# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Jianzhuang Jiang.' 'Yuting Chen.' 'Zhong-Hai Ni.' 'Laijin Tian.' 'Hailong Wang.' 'Daopeng Zhang.' _publ_contact_author_name 'Jianzhuang Jiang' _publ_contact_author_email JZJIANG@SDU.EDU.CN _publ_section_title ; Synthesis, Structures, and Magnetic Properties of Cyanide-bridged Low-dimensional Heterometallic FeIII-MnII Complexes ; # Attachment '1-5.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 732677' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H18 Fe K N4 O3' _chemical_formula_weight 445.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.380(2) _cell_length_b 7.6456(15) _cell_length_c 21.151(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.295(5) _cell_angle_gamma 90.00 _cell_volume 1963.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 916 _exptl_absorpt_coefficient_mu 1.008 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8474 _exptl_absorpt_correction_T_max 0.8972 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15467 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3442 _reflns_number_gt 2927 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0490P)^2^+0.8979P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3442 _refine_ls_number_parameters 254 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0903 _refine_ls_wR_factor_gt 0.0836 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.051 _refine_ls_shift/su_mean 0.001 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 0.50532(2) 0.72993(4) 0.187363(15) 0.03342(12) Uani 1 1 d . . . K1 K 0.69586(4) 0.08968(7) 0.24564(3) 0.04906(17) Uani 1 1 d D . . O1 O 0.61614(13) 0.8471(2) 0.15252(7) 0.0407(4) Uani 1 1 d . . . O2 O 0.59733(12) 0.7527(2) 0.27102(7) 0.0375(4) Uani 1 1 d . . . O3 O 0.5489(2) 0.2757(4) 0.31033(12) 0.0930(8) Uani 1 1 d D . . H20 H 0.4918 0.2926 0.2714 0.112 Uiso 1 1 d RD . . N1 N 0.62140(18) 0.3762(3) 0.16938(11) 0.0515(5) Uani 1 1 d . . . N2 N 0.3958(2) 1.0874(3) 0.20997(12) 0.0566(6) Uani 1 1 d . . . N3 N 0.41207(16) 0.6925(3) 0.10522(10) 0.0432(5) Uani 1 1 d . . . N4 N 0.38920(15) 0.6196(3) 0.22020(10) 0.0421(5) Uani 1 1 d . . . C1 C 0.57616(18) 0.5041(3) 0.17520(11) 0.0391(5) Uani 1 1 d . . . C2 C 0.43486(18) 0.9571(3) 0.20049(11) 0.0394(5) Uani 1 1 d . . . C3 C 0.4401(2) 0.7112(3) 0.05061(12) 0.0479(6) Uani 1 1 d . . . H7 H 0.3884 0.6812 0.0141 0.057 Uiso 1 1 calc R . . C4 C 0.5444(2) 0.7744(3) 0.04095(12) 0.0449(6) Uani 1 1 d . . . C5 C 0.5624(3) 0.7817(4) -0.02268(13) 0.0603(8) Uani 1 1 d . . . H5 H 0.5087 0.7389 -0.0561 0.072 Uiso 1 1 calc R . . C6 C 0.6576(3) 0.8506(5) -0.03643(14) 0.0683(9) Uani 1 1 d . . . H4 H 0.6684 0.8537 -0.0787 0.082 Uiso 1 1 calc R . . C7 C 0.7369(3) 0.9152(4) 0.01284(14) 0.0653(8) Uani 1 1 d . . . H3 H 0.8015 0.9616 0.0037 0.078 Uiso 1 1 calc R . . C8 C 0.7217(2) 0.9117(4) 0.07542(13) 0.0537(7) Uani 1 1 d . . . H2 H 0.7762 0.9572 0.1078 0.064 Uiso 1 1 calc R . . C9 C 0.6264(2) 0.8415(3) 0.09175(11) 0.0404(5) Uani 1 1 d . . . C10 C 0.3756(2) 0.6271(3) 0.27846(13) 0.0492(6) Uani 1 1 d . . . H10 H 0.3119 0.5775 0.2878 0.059 Uiso 1 1 calc R . . C11 C 0.4512(2) 0.7064(4) 0.33033(12) 0.0458(6) Uani 1 1 d . . . C12 C 0.4196(3) 0.7205(4) 0.39067(15) 0.0634(8) Uani 1 1 d . . . H12 H 0.3490 0.6859 0.3942 0.076 Uiso 1 1 calc R . . C13 C 0.4882(3) 0.7826(5) 0.44359(15) 0.0749(10) Uani 1 1 d . . . H13 H 0.4653 0.7916 0.4828 0.090 Uiso 1 1 calc R . . C14 C 0.5936(3) 0.8326(5) 0.43808(14) 0.0698(9) Uani 1 1 d . . . H14 H 0.6414 0.8757 0.4742 0.084 Uiso 1 1 calc R . . C15 C 0.6293(2) 0.8200(4) 0.38067(12) 0.0524(7) Uani 1 1 d . . . H15 H 0.7011 0.8521 0.3790 0.063 Uiso 1 1 calc R . . C16 C 0.5593(2) 0.7598(3) 0.32469(11) 0.0391(5) Uani 1 1 d . . . C17 C 0.3004(2) 0.6348(4) 0.11001(14) 0.0572(7) Uani 1 1 d . . . H8A H 0.2684 0.5654 0.0726 0.069 Uiso 1 1 calc R . . H8B H 0.2534 0.7352 0.1122 0.069 Uiso 1 1 calc R . . C18 C 0.3109(2) 0.5266(4) 0.17055(14) 0.0545(7) Uani 1 1 d . . . H9A H 0.2400 0.5158 0.1832 0.065 Uiso 1 1 calc R . . H9B H 0.3380 0.4105 0.1637 0.065 Uiso 1 1 calc R . . C19 C 0.4986(4) 0.2480(5) 0.3623(2) 0.0894(12) Uani 1 1 d . . . H19A H 0.5152 0.1321 0.3789 0.134 Uiso 1 1 calc R . . H19B H 0.4203 0.2606 0.3488 0.134 Uiso 1 1 calc R . . H19C H 0.5252 0.3321 0.3954 0.134 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 Fe1 0.02649(18) 0.0374(2) 0.0351(2) 0.00098(13) 0.00272(13) -0.00173(13) K1 0.0431(3) 0.0418(3) 0.0574(3) 0.0056(2) -0.0022(2) -0.0021(2) O1 0.0396(9) 0.0506(10) 0.0332(8) -0.0051(7) 0.0104(7) -0.0120(8) O2 0.0299(8) 0.0504(10) 0.0324(8) -0.0001(7) 0.0065(7) 0.0007(7) O3 0.0954(19) 0.110(2) 0.0712(16) -0.0051(14) 0.0103(14) 0.0096(16) N1 0.0444(12) 0.0469(14) 0.0605(14) 0.0005(11) 0.0036(10) 0.0056(11) N2 0.0578(14) 0.0490(15) 0.0643(15) 0.0030(11) 0.0152(12) 0.0104(12) N3 0.0351(10) 0.0429(12) 0.0462(12) 0.0008(9) -0.0054(9) -0.0010(9) N4 0.0270(10) 0.0420(12) 0.0556(13) 0.0070(9) 0.0041(9) -0.0002(8) C1 0.0318(12) 0.0449(15) 0.0376(12) 0.0021(10) -0.0004(9) -0.0036(11) C2 0.0323(11) 0.0469(15) 0.0387(12) 0.0052(11) 0.0065(10) -0.0016(11) C3 0.0507(15) 0.0471(15) 0.0393(14) -0.0052(11) -0.0072(12) 0.0040(12) C4 0.0512(15) 0.0450(15) 0.0366(13) -0.0023(10) 0.0044(11) 0.0090(11) C5 0.074(2) 0.069(2) 0.0352(14) -0.0050(13) 0.0044(14) 0.0191(16) C6 0.085(2) 0.087(2) 0.0394(15) 0.0062(15) 0.0270(15) 0.0252(19) C7 0.0682(19) 0.079(2) 0.0564(18) 0.0084(15) 0.0297(15) 0.0054(16) C8 0.0525(15) 0.0662(19) 0.0461(14) -0.0025(13) 0.0183(12) -0.0052(14) C9 0.0471(13) 0.0383(14) 0.0372(12) 0.0005(10) 0.0116(10) 0.0043(11) C10 0.0348(13) 0.0510(16) 0.0658(18) 0.0173(13) 0.0194(12) 0.0018(11) C11 0.0443(14) 0.0493(15) 0.0478(14) 0.0120(12) 0.0185(12) 0.0088(12) C12 0.0640(19) 0.072(2) 0.064(2) 0.0200(15) 0.0367(16) 0.0134(15) C13 0.089(3) 0.101(3) 0.0420(17) 0.0089(16) 0.0294(17) 0.020(2) C14 0.075(2) 0.094(2) 0.0390(15) -0.0013(15) 0.0077(14) 0.0172(19) C15 0.0475(15) 0.0699(19) 0.0382(13) 0.0016(13) 0.0046(11) 0.0106(14) C16 0.0394(13) 0.0421(14) 0.0370(13) 0.0069(10) 0.0102(10) 0.0112(10) C17 0.0322(13) 0.0668(19) 0.0652(17) 0.0038(14) -0.0086(12) -0.0073(13) C18 0.0351(13) 0.0525(17) 0.0716(18) 0.0044(14) -0.0007(12) -0.0119(12) C19 0.109(3) 0.081(3) 0.084(3) 0.0026(19) 0.033(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.9036(16) . ? Fe1 N3 1.9099(19) . ? Fe1 N4 1.911(2) . ? Fe1 O2 1.9154(16) . ? Fe1 C1 1.976(3) . ? Fe1 C2 1.987(3) . ? Fe1 K1 3.6756(8) 1_565 ? Fe1 K1 3.8459(9) 2_655 ? K1 O1 2.7445(17) 1_545 ? K1 N1 2.769(2) . ? K1 O3 2.860(3) . ? K1 O2 2.9302(17) 2_645 ? K1 O2 2.9447(17) 1_545 ? K1 C1 3.057(2) 2_645 ? K1 N1 3.069(2) 2_645 ? K1 C2 3.342(2) 1_545 ? K1 Fe1 3.6756(8) 1_545 ? K1 Fe1 3.8459(9) 2_645 ? K1 K1 4.0433(8) 2_655 ? K1 K1 4.0433(8) 2_645 ? O1 C9 1.317(3) . ? O1 K1 2.7445(17) 1_565 ? O2 C16 1.312(3) . ? O2 K1 2.9302(17) 2_655 ? O2 K1 2.9447(17) 1_565 ? O3 C19 1.382(4) . ? O3 H20 0.9824 . ? N1 C1 1.145(3) . ? N1 K1 3.069(2) 2_655 ? N2 C2 1.142(3) . ? N3 C3 1.277(3) . ? N3 C17 1.473(3) . ? N4 C10 1.277(3) . ? N4 C18 1.466(3) . ? C1 K1 3.057(2) 2_655 ? C2 K1 3.342(2) 1_565 ? C3 C4 1.431(4) . ? C3 H7 0.9300 . ? C4 C5 1.408(4) . ? C4 C9 1.421(3) . ? C5 C6 1.373(5) . ? C5 H5 0.9300 . ? C6 C7 1.376(5) . ? C6 H4 0.9300 . ? C7 C8 1.373(4) . ? C7 H3 0.9300 . ? C8 C9 1.399(4) . ? C8 H2 0.9300 . ? C10 C11 1.430(4) . ? C10 H10 0.9300 . ? C11 C12 1.410(4) . ? C11 C16 1.427(4) . ? C12 C13 1.352(5) . ? C12 H12 0.9300 . ? C13 C14 1.386(5) . ? C13 H13 0.9300 . ? C14 C15 1.374(4) . ? C14 H14 0.9300 . ? C15 C16 1.401(4) . ? C15 H15 0.9300 . ? C17 C18 1.508(4) . ? C17 H8A 0.9700 . ? C17 H8B 0.9700 . ? C18 H9A 0.9700 . ? C18 H9B 0.9700 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 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 O1 Fe1 N3 94.10(8) . . ? O1 Fe1 N4 177.37(8) . . ? N3 Fe1 N4 84.30(9) . . ? O1 Fe1 O2 88.37(7) . . ? N3 Fe1 O2 176.44(8) . . ? N4 Fe1 O2 93.33(8) . . ? O1 Fe1 C1 89.36(9) . . ? N3 Fe1 C1 87.43(9) . . ? N4 Fe1 C1 92.65(9) . . ? O2 Fe1 C1 90.04(8) . . ? O1 Fe1 C2 90.70(8) . . ? N3 Fe1 C2 93.13(9) . . ? N4 Fe1 C2 87.30(9) . . ? O2 Fe1 C2 89.40(8) . . ? C1 Fe1 C2 179.44(9) . . ? O1 Fe1 K1 46.68(5) . 1_565 ? N3 Fe1 K1 130.63(7) . 1_565 ? N4 Fe1 K1 133.44(7) . 1_565 ? O2 Fe1 K1 52.83(5) . 1_565 ? C1 Fe1 K1 115.18(7) . 1_565 ? C2 Fe1 K1 64.50(7) . 1_565 ? O1 Fe1 K1 63.87(5) . 2_655 ? N3 Fe1 K1 131.28(7) . 2_655 ? N4 Fe1 K1 118.74(6) . 2_655 ? O2 Fe1 K1 47.92(5) . 2_655 ? C1 Fe1 K1 52.04(6) . 2_655 ? C2 Fe1 K1 127.52(7) . 2_655 ? K1 Fe1 K1 64.990(14) 1_565 2_655 ? O1 K1 N1 94.86(6) 1_545 . ? O1 K1 O3 120.43(7) 1_545 . ? N1 K1 O3 73.44(7) . . ? O1 K1 O2 113.64(5) 1_545 2_645 ? N1 K1 O2 78.03(6) . 2_645 ? O3 K1 O2 119.92(7) . 2_645 ? O1 K1 O2 55.66(5) 1_545 1_545 ? N1 K1 O2 134.10(6) . 1_545 ? O3 K1 O2 91.31(7) . 1_545 ? O2 K1 O2 142.84(5) 2_645 1_545 ? O1 K1 C1 114.33(6) 1_545 2_645 ? N1 K1 C1 130.89(7) . 2_645 ? O3 K1 C1 116.74(7) . 2_645 ? O2 K1 C1 54.70(6) 2_645 2_645 ? O2 K1 C1 94.81(6) 1_545 2_645 ? O1 K1 N1 100.43(6) 1_545 2_645 ? N1 K1 N1 152.24(5) . 2_645 ? O3 K1 N1 116.69(7) . 2_645 ? O2 K1 N1 74.65(6) 2_645 2_645 ? O2 K1 N1 73.27(5) 1_545 2_645 ? C1 K1 N1 21.55(6) 2_645 2_645 ? O1 K1 C2 53.02(6) 1_545 1_545 ? N1 K1 C2 83.14(6) . 1_545 ? O3 K1 C2 67.51(7) . 1_545 ? O2 K1 C2 155.96(5) 2_645 1_545 ? O2 K1 C2 51.31(5) 1_545 1_545 ? C1 K1 C2 145.97(7) 2_645 1_545 ? N1 K1 C2 124.51(6) 2_645 1_545 ? O1 K1 Fe1 30.30(3) 1_545 1_545 ? N1 K1 Fe1 106.15(5) . 