# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Shi-Ping Yan' _publ_contact_author_email YANSP@NANKAI.EDU.CN _publ_section_title ; Synthesis, structures and magnetic properties of polynuclear mixed-valence MnIIMnIII complexes containing 3-(2-phenol)-5-(pyridin-2-yl) -1, 2, 4-triazole ligand ; loop_ _publ_author_name 'Shi-Ping Yan' 'Peng Cheng' 'Li Feng' 'Wen Gu' 'Ying-Ying Kou' 'Dongdong Li' 'Daizheng Liao' 'Xin Liu' 'Hui Liu' ; J.Ribas ; 'Jin-Lei Tian' 'Jingyan Zhang' # Attachment 'B904553H_ccdc_640936_690531_cif.txt' data_shelxl1 _database_code_depnum_ccdc_archive 'CCDC 640936' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H32 Mn2 N9 O8' _chemical_formula_sum 'C30 H32 Mn2 N9 O8' _chemical_formula_weight 756.53 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' 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 1 21/c 1' 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 14.973(11) _cell_length_b 13.324(13) _cell_length_c 17.853(13) _cell_angle_alpha 90.00 _cell_angle_beta 114.113(8) _cell_angle_gamma 90.00 _cell_volume 3251(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8014 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.0 _exptl_crystal_description prism _exptl_crystal_colour dark-green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas dark-green _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1556 _exptl_absorpt_coefficient_mu 0.842 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8497 _exptl_absorpt_correction_T_max 0.8497 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating anode' _diffrn_radiation_monochromator confacal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18273 _diffrn_reflns_av_R_equivalents 0.1568 _diffrn_reflns_av_sigmaI/netI 0.1567 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5711 _reflns_number_gt 2686 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0744P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5711 _refine_ls_number_parameters 458 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1147 _refine_ls_R_factor_gt 0.0700 _refine_ls_wR_factor_ref 0.1864 _refine_ls_wR_factor_gt 0.1542 _refine_ls_goodness_of_fit_ref 0.837 _refine_ls_restrained_S_all 0.837 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.32434(7) 0.39053(7) 0.21495(5) 0.0402(3) Uani 1 1 d . . . Mn2 Mn 0.12861(7) 0.56511(7) 0.27983(5) 0.0425(3) Uani 1 1 d . . . O1 O 0.3354(3) 0.3492(3) 0.1181(2) 0.0480(11) Uani 1 1 d . . . O2 O 0.4100(3) 0.2845(3) 0.2649(2) 0.0462(11) Uani 1 1 d . . . O3 O 0.2114(3) 0.7127(3) 0.2960(3) 0.0533(12) Uani 1 1 d . . . H3A H 0.1858 0.7694 0.3105 0.064 Uiso 1 1 d R . . O4 O 0.4540(3) 0.4970(3) 0.2447(2) 0.0534(12) Uani 1 1 d . . . H4A H 0.4572 0.5539 0.2759 0.064 Uiso 1 1 d R . . O5 O 0.1953(3) 0.2841(3) 0.1935(3) 0.0563(12) Uani 1 1 d . . . H5A H 0.1360 0.3110 0.1891 0.068 Uiso 1 1 d R . . O6 O 1.0022(4) 0.3430(4) 0.1265(3) 0.0568(12) Uani 1 1 d D . . H6A H 1.005(5) 0.389(4) 0.161(3) 0.068 Uiso 1 1 d D . . H6B H 0.967(4) 0.357(5) 0.0767(14) 0.068 Uiso 1 1 d D . . O7 O 0.5435(4) 0.6463(4) 0.3601(3) 0.0642(14) Uani 1 1 d D . . H7A H 0.567(5) 0.638(5) 0.4115(9) 0.077 Uiso 1 1 d D . . H7B H 0.557(5) 0.706(2) 0.352(4) 0.077 Uiso 1 1 d D . . O8 O -0.1187(4) 0.3857(4) 0.2851(3) 0.0744(16) Uani 1 1 d . . . N1 N 0.0127(4) 0.6549(4) 0.1785(3) 0.0475(14) Uani 1 1 d . . . N2 N 0.1165(4) 0.5733(4) 0.0352(3) 0.0450(13) Uani 1 1 d . . . N3 N 0.2207(3) 0.4905(4) 0.1444(3) 0.0405(12) Uani 1 1 d . . . N4 N 0.1561(3) 0.5389(4) 0.1691(3) 0.0414(13) Uani 1 1 d . . . N5 N 0.1588(4) 0.5752(4) 0.4155(3) 0.0474(14) Uani 1 1 d . . . N6 N 0.3730(3) 0.4164(4) 0.4635(3) 0.0409(12) Uani 1 1 d . . . N7 N 0.3298(3) 0.4248(4) 0.3274(3) 0.0403(12) Uani 1 1 d . . . N8 N 0.2627(3) 0.4782(4) 0.3455(3) 0.0411(12) Uani 1 1 d . . . N9 N 0.0131(4) 0.4640(4) 0.2666(3) 0.0598(16) Uani 1 1 d . . . C1 C -0.0605(5) 0.7065(5) 0.1850(4) 0.0570(19) Uani 1 1 d . . . H1 H -0.0610 0.7123 0.2368 0.068 Uiso 1 1 calc R . . C2 C -0.1358(5) 0.7518(5) 0.1192(4) 0.0523(18) Uani 1 1 d . . . H2 H -0.1855 0.7862 0.1268 0.063 Uiso 1 1 calc R . . C3 C -0.1351(5) 0.7449(5) 0.0433(4) 0.0568(19) Uani 1 1 d . . . H3 H -0.1838 0.7752 -0.0019 0.068 Uiso 1 1 calc R . . C4 C -0.0593(5) 0.6909(5) 0.0350(4) 0.0483(17) Uani 1 1 d . . . H4 H -0.0574 0.6851 -0.0162 0.058 Uiso 1 1 calc R . . C5 C 0.0126(4) 0.6463(4) 0.1029(4) 0.0408(15) Uani 1 1 d . . . C6 C 0.0951(4) 0.5857(4) 0.1007(4) 0.0402(15) Uani 1 1 d . . . C7 C 0.1968(4) 0.5128(4) 0.0659(4) 0.0411(15) Uani 1 1 d . . . C8 C 0.2520(5) 0.4768(5) 0.0196(4) 0.0446(16) Uani 1 1 d . . . C9 C 0.2353(5) 0.5202(5) -0.0570(4) 0.0506(17) Uani 1 1 d . . . H9 H 0.1892 0.5712 -0.0774 0.061 Uiso 1 1 calc R . . C10 C 0.2856(5) 0.4893(5) -0.1024(4) 0.065(2) Uani 1 1 d . . . H10 H 0.2731 0.5178 -0.1533 0.078 Uiso 1 1 calc R . . C11 C 0.3563(5) 0.4135(5) -0.0699(4) 0.063(2) Uani 1 1 d . . . H11 H 0.3923 0.3924 -0.0989 0.075 Uiso 1 1 calc R . . C12 C 0.3726(5) 0.3705(5) 0.0042(4) 0.0565(19) Uani 1 1 d . . . H12 H 0.4202 0.3210 0.0252 0.068 Uiso 1 1 calc R . . C13 C 0.3195(5) 0.3995(4) 0.0488(4) 0.0423(15) Uani 1 1 d . . . C14 C 0.1061(5) 0.6237(5) 0.4504(4) 0.060(2) Uani 1 1 d . . . H14 H 0.0544 0.6640 0.4171 0.071 Uiso 1 1 calc R . . C15 C 0.1246(6) 0.6169(6) 0.5315(4) 0.072(2) Uani 1 1 d . . . H15 H 0.0841 0.6489 0.5520 0.087 Uiso 1 1 calc R . . C16 C 0.2043(5) 0.5620(6) 0.5831(4) 0.070(2) Uani 1 1 d . . . H16 H 0.2191 0.5580 0.6389 0.084 Uiso 1 1 calc R . . C17 C 0.2616(5) 0.5131(5) 0.5502(4) 0.0558(19) Uani 1 1 d . . . H17 H 0.3159 0.4759 0.5835 0.067 Uiso 1 1 calc R . . C18 C 0.2363(4) 0.5208(5) 0.4666(4) 0.0418(15) Uani 1 1 d . . . C19 C 0.2935(4) 0.4704(4) 0.4267(4) 0.0397(15) Uani 1 1 d . . . C20 C 0.3949(4) 0.3893(4) 0.4003(3) 0.0380(14) Uani 1 1 d . . . C21 C 0.4804(4) 0.3292(4) 0.4082(4) 0.0393(15) Uani 1 1 d . . . C22 C 0.5580(4) 0.3192(5) 0.4842(4) 0.0477(16) Uani 1 1 d . . . H22 H 0.5552 0.3503 0.5298 0.057 Uiso 1 1 calc R . . C23 C 0.6384(5) 0.2644(5) 0.4927(4) 0.0513(18) Uani 1 1 d . . . H23 H 0.6893 0.2565 0.5443 0.062 Uiso 1 1 calc R . . C24 C 0.6444(5) 0.2202(5) 0.4244(4) 0.0567(19) Uani 1 1 d . . . H24 H 0.7001 0.1844 0.4299 0.068 Uiso 1 1 calc R . . C25 C 0.5688(4) 0.2292(5) 0.3496(4) 0.0469(16) Uani 1 1 d . . . H25 H 0.5734 0.1995 0.3042 0.056 Uiso 1 1 calc R . . C26 C 0.4844(4) 0.2823(4) 0.3395(4) 0.0423(15) Uani 1 1 d . . . C27 C 0.3007(5) 0.7230(5) 0.2849(5) 0.074(2) Uani 1 1 d . . . H27A H 0.3381 0.6622 0.3016 0.111 Uiso 1 1 calc R . . H27B H 0.3381 0.7779 0.3176 0.111 Uiso 1 1 calc R . . H27C H 0.2858 0.7359 0.2281 0.111 Uiso 1 1 calc R . . C28 C 0.5304(5) 0.4806(6) 0.2181(4) 0.072(2) Uani 1 1 d . . . H28A H 0.5919 0.4759 0.2649 0.108 Uiso 1 1 calc R . . H28B H 0.5325 0.5355 0.1840 0.108 Uiso 1 1 calc R . . H28C H 0.5184 0.4192 0.1873 0.108 Uiso 1 1 calc R . . C29 C 0.2034(5) 0.1794(5) 0.1868(5) 0.076(2) Uani 1 1 d . . . H29A H 0.2580 0.1648 0.1736 0.114 Uiso 1 1 calc R . . H29B H 0.1445 0.1540 0.1443 0.114 Uiso 1 1 calc R . . H29C H 0.2131 0.1482 0.2381 0.114 Uiso 1 1 calc R . . C30 C -0.0524(6) 0.4267(5) 0.2761(4) 0.0539(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0421(6) 0.0504(6) 0.0391(6) 0.0010(4) 0.0278(5) 0.0055(5) Mn2 0.0414(6) 0.0569(7) 0.0405(6) 0.0030(4) 0.0283(5) 0.0053(5) O1 0.062(3) 0.055(3) 0.043(3) -0.001(2) 0.038(2) 0.013(2) O2 0.042(3) 0.051(3) 0.047(3) 0.001(2) 0.021(2) 0.008(2) O3 0.052(3) 0.061(3) 0.062(3) -0.003(2) 0.039(2) -0.002(2) O4 0.056(3) 0.064(3) 0.059(3) -0.008(2) 0.043(2) -0.009(2) O5 0.046(3) 0.055(3) 0.074(3) -0.003(2) 0.031(2) -0.002(2) O6 0.056(3) 0.069(3) 0.048(3) -0.007(3) 0.024(3) 0.005(3) O7 0.068(4) 0.072(3) 0.058(3) 0.003(3) 0.032(3) 0.000(3) O8 0.087(4) 0.080(4) 0.092(4) -0.016(3) 0.074(3) -0.023(3) N1 0.045(3) 0.054(3) 0.056(4) -0.005(3) 0.032(3) -0.003(3) N2 0.044(3) 0.060(3) 0.044(3) 0.005(3) 0.032(3) 0.007(3) N3 0.037(3) 0.050(3) 0.044(3) 0.001(2) 0.026(3) 0.006(2) N4 0.036(3) 0.058(3) 0.039(3) -0.001(2) 0.023(3) 0.008(3) N5 0.050(3) 0.060(4) 0.046(3) 0.001(3) 0.033(3) 0.006(3) N6 0.041(3) 0.056(3) 0.035(3) 0.004(2) 0.025(2) 0.013(3) N7 0.042(3) 0.052(3) 0.042(3) -0.004(2) 0.033(3) 0.002(3) N8 0.040(3) 0.056(3) 0.036(3) 0.002(2) 0.024(2) 0.011(3) N9 0.063(4) 0.067(4) 0.069(4) -0.008(3) 0.047(3) -0.016(3) C1 0.049(4) 0.077(5) 0.061(5) -0.007(4) 0.038(4) 0.004(4) C2 0.043(4) 0.057(4) 0.065(5) -0.005(4) 0.031(4) 0.010(3) C3 0.047(4) 0.068(5) 0.060(5) -0.001(4) 0.026(4) 0.007(4) C4 0.054(4) 0.056(4) 0.046(4) 0.003(3) 0.031(3) 0.005(4) C5 0.046(4) 0.043(4) 0.046(4) -0.002(3) 0.031(3) -0.002(3) C6 0.035(3) 0.055(4) 0.040(4) -0.010(3) 0.024(3) -0.007(3) C7 0.046(4) 0.049(4) 0.039(4) 0.003(3) 0.029(3) -0.006(3) C8 0.050(4) 0.053(4) 0.047(4) -0.004(3) 0.036(3) 0.000(3) C9 0.056(4) 0.053(4) 0.054(4) 0.008(3) 0.033(4) 0.011(3) C10 0.088(6) 0.079(5) 0.051(4) 0.011(4) 0.053(4) 0.006(5) C11 0.085(6) 0.069(5) 0.063(5) 0.005(4) 0.060(4) 0.022(4) C12 0.071(5) 0.066(5) 0.053(4) 0.009(4) 0.046(4) 0.016(4) C13 0.051(4) 0.045(4) 0.040(4) -0.002(3) 0.028(3) 0.002(3) C14 0.054(5) 0.082(5) 0.049(5) 0.004(4) 0.027(4) 0.026(4) C15 0.075(5) 0.108(7) 0.056(5) -0.003(4) 0.050(4) 0.024(5) C16 0.077(6) 0.100(6) 0.049(5) 0.005(4) 0.042(4) 0.028(5) C17 0.058(5) 0.075(5) 0.048(4) 0.004(4) 0.036(4) 0.020(4) C18 0.042(4) 0.052(4) 0.042(4) -0.001(3) 0.028(3) 0.003(3) C19 0.046(4) 0.046(4) 0.038(4) 0.001(3) 0.029(3) -0.001(3) C20 0.036(3) 0.048(4) 0.035(4) 0.004(3) 0.019(3) 0.002(3) C21 0.040(4) 0.040(4) 0.048(4) -0.001(3) 0.029(3) -0.001(3) C22 0.048(4) 0.060(4) 0.044(4) -0.001(3) 0.027(3) 0.002(3) C23 0.037(4) 0.061(5) 0.051(4) -0.004(3) 0.013(3) 0.006(3) C24 0.041(4) 0.069(5) 0.062(5) 0.004(4) 0.023(4) 0.022(4) C25 0.046(4) 0.058(4) 0.048(4) -0.004(3) 0.031(3) 0.005(3) C26 0.041(4) 0.046(4) 0.051(4) 0.006(3) 0.030(3) 0.004(3) C27 0.047(4) 0.077(5) 0.112(7) 0.012(5) 0.046(5) -0.004(4) C28 0.052(5) 0.110(7) 0.073(5) -0.010(5) 0.046(4) -0.006(4) C29 0.074(6) 0.062(5) 0.112(7) 0.000(5) 0.057(5) -0.005(4) C30 0.068(5) 0.058(5) 0.049(4) -0.007(3) 0.038(4) 0.007(4) _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 O2 1.871(4) . ? Mn1 O1 1.885(4) . ? Mn1 N7 2.029(5) . ? Mn1 N3 2.042(5) . ? Mn1 O4 2.285(4) . ? Mn1 O5 2.299(5) . ? Mn2 N9 2.128(6) . ? Mn2 N8 2.196(5) . ? Mn2 N4 2.206(5) . ? Mn2 N1 2.270(5) . ? Mn2 O3 2.279(5) . ? Mn2 N5 2.279(5) . ? O1 C13 1.341(7) . ? O2 C26 1.343(7) . ? O3 C27 1.437(7) . ? O3 H3A 0.9300 . ? O4 C28 1.425(7) . ? O4 H4A 0.9300 . ? O5 C29 1.410(7) . ? O5 H5A 0.9300 . ? O6 H6A 0.850(10) . ? O6 H6B 0.847(10) . ? O7 H7A 0.845(10) . ? O7 H7B 0.848(10) . ? O8 C30 1.201(8) . ? N1 C1 1.337(7) . ? N1 C5 1.354(7) . ? N2 C6 1.343(7) . ? N2 C7 1.362(7) . ? N3 C7 1.330(7) . ? N3 N4 1.377(6) . ? N4 C6 1.343(7) . ? N5 C14 1.352(7) . ? N5 C18 1.356(7) . ? N6 C19 1.314(7) . ? N6 C20 1.346(7) . ? N7 C20 1.352(7) . ? N7 N8 1.373(6) . ? N8 C19 1.334(7) . ? N9 C30 1.172(8) . ? C1 C2 1.391(8) . ? C1 H1 0.9300 . ? C2 C3 1.362(9) . ? C2 H2 0.9300 . ? C3 C4 1.401(8) . ? C3 H3 0.9300 . ? C4 C5 1.384(8) . ? C4 H4 0.9300 . ? C5 C6 1.491(8) . ? C7 C8 1.469(8) . ? C8 C13 1.386(8) . ? C8 C9 1.411(8) . ? C9 C10 1.375(8) . ? C9 H9 0.9300 . ? C10 C11 1.407(9) . ? C10 H10 0.9300 . ? C11 C12 1.369(8) . ? C11 H11 0.9300 . ? C12 C13 1.390(8) . ? C12 H12 0.9300 . ? C14 C15 1.362(9) . ? C14 H14 0.9300 . ? C15 C16 1.381(9) . ? C15 H15 0.9300 . ? C16 C17 1.385(8) . ? C16 H16 0.9300 . ? C17 C18 1.386(8) . ? C17 H17 0.9300 . ? C18 C19 1.480(8) . ? C20 C21 1.466(8) . ? C21 C22 1.386(8) . ? C21 C26 1.401(8) . ? C22 C23 1.363(8) . ? C22 H22 0.9300 . ? C23 C24 1.390(8) . ? C23 H23 0.9300 . ? C24 C25 1.358(8) . ? C24 H24 0.9300 . ? C25 C26 1.394(8) . ? C25 H25 0.9300 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mn1 O1 85.19(18) . . ? O2 Mn1 N7 87.47(19) . . ? O1 Mn1 N7 172.18(19) . . ? O2 Mn1 N3 170.51(19) . . ? O1 Mn1 N3 87.37(19) . . ? N7 Mn1 N3 100.2(2) . . ? O2 Mn1 O4 90.35(18) . . ? O1 Mn1 O4 90.60(17) . . ? N7 Mn1 O4 86.74(17) . . ? N3 Mn1 O4 95.62(19) . . ? O2 Mn1 O5 88.82(18) . . ? O1 Mn1 O5 92.86(17) . . ? N7 Mn1 O5 89.69(18) . . ? N3 Mn1 O5 85.67(19) . . ? O4 Mn1 O5 176.36(15) . . ? N9 Mn2 N8 104.4(2) . . ? N9 Mn2 N4 104.0(2) . . ? N8 Mn2 N4 86.02(19) . . ? N9 Mn2 N1 85.6(2) . . ? N8 Mn2 N1 159.75(18) . . ? N4 Mn2 N1 74.39(19) . . ? N9 Mn2 O3 159.33(19) . . ? N8 Mn2 O3 93.23(18) . . ? N4 Mn2 O3 87.64(17) . . ? N1 Mn2 O3 81.09(17) . . ? N9 Mn2 N5 87.4(2) . . ? N8 Mn2 N5 73.89(18) . . ? N4 Mn2 N5 158.96(19) . . ? N1 Mn2 N5 124.82(19) . . ? O3 Mn2 N5 87.34(17) . . ? C13 O1 Mn1 130.6(4) . . ? C26 O2 Mn1 128.2(4) . . ? C27 O3 Mn2 123.7(4) . . ? C27 O3 H3A 118.2 . . ? Mn2 O3 H3A 118.2 . . ? C28 O4 Mn1 123.3(4) . . ? C28 O4 H4A 118.3 . . ? Mn1 O4 H4A 118.4 . . ? C29 O5 Mn1 122.0(4) . . ? C29 O5 H5A 119.0 . . ? Mn1 O5 H5A 119.0 . . ? H6A O6 H6B 115(7) . . ? H7A O7 H7B 107(7) . . ? C1 N1 C5 117.6(6) . . ? C1 N1 Mn2 126.0(5) . . ? C5 N1 Mn2 116.0(4) . . ? C6 N2 C7 101.9(5) . . ? C7 N3 N4 108.0(5) . . ? C7 N3 Mn1 127.3(4) . . ? N4 N3 Mn1 124.4(4) . . ? C6 N4 N3 103.4(5) . . ? C6 N4 Mn2 115.8(4) . . ? N3 N4 Mn2 140.7(4) . . ? C14 N5 C18 116.5(5) . . ? C14 N5 Mn2 128.1(4) . . ? C18 N5 Mn2 115.3(4) . . ? C19 N6 C20 102.1(5) . . ? C20 N7 N8 105.4(4) . . ? C20 N7 Mn1 126.5(4) . . ? N8 N7 Mn1 127.7(4) . . ? C19 N8 N7 104.7(5) . . ? C19 N8 Mn2 117.2(4) . . ? N7 N8 Mn2 138.2(4) . . ? C30 N9 Mn2 160.5(6) . . ? N1 C1 C2 124.0(6) . . ? N1 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? C3 C2 C1 118.6(6) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 118.4(6) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C5 C4 C3 120.1(6) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? N1 C5 C4 121.4(6) . . ? N1 C5 C6 114.1(5) . . ? C4 C5 C6 124.5(6) . . ? N4 C6 N2 114.8(5) . . ? N4 C6 C5 119.4(5) . . ? N2 C6 C5 125.8(6) . . ? N3 C7 N2 111.8(5) . . ? N3 C7 C8 123.2(6) . . ? N2 C7 C8 125.0(5) . . ? C13 C8 C9 118.9(6) . . ? C13 C8 C7 121.5(6) . . ? C9 C8 C7 119.6(6) . . ? C10 C9 C8 121.7(6) . . ? C10 C9 H9 119.1 . . ? C8 C9 H9 119.1 . . ? C9 C10 C11 118.3(6) . . ? C9 C10 H10 120.9 . . ? C11 C10 H10 120.9 . . ? C12 C11 C10 120.4(6) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 121.3(6) . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? O1 C13 C8 123.1(5) . . ? O1 C13 C12 117.5(6) . . ? C8 C13 C12 119.4(6) . . ? N5 C14 C15 123.7(6) . . ? N5 C14 H14 118.2 . . ? C15 C14 H14 118.2 . . ? C14 C15 C16 119.3(6) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C15 C16 C17 118.9(7) . . ? C15 C16 H16 120.6 . . ? C17 C16 H16 120.6 . . ? C16 C17 C18 118.5(6) . . ? C16 C17 H17 120.7 . . ? C18 C17 H17 120.7 . . ? N5 C18 C17 123.1(6) . . ? N5 C18 C19 115.1(5) . . ? C17 C18 C19 121.8(6) . . ? N6 C19 N8 115.2(5) . . ? N6 C19 C18 126.4(5) . . ? N8 C19 C18 118.4(5) . . ? N6 C20 N7 112.7(5) . . ? N6 C20 C21 124.5(5) . . ? N7 C20 C21 122.8(5) . . ? C22 C21 C26 119.7(6) . . ? C22 C21 C20 119.9(5) . . ? C26 C21 C20 120.5(5) . . ? C23 C22 C21 120.7(6) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C22 C23 C24 120.0(6) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C25 C24 C23 119.9(6) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C26 121.4(6) . . ? C24 C25 H25 119.3 . . ? C26 C25 H25 119.3 . . ? O2 C26 C25 118.7(6) . . ? O2 C26 C21 123.0(5) . . ? C25 C26 C21 118.3(6) . . ? O3 C27 H27A 109.5 . . ? O3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O4 C28 H28A 109.5 . . ? O4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O5 C29 H29A 109.5 . . ? O5 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O5 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N9 C30 O8 178.0(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 O2 Mn1 O1 C13 -157.9(5) . . . . ? N7 Mn1 O1 C13 -137.6(13) . . . . ? N3 Mn1 O1 C13 28.0(5) . . . . ? O4 Mn1 O1 C13 -67.6(5) . . . . ? O5 Mn1 O1 C13 113.5(5) . . . . ? O1 Mn1 O2 C26 140.8(5) . . . . ? N7 Mn1 O2 C26 -36.5(5) . . . . ? N3 Mn1 O2 C26 179(95) . . . . ? O4 Mn1 O2 C26 50.2(5) . . . . ? O5 Mn1 O2 C26 -126.2(5) . . . . ? N9 Mn2 O3 C27 -167.9(6) . . . . ? N8 Mn2 O3 C27 43.1(5) . . . . ? N4 Mn2 O3 C27 -42.8(5) . . . . ? N1 Mn2 O3 C27 -117.4(5) . . . . ? N5 Mn2 O3 C27 116.8(5) . . . . ? O2 Mn1 O4 C28 57.6(5) . . . . ? O1 Mn1 O4 C28 -27.6(5) . . . . ? N7 Mn1 O4 C28 145.0(5) . . . . ? N3 Mn1 O4 C28 -115.0(5) . . . . ? O5 Mn1 O4 C28 134(2) . . . . ? O2 Mn1 O5 C29 -26.1(5) . . . . ? O1 Mn1 O5 C29 59.0(5) . . . . ? N7 Mn1 O5 C29 -113.6(5) . . . . ? N3 Mn1 O5 C29 146.2(5) . . . . ? O4 Mn1 O5 C29 -103(2) . . . . ? N9 Mn2 N1 C1 69.9(5) . . . . ? N8 Mn2 N1 C1 -169.2(5) . . . . ? N4 Mn2 N1 C1 175.7(5) . . . . ? O3 Mn2 N1 C1 -94.3(5) . . . . ? N5 Mn2 N1 C1 -13.8(6) . . . . ? N9 Mn2 N1 C5 -102.9(4) . . . . ? N8 Mn2 N1 C5 18.1(8) . . . . ? N4 Mn2 N1 C5 2.9(4) . . . . ? O3 Mn2 N1 C5 93.0(4) . . . . ? N5 Mn2 N1 C5 173.4(4) . . . . ? O2 Mn1 N3 C7 -47.1(14) . . . . ? O1 Mn1 N3 C7 -8.7(5) . . . . ? N7 Mn1 N3 C7 169.3(5) . . . . ? O4 Mn1 N3 C7 81.6(5) . . . . ? O5 Mn1 N3 C7 -101.8(5) . . . . ? O2 Mn1 N3 N4 125.7(11) . . . . ? O1 Mn1 N3 N4 164.1(4) . . . . ? N7 Mn1 N3 N4 -17.9(5) . . . . ? O4 Mn1 N3 N4 -105.6(4) . . . . ? O5 Mn1 N3 N4 71.0(4) . . . . ? C7 N3 N4 C6 1.6(6) . . . . ? Mn1 N3 N4 C6 -172.4(4) . . . . ? C7 N3 N4 Mn2 -175.4(5) . . . . ? Mn1 N3 N4 Mn2 10.6(8) . . . . ? N9 Mn2 N4 C6 81.4(4) . . . . ? N8 Mn2 N4 C6 -174.7(4) . . . . ? N1 Mn2 N4 C6 0.1(4) . . . . ? O3 Mn2 N4 C6 -81.3(4) . . . . ? N5 Mn2 N4 C6 -157.6(5) . . . . ? N9 Mn2 N4 N3 -101.9(6) . . . . ? N8 Mn2 N4 N3 2.0(6) . . . . ? N1 Mn2 N4 N3 176.8(6) . . . . ? O3 Mn2 N4 N3 95.4(6) . . . . ? N5 Mn2 N4 N3 19.1(10) . . . . ? N9 Mn2 N5 C14 -73.9(6) . . . . ? N8 Mn2 N5 C14 -179.7(6) . . . . ? N4 Mn2 N5 C14 162.5(6) . . . . ? N1 Mn2 N5 C14 8.9(6) . . . . ? O3 Mn2 N5 C14 86.1(6) . . . . ? N9 Mn2 N5 C18 102.1(5) . . . . ? N8 Mn2 N5 C18 -3.7(4) . . . . ? N4 Mn2 N5 C18 -21.5(8) . . . . ? N1 Mn2 N5 C18 -175.1(4) . . . . ? O3 Mn2 N5 C18 -97.9(4) . . . . ? O2 Mn1 N7 C20 13.7(5) . . . . ? O1 Mn1 N7 C20 -6.6(17) . . . . ? N3 Mn1 N7 C20 -172.0(5) . . . . ? O4 Mn1 N7 C20 -76.8(5) . . . . ? O5 Mn1 N7 C20 102.5(5) . . . . ? O2 Mn1 N7 N8 -157.8(5) . . . . ? O1 Mn1 N7 N8 -178.0(12) . . . . ? N3 Mn1 N7 N8 16.6(5) . . . . ? O4 Mn1 N7 N8 111.7(5) . . . . ? O5 Mn1 N7 N8 -69.0(5) . . . . ? C20 N7 N8 C19 0.3(6) . . . . ? Mn1 N7 N8 C19 173.2(4) . . . . ? C20 N7 N8 Mn2 -179.4(4) . . . . ? Mn1 N7 N8 Mn2 -6.5(8) . . . . ? N9 Mn2 N8 C19 -80.8(5) . . . . ? N4 Mn2 N8 C19 175.8(4) . . . . ? N1 Mn2 N8 C19 161.2(5) . . . . ? O3 Mn2 N8 C19 88.4(4) . . . . ? N5 Mn2 N8 C19 2.1(4) . . . . ? N9 Mn2 N8 N7 98.9(6) . . . . ? N4 Mn2 N8 N7 -4.5(6) . . . . ? N1 Mn2 N8 N7 -19.1(9) . . . . ? O3 Mn2 N8 N7 -92.0(6) . . . . ? N5 Mn2 N8 N7 -178.2(6) . . . . ? N8 Mn2 N9 C30 108.2(18) . . . . ? N4 Mn2 N9 C30 -162.4(18) . . . . ? N1 Mn2 N9 C30 -89.7(18) . . . . ? O3 Mn2 N9 C30 -40(2) . . . . ? N5 Mn2 N9 C30 35.6(18) . . . . ? C5 N1 C1 C2 -0.3(9) . . . . ? Mn2 N1 C1 C2 -173.0(5) . . . . ? N1 C1 C2 C3 -0.8(10) . . . . ? C1 C2 C3 C4 1.0(10) . . . . ? C2 C3 C4 C5 0.0(10) . . . . ? C1 N1 C5 C4 1.3(9) . . . . ? Mn2 N1 C5 C4 174.7(4) . . . . ? C1 N1 C5 C6 -178.6(5) . . . . ? Mn2 N1 C5 C6 -5.2(6) . . . . ? C3 C4 C5 N1 -1.2(9) . . . . ? C3 C4 C5 C6 178.7(6) . . . . ? N3 N4 C6 N2 -1.4(7) . . . . ? Mn2 N4 C6 N2 176.5(4) . . . . ? N3 N4 C6 C5 179.2(5) . . . . ? Mn2 N4 C6 C5 -2.9(7) . . . . ? C7 N2 C6 N4 0.6(7) . . . . ? C7 N2 C6 C5 180.0(6) . . . . ? N1 C5 C6 N4 5.5(8) . . . . ? C4 C5 C6 N4 -174.4(6) . . . . ? N1 C5 C6 N2 -173.8(5) . . . . ? C4 C5 C6 N2 6.3(10) . . . . ? N4 N3 C7 N2 -1.4(7) . . . . ? Mn1 N3 C7 N2 172.4(4) . . . . ? N4 N3 C7 C8 178.0(5) . . . . ? Mn1 N3 C7 C8 -8.3(8) . . . . ? C6 N2 C7 N3 0.5(7) . . . . ? C6 N2 C7 C8 -178.9(6) . . . . ? N3 C7 C8 C13 14.5(10) . . . . ? N2 C7 C8 C13 -166.2(6) . . . . ? N3 C7 C8 C9 -166.5(6) . . . . ? N2 C7 C8 C9 12.7(10) . . . . ? C13 C8 C9 C10 -1.3(10) . . . . ? C7 C8 C9 C10 179.7(6) . . . . ? C8 C9 C10 C11 -1.1(11) . . . . ? C9 C10 C11 C12 1.5(11) . . . . ? C10 C11 C12 C13 0.7(11) . . . . ? Mn1 O1 C13 C8 -29.9(9) . . . . ? Mn1 O1 C13 C12 151.3(5) . . . . ? C9 C8 C13 O1 -175.4(6) . . . . ? C7 C8 C13 O1 3.6(10) . . . . ? C9 C8 C13 C12 3.4(10) . . . . ? C7 C8 C13 C12 -177.6(6) . . . . ? C11 C12 C13 O1 175.7(6) . . . . ? C11 C12 C13 C8 -3.1(10) . . . . ? C18 N5 C14 C15 -2.9(11) . . . . ? Mn2 N5 C14 C15 173.1(6) . . . . ? N5 C14 C15 C16 3.5(12) . . . . ? C14 C15 C16 C17 -1.7(12) . . . . ? C15 C16 C17 C18 -0.3(11) . . . . ? C14 N5 C18 C17 0.7(9) . . . . ? Mn2 N5 C18 C17 -175.8(5) . . . . ? C14 N5 C18 C19 -178.8(6) . . . . ? Mn2 N5 C18 C19 4.7(7) . . . . ? C16 C17 C18 N5 0.9(10) . . . . ? C16 C17 C18 C19 -179.7(6) . . . . ? C20 N6 C19 N8 1.0(7) . . . . ? C20 N6 C19 C18 -179.8(6) . . . . ? N7 N8 C19 N6 -0.8(7) . . . . ? Mn2 N8 C19 N6 178.9(4) . . . . ? N7 N8 C19 C18 179.8(5) . . . . ? Mn2 N8 C19 C18 -0.4(7) . . . . ? N5 C18 C19 N6 177.8(6) . . . . ? C17 C18 C19 N6 -1.7(10) . . . . ? N5 C18 C19 N8 -3.0(8) . . . . ? C17 C18 C19 N8 177.5(6) . . . . ? C19 N6 C20 N7 -0.7(7) . . . . ? C19 N6 C20 C21 178.3(6) . . . . ? N8 N7 C20 N6 0.3(7) . . . . ? Mn1 N7 C20 N6 -172.7(4) . . . . ? N8 N7 C20 C21 -178.8(5) . . . . ? Mn1 N7 C20 C21 8.2(8) . . . . ? N6 C20 C21 C22 -17.3(9) . . . . ? N7 C20 C21 C22 161.6(6) . . . . ? N6 C20 C21 C26 163.1(6) . . . . ? N7 C20 C21 C26 -18.0(9) . . . . ? C26 C21 C22 C23 0.1(10) . . . . ? C20 C21 C22 C23 -179.5(6) . . . . ? C21 C22 C23 C24 1.9(10) . . . . ? C22 C23 C24 C25 -1.9(11) . . . . ? C23 C24 C25 C26 0.0(10) . . . . ? Mn1 O2 C26 C25 -143.8(5) . . . . ? Mn1 O2 C26 C21 37.6(8) . . . . ? C24 C25 C26 O2 -176.6(6) . . . . ? C24 C25 C26 C21 2.0(10) . . . . ? C22 C21 C26 O2 176.6(6) . . . . ? C20 C21 C26 O2 -3.8(9) . . . . ? C22 C21 C26 C25 -2.1(9) . . . . ? C20 C21 C26 C25 177.6(5) . . . . ? Mn2 N9 C30 O8 -154(23) . . . . ? 