Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jie Zhang' _publ_contact_author_address ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter, Chinese Academy of Scie No.155, Yang-Qiao West road, Fuzhou Fuzhou 350002 CHINA ; _publ_contact_author_email ZHANGJIE@FJIRSM.AC.CN _publ_section_title ; The first series of molecular assemblies constructed from a Pi-Pi conjugated redox-active bipyridinium cation with magnetic dimetallic oxalate-bridged trimeric clusters ; _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA ; loop_ _publ_author_name 'Jie Zhang' 'Yan-Qiong Sun' 'Guo-Yu Yang' data_s_1 _database_code_depnum_ccdc_archive 'CCDC 265930' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H69 Fe2 Mn N12 O38.50' _chemical_formula_weight 1836.99 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.9876(4) _cell_length_b 20.4369(6) _cell_length_c 15.9420(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.3650(10) _cell_angle_gamma 90.00 _cell_volume 3853.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8260 _cell_measurement_theta_min 3.0357 _cell_measurement_theta_max 27.4835 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1892 _exptl_absorpt_coefficient_mu 0.639 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8744 _exptl_absorpt_correction_T_max 1.0000 _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 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type ; Mercury70 (2x2 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29888 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.48 _reflns_number_total 15187 _reflns_number_gt 14645 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0619P)^2^+2.0006P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.333(10) _refine_ls_number_reflns 15187 _refine_ls_number_parameters 1127 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.1062 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.080 _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 Fe1 Fe 0.48835(3) 0.71792(2) 0.96718(2) 0.01748(9) Uani 1 1 d . . . Fe2 Fe 0.92867(3) 1.03732(2) 0.57657(2) 0.01854(9) Uani 1 1 d . . . Mn1 Mn 0.70474(4) 0.88029(3) 0.77228(3) 0.01767(9) Uani 1 1 d . . . O1 O 0.57964(16) 0.80284(11) 0.76115(12) 0.0189(4) Uani 1 1 d . . . O2 O 0.67547(16) 0.86788(11) 0.90373(12) 0.0197(4) Uani 1 1 d . . . O3 O 0.48828(16) 0.73938(11) 0.84247(12) 0.0202(4) Uani 1 1 d . . . O4 O 0.57814(17) 0.80378(11) 0.97994(12) 0.0209(4) Uani 1 1 d . . . O5 O 0.63339(18) 0.66806(12) 0.96620(14) 0.0268(5) Uani 1 1 d . . . O6 O 0.53214(18) 0.70182(12) 1.09177(13) 0.0257(5) Uani 1 1 d . . . O7 O 0.7947(2) 0.64413(16) 1.0535(2) 0.0473(7) Uani 1 1 d . . . O8 O 0.6835(3) 0.6762(2) 1.18780(17) 0.0569(9) Uani 1 1 d . . . O9 O 0.38192(16) 0.64497(11) 0.93048(13) 0.0210(4) Uani 1 1 d . . . O10 O 0.34476(18) 0.76221(12) 0.98017(14) 0.0252(4) Uani 1 1 d . . . O11 O 0.19820(19) 0.61901(13) 0.91113(16) 0.0328(5) Uani 1 1 d . . . O12 O 0.1577(2) 0.74685(15) 0.96211(17) 0.0364(6) Uani 1 1 d . . . O13 O 0.73864(16) 0.88969(11) 0.64150(12) 0.0208(4) Uani 1 1 d . . . O14 O 0.82796(16) 0.95915(11) 0.78271(12) 0.0208(4) Uani 1 1 d . . . O15 O 0.84254(17) 0.95010(11) 0.56558(13) 0.0212(4) Uani 1 1 d . . . O16 O 0.92156(17) 1.02015(11) 0.70102(13) 0.0226(4) Uani 1 1 d . . . O17 O 1.07137(18) 0.99260(12) 0.56315(14) 0.0269(5) Uani 1 1 d . . . O18 O 1.03217(17) 1.11134(12) 0.61054(14) 0.0259(5) Uani 1 1 d . . . O19 O 1.2553(2) 1.01166(16) 0.56577(19) 0.0431(7) Uani 1 1 d . . . O20 O 1.21389(19) 1.13948(15) 0.62357(17) 0.0370(6) Uani 1 1 d . . . O21 O 0.89556(18) 1.05396(13) 0.45170(13) 0.0275(5) Uani 1 1 d . . . O22 O 0.77808(17) 1.08369(12) 0.56968(15) 0.0264(5) Uani 1 1 d . . . O23 O 0.7703(2) 1.10220(17) 0.35215(16) 0.0453(7) Uani 1 1 d . . . O24 O 0.62456(19) 1.10481(15) 0.47429(19) 0.0429(7) Uani 1 1 d . . . N1 N -0.3609(2) 0.45474(15) 1.21113(15) 0.0210(5) Uani 1 1 d . . . N2 N 0.11365(18) 0.45550(13) 1.00248(15) 0.0181(5) Uani 1 1 d . . . N3 N 0.1812(2) 0.41287(15) 0.88865(15) 0.0246(6) Uani 1 1 d . . . N4 N 0.2621(2) 0.39888(15) 0.84016(16) 0.0248(6) Uani 1 1 d . . . N5 N 0.44256(19) 0.40173(14) 0.81037(16) 0.0209(5) Uani 1 1 d . . . N6 N 0.8441(2) 0.2931(2) 0.56343(19) 0.0399(8) Uani 1 1 d . . . N7 N 0.7478(2) 0.42806(19) 0.90366(17) 0.0340(7) Uani 1 1 d . . . N8 N 1.1419(2) 0.33548(15) 0.64334(16) 0.0259(6) Uani 1 1 d . . . N9 N 1.3181(2) 0.35099(17) 0.60921(17) 0.0326(7) Uani 1 1 d . . . N10 N 1.3995(2) 0.34233(17) 0.55943(17) 0.0301(6) Uani 1 1 d . . . N11 N 1.47240(19) 0.30101(14) 0.44752(15) 0.0185(5) Uani 1 1 d . . . N12 N 1.9573(2) 0.30631(15) 0.25284(16) 0.0247(6) Uani 1 1 d . . . C1 C -0.3392(2) 0.40622(16) 1.15928(18) 0.0208(6) Uani 1 1 d . . . H27A H -0.3891 0.3711 1.1514 0.025 Uiso 1 1 calc R . . C2 C -0.2874(2) 0.50460(17) 1.22173(18) 0.0219(6) Uani 1 1 d . . . H28A H -0.3009 0.5390 1.2569 0.026 Uiso 1 1 calc R . . C3 C -0.2477(2) 0.40499(15) 1.11692(18) 0.0194(6) Uani 1 1 d . . . H25A H -0.2372 0.3704 1.0812 0.023 Uiso 1 1 calc R . . C4 C -0.1918(2) 0.50735(16) 1.18263(18) 0.0194(6) Uani 1 1 d . . . H26A H -0.1423 0.5426 1.1924 0.023 Uiso 1 1 calc R . . C5 C -0.1714(2) 0.45686(15) 1.12891(16) 0.0164(5) Uani 1 1 d . . . C6 C -0.0715(2) 0.45736(16) 1.08495(17) 0.0166(5) Uani 1 1 d . . . C7 C -0.0239(2) 0.39818(15) 1.06438(17) 0.0179(5) Uani 1 1 d . . . H21A H -0.0546 0.3587 1.0788 0.021 Uiso 1 1 calc R . . C8 C -0.0225(2) 0.51596(15) 1.06289(18) 0.0200(6) Uani 1 1 d . . . H22A H -0.0521 0.5560 1.0762 0.024 Uiso 1 1 calc R . . C9 C 0.0680(2) 0.39814(15) 1.02300(17) 0.0182(5) Uani 1 1 d . . . H19A H 0.0990 0.3587 1.0090 0.022 Uiso 1 1 calc R . . C10 C 0.0697(2) 0.51387(16) 1.02136(18) 0.0203(6) Uani 1 1 d . . . H20A H 0.1020 0.5526 1.0062 0.024 Uiso 1 1 calc R . . C11 C 0.2063(2) 0.45115(16) 0.95408(18) 0.0190(6) Uani 1 1 d . . . C12 C 0.3625(2) 0.42380(16) 0.86351(18) 0.0203(6) Uani 1 1 d . . . C13 C 0.3121(2) 0.48169(15) 0.98271(17) 0.0180(5) Uani 1 1 d . . . C14 C 0.3975(2) 0.46539(15) 0.93387(17) 0.0185(5) Uani 1 1 d . . . C15 C 0.3393(2) 0.51954(15) 1.05671(18) 0.0198(6) Uani 1 1 d . . . H16A H 0.2842 0.5300 1.0894 0.024 Uiso 1 1 calc R . . C16 C 0.5091(2) 0.48689(16) 0.96030(18) 0.0210(6) Uani 1 1 d . . . H15A H 0.5659 0.4756 0.9296 0.025 Uiso 1 1 calc R . . C17 C 0.4484(2) 0.54080(16) 1.08005(18) 0.0208(5) Uani 1 1 d . . . H18A H 0.4667 0.5663 1.1286 0.025 Uiso 1 1 calc R . . C18 C 0.5331(2) 0.52490(16) 1.03228(19) 0.0226(6) Uani 1 1 d . . . H17A H 0.6063 0.5402 1.0494 0.027 Uiso 1 1 calc R . . C19 C 0.4626(3) 0.33774(18) 0.8060(2) 0.0334(8) Uani 1 1 d . . . H9A H 0.4266 0.3086 0.8375 0.040 Uiso 1 1 calc R . . C20 C 0.4934(3) 0.44531(17) 0.76524(19) 0.0248(6) Uani 1 1 d . . . H10A H 0.4781 0.4897 0.7688 0.030 Uiso 1 1 calc R . . C21 C 0.5365(3) 0.31454(19) 0.7550(2) 0.0344(8) Uani 1 1 d . . . H7A H 0.5498 0.2698 0.7521 0.041 Uiso 1 1 calc R . . C22 C 0.5680(3) 0.42394(18) 0.7140(2) 0.0277(7) Uani 1 1 d . . . H8A H 0.6029 0.4542 0.6833 0.033 Uiso 1 1 calc R . . C23 C 0.5916(2) 0.35799(17) 0.70755(18) 0.0232(6) Uani 1 1 d . . . C24 C 0.6759(2) 0.3347(2) 0.6549(2) 0.0281(7) Uani 1 1 d . . . C25 C 0.7113(3) 0.2699(2) 0.6574(3) 0.0416(9) Uani 1 1 d . . . H3A H 0.6793 0.2392 0.6895 0.050 Uiso 1 1 calc R . . C26 C 0.7250(2) 0.3780(2) 0.60457(19) 0.0332(8) Uani 1 1 d . . . H4A H 0.7027 0.4216 0.5999 0.040 Uiso 1 1 calc R . . C27 C 0.7951(3) 0.2514(2) 0.6112(3) 0.0471(11) Uani 1 1 d . . . H1A H 0.8183 0.2079 0.6136 0.056 Uiso 1 1 calc R . . C28 C 0.8090(3) 0.3541(2) 0.5611(2) 0.0406(10) Uani 1 1 d . . . H2A H 0.8423 0.3836 0.5282 0.049 Uiso 1 1 calc R . . C29 C 0.7708(2) 0.3649(2) 0.89225(19) 0.0328(8) Uani 1 1 d . . . H29A H 0.7306 0.3337 0.9175 0.039 Uiso 1 1 calc R . . C30 C 0.8075(3) 0.4712(2) 0.8687(2) 0.0343(8) Uani 1 1 d . . . H30A H 0.7938 0.5154 0.8766 0.041 Uiso 1 1 calc R . . C31 C 0.8510(2) 0.3432(2) 0.84489(18) 0.0283(7) Uani 1 1 d . . . H31A H 0.8641 0.2987 0.8391 0.034 Uiso 1 1 calc R . . C32 C 0.8912(3) 0.4542(2) 0.8199(2) 0.0324(8) Uani 1 1 d . . . H32A H 0.9321 0.4865 0.7972 0.039 Uiso 1 1 calc R . . C33 C 0.9115(2) 0.38944(19) 0.80623(18) 0.0262(7) Uani 1 1 d . . . C34 C 0.9944(2) 0.36974(19) 0.75050(18) 0.0259(7) Uani 1 1 d . . . C35 C 1.0427(3) 0.30846(19) 0.7549(2) 0.0294(7) Uani 1 1 d . . . H35A H 1.0254 0.2785 0.7948 0.035 Uiso 1 1 calc R . . C36 C 1.0227(3) 0.4139(2) 0.6905(2) 0.0309(7) Uani 1 1 d . . . H36A H 0.9908 0.4555 0.6859 0.037 Uiso 1 1 calc R . . C37 C 1.1167(3) 0.29107(18) 0.7003(2) 0.0289(7) Uani 1 1 d . . . H37A H 1.1487 0.2495 0.7029 0.035 Uiso 1 1 calc R . . C38 C 1.0978(3) 0.3957(2) 0.6381(2) 0.0326(8) Uani 1 1 d . . . H38A H 1.1180 0.4254 0.5989 0.039 Uiso 1 1 calc R . . C39 C 1.2235(2) 0.31917(18) 0.5881(2) 0.0247(7) Uani 1 1 d . . . C40 C 1.3787(2) 0.30273(17) 0.49508(18) 0.0210(6) Uani 1 1 d . . . C41 C 1.1925(2) 0.27715(16) 0.51848(18) 0.0204(6) Uani 1 1 d . . . C42 C 1.2781(2) 0.26770(16) 0.46731(18) 0.0199(6) Uani 1 1 d . . . C43 C 1.0857(2) 0.24800(17) 0.49581(19) 0.0234(6) Uani 1 1 d . . . H44A H 1.0296 0.2541 0.5290 0.028 Uiso 1 1 calc R . . C44 C 1.2541(2) 0.22994(17) 0.39287(18) 0.0229(6) Uani 1 1 d . . . H43A H 1.3083 0.2244 0.3579 0.027 Uiso 1 1 calc R . . C45 C 1.0660(2) 0.21042(19) 0.42384(19) 0.0273(7) Uani 1 1 d . . . H45A H 0.9959 0.1905 0.4085 0.033 Uiso 1 1 calc R . . C46 C 1.1503(3) 0.20154(18) 0.37266(19) 0.0283(7) Uani 1 1 d . . . H46A H 1.1347 0.1758 0.3241 0.034 Uiso 1 1 calc R . . C47 C 1.5192(2) 0.24269(16) 0.42998(18) 0.0222(6) Uani 1 1 d . . . H47A H 1.4888 0.2035 0.4455 0.027 Uiso 1 1 calc R . . C48 C 1.5141(2) 0.35852(16) 0.42619(17) 0.0208(6) Uani 1 1 d . . . H48A H 1.4795 0.3974 0.4382 0.025 Uiso 1 1 calc R . . C49 C 1.6119(2) 0.24260(16) 0.38897(18) 0.0190(6) Uani 1 1 d . . . H49A H 1.6434 0.2032 0.3755 0.023 Uiso 1 1 calc R . . C50 C 1.6086(2) 0.36020(16) 0.38628(18) 0.0192(5) Uani 1 1 d . . . H50A H 1.6383 0.4000 0.3721 0.023 Uiso 1 1 calc R . . C51 C 1.6585(2) 0.30157(16) 0.36761(17) 0.0174(5) Uani 1 1 d . . . C52 C 1.7614(2) 0.30298(16) 0.32709(17) 0.0175(5) Uani 1 1 d . . . C53 C 1.7888(2) 0.25168(16) 0.27616(18) 0.0217(6) Uani 1 1 d . . . H53A H 1.7418 0.2153 0.2662 0.026 Uiso 1 1 calc R . . C54 C 1.8349(2) 0.35593(16) 0.33938(17) 0.0205(6) Uani 1 1 d . . . H54A H 1.8199 0.3911 0.3728 0.025 Uiso 1 1 calc R . . C55 C 1.8866(2) 0.25558(17) 0.24062(19) 0.0241(6) Uani 1 1 d . . . H55A H 1.9038 0.2212 0.2067 0.029 Uiso 1 1 calc R . . C56 C 1.9306(2) 0.35568(17) 0.30136(19) 0.0251(6) Uani 1 1 d . . . H56A H 1.9789 0.3915 0.3098 0.030 Uiso 1 1 calc R . . C57 C 0.5554(2) 0.78462(14) 0.83073(17) 0.0163(5) Uani 1 1 d . . . C58 C 0.6089(2) 0.82266(14) 0.91177(17) 0.0169(5) Uani 1 1 d . . . C59 C 0.6955(3) 0.66223(17) 1.0397(2) 0.0293(7) Uani 1 1 d . . . C60 C 0.6349(3) 0.68111(19) 1.1150(2) 0.0318(7) Uani 1 1 d . . . C61 C 0.2761(2) 0.65729(16) 0.93140(19) 0.0229(6) Uani 1 1 d . . . C62 C 0.2544(2) 0.72781(17) 0.96069(18) 0.0240(6) Uani 1 1 d . . . C63 C 0.8061(2) 0.93378(15) 0.63304(17) 0.0167(5) Uani 1 1 d D . . C64 C 0.8549(2) 0.97471(15) 0.71354(17) 0.0172(5) Uani 1 1 d D . . C65 C 1.1596(2) 1.02974(19) 0.5743(2) 0.0283(7) Uani 1 1 d . . . C66 C 1.1377(2) 1.10035(18) 0.6047(2) 0.0262(6) Uani 1 1 d . . . C67 C 0.7999(3) 1.08270(18) 0.4243(2) 0.0275(7) Uani 1 1 d . . . C68 C 0.7247(3) 1.09162(17) 0.4933(2) 0.0274(7) Uani 1 1 d . . . O1W O 0.83524(18) 0.80811(13) 0.80376(15) 0.0275(5) Uani 1 1 d . . . H2 H 0.9071 0.8019 0.7851 0.080 Uiso 1 1 d R . . H1 H 0.8150 0.7776 0.8172 0.080 Uiso 1 1 d R . . O2W O 0.57465(17) 0.95406(12) 0.73865(14) 0.0233(4) Uani 1 1 d . . . H4 H 0.5044 0.9567 0.7542 0.080 Uiso 1 1 d R . . H3 H 0.5842 0.9928 0.7170 0.080 Uiso 1 1 d R . . O3W O -0.0478(3) 0.7488(2) 1.0287(3) 0.0771(12) Uani 1 1 d . . . O4W O 1.0447(3) 1.15563(16) 0.78935(19) 0.0478(7) Uani 1 1 d . . . H8 H 1.0476 1.1447 0.7331 0.080 Uiso 1 1 d R . . H7 H 1.1097 1.1525 0.8246 0.080 Uiso 1 1 d R . . O5W O 0.6264(3) 1.07896(17) 0.6927(3) 0.0719(12) Uani 1 1 d . . . O6W O 0.5788(2) 1.08888(13) 0.22816(15) 0.0342(5) Uani 1 1 d . . . H12 H 0.5980 1.1014 0.1816 0.080 Uiso 1 1 d R . . H11 H 0.6451 1.0938 0.2611 0.080 Uiso 1 1 d R . . O7W O 0.7120(4) 0.5432(2) 0.6346(3) 0.0132(8) Uani 0.40 1 d P . . O71W O 0.5465(7) 0.5144(5) 0.4947(6) 0.055(2) Uani 0.40 1 d P . . O72W O 0.5963(11) 0.5416(7) 0.5592(7) 0.036(3) Uani 0.20 1 d P . . O81W O 1.4081(5) 1.1100(4) 0.5266(5) 0.069(2) Uani 0.50 1 d P . . O82W O 1.4400(4) 1.1735(4) 0.5950(4) 0.0543(17) Uani 0.50 1 d P . . O9W O 0.8551(7) 1.1493(3) 0.8720(6) 0.176(4) Uani 1 1 d . . . O11W O 0.6533(5) 1.1670(3) 0.8122(3) 0.1036(17) Uani 1 1 d . . . O10W O 0.4649(6) 1.1677(4) 0.6926(5) 0.067(2) Uani 0.50 1 d P . . O12W O 0.7780(2) 0.68275(15) 0.84246(18) 0.0445(7) Uani 1 1 d . . . H23 H 0.8368 0.6773 0.8637 0.080 Uiso 1 1 d R . . H24 H 0.7497 0.6787 0.8892 0.080 Uiso 1 1 d R . . O13W O -0.0241(3) 0.6126(2) 0.8282(3) 0.0822(13) Uani 1 1 d . . . O14W O 0.6221(3) 0.6322(2) 0.7219(2) 0.0748(12) Uani 1 1 d . . . O15W O 1.0538(3) 1.0595(2) 0.3358(3) 0.0718(11) 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 Fe1 0.01726(17) 0.0184(2) 0.01808(17) 0.00225(16) 0.00672(13) 0.00004(15) Fe2 0.01569(17) 0.0208(2) 0.02006(18) 0.00403(16) 0.00580(14) 0.00005(15) Mn1 0.01545(16) 0.0202(2) 0.01865(17) 0.00113(15) 0.00653(13) -0.00221(14) O1 0.0177(9) 0.0230(11) 0.0161(9) 0.0024(8) 0.0030(7) -0.0028(8) O2 0.0208(9) 0.0206(11) 0.0186(9) -0.0041(8) 0.0058(7) -0.0055(8) O3 0.0204(9) 0.0222(11) 0.0189(9) 0.0008(8) 0.0053(7) -0.0046(8) O4 0.0256(10) 0.0220(11) 0.0162(9) -0.0003(8) 0.0070(7) -0.0042(8) O5 0.0252(10) 0.0277(13) 0.0300(11) 0.0030(9) 0.0115(9) 0.0055(9) O6 0.0304(11) 0.0266(13) 0.0209(10) 0.0034(9) 0.0067(8) 0.0014(9) O7 0.0267(12) 0.0440(18) 0.0695(19) 0.0133(15) 0.0026(12) 0.0093(11) O8 0.0624(18) 0.073(2) 0.0288(13) 0.0065(14) -0.0128(12) 0.0131(17) O9 0.0191(9) 0.0204(11) 0.0243(10) 0.0030(8) 0.0055(8) 0.0005(8) O10 0.0226(10) 0.0223(12) 0.0327(11) 0.0006(9) 0.0101(8) 0.0027(8) O11 0.0232(10) 0.0296(14) 0.0435(14) 0.0063(11) -0.0012(9) -0.0051(9) O12 0.0232(11) 0.0408(16) 0.0470(14) 0.0040(12) 0.0112(10) 0.0082(10) O13 0.0191(9) 0.0243(12) 0.0197(9) -0.0018(8) 0.0051(7) -0.0025(8) O14 0.0197(9) 0.0265(12) 0.0170(9) 0.0002(8) 0.0056(7) -0.0060(8) O15 0.0219(9) 0.0238(11) 0.0190(9) 0.0008(8) 0.0063(7) -0.0017(8) O16 0.0221(9) 0.0265(12) 0.0194(9) -0.0016(8) 0.0044(7) -0.0096(8) O17 0.0225(10) 0.0292(13) 0.0307(11) 0.0070(10) 0.0096(9) 0.0056(9) O18 0.0216(10) 0.0250(13) 0.0316(11) 0.0057(9) 0.0064(8) -0.0030(8) O19 0.0208(11) 0.0522(18) 0.0585(17) -0.0010(14) 0.0136(11) 0.0075(11) O20 0.0233(11) 0.0428(17) 0.0433(14) 0.0075(12) 0.0008(10) -0.0076(10) O21 0.0279(10) 0.0343(14) 0.0217(10) 0.0072(9) 0.0076(8) 0.0046(9) O22 0.0210(10) 0.0263(13) 0.0331(12) 0.0035(9) 0.0077(9) 0.0042(9) O23 0.0422(14) 0.060(2) 0.0305(13) 0.0150(13) -0.0032(11) 0.0034(13) O24 0.0211(11) 0.0455(17) 0.0612(17) 0.0224(14) 0.0038(11) 0.0055(11) N1 0.0160(10) 0.0279(15) 0.0209(11) 0.0031(10) 0.0078(9) 0.0013(10) N2 0.0127(9) 0.0236(14) 0.0188(11) 0.0012(10) 0.0052(8) 0.0016(9) N3 0.0167(11) 0.0389(17) 0.0191(11) -0.0045(11) 0.0062(9) -0.0008(10) N4 0.0179(11) 0.0349(16) 0.0236(12) -0.0034(11) 0.0092(9) 0.0001(10) N5 0.0161(10) 0.0268(14) 0.0214(11) -0.0005(10) 0.0083(9) 0.0012(9) N6 0.0213(13) 0.068(3) 0.0313(15) -0.0194(15) 0.0081(11) 0.0016(14) N7 0.0191(12) 0.059(2) 0.0248(13) 0.0001(14) 0.0078(10) 0.0050(13) N8 0.0161(11) 0.0393(17) 0.0247(12) -0.0035(11) 0.0103(9) 0.0019(10) N9 0.0238(13) 0.051(2) 0.0258(13) -0.0110(13) 0.0131(10) -0.0064(12) N10 0.0183(12) 0.0478(19) 0.0262(13) -0.0086(12) 0.0100(10) -0.0036(11) N11 0.0142(10) 0.0271(14) 0.0155(10) 0.0027(10) 0.0067(8) 0.0005(9) N12 0.0158(11) 0.0333(16) 0.0270(12) 0.0010(11) 0.0089(9) -0.0010(10) C1 0.0129(11) 0.0266(16) 