1_545 ? O3 K1 Fe1 96.08(6) . 1_545 ? O2 K1 Fe1 142.79(4) 2_645 1_545 ? O2 K1 Fe1 31.22(3) 1_545 1_545 ? C1 K1 Fe1 119.11(5) 2_645 1_545 ? N1 K1 Fe1 98.60(5) 2_645 1_545 ? C2 K1 Fe1 32.46(5) 1_545 1_545 ? O1 K1 Fe1 129.61(4) 1_545 2_645 ? N1 K1 Fe1 100.40(5) . 2_645 ? O3 K1 Fe1 109.95(6) . 2_645 ? O2 K1 Fe1 29.02(3) 2_645 2_645 ? O2 K1 Fe1 125.43(3) 1_545 2_645 ? C1 K1 Fe1 30.64(5) 2_645 2_645 ? N1 K1 Fe1 52.19(4) 2_645 2_645 ? C2 K1 Fe1 175.00(4) 1_545 2_645 ? Fe1 K1 Fe1 147.147(19) 1_545 2_645 ? O1 K1 K1 137.83(4) 1_545 2_655 ? N1 K1 K1 49.32(5) . 2_655 ? O3 K1 K1 75.19(6) . 2_655 ? O2 K1 K1 46.66(3) 2_645 2_655 ? O2 K1 K1 164.68(4) 1_545 2_655 ? C1 K1 K1 85.13(5) 2_645 2_655 ? N1 K1 K1 106.04(5) 2_645 2_655 ? C2 K1 K1 126.38(5) 1_545 2_655 ? Fe1 K1 K1 155.24(2) 1_545 2_655 ? Fe1 K1 K1 55.469(15) 2_645 2_655 ? O1 K1 K1 57.53(4) 1_545 2_645 ? N1 K1 K1 147.58(6) . 2_645 ? O3 K1 K1 133.21(6) . 2_645 ? O2 K1 K1 96.77(4) 2_645 2_645 ? O2 K1 K1 46.36(3) 1_545 2_645 ? C1 K1 K1 60.68(5) 2_645 2_645 ? N1 K1 K1 43.17(4) 2_645 2_645 ? C2 K1 K1 91.13(5) 1_545 2_645 ? Fe1 K1 K1 59.541(16) 1_545 2_645 ? Fe1 K1 K1 87.73(2) 2_645 2_645 ? K1 K1 K1 141.98(3) 2_655 2_645 ? C9 O1 Fe1 125.26(15) . . ? C9 O1 K1 129.24(14) . 1_565 ? Fe1 O1 K1 103.02(6) . 1_565 ? C16 O2 Fe1 123.63(15) . . ? C16 O2 K1 126.25(13) . 2_655 ? Fe1 O2 K1 103.06(6) . 2_655 ? C16 O2 K1 110.65(14) . 1_565 ? Fe1 O2 K1 95.95(6) . 1_565 ? K1 O2 K1 86.98(4) 2_655 1_565 ? C19 O3 K1 137.1(2) . . ? C19 O3 H20 108.9 . . ? K1 O3 H20 94.9 . . ? C1 N1 K1 136.6(2) . . ? C1 N1 K1 78.63(16) . 2_655 ? K1 N1 K1 87.50(6) . 2_655 ? C3 N3 C17 121.4(2) . . ? C3 N3 Fe1 125.64(18) . . ? C17 N3 Fe1 112.98(17) . . ? C10 N4 C18 121.3(2) . . ? C10 N4 Fe1 125.55(18) . . ? C18 N4 Fe1 113.14(17) . . ? N1 C1 Fe1 177.1(2) . . ? N1 C1 K1 79.82(15) . 2_655 ? Fe1 C1 K1 97.32(9) . 2_655 ? N2 C2 Fe1 177.9(2) . . ? N2 C2 K1 95.99(18) . 1_565 ? Fe1 C2 K1 83.03(7) . 1_565 ? N3 C3 C4 125.4(2) . . ? N3 C3 H7 117.3 . . ? C4 C3 H7 117.3 . . ? C5 C4 C9 119.0(3) . . ? C5 C4 C3 117.8(2) . . ? C9 C4 C3 123.0(2) . . ? C6 C5 C4 121.4(3) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C7 119.5(3) . . ? C5 C6 H4 120.3 . . ? C7 C6 H4 120.3 . . ? C8 C7 C6 120.7(3) . . ? C8 C7 H3 119.6 . . ? C6 C7 H3 119.6 . . ? C7 C8 C9 121.8(3) . . ? C7 C8 H2 119.1 . . ? C9 C8 H2 119.1 . . ? O1 C9 C8 118.4(2) . . ? O1 C9 C4 124.0(2) . . ? C8 C9 C4 117.6(2) . . ? N4 C10 C11 124.7(2) . . ? N4 C10 H10 117.7 . . ? C11 C10 H10 117.7 . . ? C12 C11 C16 119.0(3) . . ? C12 C11 C10 118.1(3) . . ? C16 C11 C10 122.8(2) . . ? C13 C12 C11 122.4(3) . . ? C13 C12 H12 118.8 . . ? C11 C12 H12 118.8 . . ? C12 C13 C14 118.5(3) . . ? C12 C13 H13 120.8 . . ? C14 C13 H13 120.8 . . ? C15 C14 C13 121.7(3) . . ? C15 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? C14 C15 C16 121.1(3) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? O2 C16 C15 118.6(2) . . ? O2 C16 C11 124.2(2) . . ? C15 C16 C11 117.3(2) . . ? N3 C17 C18 107.29(19) . . ? N3 C17 H8A 110.3 . . ? C18 C17 H8A 110.3 . . ? N3 C17 H8B 110.3 . . ? C18 C17 H8B 110.3 . . ? H8A C17 H8B 108.5 . . ? N4 C18 C17 106.1(2) . . ? N4 C18 H9A 110.5 . . ? C17 C18 H9A 110.5 . . ? N4 C18 H9B 110.5 . . ? C17 C18 H9B 110.5 . . ? H9A C18 H9B 108.7 . . ? O3 C19 H19A 109.5 . . ? O3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.498 _refine_diff_density_min -0.323 _refine_diff_density_rms 0.050 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 732678' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H54 Fe2 Mn N12 O8' _chemical_formula_weight 1213.77 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 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 23.973(5) _cell_length_b 14.332(3) _cell_length_c 17.683(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.901(4) _cell_angle_gamma 90.00 _cell_volume 6018(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.340 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2508 _exptl_absorpt_coefficient_mu 0.744 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8594 _exptl_absorpt_correction_T_max 0.9030 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II CCD area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14594 _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_sigmaI/netI 0.0641 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5259 _reflns_number_gt 3245 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2001)' _computing_data_reduction SAINT-Plus _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material XP _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1208P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5259 _refine_ls_number_parameters 376 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1041 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.1986 _refine_ls_wR_factor_gt 0.1674 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.059 _refine_ls_shift/su_mean 0.006 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 0.67638(3) 0.29352(5) 0.80765(3) 0.0474(3) Uani 1 1 d . . . Mn1 Mn 0.5000 0.50328(7) 0.7500 0.0464(3) Uani 1 2 d S . . O1 O 0.64143(15) 0.1745(3) 0.7961(2) 0.0684(10) Uani 1 1 d . . . O2 O 0.67319(15) 0.2916(2) 0.69919(18) 0.0585(9) Uani 1 1 d . . . O3 O 0.5699(2) 0.7511(4) 0.1073(3) 0.1233(18) Uani 1 1 d . . . H3 H 0.5955 0.7325 0.1392 0.185 Uiso 1 1 d R . . O4 O 0.6823(5) 0.0970(6) 0.6405(5) 0.139(5) Uani 0.50 1 d PD . . H4A H 0.6607 0.0776 0.6029 0.167 Uiso 0.50 1 d PRD . . H4B H 0.6669 0.0790 0.6773 0.167 Uiso 0.50 1 d PRD . . O5 O 0.9128(7) 0.3159(18) 0.8381(13) 0.34(2) Uani 0.50 1 d PD . . H5A H 0.9140 0.2631 0.8574 0.410 Uiso 0.50 1 d PRD . . H5B H 0.9388 0.3308 0.8153 0.410 Uiso 0.50 1 d PRD . . N1 N 0.56347(18) 0.3986(3) 0.7872(2) 0.0564(10) Uani 1 1 d . . . N2 N 0.7949(2) 0.2082(4) 0.8307(3) 0.0958(18) Uani 1 1 d . . . N3 N 0.67944(19) 0.2980(3) 0.9145(2) 0.0623(12) Uani 1 1 d . . . N4 N 0.70939(18) 0.4134(3) 0.8179(2) 0.0594(11) Uani 1 1 d . . . N5 N 0.46639(16) 0.5349(3) 0.8602(2) 0.0504(10) Uani 1 1 d . . . N6 N 0.55879(17) 0.6102(3) 0.8152(2) 0.0591(11) Uani 1 1 d . . . C1 C 0.6035(2) 0.3551(4) 0.7961(3) 0.0511(12) Uani 1 1 d . . . C2 C 0.7500(3) 0.2384(4) 0.8196(3) 0.0680(15) Uani 1 1 d . . . C3 C 0.6561(3) 0.2406(6) 0.9549(4) 0.0819(19) Uani 1 1 d . . . H7 H 0.6596 0.2516 1.0072 0.098 Uiso 1 1 calc R . . C4 C 0.6243(3) 0.1591(6) 0.9258(4) 0.086(2) Uani 1 1 d . . . C5 C 0.5997(3) 0.1027(6) 0.9795(5) 0.114(3) Uani 1 1 d . . . H5 H 0.6037 0.1189 1.0308 0.136 Uiso 1 1 calc R . . C6 C 0.5708(4) 0.0262(7) 0.9544(7) 0.129(3) Uani 1 1 d U . . H6 H 0.5546 -0.0097 0.9894 0.155 Uiso 1 1 calc R . . C7 C 0.5641(4) -0.0018(6) 0.8794(7) 0.125(3) Uani 1 1 d U . . H3A H 0.5433 -0.0550 0.8642 0.150 Uiso 1 1 calc R . . C8 C 0.5882(3) 0.0487(5) 0.8278(5) 0.096(2) Uani 1 1 d . . . H2 H 0.5846 0.0284 0.7774 0.116 Uiso 1 1 calc R . . C9 C 0.6184(2) 0.1310(4) 0.8483(4) 0.0761(17) Uani 1 1 d . . . C10 C 0.7308(2) 0.4572(4) 0.7668(3) 0.0639(14) Uani 1 1 d . . . H10 H 0.7460 0.5158 0.7794 0.077 Uiso 1 1 calc R . . C11 C 0.7332(2) 0.4234(4) 0.6909(3) 0.0568(13) Uani 1 1 d . . . C12 C 0.7663(2) 0.4748(4) 0.6451(3) 0.0677(15) Uani 1 1 d . . . H12 H 0.7848 0.5282 0.6651 0.081 Uiso 1 1 calc R . . C13 C 0.7716(2) 0.4486(5) 0.5738(3) 0.0716(16) Uani 1 1 d . . . H13 H 0.7945 0.4822 0.5452 0.086 Uiso 1 1 calc R . . C14 C 0.7426(2) 0.3711(4) 0.5430(3) 0.0664(15) Uani 1 1 d . . . H14 H 0.7454 0.3533 0.4931 0.080 Uiso 1 1 calc R . . C15 C 0.7096(2) 0.3198(4) 0.5856(3) 0.0617(14) Uani 1 1 d . . . H15 H 0.6895 0.2688 0.5637 0.074 Uiso 1 1 calc R . . C16 C 0.70575(19) 0.3436(4) 0.6611(3) 0.0507(12) Uani 1 1 d . . . C17 C 0.7074(3) 0.4538(5) 0.8932(3) 0.0782(17) Uani 1 1 d . . . H9A H 0.6720 0.4863 0.8944 0.094 Uiso 1 1 calc R . . H9B H 0.7380 0.4978 0.9057 0.094 Uiso 1 1 calc R . . C18 C 0.7129(3) 0.3744(5) 0.9486(3) 0.0779(18) Uani 1 1 d . . . H8A H 0.7520 0.3557 0.9600 0.094 Uiso 1 1 calc R . . H8B H 0.6998 0.3932 0.9958 0.094 Uiso 1 1 calc R . . C19 C 0.6050(3) 0.6441(4) 0.7926(3) 0.0780(17) Uani 1 1 d . . . H19 H 0.6151 0.6221 0.7470 0.094 Uiso 1 1 calc R . . C20 C 0.6388(3) 0.7095(5) 0.8319(4) 0.090(2) Uani 1 1 d . . . H20 H 0.6710 0.7309 0.8134 0.108 Uiso 1 1 calc R . . C21 C 0.6244(3) 0.7428(5) 0.8994(4) 0.098(2) Uani 1 1 d . . . H21 H 0.6463 0.7881 0.9271 0.117 Uiso 1 1 calc R . . C22 C 0.5769(3) 0.7079(4) 0.9255(3) 0.0801(18) Uani 1 1 d . . . H22 H 0.5665 0.7288 0.9713 0.096 Uiso 1 1 calc R . . C23 C 0.5445(2) 0.6409(4) 0.8821(3) 0.0546(12) Uani 1 1 d . . . C24 C 0.49382(19) 0.5988(3) 0.9076(2) 0.0487(11) Uani 1 1 d . . . C25 C 0.4771(2) 0.6189(4) 0.9770(3) 0.0617(14) Uani 1 1 d . . . H24 H 0.4972 0.6614 1.0099 0.074 Uiso 1 1 calc R . . C26 C 0.4303(2) 0.5754(4) 0.9972(3) 0.0676(15) Uani 1 1 d . . . H25 H 0.4182 0.5889 1.0438 0.081 Uiso 1 1 calc R . . C27 C 0.4015(2) 0.5123(4) 0.9488(3) 0.0659(15) Uani 1 1 d . . . H26 H 0.3696 0.4824 0.9614 0.079 Uiso 1 1 calc R . . C28 C 0.4211(2) 0.4945(4) 0.8813(3) 0.0576(13) Uani 1 1 d . . . H27 H 0.4016 0.4515 0.8482 0.069 Uiso 1 1 calc R . . C29 C 0.5285(3) 0.7916(6) 0.1433(4) 0.102(2) Uani 1 1 d . . . H29A H 0.5455 0.8341 0.1817 0.153 Uiso 1 1 calc R . . H29B H 0.5085 0.7440 0.1668 0.153 Uiso 1 1 calc R . . H29C H 0.5027 0.8249 0.1066 0.153 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 Fe1 0.0352(4) 0.0647(5) 0.0432(4) 0.0000(3) 0.0089(3) 0.0044(3) Mn1 0.0359(5) 0.0663(7) 0.0374(5) 