# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2009 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Hui-Zhong Kou' _publ_contact_author_email kouhz@mail.tsinghua.edu.cn _publ_section_title ; Cyanide-bridged 1D Mn(III)-Fe(III) bimetallic complexes: synthesis, crystal structure and magnetic properties ; loop_ _publ_author_name 'Hui-Zhong Kou.' 'Ai-Li Cui.' 'Zhong-Hai Ni.' 'Cai-Ming Liu.' 'Deqing Zhang.' # Attachment '- NJC-rev-2.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 744627' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37.35 H26.01 Cl3 Fe Mn N8.67 O4.50' _chemical_formula_weight 885.37 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' Cl Cl 0.1484 0.1585 '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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 10.267(5) _cell_length_b 13.751(6) _cell_length_c 29.045(13) _cell_angle_alpha 90.00 _cell_angle_beta 95.637(3) _cell_angle_gamma 90.00 _cell_volume 4081(3) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 8740 _cell_measurement_theta_min 3.0448 _cell_measurement_theta_max 27.4835 _exptl_crystal_description platelet _exptl_crystal_colour brown _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1791 _exptl_absorpt_coefficient_mu 0.912 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8146 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'Rigaku Saturn70 CCD (4x4 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_decay_% ? _diffrn_reflns_number 39014 _diffrn_reflns_av_R_equivalents 0.0853 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7980 _reflns_number_gt 6310 _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 'XP (Sheldrick, 1998)' _computing_publication_material 'XP (Sheldrick, 1998)' _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^)+(0.1208P)^2^+8.5537P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7980 _refine_ls_number_parameters 515 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0931 _refine_ls_R_factor_gt 0.0775 _refine_ls_wR_factor_ref 0.2284 _refine_ls_wR_factor_gt 0.2129 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 0.62160(6) 0.26441(5) 0.062072(19) 0.0177(2) Uani 1 1 d . . . Mn1 Mn 1.12425(6) 0.29127(5) 0.06177(2) 0.0163(2) Uani 1 1 d . . . Cl1 Cl 0.5507(2) -0.19379(12) 0.14322(7) 0.0657(5) Uani 1 1 d . . . Cl3 Cl 1.15781(11) 0.34033(10) 0.30907(4) 0.0326(3) Uani 1 1 d . . . Cl4 Cl 1.08363(18) 0.33708(11) -0.18662(4) 0.0498(4) Uani 1 1 d . . . O1 O 0.7330(4) 0.0884(3) -0.03588(14) 0.0468(10) Uani 1 1 d . . . O2 O 0.4862(4) 0.1711(3) 0.17873(12) 0.0462(10) Uani 1 1 d . . . O3 O 1.0712(3) 0.3794(2) 0.01385(10) 0.0202(6) Uani 1 1 d . . . O4 O 1.1731(3) 0.3851(2) 0.10859(10) 0.0211(7) Uani 1 1 d . . . N1 N 0.9219(4) 0.2807(3) 0.08554(13) 0.0229(8) Uani 1 1 d . . . N2 N 0.3254(4) 0.2893(3) 0.03505(13) 0.0249(9) Uani 1 1 d . . . N3 N 0.5899(4) 0.3649(3) 0.10932(13) 0.0269(9) Uani 1 1 d . . . N4 N 0.5798(4) 0.1781(3) 0.10905(13) 0.0263(9) Uani 1 1 d . . . N5 N 0.6462(4) 0.1481(3) 0.02961(13) 0.0262(9) Uani 1 1 d . . . N6 N 0.6622(4) 0.3250(3) 0.00275(13) 0.0225(8) Uani 1 1 d . . . N7 N 1.0843(3) 0.1791(3) 0.01844(12) 0.0196(8) Uani 1 1 d . . . N8 N 1.1792(4) 0.1828(3) 0.10544(12) 0.0199(8) Uani 1 1 d . . . N9 N 0.9394(14) 0.9715(7) 0.1248(4) 0.107(5) Uani 0.67 1 d P . . C1 C 0.8096(4) 0.2750(3) 0.08005(14) 0.0182(9) Uani 1 1 d . . . C2 C 0.4361(4) 0.2797(3) 0.04197(14) 0.0187(9) Uani 1 1 d . . . C3 C 0.6605(5) 0.4184(4) -0.01026(17) 0.0308(11) Uani 1 1 d . . . H3A H 0.6340 0.4647 0.0102 0.037 Uiso 1 1 calc R . . C4 C 0.6958(5) 0.4494(5) -0.0521(2) 0.0435(15) Uani 1 1 d . . . H4A H 0.6924 0.5150 -0.0600 0.052 Uiso 1 1 calc R . . C5 C 0.7361(6) 0.3815(5) -0.0819(2) 0.0496(16) Uani 1 1 d . . . H5A H 0.7631 0.4007 -0.1101 0.059 Uiso 1 1 calc R . . C6 C 0.7367(5) 0.2855(5) -0.07021(18) 0.0410(14) Uani 1 1 d . . . H6A H 0.7625 0.2389 -0.0907 0.049 Uiso 1 1 calc R . . C7 C 0.6984(5) 0.2574(4) -0.02716(16) 0.0283(11) Uani 1 1 d . . . C8 C 0.6952(5) 0.1550(4) -0.01183(16) 0.0282(11) Uani 1 1 d . . . C9 C 0.6254(4) 0.0621(3) 0.05385(17) 0.0270(10) Uani 1 1 d . . . C10 C 0.6376(5) -0.0324(4) 0.0370(2) 0.0382(13) Uani 1 1 d . . . H10A H 0.6609 -0.0424 0.0072 0.046 Uiso 1 1 calc R . . C11 C 0.6148(6) -0.1105(4) 0.0647(2) 0.0453(15) Uani 1 1 d . . . H11A H 0.6253 -0.1736 0.0543 0.054 Uiso 1 1 calc R . . C12 C 0.5776(6) -0.0944(4) 0.1069(2) 0.0443(15) Uani 1 1 d . . . C13 C 0.5602(6) -0.0005(4) 0.1258(2) 0.0417(14) Uani 1 1 d . . . H13A H 0.5325 0.0077 0.1551 0.050 Uiso 1 1 calc R . . C14 C 0.5868(5) 0.0789(4) 0.09811(18) 0.0321(11) Uani 1 1 d . . . C15 C 0.5312(5) 0.2157(4) 0.14706(16) 0.0329(12) Uani 1 1 d . . . C16 C 0.5384(5) 0.3235(4) 0.14651(16) 0.0313(12) Uani 1 1 d . . . C17 C 0.4997(5) 0.3789(5) 0.18242(18) 0.0409(14) Uani 1 1 d . . . H17A H 0.4617 0.3492 0.2066 0.049 Uiso 1 1 calc R . . C18 C 0.5172(6) 0.4761(5) 0.18236(19) 0.0503(17) Uani 1 1 d . . . H18A H 0.4906 0.5138 0.2063 0.060 Uiso 1 1 calc R . . C19 C 0.5750(6) 0.5197(5) 0.1464(2) 0.0472(16) Uani 1 1 d . . . H19A H 0.5911 0.5862 0.1465 0.057 Uiso 1 1 calc R . . C20 C 0.6089(5) 0.4607(4) 0.10960(19) 0.0353(12) Uani 1 1 d . . . H20A H 0.6454 0.4895 0.0849 0.042 Uiso 1 1 calc R . . C21 C 1.0774(4) 0.3662(3) -0.03059(14) 0.0198(9) Uani 1 1 d . . . C22 C 1.0780(4) 0.4487(3) -0.05978(15) 0.0228(9) Uani 1 1 d . . . H22A H 1.0764 0.5105 -0.0468 0.027 Uiso 1 1 calc R . . C23 C 1.0809(5) 0.4397(4) -0.10643(16) 0.0265(10) Uani 1 1 d . . . H23A H 1.0826 0.4950 -0.1248 0.032 Uiso 1 1 calc R . . C24 C 1.0812(5) 0.3476(4) -0.12661(16) 0.0309(11) Uani 1 1 d . . . C25 C 1.0789(5) 0.2647(4) -0.09985(16) 0.0281(11) Uani 1 1 d . . . H25A H 1.0780 0.2036 -0.1136 0.034 Uiso 1 1 calc R . . C26 C 1.0780(5) 0.2737(3) -0.05178(15) 0.0223(10) Uani 1 1 d . . . C27 C 1.0751(4) 0.1847(3) -0.02571(15) 0.0229(10) Uani 1 1 d . . . H27A H 1.0658 0.1268 -0.0423 0.027 Uiso 1 1 calc R . . C28 C 1.0829(5) 0.0851(3) 0.04286(16) 0.0249(10) Uani 1 1 d . . . H28A H 1.0976 0.0321 0.0219 0.030 Uiso 1 1 calc R . . H28B H 0.9991 0.0752 0.0549 0.030 Uiso 1 1 calc R . . C29 C 1.1917(5) 0.0887(3) 0.08214(16) 0.0246(10) Uani 1 1 d . . . H29A H 1.1828 0.0356 0.1036 0.029 Uiso 1 1 calc R . . H29B H 1.2764 0.0836 0.0702 0.029 Uiso 1 1 calc R . . C30 C 1.1921(4) 0.1900(3) 0.14968(15) 0.0221(9) Uani 1 1 d . . . H30A H 1.2099 0.1334 0.1666 0.027 Uiso 1 1 calc R . . C31 C 1.1813(4) 0.2781(3) 0.17487(14) 0.0214(9) Uani 1 1 d . . . C32 C 1.1813(4) 0.2710(4) 0.22367(15) 0.0257(10) Uani 1 1 d . . . H32A H 1.1900 0.2103 0.2378 0.031 Uiso 1 1 calc R . . C33 C 1.1687(4) 0.3520(4) 0.25003(15) 0.0259(10) Uani 1 1 d . . . C34 C 1.1628(4) 0.4443(4) 0.22940(16) 0.0268(10) Uani 1 1 d . . . H34A H 1.1569 0.4996 0.2475 0.032 Uiso 1 1 calc R . . C35 C 1.1657(5) 0.4531(4) 0.18249(15) 0.0261(10) Uani 1 1 d . . . H35A H 1.1634 0.5147 0.1693 0.031 Uiso 1 1 calc R . . C36 C 1.1721(4) 0.3703(3) 0.15352(14) 0.0207(9) Uani 1 1 d . . . C37 C 0.9137(13) 1.0229(8) 0.1538(4) 0.069(3) Uani 0.67 1 d P . . C38 C 0.885(2) 1.0885(11) 0.1851(4) 0.105(6) Uani 0.67 1 d P . . O1W O 0.4176(15) 0.0604(8) 0.2465(4) 0.115(6) Uani 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 Fe1 0.0110(4) 0.0237(4) 0.0181(3) -0.0016(2) 0.0007(2) 0.0010(2) Mn1 0.0122(4) 0.0219(4) 0.0143(3) -0.0021(2) -0.0004(2) 0.0012(3) Cl1 0.0850(14) 0.0419(9) 0.0697(11) 0.0180(8) 0.0048(10) -0.0081(9) Cl3 0.0212(6) 0.0618(9) 0.0143(5) -0.0052(5) -0.0001(4) 0.0007(6) Cl4 0.0792(11) 0.0532(9) 0.0177(6) 0.0011(5) 0.0091(6) 0.0081(8) O1 0.051(3) 0.047(2) 0.044(2) -0.0136(18) 0.0114(19) 0.017(2) O2 0.033(2) 0.076(3) 0.031(2) 0.0115(19) 0.0095(16) 0.005(2) O3 0.0171(16) 0.0256(16) 0.0174(14) -0.0006(12) -0.0010(11) 0.0047(13) O4 0.0204(16) 0.0259(17) 0.0169(14) -0.0018(12) 0.0006(12) -0.0025(13) N1 0.016(2) 0.029(2) 0.0237(19) -0.0022(15) 0.0033(15) 0.0041(16) N2 0.016(2) 0.033(2) 0.025(2) -0.0042(16) 0.0004(15) -0.0009(17) N3 0.0117(19) 0.040(2) 0.028(2) -0.0104(17) -0.0032(15) 0.0040(17) N4 0.0146(19) 0.041(2) 0.0227(19) 0.0048(17) -0.0016(15) 0.0005(17) N5 0.020(2) 0.030(2) 0.027(2) -0.0061(16) -0.0036(16) 0.0051(17) N6 0.0130(19) 0.029(2) 0.0247(19) 0.0013(16) 0.0000(14) 0.0009(16) N7 0.0115(18) 0.0238(19) 0.0230(18) -0.0033(15) -0.0011(14) 0.0003(15) N8 0.0152(19) 0.025(2) 0.0197(17) -0.0026(14) 0.0007(14) 0.0035(15) N9 0.175(13) 0.048(6) 0.115(9) -0.031(6) 0.107(9) -0.042(7) C1 0.017(2) 0.021(2) 0.017(2) -0.0039(16) 0.0026(16) 0.0068(18) C2 0.019(2) 0.020(2) 0.017(2) -0.0046(16) 0.0018(17) -0.0031(17) C3 0.024(3) 0.030(3) 0.036(3) 0.009(2) -0.007(2) -0.006(2) C4 0.024(3) 0.056(4) 0.048(3) 0.024(3) -0.006(2) -0.009(3) C5 0.030(3) 0.077(5) 0.043(3) 0.024(3) 0.003(2) -0.004(3) C6 0.025(3) 0.069(4) 0.029(3) -0.002(3) 0.004(2) 0.004(3) C7 0.017(2) 0.043(3) 0.025(2) -0.001(2) 0.0018(18) 0.003(2) C8 0.021(2) 0.036(3) 0.027(2) -0.006(2) 0.0003(19) 0.007(2) C9 0.017(2) 0.022(2) 0.040(3) 0.0007(19) -0.005(2) -0.0004(19) C10 0.026(3) 0.033(3) 0.053(3) -0.006(2) -0.010(2) 0.003(2) C11 0.040(4) 0.032(3) 0.061(4) 0.001(3) -0.010(3) 0.000(3) C12 0.038(3) 0.023(3) 0.068(4) 0.011(3) -0.014(3) -0.008(2) C13 0.032(3) 0.045(3) 0.046(3) 0.017(3) -0.003(2) -0.005(3) C14 0.017(2) 0.035(3) 0.042(3) 0.003(2) -0.008(2) -0.004(2) C15 0.016(2) 0.064(4) 0.017(2) 0.002(2) -0.0020(18) 0.003(2) C16 0.014(2) 0.058(3) 0.021(2) -0.007(2) -0.0012(18) 0.002(2) C17 0.019(3) 0.071(4) 0.033(3) -0.020(3) 0.000(2) 0.005(3) C18 0.030(3) 0.087(5) 0.035(3) -0.032(3) 0.002(2) 0.011(3) C19 0.033(3) 0.046(4) 0.059(4) -0.028(3) -0.011(3) 0.012(3) C20 0.021(3) 0.038(3) 0.045(3) -0.012(2) -0.006(2) 0.006(2) C21 0.010(2) 0.030(2) 0.019(2) -0.0021(17) -0.0009(16) 0.0006(18) C22 0.018(2) 0.027(2) 0.023(2) 0.0016(18) 0.0036(17) 0.0046(19) C23 0.023(2) 0.032(3) 0.025(2) 0.0047(19) 0.0032(19) 0.003(2) C24 0.034(3) 0.042(3) 0.017(2) 0.0003(19) 0.0036(19) 0.003(2) C25 0.033(3) 0.026(3) 0.025(2) -0.0051(19) 0.001(2) 0.003(2) C26 0.019(2) 0.027(2) 0.020(2) -0.0023(17) -0.0001(17) -0.0012(19) C27 0.019(2) 0.027(2) 0.022(2) -0.0086(18) 0.0001(17) -0.0009(19) C28 0.022(2) 0.023(2) 0.030(2) -0.0039(18) 0.0037(19) -0.0015(19) C29 0.022(2) 0.024(2) 0.027(2) -0.0036(18) 0.0000(18) 0.0041(19) C30 0.012(2) 0.030(2) 0.023(2) 0.0037(18) -0.0040(17) 0.0023(18) C31 0.013(2) 0.034(3) 0.017(2) -0.0016(17) -0.0016(16) -0.0008(18) C32 0.016(2) 0.042(3) 0.019(2) 0.0028(19) 0.0006(17) 0.002(2) C33 0.014(2) 0.048(3) 0.015(2) -0.0048(19) -0.0009(16) -0.002(2) C34 0.018(2) 0.039(3) 0.023(2) -0.011(2) 0.0038(18) -0.002(2) C35 0.022(2) 0.033(3) 0.024(2) -0.0060(19) 0.0037(18) -0.004(2) C36 0.012(2) 0.033(3) 0.0164(19) -0.0060(17) -0.0005(16) -0.0036(18) C37 0.094(9) 0.050(6) 0.066(7) 0.002(5) 0.023(6) -0.014(6) C38 0.189(18) 0.076(9) 0.054(7) -0.013(6) 0.027(9) 0.024(10) O1W 0.236(17) 0.078(7) 0.038(5) -0.018(5) 0.044(9) -0.090(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 Fe1 N5 1.886(4) . ? Fe1 N4 1.889(4) . ? Fe1 C2 1.947(5) . ? Fe1 C1 1.955(5) . ? Fe1 N6 1.994(4) . ? Fe1 N3 1.996(4) . ? Mn1 O3 1.885(3) . ? Mn1 O4 1.906(3) . ? Mn1 N8 2.003(4) . ? Mn1 N7 2.008(4) . ? Mn1 N1 2.258(4) . ? Mn1 N2 2.277(4) 1_655 ? Cl1 C12 1.764(6) . ? Cl3 C33 1.737(4) . ? Cl4 C24 1.751(5) . ? O1 C8 1.237(6) . ? O2 C15 1.233(6) . ? O3 C21 1.311(5) . ? O4 C36 1.322(5) . ? N1 C1 1.151(6) . ? N2 C2 1.142(6) . ? N2 Mn1 2.277(4) 1_455 ? N3 C20 1.332(7) . ? N3 C16 1.372(6) . ? N4 C15 1.358(6) . ? N4 C14 1.404(7) . ? N5 C8 1.353(6) . ? N5 C9 1.403(6) . ? N6 C3 1.339(6) . ? N6 C7 1.349(6) . ? N7 C27 1.279(6) . ? N7 C28 1.475(6) . ? N8 C30 1.283(6) . ? N8 C29 1.472(6) . ? N9 C37 1.150(14) . ? C3 C4 1.369(7) . ? C3 H3A 0.9300 . ? C4 C5 1.365(9) . ? C4 H4A 0.9300 . ? C5 C6 1.363(9) . ? C5 H5A 0.9300 . ? C6 C7 1.402(7) . ? C6 H6A 0.9300 . ? C7 C8 1.478(7) . ? C9 C10 1.399(7) . ? C9 C14 1.401(7) . ? C10 C11 1.377(8) . ? C10 H10A 0.9300 . ? C11 C12 1.337(9) . ? C11 H11A 0.9300 . ? C12 C13 1.421(8) . ? C13 C14 1.399(7) . ? C13 H13A 0.9300 . ? C15 C16 1.484(8) . ? C16 C17 1.381(7) . ? C17 C18 1.349(9) . ? C17 H17A 0.9300 . ? C18 C19 1.387(10) . ? C18 H18A 0.9300 . ? C19 C20 1.412(7) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C26 1.414(6) . ? C21 C22 1.417(6) . ? C22 C23 1.364(6) . ? C22 H22A 0.9300 . ? C23 C24 1.397(7) . ? C23 H23A 0.9300 . ? C24 C25 1.381(7) . ? C25 C26 1.402(6) . ? C25 H25A 0.9300 . ? C26 C27 1.441(6) . ? C27 H27A 0.9300 . ? C28 C29 1.517(7) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.425(6) . ? C30 H30A 0.9300 . ? C31 C36 1.411(6) . ? C31 C32 1.421(6) . ? C32 C33 1.365(7) . ? C32 H32A 0.9300 . ? C33 C34 1.403(7) . ? C34 C35 1.371(6) . ? C34 H34A 0.9300 . ? C35 C36 1.421(6) . ? C35 H35A 0.9300 . ? C37 C38 1.336(16) . ? O1W O1W 1.68(3) 2_655 ? 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 N4 83.07(18) . . ? N5 Fe1 C2 96.69(17) . . ? N4 Fe1 C2 89.97(17) . . ? N5 Fe1 C1 91.12(17) . . ? N4 Fe1 C1 98.18(17) . . ? C2 Fe1 C1 169.35(18) . . ? N5 Fe1 N6 82.69(17) . . ? N4 Fe1 N6 165.43(17) . . ? C2 Fe1 N6 88.68(16) . . ? C1 Fe1 N6 85.13(16) . . ? N5 Fe1 N3 165.75(18) . . ? N4 Fe1 N3 82.78(18) . . ? C2 Fe1 N3 84.90(16) . . ? C1 Fe1 N3 89.32(16) . . ? N6 Fe1 N3 111.53(17) . . ? O3 Mn1 O4 97.36(14) . . ? O3 Mn1 N8 171.64(14) . . ? O4 Mn1 N8 90.82(14) . . ? O3 Mn1 N7 90.28(14) . . ? O4 Mn1 N7 172.24(14) . . ? N8 Mn1 N7 81.50(16) . . ? O3 Mn1 N1 93.40(14) . . ? O4 Mn1 N1 90.62(14) . . ? N8 Mn1 N1 88.21(15) . . ? N7 Mn1 N1 90.26(14) . . ? O3 Mn1 N2 87.83(14) . 1_655 ? O4 Mn1 N2 93.87(14) . 1_655 ? N8 Mn1 N2 89.91(15) . 1_655 ? N7 Mn1 N2 85.05(14) . 1_655 ? N1 Mn1 N2 175.16(14) . 1_655 ? C21 O3 Mn1 126.8(3) . . ? C36 O4 Mn1 125.0(3) . . ? C1 N1 Mn1 154.3(3) . . ? C2 N2 Mn1 149.5(4) . 