0.0240(13) -0.0004(12) 0.0060(10) -0.0046(11) C2 0.0193(12) 0.0258(16) 0.0209(13) -0.0022(12) 0.0041(10) 0.0007(11) C3 0.0159(12) 0.0216(15) 0.0216(13) -0.0023(11) 0.0058(10) -0.0007(10) C4 0.0149(11) 0.0217(15) 0.0221(13) -0.0030(11) 0.0040(10) -0.0019(11) C5 0.0123(11) 0.0215(15) 0.0158(11) 0.0013(10) 0.0032(9) -0.0013(10) C6 0.0121(11) 0.0204(15) 0.0180(12) -0.0013(11) 0.0047(9) -0.0002(10) C7 0.0149(11) 0.0189(15) 0.0201(12) -0.0012(11) 0.0033(9) -0.0025(10) C8 0.0161(12) 0.0201(15) 0.0257(13) 0.0014(11) 0.0083(10) 0.0008(10) C9 0.0152(11) 0.0185(15) 0.0211(13) -0.0004(11) 0.0040(10) 0.0004(10) C10 0.0180(12) 0.0201(15) 0.0244(14) 0.0024(11) 0.0078(10) 0.0003(10) C11 0.0135(12) 0.0270(16) 0.0180(12) 0.0036(11) 0.0068(10) 0.0020(11) C12 0.0171(12) 0.0262(16) 0.0189(12) 0.0022(11) 0.0067(10) 0.0032(11) C13 0.0149(11) 0.0219(15) 0.0181(12) 0.0059(11) 0.0052(9) 0.0025(10) C14 0.0150(11) 0.0234(15) 0.0181(12) 0.0065(11) 0.0057(9) 0.0028(10) C15 0.0175(12) 0.0222(16) 0.0214(13) 0.0031(11) 0.0081(10) 0.0004(10) C16 0.0156(12) 0.0257(16) 0.0234(13) 0.0055(11) 0.0087(10) 0.0042(10) C17 0.0229(12) 0.0191(14) 0.0204(12) 0.0009(11) 0.0039(10) -0.0029(11) C18 0.0156(11) 0.0252(17) 0.0271(14) 0.0082(12) 0.0034(10) -0.0030(11) C19 0.0318(16) 0.0265(18) 0.0475(19) 0.0122(15) 0.0236(15) 0.0083(13) C20 0.0288(14) 0.0214(16) 0.0270(14) -0.0006(12) 0.0126(12) -0.0006(12) C21 0.0311(16) 0.0266(18) 0.050(2) 0.0025(16) 0.0211(15) 0.0080(14) C22 0.0293(15) 0.0306(18) 0.0269(15) -0.0026(13) 0.0155(12) -0.0056(13) C23 0.0143(12) 0.0307(17) 0.0257(13) -0.0041(12) 0.0065(10) 0.0004(11) C24 0.0174(13) 0.044(2) 0.0238(14) -0.0139(14) 0.0053(11) 0.0002(13) C25 0.0291(16) 0.040(2) 0.061(2) -0.0197(19) 0.0227(16) -0.0067(15) C26 0.0209(13) 0.060(3) 0.0207(13) -0.0001(15) 0.0093(11) 0.0057(15) C27 0.0320(17) 0.047(3) 0.066(3) -0.030(2) 0.0176(17) -0.0008(16) C28 0.0222(15) 0.077(3) 0.0229(15) -0.0055(17) 0.0059(12) 0.0073(17) C29 0.0169(12) 0.061(3) 0.0213(13) 0.0063(15) 0.0058(10) 0.0018(14) C30 0.0264(15) 0.048(2) 0.0309(16) -0.0091(15) 0.0130(13) 0.0024(15) C31 0.0163(13) 0.049(2) 0.0204(13) 0.0003(14) 0.0056(10) -0.0010(13) C32 0.0248(14) 0.044(2) 0.0310(16) -0.0069(15) 0.0128(12) -0.0050(14) C33 0.0146(11) 0.046(2) 0.0182(12) -0.0060(13) 0.0034(10) -0.0003(12) C34 0.0162(12) 0.043(2) 0.0194(13) -0.0058(13) 0.0067(10) -0.0018(12) C35 0.0254(14) 0.039(2) 0.0266(15) -0.0024(14) 0.0125(12) -0.0063(13) C36 0.0262(14) 0.040(2) 0.0286(15) -0.0012(14) 0.0123(12) 0.0047(13) C37 0.0254(14) 0.0343(19) 0.0297(15) -0.0037(14) 0.0129(12) -0.0035(13) C38 0.0290(15) 0.045(2) 0.0265(15) 0.0050(14) 0.0138(12) 0.0028(14) C39 0.0199(13) 0.0339(19) 0.0229(14) 0.0018(13) 0.0112(11) 0.0014(12) C40 0.0161(12) 0.0298(17) 0.0185(13) 0.0042(12) 0.0070(10) 0.0035(11) C41 0.0159(12) 0.0254(16) 0.0212(13) 0.0032(11) 0.0065(10) 0.0043(11) C42 0.0151(12) 0.0262(16) 0.0196(12) 0.0061(11) 0.0061(10) 0.0045(11) C43 0.0164(12) 0.0306(18) 0.0245(14) 0.0040(12) 0.0074(10) 0.0024(11) C44 0.0195(12) 0.0302(18) 0.0202(13) 0.0006(12) 0.0068(10) 0.0017(11) C45 0.0192(13) 0.036(2) 0.0273(14) -0.0005(14) 0.0052(11) -0.0048(12) C46 0.0271(14) 0.038(2) 0.0210(13) -0.0033(13) 0.0072(11) -0.0046(13) C47 0.0188(12) 0.0236(16) 0.0249(14) 0.0047(12) 0.0057(11) -0.0003(11) C48 0.0156(12) 0.0261(16) 0.0211(12) -0.0037(11) 0.0044(10) 0.0033(11) C49 0.0157(11) 0.0220(15) 0.0199(13) 0.0033(11) 0.0048(10) 0.0027(10) C50 0.0139(11) 0.0231(15) 0.0216(12) -0.0020(11) 0.0052(9) -0.0040(10) C51 0.0116(11) 0.0246(15) 0.0160(12) 0.0001(11) 0.0020(9) -0.0001(10) C52 0.0122(11) 0.0235(16) 0.0173(12) 0.0020(11) 0.0041(9) 0.0024(10) C53 0.0165(12) 0.0251(16) 0.0246(13) -0.0020(12) 0.0065(10) -0.0021(11) C54 0.0156(12) 0.0273(16) 0.0194(12) -0.0023(11) 0.0050(10) -0.0025(11) C55 0.0225(13) 0.0284(17) 0.0236(14) -0.0030(12) 0.0110(11) 0.0025(12) C56 0.0176(12) 0.0285(17) 0.0295(14) 0.0005(13) 0.0045(11) -0.0065(11) C57 0.0129(11) 0.0167(14) 0.0190(12) 0.0025(10) 0.0020(9) 0.0034(10) C58 0.0146(11) 0.0178(15) 0.0189(12) 0.0003(11) 0.0042(9) 0.0041(10) C59 0.0236(14) 0.0224(17) 0.0418(18) 0.0070(14) 0.0048(13) 0.0006(12) C60 0.0370(17) 0.0276(18) 0.0285(16) 0.0059(14) -0.0013(13) -0.0031(14) C61 0.0212(13) 0.0245(17) 0.0233(14) 0.0082(12) 0.0043(11) 0.0001(11) C62 0.0216(13) 0.0291(18) 0.0229(13) 0.0060(12) 0.0086(10) 0.0036(12) C63 0.0157(12) 0.0173(14) 0.0173(12) 0.0005(10) 0.0028(9) 0.0023(10) C64 0.0131(11) 0.0200(15) 0.0187(12) -0.0008(11) 0.0027(9) -0.0002(10) C65 0.0207(13) 0.037(2) 0.0274(14) 0.0100(14) 0.0050(11) 0.0039(13) C66 0.0184(13) 0.0338(18) 0.0268(14) 0.0124(13) 0.0042(11) -0.0014(12) C67 0.0245(14) 0.0300(18) 0.0270(15) 0.0074(13) 0.0013(11) -0.0013(12) C68 0.0243(14) 0.0207(16) 0.0370(17) 0.0109(13) 0.0043(12) 0.0014(12) O1W 0.0207(10) 0.0287(13) 0.0366(12) 0.0051(10) 0.0150(9) 0.0013(9) O2W 0.0166(9) 0.0231(12) 0.0325(11) 0.0031(9) 0.0107(8) 0.0019(8) O3W 0.067(2) 0.078(3) 0.090(3) 0.016(2) 0.023(2) -0.009(2) O4W 0.0506(16) 0.0413(18) 0.0491(16) -0.0037(13) 0.0012(13) 0.0031(13) O5W 0.082(2) 0.0335(18) 0.121(3) 0.0201(19) 0.079(2) 0.0081(16) O6W 0.0360(12) 0.0335(14) 0.0334(12) 0.0073(10) 0.0059(10) -0.0038(10) O7W 0.022(2) 0.009(2) 0.0082(18) -0.0028(16) 0.0026(15) -0.0022(17) O71W 0.050(4) 0.051(5) 0.068(5) 0.003(4) 0.020(4) 0.011(4) O72W 0.048(7) 0.035(7) 0.030(6) 0.007(5) 0.021(5) 0.016(6) O81W 0.039(3) 0.094(6) 0.081(5) 0.040(4) 0.029(3) 0.012(3) O82W 0.033(3) 0.065(4) 0.068(4) 0.034(4) 0.016(3) 0.004(3) O9W 0.206(7) 0.116(5) 0.256(8) 0.096(6) 0.185(7) 0.090(5) O11W 0.139(4) 0.085(4) 0.101(3) 0.001(3) 0.062(3) 0.010(3) O10W 0.054(4) 0.059(5) 0.091(5) -0.026(4) 0.024(4) 0.002(3) O12W 0.0566(16) 0.0370(16) 0.0466(15) 0.0088(13) 0.0285(13) 0.0038(13) O13W 0.0455(18) 0.070(3) 0.123(4) 0.016(3) -0.010(2) -0.0039(18) O14W 0.0506(18) 0.105(4) 0.073(2) 0.019(2) 0.0248(17) -0.012(2) O15W 0.071(2) 0.058(2) 0.095(3) -0.019(2) 0.040(2) -0.0137(18) _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 Fe1 O10 1.985(2) . ? Fe1 O9 1.987(2) . ? Fe1 O6 1.997(2) . ? Fe1 O5 2.018(2) . ? Fe1 O3 2.036(2) . ? Fe1 O4 2.051(2) . ? Fe2 O18 1.976(2) . ? Fe2 O17 1.982(2) . ? Fe2 O21 1.995(2) . ? Fe2 O22 2.026(2) . ? Fe2 O16 2.030(2) . ? Fe2 O15 2.053(2) . ? Mn1 O1W 2.149(2) . ? Mn1 O1 2.168(2) . ? Mn1 O2W 2.173(2) . ? Mn1 O14 2.174(2) . ? Mn1 O2 2.1951(19) . ? Mn1 O13 2.1965(19) . ? O1 C57 1.248(3) . ? O2 C58 1.242(4) . ? O3 C57 1.260(4) . ? O4 C58 1.263(3) . ? O5 C59 1.288(4) . ? O6 C60 1.298(4) . ? O7 C59 1.231(4) . ? O8 C60 1.216(4) . ? O9 C61 1.296(4) . ? O10 C62 1.286(4) . ? O11 C61 1.221(4) . ? O12 C62 1.226(4) . ? O13 C63 1.233(4) . ? O14 C64 1.240(3) . ? O15 C63 1.269(3) . ? O16 C64 1.262(4) . ? O17 C65 1.291(4) . ? O18 C66 1.302(4) . ? O19 C65 1.233(4) . ? O20 C66 1.215(4) . ? O21 C67 1.300(4) . ? O22 C68 1.290(4) . ? O23 C67 1.214(4) . ? O24 C68 1.219(4) . ? N1 C2 1.340(4) . ? N1 C1 1.344(4) . ? N2 C9 1.356(4) . ? N2 C10 1.357(4) . ? N2 C11 1.454(3) . ? N3 C11 1.299(4) . ? N3 N4 1.365(3) . ? N4 C12 1.304(4) . ? N5 C19 1.334(4) . ? N5 C20 1.351(4) . ? N5 C12 1.452(3) . ? N6 C28 1.315(6) . ? N6 C27 1.341(6) . ? N7 C30 1.316(5) . ? N7 C29 1.338(5) . ? N8 C38 1.337(5) . ? N8 C37 1.353(4) . ? N8 C39 1.458(4) . ? N9 C39 1.303(4) . ? N9 N10 1.366(3) . ? N10 C40 1.299(4) . ? N11 C48 1.343(4) . ? N11 C47 1.365(4) . ? N11 C40 1.454(3) . ? N12 C55 1.333(4) . ? N12 C56 1.341(4) . ? C1 C3 1.378(4) . ? C1 H27A 0.9300 . ? C2 C4 1.391(4) . ? C2 H28A 0.9300 . ? C3 C5 1.393(4) . ? C3 H25A 0.9300 . ? C4 C5 1.388(4) . ? C4 H26A 0.9300 . ? C5 C6 1.483(3) . ? C6 C7 1.399(4) . ? C6 C8 1.404(4) . ? C7 C9 1.373(4) . ? C7 H21A 0.9300 . ? C8 C10 1.379(4) . ? C8 H22A 0.9300 . ? C9 H19A 0.9300 . ? C10 H20A 0.9300 . ? C11 C13 1.421(4) . ? C12 C14 1.416(4) . ? C13 C15 1.404(4) . ? C13 C14 1.423(4) . ? C14 C16 1.407(4) . ? C15 C17 1.372(4) . ? C15 H16A 0.9300 . ? C16 C18 1.377(4) . ? C16 H15A 0.9300 . ? C17 C18 1.402(4) . ? C17 H18A 0.9300 . ? C18 H17A 0.9300 . ? C19 C21 1.380(4) . ? C19 H9A 0.9300 . ? C20 C22 1.376(4) . ? C20 H10A 0.9300 . ? C21 C23 1.400(5) . ? C21 H7A 0.9300 . ? C22 C23 1.384(5) . ? C22 H8A 0.9300 . ? C23 C24 1.492(4) . ? C24 C26 1.388(5) . ? C24 C25 1.390(6) . ? C25 C27 1.391(5) . ? C25 H3A 0.9300 . ? C26 C28 1.399(4) . ? C26 H4A 0.9300 . ? C27 H1A 0.9300 . ? C28 H2A 0.9300 . ? C29 C31 1.388(4) . ? C29 H29A 0.9300 . ? C30 C32 1.410(4) . ? C30 H30A 0.9300 . ? C31 C33 1.394(5) . ? C31 H31A 0.9300 . ? C32 C33 1.369(5) . ? C32 H32A 0.9300 . ? C33 C34 1.492(4) . ? C34 C35 1.377(5) . ? C34 C36 1.397(5) . ? C35 C37 1.387(4) . ? C35 H35A 0.9300 . ? C36 C38 1.376(4) . ? C36 H36A 0.9300 . ? C37 H37A 0.9300 . ? C38 H38A 0.9300 . ? C39 C41 1.404(5) . ? C40 C42 1.410(4) . ? C41 C43 1.404(4) . ? C41 C42 1.424(4) . ? C42 C44 1.406(4) . ? C43 C45 1.369(5) . ? C43 H44A 0.9300 . ? C44 C46 1.363(4) . ? C44 H43A 0.9300 . ? C45 C46 1.410(4) . ? C45 H45A 0.9300 . ? C46 H46A 0.9300 . ? C47 C49 1.378(4) . ? C47 H47A 0.9300 . ? C48 C50 1.387(4) . ? C48 H48A 0.9300 . ? C49 C51 1.394(4) . ? C49 H49A 0.9300 . ? C50 C51 1.393(4) . ? C50 H50A 0.9300 . ? C51 C52 1.483(3) . ? C52 C54 1.389(4) . ? C52 C53 1.397(4) . ? C53 C55 1.386(4) . ? C53 H53A 0.9300 . ? C54 C56 1.382(4) . ? C54 H54A 0.9300 . ? C55 H55A 0.9300 . ? C56 H56A 0.9300 . ? C57 C58 1.554(4) . ? C59 C60 1.549(5) . ? C61 C62 1.550(5) . ? C63 C64 1.563(4) . ? C65 C66 1.558(5) . ? C67 C68 1.543(5) . ? O1W H2 0.9648 . ? O1W H1 0.7140 . ? O2W H4 0.9178 . ? O2W H3 0.8792 . ? O4W H8 0.9301 . ? O4W H7 0.8866 . ? O6W H12 0.8513 . ? O6W H11 0.8846 . ? O7W O72W 1.681(14) . ? O71W O72W 1.234(16) . ? O81W O82W 1.699(12) . ? O12W H23 0.7388 . ? O12W H24 0.8713 . ? 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 O10 Fe1 O9 81.18(9) . . ? O10 Fe1 O6 93.63(9) . . ? O9 Fe1 O6 102.79(9) . . ? O10 Fe1 O5 173.73(9) . . ? O9 Fe1 O5 97.56(9) . . ? O6 Fe1 O5 80.63(9) . . ? O10 Fe1 O3 98.11(9) . . ? O9 Fe1 O3 88.62(8) . . ? O6 Fe1 O3 164.78(8) . . ? O5 Fe1 O3 87.98(9) . . ? O10 Fe1 O4 92.84(9) . . ? O9 Fe1 O4 166.47(9) . . ? O6 Fe1 O4 89.63(9) . . ? O5 Fe1 O4 89.65(9) . . ? O3 Fe1 O4 80.18(8) . . ? O18 Fe2 O17 82.41(10) . . ? O18 Fe2 O21 99.04(10) . . ? O17 Fe2 O21 90.34(9) . . ? O18 Fe2 O22 99.85(10) . . ? O17 Fe2 O22 170.82(9) . . ? O21 Fe2 O22 80.52(9) . . ? O18 Fe2 O16 89.36(9) . . ? O17 Fe2 O16 101.54(9) . . ? O21 Fe2 O16 166.31(8) . . ? O22 Fe2 O16 87.42(9) . . ? O18 Fe2 O15 166.64(9) . . ? O17 Fe2 O15 91.23(9) . . ? O21 Fe2 O15 92.71(9) . . ? O22 Fe2 O15 88.29(9) . . ? O16 Fe2 O15 80.38(8) . . ? O1W Mn1 O1 89.17(9) . . ? O1W Mn1 O2W 178.89(9) . . ? O1 Mn1 O2W 91.56(8) . . ? O1W Mn1 O14 91.79(9) . . ? O1 Mn1 O14 179.03(9) . . ? O2W Mn1 O14 87.47(9) . . ? O1W Mn1 O2 85.47(8) . . ? O1 Mn1 O2 77.16(7) . . ? O2W Mn1 O2 95.50(8) . . ? O14 Mn1 O2 102.99(8) . . ? O1W Mn1 O13 92.39(8) . . ? O1 Mn1 O13 102.63(8) . . ? O2W Mn1 O13 86.64(8) . . ? O14 Mn1 O13 77.26(8) . . ? O2 Mn1 O13 177.85(9) . . ? C57 O1 Mn1 113.76(18) . . ? C58 O2 Mn1 112.95(17) . . ? C57 O3 Fe1 113.86(18) . . ? C58 O4 Fe1 113.43(18) . . ? C59 O5 Fe1 114.3(2) . . ? C60 O6 Fe1 114.9(2) . . ? C61 O9 Fe1 115.7(2) . . ? C62 O10 Fe1 115.9(2) . . ? C63 O13 Mn1 113.20(18) . . ? C64 O14 Mn1 113.22(18) . . ? C63 O15 Fe2 113.16(19) . . ? C64 O16 Fe2 114.21(18) . . ? C65 O17 Fe2 114.6(2) . . ? C66 O18 Fe2 115.0(2) . . ? C67 O21 Fe2 115.7(2) . . ? C68 O22 Fe2 114.3(2) . . ? C2 N1 C1 116.7(2) . . ? C9 N2 C10 121.3(2) . . ? C9 N2 C11 116.6(2) . . ? C10 N2 C11 121.9(3) . . ? C11 N3 N4 119.2(2) . . ? C12 N4 N3 117.7(3) . . ? C19 N5 C20 121.2(3) . . ? C19 N5 C12 118.5(3) . . ? C20 N5 C12 120.3(3) . . ? C28 N6 C27 116.8(3) . . ? C30 N7 C29 116.8(3) . . ? C38 N8 C37 122.1(3) . . ? C38 N8 C39 118.0(3) . . ? C37 N8 C39 119.8(3) . . ? C39 N9 N10 117.3(3) . . ? C40 N10 N9 118.5(3) . . ? C48 N11 C47 122.0(2) . . ? C48 N11 C40 117.5(3) . . ? C47 N11 C40 120.4(3) . . ? C55 N12 C56 117.6(2) . . ? N1 C1 C3 124.4(3) . . ? N1 C1 H27A 117.8 . . ? C3 C1 H27A 117.8 . . ? N1 C2 C4 123.1(3) . . ? N1 C2 H28A 118.4 . . ? C4 C2 H28A 118.4 . . ? C1 C3 C5 118.4(3) . . ? C1 C3 H25A 120.8 . . ? C5 C3 H25A 120.8 . . ? C5 C4 C2 119.2(3) . . ? C5 C4 H26A 120.4 . . ? C2 C4 H26A 120.4 . . ? C4 C5 C3 118.2(2) . . ? C4 C5 C6 121.6(3) . . ? C3 C5 C6 120.2(3) . . ? C7 C6 C8 118.4(2) . . ? C7 C6 C5 119.8(3) . . ? C8 C6 C5 121.8(3) . . ? C9 C7 C6 120.2(3) . . ? C9 C7 H21A 119.9 . . ? C6 C7 H21A 119.9 . . ? C10 C8 C6 119.7(3) . . ? C10 C8 H22A 120.2 . . ? C6 C8 H22A 120.2 . . ? N2 C9 C7 120.1(3) . . ? N2 C9 H19A 119.9 . . ? C7 C9 H19A 119.9 . . ? N2 C10 C8 120.3(3) . . ? N2 C10 H20A 119.9 . . ? C8 C10 H20A 119.9 . . ? N3 C11 C13 126.9(3) . . ? N3 C11 N2 111.5(2) . . ? C13 C11 N2 121.4(3) . . ? N4 C12 C14 127.0(3) . . ? N4 C12 N5 112.3(3) . . ? C14 C12 N5 120.7(2) . . ? C15 C13 C11 125.8(2) . . ? C15 C13 C14 120.0(3) . . ? C11 C13 C14 113.9(3) . . ? C16 C14 C12 124.7(3) . . ? C16 C14 C13 119.8(3) . . ? C12 C14 C13 115.3(2) . . ? C17 C15 C13 118.9(3) . . ? C17 C15 H16A 120.6 . . ? C13 C15 H16A 120.6 . . ? C18 C16 C14 119.0(3) . . ? C18 C16 H15A 120.5 . . ? C14 C16 H15A 120.5 . . ? C15 C17 C18 121.5(3) . . ? C15 C17 H18A 119.3 . . ? C18 C17 H18A 119.3 . . ? C16 C18 C17 120.8(3) . . ? C16 C18 H17A 119.6 . . ? C17 C18 H17A 119.6 . . ? N5 C19 C21 120.4(3) . . ? N5 C19 H9A 119.8 . . ? C21 C19 H9A 119.8 . . ? N5 C20 C22 120.0(3) . . ? N5 C20 H10A 120.0 . . ? C22 C20 H10A 120.0 . . ? C19 C21 C23 120.3(3) . . ? C19 C21 H7A 119.8 . . ? C23 C21 H7A 119.8 . . ? C20 C22 C23 120.9(3) . . ? C20 C22 H8A 119.5 . . ? C23 C22 H8A 119.5 . . ? C22 C23 C21 117.2(3) . . ? C22 C23 C24 121.2(3) . . ? C21 C23 C24 121.6(3) . . ? C26 C24 C25 117.9(3) . . ? C26 C24 C23 120.8(3) . . ? C25 C24 C23 121.3(3) . . ? C24 C25 C27 119.2(4) . . ? C24 C25 H3A 120.4 . . ? C27 C25 H3A 120.4 . . ? C24 C26 C28 118.2(4) . . ? C24 C26 H4A 120.9 . . ? C28 C26 H4A 120.9 . . ? N6 C27 C25 123.3(4) . . ? N6 C27 H1A 118.3 . . ? C25 C27 H1A 118.3 . . ? N6 C28 C26 124.7(4) . . ? N6 C28 H2A 117.7 . . ? C26 C28 H2A 117.7 . . ? N7 C29 C31 123.9(3) . . ? N7 C29 H29A 118.0 . . ? C31 C29 H29A 118.0 . . ? N7 C30 C32 123.6(4) . . ? N7 C30 H30A 118.2 . . ? C32 C30 H30A 118.2 . . ? C29 C31 C33 118.7(4) . . ? C29 C31 H31A 120.7 . . ? C33 C31 H31A 120.7 . . ? C33 C32 C30 119.1(3) . . ? C33 C32 H32A 120.4 . . ? C30 C32 H32A 120.4 . . ? C32 C33 C31 117.8(3) . . ? C32 C33 C34 120.5(3) . . ? C31 C33 C34 121.7(3) . . ? C35 C34 C36 118.4(3) . . ? C35 C34 C33 122.0(3) . . ? C36 C34 C33 119.6(3) . . ? C34 C35 C37 120.5(3) . . ? C34 C35 H35A 119.7 . . ? C37 C35 H35A 119.7 . . ? C38 C36 C34 119.9(3) . . ? C38 C36 H36A 120.1 . . ? C34 C36 H36A 120.1 . . ? N8 C37 C35 119.0(3) . . ? N8 C37 H37A 120.5 . . ? C35 C37 H37A 120.5 . . ? N8 C38 C36 120.1(3) . . ? N8 C38 H38A 120.0 . . ? C36 C38 H38A 120.0 . . ? N9 C39 C41 128.1(3) . . ? N9 C39 N8 111.8(3) . . ? C41 C39 N8 120.0(3) . . ? N10 C40 C42 127.5(3) . . ? N10 C40 N11 111.2(3) . . ? C42 C40 N11 121.2(3) . . ? C39 C41 C43 125.1(3) . . ? C39 C41 C42 114.4(3) . . ? C43 C41 C42 120.4(3) . . ? C44 C42 C40 126.2(2) . . ? C44 C42 C41 119.4(3) . . ? C40 C42 C41 114.2(3) . . ? C45 C43 C41 118.7(3) . . ? C45 C43 H44A 120.7 . . ? C41 C43 H44A 120.7 . . ? C46 C44 C42 119.2(3) . . ? C46 C44 H43A 120.4 . . ? C42 C44 H43A 120.4 . . ? C43 C45 C46 121.0(3) . . ? C43 C45 H45A 119.5 . . ? C46 C45 H45A 119.5 . . ? C44 C46 C45 121.4(3) . . ? C44 C46 H46A 119.3 . . ? C45 C46 H46A 119.3 . . ? N11 C47 C49 119.2(3) . . ? N11 C47 H47A 120.4 . . ? C49 C47 H47A 120.4 . . ? N11 C48 C50 120.2(3) . . ? N11 C48 H48A 119.9 . . ? C50 C48 H48A 119.9 . . ? C47 C49 C51 120.1(3) . . ? C47 C49 H49A 120.0 . . ? C51 C49 H49A 120.0 . . ? C48 C50 C51 119.2(3) . . ? C48 C50 H50A 120.4 . . ? C51 C50 H50A 120.4 . . ? C50 C51 C49 119.2(2) . . ? C50 C51 C52 119.5(3) . . ? C49 C51 C52 121.2(3) . . ? C54 C52 C53 117.6(2) . . ? C54 C52 C51 120.5(3) . . ? C53 C52 C51 121.9(3) . . ? C55 C53 C52 119.3(3) . . ? C55 C53 H53A 120.4 . . ? C52 C53 H53A 120.4 . . ? C56 C54 C52 119.2(3) . . ? C56 C54 H54A 120.4 . . ? C52 C54 H54A 120.4 . . ? N12 C55 C53 123.0(3) . . ? N12 C55 H55A 118.5 . . ? C53 C55 H55A 118.5 . . ? N12 C56 C54 123.3(3) . . ? N12 C56 H56A 118.4 . . ? C54 C56 H56A 118.4 . . ? O1 C57 O3 126.7(3) . . ? O1 C57 C58 117.7(2) . . ? O3 C57 C58 115.5(2) . . ? O2 C58 O4 126.8(3) . . ? O2 C58 C57 118.1(2) . . ? O4 C58 C57 115.1(2) . . ? O7 C59 O5 126.1(3) . . ? O7 C59 C60 119.9(3) . . ? O5 C59 C60 114.0(3) . . ? O8 C60 O6 125.8(4) . . ? O8 C60 C59 120.4(3) . . ? O6 C60 C59 113.8(3) . . ? O11 C61 O9 125.5(3) . . ? O11 C61 C62 121.1(3) . . ? O9 C61 C62 113.4(3) . . ? O12 C62 O10 125.7(3) . . ? O12 C62 C61 120.4(3) . . ? O10 C62 C61 113.9(2) . . ? O13 C63 O15 127.4(3) . . ? O13 C63 C64 117.7(2) . . ? O15 C63 C64 114.9(2) . . ? O14 C64 O16 126.4(3) . . ? O14 C64 C63 118.4(2) . . ? O16 C64 C63 115.2(2) . . ? O19 C65 O17 124.4(4) . . ? O19 C65 C66 121.3(3) . . ? O17 C65 C66 114.3(3) . . ? O20 C66 O18 124.7(4) . . ? O20 C66 C65 121.9(3) . . ? O18 C66 C65 113.4(3) . . ? O23 C67 O21 124.9(3) . . ? O23 C67 C68 121.5(3) . . ? O21 C67 C68 113.5(3) . . ? O24 C68 O22 125.5(3) . . ? O24 C68 C67 120.9(3) . . ? O22 C68 C67 113.6(3) . . ? H2 O1W H1 110.0 . . ? H4 O2W H3 103.7 . . ? H8 O4W H7 115.2 . . ? H12 O6W H11 98.0 . . ? H23 O12W H24 94.