# Electronic Supplementary Material (ESI) for Chemical Science # 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_jsk51_b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C65 H51 Mn4 N6 O12, 0.66(C4 H10 O), C3 H7 N O, 0.43(O)' _chemical_formula_sum 'C70.65 H64.63 Mn4 N7 O14.09' _chemical_formula_weight 1456.92 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.5671(8) _cell_length_b 12.5184(5) _cell_length_c 27.8828(11) _cell_angle_alpha 90.00 _cell_angle_beta 106.461(2) _cell_angle_gamma 90.00 _cell_volume 6549.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9015 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 26.79 _exptl_crystal_description Plate _exptl_crystal_colour Brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3001 _exptl_absorpt_coefficient_mu 0.826 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7335 _exptl_absorpt_correction_T_max 0.9521 _exptl_absorpt_process_details ? _exptl_special_details ; Crystals were mounted on a glass fiber using Paratone oil then placed on the diffractometer under a nitrogen stream at 100K. ; _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 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w scans; 9 settings' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 127022 _diffrn_reflns_av_R_equivalents 0.0798 _diffrn_reflns_av_sigmaI/netI 0.0612 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 28.34 _reflns_number_total 16313 _reflns_number_gt 11056 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.7-0' _computing_cell_refinement 'Bruker SAINT-Plus v7.68A' _computing_data_reduction 'Bruker SAINT-Plus v7.68A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF 2008' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The acetate bridging Mn3-Mn4 adopts two bridging modes, one mode is the usual kappa^2(O) mode as in the other acetates and the other with a single oxygen atom forming the bridge. Both orientations were refined with geometric restraints based on similar ligands in the model. The diethyl ether solvent was refined with geometric restraints, a fixed temperature factor and variable occupancy. No restraints were placed on the DMF. The lone oxygen (presumably water) was refined with a fixed temperature factor and a variable occupancy. The similar ADP and rigid-bond restraints were used on C2C. ; _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^+5.0000P] 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 16313 _refine_ls_number_parameters 891 _refine_ls_number_restraints 69 _refine_ls_R_factor_all 0.0970 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.1919 _refine_ls_wR_factor_gt 0.1784 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.012 _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 0.34565(3) 0.82186(5) 0.30024(2) 0.02264(14) Uani 1 1 d . A . Mn2 Mn 0.18691(3) 0.81124(4) 0.297058(19) 0.01774(13) Uani 1 1 d . A . Mn3 Mn 0.28522(3) 0.60272(4) 0.32293(2) 0.01797(13) Uani 1 1 d . . . Mn4 Mn 0.24663(4) 0.66777(5) 0.20206(2) 0.03636(18) Uani 1 1 d . A . O1 O 0.27679(13) 0.90029(19) 0.33365(9) 0.0194(5) Uani 1 1 d . . . O2 O 0.21557(13) 0.68353(19) 0.35276(9) 0.0208(5) Uani 1 1 d . A . O3 O 0.37401(13) 0.7120(2) 0.35607(9) 0.0245(6) Uani 1 1 d . A . O4 O 0.26804(15) 0.7281(3) 0.27284(10) 0.0390(8) Uani 1 1 d . A . O5 O 0.33570(16) 0.9011(3) 0.23348(11) 0.0378(7) Uani 1 1 d . . . O6 O 0.24004(17) 0.8324(2) 0.17787(12) 0.0402(8) Uani 1 1 d . . . O7 O 0.10131(14) 0.7665(2) 0.23448(10) 0.0283(6) Uani 1 1 d . . . O8 O 0.1361(2) 0.6403(3) 0.18953(12) 0.0455(8) Uani 1 1 d . . . C60 C 0.0901(2) 0.6961(3) 0.20083(17) 0.0368(10) Uani 1 1 d . A . C61 C 0.0126(3) 0.6803(5) 0.1710(3) 0.074(2) Uani 1 1 d . . . H61A H -0.0070 0.7482 0.1557 0.112 Uiso 1 1 calc R A . H61B H -0.0148 0.6556 0.1933 0.112 Uiso 1 1 calc R . . H61C H 0.0098 0.6270 0.1448 0.112 Uiso 1 1 calc R . . O9A O 0.3322(5) 0.4950(7) 0.2882(3) 0.033(2) Uani 0.323(6) 1 d PU A 2 O10A O 0.2645(6) 0.4934(9) 0.2117(4) 0.052(3) Uani 0.323(6) 1 d PU A 2 C62A C 0.3208(15) 0.473(2) 0.2457(12) 0.030(6) Uani 0.323(6) 1 d PU A 2 C63A C 0.3749(10) 0.3903(16) 0.2331(8) 0.061(6) Uani 0.323(6) 1 d P A 2 H63A H 0.3566 0.3671 0.1982 0.092 Uiso 0.323(6) 1 calc PR A 2 H63B H 0.3801 0.3283 0.2552 0.092 Uiso 0.323(6) 1 calc PR A 2 H63C H 0.4215 0.4246 0.2380 0.092 Uiso 0.323(6) 1 calc PR A 2 O9B O 0.2997(2) 0.5349(3) 0.25231(14) 0.0215(10) Uani 0.677(6) 1 d P A 1 O10B O 0.3346(2) 0.3714(3) 0.27914(17) 0.0324(12) Uani 0.677(6) 1 d P A 1 C62B C 0.3306(6) 0.4439(8) 0.2493(5) 0.024(2) Uani 0.677(6) 1 d PU A 1 C63B C 0.3601(5) 0.4311(6) 0.2057(3) 0.046(2) Uani 0.677(6) 1 d P A 1 H63D H 0.3808 0.3597 0.2065 0.069 Uiso 0.677(6) 1 calc PR A 1 H63E H 0.3970 0.4851 0.2075 0.069 Uiso 0.677(6) 1 calc PR A 1 H63F H 0.3217 0.4402 0.1746 0.069 Uiso 0.677(6) 1 calc PR A 1 O11 O 0.2436(3) 0.6173(4) 0.12881(16) 0.0727(13) Uani 1 1 d . . . O12 O 0.3485(2) 0.6873(4) 0.15658(18) 0.0852(16) Uani 1 1 d . . . N1 N 0.40190(16) 0.9617(2) 0.33494(12) 0.0226(6) Uani 1 1 d . . . N2 N 0.18032(16) 0.9867(2) 0.26066(11) 0.0216(6) Uani 1 1 d . . . N3 N 0.10678(17) 0.8085(3) 0.34190(12) 0.0248(7) Uani 1 1 d . . . N4 N 0.18432(16) 0.4974(2) 0.31220(11) 0.0208(6) Uani 1 1 d . A . N5 N 0.3641(2) 0.5147(3) 0.37924(14) 0.0444(11) Uani 1 1 d . A . N6 N 0.4463(2) 0.7360(4) 0.29191(15) 0.0441(10) Uani 1 1 d . . . C1 C 0.4725(2) 0.9755(4) 0.34805(16) 0.0316(9) Uani 1 1 d . A . H1 H 0.5012 0.9199 0.3409 0.038 Uiso 1 1 calc R . . C2 C 0.5059(2) 1.0661(4) 0.37139(18) 0.0410(11) Uani 1 1 d . . . H2 H 0.5563 1.0723 0.3811 0.049 Uiso 1 1 calc R A . C3 C 0.4637(2) 1.1475(4) 0.38025(19) 0.0419(11) Uani 1 1 d . A . H3 H 0.4848 1.2117 0.3958 0.050 Uiso 1 1 calc R . . C4 C 0.3898(2) 1.1356(3) 0.36640(16) 0.0323(9) Uani 1 1 d . . . H4 H 0.3602 1.1919 0.3716 0.039 Uiso 1 1 calc R A . C5 C 0.3601(2) 1.0399(3) 0.34479(14) 0.0233(8) Uani 1 1 d . A . C6 C 0.28062(19) 1.0108(3) 0.33355(13) 0.0211(7) Uani 1 1 d . A . C7 C 0.2370(2) 1.0504(3) 0.28150(14) 0.0227(7) Uani 1 1 d . A . C8 C 0.2512(2) 1.1420(3) 0.25822(15) 0.0316(9) Uani 1 1 d . . . H8 H 0.2916 1.1848 0.2735 0.038 Uiso 1 1 calc R A . C9 C 0.2053(3) 1.1703(4) 0.21200(17) 0.0389(11) Uani 1 1 d . A . H9 H 0.2138 1.2332 0.1955 0.047 Uiso 1 1 calc R . . C10 C 0.1476(2) 1.1061(3) 0.19033(16) 0.0359(10) Uani 1 1 d . . . H10 H 0.1155 1.1240 0.1588 0.043 Uiso 1 1 calc R A . C11 C 0.1372(2) 1.0147(3) 0.21566(14) 0.0256(8) Uani 1 1 d . A . H11 H 0.0979 0.9698 0.2005 0.031 Uiso 1 1 calc R . . C12 C 0.24839(19) 1.0613(3) 0.37339(14) 0.0230(8) Uani 1 1 d . . . C13 C 0.2122(2) 1.1585(3) 0.36380(16) 0.0318(9) Uani 1 1 d . A . H13 H 0.2104 1.1955 0.3337 0.038 Uiso 1 1 calc R . . C14 C 0.1785(2) 1.2031(4) 0.39684(18) 0.0375(10) Uani 1 1 d . . . H14 H 0.1545 1.2697 0.3894 0.045 Uiso 1 1 calc R A . C15 C 0.1802(2) 1.1496(4) 0.44038(18) 0.0395(11) Uani 1 1 d . A . H15 H 0.1567 1.1785 0.4630 0.047 Uiso 1 1 calc R . . C16 C 0.2163(2) 1.0540(3) 0.45094(15) 0.0301(9) Uani 1 1 d . . . H16 H 0.2171 1.0177 0.4810 0.036 Uiso 1 1 calc R A . C17 C 0.25158(19) 1.0089(3) 0.41895(13) 0.0219(7) Uani 1 1 d . A . C18 C 0.0610(2) 0.8875(3) 0.34298(17) 0.0340(9) Uani 1 1 d . A . H18 H 0.0649 0.9526 0.3264 0.041 Uiso 1 1 calc R . . C19 C 0.0081(3) 0.8791(4) 0.36698(19) 0.0410(11) Uani 1 1 d . . . H19 H -0.0234 0.9367 0.3671 0.049 Uiso 1 1 calc R A . C20 C 0.0031(2) 0.7842(4) 0.39063(17) 0.0365(10) Uani 1 1 d . A . H20 H -0.0331 0.7750 0.4069 0.044 Uiso 1 1 calc R . . C21 C 0.0500(2) 0.7033(3) 0.39071(15) 0.0290(9) Uani 1 1 d . . . H21 H 0.0469 0.6380 0.4073 0.035 Uiso 1 1 calc R A . C22 C 0.1026(2) 0.7174(3) 0.36622(13) 0.0223(7) Uani 1 1 d . A . C23 C 0.16068(19) 0.6341(3) 0.36660(13) 0.0218(7) Uani 1 1 d . . . C24 C 0.1330(2) 0.5428(3) 0.32808(13) 0.0211(7) Uani 1 1 d . A . C25 C 0.0631(2) 0.5083(3) 0.31239(15) 0.0289(9) Uani 1 1 d . . . H25 H 0.0273 0.5433 0.3235 0.035 Uiso 1 1 calc R A . C26 C 0.0462(2) 0.4214(3) 0.28000(16) 0.0320(9) Uani 1 1 d . A . H26 H -0.0013 0.3956 0.2689 0.038 Uiso 1 1 calc R . . C27 C 0.0993(2) 0.3734(3) 0.26428(15) 0.0308(9) Uani 1 1 d . . . H27 H 0.0893 0.3135 0.2425 0.037 Uiso 1 1 calc R A . C28 C 0.1673(2) 0.4139(3) 0.28076(14) 0.0261(8) Uani 1 1 d . A . H28 H 0.2038 0.3814 0.2695 0.031 Uiso 1 1 calc R . . C29 C 0.1874(2) 0.5817(3) 0.41959(14) 0.0246(8) Uani 1 1 d . A . C30 C 0.1530(2) 0.4906(3) 0.43035(16) 0.0328(9) Uani 1 1 d . . . H30 H 0.1119 0.4648 0.4060 0.039 Uiso 1 1 calc R A . C31 C 0.1772(3) 0.4362(4) 0.47580(16) 0.0395(11) Uani 1 1 d . A . H31 H 0.1520 0.3759 0.4825 0.047 Uiso 1 1 calc R . . C32 C 0.2386(3) 0.4713(4) 0.51105(16) 0.0429(12) Uani 1 1 d . . . H32 H 0.2571 0.4329 0.5413 0.051 Uiso 1 1 calc R A . C33 C 0.2724(3) 0.5624(4) 0.50169(16) 0.0384(11) Uani 1 1 d . A . H33 H 0.3137 0.5869 0.5262 0.046 Uiso 1 1 calc R . . C34 C 0.2472(2) 0.6198(3) 0.45689(14) 0.0262(8) Uani 1 1 d . . . C35 C 0.3500(3) 0.4248(4) 0.40057(19) 0.0591(17) Uani 1 1 d . . . H35 H 0.3028 0.3974 0.3906 0.071 Uiso 1 1 calc R A . C36 C 0.4011(4) 0.3704(4) 0.4365(2) 0.079(2) Uani 1 1 d . A . H36 H 0.3891 0.3089 0.4524 0.094 Uiso 1 1 calc R . . C37 C 0.4701(4) 0.4078(5) 0.4486(2) 0.079(3) Uani 1 1 d . . . H37 H 0.5071 0.3696 0.4715 0.095 Uiso 1 1 calc R A . C38 C 0.4849(3) 0.4990(4) 0.42771(19) 0.0630(19) Uani 1 1 d . A . H38 H 0.5322 0.5259 0.4366 0.076 Uiso 1 1 calc R . . C39 C 0.4306(2) 0.5540(4) 0.39297(16) 0.0417(12) Uani 1 1 d . . . C40 C 0.4400(2) 0.6634(4) 0.37090(16) 0.0363(11) Uani 1 1 d . A . C41 C 0.4679(2) 0.6550(4) 0.32414(19) 0.0442(13) Uani 1 1 d . A . C42 C 0.5120(3) 0.5740(6) 0.3162(2) 0.068(2) Uani 1 1 d . . . H42 H 0.5236 0.5132 0.3374 0.081 Uiso 1 1 calc R A . C43 C 0.5391(3) 0.5887(7) 0.2736(2) 0.075(2) Uani 1 1 d . A . H43 H 0.5711 0.5372 0.2672 0.090 Uiso 1 1 calc R . . C44 C 0.5202(3) 0.6741(7) 0.2422(3) 0.080(2) Uani 1 1 d . . . H44 H 0.5393 0.6847 0.2149 0.096 Uiso 1 1 calc R A . C45 C 0.4723(3) 0.7432(5) 0.2524(2) 0.0591(17) Uani 1 1 d . A . H45 H 0.4562 0.8008 0.2298 0.071 Uiso 1 1 calc R . . C46 C 0.4948(2) 0.7307(4) 0.41159(16) 0.0374(11) Uani 1 1 d . . . C47 C 0.5668(2) 0.7331(5) 0.4128(2) 0.0591(17) Uani 1 1 d . A . H47 H 0.5824 0.6897 0.3900 0.071 Uiso 1 1 calc R . . C48 C 0.6162(2) 0.7971(5) 0.4462(2) 0.0572(16) Uani 1 1 d . . . H48 H 0.6644 0.7986 0.4456 0.069 Uiso 1 1 calc R A . C49 C 0.5945(2) 0.8585(4) 0.48044(17) 0.0383(11) Uani 1 1 d . A . H49 H 0.6280 0.9014 0.5039 0.046 Uiso 1 1 calc R . . C50 C 0.5241(2) 0.8569(3) 0.48026(14) 0.0272(8) Uani 1 1 d . . . H50 H 0.5094 0.9006 0.5033 0.033 Uiso 1 1 calc R A . C51 C 0.4732(2) 0.7924(3) 0.44697(14) 0.0259(8) Uani 1 1 d . A . C52 C 0.3980(2) 0.7998(3) 0.44918(13) 0.0222(8) Uani 1 1 d . . . C53 C 0.36356(19) 0.8984(3) 0.43960(13) 0.0212(7) Uani 1 1 d . A . H53 H 0.3901 0.9605 0.4368 0.025 Uiso 1 1 calc R . . C54 C 0.29062(19) 0.9070(3) 0.43406(12) 0.0197(7) Uani 1 1 d . . . C55 C 0.2533(2) 0.8166(3) 0.44172(12) 0.0218(7) Uani 1 1 d . A . H55 H 0.2042 0.8224 0.4399 0.026 Uiso 1 1 calc R . . C56 C 0.2871(2) 0.7186(3) 0.45196(12) 0.0225(8) Uani 1 1 d . A . C57 C 0.3598(2) 0.7113(3) 0.45656(13) 0.0255(8) Uani 1 1 d . A . H57 H 0.3834 0.6446 0.4649 0.031 Uiso 1 1 calc R . . C58 C 0.2886(2) 0.8978(4) 0.19115(15) 0.0324(9) Uani 1 1 d . A . C59 C 0.2946(3) 0.9823(5) 0.15306(19) 0.0556(15) Uani 1 1 d . . . H59A H 0.3263 0.9564 0.1340 0.083 Uiso 1 1 calc R A . H59B H 0.3140 1.0483 0.1706 0.083 Uiso 1 1 calc R . . H59C H 0.2473 0.9964 0.1302 0.083 Uiso 1 1 calc R . . C64 C 0.3007(3) 0.6520(5) 0.12279(19) 0.0527(14) Uani 1 1 d . A . C65 C 0.3081(4) 0.6444(8) 0.0702(2) 0.096(3) Uani 1 1 d . . . H65A H 0.2628 0.6635 0.0460 0.143 Uiso 1 1 calc R A . H65B H 0.3210 0.5712 0.0638 0.143 Uiso 1 1 calc R . . H65C H 0.3454 0.6936 0.0667 0.143 Uiso 1 1 calc R . . O1C O 0.0280(2) 0.9577(4) 0.10651(14) 0.0720(13) Uani 1 1 d U . . N1C N 0.0720(2) 0.8541(5) 0.05705(18) 0.0689(16) Uani 1 1 d U . . C1C C 0.0742(3) 0.9035(5) 0.0959(2) 0.0607(16) Uani 1 1 d U . . H1C H 0.1182 0.8990 0.1213 0.073 Uiso 1 1 calc R . . C2C C 0.0071(8) 0.8463(11) 0.0188(5) 0.186(5) Uani 1 1 d U . . H2C1 H -0.0310 0.8252 0.0333 0.279 Uiso 1 1 calc R . . H2C2 H 0.0117 0.7926 -0.0057 0.279 Uiso 1 1 calc R . . H2C3 H -0.0044 0.9157 0.0022 0.279 Uiso 1 1 calc R . . C3C C 0.1280(3) 0.7946(6) 0.0459(3) 0.074(2) Uani 1 1 d U . . H3C1 H 0.1688 0.8416 0.0483 0.111 Uiso 1 1 calc R . . H3C2 H 0.1111 0.7656 0.0119 0.111 Uiso 1 1 calc R . . H3C3 H 0.1424 0.7358 0.0698 0.111 Uiso 1 1 calc R . . O1D O 0.1167(4) 0.3895(5) 0.0507(3) 0.090 Uiso 0.663(5) 1 d PD B -1 C1D C 0.0211(4) 0.5217(9) 0.0125(4) 0.090 Uiso 0.663(5) 1 d PD B -1 H1D1 H 0.0093 0.5976 0.0135 0.135 Uiso 0.663(5) 1 calc PR B -1 H1D2 H -0.0135 0.4788 0.0235 0.135 Uiso 0.663(5) 1 calc PR B -1 H1D3 H 0.0195 0.5017 -0.0218 0.135 Uiso 0.663(5) 1 calc PR B -1 C2D C 0.0964(5) 0.5012(5) 0.0473(4) 0.090 Uiso 0.663(5) 1 d PD B -1 H2D1 H 0.1312 0.5425 0.0351 0.108 Uiso 0.663(5) 1 calc PR B -1 H2D2 H 0.0987 0.5277 0.0812 0.108 Uiso 0.663(5) 1 calc PR B -1 C3D C 0.1831(5) 0.3698(6) 0.0891(4) 0.090 Uiso 0.663(5) 1 d PD B -1 H3D1 H 0.1776 0.3859 0.1226 0.108 Uiso 0.663(5) 1 calc PR B -1 H3D2 H 0.2215 0.4154 0.0836 0.108 Uiso 0.663(5) 1 calc PR B -1 C4D C 0.2011(6) 0.2509(6) 0.0854(4) 0.090 Uiso 0.663(5) 1 d PD B -1 H4D1 H 0.2432 0.2325 0.1129 0.135 Uiso 0.663(5) 1 calc PR B -1 H4D2 H 0.2110 0.2377 0.0534 0.135 Uiso 0.663(5) 1 calc PR B -1 H4D3 H 0.1606 0.2070 0.0876 0.135 Uiso 0.663(5) 1 calc PR B -1 O1E O 0.4182(7) 0.8432(11) 0.1184(5) 0.100 Uiso 0.428(10) 1 d P . . 