Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_total _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Prof. Qingliang Liu' _publ_contact_author_address ; Department of Chemistry University of Science and Technology of China Hefei P. R. China. ; _publ_contact_author_email QLIU@USTC.EDU.CN _publ_contact_author_fax +86-551-3603388 _publ_contact_author_phone +86-551-3603214 _publ_section_title ; Self-assembled hetero-bimetallic coordination cage and pseudo-capsules for inclusion of Cl- anions using a flexible two-arm ferrocene amide linker ; loop_ _publ_author_name 'Qingliang Liu' 'Yangzhong Liu' 'Jia Ni' 'Kai Wei' 'Yongshu Xie' data_ligand_3-BPFA _database_code_depnum_ccdc_archive 'CCDC 273380' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H20 Fe N4 O3' _chemical_formula_weight 444.27 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.7467(15) _cell_length_b 8.6769(12) _cell_length_c 11.5977(16) _cell_angle_alpha 90.00 _cell_angle_beta 115.636(2) _cell_angle_gamma 90.00 _cell_volume 975.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 460 _exptl_absorpt_coefficient_mu 0.806 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7492 _exptl_absorpt_correction_T_max 0.9024 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _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 area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4750 _diffrn_reflns_av_R_equivalents 0.0196 _diffrn_reflns_av_sigmaI/netI 0.0634 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3862 _reflns_number_gt 3508 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material SHELXL-97 _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^)+(0.0517P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.024(18) _refine_ls_number_reflns 3862 _refine_ls_number_parameters 271 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0483 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1058 _refine_ls_wR_factor_gt 0.1028 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.22976(4) 0.39837(5) 0.22444(4) 0.03145(13) Uani 1 1 d . . . N1 N 0.2248(3) 0.8066(3) 0.3534(3) 0.0404(7) Uani 1 1 d . . . H1A H 0.3114 0.7997 0.3725 0.048 Uiso 1 1 calc R . . N2 N 0.0264(3) 1.0108(4) 0.4992(3) 0.0511(8) Uani 1 1 d . . . N3 N 0.2883(3) 0.4675(3) 0.5832(2) 0.0362(6) Uani 1 1 d . . . H3A H 0.2005 0.4781 0.5407 0.043 Uiso 1 1 calc R . . N4 N 0.5335(3) 0.5705(5) 0.9134(3) 0.0550(9) Uani 1 1 d . . . O1 O 0.0125(2) 0.7369(3) 0.2039(3) 0.0541(7) Uani 1 1 d . . . O2 O 0.4790(2) 0.3676(3) 0.5747(2) 0.0434(7) Uani 1 1 d . . . O3 O 0.8165(3) 0.5007(5) 0.0653(4) 0.0927(13) Uani 1 1 d . . . H3F H 0.8737 0.5711 0.1060 0.111 Uiso 1 1 d R . . H3E H 0.7322 0.5234 0.0203 0.111 Uiso 1 1 d R . . C1 C 0.2063(4) 0.6293(5) 0.1882(4) 0.0370(8) Uani 1 1 d . . . C2 C 0.3501(3) 0.5867(4) 0.2388(3) 0.0380(7) Uani 1 1 d . . . H2 H 0.4209 0.6241 0.3136 0.046 Uiso 1 1 calc R . . C3 C 0.3640(4) 0.4769(5) 0.1537(4) 0.0454(8) Uani 1 1 d . . . H3 H 0.4458 0.4303 0.1630 0.055 Uiso 1 1 calc R . . C4 C 0.2320(4) 0.4512(5) 0.0528(3) 0.0501(10) Uani 1 1 d . . . H4 H 0.2121 0.3848 -0.0158 0.060 Uiso 1 1 calc R . . C5 C 0.1362(4) 0.5428(4) 0.0736(3) 0.0456(9) Uani 1 1 d . . . H5 H 0.0419 0.5465 0.0211 0.055 Uiso 1 1 calc R . . C6 C 0.1381(3) 0.7286(4) 0.2470(3) 0.0368(7) Uani 1 1 d . . . C7 C 0.1902(3) 0.8975(5) 0.4361(3) 0.0356(6) Uani 1 1 d . . . C8 C 0.0556(4) 0.9301(4) 0.4173(4) 0.0444(9) Uani 1 1 d . . . H8A H -0.0171 0.8933 0.3437 0.053 Uiso 1 1 calc R . . C9 C 0.1315(4) 1.0642(5) 0.6049(4) 0.0490(9) Uani 1 1 d . . . H9A H 0.1122 1.1200 0.6637 0.059 Uiso 1 1 calc R . . C10 C 0.2669(4) 1.0393(4) 0.6293(4) 0.0484(9) Uani 1 1 d . . . H10A H 0.3377 1.0805 0.7021 0.058 Uiso 1 1 calc R . . C11 C 0.2968(4) 0.9538(4) 0.5462(4) 0.0433(8) Uani 1 1 d . . . H11A H 0.3881 0.9334 0.5631 0.052 Uiso 1 1 calc R . . C12 C 0.2645(3) 0.3162(4) 0.4003(3) 0.0344(7) Uani 1 1 d . . . C13 C 0.3137(4) 0.2100(4) 0.3355(3) 0.0386(7) Uani 1 1 d . . . H13 H 0.4044 0.1767 0.3633 0.046 Uiso 1 1 calc R . . C14 C 0.2009(5) 0.1649(5) 0.2223(4) 0.0436(10) Uani 1 1 d . . . H14 H 0.2042 0.0952 0.1628 0.052 Uiso 1 1 calc R . . C15 C 0.0821(4) 0.2422(4) 0.2134(3) 0.0437(8) Uani 1 1 d . . . H15 H -0.0059 0.2335 0.1467 0.052 Uiso 1 1 calc R . . C16 C 0.1195(4) 0.3354(4) 0.3233(3) 0.0384(7) Uani 1 1 d . . . H16 H 0.0606 0.3979 0.3422 0.046 Uiso 1 1 calc R . . C17 C 0.3524(3) 0.3856(5) 0.5250(3) 0.0317(6) Uani 1 1 d . . . C18 C 0.3480(3) 0.5374(4) 0.7048(3) 0.0358(7) Uani 1 1 d . . . C19 C 0.2708(4) 0.6434(5) 0.7349(4) 0.0477(9) Uani 1 1 d . . . H19A H 0.1824 0.6688 0.6747 0.057 Uiso 1 1 calc R . . C20 C 0.3244(5) 0.7114(5) 0.8536(4) 0.0563(11) Uani 1 1 d . . . H20A H 0.2729 0.7820 0.8752 0.068 Uiso 1 1 calc R . . C21 C 0.4552(5) 0.6728(5) 0.9390(4) 0.0560(11) Uani 1 1 d . . . H21A H 0.4919 0.7199 1.0189 0.067 Uiso 1 1 calc R . . C22 C 0.4801(4) 0.5056(5) 0.7983(3) 0.0460(9) Uani 1 1 d . . . H22A H 0.5338 0.4353 0.7792 0.055 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 0.0322(2) 0.0297(2) 0.03253(19) -0.0005(2) 0.01411(15) -0.0006(2) N1 0.0254(13) 0.0399(17) 0.0566(17) -0.0015(13) 0.0185(13) -0.0012(12) N2 0.0407(17) 0.057(2) 0.065(2) 0.0009(16) 0.0318(16) 0.0054(15) N3 0.0225(12) 0.0463(15) 0.0353(13) -0.0017(12) 0.0085(11) 0.0034(11) N4 0.0532(19) 0.068(2) 0.0399(16) -0.0034(16) 0.0166(15) -0.0092(17) O1 0.0326(13) 0.0532(16) 0.0661(17) -0.0052(14) 0.0116(12) 0.0033(12) O2 0.0274(10) 0.057(2) 0.0449(11) -0.0005(11) 0.0145(9) 0.0084(10) O3 0.058(2) 0.082(3) 0.114(3) 0.023(2) 0.015(2) -0.0163(18) C1 0.0379(19) 0.0356(19) 0.0367(17) 0.0079(15) 0.0155(14) 0.0005(15) C2 0.0344(17) 0.0330(17) 0.0482(18) -0.0016(14) 0.0194(15) -0.0037(14) C3 0.050(2) 0.045(2) 0.055(2) -0.0007(17) 0.0349(18) -0.0024(17) C4 0.068(3) 0.048(2) 0.0397(18) -0.0006(15) 0.0281(19) -0.0085(18) C5 0.045(2) 0.048(2) 0.0350(16) 0.0103(16) 0.0090(15) -0.0039(17) C6 0.0307(16) 0.0292(16) 0.0459(17) 0.0085(13) 0.0123(14) -0.0001(13) C7 0.0326(13) 0.0281(13) 0.0500(15) 0.005(2) 0.0216(12) -0.0013(19) C8 0.0333(16) 0.045(3) 0.0582(19) -0.0022(15) 0.0227(15) -0.0007(15) C9 0.047(2) 0.050(2) 0.060(2) -0.0027(18) 0.032(2) 0.0011(18) C10 0.047(2) 0.044(2) 0.056(2) -0.0044(17) 0.0233(18) -0.0007(17) C11 0.0319(16) 0.046(2) 0.056(2) 0.0005(15) 0.0222(16) 0.0015(14) C12 0.0365(18) 0.0302(17) 0.0376(16) 0.0053(12) 0.0171(14) 0.0042(13) C13 0.0423(18) 0.0321(17) 0.0449(18) 0.0052(14) 0.0223(15) 0.0063(15) C14 0.060(2) 0.0288(19) 0.045(2) -0.0066(15) 0.0257(19) -0.0042(18) C15 0.0442(19) 0.046(2) 0.0418(18) -0.0065(15) 0.0191(15) -0.0156(17) C16 0.0355(17) 0.0423(17) 0.0424(17) -0.0016(14) 0.0215(14) -0.0039(14) C17 0.0310(13) 0.0307(15) 0.0349(12) 0.0085(15) 0.0156(11) 0.0038(16) C18 0.0378(17) 0.0361(17) 0.0390(16) 0.0022(14) 0.0217(14) -0.0035(14) C19 0.045(2) 0.046(2) 0.053(2) -0.0035(17) 0.0229(17) -0.0008(17) C20 0.067(3) 0.050(2) 0.066(3) -0.016(2) 0.043(2) -0.006(2) C21 0.070(3) 0.059(2) 0.0431(19) -0.0152(19) 0.029(2) -0.019(2) C22 0.0389(19) 0.056(2) 0.0424(19) -0.0017(16) 0.0166(16) -0.0005(17) _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 C5 2.029(3) . ? Fe1 C13 2.034(3) . ? Fe1 C12 2.037(3) . ? Fe1 C1 2.041(4) . ? Fe1 C2 2.045(3) . ? Fe1 C16 2.048(4) . ? Fe1 C14 2.048(4) . ? Fe1 C15 2.048(4) . ? Fe1 C4 2.053(4) . ? Fe1 C3 2.060(4) . ? N1 C6 1.362(4) . ? N1 C7 1.410(5) . ? N1 H1A 0.8600 . ? N2 C8 1.322(5) . ? N2 C9 1.340(5) . ? N3 C17 1.355(4) . ? N3 C18 1.409(4) . ? N3 H3A 0.8600 . ? N4 C22 1.329(5) . ? N4 C21 1.341(6) . ? O1 C6 1.222(4) . ? O2 C17 1.236(3) . ? O3 H3F 0.8500 . ? O3 H3E 0.8500 . ? C1 C5 1.425(5) . ? C1 C2 1.443(5) . ? C1 C6 1.476(5) . ? C2 C3 1.425(5) . ? C2 H2 0.9300 . ? C3 C4 1.412(5) . ? C3 H3 0.9300 . ? C4 C5 1.402(6) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C7 C11 1.384(5) . ? C7 C8 1.396(4) . ? C8 H8A 0.9300 . ? C9 C10 1.374(5) . ? C9 H9A 0.9300 . ? C10 C11 1.360(5) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C12 C13 1.428(5) . ? C12 C16 1.431(5) . ? C12 C17 1.472(4) . ? C13 C14 1.403(6) . ? C13 H13 0.9300 . ? C14 C15 1.406(6) . ? C14 H14 0.9300 . ? C15 C16 1.413(5) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C18 C19 1.381(5) . ? C18 C22 1.390(5) . ? C19 C20 1.375(6) . ? C19 H19A 0.9300 . ? C20 C21 1.365(6) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Fe1 C13 163.81(15) . . ? C5 Fe1 C12 152.49(15) . . ? C13 Fe1 C12 41.06(14) . . ? C5 Fe1 C1 40.98(15) . . ? C13 Fe1 C1 154.26(16) . . ? C12 Fe1 C1 120.19(14) . . ? C5 Fe1 C2 68.71(14) . . ? C13 Fe1 C2 119.91(14) . . ? C12 Fe1 C2 111.25(14) . . ? C1 Fe1 C2 41.37(13) . . ? C5 Fe1 C16 117.17(15) . . ? C13 Fe1 C16 68.69(14) . . ? C12 Fe1 C16 41.02(13) . . ? C1 Fe1 C16 109.14(15) . . ? C2 Fe1 C16 131.76(14) . . ? C5 Fe1 C14 125.77(15) . . ? C13 Fe1 C14 40.21(16) . . ? C12 Fe1 C14 68.10(14) . . ? C1 Fe1 C14 164.66(13) . . ? C2 Fe1 C14 151.45(15) . . ? C16 Fe1 C14 67.76(16) . . ? C5 Fe1 C15 105.86(15) . . ? C13 Fe1 C15 68.12(15) . . ? C12 Fe1 C15 68.43(14) . . ? C1 Fe1 C15 127.87(15) . . ? C2 Fe1 C15 168.26(15) . . ? C16 Fe1 C15 40.38(13) . . ? C14 Fe1 C15 40.14(16) . . ? C5 Fe1 C4 40.16(16) . . ? C13 Fe1 C4 127.25(15) . . ? C12 Fe1 C4 167.20(15) . . ? C1 Fe1 C4 68.46(16) . . ? C2 Fe1 C4 68.18(15) . . ? C16 Fe1 C4 148.77(15) . . ? C14 Fe1 C4 105.94(16) . . ? C15 Fe1 C4 114.90(15) . . ? C5 Fe1 C3 67.90(16) . . ? C13 Fe1 C3 108.82(16) . . ? C12 Fe1 C3 131.14(14) . . ? C1 Fe1 C3 68.79(15) . . ? C2 Fe1 C3 40.63(15) . . ? C16 Fe1 C3 170.38(14) . . ? C14 Fe1 C3 116.81(17) . . ? C15 Fe1 C3 148.34(15) . . ? C4 Fe1 C3 40.17(15) . . ? C6 N1 C7 128.0(3) . . ? C6 N1 H1A 116.0 . . ? C7 N1 H1A 116.0 . . ? C8 N2 C9 118.2(3) . . ? C17 N3 C18 127.9(3) . . ? C17 N3 H3A 116.1 . . ? C18 N3 H3A 116.1 . . ? C22 N4 C21 117.6(3) . . ? H3F O3 H3E 119.8 . . ? C5 C1 C2 106.6(3) . . ? C5 C1 C6 124.8(3) . . ? C2 C1 C6 128.3(3) . . ? C5 C1 Fe1 69.1(2) . . ? C2 C1 Fe1 69.5(2) . . ? C6 C1 Fe1 121.3(3) . . ? C3 C2 C1 107.7(3) . . ? C3 C2 Fe1 70.2(2) . . ? C1 C2 Fe1 69.2(2) . . ? C3 C2 H2 126.1 . . ? C1 C2 H2 126.1 . . ? Fe1 C2 H2 126.0 . . ? C4 C3 C2 108.1(3) . . ? C4 C3 Fe1 69.6(2) . . ? C2 C3 Fe1 69.1(2) . . ? C4 C3 H3 126.0 . . ? C2 C3 H3 126.0 . . ? Fe1 C3 H3 