# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 906631' #TrackingRef 'web_deposit_cif_file_0_XinChen_1358526493.1(296K).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H54 Mn3 N8 O14' _chemical_formula_weight 1492.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4021(15) _cell_length_b 11.888(3) _cell_length_c 13.5025(16) _cell_angle_alpha 103.486(3) _cell_angle_beta 112.845(2) _cell_angle_gamma 93.903(3) _cell_volume 1614.3(5) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 697 _cell_measurement_theta_min 3.097 _cell_measurement_theta_max 19.323 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 765 _exptl_absorpt_coefficient_mu 0.657 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8273 _exptl_absorpt_correction_T_max 0.8854 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruck 1000 CCD area detector' _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 8212 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.1182 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 25.10 _reflns_number_total 5699 _reflns_number_gt 3321 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _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^)+(0.1064P)^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 5699 _refine_ls_number_parameters 466 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1205 _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_ref 0.2131 _refine_ls_wR_factor_gt 0.1514 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.1427(6) 0.9434(5) 0.0474(5) 0.0307(14) Uani 1 1 d . . . C2 C -0.2498(6) 0.8520(5) 0.0358(5) 0.0286(14) Uani 1 1 d . . . C3 C -0.3770(6) 0.8667(6) -0.0123(5) 0.0374(16) Uani 1 1 d . . . H3 H -0.3944 0.9351 -0.0330 0.045 Uiso 1 1 calc R . . C4 C -0.4776(7) 0.7845(6) -0.0302(6) 0.0426(17) Uani 1 1 d . . . H4 H -0.5625 0.7949 -0.0652 0.051 Uiso 1 1 calc R . . C5 C -0.4507(6) 0.6846(5) 0.0050(5) 0.0375(16) Uani 1 1 d . . . H5 H -0.5177 0.6276 -0.0055 0.045 Uiso 1 1 calc R . . C6 C -0.3249(6) 0.6707(5) 0.0553(5) 0.0302(14) Uani 1 1 d . . . C7 C -0.2211(6) 0.7515(5) 0.0697(5) 0.0282(14) Uani 1 1 d . . . C8 C -0.0884(6) 0.7213(5) 0.1146(5) 0.0304(14) Uani 1 1 d . . . C9 C -0.2509(6) 0.5566(5) 0.1880(5) 0.0332(15) Uani 1 1 d . . . C10 C -0.2669(7) 0.6363(6) 0.2720(6) 0.0465(18) Uani 1 1 d . . . H10 H -0.3092 0.6988 0.2578 0.056 Uiso 1 1 calc R . . C11 C -0.2176(8) 0.6206(7) 0.3795(6) 0.052(2) Uani 1 1 d . . . H11 H -0.2251 0.6745 0.4379 0.063 Uiso 1 1 calc R . . C12 C -0.1583(8) 0.5263(7) 0.3994(6) 0.058(2) Uani 1 1 d . . . H12 H -0.1270 0.5165 0.4710 0.070 Uiso 1 1 calc R . . C13 C -0.1448(7) 0.4460(6) 0.3141(6) 0.0447(18) Uani 1 1 d . . . H13 H -0.1053 0.3821 0.3282 0.054 Uiso 1 1 calc R . . C14 C -0.1902(6) 0.4605(5) 0.2069(5) 0.0291(14) Uani 1 1 d . . . C15 C -0.1593(6) 0.3796(6) 0.1201(5) 0.0303(14) Uani 1 1 d . . . C16 C -0.2935(7) 0.4658(6) -0.1701(5) 0.0391(16) Uani 1 1 d . . . H16 H -0.3045 0.4613 -0.1062 0.047 Uiso 1 1 calc R . . C17 C -0.4008(7) 0.4709(6) -0.2628(5) 0.0438(18) Uani 1 1 d . . . H17 H -0.4812 0.4691 -0.2602 0.053 Uiso 1 1 calc R . . C18 C -0.3886(6) 0.4786(6) -0.3592(5) 0.0347(15) Uani 1 1 d . . . C19 C -0.4995(7) 0.4900(6) -0.4539(5) 0.0432(17) Uani 1 1 d . . . H19 H -0.5787 0.4823 -0.4490 0.052 Uiso 1 1 calc R . . C20 C -0.2654(7) 0.4784(6) -0.3556(5) 0.0417(17) Uani 1 1 d . . . H20 H -0.2513 0.4827 -0.4181 0.050 Uiso 1 1 calc R . . C21 C -0.1647(6) 0.4719(6) -0.2618(5) 0.0366(16) Uani 1 1 d . . . H21 H -0.0838 0.4707 -0.2631 0.044 Uiso 1 1 calc R . . C22 C 0.3650(7) 0.8519(7) 0.1536(6) 0.0480(19) Uani 1 1 d . . . H22 H 0.3720 0.8544 0.0878 0.058 Uiso 1 1 calc R . . C23 C 0.4758(7) 0.8591(7) 0.2457(6) 0.0494(19) Uani 1 1 d . . . H23 H 0.5550 0.8642 0.2408 0.059 Uiso 1 1 calc R . . C24 C 0.4705(6) 0.8586(6) 0.3470(5) 0.0384(16) Uani 1 1 d . . . C25 C 0.3491(7) 0.8531(6) 0.3474(6) 0.0465(18) Uani 1 1 d . . . H25 H 0.3404 0.8543 0.4132 0.056 Uiso 1 1 calc R . . C26 C 0.2419(7) 0.8459(6) 0.2522(6) 0.0471(18) Uani 1 1 d . . . H26 H 0.1621 0.8440 0.2561 0.057 Uiso 1 1 calc R . . C27 C 0.5883(7) 0.8588(6) 0.4447(5) 0.0408(17) Uani 1 1 d . . . H27 H 0.6676 0.8791 0.4430 0.049 Uiso 1 1 calc R . . C28 C 0.5890(7) 0.8318(6) 0.5357(6) 0.0455(18) Uani 1 1 d . . . H28 H 0.5087 0.8177 0.5375 0.055 Uiso 1 1 calc R . . C29 C 0.6990(7) 0.8217(6) 0.6322(5) 0.0410(17) Uani 1 1 d . . . C30 C 0.8289(7) 0.8486(6) 0.6515(5) 0.0445(18) Uani 1 1 d . . . H30 H 0.8499 0.8773 0.6009 0.053 Uiso 1 1 calc R . . C31 C 0.9241(7) 0.8333(6) 0.7430(5) 0.0390(16) Uani 1 1 d . . . H31 H 1.0094 0.8522 0.7534 0.047 Uiso 1 1 calc R . . C32 C 0.7769(7) 0.7650(6) 0.8013(5) 0.0392(16) Uani 1 1 d . . . H32 H 0.7587 0.7346 0.8523 0.047 Uiso 1 1 calc R . . C33 C 0.6762(7) 0.7796(6) 0.7128(5) 0.0429(17) Uani 1 1 d . . . H33 H 0.5920 0.7616 0.7056 0.051 Uiso 1 1 calc R . . C34 C 0.7287(11) 0.2309(8) 0.4161(10) 0.083(3) Uani 1 1 d . . . H34 H 0.7004 0.2947 0.4489 0.100 Uiso 1 1 calc R . . C35 C 0.8336(10) 0.1885(9) 0.4862(8) 0.078(3) Uani 1 1 d . . . H35 H 0.8756 0.2240 0.5629 0.093 Uiso 1 1 calc R . . C36 C 0.8701(9) 0.0913(9) 0.4342(8) 0.067(3) Uani 1 1 d . . . C37 C 0.8078(11) 0.0441(9) 0.3193(8) 0.082(3) Uani 1 1 d . . . H37 H 0.8317 -0.0214 0.2840 0.098 Uiso 1 1 calc R . . C38 C 0.7106(12) 0.0943(9) 