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H2 N12 0.96 1.83 2.780(3) 169.6 2_856 O1W H1 O12W 0.71 2.04 2.748(4) 169.2 . O2W H4 N1 0.92 1.89 2.806(3) 175.2 2_557 O2W H3 O5W 0.88 1.89 2.754(4) 167.6 . O4W H8 O18 0.93 2.05 2.971(4) 170.8 . O4W H7 O7 0.89 2.10 2.910(4) 152.3 2_757 O6W H12 O9 0.85 2.05 2.884(3) 168.3 2_656 O6W H11 O23 0.88 1.92 2.789(4) 167.6 . O12W H23 O13W 0.74 2.27 2.812(5) 131.1 1_655 O12W H24 O5 0.87 2.01 2.846(3) 159.5 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.092 _refine_diff_density_min -0.560 _refine_diff_density_rms 0.069 data_s_2 _database_code_depnum_ccdc_archive 'CCDC 265931' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H69 Co Fe2 N12 O38.50' _chemical_formula_weight 1840.98 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' Fe Fe 0.3463 0.8444 '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 monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.9844(5) _cell_length_b 20.3785(7) _cell_length_c 15.8706(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.328(2) _cell_angle_gamma 90.00 _cell_volume 3824.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8260 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour Brown _exptl_crystal_size_max 0.4000 _exptl_crystal_size_mid 0.3500 _exptl_crystal_size_min 0.3000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 0.696 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.757 _exptl_absorpt_correction_T_max 0.812 _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 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29872 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.48 _reflns_number_total 17275 _reflns_number_gt 15213 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0695P)^2^+1.4361P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.033(11) _refine_ls_number_reflns 17275 _refine_ls_number_parameters 1122 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1263 _refine_ls_wR_factor_gt 0.1201 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.49123(4) 0.71976(2) 0.96447(3) 0.01941(11) Uani 1 1 d . . . Fe2 Fe 0.92553(4) 1.03603(2) 0.57923(3) 0.02128(11) Uani 1 1 d . . . Co1 Co 0.70537(4) 0.87960(3) 0.77187(3) 0.01780(9) Uani 1 1 d . . . O1 O 0.5852(2) 0.80387(12) 0.75794(15) 0.0192(5) Uani 1 1 d . . . O2 O 0.67857(19) 0.86983(12) 0.89973(14) 0.0200(5) Uani 1 1 d . . . O3 O 0.4917(2) 0.74090(12) 0.83878(15) 0.0221(5) Uani 1 1 d . . . O4 O 0.5812(2) 0.80598(12) 0.97702(15) 0.0222(5) Uani 1 1 d . . . O5 O 0.6362(2) 0.66944(14) 0.96453(18) 0.0290(6) Uani 1 1 d . . . O6 O 0.5335(2) 0.70342(13) 1.09051(17) 0.0287(6) Uani 1 1 d . . . O7 O 0.7961(3) 0.64380(19) 1.0525(3) 0.0534(9) Uani 1 1 d . . . O8 O 0.6816(4) 0.6751(2) 1.1871(2) 0.0679(12) Uani 1 1 d . . . O9 O 0.3843(2) 0.64656(12) 0.92808(16) 0.0226(5) Uani 1 1 d . . . O10 O 0.3478(2) 0.76420(13) 0.97863(18) 0.0274(6) Uani 1 1 d . . . O11 O 0.2002(2) 0.62040(15) 0.9109(2) 0.0365(7) Uani 1 1 d . . . O12 O 0.1613(3) 0.74860(16) 0.9632(2) 0.0403(7) Uani 1 1 d . . . O13 O 0.7356(2) 0.88738(12) 0.64491(15) 0.0218(5) Uani 1 1 d . . . O14 O 0.8236(2) 0.95661(12) 0.78575(15) 0.0202(5) Uani 1 1 d . . . O15 O 0.8391(2) 0.94805(12) 0.56824(16) 0.0231(5) Uani 1 1 d . . . O16 O 0.9182(2) 1.01824(13) 0.70462(16) 0.0240(5) Uani 1 1 d . . . O17 O 1.0689(2) 0.99139(14) 0.56553(18) 0.0301(6) Uani 1 1 d . . . O18 O 1.0283(2) 1.11090(14) 0.61277(18) 0.0320(6) Uani 1 1 d . . . O19 O 1.2516(3) 1.01097(19) 0.5625(2) 0.0503(9) Uani 1 1 d . . . O20 O 1.2111(3) 1.13877(18) 0.6248(2) 0.0457(8) Uani 1 1 d . . . O21 O 0.8930(2) 1.05226(14) 0.45371(16) 0.0303(6) Uani 1 1 d . . . O22 O 0.7744(2) 1.08224(14) 0.57123(19) 0.0305(6) Uani 1 1 d . . . O23 O 0.7684(3) 1.1007(2) 0.3530(2) 0.0497(9) Uani 1 1 d . . . O24 O 0.6216(3) 1.10307(18) 0.4745(2) 0.0502(9) Uani 1 1 d . . . N1 N -0.3646(3) 0.45304(17) 1.2098(2) 0.0235(7) Uani 1 1 d . . . N2 N 0.1135(2) 0.45577(15) 1.00350(18) 0.0195(6) Uani 1 1 d . . . N3 N 0.1812(3) 0.41290(17) 0.88924(19) 0.0262(7) Uani 1 1 d . . . N4 N 0.2618(3) 0.39888(17) 0.8407(2) 0.0276(7) Uani 1 1 d . . . N5 N 0.4421(3) 0.40224(16) 0.8096(2) 0.0226(6) Uani 1 1 d . . . N6 N 0.8451(3) 0.2936(2) 0.5627(2) 0.0437(10) Uani 1 1 d . . . N7 N 0.7481(3) 0.4309(2) 0.9032(2) 0.0421(10) Uani 1 1 d . . . N8 N 1.1412(3) 0.33608(18) 0.6418(2) 0.0311(8) Uani 1 1 d . . . N9 N 1.3173(3) 0.3512(2) 0.6075(2) 0.0380(9) Uani 1 1 d . . . N10 N 1.3988(3) 0.3421(2) 0.5570(2) 0.0337(8) Uani 1 1 d . . . N11 N 1.4717(3) 0.29924(16) 0.44561(19) 0.0208(6) Uani 1 1 d . . . N12 N 1.9606(3) 0.30729(16) 0.2544(2) 0.0244(7) Uani 1 1 d . . . C1 C -0.3408(3) 0.40487(18) 1.1574(2) 0.0218(7) Uani 1 1 d . . . H27A H -0.3901 0.3694 1.1485 0.026 Uiso 1 1 calc R . . C2 C -0.2914(3) 0.50293(18) 1.2221(2) 0.0233(7) Uani 1 1 d . . . H28A H -0.3055 0.5369 1.2580 0.028 Uiso 1 1 calc R . . C3 C -0.2483(3) 0.40463(18) 1.1160(2) 0.0210(7) Uani 1 1 d . . . H25A H -0.2367 0.3703 1.0797 0.025 Uiso 1 1 calc R . . C4 C -0.1946(3) 0.50649(18) 1.1836(2) 0.0203(7) Uani 1 1 d . . . H26A H -0.1454 0.5419 1.1943 0.024 Uiso 1 1 calc R . . C5 C -0.1727(3) 0.45661(17) 1.1295(2) 0.0175(6) Uani 1 1 d . . . C6 C -0.0718(3) 0.45708(19) 1.0863(2) 0.0182(7) Uani 1 1 d . . . C7 C -0.0234(3) 0.39820(17) 1.0662(2) 0.0192(7) Uani 1 1 d . . . H21A H -0.0539 0.3586 1.0807 0.023 Uiso 1 1 calc R . . C8 C -0.0224(3) 0.51630(17) 1.0635(2) 0.0205(7) Uani 1 1 d . . . H22A H -0.0527 0.5565 1.0761 0.025 Uiso 1 1 calc R . . C9 C 0.0687(3) 0.39798(17) 1.0251(2) 0.0198(7) Uani 1 1 d . . . H19A H 0.1006 0.3584 1.0120 0.024 Uiso 1 1 calc R . . C10 C 0.0697(3) 0.51429(18) 1.0229(2) 0.0227(7) Uani 1 1 d . . . H20A H 0.1026 0.5532 1.0084 0.027 Uiso 1 1 calc R . . C11 C 0.2070(3) 0.4513(2) 0.9553(2) 0.0217(7) Uani 1 1 d . . . C12 C 0.3619(3) 0.42448(18) 0.8634(2) 0.0226(7) Uani 1 1 d . . . C13 C 0.3121(3) 0.48221(17) 0.9836(2) 0.0197(7) Uani 1 1 d . . . C14 C 0.3968(3) 0.46627(17) 0.9340(2) 0.0207(7) Uani 1 1 d . . . C15 C 0.3394(3) 0.52031(18) 1.0571(2) 0.0220(7) Uani 1 1 d . . . H16A H 0.2844 0.5309 1.0899 0.026 Uiso 1 1 calc R . . C16 C 0.5084(3) 0.48804(18) 0.9597(2) 0.0246(7) Uani 1 1 d . . . H15A H 0.5648 0.4766 0.9285 0.030 Uiso 1 1 calc R . . C17 C 0.4479(3) 0.54181(18) 1.0802(2) 0.0237(7) Uani 1 1 d . . . H18A H 0.4661 0.5672 1.1292 0.028 Uiso 1 1 calc R . . C18 C 0.5334(3) 0.52645(18) 1.0316(2) 0.0239(7) Uani 1 1 d . . . H17A H 0.6065 0.5423 1.0482 0.029 Uiso 1 1 calc R . . C19 C 0.4632(4) 0.3380(2) 0.8066(3) 0.0365(10) Uani 1 1 d . . . H9A H 0.4286 0.3088 0.8392 0.044 Uiso 1 1 calc R . . C20 C 0.4913(3) 0.44549(19) 0.7636(2) 0.0270(8) Uani 1 1 d . . . H10A H 0.4748 0.4900 0.7664 0.032 Uiso 1 1 calc R . . C21 C 0.5370(4) 0.3151(2) 0.7543(3) 0.0386(10) Uani 1 1 d . . . H7A H 0.5505 0.2703 0.7514 0.046 Uiso 1 1 calc R . . C22 C 0.5664(4) 0.4241(2) 0.7119(3) 0.0294(9) Uani 1 1 d . . . H8A H 0.6008 0.4545 0.6806 0.035 Uiso 1 1 calc R . . C23 C 0.5910(3) 0.35812(19) 0.7064(2) 0.0265(8) Uani 1 1 d . . . C24 C 0.6754(3) 0.3347(2) 0.6541(2) 0.0293(9) Uani 1 1 d . . . C25 C 0.7094(4) 0.2702(2) 0.6552(3) 0.0446(12) Uani 1 1 d . . . H3A H 0.6762 0.2391 0.6861 0.054 Uiso 1 1 calc R . . C26 C 0.7259(3) 0.3782(3) 0.6041(2) 0.0364(9) Uani 1 1 d . . . H4A H 0.7042 0.4221 0.6002 0.044 Uiso 1 1 calc R . . C27 C 0.7952(4) 0.2520(3) 0.6088(4) 0.0506(13) Uani 1 1 d . . . H1A H 0.8180 0.2084 0.6106 0.061 Uiso 1 1 calc R . . C28 C 0.8096(4) 0.3551(3) 0.5600(3) 0.0455(13) Uani 1 1 d . . . H2A H 0.8423 0.3847 0.5267 0.055 Uiso 1 1 calc R . . C29 C 0.7707(3) 0.3685(3) 0.8914(3) 0.0422(12) Uani 1 1 d . . . H29A H 0.7299 0.3372 0.9165 0.051 Uiso 1 1 calc R . . C30 C 0.8082(4) 0.4740(3) 0.8678(3) 0.0433(11) Uani 1 1 d . . . H30A H 0.7947 0.5183 0.8756 0.052 Uiso 1 1 calc R . . C31 C 0.8506(3) 0.3463(3) 0.8444(2) 0.0356(10) Uani 1 1 d . . . H31A H 0.8636 0.3016 0.8390 0.043 Uiso 1 1 calc R . . C32 C 0.8910(4) 0.4568(3) 0.8193(3) 0.0407(11) Uani 1 1 d . . . H32A H 0.9322 0.4891 0.7967 0.049 Uiso 1 1 calc R . . C33 C 0.9109(3) 0.3920(2) 0.8054(2) 0.0329(10) Uani 1 1 d . . . C34 C 0.9943(3) 0.3715(2) 0.7495(2) 0.0310(9) Uani 1 1 d . . . C35 C 1.0408(4) 0.3109(2) 0.7529(3) 0.0377(10) Uani 1 1 d . . . H35A H 1.0227 0.2810 0.7928 0.045 Uiso 1 1 calc R . . C36 C 1.0244(3) 0.4158(2) 0.6902(3) 0.0371(10) Uani 1 1 d . . . H36A H 0.9939 0.4579 0.6862 0.045 Uiso 1 1 calc R . . C37 C 1.1141(3) 0.2923(2) 0.6989(3) 0.0350(9) Uani 1 1 d . . . H37A H 1.1444 0.2502 0.7017 0.042 Uiso 1 1 calc R . . C38 C 1.1001(4) 0.3969(2) 0.6370(3) 0.0377(10) Uani 1 1 d . . . H38A H 1.1220 0.4266 0.5982 0.045 Uiso 1 1 calc R . . C39 C 1.2224(3) 0.3192(2) 0.5864(3) 0.0290(9) Uani 1 1 d . . . C40 C 1.3783(3) 0.3017(2) 0.4937(2) 0.0231(7) Uani 1 1 d . . . C41 C 1.1906(3) 0.27608(19) 0.5174(2) 0.0239(7) Uani 1 1 d . . . C42 C 1.2769(3) 0.26621(19) 0.4660(2) 0.0241(8) Uani 1 1 d . . . C43 C 1.0850(3) 0.2465(2) 0.4948(2) 0.0265(8) Uani 1 1 d . . . H44A H 1.0284 0.2531 0.5277 0.032 Uiso 1 1 calc R . . C44 C 1.2541(3) 0.2273(2) 0.3922(2) 0.0270(8) Uani 1 1 d . . . H43A H 1.3081 0.2218 0.3568 0.032 Uiso 1 1 calc R . . C45 C 1.0662(3) 0.2078(2) 0.4243(2) 0.0304(9) Uani 1 1 d . . . H45A H 0.9961 0.1877 0.4092 0.037 Uiso 1 1 calc R . . C46 C 1.1505(3) 0.1977(2) 0.3736(3) 0.0321(9) Uani 1 1 d . . . H46A H 1.1355 0.1702 0.3264 0.039 Uiso 1 1 calc R . . C47 C 1.5192(3) 0.24158(18) 0.4286(2) 0.0224(7) Uani 1 1 d . . . H47A H 1.4892 0.2022 0.4444 0.027 Uiso 1 1 calc R . . C48 C 1.5137(3) 0.35739(18) 0.4245(2) 0.0226(7) Uani 1 1 d . . . H48A H 1.4789 0.3963 0.4364 0.027 Uiso 1 1 calc R . . C49 C 1.6126(3) 0.24131(18) 0.3877(2) 0.0210(7) Uani 1 1 d . . . H49A H 1.6441 0.2017 0.3743 0.025 Uiso 1 1 calc R . . C50 C 1.6089(3) 0.35907(18) 0.3851(2) 0.0219(7) Uani 1 1 d . . . H50A H 1.6386 0.3991 0.3712 0.026 Uiso 1 1 calc R . . C51 C 1.6595(3) 0.30050(19) 0.3664(2) 0.0198(7) Uani 1 1 d . . . C52 C 1.7626(3) 0.30208(18) 0.3266(2) 0.0188(7) Uani 1 1 d . . . C53 C 1.7921(3) 0.25089(19) 0.2758(2) 0.0249(7) Uani 1 1 d . . . H53A H 1.7459 0.2142 0.2651 0.030 Uiso 1 1 calc R . . C54 C 1.8354(3) 0.35592(18) 0.3396(2) 0.0209(7) Uani 1 1 d . . . H54A H 1.8189 0.3913 0.3724 0.025 Uiso 1 1 calc R . . C55 C 1.8911(3) 0.25559(19) 0.2416(2) 0.0257(8) Uani 1 1 d . . . H55A H 1.9101 0.2212 0.2081 0.031 Uiso 1 1 calc R . . C56 C 1.9330(3) 0.35588(19) 0.3027(2) 0.0266(8) Uani 1 1 d . . . H56A H 1.9813 0.3918 0.3123 0.032 Uiso 1 1 calc R . . C57 C 0.5595(3) 0.78599(16) 0.8275(2) 0.0165(6) Uani 1 1 d . . . C58 C 0.6119(3) 0.82449(16) 0.9079(2) 0.0189(7) Uani 1 1 d . . . C59 C 0.6974(4) 0.6628(2) 1.0381(3) 0.0343(9) Uani 1 1 d . . . C60 C 0.6370(4) 0.6815(2) 1.1139(3) 0.0363(9) Uani 1 1 d . . . C61 C 0.2790(3) 0.65897(19) 0.9308(2) 0.0256(8) Uani 1 1 d . . . C62 C 0.2574(3) 0.72982(19) 0.9602(2) 0.0267(8) Uani 1 1 d . . . C63 C 0.8025(3) 0.93184(17) 0.6357(2) 0.0186(7) Uani 1 1 d . . . C64 C 0.8518(3) 0.97269(17) 0.7170(2) 0.0189(7) Uani 1 1 d . . . C65 C 1.1564(3) 1.0283(2) 0.5736(3) 0.0339(9) Uani 1 1 d . . . C66 C 1.1341(3) 1.0992(2) 0.6058(3) 0.0329(9) Uani 1 1 d . . . C67 C 0.7977(3) 1.0809(2) 0.4266(3) 0.0313(9) Uani 1 1 d . . . C68 C 0.7215(3) 1.0902(2) 0.4946(3) 0.0312(9) Uani 1 1 d . . . O1W O 0.8305(2) 0.81055(13) 0.80031(18) 0.0258(6) Uani 1 1 d . . . H2 H 0.9024 0.8044 0.7816 0.080 Uiso 1 1 d R . . H1 H 0.8103 0.7801 0.8138 0.080 Uiso 1 1 d R . . O2W O 0.5797(2) 0.94948(13) 0.74179(17) 0.0235(5) Uani 1 1 d . . . H4 H 0.5094 0.9522 0.7574 0.080 Uiso 1 1 d R . . H3 H 0.5892 0.9883 0.7201 0.080 Uiso 1 1 d R . . O3W O -0.0453(5) 0.7488(3) 1.0262(4) 0.110(2) Uani 1 1 d . . . O4W O 1.0443(3) 1.15743(19) 0.7902(3) 0.0595(10) Uani 1 1 d . . . H8 H 1.0473 1.1465 0.7340 0.080 Uiso 1 1 d R . . H7 H 1.1094 1.1543 0.8255 0.080 Uiso 1 1 d R . . O5W O 0.6256(4) 1.07579(17) 0.6954(3) 0.0711(14) Uani 1 1 d . . . O6W O 0.5760(3) 1.08957(15) 0.2304(2) 0.0406(7) Uani 1 1 d . . . H12 H 0.5952 1.1021 0.1838 0.080 Uiso 1 1 d R . . H11 H 0.6423 1.0945 0.2633 0.080 Uiso 1 1 d R . . O7W O 0.7174(7) 0.5441(3) 0.6311(4) 0.0353(16) Uani 0.40 1 d P . . O71W O 0.5477(18) 0.5146(11) 0.4918(14) 0.063(5) Uani 0.20 1 d P . . O72W O 0.6007(8) 0.5426(5) 0.5597(6) 0.056(2) Uani 0.40 1 d P . . O8W O 1.4077(7) 1.1098(6) 0.5306(6) 0.082(3) Uani 0.50 1 d P . . O8W' O 1.4385(7) 1.1697(5) 0.5975(7) 0.079(3) Uani 0.50 1 d P . . O9W O 0.8519(8) 1.1494(4) 0.8689(7) 0.219(6) Uani 1 1 d . . . O11W O 0.6510(7) 1.1677(3) 0.8113(5) 0.129(3) Uani 1 1 d . . . O10W O 0.4652(8) 1.1643(4) 0.6968(6) 0.077(3) Uani 0.50 1 d P . . O12W O 0.7774(3) 0.68441(16) 0.8388(2) 0.0485(9) Uani 1 1 d . . . H23 H 0.8361 0.6790 0.8601 0.080 Uiso 1 1 d R . . H24 H 0.7490 0.6804 0.8855 0.080 Uiso 1 1 d R . . O13W O -0.0235(5) 0.6138(3) 0.8373(7) 0.178(5) Uani 1 1 d . . . O14W O 0.9502(6) 0.5595(4) 0.6652(5) 0.126(2) Uiso 1 1 d . . . O15W O 0.6275(4) 0.6224(4) 0.7198(3) 0.101(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 Fe1 0.0186(2) 0.0212(2) 0.0199(2) 0.00277(19) 0.00759(19) 0.00006(19) Fe2 0.0186(2) 0.0247(2) 0.0219(2) 0.00511(19) 0.0074(2) 0.0002(2) Co1 0.01371(19) 0.02183(19) 0.01899(19) 0.00048(15) 0.00608(15) -0.00176(15) O1 0.0156(12) 0.0231(12) 0.0192(12) 0.0029(9) 0.0038(9) -0.0017(10) O2 0.0176(12) 0.0239(12) 0.0196(11) -0.0018(10) 0.0060(9) -0.0047(10) O3 0.0230(13) 0.0255(13) 0.0186(12) 0.0015(9) 0.0056(10) -0.0039(10) O4 0.0269(13) 0.0239(12) 0.0184(12) -0.0005(10) 0.0114(10) -0.0033(10) O5 0.0254(14) 0.0314(14) 0.0317(14) 0.0075(11) 0.0093(12) 0.0059(11) O6 0.0334(15) 0.0283(14) 0.0245(13) 0.0032(10) 0.0052(11) 0.0005(11) O7 0.0317(18) 0.054(2) 0.071(2) 0.0143(19) -0.0011(17) 0.0139(16) O8 0.084(3) 0.072(3) 0.0377(19) 0.0101(18) -0.0194(19) 0.017(2) O9 0.0219(13) 0.0202(12) 0.0266(13) 0.0016(10) 0.0066(11) -0.0009(10) O10 0.0253(14) 0.0230(13) 0.0367(15) 0.0036(11) 0.0133(12) 0.0025(11) O11 0.0248(15) 0.0331(15) 0.0491(18) 0.0073(13) -0.0015(13) -0.0048(12) O12 0.0261(15) 0.0429(17) 0.0537(19) 0.0074(15) 0.0124(14) 0.0067(13) O13 0.0180(12) 0.0263(13) 0.0225(12) -0.0016(10) 0.0077(10) -0.0018(10) O14 0.0178(12) 0.0273(13) 0.0167(11) 0.0001(10) 0.0059(9) -0.0038(10) O15 0.0242(13) 0.0250(12) 0.0206(12) 0.0032(10) 0.0057(10) -0.0026(10) O16 0.0222(13) 0.0272(13) 0.0236(12) 0.0015(10) 0.0066(10) -0.0086(10) O17 0.0249(14) 0.0326(14) 0.0341(15) 0.0095(12) 0.0087(12) 0.0057(12) O18 0.0258(14) 0.0372(16) 0.0338(15) 0.0062(12) 0.0068(12) -0.0059(12) O19 