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 O3 H3A O8 0.93 2.22 2.773(7) 117.5 2 O4 H4A O7 0.93 1.96 2.782(7) 145.6 . O5 H5A O6 0.93 1.90 2.754(7) 151.1 1_455 O6 H6B N2 0.847(10) 2.09(2) 2.922(7) 166(6) 3_665 O7 H7A N6 0.845(10) 2.161(18) 2.994(7) 168(6) 3_666 O7 H7B O1 0.848(10) 2.41(3) 3.189(7) 153(6) 2_655 O7 H7B O2 0.848(10) 2.55(5) 3.182(7) 132(6) 2_655 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.484 _refine_diff_density_min -0.660 _refine_diff_density_rms 0.100 # Attachment '6.cif' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 671748' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C67 H64 Mn4 N16 O15' _chemical_formula_weight 1553.10 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' 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 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.277(5) _cell_length_b 14.737(8) _cell_length_c 24.826(13) _cell_angle_alpha 90.00 _cell_angle_beta 99.370(6) _cell_angle_gamma 90.00 _cell_volume 3710(3) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 6951 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 27.9 _exptl_crystal_description prism _exptl_crystal_colour dark-green _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1596 _exptl_absorpt_coefficient_mu 0.738 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8898 _exptl_absorpt_correction_T_max 0.9026 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26469 _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_sigmaI/netI 0.0541 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6416 _reflns_number_gt 5750 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0542P)^2^+8.1722P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6416 _refine_ls_number_parameters 474 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.1469 _refine_ls_wR_factor_gt 0.1412 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.115 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.34697(6) 0.91888(4) 0.19647(2) 0.01716(17) Uani 1 1 d . . . Mn2 Mn 0.14878(6) 0.97816(4) 0.32914(2) 0.01959(18) Uani 1 1 d . . . N1 N 0.0760(3) 0.7269(2) 0.24890(12) 0.0199(7) Uani 1 1 d . . . N2 N 0.1337(3) 0.8648(2) 0.28223(12) 0.0171(7) Uani 1 1 d . . . N3 N 0.2055(3) 0.8472(2) 0.24146(12) 0.0182(7) Uani 1 1 d . . . N4 N 0.3229(3) 0.7734(2) 0.16239(12) 0.0197(7) Uani 1 1 d . . . N5 N 0.3831(3) 1.1817(2) 0.27465(12) 0.0193(7) Uani 1 1 d . . . N6 N 0.2752(3) 1.0578(2) 0.29604(12) 0.0183(7) Uani 1 1 d . . . N7 N 0.3472(3) 1.0334(2) 0.25668(12) 0.0177(7) Uani 1 1 d . . . N8 N 0.4909(3) 1.0284(2) 0.17511(13) 0.0198(7) Uani 1 1 d . . . O1 O 0.0250(3) 0.92649(19) 0.36660(12) 0.0355(8) Uani 1 1 d . . . O2 O 0.1524(4) 1.06893(19) 0.38272(12) 0.0390(8) Uani 1 1 d . . . O3 O 0.1898(3) 0.9667(2) 0.13674(11) 0.0315(7) Uani 1 1 d . . . O4 O 0.3197(3) 0.9251(2) 0.07809(13) 0.0350(7) Uani 1 1 d . . . O5 O 0.3208(4) 0.9077(2) 0.38184(13) 0.0406(8) Uani 1 1 d . . . H5 H 0.3106 0.8452 0.3896 0.049 Uiso 1 1 calc R . . O6 O -0.0030(3) 1.04562(19) 0.26529(12) 0.0298(7) Uani 1 1 d . . . H6 H -0.0199 1.1082 0.2700 0.036 Uiso 1 1 calc R . . O7 O 0.5325(3) 0.85599(18) 0.23941(11) 0.0223(6) Uani 1 1 d . . . H7 H 0.5530 0.7974 0.2272 0.027 Uiso 1 1 calc R . . C1 C -0.0447(4) 0.8490(3) 0.36397(16) 0.0221(9) Uani 1 1 d . . . C2 C -0.1280(4) 0.8368(3) 0.40222(16) 0.0276(9) Uani 1 1 d . . . H2 H -0.1354 0.8832 0.4281 0.033 Uiso 1 1 calc R . . C3 C -0.1997(4) 0.7583(3) 0.40300(17) 0.0287(10) Uani 1 1 d . . . H3 H -0.2554 0.7502 0.4297 0.034 Uiso 1 1 calc R . . C4 C -0.1908(4) 0.6909(3) 0.36475(16) 0.0254(9) Uani 1 1 d . . . H4 H -0.2411 0.6369 0.3649 0.030 Uiso 1 1 calc R . . C5 C -0.1094(4) 0.7023(3) 0.32677(16) 0.0234(9) Uani 1 1 d . . . H5A H -0.1044 0.6557 0.3007 0.028 Uiso 1 1 calc R . . C6 C -0.0333(4) 0.7810(2) 0.32532(15) 0.0188(8) Uani 1 1 d . . . C7 C 0.0558(4) 0.7912(2) 0.28567(15) 0.0168(8) Uani 1 1 d . . . C8 C 0.1670(4) 0.7648(3) 0.22285(15) 0.0193(8) Uani 1 1 d . . . C9 C 0.2291(4) 0.7229(3) 0.17952(15) 0.0207(8) Uani 1 1 d . . . C10 C 0.1964(5) 0.6368(3) 0.15827(18) 0.0316(10) Uani 1 1 d . . . H10 H 0.1292 0.6023 0.1709 0.038 Uiso 1 1 calc R . . C11 C 0.2623(5) 0.6024(3) 0.11900(19) 0.0390(12) Uani 1 1 d . . . H11 H 0.2406 0.5442 0.1037 0.047 Uiso 1 1 calc R . . C12 C 0.3612(5) 0.6537(3) 0.10186(17) 0.0302(10) Uani 1 1 d . . . H12 H 0.4095 0.6310 0.0752 0.036 Uiso 1 1 calc R . . C13 C 0.3875(4) 0.7383(3) 0.12449(16) 0.0238(9) Uani 1 1 d . . . H13 H 0.4547 0.7737 0.1126 0.029 Uiso 1 1 calc R . . C14 C 0.1665(4) 1.1587(3) 0.38114(16) 0.0251(9) Uani 1 1 d . . . C15 C 0.1110(5) 1.2110(3) 0.41897(19) 0.0342(11) Uani 1 1 d . . . H15 H 0.0648 1.1818 0.4443 0.041 Uiso 1 1 calc R . . C16 C 0.1228(5) 1.3033(3) 0.4197(2) 0.0375(11) Uani 1 1 d . . . H16 H 0.0852 1.3380 0.4455 0.045 Uiso 1 1 calc R . . C17 C 0.1897(5) 1.3466(3) 0.3826(2) 0.0398(12) Uani 1 1 d . . . H17 H 0.1956 1.4109 0.3823 0.048 Uiso 1 1 calc R . . C18 C 0.2477(4) 1.2960(3) 0.34616(18) 0.0303(10) Uani 1 1 d . . . H18 H 0.2957 1.3259 0.3217 0.036 Uiso 1 1 calc R . . C19 C 0.2369(4) 1.2011(3) 0.34471(16) 0.0215(8) Uani 1 1 d . . . C20 C 0.2983(4) 1.1477(2) 0.30585(15) 0.0180(8) Uani 1 1 d . . . C21 C 0.4092(4) 1.1083(2) 0.24507(14) 0.0176(8) Uani 1 1 d . . . C22 C 0.4942(4) 1.1072(2) 0.20330(14) 0.0174(8) Uani 1 1 d . . . C23 C 0.5708(4) 1.1811(3) 0.19209(16) 0.0228(9) Uani 1 1 d . . . H23 H 0.5707 1.2360 0.2122 0.027 Uiso 1 1 calc R . . C24 C 0.6461(4) 1.1730(3) 0.15150(16) 0.0265(9) Uani 1 1 d . . . H24 H 0.6986 1.2223 0.1430 0.032 Uiso 1 1 calc R . . C25 C 0.6445(4) 1.0921(3) 0.12317(16) 0.0252(9) Uani 1 1 d . . . H25 H 0.6965 1.0847 0.0951 0.030 Uiso 1 1 calc R . . C26 C 0.5656(4) 1.0220(3) 0.13645(16) 0.0250(9) Uani 1 1 d . . . H26 H 0.5651 0.9665 0.1169 0.030 Uiso 1 1 calc R . . C27 C 0.2146(5) 0.9554(3) 0.08856(17) 0.0296(10) Uani 1 1 d . . . C28 C 0.1034(4) 0.9800(3) 0.04261(16) 0.0256(9) Uani 1 1 d . . . C29 C -0.0082(5) 1.0248(3) 0.05309(17) 0.0314(10) Uani 1 1 d . . . H29 H -0.0149 1.0421 0.0894 0.038 Uiso 1 1 calc R . . C30 C 0.1111(5) 0.9555(3) -0.01061(17) 0.0302(10) Uani 1 1 d . . . H30 H 0.1873 0.9249 -0.0183 0.036 Uiso 1 1 calc R . . C31 C 0.4400(10) 0.9485(9) 0.4037(5) 0.154(5) Uani 1 1 d . . . H31A H 0.4664 0.9908 0.3770 0.231 Uiso 1 1 calc R . . H31B H 0.5080 0.9018 0.4126 0.231 Uiso 1 1 calc R . . H31C H 0.4295 0.9817 0.4370 0.231 Uiso 1 1 calc R . . C32 C -0.0744(6) 1.0023(4) 0.2190(2) 0.0560(16) Uani 1 1 d . . . H32A H -0.0148 0.9880 0.1931 0.084 Uiso 1 1 calc R . . H32B H -0.1446 1.0426 0.2015 0.084 Uiso 1 1 calc R . . H32C H -0.1133 0.9460 0.2302 0.084 Uiso 1 1 calc R . . C33 C 0.6240(5) 0.8935(3) 0.2831(2) 0.0445(13) Uani 1 1 d . . . H33A H 0.6279 0.9594 0.2787 0.067 Uiso 1 1 calc R . . H33B H 0.7115 0.8674 0.2827 0.067 Uiso 1 1 calc R . . H33C H 0.5954 0.8793 0.3179 0.067 Uiso 1 1 calc R . . C34 C 0.5480(12) 0.8614(12) -0.0011(5) 0.088(4) Uani 0.50 1 d PDU . . H34A H 0.5538 0.9277 0.0007 0.132 Uiso 0.50 1 calc PR . . H34B H 0.5737 0.8403 -0.0353 0.132 Uiso 0.50 1 calc PR . . H34C H 0.6073 0.8350 0.0298 0.132 Uiso 0.50 1 calc PR . . O8 O 0.4160(9) 0.8338(6) 0.0009(3) 0.067(2) Uani 0.50 1 d PDU . . H8 H 0.3760 0.8759 0.0142 0.100 Uiso 0.50 1 calc PR . . 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 0.0202(3) 0.0134(3) 0.0181(3) -0.0002(2) 0.0038(2) -0.0006(2) Mn2 0.0277(4) 0.0127(3) 0.0199(3) -0.0012(2) 0.0086(3) -0.0026(2) N1 0.0230(19) 0.0160(16) 0.0208(16) -0.0004(13) 0.0032(14) -0.0006(14) N2 0.0202(18) 0.0128(15) 0.0185(15) 0.0015(12) 0.0041(13) -0.0002(13) N3 0.0199(18) 0.0149(16) 0.0202(15) -0.0008(12) 0.0049(13) -0.0007(13) N4 0.0204(18) 0.0198(17) 0.0187(15) -0.0007(13) 0.0023(13) 0.0018(14) N5 0.0177(18) 0.0173(16) 0.0235(16) -0.0019(13) 0.0047(13) -0.0023(13) N6 0.0242(19) 0.0154(16) 0.0154(15) 0.0001(12) 0.0038(13) 0.0006(13) N7 0.0207(18) 0.0152(16) 0.0171(15) 0.0001(12) 0.0026(13) -0.0011(13) N8 0.0196(18) 0.0149(16) 0.0246(16) 0.0013(13) 0.0025(14) 0.0006(13) O1 0.058(2) 0.0219(16) 0.0329(16) -0.0081(12) 0.0258(15) -0.0131(15) O2 0.072(2) 0.0201(16) 0.0317(16) -0.0077(12) 0.0295(16) -0.0139(15) O3 0.0395(19) 0.0285(16) 0.0234(15) 0.0051(12) -0.0037(13) 0.0001(14) O4 0.0286(19) 0.0347(18) 0.0389(17) 0.0020(14) -0.0030(14) 0.0022(14) O5 0.048(2) 0.0337(18) 0.0352(17) 0.0046(14) -0.0071(15) 0.0017(15) O6 0.0299(17) 0.0194(15) 0.0391(17) 0.0004(12) 0.0026(13) 0.0060(13) O7 0.0213(16) 0.0155(13) 0.0285(14) -0.0016(11) -0.0009(11) 0.0012(11) C1 0.026(2) 0.0145(19) 0.026(2) 0.0022(15) 0.0058(17) -0.0028(16) C2 0.036(3) 0.024(2) 0.024(2) 0.0000(16) 0.0100(18) -0.0028(19) C3 0.032(3) 0.029(2) 0.027(2) 0.0041(17) 0.0102(19) -0.0039(19) C4 0.023(2) 0.025(2) 0.027(2) 0.0022(17) 0.0012(17) -0.0092(17) C5 0.024(2) 0.019(2) 0.027(2) -0.0030(16) 0.0029(17) -0.0029(16) C6 0.019(2) 0.0158(19) 0.0214(18) 0.0014(15) 0.0010(15) 0.0011(15) C7 0.016(2) 0.0116(18) 0.0223(18) 0.0027(14) 0.0001(15) 0.0027(15) C8 0.019(2) 0.0174(19) 0.0209(19) -0.0018(15) 0.0014(16) 0.0003(15) C9 0.022(2) 0.0164(19) 0.0228(19) 0.0010(15) 0.0014(16) 0.0000(16) C10 0.037(3) 0.023(2) 0.037(2) -0.0119(18) 0.013(2) -0.0078(19) C11 0.051(3) 0.026(2) 0.043(3) -0.016(2) 0.017(2) -0.008(2) C12 0.038(3) 0.026(2) 0.029(2) -0.0087(18) 0.0108(19) 0.0015(19) C13 0.023(2) 0.024(2) 0.026(2) 0.0000(16) 0.0079(17) 0.0018(17) C14 0.034(3) 0.016(2) 0.025(2) -0.0013(16) 0.0073(18) -0.0041(17) C15 0.042(3) 0.026(2) 0.040(2) -0.0049(19) 0.021(2) -0.007(2) C16 0.042(3) 0.024(2) 0.052(3) -0.008(2) 0.023(2) -0.001(2) C17 0.053(3) 0.014(2) 0.061(3) -0.002(2) 0.032(3) 0.000(2) C18 0.034(3) 0.019(2) 0.043(2) 0.0004(18) 0.021(2) 0.0018(18) C19 0.020(2) 0.0170(19) 0.027(2) -0.0035(16) 0.0048(16) -0.0019(16) C20 0.019(2) 0.0145(18) 0.0198(18) 0.0008(14) 0.0008(15) -0.0022(15) C21 0.019(2) 0.0148(18) 0.0183(18) 0.0017(14) -0.0002(15) 0.0020(15) C22 0.018(2) 0.0134(18) 0.0194(18) 0.0000(14) 0.0002(15) 0.0004(15) C23 0.022(2) 0.021(2) 0.025(2) 0.0018(16) 0.0025(17) -0.0015(17) C24 0.026(2) 0.026(2) 0.030(2) 0.0043(17) 0.0089(18) -0.0072(18) C25 0.024(2) 0.029(2) 0.024(2) 0.0010(17) 0.0086(17) 0.0015(18) C26 0.027(2) 0.025(2) 0.025(2) -0.0009(16) 0.0083(18) 0.0042(18) C27 0.040(3) 0.019(2) 0.026(2) 0.0049(17) -0.0052(19) -0.0078(19) C28 0.026(2) 0.022(2) 0.026(2) 0.0093(16) -0.0010(17) -0.0050(18) C29 0.036(3) 0.034(2) 0.022(2) 0.0043(18) 0.0002(19) -0.003(2) C30 0.030(3) 0.033(2) 0.028(2) 0.0040(18) 0.0024(18) 0.0040(19) C31 0.075(7) 0.195(12) 0.178(11) 0.094(10) -0.024(7) -0.019(7) C32 0.061(4) 0.036(3) 0.062(4) 0.006(3) -0.018(3) 0.003(3) C33 0.043(3) 0.033(3) 0.049(3) -0.011(2) -0.019(2) 0.006(2) C34 0.078(8) 0.146(9) 0.039(6) -0.009(6) 0.008(6) 0.035(7) O8 0.084(6) 0.096(6) 0.025(3) 0.008(3) 0.022(3) 0.056(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 O3 2.127(3) . ? Mn1 O7 2.229(3) . ? Mn1 N3 2.237(3) . ? Mn1 N7 2.254(3) . ? Mn1 N4 2.304(3) . ? Mn1 N8 2.309(3) . ? Mn2 O1 1.857(3) . ? Mn2 O2 1.882(3) . ? Mn2 N6 2.022(3) . ? Mn2 N2 2.028(3) . ? Mn2 O6 2.264(3) . ? Mn2 O5 2.272(3) . ? N1 C8 1.342(5) . ? N1 C7 1.355(5) . ? N2 C7 1.359(5) . ? N2 N3 1.371(4) . ? N3 C8 1.336(5) . ? N4 C13 1.340(5) . ? N4 C9 1.341(5) . ? N5 C20 1.353(5) . ? N5 C21 1.358(5) . ? N6 C20 1.361(5) . ? N6 N7 1.367(4) . ? N7 C21 1.330(5) . ? N8 C26 1.327(5) . ? N8 C22 1.354(5) . ? O1 C1 1.344(5) . ? O2 C14 1.331(5) . ? O3 C27 1.274(5) . ? O4 C27 1.235(6) . ? O5 C31 1.394(11) . ? O5 H5 0.9500 . ? O6 C32 1.412(6) . ? O6 H6 0.9500 . ? O7 C33 1.425(5) . ? O7 H7 0.9500 . ? C1 C2 1.390(6) . ? C1 C6 1.405(5) . ? C2 C3 1.373(6) . ? C2 H2 0.9500 . ? C3 C4 1.388(6) . ? C3 H3 0.9500 . ? C4 C5 1.369(6) . ? C4 H4 0.9500 . ? C5 C6 1.403(5) . ? C5 H5A 0.9500 . ? C6 C7 1.457(5) . ? C8 C9 1.473(5) . ? C9 C10 1.395(6) . ? C10 C11 1.372(6) . ? C10 H10 0.9500 . ? C11 C12 1.387(7) . ? C11 H11 0.9500 . ? C12 C13 1.377(6) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C19 1.395(6) . ? C14 C15 1.406(6) . ? C15 C16 1.366(6) . ? C15 H15 0.9500 . ? C16 C17 1.391(6) . ? C16 H16 0.9500 . ? C17 C18 1.380(6) . ? C17 H17 0.9500 . ? C18 C19 1.403(6) . ? C18 H18 0.9500 . ? C19 C20 1.465(5) . ? C21 C22 1.461(5) . ? C22 C23 1.398(5) . ? C23 C24 1.372(6) . ? C23 H23 0.9500 . ? C24 C25 1.383(6) . ? C24 H24 0.9500 . ? C25 C26 1.386(6) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.521(6) . ? C28 C29 1.384(6) . ? C28 C30 1.385(6) . ? C29 C30 1.397(6) 3_575 ? C29 H29 0.9500 . ? C30 C29 1.397(6) 3_575 ? C30 H30 0.9500 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 O8 1.425(9) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? O8 H8 0.8400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Mn1 O7 164.67(11) . . ? O3 Mn1 N3 91.31(12) . . ? O7 Mn1 N3 98.04(11) . . ? O3 Mn1 N7 97.64(12) . . ? O7 Mn1 N7 94.92(11) . . ? N3 Mn1 N7 87.30(12) . . ? O3 Mn1 N4 91.62(12) . . ? O7 Mn1 N4 79.68(11) . . ? N3 Mn1 N4 72.80(11) . . ? N7 Mn1 N4 158.26(11) . . ? O3 Mn1 N8 92.89(12) . . ? O7 Mn1 N8 82.56(11) . . ? N3 Mn1 N8 159.63(11) . . ? N7 Mn1 N8 72.40(11) . . ? N4 Mn1 N8 126.93(12) . . ? O1 Mn2 O2 82.76(13) . . ? O1 Mn2 N6 168.36(12) . . ? O2 Mn2 N6 86.24(13) . . ? O1 Mn2 N2 87.43(13) . . ? O2 Mn2 N2 169.11(12) . . ? N6 Mn2 N2 103.83(13) . . ? O1 Mn2 O6 94.64(14) . . ? O2 Mn2 O6 96.60(14) . . ? N6 Mn2 O6 82.84(12) . . ? N2 Mn2 O6 88.87(12) . . ? O1 Mn2 O5 93.21(15) . . ? O2 Mn2 O5 89.65(15) . . ? N6 Mn2 O5 90.49(13) . . ? N2 Mn2 O5 86.18(12) . . ? O6 Mn2 O5 170.52(12) . . ? C8 N1 C7 103.2(3) . . ? C7 N2 N3 106.8(3) . . ? C7 N2 Mn2 127.7(2) . . ? N3 N2 Mn2 125.4(2) . . ? C8 N3 N2 105.2(3) . . ? C8 N3 Mn1 115.9(2) . . ? N2 N3 Mn1 138.7(2) . . ? C13 N4 C9 118.2(3) . . ? C13 N4 Mn1 125.5(3) . . ? C9 N4 Mn1 116.1(2) . . ? C20 N5 C21 102.5(3) . . ? C20 N6 N7 106.6(3) . . ? C20 N6 Mn2 126.7(3) . . ? N7 N6 Mn2 126.6(2) . . ? C21 N7 N6 105.7(3) . . ? C21 N7 Mn1 115.3(2) . . ? N6 N7 Mn1 136.8(2) . . ? C26 N8 C22 117.8(3) . . ? C26 N8 Mn1 125.7(3) . . ? C22 N8 Mn1 116.4(2) . . ? C1 O1 Mn2 136.7(3) . . ? C14 O2 Mn2 132.4(3) . . ? C27 O3 Mn1 111.5(3) . . ? C31 O5 Mn2 125.4(5) . . ? C31 O5 H5 117.3 . . ? Mn2 O5 H5 117.3 . . ? C32 O6 Mn2 125.4(3) . . ? C32 O6 H6 117.3 . . ? Mn2 O6 H6 117.3 . . ? C33 O7 Mn1 127.6(3) . . ? C33 O7 H7 116.2 . . ? Mn1 O7 H7 116.2 . . ? O1 C1 C2 117.4(3) . . ? O1 C1 C6 122.4(3) . . ? C2 C1 C6 120.2(4) . . ? C3 C2 C1 120.7(4) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C2 C3 C4 119.8(4) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 120.0(4) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 121.6(4) . . ? C4 C5 H5A 119.2 . . ? C6 C5 H5A 119.2 . . ? C5 C6 C1 117.6(4) . . ? C5 C6 C7 121.1(3) . . ? C1 C6 C7 121.3(3) . . ? N1 C7 N2 111.0(3) . . ? N1 C7 C6 124.4(3) . . ? N2 C7 C6 124.5(3) . . ? N3 C8 N1 113.7(3) . . ? N3 C8 C9 119.7(3) . . ? N1 C8 C9 126.6(3) . . ? N4 C9 C10 121.7(4) . . ? N4 C9 C8 114.8(3) . . ? C10 C9 C8 123.5(4) . . ? C11 C10 C9 119.2(4) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? C10 C11 C12 119.2(4) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C13 C12 C11 118.2(4) . . ? C13 C12 H12 120.9 . . ? C11 C12 H12 120.9 . . ? N4 C13 C12 123.3(4) . . ? N4 C13 H13 118.3 . . ? C12 C13 H13 118.3 . . ? O2 C14 C19 122.3(4) . . ? O2 C14 C15 117.8(4) . . ? C19 C14 C15 119.8(4) . . ? C16 C15 C14 120.7(4) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 120.1(4) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C18 C17 C16 119.9(4) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 121.0(4) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C14 C19 C18 118.5(4) . . ? C14 C19 C20 120.7(3) . . ? C18 C19 C20 120.8(4) . . ? N5 C20 N6 111.6(3) . . ? N5 C20 C19 124.4(3) . . ? N6 C20 C19 124.0(3) . . ? N7 C21 N5 113.6(3) . . ? N7 C21 C22 120.5(3) . . ? N5 C21 C22 125.9(3) . . ? N8 C22 C23 122.2(3) . . ? N8 C22 C21 114.1(3) . . ? C23 C22 C21 123.6(3) . . ? C24 C23 C22 118.8(4) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C23 C24 C25 119.2(4) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C24 C25 C26 118.7(4) . . ? C24 C25 H25 120.6 . . ? C26 C25 H25 120.6 . . ? N8 C26 C25 123.3(4) . . ? N8 C26 H26 118.4 . . ? C25 C26 H26 118.4 . . ? O4 C27 O3 124.1(4) . . ? O4 C27 C28 120.3(4) . . ? O3 C27 C28 115.6(4) . . ? C29 C28 C30 118.8(4) . . ? C29 C28 C27 121.1(4) . . ? C30 C28 C27 120.0(4) . . ? C28 C29 C30 120.4(4) . 3_575 ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 3_575 . ? C28 C30 C29 120.8(4) . 3_575 ? C28 C30 H30 119.6 . . ? C29 C30 H30 119.6 3_575 . ? O5 C31 H31A 109.5 . . ? O5 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O5 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O6 C32 H32A 109.5 . . ? O6 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O6 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O7 C33 H33A 109.5 . . ? O7 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O7 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O8 C34 H34A 109.5 . . ? O8 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O8 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C34 O8 H8 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 O1 Mn2 N2 C7 0.3(3) . . . . ? O2 Mn2 N2 C7 26.0(10) . . . . ? N6 Mn2 N2 C7 -176.7(3) . . . . ? O6 Mn2 N2 C7 -94.4(3) . . . . ? O5 Mn2 N2 C7 93.7(3) . . . . ? O1 Mn2 N2 N3 -177.5(3) . . . . ? O2 Mn2 N2 N3 -151.8(7) . . . . ? N6 Mn2 N2 N3 5.5(3) . . . . ? O6 Mn2 N2 N3 87.8(3) . . . . ? O5 Mn2 N2 N3 -84.1(3) . . . . ? C7 N2 N3 C8 0.0(4) . . . . ? Mn2 N2 N3 C8 178.2(2) . . . . ? C7 N2 N3 Mn1 173.8(3) . . . . ? Mn2 N2 N3 Mn1 -8.0(5) . . . . ? O3 Mn1 N3 C8 83.7(3) . . . . ? O7 Mn1 N3 C8 -84.1(3) . . . . ? N7 Mn1 N3 C8 -178.7(3) . . . . ? N4 Mn1 N3 C8 -7.6(3) . . . . ? N8 Mn1 N3 C8 -174.3(3) . . . . ? O3 Mn1 N3 N2 -89.7(4) . . . . ? O7 Mn1 N3 N2 102.5(4) . . . . ? N7 Mn1 N3 N2 7.9(4) . . . . ? N4 Mn1 N3 N2 179.0(4) . . . . ? N8 Mn1 N3 N2 12.2(6) . . . . ? O3 Mn1 N4 C13 92.0(3) . . . . ? O7 Mn1 N4 C13 -75.3(3) . . . . ? N3 Mn1 N4 C13 -177.1(3) . . . . ? N7 Mn1 N4 C13 -152.5(3) . . . . ? N8 Mn1 N4 C13 -2.9(4) . . . . ? O3 Mn1 N4 C9 -82.9(3) . . . . ? O7 Mn1 N4 C9 109.8(3) . . . . ? N3 Mn1 N4 C9 8.0(3) . . . . ? N7 Mn1 N4 C9 32.6(5) . . . . ? N8 Mn1 N4 C9 -177.7(2) . . . . ? O1 Mn2 N6 C20 1.2(9) . . . . ? O2 Mn2 N6 C20 -17.8(3) . . . . ? N2 Mn2 N6 C20 166.4(3) . . . . ? O6 Mn2 N6 C20 79.3(3) . . . . ? O5 Mn2 N6 C20 -107.4(3) . . . . ? O1 Mn2 N6 N7 -174.0(6) . . . . ? O2 Mn2 N6 N7 167.0(3) . . . . ? N2 Mn2 N6 N7 -8.8(3) . . . . ? O6 Mn2 N6 N7 -95.8(3) . . . . ? O5 Mn2 N6 N7 77.4(3) . . . . ? C20 N6 N7 C21 0.2(4) . . . . ? Mn2 N6 N7 C21 176.1(2) . . . . ? C20 N6 N7 Mn1 -161.2(3) . . . . ? Mn2 N6 N7 Mn1 14.8(5) . . . . ? O3 Mn1 N7 C21 -80.6(3) . . . . ? O7 Mn1 N7 C21 90.6(3) . . . . ? N3 Mn1 N7 C21 -171.6(3) . . . . ? N4 Mn1 N7 C21 165.0(3) . . . . ? N8 Mn1 N7 C21 10.0(3) . . . . ? O3 Mn1 N7 N6 79.5(3) . . . . ? O7 Mn1 N7 N6 -109.3(3) . . . . ? N3 Mn1 N7 N6 -11.5(3) . . . . ? N4 Mn1 N7 N6 -34.9(5) . . . . ? N8 Mn1 N7 N6 170.1(4) . . . . ? O3 Mn1 N8 C26 -86.7(3) . . . . ? O7 Mn1 N8 C26 78.6(3) . . . . ? N3 Mn1 N8 C26 171.6(3) . . . . ? N7 Mn1 N8 C26 176.2(3) . . . . ? N4 Mn1 N8 C26 7.5(4) . . . . ? O3 Mn1 N8 C22 90.4(3) . . . . ? O7 Mn1 N8 C22 -104.3(3) . . . . ? N3 Mn1 N8 C22 -11.3(5) . . . . ? N7 Mn1 N8 C22 -6.7(3) . . . . ? N4 Mn1 N8 C22 -175.4(2) . . . . ? O2 Mn2 O1 C1 -175.7(4) . . . . ? N6 Mn2 O1 C1 165.2(6) . . . . ? N2 Mn2 O1 C1 -0.4(4) . . . . ? O6 Mn2 O1 C1 88.2(4) . . . . ? O5 Mn2 O1 C1 -86.4(4) . . . . ? O1 Mn2 O2 C14 -144.2(4) . . . . ? N6 Mn2 O2 C14 32.0(4) . . . . ? N2 Mn2 O2 C14 -170.1(6) . . . . ? O6 Mn2 O2 C14 -50.3(4) . . . . ? O5 Mn2 O2 C14 122.5(4) . . . . ? O7 Mn1 O3 C27 -6.0(6) . . . . ? N3 Mn1 O3 C27 -133.8(3) . . . . ? N7 Mn1 O3 C27 138.7(3) . . . . ? N4 Mn1 O3 C27 -61.0(3) . . . . ? N8 Mn1 O3 C27 66.1(3) . . . . ? O1 Mn2 O5 C31 -135.4(8) . . . . ? O2 Mn2 O5 C31 -52.7(8) . . . . ? N6 Mn2 O5 C31 33.5(8) . . . . ? N2 Mn2 O5 C31 137.4(8) . . . . ? O6 Mn2 O5 C31 78.7(11) . . . . ? O1 Mn2 O6 C32 -80.6(4) . . . . ? O2 Mn2 O6 C32 -163.8(4) . . . . ? N6 Mn2 O6 C32 110.8(4) . . . . ? N2 Mn2 O6 C32 6.7(4) . . . . ? O5 Mn2 O6 C32 65.2(8) . . . . ? O3 Mn1 O7 C33 134.2(5) . . . . ? N3 Mn1 O7 C33 -98.8(4) . . . . ? N7 Mn1 O7 C33 -10.8(4) . . . . ? N4 Mn1 O7 C33 -169.6(4) . . . . ? N8 Mn1 O7 C33 60.7(4) . . . . ? Mn2 O1 C1 C2 178.8(3) . . . . ? Mn2 O1 C1 C6 0.4(7) . . . . ? O1 C1 C2 C3 -178.3(4) . . . . ? C6 C1 C2 C3 0.2(6) . . . . ? C1 C2 C3 C4 -1.0(7) . . . . ? C2 C3 C4 C5 0.8(7) . . . . ? C3 C4 C5 C6 0.2(6) . . . . ? C4 C5 C6 C1 -0.9(6) . . . . ? C4 C5 C6 C7 178.2(4) . . . . ? O1 C1 C6 C5 179.1(4) . . . . ? C2 C1 C6 C5 0.7(6) . . . . ? O1 C1 C6 C7 0.0(6) . . . . ? C2 C1 C6 C7 -178.5(4) . . . . ? C8 N1 C7 N2 -0.9(4) . . . . ? C8 N1 C7 C6 -178.2(4) . . . . ? N3 N2 C7 N1 0.6(4) . . . . ? Mn2 N2 C7 N1 -177.5(2) . . . . ? N3 N2 C7 C6 177.9(3) . . . . ? Mn2 N2 C7 C6 -0.2(5) . . . . ? C5 C6 C7 N1 -2.1(6) . . . . ? C1 C6 C7 N1 177.0(4) . . . . ? C5 C6 C7 N2 -179.1(4) . . . . ? C1 C6 C7 N2 0.0(6) . . . . ? N2 N3 C8 N1 -0.6(4) . . . . ? Mn1 N3 C8 N1 -176.1(2) . . . . ? N2 N3 C8 C9 -177.7(3) . . . . ? Mn1 N3 C8 C9 6.8(4) . . . . ? C7 N1 C8 N3 0.9(4) . . . . ? C7 N1 C8 C9 177.8(4) . . . . ? C13 N4 C9 C10 -1.1(6) . . . . ? Mn1 N4 C9 C10 174.1(3) . . . . ? C13 N4 C9 C8 177.5(3) . . . . ? Mn1 N4 C9 C8 -7.3(4) . . . . ? N3 C8 C9 N4 0.5(5) . . . . ? N1 C8 C9 N4 -176.3(4) . . . . ? N3 C8 C9 C10 179.0(4) . . . . ? N1 C8 C9 C10 2.3(6) . . . . ? N4 C9 C10 C11 0.3(7) . . . . ? C8 C9 C10 C11 -178.2(4) . . . . ? C9 C10 C11 C12 0.9(7) . . . . ? C10 C11 C12 C13 -1.2(7) . . . . ? C9 N4 C13 C12 0.8(6) . . . . ? Mn1 N4 C13 C12 -174.0(3) . . . . ? C11 C12 C13 N4 0.4(7) . . . . ? Mn2 O2 C14 C19 -28.6(7) . . . . ? Mn2 O2 C14 C15 153.3(4) . . . . ? O2 C14 C15 C16 179.6(5) . . . . ? C19 C14 C15 C16 1.4(7) . . . . ? C14 C15 C16 C17 0.3(8) . . . . ? C15 C16 C17 C18 -1.9(8) . . . . ? C16 C17 C18 C19 2.0(8) . . . . ? O2 C14 C19 C18 -179.5(4) . . . . ? C15 C14 C19 C18 -1.4(6) . . . . ? O2 C14 C19 C20 0.4(6) . . . . ? C15 C14 C19 C20 178.5(4) . . . . ? C17 C18 C19 C14 -0.3(7) . . . . ? C17 C18 C19 C20 179.8(4) . . . . ? C21 N5 C20 N6 0.6(4) . . . . ? C21 N5 C20 C19 -178.4(4) . . . . ? N7 N6 C20 N5 -0.5(4) . . . . ? Mn2 N6 C20 N5 -176.4(2) . . . . ? N7 N6 C20 C19 178.5(3) . . . . ? Mn2 N6 C20 C19 2.5(5) . . . . ? C14 C19 C20 N5 -170.3(4) . . . . ? C18 C19 C20 N5 9.6(6) . . . . ? C14 C19 C20 N6 10.9(6) . . . . ? C18 C19 C20 N6 -169.2(4) . . . . ? N6 N7 C21 N5 0.2(4) . . . . ? Mn1 N7 C21 N5 166.2(2) . . . . ? N6 N7 C21 C22 -178.8(3) . . . . ? Mn1 N7 C21 C22 -12.9(4) . . . . ? C20 N5 C21 N7 -0.5(4) . . . . ? C20 N5 C21 C22 178.5(4) . . . . ? C26 N8 C22 C23 1.4(6) . . . . ? Mn1 N8 C22 C23 -176.0(3) . . . . ? C26 N8 C22 C21 -179.9(3) . . . . ? Mn1 N8 C22 C21 2.8(4) . . . . ? N7 C21 C22 N8 6.7(5) . . . . ? N5 C21 C22 N8 -172.2(3) . . . . ? N7 C21 C22 C23 -174.5(4) . . . . ? N5 C21 C22 C23 6.5(6) . . . . ? N8 C22 C23 C24 -0.7(6) . . . . ? C21 C22 C23 C24 -179.3(4) . . . . ? C22 C23 C24 C25 -0.3(6) . . . . ? C23 C24 C25 C26 0.6(6) . . . . ? C22 N8 C26 C25 -1.1(6) . . . . ? Mn1 N8 C26 C25 176.0(3) . . . . ? C24 C25 C26 N8 0.1(6) . . . . ? Mn1 O3 C27 O4 -3.8(5) . . . . ? Mn1 O3 C27 C28 175.0(3) . . . . ? O4 C27 C28 C29 -171.5(4) . . . . ? O3 C27 C28 C29 9.6(6) . . . . ? O4 C27 C28 C30 10.2(6) . . . . ? O3 C27 C28 C30 -168.6(4) . . . . ? C30 C28 C29 C30 0.1(7) . . . 3_575 ? C27 C28 C29 C30 -178.1(4) . . . 3_575 ? C29 C28 C30 C29 -0.1(7) . . . 3_575 ? C27 C28 C30 C29 178.1(4) . . . 3_575 ? 