# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2006 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_cambridge 0440 _publ_contact_author_name K.Nag _publ_contact_author_address ; Dept of Inorganic Chemistry Indian Association of the Cultivati Culcutta West Bengal 700032 INDIA ; _publ_section_title ; Formation of oxo-bridged tetrairon(III) complexes mediated by oxygen activation. Structure, spectroscopy, magnetism and electrochemistry ; _publ_contact_author_email ICKN@MAHENDRA.IACS.RES.IN loop_ _publ_author_name K.Nag P.Biswas S.K.Dutta U.Florke M.Ghosh W.Haase C.Saal # Attachment 'B610649H_CIF.txt' data_for_complex_3 _database_code_depnum_ccdc_archive 'CCDC 615601' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H58 Cl2 Fe4 N8 O18' _chemical_formula_weight 1377.36 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 16.936(3) _cell_length_b 15.203(3) _cell_length_c 21.457(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5524.7(18) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 724 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 16.51 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.656 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2832 _exptl_absorpt_coefficient_mu 1.209 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7769 _exptl_absorpt_correction_T_max 0.8887 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\p and \w scans' _diffrn_standards_number 743 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 42640 _diffrn_reflns_av_R_equivalents 0.2973 _diffrn_reflns_av_sigmaI/netI 0.3303 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 27.88 _reflns_number_total 6578 _reflns_number_gt 1604 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker (2002) SMART' _computing_cell_refinement 'Bruker (2002) SMART' _computing_data_reduction 'Bruker (2002) SAINT' _computing_structure_solution 'Bruker (2002) SHELXTL' _computing_structure_refinement 'Bruker (2002) SHELXTL' _computing_molecular_graphics 'Bruker (2002) SHELXTL' _computing_publication_material 'Bruker (2002) 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^)+(0.0252P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6578 _refine_ls_number_parameters 381 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2755 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1355 _refine_ls_wR_factor_gt 0.0876 _refine_ls_goodness_of_fit_ref 0.733 _refine_ls_restrained_S_all 0.733 _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 0.53891(10) 0.37202(7) 0.18536(7) 0.0260(4) Uani 1 1 d . . . Fe2 Fe 0.54243(9) 0.14167(7) 0.18701(7) 0.0234(4) Uani 1 1 d . . . O1 O 0.5275(5) 0.5087(4) 0.2021(3) 0.043(2) Uani 1 1 d . . . O2 O 0.4284(4) 0.3685(4) 0.2227(3) 0.0257(18) Uani 1 1 d . . . O3 O 0.5520(3) 0.2566(4) 0.17116(19) 0.0309(13) Uani 1 1 d . . . O4 O 0.4311(4) 0.1430(4) 0.2203(3) 0.0245(17) Uani 1 1 d . . . O5 O 0.5317(4) 0.0032(4) 0.2047(3) 0.0281(17) Uani 1 1 d . . . N1 N 0.6559(5) 0.3983(5) 0.1598(4) 0.027(2) Uani 1 1 d . . . N2 N 0.4879(5) 0.3928(5) 0.0987(4) 0.025(2) Uani 1 1 d . . . N3 N 0.6591(5) 0.1151(4) 0.1691(4) 0.026(2) Uani 1 1 d . . . N4 N 0.4968(5) 0.1226(5) 0.0997(4) 0.029(2) Uani 1 1 d . . . C1 C 0.7132(6) 0.4053(6) 0.1988(5) 0.031(3) Uani 1 1 d . . . H1A H 0.7643 0.4119 0.1811 0.038 Uiso 1 1 calc R . . C2 C 0.6764(6) 0.3967(6) 0.0926(4) 0.030(3) Uani 1 1 d . . . H2A H 0.6832 0.3348 0.0794 0.036 Uiso 1 1 calc R . . H2B H 0.7276 0.4270 0.0868 0.036 Uiso 1 1 calc R . . C3 C 0.6156(6) 0.4396(5) 0.0514(4) 0.036(3) Uani 1 1 d . . . H3A H 0.6025 0.4979 0.0692 0.043 Uiso 1 1 calc R . . H3B H 0.6397 0.4498 0.0100 0.043 Uiso 1 1 calc R . . C4 C 0.5401(7) 0.3892(6) 0.0424(4) 0.033(3) Uani 1 1 d . . . H4A H 0.5113 0.4136 0.0062 0.040 Uiso 1 1 calc R . . H4B H 0.5529 0.3270 0.0331 0.040 Uiso 1 1 calc R . . C5 C 0.4141(7) 0.3973(6) 0.0863(5) 0.034(3) Uani 1 1 d . . . H5A H 0.3995 0.3987 0.0435 0.040 Uiso 1 1 calc R . . C6 C 0.3501(6) 0.4005(6) 0.1324(4) 0.021(2) Uani 1 1 d . . . C7 C 0.2761(6) 0.4159(6) 0.1058(4) 0.027(2) Uani 1 1 d . . . H7A H 0.2724 0.4198 0.0617 0.032 Uiso 1 1 calc R . . C8 C 0.2079(6) 0.4256(6) 0.1406(4) 0.035(3) Uani 1 1 d . . . C9 C 0.2177(6) 0.4222(6) 0.2052(4) 0.035(3) Uani 1 1 d . . . H9A H 0.1729 0.4323 0.2308 0.042 Uiso 1 1 calc R . . C10 C 0.2903(6) 0.4044(6) 0.2345(4) 0.024(2) Uani 1 1 d . . . C11 C 0.3590(6) 0.3931(6) 0.1980(5) 0.028(3) Uani 1 1 d . . . C12 C 0.1291(6) 0.4382(6) 0.1123(4) 0.039(3) Uani 1 1 d . . . H12A H 0.1320 0.4843 0.0805 0.058 Uiso 1 1 calc R . . H12B H 0.0913 0.4556 0.1446 0.058 Uiso 1 1 calc R . . H12C H 0.1117 0.3831 0.0930 0.058 Uiso 1 1 calc R . . C13 C 0.5000 0.5468(10) 0.2500 0.038(4) Uani 1 2 d S . . C14 C 0.5000 0.6426(8) 0.2500 0.038(4) Uani 1 2 d S . . H14A H 0.5428 0.6641 0.2233 0.057 Uiso 0.50 1 calc PR . . H14B H 0.5079 0.6641 0.2926 0.057 Uiso 0.50 1 calc PR . . H14C H 0.4493 0.6641 0.2341 0.057 Uiso 0.50 1 calc PR . . C15 C 0.7155(6) 0.1323(5) 0.2079(4) 0.027(2) Uani 1 1 d . . . H15A H 0.7675 0.1318 0.1912 0.033 Uiso 1 1 calc R . . C16 C 0.6814(7) 0.0881(7) 0.1071(5) 0.042(3) Uani 1 1 d . . . H16A H 0.6729 0.0240 0.1027 0.050 Uiso 1 1 calc R . . H16B H 0.7383 0.1001 0.1007 0.050 Uiso 1 1 calc R . . C17 C 0.6331(5) 0.1369(7) 0.0566(4) 0.037(3) Uani 1 1 d . . . H17A H 0.6286 0.1997 0.0683 0.044 Uiso 1 1 calc R . . H17B H 0.6618 0.1336 0.0165 0.044 Uiso 1 1 calc R . . C18 C 0.5500(7) 0.0987(6) 0.0479(4) 0.034(3) Uani 1 1 d . . . H18A H 0.5275 0.1207 0.0083 0.040 Uiso 1 