1_455 ? C20 N3 C16 118.2(4) . . ? C20 N3 Fe1 130.9(4) . . ? C16 N3 Fe1 110.8(3) . . ? C15 N4 C14 125.8(4) . . ? C15 N4 Fe1 118.4(4) . . ? C14 N4 Fe1 115.2(3) . . ? C8 N5 C9 126.4(4) . . ? C8 N5 Fe1 117.7(3) . . ? C9 N5 Fe1 115.4(3) . . ? C3 N6 C7 118.4(4) . . ? C3 N6 Fe1 130.3(3) . . ? C7 N6 Fe1 111.3(3) . . ? C27 N7 C28 122.1(4) . . ? C27 N7 Mn1 124.9(3) . . ? C28 N7 Mn1 112.5(3) . . ? C30 N8 C29 121.5(4) . . ? C30 N8 Mn1 124.9(3) . . ? C29 N8 Mn1 113.3(3) . . ? N1 C1 Fe1 172.5(4) . . ? N2 C2 Fe1 172.7(4) . . ? N6 C3 C4 123.5(5) . . ? N6 C3 H3A 118.2 . . ? C4 C3 H3A 118.2 . . ? C5 C4 C3 118.2(6) . . ? C5 C4 H4A 120.9 . . ? C3 C4 H4A 120.9 . . ? C6 C5 C4 120.0(5) . . ? C6 C5 H5A 120.0 . . ? C4 C5 H5A 120.0 . . ? C5 C6 C7 119.6(6) . . ? C5 C6 H6A 120.2 . . ? C7 C6 H6A 120.2 . . ? N6 C7 C6 120.3(5) . . ? N6 C7 C8 116.5(4) . . ? C6 C7 C8 123.2(5) . . ? O1 C8 N5 128.0(5) . . ? O1 C8 C7 121.1(5) . . ? N5 C8 C7 110.9(4) . . ? C10 C9 C14 121.2(5) . . ? C10 C9 N5 125.7(5) . . ? C14 C9 N5 113.1(4) . . ? C11 C10 C9 119.6(6) . . ? C11 C10 H10A 120.2 . . ? C9 C10 H10A 120.2 . . ? C12 C11 C10 119.2(6) . . ? C12 C11 H11A 120.4 . . ? C10 C11 H11A 120.4 . . ? C11 C12 C13 124.2(5) . . ? C11 C12 Cl1 119.7(5) . . ? C13 C12 Cl1 116.1(5) . . ? C14 C13 C12 116.6(5) . . ? C14 C13 H13A 121.7 . . ? C12 C13 H13A 121.7 . . ? C13 C14 C9 119.2(5) . . ? C13 C14 N4 127.7(5) . . ? C9 C14 N4 113.1(4) . . ? O2 C15 N4 127.7(6) . . ? O2 C15 C16 121.9(5) . . ? N4 C15 C16 110.5(4) . . ? N3 C16 C17 121.9(5) . . ? N3 C16 C15 116.5(4) . . ? C17 C16 C15 121.6(5) . . ? C18 C17 C16 119.8(6) . . ? C18 C17 H17A 120.1 . . ? C16 C17 H17A 120.1 . . ? C17 C18 C19 119.7(5) . . ? C17 C18 H18A 120.1 . . ? C19 C18 H18A 120.1 . . ? C18 C19 C20 118.5(6) . . ? C18 C19 H19A 120.7 . . ? C20 C19 H19A 120.7 . . ? N3 C20 C19 121.8(6) . . ? N3 C20 H20A 119.1 . . ? C19 C20 H20A 119.1 . . ? O3 C21 C26 123.8(4) . . ? O3 C21 C22 118.8(4) . . ? C26 C21 C22 117.4(4) . . ? C23 C22 C21 121.6(4) . . ? C23 C22 H22A 119.2 . . ? C21 C22 H22A 119.2 . . ? C22 C23 C24 120.0(4) . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C25 C24 C23 120.8(4) . . ? C25 C24 Cl4 119.7(4) . . ? C23 C24 Cl4 119.6(4) . . ? C24 C25 C26 119.3(4) . . ? C24 C25 H25A 120.3 . . ? C26 C25 H25A 120.3 . . ? C25 C26 C21 120.9(4) . . ? C25 C26 C27 116.8(4) . . ? C21 C26 C27 122.3(4) . . ? N7 C27 C26 125.1(4) . . ? N7 C27 H27A 117.5 . . ? C26 C27 H27A 117.5 . . ? N7 C28 C29 107.0(4) . . ? N7 C28 H28A 110.3 . . ? C29 C28 H28A 110.3 . . ? N7 C28 H28B 110.3 . . ? C29 C28 H28B 110.3 . . ? H28A C28 H28B 108.6 . . ? N8 C29 C28 106.5(4) . . ? N8 C29 H29A 110.4 . . ? C28 C29 H29A 110.4 . . ? N8 C29 H29B 110.4 . . ? C28 C29 H29B 110.4 . . ? H29A C29 H29B 108.6 . . ? N8 C30 C31 125.1(4) . . ? N8 C30 H30A 117.5 . . ? C31 C30 H30A 117.5 . . ? C36 C31 C32 119.6(4) . . ? C36 C31 C30 122.9(4) . . ? C32 C31 C30 117.5(4) . . ? C33 C32 C31 120.8(5) . . ? C33 C32 H32A 119.6 . . ? C31 C32 H32A 119.6 . . ? C32 C33 C34 120.1(4) . . ? C32 C33 Cl3 119.8(4) . . ? C34 C33 Cl3 120.0(4) . . ? C35 C34 C33 120.0(4) . . ? C35 C34 H34A 120.0 . . ? C33 C34 H34A 120.0 . . ? C34 C35 C36 121.7(5) . . ? C34 C35 H35A 119.2 . . ? C36 C35 H35A 119.2 . . ? O4 C36 C31 124.5(4) . . ? O4 C36 C35 117.8(4) . . ? C31 C36 C35 117.7(4) . . ? N9 C37 C38 175.4(13) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 3.355 _refine_diff_density_min -0.831 _refine_diff_density_rms 0.132 #===End data_2 _database_code_depnum_ccdc_archive 'CCDC 744628' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H29 Cl2 Fe Mn N8 O5.50' _chemical_formula_weight 855.37 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.013(2) _cell_length_b 15.613(3) _cell_length_c 20.586(4) _cell_angle_alpha 91.74(3) _cell_angle_beta 92.56(3) _cell_angle_gamma 90.89(3) _cell_volume 3534.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6544 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 25.00 _exptl_crystal_description platelet _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 0.978 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.768 _exptl_absorpt_correction_T_max 0.874 _exptl_absorpt_process_details 'ABSCOR; Higashi, 1995' _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 'Rigaku IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0.77 _diffrn_standards_decay_% ? _diffrn_reflns_number 11519 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0783 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11524 _reflns_number_gt 8743 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalstructure 3.6.0 (Rigaku/MSC, 2004)' _computing_cell_refinement 'crystalstructure 3.6.0 (Rigaku/MSC, 2004)' _computing_data_reduction 'Crystalstructure 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XP (Sheldrick, 1998)' _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^)+(0.2000P)^2^+12.6000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11524 _refine_ls_number_parameters 982 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1364 _refine_ls_R_factor_gt 0.1031 _refine_ls_wR_factor_ref 0.3260 _refine_ls_wR_factor_gt 0.2791 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 1.133 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.87055(10) 0.72507(6) 0.20016(5) 0.0231(3) Uani 1 1 d . . . Fe2 Fe 0.81234(9) 0.77223(6) 0.69543(5) 0.0221(3) Uani 1 1 d . . . Mn1 Mn 0.84137(12) 0.71675(8) 0.95074(6) 0.0316(3) Uani 1 1 d . . . Mn2 Mn 0.83380(11) 0.78540(7) 0.44742(5) 0.0268(3) Uani 1 1 d . . . Cl1 Cl 1.4628(2) 0.8560(2) 0.54785(15) 0.0633(8) Uani 1 1 d . . . Cl2 Cl 0.2085(2) 0.81069(19) 0.33578(14) 0.0558(7) Uani 1 1 d . . . Cl3 Cl 0.2127(3) 0.7371(2) 0.84029(15) 0.0690(8) Uani 1 1 d . . . Cl4 Cl 1.4508(3) 0.6057(2) 1.04817(16) 0.0688(8) Uani 1 1 d . . . N1 N 0.9059(7) 0.7515(5) 0.3484(4) 0.0398(17) Uani 1 1 d . . . N2 N 0.8103(8) 0.6815(5) 0.0555(3) 0.0411(18) Uani 1 1 d . . . N3 N 0.7602(7) 0.8020(5) 0.5495(4) 0.0393(17) Uani 1 1 d . . . N4 N 0.8654(7) 0.7590(4) 0.8439(3) 0.0367(17) Uani 1 1 d . . . N5 N 0.7006(6) 0.6943(4) 0.2178(3) 0.0313(15) Uani 1 1 d . . . N6 N 0.8075(6) 0.8370(4) 0.1928(3) 0.0282(14) Uani 1 1 d . . . N7 N 1.0168(6) 0.7811(4) 0.1823(3) 0.0278(14) Uani 1 1 d . . . N8 N 0.9722(6) 0.6196(4) 0.1985(3) 0.0280(14) Uani 1 1 d . . . N9 N 0.6575(6) 0.8221(4) 0.7190(3) 0.0304(15) Uani 1 1 d . . . N10 N 0.7205(6) 0.6681(4) 0.6902(3) 0.0246(13) Uani 1 1 d . . . N11 N 0.9397(5) 0.6999(4) 0.6735(3) 0.0258(13) Uani 1 1 d . . . N12 N 0.9386(6) 0.8665(4) 0.6869(3) 0.0263(13) Uani 1 1 d . . . N13 N 0.9362(7) 0.6945(4) 0.4856(3) 0.0332(15) Uani 1 1 d . . . N14 N 0.7218(6) 0.6829(4) 0.4289(3) 0.0333(15) Uani 1 1 d . . . N15 N 0.7380(8) 0.8179(4) 0.9663(3) 0.0395(18) Uani 1 1 d . . . N16 N 0.9684(7) 0.8015(4) 0.9874(3) 0.0342(16) Uani 1 1 d . . . C1 C 0.8977(6) 0.7389(5) 0.2937(4) 0.0244(15) Uani 1 1 d . . . C2 C 0.8297(7) 0.6944(5) 0.1097(4) 0.0294(17) Uani 1 1 d . . . C3 C 0.7722(7) 0.7935(5) 0.6040(3) 0.0246(15) Uani 1 1 d . . . C4 C 0.8491(7) 0.7651(5) 0.7890(4) 0.0268(16) Uani 1 1 d . . . C5 C 0.9419(8) 0.5362(5) 0.2036(4) 0.0332(18) Uani 1 1 d . . . H5 H 0.8634 0.5226 0.2153 0.040 Uiso 1 1 calc R . . C6 C 1.0207(9) 0.4690(5) 0.1926(4) 0.041(2) Uani 1 1 d . . . H6 H 0.9970 0.4124 0.1982 0.050 Uiso 1 1 calc R . . C7 C 1.1324(8) 0.4891(6) 0.1736(4) 0.038(2) Uani 1 1 d . . . H7 H 1.1861 0.4458 0.1636 0.046 Uiso 1 1 calc R . . C8 C 1.1683(9) 0.5754(6) 0.1687(5) 0.048(2) Uani 1 1 d . . . H8 H 1.2465 0.5897 0.1569 0.057 Uiso 1 1 calc R . . C9 C 1.0844(7) 0.6391(5) 0.1818(3) 0.0258(16) Uani 1 1 d . . . C10 C 1.1163(7) 0.7350(5) 0.1739(4) 0.0273(16) Uani 1 1 d . . . C11 C 1.0112(8) 0.8709(5) 0.1755(4) 0.0296(17) Uani 1 1 d . . . C12 C 1.1051(8) 0.9271(5) 0.1659(4) 0.0342(18) Uani 1 1 d . . . H12 H 1.1838 0.9065 0.1651 0.041 Uiso 1 1 calc R . . C13 C 1.0854(9) 1.0167(6) 0.1571(5) 0.045(2) Uani 1 1 d . . . H13 H 1.1498 1.0540 0.1499 0.054 Uiso 1 1 calc R . . C14 C 0.9664(9) 1.0464(6) 0.1597(4) 0.043(2) Uani 1 1 d . . . H14 H 0.9508 1.1042 0.1540 0.051 Uiso 1 1 calc R . . C15 C 0.8730(9) 0.9908(6) 0.1705(4) 0.040(2) Uani 1 1 d . . . H15 H 0.7942 1.0112 0.1720 0.048 Uiso 1 1 calc R . . C16 C 0.8937(7) 0.9044(5) 0.1794(3) 0.0264(16) Uani 1 1 d . . . C17 C 0.6885(8) 0.8470(5) 0.1965(4) 0.0354(19) Uani 1 1 d . . . C18 C 0.6275(8) 0.7644(6) 0.2105(4) 0.039(2) Uani 1 1 d . . . C19 C 0.5059(8) 0.7569(6) 0.2160(4) 0.038(2) Uani 1 1 d . . . H19 H 0.4572 0.8042 0.2092 0.046 Uiso 1 1 calc R . . C20 C 0.4520(8) 0.6780(7) 0.2321(4) 0.045(2) Uani 1 1 d . . . H20 H 0.3687 0.6736 0.2372 0.054 Uiso 1 1 calc R . . C21 C 0.5254(8) 0.6071(6) 0.2402(4) 0.040(2) Uani 1 1 d . . . H21 H 0.4930 0.5540 0.2501 0.048 Uiso 1 1 calc R . . C22 C 0.6477(8) 0.6190(6) 0.2328(5) 0.041(2) Uani 1 1 d . . . H22 H 0.6977 0.5721 0.2385 0.050 Uiso 1 1 calc R . . C23 C 0.6339(8) 0.9015(6) 0.7398(4) 0.039(2) Uani 1 1 d . . . H23 H 0.6973 0.9416 0.7449 0.046 Uiso 1 1 calc R . . C24 C 0.5173(9) 0.9260(6) 0.7541(4) 0.045(2) Uani 1 1 d . . . H24 H 0.5023 0.9816 0.7688 0.054 Uiso 1 1 calc R . . C25 C 0.4245(9) 0.8665(7) 0.7460(5) 0.047(2) Uani 1 1 d . . . H25 H 0.3450 0.8824 0.7532 0.057 Uiso 1 1 calc R . . C26 C 0.4489(9) 0.7806(7) 0.7269(5) 0.045(2) Uani 1 1 d . . . H26 H 0.3876 0.7389 0.7232 0.054 Uiso 1 1 calc R . . C27 C 0.5677(7) 0.7617(6) 0.7139(4) 0.0351(19) Uani 1 1 d . . . C28 C 0.6009(8) 0.6702(6) 0.6976(4) 0.0376(19) Uani 1 1 d . . . C29 C 0.7841(7) 0.5936(5) 0.6722(4) 0.0253(15) Uani 1 1 d . . . C30 C 0.7356(9) 0.5085(6) 0.6659(5) 0.048(2) Uani 1 1 d . . . H30 H 0.6541 0.4973 0.6727 0.058 Uiso 1 1 calc R . . C31 C 0.8131(9) 0.4422(6) 0.6491(6) 0.051(3) Uani 1 1 d . . . H31 H 0.7829 0.3863 0.6441 0.061 Uiso 1 1 calc R . . C32 C 0.9306(8) 0.4586(5) 0.6402(5) 0.042(2) Uani 1 1 d . . . H32 H 0.9811 0.4137 0.6292 0.050 Uiso 1 1 calc R . . C33 C 0.9802(8) 0.5440(5) 0.6471(4) 0.0317(17) Uani 1 1 d . . . H33 H 1.0620 0.5540 0.6401 0.038 Uiso 1 1 calc R . . C34 C 0.9065(7) 0.6120(5) 0.6643(4) 0.0276(16) Uani 1 1 d . . . C35 C 1.0484(7) 0.7340(5) 0.6705(4) 0.0330(18) Uani 1 1 d . . . C36 C 1.0493(7) 0.8339(5) 0.6726(4) 0.0251(15) Uani 1 1 d . . . C37 C 1.1441(8) 0.8854(6) 0.6600(4) 0.039(2) Uani 1 1 d . . . H37 H 1.2189 0.8611 0.6523 0.047 Uiso 1 1 calc R . . C38 C 1.1328(8) 0.9734(6) 0.6583(4) 0.038(2) Uani 1 1 d . . . H38 H 1.1991 1.0081 0.6495 0.046 Uiso 1 1 calc R . . C39 C 1.0217(9) 1.0090(6) 0.6699(4) 0.041(2) Uani 1 1 d . . . H39 H 1.0095 1.0677 0.6684 0.049 Uiso 1 1 calc R . . C40 C 0.9297(8) 0.9527(5) 0.6839(4) 0.0341(18) Uani 1 1 d . . . H40 H 0.8545 0.9760 0.6920 0.041 Uiso 1 1 calc R . . C41 C 1.0686(8) 0.8649(6) 0.4819(4) 0.0362(19) Uani 1 1 d . . . C42 C 1.1423(8) 0.9393(6) 0.4846(4) 0.0370(19) Uani 1 1 d . . . H42 H 1.1092 0.9915 0.4732 0.044 Uiso 1 1 calc R . . C43 C 1.2622(8) 0.9356(6) 0.5039(4) 0.040(2) Uani 1 1 d . . . H43 H 1.3109 0.9849 0.5050 0.048 Uiso 1 1 calc R . . C44 C 1.3105(8) 0.8592(7) 0.5216(4) 0.045(2) Uani 1 1 d . . . C45 C 1.2426(9) 0.7852(7) 0.5210(5) 0.052(3) Uani 1 1 d . . . H45 H 1.2787 0.7343 0.5331 0.062 Uiso 1 1 calc R . . C46 C 1.1189(7) 0.7858(6) 0.5023(4) 0.0338(18) Uani 1 1 d . . . C47 C 1.0503(8) 0.7062(6) 0.5032(4) 0.0361(19) Uani 1 1 d . . . H47 H 1.0919 0.6586 0.5180 0.043 Uiso 1 1 calc R . . C48 C 0.8722(9) 0.6113(6) 0.4931(5) 0.044(2) Uani 1 1 d . . . H48A H 0.8319 0.6114 0.5340 0.053 Uiso 1 1 calc R . . H48B H 0.9298 0.5649 0.4928 0.053 Uiso 1 1 calc R . . C49 C 0.7807(10) 0.5994(5) 0.4373(5) 0.047(2) Uani 1 1 d . . . H49A H 0.8204 0.5820 0.3981 0.056 Uiso 1 1 calc R . . H49B H 0.7209 0.5558 0.4468 0.056 Uiso 1 1 calc R . . C50 C 0.6115(8) 0.6848(5) 0.4095(4) 0.0360(19) Uani 1 1 d . . . H50 H 0.5689 0.6330 0.4040 0.043 Uiso 1 1 calc R . . C51 C 0.5472(8) 0.7629(5) 0.3953(4) 0.0316(17) Uani 1 1 d . . . C52 C 0.4250(9) 0.7541(6) 0.3770(4) 0.043(2) Uani 1 1 d . . . H52 H 0.3869 0.7004 0.3765 0.051 Uiso 1 1 calc R . . C53 C 0.3605(8) 0.8249(5) 0.3595(4) 0.0343(18) Uani 1 1 d . . . C54 C 0.4184(9) 0.9069(7) 0.3591(4) 0.047(2) Uani 1 1 d . . . H54 H 0.3737 0.9542 0.3466 0.057 Uiso 1 1 calc R . . C55 C 0.5370(8) 0.9168(6) 0.3765(5) 0.041(2) Uani 1 1 d . . . H55 H 0.5732 0.9710 0.3760 0.049 Uiso 1 1 calc R . . C56 C 0.6073(7) 0.8468(5) 0.3954(4) 0.0290(16) Uani 1 1 d . . . C57 C 0.5977(9) 0.6720(6) 0.9011(4) 0.040(2) Uani 1 1 d . . . C58 C 0.5140(10) 0.6090(6) 0.8699(5) 0.051(3) Uani 1 1 d . . . H58 H 0.5399 0.5535 0.8616 0.061 Uiso 1 1 calc R . . C59 C 0.4016(9) 0.6300(7) 0.8532(5) 0.054(3) Uani 1 1 d . . . H59 H 0.3487 0.5889 0.8336 0.065 Uiso 1 1 calc R . . C60 C 0.3611(9) 0.7134(8) 0.8647(5) 0.051(3) Uani 1 1 d . . . C61 C 0.4320(11) 0.7742(7) 0.8933(5) 0.055(3) Uani 1 1 d . . . H61 H 0.4007 0.8282 0.9016 0.066 Uiso 1 1 calc R . . C62 C 0.5577(9) 0.7576(6) 0.9118(4) 0.042(2) Uani 1 1 d . . . C63 C 0.6280(10) 0.8241(7) 0.9468(5) 0.052(3) Uani 1 1 d . . . H63 H 0.5896 0.8755 0.9558 0.062 Uiso 1 1 calc R . . C64 C 0.7922(9) 0.8846(6) 1.0105(4) 0.040(2) Uani 1 1 d . . . H64A H 0.7808 0.8700 1.0553 0.048 Uiso 1 1 calc R . . H64B H 0.7538 0.9391 1.0027 0.048 Uiso 1 1 calc R . . C65 C 0.9256(11) 0.8911(6) 0.9982(4) 0.051(3) Uani 1 1 d . . . H65A H 0.9386 0.9247 0.9602 0.062 Uiso 1 1 calc R . . H65B H 0.9696 0.9183 1.0353 0.062 Uiso 1 1 calc R . . C66 C 1.0763(9) 0.7819(6) 1.0067(4) 0.043(2) Uani 1 1 d . . . H66 H 1.1247 0.8251 1.0271 0.051 Uiso 1 1 calc R . . C67 C 1.1286(9) 0.6989(6) 0.9995(4) 0.038(2) Uani 1 1 d . . . C68 C 1.2477(9) 0.6910(7) 1.0238(4) 0.049(2) Uani 1 1 d . . . H68 H 1.2901 0.7378 1.0433 0.059 Uiso 1 1 calc R . . C69 C 1.3010(10) 0.6123(7) 1.0182(4) 0.049(2) Uani 1 1 d . . . C70 C 1.2430(11) 0.5411(7) 0.9904(5) 0.055(3) Uani 1 1 d . . . H70 H 1.2827 0.4891 0.9883 0.065 Uiso 1 1 calc R . . C71 C 1.1254(10) 0.5474(6) 0.9656(4) 0.046(2) Uani 1 1 d . . . H71 H 1.0850 0.4994 0.9468 0.055 Uiso 1 1 calc R . . C72 C 1.0660(8) 0.6273(6) 0.9687(4) 0.0370(19) Uani 1 1 d . . . C73 C 0.4193(15) 0.9202(13) 0.0725(10) 0.115(7) Uani 1 1 d . . . C74 C 0.389(5) 0.585(3) 0.518(3) 0.29(3) Uani 1 1 d . . . O1 O 0.6329(6) 0.9152(4) 0.1877(4) 0.0539(18) Uani 1 1 d . . . O2 O 1.2159(6) 0.7593(4) 0.1644(4) 0.0485(17) Uani 1 1 d . . . O3 O 0.5253(6) 