# Electronic Supplementary Material (ESI) for CrystEngComm # 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_test_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C85 H58 Mn7 N13 O50' _chemical_formula_weight 2446.02 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.1955(19) _cell_length_b 14.1957(10) _cell_length_c 33.3812(17) _cell_angle_alpha 90.00 _cell_angle_beta 135.955(3) _cell_angle_gamma 90.00 _cell_volume 9288.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5197 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 24.20 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.749 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4936 _exptl_absorpt_coefficient_mu 1.035 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7007 _exptl_absorpt_correction_T_max 0.8437 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25610 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9130 _reflns_number_gt 6884 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0702P)^2^+6.9242P] 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 9130 _refine_ls_number_parameters 742 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.0617 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1286 _refine_ls_wR_factor_gt 0.1133 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0286(5) 0.0715(8) 0.1677(5) 0.066(3) Uani 0.808(5) 1 d PU A 1 H1 H -0.0117 0.0383 0.1391 0.079 Uiso 0.808(5) 1 calc PR A 1 C2 C 0.0433(5) 0.1032(8) 0.2143(4) 0.092(4) Uani 0.808(5) 1 d PU A 1 H2 H 0.0135 0.0917 0.2173 0.110 Uiso 0.808(5) 1 calc PR A 1 C3 C 0.1027(7) 0.1524(10) 0.2565(6) 0.114(5) Uani 0.808(5) 1 d PU A 1 H3 H 0.1131 0.1750 0.2883 0.136 Uiso 0.808(5) 1 calc PR A 1 C4 C 0.1456(5) 0.1680(8) 0.2521(4) 0.093(4) Uani 0.808(5) 1 d PU A 1 H4 H 0.1859 0.2008 0.2811 0.112 Uiso 0.808(5) 1 calc PR A 1 C5 C 0.1305(5) 0.1355(6) 0.2047(3) 0.050(2) Uani 0.808(5) 1 d PU A 1 C6 C 0.1733(6) 0.1480(12) 0.1948(7) 0.057(3) Uani 0.808(5) 1 d PU A 1 C7 C 0.2430(4) 0.1663(7) 0.2405(4) 0.078(3) Uani 0.808(5) 1 d PU A 1 H7 H 0.2623 0.1729 0.2775 0.093 Uiso 0.808(5) 1 calc PR A 1 C8 C 0.2825(6) 0.1745(8) 0.2320(5) 0.090(4) Uani 0.808(5) 1 d PU A 1 H8 H 0.3292 0.1853 0.2626 0.108 Uiso 0.808(5) 1 calc PR A 1 C9 C 0.2516(5) 0.1664(7) 0.1761(4) 0.075(3) Uani 0.808(5) 1 d PU A 1 H9 H 0.2771 0.1731 0.1683 0.090 Uiso 0.808(5) 1 calc PR A 1 C10 C 0.1840(7) 0.1486(11) 0.1330(4) 0.056(3) Uani 0.808(5) 1 d PU A 1 H10 H 0.1642 0.1431 0.0958 0.067 Uiso 0.808(5) 1 calc PR A 1 C11 C 0.11415(19) 0.4619(3) 0.20578(16) 0.0419(9) Uani 1 1 d . . . H11 H 0.0683 0.4789 0.1783 0.050 Uiso 1 1 calc R . . C12 C 0.1465(2) 0.4466(3) 0.26126(17) 0.0514(11) Uani 1 1 d . . . H12 H 0.1228 0.4523 0.2709 0.062 Uiso 1 1 calc R . . C13 C 0.2142(2) 0.4230(3) 0.30228(16) 0.0496(11) Uani 1 1 d . . . H13 H 0.2373 0.4128 0.3403 0.059 Uiso 1 1 calc R . . C14 C 0.24721(19) 0.4146(3) 0.28617(15) 0.0416(9) Uani 1 1 d . . . H14 H 0.2932 0.3988 0.3133 0.050 Uiso 1 1 calc R . . C15 C 0.21154(17) 0.4298(2) 0.22931(14) 0.0286(7) Uani 1 1 d . . . C16 C 0.24445(17) 0.4206(2) 0.20949(14) 0.0286(7) Uani 1 1 d . . . C17 C 0.31347(18) 0.4056(3) 0.24674(17) 0.0395(9) Uani 1 1 d . . . H17 H 0.3419 0.4026 0.2863 0.047 Uiso 1 1 calc R . . C18 C 0.3399(2) 0.3950(3) 0.22504(19) 0.0489(11) Uani 1 1 d . . . H18 H 0.3865 0.3856 0.2497 0.059 Uiso 1 1 calc R . . C19 C 0.2972(2) 0.3984(3) 0.16671(19) 0.0510(11) Uani 1 1 d . . . H19 H 0.3140 0.3898 0.1511 0.061 Uiso 1 1 calc R . . C20 C 0.2289(2) 0.4147(3) 0.13177(17) 0.0427(10) Uani 1 1 d . . . H20 H 0.2000 0.4174 0.0922 0.051 Uiso 1 1 calc R . . C21 C 0.11356(16) 0.7065(2) 0.10729(12) 0.0241(7) Uani 1 1 d . . . C22 C 0.13906(15) 0.7496(2) 0.08391(13) 0.0224(7) Uani 1 1 d . . . C23 C 0.18194(16) 0.6948(2) 0.08678(14) 0.0256(7) Uani 1 1 d . . . H23 H 0.1964 0.6364 0.1048 0.031 Uiso 1 1 calc R . . C24 C 0.20291(16) 0.7268(2) 0.06305(14) 0.0268(7) Uani 1 1 d . . . C25 C 0.18354(16) 0.8140(2) 0.03665(14) 0.0280(7) Uani 1 1 d . . . H25 H 0.1992 0.8349 0.0214 0.034 Uiso 1 1 calc R . . C26 C 0.14038(16) 0.8698(2) 0.03325(13) 0.0245(7) Uani 1 1 d . . . C27 C 0.11658(15) 0.8378(2) 0.05611(13) 0.0231(7) Uani 1 1 d . . . C28 C 0.06810(16) 0.9003(2) 0.05063(13) 0.0218(7) Uani 1 1 d . . . C29 C 0.11941(18) 0.9622(2) 0.00246(15) 0.0317(8) Uani 1 1 d . . . C30 C 0.0000 0.5065(4) 0.2500 0.0317(11) Uani 1 2 d S . . C31 C -0.00174(17) 0.5537(3) 0.21267(14) 0.0323(8) Uani 1 1 d . . . H31 H -0.0031 0.5205 0.1879 0.039 Uiso 1 1 calc R . . C32 C -0.00146(18) 0.6514(3) 0.21292(14) 0.0328(8) Uani 1 1 d . A . C33 C 0.0000 0.7010(4) 0.2500 0.0283(11) Uani 1 2 d S . . C34 C 0.0000 0.8054(4) 0.2500 0.0370(12) Uani 1 2 d S . . C35 C -0.0049(2) 0.7020(3) 0.17084(15) 0.0371(9) Uani 1 1 d . . . C36 C -0.00086(15) 0.3145(2) 0.06838(12) 0.0213(7) Uani 1 1 d . . . C37 C -0.04810(15) 0.3637(2) 0.06940(13) 0.0216(7) Uani 1 1 d . . . C38 C -0.06502(16) 0.3134(2) 0.09351(13) 0.0260(7) Uani 1 1 d . . . H38 H -0.0486 0.2526 0.1074 0.031 Uiso 1 1 calc R . . C39 C -0.10667(16) 0.3552(2) 0.09647(13) 0.0261(7) Uani 1 1 d . . . C40 C -0.13367(16) 0.4436(2) 0.07510(14) 0.0254(7) Uani 1 1 d . . . H40 H -0.1623 0.4691 0.0771 0.030 Uiso 1 1 calc R . . C41 C -0.11785(16) 0.4945(2) 0.05044(13) 0.0224(7) Uani 1 1 d . . . C42 C -0.07425(15) 0.4543(2) 0.04765(12) 0.0198(6) Uani 1 1 d . . . C43 C -0.05459(15) 0.5070(2) 0.02179(13) 0.0199(6) Uani 1 1 d . . . C44 C -0.14682(16) 0.5933(2) 0.02950(14) 0.0246(7) Uani 1 1 d . . . C1' C 0.050(3) 0.093(4) 0.178(2) 0.066(3) Uani 0.192(5) 1 d P A 2 H1' H 0.0090 0.0593 0.1513 0.079 Uiso 0.192(5) 1 calc PR A 2 C2' C 0.072(3) 0.136(5) 0.231(3) 0.092(4) Uani 0.192(5) 1 d P A 2 H2' H 0.0451 0.1361 0.2377 0.110 Uiso 0.192(5) 1 calc PR A 2 C3' C 0.137(3) 0.174(4) 0.270(2) 0.114(5) Uani 0.192(5) 1 d P A 2 H3' H 0.1553 0.1996 0.3043 0.136 Uiso 0.192(5) 1 calc PR A 2 C4' C 0.176(3) 0.175(4) 0.260(2) 0.093(4) Uani 0.192(5) 1 d P A 2 H4' H 0.2191 0.2007 0.2877 0.112 Uiso 0.192(5) 1 calc PR A 2 C5' C 0.152(2) 0.137(3) 0.2045(19) 0.050(2) Uani 0.192(5) 1 d P A 2 C6' C 0.189(3) 0.144(6) 0.195(3) 0.057(3) Uani 0.192(5) 1 d P A 2 C7' C 0.263(3) 0.154(4) 0.235(2) 0.078(3) Uani 0.192(5) 1 d P A 2 H7' H 0.2922 0.1528 0.2749 0.093 Uiso 0.192(5) 1 calc PR A 2 C8' C 0.290(3) 0.166(4) 0.214(2) 0.090(4) Uani 0.192(5) 1 d P A 2 H8' H 0.3363 0.1793 0.2400 0.108 Uiso 0.192(5) 1 calc PR A 2 C9' C 0.256(2) 0.159(3) 0.159(2) 0.075(3) Uani 0.192(5) 1 d P A 2 H9' H 0.2761 0.1644 0.1462 0.090 Uiso 0.192(5) 1 calc PR A 2 C10' C 0.176(3) 0.142(5) 0.118(3) 0.056(3) Uani 0.192(5) 1 d P A 2 H10' H 0.1482 0.1329 0.0785 0.067 Uiso 0.192(5) 1 calc PR A 2 Mn1 Mn 0.09630(2) 0.48652(3) 0.09928(2) 0.02206(13) Uani 1 1 d . . . Mn2 Mn -0.01870(3) 0.69918(3) 0.07161(2) 0.02441(13) Uani 1 1 d . . . Mn3 Mn 0.03829(2) 0.08330(3) 0.07807(2) 0.02540(14) Uani 1 1 d . . . Mn4 Mn -0.2500 0.7500 0.0000 0.0351(2) Uani 1 2 d S . . N2 N 0.14514(16) 0.1387(2) 0.14056(14) 0.0452(9) Uani 1 1 d . A . N1 N 0.0709(4) 0.0868(6) 0.1618(4) 0.043(2) Uani 0.808(5) 1 d P A 1 N3 N 0.14533(14) 0.4535(2) 0.18929(11) 0.0282(6) Uani 1 1 d . . . N4 N 0.20192(14) 0.4270(2) 0.15173(12) 0.0313(7) Uani 1 1 d . . . N5 N -0.12207(15) 0.3020(2) 0.12392(13) 0.0346(7) Uani 1 1 d . . . N6 N 0.24476(15) 0.6639(2) 0.06335(14) 0.0352(7) Uani 1 1 d . . . N7 N 0.0000 0.4033(3) 0.2500 0.0380(10) Uani 1 2 d S . . O1 O 0.00092(12) 0.22736(16) 0.07153(10) 0.0323(6) Uani 1 1 d . A . O2 O 0.03217(11) 0.36410(16) 0.06391(10) 0.0283(5) Uani 1 1 d . . . O3 O -0.00106(10) 0.55716(15) 0.05641(9) 0.0230(5) Uani 1 1 d . A . O4 O -0.08984(11) 0.49511(17) -0.03009(9) 0.0280(5) Uani 1 1 d . . . O5 O -0.15211(15) 0.3433(2) 0.13262(13) 0.0505(7) Uani 1 1 d . . . O6 O -0.10400(15) 0.2199(2) 0.13678(13) 0.0494(7) Uani 1 1 d . . . O7 O -0.19136(13) 0.61755(18) 0.02678(12) 0.0414(7) Uani 1 1 d . . . O8 O -0.12350(12) 0.64531(16) 0.01625(10) 0.0304(5) Uani 1 1 d . A . O9 O 0.07484(12) 0.75494(16) 0.10509(10) 0.0305(5) Uani 1 1 d . A . O10 O 0.13436(11) 0.62500(16) 0.12783(9) 0.0284(5) Uani 1 1 d . . . O11 O 0.26970(17) 0.5945(2) 0.09418(15) 0.0617(9) Uani 1 1 d . . . O12 O 0.25198(14) 0.6840(2) 0.03251(12) 0.0457(7) Uani 1 1 d . . . O13 O 0.00523(10) 0.89212(15) 0.00572(9) 0.0232(5) Uani 1 1 d . . . O14 O 0.09393(11) 0.95888(16) 0.08946(10) 0.0313(5) Uani 1 1 d . . . O15 O 0.05701(12) 0.98344(16) -0.03591(10) 0.0319(6) Uani 1 1 d . . . O16 O 0.16555(15) 1.0104(2) 0.01547(15) 0.0639(10) Uani 1 1 d . . . O17 O -0.0234(4) 0.7868(4) 0.1612(3) 0.091(2) Uani 0.808(5) 1 d P A 1 O18 O 0.00348(14) 0.65507(18) 0.14514(11) 0.0398(6) Uani 1 1 d . A . O19 O -0.05565(17) 0.8485(3) 0.21947(16) 0.0742(10) Uani 1 1 d . . . O20 O 0.01272(15) 0.3628(2) 0.22625(12) 0.0503(7) Uani 1 1 d . . . O21 O -0.04499(15) 0.83810(17) 0.07528(12) 0.0462(7) Uani 1 1 d D A . H21B H -0.0413 0.8915 0.0661 0.055 Uiso 1 1 d RD . . H21A H -0.0413 0.8448 0.1025 0.055 Uiso 1 1 d RD . . O22 O -0.06299(12) 0.73781(17) -0.01299(10) 0.0318(6) Uani 1 1 d D A . H22B H -0.0586 0.6962 -0.0285 0.038 Uiso 1 1 d RD . . H22A H -0.0408 0.7888 -0.0029 0.038 Uiso 1 1 d RD . . O23 O -0.16947(16) 0.8175(2) 0.08360(13) 0.0677(9) Uani 1 1 d D . . H23B H -0.1406 0.7783 0.1099 0.081 Uiso 1 1 d RD . . H23A H -0.1575 0.8742 0.0866 0.081 Uiso 1 1 d RD . . O24 O -0.29116(14) 0.69626(19) 0.03149(12) 0.0456(7) Uani 1 1 d D . . H24B H -0.3072 0.6412 0.0235 0.055 Uiso 1 1 d RD . . H24A H -0.3167 0.7374 0.0265 0.055 Uiso 1 1 d RD . . O25 O 0.6458(2) 0.4992(3) 0.9193(2) 0.0743(14) Uani 0.808(5) 1 d P A 1 O17' O 0.0145(18) 0.779(2) 0.1802(13) 0.091(2) Uani 0.192(5) 1 d P A 2 O25' O 0.5680(10) 0.4865(11) 0.8166(9) 0.0743(14) Uani 0.192(5) 1 d P A 2 N1' N 0.088(3) 0.105(3) 0.172(2) 0.043(2) Uani 0.192(5) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.086(6) 0.075(6) 0.057(5) 0.020(4) 0.059(5) 0.029(4) C2 0.123(8) 0.105(7) 0.071(6) 0.023(4) 0.078(6) 0.046(5) C3 0.161(11) 0.120(8) 0.069(6) 0.005(5) 0.086(7) 0.037(7) C4 0.114(8) 0.079(5) 0.044(4) -0.014(3) 0.042(5) 0.009(6) C5 0.069(6) 0.032(3) 0.024(2) -0.0015(19) 0.025(3) 0.013(3) C6 0.048(7) 0.023(3) 0.032(3) -0.0006(19) 0.006(4) 0.002(5) C7 0.052(5) 0.038(4) 0.044(3) -0.003(3) 0.001(3) -0.003(4) C8 0.043(4) 0.045(4) 0.079(7) 0.000(5) 0.009(4) -0.011(3) C9 0.036(3) 0.046(3) 0.105(7) 0.015(4) 0.038(4) 0.000(2) C10 0.034(4) 0.039(4) 0.056(7) 0.004(5) 0.020(5) 0.000(3) C11 0.031(2) 0.060(3) 0.036(2) 0.0052(19) 0.0240(18) 0.0032(18) C12 0.046(2) 0.076(3) 0.037(2) 0.005(2) 0.031(2) 0.004(2) C13 0.046(2) 0.068(3) 0.0263(19) 0.0105(19) 0.023(2) 0.007(2) C14 0.030(2) 0.050(3) 0.0276(19) 0.0076(17) 0.0152(17) 0.0079(17) C15 0.0279(18) 0.0238(18) 0.0271(17) 0.0013(14) 0.0174(15) 0.0014(14) C16 0.0264(18) 0.0231(18) 0.0306(18) 0.0013(14) 0.0185(16) 0.0005(14) C17 0.029(2) 0.040(2) 0.036(2) 0.0023(17) 0.0189(18) 0.0020(16) C18 0.030(2) 0.052(3) 0.061(3) 0.005(2) 0.031(2) 0.0063(18) C19 0.048(3) 0.063(3) 0.059(3) 0.015(2) 0.044(2) 0.018(2) C20 0.043(2) 0.053(3) 0.041(2) 0.0135(19) 0.033(2) 0.0174(19) C21 0.0208(16) 0.0260(18) 0.0161(15) -0.0008(13) 0.0101(13) -0.0025(13) C22 0.0210(16) 0.0192(17) 0.0188(15) -0.0008(12) 0.0116(14) -0.0007(12) C23 0.0225(16) 0.0190(17) 0.0295(17) 0.0011(14) 0.0167(15) 0.0012(13) C24 0.0215(16) 0.0256(18) 0.0301(17) -0.0007(14) 0.0174(15) 0.0012(14) C25 0.0260(17) 0.0258(18) 0.0325(18) 0.0027(14) 0.0212(16) -0.0006(14) C26 0.0223(16) 0.0207(17) 0.0268(17) 0.0001(13) 0.0164(15) -0.0018(13) C27 0.0196(15) 0.0223(17) 0.0183(15) -0.0016(13) 0.0106(14) -0.0014(13) C28 0.0267(17) 0.0171(16) 0.0217(16) 0.0054(13) 0.0174(15) 0.0023(13) C29 0.035(2) 0.0259(19) 0.041(2) 0.0064(16) 0.0294(18) 0.0030(15) C30 0.031(3) 0.036(3) 0.027(2) 0.000 0.020(2) 0.000 C31 0.034(2) 0.040(2) 0.0297(18) -0.0011(16) 0.0256(17) 0.0007(16) C32 0.0320(19) 0.046(2) 0.0266(18) 0.0059(16) 0.0232(17) 0.0058(16) C33 0.023(2) 0.039(3) 0.025(2) 0.000 0.018(2) 0.000 C34 0.045(3) 0.047(3) 0.031(3) 0.000 0.031(3) 0.000 C35 0.051(2) 0.041(2) 0.034(2) 0.0083(17) 0.035(2) 0.0098(18) C36 0.0219(16) 0.0199(17) 0.0157(14) 0.0004(12) 0.0114(13) 0.0025(13) C37 0.0199(15) 0.0192(16) 0.0208(15) -0.0006(12) 0.0130(14) 0.0018(12) C38 0.0289(17) 0.0209(17) 0.0256(16) 0.0043(13) 0.0187(15) 0.0017(14) C39 0.0281(18) 0.0278(19) 0.0257(17) 0.0014(14) 0.0204(15) -0.0035(14) C40 0.0274(17) 0.0253(18) 0.0309(17) -0.0008(14) 0.0234(16) -0.0005(14) C41 0.0239(16) 0.0209(17) 0.0232(16) 0.0005(13) 0.0172(14) 0.0015(13) C42 0.0200(15) 0.0185(16) 0.0160(14) -0.0011(12) 0.0113(13) -0.0017(12) C43 0.0221(16) 0.0158(15) 