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 H7 N5 0.95 1.83 2.751(4) 162.5 2_645 O6 H6 N1 0.95 1.88 2.782(4) 158.3 2 _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.018 _refine_diff_density_min -0.530 _refine_diff_density_rms 0.083 # Attachment '4.cif' data_shelxl4 _database_code_depnum_ccdc_archive 'CCDC 671749' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H66 Mn4 N16 O20' _chemical_formula_sum 'C60 H66 Mn4 N16 O20' _chemical_formula_weight 1551.05 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' 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 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.617(8) _cell_length_b 16.674(7) _cell_length_c 21.381(9) _cell_angle_alpha 90.00 _cell_angle_beta 91.018(5) _cell_angle_gamma 90.00 _cell_volume 6636(5) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 12466 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 27.9 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3192 _exptl_absorpt_coefficient_mu 0.830 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8256 _exptl_absorpt_correction_T_max 0.8515 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48249 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0468 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.01 _reflns_number_total 11670 _reflns_number_gt 10704 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0471P)^2^+16.1263P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11670 _refine_ls_number_parameters 908 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0739 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.1495 _refine_ls_wR_factor_gt 0.1452 _refine_ls_goodness_of_fit_ref 1.179 _refine_ls_restrained_S_all 1.179 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2262(2) 0.8591(3) 0.41473(19) 0.0229(9) Uani 1 1 d . . . H1 H 0.2097 0.9050 0.4365 0.027 Uiso 1 1 calc R . . C2 C 0.1960(2) 0.7854(3) 0.4283(2) 0.0265(10) Uani 1 1 d . . . H2 H 0.1599 0.7811 0.4590 0.032 Uiso 1 1 calc R . . C3 C 0.2192(2) 0.7185(3) 0.3967(2) 0.0270(10) Uani 1 1 d . . . H3 H 0.1992 0.6674 0.4053 0.032 Uiso 1 1 calc R . . C4 C 0.2723(2) 0.7266(3) 0.3521(2) 0.0233(9) Uani 1 1 d . . . H4 H 0.2894 0.6814 0.3298 0.028 Uiso 1 1 calc R . . C5 C 0.2993(2) 0.8028(2) 0.34115(18) 0.0178(8) Uani 1 1 d . . . C6 C 0.35383(19) 0.8183(2) 0.29356(18) 0.0158(8) Uani 1 1 d . . . C7 C 0.4307(2) 0.8079(2) 0.22336(19) 0.0168(8) Uani 1 1 d . . . C8 C 0.4779(2) 0.7756(2) 0.17605(19) 0.0170(8) Uani 1 1 d . . . C9 C 0.4730(2) 0.6947(2) 0.1587(2) 0.0225(9) Uani 1 1 d . . . H9 H 0.4394 0.6608 0.1786 0.027 Uiso 1 1 calc R . . C10 C 0.5165(2) 0.6636(3) 0.1129(2) 0.0237(9) Uani 1 1 d . . . H10 H 0.5133 0.6085 0.1020 0.028 Uiso 1 1 calc R . . C11 C 0.5648(2) 0.7128(3) 0.08302(19) 0.0229(9) Uani 1 1 d . . . H11 H 0.5935 0.6918 0.0506 0.027 Uiso 1 1 calc R . . C12 C 0.5714(2) 0.7923(3) 0.1002(2) 0.0226(9) Uani 1 1 d . . . H12 H 0.6049 0.8256 0.0795 0.027 Uiso 1 1 calc R . . C13 C 0.5295(2) 0.8241(2) 0.14741(19) 0.0186(8) Uani 1 1 d . . . C14 C 0.2210(2) 1.1228(3) 0.39983(19) 0.0220(9) Uani 1 1 d . . . H14 H 0.2042 1.0794 0.4244 0.026 Uiso 1 1 calc R . . C15 C 0.1897(2) 1.1974(3) 0.4074(2) 0.0261(10) Uani 1 1 d . . . H15 H 0.1522 1.2049 0.4364 0.031 Uiso 1 1 calc R . . C16 C 0.2139(2) 1.2606(3) 0.3720(2) 0.0273(10) Uani 1 1 d . . . H16 H 0.1935 1.3125 0.3764 0.033 Uiso 1 1 calc R . . C17 C 0.2687(2) 1.2476(3) 0.3296(2) 0.0232(9) Uani 1 1 d . . . H17 H 0.2866 1.2902 0.3049 0.028 Uiso 1 1 calc R . . C18 C 0.2963(2) 1.1706(2) 0.32451(19) 0.0173(8) Uani 1 1 d . . . C19 C 0.3523(2) 1.1494(2) 0.27996(19) 0.0178(8) Uani 1 1 d . . . C20 C 0.4293(2) 1.1494(2) 0.20927(19) 0.0172(8) Uani 1 1 d . . . C21 C 0.4770(2) 1.1749(2) 0.15941(19) 0.0189(9) Uani 1 1 d . . . C22 C 0.4695(2) 1.2509(2) 0.1319(2) 0.0225(9) Uani 1 1 d . . . H22 H 0.4329 1.2859 0.1459 0.027 Uiso 1 1 calc R . . C23 C 0.5145(2) 1.2758(3) 0.0849(2) 0.0286(10) Uani 1 1 d . . . H23 H 0.5086 1.3274 0.0667 0.034 Uiso 1 1 calc R . . C24 C 0.5680(2) 1.2249(3) 0.0647(2) 0.0274(10) Uani 1 1 d . . . H24 H 0.5989 1.2415 0.0322 0.033 Uiso 1 1 calc R . . C25 C 0.5768(2) 1.1498(3) 0.09161(19) 0.0221(9) Uani 1 1 d . . . H25 H 0.6135 1.1153 0.0771 0.027 Uiso 1 1 calc R . . C26 C 0.5323(2) 1.1243(2) 0.13980(19) 0.0182(8) Uani 1 1 d . . . C27 C 0.4159(2) 0.9939(2) 0.44500(19) 0.0175(8) Uani 1 1 d . . . C28 C 0.4647(2) 1.0038(2) 0.50061(19) 0.0189(8) Uani 1 1 d . . . H28 H 0.4435 1.0165 0.5395 0.023 Uiso 1 1 calc R . . C29 C 0.4243(3) 0.9549(5) 0.0566(2) 0.0617(19) Uani 1 1 d . . . H29A H 0.4760 0.9587 0.0491 0.093 Uiso 1 1 calc R . . H29B H 0.3980 0.9877 0.0258 0.093 Uiso 1 1 calc R . . H29C H 0.4090 0.8989 0.0528 0.093 Uiso 1 1 calc R . . C30 C 0.7809(2) 0.3553(3) 0.04955(19) 0.0226(9) Uani 1 1 d . . . H30 H 0.7925 0.4010 0.0252 0.027 Uiso 1 1 calc R . . C31 C 0.8078(2) 0.2814(3) 0.0321(2) 0.0236(9) Uani 1 1 d . . . H31 H 0.8364 0.2763 -0.0040 0.028 Uiso 1 1 calc R . . C32 C 0.7922(2) 0.2154(3) 0.0680(2) 0.0269(10) Uani 1 1 d . . . H32 H 0.8102 0.1641 0.0569 0.032 Uiso 1 1 calc R . . C33 C 0.7505(2) 0.2241(3) 0.1202(2) 0.0249(10) Uani 1 1 d . . . H33 H 0.7397 0.1792 0.1457 0.030 Uiso 1 1 calc R . . C34 C 0.7245(2) 0.2998(2) 0.13456(18) 0.0170(8) Uani 1 1 d . . . C35 C 0.6764(2) 0.3148(2) 0.18757(18) 0.0167(8) Uani 1 1 d . . . C36 C 0.6038(2) 0.3041(2) 0.26086(18) 0.0164(8) Uani 1 1 d . . . C37 C 0.5567(2) 0.2723(2) 0.30900(19) 0.0179(8) Uani 1 1 d . . . C38 C 0.5619(2) 0.1918(2) 0.3271(2) 0.0213(9) Uani 1 1 d . . . H38 H 0.5958 0.1581 0.3073 0.026 Uiso 1 1 calc R . . C39 C 0.5191(2) 0.1602(3) 0.3729(2) 0.0250(10) Uani 1 1 d . . . H39 H 0.5235 0.1055 0.3847 0.030 Uiso 1 1 calc R . . C40 C 0.4695(2) 0.2097(3) 0.4015(2) 0.0265(10) Uani 1 1 d . . . H40 H 0.4407 0.1889 0.4340 0.032 Uiso 1 1 calc R . . C41 C 0.4614(2) 0.2886(3) 0.3834(2) 0.0237(9) Uani 1 1 d . . . H41 H 0.4269 0.3216 0.4032 0.028 Uiso 1 1 calc R . . C42 C 0.5040(2) 0.3203(2) 0.33595(19) 0.0195(9) Uani 1 1 d . . . C43 C 0.7850(2) 0.6177(2) 0.0622(2) 0.0219(9) Uani 1 1 d . . . H43 H 0.7957 0.5747 0.0347 0.026 Uiso 1 1 calc R . . C44 C 0.8159(2) 0.6923(3) 0.0513(2) 0.0275(10) Uani 1 1 d . . . H44 H 0.8470 0.7002 0.0171 0.033 Uiso 1 1 calc R . . C45 C 0.8004(2) 0.7546(3) 0.0914(2) 0.0254(10) Uani 1 1 d . . . H45 H 0.8207 0.8062 0.0850 0.031 Uiso 1 1 calc R . . C46 C 0.7552(2) 0.7414(2) 0.1408(2) 0.0227(9) Uani 1 1 d . . . H46 H 0.7441 0.7837 0.1688 0.027 Uiso 1 1 calc R . . C47 C 0.7260(2) 0.6653(2) 0.14891(19) 0.0187(9) Uani 1 1 d . . . C48 C 0.6767(2) 0.6438(2) 0.19882(19) 0.0171(8) Uani 1 1 d . . . C49 C 0.6038(2) 0.6462(2) 0.27267(18) 0.0178(8) Uani 1 1 d . . . C50 C 0.5563(2) 0.6734(2) 0.3225(2) 0.0221(9) Uani 1 1 d . . . C51 C 0.5614(2) 0.7519(3) 0.3459(2) 0.0280(10) Uani 1 1 d . . . H51 H 0.5963 0.7873 0.3295 0.034 Uiso 1 1 calc R . . C52 C 0.5166(2) 0.7783(3) 0.3921(2) 0.0329(11) Uani 1 1 d . . . H52 H 0.5203 0.8317 0.4073 0.039 Uiso 1 1 calc R . . C53 C 0.4662(2) 0.7265(3) 0.4163(2) 0.0336(11) Uani 1 1 d . . . H53 H 0.4363 0.7440 0.4491 0.040 Uiso 1 1 calc R . . C54 C 0.4588(2) 0.6490(3) 0.3930(2) 0.0277(10) Uani 1 1 d . . . H54 H 0.4238 0.6140 0.4098 0.033 Uiso 1 1 calc R . . C55 C 0.5029(2) 0.6222(2) 0.34465(19) 0.0206(9) Uani 1 1 d . . . C56 C 0.5965(2) 0.4912(2) 0.03547(19) 0.0189(9) Uani 1 1 d . . . C57 C 0.5337(2) 0.5016(2) -0.00835(19) 0.0188(8) Uani 1 1 d . . . H57 H 0.5433 0.5111 -0.0512 0.023 Uiso 1 1 calc R . . C58 C 0.5870(3) 0.4732(3) 0.4338(2) 0.0346(11) Uani 1 1 d . . . H58A H 0.5842 0.5298 0.4457 0.052 Uiso 1 1 calc R . . H58B H 0.6173 0.4443 0.4642 0.052 Uiso 1 1 calc R . . H58C H 0.5387 0.4499 0.4330 0.052 Uiso 1 1 calc R . . C59 C 0.2096(3) 0.9765(4) 0.1139(3) 0.0508(15) Uani 1 1 d . . . H59A H 0.1707 0.9490 0.1356 0.076 Uiso 1 1 calc R . . H59B H 0.2154 0.9526 0.0724 0.076 Uiso 1 1 calc R . . H59C H 0.1978 1.0335 0.1095 0.076 Uiso 1 1 calc R . . C60 C 0.7951(3) 0.4633(3) 0.4035(3) 0.0422(13) Uani 1 1 d . . . H60A H 0.8454 0.4795 0.3997 0.063 Uiso 1 1 calc R . . H60B H 0.7864 0.4142 0.3794 0.063 Uiso 1 1 calc R . . H60C H 0.7846 0.4536 0.4476 0.063 Uiso 1 1 calc R . . Mn1 Mn 0.32849(3) 0.98738(3) 0.34380(3) 0.01557(15) Uani 1 1 d . . . Mn2 Mn 0.48298(3) 0.97824(3) 0.20206(3) 0.01544(15) Uani 1 1 d . . . Mn3 Mn 0.69405(3) 0.48283(3) 0.13300(3) 0.01580(15) Uani 1 1 d . . . Mn4 Mn 0.55140(3) 0.47436(4) 0.28384(3) 0.01689(16) Uani 1 1 d . . . N1 N 0.27727(17) 0.8685(2) 0.37238(15) 0.0178(7) Uani 1 1 d . . . N2 N 0.38682(17) 0.76295(19) 0.25822(15) 0.0175(7) Uani 1 1 d . . . N3 N 0.37356(16) 0.89335(19) 0.28202(15) 0.0162(7) Uani 1 1 d . . . N4 N 0.42389(16) 0.88733(19) 0.23597(15) 0.0160(7) Uani 1 1 d . . . N5 N 0.27346(17) 1.1089(2) 0.35963(16) 0.0192(7) Uani 1 1 d . . . N6 N 0.38438(17) 1.19904(19) 0.23880(16) 0.0182(7) Uani 1 1 d . . . N7 N 0.37534(16) 1.0740(2) 0.27700(15) 0.0167(7) Uani 1 1 d . . . N8 N 0.42510(16) 1.07364(19) 0.23086(15) 0.0167(7) Uani 1 1 d . . . N9 N 0.73925(17) 0.3650(2) 0.09939(15) 0.0177(7) Uani 1 1 d . . . N10 N 0.64608(17) 0.25927(19) 0.22407(15) 0.0173(7) Uani 1 1 d . . . N11 N 0.65627(17) 0.38978(19) 0.19995(15) 0.0166(7) Uani 1 1 d . . . N12 N 0.61007(17) 0.38346(19) 0.24810(15) 0.0163(7) Uani 1 1 d . . . N13 N 0.74096(17) 0.6042(2) 0.10944(15) 0.0179(7) Uani 1 1 d . . . N14 N 0.64723(17) 0.69504(19) 0.23990(16) 0.0188(7) Uani 1 1 d . . . N15 N 0.65603(17) 0.56828(19) 0.20546(15) 0.0160(7) Uani 1 1 d . . . N16 N 0.60888(17) 0.5689(2) 0.25366(15) 0.0174(7) Uani 1 1 d . . . O1 O 0.54264(14) 0.90048(16) 0.16600(13) 0.0205(6) Uani 1 1 d . . . O2 O 0.54658(14) 1.05324(16) 0.16727(13) 0.0198(6) Uani 1 1 d . . . O3 O 0.44192(15) 0.97747(18) 0.39212(13) 0.0236(7) Uani 1 1 d . . . O4 O 0.34938(14) 1.00379(17) 0.45160(13) 0.0226(6) Uani 1 1 d . . . O5 O 0.41008(16) 0.9826(2) 0.11654(14) 0.0302(7) Uani 1 1 d . . . H5 H 0.3642 1.0062 0.1222 0.036 Uiso 1 1 calc R . . O6 O 0.23079(14) 0.98041(16) 0.27245(14) 0.0221(6) Uani 1 1 d . . . H6A H 0.1880 0.9845 0.2854 0.027 Uiso 1 1 d R . . H6B H 0.2383 0.9738 0.2337 0.027 Uiso 1 1 d R . . O7 O 0.53883(14) 0.97695(17) 0.29681(13) 0.0228(7) Uani 1 1 d . . . H7A H 0.5146 0.9829 0.3298 0.027 Uiso 1 1 d R . . H7B H 0.5841 0.9705 0.2995 0.027 Uiso 1 1 d R . . O8 O 0.48948(14) 0.39576(17) 0.31655(14) 0.0221(6) Uani 1 1 d . . . O9 O 0.48940(14) 0.54948(17) 0.32011(13) 0.0221(6) Uani 1 1 d . . . O10 O 0.58475(14) 0.47751(16) 0.09275(13) 0.0207(6) Uani 1 1 d . . . O11 O 0.65868(14) 0.49787(17) 0.01469(14) 0.0235(7) Uani 1 1 d . . . O12 O 0.61741(16) 0.46670(19) 0.37313(13) 0.0287(7) Uani 1 1 d . . . H12A H 0.6678 0.4588 0.3703 0.034 Uiso 1 1 calc R . . O13 O 0.80506(14) 0.48052(16) 0.18539(13) 0.0203(6) Uani 1 1 d . . . H13A H 0.8330 0.5207 0.1833 0.024 Uiso 1 1 d R . . H13B H 0.8176 0.4395 0.2065 0.024 Uiso 1 1 d R . . O14 O 0.48912(15) 0.47506(17) 0.19035(13) 0.0229(6) Uani 1 1 d . . . H14A H 0.5005 0.4425 0.1616 0.027 Uiso 1 1 d R . . H14B H 0.4547 0.5079 0.1844 0.027 Uiso 1 1 d R . . O15 O 0.27446(18) 0.9682(3) 0.14908(17) 0.0586(12) Uani 1 1 d . . . H15A H 0.2667 0.9776 0.1870 0.088 Uiso 1 1 calc R . . O16 O 0.74955(17) 0.52573(19) 0.37997(17) 0.0350(8) Uani 1 1 d . . . H16A H 0.7662 0.5436 0.3465 0.052 Uiso 1 1 calc R . . O17 O 0.66719(15) 0.86030(17) 0.23568(14) 0.0268(7) Uani 1 1 d . . . O18 O 0.67534(14) 0.09175(16) 0.22022(13) 0.0217(6) Uani 1 1 d . . . O19 O 0.14037(15) 0.09704(17) 0.23990(15) 0.0286(7) Uani 1 1 d . . . O20 O 0.12358(15) 0.86727(17) 0.26609(14) 0.0253(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.023(2) 0.031(2) 0.015(2) 0.0026(18) 0.0037(17) -0.0011(18) C2 0.025(2) 0.034(3) 0.020(2) -0.0005(19) 0.0087(18) -0.0021(19) C3 0.029(2) 0.028(2) 0.025(2) 0.0017(19) 0.0071(19) -0.0081(19) C4 0.023(2) 0.019(2) 0.027(2) -0.0026(18) 0.0050(18) -0.0023(17) C5 0.0172(19) 0.020(2) 0.016(2) -0.0016(17) -0.0023(16) -0.0017(16) C6 0.0141(18) 0.015(2) 0.018(2) -0.0004(16) 0.0016(15) 0.0006(15) C7 0.0148(19) 0.013(2) 0.022(2) -0.0010(16) -0.0011(16) 0.0006(15) C8 0.0165(19) 0.015(2) 0.019(2) -0.0027(17) 0.0010(16) 0.0030(15) C9 0.022(2) 0.020(2) 0.026(2) -0.0047(18) 0.0042(17) -0.0020(17) C10 0.024(2) 0.017(2) 0.030(2) -0.0104(18) 0.0005(18) -0.0011(17) C11 0.026(2) 0.024(2) 0.019(2) -0.0069(18) 0.0049(17) 0.0024(18) C12 0.022(2) 0.023(2) 0.022(2) -0.0003(18) 0.0023(17) 0.0009(17) C13 0.021(2) 0.016(2) 0.019(2) -0.0004(17) 0.0003(16) 0.0037(16) C14 0.022(2) 0.026(2) 0.018(2) 0.0010(18) 0.0037(17) 0.0000(18) C15 0.021(2) 0.035(3) 0.023(2) -0.005(2) 0.0093(18) 0.0025(18) C16 0.029(2) 0.025(2) 0.028(3) -0.007(2) 0.0013(19) 0.0074(19) C17 0.020(2) 0.018(2) 0.032(2) -0.0025(18) 0.0007(18) 0.0026(17) C18 0.0144(19) 0.018(2) 0.020(2) -0.0025(17) 0.0011(16) 0.0011(16) C19 0.0169(19) 0.015(2) 0.022(2) 0.0016(17) -0.0011(16) -0.0006(16) C20 0.0160(19) 0.015(2) 0.020(2) -0.0009(17) 0.0018(16) 0.0004(15) C21 0.023(2) 0.017(2) 0.017(2) 0.0007(17) 0.0012(16) -0.0025(16) C22 0.023(2) 0.018(2) 0.027(2) 0.0020(18) 0.0039(18) -0.0004(17) C23 0.036(3) 0.022(2) 0.028(3) 0.0079(19) 0.003(2) -0.0015(19) C24 0.029(2) 0.029(3) 0.024(2) 0.006(2) 0.0043(19) -0.0010(19) C25 0.025(2) 0.024(2) 0.018(2) -0.0002(18) 0.0052(17) -0.0002(17) C26 0.0178(19) 0.015(2) 0.021(2) -0.0018(17) -0.0022(16) -0.0036(16) C27 0.021(2) 0.012(2) 0.020(2) 0.0030(16) 0.0031(16) 0.0000(16) C28 0.0223(19) 0.018(2) 0.017(2) -0.0012(17) 0.0010(16) -0.0011(16) C29 0.049(3) 0.113(6) 0.023(3) -0.014(3) 0.001(2) 0.020(4) C30 0.023(2) 0.027(2) 0.018(2) 0.0020(18) 0.0035(17) -0.0019(18) C31 0.022(2) 0.026(2) 0.023(2) -0.0048(19) 0.0084(17) 0.0018(18) C32 0.026(2) 0.023(2) 0.032(3) -0.004(2) 0.0069(19) 0.0019(18) C33 0.027(2) 0.018(2) 0.029(2) 0.0022(19) 0.0045(19) -0.0011(18) C34 0.0171(19) 0.016(2) 0.018(2) -0.0005(16) 0.0022(16) -0.0007(16) C35 0.0144(19) 0.016(2) 0.020(2) -0.0008(17) -0.0019(16) 0.0006(15) C36 0.0177(19) 0.012(2) 0.019(2) 0.0030(16) -0.0007(16) -0.0005(15) C37 0.019(2) 0.017(2) 0.018(2) 0.0010(17) 0.0030(16) -0.0014(16) C38 0.021(2) 0.016(2) 0.026(2) 0.0034(18) 0.0055(17) -0.0012(17) C39 0.028(2) 0.022(2) 0.025(2) 0.0050(19) 0.0043(18) -0.0026(18) C40 0.026(2) 0.028(2) 0.026(2) 0.0056(19) 0.0094(18) -0.0060(19) C41 0.023(2) 0.023(2) 0.025(2) 0.0047(18) 0.0080(18) 0.0031(17) C42 0.020(2) 0.014(2) 0.025(2) -0.0002(17) 0.0003(17) -0.0040(16) C43 0.027(2) 0.018(2) 0.021(2) 0.0019(17) 0.0025(18) 0.0004(17) C44 0.025(2) 0.030(3) 0.028(2) 0.002(2) 0.0039(19) -0.0011(19) C45 0.025(2) 0.020(2) 0.031(3) 0.0069(19) 0.0010(19) -0.0063(18) C46 0.022(2) 0.016(2) 0.029(2) 0.0008(18) -0.0005(18) -0.0004(17) C47 0.0163(19) 0.018(2) 0.022(2) 0.0019(17) -0.0019(16) 0.0004(16) C48 0.0164(19) 0.014(2) 0.021(2) 0.0015(16) -0.0026(16) 0.0017(15) C49 0.0146(19) 0.021(2) 0.017(2) -0.0046(17) -0.0003(16) 0.0008(16) C50 0.022(2) 0.019(2) 0.025(2) -0.0031(18) 0.0009(17) 0.0034(17) C51 0.026(2) 0.026(2) 0.032(3) -0.006(2) 0.003(2) 0.0000(19) C52 0.030(2) 0.026(3) 0.042(3) -0.016(2) 0.006(2) 0.000(2) C53 0.030(2) 0.039(3) 0.032(3) -0.012(2) 0.007(2) 0.007(2) C54 0.027(2) 0.027(2) 0.029(3) -0.009(2) 0.0071(19) 0.0011(19) C55 0.022(2) 0.020(2) 0.020(2) -0.0037(17) -0.0002(17) 0.0045(17) C56 0.024(2) 0.011(2) 0.022(2) -0.0033(17) -0.0002(17) 0.0000(16) C57 0.0231(19) 0.018(2) 0.015(2) -0.0001(17) 0.0027(16) 0.0001(16) C58 0.039(3) 0.046(3) 0.018(2) -0.001(2) 0.005(2) -0.001(2) C59 0.036(3) 0.069(4) 0.048(4) -0.001(3) -0.011(3) 0.005(3) C60 0.037(3) 0.036(3) 0.054(4) 0.007(3) 0.008(2) 0.002(2) Mn1 0.0169(3) 0.0135(3) 0.0165(3) -0.0005(2) 0.0024(2) 0.0001(2) Mn2 0.0152(3) 0.0123(3) 0.0189(3) -0.0003(2) 0.0039(2) -0.0002(2) Mn3 0.0166(3) 0.0131(3) 0.0178(3) 0.0006(2) 0.0020(2) -0.0003(2) Mn4 0.0168(3) 0.0144(3) 0.0195(3) -0.0002(2) 0.0043(2) 0.0010(2) N1 0.0196(17) 0.0177(18) 0.0160(18) -0.0006(14) 0.0018(14) 0.0002(14) N2 0.0163(16) 0.0166(18) 0.0197(18) -0.0009(14) 0.0047(14) -0.0015(13) N3 0.0160(16) 0.0136(17) 0.0193(18) -0.0009(14) 0.0030(13) -0.0005(13) N4 0.0146(16) 0.0172(18) 0.0163(17) -0.0036(14) 0.0020(13) 0.0022(13) N5 0.0195(17) 0.0186(18) 0.0194(18) 0.0001(15) 0.0014(14) -0.0010(14) N6 0.0178(17) 0.0149(17) 0.0219(19) 0.0008(14) 0.0024(14) 0.0000(13) N7 0.0136(16) 0.0170(18) 0.0194(18) -0.0036(14) 0.0015(13) 0.0013(13) N8 0.0157(16) 0.0157(17) 0.0189(18) 0.0009(14) 0.0040(13) 0.0018(13) N9 0.0177(17) 0.0183(18) 0.0172(18) -0.0011(14) 0.0019(14) 0.0007(14) N10 0.0163(16) 0.0165(18) 0.0191(18) 0.0016(14) 0.0021(13) -0.0005(13) N11 0.0186(16) 0.0161(18) 0.0154(17) 0.0015(14) 0.0047(13) 0.0004(13) N12 0.0169(16) 0.0138(17) 0.0182(18) 0.0020(14) 0.0020(13) -0.0024(13) N13 0.0194(17) 0.0192(18) 0.0150(18) 0.0016(14) -0.0005(14) -0.0003(14) N14 0.0174(17) 0.0143(17) 0.0246(19) -0.0011(14) -0.0004(14) -0.0010(13) N15 0.0196(16) 0.0134(17) 0.0150(17) -0.0007(13) 0.0004(13) 0.0008(13) N16 0.0181(16) 0.0175(18) 0.0169(18) -0.0028(14) 0.0046(13) 0.0010(14) O1 0.0200(14) 0.0133(14) 0.0283(16) -0.0007(12) 0.0070(12) -0.0005(11) O2 0.0200(14) 0.0134(14) 0.0262(16) 0.0037(12) 0.0038(12) -0.0007(11) O3 0.0229(15) 0.0302(17) 0.0177(16) -0.0001(13) 0.0034(12) -0.0030(12) O4 0.0177(14) 0.0244(16) 0.0255(16) -0.0028(13) 0.0003(12) 0.0016(12) O5 0.0238(15) 0.046(2) 0.0207(16) -0.0055(14) -0.0017(13) 0.0032(14) O6 0.0171(14) 0.0240(16) 0.0253(16) -0.0010(13) 0.0013(12) 0.0007(12) O7 0.0140(13) 0.0339(18) 0.0207(16) -0.0024(13) 0.0032(11) 0.0022(12) O8 0.0165(14) 0.0210(16) 0.0289(17) 0.0023(13) 0.0049(12) 0.0023(12) O9 0.0210(14) 0.0193(15) 0.0262(16) -0.0045(13) 0.0066(12) -0.0012(12) O10 0.0227(14) 0.0212(16) 0.0182(16) 0.0006(12) -0.0025(12) 0.0007(12) O11 0.0185(15) 0.0259(16) 0.0263(17) -0.0004(13) 0.0028(12) -0.0011(12) O12 0.0244(15) 0.044(2) 0.0178(16) 0.0002(14) 0.0027(12) 0.0029(14) O13 0.0210(14) 0.0133(14) 0.0267(16) 0.0040(12) -0.0001(12) -0.0021(11) O14 0.0237(15) 0.0212(16) 0.0237(16) -0.0007(12) -0.0007(12) 0.0055(12) O15 0.0275(19) 0.117(4) 0.031(2) -0.015(2) 0.0027(16) 0.003(2) O16 0.0326(18) 0.0290(19) 0.044(2) 0.0028(15) 0.0098(15) -0.0005(14) O17 0.0244(15) 0.0205(16) 0.0353(18) -0.0083(14) -0.0038(13) 0.0005(12) O18 0.0208(14) 0.0166(15) 0.0277(16) 0.0033(12) 0.0020(12) 0.0014(11) O19 0.0236(15) 0.0200(16) 0.042(2) 0.0026(14) 0.0006(14) 0.0037(12) O20 0.0224(15) 0.0194(16) 0.0341(18) -0.0024(13) 0.0028(13) -0.0013(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.334(5) . ? C1 C2 1.383(6) . ? C1 H1 0.9500 . ? C2 C3 1.378(6) . ? C2 H2 0.9500 . ? C3 C4 1.392(6) . ? C3 H3 0.9500 . ? C4 C5 1.387(6) . ? C4 H4 0.9500 . ? C5 N1 1.351(5) . ? C5 C6 1.472(5) . ? C6 N3 1.328(5) . ? C6 N2 1.348(5) . ? C7 N2 1.344(5) . ? C7 N4 1.358(5) . ? C7 C8 1.455(5) . ? C8 C9 1.402(6) . ? C8 C13 1.404(6) . ? C9 C10 1.382(6) . ? C9 H9 0.9500 . ? C10 C11 1.381(6) . ? C10 H10 0.9500 . ? C11 C12 1.381(6) . ? C11 H11 0.9500 . ? C12 C13 1.392(6) . ? C12 H12 0.9500 . ? C13 O1 1.355(5) . ? C14 N5 1.333(5) . ? C14 C15 1.385(6) . ? C14 H14 0.9500 . ? C15 C16 1.378(6) . ? C15 H15 0.9500 . ? C16 C17 1.393(6) . ? C16 H16 0.9500 . ? C17 C18 1.388(6) . ? C17 H17 0.9500 . ? C18 N5 1.346(5) . ? C18 C19 1.467(5) . ? C19 N7 1.331(5) . ? C19 N6 1.354(5) . ? C20 N6 1.343(5) . ? C20 N8 1.348(5) . ? C20 C21 1.462(5) . ? C21 C26 1.401(6) . ? C21 C22 1.402(6) . ? C22 C23 1.383(6) . ? C22 H22 0.9500 . ? C23 C24 1.384(6) . ? C23 H23 0.9500 . ? C24 C25 1.386(6) . ? C24 H24 0.9500 . ? C25 C26 1.400(6) . ? C25 H25 0.9500 . ? C26 O2 1.347(5) . ? C27 O4 1.260(5) . ? C27 O3 1.267(5) . ? C27 C28 1.492(6) . ? C28 C28 1.323(8) 3_676 ? C28 H28 0.9500 . ? C29 O5 1.392(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 N9 1.339(5) . ? C30 C31 1.383(6) . ? C30 H30 0.9500 . ? C31 C32 1.375(6) . ? C31 H31 0.9500 . ? C32 C33 1.379(6) . ? C32 H32 0.9500 . ? C33 C34 1.388(6) . ? C33 H33 0.9500 . ? C34 N9 1.353(5) . ? C34 C35 1.478(5) . ? C35 N11 1.334(5) . ? C35 N10 1.342(5) . ? C36 N10 1.349(5) . ? C36 N12 1.357(5) . ? C36 C37 1.464(5) . ? C37 C42 1.399(6) . ? C37 C38 1.400(6) . ? C38 C39 1.378(6) . ? C38 H38 0.9500 . ? C39 C40 1.389(6) . ? C39 H39 0.9500 . ? C40 C41 1.379(6) . ? C40 H40 0.9500 . ? C41 C42 1.403(6) . ? C41 H41 0.9500 . ? C42 O8 1.350(5) . ? C43 N13 1.331(5) . ? C43 C44 1.392(6) . ? C43 H43 0.9500 . ? C44 C45 1.380(6) . ? C44 H44 0.9500 . ? C45 C46 1.380(6) . ? C45 H45 0.9500 . ? C46 C47 1.393(6) . ? C46 H46 0.9500 . ? C47 N13 1.356(5) . ? C47 C48 1.464(6) . ? C48 N15 1.325(5) . ? C48 N14 1.349(5) . ? C49 N14 1.352(5) . ? C49 N16 1.355(5) . ? C49 C50 1.469(6) . ? C50 C55 1.398(6) . ? C50 C51 1.403(6) . ? C51 C52 1.378(6) . ? C51 H51 0.9500 . ? C52 C53 1.381(7) . ? C52 H52 0.9500 . ? C53 C54 1.391(6) . ? C53 H53 0.9500 . ? C54 C55 1.404(6) . ? C54 H54 0.9500 . ? C55 O9 1.344(5) . ? C56 O11 1.252(5) . ? C56 O10 1.269(5) . ? C56 C57 1.495(6) . ? C57 C57 1.312(8) 3_665 ? C57 H57 0.9500 . ? C58 O12 1.428(5) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 O15 1.418(6) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 O16 1.428(6) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? Mn1 N7 2.221(3) . ? Mn1 N3 2.224(3) . ? Mn1 N1 2.287(3) . ? Mn1 N5 2.299(3) . ? Mn1 O3 2.340(3) . ? Mn1 O4 2.347(3) . ? Mn1 O6 2.356(3) . ? Mn2 O1 1.881(3) . ? Mn2 O2 1.884(3) . ? Mn2 N4 2.015(3) . ? Mn2 N8 2.023(3) . ? Mn2 O5 2.259(3) . ? Mn2 O7 2.261(3) . ? Mn3 O10 2.197(3) . ? Mn3 N15 2.229(3) . ? Mn3 N11 2.233(3) . ? Mn3 N9 2.260(3) . ? Mn3 N13 2.264(3) . ? Mn3 O13 2.333(3) . ? Mn4 O9 1.880(3) . ? Mn4 O8 1.888(3) . ? Mn4 N16 2.018(3) . ? Mn4 N12 2.026(3) . ? Mn4 O12 2.256(3) . ? Mn4 O14 2.293(3) . ? N3 N4 1.375(4) . ? N7 N8 1.365(4) . ? N11 N12 1.357(4) . ? N15 N16 1.366(4) . ? O5 H5 0.9500 . ? O6 H6A 0.8500 . ? O6 H6B 0.8501 . ? O7 H7A 0.8501 . ? O7 H7B 0.8501 . ? O12 H12A 0.9500 . ? O13 H13A 0.8499 . ? O13 H13B 0.8502 . ? O14 H14A 0.8500 . ? O14 H14B 0.8500 . ? O15 H15A 0.8400 . ? O16 H16A 0.8400 . ? 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 C1 C2 122.9(4) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C3 C2 C1 118.9(4) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 119.4(4) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 117.9(4) . . ? C5 C4 H4 121.0 . . ? C3 C4 H4 121.0 . . ? N1 C5 C4 123.0(4) . . ? N1 C5 C6 114.7(3) . . ? C4 C5 C6 122.3(4) . . ? N3 C6 N2 114.3(3) . . ? N3 C6 C5 119.4(3) . . ? N2 C6 C5 126.4(4) . . ? N2 C7 N4 111.9(3) . . ? N2 C7 C8 124.0(4) . . ? N4 C7 C8 124.0(4) . . ? C9 C8 C13 118.7(4) . . ? C9 C8 C7 120.2(4) . . ? C13 C8 C7 121.1(4) . . ? C10 C9 C8 120.8(4) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C11 C10 C9 119.9(4) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.2(4) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C13 120.7(4) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? O1 C13 C12 118.0(4) . . ? O1 C13 C8 122.3(3) . . ? C12 C13 C8 119.6(4) . . ? N5 C14 C15 123.0(4) . . ? N5 C14 H14 118.5 . . ? C15 C14 H14 118.5 . . ? C16 C15 C14 118.7(4) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C15 C16 C17 119.2(4) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C18 C17 C16 118.2(4) . . ? C18 C17 H17 120.9 . . ? C16 C17 H17 120.9 . . ? N5 C18 C17 122.8(4) . . ? N5 C18 C19 114.5(3) . . ? C17 C18 C19 122.8(4) . . ? N7 C19 N6 113.6(3) . . ? N7 C19 C18 119.4(4) . . ? N6 C19 C18 127.0(4) . . ? N6 C20 N8 112.1(3) . . ? N6 C20 C21 123.7(4) . . ? N8 C20 C21 124.2(4) . . ? C26 C21 C22 119.1(4) . . ? C26 C21 C20 120.1(4) . . ? C22 C21 C20 120.7(4) . . ? C23 C22 C21 121.3(4) . . ? C23 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? C22 C23 C24 119.4(4) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? C23 C24 C25 120.3(4) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C24 C25 C26 120.9(4) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? O2 C26 C25 118.3(4) . . ? O2 C26 C21 122.6(4) . . ? C25 C26 C21 119.0(4) . . ? O4 C27 O3 121.3(4) . . ? O4 C27 C28 118.8(4) . . ? O3 C27 C28 119.9(3) . . ? C28 C28 C27 124.4(5) 3_676 . ? C28 C28 H28 117.8 3_676 . ? C27 C28 H28 117.8 . . ? O5 C29 H29A 109.5 . . ? O5 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O5 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N9 C30 C31 122.7(4) . . ? N9 C30 H30 118.7 . . ? C31 C30 H30 118.7 . . ? C32 C31 C30 118.8(4) . . ? C32 C31 H31 120.6 . . ? C30 C31 H31 120.6 . . ? C31 C32 C33 119.7(4) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C32 C33 C34 118.5(4) . . ? C32 C33 H33 120.7 . . ? C34 C33 H33 120.7 . . ? N9 C34 C33 122.2(4) . . ? N9 C34 C35 115.0(3) . . ? C33 C34 C35 122.8(4) . . ? N11 C35 N10 114.1(3) . . ? N11 C35 C34 119.2(3) . . ? N10 C35 C34 126.6(4) . . ? N10 C36 N12 111.7(3) . . ? N10 C36 C37 124.9(3) . . ? N12 C36 C37 123.3(4) . . ? C42 C37 C38 118.7(4) . . ? C42 C37 C36 121.1(4) . . ? C38 C37 C36 120.2(4) . . ? C39 C38 C37 121.7(4) . . ? C39 C38 H38 119.2 . . ? C37 C38 H38 119.2 . . ? C38 C39 C40 118.9(4) . . ? C38 C39 H39 120.5 . . ? C40 C39 H39 120.5 . . ? C41 C40 C39 120.9(4) . . ? C41 C40 H40 119.6 . . ? C39 C40 H40 119.6 . . ? C40 C41 C42 120.2(4) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? O8 C42 C37 123.0(4) . . ? O8 C42 C41 117.5(4) . . ? C37 C42 C41 119.5(4) . . ? N13 C43 C44 122.7(4) . . ? N13 C43 H43 118.7 . . ? C44 C43 H43 118.7 . . ? C45 C44 C43 118.5(4) . . ? C45 C44 H44 120.7 . . ? C43 C44 H44 120.7 . . ? C44 C45 C46 119.5(4) . . ? C44 C45 H45 120.2 . . ? C46 C45 H45 120.2 . . ? C45 C46 C47 119.0(4) . . ? C45 C46 H46 120.5 . . ? C47 C46 H46 120.5 . . ? N13 C47 C46 121.5(4) . . ? N13 C47 C48 114.1(3) . . ? C46 C47 C48 124.4(4) . . ? N15 C48 N14 114.2(3) . . ? N15 C48 C47 119.8(4) . . ? N14 C48 C47 125.9(4) . . ? N14 C49 N16 111.8(3) . . ? N14 C49 C50 124.3(4) . . ? N16 C49 C50 123.9(4) . . ? C55 C50 C51 119.5(4) . . ? C55 C50 C49 119.9(4) . . ? C51 C50 C49 120.5(4) . . ? C52 C51 C50 121.0(4) . . ? C52 C51 H51 119.5 . . ? C50 C51 H51 119.5 . . ? C51 C52 C53 119.5(4) . . ? C51 C52 H52 120.2 . . ? C53 C52 H52 120.2 . . ? C52 C53 C54 120.7(4) . . ? C52 C53 H53 119.7 . . ? C54 C53 H53 119.7 . . ? C53 C54 C55 120.2(4) . . ? C53 C54 H54 119.9 . . ? C55 C54 H54 119.9 . . ? O9 C55 C50 123.2(4) . . ? O9 C55 C54 117.8(4) . . ? C50 C55 C54 118.9(4) . . ? O11 C56 O10 122.3(4) . . ? O11 C56 C57 119.0(4) . . ? O10 C56 C57 118.7(4) . . ? C57 C57 C56 124.4(5) 3_665 . ? C57 C57 H57 117.8 3_665 . ? C56 C57 H57 117.8 . . ? O12 C58 H58A 109.5 . . ? O12 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? O12 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? O15 C59 H59A 109.5 . . ? O15 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? O15 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? O16 C60 H60A 109.5 . . ? O16 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? O16 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N7 Mn1 N3 85.42(12) . . ? N7 Mn1 N1 154.94(12) . . ? N3 Mn1 N1 73.21(12) . . ? N7 Mn1 N5 72.68(12) . . ? N3 Mn1 N5 151.99(12) . . ? N1 Mn1 N5 122.39(12) . . ? N7 Mn1 O3 88.18(11) . . ? N3 Mn1 O3 82.26(11) . . ? N1 Mn1 O3 101.42(11) . . ? N5 Mn1 O3 113.47(11) . . ? N7 Mn1 O4 119.72(11) . . ? N3 Mn1 O4 127.43(11) . . ? N1 Mn1 O4 84.33(11) . . ? N5 Mn1 O4 79.58(11) . . ? O3 Mn1 O4 56.09(10) . . ? N7 Mn1 O6 85.60(11) . . ? N3 Mn1 O6 82.86(11) . . ? N1 Mn1 O6 79.02(11) . . ? N5 Mn1 O6 78.34(11) . . ? O3 Mn1 O6 164.28(10) . . ? O4 Mn1 O6 138.96(10) . . ? O1 Mn2 O2 85.17(12) . . ? O1 Mn2 N4 87.66(12) . . ? O2 Mn2 N4 172.75(12) . . ? O1 Mn2 N8 171.09(13) . . ? O2 Mn2 N8 86.57(13) . . ? N4 Mn2 N8 100.65(13) . . ? O1 Mn2 O5 92.36(12) . . ? O2 Mn2 O5 91.81(12) . . ? N4 Mn2 O5 89.53(13) . . ? N8 Mn2 O5 84.56(13) . . ? O1 Mn2 O7 95.46(12) . . ? O2 Mn2 O7 94.46(12) . . ? N4 Mn2 O7 85.17(12) . . ? N8 Mn2 O7 88.50(12) . . ? O5 Mn2 O7 170.35(11) . . ? O10 