2) . . . . ? N3 Mn1 O1 C18 97.4(2) . . . . ? N2 Mn1 O1 C18 -92.6(2) . . . . ? N1 Mn1 O1 C18 -164.5(2) . . . . ? O1 Mn1 N1 C1 -73.4(2) . . . . ? O6 Mn1 N1 C1 99.4(2) . . . . ? O7 Mn1 N1 C1 -150.8(3) . . . . ? N3 Mn1 N1 C1 14.0(2) . . . . ? N2 Mn1 N1 C1 -175.3(2) . . . . ? O1 Mn1 N1 C12 104.18(17) . . . . ? O6 Mn1 N1 C12 -83.00(17) . . . . ? O7 Mn1 N1 C12 26.8(4) . . . . ? N3 Mn1 N1 C12 -168.41(16) . . . . ? N2 Mn1 N1 C12 2.26(16) . . . . ? O1 Mn1 N2 C10 96.8(2) . . . . ? O6 Mn1 N2 C10 -81.4(2) . . . . ? O7 Mn1 N2 C10 6.9(2) . . . . ? N3 Mn1 N2 C10 -134.0(3) . . . . ? N1 Mn1 N2 C10 -179.8(2) . . . . ? O1 Mn1 N2 C11 -87.15(17) . . . . ? O6 Mn1 N2 C11 94.59(17) . . . . ? O7 Mn1 N2 C11 -177.08(17) . . . . ? N3 Mn1 N2 C11 42.1(4) . . . . ? N1 Mn1 N2 C11 -3.75(16) . . . . ? O1 Mn1 N3 C17 148.7(2) . . . . ? O6 Mn1 N3 C17 -34.4(2) . . . . ? O7 Mn1 N3 C17 -122.0(2) . . . . ? N2 Mn1 N3 C17 18.4(5) . . . . ? N1 Mn1 N3 C17 62.2(2) . . . . ? O1 Mn1 N3 C13 -39.1(2) . . . . ? O6 Mn1 N3 C13 137.7(2) . . . . ? O7 Mn1 N3 C13 50.1(2) . . . . ? N2 Mn1 N3 C13 -169.4(3) . . . . ? N1 Mn1 N3 C13 -125.7(2) . . . . ? C12 N1 C1 C2 1.4(4) . . . . ? Mn1 N1 C1 C2 178.9(2) . . . . ? N1 C1 C2 C3 0.3(5) . . . . ? C1 C2 C3 C4 -0.9(5) . . . . ? C2 C3 C4 C12 -0.3(4) . . . . ? C2 C3 C4 C5 178.7(3) . . . . ? C3 C4 C5 C6 179.4(3) . . . . ? C12 C4 C5 C6 -1.6(4) . . . . ? C4 C5 C6 C7 -2.0(5) . . . . ? C5 C6 C7 C8 -176.5(3) . . . . ? C5 C6 C7 C11 3.8(4) . . . . ? C11 C7 C8 C9 -0.1(4) . . . . ? C6 C7 C8 C9 -179.8(3) . . . . ? C7 C8 C9 C10 0.8(5) . . . . ? C11 N2 C10 C9 1.1(4) . . . . ? Mn1 N2 C10 C9 177.1(2) . . . . ? C8 C9 C10 N2 -1.3(5) . . . . ? C10 N2 C11 C7 -0.4(4) . . . . ? Mn1 N2 C11 C7 -176.79(18) . . . . ? C10 N2 C11 C12 -178.8(2) . . . . ? Mn1 N2 C11 C12 4.8(3) . . . . ? C8 C7 C11 N2 -0.1(4) . . . . ? C6 C7 C11 N2 179.6(2) . . . . ? C8 C7 C11 C12 178.3(2) . . . . ? C6 C7 C11 C12 -2.1(4) . . . . ? C1 N1 C12 C4 -2.7(4) . . . . ? Mn1 N1 C12 C4 179.53(19) . . . . ? C1 N1 C12 C11 177.2(2) . . . . ? Mn1 N1 C12 C11 -0.6(3) . . . . ? C3 C4 C12 N1 2.1(4) . . . . ? C5 C4 C12 N1 -176.9(2) . . . . ? C3 C4 C12 C11 -177.7(2) . . . . ? C5 C4 C12 C11 3.3(4) . . . . ? N2 C11 C12 N1 -2.8(3) . . . . ? C7 C11 C12 N1 178.7(2) . . . . ? N2 C11 C12 C4 177.0(2) . . . . ? C7 C11 C12 C4 -1.4(4) . . . . ? C17 N3 C13 C14 -0.7(5) . . . . ? Mn1 N3 C13 C14 -173.4(3) . . . . ? N3 C13 C14 C15 -0.4(6) . . . . ? C13 C14 C15 C16 1.1(5) . . . . ? C13 C14 C15 C15 -179.9(3) . . . 3_566 ? C14 C15 C16 C17 -0.8(4) . . . . ? C15 C15 C16 C17 -179.8(3) 3_566 . . . ? C13 N3 C17 C16 1.0(4) . . . . ? Mn1 N3 C17 C16 173.5(2) . . . . ? C15 C16 C17 N3 -0.3(5) . . . . ? Mn1 O1 C18 O2 5.6(4) . . . . ? Mn1 O1 C18 C19 -173.50(15) . . . . ? O2 C18 C19 C20 -156.8(2) . . . . ? O1 C18 C19 C20 22.4(3) . . . . ? O2 C18 C19 C24 22.3(4) . . . . ? O1 C18 C19 C24 -158.6(2) . . . . ? C24 C19 C20 C21 -0.8(4) . . . . ? C18 C19 C20 C21 178.2(2) . . . . ? C19 C20 C21 C22 3.5(4) . . . . ? C19 C20 C21 S1 -172.87(18) . . . . ? O3 S1 C21 C20 -19.0(2) . . . . ? O5 S1 C21 C20 -141.0(2) . . . . ? O4 S1 C21 C20 100.0(2) . . . . ? O3 S1 C21 C22 164.6(2) . . . . ? O5 S1 C21 C22 42.6(2) . . . . ? O4 S1 C21 C22 -76.3(2) . . . . ? C20 C21 C22 C23 -2.8(4) . . . . ? S1 C21 C22 C23 173.6(3) . . . . ? C21 C22 C23 C24 -0.4(5) . . . . ? C22 C23 C24 C19 3.0(5) . . . . ? C20 C19 C24 C23 -2.4(4) . . . . ? C18 C19 C24 C23 178.5(3) . . . . ? 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 O6 H6B O4 0.849(10) 1.891(12) 2.726(3) 168(3) 4_666 O6 H6A O5 0.853(10) 1.858(10) 2.707(3) 173(3) 2 O7 H7A O2 0.847(10) 1.833(15) 2.642(3) 159(3) . O7 H7B O3 0.849(10) 1.926(11) 2.769(3) 171(3) 2 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.282 _refine_diff_density_min -0.273 _refine_diff_density_rms 0.050 data_comp-5 _database_code_depnum_ccdc_archive 'CCDC 745969' #TrackingRef '- Final_cifdata.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H37 Mn N5 O10 S' _chemical_formula_weight 798.72 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 11.5737(8) _cell_length_b 14.5456(10) _cell_length_c 22.7033(15) _cell_angle_alpha 90.00 _cell_angle_beta 104.6000(10) _cell_angle_gamma 90.00 _cell_volume 3698.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3537 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 20.98 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1660 _exptl_absorpt_coefficient_mu 0.478 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8698 _exptl_absorpt_correction_T_max 0.9537 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker SMART area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 18967 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.20 _reflns_number_total 6658 _reflns_number_gt 4738 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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. The aromatic H atoms were positioned geometrically and were included in the refinement in the riding-model approximation [C-H= 0.93 /%A and U~iso~(H)=1.2 U~eq~(C)]. The coordinated water H atoms were also placed in calculated positions (O-H=0.85 /%A) with fixed isotropic displacement parameters. Due to the large U~eq~ values for lattice water molecules, H atoms on these lattice water molecules were not added. ; _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^)+(0.0667P)^2^+2.0954P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6658 _refine_ls_number_parameters 560 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0899 _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_ref 0.1657 _refine_ls_wR_factor_gt 0.1516 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.147 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean <0.001 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 0.23004(5) 0.25325(4) 0.48692(3) 0.0484(2) Uani 1 1 d . . . S1 S 0.39046(12) 0.10943(8) 0.21837(5) 0.0699(3) Uani 1 1 d . . . O1 O 0.3469(2) 0.24022(18) 0.42908(12) 0.0558(7) Uani 1 1 d . . . O2 O 0.4715(3) 