0.0240(16) 0.0039(12) 0.0173(15) 0.0070(12) C44 0.0256(17) 0.0226(17) 0.0299(17) 0.0036(14) 0.0214(15) 0.0029(14) C1' 0.086(6) 0.075(6) 0.057(5) 0.020(4) 0.059(5) 0.029(4) C2' 0.123(8) 0.105(7) 0.071(6) 0.023(4) 0.078(6) 0.046(5) C3' 0.161(11) 0.120(8) 0.069(6) 0.005(5) 0.086(7) 0.037(7) C4' 0.114(8) 0.079(5) 0.044(4) -0.014(3) 0.042(5) 0.009(6) C5' 0.069(6) 0.032(3) 0.024(2) -0.0015(19) 0.025(3) 0.013(3) C6' 0.048(7) 0.023(3) 0.032(3) -0.0006(19) 0.006(4) 0.002(5) C7' 0.052(5) 0.038(4) 0.044(3) -0.003(3) 0.001(3) -0.003(4) C8' 0.043(4) 0.045(4) 0.079(7) 0.000(5) 0.009(4) -0.011(3) C9' 0.036(3) 0.046(3) 0.105(7) 0.015(4) 0.038(4) 0.000(2) C10' 0.034(4) 0.039(4) 0.056(7) 0.004(5) 0.020(5) 0.000(3) Mn1 0.0222(3) 0.0207(3) 0.0215(3) 0.00304(19) 0.0151(2) 0.00305(19) Mn2 0.0333(3) 0.0197(3) 0.0303(3) 0.0027(2) 0.0263(3) 0.0029(2) Mn3 0.0280(3) 0.0220(3) 0.0210(3) 0.0015(2) 0.0159(2) 0.0036(2) Mn4 0.0356(4) 0.0249(4) 0.0552(5) 0.0057(4) 0.0361(4) 0.0062(3) N2 0.0351(18) 0.0241(17) 0.0380(19) -0.0004(14) 0.0133(16) 0.0005(14) N1 0.061(6) 0.032(4) 0.025(4) 0.003(3) 0.027(4) 0.011(3) N3 0.0260(15) 0.0301(16) 0.0259(14) 0.0039(12) 0.0177(13) 0.0024(12) N4 0.0304(16) 0.0322(17) 0.0303(15) 0.0076(13) 0.0215(14) 0.0076(13) N5 0.0361(17) 0.0357(19) 0.0378(17) 0.0084(14) 0.0285(15) -0.0010(14) N6 0.0333(17) 0.0302(17) 0.0467(18) 0.0007(15) 0.0304(16) 0.0038(14) N7 0.039(3) 0.041(3) 0.034(2) 0.000 0.026(2) 0.000 O1 0.0437(15) 0.0168(12) 0.0436(14) 0.0023(10) 0.0339(13) 0.0068(10) O2 0.0323(13) 0.0231(13) 0.0379(13) -0.0036(10) 0.0280(12) -0.0009(10) O3 0.0233(12) 0.0188(12) 0.0273(11) 0.0010(9) 0.0183(10) 0.0028(9) O4 0.0291(12) 0.0338(14) 0.0230(12) 0.0012(10) 0.0194(11) 0.0017(10) O5 0.0597(19) 0.059(2) 0.0663(19) 0.0150(15) 0.0563(18) 0.0091(15) O6 0.0600(18) 0.0362(17) 0.0661(19) 0.0183(14) 0.0500(17) 0.0056(14) O7 0.0509(16) 0.0287(14) 0.0748(19) 0.0170(13) 0.0553(16) 0.0156(12) O8 0.0335(13) 0.0240(13) 0.0432(14) 0.0095(10) 0.0308(12) 0.0072(10) O9 0.0365(14) 0.0268(13) 0.0381(13) 0.0043(10) 0.0302(12) 0.0039(10) O10 0.0308(13) 0.0222(13) 0.0254(12) 0.0041(10) 0.0178(11) 0.0007(10) O11 0.076(2) 0.0432(18) 0.102(3) 0.0354(18) 0.076(2) 0.0349(16) O12 0.0502(17) 0.0523(18) 0.0535(17) 0.0034(14) 0.0436(16) 0.0076(14) O13 0.0226(12) 0.0224(12) 0.0216(11) 0.0015(9) 0.0149(10) 0.0016(9) O14 0.0301(13) 0.0232(13) 0.0280(12) -0.0033(10) 0.0167(11) 0.0036(10) O15 0.0341(14) 0.0246(13) 0.0385(14) 0.0099(10) 0.0266(12) 0.0066(10) O16 0.0457(18) 0.0399(18) 0.097(3) 0.0294(17) 0.0482(19) 0.0045(14) O17 0.195(8) 0.052(2) 0.108(5) 0.051(3) 0.137(6) 0.074(4) O18 0.0645(18) 0.0371(15) 0.0425(14) 0.0076(12) 0.0468(15) 0.0090(13) O19 0.060(2) 0.068(2) 0.089(3) -0.001(2) 0.052(2) 0.0166(18) O20 0.0602(19) 0.0478(18) 0.0521(17) -0.0081(14) 0.0435(16) 0.0004(14) O21 0.085(2) 0.0216(14) 0.0617(18) 0.0110(12) 0.0627(18) 0.0125(13) O22 0.0440(15) 0.0243(13) 0.0328(13) -0.0030(10) 0.0296(12) -0.0059(11) O23 0.061(2) 0.053(2) 0.0580(19) 0.0012(16) 0.0324(18) -0.0053(16) O24 0.0487(16) 0.0328(15) 0.0719(19) 0.0120(14) 0.0490(16) 0.0086(12) O25 0.092(3) 0.037(2) 0.136(4) -0.016(2) 0.096(3) -0.007(2) O17' 0.195(8) 0.052(2) 0.108(5) 0.051(3) 0.137(6) 0.074(4) O25' 0.092(3) 0.037(2) 0.136(4) -0.016(2) 0.096(3) -0.007(2) N1' 0.061(6) 0.032(4) 0.025(4) 0.003(3) 0.027(4) 0.011(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 C1 N1 1.358(17) . ? C1 C2 1.367(16) . ? C1 H1 0.9300 . ? C2 C3 1.374(15) . ? C2 H2 0.9300 . ? C3 C4 1.337(16) . ? C3 H3 0.9300 . ? C4 C5 1.390(12) . ? C4 H4 0.9300 . ? C5 N1 1.376(12) . ? C5 C6 1.473(16) . ? C6 N2 1.363(17) . ? C6 C7 1.395(15) . ? C7 C8 1.338(14) . ? C7 H7 0.9300 . ? C8 C9 1.385(15) . ? C8 H8 0.9300 . ? C9 C10 1.350(16) . ? C9 H9 0.9300 . ? C10 N2 1.298(17) . ? C10 H10 0.9300 . ? C11 N3 1.336(4) . ? C11 C12 1.371(5) . ? C11 H11 0.9300 . ? C12 C13 1.368(6) . ? C12 H12 0.9300 . ? C13 C14 1.375(6) . ? C13 H13 0.9300 . ? C14 C15 1.384(5) . ? C14 H14 0.9300 . ? C15 N3 1.341(4) . ? C15 C16 1.483(5) . ? C16 N4 1.356(4) . ? C16 C17 1.379(5) . ? C17 C18 1.372(6) . ? C17 H17 0.9300 . ? C18 C19 1.368(6) . ? C18 H18 0.9300 . ? C19 C20 1.377(5) . ? C19 H19 0.9300 . ? C20 N4 1.335(5) . ? C20 H20 0.9300 . ? C21 O9 1.247(4) . ? C21 O10 1.254(4) . ? C21 C22 1.519(4) . ? C22 C23 1.382(4) . ? C22 C27 1.409(4) . ? C23 C24 1.363(5) . ? C23 H23 0.9300 . ? C24 C25 1.383(5) . ? C24 N6 1.474(4) . ? C25 C26 1.387(5) . ? C25 H25 0.9300 . ? C26 C27 1.406(4) . ? C26 C29 1.500(5) . ? C27 C28 1.526(4) . ? C28 O14 1.243(4) . ? C28 O13 1.258(4) . ? C29 O16 1.240(4) . ? C29 O15 1.260(4) . ? C30 C31 1.385(4) 2 ? C30 C31 1.385(4) . ? C30 N7 1.465(7) . ? C31 C32 1.387(5) . ? C31 H31 0.9300 . ? C32 C33 1.398(4) . ? C32 C35 1.517(5) . ? C33 C32 1.398(4) 2 ? C33 C34 1.482(7) . ? C34 O19 1.255(4) 2 ? C34 O19 1.255(4) . ? C35 O17' 1.16(4) . ? C35 O18 1.236(4) . ? C35 O17 1.259(6) . ? C36 O1 1.239(4) . ? C36 O2 1.259(4) . ? C36 C37 1.526(4) . ? C37 C38 1.392(4) . ? C37 C42 1.398(4) . ? C38 C39 1.382(5) . ? C38 H38 0.9300 . ? C39 C40 1.372(5) . ? C39 N5 1.473(4) . ? C40 C41 1.388(4) . ? C40 H40 0.9300 . ? C41 C42 1.418(4) . ? C41 C44 1.517(4) . ? C42 C43 1.517(4) . ? C43 O4 1.241(4) . ? C43 O3 1.270(4) . ? C44 O7 1.241(4) . ? C44 O8 1.261(4) . ? C1' N1' 1.26(9) . ? C1' C2' 1.52(9) . ? C1' H1' 0.9300 . ? C2' C3' 1.39(9) . ? C2' H2' 0.9300 . ? C3' C4' 1.35(9) . ? C3' H3' 0.9300 . ? C4' C5' 1.54(6) . ? C4' H4' 0.9300 . ? C5' N1' 1.35(7) . ? C5' C6' 1.27(9) . ? C6' N2 1.28(8) . ? C6' C7' 1.48(9) . ? C7' C8' 1.37(9) . ? C7' H7' 0.9300 . ? C8' C9' 1.32(8) . ? C8' H8' 0.9300 . ? C9' C10' 1.60(8) . ? C9' H9' 0.9300 . ? C10' N2 1.52(8) . ? C10' H10' 0.9300 . ? Mn1 O10 2.110(2) . ? Mn1 O2 2.148(2) . ? Mn1 O4 2.198(2) 5_565 ? Mn1 O3 2.223(2) . ? Mn1 N4 2.270(3) . ? Mn1 N3 2.278(3) . ? Mn2 O21 2.141(2) . ? Mn2 O9 2.143(2) . ? Mn2 O18 2.145(2) . ? Mn2 O22 2.183(2) . ? Mn2 O8 2.209(2) . ? Mn2 O3 2.221(2) . ? Mn3 O13 2.125(2) 5_565 ? Mn3 O15 2.159(2) 5_565 ? Mn3 O14 2.206(2) 1_545 ? Mn3 O1 2.238(2) . ? Mn3 N2 2.239(3) . ? Mn3 N1 2.230(11) . ? Mn3 N1' 2.35(6) . ? Mn4 O23 2.180(3) . ? Mn4 O23 2.180(3) 7_465 ? Mn4 O24 2.188(3) . ? Mn4 O24 2.188(3) 7_465 ? Mn4 O7 2.223(2) 7_465 ? Mn4 O7 2.223(2) . ? N5 O6 1.220(4) . ? N5 O5 1.225(4) . ? N6 O12 1.218(4) . ? N6 O11 1.218(4) . ? N7 O20 1.223(3) 2 ? N7 O20 1.223(3) . ? O4 Mn1 2.198(2) 5_565 ? O13 Mn3 2.125(2) 5_565 ? O14 Mn3 2.206(2) 1_565 ? O15 Mn3 2.159(2) 5_565 ? O21 H21B 0.8517 . ? O21 H21A 0.8428 . ? O22 H22B 0.8512 . ? O22 H22A 0.8513 . ? O23 H23B 0.8455 . ? O23 H23A 0.8505 . ? O24 H24B 0.8450 . ? O24 H24A 0.8455 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 122.2(9) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 119.0(10) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C4 C3 C2 120.2(12) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 120.7(11) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? N1 C5 C4 119.7(8) . . ? N1 C5 C6 114.4(9) . . ? C4 C5 C6 125.9(11) . . ? N2 C6 C7 119.2(11) . . ? N2 C6 C5 119.8(10) . . ? C7 C6 C5 120.9(13) . . ? C8 C7 C6 121.1(10) . . ? C8 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? C7 C8 C9 117.7(9) . . ? C7 C8 H8 121.1 . . ? C9 C8 H8 121.1 . . ? C10 C9 C8 119.4(9) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? N2 C10 C9 123.7(8) . . ? N2 C10 H10 118.1 . . ? C9 C10 H10 118.1 . . ? N3 C11 C12 123.1(4) . . ? N3 C11 H11 118.5 . . ? C12 C11 H11 118.5 . . ? C13 C12 C11 119.1(4) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C12 C13 C14 118.6(4) . . ? C12 C13 H13 120.7 . . ? C14 C13 H13 120.7 . . ? C13 C14 C15 119.6(4) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? N3 C15 C14 121.6(3) . . ? N3 C15 C16 116.6(3) . . ? C14 C15 C16 121.8(3) . . ? N4 C16 C17 121.7(3) . . ? N4 C16 C15 115.5(3) . . ? C17 C16 C15 122.8(3) . . ? C18 C17 C16 119.5(4) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C19 C18 C17 119.4(4) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 118.4(4) . . ? C18 C19 H19 120.8 . . ? C20 C19 H19 120.8 . . ? N4 C20 C19 123.5(4) . . ? N4 C20 H20 118.3 . . ? C19 C20 H20 118.3 . . ? O9 C21 O10 125.9(3) . . ? O9 C21 C22 117.7(3) . . ? O10 C21 C22 116.4(3) . . ? C23 C22 C27 120.2(3) . . ? C23 C22 C21 116.8(3) . . ? C27 C22 C21 122.8(3) . . ? C24 C23 C22 119.7(3) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C25 122.1(3) . . ? C23 C24 N6 118.3(3) . . ? C25 C24 N6 119.6(3) . . ? C24 C25 C26 119.0(3) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? C25 C26 C27 120.3(3) . . ? C25 C26 C29 116.5(3) . . ? C27 C26 C29 123.2(3) . . ? C26 C27 C22 118.7(3) . . ? C26 C27 C28 118.9(3) . . ? C22 C27 C28 122.4(3) . . ? O14 C28 O13 124.9(3) . . ? O14 C28 C27 117.4(3) . . ? O13 C28 C27 117.6(3) . . ? O16 C29 O15 124.8(3) . . ? O16 C29 C26 116.4(3) . . ? O15 C29 C26 118.7(3) . . ? C31 C30 C31 122.1(5) 2 . ? C31 C30 N7 119.0(2) 2 . ? C31 C30 N7 119.0(2) . . ? C30 C31 C32 118.8(3) . . ? C30 C31 H31 120.6 . . ? C32 C31 H31 120.6 . . ? C31 C32 C33 120.3(3) . . ? C31 C32 C35 118.1(3) . . ? C33 C32 C35 121.6(4) . . ? C32 C33 C32 119.6(5) 2 . ? C32 C33 C34 120.2(2) 2 . ? C32 C33 C34 120.2(2) . . ? O19 C34 O19 121.7(6) 2 . ? O19 C34 C33 119.2(3) 2 . ? O19 C34 C33 119.2(3) . . ? O17' C35 O18 114.0(12) . . ? O17' C35 O17 36.4(14) . . ? O18 C35 O17 126.1(4) . . ? O17' C35 C32 119.5(13) . . ? O18 C35 C32 118.1(3) . . ? O17 C35 C32 115.4(4) . . ? O1 C36 O2 125.5(3) . . ? O1 C36 C37 116.0(3) . . ? O2 C36 C37 118.6(3) . . ? C38 C37 C42 120.0(3) . . ? C38 C37 C36 116.4(3) . . ? C42 C37 C36 123.5(3) . . ? C39 C38 C37 118.9(3) . . ? C39 C38 H38 120.6 . . ? C37 C38 H38 120.6 . . ? C40 C39 C38 122.6(3) . . ? C40 C39 N5 119.4(3) . . ? C38 C39 N5 118.0(3) . . ? C39 C40 C41 119.4(3) . . ? C39 C40 H40 120.3 . . ? C41 C40 H40 120.3 . . ? C40 C41 C42 119.5(3) . . ? C40 C41 C44 117.3(3) . . ? C42 C41 C44 123.2(3) . . ? C37 C42 C41 119.7(3) . . ? C37 C42 C43 118.5(3) . . ? C41 C42 C43 121.8(3) . . ? O4 C43 O3 125.6(3) . . ? O4 C43 C42 118.2(3) . . ? O3 C43 C42 116.1(3) . . ? O7 C44 O8 124.6(3) . . ? O7 C44 C41 118.1(3) . . ? O8 C44 C41 117.3(3) . . ? N1' C1' C2' 117(5) . . ? N1' C1' H1' 121.5 . . ? C2' C1' H1' 121.5 . . ? C3' C2' C1' 114(6) . . ? C3' C2' H2' 123.0 . . ? C1' C2' H2' 123.0 . . ? C4' C3' C2' 122(5) . . ? C4' C3' H3' 118.9 . . ? C2' C3' H3' 118.9 . . ? C3' C4' C5' 125(5) . . ? C3' C4' H4' 117.6 . . ? C5' C4' H4' 117.6 . . ? N1' C5' C6' 133(6) . . ? N1' C5' C4' 105(4) . . ? C6' C5' C4' 122(6) . . ? N2 C6' C5' 103(6) . . ? N2 C6' C7' 125(6) . . ? C5' C6' C7' 132(7) . . ? C8' C7' C6' 120(5) . . ? C8' C7' H7' 120.0 . . ? C6' C7' H7' 120.0 . . ? C9' C8' C7' 126(5) . . ? C9' C8' H8' 116.9 . . ? C7' C8' H8' 116.9 . . ? C8' C9' C10' 112(4) . . ? C8' C9' H9' 123.9 . . ? C10' C9' H9' 123.9 . . ? N2 C10' C9' 122(4) . . ? N2 C10' H10' 119.0 . . ? C9' C10' H10' 119.0 . . ? O10 Mn1 O2 162.87(9) . . ? O10 Mn1 O4 89.72(9) . 5_565 ? O2 Mn1 O4 96.73(9) . 5_565 ? O10 Mn1 O3 82.09(8) . . ? O2 Mn1 O3 81.31(8) . . ? O4 Mn1 O3 97.97(8) 5_565 . ? O10 Mn1 N4 92.25(10) . . ? O2 Mn1 N4 104.01(10) . . ? O4 Mn1 N4 85.79(9) 5_565 . ? O3 Mn1 N4 173.15(10) . . ? O10 Mn1 N3 88.09(9) . . ? O2 Mn1 N3 91.81(9) . . ? O4 Mn1 N3 157.51(9) 5_565 . ? O3 Mn1 N3 103.88(9) . . ? N4 Mn1 N3 71.95(10) . . ? O21 Mn2 O9 88.67(10) . . ? O21 Mn2 O18 91.81(10) . . ? O9 Mn2 O18 105.89(10) . . ? O21 Mn2 O22 86.73(9) . . ? O9 Mn2 O22 85.81(9) . . ? O18 Mn2 O22 168.18(10) . . ? O21 Mn2 O8 93.25(10) . . ? O9 Mn2 O8 165.60(9) . . ? O18 Mn2 O8 88.32(10) . . ? O22 Mn2 O8 80.06(9) . . ? O21 Mn2 O3 173.12(9) . . ? O9 Mn2 O3 93.48(8) . . ? O18 Mn2 O3 93.87(9) . . ? O22 Mn2 O3 86.92(8) . . ? O8 Mn2 O3 83.06(8) . . ? O13 Mn3 O15 86.76(9) 5_565 5_565 ? O13 Mn3 O14 91.42(8) 5_565 1_545 ? O15 Mn3 O14 99.13(9) 5_565 1_545 ? O13 Mn3 O1 86.31(9) 5_565 . ? O15 Mn3 O1 93.39(9) 5_565 . ? O14 Mn3 O1 167.13(9) 1_545 . ? O13 Mn3 N2 106.61(11) 5_565 . ? O15 Mn3 N2 166.47(11) 5_565 . ? O14 Mn3 N2 78.87(10) 1_545 . ? O1 Mn3 N2 89.63(10) . . ? O13 Mn3 N1 167.0(3) 5_565 . ? O15 Mn3 N1 91.4(2) 5_565 . ? O14 Mn3 N1 101.6(3) 1_545 . ? O1 Mn3 N1 81.0(3) . . ? N2 Mn3 N1 76.0(2) . . ? O13 Mn3 N1' 163.1(12) 5_565 . ? O15 Mn3 N1' 101.4(12) 5_565 . ? O14 Mn3 N1' 101.7(14) 1_545 . ? O1 Mn3 N1' 78.6(13) . . ? N2 Mn3 N1' 66.2(13) . . ? N1 Mn3 N1' 10.2(13) . . ? O23 Mn4 O23 180.00(16) . 7_465 ? O23 Mn4 O24 87.84(12) . . ? O23 Mn4 O24 92.16(12) 7_465 . ? O23 Mn4 O24 92.16(12) . 7_465 ? O23 Mn4 O24 87.84(12) 7_465 7_465 ? O24 Mn4 O24 180.00(11) . 7_465 ? O23 Mn4 O7 86.13(12) . 7_465 ? O23 Mn4 O7 93.87(12) 7_465 7_465 ? O24 Mn4 O7 89.43(9) . 