Mn3 N15 89.70(11) . . ? O10 Mn3 N11 85.58(11) . . ? N15 Mn3 N11 83.75(12) . . ? O10 Mn3 N9 100.82(11) . . ? N15 Mn3 N9 154.33(12) . . ? N11 Mn3 N9 73.92(12) . . ? O10 Mn3 N13 107.89(11) . . ? N15 Mn3 N13 73.27(12) . . ? N11 Mn3 N13 152.96(12) . . ? N9 Mn3 N13 123.98(12) . . ? O10 Mn3 O13 173.52(10) . . ? N15 Mn3 O13 88.08(11) . . ? N11 Mn3 O13 88.12(11) . . ? N9 Mn3 O13 78.85(11) . . ? N13 Mn3 O13 77.27(11) . . ? O9 Mn4 O8 85.78(12) . . ? O9 Mn4 N16 86.81(13) . . ? O8 Mn4 N16 172.59(13) . . ? O9 Mn4 N12 173.31(13) . . ? O8 Mn4 N12 87.55(13) . . ? N16 Mn4 N12 99.86(13) . . ? O9 Mn4 O12 91.03(12) . . ? O8 Mn4 O12 88.53(12) . . ? N16 Mn4 O12 91.77(13) . . ? N12 Mn4 O12 89.29(12) . . ? O9 Mn4 O14 92.95(12) . . ? O8 Mn4 O14 91.37(12) . . ? N16 Mn4 O14 88.85(12) . . ? N12 Mn4 O14 86.71(12) . . ? O12 Mn4 O14 176.00(11) . . ? C1 N1 C5 117.8(4) . . ? C1 N1 Mn1 126.1(3) . . ? C5 N1 Mn1 116.0(3) . . ? C7 N2 C6 102.5(3) . . ? C6 N3 N4 105.0(3) . . ? C6 N3 Mn1 116.4(3) . . ? N4 N3 Mn1 138.2(2) . . ? C7 N4 N3 106.3(3) . . ? C7 N4 Mn2 127.5(3) . . ? N3 N4 Mn2 125.9(2) . . ? C14 N5 C18 118.0(3) . . ? C14 N5 Mn1 125.5(3) . . ? C18 N5 Mn1 116.4(3) . . ? C20 N6 C19 102.4(3) . . ? C19 N7 N8 105.2(3) . . ? C19 N7 Mn1 117.0(3) . . ? N8 N7 Mn1 137.8(2) . . ? C20 N8 N7 106.7(3) . . ? C20 N8 Mn2 126.7(3) . . ? N7 N8 Mn2 126.6(2) . . ? C30 N9 C34 118.1(3) . . ? C30 N9 Mn3 125.6(3) . . ? C34 N9 Mn3 116.2(3) . . ? C35 N10 C36 102.3(3) . . ? C35 N11 N12 105.2(3) . . ? C35 N11 Mn3 115.6(3) . . ? N12 N11 Mn3 138.7(2) . . ? C36 N12 N11 106.6(3) . . ? C36 N12 Mn4 127.2(3) . . ? N11 N12 Mn4 125.5(2) . . ? C43 N13 C47 118.7(3) . . ? C43 N13 Mn3 124.5(3) . . ? C47 N13 Mn3 116.7(3) . . ? C48 N14 C49 102.1(3) . . ? C48 N15 N16 105.4(3) . . ? C48 N15 Mn3 115.9(3) . . ? N16 N15 Mn3 138.2(2) . . ? C49 N16 N15 106.4(3) . . ? C49 N16 Mn4 127.4(3) . . ? N15 N16 Mn4 126.0(2) . . ? C13 O1 Mn2 131.5(2) . . ? C26 O2 Mn2 129.5(2) . . ? C27 O3 Mn1 91.3(2) . . ? C27 O4 Mn1 91.2(2) . . ? C29 O5 Mn2 127.8(3) . . ? C29 O5 H5 116.1 . . ? Mn2 O5 H5 116.1 . . ? Mn1 O6 H6A 120.1 . . ? Mn1 O6 H6B 119.9 . . ? H6A O6 H6B 120.0 . . ? Mn2 O7 H7A 120.0 . . ? Mn2 O7 H7B 120.1 . . ? H7A O7 H7B 120.0 . . ? C42 O8 Mn4 129.8(2) . . ? C55 O9 Mn4 130.6(2) . . ? C56 O10 Mn3 101.3(2) . . ? C58 O12 Mn4 123.0(3) . . ? C58 O12 H12A 118.5 . . ? Mn4 O12 H12A 118.5 . . ? Mn3 O13 H13A 120.0 . . ? Mn3 O13 H13B 120.0 . . ? H13A O13 H13B 120.0 . . ? Mn4 O14 H14A 119.9 . . ? Mn4 O14 H14B 120.1 . . ? H14A O14 H14B 120.0 . . ? C59 O15 H15A 109.5 . . ? C60 O16 H16A 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 N1 C1 C2 C3 -0.4(7) . . . . ? C1 C2 C3 C4 0.1(7) . . . . ? C2 C3 C4 C5 -0.4(6) . . . . ? C3 C4 C5 N1 1.0(6) . . . . ? C3 C4 C5 C6 -178.0(4) . . . . ? N1 C5 C6 N3 -4.1(5) . . . . ? C4 C5 C6 N3 174.9(4) . . . . ? N1 C5 C6 N2 176.8(4) . . . . ? C4 C5 C6 N2 -4.2(6) . . . . ? N2 C7 C8 C9 8.3(6) . . . . ? N4 C7 C8 C9 -169.3(4) . . . . ? N2 C7 C8 C13 -171.1(4) . . . . ? N4 C7 C8 C13 11.3(6) . . . . ? C13 C8 C9 C10 -1.9(6) . . . . ? C7 C8 C9 C10 178.7(4) . . . . ? C8 C9 C10 C11 -1.1(6) . . . . ? C9 C10 C11 C12 2.2(6) . . . . ? C10 C11 C12 C13 -0.3(6) . . . . ? C11 C12 C13 O1 174.3(4) . . . . ? C11 C12 C13 C8 -2.6(6) . . . . ? C9 C8 C13 O1 -173.1(4) . . . . ? C7 C8 C13 O1 6.3(6) . . . . ? C9 C8 C13 C12 3.7(6) . . . . ? C7 C8 C13 C12 -176.9(4) . . . . ? N5 C14 C15 C16 -0.2(7) . . . . ? C14 C15 C16 C17 0.3(6) . . . . ? C15 C16 C17 C18 0.5(6) . . . . ? C16 C17 C18 N5 -1.5(6) . . . . ? C16 C17 C18 C19 177.9(4) . . . . ? N5 C18 C19 N7 0.5(5) . . . . ? C17 C18 C19 N7 -178.9(4) . . . . ? N5 C18 C19 N6 179.4(4) . . . . ? C17 C18 C19 N6 0.0(6) . . . . ? N6 C20 C21 C26 166.9(4) . . . . ? N8 C20 C21 C26 -13.3(6) . . . . ? N6 C20 C21 C22 -11.1(6) . . . . ? N8 C20 C21 C22 168.7(4) . . . . ? C26 C21 C22 C23 1.7(6) . . . . ? C20 C21 C22 C23 179.7(4) . . . . ? C21 C22 C23 C24 -0.2(7) . . . . ? C22 C23 C24 C25 -0.4(7) . . . . ? C23 C24 C25 C26 -0.5(7) . . . . ? C24 C25 C26 O2 -175.3(4) . . . . ? C24 C25 C26 C21 1.9(6) . . . . ? C22 C21 C26 O2 174.6(4) . . . . ? C20 C21 C26 O2 -3.5(6) . . . . ? C22 C21 C26 C25 -2.5(6) . . . . ? C20 C21 C26 C25 179.4(4) . . . . ? O4 C27 C28 C28 -179.0(5) . . . 3_676 ? O3 C27 C28 C28 -0.4(7) . . . 3_676 ? N9 C30 C31 C32 -1.3(6) . . . . ? C30 C31 C32 C33 0.1(7) . . . . ? C31 C32 C33 C34 0.7(7) . . . . ? C32 C33 C34 N9 -0.4(6) . . . . ? C32 C33 C34 C35 176.9(4) . . . . ? N9 C34 C35 N11 -5.3(5) . . . . ? C33 C34 C35 N11 177.2(4) . . . . ? N9 C34 C35 N10 170.4(4) . . . . ? C33 C34 C35 N10 -7.1(6) . . . . ? N10 C36 C37 C42 -166.6(4) . . . . ? N12 C36 C37 C42 13.6(6) . . . . ? N10 C36 C37 C38 10.8(6) . . . . ? N12 C36 C37 C38 -169.0(4) . . . . ? C42 C37 C38 C39 -3.5(6) . . . . ? C36 C37 C38 C39 179.0(4) . . . . ? C37 C38 C39 C40 0.2(7) . . . . ? C38 C39 C40 C41 1.8(7) . . . . ? C39 C40 C41 C42 -0.6(7) . . . . ? C38 C37 C42 O8 -172.4(4) . . . . ? C36 C37 C42 O8 5.1(6) . . . . ? C38 C37 C42 C41 4.6(6) . . . . ? C36 C37 C42 C41 -177.9(4) . . . . ? C40 C41 C42 O8 174.5(4) . . . . ? C40 C41 C42 C37 -2.7(6) . . . . ? N13 C43 C44 C45 0.2(7) . . . . ? C43 C44 C45 C46 0.1(6) . . . . ? C44 C45 C46 C47 -0.2(6) . . . . ? C45 C46 C47 N13 -0.1(6) . . . . ? C45 C46 C47 C48 -179.2(4) . . . . ? N13 C47 C48 N15 5.9(5) . . . . ? C46 C47 C48 N15 -175.0(4) . . . . ? N13 C47 C48 N14 -172.4(4) . . . . ? C46 C47 C48 N14 6.7(6) . . . . ? N14 C49 C50 C55 166.7(4) . . . . ? N16 C49 C50 C55 -12.7(6) . . . . ? N14 C49 C50 C51 -9.9(6) . . . . ? N16 C49 C50 C51 170.7(4) . . . . ? C55 C50 C51 C52 2.7(7) . . . . ? C49 C50 C51 C52 179.3(4) . . . . ? C50 C51 C52 C53 0.5(7) . . . . ? C51 C52 C53 C54 -2.0(7) . . . . ? C52 C53 C54 C55 0.3(7) . . . . ? C51 C50 C55 O9 172.6(4) . . . . ? C49 C50 C55 O9 -4.0(6) . . . . ? C51 C50 C55 C54 -4.4(6) . . . . ? C49 C50 C55 C54 179.0(4) . . . . ? C53 C54 C55 O9 -174.3(4) . . . . ? C53 C54 C55 C50 2.9(7) . . . . ? O11 C56 C57 C57 -177.9(5) . . . 3_665 ? O10 C56 C57 C57 0.8(7) . . . 3_665 ? C2 C1 N1 C5 0.9(6) . . . . ? C2 C1 N1 Mn1 178.0(3) . . . . ? C4 C5 N1 C1 -1.2(6) . . . . ? C6 C5 N1 C1 177.8(3) . . . . ? C4 C5 N1 Mn1 -178.6(3) . . . . ? C6 C5 N1 Mn1 0.5(4) . . . . ? N7 Mn1 N1 C1 -142.7(3) . . . . ? N3 Mn1 N1 C1 -175.3(3) . . . . ? N5 Mn1 N1 C1 -21.1(4) . . . . ? O3 Mn1 N1 C1 106.4(3) . . . . ? O4 Mn1 N1 C1 52.7(3) . . . . ? O6 Mn1 N1 C1 -89.6(3) . . . . ? N7 Mn1 N1 C5 34.4(4) . . . . ? N3 Mn1 N1 C5 1.7(3) . . . . ? N5 Mn1 N1 C5 156.0(3) . . . . ? O3 Mn1 N1 C5 -76.5(3) . . . . ? O4 Mn1 N1 C5 -130.2(3) . . . . ? O6 Mn1 N1 C5 87.5(3) . . . . ? N4 C7 N2 C6 -1.1(4) . . . . ? C8 C7 N2 C6 -178.9(4) . . . . ? N3 C6 N2 C7 1.0(4) . . . . ? C5 C6 N2 C7 -179.9(4) . . . . ? N2 C6 N3 N4 -0.6(4) . . . . ? C5 C6 N3 N4 -179.7(3) . . . . ? N2 C6 N3 Mn1 -175.0(3) . . . . ? C5 C6 N3 Mn1 5.8(5) . . . . ? N7 Mn1 N3 C6 -170.7(3) . . . . ? N1 Mn1 N3 C6 -4.0(3) . . . . ? N5 Mn1 N3 C6 -132.6(3) . . . . ? O3 Mn1 N3 C6 100.5(3) . . . . ? O4 Mn1 N3 C6 64.9(3) . . . . ? O6 Mn1 N3 C6 -84.6(3) . . . . ? N7 Mn1 N3 N4 17.3(4) . . . . ? N1 Mn1 N3 N4 -175.9(4) . . . . ? N5 Mn1 N3 N4 55.4(5) . . . . ? O3 Mn1 N3 N4 -71.5(4) . . . . ? O4 Mn1 N3 N4 -107.1(4) . . . . ? O6 Mn1 N3 N4 103.4(4) . . . . ? N2 C7 N4 N3 0.8(4) . . . . ? C8 C7 N4 N3 178.6(3) . . . . ? N2 C7 N4 Mn2 174.4(3) . . . . ? C8 C7 N4 Mn2 -7.8(6) . . . . ? C6 N3 N4 C7 -0.2(4) . . . . ? Mn1 N3 N4 C7 172.4(3) . . . . ? C6 N3 N4 Mn2 -173.9(3) . . . . ? Mn1 N3 N4 Mn2 -1.3(5) . . . . ? O1 Mn2 N4 C7 -7.2(3) . . . . ? O2 Mn2 N4 C7 -15.5(12) . . . . ? N8 Mn2 N4 C7 169.5(3) . . . . ? O5 Mn2 N4 C7 85.1(3) . . . . ? O7 Mn2 N4 C7 -102.9(3) . . . . ? O1 Mn2 N4 N3 165.1(3) . . . . ? O2 Mn2 N4 N3 156.9(9) . . . . ? N8 Mn2 N4 N3 -18.1(3) . . . . ? O5 Mn2 N4 N3 -102.5(3) . . . . ? O7 Mn2 N4 N3 69.5(3) . . . . ? C15 C14 N5 C18 -0.7(6) . . . . ? C15 C14 N5 Mn1 -179.9(3) . . . . ? C17 C18 N5 C14 1.5(6) . . . . ? C19 C18 N5 C14 -177.9(3) . . . . ? C17 C18 N5 Mn1 -179.1(3) . . . . ? C19 C18 N5 Mn1 1.5(4) . . . . ? N7 Mn1 N5 C14 177.3(3) . . . . ? N3 Mn1 N5 C14 137.2(3) . . . . ? N1 Mn1 N5 C14 19.5(4) . . . . ? O3 Mn1 N5 C14 -102.5(3) . . . . ? O4 Mn1 N5 C14 -56.8(3) . . . . ? O6 Mn1 N5 C14 88.4(3) . . . . ? N7 Mn1 N5 C18 -2.0(3) . . . . ? N3 Mn1 N5 C18 -42.1(4) . . . . ? N1 Mn1 N5 C18 -159.8(3) . . . . ? O3 Mn1 N5 C18 78.2(3) . . . . ? O4 Mn1 N5 C18 123.9(3) . . . . ? O6 Mn1 N5 C18 -90.9(3) . . . . ? N8 C20 N6 C19 0.1(4) . . . . ? C21 C20 N6 C19 179.9(4) . . . . ? N7 C19 N6 C20 0.3(4) . . . . ? C18 C19 N6 C20 -178.7(4) . . . . ? N6 C19 N7 N8 -0.5(4) . . . . ? C18 C19 N7 N8 178.5(3) . . . . ? N6 C19 N7 Mn1 178.6(2) . . . . ? C18 C19 N7 Mn1 -2.3(5) . . . . ? N3 Mn1 N7 C19 164.5(3) . . . . ? N1 Mn1 N7 C19 133.3(3) . . . . ? N5 Mn1 N7 C19 2.2(3) . . . . ? O3 Mn1 N7 C19 -113.1(3) . . . . ? O4 Mn1 N7 C19 -64.5(3) . . . . ? O6 Mn1 N7 C19 81.3(3) . . . . ? N3 Mn1 N7 N8 -16.7(4) . . . . ? N1 Mn1 N7 N8 -47.9(5) . . . . ? N5 Mn1 N7 N8 -179.0(4) . . . . ? O3 Mn1 N7 N8 65.7(4) . . . . ? O4 Mn1 N7 N8 114.3(3) . . . . ? O6 Mn1 N7 N8 -99.9(4) . . . . ? N6 C20 N8 N7 -0.4(4) . . . . ? C21 C20 N8 N7 179.7(4) . . . . ? N6 C20 N8 Mn2 -179.0(3) . . . . ? C21 C20 N8 Mn2 1.1(6) . . . . ? C19 N7 N8 C20 0.6(4) . . . . ? Mn1 N7 N8 C20 -178.3(3) . . . . ? C19 N7 N8 Mn2 179.2(3) . . . . ? Mn1 N7 N8 Mn2 0.3(5) . . . . ? O1 Mn2 N8 C20 -4.4(10) . . . . ? O2 Mn2 N8 C20 17.7(3) . . . . ? N4 Mn2 N8 C20 -163.0(3) . . . . ? O5 Mn2 N8 C20 -74.5(3) . . . . ? O7 Mn2 N8 C20 112.2(3) . . . . ? O1 Mn2 N8 N7 177.3(7) . . . . ? O2 Mn2 N8 N7 -160.7(3) . . . . ? N4 Mn2 N8 N7 18.6(3) . . . . ? O5 Mn2 N8 N7 107.1(3) . . . . ? O7 Mn2 N8 N7 -66.2(3) . . . . ? C31 C30 N9 C34 1.6(6) . . . . ? C31 C30 N9 Mn3 179.0(3) . . . . ? C33 C34 N9 C30 -0.7(6) . . . . ? C35 C34 N9 C30 -178.2(3) . . . . ? C33 C34 N9 Mn3 -178.3(3) . . . . ? C35 C34 N9 Mn3 4.2(4) . . . . ? O10 Mn3 N9 C30 98.6(3) . . . . ? N15 Mn3 N9 C30 -148.7(3) . . . . ? N11 Mn3 N9 C30 -179.2(3) . . . . ? N13 Mn3 N9 C30 -21.8(4) . . . . ? O13 Mn3 N9 C30 -88.0(3) . . . . ? O10 Mn3 N9 C34 -83.9(3) . . . . ? N15 Mn3 N9 C34 28.7(4) . . . . ? N11 Mn3 N9 C34 -1.8(3) . . . . ? N13 Mn3 N9 C34 155.7(3) . . . . ? O13 Mn3 N9 C34 89.5(3) . . . . ? N11 C35 N10 C36 0.7(4) . . . . ? C34 C35 N10 C36 -175.3(4) . . . . ? N12 C36 N10 C35 -1.7(4) . . . . ? C37 C36 N10 C35 178.5(4) . . . . ? N10 C35 N11 N12 0.5(4) . . . . ? C34 C35 N11 N12 176.8(3) . . . . ? N10 C35 N11 Mn3 -172.5(2) . . . . ? C34 C35 N11 Mn3 3.7(4) . . . . ? O10 Mn3 N11 C35 101.5(3) . . . . ? N15 Mn3 N11 C35 -168.3(3) . . . . ? N9 Mn3 N11 C35 -1.1(3) . . . . ? N13 Mn3 N11 C35 -136.7(3) . . . . ? O13 Mn3 N11 C35 -80.0(3) . . . . ? O10 Mn3 N11 N12 -68.3(4) . . . . ? N15 Mn3 N11 N12 21.9(4) . . . . ? N9 Mn3 N11 N12 -170.9(4) . . . . ? N13 Mn3 N11 N12 53.4(5) . . . . ? O13 Mn3 N11 N12 110.1(4) . . . . ? N10 C36 N12 N11 2.1(4) . . . . ? C37 C36 N12 N11 -178.1(3) . . . . ? N10 C36 N12 Mn4 173.5(2) . . . . ? C37 C36 N12 Mn4 -6.6(6) . . . . ? C35 N11 N12 C36 -1.5(4) . . . . ? Mn3 N11 N12 C36 169.0(3) . . . . ? C35 N11 N12 Mn4 -173.1(3) . . . . ? Mn3 N11 N12 Mn4 -2.6(5) . . . . ? O9 Mn4 N12 C36 -15.1(13) . . . . ? O8 Mn4 N12 C36 -10.9(3) . . . . ? N16 Mn4 N12 C36 169.3(3) . . . . ? O12 Mn4 N12 C36 77.6(3) . . . . ? O14 Mn4 N12 C36 -102.4(3) . . . . ? O9 Mn4 N12 N11 154.8(10) . . . . ? O8 Mn4 N12 N11 159.0(3) . . . . ? N16 Mn4 N12 N11 -20.8(3) . . . . ? O12 Mn4 N12 N11 -112.4(3) . . . . ? O14 Mn4 N12 N11 67.5(3) . . . . ? C44 C43 N13 C47 -0.4(6) . . . . ? C44 C43 N13 Mn3 -176.3(3) . . . . ? C46 C47 N13 C43 0.4(6) . . . . ? C48 C47 N13 C43 179.6(3) . . . . ? C46 C47 N13 Mn3 176.5(3) . . . . ? C48 C47 N13 Mn3 -4.3(4) . . . . ? O10 Mn3 N13 C43 -98.3(3) . . . . ? N15 Mn3 N13 C43 177.6(3) . . . . ? N11 Mn3 N13 C43 144.6(3) . . . . ? N9 Mn3 N13 C43 18.8(4) . . . . ? O13 Mn3 N13 C43 85.7(3) . . . . ? O10 Mn3 N13 C47 85.7(3) . . . . ? N15 Mn3 N13 C47 1.6(3) . . . . ? N11 Mn3 N13 C47 -31.3(4) . . . . ? N9 Mn3 N13 C47 -157.1(3) . . . . ? O13 Mn3 N13 C47 -90.2(3) . . . . ? N15 C48 N14 C49 -1.8(4) . . . . ? C47 C48 N14 C49 176.6(4) . . . . ? N16 C49 N14 C48 2.1(4) . . . . ? C50 C49 N14 C48 -177.4(4) . . . . ? N14 C48 N15 N16 0.8(4) . . . . ? C47 C48 N15 N16 -177.7(3) . . . . ? N14 C48 N15 Mn3 174.0(2) . . . . ? C47 C48 N15 Mn3 -4.5(5) . . . . ? O10 Mn3 N15 C48 -107.3(3) . . . . ? N11 Mn3 N15 C48 167.1(3) . . . . ? N9 Mn3 N15 C48 137.7(3) . . . . ? N13 Mn3 N15 C48 1.5(3) . . . . ? O13 Mn3 N15 C48 78.8(3) . . . . ? O10 Mn3 N15 N16 62.9(4) . . . . ? N11 Mn3 N15 N16 -22.7(4) . . . . ? N9 Mn3 N15 N16 -52.1(5) . . . . ? N13 Mn3 N15 N16 171.7(4) . . . . ? O13 Mn3 N15 N16 -111.0(4) . . . . ? N14 C49 N16 N15 -1.7(4) . . . . ? C50 C49 N16 N15 177.8(4) . . . . ? N14 C49 N16 Mn4 -176.1(3) . . . . ? C50 C49 N16 Mn4 3.4(6) . . . . ? C48 N15 N16 C49 0.5(4) . . . . ? Mn3 N15 N16 C49 -170.3(3) . . . . ? C48 N15 N16 Mn4 175.0(3) . . . . ? Mn3 N15 N16 Mn4 4.2(5) . . . . ? O9 Mn4 N16 C49 14.0(3) . . . . ? O8 Mn4 N16 C49 15.2(12) . . . . ? N12 Mn4 N16 C49 -166.6(3) . . . . ? O12 Mn4 N16 C49 -77.0(3) . . . . ? O14 Mn4 N16 C49 107.0(3) . . . . ? O9 Mn4 N16 N15 -159.4(3) . . . . ? O8 Mn4 N16 N15 -158.1(9) . . . . ? N12 Mn4 N16 N15 20.1(3) . . . . ? O12 Mn4 N16 N15 109.7(3) . . . . ? O14 Mn4 N16 N15 -66.4(3) . . . . ? C12 C13 O1 Mn2 153.4(3) . . . . ? C8 C13 O1 Mn2 -29.7(6) . . . . ? O2 Mn2 O1 C13 -154.8(3) . . . . ? N4 Mn2 O1 C13 26.2(3) . . . . ? N8 Mn2 O1 C13 -132.8(8) . . . . ? O5 Mn2 O1 C13 -63.2(3) . . . . ? O7 Mn2 O1 C13 111.1(3) . . . . ? C25 C26 O2 Mn2 -147.8(3) . . . . ? C21 C26 O2 Mn2 35.1(5) . . . . ? O1 Mn2 O2 C26 140.6(3) . . . . ? N4 Mn2 O2 C26 148.9(9) . . . . ? N8 Mn2 O2 C26 -36.1(3) . . . . ? O5 Mn2 O2 C26 48.4(3) . . . . ? O7 Mn2 O2 C26 -124.3(3) . . . . ? O4 C27 O3 Mn1 3.2(4) . . . . ? C28 C27 O3 Mn1 -175.3(3) . . . . ? N7 Mn1 O3 C27 126.5(2) . . . . ? N3 Mn1 O3 C27 -147.9(2) . . . . ? N1 Mn1 O3 C27 -76.8(2) . . . . ? N5 Mn1 O3 C27 56.3(2) . . . . ? O4 Mn1 O3 C27 -1.7(2) . . . . ? O6 Mn1 O3 C27 -166.9(3) . . . . ? O3 C27 O4 Mn1 -3.2(4) . . . . ? C28 C27 O4 Mn1 175.4(3) . . . . ? N7 Mn1 O4 C27 -62.9(3) . . . . ? N3 Mn1 O4 C27 45.8(3) . . . . ? N1 Mn1 O4 C27 109.6(2) . . . . ? N5 Mn1 O4 C27 -125.9(2) . . . . ? O3 Mn1 O4 C27 1.8(2) . . . . ? O6 Mn1 O4 C27 175.7(2) . . . . ? O1 Mn2 O5 C29 -17.1(5) . . . . ? O2 Mn2 O5 C29 68.2(5) . . . . ? N4 Mn2 O5 C29 -104.7(5) . . . . ? N8 Mn2 O5 C29 154.5(5) . . . . ? O7 Mn2 O5 C29 -161.3(7) . . . . ? C37 C42 O8 Mn4 -32.8(6) . . . . ? C41 C42 O8 Mn4 150.2(3) . . . . ? O9 Mn4 O8 C42 -149.8(3) . . . . ? N16 Mn4 O8 C42 -151.1(9) . . . . ? N12 Mn4 O8 C42 30.7(3) . . . . ? O12 Mn4 O8 C42 -58.7(3) . . . . ? O14 Mn4 O8 C42 117.3(3) . . . . ? C50 C55 O9 Mn4 32.7(6) . . . . ? C54 C55 O9 Mn4 -150.2(3) . . . . ? O8 Mn4 O9 C55 147.8(4) . . . . ? N16 Mn4 O9 C55 -32.3(3) . . . . ? N12 Mn4 O9 C55 152.1(10) . . . . ? O12 Mn4 O9 C55 59.4(3) . . . . ? O14 Mn4 O9 C55 -121.0(3) . . . . ? O11 C56 O10 Mn3 5.1(4) . . . . ? C57 C56 O10 Mn3 -173.6(3) . . . . ? N15 Mn3 O10 C56 129.1(2) . . . . ? N11 Mn3 O10 C56 -147.1(2) . . . . ? N9 Mn3 O10 C56 -74.4(2) . . . . ? N13 Mn3 O10 C56 56.9(3) . . . . ? O13 Mn3 O10 C56 -160.9(8) . . . . ? O9 Mn4 O12 C58 34.5(3) . . . . ? O8 Mn4 O12 C58 -51.3(3) . . . . ? N16 Mn4 O12 C58 121.3(3) . . . . ? N12 Mn4 O12 C58 -138.8(3) . . . . ? O14 Mn4 O12 C58 -139.8(15) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.807 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.083 # Attachment '3.cif' data_shelxl2 _database_code_depnum_ccdc_archive 'CCDC 690528' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30.50 H34.50 Cl Mn2 N9.50 O7.50' _chemical_formula_weight 799.51 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 38.349(8) _cell_length_b 16.357(4) _cell_length_c 10.909(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.620(3) _cell_angle_gamma 90.00 _cell_volume 6810(3) _cell_formula_units_Z 8 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3288 _exptl_absorpt_coefficient_mu 0.883 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8431 _exptl_absorpt_correction_T_max 0.8431 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20652 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5995 _reflns_number_gt 5284 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0455P)^2^+8.2143P] 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 5995 _refine_ls_number_parameters 511 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.0958 _refine_ls_wR_factor_gt 0.0913 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.146922(9) 0.24017(2) 0.68405(3) 0.01341(11) Uani 1 1 d . . . Mn2 Mn 0.080773(10) 0.25745(2) 0.35136(4) 0.01815(12) Uani 1 1 d . A . Cl1 Cl 0.02877(2) 0.27748(5) 0.45996(7) 0.0384(2) Uani 1 1 d . . . O1 O 0.15215(4) 0.16499(10) 0.81549(15) 0.0171(4) Uani 1 1 d . A . O2 O 0.16625(5) 0.32018(10) 0.79742(15) 0.0189(4) Uani 1 1 d . A . O3 O 0.11487(6) 0.24902(13) 0.1942(2) 0.0334(5) Uani 1 1 d D . . N1 N 0.10794(5) 0.02356(13) 0.51930(19) 0.0174(5) Uani 1 1 d . A . N2 N 0.12667(5) 0.14832(13) 0.57724(19) 0.0179(5) Uani 1 1 d . A . N3 N 0.10493(5) 0.15703(13) 0.47058(19) 0.0191(5) Uani 1 1 d . . . N4 N 0.05971(5) 0.13824(13) 0.26989(19) 0.0191(5) Uani 1 1 d . . . N5 N 0.14646(5) 0.45717(12) 0.48070(18) 0.0158(4) Uani 1 1 d . A . N6 N 0.14321(5) 0.33027(12) 0.55571(18) 0.0148(4) Uani 1 1 d . A . N7 N 0.11865(5) 0.33662(13) 0.45548(18) 0.0161(4) Uani 1 1 d . . . N8 N 0.07306(6) 0.38588(13) 0.26838(19) 0.0205(5) Uani 1 1 d . . . C1 C 0.16021(6) 0.08509(15) 0.8117(2) 0.0163(5) Uani 1 1 d . . . C2 C 0.17946(6) 0.05129(16) 0.9146(2) 0.0189(5) Uani 1 1 d . A . H2 H 0.1886 0.0860 0.9799 0.023 Uiso 1 1 calc R . . C3 C 0.18546(6) -0.03203(16) 0.9229(2) 0.0206(6) Uani 1 1 d . . . H3 H 0.1982 -0.0542 0.9944 0.025 Uiso 1 1 calc R A . C4 C 0.17301(7) -0.08325(16) 0.8273(2) 0.0218(6) Uani 1 1 d . A . H4 H 0.1769 -0.1406 0.8332 0.026 Uiso 1 1 calc R . . C5 C 0.15483(7) -0.04985(16) 0.7229(2) 0.0199(6) Uani 1 1 d . . . H5 H 0.1468 -0.0848 0.6566 0.024 Uiso 1 1 calc R A . C6 C 0.14813(6) 0.03368(15) 0.7131(2) 0.0168(5) Uani 1 1 d . A . C7 C 0.12781(6) 0.06759(15) 0.6042(2) 0.0168(5) Uani 1 1 d . . . C8 C 0.09466(6) 0.08164(15) 0.4401(2) 0.0179(5) Uani 1 1 d . A . C9 C 0.07085(6) 0.06872(16) 0.3277(2) 0.0180(5) Uani 1 1 d . A . C10 C 0.06054(7) -0.00810(16) 0.2839(2) 0.0232(6) Uani 1 1 d . . . H10 H 0.0686 -0.0562 0.3265 0.028 Uiso 1 1 calc R A . C11 C 0.03819(8) -0.01271(18) 0.1766(3) 0.0291(7) Uani 1 1 d . A . H11 H 0.0311 -0.0644 0.1433 0.035 Uiso 1 1 calc R . . C12 C 0.02635(7) 0.05818(18) 0.1185(3) 0.0282(6) Uani 1 1 d . . . H12 H 0.0107 0.0560 0.0455 0.034 Uiso 1 1 calc R A . C13 C 0.03755(7) 0.13211(17) 0.1677(2) 0.0227(6) Uani 1 1 d . A . H13 H 0.0292 0.1808 0.1275 0.027 Uiso 1 1 calc R . . C14 C 0.18997(6) 0.37654(15) 0.7731(2) 0.0169(5) Uani 1 1 d . . . C15 C 0.21803(7) 0.39297(17) 0.8618(2) 0.0233(6) Uani 1 1 d . A . H15 H 0.2200 0.3639 0.9376 0.028 Uiso 1 1 calc R . . C16 C 0.24276(7) 0.45086(17) 0.8402(3) 0.0261(6) Uani 1 1 d . . . H16 H 0.2616 0.4611 0.9013 0.031 Uiso 1 1 calc R A . C17 C 0.24057(7) 0.49436(17) 0.7312(2) 0.0234(6) Uani 1 1 d . A . H17 H 0.2579 0.5337 0.7167 0.028 Uiso 1 1 calc R . . C18 C 0.21278(6) 0.47986(16) 0.6435(2) 0.0198(6) Uani 1 1 d . . . H18 H 0.2108 0.5105 0.5692 0.024 Uiso 1 1 calc R A . C19 C 0.18751(6) 0.42055(15) 0.6625(2) 0.0150(5) Uani 1 1 d . A . C20 C 0.15916(6) 0.40403(15) 0.5674(2) 0.0145(5) Uani 1 1 d . . . C21 C 0.12162(6) 0.41268(15) 0.4146(2) 0.0150(5) Uani 1 1 d . A . C22 C 0.09761(6) 0.44125(15) 0.3095(2) 0.0164(5) Uani 1 1 d . A . C23 C 0.09937(7) 0.51862(16) 0.2588(2) 0.0195(6) Uani 1 1 d . . . H23 H 0.1170 0.5562 0.2895 0.023 Uiso 1 1 calc R A . C24 C 0.07480(7) 0.54002(17) 0.1618(2) 0.0239(6) Uani 1 1 d . A . H24 H 0.0754 0.5924 0.1246 0.029 Uiso 1 1 calc R . . C25 C 0.04952(8) 0.48384(18) 0.1207(3) 0.0285(7) Uani 1 1 d . . . H25 H 0.0324 0.4971 0.0546 0.034 Uiso 1 1 calc R A . C26 C 0.04928(7) 0.40815(18) 0.1765(2) 0.0274(6) Uani 1 1 d . A . H26 H 0.0315 0.3703 0.1486 0.033 Uiso 1 1 calc R . . C27 C 0.28684(8) 0.2093(2) 0.8031(3) 0.0378(8) Uani 1 1 d . . . H27A H 0.2761 0.2286 0.8758 0.057 Uiso 1 1 calc R . . H27B H 0.3039 0.2498 0.7799 0.057 Uiso 1 1 calc R . . H27C H 0.2988 0.1572 0.8221 0.057 Uiso 1 1 calc R . . C28 C 0.27100(8) 0.1696(2) 0.5850(3) 0.0350(8) Uani 1 1 d . . . H28A H 0.2505 0.1582 0.5266 0.052 Uiso 1 1 calc R . . H28B H 0.2849 0.1196 0.5993 0.052 Uiso 1 1 calc R . . H28C H 0.2854 0.2120 0.5510 0.052 Uiso 1 1 calc R . . C29 C 0.22624(7) 0.21000(16) 0.7163(2) 0.0186(5) Uani 1 1 d . . . H29 H 0.2208 0.2249 0.7965 0.022 Uiso 1 1 calc R A . N9 N 0.25950(5) 0.19781(14) 0.7006(2) 0.0239(5) Uani 1 1 d . A . O4 O 0.20134(4) 0.20361(11) 0.63468(16) 0.0190(4) Uani 1 1 d . A . O8 O 0.08987(16) 0.2594(3) 0.7024(5) 0.0213(11) Uani 0.50 1 d P A 1 O9 O 0.06993(13) 0.3031(3) 0.9222(4) 0.0478(13) Uani 0.50 1 d P A 1 C30 C 0.00529(19) 0.2393(4) 0.7583(11) 0.046(2) Uani 0.50 1 d PDU A -1 C31 C 0.04524(16) 0.3262(4) 0.8938(5) 0.0344(15) Uani 0.50 1 d PD A -1 C32 C 0.06823(14) 0.2475(3) 0.7274(5) 0.0216(12) Uani 0.50 1 d PD A -1 N10 N 0.04051(11) 0.2694(2) 0.7894(4) 0.0267(11) Uani 0.50 1 d PD A -1 O5 O 0.09741(14) 0.2768(3) 0.7519(5) 0.0219(12) Uani 0.50 1 d PD A -1 O6 O 0.13917(5) 0.36558(12) 0.02803(18) 0.0275(5) Uani 1 1 d D . . O7 O 0.10158(5) 0.14970(12) 0.99096(18) 0.0259(4) Uani 1 1 d D . . H7A H 0.1021(8) 0.0983(7) 1.000(3) 0.037(9) Uiso 1 1 d D . . H6A H 0.1418(9) 0.4168(7) 0.022(3) 0.044(10) Uiso 1 1 d D . . H3B H 0.1223(8) 0.2921(13) 0.162(3) 0.043(10) Uiso 1 1 d D . . H3A H 0.1093(9) 0.2157(19) 0.136(2) 0.055(12) Uiso 1 1 d D . . H7B H 0.1178(8) 0.158(3) 0.945(3) 0.083 Uiso 1 1 d D . . H6B H 0.1479(11) 0.348(3) -0.035(2) 0.083 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 0.0148(2) 0.0109(2) 0.0143(2) 0.00094(14) 0.00031(15) -0.00051(14) Mn2 0.0201(2) 0.0129(2) 0.0198(2) 0.00206(15) -0.00607(16) -0.00391(15) Cl1 0.0426(5) 0.0394(5) 0.0358(4) -0.0113(3) 0.0165(3) -0.0109(4) O1 0.0236(9) 0.0121(9) 0.0157(9) 0.0006(7) 0.0019(7) 0.0013(7) O2 0.0293(10) 0.0138(9) 0.0137(9) -0.0023(7) 0.0030(7) -0.0029(8) O3 0.0575(15) 0.0171(12) 0.0277(12) -0.0037(9) 0.0150(11) -0.0102(10) N1 0.0192(11) 0.0147(11) 0.0177(11) 0.0004(8) -0.0012(9) -0.0021(9) N2 0.0185(11) 0.0148(12) 0.0190(11) 0.0019(9) -0.0055(9) -0.0030(9) N3 0.0209(11) 0.0146(12) 0.0198(11) 0.0013(9) -0.0078(9) -0.0031(9) N4 0.0197(11) 0.0198(12) 0.0168(11) 0.0016(9) -0.0029(9) -0.0044(9) N5 0.0176(11) 0.0121(11) 0.0173(11) 0.0003(8) -0.0013(9) -0.0015(8) N6 0.0155(10) 0.0129(11) 0.0154(10) 0.0006(8) -0.0010(8) -0.0009(8) N7 0.0181(11) 0.0140(11) 0.0153(11) 0.0013(8) -0.0036(9) -0.0011(9) N8 0.0239(12) 0.0161(12) 0.0203(11) 0.0006(9) -0.0041(9) -0.0011(9) C1 0.0149(12) 0.0139(13) 0.0205(13) 0.0039(10) 0.0042(10) -0.0010(10) C2 0.0182(13) 0.0184(14) 0.0197(13) -0.0010(10) -0.0004(10) -0.0014(10) C3 0.0169(13) 0.0216(15) 0.0222(14) 0.0047(11) -0.0034(11) 0.0029(11) C4 0.0242(14) 0.0150(14) 0.0260(14) 0.0029(11) 0.0009(11) 0.0049(11) C5 0.0245(14) 0.0150(14) 0.0196(13) -0.0008(10) -0.0012(11) 0.0001(11) C6 0.0154(12) 0.0160(14) 0.0187(13) 0.0026(10) -0.0002(10) -0.0001(10) C7 0.0189(13) 0.0136(14) 0.0177(13) 0.0005(10) 0.0007(10) -0.0009(10) C8 0.0187(13) 0.0141(13) 0.0203(13) 0.0017(10) -0.0017(11) -0.0029(10) C9 0.0174(13) 0.0175(14) 0.0189(13) 0.0018(10) 0.0004(10) -0.0037(10) C10 0.0290(15) 0.0158(14) 0.0239(14) 0.0024(11) -0.0022(12) -0.0048(11) C11 0.0363(17) 0.0188(16) 0.0297(16) -0.0028(12) -0.0098(13) -0.0093(12) C12 0.0325(16) 0.0279(17) 0.0217(14) 0.0001(12) -0.0104(12) -0.0076(13) C13 0.0259(15) 0.0211(15) 0.0202(14) 0.0021(11) -0.0024(11) -0.0041(11) C14 0.0199(13) 0.0106(13) 0.0201(13) -0.0031(10) 0.0010(10) 0.0012(10) C15 0.0332(16) 0.0175(14) 0.0177(13) -0.0015(11) -0.0047(12) 0.0041(12) C16 0.0215(14) 0.0247(16) 0.0294(15) -0.0092(12) -0.0115(12) 0.0017(12) C17 0.0193(13) 0.0203(15) 0.0305(15) -0.0074(12) 0.0014(11) -0.0049(11) C18 0.0201(13) 0.0187(14) 0.0210(14) -0.0014(11) 0.0032(11) -0.0022(11) C19 0.0155(12) 0.0140(13) 0.0156(12) -0.0008(10) 0.0017(10) 0.0013(10) C20 0.0152(12) 0.0130(13) 0.0157(12) -0.0003(10) 0.0027(10) -0.0012(10) C21 0.0178(13) 0.0114(13) 0.0154(12) 0.0001(10) 0.0003(10) 0.0001(10) C22 0.0167(13) 0.0142(13) 0.0181(13) -0.0007(10) 0.0009(10) 0.0003(10) C23 0.0239(14) 0.0148(14) 0.0194(13) -0.0013(10) -0.0004(11) -0.0019(11) C24 0.0317(15) 0.0168(15) 0.0221(14) 0.0023(11) -0.0022(12) 0.0016(11) C25 0.0330(16) 0.0257(16) 0.0239(15) 0.0051(12) -0.0117(12) -0.0005(13) C26 0.0292(15) 0.0251(16) 0.0247(15) 0.0025(12) -0.0125(12) -0.0053(12) C27 0.0229(16) 0.039(2) 0.048(2) 0.0151(15) -0.0128(14) -0.0037(14) C28 0.0304(16) 0.0364(19) 0.0408(18) 0.0134(14) 0.0168(14) 0.0109(14) C29 0.0210(14) 0.0130(13) 0.0216(14) 0.0014(10) 0.0005(11) 0.0001(10) N9 0.0165(12) 0.0238(13) 0.0311(13) 0.0058(10) 0.0010(10) 0.0011(9) O4 0.0175(9) 0.0187(10) 0.0209(9) -0.0010(7) 0.0013(8) 0.0012(7) O8 0.017(3) 0.021(3) 0.027(3) -0.005(2) 0.006(2) -0.001(2) O9 0.041(3) 0.079(4) 0.024(2) -0.015(2) 0.008(2) 0.000(3) C30 0.019(6) 0.067(4) 0.046(4) -0.019(5) -0.020(4) -0.007(3) C31 0.026(3) 0.044(4) 0.035(4) -0.018(3) 0.012(3) -0.003(3) C32 0.021(3) 0.019(3) 0.025(3) 0.010(2) 0.003(3) 0.008(2) N10 0.021(2) 0.029(3) 0.030(3) -0.004(2) 0.007(2) -0.001(2) O5 0.022(3) 0.013(3) 0.031(3) -0.003(2) 0.002(2) -0.0025(19) O6 0.0408(12) 0.0149(11) 0.0281(11) 0.0001(8) 0.0098(9) -0.0032(9) O7 0.0389(12) 0.0135(11) 0.0261(11) -0.0011(8) 0.0074(9) 0.0008(9) _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 1.8847(17) . ? Mn1 O2 1.9006(17) . ? Mn1 N2 2.010(2) . ? Mn1 N6 2.028(2) . ? Mn1 O5 2.188(6) . ? Mn1 O8 2.239(6) . ? Mn1 O4 2.2854(17) . ? Mn2 N7 2.180(2) . ? Mn2 N3 2.239(2) . ? Mn2 N4 2.259(2) . ? Mn2 O3 2.260(2) . ? Mn2 N8 2.295(2) . ? Mn2 Cl1 2.4395(9) . ? O1 C1 1.345(3) . ? O2 C14 1.340(3) . ? O3 H3B 0.849(10) . ? O3 H3A 0.848(10) . ? N1 C7 1.348(3) . ? N1 C8 1.350(3) . ? N2 C7 1.353(3) . ? N2 N3 1.371(3) . ? N3 C8 1.327(3) . ? N4 C13 1.338(3) . ? N4 C9 1.349(3) . ? N5 C20 1.341(3) . ? N5 C21 1.350(3) . ? N6 C20 1.353(3) . ? N6 N7 1.375(3) . ? N7 C21 1.330(3) . ? N8 C26 1.338(3) . ? N8 C22 1.351(3) . ? C1 C2 1.396(4) . ? C1 C6 1.408(4) . ? C2 C3 1.384(4) . ? C2 H2 0.9500 . ? C3 C4 1.385(4) . ? C3 H3 0.9500 . ? C4 C5 1.388(4) . ? C4 H4 0.9500 . ? C5 C6 1.393(4) . ? C5 H5 0.9500 . ? C6 C7 1.464(3) . ? C8 C9 1.471(3) . ? C9 C10 1.388(4) . ? C10 C11 1.384(4) . ? C10 H10 0.9500 . ? C11 C12 1.377(4) . ? C11 H11 0.9500 . ? C12 C13 1.375(4) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C19 1.400(3) . ? C14 C15 1.401(4) . ? C15 C16 1.377(4) . ? C15 H15 0.9500 . ? C16 C17 1.382(4) . ? C16 H16 0.9500 . ? C17 C18 1.381(4) . ? C17 H17 0.9500 . ? C18 C19 1.401(3) . ? C18 H18 0.9500 . ? C19 C20 1.453(3) . ? C21 C22 1.474(3) . ? C22 C23 1.386(4) . ? C23 C24 1.391(4) . ? C23 H23 0.9500 . ? C24 C25 1.379(4) . ? C24 H24 0.9500 . ? C25 C26 1.380(4) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 N9 1.468(4) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 N9 1.451(4) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 O4 1.245(3) . ? C29 N9 1.319(3) . ? C29 H29 0.9500 . ? O8 O5 0.653(5) . ? O8 C32 0.920(7) . ? O9 C31 1.038(7) . ? O9 N10 1.832(6) . ? C30 N10 1.446(7) . ? C31 N10 1.468(6) . ? C32 O5 1.223(7) . ? C32 N10 1.362(6) . ? O6 H6A 0.848(10) . ? O6 H6B 0.848(10) . ? O7 H7A 0.846(10) . ? O7 H7B 0.848(10) . ? 