# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C76 H60 Fe2 Mn2 N16 O6), 4(C1.50 H3.50 N0.5)' _chemical_formula_sum 'C80.50 H70.50 Fe2 Mn2 N17.50 O7.50' _chemical_formula_weight 1624.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) _symmetry_space_group_name_Hall 'P 2yb' _chemical_absolute_configuration rm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.4204(6) _cell_length_b 20.4162(7) _cell_length_c 14.9983(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.042(4) _cell_angle_gamma 90.00 _cell_volume 3797.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2368 _cell_measurement_theta_min 2.356 _cell_measurement_theta_max 26.341 _exptl_crystal_description block _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1676 _exptl_absorpt_coefficient_mu 0.768 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8081 _exptl_absorpt_correction_T_max 0.8432 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II CCD area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15129 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0604 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 25.01 _reflns_number_total 11329 _reflns_number_gt 8889 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2001)' _computing_data_reduction 'SAINT-Plus (Bruker, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008b)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008b)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008b)' _computing_publication_material 'SHELXTL (Sheldrick, 2008b)' _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^)+(0.0634P)^2^+1.2457P] 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 none _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 0.05(2) _refine_ls_number_reflns 11329 _refine_ls_number_parameters 1014 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0719 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1385 _refine_ls_wR_factor_gt 0.1251 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 # start Validation Reply Form _vrf_PLAT111 ; PROBLEM: ADDSYM Detects (Pseudo) Centre of Symmetry ..... 95 %Fit RESPONSE: The two chiral carbon atoms and the six-member ring of cyclohexanediamine were seriously disordered, making the skeleton of the complex partly collapse, when the achirality space group was used to solve the structure of the complex. Considering the chiral starting material was employed, and also the CD spectra gave chiral characteristic, we solve the crystal structure of the complexes by using chiral space group. ; # end Validation Reply Form 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 0.29289(9) 0.69952(5) 1.39320(8) 0.0324(3) Uani 1 1 d . . . Fe2 Fe 0.28972(8) 0.35853(5) 0.89581(7) 0.0286(3) Uani 1 1 d . . . Mn1 Mn 0.24143(9) 0.57000(5) 1.08387(8) 0.0310(3) Uani 1 1 d . . . Mn2 Mn 0.24720(9) 0.48999(6) 0.58469(9) 0.0367(3) Uani 1 1 d . . . O1 O 0.4515(5) 0.8588(3) 1.3141(4) 0.0550(17) Uani 1 1 d . . . O2 O 0.2159(4) 0.6414(3) 1.0059(4) 0.0433(15) Uani 1 1 d . . . O3 O 0.0948(4) 0.5523(3) 1.0962(4) 0.0415(15) Uani 1 1 d . . . O4 O 0.4578(5) 0.2031(3) 0.8251(4) 0.0515(16) Uani 1 1 d . . . O5 O 0.1008(5) 0.5121(3) 0.5938(4) 0.0498(16) Uani 1 1 d . . . O6 O 0.2169(4) 0.4170(3) 0.5108(4) 0.0420(15) Uani 1 1 d . . . O7 O 0.7168(6) 0.5716(5) 0.9547(6) 0.101(3) Uani 1 1 d . . . O8 O 0.7489(12) 0.5084(9) 0.4441(10) 0.095(6) Uani 0.50 1 d P . . N1 N 0.2566(5) 0.6384(4) 1.2039(5) 0.0410(18) Uani 1 1 d . . . N2 N 0.3141(7) 0.7420(5) 1.5894(6) 0.071(3) Uani 1 1 d . . . N3 N 0.2604(6) 0.5581(4) 1.4631(5) 0.053(2) Uani 1 1 d . . . N4 N 0.4497(5) 0.6926(4) 1.3920(5) 0.0366(18) Uani 1 1 d . . . N6 N 0.1418(5) 0.7279(4) 1.3888(5) 0.0372(18) Uani 1 1 d . . . N7 N 0.3167(5) 0.7846(3) 1.3491(4) 0.0355(16) Uani 1 1 d . . . N8 N 0.4016(5) 0.5755(3) 1.0741(4) 0.0322(15) Uani 1 1 d . . . N9 N 0.2827(5) 0.4973(4) 1.1674(4) 0.0360(15) Uani 1 1 d . . . N10 N 0.2437(6) 0.4958(4) 0.9697(5) 0.0428(17) Uani 1 1 d . . . N11 N 0.2566(6) 0.4257(4) 0.7124(5) 0.048(2) Uani 1 1 d . . . N12 N 0.3098(7) 0.3143(4) 1.0955(5) 0.058(2) Uani 1 1 d . . . N13 N 0.4477(5) 0.3659(4) 0.8943(5) 0.0368(18) Uani 1 1 d . . . N15 N 0.1389(5) 0.3274(3) 0.8903(4) 0.0323(16) Uani 1 1 d . . . N16 N 0.3182(5) 0.2749(3) 0.8527(4) 0.0301(15) Uani 1 1 d . . . N17 N 0.4059(5) 0.4762(3) 0.5829(4) 0.0343(16) Uani 1 1 d . . . N18 N 0.2961(5) 0.5684(4) 0.6557(5) 0.0413(16) Uani 1 1 d . . . N19 N 0.8724(7) 0.6215(6) 0.9165(6) 0.075(3) Uani 1 1 d . . . N20 N 0.8745(17) 0.4367(12) 0.4140(12) 0.076(6) Uani 0.50 1 d P . . C1 C 0.2717(6) 0.6619(4) 1.2730(6) 0.034(2) Uani 1 1 d . . . C2 C 0.3076(6) 0.7257(4) 1.5180(5) 0.035(2) Uani 1 1 d . . . C3 C 0.2706(7) 0.6104(5) 1.4373(6) 0.040(2) Uani 1 1 d . . . C4 C 0.5146(7) 0.6450(5) 1.4148(6) 0.050(2) Uani 1 1 d . . . H4 H 0.4881 0.6044 1.4309 0.060 Uiso 1 1 calc R . . C5 C 0.6312(8) 0.6571(6) 1.4144(7) 0.072(3) Uani 1 1 d . . . H5 H 0.6772 0.6221 1.4277 0.086 Uiso 1 1 calc R . . C6 C 0.6734(6) 0.7118(6) 1.3971(7) 0.050(3) Uani 1 1 d . . . H6 H 0.7476 0.7180 1.4022 0.059 Uiso 1 1 calc R . . C7 C 0.6080(6) 0.7591(5) 1.3718(6) 0.048(2) Uani 1 1 d . . . H7 H 0.6361 0.7990 1.3542 0.057 Uiso 1 1 calc R . . C8 C 0.4984(8) 0.7507(5) 1.3707(6) 0.047(2) Uani 1 1 d . . . C9 C 0.4202(7) 0.8048(5) 1.3410(6) 0.045(2) Uani 1 1 d . . . C10 C 0.2260(7) 0.8229(4) 1.3326(6) 0.041(2) Uani 1 1 d . . . C11 C 0.2159(8) 0.8843(5) 1.2990(6) 0.052(3) Uani 1 1 d . . . H11 H 0.2766 0.9055 1.2796 0.063 Uiso 1 1 calc R . . C12 C 0.1139(10) 0.9177(5) 1.2926(8) 0.073(3) Uani 1 1 d . . . H12 H 0.1091 0.9602 1.2704 0.087 Uiso 1 1 calc R . . C13 C 0.0255(9) 0.8867(7) 1.3191(9) 0.083(4) Uani 1 1 d . . . H13 H -0.0401 0.9088 1.3145 0.099 Uiso 1 1 calc R . . C14 C 0.0276(8) 0.8212(6) 1.3541(7) 0.054(3) Uani 1 1 d . . . C15 C 0.1323(7) 0.7905(5) 1.3597(6) 0.041(2) Uani 1 1 d . . . C16 C -0.0613(8) 0.7851(6) 1.3841(7) 0.067(3) Uani 1 1 d . . . H16 H -0.1287 0.8050 1.3844 0.081 Uiso 1 1 calc R . . C17 C -0.0503(8) 0.7235(6) 1.4118(6) 0.059(3) Uani 1 1 d . . . H17 H -0.1093 0.6993 1.4286 0.071 Uiso 1 1 calc R . . C18 C 0.0542(7) 0.6962(6) 1.4147(6) 0.054(3) Uani 1 1 d . . . H18 H 0.0628 0.6536 1.4360 0.065 Uiso 1 1 calc R . . C19 C 0.4594(5) 0.5200(3) 1.1183(4) 0.0349(16) Uani 1 1 d . . . H19 H 0.4550 0.4824 1.0776 0.042 Uiso 1 1 calc R . . C20 C 0.5806(6) 0.5320(4) 1.1461(7) 0.051(3) Uani 1 1 d . . . H20A H 0.6206 0.5402 1.0935 0.061 Uiso 1 1 calc R . . H20B H 0.5875 0.5701 1.1846 0.061 Uiso 1 1 calc R . . C21 C 0.6254(6) 0.4732(4) 1.1943(6) 0.063(3) Uani 1 1 d . . . H21A H 0.7001 0.4815 1.2129 0.075 Uiso 1 1 calc R . . H21B H 0.6237 0.4363 1.1535 0.075 Uiso 1 1 calc R . . C22 C 0.5629(7) 0.4550(5) 1.2769(6) 0.068(3) Uani 1 1 d . . . H22A H 0.5678 0.4904 1.3202 0.081 Uiso 1 1 calc R . . H22B H 0.5936 0.4159 1.3048 0.081 Uiso 1 1 calc R . . C23 C 0.4433(7) 0.4428(5) 1.2464(6) 0.049(2) Uani 1 1 d . . . H23A H 0.4388 0.4061 1.2053 0.058 Uiso 1 1 calc R . . H23B H 0.4026 0.4318 1.2977 0.058 Uiso 1 1 calc R . . C24 C 0.3956(5) 0.5030(3) 1.2011(4) 0.0360(15) Uani 1 1 d . . . H24 H 0.4016 0.5397 1.2431 0.043 Uiso 1 1 calc R . . C25 C 0.2243(6) 0.4477(4) 1.1849(5) 0.037(2) Uani 1 1 d . . . H25 H 0.2560 0.4132 1.2171 0.044 Uiso 1 1 calc R . . C26 C 0.1140(7) 0.4428(4) 1.1575(6) 0.041(2) Uani 1 1 d . . . C27 C 0.0640(7) 0.3826(5) 1.1746(7) 0.055(3) Uani 1 1 d . . . H27 H 0.1026 0.3497 1.2049 0.067 Uiso 1 1 calc R . . C28 C -0.0445(8) 0.3719(5) 1.1458(7) 0.064(3) Uani 1 1 d . . . H28 H -0.0759 0.3311 1.1537 0.077 Uiso 1 1 calc R . . C29 C -0.1051(7) 0.4231(5) 1.1053(7) 0.057(3) Uani 1 1 d . . . H29 H -0.1776 0.4166 1.0887 0.068 Uiso 1 1 calc R . . C30 C -0.0574(7) 0.4828(5) 1.0901(6) 0.049(2) Uani 1 1 d . . . H30 H -0.0981 0.5165 1.0634 0.059 Uiso 1 1 calc R . . C31 C 0.0523(6) 0.4932(5) 1.1146(6) 0.042(2) Uani 1 1 d . . . C32 C 0.4499(7) 0.6212(4) 1.0273(5) 0.043(2) Uani 1 1 d . . . H32 H 0.5247 0.6197 1.0271 0.051 Uiso 1 1 calc R . . C33 C 0.3981(7) 0.6709(4) 0.9786(6) 0.036(2) Uani 1 1 d . . . C34 C 0.4645(7) 0.7152(4) 0.9344(6) 0.042(2) Uani 1 1 d . . . H34 H 0.5387 0.7089 0.9409 0.050 Uiso 1 1 calc R . . C35 C 0.4288(7) 0.7655(5) 0.8841(6) 0.047(2) Uani 1 1 d . . . H35 H 0.4760 0.7945 0.8587 0.057 Uiso 1 1 calc R . . C36 C 0.3160(8) 0.7725(5) 0.8711(7) 0.060(3) Uani 1 1 d . . . H36 H 0.2880 0.8051 0.8334 0.071 Uiso 1 1 calc R . . C37 C 0.2456(8) 0.7309(4) 0.9146(7) 0.052(3) Uani 1 1 d . . . H37 H 0.1716 0.7379 0.9092 0.062 Uiso 1 1 calc R . . C38 C 0.2870(7) 0.6796(4) 0.9652(6) 0.037(2) Uani 1 1 d . . . C39 C 0.2595(6) 0.4454(5) 0.9413(6) 0.035(2) Uani 1 1 d . . . C40 C 0.2695(6) 0.4005(4) 0.7784(5) 0.0316(19) Uani 1 1 d . . . C41 C 0.3028(7) 0.3310(4) 1.0232(7) 0.047(2) Uani 1 1 d . . . C42 C 0.0503(6) 0.3570(5) 0.9134(6) 