0.3578(2) 0.45419(15) 0.0932(11) Uani 1 1 d . . . O6 O 0.3510(3) 0.3500(3) 0.54184(16) 0.0693(9) Uani 1 1 d . . . N1 N 0.1046(3) 0.3441(2) 0.41755(15) 0.0581(8) Uani 1 1 d . . . N2 N 0.0866(3) 0.3061(2) 0.53115(15) 0.0518(8) Uani 1 1 d . . . N3 N 0.1308(3) 0.1250(2) 0.44330(15) 0.0551(8) Uani 1 1 d . . . N4 N 0.2812(3) 0.1370(2) 0.55540(14) 0.0504(8) Uani 1 1 d . . . N5 N 0.7264(4) 0.1932(5) 0.6521(3) 0.1031(16) Uani 1 1 d . . . C1 C 0.1134(4) 0.3632(3) 0.3626(2) 0.0742(13) Uani 1 1 d . . . H1 H 0.1791 0.3407 0.3505 0.089 Uiso 1 1 calc R . . C2 C 0.0290(5) 0.4157(4) 0.3208(2) 0.0888(15) Uani 1 1 d . . . H2 H 0.0391 0.4275 0.2821 0.107 Uiso 1 1 calc R . . C3 C -0.0665(5) 0.4489(3) 0.3375(2) 0.0803(14) Uani 1 1 d . . . H3 H -0.1234 0.4835 0.3102 0.096 Uiso 1 1 calc R . . C4 C -0.0802(4) 0.4312(3) 0.3958(2) 0.0648(12) Uani 1 1 d . . . C5 C -0.1764(4) 0.4666(3) 0.4173(3) 0.0795(15) Uani 1 1 d . . . H5 H -0.2344 0.5026 0.3918 0.095 Uiso 1 1 calc R . . C6 C -0.1845(4) 0.4486(3) 0.4745(3) 0.0766(14) Uani 1 1 d . . . H6 H -0.2479 0.4725 0.4879 0.092 Uiso 1 1 calc R . . C7 C -0.0974(3) 0.3936(3) 0.5146(2) 0.0609(11) Uani 1 1 d . . . C8 C -0.1006(4) 0.3746(3) 0.5737(2) 0.0737(13) Uani 1 1 d . . . H8 H -0.1635 0.3965 0.5884 0.088 Uiso 1 1 calc R . . C9 C -0.0132(4) 0.3244(3) 0.6106(2) 0.0754(13) Uani 1 1 d . . . H9 H -0.0150 0.3122 0.6506 0.090 Uiso 1 1 calc R . . C10 C 0.0803(4) 0.2912(3) 0.5874(2) 0.0627(11) Uani 1 1 d . . . H10 H 0.1405 0.2570 0.6130 0.075 Uiso 1 1 calc R . . C11 C -0.0010(3) 0.3578(2) 0.49495(19) 0.0523(10) Uani 1 1 d . . . C12 C 0.0082(3) 0.3774(2) 0.43452(18) 0.0529(10) Uani 1 1 d . . . C13 C 0.0574(4) 0.1183(3) 0.3889(2) 0.0693(12) Uani 1 1 d . . . H13 H 0.0408 0.1713 0.3653 0.083 Uiso 1 1 calc R . . C14 C 0.0027(4) 0.0365(4) 0.3645(2) 0.0821(14) Uani 1 1 d . . . H14 H -0.0482 0.0350 0.3256 0.099 Uiso 1 1 calc R . . C15 C 0.0256(4) -0.0405(4) 0.3987(3) 0.0804(14) Uani 1 1 d . . . H15 H -0.0099 -0.0958 0.3832 0.096 Uiso 1 1 calc R . . C16 C 0.1013(4) -0.0379(3) 0.4564(2) 0.0676(12) Uani 1 1 d . . . C17 C 0.1306(5) -0.1162(3) 0.4952(3) 0.0830(15) Uani 1 1 d . . . H17 H 0.0975 -0.1729 0.4815 0.100 Uiso 1 1 calc R . . C18 C 0.2043(5) -0.1099(3) 0.5509(3) 0.0848(15) Uani 1 1 d . . . H18 H 0.2208 -0.1623 0.5750 0.102 Uiso 1 1 calc R . . C19 C 0.2583(4) -0.0246(3) 0.5741(2) 0.0647(11) Uani 1 1 d . . . C20 C 0.3355(4) -0.0153(4) 0.6306(2) 0.0789(14) Uani 1 1 d . . . H20 H 0.3537 -0.0662 0.6561 0.095 Uiso 1 1 calc R . . C21 C 0.3860(4) 0.0681(4) 0.6498(2) 0.0776(14) Uani 1 1 d . . . H21 H 0.4391 0.0748 0.6878 0.093 Uiso 1 1 calc R . . C22 C 0.3550(4) 0.1427(3) 0.61029(19) 0.0626(11) Uani 1 1 d . . . H22 H 0.3881 0.1998 0.6233 0.075 Uiso 1 1 calc R . . C23 C 0.2323(3) 0.0539(3) 0.53721(18) 0.0524(9) Uani 1 1 d . . . C24 C 0.1526(3) 0.0474(3) 0.47739(19) 0.0546(10) Uani 1 1 d . . . C25 C 0.6678(5) 0.0399(4) 0.6211(3) 0.0835(15) Uani 1 1 d . . . H25 H 0.6722 -0.0224 0.6306 0.100 Uiso 1 1 calc R . . C26 C 0.7282(5) 0.1048(6) 0.6623(2) 0.1010(19) Uani 1 1 d . . . H26 H 0.7732 0.0839 0.6998 0.121 Uiso 1 1 calc R . . C27 C 0.6617(5) 0.2184(4) 0.5984(3) 0.0961(17) Uani 1 1 d . . . H27 H 0.6577 0.2809 0.5894 0.115 Uiso 1 1 calc R . . C28 C 0.6013(4) 0.1613(4) 0.5558(2) 0.0793(13) Uani 1 1 d . . . H28 H 0.5583 0.1846 0.5185 0.095 Uiso 1 1 calc R . . C29 C 0.6018(4) 0.0704(3) 0.5660(2) 0.0659(12) Uani 1 1 d . . . C30 C 0.5333(5) -0.0081(5) 0.5238(3) 0.114(2) Uani 1 1 d . . . H30 H 0.5455 -0.0689 0.5366 0.137 Uiso 1 1 calc R . . C31 C 0.4274(3) 0.2930(3) 0.42017(17) 0.0528(9) Uani 1 1 d . . . C32 C 0.4733(3) 0.2736(2) 0.36575(16) 0.0468(9) Uani 1 1 d . A . C33 C 0.4190(3) 0.2096(2) 0.32303(15) 0.0460(8) Uani 1 1 d . . . H33 H 0.3530 0.1774 0.3284 0.055 Uiso 1 1 calc R A . C34 C 0.4611(3) 0.1928(3) 0.27255(16) 0.0496(9) Uani 1 1 d . A . C35 C 0.5592(4) 0.2393(3) 0.26418(19) 0.0679(12) Uani 1 1 d . . . H35 H 0.5878 0.2279 0.2301 0.082 Uiso 1 1 calc R A . C36 C 0.6145(4) 0.3028(4) 0.3069(2) 0.0833(15) Uani 1 1 d . A . H36 H 0.6813 0.3341 0.3017 0.100 Uiso 1 1 calc R . . C37 C 0.5720(4) 0.3207(3) 0.3572(2) 0.0711(13) Uani 1 1 d . . . H37 H 0.6095 0.3644 0.3854 0.085 Uiso 1 1 calc R A . O1W O 0.1805(7) 0.1558(6) 0.7182(3) 0.103(2) Uani 0.50 1 d P . . O2W O 0.3905(7) 0.5332(4) 0.4041(5) 0.290(5) Uani 1 1 d . . . O3W O 0.2940(9) 0.5102(6) 0.2870(5) 0.298(5) Uani 1 1 d . . . O4W O 0.8547(5) 0.1680(5) 0.2350(2) 0.185(3) Uani 1 1 d . . . O5W O 0.1023(7) 0.1960(7) 0.2625(3) 0.118(3) Uani 0.50 1 d P . . O4 O 0.4778(8) 0.0353(6) 0.2266(4) 0.106(3) Uani 0.641(11) 1 d PU A 1 O3 O 0.2845(6) 0.0763(6) 0.2376(3) 0.110(3) Uani 0.641(11) 1 d PU A 1 O5 O 0.3612(9) 0.1492(5) 0.1628(2) 0.100(3) Uani 0.641(11) 1 d PU A 1 O3' O 0.2693(9) 0.1409(10) 0.1987(6) 0.106(5) Uani 0.359(11) 1 d PU A 2 O4' O 0.4138(16) 0.0258(8) 0.2382(6) 0.097(5) Uani 0.359(11) 1 d PU A 2 O5' O 0.4433(11) 0.1303(7) 0.1620(4) 0.071(3) Uani 0.359(11) 1 d PU A 2 H6A H 0.365(4) 0.352(3) 0.582(2) 0.090 Uiso 1 1 d . . . H6B H 0.385(5) 0.360(4) 0.528(3) 0.090 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0511(3) 0.0456(4) 0.0483(4) 0.0040(3) 0.0122(3) 0.0013(3) S1 0.0929(9) 0.0645(8) 0.0431(6) -0.0075(5) 0.0003(5) -0.0086(6) O1 0.0579(15) 0.0588(17) 0.0550(16) -0.0025(12) 0.0220(13) -0.0092(13) O2 0.127(3) 0.082(2) 0.089(2) -0.0394(19) 0.061(2) -0.048(2) O6 0.074(2) 0.081(2) 0.0554(19) -0.0131(17) 0.0202(15) -0.0167(17) N1 0.062(2) 0.053(2) 0.056(2) 0.0046(16) 0.0066(16) 0.0018(16) N2 0.0522(18) 0.0434(19) 0.060(2) 0.0005(15) 0.0142(15) -0.0057(14) N3 0.0535(18) 0.055(2) 0.058(2) -0.0018(16) 0.0153(16) -0.0026(15) N4 0.0465(17) 0.050(2) 0.056(2) 0.0071(15) 0.0139(15) 0.0041(14) N5 0.080(3) 0.120(5) 0.114(4) -0.034(4) 0.033(3) -0.012(3) C1 0.082(3) 0.076(3) 0.061(3) 0.014(2) 0.012(2) 0.007(2) C2 0.110(4) 0.080(4) 0.066(3) 0.016(3) 0.003(3) 0.009(3) C3 0.087(3) 0.058(3) 0.077(3) 0.007(2) -0.015(3) 0.007(3) C4 0.060(3) 0.040(2) 0.081(3) -0.003(2) -0.009(2) -0.0067(19) C5 0.056(3) 