126.8 . . ? C5 C4 C3 108.5(3) . . ? C5 C4 Fe1 69.0(2) . . ? C3 C4 Fe1 70.2(2) . . ? C5 C4 H4 125.8 . . ? C3 C4 H4 125.8 . . ? Fe1 C4 H4 126.6 . . ? C4 C5 C1 109.1(3) . . ? C4 C5 Fe1 70.8(2) . . ? C1 C5 Fe1 69.9(2) . . ? C4 C5 H5 125.4 . . ? C1 C5 H5 125.4 . . ? Fe1 C5 H5 125.4 . . ? O1 C6 N1 122.9(3) . . ? O1 C6 C1 121.8(3) . . ? N1 C6 C1 115.3(3) . . ? C11 C7 C8 117.4(3) . . ? C11 C7 N1 117.9(3) . . ? C8 C7 N1 124.6(3) . . ? N2 C8 C7 123.2(3) . . ? N2 C8 H8A 118.4 . . ? C7 C8 H8A 118.4 . . ? N2 C9 C10 122.2(4) . . ? N2 C9 H9A 118.9 . . ? C10 C9 H9A 118.9 . . ? C11 C10 C9 119.6(4) . . ? C11 C10 H10A 120.2 . . ? C9 C10 H10A 120.2 . . ? C10 C11 C7 119.4(3) . . ? C10 C11 H11A 120.3 . . ? C7 C11 H11A 120.3 . . ? C13 C12 C16 107.3(3) . . ? C13 C12 C17 123.7(3) . . ? C16 C12 C17 128.9(3) . . ? C13 C12 Fe1 69.37(19) . . ? C16 C12 Fe1 69.89(18) . . ? C17 C12 Fe1 127.1(2) . . ? C14 C13 C12 107.8(3) . . ? C14 C13 Fe1 70.4(2) . . ? C12 C13 Fe1 69.57(18) . . ? C14 C13 H13 126.1 . . ? C12 C13 H13 126.1 . . ? Fe1 C13 H13 125.5 . . ? C13 C14 C15 109.0(3) . . ? C13 C14 Fe1 69.4(2) . . ? C15 C14 Fe1 69.9(2) . . ? C13 C14 H14 125.5 . . ? C15 C14 H14 125.5 . . ? Fe1 C14 H14 126.8 . . ? C14 C15 C16 108.2(3) . . ? C14 C15 Fe1 69.9(2) . . ? C16 C15 Fe1 69.8(2) . . ? C14 C15 H15 125.9 . . ? C16 C15 H15 125.9 . . ? Fe1 C15 H15 126.0 . . ? C15 C16 C12 107.7(3) . . ? C15 C16 Fe1 69.8(2) . . ? C12 C16 Fe1 69.09(19) . . ? C15 C16 H16 126.1 . . ? C12 C16 H16 126.1 . . ? Fe1 C16 H16 126.5 . . ? O2 C17 N3 121.9(3) . . ? O2 C17 C12 121.0(3) . . ? N3 C17 C12 117.1(2) . . ? C19 C18 C22 117.2(3) . . ? C19 C18 N3 118.4(3) . . ? C22 C18 N3 124.4(3) . . ? C20 C19 C18 120.1(4) . . ? C20 C19 H19A 119.9 . . ? C18 C19 H19A 119.9 . . ? C21 C20 C19 118.4(4) . . ? C21 C20 H20A 120.8 . . ? C19 C20 H20A 120.8 . . ? N4 C21 C20 123.3(4) . . ? N4 C21 H21A 118.3 . . ? C20 C21 H21A 118.3 . . ? N4 C22 C18 123.4(4) . . ? N4 C22 H22A 118.3 . . ? C18 C22 H22A 118.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 Fe1 C1 C5 169.8(3) . . . . ? C12 Fe1 C1 C5 -153.5(2) . . . . ? C2 Fe1 C1 C5 118.0(3) . . . . ? C16 Fe1 C1 C5 -109.7(2) . . . . ? C14 Fe1 C1 C5 -34.1(7) . . . . ? C15 Fe1 C1 C5 -68.4(3) . . . . ? C4 Fe1 C1 C5 37.0(2) . . . . ? C3 Fe1 C1 C5 80.3(2) . . . . ? C5 Fe1 C1 C2 -118.0(3) . . . . ? C13 Fe1 C1 C2 51.8(4) . . . . ? C12 Fe1 C1 C2 88.5(2) . . . . ? C16 Fe1 C1 C2 132.3(2) . . . . ? C14 Fe1 C1 C2 -152.2(6) . . . . ? C15 Fe1 C1 C2 173.5(2) . . . . ? C4 Fe1 C1 C2 -81.0(2) . . . . ? C3 Fe1 C1 C2 -37.7(2) . . . . ? C5 Fe1 C1 C6 118.8(4) . . . . ? C13 Fe1 C1 C6 -71.3(5) . . . . ? C12 Fe1 C1 C6 -34.7(3) . . . . ? C2 Fe1 C1 C6 -123.2(4) . . . . ? C16 Fe1 C1 C6 9.1(3) . . . . ? C14 Fe1 C1 C6 84.7(7) . . . . ? C15 Fe1 C1 C6 50.4(4) . . . . ? C4 Fe1 C1 C6 155.8(3) . . . . ? C3 Fe1 C1 C6 -160.9(3) . . . . ? C5 C1 C2 C3 0.5(4) . . . . ? C6 C1 C2 C3 174.2(4) . . . . ? Fe1 C1 C2 C3 59.9(2) . . . . ? C5 C1 C2 Fe1 -59.4(2) . . . . ? C6 C1 C2 Fe1 114.3(4) . . . . ? C5 Fe1 C2 C3 -80.4(2) . . . . ? C13 Fe1 C2 C3 84.3(2) . . . . ? C12 Fe1 C2 C3 129.1(2) . . . . ? C1 Fe1 C2 C3 -118.9(3) . . . . ? C16 Fe1 C2 C3 171.6(2) . . . . ? C14 Fe1 C2 C3 46.2(4) . . . . ? C15 Fe1 C2 C3 -144.7(7) . . . . ? C4 Fe1 C2 C3 -37.1(2) . . . . ? C5 Fe1 C2 C1 38.4(2) . . . . ? C13 Fe1 C2 C1 -156.8(2) . . . . ? C12 Fe1 C2 C1 -112.0(2) . . . . ? C16 Fe1 C2 C1 -69.6(3) . . . . ? C14 Fe1 C2 C1 165.0(3) . . . . ? C15 Fe1 C2 C1 -25.9(8) . . . . ? C4 Fe1 C2 C1 81.7(2) . . . . ? C3 Fe1 C2 C1 118.9(3) . . . . ? C1 C2 C3 C4 -0.3(4) . . . . ? Fe1 C2 C3 C4 58.9(3) . . . . ? C1 C2 C3 Fe1 -59.2(2) . . . . ? C5 Fe1 C3 C4 -37.1(2) . . . . ? C13 Fe1 C3 C4 126.0(2) . . . . ? C12 Fe1 C3 C4 166.5(2) . . . . ? C1 Fe1 C3 C4 -81.3(2) . . . . ? C2 Fe1 C3 C4 -119.7(3) . . . . ? C16 Fe1 C3 C4 -160.7(9) . . . . ? C14 Fe1 C3 C4 83.0(3) . . . . ? C15 Fe1 C3 C4 47.4(4) . . . . ? C5 Fe1 C3 C2 82.6(2) . . . . ? C13 Fe1 C3 C2 -114.3(2) . . . . ? C12 Fe1 C3 C2 -73.8(3) . . . . ? C1 Fe1 C3 C2 38.4(2) . . . . ? C16 Fe1 C3 C2 -41.0(10) . . . . ? C14 Fe1 C3 C2 -157.3(2) . . . . ? C15 Fe1 C3 C2 167.1(3) . . . . ? C4 Fe1 C3 C2 119.7(3) . . . . ? C2 C3 C4 C5 -0.1(4) . . . . ? Fe1 C3 C4 C5 58.5(3) . . . . ? C2 C3 C4 Fe1 -58.6(3) . . . . ? C13 Fe1 C4 C5 165.8(2) . . . . ? C12 Fe1 C4 C5 -172.4(6) . . . . ? C1 Fe1 C4 C5 -37.7(2) . . . . ? C2 Fe1 C4 C5 -82.4(2) . . . . ? C16 Fe1 C4 C5 53.9(4) . . . . ? C14 Fe1 C4 C5 127.2(2) . . . . ? C15 Fe1 C4 C5 85.2(2) . . . . ? C3 Fe1 C4 C5 -120.0(3) . . . . ? C5 Fe1 C4 C3 120.0(3) . . . . ? C13 Fe1 C4 C3 -74.2(3) . . . . ? C12 Fe1 C4 C3 -52.5(8) . . . . ? C1 Fe1 C4 C3 82.2(2) . . . . ? C2 Fe1 C4 C3 37.5(2) . . . . ? C16 Fe1 C4 C3 173.9(3) . . . . ? C14 Fe1 C4 C3 -112.9(2) . . . . ? C15 Fe1 C4 C3 -154.8(2) . . . . ? C3 C4 C5 C1 0.4(4) . . . . ? Fe1 C4 C5 C1 59.7(3) . . . . ? C3 C4 C5 Fe1 -59.3(3) . . . . ? C2 C1 C5 C4 -0.6(4) . . . . ? C6 C1 C5 C4 -174.5(3) . . . . ? Fe1 C1 C5 C4 -60.2(3) . . . . ? C2 C1 C5 Fe1 59.6(2) . . . . ? C6 C1 C5 Fe1 -114.3(4) . . . . ? C13 Fe1 C5 C4 -44.3(6) . . . . ? C12 Fe1 C5 C4 176.4(3) . . . . ? C1 Fe1 C5 C4 119.7(3) . . . . ? C2 Fe1 C5 C4 81.0(2) . . . . ? C16 Fe1 C5 C4 -151.9(2) . . . . ? C14 Fe1 C5 C4 -70.8(3) . . . . ? C15 Fe1 C5 C4 -110.0(2) . . . . ? C3 Fe1 C5 C4 37.1(2) . . . . ? C13 Fe1 C5 C1 -164.0(5) . . . . ? C12 Fe1 C5 C1 56.6(4) . . . . ? C2 Fe1 C5 C1 -38.8(2) . . . . ? C16 Fe1 C5 C1 88.3(2) . . . . ? C14 Fe1 C5 C1 169.5(2) . . . . ? C15 Fe1 C5 C1 130.2(2) . . . . ? C4 Fe1 C5 C1 -119.7(3) . . . . ? C3 Fe1 C5 C1 -82.6(2) . . . . ? C7 N1 C6 O1 5.1(6) . . . . ? C7 N1 C6 C1 -173.5(3) . . . . ? C5 C1 C6 O1 4.2(6) . . . . ? C2 C1 C6 O1 -168.4(3) . . . . ? Fe1 C1 C6 O1 -80.8(4) . . . . ? C5 C1 C6 N1 -177.2(3) . . . . ? C2 C1 C6 N1 10.3(5) . . . . ? Fe1 C1 C6 N1 97.8(3) . . . . ? C6 N1 C7 C11 173.6(3) . . . . ? C6 N1 C7 C8 -3.9(6) . . . . ? C9 N2 C8 C7 0.3(6) . . . . ? C11 C7 C8 N2 -0.2(6) . . . . ? N1 C7 C8 N2 177.3(4) . . . . ? C8 N2 C9 C10 0.8(6) . . . . ? N2 C9 C10 C11 -2.1(6) . . . . ? C9 C10 C11 C7 2.1(6) . . . . ? C8 C7 C11 C10 -1.0(6) . . . . ? N1 C7 C11 C10 -178.7(3) . . . . ? C5 Fe1 C12 C13 164.0(3) . . . . ? C1 Fe1 C12 C13 -156.7(2) . . . . ? C2 Fe1 C12 C13 -111.6(2) . . . . ? C16 Fe1 C12 C13 118.5(3) . . . . ? C14 Fe1 C12 C13 37.7(2) . . . . ? C15 Fe1 C12 C13 81.0(2) . . . . ? C4 Fe1 C12 C13 -26.7(7) . . . . ? C3 Fe1 C12 C13 -69.5(3) . . . . ? C5 Fe1 C12 C16 45.5(4) . . . . ? C13 Fe1 C12 C16 -118.5(3) . . . . ? C1 Fe1 C12 C16 84.8(2) . . . . ? C2 Fe1 C12 C16 129.9(2) . . . . ? C14 Fe1 C12 C16 -80.8(2) . . . . ? C15 Fe1 C12 C16 -37.5(2) . . . . ? C4 Fe1 C12 C16 -145.2(6) . . . . ? C3 Fe1 C12 C16 172.1(2) . . . . ? C5 Fe1 C12 C17 -78.7(4) . . . . ? C13 Fe1 C12 C17 117.3(4) . . . . ? C1 Fe1 C12 C17 -39.4(3) . . . . ? C2 Fe1 C12 C17 5.7(3) . . . . ? C16 Fe1 C12 C17 -124.2(4) . . . . ? C14 Fe1 C12 C17 155.0(3) . . . . ? C15 Fe1 C12 C17 -161.6(3) . . . . ? C4 Fe1 C12 C17 90.7(7) . . . . ? C3 Fe1 C12 C17 47.9(4) . . . . ? C16 C12 C13 C14 -0.5(4) . . . . ? C17 C12 C13 C14 178.1(3) . . . . ? Fe1 C12 C13 C14 -60.3(3) . . . . ? C16 C12 C13 Fe1 59.8(2) . . . . ? C17 C12 C13 Fe1 -121.5(3) . . . . ? C5 Fe1 C13 C14 -34.1(7) . . . . ? C12 Fe1 C13 C14 118.6(3) . . . . ? C1 Fe1 C13 C14 170.4(3) . . . . ? C2 Fe1 C13 C14 -152.8(2) . . . . ? C16 Fe1 C13 C14 80.3(3) . . . . ? C15 Fe1 C13 C14 36.8(2) . . . . ? C4 Fe1 C13 C14 -68.6(3) . . . . ? C3 Fe1 C13 C14 -109.6(3) . . . . ? C5 Fe1 C13 C12 -152.7(5) . . . . ? C1 Fe1 C13 C12 51.8(4) . . . . ? C2 Fe1 C13 C12 88.6(2) . . . . ? C16 Fe1 C13 C12 -38.3(2) . . . . ? C14 Fe1 C13 C12 -118.6(3) . . . . ? C15 Fe1 C13 C12 -81.8(2) . . . . ? C4 Fe1 C13 C12 172.8(2) . . . . ? C3 Fe1 C13 C12 131.8(2) . . . . ? C12 C13 C14 C15 0.9(4) . . . . ? Fe1 C13 C14 C15 -58.9(3) . . . . ? C12 C13 C14 Fe1 59.8(2) . . . . ? C5 Fe1 C14 C13 168.9(2) . . . . ? C12 Fe1 C14 C13 -38.4(2) . . . . ? C1 Fe1 C14 C13 -164.1(5) . . . . ? C2 Fe1 C14 C13 56.1(4) . . . . ? C16 Fe1 C14 C13 -82.9(2) . . . . ? C15 Fe1 C14 C13 -120.5(3) . . . . ? C4 Fe1 C14 C13 129.6(2) . . . . ? C3 Fe1 C14 C13 87.8(3) . . . . ? C5 Fe1 C14 C15 -70.6(3) . . . . ? C13 Fe1 C14 C15 120.5(3) . . . . ? C12 Fe1 C14 C15 82.1(2) . . . . ? C1 Fe1 C14 C15 -43.6(7) . . . . ? C2 Fe1 C14 C15 176.6(3) . . . . ? C16 Fe1 C14 C15 37.6(2) . . . . ? C4 Fe1 C14 C15 -109.9(2) . . . . ? C3 Fe1 C14 C15 -151.7(2) . . . . ? C13 C14 C15 C16 -1.0(4) . . . . ? Fe1 C14 C15 C16 -59.5(3) . . . . ? C13 C14 C15 Fe1 58.5(3) . . . . ? C5 Fe1 C15 C14 127.3(2) . . . . ? C13 Fe1 C15 C14 -36.8(2) . . . . ? C12 Fe1 C15 C14 -81.2(2) . . . . ? C1 Fe1 C15 C14 166.6(2) . . . . ? C2 Fe1 C15 C14 -171.9(6) . . . . ? C16 Fe1 C15 C14 -119.2(3) . . . . ? C4 Fe1 C15 C14 85.4(3) . . . . ? C3 Fe1 C15 C14 53.8(4) . . . . ? C5 Fe1 C15 C16 -113.5(2) . . . . ? C13 Fe1 C15 C16 82.4(2) . . . . ? C12 Fe1 C15 C16 38.0(2) . . . . ? C1 Fe1 C15 C16 -74.1(3) . . . . ? C2 Fe1 C15 C16 -52.7(8) . . . . ? C14 Fe1 C15 C16 119.2(3) . . . . ? C4 Fe1 C15 C16 -155.4(2) . . . . ? C3 Fe1 C15 C16 173.0(3) . . . . ? C14 C15 C16 C12 0.7(4) . . . . ? Fe1 C15 C16 C12 -58.9(2) . . . . ? C14 C15 C16 Fe1 59.6(3) . . . . ? C13 C12 C16 C15 -0.1(4) . . . . ? C17 C12 C16 C15 -178.7(3) . . . . ? Fe1 C12 C16 C15 59.4(2) . . . . ? C13 C12 C16 Fe1 -59.5(2) . . . . ? C17 C12 C16 Fe1 122.0(4) . . . . ? C5 Fe1 C16 C15 82.6(2) . . . . ? C13 Fe1 C16 C15 -80.9(2) . . . . ? C12 Fe1 C16 C15 -119.2(3) . . . . ? C1 Fe1 C16 C15 126.5(2) . . . . ? C2 Fe1 C16 C15 167.5(2) . . . . ? C14 Fe1 C16 C15 -37.4(2) . . . . ? C4 Fe1 C16 C15 46.7(4) . . . . ? C3 Fe1 C16 C15 -157.6(9) . . . . ? C5 Fe1 C16 C12 -158.3(2) . . . . ? C13 Fe1 C16 C12 38.3(2) . . . . ? C1 Fe1 C16 C12 -114.3(2) . . . . ? C2 Fe1 C16 C12 -73.4(3) . . . . ? C14 Fe1 C16 C12 81.7(2) . . . . ? C15 Fe1 C16 C12 119.2(3) . . . . ? C4 Fe1 C16 C12 165.9(3) . . . . ? C3 Fe1 C16 C12 -38.5(10) . . . . ? C18 N3 C17 O2 -2.8(6) . . . . ? C18 N3 C17 C12 176.3(3) . . . . ? C13 C12 C17 O2 7.9(5) . . . . ? C16 C12 C17 O2 -173.8(4) . . . . ? Fe1 C12 C17 O2 -80.6(4) . . . . ? C13 C12 C17 N3 -171.1(3) . . . . ? C16 C12 C17 N3 7.2(5) . . . . ? Fe1 C12 C17 N3 100.4(3) . . . . ? C17 N3 C18 C19 165.9(4) . . . . ? C17 N3 C18 C22 -14.9(6) . . . . ? C22 C18 C19 C20 -0.7(6) . . . . ? N3 C18 C19 C20 178.6(4) . . . . ? C18 C19 C20 C21 0.8(7) . . . . ? C22 N4 C21 C20 0.7(6) . . . . ? C19 C20 C21 N4 -0.8(7) . . . . ? C21 N4 C22 C18 -0.7(6) . . . . ? C19 C18 C22 N4 0.7(6) . . . . ? N3 C18 C22 N4 -178.6(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3E N4 0.85 1.99 2.843(5) 178.5 1_554 O3 H3F O1 0.85 2.03 2.879(4) 179.2 1_655 N1 H1A O2 0.86 2.15 2.969(3) 159.9 2_656 N3 H3A N2 0.86 2.29 3.114(4) 159.4 2_546 _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.916 _refine_diff_density_min -0.293 _refine_diff_density_rms 0.082 # Attachment 'complex 1.cif' data_complex_1 _database_code_depnum_ccdc_archive 'CCDC 273381' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C92 H92 Cl4 Cu2 Fe4 N16 O30' _chemical_formula_weight 2394.