0.2577(9) 0.093(3) Uani 1 1 d . . . H38 H 0.6727 0.0647 0.1801 0.111 Uiso 1 1 calc R . . C39 C 0.9829(12) 0.0467(9) 0.5172(10) 0.097(4) Uani 1 1 d . . . H39 H 1.0246 0.0898 0.5922 0.116 Uiso 1 1 calc R . . Mn1 Mn 0.0000 0.5000 0.0000 0.0263(3) Uani 1 2 d S . . Mn2 Mn 0.06964(8) 0.81537(7) -0.00839(7) 0.0222(3) Uani 1 1 d . . . N1 N 0.2463(5) 0.8414(4) 0.1526(4) 0.0344(13) Uani 1 1 d . . . N2 N 0.9011(5) 0.7917(4) 0.8199(4) 0.0363(13) Uani 1 1 d . . . N3 N -0.1762(5) 0.4671(4) -0.1678(4) 0.0324(12) Uani 1 1 d . . . N4 N 0.6690(8) 0.1844(8) 0.3060(8) 0.087(3) Uani 1 1 d . . . O1 O -0.1754(4) 1.0355(4) 0.0241(4) 0.0407(12) Uani 1 1 d . . . O2 O -0.0297(4) 0.9215(3) 0.0777(3) 0.0337(10) Uani 1 1 d . . . O3 O -0.0328(4) 0.7317(4) 0.2157(4) 0.0438(12) Uani 1 1 d . . . O4 O -0.0438(4) 0.6796(3) 0.0414(3) 0.0323(10) Uani 1 1 d . . . O5 O -0.1661(5) 0.2741(4) 0.1141(4) 0.0481(13) Uani 1 1 d . . . O6 O -0.1228(5) 0.4263(4) 0.0595(4) 0.0460(12) Uani 1 1 d . . . O7 O -0.3026(4) 0.5619(3) 0.0781(3) 0.0343(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.039(4) 0.025(3) 0.031(4) 0.012(3) 0.014(3) 0.012(3) C2 0.028(4) 0.027(3) 0.034(4) 0.012(3) 0.014(3) 0.008(3) C3 0.037(4) 0.035(4) 0.046(4) 0.021(3) 0.016(3) 0.013(3) C4 0.028(4) 0.051(4) 0.051(4) 0.025(4) 0.012(3) 0.013(3) C5 0.028(4) 0.038(4) 0.047(4) 0.015(3) 0.014(3) 0.004(3) C6 0.035(4) 0.028(3) 0.032(4) 0.013(3) 0.016(3) 0.006(3) C7 0.030(4) 0.030(3) 0.030(3) 0.012(3) 0.016(3) 0.011(3) C8 0.032(4) 0.026(3) 0.038(4) 0.016(3) 0.016(3) 0.004(3) C9 0.037(4) 0.033(3) 0.037(4) 0.016(3) 0.018(3) 0.007(3) C10 0.057(5) 0.037(4) 0.053(5) 0.014(4) 0.029(4) 0.016(4) C11 0.063(6) 0.055(5) 0.039(4) 0.003(4) 0.025(4) 0.013(4) C12 0.077(6) 0.078(6) 0.040(4) 0.027(4) 0.037(4) 0.031(5) C13 0.050(5) 0.052(4) 0.047(4) 0.029(4) 0.025(4) 0.017(4) C14 0.030(4) 0.031(3) 0.031(3) 0.009(3) 0.016(3) 0.006(3) C15 0.021(3) 0.042(4) 0.029(3) 0.013(3) 0.009(3) 0.007(3) C16 0.033(4) 0.052(4) 0.034(4) 0.022(3) 0.009(3) 0.010(3) C17 0.028(4) 0.065(5) 0.035(4) 0.020(4) 0.008(3) 0.001(3) C18 0.036(4) 0.039(4) 0.027(3) 0.013(3) 0.008(3) 0.008(3) C19 0.032(4) 0.059(4) 0.026(3) 0.011(3) -0.001(3) 0.004(3) C20 0.035(4) 0.063(5) 0.028(4) 0.017(3) 0.010(3) 0.013(4) C21 0.029(4) 0.051(4) 0.029(4) 0.012(3) 0.010(3) 0.007(3) C22 0.034(4) 0.077(5) 0.040(4) 0.028(4) 0.014(4) 0.020(4) C23 0.032(4) 0.068(5) 0.049(5) 0.029(4) 0.009(4) 0.017(4) C24 0.030(4) 0.036(4) 0.036(4) 0.013(3) -0.002(3) 0.006(3) C25 0.036(4) 0.064(5) 0.033(4) 0.013(4) 0.008(3) 0.006(4) C26 0.029(4) 0.068(5) 0.043(4) 0.016(4) 0.013(3) 0.005(4) C27 0.033(4) 0.045(4) 0.039(4) 0.013(3) 0.007(3) 0.010(3) C28 0.036(4) 0.058(5) 0.038(4) 0.018(4) 0.008(3) 0.009(4) C29 0.040(4) 0.043(4) 0.032(4) 0.011(3) 0.007(3) 0.006(3) C30 0.045(5) 0.058(5) 0.032(4) 0.021(3) 0.013(3) 0.002(4) C31 0.035(4) 0.047(4) 0.026(4) 0.010(3) 0.005(3) -0.001(3) C32 0.039(4) 0.038(4) 0.032(4) 0.008(3) 0.010(3) -0.002(3) C33 0.039(4) 0.043(4) 0.040(4) 0.007(3) 0.013(3) 0.001(3) C34 0.101(9) 0.063(6) 0.102(9) 0.027(6) 0.059(7) 0.005(6) C35 0.080(8) 0.082(7) 0.065(6) 0.009(5) 0.034(6) 0.000(6) C36 0.054(6) 0.093(7) 0.063(6) 0.039(6) 0.026(5) -0.003(5) C37 0.099(9) 0.077(7) 0.073(7) 0.021(6) 0.040(6) 0.011(6) C38 0.109(10) 0.082(8) 0.078(7) 0.018(6) 0.031(7) 0.021(7) C39 0.099(9) 0.104(10) 0.087(8) 0.010(8) 0.054(7) -0.016(8) Mn1 0.0267(8) 0.0260(7) 0.0256(7) 0.0098(6) 0.0086(6) 0.0058(6) Mn2 0.0205(5) 0.0222(5) 0.0220(5) 0.0086(4) 0.0053(4) 0.0049(4) N1 0.035(3) 0.036(3) 0.032(3) 0.012(2) 0.013(3) 0.002(3) N2 0.037(3) 0.039(3) 0.030(3) 0.010(2) 0.011(3) 0.004(3) N3 0.028(3) 0.037(3) 0.032(3) 0.014(2) 0.009(2) 0.007(2) N4 0.073(6) 0.088(6) 0.087(7) 0.031(5) 0.017(5) 0.005(5) O1 0.041(3) 0.030(2) 0.053(3) 0.020(2) 0.016(2) 0.006(2) O2 0.028(3) 0.029(2) 0.042(3) 0.012(2) 0.011(2) 0.0055(19) O3 0.038(3) 0.061(3) 0.037(3) 0.023(2) 0.014(2) 0.009(2) O4 0.033(3) 0.029(2) 0.040(3) 0.011(2) 0.019(2) 0.010(2) O5 0.067(4) 0.031(3) 0.051(3) 0.014(2) 0.027(3) 0.015(2) O6 0.048(3) 0.058(3) 0.044(3) 0.017(2) 0.030(3) 0.007(2) O7 0.037(3) 0.032(2) 0.035(3) 0.016(2) 0.013(2) 0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.250(6) . ? C1 O2 1.257(7) . ? C1 C2 1.512(9) . ? C2 C3 1.383(8) . ? C2 C7 1.391(8) . ? C3 C4 1.360(9) . ? C3 H3 0.9300 . ? C4 C5 1.389(8) . ? C4 H4 0.9300 . ? C5 C6 1.369(8) . ? C5 H5 0.9300 . ? C6 C7 1.393(8) . ? C6 O7 1.415(7) . ? C7 C8 1.499(8) . ? C8 O3 1.232(7) . ? C8 O4 1.296(7) . ? C9 C10 1.379(9) . ? C9 O7 1.387(7) . ? C9 C14 1.398(8) . ? C10 C11 1.401(9) . ? C10 H10 0.9300 . ? C11 C12 1.374(10) . ? C11 H11 0.9300 . ? C12 C13 1.381(9) . ? C12 H12 0.9300 . ? C13 C14 1.392(8) . ? C13 H13 0.9300 . ? C14 C15 1.505(8) . ? C15 O5 1.234(7) . ? C15 O6 1.263(7) . ? C16 N3 1.325(8) . ? C16 C17 1.387(9) . ? C16 H16 0.9300 . ? C17 C18 1.385(9) . ? C17 H17 0.9300 . ? C18 C20 1.387(9) . ? C18 C19 1.450(9) . ? C19 C19 1.317(12) 2_464 ? C19 H19 0.9300 . ? C20 C21 1.363(8) . ? C20 H20 0.9300 . ? C21 N3 1.339(7) . ? C21 H21 0.9300 . ? C22 N1 1.344(8) . ? C22 C23 1.366(9) . ? C22 H22 0.9300 . ? C23 C24 1.393(9) . ? C23 H23 0.9300 . ? C24 C25 1.382(9) . ? C24 C27 1.472(9) . ? C25 C26 1.367(9) . ? C25 H25 0.9300 . ? C26 N1 1.355(8) . ? C26 H26 0.9300 . ? C27 C28 1.339(9) . ? C27 H27 0.9300 . ? C28 C29 