# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Chang Seop Hong' _publ_contact_author_email CSHONG@KOREA.AC.KR _publ_section_title ; Syntheses, crystal structures, and magnetic properties of cyano- and phenoxide-bridged Fe(III)-Mn(III) tetramers containing fac-Fe(III) tricyanides and Mn(III) Schiff bases ; loop_ _publ_author_name 'Chang Seop Hong' 'Beong Ki Cho' 'Hyoung Chan Kim' 'Eui Kwan Koh' 'Hyun Young Kwak' 'Dae Won Ryu' # Attachment 'complex1.cif' data_complex1 _database_code_depnum_ccdc_archive 'CCDC 705439' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H56 B2 Fe2 Mn2 N22 O4' _chemical_formula_weight 1392.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' B B 0.0013 0.0007 '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 11.2458(6) _cell_length_b 12.0481(7) _cell_length_c 13.3851(7) _cell_angle_alpha 89.382(2) _cell_angle_beta 74.959(2) _cell_angle_gamma 62.685(2) _cell_volume 1543.69(15) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2857 _cell_measurement_theta_min 2.3305 _cell_measurement_theta_max 24.719 _exptl_crystal_description Plate _exptl_crystal_colour red _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 714 _exptl_absorpt_coefficient_mu 0.928 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7767 _exptl_absorpt_correction_T_max 0.9691 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25478 _diffrn_reflns_av_R_equivalents 0.1356 _diffrn_reflns_av_sigmaI/netI 0.1621 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 28.32 _reflns_number_total 7535 _reflns_number_gt 3565 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART APEX II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SHELXTL _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics WingX _computing_publication_material WingX _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^)+(0.0590P)^2^+1.8268P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7535 _refine_ls_number_parameters 421 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1754 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1686 _refine_ls_wR_factor_gt 0.1222 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _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 0.27789(7) 0.34803(7) 0.14930(6) 0.0215(2) Uani 1 1 d . . . C1 C 0.3764(5) 0.2239(5) 0.2267(4) 0.0235(12) Uani 1 1 d . . . N1 N 0.4395(5) 0.1468(4) 0.2714(3) 0.0285(11) Uani 1 1 d . . . C2 C 0.1034(6) 0.3686(5) 0.2428(4) 0.0279(12) Uani 1 1 d . . . N2 N -0.0039(5) 0.3869(5) 0.2963(4) 0.0382(12) Uani 1 1 d . . . C3 C 0.2736(6) 0.4694(5) 0.2449(4) 0.0289(13) Uani 1 1 d . . . N3 N 0.2764(5) 0.5397(5) 0.3010(4) 0.0412(13) Uani 1 1 d . . . N4 N 0.4526(4) 0.3347(4) 0.0560(3) 0.0241(10) Uani 1 1 d . . . N5 N 0.4697(4) 0.3341(4) -0.0490(3) 0.0258(10) Uani 1 1 d . . . C4 C 0.5650(5) 0.3343(5) 0.0717(5) 0.0281(13) Uani 1 1 d . . . H4 H 0.5812 0.3335 0.1364 0.034 Uiso 1 1 calc R . . C5 C 0.6544(6) 0.3351(5) -0.0210(5) 0.0345(14) Uani 1 1 d . . . H5 H 0.7394 0.3350 -0.0309 0.041 Uiso 1 1 calc R . . C6 C 0.5898(5) 0.3362(5) -0.0952(5) 0.0314(13) Uani 1 1 d . . . H6 H 0.6237 0.3380 -0.1661 0.038 Uiso 1 1 calc R . . N6 N 0.1739(4) 0.4768(4) 0.0676(3) 0.0223(10) Uani 1 1 d . . . N7 N 0.2199(4) 0.4558(4) -0.0383(3) 0.0243(10) Uani 1 1 d . . . C7 C 0.0579(5) 0.5867(5) 0.0934(4) 0.0259(12) Uani 1 1 d . . . H7 H 0.0048 0.6230 0.1615 0.031 Uiso 1 1 calc R . . C8 C 0.0266(6) 0.6401(5) 0.0050(5) 0.0305(13) Uani 1 1 d . . . H8 H -0.0475 0.7170 0.0018 0.037 Uiso 1 1 calc R . . C9 C 0.1301(6) 0.5534(5) -0.0764(5) 0.0291(13) Uani 1 1 d . . . H9 H 0.1372 0.5606 -0.1467 0.035 Uiso 1 1 calc R . . N8 N 0.2958(4) 0.2171(4) 0.0517(3) 0.0240(10) Uani 1 1 d . . . N9 N 0.3339(4) 0.2215(4) -0.0534(3) 0.0249(10) Uani 1 1 d . . . C10 C 0.2921(5) 0.1073(5) 0.0631(5) 0.0280(12) Uani 1 1 d . . . H10 H 0.2691 0.0792 0.1267 0.034 Uiso 1 1 calc R . . C11 C 0.3274(6) 0.0423(5) -0.0336(5) 0.0359(14) Uani 1 1 d . . . H11 H 0.3327 -0.0357 -0.0472 0.043 Uiso 1 1 calc R . . C12 C 0.3531(5) 0.1168(5) -0.1056(5) 0.0300(13) Uani 1 1 d . . . H12 H 0.3791 0.0982 -0.1777 0.036 Uiso 1 1 calc R . . B1 B 0.3531(6) 0.3352(6) -0.0907(5) 0.0257(14) Uani 1 1 d . . . H1 H 0.384(6) 0.329(5) -0.168(4) 0.037(16) Uiso 1 1 d . . . Mn1 Mn 0.50324(8) 0.09212(7) 0.41281(6) 0.0215(2) Uani 1 1 d . . . O1 O 0.4508(3) -0.0380(3) 0.4292(3) 0.0236(8) Uani 1 1 d . . . O2 O 0.6906(3) -0.0148(3) 0.3443(3) 0.0234(8) Uani 1 1 d . . . C21 C 0.3172(6) 0.3098(5) 0.5590(4) 0.0334(14) Uani 1 1 d . . . H21A H 0.3466 0.2761 0.6196 0.040 Uiso 1 1 calc R . . H21B H 0.2254 0.3826 0.5829 0.040 Uiso 1 1 calc R . . C22 C 0.4195(6) 0.3474(5) 0.4922(5) 0.0364(14) Uani 1 1 d . . . H22A H 0.3731 0.4119 0.4514 0.044 Uiso 1 1 calc R . . H22B H 0.4534 0.3823 0.5364 0.044 Uiso 1 1 calc R . . C13 C 0.3284(6) -0.0182(5) 0.4132(4) 0.0282(12) Uani 1 1 d . . . C14 C 0.3253(6) -0.1186(6) 0.3673(5) 0.0394(15) Uani 1 1 d . . . H14 H 0.4057 -0.1962 0.3491 0.047 Uiso 1 1 calc R . . C15 C 0.2047(7) -0.1062(7) 0.3477(5) 0.0509(19) Uani 1 1 d . . . H15 H 0.2043 -0.1750 0.3173 0.061 Uiso 1 1 calc R . . C16 C 0.0865(7) 0.0082(7) 0.3735(5) 0.0445(17) Uani 1 1 d . . . H16 H 0.0062 0.0178 0.3586 0.053 Uiso 1 1 calc R . . C17 C 0.0862(6) 0.1086(6) 0.4213(5) 0.0371(14) Uani 1 1 d . . . H17 H 0.0046 0.1852 0.4397 0.045 Uiso 1 1 calc R . . C18 C 0.2067(5) 0.0987(5) 0.4434(4) 0.0290(13) Uani 1 1 d . . . C19 C 0.1989(5) 0.2055(5) 0.5011(4) 0.0270(12) Uani 1 1 d . . . C20 C 0.0562(6) 0.3046(6) 0.5649(5) 0.0501(18) Uani 1 1 d . . . H20A H 0.0663 0.3540 0.6147 0.075 Uiso 1 1 calc R . . H20B H 0.0038 0.2646 0.6009 0.075 Uiso 1 1 calc R . . H20C H 0.0078 0.3584 0.5196 0.075 Uiso 1 1 calc R . . N10 N 0.3112(5) 0.2131(4) 