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fddd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' _cell_length_a 17.4718(13) _cell_length_b 22.0788(16) _cell_length_c 51.605(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 19907(2) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description octahedron _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9792 _exptl_absorpt_coefficient_mu 1.183 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7180 _exptl_absorpt_correction_T_max 0.8519 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _diffrn_ambient_temperature 123(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 area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 24984 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -54 _diffrn_reflns_limit_l_max 61 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4396 _reflns_number_gt 3569 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material SHELXL-97 _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^)+(0.0906P)^2^+124.1694P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4396 _refine_ls_number_parameters 329 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.1672 _refine_ls_wR_factor_gt 0.1525 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _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 Cu1 Cu 0.6250 0.26976(3) 0.1250 0.0345(2) Uani 1 2 d S . . Fe1 Fe 0.91813(4) 0.10538(3) 0.026737(12) 0.0361(2) Uani 1 1 d . . . Cl1 Cl 0.8750 0.8750 0.06022(4) 0.0711(7) Uani 1 2 d S . . Cl2 Cl 0.6250 0.1250 0.96454(4) 0.0917(10) Uani 1 2 d S . . N1 N 0.7081(2) 0.16880(16) 0.03357(6) 0.0343(8) Uani 1 1 d . . . H1A H 0.7055 0.1701 0.0169 0.041 Uiso 1 1 calc R . . N2 N 0.6209(2) 0.25962(17) 0.08573(7) 0.0364(9) Uani 1 1 d . . . N3 N 0.88846(16) 0.07637(12) 0.09455(5) 0.0437(10) Uani 1 1 d . . . H3A H 0.8608 0.1068 0.0900 0.052 Uiso 1 1 calc R . . N4 N 0.74145(16) -0.01157(12) 0.12700(5) 0.0375(9) Uani 1 1 d R . . O1 O 0.7573(2) 0.11709(16) 0.06717(6) 0.0482(9) Uani 1 1 d . . . O2 O 1.0080(2) 0.0366(2) 0.09170(9) 0.0811(14) Uani 1 1 d . . . O3 O 0.6250 0.3688(2) 0.1250 0.0669(16) Uani 1 2 d S . . H3B H 0.6307 0.3812 0.1399 0.100 Uiso 0.50 1 calc PR . . O4 O 0.9024(3) 0.8270(2) 0.07478(9) 0.0830(14) Uani 1 1 d . . . O5 O 0.8164(6) 0.8569(5) 0.0441(2) 0.259(7) Uani 1 1 d . . . O6 O 0.6867(3) 0.1090(3) 0.94870(11) 0.112(2) Uani 1 1 d . . . O7 O 0.6459(7) 0.1736(4) 0.98028(14) 0.213(5) Uani 1 1 d . . . O8 O 0.6080(2) 0.44135(15) 0.08305(12) 0.137(3) Uani 1 1 d . . . H8A H 0.5740 0.4631 0.0888 0.205 Uiso 1 1 calc R . . C1 C 0.80355(17) 0.09303(14) 0.02522(6) 0.0342(10) Uani 1 1 d R . . C2 C 0.83074(17) 0.11238(14) 0.00039(6) 0.0411(11) Uani 1 1 d R . . H2 H 0.8152 0.1490 -0.0089 0.049 Uiso 1 1 calc R . . C3 C 0.8844(3) 0.0685(2) -0.00818(10) 0.0513(13) Uani 1 1 d . . . H3 H 0.9135 0.0704 -0.0244 0.062 Uiso 1 1 calc R . . C4 C 0.8905(3) 0.0229(2) 0.01061(10) 0.0497(13) Uani 1 1 d . . . H4 H 0.9242 -0.0125 0.0097 0.060 Uiso 1 1 calc R . . C5 C 0.8414(3) 0.0377(2) 0.03161(9) 0.0379(10) Uani 1 1 d . . . H5 H 0.8339 0.0137 0.0474 0.046 Uiso 1 1 calc R . . C6 C 0.9398(3) 0.1680(2) 0.05466(10) 0.0475(12) Uani 1 1 d . . . H6 H 0.9014 0.1895 0.0650 0.057 Uiso 1 1 calc R . . C7 C 0.9713(3) 0.1878(3) 0.03107(11) 0.0534(14) Uani 1 1 d . . . H7 H 0.9576 0.2252 0.0219 0.064 Uiso 1 1 calc R . . C8 C 1.0248(3) 0.1448(3) 0.02254(11) 0.0600(16) Uani 1 1 d . . . H8 H 1.0545 0.1469 0.0065 0.072 Uiso 1 1 calc R . . C9 C 1.0270(3) 0.0973(3) 0.04076(10) 0.0538(14) Uani 1 1 d . . . H9 H 1.0592 0.0610 0.0397 0.065 Uiso 1 1 calc R . . C10 C 0.9746(3) 0.1113(2) 0.06105(10) 0.0471(12) Uani 1 1 d . . . C11 C 0.7553(2) 0.12664(19) 0.04361(8) 0.0332(9) Uani 1 1 d . . . C12 C 0.6628(2) 0.21079(19) 0.04697(8) 0.0318(9) Uani 1 1 d . . . C13 C 0.6626(3) 0.2172(2) 0.07377(8) 0.0362(10) Uani 1 1 d . . . H13 H 0.6925 0.1911 0.0837 0.043 Uiso 1 1 calc R . . C14 C 0.5765(3) 0.2965(2) 0.07185(9) 0.0402(11) Uani 1 1 d . . . H14 H 0.5473 0.3256 0.0803 0.048 Uiso 1 1 calc R . . C15 C 0.5730(3) 0.2923(2) 0.04512(9) 0.0424(11) Uani 1 1 d . . . H15 H 0.5417 0.3183 0.0357 0.051 Uiso 1 1 calc R . . C16 C 0.6162(3) 0.2493(2) 0.03276(8) 0.0366(10) Uani 1 1 d . . . H16 H 0.6142 0.2459 0.0148 0.044 Uiso 1 1 calc R . . C17 C 0.9600(3) 0.0714(2) 0.08379(10) 0.0487(12) Uani 1 1 d . . . C18 C 0.8571(3) 0.0354(2) 0.11247(8) 0.0381(10) Uani 1 1 d . . . C19 C 0.7788(3) 0.0288(2) 0.11235(8) 0.0353(10) Uani 1 1 d . . . H19 H 0.7503 0.0537 0.1015 0.042 Uiso 1 1 calc R . . C20 C 0.7823(3) -0.0458(2) 0.14296(9) 0.0457(12) Uani 1 1 d . . . H20 H 0.7574 -0.0743 0.1532 0.055 Uiso 1 1 calc R . . C21 C 0.8603(3) -0.0402(3) 0.14477(10) 0.0514(13) Uani 1 1 d . . . H21 H 0.8871 -0.0644 0.1564 0.062 Uiso 1 1 calc R . . C22 C 0.8995(3) 0.0006(3) 0.12960(9) 0.0505(13) Uani 1 1 d . . . H22 H 0.9523 0.0047 0.1308 0.061 Uiso 1 1 calc R . . C23 C 0.6723(5) 0.4739(7) 0.0802(3) 0.179(6) Uani 1 1 d . . . H23A H 0.6768 0.5022 0.0943 0.269 Uiso 1 1 calc R . . H23B H 0.6704 0.4957 0.0641 0.269 Uiso 1 1 calc R . . H23C H 0.7157 0.4473 0.0802 0.269 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 Cu1 0.0474(5) 0.0390(4) 0.0173(4) 0.000 0.0003(3) 0.000 Fe1 0.0376(4) 0.0390(4) 0.0316(4) 0.0037(3) 0.0054(3) 0.0002(3) Cl1 0.0980(17) 0.0668(13) 0.0484(11) 0.000 0.000 0.0506(13) Cl2 0.136(2) 0.120(2) 0.0193(9) 0.000 0.000 0.0746(19) N1 0.047(2) 0.040(2) 0.0162(17) 0.0011(14) -0.0025(15) 0.0098(17) N2 0.043(2) 0.044(2) 0.0226(18) 0.0034(16) -0.0010(16) 0.0063(18) N3 0.044(2) 0.052(2) 0.035(2) 0.0151(19) 0.0017(17) 0.0064(19) N4 0.049(2) 0.041(2) 0.0221(18) 0.0049(16) -0.0004(16) 0.0022(18) O1 0.056(2) 0.060(2) 0.0289(18) 0.0154(15) 0.0065(15) 0.0216(17) O2 0.053(2) 0.114(4) 0.076(3) 0.046(3) 0.007(2) 0.025(3) O3 0.102(5) 0.044(3) 0.054(3) 0.000 0.002(3) 0.000 O4 0.101(4) 0.072(3) 0.076(3) 0.017(2) -0.003(3) 0.033(3) O5 0.318(12) 0.210(9) 0.249(10) -0.160(9) -0.219(10) 0.186(10) O6 0.112(4) 0.150(5) 0.075(4) -0.036(4) 0.018(3) 0.014(4) O7 0.350(13) 0.190(8) 0.098(5) -0.096(5) -0.114(7) 0.157(8) O8 0.152(6) 0.109(5) 0.150(7) 0.032(5) 0.011(5) 0.037(5) C1 0.037(2) 0.036(2) 0.030(2) -0.0002(19) 0.0012(18) -0.0027(19) C2 0.047(3) 0.048(3) 0.029(2) 0.001(2) 0.002(2) 0.001(2) C3 0.059(3) 0.058(3) 0.037(3) -0.012(2) 0.010(2) -0.001(3) C4 0.062(3) 0.036(3) 0.052(3) -0.008(2) 0.010(3) 0.004(2) C5 0.043(3) 0.031(2) 0.040(3) 0.0016(19) 0.004(2) -0.002(2) C6 0.055(3) 0.045(3) 0.042(3) -0.001(2) -0.006(2) -0.009(2) C7 0.060(3) 0.051(3) 0.049(3) 0.013(2) -0.011(3) -0.021(3) C8 0.038(3) 0.088(4) 0.054(3) 0.025(3) 0.001(2) -0.018(3) C9 0.036(3) 0.076(4) 0.049(3) 0.015(3) 0.002(2) 0.000(3) C10 0.040(3) 0.060(3) 0.041(3) 0.012(2) -0.007(2) -0.008(2) C11 0.034(2) 0.036(2) 0.030(2) 0.0053(18) 0.0012(18) -0.0009(19) C12 0.038(2) 0.036(2) 0.022(2) 0.0041(17) -0.0002(17) -0.0002(19) C13 0.045(3) 0.044(3) 0.020(2) 0.0055(19) -0.0032(18) 0.011(2) C14 0.049(3) 0.044(3) 0.028(2) 0.002(2) 0.001(2) 0.009(2) C15 0.053(3) 0.047(3) 0.027(2) 0.009(2) -0.004(2) 0.015(2) C16 0.048(3) 0.043(2) 0.019(2) 0.0036(18) -0.0035(19) 0.004(2) C17 0.045(3) 0.061(3) 0.040(3) 0.011(2) -0.006(2) 0.002(3) C18 0.049(3) 0.041(2) 0.024(2) 0.0009(19) -0.0006(19) 0.005(2) C19 0.045(3) 0.040(2) 0.021(2) 0.0032(18) -0.0001(18) 0.009(2) C20 0.056(3) 0.049(3) 0.032(2) 0.014(2) 0.001(2) 0.003(2) C21 0.060(3) 0.058(3) 0.036(3) 0.018(2) -0.008(2) 0.010(3) C22 0.049(3) 0.069(3) 0.033(3) 0.012(2) -0.005(2) 0.006(3) C23 0.065(6) 0.235(16) 0.237(16) 0.026(13) 0.005(8) -0.034(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 Cu1 N2 2.040(3) . ? Cu1 N2 2.040(3) 11_554 ? Cu1 N4 2.045(3) 8_544 ? Cu1 N4 2.045(3) 14_545 ? Cu1 O3 2.186(5) . ? Fe1 C1 2.022(3) . ? Fe1 C5 2.023(5) . ? Fe1 C10 2.031(5) . ? Fe1 C6 2.032(5) . ? Fe1 C9 2.043(5) . ? Fe1 C2 2.050(3) . ? Fe1 C7 2.056(5) . ? Fe1 C4 2.059(5) . ? Fe1 C3 2.063(5) . ? Fe1 C8 2.069(5) . ? Cl1 O5 1.379(8) 2_665 ? Cl1 O5 1.379(8) . ? Cl1 O4 1.386(4) . ? Cl1 O4 1.386(4) 2_665 ? Cl2 O7 1.394(7) . ? Cl2 O7 1.394(7) 14_545 ? Cl2 O6 1.399(5) 14_545 ? Cl2 O6 1.399(5) . ? N1 C11 1.346(6) . ? N1 C12 1.401(6) . ? N1 H1A 0.8600 . ? N2 C14 1.332(6) . ? N2 C13 1.338(6) . ? N3 C17 1.372(6) . ? N3 C18 1.404(5) . ? N3 H3A 0.8600 . ? N4 C20 1.326(5) . ? N4 C19 1.339(5) . ? N4 Cu1 2.045(3) 14_545 ? O1 C11 1.234(5) . ? O2 C17 1.210(6) . ? O3 H3B 0.8200 . ? O8 C23 1.342(11) . ? O8 H8A 0.8200 . ? C1 C5 1.428(5) . ? C1 C2 1.4318 . ? C1 C11 1.471(5) . ? C2 C3 1.418(6) . ? C2 H2 0.9800 . ? C3 C4 1.402(7) . ? C3 H3 0.9800 . ? C4 C5 1.420(7) . ? C4 H4 0.9800 . ? C5 H5 0.9800 . ? C6 C7 1.406(7) . ? C6 C10 1.430(7) . ? C6 H6 0.9800 . ? C7 C8 1.403(9) . ? C7 H7 0.9800 . ? C8 C9 1.410(8) . ? C8 H8 0.9800 . ? C9 C10 1.425(7) . ? C9 H9 0.9800 . ? C10 C17 1.489(7) . ? C12 C16 1.387(6) . ? C12 C13 1.390(6) . ? C13 H13 0.9300 . ? C14 C15 1.384(6) . ? C14 H14 0.9300 . ? C15 C16 1.371(7) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C18 C19 1.376(7) . ? C18 C22 1.386(7) . ? C19 H19 0.9300 . ? C20 C21 1.372(7) . ? C20 H20 0.9300 . ? C21 C22 1.376(7) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 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 N2 Cu1 N2 167.4(2) . 11_554 ? N2 Cu1 N4 88.57(13) . 8_544 ? N2 Cu1 N4 90.32(13) 11_554 8_544 ? N2 Cu1 N4 90.32(13) . 