0.6079(4) 0.6943(4) 0.059(2) Uani 1 1 d . . . O4 O 1.1451(5) 0.6986(4) 0.6598(3) 0.0427(15) Uani 1 1 d . . . O5 O 0.9537(6) 0.6298(4) 0.9436(3) 0.0413(15) Uani 1 1 d . . . O6 O 0.7072(6) 0.6478(4) 0.9178(3) 0.0380(14) Uani 1 1 d . . . O7 O 0.7221(5) 0.8608(3) 0.4111(3) 0.0297(12) Uani 1 1 d . . . O8 O 0.9542(5) 0.8715(4) 0.4648(3) 0.0366(13) Uani 1 1 d . . . O9 O 0.5228(14) 0.9758(9) 0.0769(6) 0.122(4) Uani 1 1 d . . . O10 O 0.483(3) 0.571(3) 0.5565(12) 0.295(19) Uani 1 1 d . . . O1W O 0.2823(7) 0.5570(4) 0.7004(4) 0.063(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 0.0206(6) 0.0268(6) 0.0219(5) -0.0026(4) 0.0018(4) 0.0052(4) Fe2 0.0165(6) 0.0260(6) 0.0240(5) -0.0008(4) 0.0020(4) 0.0036(4) Mn1 0.0391(8) 0.0293(6) 0.0257(6) -0.0061(5) -0.0039(5) 0.0039(5) Mn2 0.0226(6) 0.0327(7) 0.0247(6) -0.0016(4) -0.0021(5) 0.0023(5) Cl1 0.0270(13) 0.092(2) 0.0700(17) -0.0105(15) -0.0068(11) 0.0033(13) Cl2 0.0260(12) 0.0763(17) 0.0645(16) -0.0031(13) -0.0050(11) 0.0075(11) Cl3 0.0396(15) 0.099(2) 0.0687(18) 0.0091(16) -0.0052(13) 0.0058(15) Cl4 0.0451(16) 0.090(2) 0.0710(18) 0.0002(15) -0.0076(13) 0.0139(15) N1 0.040(4) 0.042(4) 0.038(4) -0.006(3) 0.003(3) 0.005(3) N2 0.051(5) 0.043(4) 0.028(4) -0.004(3) 0.002(3) -0.002(4) N3 0.033(4) 0.049(4) 0.036(4) 0.001(3) 0.000(3) 0.006(3) N4 0.049(5) 0.032(4) 0.028(4) 0.000(3) -0.004(3) 0.001(3) N5 0.033(4) 0.035(4) 0.026(3) -0.004(3) -0.002(3) 0.004(3) N6 0.024(4) 0.033(3) 0.027(3) -0.003(3) 0.003(3) 0.011(3) N7 0.026(3) 0.027(3) 0.031(3) -0.007(3) 0.002(3) 0.005(3) N8 0.033(4) 0.030(3) 0.020(3) -0.001(2) -0.005(3) 0.007(3) N9 0.031(4) 0.033(3) 0.028(3) 0.004(3) 0.001(3) 0.012(3) N10 0.019(3) 0.025(3) 0.030(3) 0.005(2) 0.007(3) -0.003(2) N11 0.012(3) 0.033(3) 0.033(3) -0.002(3) 0.002(2) 0.001(3) N12 0.022(3) 0.029(3) 0.028(3) 0.002(2) 0.003(3) -0.003(3) N13 0.032(4) 0.041(4) 0.027(3) -0.006(3) -0.001(3) 0.004(3) N14 0.027(4) 0.032(4) 0.041(4) -0.004(3) 0.000(3) 0.003(3) N15 0.054(5) 0.033(4) 0.031(4) -0.007(3) -0.003(3) 0.015(3) N16 0.046(5) 0.032(3) 0.023(3) -0.005(3) -0.006(3) -0.001(3) C1 0.012(3) 0.032(4) 0.029(4) -0.007(3) 0.000(3) 0.004(3) C2 0.021(4) 0.032(4) 0.035(5) -0.006(3) 0.007(3) 0.002(3) C3 0.021(4) 0.034(4) 0.019(4) 0.004(3) 0.004(3) 0.001(3) C4 0.022(4) 0.025(4) 0.032(4) -0.002(3) 0.000(3) -0.001(3) C5 0.027(4) 0.026(4) 0.048(5) 0.002(3) 0.008(4) 0.004(3) C6 0.055(6) 0.027(4) 0.042(5) 0.000(3) -0.007(4) 0.006(4) C7 0.036(5) 0.046(5) 0.031(4) -0.009(4) 0.004(4) 0.011(4) C8 0.038(5) 0.050(6) 0.053(6) -0.018(4) -0.003(4) 0.021(4) C9 0.023(4) 0.034(4) 0.021(3) 0.003(3) 0.008(3) 0.005(3) C10 0.013(4) 0.041(4) 0.029(4) -0.006(3) 0.007(3) 0.006(3) C11 0.034(4) 0.031(4) 0.024(4) -0.002(3) 0.002(3) 0.000(3) C12 0.033(5) 0.044(5) 0.027(4) 0.004(3) 0.008(3) -0.007(4) C13 0.045(6) 0.044(5) 0.046(5) 0.000(4) -0.003(4) 0.000(4) C14 0.050(6) 0.034(4) 0.043(5) -0.005(4) -0.011(4) 0.002(4) C15 0.037(5) 0.039(5) 0.042(5) -0.008(4) -0.007(4) 0.010(4) C16 0.032(4) 0.025(4) 0.023(4) 0.000(3) 0.006(3) 0.000(3) C17 0.026(4) 0.040(5) 0.040(5) -0.007(4) 0.002(3) 0.008(4) C18 0.028(5) 0.059(6) 0.029(4) -0.011(4) -0.006(3) 0.021(4) C19 0.026(4) 0.056(5) 0.034(4) 0.009(4) 0.009(3) 0.003(4) C20 0.018(4) 0.072(7) 0.044(5) -0.004(4) 0.005(4) -0.003(4) C21 0.028(5) 0.040(5) 0.053(5) 0.004(4) 0.013(4) -0.020(4) C22 0.023(4) 0.045(5) 0.057(6) -0.009(4) 0.009(4) 0.010(4) C23 0.029(5) 0.046(5) 0.042(5) 0.000(4) 0.008(4) 0.011(4) C24 0.044(6) 0.047(5) 0.045(5) -0.004(4) 0.014(4) 0.025(5) C25 0.031(5) 0.066(6) 0.047(5) 0.005(4) 0.014(4) 0.018(5) C26 0.032(5) 0.062(6) 0.044(5) 0.004(4) 0.012(4) 0.004(4) C27 0.014(4) 0.044(5) 0.047(5) -0.007(4) 0.003(3) 0.007(3) C28 0.027(5) 0.038(5) 0.048(5) -0.003(4) 0.005(4) 0.000(4) C29 0.020(4) 0.026(4) 0.029(4) 0.005(3) 0.002(3) -0.001(3) C30 0.033(5) 0.030(4) 0.080(7) -0.012(4) 0.001(5) -0.008(4) C31 0.045(6) 0.022(4) 0.085(7) -0.009(4) 0.002(5) -0.001(4) C32 0.029(5) 0.030(4) 0.066(6) -0.010(4) -0.005(4) 0.011(4) C33 0.023(4) 0.035(4) 0.038(4) -0.001(3) 0.005(3) 0.011(3) C34 0.025(4) 0.031(4) 0.026(4) -0.002(3) -0.007(3) 0.009(3) C35 0.020(4) 0.037(4) 0.041(4) -0.009(3) -0.004(3) 0.007(3) C36 0.018(4) 0.025(4) 0.032(4) -0.001(3) 0.002(3) -0.004(3) C37 0.025(4) 0.049(5) 0.044(5) -0.007(4) 0.005(4) 0.003(4) C38 0.037(5) 0.047(5) 0.031(4) 0.006(3) 0.015(4) -0.019(4) C39 0.046(6) 0.035(4) 0.043(5) 0.002(4) 0.008(4) -0.002(4) C40 0.033(5) 0.038(4) 0.032(4) 0.003(3) 0.004(3) 0.007(4) C41 0.034(5) 0.050(5) 0.024(4) -0.010(3) 0.002(3) 0.009(4) C42 0.021(4) 0.044(5) 0.045(5) -0.007(4) -0.004(4) -0.010(4) C43 0.026(4) 0.051(5) 0.041(5) -0.009(4) 0.002(4) -0.010(4) C44 0.021(4) 0.072(7) 0.040(5) -0.017(4) -0.003(4) -0.006(4) C45 0.038(6) 0.071(7) 0.045(5) -0.014(5) -0.010(4) 0.017(5) C46 0.022(4) 0.051(5) 0.029(4) -0.004(3) 0.005(3) 0.001(4) C47 0.031(5) 0.053(5) 0.024(4) -0.002(3) -0.007(3) 0.005(4) C48 0.045(6) 0.047(5) 0.041(5) 0.008(4) -0.002(4) 0.009(4) C49 0.051(6) 0.022(4) 0.066(6) 0.002(4) -0.007(5) 0.003(4) C50 0.032(5) 0.033(4) 0.043(5) 0.002(3) 0.008(4) -0.014(4) C51 0.025(4) 0.035(4) 0.035(4) 0.001(3) 0.001(3) -0.002(3) C52 0.035(5) 0.044(5) 0.047(5) -0.010(4) -0.004(4) 0.005(4) C53 0.029(4) 0.041(5) 0.033(4) 0.004(3) 0.002(3) -0.002(4) C54 0.039(5) 0.062(6) 0.041(5) 0.007(4) -0.002(4) 0.019(5) C55 0.033(5) 0.042(5) 0.049(5) 0.013(4) -0.001(4) 0.008(4) C56 0.028(4) 0.033(4) 0.027(4) 0.005(3) 0.006(3) 0.000(3) C57 0.048(6) 0.043(5) 0.028(4) 0.000(3) -0.006(4) -0.001(4) C58 0.054(6) 0.035(5) 0.063(6) -0.003(4) -0.008(5) -0.002(4) C59 0.037(6) 0.062(7) 0.061(6) -0.002(5) -0.006(5) -0.006(5) C60 0.037(5) 0.083(8) 0.033(5) 0.012(5) 0.000(4) 0.004(5) C61 0.059(7) 0.046(6) 0.061(6) 0.001(5) -0.001(5) 0.016(5) C62 0.040(5) 0.044(5) 0.040(5) -0.002(4) -0.008(4) 0.012(4) C63 0.056(7) 0.049(6) 0.049(6) -0.018(4) -0.008(5) 0.019(5) C64 0.050(6) 0.041(5) 0.029(4) -0.004(3) -0.006(4) 0.009(4) C65 0.084(8) 0.037(5) 0.032(5) -0.003(4) -0.016(5) 0.005(5) C66 0.047(6) 0.043(5) 0.037(5) -0.010(4) -0.006(4) -0.010(4) C67 0.040(5) 0.039(5) 0.033(4) -0.005(3) -0.007(4) -0.001(4) C68 0.043(6) 0.065(6) 0.038(5) -0.004(4) -0.008(4) 0.007(5) C69 0.052(6) 0.066(7) 0.030(4) 0.004(4) 0.006(4) 0.008(5) C70 0.067(7) 0.055(6) 0.042(5) 0.001(4) 0.003(5) 0.021(6) C71 0.054(6) 0.044(5) 0.039(5) -0.008(4) 0.004(4) 0.015(5) C72 0.033(5) 0.043(5) 0.036(4) -0.001(4) 0.004(4) 0.003(4) C73 0.065(10) 0.131(15) 0.149(17) 0.039(12) 0.008(10) -0.050(10) C74 0.33(7) 0.18(3) 0.39(8) 0.16(4) 0.10(5) 0.11(4) O1 0.038(4) 0.046(4) 0.080(5) 0.013(3) 0.022(3) 0.019(3) O2 0.022(3) 0.047(4) 0.076(5) -0.007(3) 0.008(3) 0.006(3) O3 0.018(3) 0.051(4) 0.107(6) -0.012(4) 0.022(4) -0.013(3) O4 0.022(3) 0.045(3) 0.063(4) 0.006(3) 0.011(3) 0.012(3) O5 0.048(4) 0.042(3) 0.033(3) -0.012(3) -0.004(3) 0.012(3) O6 0.034(3) 0.040(3) 0.039(3) -0.008(2) -0.004(3) 0.007(3) O7 0.015(3) 0.034(3) 0.039(3) 0.004(2) -0.003(2) -0.005(2) O8 0.027(3) 0.038(3) 0.043(3) -0.006(2) -0.006(3) 0.002(2) O9 0.146(13) 0.129(10) 0.092(8) 0.025(7) -0.001(8) 0.026(9) O10 0.29(4) 0.44(5) 0.141(19) -0.12(3) 0.00(2) -0.07(3) O1W 0.043(4) 0.044(4) 0.103(6) 0.024(4) -0.004(4) -0.010(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 N7 1.877(7) . ? Fe1 N6 1.898(6) . ? Fe1 C2 1.939(8) . ? Fe1 C1 1.940(7) . ? Fe1 N5 1.977(7) . ? Fe1 N8 2.005(6) . ? Fe2 N11 1.876(6) . ? Fe2 N10 1.898(6) . ? Fe2 C3 1.954(7) . ? Fe2 C4 1.958(8) . ? Fe2 N9 1.961(7) . ? Fe2 N12 2.026(7) . ? Mn1 O5 1.859(6) . ? Mn1 O6 1.903(6) . ? Mn1 N15 1.988(7) . ? Mn1 N16 2.017(7) . ? Mn1 N2 2.281(7) 1_556 ? Mn1 N4 2.339(7) . ? Mn2 O7 1.864(5) . ? Mn2 O8 1.889(6) . ? Mn2 N13 1.986(7) . ? Mn2 N14 2.022(7) . ? Mn2 N1 2.270(7) . ? Mn2 N3 2.294(7) . ? Cl1 C44 1.742(9) . ? Cl2 C53 1.731(9) . ? Cl3 C60 1.737(10) . ? Cl4 C69 1.741(11) . ? N1 C1 1.138(10) . ? N2 C2 1.139(10) . ? N2 Mn1 2.281(7) 1_554 ? N3 C3 1.136(10) . ? N4 C4 1.144(10) . ? N5 C22 1.353(12) . ? N5 C18 1.376(10) . ? N6 C17 1.328(11) . ? N6 C16 1.447(11) . ? N7 C10 1.336(9) . ? N7 C11 1.414(10) . ? N8 C9 1.331(11) . ? N8 C5 1.348(10) . ? N9 C23 1.333(11) . ? N9 C27 1.353(11) . ? N10 C28 1.333(11) . ? N10 C29 1.416(10) . ? N11 C35 1.307(11) . ? N11 C34 1.420(10) . ? N12 C40 1.354(10) . ? N12 C36 1.369(10) . ? N13 C47 1.301(11) . ? N13 C48 1.484(12) . ? N14 C50 1.263(11) . ? N14 C49 1.476(10) . ? N15 C63 1.266(13) . ? N15 C64 1.464(11) . ? N16 C66 1.281(12) . ? N16 C65 1.496(11) . ? C5 C6 1.391(11) . ? C5 H5 0.9300 . ? C6 C7 1.342(14) . ? C6 H6 0.9300 . ? C7 C8 1.405(14) . ? C7 H7 0.9300 . ? C8 C9 1.397(11) . ? C8 H8 0.9300 . ? C9 C10 1.547(11) . ? C10 O2 1.182(10) . ? C11 C12 1.371(12) . ? C11 C16 1.408(11) . ? C12 C13 1.436(13) . ? C12 H12 0.9300 . ? C13 C14 1.400(14) . ? C13 H13 0.9300 . ? C14 C15 1.366(14) . ? C14 H14 0.9300 . ? C15 C16 1.388(11) . ? C15 H15 0.9300 . ? C17 O1 1.250(10) . ? C17 C18 1.487(14) . ? C18 C19 1.353(13) . ? C19 C20 1.413(14) . ? C19 H19 0.9300 . ? C20 C21 1.391(13) . ? C20 H20 0.9300 . ? C21 C22 1.373(12) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.387(12) . ? C23 H23 0.9300 . ? C24 C25 1.372(15) . ? C24 H24 0.9300 . ? C25 C26 1.418(14) . ? C25 H25 0.9300 . ? C26 C27 1.381(12) . ? C26 H26 0.9300 . ? C27 C28 1.512(12) . ? C28 O3 1.269(11) . ? C29 C34 1.392(11) . ? C29 C30 1.425(11) . ? C30 C31 1.397(13) . ? C30 H30 0.9300 . ? C31 C32 1.336(14) . ? C31 H31 0.9300 . ? C32 C33 1.433(12) . ? C32 H32 0.9300 . ? C33 C34 1.393(10) . ? C33 H33 0.9300 . ? C35 O4 1.233(10) . ? C35 C36 1.559(11) . ? C36 C37 1.347(12) . ? C37 C38 1.384(13) . ? C37 H37 0.9300 . ? C38 C39 1.379(13) . ? C38 H38 0.9300 . ? C39 C40 1.376(13) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 O8 1.299(10) . ? C41 C42 1.405(13) . ? C41 C46 1.430(12) . ? C42 C43 1.364(12) . ? C42 H42 0.9300 . ? C43 C44 1.367(14) . ? C43 H43 0.9300 . ? C44 C45 1.365(16) . ? C45 C46 1.399(13) . ? C45 H45 0.9300 . ? C46 C47 1.445(13) . ? C47 H47 0.9300 . ? C48 C49 1.499(13) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.451(12) . ? C50 H50 0.9300 . ? C51 C52 1.385(12) . ? C51 C56 1.458(11) . ? C52 C53 1.372(12) . ? C52 H52 0.9300 . ? C53 C54 1.422(14) . ? C54 C55 1.345(13) . ? C54 H54 0.9300 . ? C55 C56 1.404(11) . ? C55 H55 0.9300 . ? C56 O7 1.305(10) . ? C57 O6 1.304(11) . ? C57 C62 1.427(12) . ? C57 C58 1.453(13) . ? C58 C59 1.318(14) . ? C58 H58 0.9300 . ? C59 C60 1.401(15) . ? C59 H59 0.9300 . ? C60 C61 1.326(16) . ? C61 C62 1.449(14) . ? C61 H61 0.9300 . ? C62 C63 1.441(14) . ? C63 H63 0.9300 . ? C64 C65 1.504(15) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 C67 1.433(13) . ? C66 H66 0.9300 . ? C67 C68 1.392(13) . ? C67 C72 1.422(12) . ? C68 C69 1.375(14) . ? C68 H68 0.9300 . ? C69 C70 1.370(16) . ? C70 C71 1.377(15) . ? C70 H70 0.9300 . ? C71 C72 1.419(12) . ? C71 H71 0.9300 . ? C72 O5 1.320(11) . ? C73 O9 1.42(2) . ? C74 O10 1.30(5) . ? 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 N6 82.6(3) . . ? N7 Fe1 C2 94.2(3) . . ? N6 Fe1 C2 93.1(3) . . ? N7 Fe1 C1 93.6(3) . . ? N6 Fe1 C1 92.6(3) . . ? C2 Fe1 C1 170.8(3) . . ? N7 Fe1 N5 166.1(3) . . ? N6 Fe1 N5 83.5(3) . . ? C2 Fe1 N5 86.8(3) . . ? C1 Fe1 N5 86.7(3) . . ? N7 Fe1 N8 83.9(3) . . ? N6 Fe1 N8 166.2(3) . . ? C2 Fe1 N8 85.0(3) . . ? C1 Fe1 N8 91.2(3) . . ? N5 Fe1 N8 110.0(3) . . ? N11 Fe2 N10 82.9(3) . . ? N11 Fe2 C3 91.8(3) . . ? N10 Fe2 C3 91.1(3) . . ? N11 Fe2 C4 93.3(3) . . ? N10 Fe2 C4 93.8(3) . . ? C3 Fe2 C4 173.3(3) . . ? N11 Fe2 N9 166.4(3) . . ? N10 Fe2 N9 83.6(3) . . ? C3 Fe2 N9 89.7(3) . . ? C4 Fe2 N9 86.3(3) . . ? N11 Fe2 N12 83.8(3) . . ? N10 Fe2 N12 165.7(3) . . ? C3 Fe2 N12 84.1(3) . . ? C4 Fe2 N12 92.2(3) . . ? N9 Fe2 N12 109.9(3) . . ? O5 Mn1 O6 94.6(3) . . ? O5 Mn1 N15 172.2(3) . . ? O6 Mn1 N15 92.9(3) . . ? O5 Mn1 N16 92.6(3) . . ? O6 Mn1 N16 172.8(3) . . ? N15 Mn1 N16 80.0(3) . . ? O5 Mn1 N2 90.4(3) . 1_556 ? O6 Mn1 N2 92.6(3) . 1_556 ? N15 Mn1 N2 87.1(3) . 1_556 ? N16 Mn1 N2 87.0(3) . 1_556 ? O5 Mn1 N4 92.8(3) . . ? O6 Mn1 N4 87.2(3) . . ? N15 Mn1 N4 89.7(3) . . ? N16 Mn1 N4 92.8(3) . . ? N2 Mn1 N4 176.8(3) 1_556 . ? O7 Mn2 O8 93.8(2) . . ? O7 Mn2 N13 173.0(3) . . ? O8 Mn2 N13 93.2(3) . . ? O7 Mn2 N14 92.7(3) . . ? O8 Mn2 N14 173.0(3) . . ? N13 Mn2 N14 80.4(3) . . ? O7 Mn2 N1 91.7(3) . . ? O8 Mn2 N1 92.6(3) . . ? N13 Mn2 N1 89.1(3) . . ? N14 Mn2 N1 84.4(3) . . ? O7 Mn2 N3 93.1(3) . . ? O8 Mn2 N3 92.2(3) . . ? N13 Mn2 N3 85.6(3) . . ? N14 Mn2 N3 90.3(3) . . ? N1 Mn2 N3 173.0(3) . . ? C1 N1 Mn2 154.6(7) . . ? C2 N2 Mn1 149.1(7) . 