0.4961(3) 0.0249(10) Uani 1 1 d . . . N11 N 0.5393(5) 0.2368(4) 0.4212(4) 0.0284(10) Uani 1 1 d . . . C23 C 0.6458(6) 0.2462(6) 0.3635(5) 0.0403(16) Uani 1 1 d . . . C24 C 0.6562(9) 0.3655(7) 0.3793(8) 0.102(4) Uani 1 1 d . . . H24A H 0.5926 0.4312 0.3494 0.152 Uiso 1 1 calc R . . H24B H 0.7498 0.3501 0.3461 0.152 Uiso 1 1 calc R . . H24C H 0.6326 0.3906 0.4526 0.152 Uiso 1 1 calc R . . C25 C 0.7602(6) 0.1430(5) 0.2865(4) 0.0301(13) Uani 1 1 d . . . C26 C 0.8585(6) 0.1668(6) 0.2121(5) 0.0412(16) Uani 1 1 d . . . H26 H 0.8474 0.2482 0.2126 0.049 Uiso 1 1 calc R . . C27 C 0.9702(6) 0.0726(6) 0.1389(5) 0.0406(15) Uani 1 1 d . . . H27 H 1.0327 0.0907 0.0904 0.049 Uiso 1 1 calc R . . C28 C 0.9883(6) -0.0483(6) 0.1381(5) 0.0360(14) Uani 1 1 d . . . H28 H 1.0646 -0.1126 0.0900 0.043 Uiso 1 1 calc R . . C29 C 0.8935(5) -0.0744(5) 0.2087(4) 0.0290(13) Uani 1 1 d . . . H29 H 0.9076 -0.1568 0.2076 0.035 Uiso 1 1 calc R . . C30 C 0.7771(5) 0.0194(5) 0.2814(4) 0.0228(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0172(4) 0.0249(4) 0.0222(4) 0.0075(3) -0.0055(3) -0.0099(3) C1 0.024(3) 0.022(3) 0.022(3) -0.001(2) -0.002(2) -0.011(2) N1 0.031(3) 0.029(3) 0.023(2) 0.010(2) -0.009(2) -0.011(2) C2 0.030(3) 0.028(3) 0.023(3) 0.010(2) -0.008(3) -0.012(3) N2 0.034(3) 0.046(3) 0.033(3) 0.015(2) -0.005(2) -0.019(3) C3 0.029(3) 0.025(3) 0.029(3) 0.009(3) -0.005(3) -0.012(3) N3 0.041(3) 0.037(3) 0.037(3) 0.002(2) 0.001(2) -0.017(3) N4 0.021(2) 0.027(2) 0.024(2) 0.010(2) -0.0085(19) -0.010(2) N5 0.023(2) 0.033(3) 0.025(2) 0.005(2) -0.0052(19) -0.017(2) C4 0.022(3) 0.029(3) 0.037(3) 0.004(3) -0.012(3) -0.012(2) C5 0.019(3) 0.036(3) 0.054(4) 0.005(3) -0.012(3) -0.017(3) C6 0.020(3) 0.032(3) 0.037(3) 0.001(3) 0.003(2) -0.014(3) N6 0.016(2) 0.026(2) 0.023(2) 0.0062(19) -0.0033(18) -0.010(2) N7 0.022(2) 0.030(2) 0.025(2) 0.011(2) -0.009(2) -0.014(2) C7 0.015(3) 0.025(3) 0.035(3) 0.007(2) -0.004(2) -0.009(2) C8 0.023(3) 0.026(3) 0.050(4) 0.016(3) -0.018(3) -0.014(3) C9 0.031(3) 0.040(3) 0.034(3) 0.023(3) -0.021(3) -0.025(3) N8 0.020(2) 0.030(2) 0.023(2) 0.007(2) -0.0079(19) -0.011(2) N9 0.026(2) 0.032(3) 0.021(2) 0.006(2) -0.0081(19) -0.017(2) C10 0.022(3) 0.029(3) 0.039(3) 0.013(3) -0.015(3) -0.015(2) C11 0.034(3) 0.031(3) 0.050(4) 0.000(3) -0.014(3) -0.020(3) C12 0.023(3) 0.037(3) 0.031(3) 0.001(3) -0.008(2) -0.014(3) B1 0.023(3) 0.036(4) 0.024(3) 0.009(3) -0.007(3) -0.019(3) Mn1 0.0209(4) 0.0230(4) 0.0212(4) 0.0057(3) -0.0065(3) -0.0105(4) O1 0.0208(19) 0.033(2) 0.024(2) 0.0090(16) -0.0092(15) -0.0162(17) O2 0.0223(19) 0.0235(19) 0.0221(19) 0.0068(15) -0.0030(15) -0.0107(16) C21 0.033(3) 0.031(3) 0.030(3) -0.002(3) -0.005(3) -0.012(3) C22 0.035(3) 0.027(3) 0.041(4) -0.006(3) -0.002(3) -0.014(3) C13 0.027(3) 0.040(3) 0.020(3) 0.005(2) -0.006(2) -0.018(3) C14 0.030(3) 0.046(4) 0.043(4) -0.007(3) -0.009(3) -0.019(3) C15 0.034(4) 0.077(5) 0.050(4) -0.012(4) -0.011(3) -0.034(4) C16 0.028(4) 0.074(5) 0.038(4) 0.004(3) -0.014(3) -0.028(4) C17 0.029(3) 0.051(4) 0.032(3) 0.012(3) -0.010(3) -0.019(3) C18 0.022(3) 0.039(3) 0.030(3) 0.010(3) -0.008(2) -0.017(3) C19 0.021(3) 0.029(3) 0.025(3) 0.010(2) -0.006(2) -0.008(2) C20 0.028(3) 0.055(4) 0.055(4) 0.001(3) 0.001(3) -0.016(3) N10 0.029(3) 0.023(2) 0.024(2) 0.0077(19) -0.010(2) -0.012(2) N11 0.026(2) 0.027(2) 0.032(3) 0.004(2) -0.004(2) -0.014(2) C23 0.037(4) 0.032(3) 0.052(4) -0.001(3) -0.003(3) -0.022(3) C24 0.086(7) 0.044(5) 0.147(9) -0.034(5) 0.043(6) -0.046(5) C25 0.024(3) 0.034(3) 0.038(3) 0.004(3) -0.008(3) -0.018(3) C26 0.031(3) 0.038(4) 0.056(4) 0.014(3) -0.007(3) -0.021(3) C27 0.034(3) 0.051(4) 0.043(4) 0.015(3) -0.003(3) -0.030(3) C28 0.026(3) 0.045(4) 0.036(4) 0.004(3) -0.004(3) -0.018(3) C29 0.025(3) 0.032(3) 0.029(3) 0.002(2) -0.005(2) -0.014(3) C30 0.018(3) 0.028(3) 0.025(3) 0.009(2) -0.012(2) -0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C1 1.892(6) . ? Fe1 C3 1.930(6) . ? Fe1 C2 1.940(6) . ? Fe1 N8 1.962(4) . ? Fe1 N4 1.972(4) . ? Fe1 N6 1.983(4) . ? C1 N1 1.152(6) . ? N1 Mn1 2.185(5) . ? C2 N2 1.153(6) . ? C3 N3 1.154(7) . ? N4 C4 1.332(6) . ? N4 N5 1.367(6) . ? N5 C6 1.343(6) . ? N5 B1 1.548(7) . ? C4 C5 1.383(8) . ? C4 H4 0.9300 . ? C5 C6 1.371(8) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? N6 C7 1.328(6) . ? N6 N7 1.360(6) . ? N7 C9 1.351(6) . ? N7 B1 1.526(7) . ? C7 C8 1.388(8) . ? C7 H7 0.9300 . ? C8 C9 1.373(8) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? N8 C10 1.349(6) . ? N8 N9 1.369(6) . ? N9 C12 1.348(7) . ? N9 B1 1.540(7) . ? C10 C11 1.384(8) . ? C10 H10 0.9300 . ? C11 C12 1.376(8) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? B1 H1 1.00(5) . ? Mn1 O2 1.863(3) . ? Mn1 O1 1.904(3) . ? Mn1 N11 1.973(4) . ? Mn1 N10 1.982(4) . ? Mn1 O1 2.322(3) 2_656 ? Mn1 Mn1 3.2138(15) 2_656 ? O1 C13 1.360(6) . ? O1 Mn1 2.322(3) 2_656 ? O2 C30 1.327(6) . ? C21 N10 1.480(7) . ? C21 C22 1.506(8) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 N11 1.486(7) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C13 C14 1.381(8) . ? C13 C18 1.405(7) . ? C14 C15 1.388(8) . ? C14 H14 0.9300 . ? C15 C16 1.370(9) . ? C15 H15 0.9300 . ? C16 C17 1.374(8) . ? C16 H16 0.9300 . ? C17 C18 1.413(7) . ? C17 H17 0.9300 . ? C18 C19 1.464(8) . ? C19 N10 1.293(6) . ? C19 C20 1.511(8) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? N11 C23 1.299(7) . ? C23 C25 1.461(8) . ? C23 C24 1.515(8) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C30 1.412(7) . ? C25 C26 1.417(8) . ? C26 C27 1.379(8) . ? C26 H26 0.9300 . ? C27 C28 1.374(8) . ? C27 H27 0.9300 . ? C28 C29 1.382(7) . ? C28 H28 0.9300 . ? C29 C30 1.394(7) . ? C29 H29 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe1 C3 86.6(2) . . ? C1 