14_545 ? N2 Cu1 N4 88.57(13) 11_554 14_545 ? N4 Cu1 N4 169.85(16) 8_544 14_545 ? N2 Cu1 O3 96.30(11) . . ? N2 Cu1 O3 96.30(11) 11_554 . ? N4 Cu1 O3 95.08(8) 8_544 . ? N4 Cu1 O3 95.08(8) 14_545 . ? C1 Fe1 C5 41.35(15) . . ? C1 Fe1 C10 121.56(17) . . ? C5 Fe1 C10 105.1(2) . . ? C1 Fe1 C6 107.65(18) . . ? C5 Fe1 C6 122.5(2) . . ? C10 Fe1 C6 41.2(2) . . ? C1 Fe1 C9 157.48(17) . . ? C5 Fe1 C9 120.5(2) . . ? C10 Fe1 C9 41.0(2) . . ? C6 Fe1 C9 68.6(2) . . ? C1 Fe1 C2 41.16(6) . . ? C5 Fe1 C2 69.20(16) . . ? C10 Fe1 C2 159.21(18) . . ? C6 Fe1 C2 123.86(18) . . ? C9 Fe1 C2 159.20(17) . . ? C1 Fe1 C7 124.84(19) . . ? C5 Fe1 C7 160.0(2) . . ? C10 Fe1 C7 68.2(2) . . ? C6 Fe1 C7 40.2(2) . . ? C9 Fe1 C7 67.6(2) . . ? C2 Fe1 C7 110.00(18) . . ? C1 Fe1 C4 68.45(17) . . ? C5 Fe1 C4 40.69(19) . . ? C10 Fe1 C4 121.6(2) . . ? C6 Fe1 C4 158.7(2) . . ? C9 Fe1 C4 106.5(2) . . ? C2 Fe1 C4 67.91(18) . . ? C7 Fe1 C4 158.9(2) . . ? C1 Fe1 C3 68.28(17) . . ? C5 Fe1 C3 68.2(2) . . ? C10 Fe1 C3 157.8(2) . . ? C6 Fe1 C3 160.1(2) . . ? C9 Fe1 C3 122.7(2) . . ? C2 Fe1 C3 40.33(17) . . ? C7 Fe1 C3 125.0(2) . . ? C4 Fe1 C3 39.8(2) . . ? C1 Fe1 C8 160.88(19) . . ? C5 Fe1 C8 157.0(2) . . ? C10 Fe1 C8 68.1(2) . . ? C6 Fe1 C8 67.7(2) . . ? C9 Fe1 C8 40.1(2) . . ? C2 Fe1 C8 124.74(18) . . ? C7 Fe1 C8 39.8(2) . . ? C4 Fe1 C8 122.8(2) . . ? C3 Fe1 C8 109.4(2) . . ? O5 Cl1 O5 105.6(12) 2_665 . ? O5 Cl1 O4 107.0(4) 2_665 . ? O5 Cl1 O4 111.3(5) . . ? O5 Cl1 O4 111.3(5) 2_665 2_665 ? O5 Cl1 O4 107.0(4) . 2_665 ? O4 Cl1 O4 114.3(4) . 2_665 ? O7 Cl2 O7 108.7(9) . 14_545 ? O7 Cl2 O6 110.4(4) . 14_545 ? O7 Cl2 O6 109.5(6) 14_545 14_545 ? O7 Cl2 O6 109.5(6) . . ? O7 Cl2 O6 110.4(4) 14_545 . ? O6 Cl2 O6 108.5(5) 14_545 . ? C11 N1 C12 127.8(4) . . ? C11 N1 H1A 116.1 . . ? C12 N1 H1A 116.1 . . ? C14 N2 C13 119.8(4) . . ? C14 N2 Cu1 119.2(3) . . ? C13 N2 Cu1 121.0(3) . . ? C17 N3 C18 124.8(3) . . ? C17 N3 H3A 117.6 . . ? C18 N3 H3A 117.6 . . ? C20 N4 C19 117.9(4) . . ? C20 N4 Cu1 121.1(3) . 14_545 ? C19 N4 Cu1 121.0(3) . 14_545 ? Cu1 O3 H3B 109.5 . . ? C23 O8 H8A 109.5 . . ? C5 C1 C2 108.0(2) . . ? C5 C1 C11 123.3(3) . . ? C2 C1 C11 128.1(2) . . ? C5 C1 Fe1 69.4(2) . . ? C2 C1 Fe1 70.49(10) . . ? C11 C1 Fe1 118.4(2) . . ? C3 C2 C1 107.1(3) . . ? C3 C2 Fe1 70.3(3) . . ? C1 C2 Fe1 68.35(9) . . ? C3 C2 H2 126.4 . . ? C1 C2 H2 126.4 . . ? Fe1 C2 H2 126.4 . . ? C4 C3 C2 109.0(4) . . ? C4 C3 Fe1 70.0(3) . . ? C2 C3 Fe1 69.4(2) . . ? C4 C3 H3 125.5 . . ? C2 C3 H3 125.5 . . ? Fe1 C3 H3 125.5 . . ? C3 C4 C5 108.5(4) . . ? C3 C4 Fe1 70.3(3) . . ? C5 C4 Fe1 68.3(3) . . ? C3 C4 H4 125.7 . . ? C5 C4 H4 125.7 . . ? Fe1 C4 H4 125.7 . . ? C4 C5 C1 107.5(4) . . ? C4 C5 Fe1 71.0(3) . . ? C1 C5 Fe1 69.3(2) . . ? C4 C5 H5 126.3 . . ? C1 C5 H5 126.3 . . ? Fe1 C5 H5 126.3 . . ? C7 C6 C10 107.7(5) . . ? C7 C6 Fe1 70.8(3) . . ? C10 C6 Fe1 69.3(3) . . ? C7 C6 H6 126.1 . . ? C10 C6 H6 126.1 . . ? Fe1 C6 H6 126.1 . . ? C6 C7 C8 108.8(5) . . ? C6 C7 Fe1 69.0(3) . . ? C8 C7 Fe1 70.6(3) . . ? C6 C7 H7 125.6 . . ? C8 C7 H7 125.6 . . ? Fe1 C7 H7 125.6 . . ? C7 C8 C9 108.2(5) . . ? C7 C8 Fe1 69.6(3) . . ? C9 C8 Fe1 69.0(3) . . ? C7 C8 H8 125.9 . . ? C9 C8 H8 125.9 . . ? Fe1 C8 H8 125.9 . . ? C8 C9 C10 108.1(5) . . ? C8 C9 Fe1 70.9(3) . . ? C10 C9 Fe1 69.1(3) . . ? C8 C9 H9 126.0 . . ? C10 C9 H9 126.0 . . ? Fe1 C9 H9 126.0 . . ? C9 C10 C6 107.1(5) . . ? C9 C10 C17 124.1(5) . . ? C6 C10 C17 128.8(5) . . ? C9 C10 Fe1 70.0(3) . . ? C6 C10 Fe1 69.4(3) . . ? C17 C10 Fe1 124.4(4) . . ? O1 C11 N1 121.0(4) . . ? O1 C11 C1 122.2(4) . . ? N1 C11 C1 116.8(3) . . ? C16 C12 C13 117.5(4) . . ? C16 C12 N1 118.4(4) . . ? C13 C12 N1 124.0(4) . . ? N2 C13 C12 122.1(4) . . ? N2 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? N2 C14 C15 121.4(4) . . ? N2 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C16 C15 C14 119.0(4) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? C15 C16 C12 120.1(4) . . ? C15 C16 H16 119.9 . . ? C12 C16 H16 119.9 . . ? O2 C17 N3 123.1(5) . . ? O2 C17 C10 121.5(5) . . ? N3 C17 C10 115.4(4) . . ? C19 C18 C22 118.4(4) . . ? C19 C18 N3 116.9(4) . . ? C22 C18 N3 124.7(4) . . ? N4 C19 C18 123.6(4) . . ? N4 C19 H19 118.2 . . ? C18 C19 H19 118.2 . . ? N4 C20 C21 121.7(4) . . ? N4 C20 H20 119.1 . . ? C21 C20 H20 119.1 . . ? C20 C21 C22 120.9(5) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? C21 C22 C18 117.4(5) . . ? C21 C22 H22 121.3 . . ? C18 C22 H22 121.3 . . ? O8 C23 H23A 109.5 . . ? O8 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O8 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Cu1 N2 C14 139.9(4) 11_554 . . . ? N4 Cu1 N2 C14 -135.0(4) 8_544 . . . ? N4 Cu1 N2 C14 55.0(4) 14_545 . . . ? O3 Cu1 N2 C14 -40.1(4) . . . . ? N2 Cu1 N2 C13 -40.9(3) 11_554 . . . ? N4 Cu1 N2 C13 44.2(4) 8_544 . . . ? N4 Cu1 N2 C13 -125.8(4) 14_545 . . . ? O3 Cu1 N2 C13 139.1(3) . . . . ? C10 Fe1 C1 C5 -76.5(3) . . . . ? C6 Fe1 C1 C5 -119.5(3) . . . . ? C9 Fe1 C1 C5 -42.8(6) . . . . ? C2 Fe1 C1 C5 118.9(2) . . . . ? C7 Fe1 C1 C5 -160.5(3) . . . . ? C4 Fe1 C1 C5 38.2(3) . . . . ? C3 Fe1 C1 C5 81.2(3) . . . . ? C8 Fe1 C1 C5 167.9(6) . . . . ? C5 Fe1 C1 C2 -118.9(2) . . . . ? C10 Fe1 C1 C2 164.7(2) . . . . ? C6 Fe1 C1 C2 121.63(17) . . . . ? C9 Fe1 C1 C2 -161.7(5) . . . . ? C7 Fe1 C1 C2 80.6(2) . . . . ? C4 Fe1 C1 C2 -80.63(18) . . . . ? C3 Fe1 C1 C2 -37.71(18) . . . . ? C8 Fe1 C1 C2 49.0(6) . . . . ? C5 Fe1 C1 C11 117.6(4) . . . . ? C10 Fe1 C1 C11 41.1(3) . . . . ? C6 Fe1 C1 C11 -1.9(3) . . . . ? C9 Fe1 C1 C11 74.7(6) . . . . ? C2 Fe1 C1 C11 -123.6(2) . . . . ? C7 Fe1 C1 C11 -42.9(4) . . . . ? C4 Fe1 C1 C11 155.8(3) . . . . ? C3 Fe1 C1 C11 -161.3(3) . . . . ? C8 Fe1 C1 C11 -74.6(7) . . . . ? C5 C1 C2 C3 0.4(3) . . . . ? C11 C1 C2 C3 171.2(4) . . . . ? Fe1 C1 C2 C3 59.9(3) . . . . ? C5 C1 C2 Fe1 -59.5(2) . . . . ? C11 C1 C2 Fe1 111.3(3) . . . . ? C1 Fe1 C2 C3 -118.6(3) . . . . ? C5 Fe1 C2 C3 -80.4(3) . . . . ? C10 Fe1 C2 C3 -158.0(5) . . . . ? C6 Fe1 C2 C3 163.7(3) . . . . ? C9 Fe1 C2 C3 41.6(6) . . . . ? C7 Fe1 C2 C3 120.9(3) . . . . ? C4 Fe1 C2 C3 -36.5(3) . . . . ? C8 Fe1 C2 C3 78.9(4) . . . . ? C5 Fe1 C2 C1 38.23(15) . . . . ? C10 Fe1 C2 C1 -39.4(5) . . . . ? C6 Fe1 C2 C1 -77.72(19) . . . . ? C9 Fe1 C2 C1 160.2(6) . . . . ? C7 Fe1 C2 C1 -120.48(19) . . . . ? C4 Fe1 C2 C1 82.08(17) . . . . ? C3 Fe1 C2 C1 118.6(3) . . . . ? C8 Fe1 C2 C1 -162.5(3) . . . . ? C1 C2 C3 C4 0.2(4) . . . . ? Fe1 C2 C3 C4 58.9(4) . . . . ? C1 C2 C3 Fe1 -58.65(14) . . . . ? C1 Fe1 C3 C4 -82.0(3) . . . . ? C5 Fe1 C3 C4 -37.3(3) . . . . ? C10 Fe1 C3 C4 38.9(7) . . . . ? C6 Fe1 C3 C4 -163.8(6) . . . . ? C9 Fe1 C3 C4 75.8(4) . . . . ? C2 Fe1 C3 C4 -120.5(4) . . . . ? C7 Fe1 C3 C4 159.9(3) . . . . ? C8 Fe1 C3 C4 118.3(3) . . . . ? C1 Fe1 C3 C2 38.47(16) . . . . ? C5 Fe1 C3 C2 83.2(3) . . . . ? C10 Fe1 C3 C2 159.4(5) . . . . ? C6 Fe1 C3 C2 -43.3(7) . . . . ? C9 Fe1 C3 C2 -163.7(2) . . . . ? C7 Fe1 C3 C2 -79.7(3) . . . . ? C4 Fe1 C3 C2 120.5(4) . . . . ? C8 Fe1 C3 C2 -121.2(3) . . . . ? C2 C3 C4 C5 -0.8(6) . . . . ? Fe1 C3 C4 C5 57.7(4) . . . . ? C2 C3 C4 Fe1 -58.5(3) . . . . ? C1 Fe1 C4 C3 81.5(3) . . . . ? C5 Fe1 C4 C3 120.4(5) . . . . ? C10 Fe1 C4 C3 -163.8(3) . . . . ? C6 Fe1 C4 C3 164.9(5) . . . . ? C9 Fe1 C4 C3 -121.7(3) . . . . ? C2 Fe1 C4 C3 37.0(3) . . . . ? C7 Fe1 C4 C3 -51.5(7) . . . . ? C8 Fe1 C4 C3 -81.0(4) . . . . ? C1 Fe1 C4 C5 -38.9(3) . . . . ? C10 Fe1 C4 C5 75.8(4) . . . . ? C6 Fe1 C4 C5 44.5(7) . . . . ? C9 Fe1 C4 C5 117.9(3) . . . . ? C2 Fe1 C4 C5 -83.3(3) . . . . ? C7 Fe1 C4 C5 -171.8(5) . . . . ? C3 Fe1 C4 C5 -120.4(5) . . . . ? C8 Fe1 C4 C5 158.6(3) . . . . ? C3 C4 C5 C1 1.1(6) . . . . ? Fe1 C4 C5 C1 60.0(3) . . . . ? C3 C4 C5 Fe1 -58.9(4) . . . . ? C2 C1 C5 C4 -0.9(4) . . . . ? C11 C1 C5 C4 -172.2(4) . . . . ? Fe1 C1 C5 C4 -61.1(3) . . . . ? C2 C1 C5 Fe1 60.19(12) . . . . ? C11 C1 C5 Fe1 -111.1(3) . . . . ? C1 Fe1 C5 C4 118.0(4) . . . . ? C10 Fe1 C5 C4 -121.1(3) . . . . ? C6 Fe1 C5 C4 -162.4(3) . . . . ? C9 Fe1 C5 C4 -79.6(4) . . . . ? C2 Fe1 C5 C4 79.9(3) . . . . ? C7 Fe1 C5 C4 171.4(6) . . . . ? C3 Fe1 C5 C4 36.5(3) . . . . ? C8 Fe1 C5 C4 -51.9(7) . . . . ? C10 Fe1 C5 C1 120.9(3) . . . . ? C6 Fe1 C5 C1 79.6(3) . . . . ? C9 Fe1 C5 C1 162.4(2) . . . . ? C2 Fe1 C5 C1 -38.06(15) . . . . ? C7 Fe1 C5 C1 53.4(7) . . . . ? C4 Fe1 C5 C1 -118.0(4) . . . . ? C3 Fe1 C5 C1 -81.5(3) . . . . ? C8 Fe1 C5 C1 -169.8(5) . . . . ? C1 Fe1 C6 C7 -123.5(3) . . . . ? C5 Fe1 C6 C7 -166.5(3) . . . . ? C10 Fe1 C6 C7 118.4(5) . . . . ? C9 Fe1 C6 C7 80.1(4) . . . . ? C2 Fe1 C6 C7 -81.1(4) . . . . ? C4 Fe1 C6 C7 160.7(6) . . . . ? C3 Fe1 C6 C7 -48.7(8) . . . . ? C8 Fe1 C6 C7 36.8(3) . . . . ? C1 Fe1 C6 C10 118.0(3) . . . . ? C5 Fe1 C6 C10 75.1(3) . . . . ? C9 Fe1 C6 C10 -38.4(3) . . . . ? C2 Fe1 C6 C10 160.5(3) . . . . ? C7 Fe1 C6 C10 -118.4(5) . . . . ? C4 Fe1 C6 C10 42.2(7) . . . . ? C3 Fe1 C6 C10 -167.2(6) . . . . ? C8 Fe1 C6 C10 -81.7(3) . . . . ? C10 C6 C7 C8 0.2(6) . . . . ? Fe1 C6 C7 C8 -59.6(4) . . . . ? C10 C6 C7 Fe1 59.7(3) . . . . ? C1 Fe1 C7 C6 75.5(4) . . . . ? C5 Fe1 C7 C6 35.2(8) . . . . ? C10 Fe1 C7 C6 -38.6(3) . . . . ? C9 Fe1 C7 C6 -83.0(3) . . . . ? C2 Fe1 C7 C6 119.2(3) . . . . ? C4 Fe1 C7 C6 -160.5(6) . . . . ? C3 Fe1 C7 C6 161.9(3) . . . . ? C8 Fe1 C7 C6 -120.1(5) . . . . ? C1 Fe1 C7 C8 -164.4(3) . . . . ? C5 Fe1 C7 C8 155.3(5) . . . . ? C10 Fe1 C7 C8 81.5(3) . . . . ? C6 Fe1 C7 C8 120.1(5) . . . . ? C9 Fe1 C7 C8 37.1(3) . . . . ? C2 Fe1 C7 C8 -120.7(3) . . . . ? C4 Fe1 C7 C8 -40.4(7) . . . . ? C3 Fe1 C7 C8 -78.1(4) . . . . ? C6 C7 C8 C9 0.3(6) . . . . ? Fe1 C7 C8 C9 -58.3(4) . . . . ? C6 C7 C8 Fe1 58.6(4) . . . . ? C1 Fe1 C8 C7 42.3(8) . . . . ? C5 Fe1 C8 C7 -158.6(5) . . . . ? C10 Fe1 C8 C7 -81.8(4) . . . . ? C6 Fe1 C8 C7 -37.2(3) . . . . ? C9 Fe1 C8 C7 -120.0(5) . . . . ? C2 Fe1 C8 C7 79.5(4) . . . . ? C4 Fe1 C8 C7 163.9(3) . . . . ? C3 Fe1 C8 C7 121.8(3) . . . . ? C1 Fe1 C8 C9 162.3(5) . . . . ? C5 Fe1 C8 C9 -38.6(7) . . . . ? C10 Fe1 C8 C9 38.2(4) . . . . ? C6 Fe1 C8 C9 82.9(4) . . . . ? C2 Fe1 C8 C9 -160.5(3) . . . . ? C7 Fe1 C8 C9 120.0(5) . . . . ? C4 Fe1 C8 C9 -76.1(4) . . . . ? C3 Fe1 C8 C9 -118.2(4) . . . . ? C7 C8 C9 C10 -0.6(6) . . . . ? Fe1 C8 C9 C10 -59.3(4) . . . . ? C7 C8 C9 Fe1 58.7(4) . . . . ? C1 Fe1 C9 C8 -165.0(5) . . . . ? C5 Fe1 C9 C8 163.6(3) . . . . ? C10 Fe1 C9 C8 -118.9(5) . . . . ? C6 Fe1 