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 0.0219(3) 0.0261(3) 0.0202(3) -0.0018(2) 0.0062(2) -0.0076(2) Mn2 0.0153(2) 0.0188(3) 0.0185(3) -0.0010(2) 0.0038(2) -0.0020(2) Mn3 0.0170(3) 0.0161(3) 0.0198(3) -0.0013(2) 0.0036(2) 0.0003(2) Mn4 0.0591(5) 0.0291(3) 0.0218(3) 0.0005(2) 0.0131(3) 0.0168(3) O1 0.0180(12) 0.0175(12) 0.0217(12) -0.0028(9) 0.0043(10) -0.0028(10) O2 0.0209(12) 0.0217(13) 0.0215(12) -0.0057(10) 0.0087(10) -0.0085(10) O3 0.0174(12) 0.0295(14) 0.0238(13) -0.0074(11) 0.0015(10) 0.0040(11) O4 0.0237(14) 0.075(2) 0.0162(13) -0.0086(14) 0.0018(11) 0.0188(15) O5 0.0306(15) 0.0514(19) 0.0285(15) 0.0115(14) 0.0038(12) -0.0119(14) O6 0.0375(17) 0.0360(17) 0.0387(17) 0.0020(14) -0.0026(14) 0.0011(14) O7 0.0222(13) 0.0235(14) 0.0322(15) -0.0056(11) -0.0040(11) 0.0023(11) O8 0.064(2) 0.0277(16) 0.0410(18) -0.0102(14) 0.0088(16) 0.0048(16) C60 0.038(2) 0.025(2) 0.036(2) -0.0006(17) -0.0077(19) 0.0006(18) C61 0.050(3) 0.050(3) 0.093(5) -0.035(3) -0.028(3) -0.008(3) O9A 0.040(5) 0.030(5) 0.028(5) -0.002(4) 0.009(4) 0.012(4) O10A 0.053(3) 0.052(3) 0.052(3) -0.0003(10) 0.0149(13) 0.0002(10) C62A 0.033(9) 0.027(10) 0.031(8) -0.002(8) 0.010(6) 0.005(8) C63A 0.053(11) 0.062(12) 0.055(11) -0.027(10) -0.007(9) 0.028(9) O9B 0.024(2) 0.015(2) 0.027(2) -0.0016(16) 0.0106(17) 0.0035(17) O10B 0.037(2) 0.021(2) 0.041(3) 0.0033(18) 0.014(2) 0.0053(18) C62B 0.022(4) 0.016(4) 0.032(4) -0.001(4) 0.004(3) 0.006(3) C63B 0.057(5) 0.042(4) 0.045(4) -0.001(4) 0.025(4) 0.026(4) O11 0.090(3) 0.082(3) 0.062(3) -0.029(2) 0.046(2) -0.019(3) O12 0.059(3) 0.100(4) 0.077(3) -0.029(3) -0.012(2) 0.033(3) N1 0.0200(15) 0.0231(16) 0.0249(15) 0.0012(12) 0.0066(12) -0.0025(12) N2 0.0185(14) 0.0232(16) 0.0220(15) 0.0007(12) 0.0042(12) -0.0002(12) N3 0.0250(16) 0.0237(16) 0.0272(16) -0.0056(13) 0.0095(13) -0.0025(13) N4 0.0224(15) 0.0204(15) 0.0213(14) -0.0047(12) 0.0089(12) -0.0042(12) N5 0.054(2) 0.0210(18) 0.041(2) -0.0059(15) -0.0163(18) 0.0064(17) N6 0.0259(19) 0.064(3) 0.044(2) -0.027(2) 0.0122(17) -0.0102(19) C1 0.0220(19) 0.036(2) 0.038(2) 0.0015(18) 0.0094(17) -0.0062(17) C2 0.022(2) 0.045(3) 0.053(3) -0.005(2) 0.0054(19) -0.0110(19) C3 0.034(2) 0.035(2) 0.053(3) -0.012(2) 0.008(2) -0.019(2) C4 0.031(2) 0.026(2) 0.040(2) -0.0079(17) 0.0099(18) -0.0074(17) C5 0.0235(18) 0.0210(18) 0.0237(18) -0.0015(14) 0.0042(14) -0.0046(15) C6 0.0212(17) 0.0181(17) 0.0225(17) -0.0013(13) 0.0038(14) -0.0018(14) C7 0.0219(18) 0.0210(18) 0.0254(18) 0.0004(14) 0.0072(15) -0.0011(15) C8 0.034(2) 0.028(2) 0.031(2) -0.0002(16) 0.0071(17) -0.0062(18) C9 0.047(3) 0.032(2) 0.036(2) 0.0141(18) 0.009(2) -0.002(2) C10 0.038(2) 0.035(2) 0.030(2) 0.0099(18) 0.0023(18) 0.0067(19) C11 0.0234(18) 0.029(2) 0.0233(18) 0.0030(15) 0.0043(15) 0.0035(16) C12 0.0186(17) 0.0214(18) 0.0277(19) -0.0041(14) 0.0045(14) -0.0018(14) C13 0.036(2) 0.027(2) 0.031(2) 0.0016(16) 0.0074(18) 0.0100(18) C14 0.035(2) 0.032(2) 0.044(3) -0.0044(19) 0.010(2) 0.0164(19) C15 0.040(3) 0.041(3) 0.041(3) -0.009(2) 0.017(2) 0.014(2) C16 0.030(2) 0.032(2) 0.029(2) -0.0046(17) 0.0089(17) 0.0042(17) C17 0.0177(16) 0.0221(18) 0.0238(17) -0.0063(14) 0.0026(14) -0.0020(14) C18 0.039(2) 0.025(2) 0.044(2) -0.0039(18) 0.019(2) -0.0016(18) C19 0.041(3) 0.035(2) 0.056(3) -0.009(2) 0.027(2) 0.002(2) C20 0.033(2) 0.041(2) 0.043(3) -0.011(2) 0.023(2) -0.007(2) C21 0.031(2) 0.030(2) 0.030(2) -0.0075(16) 0.0157(17) -0.0088(17) C22 0.0225(18) 0.0253(18) 0.0210(17) -0.0075(14) 0.0090(14) -0.0067(15) C23 0.0213(17) 0.0247(18) 0.0197(17) -0.0059(14) 0.0063(14) -0.0098(15) C24 0.0250(18) 0.0205(17) 0.0172(16) -0.0033(13) 0.0050(14) -0.0055(14) C25 0.0252(19) 0.034(2) 0.031(2) -0.0105(17) 0.0133(16) -0.0091(17) C26 0.025(2) 0.035(2) 0.038(2) -0.0133(18) 0.0109(17) -0.0138(17) C27 0.027(2) 0.032(2) 0.033(2) -0.0130(17) 0.0089(17) -0.0097(17) C28 0.0271(19) 0.0252(19) 0.0267(19) -0.0074(15) 0.0085(15) -0.0050(16) C29 0.030(2) 0.0232(19) 0.0235(18) -0.0028(14) 0.0120(15) -0.0030(16) C30 0.043(2) 0.029(2) 0.029(2) -0.0045(17) 0.0151(18) -0.0098(19) C31 0.060(3) 0.030(2) 0.032(2) -0.0008(18) 0.018(2) -0.012(2) C32 0.069(3) 0.032(2) 0.024(2) 0.0042(17) 0.006(2) -0.010(2) C33 0.049(3) 0.032(2) 0.027(2) 0.0012(17) 0.0005(19) -0.008(2) C34 0.032(2) 0.0236(19) 0.0225(18) -0.0051(15) 0.0077(16) -0.0045(16) C35 0.087(4) 0.024(2) 0.042(3) -0.001(2) -0.022(3) -0.001(2) C36 0.143(7) 0.021(2) 0.042(3) -0.003(2) -0.023(4) 0.023(3) C37 0.104(5) 0.043(3) 0.048(3) -0.021(3) -0.045(3) 0.039(3) C38 0.068(4) 0.049(3) 0.044(3) -0.023(2) -0.030(3) 0.036(3) C39 0.040(2) 0.033(2) 0.035(2) -0.0196(19) -0.0162(19) 0.018(2) C40 0.0184(19) 0.042(2) 0.039(2) -0.0234(19) -0.0081(17) 0.0095(17) C41 0.0151(18) 0.066(3) 0.049(3) -0.038(3) 0.0045(18) -0.001(2) C42 0.028(2) 0.094(5) 0.073(4) -0.055(4) -0.001(2) 0.016(3) C43 0.028(3) 0.129(6) 0.066(4) -0.064(4) 0.010(3) 0.009(3) C44 0.042(3) 0.137(7) 0.064(4) -0.045(5) 0.020(3) -0.001(4) C45 0.036(3) 0.095(5) 0.054(3) -0.040(3) 0.027(2) -0.018(3) C46 0.0208(19) 0.047(3) 0.036(2) -0.021(2) -0.0060(17) 0.0103(18) C47 0.023(2) 0.082(4) 0.064(3) -0.046(3) -0.002(2) 0.008(2) C48 0.020(2) 0.078(4) 0.065(3) -0.038(3) -0.003(2) 0.007(2) C49 0.022(2) 0.038(2) 0.044(3) -0.014(2) -0.0082(18) 0.0000(18) C50 0.0265(19) 0.0244(19) 0.0249(19) -0.0049(15) -0.0019(15) 0.0027(16) C51 0.0234(18) 0.0227(19) 0.0248(18) -0.0053(15) -0.0043(15) 0.0044(15) C52 0.0253(18) 0.0225(18) 0.0141(16) -0.0053(13) -0.0024(13) 0.0014(15) C53 0.0242(18) 0.0200(17) 0.0179(16) -0.0047(13) 0.0033(14) -0.0021(14) C54 0.0224(17) 0.0203(17) 0.0153(15) -0.0058(13) 0.0034(13) -0.0001(14) C55 0.0227(18) 0.0276(19) 0.0138(15) -0.0059(14) 0.0031(13) -0.0020(15) C56 0.032(2) 0.0194(17) 0.0127(15) -0.0022(13) 0.0009(14) -0.0039(15) C57 0.030(2) 0.0206(18) 0.0184(17) -0.0030(14) -0.0056(15) 0.0004(15) C58 0.031(2) 0.045(3) 0.026(2) 0.0040(18) 0.0148(17) 0.005(2) C59 0.050(3) 0.079(4) 0.040(3) 0.024(3) 0.017(2) 0.004(3) C64 0.054(3) 0.064(4) 0.035(3) 0.006(2) 0.004(2) 0.022(3) C65 0.070(4) 0.185(9) 0.037(3) 0.033(4) 0.024(3) 0.061(5) O1C 0.046(2) 0.114(4) 0.049(2) -0.025(2) 0.0018(18) 0.034(2) N1C 0.032(2) 0.128(5) 0.046(3) -0.027(3) 0.0093(19) 0.020(3) C1C 0.036(3) 0.094(5) 0.046(3) -0.013(3) 0.003(2) 0.022(3) C2C 0.185(5) 0.187(5) 0.186(5) -0.0016(10) 0.0523(17) 0.0010(10) C3C 0.048(3) 0.093(5) 0.089(5) -0.034(4) 0.030(3) 0.007(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 O4 1.900(3) . ? Mn1 O3 2.033(3) . ? Mn1 O5 2.069(3) . ? Mn1 O1 2.088(3) . ? Mn1 N1 2.147(3) . ? Mn1 N6 2.313(4) . ? Mn1 Mn2 3.0850(8) . ? Mn1 Mn3 3.1220(8) . ? Mn1 Mn4 3.4588(9) . ? Mn2 O1 2.088(2) . ? Mn2 O7 2.123(3) . ? Mn2 O4 2.160(3) . ? Mn2 O2 2.188(3) . ? Mn2 N3 2.266(3) . ? Mn2 N2 2.408(3) . ? Mn2 Mn3 3.2013(7) . ? Mn2 Mn4 3.6554(8) . ? Mn3 O9A 2.025(9) . ? Mn3 O2 2.053(3) . ? Mn3 O4 2.064(3) . ? Mn3 N5 2.165(4) . ? Mn3 O3 2.198(3) . ? Mn3 O9B 2.235(4) . ? Mn3 N4 2.322(3) . ? Mn3 Mn4 3.3391(8) . ? Mn4 O4 2.043(3) . ? Mn4 O8 2.118(4) . ? Mn4 O11 2.123(4) . ? Mn4 O6 2.161(3) . ? Mn4 O10A 2.215(12) . ? Mn4 O9B 2.233(4) . ? O1 C6 1.386(4) . ? O2 C23 1.386(4) . ? O3 C40 1.381(4) . ? O5 C58 1.275(5) . ? O6 C58 1.229(5) . ? O7 C60 1.260(5) . ? O8 C60 1.249(6) . ? C60 C61 1.521(6) . ? O9A C62A 1.18(3) . ? O10A C62A 1.26(3) . ? C62A C63A 1.59(3) . ? O9B C62B 1.304(10) . ? O10B C62B 1.217(13) . ? C62B C63B 1.494(17) . ? O11 C64 1.254(7) . ? O12 C64 1.207(7) . ? N1 C1 1.336(5) . ? N1 C5 1.352(5) . ? N2 C11 1.344(5) . ? N2 C7 1.355(5) . ? N3 C18 1.341(5) . ? N3 C22 1.341(5) . ? N4 C24 1.334(5) . ? N4 C28 1.345(5) . ? N5 C35 1.337(7) . ? N5 C39 1.341(6) . ? N6 C45 1.342(7) . ? N6 C41 1.341(7) . ? C1 C2 1.377(6) . ? C2 C3 1.377(7) . ? C3 C4 1.393(6) . ? C4 C5 1.392(5) . ? C5 C6 1.541(5) . ? C6 C7 1.542(5) . ? C6 C12 1.558(5) . ? C7 C8 1.383(5) . ? C8 C9 1.391(6) . ? C9 C10 1.379(6) . ? C10 C11 1.389(6) . ? C12 C13 1.395(5) . ? C12 C17 1.416(5) . ? C13 C14 1.393(6) . ? C14 C15 1.378(7) . ? C15 C16 1.378(6) . ? C16 C17 1.393(5) . ? C17 C54 1.485(5) . ? C18 C19 1.386(6) . ? C19 C20 1.375(7) . ? C20 C21 1.366(6) . ? C21 C22 1.398(5) . ? C22 C23 1.541(5) . ? C23 C24 1.556(5) . ? C23 C29 1.565(5) . ? C24 C25 1.382(5) . ? C25 C26 1.393(5) . ? C26 C27 1.376(6) . ? C27 C28 1.375(5) . ? C29 C30 1.399(6) . ? C29 C34 1.411(5) . ? C30 C31 1.398(6) . ? C31 C32 1.390(7) . ? C32 C33 1.379(6) . ? C33 C34 1.404(6) . ? C34 C56 1.489(5) . ? C35 C36 1.378(7) . ? C36 C37 1.378(11) . ? C37 C38 1.350(10) . ? C38 C39 1.400(6) . ? C39 C40 1.534(7) . ? C40 C41 1.552(7) . ? C40 C46 1.568(5) . ? C41 C42 1.390(7) . ? C42 C43 1.443(10) . ? C43 C44 1.365(11) . ? C44 C45 1.363(9) . ? C46 C47 1.399(6) . ? C46 C51 1.409(6) . ? C47 C48 1.391(6) . ? C48 C49 1.381(7) . ? C49 C50 1.378(6) . ? C50 C51 1.407(5) . ? C51 C52 1.492(6) . ? C52 C57 1.385(5) . ? C52 C53 1.396(5) . ? C53 C54 1.395(5) . ? C54 C55 1.395(5) . ? C55 C56 1.385(5) . ? C56 C57 1.394(6) . ? C58 C59 1.527(6) . ? C64 C65 1.518(8) . ? O1C C1C 1.231(6) . ? N1C C1C 1.237(7) . ? N1C C2C 1.411(15) . ? N1C C3C 1.430(7) . ? O1D C2D 1.4498(10) . ? O1D C3D 1.4508(10) . ? C1D C2D 1.5395(10) . ? C3D C4D 1.5396(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 O4 Mn1 O3 84.47(12) . . ? O4 Mn1 O5 94.23(12) . . ? O3 Mn1 O5 161.58(13) . . ? O4 Mn1 O1 85.79(11) . . ? O3 Mn1 O1 92.71(10) . . ? O5 Mn1 O1 105.54(12) . . ? O4 Mn1 N1 159.11(13) . . ? O3 Mn1 N1 102.29(11) . . ? O5 Mn1 N1 85.41(12) . . ? O1 Mn1 N1 74.26(11) . . ? O4 Mn1 N6 106.19(13) . . ? O3 Mn1 N6 72.96(14) . . ? O5 Mn1 N6 89.88(15) . . ? O1 Mn1 N6 159.92(12) . . ? N1 Mn1 N6 94.70(13) . . ? O4 Mn1 Mn2 43.81(9) . . ? O3 Mn1 Mn2 92.70(8) . . ? O5 Mn1 Mn2 99.06(9) . . ? O1 Mn1 Mn2 42.37(7) . . ? N1 Mn1 Mn2 115.56(9) . . ? N6 Mn1 Mn2 148.90(11) . . ? O4 Mn1 Mn3 39.93(9) . . ? O3 Mn1 Mn3 44.55(7) . . ? O5 Mn1 Mn3 131.22(9) . . ? O1 Mn1 Mn3 89.63(7) . . ? N1 Mn1 Mn3 143.18(9) . . ? N6 Mn1 Mn3 89.66(12) . . ? Mn2 Mn1 Mn3 62.092(17) . . ? O4 Mn1 Mn4 29.84(9) . . ? O3 Mn1 Mn4 101.47(7) . . ? O5 Mn1 Mn4 70.51(9) . . ? O1 Mn1 Mn4 109.14(7) . . ? N1 Mn1 Mn4 155.79(9) . . ? N6 Mn1 Mn4 87.89(9) . . ? Mn2 Mn1 Mn4 67.641(19) . . ? Mn3 Mn1 Mn4 60.725(18) . . ? O1 Mn2 O7 154.37(11) . . ? O1 Mn2 O4 79.52(11) . . ? O7 Mn2 O4 95.42(11) . . ? O1 Mn2 O2 91.85(9) . . ? O7 Mn2 O2 111.98(10) . . ? O4 Mn2 O2 78.84(11) . . ? O1 Mn2 N3 110.93(11) . . ? O7 Mn2 N3 86.63(12) . . ? O4 Mn2 N3 148.19(13) . . ? O2 Mn2 N3 71.07(11) . . ? O1 Mn2 N2 69.88(10) . . ? O7 Mn2 N2 87.64(10) . . ? O4 Mn2 N2 105.32(12) . . ? O2 Mn2 N2 159.71(10) . . ? N3 Mn2 N2 106.48(11) . . ? O1 Mn2 Mn1 42.37(7) . . ? O7 Mn2 Mn1 126.05(8) . . ? O4 Mn2 Mn1 37.51(9) . . ? O2 Mn2 Mn1 87.57(7) . . ? N3 Mn2 Mn1 146.44(8) . . ? N2 Mn2 Mn1 84.61(7) . . ? O1 Mn2 Mn3 87.48(7) . . ? O7 Mn2 Mn3 104.70(7) . . ? O4 Mn2 Mn3 39.61(9) . . ? O2 Mn2 Mn3 39.43(7) . . ? N3 Mn2 Mn3 109.20(9) . . ? N2 Mn2 Mn3 142.73(8) . . ? Mn1 Mn2 Mn3 59.522(17) . . ? O1 Mn2 Mn4 102.62(7) . . ? O7 Mn2 Mn4 67.33(8) . . ? O4 Mn2 Mn4 28.68(7) . . ? O2 Mn2 Mn4 94.88(7) . . ? N3 Mn2 Mn4 143.68(8) . . ? N2 Mn2 Mn4 97.63(8) . . ? Mn1 Mn2 Mn4 61.053(19) . . ? Mn3 Mn2 Mn4 57.830(16) . . ? O9A Mn3 O2 164.7(3) . . ? O9A Mn3 O4 101.1(3) . . ? O2 Mn3 O4 84.26(11) . . ? O9A Mn3 N5 71.4(3) . . ? O2 Mn3 N5 112.04(14) . . ? O4 Mn3 N5 145.46(15) . . ? O9A Mn3 O3 101.7(3) . . ? O2 Mn3 O3 93.40(10) . . ? O4 Mn3 O3 76.65(11) . . ? N5 Mn3 O3 72.30(12) . . ? O9A Mn3 O9B 30.5(3) . . ? O2 Mn3 O9B 143.96(13) . . ? O4 Mn3 O9B 74.32(13) . . ? N5 Mn3 O9B 101.74(15) . . ? O3 Mn3 O9B 108.93(12) . . ? O9A Mn3 N4 92.6(3) . . ? O2 Mn3 N4 72.18(10) . . ? O4 Mn3 N4 112.02(11) . . ? N5 Mn3 N4 102.11(14) . . ? O3 Mn3 N4 161.67(10) . . ? O9B Mn3 N4 89.21(12) . . ? O9A Mn3 Mn1 103.8(3) . . ? O2 Mn3 Mn1 88.98(7) . . ? O4 Mn3 Mn1 36.22(9) . . ? N5 Mn3 Mn1 111.18(11) . . ? O3 Mn3 Mn1 40.44(7) . . ? O9B Mn3 Mn1 90.32(10) . . ? N4 Mn3 Mn1 146.07(8) . . ? O9A Mn3 Mn2 139.5(3) . . ? O2 Mn3 Mn2 42.61(7) . . ? O4 Mn3 Mn2 41.87(8) . . ? N5 Mn3 Mn2 146.89(10) . . ? O3 Mn3 Mn2 86.57(7) . . ? O9B Mn3 Mn2 109.23(11) . . ? N4 Mn3 Mn2 89.94(8) . . ? Mn1 Mn3 Mn2 58.385(17) . . ? O9A Mn3 Mn4 71.6(3) . . ? O2 Mn3 Mn4 107.61(7) . . ? O4 Mn3 Mn4 35.39(8) . . ? N5 Mn3 Mn4 140.09(13) . . ? O3 Mn3 Mn4 101.44(7) . . ? O9B Mn3 Mn4 41.60(10) . . ? N4 Mn3 Mn4 93.87(8) . . ? Mn1 Mn3 Mn4 64.630(19) . . ? Mn2 Mn3 Mn4 67.922(18) . . ? O4 Mn4 O8 98.02(12) . . ? O4 Mn4 O11 169.10(16) . . ? O8 Mn4 O11 92.52(16) . . ? O4 Mn4 O6 85.80(13) . . ? O8 Mn4 O6 97.78(13) . . ? O11 Mn4 O6 90.05(16) . . ? O4 Mn4 O10A 105.3(3) . . ? O8 Mn4 O10A 88.8(3) . . ? O11 Mn4 O10A 77.5(3) . . ? O6 Mn4 O10A 166.2(3) . . ? O4 Mn4 O9B 74.77(14) . . ? O8 Mn4 O9B 104.72(14) . . ? O11 Mn4 O9B 105.26(17) . . ? O6 Mn4 O9B 151.95(13) . . ? O10A Mn4 O9B 32.9(3) . . ? O4 Mn4 Mn3 35.81(10) . . ? O8 Mn4 Mn3 93.16(10) . . ? O11 Mn4 Mn3 146.64(14) . . ? O6 Mn4 Mn3 121.60(9) . . ? O10A Mn4 Mn3 69.8(3) . . ? O9B Mn4 Mn3 41.66(11) . . ? O4 Mn4 Mn1 27.57(10) . . ? O8 Mn4 Mn1 122.52(9) . . ? O11 Mn4 Mn1 141.66(13) . . ? O6 Mn4 Mn1 71.68(8) . . ? O10A Mn4 Mn1 114.8(3) . . ? O9B Mn4 Mn1 82.08(10) . . ? Mn3 Mn4 Mn1 54.645(16) . . ? O4 Mn4 Mn2 30.50(8) . . ? O8 Mn4 Mn2 71.23(9) . . ? O11 Mn4 Mn2 156.35(14) . . ? O6 Mn4 Mn2 75.79(9) . . ? O10A Mn4 Mn2 117.9(3) . . ? O9B Mn4 Mn2 95.66(11) . . ? Mn3 Mn4 Mn2 54.248(16) . . ? Mn1 Mn4 Mn2 51.306(16) . . ? C6 O1 Mn2 124.8(2) . . ? C6 O1 Mn1 115.2(2) . . ? Mn2 O1 Mn1 95.26(10) . . ? C23 O2 Mn3 123.3(2) . . ? C23 O2 Mn2 117.4(2) . . ? Mn3 O2 Mn2 97.96(10) . . ? C40 O3 Mn1 123.8(3) . . ? C40 O3 Mn3 114.4(2) . . ? Mn1 O3 Mn3 95.01(10) . . ? Mn1 O4 Mn4 122.58(16) . . ? Mn1 O4 Mn3 103.84(12) . . ? Mn4 O4 Mn3 108.80(16) . . ? Mn1 O4 Mn2 98.68(14) . . ? Mn4 O4 Mn2 120.83(13) . . ? Mn3 O4 Mn2 98.52(13) . . ? C58 O5 Mn1 132.5(3) . . ? C58 O6 Mn4 124.6(3) . . ? C60 O7 Mn2 136.6(3) . . ? C60 O8 Mn4 130.1(3) . . ? O8 C60 O7 126.4(4) . . ? O8 C60 C61 117.9(4) . . ? O7 C60 C61 115.7(4) . . ? C62A O9A Mn3 130.9(14) . . ? C62A O10A Mn4 111.3(14) . . ? O9A C62A O10A 126(3) . . ? O9A C62A C63A 115(2) . . ? O10A C62A C63A 117(2) . . ? C62B O9B Mn4 138.8(7) . . ? C62B O9B Mn3 124.4(7) . . ? Mn4 O9B Mn3 96.74(16) . . ? O10B C62B O9B 123.3(12) . . ? O10B C62B C63B 120.7(9) . . ? O9B C62B C63B 116.0(10) . . ? C64 O11 Mn4 104.0(4) . . ? C1 N1 C5 119.2(3) . . ? C1 N1 Mn1 125.9(3) . . ? C5 N1 Mn1 114.8(2) . . ? C11 N2 C7 117.8(3) . . ? C11 N2 Mn2 125.1(3) . . ? C7 N2 Mn2 114.6(2) . . ? C18 N3 C22 118.6(3) . . ? C18 N3 Mn2 124.9(3) . . ? C22 N3 Mn2 116.3(2) . . ? C24 N4 C28 118.5(3) . . ? C24 N4 Mn3 114.1(2) . . ? C28 N4 Mn3 124.8(3) . . ? C35 N5 C39 119.1(4) . . ? C35 N5 Mn3 123.9(4) . . ? C39 N5 Mn3 117.0(3) . . ? C45 N6 C41 118.7(5) . . ? C45 N6 Mn1 125.7(4) . . ? C41 N6 Mn1 113.5(3) . . ? N1 C1 C2 123.4(4) . . ? C1 C2 C3 117.8(4) . . ? C2 C3 C4 119.9(4) . . ? C3 C4 C5 119.0(4) . . ? N1 C5 C4 120.6(4) . . ? N1 C5 C6 114.9(3) . . ? C4 C5 C6 124.4(4) . . ? O1 C6 C5 106.7(3) . . ? O1 C6 C7 107.9(3) . . ? C5 C6 C7 111.9(3) . . ? O1 C6 C12 111.7(3) . . ? C5 C6 C12 110.4(3) . . ? C7 C6 C12 108.2(3) . . ? N2 C7 C8 122.3(3) . . ? N2 C7 C6 112.5(3) . . ? C8 C7 C6 125.2(3) . . ? C7 C8 C9 118.9(4) . . ? C10 C9 C8 119.4(4) . . ? C9 C10 C11 118.4(4) . . ? N2 C11 C10 123.1(4) . . ? C13 C12 C17 117.8(4) . . ? C13 C12 C6 120.2(3) . . ? C17 C12 C6 121.9(3) . . ? C14 C13 C12 122.2(4) . . ? C15 C14 C13 119.3(4) . . ? C16 C15 C14 119.5(4) . . ? C15 C16 C17 122.2(4) . . ? C16 C17 C12 118.9(3) . . ? C16 C17 C54 118.4(3) . . ? C12 C17 C54 122.8(3) . . ? N3 C18 C19 123.3(4) . . ? C20 C19 C18 117.5(4) . . ? C21 C20 C19 120.1(4) . . ? C20 C21 C22 119.5(4) . . ? N3 C22 C21 120.9(4) . . ? N3 C22 C23 115.3(3) . . ? C21 C22 C23 123.7(3) . . ? O2 C23 C22 108.9(3) . . ? O2 C23 C24 106.3(3) . . ? C22 C23 C24 112.4(3) . . ? O2 C23 C29 111.9(3) . . ? C22 C23 C29 109.8(3) . . ? C24 C23 C29 107.6(3) . . ? N4 C24 C25 122.2(3) . . ? N4 C24 C23 113.2(3) . . ? C25 C24 C23 124.6(3) . . ? C24 C25 C26 118.8(4) . . ? C27 C26 C25 119.1(4) . . ? C28 C27 C26 118.6(4) . . ? N4 C28 C27 122.8(4) . . ? C30 C29 C34 117.8(4) . . ? C30 C29 C23 119.5(3) . . ? C34 C29 C23 122.6(3) . . ? C29 C30 C31 122.1(4) . . ? C32 C31 C30 119.4(4) . . ? C33 C32 C31 119.5(4) . . ? C32 C33 C34 121.7(4) . . ? C33 C34 C29 119.4(4) . . ? C33 C34 C56 116.5(3) . . ? C29 C34 C56 124.1(3) . . ? N5 C35 C36 122.8(6) . . ? C37 C36 C35 117.9(6) . . ? C38 C37 C36 119.9(5) . . ? C37 C38 C39 120.0(6) . . ? N5 C39 C38 120.2(5) . . ? N5 C39 C40 115.5(3) . . ? C38 C39 C40 124.2(5) . . ? O3 C40 C39 107.7(4) . . ? O3 C40 C41 107.4(4) . . ? C39 C40 C41 112.8(4) . . ? O3 C40 C46 111.7(3) . . ? C39 C40 C46 109.0(4) . . ? C41 C40 C46 108.3(4) . . ? N6 C41 C42 122.5(5) . . ? N6 C41 C40 113.2(4) . . ? C42 C41 C40 124.3(6) . . ? C41 C42 C43 115.3(7) . . ? C44 C43 C42 122.1(6) . . ? C45 C44 C43 116.2(7) . . ? N6 C45 C44 124.8(7) . . ? C47 C46 C51 118.1(4) . . ? C47 C46 C40 120.4(4) . . ? C51 C46 C40 121.5(4) . . ? C48 C47 C46 122.1(5) . . ? C49 C48 C47 119.5(5) . . ? C50 C49 C48 119.4(4) . . ? C49 C50 C51 122.1(4) . . ? C50 C51 C46 118.6(4) . . ? C50 C51 C52 117.3(3) . . ? C46 C51 C52 123.9(3) . . ? C57 C52 C53 118.9(4) . . ? C57 C52 C51 122.5(3) . . ? C53 C52 C51 118.4(3) . . ? C52 C53 C54 120.9(3) . . ? C55 C54 C53 118.9(3) . . ? C55 C54 C17 119.4(3) . . ? C53 C54 C17 121.7(3) . . ? C56 C55 C54 120.6(4) . . ? C55 C56 C57 119.5(3) . . ? C55 C56 C34 121.5(4) . . ? C57 C56 C34 119.0(3) . . ? C52 C57 C56 120.9(3) . . ? O6 C58 O5 126.5(4) . . ? O6 C58 C59 117.2(4) . . ? O5 C58 C59 116.3(4) . . ? O12 C64 O11 123.0(6) . . ? O12 C64 C65 120.8(7) . . ? O11 C64 C65 116.1(6) . . ? C1C N1C C2C 119.8(7) . . ? C1C N1C C3C 127.7(5) . . ? C2C N1C C3C 112.3(8) . . ? N1C C1C O1C 129.8(5) . . ? C2D O1D C3D 112.5(5) . . ? O1D C2D C1D 113.4(5) . . ? O1D C3D C4D 106.8(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.838 _refine_diff_density_min -1.698 _refine_diff_density_rms 0.107 _database_code_depnum_ccdc_archive 'CCDC 858642' ####################################################################### # # 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_jsk58 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '0.58(C64 H48 F3 Mn4 N6 O13 S, 0.42(C65 H51 Mn4 N6 O12), C F3 O3 S' _chemical_formula_sum 'C65.42 H49.25 F4.75 Mn4 N6 O15.58 S1.58' _chemical_formula_weight 1529.34 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' O O 0.0106 0.0060 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 12.3050(6) _cell_length_b 15.5248(7) _cell_length_c 37.6815(18) _cell_angle_alpha 90.00 _cell_angle_beta 98.567(3) _cell_angle_gamma 90.00 _cell_volume 7118.