0.000 0.0060(4) 0.000 O1 0.056(2) 0.073(2) 0.079(2) 0.007(2) 0.0194(19) -0.0027(19) O2 0.053(2) 0.074(2) 0.0495(18) -0.0116(16) 0.0113(16) -0.0104(17) O3 0.089(4) 0.200(5) 0.077(3) -0.022(3) 0.000(3) 0.034(4) O4 0.233(13) 0.114(7) 0.073(5) 0.018(5) 0.036(6) 0.152(9) O5 0.145(14) 0.51(4) 0.34(3) -0.35(3) -0.077(16) 0.036(19) N1 0.047(2) 0.076(3) 0.046(2) 0.001(2) 0.0052(18) 0.009(2) N2 0.053(3) 0.132(5) 0.105(4) 0.014(3) 0.019(3) 0.026(3) N3 0.049(3) 0.090(3) 0.049(2) 0.002(2) 0.011(2) 0.011(2) N4 0.053(3) 0.076(3) 0.050(2) -0.009(2) 0.009(2) -0.002(2) N5 0.038(2) 0.068(3) 0.046(2) 0.0021(19) 0.0086(17) -0.002(2) N6 0.050(3) 0.081(3) 0.047(2) -0.001(2) 0.0112(19) -0.012(2) C1 0.045(3) 0.068(3) 0.041(2) 0.002(2) 0.010(2) 0.001(3) C2 0.054(4) 0.091(4) 0.061(3) -0.005(3) 0.015(3) 0.006(3) C3 0.063(4) 0.122(6) 0.064(4) 0.016(4) 0.019(3) 0.034(4) C4 0.062(4) 0.112(5) 0.089(5) 0.045(4) 0.033(3) 0.028(4) C5 0.095(6) 0.130(7) 0.123(6) 0.047(5) 0.043(5) 0.032(5) C6 0.118(4) 0.131(4) 0.143(5) 0.031(4) 0.032(4) -0.008(4) C7 0.095(5) 0.111(5) 0.171(7) 0.038(5) 0.027(5) -0.011(4) C8 0.071(4) 0.086(5) 0.136(6) 0.033(4) 0.028(4) -0.009(4) C9 0.050(3) 0.078(4) 0.105(5) 0.027(4) 0.026(3) 0.015(3) C10 0.054(3) 0.074(4) 0.063(3) -0.014(3) 0.006(3) -0.006(3) C11 0.044(3) 0.068(3) 0.058(3) -0.002(3) 0.010(2) 0.000(3) C12 0.057(3) 0.074(4) 0.073(4) 0.008(3) 0.011(3) -0.007(3) C13 0.061(4) 0.084(4) 0.074(4) 0.024(3) 0.022(3) 0.008(3) C14 0.065(4) 0.087(4) 0.051(3) 0.015(3) 0.022(3) 0.020(3) C15 0.055(3) 0.075(3) 0.055(3) -0.005(3) 0.006(2) 0.008(3) C16 0.037(3) 0.067(3) 0.049(3) 0.001(2) 0.013(2) 0.003(2) C17 0.079(4) 0.103(5) 0.053(3) -0.023(3) 0.009(3) 0.003(4) C18 0.066(4) 0.118(5) 0.049(3) -0.008(3) 0.003(3) 0.023(4) C19 0.068(4) 0.106(5) 0.061(3) -0.003(3) 0.013(3) -0.034(4) C20 0.073(4) 0.121(6) 0.076(4) -0.004(4) 0.013(3) -0.041(4) C21 0.093(5) 0.111(5) 0.084(5) -0.004(4) -0.003(4) -0.054(5) C22 0.081(4) 0.098(5) 0.061(3) -0.009(3) 0.008(3) -0.028(4) C23 0.054(3) 0.065(3) 0.042(3) 0.000(2) -0.001(2) -0.010(3) C24 0.045(3) 0.059(3) 0.041(2) 0.000(2) 0.001(2) 0.004(2) C25 0.057(3) 0.075(4) 0.053(3) -0.016(3) 0.009(2) -0.005(3) C26 0.066(4) 0.088(4) 0.053(3) 0.000(3) 0.020(3) 0.012(3) C27 0.051(3) 0.096(4) 0.054(3) -0.001(3) 0.020(2) -0.005(3) C28 0.045(3) 0.078(4) 0.050(3) -0.003(2) 0.009(2) -0.004(3) C29 0.068(4) 0.145(7) 0.094(5) -0.004(4) 0.013(4) 0.016(4) _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 N3 1.883(4) . ? Fe1 N4 1.889(4) . ? Fe1 O1 1.899(4) . ? Fe1 O2 1.909(3) . ? Fe1 C2 1.918(6) . ? Fe1 C1 1.943(5) . ? Mn1 N1 2.173(4) 2_656 ? Mn1 N1 2.173(4) . ? Mn1 N5 2.255(4) . ? Mn1 N5 2.255(4) 2_656 ? Mn1 N6 2.284(4) . ? Mn1 N6 2.284(4) 2_656 ? O1 C9 1.298(7) . ? O2 C16 1.327(6) . ? O3 C29 1.379(8) . ? O3 H3 0.8200 . ? O4 H4A 0.8324 . ? O4 H4B 0.8307 . ? O5 H5A 0.8302 . ? O5 H5B 0.8150 . ? N1 C1 1.137(6) . ? N2 C2 1.153(7) . ? N3 C3 1.270(8) . ? N3 C18 1.440(7) . ? N4 C10 1.266(7) . ? N4 C17 1.459(6) . ? N5 C28 1.329(6) . ? N5 C24 1.351(6) . ? N6 C19 1.320(7) . ? N6 C23 1.349(6) . ? C3 C4 1.449(10) . ? C3 H7 0.9300 . ? C4 C9 1.416(10) . ? C4 C5 1.434(9) . ? C5 C6 1.338(12) . ? C5 H5 0.9300 . ? C6 C7 1.375(13) . ? C6 H6 0.9300 . ? C7 C8 1.353(10) . ? C7 H3A 0.9300 . ? C8 C9 1.406(9) . ? C8 H2 0.9300 . ? C10 C11 1.436(7) . ? C10 H10 0.9300 . ? C11 C16 1.388(7) . ? C11 C12 1.415(7) . ? C12 C13 1.340(8) . ? C12 H12 0.9300 . ? C13 C14 1.382(8) . ? C13 H13 0.9300 . ? C14 C15 1.378(7) . ? C14 H14 0.9300 . ? C15 C16 1.393(6) . ? C15 H15 0.9300 . ? C17 C18 1.495(8) . ? C17 H9A 0.9700 . ? C17 H9B 0.9700 . ? C18 H8A 0.9700 . ? C18 H8B 0.9700 . ? C19 C20 1.365(8) . ? C19 H19 0.9300 . ? C20 C21 1.373(9) . ? C20 H20 0.9300 . ? C21 C22 1.381(9) . ? C21 H21 0.9300 . ? C22 C23 1.396(7) . ? C22 H22 0.9300 . ? C23 C24 1.481(7) . ? C24 C25 1.373(7) . ? C25 C26 1.372(7) . ? C25 H24 0.9300 . ? C26 C27 1.366(8) . ? C26 H25 0.9300 . ? C27 C28 1.364(7) . ? C27 H26 0.9300 . ? C28 H27 0.9300 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 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 N3 Fe1 N4 85.1(2) . . ? N3 Fe1 O1 95.39(19) . . ? N4 Fe1 O1 178.51(17) . . ? N3 Fe1 O2 178.88(18) . . ? N4 Fe1 O2 93.91(16) . . ? O1 Fe1 O2 85.59(15) . . ? N3 Fe1 C2 89.7(2) . . ? N4 Fe1 C2 89.8(2) . . ? O1 Fe1 C2 91.6(2) . . ? O2 Fe1 C2 90.79(19) . . ? N3 Fe1 C1 90.04(18) . . ? N4 Fe1 C1 87.44(19) . . ? O1 Fe1 C1 91.14(19) . . ? O2 Fe1 C1 89.39(17) . . ? C2 Fe1 C1 177.3(2) . . ? N1 Mn1 N1 92.7(2) 2_656 . ? N1 Mn1 N5 94.68(15) 2_656 . ? N1 Mn1 N5 101.29(14) . . ? N1 Mn1 N5 101.29(14) 2_656 2_656 ? N1 Mn1 N5 94.68(14) . 2_656 ? N5 Mn1 N5 156.8(2) . 2_656 ? N1 Mn1 N6 166.81(14) 2_656 . ? N1 Mn1 N6 87.30(16) . . ? N5 Mn1 N6 72.42(14) . . ? N5 Mn1 N6 91.85(14) 2_656 . ? N1 Mn1 N6 87.30(16) 2_656 2_656 ? N1 Mn1 N6 166.81(14) . 2_656 ? N5 Mn1 N6 91.85(14) . 2_656 ? N5 Mn1 N6 72.42(14) 2_656 2_656 ? N6 Mn1 N6 95.7(2) . 2_656 ? C9 O1 Fe1 125.4(4) . . ? C16 O2 Fe1 123.8(3) . . ? C29 O3 H3 109.7 . . ? H4A O4 H4B 103.3 . . ? H5A O5 H5B 117.0 . . ? C1 N1 Mn1 164.3(4) . . ? C3 N3 C18 121.5(5) . . ? C3 N3 Fe1 125.7(5) . . ? C18 N3 Fe1 112.9(4) . . ? C10 N4 C17 121.4(5) . . ? C10 N4 Fe1 126.1(4) . . ? C17 N4 Fe1 112.5(4) . . ? C28 N5 C24 117.9(4) . . ? C28 N5 Mn1 124.0(3) . . ? C24 N5 Mn1 118.1(3) . . ? C19 N6 C23 118.0(5) . . ? C19 N6 Mn1 125.4(4) . . ? C23 N6 Mn1 116.6(3) . . ? N1 C1 Fe1 173.4(5) . . ? N2 C2 Fe1 176.0(6) . . ? N3 C3 C4 125.0(6) . . ? N3 C3 H7 117.5 . . ? C4 C3 H7 117.5 . . ? C9 C4 C5 118.9(8) . . ? C9 C4 C3 123.4(6) . . ? C5 C4 C3 117.6(8) . . ? C6 C5 C4 118.9(10) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C5 C6 C7 123.1(10) . . ? C5 C6 H6 118.5 . . ? C7 C6 H6 118.5 . . ? C8 C7 C6 119.3(9) . . ? C8 C7 H3A 120.3 . . ? C6 C7 H3A 120.3 . . ? C7 C8 C9 121.8(9) . . ? C7 C8 H2 119.1 . . ? C9 C8 H2 119.1 . . ? O1 C9 C8 118.3(7) . . ? O1 C9 C4 123.7(6) . . ? C8 C9 C4 117.9(6) . . ? N4 C10 C11 124.9(5) . . ? N4 C10 H10 117.6 . . ? C11 C10 H10 117.6 . . ? C16 C11 C12 119.1(5) . . ? C16 C11 C10 123.7(5) . . ? C12 C11 C10 117.2(5) . . ? C13 C12 C11 121.7(6) . . ? C13 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? C12 C13 C14 119.3(5) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C15 C14 C13 120.6(5) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 120.8(5) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? O2 C16 C11 123.5(4) . . ? O2 C16 C15 118.0(5) . . ? C11 C16 C15 118.4(5) . . ? N4 C17 C18 106.5(5) . . ? N4 C17 H9A 110.4 . . ? C18 C17 H9A 110.4 . . ? N4 C17 H9B 110.4 . . ? C18 C17 H9B 110.4 . . ? H9A C17 H9B 108.6 . . ? N3 C18 C17 108.1(4) . . ? N3 C18 H8A 110.1 . . ? C17 C18 H8A 110.1 . . ? N3 C18 H8B 110.1 . . ? C17 C18 H8B 110.1 . . ? H8A C18 H8B 108.4 . . ? N6 C19 C20 124.3(6) . . ? N6 C19 H19 117.8 . . ? C20 C19 H19 117.8 . . ? C19 C20 C21 118.5(6) . . ? C19 C20 H20 120.7 . . ? C21 C20 H20 120.7 . . ? C20 C21 C22 118.8(6) . . ? C20 C21 H21 120.6 . . ? C22 C21 H21 120.6 . . ? C21 C22 C23 119.2(6) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? N6 C23 C22 121.1(5) . . ? N6 C23 C24 116.9(4) . . ? C22 C23 C24 122.0(5) . . ? N5 C24 C25 121.3(4) . . ? N5 C24 C23 115.9(4) . . ? C25 C24 C23 122.7(4) . . ? C26 C25 C24 119.2(5) . . ? C26 C25 H24 120.4 . . ? C24 C25 H24 120.4 . . ? C27 C26 C25 119.9(5) . . ? C27 C26 H25 120.0 . . ? C25 C26 H25 120.0 . . ? C26 C27 C28 117.8(5) . . ? C26 C27 H26 121.1 . . ? C28 C27 H26 121.1 . . ? N5 C28 C27 123.9(5) . . ? N5 C28 H27 118.1 . . ? C27 C28 H27 118.1 . . ? O3 C29 H29A 109.5 . . ? O3 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O3 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.915 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.086 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 732679' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H60 Fe2 Mn N12 O8' _chemical_formula_weight 1291.88 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 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 23.8689(18) _cell_length_b 13.9731(8) _cell_length_c 18.2380(11) _cell_angle_alpha 90.00 _cell_angle_beta 97.358(4) _cell_angle_gamma 90.00 _cell_volume 6032.