C9 C8 -80.3(4) . . . . ? C2 Fe1 C9 C8 50.6(7) . . . . ? C7 Fe1 C9 C8 -36.8(4) . . . . ? C4 Fe1 C9 C8 121.6(4) . . . . ? C3 Fe1 C9 C8 81.3(4) . . . . ? C1 Fe1 C9 C10 -46.0(7) . . . . ? C5 Fe1 C9 C10 -77.5(4) . . . . ? C6 Fe1 C9 C10 38.6(3) . . . . ? C2 Fe1 C9 C10 169.5(4) . . . . ? C7 Fe1 C9 C10 82.1(4) . . . . ? C4 Fe1 C9 C10 -119.4(3) . . . . ? C3 Fe1 C9 C10 -159.7(3) . . . . ? C8 Fe1 C9 C10 118.9(5) . . . . ? C8 C9 C10 C6 0.7(6) . . . . ? Fe1 C9 C10 C6 -59.8(3) . . . . ? C8 C9 C10 C17 179.2(5) . . . . ? Fe1 C9 C10 C17 118.7(5) . . . . ? C8 C9 C10 Fe1 60.5(4) . . . . ? C7 C6 C10 C9 -0.5(6) . . . . ? Fe1 C6 C10 C9 60.1(4) . . . . ? C7 C6 C10 C17 -178.9(5) . . . . ? Fe1 C6 C10 C17 -118.3(5) . . . . ? C7 C6 C10 Fe1 -60.7(3) . . . . ? C1 Fe1 C10 C9 161.1(3) . . . . ? C5 Fe1 C10 C9 119.4(3) . . . . ? C6 Fe1 C10 C9 -118.1(4) . . . . ? C2 Fe1 C10 C9 -169.5(4) . . . . ? C7 Fe1 C10 C9 -80.4(4) . . . . ? C4 Fe1 C10 C9 78.5(4) . . . . ? C3 Fe1 C10 C9 50.4(7) . . . . ? C8 Fe1 C10 C9 -37.4(3) . . . . ? C1 Fe1 C10 C6 -80.7(3) . . . . ? C5 Fe1 C10 C6 -122.4(3) . . . . ? C9 Fe1 C10 C6 118.1(4) . . . . ? C2 Fe1 C10 C6 -51.4(6) . . . . ? C7 Fe1 C10 C6 37.7(3) . . . . ? C4 Fe1 C10 C6 -163.3(3) . . . . ? C3 Fe1 C10 C6 168.5(5) . . . . ? C8 Fe1 C10 C6 80.7(3) . . . . ? C1 Fe1 C10 C17 42.9(5) . . . . ? C5 Fe1 C10 C17 1.2(5) . . . . ? C6 Fe1 C10 C17 123.6(6) . . . . ? C9 Fe1 C10 C17 -118.2(6) . . . . ? C2 Fe1 C10 C17 72.2(7) . . . . ? C7 Fe1 C10 C17 161.3(5) . . . . ? C4 Fe1 C10 C17 -39.7(5) . . . . ? C3 Fe1 C10 C17 -67.9(8) . . . . ? C8 Fe1 C10 C17 -155.7(5) . . . . ? C12 N1 C11 O1 7.2(7) . . . . ? C12 N1 C11 C1 -172.7(4) . . . . ? C5 C1 C11 O1 16.3(6) . . . . ? C2 C1 C11 O1 -153.1(3) . . . . ? Fe1 C1 C11 O1 -66.5(5) . . . . ? C5 C1 C11 N1 -163.7(4) . . . . ? C2 C1 C11 N1 26.9(5) . . . . ? Fe1 C1 C11 N1 113.5(4) . . . . ? C11 N1 C12 C16 -178.0(4) . . . . ? C11 N1 C12 C13 3.2(7) . . . . ? C14 N2 C13 C12 1.5(7) . . . . ? Cu1 N2 C13 C12 -177.7(3) . . . . ? C16 C12 C13 N2 -1.7(7) . . . . ? N1 C12 C13 N2 177.1(4) . . . . ? C13 N2 C14 C15 -0.6(7) . . . . ? Cu1 N2 C14 C15 178.6(4) . . . . ? N2 C14 C15 C16 0.0(8) . . . . ? C14 C15 C16 C12 -0.2(7) . . . . ? C13 C12 C16 C15 1.0(7) . . . . ? N1 C12 C16 C15 -177.8(4) . . . . ? C18 N3 C17 O2 -12.1(8) . . . . ? C18 N3 C17 C10 166.6(4) . . . . ? C9 C10 C17 O2 26.9(8) . . . . ? C6 C10 C17 O2 -155.0(6) . . . . ? Fe1 C10 C17 O2 114.7(6) . . . . ? C9 C10 C17 N3 -151.9(5) . . . . ? C6 C10 C17 N3 26.3(8) . . . . ? Fe1 C10 C17 N3 -64.0(6) . . . . ? C17 N3 C18 C19 -150.4(4) . . . . ? C17 N3 C18 C22 27.8(7) . . . . ? C20 N4 C19 C18 1.8(6) . . . . ? Cu1 N4 C19 C18 -178.6(3) 14_545 . . . ? C22 C18 C19 N4 -3.3(7) . . . . ? N3 C18 C19 N4 175.1(4) . . . . ? C19 N4 C20 C21 0.5(7) . . . . ? Cu1 N4 C20 C21 -179.1(4) 14_545 . . . ? N4 C20 C21 C22 -1.3(8) . . . . ? C20 C21 C22 C18 -0.2(8) . . . . ? C19 C18 C22 C21 2.4(8) . . . . ? N3 C18 C22 C21 -175.9(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O7 0.86 2.16 2.959(7) 154.3 1_554 N3 H3A O1 0.86 2.17 2.838(4) 134.4 . O3 H3B O8 0.82 1.94 2.710(7) 156.2 11_554 O8 H8A O2 0.82 2.00 2.770(6) 157.1 13_455 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.043 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.134 # Attachment 'complex 2.cif' data_complex_2 _database_code_depnum_ccdc_archive 'CCDC 294229' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H76 Cl4 Fe4 N16 Ni2 O22' _chemical_formula_weight 2192.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fddd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' _cell_length_a 18.45(2) _cell_length_b 22.31(2) _cell_length_c 54.77(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 22541(44) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4073 _cell_measurement_theta_min 2.338 _cell_measurement_theta_max 21.673 _exptl_crystal_description octahedral _exptl_crystal_colour orange _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8960 _exptl_absorpt_coefficient_mu 0.990 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6479 _exptl_absorpt_correction_T_max 0.7232 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 19803 _diffrn_reflns_av_R_equivalents 0.0658 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -65 _diffrn_reflns_limit_l_max 63 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4315 _reflns_number_gt 2213 _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4315 _refine_ls_number_parameters 321 _refine_ls_number_restraints 267 _refine_ls_R_factor_all 0.1783 _refine_ls_R_factor_gt 0.1012 _refine_ls_wR_factor_ref 0.3331 _refine_ls_wR_factor_gt 0.2504 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.41920(8) 0.14318(6) 0.72661(3) 0.0601(5) Uani 1 1 d . . . Ni1 Ni 0.1250 0.00776(7) 0.6250 0.0496(5) Uani 1 2 d S . . Cl1 Cl 0.1250 0.1250 0.6250 0.0495(10) Uani 1 4 d S . . Cl2 Cl 0.3750 0.3750 0.69086(9) 0.110(3) Uani 0.75 2 d SPDU . . Cl3 Cl 0.3750 0.8750 0.71458(12) 0.153(4) Uani 0.75 2 d SPDU . . N1 N 0.2173(5) 0.0872(4) 0.71625(15) 0.069(2) Uani 1 1 d DU . . H1 H 0.2156 0.0850 0.7319 0.083 Uiso 1 1 calc R . . N2 N 0.1192(3) 0.0086(3) 0.66461(13) 0.0489(16) Uani 1 1 d . . . N3 N 0.3983(5) 0.1720(4) 0.65614(17) 0.078(2) Uani 1 1 d DU . . H3 H 0.3732 0.1408 0.6598 0.094 Uiso 1 1 calc R . . N4 N 0.2440(4) 0.2441(3) 0.62223(13) 0.0579(19) Uani 1 1 d . . . O1 O 0.2667(6) 0.1366(4) 0.68610(17) 0.109(3) Uani 1 1 d DU . . O2 O 0.5084(5) 0.2104(5) 0.65983(19) 0.114(3) Uani 1 1 d DU . . O3 O 0.1250 -0.0910(4) 0.6250 0.071(3) Uani 1 2 d S . . H2 H 0.0948 -0.1140 0.6320 0.086 Uiso 1 1 d R . . O4 O 0.3572(9) 0.3243(4) 0.6771(2) 0.151(5) Uani 0.75 1 d PDU . . O5 O 0.3142(5) 0.3881(7) 0.7062(3) 0.163(5) Uani 0.75 1 d PDU . . O6 O 0.3152(6) 0.8597(8) 0.6986(2) 0.176(6) Uani 0.75 1 d PDU . . O7 O 0.3565(10) 0.9240(4) 0.7296(2) 0.179(6) Uani 0.75 1 d PDU . . C1 C 0.2633(7) 0.1256(5) 0.7084(2) 0.084(2) Uani 1 1 d DU . . C2 C 0.3132(7) 0.1545(6) 0.7269(2) 0.085(2) Uani 1 1 d DU . . C3 C 0.3382(7) 0.1398(6) 0.7520(3) 0.090(2) Uani 1 1 d U . . H3A H 0.3220 0.1080 0.7615 0.108 Uiso 1 1 calc R . . C4 C 0.3966(7) 0.1870(5) 0.7596(2) 0.085(2) Uani 1 1 d U . . H4 H 0.4262 0.1878 0.7734 0.102 Uiso 1 1 calc R . . C5 C 0.3922(7) 0.2292(6) 0.7396(2) 0.084(2) Uani 1 1 d U . . H5 H 0.4190 0.2643 0.7382 0.101 Uiso 1 1 calc R . . C6 C 0.3418(7) 0.2087(6) 0.7229(2) 0.084(2) Uani 1 1 d U . . H6 H 0.3284 0.2317 0.7095 0.101 Uiso 1 1 calc R . . C7 C 0.4615(7) 0.1732(6) 0.6682(2) 0.094(3) Uani 1 1 d DU . . C8 C 0.4717(8) 0.1339(6) 0.6913(2) 0.093(2) Uani 1 1 d DU . . C9 C 0.5177(8) 0.1488(7) 0.7073(3) 0.099(2) Uani 1 1 d U . . H9 H 0.5441 0.1842 0.7062 0.119 Uiso 1 1 calc R . . C10 C 0.5260(8) 0.1106(6) 0.7260(3) 0.094(3) Uani 1 1 d U . . H10 H 0.5583 0.1155 0.7389 0.112 Uiso 1 1 calc R . . C11 C 0.4771(7) 0.0610(6) 0.7231(3) 0.094(3) Uani 1 1 d U . . H11 H 0.4744 0.0272 0.7330 0.113 Uiso 1 1 calc R . . C12 C 0.4347(8) 0.0728(7) 0.7028(3) 0.099(3) Uani 1 1 d U . . H12 H 0.3949 0.0514 0.6970 0.119 Uiso 1 1 calc R . . C13 C 0.1633(5) 0.0468(4) 0.67728(15) 0.053(2) Uani 1 1 d . . . H13 H 0.1916 0.0738 0.6685 0.063 Uiso 1 1 calc R . . C14 C 0.1683(5) 0.0474(4) 0.70430(15) 0.050(2) Uani 1 1 d . . . C15 C 0.1211(5) 0.0083(4) 0.71787(16) 0.057(2) Uani 1 1 d . . . H15 H 0.1212 0.0077 0.7348 0.068 Uiso 1 1 calc R . . C16 C 0.0736(5) -0.0301(4) 0.70387(17) 0.060(2) Uani 1 1 d . . . H16 H 0.0424 -0.0562 0.7119 0.072 Uiso 1 1 calc R . . C17 C 0.0740(5) -0.0284(4) 0.67849(18) 0.058(2) Uani 1 1 d . . . H17 H 0.0421 -0.0534 0.6702 0.070 Uiso 1 1 calc R . . C18 C 0.2827(5) 0.2072(4) 0.63698(16) 0.054(2) Uani 1 1 d . . . H18 H 0.2583 0.1793 0.6465 0.065 Uiso 1 1 calc R . . C19 C 0.3608(5) 0.2101(5) 0.63835(17) 0.060(2) Uani 1 1 d D . . C20 C 0.3973(5) 0.2462(4) 0.62099(19) 0.064(3) Uani 1 1 d . . . H20 H 0.4477 0.2459 0.6201 0.077 Uiso 1 1 calc R . . C21 C 0.3560(6) 0.2825(5) 0.6051(2) 0.080(3) Uani 1 1 d . . . H21 H 0.3784 0.3073 0.5938 0.096 Uiso 1 1 calc R . . C22 C 0.2797(6) 0.2802(5) 0.6069(2) 0.077(3) Uani 1 1 d . . . H22 H 0.2527 0.3052 0.5969 0.093 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 0.0488(9) 0.0602(9) 0.0713(10) 0.0067(6) -0.0197(7) 0.0004(6) Ni1 0.0448(10) 0.0589(10) 0.0450(9) 0.000 0.0029(6) 0.000 Cl1 0.050(2) 0.053(2) 0.046(2) 0.000 0.000 0.000 Cl2 0.151(6) 0.126(5) 0.052(3) 0.000 0.000 -0.104(5) Cl3 0.238(10) 0.167(7) 0.053(3) 0.000 0.000 -0.094(7) N1 0.072(5) 0.071(4) 0.065(4) -0.002(4) -0.019(4) 0.005(4) N2 0.039(4) 0.058(4) 0.050(4) 0.008(3) 0.006(3) -0.008(3) N3 0.068(5) 0.086(5) 0.081(5) 0.022(4) -0.001(4) 0.012(4) N4 0.052(5) 0.061(4) 0.061(5) 0.015(4) -0.004(3) -0.007(4) O1 0.110(7) 0.130(6) 0.087(5) 0.015(5) -0.027(5) -0.022(5) O2 0.087(6) 0.136(6) 0.118(6) 0.023(6) -0.003(5) -0.015(5) O3 0.063(6) 0.067(5) 0.084(7) 0.000 0.015(5) 0.000 O4 0.198(12) 0.145(10) 0.110(9) -0.027(8) -0.015(9) -0.067(9) O5 0.201(13) 0.154(10) 0.134(10) -0.021(9) 0.007(10) -0.072(10) O6 0.248(15) 0.194(12) 0.085(8) -0.036(8) 0.009(9) -0.070(11) O7 0.262(15) 0.191(12) 0.083(8) -0.035(9) 0.039(9) -0.067(11) C1 0.085(5) 0.088(5) 0.079(5) 0.006(4) -0.007(4) 0.006(4) C2 0.083(4) 0.088(4) 0.084(4) -0.001(4) -0.007(4) 0.008(4) C3 0.091(5) 0.087(5) 0.093(5) 0.006(4) 0.004(4) 0.005(4) C4 0.084(5) 0.093(5) 0.077(5) 0.003(4) -0.004(4) 0.014(4) C5 0.084(5) 0.083(5) 0.085(5) -0.004(4) -0.005(4) 0.003(4) C6 0.086(5) 0.086(5) 0.080(4) -0.002(4) -0.010(4) 0.014(4) C7 0.079(5) 0.105(5) 0.099(5) 0.017(5) 0.002(5) 0.010(5) C8 0.081(5) 0.101(5) 0.098(5) 0.015(4) -0.001(4) 0.024(4) C9 0.089(5) 0.107(5) 0.102(5) 0.010(4) 0.008(4) 0.013(4) C10 0.080(5) 0.108(5) 0.093(5) 0.004(5) -0.004(5) 0.018(5) C11 0.081(5) 0.103(5) 0.098(5) 0.012(5) 0.003(4) 0.020(4) C12 0.081(5) 0.110(5) 0.106(5) 0.003(5) -0.004(5) 0.028(5) C13 0.048(5) 0.069(5) 0.042(5) 0.008(4) 0.009(4) -0.011(4) C14 0.053(5) 0.051(5) 0.047(5) 0.009(4) -0.005(4) -0.002(4) C15 0.071(6) 0.056(5) 0.044(5) 0.007(4) 0.014(4) 0.004(4) C16 0.067(6) 0.057(5) 0.057(6) 0.000(4) 0.015(4) -0.004(5) C17 0.059(6) 0.048(5) 0.067(6) 0.002(4) 0.008(4) -0.021(4) C18 0.046(5) 0.072(6) 0.044(4) 0.014(4) -0.002(4) -0.008(4) C19 0.045(5) 0.083(6) 0.054(5) 0.009(5) 0.004(4) -0.008(5) C20 0.039(5) 0.075(6) 