0.051(3) 0.114(4) -0.014(3) -0.011(3) 0.004(2) C6 0.051(2) 0.054(3) 0.118(4) -0.021(3) 0.009(3) 0.000(2) C7 0.049(2) 0.043(2) 0.088(3) -0.015(2) 0.011(2) -0.0087(18) C8 0.062(3) 0.058(3) 0.106(4) -0.021(3) 0.030(3) -0.012(2) C9 0.082(3) 0.075(3) 0.078(3) -0.008(3) 0.035(3) -0.013(3) C10 0.063(3) 0.060(3) 0.066(3) 0.000(2) 0.020(2) -0.008(2) C11 0.0423(19) 0.035(2) 0.076(3) -0.0094(19) 0.0085(18) -0.0085(16) C12 0.051(2) 0.037(2) 0.064(3) -0.0035(18) 0.0013(19) -0.0075(17) C13 0.072(3) 0.066(3) 0.069(3) -0.007(2) 0.015(2) -0.003(2) C14 0.076(3) 0.093(4) 0.074(3) -0.025(3) 0.011(3) -0.015(3) C15 0.077(3) 0.068(3) 0.102(4) -0.025(3) 0.034(3) -0.017(3) C16 0.063(3) 0.057(3) 0.094(4) -0.009(2) 0.039(3) -0.010(2) C17 0.085(3) 0.048(3) 0.127(5) -0.003(3) 0.048(3) -0.013(2) C18 0.086(4) 0.049(3) 0.131(5) 0.019(3) 0.049(4) 0.002(3) C19 0.057(2) 0.055(3) 0.090(3) 0.020(2) 0.032(2) 0.009(2) C20 0.072(3) 0.074(3) 0.095(4) 0.038(3) 0.029(3) 0.016(3) C21 0.067(3) 0.092(4) 0.071(3) 0.029(3) 0.012(2) 0.013(3) C22 0.060(2) 0.060(3) 0.069(3) 0.012(2) 0.019(2) 0.004(2) C23 0.047(2) 0.051(2) 0.068(3) 0.007(2) 0.0286(19) 0.0045(18) C24 0.048(2) 0.048(2) 0.077(3) -0.002(2) 0.033(2) -0.0003(18) C25 0.084(3) 0.078(4) 0.097(4) 0.026(3) 0.039(3) 0.014(3) C26 0.085(4) 0.152(6) 0.065(3) 0.013(4) 0.016(3) 0.015(4) C27 0.081(4) 0.075(4) 0.140(6) 0.006(4) 0.044(4) -0.004(3) C28 0.066(3) 0.084(4) 0.086(4) 0.016(3) 0.016(3) 0.002(3) C29 0.056(2) 0.072(3) 0.076(3) -0.014(3) 0.027(2) -0.010(2) C30 0.098(5) 0.143(5) 0.126(6) 0.063(5) 0.075(4) 0.058(4) C31 0.060(2) 0.048(2) 0.051(2) -0.0017(19) 0.0160(19) -0.0057(19) C32 0.051(2) 0.045(2) 0.044(2) 0.0017(16) 0.0121(16) -0.0066(16) C33 0.0442(19) 0.043(2) 0.047(2) 0.0065(17) 0.0057(16) -0.0055(16) C34 0.058(2) 0.048(2) 0.040(2) 0.0021(17) 0.0064(17) 0.0000(18) C35 0.075(3) 0.081(3) 0.053(3) -0.005(2) 0.027(2) -0.011(2) C36 0.079(3) 0.103(4) 0.079(3) -0.018(3) 0.041(3) -0.045(3) C37 0.076(3) 0.074(3) 0.067(3) -0.018(2) 0.026(2) -0.037(2) O1W 0.104(5) 0.135(7) 0.073(4) 0.003(4) 0.028(4) -0.026(5) O2W 0.183(6) 0.101(4) 0.592(18) 0.000(7) 0.109(9) 0.002(4) O3W 0.343(12) 0.263(9) 0.356(12) 0.051(9) 0.215(10) -0.031(9) O4W 0.144(4) 0.268(7) 0.156(4) 0.091(5) 0.062(4) 0.095(4) O5W 0.088(5) 0.195(9) 0.066(4) -0.030(5) 0.008(4) 0.002(5) O4 0.112(5) 0.084(5) 0.110(5) -0.038(4) 0.007(4) 0.010(4) O3 0.113(5) 0.118(6) 0.094(5) -0.031(4) 0.018(4) -0.063(4) O5 0.133(7) 0.104(5) 0.048(3) 0.010(3) -0.003(4) -0.024(4) O3' 0.069(6) 0.131(9) 0.100(8) -0.034(7) -0.012(5) -0.001(5) O4' 0.152(10) 0.039(5) 0.075(6) 0.010(4) -0.018(7) -0.009(7) O5' 0.079(6) 0.090(6) 0.044(4) -0.013(4) 0.019(4) 0.000(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 2.118(3) . ? Mn1 O6 2.148(4) . ? Mn1 N4 2.272(3) . ? Mn1 N1 2.276(3) . ? Mn1 N2 2.279(3) . ? Mn1 N3 2.282(3) . ? S1 O4' 1.301(12) . ? S1 O5 1.352(5) . ? S1 O3' 1.435(10) . ? S1 O4 1.458(8) . ? S1 O3 1.482(6) . ? S1 O5' 1.580(10) . ? S1 C34 1.773(4) . ? O1 C31 1.262(4) . ? O2 C31 1.244(5) . ? O6 H6A 0.89(5) . ? O6 H6B 0.58(5) . ? N1 C1 1.308(5) . ? N1 C12 1.357(5) . ? N2 C10 1.316(5) . ? N2 C11 1.360(5) . ? N3 C13 1.314(5) . ? N3 C24 1.356(5) . ? N4 C22 1.324(5) . ? N4 C23 1.354(5) . ? N5 C26 1.305(7) . ? N5 C27 1.313(7) . ? C1 C2 1.404(6) . ? C1 H1 0.9300 . ? C2 C3 1.345(7) . ? C2 H2 0.9300 . ? C3 C4 1.396(6) . ? C3 H3 0.9300 . ? C4 C12 1.407(5) . ? C4 C5 1.420(6) . ? C5 C6 1.352(7) . ? C5 H5 0.9300 . ? C6 C7 1.421(6) . ? C6 H6 0.9300 . ? C7 C8 1.380(6) . ? C7 C11 1.403(5) . ? C8 C9 1.353(6) . ? C8 H8 0.9300 . ? C9 C10 1.402(6) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.431(5) . ? C13 C14 1.396(6) . ? C13 H13 0.9300 . ? C14 C15 1.350(7) . ? C14 H14 0.9300 . ? C15 C16 1.383(7) . ? C15 H15 0.9300 . ? C16 C24 1.405(5) . ? C16 C17 1.427(7) . ? C17 C18 1.337(7) . ? C17 H17 0.9300 . ? C18 C19 1.429(7) . ? C18 H18 0.9300 . ? C19 C20 1.374(6) . ? C19 C23 1.404(5) . ? C20 C21 1.370(7) . ? C20 H20 0.9300 . ? C21 C22 1.396(6) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.440(6) . ? C25 C29 1.364(7) . ? C25 C26 1.389(8) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.332(7) . ? C27 H27 0.9300 . ? C28 C29 1.342(6) . ? C28 H28 0.9300 . ? C29 C30 1.571(9) . ? C30 C30 1.183(11) 3_656 ? C30 H30 0.9300 . ? C31 C32 1.490(5) . ? C32 C33 1.377(5) . ? C32 C37 1.386(5) . ? C33 C34 1.376(5) . ? C33 H33 0.9300 . ? C34 C35 1.376(5) . ? C35 C36 1.374(6) . ? C35 H35 0.9300 . ? C36 C37 1.378(6) . ? C36 H36 0.9300 . ? C37 H37 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 O6 89.66(11) . . ? O1 Mn1 N4 105.11(10) . . ? O6 Mn1 N4 94.10(13) . . ? O1 Mn1 N1 91.07(11) . . ? O6 Mn1 N1 103.28(14) . . ? N4 Mn1 N1 156.36(12) . . ? O1 Mn1 N2 162.40(11) . . ? O6 Mn1 N2 87.91(12) . . ? N4 Mn1 N2 92.45(11) . . ? N1 Mn1 N2 72.57(12) . . ? O1 Mn1 N3 89.31(10) . . ? O6 Mn1 N3 166.09(14) . . ? N4 Mn1 N3 72.80(12) . . ? N1 Mn1 N3 90.61(12) . . ? N2 Mn1 N3 97.13(11) . . ? O4' S1 O5 134.8(7) . . ? O4' S1 O3' 120.5(9) . . ? O5 S1 O3' 65.0(6) . . ? O5 S1 O4 116.0(5) . . ? O3' S1 O4 150.2(6) . . ? O4' S1 O3 73.1(8) . . ? O5 S1 O3 112.5(4) . . ? O3' S1 O3 51.6(6) . . ? O4 S1 O3 108.7(5) . . ? O4' S1 O5' 111.8(8) . . ? O3' S1 O5' 103.5(7) . . ? O4 S1 O5' 81.3(5) . . ? O3 S1 O5' 144.9(4) . . ? O4' S1 C34 112.3(6) . . ? O5 S1 C34 108.5(3) . . ? O3' S1 C34 104.0(4) . . ? O4 S1 C34 103.5(3) . . ? O3 S1 C34 106.8(3) . . ? O5' S1 C34 103.0(4) . . ? C31 O1 Mn1 131.1(3) . . ? Mn1 O6 H6A 123(3) . . ? Mn1 O6 H6B 106(6) . . ? H6A O6 H6B 125(7) . . ? C1 N1 C12 117.6(4) . . ? C1 N1 Mn1 126.4(3) . . ? C12 N1 Mn1 115.9(3) . . ? C10 N2 C11 117.6(4) . . ? C10 N2 Mn1 126.6(3) . . ? C11 N2 Mn1 115.8(3) . . ? C13 N3 C24 117.3(4) . . ? C13 N3 Mn1 127.1(3) . . ? C24 N3 Mn1 115.6(3) . . ? C22 N4 C23 117.7(3) . . ? C22 N4 Mn1 126.3(3) . . ? C23 N4 Mn1 116.0(2) . . ? C26 N5 C27 114.8(6) . . ? N1 C1 C2 123.5(5) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C3 C2 C1 119.1(5) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 