# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author_name 'Lahcene Ouahab' _publ_contact_author_address ; Organometalliques et Materiaux Moleculaires UMR 6226 CNRS-Universite de Rennes 1 Sciences Chimiques de Rennes 35042 Rennes Cedex France. ; _publ_contact_author_email lahcene.ouahab@univ-rennes1.fr _publ_contact_author_phone '+33 2 23 23 56 59' _publ_contact_author_fax '33 2 23 23 68 40' loop_ _publ_author_name _publ_author_address K.S.Gavrilenko ;Organometalliques et Materiaux Moleculaires UMR 6226 CNRS-Universite de Rennes 1 Sciences Chimiques de Rennes 35042 Rennes Cedex France. ; 'Y.Le Gal' ;Organometalliques et Materiaux Moleculaires UMR 6226 CNRS-Universite de Rennes 1 Sciences Chimiques de Rennes 35042 Rennes Cedex France. ; O.Cador ;Organometalliques et Materiaux Moleculaires UMR 6226 CNRS-Universite de Rennes 1 Sciences Chimiques de Rennes 35042 Rennes Cedex France. ; S.Golhen ;Organometalliques et Materiaux Moleculaires UMR 6226 CNRS-Universite de Rennes 1 Sciences Chimiques de Rennes 35042 Rennes Cedex France. ; L.Ouahab ;Organometalliques et Materiaux Moleculaires UMR 6226 CNRS-Universite de Rennes 1 Sciences Chimiques de Rennes 35042 Rennes Cedex France. ; _publ_section_title ; First trinuclear paramagnetic transition metal complexes with redox active ligands derived from TTF: Co2M(PhCOO)6(TTF-CH=CH-py)2*2CH3CN, M = CoII, MnII ; data_1 _database_code_depnum_ccdc_archive 'CCDC 620532' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H54 Co3 N4 O12 S8' _chemical_formula_weight 1600.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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 10.7106(5) _cell_length_b 11.7808(7) _cell_length_c 15.0518(11) _cell_angle_alpha 94.946(2) _cell_angle_beta 105.939(2) _cell_angle_gamma 90.940(4) _cell_volume 1817.82(19) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5210 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 25.350 _exptl_crystal_description block _exptl_crystal_colour 'deep red' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 819 _exptl_absorpt_coefficient_mu 0.969 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10126 _diffrn_reflns_av_R_equivalents 0.0512 _diffrn_reflns_av_sigmaI/netI 0.0923 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 25.32 _reflns_number_total 6173 _reflns_number_gt 3440 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0600P)^2^+0.2834P] 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 6173 _refine_ls_number_parameters 449 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1172 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1538 _refine_ls_wR_factor_gt 0.1227 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 0.4043(5) 0.2428(5) 0.4589(4) 0.0589(13) Uani 1 1 d . . . C2 C 0.4093(5) 0.1368(5) 0.3953(4) 0.0627(14) Uani 1 1 d . . . C3 C 0.4611(7) 0.1421(6) 0.3231(5) 0.100(2) Uani 1 1 d . . . H3 H 0.4916 0.2120 0.3112 0.120 Uiso 1 1 calc R . . C4 C 0.4692(9) 0.0449(8) 0.2669(5) 0.116(3) Uani 1 1 d . . . H4 H 0.5072 0.0497 0.2186 0.140 Uiso 1 1 calc R . . C5 C 0.4229(7) -0.0565(7) 0.2812(6) 0.102(2) Uani 1 1 d . . . H5 H 0.4270 -0.1211 0.2423 0.123 Uiso 1 1 calc R . . C6 C 0.3702(8) -0.0642(6) 0.3525(6) 0.109(2) Uani 1 1 d . . . H6 H 0.3390 -0.1345 0.3631 0.130 Uiso 1 1 calc R . . C7 C 0.3625(6) 0.0333(6) 0.4104(5) 0.0904(19) Uani 1 1 d . . . H7 H 0.3257 0.0279 0.4592 0.108 Uiso 1 1 calc R . . C8 C 0.2426(5) 0.5426(5) 0.5525(4) 0.0586(13) Uani 1 1 d . . . C9 C 0.1532(5) 0.6395(4) 0.5503(4) 0.0588(13) Uani 1 1 d . . . C10 C 0.1727(6) 0.7365(6) 0.5103(5) 0.0900(19) Uani 1 1 d . . . H10 H 0.2413 0.7422 0.4839 0.108 Uiso 1 1 calc R . . C11 C 0.0890(8) 0.8269(6) 0.5094(6) 0.110(3) Uani 1 1 d . . . H11 H 0.1018 0.8923 0.4820 0.132 Uiso 1 1 calc R . . C12 C -0.0106(8) 0.8194(7) 0.5483(6) 0.103(2) Uani 1 1 d . . . H12 H -0.0652 0.8800 0.5478 0.124 Uiso 1 1 calc R . . C13 C -0.0311(6) 0.7248(7) 0.5877(5) 0.102(2) Uani 1 1 d . . . H13 H -0.0995 0.7205 0.6145 0.123 Uiso 1 1 calc R . . C14 C 0.0494(5) 0.6342(5) 0.5885(4) 0.0811(18) Uani 1 1 d . . . H14 H 0.0338 0.5688 0.6149 0.097 Uiso 1 1 calc R . . C15 C 0.5726(5) 0.4056(4) 0.7069(4) 0.0547(12) Uani 1 1 d . . . C16 C 0.7096(5) 0.4325(5) 0.7624(3) 0.0576(13) Uani 1 1 d . . . C17 C 0.7867(6) 0.5096(5) 0.7350(4) 0.0787(17) Uani 1 1 d . . . H17 H 0.7537 0.5441 0.6806 0.094 Uiso 1 1 calc R . . C18 C 0.9121(6) 0.5357(7) 0.7880(5) 0.095(2) Uani 1 1 d . . . H18 H 0.9633 0.5890 0.7703 0.114 Uiso 1 1 calc R . . C19 C 0.9609(6) 0.4829(7) 0.8666(5) 0.094(2) Uani 1 1 d . . . H19 H 1.0465 0.4994 0.9012 0.113 Uiso 1 1 calc R . . C20 C 0.8865(6) 0.4060(6) 0.8959(5) 0.0874(19) Uani 1 1 d . . . H20 H 0.9213 0.3713 0.9500 0.105 Uiso 1 1 calc R . . C21 C 0.7601(6) 0.3808(5) 0.8443(4) 0.0675(15) Uani 1 1 d . . . H21 H 0.7084 0.3297 0.8639 0.081 Uiso 1 1 calc R . . C22 C 0.1294(6) 0.2834(5) 0.7110(4) 0.0762(17) Uani 1 1 d . . . H22 H 0.1172 0.3610 0.7076 0.091 Uiso 1 1 calc R . . C23 C 0.0550(6) 0.2233(5) 0.7533(5) 0.0826(18) Uani 1 1 d . . . H23 H -0.0052 0.2608 0.7781 0.099 Uiso 1 1 calc R . . C24 C 0.0687(5) 0.1075(5) 0.7595(4) 0.0668(14) Uani 1 1 d . . . C25 C 0.1582(5) 0.0581(5) 0.7181(4) 0.0702(15) Uani 1 1 d . . . H25 H 0.1697 -0.0200 0.7180 0.084 Uiso 1 1 calc R . . C26 C 0.2292(5) 0.1234(5) 0.6775(4) 0.0672(15) Uani 1 1 d . . . H26 H 0.2883 0.0877 0.6504 0.081 Uiso 1 1 calc R . . C27 C -0.0054(5) 0.0400(5) 0.8067(4) 0.0727(16) Uani 1 1 d . . . H27 H -0.0076 -0.0391 0.7964 0.087 Uiso 1 1 calc R . . C28 C -0.0690(6) 0.0870(5) 0.8634(4) 0.0812(17) Uani 1 1 d . . . H28 H -0.0630 0.1661 0.8730 0.097 Uiso 1 1 calc R . . C29 C -0.1484(6) 0.0288(6) 0.9130(4) 0.0798(17) Uani 1 1 d . . . C30 C -0.2116(6) 0.0864(5) 0.9663(5) 0.0880(19) Uani 1 1 d . . . H30 H -0.2031 0.1655 0.9761 0.106 Uiso 1 1 calc R . . C31 C -0.2674(5) -0.1224(5) 0.9764(4) 0.0734(16) Uani 1 1 d . . . C32 C -0.3093(5) -0.2190(5) 1.0001(4) 0.0687(15) Uani 1 1 d . . . C33 C -0.3988(7) -0.3689(6) 1.0788(5) 0.099(2) Uani 1 1 d . . . H33 H -0.4367 -0.4062 1.1174 0.119 Uiso 1 1 calc R . . C34 C -0.3353(7) -0.4259(6) 1.0271(5) 0.100(2) Uani 1 1 d . . . H34 H -0.3290 -0.5045 1.0275 0.120 Uiso 1 1 calc R . . C35 C 0.7119(11) 0.3137(10) 0.1540(8) 0.140(4) Uani 1 1 d . . . C36 C 0.6193(12) 0.3261(12) 0.2005(7) 0.206(6) Uani 1 1 d . . . H36A H 0.6290 0.4009 0.2330 0.309 Uiso 1 1 calc R . . H36B H 0.6293 0.2699 0.2442 0.309 Uiso 1 1 calc R . . H36C H 0.5346 0.3162 0.1571 0.309 Uiso 1 1 calc R . . N1 N 0.2184(4) 0.2356(4) 0.6745(3) 0.0628(11) Uani 1 1 d . . . N2 N 0.7847(11) 0.3098(10) 0.1126(9) 0.203(5) Uani 1 1 d . . . O1 O 0.4445(4) 0.3351(3) 0.4395(3) 0.0764(11) Uani 1 1 d . . . O2 O 0.3585(3) 0.2287(3) 0.5258(3) 0.0693(10) Uani 1 1 d . . . O3 O 0.3135(3) 0.5410(3) 0.4999(3) 0.0742(11) Uani 1 1 d . . . O4 O 0.2376(3) 0.4686(3) 0.6081(3) 0.0686(10) Uani 1 1 d . . . O5 O 0.5295(3) 0.4451(3) 0.6316(2) 0.0678(10) Uani 1 1 d . . . O6 O 0.5003(3) 0.3428(3) 0.7379(2) 