0.046(2) Uani 1 1 d . . . H42 H 0.0539 0.3991 0.9369 0.056 Uiso 1 1 calc R . . C43 C -0.0500(7) 0.3249(5) 0.9025(7) 0.053(3) Uani 1 1 d . . . H43 H -0.1115 0.3469 0.9188 0.063 Uiso 1 1 calc R . . C44 C -0.0607(7) 0.2643(5) 0.8698(6) 0.047(2) Uani 1 1 d . . . H44 H -0.1282 0.2447 0.8634 0.056 Uiso 1 1 calc R . . C45 C 0.0318(7) 0.2310(4) 0.8453(6) 0.041(2) Uani 1 1 d . . . C46 C 0.1275(6) 0.2646(4) 0.8560(5) 0.0296(18) Uani 1 1 d . . . C47 C 0.0323(9) 0.1664(5) 0.8136(7) 0.058(3) Uani 1 1 d . . . H47 H -0.0313 0.1425 0.8067 0.070 Uiso 1 1 calc R . . C48 C 0.1298(9) 0.1393(5) 0.7927(7) 0.064(3) Uani 1 1 d . . . H48 H 0.1288 0.0969 0.7698 0.077 Uiso 1 1 calc R . . C49 C 0.2282(7) 0.1701(4) 0.8033(6) 0.045(2) Uani 1 1 d . . . H49 H 0.2918 0.1492 0.7898 0.054 Uiso 1 1 calc R . . C50 C 0.2279(6) 0.2339(4) 0.8352(5) 0.0308(19) Uani 1 1 d . . . C51 C 0.5124(7) 0.4203(5) 0.9143(6) 0.050(2) Uani 1 1 d . . . H51 H 0.4818 0.4610 0.9247 0.060 Uiso 1 1 calc R . . C52 C 0.6207(7) 0.4127(5) 0.9182(6) 0.053(2) Uani 1 1 d . . . H52 H 0.6635 0.4489 0.9332 0.064 Uiso 1 1 calc R . . C53 C 0.6687(6) 0.3571(5) 0.9019(6) 0.040(2) Uani 1 1 d . . . H53 H 0.7435 0.3536 0.9052 0.048 Uiso 1 1 calc R . . C54 C 0.6095(8) 0.3081(6) 0.8817(6) 0.055(3) Uani 1 1 d . . . H54 H 0.6433 0.2683 0.8716 0.066 Uiso 1 1 calc R . . C55 C 0.4949(6) 0.3099(4) 0.8732(5) 0.033(2) Uani 1 1 d . . . C56 C 0.4232(6) 0.2558(4) 0.8471(5) 0.0311(19) Uani 1 1 d . . . C57 C 0.4672(5) 0.5147(3) 0.6541(4) 0.0392(16) Uani 1 1 d . . . H57 H 0.4582 0.4921 0.7109 0.047 Uiso 1 1 calc R . . C58 C 0.4137(5) 0.5790(3) 0.6601(5) 0.0453(17) Uani 1 1 d . . . H58 H 0.4308 0.6040 0.6069 0.054 Uiso 1 1 calc R . . C59 C 0.4596(8) 0.6170(6) 0.7410(7) 0.067(3) Uani 1 1 d . . . H59A H 0.4263 0.6599 0.7426 0.080 Uiso 1 1 calc R . . H59B H 0.4437 0.5939 0.7953 0.080 Uiso 1 1 calc R . . C60 C 0.5800(7) 0.6241(5) 0.7356(7) 0.071(3) Uani 1 1 d . . . H60A H 0.5947 0.6519 0.6852 0.086 Uiso 1 1 calc R . . H60B H 0.6092 0.6456 0.7894 0.086 Uiso 1 1 calc R . . C61 C 0.6357(7) 0.5596(4) 0.7254(6) 0.070(3) Uani 1 1 d . . . H61A H 0.6293 0.5338 0.7792 0.084 Uiso 1 1 calc R . . H61B H 0.7118 0.5670 0.7175 0.084 Uiso 1 1 calc R . . C62 C 0.5851(7) 0.5210(5) 0.6431(6) 0.051(2) Uani 1 1 d . . . H62A H 0.5979 0.5443 0.5883 0.061 Uiso 1 1 calc R . . H62B H 0.6177 0.4779 0.6399 0.061 Uiso 1 1 calc R . . C63 C 0.4525(7) 0.4352(4) 0.5381(5) 0.0348(19) Uani 1 1 d . . . H63 H 0.5275 0.4348 0.5435 0.042 Uiso 1 1 calc R . . C64 C 0.3997(7) 0.3863(4) 0.4761(5) 0.036(2) Uani 1 1 d . . . C65 C 0.4655(8) 0.3427(4) 0.4313(6) 0.051(3) Uani 1 1 d . . . H65 H 0.5401 0.3439 0.4408 0.061 Uiso 1 1 calc R . . C66 C 0.4154(9) 0.2969(4) 0.3713(7) 0.059(3) Uani 1 1 d . . . H66 H 0.4572 0.2689 0.3385 0.070 Uiso 1 1 calc R . . C67 C 0.3068(8) 0.2943(5) 0.3620(8) 0.067(3) Uani 1 1 d . . . H67 H 0.2749 0.2633 0.3236 0.081 Uiso 1 1 calc R . . C68 C 0.2432(8) 0.3347(5) 0.4061(7) 0.057(3) Uani 1 1 d . . . H68 H 0.1690 0.3318 0.3948 0.068 Uiso 1 1 calc R . . C69 C 0.2835(7) 0.3815(4) 0.4690(6) 0.038(2) Uani 1 1 d . . . C71 C 0.2307(8) 0.6145(5) 0.6786(6) 0.059(3) Uani 1 1 d . . . H71 H 0.2617 0.6486 0.7119 0.070 Uiso 1 1 calc R . . C72 C 0.1151(8) 0.6192(5) 0.6587(6) 0.052(3) Uani 1 1 d . . . C73 C 0.0621(9) 0.6783(6) 0.6801(8) 0.077(4) Uani 1 1 d . . . H73 H 0.1031 0.7127 0.7043 0.092 Uiso 1 1 calc R . . C74 C -0.0428(10) 0.6865(6) 0.6671(8) 0.075(3) Uani 1 1 d . . . H74 H -0.0769 0.7247 0.6840 0.090 Uiso 1 1 calc R . . C75 C -0.0996(9) 0.6352(6) 0.6271(7) 0.074(3) Uani 1 1 d . . . H75 H -0.1734 0.6406 0.6156 0.089 Uiso 1 1 calc R . . C76 C -0.0552(8) 0.5773(6) 0.6035(7) 0.062(3) Uani 1 1 d . . . H76 H -0.0985 0.5444 0.5781 0.074 Uiso 1 1 calc R . . C77 C 0.0581(8) 0.5672(5) 0.6177(6) 0.049(2) Uani 1 1 d . . . C78 C 0.9290(14) 0.5660(7) 0.8791(9) 0.134(6) Uani 1 1 d . . . H78A H 0.8840 0.5278 0.8797 0.202 Uiso 1 1 calc R . . H78B H 0.9946 0.5579 0.9142 0.202 Uiso 1 1 calc R . . H78C H 0.9457 0.5757 0.8187 0.202 Uiso 1 1 calc R . . C79 C 0.9306(10) 0.6850(7) 0.9224(8) 0.104(5) Uani 1 1 d . . . H79A H 0.8908 0.7155 0.9566 0.157 Uiso 1 1 calc R . . H79B H 0.9380 0.7022 0.8634 0.157 Uiso 1 1 calc R . . H79C H 1.0008 0.6785 0.9509 0.157 Uiso 1 1 calc R . . C80 C 0.7734(9) 0.6221(7) 0.9500(7) 0.076(3) Uani 1 1 d . . . H80 H 0.7464 0.6616 0.9704 0.092 Uiso 1 1 calc R . . C81 C 0.898(2) 0.3724(13) 0.4079(15) 0.092(8) Uani 0.50 1 d P . . H81A H 0.8329 0.3476 0.4001 0.137 Uiso 0.50 1 calc PR . . H81B H 0.9375 0.3585 0.4615 0.137 Uiso 0.50 1 calc PR . . H81C H 0.9418 0.3654 0.3576 0.137 Uiso 0.50 1 calc PR . . C82 C 0.944(2) 0.4857(15) 0.3796(15) 0.093(8) Uani 0.50 1 d P . . H82A H 1.0117 0.4856 0.4139 0.140 Uiso 0.50 1 calc PR . . H82B H 0.9109 0.5279 0.3837 0.140 Uiso 0.50 1 calc PR . . H82C H 0.9564 0.4762 0.3183 0.140 Uiso 0.50 1 calc PR . . C83 C 0.7777(18) 0.4551(14) 0.4505(14) 0.077(7) Uani 0.50 1 d P . . H83 H 0.7370 0.4243 0.4797 0.092 Uiso 0.50 1 calc PR . . 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 0.0286(6) 0.0337(7) 0.0346(7) -0.0005(6) -0.0022(5) 0.0021(5) Fe2 0.0226(6) 0.0340(7) 0.0293(6) 0.0005(5) 0.0031(5) 0.0019(5) Mn1 0.0268(6) 0.0287(7) 0.0372(7) -0.0007(6) -0.0015(5) 0.0010(5) Mn2 0.0305(7) 0.0387(8) 0.0410(7) 0.0038(6) 0.0026(6) 0.0014(6) O1 0.057(4) 0.053(4) 0.055(4) 0.003(3) -0.002(3) -0.023(3) O2 0.033(3) 0.037(3) 0.060(4) 0.019(3) 0.003(3) 0.001(3) O3 0.029(3) 0.031(3) 0.064(4) -0.001(3) 0.002(3) 0.002(2) O4 0.052(4) 0.043(4) 0.059(4) -0.008(3) 0.002(3) 0.017(3) O5 0.035(3) 0.055(4) 0.059(4) 0.001(3) -0.001(3) 0.002(3) O6 0.032(3) 0.043(4) 0.051(4) 0.003(3) 0.000(3) -0.004(3) O7 0.071(5) 0.141(7) 0.091(5) 0.012(5) 0.009(4) -0.036(5) O8 0.100(12) 0.112(12) 0.068(9) -0.018(9) -0.029(8) 0.066(10) N1 0.030(4) 0.059(5) 0.034(4) -0.012(4) -0.001(3) 0.002(3) N2 0.077(7) 0.084(7) 0.051(6) -0.008(5) 0.001(5) -0.018(5) N3 0.054(5) 0.052(5) 0.052(5) 0.017(4) -0.008(3) -0.007(4) N4 0.031(4) 0.048(5) 0.031(4) -0.006(4) 0.003(3) -0.003(4) N6 0.023(4) 0.050(5) 0.039(4) -0.003(4) 0.003(3) -0.008(3) N7 0.034(4) 0.035(4) 0.038(4) -0.005(4) 0.007(3) 0.001(3) N8 0.026(3) 0.037(4) 0.033(3) 0.000(3) 0.000(3) 0.000(3) N9 0.025(3) 0.044(4) 0.038(3) 0.005(3) 0.000(3) -0.002(3) N10 0.049(4) 0.031(4) 0.048(4) -0.008(4) -0.003(3) 0.002(3) N11 0.049(5) 0.047(5) 0.048(5) 0.008(4) -0.002(4) -0.010(4) N12 0.070(6) 0.072(6) 0.034(5) 0.018(4) 0.010(4) 0.018(5) N13 0.026(4) 0.052(5) 0.032(4) 0.008(4) -0.004(3) -0.012(4) N15 0.029(4) 0.039(4) 0.029(4) 0.008(3) 0.003(3) -0.004(3) N16 0.025(3) 0.030(4) 0.034(4) 0.003(3) -0.006(3) 0.005(3) N17 0.030(3) 0.032(4) 0.040(4) 0.001(3) -0.003(3) -0.003(3) N18 0.043(4) 0.038(4) 0.042(4) -0.003(3) -0.003(3) 0.006(3) N19 0.061(6) 0.113(8) 0.049(5) -0.001(6) -0.001(4) -0.016(6) N20 0.087(15) 0.103(17) 0.039(10) 0.006(11) 0.000(10) 0.053(13) C1 0.023(4) 0.028(5) 0.051(6) 0.001(4) -0.002(4) 0.004(3) C2 0.024(4) 0.054(6) 0.026(4) -0.002(4) -0.004(3) -0.002(4) C3 0.027(4) 0.047(6) 0.044(5) 0.006(5) -0.003(4) -0.006(4) C4 0.050(6) 0.048(6) 0.050(6) 0.004(5) -0.003(5) 0.019(5) C5 0.039(6) 0.110(10) 0.065(7) -0.009(7) -0.009(5) 0.040(6) C6 0.009(4) 0.085(7) 0.055(6) -0.017(5) 0.003(4) -0.004(4) C7 0.023(4) 0.085(7) 0.035(5) -0.012(4) 0.007(3) -0.002(4) C8 0.046(6) 0.052(6) 0.042(6) -0.009(5) -0.005(4) -0.002(5) C9 0.034(5) 0.049(6) 0.054(6) -0.005(5) 0.015(4) -0.003(4) C10 0.033(5) 0.036(5) 0.053(6) -0.015(5) -0.005(4) 0.000(4) C11 0.054(6) 0.051(6) 0.051(6) -0.011(5) 0.001(4) -0.009(4) C12 0.077(8) 0.052(7) 0.087(8) 0.005(6) -0.021(6) 0.032(6) C13 0.048(6) 0.103(10) 0.095(9) -0.022(8) -0.016(6) 0.041(7) C14 0.042(6) 0.071(7) 0.048(6) -0.008(5) -0.010(4) 0.028(5) C15 0.042(5) 0.048(6) 0.033(5) -0.019(4) -0.010(4) 0.021(4) C16 0.031(5) 0.109(9) 0.061(6) -0.023(7) -0.004(4) 0.018(6) C17 0.034(5) 0.101(8) 0.042(5) 0.007(5) 0.004(4) 0.011(5) C18 0.044(5) 0.080(7) 0.040(5) -0.012(5) 0.008(4) 0.003(5) C19 0.027(3) 0.041(4) 0.037(4) 0.002(3) -0.002(3) 0.003(3) C20 0.024(4) 0.047(6) 0.081(7) 0.022(5) -0.005(4) 0.002(4) C21 0.027(4) 0.073(6) 0.088(7) 0.022(5) 0.000(4) 0.011(4) C22 0.045(5) 0.086(7) 0.071(6) 0.024(5) -0.008(4) 0.008(4) C23 0.036(4) 0.053(5) 0.056(6) 0.021(5) -0.008(4) -0.006(4) C24 0.033(3) 0.042(4) 0.033(4) -0.002(3) 0.002(3) 0.003(3) C25 0.041(5) 0.041(5) 0.027(4) 0.004(4) 0.000(3) -0.016(4) C26 0.037(5) 0.040(5) 0.045(5) -0.004(5) 0.008(4) -0.006(4) C27 0.048(6) 0.054(6) 0.064(7) 0.000(5) 0.009(5) -0.015(5) C28 0.048(6) 0.066(7) 0.080(7) -0.013(5) 0.019(5) -0.025(5) C29 0.032(5) 0.074(7) 0.065(6) -0.011(5) -0.003(4) -0.010(4) C30 0.032(4) 0.058(6) 0.057(5) -0.001(5) 0.006(4) -0.013(4) C31 0.023(4) 0.056(6) 0.047(5) -0.010(5) 0.010(4) -0.001(4) C32 0.031(4) 0.056(6) 0.042(5) -0.001(4) 0.009(4) 0.000(4) C33 0.036(5) 