119.9(4) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C12 117.1(4) . . ? C3 C4 C5 123.1(4) . . ? C12 C4 C5 119.8(5) . . ? C6 C5 C4 120.7(4) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C7 121.0(4) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C8 C7 C11 117.0(4) . . ? C8 C7 C6 123.2(4) . . ? C11 C7 C6 119.9(5) . . ? C9 C8 C7 120.7(4) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 118.8(5) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? N2 C10 C9 122.9(4) . . ? N2 C10 H10 118.5 . . ? C9 C10 H10 118.5 . . ? N2 C11 C7 123.0(4) . . ? N2 C11 C12 117.7(3) . . ? C7 C11 C12 119.2(4) . . ? N1 C12 C4 122.8(4) . . ? N1 C12 C11 117.8(3) . . ? C4 C12 C11 119.4(4) . . ? N3 C13 C14 123.9(5) . . ? N3 C13 H13 118.1 . . ? C14 C13 H13 118.1 . . ? C15 C14 C13 118.4(5) . . ? C15 C14 H14 120.8 . . ? C13 C14 H14 120.8 . . ? C14 C15 C16 120.5(5) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C24 117.3(4) . . ? C15 C16 C17 124.0(5) . . ? C24 C16 C17 118.8(5) . . ? C18 C17 C16 121.6(5) . . ? C18 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? C17 C18 C19 121.5(5) . . ? C17 C18 H18 119.2 . . ? C19 C18 H18 119.2 . . ? C20 C19 C23 118.0(4) . . ? C20 C19 C18 123.4(4) . . ? C23 C19 C18 118.6(5) . . ? C21 C20 C19 120.6(4) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C22 117.7(5) . . ? C20 C21 H21 121.2 . . ? C22 C21 H21 121.2 . . ? N4 C22 C21 123.8(4) . . ? N4 C22 H22 118.1 . . ? C21 C22 H22 118.1 . . ? N4 C23 C19 122.3(4) . . ? N4 C23 C24 117.8(3) . . ? C19 C23 C24 119.9(4) . . ? N3 C24 C16 122.7(4) . . ? N3 C24 C23 117.8(3) . . ? C16 C24 C23 119.6(4) . . ? C29 C25 C26 117.9(5) . . ? C29 C25 H25 121.1 . . ? C26 C25 H25 121.1 . . ? N5 C26 C25 124.5(5) . . ? N5 C26 H26 117.7 . . ? C25 C26 H26 117.7 . . ? N5 C27 C28 125.0(6) . . ? N5 C27 H27 117.5 . . ? C28 C27 H27 117.5 . . ? C27 C28 C29 120.7(5) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C28 C29 C25 117.1(5) . . ? C28 C29 C30 129.1(5) . . ? C25 C29 C30 113.7(5) . . ? C30 C30 C29 121.6(9) 3_656 . ? C30 C30 H30 119.2 3_656 . ? C29 C30 H30 119.2 . . ? O2 C31 O1 124.4(4) . . ? O2 C31 C32 118.8(3) . . ? O1 C31 C32 116.8(3) . . ? C33 C32 C37 118.8(3) . . ? C33 C32 C31 121.1(3) . . ? C37 C32 C31 120.1(3) . . ? C34 C33 C32 120.8(3) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C33 C34 C35 120.4(3) . . ? C33 C34 S1 120.1(3) . . ? C35 C34 S1 119.5(3) . . ? C36 C35 C34 119.1(4) . . ? C36 C35 H35 120.4 . . ? C34 C35 H35 120.4 . . ? C35 C36 C37 120.8(4) . . ? C35 C36 H36 119.6 . . ? C37 C36 H36 119.6 . . ? C36 C37 C32 120.1(4) . . ? C36 C37 H37 119.9 . . ? C32 C37 H37 119.9 . . ? 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 O6 Mn1 O1 C31 -21.5(3) . . . . ? N4 Mn1 O1 C31 -115.7(3) . . . . ? N1 Mn1 O1 C31 81.8(3) . . . . ? N2 Mn1 O1 C31 60.5(5) . . . . ? N3 Mn1 O1 C31 172.4(3) . . . . ? O1 Mn1 N1 C1 6.1(4) . . . . ? O6 Mn1 N1 C1 96.0(4) . . . . ? N4 Mn1 N1 C1 -127.7(4) . . . . ? N2 Mn1 N1 C1 179.5(4) . . . . ? N3 Mn1 N1 C1 -83.2(4) . . . . ? O1 Mn1 N1 C12 -177.5(3) . . . . ? O6 Mn1 N1 C12 -87.6(3) . . . . ? N4 Mn1 N1 C12 48.7(4) . . . . ? N2 Mn1 N1 C12 -4.1(2) . . . . ? N3 Mn1 N1 C12 93.2(3) . . . . ? O1 Mn1 N2 C10 -154.4(3) . . . . ? O6 Mn1 N2 C10 -72.1(3) . . . . ? N4 Mn1 N2 C10 21.9(3) . . . . ? N1 Mn1 N2 C10 -176.8(3) . . . . ? N3 Mn1 N2 C10 94.9(3) . . . . ? O1 Mn1 N2 C11 26.0(5) . . . . ? O6 Mn1 N2 C11 108.2(3) . . . . ? N4 Mn1 N2 C11 -157.7(2) . . . . ? N1 Mn1 N2 C11 3.6(2) . . . . ? N3 Mn1 N2 C11 -84.8(2) . . . . ? O1 Mn1 N3 C13 -74.1(3) . . . . ? O6 Mn1 N3 C13 -159.9(4) . . . . ? N4 Mn1 N3 C13 179.9(4) . . . . ? N1 Mn1 N3 C13 17.0(3) . . . . ? N2 Mn1 N3 C13 89.5(3) . . . . ? O1 Mn1 N3 C24 104.7(3) . . . . ? O6 Mn1 N3 C24 18.9(6) . . . . ? N4 Mn1 N3 C24 -1.4(2) . . . . ? N1 Mn1 N3 C24 -164.3(3) . . . . ? N2 Mn1 N3 C24 -91.7(3) . . . . ? O1 Mn1 N4 C22 95.4(3) . . . . ? O6 Mn1 N4 C22 4.7(3) . . . . ? N1 Mn1 N4 C22 -132.9(3) . . . . ? N2 Mn1 N4 C22 -83.4(3) . . . . ? N3 Mn1 N4 C22 179.9(3) . . . . ? O1 Mn1 N4 C23 -83.4(2) . . . . ? O6 Mn1 N4 C23 -174.1(2) . . . . ? N1 Mn1 N4 C23 48.3(4) . . . . ? N2 Mn1 N4 C23 97.8(2) . . . . ? N3 Mn1 N4 C23 1.1(2) . . . . ? C12 N1 C1 C2 0.0(7) . . . . ? Mn1 N1 C1 C2 176.3(4) . . . . ? N1 C1 C2 C3 0.1(8) . . . . ? C1 C2 C3 C4 0.4(8) . . . . ? C2 C3 C4 C12 -0.8(6) . . . . ? C2 C3 C4 C5 177.7(4) . . . . ? C3 C4 C5 C6 -179.0(4) . . . . ? C12 C4 C5 C6 -0.5(6) . . . . ? C4 C5 C6 C7 -0.2(7) . . . . ? C5 C6 C7 C8 178.8(4) . . . . ? C5 C6 C7 C11 0.4(6) . . . . ? C11 C7 C8 C9 0.7(6) . . . . ? C6 C7 C8 C9 -177.8(4) . . . . ? C7 C8 C9 C10 -0.7(6) . . . . ? C11 N2 C10 C9 1.3(6) . . . . ? Mn1 N2 C10 C9 -178.3(3) . . . . ? C8 C9 C10 N2 -0.4(7) . . . . ? C10 N2 C11 C7 -1.3(5) . . . . ? Mn1 N2 C11 C7 178.4(3) . . . . ? C10 N2 C11 C12 177.5(3) . . . . ? Mn1 N2 C11 C12 -2.9(4) . . . . ? C8 C7 C11 N2 0.3(5) . . . . ? C6 C7 C11 N2 178.8(3) . . . . ? C8 C7 C11 C12 -178.4(3) . . . . ? C6 C7 C11 C12 0.1(5) . . . . ? C1 N1 C12 C4 -0.4(6) . . . . ? Mn1 N1 C12 C4 -177.2(3) . . . . ? C1 N1 C12 C11 -179.1(3) . . . . ? Mn1 N1 C12 C11 4.1(4) . . . . ? C3 C4 C12 N1 0.9(6) . . . . ? C5 C4 C12 N1 -177.7(4) . . . . ? C3 C4 C12 C11 179.5(3) . . . . ? C5 C4 C12 C11 1.0(5) . . . . ? N2 C11 C12 N1 -0.8(5) . . . . ? C7 C11 C12 N1 178.0(3) . . . . ? N2 C11 C12 C4 -179.6(3) . . . . ? C7 C11 C12 C4 -0.7(5) . . . . ? C24 N3 C13 C14 -0.9(6) . . . . ? Mn1 N3 C13 C14 177.8(3) . . . . ? N3 C13 C14 C15 0.5(7) . . . . ? C13 C14 C15 C16 0.0(7) . . . . ? C14 C15 C16 C24 -0.1(7) . . . . ? C14 C15 C16 C17 -179.6(4) . . . . ? C15 C16 C17 C18 -179.9(5) . . . . ? C24 C16 C17 C18 0.6(7) . . . . ? C16 C17 C18 C19 -0.5(8) . . . . ? C17 C18 C19 C20 -179.2(5) . . . . ? C17 C18 C19 C23 0.1(7) . . . . ? C23 C19 C20 C21 -0.6(6) . . . . ? C18 C19 C20 C21 178.8(4) . . . . ? C19 C20 C21 C22 0.8(7) . . . . ? C23 N4 C22 C21 0.8(6) . . . . ? Mn1 N4 C22 C21 -178.0(3) . . . . ? C20 C21 C22 N4 -0.9(7) . . . . ? C22 N4 C23 C19 -0.6(5) . . . . ? Mn1 N4 C23 C19 178.3(3) . . . . ? C22 