1 calc R . . H18B H 0.5535 0.0338 0.0451 0.040 Uiso 1 1 calc R . . C19 C 0.4239(6) 0.1433(6) 0.0847(5) 0.026(3) Uani 1 1 d . . . H19A H 0.4132 0.1495 0.0415 0.032 Uiso 1 1 calc R . . C20 C 0.3576(6) 0.1579(6) 0.1268(4) 0.025(2) Uani 1 1 d . . . C21 C 0.2845(6) 0.1731(6) 0.0987(4) 0.031(2) Uani 1 1 d . . . H21A H 0.2826 0.1818 0.0549 0.037 Uiso 1 1 calc R . . C22 C 0.2162(6) 0.1759(6) 0.1315(4) 0.035(3) Uani 1 1 d . . . C23 C 0.2221(6) 0.1643(6) 0.1955(4) 0.033(3) Uani 1 1 d . . . H23A H 0.1747 0.1649 0.2192 0.040 Uiso 1 1 calc R . . C24 C 0.2910(5) 0.1523(6) 0.2265(4) 0.023(2) Uani 1 1 d . . . C25 C 0.3615(6) 0.1549(6) 0.1930(5) 0.030(3) Uani 1 1 d . . . C26 C 0.1361(6) 0.1872(7) 0.0988(4) 0.053(3) Uani 1 1 d . . . H26A H 0.1446 0.2094 0.0565 0.080 Uiso 1 1 calc R . . H26B H 0.1037 0.2291 0.1223 0.080 Uiso 1 1 calc R . . H26C H 0.1091 0.1303 0.0969 0.080 Uiso 1 1 calc R . . C27 C 0.5000 -0.0322(8) 0.2500 0.028(4) Uani 1 2 d S . . C28 C 0.5000 -0.1350(8) 0.2500 0.066(6) Uani 1 2 d S . . H28A H 0.4459 -0.1565 0.2554 0.099 Uiso 0.50 1 calc PR . . H28B H 0.5330 -0.1565 0.2843 0.099 Uiso 0.50 1 calc PR . . H28C H 0.5211 -0.1565 0.2103 0.099 Uiso 0.50 1 calc PR . . Cl1 Cl 0.12510(16) 0.2664(2) 0.41786(12) 0.0527(8) Uani 1 1 d . . . O11 O 0.1303(5) 0.3585(5) 0.4339(3) 0.068(2) Uani 1 1 d . . . O12 O 0.1750(5) 0.2176(5) 0.4587(3) 0.076(3) Uani 1 1 d . . . O13 O 0.0455(4) 0.2425(7) 0.4267(3) 0.103(3) Uani 1 1 d . . . O14 O 0.1516(4) 0.2535(6) 0.3565(2) 0.071(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0284(10) 0.0248(7) 0.0248(9) 0.0010(7) 0.0027(9) -0.0001(7) Fe2 0.0208(9) 0.0264(7) 0.0229(8) -0.0033(7) -0.0007(9) -0.0011(7) O1 0.071(6) 0.025(3) 0.034(5) 0.004(3) 0.005(4) -0.001(4) O2 0.020(4) 0.027(4) 0.030(4) 0.001(3) -0.001(4) 0.010(3) O3 0.035(3) 0.031(3) 0.027(3) -0.002(3) 0.011(3) -0.001(4) O4 0.009(4) 0.037(4) 0.027(4) 0.000(3) -0.011(3) 0.004(3) O5 0.029(5) 0.033(3) 0.022(4) 0.009(3) 0.007(4) -0.003(4) N1 0.009(5) 0.038(5) 0.033(5) 0.001(4) -0.007(4) -0.004(4) N2 0.031(6) 0.035(5) 0.008(4) 0.002(4) -0.003(4) 0.012(4) N3 0.036(6) 0.022(4) 0.018(5) 0.004(3) -0.007(4) -0.005(4) N4 0.012(5) 0.022(4) 0.052(6) -0.001(4) 0.008(4) 0.001(4) C1 0.025(6) 0.024(5) 0.045(7) 0.005(5) 0.018(6) 0.000(5) C2 0.027(7) 0.051(7) 0.012(5) 0.004(5) -0.001(5) -0.017(5) C3 0.055(8) 0.021(5) 0.031(6) -0.002(5) 0.012(6) -0.018(5) C4 0.035(7) 0.035(5) 0.029(6) 0.001(5) 0.003(6) 0.000(6) C5 0.054(8) 0.022(5) 0.025(6) -0.010(5) -0.012(6) 0.023(5) C6 0.023(6) 0.018(5) 0.024(6) -0.008(4) 0.001(5) 0.005(4) C7 0.033(7) 0.032(6) 0.015(5) -0.005(5) -0.007(5) -0.001(5) C8 0.041(7) 0.034(6) 0.031(6) -0.006(5) -0.013(6) 0.010(6) C9 0.025(6) 0.038(6) 0.042(7) -0.013(5) 0.012(5) -0.008(5) C10 0.018(6) 0.028(5) 0.027(6) 0.006(5) 0.007(5) 0.002(5) C11 0.028(7) 0.019(5) 0.036(7) -0.017(5) 0.005(5) -0.005(5) C12 0.042(7) 0.041(6) 0.034(6) -0.013(5) -0.010(6) 0.010(6) C13 0.027(11) 0.042(10) 0.044(12) 0.000 -0.002(9) 0.000 C14 0.037(11) 0.030(8) 0.048(11) 0.000 0.002(9) 0.000 C15 0.022(6) 0.020(5) 0.040(6) 0.013(5) 0.001(5) 0.007(5) C16 0.052(9) 0.053(7) 0.020(6) -0.001(5) -0.013(6) 0.006(6) C17 0.025(6) 0.065(7) 0.019(5) 0.003(6) 0.014(5) 0.008(6) C18 0.042(8) 0.036(6) 0.023(6) -0.010(5) 0.003(6) 0.007(6) C19 0.029(6) 0.028(6) 0.021(5) -0.003(5) 0.018(5) -0.007(5) C20 0.027(6) 0.030(6) 0.018(5) 0.003(4) 0.007(5) -0.006(5) C21 0.022(6) 0.048(6) 0.023(5) -0.014(5) -0.011(5) 0.005(5) C22 0.025(6) 0.041(6) 0.038(6) -0.008(5) -0.006(5) 0.010(5) C23 0.033(6) 0.047(6) 0.020(5) -0.004(5) 0.009(5) 0.015(5) C24 0.009(5) 0.033(6) 0.028(5) -0.005(5) -0.009(4) 0.001(5) C25 0.020(6) 0.024(5) 0.045(7) 0.001(5) 0.014(6) 0.016(4) C26 0.029(7) 0.084(8) 0.046(7) -0.013(6) -0.021(6) -0.002(6) C27 0.041(11) 0.023(7) 0.020(9) 0.000 -0.013(8) 0.000 C28 0.093(17) 0.025(9) 0.080(15) 0.000 0.013(13) 0.000 Cl1 0.0406(16) 0.075(2) 0.0427(15) -0.0100(18) 0.0074(14) -0.0038(18) O11 0.081(6) 0.060(5) 0.065(5) 0.001(5) 0.022(5) -0.003(6) O12 0.099(7) 0.077(6) 0.053(5) 0.011(4) -0.013(5) 0.029(5) O13 0.050(5) 0.137(7) 0.122(6) -0.026(9) 0.033(5) -0.041(8) O14 0.083(5) 0.094(5) 0.037(4) -0.021(6) 0.008(4) 0.011(7) _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 O3 1.795(6) . ? Fe1 O2 2.036(7) . ? Fe1 O2 2.050(7) 4_655 ? Fe1 N2 2.075(8) . ? Fe1 N1 2.094(8) . ? Fe1 O1 2.118(6) . ? Fe2 O3 1.787(6) . ? Fe2 O4 2.016(7) . ? Fe2 O4 2.039(6) 4_655 ? Fe2 N4 2.047(9) . ? Fe2 N3 2.053(9) . ? Fe2 O5 2.147(6) . ? O1 C13 1.267(9) . ? O2 C11 1.343(11) . ? O2 Fe1 2.050(7) 4_655 ? O4 C25 1.329(11) . ? O4 Fe2 2.039(6) 4_655 ? O5 C27 1.234(7) . ? N1 C1 1.286(12) . ? N1 C2 1.482(11) . ? N2 C5 1.279(12) . ? N2 C4 1.498(12) . ? N3 C15 1.294(11) . ? N3 C16 1.443(12) . ? N4 C19 1.315(11) . ? N4 C18 1.475(12) . ? C1 C10 1.434(12) 4_655 ? C1 H1A 0.9500 . ? C2 C3 1.506(13) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.503(14) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.470(13) . ? C5 H5A 0.9500 . ? C6 C7 1.398(12) . ? C6 C11 1.419(12) . ? C7 C8 1.384(13) . ? C7 H7A 0.9500 . ? C8 C9 1.397(12) . ? C8 C12 1.478(12) . ? C9 C10 1.406(13) . ? C9 H9A 0.9500 . ? C10 C11 1.412(12) . ? C10 C1 1.434(12) 4_655 ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 O1 1.267(9) 4_655 ? C13 C14 1.457(17) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C24 1.444(12) 4_655 ? C15 H15A 0.9500 . ? C16 C17 1.545(12) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.535(14) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.458(12) . ? C19 H19A 0.9500 . ? C20 C21 1.397(12) . ? C20 C25 1.423(12) . ? C21 C22 1.356(12) . ? C21 H21A 0.9500 . ? C22 C23 1.388(12) . ? C22 C26 1.536(12) . ? C23 C24 1.356(12) . ? C23 H23A 0.9500 . ? C24 C25 1.393(12) . ? C24 C15 1.444(12) 4_655 ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 O5 1.234(7) 4_655 ? C27 C28 1.563(17) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? Cl1 O14 1.404(5) . ? Cl1 O13 1.409(7) . ? Cl1 O12 1.426(7) . ? Cl1 O11 1.445(8) . ? 