0.0653(9) Uani 1 1 d . . . S1 S -0.16716(16) -0.11826(14) 0.90113(13) 0.0848(5) Uani 1 1 d . . . S2 S -0.30936(18) 0.01143(15) 1.01669(14) 0.0952(6) Uani 1 1 d . . . S3 S -0.26493(18) -0.35237(15) 0.95922(13) 0.0912(5) Uani 1 1 d . . . S4 S -0.41011(16) -0.22654(14) 1.07354(12) 0.0825(5) Uani 1 1 d . . . Co1 Co 0.5000 0.5000 0.5000 0.0531(3) Uani 1 2 d S . . Co2 Co 0.34087(6) 0.33405(6) 0.62677(5) 0.0582(2) 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 0.052(3) 0.062(3) 0.062(4) 0.007(3) 0.014(3) 0.002(3) C2 0.058(3) 0.062(4) 0.067(4) 0.005(3) 0.014(3) 0.008(3) C3 0.145(6) 0.080(5) 0.094(5) 0.000(4) 0.069(5) -0.003(4) C4 0.171(8) 0.098(6) 0.097(6) -0.001(5) 0.068(5) 0.023(6) C5 0.106(5) 0.086(6) 0.100(6) -0.014(5) 0.007(5) 0.034(4) C6 0.122(6) 0.067(5) 0.130(7) -0.011(5) 0.032(6) -0.003(4) C7 0.095(5) 0.073(4) 0.104(5) -0.001(4) 0.032(4) 0.003(4) C8 0.049(3) 0.067(3) 0.058(3) 0.007(3) 0.011(3) 0.000(3) C9 0.053(3) 0.062(3) 0.063(3) 0.012(3) 0.016(2) 0.004(2) C10 0.082(4) 0.090(5) 0.105(5) 0.028(4) 0.031(4) 0.008(4) C11 0.103(5) 0.073(5) 0.146(7) 0.036(5) 0.012(5) 0.011(4) C12 0.096(5) 0.092(6) 0.113(6) 0.004(5) 0.016(5) 0.036(5) C13 0.078(4) 0.129(7) 0.107(6) 0.014(5) 0.034(4) 0.039(5) C14 0.073(4) 0.084(4) 0.099(5) 0.027(4) 0.040(3) 0.022(3) C15 0.061(3) 0.056(3) 0.054(3) 0.006(3) 0.027(3) 0.006(2) C16 0.061(3) 0.069(3) 0.047(3) 0.003(3) 0.022(2) 0.005(3) C17 0.076(4) 0.106(5) 0.057(4) 0.008(3) 0.025(3) -0.021(3) C18 0.074(4) 0.135(6) 0.077(5) -0.008(5) 0.030(4) -0.030(4) C19 0.063(4) 0.139(7) 0.070(5) -0.016(4) 0.007(3) -0.002(4) C20 0.082(4) 0.102(5) 0.070(4) -0.003(4) 0.009(4) 0.013(4) C21 0.078(4) 0.065(4) 0.060(4) 0.004(3) 0.020(3) 0.007(3) C22 0.087(4) 0.061(4) 0.102(5) 0.014(3) 0.059(4) 0.002(3) C23 0.090(4) 0.071(4) 0.112(5) 0.018(4) 0.067(4) 0.008(3) C24 0.074(3) 0.064(4) 0.071(4) 0.014(3) 0.034(3) -0.008(3) C25 0.078(4) 0.063(4) 0.079(4) 0.007(3) 0.037(3) 0.000(3) C26 0.065(3) 0.072(4) 0.077(4) 0.013(3) 0.038(3) 0.003(3) C27 0.074(3) 0.071(4) 0.085(4) 0.012(3) 0.039(3) -0.006(3) C28 0.093(4) 0.073(4) 0.089(5) 0.017(3) 0.042(4) -0.016(3) C29 0.076(4) 0.092(5) 0.081(4) 0.014(4) 0.035(3) 0.002(3) C30 0.100(5) 0.076(4) 0.108(5) 0.023(4) 0.058(4) 0.003(4) C31 0.073(3) 0.078(4) 0.083(4) 0.021(3) 0.040(3) 0.004(3) C32 0.064(3) 0.072(4) 0.076(4) 0.007(3) 0.031(3) -0.001(3) C33 0.128(6) 0.092(5) 0.098(5) 0.017(4) 0.064(5) -0.014(4) C34 0.124(6) 0.081(5) 0.113(6) 0.021(4) 0.061(5) -0.002(4) C35 0.138(9) 0.144(9) 0.133(9) -0.006(7) 0.036(7) -0.033(7) C36 0.180(10) 0.338(18) 0.108(8) -0.006(9) 0.067(8) -0.072(10) N1 0.064(3) 0.060(3) 0.071(3) 0.009(2) 0.030(2) -0.002(2) N2 0.205(11) 0.166(9) 0.244(13) -0.045(8) 0.096(9) -0.035(8) O1 0.111(3) 0.063(2) 0.065(3) 0.006(2) 0.041(2) -0.007(2) O2 0.073(2) 0.072(2) 0.074(3) 0.006(2) 0.039(2) -0.0016(19) O3 0.064(2) 0.099(3) 0.075(3) 0.031(2) 0.039(2) 0.024(2) O4 0.073(2) 0.064(2) 0.084(3) 0.023(2) 0.042(2) 0.0143(19) O5 0.068(2) 0.084(3) 0.058(2) 0.024(2) 0.0227(19) 0.0008(19) O6 0.066(2) 0.069(2) 0.067(2) 0.0183(19) 0.0269(19) -0.0013(18) S1 0.0927(11) 0.0797(11) 0.1032(13) 0.0163(9) 0.0605(10) 0.0015(9) S2 0.1133(13) 0.0801(11) 0.1209(15) 0.0202(10) 0.0771(12) 0.0093(10) S3 0.1065(12) 0.0834(12) 0.1037(13) 0.0104(10) 0.0620(11) 0.0057(10) S4 0.0869(10) 0.0854(11) 0.0908(12) 0.0078(9) 0.0514(9) -0.0053(9) Co1 0.0567(5) 0.0580(6) 0.0526(6) 0.0146(5) 0.0260(5) 0.0017(4) Co2 0.0595(4) 0.0615(5) 0.0629(5) 0.0144(4) 0.0299(3) 