0.0249(16) 0.066(2) 0.063(2) 0.0038(18) 0.0164(15) 0.0053(15) O20 0.0340(17) 0.053(2) 0.049(2) 0.0093(16) 0.0010(15) -0.0066(15) O21 0.0314(15) 0.0369(16) 0.0234(13) 0.0063(11) 0.0069(11) 0.0025(12) O22 0.0268(14) 0.0301(14) 0.0365(16) 0.0050(11) 0.0109(12) 0.0078(12) O23 0.0475(19) 0.069(2) 0.0298(16) 0.0166(16) -0.0016(14) 0.0060(17) O24 0.0250(16) 0.057(2) 0.068(2) 0.0257(18) 0.0058(15) 0.0106(15) N1 0.0171(15) 0.0297(16) 0.0252(15) 0.0023(13) 0.0085(12) -0.0021(13) N2 0.0112(13) 0.0267(15) 0.0212(14) -0.0002(12) 0.0045(11) 0.0007(12) N3 0.0169(15) 0.0434(19) 0.0199(15) -0.0046(13) 0.0083(12) 0.0005(13) N4 0.0217(16) 0.0397(18) 0.0242(16) -0.0027(13) 0.0120(13) 0.0025(13) N5 0.0162(14) 0.0308(16) 0.0226(15) 0.0022(12) 0.0086(12) 0.0029(12) N6 0.0234(18) 0.080(3) 0.0287(18) -0.0169(19) 0.0065(15) 0.0021(19) N7 0.0182(17) 0.083(3) 0.0266(18) 0.0001(19) 0.0091(14) 0.0064(19) N8 0.0185(16) 0.050(2) 0.0283(17) -0.0068(15) 0.0133(13) -0.0011(14) N9 0.0256(18) 0.064(2) 0.0277(17) -0.0135(16) 0.0147(15) -0.0074(17) N10 0.0187(16) 0.057(2) 0.0275(17) -0.0091(16) 0.0112(13) -0.0061(15) N11 0.0155(14) 0.0304(16) 0.0178(14) 0.0007(12) 0.0067(12) -0.0012(12) N12 0.0142(14) 0.0322(16) 0.0286(16) 0.0021(13) 0.0084(12) 0.0013(13) C1 0.0128(16) 0.0283(17) 0.0245(17) 0.0022(14) 0.0040(13) -0.0050(14) C2 0.0194(17) 0.0280(18) 0.0234(17) -0.0002(14) 0.0060(14) 0.0004(14) C3 0.0161(16) 0.0254(17) 0.0218(17) -0.0014(13) 0.0045(14) 0.0003(13) C4 0.0137(16) 0.0241(17) 0.0234(17) -0.0022(14) 0.0036(14) -0.0002(13) C5 0.0091(14) 0.0222(16) 0.0219(16) 0.0010(13) 0.0043(12) 0.0016(13) C6 0.0112(16) 0.0274(18) 0.0172(15) -0.0019(13) 0.0059(13) -0.0025(13) C7 0.0158(16) 0.0233(16) 0.0185(16) -0.0021(12) 0.0029(13) -0.0004(13) C8 0.0163(16) 0.0215(16) 0.0252(17) 0.0003(13) 0.0082(14) -0.0014(13) C9 0.0178(17) 0.0219(16) 0.0204(16) -0.0016(13) 0.0050(13) 0.0015(13) C10 0.0203(18) 0.0240(17) 0.0249(18) 0.0021(14) 0.0066(14) 0.0011(14) C11 0.0138(16) 0.0337(19) 0.0187(16) 0.0016(14) 0.0054(13) 0.0011(15) C12 0.0180(17) 0.0292(18) 0.0219(17) 0.0031(14) 0.0074(14) 0.0019(14) C13 0.0153(16) 0.0239(16) 0.0202(16) 0.0055(13) 0.0042(13) 0.0028(13) C14 0.0175(16) 0.0243(17) 0.0219(16) 0.0067(13) 0.0080(13) 0.0021(13) C15 0.0187(17) 0.0269(18) 0.0226(17) 0.0045(14) 0.0097(14) 0.0005(14) C16 0.0174(17) 0.0329(19) 0.0256(18) 0.0069(15) 0.0096(14) 0.0048(14) C17 0.0265(18) 0.0209(16) 0.0247(17) 0.0015(13) 0.0065(14) -0.0033(14) C18 0.0172(16) 0.0280(18) 0.0268(18) 0.0090(14) 0.0046(14) -0.0059(14) C19 0.035(2) 0.028(2) 0.052(3) 0.0125(18) 0.025(2) 0.0076(17) C20 0.032(2) 0.0248(18) 0.0278(19) -0.0022(14) 0.0164(16) -0.0032(15) C21 0.035(2) 0.034(2) 0.052(3) 0.0041(19) 0.023(2) 0.0097(18) C22 0.030(2) 0.032(2) 0.030(2) -0.0037(16) 0.0160(17) -0.0075(16) C23 0.0154(17) 0.036(2) 0.0296(18) -0.0055(15) 0.0075(14) 0.0013(14) C24 0.0167(18) 0.049(2) 0.0232(18) -0.0140(17) 0.0058(14) 0.0003(17) C25 0.030(2) 0.050(3) 0.059(3) -0.023(2) 0.024(2) -0.008(2) C26 0.0220(18) 0.064(3) 0.0250(18) -0.0002(19) 0.0092(15) 0.006(2) C27 0.037(3) 0.054(3) 0.064(3) -0.027(3) 0.015(2) 0.003(2) C28 0.021(2) 0.091(4) 0.024(2) -0.007(2) 0.0042(16) 0.003(2) C29 0.0179(18) 0.086(4) 0.0247(19) 0.008(2) 0.0083(15) 0.003(2) C30 0.035(2) 0.066(3) 0.032(2) -0.014(2) 0.0142(19) 0.003(2) C31 0.0184(19) 0.068(3) 0.0214(18) -0.0037(18) 0.0047(15) -0.0012(19) C32 0.028(2) 0.062(3) 0.035(2) -0.014(2) 0.0167(18) -0.012(2) C33 0.0129(16) 0.064(3) 0.0225(18) -0.0102(17) 0.0056(14) -0.0004(17) C34 0.0169(17) 0.057(3) 0.0210(17) -0.0114(18) 0.0096(14) -0.0068(18) C35 0.029(2) 0.061(3) 0.028(2) -0.0099(19) 0.0181(17) -0.009(2) C36 0.025(2) 0.058(3) 0.032(2) -0.0055(19) 0.0147(17) 0.0044(19) C37 0.026(2) 0.045(2) 0.038(2) -0.0063(18) 0.0168(17) -0.0047(18) C38 0.029(2) 0.055(3) 0.032(2) 0.0030(19) 0.0148(17) 0.002(2) C39 0.0186(18) 0.046(2) 0.0263(19) 0.0006(17) 0.0150(16) 0.0018(16) C40 0.0164(17) 0.036(2) 0.0187(16) 0.0040(14) 0.0083(13) 0.0016(15) C41 0.0158(17) 0.036(2) 0.0220(17) 0.0038(14) 0.0097(14) 0.0053(15) C42 0.0185(17) 0.0335(19) 0.0226(17) 0.0088(14) 0.0098(14) 0.0065(14) C43 0.0163(17) 0.038(2) 0.0280(19) 0.0070(16) 0.0108(14) 0.0023(15) C44 0.0204(18) 0.042(2) 0.0197(17) -0.0009(15) 0.0078(14) 0.0007(16) C45 0.0162(17) 0.048(2) 0.0276(19) 0.0011(17) 0.0039(15) -0.0033(16) C46 0.0221(19) 0.051(2) 0.0243(18) -0.0060(16) 0.0075(15) -0.0094(17) C47 0.0160(17) 0.0275(18) 0.0252(18) 0.0039(14) 0.0082(14) -0.0002(14) C48 0.0159(17) 0.0292(18) 0.0231(17) -0.0042(14) 0.0044(14) 0.0023(14) C49 0.0162(16) 0.0265(17) 0.0217(17) 0.0019(14) 0.0070(14) 0.0031(14) C50 0.0159(16) 0.0254(18) 0.0256(17) -0.0025(14) 0.0073(14) -0.0033(13) C51 0.0111(15) 0.0302(18) 0.0179(15) 0.0018(13) 0.0019(13) 0.0012(14) C52 0.0148(16) 0.0238(17) 0.0187(16) 0.0017(13) 0.0052(13) 0.0015(14) C53 0.0202(18) 0.0284(18) 0.0276(18) 0.0001(15) 0.0084(15) -0.0015(15) C54 0.0175(17) 0.0252(17) 0.0220(17) -0.0028(13) 0.0094(14) -0.0027(13) C55 0.0216(18) 0.0311(19) 0.0273(18) -0.0034(15) 0.0126(15) 0.0023(15) C56 0.0167(17) 0.0307(19) 0.033(2) -0.0022(15) 0.0067(15) -0.0055(14) C57 0.0095(15) 0.0190(15) 0.0212(16) 0.0004(12) 0.0029(12) 0.0036(12) C58 0.0153(16) 0.0203(16) 0.0208(16) 0.0011(13) 0.0018(13) 0.0036(13) C59 0.030(2) 0.0244(19) 0.047(2) 0.0049(17) 0.0046(19) 0.0019(16) C60 0.037(2) 0.033(2) 0.036(2) 0.0067(17) -0.0028(19) -0.0016(18) C61 0.0222(19) 0.0285(19) 0.0264(18) 0.0094(15) 0.0050(15) -0.0006(15) C62 0.0269(19) 0.0285(19) 0.0268(18) 0.0058(14) 0.0103(15) 0.0040(15) C63 0.0169(17) 0.0200(16) 0.0196(16) 0.0025(13) 0.0051(13) 0.0035(13) C64 0.0133(16) 0.0240(17) 0.0201(16) 0.0020(13) 0.0045(13) -0.0023(13) C65 0.0199(19) 0.044(2) 0.038(2) 0.0167(19) 0.0041(16) 0.0018(17) C66 0.024(2) 0.038(2) 0.036(2) 0.0121(18) 0.0041(17) -0.0048(17) C67 0.0243(19) 0.032(2) 0.037(2) 0.0089(16) 0.0033(17) -0.0022(16) C68 0.028(2) 0.0264(19) 0.039(2) 0.0094(16) 0.0046(17) 0.0003(16) O1W 0.0194(13) 0.0268(13) 0.0340(15) 0.0034(11) 0.0124(11) 0.0026(11) O2W 0.0157(12) 0.0240(13) 0.0324(14) 0.0033(11) 0.0087(11) 0.0018(10) O3W 0.094(4) 0.105(4) 0.131(5) 0.034(4) 0.019(4) -0.012(3) O4W 0.061(2) 0.056(2) 0.058(2) -0.0075(18) -0.0026(19) 0.0054(19) O5W 0.082(3) 0.0346(18) 0.117(4) 0.022(2) 0.075(3) 0.0103(18) O6W 0.0440(18) 0.0373(16) 0.0407(17) 0.0096(13) 0.0072(14) -0.0034(14) O7W 0.060(5) 0.023(3) 0.023(3) -0.002(3) 0.007(3) -0.013(3) O71W 0.066(13) 0.064(12) 0.065(13) 0.013(10) 0.029(11) 0.013(10) O72W 0.057(5) 0.060(6) 0.057(6) 0.003(5) 0.027(5) 0.014(5) O8W 0.044(4) 0.124(8) 0.083(6) 0.042(6) 0.028(4) 0.007(5) O8W' 0.041(4) 0.092(7) 0.103(7) 0.031(6) 0.012(5) 0.008(4) O9W 0.228(9) 0.168(7) 0.319(12) 0.158(8) 0.218(9) 0.128(7) O11W 0.176(7) 0.101(5) 0.131(5) 0.018(4) 0.090(5) 0.026(5) O10W 0.076(6) 0.058(5) 0.099(7) -0.029(5) 0.026(5) 0.016(4) O12W 0.056(2) 0.0412(18) 0.056(2) 0.0136(16) 0.0317(17) 0.0068(16) O13W 0.068(4) 0.085(4) 0.356(13) 0.066(6) -0.042(5) -0.004(3) O15W 0.058(3) 0.171(6) 0.078(3) 0.025(3) 0.023(2) -0.028(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O10 1.988(3) . ? Fe1 O9 1.990(3) . ? Fe1 O6 2.010(3) . ? Fe1 O5 2.018(3) . ? Fe1 O3 2.042(2) . ? Fe1 O4 2.054(3) . ? Fe2 O18 1.978(3) . ? Fe2 O17 1.987(3) . ? Fe2 O21 1.994(3) . ? Fe2 O22 2.027(3) . ? Fe2 O16 2.039(3) . ? Fe2 O15 2.064(3) . ? Co1 O1W 2.052(3) . ? Co1 O2W 2.071(3) . ? Co1 O1 2.098(2) . ? Co1 O14 2.102(2) . ? Co1 O13 2.110(2) . ? Co1 O2 2.115(2) . ? O1 C57 1.248(4) . ? O2 C58 1.242(4) . ? O3 C57 1.259(4) . ? O4 C58 1.270(4) . ? O5 C59 1.282(5) . ? O6 C60 1.314(5) . ? O7 C59 1.231(5) . ? O8 C60 1.203(5) . ? O9 C61 1.294(5) . ? O10 C62 1.283(5) . ? O11 C61 1.230(5) . ? O12 C62 1.222(5) . ? O13 C63 1.234(4) . ? O14 C64 1.237(4) . ? O15 C63 1.264(4) . ? O16 C64 1.259(4) . ? O17 C65 1.279(5) . ? O18 C66 1.313(5) . ? O19 C65 1.234(5) . ? O20 C66 1.226(5) . ? O21 C67 1.293(5) . ? O22 C68 1.288(5) . ? O23 C67 1.232(5) . ? O24 C68 1.216(5) . ? N1 C2 1.336(5) . ? N1 C1 1.347(5) . ? N2 C10 1.358(5) . ? N2 C9 1.361(5) . ? N2 C11 1.458(4) . ? N3 C11 1.305(5) . ? N3 N4 1.360(4) . ? N4 C12 1.305(5) . ? N5 C19 1.336(5) . ? N5 C20 1.341(5) . ? N5 C12 1.457(4) . ? N6 C28 1.321(7) . ? N6 C27 1.325(7) . ? N7 C30 1.317(7) . ? N7 C29 1.321(7) . ? N8 C38 1.331(6) . ? N8 C37 1.347(6) . ? N8 C39 1.454(5) . ? N9 C39 1.307(5) . ? N9 N10 1.372(4) . ? N10 C40 1.291(5) . ? N11 C48 1.351(5) . ? N11 C47 1.352(5) . ? N11 C40 1.454(4) . ? N12 C56 1.326(5) . ? N12 C55 1.338(5) . ? C1 C3 1.377(5) . ? C1 H27A 0.9300 . ? C2 C4 1.397(5) . ? C2 H28A 0.9300 . ? C3 C5 1.387(5) . ? C3 H25A 0.9300 . ? C4 C5 1.383(5) . ? C4 H26A 0.9300 . ? C5 C6 1.484(4) . ? C6 C7 1.392(5) . ? C6 C8 1.417(5) . ? C7 C9 1.370(5) . ? C7 H21A 0.9300 . ? C8 C10 1.366(5) . ? C8 H22A 0.9300 . ? C9 H19A 0.9300 . ? C10 H20A 0.9300 . ? C11 C13 1.414(5) . ? C12 C14 1.415(5) . ? C13 C15 1.396(5) . ? C13 C14 1.419(5) . ? C14 C16 1.406(5) . ? C15 C17 1.365(5) . ? C15 H16A 0.9300 . ? C16 C18 1.376(5) . ? C16 H15A 0.9300 . ? C17 C18 1.414(5) . ? C17 H18A 0.9300 . ? C18 H17A 0.9300 . ? C19 C21 1.387(6) . ? C19 H9A 0.9300 . ? C20 C22 1.382(5) . ? C20 H10A 0.9300 . ? C21 C23 1.388(6) . ? C21 H7A 0.9300 . ? C22 C23 1.383(6) . ? C22 H8A 0.9300 . ? C23 C24 1.487(5) . ? C24 C25 1.374(7) . ? C24 C26 1.392(6) . ? C25 C27 1.408(6) . ? C25 H3A 0.9300 . ? C26 C28 1.395(6) . ? C26 H4A 0.9300 . ? C27 H1A 0.9300 . ? C28 H2A 0.9300 . ? C29 C31 1.382(6) . ? C29 H29A 0.9300 . ? C30 C32 1.395(6) . ? C30 H30A 0.9300 . ? C31 C33 1.385(6) . ? C31 H31A 0.9300 . ? C32 C33 1.365(7) . ? C32 H32A 0.9300 . ? C33 C34 1.500(5) . ? C34 C35 1.351(7) . ? C34 C36 1.394(6) . ? C35 C37 1.376(5) . ? C35 H35A 0.9300 . ? C36 C38 1.391(5) . ? C36 H36A 0.9300 . ? C37 H37A 0.9300 . ? C38 H38A 0.9300 . ? C39 C41 1.408(6) . ? C40 C42 1.422(5) . ? C41 C43 1.396(5) . ? C41 C42 1.430(5) . ? C42 C44 1.405(5) . ? C43 C45 1.358(6) . ? C43 H44A 0.9300 . ? C44 C46 1.369(5) . ? C44 H43A 0.9300 . ? C45 C46 1.404(5) . ? C45 H45A 0.9300 . ? C46 H46A 0.9300 . ? C47 C49 1.381(5) . ? C47 H47A 0.9300 . ? C48 C50 1.387(5) . ? C48 H48A 0.9300 . ? C49 C51 1.396(5) . ? C49 H49A 0.9300 . ? C50 C51 1.393(5) . ? C50 H50A 0.9300 . ? C51 C52 1.476(5) . ? C52 C54 1.396(5) . ? C52 C53 1.398(5) . ? C53 C55 1.386(5) . ? C53 H53A 0.9300 . ? C54 C56 1.390(5) . ? C54 H54A 0.9300 . ? C55 H55A 0.9300 . ? C56 H56A 0.9300 . ? C57 C58 1.541(5) . ? C59 C60 1.548(6) . ? C61 C62 1.552(5) . ? C63 C64 1.569(5) . ? C65 C66 1.570(7) . ? C67 C68 1.534(6) . ? O1W H2 0.9637 . ? O1W H1 0.7121 . ? O2W H4 0.9169 . ? O2W H3 0.8765 . ? O4W H8 0.9260 . ? O4W H7 0.8855 . ? O6W H12 0.8479 . ? O6W H11 0.8837 . ? O7W O72W 1.651(13) . ? O71W O72W 1.29(2) . ? O8W O8W' 1.623(16) . ? O12W H23 0.7384 . ? O12W H24 0.8680 . ? 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 O10 Fe1 O9 81.15(11) . . ? O10 Fe1 O6 92.64(12) . . ? O9 Fe1 O6 102.19(11) . . ? O10 Fe1 O5 172.79(11) . . ? O9 Fe1 O5 97.66(11) . . ? O6 Fe1 O5 80.63(11) . . ? O10 Fe1 O3 98.84(11) . . ? O9 Fe1 O3 88.75(10) . . ? O6 Fe1 O3 165.26(11) . . ? O5 Fe1 O3 88.22(11) . . ? O10 Fe1 O4 92.82(11) . . ? O9 Fe1 O4 166.50(10) . . ? O6 Fe1 O4 90.09(10) . . ? O5 Fe1 O4 89.79(11) . . ? O3 Fe1 O4 80.20(10) . . ? O18 Fe2 O17 82.59(12) . . ? O18 Fe2 O21 98.81(12) . . ? O17 Fe2 O21 89.95(11) . . ? O18 Fe2 O22 99.75(12) . . ? O17 Fe2 O22 170.25(12) . . ? O21 Fe2 O22 80.35(12) . . ? O18 Fe2 O16 89.88(11) . . ? O17 Fe2 O16 101.55(11) . . ? O21 Fe2 O16 166.43(11) . . ? O22 Fe2 O16 87.95(11) . . ? O18 Fe2 O15 167.05(11) . . ? O17 Fe2 O15 91.38(11) . . ? O21 Fe2 O15 92.61(11) . . ? O22 Fe2 O15 88.12(11) . . ? O16 Fe2 O15 80.07(10) . . ? O1W Co1 O2W 179.32(12) . . ? O1W Co1 O1 89.04(11) . . ? O2W Co1 O1 91.18(9) . . ? O1W Co1 O14 91.88(10) . . ? O2W Co1 O14 87.90(10) . . ? O1 Co1 O14 179.07(11) . . ? O1W Co1 O13 91.66(10) . . ? O2W Co1 O13 87.67(10) . . ? O1 Co1 O13 100.13(10) . . ? O14 Co1 O13 80.02(9) . . ? O1W Co1 O2 86.77(10) . . ? O2W Co1 O2 93.90(10) . . ? O1 Co1 O2 79.83(9) . . ? O14 Co1 O2 100.04(9) . . ? O13 Co1 O2 178.43(11) . . ? C57 O1 Co1 112.6(2) . . ? C58 O2 Co1 111.7(2) . . ? C57 O3 Fe1 113.4(2) . . ? C58 O4 Fe1 113.0(2) . . ? C59 O5 Fe1 114.8(3) . . ? C60 O6 Fe1 114.3(3) . . ? C61 O9 Fe1 115.4(2) . . ? C62 O10 Fe1 116.0(2) . . ? C63 O13 Co1 112.6(2) . . ? C64 O14 Co1 112.4(2) . . ? C63 O15 Fe2 113.2(2) . . ? C64 O16 Fe2 114.4(2) . . ? C65 O17 Fe2 115.4(3) . . ? C66 O18 Fe2 113.9(3) . . ? C67 O21 Fe2 115.2(3) . . ? C68 O22 Fe2 114.6(3) . . ? C2 N1 C1 116.4(3) . . ? C10 N2 C9 121.3(3) . . ? C10 N2 C11 122.1(3) . . ? C9 N2 C11 116.5(3) . . ? C11 N3 N4 119.0(3) . . ? C12 N4 N3 117.7(3) . . ? C19 N5 C20 121.5(3) . . ? C19 N5 C12 118.2(3) . . ? C20 N5 C12 120.3(3) . . ? C28 N6 C27 116.9(4) . . ? C30 N7 C29 116.2(4) . . ? C38 N8 C37 121.8(3) . . ? C38 N8 C39 117.5(4) . . ? C37 N8 C39 120.5(4) . . ? C39 N9 N10 117.1(3) . . ? C40 N10 N9 118.5(3) . . ? C48 N11 C47 121.8(3) . . ? C48 N11 C40 116.7(3) . . ? C47 N11 C40 121.3(3) . . ? C56 N12 C55 117.9(3) . . ? N1 C1 C3 124.4(3) . . ? N1 C1 H27A 117.8 . . ? C3 C1 H27A 117.8 . . ? N1 C2 C4 123.2(3) . . ? N1 C2 H28A 118.4 . . ? C4 C2 H28A 118.4 . . ? C1 C3 C5 118.6(3) . . ? C1 C3 H25A 120.7 . . ? C5 C3 H25A 120.7 . . ? C5 C4 C2 119.1(3) . . ? C5 C4 H26A 120.4 . . ? C2 C4 H26A 120.4 . . ? C4 C5 C3 118.2(3) . . ? C4 C5 C6 122.2(3) . . ? C3 C5 C6 119.6(3) . . ? C7 C6 C8 117.9(3) . . ? C7 C6 C5 120.1(3) . . ? C8 C6 C5 122.0(3) . . ? C9 C7 C6 120.6(3) . . ? C9 C7 H21A 119.7 . . ? C6 C7 H21A 119.7 . . ? C10 C8 C6 119.9(3) . . ? C10 C8 H22A 120.1 . . ? C6 C8 H22A 120.1 . . ? N2 C9 C7 119.9(3) . . ? N2 C9 H19A 120.1 . . ? C7 C9 H19A 120.1 . . ? N2 C10 C8 120.3(3) . . ? N2 C10 H20A 119.8 . . ? C8 C10 H20A 119.8 . . ? N3 C11 C13 127.2(3) . . ? N3 C11 N2 110.9(3) . . ? C13 C11 N2 121.8(3) . . ? N4 C12 C14 126.8(3) . . ? N4 C12 N5 112.3(3) . . ? C14 C12 N5 120.8(3) . . ? C15 C13 C11 126.1(3) . . ? C15 C13 C14 119.9(3) . . ? C11 C13 C14 113.7(3) . . ? C16 C14 C12 124.4(3) . . ? C16 C14 C13 119.9(3) . . ? C12 C14 C13 115.5(3) . . ? C17 C15 C13 119.2(3) . . ? C17 C15 H16A 120.4 . . ? C13 C15 H16A 120.4 . . ? C18 C16 C14 119.3(3) . . ? C18 C16 H15A 120.4 . . ? C14 C16 H15A 120.4 . . ? C15 C17 C18 121.7(3) . . ? C15 C17 H18A 119.2 . . ? C18 C17 H18A 119.2 . . ? C16 C18 C17 119.9(3) . . ? C16 C18 H17A 120.0 . . ? C17 C18 H17A 120.0 . . ? N5 C19 C21 119.6(4) . . ? N5 C19 H9A 120.2 . . ? C21 C19 H9A 120.2 . . ? N5 C20 C22 120.1(4) . . ? N5 C20 H10A 119.9 . . ? C22 C20 H10A 119.9 . . ? C19 C21 C23 121.0(4) . . ? C19 C21 H7A 119.5 . . ? C23 C21 H7A 119.5 . . ? C20 C22 C23 120.7(4) . . ? C20 C22 H8A 119.7 . . ? C23 C22 H8A 119.7 . . ? C22 C23 C21 117.2(3) . . ? C22 C23 C24 121.3(4) . . ? C21 C23 C24 121.5(4) . . ? C25 C24 C26 117.4(4) . . ? C25 C24 C23 121.8(4) . . ? C26 C24 C23 120.7(4) . . ? C24 C25 C27 119.0(5) . . ? C24 C25 H3A 120.5 . . ? C27 C25 H3A 120.5 . . ? C24 C26 C28 119.0(5) . . ? C24 C26 H4A 120.5 . . ? C28 C26 H4A 120.5 . . ? N6 C27 C25 123.6(5) . . ? N6 C27 H1A 118.2 . . ? C25 C27 H1A 118.2 . . ? N6 C28 C26 124.0(5) . . ? N6 C28 H2A 118.0 . . ? C26 C28 H2A 118.0 . . ? N7 C29 C31 124.6(5) . . ? N7 C29 H29A 117.7 . . ? C31 C29 H29A 117.7 . . ? N7 C30 C32 123.7(5) . . ? N7 C30 H30A 118.1 . . ? C32 C30 H30A 118.1 . . ? C29 C31 C33 118.6(5) . . ? C29 C31 H31A 120.7 . . ? C33 C31 H31A 120.7 . . ? C33 C32 C30 119.4(5) . . ? C33 C32 H32A 120.3 . . ? C30 C32 H32A 120.3 . . ? C32 C33 C31 117.4(4) . . ? C32 C33 C34 121.1(4) . . ? C31 C33 C34 121.5(4) . . ? C35 C34 C36 118.0(4) . . ? C35 C34 C33 122.8(4) . . ? C36 C34 C33 119.2(4) . . ? C34 C35 C37 121.8(4) . . ? C34 C35 H35A 119.1 . . ? C37 C35 H35A 119.1 . . ? C38 C36 C34 119.7(4) . . ? C38 C36 H36A 120.2 . . ? C34 C36 H36A 120.2 . . ? N8 C37 C35 119.0(4) . . ? N8 C37 H37A 120.5 . . ? C35 C37 H37A 120.5 . . ? N8 C38 C36 119.7(4) . . ? N8 C38 H38A 120.2 . . ? C36 C38 H38A 120.2 . . ? N9 C39 C41 128.7(3) . . ? N9 C39 N8 111.5(4) . . ? C41 C39 N8 119.7(3) . . ? N10 C40 C42 127.6(3) . . ? N10 C40 N11 111.4(3) . . ? C42 C40 N11 120.8(3) . . ? C43 C41 C39 126.1(3) . . ? C43 C41 C42 120.1(4) . . ? C39 C41 C42 113.7(3) . . ? C44 C42 C40 125.9(3) . . ? C44 C42 C41 119.6(3) . . ? C40 C42 C41 114.4(3) . . ? C45 C43 C41 119.0(3) . . ? C45 C43 H44A 120.5 . . ? C41 C43 H44A 120.5 . . ? C46 C44 C42 118.3(3) . . ? C46 C44 H43A 120.8 . . ? C42 C44 H43A 120.8 . . ? C43 C45 C46 121.2(4) . . ? C43 C45 H45A 119.4 . . ? C46 C45 H45A 119.4 . . ? C44 C46 C45 121.6(4) . . ? C44 C46 H46A 119.2 . . ? C45 C46 H46A 119.2 . . ? N11 C47 C49 119.8(3) . . ? N11 C47 H47A 120.1 . . ? C49 C47 H47A 120.1 . . ? N11 C48 C50 120.0(3) . . ? N11 C48 H48A 120.0 . . ? C50 C48 H48A 120.0 . . ? C47 C49 C51 120.0(3) . . ? C47 C49 H49A 120.0 . . ? C51 C49 H49A 120.0 . . ? C48 C50 C51 119.6(3) . . ? C48 C50 H50A 120.2 . . ? C51 C50 H50A 120.2 . . ? C50 C51 C49 118.8(3) . . ? C50 C51 C52 119.8(3) . . ? C49 C51 C52 121.4(3) . . ? C54 C52 C53 117.4(3) . . ? C54 C52 C51 120.0(3) . . ? C53 C52 C51 122.6(3) . . ? C55 C53 C52 119.1(3) . . ? C55 C53 H53A 120.4 . . ? C52 C53 H53A 120.4 . . ? C56 C54 C52 119.1(3) . . ? C56 C54 H54A 120.5 . . ? C52 C54 H54A 120.5 . . ? N12 C55 C53 123.1(3) . . ? N12 C55 H55A 118.5 . . ? C53 C55 H55A 118.5 . . ? N12 C56 C54 123.4(3) . . ? N12 C56 H56A 118.3 . . ? C54 C56 H56A 118.3 . . ? O1 C57 O3 126.6(3) . . ? O1 C57 C58 117.2(3) . . ? O3 C57 C58 116.1(3) . . ? O2 C58 O4 126.3(3) . . ? O2 C58 C57 118.4(3) . . ? O4 C58 C57 115.3(3) . . ? O7 C59 O5 126.3(4) . . ? O7 C59 C60 119.4(4) . . ? O5 C59 C60 114.3(4) . . ? O8 C60 O6 124.1(5) . . ? O8 C60 C59 122.1(4) . . ? O6 C60 C59 113.7(4) . . ? O11 C61 O9 125.4(4) . . ? O11 C61 C62 120.9(3) . . ? O9 C61 C62 113.8(3) . . ? O12 C62 O10 125.9(4) . . ? O12 C62 C61 120.5(4) . . ? O10 C62 C61 113.6(3) . . ? O13 C63 O15 127.8(3) . . ? O13 C63 C64 117.2(3) . . ? O15 C63 C64 115.0(3) . . ? O14 C64 O16 127.1(3) . . ? O14 C64 C63 117.7(3) . . ? O16 C64 C63 115.2(3) . . ? O19 C65 O17 125.4(4) . . ? O19 C65 C66 121.3(4) . . ? O17 C65 C66 113.2(3) . . ? O20 C66 O18 124.0(4) . . ? O20 C66 C65 121.7(4) . . ? O18 C66 C65 114.3(3) . . ? O23 C67 O21 124.3(4) . . ? O23 C67 C68 121.1(4) . . ? O21 C67 C68 114.6(4) . . ? O24 C68 O22 125.9(4) . . ? O24 C68 C67 121.0(4) . . ? O22 C68 C67 113.0(3) . . ? H2 O1W H1 110.0 . . ? H4 O2W H3 103.6 . . ? H8 O4W H7 115.1 . . ? H12 O6W H11 97.8 . . ? H23 O12W H24 94.1 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H2 N12 0.96 1.83 2.781(4) 170.6 2_856 O1W H1 O12W 0.71 2.04 2.741(4) 167.9 . O2W H4 N1 0.92 1.89 2.808(4) 177.1 2_557 O2W H3 O5W 0.88 1.89 2.757(4) 168.6 . O4W H8 O18 0.93 2.03 2.948(5) 168.9 . O4W H7 O7 0.89 2.09 2.901(6) 151.9 2_757 O6W H12 O9 0.85 2.04 2.879(4) 168.0 2_656 O6W H11 O23 0.88 1.90 2.775(5) 168.1 . O12W H23 O13W 0.74 2.22 2.790(8) 135.0 1_655 O12W H24 O5 0.87 2.00 2.834(4) 160.8 . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.674 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.078 data_s_3 _database_code_depnum_ccdc_archive 'CCDC 265932' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H69 Cr2 Mn N12 O38.50' _chemical_formula_weight 1829.29 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.059(3) _cell_length_b 20.686(5) _cell_length_c 16.154(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.544(3) _cell_angle_gamma 90.00 _cell_volume 3985.2(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8254 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour Indigo _exptl_crystal_size_max 0.3400 _exptl_crystal_size_mid 0.1800 _exptl_crystal_size_min 0.1600 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1884 _exptl_absorpt_coefficient_mu 0.527 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.892 _exptl_absorpt_correction_T_max 0.919 _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 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26486 _diffrn_reflns_av_R_equivalents 0.1200 _diffrn_reflns_av_sigmaI/netI 0.2270 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.48 _reflns_number_total 12815 _reflns_number_gt 5483 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0658P)^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 SHELXL _refine_ls_extinction_coef 0.0067(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.33(4) _refine_ls_number_reflns 12815 _refine_ls_number_parameters 1043 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1642 _refine_ls_R_factor_gt 0.1058 _refine_ls_wR_factor_ref 0.2377 _refine_ls_wR_factor_gt 0.2020 _refine_ls_goodness_of_fit_ref 0.918 _refine_ls_restrained_S_all 0.976 _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 Cr1 Cr 0.50995(15) 0.27970(8) 0.03721(10) 0.0347(4) Uani 1 1 d . . . Cr2 Cr 0.08087(17) -0.03480(9) 0.42699(12) 0.0441(5) Uani 1 1 d . . . Mn1 Mn 0.29559(15) 0.12010(10) 0.22898(12) 0.0397(4) Uani 1 1 d . . . O1 O 0.4235(6) 0.1972(5) 0.2378(4) 0.045(2) Uani 1 1 d . . . O2 O 0.3239(6) 0.1349(4) 0.0997(5) 0.0421(19) Uani 1 1 d . . . O3 O 0.5143(7) 0.2581(4) 0.1577(5) 0.050(2) Uani 1 1 d . . . O4 O 0.4162(7) 0.1985(4) 0.0202(5) 0.050(2) Uani 1 1 d . . . O5 O 0.3683(8) 0.3286(4) 0.0354(6) 0.052(2) Uani 1 1 d . . . O6 O 0.4753(7) 0.2968(4) -0.0860(5) 0.048(2) Uani 1 1 d . . . O7 O 0.2110(11) 0.3528(6) -0.0538(9) 0.100(5) Uani 1 1 d . . . O8 O 0.3447(16) 0.3348(12) -0.1795(11) 0.175(9) Uani 1 1 d . . . O9 O 0.6106(8) 0.3539(4) 0.0656(7) 0.057(2) Uani 1 1 d . . . O10 O 0.6521(8) 0.2351(5) 0.0303(6) 0.060(3) Uani 1 1 d . . . O11 O 0.7932(8) 0.3786(4) 0.0871(6) 0.064(3) Uani 1 1 d . . . O12 O 0.8429(9) 0.2540(6) 0.0424(9) 0.103(4) Uani 1 1 d . . . O13 O 0.2654(7) 0.1113(5) 0.3606(5) 0.050(2) Uani 1 1 d . . . O14 O 0.1701(7) 0.0421(4) 0.2210(5) 0.0421(19) Uani 1 1 d . . . O15 O 0.1677(9) 0.0481(4) 0.4359(6) 0.061(3) Uani 1 1 d . . . O16 O 0.0793(8) -0.0199(4) 0.3036(6) 0.060(2) Uani 1 1 d . . . O17 O -0.0629(7) 0.0082(5) 0.4314(6) 0.057(2) Uani 1 1 d . . . O18 O -0.0192(8) -0.1114(5) 0.3967(6) 0.063(3) Uani 1 1 d . . . O19 O -0.2669(18) -0.0169(8) 0.4304(8) 0.165(9) Uani 1 1 d . . . O20 O -0.2059(12) -0.1352(7) 0.3838(9) 0.117(5) Uani 1 1 d . . . O21 O 0.1005(8) -0.0497(5) 0.5453(6) 0.072(3) Uani 1 1 d . . . O22 O 0.2214(8) -0.0833(5) 0.4275(8) 0.075(3) Uani 1 1 d . . . O23 O 0.2267(13) -0.0985(8) 0.6437(8) 0.132(6) Uani 1 1 d . . . O24 O 0.3742(13) -0.1117(8) 0.5196(10) 0.138(6) Uani 1 1 d . . . N1 N 1.3606(8) 0.5425(4) -0.2110(5) 0.037(2) Uani 1 1 d . . . N2 N 0.8894(7) 0.5451(5) -0.0008(6) 0.040(2) Uani 1 1 d . . . N3 N 0.8211(8) 0.5920(5) 0.1085(7) 0.054(3) Uani 1 1 d . . . N4 N 0.7434(8) 0.6054(7) 0.1573(6) 0.064(4) Uani 1 1 d . . . N5 N 0.5577(8) 0.6008(5) 0.1900(6) 0.044(2) Uani 1 1 d . . . N6 N 0.1583(11) 0.7037(7) 0.4370(7) 0.068(4) Uani 1 1 d . . . N7 N 0.2504(10) 0.5744(8) 0.0994(8) 0.063(3) Uani 1 1 d . . . N8 N -0.1372(8) 0.6654(5) 0.3568(6) 0.045(2) Uani 1 1 d . . . N9 N -0.3179(9) 0.6448(7) 0.3931(6) 0.068(4) Uani 1 1 d . . . N10 N -0.3995(8) 0.6530(6) 0.4397(6) 0.058(3) Uani 1 1 d . . . N11 N -0.4764(8) 0.6990(5) 0.5486(6) 0.040(2) Uani 1 1 d . . . N12 N -0.9606(10) 0.6937(6) 0.7403(9) 0.074(4) Uani 1 1 d . . . C1 C 1.3237(9) 0.6008(6) -0.1832(7) 0.161(11) Uiso 1 1 d . . . H27A H 1.3464 0.6400 -0.2034 0.193 Uiso 1 1 calc R . . C2 C 1.2855(9) 0.4971(6) -0.2215(7) 0.052(3) Uani 1 1 d R . . H28A H 1.2940 0.4649 -0.2602 0.062 Uiso 1 1 d R . . C3 C 1.2443(10) 0.5981(7) -0.1182(8) 0.051(3) Uani 1 1 d . . . H25A H 1.2431 0.6285 -0.0759 0.061 Uiso 1 1 calc R . . C4 C 1.1937(10) 0.4939(7) -0.1809(7) 0.044(3) Uani 1 1 d . . . H26A H 1.1468 0.4579 -0.1881 0.053 Uiso 1 1 calc R . . C5 C 1.1710(8) 0.5425(6) -0.1306(6) 0.035(2) Uani 1 1 d . . . C6 C 1.0707(8) 0.5449(7) -0.0869(6) 0.039(3) Uani 1 1 d . . . C7 C 1.0236(8) 0.6019(5) -0.0686(6) 0.029(2) Uani 1 1 d . . . H21A H 1.0531 0.6402 -0.0863 0.035 Uiso 1 1 calc R . . C8 C 1.0229(11) 0.4871(6) -0.0564(9) 0.059(4) Uani 1 1 d . . . H22A H 1.0548 0.4469 -0.0632 0.071 Uiso 1 1 calc R . . C9 C 0.9326(11) 0.6052(6) -0.0243(9) 0.058(4) Uani 1 1 d . . . H19A H 0.9022 0.6445 -0.0109 0.070 Uiso 1 1 calc R . . C10 C 0.9336(10) 0.4921(6) -0.0189(9) 0.054(3) Uani 1 1 d . . . H20A H 0.9003 0.4540 -0.0044 0.065 Uiso 1 1 calc R . . C11 C 0.7974(11) 0.5509(8) 0.0483(8) 0.054(4) Uani 1 1 d . . . C12 C 0.6443(10) 0.5808(7) 0.1366(9) 0.055(3) Uani 1 1 d . . . C13 C 0.6895(9) 0.5220(6) 0.0168(7) 0.040(3) Uani 1 1 d . . . C14 C 0.6042(7) 0.5340(6) 0.0666(6) 0.038(3) Uani 1 1 d . . . C15 C 0.6640(9) 0.4847(5) -0.0522(7) 0.037(3) Uani 1 1 d . . . H16A H 0.7207 0.4749 -0.0834 0.045 Uiso 1 1 calc R . . C16 C 0.4899(9) 0.5154(6) 0.0396(7) 0.041(3) Uani 1 1 d . . . H15A H 0.4345 0.5295 0.0698 0.050 Uiso 1 1 calc R . . C17 C 0.5566(9) 0.4601(6) -0.0791(9) 0.055(3) Uani 1 1 d . . . H18A H 0.5421 0.4337 -0.1260 0.066 Uiso 1 1 calc R . . C18 C 0.4616(12) 0.4789(6) -0.0269(8) 0.054(3) Uani 1 1 d . . . H17A H 0.3882 0.4648 -0.0423 0.064 Uiso 1 1 calc R . . C19 C 0.5310(10) 0.6619(8) 0.1892(9) 0.062(4) Uani 1 1 d . . . H9A H 0.5613 0.6898 0.1534 0.075 Uiso 1 1 calc R . . C20 C 0.5147(12) 0.5557(6) 0.2376(9) 0.056(3) Uani 1 1 d . . . H10A H 0.5326 0.5122 0.2330 0.067 Uiso 1 1 calc R . . C21 C 0.4573(12) 0.6867(7) 0.2413(9) 0.060(4) Uani 1 1 d . . . H7A H 0.4418 0.7306 0.2439 0.072 Uiso 1 1 calc R . . C22 C 0.4444(10) 0.5750(6) 0.2930(8) 0.044(3) Uani 1 1 d . . . H8A H 0.4221 0.5459 0.3312 0.053 Uiso 1 1 calc R . . C23 C 0.4070(9) 0.6393(6) 0.2908(7) 0.042(3) Uani 1 1 d . . . C24 C 0.3209(10) 0.6584(7) 0.3458(8) 0.052(3) Uani 1 1 d . . . C25 C 0.2907(14) 0.7308(7) 0.3412(11) 0.078(5) Uani 1 1 d . . . H3A H 0.3193 0.7613 0.3078 0.094 Uiso 1 1 calc R . . C26 C 0.2763(10) 0.6204(10) 0.3920(8) 0.070(4) Uani 1 1 d . . . H4A H 0.3005 0.5777 0.3960 0.084 Uiso 1 1 calc R . . C27 C 0.2090(15) 0.7435(8) 0.3984(12) 0.088(6) Uani 1 1 d . . . H1A H 0.1931 0.7868 0.4069 0.105 Uiso 1 1 calc R . . C28 C 0.1883(10) 0.6403(7) 0.4399(7) 0.055(4) Uani 1 1 d . . . H2A H 0.1541 0.6107 0.4713 0.065 Uiso 1 1 calc R . . C29 C 0.2273(13) 0.6300(12) 0.1057(11) 0.089(6) Uani 1 1 d . . . H29A H 0.2586 0.6604 0.0736 0.107 Uiso 1 1 calc R . . C30 C 0.1937(14) 0.5264(10) 0.1335(7) 0.079(5) Uani 1 1 d . . . H30A H 0.2112 0.4834 0.1253 0.095 Uiso 1 1 calc R . . C31 C 0.1560(9) 0.6501(12) 0.1586(7) 0.102(9) Uani 1 1 d . . . H31A H 0.1527 0.6941 0.1702 0.123 Uiso 1 1 calc R . . C32 C 0.1077(11) 0.5424(9) 0.1818(9) 0.062(4) Uani 1 1 d . . . H32A H 0.0661 0.5102 0.2029 0.075 Uiso 1 1 calc R . . C33 C 0.0873(12) 0.6079(9) 0.1967(9) 0.071(5) Uani 1 1 d . . . C34 C 0.0057(9) 0.6304(7) 0.2499(7) 0.052(4) Uani 1 1 d . . . C35 C -0.0454(14) 0.6886(8) 0.2468(11) 0.078(5) Uani 1 1 d . . . H35A H -0.0381 0.7170 0.2033 0.093 Uiso 1 1 calc R . . C36 C -0.0316(12) 0.5793(9) 0.3053(8) 0.080(6) Uani 1 1 d . . . H36A H -0.0103 0.5362 0.3021 0.096 Uiso 1 1 calc R . . C37 C -0.1082(12) 0.7062(7) 0.3073(9) 0.062(4) Uani 1 1 d . . . H37A H -0.1294 0.7491 0.3115 0.074 Uiso 1 1 calc R . . C38 C -0.1006(12) 0.6004(7) 0.3623(8) 0.059(4) Uani 1 1 d . . . H38A H -0.1217 0.5727 0.4025 0.071 Uiso 1 1 calc R . . C39 C -0.2210(15) 0.6773(8) 0.4131(10) 0.068(5) Uani 1 1 d . . . C40 C -0.3797(11) 0.6952(7) 0.5040(8) 0.054(3) Uani 1 1 d . . . C41 C -0.1933(15) 0.7132(8) 0.4775(13) 0.086(6) Uani 1 1 d . . . C42 C -0.2775(10) 0.7308(6) 0.5327(8) 0.045(3) Uani 1 1 d . . . C43 C -0.0826(10) 0.7504(7) 0.5085(9) 0.056(4) Uani 1 1 d . . . H44A H -0.0220 0.7443 0.4799 0.067 Uiso 1 1 calc R . . C44 C -0.2491(12) 0.7675(7) 0.6087(7) 0.057(4) Uani 1 1 d . . . H43A H -0.2975 0.7677 0.6485 0.068 Uiso 1 1 calc R . . C45 C -0.0711(10) 0.7877(8) 0.5693(8) 0.062(4) Uani 1 1 d . . . H45A H -0.0025 0.8088 0.5817 0.075 Uiso 1 1 calc R . . C46 C -0.1535(14) 0.8014(8) 0.6223(10) 0.089(6) Uani 1 1 d . . . H46A H -0.1412 0.8324 0.6643 0.106 Uiso 1 1 calc R . . C47 C -0.5151(10) 0.7574(5) 0.5712(7) 0.039(3) Uani 1 1 d . . . H47A H -0.4760 0.7951 0.5632 0.046 Uiso 1 1 calc R . . C48 C -0.5173(9) 0.6408(6) 0.5737(7) 0.044(3) Uani 1 1 d . . . H48A H -0.4802 0.6026 0.5644 0.053 Uiso 1 1 calc R . . C49 C -0.6132(11) 0.7599(5) 0.6061(7) 0.044(3) Uani 1 1 d . . . H49A H -0.6474 0.7993 0.6139 0.053 Uiso 1 1 calc R . . C50 C -0.6107(11) 0.6382(7) 0.6120(7) 0.052(3) Uani 1 1 d . . . H50A H -0.6400 0.5987 0.6255 0.062 Uiso 1 1 calc R . . C51 C -0.6634(11) 0.6979(6) 0.6311(7) 0.046(3) Uani 1 1 d . . . C52 C -0.7628(9) 0.6959(6) 0.6687(7) 0.039(3) Uani 1 1 d . . . C53 C -0.7923(10) 0.7480(6) 0.7222(8) 0.046(3) Uani 1 1 d . . . H53A H -0.7466 0.7843 0.7312 0.056 Uiso 1 1 calc R . . C54 C -0.8386(8) 0.6453(5) 0.6615(7) 0.037(2) Uani 1 1 d . . . H54A H -0.8210 0.6079 0.6342 0.045 Uiso 1 1 calc R . . C55 C -0.8866(11) 0.7437(7) 0.7588(9) 0.058(4) Uani 1 1 d . . . H55A H -0.9010 0.7751 0.7970 0.070 Uiso 1 1 calc R . . C56 C -0.9389(9) 0.6476(5) 0.6926(6) 0.034(2) Uani 1 1 d . . . H56A H -0.9917 0.6151 0.6787 0.041 Uiso 1 1 calc R . . C57 C 0.4517(10) 0.2169(5) 0.1704(6) 0.038(3) Uani 1 1 d . . . C58 C 0.3855(8) 0.1797(5) 0.0902(6) 0.028(2) Uani 1 1 d . . . C59 C 0.3207(14) 0.3378(7) -0.0320(11) 0.064(4) Uani 1 1 d . . . C60 C 0.3778(16) 0.3213(10) -0.1069(9) 0.093(6) Uani 1 1 d . . . C61 C 0.7161(14) 0.3436(7) 0.0682(9) 0.061(4) Uani 1 1 d . . . C62 C 0.7324(10) 0.2711(5) 0.0412(7) 0.035(2) Uani 1 1 d . . . C63 C 0.1999(10) 0.0643(5) 0.3670(7) 0.040(3) Uani 1 1 d . . . C64 C 0.1475(8) 0.0287(5) 0.2884(6) 0.029(2) Uani 1 1 d . . . C65 C -0.1519(14) -0.0268(9) 0.4245(8) 0.070(4) Uani 1 1 d . . . C66 C -0.1220(13) -0.0967(8) 0.4043(9) 0.066(4) Uani 1 1 d . . . C67 C 0.2012(12) -0.0839(8) 0.5717(10) 0.070(5) Uani 1 1 d . . . C68 C 0.2739(12) -0.0938(8) 0.5072(9) 0.068(4) Uani 1 1 d . . . O1W O 0.1655(8) 0.1948(5) 0.2047(7) 0.066(3) Uani 1 1 d . . . O2W O 0.4277(7) 0.0476(5) 0.2638(6) 0.056(2) Uani 1 1 d . . . O3W O 0.1101(8) 0.2758(5) 0.0361(5) 0.058(2) Uani 1 1 d D . . O4W O 0.2256(12) 0.3188(6) 0.1663(9) 0.106(4) Uani 1 1 d D . . O5W O 0.5755(10) 0.4094(6) 0.2269(7) 0.090(4) Uani 1 1 d . . . O6W O -0.766(3) 0.9147(18) 0.730(3) 0.321(17) Uiso 1 1 d . . . O7W O 0.143(4) 0.847(3) 0.124(4) 0.27(3) Uiso 0.50 1 d PD . . O8W O -0.9792(16) 0.9070(10) 0.7560(13) 0.159(7) Uiso 1 1 d . . . O9W O 0.3774(15) 0.3942(9) 0.2634(12) 0.148(6) Uiso 1 1 d . . . O10W O -0.448(4) 0.843(2) 0.336(3) 0.41(2) Uiso 1 1 d . . . O11W O 1.039(3) 0.261(2) -0.053(3) 0.35(2) Uiso 1 1 d . . . O12W O 0.3750(15) -0.0741(9) 0.3132(11) 0.140(6) Uiso 1 1 d . . . O13W O 0.546(3) -0.014(2) 0.489(3) 0.36(2) Uiso 1 1 d . . . O14W O -0.0597(16) 0.8503(9) 0.2161(13) 0.161(7) Uiso 1 1 d D . . O15W O 0.3535(16) 0.8228(10) 0.1919(12) 0.154(6) Uiso 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 Cr1 0.0369(10) 0.0330(9) 0.0358(9) 0.0040(7) 0.0109(7) -0.0023(8) Cr2 0.0515(12) 0.0377(10) 0.0473(10) 0.0114(8) 0.0206(9) 0.0034(9) Mn1 0.0308(8) 0.0466(9) 0.0439(8) 0.0038(6) 0.0131(6) -0.0043(7) O1 0.031(4) 0.081(6) 0.024(4) 0.002(3) 0.010(3) -0.004(4) O2 0.042(4) 0.044(5) 0.041(4) -0.003(3) 0.007(3) -0.011(4) O3 0.054(5) 0.040(5) 0.053(5) 0.004(4) 0.000(4) -0.013(4) O4 0.064(6) 0.041(5) 0.052(5) -0.006(3) 0.031(4) -0.028(4) O5 0.054(5) 0.055(6) 0.056(5) 0.006(4) 0.036(5) 0.010(4) O6 0.061(6) 0.054(5) 0.035(4) 0.009(3) 0.023(4) -0.018(4) O7 0.088(9) 0.088(8) 0.119(10) 0.054(8) -0.004(8) 0.044(7) O8 0.178(19) 0.24(2) 0.130(15) 0.091(15) 0.082(14) 0.020(16) O9 0.052(6) 0.028(4) 0.096(7) -0.005(4) 0.025(5) -0.012(4) O10 0.064(6) 0.063(6) 0.061(6) 0.023(4) 0.036(5) 0.027(5) O11 0.053(6) 0.051(6) 0.087(7) 0.007(5) 0.000(5) -0.019(5) O12 0.070(7) 0.096(9) 0.158(12) 0.003(8) 0.067(8) 0.048(6) O13 0.052(5) 0.064(6) 0.037(4) -0.018(4) 0.015(4) -0.013(5) O14 0.044(5) 0.035(4) 0.047(5) 0.005(3) 0.005(4) -0.014(4) O15 0.090(7) 