1.452(9) . ? C28 H28 0.9300 . ? C29 C33 1.400(9) . ? C29 C30 1.400(10) . ? C30 C31 1.352(9) . ? C30 H30 0.9300 . ? C31 N2 1.351(8) . ? C31 H31 0.9300 . ? C32 N2 1.339(8) . ? C32 C33 1.355(9) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 N4 1.326(11) . ? C34 C35 1.416(13) . ? C34 H34 0.9300 . ? C35 C36 1.384(12) . ? C35 H35 0.9300 . ? C36 C37 1.382(12) . ? C36 C39 1.562(15) . ? C37 C38 1.371(13) . ? C37 H37 0.9300 . ? C38 N4 1.335(12) . ? C38 H38 0.9300 . ? C39 C39 1.249(19) 2_756 ? C39 H39 0.9300 . ? Mn1 O6 2.099(4) 2_565 ? Mn1 O6 2.099(4) . ? Mn1 O4 2.219(4) 2_565 ? Mn1 O4 2.219(4) . ? Mn1 N3 2.295(5) 2_565 ? Mn1 N3 2.295(5) . ? Mn2 O1 2.174(4) 2_575 ? Mn2 O2 2.182(4) . ? Mn2 O5 2.246(5) 2_565 ? Mn2 N1 2.253(5) . ? Mn2 N2 2.305(5) 1_454 ? Mn2 O4 2.372(4) . ? N2 Mn2 2.305(5) 1_656 ? O1 Mn2 2.174(4) 2_575 ? O5 Mn2 2.246(5) 2_565 ? 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 C1 O2 125.1(6) . . ? O1 C1 C2 116.1(6) . . ? O2 C1 C2 118.8(5) . . ? C3 C2 C7 119.9(6) . . ? C3 C2 C1 119.7(5) . . ? C7 C2 C1 120.3(6) . . ? C4 C3 C2 122.3(6) . . ? C4 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? C3 C4 C5 118.5(6) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? C6 C5 C4 119.6(6) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C7 122.5(5) . . ? C5 C6 O7 117.5(5) . . ? C7 C6 O7 119.3(5) . . ? C2 C7 C6 117.0(6) . . ? C2 C7 C8 124.9(6) . . ? C6 C7 C8 118.0(5) . . ? O3 C8 O4 124.8(6) . . ? O3 C8 C7 118.9(6) . . ? O4 C8 C7 116.2(5) . . ? C10 C9 O7 121.9(6) . . ? C10 C9 C14 121.9(6) . . ? O7 C9 C14 116.0(5) . . ? C9 C10 C11 118.2(6) . . ? C9 C10 H10 120.9 . . ? C11 C10 H10 120.9 . . ? C12 C11 C10 120.7(7) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C13 120.5(7) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C14 120.2(7) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C13 C14 C9 118.5(6) . . ? C13 C14 C15 118.4(6) . . ? C9 C14 C15 122.8(5) . . ? O5 C15 O6 123.7(6) . . ? O5 C15 C14 119.5(5) . . ? O6 C15 C14 116.8(5) . . ? N3 C16 C17 123.3(6) . . ? N3 C16 H16 118.4 . . ? C17 C16 H16 118.4 . . ? C18 C17 C16 120.2(7) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C20 115.6(6) . . ? C17 C18 C19 120.1(6) . . ? C20 C18 C19 124.3(6) . . ? C19 C19 C18 127.1(9) 2_464 . ? C19 C19 H19 116.4 2_464 . ? C18 C19 H19 116.4 . . ? C21 C20 C18 120.9(6) . . ? C21 C20 H20 119.5 . . ? C18 C20 H20 119.5 . . ? N3 C21 C20 123.4(6) . . ? N3 C21 H21 118.3 . . ? C20 C21 H21 118.3 . . ? N1 C22 C23 123.8(7) . . ? N1 C22 H22 118.1 . . ? C23 C22 H22 118.1 . . ? C22 C23 C24 120.2(7) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C25 C24 C23 116.0(6) . . ? C25 C24 C27 123.4(6) . . ? C23 C24 C27 120.5(7) . . ? C26 C25 C24 120.9(7) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? N1 C26 C25 123.1(7) . . ? N1 C26 H26 118.5 . . ? C25 C26 H26 118.5 . . ? C28 C27 C24 124.4(7) . . ? C28 C27 H27 117.8 . . ? C24 C27 H27 117.8 . . ? C27 C28 C29 128.4(7) . . ? C27 C28 H28 115.8 . . ? C29 C28 H28 115.8 . . ? C33 C29 C30 115.9(6) . . ? C33 C29 C28 118.7(7) . . ? C30 C29 C28 125.4(6) . . ? C31 C30 C29 120.6(6) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? N2 C31 C30 123.1(7) . . ? N2 C31 H31 118.5 . . ? C30 C31 H31 118.5 . . ? N2 C32 C33 124.1(6) . . ? N2 C32 H32 118.0 . . ? C33 C32 H32 118.0 . . ? C32 C33 C29 119.8(7) . . ? C32 C33 H33 120.1 . . ? C29 C33 H33 120.1 . . ? N4 C34 C35 123.4(10) . . ? N4 C34 H34 118.3 . . ? C35 C34 H34 118.3 . . ? C36 C35 C34 116.4(9) . . ? C36 C35 H35 121.8 . . ? C34 C35 H35 121.8 . . ? C37 C36 C35 119.7(9) . . ? C37 C36 C39 126.8(10) . . ? C35 C36 C39 113.5(9) . . ? C38 C37 C36 119.8(10) . . ? C38 C37 H37 120.1 . . ? C36 C37 H37 120.1 . . ? N4 C38 C37 121.8(10) . . ? N4 C38 H38 119.1 . . ? C37 C38 H38 119.1 . . ? C39 C39 C36 120.0(15) 2_756 . ? C39 C39 H39 120.0 2_756 . ? C36 C39 H39 120.0 . . ? O6 Mn1 O6 180.0 2_565 . ? O6 Mn1 O4 94.62(17) 2_565 2_565 ? O6 Mn1 O4 85.38(17) . 2_565 ? O6 Mn1 O4 85.38(17) 2_565 . ? O6 Mn1 O4 94.62(17) . . ? O4 Mn1 O4 180.0(2) 2_565 . ? O6 Mn1 N3 87.81(18) 2_565 2_565 ? O6 Mn1 N3 92.19(18) . 2_565 ? O4 Mn1 N3 85.99(17) 2_565 2_565 ? O4 Mn1 N3 94.01(17) . 2_565 ? O6 Mn1 N3 92.19(18) 2_565 . ? O6 Mn1 N3 87.81(18) . . ? O4 Mn1 N3 94.01(17) 2_565 . ? O4 Mn1 N3 85.99(17) . . ? N3 Mn1 N3 180.0(3) 2_565 . ? O1 Mn2 O2 94.80(16) 2_575 . ? O1 Mn2 O5 78.25(17) 2_575 2_565 ? O2 Mn2 O5 170.82(16) . 2_565 ? O1 Mn2 N1 83.98(17) 2_575 . ? O2 Mn2 N1 92.22(18) . . ? O5 Mn2 N1 92.97(19) 2_565 . ? O1 Mn2 N2 92.25(17) 2_575 1_454 ? O2 Mn2 N2 91.41(17) . 1_454 ? O5 Mn2 N2 82.98(19) 2_565 1_454 ? N1 Mn2 N2 174.97(19) . 1_454 ? O1 Mn2 O4 168.59(15) 2_575 . ? O2 Mn2 O4 75.29(14) . . ? O5 Mn2 O4 112.19(15) 2_565 . ? N1 Mn2 O4 90.67(16) . . ? N2 Mn2 O4 93.62(17) 1_454 . ? C22 N1 C26 115.8(6) . . ? C22 N1 Mn2 120.4(4) . . ? C26 N1 Mn2 123.8(5) . . ? C32 N2 C31 116.5(6) . . ? C32 N2 Mn2 122.8(4) . 1_656 ? C31 N2 Mn2 118.7(4) . 1_656 ? C16 N3 C21 116.6(5) . . ? C16 N3 Mn1 119.8(4) . . ? C21 N3 Mn1 122.3(4) . . ? C34 N4 C38 118.8(10) . . ? C1 O1 Mn2 131.9(4) . 2_575 ? C1 O2 Mn2 133.7(4) . . ? C8 O4 Mn1 126.2(3) . . ? C8 O4 Mn2 117.8(3) . . ? Mn1 O4 Mn2 112.38(17) . . ? C15 O5 Mn2 111.3(4) . 