N4 C23 C24 -179.6(3) . . . . ? Mn1 N4 C23 C24 -0.7(4) . . . . ? C20 C19 C23 N4 0.5(6) . . . . ? C18 C19 C23 N4 -178.9(4) . . . . ? C20 C19 C23 C24 179.5(4) . . . . ? C18 C19 C23 C24 0.1(6) . . . . ? C13 N3 C24 C16 0.8(5) . . . . ? Mn1 N3 C24 C16 -178.1(3) . . . . ? C13 N3 C24 C23 -179.6(3) . . . . ? Mn1 N3 C24 C23 1.5(4) . . . . ? C15 C16 C24 N3 -0.3(6) . . . . ? C17 C16 C24 N3 179.3(4) . . . . ? C15 C16 C24 C23 -179.9(4) . . . . ? C17 C16 C24 C23 -0.4(6) . . . . ? N4 C23 C24 N3 -0.6(5) . . . . ? C19 C23 C24 N3 -179.6(3) . . . . ? N4 C23 C24 C16 179.1(3) . . . . ? C19 C23 C24 C16 0.0(5) . . . . ? C27 N5 C26 C25 -0.2(8) . . . . ? C29 C25 C26 N5 0.0(8) . . . . ? C26 N5 C27 C28 -0.3(8) . . . . ? N5 C27 C28 C29 0.9(8) . . . . ? C27 C28 C29 C25 -1.0(7) . . . . ? C27 C28 C29 C30 177.2(5) . . . . ? C26 C25 C29 C28 0.6(7) . . . . ? C26 C25 C29 C30 -177.8(4) . . . . ? C28 C29 C30 C30 -2.9(10) . . . 3_656 ? C25 C29 C30 C30 175.3(7) . . . 3_656 ? Mn1 O1 C31 O2 15.6(6) . . . . ? Mn1 O1 C31 C32 -165.8(2) . . . . ? O2 C31 C32 C33 -172.7(4) . . . . ? O1 C31 C32 C33 8.7(5) . . . . ? O2 C31 C32 C37 7.0(6) . . . . ? O1 C31 C32 C37 -171.7(4) . . . . ? C37 C32 C33 C34 -0.3(6) . . . . ? C31 C32 C33 C34 179.3(3) . . . . ? C32 C33 C34 C35 0.6(6) . . . . ? C32 C33 C34 S1 179.5(3) . . . . ? O4' S1 C34 C33 -73.6(10) . . . . ? O5 S1 C34 C33 126.2(6) . . . . ? O3' S1 C34 C33 58.2(8) . . . . ? O4 S1 C34 C33 -110.0(5) . . . . ? O3 S1 C34 C33 4.6(5) . . . . ? O5' S1 C34 C33 166.0(5) . . . . ? O4' S1 C34 C35 105.4(10) . . . . ? O5 S1 C34 C35 -54.9(6) . . . . ? O3' S1 C34 C35 -122.8(8) . . . . ? O4 S1 C34 C35 68.9(5) . . . . ? O3 S1 C34 C35 -176.4(5) . . . . ? O5' S1 C34 C35 -15.1(6) . . . . ? C33 C34 C35 C36 -0.1(6) . . . . ? S1 C34 C35 C36 -179.0(4) . . . . ? C34 C35 C36 C37 -0.6(7) . . . . ? C35 C36 C37 C32 0.9(8) . . . . ? C33 C32 C37 C36 -0.4(7) . . . . ? C31 C32 C37 C36 180.0(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.669 _refine_diff_density_min -0.223 _refine_diff_density_rms 0.065 data_comp-6 _database_code_depnum_ccdc_archive 'CCDC 745970' #TrackingRef '- Final_cifdata.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H29 Mn N5 O7 S' _chemical_formula_weight 742.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7849(15) _cell_length_b 11.3475(16) _cell_length_c 14.816(2) _cell_angle_alpha 100.9090(10) _cell_angle_beta 97.8040(10) _cell_angle_gamma 109.9110(10) _cell_volume 1634.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 4138 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 26.6 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 766 _exptl_absorpt_coefficient_mu 0.529 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.904 _exptl_absorpt_correction_T_max 0.922 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker SMART area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 12170 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.20 _reflns_number_total 5822 _reflns_number_gt 4817 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0491P)^2^+0.1932P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5822 _refine_ls_number_parameters 499 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.0999 _refine_ls_wR_factor_gt 0.0946 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean <0.001 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 0.78762(3) 0.90487(3) 0.23534(2) 0.03350(12) Uani 1 1 d . . . S1 S 0.69025(7) 0.32481(7) 0.38012(6) 0.0573(2) Uani 1 1 d . . . O1 O 0.65975(16) 0.72736(14) 0.25872(12) 0.0445(4) Uani 1 1 d . . . O2 O 0.47947(17) 0.75851(16) 0.29694(13) 0.0540(5) Uani 1 1 d . . . O3 O 0.8015(3) 0.3921(4) 0.3388(3) 0.0963(16) Uani 0.766(7) 1 d PU A 1 O4 O 0.7243(5) 0.3283(5) 0.4731(2) 0.0910(16) Uani 0.766(7) 1 d PU A 1 O5 O 0.6156(5) 0.1968(4) 0.3169(4) 0.117(2) Uani 0.766(7) 1 d PU A 1 O3' O 0.8144(8) 0.4258(8) 0.4284(10) 0.075(4) Uani 0.234(7) 1 d PU A 2 O4' O 0.6399(15) 0.2453(15) 0.4540(11) 0.100(5) Uani 0.234(7) 1 d PU A 2 O5' O 0.6803(13) 0.2364(12) 0.3066(7) 0.056(3) Uani 0.234(7) 1 d PU A 2 O6 O 0.63456(17) 0.97533(16) 0.26278(14) 0.0510(4) Uani 1 1 d D . . H6A H 0.5762 0.9213 0.2796 0.076 Uiso 1 1 calc RD . . O1W O 0.0775(2) 0.4666(3) 0.36776(18) 0.0896(7) Uani 1 1 d D . . H6B H 0.633(2) 1.0504(9) 0.2816(18) 0.069(9) Uiso 1 1 d D . . H1WA H -0.0054(12) 0.456(3) 0.367(2) 0.100 Uiso 1 1 d D . . H1WB H 0.121(2) 0.521(3) 0.4209(14) 0.100 Uiso 1 1 d D . . N1 N 0.94049(18) 1.03964(17) 0.36742(12) 0.0369(4) Uani 1 1 d . . . N2 N 0.95178(18) 0.82582(17) 0.25887(13) 0.0354(4) Uani 1 1 d . . . N3 N 0.88414(18) 1.06518(17) 0.15966(13) 0.0382(4) Uani 1 1 d . . . N4 N 0.72892(18) 0.81320(17) 0.07889(13) 0.0375(4) Uani 1 1 d . . . N5 N 0.7719(3) 0.4391(2) 0.04400(19) 0.0688(7) Uani 1 1 d . . . C1 C 0.9335(3) 1.1434(2) 0.42158(16) 0.0442(6) Uani 1 1 d . . . H1 H 0.8545 1.1592 0.4102 0.053 Uiso 1 1 calc R . . C2 C 1.0388(3) 1.2294(2) 0.49442(18) 0.0540(7) Uani 1 1 d . . . H2 H 1.0308 1.3020 0.5304 0.065 Uiso 1 1 calc R . . C3 C 1.1537(3) 1.2059(2) 0.51231(18) 0.0564(7) Uani 1 1 d . . . H3 H 1.2250 1.2626 0.5612 0.068 Uiso 1 1 calc R . . C4 C 1.1656(2) 1.0974(2) 0.45808(17) 0.0453(6) Uani 1 1 d . . . C5 C 1.2816(3) 1.0639(3) 0.4743(2) 0.0620(8) Uani 1 1 d . . . H5 H 1.3557 1.1183 0.5220 0.074 Uiso 1 1 calc R . . C6 C 1.2857(3) 0.9553(3) 0.4221(2) 0.0642(8) Uani 1 1 d . . . H6 H 1.3621 0.9355 0.4345 0.077 Uiso 1 1 calc R . . C7 C 1.1743(2) 0.8698(2) 0.34776(19) 0.0480(6) Uani 1 1 d . . . C8 C 1.1701(3) 0.7525(3) 0.2941(2) 0.0621(8) Uani 1 1 d . . . H8 H 1.2436 0.7278 0.3045 0.075 Uiso 1 1 calc R . . C9 C 1.0583(3) 0.6748(3) 0.2268(2) 0.0608(8) Uani 1 1 d . . . H9 H 1.0537 0.5956 0.1918 0.073 Uiso 1 1 calc R . . C10 C 0.9511(3) 0.7147(2) 0.21045(18) 0.0467(6) Uani 1 1 d . . . H10 H 0.8755 0.6612 0.1636 0.056 Uiso 1 1 calc R . . C11 C 1.0606(2) 0.9015(2) 0.32808(16) 0.0355(5) Uani 1 1 d . . . C12 C 1.0557(2) 1.0169(2) 0.38510(15) 0.0355(5) Uani 1 1 d . . . C13 C 0.9632(3) 