1_554 ? C3 N3 Mn2 149.4(6) . . ? C4 N4 Mn1 160.8(7) . . ? C22 N5 C18 118.1(8) . . ? C22 N5 Fe1 131.7(6) . . ? C18 N5 Fe1 110.2(6) . . ? C17 N6 C16 125.0(7) . . ? C17 N6 Fe1 118.4(6) . . ? C16 N6 Fe1 116.5(5) . . ? C10 N7 C11 124.4(7) . . ? C10 N7 Fe1 119.3(5) . . ? C11 N7 Fe1 116.2(5) . . ? C9 N8 C5 118.0(7) . . ? C9 N8 Fe1 110.3(5) . . ? C5 N8 Fe1 131.2(6) . . ? C23 N9 C27 120.2(7) . . ? C23 N9 Fe2 129.5(6) . . ? C27 N9 Fe2 110.3(5) . . ? C28 N10 C29 124.2(7) . . ? C28 N10 Fe2 119.3(5) . . ? C29 N10 Fe2 116.2(5) . . ? C35 N11 C34 127.0(6) . . ? C35 N11 Fe2 117.9(5) . . ? C34 N11 Fe2 115.0(5) . . ? C40 N12 C36 115.5(7) . . ? C40 N12 Fe2 132.2(6) . . ? C36 N12 Fe2 111.6(5) . . ? C47 N13 C48 122.0(7) . . ? C47 N13 Mn2 123.3(6) . . ? C48 N13 Mn2 114.7(5) . . ? C50 N14 C49 119.5(8) . . ? C50 N14 Mn2 126.3(6) . . ? C49 N14 Mn2 114.2(6) . . ? C63 N15 C64 119.0(7) . . ? C63 N15 Mn1 125.2(6) . . ? C64 N15 Mn1 115.3(6) . . ? C66 N16 C65 119.6(8) . . ? C66 N16 Mn1 124.6(6) . . ? C65 N16 Mn1 115.5(6) . . ? N1 C1 Fe1 174.3(7) . . ? N2 C2 Fe1 175.1(8) . . ? N3 C3 Fe2 172.8(7) . . ? N4 C4 Fe2 176.8(8) . . ? N8 C5 C6 124.1(8) . . ? N8 C5 H5 117.9 . . ? C6 C5 H5 117.9 . . ? C7 C6 C5 117.4(8) . . ? C7 C6 H6 121.3 . . ? C5 C6 H6 121.3 . . ? C6 C7 C8 120.3(8) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C9 C8 C7 118.7(9) . . ? C9 C8 H8 120.6 . . ? C7 C8 H8 120.6 . . ? N8 C9 C8 121.4(8) . . ? N8 C9 C10 117.3(6) . . ? C8 C9 C10 121.2(8) . . ? O2 C10 N7 128.5(8) . . ? O2 C10 C9 122.4(7) . . ? N7 C10 C9 109.0(7) . . ? C12 C11 C16 117.8(7) . . ? C12 C11 N7 127.9(8) . . ? C16 C11 N7 114.4(7) . . ? C11 C12 C13 121.9(9) . . ? C11 C12 H12 119.1 . . ? C13 C12 H12 119.1 . . ? C14 C13 C12 118.0(9) . . ? C14 C13 H13 121.0 . . ? C12 C13 H13 121.0 . . ? C15 C14 C13 120.1(9) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 121.1(8) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C15 C16 C11 121.0(8) . . ? C15 C16 N6 128.9(8) . . ? C11 C16 N6 110.1(6) . . ? O1 C17 N6 125.7(9) . . ? O1 C17 C18 123.7(8) . . ? N6 C17 C18 110.6(7) . . ? C19 C18 N5 120.5(9) . . ? C19 C18 C17 122.5(8) . . ? N5 C18 C17 117.0(8) . . ? C18 C19 C20 120.7(9) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C21 C20 C19 119.0(8) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? C22 C21 C20 117.0(8) . . ? C22 C21 H21 121.5 . . ? C20 C21 H21 121.5 . . ? N5 C22 C21 124.5(8) . . ? N5 C22 H22 117.7 . . ? C21 C22 H22 117.7 . . ? N9 C23 C24 121.7(9) . . ? N9 C23 H23 119.1 . . ? C24 C23 H23 119.1 . . ? C25 C24 C23 118.5(8) . . ? C25 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? C24 C25 C26 120.4(8) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C27 C26 C25 117.1(9) . . ? C27 C26 H26 121.4 . . ? C25 C26 H26 121.4 . . ? N9 C27 C26 121.9(8) . . ? N9 C27 C28 118.4(7) . . ? C26 C27 C28 119.6(8) . . ? O3 C28 N10 128.0(8) . . ? O3 C28 C27 123.9(8) . . ? N10 C28 C27 108.1(7) . . ? C34 C29 N10 111.3(6) . . ? C34 C29 C30 122.0(7) . . ? N10 C29 C30 126.5(7) . . ? C31 C30 C29 118.6(9) . . ? C31 C30 H30 120.7 . . ? C29 C30 H30 120.7 . . ? C32 C31 C30 120.3(8) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C31 C32 C33 121.3(8) . . ? C31 C32 H32 119.3 . . ? C33 C32 H32 119.3 . . ? C34 C33 C32 120.3(8) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C29 C34 C33 117.3(7) . . ? C29 C34 N11 114.6(6) . . ? C33 C34 N11 128.1(8) . . ? O4 C35 N11 129.0(8) . . ? O4 C35 C36 117.2(8) . . ? N11 C35 C36 113.4(6) . . ? C37 C36 N12 121.5(7) . . ? C37 C36 C35 126.0(7) . . ? N12 C36 C35 112.4(6) . . ? C36 C37 C38 121.6(8) . . ? C36 C37 H37 119.2 . . ? C38 C37 H37 119.2 . . ? C39 C38 C37 118.9(8) . . ? C39 C38 H38 120.5 . . ? C37 C38 H38 120.5 . . ? C40 C39 C38 116.3(8) . . ? C40 C39 H39 121.9 . . ? C38 C39 H39 121.9 . . ? N12 C40 C39 126.1(8) . . ? N12 C40 H40 117.0 . . ? C39 C40 H40 117.0 . . ? O8 C41 C42 118.6(8) . . ? O8 C41 C46 121.9(9) . . ? C42 C41 C46 119.4(8) . . ? C43 C42 C41 120.5(9) . . ? C43 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? C42 C43 C44 119.7(9) . . ? C42 C43 H43 120.1 . . ? C44 C43 H43 120.1 . . ? C45 C44 C43 122.3(9) . . ? C45 C44 Cl1 118.5(8) . . ? C43 C44 Cl1 119.2(8) . . ? C44 C45 C46 120.2(10) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C45 C46 C41 117.8(9) . . ? C45 C46 C47 118.3(9) . . ? C41 C46 C47 123.9(8) . . ? N13 C47 C46 126.5(8) . . ? N13 C47 H47 116.7 . . ? C46 C47 H47 116.7 . . ? N13 C48 C49 107.7(7) . . ? N13 C48 H48A 110.2 . . ? C49 C48 H48A 110.2 . . ? N13 C48 H48B 110.2 . . ? C49 C48 H48B 110.2 . . ? H48A C48 H48B 108.5 . . ? N14 C49 C48 106.7(7) . . ? N14 C49 H49A 110.4 . . ? C48 C49 H49A 110.4 . . ? N14 C49 H49B 110.4 . . ? C48 C49 H49B 110.4 . . ? H49A C49 H49B 108.6 . . ? N14 C50 C51 124.0(8) . . ? N14 C50 H50 118.0 . . ? C51 C50 H50 118.0 . . ? C52 C51 C50 116.7(8) . . ? C52 C51 C56 120.2(8) . . ? C50 C51 C56 123.0(7) . . ? C53 C52 C51 119.6(9) . . ? C53 C52 H52 120.2 . . ? C51 C52 H52 120.2 . . ? C52 C53 C54 120.6(8) . . ? C52 C53 Cl2 118.1(7) . . ? C54 C53 Cl2 121.3(7) . . ? C55 C54 C53 120.8(9) . . ? C55 C54 H54 119.6 . . ? C53 C54 H54 119.6 . . ? C54 C55 C56 121.1(9) . . ? C54 C55 H55 119.4 . . ? C56 C55 H55 119.4 . . ? O7 C56 C55 118.0(8) . . ? O7 C56 C51 124.3(7) . . ? C55 C56 C51 117.7(8) . . ? O6 C57 C62 122.7(8) . . ? O6 C57 C58 118.2(8) . . ? C62 C57 C58 119.1(9) . . ? C59 C58 C57 120.5(9) . . ? C59 C58 H58 119.8 . . ? C57 C58 H58 119.8 . . ? C58 C59 C60 120.7(10) . . ? C58 C59 H59 119.7 . . ? C60 C59 H59 119.7 . . ? C61 C60 C59 122.2(10) . . ? C61 C60 Cl3 119.5(9) . . ? C59 C60 Cl3 118.3(8) . . ? C60 C61 C62 120.9(9) . . ? C60 C61 H61 119.5 . . ? C62 C61 H61 119.5 . . ? C57 C62 C63 124.6(8) . . ? C57 C62 C61 116.5(9) . . ? C63 C62 C61 118.4(8) . . ? N15 C63 C62 124.9(8) . . ? N15 C63 H63 117.5 . . ? C62 C63 H63 117.5 . . ? N15 C64 C65 108.0(7) . . ? N15 C64 H64A 110.1 . . ? C65 C64 H64A 110.1 . . ? N15 C64 H64B 110.1 . . ? C65 C64 H64B 110.1 . . ? H64A C64 H64B 108.4 . . ? N16 C65 C64 106.8(8) . . ? N16 C65 H65A 110.4 . . ? C64 C65 H65A 110.4 . . ? N16 C65 H65B 110.4 . . ? C64 C65 H65B 110.4 . . ? H65A C65 H65B 108.6 . . ? N16 C66 C67 125.3(8) . . ? N16 C66 H66 117.4 . . ? C67 C66 H66 117.4 . . ? C68 C67 C72 120.2(8) . . ? C68 C67 C66 116.3(8) . . ? C72 C67 C66 123.5(8) . . ? C69 C68 C67 118.1(10) . . ? C69 C68 H68 120.9 . . ? C67 C68 H68 120.9 . . ? C70 C69 C68 123.6(10) . . ? C70 C69 Cl4 119.9(8) . . ? C68 C69 Cl4 116.6(8) . . ? C69 C70 C71 119.4(9) . . ? C69 C70 H70 120.3 . . ? C71 C70 H70 120.3 . . ? C70 C71 C72 119.8(9) . . ? C70 C71 H71 120.1 . . ? C72 C71 H71 120.1 . . ? O5 C72 C71 117.2(8) . . ? O5 C72 C67 124.0(8) . . ? C71 C72 C67 118.8(8) . . ? C72 O5 Mn1 128.7(5) . . ? C57 O6 Mn1 128.1(6) . . ? C56 O7 Mn2 128.2(5) . . ? C41 O8 Mn2 130.1(6) . . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 1.264 _refine_diff_density_min -0.896 _refine_diff_density_rms 0.199 #===End data_3 _database_code_depnum_ccdc_archive 'CCDC 744629' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H29 Br2 Fe Mn N8 O5.50' _chemical_formula_weight 944.29 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' 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1567(9) _cell_length_b 15.4314(13) _cell_length_c 20.8618(17) _cell_angle_alpha 91.765(2) _cell_angle_beta 92.646(2) _cell_angle_gamma 91.871(2) _cell_volume 3584.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7124 _cell_measurement_theta_min 2.03 _cell_measurement_theta_max 30.00 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.750 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 3.046 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.598 _exptl_absorpt_correction_T_max 0.874 _exptl_absorpt_process_details 'ABSCOR; Higashi, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0.77 _diffrn_standards_decay_% ? _diffrn_reflns_number 29225 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0624 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 30.00 _reflns_number_total 20357 _reflns_number_gt 13210 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalstructure 3.6.0 (Rigaku/MSC, 2004)' _computing_cell_refinement 'crystalstructure 3.6.0 (Rigaku/MSC, 2004)' _computing_data_reduction 'Crystalstructure 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XP (Sheldrick, 1998)' _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^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20357 _refine_ls_number_parameters 982 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0869 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1214 _refine_ls_wR_factor_gt 0.1127 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 0.86903(4) 0.72365(3) 0.199703(18) 0.02615(9) Uani 1 1 d . . . Fe2 Fe 0.81651(3) 0.77408(3) 0.696035(18) 0.02536(9) Uani 1 1 d . . . Mn1 Mn 0.84241(4) 0.71674(3) 0.95095(2) 0.03333(11) Uani 1 1 d . . . Mn2 Mn 0.83633(4) 0.78502(3) 0.44740(2) 0.02925(10) Uani 1 1 d . . . Br1 Br 1.47619(3) 0.85675(3) 0.550290(19) 0.05770(11) Uani 1 1 d . . . Br2 Br 0.20009(3) 0.80705(3) 0.333940(18) 0.05177(10) Uani 1 1 d . . . Br3 Br 0.20487(4) 0.73865(3) 0.83741(2) 0.06299(12) Uani 1 1 d . . . Br4 Br 1.46517(4) 0.61113(3) 1.05048(2) 0.06481(13) Uani 1 1 d . . . N1 N 0.9047(2) 0.74931(19) 0.34777(12) 0.0407(6) Uani 1 1 d . . . N2 N 0.8094(3) 0.68076(18) 0.05527(12) 0.0410(6) Uani 1 1 d . . . N3 N 0.7659(2) 0.80270(19) 0.55042(12) 0.0415(7) Uani 1 1 d . . . N4 N 0.8685(3) 0.76000(17) 0.84420(12) 0.0392(6) Uani 1 1 d . . . N5 N 0.6984(2) 0.69404(17) 0.21719(11) 0.0325(5) Uani 1 1 d . . . N6 N 0.8068(2) 0.83602(16) 0.19153(11) 0.0295(5) Uani 1 1 d . . . N7 N 1.0151(2) 0.78022(16) 0.18172(11) 0.0294(5) Uani 1 1 d . . . N8 N 0.9708(2) 0.61894(16) 0.19755(10) 0.0301(5) Uani 1 1 d . . . N9 N 0.6623(2) 0.82424(16) 0.71982(11) 0.0305(5) Uani 1 1 d . . . N10 N 0.7215(2) 0.67065(15) 0.69084(11) 0.0293(5) Uani 1 1 d . . . N11 N 0.9417(2) 0.70023(15) 0.67469(11) 0.0274(5) Uani 1 1 d . . . N12 N 0.9441(2) 0.86610(16) 0.68754(10) 0.0285(5) Uani 1 1 d . . . N13 N 0.9393(2) 0.69513(17) 0.48538(11) 0.0347(6) Uani 1 1 d . . . N14 N 0.7242(2) 0.68306(17) 0.43110(12) 0.0368(6) Uani 1 1 d . . . N15 N 0.7377(3) 0.81653(17) 0.96691(12) 0.0391(6) Uani 1 1 d . . . N16 N 0.9676(2) 0.80147(17) 0.98858(11) 0.0359(6) Uani 1 1 d . . . C1 C 0.8961(3) 0.73760(19) 0.29302(14) 0.0301(6) Uani 1 1 d . . . C2 C 0.8286(3) 0.69390(19) 0.10887(14) 0.0308(6) Uani 1 1 d . . . C3 C 0.7778(2) 0.79559(19) 0.60464(14) 0.0286(6) Uani 1 1 d . . . C4 C 0.8538(3) 0.76650(18) 0.78981(14) 0.0290(6) Uani 1 1 d . . . C5 C 0.9410(3) 0.5354(2) 0.20369(15) 0.0386(7) Uani 1 1 d . . . H5 H 0.8645 0.5206 0.2166 0.046 Uiso 1 1 calc R . . C6 C 1.0192(3) 0.4696(2) 0.19159(16) 0.0445(8) Uani 1 1 d . . . H6 H 0.9951 0.4120 0.1962 0.053 Uiso 1 1 calc R . . C7 C 1.1317(3) 0.4899(2) 0.17290(16) 0.0450(8) Uani 1 1 d . . . H7 H 1.1850 0.4466 0.1638 0.054 Uiso 1 1 calc R . . C8 C 1.1645(3) 0.5755(2) 0.16786(15) 0.0398(7) Uani 1 1 d . . . H8 H 1.2414 0.5910 0.1560 0.048 Uiso 1 1 calc R . . C9 C 1.0837(3) 0.6385(2) 0.18035(13) 0.0325(6) Uani 1 1 d . . . C10 C 1.1130(3) 0.7331(2) 0.17400(14) 0.0323(6) Uani 1 1 d . . . C11 C 1.0092(3) 0.8695(2) 0.17440(13) 0.0316(6) Uani 1 1 d . . . C12 C 1.1052(3) 0.9268(2) 0.16393(14) 0.0388(7) Uani 1 1 d . . . H12 H 1.1827 0.9069 0.1620 0.047 Uiso 1 1 calc R . . C13 C 1.0831(3) 1.0140(2) 0.15638(15) 0.0444(8) Uani 1 1 d . . . H13 H 1.1468 1.0526 0.1500 0.053 Uiso 1 1 calc R . . C14 C 0.9685(3) 1.0442(2) 0.15826(16) 0.0461(8) Uani 1 1 d . . . H14 H 0.9557 1.1026 0.1517 0.055 Uiso 1 1 calc R . . C15 C 0.8725(3) 0.9891(2) 0.16972(15) 0.0408(7) Uani 1 1 d . . . H15 H 0.7956 1.0102 0.1716 0.049 Uiso 1 1 calc R . . C16 C 0.8919(3) 0.90118(19) 0.17852(13) 0.0308(6) Uani 1 1 d . . . C17 C 0.6885(3) 0.8460(2) 0.19530(15) 0.0384(7) Uani 1 1 d . . . C18 C 0.6267(3) 0.7629(2) 0.21039(14) 0.0348(7) Uani 1 1 d . . . C19 C 0.5044(3) 0.7551(3) 0.21712(16) 0.0466(8) Uani 1 1 d . . . H19 H 0.4566 0.8027 0.2112 0.056 Uiso 1 1 calc R . . C20 C 0.4538(3) 0.6767(3) 0.23262(17) 0.0501(9) Uani 1 1 d . . . H20 H 0.3714 0.6704 0.2370 0.060 Uiso 1 1 calc R . . C21 C 0.5263(3) 0.6080(3) 0.24154(17) 0.0496(9) Uani 1 1 d . . . H21 H 0.4939 0.5548 0.2531 0.060 Uiso 1 1 calc R . . C22 C 0.6481(3) 0.6183(2) 0.23319(16) 0.0426(8) Uani 1 1 d . . . H22 H 0.6967 0.5711 0.2389 0.051 Uiso 1 1 calc R . . C23 C 0.6396(3) 0.9045(2) 0.74013(15) 0.0389(7) Uani 1 1 d . . . H23 H 0.7031 0.9452 0.7450 0.047 Uiso 1 1 calc R . . C24 C 0.5257(3) 0.9303(2) 0.75439(16) 0.0450(8) Uani 1 1 d . . . H24 H 0.5129 0.9869 0.7684 0.054 Uiso 1 1 calc R . . C25 C 0.4323(3) 0.8701(3) 0.74728(17) 0.0499(9) Uani 1 1 d . . . H25 H 0.3546 0.8857 0.7559 0.060 Uiso 1 1 calc R . . C26 C 0.4545(3) 0.7867(2) 0.72737(16) 0.0432(8) Uani 1 1 d . . . H26 H 0.3920 0.7453 0.7223 0.052 Uiso 1 1 calc R . . C27 C 0.5699(3) 0.7651(2) 0.71504(14) 0.0348(7) Uani 1 1 d . . . C28 C 0.6028(3) 0.6747(2) 0.69805(15) 0.0381(7) Uani 1 1 d . . . C29 C 0.7829(3) 0.5961(2) 0.67361(14) 0.0332(6) Uani 1 1 d . . . C30 C 0.7357(3) 0.5123(2) 0.66578(18) 0.0474(8) Uani 1 1 d . . . H30 H 0.6547 0.5006 0.6714 0.057 Uiso 1 1 calc R . . C31 C 0.8101(4) 0.4462(2) 0.6495(2) 0.0588(10) Uani 1 1 d . . . H31 H 0.7782 0.3899 0.6442 0.071 Uiso 1 1 calc R . . C32 C 0.9301(3) 0.4617(2) 0.64094(17) 0.0470(8) Uani 1 1 d . . . H32 H 0.9784 0.4161 0.6301 0.056 Uiso 1 1 calc R . . C33 C 0.9792(3) 0.5447(2) 0.64844(15) 0.0368(7) Uani 1 1 d . . . H33 H 1.0603 0.5552 0.6422 0.044 Uiso 1 1 calc R . . C34 C 0.9065(3) 0.61327(19) 0.66556(13) 0.0298(6) Uani 1 1 d . . . C35 C 1.0527(3) 0.7353(2) 0.66970(13) 0.0302(6) Uani 1 1 d . . . C36 C 1.0511(3) 0.8319(2) 0.67505(13) 0.0303(6) Uani 1 1 d . . . C37 C 1.1495(3) 0.8834(2) 0.66184(15) 0.0406(8) Uani 1 1 d . . . H37 H 1.2226 0.8585 0.6545 0.049 Uiso 1 1 calc R . . C38 C 1.1387(3) 0.9725(2) 0.65963(17) 0.0461(8) Uani 1 1 d . . . H38 H 1.2044 1.0082 0.6510 0.055 Uiso 1 1 calc R . . C39 C 1.0289(3) 1.0075(2) 0.67046(15) 0.0424(8) Uani 1 1 d . . . H39 H 1.0189 1.0669 0.6684 0.051 Uiso 1 1 calc R . . C40 C 0.9347(3) 0.9528(2) 0.68437(14) 0.0363(7) Uani 1 1 d . . . H40 H 0.8610 0.9766 0.6920 0.044 Uiso 1 1 calc R . . C41 C 1.0694(3) 0.8649(2) 0.48231(14) 0.0353(7) Uani 1 1 d . . . C42 C 1.1443(3) 0.9398(2) 0.48365(15) 0.0414(8) Uani 1 1 d . . . H42 H 1.1130 0.9920 0.4707 0.050 Uiso 1 1 calc R . . C43 C 1.2627(3) 0.9373(3) 0.50369(15) 0.0446(8) Uani 1 1 d . . . H43 H 1.3109 0.9877 0.5045 0.053 Uiso 1 1 calc R . . C44 C 1.3112(3) 0.8605(3) 0.52265(16) 0.0447(8) Uani 1 1 d . . . C45 C 1.2415(3) 0.7859(3) 0.52256(16) 0.0445(8) Uani 1 1 d . . . H45 H 1.2748 0.7344 0.5356 0.053 Uiso 1 1 calc R . . C46 C 1.1190(3) 0.7872(2) 0.50266(14) 0.0376(7) Uani 1 1 d . . . C47 C 1.0511(3) 0.7069(2) 0.50429(15) 0.0407(8) Uani 1 1 d . . . H47 H 1.0904 0.6593 0.5202 0.049 Uiso 1 1 calc R . . C48 C 0.8753(3) 0.6118(2) 0.49259(17) 0.0432(8) Uani 1 1 d . . . H48A H 0.8372 0.6115 0.5334 0.052 Uiso 1 1 calc R . . H48B H 0.9314 0.5651 0.4916 0.052 Uiso 1 1 calc R . . C49 C 0.7825(3) 0.5990(2) 0.43870(19) 0.0491(9) Uani 1 1 d . . . H49A H 0.8198 0.5817 0.3994 0.059 Uiso 1 1 calc R . . H49B H 0.7238 0.5543 0.4487 0.059 Uiso 1 1 calc R . . C50 C 0.6145(3) 0.6848(2) 0.41085(16) 0.0404(7) Uani 1 1 d . . . H50 H 0.5715 0.6322 0.4060 0.048 Uiso 1 1 calc R . . C51 C 0.5528(3) 0.7620(2) 0.39502(14) 0.0352(7) Uani 1 1 d . . . C52 C 0.4295(3) 