0.0012(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 O1 1.250(6) . ? C1 O2 1.257(6) . ? C1 C2 1.516(7) . ? C2 C3 1.354(8) . ? C2 C7 1.372(8) . ? C3 C4 1.383(9) . ? C4 C5 1.342(10) . ? C5 C6 1.351(10) . ? C6 C7 1.398(9) . ? C8 O3 1.237(6) . ? C8 O4 1.269(6) . ? C8 C9 1.499(7) . ? C9 C10 1.376(8) . ? C9 C14 1.387(7) . ? C10 C11 1.402(9) . ? C11 C12 1.355(10) . ? C12 C13 1.350(10) . ? C13 C14 1.382(8) . ? C15 O5 1.235(6) . ? C15 O6 1.266(6) . ? C15 C16 1.489(7) . ? C16 C17 1.380(7) . ? C16 C21 1.399(7) . ? C17 C18 1.374(8) . ? C18 C19 1.363(9) . ? C19 C20 1.374(9) . ? C20 C21 1.376(8) . ? C22 N1 1.335(6) . ? C22 C23 1.370(7) . ? C23 C24 1.383(7) . ? C24 C25 1.390(7) . ? C24 C27 1.467(7) . ? C25 C26 1.365(7) . ? C26 N1 1.332(6) . ? C27 C28 1.323(8) . ? C28 C29 1.472(8) . ? C29 C30 1.335(8) . ? C29 S1 1.730(7) . ? C30 S2 1.724(6) . ? C31 C32 1.329(7) . ? C31 S2 1.750(6) . ? C31 S1 1.765(5) . ? C32 S4 1.750(5) . ? C32 S3 1.758(6) . ? C33 C34 1.317(8) . ? C33 S4 1.690(7) . ? C34 S3 1.708(7) . ? C35 N2 1.122(12) . ? C35 C36 1.366(14) . ? N1 Co2 2.048(4) . ? O1 Co1 2.078(4) . ? O2 Co2 1.930(4) . ? O3 Co1 2.063(3) . ? O4 Co2 1.944(3) . ? O5 Co1 2.080(3) . ? O5 Co2 2.370(4) . ? O6 Co2 2.029(4) . ? Co1 O3 2.063(3) 2_666 ? Co1 O1 2.078(4) 2_666 ? Co1 O5 2.080(3) 2_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 126.4(5) . . ? O1 C1 C2 117.4(5) . . ? O2 C1 C2 116.2(5) . . ? C3 C2 C7 118.6(6) . . ? C3 C2 C1 120.8(6) . . ? C7 C2 C1 120.6(5) . . ? C2 C3 C4 120.8(7) . . ? C5 C4 C3 120.7(8) . . ? C4 C5 C6 119.8(7) . . ? C5 C6 C7 120.1(8) . . ? C2 C7 C6 120.0(7) . . ? O3 C8 O4 125.9(5) . . ? O3 C8 C9 117.6(5) . . ? O4 C8 C9 116.5(4) . . ? C10 C9 C14 118.3(5) . . ? C10 C9 C8 120.4(5) . . ? C14 C9 C8 121.3(5) . . ? C9 C10 C11 119.8(6) . . ? C12 C11 C10 120.3(7) . . ? C13 C12 C11 120.6(7) . . ? C12 C13 C14 120.0(7) . . ? C13 C14 C9 120.9(6) . . ? O5 C15 O6 120.2(5) . . ? O5 C15 C16 120.2(5) . . ? O6 C15 C16 119.6(5) . . ? C17 C16 C21 119.5(5) . . ? C17 C16 C15 120.8(5) . . ? C21 C16 C15 119.7(5) . . ? C18 C17 C16 120.2(6) . . ? C19 C18 C17 119.6(7) . . ? C18 C19 C20 121.6(6) . . ? C19 C20 C21 119.3(6) . . ? C20 C21 C16 119.7(6) . . ? N1 C22 C23 123.0(5) . . ? C22 C23 C24 120.7(5) . . ? C23 C24 C25 115.6(5) . . ? C23 C24 C27 122.9(5) . . ? C25 C24 C27 121.5(5) . . ? C26 C25 C24 120.4(5) . . ? N1 C26 C25 123.5(5) . . ? C28 C27 C24 122.7(6) . . ? C27 C28 C29 127.7(6) . . ? C30 C29 C28 122.0(6) . . ? C30 C29 S1 117.3(5) . . ? C28 C29 S1 120.7(5) . . ? C29 C30 S2 118.8(5) . . ? C32 C31 S2 122.3(4) . . ? C32 C31 S1 123.0(5) . . ? S2 C31 S1 114.7(3) . . ? C31 C32 S4 124.3(4) . . ? C31 C32 S3 121.4(4) . . ? S4 C32 S3 114.2(3) . . ? C34 C33 S4 118.7(5) . . ? C33 C34 S3 118.5(5) . . ? N2 C35 C36 175.2(16) . . ? C26 N1 C22 116.7(4) . . ? C26 N1 Co2 122.5(3) . . ? C22 N1 Co2 120.6(4) . . ? C1 O1 Co1 139.8(4) . . ? C1 O2 Co2 131.2(4) . . ? C8 O3 Co1 139.2(3) . . ? C8 O4 Co2 126.2(3) . . ? C15 O5 Co1 166.0(3) . . ? C15 O5 Co2 83.1(3) . . ? Co1 O5 Co2 106.16(15) . . ? C15 O6 Co2 98.0(3) . . ? C29 S1 C31 94.6(3) . . ? C30 S2 C31 94.4(3) . . ? C34 S3 C32 93.7(3) . . ? C33 S4 C32 94.3(3) . . ? O3 Co1 O3 180.000(1) 2_666 . ? O3 Co1 O1 86.36(16) 2_666 . ? O3 Co1 O1 93.64(16) . . ? O3 Co1 O1 93.64(16) 2_666 2_666 ? O3 Co1 O1 86.36(16) . 2_666 ? O1 Co1 O1 180.000(1) . 2_666 ? O3 Co1 O5 90.45(14) 2_666 . ? O3 Co1 O5 89.55(14) . . ? O1 Co1 O5 90.64(15) . . ? O1 Co1 O5 89.36(15) 2_666 . ? O3 Co1 O5 89.55(14) 2_666 2_666 ? O3 Co1 O5 90.45(14) . 