1.1882(2) 0.19843(19) 0.0477(6) Uani 1 1 d . . . H13 H 0.9866 1.2167 0.2638 0.057 Uiso 1 1 calc R . . C14 C 1.0128(3) 1.2765(2) 0.1465(2) 0.0522(7) Uani 1 1 d . . . H14 H 1.0678 1.3619 0.1769 0.063 Uiso 1 1 calc R . . C15 C 0.9806(3) 1.2378(2) 0.0512(2) 0.0519(7) Uani 1 1 d . . . H15 H 1.0141 1.2960 0.0157 0.062 Uiso 1 1 calc R . . C16 C 0.8961(2) 1.1089(2) 0.00681(17) 0.0425(6) Uani 1 1 d . . . C17 C 0.8534(3) 1.0602(3) -0.09302(18) 0.0561(7) Uani 1 1 d . . . H17 H 0.8818 1.1159 -0.1313 0.067 Uiso 1 1 calc R . . C18 C 0.7739(3) 0.9368(3) -0.13267(19) 0.0574(7) Uani 1 1 d . . . H18 H 0.7469 0.9084 -0.1979 0.069 Uiso 1 1 calc R . . C19 C 0.7296(2) 0.8480(2) -0.07713(16) 0.0428(6) Uani 1 1 d . . . C20 C 0.6495(3) 0.7170(3) -0.11513(19) 0.0540(7) Uani 1 1 d . . . H20 H 0.6213 0.6841 -0.1801 0.065 Uiso 1 1 calc R . . C21 C 0.6130(3) 0.6380(3) -0.05767(19) 0.0537(7) Uani 1 1 d . . . H21 H 0.5609 0.5504 -0.0826 0.064 Uiso 1 1 calc R . . C22 C 0.6541(2) 0.6893(2) 0.03910(18) 0.0478(6) Uani 1 1 d . . . H22 H 0.6279 0.6341 0.0780 0.057 Uiso 1 1 calc R . . C23 C 0.7679(2) 0.8919(2) 0.02162(16) 0.0350(5) Uani 1 1 d . . . C24 C 0.8516(2) 1.0258(2) 0.06425(16) 0.0347(5) Uani 1 1 d . . . C25 C 0.6601(3) 0.2469(3) 0.09139(19) 0.0548(7) Uani 1 1 d . . . H25 H 0.6417 0.2085 0.1407 0.066 Uiso 1 1 calc R . . C26 C 0.7406(3) 0.3756(3) 0.1097(2) 0.0646(8) Uani 1 1 d . . . H26 H 0.7756 0.4217 0.1724 0.078 Uiso 1 1 calc R . . C27 C 0.7198(3) 0.3688(3) -0.0444(2) 0.0671(8) Uani 1 1 d . . . H27 H 0.7395 0.4098 -0.0923 0.080 Uiso 1 1 calc R . . C28 C 0.6389(3) 0.2396(3) -0.0695(2) 0.0581(7) Uani 1 1 d . . . H28 H 0.6059 0.1959 -0.1328 0.070 Uiso 1 1 calc R . . C29 C 0.6064(2) 0.1746(3) -0.00114(18) 0.0485(6) Uani 1 1 d . . . C30 C 0.5186(3) 0.0368(3) -0.02847(18) 0.0506(6) Uani 1 1 d . . . H30 H 0.4862 -0.0017 -0.0926 0.061 Uiso 1 1 calc R . . C31 C 0.5519(2) 0.6945(2) 0.28882(15) 0.0346(5) Uani 1 1 d . . . C32 C 0.5143(2) 0.5711(2) 0.32056(15) 0.0321(5) Uani 1 1 d . A . C33 C 0.6037(2) 0.5081(2) 0.32849(15) 0.0341(5) Uani 1 1 d . . . H33 H 0.6848 0.5385 0.3092 0.041 Uiso 1 1 calc R A . C34 C 0.5733(2) 0.4012(2) 0.36458(16) 0.0368(5) Uani 1 1 d . A . C35 C 0.4511(3) 0.3530(2) 0.39029(18) 0.0488(6) Uani 1 1 d . . . H35 H 0.4301 0.2802 0.4143 0.059 Uiso 1 1 calc R A . C36 C 0.3604(3) 0.4130(2) 0.3803(2) 0.0543(7) Uani 1 1 d . A . H36 H 0.2773 0.3797 0.3965 0.065 Uiso 1 1 calc R . . C37 C 0.3923(2) 0.5221(2) 0.34643(17) 0.0440(6) Uani 1 1 d . . . H37 H 0.3313 0.5631 0.3409 0.053 Uiso 1 1 calc R A . 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 0.0329(2) 0.02950(19) 0.0391(2) 0.01082(15) 0.00681(15) 0.01215(15) S1 0.0580(4) 0.0468(4) 0.0763(5) 0.0122(4) 0.0104(4) 0.0345(3) O1 0.0409(9) 0.0367(9) 0.0635(11) 0.0209(8) 0.0238(8) 0.0150(7) O2 0.0438(10) 0.0502(10) 0.0883(14) 0.0360(10) 0.0268(9) 0.0282(9) O3 0.064(2) 0.149(3) 0.131(4) 0.080(3) 0.049(2) 0.073(2) O4 0.116(4) 0.129(4) 0.065(2) 0.038(2) 0.010(2) 0.089(3) O5 0.108(4) 0.056(3) 0.182(4) -0.010(2) 0.016(3) 0.052(3) O3' 0.042(5) 0.044(5) 0.122(9) 0.000(5) -0.021(5) 0.020(4) O4' 0.086(8) 0.111(8) 0.129(8) 0.071(7) 0.013(6) 0.051(6) O5' 0.090(7) 0.064(7) 0.034(4) 0.011(4) 0.010(4) 0.053(6) O6 0.0461(10) 0.0359(10) 0.0771(13) 0.0150(9) 0.0204(9) 0.0200(8) O1W 0.0620(14) 0.102(2) 0.100(2) 0.0184(15) 0.0238(13) 0.0266(14) N1 0.0414(11) 0.0346(10) 0.0365(11) 0.0118(8) 0.0059(9) 0.0160(9) N2 0.0345(10) 0.0319(10) 0.0440(11) 0.0131(9) 0.0124(9) 0.0145(8) N3 0.0392(11) 0.0328(10) 0.0426(12) 0.0106(9) 0.0071(9) 0.0136(9) N4 0.0349(10) 0.0341(10) 0.0418(11) 0.0107(9) 0.0055(8) 0.0115(9) N5 0.0786(18) 0.0510(14) 0.0716(18) 0.0081(14) 0.0173(14) 0.0217(13) C1 0.0599(16) 0.0357(13) 0.0417(14) 0.0126(11) 0.0113(12) 0.0222(12) C2 0.081(2) 0.0339(13) 0.0421(15) 0.0099(12) 0.0085(14) 0.0170(14) C3 0.0656(18) 0.0426(15) 0.0400(15) 0.0128(12) -0.0042(13) -0.0010(13) C4 0.0450(14) 0.0424(14) 0.0409(14) 0.0199(12) 0.0020(11) 0.0049(11) C5 0.0391(15) 0.070(2) 0.0645(19) 0.0303(16) -0.0063(13) 0.0050(14) C6 0.0344(14) 0.077(2) 0.087(2) 0.0384(18) 0.0052(14) 0.0218(14) C7 0.0356(13) 0.0539(16) 0.0651(17) 0.0318(14) 0.0155(12) 0.0192(12) C8 0.0490(17) 0.0646(18) 0.098(2) 0.0394(17) 0.0293(16) 0.0379(15) C9 0.0613(18) 0.0433(15) 0.095(2) 0.0220(15) 0.0323(17) 0.0320(14) C10 0.0471(14) 0.0343(13) 0.0619(17) 0.0130(12) 0.0200(12) 0.0158(11) C11 0.0315(12) 0.0378(12) 0.0436(13) 0.0216(11) 0.0128(10) 0.0131(10) C12 0.0357(12) 0.0336(12) 0.0375(12) 0.0188(10) 0.0065(10) 0.0087(10) C13 0.0514(15) 0.0341(13) 0.0526(15) 0.0100(11) 0.0079(12) 0.0119(12) C14 0.0533(16) 0.0323(13) 0.0664(19) 0.0145(13) 0.0136(14) 0.0091(12) C15 0.0549(16) 0.0455(15) 0.0683(19) 0.0305(14) 0.0268(14) 0.0212(13) C16 0.0433(14) 0.0439(14) 0.0502(15) 0.0210(12) 0.0188(11) 0.0204(11) C17 0.0705(19) 0.0631(18) 0.0489(16) 0.0295(14) 0.0273(14) 0.0291(16) C18 0.0686(18) 0.0664(19) 0.0405(15) 0.0154(14) 0.0157(13) 0.0272(16) C19 0.0420(13) 0.0495(14) 0.0407(14) 0.0095(11) 0.0097(11) 0.0227(12) C20 0.0515(16) 0.0566(17) 0.0452(15) -0.0015(13) 0.0023(12) 0.0203(14) C21 0.0484(15) 0.0414(14) 0.0559(17) -0.0024(13) 0.0018(13) 0.0093(12) C22 0.0471(14) 0.0349(13) 0.0557(16) 0.0098(12) 0.0101(12) 0.0096(11) C23 0.0314(12) 0.0365(12) 0.0416(13) 0.0101(10) 0.0078(10) 0.0182(10) C24 0.0332(12) 0.0380(12) 0.0405(13) 0.0138(10) 0.0109(10) 0.0196(10) C25 0.0550(16) 0.0576(17) 0.0543(17) 0.0123(14) 0.0093(13) 0.0264(14) C26 0.0657(19) 0.0574(18) 0.0614(19) -0.0032(15) 0.0090(15) 0.0232(16) C27 0.079(2) 0.0575(19) 0.070(2) 0.0188(16) 0.0197(17) 0.0302(17) C28 0.0633(18) 0.0607(18) 0.0531(17) 0.0100(14) 0.0062(14) 0.0317(15) C29 0.0428(14) 0.0541(15) 0.0526(16) 0.0085(13) 0.0063(12) 0.0273(12) C30 0.0479(15) 0.0570(17) 0.0480(16) 0.0077(12) 0.0024(12) 0.0271(13) C31 0.0308(12) 0.0356(12) 0.0356(12) 0.0096(10) 0.0052(10) 0.0108(10) C32 0.0304(11) 0.0309(11) 0.0335(12) 0.0070(9) 0.0065(9) 0.0106(9) C33 0.0297(11) 0.0309(11) 0.0370(12) 0.0026(9) 0.0077(9) 0.0087(9) C34 