# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author ; Dr. Eugenia V. Peresypkina Institute of Inorganic Chemistry SD RAS Ak.Lavrentiev prosp. 3 Novosibirsk 630090 Russia ; _publ_contact_author_phone none _publ_contact_author_fax '007 383 3309489' _publ_contact_author_email peresyp@niic.nsc.ru _publ_contact_author_name 'Dr. Eugenia V. Peresypkina' _publ_author_name E.V.Peresypkina # 2. Data data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 849758' #TrackingRef '- deposit_NEW.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H40 Fe Mn2 N10 O7, C2 H5 OH' _chemical_formula_structural '[Fe (C N)5 (N O)] (Mn (C12 H18 N2 O2) (H2 O))2] * C2 H5 O H' _chemical_formula_sum 'C31 H46 Fe Mn2 N10 O8' _chemical_formula_weight 852.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.0620(5) _cell_length_b 14.5264(4) _cell_length_c 14.3781(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.3120(10) _cell_angle_gamma 90.00 _cell_volume 3978.09(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100.0(2) _cell_measurement_reflns_used 6895 _cell_measurement_theta_min 3.1428 _cell_measurement_theta_max 30.9337 _exptl_crystal_description lath _exptl_crystal_colour brown _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 1.043 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.875585 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'based on intensities (SADABS, Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8Apex CCD detector' _diffrn_measurement_method 'combined omega- and phi-scans' _diffrn_detector_area_resol_mean 25 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 18426 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 31.54 _reflns_number_total 5529 _reflns_number_gt 5037 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 V.1.27 (Bruker, 2005)' _computing_cell_refinement 'Apex2 V.1.27 (Bruker, 2005)' _computing_data_reduction 'Apex2 V.1.27 (Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V6.22 (Bruker, 2000-2005)' _computing_publication_material 'local programs' _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^)+(0.0286P)^2^+17.8008P] 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 5529 _refine_ls_number_parameters 250 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0728 _refine_ls_R_factor_gt 0.0654 _refine_ls_wR_factor_ref 0.1263 _refine_ls_wR_factor_gt 0.1234 _refine_ls_goodness_of_fit_ref 1.276 _refine_ls_restrained_S_all 1.276 _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 Mn1 Mn 0.69348(2) 0.09712(3) 0.04774(3) 0.00829(10) Uani 1 1 d . . . O3 O 0.68664(12) 0.24285(14) 0.10226(15) 0.0138(4) Uani 1 1 d . . . H31 H 0.704(2) 0.250(2) 0.153(3) 0.017 Uiso 1 1 d . . . H32 H 0.6954(19) 0.282(3) 0.072(3) 0.017 Uiso 1 1 d . . . N1 N 0.71665(12) 0.05001(16) 0.17442(15) 0.0117(4) Uani 1 1 d . . . N2 N 0.59566(12) 0.08055(15) 0.08423(16) 0.0121(4) Uani 1 1 d . . . C1 C 0.91108(15) 0.0728(2) 0.0164(2) 0.0193(6) Uani 1 1 d . . . H1A H 0.9214 0.1367 -0.0001 0.029 Uiso 1 1 calc R . . H1B H 0.9073 0.0354 -0.0403 0.029 Uiso 1 1 calc R . . H1C H 0.9489 0.0487 0.0576 0.029 Uiso 1 1 calc R . . C2 C 0.84288(14) 0.06902(19) 0.06525(18) 0.0120(5) Uani 1 1 d . . . C3 C 0.83846(15) 0.0256(2) 0.14903(19) 0.0159(6) Uani 1 1 d . . . H3A H 0.8796 -0.0049 0.1725 0.019 Uiso 1 1 calc R . . C4 C 0.77821(16) 0.0213(2) 0.20494(19) 0.0144(5) Uani 1 1 d . . . C5 C 0.78915(17) -0.0160(2) 0.3021(2) 0.0218(7) Uani 1 1 d . . . H5A H 0.7562 -0.0667 0.3116 0.033 Uiso 1 1 calc R . . H5B H 0.7809 0.0330 0.3473 0.033 Uiso 1 1 calc R . . H5C H 0.8374 -0.0386 0.3109 0.033 Uiso 1 1 calc R . . C6 C 0.65477(15) 0.0484(2) 0.23279(19) 0.0161(6) Uani 1 1 d . . . H6A H 0.6485 0.1091 0.2626 0.019 Uiso 1 1 calc R . . H6B H 0.6609 0.0013 0.2822 0.019 Uiso 1 1 calc R . . C7 C 0.59137(15) 0.0255(2) 0.1697(2) 0.0173(6) Uani 1 1 d . . . H7A H 0.5911 -0.0409 0.1543 0.021 Uiso 1 1 calc R . . H7B H 0.5476 0.0402 0.2014 0.021 Uiso 1 1 calc R . . C8 C 0.46809(16) 0.1035(3) 0.0793(3) 0.0303(8) Uani 1 1 d . . . H8A H 0.4588 0.0378 0.0884 0.045 Uiso 1 1 calc R . . H8B H 0.4326 0.1293 0.0355 0.045 Uiso 1 1 calc R . . H8C H 0.4662 0.1356 0.1391 0.045 Uiso 1 1 calc R . . C9 C 0.54004(15) 0.1154(2) 0.0408(2) 0.0176(6) Uani 1 1 d . . . C10 C 0.54373(16) 0.1642(2) -0.0445(2) 0.0233(7) Uani 1 1 d . . . H10A H 0.5017 0.1923 -0.0684 0.028 Uiso 1 1 calc R . . C11 C 0.60269(16) 0.17444(19) -0.0956(2) 0.0164(6) Uani 1 1 d . . . C12 C 0.59960(19) 0.2236(2) -0.1876(2) 0.0250(7) Uani 1 1 d . . . H12A H 0.6347 0.2729 -0.1867 0.038 Uiso 1 1 calc R . . H12B H 0.5527 0.2501 -0.1987 0.038 Uiso 1 1 calc R . . H12C H 0.6093 0.1799 -0.2374 0.038 Uiso 1 1 calc R . . O1 O 0.79055(10) 0.11160(13) 0.02144(13) 0.0124(4) Uani 1 1 d . . . O2 O 0.66464(11) 0.14266(14) -0.07167(13) 0.0137(4) Uani 1 1 d . . . Fe1 Fe 0.76135(7) -0.2459(2) 0.0007(2) 0.0089(3) Uani 0.50 1 d P . . N21 N 0.69791(12) -0.05026(16) -0.00348(16) 0.0134(5) Uani 1 1 d . . . C21 C 0.71672(14) -0.12530(19) -0.00278(18) 0.0115(5) Uani 1 1 d . . . C31 C 0.6654(5) -0.2911(7) 0.0191(6) 0.0161(8) Uiso 0.50 1 d P . . N31 N 0.6089(4) -0.3185(5) 0.0343(5) 0.0282(9) Uiso 0.50 1 d P . . N51 N 0.8411(4) -0.2057(6) -0.0037(5) 0.0161(8) Uiso 0.50 1 d P . . O51 O 0.8961(3) -0.1770(4) -0.0041(4) 0.0282(9) Uiso 0.50 1 d P . . C41 C 0.76063(18) -0.2429(2) 0.1338(2) 0.0192(6) Uani 1 1 d . . . N41 N 0.76679(19) -0.2388(2) 0.21331(19) 0.0315(7) Uani 1 1 d . . . O1S O 0.5510(3) 0.2479(4) 0.1988(5) 0.0442(15) Uani 0.50 1 d P . . C1S C 0.5352(3) 0.3304(4) 0.2295(5) 0.081(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 Mn1 0.00903(18) 0.00896(18) 0.00697(18) 0.00126(14) 0.00127(13) 0.00150(15) O3 0.0212(11) 0.0107(9) 0.0095(9) 0.0016(7) -0.0002(8) -0.0011(8) N1 0.0138(11) 0.0125(11) 0.0090(10) 0.0012(8) 0.0028(8) 0.0006(9) N2 0.0128(11) 0.0105(11) 0.0130(11) -0.0004(8) 0.0019(9) -0.0014(9) C1 0.0137(14) 0.0267(16) 0.0177(14) 0.0005(12) 0.0018(11) 0.0022(12) C2 0.0119(12) 0.0138(12) 0.0102(12) -0.0028(9) 0.0008(10) 0.0006(10) C3 0.0144(13) 0.0217(14) 0.0114(13) 0.0031(10) -0.0015(10) 0.0061(11) C4 0.0205(14) 0.0152(13) 0.0074(12) -0.0006(10) -0.0002(10) 0.0020(11) C5 0.0230(16) 0.0320(17) 0.0102(13) 0.0073(12) -0.0003(11) 0.0086(13) C6 0.0166(14) 0.0213(14) 0.0106(13) 0.0029(10) 0.0049(10) 0.0010(11) C7 0.0158(14) 0.0205(14) 0.0161(14) 0.0033(11) 0.0059(11) -0.0017(11) C8 0.0103(14) 0.0357(19) 0.045(2) 0.0110(17) 0.0012(14) 0.0003(14) C9 0.0114(13) 0.0148(14) 0.0267(16) 0.0010(11) 0.0003(11) -0.0006(11) C10 0.0123(14) 0.0260(16) 0.0312(18) 0.0099(13) -0.0062(12) 0.0014(12) C11 0.0214(15) 0.0104(12) 0.0167(14) 0.0001(10) -0.0070(11) -0.0011(11) C12 0.0308(18) 0.0246(16) 0.0188(16) 0.0071(12) -0.0104(13) 0.0003(14) O1 0.0131(9) 0.0126(9) 0.0116(9) 0.0023(7) 0.0009(7) 0.0011(7) O2 0.0177(10) 0.0156(10) 0.0076(9) 0.0003(7) -0.0001(7) 0.0042(8) Fe1 0.0124(11) 0.0081(5) 0.0061(3) -0.0006(3) 0.0000(9) 0.0024(8) N21 0.0131(11) 0.0131(11) 0.0140(11) -0.0014(9) 0.0015(9) 0.0011(9) C21 0.0131(12) 0.0136(12) 0.0078(12) 0.0006(9) 0.0009(9) -0.0009(10) C41 0.0332(18) 0.0112(13) 0.0133(14) 0.0014(10) -0.0004(12) 0.0079(12) N41 0.056(2) 0.0258(15) 0.0125(14) 0.0000(11) -0.0027(13) 0.0104(14) O1S 0.031(3) 0.032(3) 0.072(4) -0.012(3) 0.030(3) -0.003(2) C1S 0.080(4) 0.040(3) 0.127(6) -0.018(3) 0.072(4) -0.016(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 Mn1 O2 1.9004(19) . ? Mn1 O1 1.915(2) . ? Mn1 N2 1.972(2) . ? Mn1 N1 1.979(2) . ? Mn1 O3 2.263(2) . ? Mn1 N21 2.267(2) . ? O3 H31 0.79(4) . ? O3 H32 0.75(4) . ? N1 C4 1.305(4) . ? N1 C6 1.475(3) . ? N2 C9 1.311(4) . ? N2 C7 1.471(4) . ? C1 C2 1.504(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 O1 1.313(3) . ? C2 C3 1.366(4) . ? C3 C4 1.429(4) . ? C3 H3A 0.9500 . ? C4 C5 1.505(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.518(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.510(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.421(4) . ? C10 C11 1.376(4) . ? C10 H10A 0.9500 . ? C11 O2 1.301(4) . ? C11 C12 1.501(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? Fe1 Fe1 0.448(2) 7_645 ? Fe1 C31 1.534(9) 7_645 ? Fe1 N51 1.632(8) . ? Fe1 C41 1.914(4) . ? Fe1 C21 1.917(4) 7_645 ? Fe1 C21 1.947(4) . ? Fe1 C41 1.969(4) 7_645 ? Fe1 C31 1.971(10) . ? Fe1 N51 2.078(8) 7_645 ? N21 C21 1.147(4) . ? C21 Fe1 1.917(4) 7_645 ? C31 N51 0.254(14) 7_645 ? C31 N31 1.176(12) . ? C31 O51 1.271(11) 7_645 ? C31 Fe1 1.534(9) 7_645 ? N31 O51 0.445(9) 7_645 ? N31 N51 1.122(11) 7_645 ? N51 C31 0.254(14) 7_645 ? N51 N31 1.122(11) 7_645 ? N51 O51 1.129(9) . ? N51 Fe1 2.078(8) 7_645 ? O51 N31 0.445(9) 7_645 ? O51 C31 1.271(11) 7_645 ? C41 N41 1.146(4) . ? C41 Fe1 1.969(4) 7_645 ? O1S C1S 1.318(7) . ? C1S C1S 1.489(10) 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 O2 Mn1 O1 91.72(8) . . ? O2 Mn1 N2 92.33(9) . . ? O1 Mn1 N2 175.88(9) . . ? O2 Mn1 N1 176.05(9) . . ? O1 Mn1 N1 92.19(9) . . ? N2 Mn1 N1 83.75(10) . . ? O2 Mn1 O3 88.21(8) . . ? O1 Mn1 O3 92.03(8) . . ? N2 Mn1 O3 87.35(9) . . ? N1 Mn1 O3 91.06(9) . . ? O2 Mn1 N21 92.77(9) . . ? O1 Mn1 N21 89.46(8) . . ? N2 Mn1 N21 91.10(9) . . ? N1 Mn1 N21 87.85(9) . . ? O3 Mn1 N21 178.19(8) . . ? Mn1 O3 H31 114(3) . . ? Mn1 O3 H32 120(3) . . ? H31 O3 H32 111(4) . . ? C4 N1 C6 122.2(2) . . ? C4 N1 Mn1 125.77(19) . . ? C6 N1 Mn1 112.05(18) . . ? C9 N2 C7 122.5(2) . . ? C9 N2 Mn1 125.5(2) . . ? C7 N2 Mn1 111.93(18) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 124.6(3) . . ? O1 C2 C1 114.4(2) . . ? C3 C2 C1 121.0(3) . . ? C2 C3 C4 126.6(3) . . ? C2 C3 H3A 116.7 . . ? C4 C3 H3A 116.7 . . ? N1 C4 C3 121.9(3) . . ? N1 C4 C5 121.1(3) . . ? C3 C4 C5 117.0(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C7 107.4(2) . . ? N1 C6 H6A 110.2 . . ? C7 C6 H6A 110.2 . . ? N1 C6 H6B 110.2 . . ? C7 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? N2 C7 C6 108.1(2) . . ? N2 C7 H7A 110.1 . . ? C6 C7 H7A 110.1 . . ? N2 C7 H7B 110.1 . . ? C6 C7 H7B 110.1 . . ? H7A C7 H7B 108.4 . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C9 C10 122.5(3) . . ? N2 C9 C8 120.7(3) . . ? C10 C9 C8 116.8(3) . . ? C11 C10 C9 125.8(3) . . ? C11 C10 H10A 117.1 . . ? C9 C10 H10A 117.1 . . ? O2 C11 C10 124.9(3) . . ? O2 C11 C12 113.9(3) . . ? C10 C11 C12 121.2(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C2 O1 Mn1 125.10(17) . . ? C11 O2 Mn1 126.10(19) . . ? Fe1 Fe1 C31 165.5(10) 7_645 7_645 ? Fe1 Fe1 N51 172.5(10) 7_645 . ? C31 Fe1 N51 8.5(5) 7_645 . ? Fe1 Fe1 C41 90.5(8) 7_645 . ? C31 Fe1 C41 102.8(4) 7_645 . ? N51 Fe1 C41 94.3(3) . . ? Fe1 Fe1 C21 87.2(8) 7_645 7_645 ? C31 Fe1 C21 98.4(4) 7_645 7_645 ? N51 Fe1 C21 98.5(3) . 