2_565 ? C15 O6 Mn1 160.1(4) . . ? C9 O7 C6 119.8(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 C1 C2 C3 8.1(8) . . . . ? O2 C1 C2 C3 -170.9(6) . . . . ? O1 C1 C2 C7 -174.0(6) . . . . ? O2 C1 C2 C7 6.9(9) . . . . ? C7 C2 C3 C4 -1.3(10) . . . . ? C1 C2 C3 C4 176.5(6) . . . . ? C2 C3 C4 C5 2.5(10) . . . . ? C3 C4 C5 C6 -0.7(10) . . . . ? C4 C5 C6 C7 -2.2(10) . . . . ? C4 C5 C6 O7 -172.9(5) . . . . ? C3 C2 C7 C6 -1.5(9) . . . . ? C1 C2 C7 C6 -179.3(5) . . . . ? C3 C2 C7 C8 175.1(6) . . . . ? C1 C2 C7 C8 -2.7(9) . . . . ? C5 C6 C7 C2 3.3(9) . . . . ? O7 C6 C7 C2 173.8(5) . . . . ? C5 C6 C7 C8 -173.6(6) . . . . ? O7 C6 C7 C8 -3.0(8) . . . . ? C2 C7 C8 O3 106.0(7) . . . . ? C6 C7 C8 O3 -77.4(8) . . . . ? C2 C7 C8 O4 -77.5(8) . . . . ? C6 C7 C8 O4 99.1(6) . . . . ? O7 C9 C10 C11 176.5(6) . . . . ? C14 C9 C10 C11 1.4(11) . . . . ? C9 C10 C11 C12 -1.8(12) . . . . ? C10 C11 C12 C13 0.8(13) . . . . ? C11 C12 C13 C14 0.6(12) . . . . ? C12 C13 C14 C9 -1.0(10) . . . . ? C12 C13 C14 C15 172.7(7) . . . . ? C10 C9 C14 C13 -0.1(10) . . . . ? O7 C9 C14 C13 -175.4(6) . . . . ? C10 C9 C14 C15 -173.5(6) . . . . ? O7 C9 C14 C15 11.2(9) . . . . ? C13 C14 C15 O5 41.5(9) . . . . ? C9 C14 C15 O5 -145.1(6) . . . . ? C13 C14 C15 O6 -135.9(6) . . . . ? C9 C14 C15 O6 37.5(9) . . . . ? N3 C16 C17 C18 -0.5(11) . . . . ? C16 C17 C18 C20 1.2(10) . . . . ? C16 C17 C18 C19 -176.8(6) . . . . ? C17 C18 C19 C19 172.6(9) . . . 2_464 ? C20 C18 C19 C19 -5.3(14) . . . 2_464 ? C17 C18 C20 C21 -0.5(10) . . . . ? C19 C18 C20 C21 177.4(6) . . . . ? C18 C20 C21 N3 -1.0(11) . . . . ? N1 C22 C23 C24 -1.6(12) . . . . ? C22 C23 C24 C25 -1.3(11) . . . . ? C22 C23 C24 C27 176.2(6) . . . . ? C23 C24 C25 C26 1.4(11) . . . . ? C27 C24 C25 C26 -176.0(7) . . . . ? C24 C25 C26 N1 1.3(12) . . . . ? C25 C24 C27 C28 13.2(11) . . . . ? C23 C24 C27 C28 -164.1(7) . . . . ? C24 C27 C28 C29 175.3(6) . . . . ? C27 C28 C29 C33 -173.0(7) . . . . ? C27 C28 C29 C30 5.6(13) . . . . ? C33 C29 C30 C31 0.3(10) . . . . ? C28 C29 C30 C31 -178.4(7) . . . . ? C29 C30 C31 N2 0.2(11) . . . . ? N2 C32 C33 C29 1.9(11) . . . . ? C30 C29 C33 C32 -1.3(10) . . . . ? C28 C29 C33 C32 177.4(6) . . . . ? N4 C34 C35 C36 -1.9(14) . . . . ? C34 C35 C36 C37 2.3(13) . . . . ? C34 C35 C36 C39 -178.0(8) . . . . ? C35 C36 C37 C38 0.2(14) . . . . ? C39 C36 C37 C38 -179.4(9) . . . . ? C36 C37 C38 N4 -3.6(16) . . . . ? C37 C36 C39 C39 -7.0(19) . . . 2_756 ? C35 C36 C39 C39 173.3(13) . . . 2_756 ? C23 C22 N1 C26 4.2(11) . . . . ? C23 C22 N1 Mn2 -174.9(6) . . . . ? C25 C26 N1 C22 -4.0(10) . . . . ? C25 C26 N1 Mn2 175.0(5) . . . . ? O1 Mn2 N1 C22 -49.6(5) 2_575 . . . ? O2 Mn2 N1 C22 -144.2(5) . . . . ? O5 Mn2 N1 C22 28.3(5) 2_565 . . . ? N2 Mn2 N1 C22 -8(2) 1_454 . . . ? O4 Mn2 N1 C22 140.5(5) . . . . ? O1 Mn2 N1 C26 131.4(5) 2_575 . . . ? O2 Mn2 N1 C26 36.8(5) . . . . ? O5 Mn2 N1 C26 -150.7(5) 2_565 . . . ? N2 Mn2 N1 C26 173.0(19) 1_454 . . . ? O4 Mn2 N1 C26 -38.5(5) . . . . ? C33 C32 N2 C31 -1.4(10) . . . . ? C33 C32 N2 Mn2 162.4(5) . . . 1_656 ? C30 C31 N2 C32 0.3(10) . . . . ? C30 C31 N2 Mn2 -164.2(5) . . . 1_656 ? C17 C16 N3 C21 -1.0(10) . . . . ? C17 C16 N3 Mn1 166.2(5) . . . . ? C20 C21 N3 C16 1.7(10) . . . . ? C20 C21 N3 Mn1 -165.2(5) . . . . ? O6 Mn1 N3 C16 -151.8(5) 2_565 . . . ? O6 Mn1 N3 C16 28.2(5) . . . . ? O4 Mn1 N3 C16 113.4(5) 2_565 . . . ? O4 Mn1 N3 C16 -66.5(5) . . . . ? N3 Mn1 N3 C16 10(100) 2_565 . . . ? O6 Mn1 N3 C21 14.7(5) 2_565 . . . ? O6 Mn1 N3 C21 -165.3(5) . . . . ? O4 Mn1 N3 C21 -80.1(5) 2_565 . . . ? O4 Mn1 N3 C21 99.9(5) . . . . ? N3 Mn1 N3 C21 176(100) 2_565 . . . ? C35 C34 N4 C38 -1.3(15) . . . . ? C37 C38 N4 C34 4.1(16) . . . . ? O2 C1 O1 Mn2 6.6(9) . . . 2_575 ? C2 C1 O1 Mn2 -172.4(4) . . . 2_575 ? O1 C1 O2 Mn2 -100.7(7) . . . . ? C2 C1 O2 Mn2 78.3(7) . . . . ? O1 Mn2 O2 C1 103.1(5) 2_575 . . . ? O5 Mn2 O2 C1 62.8(13) 2_565 . . . ? N1 Mn2 O2 C1 -172.7(5) . . . . ? N2 Mn2 O2 C1 10.7(5) 1_454 . . . ? O4 Mn2 O2 C1 -82.6(5) . . . . ? O3 C8 O4 Mn1 61.3(8) . . . . ? C7 C8 O4 Mn1 -114.9(5) . . . . ? O3 C8 O4 Mn2 -95.7(6) . . . . ? C7 C8 O4 Mn2 88.1(5) . . . . ? O6 Mn1 O4 C8 -157.8(5) 2_565 . . . ? O6 Mn1 O4 C8 22.2(5) . . . . ? O4 Mn1 O4 C8 15(47) 2_565 . . . ? N3 Mn1 O4 C8 -70.3(5) 2_565 . . . ? N3 Mn1 O4 C8 109.7(5) . . . . ? O6 Mn1 O4 Mn2 0.32(19) 2_565 . . . ? O6 Mn1 O4 Mn2 -179.68(19) . . . . ? O4 Mn1 O4 Mn2 173(41) 2_565 . . . ? N3 Mn1 O4 Mn2 87.8(2) 2_565 . . . ? N3 Mn1 O4 Mn2 -92.2(2) . . . . ? O1 Mn2 O4 C8 15.4(10) 2_575 . . . ? O2 Mn2 O4 C8 -14.9(4) . . . . ? O5 Mn2 O4 C8 170.7(4) 2_565 . . . ? N1 Mn2 O4 C8 77.2(4) . . . . ? N2 Mn2 O4 C8 -105.4(4) 1_454 . . . ? O1 Mn2 O4 Mn1 -144.7(7) 2_575 . . . ? O2 Mn2 O4 Mn1 -175.0(2) . . . . ? O5 Mn2 O4 Mn1 10.6(2) 2_565 . . . ? N1 Mn2 O4 Mn1 -82.9(2) . . . . ? N2 Mn2 O4 Mn1 94.5(2) 1_454 . . . ? O6 C15 O5 Mn2 11.2(8) . . . 2_565 ? C14 C15 O5 Mn2 -166.1(4) . . . 2_565 ? O5 C15 O6 Mn1 -79.4(15) . . . . ? C14 C15 O6 Mn1 97.9(13) . . . . ? O6 Mn1 O6 C15 -63(100) 2_565 . . . ? O4 Mn1 O6 C15 68.2(13) 2_565 . . . ? O4 Mn1 O6 C15 -111.8(13) . . . . ? N3 Mn1 O6 C15 -17.6(13) 2_565 . . . ? N3 Mn1 O6 C15 162.4(13) . . . . ? C10 C9 O7 C6 26.5(9) . . . . ? C14 C9 O7 C6 -158.2(6) . . . . ? C5 C6 O7 C9 -111.0(6) . . . . ? C7 C6 O7 C9 77.9(7) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.554 _refine_diff_density_min -0.607 _refine_diff_density_rms 0.159 data_1' _database_code_depnum_ccdc_archive 'CCDC 920717' #TrackingRef '(100K).