2_666 ? O1 Co1 O5 89.36(15) . 2_666 ? O1 Co1 O5 90.64(15) 2_666 2_666 ? O5 Co1 O5 180.00(7) . 2_666 ? O2 Co2 O4 123.02(16) . . ? O2 Co2 O6 112.44(15) . . ? O4 Co2 O6 117.55(16) . . ? O2 Co2 N1 98.50(17) . . ? O4 Co2 N1 98.48(16) . . ? O6 Co2 N1 99.62(16) . . ? O2 Co2 O5 93.73(14) . . ? O4 Co2 O5 90.12(14) . . ? O6 Co2 O5 58.47(13) . . ? N1 Co2 O5 157.84(16) . . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 25.32 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 0.292 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.059 data_2 _database_code_depnum_ccdc_archive 'CCDC 620533' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H54 Co2 Mn N4 O12 S8' _chemical_formula_weight 1596.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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 10.6124(3) _cell_length_b 11.7260(3) _cell_length_c 14.9724(5) _cell_angle_alpha 95.5940(10) _cell_angle_beta 106.8340(11) _cell_angle_gamma 90.2950(12) _cell_volume 1773.76(9) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7634 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description losange _exptl_crystal_colour 'deep red' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 817 _exptl_absorpt_coefficient_mu 0.937 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14183 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 27.57 _reflns_number_total 8135 _reflns_number_gt 6262 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0487P)^2^+1.0328P] 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 8135 _refine_ls_number_parameters 449 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1185 _refine_ls_wR_factor_gt 0.1064 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4034(3) 0.2334(2) 0.45897(19) 0.0369(5) Uani 1 1 d . . . C2 C 0.4067(3) 0.1269(2) 0.3947(2) 0.0400(6) Uani 1 1 d . . . C3 C 0.4580(4) 0.1338(3) 0.3209(2) 0.0567(8) Uani 1 1 d . . . H3 H 0.4893 0.2041 0.3107 0.068 Uiso 1 1 calc R . . C4 C 0.4634(4) 0.0362(3) 0.2613(3) 0.0651(9) Uani 1 1 d . . . H4 H 0.4985 0.0413 0.2116 0.078 Uiso 1 1 calc R . . C5 C 0.4169(4) -0.0677(3) 0.2761(3) 0.0605(9) Uani 1 1 d . . . H5 H 0.4203 -0.1328 0.2362 0.073 Uiso 1 1 calc R . . C6 C 0.3655(3) -0.0758(3) 0.3492(3) 0.0600(9) Uani 1 1 d . . . H6 H 0.3344 -0.1464 0.3590 0.072 Uiso 1 1 calc R . . C7 C 0.3596(3) 0.0219(2) 0.4095(2) 0.0482(7) Uani 1 1 d . . . H7 H 0.3244 0.0164 0.4591 0.058 Uiso 1 1 calc R . . C8 C 0.2325(2) 0.5400(2) 0.55346(18) 0.0355(5) Uani 1 1 d . . . C9 C 0.1414(2) 0.6374(2) 0.55344(19) 0.0366(5) Uani 1 1 d . . . C10 C 0.1583(3) 0.7354(3) 0.5124(2) 0.0479(7) Uani 1 1 d . . . H10 H 0.2247 0.7399 0.4836 0.057 Uiso 1 1 calc R . . C11 C 0.0759(3) 0.8264(3) 0.5146(3) 0.0574(8) Uani 1 1 d . . . H11 H 0.0885 0.8928 0.4885 0.069 Uiso 1 1 calc R . . C12 C -0.0240(3) 0.8190(3) 0.5550(2) 0.0546(8) Uani 1 1 d . . . H12 H -0.0798 0.8799 0.5551 0.066 Uiso 1 1 calc R . . C13 C -0.0425(3) 0.7227(3) 0.5952(2) 0.0508(7) Uani 1 1 d . . . H13 H -0.1103 0.7183 0.6228 0.061 Uiso 1 1 calc R . . C14 C 0.0406(3) 0.6316(3) 0.5947(2) 0.0439(6) Uani 1 1 d . . . H14 H 0.0284 0.5662 0.6222 0.053 Uiso 1 1 calc R . . C15 C 0.5741(3) 0.4046(2) 0.71221(17) 0.0337(5) Uani 1 1 d . . . C16 C 0.7133(3) 0.4283(2) 0.76829(18) 0.0360(5) Uani 1 1 d . . . C17 C 0.7918(3) 0.5038(3) 0.7396(2) 0.0445(6) Uani 1 1 d . . . H17 H 0.7574 0.5383 0.6847 0.053 Uiso 1 1 calc R . . C18 C 0.9208(3) 0.5272(3) 0.7928(2) 0.0504(7) Uani 1 1 d . . . H18 H 