0.7522(2) 0.37734(15) 0.0405(7) Uani 1 1 d . . . H52 H 0.3918 0.6976 0.3777 0.049 Uiso 1 1 calc R . . C53 C 0.3648(3) 0.8220(2) 0.35973(15) 0.0384(7) Uani 1 1 d . . . C54 C 0.4204(3) 0.9037(2) 0.35937(17) 0.0471(9) Uani 1 1 d . . . H54 H 0.3760 0.9512 0.3479 0.057 Uiso 1 1 calc R . . C55 C 0.5407(3) 0.9147(2) 0.37590(16) 0.0433(8) Uani 1 1 d . . . H55 H 0.5769 0.9697 0.3746 0.052 Uiso 1 1 calc R . . C56 C 0.6105(3) 0.8447(2) 0.39470(13) 0.0327(6) Uani 1 1 d . . . C57 C 0.6012(3) 0.6725(2) 0.89943(14) 0.0374(7) Uani 1 1 d . . . C58 C 0.5221(3) 0.6105(2) 0.86762(17) 0.0491(9) Uani 1 1 d . . . H58 H 0.5488 0.5553 0.8581 0.059 Uiso 1 1 calc R . . C59 C 0.4060(3) 0.6304(3) 0.85037(17) 0.0523(9) Uani 1 1 d . . . H59 H 0.3549 0.5884 0.8298 0.063 Uiso 1 1 calc R . . C60 C 0.3649(3) 0.7120(3) 0.86339(17) 0.0476(9) Uani 1 1 d . . . C61 C 0.4385(3) 0.7745(2) 0.89318(16) 0.0480(9) Uani 1 1 d . . . H61 H 0.4101 0.8295 0.9014 0.058 Uiso 1 1 calc R . . C62 C 0.5582(3) 0.7558(2) 0.91167(15) 0.0410(8) Uani 1 1 d . . . C63 C 0.6272(3) 0.8222(2) 0.94686(16) 0.0441(8) Uani 1 1 d . . . H63 H 0.5896 0.8737 0.9561 0.053 Uiso 1 1 calc R . . C64 C 0.7937(3) 0.8839(2) 1.01110(17) 0.0475(9) Uani 1 1 d . . . H64A H 0.7822 0.8687 1.0552 0.057 Uiso 1 1 calc R . . H64B H 0.7574 0.9392 1.0037 0.057 Uiso 1 1 calc R . . C65 C 0.9254(3) 0.8900(2) 0.99885(16) 0.0451(8) Uani 1 1 d . . . H65A H 0.9385 0.9238 0.9612 0.054 Uiso 1 1 calc R . . H65B H 0.9694 0.9182 1.0353 0.054 Uiso 1 1 calc R . . C66 C 1.0749(3) 0.7827(2) 1.00709(15) 0.0412(8) Uani 1 1 d . . . H66 H 1.1227 0.8272 1.0270 0.049 Uiso 1 1 calc R . . C67 C 1.1276(3) 0.7004(2) 1.00003(15) 0.0394(7) Uani 1 1 d . . . C68 C 1.2478(3) 0.6932(2) 1.02328(16) 0.0460(8) Uani 1 1 d . . . H68 H 1.2893 0.7414 1.0421 0.055 Uiso 1 1 calc R . . C69 C 1.3029(3) 0.6166(3) 1.01823(16) 0.0480(9) Uani 1 1 d . . . C70 C 1.2424(3) 0.5432(2) 0.98995(16) 0.0476(9) Uani 1 1 d . . . H70 H 1.2806 0.4907 0.9872 0.057 Uiso 1 1 calc R . . C71 C 1.1264(3) 0.5493(2) 0.96633(16) 0.0439(8) Uani 1 1 d . . . H71 H 1.0868 0.5002 0.9476 0.053 Uiso 1 1 calc R . . C72 C 1.0657(3) 0.6272(2) 0.96950(14) 0.0379(7) Uani 1 1 d . . . C73 C 0.4155(6) 0.9204(5) 0.0690(4) 0.125(3) Uani 1 1 d . . . C74 C 0.4172(18) 0.5939(8) 0.5193(9) 0.339(13) Uani 1 1 d . . . O1 O 0.6319(2) 0.91330(17) 0.18823(14) 0.0584(7) Uani 1 1 d . . . O2 O 1.2151(2) 0.75911(15) 0.16207(12) 0.0458(6) Uani 1 1 d . . . O3 O 0.5269(2) 0.61480(17) 0.69191(15) 0.0630(8) Uani 1 1 d . . . O4 O 1.14608(19) 0.69778(15) 0.65940(12) 0.0453(6) Uani 1 1 d . . . O5 O 0.9557(2) 0.63000(14) 0.94451(10) 0.0393(5) Uani 1 1 d . . . O6 O 0.7101(2) 0.64802(14) 0.91667(10) 0.0376(5) Uani 1 1 d . . . O7 O 0.72374(18) 0.86019(14) 0.41101(10) 0.0361(5) Uani 1 1 d . . . O8 O 0.95600(19) 0.87156(14) 0.46300(10) 0.0373(5) Uani 1 1 d . . . O9 O 0.5202(5) 0.9735(3) 0.0775(2) 0.1278(16) Uani 1 1 d . . . O10 O 0.4720(12) 0.5610(9) 0.5596(5) 0.334(7) Uani 1 1 d . . . O1W O 0.2864(2) 0.55910(19) 0.69890(16) 0.0729(9) 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 0.0291(2) 0.0272(2) 0.02249(19) 0.00122(16) 0.00233(15) 0.00412(16) Fe2 0.0258(2) 0.0268(2) 0.02397(19) 0.00351(16) 0.00300(15) 0.00270(16) Mn1 0.0439(3) 0.0292(2) 0.0266(2) -0.00106(18) -0.00117(19) 0.0021(2) Mn2 0.0299(2) 0.0310(2) 0.0267(2) 0.00273(18) -0.00052(17) 0.00099(18) Br1 0.03565(19) 0.0799(3) 0.0564(2) -0.0030(2) -0.00500(16) -0.00030(18) Br2 0.03456(18) 0.0611(2) 0.0588(2) -0.00362(19) -0.00733(15) 0.00760(16) Br3 0.0445(2) 0.0832(3) 0.0615(2) 0.0122(2) -0.00299(18) 0.0033(2) Br4 0.0517(2) 0.0829(3) 0.0599(2) 0.0028(2) -0.00526(19) 0.0146(2) N1 0.0425(15) 0.0511(18) 0.0284(13) -0.0005(12) 0.0022(11) 0.0012(13) N2 0.0521(17) 0.0403(16) 0.0306(14) 0.0004(12) 0.0003(12) 0.0028(13) N3 0.0428(15) 0.0523(18) 0.0304(14) 0.0036(13) 0.0048(11) 0.0118(13) N4 0.0516(17) 0.0357(15) 0.0305(13) 0.0033(11) 0.0021(12) 0.0010(13) N5 0.0316(13) 0.0385(15) 0.0275(12) -0.0010(11) 0.0028(10) 0.0022(11) N6 0.0335(13) 0.0274(13) 0.0281(12) 0.0011(10) 0.0035(10) 0.0077(10) N7 0.0310(13) 0.0292(13) 0.0284(12) 0.0033(10) 0.0041(10) 0.0009(10) N8 0.0338(13) 0.0339(14) 0.0231(11) 0.0014(10) 0.0035(9) 0.0065(11) N9 0.0302(13) 0.0357(14) 0.0265(12) 0.0044(11) 0.0047(10) 0.0064(11) N10 0.0279(12) 0.0272(13) 0.0332(13) 0.0049(10) 0.0021(10) 0.0015(10) N11 0.0260(12) 0.0270(13) 0.0296(12) 0.0037(10) 0.0025(9) 0.0039(10) N12 0.0293(12) 0.0319(13) 0.0248(11) 0.0067(10) 0.0036(9) 0.0012(10) N13 0.0407(14) 0.0344(14) 0.0290(12) 0.0018(11) 0.0000(11) 0.0036(12) N14 0.0385(14) 0.0299(14) 0.0419(14) 0.0056(12) -0.0010(11) 0.0016(11) N15 0.0539(17) 0.0332(15) 0.0298(13) -0.0019(11) -0.0032(12) 0.0058(13) N16 0.0487(16) 0.0301(14) 0.0287(12) 0.0016(11) 0.0007(11) -0.0011(12) C1 0.0274(14) 0.0297(16) 0.0336(15) 0.0003(12) 0.0055(11) 0.0040(12) C2 0.0333(15) 0.0269(15) 0.0328(16) 0.0041(12) 0.0024(12) 0.0050(12) C3 0.0250(14) 0.0293(15) 0.0320(15) 0.0006(12) 0.0051(11) 0.0038(12) C4 0.0321(15) 0.0232(14) 0.0322(15) 0.0041(12) 0.0049(12) -0.0003(12) C5 0.0438(18) 0.0347(18) 0.0377(17) 0.0021(14) 0.0010(14) 0.0052(14) C6 0.056(2) 0.0315(18) 0.0454(19) -0.0020(15) -0.0049(16) 0.0076(16) C7 0.050(2) 0.0396(19) 0.0452(19) -0.0110(15) -0.0018(16) 0.0195(16) C8 0.0354(17) 0.045(2) 0.0392(17) -0.0047(15) 0.0032(13) 0.0117(15) C9 0.0324(15) 0.0392(17) 0.0260(14) -0.0021(13) 0.0011(11) 0.0063(13) C10 0.0308(15) 0.0372(17) 0.0288(14) -0.0013(13) 0.0003(11) 0.0029(13) C11 0.0391(16) 0.0306(16) 0.0250(14) 0.0004(12) 0.0011(12) 0.0000(13) C12 0.0411(18) 0.0403(19) 0.0346(16) 0.0017(14) 0.0011(13) -0.0042(15) C13 0.053(2) 0.0390(19) 0.0401(18) 0.0049(15) -0.0030(15) -0.0093(16) C14 0.068(2) 0.0267(17) 0.0424(18) 0.0016(14) -0.0043(17) -0.0012(17) C15 0.051(2) 0.0318(17) 0.0399(17) 0.0024(14) 0.0013(15) 0.0077(15) C16 0.0382(16) 0.0300(16) 0.0241(13) -0.0033(12) 0.0004(11) 0.0055(13) C17 0.0403(18) 0.0407(19) 0.0351(16) -0.0007(14) 0.0061(13) 0.0102(15) C18 0.0340(16) 0.0393(18) 0.0317(15) 0.0008(13) 0.0037(12) 0.0087(14) C19 0.0349(17) 0.058(2) 0.0470(19) -0.0020(17) 0.0030(15) 0.0123(17) C20 0.0293(17) 0.067(3) 0.054(2) -0.0055(19) 0.0055(15) -0.0033(17) C21 0.042(2) 0.055(2) 0.052(2) 0.0013(18) 0.0131(16) -0.0099(17) C22 0.0399(18) 0.0405(19) 0.0481(19) 0.0021(16) 0.0096(15) 0.0015(15) C23 0.0401(17) 0.0395(19) 0.0384(17) 0.0047(14) 0.0095(14) 0.0066(15) C24 0.050(2) 0.044(2) 0.0437(19) 0.0027(16) 0.0129(15) 0.0204(17) C25 0.0355(18) 0.067(3) 0.050(2) 0.0075(19) 0.0116(15) 0.0184(18) C26 0.0310(16) 0.054(2) 0.0459(18) 0.0019(17) 0.0092(14) 0.0081(15) C27 0.0319(15) 0.0409(18) 0.0323(15) 0.0048(14) 0.0052(12) 0.0058(14) C28 0.0308(16) 0.0408(19) 0.0429(17) 0.0010(15) 0.0044(13) 0.0014(14) C29 0.0368(16) 0.0310(16) 0.0321(15) 0.0048(13) 0.0010(12) 0.0025(13) C30 0.0371(18) 0.0359(19) 0.069(2) -0.0003(17) 0.0080(16) -0.0032(15) C31 0.056(2) 0.0291(19) 0.090(3) -0.004(2) 0.004(2) -0.0057(17) C32 0.047(2) 0.0329(18) 0.061(2) -0.0048(16) 0.0007(17) 0.0076(15) C33 0.0343(16) 0.0371(18) 0.0391(17) 0.0008(14) 0.0025(13) 0.0053(14) C34 0.0309(15) 0.0324(16) 0.0263(14) 0.0048(12) -0.0015(11) 0.0028(12) C35 0.0284(15) 0.0335(16) 0.0291(14) 0.0052(12) 0.0016(11) 0.0025(12) C36 0.0300(15) 0.0349(16) 0.0260(14) 0.0033(12) 0.0004(11) 0.0004(12) C37 0.0353(17) 0.046(2) 0.0414(17) 0.0033(15) 0.0070(14) -0.0021(15) C38 0.046(2) 0.042(2) 0.051(2) 0.0050(16) 0.0078(16) -0.0131(16) C39 0.054(2) 0.0310(17) 0.0428(18) 0.0085(15) 0.0059(15) -0.0032(15) C40 0.0398(17) 0.0307(17) 0.0387(17) 0.0029(13) 0.0035(13) 0.0011(14) C41 0.0358(16) 0.0430(19) 0.0269(14) -0.0045(13) 0.0028(12) 0.0007(14) C42 0.0422(18) 0.043(2) 0.0389(17) 0.0004(15) 0.0027(14) -0.0001(15) C43 0.0375(18) 0.055(2) 0.0404(18) -0.0061(16) 0.0023(14) -0.0060(16) C44 0.0324(17) 0.063(2) 0.0381(17) -0.0035(17) -0.0004(13) 0.0002(16) C45 0.0392(18) 0.053(2) 0.0411(18) 0.0000(16) 0.0008(14) 0.0054(16) C46 0.0357(16) 0.046(2) 0.0309(15) 0.0006(14) -0.0009(13) 0.0031(15) C47 0.0416(18) 0.043(2) 0.0377(17) 0.0048(15) -0.0034(14) 0.0115(15) C48 0.048(2) 0.0309(17) 0.0508(19) 0.0109(15) -0.0048(16) 0.0042(15) C49 0.048(2) 0.0353(19) 0.064(2) 0.0032(17) -0.0065(17) 0.0033(16) C50 0.0369(17) 0.0365(18) 0.0471(19) 0.0046(15) -0.0021(14) -0.0056(14) C51 0.0386(17) 0.0337(17) 0.0331(15) 0.0011(13) -0.0025(13) 0.0016(14) C52 0.0375(17) 0.0403(19) 0.0433(18) 0.0007(15) -0.0007(14) -0.0018(15) C53 0.0288(15) 0.050(2) 0.0364(16) -0.0001(15) -0.0023(12) 0.0055(14) C54 0.0423(19) 0.046(2) 0.054(2) 0.0135(17) -0.0013(16) 0.0106(16) C55 0.0396(18) 0.0389(19) 0.051(2) 0.0099(16) -0.0044(15) -0.0004(15) C56 0.0342(16) 0.0357(17) 0.0281(14) 0.0034(13) -0.0005(12) 0.0013(13) C57 0.0440(18) 0.0389(18) 0.0296(15) 0.0042(13) 0.0028(13) 0.0010(15) C58 0.058(2) 0.043(2) 0.0459(19) 0.0029(16) -0.0034(17) 0.0008(17) C59 0.050(2) 0.056(2) 0.049(2) 0.0038(18) -0.0076(17) -0.0093(19) C60 0.0407(19) 0.060(2) 0.0427(19) 0.0094(17) -0.0001(15) -0.0007(17) C61 0.053(2) 0.046(2) 0.0459(19) 0.0075(17) 0.0019(16) 0.0099(17) C62 0.0455(19) 0.0420(19) 0.0351(16) -0.0007(15) 0.0000(14) 0.0029(15) C63 0.052(2) 0.0393(19) 0.0416(18) 0.0024(15) -0.0009(15) 0.0130(16) C64 0.062(2) 0.0357(19) 0.0436(19) -0.0087(15) -0.0087(16) 0.0084(17) C65 0.062(2) 0.0333(18) 0.0390(17) -0.0011(14) -0.0058(16) 0.0017(16) C66 0.049(2) 0.0395(19) 0.0346(16) 0.0009(14) 0.0012(14) -0.0066(16) C67 0.0480(19) 0.0382(18) 0.0321(16) -0.0009(14) 0.0033(14) 0.0029(15) C68 0.050(2) 0.050(2) 0.0377(18) -0.0012(16) 0.0011(15) -0.0002(17) C69 0.047(2) 0.058(2) 0.0402(18) 0.0042(17) 0.0042(15) 0.0073(18) C70 0.054(2) 0.045(2) 0.0452(19) 0.0030(16) 0.0086(16) 0.0117(17) C71 0.053(2) 0.0372(19) 0.0418(18) 0.0008(15) 0.0051(15) 0.0034(16) C72 0.0477(19) 0.0396(19) 0.0269(15) 0.0046(13) 0.0035(13) 0.0035(15) C73 0.098(5) 0.132(6) 0.145(6) 0.019(5) 0.007(4) -0.037(4) C74 0.48(3) 0.186(11) 0.39(2) 0.202(15) 0.25(2) 0.186(15) O1 0.0467(15) 0.0446(15) 0.086(2) 0.0109(14) 0.0108(13) 0.0204(12) O2 0.0326(12) 0.0450(14) 0.0605(15) 0.0003(12) 0.0106(11) 0.0019(11) O3 0.0327(13) 0.0510(16) 0.105(2) -0.0118(15) 0.0161(14) -0.0073(12) O4 0.0302(12) 0.0397(13) 0.0673(16) 0.0081(12) 0.0094(11) 0.0066(10) O5 0.0465(13) 0.0339(12) 0.0369(11) -0.0036(10) -0.0013(10) 0.0037(10) O6 0.0444(13) 0.0322(12) 0.0357(11) -0.0013(9) -0.0020(9) 0.0022(10) O7 0.0325(11) 0.0346(12) 0.0411(12) 0.0078(10) -0.0030(9) -0.0009(9) O8 0.0358(12) 0.0328(12) 0.0425(12) 0.0019(10) -0.0049(9) -0.0009(9) O9 0.157(4) 0.127(4) 0.102(3) 0.041(3) -0.005(3) 0.032(3) O10 0.376(15) 0.393(17) 0.213(9) -0.136(11) -0.058(9) -0.052(14) O1W 0.0470(16) 0.0541(18) 0.117(3) 0.0170(17) -0.0074(16) -0.0021(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 1.882(2) . ? Fe1 N6 1.899(2) . ? Fe1 C1 1.960(3) . ? Fe1 C2 1.964(3) . ? Fe1 N5 1.996(2) . ? Fe1 N8 2.006(2) . ? Fe2 N10 1.885(2) . ? Fe2 N11 1.892(2) . ? Fe2 C3 1.976(3) . ? Fe2 N9 1.987(2) . ? Fe2 C4 1.989(3) . ? Fe2 N12 1.995(2) . ? Mn1 O5 1.877(2) . ? Mn1 O6 1.889(2) . ? Mn1 N15 1.992(3) . ? Mn1 N16 1.998(3) . ? Mn1 N2 2.305(3) 1_556 ? Mn1 N4 2.372(3) . ? Mn2 O8 1.868(2) . ? Mn2 O7 1.887(2) . ? Mn2 N14 1.989(3) . ? Mn2 N13 1.990(3) . ? Mn2 N1 2.304(3) . ? Mn2 N3 2.333(3) . ? Br1 C44 1.907(3) . ? Br2 C53 1.896(3) . ? Br3 C60 1.903(4) . ? Br4 C69 1.908(4) . ? N1 C1 1.150(4) . ? N2 C2 1.139(4) . ? N2 Mn1 2.305(3) 1_554 ? N3 C3 1.142(4) . ? N4 C4 1.147(4) . ? N5 C22 1.338(4) . ? N5 C18 1.358(4) . ? N6 C17 1.339(4) . ? N6 C16 1.402(4) . ? N7 C10 1.344(4) . ? N7 C11 1.394(4) . ? N8 C5 1.333(4) . ? N8 C9 1.352(4) . ? N9 C23 1.333(4) . ? N9 C27 1.352(4) . ? N10 C28 1.342(4) . ? N10 C29 1.404(4) . ? N11 C35 1.345(4) . ? N11 C34 1.391(4) . ? N12 C40 1.348(4) . ? N12 C36 1.353(4) . ? N13 C47 1.296(4) . ? N13 C48 1.465(4) . ? N14 C50 1.277(4) . ? N14 C49 1.480(4) . ? N15 C63 1.290(4) . ? N15 C64 1.471(4) . ? N16 C66 1.286(4) . ? N16 C65 1.471(4) . ? C5 C6 1.385(4) . ? C5 H5 0.9300 . ? C6 C7 1.360(5) . ? C6 H6 0.9300 . ? C7 C8 1.367(5) . ? C7 H7 0.9300 . ? C8 C9 1.374(4) . ? C8 H8 0.9300 . ? C9 C10 1.497(4) . ? C10 O2 1.235(4) . ? C11 C12 1.396(4) . ? C11 C16 1.418(4) . ? C12 C13 1.388(5) . ? C12 H12 0.9300 . ? C13 C14 1.377(5) . ? C13 H13 0.9300 . ? C14 C15 1.381(5) . ? C14 H14 0.9300 . ? C15 C16 1.396(4) . ? C15 H15 0.9300 . ? C17 O1 1.242(4) . ? C17 C18 1.486(5) . ? C18 C19 1.379(4) . ? C19 C20 1.372(5) . ? C19 H19 0.9300 . ? C20 C21 1.366(5) . ? C20 H20 0.9300 . ? C21 C22 1.383(5) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.387(4) . ? C23 H23 0.9300 . ? C24 C25 1.372(5) . ? C24 H24 0.9300 . ? C25 C26 1.374(5) . ? C25 H25 0.9300 . ? C26 C27 1.375(4) . ? C26 H26 0.9300 . ? C27 C28 1.491(5) . ? C28 O3 1.233(4) . ? C29 C30 1.383(4) . ? C29 C34 1.414(4) . ? C30 C31 1.380(5) . ? C30 H30 0.9300 . ? C31 C32 1.372(5) . ? C31 H31 0.9300 . ? C32 C33 1.378(5) . ? C32 H32 0.9300 . ? C33 C34 1.401(4) . ? C33 H33 0.9300 . ? C35 O4 1.232(3) . ? C35 C36 1.493(4) . ? C36 C37 1.377(4) . ? C37 C38 1.387(5) . ? C37 H37 0.9300 . ? C38 C39 1.379(5) . ? C38 H38 0.9300 . ? C39 C40 1.373(4) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 O8 1.319(4) . ? C41 C42 1.403(5) . ? C41 C46 1.406(5) . ? C42 C43 1.370(5) . ? C42 H42 0.9300 . ? C43 C44 1.380(5) . ? C43 H43 0.9300 . ? C44 C45 1.368(5) . ? C45 C46 1.411(4) . ? C45 H45 0.9300 . ? C46 C47 1.433(5) . ? C47 H47 0.9300 . ? C48 C49 1.497(5) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.434(5) . ? C50 H50 0.9300 . ? C51 C52 1.409(4) . ? C51 C56 1.412(4) . ? C52 C53 1.365(5) . ? C52 H52 0.9300 . ? C53 C54 1.387(5) . ? C54 C55 1.374(5) . ? C54 H54 0.9300 . ? C55 C56 1.406(4) . ? C55 H55 0.9300 . ? C56 O7 1.305(3) . ? C57 O6 1.322(4) . ? C57 C62 1.407(5) . ? C57 C58 1.409(5) . ? C58 C59 1.375(5) . ? C58 H58 0.9300 . ? C59 C60 1.379(5) . ? C59 H59 0.9300 . ? C60 C61 1.362(5) . ? C61 C62 1.414(5) . ? C61 H61 0.9300 . ? C62 C63 1.425(5) . ? C63 H63 0.9300 . ? C64 C65 1.504(5) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 C67 1.424(5) . ? C66 H66 0.9300 . ? C67 C68 1.414(5) . ? C67 C72 1.422(5) . ? C68 C69 1.353(5) . ? C68 H68 0.9300 . ? C69 C70 1.399(5) . ? C70 C71 1.370(5) . ? C70 H70 0.9300 . ? C71 C72 1.401(5) . ? C71 H71 0.9300 . ? C72 O5 1.313(4) . ? C73 O9 1.406(7) . ? C74 O10 1.157(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Fe1 N6 83.60(10) . . ? N7 Fe1 C1 94.06(11) . . ? N6 Fe1 C1 93.37(11) . . ? N7 Fe1 C2 93.23(11) . . ? N6 Fe1 C2 91.69(11) . . ? C1 Fe1 C2 171.55(12) . . ? N7 Fe1 N5 165.39(11) . . ? N6 Fe1 N5 81.80(11) . . ? C1 Fe1 N5 86.41(11) . . ? C2 Fe1 N5 87.63(11) . . ? N7 Fe1 N8 82.13(10) . . ? N6 Fe1 N8 165.27(10) . . ? C1 Fe1 N8 91.29(11) . . ? C2 Fe1 N8 85.47(11) . . ? N5 Fe1 N8 112.46(10) . . ? N10 Fe2 N11 83.89(10) . . ? N10 Fe2 C3 90.99(11) . . ? N11 Fe2 C3 91.72(11) . . ? N10 Fe2 N9 82.10(10) . . ? N11 Fe2 N9 165.89(11) . . ? C3 Fe2 N9 90.25(10) . . ? N10 Fe2 C4 93.90(11) . . ? N11 Fe2 C4 92.85(11) . . ? C3 Fe2 C4 173.64(12) . . ? N9 Fe2 C4 86.39(11) . . ? N10 Fe2 N12 165.40(10) . . ? N11 Fe2 N12 82.53(10) . . ? C3 Fe2 N12 84.10(10) . . ? N9 Fe2 N12 111.58(10) . . ? C4 Fe2 N12 92.11(10) . . ? O5 Mn1 O6 96.03(10) . . ? O5 Mn1 N15 172.12(11) . . ? O6 Mn1 N15 91.29(11) . . ? O5 Mn1 N16 91.26(11) . . ? O6 Mn1 N16 172.70(10) . . ? N15 Mn1 N16 81.42(11) . . ? O5 Mn1 N2 90.65(10) . 