0.029(5) 0.043(5) -0.007(4) 0.006(4) 0.000(4) C34 0.036(5) 0.050(6) 0.040(5) -0.001(5) 0.009(4) 0.001(4) C35 0.032(4) 0.058(6) 0.052(5) 0.009(5) 0.006(4) -0.005(4) C36 0.065(6) 0.038(5) 0.075(7) 0.025(5) -0.011(5) -0.003(5) C37 0.047(5) 0.032(5) 0.076(7) 0.017(5) -0.002(5) 0.013(4) C38 0.046(5) 0.032(5) 0.032(5) -0.005(4) 0.001(4) -0.006(4) C39 0.029(4) 0.039(5) 0.037(5) 0.006(4) -0.007(3) -0.009(4) C40 0.026(4) 0.041(5) 0.027(4) -0.001(4) 0.005(3) 0.003(4) C41 0.042(5) 0.037(5) 0.063(7) 0.000(5) 0.016(4) 0.007(4) C42 0.031(4) 0.050(5) 0.058(6) -0.015(5) 0.000(4) 0.005(4) C43 0.021(4) 0.071(6) 0.068(6) 0.007(5) 0.012(4) 0.009(4) C44 0.031(5) 0.068(6) 0.043(5) 0.002(4) 0.009(4) -0.019(4) C45 0.040(5) 0.046(5) 0.039(5) 0.011(4) 0.007(4) -0.010(4) C46 0.025(4) 0.031(4) 0.033(4) -0.001(4) 0.000(3) 0.000(3) C47 0.081(7) 0.040(5) 0.054(6) 0.006(5) 0.007(5) -0.021(5) C48 0.074(7) 0.040(6) 0.079(8) 0.003(5) 0.002(6) -0.007(5) C49 0.048(5) 0.028(4) 0.059(6) -0.006(4) -0.010(4) 0.000(4) C50 0.042(5) 0.032(5) 0.018(4) 0.001(4) -0.003(3) -0.008(4) C51 0.036(5) 0.064(6) 0.049(6) 0.006(5) -0.004(4) -0.018(5) C52 0.039(5) 0.070(6) 0.051(6) 0.013(5) -0.005(4) -0.018(5) C53 0.017(4) 0.061(6) 0.043(5) 0.008(5) 0.003(3) -0.003(4) C54 0.041(5) 0.074(7) 0.049(5) 0.011(5) 0.002(4) 0.023(5) C55 0.021(4) 0.051(6) 0.026(4) 0.010(4) 0.005(3) 0.012(4) C56 0.038(5) 0.037(5) 0.018(4) 0.009(4) -0.005(3) 0.015(4) C57 0.037(4) 0.045(4) 0.035(4) 0.002(3) -0.006(3) -0.001(3) C58 0.037(4) 0.045(4) 0.053(5) -0.001(4) -0.005(3) -0.002(3) C59 0.063(7) 0.070(7) 0.065(7) -0.026(6) -0.017(5) -0.006(5) C60 0.057(6) 0.069(6) 0.086(7) -0.027(5) -0.021(5) -0.001(5) C61 0.053(5) 0.069(6) 0.085(7) -0.002(5) -0.019(5) -0.011(4) C62 0.045(5) 0.049(6) 0.058(6) 0.006(5) -0.008(4) -0.001(4) C63 0.028(4) 0.037(5) 0.037(4) 0.011(4) -0.010(3) 0.004(4) C64 0.042(5) 0.036(5) 0.030(5) 0.004(4) -0.004(4) 0.000(4) C65 0.054(6) 0.033(5) 0.066(7) 0.000(5) -0.007(5) 0.007(5) C66 0.093(8) 0.027(5) 0.056(6) -0.008(4) 0.006(5) 0.012(5) C67 0.051(6) 0.052(6) 0.099(8) -0.027(6) 0.002(6) -0.013(5) C68 0.045(6) 0.067(7) 0.057(6) -0.010(5) -0.005(5) 0.001(5) C69 0.032(5) 0.029(5) 0.053(6) 0.005(4) 0.000(4) -0.005(4) C71 0.065(7) 0.055(6) 0.056(6) -0.001(5) 0.011(5) -0.014(5) C72 0.046(6) 0.056(6) 0.053(6) -0.003(6) 0.012(5) 0.008(5) C73 0.061(8) 0.069(8) 0.100(10) -0.014(7) 0.011(7) 0.009(6) C74 0.069(8) 0.075(8) 0.082(8) 0.002(6) 0.014(6) 0.025(6) C75 0.051(6) 0.100(9) 0.073(7) 0.020(6) 0.018(5) 0.034(6) C76 0.049(6) 0.082(8) 0.055(6) 0.011(6) -0.001(4) -0.003(6) C77 0.054(6) 0.052(6) 0.042(5) 0.013(5) 0.013(4) 0.016(5) C78 0.254(19) 0.085(10) 0.067(9) -0.004(8) 0.034(10) 0.038(11) C79 0.100(9) 0.127(11) 0.088(9) -0.045(8) 0.024(7) -0.062(8) C80 0.059(6) 0.115(9) 0.055(6) 0.005(6) 0.002(5) -0.006(6) C81 0.113(19) 0.11(2) 0.050(12) 0.017(12) 0.010(12) 0.039(15) C82 0.12(2) 0.11(2) 0.051(14) 0.001(14) -0.001(13) 0.045(17) C83 0.060(13) 0.11(2) 0.050(12) -0.002(12) -0.049(10) -0.006(13) _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 N7 1.889(7) . ? Fe1 C2 1.946(8) . ? Fe1 N4 1.953(7) . ? Fe1 C3 1.961(10) . ? Fe1 N6 1.962(7) . ? Fe1 C1 1.965(9) . ? Fe2 N16 1.866(7) . ? Fe2 C39 1.944(10) . ? Fe2 C40 1.963(9) . ? Fe2 N13 1.969(6) . ? Fe2 N15 1.976(6) . ? Fe2 C41 1.991(10) . ? Mn1 O3 1.876(5) . ? Mn1 O2 1.884(6) . ? Mn1 N9 1.991(7) . ? Mn1 N8 2.005(6) . ? Mn1 N1 2.278(7) . ? Mn1 N10 2.287(7) . ? Mn2 O6 1.883(6) . ? Mn2 O5 1.886(6) . ? Mn2 N17 1.992(7) . ? Mn2 N18 2.000(7) . ? Mn2 N3 2.306(8) 1_554 ? Mn2 N11 2.321(8) . ? O1 C9 1.244(10) . ? O2 C38 1.349(9) . ? O3 C31 1.350(11) . ? O4 C56 1.212(9) . ? O5 C77 1.302(11) . ? O6 C69 1.287(10) . ? O7 C80 1.252(13) . ? O8 C83 1.15(3) . ? N1 C1 1.148(10) . ? N2 C2 1.121(11) . ? N3 C3 1.145(10) . ? N3 Mn2 2.306(8) 1_556 ? N4 C4 1.297(11) . ? N4 C8 1.376(12) . ? N6 C18 1.341(11) . ? N6 C15 1.353(11) . ? N7 C9 1.361(10) . ? N7 C10 1.383(11) . ? N8 C32 1.330(10) . ? N8 C19 1.479(9) . ? N9 C25 1.282(10) . ? N9 C24 1.469(8) . ? N10 C39 1.135(10) . ? N11 C40 1.119(10) . ? N12 C41 1.135(11) . ? N13 C55 1.331(11) . ? N13 C51 1.394(11) . ? N15 C42 1.319(10) . ? N15 C46 1.385(10) . ? N16 C56 1.368(9) . ? N16 C50 1.413(10) . ? N17 C63 1.237(9) . ? N17 C57 1.501(9) . ? N18 C71 1.301(11) . ? N18 C58 1.475(9) . ? N19 C80 1.352(12) . ? N19 C78 1.463(15) . ? N19 C79 1.485(15) . ? N20 C81 1.35(3) . ? N20 C83 1.40(3) . ? N20 C82 1.44(3) . ? C4 C5 1.469(13) . ? C4 H4 0.9300 . ? C5 C6 1.267(15) . ? C5 H5 0.9300 . ? C6 C7 1.305(14) . ? C6 H6 0.9300 . ? C7 C8 1.372(12) . ? C7 H7 0.9300 . ? C8 C9 1.522(13) . ? C10 C11 1.355(13) . ? C10 C15 1.417(12) . ? C11 C12 1.436(14) . ? C11 H11 0.9300 . ? C12 C13 1.345(15) . ? C12 H12 0.9300 . ? C13 C14 1.437(16) . ? C13 H13 0.9300 . ? C14 C16 1.421(15) . ? C14 C15 1.442(12) . ? C16 C17 1.330(15) . ? C16 H16 0.9300 . ? C17 C18 1.410(13) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C24 1.548(8) . ? C19 C20 1.560(10) . ? C19 H19 0.9800 . ? C20 C21 1.493(11) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.542(11) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.551(12) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.510(11) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24 0.9800 . ? C25 C26 1.412(11) . ? C25 H25 0.9300 . ? C26 C27 1.407(12) . ? C26 C31 1.417(13) . ? C27 C28 1.410(13) . ? C27 H27 0.9300 . ? C28 C29 1.407(14) . ? C28 H28 0.9300 . ? C29 C30 1.381(13) . ? C29 H29 0.9300 . ? C30 C31 1.409(11) . ? C30 H30 0.9300 . ? C32 C33 1.388(12) . ? C32 H32 0.9300 . ? C33 C38 1.396(11) . ? C33 C34 1.413(11) . ? C34 C35 1.336(12) . ? C34 H34 0.9300 . ? C35 C36 1.410(12) . ? C35 H35 0.9300 . ? C36 C37 1.405(13) . ? C36 H36 0.9300 . ? C37 C38 1.376(12) . ? C37 H37 0.9300 . ? C42 C43 1.409(12) . ? C42 H42 0.9300 . ? C43 C44 1.333(14) . ? C43 H43 0.9300 . ? C44 C45 1.401(12) . ? C44 H44 0.9300 . ? C45 C46 1.374(11) . ? C45 C47 1.402(13) . ? C46 C50 1.446(10) . ? C47 C48 1.383(13) . ? C47 H47 0.9300 . ? C48 C49 1.377(13) . ? C48 H48 0.9300 . ? C49 C50 1.386(11) . ? C49 H49 0.9300 . ? C51 C52 1.352(12) . ? C51 H51 0.9300 . ? C52 C53 1.312(13) . ? C52 H52 0.9300 . ? C53 C54 1.269(13) . ? C53 H53 0.9300 . ? C54 C55 1.423(11) . ? C54 H54 0.9300 . ? C55 C56 1.460(12) . ? C57 C58 1.475(9) . ? C57 C62 1.488(10) . ? C57 H57 0.9800 . ? C58 C59 1.525(11) . ? C58 H58 0.9800 . ? C59 C60 1.509(13) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 C61 1.500(12) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 C62 1.568(12) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 C64 1.493(12) . ? C63 H63 0.9300 . ? C64 C65 1.403(11) . ? C64 C69 1.445(11) . ? C65 C66 1.419(13) . ? C65 H65 0.9300 . ? C66 C67 1.350(14) . ? C66 H66 0.9300 . ? C67 C68 1.340(14) . ? C67 H67 0.9300 . ? C68 C69 1.416(13) . ? C68 H68 0.9300 . ? C71 C72 1.454(13) . ? C71 H71 0.9300 . ? C72 C77 1.401(14) . ? C72 C73 1.420(14) . ? C73 C74 1.318(14) . ? C73 H73 0.9300 . ? C74 C75 1.382(16) . ? C74 H74 0.9300 . ? C75 C76 1.359(14) . ? C75 H75 0.9300 . ? C76 C77 1.427(13) . ? C76 H76 0.9300 . ? C78 H78A 0.9600 . ? C78 H78B 0.9600 . ? C78 H78C 0.9600 . ? C79 H79A 0.9600 . ? C79 H79B 0.9600 . ? C79 H79C 0.9600 . ? C80 H80 0.9300 . ? C81 H81A 0.9600 . ? C81 H81B 0.9600 . ? C81 H81C 0.9600 . ? C82 H82A 0.9600 . ? C82 H82B 0.9600 . ? C82 H82C 0.9600 . ? C83 H83 0.9300 . ? 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 N7 Fe1 C2 94.3(3) . . ? N7 Fe1 N4 83.6(3) . . ? C2 Fe1 N4 89.2(3) . . ? N7 Fe1 C3 178.7(3) . . ? C2 Fe1 C3 86.5(4) . . ? N4 Fe1 C3 95.4(3) . . ? N7 Fe1 N6 83.3(3) . . ? C2 Fe1 N6 89.6(3) . . ? N4 Fe1 N6 166.7(3) . . ? C3 Fe1 N6 97.7(3) . . ? N7 Fe1 C1 93.1(3) . . ? C2 Fe1 C1 172.5(4) . . ? N4 Fe1 C1 92.8(3) . . ? C3 Fe1 C1 86.1(4) . . ? N6 Fe1 C1 90.2(3) . . ? N16 Fe2 C39 179.7(3) . . ? N16 Fe2 C40 96.1(3) . . ? C39 Fe2 C40 84.2(3) . . ? N16 Fe2 N13 81.9(3) . . ? C39 Fe2 N13 98.3(3) . . ? C40 Fe2 N13 92.1(3) . . ? N16 Fe2 N15 83.5(3) . . ? C39 Fe2 N15 96.2(3) . . ? C40 Fe2 N15 91.5(3) . . ? N13 Fe2 N15 165.3(3) . . ? N16 Fe2 C41 93.8(3) . . ? C39 Fe2 C41 85.9(4) . . ? C40 Fe2 C41 170.1(4) . . ? N13 Fe2 C41 90.1(3) . . ? N15 Fe2 C41 88.8(3) . . ? O3 Mn1 O2 94.5(3) . . ? O3 Mn1 N9 90.7(3) . . ? O2 Mn1 N9 174.6(3) . . ? O3 Mn1 N8 171.9(3) . . ? O2 Mn1 N8 92.7(3) . . ? N9 Mn1 N8 82.2(3) . . ? O3 Mn1 N1 94.6(3) . . ? O2 Mn1 N1 91.2(3) . . ? N9 Mn1 N1 87.2(3) . . ? N8 Mn1 N1 89.0(2) . . ? O3 Mn1 N10 89.8(3) . . ? O2 Mn1 N10 93.2(3) . . ? N9 Mn1 N10 88.0(3) . . ? N8 Mn1 N10 86.0(3) . . ? N1 Mn1 N10 173.5(3) . . ? O6 Mn2 O5 93.9(3) . . ? O6 Mn2 N17 92.7(3) . . ? O5 Mn2 N17 173.3(3) . . ? O6 Mn2 N18 173.1(3) . . ? O5 Mn2 N18 92.1(3) . . ? N17 Mn2 N18 81.2(3) . . ? O6 Mn2 N3 91.8(3) . 1_554 ? O5 Mn2 N3 91.3(3) . 1_554 ? N17 Mn2 N3 87.9(3) . 