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H54 Mn3 N8 O14' _chemical_formula_weight 1492.11 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 11.313(2) _cell_length_b 11.826(2) _cell_length_c 13.416(3) _cell_angle_alpha 103.917(4) _cell_angle_beta 112.404(3) _cell_angle_gamma 93.820(3) _cell_volume 1585.4(5) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1292 _cell_measurement_theta_min 3.105 _cell_measurement_theta_max 25.021 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 765 _exptl_absorpt_coefficient_mu 0.669 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8246 _exptl_absorpt_correction_T_max 0.8668 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruck 1000 CCD area detector' _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 7902 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.1088 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5461 _reflns_number_gt 3488 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _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^)+(0.1000P)^2^+0.5000P] 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 5461 _refine_ls_number_parameters 466 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1545 _refine_ls_R_factor_gt 0.0947 _refine_ls_wR_factor_ref 0.3351 _refine_ls_wR_factor_gt 0.2247 _refine_ls_goodness_of_fit_ref 1.836 _refine_ls_restrained_S_all 1.836 _refine_ls_shift/su_max 1.381 _refine_ls_shift/su_mean 0.005 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 0.5000 0.5000 0.0000 0.0053(5) Uani 1 2 d S . . Mn2 Mn 0.57064(13) 0.81454(12) -0.00635(12) 0.0054(4) Uani 1 1 d . . . C1 C 0.3578(10) 0.9451(9) 0.0469(9) 0.016(2) Uani 1 1 d . . . C2 C 0.2490(10) 0.8537(8) 0.0332(8) 0.009(2) Uani 1 1 d . . . C3 C 0.1192(9) 0.8668(9) -0.0163(8) 0.011(2) Uani 1 1 d . . . H3 H 0.1000 0.9359 -0.0391 0.014 Uiso 1 1 calc R . . C4 C 0.0172(10) 0.7808(9) -0.0332(9) 0.016(2) Uani 1 1 d . . . H4 H -0.0702 0.7903 -0.0698 0.019 Uiso 1 1 calc R . . C5 C 0.0429(9) 0.6844(9) 0.0025(9) 0.012(2) Uani 1 1 d . . . H5 H -0.0265 0.6268 -0.0075 0.014 Uiso 1 1 calc R . . C6 C 0.1732(9) 0.6684(8) 0.0550(8) 0.006(2) Uani 1 1 d . . . C7 C 0.2774(9) 0.7519(8) 0.0696(8) 0.006(2) Uani 1 1 d . . . C8 C 0.4087(10) 0.7206(8) 0.1159(9) 0.010(2) Uani 1 1 d . . . C9 C 0.2483(9) 0.5576(8) 0.1899(8) 0.005(2) Uani 1 1 d . . . C10 C 0.2329(10) 0.6394(9) 0.2757(8) 0.014(2) Uani 1 1 d . . . H10 H 0.1879 0.7025 0.2604 0.017 Uiso 1 1 calc R . . C11 C 0.2848(10) 0.6279(9) 0.3860(8) 0.011(2) Uani 1 1 d . . . H11 H 0.2800 0.6852 0.4469 0.013 Uiso 1 1 calc R . . C12 C 0.3418(10) 0.5321(10) 0.4023(9) 0.016(2) Uani 1 1 d . . . H12 H 0.3739 0.5215 0.4754 0.020 Uiso 1 1 calc R . . C13 C 0.3544(10) 0.4490(9) 0.3150(9) 0.016(2) Uani 1 1 d . . . H13 H 0.3955 0.3836 0.3295 0.020 Uiso 1 1 calc R . . C14 C 0.3087(9) 0.4611(8) 0.2109(8) 0.011(2) Uani 1 1 d . . . C15 C 0.3382(9) 0.3802(9) 0.1220(8) 0.010(2) Uani 1 1 d . . . C16 C 0.2053(9) 0.4635(8) -0.1687(8) 0.007(2) Uani 1 1 d . . . H16 H 0.1951 0.4612 -0.1022 0.009 Uiso 1 1 calc R . . C17 C 0.0976(10) 0.4650(10) -0.2619(9) 0.018(3) Uani 1 1 d . . . H17 H 0.0140 0.4589 -0.2606 0.021 Uiso 1 1 calc R . . C18 C 0.1122(10) 0.4756(9) -0.3570(8) 0.014(2) Uani 1 1 d . . . C19 C -0.0009(10) 0.4889(9) -0.4567(8) 0.013(2) Uani 1 1 d . . . H19 H -0.0835 0.4794 -0.4538 0.015 Uiso 1 1 calc R . . C20 C 0.2327(9) 0.4759(8) -0.3596(8) 0.010(2) Uani 1 1 d . . . H20 H 0.2455 0.4808 -0.4245 0.013 Uiso 1 1 calc R . . C21 C 0.3378(9) 0.4684(8) -0.2606(8) 0.006(2) Uani 1 1 d . . . H21 H 0.4211 0.4657 -0.2617 0.008 Uiso 1 1 calc R . . C22 C 0.8663(9) 0.8505(9) 0.1547(9) 0.014(2) Uani 1 1 d . . . H22 H 0.8732 0.8512 0.0864 0.017 Uiso 1 1 calc R . . C23 C 0.9799(10) 0.8605(9) 0.2487(8) 0.014(2) Uani 1 1 d . . . H23 H 1.0611 0.8681 0.2432 0.016 Uiso 1 1 calc R . . C24 C 0.9758(10) 0.8595(9) 0.3491(8) 0.011(2) Uani 1 1 d . . . C25 C 0.8495(10) 0.8518(9) 0.3525(9) 0.016(2) Uani 1 1 d . . . H25 H 0.8397 0.8522 0.4198 0.019 Uiso 1 1 calc R . . C26 C 0.7416(9) 0.8436(8) 0.2524(8) 0.009(2) Uani 1 1 d . . . H26 H 0.6585 0.8404 0.2546 0.011 Uiso 1 1 calc R . . C27 C 1.0906(10) 0.8610(9) 0.4478(9) 0.014(2) Uani 1 1 d . . . H27 H 1.1728 0.8842 0.4481 0.016 Uiso 1 1 calc R . . C28 C 1.0901(10) 0.8327(9) 0.5369(9) 0.015(2) Uani 1 1 d . . . H28 H 1.0071 0.8172 0.5378 0.018 Uiso 1 1 calc R . . C29 C 1.1991(10) 0.8221(10) 0.6337(8) 0.018(3) Uani 1 1 d . . . C30 C 1.3301(10) 0.8517(9) 0.6519(8) 0.011(2) Uani 1 1 d . . . H30 H 1.3531 0.8834 0.6017 0.013 Uiso 1 1 calc R . . C31 C 1.4266(9) 0.8321(8) 0.7491(9) 0.012(2) Uani 1 1 d . . . H31 H 1.5149 0.8527 0.7621 0.014 Uiso 1 1 calc R . . C32 C 1.2811(10) 0.7587(8) 0.8037(8) 0.012(2) Uani 1 1 d . . . H32 H 1.2640 0.7248 0.8553 0.015 Uiso 1 1 calc R . . C33 C 1.1784(10) 0.7744(9) 0.7153(8) 0.016(3) Uani 1 1 d . . . H33 H 1.0924 0.7534 0.7081 0.019 Uiso 1 1 calc R . . C34 C 0.2096(13) 0.0961(12) 0.2544(11) 0.037(3) Uani 1 1 d . . . H34 H 0.1683 0.0619 0.1751 0.044 Uiso 1 1 calc R . . C35 C 0.3116(14) 0.0419(12) 0.3187(12) 0.038(4) Uani 1 1 d . . . H35 H 0.3361 -0.0262 0.2828 0.046 Uiso 1 1 calc R . . C36 C 0.3723(12) 0.0917(12) 0.4336(11) 0.034(3) Uani 1 1 d . . . C37 C 0.3311(12) 0.1933(11) 