1_556 ? O6 Mn1 N2 93.55(10) . 1_556 ? N15 Mn1 N2 85.98(10) . 1_556 ? N16 Mn1 N2 86.16(10) . 1_556 ? O5 Mn1 N4 92.56(9) . . ? O6 Mn1 N4 86.20(9) . . ? N15 Mn1 N4 90.83(10) . . ? N16 Mn1 N4 93.69(10) . . ? N2 Mn1 N4 176.79(10) 1_556 . ? O8 Mn2 O7 94.65(9) . . ? O8 Mn2 N14 173.33(10) . . ? O7 Mn2 N14 91.53(10) . . ? O8 Mn2 N13 92.09(10) . . ? O7 Mn2 N13 173.19(10) . . ? N14 Mn2 N13 81.78(11) . . ? O8 Mn2 N1 92.61(10) . . ? O7 Mn2 N1 91.36(10) . . ? N14 Mn2 N1 84.72(10) . . ? N13 Mn2 N1 89.31(10) . . ? O8 Mn2 N3 92.29(10) . . ? O7 Mn2 N3 93.39(9) . . ? N14 Mn2 N3 89.84(11) . . ? N13 Mn2 N3 85.34(10) . . ? N1 Mn2 N3 172.87(11) . . ? C1 N1 Mn2 155.1(2) . . ? C2 N2 Mn1 149.0(3) . 1_554 ? C3 N3 Mn2 150.5(2) . . ? C4 N4 Mn1 161.3(2) . . ? C22 N5 C18 118.2(3) . . ? C22 N5 Fe1 129.5(2) . . ? C18 N5 Fe1 112.3(2) . . ? C17 N6 C16 126.0(3) . . ? C17 N6 Fe1 119.1(2) . . ? C16 N6 Fe1 114.84(18) . . ? C10 N7 C11 125.5(3) . . ? C10 N7 Fe1 119.3(2) . . ? C11 N7 Fe1 115.05(19) . . ? C5 N8 C9 117.3(3) . . ? C5 N8 Fe1 130.2(2) . . ? C9 N8 Fe1 112.1(2) . . ? C23 N9 C27 117.9(3) . . ? C23 N9 Fe2 129.7(2) . . ? C27 N9 Fe2 112.4(2) . . ? C28 N10 C29 125.9(3) . . ? C28 N10 Fe2 119.1(2) . . ? C29 N10 Fe2 114.75(19) . . ? C35 N11 C34 126.9(2) . . ? C35 N11 Fe2 118.6(2) . . ? C34 N11 Fe2 114.51(18) . . ? C40 N12 C36 117.9(3) . . ? C40 N12 Fe2 129.7(2) . . ? C36 N12 Fe2 111.74(19) . . ? C47 N13 C48 121.4(3) . . ? C47 N13 Mn2 125.3(2) . . ? C48 N13 Mn2 113.3(2) . . ? C50 N14 C49 120.0(3) . . ? C50 N14 Mn2 126.4(2) . . ? C49 N14 Mn2 113.3(2) . . ? C63 N15 C64 120.0(3) . . ? C63 N15 Mn1 126.1(2) . . ? C64 N15 Mn1 113.6(2) . . ? C66 N16 C65 120.1(3) . . ? C66 N16 Mn1 125.3(2) . . ? C65 N16 Mn1 114.5(2) . . ? N1 C1 Fe1 175.0(3) . . ? N2 C2 Fe1 175.9(3) . . ? N3 C3 Fe2 172.5(3) . . ? N4 C4 Fe2 175.9(3) . . ? N8 C5 C6 122.6(3) . . ? N8 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C7 C6 C5 119.6(3) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C6 C7 C8 118.4(3) . . ? C6 C7 H7 120.8 . . ? C8 C7 H7 120.8 . . ? C7 C8 C9 119.9(3) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? N8 C9 C8 122.2(3) . . ? N8 C9 C10 115.3(3) . . ? C8 C9 C10 122.5(3) . . ? O2 C10 N7 128.0(3) . . ? O2 C10 C9 121.1(3) . . ? N7 C10 C9 110.8(3) . . ? N7 C11 C12 126.4(3) . . ? N7 C11 C16 113.8(3) . . ? C12 C11 C16 119.8(3) . . ? C13 C12 C11 119.0(3) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C14 C13 C12 121.1(3) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C15 120.9(3) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C14 C15 C16 119.4(3) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C15 C16 N6 127.6(3) . . ? C15 C16 C11 119.7(3) . . ? N6 C16 C11 112.6(3) . . ? O1 C17 N6 127.9(3) . . ? O1 C17 C18 121.2(3) . . ? N6 C17 C18 110.9(3) . . ? N5 C18 C19 121.5(3) . . ? N5 C18 C17 115.7(3) . . ? C19 C18 C17 122.9(3) . . ? C20 C19 C18 119.6(3) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C21 C20 C19 119.0(3) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? C20 C21 C22 119.5(3) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? N5 C22 C21 122.1(3) . . ? N5 C22 H22 118.9 . . ? C21 C22 H22 118.9 . . ? N9 C23 C24 123.0(3) . . ? N9 C23 H23 118.5 . . ? C24 C23 H23 118.5 . . ? C25 C24 C23 118.3(3) . . ? C25 C24 H24 120.8 . . ? C23 C24 H24 120.8 . . ? C24 C25 C26 119.4(3) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C25 C26 C27 119.3(3) . . ? C25 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? N9 C27 C26 122.0(3) . . ? N9 C27 C28 115.4(3) . . ? C26 C27 C28 122.6(3) . . ? O3 C28 N10 127.6(3) . . ? O3 C28 C27 121.8(3) . . ? N10 C28 C27 110.6(3) . . ? C30 C29 N10 127.1(3) . . ? C30 C29 C34 120.0(3) . . ? N10 C29 C34 112.9(3) . . ? C31 C30 C29 119.3(3) . . ? C31 C30 H30 120.4 . . ? C29 C30 H30 120.4 . . ? C32 C31 C30 121.5(3) . . ? C32 C31 H31 119.2 . . ? C30 C31 H31 119.2 . . ? C31 C32 C33 120.2(3) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C32 C33 C34 119.8(3) . . ? C32 C33 H33 120.1 . . ? C34 C33 H33 120.1 . . ? N11 C34 C33 126.9(3) . . ? N11 C34 C29 113.9(3) . . ? C33 C34 C29 119.2(3) . . ? O4 C35 N11 128.2(3) . . ? O4 C35 C36 121.1(3) . . ? N11 C35 C36 110.7(2) . . ? N12 C36 C37 121.8(3) . . ? N12 C36 C35 116.1(3) . . ? C37 C36 C35 121.8(3) . . ? C36 C37 C38 119.5(3) . . ? C36 C37 H37 120.3 . . ? C38 C37 H37 120.3 . . ? C39 C38 C37 118.9(3) . . ? C39 C38 H38 120.5 . . ? C37 C38 H38 120.5 . . ? C40 C39 C38 118.7(3) . . ? C40 C39 H39 120.6 . . ? C38 C39 H39 120.6 . . ? N12 C40 C39 123.1(3) . . ? N12 C40 H40 118.5 . . ? C39 C40 H40 118.5 . . ? O8 C41 C42 118.1(3) . . ? O8 C41 C46 123.6(3) . . ? C42 C41 C46 118.2(3) . . ? C43 C42 C41 120.9(3) . . ? C43 C42 H42 119.5 . . ? C41 C42 H42 119.5 . . ? C42 C43 C44 120.5(3) . . ? C42 C43 H43 119.7 . . ? C44 C43 H43 119.7 . . ? C45 C44 C43 120.7(3) . . ? C45 C44 Br1 118.8(3) . . ? C43 C44 Br1 120.5(3) . . ? C44 C45 C46 119.8(3) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C41 C46 C45 119.9(3) . . ? C41 C46 C47 123.3(3) . . ? C45 C46 C47 116.9(3) . . ? N13 C47 C46 125.4(3) . . ? N13 C47 H47 117.3 . . ? C46 C47 H47 117.3 . . ? N13 C48 C49 108.7(3) . . ? N13 C48 H48A 110.0 . . ? C49 C48 H48A 110.0 . . ? N13 C48 H48B 110.0 . . ? C49 C48 H48B 110.0 . . ? H48A C48 H48B 108.3 . . ? N14 C49 C48 106.8(3) . . ? N14 C49 H49A 110.4 . . ? C48 C49 H49A 110.4 . . ? N14 C49 H49B 110.4 . . ? C48 C49 H49B 110.4 . . ? H49A C49 H49B 108.6 . . ? N14 C50 C51 124.8(3) . . ? N14 C50 H50 117.6 . . ? C51 C50 H50 117.6 . . ? C52 C51 C56 119.8(3) . . ? C52 C51 C50 117.0(3) . . ? C56 C51 C50 123.1(3) . . ? C53 C52 C51 120.8(3) . . ? C53 C52 H52 119.6 . . ? C51 C52 H52 119.6 . . ? C52 C53 C54 119.9(3) . . ? C52 C53 Br2 120.2(3) . . ? C54 C53 Br2 119.9(2) . . ? C55 C54 C53 120.3(3) . . ? C55 C54 H54 119.8 . . ? C53 C54 H54 119.8 . . ? C54 C55 C56 121.6(3) . . ? C54 C55 H55 119.2 . . ? C56 C55 H55 119.2 . . ? O7 C56 C55 118.4(3) . . ? O7 C56 C51 124.2(3) . . ? C55 C56 C51 117.5(3) . . ? O6 C57 C62 124.4(3) . . ? O6 C57 C58 117.8(3) . . ? C62 C57 C58 117.8(3) . . ? C59 C58 C57 121.0(4) . . ? C59 C58 H58 119.5 . . ? C57 C58 H58 119.5 . . ? C58 C59 C60 120.5(4) . . ? C58 C59 H59 119.8 . . ? C60 C59 H59 119.8 . . ? C61 C60 C59 120.7(3) . . ? C61 C60 Br3 119.7(3) . . ? C59 C60 Br3 119.7(3) . . ? C60 C61 C62 120.1(3) . . ? C60 C61 H61 119.9 . . ? C62 C61 H61 119.9 . . ? C57 C62 C61 119.9(3) . . ? C57 C62 C63 122.9(3) . . ? C61 C62 C63 117.0(3) . . ? N15 C63 C62 125.2(3) . . ? N15 C63 H63 117.4 . . ? C62 C63 H63 117.4 . . ? N15 C64 C65 107.9(3) . . ? N15 C64 H64A 110.1 . . ? C65 C64 H64A 110.1 . . ? N15 C64 H64B 110.1 . . ? C65 C64 H64B 110.1 . . ? H64A C64 H64B 108.4 . . ? N16 C65 C64 108.2(3) . . ? N16 C65 H65A 110.1 . . ? C64 C65 H65A 110.1 . . ? N16 C65 H65B 110.1 . . ? C64 C65 H65B 110.1 . . ? H65A C65 H65B 108.4 . . ? N16 C66 C67 126.2(3) . . ? N16 C66 H66 116.9 . . ? C67 C66 H66 116.9 . . ? C68 C67 C72 119.6(3) . . ? C68 C67 C66 117.5(3) . . ? C72 C67 C66 122.8(3) . . ? C69 C68 C67 120.4(3) . . ? C69 C68 H68 119.8 . . ? C67 C68 H68 119.8 . . ? C68 C69 C70 120.9(3) . . ? C68 C69 Br4 118.3(3) . . ? C70 C69 Br4 120.8(3) . . ? C71 C70 C69 119.6(3) . . ? C71 C70 H70 120.2 . . ? C69 C70 H70 120.2 . . ? C70 C71 C72 121.9(3) . . ? C70 C71 H71 119.0 . . ? C72 C71 H71 119.0 . . ? O5 C72 C71 119.4(3) . . ? O5 C72 C67 123.0(3) . . ? C71 C72 C67 117.5(3) . . ? C72 O5 Mn1 130.2(2) . . ? C57 O6 Mn1 128.6(2) . . ? C56 O7 Mn2 129.0(2) . . ? C41 O8 Mn2 129.7(2) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.930 _refine_diff_density_min -0.512 _refine_diff_density_rms 0.092 #===End data_4 _database_code_depnum_ccdc_archive 'CCDC 744630' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H35 Fe Mn N8 O5.50' _chemical_formula_weight 814.54 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2920(13) _cell_length_b 15.4950(17) _cell_length_c 20.801(3) _cell_angle_alpha 92.693(7) _cell_angle_beta 93.138(6) _cell_angle_gamma 92.0650(13) _cell_volume 3627.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7325 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 27.00 _exptl_crystal_description platelet _exptl_crystal_colour brown _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 0.807 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.832 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'ABSCOR; Higashi, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Rigaku IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0.77 _diffrn_standards_decay_% ? _diffrn_reflns_number 15121 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0879 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.00 _reflns_number_total 15121 _reflns_number_gt 12679 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalstructure 3.6.0 (Rigaku/MSC, 2004)' _computing_cell_refinement 'crystalstructure 3.6.0 (Rigaku/MSC, 2004)' _computing_data_reduction 'Crystalstructure 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XP (Sheldrick, 1998)' _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^)+(0.1275P)^2^+4.0416P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15121 _refine_ls_number_parameters 982 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0880 _refine_ls_R_factor_gt 0.0700 _refine_ls_wR_factor_ref 0.1925 _refine_ls_wR_factor_gt 0.1767 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.004 _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 0.87935(4) 0.72381(3) 0.201446(19) 0.01485(12) Uani 1 1 d . . . Fe2 Fe 0.80131(4) 0.77179(3) 0.693694(19) 0.01386(12) Uani 1 1 d . . . Mn1 Mn 0.83470(5) 0.71763(3) 0.95065(2) 0.02140(13) Uani 1 1 d . . . Mn2 Mn 0.84010(4) 0.78415(3) 0.44748(2) 0.01745(13) Uani 1 1 d . . . N1 N 0.9242(3) 0.74988(19) 0.35121(13) 0.0241(6) Uani 1 1 d . . . N2 N 0.8088(3) 0.68133(19) 0.05546(13) 0.0271(6) Uani 1 1 d . . . N3 N 0.7535(3) 0.79908(19) 0.54592(13) 0.0237(6) Uani 1 1 d . . . N4 N 0.8561(3) 0.76021(18) 0.84351(14) 0.0250(6) Uani 1 1 d . . . N5 N 0.7104(2) 0.69500(17) 0.21956(12) 0.0185(5) Uani 1 1 d . . . N6 N 0.8193(2) 0.83818(17) 0.19414(12) 0.0185(5) Uani 1 1 d . . . N7 N 1.0243(2) 0.77926(17) 0.18300(12) 0.0175(5) Uani 1 1 d . . . N8 N 0.9778(2) 0.61691(17) 0.19912(12) 0.0183(5) Uani 1 1 d . . . N9 N 0.6483(2) 0.82143(17) 0.71717(12) 0.0184(5) Uani 1 1 d . . . N10 N 0.7079(2) 0.66614(17) 0.68650(13) 0.0181(5) Uani 1 1 d . . . N11 N 0.9271(2) 0.69868(16) 0.67307(12) 0.0161(5) Uani 1 1 d . . . N12 N 0.9256(2) 0.86646(17) 0.68630(12) 0.0165(5) Uani 1 1 d . . . N13 N 0.9382(3) 0.69127(18) 0.48738(13) 0.0223(6) Uani 1 1 d . . . N14 N 0.7294(2) 0.68099(17) 0.42443(13) 0.0198(5) Uani 1 1 d . . . N15 N 0.7313(3) 0.81929(19) 0.96834(14) 0.0266(6) Uani 1 1 d . . . N16 N 0.9607(3) 0.80326(18) 0.98915(13) 0.0251(6) Uani 1 1 d . . . C1 C 0.9117(3) 0.73836(19) 0.29601(15) 0.0184(6) Uani 1 1 d . . . C2 C 0.8334(3) 0.6935(2) 0.10971(15) 0.0198(6) Uani 1 1 d . . . C3 C 0.7627(3) 0.7922(2) 0.60103(15) 0.0188(6) Uani 1 1 d . . . C4 C 0.8389(3) 0.76579(19) 0.78851(15) 0.0182(6) Uani 1 1 d . . . C5 C 0.9471(3) 0.5319(2) 0.20499(15) 0.0221(6) Uani 1 1 d . . . H5 H 0.8706 0.5178 0.2165 0.027 Uiso 1 1 calc R . . C6 C 1.0244(3) 0.4646(2) 0.19461(16) 0.0254(7) Uani 1 1 d . . . H6 H 0.9998 0.4075 0.1995 0.031 Uiso 1 1 calc R . . C7 C 1.1379(3) 0.4847(2) 0.17699(17) 0.0272(7) Uani 1 1 d . . . H7 H 1.1908 0.4414 0.1690 0.033 Uiso 1 1 calc R . . C8 C 1.1713(3) 0.5717(2) 0.17141(16) 0.0254(7) Uani 1 1 d . . . H8 H 1.2473 0.5868 0.1597 0.030 Uiso 1 1 calc R . . C9 C 1.0906(3) 0.6360(2) 0.18338(14) 0.0195(6) Uani 1 1 d . . . C10 C 1.1220(3) 0.7316(2) 0.17772(15) 0.0202(6) Uani 1 1 d . . . C11 C 1.0194(3) 0.8705(2) 0.17605(14) 0.0182(6) Uani 1 1 d . . . C12 C 1.1148(3) 0.9274(2) 0.16447(15) 0.0231(6) Uani 1 1 d . . . H12 H 1.1909 0.9069 0.1617 0.028 Uiso 1 1 calc R . . C13 C 1.0944(3) 1.0160(2) 0.15711(16) 0.0262(7) Uani 1 1 d . . . H13 H 1.1577 1.0537 0.1500 0.031 Uiso 1 1 calc R . . C14 C 0.9802(3) 1.0476(2) 0.16044(16) 0.0258(7) Uani 1 1 d . . . H14 H 0.9680 1.1059 0.1548 0.031 Uiso 1 1 calc R . . C15 C 0.8845(3) 0.9920(2) 0.17219(15) 0.0225(6) Uani 1 1 d . . . H15 H 0.8086 1.0130 0.1744 0.027 Uiso 1 1 calc R . . C16 C 0.9043(3) 0.9030(2) 0.18081(14) 0.0178(6) Uani 1 1 d . . . C17 C 0.7013(3) 0.8488(2) 0.19672(15) 0.0207(6) Uani 1 1 d . . . C18 C 0.6396(3) 0.7645(2) 0.21135(15) 0.0215(6) Uani 1 1 d . . . C19 C 0.5181(3) 0.7580(2) 0.21653(17) 0.0274(7) Uani 1 1 d . . . H19 H 0.4718 0.8057 0.2104 0.033 Uiso 1 1 calc R . . C20 C 0.4661(3) 0.6791(3) 0.23103(18) 0.0302(8) Uani 1 1 d . . . H20 H 0.3842 0.6732 0.2337 0.036 Uiso 1 1 