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9457 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 28.44 _exptl_crystal_description Block _exptl_crystal_colour 'Deep purple' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3106 _exptl_absorpt_coefficient_mu 0.819 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7912 _exptl_absorpt_correction_T_max 0.8534 _exptl_absorpt_process_details ? _exptl_special_details ; Crystals were mounted on a glass fiber using Paratone oil then placed on the diffractometer under a nitrogen stream at 100K. ; _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 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w scans; 12 settings' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 217916 _diffrn_reflns_av_R_equivalents 0.0681 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 27.50 _reflns_number_total 16330 _reflns_number_gt 13930 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.7-0' _computing_cell_refinement 'Bruker SAINT-Plus v7.68A' _computing_data_reduction 'Bruker SAINT-Plus v7.68A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF 2008' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The electron density map of the solvent area in this crystal contains a very clearly define triflate anion and another long ill-defined chain of density, presumably arising from disorder ether solvents. This latter are was solvent flattened using the program SQUEEZE. The total potential solvent are is 1203 cubic angstroms, about 17% of total unit cell volume, which required 315 electrons to adjust the observed intensities such that this area contained no electron density. This is reasonably consistent with two hexane molecules per asymmetric unit. The trifluoromethanesulfonate anion coordinating Mn4 has compositional disorder with an acetate anion, with populations at 58% and 42%, respectively. The acetate was modeled isotropically. The similar ADP and rigid-bond restraints were used on C64 and O8. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.250 0.715 0.250 600 157 ' ' 2 0.250 0.471 0.750 600 157 ' ' _platon_squeeze_details ; ; _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^)+(0.0563P)^2^+41.0900P] 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 16330 _refine_ls_number_parameters 902 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.0949 _refine_ls_R_factor_gt 0.0848 _refine_ls_wR_factor_ref 0.2089 _refine_ls_wR_factor_gt 0.2042 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.138 _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 0.36961(6) 0.17512(5) 0.58417(2) 0.02664(17) Uani 1 1 d . A 2 Mn2 Mn 0.46468(5) 0.35895(5) 0.572298(19) 0.02573(16) Uani 1 1 d . A 2 Mn3 Mn 0.58390(6) 0.23836(5) 0.63205(2) 0.02750(17) Uani 1 1 d . A 2 Mn4 Mn 0.61565(9) 0.18517(6) 0.54500(2) 0.0479(2) Uani 1 1 d . A 2 O1 O 0.3204(2) 0.3045(2) 0.58148(9) 0.0278(7) Uani 1 1 d . A 2 O2 O 0.5209(2) 0.3558(2) 0.63084(8) 0.0220(6) Uani 1 1 d . A 2 O3 O 0.4148(2) 0.18757(19) 0.63495(8) 0.0229(6) Uani 1 1 d . A 2 O4 O 0.5196(3) 0.2323(2) 0.58066(9) 0.0309(7) Uani 1 1 d . A 2 O5 O 0.3429(3) 0.1387(3) 0.53445(11) 0.0466(10) Uani 1 1 d . A 2 O6 O 0.4935(4) 0.1395(4) 0.50690(16) 0.0811(19) Uani 1 1 d . A 2 O7 O 0.5915(3) 0.3943(3) 0.54404(13) 0.0463(10) Uani 1 1 d U A 2 O8 O 0.7145(5) 0.2926(4) 0.5487(2) 0.098(2) Uani 1 1 d U A 2 S2 S 0.78727(12) 0.75353(10) 0.65355(4) 0.0425(3) Uani 1 1 d . B 2 C65 C 0.9320(5) 0.7783(5) 0.65443(19) 0.0498(15) Uani 1 1 d . B 2 F4 F 0.9474(3) 0.8580(3) 0.64480(16) 0.0876(16) Uani 1 1 d . B 2 F5 F 0.9780(4) 0.7258(4) 0.63292(14) 0.0943(18) Uani 1 1 d . B 2 F6 F 0.9888(3) 0.7689(3) 0.68708(11) 0.0588(10) Uani 1 1 d . B 2 O14 O 0.7526(3) 0.8136(3) 0.67843(11) 0.0492(11) Uani 1 1 d . B 2 O15 O 0.7419(4) 0.7690(4) 0.61692(12) 0.0638(14) Uani 1 1 d . B 2 O16 O 0.7875(4) 0.6660(3) 0.66589(15) 0.0683(15) Uani 1 1 d . B 2 S1 S 0.7870(2) 0.18822(18) 0.47730(7) 0.0416(7) Uani 0.582(5) 1 d PU C 1 C64 C 0.8794(10) 0.1014(8) 0.4685(3) 0.055(3) Uani 0.582(5) 1 d PU C 1 F1 F 0.8248(7) 0.0292(5) 0.4634(2) 0.069(2) Uani 0.582(5) 1 d P C 1 F2 F 0.9252(8) 0.1205(6) 0.4390(2) 0.087(3) Uani 0.582(5) 1 d P C 1 F3 F 0.9610(6) 0.0907(6) 0.4937(2) 0.082(3) Uani 0.582(5) 1 d P C 1 O11 O 0.7360(6) 0.1465(5) 0.50798(18) 0.094(4) Uani 0.582(5) 1 d P C 1 O12 O 0.7068(10) 0.1962(7) 0.4456(2) 0.088(4) Uani 0.582(5) 1 d PU C 1 O13 O 0.8597(7) 0.2598(5) 0.4861(2) 0.056(2) Uani 0.582(5) 1 d P C 1 N1 N 0.1886(4) 0.1747(3) 0.57863(14) 0.0398(11) Uani 1 1 d . . . N2 N 0.3476(3) 0.3563(3) 0.51837(11) 0.0338(9) Uani 1 1 d . . . N3 N 0.4697(3) 0.4910(3) 0.59181(11) 0.0329(9) Uani 1 1 d . . . N4 N 0.7313(3) 0.3309(3) 0.63800(12) 0.0332(9) Uani 1 1 d . . . N5 N 0.5809(3) 0.1958(3) 0.68563(11) 0.0315(9) Uani 1 1 d . . . N6 N 0.4158(3) 0.0429(3) 0.60265(13) 0.0351(10) Uani 1 1 d . . . C1 C 0.1259(6) 0.1085(4) 0.5860(2) 0.0566(18) Uani 1 1 d . A . H1 H 0.1606 0.0573 0.5957 0.068 Uiso 1 1 calc R . . C2 C 0.0124(6) 0.1119(5) 0.5799(2) 0.070(2) Uani 1 1 d . . . H2 H -0.0304 0.0646 0.5858 0.083 Uiso 1 1 calc R A . C3 C -0.0367(5) 0.1853(6) 0.5652(2) 0.066(2) Uani 1 1 d . A . H3 H -0.1145 0.1890 0.5602 0.079 Uiso 1 1 calc R . . C4 C 0.0287(4) 0.2552(5) 0.55753(17) 0.0476(15) Uani 1 1 d . . . H4 H -0.0044 0.3069 0.5476 0.057 Uiso 1 1 calc R A . C5 C 0.1412(4) 0.2478(4) 0.56459(15) 0.0358(12) Uani 1 1 d . A . C6 C 0.2208(3) 0.3219(3) 0.55950(13) 0.0289(10) Uani 1 1 d . . . C7 C 0.2469(4) 0.3253(4) 0.52073(13) 0.0342(11) Uani 1 1 d . A . C8 C 0.1760(5) 0.3000(4) 0.49024(15) 0.0436(14) Uani 1 1 d . . . H8 H 0.1047 0.2788 0.4923 0.052 Uiso 1 1 calc R A . C9 C 0.2099(5) 0.3057(5) 0.45721(16) 0.0501(16) Uani 1 1 d . A . H9 H 0.1624 0.2885 0.4362 0.060 Uiso 1 1 calc R . . C10 C 0.3138(5) 0.3368(5) 0.45487(16) 0.0522(16) Uani 1 1 d . . . H10 H 0.3395 0.3407 0.4324 0.063 Uiso 1 1 calc R A . C11 C 0.3791(5) 0.3618(4) 0.48592(14) 0.0434(14) Uani 1 1 d . A . H11 H 0.4501 0.3840 0.4843 0.052 Uiso 1 1 calc R . . C12 C 0.1731(3) 0.4104(3) 0.56905(13) 0.0275(10) Uani 1 1 d . A . C13 C 0.1833(3) 0.4404(3) 0.60476(12) 0.0232(9) Uani 1 1 d . . . C14 C 0.1454(4) 0.5235(3) 0.61087(13) 0.0291(10) Uani 1 1 d . A . H14 H 0.1525 0.5444 0.6348 0.035 Uiso 1 1 calc R . . C15 C 0.0982(4) 0.5759(3) 0.58324(15) 0.0343(11) Uani 1 1 d . . . H15 H 0.0757 0.6327 0.5880 0.041 Uiso 1 1 calc R A . C16 C 0.0840(4) 0.5445(4) 0.54836(15) 0.0381(12) Uani 1 1 d . A . H16 H 0.0490 0.5789 0.5291 0.046 Uiso 1 1 calc R . . C17 C 0.1214(4) 0.4629(4) 0.54181(13) 0.0356(12) Uani 1 1 d . . . H17 H 0.1113 0.4420 0.5178 0.043 Uiso 1 1 calc R A . C18 C 0.4191(6) 0.5569(4) 0.57347(18) 0.0533(17) Uani 1 1 d . A . H18 H 0.3774 0.5458 0.5506 0.064 Uiso 1 1 calc R . . C19 C 0.4249(7) 0.6406(5) 0.5863(3) 0.069(2) Uani 1 1 d . . . H19 H 0.3864 0.6858 0.5728 0.083 Uiso 1 1 calc R A . C20 C 0.4868(6) 0.6564(4) 0.6183(3) 0.063(2) Uani 1 1 d . A . H20 H 0.4935 0.7134 0.6275 0.076 Uiso 1 1 calc R . . C21 C 0.5401(5) 0.5896(4) 0.63758(19) 0.0455(15) Uani 1 1 d . . . H21 H 0.5840 0.6001 0.6601 0.055 Uiso 1 1 calc R A . C22 C 0.5291(3) 0.5067(3) 0.62380(14) 0.0272(10) Uani 1 1 d . A . C23 C 0.5810(3) 0.4278(3) 0.64428(12) 0.0244(9) Uani 1 1 d . . . C24 C 0.7002(4) 0.4145(3) 0.63645(13) 0.0287(10) Uani 1 1 d . A . C25 C 0.7703(4) 0.4798(4) 0.62955(16) 0.0395(13) Uani 1 1 d . . . H25 H 0.7454 0.5378 0.6279 0.047 Uiso 1 1 calc R A . C26 C 0.8772(4) 0.4602(5) 0.62511(19) 0.0536(17) Uani 1 1 d . A . H26 H 0.9272 0.5042 0.6208 0.064 Uiso 1 1 calc R . . C27 C 0.9093(4) 0.3741(5) 0.62721(19) 0.0555(18) Uani 1 1 d . . . H27 H 0.9821 0.3581 0.6244 0.067 Uiso 1 1 calc R A . C28 C 0.8351(4) 0.3136(4) 0.63338(17) 0.0460(14) Uani 1 1 d . A . H28 H 0.8580 0.2551 0.6345 0.055 Uiso 1 1 calc R . . C29 C 0.5857(4) 0.4382(3) 0.68558(13) 0.0265(9) Uani 1 1 d . A . C30 C 0.6810(4) 0.4689(4) 0.70665(15) 0.0417(13) Uani 1 1 d . . . H30 H 0.7402 0.4883 0.6952 0.050 Uiso 1 1 calc R A . C31 C 0.6914(5) 0.4721(4) 0.74350(16) 0.0473(15) Uani 1 1 d . A . H31 H 0.7578 0.4925 0.7570 0.057 Uiso 1 1 calc R . . C32 C 0.6073(4) 0.4463(3) 0.76084(14) 0.0361(12) Uani 1 1 d . . . H32 H 0.6149 0.4476 0.7863 0.043 Uiso 1 1 calc R A . C33 C 0.5106(4) 0.4181(3) 0.74067(13) 0.0305(10) Uani 1 1 d . A . H33 H 0.4515 0.4006 0.7526 0.037 Uiso 1 1 calc R . . C34 C 0.4973(4) 0.4146(3) 0.70328(12) 0.0236(9) Uani 1 1 d . . . C35 C 0.6542(4) 0.2197(4) 0.71354(15) 0.0394(12) Uani 1 1 d . A . H35 H 0.7094 0.2596 0.7094 0.047 Uiso 1 1 calc R . . C36 C 0.6552(4) 0.1906(4) 0.74760(16) 0.0438(14) Uani 1 1 d . . . H36 H 0.7068 0.2120 0.7669 0.053 Uiso 1 1 calc R A . C37 C 0.5783(5) 0.1283(4) 0.75335(15) 0.0415(13) Uani 1 1 d . A . H37 H 0.5783 0.1043 0.7765 0.050 Uiso 1 1 calc R . . C38 C 0.5019(4) 0.1020(3) 0.72486(15) 0.0345(11) Uani 1 1 d . . . H38 H 0.4486 0.0597 0.7283 0.041 Uiso 1 1 calc R A . C39 C 0.5034(4) 0.1376(3) 0.69131(13) 0.0271(9) Uani 1 1 d . A . C40 C 0.4178(4) 0.1172(3) 0.65860(12) 0.0239(9) Uani 1 1 d . . . C41 C 0.4510(4) 0.0384(3) 0.63794(14) 0.0283(10) Uani 1 1 d . A . C42 C 0.5098(4) -0.0316(3) 0.65335(17) 0.0386(12) Uani 1 1 d . . . H42 H 0.5341 -0.0338 0.6785 0.046 Uiso 1 1 calc R A . C43 C 0.5323(5) -0.0987(4) 0.6311(2) 0.0490(16) Uani 1 1 d . A . H43 H 0.5742 -0.1469 0.6408 0.059 Uiso 1 1 calc R . . C44 C 0.4936(5) -0.0948(4) 0.5951(2) 0.0525(17) Uani 1 1 d . . . H44 H 0.5067 -0.1408 0.5797 0.063 Uiso 1 1 calc R A . C45 C 0.4361(5) -0.0239(4) 0.58178(18) 0.0479(15) Uani 1 1 d . A . H45 H 0.4093 -0.0216 0.5568 0.057 Uiso 1 1 calc R . . C46 C 0.3026(4) 0.1024(3) 0.67020(13) 0.0259(9) Uani 1 1 d . A . C47 C 0.2640(4) 0.0170(3) 0.67362(15) 0.0333(11) Uani 1 1 d . . . H47 H 0.3098 -0.0301 0.6696 0.040 Uiso 1 1 calc R A . C48 C 0.1616(4) 0.0014(4) 0.68269(16) 0.0399(13) Uani 1 1 d . A . H48 H 0.1374 -0.0562 0.6849 0.048 Uiso 1 1 calc R . . C49 C 0.0941(4) 0.0689(4) 0.68856(16) 0.0410(13) Uani 1 1 d . . . H49 H 0.0232 0.0583 0.6947 0.049 Uiso 1 1 calc R A . C50 C 0.1308(4) 0.1533(4) 0.68541(15) 0.0367(12) Uani 1 1 d . A . H50 H 0.0838 0.1998 0.6893 0.044 Uiso 1 1 calc R . . C51 C 0.2337(4) 0.1709(3) 0.67673(13) 0.0260(9) Uani 1 1 d . . . C52 C 0.2649(3) 0.2629(3) 0.67253(12) 0.0229(9) Uani 1 1 d . A . C53 C 0.2045(3) 0.3092(3) 0.64491(12) 0.0233(9) Uani 1 1 d . . . H53 H 0.1399 0.2847 0.6318 0.028 Uiso 1 1 calc R A . C54 C 0.2378(3) 0.3919(3) 0.63614(11) 0.0214(8) Uani 1 1 d . A . C55 C 0.3292(3) 0.4282(3) 0.65681(11) 0.0203(8) Uani 1 1 d . . . H55 H 0.3499 0.4856 0.6522 0.024 Uiso 1 1 calc R A . C56 C 0.3908(3) 0.3814(3) 0.68429(11) 0.0211(8) Uani 1 1 d . A . C57 C 0.3555(4) 0.3002(3) 0.69304(12) 0.0242(9) Uani 1 1 d . . . H57 H 0.3935 0.2701 0.7131 0.029 Uiso 1 1 calc R A . C58 C 0.3934(5) 0.1247(4) 0.5080(2) 0.0532(17) Uani 1 1 d . . . C59 C 0.3239(7) 0.0912(6) 0.4744(2) 0.081(3) Uani 1 1 d . A . H59A H 0.3288 0.1308 0.4545 0.121 Uiso 1 1 calc R . . H59B H 0.2472 0.0868 0.4785 0.121 Uiso 1 1 calc R . . H59C H 0.3505 0.0342 0.4686 0.121 Uiso 1 1 calc R . . C60 C 0.6851(5) 0.3676(4) 0.54157(19) 0.0483(14) Uani 1 1 d U . . C61 C 0.7670(5) 0.4282(5) 0.53058(18) 0.0524(16) Uani 1 1 d U A . H61A H 0.7412 0.4875 0.5326 0.079 Uiso 1 1 calc R . . H61B H 0.7764 0.4166 0.5057 0.079 Uiso 1 1 calc R . . H61C H 0.8374 0.4206 0.5462 0.079 Uiso 1 1 calc R . . O9 O 0.6845(5) 0.1376(3) 0.63103(13) 0.0706(17) Uani 1 1 d . . . O10 O 0.6997(4) 0.0928(3) 0.57725(13) 0.0614(13) Uani 1 1 d . . . C62 C 0.7181(4) 0.0855(3) 0.60995(16) 0.0341(11) Uani 1 1 d . A . C63 C 0.7858(4) 0.0106(4) 0.62612(19) 0.0460(15) Uani 1 1 d . . . H63A H 0.7905 -0.0330 0.6076 0.069 Uiso 1 1 calc R A . H63B H 0.7512 -0.0145 0.6455 0.069 Uiso 1 1 calc R . . H63C H 0.8599 0.0306 0.6358 0.069 Uiso 1 1 calc R . . O11B O 0.7360(6) 0.1465(5) 0.50798(18) 0.100 Uiso 0.418(5) 1 d PD C 3 O12B O 0.6310(14) 0.2430(11) 0.4818(5) 0.100 Uiso 0.418(5) 1 d PD C 3 C64B C 0.7078(15) 0.1897(11) 0.4825(6) 0.100 Uiso 0.418(5) 1 d PD C 3 C65B C 0.770(2) 0.1767(19) 0.4515(8) 0.100 Uiso 0.418(5) 1 d PD C 3 H65D H 0.8261 0.1326 0.4577 0.150 Uiso 0.418(5) 1 calc PR C 3 H65E H 0.8044 0.2310 0.4462 0.150 Uiso 0.418(5) 1 calc PR C 3 H65F H 0.7185 0.1581 0.4305 0.150 Uiso 0.418(5) 1 calc PR C 3 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 0.0216(3) 0.0280(4) 0.0311(4) -0.0098(3) 0.0063(3) -0.0026(3) Mn2 0.0153(3) 0.0329(4) 0.0290(4) -0.0058(3) 0.0032(3) -0.0019(3) Mn3 0.0348(4) 0.0200(3) 0.0285(4) -0.0028(3) 0.0070(3) 0.0011(3) Mn4 0.0640(6) 0.0462(5) 0.0362(5) 0.0004(4) 0.0164(4) 0.0171(5) O1 0.0140(14) 0.0415(19) 0.0283(16) 0.0000(14) 0.0040(12) -0.0001(13) O2 0.0160(13) 0.0226(15) 0.0266(15) -0.0069(12) 0.0004(11) -0.0016(12) O3 0.0235(15) 0.0194(15) 0.0263(15) -0.0002(12) 0.0053(12) -0.0025(12) O4 0.0283(17) 0.0295(17) 0.0368(19) -0.0036(15) 0.0117(14) -0.0006(14) O5 0.048(2) 0.053(3) 0.037(2) -0.0105(19) -0.0005(18) -0.007(2) O6 0.042(3) 0.119(5) 0.083(4) -0.037(4) 0.009(3) 0.019(3) O7 0.0176(16) 0.042(2) 0.080(3) 0.002(2) 0.0088(18) 0.0041(15) O8 0.063(3) 0.066(3) 0.179(6) 0.027(4) 0.066(4) 0.034(3) S2 0.0345(7) 0.0453(8) 0.0440(8) -0.0157(6) -0.0065(6) -0.0043(6) C65 0.034(3) 0.055(4) 0.060(4) -0.005(3) 0.007(3) 0.010(3) F4 0.042(2) 0.078(3) 0.141(5) 0.038(3) 0.007(3) -0.005(2) F5 0.057(3) 0.143(5) 0.085(3) -0.039(3) 0.018(2) 0.034(3) F6 0.0313(17) 0.068(3) 0.072(3) -0.008(2) -0.0112(17) -0.0027(17) O14 0.038(2) 0.068(3) 0.041(2) -0.018(2) 0.0033(17) 0.002(2) O15 0.050(3) 0.096(4) 0.042(2) -0.025(3) -0.005(2) 0.015(3) O16 0.059(3) 0.051(3) 0.086(4) -0.016(3) -0.020(3) -0.017(2) S1 0.0423(14) 0.0496(15) 0.0333(13) -0.0015(10) 0.0066(10) 0.0166(11) C64 0.053(6) 0.062(7) 0.046(6) -0.027(5) 0.000(5) 0.023(5) F1 0.082(5) 0.052(4) 0.076(5) -0.020(4) 0.016(4) 0.013(4) F2 0.120(7) 0.092(6) 0.062(5) -0.009(4) 0.057(5) 0.007(5) F3 0.053(4) 0.100(6) 0.085(6) -0.019(5) -0.014(4) 0.035(4) O11 0.111(9) 0.115(9) 0.065(6) 0.018(6) 0.046(6) 0.053(7) O12 0.106(8) 0.090(7) 0.053(5) -0.003(5) -0.032(5) 0.047(6) O13 0.077(6) 0.045(4) 0.051(5) -0.005(4) 0.023(4) -0.004(4) N1 0.031(2) 0.037(2) 0.055(3) -0.014(2) 0.016(2) -0.0066(19) N2 0.0238(19) 0.050(3) 0.028(2) -0.0078(19) 0.0053(16) 0.0009(18) N3 0.029(2) 0.039(2) 0.034(2) 0.0065(18) 0.0141(17) 0.0083(18) N4 0.0193(19) 0.043(2) 0.036(2) -0.0059(19) 0.0009(16) 0.0082(17) N5 0.0243(19) 0.039(2) 0.032(2) -0.0068(18) 0.0044(16) -0.0099(17) N6 0.030(2) 0.029(2) 0.046(3) -0.0133(19) 0.0045(18) 0.0012(17) C1 0.055(4) 0.039(3) 0.082(5) -0.024(3) 0.032(4) -0.017(3) C2 0.059(4) 0.057(4) 0.103(6) -0.033(4) 0.046(4) -0.024(4) C3 0.033(3) 0.090(6) 0.079(5) -0.041(5) 0.027(3) -0.026(4) C4 0.019(2) 0.064(4) 0.060(4) -0.026(3) 0.008(2) -0.006(2) C5 0.026(2) 0.042(3) 0.042(3) -0.015(2) 0.013(2) -0.006(2) C6 0.0139(19) 0.045(3) 0.027(2) -0.005(2) 0.0006(16) 0.0013(19) C7 0.021(2) 0.052(3) 0.029(2) -0.008(2) 0.0037(18) 0.004(2) C8 0.029(3) 0.063(4) 