7_645 ? C41 Fe1 C21 91.01(18) . 7_645 ? Fe1 Fe1 C21 79.5(8) 7_645 . ? C31 Fe1 C21 94.6(4) 7_645 . ? N51 Fe1 C21 94.8(3) . . ? C41 Fe1 C21 89.11(17) . . ? C21 Fe1 C21 166.70(7) 7_645 . ? Fe1 Fe1 C41 76.4(8) 7_645 7_645 ? C31 Fe1 C41 90.3(4) 7_645 7_645 ? N51 Fe1 C41 98.8(3) . 7_645 ? C41 Fe1 C41 166.84(7) . 7_645 ? C21 Fe1 C41 88.38(17) 7_645 7_645 ? C21 Fe1 C41 88.49(17) . 7_645 ? Fe1 Fe1 C31 11.2(8) 7_645 . ? C31 Fe1 C31 176.7(2) 7_645 . ? N51 Fe1 C31 174.4(5) . . ? C41 Fe1 C31 80.2(3) . . ? C21 Fe1 C31 82.8(3) 7_645 . ? C21 Fe1 C31 84.1(3) . . ? C41 Fe1 C31 86.7(3) 7_645 . ? Fe1 Fe1 N51 5.9(8) 7_645 7_645 ? C31 Fe1 N51 170.4(5) 7_645 7_645 ? N51 Fe1 N51 178.4(2) . 7_645 ? C41 Fe1 N51 86.7(2) . 7_645 ? C21 Fe1 N51 82.7(3) 7_645 7_645 ? C21 Fe1 N51 84.0(2) . 7_645 ? C41 Fe1 N51 80.1(2) 7_645 7_645 ? C31 Fe1 N51 6.5(4) . 7_645 ? C21 N21 Mn1 155.5(2) . . ? N21 C21 Fe1 174.4(3) . 7_645 ? N21 C21 Fe1 172.3(3) . . ? Fe1 C21 Fe1 13.30(7) 7_645 . ? N51 C31 N31 72(4) 7_645 . ? N51 C31 O51 51(4) 7_645 7_645 ? N31 C31 O51 20.5(4) . 7_645 ? N51 C31 Fe1 108(4) 7_645 7_645 ? N31 C31 Fe1 179.2(9) . 7_645 ? O51 C31 Fe1 159.5(7) 7_645 7_645 ? N51 C31 Fe1 111(4) 7_645 . ? N31 C31 Fe1 177.0(7) . . ? O51 C31 Fe1 162.5(7) 7_645 . ? Fe1 C31 Fe1 3.3(2) 7_645 . ? O51 N31 N51 79.5(15) 7_645 7_645 ? O51 N31 C31 91.9(16) 7_645 . ? N51 N31 C31 12.4(7) 7_645 . ? C31 N51 N31 96(4) 7_645 7_645 ? C31 N51 O51 119(4) 7_645 . ? N31 N51 O51 22.8(5) 7_645 . ? C31 N51 Fe1 63(4) 7_645 . ? N31 N51 Fe1 159.1(7) 7_645 . ? O51 N51 Fe1 178.0(7) . . ? C31 N51 Fe1 62(4) 7_645 7_645 ? N31 N51 Fe1 158.1(7) 7_645 7_645 ? O51 N51 Fe1 178.0(7) . 7_645 ? Fe1 N51 Fe1 1.6(2) . 7_645 ? N31 O51 N51 77.7(15) 7_645 . ? N31 O51 C31 67.6(15) 7_645 7_645 ? N51 O51 C31 10.1(7) . 7_645 ? N41 C41 Fe1 173.5(3) . . ? N41 C41 Fe1 173.3(3) . 7_645 ? Fe1 C41 Fe1 13.16(7) . 7_645 ? O1S C1S C1S 110.8(4) . 2_655 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Mn1 N1 C4 173.8(12) . . . . ? O1 Mn1 N1 C4 -14.8(2) . . . . ? N2 Mn1 N1 C4 165.9(2) . . . . ? O3 Mn1 N1 C4 -106.9(2) . . . . ? N21 Mn1 N1 C4 74.6(2) . . . . ? O2 Mn1 N1 C6 -4.8(15) . . . . ? O1 Mn1 N1 C6 166.58(19) . . . . ? N2 Mn1 N1 C6 -12.70(19) . . . . ? O3 Mn1 N1 C6 74.51(19) . . . . ? N21 Mn1 N1 C6 -104.04(19) . . . . ? O2 Mn1 N2 C9 -14.3(2) . . . . ? O1 Mn1 N2 C9 155.1(12) . . . . ? N1 Mn1 N2 C9 165.2(3) . . . . ? O3 Mn1 N2 C9 73.8(2) . . . . ? N21 Mn1 N2 C9 -107.1(2) . . . . ? O2 Mn1 N2 C7 167.49(19) . . . . ? O1 Mn1 N2 C7 -23.1(14) . . . . ? N1 Mn1 N2 C7 -13.05(19) . . . . ? O3 Mn1 N2 C7 -104.41(19) . . . . ? N21 Mn1 N2 C7 74.67(19) . . . . ? O1 C2 C3 C4 -2.4(5) . . . . ? C1 C2 C3 C4 176.4(3) . . . . ? C6 N1 C4 C3 -178.1(3) . . . . ? Mn1 N1 C4 C3 3.4(4) . . . . ? C6 N1 C4 C5 0.4(4) . . . . ? Mn1 N1 C4 C5 -178.1(2) . . . . ? C2 C3 C4 N1 9.1(5) . . . . ? C2 C3 C4 C5 -169.5(3) . . . . ? C4 N1 C6 C7 -144.2(3) . . . . ? Mn1 N1 C6 C7 34.5(3) . . . . ? C9 N2 C7 C6 -143.3(3) . . . . ? Mn1 N2 C7 C6 35.0(3) . . . . ? N1 C6 C7 N2 -44.3(3) . . . . ? C7 N2 C9 C10 -176.4(3) . . . . ? Mn1 N2 C9 C10 5.5(4) . . . . ? C7 N2 C9 C8 2.4(4) . . . . ? Mn1 N2 C9 C8 -175.6(2) . . . . ? N2 C9 C10 C11 5.9(5) . . . . ? C8 C9 C10 C11 -173.0(3) . . . . ? C9 C10 C11 O2 -2.0(5) . . . . ? C9 C10 C11 C12 176.8(3) . . . . ? C3 C2 O1 Mn1 -16.3(4) . . . . ? C1 C2 O1 Mn1 164.87(19) . . . . ? O2 Mn1 O1 C2 -159.6(2) . . . . ? N2 Mn1 O1 C2 31.0(14) . . . . ? N1 Mn1 O1 C2 20.9(2) . . . . ? O3 Mn1 O1 C2 112.1(2) . . . . ? N21 Mn1 O1 C2 -66.9(2) . . . . ? C10 C11 O2 Mn1 -13.3(4) . . . . ? C12 C11 O2 Mn1 167.8(2) . . . . ? O1 Mn1 O2 C11 -161.2(2) . . . . ? N2 Mn1 O2 C11 18.0(2) . . . . ? N1 Mn1 O2 C11 10.2(15) . . . . ? O3 Mn1 O2 C11 -69.3(2) . . . . ? N21 Mn1 O2 C11 109.2(2) . . . . ? O2 Mn1 N21 C21 154.5(5) . . . . ? O1 Mn1 N21 C21 62.8(5) . . . . ? N2 Mn1 N21 C21 -113.1(5) . . . . ? N1 Mn1 N21 C21 -29.4(5) . . . . ? O3 Mn1 N21 C21 -83(3) . . . . ? Mn1 N21 C21 Fe1 123(2) . . . 7_645 ? Mn1 N21 C21 Fe1 -46(2) . . . . ? Fe1 Fe1 C21 N21 175.2(18) 7_645 . . . ? C31 Fe1 C21 N21 -18(2) 7_645 . . . ? N51 Fe1 C21 N21 -9.6(19) . . . . ? C41 Fe1 C21 N21 84.6(19) . . . . ? C21 Fe1 C21 N21 175.2(18) 7_645 . . . ? C41 Fe1 C21 N21 -108.3(19) 7_645 . . . ? C31 Fe1 C21 N21 164.8(19) . . . . ? N51 Fe1 C21 N21 171.4(19) 7_645 . . . ? C31 Fe1 C21 Fe1 166.6(10) 7_645 . . 7_645 ? N51 Fe1 C21 Fe1 175.1(10) . . . 7_645 ? C41 Fe1 C21 Fe1 -90.6(8) . . . 7_645 ? C21 Fe1 C21 Fe1 0.0 7_645 . . 7_645 ? C41 Fe1 C21 Fe1 76.4(8) 7_645 . . 7_645 ? C31 Fe1 C21 Fe1 -10.4(8) . . . 7_645 ? N51 Fe1 C21 Fe1 -3.8(8) 7_645 . . 7_645 ? Fe1 Fe1 C31 N51 24(5) 7_645 . . 7_645 ? C31 Fe1 C31 N51 24(5) 7_645 . . 7_645 ? N51 Fe1 C31 N51 167(3) . . . 7_645 ? C41 Fe1 C31 N51 179(4) . . . 7_645 ? C21 Fe1 C31 N51 -89(4) 7_645 . . 7_645 ? C21 Fe1 C31 N51 89(4) . . . 7_645 ? C41 Fe1 C31 N51 0(4) 7_645 . . 7_645 ? Fe1 Fe1 C31 N31 -167(17) 7_645 . . . ? C31 Fe1 C31 N31 -167(17) 7_645 . . . ? N51 Fe1 C31 N31 -23(20) . . . . ? C41 Fe1 C31 N31 -11(16) . . . . ? C21 Fe1 C31 N31 81(16) 7_645 . . . ? C21 Fe1 C31 N31 -101(16) . . . . ? C41 Fe1 C31 N31 170(16) 7_645 . . . ? N51 Fe1 C31 N31 170(19) 7_645 . . . ? Fe1 Fe1 C31 O51 29(4) 7_645 . . 7_645 ? C31 Fe1 C31 O51 29(4) 7_645 . . 7_645 ? N51 Fe1 C31 O51 173(4) . . . 7_645 ? C41 Fe1 C31 O51 -176(3) . . . 7_645 ? C21 Fe1 C31 O51 -83(2) 7_645 . . 7_645 ? C21 Fe1 C31 O51 94(2) . . . 7_645 ? C41 Fe1 C31 O51 6(2) 7_645 . . 7_645 ? N51 Fe1 C31 O51 5(2) 7_645 . . 7_645 ? C31 Fe1 C31 Fe1 0.00(8) 7_645 . . 7_645 ? N51 Fe1 C31 Fe1 144(7) . . . 7_645 ? C41 Fe1 C31 Fe1 156(4) . . . 7_645 ? C21 Fe1 C31 Fe1 -112(4) 7_645 . . 7_645 ? C21 Fe1 C31 Fe1 65(4) . . . 7_645 ? C41 Fe1 C31 Fe1 -23(4) 7_645 . . 7_645 ? N51 Fe1 C31 Fe1 -24(5) 7_645 . . 7_645 ? N51 C31 N31 O51 3(4) 7_645 . . 7_645 ? Fe1 C31 N31 O51 93(58) 7_645 . . 7_645 ? Fe1 C31 N31 O51 -167(15) . . . 7_645 ? O51 C31 N31 N51 -3(4) 7_645 . . 7_645 ? Fe1 C31 N31 N51 89(58) 7_645 . . 7_645 ? Fe1 C31 N31 N51 -170(19) . . . 7_645 ? Fe1 Fe1 N51 C31 -49(9) 7_645 . . 7_645 ? C41 Fe1 N51 C31 -178(4) . . . 7_645 ? C21 Fe1 N51 C31 90(4) 7_645 . . 7_645 ? C21 Fe1 N51 C31 -89(4) . . . 7_645 ? C41 Fe1 N51 C31 0(4) 7_645 . . 7_645 ? C31 Fe1 N51 C31 -167(3) . . . 7_645 ? N51 Fe1 N51 C31 -49(9) 7_645 . . 7_645 ? Fe1 Fe1 N51 N31 -51(8) 7_645 . . 7_645 ? C31 Fe1 N51 N31 -2(3) 7_645 . . 7_645 ? C41 Fe1 N51 N31 179(2) . . . 7_645 ? C21 Fe1 N51 N31 88(2) 7_645 . . 7_645 ? C21 Fe1 N51 N31 -91(2) . . . 7_645 ? C41 Fe1 N51 N31 -2(2) 7_645 . . 7_645 ? C31 Fe1 N51 N31 -169(4) . . . 7_645 ? N51 Fe1 N51 N31 -51(9) 7_645 . . 7_645 ? Fe1 Fe1 N51 O51 112(23) 7_645 . . . ? C31 Fe1 N51 O51 161(26) 7_645 . . . ? C41 Fe1 N51 O51 -17(23) . . . . ? C21 Fe1 N51 O51 -109(23) 7_645 . . . ? C21 Fe1 N51 O51 73(23) . . . . ? C41 Fe1 N51 O51 162(23) 7_645 . . . ? C31 Fe1 N51 O51 -5(28) . . . . ? N51 Fe1 N51 O51 112(24) 7_645 . . . ? C31 Fe1 N51 Fe1 49(9) 7_645 . . 7_645 ? C41 Fe1 N51 Fe1 -129(8) . . . 7_645 ? C21 Fe1 N51 Fe1 139(8) 7_645 . . 7_645 ? C21 Fe1 N51 Fe1 -40(7) . . . 7_645 ? C41 Fe1 N51 Fe1 49(7) 7_645 . . 7_645 ? C31 Fe1 N51 Fe1 -118(11) . . . 7_645 ? N51 Fe1 N51 Fe1 0.0(4) 7_645 . . 7_645 ? C31 N51 O51 N31 -4(5) 7_645 . . 7_645 ? Fe1 N51 O51 N31 -165(23) . . . 7_645 ? Fe1 N51 O51 N31 -118(19) 7_645 . . 7_645 ? N31 N51 O51 C31 4(5) 7_645 . . 7_645 ? Fe1 N51 O51 C31 -161(27) . . . 7_645 ? Fe1 N51 O51 C31 -114(22) 7_645 . . 7_645 ? Fe1 Fe1 C41 N41 179(100) 7_645 . . . ? C31 Fe1 C41 N41 -7(3) 7_645 . . . ? N51 Fe1 C41 N41 -7(3) . . . . ? C21 Fe1 C41 N41 92(3) 7_645 . . . ? C21 Fe1 C41 N41 -102(3) . . . . ? C41 Fe1 C41 N41 179(100) 7_645 . . . ? C31 Fe1 C41 N41 174(3) . . . . ? N51 Fe1 C41 N41 174(3) 7_645 . . . ? C31 Fe1 C41 Fe1 174.0(10) 7_645 . . 7_645 ? N51 Fe1 C41 Fe1 174.2(9) . . . 7_645 ? C21 Fe1 C41 Fe1 -87.2(8) 7_645 . . 7_645 ? C21 Fe1 C41 Fe1 79.5(8) . . . 7_645 ? C41 Fe1 C41 Fe1 0.000(2) 7_645 . . 7_645 ? C31 Fe1 C41 Fe1 -4.6(8) . . . 7_645 ? N51 Fe1 C41 Fe1 -4.5(7) 7_645 . . 7_645 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H31 N41 0.79(4) 1.99(4) 2.775(4) 172(4) 4_655 O3 H32 O1 0.75(4) 2.06(4) 2.808(3) 174(4) 7_655 _diffrn_measured_fraction_theta_max 0.832 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.901 _refine_diff_density_min -0.750 _refine_diff_density_rms 0.095 #= END of data for compound 2 data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 849759' #TrackingRef '- deposit_NEW.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C53 H80 Fe Mn4 N14 O13, C5 Fe N6 O, 4(C2 H3 N)' _chemical_formula_structural '[{Mn(C12 H18 N2 O2)(H2 O)}4(Fe(N O)(C N)5)][Fe(N O)(CN)5]*4(C H3 C N)' _chemical_formula_sum 'C66 H92 Fe2 Mn4 N24 O14' _chemical_formula_weight 1777.10 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 tetragonal _symmetry_space_group_name_H-M P4/n _symmetry_space_group_name_Hall '-P 4a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' _cell_length_a 20.6997(4) _cell_length_b 20.6997(4) _cell_length_c 9.9205(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4250.