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 87.05(8) . . ? O1 Mn1 N2 87.68(8) . . ? O2 Mn1 N2 174.72(8) . . ? O1 Mn1 N6 173.91(8) . . ? O2 Mn1 N6 86.87(8) . . ? N2 Mn1 N6 98.40(8) . . ? O1 Mn1 O5 87.28(16) . . ? O2 Mn1 O5 83.53(14) . . ? N2 Mn1 O5 95.85(14) . . ? N6 Mn1 O5 91.72(16) . . ? O1 Mn1 O8 93.20(16) . . ? O2 Mn1 O8 99.64(14) . . ? N2 Mn1 O8 80.28(14) . . ? N6 Mn1 O8 87.50(16) . . ? O5 Mn1 O8 16.91(12) . . ? O1 Mn1 O4 88.68(7) . . ? O2 Mn1 O4 91.52(7) . . ? N2 Mn1 O4 88.72(8) . . ? N6 Mn1 O4 91.80(7) . . ? O5 Mn1 O4 173.77(14) . . ? O8 Mn1 O4 168.75(14) . . ? N7 Mn2 N3 85.21(8) . . ? N7 Mn2 N4 155.77(8) . . ? N3 Mn2 N4 72.96(8) . . ? N7 Mn2 O3 91.50(8) . . ? N3 Mn2 O3 99.13(8) . . ? N4 Mn2 O3 81.96(8) . . ? N7 Mn2 N8 73.46(8) . . ? N3 Mn2 N8 158.54(8) . . ? N4 Mn2 N8 127.41(8) . . ? O3 Mn2 N8 79.54(8) . . ? N7 Mn2 Cl1 101.64(6) . . ? N3 Mn2 Cl1 97.35(6) . . ? N4 Mn2 Cl1 91.67(6) . . ? O3 Mn2 Cl1 159.70(7) . . ? N8 Mn2 Cl1 89.35(6) . . ? C1 O1 Mn1 128.22(15) . . ? C14 O2 Mn1 125.02(15) . . ? Mn2 O3 H3B 120(2) . . ? Mn2 O3 H3A 119(3) . . ? H3B O3 H3A 107(3) . . ? C7 N1 C8 102.5(2) . . ? C7 N2 N3 106.9(2) . . ? C7 N2 Mn1 126.96(17) . . ? N3 N2 Mn1 125.63(16) . . ? C8 N3 N2 104.9(2) . . ? C8 N3 Mn2 116.14(16) . . ? N2 N3 Mn2 138.77(16) . . ? C13 N4 C9 118.2(2) . . ? C13 N4 Mn2 124.47(18) . . ? C9 N4 Mn2 117.32(16) . . ? C20 N5 C21 102.5(2) . . ? C20 N6 N7 106.00(19) . . ? C20 N6 Mn1 125.62(16) . . ? N7 N6 Mn1 126.86(15) . . ? C21 N7 N6 105.22(19) . . ? C21 N7 Mn2 117.10(16) . . ? N6 N7 Mn2 137.62(16) . . ? C26 N8 C22 117.9(2) . . ? C26 N8 Mn2 126.63(18) . . ? C22 N8 Mn2 115.08(16) . . ? O1 C1 C2 117.8(2) . . ? O1 C1 C6 123.0(2) . . ? C2 C1 C6 119.1(2) . . ? C3 C2 C1 120.9(2) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C2 C3 C4 120.3(2) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C3 C4 C5 119.2(2) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C4 C5 C6 121.6(2) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 118.8(2) . . ? C5 C6 C7 120.9(2) . . ? C1 C6 C7 120.2(2) . . ? N1 C7 N2 111.6(2) . . ? N1 C7 C6 125.1(2) . . ? N2 C7 C6 123.3(2) . . ? N3 C8 N1 114.2(2) . . ? N3 C8 C9 119.2(2) . . ? N1 C8 C9 126.7(2) . . ? N4 C9 C10 122.4(2) . . ? N4 C9 C8 114.3(2) . . ? C10 C9 C8 123.3(2) . . ? C11 C10 C9 118.2(3) . . ? C11 C10 H10 120.9 . . ? C9 C10 H10 120.9 . . ? C12 C11 C10 119.5(3) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C13 C12 C11 119.0(3) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? N4 C13 C12 122.7(3) . . ? N4 C13 H13 118.7 . . ? C12 C13 H13 118.7 . . ? O2 C14 C19 122.3(2) . . ? O2 C14 C15 119.0(2) . . ? C19 C14 C15 118.6(2) . . ? C16 C15 C14 120.6(3) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 121.1(2) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C18 C17 C16 119.0(3) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C17 C18 C19 121.0(2) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C14 C19 C18 119.6(2) . . ? C14 C19 C20 120.2(2) . . ? C18 C19 C20 120.2(2) . . ? N5 C20 N6 112.5(2) . . ? N5 C20 C19 125.3(2) . . ? N6 C20 C19 122.2(2) . . ? N7 C21 N5 113.8(2) . . ? N7 C21 C22 119.3(2) . . ? N5 C21 C22 126.8(2) . . ? N8 C22 C23 122.6(2) . . ? N8 C22 C21 114.1(2) . . ? C23 C22 C21 123.3(2) . . ? C22 C23 C24 118.5(2) . . ? C22 C23 H23 120.7 . . ? C24 C23 H23 120.7 . . ? C25 C24 C23 118.8(3) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? C24 C25 C26 119.3(3) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? N8 C26 C25 122.8(3) . . ? N8 C26 H26 118.6 . . ? C25 C26 H26 118.6 . . ? N9 C27 H27A 109.5 . . ? N9 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N9 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N9 C28 H28A 109.5 . . ? N9 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N9 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O4 C29 N9 125.3(2) . . ? O4 C29 H29 117.4 . . ? N9 C29 H29 117.4 . . ? C29 N9 C28 122.8(2) . . ? C29 N9 C27 120.6(2) . . ? C28 N9 C27 116.6(2) . . ? C29 O4 Mn1 117.62(16) . . ? O5 O8 C32 100.7(11) . . ? O5 O8 Mn1 77.1(9) . . ? C32 O8 Mn1 156.2(6) . . ? C31 O9 N10 53.2(4) . . ? O9 C31 N10 92.3(5) . . ? O8 C32 O5 31.6(4) . . ? O8 C32 N10 149.6(6) . . ? O5 C32 N10 122.0(5) . . ? C32 N10 C30 123.4(5) . . ? C32 N10 C31 120.6(4) . . ? C30 N10 C31 116.0(5) . . ? C32 N10 O9 91.2(3) . . ? C30 N10 O9 140.9(5) . . ? C31 N10 O9 34.5(3) . . ? O8 O5 C32 47.6(8) . . ? O8 O5 Mn1 86.0(9) . . ? C32 O5 Mn1 128.7(4) . . ? H6A O6 H6B 102(4) . . ? H7A O7 H7B 103(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.496 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.066 # Attachment '2.cif' data_shelxla _database_code_depnum_ccdc_archive 'CCDC 690529' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39.50 H41 Mn2 N10 O9.50' _chemical_formula_weight 917.70 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' 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 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.667(6) _cell_length_b 19.462(5) _cell_length_c 22.363(6) _cell_angle_alpha 90.00 _cell_angle_beta 116.436(3) _cell_angle_gamma 90.00 _cell_volume 8444(4) _cell_formula_units_Z 8 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 10164 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 27.9 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3792 _exptl_absorpt_coefficient_mu 0.666 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8674 _exptl_absorpt_correction_T_max 0.9010 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn CCD arae detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 25643 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7449 _reflns_number_gt 6592 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0637P)^2^+21.9552P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7449 _refine_ls_number_parameters 588 _refine_ls_number_restraints 44 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1280 _refine_ls_wR_factor_gt 0.1231 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.84367(2) 0.48412(2) 1.02106(2) 0.01672(13) Uani 1 1 d . . . Mn2 Mn 0.82372(2) 0.32291(2) 0.89090(2) 0.01715(13) Uani 1 1 d . . . N1 N 0.95252(13) 0.50971(12) 1.10055(12) 0.0207(5) Uani 1 1 d . . . N2 N 1.02080(12) 0.39269(12) 1.01668(11) 0.0199(5) Uani 1 1 d . . . N3 N 0.91371(12) 0.42229(12) 0.99863(11) 0.0177(5) Uani 1 1 d . . . N4 N 0.90826(12) 0.37514(11) 0.95127(11) 0.0172(5) Uani 1 1 d . . . N5 N 0.78070(12) 0.47794(12) 1.07988(11) 0.0188(5) Uani 1 1 d . . . N6 N 0.68826(13) 0.33024(12) 0.97797(12) 0.0186(5) Uani 1 1 d . . . N7 N 0.77871(12) 0.39191(12) 0.98613(11) 0.0171(5) Uani 1 1 d . . . N8 N 0.76692(12) 0.34122(11) 0.93999(11) 0.0162(5) Uani 1 1 d . . . O1 O 0.87189(10) 0.30160(11) 0.83995(9) 0.0225(4) Uani 1 1 d . . . O2 O 0.75042(11) 0.26930(11) 0.83146(10) 0.0248(5) Uani 1 1 d . . . O3 O 0.69123(12) 0.82746(10) 0.78892(10) 0.0254(5) Uani 1 1 d . . . H3 H 0.6712 0.8184 0.7479 0.038 Uiso 1 1 calc R . . O4 O 0.81197(11) 0.59138(10) 1.00482(10) 0.0237(5) Uani 1 1 d . . . O5 O 0.79414(12) 0.53008(10) 0.91591(10) 0.0267(5) Uani 1 1 d . . . O6 O 0.77528(11) 0.41840(11) 0.82947(10) 0.0235(5) Uani 1 1 d . . . H6A H 0.7875 0.4580 0.8467 0.028 Uiso 1 1 d R . . H6B H 0.7449 0.4145 0.7892 0.028 Uiso 1 1 d R . . O7 O 0.87751(11) 0.23625(10) 0.95986(11) 0.0270(5) Uani 1 1 d . . . H7A H 0.9074 0.2446 0.9996 0.032 Uiso 1 1 d R . . H7B H 0.8682 0.1950 0.9464 0.032 Uiso 1 1 d R . . C1 C 0.97022(17) 0.55529(16) 1.15042(15) 0.0263(7) Uani 1 1 d . . . H1 H 0.9344 0.5785 1.1558 0.032 Uiso 1 1 calc R . . C2 C 1.03757(17) 0.57026(17) 1.19438(15) 0.0290(7) Uani 1 1 d . . . H2 H 1.0478 0.6027 1.2293 0.035 Uiso 1 1 calc R . . C3 C 1.08994(17) 0.53689(17) 1.18638(15) 0.0282(7) Uani 1 1 d . . . H3A H 1.1368 0.5461 1.2159 0.034 Uiso 1 1 calc R . . C4 C 1.07305(16) 0.48987(15) 1.13463(14) 0.0233(6) Uani 1 1 d . . . H4 H 1.1080 0.4664 1.1280 0.028 Uiso 1 1 calc R . . C5 C 1.00405(15) 0.47807(14) 1.09296(13) 0.0189(6) Uani 1 1 d . . . C6 C 0.98086(15) 0.43059(14) 1.03600(13) 0.0175(6) Uani 1 1 d . . . C7 C 0.97326(15) 0.35889(14) 0.96330(13) 0.0185(6) Uani 1 1 d . . . C8 C 0.99032(16) 0.31106(15) 0.92246(15) 0.0220(6) Uani 1 1 d . . . C9 C 1.05924(17) 0.29467(18) 0.94125(16) 0.0304(7) Uani 1 1 d . . . H9 H 1.0940 0.3126 0.9818 0.036 Uiso 1 1 calc R . . C10 C 1.07766(18) 0.2530(2) 0.90199(18) 0.0404(9) Uani 1 1 d . . . H10 H 1.1247 0.2423 0.9153 0.048 Uiso 1 1 calc R . . C11 C 1.02684(19) 0.2269(2) 0.84295(18) 0.0429(9) Uani 1 1 d . . . H11 H 1.0393 0.1980 0.8159 0.051 Uiso 1 1 calc R . . C12 C 0.95815(18) 0.2424(2) 0.82294(17) 0.0365(8) Uani 1 1 d . . . H12 H 0.9239 0.2239 0.7824 0.044 Uiso 1 1 calc R . . C13 C 0.93878(16) 0.28524(16) 0.86226(15) 0.0240(6) Uani 1 1 d . . . C14 C 0.78316(16) 0.52251(15) 1.12648(15) 0.0239(6) Uani 1 1 d . . . H14 H 0.8168 0.5580 1.1397 0.029 Uiso 1 1 calc R . . C15 C 0.73968(18) 0.51983(17) 1.15627(17) 0.0324(8) Uani 1 1 d . . . H15 H 0.7435 0.5523 1.1895 0.039 Uiso 1 1 calc R . . C16 C 0.6904(2) 0.4687(2) 1.1366(2) 0.0426(9) Uani 1 1 d . . . H16 H 0.6602 0.4649 1.1569 0.051 Uiso 1 1 calc R . . C17 C 0.68530(19) 0.42285(18) 1.08710(18) 0.0354(8) Uani 1 1 d . . . H17 H 0.6507 0.3883 1.0718 0.042 Uiso 1 1 calc R . . C18 C 0.73171(16) 0.42869(14) 1.06045(14) 0.0207(6) Uani 1 1 d . . . C19 C 0.73146(15) 0.38281(14) 1.00770(13) 0.0177(6) Uani 1 1 d . . . C20 C 0.71154(15) 0.30559(14) 0.93519(13) 0.0169(6) Uani 1 1 d . . . C21 C 0.67998(15) 0.24904(14) 0.88849(14) 0.0185(6) Uani 1 1 d . . . C22 C 0.62695(16) 0.21010(15) 0.89120(15) 0.0221(6) Uani 1 1 d . . . H22 H 0.6127 0.2198 0.9248 0.027 Uiso 1 1 calc R . . C23 C 0.59493(16) 0.15785(15) 0.84606(15) 0.0258(7) Uani 1 1 d . . . H23 H 0.5589 0.1321 0.8484 0.031 Uiso 1 1 calc R . . C24 C 0.61603(16) 0.14351(15) 0.79733(15) 0.0265(7) Uani 1 1 d . . . H24 H 0.5942 0.1077 0.7661 0.032 Uiso 1 1 calc R . . C25 C 0.66818(16) 0.18061(15) 0.79364(15) 0.0252(7) Uani 1 1 d . . . H25 H 0.6820 0.1699 0.7599 0.030 Uiso 1 1 calc R . . C26 C 0.70153(15) 0.23413(15) 0.83887(14) 0.0201(6) Uani 1 1 d . . . C27 C 0.79194(15) 0.58733(15) 0.94237(14) 0.0203(6) Uani 1 1 d . . . C28 C 0.76632(14) 0.64997(14) 0.90079(14) 0.0186(6) Uani 1 1 d . . . C29 C 0.74339(16) 0.64828(15) 0.83183(14) 0.0224(6) Uani 1 1 d . . . H29 H 0.7448 0.6063 0.8108 0.027 Uiso 1 1 calc R . . C30 C 0.71856(16) 0.70698(15) 0.79363(14) 0.0223(6) Uani 1 1 d . . . H30 H 0.7032 0.7052 0.7467 0.027 Uiso 1 1 calc R . . C31 C 0.71608(15) 0.76869(14) 0.82404(14) 0.0200(6) Uani 1 1 d . . . C32 C 0.74006(15) 0.77131(15) 0.89333(14) 0.0206(6) Uani 1 1 d . . . H32 H 0.7394 0.8134 0.9145 0.025 Uiso 1 1 calc R . . C33 C 0.76477(15) 0.71221(15) 0.93070(14) 0.0203(6) Uani 1 1 d . . . H33 H 0.7810 0.7141 0.9777 0.024 Uiso 1 1 calc R . . C34 C 0.5717(2) 0.2477(2) 0.6257(2) 0.0556(11) Uani 1 1 d . . . H34A H 0.6170 0.2362 0.6286 0.083 Uiso 1 1 calc R . . H34B H 0.5387 0.2544 0.5787 0.083 Uiso 1 1 calc R . . H34C H 0.5559 0.2102 0.6446 0.083 Uiso 1 1 calc R . . C35 C 0.5135(3) 0.3375(4) 0.6594(5) 0.152(4) Uani 1 1 d . . . H35A H 0.5211 0.3848 0.6764 0.229 Uiso 1 1 calc R . . H35B H 0.4986 0.3091 0.6867 0.229 Uiso 1 1 calc R . . H35C H 0.4779 0.3372 0.6130 0.229 Uiso 1 1 calc R . . C36 C 0.63591(19) 0.34127(19) 0.69930(18) 0.0386(8) Uani 1 1 d . . . H36 H 0.6761 0.3208 0.7002 0.046 Uiso 1 1 calc R . . N9 N 0.57684(18) 0.31038(19) 0.66255(18) 0.0515(9) Uani 1 1 d . . . O8 O 0.64433(13) 0.39408(14) 0.73269(13) 0.0469(7) Uani 1 1 d . . . C37 C 0.4846(6) 0.4744(5) 0.0712(7) 0.145(5) Uani 0.631(5) 1 d PD A 1 H37A H 0.5135 0.4612 0.1177 0.217 Uiso 0.631(5) 1 calc PR A 1 H37B H 0.4561 0.5140 0.0699 0.217 Uiso 0.631(5) 1 calc PR A 1 H37C H 0.5139 0.4865 0.0498 0.217 Uiso 0.631(5) 1 calc PR A 1 C38 C 0.3698(3) 0.4151(4) 0.0312(5) 0.077(2) Uani 0.631(5) 1 d PD A 1 H38A H 0.3448 0.3753 0.0047 0.116 Uiso 0.631(5) 1 calc PR A 1 H38B H 0.3452 0.4573 0.0098 0.116 Uiso 0.631(5) 1 calc PR A 1 H38C H 0.3730 0.4117 0.0762 0.116 Uiso 0.631(5) 1 calc PR A 1 C39 C 0.4605(4) 0.3659(4) 0.0073(4) 0.0687(19) Uani 0.631(5) 1 d PD A 1 H39 H 0.4272 0.3343 -0.0216 0.082 Uiso 0.631(5) 1 calc PR A 1 N10 N 0.4399(3) 0.4168(3) 0.0356(3) 0.0709(13) Uani 0.631(5) 1 d PD A 1 O9 O 0.5214(6) 0.359(3) 0.0180(14) 0.076(3) Uani 0.631(5) 1 d PD A 1 N10' N 0.4367(5) 0.4111(5) 0.0420(6) 0.0709(13) Uani 0.369(5) 1 d PD A 2 O9' O 0.5184(12) 0.357(4) 0.022(2) 0.076(3) Uani 0.369(5) 1 d PD A 2 C37' C 0.4203(8) 0.4525(10) 0.0887(9) 0.145(5) Uani 0.369(5) 1 d PD A 2 H37D H 0.4622 0.4589 0.1307 0.217 Uiso 0.369(5) 1 calc PR A 2 H37E H 0.3856 0.4285 0.0977 0.217 Uiso 0.369(5) 1 calc PR A 2 H37F H 0.4024 0.4974 0.0687 0.217 Uiso 0.369(5) 1 calc PR A 2 C38' C 0.3828(5) 0.3956(8) -0.0234(6) 0.077(2) Uani 0.369(5) 1 d PD A 2 H38D H 0.3965 0.4115 -0.0574 0.116 Uiso 0.369(5) 1 calc PR A 2 H38E H 0.3403 0.4189 -0.0297 0.116 Uiso 0.369(5) 1 calc PR A 2 H38F H 0.3750 0.3458 -0.0278 0.116 Uiso 0.369(5) 1 calc PR A 2 C39' C 0.5033(4) 0.3882(4) 0.0622(4) 0.0687(19) Uani 0.369(5) 1 d PD A 2 H39' H 0.5374 0.3962 0.1066 0.082 Uiso 0.369(5) 1 calc PR A 2 O10 O 0.4024(4) 0.4561(4) 0.2178(4) 0.135(6) Uani 0.30 1 d PRDU A 1 C40 C 0.4134(4) 0.4807(4) 0.2808(4) 0.087(6) Uani 0.30 1 d PRDU A 1 O11 O 0.4352(4) 0.5065(4) 0.2085(4) 0.085(6) Uani 0.20 1 d PRDU A 2 C41 C 0.3803(4) 0.5415(4) 0.1509(4) 0.059(6) Uani 0.20 1 d PRDU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0186(2) 0.0158(2) 0.0154(2) -0.00064(15) 0.00725(19) -0.00309(17) Mn2 0.0161(2) 0.0215(2) 0.0155(2) -0.00515(16) 0.00851(19) -0.00554(17) N1 0.0225(13) 0.0227(13) 0.0179(12) -0.0018(9) 0.0099(11) -0.0069(10) N2 0.0196(13) 0.0217(12) 0.0173(12) 0.0000(9) 0.0072(10) -0.0036(10) N3 0.0202(13) 0.0174(11) 0.0157(11) -0.0013(9) 0.0082(10) -0.0042(10) N4 0.0190(13) 0.0178(11) 0.0161(11) -0.0019(9) 0.0089(10) -0.0027(10) N5 0.0198(13) 0.0181(12) 0.0192(12) -0.0008(9) 0.0092(11) -0.0004(10) N6 0.0200(13) 0.0173(12) 0.0218(12) -0.0012(9) 0.0123(11) -0.0024(10) N7 0.0196(13) 0.0163(11) 0.0170(11) -0.0040(9) 0.0094(10) -0.0022(10) N8 0.0175(12) 0.0158(11) 0.0157(11) -0.0030(9) 0.0079(10) -0.0041(9) O1 0.0177(11) 0.0330(11) 0.0180(10) -0.0060(8) 0.0091(9) -0.0044(9) O2 0.0222(11) 0.0338(12) 0.0219(10) -0.0109(9) 0.0128(9) -0.0113(9) O3 0.0341(13) 0.0208(11) 0.0180(10) 0.0031(8) 0.0084(10) 0.0042(9) O4 0.0292(12) 0.0232(11) 0.0183(10) 0.0030(8) 0.0102(9) -0.0005(9) O5 0.0341(13) 0.0199(11) 0.0229(11) 0.0008(8) 0.0098(10) 0.0012(9) O6 0.0242(11) 0.0271(11) 0.0170(10) -0.0028(8) 0.0072(9) -0.0068(9) O7 0.0326(13) 0.0200(10) 0.0334(12) -0.0016(9) 0.0192(11) -0.0044(9) C1 0.0308(18) 0.0310(17) 0.0227(15) -0.0059(13) 0.0169(14) -0.0099(14) C2 0.0349(19) 0.0359(18) 0.0210(15) -0.0095(13) 0.0167(15) -0.0171(15) C3 0.0251(17) 0.0395(18) 0.0183(15) -0.0024(13) 0.0080(14) -0.0164(14) C4 0.0235(16) 0.0279(16) 0.0178(14) 0.0013(12) 0.0086(13) -0.0060(13) C5 0.0227(16) 0.0182(14) 0.0158(13) 0.0033(11) 0.0085(12) -0.0059(12) C6 0.0187(15) 0.0173(13) 0.0151(13) 0.0029(11) 0.0062(12) -0.0034(11) C7 0.0207(15) 0.0187(14) 0.0177(13) 0.0014(11) 0.0101(12) -0.0050(12) C8 0.0206(16) 0.0258(15) 0.0241(15) -0.0009(12) 0.0139(13) -0.0054(12) C9 0.0197(17) 0.0403(19) 0.0284(17) -0.0093(14) 0.0082(14) -0.0045(14) C10 0.0207(18) 0.059(2) 0.043(2) -0.0131(18) 0.0151(16) 0.0035(16) C11 0.032(2) 0.065(3) 0.0375(19) -0.0185(18) 0.0199(17) 0.0022(18) C12 0.0263(19) 0.058(2) 0.0278(17) -0.0139(16) 0.0142(15) -0.0018(16) C13 0.0206(16) 0.0321(17) 0.0227(15) -0.0040(12) 0.0128(13) -0.0045(13) C14 0.0278(17) 0.0195(14) 0.0242(15) -0.0060(12) 0.0114(14) -0.0050(13) C15 0.0351(19) 0.0340(18) 0.0329(18) -0.0170(14) 0.0194(16) -0.0051(15) C16 0.048(2) 0.046(2) 0.053(2) -0.0215(18) 0.040(2) -0.0161(18) C17 0.042(2) 0.0331(18) 0.045(2) -0.0202(15) 0.0323(18) -0.0176(16) C18 0.0242(16) 0.0179(14) 0.0218(14) -0.0019(11) 0.0117(13) -0.0021(12) C19 0.0204(15) 0.0159(13) 0.0184(13) 0.0007(11) 0.0101(12) -0.0006(11) C20 0.0171(14) 0.0164(13) 0.0174(13) 0.0013(11) 0.0079(12) 0.0014(11) C21 0.0158(15) 0.0175(14) 0.0207(14) 0.0001(11) 0.0067(12) 0.0000(11) C22 0.0240(16) 0.0206(15) 0.0239(15) -0.0004(12) 0.0126(13) -0.0025(12) C23 0.0234(16) 0.0232(15) 0.0290(16) -0.0011(12) 0.0100(14) -0.0079(13) C24 0.0262(17) 0.0217(15) 0.0272(16) -0.0073(12) 0.0079(14) -0.0070(13) C25 0.0252(17) 0.0268(16) 0.0242(15) -0.0085(12) 0.0115(14) -0.0032(13) C26 0.0168(15) 0.0217(14) 0.0202(14) -0.0016(11) 0.0068(12) -0.0019(12) C27 0.0166(15) 0.0225(15) 0.0227(15) 0.0035(12) 0.0096(13) -0.0011(12) C28 0.0156(14) 0.0203(14) 0.0198(14) 0.0009(11) 0.0079(12) -0.0013(11) C29 0.0252(16) 0.0208(15) 0.0215(14) -0.0028(12) 0.0106(13) 0.0017(12) C30 0.0266(16) 0.0246(15) 0.0162(14) 0.0005(11) 0.0101(13) 0.0015(13) C31 0.0200(15) 0.0190(14) 0.0217(14) 0.0039(11) 0.0100(13) 0.0005(12) C32 0.0220(16) 0.0191(14) 0.0203(14) -0.0014(11) 0.0092(13) 0.0009(12) C33 0.0193(15) 0.0250(15) 0.0174(14) -0.0017(11) 0.0088(12) 0.0001(12) C34 0.063(3) 0.050(2) 0.040(2) -0.0104(18) 0.011(2) -0.010(2) C35 0.056(4) 0.179(8) 0.219(9) -0.145(8) 0.058(5) -0.047(5) C36 0.0266(19) 0.043(2) 0.0371(19) -0.0027(16) 0.0062(16) -0.0022(16) N9 0.0351(19) 0.060(2) 0.054(2) -0.0238(17) 0.0146(17) -0.0149(16) O8 0.0312(14) 0.0446(15) 0.0498(16) -0.0128(13) 0.0044(13) -0.0053(12) C37 0.102(9) 0.131(9) 0.209(13) -0.086(9) 0.076(9) -0.047(7) C38 0.049(4) 0.077(5) 0.101(6) 0.013(4) 0.029(4) 0.021(4) C39 0.055(5) 0.058(4) 0.101(6) 0.006(4) 0.042(4) 0.004(3) N10 0.041(2) 0.059(3) 0.106(4) -0.008(2) 0.027(2) 0.007(2) O9 0.052(2) 0.056(3) 0.138(4) 0.013(4) 0.057(3) 0.014(3) N10' 0.041(2) 0.059(3) 0.106(4) -0.008(2) 0.027(2) 0.007(2) O9' 0.052(2) 0.056(3) 0.138(4) 0.013(4) 0.057(3) 0.014(3) C37' 0.102(9) 0.131(9) 0.209(13) -0.086(9) 0.076(9) -0.047(7) C38' 0.049(4) 0.077(5) 0.101(6) 0.013(4) 0.029(4) 0.021(4) C39' 0.055(5) 0.058(4) 0.101(6) 0.006(4) 0.042(4) 0.004(3) O10 0.128(10) 0.140(10) 0.142(10) -0.034(8) 0.065(8) -0.021(8) C40 0.083(9) 0.091(9) 0.095(9) 0.012(7) 0.046(8) 0.010(7) O11 0.089(9) 0.074(9) 0.101(9) -0.001(7) 0.051(8) -0.008(7) C41 0.061(9) 0.076(10) 0.051(9) -0.012(7) 0.035(7) 0.025(8) _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 N3 2.163(2) . ? Mn1 O4 2.177(2) . ? Mn1 N7 2.198(2) . ? Mn1 N5 2.281(2) . ? Mn1 O5 2.288(2) . ? Mn1 N1 2.288(3) . ? Mn1 C27 2.575(3) . ? Mn2 O2 1.870(2) . ? Mn2 O1 1.9024(19) . ? Mn2 N4 2.002(2) . ? Mn2 N8 2.012(2) . ? Mn2 O7 2.232(2) . ? Mn2 O6 2.271(2) . ? N1 C1 1.341(4) . ? N1 C5 1.350(4) . ? N2 C6 1.346(4) . ? N2 C7 1.351(4) . ? N3 C6 1.326(4) . ? N3 N4 1.366(3) . ? N4 C7 1.348(4) . ? N5 C14 1.339(4) . ? N5 C18 1.350(4) . ? N6 C19 1.346(4) . ? N6 C20 1.352(4) . ? N7 C19 1.323(4) . ? N7 N8 1.367(3) . ? N8 C20 1.348(4) . ? O1 C13 1.344(4) . ? O2 C26 1.332(4) . ? O3 C31 1.356(3) . ? O3 H3 0.8400 . ? O4 C27 1.267(3) . ? O5 C27 1.272(4) . ? O6 H6A 0.8500 . ? O6 H6B 0.8499 . ? O7 H7A 0.8500 . ? O7 H7B 0.8499 . ? C1 C2 1.380(5) . ? C1 H1 0.9500 . ? C2 C3 1.386(5) . ? C2 H2 0.9500 . ? C3 C4 1.391(4) . ? C3 H3A 0.9500 . ? C4 C5 1.384(4) . ? C4 H4 0.9500 . ? C5 C6 1.469(4) . ? C7 C8 1.462(4) . ? C8 C9 1.396(4) . ? C8 C13 1.405(4) . ? C9 C10 1.378(5) . ? C9 H9 0.9500 . ? C10 C11 1.385(5) . ? C10 H10 0.9500 . ? C11 C12 1.383(5) . ? C11 H11 0.9500 . ? C12 C13 1.405(4) . ? C12 H12 0.9500 . ? C14 C15 1.376(4) . ? C14 H14 0.9500 . ? C15 C16 1.381(5) . ? C15 H15 0.9500 . ? C16 C17 1.387(5) . ? C16 H16 0.9500 . ? C17 C18 1.383(4) . ? C17 H17 0.9500 . ? C18 C19 1.478(4) . ? C20 C21 1.461(4) . ? C21 C22 1.400(4) . ? C21 C26 1.412(4) . ? C22 C23 1.382(4) . ? C22 H22 0.9500 . ? C23 C24 1.385(4) . ? C23 H23 0.9500 . ? C24 C25 1.374(4) . ? C24 H24 0.9500 . ? C25 C26 1.407(4) . ? C25 H25 0.9500 . ? C27 C28 1.483(4) . ? C28 C33 1.391(4) . ? C28 C29 1.394(4) . ? C29 C30 1.384(4) . ? C29 H29 0.9500 . ? C30 C31 1.393(4) . ? C30 H30 0.9500 . ? C31 C32 1.399(4) . ? C32 C33 1.382(4) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 N9 1.449(5) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 N9 1.442(7) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 O8 1.235(4) . ? C36 N9 1.318(5) . ? C36 H36 0.9500 . ? C37 N10 1.463(8) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 N10 1.479(7) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 O9 1.239(10) . ? C39 N10 1.351(7) . ? C39 H39 0.9500 . ? N10' C39' 1.379(8) . ? N10' C38' 1.442(9) . ? N10' C37' 1.481(9) . ? O9' C39' 1.241(10) . ? C37' H37D 0.9800 . ? C37' H37E 0.9800 . ? C37' H37F 0.9800 . ? C38' H38D 0.9800 . ? C38' H38E 0.9800 . ? C38' H38F 0.9800 . ? C39' H39' 0.9500 . ? O10 C40 1.4052 . ? O11 C41 1.4737 . ? 