0.036(3) -0.014(3) -0.005(2) 0.005(3) C9 0.033(3) 0.080(5) 0.034(3) -0.017(3) -0.008(2) 0.008(3) C10 0.051(4) 0.078(5) 0.028(3) -0.011(3) 0.007(2) 0.012(3) C11 0.036(3) 0.066(4) 0.029(3) -0.003(3) 0.010(2) 0.000(3) C12 0.0118(18) 0.041(3) 0.029(2) -0.001(2) -0.0007(16) -0.0035(18) C13 0.0144(18) 0.027(2) 0.028(2) -0.0003(18) 0.0017(16) -0.0024(16) C14 0.023(2) 0.031(2) 0.032(2) -0.002(2) 0.0004(18) -0.0002(19) C15 0.024(2) 0.032(3) 0.045(3) 0.004(2) 0.000(2) 0.004(2) C16 0.027(2) 0.049(3) 0.036(3) 0.009(2) -0.002(2) 0.006(2) C17 0.025(2) 0.056(3) 0.025(2) 0.001(2) -0.0017(18) 0.003(2) C18 0.057(4) 0.059(4) 0.049(4) 0.026(3) 0.024(3) 0.025(3) C19 0.077(5) 0.047(4) 0.094(6) 0.032(4) 0.049(5) 0.031(4) C20 0.069(5) 0.023(3) 0.111(7) 0.004(3) 0.053(5) 0.006(3) C21 0.035(3) 0.031(3) 0.075(4) -0.010(3) 0.023(3) -0.007(2) C22 0.0144(19) 0.026(2) 0.044(3) -0.001(2) 0.0131(18) -0.0003(17) C23 0.0158(19) 0.026(2) 0.031(2) -0.0102(18) 0.0035(17) -0.0008(16) C24 0.019(2) 0.035(3) 0.033(2) -0.012(2) 0.0062(18) -0.0015(18) C25 0.019(2) 0.048(3) 0.053(3) -0.017(3) 0.011(2) -0.009(2) C26 0.020(2) 0.078(5) 0.065(4) -0.018(4) 0.012(3) -0.015(3) C27 0.017(2) 0.087(5) 0.064(4) -0.012(4) 0.014(2) 0.008(3) C28 0.024(3) 0.061(4) 0.054(3) -0.003(3) 0.009(2) 0.017(3) C29 0.018(2) 0.025(2) 0.036(2) -0.0099(19) 0.0008(18) 0.0025(17) C30 0.025(2) 0.057(4) 0.042(3) -0.020(3) 0.002(2) -0.010(2) C31 0.030(3) 0.061(4) 0.047(3) -0.025(3) -0.008(2) -0.006(3) C32 0.035(3) 0.036(3) 0.032(3) -0.008(2) -0.010(2) 0.008(2) C33 0.032(2) 0.031(2) 0.027(2) -0.0036(19) -0.0021(19) 0.003(2) C34 0.022(2) 0.021(2) 0.026(2) -0.0045(17) -0.0009(17) 0.0019(17) C35 0.031(3) 0.047(3) 0.041(3) -0.007(2) 0.007(2) -0.014(2) C36 0.029(3) 0.060(4) 0.039(3) -0.007(3) -0.005(2) -0.004(3) C37 0.038(3) 0.049(3) 0.036(3) 0.011(2) 0.001(2) 0.007(2) C38 0.029(2) 0.032(3) 0.041(3) 0.006(2) 0.000(2) -0.002(2) C39 0.020(2) 0.026(2) 0.036(3) -0.0019(19) 0.0030(18) 0.0013(17) C40 0.022(2) 0.021(2) 0.029(2) -0.0004(17) 0.0051(17) -0.0022(16) C41 0.019(2) 0.023(2) 0.044(3) -0.002(2) 0.0080(19) -0.0054(17) C42 0.033(3) 0.022(2) 0.061(4) -0.001(2) 0.007(2) -0.005(2) C43 0.030(3) 0.023(3) 0.097(5) 0.000(3) 0.017(3) 0.001(2) C44 0.046(3) 0.033(3) 0.083(5) -0.019(3) 0.023(3) 0.001(3) C45 0.045(3) 0.042(3) 0.058(4) -0.021(3) 0.009(3) 0.008(3) C46 0.025(2) 0.024(2) 0.029(2) 0.0008(18) 0.0031(18) -0.0021(17) C47 0.029(2) 0.025(2) 0.045(3) 0.003(2) 0.004(2) -0.0023(19) C48 0.034(3) 0.035(3) 0.051(3) 0.005(2) 0.006(2) -0.018(2) C49 0.025(2) 0.046(3) 0.055(3) 0.003(3) 0.016(2) -0.012(2) C50 0.028(2) 0.036(3) 0.049(3) 0.005(2) 0.014(2) 0.000(2) C51 0.021(2) 0.027(2) 0.029(2) 0.0005(18) 0.0026(17) -0.0046(18) C52 0.0175(19) 0.023(2) 0.030(2) -0.0014(17) 0.0092(17) 0.0014(16) C53 0.0141(18) 0.024(2) 0.032(2) -0.0050(18) 0.0062(16) -0.0013(16) C54 0.0137(18) 0.028(2) 0.023(2) -0.0017(17) 0.0049(15) 0.0032(16) C55 0.0164(18) 0.022(2) 0.024(2) -0.0011(16) 0.0083(15) 0.0009(15) C56 0.0157(18) 0.025(2) 0.023(2) -0.0025(17) 0.0037(15) -0.0008(16) C57 0.022(2) 0.025(2) 0.026(2) -0.0001(17) 0.0051(17) 0.0023(17) C58 0.043(3) 0.048(4) 0.066(4) -0.021(3) -0.001(3) 0.011(3) C59 0.081(6) 0.095(7) 0.065(5) -0.046(5) 0.006(4) -0.002(5) C60 0.033(3) 0.048(3) 0.069(4) 0.006(3) 0.021(3) 0.011(2) C61 0.031(3) 0.070(4) 0.059(4) 0.024(3) 0.019(3) 0.015(3) O9 0.114(4) 0.033(2) 0.053(3) -0.014(2) -0.026(3) 0.030(3) O10 0.072(3) 0.061(3) 0.054(3) 0.001(2) 0.019(2) 0.039(3) C62 0.025(2) 0.029(3) 0.049(3) 0.000(2) 0.007(2) 0.0002(19) C63 0.026(3) 0.031(3) 0.078(4) 0.001(3) -0.003(3) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O3 1.921(3) . ? Mn1 O5 1.937(4) . ? Mn1 O4 2.070(3) . ? Mn1 O1 2.096(4) . ? Mn1 N1 2.206(4) . ? Mn1 N6 2.214(5) . ? Mn1 Mn3 3.1232(10) . ? Mn1 Mn2 3.1415(11) . ? Mn1 Mn4 3.5638(12) . ? Mn2 O1 2.042(3) . ? Mn2 O4 2.087(4) . ? Mn2 O7 2.089(4) . ? Mn2 N3 2.176(5) . ? Mn2 O2 2.212(3) . ? Mn2 N2 2.310(4) . ? Mn2 Mn3 3.1212(11) . ? Mn2 Mn4 3.5152(12) . ? Mn3 O2 1.979(3) . ? Mn3 O4 1.982(4) . ? Mn3 O9 1.999(5) . ? Mn3 N5 2.130(4) . ? Mn3 O3 2.243(3) . ? Mn3 N4 2.298(5) . ? Mn3 Mn4 3.4605(11) . ? Mn4 O6 2.045(6) . ? Mn4 O4 2.052(3) . ? Mn4 O10 2.057(5) . ? Mn4 O8 2.057(7) . ? O1 C6 1.399(5) . ? O2 C23 1.393(5) . ? O3 C40 1.407(5) . ? O5 C58 1.271(8) . ? O6 C58 1.259(8) . ? O7 C60 1.240(6) . ? O8 C60 1.237(8) . ? S2 O15 1.430(5) . ? S2 O14 1.431(4) . ? S2 O16 1.437(5) . ? S2 C65 1.818(6) . ? C65 F4 1.311(8) . ? C65 F6 1.329(8) . ? C65 F5 1.333(7) . ? S1 O13 1.433(9) . ? S1 O12 1.436(9) . ? S1 O11 1.539(7) . ? S1 C64 1.825(10) . ? C64 F3 1.287(13) . ? C64 F1 1.307(15) . ? C64 F2 1.351(14) . ? N1 C1 1.338(8) . ? N1 C5 1.348(8) . ? N2 C11 1.340(7) . ? N2 C7 1.344(6) . ? N3 C18 1.335(7) . ? N3 C22 1.336(7) . ? N4 C28 1.342(6) . ? N4 C24 1.353(7) . ? N5 C35 1.332(7) . ? N5 C39 1.354(6) . ? N6 C41 1.338(7) . ? N6 C45 1.347(7) . ? C1 C2 1.382(10) . ? C2 C3 1.367(12) . ? C3 C4 1.407(10) . ? C4 C5 1.375(7) . ? C5 C6 1.540(7) . ? C6 C7 1.543(7) . ? C6 C12 1.559(7) . ? C7 C8 1.391(7) . ? C8 C9 1.373(8) . ? C9 C10 1.381(9) . ? C10 C11 1.373(8) . ? C12 C17 1.388(7) . ? C12 C13 1.412(6) . ? C13 C14 1.403(7) . ? C13 C54 1.476(6) . ? C14 C15 1.379(7) . ? C15 C16 1.388(8) . ? C16 C17 1.382(8) . ? C18 C19 1.385(11) . ? C19 C20 1.351(12) . ? C20 C21 1.375(10) . ? C21 C22 1.387(7) . ? C22 C23 1.536(7) . ? C23 C24 1.553(6) . ? C23 C29 1.557(7) . ? C24 C25 1.380(7) . ? C25 C26 1.384(7) . ? C26 C27 1.393(10) . ? C27 C28 1.354(9) . ? C29 C30 1.398(6) . ? C29 C34 1.406(7) . ? C30 C31 1.376(8) . ? C31 C32 1.364(9) . ? C32 C33 1.384(7) . ? C33 C34 1.395(6) . ? C34 C56 1.488(6) . ? C35 C36 1.359(8) . ? C36 C37 1.393(8) . ? C37 C38 1.379(8) . ? C38 C39 1.382(7) . ? C39 C40 1.530(6) . ? C40 C41 1.537(6) . ? C40 C46 1.561(6) . ? C41 C42 1.385(7) . ? C42 C43 1.390(8) . ? C43 C44 1.370(10) . ? C44 C45 1.363(9) . ? C46 C51 1.405(7) . ? C46 C47 1.420(7) . ? C47 C48 1.376(7) . ? C48 C49 1.376(8) . ? C49 C50 1.397(8) . ? C50 C51 1.381(6) . ? C51 C52 1.493(6) . ? C52 C57 1.385(6) . ? C52 C53 1.387(6) . ? C53 C54 1.403(6) . ? C54 C55 1.388(6) . ? C55 C56 1.393(6) . ? C56 C57 1.390(6) . ? C58 C59 1.509(9) . ? C60 C61 1.482(9) . ? O9 C62 1.246(7) . ? O10 C62 1.224(7) . ? C62 C63 1.506(7) . ? O12B C64B 1.253(17) . ? C64B C65B 1.497(18) . ? 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 O5 167.07(17) . . ? O3 Mn1 O4 83.78(14) . . ? O5 Mn1 O4 95.04(16) . . ? O3 Mn1 O1 89.46(13) . . ? O5 Mn1 O1 103.10(17) . . ? O4 Mn1 O1 80.78(13) . . ? O3 Mn1 N1 103.49(16) . . ? O5 Mn1 N1 83.34(18) . . ? O4 Mn1 N1 153.20(17) . . ? O1 Mn1 N1 73.62(15) . . ? O3 Mn1 N6 75.96(15) . . ? O5 Mn1 N6 91.85(18) . . ? O4 Mn1 N6 103.21(15) . . ? O1 Mn1 N6 164.21(15) . . ? N1 Mn1 N6 103.58(18) . . ? O3 Mn1 Mn3 45.47(9) . . ? O5 Mn1 Mn3 131.10(13) . . ? O4 Mn1 Mn3 38.56(10) . . ? O1 Mn1 Mn3 86.55(9) . . ? N1 Mn1 Mn3 144.04(12) . . ? N6 Mn1 Mn3 87.41(11) . . ? O3 Mn1 Mn2 89.52(9) . . ? O5 Mn1 Mn2 98.08(14) . . ? O4 Mn1 Mn2 41.12(10) . . ? O1 Mn1 Mn2 39.98(8) . . ? N1 Mn1 Mn2 112.44(13) . . ? N6 Mn1 Mn2 143.45(12) . . ? Mn3 Mn1 Mn2 59.76(2) . . ? O3 Mn1 Mn4 105.67(9) . . ? O5 Mn1 Mn4 69.18(13) . . ? O4 Mn1 Mn4 30.03(10) . . ? O1 Mn1 Mn4 101.26(9) . . ? N1 Mn1 Mn4 150.35(14) . . ? N6 Mn1 Mn4 88.67(12) . . ? Mn3 Mn1 Mn4 61.91(2) . . ? Mn2 Mn1 Mn4 62.86(2) . . ? O1 Mn2 O4 81.65(14) . . ? O1 Mn2 O7 158.34(16) . . ? O4 Mn2 O7 94.27(14) . . ? O1 Mn2 N3 108.32(15) . . ? O4 Mn2 N3 147.58(15) . . ? O7 Mn2 N3 86.52(16) . . ? O1 Mn2 O2 88.43(12) . . ? O4 Mn2 O2 77.43(13) . . ? O7 Mn2 O2 111.56(15) . . ? N3 Mn2 O2 72.25(14) . . ? O1 Mn2 N2 72.39(14) . . ? O4 Mn2 N2 105.17(16) . . ? O7 Mn2 N2 88.39(16) . . ? N3 Mn2 N2 107.25(17) . . ? O2 Mn2 N2 159.80(13) . . ? O1 Mn2 Mn3 87.51(10) . . ? O4 Mn2 Mn3 38.68(10) . . ? O7 Mn2 Mn3 102.62(12) . . ? N3 Mn2 Mn3 109.57(12) . . ? O2 Mn2 Mn3 39.07(8) . . ? N2 Mn2 Mn3 142.05(13) . . ? O1 Mn2 Mn1 41.26(10) . . ? O4 Mn2 Mn1 40.71(9) . . ? O7 Mn2 Mn1 129.29(12) . . ? N3 Mn2 Mn1 143.16(11) . . ? O2 Mn2 Mn1 84.58(8) . . ? N2 Mn2 Mn1 84.97(12) . . ? Mn3 Mn2 Mn1 59.83(2) . . ? O1 Mn2 Mn4 104.05(10) . . ? O4 Mn2 Mn4 31.58(9) . . ? O7 Mn2 Mn4 65.47(11) . . ? N3 Mn2 Mn4 146.35(11) . . ? O2 Mn2 Mn4 100.03(8) . . ? N2 Mn2 Mn4 90.95(11) . . ? Mn3 Mn2 Mn4 62.53(2) . . ? Mn1 Mn2 Mn4 64.45(3) . . ? O2 Mn3 O4 85.58(13) . . ? O2 Mn3 O9 164.2(2) . . ? O4 Mn3 O9 95.90(16) . . ? O2 Mn3 N5 104.21(15) . . ? O4 Mn3 N5 148.30(15) . . ? O9 Mn3 N5 82.7(2) . . ? O2 Mn3 O3 87.83(12) . . ? O4 Mn3 O3 78.05(13) . . ? O9 Mn3 O3 107.9(2) . . ? N5 Mn3 O3 72.39(13) . . ? O2 Mn3 N4 74.16(14) . . ? O4 Mn3 N4 108.61(15) . . ? O9 Mn3 N4 90.5(2) . . ? N5 Mn3 N4 103.07(16) . . ? O3 Mn3 N4 159.94(13) . . ? O2 Mn3 Mn2 44.80(9) . . ? O4 Mn3 Mn2 41.16(10) . . ? O9 Mn3 Mn2 132.96(15) . . ? N5 Mn3 Mn2 142.86(12) . . ? O3 Mn3 Mn2 84.63(8) . . ? N4 Mn3 Mn2 88.56(11) . . ? O2 Mn3 Mn1 88.99(9) . . ? O4 Mn3 Mn1 40.62(10) . . ? O9 Mn3 Mn1 102.41(15) . . ? N5 Mn3 Mn1 108.53(11) . . ? O3 Mn3 Mn1 37.64(8) . . ? N4 Mn3 Mn1 147.03(12) . . ? Mn2 Mn3 Mn1 60.41(2) . . ? O2 Mn3 Mn4 107.29(9) . . ? O4 Mn3 Mn4 31.54(10) . . ? O9 Mn3 Mn4 68.74(14) . . ? N5 Mn3 Mn4 147.66(12) . . ? O3 Mn3 Mn4 101.47(8) . . ? N4 Mn3 Mn4 92.45(11) . . ? Mn2 Mn3 Mn4 64.32(2) . . ? Mn1 Mn3 Mn4 65.31(3) . . ? O6 Mn4 O4 98.55(18) . . ? O6 Mn4 O10 115.2(3) . . ? O4 Mn4 O10 98.63(16) . . ? O6 Mn4 O8 134.0(3) . . ? O4 Mn4 O8 93.4(2) . . ? O10 Mn4 O8 106.6(3) . . ? O6 Mn4 Mn3 124.98(16) . . ? O4 Mn4 Mn3 30.34(10) . . ? O10 Mn4 Mn3 73.99(13) . . ? O8 Mn4 Mn3 83.8(2) . . ? O6 Mn4 Mn2 96.11(15) . . ? O4 Mn4 Mn2 32.17(10) . . ? O10 Mn4 Mn2 127.13(13) . . ? O8 Mn4 Mn2 72.01(14) . . ? Mn3 Mn4 Mn2 53.15(2) . . ? O6 Mn4 Mn1 72.22(15) . . ? O4 Mn4 Mn1 30.32(10) . . ? O10 Mn4 Mn1 96.21(14) . . ? O8 Mn4 Mn1 122.56(16) . . ? Mn3 Mn4 Mn1 52.77(2) . . ? Mn2 Mn4 Mn1 52.68(2) . . ? C6 O1 Mn2 121.8(3) . . ? C6 O1 Mn1 115.7(3) . . ? Mn2 O1 Mn1 98.77(13) . . ? C23 O2 Mn3 123.1(3) . . ? C23 O2 Mn2 114.5(3) . . ? Mn3 O2 Mn2 96.12(12) . . ? C40 O3 Mn1 122.0(3) . . ? C40 O3 Mn3 111.5(2) . . ? Mn1 O3 Mn3 96.89(13) . . ? Mn3 O4 Mn4 118.13(17) . . ? Mn3 O4 Mn1 100.82(15) . . ? Mn4 O4 Mn1 119.64(17) . . ? Mn3 O4 Mn2 100.16(15) . . ? Mn4 O4 Mn2 116.25(17) . . ? Mn1 O4 Mn2 98.17(14) . . ? C58 O5 Mn1 141.0(4) . . ? C58 O6 Mn4 131.4(5) . . ? C60 O7 Mn2 136.3(4) . . ? C60 O8 Mn4 126.7(5) . . ? O15 S2 O14 114.3(3) . . ? O15 S2 O16 117.0(3) . . ? O14 S2 O16 113.0(3) . . ? O15 S2 C65 102.9(3) . . ? O14 S2 C65 103.7(3) . . ? O16 S2 C65 103.9(3) . . ? F4 C65 F6 106.4(6) . . ? F4 C65 F5 108.4(6) . . ? F6 C65 F5 106.5(5) . . ? F4 C65 S2 112.1(4) . . ? F6 C65 S2 111.9(5) . . ? F5 C65 S2 111.3(5) . . ? O13 S1 O12 116.9(6) . . ? O13 S1 O11 117.6(5) . . ? O12 S1 O11 110.7(7) . . ? O13 S1 C64 103.3(6) . . ? O12 S1 C64 106.4(6) . . ? O11 S1 C64 99.3(5) . . ? F3 C64 F1 109.0(11) . . ? F3 C64 F2 105.1(11) . . ? F1 C64 F2 109.6(9) . . ? F3 C64 S1 113.5(7) . . ? F1 C64 S1 109.9(8) . . ? F2 C64 S1 109.6(9) . . ? C1 N1 C5 120.0(5) . . ? C1 N1 Mn1 126.0(5) . . ? C5 N1 Mn1 113.9(3) . . ? C11 N2 C7 118.6(5) . . ? C11 N2 Mn2 125.0(4) . . ? C7 N2 Mn2 114.1(3) . . ? C18 N3 C22 118.6(5) . . ? C18 N3 Mn2 124.0(5) . . ? C22 N3 Mn2 117.4(3) . . ? C28 N4 C24 117.0(5) . . ? C28 N4 Mn3 128.0(4) . . ? C24 N4 Mn3 112.5(3) . . ? C35 N5 C39 118.1(5) . . ? C35 N5 Mn3 123.8(4) . . ? C39 N5 Mn3 118.0(3) . . ? C41 N6 C45 118.7(5) . . ? C41 N6 Mn1 113.0(3) . . ? C45 N6 Mn1 126.3(4) . . ? N1 C1 C2 122.4(7) . . ? C3 C2 C1 118.3(7) . . ? C2 C3 C4 119.7(6) . . ? C5 C4 C3 119.0(7) . . ? N1 C5 C4 120.7(5) . . ? N1 C5 C6 115.6(4) . . ? C4 C5 C6 123.6(5) . . ? O1 C6 C5 107.4(4) . . ? O1 C6 C7 106.3(4) . . ? C5 C6 C7 111.7(4) . . ? O1 C6 C12 111.1(4) . . ? C5 C6 C12 111.2(4) . . ? C7 C6 C12 109.1(4) . . ? N2 C7 C8 121.1(5) . . ? N2 C7 C6 113.5(4) . . ? C8 C7 C6 125.4(5) . . ? C9 C8 C7 119.5(5) . . ? C8 C9 C10 119.3(5) . . ? C11 C10 C9 118.3(6) . . ? N2 C11 C10 123.2(6) . . ? C17 C12 C13 118.5(5) . . ? C17 C12 C6 119.6(4) . . ? C13 C12 C6 121.8(4) . . ? C14 C13 C12 118.4(4) . . ? C14 C13 C54 117.4(4) . . ? C12 C13 C54 124.1(4) . . ? C15 C14 C13 122.1(5) . . ? C14 C15 C16 119.2(5) . . ? C17 C16 C15 119.5(5) . . ? C16 C17 C12 122.2(5) . . ? N3 C18 C19 122.9(7) . . ? C20 C19 C18 118.3(7) . . ? C19 C20 C21 119.8(6) . . ? C20 C21 C22 119.3(7) . . ? N3 C22 C21 121.1(5) . . ? N3 C22 C23 116.0(4) . . ? C21 C22 C23 122.8(5) . . ? O2 C23 C22 107.4(4) . . ? O2 C23 C24 106.8(3) . . ? C22 C23 C24 110.1(4) . . ? O2 C23 C29 112.7(4) . . ? C22 C23 C29 111.8(4) . . ? C24 C23 C29 107.9(4) . . ? N4 C24 C25 122.2(4) . . ? N4 C24 C23 112.8(4) . . ? C25 C24 C23 125.0(5) . . ? C24 C25 C26 119.5(6) . . ? C25 C26 C27 118.1(6) . . ? C28 C27 C26 118.8(5) . . ? N4 C28 C27 124.3(6) . . ? C30 C29 C34 117.5(5) . . ? C30 C29 C23 120.4(4) . . ? C34 C29 C23 122.0(4) . . ? C31 C30 C29 122.0(5) . . ? C32 C31 C30 120.6(5) . . ? C31 C32 C33 118.8(5) . . ? C32 C33 C34 121.9(5) . . ? C33 C34 C29 119.1(4) . . ? C33 C34 C56 117.4(4) . . ? C29 C34 C56 123.4(4) . . ? N5 C35 C36 124.3(5) . . ? C35 C36 C37 117.8(5) . . ? C38 C37 C36 119.0(5) . . ? C37 C38 C39 119.6(5) . . ? N5 C39 C38 121.1(4) . . ? N5 C39 C40 115.3(4) . . ? C38 C39 C40 123.6(4) . . ? O3 C40 C39 107.5(4) . . ? O3 C40 C41 106.3(4) . . ? C39 C40 C41 111.7(4) . . ? O3 C40 C46 110.6(4) . . ? C39 C40 C46 110.4(4) . . ? C41 C40 C46 110.2(4) . . ? N6 C41 C42 121.9(5) . . ? N6 C41 C40 113.0(4) . . ? C42 C41 C40 125.0(5) . . ? C41 C42 C43 118.3(6) . . ? C44 C43 C42 119.5(6) . . ? C45 C44 C43 119.1(6) . . ? N6 C45 C44 122.5(6) . . ? C51 C46 C47 118.1(4) . . ? C51 C46 C40 122.3(4) . . ? C47 C46 C40 119.5(4) . . ? C48 C47 C46 121.2(5) . . ? C49 C48 C47 120.2(5) . . ? C48 C49 C50 119.4(5) . . ? C51 C50 C49 121.7(5) . . ? C50 C51 C46 119.4(4) . . ? C50 C51 C52 118.3(4) . . ? C46 C51 C52 122.3(4) . . ? C57 C52 C53 119.9(4) . . ? C57 C52 C51 122.6(4) . . ? C53 C52 C51 117.3(4) . . ? C52 C53 C54 120.6(4) . . ? C55 C54 C53 118.7(4) . . ? C55 C54 C13 118.4(4) . . ? C53 C54 C13 122.8(4) . . ? C54 C55 C56 120.7(4) . . ? C57 C56 C55 119.6(4) . . ? C57 C56 C34 118.9(4) . . ? C55 C56 C34 121.3(4) . . ? C52 C57 C56 120.1(4) . . ? O6 C58 O5 126.1(6) . . ? O6 C58 C59 118.1(7) . . ? O5 C58 C59 115.7(6) . . ? O8 C60 O7 122.9(6) . . ? O8 C60 C61 117.9(5) . . ? O7 C60 C61 119.1(6) . . ? C62 O9 Mn3 141.7(4) . . ? C62 O10 Mn4 131.3(4) . . ? O10 C62 O9 123.5(5) . . ? O10 C62 C63 119.1(5) . . ? O9 C62 C63 117.3(5) . . ? O12B C64B C65B 122.9(19) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.214 _refine_diff_density_min -1.172 _refine_diff_density_rms 0.112 _database_code_depnum_ccdc_archive 'CCDC 858643' ####################################################################### # # 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_jsk35 #TrackingRef 'jsk35.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C63 H48 Mn4 N6 O11, 3(C3 H7 N O)' _chemical_formula_sum 'C72 H69 Mn4 N9 O14' _chemical_formula_weight 1504.12 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 12.6007(5) _cell_length_b 13.0991(5) _cell_length_c 20.5699(8) _cell_angle_alpha 99.263(2) _cell_angle_beta 95.161(2) _cell_angle_gamma 94.247(2) _cell_volume 3323.