7_465 ? O24 Mn4 O7 90.57(9) 7_465 7_465 ? O23 Mn4 O7 93.87(12) . . ? O23 Mn4 O7 86.13(12) 7_465 . ? O24 Mn4 O7 90.57(9) . . ? O24 Mn4 O7 89.43(9) 7_465 . ? O7 Mn4 O7 180.0 7_465 . ? C6' N2 C10 101(3) . . ? C6' N2 C6 18(3) . . ? C10 N2 C6 118.7(7) . . ? C6' N2 C10' 114(4) . . ? C10 N2 C10' 13(3) . . ? C6 N2 C10' 132(2) . . ? C6' N2 Mn3 128(4) . . ? C10 N2 Mn3 128.0(5) . . ? C6 N2 Mn3 112.4(6) . . ? C10' N2 Mn3 115(2) . . ? C1 N1 C5 118.3(10) . . ? C1 N1 Mn3 124.3(6) . . ? C5 N1 Mn3 114.2(7) . . ? C11 N3 C15 118.0(3) . . ? C11 N3 Mn1 124.7(2) . . ? C15 N3 Mn1 117.1(2) . . ? C20 N4 C16 117.5(3) . . ? C20 N4 Mn1 124.5(2) . . ? C16 N4 Mn1 116.8(2) . . ? O6 N5 O5 124.0(3) . . ? O6 N5 C39 118.3(3) . . ? O5 N5 C39 117.7(3) . . ? O12 N6 O11 123.9(3) . . ? O12 N6 C24 118.1(3) . . ? O11 N6 C24 118.0(3) . . ? O20 N7 O20 124.0(5) 2 . ? O20 N7 C30 118.0(2) 2 . ? O20 N7 C30 118.0(2) . . ? C36 O1 Mn3 155.2(2) . . ? C36 O2 Mn1 142.1(2) . . ? C43 O3 Mn2 113.70(18) . . ? C43 O3 Mn1 116.29(18) . . ? Mn2 O3 Mn1 129.65(10) . . ? C43 O4 Mn1 145.9(2) . 5_565 ? C44 O7 Mn4 133.2(2) . . ? C44 O8 Mn2 129.1(2) . . ? C21 O9 Mn2 121.6(2) . . ? C21 O10 Mn1 136.5(2) . . ? C28 O13 Mn3 122.65(19) . 5_565 ? C28 O14 Mn3 123.0(2) . 1_565 ? C29 O15 Mn3 137.0(2) . 5_565 ? C35 O18 Mn2 126.4(2) . . ? Mn2 O21 H21B 131.6 . . ? Mn2 O21 H21A 112.7 . . ? H21B O21 H21A 109.5 . . ? Mn2 O22 H22B 114.5 . . ? Mn2 O22 H22A 97.4 . . ? H22B O22 H22A 116.2 . . ? Mn4 O23 H23B 112.3 . . ? Mn4 O23 H23A 121.8 . . ? H23B O23 H23A 119.6 . . ? Mn4 O24 H24B 121.2 . . ? Mn4 O24 H24A 109.5 . . ? H24B O24 H24A 113.0 . . ? C5' N1' C1' 137(6) . . ? C5' N1' Mn3 107(4) . . ? C1' N1' Mn3 116(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 0.2(17) . . . . ? C1 C2 C3 C4 -0.6(17) . . . . ? C2 C3 C4 C5 0.6(17) . . . . ? C3 C4 C5 N1 -0.1(15) . . . . ? C3 C4 C5 C6 180.0(12) . . . . ? N1 C5 C6 N2 19.6(16) . . . . ? C4 C5 C6 N2 -160.5(10) . . . . ? N1 C5 C6 C7 -158.3(11) . . . . ? C4 C5 C6 C7 21.6(19) . . . . ? N2 C6 C7 C8 -0.2(18) . . . . ? C5 C6 C7 C8 177.7(11) . . . . ? C6 C7 C8 C9 1.4(16) . . . . ? C7 C8 C9 C10 -1.5(16) . . . . ? C8 C9 C10 N2 0.3(19) . . . . ? N3 C11 C12 C13 1.0(7) . . . . ? C11 C12 C13 C14 -0.5(7) . . . . ? C12 C13 C14 C15 -0.2(7) . . . . ? C13 C14 C15 N3 0.6(6) . . . . ? C13 C14 C15 C16 -179.3(4) . . . . ? N3 C15 C16 N4 -7.0(4) . . . . ? C14 C15 C16 N4 172.8(3) . . . . ? N3 C15 C16 C17 173.7(3) . . . . ? C14 C15 C16 C17 -6.5(5) . . . . ? N4 C16 C17 C18 -1.2(6) . . . . ? C15 C16 C17 C18 178.1(4) . . . . ? C16 C17 C18 C19 -0.9(6) . . . . ? C17 C18 C19 C20 1.6(7) . . . . ? C18 C19 C20 N4 -0.4(7) . . . . ? O9 C21 C22 C23 180.0(3) . . . . ? O10 C21 C22 C23 0.8(4) . . . . ? O9 C21 C22 C27 -5.2(4) . . . . ? O10 C21 C22 C27 175.6(3) . . . . ? C27 C22 C23 C24 0.6(5) . . . . ? C21 C22 C23 C24 175.6(3) . . . . ? C22 C23 C24 C25 1.1(5) . . . . ? C22 C23 C24 N6 -175.9(3) . . . . ? C23 C24 C25 C26 -1.3(5) . . . . ? N6 C24 C25 C26 175.7(3) . . . . ? C24 C25 C26 C27 -0.3(5) . . . . ? C24 C25 C26 C29 -178.1(3) . . . . ? C25 C26 C27 C22 1.9(5) . . . . ? C29 C26 C27 C22 179.6(3) . . . . ? C25 C26 C27 C28 -178.9(3) . . . . ? C29 C26 C27 C28 -1.2(5) . . . . ? C23 C22 C27 C26 -2.1(4) . . . . ? C21 C22 C27 C26 -176.7(3) . . . . ? C23 C22 C27 C28 178.7(3) . . . . ? C21 C22 C27 C28 4.1(4) . . . . ? C26 C27 C28 O14 -88.3(4) . . . . ? C22 C27 C28 O14 90.9(4) . . . . ? C26 C27 C28 O13 88.0(4) . . . . ? C22 C27 C28 O13 -92.8(4) . . . . ? C25 C26 C29 O16 -46.7(5) . . . . ? C27 C26 C29 O16 135.6(4) . . . . ? C25 C26 C29 O15 130.3(3) . . . . ? C27 C26 C29 O15 -47.4(5) . . . . ? C31 C30 C31 C32 0.2(2) 2 . . . ? N7 C30 C31 C32 -179.8(2) . . . . ? C30 C31 C32 C33 -0.5(5) . . . . ? C30 C31 C32 C35 -178.7(3) . . . . ? C31 C32 C33 C32 0.3(2) . . . 2 ? C35 C32 C33 C32 178.4(4) . . . 2 ? C31 C32 C33 C34 -179.7(2) . . . . ? C35 C32 C33 C34 -1.6(4) . . . . ? C32 C33 C34 O19 94.3(3) 2 . . 2 ? C32 C33 C34 O19 -85.7(3) . . . 2 ? C32 C33 C34 O19 -85.7(3) 2 . . . ? C32 C33 C34 O19 94.3(3) . . . . ? C31 C32 C35 O17' -158.0(16) . . . . ? C33 C32 C35 O17' 23.8(17) . . . . ? C31 C32 C35 O18 -11.7(5) . . . . ? C33 C32 C35 O18 170.1(3) . . . . ? C31 C32 C35 O17 161.0(5) . . . . ? C33 C32 C35 O17 -17.2(6) . . . . ? O1 C36 C37 C38 22.0(4) . . . . ? O2 C36 C37 C38 -158.7(3) . . . . ? O1 C36 C37 C42 -157.9(3) . . . . ? O2 C36 C37 C42 21.4(4) . . . . ? C42 C37 C38 C39 -1.3(5) . . . . ? C36 C37 C38 C39 178.9(3) . . . . ? C37 C38 C39 C40 1.9(5) . . . . ? C37 C38 C39 N5 -178.0(3) . . . . ? C38 C39 C40 C41 -1.3(5) . . . . ? N5 C39 C40 C41 178.5(3) . . . . ? C39 C40 C41 C42 0.2(5) . . . . ? C39 C40 C41 C44 -177.7(3) . . . . ? C38 C37 C42 C41 0.2(4) . . . . ? C36 C37 C42 C41 -180.0(3) . . . . ? C38 C37 C42 C43 179.9(3) . . . . ? C36 C37 C42 C43 -0.2(4) . . . . ? C40 C41 C42 C37 0.4(4) . . . . ? C44 C41 C42 C37 178.2(3) . . . . ? C40 C41 C42 C43 -179.3(3) . . . . ? C44 C41 C42 C43 -1.6(5) . . . . ? C37 C42 C43 O4 87.6(4) . . . . ? C41 C42 C43 O4 -92.6(4) . . . . ? C37 C42 C43 O3 -89.6(3) . . . . ? C41 C42 C43 O3 90.1(3) . . . . ? C40 C41 C44 O7 -11.5(5) . . . . ? C42 C41 C44 O7 170.7(3) . . . . ? C40 C41 C44 O8 168.2(3) . . . . ? C42 C41 C44 O8 -9.6(5) . . . . ? N1' C1' C2' C3' -7(8) . . . . ? C1' C2' C3' C4' 2(9) . . . . ? C2' C3' C4' C5' 1(9) . . . . ? C3' C4' C5' N1' 0(7) . . . . ? C3' C4' C5' C6' 176(7) . . . . ? N1' C5' C6' N2 18(11) . . . . ? C4' C5' C6' N2 -157(4) . . . . ? N1' C5' C6' C7' -160(6) . . . . ? C4' C5' C6' C7' 25(13) . . . . ? N2 C6' C7' C8' 5(10) . . . . ? C5' C6' C7' C8' -177(8) . . . . ? C6' C7' C8' C9' -8(9) . . . . ? C7' C8' C9' C10' 3(8) . . . . ? C8' C9' C10' N2 3(8) . . . . ? C5' C6' N2 C10 179(5) . . . . ? C7' C6' N2 C10 -3(8) . . . . ? C5' C6' N2 C6 13(9) . . . . ? C7' C6' N2 C6 -169(20) . . . . ? C5' C6' N2 C10' -178(5) . . . . ? C7' C6' N2 C10' 1(9) . . . . ? C5' C6' N2 Mn3 -18(8) . . . . ? C7' C6' N2 Mn3 161(5) . . . . ? C9 C10 N2 C6' -4(4) . . . . ? C9 C10 N2 C6 1.0(19) . . . . ? C9 C10 N2 C10' -169(16) . . . . ? C9 C10 N2 Mn3 -167.5(9) . . . . ? C7 C6 N2 C6' 15(13) . . . . ? C5 C6 N2 C6' -163(15) . . . . ? C7 C6 N2 C10 -1.0(17) . . . . ? C5 C6 N2 C10 -178.9(11) . . . . ? C7 C6 N2 C10' 2(4) . . . . ? C5 C6 N2 C10' -176(4) . . . . ? C7 C6 N2 Mn3 169.2(10) . . . . ? C5 C6 N2 Mn3 -8.7(14) . . . . ? C9' C10' N2 C6' -5(8) . . . . ? C9' C10' N2 C10 11(10) . . . . ? C9' C10' N2 C6 -1(8) . . . . ? C9' C10' N2 Mn3 -168(4) . . . . ? O13 Mn3 N2 C6' 175(4) 5_565 . . . ? O15 Mn3 N2 C6' -14(4) 5_565 . . . ? O14 Mn3 N2 C6' -97(4) 1_545 . . . ? O1 Mn3 N2 C6' 89(4) . . . . ? N1 Mn3 N2 C6' 8(4) . . . . ? N1' Mn3 N2 C6' 11(5) . . . . ? O13 Mn3 N2 C10 -25.6(9) 5_565 . . . ? O15 Mn3 N2 C10 145.3(9) 5_565 . . . ? O14 Mn3 N2 C10 62.5(9) 1_545 . . . ? O1 Mn3 N2 C10 -111.7(9) . . . . ? N1 Mn3 N2 C10 167.5(9) . . . . ? N1' Mn3 N2 C10 170.7(17) . . . . ? O13 Mn3 N2 C6 165.3(7) 5_565 . . . ? O15 Mn3 N2 C6 -23.8(9) 5_565 . . . ? O14 Mn3 N2 C6 -106.6(7) 1_545 . . . ? O1 Mn3 N2 C6 79.3(7) . . . . ? N1 Mn3 N2 C6 -1.5(7) . . . . ? N1' Mn3 N2 C6 1.6(16) . . . . ? O13 Mn3 N2 C10' -25(3) 5_565 . . . ? O15 Mn3 N2 C10' 146(3) 5_565 . . . ? O14 Mn3 N2 C10' 63(3) 1_545 . . . ? O1 Mn3 N2 C10' -111(3) . . . . ? N1 Mn3 N2 C10' 168(3) . . . . ? N1' Mn3 N2 C10' 171(3) . . . . ? C2 C1 N1 C5 0.3(17) . . . . ? C2 C1 N1 Mn3 -158.2(9) . . . . ? C4 C5 N1 C1 -0.4(14) . . . . ? C6 C5 N1 C1 179.6(11) . . . . ? C4 C5 N1 Mn3 160.2(8) . . . . ? C6 C5 N1 Mn3 -19.8(11) . . . . ? O13 Mn3 N1 C1 67.9(12) 5_565 . . . ? O15 Mn3 N1 C1 -14.0(9) 5_565 . . . ? O14 Mn3 N1 C1 -113.6(9) 1_545 . . . ? O1 Mn3 N1 C1 79.3(9) . . . . ? N2 Mn3 N1 C1 171.1(10) . . . . ? N1' Mn3 N1 C1 155(10) . . . . ? O13 Mn3 N1 C5 -91.4(12) 5_565 . . . ? O15 Mn3 N1 C5 -173.2(7) 5_565 . . . ? O14 Mn3 N1 C5 87.2(7) 1_545 . . . ? O1 Mn3 N1 C5 -80.0(7) . . . . ? N2 Mn3 N1 C5 11.9(6) . . . . ? N1' Mn3 N1 C5 -4(9) . . . . ? C12 C11 N3 C15 -0.6(6) . . . . ? C12 C11 N3 Mn1 -176.1(3) . . . . ? C14 C15 N3 C11 -0.2(5) . . . . ? C16 C15 N3 C11 179.7(3) . . . . ? C14 C15 N3 Mn1 175.6(3) . . . . ? C16 C15 N3 Mn1 -4.5(4) . . . . ? O10 Mn1 N3 C11 91.5(3) . . . . ? O2 Mn1 N3 C11 -71.4(3) . . . . ? O4 Mn1 N3 C11 176.1(3) 5_565 . . . ? O3 Mn1 N3 C11 10.1(3) . . . . ? N4 Mn1 N3 C11 -175.5(3) . . . . ? O10 Mn1 N3 C15 -84.0(2) . . . . ? O2 Mn1 N3 C15 113.2(2) . . . . ? O4 Mn1 N3 C15 0.7(4) 5_565 . . . ? O3 Mn1 N3 C15 -165.3(2) . . . . ? N4 Mn1 N3 C15 9.0(2) . . . . ? C19 C20 N4 C16 -1.6(6) . . . . ? C19 C20 N4 Mn1 165.3(3) . . . . ? C17 C16 N4 C20 2.3(5) . . . . ? C15 C16 N4 C20 -177.0(3) . . . . ? C17 C16 N4 Mn1 -165.5(3) . . . . ? C15 C16 N4 Mn1 15.2(4) . . . . ? O10 Mn1 N4 C20 -92.6(3) . . . . ? O2 Mn1 N4 C20 92.9(3) . . . . ? O4 Mn1 N4 C20 -3.0(3) 5_565 . . . ? O3 Mn1 N4 C20 -126.6(7) . . . . ? N3 Mn1 N4 C20 -179.8(3) . . . . ? O10 Mn1 N4 C16 74.3(2) . . . . ? O2 Mn1 N4 C16 -100.2(2) . . . . ? O4 Mn1 N4 C16 163.9(3) 5_565 . . . ? O3 Mn1 N4 C16 40.3(9) . . . . ? N3 Mn1 N4 C16 -12.9(2) . . . . ? C40 C39 N5 O6 171.9(3) . . . . ? C38 C39 N5 O6 -8.2(5) . . . . ? C40 C39 N5 O5 -8.4(5) . . . . ? C38 C39 N5 O5 171.5(3) . . . . ? C23 C24 N6 O12 165.5(3) . . . . ? C25 C24 N6 O12 -11.5(5) . . . . ? C23 C24 N6 O11 -14.0(5) . . . . ? C25 C24 N6 O11 168.9(3) . . . . ? C31 C30 N7 O20 15.0(2) 2 . . 2 ? C31 C30 N7 O20 -165.0(2) . . . 2 ? C31 C30 N7 O20 -165.0(2) 2 . . . ? C31 C30 N7 O20 15.0(2) . . . . ? O2 C36 O1 Mn3 5.3(7) . . . . ? C37 C36 O1 Mn3 -175.4(4) . . . . ? O13 Mn3 O1 C36 -66.5(5) 5_565 . . . ? O15 Mn3 O1 C36 -153.0(5) 5_565 . . . ? O14 Mn3 O1 C36 13.7(8) 1_545 . . . ? N2 Mn3 O1 C36 40.2(5) . . . . ? N1 Mn3 O1 C36 116.1(6) . . . . ? N1' Mn3 O1 C36 106.0(14) . . . . ? O1 C36 O2 Mn1 -132.2(3) . . . . ? C37 C36 O2 Mn1 48.5(5) . . . . ? O10 Mn1 O2 C36 -53.5(5) . . . . ? O4 Mn1 O2 C36 -165.0(3) 5_565 . . . ? O3 Mn1 O2 C36 -67.9(3) . . . . ? N4 Mn1 O2 C36 107.7(3) . . . . ? N3 Mn1 O2 C36 35.9(3) . . . . ? O4 C43 O3 Mn2 99.5(3) . . . . ? C42 C43 O3 Mn2 -83.5(3) . . . . ? O4 C43 O3 Mn1 -86.8(3) . . . . ? C42 C43 O3 Mn1 90.2(3) . . . . ? O21 Mn2 O3 C43 -53.9(8) . . . . ? O9 Mn2 O3 C43 -162.0(2) . . . . ? O18 Mn2 O3 C43 91.8(2) . . . . ? O22 Mn2 O3 C43 -76.4(2) . . . . ? O8 Mn2 O3 C43 4.0(2) . . . . ? O21 Mn2 O3 Mn1 133.3(7) . . . . ? O9 Mn2 O3 Mn1 25.26(13) . . . . ? O18 Mn2 O3 Mn1 -80.95(14) . . . . ? O22 Mn2 O3 Mn1 110.87(13) . . . . ? O8 Mn2 O3 Mn1 -168.78(13) . . . . ? O10 Mn1 O3 C43 172.3(2) . . . . ? O2 Mn1 O3 C43 -12.0(2) . . . . ? O4 Mn1 O3 C43 83.7(2) 5_565 . . . ? N4 Mn1 O3 C43 -153.3(7) . . . . ? N3 Mn1 O3 C43 -101.7(2) . . . . ? O10 Mn1 O3 Mn2 -15.13(12) . . . . ? O2 Mn1 O3 Mn2 160.63(14) . . . . ? O4 Mn1 O3 Mn2 -103.73(13) 5_565 . . . ? N4 Mn1 O3 Mn2 19.3(8) . . . . ? N3 Mn1 O3 Mn2 70.91(14) . . . . ? O3 C43 O4 Mn1 12.0(6) . . . 5_565 ? C42 C43 O4 Mn1 -164.9(3) . . . 5_565 ? O8 C44 O7 Mn4 0.3(6) . . . . ? C41 C44 O7 Mn4 180.0(2) . . . . ? O23 Mn4 O7 C44 -83.2(3) . . . . ? O23 Mn4 O7 C44 96.8(3) 7_465 . . . ? O24 Mn4 O7 C44 -171.1(3) . . . . ? O24 Mn4 O7 C44 8.9(3) 7_465 . . . ? O7 Mn4 O7 C44 106(100) 7_465 . . . ? O7 C44 O8 Mn2 116.2(3) . . . . ? C41 C44 O8 Mn2 -63.5(4) . . . . ? O21 Mn2 O8 C44 -104.5(3) . . . . ? O9 Mn2 O8 C44 158.1(3) . . . . ? O18 Mn2 O8 C44 -12.8(3) . . . . ? O22 Mn2 O8 C44 169.4(3) . . . . ? O3 Mn2 O8 C44 81.3(3) . . . . ? O10 C21 O9 Mn2 -49.7(4) . . . . ? C22 C21 O9 Mn2 131.2(2) . . . . ? O21 Mn2 O9 C21 -171.1(2) . . . . ? O18 Mn2 O9 C21 97.4(2) . . . . ? O22 Mn2 O9 C21 -84.3(2) . . . . ? O8 Mn2 O9 C21 -73.2(4) . . . . ? O3 Mn2 O9 C21 2.3(2) . . . . ? O9 C21 O10 Mn1 82.0(4) . . . . ? C22 C21 O10 Mn1 -99.0(3) . . . . ? O2 Mn1 O10 C21 -51.4(5) . . . . ? O4 Mn1 O10 C21 61.0(3) 5_565 . . . ? O3 Mn1 O10 C21 -37.1(3) . . . . ? N4 Mn1 O10 C21 146.8(3) . . . . ? N3 Mn1 O10 C21 -141.3(3) . . . . ? O14 C28 O13 Mn3 116.2(3) . . . 5_565 ? C27 C28 O13 Mn3 -59.7(3) . . . 5_565 ? O13 C28 O14 Mn3 -15.9(4) . . . 1_565 ? C27 C28 O14 Mn3 160.0(2) . . . 1_565 ? O16 C29 O15 Mn3 171.7(3) . . . 5_565 ? C26 C29 O15 Mn3 -5.1(5) . . . 