0.079(7) 0.016(5) 0.007(4) -0.007(4) C21 0.058(6) 0.105(8) 0.075(7) 0.049(6) -0.015(5) -0.038(6) C22 0.064(7) 0.086(7) 0.081(7) 0.034(6) -0.019(5) -0.013(5) _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 C2 1.972(13) . ? Fe1 C3 2.042(14) . ? Fe1 C6 2.053(12) . ? Fe1 C12 2.062(14) . ? Fe1 C4 2.098(13) . ? Fe1 C10 2.100(14) . ? Fe1 C9 2.105(15) . ? Fe1 C5 2.106(13) . ? Fe1 C11 2.131(13) . ? Fe1 C8 2.171(14) . ? Ni1 N2 2.172(7) . ? Ni1 N2 2.172(7) 11_455 ? Ni1 N4 2.200(8) 8_545 ? Ni1 N4 2.200(8) 14_445 ? Ni1 O3 2.203(10) . ? Ni1 Cl1 2.615(3) . ? Cl1 Ni1 2.615(3) 14_445 ? Cl2 O4 1.397(9) . ? Cl2 O4 1.397(9) 2 ? Cl2 O5 1.433(10) 2 ? Cl2 O5 1.433(10) . ? Cl3 O7 1.411(9) . ? Cl3 O7 1.411(9) 2_565 ? Cl3 O6 1.448(9) . ? Cl3 O6 1.448(9) 2_565 ? N1 C1 1.279(12) . ? N1 C14 1.427(12) . ? N1 H1 0.8600 . ? N2 C13 1.367(11) . ? N2 C17 1.397(10) . ? N3 C7 1.340(13) . ? N3 C19 1.466(11) . ? N3 H3 0.8600 . ? N4 C22 1.336(13) . ? N4 C18 1.357(11) . ? N4 Ni1 2.200(8) 14_445 ? O1 C1 1.246(12) . ? O2 C7 1.284(12) . ? O3 H2 0.8477 . ? C1 C2 1.513(14) . ? C2 C6 1.337(18) . ? C2 C3 1.489(18) . ? C3 C4 1.564(19) . ? C3 H3A 0.9300 . ? C4 C5 1.445(17) . ? C4 H4 0.9300 . ? C5 C6 1.381(18) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.552(14) . ? C8 C9 1.26(2) . ? C8 C12 1.65(2) . ? C9 C10 1.341(18) . ? C9 H9 0.9300 . ? C10 C11 1.44(2) . ? C10 H10 0.9300 . ? C11 C12 1.386(19) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.483(12) . ? C13 H13 0.9300 . ? C14 C15 1.440(12) . ? C15 C16 1.445(13) . ? C15 H15 0.9300 . ? C16 C17 1.391(14) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.444(13) . ? C18 H18 0.9300 . ? C19 C20 1.416(13) . ? C20 C21 1.412(14) . ? C20 H20 0.9300 . ? C21 C22 1.412(15) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Fe1 C3 43.5(5) . . ? C2 Fe1 C6 38.7(5) . . ? C3 Fe1 C6 65.4(5) . . ? C2 Fe1 C12 103.8(6) . . ? C3 Fe1 C12 120.2(6) . . ? C6 Fe1 C12 125.2(5) . . ? C2 Fe1 C4 74.8(5) . . ? C3 Fe1 C4 44.4(5) . . ? C6 Fe1 C4 67.3(5) . . ? C12 Fe1 C4 158.2(5) . . ? C2 Fe1 C10 167.1(6) . . ? C3 Fe1 C10 133.1(5) . . ? C6 Fe1 C10 153.8(6) . . ? C12 Fe1 C10 66.2(6) . . ? C4 Fe1 C10 111.2(5) . . ? C2 Fe1 C9 148.4(6) . . ? C3 Fe1 C9 167.2(6) . . ? C6 Fe1 C9 120.6(6) . . ? C12 Fe1 C9 67.0(6) . . ? C4 Fe1 C9 125.2(6) . . ? C10 Fe1 C9 37.2(5) . . ? C2 Fe1 C5 69.3(5) . . ? C3 Fe1 C5 68.3(5) . . ? C6 Fe1 C5 38.8(5) . . ? C12 Fe1 C5 160.2(5) . . ? C4 Fe1 C5 40.2(5) . . ? C10 Fe1 C5 122.8(6) . . ? C9 Fe1 C5 108.6(6) . . ? C2 Fe1 C11 127.4(6) . . ? C3 Fe1 C11 113.3(5) . . ? C6 Fe1 C11 162.3(6) . . ? C12 Fe1 C11 38.6(5) . . ? C4 Fe1 C11 125.4(5) . . ? C10 Fe1 C11 39.7(5) . . ? C9 Fe1 C11 64.8(6) . . ? C5 Fe1 C11 158.9(6) . . ? C2 Fe1 C8 117.5(5) . . ? C3 Fe1 C8 158.2(6) . . ? C6 Fe1 C8 106.9(5) . . ? C12 Fe1 C8 45.8(6) . . ? C4 Fe1 C8 154.2(6) . . ? C10 Fe1 C8 62.3(5) . . ? C9 Fe1 C8 34.3(5) . . ? C5 Fe1 C8 119.6(5) . . ? C11 Fe1 C8 67.3(5) . . ? N2 Ni1 N2 179.0(4) . 11_455 ? N2 Ni1 N4 88.9(3) . 8_545 ? N2 Ni1 N4 91.2(3) 11_455 8_545 ? N2 Ni1 N4 91.2(3) . 14_445 ? N2 Ni1 N4 88.9(3) 11_455 14_445 ? N4 Ni1 N4 177.8(4) 8_545 14_445 ? N2 Ni1 O3 90.49(18) . . ? N2 Ni1 O3 90.49(18) 11_455 . ? N4 Ni1 O3 88.92(19) 8_545 . ? N4 Ni1 O3 88.92(19) 14_445 . ? N2 Ni1 Cl1 89.51(18) . . ? N2 Ni1 Cl1 89.51(18) 11_455 . ? N4 Ni1 Cl1 91.08(19) 8_545 . ? N4 Ni1 Cl1 91.08(19) 14_445 . ? O3 Ni1 Cl1 180.000(1) . . ? Ni1 Cl1 Ni1 180.000(1) . 14_445 ? O4 Cl2 O4 114.9(11) . 2 ? O4 Cl2 O5 109.6(7) . 2 ? O4 Cl2 O5 107.3(8) 2 2 ? O4 Cl2 O5 107.3(8) . . ? O4 Cl2 O5 109.6(7) 2 . ? O5 Cl2 O5 108.0(12) 2 . ? O7 Cl3 O7 108.5(11) . 2_565 ? O7 Cl3 O6 110.6(8) . . ? O7 Cl3 O6 110.7(7) 2_565 . ? O7 Cl3 O6 110.7(7) . 2_565 ? O7 Cl3 O6 110.6(8) 2_565 2_565 ? O6 Cl3 O6 105.8(10) . 2_565 ? C1 N1 C14 132.9(9) . . ? C1 N1 H1 113.5 . . ? C14 N1 H1 113.5 . . ? C13 N2 C17 116.5(7) . . ? C13 N2 Ni1 118.9(5) . . ? C17 N2 Ni1 124.6(6) . . ? C7 N3 C19 136.7(10) . . ? C7 N3 H3 111.7 . . ? C19 N3 H3 111.7 . . ? C22 N4 C18 118.6(8) . . ? C22 N4 Ni1 123.2(6) . 14_445 ? C18 N4 Ni1 118.3(6) . 14_445 ? Ni1 O3 H2 127.2 . . ? O1 C1 N1 119.7(11) . . ? O1 C1 C2 122.7(11) . . ? N1 C1 C2 117.5(10) . . ? C6 C2 C3 103.0(11) . . ? C6 C2 C1 121.2(11) . . ? C3 C2 C1 135.5(12) . . ? C6 C2 Fe1 73.9(8) . . ? C3 C2 Fe1 70.8(7) . . ? C1 C2 Fe1 123.0(9) . . ? C2 C3 C4 108.2(11) . . ? C2 C3 Fe1 65.7(7) . . ? C4 C3 Fe1 69.7(7) . . ? C2 C3 H3A 125.9 . . ? C4 C3 H3A 125.9 . . ? Fe1 C3 H3A 130.2 . . ? C5 C4 C3 101.4(10) . . ? C5 C4 Fe1 70.2(7) . . ? C3 C4 Fe1 65.9(7) . . ? C5 C4 H4 129.3 . . ? C3 C4 H4 129.3 . . ? Fe1 C4 H4 126.1 . . ? C6 C5 C4 108.9(11) . . ? C6 C5 Fe1 68.5(7) . . ? C4 C5 Fe1 69.6(7) . . ? C6 C5 H5 125.5 . . ? C4 C5 H5 125.5 . . ? Fe1 C5 H5 127.9 . . ? C2 C6 C5 117.3(12) . . ? C2 C6 Fe1 67.4(8) . . ? C5 C6 Fe1 72.7(7) . . ? C2 C6 H6 121.4 . . ? C5 C6 H6 121.4 . . ? Fe1 C6 H6 131.0 . . ? O2 C7 N3 115.0(10) . . ? O2 C7 C8 125.1(11) . . ? N3 C7 C8 119.9(11) . . ? C9 C8 C7 120.0(13) . . ? C9 C8 C12 103.4(12) . . ? C7 C8 C12 136.6(13) . . ? C9 C8 Fe1 70.0(9) . . ? C7 C8 Fe1 128.2(9) . . ? C12 C8 Fe1 63.6(6) . . ? C8 C9 C10 116.0(15) . . ? C8 C9 Fe1 75.7(10) . . ? C10 C9 Fe1 71.2(9) . . ? C8 C9 H9 122.0 . . ? C10 C9 H9 122.0 . . ? Fe1 C9 H9 122.5 . . ? C9 C10 C11 109.5(14) . . ? C9 C10 Fe1 71.6(8) . . ? C11 C10 Fe1 71.3(8) . . ? C9 C10 H10 125.3 . . ? C11 C10 H10 125.3 . . ? Fe1 C10 H10 123.4 . . ? C12 C11 C10 107.3(13) . . ? C12 C11 Fe1 68.0(8) . . ? C10 C11 Fe1 69.0(8) . . ? C12 C11 H11 126.3 . . ? C10 C11 H11 126.3 . . ? Fe1 C11 H11 128.2 . . ? C11 C12 C8 103.2(13) . . ? C11 C12 Fe1 73.4(9) . . ? C8 C12 Fe1 70.6(8) . . ? C11 C12 H12 128.4 . . ? C8 C12 H12 128.4 . . ? Fe1 C12 H12 119.8 . . ? N2 C13 C14 123.3(7) . . ? N2 C13 H13 118.3 . . ? C14 C13 H13 118.3 . . ? N1 C14 C15 121.6(8) . . ? N1 C14 C13 120.2(8) . . ? C15 C14 C13 118.1(8) . . ? C14 C15 C16 116.9(8) . . ? C14 C15 H15 121.5 . . ? C16 C15 H15 121.5 . . ? C17 C16 C15 120.7(8) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 N2 124.3(8) . . ? C16 C17 H17 117.8 . . ? N2 C17 H17 117.8 . . ? N4 C18 C19 122.0(8) . . ? N4 C18 H18 119.0 . . ? C19 C18 H18 119.0 . . ? C20 C19 C18 117.7(8) . . ? C20 C19 N3 123.4(9) . . ? C18 C19 N3 118.7(8) . . ? C21 C20 C19 118.9(9) . . ? C21 C20 H20 120.6 . . ? C19 C20 H20 120.6 . . ? C22 C21 C20 118.3(8) . . ? C22 C21 H21 120.8 . . ? C20 C21 H21 120.8 . . ? N4 C22 C21 123.9(9) . . ? N4 C22 H22 118.0 . . ? C21 C22 H22 118.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O7 0.86 2.50 3.272(16) 149.8 25_566 N3 H3 O1 0.86 2.44 3.036(15) 127.0 . _diffrn_measured_fraction_theta_max 0.866 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.866 _refine_diff_density_max 1.228 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.128 # Attachment 'complex 3.cif' data_complex_3 _database_code_depnum_ccdc_archive 'CCDC 617811' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H46 Cl2 Co Fe1 N8 O13' _chemical_formula_weight 1160.44 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fddd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' _cell_length_a 17.9062(8) _cell_length_b 21.4295(9) _cell_length_c 53.006(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 20339.7(16) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description octahedron _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9520 _exptl_absorpt_coefficient_mu 1.061 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6763 _exptl_absorpt_correction_T_max 0.7210 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _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 area-dectector diffractometer' _diffrn_measurement_method '\f and \w-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23061 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0254 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -60 _diffrn_reflns_limit_l_max 59 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4168 _reflns_number_gt 3410 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material SHELXL-97 _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^)+(0.1623P)^2^+227.0368P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4168 _refine_ls_number_parameters 329 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0987 _refine_ls_R_factor_gt 0.0869 _refine_ls_wR_factor_ref 0.2649 _refine_ls_wR_factor_gt 0.2515 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 0.82771(5) 0.64403(4) 0.024417(18) 0.0499(4) Uani 1 1 d . . . Co1 Co 1.1250 0.50544(6) 0.1250 0.0444(4) Uani 1 2 d S . . C1 C 0.9378(4) 0.6589(4) 0.02274(15) 0.0634(19) Uani 1 1 d . . . C2 C 0.9124(5) 0.6389(3) -0.00097(18) 0.078(3) Uani 1 1 d . . . H2 H 0.9287 0.6038 -0.0097 0.094 Uiso 1 1 calc R . . C3 C 0.8556(5) 0.6833(4) -0.00942(15) 0.073(2) Uani 1 1 d . . . H3 H 0.8269 0.6814 -0.0240 0.088 Uiso 1 1 calc R . . C4 C 0.8538(5) 0.7292(3) 0.00925(15) 0.0661(19) Uani 1 1 d . . . H4 H 0.8245 0.7650 0.0089 0.079 Uiso 1 1 calc R . . C5 C 0.9032(5) 0.7130(4) 0.02868(17) 0.071(2) Uani 1 1 d . . . H5 H 0.9110 0.7359 0.0434 0.085 Uiso 1 1 calc R . . C6 C 0.9876(4) 0.6250(4) 0.04119(14) 0.0602(18) Uani 1 1 d . . . C7 C 1.0839(3) 0.5468(3) 0.04570(11) 0.0416(13) Uani 1 1 d . . . C8 C 1.0871(3) 0.5456(3) 0.07178(11) 0.0445(14) Uani 1 1 d . . . H8 H 1.0570 0.5727 0.0809 0.053 Uiso 1 1 calc R . . C9 C 1.1763(4) 0.4680(3) 0.07121(12) 0.0514(16) Uani 1 1 d . . . H9 H 1.2066 0.4401 0.0799 0.062 Uiso 1 1 calc R . . C10 C 1.1781(4) 0.4685(3) 0.04533(12) 0.0521(16) Uani 1 1 d . . . H10 H 1.2109 0.4427 0.0366 0.063 Uiso 1 1 calc R . . C11 C 1.1311(3) 0.5076(3) 0.03249(12) 0.0477(15) Uani 1 1 d . . . H11 H 1.1309 0.5078 0.0149 0.057 Uiso 1 1 calc R . . C12 C 0.8093(5) 0.5788(5) 0.05146(18) 0.082(3) Uani 1 1 d . . . H12 H 0.8471 0.5582 0.0601 0.098 Uiso 1 1 calc R . . C13 C 0.7740(5) 0.5596(4) 0.02834(16) 0.070(2) Uani 1 1 d . . . H13 H 0.7835 0.5234 0.0192 0.084 Uiso 1 1 calc R . . C14 C 0.7223(4) 0.6065(4) 0.02232(16) 0.073(2) Uani 1 1 d . . . H14 H 0.6922 0.6066 0.0080 0.088 Uiso 1 1 calc R . . C15 C 0.7226(5) 0.6516(4) 0.04016(18) 0.080(2) Uani 1 1 d . . . H15 H 0.6925 0.6870 0.0400 0.096 Uiso 1 1 calc R . . C16 C 0.7733(5) 0.6375(4) 0.05850(17) 0.074(2) Uani 1 1 d . . . C17 C 