1_554 ? N18 Mn2 N3 84.6(3) . 1_554 ? O6 Mn2 N11 92.2(3) . . ? O5 Mn2 N11 94.7(3) . . ? N17 Mn2 N11 85.7(3) . . ? N18 Mn2 N11 90.7(3) . . ? N3 Mn2 N11 172.6(3) 1_554 . ? C38 O2 Mn1 129.5(5) . . ? C31 O3 Mn1 125.8(5) . . ? C77 O5 Mn2 129.4(6) . . ? C69 O6 Mn2 128.2(5) . . ? C1 N1 Mn1 166.4(7) . . ? C3 N3 Mn2 147.5(8) . 1_556 ? C4 N4 C8 115.6(8) . . ? C4 N4 Fe1 131.2(7) . . ? C8 N4 Fe1 113.0(6) . . ? C18 N6 C15 119.4(8) . . ? C18 N6 Fe1 129.6(7) . . ? C15 N6 Fe1 110.9(5) . . ? C9 N7 C10 125.3(8) . . ? C9 N7 Fe1 118.4(6) . . ? C10 N7 Fe1 116.2(6) . . ? C32 N8 C19 123.5(6) . . ? C32 N8 Mn1 123.7(6) . . ? C19 N8 Mn1 112.6(4) . . ? C25 N9 C24 122.1(7) . . ? C25 N9 Mn1 126.0(6) . . ? C24 N9 Mn1 111.6(5) . . ? C39 N10 Mn1 153.0(7) . . ? C40 N11 Mn2 171.4(7) . . ? C55 N13 C51 118.6(7) . . ? C55 N13 Fe2 112.9(6) . . ? C51 N13 Fe2 128.5(7) . . ? C42 N15 C46 116.8(7) . . ? C42 N15 Fe2 130.1(6) . . ? C46 N15 Fe2 113.1(5) . . ? C56 N16 C50 124.7(7) . . ? C56 N16 Fe2 118.7(6) . . ? C50 N16 Fe2 116.4(5) . . ? C63 N17 C57 120.5(6) . . ? C63 N17 Mn2 126.5(6) . . ? C57 N17 Mn2 112.4(5) . . ? C71 N18 C58 120.9(7) . . ? C71 N18 Mn2 122.9(7) . . ? C58 N18 Mn2 114.4(5) . . ? C80 N19 C78 127.9(12) . . ? C80 N19 C79 114.8(11) . . ? C78 N19 C79 117.2(10) . . ? C81 N20 C83 119(2) . . ? C81 N20 C82 121(2) . . ? C83 N20 C82 120(2) . . ? N1 C1 Fe1 177.5(7) . . ? N2 C2 Fe1 178.2(9) . . ? N3 C3 Fe1 178.3(8) . . ? N4 C4 C5 118.2(10) . . ? N4 C4 H4 120.9 . . ? C5 C4 H4 120.9 . . ? C6 C5 C4 124.5(10) . . ? C6 C5 H5 117.7 . . ? C4 C5 H5 117.7 . . ? C5 C6 C7 117.0(9) . . ? C5 C6 H6 121.5 . . ? C7 C6 H6 121.5 . . ? C6 C7 C8 120.8(10) . . ? C6 C7 H7 119.6 . . ? C8 C7 H7 119.6 . . ? C7 C8 N4 123.6(9) . . ? C7 C8 C9 122.0(9) . . ? N4 C8 C9 114.3(8) . . ? O1 C9 N7 127.5(9) . . ? O1 C9 C8 122.3(8) . . ? N7 C9 C8 110.2(8) . . ? C11 C10 N7 130.4(9) . . ? C11 C10 C15 118.5(9) . . ? N7 C10 C15 111.0(8) . . ? C10 C11 C12 121.8(10) . . ? C10 C11 H11 119.1 . . ? C12 C11 H11 119.1 . . ? C13 C12 C11 119.2(10) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C12 C13 C14 123.1(10) . . ? C12 C13 H13 118.5 . . ? C14 C13 H13 118.5 . . ? C16 C14 C13 126.8(10) . . ? C16 C14 C15 118.1(10) . . ? C13 C14 C15 115.2(10) . . ? N6 C15 C10 118.3(8) . . ? N6 C15 C14 119.5(9) . . ? C10 C15 C14 122.2(9) . . ? C17 C16 C14 121.3(10) . . ? C17 C16 H16 119.3 . . ? C14 C16 H16 119.3 . . ? C16 C17 C18 117.6(10) . . ? C16 C17 H17 121.2 . . ? C18 C17 H17 121.2 . . ? N6 C18 C17 124.0(10) . . ? N6 C18 H18 118.0 . . ? C17 C18 H18 118.0 . . ? N8 C19 C24 105.9(5) . . ? N8 C19 C20 116.0(6) . . ? C24 C19 C20 110.4(6) . . ? N8 C19 H19 108.1 . . ? C24 C19 H19 108.1 . . ? C20 C19 H19 108.1 . . ? C21 C20 C19 109.4(7) . . ? C21 C20 H20A 109.8 . . ? C19 C20 H20A 109.8 . . ? C21 C20 H20B 109.8 . . ? C19 C20 H20B 109.8 . . ? H20A C20 H20B 108.2 . . ? C20 C21 C22 113.1(7) . . ? C20 C21 H21A 109.0 . . ? C22 C21 H21A 109.0 . . ? C20 C21 H21B 109.0 . . ? C22 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? C21 C22 C23 108.4(7) . . ? C21 C22 H22A 110.0 . . ? C23 C22 H22A 110.0 . . ? C21 C22 H22B 110.0 . . ? C23 C22 H22B 110.0 . . ? H22A C22 H22B 108.4 . . ? C24 C23 C22 110.4(7) . . ? C24 C23 H23A 109.6 . . ? C22 C23 H23A 109.6 . . ? C24 C23 H23B 109.6 . . ? C22 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? N9 C24 C23 115.8(6) . . ? N9 C24 C19 105.1(5) . . ? C23 C24 C19 109.8(6) . . ? N9 C24 H24 108.6 . . ? C23 C24 H24 108.6 . . ? C19 C24 H24 108.6 . . ? N9 C25 C26 123.2(8) . . ? N9 C25 H25 118.4 . . ? C26 C25 H25 118.4 . . ? C27 C26 C25 116.1(9) . . ? C27 C26 C31 118.9(8) . . ? C25 C26 C31 125.0(8) . . ? C26 C27 C28 120.3(10) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C29 C28 C27 119.8(9) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C30 C29 C28 120.2(9) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C29 C30 C31 120.5(9) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? O3 C31 C30 117.7(8) . . ? O3 C31 C26 122.2(7) . . ? C30 C31 C26 120.1(9) . . ? N8 C32 C33 125.5(8) . . ? N8 C32 H32 117.2 . . ? C33 C32 H32 117.2 . . ? C32 C33 C38 126.5(8) . . ? C32 C33 C34 116.7(8) . . ? C38 C33 C34 116.7(8) . . ? C35 C34 C33 124.9(9) . . ? C35 C34 H34 117.6 . . ? C33 C34 H34 117.6 . . ? C34 C35 C36 117.0(8) . . ? C34 C35 H35 121.5 . . ? C36 C35 H35 121.5 . . ? C37 C36 C35 120.8(9) . . ? C37 C36 H36 119.6 . . ? C35 C36 H36 119.6 . . ? C38 C37 C36 119.5(9) . . ? C38 C37 H37 120.2 . . ? C36 C37 H37 120.2 . . ? O2 C38 C37 117.1(8) . . ? O2 C38 C33 121.8(8) . . ? C37 C38 C33 120.9(8) . . ? N10 C39 Fe2 178.2(8) . . ? N11 C40 Fe2 178.3(8) . . ? N12 C41 Fe2 179.0(9) . . ? N15 C42 C43 120.1(9) . . ? N15 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C44 C43 C42 123.0(8) . . ? C44 C43 H43 118.5 . . ? C42 C43 H43 118.5 . . ? C43 C44 C45 118.7(8) . . ? C43 C44 H44 120.7 . . ? C45 C44 H44 120.7 . . ? C46 C45 C44 116.3(8) . . ? C46 C45 C47 119.3(9) . . ? C44 C45 C47 124.4(9) . . ? C45 C46 N15 125.2(7) . . ? C45 C46 C50 120.6(7) . . ? N15 C46 C50 114.2(7) . . ? C48 C47 C45 118.3(10) . . ? C48 C47 H47 120.9 . . ? C45 C47 H47 120.9 . . ? C49 C48 C47 125.0(10) . . ? C49 C48 H48 117.5 . . ? C47 C48 H48 117.5 . . ? C48 C49 C50 116.8(9) . . ? C48 C49 H49 121.6 . . ? C50 C49 H49 121.6 . . ? C49 C50 N16 127.2(8) . . ? C49 C50 C46 120.0(8) . . ? N16 C50 C46 112.8(7) . . ? C52 C51 N13 118.6(10) . . ? C52 C51 H51 120.7 . . ? N13 C51 H51 120.7 . . ? C53 C52 C51 123.5(10) . . ? C53 C52 H52 118.3 . . ? C51 C52 H52 118.3 . . ? C54 C53 C52 117.7(8) . . ? C54 C53 H53 121.2 . . ? C52 C53 H53 121.2 . . ? C53 C54 C55 124.4(10) . . ? C53 C54 H54 117.8 . . ? C55 C54 H54 117.8 . . ? N13 C55 C54 117.0(9) . . ? N13 C55 C56 116.3(7) . . ? C54 C55 C56 126.7(8) . . ? O4 C56 N16 128.5(8) . . ? O4 C56 C55 121.7(7) . . ? N16 C56 C55 109.8(7) . . ? C58 C57 C62 112.3(6) . . ? C58 C57 N17 107.2(6) . . ? C62 C57 N17 115.5(6) . . ? C58 C57 H57 107.2 . . ? C62 C57 H57 107.2 . . ? N17 C57 H57 107.2 . . ? N18 C58 C57 108.4(6) . . ? N18 C58 C59 115.9(7) . . ? C57 C58 C59 110.5(7) . . ? N18 C58 H58 107.2 . . ? C57 C58 H58 107.2 . . ? C59 C58 H58 107.2 . . ? C60 C59 C58 109.6(8) . . ? C60 C59 H59A 109.7 . . ? C58 C59 H59A 109.7 . . ? C60 C59 H59B 109.7 . . ? C58 C59 H59B 109.7 . . ? H59A C59 H59B 108.2 . . ? C61 C60 C59 112.6(8) . . ? C61 C60 H60A 109.1 . . ? C59 C60 H60A 109.1 . . ? C61 C60 H60B 109.1 . . ? C59 C60 H60B 109.1 . . ? H60A C60 H60B 107.8 . . ? C60 C61 C62 110.7(7) . . ? C60 C61 H61A 109.5 . . ? C62 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? C62 C61 H61B 109.5 . . ? H61A C61 H61B 108.1 . . ? C57 C62 C61 108.1(7) . . ? C57 C62 H62A 110.1 . . ? C61 C62 H62A 110.1 . . ? C57 C62 H62B 110.1 . . ? C61 C62 H62B 110.1 . . ? H62A C62 H62B 108.4 . . ? N17 C63 C64 126.0(8) . . ? N17 C63 H63 117.0 . . ? C64 C63 H63 117.0 . . ? C65 C64 C69 121.8(8) . . ? C65 C64 C63 118.3(8) . . ? C69 C64 C63 119.7(8) . . ? C64 C65 C66 118.3(9) . . ? C64 C65 H65 120.8 . . ? C66 C65 H65 120.8 . . ? C67 C66 C65 119.6(9) . . ? C67 C66 H66 120.2 . . ? C65 C66 H66 120.2 . . ? C68 C67 C66 122.4(10) . . ? C68 C67 H67 118.8 . . ? C66 C67 H67 118.8 . . ? C67 C68 C69 123.2(10) . . ? C67 C68 H68 118.4 . . ? C69 C68 H68 118.4 . . ? O6 C69 C68 119.4(8) . . ? O6 C69 C64 126.3(8) . . ? C68 C69 C64 114.2(8) . . ? N18 C71 C72 128.2(10) . . ? N18 C71 H71 115.9 . . ? C72 C71 H71 115.9 . . ? C77 C72 C73 120.9(10) . . ? C77 C72 C71 120.7(9) . . ? C73 C72 C71 118.4(10) . . ? C74 C73 C72 122.7(12) . . ? C74 C73 H73 118.6 . . ? C72 C73 H73 118.6 . . ? C73 C74 C75 116.5(11) . . ? C73 C74 H74 121.7 . . ? C75 C74 H74 121.7 . . ? C76 C75 C74 124.6(10) . . ? C76 C75 H75 117.7 . . ? C74 C75 H75 117.7 . . ? C75 C76 C77 119.8(11) . . ? C75 C76 H76 120.1 . . ? C77 C76 H76 120.1 . . ? O5 C77 C72 124.9(9) . . ? O5 C77 C76 119.8(10) . . ? C72 C77 C76 115.3(9) . . ? N19 C78 H78A 109.5 . . ? N19 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? N19 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? N19 C79 H79A 109.5 . . ? N19 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? N19 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? O7 C80 N19 122.5(13) . . ? O7 C80 H80 118.7 . . ? N19 C80 H80 118.7 . . ? N20 C81 H81A 109.5 . . ? N20 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? N20 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? N20 C82 H82A 109.5 . . ? N20 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? N20 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? O8 C83 N20 119(3) . . ? O8 C83 H83 120.3 . . ? N20 C83 H83 120.3 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.604 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.068 _database_code_depnum_ccdc_archive 'CCDC 951679' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C76 H60 Fe2 Mn2 N16 O6), 4(C1.50 H3.50 N0.50 O0.50)' _chemical_formula_sum 'C80.50 H70.50 Fe2 Mn2 N17.50 O7.50' _chemical_formula_weight 1624.