5_565 ? O17' C35 O18 Mn2 -45.5(17) . . . . ? O17 C35 O18 Mn2 -5.4(8) . . . . ? C32 C35 O18 Mn2 166.4(2) . . . . ? O21 Mn2 O18 C35 4.9(3) . . . . ? O9 Mn2 O18 C35 94.0(3) . . . . ? O22 Mn2 O18 C35 -77.8(6) . . . . ? O8 Mn2 O18 C35 -88.3(3) . . . . ? O3 Mn2 O18 C35 -171.3(3) . . . . ? C6' C5' N1' C1' 178(8) . . . . ? C4' C5' N1' C1' -7(9) . . . . ? C6' C5' N1' Mn3 -10(9) . . . . ? C4' C5' N1' Mn3 165(3) . . . . ? C2' C1' N1' C5' 11(10) . . . . ? C2' C1' N1' Mn3 -161(4) . . . . ? O13 Mn3 N1' C5' -69(7) 5_565 . . . ? O15 Mn3 N1' C5' 173(3) 5_565 . . . ? O14 Mn3 N1' C5' 72(3) 1_545 . . . ? O1 Mn3 N1' C5' -95(3) . . . . ? N2 Mn3 N1' C5' -1(3) . . . . ? N1 Mn3 N1' C5' 162(12) . . . . ? O13 Mn3 N1' C1' 105(5) 5_565 . . . ? O15 Mn3 N1' C1' -13(5) 5_565 . . . ? O14 Mn3 N1' C1' -115(4) 1_545 . . . ? O1 Mn3 N1' C1' 78(4) . . . . ? N2 Mn3 N1' C1' 173(5) . . . . ? N1 Mn3 N1' C1' -24(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.834 _refine_diff_density_min -0.537 _refine_diff_density_rms 0.118 _database_code_depnum_ccdc_archive 'CCDC 910423' ####################################################################### # # 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_shelx _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H29 Mn4 N9 O27' _chemical_formula_weight 1311.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 12.273(8) _cell_length_b 13.134(8) _cell_length_c 15.830(9) _cell_angle_alpha 95.556(11) _cell_angle_beta 94.659(6) _cell_angle_gamma 107.710(10) _cell_volume 2403(3) _cell_formula_units_Z 2 _cell_measurement_temperature 386(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.813 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 1.135 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8048 _exptl_absorpt_correction_T_max 0.8048 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 386(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17992 _diffrn_reflns_av_R_equivalents 0.0779 _diffrn_reflns_av_sigmaI/netI 0.1578 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8428 _reflns_number_gt 4637 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8428 _refine_ls_number_parameters 739 _refine_ls_number_restraints 117 _refine_ls_R_factor_all 0.0931 _refine_ls_R_factor_gt 0.0707 _refine_ls_wR_factor_ref 0.1652 _refine_ls_wR_factor_gt 0.1552 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0192(6) 0.1035(5) 0.3810(4) 0.0194(15) Uani 1 1 d U . . C2 C 0.0882(6) 0.2056(5) 0.3514(4) 0.0220(16) Uani 1 1 d U . . C3 C 0.2040(6) 0.2585(5) 0.3813(4) 0.0191(15) Uani 1 1 d U . . C4 C 0.2617(6) 0.3593(5) 0.3561(4) 0.0178(15) Uani 1 1 d . . . C5 C 0.2002(6) 0.4039(5) 0.2995(4) 0.0219(16) Uani 1 1 d U . . H5 H 0.2361 0.4708 0.2828 0.026 Uiso 1 1 calc R . . C6 C 0.0885(6) 0.3496(5) 0.2689(4) 0.0193(15) Uani 1 1 d U . . C7 C 0.0292(6) 0.2498(5) 0.2939(4) 0.0213(16) Uani 1 1 d U . . H7 H -0.0473 0.2141 0.2726 0.026 Uiso 1 1 calc R . . C8 C 0.2691(6) 0.1994(5) 0.4340(4) 0.0214(16) Uani 1 1 d U . . C9 C 0.3857(6) 0.4240(5) 0.3905(4) 0.0175(16) Uani 1 1 d . . . C10 C 0.5053(6) -0.0532(4) 0.3340(4) 0.0161(15) Uani 1 1 d U . . C11 C 0.5050(6) -0.0925(5) 0.2405(4) 0.0214(16) Uani 1 1 d . . . C12 C 0.5770(6) -0.1526(4) 0.2159(4) 0.0186(16) Uani 1 1 d . . . C13 C 0.5777(6) -0.1818(5) 0.1269(4) 0.0199(16) Uani 1 1 d . . . C14 C 0.5045(6) -0.1575(5) 0.0673(4) 0.0237(17) Uani 1 1 d . . . H14 H 0.5020 -0.1805 0.0095 0.028 Uiso 1 1 calc R . . C15 C 0.4334(6) -0.0976(5) 0.0946(4) 0.0271(18) Uani 1 1 d . . . C16 C 0.4345(6) -0.0649(5) 0.1810(4) 0.0216(16) Uani 1 1 d . . . H16 H 0.3878 -0.0247 0.1984 0.026 Uiso 1 1 calc R . . C17 C 0.6421(6) -0.1911(5) 0.2833(4) 0.0158(15) Uani 1 1 d . . . C18 C 0.6663(6) -0.2296(5) 0.0923(4) 0.0206(16) Uani 1 1 d . . . C19 C 0.0226(6) -0.1543(5) 0.3165(4) 0.0212(17) Uani 1 1 d . . . C20 C 0.1264(6) -0.1976(4) 0.3181(4) 0.0144(15) Uani 1 1 d . . . C21 C 0.2003(6) -0.1895(5) 0.3917(4) 0.0201(16) Uani 1 1 d U . . C22 C 0.2904(6) -0.2334(4) 0.3873(4) 0.0159(15) Uani 1 1 d . . . C23 C 0.3065(6) -0.2873(4) 0.3096(4) 0.0191(16) Uani 1 1 d U . . H23 H 0.3622 -0.3219 0.3072 0.023 Uiso 1 1 calc R . . C24 C 0.2342(6) -0.2858(5) 0.2365(4) 0.0158(15) Uani 1 1 d . . . C25 C 0.1801(5) -0.1444(5) 0.4808(4) 0.0137(15) Uani 1 1 d . . . C26 C 0.1486(6) -0.2416(5) 0.2389(4) 0.0236(17) Uani 1 1 d . . . H26 H 0.1045 -0.2400 0.1887 0.028 Uiso 1 1 calc R . . C27 C 0.3911(6) -0.2083(5) 0.4570(4) 0.0207(16) Uani 1 1 d U . . C28 C 0.0985(7) 0.0660(6) 0.1311(5) 0.036(2) Uani 1 1 d . . . H28 H 0.1443 0.0344 0.1619 0.043 Uiso 1 1 calc R . . C29 C 0.1362(7) 0.1385(6) 0.0763(5) 0.036(2) Uani 1 1 d . . . H29 H 0.2111 0.1652 0.0626 0.043 Uiso 1 1 calc R . . C30 C -0.0461(7) 0.1080(5) 0.0823(4) 0.0302(19) Uani 1 1 d . . . H30 H -0.1206 0.1114 0.0727 0.036 Uiso 1 1 calc R . . C31 C 0.0350(6) 0.2375(5) -0.0193(4) 0.0264(17) Uani 1 1 d . . . H31A H -0.0439 0.2381 -0.0288 0.032 Uiso 1 1 calc R . . H31B H 0.0546 0.2095 -0.0729 0.032 Uiso 1 1 calc R . . C32 C 0.1136(7) 0.3522(5) 0.0067(4) 0.0299(19) Uani 1 1 d . . . H32A H 0.1933 0.3533 0.0106 0.036 Uiso 1 1 calc R . . H32B H 0.0990 0.3788 0.0626 0.036 Uiso 1 1 calc R . . C33 C 0.0937(6) 0.4264(5) -0.0587(4) 0.0301(18) Uani 1 1 d . . . H33A H 0.0115 0.4082 -0.0753 0.036 Uiso 1 1 calc R . . H33B H 0.1209 0.5003 -0.0311 0.036 Uiso 1 1 calc R . . C34 C 0.1531(6) 0.4196(5) -0.1390(4) 0.0255(18) Uani 1 1 d . . . H34A H 0.1346 0.3445 -0.1624 0.031 Uiso 1 1 calc R . . H34B H 0.1232 0.4559 -0.1813 0.031 Uiso 1 1 calc R . . C35 C 0.3539(7) 0.4461(6) -0.1772(4) 0.0323(19) Uani 1 1 d U . . H35 H 0.3343 0.3970 -0.2267 0.039 Uiso 1 1 calc R . . C36 C 0.4604(7) 0.5080(5) -0.1459(4) 0.0327(19) Uani 1 1 d . . . H36 H 0.5279 0.5107 -0.1697 0.039 Uiso 1 1 calc R . . C37 C 0.3408(7) 0.5427(5) -0.0604(4) 0.0306(19) Uani 1 1 d . . . H37 H 0.3112 0.5731 -0.0158 0.037 Uiso 1 1 calc R . . C38 C 0.6814(7) 0.4608(5) 0.3571(5) 0.035(2) Uani 1 1 d . . . H38 H 0.6101 0.4088 0.3407 0.042 Uiso 1 1 calc R . . C39 C 0.7833(7) 0.4465(5) 0.3478(4) 0.0297(19) Uani 1 1 d . . . H39 H 0.7953 0.3839 0.3237 0.036 Uiso 1 1 calc R . . C40 C 0.8100(6) 0.6085(5) 0.4088(4) 0.0201(16) Uani 1 1 d U . . H40 H 0.8468 0.6783 0.4353 0.024 Uiso 1 1 calc R . . C41 C 0.9901(6) 0.5604(5) 0.3953(4) 0.0269(18) Uani 1 1 d . . . H41A H 1.0278 0.6354 0.4179 0.032 Uiso 1 1 calc R . . H41B H 1.0187 0.5470 0.3413 0.032 Uiso 1 1 calc R . . C42 C 1.0214(6) 0.4893(5) 0.4574(3) 0.0270(18) Uani 1 1 d . . . H42A H 0.9866 0.4141 0.4342 0.032 Uiso 1 1 calc R . . H42B H 1.1043 0.5046 0.4653 0.032 Uiso 1 1 calc R . . H1W H -0.2843 0.0616 0.1520 0.040 Uiso 1 1 d RD . . H2W H -0.2556 0.0933 0.2301 0.040 Uiso 1 1 d RD . . Mn1 Mn -0.13528(9) -0.05323(7) 0.21449(6) 0.0190(3) Uani 1 1 d . . . Mn2 Mn 0.14349(9) 0.07483(7) 0.57122(6) 0.0177(3) Uani 1 1 d . . . Mn3 Mn 0.39194(9) 0.04340(7) 0.47383(6) 0.0184(3) Uani 1 1 d . . . Mn4 Mn 0.56933(9) 0.64423(7) 0.42383(6) 0.0189(3) Uani 1 1 d . . . N1 N -0.0157(5) 0.0464(4) 0.1345(3) 0.0241(14) Uani 1 1 d . . . N2 N 0.0424(5) 0.1649(4) 0.0447(3) 0.0241(14) Uani 1 1 d . . . N3 N 0.2776(5) 0.4673(4) -0.1236(3) 0.0249(14) Uani 1 1 d . . . N4 N 0.4513(6) 0.5678(4) -0.0707(4) 0.0329(16) Uani 1 1 d . . . N5 N 0.6984(5) 0.5657(4) 0.3951(3) 0.0217(14) Uani 1 1 d . . . N6 N 0.8666(5) 0.5410(4) 0.3803(3) 0.0286(15) Uani 1 1 d . . . N7 N 0.0252(5) 0.3975(5) 0.2111(3) 0.0255(14) Uani 1 1 d . . . N8 N 0.3591(6) -0.0709(5) 0.0316(4) 0.0336(16) Uani 1 1 d . . . N9 N 0.2561(5) -0.3354(4) 0.1539(3) 0.0223(14) Uani 1 1 d . . . O1 O -0.0776(4) 0.0487(3) 0.3390(3) 0.0210(11) Uani 1 1 d . . . O2 O 0.0533(4) 0.0747(3) 0.4486(2) 0.0213(11) Uani 1 1 d U . . O3 O 0.3136(4) 0.1376(3) 0.3957(3) 0.0202(11) Uani 1 1 d . . . O4 O 0.2736(4) 0.2118(3) 0.5162(2) 0.0170(11) Uani 1 1 d U . . O5 O 0.4349(4) 0.3848(3) 0.4452(3) 0.0177(11) Uani 1 1 d . . . O6 O 0.4263(4) 0.5112(3) 0.3611(3) 0.0210(11) Uani 1 1 d . . . O7 O 0.0758(4) 0.4898(3) 0.1951(3) 0.0279(12) Uani 1 1 d . . . O8 O -0.0722(4) 0.3451(4) 0.1796(3) 0.0327(13) Uani 1 1 d . . . O9 O 0.4306(4) -0.0083(3) 0.3502(3) 0.0214(11) Uani 1 1 d . . . O10 O 0.5757(4) -0.0722(3) 0.3874(3) 0.0200(11) Uani 1 1 d . . . O11 O 0.7476(4) -0.1406(3) 0.3069(2) 0.0156(10) Uani 1 1 d . . . O12 O 0.5860(4) -0.2775(3) 0.3091(2) 0.0172(11) Uani 1 1 d . . . O13 O 0.7663(4) -0.1938(3) 0.1292(3) 0.0219(11) Uani 1 1 d . . . O14 O 0.6343(4) -0.2974(3) 0.0256(3) 0.0292(12) Uani 1 1 d . . . O15 O 0.3596(5) -0.1031(4) -0.0445(3) 0.0463(16) Uani 1 1 d . . . O16 O 0.2997(6) -0.0153(5) 0.0531(3) 0.0579(18) Uani 1 1 d . . . O17 O -0.0093(4) -0.1301(3) 0.2476(3) 0.0249(12) Uani 1 1 d . . . O18 O -0.0233(4) -0.1566(3) 0.3853(2) 0.0178(11) Uani 1 1 d . . . O19 O 0.2124(4) -0.0378(3) 0.4942(2) 0.0165(10) Uani 1 1 d . . . O20 O 0.1372(4) -0.2061(3) 0.5278(3) 0.0223(11) Uani 1 1 d . . . O21 O 0.4124(4) -0.1188(3) 0.5036(2) 0.0174(11) Uani 1 1 d . . . O22 O 0.4477(4) -0.2716(3) 0.4625(3) 0.0177(11) Uani 1 1 d . . . O23 O 0.3219(4) -0.3896(4) 0.1547(3) 0.0320(12) Uani 1 1 d U . . O24 O 0.2101(4) -0.3162(3) 0.0880(3) 0.0288(12) Uani 1 1 d . . . O25 O -0.2425(4) 0.0489(3) 0.1925(2) 0.0252(12) Uani 1 1 d D . . O26 O 0.7309(5) 0.1820(3) 0.3175(3) 0.0392(15) Uani 1 1 d . . . O27 O 0.4749(5) 0.7789(4) 0.6750(4) 0.0625(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.018(3) 0.021(3) 0.019(3) -0.009(2) 0.009(2) 0.007(2) C2 0.024(3) 0.020(3) 0.020(3) -0.014(3) 0.005(3) 0.008(3) C3 0.019(3) 0.023(3) 0.014(2) -0.010(2) 0.004(2) 0.009(2) C4 0.016(4) 0.021(4) 0.013(3) -0.011(3) 0.003(3) 0.006(3) C5 0.026(4) 0.022(3) 0.019(3) -0.007(3) 0.010(3) 0.011(3) C6 0.019(3) 0.022(3) 0.018(3) -0.010(3) 0.008(3) 0.009(3) C7 0.021(3) 0.023(3) 0.018(3) -0.012(3) 0.007(3) 0.009(3) C8 0.012(3) 0.022(3) 0.023(3) -0.007(3) 0.009(3) -0.003(3) C9 0.027(4) 0.012(3) 0.016(3) -0.002(3) 0.010(3) 0.009(3) C10 0.025(3) 0.007(3) 0.019(3) 0.009(2) 0.004(3) 0.005(2) C11 0.021(4) 0.017(3) 0.022(4) -0.013(3) 0.009(3) 0.004(3) C12 0.027(4) 0.007(3) 0.021(3) 0.009(3) 0.006(3) 0.000(3) C13 0.016(4) 0.028(4) 0.014(3) -0.008(3) 0.009(3) 0.006(3) C14 0.030(5) 0.021(4) 0.020(4) -0.010(3) 0.007(3) 0.010(3) C15 0.030(5) 0.033(4) 0.019(4) -0.002(3) 0.006(3) 0.012(4) C16 0.030(5) 0.017(3) 0.018(3) -0.002(3) 0.009(3) 0.008(3) C17 0.032(5) 0.009(3) 0.014(3) 0.004(3) 0.014(3) 0.013(3) C18 0.023(4) 0.030(4) 0.013(3) -0.001(3) 0.005(3) 0.013(3) C19 0.019(4) 0.022(4) 0.014(3) -0.014(3) -0.005(3) -0.001(3) C20 0.024(4) 0.005(3) 0.014(3) 0.000(3) 0.004(3) 0.003(3) C21 0.015(3) 0.023(3) 0.021(3) -0.012(3) 0.006(3) 0.008(3) C22 0.031(4) 0.007(3) 0.012(3) 0.005(3) 0.001(3) 0.008(3) C23 0.023(3) 0.014(3) 0.020(3) -0.007(2) 0.007(3) 0.008(3) C24 0.025(4) 0.010(3) 0.013(3) 0.002(3) 0.011(3) 0.005(3) C25 0.014(4) 0.017(3) 0.013(3) 0.006(3) 0.000(3) 0.008(3) C26 0.021(4) 0.024(4) 0.018(3) -0.012(3) 0.003(3) 0.001(3) C27 0.021(3) 0.027(3) 0.012(3) -0.006(3) 0.006(3) 0.007(3) C28 0.046(6) 0.037(5) 0.035(4) 0.011(4) 0.010(4) 0.027(4) C29 0.031(5) 0.047(5) 0.041(5) 0.022(4) 0.025(4) 0.019(4) C30 0.035(5) 0.036(4) 0.022(4) 0.005(3) 0.006(4) 0.013(4) C31 0.029(5) 0.037(4) 0.018(3) -0.001(3) 0.012(3) 0.017(4) C32 0.043(5) 0.027(4) 0.022(4) -0.005(3) 0.013(4) 0.014(4) C33 0.034(5) 0.032(4) 0.026(4) -0.005(3) 0.006(4) 0.015(4) C34 0.037(5) 0.023(4) 0.019(4) 0.006(3) 0.002(3) 0.013(3) C35 0.035(4) 0.037(3) 0.025(3) -0.010(3) 0.014(3) 0.012(3) C36 0.034(5) 0.034(4) 0.031(4) -0.007(3) 0.017(4) 0.012(4) C37 0.036(5) 0.037(4) 0.017(4) -0.006(3) 0.004(4) 0.012(4) C38 0.025(5) 0.024(4) 0.049(5) -0.013(4) -0.006(4) 0.006(3) C39 0.042(5) 0.012(4) 0.034(4) -0.002(3) 0.000(4) 0.010(3) C40 0.032(4) 0.017(3) 0.017(3) 0.010(3) 0.005(3) 0.013(3) C41 0.024(5) 0.026(4) 0.027(4) -0.013(3) 0.013(3) 0.005(3) C42 0.031(5) 0.031(4) 0.020(4) -0.008(3) 0.010(4) 0.014(3) Mn1 0.0237(7) 0.0200(5) 0.0129(5) -0.0067(4) 0.0054(5) 0.0082(5) Mn2 0.0225(6) 0.0176(5) 0.0125(5) -0.0075(4) 0.0063(5) 0.0075(5) Mn3 0.0228(6) 0.0187(5) 0.0134(5) -0.0081(4) 0.0056(5) 0.0082(5) Mn4 0.0228(7) 0.0173(5) 0.0156(5) -0.0069(4) 0.0045(5) 0.0069(5) N1 0.034(4) 0.024(3) 0.020(3) 0.001(3) 0.015(3) 0.014(3) N2 0.027(4) 0.022(3) 0.023(3) 0.004(3) 0.009(3) 0.005(3) N3 0.032(4) 0.025(3) 0.018(3) -0.002(3) 0.008(3) 0.011(3) N4 0.039(4) 0.030(3) 0.028(3) -0.009(3) 0.008(3) 0.010(3) N5 0.027(4) 0.013(3) 0.024(3) -0.006(2) 0.003(3) 0.008(3) N6 0.028(4) 0.030(3) 0.027(3) -0.017(3) 0.005(3) 0.015(3) N7 0.019(4) 0.034(4) 0.020(3) -0.015(3) 0.008(3) 0.007(3) N8 0.040(5) 0.043(4) 0.019(3) -0.006(3) 0.000(3) 0.020(3) N9 0.027(4) 0.024(3) 0.016(3) -0.006(3) 0.003(3) 0.011(3) O1 0.021(3) 0.020(2) 0.017(2) -0.0122(19) 0.005(2) 0.002(2) O2 0.025(2) 0.023(2) 0.0113(19) -0.0105(17) 0.0038(18) 0.0049(18) O3 0.024(3) 0.021(2) 0.016(2) -0.0074(19) 0.008(2) 0.010(2) O4 0.032(3) 0.010(2) 0.0104(19) 0.0085(17) 0.0042(19) 0.0073(19) O5 0.026(3) 0.013(2) 0.017(2) 0.0060(19) 0.003(2) 0.008(2) O6 0.023(3) 0.019(2) 0.020(2) 0.003(2) 0.004(2) 0.006(2) O7 0.033(3) 0.018(2) 0.029(3) -0.003(2) 0.006(2) 0.004(2) O8 0.026(3) 0.037(3) 0.035(3) -0.002(2) 0.003(3) 0.012(3) O9 