0.7889(5) 0.6757(4) 0.08145(18) 0.080(2) Uani 1 1 d . . . C18 C 0.8874(3) 0.7085(3) 0.11116(12) 0.0479(15) Uani 1 1 d . . . C19 C 0.9647(3) 0.7092(3) 0.11238(11) 0.0478(14) Uani 1 1 d . . . H19 H 0.9909 0.6828 0.1016 0.057 Uiso 1 1 calc R . . C20 C 0.9658(4) 0.7813(3) 0.14386(12) 0.0571(17) Uani 1 1 d . . . H20 H 0.9918 0.8076 0.1547 0.069 Uiso 1 1 calc R . . C21 C 0.8885(4) 0.7809(4) 0.14460(15) 0.071(2) Uani 1 1 d . . . H21 H 0.8634 0.8055 0.1563 0.085 Uiso 1 1 calc R . . C22 C 0.8494(4) 0.7448(4) 0.12828(13) 0.0629(19) Uani 1 1 d . . . H22 H 0.7975 0.7446 0.1287 0.075 Uiso 1 1 calc R . . C23 C 0.0702(15) 0.2978(12) 0.0788(5) 0.235(11) Uiso 1 1 d . . . H23A H 0.0660 0.2531 0.0788 0.352 Uiso 1 1 calc R . . H23B H 0.0632 0.3134 0.0620 0.352 Uiso 1 1 calc R . . H23C H 0.0328 0.3152 0.0897 0.352 Uiso 1 1 calc R . . Cl1 Cl 1.1250 0.6250 0.1250 0.0454(7) Uani 1 4 d S . . Cl2 Cl 0.1250 0.6250 0.96510(7) 0.107(2) Uani 0.75 2 d SP . . Cl3 Cl 0.8750 0.8750 0.05970(9) 0.122(2) Uani 0.75 2 d SP . . N1 N 1.0342(3) 0.5858(2) 0.03241(10) 0.0490(13) Uani 1 1 d . . . H1A H 1.0356 0.5828 0.0162 0.059 Uiso 1 1 calc R . . N2 N 1.1322(3) 0.5066(2) 0.08428(9) 0.0464(12) Uani 1 1 d . . . N3 N 0.8529(3) 0.6713(3) 0.09256(11) 0.0565(14) Uani 1 1 d . . . H3A H 0.8793 0.6402 0.0875 0.068 Uiso 1 1 d R . . N4 N 1.0039(3) 0.7451(2) 0.12801(9) 0.0473(12) Uani 1 1 d . . . O1 O 0.9819(3) 0.6356(3) 0.06391(11) 0.088(2) Uani 1 1 d . . . O2 O 0.7412(4) 0.7140(5) 0.08907(16) 0.137(3) Uani 1 1 d . . . O3 O 1.1250 0.4063(3) 0.1250 0.071(2) Uani 1 2 d S . . H3B H 1.1240 0.3935 0.1104 0.107 Uiso 1 1 calc R . . O4 O 0.1804(9) 0.6105(9) 0.9478(2) 0.177(7) Uani 0.75 1 d P . . O5 O 0.1027(17) 0.5774(9) 0.9793(3) 0.292(16) Uani 0.75 1 d P . . O6 O 0.8982(8) 0.8248(6) 0.0734(2) 0.143(5) Uani 0.75 1 d P . . O7 O 0.8174(19) 0.8579(14) 0.0460(6) 0.48(3) Uani 0.75 1 d P . . O8 O 0.1465(14) 0.3161(10) 0.0882(5) 0.300(10) Uiso 1 1 d . . . H8A H 0.1524 0.3031 0.1026 0.450 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 0.0384(6) 0.0541(6) 0.0573(7) -0.0018(4) -0.0159(4) -0.0011(4) Co1 0.0390(7) 0.0622(7) 0.0320(7) 0.000 0.0004(5) 0.000 C1 0.036(4) 0.078(5) 0.076(5) 0.002(4) -0.010(3) -0.002(3) C2 0.084(6) 0.053(4) 0.097(7) -0.004(4) 0.045(5) 0.002(4) C3 0.067(5) 0.098(6) 0.055(5) 0.013(4) -0.019(4) -0.017(4) C4 0.066(5) 0.056(4) 0.077(5) 0.013(4) -0.010(4) 0.006(3) C5 0.064(5) 0.064(4) 0.083(6) 0.002(4) -0.024(4) -0.014(4) C6 0.045(4) 0.086(5) 0.050(4) -0.011(3) -0.001(3) 0.001(4) C7 0.043(3) 0.047(3) 0.035(3) -0.004(2) 0.003(2) -0.003(3) C8 0.041(3) 0.058(3) 0.035(3) -0.005(3) 0.002(3) 0.010(3) C9 0.047(4) 0.058(4) 0.049(4) -0.003(3) -0.003(3) 0.016(3) C10 0.052(4) 0.060(4) 0.044(4) -0.007(3) 0.009(3) 0.011(3) C11 0.053(4) 0.058(3) 0.033(3) -0.007(3) 0.004(3) 0.002(3) C12 0.050(4) 0.101(6) 0.093(6) 0.042(5) -0.012(4) -0.019(4) C13 0.067(5) 0.068(4) 0.075(5) -0.020(4) 0.017(4) -0.019(4) C14 0.040(4) 0.109(7) 0.071(5) -0.008(5) -0.003(3) -0.012(4) C15 0.063(5) 0.092(6) 0.086(6) -0.010(5) 0.009(5) 0.003(4) C16 0.065(5) 0.078(5) 0.080(6) -0.024(4) 0.004(4) -0.019(4) C17 0.053(5) 0.102(6) 0.086(6) -0.020(5) 0.012(4) 0.009(4) C18 0.037(3) 0.061(4) 0.046(4) -0.005(3) 0.000(3) 0.009(3) C19 0.038(3) 0.066(4) 0.040(3) -0.011(3) 0.003(3) 0.007(3) C20 0.051(4) 0.070(4) 0.050(4) -0.018(3) -0.002(3) 0.007(3) C21 0.057(5) 0.093(5) 0.064(5) -0.032(4) 0.011(4) 0.017(4) C22 0.042(4) 0.090(5) 0.056(4) -0.018(4) 0.005(3) 0.009(4) Cl1 0.0451(17) 0.0532(15) 0.0378(15) 0.000 0.000 0.000 Cl2 0.151(5) 0.136(4) 0.0343(19) 0.000 0.000 0.087(4) Cl3 0.162(6) 0.133(4) 0.071(3) 0.000 0.000 0.103(4) N1 0.051(3) 0.060(3) 0.036(3) -0.003(2) -0.009(2) 0.010(3) N2 0.039(3) 0.065(3) 0.035(3) -0.002(2) 0.000(2) 0.010(2) N3 0.041(3) 0.075(3) 0.054(3) -0.013(3) -0.008(3) 0.005(3) N4 0.041(3) 0.064(3) 0.037(3) -0.008(2) 0.001(2) 0.006(2) O1 0.081(4) 0.125(5) 0.059(3) -0.030(3) -0.022(3) 0.047(4) O2 0.070(4) 0.192(8) 0.149(7) -0.086(7) -0.022(5) 0.046(5) O3 0.085(6) 0.069(4) 0.060(4) 0.000 0.000(4) 0.000 O4 0.176(14) 0.255(18) 0.100(8) -0.077(10) 0.018(8) 0.038(12) O5 0.54(4) 0.233(17) 0.103(10) 0.095(11) 0.130(16) 0.22(2) O6 0.142(10) 0.151(10) 0.136(10) 0.068(8) 0.002(8) 0.056(8) O7 0.55(5) 0.36(3) 0.53(4) -0.35(3) -0.46(4) 0.37(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 C1 1.999(7) . ? Fe1 C5 2.016(7) . ? Fe1 C12 2.029(8) . ? Fe1 C2 2.031(8) . ? Fe1 C4 2.049(7) . ? Fe1 C3 2.043(8) . ? Fe1 C16 2.057(9) . ? Fe1 C13 2.060(7) . ? Fe1 C14 2.054(8) . ? Fe1 C15 2.066(9) . ? Co1 O3 2.125(7) . ? Co1 N2 2.162(5) 11_654 ? Co1 N2 2.162(5) . ? Co1 N4 2.175(5) 8_554 ? Co1 N4 2.175(5) 14_655 ? Co1 Cl1 2.5621(12) . ? C1 C5 1.352(11) . ? C1 C2 1.404(12) . ? C1 C6 1.510(11) . ? C2 C3 1.464(12) . ? C2 H2 0.9300 . ? C3 C4 1.396(11) . ? C3 H3 0.9300 . ? C4 C5 1.401(11) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 O1 1.230(9) . ? C6 N1 1.271(9) . ? C7 C8 1.384(8) . ? C7 C11 1.382(8) . ? C7 N1 1.410(8) . ? C8 N2 1.337(8) . ? C8 H8 0.9300 . ? C9 N2 1.336(8) . ? C9 C10 1.372(9) . ? C9 H9 0.9300 . ? C10 C11 1.369(9) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C16 1.462(13) . ? C12 C13 1.439(12) . ? C12 H12 0.9300 . ? C13 C14 1.404(12) . ? C13 H13 0.9300 . ? C14 C15 1.351(12) . ? C14 H14 0.9300 . ? C15 C16 1.364(13) . ? C15 H15 0.9300 . ? C16 C17 1.493(12) . ? C17 O2 1.252(10) . ? C17 N3 1.292(10) . ? C18 C19 1.387(9) . ? C18 C22 1.374(9) . ? C18 N3 1.410(8) . ? C19 N4 1.331(8) . ? C19 H19 0.9300 . ? C20 N4 1.331(8) . ? C20 C21 1.385(11) . ? C20 H20 0.9300 . ? C21 C22 1.355(11) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 O8 1.51(3) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? Cl1 Co1 2.5621(12) 14_655 ? Cl2 O5 1.327(18) 14_455 ? Cl2 O5 1.327(18) . ? Cl2 O4 1.387(13) . ? Cl2 O4 1.387(13) 14_455 ? Cl3 O7 1.31(2) . ? Cl3 O7 1.31(2) 2_665 ? Cl3 O6 1.364(10) 2_665 ? Cl3 O6 1.364(10) . ? N1 H1A 0.8600 . ? N3 H3A 0.8605 . ? N4 Co1 2.175(5) 14_655 ? O3 H3B 0.8200 . ? O8 H8A 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe1 C5 39.4(3) . . ? C1 Fe1 C12 107.6(3) . . ? C5 Fe1 C12 122.4(4) . . ? C1 Fe1 C2 40.8(4) . . ? C5 Fe1 C2 67.3(4) . . ? C12 Fe1 C2 123.5(4) . . ? C1 Fe1 C4 67.4(3) . . ? C5 Fe1 C4 40.3(3) . . ? C12 Fe1 C4 158.1(4) . . ? C2 Fe1 C4 67.5(3) . . ? C1 Fe1 C3 69.8(3) . . ? C5 Fe1 C3 68.4(3) . . ? C12 Fe1 C3 160.7(4) . . ? C2 Fe1 C3 42.1(4) . . ? C4 Fe1 C3 39.9(3) . . ? C1 Fe1 C16 121.1(3) . . ? C5 Fe1 C16 105.6(3) . . ? C12 Fe1 C16 41.9(4) . . ? C2 Fe1 C16 158.7(4) . . ? C4 Fe1 C16 120.9(3) . . ? C3 Fe1 C16 156.1(4) . . ? C1 Fe1 C13 127.2(3) . . ? C5 Fe1 C13 161.1(4) . . ? C12 Fe1 C13 41.2(4) . . ? C2 Fe1 C13 111.6(3) . . ? C4 Fe1 C13 158.3(3) . . ? C3 Fe1 C13 124.4(3) . . ? C16 Fe1 C13 68.3(3) . . ? C1 Fe1 C14 165.0(4) . . ? C5 Fe1 C14 155.4(4) . . ? C12 Fe1 C14 67.6(3) . . ? C2 Fe1 C14 129.0(4) . . ? C4 Fe1 C14 122.5(3) . . ? C3 Fe1 C14 109.8(3) . . ? C16 Fe1 C14 65.5(3) . . ? C13 Fe1 C14 39.9(3) . . ? C1 Fe1 C15 154.7(4) . . ? C5 Fe1 C15 120.6(4) . . ? C12 Fe1 C15 67.7(4) . . ? C2 Fe1 C15 162.3(4) . . ? C4 Fe1 C15 107.3(4) . . ? C3 Fe1 C15 123.0(4) . . ? C16 Fe1 C15 38.6(4) . . ? C13 Fe1 C15 66.6(4) . . ? C14 Fe1 C15 38.3(3) . . ? O3 Co1 N2 90.64(14) . 11_654 ? O3 Co1 N2 90.64(14) . . ? N2 Co1 N2 178.7(3) 11_654 . ? O3 Co1 N4 89.68(14) . 8_554 ? N2 Co1 N4 90.80(18) 11_654 8_554 ? N2 Co1 N4 89.20(18) . 8_554 ? O3 Co1 N4 89.68(14) . 14_655 ? N2 Co1 N4 89.20(18) 11_654 14_655 ? N2 Co1 N4 90.80(18) . 14_655 ? N4 Co1 N4 179.4(3) 8_554 14_655 ? O3 Co1 Cl1 180.000(1) . . ? N2 Co1 Cl1 89.36(14) 11_654 . ? N2 Co1 Cl1 89.36(14) . . ? N4 Co1 Cl1 90.32(14) 8_554 . ? N4 Co1 Cl1 90.32(14) 14_655 . ? C5 C1 C2 108.8(7) . . ? C5 C1 C6 122.2(7) . . ? C2 C1 C6 128.6(7) . . ? C5 C1 Fe1 71.0(4) . . ? C2 C1 Fe1 70.8(4) . . ? C6 C1 Fe1 118.5(5) . . ? C1 C2 C3 107.5(7) . . ? C1 C2 Fe1 68.4(4) . . ? C3 C2 Fe1 69.4(5) . . ? C1 C2 H2 126.3 . . ? C3 C2 H2 126.3 . . ? Fe1 C2 H2 127.5 . . ? C4 C3 C2 104.9(7) . . ? C4 C3 Fe1 70.3(5) . . ? C2 C3 Fe1 68.5(4) . . ? C4 C3 H3 127.5 . . ? C2 C3 H3 127.5 . . ? Fe1 C3 H3 125.3 . . ? C5 C4 C3 109.4(7) . . ? C5 C4 Fe1 68.6(4) . . ? C3 C4 Fe1 69.8(4) . . ? C5 C4 H4 125.3 . . ? C3 C4 H4 125.3 . . ? Fe1 C4 H4 127.9 . . ? C1 C5 C4 109.3(7) . . ? C1 C5 Fe1 69.6(4) . . ? C4 C5 Fe1 71.1(4) . . ? C1 C5 H5 125.4 . . ? C4 C5 H5 125.4 . . ? Fe1 C5 H5 125.5 . . ? O1 C6 N1 122.3(7) . . ? O1 C6 C1 119.8(7) . . ? N1 C6 C1 117.9(6) . . ? C8 C7 C11 118.0(6) . . ? C8 C7 N1 122.4(5) . . ? C11 C7 N1 119.6(5) . . ? N2 C8 C7 122.1(5) . . ? N2 C8 H8 118.9 . . ? C7 C8 H8 118.9 . . ? N2 C9 C10 121.8(6) . . ? N2 C9 H9 119.1 . . ? C10 C9 H9 119.1 . . ? C9 C10 C11 119.2(6) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C10 C11 C7 119.7(6) . . ? C10 C11 H11 120.1 . . ? C7 C11 H11 120.1 . . ? C16 C12 C13 105.7(7) . . ? C16 C12 Fe1 70.1(5) . . ? C13 C12 Fe1 70.6(5) . . ? C16 C12 H12 127.1 . . ? C13 C12 H12 127.1 . . ? Fe1 C12 H12 123.9 . . ? C14 C13 C12 106.1(7) . . ? C14 C13 Fe1 69.8(5) . . ? C12 C13 Fe1 68.2(4) . . ? C14 C13 H13 127.0 . . ? C12 C13 H13 127.0 . . ? Fe1 C13 H13 126.5 . . ? C15 C14 C13 110.6(8) . . ? C15 C14 Fe1 71.3(5) . . ? C13 C14 Fe1 70.3(4) . . ? C15 C14 H14 124.7 . . ? C13 C14 H14 124.7 . . ? Fe1 C14 H14 125.2 . . ? C14 C15 C16 110.1(8) . . ? C14 C15 Fe1 70.4(5) . . ? C16 C15 Fe1 70.3(5) . . ? C14 C15 H15 125.0 . . ? C16 C15 H15 125.0 . . ? Fe1 C15 H15 125.9 . . ? C15 C16 C12 107.5(7) . . ? C15 C16 C17 125.8(8) . . ? C12 C16 C17 126.7(9) . . ? C15 C16 Fe1 71.0(5) . . ? C12 C16 Fe1 68.0(5) . . ? C17 C16 Fe1 126.2(6) . . ? O2 C17 N3 120.4(8) . . ? O2 C17 C16 119.6(8) . . ? N3 C17 C16 119.9(7) . . ? C19 C18 C22 117.2(6) . . ? C19 C18 N3 118.4(5) . . ? C22 C18 N3 124.4(6) . . ? N4 C19 C18 124.1(5) . . ? N4 C19 H19 117.9 . . ? C18 C19 H19 117.9 . . ? N4 C20 C21 121.7(6) . . ? N4 C20 H20 119.2 . . ? C21 C20 H20 119.2 . . ? C22 C21 C20 120.1(6) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C18 119.3(7) . . ? C21 C22 H22 120.4 . . ? C18 C22 H22 120.4 . . ? O8 C23 H23A 109.5 . . ? O8 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O8 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Co1 Cl1 Co1 180.0 14_655 . ? O5 Cl2 O5 111(2) 14_455 . ? O5 Cl2 O4 109.4(15) 14_455 . ? O5 Cl2 O4 114.6(11) . . ? O5 Cl2 O4 114.6(11) 14_455 14_455 ? O5 Cl2 O4 109.4(15) . 