Fe1 C2 89.4(2) . . ? C3 Fe1 C2 88.6(2) . . ? C1 Fe1 N8 90.45(19) . . ? C3 Fe1 N8 176.0(2) . . ? C2 Fe1 N8 94.1(2) . . ? C1 Fe1 N4 91.8(2) . . ? C3 Fe1 N4 89.4(2) . . ? C2 Fe1 N4 177.6(2) . . ? N8 Fe1 N4 88.01(17) . . ? C1 Fe1 N6 179.3(2) . . ? C3 Fe1 N6 94.0(2) . . ? C2 Fe1 N6 90.35(19) . . ? N8 Fe1 N6 88.95(17) . . ? N4 Fe1 N6 88.44(17) . . ? N1 C1 Fe1 178.1(5) . . ? C1 N1 Mn1 149.5(4) . . ? N2 C2 Fe1 176.3(5) . . ? N3 C3 Fe1 177.5(5) . . ? C4 N4 N5 106.1(4) . . ? C4 N4 Fe1 133.9(4) . . ? N5 N4 Fe1 119.7(3) . . ? C6 N5 N4 109.2(4) . . ? C6 N5 B1 133.0(5) . . ? N4 N5 B1 117.8(4) . . ? N4 C4 C5 111.1(5) . . ? N4 C4 H4 124.5 . . ? C5 C4 H4 124.5 . . ? C6 C5 C4 104.6(5) . . ? C6 C5 H5 127.7 . . ? C4 C5 H5 127.7 . . ? N5 C6 C5 109.0(5) . . ? N5 C6 H6 125.5 . . ? C5 C6 H6 125.5 . . ? C7 N6 N7 107.0(4) . . ? C7 N6 Fe1 133.7(4) . . ? N7 N6 Fe1 119.3(3) . . ? C9 N7 N6 108.6(4) . . ? C9 N7 B1 132.7(5) . . ? N6 N7 B1 118.7(4) . . ? N6 C7 C8 110.9(5) . . ? N6 C7 H7 124.5 . . ? C8 C7 H7 124.5 . . ? C9 C8 C7 104.3(5) . . ? C9 C8 H8 127.9 . . ? C7 C8 H8 127.9 . . ? N7 C9 C8 109.2(5) . . ? N7 C9 H9 125.4 . . ? C8 C9 H9 125.4 . . ? C10 N8 N9 106.1(4) . . ? C10 N8 Fe1 133.7(4) . . ? N9 N8 Fe1 119.9(3) . . ? C12 N9 N8 109.9(4) . . ? C12 N9 B1 132.1(5) . . ? N8 N9 B1 118.0(4) . . ? N8 C10 C11 110.2(5) . . ? N8 C10 H10 124.9 . . ? C11 C10 H10 124.9 . . ? C12 C11 C10 105.8(5) . . ? C12 C11 H11 127.1 . . ? C10 C11 H11 127.1 . . ? N9 C12 C11 108.1(5) . . ? N9 C12 H12 126.0 . . ? C11 C12 H12 126.0 . . ? N7 B1 N9 108.7(4) . . ? N7 B1 N5 106.7(4) . . ? N9 B1 N5 106.5(4) . . ? N7 B1 H1 114(3) . . ? N9 B1 H1 112(3) . . ? N5 B1 H1 108(3) . . ? O2 Mn1 O1 95.14(15) . . ? O2 Mn1 N11 91.59(17) . . ? O1 Mn1 N11 170.20(17) . . ? O2 Mn1 N10 173.76(17) . . ? O1 Mn1 N10 88.75(16) . . ? N11 Mn1 N10 83.96(18) . . ? O2 Mn1 N1 95.72(16) . . ? O1 Mn1 N1 95.59(16) . . ? N11 Mn1 N1 90.79(18) . . ? N10 Mn1 N1 88.73(17) . . ? O2 Mn1 O1 89.17(14) . 2_656 ? O1 Mn1 O1 81.48(14) . 2_656 ? N11 Mn1 O1 91.53(16) . 2_656 ? N10 Mn1 O1 86.59(15) . 2_656 ? N1 Mn1 O1 174.52(15) . 2_656 ? O2 Mn1 Mn1 92.44(11) . 2_656 ? O1 Mn1 Mn1 45.62(10) . 2_656 ? N11 Mn1 Mn1 127.09(14) . 2_656 ? N10 Mn1 Mn1 86.80(12) . 2_656 ? N1 Mn1 Mn1 140.99(13) . 2_656 ? O1 Mn1 Mn1 35.87(8) 2_656 2_656 ? C13 O1 Mn1 119.5(3) . . ? C13 O1 Mn1 121.0(3) . 2_656 ? Mn1 O1 Mn1 98.52(14) . 2_656 ? C30 O2 Mn1 125.3(3) . . ? N10 C21 C22 108.6(4) . . ? N10 C21 H21A 110.0 . . ? C22 C21 H21A 110.0 . . ? N10 C21 H21B 110.0 . . ? C22 C21 H21B 110.0 . . ? H21A C21 H21B 108.3 . . ? N11 C22 C21 110.5(4) . . ? N11 C22 H22A 109.6 . . ? C21 C22 H22A 109.6 . . ? N11 C22 H22B 109.6 . . ? C21 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? O1 C13 C14 117.7(5) . . ? O1 C13 C18 122.4(5) . . ? C14 C13 C18 119.9(5) . . ? C13 C14 C15 121.3(6) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C16 C15 C14 119.5(6) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 C16 C17 120.1(6) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C18 121.8(6) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C13 C18 C17 117.3(5) . . ? C13 C18 C19 122.8(5) . . ? C17 C18 C19 119.8(5) . . ? N10 C19 C18 120.2(5) . . ? N10 C19 C20 122.2(5) . . ? C18 C19 C20 117.6(5) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 N10 C21 124.7(5) . . ? C19 N10 Mn1 126.1(4) . . ? C21 N10 Mn1 109.0(3) . . ? C23 N11 C22 120.4(5) . . ? C23 N11 Mn1 126.3(4) . . ? C22 N11 Mn1 112.8(3) . . ? N11 C23 C25 122.1(5) . . ? N11 C23 C24 119.4(6) . . ? C25 C23 C24 118.4(5) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C30 C25 C26 117.7(5) . . ? C30 C25 C23 123.0(5) . . ? C26 C25 C23 119.3(5) . . ? C27 C26 C25 121.9(6) . . ? C27 C26 H26 119.1 . . ? C25 C26 H26 119.1 . . ? C28 C27 C26 119.5(5) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C27 C28 C29 120.1(5) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C28 C29 C30 121.7(5) . . ? C28 C29 H29 119.1 . . ? C30 C29 H29 119.1 . . ? O2 C30 C29 117.1(5) . . ? O2 C30 C25 124.0(5) . . ? C29 C30 C25 118.9(5) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.220 _refine_diff_density_min -0.804 _refine_diff_density_rms 0.116 # Attachment 'complex2.cif' data_complex2 _database_code_depnum_ccdc_archive 'CCDC 705440' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H52 B2 Br4 Fe2 Mn2 N22 O4' _chemical_formula_weight 1708.08 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' B B 0.0013 0.0007 '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' 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 8.5984(3) _cell_length_b 14.1782(5) _cell_length_c 15.9157(6) _cell_angle_alpha 67.8170(10) _cell_angle_beta 86.145(2) _cell_angle_gamma 73.8680(10) _cell_volume 1724.37(11) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1301 _cell_measurement_theta_min 2.468 _cell_measurement_theta_max 23.8785 _exptl_crystal_description Plate _exptl_crystal_colour red _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.645 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 850 _exptl_absorpt_coefficient_mu 3.150 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6758 _exptl_absorpt_correction_T_max 0.9282 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23860 _diffrn_reflns_av_R_equivalents 0.0607 _diffrn_reflns_av_sigmaI/netI 0.0883 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 28.34 _reflns_number_total 8182 _reflns_number_gt 4352 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART APEX II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SHELXTL _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics WingX _computing_publication_material WingX _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. The large residual