0.049(5) 0.049(5) -0.003(4) 0.022(5) -0.024(5) O16 0.077(6) 0.056(6) 0.053(5) 0.005(4) 0.029(5) -0.016(5) O17 0.038(5) 0.072(7) 0.062(6) 0.013(5) 0.007(4) 0.011(5) O18 0.059(6) 0.052(6) 0.081(7) 0.021(5) 0.018(5) -0.016(5) O19 0.27(2) 0.158(14) 0.060(7) 0.022(8) -0.001(10) 0.177(15) O20 0.103(10) 0.113(11) 0.117(11) 0.026(8) -0.045(9) -0.050(9) O21 0.071(7) 0.097(8) 0.051(6) 0.004(5) 0.022(5) 0.034(6) O22 0.055(6) 0.044(6) 0.131(10) 0.020(6) 0.030(6) 0.009(5) O23 0.171(14) 0.169(14) 0.047(7) 0.056(8) -0.015(8) 0.052(12) O24 0.125(12) 0.153(14) 0.129(13) 0.022(10) 0.001(10) 0.086(12) N1 0.055(6) 0.024(4) 0.033(5) 0.004(3) 0.012(4) 0.003(4) N2 0.021(4) 0.061(6) 0.041(5) -0.006(4) 0.013(4) -0.003(5) N3 0.040(6) 0.071(8) 0.054(6) -0.022(5) 0.019(5) 0.005(5) N4 0.028(5) 0.134(11) 0.031(5) -0.012(6) 0.011(4) 0.023(6) N5 0.044(6) 0.051(6) 0.036(5) -0.008(4) 0.006(4) -0.004(5) N6 0.062(8) 0.098(10) 0.042(6) -0.027(6) 0.004(5) 0.014(8) N7 0.039(7) 0.087(10) 0.066(8) 0.004(7) 0.017(6) -0.006(7) N8 0.045(6) 0.055(6) 0.037(5) -0.015(4) 0.007(4) -0.010(5) N9 0.049(6) 0.120(11) 0.041(6) -0.008(6) 0.029(5) -0.037(7) N10 0.029(5) 0.118(10) 0.025(5) -0.012(5) 0.005(4) 0.003(6) N11 0.036(5) 0.030(5) 0.057(6) 0.002(4) 0.015(5) -0.001(4) N12 0.060(7) 0.062(8) 0.118(11) -0.022(7) 0.066(7) -0.011(7) C2 0.038(7) 0.068(9) 0.056(8) -0.004(6) 0.028(6) -0.010(6) C3 0.044(7) 0.059(8) 0.048(7) 0.013(6) 0.007(6) -0.005(6) C4 0.032(6) 0.063(8) 0.034(6) 0.009(5) -0.002(5) 0.003(6) C5 0.020(5) 0.054(7) 0.031(5) 0.005(4) 0.007(4) -0.017(5) C6 0.023(5) 0.072(9) 0.021(5) -0.002(5) 0.000(4) -0.005(6) C7 0.032(5) 0.023(5) 0.036(5) 0.004(4) 0.017(4) -0.009(4) C8 0.043(7) 0.046(7) 0.095(10) -0.042(7) 0.033(7) 0.002(6) C9 0.051(8) 0.039(7) 0.086(10) -0.011(6) 0.018(7) -0.018(6) C10 0.032(7) 0.043(7) 0.088(10) -0.009(6) 0.010(7) -0.010(6) C11 0.050(8) 0.081(10) 0.034(6) 0.009(6) 0.014(6) 0.024(7) C12 0.028(6) 0.071(9) 0.069(9) -0.012(7) 0.012(6) 0.007(6) C13 0.032(6) 0.046(6) 0.042(6) 0.014(5) 0.006(5) 0.003(5) C14 0.007(4) 0.073(8) 0.035(5) 0.006(5) 0.006(4) 0.006(5) C15 0.033(6) 0.039(6) 0.038(6) -0.009(4) 0.001(5) -0.009(5) C16 0.026(5) 0.059(7) 0.036(5) -0.002(5) -0.004(4) 0.012(5) C17 0.041(7) 0.053(7) 0.079(9) 0.034(6) 0.036(6) 0.001(6) C18 0.064(9) 0.043(7) 0.062(8) -0.006(5) 0.033(7) 0.016(6) C19 0.027(6) 0.085(11) 0.077(10) 0.018(7) 0.020(6) 0.037(7) C20 0.067(9) 0.033(7) 0.076(9) -0.002(6) 0.038(7) -0.004(6) C21 0.061(9) 0.060(9) 0.059(8) -0.009(6) 0.011(7) -0.016(7) C22 0.038(6) 0.047(7) 0.054(7) -0.003(5) 0.030(6) -0.003(5) C23 0.038(6) 0.043(6) 0.039(6) -0.018(5) -0.012(5) -0.002(5) C24 0.031(6) 0.078(10) 0.049(7) -0.008(6) 0.014(5) -0.002(6) C25 0.085(11) 0.063(10) 0.103(12) 0.000(8) 0.065(10) 0.012(8) C26 0.038(7) 0.128(14) 0.041(7) 0.011(8) 0.001(5) 0.006(9) C27 0.098(13) 0.069(11) 0.113(14) -0.038(10) 0.070(11) -0.016(10) C28 0.032(6) 0.097(11) 0.029(5) -0.006(6) -0.013(5) 0.004(7) C29 0.046(9) 0.144(19) 0.087(12) -0.029(12) 0.041(8) -0.047(11) C30 0.094(12) 0.120(14) 0.024(6) -0.017(7) 0.011(7) 0.031(11) C31 0.018(6) 0.27(3) 0.021(6) 0.038(10) -0.001(5) -0.014(10) C32 0.032(7) 0.094(12) 0.059(8) 0.006(8) -0.001(6) 0.003(8) C33 0.059(9) 0.104(13) 0.053(8) 0.044(8) 0.023(7) 0.029(9) C34 0.032(6) 0.086(10) 0.045(6) 0.027(6) 0.022(5) 0.025(7) C35 0.079(11) 0.079(11) 0.084(11) 0.012(8) 0.040(9) -0.002(9) C36 0.061(9) 0.156(16) 0.033(7) 0.034(8) 0.034(6) 0.050(10) C37 0.059(8) 0.070(9) 0.065(9) 0.021(7) 0.036(7) 0.007(7) C38 0.066(9) 0.065(9) 0.051(7) 0.004(6) 0.026(7) 0.018(7) C39 0.093(12) 0.064(9) 0.064(9) 0.031(7) 0.070(9) 0.040(9) C40 0.055(8) 0.071(9) 0.043(6) -0.015(6) 0.027(6) -0.040(7) C41 0.106(14) 0.050(9) 0.121(15) 0.029(9) 0.082(12) -0.013(9) C42 0.032(6) 0.055(7) 0.048(7) 0.013(5) 0.006(5) 0.016(5) C43 0.035(7) 0.078(10) 0.059(8) 0.016(7) 0.026(6) 0.005(7) C44 0.075(9) 0.064(9) 0.029(6) 0.005(5) -0.001(6) -0.023(7) C45 0.021(6) 0.112(12) 0.057(7) -0.045(8) 0.016(5) -0.007(7) C46 0.086(12) 0.076(11) 0.082(11) -0.010(8) -0.060(10) -0.010(9) C47 0.048(7) 0.031(5) 0.045(6) 0.012(4) 0.031(5) 0.004(5) C48 0.039(6) 0.054(7) 0.040(6) -0.019(5) 0.008(5) 0.002(6) C49 0.051(7) 0.033(6) 0.046(6) -0.021(5) 0.002(6) -0.011(5) C50 0.059(8) 0.059(8) 0.038(6) -0.005(5) 0.013(6) 0.000(7) C51 0.069(8) 0.039(6) 0.037(6) 0.016(4) 0.029(6) 0.020(6) C52 0.030(6) 0.039(6) 0.045(6) -0.006(5) -0.002(5) 0.004(5) C53 0.036(6) 0.039(6) 0.067(8) -0.008(5) 0.020(6) -0.001(5) C54 0.029(6) 0.038(6) 0.047(6) -0.009(4) 0.015(5) -0.007(5) C55 0.056(8) 0.063(9) 0.061(8) 0.003(6) 0.027(7) 0.021(7) C56 0.038(6) 0.032(5) 0.037(5) -0.002(4) 0.019(4) -0.002(4) C57 0.048(7) 0.036(6) 0.030(5) -0.007(4) 0.006(5) -0.018(5) C58 0.019(5) 0.035(6) 0.031(5) 0.010(4) 0.002(4) 0.006(4) C59 0.071(10) 0.042(8) 0.085(11) 0.013(7) 0.027(9) 0.008(7) C60 0.098(14) 0.129(16) 0.039(8) 0.033(9) -0.029(9) 0.016(12) C61 0.069(10) 0.047(8) 0.065(9) 0.022(6) 0.008(8) -0.008(7) C62 0.047(6) 0.013(5) 0.050(6) -0.003(4) 0.023(5) -0.001(5) C63 0.037(6) 0.038(6) 0.046(6) -0.001(5) 0.007(5) 0.016(5) C64 0.019(5) 0.027(5) 0.036(5) 0.004(4) -0.016(4) 0.009(4) C65 0.069(10) 0.106(14) 0.036(7) 0.012(7) 0.006(7) -0.008(10) C66 0.055(9) 0.082(11) 0.061(9) 0.036(8) 0.012(7) 0.009(9) C67 0.052(9) 0.076(10) 0.081(10) 0.059(8) 0.010(7) 0.025(7) C68 0.052(8) 0.099(12) 0.053(8) 0.042(8) 0.010(7) 0.034(8) O1W 0.048(6) 0.053(6) 0.099(8) 0.009(5) 0.024(5) 0.004(5) O2W 0.044(5) 0.066(6) 0.062(6) -0.004(5) 0.016(4) -0.013(5) O3W 0.076(6) 0.062(5) 0.035(4) 0.001(4) 0.009(4) -0.002(5) O4W 0.124(11) 0.075(8) 0.139(11) 0.034(7) 0.083(9) 0.005(7) O5W 0.101(9) 0.091(9) 0.078(7) -0.027(6) 0.010(6) 0.017(7) _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 Cr1 O10 1.964(9) . ? Cr1 O9 1.968(8) . ? Cr1 O5 1.982(9) . ? Cr1 O3 1.990(8) . ? Cr1 O6 2.004(8) . ? Cr1 O4 2.020(8) . ? Cr2 O21 1.915(9) . ? Cr2 O17 1.960(9) . ? Cr2 O22 1.968(10) . ? Cr2 O15 2.004(9) . ? Cr2 O18 2.008(9) . ? Cr2 O16 2.015(9) . ? Mn1 O2 2.187(8) . ? Mn1 O1W 2.196(10) . ? Mn1 O2W 2.199(10) . ? Mn1 O14 2.203(7) . ? Mn1 O1 2.208(9) . ? Mn1 O13 2.218(8) . ? O1 C57 1.255(13) . ? O2 C58 1.211(12) . ? O3 C57 1.176(12) . ? O4 C58 1.300(12) . ? O5 C59 1.168(18) . ? O6 C60 1.278(19) . ? O7 C59 1.355(19) . ? O8 C60 1.21(2) . ? O9 C61 1.285(17) . ? O10 C62 1.213(14) . ? O11 C61 1.181(16) . ? O12 C62 1.376(15) . ? O13 C63 1.266(14) . ? O14 C64 1.193(12) . ? O15 C63 1.277(15) . ? O16 C64 1.345(13) . ? O17 C65 1.285(18) . ? O18 C66 1.299(17) . ? O19 C65 1.42(2) . ? O20 C66 1.291(19) . ? O21 C67 1.416(15) . ? O22 C68 1.366(16) . ? O23 C67 1.196(16) . ? O23 O6W 1.40(4) 1_645 ? O24 C68 1.252(18) . ? N1 C2 1.299(14) . ? N1 C1 1.382(15) . ? N2 C10 1.271(16) . ? N2 C9 1.420(16) . ? N2 C11 1.462(15) . ? N3 C11 1.291(17) . ? N3 N4 1.342(13) . ? N4 C12 1.296(16) . ? N5 C19 1.305(17) . ? N5 C20 1.360(15) . ? N5 C12 1.508(16) . ? N6 C27 1.25(2) . ? N6 C28 1.360(18) . ? N7 C29 1.19(2) . ? N7 C30 1.37(2) . ? N8 C37 1.247(16) . ? N8 C38 1.413(17) . ? N8 C39 1.478(15) . ? N9 N10 1.337(14) . ? N9 C39 1.35(2) . ? N10 C40 1.351(15) . ? N11 C47 1.365(14) . ? N11 C48 1.384(15) . ? N11 C40 1.461(15) . ? N12 C56 1.276(15) . ? N12 C55 1.370(18) . ? C1 C3 1.524(16) . ? C1 H27A 0.9300 . ? C2 C4 1.370(16) . ? C2 H28A 0.9299 . ? C3 C5 1.447(16) . ? C3 H25A 0.9300 . ? C4 C5 1.347(17) . ? C4 H26A 0.9300 . ? C5 C6 1.488(14) . ? C6 C7 1.360(16) . ? C6 C8 1.446(19) . ? C7 C9 1.398(17) . ? C7 H21A 0.9300 . ? C8 C10 1.317(18) . ? C8 H22A 0.9300 . ? C9 H19A 0.9300 . ? C10 H20A 0.9300 . ? C11 C13 1.453(18) . ? C12 C14 1.513(18) . ? C13 C15 1.353(15) . ? C13 C14 1.419(15) . ? C14 C16 1.436(14) . ? C15 C17 1.399(16) . ? C15 H16A 0.9300 . ? C16 C18 1.315(16) . ? C16 H15A 0.9300 . ? C17 C18 1.569(17) . ? C17 H18A 0.9300 . ? C18 H17A 0.9300 . ? C19 C21 1.408(19) . ? C19 H9A 0.9300 . ? C20 C22 1.380(17) . ? C20 H10A 0.9300 . ? C21 C23 1.454(19) . ? C21 H7A 0.9300 . ? C22 C23 1.402(16) . ? C22 H8A 0.9300 . ? C23 C24 1.516(18) . ? C24 C26 1.26(2) . ? C24 C25 1.54(2) . ? C25 C27 1.47(2) . ? C25 H3A 0.9300 . ? C26 C28 1.462(19) . ? C26 H4A 0.9300 . ? C27 H1A 0.9300 . ? C28 H2A 0.9300 . ? C29 C31 1.37(2) . ? C29 H29A 0.9300 . ? C30 C32 1.425(19) . ? C30 H30A 0.9300 . ? C31 C33 1.41(2) . ? C31 H31A 0.9300 . ? C32 C33 1.40(2) . ? C32 H32A 0.9300 . ? C33 C34 1.474(18) . ? C34 C35 1.35(2) . ? C34 C36 1.497(18) . ? C35 C37 1.37(2) . ? C35 H35A 0.9300 . ? C36 C38 1.401(17) . ? C36 H36A 0.9300 . ? C37 H37A 0.9300 . ? C38 H38A 0.9300 . ? C39 C41 1.28(2) . ? C40 C42 1.450(17) . ? C41 C42 1.49(2) . ? C41 C43 1.56(2) . ? C42 C44 1.441(17) . ? C43 C45 1.242(18) . ? C43 H44A 0.9300 . ? C44 C46 1.339(19) . ? C44 H43A 0.9300 . ? C45 C46 1.43(2) . ? C45 H45A 0.9300 . ? C46 H46A 0.9300 . ? C47 C49 1.386(17) . ? C47 H47A 0.9300 . ? C48 C50 1.365(17) . ? C48 H48A 0.9300 . ? C49 C51 1.499(17) . ? C49 H49A 0.9300 . ? C50 C51 1.441(17) . ? C50 H50A 0.9300 . ? C51 C52 1.423(16) . ? C52 C54 1.383(15) . ? C52 C53 1.459(16) . ? C53 C55 1.361(17) . ? C53 H53A 0.9300 . ? C54 C56 1.379(14) . ? C54 H54A 0.9300 . ? C55 H55A 0.9300 . ? C56 H56A 0.9300 . ? C57 C58 1.614(13) . ? C59 C60 1.52(2) . ? C61 C62 1.582(17) . ? C63 C64 1.522(14) . ? C65 C66 1.54(2) . ? C67 C68 1.47(2) . ? 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 O10 Cr1 O9 82.3(4) . . ? O10 Cr1 O5 175.1(4) . . ? O9 Cr1 O5 96.0(4) . . ? O10 Cr1 O3 93.1(4) . . ? O9 Cr1 O3 91.2(4) . . ? O5 Cr1 O3 91.5(4) . . ? O10 Cr1 O6 94.7(4) . . ? O9 Cr1 O6 97.1(4) . . ? O5 Cr1 O6 81.0(4) . . ? O3 Cr1 O6 169.3(4) . . ? O10 Cr1 O4 94.4(4) . . ? O9 Cr1 O4 173.3(4) . . ? O5 Cr1 O4 87.6(4) . . ? O3 Cr1 O4 83.1(3) . . ? O6 Cr1 O4 89.0(3) . . ? O21 Cr2 O17 90.9(4) . . ? O21 Cr2 O22 86.3(5) . . ? O17 Cr2 O22 175.7(4) . . ? O21 Cr2 O15 94.6(4) . . ? O17 Cr2 O15 93.7(4) . . ? O22 Cr2 O15 89.7(4) . . ? O21 Cr2 O18 95.5(5) . . ? O17 Cr2 O18 82.2(4) . . ? O22 Cr2 O18 94.9(4) . . ? O15 Cr2 O18 169.1(4) . . ? O21 Cr2 O16 173.5(4) . . ? O17 Cr2 O16 95.1(4) . . ? O22 Cr2 O16 87.9(5) . . ? O15 Cr2 O16 82.4(4) . . ? O18 Cr2 O16 87.9(4) . . ? O2 Mn1 O1W 86.5(4) . . ? O2 Mn1 O2W 97.5(3) . . ? O1W Mn1 O2W 175.4(4) . . ? O2 Mn1 O14 104.5(3) . . ? O1W Mn1 O14 92.2(3) . . ? O2W Mn1 O14 88.9(3) . . ? O2 Mn1 O1 75.7(3) . . ? O1W Mn1 O1 88.7(4) . . ? O2W Mn1 O1 90.2(3) . . ? O14 Mn1 O1 179.1(4) . . ? O2 Mn1 O13 176.6(4) . . ? O1W Mn1 O13 90.8(4) . . ? O2W Mn1 O13 85.1(4) . . ? O14 Mn1 O13 77.7(3) . . ? O1 Mn1 O13 102.1(3) . . ? C57 O1 Mn1 117.1(7) . . ? C58 O2 Mn1 114.5(6) . . ? C57 O3 Cr1 114.2(7) . . ? C58 O4 Cr1 110.9(7) . . ? C59 O5 Cr1 113.5(10) . . ? C60 O6 Cr1 112.3(9) . . ? C61 O9 Cr1 116.9(9) . . ? C62 O10 Cr1 112.8(8) . . ? C63 O13 Mn1 109.5(7) . . ? C64 O14 Mn1 111.4(7) . . ? C63 O15 Cr2 112.7(8) . . ? C64 O16 Cr2 112.2(7) . . ? C65 O17 Cr2 118.2(11) . . ? C66 O18 Cr2 109.9(11) . . ? C67 O21 Cr2 110.8(8) . . ? C68 O22 Cr2 111.4(10) . . ? C67 O23 O6W 152(2) . 1_645 ? C2 N1 C1 114.9(10) . . ? C10 N2 C9 120.7(10) . . ? C10 N2 C11 124.9(11) . . ? C9 N2 C11 114.3(11) . . ? C11 N3 N4 119.0(11) . . ? C12 N4 N3 117.6(11) . . ? C19 N5 C20 123.8(12) . . ? C19 N5 C12 116.9(11) . . ? C20 N5 C12 119.4(11) . . ? C27 N6 C28 120.5(14) . . ? C29 N7 C30 122.0(15) . . ? C37 N8 C38 124.7(12) . . ? C37 N8 C39 124.4(12) . . ? C38 N8 C39 110.8(11) . . ? N10 N9 C39 119.1(11) . . ? N9 N10 C40 117.1(10) . . ? C47 N11 C48 122.8(9) . . ? C47 N11 C40 120.5(10) . . ? C48 N11 C40 116.3(10) . . ? C56 N12 C55 120.7(11) . . ? N1 C1 C3 117.3(10) . . ? N1 C1 H27A 121.4 . . ? C3 C1 H27A 121.4 . . ? N1 C2 C4 124.8(12) . . ? N1 C2 H28A 117.4 . . ? C4 C2 H28A 117.8 . . ? C5 C3 C1 111.5(11) . . ? C5 C3 H25A 124.2 . . ? C1 C3 H25A 124.2 . . ? C5 C4 C2 120.2(12) . . ? C5 C4 H26A 119.9 . . ? C2 C4 H26A 119.9 . . ? C4 C5 C3 120.2(11) . . ? C4 C5 C6 124.3(10) . . ? C3 C5 C6 115.5(11) . . ? C7 C6 C8 116.2(9) . . ? C7 C6 C5 121.8(11) . . ? C8 C6 C5 121.8(11) . . ? C6 C7 C9 122.6(10) . . ? C6 C7 H21A 118.7 . . ? C9 C7 H21A 118.7 . . ? C10 C8 C6 119.1(11) . . ? C10 C8 H22A 120.5 . . ? C6 C8 H22A 120.5 . . ? C7 C9 N2 116.1(11) . . ? C7 C9 H19A 121.9 . . ? N2 C9 H19A 121.9 . . ? N2 C10 C8 125.0(13) . . ? N2 C10 H20A 117.5 . . ? C8 C10 H20A 117.5 . . ? N3 C11 C13 128.4(12) . . ? N3 C11 N2 111.2(12) . . ? C13 C11 N2 119.3(11) . . ? N4 C12 N5 115.8(11) . . ? N4 C12 C14 128.7(11) . . ? N5 C12 C14 115.6(10) . . ? C15 C13 C14 118.1(10) . . ? C15 C13 C11 127.3(11) . . ? C14 C13 C11 114.6(10) . . ? C13 C14 C16 121.7(10) . . ? C13 C14 C12 111.0(9) . . ? C16 C14 C12 125.8(10) . . ? C13 C15 C17 123.4(12) . . ? C13 C15 H16A 118.3 . . ? C17 C15 H16A 118.3 . . ? C18 C16 C14 121.5(11) . . ? C18 C16 H15A 119.2 . . ? C14 C16 H15A 119.2 . . ? C15 C17 C18 117.3(13) . . ? C15 C17 H18A 121.3 . . ? C18 C17 H18A 121.3 . . ? C16 C18 C17 117.4(13) . . ? C16 C18 H17A 121.3 . . ? C17 C18 H17A 121.3 . . ? N5 C19 C21 121.6(14) . . ? N5 C19 H9A 119.2 . . ? C21 C19 H9A 119.2 . . ? N5 C20 C22 119.4(11) . . ? N5 C20 H10A 120.3 . . ? C22 C20 H10A 120.3 . . ? C19 C21 C23 115.8(13) . . ? C19 C21 H7A 122.1 . . ? C23 C21 H7A 122.1 . . ? C20 C22 C23 119.0(12) . . ? C20 C22 H8A 120.5 . . ? C23 C22 H8A 120.5 . . ? C22 C23 C21 119.7(12) . . ? C22 C23 C24 118.6(12) . . ? C21 C23 C24 121.6(11) . . ? C26 C24 C23 125.2(15) . . ? C26 C24 C25 121.1(14) . . ? C23 C24 C25 113.8(12) . . ? C27 C25 C24 108.6(14) . . ? C27 C25 H3A 125.7 . . ? C24 C25 H3A 125.7 . . ? C24 C26 C28 123.1(18) . . ? C24 C26 H4A 118.4 . . ? C28 C26 H4A 118.4 . . ? N6 C27 C25 128.3(15) . . ? N6 C27 H1A 115.9 . . ? C25 C27 H1A 115.9 . . ? N6 C28 C26 117.6(14) . . ? N6 C28 H2A 121.2 . . ? C26 C28 H2A 121.2 . . ? N7 C29 C31 121.7(19) . . ? N7 C29 H29A 119.2 . . ? C31 C29 H29A 119.2 . . ? N7 C30 C32 120.0(16) . . ? N7 C30 H30A 120.0 . . ? C32 C30 H30A 120.0 . . ? C29 C31 C33 123(2) . . ? C29 C31 H31A 118.3 . . ? C33 C31 H31A 118.3 . . ? C33 C32 C30 118.6(16) . . ? C33 C32 H32A 120.7 . . ? C30 C32 H32A 120.7 . . ? C32 C33 C31 113.2(16) . . ? C32 C33 C34 123.6(14) . . ? C31 C33 C34 123.1(17) . . ? C35 C34 C33 126.9(12) . . ? C35 C34 C36 118.4(12) . . ? C33 C34 C36 114.3(12) . . ? C34 C35 C37 120.5(14) . . ? C34 C35 H35A 119.8 . . ? C37 C35 H35A 119.8 . . ? C38 C36 C34 115.7(15) . . ? C38 C36 H36A 122.2 . . ? C34 C36 H36A 122.2 . . ? N8 C37 C35 121.0(15) . . ? N8 C37 H37A 119.5 . . ? C35 C37 H37A 119.5 . . ? C36 C38 N8 117.8(13) . . ? C36 C38 H38A 121.1 . . ? N8 C38 H38A 121.1 . . ? C41 C39 N9 126.7(13) . . ? C41 C39 N8 118.5(17) . . ? N9 C39 N8 114.7(14) . . ? N10 C40 C42 128.1(11) . . ? N10 C40 N11 110.5(9) . . ? C42 C40 N11 121.3(10) . . ? C39 C41 C42 120.5(16) . . ? C39 C41 C43 130.9(15) . . ? C42 C41 C43 108.3(14) . . ? C44 C42 C40 128.5(11) . . ? C44 C42 C41 122.7(13) . . ? C40 C42 C41 107.9(12) . . ? C45 C43 C41 123.5(13) . . ? C45 C43 H44A 118.3 . . ? C41 C43 H44A 118.3 . . ? C46 C44 C42 120.4(14) . . ? C46 C44 H43A 119.8 . . ? C42 C44 H43A 119.8 . . ? C43 C45 C46 126.1(13) . . ? C43 C45 H45A 116.9 . . ? C46 C45 H45A 116.9 . . ? C44 C46 C45 117.1(14) . . ? C44 C46 H46A 121.5 . . ? C45 C46 H46A 121.5 . . ? N11 C47 C49 119.2(10) . . ? N11 C47 H47A 120.4 . . ? C49 C47 H47A 120.4 . . ? C50 C48 N11 121.4(11) . . ? C50 C48 H48A 119.3 . . ? N11 C48 H48A 119.3 . . ? C47 C49 C51 118.8(10) . . ? C47 C49 H49A 120.6 . . ? C51 C49 H49A 120.6 . . ? C48 C50 C51 118.9(12) . . ? C48 C50 H50A 120.5 . . ? C51 C50 H50A 120.5 . . ? C52 C51 C50 119.5(11) . . ? C52 C51 C49 122.6(10) . . ? C50 C51 C49 117.8(11) . . ? C54 C52 C51 125.0(11) . . ? C54 C52 C53 113.2(10) . . ? C51 C52 C53 121.8(11) . . ? C55 C53 C52 120.1(12) . . ? C55 C53 H53A 120.0 . . ? C52 C53 H53A 120.0 . . ? C56 C54 C52 123.2(10) . . ? C56 C54 H54A 118.4 . . ? C52 C54 H54A 118.4 . . ? C53 C55 N12 121.0(12) . . ? C53 C55 H55A 119.5 . . ? N12 C55 H55A 119.5 . . ? N12 C56 C54 121.1(11) . . ? N12 C56 H56A 119.5 . . ? C54 C56 H56A 119.5 . . ? O3 C57 O1 130.6(10) . . ? O3 C57 C58 117.3(9) . . ? O1 C57 C58 112.0(9) . . ? O2 C58 O4 126.8(10) . . ? O2 C58 C57 120.1(8) . . ? O4 C58 C57 112.6(9) . . ? O5 C59 O7 127.2(15) . . ? O5 C59 C60 119.3(14) . . ? O7 C59 C60 112.7(15) . . ? O8 C60 O6 120(2) . . ? O8 C60 C59 126.5(19) . . ? O6 C60 C59 112.8(12) . . ? O11 C61 O9 130.2(14) . . ? O11 C61 C62 121.7(14) . . ? O9 C61 C62 108.1(12) . . ? O10 C62 O12 126.5(10) . . ? O10 C62 C61 119.5(11) . . ? O12 C62 C61 113.5(11) . . ? O13 C63 O15 123.1(11) . . ? O13 C63 C64 119.4(10) . . ? O15 C63 C64 117.3(11) . . ? O14 C64 O16 124.6(9) . . ? O14 C64 C63 121.8(10) . . ? O16 C64 C63 113.5(9) . . ? O17 C65 O19 136.4(19) . . ? O17 C65 C66 109.3(14) . . ? O19 C65 C66 114.3(15) . . ? O20 C66 O18 123.7(17) . . ? O20 C66 C65 115.8(15) . . ? O18 C66 C65 119.8(15) . . ? O23 C67 O21 120.3(16) . . ? O23 C67 C68 124.0(14) . . ? O21 C67 C68 115.5(11) . . ? O24 C68 O22 120.0(14) . . ? O24 C68 C67 126.2(13) . . ? O22 C68 C67 113.8(11) . . ? _diffrn_measured_fraction_theta_max 0.901 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.901 _refine_diff_density_max 0.776 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.084 data_s_4 _database_code_depnum_ccdc_archive 'CCDC 265933' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H69 Co Cr2 N12 O38.50' _chemical_formula_weight 1833.28 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' Cr Cr 0.3209 0.6236 '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 monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.0013(12) _cell_length_b 20.4966(18) _cell_length_c 16.0309(15) _cell_angle_alpha 90.00 _cell_angle_beta 98.605(5) _cell_angle_gamma 90.00 _cell_volume 3899.