calc R . . C21 C 0.5384(3) 0.6075(2) 0.24175(18) 0.0288(7) Uani 1 1 d . . . H21 H 0.5053 0.5545 0.2523 0.035 Uiso 1 1 calc R . . C22 C 0.6605(3) 0.6190(2) 0.23598(16) 0.0240(7) Uani 1 1 d . . . H22 H 0.7091 0.5729 0.2437 0.029 Uiso 1 1 calc R . . C23 C 0.6261(3) 0.9024(2) 0.73996(15) 0.0227(6) Uani 1 1 d . . . H23 H 0.6894 0.9423 0.7472 0.027 Uiso 1 1 calc R . . C24 C 0.5128(3) 0.9282(2) 0.75298(17) 0.0271(7) Uani 1 1 d . . . H24 H 0.5000 0.9846 0.7675 0.032 Uiso 1 1 calc R . . C25 C 0.4191(3) 0.8673(2) 0.74366(18) 0.0289(7) Uani 1 1 d . . . H25 H 0.3423 0.8825 0.7519 0.035 Uiso 1 1 calc R . . C26 C 0.4418(3) 0.7820(2) 0.72159(18) 0.0279(7) Uani 1 1 d . . . H26 H 0.3801 0.7406 0.7149 0.033 Uiso 1 1 calc R . . C27 C 0.5567(3) 0.7613(2) 0.71012(15) 0.0220(6) Uani 1 1 d . . . C28 C 0.5905(3) 0.6694(2) 0.69112(16) 0.0231(7) Uani 1 1 d . . . C29 C 0.7714(3) 0.5916(2) 0.66887(15) 0.0182(6) Uani 1 1 d . . . C30 C 0.7241(3) 0.5062(2) 0.6572(2) 0.0333(8) Uani 1 1 d . . . H30 H 0.6435 0.4940 0.6607 0.040 Uiso 1 1 calc R . . C31 C 0.7997(4) 0.4401(2) 0.6402(2) 0.0391(10) Uani 1 1 d . . . H31 H 0.7685 0.3840 0.6323 0.047 Uiso 1 1 calc R . . C32 C 0.9195(3) 0.4570(2) 0.63492(19) 0.0284(7) Uani 1 1 d . . . H32 H 0.9685 0.4121 0.6244 0.034 Uiso 1 1 calc R . . C33 C 0.9678(3) 0.5416(2) 0.64545(15) 0.0218(6) Uani 1 1 d . . . H33 H 1.0484 0.5530 0.6412 0.026 Uiso 1 1 calc R . . C34 C 0.8932(3) 0.60951(19) 0.66249(14) 0.0166(6) Uani 1 1 d . . . C35 C 1.0373(3) 0.7352(2) 0.67069(15) 0.0189(6) Uani 1 1 d . . . C36 C 1.0330(3) 0.8333(2) 0.67433(14) 0.0176(6) Uani 1 1 d . . . C37 C 1.1297(3) 0.8856(2) 0.66007(16) 0.0233(6) Uani 1 1 d . . . H37 H 1.2023 0.8614 0.6528 0.028 Uiso 1 1 calc R . . C38 C 1.1170(3) 0.9750(2) 0.65666(17) 0.0255(7) Uani 1 1 d . . . H38 H 1.1809 1.0108 0.6471 0.031 Uiso 1 1 calc R . . C39 C 1.0071(3) 1.0095(2) 0.66773(16) 0.0234(7) Uani 1 1 d . . . H39 H 0.9959 1.0685 0.6652 0.028 Uiso 1 1 calc R . . C40 C 0.9147(3) 0.9534(2) 0.68275(15) 0.0204(6) Uani 1 1 d . . . H40 H 0.8418 0.9764 0.6908 0.024 Uiso 1 1 calc R . . C41 C 1.0715(3) 0.8611(2) 0.48743(15) 0.0251(7) Uani 1 1 d . . . C42 C 1.1490(3) 0.9363(3) 0.48955(17) 0.0294(7) Uani 1 1 d . . . H42 H 1.1195 0.9894 0.4791 0.035 Uiso 1 1 calc R . . C43 C 1.2682(3) 0.9295(3) 0.50720(18) 0.0352(9) Uani 1 1 d . . . H43 H 1.3177 0.9789 0.5078 0.042 Uiso 1 1 calc R . . C44 C 1.3180(3) 0.8502(3) 0.52446(18) 0.0342(9) Uani 1 1 d . . . C45 C 1.2429(3) 0.7770(3) 0.52349(18) 0.0335(8) Uani 1 1 d . . . H45 H 1.2735 0.7248 0.5353 0.040 Uiso 1 1 calc R . . C46 C 1.1197(3) 0.7804(3) 0.50468(16) 0.0286(7) Uani 1 1 d . . . C47 C 1.0495(3) 0.7007(2) 0.50596(16) 0.0264(7) Uani 1 1 d . . . H47 H 1.0870 0.6526 0.5212 0.032 Uiso 1 1 calc R . . C48 C 0.8726(3) 0.6075(2) 0.49202(17) 0.0272(7) Uani 1 1 d . . . H48A H 0.8295 0.6076 0.5311 0.033 Uiso 1 1 calc R . . H48B H 0.9272 0.5606 0.4928 0.033 Uiso 1 1 calc R . . C49 C 0.7861(3) 0.5962(2) 0.43251(17) 0.0252(7) Uani 1 1 d . . . H49A H 0.8283 0.5802 0.3946 0.030 Uiso 1 1 calc R . . H49B H 0.7264 0.5513 0.4386 0.030 Uiso 1 1 calc R . . C50 C 0.6199(3) 0.6845(2) 0.40485(17) 0.0243(7) Uani 1 1 d . . . H50 H 0.5759 0.6326 0.3984 0.029 Uiso 1 1 calc R . . C51 C 0.5594(3) 0.7644(2) 0.39188(15) 0.0218(6) Uani 1 1 d . . . C52 C 0.4361(3) 0.7567(2) 0.37482(18) 0.0273(7) Uani 1 1 d . . . H52 H 0.3979 0.7025 0.3745 0.033 Uiso 1 1 calc R . . C53 C 0.3700(3) 0.8276(2) 0.35846(16) 0.0249(7) Uani 1 1 d . . . C54 C 0.4306(3) 0.9094(3) 0.35913(18) 0.0298(7) Uani 1 1 d . . . H54 H 0.3880 0.9578 0.3492 0.036 Uiso 1 1 calc R . . C55 C 0.5514(3) 0.9194(2) 0.37411(18) 0.0271(7) Uani 1 1 d . . . H55 H 0.5889 0.9737 0.3728 0.032 Uiso 1 1 calc R . . C56 C 0.6191(3) 0.8469(2) 0.39159(14) 0.0197(6) Uani 1 1 d . . . C57 C 0.5945(3) 0.6735(2) 0.89737(16) 0.0269(7) Uani 1 1 d . . . C58 C 0.5154(4) 0.6118(3) 0.86371(18) 0.0337(8) Uani 1 1 d . . . H58 H 0.5416 0.5570 0.8530 0.040 Uiso 1 1 calc R . . C59 C 0.3993(4) 0.6319(3) 0.84640(19) 0.0379(9) Uani 1 1 d . . . H59 H 0.3494 0.5900 0.8245 0.046 Uiso 1 1 calc R . . C60 C 0.3545(4) 0.7153(3) 0.86126(18) 0.0359(9) Uani 1 1 d . . . C61 C 0.4319(4) 0.7765(3) 0.89302(18) 0.0341(8) Uani 1 1 d . . . H61 H 0.4051 0.8314 0.9027 0.041 Uiso 1 1 calc R . . C62 C 0.5518(3) 0.7580(2) 0.91144(17) 0.0283(7) Uani 1 1 d . . . C63 C 0.6216(4) 0.8252(2) 0.94882(17) 0.0296(8) Uani 1 1 d . . . H63 H 0.5846 0.8762 0.9594 0.036 Uiso 1 1 calc R . . C64 C 0.7894(4) 0.8866(2) 1.01406(17) 0.0300(8) Uani 1 1 d . . . H64A H 0.7801 0.8709 1.0581 0.036 Uiso 1 1 calc R . . H64B H 0.7536 0.9418 1.0081 0.036 Uiso 1 1 calc R . . C65 C 0.9201(4) 0.8929(2) 1.00052(17) 0.0291(7) Uani 1 1 d . . . H65A H 0.9314 0.9262 0.9628 0.035 Uiso 1 1 calc R . . H65B H 0.9653 0.9214 1.0370 0.035 Uiso 1 1 calc R . . C66 C 1.0675(3) 0.7843(2) 1.00763(16) 0.0268(7) Uani 1 1 d . . . H66 H 1.1154 0.8285 1.0282 0.032 Uiso 1 1 calc R . . C67 C 1.1196(3) 0.7007(2) 0.99935(16) 0.0280(7) Uani 1 1 d . . . C68 C 1.2388(4) 0.6924(3) 1.02294(17) 0.0310(8) Uani 1 1 d . . . H68 H 1.2794 0.7406 1.0429 0.037 Uiso 1 1 calc R . . C69 C 1.2975(4) 0.6150(3) 1.01735(18) 0.0339(8) Uani 1 1 d . . . C70 C 1.2325(4) 0.5418(3) 0.98720(18) 0.0331(8) Uani 1 1 d . . . H70 H 1.2689 0.4890 0.9835 0.040 Uiso 1 1 calc R . . C71 C 1.1161(4) 0.5478(2) 0.96331(18) 0.0307(8) Uani 1 1 d . . . H71 H 1.0762 0.4991 0.9437 0.037 Uiso 1 1 calc R . . C72 C 1.0566(3) 0.6269(2) 0.96813(15) 0.0253(7) Uani 1 1 d . . . C73 C 0.4260(6) 0.9264(5) 0.0733(3) 0.080(2) Uani 1 1 d . . . C74 C 0.417(3) 0.5946(16) 0.5242(17) 0.38(2) Uani 1 1 d . . . C75 C 1.4517(3) 0.8465(3) 0.5444(2) 0.0390(9) Uani 1 1 d . . . H75A H 1.4699 0.7885 0.5544 0.059 Uiso 1 1 calc R . . H75B H 1.4703 0.8846 0.5817 0.059 Uiso 1 1 calc R . . H75C H 1.4977 0.8643 0.5096 0.059 Uiso 1 1 calc R . . C76 C 0.2364(3) 0.8182(3) 0.3395(2) 0.0324(8) Uani 1 1 d . . . H76A H 0.2101 0.7589 0.3416 0.049 Uiso 1 1 calc R . . H76B H 0.2222 0.8365 0.2964 0.049 Uiso 1 1 calc R . . H76C H 0.1936 0.8536 0.3687 0.049 Uiso 1 1 calc R . . C77 C 0.2254(4) 0.7363(3) 0.8414(2) 0.0403(9) Uani 1 1 d . . . H77A H 0.2110 0.7947 0.8553 0.060 Uiso 1 1 calc R . . H77B H 0.1718 0.6974 0.8612 0.060 Uiso 1 1 calc R . . H77C H 0.2131 0.7297 0.7954 0.060 Uiso 1 1 calc R . . C78 C 1.4278(4) 0.6073(3) 1.0431(2) 0.0367(9) Uani 1 1 d . . . H78A H 1.4575 0.6623 1.0617 0.055 Uiso 1 1 calc R . . H78B H 1.4753 0.5899 1.0083 0.055 Uiso 1 1 calc R . . H78C H 1.4312 0.5650 1.0754 0.055 Uiso 1 1 calc R . . O1 O 0.6461(2) 0.91718(17) 0.18909(14) 0.0318(6) Uani 1 1 d . . . O2 O 1.2242(2) 0.75741(16) 0.16942(13) 0.0287(5) Uani 1 1 d . . . O3 O 0.5145(2) 0.60897(18) 0.68228(17) 0.0409(7) Uani 1 1 d . . . O4 O 1.1318(2) 0.69764(16) 0.66322(13) 0.0277(5) Uani 1 1 d . . . O5 O 0.9461(2) 0.63001(16) 0.94262(11) 0.0274(5) Uani 1 1 d . . . O6 O 0.7023(2) 0.64792(16) 0.91530(11) 0.0271(5) Uani 1 1 d . . . O7 O 0.7340(2) 0.86072(15) 0.40670(11) 0.0225(5) Uani 1 1 d . . . O8 O 0.9580(2) 0.87071(16) 0.47084(12) 0.0249(5) Uani 1 1 d . . . O9 O 0.5336(4) 0.9747(3) 0.07669(18) 0.0599(10) Uani 1 1 d . . . O10 O 0.4770(19) 0.5344(13) 0.5494(13) 0.395(16) Uani 1 1 d . . . O1W O 0.2742(2) 0.55753(18) 0.69561(16) 0.0394(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0162(2) 0.0165(2) 0.0119(2) -0.00035(15) 0.00193(16) 0.00183(16) Fe2 0.0131(2) 0.0160(2) 0.0127(2) 0.00045(15) 0.00209(15) 0.00079(15) Mn1 0.0307(3) 0.0188(3) 0.0140(2) -0.00206(17) -0.00112(19) -0.00090(19) Mn2 0.0164(2) 0.0215(2) 0.0142(2) -0.00027(17) -0.00036(17) -0.00049(18) N1 0.0229(14) 0.0316(15) 0.0176(13) -0.0018(11) 0.0025(11) 0.0004(11) N2 0.0365(17) 0.0268(15) 0.0174(13) -0.0015(11) -0.0009(12) -0.0010(12) N3 0.0206(14) 0.0324(15) 0.0180(13) 0.0007(11) 0.0010(11) 0.0040(11) N4 0.0302(15) 0.0238(14) 0.0211(14) 0.0013(10) 0.0018(11) -0.0010(11) N5 0.0173(13) 0.0220(13) 0.0160(12) -0.0018(9) 0.0021(10) 0.0007(10) N6 0.0217(13) 0.0185(13) 0.0154(12) -0.0004(9) 0.0025(10) 0.0013(10) N7 0.0179(13) 0.0201(13) 0.0147(11) 0.0000(9) 0.0020(10) 0.0012(10) N8 0.0212(13) 0.0198(13) 0.0138(11) -0.0010(9) 0.0004(10) 0.0026(10) N9 0.0152(12) 0.0241(13) 0.0165(12) 0.0024(10) 0.0030(10) 0.0031(10) N10 0.0158(12) 0.0186(12) 0.0205(12) 0.0026(10) 0.0040(10) 0.0016(10) N11 0.0144(12) 0.0184(12) 0.0154(11) 0.0014(9) 0.0001(9) 0.0016(9) N12 0.0163(12) 0.0194(12) 0.0137(11) 0.0003(9) 0.0016(9) -0.0005(9) N13 0.0234(14) 0.0263(14) 0.0171(12) -0.0009(10) 0.0004(11) 0.0033(11) N14 0.0209(13) 0.0202(13) 0.0182(12) 0.0028(10) -0.0010(10) 0.0008(10) N15 0.0371(17) 0.0218(14) 0.0203(13) -0.0030(11) -0.0004(12) 0.0011(12) N16 0.0374(17) 0.0213(14) 0.0159(12) -0.0016(10) 0.0016(12) -0.0033(12) C1 0.0158(14) 0.0174(14) 0.0222(15) 0.0005(11) 0.0035(12) 0.0019(11) C2 0.0216(15) 0.0177(14) 0.0204(15) 0.0012(11) 0.0050(12) 0.0017(11) C3 0.0152(14) 0.0201(15) 0.0211(15) -0.0027(11) 0.0040(12) 0.0018(11) C4 0.0183(15) 0.0159(14) 0.0205(15) 0.0012(11) 0.0018(12) -0.0013(11) C5 0.0225(16) 0.0229(16) 0.0208(15) 0.0012(12) 0.0001(12) 0.0022(12) C6 0.0334(19) 0.0225(16) 0.0201(15) -0.0017(12) -0.0017(13) 0.0052(13) C7 0.0288(18) 0.0240(16) 0.0278(17) -0.0074(13) -0.0058(14) 0.0112(14) C8 0.0233(17) 0.0291(17) 0.0236(16) -0.0052(13) 0.0007(13) 0.0078(13) C9 0.0193(15) 0.0247(16) 0.0144(13) -0.0005(11) -0.0005(11) 0.0041(12) C10 0.0210(15) 0.0230(15) 0.0166(14) -0.0022(11) 0.0015(12) 0.0052(12) C11 0.0248(16) 0.0179(14) 0.0121(13) -0.0011(10) 0.0029(11) 0.0015(12) C12 0.0214(16) 0.0284(17) 0.0190(15) -0.0014(12) 0.0003(12) -0.0028(13) C13 0.0322(18) 0.0226(16) 0.0228(16) -0.0006(12) -0.0012(14) -0.0066(13) C14 0.0370(19) 0.0179(15) 0.0218(15) -0.0006(12) -0.0019(14) -0.0028(13) C15 0.0274(17) 0.0201(15) 0.0195(15) -0.0024(11) -0.0020(13) 0.0018(12) C16 0.0200(15) 0.0198(15) 0.0131(13) -0.0016(10) 0.0000(11) -0.0011(11) C17 0.0235(16) 0.0220(15) 0.0172(14) 0.0002(11) 0.0035(12) 0.0063(12) C18 0.0176(15) 0.0289(17) 0.0182(14) -0.0001(12) 0.0017(12) 0.0034(12) C19 0.0197(16) 0.0358(19) 0.0265(17) -0.0018(14) -0.0001(13) 0.0047(14) C20 0.0193(16) 0.041(2) 0.0293(18) -0.0054(15) 0.0020(14) -0.0034(14) C21 0.0247(18) 0.0296(18) 0.0316(18) -0.0031(14) 0.0057(14) -0.0075(14) C22 0.0239(17) 0.0235(16) 0.0248(16) 0.0005(12) 0.0038(13) -0.0009(13) C23 0.0239(16) 0.0243(16) 0.0200(15) -0.0016(12) 0.0040(13) 0.0020(12) C24 0.0290(18) 0.0268(17) 0.0265(17) 0.0002(13) 0.0079(14) 0.0081(14) C25 0.0172(16) 0.0365(19) 0.0345(18) 0.0018(15) 0.0091(14) 0.0109(14) C26 0.0187(16) 0.0327(19) 0.0324(18) -0.0022(14) 0.0041(14) 0.0023(13) C27 0.0195(15) 0.0289(17) 0.0186(14) 0.0022(12) 0.0069(12) 0.0038(12) C28 0.0176(15) 0.0283(17) 0.0236(16) -0.0013(12) 0.0059(13) -0.0003(12) C29 0.0170(14) 0.0172(14) 0.0206(14) 0.0026(11) 0.0019(12) 0.0018(11) C30 0.0212(17) 0.0217(17) 0.057(2) -0.0021(15) 0.0065(17) -0.0042(13) C31 0.031(2) 0.0201(17) 0.067(3) -0.0046(17) 0.0087(19) -0.0019(14) C32 0.0245(17) 0.0205(16) 0.040(2) -0.0030(14) 0.0015(15) 0.0053(13) C33 0.0180(15) 0.0248(16) 0.0225(15) -0.0014(12) -0.0012(12) 0.0045(12) C34 0.0167(14) 0.0180(14) 0.0151(13) 0.0015(10) 0.0006(11) 0.0005(11) C35 0.0141(14) 0.0246(16) 0.0183(14) 0.0022(11) 0.0017(11) 0.0016(11) C36 0.0175(14) 0.0188(14) 0.0160(13) -0.0005(10) -0.0003(11) -0.0014(11) C37 0.0174(15) 0.0298(17) 0.0222(15) -0.0012(12) 0.0030(12) -0.0044(12) C38 0.0248(17) 0.0238(16) 0.0275(17) 0.0005(13) 0.0049(14) -0.0102(13) C39 0.0271(17) 0.0194(15) 0.0234(16) 0.0020(12) 0.0022(13) -0.0040(12) C40 0.0221(16) 0.0185(15) 0.0207(15) -0.0004(11) 0.0031(12) 0.0012(12) C41 0.0231(17) 0.0355(18) 0.0161(14) -0.0064(12) 0.0046(12) -0.0023(13) C42 0.0271(18) 0.0369(19) 0.0227(16) -0.0080(14) -0.0004(14) -0.0038(15) C43 0.0261(19) 0.052(2) 0.0261(18) -0.0103(16) 0.0034(15) -0.0103(16) C44 0.0186(17) 0.060(3) 0.0228(17) -0.0074(16) 0.0014(14) -0.0016(16) C45 0.0234(18) 0.051(2) 0.0248(17) -0.0048(15) -0.0036(14) 0.0070(16) C46 0.0229(17) 0.045(2) 0.0175(15) -0.0048(14) 0.0013(13) 0.0025(15) C47 0.0238(17) 0.0385(19) 0.0173(15) 0.0015(13) -0.0021(13) 0.0091(14) C48 0.0277(18) 0.0288(17) 0.0255(16) 0.0050(13) -0.0021(14) 0.0064(14) C49 0.0250(17) 0.0199(15) 0.0302(17) -0.0018(12) -0.0008(14) 0.0019(12) C50 0.0227(16) 0.0214(16) 0.0281(17) 0.0011(12) -0.0008(13) -0.0056(12) C51 0.0198(15) 0.0262(16) 0.0196(15) 0.0030(12) -0.0002(12) 0.0013(12) C52 0.0222(17) 0.0268(17) 0.0322(18) 0.0049(13) -0.0027(14) -0.0052(13) C53 0.0163(15) 0.0341(18) 0.0243(16) 0.0024(13) 0.0012(13) 0.0011(13) C54 0.0240(17) 0.0348(19) 0.0310(18) 0.0062(14) -0.0021(14) 0.0039(14) C55 0.0258(17) 0.0241(16) 0.0315(18) 0.0062(13) 0.0002(14) -0.0009(13) C56 0.0205(15) 0.0239(16) 0.0147(13) 0.0012(11) 0.0013(12) -0.0005(12) C57 0.0354(19) 0.0271(17) 0.0179(15) 0.0011(12) 0.0029(14) -0.0049(14) C58 0.042(2) 0.0315(19) 0.0269(18) -0.0008(14) -0.0011(16) -0.0052(16) C59 0.043(2) 0.039(2) 0.0298(19) 0.0008(16) -0.0039(17) -0.0149(17) C60 0.033(2) 0.050(2) 0.0239(17) 0.0074(16) -0.0001(15) -0.0067(17) C61 0.037(2) 0.040(2) 0.0261(17) 0.0026(15) 0.0054(16) -0.0001(16) C62 0.0301(18) 0.0313(18) 0.0231(16) 0.0008(13) -0.0009(14) -0.0021(14) C63 0.041(2) 0.0208(16) 0.0269(17) -0.0040(13) 0.0030(15) 0.0037(14) C64 0.040(2) 0.0235(17) 0.0252(17) -0.0073(13) -0.0016(15) 0.0011(14) C65 0.042(2) 0.0231(17) 0.0213(16) -0.0021(12) -0.0001(15) -0.0058(14) C66 0.0337(19) 0.0292(18) 0.0170(15) -0.0012(12) 0.0012(13) -0.0044(14) C67 0.036(2) 0.0299(18) 0.0173(15) -0.0020(12) 0.0019(14) -0.0030(14) C68 0.036(2) 0.0338(19) 0.0225(16) -0.0013(14) 0.0011(15) -0.0025(15) C69 0.039(2) 0.042(2) 0.0209(16) 0.0045(14) 0.0051(15) 0.0043(17) C70 0.038(2) 0.0333(19) 0.0289(18) 0.0037(14) 0.0049(16) 0.0063(16) C71 0.040(2) 0.0262(18) 0.0258(17) -0.0007(13) 0.0038(15) -0.0009(15) C72 0.0334(19) 0.0275(17) 0.0150(14) 0.0006(12) 0.0034(13) -0.0004(14) C73 0.056(4) 0.116(6) 0.069(4) 0.030(4) -0.010(3) -0.012(4) C74 0.49(5) 0.22(2) 0.46(5) 0.10(3) 0.17(4) 0.22(3) C75 0.0202(18) 