0.026(3) 0.024(3) 0.016(2) -0.0090(19) 0.007(2) 0.013(2) O10 0.030(3) 0.014(2) 0.018(2) -0.002(2) 0.005(2) 0.010(2) O11 0.018(3) 0.019(2) 0.011(2) -0.0024(18) 0.003(2) 0.008(2) O12 0.029(3) 0.014(2) 0.010(2) 0.0000(18) 0.006(2) 0.007(2) O13 0.026(3) 0.024(2) 0.017(2) -0.005(2) 0.007(2) 0.010(2) O14 0.035(3) 0.029(3) 0.022(3) -0.014(2) 0.005(2) 0.013(2) O15 0.067(4) 0.073(4) 0.013(3) -0.007(3) 0.000(3) 0.047(3) O16 0.078(5) 0.093(5) 0.027(3) -0.009(3) 0.002(3) 0.070(4) O17 0.025(3) 0.030(3) 0.020(3) -0.010(2) 0.006(2) 0.012(2) O18 0.028(3) 0.014(2) 0.014(2) 0.0017(18) 0.004(2) 0.009(2) O19 0.023(3) 0.011(2) 0.018(2) 0.0016(18) 0.009(2) 0.007(2) O20 0.030(3) 0.019(2) 0.017(2) -0.007(2) 0.011(2) 0.008(2) O21 0.029(3) 0.007(2) 0.012(2) -0.0010(18) 0.004(2) -0.001(2) O22 0.029(3) 0.010(2) 0.018(2) 0.0024(19) 0.004(2) 0.012(2) O23 0.034(3) 0.037(3) 0.029(2) -0.014(2) 0.005(2) 0.023(2) O24 0.039(3) 0.035(3) 0.016(2) -0.007(2) 0.005(2) 0.019(2) O25 0.036(3) 0.024(3) 0.018(2) 0.001(2) 0.008(2) 0.013(2) O26 0.070(4) 0.026(3) 0.024(3) -0.007(2) 0.002(3) 0.023(3) O27 0.061(5) 0.064(4) 0.066(4) -0.003(3) 0.025(4) 0.024(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 C1 O2 1.252(7) . ? C1 O1 1.276(7) . ? C1 C2 1.494(9) . ? C2 C7 1.394(9) . ? C2 C3 1.397(9) . ? C3 C4 1.411(8) . ? C3 C8 1.527(9) . ? C4 C5 1.406(9) . ? C4 C9 1.525(9) . ? C5 C6 1.362(9) . ? C5 H5 0.9300 . ? C6 C7 1.404(8) . ? C6 N7 1.459(8) . ? C7 H7 0.9300 . ? C8 O3 1.246(8) . ? C8 O4 1.290(7) . ? C9 O5 1.252(7) . ? C9 O6 1.253(7) . ? C10 O10 1.255(7) . ? C10 O9 1.262(8) . ? C10 C11 1.518(8) . ? C11 C16 1.375(9) . ? C11 C12 1.407(9) . ? C12 C13 1.425(8) . ? C12 C17 1.499(9) . ? C13 C14 1.376(9) . ? C13 C18 1.523(9) . ? C14 C15 1.407(9) . ? C14 H14 0.9300 . ? C15 C16 1.391(9) . ? C15 N8 1.436(9) . ? C16 H16 0.9300 . ? C17 O12 1.259(6) . ? C17 O11 1.268(7) . ? C18 O13 1.244(7) . ? C18 O14 1.265(7) . ? C19 O17 1.232(7) . ? C19 O18 1.265(8) . ? C19 C20 1.545(9) . ? C20 C21 1.391(8) . ? C20 C26 1.412(8) . ? C21 C22 1.396(9) . ? C21 C25 1.545(8) . ? C22 C23 1.418(8) . ? C22 C27 1.522(9) . ? C23 C24 1.407(8) . ? C23 H23 0.9300 . ? C24 C26 1.347(9) . ? C24 N9 1.485(8) . ? C25 O20 1.188(7) . ? C25 O19 1.324(7) . ? C26 H26 0.9300 . ? C27 O22 1.240(8) . ? C27 O21 1.268(7) . ? C28 N1 1.352(9) . ? C28 C29 1.353(9) . ? C28 H28 0.9300 . ? C29 N2 1.370(9) . ? C29 H29 0.9300 . ? C30 N1 1.319(8) . ? C30 N2 1.338(9) . ? C30 H30 0.9300 . ? C31 N2 1.473(8) . ? C31 C32 1.517(8) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.543(8) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.525(9) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 N3 1.454(9) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.337(9) . ? C35 N3 1.384(9) . ? C35 H35 0.9300 . ? C36 N4 1.392(9) . ? C36 H36 0.9300 . ? C37 N4 1.323(9) . ? C37 N3 1.341(8) . ? C37 H37 0.9300 . ? C38 C39 1.338(10) . ? C38 N5 1.396(8) . ? C38 H38 0.9300 . ? C39 N6 1.367(8) . ? C39 H39 0.9300 . ? C40 N5 1.304(8) . ? C40 N6 1.349(8) . ? C40 H40 0.9300 . ? C41 N6 1.454(9) . ? C41 C42 1.522(8) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C42 1.519(11) 2_766 ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? Mn1 O13 2.142(4) 1_455 ? Mn1 O17 2.146(5) . ? Mn1 O25 2.178(4) . ? Mn1 O1 2.205(4) . ? Mn1 N1 2.219(5) . ? Mn1 O11 2.278(4) 1_455 ? Mn2 O2 2.154(4) . ? Mn2 O18 2.188(5) 2_556 ? Mn2 O11 2.193(4) 2_656 ? Mn2 O19 2.229(4) . ? Mn2 O1 2.268(4) 2_556 ? Mn2 O4 2.308(4) . ? Mn3 O9 2.147(4) . ? Mn3 O10 2.175(4) 2_656 ? Mn3 O3 2.193(4) . ? Mn3 O19 2.202(4) . ? Mn3 O21 2.284(5) 2_656 ? Mn3 O21 2.307(4) . ? Mn4 O5 2.146(4) 2_666 ? Mn4 O6 2.153(4) . ? Mn4 O12 2.167(4) 1_565 ? Mn4 N5 2.190(6) . ? Mn4 O22 2.201(5) 1_565 ? Mn4 O4 2.309(4) 2_666 ? N7 O8 1.221(7) . ? N7 O7 1.243(6) . ? N8 O16 1.224(8) . ? N8 O15 1.238(7) . ? N9 O23 1.230(7) . ? N9 O24 1.229(6) . ? O1 Mn2 2.268(4) 2_556 ? O4 Mn4 2.309(4) 2_666 ? O5 Mn4 2.146(4) 2_666 ? O10 Mn3 2.175(4) 2_656 ? O11 Mn2 2.193(4) 2_656 ? O11 Mn1 2.278(4) 1_655 ? O12 Mn4 2.167(4) 1_545 ? O13 Mn1 2.142(4) 1_655 ? O18 Mn2 2.188(5) 2_556 ? O21 Mn3 2.284(5) 2_656 ? O22 Mn4 2.201(5) 1_545 ? O25 H1W 0.8483 . ? O25 H2W 0.8516 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 O1 120.3(6) . . ? O2 C1 C2 120.2(6) . . ? O1 C1 C2 119.4(6) . . ? C7 C2 C3 120.5(6) . . ? C7 C2 C1 116.1(6) . . ? C3 C2 C1 123.3(6) . . ? C2 C3 C4 120.5(6) . . ? C2 C3 C8 118.3(5) . . ? C4 C3 C8 120.9(6) . . ? C5 C4 C3 118.3(6) . . ? C5 C4 C9 118.7(5) . . ? C3 C4 C9 123.0(6) . . ? C6 C5 C4 120.4(6) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 122.2(6) . . ? C5 C6 N7 119.8(6) . . ? C7 C6 N7 118.0(6) . . ? C2 C7 C6 118.1(6) . . ? C2 C7 H7 121.0 . . ? C6 C7 H7 121.0 . . ? O3 C8 O4 121.8(6) . . ? O3 C8 C3 118.5(6) . . ? O4 C8 C3 119.6(6) . . ? O5 C9 O6 127.5(6) . . ? O5 C9 C4 116.7(5) . . ? O6 C9 C4 115.8(5) . . ? O10 C10 O9 126.5(6) . . ? O10 C10 C11 117.6(6) . . ? O9 C10 C11 115.8(6) . . ? C16 C11 C12 121.3(6) . . ? C16 C11 C10 117.9(6) . . ? C12 C11 C10 120.8(6) . . ? C11 C12 C13 118.2(6) . . ? C11 C12 C17 119.2(6) . . ? C13 C12 C17 122.5(6) . . ? C14 C13 C12 120.6(6) . . ? C14 C13 C18 116.5(5) . . ? C12 C13 C18 122.6(6) . . ? C13 C14 C15 119.4(6) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 120.8(7) . . ? C16 C15 N8 120.4(7) . . ? C14 C15 N8 118.8(6) . . ? C11 C16 C15 119.6(7) . . ? C11 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? O12 C17 O11 124.9(6) . . ? O12 C17 C12 115.1(6) . . ? O11 C17 C12 119.9(5) . . ? O13 C18 O14 125.1(7) . . ? O13 C18 C13 117.1(6) . . ? O14 C18 C13 117.6(6) . . ? O17 C19 O18 128.9(7) . . ? O17 C19 C20 116.4(6) . . ? O18 C19 C20 114.4(6) . . ? C21 C20 C26 119.9(6) . . ? C21 C20 C19 123.4(6) . . ? C26 C20 C19 116.6(6) . . ? C20 C21 C22 119.3(6) . . ? C20 C21 C25 122.7(6) . . ? C22 C21 C25 117.7(6) . . ? C21 C22 C23 121.1(6) . . ? C21 C22 C27 123.7(6) . . ? C23 C22 C27 114.0(6) . . ? C24 C23 C22 116.7(6) . . ? C24 C23 H23 121.7 . . ? C22 C23 H23 121.7 . . ? C26 C24 C23 123.0(6) . . ? C26 C24 N9 120.1(6) . . ? C23 C24 N9 116.9(6) . . ? O20 C25 O19 127.8(6) . . ? O20 C25 C21 118.6(5) . . ? O19 C25 C21 113.6(5) . . ? C24 C26 C20 119.6(6) . . ? C24 C26 H26 120.2 . . ? C20 C26 H26 120.2 . . ? O22 C27 O21 125.2(6) . . ? O22 C27 C22 119.8(6) . . ? O21 C27 C22 114.8(6) . . ? N1 C28 C29 110.0(6) . . ? N1 C28 H28 125.0 . . ? C29 C28 H28 125.0 . . ? C28 C29 N2 106.5(7) . . ? C28 C29 H29 126.7 . . ? N2 C29 H29 126.7 . . ? N1 C30 N2 112.3(7) . . ? N1 C30 H30 123.8 . . ? N2 C30 H30 123.8 . . ? N2 C31 C32 113.4(5) . . ? N2 C31 H31A 108.9 . . ? C32 C31 H31A 108.9 . . ? N2 C31 H31B 108.9 . . ? C32 C31 H31B 108.9 . . ? H31A C31 H31B 107.7 . . ? C31 C32 C33 110.8(5) . . ? C31 C32 H32A 109.5 . . ? C33 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C33 C32 H32B 109.5 . . ? H32A C32 H32B 108.1 . . ? C34 C33 C32 114.5(6) . . ? C34 C33 H33A 108.6 . . ? C32 C33 H33A 108.6 . . ? C34 C33 H33B 108.6 . . ? C32 C33 H33B 108.6 . . ? H33A C33 H33B 107.6 . . ? N3 C34 C33 113.2(6) . . ? N3 C34 H34A 108.9 . . ? C33 C34 H34A 108.9 . . ? N3 C34 H34B 108.9 . . ? C33 C34 H34B 108.9 . . ? H34A C34 H34B 107.8 . . ? C36 C35 N3 108.5(6) . . ? C36 C35 H35 125.7 . . ? N3 C35 H35 125.7 . . ? C35 C36 N4 107.0(7) . . ? C35 C36 H36 126.5 . . ? N4 C36 H36 126.5 . . ? N4 C37 N3 110.2(7) . . ? N4 C37 H37 124.9 . . ? N3 C37 H37 124.9 . . ? C39 C38 N5 109.6(6) . . ? C39 C38 H38 125.2 . . ? N5 C38 H38 125.2 . . ? C38 C39 N6 107.3(7) . . ? C38 C39 H39 126.3 . . ? N6 C39 H39 126.3 . . ? N5 C40 N6 113.1(6) . . ? N5 C40 H40 123.5 . . ? N6 C40 H40 123.5 . . ? N6 C41 C42 112.5(6) . . ? N6 C41 H41A 109.1 . . ? C42 C41 H41A 109.1 . . ? N6 C41 H41B 109.1 . . ? C42 C41 H41B 109.1 . . ? H41A C41 H41B 107.8 . . ? C42 C42 C41 109.6(6) 2_766 . ? C42 C42 H42A 109.7 2_766 . ? C41 C42 H42A 109.7 . . ? C42 C42 H42B 109.7 2_766 . ? C41 C42 H42B 109.7 . . ? H42A C42 H42B 108.2 . . ? O13 Mn1 O17 90.39(17) 1_455 . ? O13 Mn1 O25 98.98(17) 1_455 . ? O17 Mn1 O25 170.49(16) . . ? O13 Mn1 O1 155.58(16) 1_455 . ? O17 Mn1 O1 87.47(17) . . ? O25 Mn1 O1 84.67(16) . . ? O13 Mn1 N1 104.53(18) 1_455 . ? O17 Mn1 N1 89.7(2) . . ? O25 Mn1 N1 86.39(19) . . ? O1 Mn1 N1 99.78(18) . . ? O13 Mn1 O11 81.19(16) 1_455 1_455 ? O17 Mn1 O11 91.42(16) . 1_455 ? O25 Mn1 O11 91.64(16) . 1_455 ? O1 Mn1 O11 74.55(15) . 1_455 ? N1 Mn1 O11 174.17(17) . 1_455 ? O2 Mn2 O18 81.61(17) . 2_556 ? O2 Mn2 O11 158.22(15) . 2_656 ? O18 Mn2 O11 88.44(16) 2_556 2_656 ? O2 Mn2 O19 81.85(16) . . ? O18 Mn2 O19 159.98(16) 2_556 . ? O11 Mn2 O19 110.85(17) 2_656 . ? O2 Mn2 O1 123.71(16) . 2_556 ? O18 Mn2 O1 88.40(16) 2_556 2_556 ? O11 Mn2 O1 74.99(15) 2_656 2_556 ? O19 Mn2 O1 91.46(15) . 2_556 ? O2 Mn2 O4 77.96(15) . . ? O18 Mn2 O4 100.96(16) 2_556 . ? O11 Mn2 O4 85.04(15) 2_656 . ? O19 Mn2 O4 86.50(15) . . ? O1 Mn2 O4 157.75(16) 2_556 . ? O9 Mn3 O10 152.60(18) . 2_656 ? O9 Mn3 O3 80.28(17) . . ? O10 Mn3 O3 124.13(16) 2_656 . ? O9 Mn3 O19 112.36(16) . . ? O10 Mn3 O19 85.10(16) 2_656 . ? O3 Mn3 O19 83.39(16) . . ? O9 Mn3 O21 81.78(16) . 2_656 ? O10 Mn3 O21 77.76(15) 2_656 2_656 ? O3 Mn3 O21 110.99(15) . 2_656 ? O19 Mn3 O21 161.92(14) . 2_656 ? O9 Mn3 O21 82.45(15) . . ? O10 Mn3 O21 79.25(14) 2_656 . ? O3 Mn3 O21 151.02(15) . . ? O19 Mn3 O21 81.90(15) . . ? O21 Mn3 O21 89.21(13) 2_656 . ? O5 Mn4 O6 101.57(16) 2_666 . ? O5 Mn4 O12 162.94(15) 2_666 1_565 ? O6 Mn4 O12 91.79(15) . 1_565 ? O5 Mn4 N5 96.62(18) 2_666 . ? O6 Mn4 N5 94.24(19) . . ? O12 Mn4 N5 92.88(19) 1_565 . ? O5 Mn4 O22 79.95(16) 2_666 1_565 ? O6 Mn4 O22 89.34(17) . 1_565 ? O12 Mn4 O22 89.75(16) 1_565 1_565 ? N5 Mn4 O22 175.49(18) . 1_565 ? O5 Mn4 O4 81.46(14) 2_666 2_666 ? O6 Mn4 O4 176.83(16) . 2_666 ? O12 Mn4 O4 85.41(14) 1_565 2_666 ? N5 Mn4 O4 84.42(18) . 2_666 ? O22 Mn4 O4 92.14(16) 1_565 2_666 ? C30 N1 C28 105.2(6) . . ? C30 N1 Mn1 123.3(5) . . ? C28 N1 Mn1 131.2(5) . . ? C30 N2 C29 105.9(6) . . ? C30 N2 C31 125.2(6) . . ? C29 N2 C31 128.9(6) . . ? C37 N3 C35 106.6(6) . . ? C37 N3 C34 128.6(6) . . ? C35 N3 C34 124.7(6) . . ? C37 N4 C36 107.6(6) . . ? C40 N5 C38 104.2(6) . . ? C40 N5 Mn4 127.1(4) . . ? C38 N5 Mn4 128.7(5) . . ? C40 N6 C39 105.7(6) . . ? C40 N6 C41 125.9(6) . . ? C39 N6 C41 127.6(6) . . ? O8 N7 O7 123.5(6) . . ? O8 N7 C6 119.1(5) . . ? O7 N7 C6 117.3(5) . . ? O16 N8 O15 121.5(6) . . ? O16 N8 C15 120.3(6) . . ? O15 N8 C15 118.2(7) . . ? O23 N9 O24 123.7(6) . . ? O23 N9 C24 118.7(5) . . ? O24 N9 C24 117.6(6) . . ? C1 O1 Mn1 136.0(4) . . ? C1 O1 Mn2 100.1(4) . 2_556 ? Mn1 O1 Mn2 100.46(16) . 2_556 ? C1 O2 Mn2 162.8(4) . . ? C8 O3 Mn3 117.0(4) . . ? C8 O4 Mn2 114.6(4) . . ? C8 O4 Mn4 110.9(4) . 2_666 ? Mn2 O4 Mn4 133.77(17) . 2_666 ? C9 O5 Mn4 140.0(4) . 2_666 ? C9 O6 Mn4 124.6(4) . . ? C10 O9 Mn3 127.2(4) . . ? C10 O10 Mn3 133.5(4) . 2_656 ? C17 O11 Mn2 136.5(4) . 2_656 ? C17 O11 Mn1 121.2(4) . 1_655 ? Mn2 O11 Mn1 100.52(17) 2_656 1_655 ? C17 O12 Mn4 140.6(4) . 1_545 ? C18 O13 Mn1 136.1(4) . 1_655 ? C19 O17 Mn1 131.0(5) . . ? C19 O18 Mn2 129.7(4) . 2_556 ? C25 O19 Mn3 114.9(4) . . ? C25 O19 Mn2 131.5(4) . . ? Mn3 O19 Mn2 110.47(16) . . ? C27 O21 Mn3 107.2(4) . 2_656 ? C27 O21 Mn3 131.4(4) . . ? Mn3 O21 Mn3 90.79(13) 2_656 . ? C27 O22 Mn4 156.3(4) . 1_545 ? Mn1 O25 H1W 139.4 . . ? Mn1 O25 H2W 125.8 . . ? H1W O25 H2W 94.