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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) _symmetry_space_group_name_Hall 'P 2yb' _chemical_absolute_configuration rm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.4080(6) _cell_length_b 20.4024(9) _cell_length_c 15.0189(9) _cell_angle_alpha 90.00 _cell_angle_beta 92.969(5) _cell_angle_gamma 90.00 _cell_volume 3797.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3218 _cell_measurement_theta_min 2.128 _cell_measurement_theta_max 26.521 _exptl_crystal_description block _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1676 _exptl_absorpt_coefficient_mu 0.768 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7238 _exptl_absorpt_correction_T_max 0.7968 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II CCD area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14601 _diffrn_reflns_av_R_equivalents 0.0811 _diffrn_reflns_av_sigmaI/netI 0.1322 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 25.01 _reflns_number_total 11113 _reflns_number_gt 6791 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2001)' _computing_data_reduction 'SAINT-Plus (Bruker, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008b)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008b)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008b)' _computing_publication_material 'SHELXTL (Sheldrick, 2008b)' _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^)+(0.1256P)^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 none _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 0.02(4) _refine_ls_number_reflns 11113 _refine_ls_number_parameters 1014 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1348 _refine_ls_R_factor_gt 0.0934 _refine_ls_wR_factor_ref 0.2692 _refine_ls_wR_factor_gt 0.2226 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 # start Validation Reply Form _vrf_PLAT111 ; PROBLEM: ADDSYM Detects (Pseudo) Centre of Symmetry ..... 95 %Fit RESPONSE: The two chiral carbon atoms and the six-member ring of cyclohexanediamine were seriously disordered, making the skeleton of the complex partly collapse, when the achirality space group was used to solve the structure of the complex. Considering the chiral starting material was employed, and also the CD spectra gave chiral characteristic, we solve the crystal structure of the complexes by using chiral space group. ; # end Validation Reply Form 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 0.79358(16) 0.63471(8) 1.39383(13) 0.0390(5) Uani 1 1 d . . . Fe2 Fe 0.78973(16) 0.29389(8) 0.89533(14) 0.0391(5) Uani 1 1 d . . . Mn1 Mn 0.74197(16) 0.50490(9) 1.08406(14) 0.0411(6) Uani 1 1 d . . . Mn2 Mn 0.74772(16) 0.42527(9) 0.58516(15) 0.0423(6) Uani 1 1 d . . . O1 O 0.9508(8) 0.7952(6) 1.3151(7) 0.062(3) Uani 1 1 d . . . O2 O 0.7164(7) 0.5765(5) 1.0046(6) 0.047(3) Uani 1 1 d . . . O3 O 0.5951(7) 0.4874(5) 1.0971(7) 0.047(3) Uani 1 1 d . . . O4 O 0.9579(8) 0.1385(5) 0.8246(7) 0.056(3) Uani 1 1 d . . . O5 O 0.6012(8) 0.4485(6) 0.5943(8) 0.056(3) Uani 1 1 d . . . O6 O 0.7164(8) 0.3517(5) 0.5135(7) 0.052(3) Uani 1 1 d . . . O7 O 0.249(2) 0.4463(16) 0.4446(18) 0.106(10) Uani 0.50 1 d P . . O8 O 0.2164(12) 0.5065(8) 0.9539(10) 0.110(5) Uani 1 1 d . . . N1 N 0.7555(9) 0.5744(6) 1.2044(9) 0.050(3) Uani 1 1 d . . . N2 N 0.7629(10) 0.4931(6) 1.4643(9) 0.054(3) Uani 1 1 d . . . N3 N 0.8166(12) 0.6766(8) 1.5911(10) 0.065(4) Uani 1 1 d . . . N4 N 0.6426(9) 0.6629(6) 1.3905(8) 0.044(3) Uani 1 1 d . . . N5 N 0.8168(9) 0.7188(6) 1.3488(8) 0.040(3) Uani 1 1 d . . . N6 N 0.9511(9) 0.6291(7) 1.3922(8) 0.042(3) Uani 1 1 d . . . N7 N 0.7842(9) 0.4311(6) 1.1657(8) 0.046(3) Uani 1 1 d . . . N8 N 0.9014(9) 0.5103(6) 1.0748(8) 0.044(3) Uani 1 1 d . . . N9 N 0.7455(10) 0.4314(6) 0.9698(8) 0.051(3) Uani 1 1 d . . . N10 N 0.8085(13) 0.2494(7) 1.0942(11) 0.070(4) Uani 1 1 d . . . N11 N 0.7558(10) 0.3617(6) 0.7124(9) 0.050(3) Uani 1 1 d . . . N12 N 0.6388(9) 0.2634(6) 0.8907(8) 0.043(3) Uani 1 1 d . . . N13 N 0.8179(9) 0.2088(5) 0.8526(8) 0.042(3) Uani 1 1 d . . . N14 N 0.9483(10) 0.3010(6) 0.8939(8) 0.045(3) Uani 1 1 d . . . N15 N 0.9068(10) 0.4113(6) 0.5825(8) 0.044(3) Uani 1 1 d . . . N16 N 0.7968(10) 0.5046(6) 0.6564(8) 0.050(3) Uani 1 1 d . . . N17 N 0.3735(15) 0.5563(10) 0.9190(12) 0.093(6) Uani 1 1 d . . . N18 N 0.376(3) 0.3744(17) 0.4129(17) 0.069(9) Uani 0.50 1 d P . . C1 C 0.7731(11) 0.5954(7) 1.2740(10) 0.043(3) Uani 1 1 d . . . C2 C 0.7720(12) 0.5457(8) 1.4371(10) 0.047(4) Uani 1 1 d . . . C3 C 0.8084(12) 0.6619(8) 1.5205(11) 0.048(4) Uani 1 1 d . . . C4 C 1.0127(13) 0.5803(9) 1.4146(11) 0.057(4) Uani 1 1 d . . . H4 H 0.9858 0.5396 1.4302 0.069 Uiso 1 1 calc R . . C5 C 1.1331(14) 0.5945(10) 1.4134(11) 0.070(5) Uani 1 1 d . . . H5 H 1.1796 0.5596 1.4265 0.084 Uiso 1 1 calc R . . C6 C 1.1760(11) 0.6483(9) 1.3965(10) 0.049(4) Uani 1 1 d . . . H6 H 1.2504 0.6546 1.4001 0.059 Uiso 1 1 calc R . . C7 C 1.1092(11) 0.6941(9) 1.3739(11) 0.054(4) Uani 1 1 d . . . H7 H 1.1372 0.7350 1.3605 0.064 Uiso 1 1 calc R . . C8 C 0.9977(12) 0.6865(8) 1.3681(10) 0.046(4) Uani 1 1 d . . . C9 C 0.9205(12) 0.7391(8) 1.3415(11) 0.048(4) Uani 1 1 d . . . C10 C 0.7255(12) 0.7578(7) 1.3322(10) 0.044(4) Uani 1 1 d . . . C11 C 0.7178(13) 0.8200(8) 1.2960(11) 0.058(4) Uani 1 1 d . . . H11 H 0.7775 0.8409 1.2738 0.069 Uiso 1 1 calc R . . C12 C 0.6125(14) 0.8517(8) 1.2938(11) 0.063(5) Uani 1 1 d . . . H12 H 0.6066 0.8949 1.2745 0.076 Uiso 1 1 calc R . . C13 C 0.5228(15) 0.8203(9) 1.3191(12) 0.066(5) Uani 1 1 d . . . H13 H 0.4565 0.8414 1.3116 0.079 Uiso 1 1 calc R . . C14 C 0.5259(14) 0.7579(9) 1.3556(11) 0.058(4) Uani 1 1 d . . . C15 C 0.4379(13) 0.7192(10) 1.3833(11) 0.062(5) Uani 1 1 d . . . H15 H 0.3692 0.7375 1.3831 0.074 Uiso 1 1 calc R . . C16 C 0.4521(13) 0.6583(9) 1.4089(11) 0.058(4) Uani 1 1 d . . . H16 H 0.3937 0.6324 1.4227 0.070 Uiso 1 1 calc R . . C17 C 0.5564(12) 0.6332(9) 1.4150(10) 0.054(4) Uani 1 1 d . . . H17 H 0.5653 0.5913 1.4388 0.065 Uiso 1 1 calc R . . C18 C 0.6294(12) 0.7255(8) 1.3604(10) 0.050(4) Uani 1 1 d . . . C19 C 0.9593(10) 0.4551(7) 1.1209(9) 0.052(3) Uani 1 1 d . . . H19 H 0.9564 0.4174 1.0804 0.062 Uiso 1 1 calc R . . C20 C 0.8945(9) 0.4379(6) 1.2008(9) 0.052(3) Uani 1 1 d . . . H20 H 0.8984 0.4746 1.2429 0.062 Uiso 1 1 calc R . . C21 C 0.9413(13) 0.3782(8) 1.2461(11) 0.058(4) Uani 1 1 d . . . H21A H 0.9357 0.3410 1.2060 0.069 Uiso 1 1 calc R . . H21B H 0.9016 0.3681 1.2984 0.069 Uiso 1 1 calc R . . C22 C 1.0646(12) 0.3915(8) 1.2747(11) 0.071(4) Uani 1 1 d . . . H22A H 1.0697 0.4278 1.3165 0.085 Uiso 1 1 calc R . . H22B H 1.0953 0.3530 1.3043 0.085 Uiso 1 1 calc R . . C23 C 1.1272(11) 0.4074(8) 1.1945(11) 0.070(4) Uani 1 1 d . . . H23A H 1.1247 0.3706 1.1537 0.083 Uiso 1 1 calc R . . H23B H 1.2021 0.4157 1.2128 0.083 Uiso 1 1 calc R . . C24 C 1.0782(12) 0.4684(8) 1.1476(12) 0.057(4) Uani 1 1 d . . . H24A H 1.0839 0.5058 1.1874 0.068 Uiso 1 1 calc R . . H24B H 1.1174 0.4784 1.0950 0.068 Uiso 1 1 calc R . . C25 C 0.7253(12) 0.3818(8) 1.1837(10) 0.049(4) Uani 1 1 d . . . H25 H 0.7570 0.3475 1.2164 0.059 Uiso 1 1 calc R . . C26 C 0.6176(12) 0.3768(8) 1.1574(10) 0.050(4) Uani 1 1 d . . . C27 C 0.5614(13) 0.3158(9) 1.1726(12) 0.064(5) Uani 1 1 d . . . H27 H 0.5978 0.2812 1.2011 0.077 Uiso 1 1 calc R . . C28 C 0.4565(14) 0.3089(9) 1.1454(12) 0.067(5) Uani 1 1 d . . . H28 H 0.4243 0.2684 1.1540 0.080 Uiso 1 1 calc R . . C29 C 0.3923(13) 0.3588(8) 1.1049(11) 0.065(5) Uani 1 1 d . . . H29 H 0.3195 0.3522 1.0896 0.078 Uiso 1 1 calc R . . C30 C 0.4419(12) 0.4171(9) 1.0891(11) 0.061(4) Uani 1 1 d . . . H30 H 0.4020 0.4504 1.0608 0.073 Uiso 1 1 calc R . . C31 C 0.5524(11) 0.4288(8) 1.1143(10) 0.048(4) Uani 1 1 d . . . C32 C 0.9499(13) 0.5546(8) 1.0310(10) 0.047(4) Uani 1 1 d . . . H32 H 1.0249 0.5529 1.0326 0.057 Uiso 1 1 calc R . . C33 C 0.8983(12) 0.6071(7) 0.9793(10) 0.044(4) Uani 1 1 d . . . C34 C 0.9652(13) 0.6494(7) 0.9318(10) 0.050(4) Uani 1 1 d . . . H34 H 1.0392 0.6417 0.9343 0.060 Uiso 1 1 calc R . . C35 C 0.9274(13) 0.6989(8) 0.8844(11) 0.055(4) Uani 1 1 d . . . H35 H 0.9742 0.7277 0.8578 0.066 Uiso 1 1 calc R . . C36 C 0.8164(14) 0.7080(8) 0.8745(12) 0.063(4) Uani 1 1 d . . . H36 H 0.7890 0.7429 0.8405 0.076 Uiso 1 1 calc R . . C37 C 0.7465(13) 0.6661(8) 0.9144(12) 0.059(4) Uani 1 1 d . . . H37 H 0.6725 0.6730 0.9073 0.071 Uiso 1 1 calc R . . C38 C 0.7852(13) 0.6142(7) 0.9645(11) 0.046(4) Uani 1 1 d . . . C39 C 0.7604(12) 0.3798(8) 0.9423(11) 0.048(4) Uani 1 1 d . . . C40 C 0.8021(12) 0.2670(8) 1.0204(11) 0.048(4) Uani 1 1 d . . . C41 C 0.7693(11) 0.3362(7) 0.7781(10) 0.040(3) Uani 1 1 d . . . C42 C 1.0144(13) 0.3529(8) 0.9129(10) 0.054(4) Uani 1 1 d . . . H42 H 0.9835 0.3937 0.9223 0.065 Uiso 1 1 calc R . . C43 C 1.1221(13) 0.3478(9) 0.9186(11) 0.057(4) Uani 1 1 d . . . H43 H 1.1645 0.3840 0.9341 0.069 Uiso 1 1 calc R . . C44 C 1.1665(11) 0.2922(8) 0.9025(10) 0.048(4) Uani 1 1 d . . . H44 H 1.2413 0.2883 0.9075 0.058 Uiso 1 1 calc R . . C45 C 1.1095(13) 0.2428(9) 0.8801(11) 0.059(4) Uani 1 1 d . . . H45 H 1.1440 0.2038 0.8666 0.071 Uiso 1 1 calc R . . C46 C 0.9950(12) 0.2447(8) 0.8746(10) 0.047(4) Uani 1 1 d . . . C47 C 0.7276(12) 0.1687(7) 0.8355(10) 0.045(4) Uani 1 1 d . . . C48 C 0.7249(13) 0.1073(7) 0.8052(11) 0.055(4) Uani 1 1 d . . . H48 H 0.7894 0.0865 0.7933 0.065 Uiso 1 1 calc R . . C49 C 0.6328(14) 0.0749(9) 0.7914(12) 0.069(5) Uani 1 1 d . . . H49 H 0.6355 0.0332 0.7667 0.082 Uiso 1 1 calc R . . C50 C 0.5342(15) 0.0991(9) 0.8112(12) 0.065(5) Uani 1 1 d . . . H50 H 0.4717 0.0742 0.8043 0.078 Uiso 1 1 calc R . . C51 C 0.5327(14) 0.1675(8) 0.8443(11) 0.053(4) Uani 1 1 d . . . C52 C 0.4395(14) 0.1996(9) 0.8702(12) 0.061(5) Uani 1 1 d . . . H52 H 0.3723 0.1796 0.8622 0.073 Uiso 1 1 calc R . . C53 C 0.4487(14) 0.2601(9) 0.9072(12) 0.066(5) Uani 1 1 d . . . H53 H 0.3883 0.2803 0.9289 0.079 Uiso 1 1 calc R . . C54 C 0.6315(12) 0.2011(8) 0.8564(10) 0.047(4) Uani 1 1 d . . . C55 C 0.5499(11) 0.2928(9) 0.9130(10) 0.050(4) Uani 1 1 d . . . H55 H 0.5534 0.3359 0.9330 0.060 Uiso 1 1 calc R . . C56 C 0.9665(10) 0.4488(6) 0.6538(9) 0.052(3) Uani 1 1 d . . . H56 H 0.9580 0.4260 0.7104 0.063 Uiso 1 1 calc R . . C57 C 0.9153(10) 0.5149(6) 0.6600(9) 0.054(3) Uani 1 1 d . . . H57 H 0.9324 0.5394 0.6064 0.064 Uiso 1 1 calc R . . C58 C 0.9655(12) 0.5519(9) 0.7402(10) 0.059(4) Uani 1 1 d . . . H58A H 0.9323 0.5949 0.7432 0.071 Uiso 1 1 calc R . . H58B H 0.9501 0.5284 0.7943 0.071 Uiso 1 1 calc R . . C59 C 1.0812(11) 0.5597(8) 0.7364(11) 0.070(4) Uani 1 1 d . . . H59A H 1.1093 0.5807 0.7907 0.084 Uiso 1 1 calc R . . H59B H 1.0964 0.5880 0.6867 0.084 Uiso 1 1 calc R . . C60 C 1.1392(12) 0.4929(7) 0.7252(10) 0.067(4) Uani 1 1 d . . . H60A H 1.1321 0.4662 0.7780 0.081 Uiso 1 1 calc R . . H60B H 1.2153 0.5000 0.7171 0.081 Uiso 1 1 calc R . . C61 C 1.0859(12) 0.4576(8) 0.6418(12) 0.058(4) Uani 1 1 d . . . H61A H 1.0965 0.4834 0.5888 0.070 Uiso 1 1 calc R . . H61B H 1.1195 0.4152 0.6344 0.070 Uiso 1 1 calc R . . C62 C 0.9519(12) 0.3678(7) 0.5352(10) 0.045(4) Uani 1 1 d . . . H62 H 1.0269 0.3662 0.5393 0.054 Uiso 1 1 calc R . . C63 C 0.8979(12) 0.3214(7) 0.4767(10) 0.047(4) Uani 1 1 d . . . C64 C 0.9633(13) 0.2773(7) 0.4325(11) 0.052(4) Uani 1 1 d . . . H64 H 1.0375 0.2779 0.4448 0.062 Uiso 1 1 calc R . . C65 C 0.9183(15) 0.2315(8) 0.3691(12) 0.060(5) Uani 1 1 d . . . H65 H 0.9614 0.2034 0.3376 0.072 Uiso 1 1 calc R . . C66 C 0.8067(14) 0.2313(8) 0.3572(13) 0.067(5) Uani 1 1 d . . . H66 H 0.7748 0.2034 0.3146 0.080 Uiso 1 1 calc R . . C67 C 0.7405(14) 0.2708(8) 0.4059(12) 0.061(5) Uani 1 1 d . . . H67 H 0.6660 0.2680 0.3966 0.073 Uiso 1 1 calc R . . C68 C 0.7855(13) 0.3153(7) 0.4697(11) 0.048(4) Uani 1 1 d . . . C69 C 0.7335(13) 0.5487(9) 0.6811(10) 0.056(4) Uani 1 1 d . . . H69 H 0.7639 0.5819 0.7166 0.068 Uiso 1 1 calc R . . C70 C 0.6150(13) 0.5533(9) 0.6594(11) 0.057(4) Uani 1 1 d . . . C71 C 0.5650(15) 0.6121(10) 0.6832(12) 0.070(5) Uani 1 1 d . . . H71 H 0.6075 0.6444 0.7112 0.084 Uiso 1 1 calc R . . C72 C 0.4601(15) 0.6242(10) 0.6679(12) 0.076(5) Uani 1 1 d . . . H72 H 0.4276 0.6637 0.6820 0.091 Uiso 1 1 calc R . . C73 C 0.4045(13) 0.5720(9) 0.6288(11) 0.067(5) Uani 1 1 d . . . H73 H 0.3307 0.5776 0.6174 0.080 Uiso 1 1 calc R . . C74 C 0.4479(12) 0.5120(9) 0.6048(11) 0.060(4) Uani 1 1 d . . . H74 H 0.4037 0.4789 0.5809 0.072 Uiso 1 1 calc R . . C75 C 0.5589(12) 0.5025(9) 0.6172(11) 0.053(4) Uani 1 1 d . . . C76 C 0.389(3) 0.303(2) 0.407(2) 0.093(13) Uani 0.50 1 d P . . H76A H 0.4294 0.2924 0.3562 0.139 Uiso 0.50 1 calc PR . . H76B H 0.3196 0.2826 0.4017 0.139 Uiso 0.50 1 calc PR . . H76C H 0.4277 0.2874 0.4603 0.139 Uiso 0.50 1 calc PR . . C77 C 0.459(3) 0.422(2) 0.388(2) 0.092(13) Uani 0.50 1 d P . . H77A H 0.5293 0.4060 0.4048 0.138 Uiso 0.50 1 calc PR . . H77B H 0.4472 0.4633 0.4175 0.138 Uiso 0.50 1 calc PR . . H77C H 0.4532 0.4292 0.3243 0.138 Uiso 0.50 1 calc PR . . C78 C 0.279(4) 0.389(2) 0.442(2) 0.081(12) Uani 0.50 1 d P . . H78 H 0.2345 0.3554 0.4612 0.097 Uiso 0.50 1 calc PR . . C79 C 0.4231(18) 0.4988(11) 0.8766(14) 0.108(8) Uani 1 1 d . . . H79A H 0.3748 0.4621 0.8781 0.162 Uiso 1 1 calc R . . H79B H 0.4899 0.4880 0.9084 0.162 Uiso 1 1 calc R . . H79C H 0.4368 0.5090 0.8158 0.162 Uiso 1 1 calc R . . C80 C 0.4325(16) 0.6196(12) 0.9248(14) 0.109(8) Uani 1 1 d . . . H80A H 0.4437 0.6354 0.8658 0.163 Uiso 1 1 calc R . . H80B H 0.5010 0.6133 0.9563 0.163 Uiso 1 1 calc R . . H80C H 0.3909 0.6510 0.9559 0.163 Uiso 1 1 calc R . . C81 C 0.2737(16) 0.5572(13) 0.9529(13) 0.090(6) Uani 1 1 d . . . H81 H 0.2475 0.5962 0.9757 0.107 Uiso 1 1 calc R . . C82 C 0.9196(12) 0.1900(7) 0.8465(10) 0.042(4) 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 0.0323(11) 0.0386(12) 0.0459(12) -0.0003(9) 0.0005(9) 0.0002(9) Fe2 0.0353(11) 0.0366(11) 0.0453(12) -0.0010(10) 0.0022(9) 0.0018(9) Mn1 0.0370(12) 0.0332(12) 0.0529(14) -0.0003(11) 0.0008(10) 0.0008(10) Mn2 0.0358(12) 0.0390(13) 0.0521(14) 0.0024(11) 0.0017(10) 0.0009(10) O1 0.054(7) 0.063(7) 0.069(7) 0.004(6) 0.000(5) -0.021(6) O2 0.039(6) 0.042(6) 0.060(6) 0.009(5) 0.002(5) -0.004(5) O3 0.031(5) 0.042(6) 0.069(7) -0.003(5) 0.006(4) -0.002(4) O4 0.059(7) 0.031(5) 0.080(8) 0.000(5) 0.003(5) 0.016(5) O5 0.047(6) 0.056(7) 0.066(7) 0.002(6) 0.006(5) 0.002(5) O6 0.043(6) 0.050(6) 0.062(7) 0.003(5) 0.004(5) -0.008(5) O7 0.11(2) 0.12(2) 0.079(16) -0.040(16) -0.042(14) 0.059(18) O8 0.098(10) 0.123(12) 0.107(10) 0.009(9) 0.004(8) -0.039(9) N1 0.039(7) 0.054(8) 0.058(8) -0.008(7) 0.007(6) 0.004(6) N2 0.053(7) 0.047(8) 0.064(8) 0.009(7) -0.002(6) -0.009(6) N3 0.068(10) 0.083(10) 0.044(9) 0.001(8) 0.011(7) -0.019(8) N4 0.030(7) 0.051(8) 0.051(8) -0.004(6) -0.001(5) -0.004(6) N5 0.034(7) 0.037(6) 0.050(8) -0.009(6) 0.001(5) 0.001(5) N6 0.028(6) 0.050(8) 0.049(8) -0.006(6) -0.002(5) 0.004(6) N7 0.036(6) 0.042(6) 0.059(7) 0.002(6) 0.000(5) 0.004(5) N8 0.040(6) 0.041(6) 0.051(7) 0.002(6) 0.000(5) 0.004(6) N9 0.052(7) 0.043(8) 0.059(8) -0.005(6) -0.001(6) 0.006(6) N10 0.080(11) 0.065(9) 0.062(10) 0.012(8) -0.007(8) 0.016(8) N11 0.048(8) 0.050(8) 0.053(8) 0.003(6) 0.000(6) 0.005(6) N12 0.036(7) 0.046(7) 0.048(7) 0.005(6) 0.003(5) 0.001(6) N13 0.036(7) 0.034(6) 0.054(8) 0.004(6) 0.003(5) 0.005(6) N14 0.042(7) 0.045(8) 0.047(7) 0.002(6) 0.003(5) -0.007(6) N15 0.041(6) 0.042(7) 0.049(7) -0.005(6) -0.004(5) -0.001(5) N16 0.049(7) 0.043(7) 0.057(7) -0.009(6) 0.002(5) 0.010(6) N17 0.085(13) 0.122(16) 0.073(11) -0.015(12) 0.009(9) -0.030(12) N18 0.08(2) 0.09(2) 0.033(14) 0.008(15) -0.007(13) 0.05(2) C1 0.034(8) 0.042(8) 0.052(10) -0.002(8) 0.002(7) 0.001(7) C2 0.041(8) 0.048(9) 0.050(9) 0.003(8) -0.005(6) 0.003(7) C3 0.035(8) 0.058(10) 0.050(10) -0.002(8) 0.005(7) -0.004(7) C4 0.049(10) 0.062(11) 0.061(11) -0.003(9) 0.003(8) 0.007(9) C5 0.051(10) 0.091(14) 0.067(12) -0.015(10) 0.003(8) 0.026(10) C6 0.019(7) 0.073(10) 0.055(9) -0.013(8) 0.012(6) -0.001(7) C7 0.032(8) 0.068(10) 0.062(10) -0.022(8) 0.016(7) -0.008(8) C8 0.040(8) 0.047(9) 0.051(9) -0.014(7) 0.006(7) -0.010(7) C9 0.041(9) 0.046(10) 0.055(10) -0.011(8) 0.004(7) -0.004(8) C10 0.041(9) 0.043(9) 0.048(9) -0.007(7) -0.002(6) 0.000(7) C11 0.053(10) 0.052(10) 0.066(11) -0.005(8) -0.006(8) -0.002(8) C12 0.068(11) 0.047(9) 0.074(11) 0.001(9) -0.005(8) 0.031(9) C13 0.059(10) 0.065(11) 0.072(12) -0.008(9) -0.007(8) 0.018(9) C14 0.047(9) 0.066(10) 0.061(10) -0.009(9) -0.004(7) 0.019(8) C15 0.042(9) 0.079(12) 0.063(10) -0.008(9) -0.010(7) 0.015(8) C16 0.044(9) 0.076(11) 0.055(10) -0.007(8) -0.002(7) 0.004(8) C17 0.044(9) 0.062(10) 0.055(10) 0.000(9) -0.002(7) -0.001(8) C18 0.043(9) 0.057(10) 0.050(9) -0.010(8) -0.006(7) 0.008(8) C19 0.041(7) 0.052(8) 0.062(9) 0.005(7) 0.002(6) 0.003(6) C20 0.041(7) 0.053(8) 0.061(8) 0.002(6) -0.003(6) 0.001(6) C21 0.045(8) 0.061(9) 0.066(10) 0.016(8) -0.006(7) -0.003(7) C22 0.056(9) 0.077(11) 0.077(11) 0.008(8) -0.012(8) -0.001(8) C23 0.050(9) 0.071(10) 0.086(11) 0.009(9) -0.005(8) 0.004(8) C24 0.041(8) 0.055(10) 0.073(11) 0.009(9) -0.003(7) -0.003(7) C25 0.048(9) 0.051(9) 0.049(9) 0.006(8) 0.005(7) -0.001(8) C26 0.048(9) 0.046(9) 0.055(10) -0.010(8) 0.010(7) -0.004(8) C27 0.055(11) 0.067(12) 0.070(11) 0.002(9) 0.003(8) -0.005(9) C28 0.056(10) 0.069(11) 0.075(11) -0.002(8) 0.003(8) -0.014(8) C29 0.043(9) 0.071(11) 0.081(11) -0.009(9) 0.003(7) -0.022(8) C30 0.047(9) 0.067(11) 0.069(10) -0.007(9) 0.000(7) -0.010(8) C31 