density is located around Br1. ; _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^)+(0.0893P)^2^+6.1512P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8182 _refine_ls_number_parameters 439 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1544 _refine_ls_R_factor_gt 0.0748 _refine_ls_wR_factor_ref 0.2230 _refine_ls_wR_factor_gt 0.1808 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 0.06902(11) 0.47660(8) 0.24391(6) 0.0334(3) Uani 1 1 d . . . C1 C 0.1532(8) 0.3323(6) 0.3173(5) 0.0419(17) Uani 1 1 d . . . N1 N 0.2060(8) 0.2433(5) 0.3616(4) 0.0491(16) Uani 1 1 d . . . C2 C 0.2758(8) 0.4657(6) 0.1875(5) 0.0442(17) Uani 1 1 d . . . N2 N 0.3989(8) 0.4568(7) 0.1546(5) 0.068(2) Uani 1 1 d . . . C3 C 0.1597(9) 0.5137(6) 0.3310(5) 0.0425(17) Uani 1 1 d . . . N3 N 0.2122(9) 0.5364(6) 0.3828(5) 0.064(2) Uani 1 1 d . . . N4 N -0.1400(7) 0.4869(4) 0.3060(4) 0.0370(13) Uani 1 1 d . . . N5 N -0.2815(7) 0.5360(5) 0.2552(4) 0.0435(14) Uani 1 1 d . . . C4 C -0.1800(10) 0.4557(6) 0.3928(5) 0.0452(18) Uani 1 1 d . . . H10 H -0.1065 0.4199 0.4423 0.054 Uiso 1 1 calc R . . C5 C -0.3448(10) 0.4841(7) 0.3982(6) 0.058(2) Uani 1 1 d . . . H11 H -0.4030 0.4719 0.4508 0.070 Uiso 1 1 calc R . . C6 C -0.4062(10) 0.5334(6) 0.3116(7) 0.056(2) Uani 1 1 d . . . H12 H -0.5156 0.5609 0.2939 0.068 Uiso 1 1 calc R . . N6 N -0.0248(7) 0.4384(5) 0.1560(4) 0.0391(13) Uani 1 1 d . . . N7 N -0.1781(8) 0.4933(5) 0.1205(4) 0.0448(15) Uani 1 1 d . . . C7 C 0.0267(11) 0.3653(6) 0.1191(5) 0.053(2) Uani 1 1 d . . . H4 H 0.1285 0.3167 0.1314 0.064 Uiso 1 1 calc R . . C8 C -0.0888(13) 0.3708(8) 0.0612(6) 0.068(3) Uani 1 1 d . . . H5 H -0.0820 0.3286 0.0276 0.082 Uiso 1 1 calc R . . C9 C -0.2175(11) 0.4528(7) 0.0639(5) 0.059(2) Uani 1 1 d . . . H6 H -0.3160 0.4764 0.0316 0.071 Uiso 1 1 calc R . . N8 N -0.0172(7) 0.6283(4) 0.1655(4) 0.0374(13) Uani 1 1 d . . . N9 N -0.1727(7) 0.6635(5) 0.1294(4) 0.0453(15) Uani 1 1 d . . . C10 C 0.0405(10) 0.7126(6) 0.1372(5) 0.0448(18) Uani 1 1 d . . . H7 H 0.1440 0.7118 0.1518 0.054 Uiso 1 1 calc R . . C11 C -0.0738(11) 0.8011(6) 0.0836(6) 0.060(2) Uani 1 1 d . . . H8 H -0.0624 0.8692 0.0553 0.072 Uiso 1 1 calc R . . C12 C -0.2071(11) 0.7685(6) 0.0805(6) 0.060(2) Uani 1 1 d . . . H9 H -0.3052 0.8113 0.0498 0.072 Uiso 1 1 calc R . . B1 B -0.2746(11) 0.5836(7) 0.1510(6) 0.046(2) Uani 1 1 d . . . H1 H -0.391(9) 0.616(5) 0.123(5) 0.04(2) Uiso 1 1 d . . . Mn1 Mn 0.36381(12) 0.11660(7) 0.47174(6) 0.0310(3) Uani 1 1 d . . . O2 O 0.1993(5) 0.0539(4) 0.5241(3) 0.0395(11) Uani 1 1 d . . . O1 O 0.4504(5) 0.0226(3) 0.4098(3) 0.0329(10) Uani 1 1 d . . . N10 N 0.3263(7) 0.2005(4) 0.5509(4) 0.0366(13) Uani 1 1 d . . . N11 N 0.5438(7) 0.1832(4) 0.4244(4) 0.0353(13) Uani 1 1 d . . . C13 C 0.1103(7) 0.0624(5) 0.5928(4) 0.0341(15) Uani 1 1 d . . . C14 C 0.0088(8) -0.0052(6) 0.6243(5) 0.0444(17) Uani 1 1 d . . . H22 H 0.0019 -0.0477 0.5930 0.053 Uiso 1 1 calc R . . C15 C -0.0802(10) -0.0103(8) 0.6999(5) 0.061(2) Uani 1 1 d . . . H23 H -0.1446 -0.0569 0.7208 0.073 Uiso 1 1 calc R . . C16 C -0.0721(13) 0.0549(11) 0.7438(7) 0.091(4) Uani 1 1 d . . . C17 C 0.0212(12) 0.1232(10) 0.7143(7) 0.086(4) Uani 1 1 d . . . H25 H 0.0235 0.1665 0.7456 0.103 Uiso 1 1 calc R . . C18 C 0.1147(8) 0.1298(7) 0.6372(5) 0.0470(19) Uani 1 1 d . . . C19 C 0.2183(9) 0.2032(6) 0.6108(5) 0.0480(19) Uani 1 1 d . . . C20 C 0.1959(12) 0.2800(8) 0.6579(8) 0.081(3) Uani 1 1 d . . . H20A H 0.2681 0.2490 0.7106 0.122 Uiso 1 1 calc R . . H20B H 0.0860 0.2962 0.6761 0.122 Uiso 1 1 calc R . . H20C H 0.2193 0.3439 0.6172 0.122 Uiso 1 1 calc R . . C21 C 0.4327(10) 0.2720(6) 0.5270(5) 0.0487(19) Uani 1 1 d . . . H29A H 0.4577 0.2836 0.5803 0.058 Uiso 1 1 calc R . . H29B H 0.3784 0.3400 0.4813 0.058 Uiso 1 1 calc R . . C22 C 0.5875(9) 0.2216(6) 0.4906(5) 0.0456(18) Uani 1 1 d . . . H30A H 0.6479 0.2732 0.4618 0.055 Uiso 1 1 calc R . . H30B H 0.6548 0.1632 0.5399 0.055 Uiso 1 1 calc R . . C23 C 0.6095(8) 0.1955(5) 0.3474(4) 0.0362(15) Uani 1 1 d . . . C24 C 0.7285(10) 0.2617(6) 0.3135(6) 0.055(2) Uani 1 1 d . . . H24A H 0.6706 0.3340 0.2802 0.083 Uiso 1 1 calc R . . H24B H 0.8027 0.2352 0.2745 0.083 Uiso 1 1 calc R . . H24C H 0.7877 0.2579 0.3643 0.083 Uiso 1 1 calc R . . C25 C 0.5706(8) 0.1440(5) 0.2898(5) 0.0385(16) Uani 1 1 d . . . C26 C 0.6182(9) 0.1730(6) 0.1995(5) 0.0480(19) Uani 1 1 d . . . H16 H 0.6612 0.2306 0.1745 0.058 Uiso 1 1 calc R . . C27 C 0.6021(10) 0.1180(7) 0.1478(5) 0.055(2) Uani 1 1 d . . . C28 C 0.5380(10) 0.0337(7) 0.1816(5) 0.055(2) Uani 1 1 d . . . H18 H 0.5285 -0.0033 0.1458 0.066 Uiso 1 1 calc R . . C29 C 0.4874(8) 0.0040(6) 0.2698(5) 0.0406(16) Uani 1 1 d . . . H19 H 0.4439 -0.0535 0.2931 0.049 Uiso 1 1 calc R . . C30 C 0.5004(8) 0.0587(5) 0.3242(4) 0.0339(15) Uani 1 1 d . . . Br1 Br -0.1880(2) 0.0474(2) 0.85150(11) 0.1918(12) Uani 1 1 d . . . Br2 Br 0.67166(15) 0.15842(11) 0.02605(6) 0.0951(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0313(5) 0.0399(5) 0.0308(5) -0.0155(4) 0.0064(4) -0.0104(4) C1 0.032(4) 0.055(5) 0.044(4) -0.025(4) 0.006(3) -0.012(3) N1 0.047(4) 0.045(4) 0.048(4) -0.013(3) 0.002(3) -0.008(3) C2 0.035(4) 0.054(5) 0.045(4) -0.021(4) 0.008(3) -0.013(3) N2 0.039(4) 0.101(6) 0.068(5) -0.040(4) 0.018(4) -0.018(4) C3 0.039(4) 0.052(4) 0.042(4) -0.023(4) 0.004(3) -0.013(3) N3 0.057(5) 0.088(6) 0.065(5) -0.045(4) 0.002(4) -0.025(4) N4 0.038(3) 0.043(3) 0.037(3) -0.021(3) 0.008(3) -0.013(3) N5 0.035(3) 0.045(3) 0.054(4) -0.022(3) 0.011(3) -0.014(3) C4 0.059(5) 0.047(4) 0.042(4) -0.027(3) 0.020(4) -0.024(4) C5 0.064(5) 0.063(5) 0.073(6) -0.046(5) 0.045(5) -0.039(4) C6 0.040(4) 0.052(5) 0.094(7) -0.041(5) 0.031(4) -0.024(4) N6 0.041(3) 0.045(3) 0.032(3) -0.014(3) 