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8974 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour Indigo _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 0.589 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.932 _exptl_absorpt_correction_T_max 0.954 _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 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30528 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0665 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.48 _reflns_number_total 17239 _reflns_number_gt 13045 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0954P)^2^+0.6062P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.045(18) _refine_ls_number_reflns 17239 _refine_ls_number_parameters 1081 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0963 _refine_ls_R_factor_gt 0.0712 _refine_ls_wR_factor_ref 0.1906 _refine_ls_wR_factor_gt 0.1722 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.007 _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 Cr1 Cr 0.49386(8) 0.72193(4) 0.96036(6) 0.0422(2) Uani 1 1 d . . . Cr2 Cr 0.91663(8) 1.03391(4) 0.57675(6) 0.0455(2) Uani 1 1 d . . . Co1 Co 0.70460(6) 0.87918(4) 0.76995(5) 0.03740(15) Uani 1 1 d . . . O1 O 0.5841(3) 0.80478(18) 0.7572(2) 0.0417(9) Uani 1 1 d . . . O2 O 0.6789(3) 0.86842(18) 0.8965(2) 0.0427(8) Uani 1 1 d . . . O3 O 0.4891(3) 0.74263(17) 0.8378(2) 0.0431(9) Uani 1 1 d . . . O4 O 0.5870(3) 0.80351(19) 0.9749(2) 0.0467(9) Uani 1 1 d . . . O5 O 0.6356(4) 0.6731(2) 0.9590(3) 0.0547(10) Uani 1 1 d . . . O6 O 0.5264(4) 0.70474(19) 1.0823(3) 0.0544(10) Uani 1 1 d . . . O7 O 0.7873(5) 0.6423(3) 1.0481(4) 0.0974(19) Uani 1 1 d . . . O8 O 0.6659(7) 0.6718(4) 1.1794(4) 0.117(2) Uani 1 1 d . . . O9 O 0.3919(4) 0.64754(18) 0.9322(3) 0.0484(9) Uani 1 1 d . . . O10 O 0.3543(4) 0.76764(19) 0.9708(3) 0.0532(10) Uani 1 1 d . . . O11 O 0.2079(4) 0.6221(2) 0.9153(4) 0.0728(14) Uani 1 1 d . . . O12 O 0.1683(4) 0.7499(3) 0.9622(4) 0.0760(14) Uani 1 1 d . . . O13 O 0.7315(3) 0.88826(18) 0.6430(2) 0.0403(8) Uani 1 1 d . . . O14 O 0.8263(3) 0.95481(19) 0.7816(2) 0.0421(9) Uani 1 1 d . . . O15 O 0.8273(3) 0.95086(19) 0.5641(2) 0.0449(9) Uani 1 1 d . . . O16 O 0.9166(3) 1.01679(19) 0.6990(3) 0.0496(10) Uani 1 1 d . . . O17 O 1.0585(4) 0.9898(2) 0.5702(3) 0.0584(11) Uani 1 1 d . . . O18 O 1.0146(4) 1.1091(2) 0.6016(3) 0.0595(11) Uani 1 1 d . . . O19 O 1.2389(5) 1.0100(3) 0.5684(4) 0.0949(18) Uani 1 1 d . . . O20 O 1.1943(5) 1.1375(3) 0.6231(4) 0.0909(18) Uani 1 1 d . . . O21 O 0.8914(4) 1.0499(2) 0.4551(3) 0.0603(12) Uani 1 1 d . . . O22 O 0.7735(4) 1.0813(2) 0.5713(3) 0.0583(11) Uani 1 1 d . . . O23 O 0.7682(6) 1.0973(4) 0.3552(4) 0.114(2) Uani 1 1 d . . . O24 O 0.6237(5) 1.1086(3) 0.4761(5) 0.110(2) Uani 1 1 d . . . N1 N -0.3635(4) 0.4538(3) 1.2092(3) 0.0484(12) Uani 1 1 d . . . N2 N 0.1126(4) 0.4537(2) 1.0048(3) 0.0406(10) Uani 1 1 d . . . N3 N 0.1821(4) 0.4103(3) 0.8912(3) 0.0532(13) Uani 1 1 d . . . N4 N 0.2621(4) 0.3965(3) 0.8429(3) 0.0575(14) Uani 1 1 d . . . N5 N 0.4410(4) 0.4022(2) 0.8097(3) 0.0446(11) Uani 1 1 d . . . N6 N 0.8444(5) 0.2972(4) 0.5614(4) 0.0768(19) Uani 1 1 d . . . N7 N 0.7481(5) 0.4293(4) 0.9028(4) 0.078(2) Uani 1 1 d . . . N8 N 1.1406(4) 0.3379(3) 0.6422(3) 0.0511(12) Uani 1 1 d . . . N9 N 1.3168(4) 0.3523(3) 0.6072(3) 0.0632(15) Uani 1 1 d . . . N10 N 1.3993(4) 0.3429(3) 0.5570(3) 0.0584(14) Uani 1 1 d . . . N11 N 1.4721(4) 0.3002(2) 0.4475(3) 0.0419(11) Uani 1 1 d . . . N12 N 1.9615(4) 0.3065(3) 0.2561(3) 0.0526(13) Uani 1 1 d . . . C1 C -0.3399(3) 0.4054(2) 1.1585(3) 0.0474(13) Uani 1 1 d . . . H27A H -0.3894 0.3703 1.1503 0.057 Uiso 1 1 calc R . . C2 C -0.2908(3) 0.5029(2) 1.2203(3) 0.0466(13) Uani 1 1 d R . . H28A H -0.3055 0.5369 1.2555 0.056 Uiso 1 1 d R . . C3 C -0.2461(5) 0.4047(3) 1.1176(4) 0.0443(13) Uani 1 1 d . . . H25A H -0.2336 0.3704 1.0823 0.053 Uiso 1 1 calc R . . C4 C -0.1950(5) 0.5061(3) 1.1826(3) 0.0408(12) Uani 1 1 d . . . H26A H -0.1467 0.5417 1.1923 0.049 Uiso 1 1 calc R . . C5 C -0.1718(4) 0.4563(3) 1.1306(3) 0.0396(11) Uani 1 1 d . . . C6 C -0.0725(4) 0.4564(3) 1.0872(3) 0.0363(11) Uani 1 1 d . . . C7 C -0.0215(4) 0.3979(2) 1.0682(3) 0.0384(11) Uani 1 1 d . . . H21A H -0.0511 0.3585 1.0838 0.046 Uiso 1 1 calc R . . C8 C -0.0236(4) 0.5143(3) 1.0618(4) 0.0426(12) Uani 1 1 d . . . H22A H -0.0538 0.5545 1.0732 0.051 Uiso 1 1 calc R . . C9 C 0.0699(4) 0.3970(3) 1.0276(3) 0.0393(11) Uani 1 1 d . . . H19A H 0.1026 0.3576 1.0157 0.047 Uiso 1 1 calc R . . C10 C 0.0673(5) 0.5115(3) 1.0207(4) 0.0446(12) Uani 1 1 d . . . H20A H 0.0984 0.5499 1.0034 0.054 Uiso 1 1 calc R . . C11 C 0.2072(4) 0.4485(3) 0.9559(3) 0.0414(12) Uani 1 1 d . . . C12 C 0.3619(5) 0.4231(3) 0.8648(4) 0.0472(13) Uani 1 1 d . . . C13 C 0.3113(4) 0.4793(2) 0.9838(3) 0.0370(11) Uani 1 1 d . . . C14 C 0.3962(4) 0.4638(3) 0.9342(3) 0.0392(11) Uani 1 1 d . . . C15 C 0.3384(5) 0.5176(3) 1.0568(3) 0.0409(12) Uani 1 1 d . . . H16A H 0.2838 0.5283 1.0900 0.049 Uiso 1 1 calc R . . C16 C 0.5071(5) 0.4867(3) 0.9587(4) 0.0485(14) Uani 1 1 d . . . H15A H 0.5641 0.4763 0.9275 0.058 Uiso 1 1 calc R . . C17 C 0.4471(5) 0.5386(3) 1.0776(4) 0.0454(12) Uani 1 1 d . . . H18A H 0.4665 0.5634 1.1261 0.055 Uiso 1 1 calc R . . C18 C 0.5283(5) 0.5240(3) 1.0288(4) 0.0489(14) Uani 1 1 d . . . H17A H 0.6006 0.5405 1.0444 0.059 Uiso 1 1 calc R . . C19 C 0.4684(6) 0.3389(3) 0.8081(5) 0.0629(18) Uani 1 1 d . . . H9A H 0.4365 0.3093 0.8417 0.076 Uiso 1 1 calc R . . C20 C 0.4859(6) 0.4448(3) 0.7616(4) 0.0608(17) Uani 1 1 d . . . H10A H 0.4672 0.4888 0.7634 0.073 Uiso 1 1 calc R . . C21 C 0.5433(6) 0.3172(4) 0.7571(5) 0.067(2) Uani 1 1 d . . . H7A H 0.5619 0.2732 0.7571 0.080 Uiso 1 1 calc R . . C22 C 0.5601(6) 0.4240(3) 0.7090(4) 0.0572(17) Uani 1 1 d . . . H8A H 0.5899 0.4539 0.6748 0.069 Uiso 1 1 calc R . . C23 C 0.5903(5) 0.3591(3) 0.7069(3) 0.0452(13) Uani 1 1 d . . . C24 C 0.6753(5) 0.3377(4) 0.6549(4) 0.0519(15) Uani 1 1 d . . . C25 C 0.7069(7) 0.2737(4) 0.6530(5) 0.077(2) Uani 1 1 d . . . H3A H 0.6727 0.2423 0.6824 0.092 Uiso 1 1 calc R . . C26 C 0.7277(5) 0.3812(4) 0.6069(4) 0.0600(16) Uani 1 1 d . . . H4A H 0.7074 0.4250 0.6044 0.072 Uiso 1 1 calc R . . C27 C 0.7928(7) 0.2561(4) 0.6053(6) 0.083(2) Uani 1 1 d . . . H1A H 0.8139 0.2125 0.6052 0.100 Uiso 1 1 calc R . . C28 C 0.8116(6) 0.3581(5) 0.5621(4) 0.076(2) Uani 1 1 d . . . H2A H 0.8463 0.3881 0.5309 0.092 Uiso 1 1 calc R . . C29 C 0.7732(5) 0.3678(5) 0.8929(4) 0.071(2) Uani 1 1 d . . . H29A H 0.7347 0.3364 0.9192 0.085 Uiso 1 1 calc R . . C30 C 0.8059(7) 0.4728(5) 0.8660(5) 0.080(2) Uani 1 1 d . . . H30A H 0.7908 0.5167 0.8736 0.096 Uiso 1 1 calc R . . C31 C 0.8527(6) 0.3474(4) 0.8461(4) 0.0635(18) Uani 1 1 d . . . H31A H 0.8675 0.3031 0.8418 0.076 Uiso 1 1 calc R . . C32 C 0.8872(6) 0.4571(5) 0.8169(5) 0.075(2) Uani 1 1 d . . . H32A H 0.9253 0.4896 0.7921 0.090 Uiso 1 1 calc R . . C33 C 0.9110(5) 0.3920(4) 0.8052(4) 0.0547(16) Uani 1 1 d . . . C34 C 0.9945(5) 0.3727(4) 0.7495(3) 0.0513(14) Uani 1 1 d . . . C35 C 1.0390(6) 0.3114(4) 0.7511(4) 0.0636(18) Uani 1 1 d . . . H35A H 1.0196 0.2806 0.7890 0.076 Uiso 1 1 calc R . . C36 C 1.0287(6) 0.4167(3) 0.6926(4) 0.0603(16) Uani 1 1 d . . . H36A H 1.0013 0.4592 0.6903 0.072 Uiso 1 1 calc R . . C37 C 1.1118(6) 0.2953(4) 0.6968(4) 0.0625(18) Uani 1 1 d . . . H37A H 1.1419 0.2534 0.6984 0.075 Uiso 1 1 calc R . . C38 C 1.1019(6) 0.3980(4) 0.6403(4) 0.0634(18) Uani 1 1 d . . . H38A H 1.1250 0.4279 0.6028 0.076 Uiso 1 1 calc R . . C39 C 1.2224(5) 0.3206(3) 0.5867(4) 0.0497(15) Uani 1 1 d . . . C40 C 1.3782(5) 0.3032(3) 0.4943(3) 0.0438(12) Uani 1 1 d . . . C41 C 1.1925(5) 0.2783(3) 0.5189(3) 0.0445(13) Uani 1 1 d . . . C42 C 1.2788(5) 0.2680(3) 0.4678(4) 0.0435(12) Uani 1 1 d . . . C43 C 1.0874(5) 0.2490(3) 0.4974(4) 0.0527(15) Uani 1 1 d . . . H44A H 1.0306 0.2560 0.5301 0.063 Uiso 1 1 calc R . . C44 C 1.2550(5) 0.2294(3) 0.3946(4) 0.0534(15) Uani 1 1 d . . . H43A H 1.3083 0.2242 0.3586 0.064 Uiso 1 1 calc R . . C45 C 1.0688(5) 0.2100(3) 0.4279(4) 0.0545(15) Uani 1 1 d . . . H45A H 0.9991 0.1898 0.4141 0.065 Uiso 1 1 calc R . . C46 C 1.1509(6) 0.1997(3) 0.3773(4) 0.0592(16) Uani 1 1 d . . . H46A H 1.1358 0.1721 0.3309 0.071 Uiso 1 1 calc R . . C47 C 1.5204(5) 0.2434(3) 0.4307(4) 0.0488(14) Uani 1 1 d . . . H47A H 1.4907 0.2044 0.4471 0.059 Uiso 1 1 calc R . . C48 C 1.5161(5) 0.3585(3) 0.4266(3) 0.0465(13) Uani 1 1 d . . . H48A H 1.4826 0.3974 0.4392 0.056 Uiso 1 1 calc R . . C49 C 1.6131(5) 0.2424(3) 0.3896(4) 0.0452(13) Uani 1 1 d . . . H49A H 1.6440 0.2028 0.3762 0.054 Uiso 1 1 calc R . . C50 C 1.6105(5) 0.3593(3) 0.3868(4) 0.0475(14) Uani 1 1 d . . . H50A H 1.6406 0.3988 0.3725 0.057 Uiso 1 1 calc R . . C51 C 1.6605(4) 0.3012(3) 0.3681(3) 0.0391(11) Uani 1 1 d . . . C52 C 1.7646(5) 0.3036(3) 0.3283(3) 0.0413(12) Uani 1 1 d . . . C53 C 1.7918(5) 0.2522(3) 0.2777(4) 0.0518(14) Uani 1 1 d . . . H53A H 1.7447 0.2161 0.2674 0.062 Uiso 1 1 calc R . . C54 C 1.8381(4) 0.3552(3) 0.3414(3) 0.0441(13) Uani 1 1 d . . . H54A H 1.8230 0.3901 0.3750 0.053 Uiso 1 1 calc R . . C55 C 1.8920(5) 0.2566(3) 0.2430(4) 0.0565(16) Uani 1 1 d . . . H55A H 1.9104 0.2226 0.2091 0.068 Uiso 1 1 calc R . . C56 C 1.9342(5) 0.3546(3) 0.3045(4) 0.0556(15) Uani 1 1 d . . . H56A H 1.9829 0.3900 0.3140 0.067 Uiso 1 1 calc R . . C57 C 0.5580(4) 0.7874(2) 0.8267(3) 0.0368(11) Uani 1 1 d . . . C58 C 0.6147(4) 0.8227(2) 0.9061(3) 0.0363(11) Uani 1 1 d . . . C59 C 0.6914(6) 0.6628(3) 1.0329(5) 0.0642(18) Uani 1 1 d . . . C60 C 0.6270(8) 0.6811(4) 1.1060(5) 0.072(2) Uani 1 1 d . . . C61 C 0.2871(6) 0.6603(3) 0.9321(4) 0.0546(15) Uani 1 1 d D . . C62 C 0.2642(5) 0.7317(3) 0.9566(4) 0.0519(14) Uani 1 1 d D . . C63 C 0.7965(4) 0.9330(2) 0.6331(3) 0.0371(11) Uani 1 1 d . . . C64 C 0.8484(4) 0.9716(2) 0.7129(3) 0.0355(11) Uani 1 1 d . . . C65 C 1.1442(5) 1.0272(4) 0.5768(4) 0.0578(16) Uani 1 1 d . . . C66 C 1.1209(6) 1.0973(4) 0.6026(4) 0.0633(17) Uani 1 1 d . . . C67 C 0.7971(7) 1.0796(4) 0.4278(5) 0.071(2) Uani 1 1 d D . . C68 C 0.7216(7) 1.0912(4) 0.4967(6) 0.072(2) Uani 1 1 d D . . O1W O 0.8282(4) 0.8101(2) 0.7949(3) 0.0551(11) Uani 1 1 d . . . H2 H 0.9001 0.8040 0.7763 0.080 Uiso 1 1 d R . . H1 H 0.8150 0.7778 0.8165 0.080 Uiso 1 1 d R . . O2W O 0.5809(3) 0.9492(2) 0.7447(3) 0.0487(10) Uani 1 1 d . . . H4 H 0.5106 0.9518 0.7603 0.080 Uiso 1 1 d R . . H3 H 0.5904 0.9880 0.7231 0.080 Uiso 1 1 d R . . O3W O -0.0254(15) 0.7306(12) 1.0392(13) 0.366(15) Uani 1 1 d . . . O4W O 1.0579(9) 1.1605(4) 0.7888(6) 0.157(4) Uani 1 1 d . . . H8 H 1.0609 1.1495 0.7326 0.080 Uiso 1 1 d R . . H7 H 1.1230 1.1573 0.8241 0.080 Uiso 1 1 d R . . O5W O 0.6179(7) 1.0728(4) 0.6916(6) 0.139(3) Uani 1 1 d . . . O6W O 0.5771(7) 1.0916(3) 0.2327(5) 0.123(3) Uani 1 1 d . . . O7W O 0.718(2) 0.5466(13) 0.6143(16) 0.380(12) Uiso 1 1 d . . . O8W O 1.0004(18) 0.5728(10) 0.7006 0.323(9) Uiso 1 1 d . . . O9W O 0.8628(16) 1.1479(11) 0.8559(19) 0.400(17) Uani 1 1 d . . . O10W O 0.4302(11) 1.1614(7) 0.6440(16) 0.334(12) Uani 1 1 d . . . O11W O 0.6518(10) 1.1758(6) 0.8149(7) 0.196(5) Uani 1 1 d . . . O12W O 0.7770(6) 0.6835(3) 0.8340(4) 0.103(2) Uani 1 1 d . . . H23 H 0.8358 0.6781 0.8552 0.080 Uiso 1 1 d R . . H24 H 0.7486 0.6795 0.8806 0.080 Uiso 1 1 d R . . O13W O -0.0162(10) 0.6180(6) 0.8520(12) 0.263(9) Uani 1 1 d . . . O14W O 0.6298(10) 0.6137(7) 0.7162(7) 0.191(5) Uani 1 1 d . . . O15W O 1.559(2) 0.5158(15) 0.4892(19) 0.228(11) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0432(5) 0.0397(4) 0.0469(5) 0.0059(4) 0.0176(4) -0.0001(4) Cr2 0.0460(5) 0.0453(5) 0.0487(5) 0.0096(4) 0.0190(4) -0.0002(4) Co1 0.0315(3) 0.0429(3) 0.0401(3) 0.0018(3) 0.0126(2) -0.0032(3) O1 0.041(2) 0.047(2) 0.038(2) 0.0027(16) 0.0071(16) -0.0064(17) O2 0.041(2) 0.050(2) 0.0414(19) -0.0042(16) 0.0179(16) -0.0066(17) O3 0.044(2) 0.0416(19) 0.046(2) 0.0034(15) 0.0121(17) -0.0143(16) O4 0.051(2) 0.051(2) 0.040(2) 0.0038(17) 0.0129(18) -0.0083(19) O5 0.048(2) 0.053(2) 0.065(3) 0.005(2) 0.015(2) 0.0072(19) O6 0.062(3) 0.051(2) 0.053(2) 0.0086(18) 0.018(2) 0.001(2) O7 0.060(4) 0.114(5) 0.115(5) 0.034(4) 0.002(3) 0.024(3) O8 0.136(6) 0.140(6) 0.065(4) 0.025(4) -0.016(4) 0.032(5) O9 0.050(2) 0.0389(19) 0.060(2) 0.0078(17) 0.019(2) 0.0005(17) O10 0.046(2) 0.044(2) 0.073(3) 0.0042(19) 0.023(2) 0.0020(18) O11 0.050(3) 0.064(3) 0.100(4) 0.007(3) 0.001(3) -0.017(2) O12 0.051(3) 0.078(3) 0.105(4) 0.002(3) 0.028(3) 0.011(2) O13 0.0340(18) 0.045(2) 0.0434(19) -0.0003(15) 0.0101(15) -0.0035(16) O14 0.038(2) 0.053(2) 0.0369(19) 0.0012(16) 0.0096(16) -0.0122(17) O15 0.049(2) 0.049(2) 0.039(2) 0.0006(16) 0.0145(17) -0.0051(18) O16 0.046(2) 0.049(2) 0.055(2) 0.0029(17) 0.0134(19) -0.0126(18) O17 0.054(3) 0.056(2) 0.069(3) 0.015(2) 0.023(2) 0.007(2) O18 0.060(3) 0.051(2) 0.071(3) 0.008(2) 0.023(2) -0.004(2) O19 0.059(3) 0.108(4) 0.124(5) 0.018(4) 0.033(3) 0.014(3) O20 0.066(4) 0.086(4) 0.113(5) 0.015(3) -0.013(3) -0.025(3) O21 0.068(3) 0.067(3) 0.050(2) 0.016(2) 0.024(2) 0.007(2) O22 0.057(3) 0.055(2) 0.068(3) 0.010(2) 0.025(2) 0.008(2) O23 0.123(6) 0.138(6) 0.075(4) 0.045(4) -0.004(4) 0.019(5) O24 0.054(3) 0.111(5) 0.165(7) 0.059(5) 0.020(4) 0.027(3) N1 0.043(3) 0.056(3) 0.051(3) -0.001(2) 0.023(2) -0.001(2) N2 0.025(2) 0.057(3) 0.042(2) -0.001(2) 0.0123(18) 0.005(2) N3 0.030(2) 0.089(4) 0.042(3) -0.012(2) 0.010(2) 0.003(2) N4 0.044(3) 0.087(4) 0.046(3) -0.012(2) 0.019(2) -0.008(3) N5 0.036(2) 0.060(3) 0.041(2) -0.002(2) 0.014(2) 0.001(2) N6 0.046(3) 0.131(6) 0.056(3) -0.024(4) 0.016(3) 0.015(4) N7 0.050(4) 0.136(6) 0.051(3) -0.002(4) 0.024(3) 0.015(4) N8 0.037(3) 0.075(3) 0.047(3) -0.004(2) 0.024(2) 0.000(2) N9 0.040(3) 0.106(4) 0.048(3) -0.012(3) 0.022(2) -0.005(3) N10 0.036(3) 0.097(4) 0.045(3) -0.007(3) 0.017(2) -0.009(3) N11 0.033(2) 0.057(3) 0.038(2) 0.006(2) 0.014(2) 0.002(2) N12 0.029(2) 0.069(3) 0.062(3) 0.010(3) 0.016(2) -0.001(2) C1 0.030(3) 0.053(3) 0.061(4) 0.003(3) 0.012(3) -0.010(2) C2 0.044(3) 0.052(3) 0.047(3) -0.005(2) 0.019(3) 0.001(3) C3 0.045(3) 0.041(3) 0.048(3) -0.007(2) 0.014(3) -0.007(2) C4 0.030(3) 0.047(3) 0.047(3) -0.007(2) 0.011(2) -0.007(2) C5 0.034(3) 0.043(3) 