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 N3 Mn1 O4 134.15(8) . . ? N3 Mn1 N7 82.41(9) . . ? O4 Mn1 N7 128.24(9) . . ? N3 Mn1 N5 139.97(9) . . ? O4 Mn1 N5 85.49(8) . . ? N7 Mn1 N5 73.09(8) . . ? N3 Mn1 O5 92.05(8) . . ? O4 Mn1 O5 58.99(7) . . ? N7 Mn1 O5 91.19(8) . . ? N5 Mn1 O5 119.07(9) . . ? N3 Mn1 N1 73.41(9) . . ? O4 Mn1 N1 93.46(9) . . ? N7 Mn1 N1 136.80(9) . . ? N5 Mn1 N1 103.74(9) . . ? O5 Mn1 N1 124.26(8) . . ? N3 Mn1 C27 114.35(9) . . ? O4 Mn1 C27 29.43(8) . . ? N7 Mn1 C27 112.27(9) . . ? N5 Mn1 C27 104.18(9) . . ? O5 Mn1 C27 29.59(8) . . ? N1 Mn1 C27 110.21(9) . . ? O2 Mn2 O1 88.36(9) . . ? O2 Mn2 N4 174.18(9) . . ? O1 Mn2 N4 86.17(9) . . ? O2 Mn2 N8 87.39(9) . . ? O1 Mn2 N8 175.75(9) . . ? N4 Mn2 N8 98.07(9) . . ? O2 Mn2 O7 94.96(9) . . ? O1 Mn2 O7 89.55(8) . . ? N4 Mn2 O7 83.01(9) . . ? N8 Mn2 O7 90.86(9) . . ? O2 Mn2 O6 90.52(9) . . ? O1 Mn2 O6 92.58(8) . . ? N4 Mn2 O6 91.72(9) . . ? N8 Mn2 O6 87.42(8) . . ? O7 Mn2 O6 174.18(8) . . ? C1 N1 C5 117.4(3) . . ? C1 N1 Mn1 127.2(2) . . ? C5 N1 Mn1 115.27(18) . . ? C6 N2 C7 101.8(2) . . ? C6 N3 N4 105.2(2) . . ? C6 N3 Mn1 118.18(18) . . ? N4 N3 Mn1 136.54(18) . . ? C7 N4 N3 106.3(2) . . ? C7 N4 Mn2 125.18(18) . . ? N3 N4 Mn2 126.95(18) . . ? C14 N5 C18 117.6(2) . . ? C14 N5 Mn1 126.0(2) . . ? C18 N5 Mn1 115.98(18) . . ? C19 N6 C20 102.9(2) . . ? C19 N7 N8 105.3(2) . . ? C19 N7 Mn1 117.17(18) . . ? N8 N7 Mn1 137.08(17) . . ? C20 N8 N7 107.0(2) . . ? C20 N8 Mn2 127.18(18) . . ? N7 N8 Mn2 125.83(17) . . ? C13 O1 Mn2 128.14(18) . . ? C26 O2 Mn2 131.98(18) . . ? C31 O3 H3 109.5 . . ? C27 O4 Mn1 92.98(17) . . ? C27 O5 Mn1 87.82(16) . . ? Mn2 O6 H6A 120.0 . . ? Mn2 O6 H6B 120.0 . . ? H6A O6 H6B 120.0 . . ? Mn2 O7 H7A 119.9 . . ? Mn2 O7 H7B 120.1 . . ? H7A O7 H7B 120.0 . . ? N1 C1 C2 123.5(3) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C1 C2 C3 118.4(3) . . ? C1 C2 H2 120.8 . . ? C3 C2 H2 120.8 . . ? C2 C3 C4 119.2(3) . . ? C2 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? C5 C4 C3 118.3(3) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? N1 C5 C4 123.1(3) . . ? N1 C5 C6 114.4(3) . . ? C4 C5 C6 122.5(3) . . ? N3 C6 N2 114.4(2) . . ? N3 C6 C5 118.6(3) . . ? N2 C6 C5 127.0(3) . . ? N4 C7 N2 112.3(2) . . ? N4 C7 C8 123.8(3) . . ? N2 C7 C8 123.8(3) . . ? C9 C8 C13 119.6(3) . . ? C9 C8 C7 119.4(3) . . ? C13 C8 C7 120.8(3) . . ? C10 C9 C8 121.1(3) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C11 119.3(3) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C12 C11 C10 120.8(3) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C13 120.3(3) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? O1 C13 C8 122.5(3) . . ? O1 C13 C12 118.8(3) . . ? C8 C13 C12 118.7(3) . . ? N5 C14 C15 123.6(3) . . ? N5 C14 H14 118.2 . . ? C15 C14 H14 118.2 . . ? C14 C15 C16 118.2(3) . . ? C14 C15 H15 120.9 . . ? C16 C15 H15 120.9 . . ? C15 C16 C17 119.5(3) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C18 C17 C16 118.4(3) . . ? C18 C17 H17 120.8 . . ? C16 C17 H17 120.8 . . ? N5 C18 C17 122.5(3) . . ? N5 C18 C19 114.1(2) . . ? C17 C18 C19 123.3(3) . . ? N7 C19 N6 113.7(2) . . ? N7 C19 C18 118.8(2) . . ? N6 C19 C18 127.5(3) . . ? N8 C20 N6 111.1(2) . . ? N8 C20 C21 124.1(2) . . ? N6 C20 C21 124.7(3) . . ? C22 C21 C26 119.2(3) . . ? C22 C21 C20 120.6(2) . . ? C26 C21 C20 120.2(3) . . ? C23 C22 C21 121.4(3) . . ? C23 C22 H22 119.3 . . ? C21 C22 H22 119.3 . . ? C22 C23 C24 119.3(3) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? C25 C24 C23 120.6(3) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 121.3(3) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? O2 C26 C25 118.3(3) . . ? O2 C26 C21 123.5(3) . . ? C25 C26 C21 118.3(3) . . ? O4 C27 O5 120.1(3) . . ? O4 C27 C28 119.3(3) . . ? O5 C27 C28 120.6(2) . . ? O4 C27 Mn1 57.59(14) . . ? O5 C27 Mn1 62.59(15) . . ? C28 C27 Mn1 175.7(2) . . ? C33 C28 C29 118.6(3) . . ? C33 C28 C27 119.8(3) . . ? C29 C28 C27 121.6(3) . . ? C30 C29 C28 120.8(3) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C29 C30 C31 120.0(3) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? O3 C31 C30 122.4(2) . . ? O3 C31 C32 117.8(3) . . ? C30 C31 C32 119.7(3) . . ? C33 C32 C31 119.5(3) . . ? C33 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? C32 C33 C28 121.3(3) . . ? C32 C33 H33 119.3 . . ? C28 C33 H33 119.3 . . ? N9 C34 H34A 109.5 . . ? N9 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N9 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N9 C35 H35A 109.5 . . ? N9 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N9 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O8 C36 N9 126.7(4) . . ? O8 C36 H36 116.7 . . ? N9 C36 H36 116.7 . . ? C36 N9 C35 120.1(4) . . ? C36 N9 C34 123.1(4) . . ? C35 N9 C34 116.8(4) . . ? O9 C39 N10 122.1(12) . . ? O9 C39 H39 118.9 . . ? N10 C39 H39 118.9 . . ? C39 N10 C37 122.7(6) . . ? C39 N10 C38 119.7(6) . . ? C37 N10 C38 117.6(7) . . ? C39' N10' C38' 121.4(7) . . ? C39' N10' C37' 119.3(8) . . ? C38' N10' C37' 119.3(9) . . ? N10' C37' H37D 109.5 . . ? N10' C37' H37E 109.5 . . ? H37D C37' H37E 109.5 . . ? N10' C37' H37F 109.5 . . ? H37D C37' H37F 109.5 . . ? H37E C37' H37F 109.5 . . ? N10' C38' H38D 109.5 . . ? N10' C38' H38E 109.5 . . ? H38D C38' H38E 109.5 . . ? N10' C38' H38F 109.5 . . ? H38D C38' H38F 109.5 . . ? H38E C38' H38F 109.5 . . ? O9' C39' N10' 119.7(11) . . ? O9' C39' H39' 120.2 . . ? N10' C39' H39' 120.2 . . ? 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 N3 Mn1 N1 C1 178.4(3) . . . . ? O4 Mn1 N1 C1 43.1(2) . . . . ? N7 Mn1 N1 C1 -122.9(2) . . . . ? N5 Mn1 N1 C1 -43.1(2) . . . . ? O5 Mn1 N1 C1 97.5(2) . . . . ? C27 Mn1 N1 C1 68.0(2) . . . . ? N3 Mn1 N1 C5 2.93(18) . . . . ? O4 Mn1 N1 C5 -132.31(19) . . . . ? N7 Mn1 N1 C5 61.7(2) . . . . ? N5 Mn1 N1 C5 141.49(18) . . . . ? O5 Mn1 N1 C5 -78.0(2) . . . . ? C27 Mn1 N1 C5 -107.48(19) . . . . ? O4 Mn1 N3 C6 74.9(2) . . . . ? N7 Mn1 N3 C6 -147.3(2) . . . . ? N5 Mn1 N3 C6 -95.2(2) . . . . ? O5 Mn1 N3 C6 121.8(2) . . . . ? N1 Mn1 N3 C6 -3.45(19) . . . . ? C27 Mn1 N3 C6 101.7(2) . . . . ? O4 Mn1 N3 N4 -101.4(3) . . . . ? N7 Mn1 N3 N4 36.4(2) . . . . ? N5 Mn1 N3 N4 88.5(3) . . . . ? O5 Mn1 N3 N4 -54.5(2) . . . . ? N1 Mn1 N3 N4 -179.7(3) . . . . ? C27 Mn1 N3 N4 -74.6(3) . . . . ? C6 N3 N4 C7 -0.6(3) . . . . ? Mn1 N3 N4 C7 176.0(2) . . . . ? C6 N3 N4 Mn2 165.52(18) . . . . ? Mn1 N3 N4 Mn2 -17.9(4) . . . . ? O2 Mn2 N4 C7 -11.3(11) . . . . ? O1 Mn2 N4 C7 -31.4(2) . . . . ? N8 Mn2 N4 C7 148.5(2) . . . . ? O7 Mn2 N4 C7 58.6(2) . . . . ? O6 Mn2 N4 C7 -123.9(2) . . . . ? O2 Mn2 N4 N3 -175.0(8) . . . . ? O1 Mn2 N4 N3 164.9(2) . . . . ? N8 Mn2 N4 N3 -15.2(2) . . . . ? O7 Mn2 N4 N3 -105.1(2) . . . . ? O6 Mn2 N4 N3 72.4(2) . . . . ? N3 Mn1 N5 C14 125.4(2) . . . . ? O4 Mn1 N5 C14 -47.5(2) . . . . ? N7 Mn1 N5 C14 -179.8(3) . . . . ? O5 Mn1 N5 C14 -98.1(2) . . . . ? N1 Mn1 N5 C14 45.0(3) . . . . ? C27 Mn1 N5 C14 -70.4(3) . . . . ? N3 Mn1 N5 C18 -61.8(3) . . . . ? O4 Mn1 N5 C18 125.2(2) . . . . ? N7 Mn1 N5 C18 -7.1(2) . . . . ? O5 Mn1 N5 C18 74.7(2) . . . . ? N1 Mn1 N5 C18 -142.3(2) . . . . ? C27 Mn1 N5 C18 102.3(2) . . . . ? N3 Mn1 N7 C19 156.2(2) . . . . ? O4 Mn1 N7 C19 -61.7(2) . . . . ? N5 Mn1 N7 C19 8.17(19) . . . . ? O5 Mn1 N7 C19 -111.9(2) . . . . ? N1 Mn1 N7 C19 100.4(2) . . . . ? C27 Mn1 N7 C19 -90.6(2) . . . . ? N3 Mn1 N7 N8 -33.2(3) . . . . ? O4 Mn1 N7 N8 109.0(3) . . . . ? N5 Mn1 N7 N8 178.8(3) . . . . ? O5 Mn1 N7 N8 58.7(3) . . . . ? N1 Mn1 N7 N8 -88.9(3) . . . . ? C27 Mn1 N7 N8 80.1(3) . . . . ? C19 N7 N8 C20 1.7(3) . . . . ? Mn1 N7 N8 C20 -169.7(2) . . . . ? C19 N7 N8 Mn2 -176.91(18) . . . . ? Mn1 N7 N8 Mn2 11.7(4) . . . . ? O2 Mn2 N8 C20 17.3(2) . . . . ? O1 Mn2 N8 C20 17.8(14) . . . . ? N4 Mn2 N8 C20 -160.7(2) . . . . ? O7 Mn2 N8 C20 -77.7(2) . . . . ? O6 Mn2 N8 C20 107.9(2) . . . . ? O2 Mn2 N8 N7 -164.4(2) . . . . ? O1 Mn2 N8 N7 -163.8(12) . . . . ? N4 Mn2 N8 N7 17.6(2) . . . . ? O7 Mn2 N8 N7 100.7(2) . . . . ? O6 Mn2 N8 N7 -73.7(2) . . . . ? O2 Mn2 O1 C13 -137.9(2) . . . . ? N4 Mn2 O1 C13 40.1(2) . . . . ? N8 Mn2 O1 C13 -138.5(12) . . . . ? O7 Mn2 O1 C13 -42.9(2) . . . . ? O6 Mn2 O1 C13 131.6(2) . . . . ? O1 Mn2 O2 C26 152.7(3) . . . . ? N4 Mn2 O2 C26 132.6(9) . . . . ? N8 Mn2 O2 C26 -27.3(3) . . . . ? O7 Mn2 O2 C26 63.3(3) . . . . ? O6 Mn2 O2 C26 -114.7(3) . . . . ? N3 Mn1 O4 C27 56.5(2) . . . . ? N7 Mn1 O4 C27 -65.49(19) . . . . ? N5 Mn1 O4 C27 -129.79(18) . . . . ? O5 Mn1 O4 C27 -1.77(16) . . . . ? N1 Mn1 O4 C27 126.67(17) . . . . ? N3 Mn1 O5 C27 -140.58(17) . . . . ? O4 Mn1 O5 C27 1.76(16) . . . . ? N7 Mn1 O5 C27 136.97(17) . . . . ? N5 Mn1 O5 C27 65.71(19) . . . . ? N1 Mn1 O5 C27 -69.33(19) . . . . ? C5 N1 C1 C2 -1.2(4) . . . . ? Mn1 N1 C1 C2 -176.5(2) . . . . ? N1 C1 C2 C3 0.6(5) . . . . ? C1 C2 C3 C4 0.1(4) . . . . ? C2 C3 C4 C5 -0.1(4) . . . . ? C1 N1 C5 C4 1.1(4) . . . . ? Mn1 N1 C5 C4 177.1(2) . . . . ? C1 N1 C5 C6 -178.0(2) . . . . ? Mn1 N1 C5 C6 -2.1(3) . . . . ? C3 C4 C5 N1 -0.5(4) . . . . ? C3 C4 C5 C6 178.6(3) . . . . ? N4 N3 C6 N2 0.5(3) . . . . ? Mn1 N3 C6 N2 -176.88(17) . . . . ? N4 N3 C6 C5 -179.0(2) . . . . ? Mn1 N3 C6 C5 3.6(3) . . . . ? C7 N2 C6 N3 -0.1(3) . . . . ? C7 N2 C6 C5 179.3(3) . . . . ? N1 C5 C6 N3 -0.9(4) . . . . ? C4 C5 C6 N3 180.0(3) . . . . ? N1 C5 C6 N2 179.7(2) . . . . ? C4 C5 C6 N2 0.6(4) . . . . ? N3 N4 C7 N2 0.6(3) . . . . ? Mn2 N4 C7 N2 -165.85(18) . . . . ? N3 N4 C7 C8 -178.3(2) . . . . ? Mn2 N4 C7 C8 15.2(4) . . . . ? C6 N2 C7 N4 -0.3(3) . . . . ? C6 N2 C7 C8 178.6(3) . . . . ? N4 C7 C8 C9 -176.4(3) . . . . ? N2 C7 C8 C9 4.7(4) . . . . ? N4 C7 C8 C13 8.0(4) . . . . ? N2 C7 C8 C13 -170.8(3) . . . . ? C13 C8 C9 C10 -0.6(5) . . . . ? C7 C8 C9 C10 -176.2(3) . . . . ? C8 C9 C10 C11 -0.1(6) . . . . ? C9 C10 C11 C12 0.3(6) . . . . ? C10 C11 C12 C13 0.2(6) . . . . ? Mn2 O1 C13 C8 -30.9(4) . . . . ? Mn2 O1 C13 C12 151.1(2) . . . . ? C9 C8 C13 O1 -177.0(3) . . . . ? C7 C8 C13 O1 -1.4(4) . . . . ? C9 C8 C13 C12 1.1(5) . . . . ? C7 C8 C13 C12 176.6(3) . . . . ? C11 C12 C13 O1 177.2(3) . . . . ? C11 C12 C13 C8 -0.9(5) . . . . ? C18 N5 C14 C15 1.4(5) . . . . ? Mn1 N5 C14 C15 174.0(2) . . . . ? N5 C14 C15 C16 -0.5(5) . . . . ? C14 C15 C16 C17 -1.3(6) . . . . ? C15 C16 C17 C18 2.2(6) . . . . ? C14 N5 C18 C17 -0.4(4) . . . . ? Mn1 N5 C18 C17 -173.8(3) . . . . ? C14 N5 C18 C19 178.5(3) . . . . ? Mn1 N5 C18 C19 5.2(3) . . . . ? C16 C17 C18 N5 -1.3(5) . . . . ? C16 C17 C18 C19 179.8(3) . . . . ? N8 N7 C19 N6 -1.2(3) . . . . ? Mn1 N7 C19 N6 172.21(18) . . . . ? N8 N7 C19 C18 178.0(2) . . . . ? Mn1 N7 C19 C18 -8.6(3) . . . . ? C20 N6 C19 N7 0.2(3) . . . . ? C20 N6 C19 C18 -178.9(3) . . . . ? N5 C18 C19 N7 2.1(4) . . . . ? C17 C18 C19 N7 -179.0(3) . . . . ? N5 C18 C19 N6 -178.9(3) . . . . ? C17 C18 C19 N6 0.1(5) . . . . ? N7 N8 C20 N6 -1.7(3) . . . . ? Mn2 N8 C20 N6 176.89(18) . . . . ? N7 N8 C20 C21 176.7(2) . . . . ? Mn2 N8 C20 C21 -4.7(4) . . . . ? C19 N6 C20 N8 1.0(3) . . . . ? C19 N6 C20 C21 -177.5(3) . . . . ? N8 C20 C21 C22 173.5(3) . . . . ? N6 C20 C21 C22 -8.3(4) . . . . ? N8 C20 C21 C26 -8.1(4) . . . . ? N6 C20 C21 C26 170.1(3) . . . . ? C26 C21 C22 C23 -0.5(4) . . . . ? C20 C21 C22 C23 177.9(3) . . . . ? C21 C22 C23 C24 0.3(5) . . . . ? C22 C23 C24 C25 0.0(5) . . . . ? C23 C24 C25 C26 -0.1(5) . . . . ? Mn2 O2 C26 C25 -158.5(2) . . . . ? Mn2 O2 C26 C21 23.5(4) . . . . ? C24 C25 C26 O2 -178.2(3) . . . . ? C24 C25 C26 C21 -0.1(5) . . . . ? C22 C21 C26 O2 178.5(3) . . . . ? C20 C21 C26 O2 0.0(4) . . . . ? C22 C21 C26 C25 0.4(4) . . . . ? C20 C21 C26 C25 -178.0(3) . . . . ? Mn1 O4 C27 O5 3.1(3) . . . . ? Mn1 O4 C27 C28 -176.6(2) . . . . ? Mn1 O5 C27 O4 -3.0(3) . . . . ? Mn1 O5 C27 C28 176.8(2) . . . . ? N3 Mn1 C27 O4 -138.92(16) . . . . ? N7 Mn1 C27 O4 129.44(17) . . . . ? N5 Mn1 C27 O4 52.19(18) . . . . ? O5 Mn1 C27 O4 176.9(3) . . . . ? N1 Mn1 C27 O4 -58.55(18) . . . . ? N3 Mn1 C27 O5 44.15(19) . . . . ? O4 Mn1 C27 O5 -176.9(3) . . . . ? N7 Mn1 C27 O5 -47.49(18) . . . . ? N5 Mn1 C27 O5 -124.74(17) . . . . ? N1 Mn1 C27 O5 124.51(17) . . . . ? N3 Mn1 C27 C28 -95(3) . . . . ? O4 Mn1 C27 C28 44(3) . . . . ? N7 Mn1 C27 C28 173(3) . . . . ? N5 Mn1 C27 C28 96(3) . . . . ? O5 Mn1 C27 C28 -139(3) . . . . ? N1 Mn1 C27 C28 -15(3) . . . . ? O4 C27 C28 C33 0.2(4) . . . . ? O5 C27 C28 C33 -179.5(3) . . . . ? Mn1 C27 C28 C33 -42(3) . . . . ? O4 C27 C28 C29 -179.7(3) . . . . ? O5 C27 C28 C29 0.6(4) . . . . ? Mn1 C27 C28 C29 138(3) . . . . ? C33 C28 C29 C30 -1.0(4) . . . . ? C27 C28 C29 C30 178.9(3) . . . . ? C28 C29 C30 C31 -0.2(5) . . . . ? C29 C30 C31 O3 -178.9(3) . . . . ? C29 C30 C31 C32 1.3(5) . . . . ? O3 C31 C32 C33 179.0(3) . . . . ? C30 C31 C32 C33 -1.2(4) . . . . ? C31 C32 C33 C28 0.0(4) . . . . ? C29 C28 C33 C32 1.1(4) . . . . ? C27 C28 C33 C32 -178.8(3) . . . . ? O8 C36 N9 C35 -1.0(8) . . . . ? O8 C36 N9 C34 -179.0(4) . . . . ? O9 C39 N10 C37 11(3) . . . . ? O9 C39 N10 C38 -169(3) . . . . ? C38' N10' C39' O9' 4(5) . . . . ? C37' N10' C39' O9' -176(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.867 _refine_diff_density_min -0.748 _refine_diff_density_rms 0.079 # Attachment '5.cif' data_071008c _database_code_depnum_ccdc_archive 'CCDC 690530' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H84 Mn4 N16 O24 S4' _chemical_formula_weight 1809.47 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 C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 19.760(3) _cell_length_b 16.999(3) _cell_length_c 11.6453(18) _cell_angle_alpha 90.00 _cell_angle_beta 93.914(2) _cell_angle_gamma 90.00 _cell_volume 3902.5(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3465 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 26.15 _exptl_crystal_description block _exptl_crystal_colour dark-green _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 0.825 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.808891 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10067 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3579 _reflns_number_gt 2680 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+8.4082P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3579 _refine_ls_number_parameters 273 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0600 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.1060 _refine_ls_wR_factor_gt 0.0926 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.28627(3) 0.0000 0.63438(5) 0.02480(18) Uani 1 2 d S . . Mn2 Mn 0.15869(3) 0.0000 0.31991(5) 0.02486(18) Uani 1 2 d S . . S1 S 0.21122(7) 0.0000 0.89446(11) 0.0504(4) Uani 1 2 d S . . S2 S -0.01367(5) 0.0000 0.30684(9) 0.0292(3) Uani 1 2 d S . . O1 O 0.13283(10) 0.07938(14) 0.21237(17) 0.0343(5) Uani 1 1 d . . . O2 O 0.37706(14) 0.0000 0.5439(3) 0.0354(8) Uani 1 2 d S . . O3 O 0.42768(17) 0.0000 0.7186(3) 0.0493(9) Uani 1 2 d S . . O6 O 0.26432(19) 0.0000 0.2617(4) 0.0797(14) Uani 1 2 d S . . H5 H 0.2776 0.0484 0.2601 0.120 Uiso 1 1 d R . . O4 O 0.20342(15) 0.0000 0.7656(3) 0.0379(8) Uani 1 2 d S . . O5 O 0.05340(13) 0.0000 0.3793(2) 0.0301(7) Uani 1 2 d S . . N1 N 0.30135(12) 0.12025(16) 0.7239(2) 0.0307(6) Uani 1 1 d . . . N2 N 0.22471(11) 0.08696(15) 0.5288(2) 0.0247(5) Uani 1 1 d . . . N3 N 0.18090(11) 0.08794(15) 0.4325(2) 0.0252(6) Uani 1 1 d . . . N4 N 0.17291(12) 0.20453(15) 0.5194(2) 0.0289(6) Uani 1 1 d . . . C1 C 0.33636(17) 0.1336(2) 0.8240(3) 0.0394(8) Uani 1 1 d . . . H1 H 0.3687 0.0968 0.8500 0.047 Uiso 1 1 calc R . . C2 C 0.32726(18) 0.1989(2) 0.8908(3) 0.0443(9) Uani 1 1 d . . . H2 H 0.3521 0.2054 0.9610 0.053 Uiso 1 1 calc R . . C3 C 0.28087(19) 0.2543(2) 0.8520(3) 0.0464(9) Uani 1 1 d . . . H3 H 0.2736 0.2989 0.8956 0.056 Uiso 1 1 calc R . . C4 C 0.24504(17) 0.2432(2) 0.7476(3) 0.0393(8) Uani 1 1 d . . . H4 H 0.2139 0.2806 0.7190 0.047 Uiso 1 1 calc R . . C5 C 0.25614(14) 0.17570(18) 0.6865(3) 0.0270(7) Uani 1 1 d . . . C6 C 0.21781(14) 0.15714(18) 0.5767(2) 0.0262(7) Uani 1 1 d . . . C7 C 0.15123(14) 0.15917(18) 0.4292(3) 0.0271(7) Uani 1 1 d . . . C8 C 0.10080(15) 0.18291(19) 0.3380(3) 0.0311(7) Uani 1 1 d . . . C9 C 0.05938(16) 0.2485(2) 0.3538(3) 0.0417(8) Uani 1 1 d . . . H9 H 0.0639 0.2763 0.4226 0.050 Uiso 1 1 calc R . . C10 C 0.01180(18) 0.2721(2) 0.2681(3) 0.0522(10) Uani 1 1 d . . . H10 H -0.0152 0.3159 0.2789 0.063 Uiso 1 1 calc R . . C11 C 0.00474(18) 0.2303(2) 0.1666(3) 0.0515(10) Uani 1 1 d . . . H11 H -0.0272 0.2461 0.1089 0.062 Uiso 1 1 calc R . . C12 C 0.04433(17) 0.1657(2) 0.1500(3) 0.0426(9) Uani 1 1 d . . . H12 H 0.0383 0.1378 0.0814 0.051 Uiso 1 1 calc R . . C13 C 0.09382(15) 0.14069(19) 0.2344(3) 0.0319(7) Uani 1 1 d . . . C14 C 0.1609(3) 0.0785(3) 0.9398(4) 0.0760(14) Uani 1 1 d . . . H14A H 0.1781 0.1272 0.9122 0.114 Uiso 1 1 calc R . . H14B H 0.1623 0.0794 1.0223 0.114 Uiso 1 1 calc R . . H14C H 0.1149 0.0714 0.9094 0.114 Uiso 1 1 calc R . . C15 C -0.06101(15) 0.0793(2) 0.3612(3) 0.0366(8) Uani 1 1 d . . . H15A H -0.0605 0.0755 0.4435 0.055 Uiso 1 1 calc R . . H15B H -0.1070 0.0768 0.3290 0.055 Uiso 1 1 calc R . . H15C H -0.0411 0.1284 0.3404 0.055 Uiso 1 1 calc R . . C16 C 0.4303(2) 0.0000 0.6128(4) 0.0327(11) Uani 1 2 d S . . C17 C 0.4982(2) 0.0000 0.5619(4) 0.0543(15) Uani 1 2 d S . . H17A H 0.5228 0.0458 0.5917 0.065 Uiso 0.50 1 calc PR . . H17B H 0.5228 -0.0458 0.5917 0.065 Uiso 0.50 1 calc PR . . O7 O 0.36890(15) 0.13937(17) 0.3998(2) 0.0695(9) Uani 1 1 d D . . H7A H 0.3522 0.1841 0.4137 0.083 Uiso 1 1 d RD . . H7B H 0.3651 0.1034 0.4495 0.083 Uiso 1 1 d RD . . O8 O 0.4688(3) 0.0000 0.1122(4) 0.109(2) Uani 1 2 d S . . H8A H 0.4543 0.0461 0.0972 0.163 Uiso 1 1 d R . . O9 O 0.3567(2) 0.1028(3) 0.1720(4) 0.1403(18) Uani 1 1 d . . . H9A H 0.3915 0.1017 0.1342 0.210 Uiso 1 1 d R . . H9B H 0.3618 0.1044 0.2442 0.210 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0178(3) 0.0324(4) 0.0242(4) 0.000 0.0014(3) 0.000 Mn2 0.0196(3) 0.0367(4) 0.0183(3) 0.000 0.0016(3) 0.000 S1 0.0444(8) 0.0796(10) 0.0277(7) 0.000 0.0052(6) 0.000 S2 0.0198(5) 0.0442(7) 0.0238(6) 0.000 0.0029(4) 0.000 O1 0.0348(12) 0.0472(14) 0.0211(11) 0.0063(10) 0.0038(9) 0.0017(11) O2 0.0189(15) 0.045(2) 0.0431(19) 0.000 0.0090(14) 0.000 O3 0.041(2) 0.068(3) 0.041(2) 0.000 0.0135(17) 0.000 O6 0.037(2) 0.111(4) 0.095(3) 0.000 0.030(2) 0.000 O4 0.0359(18) 0.052(2) 0.0273(17) 0.000 0.0098(14) 0.000 O5 0.0180(14) 0.0449(19) 0.0274(16) 0.000 0.0009(12) 0.000 N1 0.0245(13) 0.0390(15) 0.0282(14) -0.0027(12) -0.0025(11) -0.0029(11) N2 0.0203(12) 0.0317(14) 0.0216(12) 0.0000(11) -0.0020(10) -0.0017(10) N3 0.0194(12) 0.0340(15) 0.0221(13) 0.0026(11) 0.0013(10) -0.0019(11) N4 0.0279(13) 0.0295(14) 0.0292(14) 0.0023(12) 0.0013(11) -0.0012(11) C1 0.0334(18) 0.051(2) 0.0329(18) -0.0009(17) -0.0047(15) -0.0062(16) C2 0.048(2) 0.054(2) 0.0299(18) -0.0063(18) -0.0072(16) -0.0132(18) C3 0.061(2) 0.039(2) 0.040(2) -0.0096(17) 0.0025(18) -0.0117(19) C4 0.045(2) 0.0336(19) 0.0388(19) -0.0015(16) -0.0014(16) -0.0038(15) C5 0.0249(15) 0.0295(17) 0.0267(16) 0.0017(13) 0.0030(13) -0.0078(13) C6 0.0226(15) 0.0303(17) 0.0261(16) 0.0045(14) 0.0038(12) -0.0041(13) C7 0.0208(15) 0.0330(18) 0.0278(16) 0.0049(14) 0.0033(12) -0.0034(13) C8 0.0259(16) 0.0367(18) 0.0305(17) 0.0069(15) 0.0002(13) -0.0021(14) C9 0.0372(18) 0.046(2) 0.041(2) 0.0032(17) -0.0044(16) 0.0029(17) C10 0.044(2) 0.051(2) 0.059(3) 0.010(2) -0.0088(19) 0.0134(18) C11 0.039(2) 0.064(3) 0.049(2) 0.016(2) -0.0133(18) 0.0074(19) C12 0.0383(19) 0.058(2) 0.0302(18) 0.0093(17) -0.0054(15) -0.0021(18) C13 0.0254(16) 0.0421(19) 0.0283(17) 0.0115(15) 0.0028(13) -0.0041(14) C14 0.114(4) 0.070(3) 0.046(2) -0.013(2) 0.023(3) 0.003(3) C15 0.0265(16) 0.046(2) 0.0371(19) 0.0018(16) 0.0048(14) 0.0040(15) C16 0.024(2) 0.032(3) 0.044(3) 0.000 0.007(2) 0.000 C17 0.023(2) 0.097(5) 0.044(3) 0.000 0.009(2) 0.000 O7 0.085(2) 0.0549(18) 0.072(2) 0.0210(16) 0.0281(17) 0.0260(16) O8 0.085(4) 0.180(6) 0.061(3) 0.000 0.001(3) 0.000 O9 0.136(4) 0.143(4) 0.137(4) -0.024(3) -0.022(3) 0.023(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O2 2.142(3) . ? Mn1 N2 2.230(2) 6 ? Mn1 N2 2.230(2) . ? Mn1 N1 2.305(3) . ? Mn1 N1 2.305(3) 6 ? Mn1 O4 2.314(3) . ? Mn2 O1 1.888(2) 6 ? Mn2 O1 1.888(2) . ? Mn2 N3 2.017(2) . ? Mn2 N3 2.017(2) 6 ? Mn2 O5 2.237(3) . ? Mn2 O6 2.238(4) . ? S1 O4 1.498(3) . ? S1 C14 1.765(5) 6 ? S1 C14 1.765(5) . ? S2 O5 1.522(3) . ? S2 C15 1.782(3) 6 ? S2 C15 1.782(3) . ? O1 C13 1.332(4) . ? O2 C16 1.278(5) . ? O3 C16 1.237(6) . ? O6 H5 0.8636 . ? N1 C1 1.334(4) . ? N1 C5 1.350(4) . ? N2 C6 1.328(4) . ? N2 N3 1.370(3) . ? N3 C7 1.345(4) . ? N4 C6 1.342(4) . ? N4 C7 1.349(4) . ? C1 C2 1.374(5) . ? C1 H1 0.9300 . ? C2 C3 1.369(5) . ? C2 H2 0.9300 . ? C3 C4 1.377(5) . ? C3 H3 0.9300 . ? C4 C5 1.375(4) . ? C4 H4 0.9300 . ? C5 C6 1.475(4) . ? C7 C8 1.463(4) . ? C8 C13 1.402(4) . ? C8 C9 1.402(5) . ? C9 C10 1.383(5) . ? C9 H9 0.9300 . ? C10 C11 1.378(5) . ? C10 H10 0.9300 . ? C11 C12 1.369(5) . ? C11 H11 0.9300 . ? C12 C13 1.404(4) . ? C12 H12 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.504(6) . ? C17 C17 1.449(10) 5_656 ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? O7 H7A 0.8489 . ? O7 H7B 0.8484 . ? O8 H8A 0.8479 . ? O9 H9A 0.8418 . ? O9 H9B 0.8404 . ? 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 O2 Mn1 N2 99.94(9) . 6 ? O2 Mn1 N2 99.94(9) . . ? N2 Mn1 N2 83.05(12) 6 . ? O2 Mn1 N1 97.80(7) . . ? N2 Mn1 N1 152.39(9) 6 . ? N2 Mn1 N1 73.14(9) . . ? O2 Mn1 N1 97.80(7) . 6 ? N2 Mn1 N1 73.14(9) 6 6 ? N2 Mn1 N1 152.39(9) . 6 ? N1 Mn1 N1 125.00(13) . 6 ? O2 Mn1 O4 168.20(11) . . ? N2 Mn1 O4 88.85(8) 6 . ? N2 Mn1 O4 88.85(8) . . ? N1 Mn1 O4 77.11(7) . . ? N1 Mn1 O4 77.11(7) 6 . ? O1 Mn2 O1 91.27(14) 6 . ? O1 Mn2 N3 176.56(10) 6 . ? O1 Mn2 N3 86.46(9) . . ? O1 Mn2 N3 86.46(9) 6 6 ? O1 Mn2 N3 176.56(10) . 6 ? N3 Mn2 N3 95.68(14) . 6 ? O1 Mn2 O5 89.41(8) 6 . ? O1 Mn2 O5 89.41(8) . . ? N3 Mn2 O5 87.98(8) . . ? N3 Mn2 O5 87.98(8) 6 . ? O1 Mn2 O6 90.86(10) 6 . ? O1 Mn2 O6 90.86(11) . . ? N3 Mn2 O6 91.76(10) . . ? N3 Mn2 O6 91.76(10) 6 . ? O5 Mn2 O6 179.61(14) . . ? O4 S1 C14 106.12(17) . 6 ? O4 S1 C14 106.12(17) . . ? C14 S1 C14 98.1(3) 6 . ? O5 S2 C15 105.15(13) . 6 ? O5 S2 C15 105.15(13) . . ? C15 S2 C15 98.4(2) 6 . ? C13 O1 Mn2 124.45(18) . . ? C16 O2 Mn1 111.8(3) . . ? Mn2 O6 H5 107.4 . . ? S1 O4 Mn1 129.21(18) . . ? S2 O5 Mn2 128.45(17) . . ? C1 N1 C5 117.1(3) . . ? C1 N1 Mn1 126.1(2) . . ? C5 N1 Mn1 114.28(18) . . ? C6 N2 N3 104.8(2) . . ? C6 N2 Mn1 115.61(18) . . ? N3 N2 Mn1 138.61(19) . . ? C7 N3 N2 106.5(2) . . ? C7 N3 Mn2 125.02(19) . . ? N2 N3 Mn2 128.37(19) . . ? C6 N4 C7 102.0(2) . . ? N1 C1 C2 123.5(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 119.4(3) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 118.7(3) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? N1 C5 C4 122.7(3) . . ? N1 C5 C6 114.8(3) . . ? C4 C5 C6 122.4(3) . . ? N2 C6 N4 114.5(3) . . ? N2 C6 C5 119.6(3) . . ? N4 C6 C5 125.9(3) . . ? N3 C7 N4 112.2(2) . . ? N3 C7 C8 122.9(3) . . ? N4 C7 C8 124.9(3) . . ? C13 C8 C9 119.7(3) . . ? C13 C8 C7 120.4(3) . . ? C9 C8 C7 119.9(3) . . ? C10 C9 C8 120.7(3) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C11 C10 C9 119.5(4) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C12 C11 C10 120.6(3) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C13 121.4(3) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? O1 C13 C8 122.8(3) . . ? O1 C13 C12 119.1(3) . . ? C8 C13 C12 118.0(3) . . ? S1 C14 H14A 109.5 . . ? S1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? S1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? S2 C15 H15A 109.5 . . ? S2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? S2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O3 C16 O2 122.5(4) . . ? O3 C16 C17 119.4(4) . . ? O2 C16 C17 118.1(4) . . ? C17 C17 C16 119.8(5) 5_656 . ? C17 C17 H17A 107.4 5_656 . ? C16 C17 H17A 107.4 . . ? C17 C17 H17B 107.4 5_656 . ? C16 C17 H17B 107.4 . . ? H17A C17 H17B 106.9 . . ? H7A O7 H7B 117.4 . . ? H9A O9 H9B 118.5 . . ? 