0.004(3) -0.013(3) N7 0.048(4) 0.056(4) 0.036(3) -0.017(3) -0.002(3) -0.021(3) C7 0.063(5) 0.058(5) 0.052(5) -0.033(4) 0.020(4) -0.022(4) C8 0.091(7) 0.091(7) 0.053(5) -0.045(5) 0.022(5) -0.052(6) C9 0.066(6) 0.081(6) 0.037(4) -0.019(4) -0.001(4) -0.036(5) N8 0.036(3) 0.042(3) 0.039(3) -0.019(3) 0.007(3) -0.014(3) N9 0.044(4) 0.041(3) 0.047(3) -0.012(3) 0.001(3) -0.012(3) C10 0.053(5) 0.047(4) 0.045(4) -0.023(4) 0.011(4) -0.025(4) C11 0.081(6) 0.036(4) 0.060(5) -0.010(4) 0.005(5) -0.026(4) C12 0.066(6) 0.034(4) 0.067(6) -0.009(4) -0.010(5) -0.006(4) B1 0.034(5) 0.043(5) 0.054(5) -0.009(4) -0.007(4) -0.010(4) Mn1 0.0353(5) 0.0311(5) 0.0320(5) -0.0163(4) 0.0112(4) -0.0131(4) O2 0.040(3) 0.046(3) 0.046(3) -0.028(2) 0.017(2) -0.021(2) O1 0.041(3) 0.035(2) 0.027(2) -0.0148(19) 0.0110(19) -0.013(2) N10 0.046(3) 0.028(3) 0.041(3) -0.017(2) 0.013(3) -0.014(2) N11 0.041(3) 0.031(3) 0.036(3) -0.015(2) 0.010(2) -0.013(2) C13 0.028(3) 0.044(4) 0.031(3) -0.014(3) 0.006(3) -0.012(3) C14 0.034(4) 0.054(5) 0.051(4) -0.024(4) 0.002(3) -0.014(3) C15 0.053(5) 0.099(7) 0.051(5) -0.033(5) 0.021(4) -0.048(5) C16 0.086(7) 0.180(12) 0.067(6) -0.084(7) 0.054(6) -0.090(8) C17 0.076(6) 0.156(10) 0.096(7) -0.098(8) 0.056(6) -0.082(7) C18 0.037(4) 0.076(5) 0.051(4) -0.044(4) 0.019(3) -0.027(4) C19 0.044(4) 0.049(4) 0.062(5) -0.034(4) 0.016(4) -0.013(3) C20 0.083(7) 0.093(7) 0.123(9) -0.091(7) 0.058(6) -0.049(6) C21 0.068(5) 0.041(4) 0.052(4) -0.026(4) 0.019(4) -0.028(4) C22 0.053(5) 0.053(4) 0.044(4) -0.023(4) 0.014(3) -0.029(4) C23 0.034(4) 0.033(3) 0.039(4) -0.012(3) 0.009(3) -0.008(3) C24 0.066(5) 0.057(5) 0.061(5) -0.031(4) 0.032(4) -0.039(4) C25 0.038(4) 0.039(4) 0.040(4) -0.017(3) 0.012(3) -0.012(3) C26 0.047(4) 0.056(5) 0.035(4) -0.013(3) 0.013(3) -0.014(4) C27 0.052(5) 0.084(6) 0.032(4) -0.022(4) 0.015(4) -0.024(4) C28 0.051(5) 0.089(6) 0.036(4) -0.035(4) 0.006(4) -0.022(4) C29 0.038(4) 0.046(4) 0.043(4) -0.021(3) 0.006(3) -0.012(3) C30 0.033(3) 0.038(4) 0.030(3) -0.016(3) 0.010(3) -0.006(3) Br1 0.2000(17) 0.413(3) 0.1446(13) -0.2077(19) 0.1392(13) -0.250(2) Br2 0.1028(9) 0.1540(11) 0.0385(5) -0.0357(6) 0.0305(5) -0.0572(8) _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 C1 1.887(8) . ? Fe1 C2 1.931(7) . ? Fe1 C3 1.932(8) . ? Fe1 N6 1.966(6) . ? Fe1 N8 1.987(6) . ? Fe1 N4 1.988(5) . ? C1 N1 1.161(9) . ? N1 Mn1 2.175(7) . ? C2 N2 1.145(9) . ? C3 N3 1.147(9) . ? N4 C4 1.335(8) . ? N4 N5 1.361(8) . ? N5 C6 1.351(9) . ? N5 B1 1.541(11) . ? C4 C5 1.368(11) . ? C4 H10 0.9300 . ? C5 C6 1.353(12) . ? C5 H11 0.9300 . ? C6 H12 0.9300 . ? N6 C7 1.336(9) . ? N6 N7 1.364(8) . ? N7 C9 1.340(10) . ? N7 B1 1.545(11) . ? C7 C8 1.367(12) . ? C7 H4 0.9300 . ? C8 C9 1.377(13) . ? C8 H5 0.9300 . ? C9 H6 0.9300 . ? N8 C10 1.331(9) . ? N8 N9 1.372(8) . ? N9 C12 1.349(9) . ? N9 B1 1.545(10) . ? C10 C11 1.374(11) . ? C10 H7 0.9300 . ? C11 C12 1.359(12) . ? C11 H8 0.9300 . ? C12 H9 0.9300 . ? B1 H1 1.03(7) . ? Mn1 O2 1.862(4) . ? Mn1 O1 1.908(4) . ? Mn1 N10 1.992(5) . ? Mn1 N11 1.994(5) . ? Mn1 O1 2.418(4) 2_656 ? O2 C13 1.316(7) . ? O1 C30 1.350(7) . ? O1 Mn1 2.418(4) 2_656 ? N10 C19 1.290(8) . ? N10 C21 1.479(9) . ? N11 C23 1.285(8) . ? N11 C22 1.466(9) . ? C13 C18 1.395(9) . ? C13 C14 1.405(9) . ? C14 C15 1.370(10) . ? C14 H22 0.9300 . ? C15 C16 1.371(13) . ? C15 H23 0.9300 . ? C16 C17 1.357(13) . ? C16 Br1 1.907(8) . ? C17 C18 1.409(10) . ? C17 H25 0.9300 . ? C18 C19 1.479(10) . ? C19 C20 1.506(10) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.516(10) . ? C21 H29A 0.9700 . ? C21 H29B 0.9700 . ? C22 H30A 0.9700 . ? C22 H30B 0.9700 . ? C23 C25 1.473(10) . ? C23 C24 1.515(9) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.404(9) . ? C25 C30 1.409(9) . ? C26 C27 1.366(11) . ? C26 H16 0.9300 . ? C27 C28 1.365(12) . ? C27 Br2 1.906(7) . ? C28 C29 1.381(9) . ? C28 H18 0.9300 . ? C29 C30 1.390(9) . ? C29 H19 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe1 C2 86.3(3) . . ? C1 Fe1 C3 89.1(3) . . ? C2 Fe1 C3 87.7(3) . . ? C1 Fe1 N6 90.8(3) . . ? C2 Fe1 N6 92.7(3) . . ? C3 Fe1 N6 179.5(3) . . ? C1 Fe1 N8 179.2(3) . . ? C2 Fe1 N8 93.0(3) . . ? C3 Fe1 N8 91.1(3) . . ? N6 Fe1 N8 89.0(2) . . ? C1 Fe1 N4 92.8(3) . . ? C2 Fe1 N4 178.0(3) . . ? C3 Fe1 N4 90.5(3) . . ? N6 Fe1 N4 89.0(2) . . ? N8 Fe1 N4 87.9(2) . . ? N1 C1 Fe1 179.1(6) . . ? C1 N1 Mn1 151.5(6) . . ? N2 C2 Fe1 178.4(7) . . ? N3 C3 Fe1 179.3(7) . . ? C4 N4 N5 106.6(6) . . ? C4 N4 Fe1 134.1(5) . . ? N5 N4 Fe1 119.3(4) . . ? C6 N5 N4 108.7(7) . . ? C6 N5 B1 132.4(7) . . ? N4 N5 B1 118.9(5) . . ? N4 C4 C5 110.0(8) . . ? N4 C4 H10 125.0 . . ? C5 C4 H10 125.0 . . ? C6 C5 C4 106.3(7) . . ? C6 C5 H11 126.9 . . ? C4 C5 H11 126.9 . . ? N5 C6 C5 108.3(7) . . ? N5 C6 H12 125.8 . . ? C5 C6 H12 125.8 . . ? C7 N6 N7 105.9(6) . . ? C7 N6 Fe1 134.7(6) . . ? N7 N6 Fe1 119.4(4) . . ? C9 N7 N6 109.1(7) . . ? C9 N7 B1 131.8(7) . . ? N6 N7 B1 119.1(6) . . ? N6 C7 C8 111.6(8) . . ? N6 C7 H4 124.2 . . ? C8 C7 H4 124.2 . . ? C7 C8 C9 104.4(8) . . ? C7 C8 H5 127.8 . . ? C9 C8 H5 127.8 . . ? N7 C9 C8 109.1(8) . . ? N7 C9 H6 125.4 . . ? C8 C9 H6 125.4 . . ? C10 N8 N9 106.1(6) . . ? C10 N8 Fe1 134.9(5) . . ? N9 N8 Fe1 118.9(4) . . ? C12 N9 N8 109.0(6) . . ? C12 N9 B1 132.2(7) . . ? N8 N9 B1 118.8(6) . . ? N8 C10 C11 110.6(7) . . ? N8 C10 H7 124.7 . . ? C11 C10 H7 124.7 . . ? C12 C11 C10 105.9(7) . . ? C12 C11 H8 127.0 . . ? C10 C11 H8 127.0 . . ? N9 C12 C11 108.3(8) . . ? N9 C12 H9 125.8 . . ? C11 C12 H9 125.8 . . ? N5 B1 N9 106.4(7) . . ? N5 B1 N7 107.3(6) . . ? N9 B1 N7 107.0(6) . . ? N5 B1 H1 109(4) . . ? N9 B1 H1 114(4) . . ? N7 B1 H1 113(4) . . ? O2 Mn1 O1 94.90(18) . . ? O2 Mn1 N10 91.9(2) . . ? O1 Mn1 N10 166.2(2) . . ? O2 Mn1 N11 175.9(2) . . ? O1 Mn1 N11 87.8(2) . . ? N10 Mn1 N11 84.8(2) . . ? O2 Mn1 N1 93.7(2) . . ? O1 Mn1 N1 98.1(2) . . ? N10 Mn1 N1 93.4(2) . . ? N11 Mn1 N1 88.9(2) . . ? O2 Mn1 O1 88.70(19) . 