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 1.432 _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2676 _exptl_absorpt_coefficient_mu 0.747 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8962 _exptl_absorpt_correction_T_max 0.9223 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II CCD area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24707 _diffrn_reflns_av_R_equivalents 0.0386 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5326 _reflns_number_gt 4150 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2001)' _computing_data_reduction SAINT-Plus _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material XP _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^)+(0.0884P)^2^+9.9909P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5326 _refine_ls_number_parameters 394 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1549 _refine_ls_wR_factor_gt 0.1408 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 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 0.317665(19) 0.70628(4) 0.18207(3) 0.04078(18) Uani 1 1 d . . . Mn1 Mn 0.5000 0.50702(5) 0.2500 0.0388(2) Uani 1 2 d S . . O1 O 0.32357(10) 0.71310(17) 0.28678(13) 0.0461(6) Uani 1 1 d . . . O2 O 0.34820(10) 0.83145(18) 0.17985(14) 0.0514(6) Uani 1 1 d . . . O3 O 0.4280(8) 0.8457(8) 0.3370(5) 0.399(11) Uani 1 1 d D . . H1O3 H 0.4279 0.7849 0.3384 0.479 Uiso 1 1 d R . . O4 O 0.0655(10) 0.6971(14) 0.1747(11) 0.67(2) Uani 1 1 d . . . H104 H 0.0513 0.7326 0.1316 0.799 Uiso 1 1 d R . . N1 N 0.43725(13) 0.6109(2) 0.20461(17) 0.0507(7) Uani 1 1 d . . . N2 N 0.19471(15) 0.7866(3) 0.1680(2) 0.0775(12) Uani 1 1 d . . . N3 N 0.28635(12) 0.5802(2) 0.17914(16) 0.0471(7) Uani 1 1 d . . . N4 N 0.31268(12) 0.6907(2) 0.07734(17) 0.0495(8) Uani 1 1 d . . . N5 N 0.44388(11) 0.3920(2) 0.18648(16) 0.0456(7) Uani 1 1 d . . . N6 N 0.53800(11) 0.4766(2) 0.14519(16) 0.0417(7) Uani 1 1 d . . . C1 C 0.39508(14) 0.6505(3) 0.19341(18) 0.0422(8) Uani 1 1 d . . . C2 C 0.23957(16) 0.7582(3) 0.1742(2) 0.0509(9) Uani 1 1 d . . . C3 C 0.26489(16) 0.5391(3) 0.2321(2) 0.0530(9) Uani 1 1 d . . . H3 H 0.2495 0.4784 0.2232 0.064 Uiso 1 1 calc R . . C4 C 0.26297(15) 0.5797(3) 0.3036(2) 0.0480(8) Uani 1 1 d . . . C5 C 0.29241(14) 0.6641(3) 0.32774(19) 0.0423(8) Uani 1 1 d . . . C6 C 0.29016(16) 0.6938(3) 0.4009(2) 0.0515(9) Uani 1 1 d . . . H6 H 0.3099 0.7481 0.4188 0.062 Uiso 1 1 calc R . . C7 C 0.25883(17) 0.6432(3) 0.4465(2) 0.0584(10) Uani 1 1 d . . . H7 H 0.2579 0.6642 0.4947 0.070 Uiso 1 1 calc R . . C8 C 0.22904(17) 0.5627(3) 0.4224(2) 0.0623(11) Uani 1 1 d . . . H8 H 0.2074 0.5306 0.4534 0.075 Uiso 1 1 calc R . . C9 C 0.23166(17) 0.5306(3) 0.3525(2) 0.0585(10) Uani 1 1 d . . . H9 H 0.2124 0.4751 0.3366 0.070 Uiso 1 1 calc R . . C10 C 0.33752(18) 0.7436(3) 0.0332(2) 0.0611(11) Uani 1 1 d . . . H10 H 0.3336 0.7265 -0.0165 0.073 Uiso 1 1 calc R . . C11 C 0.36997(17) 0.8249(3) 0.0547(2) 0.0616(11) Uani 1 1 d . . . C12 C 0.3969(2) 0.8726(5) -0.0001(3) 0.0944(18) Uani 1 1 d . . . H12 H 0.3935 0.8477 -0.0477 0.113 Uiso 1 1 calc R . . C13 C 0.4274(3) 0.9535(6) 0.0155(4) 0.114(2) Uani 1 1 d . . . H13 H 0.4457 0.9819 -0.0210 0.137 Uiso 1 1 calc R . . C14 C 0.4316(2) 0.9941(4) 0.0849(4) 0.097(2) Uani 1 1 d . . . H14 H 0.4522 1.0502 0.0947 0.116 Uiso 1 1 calc R . . C15 C 0.40516(19) 0.9516(4) 0.1401(3) 0.0733(13) Uani 1 1 d . . . H15 H 0.4079 0.9798 0.1867 0.088 Uiso 1 1 calc R . . C16 C 0.37414(15) 0.8660(3) 0.1263(2) 0.0568(10) Uani 1 1 d . . . C17 C 0.28794(19) 0.5316(3) 0.1079(2) 0.0607(11) Uani 1 1 d . . . H17A H 0.2590 0.4826 0.1004 0.073 Uiso 1 1 calc R . . H17B H 0.3245 0.5020 0.1061 0.073 Uiso 1 1 calc R . . C18 C 0.27731(19) 0.6086(3) 0.0500(2) 0.0638(11) Uani 1 1 d . . . H18A H 0.2876 0.5863 0.0032 0.077 Uiso 1 1 calc R . . H18B H 0.2377 0.6265 0.0431 0.077 Uiso 1 1 calc R . . C19 C 0.39757(16) 0.3531(3) 0.2055(2) 0.0595(10) Uani 1 1 d . . . H19 H 0.3857 0.3714 0.2501 0.071 Uiso 1 1 calc R . . C20 C 0.36510(18) 0.2849(3) 0.1615(3) 0.0684(12) Uani 1 1 d . . . H20 H 0.3324 0.2595 0.1765 0.082 Uiso 1 1 calc R . . C21 C 0.38270(18) 0.2571(3) 0.0965(3) 0.0654(11) Uani 1 1 d . . . H21 H 0.3624 0.2112 0.0672 0.079 Uiso 1 1 calc R . . C22 C 0.43130(16) 0.2976(3) 0.0740(2) 0.0530(9) Uani 1 1 d . . . C23 C 0.46086(14) 0.3652(3) 0.1208(2) 0.0440(8) Uani 1 1 d . . . C24 C 0.45183(19) 0.2728(3) 0.0060(2) 0.0644(11) Uani 1 1 d . . . H24 H 0.4330 0.2265 -0.0245 0.077 Uiso 1 1 calc R . . C25 C 0.49787(18) 0.3154(3) -0.0145(2) 0.0605(10) Uani 1 1 d . . . H25 H 0.5099 0.2988 -0.0593 0.073 Uiso 1 1 calc R . . C26 C 0.52854(15) 0.3853(3) 0.0310(2) 0.0471(8) Uani 1 1 d . . . C27 C 0.57590(16) 0.4329(3) 0.0116(2) 0.0550(10) Uani 1 1 d . . . H27 H 0.5887 0.4195 -0.0334 0.066 Uiso 1 1 calc R . . C28 C 0.60364(16) 0.4988(3) 0.0579(2) 0.0567(10) Uani 1 1 d . . . H28 H 0.6356 0.5295 0.0454 0.068 Uiso 1 1 calc R . . C29 C 0.58303(15) 0.5192(3) 0.1245(2) 0.0502(9) Uani 1 1 d . . . H29 H 0.6018 0.5647 0.1557 0.060 Uiso 1 1 calc R . . C30 C 0.51063(14) 0.4099(2) 0.09933(18) 0.0411(8) Uani 1 1 d . . . C31 C 0.3754(9) 0.8981(13) 0.3517(13) 0.72(5) Uani 1 1 d D . . H31A H 0.3471 0.8916 0.3096 1.080 Uiso 1 1 d R . . H31B H 0.3841 0.9646 0.3600 1.080 Uiso 1 1 d R . . H31C H 0.3616 0.8717 0.3946 1.080 Uiso 1 1 d R . . C32 C 0.0954(8) 0.6210(8) 0.1933(6) 0.266(9) Uani 1 1 d . . . H32A H 0.1268 0.6183 0.1653 0.400 Uiso 1 1 calc R . . H32B H 0.0724 0.5651 0.1833 0.400 Uiso 1 1 calc R . . H32C H 0.1092 0.6237 0.2451 0.400 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 Fe1 0.0367(3) 0.0425(3) 0.0435(3) -0.0016(2) 0.0068(2) 0.0046(2) Mn1 0.0302(4) 0.0440(4) 0.0427(4) 0.000 0.0066(3) 0.000 O1 0.0471(13) 0.0488(15) 0.0437(13) -0.0040(11) 0.0106(11) -0.0069(11) O2 0.0514(14) 0.0463(15) 0.0584(16) 0.0027(12) 0.0150(12) 0.0008(12) O3 0.74(3) 0.191(10) 0.186(8) 0.020(7) -0.269(13) -0.094(14) O4 0.79(4) 0.52(3) 0.55(3) -0.32(2) -0.46(3) 0.41(3) N1 0.0420(17) 0.0533(19) 0.0560(19) 0.0026(15) 0.0028(14) 0.0090(15) N2 0.045(2) 0.100(3) 0.089(3) -0.002(2) 0.0153(19) 0.020(2) N3 0.0463(16) 0.0438(17) 0.0508(17) -0.0070(14) 0.0047(13) 0.0019(14) N4 0.0435(16) 0.057(2) 0.0479(17) -0.0029(15) 0.0037(14) 0.0154(14) N5 0.0354(14) 0.0520(18) 0.0500(17) 0.0021(14) 0.0077(12) -0.0057(13) N6 0.0339(14) 0.0443(17) 0.0482(16) -0.0020(13) 0.0098(12) -0.0030(12) C1 0.0425(19) 0.045(2) 0.0396(18) 0.0002(15) 0.0065(14) 0.0009(16) C2 0.049(2) 0.053(2) 0.052(2) -0.0022(18) 0.0114(17) 0.0040(18) C3 0.050(2) 0.042(2) 0.067(2) -0.0060(18) 0.0068(18) -0.0059(17) C4 0.0428(19) 0.042(2) 0.060(2) 0.0031(17) 0.0095(16) 0.0023(16) C5 0.0357(16) 0.046(2) 0.0462(19) 0.0002(16) 0.0071(14) 0.0057(15) C6 0.053(2) 0.053(2) 0.051(2) -0.0012(17) 0.0135(17) 0.0073(17) C7 0.062(2) 0.064(3) 0.053(2) 0.0082(19) 0.0184(19) 0.017(2) C8 0.053(2) 0.064(3) 0.073(3) 0.024(2) 0.022(2) 0.010(2) C9 0.056(2) 0.049(2) 0.073(3) 0.013(2) 0.018(2) 0.0002(18) C10 0.062(2) 0.077(3) 0.046(2) 0.010(2) 0.0130(19) 0.028(2) C11 0.054(2) 0.071(3) 0.062(3) 0.018(2) 0.016(2) 0.015(2) C12 0.089(4) 0.118(5) 0.083(4) 0.033(3) 0.035(3) 0.006(4) C13 0.098(5) 0.142(6) 0.111(5) 0.042(5) 0.048(4) -0.016(4) C14 0.066(3) 0.093(4) 0.134(6) 0.043(4) 0.021(3) -0.013(3) C15 0.061(3) 0.069(3) 0.091(3) 0.023(3) 0.015(2) -0.006(2) C16 0.042(2) 0.059(3) 0.071(3) 0.018(2) 0.0124(18) 0.0105(18) C17 0.068(3) 0.055(2) 0.059(2) -0.017(2) 0.005(2) 0.001(2) C18 0.066(3) 0.074(3) 0.049(2) -0.015(2) -0.0011(19) 0.010(2) C19 0.047(2) 0.069(3) 0.065(2) -0.001(2) 0.0146(18) -0.0102(19) C20 0.050(2) 0.076(3) 0.079(3) 0.000(2) 0.010(2) -0.029(2) C21 0.062(3) 0.059(3) 0.073(3) -0.003(2) -0.001(2) -0.019(2) C22 0.050(2) 0.049(2) 0.058(2) -0.0025(18) 0.0000(18) -0.0070(17) C23 0.0395(18) 0.0412(19) 0.051(2) 0.0021(16) 0.0025(15) -0.0014(15) C24 0.066(3) 0.059(3) 0.066(3) -0.018(2) -0.001(2) -0.004(2) C25 0.058(2) 0.067(3) 0.056(2) -0.014(2) 0.0065(19) 0.005(2) C26 0.0446(19) 0.047(2) 0.050(2) -0.0025(16) 0.0077(16) 0.0091(16) C27 0.051(2) 0.065(3) 0.053(2) -0.0028(19) 0.0206(18) 0.0097(19) C28 0.043(2) 0.064(3) 0.067(3) -0.001(2) 0.0227(19) -0.0034(18) C29 0.0407(19) 0.053(2) 0.058(2) -0.0052(18) 0.0131(17) -0.0068(16) C30 0.0376(17) 0.0425(19) 0.0431(18) 0.0012(15) 0.0048(14) 0.0043(15) C31 0.89(7) 0.23(2) 0.84(6) 0.25(3) -0.69(6) -0.32(3) C32 0.54(3) 0.127(8) 0.119(8) 0.021(7) 0.005(12) -0.095(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 O2 1.897(3) . ? Fe1 O1 1.899(2) . ? Fe1 N4 1.911(3) . ? Fe1 N3 1.911(3) . ? Fe1 C2 1.988(4) . ? Fe1 C1 1.992(3) . ? Mn1 N1 2.172(3) 2_655 ? Mn1 N1 2.172(3) . ? Mn1 N6 2.259(3) . ? Mn1 N6 2.259(3) 2_655 ? Mn1 N5 2.307(3) . ? Mn1 N5 2.307(3) 2_655 ? O1 C5 1.312(4) . ? O2 C16 1.313(4) . ? O3 C31 1.507(19) . ? O3 H1O3 0.8500 . ? O4 C32 1.301(18) . ? O4 H104 0.9544 . ? N1 C1 1.144(4) . ? N2 C2 1.134(5) . ? N3 C3 1.286(5) . ? N3 C17 1.471(5) . ? N4 C10 1.291(5) . ? N4 C18 1.473(5) . ? N5 C19 1.318(5) . ? N5 C23 1.365(5) . ? N6 C29 1.325(4) . ? N6 C30 1.362(4) . ? C3 C4 1.429(5) . ? C3 H3 0.9300 . ? C4 C9 1.413(5) . ? C4 C5 1.413(5) . ? C5 C6 1.405(5) . ? C6 C7 1.382(5) . ? C6 H6 0.9300 . ? C7 C8 1.372(6) . ? C7 H7 0.9300 . ? C8 C9 1.359(6) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.403(7) . ? C10 H10 0.9300 . ? C11 C16 1.418(6) . ? C11 C12 1.421(6) . ? C12 C13 1.354(9) . ? C12 H12 0.9300 . ? C13 C14 1.380(9) . ? C13 H13 0.9300 . ? C14 C15 1.389(7) . ? C14 H14 0.9300 . ? C15 C16 1.413(6) . ? C15 H15 0.9300 . ? C17 C18 1.506(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.412(6) . ? C19 H19 0.9300 . ? C20 C21 1.364(6) . ? C20 H20 0.9300 . ? C21 C22 1.399(6) . ? C21 H21 0.9300 . ? C22 C23 1.402(5) . ? C22 C24 1.433(6) . ? C23 C30 1.441(5) . ? C24 C25 1.344(6) . ? C24 H24 0.9300 . ? C25 C26 1.422(6) . ? C25 H25 0.9300 . ? C26 C27 1.395(5) . ? C26 C30 1.411(5) . ? C27 C28 1.362(6) . ? C27 H27 0.9300 . ? C28 C29 1.397(5) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 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 O2 Fe1 O1 89.77(11) . . ? O2 Fe1 N4 93.36(13) . . ? O1 Fe1 N4 176.27(12) . . ? O2 Fe1 N3 177.20(12) . . ? O1 Fe1 N3 93.02(12) . . ? N4 Fe1 N3 83.85(14) . . ? O2 Fe1 C2 91.21(14) . . ? O1 Fe1 C2 90.15(13) . . ? N4 Fe1 C2 91.80(14) . . ? N3 Fe1 C2 88.55(15) . . ? O2 Fe1 C1 90.53(13) . . ? O1 Fe1 C1 88.10(12) . . ? N4 Fe1 C1 89.85(13) . . ? N3 Fe1 C1 89.80(13) . . ? C2 Fe1 C1 177.53(15) . . ? N1 Mn1 N1 96.11(17) 2_655 . ? N1 Mn1 N6 96.68(11) 2_655 . ? N1 Mn1 N6 97.78(11) . . ? N1 Mn1 N6 97.78(11) 2_655 2_655 ? N1 Mn1 N6 96.68(11) . 2_655 ? N6 Mn1 N6 158.31(15) . 2_655 ? N1 Mn1 N5 169.95(11) 2_655 . ? N1 Mn1 N5 86.94(11) . . ? N6 Mn1 N5 73.39(10) . . ? N6 Mn1 N5 91.35(10) 2_655 . ? N1 Mn1 N5 86.94(11) 2_655 2_655 ? N1 Mn1 N5 169.95(11) . 2_655 ? N6 Mn1 N5 91.35(10) . 