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 O3 Fe1 O2 98.9(2) . . ? O3 Fe1 O2 96.0(2) . 4_655 ? O2 Fe1 O2 82.5(3) . 4_655 ? O3 Fe1 N2 92.8(3) . . ? O2 Fe1 N2 88.5(3) . . ? O2 Fe1 N2 168.3(3) 4_655 . ? O3 Fe1 N1 91.5(3) . . ? O2 Fe1 N1 167.8(3) . . ? O2 Fe1 N1 90.1(3) 4_655 . ? N2 Fe1 N1 97.5(3) . . ? O3 Fe1 O1 178.2(3) . . ? O2 Fe1 O1 82.8(3) . . ? O2 Fe1 O1 83.5(3) 4_655 . ? N2 Fe1 O1 88.0(3) . . ? N1 Fe1 O1 86.8(3) . . ? O3 Fe2 O4 98.2(2) . . ? O3 Fe2 O4 99.0(2) . 4_655 ? O4 Fe2 O4 81.9(3) . 4_655 ? O3 Fe2 N4 89.9(3) . . ? O4 Fe2 N4 88.4(3) . . ? O4 Fe2 N4 167.7(3) 4_655 . ? O3 Fe2 N3 94.0(3) . . ? O4 Fe2 N3 165.5(3) . . ? O4 Fe2 N3 88.5(3) 4_655 . ? N4 Fe2 N3 99.4(3) . . ? O3 Fe2 O5 179.1(3) . . ? O4 Fe2 O5 82.4(2) . . ? O4 Fe2 O5 81.7(2) 4_655 . ? N4 Fe2 O5 89.5(3) . . ? N3 Fe2 O5 85.5(3) . . ? C13 O1 Fe1 128.2(8) . . ? C11 O2 Fe1 130.0(6) . . ? C11 O2 Fe1 127.5(6) . 4_655 ? Fe1 O2 Fe1 97.4(3) . 4_655 ? Fe2 O3 Fe1 155.8(3) . . ? C25 O4 Fe2 132.5(6) . . ? C25 O4 Fe2 128.7(6) . 4_655 ? Fe2 O4 Fe2 98.1(3) . 4_655 ? C27 O5 Fe2 127.1(7) . . ? C1 N1 C2 117.2(8) . . ? C1 N1 Fe1 124.0(7) . . ? C2 N1 Fe1 118.3(6) . . ? C5 N2 C4 114.2(9) . . ? C5 N2 Fe1 127.0(8) . . ? C4 N2 Fe1 118.1(7) . . ? C15 N3 C16 117.3(9) . . ? C15 N3 Fe2 123.4(7) . . ? C16 N3 Fe2 118.7(7) . . ? C19 N4 C18 116.6(9) . . ? C19 N4 Fe2 123.0(7) . . ? C18 N4 Fe2 119.6(7) . . ? N1 C1 C10 128.2(10) . 4_655 ? N1 C1 H1A 115.9 . . ? C10 C1 H1A 115.9 4_655 . ? N1 C2 C3 113.8(9) . . ? N1 C2 H2A 108.8 . . ? C3 C2 H2A 108.8 . . ? N1 C2 H2B 108.8 . . ? C3 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C4 C3 C2 115.8(8) . . ? C4 C3 H3A 108.3 . . ? C2 C3 H3A 108.3 . . ? C4 C3 H3B 108.3 . . ? C2 C3 H3B 108.3 . . ? H3A C3 H3B 107.4 . . ? N2 C4 C3 112.4(8) . . ? N2 C4 H4A 109.1 . . ? C3 C4 H4A 109.1 . . ? N2 C4 H4B 109.1 . . ? C3 C4 H4B 109.1 . . ? H4A C4 H4B 107.9 . . ? N2 C5 C6 125.5(10) . . ? N2 C5 H5A 117.2 . . ? C6 C5 H5A 117.2 . . ? C7 C6 C11 120.9(9) . . ? C7 C6 C5 113.0(8) . . ? C11 C6 C5 126.0(9) . . ? C8 C7 C6 123.1(9) . . ? C8 C7 H7A 118.5 . . ? C6 C7 H7A 118.5 . . ? C7 C8 C9 115.6(9) . . ? C7 C8 C12 123.0(9) . . ? C9 C8 C12 121.4(10) . . ? C8 C9 C10 123.7(10) . . ? C8 C9 H9A 118.2 . . ? C10 C9 H9A 118.2 . . ? C9 C10 C11 119.7(9) . . ? C9 C10 C1 114.1(9) . 4_655 ? C11 C10 C1 126.0(10) . 4_655 ? O2 C11 C10 122.4(9) . . ? O2 C11 C6 120.3(9) . . ? C10 C11 C6 116.9(9) . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O1 C13 O1 125.7(14) 4_655 . ? O1 C13 C14 117.1(7) 4_655 . ? O1 C13 C14 117.1(7) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 C24 127.8(10) . 4_655 ? N3 C15 H15A 116.1 . . ? C24 C15 H15A 116.1 4_655 . ? N3 C16 C17 111.8(8) . . ? N3 C16 H16A 109.3 . . ? C17 C16 H16A 109.3 . . ? N3 C16 H16B 109.3 . . ? C17 C16 H16B 109.3 . . ? H16A C16 H16B 107.9 . . ? C18 C17 C16 112.9(9) . . ? C18 C17 H17A 109.0 . . ? C16 C17 H17A 109.0 . . ? C18 C17 H17B 109.0 . . ? C16 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? N4 C18 C17 112.0(8) . . ? N4 C18 H18A 109.2 . . ? C17 C18 H18A 109.2 . . ? N4 C18 H18B 109.2 . . ? C17 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? N4 C19 C20 127.5(10) . . ? N4 C19 H19A 116.3 . . ? C20 C19 H19A 116.3 . . ? C21 C20 C25 118.5(9) . . ? C21 C20 C19 116.1(8) . . ? C25 C20 C19 125.3(9) . . ? C22 C21 C20 122.5(9) . . ? C22 C21 H21A 118.7 . . ? C20 C21 H21A 118.7 . . ? C21 C22 C23 116.7(9) . . ? C21 C22 C26 121.3(9) . . ? C23 C22 C26 122.0(9) . . ? C24 C23 C22 124.3(9) . . ? C24 C23 H23A 117.8 . . ? C22 C23 H23A 117.8 . . ? C23 C24 C25 118.8(9) . . ? C23 C24 C15 116.1(9) . 4_655 ? C25 C24 C15 125.0(9) . 4_655 ? O4 C25 C24 122.0(9) . . ? O4 C25 C20 119.0(9) . . ? C24 C25 C20 118.4(9) . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O5 C27 O5 128.3(12) . 4_655 ? O5 C27 C28 115.9(6) . . ? O5 C27 C28 115.9(6) 4_655 . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O14 Cl1 O13 113.3(5) . . ? O14 Cl1 O12 108.3(5) . . ? O13 Cl1 O12 110.5(5) . . ? O14 Cl1 O11 109.8(6) . . ? O13 Cl1 O11 106.1(6) . . ? O12 Cl1 O11 108.8(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 O3 Fe1 O1 C13 -114(8) . . . . ? O2 Fe1 O1 C13 43.4(7) . . . . ? O2 Fe1 O1 C13 -39.8(7) 4_655 . . . ? N2 Fe1 O1 C13 132.1(7) . . . . ? N1 Fe1 O1 C13 -130.3(7) . . . . ? O3 Fe1 O2 C11 -106.5(7) . . . . ? O2 Fe1 O2 C11 158.6(6) 4_655 . . . ? N2 Fe1 O2 C11 -13.9(7) . . . . ? N1 Fe1 O2 C11 105.7(15) . . . . ? O1 Fe1 O2 C11 74.2(7) . . . . ? O3 Fe1 O2 Fe1 98.0(2) . . . 4_655 ? O2 Fe1 O2 Fe1 3.0(3) 4_655 . . 4_655 ? N2 Fe1 O2 Fe1 -169.5(3) . . . 4_655 ? N1 Fe1 O2 Fe1 -49.8(15) . . . 4_655 ? O1 Fe1 O2 Fe1 -81.3(3) . . . 4_655 ? O4 Fe2 O3 Fe1 39.0(8) . . . . ? O4 Fe2 O3 Fe1 -44.1(8) 4_655 . . . ? N4 Fe2 O3 Fe1 127.4(8) . . . . ? N3 Fe2 O3 Fe1 -133.1(8) . . . . ? O5 Fe2 O3 Fe1 174(100) . . . . ? O2 Fe1 O3 Fe2 -36.7(8) . . . . ? O2 Fe1 O3 Fe2 46.6(8) 4_655 . . . ? N2 Fe1 O3 Fe2 -125.6(8) . . . . ? N1 Fe1 O3 Fe2 136.9(8) . . . . ? O1 Fe1 O3 Fe2 121(8) . . . . ? O3 Fe2 O4 C25 71.4(8) . . . . ? O4 Fe2 O4 C25 169.4(7) 4_655 . . . ? N4 Fe2 O4 C25 -18.2(8) . . . . ? N3 Fe2 O4 C25 -141.7(11) . . . . ? O5 Fe2 O4 C25 -107.9(8) . . . . ? O3 Fe2 O4 Fe2 -99.1(2) . . . 