0.039(8) 0.049(9) 0.057(10) -0.010(8) 0.011(7) -0.001(8) C32 0.042(8) 0.047(8) 0.053(8) -0.002(8) 0.000(7) 0.004(7) C33 0.044(9) 0.035(8) 0.053(9) -0.007(7) 0.002(7) 0.000(7) C34 0.052(10) 0.042(9) 0.057(10) 0.000(8) -0.001(8) 0.002(8) C35 0.059(10) 0.045(9) 0.062(10) 0.015(7) 0.008(7) -0.010(8) C36 0.069(11) 0.040(8) 0.079(11) 0.016(8) -0.010(8) -0.007(8) C37 0.047(9) 0.051(10) 0.079(12) 0.019(8) -0.004(8) 0.002(7) C38 0.046(9) 0.041(9) 0.052(9) 0.003(7) 0.004(7) -0.001(7) C39 0.044(9) 0.044(9) 0.055(9) 0.009(8) 0.004(7) 0.003(7) C40 0.042(9) 0.048(9) 0.053(10) -0.004(8) 0.005(7) 0.011(7) C41 0.035(8) 0.039(8) 0.048(9) 0.001(7) 0.002(7) 0.000(7) C42 0.050(10) 0.055(10) 0.057(10) 0.004(8) -0.001(7) -0.011(8) C43 0.043(9) 0.064(10) 0.064(10) 0.002(8) -0.004(7) -0.009(8) C44 0.028(7) 0.060(9) 0.058(9) 0.002(8) 0.005(6) -0.003(7) C45 0.048(10) 0.070(11) 0.060(10) 0.011(8) 0.002(8) 0.006(9) C46 0.042(9) 0.049(9) 0.049(9) 0.000(8) -0.004(7) 0.005(7) C47 0.050(9) 0.036(8) 0.047(9) 0.002(7) 0.001(7) -0.001(7) C48 0.059(10) 0.038(8) 0.067(10) -0.001(7) -0.003(8) -0.005(7) C49 0.076(12) 0.052(10) 0.077(12) -0.002(9) -0.004(9) 0.003(9) C50 0.068(12) 0.062(10) 0.065(11) 0.001(8) 0.006(9) -0.017(9) C51 0.053(10) 0.050(9) 0.057(10) 0.002(7) 0.008(7) -0.016(8) C52 0.053(10) 0.067(10) 0.063(10) -0.006(8) 0.008(8) -0.011(8) C53 0.051(10) 0.075(12) 0.073(12) 0.004(10) 0.017(8) 0.005(9) C54 0.049(9) 0.043(9) 0.047(9) 0.004(7) 0.002(7) -0.008(7) C55 0.041(9) 0.057(9) 0.053(9) -0.006(8) 0.010(7) -0.001(8) C56 0.046(7) 0.049(8) 0.061(9) 0.001(6) -0.002(6) -0.001(6) C57 0.046(8) 0.049(8) 0.064(9) -0.001(6) -0.006(6) -0.007(6) C58 0.056(10) 0.058(9) 0.063(10) -0.006(8) -0.006(7) -0.004(7) C59 0.056(9) 0.067(9) 0.084(11) -0.008(9) -0.025(8) -0.012(8) C60 0.055(9) 0.059(9) 0.087(11) 0.008(8) -0.014(7) -0.011(7) C61 0.050(9) 0.051(10) 0.074(11) 0.005(9) -0.001(8) -0.003(8) C62 0.039(8) 0.044(8) 0.051(8) 0.006(7) -0.002(6) 0.001(7) C63 0.050(10) 0.038(8) 0.053(10) 0.007(7) 0.009(7) 0.003(7) C64 0.051(10) 0.039(9) 0.064(10) 0.000(8) 0.000(8) 0.012(8) C65 0.065(11) 0.039(9) 0.078(12) -0.009(8) 0.011(8) 0.001(8) C66 0.063(11) 0.052(10) 0.084(12) -0.014(8) -0.001(8) -0.005(8) C67 0.050(9) 0.047(10) 0.085(12) -0.013(8) -0.003(8) 0.001(8) C68 0.051(10) 0.032(8) 0.061(10) 0.004(7) 0.003(8) 0.000(7) C69 0.058(11) 0.054(10) 0.057(10) 0.004(9) -0.001(8) 0.003(8) C70 0.049(10) 0.058(10) 0.064(11) 0.002(9) 0.014(8) 0.018(9) C71 0.066(12) 0.069(12) 0.076(12) 0.002(10) 0.001(9) 0.005(10) C72 0.070(12) 0.078(12) 0.079(12) 0.003(10) 0.007(9) 0.022(10) C73 0.046(9) 0.083(12) 0.072(11) 0.005(9) 0.000(7) 0.020(9) C74 0.044(9) 0.070(11) 0.065(10) 0.005(9) 0.006(7) 0.009(8) C75 0.041(9) 0.055(10) 0.063(10) 0.004(9) 0.005(7) 0.013(8) C76 0.12(3) 0.11(3) 0.051(19) 0.027(19) 0.007(19) 0.04(3) C77 0.12(3) 0.10(3) 0.06(2) 0.01(2) 0.00(2) 0.04(3) C78 0.09(3) 0.10(3) 0.048(19) -0.006(18) -0.038(19) 0.01(2) C79 0.136(19) 0.113(18) 0.074(13) -0.021(12) 0.009(13) 0.020(15) C80 0.085(14) 0.137(18) 0.105(17) -0.032(14) 0.010(11) -0.038(13) C81 0.066(12) 0.126(17) 0.076(12) -0.026(12) -0.004(9) -0.009(12) C82 0.048(9) 0.036(8) 0.041(8) 0.001(7) -0.001(7) 0.001(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 Fe1 N5 1.872(12) . ? Fe1 C2 1.952(16) . ? Fe1 N4 1.957(12) . ? Fe1 N6 1.959(11) . ? Fe1 C1 1.974(16) . ? Fe1 C3 1.982(17) . ? Fe2 N13 1.891(11) . ? Fe2 C39 1.931(17) . ? Fe2 C40 1.955(16) . ? Fe2 C41 1.965(15) . ? Fe2 N12 1.972(12) . ? Fe2 N14 1.974(12) . ? Mn1 O3 1.877(9) . ? Mn1 O2 1.902(10) . ? Mn1 N8 1.993(11) . ? Mn1 N7 1.995(12) . ? Mn1 N9 2.281(13) . ? Mn1 N1 2.296(13) . ? Mn2 O6 1.875(11) . ? Mn2 O5 1.891(10) . ? Mn2 N15 1.997(12) . ? Mn2 N16 2.016(13) . ? Mn2 N2 2.298(14) 1_554 ? Mn2 N11 2.307(13) . ? O1 C9 1.275(18) . ? O2 C38 1.319(17) . ? O3 C31 1.338(19) . ? O4 C82 1.207(16) . ? O5 C75 1.275(19) . ? O6 C68 1.333(17) . ? O7 C78 1.23(4) . ? O8 C81 1.26(2) . ? N1 C1 1.141(17) . ? N2 C2 1.156(18) . ? N2 Mn2 2.298(14) 1_556 ? N3 C3 1.101(19) . ? N4 C17 1.299(18) . ? N4 C18 1.36(2) . ? N5 C9 1.361(18) . ? N5 C10 1.396(18) . ? N6 C4 1.290(19) . ? N6 C8 1.363(19) . ? N7 C25 1.280(18) . ? N7 C20 1.448(16) . ? N8 C32 1.285(18) . ? N8 C19 1.488(17) . ? N9 C39 1.150(18) . ? N10 C40 1.164(19) . ? N11 C41 1.121(17) . ? N12 C55 1.313(17) . ? N12 C54 1.372(19) . ? N13 C82 1.327(17) . ? N13 C47 1.399(18) . ? N14 C46 1.327(19) . ? N14 C42 1.361(19) . ? N15 C62 1.283(17) . ? N15 C56 1.483(17) . ? N16 C69 1.264(18) . ? N16 C57 1.483(16) . ? N17 C81 1.36(2) . ? N17 C79 1.48(3) . ? N17 C80 1.49(3) . ? N18 C78 1.34(5) . ? N18 C76 1.47(5) . ? N18 C77 1.48(5) . ? C4 C5 1.52(2) . ? C4 H4 0.9300 . ? C5 C6 1.25(2) . ? C5 H5 0.9300 . ? C6 C7 1.28(2) . ? C6 H6 0.9300 . ? C7 C8 1.391(19) . ? C7 H7 0.9300 . ? C8 C9 1.48(2) . ? C10 C11 1.38(2) . ? C10 C18 1.45(2) . ? C11 C12 1.46(2) . ? C11 H11 0.9300 . ? C12 C13 1.36(2) . ? C12 H12 0.9300 . ? C13 C14 1.39(2) . ? C13 H13 0.9300 . ? C14 C15 1.43(2) . ? C14 C18 1.44(2) . ? C15 C16 1.31(2) . ? C15 H15 0.9300 . ? C16 C17 1.39(2) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C19 C20 1.520(18) . ? C19 C24 1.533(19) . ? C19 H19 0.9800 . ? C20 C21 1.498(19) . ? C20 H20 0.9800 . ? C21 C22 1.59(2) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.50(2) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.54(2) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.38(2) . ? C25 H25 0.9300 . ? C26 C27 1.45(2) . ? C26 C31 1.46(2) . ? C27 C28 1.35(2) . ? C27 H27 0.9300 . ? C28 C29 1.41(2) . ? C28 H28 0.9300 . ? C29 C30 1.37(2) . ? C29 H29 0.9300 . ? C30 C31 1.42(2) . ? C30 H30 0.9300 . ? C32 C33 1.45(2) . ? C32 H32 0.9300 . ? C33 C34 1.42(2) . ? C33 C38 1.42(2) . ? C34 C35 1.31(2) . ? C34 H34 0.9300 . ? C35 C36 1.39(2) . ? C35 H35 0.9300 . ? C36 C37 1.38(2) . ? C36 H36 0.9300 . ? C37 C38 1.37(2) . ? C37 H37 0.9300 . ? C42 C43 1.34(2) . ? C42 H42 0.9300 . ? C43 C44 1.29(2) . ? C43 H43 0.9300 . ? C44 C45 1.27(2) . ? C44 H44 0.9300 . ? C45 C46 1.42(2) . ? C45 H45 0.9300 . ? C46 C82 1.50(2) . ? C47 C48 1.33(2) . ? C47 C54 1.41(2) . ? C48 C49 1.33(2) . ? C48 H48 0.9300 . ? C49 C50 1.37(2) . ? C49 H49 0.9300 . ? C50 C51 1.48(2) . ? C50 H50 0.9300 . ? C51 C52 1.40(2) . ? C51 C54 1.41(2) . ? C52 C53 1.36(2) . ? C52 H52 0.9300 . ? C53 C55 1.42(2) . ? C53 H53 0.9300 . ? C55 H55 0.9300 . ? C56 C57 1.496(17) . ? C56 C61 1.512(19) . ? C56 H56 0.9800 . ? C57 C58 1.527(18) . ? C57 H57 0.9800 . ? C58 C59 1.45(2) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 C60 1.55(2) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 C61 1.56(2) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C63 1.43(2) . ? C62 H62 0.9300 . ? C63 C68 1.40(2) . ? C63 C64 1.401(19) . ? C64 C65 1.43(2) . ? C64 H64 0.9300 . ? C65 C66 1.39(2) . ? C65 H65 0.9300 . ? C66 C67 1.39(2) . ? C66 H66 0.9300 . ? C67 C68 1.41(2) . ? C67 H67 0.9300 . ? C69 C70 1.49(2) . ? C69 H69 0.9300 . ? C70 C75 1.38(2) . ? C70 C71 1.41(2) . ? C71 C72 1.33(2) . ? C71 H71 0.9300 . ? C72 C73 1.38(3) . ? C72 H72 0.9300 . ? C73 C74 1.39(2) . ? C73 H73 0.9300 . ? C74 C75 1.39(2) . ? C74 H74 0.9300 . ? C76 H76A 0.9600 . ? C76 H76B 0.9600 . ? C76 H76C 0.9600 . ? C77 H77A 0.9600 . ? C77 H77B 0.9600 . ? C77 H77C 0.9600 . ? C78 H78 0.9300 . ? C79 H79A 0.9600 . ? C79 H79B 0.9600 . ? C79 H79C 0.9600 . ? C80 H80A 0.9600 . ? C80 H80B 0.9600 . ? C80 H80C 0.9600 . ? C81 H81 0.9300 . ? 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 N5 Fe1 C2 177.9(6) . . ? N5 Fe1 N4 83.5(5) . . ? C2 Fe1 N4 97.7(6) . . ? N5 Fe1 N6 82.9(5) . . ? C2 Fe1 N6 95.9(6) . . ? N4 Fe1 N6 166.1(6) . . ? N5 Fe1 C1 93.3(6) . . ? C2 Fe1 C1 85.0(6) . . ? N4 Fe1 C1 91.0(5) . . ? N6 Fe1 C1 92.7(5) . . ? N5 Fe1 C3 94.7(6) . . ? C2 Fe1 C3 87.0(6) . . ? N4 Fe1 C3 89.1(6) . . ? N6 Fe1 C3 89.1(5) . . ? C1 Fe1 C3 172.0(6) . . ? N13 Fe2 C39 178.4(6) . . ? N13 Fe2 C40 93.6(6) . . ? C39 Fe2 C40 84.9(6) . . ? N13 Fe2 C41 96.7(6) . . ? C39 Fe2 C41 84.9(6) . . ? C40 Fe2 C41 169.7(6) . . ? N13 Fe2 N12 83.7(5) . . ? C39 Fe2 N12 95.9(6) . . ? C40 Fe2 N12 88.4(6) . . ? C41 Fe2 N12 91.6(5) . . ? N13 Fe2 N14 82.1(5) . . ? C39 Fe2 N14 98.3(6) . . ? C40 Fe2 N14 90.1(6) . . ? C41 Fe2 N14 92.3(5) . . ? N12 Fe2 N14 165.6(5) . . ? O3 Mn1 O2 94.6(4) . . ? O3 Mn1 N8 172.0(5) . . ? O2 Mn1 N8 92.7(5) . . ? O3 Mn1 N7 91.0(5) . . ? O2 Mn1 N7 174.4(4) . . ? N8 Mn1 N7 81.6(5) . . ? O3 Mn1 N9 90.6(4) . . ? O2 Mn1 N9 92.4(4) . . ? N8 Mn1 N9 85.8(5) . . ? N7 Mn1 N9 87.2(5) . . ? O3 Mn1 N1 93.9(4) . . ? O2 Mn1 N1 91.3(5) . . ? N8 Mn1 N1 89.3(5) . . ? N7 Mn1 N1 88.6(5) . . ? N9 Mn1 N1 174.0(5) . . ? O6 Mn2 O5 94.1(5) . . ? O6 Mn2 N15 92.8(5) . . ? O5 Mn2 N15 173.0(5) . . ? O6 Mn2 N16 173.9(5) . . ? O5 Mn2 N16 91.5(5) . . ? N15 Mn2 N16 81.6(5) . . ? O6 Mn2 N2 92.9(5) . 1_554 ? O5 Mn2 N2 91.5(5) . 