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9856 _cell_measurement_theta_min 2.2765 _cell_measurement_theta_max 29.2615 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1840 _exptl_absorpt_coefficient_mu 0.979 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.851117 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'based on intensities (SADABS, Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8Apex CCD detector' _diffrn_measurement_method 'combined omega- and phi-scans' _diffrn_detector_area_resol_mean 25 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28719 _diffrn_reflns_av_R_equivalents 0.0196 _diffrn_reflns_av_sigmaI/netI 0.0165 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 29.66 _reflns_number_total 5309 _reflns_number_gt 4574 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 V.1.27 (Bruker, 2005)' _computing_cell_refinement 'Apex2 V.1.27 (Bruker, 2005)' _computing_data_reduction 'Apex2 V.1.27 (Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V6.22 (Bruker, 2000-2005)' _computing_publication_material 'local programs' _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^)+(0.0306P)^2^+2.4027P] 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 5309 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0731 _refine_ls_wR_factor_gt 0.0690 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _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 Mn1 Mn 0.901721(10) 0.564674(10) 0.94922(2) 0.01710(6) Uani 1 1 d . . . Fe1 Fe 0.7500 0.7500 1.07140(4) 0.01673(9) Uani 1 4 d S . . N13 N 0.87100(6) 0.66566(6) 1.03150(14) 0.0232(3) Uani 1 1 d . . . C13 C 0.82693(7) 0.69794(7) 1.05067(15) 0.0196(3) Uani 1 1 d . . . O4 O 0.7500 0.7500 1.3541(3) 0.0475(7) Uani 1 4 d S . . N4 N 0.7500 0.7500 1.2385(3) 0.0245(5) Uani 1 4 d S . . N15 N 0.7500 0.7500 0.7597(3) 0.0262(6) Uani 1 4 d S . . C15 C 0.7500 0.7500 0.8754(3) 0.0189(5) Uani 1 4 d S . . O1 O 0.98181(5) 0.59540(5) 0.88191(11) 0.0217(2) Uani 1 1 d . . . O2 O 0.93995(5) 0.54874(5) 1.12106(10) 0.0199(2) Uani 1 1 d . . . O3 O 0.92593(5) 0.46427(5) 0.87946(12) 0.0232(2) Uani 1 1 d . . . H32 H 0.9632(12) 0.4574(11) 0.885(2) 0.050 Uiso 1 1 d . . . H31 H 0.9071(11) 0.4346(12) 0.922(2) 0.050 Uiso 1 1 d . . . N1 N 0.85629(6) 0.58499(6) 0.77984(13) 0.0216(3) Uani 1 1 d . . . N2 N 0.81725(6) 0.53079(6) 1.00716(13) 0.0197(2) Uani 1 1 d . . . C1 C 1.06267(8) 0.63998(8) 0.74250(18) 0.0292(3) Uani 1 1 d . . . H1A H 1.0777 0.6661 0.8186 0.044 Uiso 1 1 calc R . . H1B H 1.0661 0.6652 0.6592 0.044 Uiso 1 1 calc R . . H1C H 1.0893 0.6010 0.7351 0.044 Uiso 1 1 calc R . . C2 C 0.99335(7) 0.62097(7) 0.76488(16) 0.0223(3) Uani 1 1 d . . . C3 C 0.94758(8) 0.63150(7) 0.66726(16) 0.0248(3) Uani 1 1 d . . . H3A H 0.9617 0.6515 0.5862 0.030 Uiso 1 1 calc R . . C4 C 0.88093(8) 0.61529(7) 0.67618(15) 0.0235(3) Uani 1 1 d . . . C5 C 0.83816(9) 0.63542(9) 0.56020(17) 0.0322(4) Uani 1 1 d . . . H5A H 0.8177 0.5971 0.5209 0.048 Uiso 1 1 calc R . . H5B H 0.8643 0.6572 0.4915 0.048 Uiso 1 1 calc R . . H5C H 0.8047 0.6650 0.5930 0.048 Uiso 1 1 calc R . . C6 C 0.78617(7) 0.57225(8) 0.78801(17) 0.0263(3) Uani 1 1 d . . . H6A H 0.7697 0.5585 0.6988 0.032 Uiso 1 1 calc R . . H6B H 0.7631 0.6121 0.8148 0.032 Uiso 1 1 calc R . . C7 C 0.77434(7) 0.51969(7) 0.89097(17) 0.0247(3) Uani 1 1 d . . . H7A H 0.7287 0.5205 0.9205 0.030 Uiso 1 1 calc R . . H7B H 0.7833 0.4769 0.8507 0.030 Uiso 1 1 calc R . . C8 C 0.73562(7) 0.48511(8) 1.15879(19) 0.0296(3) Uani 1 1 d . . . H8A H 0.7018 0.5160 1.1334 0.044 Uiso 1 1 calc R . . H8B H 0.7324 0.4755 1.2553 0.044 Uiso 1 1 calc R . . H8C H 0.7302 0.4452 1.1070 0.044 Uiso 1 1 calc R . . C9 C 0.80122(7) 0.51393(7) 1.12889(16) 0.0218(3) Uani 1 1 d . . . C10 C 0.84458(7) 0.52030(7) 1.24039(16) 0.0242(3) Uani 1 1 d . . . H10A H 0.8273 0.5134 1.3279 0.029 Uiso 1 1 calc R . . C11 C 0.90896(7) 0.53544(7) 1.23206(16) 0.0216(3) Uani 1 1 d . . . C12 C 0.95052(8) 0.53584(8) 1.35612(16) 0.0292(3) Uani 1 1 d . . . H12A H 0.9682 0.5793 1.3700 0.044 Uiso 1 1 calc R . . H12B H 0.9861 0.5050 1.3449 0.044 Uiso 1 1 calc R . . H12C H 0.9245 0.5235 1.4345 0.044 Uiso 1 1 calc R . . Fe2 Fe 0.7500 0.2500 0.97269(6) 0.0200(2) Uani 0.50 2 d SP . . C21 C 0.7500 0.2500 0.8183(3) 0.0403(6) Uani 0.50 2 d SP A 1 N21 N 0.7500 0.2500 0.7020(3) 0.0804(10) Uani 0.50 2 d SP A 1 N21N N 0.7500 0.2500 0.8183(3) 0.0403(6) Uani 0.50 2 d SP A 2 O21N O 0.7500 0.2500 0.7020(3) 0.0804(10) Uani 0.50 2 d SP A 2 N22 N 0.83943(7) 0.36852(7) 0.97995(18) 0.0351(3) Uani 1 1 d . . . C22 C 0.80602(8) 0.32475(7) 0.99264(19) 0.0296(3) Uani 1 1 d . A . N1S N 0.78225(12) 0.44887(13) 0.5357(2) 0.0668(6) Uani 1 1 d . . . C1S C 0.81857(12) 0.41138(12) 0.5730(2) 0.0509(5) Uani 1 1 d . . . C2S C 0.86510(14) 0.36464(13) 0.6236(3) 0.0659(7) Uani 1 1 d . . . H2S1 H 0.8546 0.3538 0.7172 0.099 Uiso 1 1 calc R . . H2S2 H 0.9086 0.3832 0.6194 0.099 Uiso 1 1 calc R . . H2S3 H 0.8634 0.3255 0.5682 0.099 Uiso 1 1 calc R . . 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 Mn1 0.01213(10) 0.01493(11) 0.02423(11) -0.00043(8) -0.00196(8) 0.00072(7) Fe1 0.01229(11) 0.01229(11) 0.0256(2) 0.000 0.000 0.000 N13 0.0175(6) 0.0170(6) 0.0351(7) -0.0018(5) -0.0034(5) 0.0005(5) C13 0.0157(6) 0.0146(6) 0.0286(7) 0.0010(5) -0.0031(5) -0.0024(5) O4 0.0571(11) 0.0571(11) 0.0282(14) 0.000 0.000 0.000 N4 0.0203(7) 0.0203(7) 0.0330(14) 0.000 0.000 0.000 N15 0.0212(8) 0.0212(8) 0.0361(15) 0.000 0.000 0.000 C15 0.0141(8) 0.0141(8) 0.0285(15) 0.000 0.000 0.000 O1 0.0154(5) 0.0203(5) 0.0295(5) 0.0026(4) -0.0005(4) -0.0003(4) O2 0.0149(5) 0.0199(5) 0.0250(5) -0.0008(4) -0.0017(4) 0.0024(4) O3 0.0149(5) 0.0184(5) 0.0364(6) -0.0034(4) -0.0008(4) 0.0016(4) N1 0.0181(6) 0.0192(6) 0.0274(6) -0.0021(5) -0.0041(5) 0.0029(4) N2 0.0136(5) 0.0153(5) 0.0303(6) -0.0031(5) -0.0029(5) 0.0015(4) C1 0.0228(7) 0.0255(8) 0.0392(9) 0.0020(7) 0.0091(7) 0.0013(6) C2 0.0225(7) 0.0135(6) 0.0310(8) -0.0034(6) 0.0055(6) 0.0027(5) C3 0.0284(8) 0.0204(7) 0.0256(7) -0.0016(6) 0.0042(6) 0.0038(6) C4 0.0277(8) 0.0183(7) 0.0245(7) -0.0064(6) -0.0026(6) 0.0070(6) C5 0.0351(9) 0.0345(9) 0.0270(8) -0.0005(7) -0.0048(7) 0.0111(7) C6 0.0173(7) 0.0273(8) 0.0343(8) -0.0009(6) -0.0075(6) 0.0031(6) C7 0.0159(7) 0.0221(7) 0.0361(8) -0.0046(6) -0.0059(6) -0.0014(5) C8 0.0182(7) 0.0263(8) 0.0443(10) 0.0050(7) 0.0041(7) -0.0023(6) C9 0.0168(6) 0.0132(6) 0.0354(8) -0.0015(6) 0.0019(6) 0.0018(5) C10 0.0219(7) 0.0232(7) 0.0274(8) -0.0008(6) 0.0035(6) 0.0021(6) C11 0.0212(7) 0.0167(7) 0.0267(7) -0.0034(6) 0.0000(6) 0.0048(5) C12 0.0266(8) 0.0354(9) 0.0256(8) -0.0054(7) -0.0022(6) 0.0038(6) Fe2 0.0149(3) 0.0147(3) 0.0305(6) 0.000 0.000 0.0001(3) C21 0.0362(13) 0.0360(13) 0.0486(15) 0.000 0.000 -0.0146(10) N21 0.094(2) 0.098(2) 0.0486(16) 0.000 0.000 -0.0456(19) N21N 0.0362(13) 0.0360(13) 0.0486(15) 0.000 0.000 -0.0146(10) O21N 0.094(2) 0.098(2) 0.0486(16) 0.000 0.000 -0.0456(19) N22 0.0241(7) 0.0226(7) 0.0586(10) -0.0029(7) -0.0036(7) -0.0031(5) C22 0.0188(7) 0.0180(7) 0.0520(10) -0.0023(7) -0.0033(7) 0.0020(6) N1S 0.0711(15) 0.0830(16) 0.0465(11) 0.0085(11) 0.0206(10) 0.0013(13) C1S 0.0570(14) 0.0578(14) 0.0379(11) 0.0004(10) 0.0153(10) -0.0099(11) C2S 0.0719(17) 0.0678(17) 0.0581(15) 0.0026(13) 0.0047(13) 0.0019(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 Mn1 O1 1.8970(10) . ? Mn1 O2 1.9082(10) . ? Mn1 N2 1.9697(12) . ? Mn1 N1 1.9710(13) . ? Mn1 O3 2.2471(11) . ? Mn1 N13 2.3325(13) . ? Fe1 N4 1.658(3) . ? Fe1 C13 1.9337(14) 4_565 ? Fe1 C13 1.9337(14) 2_665 ? Fe1 C13 1.9337(14) . ? Fe1 C13 1.9337(14) 3_655 ? Fe1 C15 1.945(3) . ? N13 C13 1.1467(19) . ? O4 N4 1.146(4) . ? N15 C15 1.147(4) . ? O1 C2 1.2982(19) . ? O2 C11 1.3036(18) . ? O3 H32 0.79(2) . ? O3 H31 0.84(3) . ? N1 C4 1.308(2) . ? N1 C6 1.4774(19) . ? N2 C9 1.300(2) . ? N2 C7 1.4732(19) . ? C1 C2 1.504(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.372(2) . ? C3 C4 1.423(2) . ? C3 H3A 0.9500 . ? C4 C5 1.510(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.512(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.512(2) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.431(2) . ? C10 C11 1.371(2) . ? C10 H10A 0.9500 . ? C11 C12 1.502(2) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? Fe2 Fe2 0.5418(12) 7_667 ? Fe2 C21 1.532(3) . ? Fe2 C22 1.9438(16) . ? Fe2 C22 1.9438(16) 2_655 ? Fe2 C22 1.9640(16) 7_667 ? Fe2 C22 1.9640(16) 8_657 ? Fe2 C21 2.073(3) 7_667 ? Fe2 N21N 2.073(3) 7_667 ? C21 N21 1.154(4) . ? C21 Fe2 2.073(3) 7_667 ? N22 C22 1.147(2) . ? C22 Fe2 1.9640(16) 7_667 ? N1S C1S 1.142(3) . ? C1S C2S 1.454(4) . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O2 90.58(4) . . ? O1 Mn1 N2 176.26(5) . . ? O2 Mn1 N2 92.63(5) . . ? O1 Mn1 N1 92.60(5) . . ? O2 Mn1 N1 175.13(5) . . ? N2 Mn1 N1 84.33(5) . . ? O1 Mn1 O3 90.39(4) . . ? O2 Mn1 O3 91.31(4) . . ? N2 Mn1 O3 87.62(5) . . ? N1 Mn1 O3 92.36(5) . . ? O1 Mn1 N13 93.49(4) . . ? O2 Mn1 N13 87.44(4) . . ? N2 Mn1 N13 88.57(5) . . ? N1 Mn1 N13 88.68(5) . . ? O3 Mn1 N13 175.93(5) . . ? N4 Fe1 C13 96.11(5) . 4_565 ? N4 Fe1 C13 96.11(5) . 2_665 ? C13 Fe1 C13 89.352(10) 4_565 2_665 ? N4 Fe1 C13 96.11(5) . . ? C13 Fe1 C13 89.352(10) 4_565 . ? C13 Fe1 C13 167.79(9) 2_665 . ? N4 Fe1 C13 96.11(5) . 3_655 ? C13 Fe1 C13 167.79(9) 4_565 3_655 ? C13 Fe1 C13 89.352(10) 2_665 3_655 ? C13 Fe1 C13 89.352(11) . 3_655 ? N4 Fe1 C15 180.000(2) . . ? C13 Fe1 C15 83.89(5) 4_565 . ? C13 Fe1 C15 83.89(5) 2_665 . ? C13 Fe1 C15 83.89(5) . . ? C13 Fe1 C15 83.89(5) 3_655 . ? C13 N13 Mn1 142.86(11) . . ? N13 C13 Fe1 175.96(14) . . ? O4 N4 Fe1 180.000(2) . . ? N15 C15 Fe1 180.000(1) . . ? C2 O1 Mn1 127.76(10) . . ? C11 O2 Mn1 125.95(9) . . ? Mn1 O3 H32 111.3(17) . . ? Mn1 O3 H31 114.6(16) . . ? H32 O3 H31 107(2) . . ? C4 N1 C6 120.78(13) . . ? C4 N1 Mn1 125.91(10) . . ? C6 N1 Mn1 112.57(10) . . ? C9 N2 C7 122.08(12) . . ? C9 N2 Mn1 126.38(10) . . ? C7 N2 Mn1 111.25(10) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 124.68(14) . . ? O1 C2 C1 114.46(14) . . ? C3 C2 C1 120.86(15) . . ? C2 C3 C4 126.03(15) . . ? C2 C3 H3A 117.0 . . ? C4 C3 H3A 117.0 . . ? N1 C4 C3 122.69(14) . . ? N1 C4 C5 120.17(14) . . ? C3 C4 C5 117.13(15) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C7 108.94(12) . . ? N1 C6 H6A 109.9 . . ? C7 C6 H6A 109.9 . . ? N1 C6 H6B 109.9 . . ? C7 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? N2 C7 C6 108.58(12) . . ? N2 C7 H7A 110.0 . . ? C6 C7 H7A 110.0 . . ? N2 C7 H7B 110.0 . . ? C6 C7 H7B 110.0 . . ? H7A C7 H7B 108.4 . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C9 C10 122.23(13) . . ? N2 C9 C8 121.14(14) . . ? C10 C9 C8 116.62(14) . . ? C11 C10 C9 125.74(15) . . ? C11 C10 H10A 117.1 . . ? C9 C10 H10A 117.1 . . ? O2 C11 C10 125.25(14) . . ? O2 C11 C12 114.16(13) . . ? C10 C11 C12 120.56(14) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Fe2 Fe2 C21 180.000(3) 7_667 . ? Fe2 Fe2 C22 84.16(6) 7_667 . ? C21 Fe2 C22 95.84(6) . . ? Fe2 Fe2 C22 84.16(6) 7_667 2_655 ? C21 Fe2 C22 95.84(6) . 2_655 ? C22 Fe2 C22 168.32(12) . 2_655 ? Fe2 Fe2 C22 79.91(6) 7_667 7_667 ? C21 Fe2 C22 100.09(6) . 7_667 ? C22 Fe2 C22 88.979(7) . 7_667 ? C22 Fe2 C22 88.979(7) 2_655 7_667 ? Fe2 Fe2 C22 79.91(6) 7_667 8_657 ? C21 Fe2 C22 100.09(6) . 8_657 ? C22 Fe2 C22 88.979(7) . 8_657 ? C22 Fe2 C22 88.979(7) 2_655 8_657 ? C22 Fe2 C22 159.83(12) 7_667 8_657 ? Fe2 Fe2 C21 0.000(1) 7_667 7_667 ? C21 Fe2 C21 180.000(1) . 7_667 ? C22 Fe2 C21 84.16(6) . 7_667 ? C22 Fe2 C21 84.16(6) 2_655 7_667 ? C22 Fe2 C21 79.91(6) 7_667 7_667 ? C22 Fe2 C21 79.91(6) 8_657 7_667 ? Fe2 Fe2 N21N 0.000(1) 7_667 7_667 ? C21 Fe2 N21N 180.000(1) . 7_667 ? C22 Fe2 N21N 84.16(6) . 