4_655 ? O4 Fe2 O4 Fe2 -1.2(3) 4_655 . . 4_655 ? N4 Fe2 O4 Fe2 171.2(3) . . . 4_655 ? N3 Fe2 O4 Fe2 47.7(12) . . . 4_655 ? O5 Fe2 O4 Fe2 81.5(3) . . . 4_655 ? O3 Fe2 O5 C27 -175(100) . . . . ? O4 Fe2 O5 C27 -40.3(6) . . . . ? O4 Fe2 O5 C27 42.6(6) 4_655 . . . ? N4 Fe2 O5 C27 -128.8(6) . . . . ? N3 Fe2 O5 C27 131.6(6) . . . . ? O3 Fe1 N1 C1 -95.8(8) . . . . ? O2 Fe1 N1 C1 52.4(18) . . . . ? O2 Fe1 N1 C1 0.2(8) 4_655 . . . ? N2 Fe1 N1 C1 171.2(8) . . . . ? O1 Fe1 N1 C1 83.7(8) . . . . ? O3 Fe1 N1 C2 75.4(7) . . . . ? O2 Fe1 N1 C2 -136.4(13) . . . . ? O2 Fe1 N1 C2 171.4(7) 4_655 . . . ? N2 Fe1 N1 C2 -17.6(7) . . . . ? O1 Fe1 N1 C2 -105.1(7) . . . . ? O3 Fe1 N2 C5 97.8(9) . . . . ? O2 Fe1 N2 C5 -1.0(9) . . . . ? O2 Fe1 N2 C5 -40(2) 4_655 . . . ? N1 Fe1 N2 C5 -170.4(8) . . . . ? O1 Fe1 N2 C5 -83.9(9) . . . . ? O3 Fe1 N2 C4 -72.3(6) . . . . ? O2 Fe1 N2 C4 -171.1(6) . . . . ? O2 Fe1 N2 C4 149.5(12) 4_655 . . . ? N1 Fe1 N2 C4 19.6(7) . . . . ? O1 Fe1 N2 C4 106.1(7) . . . . ? O3 Fe2 N3 C15 77.5(7) . . . . ? O4 Fe2 N3 C15 -69.7(14) . . . . ? O4 Fe2 N3 C15 -21.4(7) 4_655 . . . ? N4 Fe2 N3 C15 168.0(7) . . . . ? O5 Fe2 N3 C15 -103.2(7) . . . . ? O3 Fe2 N3 C16 -93.0(7) . . . . ? O4 Fe2 N3 C16 119.9(12) . . . . ? O4 Fe2 N3 C16 168.1(7) 4_655 . . . ? N4 Fe2 N3 C16 -2.4(7) . . . . ? O5 Fe2 N3 C16 86.3(7) . . . . ? O3 Fe2 N4 C19 -76.6(7) . . . . ? O4 Fe2 N4 C19 21.6(7) . . . . ? O4 Fe2 N4 C19 59.9(17) 4_655 . . . ? N3 Fe2 N4 C19 -170.6(7) . . . . ? O5 Fe2 N4 C19 104.0(8) . . . . ? O3 Fe2 N4 C18 92.9(7) . . . . ? O4 Fe2 N4 C18 -168.9(7) . . . . ? O4 Fe2 N4 C18 -130.6(13) 4_655 . . . ? N3 Fe2 N4 C18 -1.1(7) . . . . ? O5 Fe2 N4 C18 -86.5(7) . . . . ? C2 N1 C1 C10 -177.0(9) . . . 4_655 ? Fe1 N1 C1 C10 -5.6(14) . . . 4_655 ? C1 N1 C2 C3 -146.4(9) . . . . ? Fe1 N1 C2 C3 41.8(10) . . . . ? N1 C2 C3 C4 -72.9(11) . . . . ? C5 N2 C4 C3 143.0(9) . . . . ? Fe1 N2 C4 C3 -45.7(10) . . . . ? C2 C3 C4 N2 74.7(11) . . . . ? C4 N2 C5 C6 179.2(8) . . . . ? Fe1 N2 C5 C6 8.8(15) . . . . ? N2 C5 C6 C7 172.8(9) . . . . ? N2 C5 C6 C11 -4.6(16) . . . . ? C11 C6 C7 C8 0.7(15) . . . . ? C5 C6 C7 C8 -176.9(9) . . . . ? C6 C7 C8 C9 2.1(15) . . . . ? C6 C7 C8 C12 -177.5(9) . . . . ? C7 C8 C9 C10 -4.0(16) . . . . ? C12 C8 C9 C10 175.6(8) . . . . ? C8 C9 C10 C11 3.0(16) . . . . ? C8 C9 C10 C1 179.2(10) . . . 4_655 ? Fe1 O2 C11 C10 -165.7(6) . . . . ? Fe1 O2 C11 C10 -16.9(12) 4_655 . . . ? Fe1 O2 C11 C6 20.5(12) . . . . ? Fe1 O2 C11 C6 169.3(6) 4_655 . . . ? C9 C10 C11 O2 -174.0(8) . . . . ? C1 C10 C11 O2 10.3(15) 4_655 . . . ? C9 C10 C11 C6 0.0(13) . . . . ? C1 C10 C11 C6 -175.7(9) 4_655 . . . ? C7 C6 C11 O2 172.3(8) . . . . ? C5 C6 C11 O2 -10.4(14) . . . . ? C7 C6 C11 C10 -1.8(13) . . . . ? C5 C6 C11 C10 175.5(8) . . . . ? Fe1 O1 C13 O1 -1.0(4) . . . 4_655 ? Fe1 O1 C13 C14 179.0(4) . . . . ? C16 N3 C15 C24 -173.7(9) . . . 4_655 ? Fe2 N3 C15 C24 15.7(13) . . . 4_655 ? C15 N3 C16 C17 -134.0(9) . . . . ? Fe2 N3 C16 C17 37.0(11) . . . . ? N3 C16 C17 C18 -78.9(11) . . . . ? C19 N4 C18 C17 139.9(9) . . . . ? Fe2 N4 C18 C17 -30.3(10) . . . . ? C16 C17 C18 N4 74.2(10) . . . . ? C18 N4 C19 C20 171.2(8) . . . . ? Fe2 N4 C19 C20 -19.0(13) . . . . ? N4 C19 C20 C21 -175.6(9) . . . . ? N4 C19 C20 C25 2.3(16) . . . . ? C25 C20 C21 C22 -7.1(15) . . . . ? C19 C20 C21 C22 170.9(9) . . . . ? C20 C21 C22 C23 1.1(16) . . . . ? C20 C21 C22 C26 -176.3(9) . . . . ? C21 C22 C23 C24 1.3(16) . . . . ? C26 C22 C23 C24 178.6(9) . . . . ? C22 C23 C24 C25 2.6(15) . . . . ? C22 C23 C24 C15 -173.8(9) . . . 4_655 ? Fe2 O4 C25 C24 179.6(6) . . . . ? Fe2 O4 C25 C24 -12.4(12) 4_655 . . . ? Fe2 O4 C25 C20 8.7(13) . . . . ? Fe2 O4 C25 C20 176.7(6) 4_655 . . . ? C23 C24 C25 O4 -179.5(8) . . . . ? C15 C24 C25 O4 -3.5(14) 4_655 . . . ? C23 C24 C25 C20 -8.5(13) . . . . ? C15 C24 C25 C20 167.5(9) 4_655 . . . ? C21 C20 C25 O4 -178.1(8) . . . . ? C19 C20 C25 O4 4.1(14) . . . . ? C21 C20 C25 C24 10.7(13) . . . . ? C19 C20 C25 C24 -167.1(8) . . . . ? Fe2 O5 C27 O5 -0.9(3) . . . 4_655 ? Fe2 O5 C27 C28 179.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.477 _refine_diff_density_min -0.538 _refine_diff_density_rms 0.086 data_for_complex_6 _database_code_depnum_ccdc_archive 'CCDC 615602' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H62 Cl2 Fe4 N8 O18' _chemical_formula_weight 1501.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.958(4) _cell_length_b 15.182(3) _cell_length_c 19.591(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.61(2) _cell_angle_gamma 90.00 _cell_volume 6528(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 8 _cell_measurement_theta_max 19 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.528 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3088 _exptl_absorpt_coefficient_mu 1.030 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.5865 _exptl_absorpt_correction_T_max 0.8205 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker P4' _diffrn_measurement_method omega _diffrn_standards_number 3 _diffrn_standards_interval_count 400 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 6 _diffrn_reflns_number 7732 _diffrn_reflns_av_R_equivalents 0.0567 _diffrn_reflns_av_sigmaI/netI 0.0707 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.56 _reflns_number_total 7547 _reflns_number_gt 4062 