2_655 ? N6 Mn1 N5 73.39(10) 2_655 2_655 ? N5 Mn1 N5 91.68(15) . 2_655 ? C5 O1 Fe1 124.9(2) . . ? C16 O2 Fe1 125.0(3) . . ? C31 O3 H1O3 118.3 . . ? C32 O4 H104 139.9 . . ? C1 N1 Mn1 159.9(3) . . ? C3 N3 C17 121.0(3) . . ? C3 N3 Fe1 125.7(3) . . ? C17 N3 Fe1 113.3(2) . . ? C10 N4 C18 121.6(4) . . ? C10 N4 Fe1 125.7(3) . . ? C18 N4 Fe1 112.8(3) . . ? C19 N5 C23 118.1(3) . . ? C19 N5 Mn1 127.4(3) . . ? C23 N5 Mn1 114.4(2) . . ? C29 N6 C30 118.4(3) . . ? C29 N6 Mn1 125.8(2) . . ? C30 N6 Mn1 115.8(2) . . ? N1 C1 Fe1 172.5(3) . . ? N2 C2 Fe1 178.2(4) . . ? N3 C3 C4 124.8(3) . . ? N3 C3 H3 117.6 . . ? C4 C3 H3 117.6 . . ? C9 C4 C5 119.4(4) . . ? C9 C4 C3 117.7(4) . . ? C5 C4 C3 122.9(3) . . ? O1 C5 C6 118.7(3) . . ? O1 C5 C4 123.6(3) . . ? C6 C5 C4 117.7(3) . . ? C7 C6 C5 120.6(4) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C8 C7 C6 121.6(4) . . ? C8 C7 H7 119.2 . . ? C6 C7 H7 119.2 . . ? C9 C8 C7 119.1(4) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C8 C9 C4 121.5(4) . . ? C8 C9 H9 119.2 . . ? C4 C9 H9 119.2 . . ? N4 C10 C11 124.8(4) . . ? N4 C10 H10 117.6 . . ? C11 C10 H10 117.6 . . ? C10 C11 C16 123.8(4) . . ? C10 C11 C12 117.8(5) . . ? C16 C11 C12 118.2(5) . . ? C13 C12 C11 121.6(6) . . ? C13 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? C12 C13 C14 120.6(5) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C13 C14 C15 120.2(6) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C16 120.6(5) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? O2 C16 C15 117.7(4) . . ? O2 C16 C11 123.5(4) . . ? C15 C16 C11 118.8(4) . . ? N3 C17 C18 105.6(3) . . ? N3 C17 H17A 110.6 . . ? C18 C17 H17A 110.6 . . ? N3 C17 H17B 110.6 . . ? C18 C17 H17B 110.6 . . ? H17A C17 H17B 108.8 . . ? N4 C18 C17 106.3(3) . . ? N4 C18 H18A 110.5 . . ? C17 C18 H18A 110.5 . . ? N4 C18 H18B 110.5 . . ? C17 C18 H18B 110.5 . . ? H18A C18 H18B 108.7 . . ? N5 C19 C20 123.1(4) . . ? N5 C19 H19 118.4 . . ? C20 C19 H19 118.4 . . ? C21 C20 C19 118.6(4) . . ? C21 C20 H20 120.7 . . ? C19 C20 H20 120.7 . . ? C20 C21 C22 120.0(4) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C21 C22 C23 117.7(4) . . ? C21 C22 C24 123.0(4) . . ? C23 C22 C24 119.3(3) . . ? N5 C23 C22 122.5(3) . . ? N5 C23 C30 117.9(3) . . ? C22 C23 C30 119.7(3) . . ? C25 C24 C22 121.0(4) . . ? C25 C24 H24 119.5 . . ? C22 C24 H24 119.5 . . ? C24 C25 C26 121.4(4) . . ? C24 C25 H25 119.3 . . ? C26 C25 H25 119.3 . . ? C27 C26 C30 117.0(3) . . ? C27 C26 C25 123.6(3) . . ? C30 C26 C25 119.4(3) . . ? C28 C27 C26 120.7(3) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C29 118.6(3) . . ? C27 C28 H28 120.7 . . ? C29 C28 H28 120.7 . . ? N6 C29 C28 123.0(3) . . ? N6 C29 H29 118.5 . . ? C28 C29 H29 118.5 . . ? N6 C30 C26 122.2(3) . . ? N6 C30 C23 118.5(3) . . ? C26 C30 C23 119.2(3) . . ? O3 C31 H31A 109.3 . . ? O3 C31 H31B 109.3 . . ? H31A C31 H31B 109.5 . . ? O3 C31 H31C 109.9 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O4 C32 H32A 109.5 . . ? O4 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O4 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.906 _refine_diff_density_min -0.557 _refine_diff_density_rms 0.066 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 732680' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H41 Cl Fe Mn N9 O7' _chemical_formula_weight 834.00 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' Cl Cl 0.1484 0.1585 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.7094(13) _cell_length_b 18.836(2) _cell_length_c 15.5703(18) _cell_angle_alpha 90.00 _cell_angle_beta 92.015(2) _cell_angle_gamma 90.00 _cell_volume 3725.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 0.860 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8747 _exptl_absorpt_correction_T_max 0.9266 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II CCD area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18207 _diffrn_reflns_av_R_equivalents 0.0740 _diffrn_reflns_av_sigmaI/netI 0.0925 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6517 _reflns_number_gt 3355 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2001)' _computing_data_reduction SAINT-Plus _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material XP _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^)+(0.0928P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6517 _refine_ls_number_parameters 480 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1453 _refine_ls_R_factor_gt 0.0716 _refine_ls_wR_factor_ref 0.2026 _refine_ls_wR_factor_gt 0.1642 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 2.675 _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 0.84004(17) 0.25747(12) 0.18221(15) 0.0522(8) Uani 1 1 d . . . Mn1 Mn 1.08998(18) 0.20042(11) -0.06845(15) 0.0469(7) Uani 1 1 d . . . Cl1 Cl 0.2059(5) 0.5372(3) 0.1338(4) 0.0929(18) Uani 1 1 d . . . O1 O 0.9598(8) 0.2197(5) 0.2412(7) 0.057(3) Uani 1 1 d . . . O2 O 0.7721(9) 0.1686(6) 0.1934(8) 0.076(4) Uani 1 1 d . . . O3 O 0.1130(18) 0.5057(12) 0.1063(16) 0.186(9) Uani 1 1 d . . . O4 O 0.194(2) 0.6072(11) 0.1040(19) 0.221(12) Uani 1 1 d . . . O5 O 0.220(3) 0.541(2) 0.2166(14) 0.295(19) Uani 1 1 d . . . O6 O 0.290(2) 0.5116(17) 0.094(2) 0.253(15) Uani 1 1 d . . . O7 O 0.905(3) 0.162(4) 0.435(3) 0.43(4) Uani 1 1 d . . . H7 H 0.8767 0.1854 0.3961 0.640 Uiso 1 1 calc R . . N1 N 0.9428(10) 0.2074(7) 0.0117(9) 0.055(3) Uani 1 1 d . . . N2 N 1.2405(12) 0.1997(7) -0.1470(10) 0.067(4) Uani 1 1 d . . . N3 N 0.9007(11) 0.3502(7) 0.1734(9) 0.055(3) Uani 1 1 d . . . N4 N 0.7254(12) 0.2993(10) 0.1172(10) 0.074(4) Uani 1 1 d . . . N5 N 1.0622(10) 0.0893(6) -0.1173(8) 0.050(3) Uani 1 1 d . . . N6 N 0.9949(10) 0.2019(7) -0.1961(9) 0.059(4) Uani 1 1 d . . . N7 N 1.1643(10) 0.1201(8) 0.0262(9) 0.060(4) Uani 1 1 d D . . N8 N 1.1793(13) 0.2660(9) 0.0355(12) 0.088(6) Uani 1 1 d D . . H8 H 1.2450 0.2662 0.0141 0.106 Uiso 1 1 calc R . . N9 N 1.0590(18) 0.3178(7) -0.1020(11) 0.101(6) Uani 1 1 d . . . H9A H 0.9959 0.3231 -0.0769 0.121 Uiso 1 1 calc R . . C1 C 0.9002(12) 0.2254(8) 0.0720(12) 0.053(4) Uani 1 1 d . . . C2 C 0.7806(13) 0.2870(8) 0.2913(12) 0.056(4) Uani 1 1 d . . . C3 C 0.9835(15) 0.3721(9) 0.2141(13) 0.067(5) Uani 1 1 d . . . H3 H 1.0018 0.4196 0.2073 0.080 Uiso 1 1 calc R . . C4 C 1.0506(13) 0.3296(9) 0.2695(11) 0.058(4) Uani 1 1 d . . . C5 C 1.0367(13) 0.2560(9) 0.2792(10) 0.053(4) Uani 1 1 d . . . C6 C 1.1138(14) 0.2193(10) 0.3285(12) 0.065(5) Uani 1 1 d . . . H6 H 1.1073 0.1706 0.3362 0.078 Uiso 1 1 calc R . . C7 C 1.1972(16) 0.2537(12) 0.3651(13) 0.079(6) Uani 1 1 d . . . H7B H 1.2474 0.2278 0.3966 0.095 Uiso 1 1 calc R . . C8 C 1.2097(16) 0.3246(13) 0.3570(15) 0.090(7) Uani 1 1 d . . . H8A H 1.2666 0.3474 0.3844 0.108 Uiso 1 1 calc R . . C9 C 1.1393(16) 0.3621(11) 0.3091(14) 0.083(6) Uani 1 1 d . . . H9 H 1.1495 0.4106 0.3021 0.099 Uiso 1 1 calc R . . C10 C 0.6498(17) 0.2645(19) 0.0797(14) 0.103(8) Uani 1 1 d . . . H10 H 0.6018 0.2902 0.0456 0.124 Uiso 1 1 calc R . . C11 C 0.6333(18) 0.1895(18) 0.0860(16) 0.097(8) Uani 1 1 d . . . C12 C 0.5425(19) 0.162(2) 0.0374(19) 0.153(14) Uani 1 1 d . . . H12 H 0.5022 0.1900 0.0001 0.183 Uiso 1 1 calc R . . C13 C 0.519(3) 0.090(3) 0.050(3) 0.19(3) Uani 1 1 d . . . H13 H 0.4646 0.0691 0.0173 0.231 Uiso 1 1 calc R . . C14 C 0.573(3) 0.049(3) 0.108(3) 0.18(2) Uani 1 1 d . . . H14 H 0.5512 0.0028 0.1174 0.214 Uiso 1 1 calc R . . C15 C 0.6600(19) 0.0745(14) 0.1546(17) 0.127(10) Uani 1 1 d . . . H15 H 0.6975 0.0446 0.1921 0.152 Uiso 1 1 calc R . . C16 C 0.692(2) 0.1463(14) 0.1448(17) 0.097(8) Uani 1 1 d . . . C17 C 0.8450(16) 0.3966(11) 0.1114(13) 0.083(6) Uani 1 1 d . . . H17A H 0.8706 0.3892 0.0541 0.100 Uiso 1 1 calc R . . H17B H 0.8556 0.4460 0.1269 0.100 Uiso 1 1 calc R . . C18 C 0.7305(17) 0.3774(13) 0.1143(15) 0.098(7) Uani 1 1 d . . . H18A H 0.6996 0.3977 0.1648 0.118 Uiso 1 1 calc R . . H18B H 0.6924 0.3952 0.0636 0.118 Uiso 1 1 calc R . . C19 C 1.1019(13) 0.0342(8) -0.0725(12) 0.060(5) Uani 1 1 d . . . C20 C 1.0856(17) -0.0341(10) -0.1010(16) 0.081(6) Uani 1 1 d . . . H20 H 1.1123 -0.0721 -0.0690 0.098 Uiso 1 1 calc R . . C21 C 1.0313(18) -0.0459(11) -0.175(2) 0.094(7) Uani 1 1 d . . . H21 H 1.0198 -0.0921 -0.1942 0.113 Uiso 1 1 calc R . . C22 C 0.9927(16) 0.0103(12) -0.2224(14) 0.086(6) Uani 1 1 d . . . H22 H 0.9562 0.0027 -0.2744 0.104 Uiso 1 1 calc R . . C23 C 1.0089(13) 0.0788(9) -0.1917(12) 0.062(5) Uani 1 1 d . . . C24 C 0.9733(13) 0.1458(11) -0.2360(12) 0.065(5) Uani 1 1 d . . . C25 C 0.9186(18) 0.1400(13) -0.3242(14) 0.108(8) Uani 1 1 d . . . H25A H 0.8457 0.1284 -0.3178 0.162 Uiso 1 1 calc R . . H25B H 0.9516 0.1034 -0.3568 0.162 Uiso 1 1 calc R . . H25C H 0.9240 0.1845 -0.3538 0.162 Uiso 1 1 calc R . . C26 C 0.9665(15) 0.2725(10) -0.2297(12) 0.074(5) Uani 1 1 d . . . H26A H 0.9794 0.2744 -0.2907 0.089 Uiso 1 1 calc R . . H26B H 0.8920 0.2809 -0.2223 0.089 Uiso 1 1 calc R . . C27 C 1.026(2) 0.3259(14) -0.1867(19) 0.120(8) Uani 1 1 d DU . . H27A H 1.0861 0.3375 -0.2204 0.144 Uiso 1 1 d R . . H27B H 0.9811 0.3677 -0.1870 0.144 Uiso 1 1 d R . . C28 C 1.1191(17) 0.3641(10) -0.050(2) 0.107(9) Uani 1 1 d . . . H28A H 1.0772 0.4062 -0.0397 0.128 Uiso 1 1 calc R . . H28B H 1.1797 0.3790 -0.0816 0.128 Uiso 1 1 calc R . . C29 C 1.156(2) 0.3366(13) 0.0323(15) 0.115(9) Uani 1 1 d . . . H29A H 1.2192 0.3627 0.0502 0.139 Uiso 1 1 calc R . . H29B H 1.1033 0.3462 0.0741 0.139 Uiso 1 1 calc R . . C30 C 1.197(2) 0.2266(14) 0.1073(17) 