7_667 ? C22 Fe2 N21N 84.16(6) 2_655 7_667 ? C22 Fe2 N21N 79.91(6) 7_667 7_667 ? C22 Fe2 N21N 79.91(6) 8_657 7_667 ? C21 Fe2 N21N 0.000(1) 7_667 7_667 ? N21 C21 Fe2 180.000(1) . . ? N21 C21 Fe2 180.000(1) . 7_667 ? Fe2 C21 Fe2 0.0 . 7_667 ? N22 C22 Fe2 167.85(18) . . ? N22 C22 Fe2 176.18(18) . 7_667 ? Fe2 C22 Fe2 15.93(4) . 7_667 ? N1S C1S C2S 178.6(3) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Mn1 N13 C13 147.8(2) . . . . ? O2 Mn1 N13 C13 -121.8(2) . . . . ? N2 Mn1 N13 C13 -29.1(2) . . . . ? N1 Mn1 N13 C13 55.2(2) . . . . ? O3 Mn1 N13 C13 -49.7(7) . . . . ? Mn1 N13 C13 Fe1 -37(2) . . . . ? N4 Fe1 C13 N13 148.6(19) . . . . ? C13 Fe1 C13 N13 52.5(19) 4_565 . . . ? C13 Fe1 C13 N13 -31.4(19) 2_665 . . . ? C13 Fe1 C13 N13 -115.4(19) 3_655 . . . ? C15 Fe1 C13 N13 -31.4(19) . . . . ? C13 Fe1 N4 O4 0(100) 4_565 . . . ? C13 Fe1 N4 O4 0(100) 2_665 . . . ? C13 Fe1 N4 O4 0(100) . . . . ? C13 Fe1 N4 O4 0(100) 3_655 . . . ? C15 Fe1 N4 O4 0(100) . . . . ? N4 Fe1 C15 N15 0(100) . . . . ? C13 Fe1 C15 N15 -169(100) 4_565 . . . ? C13 Fe1 C15 N15 101(100) 2_665 . . . ? C13 Fe1 C15 N15 -79(100) . . . . ? C13 Fe1 C15 N15 11(100) 3_655 . . . ? O2 Mn1 O1 C2 -174.59(12) . . . . ? N2 Mn1 O1 C2 36.3(8) . . . . ? N1 Mn1 O1 C2 1.72(12) . . . . ? O3 Mn1 O1 C2 94.10(12) . . . . ? N13 Mn1 O1 C2 -87.12(12) . . . . ? O1 Mn1 O2 C11 168.10(11) . . . . ? N2 Mn1 O2 C11 -13.82(12) . . . . ? N1 Mn1 O2 C11 37.4(6) . . . . ? O3 Mn1 O2 C11 -101.49(11) . . . . ? N13 Mn1 O2 C11 74.63(11) . . . . ? O1 Mn1 N1 C4 -5.91(12) . . . . ? O2 Mn1 N1 C4 124.8(5) . . . . ? N2 Mn1 N1 C4 176.22(13) . . . . ? O3 Mn1 N1 C4 -96.41(12) . . . . ? N13 Mn1 N1 C4 87.53(12) . . . . ? O1 Mn1 N1 C6 -176.07(10) . . . . ? O2 Mn1 N1 C6 -45.4(6) . . . . ? N2 Mn1 N1 C6 6.06(10) . . . . ? O3 Mn1 N1 C6 93.43(10) . . . . ? N13 Mn1 N1 C6 -82.64(10) . . . . ? O1 Mn1 N2 C9 156.4(7) . . . . ? O2 Mn1 N2 C9 7.33(12) . . . . ? N1 Mn1 N2 C9 -168.86(13) . . . . ? O3 Mn1 N2 C9 98.53(12) . . . . ? N13 Mn1 N2 C9 -80.04(12) . . . . ? O1 Mn1 N2 C7 -17.5(8) . . . . ? O2 Mn1 N2 C7 -166.54(9) . . . . ? N1 Mn1 N2 C7 17.27(9) . . . . ? O3 Mn1 N2 C7 -75.34(9) . . . . ? N13 Mn1 N2 C7 106.09(10) . . . . ? Mn1 O1 C2 C3 1.2(2) . . . . ? Mn1 O1 C2 C1 -179.59(10) . . . . ? O1 C2 C3 C4 -1.3(2) . . . . ? C1 C2 C3 C4 179.51(14) . . . . ? C6 N1 C4 C3 176.70(13) . . . . ? Mn1 N1 C4 C3 7.3(2) . . . . ? C6 N1 C4 C5 -2.5(2) . . . . ? Mn1 N1 C4 C5 -171.88(11) . . . . ? C2 C3 C4 N1 -3.3(2) . . . . ? C2 C3 C4 C5 175.92(14) . . . . ? C4 N1 C6 C7 162.04(13) . . . . ? Mn1 N1 C6 C7 -27.23(15) . . . . ? C9 N2 C7 C6 149.58(13) . . . . ? Mn1 N2 C7 C6 -36.24(14) . . . . ? N1 C6 C7 N2 40.61(16) . . . . ? C7 N2 C9 C10 175.34(13) . . . . ? Mn1 N2 C9 C10 2.1(2) . . . . ? C7 N2 C9 C8 -3.4(2) . . . . ? Mn1 N2 C9 C8 -176.65(10) . . . . ? N2 C9 C10 C11 -9.7(2) . . . . ? C8 C9 C10 C11 169.12(14) . . . . ? Mn1 O2 C11 C10 11.2(2) . . . . ? Mn1 O2 C11 C12 -170.53(10) . . . . ? C9 C10 C11 O2 2.7(2) . . . . ? C9 C10 C11 C12 -175.41(14) . . . . ? Fe2 Fe2 C22 N22 177.6(7) 7_667 . . . ? C21 Fe2 C22 N22 -2.4(7) . . . . ? C22 Fe2 C22 N22 177.6(7) 2_655 . . . ? C22 Fe2 C22 N22 97.6(7) 7_667 . . . ? C22 Fe2 C22 N22 -102.5(7) 8_657 . . . ? C21 Fe2 C22 N22 177.6(7) 7_667 . . . ? N21N Fe2 C22 N22 177.6(7) 7_667 . . . ? C21 Fe2 C22 Fe2 180.0 . . . 7_667 ? C22 Fe2 C22 Fe2 0.0 2_655 . . 7_667 ? C22 Fe2 C22 Fe2 -79.97(6) 7_667 . . 7_667 ? C22 Fe2 C22 Fe2 79.97(6) 8_657 . . 7_667 ? C21 Fe2 C22 Fe2 0.0 7_667 . . 7_667 ? N21N Fe2 C22 Fe2 0.0 7_667 . . 7_667 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H32 O2 0.79(2) 2.01(2) 2.7894(14) 171(2) 5_767 O3 H31 N22 0.84(3) 2.04(2) 2.8510(19) 162(2) . _diffrn_measured_fraction_theta_max 0.884 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.846 _refine_diff_density_min -0.250 _refine_diff_density_rms 0.053 #= END of data for compound 3 data_compound_4 _database_code_depnum_ccdc_archive 'CCDC 849760' #TrackingRef '- deposit_NEW.CIF' # start Validation Reply Form _vrf_PLAT222_I ; PROBLEM: Large Non-Solvent H Uiso(max)/Uiso(min) .. 10.0 Ratio RESPONSE: All attempts to split the positions of disordered i-PrOH molecule failed. The minor position appeared to be flat and cannot be refined without geometric restrictions. We preffered to describe the disorder with a.d.p. parameters. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H44 Fe Mn2 N10 O6' _chemical_formula_structural '[Mn (C12 H18 N2 O2)]2 [Fe (N O) (C N)5] (C3 H7 O H)' _chemical_formula_sum 'C32 H44 Fe Mn2 N10 O6' _chemical_formula_weight 830.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.8861(6) _cell_length_b 12.6888(6) _cell_length_c 16.0244(9) _cell_angle_alpha 90.00 _cell_angle_beta 107.5510(10) _cell_angle_gamma 90.00 _cell_volume 1916.57(18) _cell_formula_units_Z 2 _cell_measurement_temperature 150.0(2) _cell_measurement_reflns_used 4603 _cell_measurement_theta_min 2.6663 _cell_measurement_theta_max 26.3438 _exptl_crystal_description lath _exptl_crystal_colour brown _exptl_crystal_size_max 0.145 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.075 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 860 _exptl_absorpt_coefficient_mu 1.077 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.750 _exptl_absorpt_correction_T_max 0.922 _exptl_absorpt_process_details 'based on intensities (SADABS, Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8Apex CCD detector' _diffrn_measurement_method 'combined omega- and phi-scans' _diffrn_detector_area_resol_mean 25 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12744 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0492 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 26.39 _reflns_number_total 5791 _reflns_number_gt 5111 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 V.1.27 (Bruker, 2005)' _computing_cell_refinement 'Apex2 V.1.27 (Bruker, 2005)' _computing_data_reduction 'Apex2 V.1.27 (Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V6.22 (Bruker, 2000-2005)' _computing_publication_material 'local programs' _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^)+(0.0266P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.013(13) _refine_ls_number_reflns 5791 _refine_ls_number_parameters 473 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0625 _refine_ls_wR_factor_gt 0.0598 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 0.67277(5) 0.54031(3) 0.23771(3) 0.01701(10) Uani 1 1 d . . . Mn1 Mn 0.63708(5) 0.87063(4) 0.05195(3) 0.01793(11) Uani 1 1 d . . . Mn2 Mn 1.16618(5) 0.60934(4) 0.48052(3) 0.02002(12) Uani 1 1 d . . . O1S O 1.4012(3) 0.6617(2) 0.56596(16) 0.0324(6) Uani 1 1 d . . . H1 H 1.406(4) 0.709(4) 0.603(3) 0.050 Uiso 1 1 d . . . C1S C 1.5188(5) 0.6812(5) 0.5320(4) 0.0725(18) Uani 1 1 d . . . H1SA H 1.4692 0.7033 0.4704 0.087 Uiso 1 1 calc R . . C2S C 1.5769(6) 0.5747(5) 0.5188(4) 0.098(2) Uani 1 1 d . . . H2SA H 1.6542 0.5837 0.4929 0.148 Uiso 1 1 calc R . . H2SB H 1.5014 0.5322 0.4796 0.148 Uiso 1 1 calc R . . H2SC H 1.6130 0.5389 0.5754 0.148 Uiso 1 1 calc R . . C3S C 1.6015(9) 0.7637(8) 0.5628(7) 0.220(7) Uani 1 1 d . . . H3SA H 1.5762 0.7941 0.6124 0.330 Uiso 1 1 calc R . . H3SB H 1.5882 0.8168 0.5166 0.330 Uiso 1 1 calc R . . H3SC H 1.7009 0.7412 0.5822 0.330 Uiso 1 1 calc R . . N11 N 1.1384(3) 0.7511(2) 0.42737(17) 0.0225(6) Uani 1 1 d . . . N12 N 1.1131(3) 0.6777(2) 0.57629(17) 0.0212(6) Uani 1 1 d . . . N21 N 0.6817(3) 0.7901(2) -0.04180(17) 0.0217(6) Uani 1 1 d . . . N22 N 0.4573(3) 0.7889(2) 0.01460(17) 0.0220(6) Uani 1 1 d . . . C11 C 1.2203(4) 0.5166(3) 0.2447(2) 0.0401(10) Uani 1 1 d . . . H11B H 1.3135 0.4831 0.2676 0.060 Uiso 1 1 calc R . . H11C H 1.2152 0.5543 0.1905 0.060 Uiso 1 1 calc R . . H11D H 1.1461 0.4625 0.2328 0.060 Uiso 1 1 calc R . . C12 C 1.1991(3) 0.5923(3) 0.3105(2) 0.0275(8) Uani 1 1 d . . . C13 C 1.1535(4) 0.6931(3) 0.2889(2) 0.0325(9) Uani 1 1 d . . . H13A H 1.1313 0.7118 0.2289 0.039 Uiso 1 1 calc R . . C14 C 1.1359(4) 0.7732(3) 0.3472(2) 0.0295(8) Uani 1 1 d . . . C15 C 1.1167(5) 0.8826(3) 0.3119(3) 0.0518(12) Uani 1 1 d . . . H15A H 1.0394 0.9168 0.3282 0.078 Uiso 1 1 calc R . . H15B H 1.0933 0.8804 0.2480 0.078 Uiso 1 1 calc R . . H15C H 1.2047 0.9224 0.3364 0.078 Uiso 1 1 calc R . . C16 C 1.1284(4) 0.8322(3) 0.4909(2) 0.0258(8) Uani 1 1 d . . . H16A H 1.0736 0.8934 0.4599 0.031 Uiso 1 1 calc R . . H16B H 1.2244 0.8569 0.5244 0.031 Uiso 1 1 calc R . . C17 C 1.0555(4) 0.7851(3) 0.5521(2) 0.0289(8) Uani 1 1 d . . . H17A H 1.0728 0.8293 0.6052 0.035 Uiso 1 1 calc R . . H17B H 0.9519 0.7816 0.5230 0.035 Uiso 1 1 calc R . . C18 C 1.0750(5) 0.6949(3) 0.7199(2) 0.0443(11) Uani 1 1 d . . . H18A H 0.9780 0.7208 0.6938 0.066 Uiso 1 1 calc R . . H18B H 1.1389 0.7548 0.7408 0.066 Uiso 1 1 calc R . . H18C H 1.0779 0.6483 0.7692 0.066 Uiso 1 1 calc R . . C19 C 1.1215(4) 0.6347(3) 0.6520(2) 0.0261(8) Uani 1 1 d . . . C21 C 1.0257(3) 1.0202(3) 0.0719(2) 0.0322(9) Uani 1 1 d . . . H21A H 0.9918 1.0928 0.0716 0.048 Uiso 1 1 calc R . . H21B H 1.0890 1.0155 0.0353 0.048 Uiso 1 1 calc R . . H21C H 1.0775 0.9995 0.1320 0.048 Uiso 1 1 calc R . . C22 C 0.9004(3) 0.9472(3) 0.0361(2) 0.0235(8) Uani 1 1 d . . . C23 C 0.8887(3) 0.8897(3) -0.0384(2) 0.0267(8) Uani 1 1 d . . . H23A H 0.9572 0.9026 -0.0679 0.032 Uiso 1 1 calc R . . C24 C 0.7837(4) 0.8132(3) -0.0752(2) 0.0235(8) Uani 1 1 d . . . C25 C 0.7933(4) 0.7565(3) -0.1560(2) 0.0334(9) Uani 1 1 d . . . H25A H 0.8008 0.6805 -0.1448 0.050 Uiso 1 1 calc R . . H25B H 0.8773 0.7810 -0.1708 0.050 Uiso 1 1 calc R . . H25C H 0.7081 0.7713 -0.2049 0.050 Uiso 1 1 calc R . . C26 C 0.5824(4) 0.7030(3) -0.0740(2) 0.0307(9) Uani 1 1 d . . . H26A H 0.6174 0.6389 -0.0389 0.037 Uiso 1 1 calc R . . H26B H 0.5755 0.6876 -0.1357 0.037 Uiso 1 1 calc R . . C27 C 0.4396(4) 0.7318(3) -0.0674(2) 0.0266(8) Uani 1 1 d . . . H27A H 0.3890 0.7766 -0.1177 0.032 Uiso 1 1 calc R . . H27B H 0.3827 0.6673 -0.0687 0.032 Uiso 1 1 calc R . . C28 C 0.2265(4) 0.7225(3) 0.0165(2) 0.0334(9) Uani 1 1 d . . . H28A H 0.2532 0.6480 0.0178 0.050 Uiso 1 1 calc R . . H28B H 0.1786 0.7438 -0.0440 0.050 Uiso 1 1 calc R . . H28C H 0.1622 0.7328 0.0519 0.050 Uiso 1 1 calc R . . C29 C 0.3579(3) 0.7887(3) 0.0531(2) 0.0230(7) Uani 1 1 d . . . C110 C 1.1737(3) 0.5316(3) 0.6746(2) 0.0300(8) Uani 1 1 d . . . H11A H 1.1879 0.5098 0.7333 0.036 Uiso 1 1 calc R . . C111 C 1.2056(4) 0.4605(3) 0.6195(2) 0.0276(8) Uani 1 1 d . . . C112 C 1.2523(4) 0.3511(3) 0.6501(3) 0.0426(10) Uani 1 1 d . . . H11E H 1.3301 0.3298 