1_554 ? N15 Mn2 N2 87.1(5) . 1_554 ? N16 Mn2 N2 84.3(5) . 1_554 ? O6 Mn2 N11 91.4(5) . . ? O5 Mn2 N11 94.6(5) . . ? N15 Mn2 N11 86.3(5) . . ? N16 Mn2 N11 90.7(5) . . ? N2 Mn2 N11 172.2(5) 1_554 . ? C38 O2 Mn1 130.1(9) . . ? C31 O3 Mn1 125.9(9) . . ? C75 O5 Mn2 130.3(11) . . ? C68 O6 Mn2 127.6(10) . . ? C1 N1 Mn1 163.1(13) . . ? C2 N2 Mn2 148.3(13) . 1_556 ? C17 N4 C18 116.4(14) . . ? C17 N4 Fe1 131.0(12) . . ? C18 N4 Fe1 112.5(10) . . ? C9 N5 C10 125.0(13) . . ? C9 N5 Fe1 118.2(10) . . ? C10 N5 Fe1 116.6(9) . . ? C4 N6 C8 118.6(13) . . ? C4 N6 Fe1 128.3(12) . . ? C8 N6 Fe1 113.0(10) . . ? C25 N7 C20 122.5(13) . . ? C25 N7 Mn1 126.0(11) . . ? C20 N7 Mn1 111.4(9) . . ? C32 N8 C19 122.9(11) . . ? C32 N8 Mn1 124.6(10) . . ? C19 N8 Mn1 112.5(9) . . ? C39 N9 Mn1 151.9(13) . . ? C41 N11 Mn2 171.4(13) . . ? C55 N12 C54 118.6(14) . . ? C55 N12 Fe2 130.9(11) . . ? C54 N12 Fe2 110.5(10) . . ? C82 N13 C47 125.1(12) . . ? C82 N13 Fe2 118.8(10) . . ? C47 N13 Fe2 116.0(9) . . ? C46 N14 C42 117.0(13) . . ? C46 N14 Fe2 112.7(10) . . ? C42 N14 Fe2 130.2(11) . . ? C62 N15 C56 122.7(12) . . ? C62 N15 Mn2 124.7(10) . . ? C56 N15 Mn2 111.7(9) . . ? C69 N16 C57 121.3(13) . . ? C69 N16 Mn2 123.5(12) . . ? C57 N16 Mn2 113.9(8) . . ? C81 N17 C79 125(2) . . ? C81 N17 C80 115(2) . . ? C79 N17 C80 119.9(17) . . ? C78 N18 C76 110(4) . . ? C78 N18 C77 126(3) . . ? C76 N18 C77 124(3) . . ? N1 C1 Fe1 176.0(13) . . ? N2 C2 Fe1 177.6(15) . . ? N3 C3 Fe1 179.6(16) . . ? N6 C4 C5 114.7(16) . . ? N6 C4 H4 122.6 . . ? C5 C4 H4 122.6 . . ? C6 C5 C4 126.7(17) . . ? C6 C5 H5 116.7 . . ? C4 C5 H5 116.7 . . ? C5 C6 C7 114.6(15) . . ? C5 C6 H6 122.7 . . ? C7 C6 H6 122.7 . . ? C6 C7 C8 124.2(17) . . ? C6 C7 H7 117.9 . . ? C8 C7 H7 117.9 . . ? N6 C8 C7 121.0(16) . . ? N6 C8 C9 114.6(13) . . ? C7 C8 C9 124.3(15) . . ? O1 C9 N5 126.4(15) . . ? O1 C9 C8 122.6(14) . . ? N5 C9 C8 111.0(13) . . ? C11 C10 N5 129.2(15) . . ? C11 C10 C18 119.5(15) . . ? N5 C10 C18 111.2(13) . . ? C10 C11 C12 117.4(16) . . ? C10 C11 H11 121.3 . . ? C12 C11 H11 121.3 . . ? C13 C12 C11 122.2(15) . . ? C13 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? C12 C13 C14 122.6(17) . . ? C12 C13 H13 118.7 . . ? C14 C13 H13 118.7 . . ? C13 C14 C15 128.1(17) . . ? C13 C14 C18 116.6(18) . . ? C15 C14 C18 115.1(16) . . ? C16 C15 C14 121.1(16) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C17 118.7(17) . . ? C15 C16 H16 120.7 . . ? C17 C16 H16 120.7 . . ? N4 C17 C16 125.9(17) . . ? N4 C17 H17 117.0 . . ? C16 C17 H17 117.0 . . ? N4 C18 C14 122.6(15) . . ? N4 C18 C10 116.0(13) . . ? C14 C18 C10 121.5(16) . . ? N8 C19 C20 106.2(10) . . ? N8 C19 C24 115.0(12) . . ? C20 C19 C24 112.0(12) . . ? N8 C19 H19 107.8 . . ? C20 C19 H19 107.8 . . ? C24 C19 H19 107.8 . . ? N7 C20 C21 115.1(11) . . ? N7 C20 C19 105.3(10) . . ? C21 C20 C19 109.8(12) . . ? N7 C20 H20 108.8 . . ? C21 C20 H20 108.8 . . ? C19 C20 H20 108.8 . . ? C20 C21 C22 109.2(12) . . ? C20 C21 H21A 109.8 . . ? C22 C21 H21A 109.8 . . ? C20 C21 H21B 109.8 . . ? C22 C21 H21B 109.8 . . ? H21A C21 H21B 108.3 . . ? C23 C22 C21 110.5(13) . . ? C23 C22 H22A 109.5 . . ? C21 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C22 C23 C24 109.5(13) . . ? C22 C23 H23A 109.8 . . ? C24 C23 H23A 109.8 . . ? C22 C23 H23B 109.8 . . ? C24 C23 H23B 109.8 . . ? H23A C23 H23B 108.2 . . ? C19 C24 C23 109.2(12) . . ? C19 C24 H24A 109.8 . . ? C23 C24 H24A 109.8 . . ? C19 C24 H24B 109.8 . . ? C23 C24 H24B 109.8 . . ? H24A C24 H24B 108.3 . . ? N7 C25 C26 123.5(15) . . ? N7 C25 H25 118.2 . . ? C26 C25 H25 118.2 . . ? C25 C26 C27 119.0(15) . . ? C25 C26 C31 125.4(14) . . ? C27 C26 C31 115.6(14) . . ? C28 C27 C26 120.2(18) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C29 124.8(17) . . ? C27 C28 H28 117.6 . . ? C29 C28 H28 117.6 . . ? C30 C29 C28 116.9(15) . . ? C30 C29 H29 121.5 . . ? C28 C29 H29 121.5 . . ? C29 C30 C31 122.5(17) . . ? C29 C30 H30 118.8 . . ? C31 C30 H30 118.8 . . ? O3 C31 C30 118.9(15) . . ? O3 C31 C26 121.2(13) . . ? C30 C31 C26 119.9(15) . . ? N8 C32 C33 125.9(14) . . ? N8 C32 H32 117.0 . . ? C33 C32 H32 117.0 . . ? C34 C33 C38 117.4(14) . . ? C34 C33 C32 117.7(14) . . ? C38 C33 C32 124.4(14) . . ? C35 C34 C33 122.8(16) . . ? C35 C34 H34 118.6 . . ? C33 C34 H34 118.6 . . ? C34 C35 C36 119.1(15) . . ? C34 C35 H35 120.5 . . ? C36 C35 H35 120.5 . . ? C37 C36 C35 120.9(16) . . ? C37 C36 H36 119.5 . . ? C35 C36 H36 119.5 . . ? C38 C37 C36 120.5(16) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? O2 C38 C37 119.0(15) . . ? O2 C38 C33 121.9(14) . . ? C37 C38 C33 118.8(15) . . ? N9 C39 Fe2 178.3(14) . . ? N10 C40 Fe2 178.2(15) . . ? N11 C41 Fe2 177.9(14) . . ? C43 C42 N14 122.7(17) . . ? C43 C42 H42 118.6 . . ? N14 C42 H42 118.6 . . ? C44 C43 C42 119.5(17) . . ? C44 C43 H43 120.2 . . ? C42 C43 H43 120.2 . . ? C45 C44 C43 120.8(16) . . ? C45 C44 H44 119.6 . . ? C43 C44 H44 119.6 . . ? C44 C45 C46 122.5(17) . . ? C44 C45 H45 118.8 . . ? C46 C45 H45 118.8 . . ? N14 C46 C45 117.3(15) . . ? N14 C46 C82 115.6(13) . . ? C45 C46 C82 127.1(15) . . ? C48 C47 N13 128.1(15) . . ? C48 C47 C54 120.6(15) . . ? N13 C47 C54 111.3(12) . . ? C49 C48 C47 121.8(17) . . ? C49 C48 H48 119.1 . . ? C47 C48 H48 119.1 . . ? C48 C49 C50 124.0(17) . . ? C48 C49 H49 118.0 . . ? C50 C49 H49 118.0 . . ? C49 C50 C51 116.2(16) . . ? C49 C50 H50 121.9 . . ? C51 C50 H50 121.9 . . ? C52 C51 C54 117.5(15) . . ? C52 C51 C50 123.9(16) . . ? C54 C51 C50 118.4(15) . . ? C53 C52 C51 119.0(16) . . ? C53 C52 H52 120.5 . . ? C51 C52 H52 120.5 . . ? C52 C53 C55 120.6(16) . . ? C52 C53 H53 119.7 . . ? C55 C53 H53 119.7 . . ? N12 C54 C51 122.6(14) . . ? N12 C54 C47 118.5(13) . . ? C51 C54 C47 118.9(14) . . ? N12 C55 C53 121.4(16) . . ? N12 C55 H55 119.3 . . ? C53 C55 H55 119.3 . . ? N15 C56 C57 108.2(11) . . ? N15 C56 C61 115.6(11) . . ? C57 C56 C61 108.8(12) . . ? N15 C56 H56 108.0 . . ? C57 C56 H56 108.0 . . ? C61 C56 H56 108.0 . . ? N16 C57 C56 107.0(10) . . ? N16 C57 C58 117.5(12) . . ? C56 C57 C58 109.8(12) . . ? N16 C57 H57 107.4 . . ? C56 C57 H57 107.4 . . ? C58 C57 H57 107.4 . . ? C59 C58 C57 112.8(13) . . ? C59 C58 H58A 109.0 . . ? C57 C58 H58A 109.0 . . ? C59 C58 H58B 109.0 . . ? C57 C58 H58B 109.0 . . ? H58A C58 H58B 107.8 . . ? C58 C59 C60 111.9(13) . . ? C58 C59 H59A 109.2 . . ? C60 C59 H59A 109.2 . . ? C58 C59 H59B 109.2 . . ? C60 C59 H59B 109.2 . . ? H59A C59 H59B 107.9 . . ? C59 C60 C61 108.2(12) . . ? C59 C60 H60A 110.1 . . ? C61 C60 H60A 110.1 . . ? C59 C60 H60B 110.1 . . ? C61 C60 H60B 110.1 . . ? H60A C60 H60B 108.4 . . ? C56 C61 C60 109.7(12) . . ? C56 C61 H61A 109.7 . . ? C60 C61 H61A 109.7 . . ? C56 C61 H61B 109.7 . . ? C60 C61 H61B 109.7 . . ? H61A C61 H61B 108.2 . . ? N15 C62 C63 126.3(14) . . ? N15 C62 H62 116.8 . . ? C63 C62 H62 116.8 . . ? C68 C63 C64 120.5(15) . . ? C68 C63 C62 122.5(14) . . ? C64 C63 C62 116.8(15) . . ? C63 C64 C65 121.4(16) . . ? C63 C64 H64 119.3 . . ? C65 C64 H64 119.3 . . ? C66 C65 C64 116.2(16) . . ? C66 C65 H65 121.9 . . ? C64 C65 H65 121.9 . . ? C67 C66 C65 123.0(17) . . ? C67 C66 H66 118.5 . . ? C65 C66 H66 118.5 . . ? C66 C67 C68 120.5(16) . . ? C66 C67 H67 119.8 . . ? C68 C67 H67 119.8 . . ? O6 C68 C63 125.3(15) . . ? O6 C68 C67 116.8(15) . . ? C63 C68 C67 117.7(15) . . ? N16 C69 C70 127.0(16) . . ? N16 C69 H69 116.5 . . ? C70 C69 H69 116.5 . . ? C75 C70 C71 122.6(16) . . ? C75 C70 C69 121.3(14) . . ? C71 C70 C69 116.1(17) . . ? C72 C71 C70 124(2) . . ? C72 C71 H71 118.2 . . ? C70 C71 H71 118.2 . . ? C71 C72 C73 113.1(18) . . ? C71 C72 H72 123.5 . . ? C73 C72 H72 123.5 . . ? C72 C73 C74 126.6(16) . . ? C72 C73 H73 116.7 . . ? C74 C73 H73 116.7 . . ? C73 C74 C75 118.7(17) . . ? C73 C74 H74 120.6 . . ? C75 C74 H74 120.6 . . ? O5 C75 C70 124.5(14) . . ? O5 C75 C74 120.2(17) . . ? C70 C75 C74 115.2(15) . . ? N18 C76 H76A 109.5 . . ? N18 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? N18 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? N18 C77 H77A 109.5 . . ? N18 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? N18 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? O7 C78 N18 120(4) . . ? O7 C78 H78 120.2 . . ? N18 C78 H78 120.2 . . ? N17 C79 H79A 109.5 . . ? N17 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? N17 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? N17 C80 H80A 109.5 . . ? N17 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? N17 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? O8 C81 N17 121(2) . . ? O8 C81 H81 119.4 . . ? N17 C81 H81 119.4 . . ? O4 C82 N13 131.3(14) . . ? O4 C82 C46 118.3(14) . . ? N13 C82 C46 110.3(13) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.296 _refine_diff_density_min -0.561 _refine_diff_density_rms 0.109 _database_code_depnum_ccdc_archive 'CCDC 951680'