14_455 ? O4 Cl2 O4 97.1(13) . 14_455 ? O7 Cl3 O7 113(4) . 2_665 ? O7 Cl3 O6 106.1(10) . 2_665 ? O7 Cl3 O6 108.3(17) 2_665 2_665 ? O7 Cl3 O6 108.3(17) . . ? O7 Cl3 O6 106.1(10) 2_665 . ? O6 Cl3 O6 115.4(13) 2_665 . ? C6 N1 C7 128.5(6) . . ? C6 N1 H1A 115.7 . . ? C7 N1 H1A 115.7 . . ? C8 N2 C9 119.1(5) . . ? C8 N2 Co1 117.8(4) . . ? C9 N2 Co1 123.1(4) . . ? C17 N3 C18 131.7(6) . . ? C17 N3 H3A 113.8 . . ? C18 N3 H3A 114.5 . . ? C20 N4 C19 117.5(6) . . ? C20 N4 Co1 124.0(4) . 14_655 ? C19 N4 Co1 118.4(4) . 14_655 ? Co1 O3 H3B 109.5 . . ? C23 O8 H8A 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 Fe1 C1 C5 -120.0(6) . . . . ? C2 Fe1 C1 C5 118.7(7) . . . . ? C4 Fe1 C1 C5 37.4(5) . . . . ? C3 Fe1 C1 C5 80.3(6) . . . . ? C16 Fe1 C1 C5 -76.1(6) . . . . ? C13 Fe1 C1 C5 -161.3(5) . . . . ? C14 Fe1 C1 C5 171.3(12) . . . . ? C15 Fe1 C1 C5 -45.2(11) . . . . ? C5 Fe1 C1 C2 -118.7(7) . . . . ? C12 Fe1 C1 C2 121.3(5) . . . . ? C4 Fe1 C1 C2 -81.4(5) . . . . ? C3 Fe1 C1 C2 -38.4(5) . . . . ? C16 Fe1 C1 C2 165.2(5) . . . . ? C13 Fe1 C1 C2 80.0(6) . . . . ? C14 Fe1 C1 C2 52.6(15) . . . . ? C15 Fe1 C1 C2 -163.9(8) . . . . ? C5 Fe1 C1 C6 117.1(8) . . . . ? C12 Fe1 C1 C6 -2.9(7) . . . . ? C2 Fe1 C1 C6 -124.2(8) . . . . ? C4 Fe1 C1 C6 154.4(7) . . . . ? C3 Fe1 C1 C6 -162.6(7) . . . . ? C16 Fe1 C1 C6 41.0(8) . . . . ? C13 Fe1 C1 C6 -44.2(8) . . . . ? C14 Fe1 C1 C6 -71.6(15) . . . . ? C15 Fe1 C1 C6 71.8(11) . . . . ? C5 C1 C2 C3 -2.6(9) . . . . ? C6 C1 C2 C3 170.2(7) . . . . ? Fe1 C1 C2 C3 58.6(6) . . . . ? C5 C1 C2 Fe1 -61.2(6) . . . . ? C6 C1 C2 Fe1 111.6(8) . . . . ? C5 Fe1 C2 C1 37.1(5) . . . . ? C12 Fe1 C2 C1 -77.6(6) . . . . ? C4 Fe1 C2 C1 80.9(5) . . . . ? C3 Fe1 C2 C1 119.6(7) . . . . ? C16 Fe1 C2 C1 -37.1(10) . . . . ? C13 Fe1 C2 C1 -122.5(5) . . . . ? C14 Fe1 C2 C1 -164.7(5) . . . . ? C15 Fe1 C2 C1 157.1(11) . . . . ? C1 Fe1 C2 C3 -119.6(7) . . . . ? C5 Fe1 C2 C3 -82.5(5) . . . . ? C12 Fe1 C2 C3 162.8(5) . . . . ? C4 Fe1 C2 C3 -38.7(4) . . . . ? C16 Fe1 C2 C3 -156.6(8) . . . . ? C13 Fe1 C2 C3 117.9(5) . . . . ? C14 Fe1 C2 C3 75.7(6) . . . . ? C15 Fe1 C2 C3 37.6(13) . . . . ? C1 C2 C3 C4 3.3(9) . . . . ? Fe1 C2 C3 C4 61.3(6) . . . . ? C1 C2 C3 Fe1 -57.9(5) . . . . ? C1 Fe1 C3 C4 -78.5(5) . . . . ? C5 Fe1 C3 C4 -36.3(5) . . . . ? C12 Fe1 C3 C4 -164.0(9) . . . . ? C2 Fe1 C3 C4 -115.8(7) . . . . ? C16 Fe1 C3 C4 43.4(10) . . . . ? C13 Fe1 C3 C4 159.5(5) . . . . ? C14 Fe1 C3 C4 117.4(5) . . . . ? C15 Fe1 C3 C4 77.0(6) . . . . ? C1 Fe1 C3 C2 37.3(5) . . . . ? C5 Fe1 C3 C2 79.5(5) . . . . ? C12 Fe1 C3 C2 -48.2(11) . . . . ? C4 Fe1 C3 C2 115.8(7) . . . . ? C16 Fe1 C3 C2 159.2(7) . . . . ? C13 Fe1 C3 C2 -84.7(6) . . . . ? C14 Fe1 C3 C2 -126.8(5) . . . . ? C15 Fe1 C3 C2 -167.2(5) . . . . ? C2 C3 C4 C5 -2.9(9) . . . . ? Fe1 C3 C4 C5 57.2(6) . . . . ? C2 C3 C4 Fe1 -60.1(5) . . . . ? C1 Fe1 C4 C5 -36.5(5) . . . . ? C12 Fe1 C4 C5 44.2(11) . . . . ? C2 Fe1 C4 C5 -80.8(6) . . . . ? C3 Fe1 C4 C5 -121.6(8) . . . . ? C16 Fe1 C4 C5 77.3(6) . . . . ? C13 Fe1 C4 C5 -173.0(8) . . . . ? C14 Fe1 C4 C5 156.2(5) . . . . ? C15 Fe1 C4 C5 117.2(6) . . . . ? C1 Fe1 C4 C3 85.1(5) . . . . ? C5 Fe1 C4 C3 121.6(8) . . . . ? C12 Fe1 C4 C3 165.8(8) . . . . ? C2 Fe1 C4 C3 40.8(5) . . . . ? C16 Fe1 C4 C3 -161.1(5) . . . . ? C13 Fe1 C4 C3 -51.3(11) . . . . ? C14 Fe1 C4 C3 -82.1(6) . . . . ? C15 Fe1 C4 C3 -121.2(5) . . . . ? C2 C1 C5 C4 0.8(10) . . . . ? C6 C1 C5 C4 -172.5(7) . . . . ? Fe1 C1 C5 C4 -60.3(6) . . . . ? C2 C1 C5 Fe1 61.1(6) . . . . ? C6 C1 C5 Fe1 -112.3(7) . . . . ? C3 C4 C5 C1 1.4(10) . . . . ? Fe1 C4 C5 C1 59.4(6) . . . . ? C3 C4 C5 Fe1 -57.9(6) . . . . ? C12 Fe1 C5 C1 77.9(6) . . . . ? C2 Fe1 C5 C1 -38.4(5) . . . . ? C4 Fe1 C5 C1 -120.0(8) . . . . ? C3 Fe1 C5 C1 -84.0(6) . . . . ? C16 Fe1 C5 C1 120.4(5) . . . . ? C13 Fe1 C5 C1 52.0(13) . . . . ? C14 Fe1 C5 C1 -174.6(7) . . . . ? C15 Fe1 C5 C1 159.4(5) . . . . ? C1 Fe1 C5 C4 120.0(8) . . . . ? C12 Fe1 C5 C4 -162.1(5) . . . . ? C2 Fe1 C5 C4 81.6(6) . . . . ? C3 Fe1 C5 C4 36.0(5) . . . . ? C16 Fe1 C5 C4 -119.6(6) . . . . ? C13 Fe1 C5 C4 172.0(9) . . . . ? C14 Fe1 C5 C4 -54.6(11) . . . . ? C15 Fe1 C5 C4 -80.6(6) . . . . ? C5 C1 C6 O1 20.3(12) . . . . ? C2 C1 C6 O1 -151.6(9) . . . . ? Fe1 C1 C6 O1 -64.2(10) . . . . ? C5 C1 C6 N1 -159.9(8) . . . . ? C2 C1 C6 N1 28.2(12) . . . . ? Fe1 C1 C6 N1 115.6(7) . . . . ? C11 C7 C8 N2 -2.3(9) . . . . ? N1 C7 C8 N2 177.1(6) . . . . ? N2 C9 C10 C11 -3.0(10) . . . . ? C9 C10 C11 C7 1.5(10) . . . . ? C8 C7 C11 C10 1.0(9) . . . . ? N1 C7 C11 C10 -178.4(6) . . . . ? C1 Fe1 C12 C16 117.3(5) . . . . ? C5 Fe1 C12 C16 76.7(6) . . . . ? C2 Fe1 C12 C16 159.3(5) . . . . ? C4 Fe1 C12 C16 44.5(11) . . . . ? C3 Fe1 C12 C16 -163.8(9) . . . . ? C13 Fe1 C12 C16 -115.7(7) . . . . ? C14 Fe1 C12 C16 -77.8(5) . . . . ? C15 Fe1 C12 C16 -36.2(5) . . . . ? C1 Fe1 C12 C13 -127.0(5) . . . . ? C5 Fe1 C12 C13 -167.6(5) . . . . ? C2 Fe1 C12 C13 -85.0(6) . . . . ? C4 Fe1 C12 C13 160.2(8) . . . . ? C3 Fe1 C12 C13 -48.1(12) . . . . ? C16 Fe1 C12 C13 115.7(7) . . . . ? C14 Fe1 C12 C13 37.9(5) . . . . ? C15 Fe1 C12 C13 79.4(5) . . . . ? C16 C12 C13 C14 1.8(9) . . . . ? Fe1 C12 C13 C14 -59.9(6) . . . . ? C16 C12 C13 Fe1 61.7(5) . . . . ? C1 Fe1 C13 C14 -169.3(5) . . . . ? C5 Fe1 C13 C14 151.8(10) . . . . ? C12 Fe1 C13 C14 117.7(7) . . . . ? C2 Fe1 C13 C14 -125.6(5) . . . . ? C4 Fe1 C13 C14 -42.3(11) . . . . ? C3 Fe1 C13 C14 -79.7(6) . . . . ? C16 Fe1 C13 C14 77.3(5) . . . . ? C15 Fe1 C13 C14 35.4(5) . . . . ? C1 Fe1 C13 C12 73.0(6) . . . . ? C5 Fe1 C13 C12 34.1(13) . . . . ? C2 Fe1 C13 C12 116.7(6) . . . . ? C4 Fe1 C13 C12 -160.0(9) . . . . ? C3 Fe1 C13 C12 162.6(6) . . . . ? C16 Fe1 C13 C12 -40.4(6) . . . . ? C14 Fe1 C13 C12 -117.7(7) . . . . ? C15 Fe1 C13 C12 -82.3(6) . . . . ? C12 C13 C14 C15 -1.3(9) . . . . ? Fe1 C13 C14 C15 -60.2(6) . . . . ? C12 C13 C14 Fe1 58.9(5) . . . . ? C1 Fe1 C14 C15 155.8(12) . . . . ? C5 Fe1 C14 C15 -37.5(11) . . . . ? C12 Fe1 C14 C15 81.9(6) . . . . ? C2 Fe1 C14 C15 -162.3(6) . . . . ? C4 Fe1 C14 C15 -76.2(7) . . . . ? C3 Fe1 C14 C15 -118.7(6) . . . . ? C16 Fe1 C14 C15 36.0(6) . . . . ? C13 Fe1 C14 C15 121.0(8) . . . . ? C1 Fe1 C14 C13 34.8(15) . . . . ? C5 Fe1 C14 C13 -158.5(8) . . . . ? C12 Fe1 C14 C13 -39.1(5) . . . . ? C2 Fe1 C14 C13 76.7(6) . . . . ? C4 Fe1 C14 C13 162.8(5) . . . . ? C3 Fe1 C14 C13 120.3(5) . . . . ? C16 Fe1 C14 C13 -84.9(5) . . . . ? C15 Fe1 C14 C13 -121.0(8) . . . . ? C13 C14 C15 C16 0.2(10) . . . . ? Fe1 C14 C15 C16 -59.3(7) . . . . ? C13 C14 C15 Fe1 59.5(6) . . . . ? C1 Fe1 C15 C14 -165.6(7) . . . . ? C5 Fe1 C15 C14 162.9(5) . . . . ? C12 Fe1 C15 C14 -81.7(6) . . . . ? C2 Fe1 C15 C14 50.9(14) . . . . ? C4 Fe1 C15 C14 120.9(6) . . . . ? C3 Fe1 C15 C14 80.1(6) . . . . ? C16 Fe1 C15 C14 -120.9(8) . . . . ? C13 Fe1 C15 C14 -36.8(5) . . . . ? C1 Fe1 C15 C16 -44.7(11) . . . . ? C5 Fe1 C15 C16 -76.2(6) . . . . ? C12 Fe1 C15 C16 39.2(5) . . . . ? C2 Fe1 C15 C16 171.8(9) . . . . ? C4 Fe1 C15 C16 -118.1(5) . . . . ? C3 Fe1 C15 C16 -159.0(5) . . . . ? C13 Fe1 C15 C16 84.1(6) . . . . ? C14 Fe1 C15 C16 120.9(8) . . . . ? C14 C15 C16 C12 0.9(10) . . . . ? Fe1 C15 C16 C12 -58.4(6) . . . . ? C14 C15 C16 C17 -179.2(8) . . . . ? Fe1 C15 C16 C17 121.4(9) . . . . ? C14 C15 C16 Fe1 59.3(6) . . . . ? C13 C12 C16 C15 -1.7(9) . . . . ? Fe1 C12 C16 C15 60.3(6) . . . . ? C13 C12 C16 C17 178.5(8) . . . . ? Fe1 C12 C16 C17 -119.5(9) . . . . ? C13 C12 C16 Fe1 -62.0(5) . . . . ? C1 Fe1 C16 C15 159.5(5) . . . . ? C5 Fe1 C16 C15 119.8(5) . . . . ? C12 Fe1 C16 C15 -118.9(7) . . . . ? C2 Fe1 C16 C15 -173.1(8) . . . . ? C4 Fe1 C16 C15 78.8(6) . . . . ? C3 Fe1 C16 C15 48.0(10) . . . . ? C13 Fe1 C16 C15 -79.2(6) . . . . ? C14 Fe1 C16 C15 -35.7(5) . . . . ? C1 Fe1 C16 C12 -81.7(5) . . . . ? C5 Fe1 C16 C12 -121.4(5) . . . . ? C2 Fe1 C16 C12 -54.3(10) . . . . ? C4 Fe1 C16 C12 -162.3(5) . . . . ? C3 Fe1 C16 C12 166.8(7) . . . . ? C13 Fe1 C16 C12 39.7(5) . . . . ? C14 Fe1 C16 C12 83.1(5) . . . . ? C15 Fe1 C16 C12 118.9(7) . . . . ? C1 Fe1 C16 C17 38.5(10) . . . . ? C5 Fe1 C16 C17 -1.2(9) . . . . ? C12 Fe1 C16 C17 120.2(10) . . . . ? C2 Fe1 C16 C17 65.9(13) . . . . ? C4 Fe1 C16 C17 -42.1(10) . . . . ? C3 Fe1 C16 C17 -73.0(12) . . . . ? C13 Fe1 C16 C17 159.9(9) . . . . ? C14 Fe1 C16 C17 -156.7(10) . . . . ? C15 Fe1 C16 C17 -121.0(11) . . . . ? C15 C16 C17 O2 20.9(15) . . . . ? C12 C16 C17 O2 -159.3(10) . . . . ? Fe1 C16 C17 O2 112.6(10) . . . . ? C15 C16 C17 N3 -155.6(9) . . . . ? C12 C16 C17 N3 24.2(14) . . . . ? Fe1 C16 C17 N3 -63.9(12) . . . . ? C22 C18 C19 N4 -4.0(10) . . . . ? N3 C18 C19 N4 175.8(6) . . . . ? N4 C20 C21 C22 -2.6(13) . . . . ? C20 C21 C22 C18 0.3(13) . . . . ? C19 C18 C22 C21 2.7(11) . . . . ? N3 C18 C22 C21 -177.1(7) . . . . ? O3 Co1 Cl1 Co1 0(20) . . . 14_655 ? N2 Co1 Cl1 Co1 -177(62) 11_654 . . 14_655 ? N2 Co1 Cl1 Co1 3(19) . . . 14_655 ? N4 Co1 Cl1 Co1 -86(19) 8_554 . . 14_655 ? N4 Co1 Cl1 Co1 94(19) 14_655 . . 14_655 ? O1 C6 N1 C7 2.8(13) . . . . ? C1 C6 N1 C7 -177.1(6) . . . . ? C8 C7 N1 C6 1.3(11) . . . . ? C11 C7 N1 C6 -179.3(7) . . . . ? C7 C8 N2 C9 0.9(9) . . . . ? C7 C8 N2 Co1 -175.6(5) . . . . ? C10 C9 N2 C8 1.8(10) . . . . ? C10 C9 N2 Co1 178.1(5) . . . . ? O3 Co1 N2 C8 134.5(4) . . . . ? N2 Co1 N2 C8 -45.5(5) 11_654 . . . ? N4 Co1 N2 C8 44.8(5) 8_554 . . . ? N4 Co1 N2 C8 -135.8(5) 14_655 . . . ? Cl1 Co1 N2 C8 -45.5(4) . . . . ? O3 Co1 N2 C9 -41.9(5) . . . . ? N2 Co1 N2 C9 138.1(5) 11_654 . . . ? N4 Co1 N2 C9 -131.5(5) 8_554 . . . ? N4 Co1 N2 C9 47.8(5) 14_655 . . . ? Cl1 Co1 N2 C9 138.1(5) . . . . ? O2 C17 N3 C18 -9.6(16) . . . . ? C16 C17 N3 C18 166.9(7) . . . . ? C19 C18 N3 C17 -154.0(9) . . . . ? C22 C18 N3 C17 25.7(13) . . . . ? C21 C20 N4 C19 1.5(10) . . . . ? C21 C20 N4 Co1 178.4(6) . . . 14_655 ? C18 C19 N4 C20 1.9(10) . . . . ? C18 C19 N4 Co1 -175.3(5) . . . 14_655 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O5 0.86 2.30 3.079(14) 150.2 1_654 O3 H3B O8 0.82 2.07 2.77(2) 142.9 1_655 N3 H3A O1 0.86 2.23 2.869(8) 131.5 . _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 1.725 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.143