0.6277 0.064 Uiso 1 1 calc R . . H11F H 1.1725 0.3024 0.6284 0.064 Uiso 1 1 calc R . . H11G H 1.2847 0.3496 0.7143 0.064 Uiso 1 1 calc R . . C210 C 0.3672(4) 0.8492(3) 0.1279(2) 0.0318(9) Uani 1 1 d . . . H21D H 0.2983 0.8359 0.1570 0.038 Uiso 1 1 calc R . . C211 C 0.4661(3) 0.9259(3) 0.1632(2) 0.0217(7) Uani 1 1 d . . . C212 C 0.4513(4) 0.9929(3) 0.2383(2) 0.0324(9) Uani 1 1 d . . . H21E H 0.5147 1.0539 0.2462 0.049 Uiso 1 1 calc R . . H21F H 0.4765 0.9508 0.2921 0.049 Uiso 1 1 calc R . . H21G H 0.3530 1.0172 0.2252 0.049 Uiso 1 1 calc R . . O11 O 1.2307(2) 0.5546(2) 0.39014(14) 0.0288(6) Uani 1 1 d . . . O12 O 1.1945(3) 0.47718(18) 0.53816(15) 0.0272(6) Uani 1 1 d . . . O21 O 0.8130(2) 0.94513(18) 0.08238(14) 0.0227(5) Uani 1 1 d . . . O22 O 0.5745(2) 0.94675(18) 0.13666(14) 0.0234(5) Uani 1 1 d . . . N1 N 0.5653(3) 0.6100(2) 0.27738(16) 0.0223(6) Uani 1 1 d . . . C41 C 0.8376(3) 0.5569(3) 0.3408(2) 0.0210(7) Uani 1 1 d . . . C51 C 0.8014(3) 0.4636(3) 0.1875(2) 0.0215(7) Uani 1 1 d . . . C61 C 0.7253(3) 0.6637(3) 0.1835(2) 0.0201(7) Uani 1 1 d . . . C71 C 0.5361(3) 0.5123(2) 0.1247(2) 0.0195(7) Uani 1 1 d . . . C81 C 0.6286(3) 0.4038(3) 0.2793(2) 0.0201(7) Uani 1 1 d . . . O1 O 0.4937(3) 0.6637(2) 0.30322(17) 0.0381(7) Uani 1 1 d . . . N41 N 0.9338(3) 0.5689(2) 0.40085(18) 0.0254(7) Uani 1 1 d . . . N51 N 0.8730(3) 0.4170(2) 0.1582(2) 0.0319(7) Uani 1 1 d . . . N61 N 0.7409(3) 0.7397(2) 0.14976(18) 0.0262(7) Uani 1 1 d . . . N71 N 0.4605(3) 0.4950(2) 0.05701(18) 0.0243(7) Uani 1 1 d . . . N81 N 0.6020(3) 0.3243(2) 0.30423(19) 0.0290(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 0.0186(2) 0.0170(2) 0.0142(2) -0.00018(19) 0.00297(17) -0.0001(2) Mn1 0.0192(2) 0.0183(3) 0.0160(2) 0.0011(2) 0.00482(19) -0.0013(2) Mn2 0.0243(3) 0.0173(3) 0.0169(2) -0.0004(2) 0.0040(2) 0.0015(2) O1S 0.0266(14) 0.0375(16) 0.0316(15) -0.0110(11) 0.0064(12) -0.0032(12) C1S 0.038(3) 0.081(4) 0.113(5) -0.044(3) 0.044(3) -0.016(3) C2S 0.089(4) 0.127(7) 0.101(5) 0.021(4) 0.061(4) 0.050(4) C3S 0.222(10) 0.192(11) 0.361(15) -0.136(10) 0.260(11) -0.133(9) N11 0.0208(15) 0.0228(17) 0.0231(15) -0.0004(12) 0.0053(12) -0.0014(12) N12 0.0234(15) 0.0210(16) 0.0167(14) -0.0006(11) 0.0022(12) -0.0005(12) N21 0.0240(15) 0.0200(16) 0.0200(15) 0.0014(12) 0.0049(12) -0.0005(12) N22 0.0236(15) 0.0205(16) 0.0202(15) 0.0039(12) 0.0039(12) 0.0002(12) C11 0.042(2) 0.048(3) 0.036(2) -0.0193(19) 0.0203(18) -0.0129(19) C12 0.0212(17) 0.038(2) 0.0248(18) -0.0048(16) 0.0092(14) -0.0083(16) C13 0.035(2) 0.044(3) 0.0202(18) 0.0083(17) 0.0116(16) 0.0034(18) C14 0.0236(19) 0.034(2) 0.035(2) 0.0126(17) 0.0153(16) 0.0046(16) C15 0.067(3) 0.037(3) 0.066(3) 0.025(2) 0.043(2) 0.015(2) C16 0.0281(19) 0.0169(19) 0.0270(19) -0.0001(14) 0.0002(15) 0.0032(14) C17 0.027(2) 0.028(2) 0.029(2) -0.0090(16) 0.0042(16) 0.0044(16) C18 0.062(3) 0.050(3) 0.029(2) -0.009(2) 0.026(2) -0.006(2) C19 0.0242(18) 0.033(2) 0.0205(18) -0.0053(15) 0.0064(14) -0.0111(15) C21 0.0191(17) 0.032(2) 0.043(2) 0.0084(17) 0.0047(15) -0.0034(16) C22 0.0188(17) 0.021(2) 0.0289(19) 0.0142(15) 0.0045(14) 0.0038(14) C23 0.0262(18) 0.026(2) 0.0309(19) 0.0094(16) 0.0136(15) 0.0052(15) C24 0.0279(19) 0.0234(19) 0.0213(18) 0.0077(14) 0.0104(15) 0.0120(15) C25 0.043(2) 0.032(2) 0.031(2) 0.0006(17) 0.0206(18) 0.0067(18) C26 0.040(2) 0.023(2) 0.030(2) -0.0058(16) 0.0127(17) -0.0023(17) C27 0.032(2) 0.022(2) 0.0238(18) 0.0013(15) 0.0053(15) -0.0073(16) C28 0.028(2) 0.027(2) 0.044(2) 0.0052(17) 0.0100(17) -0.0046(17) C29 0.0147(16) 0.0219(19) 0.0292(19) 0.0055(15) 0.0017(14) 0.0022(14) C110 0.036(2) 0.033(2) 0.0163(16) 0.0048(17) 0.0008(14) -0.0095(19) C111 0.0250(18) 0.024(2) 0.026(2) 0.0045(16) -0.0032(15) -0.0053(15) C112 0.047(2) 0.029(2) 0.039(2) 0.0127(18) -0.0065(19) -0.0020(19) C210 0.0248(18) 0.043(3) 0.031(2) 0.0051(18) 0.0145(16) 0.0017(17) C211 0.0237(18) 0.023(2) 0.0193(17) 0.0045(14) 0.0079(14) 0.0054(15) C212 0.037(2) 0.037(2) 0.0254(19) 0.0022(16) 0.0126(17) 0.0070(17) O11 0.0356(14) 0.0257(15) 0.0263(13) -0.0025(11) 0.0111(10) 0.0042(11) O12 0.0350(14) 0.0203(14) 0.0221(13) 0.0063(10) 0.0024(11) 0.0035(11) O21 0.0228(12) 0.0239(14) 0.0222(12) 0.0012(10) 0.0078(10) -0.0023(10) O22 0.0252(13) 0.0250(13) 0.0200(12) 0.0005(10) 0.0068(10) -0.0021(10) N1 0.0218(14) 0.0227(15) 0.0218(14) -0.0025(13) 0.0058(11) -0.0059(14) C41 0.0252(18) 0.0162(18) 0.0219(17) 0.0004(14) 0.0075(15) 0.0001(14) C51 0.0209(18) 0.0224(19) 0.0194(18) 0.0037(15) 0.0032(14) -0.0027(15) C61 0.0207(18) 0.0204(19) 0.0181(17) -0.0030(14) 0.0041(14) 0.0004(14) C71 0.0185(16) 0.0167(19) 0.0243(18) -0.0003(13) 0.0078(14) -0.0002(13) C81 0.0178(17) 0.0220(19) 0.0182(17) 0.0004(14) 0.0019(13) -0.0019(14) O1 0.0337(15) 0.0383(16) 0.0477(17) -0.0126(13) 0.0205(13) 0.0027(12) N41 0.0286(16) 0.0234(17) 0.0208(15) -0.0002(12) 0.0025(13) -0.0040(12) N51 0.0323(18) 0.0278(19) 0.0401(19) -0.0040(14) 0.0177(15) 0.0004(14) N61 0.0287(17) 0.0252(18) 0.0229(15) 0.0020(13) 0.0051(13) -0.0009(13) N71 0.0267(16) 0.0212(16) 0.0214(16) 0.0019(12) 0.0016(13) 0.0020(12) N81 0.0300(17) 0.0251(18) 0.0310(17) 0.0069(13) 0.0078(14) -0.0024(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 N1 1.650(3) . ? Fe1 C61 1.935(4) . ? Fe1 C71 1.938(3) . ? Fe1 C41 1.951(3) . ? Fe1 C81 1.952(3) . ? Fe1 C51 1.957(4) . ? Mn1 O21 1.909(2) . ? Mn1 O22 1.914(2) . ? Mn1 N21 1.973(3) . ? Mn1 N22 1.988(3) . ? Mn1 N61 2.302(3) . ? Mn1 N71 2.336(3) 2_655 ? Mn2 O11 1.883(2) . ? Mn2 O12 1.894(2) . ? Mn2 N12 1.967(3) . ? Mn2 N11 1.974(3) . ? Mn2 N41 2.324(3) . ? Mn2 O1S 2.407(3) . ? O1S C1S 1.446(5) . ? O1S H1 0.84(4) . ? C1S C3S 1.329(9) . ? C1S C2S 1.507(8) . ? C1S H1SA 1.0000 . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? C3S H3SA 0.9800 . ? C3S H3SB 0.9800 . ? C3S H3SC 0.9800 . ? N11 C14 1.308(4) . ? N11 C16 1.472(4) . ? N12 C19 1.310(4) . ? N12 C17 1.483(4) . ? N21 C24 1.309(4) . ? N21 C26 1.466(4) . ? N22 C29 1.308(4) . ? N22 C27 1.465(4) . ? C11 C12 1.487(5) . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C11 H11D 0.9800 . ? C12 O11 1.309(4) . ? C12 C13 1.366(5) . ? C13 C14 1.426(5) . ? C13 H13A 0.9500 . ? C14 C15 1.489(5) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.504(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.511(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C110 1.413(5) . ? C21 C22 1.514(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 O21 1.298(4) . ? C22 C23 1.374(5) . ? C23 C24 1.413(5) . ? C23 H23A 0.9500 . ? C24 C25 1.509(5) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.492(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.509(5) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C210 1.402(5) . ? C110 C111 1.364(5) . ? C110 H11A 0.9500 . ? C111 O12 1.292(4) . ? C111 C112 1.498(5) . ? C112 H11E 0.9800 . ? C112 H11F 0.9800 . ? C112 H11G 0.9800 . ? C210 C211 1.374(5) . ? C210 H21D 0.9500 . ? C211 O22 1.295(4) . ? C211 C212 1.516(5) . ? C212 H21E 0.9800 . ? C212 H21F 0.9800 . ? C212 H21G 0.9800 . ? N1 O1 1.146(3) . ? C41 N41 1.141(4) . ? C51 N51 1.128(4) . ? C61 N61 1.139(4) . ? C71 N71 1.137(4) . ? C81 N81 1.145(4) . ? N71 Mn1 2.336(3) 2_645 ? 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 N1 Fe1 C61 91.75(14) . . ? N1 Fe1 C71 96.31(13) . . ? C61 Fe1 C71 86.25(13) . . ? N1 Fe1 C41 94.93(13) . . ? C61 Fe1 C41 91.38(14) . . ? C71 Fe1 C41 168.57(13) . . ? N1 Fe1 C81 96.20(14) . . ? C61 Fe1 C81 171.37(14) . . ? C71 Fe1 C81 89.53(13) . . ? C41 Fe1 C81 91.28(13) . . ? N1 Fe1 C51 177.26(15) . . ? C61 Fe1 C51 85.54(14) . . ? C71 Fe1 C51 83.15(13) . . ? C41 Fe1 C51 85.52(13) . . ? C81 Fe1 C51 86.49(14) . . ? O21 Mn1 O22 91.90(9) . . ? O21 Mn1 N21 93.16(10) . . ? O22 Mn1 N21 174.37(11) . . ? O21 Mn1 N22 176.61(11) . . ? O22 Mn1 N22 91.48(10) . . ? N21 Mn1 N22 83.45(11) . . ? O21 Mn1 N61 89.92(10) . . ? O22 Mn1 N61 93.12(10) . . ? N21 Mn1 N61 89.34(11) . . ? N22 Mn1 N61 90.19(10) . . ? O21 Mn1 N71 89.74(10) . 2_655 ? O22 Mn1 N71 92.30(10) . 2_655 ? N21 Mn1 N71 85.27(11) . 2_655 ? N22 Mn1 N71 89.83(10) . 2_655 ? N61 Mn1 N71 174.58(10) . 2_655 ? O11 Mn2 O12 90.81(11) . . ? O11 Mn2 N12 174.24(12) . . ? O12 Mn2 N12 92.58(11) . . ? O11 Mn2 N11 92.25(11) . . ? O12 Mn2 N11 176.56(11) . . ? N12 Mn2 N11 84.24(11) . . ? O11 Mn2 N41 90.24(10) . . ? O12 Mn2 N41 92.78(10) . . ? N12 Mn2 N41 94.24(10) . . ? N11 Mn2 N41 88.77(10) . . ? O11 Mn2 O1S 92.65(9) . . ? O12 Mn2 O1S 89.53(10) . . ? N12 Mn2 O1S 82.73(10) . . ? N11 Mn2 O1S 88.77(10) . . ? N41 Mn2 O1S 176.27(10) . . ? C1S O1S Mn2 125.5(3) . . ? C1S O1S H1 106(3) . . ? Mn2 O1S H1 116(3) . . ? C3S C1S O1S 117.9(5) . . ? C3S C1S C2S 122.8(6) . . ? O1S C1S C2S 106.5(5) . . ? C3S C1S H1SA 102.0 . . ? O1S C1S H1SA 102.0 . . ? C2S C1S H1SA 102.0 . . ? C1S C2S H2SA 109.5 . . ? C1S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? C1S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? C1S C3S H3SA 109.5 . . ? C1S C3S H3SB 109.5 . . ? H3SA C3S H3SB 109.5 . . ? C1S C3S H3SC 109.5 . . ? H3SA C3S H3SC 109.5 . . ? H3SB C3S H3SC 109.5 . . ? C14 N11 C16 123.0(3) . . ? C14 N11 Mn2 125.3(2) . . ? C16 N11 Mn2 111.6(2) . . ? C19 N12 C17 122.5(3) . . ? C19 N12 Mn2 125.5(3) . . ? C17 N12 Mn2 111.9(2) . . ? C24 N21 C26 122.8(3) . . ? C24 N21 Mn1 124.9(2) . . ? C26 N21 Mn1 112.3(2) . . ? C29 N22 C27 121.3(3) . . ? C29 N22 Mn1 126.1(2) . . ? C27 N22 Mn1 112.5(2) . . ? C12 C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C12 C11 H11D 109.5 . . ? H11B C11 H11D 109.5 . . ? H11C C11 H11D 109.5 . . ? O11 C12 C13 123.6(3) . . ? O11 C12 C11 114.3(3) . . ? C13 C12 C11 122.1(3) . . ? C12 C13 C14 126.7(3) . . ? C12 C13 H13A 116.7 . . ? C14 C13 H13A 116.7 . . ? N11 C14 C13 121.4(3) . . ? N11 C14 C15 122.3(3) . . ? C13 C14 C15 116.3(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N11 C16 C17 108.6(3) . . ? N11 C16 H16A 110.0 . . ? C17 C16 H16A 110.0 . . ? N11 C16 H16B 110.0 . . ? C17 C16 H16B 110.0 . . ? H16A C16 H16B 108.4 . . ? N12 C17 C16 108.3(3) . . ? N12 C17 H17A 110.0 . . ? C16 C17 H17A 110.0 . . ? N12 C17 H17B 110.0 . . ? C16 C17 H17B 110.0 . . ? H17A C17 H17B 108.4 . . ? C19 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C19 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N12 C19 C110 122.7(3) . . ? N12 C19 C18 120.5(3) . . ? C110 C19 C18 116.8(3) . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O21 C22 C23 126.1(3) . . ? O21 C22 C21 113.9(3) . . ? C23 C22 C21 119.9(3) . . ? C22 C23 C24 125.9(3) . . ? C22 C23 H23A 117.1 . . ? C24 C23 H23A 117.1 . . ? N21 C24 C23 122.9(3) . . ? N21 C24 C25 119.9(3) . . ? C23 C24 C25 117.2(3) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N21 C26 C27 109.7(3) . . ? N21 C26 H26A 109.7 . . ? C27 C26 H26A 109.7 . . ? N21 C26 H26B 109.7 . . ? C27 C26 H26B 109.7 . . ? H26A C26 H26B 108.2 . . ? N22 C27 C26 109.0(3) . . ? N22 C27 H27A 109.9 . . ? C26 C27 H27A 109.9 . . ? N22 C27 H27B 109.9 . . ? C26 C27 H27B 109.9 . . ? H27A C27 H27B 108.3 . . ? C29 C28 H28A 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C29 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N22 C29 C210 122.4(3) . . ? N22 C29 C28 119.9(3) . . ? C210 C29 C28 117.6(3) . . ? C111 C110 C19 125.7(3) . . ? C111 C110 H11A 117.1 . . ? C19 C110 H11A 117.1 . . ? O12 C111 C110 125.4(3) . . ? O12 C111 C112 114.0(3) . . ? C110 C111 C112 120.6(3) . . ? C111 C112 H11E 109.5 . . ? C111 C112 H11F 109.5 . . ? H11E C112 H11F 109.5 . . ? C111 C112 H11G 109.5 . . ? H11E C112 H11G 109.5 . . ? H11F C112 H11G 109.5 . . ? C211 C210 C29 126.5(3) . . ? C211 C210 H21D 116.7 . . ? C29 C210 H21D 116.7 . . ? O22 C211 C210 124.4(3) . . ? O22 C211 C212 115.8(3) . . ? C210 C211 C212 119.8(3) . . ? C211 C212 H21E 109.5 . . ? C211 C212 H21F 109.5 . . ? H21E C212 H21F 109.5 . . ? C211 C212 H21G 109.5 . . ? H21E C212 H21G 109.5 . . ? H21F C212 H21G 109.5 . . ? C12 O11 Mn2 125.3(2) . . ? C111 O12 Mn2 126.3(2) . . ? C22 O21 Mn1 125.2(2) . . ? C211 O22 Mn1 127.4(2) . . ? O1 N1 Fe1 175.9(3) . . ? N41 C41 Fe1 178.5(3) . . ? N51 C51 Fe1 178.1(3) . . ? N61 C61 Fe1 172.3(3) . . ? N71 C71 Fe1 177.1(3) . . ? N81 C81 Fe1 179.3(3) . . ? C41 N41 Mn2 158.1(3) . . ? C61 N61 Mn1 147.0(3) . . ? C71 N71 Mn1 148.0(2) . 2_645 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O11 Mn2 O1S C1S 22.5(4) . . . . ? O12 Mn2 O1S C1S 113.3(4) . . . . ? N12 Mn2 O1S C1S -154.0(4) . . . . ? N11 Mn2 O1S C1S -69.7(4) . . . . ? N41 Mn2 O1S C1S -118.4(15) . . . . ? Mn2 O1S C1S C3S 138.3(8) . . . . ? Mn2 O1S C1S C2S -79.1(5) . . . . ? O11 Mn2 N11 C14 14.6(3) . . . . ? O12 Mn2 N11 C14 167.6(18) . . . . ? N12 Mn2 N11 C14 -170.0(3) . . . . ? N41 Mn2 N11 C14 -75.6(3) . . . . ? O1S Mn2 N11 C14 107.2(3) . . . . ? O11 Mn2 N11 C16 -162.3(2) . . . . ? O12 Mn2 N11 C16 -9(2) . . . . ? N12 Mn2 N11 C16 13.2(2) . . . . ? N41 Mn2 N11 C16 107.6(2) . . . . ? O1S Mn2 N11 C16 -69.6(2) . . . . ? O11 Mn2 N12 C19 -118.4(11) . . . . ? O12 Mn2 N12 C19 7.7(3) . . . . ? N11 Mn2 N12 C19 -171.0(3) . . . . ? N41 Mn2 N12 C19 100.7(3) . . . . ? O1S Mn2 N12 C19 -81.5(3) . . . . ? O11 Mn2 N12 C17 63.9(12) . . . . ? O12 Mn2 N12 C17 -170.1(2) . . . . ? N11 Mn2 N12 C17 11.2(2) . . . . ? N41 Mn2 N12 C17 -77.1(2) . . . . ? O1S Mn2 N12 C17 100.7(2) . . . . ? O21 Mn1 N21 C24 -14.7(3) . . . . ? O22 Mn1 N21 C24 139.4(11) . . . . ? N22 Mn1 N21 C24 165.2(3) . . . . ? N61 Mn1 N21 C24 -104.5(3) . . . . ? N71 Mn1 N21 C24 74.8(3) 2_655 . . . ? O21 Mn1 N21 C26 168.3(2) . . . . ? O22 Mn1 N21 C26 -37.7(13) . . . . ? N22 Mn1 N21 C26 -11.9(2) . . . . ? N61 Mn1 N21 C26 78.4(2) . . . . ? N71 Mn1 N21 C26 -102.3(2) 2_655 . . . ? O21 Mn1 N22 C29 176.2(17) . . . . ? O22 Mn1 N22 C29 -8.8(3) . . . . ? N21 Mn1 N22 C29 173.6(3) . . . . ? N61 Mn1 N22 C29 84.3(3) . . . . ? N71 Mn1 N22 C29 -101.1(3) 2_655 . . . ? O21 Mn1 N22 C27 -8.1(19) . . . . ? O22 Mn1 N22 C27 166.9(2) . . . . ? N21 Mn1 N22 C27 -10.7(2) . . . . ? N61 Mn1 N22 C27 -100.0(2) . . . . ? N71 Mn1 N22 C27 74.6(2) 2_655 . . . ? O11 C12 C13 C14 1.4(6) . . . . ? C11 C12 C13 C14 -177.0(3) . . . . ? C16 N11 C14 C13 176.6(3) . . . . ? Mn2 N11 C14 C13 0.1(5) . . . . ? C16 N11 C14 C15 -2.5(5) . . . . ? Mn2 N11 C14 C15 -179.0(3) . . . . ? C12 C13 C14 N11 -12.5(6) . . . . ? C12 C13 C14 C15 166.6(4) . . . . ? C14 N11 C16 C17 148.9(3) . . . . ? Mn2 N11 C16 C17 -34.2(3) . . . . ? C19 N12 C17 C16 149.7(3) . . . . ? Mn2 N12 C17 C16 -32.5(3) . . . . ? N11 C16 C17 N12 42.6(3) . . . . ? C17 N12 C19 C110 178.7(3) . . . . ? Mn2 N12 C19 C110 1.1(5) . . . . ? C17 N12 C19 C18 -1.4(5) . . . . ? Mn2 N12 C19 C18 -178.9(3) . . . . ? O21 C22 C23 C24 -4.0(6) . . . . ? C21 C22 C23 C24 175.0(3) . . . . ? C26 N21 C24 C23 -173.1(3) . . . . ? Mn1 N21 C24 C23 10.1(5) . . . . ? C26 N21 C24 C25 6.4(5) . . . . ? Mn1 N21 C24 C25 -170.4(2) . . . . ? C22 C23 C24 N21 1.5(5) . . . . ? C22 C23 C24 C25 -178.0(3) . . . . ? C24 N21 C26 C27 -145.6(3) . . . . ? Mn1 N21 C26 C27 31.6(3) . . . . ? C29 N22 C27 C26 -153.7(3) . . . . ? Mn1 N22 C27 C26 30.3(3) . . . . ? N21 C26 C27 N22 -39.6(4) . . . . ? C27 N22 C29 C210 -174.9(3) . . . . ? Mn1 N22 C29 C210 0.4(5) . . . . ? C27 N22 C29 C28 4.4(5) . . . . ? Mn1 N22 C29 C28 179.8(2) . . . . ? N12 C19 C110 C111 -8.0(6) . . . . ? C18 C19 C110 C111 172.1(3) . . . . ? C19 C110 C111 O12 0.9(6) . . . . ? C19 C110 C111 C112 -176.4(3) . . . . ? N22 C29 C210 C211 9.9(6) . . . . ? C28 C29 C210 C211 -169.5(3) . . . . ? C29 C210 C211 O22 -6.8(6) . . . . ? C29 C210 C211 C212 172.9(3) . . . . ? C13 C12 O11 Mn2 21.5(5) . . . . ? C11 C12 O11 Mn2 -160.0(2) . . . . ? O12 Mn2 O11 C12 156.3(3) . . . . ? N12 Mn2 O11 C12 -77.6(12) . . . . ? N11 Mn2 O11 C12 -25.2(3) . . . . ? N41 Mn2 O11 C12 63.5(3) . . . . ? O1S Mn2 O11 C12 -114.1(3) . . . . ? C110 C111 O12 Mn2 12.6(5) . . . . ? C112 C111 O12 Mn2 -170.0(2) . . . . ? O11 Mn2 O12 C111 161.0(3) . . . . ? N12 Mn2 O12 C111 -14.4(3) . . . . ? N11 Mn2 O12 C111 8(2) . . . . ? N41 Mn2 O12 C111 -108.8(3) . . . . ? O1S Mn2 O12 C111 68.3(3) . . . . ? C23 C22 O21 Mn1 -6.0(4) . . . . ? C21 C22 O21 Mn1 175.0(2) . . . . ? O22 Mn1 O21 C22 -165.0(2) . . . . ? N21 Mn1 O21 C22 12.5(3) . . . . ? N22 Mn1 O21 C22 10.0(19) . . . . ? N61 Mn1 O21 C22 101.8(2) . . . . ? N71 Mn1 O21 C22 -72.8(2) 2_655 . . . ? C210 C211 O22 Mn1 -6.7(5) . . . . ? C212 C211 O22 Mn1 173.6(2) . . . . ? O21 Mn1 O22 C211 -168.3(3) . . . . ? N21 Mn1 O22 C211 37.6(13) . . . . ? N22 Mn1 O22 C211 12.0(3) . . . . ? N61 Mn1 O22 C211 -78.3(3) . . . . ? N71 Mn1 O22 C211 101.9(3) 2_655 . . . ? C61 Fe1 N1 O1 -7(4) . . . . ? C71 Fe1 N1 O1 -93(4) . . . . ? C41 Fe1 N1 O1 84(4) . . . . ? C81 Fe1 N1 O1 176(4) . . . . ? C51 Fe1 N1 O1 -15(6) . . . . ? N1 Fe1 C41 N41 -62(12) . . . . ? C61 Fe1 C41 N41 29(12) . . . . ? C71 Fe1 C41 N41 107(12) . . . . ? C81 Fe1 C41 N41 -159(12) . . . . ? C51 Fe1 C41 N41 115(12) . . . . ? N1 Fe1 C51 N51 -138(8) . . . . ? C61 Fe1 C51 N51 -146(9) . . . . ? C71 Fe1 C51 N51 -59(9) . . . . ? C41 Fe1 C51 N51 123(9) . . . . ? C81 Fe1 C51 N51 31(9) . . . . ? N1 Fe1 C61 N61 -37(2) . . . . ? C71 Fe1 C61 N61 59(2) . . . . ? C41 Fe1 C61 N61 -132(2) . . . . ? C81 Fe1 C61 N61 120(2) . . . . ? C51 Fe1 C61 N61 143(2) . . . . ? N1 Fe1 C71 N71 160(6) . . . . ? C61 Fe1 C71 N71 69(6) . . . . ? C41 Fe1 C71 N71 -10(6) . . . . ? C81 Fe1 C71 N71 -104(6) . . . . ? C51 Fe1 C71 N71 -17(6) . . . . ? C71 Fe1 C81 N81 -109(28) . . . . ? C41 Fe1 C81 N81 82(28) . . . . ? Fe1 C41 N41 Mn2 -69(12) . . . . ? O11 Mn2 N41 C41 -33.6(7) . . . . ? O12 Mn2 N41 C41 -124.4(7) . . . . ? N12 Mn2 N41 C41 142.8(7) . . . . ? N11 Mn2 N41 C41 58.6(7) . . . . ? O1S Mn2 N41 C41 107.3(16) . . . . ? Fe1 C61 N61 Mn1 -23(3) . . . . ? O21 Mn1 N61 C61 174.1(5) . . . . ? O22 Mn1 N61 C61 82.2(5) . . . . ? N21 Mn1 N61 C61 -92.7(5) . . . . ? N22 Mn1 N61 C61 -9.3(5) . . . . ? N71 Mn1 N61 C61 -99.5(11) 2_655 . . . ? Fe1 C71 N71 Mn1 68(6) . . . 2_645 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1S H1 N81 0.84(4) 2.10(4) 2.936(4) 175(4) 2_756 _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.408 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.055 #= END of data for compound 4 data_compound_5 _database_code_depnum_ccdc_archive 'CCDC 849761' #TrackingRef '- deposit_NEW.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H36 Fe Mn2 N10 O5' _chemical_formula_structural '(Mn (C12 H18 N2 O2))2 (Fe (N O) (C N)5)' _chemical_formula_sum 'C29 H36 Fe Mn2 N10 O5' _chemical_formula_weight 770.41 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 Tetragonal _symmetry_space_group_name_H-M P4(3) _symmetry_space_group_name_Hall 'P 4cw' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+3/4' 'y, -x, z+1/4' _cell_length_a 10.8355(4) _cell_length_b 10.8355(4) _cell_length_c 29.115(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3418.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used 5943 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 26.79 _exptl_crystal_description black _exptl_crystal_colour block _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 1.199 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8501 _exptl_absorpt_correction_T_max 0.8695 _exptl_absorpt_process_details 'SADABS (Bruker-AXS, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 301(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8Apex CCD detector' _diffrn_measurement_method 'combined omega- and phi-scans' _diffrn_detector_area_resol_mean 25 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26240 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7849 _reflns_number_gt 6158 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 V.1.27 (Bruker, 2005)' _computing_cell_refinement 'Apex2 V.1.27 (Bruker, 2005)' _computing_data_reduction 'Apex2 V.1.27 (Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V6.22 (Bruker, 2000-2005)' _computing_publication_material 'local programs' _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^)+(0.0460P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.580(14) _refine_ls_number_reflns 7849 _refine_ls_number_parameters 434 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0834 _refine_ls_wR_factor_gt 0.0752 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.955 _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 0.98568(4) 0.54433(3) 0.094427(16) 0.02661(10) Uani 1 1 d . . . C11 C 0.8081(3) 0.5203(3) 0.09513(12) 0.0295(7) Uani 1 1 d . . . N11 N 0.7024(2) 0.5098(2) 0.09541(11) 0.0380(6) Uani 1 1 d . . . C12 C 1.0103(3) 0.3662(3) 0.09884(12) 0.0318(7) Uani 1 1 d . . . N12 N 1.0225(2) 0.2620(3) 0.10288(11) 0.0441(8) Uani 1 1 d . . . C13 C 0.9569(3) 0.7210(3) 0.08348(12) 0.0341(7) Uani 1 1 d . . . N13 N 0.9393(2) 0.8239(3) 0.08124(11) 0.0437(7) Uani 1 1 d . . . C14 C 1.1625(3) 0.5672(3) 0.08197(12) 0.0321(7) Uani 1 1 d . . . N14 N 1.2663(2) 0.5795(2) 0.07604(11) 0.0404(7) Uani 1 1 d . . . C15 C 0.9642(3) 0.5165(3) 0.02968(13) 0.0394(8) Uani 1 1 d . . . N15 N 0.9472(3) 0.4934(4) -0.00837(12) 0.0662(10) Uani 1 1 d . . . N16 N 0.9925(3) 0.5638(3) 