2_656 ? O1 Mn1 O1 80.83(18) . 2_656 ? N10 Mn1 O1 87.40(19) . 2_656 ? N11 Mn1 O1 88.73(19) . 2_656 ? N1 Mn1 O1 177.42(19) . 2_656 ? C13 O2 Mn1 129.3(4) . . ? C30 O1 Mn1 121.0(4) . . ? C30 O1 Mn1 119.6(4) . 2_656 ? Mn1 O1 Mn1 99.17(17) . 2_656 ? C19 N10 C21 121.0(6) . . ? C19 N10 Mn1 128.1(5) . . ? C21 N10 Mn1 110.7(4) . . ? C23 N11 C22 124.0(6) . . ? C23 N11 Mn1 127.1(5) . . ? C22 N11 Mn1 108.9(4) . . ? O2 C13 C18 124.9(6) . . ? O2 C13 C14 116.1(6) . . ? C18 C13 C14 119.0(6) . . ? C15 C14 C13 121.9(7) . . ? C15 C14 H22 119.0 . . ? C13 C14 H22 119.0 . . ? C14 C15 C16 118.3(7) . . ? C14 C15 H23 120.8 . . ? C16 C15 H23 120.8 . . ? C17 C16 C15 121.7(7) . . ? C17 C16 Br1 118.4(7) . . ? C15 C16 Br1 119.9(7) . . ? C16 C17 C18 121.2(8) . . ? C16 C17 H25 119.4 . . ? C18 C17 H25 119.4 . . ? C13 C18 C17 117.8(7) . . ? C13 C18 C19 123.8(6) . . ? C17 C18 C19 118.4(7) . . ? N10 C19 C18 121.4(6) . . ? N10 C19 C20 120.9(7) . . ? C18 C19 C20 117.7(6) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N10 C21 C22 108.6(5) . . ? N10 C21 H29A 110.0 . . ? C22 C21 H29A 110.0 . . ? N10 C21 H29B 110.0 . . ? C22 C21 H29B 110.0 . . ? H29A C21 H29B 108.3 . . ? N11 C22 C21 108.3(6) . . ? N11 C22 H30A 110.0 . . ? C21 C22 H30A 110.0 . . ? N11 C22 H30B 110.0 . . ? C21 C22 H30B 110.0 . . ? H30A C22 H30B 108.4 . . ? N11 C23 C25 120.0(6) . . ? N11 C23 C24 121.8(6) . . ? C25 C23 C24 118.2(6) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C30 117.8(7) . . ? C26 C25 C23 119.5(6) . . ? C30 C25 C23 122.4(6) . . ? C27 C26 C25 121.0(7) . . ? C27 C26 H16 119.5 . . ? C25 C26 H16 119.5 . . ? C28 C27 C26 121.3(7) . . ? C28 C27 Br2 119.0(6) . . ? C26 C27 Br2 119.7(6) . . ? C27 C28 C29 119.3(7) . . ? C27 C28 H18 120.3 . . ? C29 C28 H18 120.3 . . ? C28 C29 C30 121.0(7) . . ? C28 C29 H19 119.5 . . ? C30 C29 H19 119.5 . . ? O1 C30 C29 116.7(6) . . ? O1 C30 C25 123.7(6) . . ? C29 C30 C25 119.5(6) . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 3.457 _refine_diff_density_min -2.198 _refine_diff_density_rms 0.120 # Attachment 'complex3.cif' data_complex3 _database_code_depnum_ccdc_archive 'CCDC 705441' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(Tp)Fe(CN)3]2[Mn(salen)]26H2O' _chemical_formula_sum 'C56 H60 B2 Fe2 Mn2 N22 O10' _chemical_formula_weight 1444.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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 11.2358(3) _cell_length_b 12.0137(4) _cell_length_c 14.2050(4) _cell_angle_alpha 82.2640(10) _cell_angle_beta 68.1050(10) _cell_angle_gamma 63.3820(10) _cell_volume 1589.35(8) _cell_formula_units_Z 1 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 2981 _cell_measurement_theta_min 2.167 _cell_measurement_theta_max 23.3475 _exptl_crystal_description Plate _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 742 _exptl_absorpt_coefficient_mu 0.910 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8511 _exptl_absorpt_correction_T_max 0.9723 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26464 _diffrn_reflns_av_R_equivalents 0.0839 _diffrn_reflns_av_sigmaI/netI 0.0998 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7758 _reflns_number_gt 4914 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART APEX II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SHELXTL _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics WingX _computing_publication_material WingX _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^)+(0.0424P)^2^+1.0117P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7758 _refine_ls_number_parameters 428 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1081 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1215 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 0.24732(5) 0.34300(5) 0.15498(3) 0.01732(13) Uani 1 1 d . . . C1 C 0.2166(3) 0.2185(3) 0.2471(2) 0.0175(7) Uani 1 1 d . . . N1 N 0.1953(3) 0.1485(3) 0.3072(2) 0.0211(6) Uani 1 1 d . . . C2 C 0.3276(4) 0.3728(3) 0.2414(3) 0.0237(8) Uani 1 1 d . . . N2 N 0.3743(4) 0.3952(3) 0.2923(3) 0.0371(8) Uani 1 1 d . . . C3 C 0.0594(4) 0.4558(3) 0.2415(3) 0.0216(8) Uani 1 1 d . . . N3 N -0.0566(3) 0.5179(3) 0.2920(2) 0.0286(7) Uani 1 1 d . . . N4 N 0.4302(3) 0.2194(3) 0.0642(2) 0.0208(6) Uani 1 1 d . . . C4 C 0.5367(4) 0.1165(3) 0.0790(3) 0.0259(8) Uani 1 1 d . . . H4 H 0.5430 0.0883 0.1435 0.031 Uiso 1 1 calc R . . C5 C 0.6363(4) 0.0569(4) -0.0135(3) 0.0306(9) Uani 1 1 d . . . H5 H 0.7220 -0.0175 -0.0247 0.037 Uiso 1 1 calc R . . C6 C 0.5835(4) 0.1295(4) -0.0856(3) 0.0297(9) Uani 1 1 d . . . H6 H 0.6270 0.1130 -0.1569 0.036 Uiso 1 1 calc R . . N5 N 0.4616(3) 0.2265(3) -0.0386(2) 0.0250(7) Uani 1 1 d . . . B1 B 0.3563(5) 0.3369(4) -0.0796(3) 0.0276(10) Uani 1 1 d . . . H1 H 0.394(4) 0.335(3) -0.164(3) 0.029(10) Uiso 1 1 d . . . N6 N 0.1561(3) 0.3233(3) 0.0685(2) 0.0197(6) Uani 1 1 d . . . C7 C 0.0360(4) 0.3125(3) 0.0879(3) 0.0267(8) Uani 1 1 d . . . H7 H -0.0257 0.3066 0.1537 0.032 Uiso 1 1 calc R . . C8 C 0.0144(4) 0.3112(4) -0.0010(3) 0.0354(10) Uani 1 1 d . . . H8 H -0.0628 0.3045 -0.0085 0.042 Uiso 1 1 calc R . . C9 C 0.1285(4) 0.3216(4) -0.0769(3) 0.0338(10) Uani 1 1 d . . . H9 H 0.1445 0.3237 -0.1475 0.041 Uiso 1 1 calc R . . N7 N 0.2130(3) 0.3284(3) -0.0342(2) 0.0257(7) Uani 1 1 d . . . N8 N 0.2850(3) 0.4748(3) 0.0660(2) 0.0244(7) Uani 1 1 d . . . C10 C 0.2858(4) 0.5812(4) 0.0838(3) 0.0297(9) Uani 1 1 d . . . H10 H 0.2553 0.6164 0.1494 0.036 Uiso 1 1 calc R . . C11 C 0.3372(4) 0.6328(4) -0.0065(3) 0.0381(10) Uani 1 1 d . . . H11 H 0.3483 