0.4845(11) 0.028(3) Uani 1 1 d . . . H37 H 0.3733 0.2320 0.5630 0.034 Uiso 1 1 calc R . . C38 C 0.2305(13) 0.2319(12) 0.4170(12) 0.041(4) Uani 1 1 d . . . H38 H 0.1974 0.2929 0.4533 0.049 Uiso 1 1 calc R . . C39 C 0.4775(14) 0.0520(13) 0.5097(13) 0.049(4) Uani 1 1 d . . . H39 H 0.5217 0.1050 0.5833 0.058 Uiso 1 1 calc R . . N1 N 0.7480(7) 0.8401(7) 0.1546(7) 0.0063(17) Uani 1 1 d . . . N2 N 1.4040(8) 0.7890(7) 0.8201(7) 0.0080(18) Uani 1 1 d . . . N3 N 0.3237(7) 0.4652(7) -0.1685(7) 0.013(2) Uani 1 1 d . . . N4 N 0.1692(10) 0.1926(10) 0.3002(9) 0.036(3) Uani 1 1 d . . . O1 O 0.3207(6) 1.0338(5) 0.0197(6) 0.0095(15) Uani 1 1 d . . . O2 O 0.4693(6) 0.9230(5) 0.0807(6) 0.0091(15) Uani 1 1 d . . . O3 O 0.4649(6) 0.7330(6) 0.2163(6) 0.0108(15) Uani 1 1 d . . . O4 O 0.4569(6) 0.6809(6) 0.0424(6) 0.0123(16) Uani 1 1 d . . . O5 O 0.3293(7) 0.2730(6) 0.1138(5) 0.0118(16) Uani 1 1 d . . . O6 O 0.3756(6) 0.4266(6) 0.0598(6) 0.0110(15) Uani 1 1 d . . . O7 O 0.1924(6) 0.5619(5) 0.0791(5) 0.0082(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0036(10) 0.0052(11) 0.0020(11) -0.0018(8) -0.0021(9) -0.0011(8) Mn2 0.0019(8) 0.0047(8) 0.0032(8) -0.0001(6) -0.0049(6) 0.0003(6) C1 0.015(6) 0.006(5) 0.013(6) -0.015(4) 0.003(5) -0.004(4) C2 0.015(5) 0.007(5) 0.009(5) 0.005(4) 0.008(4) -0.005(4) C3 0.012(5) 0.009(5) 0.014(6) 0.004(4) 0.006(5) -0.002(4) C4 0.000(5) 0.020(6) 0.021(6) 0.005(5) -0.001(4) 0.003(4) C5 0.002(5) 0.014(6) 0.020(6) 0.010(5) 0.003(4) -0.004(4) C6 0.001(5) 0.002(5) 0.015(5) 0.002(4) 0.002(4) -0.004(4) C7 0.000(4) 0.008(5) 0.009(5) 0.010(4) -0.003(4) -0.001(4) C8 0.012(5) 0.003(5) 0.018(6) 0.010(4) 0.005(5) 0.002(4) C9 0.001(5) 0.010(5) 0.002(5) 0.004(4) -0.003(4) 0.000(4) C10 0.013(5) 0.016(6) 0.008(5) -0.004(4) 0.002(5) 0.006(4) C11 0.018(6) 0.012(5) 0.007(5) 0.002(4) 0.012(5) 0.001(4) C12 0.008(5) 0.030(7) 0.013(6) 0.003(5) 0.008(5) 0.008(5) C13 0.016(6) 0.012(6) 0.018(6) -0.001(5) 0.007(5) 0.000(4) C14 0.009(5) 0.006(5) 0.007(5) -0.001(4) -0.004(4) -0.003(4) C15 0.000(5) 0.021(6) 0.005(5) 0.002(4) -0.004(4) 0.003(4) C16 0.008(5) 0.011(5) 0.004(5) 0.005(4) 0.003(4) 0.001(4) C17 0.004(5) 0.023(6) 0.021(6) 0.006(5) 0.001(5) -0.003(4) C18 0.018(6) 0.010(5) 0.008(5) 0.008(4) -0.003(5) -0.004(4) C19 0.003(5) 0.020(6) 0.007(5) 0.004(5) -0.007(4) -0.002(4) C20 0.013(5) 0.008(5) 0.004(5) 0.000(4) -0.002(4) -0.001(4) C21 0.011(5) 0.010(5) 0.000(5) 0.008(4) 0.000(4) 0.009(4) C22 0.008(5) 0.023(6) 0.013(6) 0.008(5) 0.003(5) 0.006(4) C23 0.005(5) 0.020(6) 0.011(6) -0.001(5) 0.001(4) -0.001(4) C24 0.013(5) 0.010(5) 0.006(5) 0.008(4) -0.003(4) 0.004(4) C25 0.012(5) 0.017(6) 0.007(5) 0.002(4) -0.010(4) 0.009(4) C26 0.004(5) 0.010(5) 0.010(5) 0.002(4) -0.003(4) 0.006(4) C27 0.008(5) 0.009(5) 0.015(6) -0.003(4) -0.001(4) -0.001(4) C28 0.007(5) 0.018(6) 0.016(6) 0.002(5) 0.003(5) -0.002(4) C29 0.009(5) 0.021(6) 0.000(5) -0.015(4) -0.012(4) 0.005(5) C30 0.018(6) 0.014(5) 0.000(5) 0.000(4) 0.005(4) -0.007(4) C31 0.003(5) 0.007(5) 0.015(6) -0.005(4) -0.003(4) 0.000(4) C32 0.023(6) 0.005(5) 0.009(5) 0.008(4) 0.004(5) -0.003(4) C33 0.010(5) 0.016(6) 0.006(5) -0.004(4) -0.012(4) 0.008(4) C34 0.043(8) 0.032(8) 0.015(7) -0.009(6) 0.002(6) -0.006(6) C35 0.060(10) 0.026(7) 0.039(9) 0.011(6) 0.030(8) 0.006(7) C36 0.021(7) 0.050(9) 0.035(8) 0.018(7) 0.014(6) -0.001(6) C37 0.032(7) 0.031(7) 0.025(7) 0.012(6) 0.013(6) -0.005(6) C38 0.029(8) 0.039(8) 0.041(9) -0.010(7) 0.012(7) 0.009(6) C39 0.046(9) 0.053(10) 0.043(9) 0.024(8) 0.009(8) 0.011(8) N1 0.000(4) 0.012(4) 0.009(4) 0.005(3) 0.003(3) -0.002(3) N2 0.006(4) 0.013(5) 0.010(4) 0.013(4) 0.001(4) 0.009(3) N3 0.004(4) 0.009(4) 0.015(5) -0.011(4) 0.001(4) -0.006(3) N4 0.037(7) 0.032(7) 0.032(7) 0.008(5) 0.007(6) -0.001(5) O1 0.011(4) 0.002(3) 0.020(4) 0.015(3) 0.003(3) 0.006(3) O2 0.003(3) 0.004(3) 0.016(4) 0.004(3) -0.001(3) 0.004(3) O3 0.006(3) 0.016(4) 0.012(4) 0.010(3) 0.002(3) 0.003(3) O4 0.007(4) 0.014(4) 0.016(4) -0.004(3) 0.013(3) -0.009(3) O5 0.029(4) 0.003(4) 0.004(3) 0.001(3) 0.006(3) 0.008(3) O6 0.009(4) 0.019(4) 0.009(4) 0.006(3) 0.007(3) -0.001(3) O7 0.010(4) 0.005(3) 0.011(4) 0.009(3) 0.001(3) 0.003(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 O6 2.101(6) 2_665 ? Mn1 O6 2.101(6) . ? Mn1 O4 2.214(7) . ? Mn1 O4 2.214(7) 2_665 ? Mn1 N3 2.294(8) . ? Mn1 N3 2.294(8) 2_665 ? Mn2 O1 2.188(6) 2_675 ? Mn2 O2 2.195(7) . ? Mn2 N1 2.254(8) . ? Mn2 O5 2.261(7) 2_665 ? Mn2 N2 2.304(8) 1_454 ? Mn2 O4 2.335(7) . ? C1 O2 1.237(12) . ? C1 O1 1.239(12) . ? C1 C2 1.507(14) . ? C2 C3 1.399(14) . ? C2 C7 1.416(13) . ? C3 C4 1.397(14) . ? C3 H3 0.9500 . ? C4 C5 1.348(14) . ? C4 H4 0.9500 . ? C5 C6 1.419(13) . ? C5 H5 0.9500 . ? C6 O7 1.383(11) . ? C6 C7 1.407(12) . ? C7 C8 1.486(13) . ? C8 O3 1.217(12) . ? C8 O4 1.308(12) . ? C9 C10 1.390(13) . ? C9 O7 1.392(11) . ? C9 C14 1.400(13) . ? C10 C11 1.413(14) . ? C10 H10 0.9500 . ? C11 C12 1.363(14) . ? C11 H11 0.9500 . ? C12 C13 1.397(14) . ? C12 H12 0.9500 . ? C13 C14 1.339(15) . ? C13 H13 0.9500 . ? C14 C15 1.499(14) . ? C15 O5 1.239(12) . ? C15 O6 1.278(12) . ? C16 N3 1.337(12) . ? C16 C17 1.379(14) . ? C16 H16 0.9500 . ? C17 C18 1.380(15) . ? C17 H17 0.9500 . ? C18 C20 1.377(15) . ? C18 C19 1.509(14) . ? C19 C19 1.26(2) 2_564 ? C19 H19 0.9500 . ? C20 C21 1.433(13) . ? C20 