0.118(8) Uani 1 1 d DU . . H30A H 1.1369 0.2318 0.1436 0.141 Uiso 1 1 d R . . H30B H 1.2566 0.2480 0.1378 0.141 Uiso 1 1 d R . . C31 C 1.2218(16) 0.1519(13) 0.0997(12) 0.098(8) Uani 1 1 d . . . H31A H 1.2034 0.1274 0.1519 0.117 Uiso 1 1 calc R . . H31B H 1.2968 0.1463 0.0927 0.117 Uiso 1 1 calc R . . C32 C 1.1609(14) 0.0544(10) 0.0091(12) 0.064(5) Uani 1 1 d . . . C33 C 1.2156(18) -0.0041(11) 0.0603(14) 0.106(8) Uani 1 1 d . . . H33A H 1.2489 0.0156 0.1112 0.159 Uiso 1 1 d R . . H33B H 1.2677 -0.0261 0.0259 0.159 Uiso 1 1 d R . . H33C H 1.1648 -0.0390 0.0762 0.159 Uiso 1 1 d R . . C34 C 0.898(8) 0.081(3) 0.411(6) 0.68(13) Uani 1 1 d . . . H34A H 0.9645 0.0590 0.4227 1.014 Uiso 1 1 d R . . H34B H 0.8792 0.0764 0.3506 1.014 Uiso 1 1 d R . . H34C H 0.8448 0.0587 0.4439 1.014 Uiso 1 1 d 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 Fe1 0.0463(14) 0.0603(15) 0.0505(16) -0.0054(11) 0.0108(10) -0.0037(11) Mn1 0.0576(16) 0.0445(13) 0.0392(15) -0.0007(11) 0.0088(10) -0.0026(11) Cl1 0.122(5) 0.071(4) 0.085(5) -0.001(3) -0.012(4) -0.002(3) O1 0.056(7) 0.044(6) 0.072(8) -0.003(5) -0.002(6) -0.001(5) O2 0.069(8) 0.085(8) 0.074(9) -0.021(7) 0.017(7) -0.038(7) O3 0.18(2) 0.164(18) 0.22(2) -0.048(17) -0.014(18) -0.067(15) O4 0.28(3) 0.098(15) 0.29(3) 0.038(17) 0.00(2) -0.022(16) O5 0.33(3) 0.51(6) 0.050(15) 0.03(2) -0.043(19) 0.00(4) O6 0.21(3) 0.31(4) 0.24(3) -0.05(3) 0.05(2) 0.12(2) O7 0.16(3) 0.74(10) 0.39(6) 0.34(7) 0.08(3) 0.04(4) N1 0.057(9) 0.058(9) 0.053(10) -0.007(7) 0.014(7) -0.003(7) N2 0.071(10) 0.071(10) 0.060(11) 0.000(8) 0.021(8) -0.004(8) N3 0.059(9) 0.055(8) 0.053(9) 0.001(7) 0.010(7) 0.007(7) N4 0.051(10) 0.115(14) 0.056(10) -0.004(9) 0.007(8) 0.009(9) N5 0.056(8) 0.046(8) 0.047(9) 0.000(7) 0.011(7) -0.002(6) N6 0.064(9) 0.061(9) 0.051(9) 0.009(8) 0.006(7) 0.006(7) N7 0.064(9) 0.070(10) 0.046(9) 0.013(8) 0.007(7) 0.006(7) N8 0.081(12) 0.075(11) 0.106(16) -0.024(11) -0.030(10) 0.017(9) N9 0.20(2) 0.044(9) 0.059(12) -0.005(8) 0.018(12) -0.020(11) C1 0.044(10) 0.055(10) 0.059(12) 0.002(9) 0.002(8) -0.004(8) C2 0.054(11) 0.052(10) 0.063(13) 0.005(9) 0.009(9) -0.004(8) C3 0.073(13) 0.046(10) 0.083(15) -0.011(10) 0.026(11) -0.005(9) C4 0.064(12) 0.054(10) 0.057(12) -0.014(9) 0.007(9) -0.001(9) C5 0.055(11) 0.062(11) 0.042(10) -0.007(8) 0.009(8) 0.002(9) C6 0.059(12) 0.074(12) 0.062(12) 0.001(10) -0.004(9) 0.013(9) C7 0.068(14) 0.095(16) 0.074(15) -0.017(12) -0.012(11) 0.019(11) C8 0.067(14) 0.102(17) 0.100(18) -0.026(14) -0.014(12) -0.007(12) C9 0.078(15) 0.074(13) 0.096(17) -0.028(12) -0.008(12) -0.014(11) C10 0.048(14) 0.21(3) 0.056(14) -0.025(17) 0.003(10) 0.017(16) C11 0.065(16) 0.15(3) 0.072(17) -0.033(17) 0.022(12) -0.030(16) C12 0.056(17) 0.28(4) 0.12(2) -0.10(3) 0.010(14) -0.02(2) C13 0.11(3) 0.29(7) 0.18(5) -0.16(5) 0.06(3) -0.10(4) C14 0.16(4) 0.23(5) 0.16(4) -0.11(4) 0.06(3) -0.13(4) C15 0.12(2) 0.14(2) 0.13(2) -0.063(18) 0.066(16) -0.072(18) C16 0.090(18) 0.12(2) 0.082(18) -0.046(16) 0.052(14) -0.044(16) C17 0.089(16) 0.083(14) 0.078(15) 0.021(11) 0.014(11) 0.020(11) C18 0.090(18) 0.12(2) 0.091(18) 0.013(14) 0.014(12) 0.045(14) C19 0.060(11) 0.048(10) 0.074(14) 0.006(9) 0.030(9) 0.002(8) C20 0.095(16) 0.048(12) 0.105(19) 0.000(11) 0.041(14) 0.001(10) C21 0.096(17) 0.044(12) 0.14(2) -0.022(14) 0.030(16) -0.010(11) C22 0.094(15) 0.085(15) 0.082(16) -0.038(13) 0.020(12) -0.016(12) C23 0.065(12) 0.061(11) 0.060(13) -0.017(10) 0.010(9) -0.005(9) C24 0.058(12) 0.080(13) 0.058(13) -0.010(11) 0.004(9) 0.002(10) C25 0.108(18) 0.14(2) 0.069(16) -0.026(15) -0.031(13) 0.001(15) C26 0.084(14) 0.081(13) 0.058(13) 0.013(11) 0.002(10) 0.015(11) C27 0.127(13) 0.106(12) 0.127(14) 0.015(11) -0.011(11) 0.003(10) C28 0.082(16) 0.053(13) 0.18(3) -0.012(16) -0.016(16) 0.007(10) C29 0.19(3) 0.080(17) 0.073(18) -0.018(14) 0.016(17) -0.054(17) C30 0.133(13) 0.110(12) 0.109(13) -0.005(11) -0.007(11) -0.019(11) C31 0.085(15) 0.16(2) 0.052(14) -0.013(13) -0.023(11) 0.057(14) C32 0.074(12) 0.064(12) 0.056(13) 0.022(10) 0.022(9) 0.019(10) C33 0.130(19) 0.096(16) 0.093(17) 0.029(13) 0.020(14) 0.055(14) C34 1.2(3) 0.16(4) 0.77(17) -0.19(7) 0.83(19) -0.19(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.889(10) . ? Fe1 O2 1.895(11) . ? Fe1 N4 1.915(15) . ? Fe1 N3 1.916(14) . ? Fe1 C2 1.964(19) . ? Fe1 C1 1.997(19) . ? Mn1 N5 2.250(12) . ? Mn1 N1 2.288(14) . ? Mn1 N6 2.290(14) . ? Mn1 N7 2.292(13) . ? Mn1 N9 2.303(15) . ? Mn1 N8 2.304(15) . ? Mn1 N2 2.307(15) . ? Cl1 O5 1.30(2) . ? Cl1 O6 1.34(2) . ? Cl1 O3 1.376(19) . ? Cl1 O4 1.40(2) . ? O1 C5 1.316(18) . ? O2 C16 1.32(3) . ? O7 C34 1.56(8) . ? O7 H7 0.8200 . ? N1 C1 1.151(19) . ? N2 C2 1.13(2) 4_665 ? N3 C3 1.28(2) . ? N3 C17 1.47(2) . ? N4 C10 1.29(3) . ? N4 C18 1.47(2) . ? N5 C23 1.34(2) . ? N5 C19 1.339(19) . ? N6 C24 1.25(2) . ? N6 C26 1.47(2) . ? N7 C32 1.27(2) . ? N7 C31 1.46(2) . ? N8 C30 1.35(2) . ? N8 C29 1.36(3) . ? N8 H8 0.9100 . ? N9 C27 1.38(3) . ? N9 C28 1.40(3) . ? N9 H9A 0.9100 . ? C2 N2 1.13(2) 4_566 ? C3 C4 1.44(2) . ? C3 H3 0.9300 . ? C4 C9 1.41(2) . ? C4 C5 1.41(2) . ? C5 C6 1.41(2) . ? C6 C7 1.35(2) . ? C6 H6 0.9300 . ? C7 C8 1.35(3) . ? C7 H7B 0.9300 . ? C8 C9 1.34(3) . ? C8 H8A 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.43(3) . ? C10 H10 0.9300 . ? C11 C16 1.42(3) . ? C11 C12 1.45(3) . ? C12 C13 1.40(6) . ? C12 H12 0.9300 . ? C13 C14 1.35(6) . ? C13 H13 0.9300 . ? C14 C15 1.38(4) . ? C14 H14 0.9300 . ? C15 C16 1.42(3) . ? C15 H15 0.9300 . ? C17 C18 1.50(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.37(2) . ? C19 C32 1.50(2) . ? C20 C21 1.34(3) . ? C20 H20 0.9300 . ? C21 C22 1.37(3) . ? C21 H21 0.9300 . ? C22 C23 1.39(2) . ? C22 H22 0.9300 . ? C23 C24 1.50(2) . ? C24 C25 1.52(2) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.41(3) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.45(3) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.45(3) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.52(2) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 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 O1 Fe1 O2 89.1(5) . . ? O1 Fe1 N4 175.9(6) . . ? O2 Fe1 N4 94.1(7) . . ? O1 Fe1 N3 93.4(5) . . ? O2 Fe1 N3 176.3(5) . . ? N4 Fe1 N3 83.5(7) . . ? O1 Fe1 C2 90.8(6) . . ? O2 Fe1 C2 88.8(6) . . ? N4 Fe1 C2 91.8(7) . . ? N3 Fe1 C2 88.4(6) . . ? O1 Fe1 C1 88.7(6) . . ? O2 Fe1 C1 90.1(6) . . ? N4 Fe1 C1 88.7(6) . . ? N3 Fe1 C1 92.7(6) . . ? C2 Fe1 C1 178.8(6) . . ? N5 Mn1 N1 96.7(4) . . ? N5 Mn1 N6 69.3(5) . . ? N1 Mn1 N6 93.2(5) . . ? N5 Mn1 N7 70.1(5) . . ? N1 Mn1 N7 90.8(5) . . ? N6 Mn1 N7 139.4(5) . . ? N5 Mn1 N9 142.4(6) . . ? N1 Mn1 N9 86.1(6) . . ? N6 Mn1 N9 73.2(6) . . ? N7 Mn1 N9 147.5(6) . . ? N5 Mn1 N8 143.5(5) . . ? N1 Mn1 N8 88.7(6) . . ? N6 Mn1 N8 146.7(6) . . ? N7 Mn1 N8 73.7(6) . . ? N9 Mn1 N8 73.8(6) . . ? N5 Mn1 N2 86.5(5) . . ? N1 Mn1 N2 176.9(5) . . ? N6 Mn1 N2 87.8(5) . . ? N7 Mn1 N2 90.4(5) . . ? N9 Mn1 N2 91.3(6) . . ? N8 Mn1 N2 88.7(6) . . ? O5 Cl1 O6 113(2) . . ? O5 Cl1 O3 115(2) . . ? O6 Cl1 O3 113.0(19) . . ? O5 Cl1 O4 107(2) . . ? O6 Cl1 O4 105(2) . . ? O3 Cl1 O4 102.6(16) . . ? C5 O1 Fe1 126.6(9) . . ? C16 O2 Fe1 125.1(16) . . ? C34 O7 H7 109.5 . . ? C1 N1 Mn1 151.5(13) . . ? C2 N2 Mn1 148.9(15) 4_665 . ? C3 N3 C17 120.3(15) . . ? C3 N3 Fe1 125.8(12) . . ? C17 N3 Fe1 113.9(12) . . ? C10 N4 C18 122(2) . . ? C10 N4 Fe1 124.9(18) . . ? C18 N4 Fe1 113.2(13) . . ? C23 N5 C19 120.5(14) . . ? C23 N5 Mn1 120.0(11) . . ? C19 N5 Mn1 119.6(11) . . ? C24 N6 C26 122.8(16) . . ? C24 N6 Mn1 121.4(12) . . ? C26 N6 Mn1 115.8(11) . . ? C32 N7 C31 125.2(16) . . ? C32 N7 Mn1 120.0(12) . . ? C31 N7 Mn1 114.6(12) . . ? C30 N8 C29 127(2) . . ? C30 N8 Mn1 110.4(14) . . ? C29 N8 Mn1 113.4(14) . . ? C30 N8 H8 100.4 . . ? C29 N8 H8 100.4 . . ? Mn1 N8 H8 100.4 . . ? C27 N9 C28 129(2) . . ? C27 N9 Mn1 111.6(14) . . ? C28 N9 Mn1 112.4(15) . . ? C27 N9 H9A 98.8 . . ? C28 N9 H9A 98.8 . . ? Mn1 N9 H9A 98.8 . . ? N1 C1 Fe1 174.4(15) . . ? N2 C2 Fe1 174.8(16) 4_566 . ? N3 C3 C4 125.4(15) . . ? N3 C3 H3 117.3 . . ? C4 C3 H3 117.3 . . ? C9 C4 C5 119.0(17) . . ? C9 C4 C3 118.1(17) . . ? C5 C4 C3 122.7(15) . . ? O1 C5 C6 118.9(15) . . ? O1 C5 C4 124.0(14) . . ? C6 C5 C4 117.1(15) . . ? C7 C6 C5 121.1(17) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C8 121.9(18) . . ? C6 C7 H7B 119.1 . . ? C8 C7 H7B 119.1 . . ? C9 C8 C7 119.4(19) . . ? C9 C8 H8A 120.3 . . ? C7 C8 H8A 120.3 . . ? C8 C9 C4 121.5(19) . . ? C8 C9 H9 119.2 . . ? C4 C9 H9 119.2 . . ? N4 C10 C11 125(2) . . ? N4 C10 H10 117.3 . . ? C11 C10 H10 117.3 . . ? C16 C11 C10 122(2) . . ? C16 C11 C12 121(3) . . ? C10 C11 C12 116(3) . . ? C13 C12 C11 116(4) . . ? C13 C12 H12 121.8 . . ? C11 C12 H12 121.8 . . ? C14 C13 C12 122(4) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? C13 C14 C15 122(5) . . ? C13 C14 H14 118.9 . . ? C15 C14 H14 118.9 . . ? C14 C15 C16 120(3) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? O2 C16 C11 125(2) . . ? O2 C16 C15 117(3) . . ? C11 C16 C15 118(3) . . ? N3 C17 C18 106.4(16) . . ? N3 C17 H17A 110.4 . . ? C18 C17 H17A 110.4 . . ? N3 C17 H17B 110.4 . . ? C18 C17 H17B 110.4 . . ? H17A C17 H17B 108.6 . . ? N4 C18 C17 106.6(15) . . ? N4 C18 H18A 110.4 . . ? C17 C18 H18A 110.4 . . ? N4 C18 H18B 110.4 . . ? C17 C18 H18B 110.4 . . ? H18A C18 H18B 108.6 . . ? N5 C19 C20 120.5(19) . . ? N5 C19 C32 114.3(14) . . ? C20 C19 C32 125.2(18) . . ? C21 C20 C19 120(2) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 119.9(19) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C21 C22 C23 119(2) . . ? C21 C22 H22 120.5 . . ? C23 C22 H22 120.5 . . ? N5 C23 C22 120.0(18) . . ? N5 C23 C24 114.2(14) . . ? C22 C23 C24 125.7(18) . . ? N6 C24 C23 115.1(16) . . ? N6 C24 C25 126.4(18) . . ? C23 C24 C25 118.5(17) . . ? 