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C7 -159.6(6) . . . . ? O1 C1 C2 C7 16.9(9) . . . . ? O2 C1 C2 C3 17.6(10) . . . . ? O1 C1 C2 C3 -165.9(6) . . . . ? C7 C2 C3 C4 2.3(10) . . . . ? C1 C2 C3 C4 -174.8(6) . . . . ? C7 C2 C3 C8 -171.5(6) . . . . ? C1 C2 C3 C8 11.4(9) . . . . ? C2 C3 C4 C5 -0.9(9) . . . . ? C8 C3 C4 C5 172.7(6) . . . . ? C2 C3 C4 C9 176.3(6) . . . . ? C8 C3 C4 C9 -10.1(9) . . . . ? C3 C4 C5 C6 -1.1(9) . . . . ? C9 C4 C5 C6 -178.5(6) . . . . ? C4 C5 C6 C7 1.8(10) . . . . ? C4 C5 C6 N7 179.2(6) . . . . ? C3 C2 C7 C6 -1.7(9) . . . . ? C1 C2 C7 C6 175.6(6) . . . . ? C5 C6 C7 C2 -0.4(10) . . . . ? N7 C6 C7 C2 -177.8(5) . . . . ? C2 C3 C8 O3 85.5(8) . . . . ? C4 C3 C8 O3 -88.3(7) . . . . ? C2 C3 C8 O4 -92.3(7) . . . . ? C4 C3 C8 O4 93.9(8) . . . . ? C5 C4 C9 O5 175.3(6) . . . . ? C3 C4 C9 O5 -1.9(9) . . . . ? C5 C4 C9 O6 -4.1(8) . . . . ? C3 C4 C9 O6 178.7(6) . . . . ? O10 C10 C11 C16 -175.1(5) . . . . ? O9 C10 C11 C16 7.7(8) . . . . ? O10 C10 C11 C12 3.2(8) . . . . ? O9 C10 C11 C12 -174.0(5) . . . . ? C16 C11 C12 C13 1.9(9) . . . . ? C10 C11 C12 C13 -176.4(5) . . . . ? C16 C11 C12 C17 -173.2(5) . . . . ? C10 C11 C12 C17 8.5(9) . . . . ? C11 C12 C13 C14 -4.0(9) . . . . ? C17 C12 C13 C14 170.8(6) . . . . ? C11 C12 C13 C18 169.2(6) . . . . ? C17 C12 C13 C18 -15.9(9) . . . . ? C12 C13 C14 C15 3.8(9) . . . . ? C18 C13 C14 C15 -169.8(6) . . . . ? C13 C14 C15 C16 -1.5(10) . . . . ? C13 C14 C15 N8 178.7(6) . . . . ? C12 C11 C16 C15 0.5(9) . . . . ? C10 C11 C16 C15 178.8(6) . . . . ? C14 C15 C16 C11 -0.7(10) . . . . ? N8 C15 C16 C11 179.1(6) . . . . ? C11 C12 C17 O12 83.4(7) . . . . ? C13 C12 C17 O12 -91.4(7) . . . . ? C11 C12 C17 O11 -100.3(7) . . . . ? C13 C12 C17 O11 84.9(8) . . . . ? C14 C13 C18 O13 136.2(6) . . . . ? C12 C13 C18 O13 -37.3(9) . . . . ? C14 C13 C18 O14 -39.6(8) . . . . ? C12 C13 C18 O14 146.9(6) . . . . ? O17 C19 C20 C21 154.2(6) . . . . ? O18 C19 C20 C21 -31.0(8) . . . . ? O17 C19 C20 C26 -22.0(8) . . . . ? O18 C19 C20 C26 152.7(5) . . . . ? C26 C20 C21 C22 -5.4(9) . . . . ? C19 C20 C21 C22 178.5(5) . . . . ? C26 C20 C21 C25 -178.7(5) . . . . ? C19 C20 C21 C25 5.1(9) . . . . ? C20 C21 C22 C23 -0.9(9) . . . . ? C25 C21 C22 C23 172.8(5) . . . . ? C20 C21 C22 C27 165.9(5) . . . . ? C25 C21 C22 C27 -20.4(9) . . . . ? C21 C22 C23 C24 5.4(9) . . . . ? C27 C22 C23 C24 -162.6(5) . . . . ? C22 C23 C24 C26 -3.8(9) . . . . ? C22 C23 C24 N9 175.8(5) . . . . ? C20 C21 C25 O20 99.2(8) . . . . ? C22 C21 C25 O20 -74.3(8) . . . . ? C20 C21 C25 O19 -79.7(7) . . . . ? C22 C21 C25 O19 106.9(6) . . . . ? C23 C24 C26 C20 -2.3(9) . . . . ? N9 C24 C26 C20 178.1(5) . . . . ? C21 C20 C26 C24 7.0(9) . . . . ? C19 C20 C26 C24 -176.6(5) . . . . ? C21 C22 C27 O22 158.1(6) . . . . ? C23 C22 C27 O22 -34.2(8) . . . . ? C21 C22 C27 O21 -24.7(9) . . . . ? C23 C22 C27 O21 143.0(5) . . . . ? N1 C28 C29 N2 0.1(9) . . . . ? N2 C31 C32 C33 -174.7(6) . . . . ? C31 C32 C33 C34 -80.1(8) . . . . ? C32 C33 C34 N3 -70.9(7) . . . . ? N3 C35 C36 N4 1.0(8) . . . . ? N5 C38 C39 N6 0.6(9) . . . . ? N6 C41 C42 C42 -59.6(8) . . . 2_766 ? N2 C30 N1 C28 0.9(8) . . . . ? N2 C30 N1 Mn1 176.4(4) . . . . ? C29 C28 N1 C30 -0.6(8) . . . . ? C29 C28 N1 Mn1 -175.6(5) . . . . ? O13 Mn1 N1 C30 80.2(5) 1_455 . . . ? O17 Mn1 N1 C30 170.6(5) . . . . ? O25 Mn1 N1 C30 -18.1(5) . . . . ? O1 Mn1 N1 C30 -102.1(5) . . . . ? O11 Mn1 N1 C30 -88(2) 1_455 . . . ? O13 Mn1 N1 C28 -105.5(6) 1_455 . . . ? O17 Mn1 N1 C28 -15.2(6) . . . . ? O25 Mn1 N1 C28 156.1(6) . . . . ? O1 Mn1 N1 C28 72.2(7) . . . . ? O11 Mn1 N1 C28 86(2) 1_455 . . . ? N1 C30 N2 C29 -0.8(8) . . . . ? N1 C30 N2 C31 177.5(5) . . . . ? C28 C29 N2 C30 0.4(8) . . . . ? C28 C29 N2 C31 -177.8(6) . . . . ? C32 C31 N2 C30 122.4(7) . . . . ? C32 C31 N2 C29 -59.7(9) . . . . ? N4 C37 N3 C35 -1.3(8) . . . . ? N4 C37 N3 C34 -177.6(6) . . . . ? C36 C35 N3 C37 0.1(8) . . . . ? C36 C35 N3 C34 176.6(6) . . . . ? C33 C34 N3 C37 -23.6(9) . . . . ? C33 C34 N3 C35 160.8(6) . . . . ? N3 C37 N4 C36 1.9(8) . . . . ? C35 C36 N4 C37 -1.8(8) . . . . ? N6 C40 N5 C38 1.9(7) . . . . ? N6 C40 N5 Mn4 -177.0(4) . . . . ? C39 C38 N5 C40 -1.5(8) . . . . ? C39 C38 N5 Mn4 177.3(5) . . . . ? O5 Mn4 N5 C40 -85.1(5) 2_666 . . . ? O6 Mn4 N5 C40 172.7(5) . . . . ? O12 Mn4 N5 C40 80.7(5) 1_565 . . . ? O22 Mn4 N5 C40 -45(2) 1_565 . . . ? O4 Mn4 N5 C40 -4.4(5) 2_666 . . . ? O5 Mn4 N5 C38 96.3(6) 2_666 . . . ? O6 Mn4 N5 C38 -5.9(6) . . . . ? O12 Mn4 N5 C38 -97.9(6) 1_565 . . . ? O22 Mn4 N5 C38 137(2) 1_565 . . . ? O4 Mn4 N5 C38 177.0(6) 2_666 . . . ? N5 C40 N6 C39 -1.6(7) . . . . ? N5 C40 N6 C41 -172.1(6) . . . . ? C38 C39 N6 C40 0.5(8) . . . . ? C38 C39 N6 C41 170.8(7) . . . . ? C42 C41 N6 C40 108.8(7) . . . . ? C42 C41 N6 C39 -59.7(8) . . . . ? C5 C6 N7 O8 175.0(6) . . . . ? C7 C6 N7 O8 -7.6(9) . . . . ? C5 C6 N7 O7 -3.2(9) . . . . ? C7 C6 N7 O7 174.2(6) . . . . ? C16 C15 N8 O16 3.1(11) . . . . ? C14 C15 N8 O16 -177.1(7) . . . . ? C16 C15 N8 O15 -178.9(6) . . . . ? C14 C15 N8 O15 0.9(10) . . . . ? C26 C24 N9 O23 -168.8(6) . . . . ? C23 C24 N9 O23 11.6(8) . . . . ? C26 C24 N9 O24 13.8(8) . . . . ? C23 C24 N9 O24 -165.8(5) . . . . ? O2 C1 O1 Mn1 -111.8(6) . . . . ? C2 C1 O1 Mn1 71.7(8) . . . . ? O2 C1 O1 Mn2 4.9(7) . . . 2_556 ? C2 C1 O1 Mn2 -171.6(5) . . . 2_556 ? O13 Mn1 O1 C1 132.6(6) 1_455 . . . ? O17 Mn1 O1 C1 47.2(6) . . . . ? O25 Mn1 O1 C1 -127.4(6) . . . . ? N1 Mn1 O1 C1 -42.0(6) . . . . ? O11 Mn1 O1 C1 139.4(6) 1_455 . . . ? O13 Mn1 O1 Mn2 16.0(5) 1_455 . . 2_556 ? O17 Mn1 O1 Mn2 -69.35(19) . . . 2_556 ? O25 Mn1 O1 Mn2 116.02(19) . . . 2_556 ? N1 Mn1 O1 Mn2 -158.6(2) . . . 2_556 ? O11 Mn1 O1 Mn2 22.83(16) 1_455 . . 2_556 ? O1 C1 O2 Mn2 -159.4(12) . . . . ? C2 C1 O2 Mn2 17(2) . . . . ? O18 Mn2 O2 C1 76.0(16) 2_556 . . . ? O11 Mn2 O2 C1 12.3(18) 2_656 . . . ? O19 Mn2 O2 C1 -115.3(16) . . . . ? O1 Mn2 O2 C1 158.4(15) 2_556 . . . ? O4 Mn2 O2 C1 -27.2(15) . . . . ? O4 C8 O3 Mn3 3.3(8) . . . . ? C3 C8 O3 Mn3 -174.4(4) . . . . ? O9 Mn3 O3 C8 -178.1(5) . . . . ? O10 Mn3 O3 C8 -11.6(5) 2_656 . . . ? O19 Mn3 O3 C8 67.8(4) . . . . ? O21 Mn3 O3 C8 -100.8(4) 2_656 . . . ? O21 Mn3 O3 C8 127.7(4) . . . . ? O3 C8 O4 Mn2 -78.5(7) . . . . ? C3 C8 O4 Mn2 99.2(5) . . . . ? O3 C8 O4 Mn4 93.0(6) . . . 2_666 ? C3 C8 O4 Mn4 -89.3(6) . . . 2_666 ? O2 Mn2 O4 C8 -30.3(5) . . . . ? O18 Mn2 O4 C8 -109.1(5) 2_556 . . . ? O11 Mn2 O4 C8 163.4(5) 2_656 . . . ? O19 Mn2 O4 C8 52.1(5) . . . . ? O1 Mn2 O4 C8 137.4(5) 2_556 . . . ? O2 Mn2 O4 Mn4 160.7(3) . . . 2_666 ? O18 Mn2 O4 Mn4 81.9(3) 2_556 . . 2_666 ? O11 Mn2 O4 Mn4 -5.6(3) 2_656 . . 2_666 ? O19 Mn2 O4 Mn4 -116.9(3) . . . 2_666 ? O1 Mn2 O4 Mn4 -31.6(6) 2_556 . . 2_666 ? O6 C9 O5 Mn4 108.3(8) . . . 2_666 ? C4 C9 O5 Mn4 -71.0(7) . . . 2_666 ? O5 C9 O6 Mn4 -21.7(9) . . . . ? C4 C9 O6 Mn4 157.6(4) . . . . ? O5 Mn4 O6 C9 -23.4(5) 2_666 . . . ? O12 Mn4 O6 C9 167.3(5) 1_565 . . . ? N5 Mn4 O6 C9 74.3(5) . . . . ? O22 Mn4 O6 C9 -103.0(5) 1_565 . . . ? O4 Mn4 O6 C9 139(3) 2_666 . . . ? O10 C10 O9 Mn3 -3.5(9) . . . . ? C11 C10 O9 Mn3 173.4(4) . . . . ? O10 Mn3 O9 C10 6.8(7) 2_656 . . . ? O3 Mn3 O9 C10 161.8(5) . . . . ? O19 Mn3 O9 C10 -119.6(5) . . . . ? O21 Mn3 O9 C10 48.7(5) 2_656 . . . ? O21 Mn3 O9 C10 -41.6(5) . . . . ? O9 C10 O10 Mn3 0.5(9) . . . 2_656 ? C11 C10 O10 Mn3 -176.4(4) . . . 2_656 ? O12 C17 O11 Mn2 -54.1(9) . . . 2_656 ? C12 C17 O11 Mn2 130.1(5) . . . 2_656 ? O12 C17 O11 Mn1 144.4(5) . . . 1_655 ? C12 C17 O11 Mn1 -31.5(7) . . . 1_655 ? O11 C17 O12 Mn4 37.9(10) . . . 1_545 ? C12 C17 O12 Mn4 -146.1(5) . . . 1_545 ? O14 C18 O13 Mn1 157.7(4) . . . 1_655 ? C13 C18 O13 Mn1 -17.7(9) . . . 1_655 ? O18 C19 O17 Mn1 13.0(10) . . . . ? C20 C19 O17 Mn1 -173.1(3) . . . . ? O13 Mn1 O17 C19 -118.3(5) 1_455 . . . ? O25 Mn1 O17 C19 71.6(12) . . . . ? O1 Mn1 O17 C19 37.4(5) . . . . ? N1 Mn1 O17 C19 137.2(5) . . . . ? O11 Mn1 O17 C19 -37.1(5) 1_455 . . . ? O17 C19 O18 Mn2 -21.3(10) . . . 2_556 ? C20 C19 O18 Mn2 164.7(3) . . . 2_556 ? O20 C25 O19 Mn3 126.9(6) . . . . ? C21 C25 O19 Mn3 -54.4(6) . . . . ? O20 C25 O19 Mn2 -30.7(9) . . . . ? C21 C25 O19 Mn2 148.0(4) . . . . ? O9 Mn3 O19 C25 53.5(4) . . . . ? O10 Mn3 O19 C25 -104.7(4) 2_656 . . . ? O3 Mn3 O19 C25 130.1(4) . . . . ? O21 Mn3 O19 C25 -86.1(6) 2_656 . . . ? O21 Mn3 O19 C25 -24.8(4) . . . . ? O9 Mn3 O19 Mn2 -144.26(17) . . . . ? O10 Mn3 O19 Mn2 57.59(18) 2_656 . . . ? O3 Mn3 O19 Mn2 -67.64(18) . . . . ? O21 Mn3 O19 Mn2 76.2(5) 2_656 . . . ? O21 Mn3 O19 Mn2 137.40(18) . . . . ? O2 Mn2 O19 C25 -96.2(5) . . . . ? O18 Mn2 O19 C25 -61.7(7) 2_556 . . . ? O11 Mn2 O19 C25 102.1(5) 2_656 . . . ? O1 Mn2 O19 C25 27.6(5) 2_556 . . . ? O4 Mn2 O19 C25 -174.6(5) . . . . ? O2 Mn2 O19 Mn3 105.45(18) . . . . ? O18 Mn2 O19 Mn3 140.0(4) 2_556 . . . ? O11 Mn2 O19 Mn3 -56.2(2) 2_656 . . . ? O1 Mn2 O19 Mn3 -130.70(18) 2_556 . . . ? O4 Mn2 O19 Mn3 27.12(17) . . . . ? O22 C27 O21 Mn3 38.0(7) . . . 2_656 ? C22 C27 O21 Mn3 -139.0(4) . . . 2_656 ? O22 C27 O21 Mn3 145.0(5) . . . . ? C22 C27 O21 Mn3 -32.0(8) . . . . ? O9 Mn3 O21 C27 -32.2(6) . . . . ? O10 Mn3 O21 C27 168.3(6) 2_656 . . . ? O3 Mn3 O21 C27 21.6(8) . . . . ? O19 Mn3 O21 C27 81.8(6) . . . . ? O21 Mn3 O21 C27 -114.0(6) 2_656 . . . ? O9 Mn3 O21 Mn3 81.81(16) . . . 2_656 ? O10 Mn3 O21 Mn3 -77.69(16) 2_656 . . 2_656 ? O3 Mn3 O21 Mn3 135.6(3) . . . 2_656 ? O19 Mn3 O21 Mn3 -164.21(16) . . . 2_656 ? O21 Mn3 O21 Mn3 0.0 2_656 . . 2_656 ? O21 C27 O22 Mn4 -106.3(10) . . . 1_545 ? C22 C27 O22 Mn4 70.6(12) . . . 1_545 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.988 _refine_diff_density_min -0.938 _refine_diff_density_rms 0.150 _database_code_depnum_ccdc_archive 'CCDC 910424' ####################################################################### # # 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_test_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H41 Mn3 N8 O25' _chemical_formula_weight 1186.62 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 21.2387(10) _cell_length_b 16.0539(8) _cell_length_c 14.6979(7) _cell_angle_alpha 90.00 _cell_angle_beta 108.8370(10) _cell_angle_gamma 90.00 _cell_volume 4743.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6303 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 26.49 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2424 _exptl_absorpt_coefficient_mu 0.886 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8427 _exptl_absorpt_correction_T_max 0.8427 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19828 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8336 _reflns_number_gt 6624 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0562P)^2^+1.7894P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8336 _refine_ls_number_parameters 676 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.1057 _refine_ls_wR_factor_gt 0.0928 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.067 _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 0.259095(19) -0.00022(2) 0.78058(3) 0.02055(11) Uani 1 1 d . . . Mn2 Mn 0.40519(2) -0.14198(3) 0.89055(3) 0.02526(12) Uani 1 1 d . . . Mn3 Mn 0.36966(2) 0.11601(3) 1.24836(3) 0.02800(12) Uani 1 1 d . . . O1 O 0.25211(10) -0.04366(12) 0.91648(14) 0.0337(5) Uani 1 1 d . . . O2 O 0.34016(10) -0.12678(13) 0.97392(15) 0.0338(5) Uani 1 1 d . . . O3 O 0.38664(10) -0.14640(13) 1.18340(15) 0.0376(5) Uani 1 1 d . . . O4 O 0.38214(10) -0.27299(12) 1.11943(15) 0.0345(5) Uani 1 1 d . . . O5 O 0.33169(10) -0.20186(13) 0.77692(15) 0.0361(5) Uani 1 1 d . . . O6 O 0.24143(11) -0.12209(13) 0.72431(17) 0.0444(6) Uani 1 1 d . . . O7 O 0.40439(9) 0.20714(11) 1.16253(13) 0.0262(4) Uani 1 1 d . . . O8 O 0.42833(9) 0.28232(12) 1.05118(14) 0.0314(5) Uani 1 1 d . . . O9 O 0.27519(10) 0.12258(12) 0.83730(14) 0.0337(5) Uani 1 1 d . . . O10 O 0.36167(9) 0.11228(12) 0.97113(14) 0.0296(5) Uani 1 1 d . . . O11 O 0.08511(14) 0.3721(2) 0.9158(3) 0.0975(13) Uani 1 1 d . . . O12 O 0.08451(13) 0.2766(2) 0.8138(2) 0.0759(9) Uani 1 1 d . . . O13 O 0.27683(11) 0.04483(13) 0.65527(14) 0.0378(5) Uani 1 1 d . . . O14 O 0.37625(11) 0.10231(14) 0.68466(16) 0.0415(5) Uani 1 1 d . . . O15 O 0.37808(9) -0.00612(11) 0.84195(14) 0.0292(4) Uani 1 1 d . . . O16 O 0.04025(11) -0.22566(15) 1.05287(19) 0.0499(6) Uani 1 1 d . . . O17 O 0.04189(11) -0.16172(15) 0.92363(17) 0.0492(6) Uani 1 1 d . . . O18 O 0.46235(9) -0.15948(13) 0.79142(14) 0.0328(5) Uani 1 1 d D . . O19 O 0.39037(12) 0.21688(14) 1.35151(16) 0.0450(6) Uani 1 1 d . . . O20 O 0.43028(12) -0.25943(14) 0.96665(16) 0.0468(6) Uani 1 1 d . . . O23 O 0.47330(11) 0.06999(15) 1.32488(18) 0.0506(6) Uani 1 1 d D . . O22 O 0.36939(13) 0.02238(13) 1.13901(16) 0.0488(6) Uani 1 1 d . . . O45 O 0.49278(13) -0.09009(18) 0.99481(17) 0.0615(8) Uani 1 1 d . . . N1 N 0.15051(12) 0.01808(15) 0.72898(18) 0.0323(6) Uani 1 1 d . . . N2 N 0.26102(12) 0.13206(16) 1.16598(18) 0.0335(6) Uani 1 1 d . . . N3 N 0.16270(12) 0.11433(16) 1.05701(19) 0.0362(6) Uani 1 1 d . . . N4 N 0.30176(12) -0.07937(15) 1.39823(19) 0.0329(6) Uani 1 1 d . . . N5 N 0.34308(13) 0.03043(16) 1.34805(18) 0.0361(6) Uani 1 1 d . . . N6 N 0.05195(12) 0.06723(18) 0.6482(2) 0.0458(7) Uani 1 1 d . . . N7 N 0.11310(14) 0.3188(2) 0.8834(2) 0.0526(8) Uani 1 1 d . . . N8 N 0.06987(12) -0.19350(16) 1.0021(2) 0.0361(6) Uani 1 1 d . . . C1 C 0.28301(14) -0.10257(16) 0.96743(19) 0.0245(6) Uani 1 1 d . . . C2 C 0.24695(13) -0.15027(16) 1.02419(19) 0.0230(6) Uani 1 1 d . . . C3 C 0.28050(13) -0.20260(16) 1.10123(19) 0.0215(6) Uani 1 1 d . . . C4 C 0.24306(13) -0.25328(16) 1.14265(19) 0.0218(6) Uani 1 1 d . . . C5 C 0.17458(13) -0.24991(17) 1.1100(2) 0.0263(6) Uani 1 1 d . . . H5 H 0.1499 -0.2841 1.1368 0.032 Uiso 1 1 calc R . . C6 C 0.14300(13) -0.19516(17) 1.0369(2) 0.0275(6) Uani 1 1 d . . . C7 C 0.17796(14) -0.14596(17) 0.9935(2) 0.0279(6) Uani 1 1 d . . . H7 H 0.1556 -0.1101 0.9439 0.033 Uiso 1 1 