0.7078 -0.0152 0.046 Uiso 1 1 calc R . . C12 C 0.3686(4) 0.5512(4) -0.0807(3) 0.0387(11) Uani 1 1 d . . . H12 H 0.4071 0.5599 -0.1518 0.046 Uiso 1 1 calc R . . N9 N 0.3361(3) 0.4568(3) -0.0365(2) 0.0282(7) Uani 1 1 d . . . Mn1 Mn 0.07983(5) 0.09422(5) 0.45604(4) 0.01584(13) Uani 1 1 d . . . O1 O 0.0650(2) -0.0300(2) 0.39571(16) 0.0175(5) Uani 1 1 d . . . C13 C 0.0206(3) -0.0066(3) 0.3158(2) 0.0180(7) Uani 1 1 d . . . C14 C 0.0773(4) -0.1013(3) 0.2437(3) 0.0241(8) Uani 1 1 d . . . H14 H 0.1523 -0.1788 0.2481 0.029 Uiso 1 1 calc R . . C15 C 0.0262(4) -0.0844(4) 0.1653(3) 0.0297(9) Uani 1 1 d . . . H15 H 0.0660 -0.1504 0.1169 0.036 Uiso 1 1 calc R . . C16 C -0.0825(4) 0.0281(4) 0.1573(3) 0.0324(9) Uani 1 1 d . . . H16 H -0.1172 0.0393 0.1035 0.039 Uiso 1 1 calc R . . C17 C -0.1401(4) 0.1237(4) 0.2272(3) 0.0280(9) Uani 1 1 d . . . H17 H -0.2162 0.2001 0.2224 0.034 Uiso 1 1 calc R . . C18 C -0.0873(3) 0.1094(3) 0.3061(2) 0.0201(7) Uani 1 1 d . . . C19 C -0.1533(4) 0.2126(3) 0.3780(3) 0.0216(8) Uani 1 1 d . . . H19 H -0.2400 0.2797 0.3770 0.026 Uiso 1 1 calc R . . N10 N -0.1026(3) 0.2196(3) 0.4432(2) 0.0195(6) Uani 1 1 d . . . C20 C -0.1765(4) 0.3268(3) 0.5160(3) 0.0274(9) Uani 1 1 d . . . H20A H -0.2305 0.3060 0.5831 0.033 Uiso 1 1 calc R . . H20B H -0.2437 0.3997 0.4914 0.033 Uiso 1 1 calc R . . C21 C -0.0613(4) 0.3551(3) 0.5237(3) 0.0276(9) Uani 1 1 d . . . H21A H -0.0251 0.3973 0.4626 0.033 Uiso 1 1 calc R . . H21B H -0.0996 0.4100 0.5842 0.033 Uiso 1 1 calc R . . N11 N 0.0540(3) 0.2342(3) 0.5324(2) 0.0194(6) Uani 1 1 d . . . C22 C 0.1286(4) 0.2275(3) 0.5854(2) 0.0227(8) Uani 1 1 d . . . H22 H 0.1035 0.3021 0.6194 0.027 Uiso 1 1 calc R . . C23 C 0.2453(4) 0.1184(3) 0.5975(2) 0.0206(8) Uani 1 1 d . . . C24 C 0.3139(4) 0.1296(4) 0.6591(3) 0.0274(9) Uani 1 1 d . . . H24 H 0.2799 0.2079 0.6913 0.033 Uiso 1 1 calc R . . C25 C 0.4283(4) 0.0300(4) 0.6731(3) 0.0297(9) Uani 1 1 d . . . H25 H 0.4737 0.0392 0.7142 0.036 Uiso 1 1 calc R . . C26 C 0.4774(4) -0.0845(4) 0.6267(3) 0.0271(9) Uani 1 1 d . . . H26 H 0.5560 -0.1541 0.6370 0.033 Uiso 1 1 calc R . . C27 C 0.4135(4) -0.0989(3) 0.5655(3) 0.0237(8) Uani 1 1 d . . . H27 H 0.4483 -0.1781 0.5346 0.028 Uiso 1 1 calc R . . C28 C 0.2981(3) 0.0022(3) 0.5488(2) 0.0182(7) Uani 1 1 d . . . O2 O 0.2410(2) -0.0150(2) 0.48761(16) 0.0176(5) Uani 1 1 d . . . O3 O 0.5215(3) 0.4184(2) 0.4025(2) 0.0347(7) Uani 1 1 d . . . O4 O 0.6271(3) 0.5918(3) 0.3858(2) 0.0392(7) Uani 1 1 d . . . O5 O 0.3941(4) 0.7904(3) 0.3280(2) 0.0616(10) 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 0.0196(3) 0.0196(3) 0.0167(2) 0.0043(2) -0.0079(2) -0.0114(2) C1 0.0143(16) 0.0202(19) 0.0163(16) 0.0005(14) -0.0058(13) -0.0057(15) N1 0.0198(15) 0.0222(17) 0.0206(15) 0.0019(13) -0.0067(12) -0.0091(13) C2 0.028(2) 0.025(2) 0.0235(18) 0.0070(15) -0.0115(16) -0.0160(17) N2 0.048(2) 0.041(2) 0.0377(19) 0.0089(16) -0.0255(18) -0.0253(19) C3 0.033(2) 0.0179(19) 0.0216(17) 0.0053(15) -0.0154(16) -0.0138(17) N3 0.0324(19) 0.0247(18) 0.0264(16) -0.0025(14) -0.0109(15) -0.0090(15) N4 0.0207(15) 0.0276(17) 0.0176(14) 0.0073(12) -0.0080(12) -0.0141(14) C4 0.0227(19) 0.029(2) 0.030(2) 0.0087(17) -0.0102(16) -0.0150(17) C5 0.0191(19) 0.028(2) 0.038(2) -0.0012(18) -0.0023(17) -0.0099(17) C6 0.0204(19) 0.037(2) 0.028(2) -0.0026(18) -0.0017(16) -0.0146(18) N5 0.0229(16) 0.0352(19) 0.0174(14) 0.0051(13) -0.0050(13) -0.0156(15) B1 0.024(2) 0.038(3) 0.017(2) 0.0094(18) -0.0058(17) -0.014(2) N6 0.0172(15) 0.0249(17) 0.0174(14) 0.0018(12) -0.0067(12) -0.0094(13) C7 0.0210(19) 0.031(2) 0.030(2) -0.0033(17) -0.0070(16) -0.0126(17) C8 0.028(2) 0.043(3) 0.042(2) -0.008(2) -0.0191(19) -0.013(2) C9 0.028(2) 0.045(3) 0.027(2) -0.0055(18) -0.0154(17) -0.0084(19) N7 0.0273(17) 0.0349(19) 0.0163(14) 0.0037(13) -0.0104(13) -0.0132(15) N8 0.0256(16) 0.0274(18) 0.0264(16) 0.0109(13) -0.0121(13) -0.0169(14) C10 0.026(2) 0.026(2) 0.048(2) 0.0128(18) -0.0217(18) -0.0159(18) C11 0.029(2) 0.032(2) 0.065(3) 0.022(2) -0.024(2) -0.021(2) C12 0.023(2) 0.045(3) 0.047(3) 0.031(2) -0.0140(19) -0.021(2) N9 0.0234(16) 0.037(2) 0.0263(16) 0.0165(14) -0.0102(13) -0.0177(15) Mn1 0.0156(3) 0.0140(3) 0.0173(3) 0.0018(2) -0.0059(2) -0.0061(2) O1 0.0169(12) 0.0204(13) 0.0159(11) 0.0035(10) -0.0073(9) -0.0081(10) C13 0.0171(17) 0.0240(19) 0.0166(16) 0.0044(14) -0.0063(14) -0.0129(15) C14 0.0234(19) 0.027(2) 0.0213(18) 0.0022(15) -0.0051(15) -0.0130(17) C15 0.031(2) 0.041(2) 0.0221(19) -0.0044(17) -0.0052(16) -0.023(2) C16 0.038(2) 0.048(3) 0.0237(19) 0.0081(18) -0.0171(18) -0.026(2) C17 0.026(2) 0.037(2) 0.0263(19) 0.0140(17) -0.0128(16) -0.0182(18) C18 0.0167(17) 0.026(2) 0.0222(17) 0.0080(15) -0.0072(14) -0.0147(16) C19 0.0184(17) 0.0181(18) 0.0264(18) 0.0094(15) -0.0110(15) -0.0063(15) N10 0.0194(15) 0.0173(15) 0.0205(14) 0.0025(12) -0.0066(12) -0.0075(13) C20 0.0234(19) 0.018(2) 0.0262(19) -0.0040(16) -0.0057(16) 0.0019(16) C21 0.035(2) 0.0146(19) 0.0277(19) 0.0000(15) -0.0108(17) -0.0064(17) N11 0.0225(15) 0.0148(15) 0.0179(14) 0.0015(12) -0.0039(12) -0.0084(13) C22 0.0263(19) 0.023(2) 0.0172(17) -0.0019(15) -0.0018(15) -0.0139(17) C23 0.0244(19) 0.0227(19) 0.0170(16) 0.0036(14) -0.0068(14) -0.0133(16) C24 0.031(2) 0.037(2) 0.0218(18) 0.0017(17) -0.0077(16) -0.0233(19) C25 0.035(2) 0.044(3) 0.0236(19) 0.0091(18) -0.0153(17) -0.026(2) C26 0.0234(19) 0.039(2) 0.0236(19) 0.0160(17) -0.0130(16) -0.0178(18) C27 0.0255(19) 0.025(2) 0.0250(19) 0.0085(16) -0.0095(16) -0.0163(17) C28 0.0209(18) 0.0248(19) 0.0150(16) 0.0065(14) -0.0062(14) -0.0166(16) O2 0.0173(12) 0.0159(12) 0.0211(12) 0.0024(10) -0.0083(10) -0.0078(10) O3 0.0286(15) 0.0328(16) 0.0453(16) -0.0069(13) -0.0209(13) -0.0069(13) O4 0.0404(17) 