0.044(3) -0.001(2) 0.012(2) -0.008(2) C6 0.023(2) 0.049(3) 0.038(3) -0.005(2) 0.010(2) -0.006(2) C7 0.034(3) 0.038(3) 0.045(3) 0.001(2) 0.011(2) -0.002(2) C8 0.033(3) 0.039(3) 0.058(3) 0.003(2) 0.016(2) 0.000(2) C9 0.028(3) 0.047(3) 0.044(3) 0.000(2) 0.011(2) 0.002(2) C10 0.041(3) 0.041(3) 0.056(3) 0.003(2) 0.018(3) 0.000(2) C11 0.024(3) 0.062(3) 0.039(3) 0.001(2) 0.007(2) -0.006(2) C12 0.040(3) 0.060(3) 0.046(3) 0.000(2) 0.021(2) 0.001(3) C13 0.035(3) 0.042(3) 0.035(2) 0.008(2) 0.006(2) 0.003(2) C14 0.035(3) 0.044(3) 0.043(3) 0.004(2) 0.019(2) 0.000(2) C15 0.039(3) 0.046(3) 0.040(3) 0.005(2) 0.016(2) 0.004(2) C16 0.028(3) 0.066(4) 0.053(3) 0.011(3) 0.011(2) 0.006(2) C17 0.048(3) 0.040(3) 0.050(3) -0.001(2) 0.014(3) -0.004(2) C18 0.035(3) 0.050(3) 0.061(4) 0.010(3) 0.002(3) -0.008(2) C19 0.057(4) 0.059(4) 0.081(5) 0.018(3) 0.037(4) 0.010(3) C20 0.070(4) 0.048(3) 0.071(4) 0.004(3) 0.031(3) -0.003(3) C21 0.071(5) 0.064(4) 0.075(5) 0.005(3) 0.043(4) 0.008(3) C22 0.063(4) 0.057(4) 0.059(4) -0.001(3) 0.030(3) -0.007(3) C23 0.032(3) 0.066(4) 0.038(3) -0.006(2) 0.006(2) 0.003(2) C24 0.038(3) 0.076(4) 0.044(3) -0.010(3) 0.012(3) 0.001(3) C25 0.063(5) 0.077(5) 0.100(6) -0.025(4) 0.044(4) -0.005(4) C26 0.048(3) 0.084(4) 0.051(3) 0.008(3) 0.018(3) 0.007(3) C27 0.069(5) 0.089(5) 0.100(6) -0.034(5) 0.041(5) 0.000(4) C28 0.046(4) 0.143(8) 0.042(3) 0.002(4) 0.015(3) 0.008(4) C29 0.039(3) 0.129(7) 0.047(3) 0.005(4) 0.013(3) 0.006(4) C30 0.071(5) 0.102(6) 0.072(5) -0.008(4) 0.027(4) 0.019(5) C31 0.043(4) 0.106(5) 0.045(3) 0.002(3) 0.017(3) 0.001(4) C32 0.056(4) 0.110(6) 0.064(4) -0.015(4) 0.026(4) -0.006(4) C33 0.034(3) 0.091(5) 0.042(3) -0.013(3) 0.013(2) 0.001(3) C34 0.037(3) 0.079(4) 0.042(3) -0.012(3) 0.016(2) -0.008(3) C35 0.055(4) 0.087(5) 0.057(4) 0.001(3) 0.036(3) -0.008(4) C36 0.058(4) 0.066(4) 0.062(4) 0.004(3) 0.025(3) 0.009(3) C37 0.053(4) 0.078(4) 0.065(4) 0.008(3) 0.035(3) 0.010(3) C38 0.058(4) 0.081(5) 0.058(4) 0.010(3) 0.031(3) 0.008(3) C39 0.034(3) 0.076(4) 0.043(3) -0.001(3) 0.020(3) 0.007(3) C40 0.035(3) 0.059(3) 0.040(3) 0.007(2) 0.014(2) 0.004(3) C41 0.033(3) 0.060(3) 0.043(3) 0.006(2) 0.013(2) -0.001(2) C42 0.031(3) 0.057(3) 0.045(3) 0.010(2) 0.017(2) 0.001(2) C43 0.042(3) 0.065(4) 0.055(4) 0.009(3) 0.018(3) 0.002(3) C44 0.050(3) 0.072(4) 0.041(3) -0.007(3) 0.015(3) -0.007(3) C45 0.038(3) 0.067(4) 0.059(4) -0.008(3) 0.009(3) -0.013(3) C46 0.050(4) 0.071(4) 0.059(4) -0.017(3) 0.013(3) -0.011(3) C47 0.041(3) 0.055(3) 0.054(3) 0.018(3) 0.020(3) 0.000(3) C48 0.037(3) 0.056(3) 0.046(3) -0.007(2) 0.008(2) 0.006(2) C49 0.030(3) 0.052(3) 0.055(3) 0.003(3) 0.013(2) 0.003(2) C50 0.030(3) 0.063(4) 0.050(3) -0.002(3) 0.008(2) -0.008(2) C51 0.034(3) 0.047(3) 0.038(3) 0.005(2) 0.010(2) 0.004(2) C52 0.034(3) 0.054(3) 0.037(3) 0.006(2) 0.008(2) 0.007(3) C53 0.043(3) 0.061(4) 0.055(3) -0.006(3) 0.019(3) -0.004(3) C54 0.030(3) 0.058(3) 0.048(3) -0.003(2) 0.015(2) -0.009(2) C55 0.052(4) 0.062(4) 0.061(4) -0.008(3) 0.027(3) 0.006(3) C56 0.044(3) 0.066(4) 0.060(4) -0.005(3) 0.016(3) -0.008(3) C57 0.030(3) 0.039(3) 0.042(3) 0.003(2) 0.006(2) 0.008(2) C58 0.032(3) 0.041(3) 0.038(3) 0.006(2) 0.013(2) 0.000(2) C59 0.054(4) 0.054(4) 0.086(5) 0.012(3) 0.017(4) 0.005(3) C60 0.085(6) 0.066(4) 0.062(4) 0.016(3) 0.007(4) -0.003(4) C61 0.051(4) 0.052(3) 0.063(4) 0.016(3) 0.018(3) 0.001(3) C62 0.046(3) 0.057(3) 0.056(3) 0.012(3) 0.019(3) 0.008(3) C63 0.032(3) 0.036(3) 0.042(3) 0.001(2) 0.004(2) 0.002(2) C64 0.027(2) 0.037(3) 0.044(3) 0.002(2) 0.009(2) -0.003(2) C65 0.043(3) 0.073(4) 0.058(4) 0.023(3) 0.013(3) 0.004(3) C66 0.056(4) 0.071(4) 0.062(4) 0.016(3) 0.006(3) -0.008(4) C67 0.072(5) 0.070(4) 0.069(5) 0.031(4) 0.010(4) -0.003(4) C68 0.069(5) 0.060(4) 0.095(6) 0.029(4) 0.032(4) 0.011(4) O1W 0.042(2) 0.052(2) 0.077(3) 0.009(2) 0.028(2) 0.0061(19) O2W 0.035(2) 0.050(2) 0.064(3) 0.0119(19) 0.0186(19) 0.0076(18) O3W 0.264(19) 0.49(3) 0.40(3) -0.20(2) 0.217(18) -0.24(2) O4W 0.216(10) 0.114(6) 0.126(7) -0.015(5) -0.023(6) 0.024(6) O5W 0.140(7) 0.100(5) 0.202(8) 0.060(5) 0.109(6) 0.034(5) O6W 0.163(7) 0.090(4) 0.110(5) 0.026(4) 0.004(5) -0.025(5) O9W 0.214(18) 0.31(2) 0.71(5) 0.23(3) 0.19(2) 0.076(17) O10W 0.119(9) 0.173(12) 0.73(4) -0.002(17) 0.142(16) 0.012(9) O11W 0.212(11) 0.208(10) 0.193(10) 0.043(8) 0.116(9) 0.084(9) O12W 0.112(5) 0.089(4) 0.123(5) 0.026(4) 0.065(4) 0.017(4) O13W 0.159(10) 0.162(10) 0.44(2) 0.137(12) -0.053(12) -0.001(8) O14W 0.183(10) 0.220(11) 0.177(10) 0.012(8) 0.044(8) -0.063(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 O10 1.948(4) . ? Cr1 O9 1.964(4) . ? Cr1 O6 1.968(4) . ? Cr1 O5 1.976(4) . ? Cr1 O3 2.002(4) . ? Cr1 O4 2.005(4) . ? Cr2 O18 1.943(5) . ? Cr2 O17 1.945(4) . ? Cr2 O21 1.956(4) . ? Cr2 O22 1.964(5) . ? Cr2 O16 1.991(4) . ? Cr2 O15 2.006(4) . ? Co1 O1W 2.046(4) . ? Co1 O2W 2.061(4) . ? Co1 O1 2.091(4) . ? Co1 O2 2.109(3) . ? Co1 O13 2.116(3) . ? Co1 O14 2.119(4) . ? O1 C57 1.252(6) . ? O2 C58 1.238(6) . ? O3 C57 1.265(6) . ? O4 C58 1.260(6) . ? O5 C59 1.288(9) . ? O6 C60 1.304(9) . ? O7 C59 1.215(9) . ? O8 C60 1.214(9) . ? O9 C61 1.284(7) . ? O10 C62 1.300(8) . ? O11 C61 1.230(8) . ? O12 C62 1.226(7) . ? O13 C63 1.230(6) . ? O14 C64 1.221(6) . ? O15 C63 1.271(6) . ? O16 C64 1.277(6) . ? O17 C65 1.274(8) . ? O18 C66 1.297(8) . ? O19 C65 1.217(8) . ? O20 C66 1.215(9) . ? O21 C67 1.301(9) . ? O22 C68 1.279(9) . ? O23 C67 1.220(9) . ? O24 C68 1.225(9) . ? N1 C2 1.325(7) . ? N1 C1 1.339(6) . ? N2 C9 1.342(7) . ? N2 C10 1.344(7) . ? N2 C11 1.477(6) . ? N3 C11 1.298(7) . ? N3 N4 1.350(6) . ? N4 C12 1.315(8) . ? N5 C20 1.331(8) . ? N5 C19 1.340(8) . ? N5 C12 1.454(7) . ? N6 C28 1.310(11) . ? N6 C27 1.311(11) . ? N7 C29 1.310(11) . ? N7 C30 1.323(11) . ? N8 C38 1.314(9) . ? N8 C37 1.319(8) . ? N8 C39 1.464(6) . ? N9 C39 1.304(8) . ? N9 N10 1.380(6) . ? N10 C40 1.288(8) . ? N11 C47 1.346(8) . ? N11 C48 1.367(8) . ? N11 C40 1.445(6) . ? N12 C55 1.317(8) . ? N12 C56 1.327(8) . ? C1 C3 1.386(6) . ? C1 H27A 0.9300 . ? C2 C4 1.378(6) . ? C2 H28A 0.9299 . ? C3 C5 1.379(7) . ? C3 H25A 0.9300 . ? C4 C5 1.373(7) . ? C4 H26A 0.9300 . ? C5 C6 1.467(7) . ? C6 C7 1.401(7) . ? C6 C8 1.410(7) . ? C7 C9 1.357(7) . ? C7 H21A 0.9300 . ? C8 C10 1.358(7) . ? C8 H22A 0.9300 . ? C9 H19A 0.9300 . ? C10 H20A 0.9300 . ? C11 C13 1.412(8) . ? C12 C14 1.402(8) . ? C13 C15 1.405(8) . ? C13 C14 1.419(7) . ? C14 C16 1.411(8) . ? C15 C17 1.368(8) . ? C15 H16A 0.9300 . ? C16 C18 1.352(9) . ? C16 H15A 0.9300 . ? C17 C18 1.371(8) . ? C17 H18A 0.9300 . ? C18 H17A 0.9300 . ? C19 C21 1.376(9) . ? C19 H9A 0.9300 . ? C20 C22 1.383(9) . ? C20 H10A 0.9300 . ? C21 C23 1.356(9) . ? C21 H7A 0.9300 . ? C22 C23 1.380(9) . ? C22 H8A 0.9300 . ? C23 C24 1.477(8) . ? C24 C25 1.366(10) . ? C24 C26 1.388(9) . ? C25 C27 1.419(9) . ? C25 H3A 0.9300 . ? C26 C28 1.404(9) . ? C26 H4A 0.9300 . ? C27 H1A 0.9300 . ? C28 H2A 0.9300 . ? C29 C31 1.364(9) . ? C29 H29A 0.9300 . ? C30 C32 1.381(9) . ? C30 H30A 0.9300 . ? C31 C33 1.377(10) . ? C31 H31A 0.9300 . ? C32 C33 1.382(11) . ? C32 H32A 0.9300 . ? C33 C34 1.491(7) . ? C34 C35 1.366(10) . ? C34 C36 1.387(9) . ? C35 C37 1.362(8) . ? C35 H35A 0.9300 . ? C36 C38 1.357(8) . ? C36 H36A 0.9300 . ? C37 H37A 0.9300 . ? C38 H38A 0.9300 . ? C39 C41 1.394(8) . ? C40 C42 1.405(8) . ? C41 C43 1.393(8) . ? C41 C42 1.429(7) . ? C42 C44 1.409(8) . ? C43 C45 1.363(9) . ? C43 H44A 0.9300 . ? C44 C46 1.380(9) . ? C44 H43A 0.9300 . ? C45 C46 1.383(8) . ? C45 H45A 0.9300 . ? C46 H46A 0.9300 . ? C47 C49 1.375(8) . ? C47 H47A 0.9300 . ? C48 C50 1.381(7) . ? C48 H48A 0.9300 . ? C49 C51 1.399(8) . ? C49 H49A 0.9300 . ? C50 C51 1.385(8) . ? C50 H50A 0.9300 . ? C51 C52 1.485(7) . ? C52 C54 1.373(8) . ? C52 C53 1.399(8) . ? C53 C55 1.402(8) . ? C53 H53A 0.9300 . ? C54 C56 1.372(7) . ? C54 H54A 0.9300 . ? C55 H55A 0.9300 . ? C56 H56A 0.9300 . ? C57 C58 1.533(7) . ? C59 C60 1.543(11) . ? C61 C62 1.550(9) . ? C63 C64 1.553(7) . ? C65 C66 1.532(11) . ? C67 C68 1.547(11) . ? O1W H2 0.9630 . ? O1W H1 0.7757 . ? O2W H4 0.9163 . ? O2W H3 0.8816 . ? O4W H8 0.9346 . ? O4W H7 0.8953 . ? O12W H23 0.7444 . ? O12W H24 0.8715 . ? 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 O10 Cr1 O9 83.06(17) . . ? O10 Cr1 O6 92.64(19) . . ? O9 Cr1 O6 96.50(18) . . ? O10 Cr1 O5 175.46(19) . . ? O9 Cr1 O5 96.41(18) . . ? O6 Cr1 O5 82.93(19) . . ? O10 Cr1 O3 94.81(18) . . ? O9 Cr1 O3 90.80(16) . . ? O6 Cr1 O3 170.15(18) . . ? O5 Cr1 O3 89.70(18) . . ? O10 Cr1 O4 93.47(17) . . ? O9 Cr1 O4 172.26(17) . . ? O6 Cr1 O4 90.56(16) . . ? O5 Cr1 O4 87.58(18) . . ? O3 Cr1 O4 82.57(15) . . ? O18 Cr2 O17 82.7(2) . . ? O18 Cr2 O21 94.0(2) . . ? O17 Cr2 O21 91.73(19) . . ? O18 Cr2 O22 96.66(19) . . ? O17 Cr2 O22 174.09(19) . . ? O21 Cr2 O22 82.45(19) . . ? O18 Cr2 O16 91.56(17) . . ? O17 Cr2 O16 95.77(18) . . ? O21 Cr2 O16 171.17(19) . . ? O22 Cr2 O16 90.11(18) . . ? O18 Cr2 O15 172.61(19) . . ? O17 Cr2 O15 93.38(18) . . ? O21 Cr2 O15 92.33(18) . . ? O22 Cr2 O15 87.93(18) . . ? O16 Cr2 O15 82.61(15) . . ? O1W Co1 O2W 179.6(2) . . ? O1W Co1 O1 89.17(18) . . ? O2W Co1 O1 91.21(15) . . ? O1W Co1 O2 86.87(16) . . ? O2W Co1 O2 93.27(16) . . ? O1 Co1 O2 79.57(14) . . ? O1W Co1 O13 92.22(16) . . ? O2W Co1 O13 87.64(16) . . ? O1 Co1 O13 99.98(14) . . ? O2 Co1 O13 178.98(17) . . ? O1W Co1 O14 91.07(16) . . ? O2W Co1 O14 88.55(17) . . ? O1 Co1 O14 179.46(17) . . ? O2 Co1 O14 100.92(14) . . ? O13 Co1 O14 79.53(14) . . ? C57 O1 Co1 112.5(3) . . ? C58 O2 Co1 112.5(3) . . ? C57 O3 Cr1 111.7(3) . . ? C58 O4 Cr1 112.0(3) . . ? C59 O5 Cr1 113.7(4) . . ? C60 O6 Cr1 113.1(4) . . ? C61 O9 Cr1 114.7(4) . . ? C62 O10 Cr1 114.6(4) . . ? C63 O13 Co1 112.4(3) . . ? C64 O14 Co1 111.5(3) . . ? C63 O15 Cr2 112.1(3) . . ? C64 O16 Cr2 113.2(3) . . ? C65 O17 Cr2 114.7(4) . . ? C66 O18 Cr2 114.7(5) . . ? C67 O21 Cr2 114.2(4) . . ? C68 O22 Cr2 114.9(4) . . ? C2 N1 C1 116.7(4) . . ? C9 N2 C10 122.0(4) . . ? C9 N2 C11 115.9(4) . . ? C10 N2 C11 122.0(5) . . ? C11 N3 N4 119.0(5) . . ? C12 N4 N3 117.2(5) . . ? C20 N5 C19 120.2(5) . . ? C20 N5 C12 121.0(5) . . ? C19 N5 C12 118.8(5) . . ? C28 N6 C27 116.1(6) . . ? C29 N7 C30 116.7(6) . . ? C38 N8 C37 120.6(5) . . ? C38 N8 C39 118.7(5) . . ? C37 N8 C39 120.6(6) . . ? C39 N9 N10 117.1(5) . . ? C40 N10 N9 118.0(5) . . ? C47 N11 C48 120.8(4) . . ? C47 N11 C40 122.2(5) . . ? C48 N11 C40 116.8(5) . . ? C55 N12 C56 117.7(5) . . ? N1 C1 C3 123.7(4) . . ? N1 C1 H27A 118.1 . . ? C3 C1 H27A 118.1 . . ? N1 C2 C4 123.5(4) . . ? N1 C2 H28A 118.0 . . ? C4 C2 H28A 118.5 . . ? C5 C3 C1 118.3(5) . . ? C5 C3 H25A 120.9 . . ? C1 C3 H25A 120.9 . . ? C5 C4 C2 119.3(5) . . ? C5 C4 H26A 120.3 . . ? C2 C4 H26A 120.3 . . ? C4 C5 C3 118.4(5) . . ? C4 C5 C6 122.7(5) . . ? C3 C5 C6 118.8(5) . . ? C7 C6 C8 116.3(4) . . ? C7 C6 C5 120.9(5) . . ? C8 C6 C5 122.7(5) . . ? C9 C7 C6 121.7(5) . . ? C9 C7 H21A 119.1 . . ? C6 C7 H21A 119.1 . . ? C10 C8 C6 120.3(5) . . ? C10 C8 H22A 119.9 . . ? C6 C8 H22A 119.9 . . ? N2 C9 C7 119.3(5) . . ? N2 C9 H19A 120.4 . . ? C7 C9 H19A 120.4 . . ? N2 C10 C8 120.4(5) . . ? N2 C10 H20A 119.8 . . ? C8 C10 H20A 119.8 . . ? N3 C11 C13 127.7(5) . . ? N3 C11 N2 111.3(5) . . ? C13 C11 N2 120.9(5) . . ? N4 C12 C14 127.2(5) . . ? N4 C12 N5 111.5(5) . . ? C14 C12 N5 121.1(5) . . ? C15 C13 C11 126.6(5) . . ? C15 C13 C14 119.7(5) . . ? C11 C13 C14 113.4(5) . . ? C12 C14 C16 124.8(5) . . ? C12 C14 C13 115.4(5) . . ? C16 C14 C13 119.8(5) . . ? C17 C15 C13 118.1(5) . . ? C17 C15 H16A 120.9 . . ? C13 C15 H16A 120.9 . . ? C18 C16 C14 118.1(5) . . ? C18 C16 H15A 120.9 . . ? C14 C16 H15A 120.9 . . ? C15 C17 C18 121.8(5) . . ? C15 C17 H18A 119.1 . . ? C18 C17 H18A 119.1 . . ? C16 C18 C17 122.4(6) . . ? C16 C18 H17A 118.8 . . ? C17 C18 H17A 118.8 . . ? N5 C19 C21 120.5(6) . . ? N5 C19 H9A 119.7 . . ? C21 C19 H9A 119.7 . . ? N5 C20 C22 120.2(6) . . ? N5 C20 H10A 119.9 . . ? C22 C20 H10A 119.9 . . ? C23 C21 C19 121.0(6) . . ? C23 C21 H7A 119.5 . . ? C19 C21 H7A 119.5 . . ? C23 C22 C20 120.6(6) . . ? C23 C22 H8A 119.7 . . ? C20 C22 H8A 119.7 . . ? C21 C23 C22 117.5(5) . . ? C21 C23 C24 122.0(6) . . ? C22 C23 C24 120.4(5) . . ? C25 C24 C26 116.9(6) . . ? C25 C24 C23 121.0(6) . . ? C26 C24 C23 122.0(6) . . ? C24 C25 C27 118.9(7) . . ? C24 C25 H3A 120.6 . . ? C27 C25 H3A 120.6 . . ? C24 C26 C28 119.1(7) . . ? C24 C26 H4A 120.4 . . ? C28 C26 H4A 120.4 . . ? N6 C27 C25 124.5(8) . . ? N6 C27 H1A 117.7 . . ? C25 C27 H1A 117.7 . . ? N6 C28 C26 124.4(7) . . ? N6 C28 H2A 117.8 . . ? C26 C28 H2A 117.8 . . ? N7 C29 C31 123.6(8) . . ? N7 C29 H29A 118.2 . . ? C31 C29 H29A 118.2 . . ? N7 C30 C32 124.0(9) . . ? N7 C30 H30A 118.0 . . ? C32 C30 H30A 118.0 . . ? C29 C31 C33 120.4(8) . . ? C29 C31 H31A 119.8 . . ? C33 C31 H31A 119.8 . . ? C30 C32 C33 118.7(8) . . ? C30 C32 H32A 120.6 . . ? C33 C32 H32A 120.6 . . ? C31 C33 C32 116.5(6) . . ? C31 C33 C34 123.0(7) . . ? C32 C33 C34 120.5(6) . . ? C35 C34 C36 117.2(5) . . ? C35 C34 C33 121.9(6) . . ? C36 C34 C33 120.9(6) . . ? C37 C35 C34 119.8(6) . . ? C37 C35 H35A 120.1 . . ? C34 C35 H35A 120.1 . . ? C38 C36 C34 120.3(6) . . ? C38 C36 H36A 119.8 . . ? C34 C36 H36A 119.8 . . ? N8 C37 C35 121.4(7) . . ? N8 C37 H37A 119.3 . . ? C35 C37 H37A 119.3 . . ? N8 C38 C36 120.7(6) . . ? N8 C38 H38A 119.7 . . ? C36 C38 H38A 119.7 . . ? N9 C39 C41 128.2(5) . . ? N9 C39 N8 111.2(5) . . ? C41 C39 N8 120.4(5) . . ? N10 C40 C42 128.2(5) . . ? N10 C40 N11 110.7(5) . . ? C42 C40 N11 121.0(5) . . ? C43 C41 C39 125.4(5) . . ? C43 C41 C42 120.1(5) . . ? C39 C41 C42 114.4(5) . . ? C40 C42 C44 126.7(5) . . ? C40 C42 C41 114.0(5) . . ? C44 C42 C41 119.1(5) . . ? C45 C43 C41 119.1(5) . . ? C45 C43 H44A 120.4 . . ? C41 C43 H44A 120.4 . . ? C46 C44 C42 118.7(5) . . ? C46 C44 H43A 120.7 . . ? C42 C44 H43A 120.7 . . ? C43 C45 C46 121.7(6) . . ? C43 C45 H45A 119.1 . . ? C46 C45 H45A 119.1 . . ? C44 C46 C45 121.2(6) . . ? C44 C46 H46A 119.4 . . ? C45 C46 H46A 119.4 . . ? N11 C47 C49 120.9(5) . . ? N11 C47 H47A 119.6 . . ? C49 C47 H47A 119.6 . . ? N11 C48 C50 119.8(5) . . ? N11 C48 H48A 120.1 . . ? C50 C48 H48A 120.1 . . ? C47 C49 C51 119.5(5) . . ? C47 C49 H49A 120.2 . . ? C51 C49 H49A 120.2 . . ? C48 C50 C51 120.1(5) . . ? C48 C50 H50A 119.9 . . ? C51 C50 H50A 119.9 . . ? C50 C51 C49 118.8(5) . . ? C50 C51 C52 118.9(5) . . ? C49 C51 C52 122.3(5) . . ? C54 C52 C53 118.0(5) . . ? C54 C52 C51 121.5(5) . . ? C53 C52 C51 120.5(5) . . ? C52 C53 C55 118.0(6) . . ? C52 C53 H53A 121.0 . . ? C55 C53 H53A 121.0 . . ? C56 C54 C52 119.4(5) . . ? C56 C54 H54A 120.3 . . ? C52 C54 H54A 120.3 . . ? N12 C55 C53 123.2(6) . . ? N12 C55 H55A 118.4 . . ? C53 C55 H55A 118.4 . . ? N12 C56 C54 123.7(6) . . ? N12 C56 H56A 118.1 . . ? C54 C56 H56A 118.1 . . ? O1 C57 O3 126.0(5) . . ? O1 C57 C58 117.7(4) . . ? O3 C57 C58 116.3(4) . . ? O2 C58 O4 126.5(5) . . ? O2 C58 C57 117.5(4) . . ? O4 C58 C57 115.9(4) . . ? O7 C59 O5 125.9(7) . . ? O7 C59 C60 119.9(8) . . ? O5 C59 C60 114.1(6) . . ? O8 C60 O6 123.0(8) . . ? O8 C60 C59 122.3(8) . . ? O6 C60 C59 114.6(6) . . ? O11 C61 O9 126.6(6) . . ? O11 C61 C62 119.7(6) . . ? O9 C61 C62 113.8(6) . . ? O12 C62 O10 125.5(6) . . ? O12 C62 C61 120.7(6) . . ? O10 C62 C61 113.9(5) . . ? O13 C63 O15 126.8(5) . . ? O13 C63 C64 117.2(4) . . ? O15 C63 C64 116.0(4) . . ? O14 C64 O16 126.4(5) . . ? O14 C64 C63 119.0(4) . . ? O16 C64 C63 114.4(4) . . ? O19 C65 O17 124.9(7) . . ? O19 C65 C66 120.8(7) . . ? O17 C65 C66 114.2(6) . . ? O20 C66 O18 123.3(8) . . ? O20 C66 C65 123.7(7) . . ? O18 C66 C65 113.0(6) . . ? O23 C67 O21 124.6(8) . . ? O23 C67 C68 121.5(8) . . ? O21 C67 C68 113.9(6) . . ? O24 C68 O22 127.7(8) . . ? O24 C68 C67 119.5(8) . . ? O22 C68 C67 112.8(7) . . ? H2 O1W H1 106.2 . . ? H4 O2W H3 103.4 . . ? H8 O4W H7 115.9 . . ? H23 O12W H24 93.3 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.696 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.069