calc R . . C8 C 0.35612(14) -0.20748(17) 1.13726(19) 0.0256(6) Uani 1 1 d . . . C9 C 0.27540(14) -0.18469(17) 0.7210(2) 0.0261(6) Uani 1 1 d . . . C10 C 0.30190(15) -0.0332(2) 1.3227(2) 0.0382(7) Uani 1 1 d . . . H10 H 0.2760 -0.0445 1.2597 0.046 Uiso 1 1 calc R . . C11 C 0.37080(17) 0.0236(2) 1.4463(2) 0.0418(8) Uani 1 1 d . . . H11 H 0.4021 0.0600 1.4852 0.050 Uiso 1 1 calc R . . C12 C 0.34586(16) -0.0433(2) 1.4776(2) 0.0410(8) Uani 1 1 d . . . H12 H 0.3565 -0.0615 1.5408 0.049 Uiso 1 1 calc R . . C13 C 0.26211(16) -0.15450(19) 1.3950(3) 0.0446(9) Uani 1 1 d . . . H13A H 0.2849 -0.1894 1.4495 0.054 Uiso 1 1 calc R . . H13B H 0.2593 -0.1854 1.3371 0.054 Uiso 1 1 calc R . . C14 C -0.19267(15) 0.13766(18) 0.6035(2) 0.0324(7) Uani 1 1 d . . . C15 C -0.13875(18) 0.1746(2) 0.6707(3) 0.0503(9) Uani 1 1 d . . . H15 H -0.1452 0.2053 0.7206 0.060 Uiso 1 1 calc R . . C16 C -0.07539(18) 0.1667(3) 0.6649(3) 0.0565(11) Uani 1 1 d . . . H16 H -0.0398 0.1925 0.7107 0.068 Uiso 1 1 calc R . . C17 C -0.06435(16) 0.1213(2) 0.5927(3) 0.0494(10) Uani 1 1 d . . . C18 C -0.11785(17) 0.0816(2) 0.5271(3) 0.0455(9) Uani 1 1 d . . . H18 H -0.1110 0.0493 0.4786 0.055 Uiso 1 1 calc R . . C19 C -0.18137(15) 0.08949(19) 0.5328(2) 0.0368(7) Uani 1 1 d . . . H19 H -0.2167 0.0620 0.4886 0.044 Uiso 1 1 calc R . . C20 C 0.22632(14) 0.09079(19) 1.0880(2) 0.0336(7) Uani 1 1 d . . . H20 H 0.2442 0.0502 1.0584 0.040 Uiso 1 1 calc R . . C33 C 0.15561(17) 0.1749(2) 1.1181(3) 0.0528(10) Uani 1 1 d . . . H33 H 0.1168 0.2033 1.1149 0.063 Uiso 1 1 calc R . . C34 C 0.21627(17) 0.1852(2) 1.1840(3) 0.0475(9) Uani 1 1 d . . . H34 H 0.2262 0.2231 1.2345 0.057 Uiso 1 1 calc R . . C35 C 0.11222(16) 0.0852(2) 0.9695(2) 0.0433(8) Uani 1 1 d . . . H35A H 0.1329 0.0474 0.9361 0.052 Uiso 1 1 calc R . . H35B H 0.0954 0.1325 0.9277 0.052 Uiso 1 1 calc R . . C36 C 0.05434(15) 0.04112(19) 0.9878(2) 0.0354(7) Uani 1 1 d . . . C37 C -0.00540(15) 0.0368(2) 0.9134(2) 0.0389(8) Uani 1 1 d . . . H37 H -0.0093 0.0615 0.8546 0.047 Uiso 1 1 calc R . . C38 C 0.05907(15) 0.0039(2) 1.0739(2) 0.0388(8) Uani 1 1 d . . . H38 H 0.0990 0.0061 1.1243 0.047 Uiso 1 1 calc R . . C23 C 0.11747(15) 0.0804(2) 0.6777(2) 0.0390(8) Uani 1 1 d . . . H23 H 0.1374 0.1282 0.6636 0.047 Uiso 1 1 calc R . . C22 C 0.04191(16) -0.0092(2) 0.6820(3) 0.0457(9) Uani 1 1 d . . . H22 H 0.0013 -0.0355 0.6726 0.055 Uiso 1 1 calc R . . C24 C 0.10220(16) -0.0385(2) 0.7313(2) 0.0390(8) Uani 1 1 d . . . H24 H 0.1104 -0.0897 0.7626 0.047 Uiso 1 1 calc R . . C32 C 0.30865(14) 0.14604(16) 0.9205(2) 0.0243(6) Uani 1 1 d . . . C29 C 0.28000(13) 0.21984(16) 0.95794(19) 0.0228(6) Uani 1 1 d . . . C30 C 0.21370(13) 0.23690(18) 0.9086(2) 0.0273(6) Uani 1 1 d . . . H30 H 0.1900 0.2032 0.8576 0.033 Uiso 1 1 calc R . . C25 C 0.18335(14) 0.30344(19) 0.9350(2) 0.0326(7) Uani 1 1 d . . . C26 C 0.21736(14) 0.35536(18) 1.0092(2) 0.0316(7) Uani 1 1 d . . . H26 H 0.1959 0.4010 1.0249 0.038 Uiso 1 1 calc R . . C27 C 0.28341(13) 0.33981(17) 1.06042(19) 0.0249(6) Uani 1 1 d . . . C28 C 0.31571(13) 0.27037(16) 1.03624(19) 0.0209(6) Uani 1 1 d . . . C31 C 0.38822(13) 0.25197(16) 1.08786(19) 0.0216(6) Uani 1 1 d . . . C59 C 0.31592(15) 0.09862(18) 0.6406(2) 0.0284(6) Uani 1 1 d . . . C21 C 0.00259(17) 0.1205(3) 0.5784(3) 0.0753(15) Uani 1 1 d U . . H21A H -0.0027 0.1010 0.5139 0.090 Uiso 1 1 calc R . . H21B H 0.0195 0.1770 0.5837 0.090 Uiso 1 1 calc R . . O21 O 0.51791(11) 0.84063(15) 0.16845(16) 0.0465(6) Uani 1 1 d D . . O24 O 0.52782(12) 0.10094(15) 0.63394(17) 0.0632(8) Uani 1 1 d D . . H19A H 0.3828 0.2475 1.3929 0.076 Uiso 1 1 d R . . H19B H 0.4159 0.2429 1.3268 0.076 Uiso 1 1 d R . . H20A H 0.4143 -0.3059 0.9802 0.076 Uiso 1 1 d R . . H20B H 0.4727 -0.2655 0.9880 0.076 Uiso 1 1 d R . . H22A H 0.3598 -0.0308 1.1294 0.076 Uiso 1 1 d R . . H22B H 0.3587 0.0432 1.0820 0.076 Uiso 1 1 d R . . H45A H 0.5317 -0.0847 0.9890 0.076 Uiso 1 1 d R . . H45B H 0.4975 -0.0868 1.0538 0.076 Uiso 1 1 d R . . H18A H 0.4989 -0.1844 0.8079 0.076 Uiso 1 1 d RD . . H18B H 0.4421 -0.1899 0.7443 0.076 Uiso 1 1 d RD . . H23A H 0.5052 0.0776 1.3037 0.076 Uiso 1 1 d RD . . H23B H 0.4820 0.0198 1.3417 0.076 Uiso 1 1 d RD . . H2W H 0.5421 0.8608 0.2214 0.076 Uiso 1 1 d RD . . H1W H 0.4825 0.8395 0.1836 0.076 Uiso 1 1 d RD . . H4W H 0.5504 0.1241 0.6857 0.076 Uiso 1 1 d RD . . H3W H 0.4940 0.1314 0.6231 0.076 Uiso 1 1 d RD . . 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 0.0239(2) 0.0172(2) 0.0191(2) 0.00024(16) 0.00483(18) 0.00010(16) Mn2 0.0214(2) 0.0300(2) 0.0234(2) -0.00368(18) 0.00589(18) -0.00196(18) Mn3 0.0309(3) 0.0277(2) 0.0263(2) 0.00159(18) 0.0104(2) -0.00321(18) O1 0.0404(12) 0.0335(11) 0.0297(11) 0.0121(9) 0.0150(10) 0.0086(10) O2 0.0347(12) 0.0390(12) 0.0327(12) 0.0116(9) 0.0176(10) 0.0100(9) O3 0.0349(12) 0.0334(12) 0.0356(12) 0.0022(10) -0.0009(10) -0.0077(10) O4 0.0353(11) 0.0342(12) 0.0355(12) 0.0094(9) 0.0138(10) 0.0146(9) O5 0.0308(12) 0.0402(12) 0.0315(12) -0.0148(10) 0.0017(10) -0.0014(10) O6 0.0461(14) 0.0253(11) 0.0543(15) -0.0160(10) 0.0059(12) 0.0027(10) O7 0.0271(10) 0.0281(10) 0.0209(10) 0.0038(8) 0.0041(8) -0.0003(8) O8 0.0244(10) 0.0375(12) 0.0326(11) 0.0037(9) 0.0098(9) -0.0028(9) O9 0.0425(12) 0.0235(10) 0.0271(11) -0.0079(9) 0.0001(10) 0.0009(9) O10 0.0295(11) 0.0279(10) 0.0281(11) -0.0028(9) 0.0048(9) 0.0049(9) O11 0.0449(17) 0.102(3) 0.122(3) -0.040(2) -0.0053(18) 0.0366(17) O12 0.0377(15) 0.092(2) 0.073(2) -0.0287(18) -0.0168(14) 0.0074(15) O13 0.0498(13) 0.0382(12) 0.0240(11) 0.0053(9) 0.0099(10) -0.0180(10) O14 0.0361(13) 0.0434(13) 0.0363(13) 0.0139(10) -0.0005(11) -0.0031(10) O15 0.0302(11) 0.0250(10) 0.0314(11) 0.0009(8) 0.0087(9) -0.0005(8) O16 0.0317(12) 0.0491(15) 0.0723(17) 0.0068(13) 0.0215(13) -0.0002(11) O17 0.0344(13) 0.0533(15) 0.0475(15) 0.0067(12) -0.0038(11) 0.0117(11) O18 0.0244(10) 0.0410(12) 0.0330(12) -0.0072(9) 0.0092(9) -0.0007(9) O19 0.0654(15) 0.0370(12) 0.0398(13) -0.0094(10) 0.0269(12) -0.0080(11) O20 0.0555(14) 0.0390(13) 0.0461(14) 0.0053(11) 0.0165(12) 0.0148(11) O23 0.0386(13) 0.0557(15) 0.0602(16) 0.0154(13) 0.0194(12) 0.0064(11) O22 0.0809(18) 0.0309(12) 0.0337(13) -0.0015(10) 0.0172(13) 0.0084(12) O45 0.0579(16) 0.0781(19) 0.0349(13) -0.0006(13) -0.0041(12) -0.0417(14) N1 0.0273(13) 0.0322(14) 0.0337(14) 0.0012(11) 0.0047(11) 0.0018(11) N2 0.0335(14) 0.0342(14) 0.0337(15) -0.0015(11) 0.0119(12) -0.0043(11) N3 0.0294(14) 0.0365(15) 0.0404(16) -0.0025(12) 0.0082(12) -0.0069(11) N4 0.0330(14) 0.0306(13) 0.0403(15) 0.0059(12) 0.0189(13) -0.0008(11) N5 0.0380(15) 0.0375(15) 0.0334(15) 0.0058(12) 0.0125(12) -0.0069(12) N6 0.0232(14) 0.0549(18) 0.0561(19) 0.0239(15) 0.0085(13) 0.0052(12) N7 0.0295(15) 0.0547(19) 0.064(2) -0.0050(17) 0.0010(15) 0.0124(14) N8 0.0268(14) 0.0299(14) 0.0480(17) -0.0021(13) 0.0070(13) 0.0030(11) C1 0.0330(16) 0.0220(14) 0.0173(14) -0.0012(11) 0.0063(12) 0.0005(12) C2 0.0297(15) 0.0204(13) 0.0192(14) 0.0010(11) 0.0083(12) 0.0033(11) C3 0.0280(14) 0.0169(13) 0.0191(14) -0.0018(11) 0.0068(12) 0.0016(11) C4 0.0269(14) 0.0170(13) 0.0206(14) 0.0006(11) 0.0066(12) 0.0032(11) C5 0.0268(15) 0.0239(14) 0.0289(15) -0.0001(12) 0.0099(13) -0.0033(12) C6 0.0227(14) 0.0261(15) 0.0311(16) -0.0015(12) 0.0050(13) 0.0032(12) C7 0.0288(15) 0.0284(15) 0.0231(15) 0.0054(12) 0.0037(13) 0.0061(12) C8 0.0283(15) 0.0274(15) 0.0211(14) 0.0079(12) 0.0078(13) 0.0014(13) C9 0.0319(16) 0.0245(15) 0.0259(15) -0.0037(12) 0.0146(14) -0.0065(13) C10 0.0370(18) 0.0451(19) 0.0318(17) 0.0018(15) 0.0102(15) -0.0097(15) C11 0.047(2) 0.0426(19) 0.0344(19) -0.0028(15) 0.0105(16) -0.0114(16) C12 0.047(2) 0.0461(19) 0.0292(17) 0.0082(15) 0.0120(16) -0.0013(16) C13 0.045(2) 0.0280(17) 0.070(2) 0.0032(16) 0.0322(19) -0.0027(14) C14 0.0331(16) 0.0290(16) 0.0358(17) 0.0073(13) 0.0121(14) 0.0001(13) C15 0.056(2) 0.055(2) 0.037(2) -0.0089(17) 0.0119(18) -0.0136(19) C16 0.037(2) 0.073(3) 0.045(2) 0.014(2) -0.0074(18) -0.0182(19) C17 0.0280(18) 0.063(2) 0.055(2) 0.031(2) 0.0095(17) 0.0100(16) C18 0.043(2) 0.047(2) 0.052(2) 0.0092(17) 0.0227(18) 0.0128(16) C19 0.0310(17) 0.0362(17) 0.0399(18) -0.0021(14) 0.0069(15) -0.0010(14) C20 0.0293(16) 0.0332(16) 0.0383(18) -0.0004(14) 0.0110(14) -0.0037(13) C33 0.037(2) 0.051(2) 0.069(3) -0.016(2) 0.0163(19) 0.0038(17) C34 0.043(2) 0.053(2) 0.046(2) -0.0165(17) 0.0144(17) -0.0049(17) C35 0.0380(18) 0.050(2) 0.0370(19) 0.0006(16) 0.0057(16) -0.0126(16) C36 0.0314(17) 0.0299(16) 0.0408(18) -0.0021(14) 0.0061(15) -0.0043(13) C37 0.0389(18) 0.0383(18) 0.0355(18) 0.0047(14) 0.0064(15) -0.0023(15) C38 0.0288(17) 0.0419(18) 0.0379(19) 0.0032(15) -0.0001(14) -0.0042(14) C23 0.0277(16) 0.0354(18) 0.053(2) 0.0100(16) 0.0124(16) 0.0009(14) C22 0.0294(18) 0.054(2) 0.050(2) 0.0106(17) 0.0079(16) -0.0106(16) C24 0.0379(18) 0.0339(17) 0.0433(19) 0.0080(15) 0.0104(16) -0.0025(14) C32 0.0289(15) 0.0175(13) 0.0253(15) -0.0011(12) 0.0070(13) -0.0044(12) C29 0.0237(14) 0.0208(14) 0.0227(14) 0.0007(11) 0.0058(12) -0.0013(11) C30 0.0229(14) 0.0300(15) 0.0246(15) -0.0040(12) 0.0013(12) -0.0049(12) C25 0.0207(15) 0.0387(17) 0.0332(17) -0.0004(14) 0.0013(13) 0.0027(13) C26 0.0285(16) 0.0297(16) 0.0344(17) -0.0028(13) 0.0070(14) 0.0083(13) C27 0.0275(15) 0.0242(14) 0.0227(14) 0.0003(11) 0.0078(12) 0.0011(12) C28 0.0240(14) 0.0202(13) 0.0190(13) 0.0016(11) 0.0075(12) 0.0001(11) C31 0.0250(14) 0.0160(13) 0.0227(14) -0.0037(11) 0.0063(12) -0.0011(11) C59 0.0369(17) 0.0277(15) 0.0194(15) 0.0007(12) 0.0076(14) -0.0030(13) C21 0.0296(19) 0.106(3) 0.090(3) 0.061(3) 0.019(2) 0.021(2) O21 0.0379(13) 0.0619(16) 0.0355(13) -0.0019(11) 0.0061(11) -0.0051(11) O24 0.0605(17) 0.0624(17) 0.0514(16) -0.0110(13) -0.0033(14) 0.0252(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O6 2.110(2) . ? Mn1 O13 2.123(2) . ? Mn1 O9 2.1246(19) . ? Mn1 O1 2.1657(19) . ? Mn1 N1 2.202(2) . ? Mn1 O15 2.3951(19) . ? Mn2 O5 2.113(2) . ? Mn2 O2 2.136(2) . ? Mn2 O45 2.159(2) . ? Mn2 O20 2.169(2) . ? Mn2 O18 2.1951(19) . ? Mn2 O15 2.3095(19) . ? Mn3 O19 2.164(2) . ? Mn3 O22 2.199(2) . ? Mn3 O7 2.2084(19) . ? Mn3 N5 2.211(2) . ? Mn3 N2 2.248(3) . ? Mn3 O23 2.249(2) . ? O1 C1 1.252(3) . ? O2 C1 1.248(3) . ? O3 C8 1.248(3) . ? O4 C8 1.255(3) . ? O5 C9 1.244(3) . ? O6 C9 1.247(3) . ? O7 C31 1.264(3) . ? O8 C31 1.245(3) . ? O9 C32 1.257(3) . ? O10 C32 1.255(3) . ? O11 N7 1.222(4) . ? O12 N7 1.213(4) . ? O13 C59 1.264(3) . ? O14 C59 1.237(3) . ? O16 N8 1.234(3) . ? O17 N8 1.226(3) . ? O18 H18A 0.8358 . ? O18 H18B 0.8431 . ? O19 H19A 0.8367 . ? O19 H19B 0.8537 . ? O20 H20A 0.8693 . ? O20 H20B 0.8592 . ? O23 H23A 0.8409 . ? O23 H23B 0.8451 . ? O22 H22A 0.8784 . ? O22 H22B 0.8611 . ? O45 H45A 0.8628 . ? O45 H45B 0.8420 . ? N1 C23 1.312(4) . ? N1 C24 1.379(4) . ? N2 C20 1.323(4) . ? N2 C34 1.365(4) . ? N3 C20 1.334(4) . ? N3 C33 1.364(4) . ? N3 C35 1.460(4) . ? N4 C10 1.336(4) . ? N4 C12 1.366(4) . ? N4 C13 1.463(4) . ? N5 C10 1.317(4) . ? N5 C11 1.376(4) . ? N6 C23 1.334(4) . ? N6 C22 1.366(4) . ? N6 C21 1.480(4) . ? N7 C25 1.460(4) . ? N8 C6 1.470(4) . ? C1 C2 1.510(4) . ? C2 C7 1.389(4) . ? C2 C3 1.405(4) . ? C3 C4 1.406(4) . ? C3 C8 1.522(4) . ? C4 C5 1.378(4) . ? C4 C9 1.509(4) 4_556 ? C5 C6 1.382(4) . ? C5 H5 0.9300 . ? C6 C7 1.374(4) . ? C7 H7 0.9300 . ? C9 C4 1.509(4) 4 ? C10 H10 0.9300 . ? C11 C12 1.343(5) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.507(4) 3_557 ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C19 1.377(4) . ? C14 C15 1.381(5) . ? C14 C13 1.507(4) 3_557 ? C15 C16 1.381(5) . ? C15 H15 0.9300 . ? C16 C17 1.368(6) . ? C16 H16 0.9300 . ? C17 C18 1.386(5) . ? C17 C21 1.503(5) . ? C18 C19 1.384(4) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C33 C34 1.349(5) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C36 1.515(4) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C38 1.374(5) . ? C36 C37 1.383(4) . ? C37 C38 1.377(4) 3_557 ? C37 H37 0.9300 . ? C38 C37 1.377(4) 3_557 ? C38 H38 0.9300 . ? C23 H23 0.9300 . ? C22 C24 1.337(4) . ? C22 H22 0.9300 . ? C24 H24 0.9300 . ? C32 C29 1.514(4) . ? C29 C30 1.387(4) . ? C29 C28 1.412(4) . ? C30 C25 1.367(4) . ? C30 H30 0.9300 . ? C25 C26 1.377(4) . ? C26 C27 1.384(4) . ? C26 H26 0.9300 . ? C27 C28 1.413(4) . ? C27 C59 1.522(4) 4_566 ? C28 C31 1.510(4) . ? C59 C27 1.522(4) 4_565 ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? O21 H2W 0.8460 . ? O21 H1W 0.8512 . ? O24 H4W 0.8434 . ? O24 H3W 0.8417 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Mn1 O13 91.99(9) . . ? O6 Mn1 O9 179.02(9) . . ? O13 Mn1 O9 88.47(8) . . ? O6 Mn1 