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 O1 Mn2 O1 C13 131.0(2) 6 . . . ? N3 Mn2 O1 C13 -46.4(2) . . . . ? N3 Mn2 O1 C13 82.3(17) 6 . . . ? O5 Mn2 O1 C13 41.6(2) . . . . ? O6 Mn2 O1 C13 -138.1(2) . . . . ? N2 Mn1 O2 C16 -137.69(6) 6 . . . ? N2 Mn1 O2 C16 137.69(6) . . . . ? N1 Mn1 O2 C16 63.55(7) . . . . ? N1 Mn1 O2 C16 -63.55(7) 6 . . . ? O4 Mn1 O2 C16 0.000(1) . . . . ? C14 S1 O4 Mn1 -128.15(18) 6 . . . ? C14 S1 O4 Mn1 128.15(18) . . . . ? O2 Mn1 O4 S1 0.000(1) . . . . ? N2 Mn1 O4 S1 138.46(6) 6 . . . ? N2 Mn1 O4 S1 -138.46(6) . . . . ? N1 Mn1 O4 S1 -65.50(7) . . . . ? N1 Mn1 O4 S1 65.50(7) 6 . . . ? C15 S2 O5 Mn2 128.36(12) 6 . . . ? C15 S2 O5 Mn2 -128.36(12) . . . . ? O1 Mn2 O5 S2 -45.64(7) 6 . . . ? O1 Mn2 O5 S2 45.64(7) . . . . ? N3 Mn2 O5 S2 132.12(7) . . . . ? N3 Mn2 O5 S2 -132.12(7) 6 . . . ? O6 Mn2 O5 S2 180.00(2) . . . . ? O2 Mn1 N1 C1 -86.3(3) . . . . ? N2 Mn1 N1 C1 144.1(2) 6 . . . ? N2 Mn1 N1 C1 175.6(3) . . . . ? N1 Mn1 N1 C1 19.0(3) 6 . . . ? O4 Mn1 N1 C1 82.9(3) . . . . ? O2 Mn1 N1 C5 112.4(2) . . . . ? N2 Mn1 N1 C5 -17.3(3) 6 . . . ? N2 Mn1 N1 C5 14.3(2) . . . . ? N1 Mn1 N1 C5 -142.39(16) 6 . . . ? O4 Mn1 N1 C5 -78.5(2) . . . . ? O2 Mn1 N2 C6 -106.0(2) . . . . ? N2 Mn1 N2 C6 155.04(16) 6 . . . ? N1 Mn1 N2 C6 -10.82(19) . . . . ? N1 Mn1 N2 C6 124.7(2) 6 . . . ? O4 Mn1 N2 C6 66.1(2) . . . . ? O2 Mn1 N2 N3 87.5(3) . . . . ? N2 Mn1 N2 N3 -11.5(3) 6 . . . ? N1 Mn1 N2 N3 -177.3(3) . . . . ? N1 Mn1 N2 N3 -41.8(4) 6 . . . ? O4 Mn1 N2 N3 -100.5(3) . . . . ? C6 N2 N3 C7 0.5(3) . . . . ? Mn1 N2 N3 C7 167.9(2) . . . . ? C6 N2 N3 Mn2 -176.07(19) . . . . ? Mn1 N2 N3 Mn2 -8.6(4) . . . . ? O1 Mn2 N3 C7 -21.3(17) 6 . . . ? O1 Mn2 N3 C7 27.5(2) . . . . ? N3 Mn2 N3 C7 -149.80(19) 6 . . . ? O5 Mn2 N3 C7 -62.0(2) . . . . ? O6 Mn2 N3 C7 118.3(2) . . . . ? O1 Mn2 N3 N2 154.6(15) 6 . . . ? O1 Mn2 N3 N2 -156.6(2) . . . . ? N3 Mn2 N3 N2 26.1(3) 6 . . . ? O5 Mn2 N3 N2 113.9(2) . . . . ? O6 Mn2 N3 N2 -65.8(2) . . . . ? C5 N1 C1 C2 1.8(5) . . . . ? Mn1 N1 C1 C2 -159.1(3) . . . . ? N1 C1 C2 C3 -1.4(5) . . . . ? C1 C2 C3 C4 -0.2(5) . . . . ? C2 C3 C4 C5 1.3(5) . . . . ? C1 N1 C5 C4 -0.7(4) . . . . ? Mn1 N1 C5 C4 162.5(2) . . . . ? C1 N1 C5 C6 -178.7(3) . . . . ? Mn1 N1 C5 C6 -15.6(3) . . . . ? C3 C4 C5 N1 -0.8(5) . . . . ? C3 C4 C5 C6 177.1(3) . . . . ? N3 N2 C6 N4 -0.1(3) . . . . ? Mn1 N2 C6 N4 -170.91(18) . . . . ? N3 N2 C6 C5 177.6(2) . . . . ? Mn1 N2 C6 C5 6.8(3) . . . . ? C7 N4 C6 N2 -0.3(3) . . . . ? C7 N4 C6 C5 -177.8(3) . . . . ? N1 C5 C6 N2 6.3(4) . . . . ? C4 C5 C6 N2 -171.7(3) . . . . ? N1 C5 C6 N4 -176.3(3) . . . . ? C4 C5 C6 N4 5.7(5) . . . . ? N2 N3 C7 N4 -0.7(3) . . . . ? Mn2 N3 C7 N4 175.98(18) . . . . ? N2 N3 C7 C8 180.0(3) . . . . ? Mn2 N3 C7 C8 -3.3(4) . . . . ? C6 N4 C7 N3 0.6(3) . . . . ? C6 N4 C7 C8 179.9(3) . . . . ? N3 C7 C8 C13 -16.7(4) . . . . ? N4 C7 C8 C13 164.1(3) . . . . ? N3 C7 C8 C9 163.6(3) . . . . ? N4 C7 C8 C9 -15.6(5) . . . . ? C13 C8 C9 C10 -0.2(5) . . . . ? C7 C8 C9 C10 179.5(3) . . . . ? C8 C9 C10 C11 0.5(6) . . . . ? C9 C10 C11 C12 0.0(6) . . . . ? C10 C11 C12 C13 -1.0(6) . . . . ? Mn2 O1 C13 C8 41.7(4) . . . . ? Mn2 O1 C13 C12 -139.7(3) . . . . ? C9 C8 C13 O1 177.9(3) . . . . ? C7 C8 C13 O1 -1.8(4) . . . . ? C9 C8 C13 C12 -0.7(4) . . . . ? C7 C8 C13 C12 179.6(3) . . . . ? C11 C12 C13 O1 -177.4(3) . . . . ? C11 C12 C13 C8 1.3(5) . . . . ? Mn1 O2 C16 O3 0.0 . . . . ? Mn1 O2 C16 C17 180.0 . . . . ? O3 C16 C17 C17 180.0 . . . 5_656 ? O2 C16 C17 C17 0.000(1) . . . 5_656 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.448 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.067 # Attachment '7.cif' data_r71223d _database_code_depnum_ccdc_archive 'CCDC 690531' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H76 Mn4 N18 O20' _chemical_formula_weight 1685.23 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' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.473(3) _cell_length_b 15.913(3) _cell_length_c 18.590(4) _cell_angle_alpha 94.98(3) _cell_angle_beta 110.50(3) _cell_angle_gamma 112.14(3) _cell_volume 3594.1(12) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 10050 _cell_measurement_theta_min 1.428 _cell_measurement_theta_max 32.726 _exptl_crystal_description block _exptl_crystal_colour dark-green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1740 _exptl_absorpt_coefficient_mu 0.774 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9128 _exptl_absorpt_correction_T_max 0.9407 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'rigaku saturn' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 22147 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.02 _reflns_number_total 12613 _reflns_number_gt 11073 _reflns_threshold_expression >2sigma(I) _computing_data_collection crystalclear _computing_cell_refinement crystalclear _computing_data_reduction crystalclear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+2.9849P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12613 _refine_ls_number_parameters 1007 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1143 _refine_ls_wR_factor_gt 0.1070 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.365 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn -0.01609(6) 0.73127(5) 0.99224(4) 0.01737(18) Uani 1 1 d . . . Mn2 Mn 0.21383(6) 0.79748(4) 0.90382(4) 0.01377(18) Uani 1 1 d . . . Mn3 Mn 0.35081(5) 0.82196(4) 0.64244(4) 0.01233(17) Uani 1 1 d . . . Mn4 Mn 0.04393(5) 0.76061(4) 0.46147(4) 0.01235(17) Uani 1 1 d . . . O1 O 0.2762(3) 0.7320(2) 0.86447(18) 0.0177(7) Uani 1 1 d . . . O2 O 0.2422(3) 0.8817(2) 0.83911(18) 0.0168(7) Uani 1 1 d . . . O3 O -0.1924(3) 0.6674(3) 0.9663(2) 0.0266(8) Uani 1 1 d D . . H3A H -0.2195 0.7067 0.9488 0.040 Uiso 1 1 d RD . . H3B H -0.2285 0.6131 0.9333 0.040 Uiso 1 1 d RD . . O4 O 0.4019(3) 0.8880(2) 1.00467(19) 0.0216(7) Uani 1 1 d D . . H4A H 0.4351 0.8564 1.0258 0.032 Uiso 1 1 d RD . . H4B H 0.4213 0.9413 1.0342 0.032 Uiso 1 1 d RD . . O5 O -0.0807(3) 0.7125(3) 0.8674(2) 0.0298(9) Uani 1 1 d . . . O6 O 0.0467(3) 0.7185(2) 0.82329(19) 0.0198(7) Uani 1 1 d . . . O7 O -0.0003(3) 0.7448(2) 0.55950(18) 0.0167(7) Uani 1 1 d . . . O8 O -0.1600(3) 0.7222(2) 0.46651(18) 0.0186(7) Uani 1 1 d . . . O9 O 0.4197(3) 0.7519(2) 0.69698(18) 0.0163(7) Uani 1 1 d . . . O10 O 0.4520(3) 0.9256(2) 0.73043(18) 0.0156(7) Uani 1 1 d . . . O11 O 0.2151(3) 0.7919(2) 0.68754(19) 0.0171(7) Uani 1 1 d D . . H11A H 0.2410 0.8252 0.7324 0.026 Uiso 1 1 calc RD . . H11B H 0.1498(19) 0.778(4) 0.6553(18) 0.041(19) Uiso 1 1 d D . . O12 O 0.1015(3) 0.7770(2) 0.36093(19) 0.0206(7) Uani 1 1 d D . . H12A H 0.131(5) 0.741(4) 0.359(4) 0.044(19) Uiso 1 1 d D . . O13 O 0.4704(3) 0.8644(2) 0.58401(19) 0.0213(7) Uani 1 1 d . . . O14 O 0.1975(3) 0.6709(3) 0.3452(2) 0.0338(9) Uani 1 1 d . . . O15 O 0.6268(4) 0.8656(3) 0.8230(3) 0.0587(14) Uani 1 1 d D . . H15A H 0.5688 0.8387 0.7809 0.088 Uiso 1 1 d RD . . H15B H 0.6628 0.8167 0.8252 0.088 Uiso 1 1 d RD . . O16 O 0.6630(3) 0.7543(2) 0.3791(2) 0.0242(8) Uani 1 1 d D . . H16A H 0.6744 0.8107 0.3937 0.036 Uiso 1 1 d RD . . H16B H 0.7126 0.7392 0.4046 0.036 Uiso 1 1 d RD . . O17 O 0.6989(3) 0.4940(3) 0.8589(2) 0.0336(9) Uani 1 1 d . . . H17A H 0.7299 0.4670 0.8859 0.050 Uiso 1 1 d RD . . H17B H 0.6265 0.4533 0.8249 0.050 Uiso 1 1 d RD . . O18 O 0.4796(3) 0.3602(3) 0.7731(3) 0.0435(11) Uani 1 1 d . . . H18 H 0.4446 0.3226 0.7294 0.065 Uiso 1 1 calc R . . O19 O 0.7471(4) 0.7944(3) 0.9145(3) 0.0503(12) Uani 1 1 d D . . H19A H 0.8307 0.8004 0.9454 0.075 Uiso 1 1 d RD . . H19B H 0.6874 0.7587 0.9426 0.075 Uiso 1 1 d RD . . O20 O 0.4857(3) 0.0638(2) 0.1014(2) 0.0235(7) Uani 1 1 d D . . H20A H 0.5182 0.0696 0.1513 0.035 Uiso 1 1 d RD . . H20B H 0.5275 0.0909 0.0796 0.035 Uiso 1 1 d RD . . N1 N -0.0169(3) 0.6265(3) 1.0730(2) 0.0195(8) Uani 1 1 d . . . N2 N 0.1160(3) 0.6891(3) 1.0029(2) 0.0163(8) Uani 1 1 d . . . N3 N 0.1920(3) 0.7083(3) 0.9717(2) 0.0155(8) Uani 1 1 d . . . N4 N 0.2086(3) 0.6036(3) 1.0413(2) 0.0184(8) Uani 1 1 d . . . N5 N -0.0104(3) 0.8582(3) 1.0748(2) 0.0199(9) Uani 1 1 d . . . N6 N 0.1157(3) 0.8659(3) 1.0002(2) 0.0179(8) Uani 1 1 d . . . N7 N 0.1785(3) 0.8871(3) 0.9581(2) 0.0156(8) Uani 1 1 d . . . N8 N 0.1854(3) 1.0203(3) 1.0122(2) 0.0170(8) Uani 1 1 d D . . H8A H 0.1727 1.0708 1.0210 0.020 Uiso 1 1 d RD . . N9 N -0.0609(3) 0.6112(3) 0.3899(2) 0.0149(8) Uani 1 1 d . . . N10 N 0.1458(3) 0.6867(2) 0.5026(2) 0.0134(8) Uani 1 1 d . . . N11 N 0.2471(3) 0.7038(2) 0.5573(2) 0.0131(8) Uani 1 1 d . . . N12 N 0.1642(3) 0.5535(2) 0.4902(2) 0.0146(8) Uani 1 1 d . . . H12 H 0.1506 0.4962 0.4735 0.018 Uiso 1 1 calc R . . N13 N 0.0101(3) 0.8835(3) 0.4292(2) 0.0151(8) Uani 1 1 d . . . N14 N 0.1966(3) 0.8894(2) 0.5341(2) 0.0132(8) Uani 1 1 d . . . N15 N 0.2973(3) 0.9124(2) 0.5917(2) 0.0131(8) Uani 1 1 d . . . N16 N 0.2891(3) 1.0464(2) 0.5709(2) 0.0138(8) Uani 1 1 d . . . N17 N 0.6539(3) 0.9576(3) 0.6328(3) 0.0271(10) Uani 1 1 d . . . N18 N 0.3435(4) 0.6384(3) 0.3966(3) 0.0247(9) Uani 1 1 d . . . C1 C -0.0877(4) 0.5958(3) 1.1059(3) 0.0245(11) Uani 1 1 d . . . H1 H -0.1417 0.6168 1.0964 0.029 Uiso 1 1 calc R . . C2 C -0.0841(5) 0.5335(3) 1.1540(3) 0.0270(12) Uani 1 1 d . . . H2 H -0.1336 0.5150 1.1772 0.032 Uiso 1 1 calc R . . C3 C -0.0070(5) 0.5000(3) 1.1666(3) 0.0269(12) Uani 1 1 d . . . H3 H -0.0035 0.4582 1.1983 0.032 Uiso 1 1 calc R . . C4 C 0.0659(4) 0.5294(3) 1.1315(3) 0.0249(11) Uani 1 1 d . . . H4 H 0.1190 0.5075 1.1391 0.030 Uiso 1 1 calc R . . C5 C 0.0582(4) 0.5919(3) 1.0849(3) 0.0186(10) Uani 1 1 d . . . C6 C 0.1300(4) 0.6272(3) 1.0440(3) 0.0178(10) Uani 1 1 d . . . C7 C 0.2451(4) 0.6554(3) 0.9943(3) 0.0161(9) Uani 1 1 d . . . C8 C 0.3265(4) 0.6520(3) 0.9665(3) 0.0175(10) Uani 1 1 d . . . C9 C 0.3910(4) 0.6063(3) 0.9992(3) 0.0227(11) Uani 1 1 d . . . H9 H 0.3825 0.5787 1.0399 0.027 Uiso 1 1 calc R . . C10 C 0.4664(4) 0.6013(3) 0.9725(3) 0.0260(11) Uani 1 1 d . . . H10 H 0.5084 0.5706 0.9952 0.031 Uiso 1 1 calc R . . C11 C 0.4799(4) 0.6423(3) 0.9114(3) 0.0234(11) Uani 1 1 d . . . H11 H 0.5314 0.6395 0.8936 0.028 Uiso 1 1 calc R . . C12 C 0.4166(4) 0.6871(3) 0.8773(3) 0.0188(10) Uani 1 1 d . . . H12B H 0.4263 0.7144 0.8367 0.023 Uiso 1 1 calc R . . C13 C 0.3381(4) 0.6919(3) 0.9030(3) 0.0165(9) Uani 1 1 d . . . C14 C -0.0712(4) 0.8511(4) 1.1162(3) 0.0226(11) Uani 1 1 d . . . H14 H -0.1201 0.7916 1.1138 0.027 Uiso 1 1 calc R . . C15 C -0.0651(4) 0.9275(4) 1.1624(3) 0.0235(11) Uani 1 1 d . . . H15 H -0.1079 0.9193 1.1910 0.028 Uiso 1 1 calc R . . C16 C 0.0058(4) 1.0165(4) 1.1653(3) 0.0250(11) Uani 1 1 d . . . H16 H 0.0109 1.0691 1.1956 0.030 Uiso 1 1 calc R . . C17 C 0.0691(4) 1.0265(4) 1.1227(3) 0.0215(10) Uani 1 1 d . . . H17 H 0.1171 1.0856 1.1235 0.026 Uiso 1 1 calc R . . C18 C 0.0594(4) 0.9458(3) 1.0784(3) 0.0178(10) Uani 1 1 d . . . C19 C 0.1222(4) 0.9469(3) 1.0311(3) 0.0161(9) Uani 1 1 d . . . C20 C 0.2188(4) 0.9799(3) 0.9658(3) 0.0156(9) Uani 1 1 d . . . C21 C 0.2812(4) 1.0274(3) 0.9229(3) 0.0154(9) Uani 1 1 d . . . C22 C 0.3323(4) 1.1255(3) 0.9404(3) 0.0209(10) Uani 1 1 d . . . H22 H 0.3327 1.1601 0.9836 0.025 Uiso 1 1 calc R . . C23 C 0.3822(4) 1.1725(3) 0.8952(3) 0.0229(11) Uani 1 1 d . . . H23 H 0.4164 1.2376 0.9082 0.027 Uiso 1 1 calc R . . C24 C 0.3805(4) 1.1210(3) 0.8301(3) 0.0219(10) Uani 1 1 d . . . H24 H 0.4117 1.1518 0.7983 0.026 Uiso 1 1 calc R . . C25 C 0.3326(4) 1.0241(3) 0.8123(3) 0.0177(10) Uani 1 1 d . . . H25 H 0.3324 0.9905 0.7687 0.021 Uiso 1 1 calc R . . C26 C 0.2843(4) 0.9756(3) 0.8589(3) 0.0147(9) Uani 1 1 d . . . C27 C -0.0447(4) 0.7150(3) 0.8148(3) 0.0185(10) Uani 1 1 d . . . C28 C -0.1194(4) 0.7120(3) 0.7332(3) 0.0166(9) Uani 1 1 d . . . C29 C -0.2243(4) 0.7045(3) 0.7162(3) 0.0220(10) Uani 1 1 d . . . H29 H -0.2501 0.7013 0.7556 0.026 Uiso 1 1 calc R . . C30 C -0.2901(4) 0.7019(4) 0.6403(3) 0.0243(11) Uani 1 1 d . . . H30 H -0.3603 0.6965 0.6289 0.029 Uiso 1 1 calc R . . C31 C -0.2524(4) 0.7074(3) 0.5811(3) 0.0202(10) Uani 1 1 d . . . H31 H -0.2973 0.7053 0.5303 0.024 Uiso 1 1 calc R . . C32 C -0.1469(4) 0.7159(3) 0.5976(3) 0.0147(9) Uani 1 1 d . . . C33 C -0.0820(4) 0.7173(3) 0.6735(3) 0.0162(9) Uani 1 1 d . . . H33 H -0.0122 0.7219 0.6846 0.019 Uiso 1 1 calc R . . C34 C -0.1012(4) 0.7271(3) 0.5361(3) 0.0148(9) Uani 1 1 d . . . C35 C -0.1647(4) 0.5758(3) 0.3357(3) 0.0171(10) Uani 1 1 d . . . H35 H -0.1996 0.6149 0.3276 0.021 Uiso 1 1 calc R . . C36 C -0.2224(4) 0.4836(3) 0.2911(3) 0.0174(10) Uani 1 1 d . . . H36 H -0.2941 0.4615 0.2535 0.021 Uiso 1 1 calc R . . C37 C -0.1709(4) 0.4250(3) 0.3037(3) 0.0181(10) Uani 1 1 d . . . H37 H -0.2074 0.3629 0.2743 0.022 Uiso 1 1 calc R . . C38 C -0.0643(4) 0.4602(3) 0.3607(3) 0.0171(10) Uani 1 1 d . . . H38 H -0.0286 0.4218 0.3710 0.021 Uiso 1 1 calc R . . C39 C -0.0116(4) 0.5537(3) 0.4023(3) 0.0152(9) Uani 1 1 d . . . C40 C 0.1001(4) 0.5965(3) 0.4644(3) 0.0138(9) Uani 1 1 d . . . C41 C 0.2542(4) 0.6210(3) 0.5483(3) 0.0134(9) Uani 1 1 d . . . C42 C 0.3466(4) 0.6068(3) 0.5991(3) 0.0139(9) Uani 1 1 d . . . C43 C 0.3522(4) 0.5227(3) 0.5787(3) 0.0176(10) Uani 1 1 d . . . H43 H 0.3008 0.4797 0.5306 0.021 Uiso 1 1 calc R . . C44 C 0.4326(4) 0.5021(3) 0.6287(3) 0.0218(10) Uani 1 1 d . . . H44 H 0.4355 0.4459 0.6146 0.026 Uiso 1 1 calc R . . C45 C 0.5088(4) 0.5666(3) 0.7001(3) 0.0213(10) Uani 1 1 d . . . H45 H 0.5631 0.5533 0.7343 0.026 Uiso 1 1 calc R . . C46 C 0.5056(4) 0.6506(3) 0.7216(3) 0.0174(9) Uani 1 1 d . . . H46 H 0.5582 0.6933 0.7695 0.021 Uiso 1 1 calc R . . C47 C 0.4234(4) 0.6719(3) 0.6715(3) 0.0144(9) Uani 1 1 d . . . C48 C -0.0839(4) 0.8766(3) 0.3746(3) 0.0165(9) Uani 1 1 d . . . H48 H -0.1433 0.8178 0.3516 0.020 Uiso 1 1 calc R . . C49 C -0.0966(4) 0.9533(3) 0.3508(3) 0.0179(10) Uani 1 1 d . . . H49 H -0.1630 0.9463 0.3128 0.021 Uiso 1 1 calc R . . C50 C -0.0076(4) 1.0408(3) 0.3851(3) 0.0210(10) Uani 1 1 d . . . H50 H -0.0133 1.0934 0.3701 0.025 Uiso 1 1 calc R . . C51 C 0.0896(4) 1.0490(3) 0.4418(3) 0.0185(10) Uani 1 1 d . . . H51 H 0.1499 1.1073 0.4655 0.022 Uiso 1 1 calc R . . C52 C 0.0962(4) 0.9694(3) 0.4630(3) 0.0145(9) Uani 1 1 d . . . C53 C 0.1952(4) 0.9703(3) 0.5230(3) 0.0136(9) Uani 1 1 d . . . C54 C 0.3509(4) 1.0071(3) 0.6133(3) 0.0145(9) Uani 1 1 d . . . C55 C 0.4615(4) 1.0595(3) 0.6758(3) 0.0145(9) Uani 1 1 d . . . C56 C 0.5221(4) 1.1551(3) 0.6832(3) 0.0197(10) Uani 1 1 d . . . H56 H 0.4922 1.1841 0.6465 0.024 Uiso 1 1 calc R . . C57 C 0.6250(4) 1.2069(3) 0.7437(3) 0.0235(11) Uani 1 1 d . . . H57 H 0.6636 1.2703 0.7483 0.028 Uiso 1 1 calc R . . C58 C 0.6702(4) 1.1629(3) 0.7978(3) 0.0243(11) Uani 1 1 d . . . H58 H 0.7396 1.1973 0.8388 0.029 Uiso 1 1 calc R . . C59 C 0.6132(4) 1.0688(3) 0.7916(3) 0.0199(10) Uani 1 1 d . . . H59 H 0.6450 1.0403 0.8278 0.024 Uiso 1 1 calc R . . C60 C 0.5078(4) 1.0158(3) 0.7311(3) 0.0150(9) Uani 1 1 d . . . C61 C 0.0372(5) 0.7739(4) 0.2820(3) 0.0307(12) Uani 1 1 d . . . H61A H -0.0330 0.7206 0.2624 0.046 Uiso 1 1 calc R . . H61B H 0.0739 0.7688 0.2488 0.046 Uiso 1 1 calc R . . H61C H 0.0272 0.8302 0.2813 0.046 Uiso 1 1 calc R . . C62 C 0.5678(4) 0.8849(4) 0.6286(3) 0.0234(11) Uani 1 1 d . . . H62 H 0.5801 0.8456 0.6612 0.028 Uiso 1 1 calc R . . C63 C 0.6412(5) 1.0253(4) 0.5873(4) 0.0412(15) Uani 1 1 d . . . H63A H 0.5829 0.9930 0.5354 0.062 Uiso 1 1 calc R . . H63B H 0.7083 1.0597 0.5823 0.062 Uiso 1 1 calc R . . H63C H 0.6241 1.0679 0.6139 0.062 Uiso 1 1 calc R . . C64 C 0.7626(5) 0.9779(5) 0.6915(4) 0.0460(16) Uani 1 1 d . . . H64A H 0.7904 1.0353 0.7303 0.069 Uiso 1 1 calc R . . H64B H 0.8110 0.9842 0.6657 0.069 Uiso 1 1 calc R . . H64C H 0.7581 0.9277 0.7172 0.069 Uiso 1 1 calc R . . C65 C 0.2924(5) 0.6926(4) 0.3929(3) 0.0264(12) Uani 1 1 d . . . H65 H 0.3308 0.7512 0.4287 0.032 Uiso 1 1 calc R . . C66 C 0.4557(4) 0.6695(4) 0.4521(3) 0.0319(12) Uani 1 1 d . . . H66A H 0.5012 0.6772 0.4237 0.048 Uiso 1 1 calc R . . H66B H 0.4608 0.6237 0.4818 0.048 Uiso 1 1 calc R . . H66C H 0.4798 0.7283 0.4878 0.048 Uiso 1 1 calc R . . C67 C 0.2872(5) 0.5443(4) 0.3445(4) 0.0416(15) Uani 1 1 d . . . H67A H 0.2097 0.5255 0.3215 0.062 Uiso 1 1 calc R . . H67B H 0.3027 0.5014 0.3745 0.062 Uiso 1 1 calc R . . H67C H 0.3123 0.5439 0.3030 0.062 Uiso 1 1 calc R . . C68 C 0.4081(5) 0.3841(5) 0.7966(4) 0.0427(15) Uani 1 1 d . . . H68A H 0.4463 0.4194 0.8511 0.064 Uiso 1 1 calc R . . H68B H 0.3464 0.3280 0.7909 0.064 Uiso 1 1 calc R . . H68C H 0.3829 0.4212 0.7638 0.064 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0180(4) 0.0194(4) 0.0136(4) 0.0051(3) 0.0076(3) 0.0059(3) Mn2 0.0173(4) 0.0123(3) 0.0133(4) 0.0047(3) 0.0074(3) 0.0068(3) Mn3 0.0119(4) 0.0104(3) 0.0124(3) 0.0013(3) 0.0031(3) 0.0047(3) Mn4 0.0126(4) 0.0105(3) 0.0122(3) 0.0022(3) 0.0039(3) 0.0046(3) O1 0.0227(19) 0.0194(16) 0.0144(16) 0.0060(13) 0.0071(14) 0.0127(14) O2 0.0236(19) 0.0122(15) 0.0158(16) 0.0047(13) 0.0090(14) 0.0079(14) O3 0.022(2) 0.0310(19) 0.0229(19) 0.0057(15) 0.0103(16) 0.0071(16) O4 0.0219(19) 0.0191(16) 0.0188(17) 0.0033(14) 0.0034(15) 0.0088(15) O5 0.021(2) 0.048(2) 0.0160(18) 0.0103(16) 0.0089(16) 0.0095(17) O6 0.0182(19) 0.0202(17) 0.0171(17) 0.0055(13) 0.0039(15) 0.0073(14) O7 0.0141(18) 0.0195(16) 0.0166(16) 0.0039(13) 0.0072(14) 0.0068(14) O8 0.0215(18) 0.0190(16) 0.0165(17) 0.0056(13) 0.0078(15) 0.0101(14) O9 0.0186(18) 0.0140(15) 0.0147(16) 0.0009(13) 0.0030(14) 0.0096(14) O10 0.0172(17) 0.0124(15) 0.0125(16) 0.0018(12) 0.0036(14) 0.0045(13) O11 0.0156(19) 0.0184(16) 0.0149(16) 0.0026(13) 0.0053(15) 0.0061(14) O12 0.024(2) 0.0248(18) 0.0157(17) 0.0071(14) 0.0090(15) 0.0125(16) O13 0.0165(19) 0.0271(18) 0.0185(17) 0.0020(14) 0.0075(15) 0.0082(15) O14 0.036(2) 0.045(2) 0.035(2) 0.0142(18) 0.020(2) 0.026(2) O15 0.066(3) 0.040(3) 0.046(3) 0.002(2) -0.003(3) 0.026(2) O16 0.0200(19) 0.0178(17) 0.0292(19) 0.0032(14) 0.0031(16) 0.0097(15) O17 0.032(2) 0.030(2) 0.036(2) 0.0191(17) 0.0085(18) 0.0142(18) O18 0.038(3) 0.039(2) 0.036(2) -0.0054(19) -0.004(2) 0.019(2) O19 0.059(3) 0.036(2) 0.055(3) 0.006(2) 0.027(3) 0.017(2) O20 0.0225(19) 0.0262(18) 0.0190(18) 0.0062(14) 0.0078(16) 0.0084(15) N1 0.022(2) 0.0161(19) 0.0131(19) 0.0019(15) 0.0067(18) 0.0020(17) N2 0.017(2) 0.0147(18) 0.0135(19) 0.0036(15) 0.0065(17) 0.0030(16) N3 0.016(2) 0.0146(18) 0.0142(19) 0.0048(15) 0.0065(17) 0.0049(16) N4 0.022(2) 0.0136(18) 0.015(2) 0.0036(15) 0.0054(18) 0.0049(17) N5 0.018(2) 0.025(2) 0.017(2) 0.0073(17) 0.0075(18) 0.0095(18) N6 0.021(2) 0.019(2) 0.017(2) 0.0059(16) 0.0113(18) 0.0094(17) N7 0.018(2) 0.0157(19) 0.0149(19) 0.0054(15) 0.0088(17) 0.0063(16) N8 0.020(2) 0.0164(19) 0.018(2) 0.0033(16) 0.0082(18) 0.0108(17) N9 0.012(2) 0.0153(18) 0.0150(19) 0.0021(15) 0.0047(17) 0.0053(16) N10 0.012(2) 0.0130(18) 0.0125(19) 0.0020(15) 0.0030(16) 0.0043(16) N11 0.013(2) 0.0133(18) 0.0138(19) 0.0042(15) 0.0048(16) 0.0063(16) N12 0.017(2) 0.0096(17) 0.0156(19) 0.0015(15) 0.0061(17) 0.0057(16) N13 0.015(2) 0.0160(19) 0.0158(19) 0.0046(15) 0.0068(17) 0.0074(16) N14 0.013(2) 0.0128(18) 0.0130(19) 0.0032(15) 0.0055(16) 0.0051(16) N15 0.011(2) 0.0131(18) 0.0120(18) 0.0022(15) 0.0026(16) 0.0043(15) N16 0.013(2) 0.0117(18) 0.0140(19) 0.0024(15) 0.0044(16) 0.0040(16) N17 0.014(2) 0.034(2) 0.027(2) 0.0012(19) 0.0081(19) 0.0054(19) N18 0.029(3) 0.027(2) 0.025(2) 0.0066(18) 0.014(2) 0.016(2) C1 0.026(3) 0.023(2) 0.019(3) 0.002(2) 0.010(2) 0.004(2) C2 0.036(3) 0.016(2) 0.019(3) 0.001(2) 0.015(2) -0.001(2) C3 0.039(3) 0.016(2) 0.020(3) 0.006(2) 0.015(2) 0.004(2) C4 0.034(3) 0.015(2) 0.018(3) 0.0048(19) 0.009(2) 0.006(2) C5 0.020(3) 0.013(2) 0.012(2) 0.0000(18) 0.003(2) 0.001(2) C6 0.020(3) 0.013(2) 0.010(2) -0.0001(17) 0.002(2) 0.0018(19) C7 0.019(3) 0.010(2) 0.014(2) 0.0034(17) 0.004(2) 0.0035(19) C8 0.018(3) 0.011(2) 0.016(2) 0.0005(18) 0.003(2) 0.0043(19) C9 0.028(3) 0.016(2) 0.023(3) 0.009(2) 0.008(2) 0.010(2) C10 0.031(3) 0.024(3) 0.026(3) 0.008(2) 0.009(2) 0.018(2) C11 0.027(3) 0.023(2) 0.023(3) 0.004(2) 0.010(2) 0.015(2) C12 0.022(3) 0.015(2) 0.016(2) 0.0008(18) 0.006(2) 0.007(2) C13 0.019(3) 0.010(2) 0.013(2) -0.0014(17) 0.001(2) 0.0052(19) C14 0.022(3) 0.032(3) 0.016(2) 0.010(2) 0.009(2) 0.012(2) C15 0.022(3) 0.040(3) 0.016(2) 0.009(2) 0.009(2) 0.019(2) C16 0.025(3) 0.034(3) 0.018(3) 0.003(2) 0.009(2) 0.016(2) C17 0.020(3) 0.025(3) 0.016(2) 0.003(2) 0.005(2) 0.010(2) C18 0.019(3) 0.024(2) 0.011(2) 0.0054(19) 0.004(2) 0.013(2) C19 0.013(2) 0.019(2) 0.014(2) 0.0042(18) 0.003(2) 0.0068(19) C20 0.012(2) 0.017(2) 0.014(2) 0.0029(18) 0.0017(19) 0.0062(19) C21 0.012(2) 0.016(2) 0.016(2) 0.0045(18) 0.002(2) 0.0071(19) C22 0.020(3) 0.019(2) 0.023(3) 0.002(2) 0.009(2) 0.008(2) C23 0.024(3) 0.013(2) 0.033(3) 0.007(2) 0.014(2) 0.007(2) C24 0.023(3) 0.020(2) 0.028(3) 0.012(2) 0.014(2) 0.010(2) C25 0.019(3) 0.019(2) 0.019(2) 0.0078(19) 0.010(2) 0.010(2) C26 0.013(2) 0.014(2) 0.016(2) 0.0035(18) 0.0021(19) 0.0068(18) C27 0.016(3) 0.017(2) 0.017(2) 0.0042(19) 0.006(2) 0.003(2) C28 0.015(2) 0.014(2) 0.018(2) 0.0028(18) 0.006(2) 0.0047(19) C29 0.023(3) 0.029(3) 0.019(3) 0.008(2) 0.014(2) 0.012(2) C30 0.016(3) 0.035(3) 0.025(3) 0.009(2) 0.010(2) 0.013(2) C31 0.020(3) 0.024(2) 0.016(2) 0.007(2) 0.006(2) 0.010(2) C32 0.016(2) 0.012(2) 0.017(2) 0.0037(18) 0.008(2) 0.0058(19) C33 0.014(2) 0.013(2) 0.020(2) 0.0030(18) 0.006(2) 0.0047(19) C34 0.021(3) 0.009(2) 0.017(2) 0.0044(17) 0.009(2) 0.0081(19) C35 0.015(3) 0.021(2) 0.015(2) 0.0034(19) 0.005(2) 0.008(2) C36 0.014(2) 0.019(2) 0.012(2) 0.0013(18) 0.004(2) 0.0020(19) C37 0.023(3) 0.012(2) 0.016(2) 0.0019(18) 0.009(2) 0.004(2) C38 0.019(3) 0.015(2) 0.016(2) 0.0037(18) 0.006(2) 0.007(2) C39 0.017(2) 0.013(2) 0.014(2) 0.0044(18) 0.008(2) 0.0044(19) C40 0.014(2) 0.014(2) 0.012(2) 0.0021(17) 0.0062(19) 0.0044(19) C41 0.016(2) 0.014(2) 0.014(2) 0.0047(18) 0.009(2) 0.0070(19) C42 0.013(2) 0.014(2) 0.016(2) 0.0057(18) 0.008(2) 0.0061(19) C43 0.020(3) 0.015(2) 0.017(2) 0.0031(18) 0.008(2) 0.009(2) C44 0.023(3) 0.018(2) 0.029(3) 0.006(2) 0.011(2) 0.013(2) C45 0.019(3) 0.022(2) 0.027(3) 0.011(2) 0.009(2) 0.012(2) C46 0.013(2) 0.019(2) 0.018(2) 0.0050(19) 0.005(2) 0.0057(19) C47 0.017(2) 0.013(2) 0.018(2) 0.0068(18) 0.011(2) 0.0073(19) C48 0.014(2) 0.019(2) 0.016(2) 0.0031(18) 0.005(2) 0.0067(19) C49 0.020(3) 0.024(2) 0.014(2) 0.0056(19) 0.007(2) 0.014(2) C50 0.028(3) 0.019(2) 0.020(2) 0.005(2) 0.008(2) 0.015(2) C51 0.022(3) 0.014(2) 0.018(2) 0.0039(19) 0.007(2) 0.008(2) C52 0.018(3) 0.015(2) 0.014(2) 0.0027(18) 0.010(2) 0.0084(19) C53 0.014(2) 0.012(2) 0.015(2) 0.0025(17) 0.007(2) 0.0051(19) C54 0.017(2) 0.013(2) 0.015(2) 0.0035(18) 0.009(2) 0.0060(19) C55 0.013(2) 0.014(2) 0.015(2) 0.0008(18) 0.006(2) 0.0032(19) C56 0.020(3) 0.018(2) 0.019(2) 0.0058(19) 0.007(2) 0.006(2) C57 0.020(3) 0.016(2) 0.022(3) 0.001(2) 0.006(2) -0.001(2) C58 0.017(3) 0.022(2) 0.020(3) 0.000(2) 0.003(2) 0.001(2) C59 0.018(3) 0.021(2) 0.016(2) 0.0038(19) 0.003(2) 0.007(2) C60 0.018(2) 0.013(2) 0.013(2) 0.0005(17) 0.008(2) 0.0050(19) C61 0.039(3) 0.039(3) 0.017(3) 0.007(2) 0.011(2) 0.020(3) C62 0.022(3) 0.028(3) 0.024(3) 0.006(2) 0.012(2) 0.013(2) C63 0.034(4) 0.040(3) 0.058(4) 0.021(3) 0.029(3) 0.014(3) C64 0.019(3) 0.066(4) 0.039(4) 0.002(3) 0.007(3) 0.010(3) C65 0.032(3) 0.032(3) 0.026(3) 0.010(2) 0.021(3) 0.015(2) C66 0.028(3) 0.039(3) 0.032(3) 0.009(2) 0.013(3) 0.016(3) C67 0.044(4) 0.037(3) 0.039(3) -0.002(3) 0.008(3) 0.023(3) C68 0.048(4) 0.046(4) 0.037(3) 0.013(3) 0.013(3) 0.028(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O5 2.121(3) . ? Mn1 N2 2.206(4) . ? Mn1 O3 2.207(4) . ? Mn1 N6 2.217(4) . ? Mn1 N1 2.338(4) . ? Mn1 N5 2.385(4) . ? Mn2 O1 1.864(3) . ? Mn2 O2 1.904(3) . ? Mn2 N3 1.989(4) . ? Mn2 N7 1.993(4) . ? Mn2 O6 2.125(4) . ? Mn2 O4 2.449(4) . ? Mn3 O10 1.890(3) . ? Mn3 O9 1.895(3) . ? Mn3 N11 1.996(4) . ? Mn3 N15 2.031(4) . ? Mn3 O13 2.280(3) . ? Mn3 O11 2.303(3) . ? Mn4 O7 2.138(3) . ? Mn4 N10 2.195(4) . ? Mn4 N14 2.219(4) . ? Mn4 N9 2.245(4) . ? Mn4 N13 2.267(4) . ? Mn4 O12 2.295(3) . ? O1 C13 1.336(5) . ? O2 C26 1.341(5) . ? O3 H3A 0.8843 . ? O3 H3B 0.8590 . ? O4 H4A 0.8488 . ? O4 H4B 0.8555 . ? O5 C27 1.256(6) . ? O6 C27 1.254(6) . ? O7 C34 1.275(6) . ? O8 C34 1.251(6) . ? O9 C47 1.345(5) . ? O10 C60 1.353(5) . ? O11 H11A 0.8200 . ? O11 H11B 0.851(9) . ? O12 C61 1.421(6) . ? O12 H12A 0.851(9) . ? O13 C62 1.251(6) . ? O14 C65 1.236(7) . ? O15 H15A 0.8423 . ? O15 H15B 1.0846 . ? O16 H16A 0.8483 . ? O16 H16B 0.8430 . ? O17 H17A 0.8155 . ? O17 H17B 0.9330 . ? O18 C68 1.412(8) . ? O18 H18 0.8200 . ? O19 H19A 1.1042 . ? O19 H19B 1.1576 . ? O20 H20A 0.8586 . ? O20 H20B 0.8489 . ? N1 C1 1.333(6) . ? N1 C5 1.356(6) . ? N2 C6 1.330(6) . ? N2 N3 1.365(5) . ? N3 C7 1.342(6) . ? N4 C6 1.340(6) . ? N4 C7 1.357(6) . ? N5 C14 1.339(6) . ? N5 C18 1.358(6) . ? N6 C19 1.320(6) . ? N6 N7 1.367(5) . ? N7 C20 1.340(6) . ? N8 C19 1.347(6) . ? N8 C20 1.349(6) . ? N8 H8A 0.9023 . ? N9 C35 1.339(6) . ? N9 C39 1.347(6) . ? N10 C40 1.333(6) . ? N10 N11 1.365(5) . ? N11 C41 1.360(6) . ? N12 C41 1.332(6) . ? N12 C40 1.335(6) . ? N12 H12 0.8600 . ? N13 C48 1.339(6) . ? N13 C52 1.355(6) . ? N14 C53 1.328(6) . ? N14 N15 1.357(5) . ? N15 C54 1.352(6) . ? N16 C54 1.350(6) . ? N16 C53 1.353(6) . ? N17 C62 1.314(7) . ? N17 C63 1.452(7) . ? N17 C64 1.457(7) . ? N18 C65 1.323(7) . ? N18 C66 1.442(7) . ? N18 C67 1.456(7) . ? C1 C2 1.393(7) . ? C1 H1 0.9300 . ? C2 C3 1.369(8) . ? C2 H2 