H20 0.9500 . ? C21 N3 1.315(12) . ? C21 H21 0.9500 . ? C22 N1 1.335(12) . ? C22 C23 1.389(14) . ? C22 H22 0.9500 . ? C23 C24 1.368(14) . ? C23 H23 0.9500 . ? C24 C25 1.444(15) . ? C24 C27 1.455(14) . ? C25 C26 1.405(13) . ? C25 H25 0.9500 . ? C26 N1 1.333(12) . ? C26 H26 0.9500 . ? C27 C28 1.319(15) . ? C27 H27 0.9500 . ? C28 C29 1.449(14) . ? C28 H28 0.9500 . ? C29 C30 1.412(15) . ? C29 C33 1.430(16) . ? C30 C31 1.429(14) . ? C30 H30 0.9500 . ? C31 N2 1.277(13) . ? C31 H31 0.9500 . ? C32 N2 1.332(13) . ? C32 C33 1.370(14) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 N4 1.355(17) . ? C34 C35 1.447(19) . ? C34 H34 0.9500 . ? C35 C36 1.377(19) . ? C35 H35 0.9500 . ? C36 C37 1.432(18) . ? C36 C39 1.435(19) . ? C37 C38 1.343(18) . ? C37 H37 0.9500 . ? C38 N4 1.389(17) . ? C38 H38 0.9500 . ? C39 C39 1.37(3) 2_656 ? C39 H39 0.9500 . ? N2 Mn2 2.304(8) 1_656 ? O1 Mn2 2.188(6) 2_675 ? O5 Mn2 2.261(7) 2_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Mn1 O6 180.0 2_665 . ? O6 Mn1 O4 85.3(3) 2_665 . ? O6 Mn1 O4 94.7(3) . . ? O6 Mn1 O4 94.7(3) 2_665 2_665 ? O6 Mn1 O4 85.3(3) . 2_665 ? O4 Mn1 O4 180.0 . 2_665 ? O6 Mn1 N3 92.4(3) 2_665 . ? O6 Mn1 N3 87.6(3) . . ? O4 Mn1 N3 86.5(3) . . ? O4 Mn1 N3 93.5(3) 2_665 . ? O6 Mn1 N3 87.6(3) 2_665 2_665 ? O6 Mn1 N3 92.4(3) . 2_665 ? O4 Mn1 N3 93.5(3) . 2_665 ? O4 Mn1 N3 86.5(3) 2_665 2_665 ? N3 Mn1 N3 180.0(4) . 2_665 ? O1 Mn2 O2 94.3(2) 2_675 . ? O1 Mn2 N1 83.4(3) 2_675 . ? O2 Mn2 N1 92.8(3) . . ? O1 Mn2 O5 77.5(3) 2_675 2_665 ? O2 Mn2 O5 169.7(2) . 2_665 ? N1 Mn2 O5 92.5(3) . 2_665 ? O1 Mn2 N2 92.7(3) 2_675 1_454 ? O2 Mn2 N2 92.1(3) . 1_454 ? N1 Mn2 N2 174.0(3) . 1_454 ? O5 Mn2 N2 82.1(3) 2_665 1_454 ? O1 Mn2 O4 167.9(3) 2_675 . ? O2 Mn2 O4 75.3(2) . . ? N1 Mn2 O4 90.9(3) . . ? O5 Mn2 O4 113.5(2) 2_665 . ? N2 Mn2 O4 93.8(3) 1_454 . ? O2 C1 O1 128.5(10) . . ? O2 C1 C2 118.0(9) . . ? O1 C1 C2 113.5(9) . . ? C3 C2 C7 118.9(9) . . ? C3 C2 C1 121.1(9) . . ? C7 C2 C1 120.0(9) . . ? C4 C3 C2 121.7(9) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C5 C4 C3 119.9(9) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.4(9) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? O7 C6 C7 121.5(8) . . ? O7 C6 C5 117.3(8) . . ? C7 C6 C5 120.7(8) . . ? C6 C7 C2 118.3(8) . . ? C6 C7 C8 116.1(8) . . ? C2 C7 C8 125.5(8) . . ? O3 C8 O4 123.9(9) . . ? O3 C8 C7 120.3(9) . . ? O4 C8 C7 115.7(9) . . ? C10 C9 O7 121.2(8) . . ? C10 C9 C14 120.5(9) . . ? O7 C9 C14 118.0(8) . . ? C9 C10 C11 119.4(9) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C12 C11 C10 118.0(9) . . ? C12 C11 H11 121.0 . . ? C10 C11 H11 121.0 . . ? C11 C12 C13 122.1(10) . . ? C11 C12 H12 119.0 . . ? C13 C12 H12 119.0 . . ? C14 C13 C12 120.2(10) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C9 119.7(9) . . ? C13 C14 C15 119.3(9) . . ? C9 C14 C15 120.5(9) . . ? O5 C15 O6 122.9(9) . . ? O5 C15 C14 119.4(9) . . ? O6 C15 C14 117.7(9) . . ? N3 C16 C17 122.6(9) . . ? N3 C16 H16 118.7 . . ? C17 C16 H16 118.7 . . ? C16 C17 C18 119.4(10) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C20 C18 C17 119.2(9) . . ? C20 C18 C19 119.7(9) . . ? C17 C18 C19 121.1(10) . . ? C19 C19 C18 127.8(13) 2_564 . ? C19 C19 H19 116.1 2_564 . ? C18 C19 H19 116.1 . . ? C18 C20 C21 117.3(9) . . ? C18 C20 H20 121.3 . . ? C21 C20 H20 121.3 . . ? N3 C21 C20 122.7(9) . . ? N3 C21 H21 118.7 . . ? C20 C21 H21 118.7 . . ? N1 C22 C23 123.9(10) . . ? N1 C22 H22 118.1 . . ? C23 C22 H22 118.1 . . ? C24 C23 C22 120.6(10) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 116.8(9) . . ? C23 C24 C27 122.8(10) . . ? C25 C24 C27 120.3(9) . . ? C26 C25 C24 117.5(10) . . ? C26 C25 H25 121.3 . . ? C24 C25 H25 121.3 . . ? N1 C26 C25 124.4(9) . . ? N1 C26 H26 117.8 . . ? C25 C26 H26 117.8 . . ? C28 C27 C24 125.4(10) . . ? C28 C27 H27 117.3 . . ? C24 C27 H27 117.3 . . ? C27 C28 C29 128.8(10) . . ? C27 C28 H28 115.6 . . ? C29 C28 H28 115.6 . . ? C30 C29 C33 115.6(9) . . ? C30 C29 C28 123.6(11) . . ? C33 C29 C28 120.7(10) . . ? C29 C30 C31 117.0(9) . . ? C29 C30 H30 121.5 . . ? C31 C30 H30 121.5 . . ? N2 C31 C30 125.4(9) . . ? N2 C31 H31 117.3 . . ? C30 C31 H31 117.3 . . ? N2 C32 C33 122.5(10) . . ? N2 C32 H32 118.7 . . ? C33 C32 H32 118.7 . . ? C32 C33 C29 120.8(10) . . ? C32 C33 H33 119.6 . . ? C29 C33 H33 119.6 . . ? N4 C34 C35 124.0(12) . . ? N4 C34 H34 118.0 . . ? C35 C34 H34 118.0 . . ? C36 C35 C34 118.2(12) . . ? C36 C35 H35 120.9 . . ? C34 C35 H35 120.9 . . ? C35 C36 C37 119.1(12) . . ? C35 C36 C39 125.6(14) . . ? C37 C36 C39 115.3(13) . . ? C38 C37 C36 117.5(12) . . ? C38 C37 H37 121.3 . . ? C36 C37 H37 121.3 . . ? C37 C38 N4 127.4(13) . . ? C37 C38 H38 116.3 . . ? N4 C38 H38 116.3 . . ? C39 C39 C36 128.6(19) 2_656 . ? C39 C39 H39 115.7 2_656 . ? C36 C39 H39 115.7 . . ? C26 N1 C22 116.8(8) . . ? C26 N1 Mn2 122.9(6) . . ? C22 N1 Mn2 120.3(7) . . ? C31 N2 C32 118.6(8) . . ? C31 N2 Mn2 118.6(7) . 1_656 ? C32 N2 Mn2 120.5(7) . 1_656 ? C21 N3 C16 118.7(9) . . ? C21 N3 Mn1 121.3(6) . . ? C16 N3 Mn1 118.9(7) . . ? C34 N4 C38 113.5(11) . . ? C1 O1 Mn2 129.9(7) . 2_675 ? C1 O2 Mn2 131.8(6) . . ? C8 O4 Mn1 124.9(6) . . ? C8 O4 Mn2 119.6(6) . . ? Mn1 O4 Mn2 112.4(3) . . ? C15 O5 Mn2 110.3(6) . 2_665 ? C15 O6 Mn1 159.9(6) . . ? C6 O7 C9 120.8(7) . . ? 