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9938 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 25.55 _exptl_crystal_description Needle _exptl_crystal_colour Red _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 0.817 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8095 _exptl_absorpt_correction_T_max 0.9450 _exptl_absorpt_process_details ? _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 'Bruker SMART 1000' _diffrn_measurement_method '\w scans at 16 \f settings' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 127889 _diffrn_reflns_av_R_equivalents 0.0973 _diffrn_reflns_av_sigmaI/netI 0.0980 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 30.62 _reflns_number_total 20364 _reflns_number_gt 12128 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.630' _computing_cell_refinement 'Bruker SAINT-Plus v7.68A' _computing_data_reduction 'Bruker SAINT-Plus v7.68A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF 2008' _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 matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details w=1/s^2^(Fo^2^) _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20364 _refine_ls_number_parameters 918 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1066 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.0661 _refine_ls_wR_factor_gt 0.0634 _refine_ls_goodness_of_fit_ref 1.542 _refine_ls_restrained_S_all 1.542 _refine_ls_shift/su_max 0.012 _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 0.46796(3) 0.36397(3) 0.19844(2) 0.01466(10) Uani 1 1 d . A . Mn2 Mn 0.39889(3) 0.41940(3) 0.341303(19) 0.01282(9) Uani 1 1 d . A . Mn3 Mn 0.28055(3) 0.51180(3) 0.219113(19) 0.01364(9) Uani 1 1 d . A . Mn4 Mn 0.55521(4) 0.56815(3) 0.24294(2) 0.02070(11) Uani 1 1 d . . . O1 O 0.41705(13) 0.28185(12) 0.26548(8) 0.0125(4) Uani 1 1 d . . . O2 O 0.24330(13) 0.43235(12) 0.29892(8) 0.0124(4) Uani 1 1 d . . . O3 O 0.30406(13) 0.37521(13) 0.15844(8) 0.0140(4) Uani 1 1 d . . . O4 O 0.55499(14) 0.47341(14) 0.39342(8) 0.0206(4) Uani 1 1 d . . . O5 O 0.65645(14) 0.54376(14) 0.32480(9) 0.0242(5) Uani 1 1 d . A . O6 O 0.50144(16) 0.69947(14) 0.28790(9) 0.0275(5) Uani 1 1 d . A . O7 O 0.32419(16) 0.67658(14) 0.25510(9) 0.0249(5) Uani 1 1 d . . . O8 O 0.7441(2) 0.7570(2) 0.15599(14) 0.0295(8) Uani 0.786(4) 1 d P A 1 O9 O 0.6788(2) 0.6485(2) 0.21921(13) 0.0155(6) Uani 0.786(4) 1 d P A 1 N1 N 0.61539(17) 0.29313(16) 0.24210(10) 0.0172(5) Uani 1 1 d . . . N2 N 0.40460(17) 0.28198(16) 0.39232(10) 0.0161(5) Uani 1 1 d . . . N3 N 0.32381(17) 0.54293(16) 0.41153(10) 0.0162(5) Uani 1 1 d . . . N4 N 0.11105(18) 0.53595(17) 0.23737(10) 0.0209(6) Uani 1 1 d . . . N5 N 0.28673(17) 0.54738(16) 0.10998(10) 0.0153(5) Uani 1 1 d . . . N6 N 0.44498(18) 0.26674(16) 0.10306(11) 0.0195(5) Uani 1 1 d . . . C1 C 0.7167(2) 0.3216(2) 0.23470(14) 0.0234(7) Uani 1 1 d . A . H1 H 0.7311 0.3605 0.2008 0.028 Uiso 1 1 calc R . . C2 C 0.8018(2) 0.2962(2) 0.27489(14) 0.0253(7) Uani 1 1 d . . . H2 H 0.8734 0.3155 0.2678 0.030 Uiso 1 1 calc R A . C3 C 0.7808(2) 0.2426(2) 0.32515(14) 0.0259(7) Uani 1 1 d . A . H3 H 0.8377 0.2248 0.3535 0.031 Uiso 1 1 calc R . . C4 C 0.6757(2) 0.21476(19) 0.33400(13) 0.0189(6) Uani 1 1 d . . . H4 H 0.6595 0.1795 0.3693 0.023 Uiso 1 1 calc R A . C5 C 0.5942(2) 0.23896(19) 0.29072(12) 0.0148(6) Uani 1 1 d . A . C6 C 0.4741(2) 0.20584(19) 0.28944(12) 0.0125(6) Uani 1 1 d . A . C7 C 0.4440(2) 0.19743(19) 0.35979(12) 0.0140(6) Uani 1 1 d . A . C8 C 0.4515(2) 0.1087(2) 0.38782(13) 0.0206(7) Uani 1 1 d . . . H8 H 0.4811 0.0504 0.3649 0.025 Uiso 1 1 calc R A . C9 C 0.4161(2) 0.1048(2) 0.44898(13) 0.0260(7) Uani 1 1 d . A . H9 H 0.4200 0.0438 0.4683 0.031 Uiso 1 1 calc R . . C10 C 0.3752(2) 0.1904(2) 0.48129(14) 0.0283(8) Uani 1 1 d . . . H10 H 0.3498 0.1899 0.5234 0.034 Uiso 1 1 calc R A . C11 C 0.3715(2) 0.2773(2) 0.45159(13) 0.0232(7) Uani 1 1 d . A . H11 H 0.3440 0.3368 0.4745 0.028 Uiso 1 1 calc R . . C12 C 0.4497(2) 0.09876(19) 0.24373(12) 0.0132(6) Uani 1 1 d . . . C13 C 0.5314(2) 0.0327(2) 0.23405(13) 0.0221(7) Uani 1 1 d . A . H13 H 0.5994 0.0523 0.2586 0.027 Uiso 1 1 calc R . . C14 C 0.5168(2) -0.0600(2) 0.19005(14) 0.0278(7) Uani 1 1 d . . . H14 H 0.5735 -0.1035 0.1849 0.033 Uiso 1 1 calc R A . C15 C 0.4190(2) -0.0881(2) 0.15395(13) 0.0268(7) Uani 1 1 d . A . H15 H 0.4086 -0.1505 0.1225 0.032 Uiso 1 1 calc R . . C16 C 0.3361(2) -0.02616(19) 0.16323(13) 0.0207(7) Uani 1 1 d . . . H16 H 0.2688 -0.0468 0.1380 0.025 Uiso 1 1 calc R A . C17 C 0.3487(2) 0.06645(19) 0.20899(12) 0.0143(6) Uani 1 1 d . A . C18 C 0.3812(2) 0.6157(2) 0.45655(13) 0.0232(7) Uani 1 1 d . A . H18 H 0.4523 0.6039 0.4709 0.028 Uiso 1 1 calc R . . C19 C 0.3420(2) 0.7077(2) 0.48339(13) 0.0268(7) Uani 1 1 d . . . H19 H 0.3853 0.7578 0.5153 0.032 Uiso 1 1 calc R A . C20 C 0.2392(2) 0.7248(2) 0.46269(13) 0.0241(7) Uani 1 1 d . A . H20 H 0.2098 0.7869 0.4802 0.029 Uiso 1 1 calc R . . C21 C 0.1789(2) 0.64972(19) 0.41559(12) 0.0176(6) Uani 1 1 d . . . H21 H 0.1079 0.6606 0.4002 0.021 Uiso 1 1 calc R A . C22 C 0.2226(2) 0.5589(2) 0.39115(12) 0.0142(6) Uani 1 1 d . A . C23 C 0.1664(2) 0.46951(19) 0.33780(12) 0.0126(6) Uani 1 1 d . A . C24 C 0.0792(2) 0.51224(19) 0.29405(12) 0.0147(6) Uani 1 1 d . A . C25 C -0.0240(2) 0.52386(19) 0.31008(13) 0.0182(6) Uani 1 1 d . . . H25 H -0.0445 0.5063 0.3505 0.022 Uiso 1 1 calc R A . C26 C -0.0971(2) 0.5608(2) 0.26785(14) 0.0271(7) Uani 1 1 d . A . H26 H -0.1678 0.5698 0.2789 0.033 Uiso 1 1 calc R . . C27 C -0.0653(2) 0.5843(3) 0.20918(15) 0.0413(9) Uani 1 1 d . . . H27 H -0.1137 0.6098 0.1788 0.050 Uiso 1 1 calc R A . C28 C 0.0394(2) 0.5698(2) 0.19532(14) 0.0354(9) Uani 1 1 d . A . H28 H 0.0609 0.5845 0.1544 0.042 Uiso 1 1 calc R . . C29 C 0.11409(19) 0.38370(19) 0.37232(12) 0.0136(6) Uani 1 1 d . . . C30 C 0.0786(2) 0.4109(2) 0.43455(12) 0.0167(6) Uani 1 1 d . A . H30 H 0.0836 0.4822 0.4539 0.020 Uiso 1 1 calc R . . C31 C 0.0366(2) 0.3380(2) 0.46897(12) 0.0184(6) Uani 1 1 d . . . H31 H 0.0121 0.3598 0.5109 0.022 Uiso 1 1 calc R A . C32 C 0.0301(2) 0.2344(2) 0.44297(12) 0.0190(6) Uani 1 1 d . A . H32 H 0.0021 0.1839 0.4667 0.023 Uiso 1 1 calc R . . C33 C 0.0649(2) 0.2049(2) 0.38159(12) 0.0180(6) Uani 1 1 d . . . H33 H 0.0616 0.1331 0.3638 0.022 Uiso 1 1 calc R A . C34 C 0.10496(19) 0.27731(19) 0.34452(12) 0.0136(6) Uani 1 1 d . A . C35 C 0.2957(2) 0.6409(2) 0.09143(13) 0.0201(7) Uani 1 1 d . A . H35 H 0.2761 0.6988 0.1205 0.024 Uiso 1 1 calc R . . C36 C 0.3323(2) 0.6575(2) 0.03187(13) 0.0207(7) Uani 1 1 d . . . H36 H 0.3353 0.7247 0.0200 0.025 Uiso 1 1 calc R A . C37 C 0.3640(2) 0.5750(2) -0.00931(13) 0.0237(7) Uani 1 1 d . A . H37 H 0.3911 0.5840 -0.0498 0.028 Uiso 1 1 calc R . . C38 C 0.3555(2) 0.4785(2) 0.00937(12) 0.0210(7) Uani 1 1 d . . . H38 H 0.3783 0.4204 -0.0180 0.025 Uiso 1 1 calc R A . C39 C 0.3141(2) 0.4660(2) 0.06797(12) 0.0157(6) Uani 1 1 d . A . C40 C 0.2860(2) 0.36083(19) 0.09025(12) 0.0151(6) Uani 1 1 d . A . C41 C 0.3580(2) 0.2773(2) 0.06154(13) 0.0195(6) Uani 1 1 d . A . C42 C 0.3369(2) 0.2160(2) 0.00008(13) 0.0264(7) Uani 1 1 d . . . H42 H 0.2755 0.2238 -0.0284 0.032 Uiso 1 1 calc R A . C43 C 0.4060(3) 0.1432(2) -0.01947(14) 0.0330(8) Uani 1 1 d . A . H43 H 0.3917 0.0995 -0.0614 0.040 Uiso 1 1 calc R . . C44 C 0.4947(2) 0.1337(2) 0.02104(15) 0.0337(8) Uani 1 1 d . . . H44 H 0.5439 0.0850 0.0074 0.040 Uiso 1 1 calc R A . C45 C 0.5118(2) 0.1960(2) 0.08217(14) 0.0256(7) Uani 1 1 d . A . H45 H 0.5732 0.1887 0.1108 0.031 Uiso 1 1 calc R . . C46 C 0.1652(2) 0.3286(2) 0.06454(12) 0.0174(6) Uani 1 1 d . . . C47 C 0.1204(2) 0.3608(2) 0.00761(13) 0.0257(7) Uani 1 1 d . A . H47 H 0.1655 0.3965 -0.0176 0.031 Uiso 1 1 calc R . . C48 C 0.0130(3) 0.3424(2) -0.01314(15) 0.0344(8) Uani 1 1 d . . . H48 H -0.0148 0.3640 -0.0527 0.041 Uiso 1 1 calc R A . C49 C -0.0544(2) 0.2929(2) 0.02315(14) 0.0335(8) Uani 1 1 d . A . H49 H -0.1291 0.2820 0.0098 0.040 Uiso 1 1 calc R . . C50 C -0.0119(2) 0.2594(2) 0.07922(13) 0.0258(7) Uani 1 1 d . . . H50 H -0.0582 0.2244 0.1041 0.031 Uiso 1 1 calc R A . C51 C 0.0969(2) 0.2754(2) 0.10032(12) 0.0164(6) Uani 1 1 d . A . C52 C 0.1344(2) 0.23286(19) 0.16022(13) 0.0156(6) Uani 1 1 d . . . C53 C 0.2122(2) 0.16229(18) 0.15765(12) 0.0157(6) Uani 1 1 d . A . H53 H 0.2361 0.1362 0.1162 0.019 Uiso 1 1 calc R . . C54 C 0.2552(2) 0.12949(19) 0.21436(12) 0.0142(6) Uani 1 1 d . . . C55 C 0.2150(2) 0.16314(19) 0.27387(12) 0.0144(6) Uani 1 1 d . A . H55 H 0.2401 0.1369 0.3123 0.017 Uiso 1 1 calc R . . C56 C 0.1386(2) 0.23447(18) 0.27840(12) 0.0130(6) Uani 1 1 d . . . C57 C 0.0977(2) 0.26709(19) 0.22089(12) 0.0156(6) Uani 1 1 d . A . H57 H 0.0434 0.3138 0.2232 0.019 Uiso 1 1 calc R . . C58 C 0.6420(2) 0.5070(2) 0.37690(13) 0.0191(6) Uani 1 1 d . A . C59 C 0.7436(2) 0.5023(2) 0.42240(12) 0.0235(7) Uani 1 1 d . . . H59A H 0.7254 0.5027 0.4678 0.035 Uiso 1 1 calc R A . H59B H 0.7938 0.5627 0.4213 0.035 Uiso 1 1 calc R . . H59C H 0.7767 0.4385 0.4073 0.035 Uiso 1 1 calc R . . C60 C 0.4067(3) 0.7263(2) 0.28736(14) 0.0241(7) Uani 1 1 d . A . C61 C 0.3934(2) 0.8299(2) 0.32887(14) 0.0340(8) Uani 1 1 d . . . H61A H 0.3758 0.8799 0.2998 0.051 Uiso 1 1 calc R A . H61B H 0.4602 0.8553 0.3568 0.051 Uiso 1 1 calc R . . H61C H 0.3355 0.8217 0.3569 0.051 Uiso 1 1 calc R . . C62 C 0.6688(5) 0.6987(4) 0.1711(3) 0.0185(11) Uani 0.786(4) 1 d P A 1 C63 C 0.5613(3) 0.6869(2) 0.13272(16) 0.0202(9) Uani 0.786(4) 1 d P A 1 H63A H 0.5425 0.6136 0.1136 0.030 Uiso 0.786(4) 1 calc PR A 1 H63B H 0.5627 0.7283 0.0971 0.030 Uiso 0.786(4) 1 calc PR A 1 H63C H 0.5081 0.7109 0.1622 0.030 Uiso 0.786(4) 1 calc PR A 1 O10 O 0.43984(13) 0.48733(12) 0.26023(8) 0.0128(4) Uani 1 1 d . A . O11 O 0.55926(14) 0.46340(13) 0.17090(8) 0.0211(5) Uani 1 1 d . A . O8B O 0.7060(10) 0.6197(10) 0.1347(6) 0.075(5) Uiso 0.214(4) 1 d P A 2 O9B O 0.6512(10) 0.6882(9) 0.2255(6) 0.036(4) Uiso 0.214(4) 1 d P A 2 C62B C 0.7053(19) 0.706(2) 0.1765(15) 0.041(9) Uiso 0.214(4) 1 d P A 2 C63B C 0.7823(14) 0.7843(13) 0.1868(9) 0.041(5) Uiso 0.214(4) 1 d P A 2 H63D H 0.7627 0.8408 0.2196 0.061 Uiso 0.214(4) 1 calc PR A 2 H63E H 0.7909 0.8096 0.1451 0.061 Uiso 0.214(4) 1 calc PR A 2 H63F H 0.8498 0.7600 0.2031 0.061 Uiso 0.214(4) 1 calc PR A 2 C1B C 1.0351(4) 0.0663(3) 0.7277(2) 0.1036(19) Uani 1 1 d . . . H1B1 H 1.0512 0.0363 0.6833 0.155 Uiso 1 1 calc R . . H1B2 H 1.0185 0.0104 0.7526 0.155 Uiso 1 1 calc R . . H1B3 H 1.0973 0.1112 0.7508 0.155 Uiso 1 1 calc R . . C3B C 0.9024(4) 0.1587(4) 0.7861(2) 0.112(2) Uani 1 1 d . . . H3B1 H 0.8452 0.2043 0.7803 0.167 Uiso 1 1 calc R . . H3B2 H 0.9602 0.1960 0.8181 0.167 Uiso 1 1 calc R . . H3B3 H 0.8738 0.0970 0.8024 0.167 Uiso 1 1 calc R . . C5B C 0.8991(4) 0.1514(5) 0.6699(3) 0.135(3) Uani 1 1 d . . . H5B H 0.8375 0.1889 0.6733 0.162 Uiso 1 1 calc R . . N1B N 0.9440(3) 0.1268(3) 0.7225(2) 0.0823(12) Uani 1 1 d . . . O1B O 0.9326(3) 0.1283(4) 0.6123(2) 0.1512(18) Uani 1 1 d . . . N1C N 0.1574(2) 0.9934(2) 0.92348(14) 0.0462(8) Uani 1 1 d . . . O1C O 0.2596(2) 0.89546(18) 0.98141(13) 0.0618(8) Uani 1 1 d . . . C2C C 0.1934(3) 0.9562(3) 0.85886(17) 0.0706(13) Uani 1 1 d . . . H2C1 H 0.2449 0.9046 0.8635 0.106 Uiso 1 1 calc R . . H2C2 H 0.2276 1.0147 0.8419 0.106 Uiso 1 1 calc R . . H2C3 H 0.1318 0.9243 0.8279 0.106 Uiso 1 1 calc R . . C3C C 0.0761(3) 1.0674(3) 0.92553(17) 0.0692(13) Uani 1 1 d . . . H3C1 H 0.0618 1.0894 0.9715 0.104 Uiso 1 1 calc R . . H3C2 H 0.0101 1.0343 0.8993 0.104 Uiso 1 1 calc R . . H3C3 H 0.1017 1.1280 0.9071 0.104 Uiso 1 1 calc R . . C5C C 0.1940(3) 0.9602(3) 0.97880(18) 0.0480(10) Uani 1 1 d . . . H5C H 0.1674 0.9886 1.0190 0.058 Uiso 1 1 calc R . . C1D C 0.3069(3) 0.0988(4) 0.6392(3) 0.104(2) Uani 1 1 d . . . H1D H 0.3443 0.1431 0.6767 0.125 Uiso 1 1 calc R . . N1D N 0.2185(2) 0.1169(2) 0.60606(15) 0.0518(9) Uani 1 1 d . . . O1D O 0.3357(3) 0.0056(3) 0.6105(2) 0.1536(18) Uani 1 1 d . . . C2D C 0.1860(3) 0.2228(3) 0.62158(18) 0.0714(14) Uani 1 1 d . . . H2D1 H 0.1139 0.2200 0.6360 0.107 Uiso 1 1 calc R . . H2D2 H 0.1861 0.2557 0.5820 0.107 Uiso 1 1 calc R . . H2D3 H 0.2364 0.2634 0.6571 0.107 Uiso 1 1 calc R . . C3D C 0.1586(4) 0.0367(4) 0.5507(2) 0.119(2) Uani 1 1 d . . . H3D1 H 0.1699 0.0569 0.5079 0.179 Uiso 1 1 calc R . . H3D2 H 0.0820 0.0327 0.5561 0.179 Uiso 1 1 calc R . . H3D3 H 0.1852 -0.0313 0.5525 0.179 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 0.0115(2) 0.0182(2) 0.0158(2) 0.00530(19) 0.00420(18) 0.00273(18) Mn2 0.0100(2) 0.0162(2) 0.0125(2) 0.00209(18) 0.00163(17) 0.00264(18) Mn3 0.0115(2) 0.0182(2) 0.0124(2) 0.00426(18) 0.00323(18) 0.00360(18) Mn4 0.0170(3) 0.0239(2) 0.0207(3) 0.0054(2) 0.0022(2) -0.0052(2) O1 0.0107(10) 0.0148(9) 0.0129(10) 0.0037(8) 0.0016(8) 0.0042(8) O2 0.0090(10) 0.0175(10) 0.0109(10) 0.0010(8) 0.0042(8) 0.0019(8) O3 0.0136(10) 0.0186(10) 0.0105(10) 0.0033(8) 0.0025(8) 0.0027(8) O4 0.0108(11) 0.0330(12) 0.0169(11) 0.0029(9) 0.0013(8) -0.0012(9) O5 0.0171(12) 0.0343(12) 0.0209(12) 0.0072(10) -0.0008(9) -0.0030(9) O6 0.0285(13) 0.0200(11) 0.0323(13) 0.0003(9) 0.0039(10) -0.0006(10) O7 0.0293(13) 0.0190(11) 0.0248(12) 0.0019(9) -0.0021(10) 0.0019(9) O8 0.0213(17) 0.0390(19) 0.0314(19) 0.0234(16) -0.0005(14) -0.0101(14) O9 0.0111(14) 0.0163(14) 0.0210(15) 0.0081(12) 0.0025(11) 0.0016(12) N1 0.0121(13) 0.0172(12) 0.0217(14) 0.0008(10) 0.0040(10) 0.0000(10) N2 0.0146(13) 0.0232(13) 0.0116(12) 0.0044(10) 0.0041(10) 0.0026(10) N3 0.0127(13) 0.0222(13) 0.0130(13) 0.0010(10) 0.0021(10) 0.0010(10) N4 0.0165(13) 0.0336(14) 0.0173(13) 0.0132(11) 0.0033(10) 0.0109(11) N5 0.0140(13) 0.0182(12) 0.0142(13) 0.0050(10) 0.0004(10) 0.0017(10) N6 0.0154(13) 0.0156(12) 0.0280(15) 0.0025(11) 0.0067(11) 0.0033(10) C1 0.0173(17) 0.0250(16) 0.0293(18) 0.0062(14) 0.0082(14) 0.0004(13) C2 0.0092(15) 0.0275(17) 0.038(2) -0.0006(15) 0.0054(14) 0.0005(13) C3 0.0156(17) 0.0286(17) 0.0316(19) 0.0010(15) -0.0040(14) 0.0066(14) C4 0.0184(16) 0.0220(15) 0.0161(16) 0.0023(12) -0.0003(12) 0.0055(13) C5 0.0151(15) 0.0133(13) 0.0147(15) -0.0031(11) 0.0026(12) 0.0039(12) C6 0.0122(14) 0.0136(13) 0.0115(14) 0.0014(11) 0.0013(11) 0.0003(11) C7 0.0099(14) 0.0175(14) 0.0138(15) 0.0030(12) -0.0012(11) -0.0021(11) C8 0.0213(17) 0.0192(15) 0.0217(17) 0.0046(13) -0.0001(13) 0.0045(13) C9 0.033(2) 0.0246(16) 0.0215(17) 0.0109(14) -0.0024(14) 0.0025(14) C10 0.033(2) 0.0369(19) 0.0186(17) 0.0123(15) 0.0074(14) 0.0052(16) C11 0.0242(18) 0.0312(17) 0.0152(16) 0.0037(13) 0.0049(13) 0.0066(14) C12 0.0163(15) 0.0151(14) 0.0095(14) 0.0034(11) 0.0044(11) 0.0033(12) C13 0.0184(16) 0.0231(16) 0.0234(17) -0.0002(13) 0.0009(13) 0.0032(13) C14 0.0242(18) 0.0218(16) 0.035(2) -0.0043(14) 0.0060(15) 0.0063(14) C15 0.0323(19) 0.0183(15) 0.0270(18) -0.0075(13) 0.0075(15) 0.0026(14) C16 0.0174(16) 0.0208(15) 0.0229(17) 0.0018(13) 0.0013(13) -0.0012(13) C17 0.0176(15) 0.0140(14) 0.0125(15) 0.0041(11) 0.0047(12) 0.0008(12) C18 0.0167(16) 0.0345(18) 0.0163(16) -0.0001(14) 0.0000(13) 0.0009(14) C19 0.0274(19) 0.0291(17) 0.0193(17) -0.0086(14) 0.0036(14) -0.0023(14) C20 0.0277(18) 0.0217(16) 0.0227(17) -0.0023(13) 0.0115(14) 0.0038(14) C21 0.0151(15) 0.0208(15) 0.0181(16) 0.0038(12) 0.0053(12) 0.0038(12) C22 0.0149(15) 0.0214(15) 0.0075(14) 0.0043(11) 0.0055(11) 0.0011(12) C23 0.0104(14) 0.0172(14) 0.0115(14) 0.0036(11) 0.0044(11) 0.0039(11) C24 0.0143(15) 0.0150(14) 0.0156(15) 0.0028(12) 0.0044(12) 0.0028(11) C25 0.0142(15) 0.0235(15) 0.0187(16) 0.0066(13) 0.0042(12) 0.0038(12) C26 0.0152(17) 0.0359(18) 0.0326(19) 0.0099(15) 0.0030(14) 0.0081(14) C27 0.0214(19) 0.072(3) 0.039(2) 0.030(2) 0.0017(16) 0.0167(18) C28 0.0231(19) 0.067(2) 0.0249(19) 0.0275(18) 0.0055(15) 0.0153(18) C29 0.0071(13) 0.0213(14) 0.0132(15) 0.0044(12) 0.0003(11) 0.0035(11) C30 0.0113(14) 0.0225(15) 0.0170(15) 0.0035(12) 0.0032(12) 0.0044(12) C31 0.0135(15) 0.0304(17) 0.0134(15) 0.0056(13) 0.0059(12) 0.0051(13) C32 0.0136(15) 0.0292(16) 0.0166(16) 0.0109(13) 0.0031(12) 0.0012(13) C33 0.0153(15) 0.0207(15) 0.0184(16) 0.0045(12) 0.0019(12) 0.0008(12) C34 0.0070(13) 0.0192(14) 0.0146(15) 0.0037(12) 0.0009(11) 0.0008(11) C35 0.0171(16) 0.0200(15) 0.0221(17) 0.0013(13) -0.0010(13) 0.0030(13) C36 0.0194(16) 0.0232(16) 0.0221(17) 