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 . . ? C27 C26 N6 110.8(17) . . ? C27 C26 H26A 109.5 . . ? N6 C26 H26A 109.5 . . ? C27 C26 H26B 109.5 . . ? N6 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? N9 C27 C26 121(2) . . ? N9 C27 H27A 108.7 . . ? C26 C27 H27A 108.9 . . ? N9 C27 H27B 104.7 . . ? C26 C27 H27B 105.9 . . ? H27A C27 H27B 106.7 . . ? N9 C28 C29 116.4(19) . . ? N9 C28 H28A 108.2 . . ? C29 C28 H28A 108.2 . . ? N9 C28 H28B 108.2 . . ? C29 C28 H28B 108.2 . . ? H28A C28 H28B 107.3 . . ? N8 C29 C28 116.5(19) . . ? N8 C29 H29A 108.2 . . ? C28 C29 H29A 108.2 . . ? N8 C29 H29B 108.2 . . ? C28 C29 H29B 108.2 . . ? H29A C29 H29B 107.3 . . ? N8 C30 C31 120(2) . . ? N8 C30 H30A 108.5 . . ? C31 C30 H30A 109.0 . . ? N8 C30 H30B 106.2 . . ? C31 C30 H30B 105.9 . . ? H30A C30 H30B 106.8 . . ? C30 C31 N7 110.8(16) . . ? C30 C31 H31A 109.5 . . ? N7 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? N7 C31 H31B 109.5 . . ? H31A C31 H31B 108.1 . . ? N7 C32 C19 116.0(15) . . ? N7 C32 C33 126.1(19) . . ? C19 C32 C33 117.8(17) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O7 C34 H34A 109.5 . . ? O7 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O7 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.593 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.073 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 732681' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H39 Cl Fe Mn N7 O9' _chemical_formula_weight 835.96 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' Cl Cl 0.1484 0.1585 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.7057(8) _cell_length_b 18.7334(11) _cell_length_c 15.4764(9) _cell_angle_alpha 90.00 _cell_angle_beta 93.1310(10) _cell_angle_gamma 90.00 _cell_volume 3678.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 0.874 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8378 _exptl_absorpt_correction_T_max 0.8801 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II CCD area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18037 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6450 _reflns_number_gt 4383 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2001)' _computing_data_reduction SAINT-Plus _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material XP _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^)+(0.0776P)^2^+3.4361P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6450 _refine_ls_number_parameters 491 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0825 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1591 _refine_ls_wR_factor_gt 0.1400 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 0.33561(5) 0.25349(3) 0.18893(4) 0.03790(19) Uani 1 1 d . . . Mn1 Mn 0.58406(5) 0.20036(3) -0.06344(4) 0.03481(19) Uani 1 1 d . . . Cl1 Cl 0.80146(12) 0.03044(7) 0.36066(10) 0.0656(4) Uani 1 1 d . . . O1 O 0.2679(3) 0.16316(18) 0.1950(2) 0.0571(9) Uani 1 1 d . . . O2 O 0.4538(2) 0.21426(15) 0.25064(18) 0.0426(7) Uani 1 1 d . . . O3 O 0.5490(3) 0.31661(15) -0.0865(2) 0.0494(8) Uani 1 1 d . . . O4 O 0.6773(3) 0.26371(17) 0.04315(19) 0.0514(8) Uani 1 1 d . . . O5 O 0.7191(7) 0.0090(5) 0.4082(5) 0.220(4) Uani 1 1 d . . . O6 O 0.7924(12) -0.0048(11) 0.2945(9) 0.400(12) Uani 1 1 d . . . O7 O 0.7924(10) 0.0797(7) 0.2948(8) 0.136(5) Uani 0.50 1 d P . . O7' O 0.8138(9) 0.0972(5) 0.3988(8) 0.126(4) Uani 0.50 1 d P . . O8 O 0.9013(5) 0.0053(4) 0.3901(5) 0.173(3) Uani 1 1 d . . . O9 O 0.3302(9) 0.0696(5) 0.3506(7) 0.242(5) Uani 1 1 d . . . H9A H 0.2885 0.1016 0.3370 0.363 Uiso 1 1 calc R . . N1 N 0.4425(3) 0.20619(18) 0.0196(2) 0.0409(8) Uani 1 1 d . . . N2 N 0.7283(3) 0.2089(2) -0.1411(2) 0.0484(9) Uani 1 1 d . . . N3 N 0.2203(3) 0.2970(2) 0.1215(2) 0.0533(10) Uani 1 1 d . . . N4 N 0.3964(3) 0.34684(18) 0.1837(2) 0.0409(8) Uani 1 1 d . . . N5 N 0.5575(3) 0.09197(18) -0.1167(2) 0.0415(8) Uani 1 1 d . . . N6 N 0.6618(3) 0.1210(2) 0.0285(2) 0.0443(9) Uani 1 1 d . . . N7 N 0.4893(3) 0.20855(19) -0.1911(2) 0.0427(9) Uani 1 1 d . . . C1 C 0.3986(3) 0.2239(2) 0.0787(3) 0.0395(10) Uani 1 1 d . . . C2 C 0.2717(3) 0.2800(2) 0.2984(3) 0.0425(10) Uani 1 1 d . . . C3 C 0.1423(4) 0.2630(4) 0.0837(3) 0.0707(17) Uani 1 1 d . . . H3 H 0.0941 0.2892 0.0493 0.085 Uiso 1 1 calc R . . C4 C 0.1247(4) 0.1878(4) 0.0909(4) 0.0752(19) Uani 1 1 d . . . C5 C 0.1858(4) 0.1420(3) 0.1471(3) 0.0662(16) Uani 1 1 d . . . C6 C 0.1556(5) 0.0681(4) 0.1580(4) 0.093(2) Uani 1 1 d . . . H6 H 0.1941 0.0372 0.1946 0.111 Uiso 1 1 calc R . . C7 C 0.0631(7) 0.0457(5) 0.1091(6) 0.122(4) Uani 1 1 d . . . H7 H 0.0405 -0.0011 0.1158 0.146 Uiso 1 1 calc R . . C8 C 0.0043(7) 0.0900(6) 0.0517(6) 0.122(4) Uani 1 1 d . . . H8 H -0.0537 0.0715 0.0200 0.146 Uiso 1 1 calc R . . C9 C 0.0321(5) 0.1626(5) 0.0412(4) 0.109(3) Uani 1 1 d . . . H9 H -0.0073 0.1926 0.0042 0.131 Uiso 1 1 calc R . . C10 C 0.4792(3) 0.3691(2) 0.2280(3) 0.0435(11) Uani 1 1 d . . . H10 H 0.4977 0.4169 0.2230 0.052 Uiso 1 1 calc R . . C11 C 0.5442(3) 0.3250(2) 0.2842(3) 0.0427(10) Uani 1 1 d . . . C12 C 0.6349(4) 0.3587(3) 0.3248(3) 0.0588(13) Uani 1 1 d . . . H12 H 0.6445 0.4076 0.3195 0.071 Uiso 1 1 calc R . . C13 C 0.7092(4) 0.3175(3) 0.3726(3) 0.0666(15) Uani 1 1 d . . . H13 H 0.7679 0.3393 0.3995 0.080 Uiso 1 1 calc R . . C14 C 0.6961(4) 0.2449(3) 0.3800(3) 0.0607(14) Uani 1 1 d . . . H14 H 0.7463 0.2182 0.4119 0.073 Uiso 1 1 calc R . . C15 C 0.6085(4) 0.2108(3) 0.3404(3) 0.0506(12) Uani 1 1 d . . . H15 H 0.6010 0.1617 0.3465 0.061 Uiso 1 1 calc R . . C16 C 0.5309(3) 0.2499(2) 0.2911(3) 0.0414(10) Uani 1 1 d . . . C17 C 0.2266(4) 0.3754(3) 0.1175(4) 0.0681(15) Uani 1 1 d . . . H17A H 0.1936 0.3965 0.1665 0.082 Uiso 1 1 calc R . . H17B H 0.1907 0.3929 0.0647 0.082 Uiso 1 1 calc R . . C18 C 0.3430(4) 0.3950(3) 0.1194(3) 0.0633(14) Uani 1 1 d . . . H18A H 0.3707 0.3881 0.0628 0.076 Uiso 1 1 calc R . . H18B H 0.3532 0.4444 0.1364 0.076 Uiso 1 1 calc R . . C19 C 0.5045(3) 0.0830(2) -0.1919(3) 0.0458(11) Uani 1 1 d . . . C20 C 0.4877(4) 0.0156(3) -0.2273(4) 0.0671(15) Uani 1 1 d . . . H20 H 0.4508 0.0096 -0.2803 0.080 Uiso 1 1 calc R . . C21 C 0.5280(5) -0.0421(3) -0.1809(4) 0.0734(17) Uani 1 1 d . . . H21 H 0.5167 -0.0880 -0.2026 0.088 Uiso 1 1 calc R . . C22 C 0.5845(4) -0.0332(3) -0.1031(4) 0.0668(15) Uani 1 1 d . . . H22 H 0.6120 -0.0723 -0.0725 0.080 Uiso 1 1 calc R . . C23 C 0.5992(3) 0.0354(2) -0.0718(3) 0.0451(11) Uani 1 1 d . . . C24 C 0.6599(4) 0.0552(3) 0.0097(3) 0.0489(12) Uani 1 1 d . . . C25 C 0.7164(5) -0.0047(3) 0.0616(4) 0.0776(18) Uani 1 1 d . . . H25A H 0.7522 0.0151 0.1123 0.116 Uiso 1 1 calc R . . H25B H 0.7666 -0.0273 0.0265 0.116 Uiso 1 1 calc R . . H25C H 0.6656 -0.0392 0.0785 0.116 Uiso 1 1 calc R . . C26 C 0.7233(4) 0.1513(3) 0.1050(3) 0.0592(13) Uani 1 1 d . . . H26A H 0.7176 0.1204 0.1549 0.071 Uiso 1 1 calc R . . H26B H 0.7972 0.1554 0.0928 0.071 Uiso 1 1 calc R . . C27 C 0.6788(4) 0.2231(3) 0.1228(3) 0.0571(13) Uani 1 1 d . . . H27A H 0.6079 0.2185 0.1424 0.068 Uiso 1 1 calc R . . H27B H 0.7219 0.2471 0.1675 0.068 Uiso 1 1 calc R . . C28 C 0.6351(5) 0.3343(3) 0.0508(3) 0.0645(14) Uani 1 1 d . . . H28A H 0.6833 0.3640 0.0857 0.077 Uiso 1 1 calc R . . H28B H 0.5682 0.3327 0.0781 0.077 Uiso 1 1 calc R . . C29 C 0.6201(5) 0.3643(3) -0.0396(3) 0.0656(15) Uani 1 1 d . . . H29A H 0.5904 0.4120 -0.0382 0.079 Uiso 1 1 calc R . . H29B H 0.6870 0.3666 -0.0669 0.079 Uiso 1 1 calc R . . C30 C 0.5374(4) 0.3331(3) -0.1786(3) 0.0566(13) Uani 1 1 d . . . H30A H 0.6047 0.3289 -0.2048 0.068 Uiso 1 1 calc R . . H30B H 0.5117 0.3815 -0.1871 0.068 Uiso 1 1 calc R . . C31 C 0.4588(4) 0.2800(2) -0.2195(3) 0.0524(12) Uani 1 1 d . . . H31A H 0.3884 0.2907 -0.2020 0.063 Uiso 1 1 calc R . . H31B H 0.4586 0.2830 -0.2821 0.063 Uiso 1 1 calc R . . C32 C 0.4681(3) 0.1522(3) -0.2347(3) 0.0467(11) Uani 1 1 d . . . C33 C 0.4111(5) 0.1476(4) -0.3232(3) 0.0791(17) Uani 1 1 d . . . H33A H 0.3407 0.1304 -0.3172 0.119 Uiso 1 1 calc R . . H33B H 0.4481 0.1155 -0.3592 0.119 Uiso 1 1 calc R . . H33C H 0.4083 0.1941 -0.3493 0.119 Uiso 1 1 calc R . . C34 C 0.4039(10) 0.0944(10) 0.4301(8) 0.246(10) Uani 1 1 d . . . H34A H 0.3909 0.1438 0.4420 0.370 Uiso 1 1 calc R . . H34B H 0.4763 0.0882 0.4168 0.370 Uiso 1 1 calc R . . H34C H 0.3894 0.0662 0.4799 0.370 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 Fe1 0.0346(3) 0.0453(4) 0.0349(3) -0.0079(3) 0.0118(2) -0.0049(3) Mn1 0.0426(4) 0.0327(3) 0.0301(3) 0.0009(3) 0.0111(3) 0.0003(3) Cl1 0.0802(10) 0.0450(7) 0.0706(9) 0.0057(6) -0.0064(7) -0.0071(6) O1 0.055(2) 0.064(2) 0.055(2) -0.0181(17) 0.0214(16) -0.0225(17) O2 0.0445(17) 0.0385(17) 0.0448(17) -0.0051(13) 0.0034(14) -0.0046(13) O3 0.061(2) 0.0367(16) 0.0524(19) -0.0014(14) 0.0167(15) -0.0059(15) O4 0.055(2) 0.0521(19) 0.0479(18) -0.0061(15) 0.0095(15) -0.0035(15) O5 0.189(8) 0.294(11) 0.184(7) 0.037(7) 0.078(6) -0.077(7) O6 0.356(17) 0.61(3) 0.224(12) -0.261(17) -0.052(12) 0.121(19) O7 0.181(11) 0.138(10) 0.090(8) 0.078(8) 0.008(7) 0.048(9) O7' 0.141(9) 0.054(5) 0.183(11) -0.054(6) 0.024(8) -0.016(5) O8 0.121(5) 0.154(6) 0.239(8) 0.076(5) -0.040(5) 0.008(4) O9 0.325(13) 0.158(7) 0.261(11) 