0.9730 0.5785 0.7742 0.061 Uiso 1 1 calc R . . C19 C 0.9724(3) 0.4748(3) 0.8734(2) 0.0523(7) Uani 1 1 d . . . H19 H 1.0597 0.4902 0.9085 0.063 Uiso 1 1 calc R . . C20 C 0.8950(3) 0.3990(3) 0.9028(2) 0.0479(7) Uani 1 1 d . . . H20 H 0.9304 0.3638 0.9572 0.057 Uiso 1 1 calc R . . C21 C 0.7649(3) 0.3764(2) 0.85046(19) 0.0390(6) Uani 1 1 d . . . H21 H 0.7121 0.3267 0.8701 0.047 Uiso 1 1 calc R . . C22 C 0.1273(3) 0.2782(2) 0.7128(2) 0.0446(6) Uani 1 1 d . . . H22 H 0.1154 0.3566 0.7109 0.053 Uiso 1 1 calc R . . C23 C 0.0526(3) 0.2181(3) 0.7543(2) 0.0481(7) Uani 1 1 d . . . H23 H -0.0090 0.2555 0.7789 0.058 Uiso 1 1 calc R . . C24 C 0.0689(3) 0.1003(2) 0.7596(2) 0.0400(6) Uani 1 1 d . . . C25 C 0.1590(3) 0.0497(2) 0.7175(2) 0.0401(6) Uani 1 1 d . . . H25 H 0.1715 -0.0288 0.7173 0.048 Uiso 1 1 calc R . . C26 C 0.2294(3) 0.1158(2) 0.67643(19) 0.0384(6) Uani 1 1 d . . . H26 H 0.2885 0.0801 0.6484 0.046 Uiso 1 1 calc R . . C27 C -0.0047(3) 0.0336(2) 0.8070(2) 0.0430(6) Uani 1 1 d . . . H27 H -0.0093 -0.0459 0.7947 0.052 Uiso 1 1 calc R . . C28 C -0.0652(3) 0.0817(3) 0.8668(2) 0.0457(6) Uani 1 1 d . . . H28 H -0.0553 0.1610 0.8793 0.055 Uiso 1 1 calc R . . C29 C -0.1447(3) 0.0254(3) 0.9150(2) 0.0439(6) Uani 1 1 d . . . C30 C -0.2057(3) 0.0841(3) 0.9702(2) 0.0475(7) Uani 1 1 d . . . H30 H -0.1932 0.1632 0.9828 0.057 Uiso 1 1 calc R . . C31 C -0.2702(3) -0.1248(2) 0.9752(2) 0.0409(6) Uani 1 1 d . . . C32 C -0.3126(3) -0.2222(2) 0.9977(2) 0.0400(6) Uani 1 1 d . . . C33 C -0.3977(3) -0.3739(3) 1.0790(2) 0.0517(7) Uani 1 1 d . . . H33 H -0.4323 -0.4111 1.1192 0.062 Uiso 1 1 calc R . . C34 C -0.3369(3) -0.4315(3) 1.0242(2) 0.0518(7) Uani 1 1 d . . . H34 H -0.3280 -0.5103 1.0247 0.062 Uiso 1 1 calc R . . C35 C 0.7178(4) 0.3146(3) 0.1522(3) 0.0632(9) Uani 1 1 d . . . C36 C 0.6285(5) 0.3149(6) 0.2075(3) 0.1047(18) Uani 1 1 d . . . H36A H 0.6197 0.3921 0.2325 0.157 Uiso 1 1 calc R . . H36B H 0.6617 0.2686 0.2582 0.157 Uiso 1 1 calc R . . H36C H 0.5440 0.2843 0.1691 0.157 Uiso 1 1 calc R . . N1 N 0.2166(2) 0.22999(19) 0.67495(16) 0.0375(5) Uani 1 1 d . . . N2 N 0.7873(4) 0.3149(3) 0.1072(3) 0.0860(11) Uani 1 1 d . . . O1 O 0.4437(2) 0.32599(17) 0.44043(15) 0.0525(5) Uani 1 1 d . . . O2 O 0.35834(18) 0.21988(15) 0.52701(13) 0.0394(4) Uani 1 1 d . . . O3 O 0.30134(19) 0.53668(19) 0.49888(14) 0.0467(5) Uani 1 1 d . . . O4 O 0.23116(18) 0.46564(16) 0.61053(14) 0.0407(4) Uani 1 1 d . . . O5 O 0.52857(18) 0.44464(18) 0.63578(13) 0.0443(5) Uani 1 1 d . . . O6 O 0.50009(18) 0.34158(15) 0.74177(13) 0.0383(4) Uani 1 1 d . . . S1 S -0.17111(7) -0.12363(6) 0.89862(6) 0.04604(18) Uani 1 1 d . . . S2 S -0.30848(8) 0.01132(6) 1.01823(6) 0.04869(19) Uani 1 1 d . . . S3 S -0.27415(8) -0.35656(6) 0.95170(6) 0.04767(18) Uani 1 1 d . . . S4 S -0.41123(7) -0.22798(6) 1.07403(5) 0.04423(17) Uani 1 1 d . . . Co2 Co 0.33881(3) 0.32995(3) 0.62771(2) 0.03456(10) Uani 1 1 d . . . Mn1 Mn 0.5000 0.5000 0.5000 0.03172(13) Uani 1 2 d S . . 