0.0141(13) -0.0004(13) 0.0003(13) C37 0.0201(17) 0.0342(18) 0.0206(17) 0.0137(14) 0.0057(13) 0.0040(14) C38 0.0216(17) 0.0290(16) 0.0142(16) 0.0044(13) 0.0064(13) 0.0056(13) C39 0.0123(15) 0.0218(15) 0.0129(15) 0.0043(12) -0.0025(12) 0.0019(12) C40 0.0170(15) 0.0177(14) 0.0120(15) 0.0042(12) 0.0037(12) 0.0033(12) C41 0.0223(17) 0.0169(15) 0.0212(16) 0.0049(13) 0.0102(13) 0.0007(13) C42 0.0317(19) 0.0301(17) 0.0163(17) -0.0013(14) 0.0056(14) 0.0029(15) C43 0.044(2) 0.0287(18) 0.0242(19) -0.0064(14) 0.0116(16) 0.0022(16) C44 0.034(2) 0.0147(15) 0.053(2) -0.0022(15) 0.0218(17) 0.0049(14) C45 0.0186(17) 0.0185(15) 0.041(2) 0.0070(14) 0.0089(14) 0.0013(13) C46 0.0164(16) 0.0202(15) 0.0145(15) 0.0020(12) -0.0016(12) 0.0008(12) C47 0.0245(18) 0.0338(18) 0.0188(17) 0.0102(14) -0.0027(14) -0.0038(14) C48 0.030(2) 0.045(2) 0.029(2) 0.0199(16) -0.0121(16) -0.0014(17) C49 0.0167(17) 0.047(2) 0.036(2) 0.0139(17) -0.0114(15) -0.0015(15) C50 0.0213(17) 0.0338(18) 0.0231(18) 0.0089(14) 0.0011(14) -0.0007(14) C51 0.0148(15) 0.0184(14) 0.0146(15) 0.0000(12) -0.0016(12) 0.0019(12) C52 0.0113(14) 0.0170(14) 0.0162(15) 0.0003(12) -0.0011(12) -0.0039(11) C53 0.0155(15) 0.0173(14) 0.0125(15) -0.0022(12) 0.0051(12) -0.0049(12) C54 0.0113(14) 0.0136(13) 0.0163(15) 0.0013(12) -0.0005(12) -0.0020(11) C55 0.0106(14) 0.0193(14) 0.0137(15) 0.0056(12) 0.0003(11) -0.0007(11) C56 0.0117(14) 0.0138(13) 0.0131(15) 0.0020(11) 0.0040(11) -0.0041(11) C57 0.0094(14) 0.0180(14) 0.0196(16) 0.0033(12) 0.0014(12) 0.0013(11) C58 0.0195(17) 0.0201(15) 0.0158(16) -0.0045(12) 0.0019(13) 0.0057(13) C59 0.0145(16) 0.0330(17) 0.0215(17) 0.0016(14) -0.0012(13) 0.0039(13) C60 0.040(2) 0.0175(15) 0.0168(17) 0.0059(13) 0.0075(15) 0.0022(15) C61 0.039(2) 0.0254(18) 0.037(2) 0.0008(15) 0.0053(16) 0.0047(16) C62 0.016(3) 0.020(2) 0.018(3) -0.0001(17) 0.004(2) -0.003(2) C63 0.023(2) 0.0193(19) 0.020(2) 0.0067(16) 0.0058(17) 0.0068(16) O10 0.0112(10) 0.0147(9) 0.0121(10) 0.0015(8) 0.0034(8) -0.0012(8) O11 0.0239(12) 0.0253(11) 0.0164(11) 0.0047(9) 0.0089(9) 0.0071(9) C1B 0.091(4) 0.075(3) 0.135(5) -0.013(3) -0.009(3) 0.040(3) C3B 0.091(4) 0.130(5) 0.134(5) 0.060(4) 0.054(4) 0.008(4) C5B 0.070(4) 0.251(8) 0.124(6) 0.123(6) 0.022(4) 0.060(5) N1B 0.053(3) 0.095(3) 0.110(4) 0.053(3) 0.005(3) 0.009(2) O1B 0.105(4) 0.235(5) 0.129(4) 0.077(4) -0.004(3) 0.036(3) N1C 0.050(2) 0.0374(18) 0.049(2) 0.0022(15) 0.0029(17) 0.0055(15) O1C 0.0432(18) 0.0522(17) 0.089(2) 0.0192(15) -0.0100(15) 0.0031(14) C2C 0.075(3) 0.075(3) 0.060(3) -0.006(2) 0.027(2) 0.007(3) C3C 0.057(3) 0.062(3) 0.083(3) -0.006(2) -0.007(2) 0.027(2) C5C 0.043(3) 0.047(2) 0.050(3) 0.011(2) -0.010(2) -0.0109(19) C1D 0.042(3) 0.083(4) 0.198(6) 0.052(4) -0.005(3) 0.033(3) N1D 0.039(2) 0.0362(18) 0.083(3) 0.0107(17) 0.0145(18) 0.0100(16) O1D 0.133(4) 0.117(3) 0.255(5) 0.105(3) 0.068(3) 0.074(3) C2D 0.085(4) 0.045(3) 0.080(3) -0.008(2) 0.005(3) 0.023(2) C3D 0.113(5) 0.130(5) 0.089(4) -0.037(3) 0.029(3) -0.065(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 O11 1.8638(19) . yes Mn1 O10 1.9639(16) . yes Mn1 O1 2.0012(17) . yes Mn1 N6 2.143(2) . yes Mn1 O3 2.1777(17) . yes Mn1 N1 2.311(2) . yes Mn1 Mn4 2.7921(6) . yes Mn1 Mn2 3.1285(6) . yes Mn1 Mn3 3.1781(5) . yes Mn2 O10 2.0985(16) . yes Mn2 O2 2.1028(16) . yes Mn2 O4 2.1654(18) . yes Mn2 O1 2.2253(16) . yes Mn2 N2 2.227(2) . yes Mn2 N3 2.307(2) . yes Mn2 Mn3 3.2524(6) . yes Mn2 Mn4 3.6315(6) . yes Mn3 O3 2.0671(16) . yes Mn3 O2 2.1483(16) . yes Mn3 O10 2.1735(17) . yes Mn3 O7 2.1786(18) . yes Mn3 N4 2.238(2) . yes Mn3 N5 2.372(2) . yes Mn3 Mn4 3.4588(6) . yes Mn4 O10 1.8295(17) . yes Mn4 O11 1.8576(17) . yes Mn4 O9 1.957(3) . yes Mn4 O9B 2.011(13) . yes Mn4 O6 2.0116(18) . yes Mn4 O5 2.1004(18) . yes O1 C6 1.397(3) . ? O2 C23 1.378(3) . ? O3 C40 1.380(3) . ? O4 C58 1.247(3) . ? O5 C58 1.266(3) . ? O6 C60 1.268(3) . ? O7 C60 1.258(3) . ? O8 C62 1.265(7) . ? O9 C62 1.277(6) . ? N1 C1 1.332(3) . ? N1 C5 1.350(3) . ? N2 C11 1.333(3) . ? N2 C7 1.350(3) . ? N3 C18 1.335(3) . ? N3 C22 1.348(3) . ? N4 C24 1.341(3) . ? N4 C28 1.343(3) . ? N5 C35 1.340(3) . ? N5 C39 1.346(3) . ? N6 C45 1.343(3) . ? N6 C41 1.358(3) . ? C1 C2 1.388(3) . ? C2 C3 1.374(4) . ? C3 C4 1.383(4) . ? C4 C5 1.386(3) . ? C5 C6 1.540(3) . ? C6 C7 1.548(3) . ? C6 C12 1.551(3) . ? C7 C8 1.383(3) . ? C8 C9 1.380(3) . ? C9 C10 1.368(3) . ? C10 C11 1.378(3) . ? C12 C13 1.400(3) . ? C12 C17 1.403(3) . ? C13 C14 1.382(3) . ? C14 C15 1.373(4) . ? C15 C16 1.379(3) . ? C16 C17 1.400(3) . ? C17 C54 1.491(3) . ? C18 C19 1.388(3) . ? C19 C20 1.373(4) . ? C20 C21 1.391(4) . ? C21 C22 1.388(3) . ? C22 C23 1.549(3) . ? C23 C24 1.551(3) . ? C23 C29 1.560(3) . ? C24 C25 1.383(3) . ? C25 C26 1.377(3) . ? C26 C27 1.378(4) . ? C27 C28 1.395(4) . ? C29 C30 1.394(3) . ? C29 C34 1.411(3) . ? C30 C31 1.379(3) . ? C31 C32 1.370(3) . ? C32 C33 1.380(3) . ? C33 C34 1.402(3) . ? C34 C56 1.496(3) . ? C35 C36 1.391(3) . ? C36 C37 1.369(3) . ? C37 C38 1.379(3) . ? C38 C39 1.384(3) . ? C39 C40 1.547(3) . ? C40 C41 1.550(3) . ? C40 C46 1.570(4) . ? C41 C42 1.377(3) . ? C42 C43 1.375(4) . ? C43 C44 1.358(4) . ? C44 C45 1.374(4) . ? C46 C47 1.394(3) . ? C46 C51 1.400(3) . ? C47 C48 1.373(4) . ? C48 C49 1.374(4) . ? C49 C50 1.377(3) . ? C50 C51 1.390(4) . ? C51 C52 1.486(3) . ? C52 C57 1.388(3) . ? C52 C53 1.394(3) . ? C53 C54 1.386(3) . ? C54 C55 1.386(3) . ? C55 C56 1.389(3) . ? C56 C57 1.390(3) . ? C58 C59 1.527(3) . ? C60 C61 1.512(3) . ? C62 C63 1.489(6) . ? O8B C62B 1.31(3) . ? O9B C62B 1.31(3) . ? C62B C63B 1.34(3) . ? C1B N1B 1.449(4) . ? C3B N1B 1.463(5) . ? C5B N1B 1.274(5) . ? C5B O1B 1.292(6) . ? N1C C5C 1.338(4) . ? N1C C3C 1.461(4) . ? N1C C2C 1.464(4) . ? O1C C5C 1.232(4) . ? C1D N1D 1.311(4) . ? C1D O1D 1.358(5) . ? N1D C2D 1.469(4) . ? N1D C3D 1.521(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Mn1 O10 80.49(7) . . yes O11 Mn1 O1 153.20(8) . . yes O10 Mn1 O1 86.08(7) . . yes O11 Mn1 N6 93.74(8) . . yes O10 Mn1 N6 151.71(7) . . yes O1 Mn1 N6 108.60(8) . . yes O11 Mn1 O3 109.66(7) . . yes O10 Mn1 O3 82.36(6) . . yes O1 Mn1 O3 91.21(6) . . yes N6 Mn1 O3 73.51(7) . . yes O11 Mn1 N1 89.35(8) . . yes O10 Mn1 N1 109.17(7) . . yes O1 Mn1 N1 73.27(7) . . yes N6 Mn1 N1 98.36(8) . . yes O3 Mn1 N1 159.49(7) . . yes O11 Mn1 Mn4 41.30(5) . . yes O10 Mn1 Mn4 40.77(5) . . yes O1 Mn1 Mn4 118.01(5) . . yes N6 Mn1 Mn4 133.37(6) . . yes O3 Mn1 Mn4 105.74(5) . . yes N1 Mn1 Mn4 93.56(6) . . yes O11 Mn1 Mn2 116.44(5) . . yes O10 Mn1 Mn2 41.24(5) . . yes O1 Mn1 Mn2 45.09(5) . . yes N6 Mn1 Mn2 149.04(6) . . yes O3 Mn1 Mn2 89.03(4) . . yes N1 Mn1 Mn2 89.19(5) . . yes Mn4 Mn1 Mn2 75.430(15) . . yes O11 Mn1 Mn3 94.36(5) . . yes O10 Mn1 Mn3 42.30(5) . . yes O1 Mn1 Mn3 91.05(5) . . yes N6 Mn1 Mn3 111.58(6) . . yes O3 Mn1 Mn3 40.22(4) . . yes N1 Mn1 Mn3 149.47(5) . . yes Mn4 Mn1 Mn3 70.472(15) . . yes Mn2 Mn1 Mn3 62.086(12) . . yes O10 Mn2 O2 81.76(6) . . yes O10 Mn2 O4 90.23(7) . . yes O2 Mn2 O4 156.62(7) . . yes O10 Mn2 O1 77.43(6) . . yes O2 Mn2 O1 91.55(6) . . yes O4 Mn2 O1 108.19(6) . . yes O10 Mn2 N2 147.05(7) . . yes O2 Mn2 N2 111.47(7) . . yes O4 Mn2 N2 87.03(7) . . yes O1 Mn2 N2 72.33(7) . . yes O10 Mn2 N3 107.29(7) . . yes O2 Mn2 N3 72.17(7) . . yes O4 Mn2 N3 89.56(7) . . yes O1 Mn2 N3 161.80(7) . . yes N2 Mn2 N3 105.52(7) . . yes O10 Mn2 Mn1 38.09(4) . . yes O2 Mn2 Mn1 88.74(4) . . yes O4 Mn2 Mn1 98.46(5) . . yes O1 Mn2 Mn1 39.56(4) . . yes N2 Mn2 Mn1 110.02(5) . . yes N3 Mn2 Mn1 143.86(5) . . yes O10 Mn2 Mn3 41.28(5) . . yes O2 Mn2 Mn3 40.60(4) . . yes O4 Mn2 Mn3 126.65(5) . . yes O1 Mn2 Mn3 85.28(4) . . yes N2 Mn2 Mn3 144.60(6) . . yes N3 Mn2 Mn3 87.29(5) . . yes Mn1 Mn2 Mn3 59.706(12) . . yes O10 Mn2 Mn4 20.84(5) . . yes O2 Mn2 Mn4 100.44(5) . . yes O4 Mn2 Mn4 69.46(5) . . yes O1 Mn2 Mn4 86.13(4) . . yes N2 Mn2 Mn4 141.44(5) . . yes N3 Mn2 Mn4 104.43(5) . . yes Mn1 Mn2 Mn4 48.083(12) . . yes Mn3 Mn2 Mn4 60.024(12) . . yes O3 Mn3 O2 92.55(6) . . yes O3 Mn3 O10 80.16(6) . . yes O2 Mn3 O10 79.02(6) . . yes O3 Mn3 O7 150.22(7) . . yes O2 Mn3 O7 110.88(7) . . yes O10 Mn3 O7 86.38(7) . . yes O3 Mn3 N4 116.10(8) . . yes O2 Mn3 N4 72.49(7) . . yes O10 Mn3 N4 147.39(7) . . yes O7 Mn3 N4 89.17(8) . . yes O3 Mn3 N5 72.10(7) . . yes O2 Mn3 N5 160.08(7) . . yes O10 Mn3 N5 109.71(7) . . yes O7 Mn3 N5 87.94(7) . . yes N4 Mn3 N5 102.38(7) . . yes O3 Mn3 Mn1 42.86(5) . . yes O2 Mn3 Mn1 86.66(4) . . yes O10 Mn3 Mn1 37.45(4) . . yes O7 Mn3 Mn1 118.02(5) . . yes N4 Mn3 Mn1 150.66(6) . . yes N5 Mn3 Mn1 90.17(5) . . yes O3 Mn3 Mn2 87.65(5) . . yes O2 Mn3 Mn2 39.57(4) . . yes O10 Mn3 Mn2 39.57(4) . . yes O7 Mn3 Mn2 98.72(5) . . yes N4 Mn3 Mn2 109.86(5) . . yes N5 Mn3 Mn2 147.10(5) . . yes Mn1 Mn3 Mn2 58.208(12) . . yes O3 Mn3 Mn4 88.40(5) . . yes O2 Mn3 Mn4 104.81(5) . . yes O10 Mn3 Mn4 27.47(4) . . yes O7 Mn3 Mn4 68.49(5) . . yes N4 Mn3 Mn4 155.27(6) . . yes N5 Mn3 Mn4 87.80(5) . . yes Mn1 Mn3 Mn4 49.534(12) . . yes Mn2 Mn3 Mn4 65.434(13) . . yes O10 Mn4 O11 84.29(8) . . yes O10 Mn4 O9 176.37(10) . . yes O11 Mn4 O9 92.10(10) . . yes O10 Mn4 O9B 163.3(3) . . yes O11 Mn4 O9B 105.3(4) . . yes O9 Mn4 O9B 18.8(3) . . yes O10 Mn4 O6 92.70(8) . . yes O11 Mn4 O6 152.71(8) . . yes O9 Mn4 O6 90.35(10) . . yes O9B Mn4 O6 72.5(3) . . yes O10 Mn4 O5 95.48(7) . . yes O11 Mn4 O5 111.07(7) . . yes O9 Mn4 O5 86.14(9) . . yes O9B Mn4 O5 93.7(4) . . yes O6 Mn4 O5 96.21(7) . . yes O10 Mn4 Mn1 44.51(5) . . yes O11 Mn4 Mn1 41.47(6) . . yes O9 Mn4 Mn1 132.06(8) . . yes O9B Mn4 Mn1 146.8(3) . . yes O6 Mn4 Mn1 135.54(6) . . yes O5 Mn4 Mn1 98.96(5) . . yes O10 Mn4 Mn3 33.23(5) . . yes O11 Mn4 Mn3 85.80(6) . . yes O9 Mn4 Mn3 146.30(8) . . yes O9B Mn4 Mn3 132.3(3) . . yes O6 Mn4 Mn3 77.30(6) . . yes O5 Mn4 Mn3 125.91(5) . . yes Mn1 Mn4 Mn3 59.994(13) . . yes O10 Mn4 Mn2 24.08(5) . . yes O11 Mn4 Mn2 97.73(6) . . yes O9 Mn4 Mn2 158.06(8) . . yes O9B Mn4 Mn2 156.2(4) . . yes O6 Mn4 Mn2 89.81(6) . . yes O5 Mn4 Mn2 72.04(5) . . yes Mn1 Mn4 Mn2 56.487(13) . . yes Mn3 Mn4 Mn2 54.542(11) . . yes C6 O1 Mn1 123.53(15) . . ? C6 O1 Mn2 114.45(14) . . ? Mn1 O1 Mn2 95.35(7) . . ? C23 O2 Mn2 120.69(15) . . ? C23 O2 Mn3 117.90(14) . . ? Mn2 O2 Mn3 99.82(7) . . ? C40 O3 Mn3 123.24(14) . . ? C40 O3 Mn1 115.63(14) . . ? Mn3 O3 Mn1 96.92(7) . . ? C58 O4 Mn2 134.70(18) . . ? C58 O5 Mn4 134.34(18) . . ? C60 O6 Mn4 129.44(19) . . ? C60 O7 Mn3 132.89(18) . . ? C62 O9 Mn4 120.4(3) . . ? C1 N1 C5 119.2(2) . . ? C1 N1 Mn1 125.13(18) . . ? C5 N1 Mn1 113.55(16) . . ? C11 N2 C7 118.4(2) . . ? C11 N2 Mn2 124.95(18) . . ? C7 N2 Mn2 116.68(16) . . ? C18 N3 C22 118.7(2) . . ? C18 N3 Mn2 123.46(18) . . ? C22 N3 Mn2 114.66(16) . . ? C24 N4 C28 118.3(2) . . ? C24 N4 Mn3 116.80(16) . . ? C28 N4 Mn3 124.85(19) . . ? C35 N5 C39 117.5(2) . . ? C35 N5 Mn3 127.21(17) . . ? C39 N5 Mn3 112.45(16) . . ? C45 N6 C41 118.3(2) . . ? C45 N6 Mn1 123.7(2) . . ? C41 N6 Mn1 118.06(16) . . ? N1 C1 C2 122.1(3) . . ? C3 C2 C1 118.9(3) . . ? C2 C3 C4 119.2(3) . . ? C3 C4 C5 119.2(3) . . ? N1 C5 C4 121.3(3) . . ? N1 C5 C6 112.6(2) . . ? C4 C5 C6 126.1(2) . . ? O1 C6 C5 107.8(2) . . ? O1 C6 C7 108.64(19) . . ? C5 C6 C7 111.1(2) . . ? O1 C6 C12 111.6(2) . . ? C5 C6 C12 107.85(19) . . ? C7 C6 C12 109.8(2) . . ? N2 C7 C8 120.8(2) . . ? N2 C7 C6 115.6(2) . . ? C8 C7 C6 123.5(2) . . ? C9 C8 C7 120.1(3) . . ? C10 C9 C8 118.7(3) . . ? C9 C10 C11 118.7(3) . . ? N2 C11 C10 123.3(3) . . ? C13 C12 C17 117.9(2) . . ? C13 C12 C6 119.7(2) . . ? C17 C12 C6 122.3(2) . . ? C14 C13 C12 122.4(3) . . ? C15 C14 C13 119.0(3) . . ? C14 C15 C16 120.2(3) . . ? C15 C16 C17 121.5(3) . . ? C16 C17 C12 118.9(2) . . ? C16 C17 C54 117.5(2) . . ? C12 C17 C54 123.4(2) . . ? N3 C18 C19 123.2(3) . . ? C20 C19 C18 118.4(3) . . ? C19 C20 C21 118.9(2) . . ? C22 C21 C20 119.8(3) . . ? N3 C22 C21 120.9(2) . . ? N3 C22 C23 113.2(2) . . ? C21 C22 C23 125.8(2) . . ? O2 C23 C22 107.1(2) . . ? O2 C23 C24 109.0(2) . . ? C22 C23 C24 109.6(2) . . ? O2 C23 C29 111.88(19) . . ? C22 C23 C29 109.40(19) . . ? C24 C23 C29 109.7(2) . . ? N4 C24 C25 121.5(2) . . ? N4 C24 C23 114.3(2) . . ? C25 C24 C23 124.1(2) . . ? C26 C25 C24 120.4(3) . . ? C25 C26 C27 118.4(3) . . ? C26 C27 C28 118.6(3) . . ? N4 C28 C27 122.7(3) . . ? C30 C29 C34 117.5(2) . . ? C30 C29 C23 119.7(2) . . ? C34 C29 C23 122.7(2) . . ? C31 C30 C29 122.4(2) . . ? C32 C31 C30 120.3(2) . . ? C31 C32 C33 118.7(3) . . ? C32 C33 C34 122.3(2) . . ? C33 C34 C29 118.7(2) . . ? C33 C34 C56 116.6(2) . . ? C29 C34 C56 124.7(2) . . ? N5 C35 C36 123.4(2) . . ? C37 C36 C35 118.6(2) . . ? C36 C37 C38 118.5(3) . . ? C37 C38 C39 120.2(3) . . ? N5 C39 C38 121.7(2) . . ? N5 C39 C40 112.7(2) . . ? C38 C39 C40 125.5(2) . . ? O3 C40 C39 108.1(2) . . ? O3 C40 C41 108.0(2) . . ? C39 C40 C41 111.4(2) . . ? O3 C40 C46 112.4(2) . . ? C39 C40 C46 106.0(2) . . ? C41 C40 C46 111.0(2) . . ? N6 C41 C42 121.2(2) . . ? N6 C41 C40 114.3(2) . . ? C42 C41 C40 124.5(3) . . ? C43 C42 C41 119.1(3) . . ? C44 C43 C42 120.2(3) . . ? C43 C44 C45 118.6(3) . . ? N6 C45 C44 122.6(3) . . ? C47 C46 C51 117.7(3) . . ? C47 C46 C40 120.2(2) . . ? C51 C46 C40 121.9(2) . . ? C48 C47 C46 122.0(3) . . ? C47 C48 C49 120.2(3) . . ? C48 C49 C50 118.9(3) . . ? C49 C50 C51 121.8(3) . . ? C50 C51 C46 119.4(2) . . ? C50 C51 C52 117.2(3) . . ? C46 C51 C52 123.4(2) . . ? C57 C52 C53 118.4(2) . . ? C57 C52 C51 120.8(2) . . ? C53 C52 C51 120.7(2) . . ? C54 C53 C52 121.3(2) . . ? C55 C54 C53 118.8(2) . . ? C55 C54 C17 123.2(2) . . ? C53 C54 C17 117.8(2) . . ? C54 C55 C56 121.3(2) . . ? C55 C56 C57 118.6(2) . . ? C55 C56 C34 119.9(2) . . ? C57 C56 C34 121.4(2) . . ? C52 C57 C56 121.4(2) . . ? O4 C58 O5 126.7(3) . . ? O4 C58 C59 118.2(2) . . ? O5 C58 C59 115.1(2) . . ? O7 C60 O6 126.7(3) . . ? O7 C60 C61 117.4(3) . . ? O6 C60 C61 115.9(3) . . ? O8 C62 O9 123.3(5) . . ? O8 C62 C63 120.4(5) . . ? O9 C62 C63 116.3(4) . . ? Mn4 O10 Mn1 94.72(7) . . ? Mn4 O10 Mn2 135.09(9) . . ? Mn1 O10 Mn2 100.68(7) . . ? Mn4 O10 Mn3 119.30(8) . . ? Mn1 O10 Mn3 100.25(7) . . ? Mn2 O10 Mn3 99.15(7) . . ? Mn4 O11 Mn1 97.23(8) . . ? C62B O9B Mn4 134.8(16) . . ? O8B C62B O9B 109(3) . . ? O8B C62B C63B 125(2) . . ? O9B C62B C63B 119(3) . . ? N1B C5B O1B 123.7(5) . . ? C5B N1B C1B 126.9(5) . . ? C5B N1B C3B 120.1(4) . . ? C1B N1B C3B 113.0(4) . . ? C5C N1C C3C 120.2(3) . . ? C5C N1C C2C 122.6(3) . . ? C3C N1C C2C 117.2(3) . . ? O1C C5C N1C 124.7(4) . . ? N1D C1D O1D 107.9(5) . . ? C1D N1D C2D 115.7(4) . . ? C1D N1D C3D 122.2(4) . . ? C2D N1D C3D 121.8(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.62 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.532 _refine_diff_density_min -1.220 _refine_diff_density_rms 0.096 _database_code_depnum_ccdc_archive 'CCDC 842512' ####################################################################### # # 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_syncjsk78_b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H61 F3 Mn4 N10 O14 S' _chemical_formula_weight 1671.19 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 15.410(3) _cell_length_b 24.640(5) _cell_length_c 19.230(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.16(3) _cell_angle_gamma 90.00 _cell_volume 7110(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 385046 _cell_measurement_theta_min . _cell_measurement_theta_max . _exptl_crystal_description rhombus _exptl_crystal_colour brown _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3416 _exptl_absorpt_coefficient_mu 0.807 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min . _exptl_absorpt_correction_T_max . _exptl_absorpt_process_details 'XDS (Kabsh, 2010)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.72930 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'insertion