0.066(7) 0.186(10) 0.073(8) N1 0.044(2) 0.044(2) 0.035(2) -0.0036(16) 0.0133(16) -0.0028(16) N2 0.051(2) 0.052(2) 0.044(2) 0.0042(18) 0.0217(18) 0.0010(18) N3 0.037(2) 0.077(3) 0.046(2) -0.006(2) 0.0067(17) 0.004(2) N4 0.043(2) 0.041(2) 0.040(2) -0.0056(16) 0.0092(16) 0.0007(17) N5 0.044(2) 0.035(2) 0.046(2) -0.0017(16) 0.0163(17) 0.0018(16) N6 0.045(2) 0.049(2) 0.040(2) 0.0095(17) 0.0109(16) 0.0057(17) N7 0.045(2) 0.046(2) 0.037(2) 0.0051(17) 0.0081(16) 0.0068(17) C1 0.035(2) 0.046(2) 0.037(2) -0.0037(19) 0.0030(19) -0.0055(19) C2 0.043(3) 0.045(3) 0.041(2) -0.006(2) 0.008(2) -0.006(2) C3 0.044(3) 0.123(6) 0.045(3) -0.023(3) 0.007(2) -0.004(3) C4 0.045(3) 0.125(6) 0.058(4) -0.046(4) 0.024(3) -0.030(3) C5 0.054(3) 0.092(4) 0.055(3) -0.035(3) 0.032(3) -0.029(3) C6 0.094(5) 0.097(5) 0.093(4) -0.054(4) 0.054(4) -0.063(4) C7 0.106(6) 0.148(8) 0.117(7) -0.084(6) 0.065(5) -0.084(6) C8 0.082(6) 0.181(10) 0.106(7) -0.078(7) 0.033(5) -0.061(6) C9 0.063(4) 0.186(9) 0.079(4) -0.069(5) 0.020(3) -0.040(5) C10 0.050(3) 0.040(3) 0.042(2) -0.007(2) 0.013(2) -0.004(2) C11 0.043(3) 0.041(2) 0.044(3) -0.008(2) 0.007(2) -0.003(2) C12 0.053(3) 0.073(3) 0.050(3) -0.016(3) -0.002(2) -0.014(3) C13 0.059(3) 0.082(4) 0.058(3) -0.017(3) -0.005(3) -0.014(3) C14 0.056(3) 0.078(4) 0.048(3) -0.007(3) 0.003(2) 0.004(3) C15 0.052(3) 0.059(3) 0.042(3) -0.001(2) 0.007(2) 0.011(2) C16 0.043(3) 0.053(3) 0.029(2) -0.0079(19) 0.0097(18) -0.002(2) C17 0.056(3) 0.076(4) 0.072(4) 0.007(3) 0.001(3) 0.011(3) C18 0.057(3) 0.070(4) 0.063(3) 0.017(3) -0.002(3) 0.007(3) C19 0.043(3) 0.048(3) 0.047(3) -0.012(2) 0.011(2) -0.005(2) C20 0.064(3) 0.063(4) 0.076(4) -0.027(3) 0.020(3) -0.010(3) C21 0.077(4) 0.046(3) 0.099(5) -0.022(3) 0.026(4) -0.010(3) C22 0.074(4) 0.043(3) 0.087(4) -0.008(3) 0.031(3) -0.005(3) C23 0.051(3) 0.034(2) 0.053(3) 0.005(2) 0.025(2) 0.006(2) C24 0.049(3) 0.049(3) 0.050(3) 0.020(2) 0.021(2) 0.011(2) C25 0.085(4) 0.066(4) 0.083(4) 0.034(3) 0.018(3) 0.034(3) C26 0.059(3) 0.076(4) 0.041(3) 0.004(2) -0.006(2) 0.008(3) C27 0.054(3) 0.078(4) 0.039(3) -0.003(2) 0.003(2) -0.006(3) C28 0.078(4) 0.045(3) 0.070(4) -0.016(3) 0.003(3) -0.003(3) C29 0.080(4) 0.044(3) 0.073(4) -0.001(3) 0.003(3) -0.017(3) C30 0.070(3) 0.048(3) 0.053(3) 0.020(2) 0.017(2) 0.008(2) C31 0.053(3) 0.052(3) 0.052(3) 0.012(2) 0.003(2) 0.014(2) C32 0.039(3) 0.057(3) 0.044(3) -0.008(2) 0.007(2) -0.001(2) C33 0.080(4) 0.099(5) 0.057(3) -0.003(3) -0.022(3) -0.007(4) C34 0.145(10) 0.48(3) 0.111(9) 0.033(13) 0.005(8) -0.022(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 O2 1.884(3) . ? Fe1 O1 1.903(3) . ? Fe1 N4 1.915(4) . ? Fe1 N3 1.932(4) . ? Fe1 C2 1.982(4) . ? Fe1 C1 2.001(4) . ? Mn1 N5 2.211(3) . ? Mn1 O3 2.247(3) . ? Mn1 N6 2.248(4) . ? Mn1 N2 2.252(4) . ? Mn1 N7 2.262(4) . ? Mn1 N1 2.269(3) . ? Mn1 O4 2.306(3) . ? Cl1 O6 1.218(9) . ? Cl1 O5 1.372(7) . ? Cl1 O7 1.375(8) . ? Cl1 O7' 1.388(8) . ? Cl1 O8 1.406(6) . ? O1 C5 1.308(6) . ? O2 C16 1.315(5) . ? O3 C29 1.438(6) . ? O3 C30 1.459(5) . ? O4 C28 1.435(6) . ? O4 C27 1.447(5) . ? O9 C34 1.574(14) . ? O9 H9A 0.8200 . ? N1 C1 1.147(5) . ? N2 C2 1.131(5) 4_665 ? N3 C3 1.290(6) . ? N3 C17 1.474(7) . ? N4 C10 1.294(5) . ? N4 C18 1.479(6) . ? N5 C19 1.323(5) . ? N5 C23 1.359(5) . ? N6 C24 1.267(6) . ? N6 C26 1.494(6) . ? N7 C32 1.274(5) . ? N7 C31 1.455(6) . ? C2 N2 1.131(5) 4_566 ? C3 C4 1.432(9) . ? C3 H3 0.9300 . ? C4 C5 1.421(9) . ? C4 C9 1.450(8) . ? C5 C6 1.449(8) . ? C6 C7 1.425(10) . ? C6 H6 0.9300 . ? C7 C8 1.402(12) . ? C7 H7 0.9300 . ? C8 C9 1.416(12) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.428(6) . ? C10 H10 0.9300 . ? C11 C16 1.423(6) . ? C11 C12 1.429(6) . ? C12 C13 1.399(7) . ? C12 H12 0.9300 . ? C13 C14 1.375(7) . ? C13 H13 0.9300 . ? C14 C15 1.396(7) . ? C14 H14 0.9300 . ? C15 C16 1.418(6) . ? C15 H15 0.9300 . ? C17 C18 1.522(7) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.388(7) . ? C19 C32 1.515(7) . ? C20 C21 1.381(8) . ? C20 H20 0.9300 . ? C21 C22 1.378(8) . ? C21 H21 0.9300 . ? C22 C23 1.383(7) . ? C22 H22 0.9300 . ? C23 C24 1.490(7) . ? C24 C25 1.534(6) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.491(7) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.511(7) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.523(7) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.517(6) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 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 O2 Fe1 O1 88.73(14) . . ? O2 Fe1 N4 93.76(14) . . ? O1 Fe1 N4 176.85(14) . . ? O2 Fe1 N3 176.50(15) . . ? O1 Fe1 N3 94.02(17) . . ? N4 Fe1 N3 83.56(17) . . ? O2 Fe1 C2 90.97(15) . . ? O1 Fe1 C2 88.45(15) . . ? N4 Fe1 C2 89.58(16) . . ? N3 Fe1 C2 91.27(17) . . ? O2 Fe1 C1 88.81(15) . . ? O1 Fe1 C1 89.95(15) . . ? N4 Fe1 C1 92.03(16) . . ? N3 Fe1 C1 89.02(16) . . ? C2 Fe1 C1 178.39(18) . . ? N5 Mn1 O3 143.70(13) . . ? N5 Mn1 N6 71.46(14) . . ? O3 Mn1 N6 144.81(13) . . ? N5 Mn1 N2 88.75(13) . . ? O3 Mn1 N2 90.37(12) . . ? N6 Mn1 N2 92.44(13) . . ? N5 Mn1 N7 70.93(13) . . ? O3 Mn1 N7 72.80(12) . . ? N6 Mn1 N7 142.39(14) . . ? N2 Mn1 N7 86.49(13) . . ? N5 Mn1 N1 98.40(12) . . ? O3 Mn1 N1 83.51(12) . . ? N6 Mn1 N1 90.44(13) . . ? N2 Mn1 N1 172.82(13) . . ? N7 Mn1 N1 95.23(12) . . ? N5 Mn1 O4 143.28(13) . . ? O3 Mn1 O4 72.81(12) . . ? N6 Mn1 O4 72.34(13) . . ? N2 Mn1 O4 86.78(13) . . ? N7 Mn1 O4 144.87(12) . . ? N1 Mn1 O4 87.83(12) . . ? O6 Cl1 O5 104.5(10) . . ? O6 Cl1 O7 75.0(10) . . ? O5 Cl1 O7 123.9(7) . . ? O6 Cl1 O7' 148.2(12) . . ? O5 Cl1 O7' 96.2(6) . . ? O7 Cl1 O7' 73.4(8) . . ? O6 Cl1 O8 97.6(8) . . ? O5 Cl1 O8 115.5(5) . . ? O7 Cl1 O8 120.2(6) . . ? O7' Cl1 O8 94.9(6) . . ? C5 O1 Fe1 126.2(4) . . ? C16 O2 Fe1 126.6(3) . . ? C29 O3 C30 112.9(4) . . ? C29 O3 Mn1 114.1(3) . . ? C30 O3 Mn1 111.7(3) . . ? C28 O4 C27 113.7(4) . . ? C28 O4 Mn1 110.7(3) . . ? C27 O4 Mn1 108.7(3) . . ? C34 O9 H9A 109.5 . . ? C1 N1 Mn1 154.3(3) . . ? C2 N2 Mn1 154.4(4) 4_665 . ? C3 N3 C17 121.0(5) . . ? C3 N3 Fe1 125.3(4) . . ? C17 N3 Fe1 113.7(3) . . ? C10 N4 C18 119.3(4) . . ? C10 N4 Fe1 126.2(3) . . ? C18 N4 Fe1 114.4(3) . . ? C19 N5 C23 121.1(4) . . ? C19 N5 Mn1 120.3(3) . . ? C23 N5 Mn1 118.6(3) . . ? C24 N6 C26 123.6(4) . . ? C24 N6 Mn1 119.7(3) . . ? C26 N6 Mn1 116.3(3) . . ? C32 N7 C31 123.9(4) . . ? C32 N7 Mn1 119.5(3) . . ? C31 N7 Mn1 116.5(3) . . ? N1 C1 Fe1 174.2(4) . . ? N2 C2 Fe1 174.0(4) 4_566 . ? N3 C3 C4 124.7(6) . . ? N3 C3 H3 117.6 . . ? C4 C3 H3 117.6 . . ? C5 C4 C3 124.0(5) . . ? C5 C4 C9 121.9(7) . . ? C3 C4 C9 113.9(7) . . ? O1 C5 C4 123.8(5) . . ? O1 C5 C6 115.6(6) . . ? C4 C5 C6 120.5(6) . . ? C7 C6 C5 115.8(8) . . ? C7 C6 H6 122.1 . . ? C5 C6 H6 122.1 . . ? C8 C7 C6 123.9(8) . . ? C8 C7 H7 118.1 . . ? C6 C7 H7 118.1 . . ? C7 C8 C9 120.9(8) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C8 C9 C4 116.9(9) . . ? C8 C9 H9 121.6 . . ? C4 C9 H9 121.6 . . ? N4 C10 C11 124.2(4) . . ? N4 C10 H10 117.9 . . ? C11 C10 H10 117.9 . . ? C16 C11 C10 123.4(4) . . ? C16 C11 C12 120.0(4) . . ? C10 C11 C12 116.0(4) . . ? C13 C12 C11 119.6(5) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C14 C13 C12 120.6(5) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C15 120.9(5) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C14 C15 C16 120.9(5) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? O2 C16 C15 118.2(4) . . ? O2 C16 C11 123.7(4) . . ? C15 C16 C11 118.0(4) . . ? N3 C17 C18 107.1(4) . . ? N3 C17 H17A 110.3 . . ? C18 C17 H17A 110.3 . . ? N3 C17 H17B 110.3 . . ? C18 C17 H17B 110.3 . . ? H17A C17 H17B 108.6 . . ? N4 C18 C17 106.0(4) . . ? N4 C18 H18A 110.5 . . ? C17 C18 H18A 110.5 . . ? N4 C18 H18B 110.5 . . ? C17 C18 H18B 110.5 . . ? H18A C18 H18B 108.7 . . ? N5 C19 C20 121.5(5) . . ? N5 C19 C32 113.9(4) . . ? C20 C19 C32 124.6(5) . . ? C21 C20 C19 117.6(5) . . ? C21 C20 H20 121.2 . . ? C19 C20 H20 121.2 . . ? C22 C21 C20 121.3(5) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C23 118.2(5) . . ? C21 C22 H22 120.9 . . ? C23 C22 H22 120.9 . . ? N5 C23 C22 120.3(5) . . ? N5 C23 C24 114.1(4) . . ? C22 C23 C24 125.6(5) . . ? N6 C24 C23 116.0(4) . . ? N6 C24 C25 126.1(5) . . ? C23 C24 C25 117.9(5) . . ? 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 . . ? C27 C26 N6 107.5(4) . . ? C27 C26 H26A 110.2 . . ? N6 C26 H26A 110.2 . . ? C27 C26 H26B 110.2 . . ? N6 C26 H26B 110.2 . . ? H26A C26 H26B 108.5 . . ? O4 C27 C26 107.8(4) . . ? O4 C27 H27A 110.2 . . ? C26 C27 H27A 110.2 . . ? O4 C27 H27B 110.2 . . ? C26 C27 H27B 110.2 . . ? H27A C27 H27B 108.5 . . ? O4 C28 C29 107.1(4) . . ? O4 C28 H28A 110.3 . . ? C29 C28 H28A 110.3 . . ? O4 C28 H28B 110.3 . . ? C29 C28 H28B 110.3 . . ? H28A C28 H28B 108.5 . . ? O3 C29 C28 106.3(4) . . ? O3 C29 H29A 110.5 . . ? C28 C29 H29A 110.5 . . ? O3 C29 H29B 110.5 . . ? C28 C29 H29B 110.5 . . ? H29A C29 H29B 108.7 . . ? O3 C30 C31 107.2(4) . . ? O3 C30 H30A 110.3 . . ? C31 C30 H30A 110.3 . . ? O3 C30 H30B 110.3 . . ? C31 C30 H30B 110.3 . . ? H30A C30 H30B 108.5 . . ? N7 C31 C30 108.6(4) . . ? N7 C31 H31A 110.0 . . ? C30 C31 H31A 110.0 . . ? N7 C31 H31B 110.0 . . ? C30 C31 H31B 110.0 . . ? H31A C31 H31B 108.4 . . ? N7 C32 C19 115.3(4) . . ? N7 C32 C33 126.9(5) . . ? C19 C32 C33 117.8(4) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O9 C34 H34A 109.5 . . ? O9 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O9 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.824 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.072