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 0.0334(13) 0.0387(13) 0.0374(14) 0.0029(11) 0.0086(11) 0.0043(10) C2 0.0356(13) 0.0420(14) 0.0390(14) 0.0015(11) 0.0062(11) 0.0077(11) C3 0.077(2) 0.0481(17) 0.0488(18) 0.0001(14) 0.0253(17) 0.0081(15) C4 0.084(3) 0.062(2) 0.0497(19) -0.0025(16) 0.0231(18) 0.0186(18) C5 0.064(2) 0.0485(18) 0.055(2) -0.0100(15) 0.0010(17) 0.0215(15) C6 0.0571(19) 0.0391(16) 0.075(2) -0.0065(15) 0.0093(18) 0.0038(13) C7 0.0433(15) 0.0426(15) 0.0565(18) -0.0006(13) 0.0129(14) 0.0029(12) C8 0.0317(12) 0.0422(13) 0.0342(13) 0.0071(10) 0.0113(10) 0.0028(10) C9 0.0315(13) 0.0397(13) 0.0372(14) 0.0049(11) 0.0075(11) 0.0019(10) C10 0.0432(15) 0.0491(16) 0.0525(17) 0.0140(13) 0.0131(13) 0.0016(12) C11 0.061(2) 0.0420(16) 0.066(2) 0.0165(15) 0.0105(17) 0.0027(14) C12 0.0462(17) 0.0492(17) 0.061(2) -0.0003(14) 0.0055(15) 0.0130(13) C13 0.0409(16) 0.0590(18) 0.0549(18) 0.0079(15) 0.0170(14) 0.0135(13) C14 0.0386(14) 0.0488(16) 0.0485(16) 0.0115(13) 0.0173(13) 0.0082(12) C15 0.0389(13) 0.0369(12) 0.0282(12) 0.0020(10) 0.0149(10) 0.0043(10) C16 0.0400(14) 0.0382(13) 0.0318(13) 0.0005(10) 0.0145(11) 0.0014(10) C17 0.0435(15) 0.0579(17) 0.0346(14) 0.0033(12) 0.0159(12) -0.0035(12) C18 0.0455(16) 0.0653(19) 0.0426(16) -0.0028(14) 0.0189(14) -0.0109(14) C19 0.0384(15) 0.070(2) 0.0434(16) -0.0085(15) 0.0094(13) -0.0018(14) C20 0.0493(17) 0.0530(17) 0.0367(15) 0.0016(12) 0.0061(13) 0.0084(13) C21 0.0408(14) 0.0412(14) 0.0353(13) 0.0025(11) 0.0120(11) 0.0050(11) C22 0.0499(16) 0.0419(15) 0.0505(17) 0.0092(12) 0.0267(14) 0.0050(12) C23 0.0523(17) 0.0447(15) 0.0594(19) 0.0107(13) 0.0337(15) 0.0075(13) C24 0.0377(14) 0.0454(15) 0.0397(14) 0.0074(12) 0.0147(12) -0.0033(11) C25 0.0420(14) 0.0376(13) 0.0428(15) 0.0053(11) 0.0154(12) 0.0001(11) C26 0.0378(13) 0.0406(14) 0.0388(14) 0.0033(11) 0.0146(11) 0.0012(11) C27 0.0413(15) 0.0442(15) 0.0470(16) 0.0087(12) 0.0174(13) -0.0006(11) C28 0.0451(16) 0.0506(16) 0.0435(16) 0.0112(13) 0.0144(13) 0.0029(12) C29 0.0439(15) 0.0487(16) 0.0426(15) 0.0101(12) 0.0165(13) 0.0049(12) C30 0.0529(17) 0.0469(16) 0.0485(17) 0.0118(13) 0.0216(14) 0.0036(13) C31 0.0379(14) 0.0492(15) 0.0400(15) 0.0064(12) 0.0175(12) 0.0031(11) C32 0.0382(14) 0.0458(15) 0.0387(14) 0.0038(11) 0.0158(12) 0.0029(11) C33 0.0565(18) 0.0515(17) 0.0539(18) 0.0057(14) 0.0269(15) -0.0087(14) C34 0.0549(18) 0.0484(16) 0.0581(19) 0.0026(14) 0.0268(16) -0.0044(13) C35 0.065(2) 0.065(2) 0.054(2) -0.0016(16) 0.0124(18) -0.0117(17) C36 0.077(3) 0.176(6) 0.060(3) 0.004(3) 0.022(2) -0.017(3) N1 0.0373(12) 0.0426(12) 0.0357(11) 0.0059(9) 0.0150(10) 0.0013(9) N2 0.092(3) 0.077(2) 0.093(3) -0.005(2) 0.039(2) -0.0158(19) O1 0.0779(15) 0.0383(10) 0.0500(12) -0.0015(9) 0.0344(11) -0.0068(10) O2 0.0395(10) 0.0407(10) 0.0424(10) 0.0049(8) 0.0184(8) 0.0037(8) O3 0.0392(10) 0.0676(13) 0.0415(11) 0.0185(9) 0.0203(9) 0.0142(9) O4 0.0400(10) 0.0437(10) 0.0461(11) 0.0131(8) 0.0219(9) 0.0080(8) O5 0.0406(10) 0.0618(12) 0.0335(10) 0.0153(9) 0.0121(8) 0.0036(9) O6 0.0386(10) 0.0384(9) 0.0402(10) 0.0067(8) 0.0144(8) 0.0003(7) S1 0.0482(4) 0.0478(4) 0.0509(4) 0.0080(3) 0.0272(3) 0.0034(3) S2 0.0535(4) 0.0465(4) 0.0563(5) 0.0095(3) 0.0307(4) 0.0069(3) S3 0.0528(4) 0.0475(4) 0.0506(4) 0.0026(3) 0.0283(4) 0.0036(3) S4 0.0426(4) 0.0501(4) 0.0459(4) 0.0016(3) 0.0232(3) -0.0014(3) Co2 0.03478(19) 0.03751(19) 0.03548(19) 0.00730(14) 0.01549(15) 0.00256(13) Mn1 0.0338(3) 0.0355(3) 0.0300(3) 0.0064(2) 0.0148(2) 0.0023(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.249(3) . ? C1 O2 1.267(3) . ? C1 C2 1.508(4) . ? C2 C3 1.373(4) . ? C2 C7 1.387(4) . ? C3 C4 1.394(4) . ? C4 C5 1.373(5) . ? C5 C6 1.368(5) . ? C6 C7 1.401(4) . ? C8 O3 1.242(3) . ? C8 O4 1.282(3) . ? C8 C9 1.500(3) . ? C9 C14 1.387(4) . ? C9 C10 1.388(4) . ? C10 C11 1.388(4) . ? C11 C12 1.371(5) . ? C12 C13 1.370(5) . ? C13 C14 1.389(4) . ? C15 O5 1.245(3) . ? C15 O6 1.272(3) . ? C15 C16 1.482(4) . ? C16 C17 1.391(4) . ? C16 C21 1.394(4) . ? C17 