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0550P)^2^+9.0788P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7547 _refine_ls_number_parameters 482 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.1307 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1511 _refine_ls_wR_factor_gt 0.1212 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.003 _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 0.18378(3) 0.32430(4) 0.06782(3) 0.03923(18) Uani 1 1 d . . . Fe2 Fe 0.27435(3) 0.17980(4) 0.10470(3) 0.04139(19) Uani 1 1 d . . . O1 O 0.27353(13) 0.31605(18) 0.10137(13) 0.0389(7) Uani 1 1 d . B . O2 O 0.18564(14) 0.19133(18) 0.07467(14) 0.0438(7) Uani 1 1 d . B . O3 O 0.16633(14) 0.3089(2) 0.17614(15) 0.0516(8) Uani 1 1 d . . . O4 O 0.23594(15) 0.2046(2) 0.20258(14) 0.0492(8) Uani 1 1 d . . . O5 O 0.19822(14) 0.33815(19) -0.02078(14) 0.0488(8) Uani 1 1 d . . . N1 N 0.18493(18) 0.4564(2) 0.09247(19) 0.0482(10) Uani 1 1 d . B . N2 N 0.09041(18) 0.3124(3) 0.0445(2) 0.0509(10) Uani 1 1 d . B . N3 N 0.2572(2) 0.0454(3) 0.11983(19) 0.0542(11) Uani 1 1 d . B . N4 N 0.35686(18) 0.1835(3) 0.15689(18) 0.0492(10) Uani 1 1 d . B . C1 C 0.1323(2) 0.5102(3) 0.0695(3) 0.0696(16) Uani 1 1 d . . . H1A H 0.1337 0.5193 0.0206 0.084 Uiso 1 1 calc R A 1 H1B H 0.1343 0.5673 0.0916 0.084 Uiso 1 1 calc R A 1 C2 C 0.0730(3) 0.4650(5) 0.0866(5) 0.074(3) Uani 0.797(14) 1 d P B 1 H2A H 0.0771 0.4427 0.1329 0.088 Uiso 0.797(14) 1 calc PR B 1 H2B H 0.0413 0.5095 0.0864 0.088 Uiso 0.797(14) 1 calc PR B 1 C2' C 0.0872(14) 0.4748(16) 0.0271(18) 0.065(11) Uani 0.203(14) 1 d P B 2 H2C H 0.1058 0.4648 -0.0166 0.078 Uiso 0.203(14) 1 calc PR B 2 H2D H 0.0572 0.5210 0.0197 0.078 Uiso 0.203(14) 1 calc PR B 2 C3 C 0.0520(3) 0.3924(4) 0.0426(3) 0.0771(17) Uani 1 1 d . . . H3A H 0.0494 0.4136 -0.0041 0.093 Uiso 1 1 calc R B 1 H3B H 0.0112 0.3762 0.0555 0.093 Uiso 1 1 calc R B 1 C4 C 0.0695(2) 0.2445(3) 0.0130(3) 0.0565(13) Uani 1 1 d . . . H4 H 0.0312 0.2509 -0.0078 0.068 Uiso 1 1 calc R B . C5 C 0.1526(2) 0.1333(3) 0.0399(2) 0.0439(11) Uani 1 1 d . . . C6 C 0.0979(2) 0.1585(3) 0.0054(2) 0.0492(12) Uani 1 1 d . B . C7 C 0.0665(2) 0.0955(4) -0.0340(3) 0.0607(14) Uani 1 1 d . . . H7 H 0.0314 0.1129 -0.0579 0.073 Uiso 1 1 calc R B . C8 C 0.0847(3) 0.0100(4) -0.0392(3) 0.0627(14) Uani 1 1 d . B . C9 C 0.1339(3) -0.0164(3) 0.0002(3) 0.0622(14) Uani 1 1 d . . . H9 H 0.1444 -0.0757 0.0008 0.075 Uiso 1 1 calc R B . C10 C 0.1688(2) 0.0426(3) 0.0394(2) 0.0505(12) Uani 1 1 d . B . C11 C 0.0500(3) -0.0559(4) -0.0839(3) 0.086(2) Uani 1 1 d . . . H11A H 0.0420 -0.1081 -0.0579 0.129 Uiso 1 1 calc R B . H11B H 0.0740 -0.0710 -0.1224 0.129 Uiso 1 1 calc R . . H11C H 0.0122 -0.0303 -0.0996 0.129 Uiso 1 1 calc R . . C12 C 0.2272(2) 0.4947(3) 0.1265(2) 0.0497(12) Uani 1 1 d . . . H12 H 0.2223 0.5550 0.1328 0.060 Uiso 1 1 calc R B . C13 C 0.3022(2) 0.3694(3) 0.1460(2) 0.0402(10) Uani 1 1 d . . . C14 C 0.2821(2) 0.4566(3) 0.1569(2) 0.0452(11) Uani 1 1 d . B . C15 C 0.3151(2) 0.5119(3) 0.2011(2) 0.0534(12) Uani 1 1 d . . . H15 H 0.3007 0.5688 0.2078 0.064 Uiso 1 1 calc R B . C16 C 0.3677(2) 0.4868(3) 0.2353(3) 0.0578(13) Uani 1 1 d . B . C17 C 0.3867(2) 0.4012(3) 0.2251(2) 0.0569(13) Uani 1 1 d . . . H17 H 0.4219 0.3821 0.2481 0.068 Uiso 1 1 calc R B . C18 C 0.3558(2) 0.3416(3) 0.1820(2) 0.0460(11) Uani 1 1 d . B . C19 C 0.4016(3) 0.5482(4) 0.2835(3) 0.0823(19) Uani 1 1 d . . . H19A H 0.4314 0.5807 0.2588 0.123 Uiso 1 1 calc R B . H19B H 0.4217 0.5146 0.3190 0.123 Uiso 1 1 calc R . . H19C H 0.3734 0.5884 0.3033 0.123 Uiso 1 1 calc R . . C20 C 0.1951(2) 0.2591(3) 0.2168(2) 0.0460(11) Uani 1 1 d . . . C21 C 0.1800(3) 0.2647(3) 0.2912(2) 0.0590(15) Uani 1 1 d D . . C22 C 0.1218(3) 0.2864(4) 0.3105(3) 0.087(2) Uani 1 1 d D . . H22 H 0.0910 0.2992 0.2785 0.105 Uiso 1 1 calc R . . C23 C 0.1116(5) 0.2882(5) 0.3820(5) 0.132(4) Uani 1 1 d D . . H23 H 0.0729 0.3019 0.3969 0.159 Uiso 1 1 calc R . . C24 C 0.1559(8) 0.2708(6) 0.4287(5) 0.163(6) Uani 1 1 d D . . H24 H 0.1474 0.2725 0.4750 0.196 Uiso 1 1 calc R . . C25 C 0.2128(6) 0.2507(5) 0.4089(3) 0.140(4) Uani 1 1 d D . . H25 H 0.2434 0.2394 0.4415 0.168 Uiso 1 1 calc R . . C26 C 0.2252(3) 0.2469(3) 0.3402(3) 0.0795(19) Uani 1 1 d D . . H26 H 0.2642 0.2325 0.3266 0.095 Uiso 1 1 calc R . . C27 C 0.2997(3) -0.0107(3) 0.1606(3) 0.0745(17) Uani 1 1 d . . . H27A H 0.2759 -0.0507 0.1878 0.089 Uiso 1 1 calc R C 3 H27B H 0.3229 -0.0462 0.1294 0.089 Uiso 1 1 calc R C 3 C28 C 0.3426(3) 0.0364(4) 0.2064(3) 0.072(3) Uani 0.861(11) 1 d P D 3 H28A H 0.3661 -0.0067 0.2325 0.087 Uiso 0.861(11) 1 calc PR D 3 H28B H 0.3194 0.0704 0.2385 0.087 Uiso 0.861(11) 1 calc PR D 3 C28' C 0.3708(18) 0.027(3) 0.141(2) 0.070(15) Uani 0.139(11) 1 d P D 4 H28C H 0.4002 -0.0190 0.1531 0.084 Uiso 0.139(11) 1 calc PR D 4 H28D H 0.3720 0.0352 0.0921 0.084 Uiso 0.139(11) 1 calc PR D 4 C29 C 0.3877(3) 0.0994(4) 0.1711(3) 0.0730(18) Uani 1 1 d . . . H29A H 0.4233 0.1091 0.2006 0.088 Uiso 1 1 calc R D 3 H29B H 0.4011 0.0734 0.1288 0.088 Uiso 1 1 calc R D 3 C30 C 0.2166(3) 0.0055(3) 0.0833(3) 0.0589(14) Uani 1 1 d . . . H30 H 0.2179 -0.0557 0.0851 0.071 Uiso 1 1 calc R B . C31 C 0.3811(2) 0.2528(3) 0.1819(2) 0.0503(12) Uani 1 1 d . . . H31 H 0.4195 0.2460 0.2026 0.060 Uiso 1 1 calc R B . Cl1 Cl 0.42590(9) 0.23953(12) 0.37689(8) 0.0840(5) Uani 1 1 d D . . O111 O 0.4545(10) 0.3119(12) 0.3629(11) 0.191(13) Uani 0.50 1 d PD E 5 O121 O 0.3667(6) 0.245(2) 0.3654(14) 0.31(2) Uani 0.50 1 d PD E 5 O131 O 0.4345(7) 0.2142(11) 0.4406(5) 