0.15039(11) 0.0455(8) Uani 1 1 d . . . O16 O 0.9900(3) 0.5764(5) 0.18896(12) 0.1117(16) Uani 1 1 d . . . Mn1 Mn 0.48970(4) 0.54815(4) 0.081923(15) 0.02897(12) Uani 1 1 d . . . O101 O 0.4943(2) 0.6478(2) 0.13563(8) 0.0394(6) Uani 1 1 d . . . C101 C 0.5725(4) 0.7897(4) 0.18952(14) 0.0642(12) Uani 1 1 d . . . H10A H 0.4945 0.7838 0.2050 0.096 Uiso 1 1 calc R . . H10B H 0.6007 0.8737 0.1902 0.096 Uiso 1 1 calc R . . H10C H 0.6317 0.7379 0.2047 0.096 Uiso 1 1 calc R . . C102 C 0.5580(3) 0.7487(3) 0.14064(13) 0.0427(9) Uani 1 1 d . . . C103 C 0.6079(3) 0.8144(3) 0.10534(14) 0.0468(10) Uani 1 1 d . . . H10D H 0.6534 0.8840 0.1132 0.056 Uiso 1 1 calc R . . C104 C 0.5976(3) 0.7877(3) 0.05819(14) 0.0424(9) Uani 1 1 d . . . C105 C 0.6516(4) 0.8822(4) 0.02538(16) 0.0676(13) Uani 1 1 d . . . H10E H 0.5954 0.8953 0.0004 0.101 Uiso 1 1 calc R . . H10F H 0.7289 0.8524 0.0137 0.101 Uiso 1 1 calc R . . H10G H 0.6647 0.9585 0.0414 0.101 Uiso 1 1 calc R . . N101 N 0.5448(2) 0.6867(2) 0.04310(10) 0.0335(6) Uani 1 1 d . . . C106 C 0.5309(4) 0.6591(3) -0.00583(12) 0.0466(9) Uani 1 1 d . . . H10H H 0.5887 0.7079 -0.0236 0.056 Uiso 1 1 calc R . . H10I H 0.4479 0.6793 -0.0158 0.056 Uiso 1 1 calc R . . C107 C 0.5553(4) 0.5245(3) -0.01298(13) 0.0451(9) Uani 1 1 d . . . H10J H 0.5263 0.4989 -0.0430 0.054 Uiso 1 1 calc R . . H10K H 0.6432 0.5079 -0.0110 0.054 Uiso 1 1 calc R . . N102 N 0.4888(3) 0.4574(2) 0.02334(10) 0.0320(6) Uani 1 1 d . . . C108 C 0.4371(4) 0.2923(4) -0.03059(13) 0.0490(9) Uani 1 1 d . . . H10L H 0.5205 0.2868 -0.0415 0.074 Uiso 1 1 calc R . . H10M H 0.3895 0.3422 -0.0513 0.074 Uiso 1 1 calc R . . H10N H 0.4019 0.2111 -0.0290 0.074 Uiso 1 1 calc R . . C109 C 0.4360(3) 0.3499(3) 0.01637(11) 0.0338(7) Uani 1 1 d . . . C110 C 0.3794(3) 0.2842(3) 0.05208(13) 0.0403(8) Uani 1 1 d . . . H11A H 0.3332 0.2154 0.0437 0.048 Uiso 1 1 calc R . . C111 C 0.3851(3) 0.3107(3) 0.09776(13) 0.0353(7) Uani 1 1 d . . . C112 C 0.3240(4) 0.2307(4) 0.13291(14) 0.0550(10) Uani 1 1 d . . . H11B H 0.3757 0.2249 0.1596 0.082 Uiso 1 1 calc R . . H11C H 0.3112 0.1498 0.1204 0.082 Uiso 1 1 calc R . . H11D H 0.2460 0.2660 0.1413 0.082 Uiso 1 1 calc R . . O102 O 0.44324(19) 0.40461(19) 0.11487(7) 0.0341(5) Uani 1 1 d . . . Mn2 Mn 0.97848(4) 0.04200(4) 0.095498(15) 0.03044(12) Uani 1 1 d . . . O201 O 1.1249(2) 0.0140(2) 0.06167(8) 0.0416(6) Uani 1 1 d . . . C201 C 1.2949(5) -0.1000(5) 0.0360(2) 0.0875(17) Uani 1 1 d . . . H20A H 1.2469 -0.1069 0.0083 0.131 Uiso 1 1 calc R . . H20B H 1.3311 -0.1786 0.0431 0.131 Uiso 1 1 calc R . . H20C H 1.3590 -0.0400 0.0316 0.131 Uiso 1 1 calc R . . C202 C 1.2124(3) -0.0600(3) 0.07506(15) 0.0461(9) Uani 1 1 d . . . C203 C 1.2320(3) -0.0989(3) 0.11854(16) 0.0496(10) Uani 1 1 d . . . H20D H 1.2981 -0.1521 0.1233 0.060 Uiso 1 1 calc R . . C204 C 1.1619(3) -0.0663(3) 0.15704(14) 0.0470(9) Uani 1 1 d . . . C205 C 1.2114(5) -0.1056(5) 0.20408(17) 0.0831(16) Uani 1 1 d . . . H20E H 1.2133 -0.0354 0.2242 0.125 Uiso 1 1 calc R . . H20F H 1.2933 -0.1381 0.2007 0.125 Uiso 1 1 calc R . . H20G H 1.1585 -0.1678 0.2169 0.125 Uiso 1 1 calc R . . N201 N 1.0582(3) -0.0072(3) 0.15381(10) 0.0376(7) Uani 1 1 d . . . C206 C 0.9816(4) 0.0258(5) 0.19327(15) 0.0671(13) Uani 1 1 d . . . H20H H 0.9992 -0.0291 0.2188 0.081 Uiso 1 1 calc R . . H20I H 0.9997 0.1096 0.2028 0.081 Uiso 1 1 calc R . . C207 C 0.8528(4) 0.0156(5) 0.18039(14) 0.0639(12) Uani 1 1 d . . . H20J H 0.8287 -0.0706 0.1793 0.077 Uiso 1 1 calc R . . H20K H 0.8015 0.0572 0.2029 0.077 Uiso 1 1 calc R . . N202 N 0.8361(2) 0.0718(3) 0.13548(9) 0.0358(6) Uani 1 1 d . . . C208 C 0.6529(4) 0.1865(5) 0.16150(17) 0.0812(15) Uani 1 1 d . . . H20L H 0.6950 0.1995 0.1901 0.122 Uiso 1 1 calc R . . H20M H 0.5916 0.1233 0.1653 0.122 Uiso 1 1 calc R . . H20N H 0.6137 0.2619 0.1521 0.122 Uiso 1 1 calc R . . C209 C 0.7445(3) 0.1472(3) 0.12537(13) 0.0400(8) Uani 1 1 d . . . C210 C 0.7277(3) 0.1947(3) 0.08105(13) 0.0427(9) Uani 1 1 d . . . H21A H 0.6646 0.2519 0.0772 0.051 Uiso 1 1 calc R . . C211 C 0.7942(3) 0.1654(3) 0.04339(13) 0.0401(9) Uani 1 1 d . . . C212 C 0.7618(4) 0.2182(4) -0.00275(14) 0.0661(13) Uani 1 1 d . . . H21B H 0.8333 0.2569 -0.0158 0.099 Uiso 1 1 calc R . . H21C H 0.6973 0.2782 0.0008 0.099 Uiso 1 1 calc R . . H21D H 0.7341 0.1532 -0.0226 0.099 Uiso 1 1 calc R . . O202 O 0.8879(2) 0.0904(2) 0.04280(8) 0.0379(5) 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 0.0182(2) 0.0201(2) 0.0415(3) 0.00133(19) -0.00075(19) 0.00017(17) C11 0.0261(16) 0.0230(15) 0.0394(17) 0.0016(14) 0.0000(14) 0.0002(11) N11 0.0240(14) 0.0315(14) 0.0585(19) 0.0007(14) 0.0008(14) 0.0019(10) C12 0.0198(14) 0.0280(17) 0.048(2) 0.0020(15) -0.0013(14) 0.0001(11) N12 0.0310(15) 0.0311(17) 0.070(2) 0.0062(15) -0.0047(14) 0.0002(12) C13 0.0234(16) 0.0260(17) 0.053(2) -0.0006(15) 0.0000(14) 0.0005(12) N13 0.0371(16) 0.0266(16) 0.068(2) 0.0029(14) -0.0036(14) 0.0009(12) C14 0.0265(17) 0.0199(15) 0.050(2) -0.0024(14) -0.0029(14) 0.0017(12) N14 0.0215(14) 0.0347(16) 0.065(2) -0.0015(14) 0.0049(13) 0.0002(11) C15 0.0330(19) 0.042(2) 0.043(2) 0.0035(17) 0.0009(15) -0.0036(15) N15 0.070(3) 0.091(3) 0.038(2) 0.0012(19) -0.0032(18) -0.009(2) N16 0.0327(16) 0.061(2) 0.042(2) -0.0076(16) -0.0027(13) -0.0017(14) O16 0.100(3) 0.195(5) 0.041(2) -0.024(2) -0.0069(19) -0.006(3) Mn1 0.0273(2) 0.0222(2) 0.0375(3) -0.0027(2) 0.0031(2) -0.00438(18) O101 0.0347(12) 0.0335(13) 0.0499(15) -0.0126(11) 0.0065(11) -0.0094(10) C101 0.072(3) 0.057(3) 0.064(3) -0.019(2) -0.009(2) -0.015(2) C102 0.0333(18) 0.0297(18) 0.065(3) -0.0165(17) -0.0083(17) 0.0031(14) C103 0.046(2) 0.0285(19) 0.066(3) -0.0030(17) -0.0116(19) -0.0110(15) C104 0.0292(18) 0.0280(18) 0.070(3) 0.0055(17) -0.0063(17) -0.0060(14) C105 0.073(3) 0.048(2) 0.082(3) 0.017(2) -0.015(2) -0.032(2) N101 0.0258(14) 0.0237(14) 0.0509(18) 0.0056(12) 0.0007(12) -0.0044(10) C106 0.052(2) 0.043(2) 0.045(2) 0.0108(16) 0.0032(17) -0.0145(17) C107 0.052(2) 0.044(2) 0.040(2) -0.0042(16) 0.0133(17) -0.0081(17) N102 0.0291(14) 0.0308(15) 0.0361(16) -0.0038(12) 0.0012(11) -0.0049(11) C108 0.051(2) 0.047(2) 0.049(2) -0.0133(17) -0.0068(18) -0.0031(17) C109 0.0301(17) 0.0288(17) 0.0425(19) -0.0067(14) -0.0058(14) 0.0021(13) C110 0.043(2) 0.0252(17) 0.053(2) -0.0029(15) -0.0073(17) -0.0088(14) C111 0.0254(15) 0.0297(17) 0.051(2) 0.0048(16) -0.0045(15) -0.0002(12) C112 0.052(2) 0.048(2) 0.065(3) 0.014(2) -0.004(2) -0.0181(19) O102 0.0318(12) 0.0321(12) 0.0383(13) 0.0024(10) -0.0036(10) -0.0067(9) Mn2 0.0247(2) 0.0324(3) 0.0343(3) 0.0010(2) -0.0003(2) 0.00710(17) O201 0.0326(13) 0.0364(13) 0.0559(16) 0.0067(11) 0.0092(11) 0.0090(10) C201 0.063(3) 0.084(4) 0.115(4) 0.003(3) 0.037(3) 0.035(3) C202 0.0294(18) 0.0292(18) 0.080(3) -0.0059(19) 0.0064(18) 0.0070(14) C203 0.034(2) 0.033(2) 0.082(3) 0.003(2) -0.009(2) 0.0112(16) C204 0.045(2) 0.0304(19) 0.065(3) 0.0030(17) -0.0236(19) -0.0016(15) C205 0.085(4) 0.078(4) 0.087(4) 0.010(3) -0.044(3) 0.031(3) N201 0.0379(16) 0.0368(16) 0.0382(17) 0.0001(13) -0.0078(13) 0.0056(13) C206 0.069(3) 0.091(4) 0.041(3) -0.004(2) -0.009(2) 0.016(3) C207 0.057(3) 0.086(3) 0.048(3) 0.014(2) 0.017(2) 0.008(2) N202 0.0311(15) 0.0341(15) 0.0420(17) 0.0021(12) 0.0043(12) 0.0001(12) C208 0.064(3) 0.089(4) 0.090(4) -0.001(3) 0.029(3) 0.033(3) C209 0.0267(18) 0.0317(18) 0.062(2) -0.0068(17) 0.0078(16) -0.0014(14) C210 0.0273(17) 0.0312(18) 0.070(3) 0.0009(18) -0.0041(17) 0.0069(14) C211 0.0327(19) 0.0257(17) 0.062(2) 0.0076(16) -0.0179(17) -0.0008(14) C212 0.064(3) 0.066(3) 0.068(3) 0.027(2) -0.023(2) 0.007(2) O202 0.0409(13) 0.0326(12) 0.0401(14) 0.0018(10) -0.0094(10) 0.0068(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 N16 1.645(3) . ? Fe1 C15 1.923(4) . ? Fe1 C11 1.942(3) . ? Fe1 C12 1.953(3) . ? Fe1 C14 1.966(3) . ? Fe1 C13 1.966(3) . ? C11 N11 1.150(4) . ? N11 Mn1 2.375(3) . ? C12 N12 1.143(4) . ? N12 Mn2 2.441(3) . ? C13 N13 1.132(4) . ? N13 Mn2 2.437(3) 1_565 ? C14 N14 1.145(4) . ? N14 Mn1 2.450(3) 1_655 ? C15 N15 1.151(5) . ? N16 O16 1.132(4) . ? Mn1 O102 1.895(2) . ? Mn1 O101 1.901(2) . ? Mn1 N102 1.969(3) . ? Mn1 N101 1.972(3) . ? Mn1 N14 2.450(3) 1_455 ? O101 C102 1.301(4) . ? C101 C102 1.499(5) . ? C101 H10A 0.9600 . ? C101 H10B 0.9600 . ? C101 H10C 0.9600 . ? C102 C103 1.362(5) . ? C103 C104 1.408(5) . ? C103 H10D 0.9300 . ? C104 N101 1.310(4) . ? C104 C105 1.518(5) . ? C105 H10E 0.9600 . ? C105 H10F 0.9600 . ? C105 H10G 0.9600 . ? N101 C106 1.463(4) . ? C106 C107 1.497(5) . ? C106 H10H 0.9700 . ? C106 H10I 0.9700 . ? C107 N102 1.472(4) . ? C107 H10J 0.9700 . ? C107 H10K 0.9700 . ? N102 C109 1.313(4) . ? C108 C109 1.503(5) . ? C108 H10L 0.9600 . ? C108 H10M 0.9600 . ? C108 H10N 0.9600 . ? C109 C110 1.402(5) . ? C110 C111 1.362(5) . ? C110 H11A 0.9300 . ? C111 O102 1.296(4) . ? C111 C112 1.496(5) . ? C112 H11B 0.9600 . ? C112 H11C 0.9600 . ? C112 H11D 0.9600 . ? Mn2 O202 1.896(2) . ? Mn2 O201 1.892(2) . ? Mn2 N202 1.960(3) . ? Mn2 N201 1.978(3) . ? Mn2 N13 2.437(3) 1_545 ? O201 C202 1.301(4) . ? C201 C202 1.511(6) . ? C201 H20A 0.9600 . ? C201 H20B 0.9600 . ? C201 H20C 0.9600 . ? C202 C203 1.351(6) . ? C203 C204 1.399(6) . ? C203 H20D 0.9300 . ? C204 N201 1.297(4) . ? C204 C205 1.531(5) . ? C205 H20E 0.9600 . ? C205 H20F 0.9600 . ? C205 H20G 0.9600 . ? N201 C206 1.462(5) . ? C206 C207 1.449(6) . ? C206 H20H 0.9700 . ? C206 H20I 0.9700 . ? C207 N202 1.454(5) . ? C207 H20J 0.9700 . ? C207 H20K 0.9700 . ? N202 C209 1.318(4) . ? C208 C209 1.508(5) . ? C208 H20L 0.9600 . ? C208 H20M 0.9600 . ? C208 H20N 0.9600 . ? C209 C210 1.401(5) . ? C210 C211 1.350(5) . ? C210 H21A 0.9300 . ? C211 O202 1.300(4) . ? C211 C212 1.502(5) . ? C212 H21B 0.9600 . ? C212 H21C 0.9600 . ? C212 H21D 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 N16 Fe1 C15 175.29(15) . . ? N16 Fe1 C11 92.92(14) . . ? C15 Fe1 C11 82.50(14) . . ? N16 Fe1 C12 93.18(15) . . ? C15 Fe1 C12 85.75(15) . . ? C11 Fe1 C12 90.15(12) . . ? N16 Fe1 C14 97.07(14) . . ? C15 Fe1 C14 87.52(14) . . ? C11 Fe1 C14 169.96(15) . . ? C12 Fe1 C14 90.20(12) . . ? N16 Fe1 C13 92.46(15) . . ? C15 Fe1 C13 88.55(15) . . ? C11 Fe1 C13 88.56(13) . . ? C12 Fe1 C13 174.27(15) . . ? C14 Fe1 C13 90.10(12) . . ? N11 C11 Fe1 178.0(3) . . ? C11 N11 Mn1 161.3(3) . . ? N12 C12 Fe1 177.5(3) . . ? C12 N12 Mn2 159.0(3) . . ? N13 C13 Fe1 173.9(3) . . ? C13 N13 Mn2 156.2(3) . 1_565 ? N14 C14 Fe1 177.9(3) . . ? C14 N14 Mn1 160.6(3) . 