device' _diffrn_radiation_monochromator 'liquid nitrogen-cooled double Si(111)' _diffrn_measurement_device_type 'SSRL BL 12-2' _diffrn_measurement_method 'fine sliced shutterless \f scans' _diffrn_measurement_device_details ; custom air bearing single axis goniometer ; _diffrn_detector 'pixel array detector' _diffrn_detector_type 'DECTIRS PILATUS 6M' _diffrn_detector_area_resol_mean 5.814 _diffrn_reflns_number 385046 _diffrn_reflns_av_R_equivalents 0.0748 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 31.33 _reflns_number_total 20713 _reflns_number_gt 17627 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BluIce (SSRL, 2001)' _computing_cell_refinement 'XDS (Kabsh, 2010)' _computing_data_reduction 'XDS (Kabsh, 2010)' _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. A molecule of benzene (the crystallization solvent) was found in the lattice and could not be satisfactorily modeled anisotropically. It was thus modeled isotropically and hydrogens were not calculated for this molecule. ; _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^)+(0.0700P)^2^+1.0000P] 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 20713 _refine_ls_number_parameters 955 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1739 _refine_ls_wR_factor_gt 0.1694 _refine_ls_goodness_of_fit_ref 1.640 _refine_ls_restrained_S_all 1.640 _refine_ls_shift/su_max 0.018 _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 C78 C 0.6563(4) 0.0762(2) 0.5996(2) 0.240(6) Uiso 1 1 d G . . C73 C 0.6434(3) 0.02497(19) 0.5688(3) 0.0916(14) Uiso 1 1 d G . . C74 C 0.6426(4) 0.0183(2) 0.4968(3) 0.235(6) Uiso 1 1 d G . . C75 C 0.6546(4) 0.0628(3) 0.4557(2) 0.136(2) Uiso 1 1 d G . . C76 C 0.6674(4) 0.1141(2) 0.4865(4) 0.188(4) Uiso 1 1 d G . . C77 C 0.6682(5) 0.12081(18) 0.5584(4) 0.165(3) Uiso 1 1 d G . . Mn1 Mn 0.24560(2) 0.685082(13) 0.576882(18) 0.02537(9) Uani 1 1 d . . . Mn2 Mn 0.41641(2) 0.724957(13) 0.643587(18) 0.02639(9) Uani 1 1 d . . . Mn3 Mn 0.32672(2) 0.638795(14) 0.712629(19) 0.02814(9) Uani 1 1 d . . . Mn4 Mn 0.27791(2) 0.753495(15) 0.71108(2) 0.03066(9) Uani 1 1 d . . . S5 S 0.01782(4) 0.63748(3) 0.76249(4) 0.04167(16) Uani 1 1 d . . . C2 C 0.38767(14) 0.52907(9) 0.58679(12) 0.0279(4) Uani 1 1 d . . . H2 H 0.3561 0.5028 0.6056 0.034 Uiso 1 1 calc R . . C5 C 0.48329(14) 0.60739(9) 0.52962(12) 0.0269(4) Uani 1 1 d . . . C1 C 0.35044(14) 0.55221(9) 0.52066(12) 0.0280(4) Uani 1 1 d . . . C3 C 0.47233(14) 0.54505(9) 0.62527(12) 0.0278(4) Uani 1 1 d . . . C19 C 0.53941(14) 0.63974(9) 0.49070(13) 0.0282(4) Uani 1 1 d . . . C6 C 0.39841(14) 0.59127(9) 0.49251(12) 0.0273(4) Uani 1 1 d . . . H6 H 0.3735 0.6068 0.4484 0.033 Uiso 1 1 calc R . . C24 C 0.57685(14) 0.69167(10) 0.50902(13) 0.0306(5) Uani 1 1 d . . . C4 C 0.51955(14) 0.58408(9) 0.59609(12) 0.0282(4) Uani 1 1 d . . . H4 H 0.5759 0.5947 0.6213 0.034 Uiso 1 1 calc R . . C8 C 0.27938(16) 0.47410(10) 0.45273(14) 0.0340(5) Uani 1 1 d . . . H8 H 0.3314 0.4556 0.4735 0.041 Uiso 1 1 calc R . . C7 C 0.26896(14) 0.52733(9) 0.47344(12) 0.0285(4) Uani 1 1 d . . . C13 C 0.52095(15) 0.51456(9) 0.69019(13) 0.0303(4) Uani 1 1 d . . . C20 C 0.55599(15) 0.61425(10) 0.43033(13) 0.0329(5) Uani 1 1 d . . . H20 H 0.5301 0.5806 0.4171 0.039 Uiso 1 1 calc R . . C12 C 0.18735(15) 0.55371(10) 0.44502(13) 0.0308(4) Uani 1 1 d . . . C18 C 0.49943(16) 0.51330(10) 0.75702(13) 0.0332(5) Uani 1 1 d . . . C14 C 0.59639(17) 0.48608(11) 0.68163(14) 0.0376(5) Uani 1 1 d . . . H14 H 0.6112 0.4868 0.6374 0.045 Uiso 1 1 calc R . . C22 C 0.64736(18) 0.68721(11) 0.40764(15) 0.0404(6) Uani 1 1 d . . . H22 H 0.6838 0.7030 0.3808 0.048 Uiso 1 1 calc R . . C11 C 0.12392(16) 0.52652(11) 0.39316(15) 0.0380(5) Uani 1 1 d . . . H11 H 0.0711 0.5443 0.3726 0.046 Uiso 1 1 calc R . . C9 C 0.21461(18) 0.44760(11) 0.40204(16) 0.0406(6) Uani 1 1 d . . . H9 H 0.2237 0.4121 0.3888 0.049 Uiso 1 1 calc R . . C23 C 0.63021(17) 0.71370(11) 0.46659(15) 0.0379(5) Uani 1 1 d . . . H23 H 0.6554 0.7477 0.4784 0.046 Uiso 1 1 calc R . . C10 C 0.13635(18) 0.47460(12) 0.37136(16) 0.0439(6) Uani 1 1 d . . . H10 H 0.0929 0.4578 0.3365 0.053 Uiso 1 1 calc R . . C17 C 0.5539(2) 0.48394(12) 0.81188(16) 0.0460(6) Uani 1 1 d . . . H17 H 0.5404 0.4833 0.8566 0.055 Uiso 1 1 calc R . . C21 C 0.60967(17) 0.63714(11) 0.38936(14) 0.0367(5) Uani 1 1 d . . . H21 H 0.6201 0.6188 0.3498 0.044 Uiso 1 1 calc R . . C15 C 0.6497(2) 0.45687(13) 0.73642(17) 0.0488(7) Uani 1 1 d . . . H15 H 0.6995 0.4384 0.7292 0.059 Uiso 1 1 calc R . . C16 C 0.6278(2) 0.45562(14) 0.80163(17) 0.0534(8) Uani 1 1 d . . . H16 H 0.6625 0.4358 0.8390 0.064 Uiso 1 1 calc R . . C49 C 0.68570(16) 0.68269(10) 0.66460(15) 0.0364(5) Uani 1 1 d . . . H49 H 0.7239 0.6851 0.6337 0.044 Uiso 1 1 calc R . . C48 C 0.59829(14) 0.70028(9) 0.64315(13) 0.0309(5) Uani 1 1 d . . . C26 C 0.21121(15) 0.65325(10) 0.42964(12) 0.0300(4) Uani 1 1 d . . . C25 C 0.16666(14) 0.61135(9) 0.46821(12) 0.0290(4) Uani 1 1 d . . . C36 C 0.42076(16) 0.54672(10) 0.77260(13) 0.0319(5) Uani 1 1 d . . . C31 C 0.06449(15) 0.61973(11) 0.45265(14) 0.0363(5) Uani 1 1 d . . . C38 C 0.30829(19) 0.46898(11) 0.73406(15) 0.0394(5) Uani 1 1 d . . . H38 H 0.3496 0.4433 0.7562 0.047 Uiso 1 1 calc R . . C42 C 0.42292(17) 0.54806(10) 0.85335(13) 0.0351(5) Uani 1 1 d . . . C37 C 0.33117(16) 0.52339(10) 0.73471(13) 0.0321(5) Uani 1 1 d . . . C47 C 0.55651(15) 0.72566(10) 0.57090(13) 0.0311(5) Uani 1 1 d . . . C53 C 0.59359(17) 0.78372(11) 0.57067(14) 0.0368(5) Uani 1 1 d . . . C50 C 0.71551(16) 0.66156(11) 0.73215(15) 0.0384(5) Uani 1 1 d . . . H50 H 0.7736 0.6489 0.7471 0.046 Uiso 1 1 calc R . . C29 C 0.30496(19) 0.72958(12) 0.37362(15) 0.0423(6) Uani 1 1 d . . . H29 H 0.3388 0.7551 0.3558 0.051 Uiso 1 1 calc R . . C30 C 0.30576(16) 0.72817(10) 0.44580(14) 0.0344(5) Uani 1 1 d . . . H30 H 0.3399 0.7533 0.4763 0.041 Uiso 1 1 calc R . . C41 C 0.18986(16) 0.54611(12) 0.66928(14) 0.0384(5) Uani 1 1 d . . . H41 H 0.1494 0.5723 0.6472 0.046 Uiso 1 1 calc R . . C27 C 0.20749(18) 0.65360(11) 0.35629(14) 0.0388(5) Uani 1 1 d . . . H27 H 0.1743 0.6276 0.3267 0.047 Uiso 1 1 calc R . . C52 C 0.57079(16) 0.67785(10) 0.75376(13) 0.0328(5) Uani 1 1 d . . . H52 H 0.5317 0.6767 0.7841 0.039 Uiso 1 1 calc R . . C51 C 0.65672(17) 0.65947(11) 0.77789(15) 0.0384(5) Uani 1 1 d . . . H51 H 0.6755 0.6458 0.8240 0.046 Uiso 1 1 calc R . . C40 C 0.16324(19) 0.49276(13) 0.66724(16) 0.0453(6) Uani 1 1 d . . . H40 H 0.1055 0.4831 0.6441 0.054 Uiso 1 1 calc R . . C39 C 0.22306(19) 0.45351(12) 0.69995(16) 0.0437(6) Uani 1 1 d . . . H39 H 0.2061 0.4172 0.6990 0.052 Uiso 1 1 calc R . . C54 C 0.5391(2) 0.82453(12) 0.53643(17) 0.0454(6) Uani 1 1 d . . . H54 H 0.4799 0.8175 0.5147 0.054 Uiso 1 1 calc R . . C32 C 0.01536(18) 0.58874(14) 0.49024(17) 0.0479(7) Uani 1 1 d . . . H32 H 0.0435 0.5635 0.5238 0.058 Uiso 1 1 calc R . . C28 C 0.2530(2) 0.69238(12) 0.32849(15) 0.0441(6) Uani 1 1 d . . . H28 H 0.2491 0.6938 0.2796 0.053 Uiso 1 1 calc R . . C56 C 0.6638(3) 0.88403(15) 0.5667(2) 0.0690(10) Uani 1 1 d . . . H56 H 0.6899 0.9180 0.5661 0.083 Uiso 1 1 calc R . . C34 C -0.1135(2) 0.63470(18) 0.4288(2) 0.0711(12) Uani 1 1 d . . . H34 H -0.1746 0.6408 0.4192 0.085 Uiso 1 1 calc R . . C45 C 0.4162(2) 0.55559(14) 0.99169(17) 0.0555(8) Uani 1 1 d . . . H45 H 0.4104 0.5581 1.0387 0.067 Uiso 1 1 calc R . . C43 C 0.4720(2) 0.58698(13) 0.89507(16) 0.0501(7) Uani 1 1 d . . . H43 H 0.5073 0.6108 0.8761 0.060 Uiso 1 1 calc R . . C55 C 0.5741(2) 0.87616(13) 0.53499(19) 0.0556(8) Uani 1 1 d . . . H55 H 0.5386 0.9048 0.5134 0.067 Uiso 1 1 calc R . . C44 C 0.4685(3) 0.59033(14) 0.96687(17) 0.0574(8) Uani 1 1 d . . . H44 H 0.5018 0.6162 0.9967 0.069 Uiso 1 1 calc R . . C57 C 0.7118(3) 0.84176(16) 0.5982(2) 0.0768(12) Uani 1 1 d . . . H57 H 0.7717 0.8476 0.6189 0.092 Uiso 1 1 calc R . . C33 C -0.0754(2) 0.59589(17) 0.4772(2) 0.0617(10) Uani 1 1 d . . . H33 H -0.1101 0.5749 0.5005 0.074 Uiso 1 1 calc R . . C35 C -0.0607(2) 0.66447(16) 0.3947(2) 0.0621(10) Uani 1 1 d . . . H35 H -0.0874 0.6914 0.3631 0.074 Uiso 1 1 calc R . . C46 C 0.3712(3) 0.51641(16) 0.94749(18) 0.0603(9) Uani 1 1 d . . . H46 H 0.3367 0.4917 0.9660 0.072 Uiso 1 1 calc R . . N6 N 0.25825(12) 0.69119(8) 0.47254(11) 0.0295(4) Uani 1 1 d . . . N2 N 0.54220(12) 0.69745(8) 0.68706(11) 0.0288(4) Uani 1 1 d . . . N4 N 0.27288(13) 0.56150(8) 0.70244(11) 0.0324(4) Uani 1 1 d . . . N3 N 0.37442(18) 0.51190(11) 0.87887(13) 0.0504(6) Uani 1 1 d . . . N5 N 0.02867(15) 0.65684(10) 0.40456(13) 0.0441(5) Uani 1 1 d . . . N1 N 0.67927(19) 0.79119(12) 0.60187(17) 0.0613(8) Uani 1 1 d . . . O1 O 0.35890(10) 0.65776(6) 0.61628(9) 0.0290(3) Uani 1 1 d . . . O2 O 0.38504(10) 0.71327(7) 0.73122(8) 0.0283(3) Uani 1 1 d . . . O3 O 0.22319(10) 0.67656(6) 0.66689(9) 0.0282(3) Uani 1 1 d . . . O4 O 0.30223(10) 0.75219(6) 0.60642(9) 0.0299(3) Uani 1 1 d . . . O6 O 0.46356(10) 0.72786(7) 0.56290(9) 0.0296(3) Uani 1 1 d . . . O5 O 0.42943(10) 0.59967(7) 0.74865(9) 0.0313(3) Uani 1 1 d . . . O7 O 0.19937(10) 0.61788(6) 0.54257(8) 0.0280(3) Uani 1 1 d . . . O8 O 0.46128(11) 0.79797(7) 0.67432(10) 0.0338(4) Uani 1 1 d . . . O11 O 0.26134(11) 0.73524(7) 0.81019(10) 0.0355(4) Uani 1 1 d . . . O10 O 0.29676(11) 0.64675(7) 0.81081(9) 0.0344(4) Uani 1 1 d . . . O9 O 0.35087(11) 0.82613(7) 0.72507(10) 0.0371(4) Uani 1 1 d . . . O12 O 0.03441(14) 0.62724(9) 0.69309(12) 0.0498(5) Uani 1 1 d . . . O13 O 0.06848(15) 0.68160(9) 0.80111(13) 0.0536(5) Uani 1 1 d . . . O14 O -0.07438(14) 0.63639(11) 0.76510(14) 0.0619(6) Uani 1 1 d . . . N7 N 0.12180(13) 0.72228(8) 0.54933(11) 0.0305(4) Uani 1 1 d . . . N8 N 0.05912(12) 0.70373(9) 0.58295(11) 0.0329(4) Uani 1 1 d . . . H8A H 0.0687 0.6788 0.6151 0.039 Uiso 1 1 calc R . . N10 N 0.09525(15) 0.77786(10) 0.72989(13) 0.0410(5) Uani 1 1 d . . . H10A H 0.0993 0.7493 0.7561 0.049 Uiso 1 1 calc R . . N9 N 0.15944(15) 0.79425(9) 0.69546(12) 0.0389(5) Uani 1 1 d . . . C60 C 0.27466(15) 0.68826(10) 0.83933(14) 0.0336(5) Uani 1 1 d . . . C70 C -0.01920(15) 0.72870(11) 0.56026(15) 0.0368(5) Uani 1 1 d . . . C67 C 0.12501(19) 0.78877(12) 0.45253(16) 0.0437(6) Uani 1 1 d . . . H67A H 0.1855 0.7971 0.4758 0.066 Uiso 1 1 calc R . . H67B H 0.0934 0.8218 0.4373 0.066 Uiso 1 1 calc R . . H67C H 0.1244 0.7661 0.4118 0.066 Uiso 1 1 calc R . . C68 C 0.08123(16) 0.75974(10) 0.50332(14) 0.0352(5) Uani 1 1 d . . . C58 C 0.42353(16) 0.83330(10) 0.70588(14) 0.0345(5) Uani 1 1 d . . . C63 C 0.1283(2) 0.83966(11) 0.66065(16) 0.0452(6) Uani 1 1 d . . . C71 C -0.10013(17) 0.71556(13) 0.58739(17) 0.0448(6) Uani 1 1 d . . . H71A H -0.1339 0.6878 0.5581 0.067 Uiso 1 1 calc R . . H71B H -0.1362 0.7475 0.5857 0.067 Uiso 1 1 calc R . . H71C H -0.0824 0.7029 0.6358 0.067 Uiso 1 1 calc R . . C69 C -0.00751(17) 0.76509(11) 0.50911(16) 0.0408(6) Uani 1 1 d . . . H69 H -0.0501 0.7887 0.4833 0.049 Uiso 1 1 calc R . . C72 C 0.0644(2) 0.57769(13) 0.81457(17) 0.0486(7) Uani 1 1 d . . . C59 C 0.4717(2) 0.88587(11) 0.72264(17) 0.0464(6) Uani 1 1 d . . . H59A H 0.5053 0.8855 0.7712 0.070 Uiso 1 1 calc R . . H59B H 0.4294 0.9151 0.7162 0.070 Uiso 1 1 calc R . . H59C H 0.5114 0.8909 0.6913 0.070 Uiso 1 1 calc R . . C62 C 0.1803(2) 0.86965(13) 0.61691(18) 0.0542(7) Uani 1 1 d . . . H62A H 0.2085 0.9005 0.6432 0.081 Uiso 1 1 calc R . . H62B H 0.1412 0.8817 0.5734 0.081 Uiso 1 1 calc R . . H62C H 0.2250 0.8462 0.6058 0.081 Uiso 1 1 calc R . . C65 C 0.0255(2) 0.81163(12) 0.71788(17) 0.0476(7) Uani 1 1 d . . . C66 C -0.0512(2) 0.80266(15) 0.7516(2) 0.0556(8) Uani 1 1 d . . . H66A H -0.0323 0.7810 0.7938 0.083 Uiso 1 1 calc R . . H66B H -0.0980 0.7842 0.7186 0.083 Uiso 1 1 calc R . . H66C H -0.0728 0.8370 0.7642 0.083 Uiso 1 1 calc R . . C61 C 0.26196(19) 0.68334(13) 0.91428(15) 0.0456(6) Uani 1 1 d . . . H61A H 0.1994 0.6818 0.9133 0.068 Uiso 1 1 calc R . . H61B H 0.2879 0.7143 0.9417 0.068 Uiso 1 1 calc R . . H61C H 0.2904 0.6509 0.9358 0.068 Uiso 1 1 calc R . . C64 C 0.0451(2) 0.85169(13) 0.67328(18) 0.0512(7) Uani 1 1 d . . . H64 H 0.0092 0.8811 0.6552 0.061 Uiso 1 1 calc R . . F1 F 0.15070(12) 0.57257(8) 0.81967(11) 0.0611(5) Uani 1 1 d . . . F3 F 0.05195(17) 0.58082(11) 0.88021(12) 0.0771(7) Uani 1 1 d . . . F2 F 0.02602(16) 0.53241(9) 0.78490(14) 0.0812(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.01697(15) 0.02843(16) 0.03153(18) -0.00076(12) 0.00725(13) 0.00132(11) Mn2 0.01801(16) 0.02805(16) 0.03495(18) -0.00201(13) 0.00986(13) -0.00036(11) Mn3 0.02003(16) 0.03262(18) 0.03323(18) 0.00252(13) 0.00907(14) 0.00484(12) Mn4 0.02385(17) 0.03309(18) 0.0376(2) -0.00491(14) 0.01238(15) -0.00289(13) S5 0.0265(3) 0.0456(3) 0.0544(4) 0.0059(3) 0.0124(3) -0.0022(2) C2 0.0211(10) 0.0292(10) 0.0355(11) -0.0021(8) 0.0104(9) 0.0007(8) C5 0.0189(9) 0.0284(10) 0.0357(11) -0.0023(8) 0.0107(8) 0.0006(7) C1 0.0202(9) 0.0305(10) 0.0342(11) -0.0047(8) 0.0083(8) 0.0018(8) C3 0.0226(10) 0.0294(10) 0.0323(11) -0.0023(8) 0.0083(8) 0.0024(8) C19 0.0163(9) 0.0348(11) 0.0348(11) 0.0014(9) 0.0087(8) 0.0017(8) C6 0.0203(9) 0.0310(10) 0.0317(10) -0.0010(8) 0.0083(8) 0.0030(8) C24 0.0196(10) 0.0365(11) 0.0378(12) -0.0003(9) 0.0110(9) -0.0012(8) C4 0.0192(9) 0.0314(10) 0.0348(11) -0.0045(8) 0.0077(8) 0.0015(8) C8 0.0257(11) 0.0344(11) 0.0431(13) -0.0009(10) 0.0102(10) 0.0006(9) C7 0.0200(9) 0.0329(11) 0.0341(11) -0.0032(9) 0.0095(8) -0.0033(8) C13 0.0228(10) 0.0287(10) 0.0389(12) 0.0008(9) 0.0061(9) 0.0020(8) C20 0.0259(11) 0.0353(11) 0.0393(12) 0.0002(9) 0.0112(9) 0.0014(9) C12 0.0221(10) 0.0351(11) 0.0364(12) -0.0023(9) 0.0094(9) -0.0022(8) C18 0.0270(11) 0.0344(11) 0.0393(12) 0.0025(9) 0.0097(10) 0.0049(9) C14 0.0300(12) 0.0423(13) 0.0418(13) 0.0006(10) 0.0110(10) 0.0066(10) C22 0.0338(13) 0.0456(14) 0.0483(15) 0.0060(11) 0.0231(11) 0.0008(10) C11 0.0240(11) 0.0424(13) 0.0442(13) -0.0050(11) 0.0007(10) 0.0012(9) C9 0.0334(13) 0.0360(12) 0.0534(15) -0.0114(11) 0.0119(11) -0.0024(10) C23 0.0312(12) 0.0382(12) 0.0493(14) 0.0003(11) 0.0191(11) -0.0048(10) C10 0.0310(12) 0.0455(14) 0.0513(15) -0.0151(12) 0.0014(11) -0.0055(10) C17 0.0445(15) 0.0514(16) 0.0446(14) 0.0148(12) 0.0157(12) 0.0182(12) C21 0.0312(12) 0.0434(13) 0.0397(13) 0.0007(10) 0.0169(10) 0.0036(10) C15 0.0374(14) 0.0552(17) 0.0553(17) 0.0070(13) 0.0141(13) 0.0209(12) C16 0.0445(16) 0.0642(19) 0.0526(17) 0.0179(14) 0.0130(14) 0.0264(14) C49 0.0211(10) 0.0431(13) 0.0482(14) -0.0090(11) 0.0144(10) -0.0034(9) C48 0.0211(10) 0.0325(11) 0.0407(12) -0.0053(9) 0.0101(9) -0.0045(8) C26 0.0206(10) 0.0364(11) 0.0336(11) 0.0003(9) 0.0073(9) 0.0067(8) C25 0.0186(9) 0.0350(11) 0.0339(11) -0.0042(9) 0.0070(8) 0.0005(8) C36 0.0284(11) 0.0334(11) 0.0353(11) 0.0048(9) 0.0103(9) 0.0053(9) C31 0.0197(10) 0.0467(13) 0.0414(13) -0.0129(11) 0.0045(9) 0.0023(9) C38 0.0397(14) 0.0376(13) 0.0430(14) 0.0018(10) 0.0140(11) 0.0011(10) C42 0.0315(12) 0.0364(12) 0.0375(12) 0.0017(10) 0.0084(10) 0.0079(9) C37 0.0295(11) 0.0362(11) 0.0330(11) 0.0015(9) 0.0125(9) 0.0038(9) C47 0.0220(10) 0.0338(11) 0.0399(12) -0.0024(9) 0.0118(9) -0.0036(8) C53 0.0335(12) 0.0381(12) 0.0428(13) -0.0042(10) 0.0170(11) -0.0078(10) C50 0.0194(10) 0.0457(14) 0.0491(14) -0.0072(11) 0.0058(10) 0.0026(9) C29 0.0392(14) 0.0470(14) 0.0444(14) 0.0090(11) 0.0176(12) 0.0008(11) C30 0.0250(11) 0.0385(12) 0.0405(13) 0.0053(10) 0.0092(10) 0.0016(9) C41 0.0254(11) 0.0511(14) 0.0392(13) -0.0006(11) 0.0085(10) 0.0015(10) C27 0.0344(13) 0.0466(14) 0.0364(12) -0.0023(11) 0.0103(10) 0.0047(10) C52 0.0270(11) 0.0343(11) 0.0380(12) -0.0042(9) 0.0091(10) 0.0009(9) C51 0.0282(12) 0.0452(14) 0.0407(13) -0.0018(11) 0.0053(10) 0.0026(10) C40 0.0320(13) 0.0545(16) 0.0503(15) -0.0053(13) 