0.0350(17) 0.0420(16) 0.0072(13) -0.0163(14) -0.0164(14) O5 0.057(2) 0.063(2) 0.057(2) -0.0052(18) -0.0178(18) -0.0197(19) _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 C1 1.915(3) . ? Fe1 C2 1.919(4) . ? Fe1 C3 1.937(4) . ? Fe1 N6 1.963(3) . ? Fe1 N4 1.974(3) . ? Fe1 N8 1.987(3) . ? C1 N1 1.153(4) . ? N1 Mn1 2.218(3) . ? C2 N2 1.155(4) . ? C3 N3 1.160(4) . ? N4 C4 1.340(4) . ? N4 N5 1.369(4) . ? C4 C5 1.389(5) . ? C4 H4 0.9500 . ? C5 C6 1.382(5) . ? C5 H5 0.9500 . ? C6 N5 1.333(5) . ? C6 H6 0.9500 . ? N5 B1 1.549(5) . ? B1 N9 1.531(6) . ? B1 N7 1.541(5) . ? B1 H1 1.11(3) . ? N6 C7 1.336(4) . ? N6 N7 1.362(4) . ? C7 C8 1.374(5) . ? C7 H7 0.9500 . ? C8 C9 1.379(6) . ? C8 H8 0.9500 . ? C9 N7 1.336(4) . ? C9 H9 0.9500 . ? N8 C10 1.341(5) . ? N8 N9 1.359(4) . ? C10 C11 1.385(5) . ? C10 H10 0.9500 . ? C11 C12 1.373(6) . ? C11 H11 0.9500 . ? C12 N9 1.350(5) . ? C12 H12 0.9500 . ? Mn1 O2 1.876(2) . ? Mn1 O1 1.913(2) . ? Mn1 N11 1.977(3) . ? Mn1 N10 1.985(3) . ? Mn1 O1 2.411(2) 2_556 ? O1 C13 1.352(4) . ? O1 Mn1 2.411(2) 2_556 ? C13 C14 1.388(5) . ? C13 C18 1.411(5) . ? C14 C15 1.386(5) . ? C14 H14 0.9500 . ? C15 C16 1.384(5) . ? C15 H15 0.9500 . ? C16 C17 1.373(5) . ? C16 H16 0.9500 . ? C17 C18 1.411(5) . ? C17 H17 0.9500 . ? C18 C19 1.442(5) . ? C19 N10 1.284(4) . ? C19 H19 0.9500 . ? N10 C20 1.476(4) . ? C20 C21 1.521(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 N11 1.479(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? N11 C22 1.292(4) . ? C22 C23 1.426(5) . ? C22 H22 0.9500 . ? C23 C28 1.411(5) . ? C23 C24 1.417(5) . ? C24 C25 1.368(5) . ? C24 H24 0.9500 . ? C25 C26 1.388(5) . ? C25 H25 0.9500 . ? C26 C27 1.385(5) . ? C26 H26 0.9500 . ? C27 C28 1.397(5) . ? C27 H27 0.9500 . ? C28 O2 1.339(4) . ? 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 C1 Fe1 C2 86.89(14) . . ? C1 Fe1 C3 85.08(14) . . ? C2 Fe1 C3 89.59(15) . . ? C1 Fe1 N6 94.79(13) . . ? C2 Fe1 N6 176.45(14) . . ? C3 Fe1 N6 87.44(13) . . ? C1 Fe1 N4 92.37(13) . . ? C2 Fe1 N4 95.03(14) . . ? C3 Fe1 N4 174.60(13) . . ? N6 Fe1 N4 88.03(11) . . ? C1 Fe1 N8 175.79(13) . . ? C2 Fe1 N8 88.91(13) . . ? C3 Fe1 N8 94.80(14) . . ? N6 Fe1 N8 89.41(12) . . ? N4 Fe1 N8 88.10(12) . . ? N1 C1 Fe1 176.0(3) . . ? C1 N1 Mn1 154.4(3) . . ? N2 C2 Fe1 177.4(3) . . ? N3 C3 Fe1 175.3(3) . . ? C4 N4 N5 106.4(3) . . ? C4 N4 Fe1 134.3(2) . . ? N5 N4 Fe1 119.1(2) . . ? N4 C4 C5 110.3(3) . . ? N4 C4 H4 124.9 . . ? C5 C4 H4 124.9 . . ? C6 C5 C4 104.8(3) . . ? C6 C5 H5 127.6 . . ? C4 C5 H5 127.6 . . ? N5 C6 C5 108.8(3) . . ? N5 C6 H6 125.6 . . ? C5 C6 H6 125.6 . . ? C6 N5 N4 109.6(3) . . ? C6 N5 B1 131.8(3) . . ? N4 N5 B1 118.5(3) . . ? N9 B1 N7 107.8(3) . . ? N9 B1 N5 107.2(3) . . ? N7 B1 N5 106.5(3) . . ? N9 B1 H1 111.4(19) . . ? N7 B1 H1 111.2(19) . . ? N5 B1 H1 112.5(19) . . ? C7 N6 N7 106.6(3) . . ? C7 N6 Fe1 133.5(2) . . ? N7 N6 Fe1 119.8(2) . . ? N6 C7 C8 110.3(3) . . ? N6 C7 H7 124.8 . . ? C8 C7 H7 124.8 . . ? C7 C8 C9 105.3(3) . . ? C7 C8 H8 127.4 . . ? C9 C8 H8 127.4 . . ? N7 C9 C8 108.4(3) . . ? N7 C9 H9 125.8 . . ? C8 C9 H9 125.8 . . ? C9 N7 N6 109.4(3) . . ? C9 N7 B1 132.2(3) . . ? N6 N7 B1 118.3(3) . . ? C10 N8 N9 106.6(3) . . ? C10 N8 Fe1 133.3(3) . . ? N9 N8 Fe1 119.6(2) . . ? N8 C10 C11 110.7(4) . . ? N8 C10 H10 124.7 . . ? C11 C10 H10 124.7 . . ? C12 C11 C10 104.6(4) . . ? C12 C11 H11 127.7 . . ? C10 C11 H11 127.7 . . ? N9 C12 C11 109.1(4) . . ? N9 C12 H12 125.5 . . ? C11 C12 H12 125.5 . . ? C12 N9 N8 109.0(3) . . ? C12 N9 B1 132.5(3) . . ? N8 N9 B1 118.3(3) . . ? O2 Mn1 O1 96.16(10) . . ? O2 Mn1 N11 91.81(11) . . ? O1 Mn1 N11 168.62(11) . . ? O2 Mn1 N10 171.67(10) . . ? O1 Mn1 N10 89.44(10) . . ? N11 Mn1 N10 81.81(11) . . ? O2 Mn1 N1 96.72(10) . . ? O1 Mn1 N1 93.04(10) . . ? N11 Mn1 N1 94.07(11) . . ? N10 Mn1 N1 89.11(11) . . ? O2 Mn1 O1 89.08(9) . 2_556 ? O1 Mn1 O1 79.77(9) . 2_556 ? N11 Mn1 O1 92.29(9) . 2_556 ? N10 Mn1 O1 85.83(10) . 2_556 ? N1 Mn1 O1 171.24(9) . 2_556 ? C13 O1 Mn1 122.1(2) . . ? C13 O1 Mn1 114.10(19) . 2_556 ? Mn1 O1 Mn1 100.23(9) . 2_556 ? O1 C13 C14 119.2(3) . . ? O1 C13 C18 121.9(3) . . ? C14 C13 C18 118.8(3) . . ? C15 C14 C13 121.0(3) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C16 C15 C14 120.4(3) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C17 C16 C15 119.9(3) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 120.6(4) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C13 C18 C17 119.2(3) . . ? C13 C18 C19 122.6(3) . . ? C17 C18 C19 118.1(3) . . ? N10 C19 C18 124.3(3) . . ? N10 C19 H19 117.9 . . ? C18 C19 H19 117.9 . . ? C19 N10 C20 121.7(3) . . ? C19 N10 Mn1 125.1(2) . . ? C20 N10 Mn1 113.2(2) . . ? N10 C20 C21 106.2(3) . . ? N10 C20 H20A 110.5 . . ? C21 C20 H20A 110.5 . . ? N10 C20 H20B 110.5 . . ? C21 C20 H20B 110.5 . . ? H20A C20 H20B 108.7 . . ? N11 C21 C20 106.8(3) . . ? N11 C21 H21A 110.4 . . ? C20 C21 H21A 110.4 . . ? N11 C21 H21B 110.4 . . ? C20 C21 H21B 110.4 . . ? H21A C21 H21B 108.6 . . ? C22 N11 C21 120.0(3) . . ? C22 N11 Mn1 125.9(2) . . ? C21 N11 Mn1 114.1(2) . . ? N11 C22 C23 125.9(3) . . ? N11 C22 H22 117.1 . . ? C23 C22 H22 117.1 . . ? C28 C23 C24 118.8(3) . . ? C28 C23 C22 123.5(3) . . ? C24 C23 C22 117.6(3) . . ? C25 C24 C23 121.3(4) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C24 C25 C26 119.3(3) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C27 C26 C25 121.0(3) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 C28 120.6(3) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? O2 C28 C27 118.7(3) . . ? O2 C28 C23 122.3(3) . . ? C27 C28 C23 119.0(3) . . ? C28 O2 Mn1 130.2(2) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.589 _refine_diff_density_min -0.648 _refine_diff_density_rms 0.095