0.0386(12) 0.0303(11) 0.0393(13) 0.0043(10) 0.0031(10) 0.0145(10) C35 0.0518(15) 0.0395(13) 0.0620(17) 0.0247(12) 0.0196(13) 0.0167(12) C36 0.0427(14) 0.0569(16) 0.079(2) 0.0370(15) 0.0294(14) 0.0210(13) C37 0.0361(13) 0.0467(14) 0.0604(16) 0.0232(12) 0.0171(11) 0.0215(11) _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 2.1184(16) . ? Mn1 O1 2.1403(15) . ? Mn1 N2 2.2568(18) . ? Mn1 N4 2.2575(19) . ? Mn1 N1 2.2716(18) . ? Mn1 N3 2.3343(18) . ? S1 O5' 1.299(11) . ? S1 O4 1.366(3) . ? S1 O3' 1.415(8) . ? S1 O5 1.456(5) . ? S1 O3 1.466(3) . ? S1 O4' 1.584(13) . ? S1 C34 1.771(2) . ? O1 C31 1.265(3) . ? O2 C31 1.237(3) . ? O6 H6A 0.8200 . ? O6 H6B 0.851(9) . ? O1W H1WA 0.858(10) . ? O1W H1WB 0.861(10) . ? N1 C1 1.324(3) . ? N1 C12 1.354(3) . ? N2 C10 1.324(3) . ? N2 C11 1.349(3) . ? N3 C13 1.326(3) . ? N3 C24 1.357(3) . ? N4 C22 1.326(3) . ? N4 C23 1.350(3) . ? N5 C27 1.329(4) . ? N5 C26 1.330(4) . ? C1 C2 1.386(3) . ? C1 H1 0.9300 . ? C2 C3 1.356(4) . ? C2 H2 0.9300 . ? C3 C4 1.393(4) . ? C3 H3 0.9300 . ? C4 C12 1.396(3) . ? C4 C5 1.429(4) . ? C5 C6 1.343(4) . ? C5 H5 0.9300 . ? C6 C7 1.428(4) . ? C6 H6 0.9300 . ? C7 C8 1.398(4) . ? C7 C11 1.400(3) . ? C8 C9 1.357(4) . ? C8 H8 0.9300 . ? C9 C10 1.387(3) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.439(3) . ? C13 C14 1.386(3) . ? C13 H13 0.9300 . ? C14 C15 1.354(4) . ? C14 H14 0.9300 . ? C15 C16 1.403(3) . ? C15 H15 0.9300 . ? C16 C24 1.397(3) . ? C16 C17 1.427(3) . ? C17 C18 1.333(4) . ? C17 H17 0.9300 . ? C18 C19 1.419(4) . ? C18 H18 0.9300 . ? C19 C20 1.396(3) . ? C19 C23 1.407(3) . ? C20 C21 1.350(4) . ? C20 H20 0.9300 . ? C21 C22 1.388(4) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.438(3) . ? C25 C26 1.372(4) . ? C25 C29 1.387(4) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.372(4) . ? C27 H27 0.9300 . ? C28 C29 1.378(4) . ? C28 H28 0.9300 . ? C29 C30 1.467(4) . ? C30 C30 1.304(5) 2_655 ? C30 H30 0.9300 . ? C31 C32 1.504(3) . ? C32 C37 1.381(3) . ? C32 C33 1.387(3) . ? C33 C34 1.374(3) . ? C33 H33 0.9300 . ? C34 C35 1.381(3) . ? C35 C36 1.377(3) . ? C35 H35 0.9300 . ? C36 C37 1.377(3) . ? C36 H36 0.9300 . ? C37 H37 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 O1 86.12(6) . . ? O6 Mn1 N2 159.83(7) . . ? O1 Mn1 N2 84.62(6) . . ? O6 Mn1 N4 104.47(7) . . ? O1 Mn1 N4 89.73(6) . . ? N2 Mn1 N4 93.37(7) . . ? O6 Mn1 N1 94.27(7) . . ? O1 Mn1 N1 112.90(7) . . ? N2 Mn1 N1 73.06(7) . . ? N4 Mn1 N1 151.67(7) . . ? O6 Mn1 N3 93.01(7) . . ? O1 Mn1 N3 161.04(7) . . ? N2 Mn1 N3 101.48(6) . . ? N4 Mn1 N3 72.13(7) . . ? N1 Mn1 N3 86.05(7) . . ? O5' S1 O4 128.7(5) . . ? O5' S1 O3' 122.7(7) . . ? O4 S1 O3' 66.5(5) . . ? O5' S1 O5 30.7(5) . . ? O4 S1 O5 115.9(3) . . ? O3' S1 O5 150.2(4) . . ? O5' S1 O3 77.3(6) . . ? O4 S1 O3 115.8(2) . . ? O3' S1 O3 52.9(5) . . ? O5 S1 O3 107.6(3) . . ? O5' S1 O4' 103.8(7) . . ? O4 S1 O4' 39.6(5) . . ? O3' S1 O4' 106.0(7) . . ? O5 S1 O4' 80.1(6) . . ? O3 S1 O4' 148.8(5) . . ? O5' S1 C34 114.0(5) . . ? O4 S1 C34 109.67(16) . . ? O3' S1 C34 105.4(3) . . ? O5 S1 C34 101.4(2) . . ? O3 S1 C34 104.96(14) . . ? O4' S1 C34 102.9(5) . . ? C31 O1 Mn1 133.66(14) . . ? Mn1 O6 H6A 109.5 . . ? Mn1 O6 H6B 134.3(15) . . ? H6A O6 H6B 110.6 . . ? H1WA O1W H1WB 104.5(15) . . ? C1 N1 C12 118.0(2) . . ? C1 N1 Mn1 126.68(16) . . ? C12 N1 Mn1 114.90(14) . . ? C10 N2 C11 118.2(2) . . ? C10 N2 Mn1 126.06(16) . . ? C11 N2 Mn1 115.72(14) . . ? C13 N3 C24 117.3(2) . . ? C13 N3 Mn1 128.03(16) . . ? C24 N3 Mn1 114.65(14) . . ? C22 N4 C23 117.7(2) . . ? C22 N4 Mn1 124.90(16) . . ? C23 N4 Mn1 117.28(14) . . ? C27 N5 C26 115.4(3) . . ? N1 C1 C2 123.0(2) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C3 C2 C1 118.8(2) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C2 C3 C4 120.5(2) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C3 C4 C12 117.0(2) . . ? C3 C4 C5 123.8(2) . . ? C12 C4 C5 119.2(2) . . ? C6 C5 C4 121.3(3) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C7 121.0(3) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C8 C7 C11 117.2(2) . . ? C8 C7 C6 123.5(2) . . ? C11 C7 C6 119.3(2) . . ? C9 C8 C7 119.7(2) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 119.4(3) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? N2 C10 C9 122.7(3) . . ? N2 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? N2 C11 C7 122.7(2) . . ? N2 C11 C12 117.69(19) . . ? C7 C11 C12 119.6(2) . . ? N1 C12 C4 122.7(2) . . ? N1 C12 C11 117.66(19) . . ? C4 C12 C11 119.6(2) . . ? N3 C13 C14 123.3(2) . . ? N3 C13 H13 118.3 . . ? C14 C13 H13 118.3 . . ? C15 C14 C13 119.7(2) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 119.2(2) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C24 C16 C15 117.5(2) . . ? C24 C16 C17 119.2(2) . . ? C15 C16 C17 123.2(2) . . ? C18 C17 C16 121.5(2) . . ? C18 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C17 C18 C19 121.2(3) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C20 C19 C23 117.2(2) . . ? C20 C19 C18 123.5(2) . . ? C23 C19 C18 119.3(2) . . ? C21 C20 C19 120.1(2) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 119.1(2) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? N4 C22 C21 123.3(2) . . ? N4 C22 H22 118.4 . . ? C21 C22 H22 118.4 . . ? N4 C23 C19 122.6(2) . . ? N4 C23 C24 118.1(2) . . ? C19 C23 C24 119.4(2) . . ? N3 C24 C16 122.9(2) . . ? N3 C24 C23 117.68(19) . . ? C16 C24 C23 119.4(2) . . ? C26 C25 C29 119.5(3) . . ? C26 C25 H25 120.2 . . ? C29 C25 H25 120.2 . . ? N5 C26 C25 124.5(3) . . ? N5 C26 H26 117.7 . . ? C25 C26 H26 117.7 . . ? N5 C27 C28 124.3(3) . . ? N5 C27 H27 117.9 . . ? C28 C27 H27 117.9 . . ? C27 C28 C29 120.1(3) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C28 C29 C25 116.2(3) . . ? C28 C29 C30 119.8(2) . . ? C25 C29 C30 124.0(3) . . ? C30 C30 C29 126.3(3) 2_655 . ? C30 C30 H30 116.8 2_655 . ? C29 C30 H30 116.8 . . ? O2 C31 O1 124.8(2) . . ? O2 C31 C32 118.67(19) . . ? O1 C31 C32 116.44(19) . . ? C37 C32 C33 119.0(2) . . ? C37 C32 C31 120.17(19) . . ? C33 C32 C31 120.74(19) . . ? C34 C33 C32 120.5(2) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 120.1(2) . . ? C33 C34 S1 120.76(17) . . ? C35 C34 S1 119.16(18) . . ? C36 C35 C34 119.8(2) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C37 120.2(2) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C36 C37 C32 120.5(2) . . ? C36 C37 H37 119.8 . . ? C32 C37 H37 119.8 . . ? 