0.114(7) Uani 0.50 1 d PD E 5 O141 O 0.4461(17) 0.1759(12) 0.3374(11) 0.330(18) Uani 0.50 1 d PD E 5 O112 O 0.4734(6) 0.2775(11) 0.3386(8) 0.110(6) Uani 0.50 1 d PD E 6 O122 O 0.3866(6) 0.1933(7) 0.3330(5) 0.079(4) Uani 0.50 1 d PD E 6 O132 O 0.4501(8) 0.1836(10) 0.4279(8) 0.173(12) Uani 0.50 1 d PD E 6 O142 O 0.3942(9) 0.3119(10) 0.4068(8) 0.195(8) Uani 0.50 1 d PD E 6 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 0.0467(4) 0.0375(3) 0.0335(3) -0.0013(3) 0.0015(3) 0.0095(3) Fe2 0.0556(4) 0.0374(4) 0.0311(3) 0.0022(3) 0.0000(3) 0.0116(3) O1 0.0450(17) 0.0351(15) 0.0368(15) 0.0010(13) 0.0021(13) 0.0043(14) O2 0.056(2) 0.0373(18) 0.0384(16) -0.0029(13) -0.0019(14) 0.0051(15) O3 0.057(2) 0.054(2) 0.0436(17) 0.0009(16) 0.0083(15) 0.0142(17) O4 0.066(2) 0.0476(19) 0.0344(16) 0.0012(14) 0.0056(15) 0.0079(16) O5 0.062(2) 0.050(2) 0.0344(15) -0.0006(14) 0.0026(14) 0.0148(16) N1 0.058(3) 0.040(2) 0.046(2) -0.0026(18) -0.0016(19) 0.0167(19) N2 0.048(2) 0.050(2) 0.054(2) -0.002(2) 0.0022(19) 0.009(2) N3 0.080(3) 0.040(2) 0.043(2) 0.0067(18) 0.000(2) 0.016(2) N4 0.062(3) 0.048(2) 0.037(2) 0.0003(19) -0.0052(18) 0.016(2) C1 0.070(4) 0.046(3) 0.092(4) -0.010(3) -0.016(3) 0.019(3) C2 0.066(5) 0.075(5) 0.079(6) -0.014(4) -0.002(4) 0.036(4) C2' 0.08(2) 0.039(15) 0.07(2) -0.014(14) -0.016(16) 0.020(14) C3 0.059(4) 0.073(4) 0.099(5) -0.007(4) -0.004(3) 0.021(3) C4 0.047(3) 0.065(4) 0.058(3) 0.002(3) -0.002(2) -0.002(3) C5 0.053(3) 0.043(3) 0.036(2) -0.002(2) 0.008(2) -0.004(2) C6 0.053(3) 0.050(3) 0.045(3) 0.000(2) 0.001(2) -0.006(2) C7 0.051(3) 0.074(4) 0.057(3) -0.005(3) 0.003(3) -0.010(3) C8 0.064(4) 0.063(4) 0.062(3) -0.011(3) 0.012(3) -0.018(3) C9 0.080(4) 0.041(3) 0.066(3) -0.008(3) 0.012(3) -0.009(3) C10 0.064(3) 0.041(3) 0.047(3) 0.001(2) 0.007(2) -0.003(2) C11 0.077(4) 0.091(5) 0.091(4) -0.033(4) 0.008(3) -0.032(4) C12 0.064(3) 0.035(3) 0.049(3) -0.004(2) 0.003(2) 0.008(2) C13 0.042(3) 0.041(2) 0.037(2) 0.003(2) 0.002(2) 0.002(2) C14 0.046(3) 0.042(3) 0.047(3) 0.001(2) 0.000(2) 0.001(2) C15 0.059(3) 0.042(3) 0.059(3) -0.006(2) -0.002(3) -0.001(2) C16 0.064(3) 0.057(3) 0.053(3) -0.003(2) -0.002(3) -0.010(3) C17 0.056(3) 0.063(3) 0.051(3) 0.006(3) -0.002(2) 0.000(3) C18 0.049(3) 0.051(3) 0.039(2) 0.002(2) 0.007(2) 0.003(2) C19 0.081(4) 0.078(4) 0.088(4) -0.016(3) -0.017(3) -0.015(3) C20 0.060(3) 0.040(3) 0.038(2) -0.001(2) 0.009(2) -0.004(2) C21 0.103(5) 0.036(3) 0.039(3) -0.002(2) 0.019(3) -0.009(3) C22 0.113(6) 0.068(4) 0.084(4) -0.013(3) 0.052(4) -0.019(4) C23 0.193(11) 0.083(6) 0.128(8) -0.013(6) 0.114(8) -0.020(6) C24 0.36(2) 0.071(6) 0.067(5) 0.000(5) 0.090(9) -0.017(9) C25 0.307(15) 0.074(5) 0.040(4) -0.007(3) 0.011(6) 0.000(7) C26 0.143(6) 0.053(3) 0.042(3) -0.002(3) 0.000(3) -0.003(4) C27 0.105(5) 0.048(3) 0.070(4) 0.012(3) -0.012(4) 0.022(3) C28 0.109(6) 0.051(4) 0.055(4) 0.010(3) -0.019(4) 0.028(4) C28' 0.07(3) 0.06(3) 0.08(3) 0.02(2) 0.03(2) 0.03(2) C29 0.088(5) 0.063(4) 0.068(4) -0.008(3) -0.015(3) 0.033(3) C30 0.089(4) 0.034(3) 0.054(3) 0.002(2) 0.009(3) 0.003(3) C31 0.041(3) 0.066(3) 0.044(3) 0.004(2) -0.001(2) 0.012(3) Cl1 0.1032(14) 0.0820(12) 0.0658(10) 0.0172(9) -0.0163(9) -0.0358(10) O111 0.22(3) 0.145(15) 0.21(2) 0.094(16) -0.094(18) -0.117(18) O121 0.096(13) 0.46(5) 0.37(4) 0.25(3) -0.11(2) -0.07(2) O131 0.103(9) 0.184(18) 0.055(6) -0.004(8) 0.018(7) -0.049(10) O141 0.58(5) 0.19(2) 0.23(2) -0.051(18) 0.23(3) -0.03(3) O112 0.050(6) 0.182(18) 0.100(8) 0.039(9) 0.023(6) -0.003(8) O122 0.098(9) 0.084(7) 0.052(5) 0.003(5) -0.036(5) -0.036(6) O132 0.213(19) 0.086(9) 0.21(2) 0.093(11) -0.174(17) -0.088(10) O142 0.24(2) 0.139(13) 0.211(17) -0.097(12) 0.089(17) 0.028(14) _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 O5 1.786(3) . ? Fe1 O2 2.024(3) . ? Fe1 O1 2.064(3) . ? Fe1 N1 2.063(4) . ? Fe1 N2 2.096(4) . ? Fe1 O3 2.180(3) . ? Fe2 O5 1.788(3) 7 ? Fe2 O2 2.026(3) . ? Fe2 N4 2.056(4) . ? Fe2 O1 2.070(3) . ? Fe2 N3 2.098(4) . ? Fe2 O4 2.150(3) . ? O1 C13 1.336(5) . ? O2 C5 1.319(5) . ? O3 C20 1.256(5) . ? O4 C20 1.257(5) . ? O5 Fe2 1.788(3) 7 ? N1 C12 1.268(6) . ? N1 C1 1.475(6) . ? N2 C4 1.279(6) . ? N2 C3 1.479(6) . ? N3 C30 1.280(6) . ? N3 C27 1.481(6) . ? N4 C31 1.270(6) . ? N4 C29 1.469(6) . ? C1 C2' 1.38(3) . ? C1 C2 1.516(9) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.466(9) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2' C3 1.51(3) . ? C2' H2C 0.9700 . ? C2' H2D 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C6 1.456(7) . ? C4 H4 0.9300 . ? C5 C6 1.414(6) . ? C5 C10 1.422(6) . ? C6 C7 1.399(6) . ? C7 C8 1.364(7) . ? C7 H7 0.9300 . ? C8 C9 1.370(7) . ? C8 C11 1.520(7) . ? C9 C10 1.395(7) . ? C9 H9 0.9300 . ? C10 C30 1.452(7) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C14 1.449(6) . ? C12 H12 0.9300 . ? C13 C14 1.414(6) . ? C13 C18 1.419(6) . ? C14 C15 1.396(6) . ? C15 C16 1.372(7) . ? C15 H15 0.9300 . ? C16 C17 1.381(7) . ? C16 C19 1.509(7) . ? C17 C18 1.400(6) . ? C17 H17 0.9300 . ? C18 C31 1.459(6) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.506(6) . ? C21 C22 1.381(8) . ? C21 C26 1.387(8) . ? C22 C23 1.426(10) . ? C22 H22 0.9300 . ? C23 C24 1.342(15) . ? C23 H23 0.9300 . ? C24 C25 1.353(15) . ? C24 H24 0.9300 . ? C25 C26 1.383(9) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.469(8) . ? C27 C28' 1.71(4) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.553(9) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28' C29 1.30(5) . ? C28' H28C 0.9700 . ? C28' H28D 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? Cl1 O121 1.315(13) . ? Cl1 O111 1.298(12) . ? Cl1 O131 1.314(11) . ? Cl1 O141 1.322(13) . ? Cl1 O122 1.391(8) . ? Cl1 O132 1.404(10) . ? Cl1 O112 1.423(10) . ? Cl1 O142 1.435(10) . ? 