0.0108(12) -0.0058(11) C39 0.0418(15) 0.0414(14) 0.0504(15) -0.0009(12) 0.0157(12) -0.0066(11) C54 0.0384(14) 0.0408(14) 0.0606(17) 0.0026(12) 0.0191(13) -0.0055(11) C32 0.0254(12) 0.0698(19) 0.0503(16) -0.0167(14) 0.0119(11) -0.0103(12) C28 0.0439(15) 0.0553(16) 0.0361(13) 0.0033(11) 0.0150(11) 0.0056(12) C56 0.080(3) 0.0447(17) 0.078(2) -0.0007(16) 0.009(2) -0.0266(17) C34 0.0191(13) 0.107(3) 0.084(3) -0.050(2) 0.0056(15) 0.0045(16) C45 0.067(2) 0.0622(19) 0.0399(15) 0.0016(13) 0.0168(14) 0.0163(16) C43 0.0549(18) 0.0494(16) 0.0412(14) 0.0038(12) 0.0007(13) -0.0090(13) C55 0.064(2) 0.0397(15) 0.068(2) 0.0059(14) 0.0263(17) -0.0045(14) C44 0.076(2) 0.0489(17) 0.0418(15) -0.0052(13) 0.0019(15) 0.0018(16) C57 0.064(2) 0.058(2) 0.093(3) 0.009(2) -0.012(2) -0.0345(18) C33 0.0267(14) 0.091(3) 0.071(2) -0.031(2) 0.0191(15) -0.0126(15) C35 0.0317(15) 0.078(2) 0.066(2) -0.0252(18) -0.0102(14) 0.0226(15) C46 0.066(2) 0.074(2) 0.0447(16) 0.0061(15) 0.0214(15) -0.0087(17) N6 0.0204(8) 0.0331(9) 0.0353(10) 0.0013(8) 0.0068(7) 0.0030(7) N2 0.0204(8) 0.0313(9) 0.0361(10) -0.0033(7) 0.0093(7) -0.0011(7) N4 0.0258(9) 0.0379(10) 0.0355(10) -0.0004(8) 0.0112(8) 0.0020(8) N3 0.0565(15) 0.0562(15) 0.0435(13) 0.0041(11) 0.0218(12) -0.0089(12) N5 0.0269(10) 0.0531(13) 0.0479(13) -0.0101(10) -0.0004(9) 0.0106(9) N1 0.0479(15) 0.0495(15) 0.080(2) 0.0044(14) 0.0000(14) -0.0233(12) O1 0.0186(7) 0.0308(8) 0.0389(8) -0.0059(6) 0.0090(6) 0.0005(6) O2 0.0194(7) 0.0332(8) 0.0332(8) -0.0025(6) 0.0078(6) 0.0003(6) O3 0.0192(7) 0.0332(8) 0.0339(8) 0.0006(6) 0.0099(6) 0.0027(6) O4 0.0202(7) 0.0288(8) 0.0405(9) 0.0002(6) 0.0065(7) 0.0010(6) O6 0.0194(7) 0.0350(8) 0.0360(8) -0.0010(6) 0.0097(6) 0.0002(6) O5 0.0232(7) 0.0337(8) 0.0372(8) 0.0037(7) 0.0077(7) 0.0050(6) O7 0.0196(7) 0.0315(8) 0.0331(8) -0.0023(6) 0.0063(6) -0.0014(6) O8 0.0253(8) 0.0349(8) 0.0431(9) -0.0027(7) 0.0120(7) -0.0036(6) O11 0.0280(8) 0.0385(9) 0.0424(9) -0.0046(7) 0.0132(7) 0.0039(7) O10 0.0285(8) 0.0366(9) 0.0395(9) -0.0001(7) 0.0105(7) -0.0005(7) O9 0.0279(8) 0.0342(8) 0.0512(10) -0.0080(7) 0.0132(8) -0.0004(7) O12 0.0397(11) 0.0552(12) 0.0555(12) 0.0089(10) 0.0133(9) 0.0011(9) O13 0.0455(12) 0.0482(12) 0.0680(14) 0.0003(10) 0.0146(11) -0.0025(9) O14 0.0278(10) 0.0820(17) 0.0791(16) 0.0159(13) 0.0187(10) 0.0008(10) N7 0.0219(9) 0.0350(10) 0.0358(10) 0.0011(8) 0.0094(8) 0.0024(7) N8 0.0206(9) 0.0385(10) 0.0408(11) 0.0030(8) 0.0097(8) 0.0036(7) N10 0.0360(11) 0.0416(12) 0.0465(12) -0.0039(9) 0.0119(10) -0.0009(9) N9 0.0358(11) 0.0372(11) 0.0449(12) -0.0018(9) 0.0117(9) -0.0029(9) C60 0.0223(10) 0.0406(12) 0.0393(12) -0.0014(10) 0.0098(9) 0.0004(9) C70 0.0195(10) 0.0430(13) 0.0479(14) -0.0032(11) 0.0079(10) 0.0065(9) C67 0.0411(14) 0.0414(13) 0.0518(15) 0.0107(12) 0.0170(12) 0.0116(11) C68 0.0271(11) 0.0385(12) 0.0405(13) -0.0008(10) 0.0086(10) 0.0060(9) C58 0.0263(11) 0.0343(11) 0.0426(13) -0.0019(10) 0.0074(10) 0.0003(9) C63 0.0461(15) 0.0385(13) 0.0487(15) -0.0042(11) 0.0062(13) -0.0006(11) C71 0.0247(12) 0.0538(16) 0.0588(17) -0.0004(13) 0.0151(12) 0.0040(11) C69 0.0266(12) 0.0456(14) 0.0492(15) 0.0020(11) 0.0063(11) 0.0123(10) C72 0.0409(15) 0.0516(16) 0.0532(17) 0.0062(13) 0.0106(13) -0.0027(12) C59 0.0468(15) 0.0349(13) 0.0594(17) -0.0070(12) 0.0160(13) -0.0091(11) C62 0.061(2) 0.0431(15) 0.0577(18) 0.0063(13) 0.0123(15) -0.0004(14) C65 0.0383(14) 0.0485(15) 0.0539(17) -0.0098(13) 0.0061(13) 0.0025(12) C66 0.0352(15) 0.065(2) 0.068(2) -0.0082(16) 0.0147(14) 0.0044(13) C61 0.0372(14) 0.0613(18) 0.0429(14) 0.0013(12) 0.0186(12) 0.0065(12) C64 0.0500(17) 0.0437(15) 0.0570(18) -0.0026(13) 0.0062(14) 0.0061(12) F1 0.0429(10) 0.0667(12) 0.0725(12) 0.0116(10) 0.0103(9) 0.0109(9) F3 0.0804(15) 0.0955(17) 0.0599(12) 0.0214(12) 0.0255(11) 0.0159(13) F2 0.0815(16) 0.0492(11) 0.0953(17) 0.0128(11) -0.0163(13) -0.0150(10) _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 C78 C73 1.3900 . ? C78 C77 1.3900 . ? C73 C74 1.3900 . ? C74 C75 1.3900 . ? C75 C76 1.3900 . ? C76 C77 1.3900 . ? Mn1 O3 1.8524(17) . ? Mn1 O1 1.8636(16) . ? Mn1 O7 1.8630(16) . ? Mn1 O4 1.8955(16) . ? Mn1 N6 2.065(2) . ? Mn1 N7 2.074(2) . ? Mn1 Mn2 2.8287(9) . ? Mn1 Mn3 2.8622(9) . ? Mn1 Mn4 3.0273(7) . ? Mn2 O6 1.8585(17) . ? Mn2 O4 1.8666(17) . ? Mn2 O2 1.8780(17) . ? Mn2 O1 1.8949(16) . ? Mn2 O8 1.9694(17) . ? Mn2 N2 2.044(2) . ? Mn2 Mn4 2.8276(8) . ? Mn2 Mn3 3.0026(7) . ? Mn3 O5 1.8480(16) . ? Mn3 O3 1.8831(16) . ? Mn3 O2 2.0388(17) . ? Mn3 O10 2.0527(18) . ? Mn3 N4 2.069(2) . ? Mn3 O1 2.0773(17) . ? Mn3 Mn4 2.9230(7) . ? Mn4 O2 1.8886(16) . ? Mn4 O11 2.0300(19) . ? Mn4 N9 2.045(2) . ? Mn4 O9 2.0981(18) . ? Mn4 O4 2.1299(18) . ? Mn4 O3 2.1681(17) . ? S5 O12 1.437(2) . ? S5 O14 1.433(2) . ? S5 O13 1.442(2) . ? S5 C72 1.833(3) . ? C2 C1 1.393(3) . ? C2 C3 1.402(3) . ? C5 C4 1.397(3) . ? C5 C6 1.398(3) . ? C5 C19 1.496(3) . ? C1 C6 1.396(3) . ? C1 C7 1.503(3) . ? C3 C4 1.398(3) . ? C3 C13 1.503(3) . ? C19 C20 1.394(3) . ? C19 C24 1.415(3) . ? C24 C23 1.394(3) . ? C24 C47 1.544(3) . ? C8 C9 1.389(4) . ? C8 C7 1.391(3) . ? C7 C12 1.411(3) . ? C13 C18 1.399(3) . ? C13 C14 1.399(3) . ? C20 C21 1.386(3) . ? C12 C11 1.398(3) . ? C12 C25 1.544(3) . ? C18 C17 1.392(4) . ? C18 C36 1.550(3) . ? C14 C15 1.382(4) . ? C22 C21 1.375(4) . ? C22 C23 1.385(4) . ? C11 C10 1.373(4) . ? C9 C10 1.386(4) . ? C17 C16 1.388(4) . ? C15 C16 1.371(4) . ? C49 C50 1.378(4) . ? C49 C48 1.385(3) . ? C48 N2 1.341(3) . ? C48 C47 1.526(4) . ? C26 N6 1.345(3) . ? C26 C27 1.399(3) . ? C26 C25 1.523(3) . ? C25 O7 1.413(3) . ? C25 C31 1.548(3) . ? C36 O5 1.400(3) . ? C36 C37 1.520(4) . ? C36 C42 1.546(3) . ? C31 N5 1.328(4) . ? C31 C32 1.388(4) . ? C38 C39 1.381(4) . ? C38 C37 1.386(4) . ? C42 N3 1.327(4) . ? C42 C43 1.364(4) . ? C37 N4 1.349(3) . ? C47 O6 1.406(3) . ? C47 C53 1.541(3) . ? C53 N1 1.333(4) . ? C53 C54 1.377(4) . ? C50 C51 1.400(4) . ? C29 C30 1.386(4) . ? C29 C28 1.385(4) . ? C30 N6 1.342(3) . ? C41 N4 1.348(3) . ? C41 C40 1.375(4) . ? C27 C28 1.364(4) . ? C52 N2 1.347(3) . ? C52 C51 1.376(3) . ? C40 C39 1.384(4) . ? C54 C55 1.384(4) . ? C32 C33 1.376(4) . ? C56 C57 1.340(6) . ? C56 C55 1.391(5) . ? C34 C33 1.369(6) . ? C34 C35 1.369(6) . ? C45 C44 1.336(5) . ? C45 C46 1.366(5) . ? C43 C44 1.397(4) . ? C57 N1 1.351(4) . ? C35 N5 1.359(4) . ? C46 N3 1.337(4) . ? O8 C58 1.275(3) . ? O11 C60 1.282(3) . ? O10 C60 1.244(3) . ? O9 C58 1.269(3) . ? N7 C68 1.332(3) . ? N7 N8 1.358(3) . ? N8 C70 1.336(3) . ? N10 C65 1.337(4) . ? N10 N9 1.370(3) . ? N9 C63 1.336(4) . ? C60 C61 1.503(4) . ? C70 C69 1.373(4) . ? C70 C71 1.493(4) . ? C67 C68 1.490(4) . ? C68 C69 1.403(3) . ? C58 C59 1.491(4) . ? C63 C64 1.390(5) . ? C63 C62 1.485(4) . ? C72 F3 1.321(4) . ? C72 F1 1.317(4) . ? C72 F2 1.329(4) . ? C65 C64 1.385(5) . ? C65 C66 1.489(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C73 C78 C77 120.0 . . ? C74 C73 C78 120.0 . . ? C75 C74 C73 120.0 . . ? C76 C75 C74 120.0 . . ? C77 C76 C75 120.0 . . ? C76 C77 C78 120.0 . . ? O3 Mn1 O1 86.32(7) . . ? O3 Mn1 O7 95.31(7) . . ? O1 Mn1 O7 94.03(7) . . ? O3 Mn1 O4 89.43(8) . . ? O1 Mn1 O4 82.45(7) . . ? O7 Mn1 O4 173.92(7) . . ? O3 Mn1 N6 174.29(7) . . ? O1 Mn1 N6 97.72(8) . . ? O7 Mn1 N6 80.43(8) . . ? O4 Mn1 N6 95.09(8) . . ? O3 Mn1 N7 86.13(8) . . ? O1 Mn1 N7 170.32(8) . . ? O7 Mn1 N7 92.69(8) . . ? O4 Mn1 N7 91.43(7) . . ? N6 Mn1 N7 90.25(8) . . ? O3 Mn1 Mn2 88.16(6) . . ? O1 Mn1 Mn2 41.60(5) . . ? O7 Mn1 Mn2 135.29(5) . . ? O4 Mn1 Mn2 40.86(5) . . ? N6 Mn1 Mn2 97.55(6) . . ? N7 Mn1 Mn2 132.01(6) . . ? O3 Mn1 Mn3 40.38(5) . . ? O1 Mn1 Mn3 46.45(6) . . ? O7 Mn1 Mn3 91.22(5) . . ? O4 Mn1 Mn3 89.92(6) . . ? N6 Mn1 Mn3 142.84(5) . . ? N7 Mn1 Mn3 126.48(6) . . ? Mn2 Mn1 Mn3 63.69(3) . . ? O3 Mn1 Mn4 45.26(5) . . ? O1 Mn1 Mn4 84.12(6) . . ? O7 Mn1 Mn4 140.56(5) . . ? O4 Mn1 Mn4 44.25(5) . . ? N6 Mn1 Mn4 138.95(6) . . ? N7 Mn1 Mn4 86.26(6) . . ? Mn2 Mn1 Mn4 57.62(2) . . ? Mn3 Mn1 Mn4 59.43(2) . . ? O6 Mn2 O4 100.37(8) . . ? O6 Mn2 O2 169.88(7) . . ? O4 Mn2 O2 89.20(8) . . ? O6 Mn2 O1 92.83(7) . . ? O4 Mn2 O1 82.38(7) . . ? O2 Mn2 O1 85.12(7) . . ? O6 Mn2 O8 92.18(7) . . ? O4 Mn2 O8 91.29(7) . . ? O2 Mn2 O8 90.88(7) . . ? O1 Mn2 O8 172.55(7) . . ? O6 Mn2 N2 80.77(8) . . ? O4 Mn2 N2 177.84(8) . . ? O2 Mn2 N2 89.77(8) . . ? O1 Mn2 N2 99.43(7) . . ? O8 Mn2 N2 86.82(7) . . ? O6 Mn2 Mn4 148.55(5) . . ? O4 Mn2 Mn4 48.87(6) . . ? O2 Mn2 Mn4 41.49(5) . . ? O1 Mn2 Mn4 89.44(5) . . ? O8 Mn2 Mn4 83.41(5) . . ? N2 Mn2 Mn4 129.74(6) . . ? O6 Mn2 Mn1 97.76(6) . . ? O4 Mn2 Mn1 41.63(5) . . ? O2 Mn2 Mn1 87.17(5) . . ? O1 Mn2 Mn1 40.77(5) . . ? O8 Mn2 Mn1 132.87(5) . . ? N2 Mn2 Mn1 140.19(6) . . ? Mn4 Mn2 Mn1 64.716(18) . . ? O6 Mn2 Mn3 134.68(5) . . ? O4 Mn2 Mn3 86.27(5) . . ? O2 Mn2 Mn3 41.96(5) . . ? O1 Mn2 Mn3 43.23(5) . . ? O8 Mn2 Mn3 132.75(5) . . ? N2 Mn2 Mn3 94.23(6) . . ? Mn4 Mn2 Mn3 60.091(18) . . ? Mn1 Mn2 Mn3 58.700(18) . . ? O5 Mn3 O3 174.34(7) . . ? O5 Mn3 O2 95.63(7) . . ? O3 Mn3 O2 85.98(7) . . ? O5 Mn3 O10 93.32(8) . . ? O3 Mn3 O10 92.20(7) . . ? O2 Mn3 O10 86.29(7) . . ? O5 Mn3 N4 81.14(8) . . ? O3 Mn3 N4 97.57(8) . . ? O2 Mn3 N4 175.19(8) . . ? O10 Mn3 N4 90.33(8) . . ? O5 Mn3 O1 95.38(7) . . ? O3 Mn3 O1 79.70(7) . . ? O2 Mn3 O1 76.63(6) . . ? O10 Mn3 O1 161.49(7) . . ? N4 Mn3 O1 107.14(7) . . ? O5 Mn3 Mn1 135.13(6) . . ? O3 Mn3 Mn1 39.59(5) . . ? O2 Mn3 Mn1 83.39(5) . . ? O10 Mn3 Mn1 131.14(5) . . ? N4 Mn3 Mn1 101.42(6) . . ? O1 Mn3 Mn1 40.56(4) . . ? O5 Mn3 Mn4 134.81(6) . . ? O3 Mn3 Mn4 47.84(5) . . ? O2 Mn3 Mn4 39.97(4) . . ? O10 Mn3 Mn4 78.80(5) . . ? N4 Mn3 Mn4 142.41(6) . . ? O1 Mn3 Mn4 83.49(5) . . ? Mn1 Mn3 Mn4 63.095(14) . . ? O5 Mn3 Mn2 95.36(5) . . ? O3 Mn3 Mn2 82.55(5) . . ? O2 Mn3 Mn2 38.02(5) . . ? O10 Mn3 Mn2 124.18(5) . . ? N4 Mn3 Mn2 145.50(6) . . ? O1 Mn3 Mn2 38.67(4) . . ? Mn1 Mn3 Mn2 57.615(19) . . ? Mn4 Mn3 Mn2 56.985(17) . . ? O2 Mn4 O11 88.98(7) . . ? O2 Mn4 N9 175.81(8) . . ? O11 Mn4 N9 87.01(8) . . ? O2 Mn4 O9 90.20(7) . . ? O11 Mn4 O9 104.29(8) . . ? N9 Mn4 O9 91.97(8) . . ? O2 Mn4 O4 81.50(7) . . ? O11 Mn4 O4 166.08(7) . . ? N9 Mn4 O4 102.23(8) . . ? O9 Mn4 O4 85.96(7) . . ? O2 Mn4 O3 82.26(7) . . ? O11 Mn4 O3 93.06(7) . . ? N9 Mn4 O3 96.73(8) . . ? O9 Mn4 O3 160.97(7) . . ? O4 Mn4 O3 75.69(6) . . ? O2 Mn4 Mn2 41.21(5) . . ? O11 Mn4 Mn2 130.18(5) . . ? N9 Mn4 Mn2 142.81(7) . . ? O9 Mn4 Mn2 80.36(5) . . ? O4 Mn4 Mn2 41.31(5) . . ? O3 Mn4 Mn2 82.50(4) . . ? O2 Mn4 Mn3 43.91(5) . . ? O11 Mn4 Mn3 82.14(5) . . ? N9 Mn4 Mn3 134.05(6) . . ? O9 Mn4 Mn3 133.97(5) . . ? O4 Mn4 Mn3 83.96(4) . . ? O3 Mn4 Mn3 40.08(4) . . ? Mn2 Mn4 Mn3 62.925(12) . . ? O2 Mn4 Mn1 81.31(6) . . ? O11 Mn4 Mn1 130.20(5) . . ? N9 Mn4 Mn1 100.38(7) . . ? O9 Mn4 Mn1 124.31(6) . . ? O4 Mn4 Mn1 38.39(4) . . ? O3 Mn4 Mn1 37.36(4) . . ? Mn2 Mn4 Mn1 57.66(2) . . ? Mn3 Mn4 Mn1 57.471(17) . . ? O12 S5 O14 114.61(15) . . ? O12 S5 O13 114.88(14) . . ? O14 S5 O13 114.90(15) . . ? O12 S5 C72 103.64(14) . . ? O14 S5 C72 103.52(14) . . ? O13 S5 C72 103.05(14) . . ? C1 C2 C3 120.5(2) . . ? C4 C5 C6 118.9(2) . . ? C4 C5 C19 121.37(19) . . ? C6 C5 C19 118.4(2) . . ? C2 C1 C6 119.5(2) . . ? C2 C1 C7 119.9(2) . . ? C6 C1 C7 119.4(2) . . ? C2 C3 C4 119.2(2) . . ? C2 C3 C13 121.7(2) . . ? C4 C3 C13 118.1(2) . . ? C20 C19 C24 118.2(2) . . ? C20 C19 C5 114.4(2) . . ? C24 C19 C5 127.4(2) . . ? C1 C6 C5 121.0(2) . . ? C23 C24 C19 117.9(2) . . ? C23 C24 C47 119.4(2) . . ? C19 C24 C47 122.64(19) . . ? C5 C4 C3 120.9(2) . . ? C9 C8 C7 122.2(2) . . ? C8 C7 C12 118.3(2) . . ? C8 C7 C1 115.0(2) . . ? C12 C7 C1 126.5(2) . . ? C18 C13 C14 118.3(2) . . ? C18 C13 C3 126.6(2) . . ? C14 C13 C3 115.0(2) . . ? C21 C20 C19 122.5(2) . . ? C11 C12 C7 118.2(2) . . ? C11 C12 C25 119.3(2) . . ? C7 C12 C25 122.5(2) . . ? C17 C18 C13 118.7(2) . . ? C17 C18 C36 119.5(2) . . ? C13 C18 C36 121.7(2) . . ? C15 C14 C13 122.5(3) . . ? C21 C22 C23 119.0(2) . . ? C10 C11 C12 122.7(2) . . ? C8 C9 C10 119.3(2) . . ? C22 C23 C24 122.9(2) . . ? C11 C10 C9 119.1(2) . . ? C16 C17 C18 121.8(3) . . ? C22 C21 C20 119.5(2) . . ? C16 C15 C14 118.8(2) . . ? C15 C16 C17 119.9(3) . . ? C50 C49 C48 119.5(2) . . ? N2 C48 C49 121.3(2) . . ? N2 C48 C47 113.31(19) . . ? C49 C48 C47 125.4(2) . . ? N6 C26 C27 120.5(2) . . ? N6 C26 C25 114.4(2) . . ? C27 C26 C25 125.2(2) . . ? O7 C25 C26 108.61(18) . . ? O7 C25 C12 110.34(19) . . ? C26 C25 C12 109.73(18) . . ? O7 C25 C31 107.05(18) . . ? C26 C25 C31 111.5(2) . . ? C12 C25 C31 109.55(19) . . ? O5 C36 C37 109.82(19) . . ? O5 C36 C18 107.10(18) . . ? C37 C36 C18 111.8(2) . . ? O5 C36 C42 109.2(2) . . ? C37 C36 C42 107.4(2) . . ? C18 C36 C42 111.50(19) . . ? N5 C31 C32 123.5(2) . . ? N5 C31 C25 118.0(2) . . ? C32 C31 C25 118.5(2) . . ? C39 C38 C37 118.9(3) . . ? N3 C42 C43 122.6(3) . . ? N3 C42 C36 118.2(2) . . ? C43 C42 C36 119.2(2) . . ? N4 C37 C38 121.9(2) . . ? N4 C37 C36 113.2(2) . . ? C38 C37 C36 124.9(2) . . ? O6 C47 C48 108.88(18) . . ? O6 C47 C53 109.45(19) . . ? C48 C47 C53 107.6(2) . . ? O6 C47 C24 108.48(19) . . ? C48 C47 C24 111.20(19) . . ? C53 C47 C24 111.15(19) . . ? N1 C53 C54 123.2(3) . . ? N1 C53 C47 117.2(2) . . ? C54 C53 C47 119.5(2) . . ? C49 C50 C51 118.8(2) . . ? C30 C29 C28 118.9(3) . . ? N6 C30 C29 121.3(2) . . ? N4 C41 C40 121.8(3) . . ? C28 C27 C26 119.5(3) . . ? N2 C52 C51 121.3(2) . . ? C52 C51 C50 119.1(3) . . ? C39 C40 C41 119.4(3) . . ? C38 C39 C40 119.1(3) . . ? C53 C54 C55 118.9(3) . . ? C33 C32 C31 119.1(3) . . ? C27 C28 C29 119.6(3) . . ? C57 C56 C55 118.7(3) . . ? C33 C34 C35 119.4(3) . . ? C44 C45 C46 119.5(3) . . ? C42 C43 C44 118.8(3) . . ? C54 C55 C56 118.1(3) . . ? C45 C44 C43 118.6(3) . . ? C56 C57 N1 124.6(4) . . ? C34 C33 C32 118.3(3) . . ? N5 C35 C34 123.6(4) . . ? N3 C46 C45 123.0(3) . . ? C30 N6 C26 120.1(2) . . ? C30 N6 Mn1 127.02(17) . . ? C26 N6 Mn1 112.85(15) . . ? C48 N2 C52 120.0(2) . . ? C48 N2 Mn2 114.37(16) . . ? C52 N2 Mn2 125.62(15) . . ? C41 N4 C37 118.9(2) . . ? C41 N4 Mn3 128.39(18) . . ? C37 N4 Mn3 112.74(16) . . ? C42 N3 C46 117.4(3) . . ? C31 N5 C35 116.1(3) . . ? C53 N1 C57 116.4(3) . . ? Mn1 O1 Mn2 97.63(7) . . ? Mn1 O1 Mn3 92.99(7) . . ? Mn2 O1 Mn3 98.10(7) . . ? Mn2 O2 Mn4 97.30(8) . . ? Mn2 O2 Mn3 100.02(7) . . ? Mn4 O2 Mn3 96.12(7) . . ? Mn1 O3 Mn3 100.03(7) . . ? Mn1 O3 Mn4 97.38(7) . . ? Mn3 O3 Mn4 92.09(7) . . ? Mn2 O4 Mn1 97.51(7) . . ? Mn2 O4 Mn4 89.82(7) . . ? Mn1 O4 Mn4 97.37(7) . . ? C47 O6 Mn2 119.29(15) . . ? C36 O5 Mn3 118.15(14) . . ? C25 O7 Mn1 118.63(14) . . ? C58 O8 Mn2 126.84(15) . . ? C60 O11 Mn4 124.66(16) . . ? C60 O10 Mn3 128.71(17) . . ? C58 O9 Mn4 124.34(16) . . ? C68 N7 N8 105.81(19) . . ? C68 N7 Mn1 137.86(17) . . ? N8 N7 Mn1 116.25(15) . . ? C70 N8 N7 112.1(2) . . ? C65 N10 N9 111.9(2) . . ? C63 N9 N10 105.8(2) . . ? C63 N9 Mn4 133.8(2) . . ? N10 N9 Mn4 120.19(17) . . ? O10 C60 O11 125.6(2) . . ? O10 C60 C61 117.7(2) . . ? O11 C60 C61 116.7(2) . . ? N8 C70 C69 106.2(2) . . ? N8 C70 C71 123.4(2) . . ? C69 C70 C71 130.4(2) . . ? N7 C68 C69 109.3(2) . . ? N7 C68 C67 123.6(2) . . ? C69 C68 C67 127.0(2) . . ? O9 C58 O8 124.9(2) . . ? O9 C58 C59 119.1(2) . . ? O8 C58 C59 115.9(2) . . ? N9 C63 C64 109.4(3) . . ? N9 C63 C62 121.5(3) . . ? C64 C63 C62 129.2(3) . . ? C70 C69 C68 106.5(2) . . ? F3 C72 F1 107.3(3) . . ? F3 C72 F2 108.2(3) . . ? F1 C72 F2 107.1(3) . . ? F3 C72 S5 110.5(2) . . ? F1 C72 S5 112.4(2) . . ? F2 C72 S5 111.1(2) . . ? N10 C65 C64 105.7(3) . . ? N10 C65 C66 121.3(3) . . ? C64 C65 C66 133.0(3) . . ? C63 C64 C65 107.2(3) . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 31.33 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.946 _refine_diff_density_min -0.816 _refine_diff_density_rms 0.090 _database_code_depnum_ccdc_archive 'CCDC 938750'