0.9300 . ? C3 C4 1.386(7) . ? C3 H3 0.9300 . ? C4 C5 1.385(7) . ? C4 H4 0.9300 . ? C5 C6 1.471(7) . ? C7 C8 1.458(7) . ? C8 C9 1.399(7) . ? C8 C13 1.419(6) . ? C9 C10 1.371(7) . ? C9 H9 0.9300 . ? C10 C11 1.393(7) . ? C10 H10 0.9300 . ? C11 C12 1.383(7) . ? C11 H11 0.9300 . ? C12 C13 1.402(7) . ? C12 H12B 0.9300 . ? C14 C15 1.381(7) . ? C14 H14 0.9300 . ? C15 C16 1.384(8) . ? C15 H15 0.9300 . ? C16 C17 1.383(7) . ? C16 H16 0.9300 . ? C17 C18 1.395(7) . ? C17 H17 0.9300 . ? C18 C19 1.466(6) . ? C20 C21 1.455(6) . ? C21 C22 1.402(6) . ? C21 C26 1.412(6) . ? C22 C23 1.383(7) . ? C22 H22 0.9300 . ? C23 C24 1.388(7) . ? C23 H23 0.9300 . ? C24 C25 1.383(7) . ? C24 H24 0.9300 . ? C25 C26 1.402(6) . ? C25 H25 0.9300 . ? C27 C28 1.508(6) . ? C28 C33 1.390(6) . ? C28 C29 1.393(7) . ? C29 C30 1.385(7) . ? C29 H29 0.9300 . ? C30 C31 1.385(7) . ? C30 H30 0.9300 . ? C31 C32 1.396(7) . ? C31 H31 0.9300 . ? C32 C33 1.386(6) . ? C32 C34 1.501(6) . ? C33 H33 0.9300 . ? C35 C36 1.385(6) . ? C35 H35 0.9300 . ? C36 C37 1.385(7) . ? C36 H36 0.9300 . ? C37 C38 1.385(7) . ? C37 H37 0.9300 . ? C38 C39 1.387(6) . ? C38 H38 0.9300 . ? C39 C40 1.462(7) . ? C41 C42 1.453(6) . ? C42 C43 1.400(6) . ? C42 C47 1.401(7) . ? C43 C44 1.380(7) . ? C43 H43 0.9300 . ? C44 C45 1.385(7) . ? C44 H44 0.9300 . ? C45 C46 1.383(7) . ? C45 H45 0.9300 . ? C46 C47 1.407(6) . ? C46 H46 0.9300 . ? C48 C49 1.388(6) . ? C48 H48 0.9300 . ? C49 C50 1.386(7) . ? C49 H49 0.9300 . ? C50 C51 1.380(7) . ? C50 H50 0.9300 . ? C51 C52 1.385(6) . ? C51 H51 0.9300 . ? C52 C53 1.469(6) . ? C54 C55 1.460(7) . ? C55 C56 1.406(6) . ? C55 C60 1.408(6) . ? C56 C57 1.379(7) . ? C56 H56 0.9300 . ? C57 C58 1.391(7) . ? C57 H57 0.9300 . ? C58 C59 1.382(7) . ? C58 H58 0.9300 . ? C59 C60 1.401(7) . ? C59 H59 0.9300 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 H62 0.9300 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 H65 0.9300 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Mn1 N2 97.11(14) . . ? O5 Mn1 O3 81.21(14) . . ? N2 Mn1 O3 139.70(14) . . ? O5 Mn1 N6 87.11(15) . . ? N2 Mn1 N6 79.21(14) . . ? O3 Mn1 N6 140.29(14) . . ? O5 Mn1 N1 132.96(15) . . ? N2 Mn1 N1 70.70(14) . . ? O3 Mn1 N1 81.17(14) . . ? N6 Mn1 N1 131.34(15) . . ? O5 Mn1 N5 119.68(15) . . ? N2 Mn1 N5 128.93(15) . . ? O3 Mn1 N5 83.71(14) . . ? N6 Mn1 N5 69.50(14) . . ? N1 Mn1 N5 101.19(13) . . ? O1 Mn2 O2 89.66(13) . . ? O1 Mn2 N3 87.36(14) . . ? O2 Mn2 N3 176.59(15) . . ? O1 Mn2 N7 168.33(16) . . ? O2 Mn2 N7 86.99(14) . . ? N3 Mn2 N7 95.61(15) . . ? O1 Mn2 O6 99.66(14) . . ? O2 Mn2 O6 93.13(13) . . ? N3 Mn2 O6 89.02(15) . . ? N7 Mn2 O6 91.69(15) . . ? O1 Mn2 O4 83.32(13) . . ? O2 Mn2 O4 89.96(13) . . ? N3 Mn2 O4 88.04(14) . . ? N7 Mn2 O4 85.50(14) . . ? O6 Mn2 O4 175.71(12) . . ? O10 Mn3 O9 86.84(13) . . ? O10 Mn3 N11 173.87(14) . . ? O9 Mn3 N11 87.47(14) . . ? O10 Mn3 N15 86.38(14) . . ? O9 Mn3 N15 172.14(15) . . ? N11 Mn3 N15 99.45(15) . . ? O10 Mn3 O13 89.38(13) . . ? O9 Mn3 O13 90.69(13) . . ? N11 Mn3 O13 92.97(14) . . ? N15 Mn3 O13 85.25(14) . . ? O10 Mn3 O11 92.18(13) . . ? O9 Mn3 O11 99.14(13) . . ? N11 Mn3 O11 86.48(14) . . ? N15 Mn3 O11 85.10(13) . . ? O13 Mn3 O11 170.11(12) . . ? O7 Mn4 N10 89.60(13) . . ? O7 Mn4 N14 92.04(13) . . ? N10 Mn4 N14 84.92(14) . . ? O7 Mn4 N9 96.63(13) . . ? N10 Mn4 N9 74.62(14) . . ? N14 Mn4 N9 157.66(14) . . ? O7 Mn4 N13 101.79(13) . . ? N10 Mn4 N13 155.67(14) . . ? N14 Mn4 N13 73.37(14) . . ? N9 Mn4 N13 124.34(14) . . ? O7 Mn4 O12 176.36(12) . . ? N10 Mn4 O12 87.13(13) . . ? N14 Mn4 O12 86.09(13) . . ? N9 Mn4 O12 84.04(13) . . ? N13 Mn4 O12 80.68(13) . . ? C13 O1 Mn2 128.4(3) . . ? C26 O2 Mn2 128.5(3) . . ? Mn1 O3 H3A 108.4 . . ? Mn1 O3 H3B 113.4 . . ? H3A O3 H3B 111.2 . . ? Mn2 O4 H4A 116.2 . . ? Mn2 O4 H4B 121.0 . . ? H4A O4 H4B 115.5 . . ? C27 O5 Mn1 136.4(3) . . ? C27 O6 Mn2 137.9(3) . . ? C34 O7 Mn4 108.8(3) . . ? C47 O9 Mn3 132.0(3) . . ? C60 O10 Mn3 128.8(3) . . ? Mn3 O11 H11A 109.5 . . ? Mn3 O11 H11B 120(3) . . ? H11A O11 H11B 120.3 . . ? C61 O12 Mn4 125.8(3) . . ? C61 O12 H12A 108(4) . . ? Mn4 O12 H12A 109(4) . . ? C62 O13 Mn3 115.0(3) . . ? H15A O15 H15B 102.4 . . ? H16A O16 H16B 117.0 . . ? H17A O17 H17B 111.6 . . ? C68 O18 H18 109.5 . . ? H19A O19 H19B 114.6 . . ? H20A O20 H20B 115.2 . . ? C1 N1 C5 117.5(4) . . ? C1 N1 Mn1 125.1(3) . . ? C5 N1 Mn1 117.3(3) . . ? C6 N2 N3 104.7(4) . . ? C6 N2 Mn1 120.7(3) . . ? N3 N2 Mn1 134.6(3) . . ? C7 N3 N2 107.3(3) . . ? C7 N3 Mn2 128.0(3) . . ? N2 N3 Mn2 124.7(3) . . ? C6 N4 C7 102.4(4) . . ? C14 N5 C18 117.3(4) . . ? C14 N5 Mn1 126.2(3) . . ? C18 N5 Mn1 116.5(3) . . ? C19 N6 N7 105.1(4) . . ? C19 N6 Mn1 121.1(3) . . ? N7 N6 Mn1 130.8(3) . . ? C20 N7 N6 107.3(4) . . ? C20 N7 Mn2 126.7(3) . . ? N6 N7 Mn2 125.7(3) . . ? C19 N8 C20 102.9(4) . . ? C19 N8 H8A 111.6 . . ? C20 N8 H8A 141.4 . . ? C35 N9 C39 118.1(4) . . ? C35 N9 Mn4 126.4(3) . . ? C39 N9 Mn4 115.5(3) . . ? C40 N10 N11 105.3(3) . . ? C40 N10 Mn4 115.1(3) . . ? N11 N10 Mn4 139.6(3) . . ? C41 N11 N10 105.8(3) . . ? C41 N11 Mn3 128.1(3) . . ? N10 N11 Mn3 125.5(3) . . ? C41 N12 C40 103.0(4) . . ? C41 N12 H12 128.5 . . ? C40 N12 H12 128.5 . . ? C48 N13 C52 118.3(4) . . ? C48 N13 Mn4 125.2(3) . . ? C52 N13 Mn4 116.2(3) . . ? C53 N14 N15 105.6(3) . . ? C53 N14 Mn4 116.5(3) . . ? N15 N14 Mn4 137.9(3) . . ? C54 N15 N14 106.7(4) . . ? C54 N15 Mn3 126.9(3) . . ? N14 N15 Mn3 126.2(3) . . ? C54 N16 C53 102.2(4) . . ? C62 N17 C63 120.8(5) . . ? C62 N17 C64 119.8(5) . . ? C63 N17 C64 118.9(5) . . ? C65 N18 C66 121.7(5) . . ? C65 N18 C67 120.7(5) . . ? C66 N18 C67 117.6(4) . . ? N1 C1 C2 122.8(5) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 119.2(5) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 119.0(5) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 118.8(5) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? N1 C5 C4 122.7(5) . . ? N1 C5 C6 113.6(4) . . ? C4 C5 C6 123.7(5) . . ? N2 C6 N4 114.3(4) . . ? N2 C6 C5 117.7(4) . . ? N4 C6 C5 128.0(4) . . ? N3 C7 N4 111.3(4) . . ? N3 C7 C8 122.6(4) . . ? N4 C7 C8 126.0(4) . . ? C9 C8 C13 118.8(4) . . ? C9 C8 C7 121.2(4) . . ? C13 C8 C7 120.0(4) . . ? C10 C9 C8 121.6(4) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C9 C10 C11 119.8(5) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C12 C11 C10 120.0(5) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 121.0(4) . . ? C11 C12 H12B 119.5 . . ? C13 C12 H12B 119.5 . . ? O1 C13 C12 117.6(4) . . ? O1 C13 C8 123.7(4) . . ? C12 C13 C8 118.7(4) . . ? N5 C14 C15 123.5(5) . . ? N5 C14 H14 118.2 . . ? C15 C14 H14 118.2 . . ? C14 C15 C16 118.7(5) . . ? C14 C15 H15 120.6 . . ? C16 C15 H15 120.6 . . ? C17 C16 C15 119.3(5) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 118.4(5) . . ? C16 C17 H17 120.8 . . ? C18 C17 H17 120.8 . . ? N5 C18 C17 122.7(4) . . ? N5 C18 C19 113.6(4) . . ? C17 C18 C19 123.7(4) . . ? N6 C19 N8 113.6(4) . . ? N6 C19 C18 117.5(4) . . ? N8 C19 C18 128.8(4) . . ? N7 C20 N8 111.1(4) . . ? N7 C20 C21 123.2(4) . . ? N8 C20 C21 125.5(4) . . ? C22 C21 C26 118.7(4) . . ? C22 C21 C20 120.5(4) . . ? C26 C21 C20 120.6(4) . . ? C23 C22 C21 121.8(4) . . ? C23 C22 H22 119.1 . . ? C21 C22 H22 119.1 . . ? C22 C23 C24 119.1(4) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? C25 C24 C23 120.3(4) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 121.2(4) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? O2 C26 C25 117.7(4) . . ? O2 C26 C21 123.6(4) . . ? C25 C26 C21 118.8(4) . . ? O6 C27 O5 126.4(4) . . ? O6 C27 C28 116.8(4) . . ? O5 C27 C28 116.7(4) . . ? C33 C28 C29 119.3(4) . . ? C33 C28 C27 118.9(4) . . ? C29 C28 C27 121.8(4) . . ? C30 C29 C28 119.8(4) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C31 C30 C29 120.6(5) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C30 C31 C32 120.1(4) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C33 C32 C31 118.9(4) . . ? C33 C32 C34 119.5(4) . . ? C31 C32 C34 121.5(4) . . ? C32 C33 C28 121.3(4) . . ? C32 C33 H33 119.4 . . ? C28 C33 H33 119.4 . . ? O8 C34 O7 122.9(4) . . ? O8 C34 C32 120.4(4) . . ? O7 C34 C32 116.6(4) . . ? N9 C35 C36 123.0(4) . . ? N9 C35 H35 118.5 . . ? C36 C35 H35 118.5 . . ? C35 C36 C37 118.6(4) . . ? C35 C36 H36 120.7 . . ? C37 C36 H36 120.7 . . ? C36 C37 C38 119.1(4) . . ? C36 C37 H37 120.5 . . ? C38 C37 H37 120.5 . . ? C37 C38 C39 118.8(4) . . ? C37 C38 H38 120.6 . . ? C39 C38 H38 120.6 . . ? N9 C39 C38 122.4(4) . . ? N9 C39 C40 115.0(4) . . ? C38 C39 C40 122.6(4) . . ? N10 C40 N12 113.8(4) . . ? N10 C40 C39 119.7(4) . . ? N12 C40 C39 126.5(4) . . ? N12 C41 N11 112.1(4) . . ? N12 C41 C42 124.0(4) . . ? N11 C41 C42 123.8(4) . . ? C43 C42 C47 119.9(4) . . ? C43 C42 C41 119.1(4) . . ? C47 C42 C41 120.7(4) . . ? C44 C43 C42 121.3(4) . . ? C44 C43 H43 119.4 . . ? C42 C43 H43 119.4 . . ? C43 C44 C45 118.9(4) . . ? C43 C44 H44 120.6 . . ? C45 C44 H44 120.6 . . ? C46 C45 C44 121.1(4) . . ? C46 C45 H45 119.5 . . ? C44 C45 H45 119.5 . . ? C45 C46 C47 120.6(4) . . ? C45 C46 H46 119.7 . . ? C47 C46 H46 119.7 . . ? O9 C47 C42 123.3(4) . . ? O9 C47 C46 118.4(4) . . ? C42 C47 C46 118.2(4) . . ? N13 C48 C49 122.9(4) . . ? N13 C48 H48 118.5 . . ? C49 C48 H48 118.5 . . ? C50 C49 C48 118.2(4) . . ? C50 C49 H49 120.9 . . ? C48 C49 H49 120.9 . . ? C51 C50 C49 119.5(4) . . ? C51 C50 H50 120.3 . . ? C49 C50 H50 120.3 . . ? C50 C51 C52 119.1(4) . . ? C50 C51 H51 120.4 . . ? C52 C51 H51 120.4 . . ? N13 C52 C51 121.9(4) . . ? N13 C52 C53 114.5(4) . . ? C51 C52 C53 123.7(4) . . ? N14 C53 N16 113.7(4) . . ? N14 C53 C52 119.1(4) . . ? N16 C53 C52 127.2(4) . . ? N16 C54 N15 111.8(4) . . ? N16 C54 C55 124.8(4) . . ? N15 C54 C55 123.4(4) . . ? C56 C55 C60 119.0(4) . . ? C56 C55 C54 120.5(4) . . ? C60 C55 C54 120.6(4) . . ? C57 C56 C55 121.5(4) . . ? C57 C56 H56 119.3 . . ? C55 C56 H56 119.3 . . ? C56 C57 C58 119.1(4) . . ? C56 C57 H57 120.5 . . ? C58 C57 H57 120.5 . . ? C59 C58 C57 120.8(5) . . ? C59 C58 H58 119.6 . . ? C57 C58 H58 119.6 . . ? C58 C59 C60 120.6(5) . . ? C58 C59 H59 119.7 . . ? C60 C59 H59 119.7 . . ? O10 C60 C59 118.7(4) . . ? O10 C60 C55 122.2(4) . . ? C59 C60 C55 119.0(4) . . ? O12 C61 H61A 109.5 . . ? O12 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? O12 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? O13 C62 N17 125.1(5) . . ? O13 C62 H62 117.5 . . ? N17 C62 H62 117.5 . . ? N17 C63 H63A 109.5 . . ? N17 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? N17 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? N17 C64 H64A 109.5 . . ? N17 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? N17 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? O14 C65 N18 124.7(5) . . ? O14 C65 H65 117.6 . . ? N18 C65 H65 117.6 . . ? N18 C66 H66A 109.5 . . ? N18 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? N18 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N18 C67 H67A 109.5 . . ? N18 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? N18 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? O18 C68 H68A 109.5 . . ? O18 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? O18 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 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 Mn2 O1 C13 142.9(4) . . . . ? N3 Mn2 O1 C13 -35.5(4) . . . . ? N7 Mn2 O1 C13 69.6(8) . . . . ? O6 Mn2 O1 C13 -124.0(4) . . . . ? O4 Mn2 O1 C13 52.9(4) . . . . ? O1 Mn2 O2 C26 -135.0(4) . . . . ? N3 Mn2 O2 C26 -106(2) . . . . ? N7 Mn2 O2 C26 33.8(4) . . . . ? O6 Mn2 O2 C26 125.4(4) . . . . ? O4 Mn2 O2 C26 -51.7(4) . . . . ? N2 Mn1 O5 C27 -27.0(5) . . . . ? O3 Mn1 O5 C27 -166.4(5) . . . . ? N6 Mn1 O5 C27 51.7(5) . . . . ? N1 Mn1 O5 C27 -97.2(5) . . . . ? N5 Mn1 O5 C27 116.1(5) . . . . ? O1 Mn2 O6 C27 173.5(4) . . . . ? O2 Mn2 O6 C27 -96.4(4) . . . . ? N3 Mn2 O6 C27 86.3(4) . . . . ? N7 Mn2 O6 C27 -9.3(4) . . . . ? O4 Mn2 O6 C27 39.7(18) . . . . ? N10 Mn4 O7 C34 -141.1(3) . . . . ? N14 Mn4 O7 C34 134.0(3) . . . . ? N9 Mn4 O7 C34 -66.6(3) . . . . ? N13 Mn4 O7 C34 60.6(3) . . . . ? O12 Mn4 O7 C34 -166.9(18) . . . . ? O10 Mn3 O9 C47 -158.7(4) . . . . ? N11 Mn3 O9 C47 23.5(4) . . . . ? N15 Mn3 O9 C47 -128.2(10) . . . . ? O13 Mn3 O9 C47 -69.4(4) . . . . ? O11 Mn3 O9 C47 109.6(4) . . . . ? O9 Mn3 O10 C60 138.1(4) . . . . ? N11 Mn3 O10 C60 160.0(12) . . . . ? N15 Mn3 O10 C60 -37.9(4) . . . . ? O13 Mn3 O10 C60 47.4(4) . . . . ? O11 Mn3 O10 C60 -122.8(4) . . . . ? O7 Mn4 O12 C61 170.1(18) . . . . ? N10 Mn4 O12 C61 144.3(4) . . . . ? N14 Mn4 O12 C61 -130.6(4) . . . . ? N9 Mn4 O12 C61 69.4(4) . . . . ? N13 Mn4 O12 C61 -56.9(4) . . . . ? O10 Mn3 O13 C62 45.9(3) . . . . ? O9 Mn3 O13 C62 -40.9(3) . . . . ? N11 Mn3 O13 C62 -128.4(3) . . . . ? N15 Mn3 O13 C62 132.3(3) . . . . ? O11 Mn3 O13 C62 145.1(7) . . . . ? O5 Mn1 N1 C1 -97.2(4) . . . . ? N2 Mn1 N1 C1 -178.7(4) . . . . ? O3 Mn1 N1 C1 -28.0(4) . . . . ? N6 Mn1 N1 C1 126.2(4) . . . . ? N5 Mn1 N1 C1 53.7(4) . . . . ? O5 Mn1 N1 C5 80.4(4) . . . . ? N2 Mn1 N1 C5 -1.1(3) . . . . ? O3 Mn1 N1 C5 149.6(3) . . . . ? N6 Mn1 N1 C5 -56.2(4) . . . . ? N5 Mn1 N1 C5 -128.7(3) . . . . ? O5 Mn1 N2 C6 -131.0(3) . . . . ? O3 Mn1 N2 C6 -46.2(4) . . . . ? N6 Mn1 N2 C6 143.4(4) . . . . ? N1 Mn1 N2 C6 2.2(3) . . . . ? N5 Mn1 N2 C6 91.1(4) . . . . ? O5 Mn1 N2 N3 44.5(4) . . . . ? O3 Mn1 N2 N3 129.3(4) . . . . ? N6 Mn1 N2 N3 -41.1(4) . . . . ? N1 Mn1 N2 N3 177.7(4) . . . . ? N5 Mn1 N2 N3 -93.4(4) . . . . ? C6 N2 N3 C7 1.4(5) . . . . ? Mn1 N2 N3 C7 -174.6(3) . . . . ? C6 N2 N3 Mn2 -179.7(3) . . . . ? Mn1 N2 N3 Mn2 4.3(6) . . . . ? O1 Mn2 N3 C7 21.7(4) . . . . ? O2 Mn2 N3 C7 -8(3) . . . . ? N7 Mn2 N3 C7 -147.0(4) . . . . ? O6 Mn2 N3 C7 121.4(4) . . . . ? O4 Mn2 N3 C7 -61.7(4) . . . . ? O1 Mn2 N3 N2 -157.1(3) . . . . ? O2 Mn2 N3 N2 174(2) . . . . ? N7 Mn2 N3 N2 34.3(4) . . . . ? O6 Mn2 N3 N2 -57.3(3) . . . . ? O4 Mn2 N3 N2 119.5(3) . . . . ? O5 Mn1 N5 C14 110.7(4) . . . . ? N2 Mn1 N5 C14 -119.2(4) . . . . ? O3 Mn1 N5 C14 34.6(4) . . . . ? N6 Mn1 N5 C14 -175.3(4) . . . . ? N1 Mn1 N5 C14 -45.1(4) . . . . ? O5 Mn1 N5 C18 -67.6(4) . . . . ? N2 Mn1 N5 C18 62.4(4) . . . . ? O3 Mn1 N5 C18 -143.8(3) . . . . ? N6 Mn1 N5 C18 6.4(3) . . . . ? N1 Mn1 N5 C18 136.6(3) . . . . ? O5 Mn1 N6 C19 111.4(4) . . . . ? N2 Mn1 N6 C19 -150.8(4) . . . . ? O3 Mn1 N6 C19 38.9(4) . . . . ? N1 Mn1 N6 C19 -98.8(4) . . . . ? N5 Mn1 N6 C19 -11.8(3) . . . . ? O5 Mn1 N6 N7 -46.0(4) . . . . ? N2 Mn1 N6 N7 51.8(4) . . . . ? O3 Mn1 N6 N7 -118.5(4) . . . . ? N1 Mn1 N6 N7 103.8(4) . . . . ? N5 Mn1 N6 N7 -169.2(4) . . . . ? C19 N6 N7 C20 -0.3(5) . . . . ? Mn1 N6 N7 C20 159.8(3) . . . . ? C19 N6 N7 Mn2 174.6(3) . . . . ? Mn1 N6 N7 Mn2 -25.3(5) . . . . ? O1 Mn2 N7 C20 45.6(9) . . . . ? O2 Mn2 N7 C20 -27.9(4) . . . . ? N3 Mn2 N7 C20 149.9(4) . . . . ? O6 Mn2 N7 C20 -121.0(4) . . . . ? O4 Mn2 N7 C20 62.3(4) . . . . ? O1 Mn2 N7 N6 -128.3(7) . . . . ? O2 Mn2 N7 N6 158.2(4) . . . . ? N3 Mn2 N7 N6 -24.1(4) . . . . ? O6 Mn2 N7 N6 65.1(4) . . . . ? O4 Mn2 N7 N6 -111.6(4) . . . . ? O7 Mn4 N9 C35 90.4(4) . . . . ? N10 Mn4 N9 C35 178.2(4) . . . . ? N14 Mn4 N9 C35 -157.4(4) . . . . ? N13 Mn4 N9 C35 -18.7(4) . . . . ? O12 Mn4 N9 C35 -93.1(4) . . . . ? O7 Mn4 N9 C39 -91.6(3) . . . . ? N10 Mn4 N9 C39 -3.9(3) . . . . ? N14 Mn4 N9 C39 20.5(5) . . . . ? N13 Mn4 N9 C39 159.2(3) . . . . ? O12 Mn4 N9 C39 84.8(3) . . . . ? O7 Mn4 N10 C40 100.0(3) . . . . ? N14 Mn4 N10 C40 -167.9(3) . . . . ? N9 Mn4 N10 C40 3.0(3) . . . . ? N13 Mn4 N10 C40 -141.3(3) . . . . ? O12 Mn4 N10 C40 -81.6(3) . . . . ? O7 Mn4 N10 N11 -80.6(4) . . . . ? N14 Mn4 N10 N11 11.5(4) . . . . ? N9 Mn4 N10 N11 -177.6(4) . . . . ? N13 Mn4 N10 N11 38.1(6) . . . . ? O12 Mn4 N10 N11 97.8(4) . . . . ? C40 N10 N11 C41 -0.6(4) . . . . ? Mn4 N10 N11 C41 180.0(3) . . . . ? C40 N10 N11 Mn3 -172.3(3) . . . . ? Mn4 N10 N11 Mn3 8.2(6) . . . . ? O10 Mn3 N11 C41 -32.6(15) . . . . ? O9 Mn3 N11 C41 -10.7(4) . . . . ? N15 Mn3 N11 C41 165.5(3) . . . . ? O13 Mn3 N11 C41 79.8(4) . . . . ? O11 Mn3 N11 C41 -110.1(4) . . . . ? O10 Mn3 N11 N10 137.3(12) . . . . ? O9 Mn3 N11 N10 159.1(3) . . . . ? N15 Mn3 N11 N10 -24.6(3) . . . . ? O13 Mn3 N11 N10 -110.3(3) . . . . ? O11 Mn3 N11 N10 59.8(3) . . . . ? O7 Mn4 N13 C48 -93.4(4) . . . . ? N10 Mn4 N13 C48 150.3(4) . . . . ? N14 Mn4 N13 C48 178.0(4) . . . . ? N9 Mn4 N13 C48 13.2(4) . . . . ? O12 Mn4 N13 C48 89.3(4) . . . . ? O7 Mn4 N13 C52 93.3(3) . . . . ? N10 Mn4 N13 C52 -23.1(5) . . . . ? N14 Mn4 N13 C52 4.7(3) . . . . ? N9 Mn4 N13 C52 -160.1(3) . . . . ? O12 Mn4 N13 C52 -84.0(3) . . . . ? O7 Mn4 N14 C53 -103.0(3) . . . . ? N10 Mn4 N14 C53 167.6(3) . . . . ? N9 Mn4 N14 C53 144.0(4) . . . . ? N13 Mn4 N14 C53 -1.3(3) . . . . ? O12 Mn4 N14 C53 80.1(3) . . . . ? O7 Mn4 N14 N15 75.0(4) . . . . ? N10 Mn4 N14 N15 -14.4(4) . . . . ? N9 Mn4 N14 N15 -38.0(6) . . . . ? N13 Mn4 N14 N15 176.7(4) . . . . ? O12 Mn4 N14 N15 -101.9(4) . . . . ? C53 N14 N15 C54 1.1(4) . . . . ? Mn4 N14 N15 C54 -177.1(3) . . . . ? C53 N14 N15 Mn3 175.7(3) . . . . ? Mn4 N14 N15 Mn3 -2.5(6) . . . . ? O10 Mn3 N15 C54 17.6(4) . . . . ? O9 Mn3 N15 C54 -13.0(12) . . . . ? N11 Mn3 N15 C54 -164.3(4) . . . . ? O13 Mn3 N15 C54 -72.1(4) . . . . ? O11 Mn3 N15 C54 110.1(4) . . . . ? O10 Mn3 N15 N14 -155.9(3) . . . . ? O9 Mn3 N15 N14 173.5(9) . . . . ? N11 Mn3 N15 N14 22.2(3) . . . . ? O13 Mn3 N15 N14 114.4(3) . . . . ? O11 Mn3 N15 N14 -63.4(3) . . . . ? C5 N1 C1 C2 2.7(7) . . . . ? Mn1 N1 C1 C2 -179.7(4) . . . . ? N1 C1 C2 C3 -1.8(8) . . . . ? C1 C2 C3 C4 0.3(7) . . . . ? C2 C3 C4 C5 0.1(7) . . . . ? C1 N1 C5 C4 -2.2(7) . . . . ? Mn1 N1 C5 C4 180.0(4) . . . . ? C1 N1 C5 C6 177.9(4) . . . . ? Mn1 N1 C5 C6 0.1(5) . . . . ? C3 C4 C5 N1 0.9(7) . . . . ? C3 C4 C5 C6 -179.3(4) . . . . ? N3 N2 C6 N4 -0.7(5) . . . . ? Mn1 N2 C6 N4 176.0(3) . . . . ? N3 N2 C6 C5 -179.7(4) . . . . ? Mn1 N2 C6 C5 -3.0(5) . . . . ? C7 N4 C6 N2 -0.2(5) . . . . ? C7 N4 C6 C5 178.6(4) . . . . ? N1 C5 C6 N2 1.8(6) . . . . ? C4 C5 C6 N2 -178.1(4) . . . . ? N1 C5 C6 N4 -177.0(4) . . . . ? C4 C5 C6 N4 3.1(8) . . . . ? N2 N3 C7 N4 -1.6(5) . . . . ? Mn2 N3 C7 N4 179.5(3) . . . . ? N2 N3 C7 C8 174.9(4) . . . . ? Mn2 N3 C7 C8 -4.0(6) . . . . ? C6 N4 C7 N3 1.1(5) . . . . ? C6 N4 C7 C8 -175.3(4) . . . . ? N3 C7 C8 C9 171.3(4) . . . . ? N4 C7 C8 C9 -12.6(7) . . . . ? N3 C7 C8 C13 -11.4(7) . . . . ? N4 C7 C8 C13 164.6(4) . . . . ? C13 C8 C9 C10 1.6(7) . . . . ? C7 C8 C9 C10 178.9(5) . . . . ? C8 C9 C10 C11 -0.1(8) . . . . ? C9 C10 C11 C12 -0.6(8) . . . . ? C10 C11 C12 C13 -0.2(7) . . . . ? Mn2 O1 C13 C12 -149.9(3) . . . . ? Mn2 O1 C13 C8 31.9(6) . . . . ? C11 C12 C13 O1 -176.6(4) . . . . ? C11 C12 C13 C8 1.6(7) . . . . ? C9 C8 C13 O1 175.8(4) . . . . ? C7 C8 C13 O1 -1.5(7) . . . . ? C9 C8 C13 C12 -2.3(7) . . . . ? C7 C8 C13 C12 -179.6(4) . . . . ? C18 N5 C14 C15 -0.9(7) . . . . ? Mn1 N5 C14 C15 -179.2(3) . . . . ? N5 C14 C15 C16 1.2(7) . . . . ? C14 C15 C16 C17 -0.6(7) . . . . ? C15 C16 C17 C18 -0.4(7) . . . . ? C14 N5 C18 C17 -0.1(7) . . . . ? Mn1 N5 C18 C17 178.3(3) . . . . ? C14 N5 C18 C19 -179.7(4) . . . . ? Mn1 N5 C18 C19 -1.3(5) . . . . ? C16 C17 C18 N5 0.7(7) . . . . ? C16 C17 C18 C19 -179.7(4) . . . . ? N7 N6 C19 N8 -0.1(5) . . . . ? Mn1 N6 C19 N8 -162.6(3) . . . . ? N7 N6 C19 C18 178.3(4) . . . . ? Mn1 N6 C19 C18 15.9(6) . . . . ? C20 N8 C19 N6 0.4(5) . . . . ? C20 N8 C19 C18 -177.8(5) . . . . ? N5 C18 C19 N6 -8.8(6) . . . . ? C17 C18 C19 N6 171.6(4) . . . . ? N5 C18 C19 N8 169.3(4) . . . . ? C17 C18 C19 N8 -10.3(8) . . . . ? N6 N7 C20 N8 0.6(5) . . . . ? Mn2 N7 C20 N8 -174.3(3) . . . . ? N6 N7 C20 C21 -173.9(4) . . . . ? Mn2 N7 C20 C21 11.3(6) . . . . ? C19 N8 C20 N7 -0.6(5) . . . . ? C19 N8 C20 C21 173.7(4) . . . . ? N7 C20 C21 C22 -172.4(4) . . . . ? N8 C20 C21 C22 14.0(7) . . . . ? N7 C20 C21 C26 12.5(7) . . . . ? N8 C20 C21 C26 -161.1(4) . . . . ? C26 C21 C22 C23 2.2(7) . . . . ? C20 C21 C22 C23 -173.0(4) . . . . ? C21 C22 C23 C24 0.8(8) . . . . ? C22 C23 C24 C25 -2.0(8) . . . . ? C23 C24 C25 C26 0.3(7) . . . . ? Mn2 O2 C26 C25 158.3(3) . . . . ? Mn2 O2 C26 C21 -22.6(6) . . . . ? C24 C25 C26 O2 -178.2(4) . . . . ? C24 C25 C26 C21 2.6(7) . . . . ? C22 C21 C26 O2 177.1(4) . . . . ? C20 C21 C26 O2 -7.7(7) . . . . ? C22 C21 C26 C25 -3.8(6) . . . . ? C20 C21 C26 C25 171.4(4) . . . . ? Mn2 O6 C27 O5 -48.5(7) . . . . ? Mn2 O6 C27 C28 132.4(4) . . . . ? Mn1 O5 C27 O6 10.5(8) . . . . ? Mn1 O5 C27 C28 -170.3(3) . . . . ? O6 C27 C28 C33 -2.7(6) . . . . ? O5 C27 C28 C33 178.1(4) . . . . ? O6 C27 C28 C29 177.6(4) . . . . ? O5 C27 C28 C29 -1.6(7) . . . . ? C33 C28 C29 C30 0.4(7) . . . . ? C27 C28 C29 C30 -179.9(4) . . . . ? C28 C29 C30 C31 -0.4(8) . . . . ? C29 C30 C31 C32 -0.2(8) . . . . ? C30 C31 C32 C33 1.0(7) . . . . ? C30 C31 C32 C34 -176.7(4) . . . . ? C31 C32 C33 C28 -1.1(7) . . . . ? C34 C32 C33 C28 176.7(4) . . . . ? C29 C28 C33 C32 0.4(7) . . . . ? C27 C28 C33 C32 -179.3(4) . . . . ? Mn4 O7 C34 O8 -1.1(5) . . . . ? Mn4 O7 C34 C32 -178.6(3) . . . . ? C33 C32 C34 O8 177.1(4) . . . . ? C31 C32 C34 O8 -5.2(6) . . . . ? C33 C32 C34 O7 -5.3(6) . . . . ? C31 C32 C34 O7 172.4(4) . . . . ? C39 N9 C35 C36 -1.1(6) . . . . ? Mn4 N9 C35 C36 176.7(3) . . . . ? N9 C35 C36 C37 0.7(7) . . . . ? C35 C36 C37 C38 0.6(6) . . . . ? C36 C37 C38 C39 -1.3(6) . . . . ? C35 N9 C39 C38 0.3(6) . . . . ? Mn4 N9 C39 C38 -177.8(3) . . . . ? C35 N9 C39 C40 -177.8(4) . . . . ? Mn4 N9 C39 C40 4.1(5) . . . . ? C37 C38 C39 N9 1.0(7) . . . . ? C37 C38 C39 C40 178.9(4) . . . . ? N11 N10 C40 N12 -0.1(5) . . . . ? Mn4 N10 C40 N12 179.5(3) . . . . ? N11 N10 C40 C39 178.4(4) . . . . ? Mn4 N10 C40 C39 -2.0(5) . . . . ? C41 N12 C40 N10 0.7(5) . . . . ? C41 N12 C40 C39 -177.6(4) . . . . ? N9 C39 C40 N10 -1.4(6) . . . . ? C38 C39 C40 N10 -179.5(4) . . . . ? N9 C39 C40 N12 176.8(4) . . . . ? C38 C39 C40 N12 -1.3(7) . . . . ? C40 N12 C41 N11 -1.1(5) . . . . ? C40 N12 C41 C42 175.6(4) . . . . ? N10 N11 C41 N12 1.1(5) . . . . ? Mn3 N11 C41 N12 172.5(3) . . . . ? N10 N11 C41 C42 -175.6(4) . . . . ? Mn3 N11 C41 C42 -4.2(6) . . . . ? N12 C41 C42 C43 11.6(6) . . . . ? N11 C41 C42 C43 -172.0(4) . . . . ? N12 C41 C42 C47 -161.9(4) . . . . ? N11 C41 C42 C47 14.4(6) . . . . ? C47 C42 C43 C44 -0.2(7) . . . . ? C41 C42 C43 C44 -173.8(4) . . . . ? C42 C43 C44 C45 -0.1(7) . . . . ? C43 C44 C45 C46 -0.2(7) . . . . ? C44 C45 C46 C47 0.9(7) . . . . ? Mn3 O9 C47 C42 -20.6(6) . . . . ? Mn3 O9 C47 C46 162.1(3) . . . . ? C43 C42 C47 O9 -176.4(4) . . . . ? C41 C42 C47 O9 -2.9(6) . . . . ? C43 C42 C47 C46 0.9(6) . . . . ? C41 C42 C47 C46 174.4(4) . . . . ? C45 C46 C47 O9 176.2(4) . . . . ? C45 C46 C47 C42 -1.2(6) . . . . ? C52 N13 C48 C49 0.5(6) . . . . ? Mn4 N13 C48 C49 -172.7(3) . . . . ? N13 C48 C49 C50 0.2(7) . . . . ? C48 C49 C50 C51 -0.6(7) . . . . ? C49 C50 C51 C52 0.2(7) . . . . ? C48 N13 C52 C51 -0.8(6) . . . . ? Mn4 N13 C52 C51 173.0(3) . . . . ? C48 N13 C52 C53 179.1(4) . . . . ? Mn4 N13 C52 C53 -7.0(5) . . . . ? C50 C51 C52 N13 0.5(7) . . . . ? C50 C51 C52 C53 -179.5(4) . . . . ? N15 N14 C53 N16 -0.8(5) . . . . ? Mn4 N14 C53 N16 177.8(3) . . . . ? N15 N14 C53 C52 179.5(4) . . . . ? Mn4 N14 C53 C52 -1.9(5) . . . . ? C54 N16 C53 N14 0.2(5) . . . . ? C54 N16 C53 C52 179.9(4) . . . . ? N13 C52 C53 N14 6.1(6) . . . . ? C51 C52 C53 N14 -174.0(4) . . . . ? N13 C52 C53 N16 -173.6(4) . . . . ? C51 C52 C53 N16 6.4(7) . . . . ? C53 N16 C54 N15 0.5(5) . . . . ? C53 N16 C54 C55 -178.7(4) . . . . ? N14 N15 C54 N16 -1.0(5) . . . . ? Mn3 N15 C54 N16 -175.6(3) . . . . ? N14 N15 C54 C55 178.2(4) . . . . ? Mn3 N15 C54 C55 3.7(6) . . . . ? N16 C54 C55 C56 -15.7(7) . . . . ? N15 C54 C55 C56 165.2(4) . . . . ? N16 C54 C55 C60 162.3(4) . . . . ? N15 C54 C55 C60 -16.8(6) . . . . ? C60 C55 C56 C57 -0.7(7) . . . . ? C54 C55 C56 C57 177.3(4) . . . . ? C55 C56 C57 C58 0.9(7) . . . . ? C56 C57 C58 C59 -0.1(8) . . . . ? C57 C58 C59 C60 -0.9(8) . . . . ? Mn3 O10 C60 C59 -147.1(3) . . . . ? Mn3 O10 C60 C55 36.4(6) . . . . ? C58 C59 C60 O10 -175.5(4) . . . . ? C58 C59 C60 C55 1.2(7) . . . . ? C56 C55 C60 O10 176.1(4) . . . . ? C54 C55 C60 O10 -1.9(6) . . . . ? C56 C55 C60 C59 -0.4(6) . . . . ? C54 C55 C60 C59 -178.4(4) . . . . ? Mn3 O13 C62 N17 -135.5(4) . . . . ? C63 N17 C62 O13 3.6(8) . . . . ? C64 N17 C62 O13 175.3(5) . . . . ? C66 N18 C65 O14 178.0(5) . . . . ? C67 N18 C65 O14 -2.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.055 _refine_diff_density_min -0.757 _refine_diff_density_rms 0.101