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 O5 Fe1 O2 100.26(12) . . ? O5 Fe1 O1 97.04(13) . . ? O2 Fe1 O1 84.32(11) . . ? O5 Fe1 N1 96.41(14) . . ? O2 Fe1 N1 162.61(13) . . ? O1 Fe1 N1 88.81(13) . . ? O5 Fe1 N2 89.86(15) . . ? O2 Fe1 N2 86.91(14) . . ? O1 Fe1 N2 169.68(14) . . ? N1 Fe1 N2 98.07(16) . . ? O5 Fe1 O3 179.40(14) . . ? O2 Fe1 O3 80.32(12) . . ? O1 Fe1 O3 82.86(11) . . ? N1 Fe1 O3 82.99(14) . . ? N2 Fe1 O3 90.32(14) . . ? O5 Fe2 O2 95.28(13) 7 . ? O5 Fe2 N4 98.43(14) 7 . ? O2 Fe2 N4 165.56(13) . . ? O5 Fe2 O1 97.26(12) 7 . ? O2 Fe2 O1 84.09(11) . . ? N4 Fe2 O1 89.71(14) . . ? O5 Fe2 N3 92.75(14) 7 . ? O2 Fe2 N3 87.15(14) . . ? N4 Fe2 N3 96.63(16) . . ? O1 Fe2 N3 167.25(14) . . ? O5 Fe2 O4 176.25(13) 7 . ? O2 Fe2 O4 81.13(12) . . ? N4 Fe2 O4 85.06(14) . . ? O1 Fe2 O4 81.35(11) . . ? N3 Fe2 O4 88.17(13) . . ? C13 O1 Fe1 126.9(3) . . ? C13 O1 Fe2 125.6(3) . . ? Fe1 O1 Fe2 94.48(12) . . ? C5 O2 Fe1 128.5(3) . . ? C5 O2 Fe2 127.1(3) . . ? Fe1 O2 Fe2 97.06(13) . . ? C20 O3 Fe1 125.7(3) . . ? C20 O4 Fe2 127.9(3) . . ? Fe1 O5 Fe2 161.74(18) . 7 ? C12 N1 C1 117.5(4) . . ? C12 N1 Fe1 124.9(3) . . ? C1 N1 Fe1 117.5(3) . . ? C4 N2 C3 117.0(4) . . ? C4 N2 Fe1 120.7(3) . . ? C3 N2 Fe1 119.2(3) . . ? C30 N3 C27 116.6(4) . . ? C30 N3 Fe2 120.4(3) . . ? C27 N3 Fe2 121.5(4) . . ? C31 N4 C29 117.4(4) . . ? C31 N4 Fe2 124.7(3) . . ? C29 N4 Fe2 117.8(3) . . ? C2' C1 N1 120.6(11) . . ? C2' C1 C2 49.7(15) . . ? N1 C1 C2 110.7(5) . . ? C2' C1 H1A 60.2 . . ? N1 C1 H1A 109.5 . . ? C2 C1 H1A 109.5 . . ? C2' C1 H1B 129.7 . . ? N1 C1 H1B 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? C3 C2 C1 117.9(7) . . ? C3 C2 H2A 107.8 . . ? C1 C2 H2A 107.8 . . ? C3 C2 H2B 107.8 . . ? C1 C2 H2B 107.8 . . ? H2A C2 H2B 107.2 . . ? C1 C2' C3 124(2) . . ? C1 C2' H2C 106.2 . . ? C3 C2' H2C 106.2 . . ? C1 C2' H2D 106.2 . . ? C3 C2' H2D 106.2 . . ? H2C C2' H2D 106.4 . . ? C2 C3 N2 115.7(5) . . ? C2 C3 C2' 48.7(12) . . ? N2 C3 C2' 113.1(11) . . ? C2 C3 H3A 108.4 . . ? N2 C3 H3A 108.4 . . ? C2' C3 H3A 63.4 . . ? C2 C3 H3B 108.4 . . ? N2 C3 H3B 108.4 . . ? C2' C3 H3B 138.4 . . ? H3A C3 H3B 107.4 . . ? N2 C4 C6 128.5(5) . . ? N2 C4 H4 115.7 . . ? C6 C4 H4 115.7 . . ? O2 C5 C6 120.9(4) . . ? O2 C5 C10 121.1(4) . . ? C6 C5 C10 117.9(4) . . ? C7 C6 C5 118.5(5) . . ? C7 C6 C4 117.6(5) . . ? C5 C6 C4 123.7(4) . . ? C8 C7 C6 123.5(5) . . ? C8 C7 H7 118.2 . . ? C6 C7 H7 118.2 . . ? C7 C8 C9 117.6(5) . . ? C7 C8 C11 121.8(6) . . ? C9 C8 C11 120.5(5) . . ? C8 C9 C10 122.3(5) . . ? C8 C9 H9 118.8 . . ? C10 C9 H9 118.8 . . ? C9 C10 C5 119.5(5) . . ? C9 C10 C30 117.0(5) . . ? C5 C10 C30 123.3(4) . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 C14 128.3(4) . . ? N1 C12 H12 115.8 . . ? C14 C12 H12 115.8 . . ? O1 C13 C14 121.5(4) . . ? O1 C13 C18 120.9(4) . . ? C14 C13 C18 117.5(4) . . ? C15 C14 C13 119.9(4) . . ? C15 C14 C12 115.2(4) . . ? C13 C14 C12 124.9(4) . . ? C16 C15 C14 123.4(5) . . ? C16 C15 H15 118.3 . . ? C14 C15 H15 118.3 . . ? C15 C16 C17 116.4(5) . . ? C15 C16 C19 121.8(5) . . ? C17 C16 C19 121.8(5) . . ? C16 C17 C18 123.5(5) . . ? C16 C17 H17 118.3 . . ? C18 C17 H17 118.3 . . ? C17 C18 C13 119.3(4) . . ? C17 C18 C31 114.8(4) . . ? C13 C18 C31 125.8(4) . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O3 C20 O4 127.1(4) . . ? O3 C20 C21 117.4(4) . . ? O4 C20 C21 115.5(4) . . ? C22 C21 C26 120.4(5) . . ? C22 C21 C20 120.6(5) . . ? C26 C21 C20 119.0(5) . . ? C21 C22 C23 116.4(8) . . ? C21 C22 H22 121.8 . . ? C23 C22 H22 121.8 . . ? C24 C23 C22 122.4(10) . . ? C24 C23 H23 118.8 . . ? C22 C23 H23 118.8 . . ? C23 C24 C25 120.3(9) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C26 119.9(10) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C21 C26 C25 120.5(8) . . ? C21 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C28 C27 N3 115.6(5) . . ? C28 C27 C28' 53.3(16) . . ? N3 C27 C28' 104.7(13) . . ? C28 C27 H27A 108.4 . . ? N3 C27 H27A 108.4 . . ? C28' C27 H27A 146.8 . . ? C28 C27 H27B 108.4 . . ? N3 C27 H27B 108.4 . . ? C28' C27 H27B 62.9 . . ? H27A C27 H27B 107.4 . . ? C27 C28 C29 115.8(5) . . ? C27 C28 H28A 108.3 . . ? C29 C28 H28A 108.3 . . ? C27 C28 H28B 108.3 . . ? C29 C28 H28B 108.3 . . ? H28A C28 H28B 107.4 . . ? C29 C28' C27 116(3) . . ? C29 C28' H28C 108.4 . . ? C27 C28' H28C 108.4 . . ? C29 C28' H28D 108.4 . . ? C27 C28' H28D 108.4 . . ? H28C C28' H28D 107.5 . . ? C28' C29 N4 121.9(18) . . ? C28' C29 C28 60.0(17) . . ? N4 C29 C28 108.8(5) . . ? C28' C29 H29A 127.8 . . ? N4 C29 H29A 109.9 . . ? C28 C29 H29A 109.9 . . ? C28' C29 H29B 50.1 . . ? N4 C29 H29B 109.9 . . ? C28 C29 H29B 109.9 . . ? H29A C29 H29B 108.3 . . ? N3 C30 C10 129.0(5) . . ? N3 C30 H30 115.5 . . ? C10 C30 H30 115.5 . . ? N4 C31 C18 127.5(4) . . ? N4 C31 H31 116.2 . . ? C18 C31 H31 116.2 . . ? O121 Cl1 O111 112.9(10) . . ? O121 Cl1 O131 107.2(9) . . ? O111 Cl1 O131 113.0(9) . . ? O121 Cl1 O141 107.1(10) . . ? O111 Cl1 O141 108.8(10) . . ? O131 Cl1 O141 107.5(10) . . ? O121 Cl1 O122 48.3(14) . . ? O111 Cl1 O122 126.3(10) . . ? O131 Cl1 O122 120.6(9) . . ? O141 Cl1 O122 58.9(15) . . ? O121 Cl1 O132 120.9(12) . . ? O111 Cl1 O132 119.1(11) . . ? O131 Cl1 O132 26.6(11) . . ? O141 Cl1 O132 81.2(12) . . ? O122 Cl1 O132 110.5(7) . . ? O121 Cl1 O112 128.2(11) . . ? O111 Cl1 O112 35.0(11) . . ? O131 Cl1 O112 122.1(10) . . ? O141 Cl1 O112 74.0(12) . . ? O122 Cl1 O112 109.3(7) . . ? O132 Cl1 O112 110.6(8) . . ? O121 Cl1 O142 62.1(14) . . ? O111 Cl1 O142 71.4(11) . . ? O131 Cl1 O142 83.9(10) . . ? O141 Cl1 O142 166.8(14) . . ? O122 Cl1 O142 109.9(8) . . ? O132 Cl1 O142 110.5(8) . . ? O112 Cl1 O142 106.0(7) . . ? 