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 O6 Mn1 O1 C31 -8.7(2) . . . . ? N2 Mn1 O1 C31 153.3(2) . . . . ? N4 Mn1 O1 C31 -113.2(2) . . . . ? N1 Mn1 O1 C31 84.3(2) . . . . ? N3 Mn1 O1 C31 -96.7(3) . . . . ? O6 Mn1 N1 C1 -14.73(19) . . . . ? O1 Mn1 N1 C1 -102.32(19) . . . . ? N2 Mn1 N1 C1 -178.7(2) . . . . ? N4 Mn1 N1 C1 117.1(2) . . . . ? N3 Mn1 N1 C1 78.00(19) . . . . ? O6 Mn1 N1 C12 172.61(14) . . . . ? O1 Mn1 N1 C12 85.02(15) . . . . ? N2 Mn1 N1 C12 8.62(14) . . . . ? N4 Mn1 N1 C12 -55.6(2) . . . . ? N3 Mn1 N1 C12 -94.66(15) . . . . ? O6 Mn1 N2 C10 120.6(2) . . . . ? O1 Mn1 N2 C10 57.59(18) . . . . ? N4 Mn1 N2 C10 -31.82(19) . . . . ? N1 Mn1 N2 C10 173.52(19) . . . . ? N3 Mn1 N2 C10 -104.26(18) . . . . ? O6 Mn1 N2 C11 -60.5(3) . . . . ? O1 Mn1 N2 C11 -123.54(15) . . . . ? N4 Mn1 N2 C11 147.06(15) . . . . ? N1 Mn1 N2 C11 -7.60(14) . . . . ? N3 Mn1 N2 C11 74.62(15) . . . . ? O6 Mn1 N3 C13 77.6(2) . . . . ? O1 Mn1 N3 C13 164.47(19) . . . . ? N2 Mn1 N3 C13 -88.3(2) . . . . ? N4 Mn1 N3 C13 -178.1(2) . . . . ? N1 Mn1 N3 C13 -16.4(2) . . . . ? O6 Mn1 N3 C24 -100.95(15) . . . . ? O1 Mn1 N3 C24 -14.1(3) . . . . ? N2 Mn1 N3 C24 93.16(15) . . . . ? N4 Mn1 N3 C24 3.30(14) . . . . ? N1 Mn1 N3 C24 164.97(15) . . . . ? O6 Mn1 N4 C22 -92.34(19) . . . . ? O1 Mn1 N4 C22 -6.41(19) . . . . ? N2 Mn1 N4 C22 78.18(19) . . . . ? N1 Mn1 N4 C22 137.80(19) . . . . ? N3 Mn1 N4 C22 179.2(2) . . . . ? O6 Mn1 N4 C23 84.49(16) . . . . ? O1 Mn1 N4 C23 170.41(15) . . . . ? N2 Mn1 N4 C23 -105.00(15) . . . . ? N1 Mn1 N4 C23 -45.4(2) . . . . ? N3 Mn1 N4 C23 -4.01(14) . . . . ? C12 N1 C1 C2 0.6(3) . . . . ? Mn1 N1 C1 C2 -171.89(17) . . . . ? N1 C1 C2 C3 -1.0(4) . . . . ? C1 C2 C3 C4 0.3(4) . . . . ? C2 C3 C4 C12 0.8(4) . . . . ? C2 C3 C4 C5 -178.0(2) . . . . ? C3 C4 C5 C6 177.4(3) . . . . ? C12 C4 C5 C6 -1.4(4) . . . . ? C4 C5 C6 C7 0.5(4) . . . . ? C5 C6 C7 C8 -176.8(3) . . . . ? C5 C6 C7 C11 1.4(4) . . . . ? C11 C7 C8 C9 -0.4(4) . . . . ? C6 C7 C8 C9 177.8(3) . . . . ? C7 C8 C9 C10 1.7(4) . . . . ? C11 N2 C10 C9 -1.4(3) . . . . ? Mn1 N2 C10 C9 177.46(18) . . . . ? C8 C9 C10 N2 -0.8(4) . . . . ? C10 N2 C11 C7 2.8(3) . . . . ? Mn1 N2 C11 C7 -176.20(16) . . . . ? C10 N2 C11 C12 -175.16(19) . . . . ? Mn1 N2 C11 C12 5.9(2) . . . . ? C8 C7 C11 N2 -1.9(3) . . . . ? C6 C7 C11 N2 179.8(2) . . . . ? C8 C7 C11 C12 176.0(2) . . . . ? C6 C7 C11 C12 -2.3(3) . . . . ? C1 N1 C12 C4 0.6(3) . . . . ? Mn1 N1 C12 C4 173.92(17) . . . . ? C1 N1 C12 C11 177.83(19) . . . . ? Mn1 N1 C12 C11 -8.8(2) . . . . ? C3 C4 C12 N1 -1.2(3) . . . . ? C5 C4 C12 N1 177.6(2) . . . . ? C3 C4 C12 C11 -178.4(2) . . . . ? C5 C4 C12 C11 0.4(3) . . . . ? N2 C11 C12 N1 2.1(3) . . . . ? C7 C11 C12 N1 -175.92(19) . . . . ? N2 C11 C12 C4 179.41(19) . . . . ? C7 C11 C12 C4 1.4(3) . . . . ? C24 N3 C13 C14 0.1(4) . . . . ? Mn1 N3 C13 C14 -178.42(18) . . . . ? N3 C13 C14 C15 -0.1(4) . . . . ? C13 C14 C15 C16 0.7(4) . . . . ? C14 C15 C16 C24 -1.4(4) . . . . ? C14 C15 C16 C17 178.1(2) . . . . ? C24 C16 C17 C18 -1.0(4) . . . . ? C15 C16 C17 C18 179.5(3) . . . . ? C16 C17 C18 C19 -0.8(4) . . . . ? C17 C18 C19 C20 -178.1(3) . . . . ? C17 C18 C19 C23 1.5(4) . . . . ? C23 C19 C20 C21 -0.5(4) . . . . ? C18 C19 C20 C21 179.0(3) . . . . ? C19 C20 C21 C22 1.1(4) . . . . ? C23 N4 C22 C21 -1.0(4) . . . . ? Mn1 N4 C22 C21 175.84(18) . . . . ? C20 C21 C22 N4 -0.4(4) . . . . ? C22 N4 C23 C19 1.6(3) . . . . ? Mn1 N4 C23 C19 -175.50(16) . . . . ? C22 N4 C23 C24 -178.6(2) . . . . ? Mn1 N4 C23 C24 4.3(2) . . . . ? C20 C19 C23 N4 -0.8(3) . . . . ? C18 C19 C23 N4 179.6(2) . . . . ? C20 C19 C23 C24 179.3(2) . . . . ? C18 C19 C23 C24 -0.2(3) . . . . ? C13 N3 C24 C16 -0.9(3) . . . . ? Mn1 N3 C24 C16 177.87(17) . . . . ? C13 N3 C24 C23 178.9(2) . . . . ? Mn1 N3 C24 C23 -2.4(2) . . . . ? C15 C16 C24 N3 1.5(3) . . . . ? C17 C16 C24 N3 -178.0(2) . . . . ? C15 C16 C24 C23 -178.3(2) . . . . ? C17 C16 C24 C23 2.2(3) . . . . ? N4 C23 C24 N3 -1.2(3) . . . . ? C19 C23 C24 N3 178.63(19) . . . . ? N4 C23 C24 C16 178.57(19) . . . . ? C19 C23 C24 C16 -1.6(3) . . . . ? C27 N5 C26 C25 -0.3(4) . . . . ? C29 C25 C26 N5 0.3(4) . . . . ? C26 N5 C27 C28 0.0(5) . . . . ? N5 C27 C28 C29 0.2(5) . . . . ? C27 C28 C29 C25 -0.2(4) . . . . ? C27 C28 C29 C30 179.3(2) . . . . ? C26 C25 C29 C28 -0.1(4) . . . . ? C26 C25 C29 C30 -179.5(2) . . . . ? C28 C29 C30 C30 178.9(3) . . . 2_655 ? C25 C29 C30 C30 -1.7(5) . . . 2_655 ? Mn1 O1 C31 O2 14.0(4) . . . . ? Mn1 O1 C31 C32 -163.20(14) . . . . ? O2 C31 C32 C37 8.4(3) . . . . ? O1 C31 C32 C37 -174.2(2) . . . . ? O2 C31 C32 C33 -168.6(2) . . . . ? O1 C31 C32 C33 8.8(3) . . . . ? C37 C32 C33 C34 -2.2(3) . . . . ? C31 C32 C33 C34 174.8(2) . . . . ? C32 C33 C34 C35 2.2(3) . . . . ? C32 C33 C34 S1 -177.00(16) . . . . ? O5' S1 C34 C33 -88.0(6) . . . . ? O4 S1 C34 C33 119.5(3) . . . . ? O3' S1 C34 C33 49.4(7) . . . . ? O5 S1 C34 C33 -117.5(3) . . . . ? O3 S1 C34 C33 -5.5(3) . . . . ? O4' S1 C34 C33 160.3(7) . . . . ? O5' S1 C34 C35 92.7(7) . . . . ? O4 S1 C34 C35 -59.7(3) . . . . ? O3' S1 C34 C35 -129.8(7) . . . . ? O5 S1 C34 C35 63.3(3) . . . . ? O3 S1 C34 C35 175.2(3) . . . . ? O4' S1 C34 C35 -19.0(7) . . . . ? C33 C34 C35 C36 -0.5(4) . . . . ? S1 C34 C35 C36 178.7(2) . . . . ? C34 C35 C36 C37 -1.2(4) . . . . ? C35 C36 C37 C32 1.2(4) . . . . ? C33 C32 C37 C36 0.5(4) . . . . ? C31 C32 C37 C36 -176.5(2) . . . . ? 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 O6 H6A O2 0.82 1.87 2.647(2) 157.0 . _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.452 _refine_diff_density_min -0.265 _refine_diff_density_rms 0.049 #===END