O1 90.37(9) . . ? O13 Mn1 O1 173.89(8) . . ? O9 Mn1 O1 89.26(8) . . ? O6 Mn1 N1 87.41(9) . . ? O13 Mn1 N1 96.62(9) . . ? O9 Mn1 N1 91.68(9) . . ? O1 Mn1 N1 89.12(9) . . ? O6 Mn1 O15 98.24(8) . . ? O13 Mn1 O15 83.05(8) . . ? O9 Mn1 O15 82.67(7) . . ? O1 Mn1 O15 91.04(7) . . ? N1 Mn1 O15 174.34(8) . . ? O5 Mn2 O2 93.21(8) . . ? O5 Mn2 O45 169.62(10) . . ? O2 Mn2 O45 96.73(10) . . ? O5 Mn2 O20 90.45(9) . . ? O2 Mn2 O20 84.27(8) . . ? O45 Mn2 O20 87.56(10) . . ? O5 Mn2 O18 80.97(8) . . ? O2 Mn2 O18 173.83(8) . . ? O45 Mn2 O18 89.20(9) . . ? O20 Mn2 O18 97.73(8) . . ? O5 Mn2 O15 97.95(8) . . ? O2 Mn2 O15 85.80(7) . . ? O45 Mn2 O15 85.80(9) . . ? O20 Mn2 O15 167.33(8) . . ? O18 Mn2 O15 92.96(7) . . ? O19 Mn3 O22 167.25(9) . . ? O19 Mn3 O7 82.80(8) . . ? O22 Mn3 O7 87.58(8) . . ? O19 Mn3 N5 92.20(9) . . ? O22 Mn3 N5 96.81(10) . . ? O7 Mn3 N5 173.83(9) . . ? O19 Mn3 N2 103.46(9) . . ? O22 Mn3 N2 85.68(9) . . ? O7 Mn3 N2 95.19(8) . . ? N5 Mn3 N2 89.48(9) . . ? O19 Mn3 O23 87.18(9) . . ? O22 Mn3 O23 84.95(9) . . ? O7 Mn3 O23 92.85(8) . . ? N5 Mn3 O23 83.25(9) . . ? N2 Mn3 O23 167.38(9) . . ? C1 O1 Mn1 128.01(18) . . ? C1 O2 Mn2 141.68(19) . . ? C9 O5 Mn2 136.78(19) . . ? C9 O6 Mn1 136.9(2) . . ? C31 O7 Mn3 145.71(17) . . ? C32 O9 Mn1 128.93(18) . . ? C59 O13 Mn1 133.74(19) . . ? Mn2 O15 Mn1 106.33(7) . . ? Mn2 O18 H18A 121.9 . . ? Mn2 O18 H18B 112.0 . . ? H18A O18 H18B 98.0 . . ? Mn3 O19 H19A 154.9 . . ? Mn3 O19 H19B 94.7 . . ? H19A O19 H19B 108.6 . . ? Mn2 O20 H20A 144.6 . . ? Mn2 O20 H20B 109.9 . . ? H20A O20 H20B 105.1 . . ? Mn3 O23 H23A 122.9 . . ? Mn3 O23 H23B 123.1 . . ? H23A O23 H23B 96.9 . . ? Mn3 O22 H22A 136.7 . . ? Mn3 O22 H22B 112.6 . . ? H22A O22 H22B 104.2 . . ? Mn2 O45 H45A 127.0 . . ? Mn2 O45 H45B 122.9 . . ? H45A O45 H45B 107.3 . . ? C23 N1 C24 104.6(3) . . ? C23 N1 Mn1 127.3(2) . . ? C24 N1 Mn1 127.5(2) . . ? C20 N2 C34 104.7(3) . . ? C20 N2 Mn3 126.7(2) . . ? C34 N2 Mn3 128.7(2) . . ? C20 N3 C33 107.0(3) . . ? C20 N3 C35 125.8(3) . . ? C33 N3 C35 127.0(3) . . ? C10 N4 C12 106.8(3) . . ? C10 N4 C13 125.9(3) . . ? C12 N4 C13 127.3(3) . . ? C10 N5 C11 104.8(3) . . ? C10 N5 Mn3 125.6(2) . . ? C11 N5 Mn3 129.1(2) . . ? C23 N6 C22 107.1(3) . . ? C23 N6 C21 124.4(3) . . ? C22 N6 C21 127.8(3) . . ? O12 N7 O11 123.0(3) . . ? O12 N7 C25 119.6(3) . . ? O11 N7 C25 117.4(3) . . ? O17 N8 O16 123.8(3) . . ? O17 N8 C6 118.2(3) . . ? O16 N8 C6 118.0(3) . . ? O2 C1 O1 126.1(3) . . ? O2 C1 C2 117.0(2) . . ? O1 C1 C2 116.8(2) . . ? C7 C2 C3 119.9(3) . . ? C7 C2 C1 117.7(2) . . ? C3 C2 C1 122.2(2) . . ? C2 C3 C4 119.0(2) . . ? C2 C3 C8 121.0(2) . . ? C4 C3 C8 120.0(2) . . ? C5 C4 C3 120.5(2) . . ? C5 C4 C9 117.5(2) . 4_556 ? C3 C4 C9 122.0(2) . 4_556 ? C4 C5 C6 119.3(3) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C7 C6 C5 121.8(3) . . ? C7 C6 N8 119.8(3) . . ? C5 C6 N8 118.4(3) . . ? C6 C7 C2 119.5(3) . . ? C6 C7 H7 120.3 . . ? C2 C7 H7 120.3 . . ? O3 C8 O4 125.8(3) . . ? O3 C8 C3 116.9(2) . . ? O4 C8 C3 117.2(2) . . ? O5 C9 O6 126.7(3) . . ? O5 C9 C4 117.5(2) . 4 ? O6 C9 C4 115.8(3) . 4 ? N5 C10 N4 112.0(3) . . ? N5 C10 H10 124.0 . . ? N4 C10 H10 124.0 . . ? C12 C11 N5 109.9(3) . . ? C12 C11 H11 125.1 . . ? N5 C11 H11 125.1 . . ? C11 C12 N4 106.5(3) . . ? C11 C12 H12 126.7 . . ? N4 C12 H12 126.7 . . ? N4 C13 C14 114.1(3) . 3_557 ? N4 C13 H13A 108.7 . . ? C14 C13 H13A 108.7 3_557 . ? N4 C13 H13B 108.7 . . ? C14 C13 H13B 108.7 3_557 . ? H13A C13 H13B 107.6 . . ? C19 C14 C15 118.3(3) . . ? C19 C14 C13 121.5(3) . 3_557 ? C15 C14 C13 120.1(3) . 3_557 ? C14 C15 C16 121.1(3) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C17 C16 C15 120.7(3) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 118.5(3) . . ? C16 C17 C21 121.4(4) . . ? C18 C17 C21 119.9(4) . . ? C19 C18 C17 120.8(3) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C14 C19 C18 120.5(3) . . ? C14 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? N2 C20 N3 112.0(3) . . ? N2 C20 H20 124.0 . . ? N3 C20 H20 124.0 . . ? C34 C33 N3 106.1(3) . . ? C34 C33 H33 126.9 . . ? N3 C33 H33 126.9 . . ? C33 C34 N2 110.3(3) . . ? C33 C34 H34 124.9 . . ? N2 C34 H34 124.9 . . ? N3 C35 C36 113.6(3) . . ? N3 C35 H35A 108.8 . . ? C36 C35 H35A 108.8 . . ? N3 C35 H35B 108.8 . . ? C36 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? C38 C36 C37 118.8(3) . . ? C38 C36 C35 123.0(3) . . ? C37 C36 C35 118.2(3) . . ? C38 C37 C36 120.4(3) 3_557 . ? C38 C37 H37 119.8 3_557 . ? C36 C37 H37 119.8 . . ? C36 C38 C37 120.9(3) . 3_557 ? C36 C38 H38 119.6 . . ? C37 C38 H38 119.6 3_557 . ? N1 C23 N6 111.9(3) . . ? N1 C23 H23 124.0 . . ? N6 C23 H23 124.0 . . ? C24 C22 N6 106.2(3) . . ? C24 C22 H22 126.9 . . ? N6 C22 H22 126.9 . . ? C22 C24 N1 110.1(3) . . ? C22 C24 H24 124.9 . . ? N1 C24 H24 124.9 . . ? O10 C32 O9 124.4(3) . . ? O10 C32 C29 120.8(2) . . ? O9 C32 C29 114.9(2) . . ? C30 C29 C28 120.0(2) . . ? C30 C29 C32 115.1(2) . . ? C28 C29 C32 124.9(2) . . ? C25 C30 C29 119.8(3) . . ? C25 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C30 C25 C26 121.5(3) . . ? C30 C25 N7 118.7(3) . . ? C26 C25 N7 119.7(3) . . ? C25 C26 C27 120.1(3) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C26 C27 C28 119.6(3) . . ? C26 C27 C59 115.5(2) . 4_566 ? C28 C27 C59 124.8(2) . 4_566 ? C29 C28 C27 118.8(2) . . ? C29 C28 C31 119.3(2) . . ? C27 C28 C31 121.8(2) . . ? O8 C31 O7 124.5(2) . . ? O8 C31 C28 115.8(2) . . ? O7 C31 C28 119.6(2) . . ? O14 C59 O13 124.7(3) . . ? O14 C59 C27 120.6(3) . 4_565 ? O13 C59 C27 114.7(3) . 4_565 ? N6 C21 C17 113.5(3) . . ? N6 C21 H21A 108.9 . . ? C17 C21 H21A 108.9 . . ? N6 C21 H21B 108.9 . . ? C17 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? H2W O21 H1W 95.3 . . ? H4W O24 H3W 96.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Mn1 O1 C1 52.7(2) . . . . ? O13 Mn1 O1 C1 -60.0(9) . . . . ? O9 Mn1 O1 C1 -128.2(2) . . . . ? N1 Mn1 O1 C1 140.1(2) . . . . ? O15 Mn1 O1 C1 -45.5(2) . . . . ? O5 Mn2 O2 C1 -48.0(3) . . . . ? O45 Mn2 O2 C1 135.1(3) . . . . ? O20 Mn2 O2 C1 -138.1(3) . . . . ? O18 Mn2 O2 C1 -28.8(9) . . . . ? O15 Mn2 O2 C1 49.8(3) . . . . ? O2 Mn2 O5 C9 59.4(3) . . . . ? O45 Mn2 O5 C9 -137.5(5) . . . . ? O20 Mn2 O5 C9 143.7(3) . . . . ? O18 Mn2 O5 C9 -118.6(3) . . . . ? O15 Mn2 O5 C9 -26.8(3) . . . . ? O13 Mn1 O6 C9 85.6(3) . . . . ? O9 Mn1 O6 C9 -156(5) . . . . ? O1 Mn1 O6 C9 -88.7(3) . . . . ? N1 Mn1 O6 C9 -177.8(3) . . . . ? O15 Mn1 O6 C9 2.4(3) . . . . ? O19 Mn3 O7 C31 -113.5(3) . . . . ? O22 Mn3 O7 C31 74.9(3) . . . . ? N5 Mn3 O7 C31 -149.5(8) . . . . ? N2 Mn3 O7 C31 -10.5(3) . . . . ? O23 Mn3 O7 C31 159.7(3) . . . . ? O6 Mn1 O9 C32 106(5) . . . . ? O13 Mn1 O9 C32 -135.6(2) . . . . ? O1 Mn1 O9 C32 38.7(2) . . . . ? N1 Mn1 O9 C32 127.8(2) . . . . ? O15 Mn1 O9 C32 -52.4(2) . . . . ? O6 Mn1 O13 C59 -144.3(3) . . . . ? O9 Mn1 O13 C59 36.6(3) . . . . ? O1 Mn1 O13 C59 -31.6(9) . . . . ? N1 Mn1 O13 C59 128.1(3) . . . . ? O15 Mn1 O13 C59 -46.2(3) . . . . ? O5 Mn2 O15 Mn1 38.98(9) . . . . ? O2 Mn2 O15 Mn1 -53.68(8) . . . . ? O45 Mn2 O15 Mn1 -150.76(10) . . . . ? O20 Mn2 O15 Mn1 -92.2(4) . . . . ? O18 Mn2 O15 Mn1 120.26(8) . . . . ? O6 Mn1 O15 Mn2 -32.63(10) . . . . ? O13 Mn1 O15 Mn2 -123.65(9) . . . . ? O9 Mn1 O15 Mn2 147.01(9) . . . . ? O1 Mn1 O15 Mn2 57.89(9) . . . . ? N1 Mn1 O15 Mn2 149.4(8) . . . . ? O6 Mn1 N1 C23 -130.4(3) . . . . ? O13 Mn1 N1 C23 -38.7(3) . . . . ? O9 Mn1 N1 C23 49.9(3) . . . . ? O1 Mn1 N1 C23 139.2(3) . . . . ? O15 Mn1 N1 C23 47.6(10) . . . . ? O6 Mn1 N1 C24 39.3(3) . . . . ? O13 Mn1 N1 C24 131.0(3) . . . . ? O9 Mn1 N1 C24 -140.3(3) . . . . ? O1 Mn1 N1 C24 -51.1(3) . . . . ? O15 Mn1 N1 C24 -142.7(7) . . . . ? O19 Mn3 N2 C20 172.3(2) . . . . ? O22 Mn3 N2 C20 1.3(2) . . . . ? O7 Mn3 N2 C20 88.5(2) . . . . ? N5 Mn3 N2 C20 -95.6(3) . . . . ? O23 Mn3 N2 C20 -40.9(6) . . . . ? O19 Mn3 N2 C34 -7.8(3) . . . . ? O22 Mn3 N2 C34 -178.8(3) . . . . ? O7 Mn3 N2 C34 -91.6(3) . . . . ? N5 Mn3 N2 C34 84.3(3) . . . . ? O23 Mn3 N2 C34 139.0(4) . . . . ? O19 Mn3 N5 C10 152.7(3) . . . . ? O22 Mn3 N5 C10 -36.3(3) . . . . ? O7 Mn3 N5 C10 -171.5(7) . . . . ? N2 Mn3 N5 C10 49.2(3) . . . . ? O23 Mn3 N5 C10 -120.4(3) . . . . ? O19 Mn3 N5 C11 -36.8(3) . . . . ? O22 Mn3 N5 C11 134.2(3) . . . . ? O7 Mn3 N5 C11 -1.0(10) . . . . ? N2 Mn3 N5 C11 -140.3(3) . . . . ? O23 Mn3 N5 C11 50.1(3) . . . . ? Mn2 O2 C1 O1 -35.4(5) . . . . ? Mn2 O2 C1 C2 142.8(2) . . . . ? Mn1 O1 C1 O2 30.7(4) . . . . ? Mn1 O1 C1 C2 -147.45(19) . . . . ? O2 C1 C2 C7 -157.2(3) . . . . ? O1 C1 C2 C7 21.2(4) . . . . ? O2 C1 C2 C3 18.1(4) . . . . ? O1 C1 C2 C3 -163.5(2) . . . . ? C7 C2 C3 C4 3.4(4) . . . . ? C1 C2 C3 C4 -171.8(2) . . . . ? C7 C2 C3 C8 -179.1(2) . . . . ? C1 C2 C3 C8 5.8(4) . . . . ? C2 C3 C4 C5 -1.8(4) . . . . ? C8 C3 C4 C5 -179.4(2) . . . . ? C2 C3 C4 C9 175.7(2) . . . 4_556 ? C8 C3 C4 C9 -1.8(4) . . . 4_556 ? C3 C4 C5 C6 -1.0(4) . . . . ? C9 C4 C5 C6 -178.7(2) 4_556 . . . ? C4 C5 C6 C7 2.3(4) . . . . ? C4 C5 C6 N8 179.1(2) . . . . ? O17 N8 C6 C7 14.7(4) . . . . ? O16 N8 C6 C7 -166.7(3) . . . . ? O17 N8 C6 C5 -162.1(3) . . . . ? O16 N8 C6 C5 16.5(4) . . . . ? C5 C6 C7 C2 -0.8(4) . . . . ? N8 C6 C7 C2 -177.5(3) . . . . ? C3 C2 C7 C6 -2.1(4) . . . . ? C1 C2 C7 C6 173.3(3) . . . . ? C2 C3 C8 O3 72.8(3) . . . . ? C4 C3 C8 O3 -109.7(3) . . . . ? C2 C3 C8 O4 -108.4(3) . . . . ? C4 C3 C8 O4 69.1(3) . . . . ? Mn2 O5 C9 O6 -8.0(5) . . . . ? Mn2 O5 C9 C4 174.38(19) . . . 4 ? Mn1 O6 C9 O5 23.7(5) . . . . ? Mn1 O6 C9 C4 -158.6(2) . . . 4 ? C11 N5 C10 N4 0.1(4) . . . . ? Mn3 N5 C10 N4 172.5(2) . . . . ? C12 N4 C10 N5 -0.1(4) . . . . ? C13 N4 C10 N5 -179.6(3) . . . . ? C10 N5 C11 C12 0.0(4) . . . . ? Mn3 N5 C11 C12 -172.0(2) . . . . ? N5 C11 C12 N4 0.0(4) . . . . ? C10 N4 C12 C11 0.1(4) . . . . ? C13 N4 C12 C11 179.5(3) . . . . ? C10 N4 C13 C14 -85.2(4) . . . 3_557 ? C12 N4 C13 C14 95.4(4) . . . 3_557 ? C19 C14 C15 C16 2.9(5) . . . . ? C13 C14 C15 C16 -173.5(3) 3_557 . . . ? C14 C15 C16 C17 -0.5(6) . . . . ? C15 C16 C17 C18 -1.8(5) . . . . ? C15 C16 C17 C21 172.5(3) . . . . ? C16 C17 C18 C19 1.8(5) . . . . ? C21 C17 C18 C19 -172.6(3) . . . . ? C15 C14 C19 C18 -2.9(5) . . . . ? C13 C14 C19 C18 173.5(3) 3_557 . . . ? C17 C18 C19 C14 0.6(5) . . . . ? C34 N2 C20 N3 -0.6(4) . . . . ? Mn3 N2 C20 N3 179.31(19) . . . . ? C33 N3 C20 N2 0.3(4) . . . . ? C35 N3 C20 N2 175.7(3) . . . . ? C20 N3 C33 C34 0.1(4) . . . . ? C35 N3 C33 C34 -175.2(3) . . . . ? N3 C33 C34 N2 -0.4(4) . . . . ? C20 N2 C34 C33 0.6(4) . . . . ? Mn3 N2 C34 C33 -179.3(2) . . . . ? C20 N3 C35 C36 119.2(3) . . . . ? C33 N3 C35 C36 -66.3(4) . . . . ? N3 C35 C36 C38 -23.6(5) . . . . ? N3 C35 C36 C37 157.9(3) . . . . ? C38 C36 C37 C38 0.3(5) . . . 3_557 ? C35 C36 C37 C38 178.9(3) . . . 3_557 ? C37 C36 C38 C37 -0.3(5) . . . 3_557 ? C35 C36 C38 C37 -178.8(3) . . . 3_557 ? C24 N1 C23 N6 0.4(4) . . . . ? Mn1 N1 C23 N6 172.0(2) . . . . ? C22 N6 C23 N1 -0.6(4) . . . . ? C21 N6 C23 N1 -171.1(4) . . . . ? C23 N6 C22 C24 0.5(4) . . . . ? C21 N6 C22 C24 170.6(4) . . . . ? N6 C22 C24 N1 -0.3(4) . . . . ? C23 N1 C24 C22 -0.1(4) . . . . ? Mn1 N1 C24 C22 -171.7(2) . . . . ? Mn1 O9 C32 O10 35.5(4) . . . . ? Mn1 O9 C32 C29 -144.10(19) . . . . ? O10 C32 C29 C30 -162.9(2) . . . . ? O9 C32 C29 C30 16.7(3) . . . . ? O10 C32 C29 C28 17.7(4) . . . . ? O9 C32 C29 C28 -162.7(3) . . . . ? C28 C29 C30 C25 0.9(4) . . . . ? C32 C29 C30 C25 -178.5(3) . . . . ? C29 C30 C25 C26 1.0(5) . . . . ? C29 C30 C25 N7 -178.5(3) . . . . ? O12 N7 C25 C30 -5.7(5) . . . . ? O11 N7 C25 C30 171.2(4) . . . . ? O12 N7 C25 C26 174.7(3) . . . . ? O11 N7 C25 C26 -8.3(5) . . . . ? C30 C25 C26 C27 -1.5(5) . . . . ? N7 C25 C26 C27 178.0(3) . . . . ? C25 C26 C27 C28 -0.1(4) . . . . ? C25 C26 C27 C59 179.9(3) . . . 4_566 ? C30 C29 C28 C27 -2.4(4) . . . . ? C32 C29 C28 C27 177.0(2) . . . . ? C30 C29 C28 C31 -178.7(2) . . . . ? C32 C29 C28 C31 0.6(4) . . . . ? C26 C27 C28 C29 2.0(4) . . . . ? C59 C27 C28 C29 -178.0(2) 4_566 . . . ? C26 C27 C28 C31 178.2(2) . . . . ? C59 C27 C28 C31 -1.7(4) 4_566 . . . ? Mn3 O7 C31 O8 -161.3(2) . . . . ? Mn3 O7 C31 C28 17.6(4) . . . . ? C29 C28 C31 O8 84.3(3) . . . . ? C27 C28 C31 O8 -92.0(3) . . . . ? C29 C28 C31 O7 -94.7(3) . . . . ? C27 C28 C31 O7 89.1(3) . . . . ? Mn1 O13 C59 O14 49.2(4) . . . . ? Mn1 O13 C59 C27 -132.2(2) . . . 4_565 ? C23 N6 C21 C17 -151.1(4) . . . . ? C22 N6 C21 C17 40.3(6) . . . . ? C16 C17 C21 N6 76.9(5) . . . . ? C18 C17 C21 N6 -108.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.525 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.084 _database_code_depnum_ccdc_archive 'CCDC 823182'