1_655 ? N15 C15 Fe1 175.8(3) . . ? O16 N16 Fe1 176.1(3) . . ? O102 Mn1 O101 93.26(10) . . ? O102 Mn1 N102 91.56(10) . . ? O101 Mn1 N102 175.18(10) . . ? O102 Mn1 N101 174.45(11) . . ? O101 Mn1 N101 91.77(11) . . ? N102 Mn1 N101 83.42(11) . . ? O102 Mn1 N11 91.76(9) . . ? O101 Mn1 N11 86.45(10) . . ? N102 Mn1 N11 93.48(11) . . ? N101 Mn1 N11 86.20(10) . . ? O102 Mn1 N14 83.49(9) . 1_455 ? O101 Mn1 N14 90.25(10) . 1_455 ? N102 Mn1 N14 90.22(11) . 1_455 ? N101 Mn1 N14 98.84(10) . 1_455 ? N11 Mn1 N14 174.06(10) . 1_455 ? C102 O101 Mn1 125.7(2) . . ? C102 C101 H10A 109.5 . . ? C102 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C102 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? O101 C102 C103 124.4(3) . . ? O101 C102 C101 114.3(3) . . ? C103 C102 C101 121.3(3) . . ? C102 C103 C104 126.6(3) . . ? C102 C103 H10D 116.7 . . ? C104 C103 H10D 116.7 . . ? N101 C104 C103 122.3(3) . . ? N101 C104 C105 121.4(4) . . ? C103 C104 C105 116.4(3) . . ? C104 C105 H10E 109.5 . . ? C104 C105 H10F 109.5 . . ? H10E C105 H10F 109.5 . . ? C104 C105 H10G 109.5 . . ? H10E C105 H10G 109.5 . . ? H10F C105 H10G 109.5 . . ? C104 N101 C106 122.8(3) . . ? C104 N101 Mn1 125.2(3) . . ? C106 N101 Mn1 111.8(2) . . ? N101 C106 C107 108.4(3) . . ? N101 C106 H10H 110.0 . . ? C107 C106 H10H 110.0 . . ? N101 C106 H10I 110.0 . . ? C107 C106 H10I 110.0 . . ? H10H C106 H10I 108.4 . . ? N102 C107 C106 107.2(3) . . ? N102 C107 H10J 110.3 . . ? C106 C107 H10J 110.3 . . ? N102 C107 H10K 110.3 . . ? C106 C107 H10K 110.3 . . ? H10J C107 H10K 108.5 . . ? C109 N102 C107 122.7(3) . . ? C109 N102 Mn1 125.4(2) . . ? C107 N102 Mn1 111.9(2) . . ? C109 C108 H10L 109.5 . . ? C109 C108 H10M 109.5 . . ? H10L C108 H10M 109.5 . . ? C109 C108 H10N 109.5 . . ? H10L C108 H10N 109.5 . . ? H10M C108 H10N 109.5 . . ? N102 C109 C110 121.8(3) . . ? N102 C109 C108 120.3(3) . . ? C110 C109 C108 117.9(3) . . ? C111 C110 C109 126.7(3) . . ? C111 C110 H11A 116.7 . . ? C109 C110 H11A 116.7 . . ? O102 C111 C110 124.3(3) . . ? O102 C111 C112 114.0(3) . . ? C110 C111 C112 121.7(3) . . ? C111 C112 H11B 109.5 . . ? C111 C112 H11C 109.5 . . ? H11B C112 H11C 109.5 . . ? C111 C112 H11D 109.5 . . ? H11B C112 H11D 109.5 . . ? H11C C112 H11D 109.5 . . ? C111 O102 Mn1 125.4(2) . . ? O202 Mn2 O201 93.29(10) . . ? O202 Mn2 N202 91.57(11) . . ? O201 Mn2 N202 174.86(12) . . ? O202 Mn2 N201 174.54(11) . . ? O201 Mn2 N201 92.15(11) . . ? N202 Mn2 N201 83.01(12) . . ? O202 Mn2 N13 92.30(10) . 1_545 ? O201 Mn2 N13 84.36(10) . 1_545 ? N202 Mn2 N13 97.12(11) . 1_545 ? N201 Mn2 N13 87.75(11) . 1_545 ? O202 Mn2 N12 84.40(10) . . ? O201 Mn2 N12 92.22(10) . . ? N202 Mn2 N12 86.59(11) . . ? N201 Mn2 N12 95.88(11) . . ? N13 Mn2 N12 175.12(11) 1_545 . ? C202 O201 Mn2 123.6(2) . . ? C202 C201 H20A 109.5 . . ? C202 C201 H20B 109.5 . . ? H20A C201 H20B 109.5 . . ? C202 C201 H20C 109.5 . . ? H20A C201 H20C 109.5 . . ? H20B C201 H20C 109.5 . . ? O201 C202 C203 126.0(3) . . ? O201 C202 C201 112.5(4) . . ? C203 C202 C201 121.6(4) . . ? C202 C203 C204 125.9(3) . . ? C202 C203 H20D 117.0 . . ? C204 C203 H20D 117.0 . . ? N201 C204 C203 122.5(3) . . ? N201 C204 C205 120.3(4) . . ? C203 C204 C205 117.2(3) . . ? C204 C205 H20E 109.5 . . ? C204 C205 H20F 109.5 . . ? H20E C205 H20F 109.5 . . ? C204 C205 H20G 109.5 . . ? H20E C205 H20G 109.5 . . ? H20F C205 H20G 109.5 . . ? C204 N201 C206 123.8(3) . . ? C204 N201 Mn2 125.0(3) . . ? C206 N201 Mn2 111.2(2) . . ? C207 C206 N201 108.9(3) . . ? C207 C206 H20H 109.9 . . ? N201 C206 H20H 109.9 . . ? C207 C206 H20I 109.9 . . ? N201 C206 H20I 109.9 . . ? H20H C206 H20I 108.3 . . ? N202 C207 C206 108.7(3) . . ? N202 C207 H20J 110.0 . . ? C206 C207 H20J 110.0 . . ? N202 C207 H20K 110.0 . . ? C206 C207 H20K 110.0 . . ? H20J C207 H20K 108.3 . . ? C209 N202 C207 123.6(3) . . ? C209 N202 Mn2 124.2(2) . . ? C207 N202 Mn2 111.5(2) . . ? C209 C208 H20L 109.5 . . ? C209 C208 H20M 109.5 . . ? H20L C208 H20M 109.5 . . ? C209 C208 H20N 109.5 . . ? H20L C208 H20N 109.5 . . ? H20M C208 H20N 109.5 . . ? N202 C209 C210 122.1(3) . . ? N202 C209 C208 121.0(4) . . ? C210 C209 C208 116.9(3) . . ? C211 C210 C209 126.3(3) . . ? C211 C210 H21A 116.9 . . ? C209 C210 H21A 116.9 . . ? O202 C211 C210 125.1(3) . . ? O202 C211 C212 114.1(3) . . ? C210 C211 C212 120.8(3) . . ? C211 C212 H21B 109.5 . . ? C211 C212 H21C 109.5 . . ? H21B C212 H21C 109.5 . . ? C211 C212 H21D 109.5 . . ? H21B C212 H21D 109.5 . . ? H21C C212 H21D 109.5 . . ? C211 O202 Mn2 124.5(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N16 Fe1 C11 N11 89(9) . . . . ? C15 Fe1 C11 N11 -93(9) . . . . ? C12 Fe1 C11 N11 -178(100) . . . . ? C14 Fe1 C11 N11 -86(9) . . . . ? C13 Fe1 C11 N11 -4(9) . . . . ? Fe1 C11 N11 Mn1 27(9) . . . . ? N16 Fe1 C12 N12 33(7) . . . . ? C15 Fe1 C12 N12 -142(7) . . . . ? C11 Fe1 C12 N12 -60(7) . . . . ? C14 Fe1 C12 N12 130(7) . . . . ? C13 Fe1 C12 N12 -137(7) . . . . ? Fe1 C12 N12 Mn2 91(7) . . . . ? N16 Fe1 C13 N13 -8(3) . . . . ? C15 Fe1 C13 N13 167(3) . . . . ? C11 Fe1 C13 N13 85(3) . . . . ? C12 Fe1 C13 N13 162(2) . . . . ? C14 Fe1 C13 N13 -105(3) . . . . ? Fe1 C13 N13 Mn2 61(3) . . . 1_565 ? N16 Fe1 C14 N14 25(8) . . . . ? C15 Fe1 C14 N14 -154(8) . . . . ? C11 Fe1 C14 N14 -160(8) . . . . ? C12 Fe1 C14 N14 -68(8) . . . . ? C13 Fe1 C14 N14 117(8) . . . . ? Fe1 C14 N14 Mn1 32(9) . . . 1_655 ? N16 Fe1 C15 N15 -36(6) . . . . ? C11 Fe1 C15 N15 -49(5) . . . . ? C12 Fe1 C15 N15 41(5) . . . . ? C14 Fe1 C15 N15 132(5) . . . . ? C13 Fe1 C15 N15 -138(5) . . . . ? C15 Fe1 N16 O16 -15(7) . . . . ? C11 Fe1 N16 O16 -1(6) . . . . ? C12 Fe1 N16 O16 -92(6) . . . . ? C14 Fe1 N16 O16 178(100) . . . . ? C13 Fe1 N16 O16 87(6) . . . . ? C11 N11 Mn1 O102 180(100) . . . . ? C11 N11 Mn1 O101 -86.8(8) . . . . ? C11 N11 Mn1 N102 88.3(8) . . . . ? C11 N11 Mn1 N101 5.2(8) . . . . ? C11 N11 Mn1 N14 -143.2(9) . . . 1_455 ? O102 Mn1 O101 C102 155.9(3) . . . . ? N102 Mn1 O101 C102 -25.0(15) . . . . ? N101 Mn1 O101 C102 -21.7(3) . . . . ? N11 Mn1 O101 C102 64.4(3) . . . . ? N14 Mn1 O101 C102 -120.6(3) 1_455 . . . ? Mn1 O101 C102 C103 16.3(5) . . . . ? Mn1 O101 C102 C101 -164.1(3) . . . . ? O101 C102 C103 C104 1.6(6) . . . . ? C101 C102 C103 C104 -178.0(4) . . . . ? C102 C103 C104 N101 -5.9(6) . . . . ? C102 C103 C104 C105 174.4(4) . . . . ? C103 C104 N101 C106 178.5(3) . . . . ? C105 C104 N101 C106 -1.8(5) . . . . ? C103 C104 N101 Mn1 -7.6(5) . . . . ? C105 C104 N101 Mn1 172.1(3) . . . . ? O102 Mn1 N101 C104 -137.4(10) . . . . ? O101 Mn1 N101 C104 17.5(3) . . . . ? N102 Mn1 N101 C104 -162.8(3) . . . . ? N11 Mn1 N101 C104 -68.8(3) . . . . ? N14 Mn1 N101 C104 108.0(3) 1_455 . . . ? O102 Mn1 N101 C106 37.0(11) . . . . ? O101 Mn1 N101 C106 -168.0(2) . . . . ? N102 Mn1 N101 C106 11.7(2) . . . . ? N11 Mn1 N101 C106 105.6(2) . . . . ? N14 Mn1 N101 C106 -77.5(2) 1_455 . . . ? C104 N101 C106 C107 140.1(3) . . . . ? Mn1 N101 C106 C107 -34.5(3) . . . . ? N101 C106 C107 N102 45.0(4) . . . . ? C106 C107 N102 C109 143.8(3) . . . . ? C106 C107 N102 Mn1 -36.1(4) . . . . ? O102 Mn1 N102 C109 16.6(3) . . . . ? O101 Mn1 N102 C109 -162.5(12) . . . . ? N101 Mn1 N102 C109 -165.7(3) . . . . ? N11 Mn1 N102 C109 108.5(3) . . . . ? N14 Mn1 N102 C109 -66.9(3) 1_455 . . . ? O102 Mn1 N102 C107 -163.4(2) . . . . ? O101 Mn1 N102 C107 17.5(15) . . . . ? N101 Mn1 N102 C107 14.2(2) . . . . ? N11 Mn1 N102 C107 -71.6(2) . . . . ? N14 Mn1 N102 C107 113.1(2) 1_455 . . . ? C107 N102 C109 C110 176.2(3) . . . . ? Mn1 N102 C109 C110 -3.9(5) . . . . ? C107 N102 C109 C108 -2.6(5) . . . . ? Mn1 N102 C109 C108 177.4(2) . . . . ? N102 C109 C110 C111 -9.6(6) . . . . ? C108 C109 C110 C111 169.2(3) . . . . ? C109 C110 C111 O102 1.6(6) . . . . ? C109 C110 C111 C112 -177.8(3) . . . . ? C110 C111 O102 Mn1 19.7(4) . . . . ? C112 C111 O102 Mn1 -160.9(2) . . . . ? O101 Mn1 O102 C111 155.6(2) . . . . ? N102 Mn1 O102 C111 -24.3(2) . . . . ? N101 Mn1 O102 C111 -49.4(11) . . . . ? N11 Mn1 O102 C111 -117.8(2) . . . . ? N14 Mn1 O102 C111 65.8(2) 1_455 . . . ? C12 N12 Mn2 O202 24.4(8) . . . . ? C12 N12 Mn2 O201 117.5(8) . . . . ? C12 N12 Mn2 N202 -67.5(8) . . . . ? C12 N12 Mn2 N201 -150.1(8) . . . . ? C12 N12 Mn2 N13 72.0(14) . . . 1_545 ? O202 Mn2 O201 C202 -155.8(3) . . . . ? N202 Mn2 O201 C202 43.1(13) . . . . ? N201 Mn2 O201 C202 23.7(3) . . . . ? N13 Mn2 O201 C202 -63.9(3) 1_545 . . . ? N12 Mn2 O201 C202 119.6(3) . . . . ? Mn2 O201 C202 C203 -20.5(5) . . . . ? Mn2 O201 C202 C201 160.0(3) . . . . ? O201 C202 C203 C204 -0.1(6) . . . . ? C201 C202 C203 C204 179.4(4) . . . . ? C202 C203 C204 N201 9.9(6) . . . . ? C202 C203 C204 C205 -171.3(4) . . . . ? C203 C204 N201 C206 178.7(4) . . . . ? C205 C204 N201 C206 -0.2(6) . . . . ? C203 C204 N201 Mn2 2.1(5) . . . . ? C205 C204 N201 Mn2 -176.8(3) . . . . ? O202 Mn2 N201 C204 159.6(10) . . . . ? O201 Mn2 N201 C204 -15.2(3) . . . . ? N202 Mn2 N201 C204 166.5(3) . . . . ? N13 Mn2 N201 C204 69.0(3) 1_545 . . . ? N12 Mn2 N201 C204 -107.7(3) . . . . ? O202 Mn2 N201 C206 -17.3(13) . . . . ? O201 Mn2 N201 C206 167.8(3) . . . . ? N202 Mn2 N201 C206 -10.4(3) . . . . ? N13 Mn2 N201 C206 -107.9(3) 1_545 . . . ? N12 Mn2 N201 C206 75.4(3) . . . . ? C204 N201 C206 C207 -143.9(4) . . . . ? Mn2 N201 C206 C207 33.1(5) . . . . ? N201 C206 C207 N202 -44.6(5) . . . . ? C206 C207 N202 C209 -135.0(4) . . . . ? C206 C207 N202 Mn2 36.4(4) . . . . ? O202 Mn2 N202 C209 -23.7(3) . . . . ? O201 Mn2 N202 C209 137.4(12) . . . . ? N201 Mn2 N202 C209 157.0(3) . . . . ? N13 Mn2 N202 C209 -116.2(3) 1_545 . . . ? N12 Mn2 N202 C209 60.6(3) . . . . ? O202 Mn2 N202 C207 165.0(3) . . . . ? O201 Mn2 N202 C207 -33.9(14) . . . . ? N201 Mn2 N202 C207 -14.3(3) . . . . ? N13 Mn2 N202 C207 72.5(3) 1_545 . . . ? N12 Mn2 N202 C207 -110.7(3) . . . . ? C207 N202 C209 C210 -176.6(4) . . . . ? Mn2 N202 C209 C210 13.1(5) . . . . ? C207 N202 C209 C208 3.6(6) . . . . ? Mn2 N202 C209 C208 -166.7(3) . . . . ? N202 C209 C210 C211 4.6(6) . . . . ? C208 C209 C210 C211 -175.6(4) . . . . ? C209 C210 C211 O202 -2.3(6) . . . . ? C209 C210 C211 C212 176.6(3) . . . . ? C210 C211 O202 Mn2 -18.1(5) . . . . ? C212 C211 O202 Mn2 162.9(2) . . . . ? O201 Mn2 O202 C211 -152.4(3) . . . . ? N202 Mn2 O202 C211 25.9(3) . . . . ? N201 Mn2 O202 C211 32.7(13) . . . . ? N13 Mn2 O202 C211 123.1(3) 1_545 . . . ? N12 Mn2 O202 C211 -60.5(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.339 _refine_diff_density_min -0.222 _refine_diff_density_rms 0.049 #= END of data for compound 5 #= END of CIF file submission