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 C1 C2 C3 -172.8(9) . . . . ? O1 C1 C2 C3 5.9(14) . . . . ? O2 C1 C2 C7 6.4(14) . . . . ? O1 C1 C2 C7 -174.8(9) . . . . ? C7 C2 C3 C4 -1.6(15) . . . . ? C1 C2 C3 C4 177.7(9) . . . . ? C2 C3 C4 C5 2.5(16) . . . . ? C3 C4 C5 C6 -1.4(16) . . . . ? C4 C5 C6 O7 -173.4(9) . . . . ? C4 C5 C6 C7 -0.7(16) . . . . ? O7 C6 C7 C2 174.1(9) . . . . ? C5 C6 C7 C2 1.6(15) . . . . ? O7 C6 C7 C8 -2.1(14) . . . . ? C5 C6 C7 C8 -174.5(9) . . . . ? C3 C2 C7 C6 -0.5(14) . . . . ? C1 C2 C7 C6 -179.7(9) . . . . ? C3 C2 C7 C8 175.2(10) . . . . ? C1 C2 C7 C8 -4.0(15) . . . . ? C6 C7 C8 O3 -78.9(12) . . . . ? C2 C7 C8 O3 105.3(12) . . . . ? C6 C7 C8 O4 101.4(10) . . . . ? C2 C7 C8 O4 -74.4(13) . . . . ? O7 C9 C10 C11 176.3(9) . . . . ? C14 C9 C10 C11 3.3(15) . . . . ? C9 C10 C11 C12 -3.8(15) . . . . ? C10 C11 C12 C13 2.5(15) . . . . ? C11 C12 C13 C14 -0.7(16) . . . . ? C12 C13 C14 C9 0.1(15) . . . . ? C12 C13 C14 C15 172.2(9) . . . . ? C10 C9 C14 C13 -1.5(15) . . . . ? O7 C9 C14 C13 -174.7(9) . . . . ? C10 C9 C14 C15 -173.4(9) . . . . ? O7 C9 C14 C15 13.4(13) . . . . ? C13 C14 C15 O5 43.5(13) . . . . ? C9 C14 C15 O5 -144.5(9) . . . . ? C13 C14 C15 O6 -134.4(10) . . . . ? C9 C14 C15 O6 37.6(13) . . . . ? N3 C16 C17 C18 -3.9(16) . . . . ? C16 C17 C18 C20 4.6(16) . . . . ? C16 C17 C18 C19 -174.3(9) . . . . ? C20 C18 C19 C19 -7(2) . . . 2_564 ? C17 C18 C19 C19 172.3(14) . . . 2_564 ? C17 C18 C20 C21 -1.8(14) . . . . ? C19 C18 C20 C21 177.2(9) . . . . ? C18 C20 C21 N3 -2.2(14) . . . . ? N1 C22 C23 C24 0.3(17) . . . . ? C22 C23 C24 C25 -2.0(15) . . . . ? C22 C23 C24 C27 175.4(9) . . . . ? C23 C24 C25 C26 1.2(14) . . . . ? C27 C24 C25 C26 -176.3(9) . . . . ? C24 C25 C26 N1 1.5(15) . . . . ? C23 C24 C27 C28 -163.2(11) . . . . ? C25 C24 C27 C28 14.1(16) . . . . ? C24 C27 C28 C29 174.2(10) . . . . ? C27 C28 C29 C30 5.8(18) . . . . ? C27 C28 C29 C33 -171.2(10) . . . . ? C33 C29 C30 C31 -0.5(14) . . . . ? C28 C29 C30 C31 -177.6(9) . . . . ? C29 C30 C31 N2 0.7(15) . . . . ? N2 C32 C33 C29 1.7(15) . . . . ? C30 C29 C33 C32 -0.6(14) . . . . ? C28 C29 C33 C32 176.6(10) . . . . ? N4 C34 C35 C36 0(2) . . . . ? C34 C35 C36 C37 0.8(19) . . . . ? C34 C35 C36 C39 -178.0(13) . . . . ? C35 C36 C37 C38 2.8(19) . . . . ? C39 C36 C37 C38 -178.2(13) . . . . ? C36 C37 C38 N4 -8(2) . . . . ? C35 C36 C39 C39 -13(3) . . . 2_656 ? C37 C36 C39 C39 168(2) . . . 2_656 ? C25 C26 N1 C22 -3.2(14) . . . . ? C25 C26 N1 Mn2 175.7(7) . . . . ? C23 C22 N1 C26 2.3(15) . . . . ? C23 C22 N1 Mn2 -176.6(8) . . . . ? O1 Mn2 N1 C26 131.5(8) 2_675 . . . ? O2 Mn2 N1 C26 37.5(8) . . . . ? O5 Mn2 N1 C26 -151.4(7) 2_665 . . . ? N2 Mn2 N1 C26 -178(2) 1_454 . . . ? O4 Mn2 N1 C26 -37.8(8) . . . . ? O1 Mn2 N1 C22 -49.7(8) 2_675 . . . ? O2 Mn2 N1 C22 -143.7(8) . . . . ? O5 Mn2 N1 C22 27.4(8) 2_665 . . . ? N2 Mn2 N1 C22 0(3) 1_454 . . . ? O4 Mn2 N1 C22 141.0(8) . . . . ? C30 C31 N2 C32 0.3(15) . . . . ? C30 C31 N2 Mn2 -162.7(8) . . . 1_656 ? C33 C32 N2 C31 -1.5(15) . . . . ? C33 C32 N2 Mn2 161.2(8) . . . 1_656 ? C20 C21 N3 C16 3.1(14) . . . . ? C20 C21 N3 Mn1 -164.5(7) . . . . ? C17 C16 N3 C21 0.0(14) . . . . ? C17 C16 N3 Mn1 167.8(8) . . . . ? O6 Mn1 N3 C21 15.2(7) 2_665 . . . ? O6 Mn1 N3 C21 -164.8(7) . . . . ? O4 Mn1 N3 C21 100.4(7) . . . . ? O4 Mn1 N3 C21 -79.6(7) 2_665 . . . ? N3 Mn1 N3 C21 -106(100) 2_665 . . . ? O6 Mn1 N3 C16 -152.3(7) 2_665 . . . ? O6 Mn1 N3 C16 27.7(7) . . . . ? O4 Mn1 N3 C16 -67.1(7) . . . . ? O4 Mn1 N3 C16 112.9(7) 2_665 . . . ? N3 Mn1 N3 C16 86(100) 2_665 . . . ? C35 C34 N4 C38 -3.4(19) . . . . ? C37 C38 N4 C34 8(2) . . . . ? O2 C1 O1 Mn2 5.0(16) . . . 2_675 ? C2 C1 O1 Mn2 -173.6(6) . . . 2_675 ? O1 C1 O2 Mn2 -98.4(12) . . . . ? C2 C1 O2 Mn2 80.1(12) . . . . ? O1 Mn2 O2 C1 101.5(9) 2_675 . . . ? N1 Mn2 O2 C1 -174.9(9) . . . . ? O5 Mn2 O2 C1 64.3(18) 2_665 . . . ? N2 Mn2 O2 C1 8.7(9) 1_454 . . . ? O4 Mn2 O2 C1 -84.7(9) . . . . ? O3 C8 O4 Mn1 64.9(12) . . . . ? C7 C8 O4 Mn1 -115.4(8) . . . . ? O3 C8 O4 Mn2 -93.4(10) . . . . ? C7 C8 O4 Mn2 86.3(9) . . . . ? O6 Mn1 O4 C8 -159.3(7) 2_665 . . . ? O6 Mn1 O4 C8 20.7(7) . . . . ? O4 Mn1 O4 C8 14(100) 2_665 . . . ? N3 Mn1 O4 C8 108.0(7) . . . . ? N3 Mn1 O4 C8 -72.0(7) 2_665 . . . ? O6 Mn1 O4 Mn2 0.2(3) 2_665 . . . ? O6 Mn1 O4 Mn2 -179.8(3) . . . . ? O4 Mn1 O4 Mn2 174(100) 2_665 . . . ? N3 Mn1 O4 Mn2 -92.4(3) . . . . ? N3 Mn1 O4 Mn2 87.6(3) 2_665 . . . ? O1 Mn2 O4 C8 16.7(16) 2_675 . . . ? O2 Mn2 O4 C8 -14.5(7) . . . . ? N1 Mn2 O4 C8 78.2(7) . . . . ? O5 Mn2 O4 C8 171.3(7) 2_665 . . . ? N2 Mn2 O4 C8 -105.6(7) 1_454 . . . ? O1 Mn2 O4 Mn1 -144.1(10) 2_675 . . . ? O2 Mn2 O4 Mn1 -175.3(4) . . . . ? N1 Mn2 O4 Mn1 -82.6(3) . . . . ? O5 Mn2 O4 Mn1 10.5(4) 2_665 . . . ? N2 Mn2 O4 Mn1 93.6(3) 1_454 . . . ? O6 C15 O5 Mn2 12.8(11) . . . 2_665 ? C14 C15 O5 Mn2 -165.0(7) . . . 2_665 ? O5 C15 O6 Mn1 -82(2) . . . . ? C14 C15 O6 Mn1 96(2) . . . . ? O6 Mn1 O6 C15 84(100) 2_665 . . . ? O4 Mn1 O6 C15 -111(2) . . . . ? O4 Mn1 O6 C15 69(2) 2_665 . . . ? N3 Mn1 O6 C15 163(2) . . . . ? N3 Mn1 O6 C15 -17(2) 2_665 . . . ? C7 C6 O7 C9 73.5(12) . . . . ? C5 C6 O7 C9 -113.8(10) . . . . ? C10 C9 O7 C6 30.0(13) . . . . ? C14 C9 O7 C6 -156.9(8) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.478 _refine_diff_density_min -2.451 _refine_diff_density_rms 0.303