0.063(3) 0.033(2) -0.0045(18) -0.0002(15) 0.0023(17) C76 0.0216(18) 0.038(2) 0.037(2) 0.0042(16) -0.0021(15) 0.0025(15) C77 0.034(2) 0.055(3) 0.032(2) 0.0029(18) 0.0016(17) -0.0082(18) C78 0.036(2) 0.041(2) 0.033(2) 0.0040(16) 0.0018(17) 0.0027(17) O1 0.0291(13) 0.0255(13) 0.0424(15) 0.0049(11) 0.0072(11) 0.0118(10) O2 0.0199(12) 0.0277(13) 0.0389(14) 0.0006(10) 0.0063(10) -0.0004(10) O3 0.0181(12) 0.0313(14) 0.072(2) -0.0114(13) 0.0110(13) -0.0061(10) O4 0.0144(11) 0.0234(12) 0.0461(15) 0.0044(10) 0.0054(10) 0.0028(9) O5 0.0362(14) 0.0247(12) 0.0203(11) -0.0040(9) -0.0033(10) 0.0016(10) O6 0.0353(14) 0.0240(12) 0.0210(11) -0.0031(9) -0.0023(10) -0.0027(10) O7 0.0188(11) 0.0254(12) 0.0231(11) 0.0040(9) -0.0018(9) -0.0022(9) O8 0.0195(12) 0.0287(12) 0.0258(12) -0.0017(9) -0.0021(9) -0.0002(9) O9 0.066(2) 0.065(2) 0.050(2) 0.0156(17) 0.0007(18) 0.0065(19) O10 0.34(2) 0.258(19) 0.54(4) -0.16(2) -0.21(3) 0.005(17) O1W 0.0225(13) 0.0288(14) 0.067(2) 0.0083(13) -0.0030(13) -0.0013(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N7 1.888(3) . ? Fe1 N6 1.930(3) . ? Fe1 C2 1.980(3) . ? Fe1 C1 1.982(3) . ? Fe1 N5 2.003(3) . ? Fe1 N8 2.028(3) . ? Fe2 N11 1.903(2) . ? Fe2 N10 1.910(3) . ? Fe2 N9 1.992(3) . ? Fe2 C3 1.995(3) . ? Fe2 C4 2.002(3) . ? Fe2 N12 2.010(3) . ? Mn1 O5 1.892(3) . ? Mn1 O6 1.906(3) . ? Mn1 N16 2.016(3) . ? Mn1 N15 2.026(3) . ? Mn1 N2 2.308(3) 1_556 ? Mn1 N4 2.376(3) . ? Mn2 O8 1.883(3) . ? Mn2 O7 1.910(2) . ? Mn2 N14 2.016(3) . ? Mn2 N13 2.028(3) . ? Mn2 N1 2.311(3) . ? Mn2 N3 2.322(3) . ? N1 C1 1.154(4) . ? N2 C2 1.153(4) . ? N2 Mn1 2.308(3) 1_554 ? N3 C3 1.156(4) . ? N4 C4 1.158(4) . ? N5 C22 1.354(4) . ? N5 C18 1.375(4) . ? N6 C17 1.352(4) . ? N6 C16 1.412(4) . ? N7 C10 1.356(4) . ? N7 C11 1.430(4) . ? N8 C9 1.359(4) . ? N8 C5 1.362(4) . ? N9 C23 1.356(4) . ? N9 C27 1.364(4) . ? N10 C28 1.338(4) . ? N10 C29 1.425(4) . ? N11 C35 1.352(4) . ? N11 C34 1.424(4) . ? N12 C40 1.362(4) . ? N12 C36 1.365(4) . ? N13 C47 1.296(5) . ? N13 C48 1.481(5) . ? N14 C50 1.284(5) . ? N14 C49 1.494(4) . ? N15 C63 1.290(5) . ? N15 C64 1.487(4) . ? N16 C66 1.294(5) . ? N16 C65 1.490(5) . ? C5 C6 1.400(5) . ? C5 H5 0.9300 . ? C6 C7 1.381(5) . ? C6 H6 0.9300 . ? C7 C8 1.399(5) . ? C7 H7 0.9300 . ? C8 C9 1.396(4) . ? C8 H8 0.9300 . ? C9 C10 1.523(5) . ? C10 O2 1.232(4) . ? C11 C12 1.405(5) . ? C11 C16 1.418(4) . ? C12 C13 1.414(5) . ? C12 H12 0.9300 . ? C13 C14 1.400(5) . ? C13 H13 0.9300 . ? C14 C15 1.396(5) . ? C14 H14 0.9300 . ? C15 C16 1.423(4) . ? C15 H15 0.9300 . ? C17 O1 1.260(4) . ? C17 C18 1.510(5) . ? C18 C19 1.383(5) . ? C19 C20 1.391(5) . ? C19 H19 0.9300 . ? C20 C21 1.419(5) . ? C20 H20 0.9300 . ? C21 C22 1.397(5) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.391(5) . ? C23 H23 0.9300 . ? C24 C25 1.391(5) . ? C24 H24 0.9300 . ? C25 C26 1.415(5) . ? C25 H25 0.9300 . ? C26 C27 1.379(4) . ? C26 H26 0.9300 . ? C27 C28 1.526(5) . ? C28 O3 1.248(4) . ? C29 C34 1.408(4) . ? C29 C30 1.414(5) . ? C30 C31 1.401(5) . ? C30 H30 0.9300 . ? C31 C32 1.380(5) . ? C31 H31 0.9300 . ? C32 C33 1.405(5) . ? C32 H32 0.9300 . ? C33 C34 1.416(4) . ? C33 H33 0.9300 . ? C35 O4 1.248(4) . ? C35 C36 1.521(4) . ? C36 C37 1.390(4) . ? C37 C38 1.404(5) . ? C37 H37 0.9300 . ? C38 C39 1.395(5) . ? C38 H38 0.9300 . ? C39 C40 1.393(5) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 O8 1.324(4) . ? C41 C42 1.429(5) . ? C41 C46 1.435(5) . ? C42 C43 1.385(5) . ? C42 H42 0.9300 . ? C43 C44 1.422(6) . ? C43 H43 0.9300 . ? C44 C45 1.390(6) . ? C44 C75 1.548(5) . ? C45 C46 1.427(5) . ? C45 H45 0.9300 . ? C46 C47 1.445(6) . ? C47 H47 0.9300 . ? C48 C49 1.534(5) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.465(5) . ? C50 H50 0.9300 . ? C51 C52 1.418(5) . ? C51 C56 1.424(5) . ? C52 C53 1.395(5) . ? C52 H52 0.9300 . ? C53 C54 1.419(5) . ? C53 C76 1.538(5) . ? C54 C55 1.384(5) . ? C54 H54 0.9300 . ? C55 C56 1.431(5) . ? C55 H55 0.9300 . ? C56 O7 1.326(4) . ? C57 O6 1.333(5) . ? C57 C58 1.418(5) . ? C57 C62 1.434(5) . ? C58 C59 1.390(6) . ? C58 H58 0.9300 . ? C59 C60 1.431(6) . ? C59 H59 0.9300 . ? C60 C61 1.386(6) . ? C60 C77 1.543(6) . ? C61 C62 1.429(6) . ? C61 H61 0.9300 . ? C62 C63 1.452(5) . ? C63 H63 0.9300 . ? C64 C65 1.517(6) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 C67 1.449(5) . ? C66 H66 0.9300 . ? C67 C68 1.420(6) . ? C67 C72 1.434(5) . ? C68 C69 1.394(6) . ? C68 H68 0.9300 . ? C69 C70 1.429(6) . ? C69 C78 1.549(6) . ? C70 C71 1.388(6) . ? C70 H70 0.9300 . ? C71 C72 1.420(5) . ? C71 H71 0.9300 . ? C72 O5 1.333(5) . ? C73 O9 1.401(8) . ? C74 O10 1.29(3) . ? C75 H75A 0.9600 . ? C75 H75B 0.9600 . ? C75 H75C 0.9600 . ? 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 H78A 0.9600 . ? C78 H78B 0.9600 . ? C78 H78C 0.9600 . ? 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 N6 83.32(11) . . ? N7 Fe1 C2 93.80(12) . . ? N6 Fe1 C2 91.31(12) . . ? N7 Fe1 C1 93.55(12) . . ? N6 Fe1 C1 93.77(12) . . ? C2 Fe1 C1 171.50(13) . . ? N7 Fe1 N5 165.58(11) . . ? N6 Fe1 N5 82.27(11) . . ? C2 Fe1 N5 86.84(12) . . ? C1 Fe1 N5 87.10(12) . . ? N7 Fe1 N8 82.83(11) . . ? N6 Fe1 N8 165.80(11) . . ? C2 Fe1 N8 86.49(11) . . ? C1 Fe1 N8 90.21(11) . . ? N5 Fe1 N8 111.58(11) . . ? N11 Fe2 N10 83.56(11) . . ? N11 Fe2 N9 166.21(12) . . ? N10 Fe2 N9 82.85(11) . . ? N11 Fe2 C3 92.12(11) . . ? N10 Fe2 C3 90.66(12) . . ? N9 Fe2 C3 90.32(11) . . ? N11 Fe2 C4 92.34(12) . . ? N10 Fe2 C4 94.51(12) . . ? N9 Fe2 C4 86.46(12) . . ? C3 Fe2 C4 173.52(12) . . ? N11 Fe2 N12 83.30(11) . . ? N10 Fe2 N12 165.52(11) . . ? N9 Fe2 N12 110.46(11) . . ? C3 Fe2 N12 83.78(12) . . ? C4 Fe2 N12 92.08(11) . . ? O5 Mn1 O6 95.30(11) . . ? O5 Mn1 N16 91.76(12) . . ? O6 Mn1 N16 172.93(12) . . ? O5 Mn1 N15 172.24(12) . . ? O6 Mn1 N15 91.95(12) . . ? N16 Mn1 N15 81.00(13) . . ? O5 Mn1 N2 89.68(11) . 1_556 ? O6 Mn1 N2 94.46(11) . 1_556 ? N16 Mn1 N2 85.63(11) . 1_556 ? N15 Mn1 N2 87.01(11) . 1_556 ? O5 Mn1 N4 92.79(10) . . ? O6 Mn1 N4 85.61(11) . . ? N16 Mn1 N4 94.00(11) . . ? N15 Mn1 N4 90.51(11) . . ? N2 Mn1 N4 177.51(11) 1_556 . ? O8 Mn2 O7 94.70(10) . . ? O8 Mn2 N14 172.99(11) . . ? O7 Mn2 N14 92.00(11) . . ? O8 Mn2 N13 92.19(11) . . ? O7 Mn2 N13 173.11(11) . . ? N14 Mn2 N13 81.10(11) . . ? O8 Mn2 N1 92.40(11) . . ? O7 Mn2 N1 91.68(10) . . ? N14 Mn2 N1 85.35(11) . . ? N13 Mn2 N1 87.69(11) . . ? O8 Mn2 N3 92.84(11) . . ? O7 Mn2 N3 93.31(10) . . ? N14 Mn2 N3 88.80(11) . . ? N13 Mn2 N3 86.67(10) . . ? N1 Mn2 N3 172.44(11) . . ? C1 N1 Mn2 148.0(3) . . ? C2 N2 Mn1 148.8(3) . 1_554 ? C3 N3 Mn2 147.5(2) . . ? C4 N4 Mn1 160.9(3) . . ? C22 N5 C18 119.1(3) . . ? C22 N5 Fe1 129.2(2) . . ? C18 N5 Fe1 111.7(2) . . ? C17 N6 C16 125.5(3) . . ? C17 N6 Fe1 119.0(2) . . ? C16 N6 Fe1 115.3(2) . . ? C10 N7 C11 125.8(3) . . ? C10 N7 Fe1 119.2(2) . . ? C11 N7 Fe1 115.0(2) . . ? C9 N8 C5 117.1(3) . . ? C9 N8 Fe1 111.4(2) . . ? C5 N8 Fe1 131.2(2) . . ? C23 N9 C27 118.7(3) . . ? C23 N9 Fe2 129.5(2) . . ? C27 N9 Fe2 111.8(2) . . ? C28 N10 C29 126.2(3) . . ? C28 N10 Fe2 118.7(2) . . ? C29 N10 Fe2 114.7(2) . . ? C35 N11 C34 127.0(3) . . ? C35 N11 Fe2 118.1(2) . . ? C34 N11 Fe2 114.9(2) . . ? C40 N12 C36 117.8(3) . . ? C40 N12 Fe2 130.3(2) . . ? C36 N12 Fe2 111.1(2) . . ? C47 N13 C48 121.0(3) . . ? C47 N13 Mn2 124.9(3) . . ? C48 N13 Mn2 114.1(2) . . ? C50 N14 C49 121.1(3) . . ? C50 N14 Mn2 125.3(2) . . ? C49 N14 Mn2 113.6(2) . . ? C63 N15 C64 120.2(3) . . ? C63 N15 Mn1 126.2(2) . . ? C64 N15 Mn1 113.3(2) . . ? C66 N16 C65 120.0(3) . . ? C66 N16 Mn1 125.0(2) . . ? C65 N16 Mn1 114.9(2) . . ? N1 C1 Fe1 175.7(3) . . ? N2 C2 Fe1 175.6(3) . . ? N3 C3 Fe2 171.4(3) . . ? N4 C4 Fe2 177.0(3) . . ? N8 C5 C6 123.6(3) . . ? N8 C5 H5 118.2 . . ? C6 C5 H5 118.2 . . ? C7 C6 C5 118.8(3) . . ? C7 C6 H6 120.6 . . ? C5 C6 H6 120.6 . . ? C6 C7 C8 118.4(3) . . ? C6 C7 H7 120.8 . . ? C8 C7 H7 120.8 . . ? C9 C8 C7 120.1(3) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? N8 C9 C8 122.0(3) . . ? N8 C9 C10 115.6(3) . . ? C8 C9 C10 122.3(3) . . ? O2 C10 N7 127.9(3) . . ? O2 C10 C9 121.5(3) . . ? N7 C10 C9 110.6(3) . . ? C12 C11 C16 119.4(3) . . ? C12 C11 N7 126.6(3) . . ? C16 C11 N7 114.0(3) . . ? C11 C12 C13 119.6(3) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C14 C13 C12 120.9(3) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C15 C14 C13 120.3(3) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 119.4(3) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? N6 C16 C11 112.4(3) . . ? N6 C16 C15 127.2(3) . . ? C11 C16 C15 120.5(3) . . ? O1 C17 N6 127.6(3) . . ? O1 C17 C18 122.5(3) . . ? N6 C17 C18 109.9(3) . . ? N5 C18 C19 122.0(3) . . ? N5 C18 C17 116.7(3) . . ? C19 C18 C17 121.4(3) . . ? C18 C19 C20 119.0(3) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C19 C20 C21 119.7(3) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C22 C21 C20 118.1(3) . . ? C22 C21 H21 121.0 . . ? C20 C21 H21 121.0 . . ? N5 C22 C21 122.1(3) . . ? N5 C22 H22 119.0 . . ? C21 C22 H22 119.0 . . ? N9 C23 C24 122.8(3) . . ? N9 C23 H23 118.6 . . ? C24 C23 H23 118.6 . . ? C23 C24 C25 118.2(3) . . ? C23 C24 H24 120.9 . . ? C25 C24 H24 120.9 . . ? C24 C25 C26 119.4(3) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C27 C26 C25 119.0(3) . . ? C27 C26 H26 120.5 . . ? C25 C26 H26 120.5 . . ? N9 C27 C26 121.8(3) . . ? N9 C27 C28 115.7(3) . . ? C26 C27 C28 122.4(3) . . ? O3 C28 N10 127.9(3) . . ? O3 C28 C27 121.8(3) . . ? N10 C28 C27 110.3(3) . . ? C34 C29 C30 119.8(3) . . ? C34 C29 N10 113.3(3) . . ? C30 C29 N10 126.9(3) . . ? C31 C30 C29 119.4(3) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C32 C31 C30 121.1(4) . . ? C32 C31 H31 119.4 . . ? C30 C31 H31 119.4 . . ? C31 C32 C33 120.3(3) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C32 C33 C34 119.6(3) . . ? C32 C33 H33 120.2 . . ? C34 C33 H33 120.2 . . ? C29 C34 C33 119.7(3) . . ? C29 C34 N11 113.5(3) . . ? C33 C34 N11 126.7(3) . . ? O4 C35 N11 127.5(3) . . ? O4 C35 C36 121.8(3) . . ? N11 C35 C36 110.6(3) . . ? N12 C36 C37 121.9(3) . . ? N12 C36 C35 116.1(3) . . ? C37 C36 C35 121.7(3) . . ? C36 C37 C38 119.5(3) . . ? C36 C37 H37 120.2 . . ? C38 C37 H37 120.2 . . ? C39 C38 C37 119.1(3) . . ? C39 C38 H38 120.5 . . ? C37 C38 H38 120.5 . . ? C40 C39 C38 118.2(3) . . ? C40 C39 H39 120.9 . . ? C38 C39 H39 120.9 . . ? N12 C40 C39 123.4(3) . . ? N12 C40 H40 118.3 . . ? C39 C40 H40 118.3 . . ? O8 C41 C42 117.6(3) . . ? O8 C41 C46 123.8(3) . . ? C42 C41 C46 118.6(3) . . ? C43 C42 C41 119.7(4) . . ? C43 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C42 C43 C44 122.7(4) . . ? C42 C43 H43 118.7 . . ? C44 C43 H43 118.7 . . ? C45 C44 C43 118.1(3) . . ? C45 C44 C75 121.4(4) . . ? C43 C44 C75 120.6(4) . . ? C44 C45 C46 121.4(4) . . ? C44 C45 H45 119.3 . . ? C46 C45 H45 119.3 . . ? C45 C46 C41 119.6(4) . . ? C45 C46 C47 116.8(4) . . ? C41 C46 C47 123.6(3) . . ? N13 C47 C46 124.8(3) . . ? N13 C47 H47 117.6 . . ? C46 C47 H47 117.6 . . ? N13 C48 C49 106.9(3) . . ? N13 C48 H48A 110.3 . . ? C49 C48 H48A 110.3 . . ? N13 C48 H48B 110.3 . . ? C49 C48 H48B 110.3 . . ? H48A C48 H48B 108.6 . . ? N14 C49 C48 107.0(3) . . ? N14 C49 H49A 110.3 . . ? C48 C49 H49A 110.3 . . ? N14 C49 H49B 110.3 . . ? C48 C49 H49B 110.3 . . ? H49A C49 H49B 108.6 . . ? N14 C50 C51 124.6(3) . . ? N14 C50 H50 117.7 . . ? C51 C50 H50 117.7 . . ? C52 C51 C56 119.3(3) . . ? C52 C51 C50 117.0(3) . . ? C56 C51 C50 123.6(3) . . ? C53 C52 C51 122.3(3) . . ? C53 C52 H52 118.8 . . ? C51 C52 H52 118.8 . . ? C52 C53 C54 117.6(3) . . ? C52 C53 C76 121.8(3) . . ? C54 C53 C76 120.6(3) . . ? C55 C54 C53 121.9(3) . . ? C55 C54 H54 119.1 . . ? C53 C54 H54 119.1 . . ? C54 C55 C56 120.6(3) . . ? C54 C55 H55 119.7 . . ? C56 C55 H55 119.7 . . ? O7 C56 C51 123.8(3) . . ? O7 C56 C55 117.9(3) . . ? C51 C56 C55 118.3(3) . . ? O6 C57 C58 117.5(3) . . ? O6 C57 C62 124.7(3) . . ? C58 C57 C62 117.8(4) . . ? C59 C58 C57 121.0(4) . . ? C59 C58 H58 119.5 . . ? C57 C58 H58 119.5 . . ? C58 C59 C60 121.9(4) . . ? C58 C59 H59 119.0 . . ? C60 C59 H59 119.0 . . ? C61 C60 C59 117.4(4) . . ? C61 C60 C77 121.6(4) . . ? C59 C60 C77 121.0(4) . . ? C60 C61 C62 122.1(4) . . ? C60 C61 H61 119.0 . . ? C62 C61 H61 119.0 . . ? C61 C62 C57 119.7(3) . . ? C61 C62 C63 117.0(3) . . ? C57 C62 C63 123.1(3) . . ? N15 C63 C62 124.7(3) . . ? N15 C63 H63 117.6 . . ? C62 C63 H63 117.6 . . ? N15 C64 C65 107.7(3) . . ? N15 C64 H64A 110.2 . . ? C65 C64 H64A 110.2 . . ? N15 C64 H64B 110.2 . . ? C65 C64 H64B 110.2 . . ? H64A C64 H64B 108.5 . . ? N16 C65 C64 107.7(3) . . ? N16 C65 H65A 110.2 . . ? C64 C65 H65A 110.2 . . ? N16 C65 H65B 110.2 . . ? C64 C65 H65B 110.2 . . ? H65A C65 H65B 108.5 . . ? N16 C66 C67 126.2(3) . . ? N16 C66 H66 116.9 . . ? C67 C66 H66 116.9 . . ? C68 C67 C72 119.0(3) . . ? C68 C67 C66 118.0(3) . . ? C72 C67 C66 123.0(3) . . ? C69 C68 C67 122.6(4) . . ? C69 C68 H68 118.7 . . ? C67 C68 H68 118.7 . . ? C68 C69 C70 117.5(4) . . ? C68 C69 C78 121.9(4) . . ? C70 C69 C78 120.6(4) . . ? C71 C70 C69 121.3(4) . . ? C71 C70 H70 119.3 . . ? C69 C70 H70 119.3 . . ? C70 C71 C72 121.3(4) . . ? C70 C71 H71 119.3 . . ? C72 C71 H71 119.3 . . ? O5 C72 C71 119.0(3) . . ? O5 C72 C67 122.8(3) . . ? C71 C72 C67 118.2(3) . . ? C44 C75 H75A 109.5 . . ? C44 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C44 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C53 C76 H76A 109.5 . . ? C53 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C53 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C60 C77 H77A 109.5 . . ? C60 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C60 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C69 C78 H78A 109.5 . . ? C69 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C69 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C72 O5 Mn1 130.0(2) . . ? C57 O6 Mn1 127.7(2) . . ? C56 O7 Mn2 127.5(2) . . ? C41 O8 Mn2 128.2(2) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.928 _refine_diff_density_min -0.993 _refine_diff_density_rms 0.160 #===End