C18 1.381(4) . ? C18 C19 1.378(5) . ? C19 C20 1.391(5) . ? C20 C21 1.386(4) . ? C22 N1 1.340(3) . ? C22 C23 1.370(4) . ? C23 C24 1.400(4) . ? C24 C25 1.395(4) . ? C24 C27 1.466(4) . ? C25 C26 1.375(4) . ? C26 N1 1.349(3) . ? C27 C28 1.331(4) . ? C28 C29 1.452(4) . ? C29 C30 1.334(4) . ? C29 S1 1.750(3) . ? C30 S2 1.731(3) . ? C31 C32 1.332(4) . ? C31 S2 1.757(3) . ? C31 S1 1.767(3) . ? C32 S3 1.755(3) . ? C32 S4 1.765(3) . ? C33 C34 1.322(4) . ? C33 S4 1.725(3) . ? C34 S3 1.730(3) . ? C35 N2 1.135(5) . ? C35 C36 1.427(6) . ? N1 Co2 2.057(2) . ? O1 Mn1 2.1541(19) . ? O2 Co2 1.9459(19) . ? O3 Mn1 2.1495(18) . ? O4 Co2 1.9573(18) . ? O5 Mn1 2.1327(18) . ? O5 Co2 2.383(2) . ? O6 Co2 2.0307(19) . ? Mn1 O5 2.1327(18) 2_666 ? Mn1 O3 2.1495(18) 2_666 ? Mn1 O1 2.154(2) 2_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 126.1(2) . . ? O1 C1 C2 117.9(2) . . ? O2 C1 C2 115.9(2) . . ? C3 C2 C7 119.6(3) . . ? C3 C2 C1 119.5(3) . . ? C7 C2 C1 120.9(3) . . ? C2 C3 C4 120.5(3) . . ? C5 C4 C3 119.8(3) . . ? C6 C5 C4 120.3(3) . . ? C5 C6 C7 120.2(3) . . ? C2 C7 C6 119.5(3) . . ? O3 C8 O4 125.4(2) . . ? O3 C8 C9 118.6(2) . . ? O4 C8 C9 116.0(2) . . ? C14 C9 C10 119.2(3) . . ? C14 C9 C8 120.8(2) . . ? C10 C9 C8 120.0(2) . . ? C11 C10 C9 119.8(3) . . ? C12 C11 C10 120.3(3) . . ? C13 C12 C11 120.6(3) . . ? C12 C13 C14 119.6(3) . . ? C9 C14 C13 120.5(3) . . ? O5 C15 O6 119.3(2) . . ? O5 C15 C16 120.9(2) . . ? O6 C15 C16 119.8(2) . . ? C17 C16 C21 120.1(3) . . ? C17 C16 C15 119.9(2) . . ? C21 C16 C15 120.0(2) . . ? C18 C17 C16 119.8(3) . . ? C19 C18 C17 120.2(3) . . ? C18 C19 C20 120.6(3) . . ? C21 C20 C19 119.5(3) . . ? C20 C21 C16 119.8(3) . . ? N1 C22 C23 123.4(3) . . ? C22 C23 C24 119.9(3) . . ? C25 C24 C23 116.5(2) . . ? C25 C24 C27 121.7(3) . . ? C23 C24 C27 121.8(3) . . ? C26 C25 C24 120.0(3) . . ? N1 C26 C25 122.9(2) . . ? C28 C27 C24 122.9(3) . . ? C27 C28 C29 127.9(3) . . ? C30 C29 C28 122.2(3) . . ? C30 C29 S1 116.7(2) . . ? C28 C29 S1 121.0(2) . . ? C29 C30 S2 119.3(2) . . ? C32 C31 S2 123.1(2) . . ? C32 C31 S1 122.0(2) . . ? S2 C31 S1 114.86(16) . . ? C31 C32 S3 121.7(2) . . ? C31 C32 S4 123.7(2) . . ? S3 C32 S4 114.56(15) . . ? C34 C33 S4 118.3(2) . . ? C33 C34 S3 118.3(3) . . ? N2 C35 C36 179.0(5) . . ? C22 N1 C26 117.1(2) . . ? C22 N1 Co2 120.49(18) . . ? C26 N1 Co2 122.15(17) . . ? C1 O1 Mn1 141.76(19) . . ? C1 O2 Co2 130.41(17) . . ? C8 O3 Mn1 138.73(18) . . ? C8 O4 Co2 125.85(16) . . ? C15 O5 Mn1 164.65(18) . . ? C15 O5 Co2 83.27(15) . . ? Mn1 O5 Co2 106.78(8) . . ? C15 O6 Co2 98.81(16) . . ? C29 S1 C31 94.46(13) . . ? C30 S2 C31 94.14(14) . . ? C34 S3 C32 93.94(14) . . ? C33 S4 C32 93.91(14) . . ? O2 Co2 O4 125.17(8) . . ? O2 Co2 O6 112.39(8) . . ? O4 Co2 O6 116.28(8) . . ? O2 Co2 N1 97.49(8) . . ? O4 Co2 N1 98.05(8) . . ? O6 Co2 N1 99.42(8) . . ? O2 Co2 O5 94.99(7) . . ? O4 Co2 O5 89.94(7) . . ? O6 Co2 O5 58.31(7) . . ? N1 Co2 O5 157.43(8) . . ? O5 Mn1 O5 180.00(4) . 2_666 ? O5 Mn1 O3 87.55(7) . . ? O5 Mn1 O3 92.45(7) 2_666 . ? O5 Mn1 O3 92.45(7) . 2_666 ? O5 Mn1 O3 87.55(7) 2_666 2_666 ? O3 Mn1 O3 180.00(11) . 2_666 ? O5 Mn1 O1 91.37(8) . 2_666 ? O5 Mn1 O1 88.63(8) 2_666 2_666 ? O3 Mn1 O1 88.31(9) . 2_666 ? O3 Mn1 O1 91.69(9) 2_666 2_666 ? O5 Mn1 O1 88.63(8) . . ? O5 Mn1 O1 91.37(8) 2_666 . ? O3 Mn1 O1 91.69(9) . . ? O3 Mn1 O1 88.31(9) 2_666 . ? O1 Mn1 O1 180.0 2_666 . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.464 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.072