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 O5 Fe1 O1 C13 120.0(3) . . . . ? O2 Fe1 O1 C13 -140.3(3) . . . . ? N1 Fe1 O1 C13 23.7(3) . . . . ? N2 Fe1 O1 C13 -108.3(8) . . . . ? O3 Fe1 O1 C13 -59.4(3) . . . . ? O5 Fe1 O1 Fe2 -97.97(13) . . . . ? O2 Fe1 O1 Fe2 1.71(11) . . . . ? N1 Fe1 O1 Fe2 165.72(14) . . . . ? N2 Fe1 O1 Fe2 33.7(8) . . . . ? O3 Fe1 O1 Fe2 82.63(12) . . . . ? O5 Fe2 O1 C13 -124.4(3) 7 . . . ? O2 Fe2 O1 C13 141.0(3) . . . . ? N4 Fe2 O1 C13 -25.9(3) . . . . ? N3 Fe2 O1 C13 94.2(7) . . . . ? O4 Fe2 O1 C13 59.1(3) . . . . ? O5 Fe2 O1 Fe1 92.89(13) 7 . . . ? O2 Fe2 O1 Fe1 -1.71(11) . . . . ? N4 Fe2 O1 Fe1 -168.65(13) . . . . ? N3 Fe2 O1 Fe1 -48.6(6) . . . . ? O4 Fe2 O1 Fe1 -83.60(12) . . . . ? O5 Fe1 O2 C5 -56.6(4) . . . . ? O1 Fe1 O2 C5 -152.7(3) . . . . ? N1 Fe1 O2 C5 140.1(5) . . . . ? N2 Fe1 O2 C5 32.7(3) . . . . ? O3 Fe1 O2 C5 123.6(4) . . . . ? O5 Fe1 O2 Fe2 94.40(14) . . . . ? O1 Fe1 O2 Fe2 -1.75(11) . . . . ? N1 Fe1 O2 Fe2 -68.9(5) . . . . ? N2 Fe1 O2 Fe2 -176.30(14) . . . . ? O3 Fe1 O2 Fe2 -85.45(13) . . . . ? O5 Fe2 O2 C5 56.6(3) 7 . . . ? N4 Fe2 O2 C5 -141.7(6) . . . . ? O1 Fe2 O2 C5 153.3(3) . . . . ? N3 Fe2 O2 C5 -36.0(3) . . . . ? O4 Fe2 O2 C5 -124.5(3) . . . . ? O5 Fe2 O2 Fe1 -95.02(13) 7 . . . ? N4 Fe2 O2 Fe1 66.8(6) . . . . ? O1 Fe2 O2 Fe1 1.75(11) . . . . ? N3 Fe2 O2 Fe1 172.47(14) . . . . ? O4 Fe2 O2 Fe1 83.88(12) . . . . ? O5 Fe1 O3 C20 -120(13) . . . . ? O2 Fe1 O3 C20 46.4(4) . . . . ? O1 Fe1 O3 C20 -39.1(4) . . . . ? N1 Fe1 O3 C20 -128.7(4) . . . . ? N2 Fe1 O3 C20 133.2(4) . . . . ? O5 Fe2 O4 C20 -25(2) 7 . . . ? O2 Fe2 O4 C20 -41.6(4) . . . . ? N4 Fe2 O4 C20 134.2(4) . . . . ? O1 Fe2 O4 C20 43.7(4) . . . . ? N3 Fe2 O4 C20 -129.0(4) . . . . ? O2 Fe1 O5 Fe2 -30.0(7) . . . 7 ? O1 Fe1 O5 Fe2 55.5(7) . . . 7 ? N1 Fe1 O5 Fe2 145.1(6) . . . 7 ? N2 Fe1 O5 Fe2 -116.8(6) . . . 7 ? O3 Fe1 O5 Fe2 136(13) . . . 7 ? O5 Fe1 N1 C12 -107.6(4) . . . . ? O2 Fe1 N1 C12 55.9(7) . . . . ? O1 Fe1 N1 C12 -10.6(4) . . . . ? N2 Fe1 N1 C12 161.7(4) . . . . ? O3 Fe1 N1 C12 72.3(4) . . . . ? O5 Fe1 N1 C1 73.3(4) . . . . ? O2 Fe1 N1 C1 -123.2(5) . . . . ? O1 Fe1 N1 C1 170.2(4) . . . . ? N2 Fe1 N1 C1 -17.5(4) . . . . ? O3 Fe1 N1 C1 -106.8(4) . . . . ? O5 Fe1 N2 C4 69.5(4) . . . . ? O2 Fe1 N2 C4 -30.8(4) . . . . ? O1 Fe1 N2 C4 -62.6(9) . . . . ? N1 Fe1 N2 C4 165.9(4) . . . . ? O3 Fe1 N2 C4 -111.1(4) . . . . ? O5 Fe1 N2 C3 -89.8(4) . . . . ? O2 Fe1 N2 C3 169.9(4) . . . . ? O1 Fe1 N2 C3 138.1(7) . . . . ? N1 Fe1 N2 C3 6.7(4) . . . . ? O3 Fe1 N2 C3 89.6(4) . . . . ? O5 Fe2 N3 C30 -65.1(4) 7 . . . ? O2 Fe2 N3 C30 30.1(4) . . . . ? N4 Fe2 N3 C30 -163.9(4) . . . . ? O1 Fe2 N3 C30 76.7(7) . . . . ? O4 Fe2 N3 C30 111.3(4) . . . . ? O5 Fe2 N3 C27 100.8(4) 7 . . . ? O2 Fe2 N3 C27 -164.0(4) . . . . ? N4 Fe2 N3 C27 2.0(4) . . . . ? O1 Fe2 N3 C27 -117.4(7) . . . . ? O4 Fe2 N3 C27 -82.8(4) . . . . ? O5 Fe2 N4 C31 107.9(4) 7 . . . ? O2 Fe2 N4 C31 -53.8(8) . . . . ? O1 Fe2 N4 C31 10.6(4) . . . . ? N3 Fe2 N4 C31 -158.3(4) . . . . ? O4 Fe2 N4 C31 -70.8(4) . . . . ? O5 Fe2 N4 C29 -77.3(4) 7 . . . ? O2 Fe2 N4 C29 121.0(6) . . . . ? O1 Fe2 N4 C29 -174.6(4) . . . . ? N3 Fe2 N4 C29 16.5(4) . . . . ? O4 Fe2 N4 C29 104.1(4) . . . . ? C12 N1 C1 C2' 174.1(19) . . . . ? Fe1 N1 C1 C2' -7(2) . . . . ? C12 N1 C1 C2 -131.3(6) . . . . ? Fe1 N1 C1 C2 47.9(6) . . . . ? C2' C1 C2 C3 35.1(14) . . . . ? N1 C1 C2 C3 -78.1(8) . . . . ? N1 C1 C2' C3 55(3) . . . . ? C2 C1 C2' C3 -36.9(19) . . . . ? C1 C2 C3 N2 66.5(9) . . . . ? C1 C2 C3 C2' -32.5(14) . . . . ? C4 N2 C3 C2 172.0(6) . . . . ? Fe1 N2 C3 C2 -28.0(8) . . . . ? C4 N2 C3 C2' -134.3(14) . . . . ? Fe1 N2 C3 C2' 25.7(15) . . . . ? C1 C2' C3 C2 39.1(19) . . . . ? C1 C2' C3 N2 -66(3) . . . . ? C3 N2 C4 C6 178.6(5) . . . . ? Fe1 N2 C4 C6 18.9(7) . . . . ? Fe1 O2 C5 C6 -18.5(6) . . . . ? Fe2 O2 C5 C6 -161.4(3) . . . . ? Fe1 O2 C5 C10 165.4(3) . . . . ? Fe2 O2 C5 C10 22.5(6) . . . . ? O2 C5 C6 C7 176.3(4) . . . . ? C10 C5 C6 C7 -7.5(6) . . . . ? O2 C5 C6 C4 -9.0(7) . . . . ? C10 C5 C6 C4 167.1(4) . . . . ? N2 C4 C6 C7 -177.6(5) . . . . ? N2 C4 C6 C5 7.7(8) . . . . ? C5 C6 C7 C8 2.3(7) . . . . ? C4 C6 C7 C8 -172.7(5) . . . . ? C6 C7 C8 C9 4.7(8) . . . . ? C6 C7 C8 C11 -178.5(5) . . . . ? C7 C8 C9 C10 -6.4(8) . . . . ? C11 C8 C9 C10 176.8(5) . . . . ? C8 C9 C10 C5 1.1(8) . . . . ? C8 C9 C10 C30 175.0(5) . . . . ? O2 C5 C10 C9 -177.9(4) . . . . ? C6 C5 C10 C9 6.0(7) . . . . ? O2 C5 C10 C30 8.6(7) . . . . ? C6 C5 C10 C30 -167.5(4) . . . . ? C1 N1 C12 C14 177.5(5) . . . . ? Fe1 N1 C12 C14 -1.7(7) . . . . ? Fe1 O1 C13 C14 -24.2(5) . . . . ? Fe2 O1 C13 C14 -155.2(3) . . . . ? Fe1 O1 C13 C18 158.6(3) . . . . ? Fe2 O1 C13 C18 27.6(5) . . . . ? O1 C13 C14 C15 -176.5(4) . . . . ? C18 C13 C14 C15 0.7(6) . . . . ? O1 C13 C14 C12 5.3(7) . . . . ? C18 C13 C14 C12 -177.5(4) . . . . ? N1 C12 C14 C15 -169.6(5) . . . . ? N1 C12 C14 C13 8.7(8) . . . . ? C13 C14 C15 C16 0.6(7) . . . . ? C12 C14 C15 C16 179.0(5) . . . . ? C14 C15 C16 C17 -1.4(8) . . . . ? C14 C15 C16 C19 -179.1(5) . . . . ? C15 C16 C17 C18 0.8(8) . . . . ? C19 C16 C17 C18 178.6(5) . . . . ? C16 C17 C18 C13 0.5(7) . . . . ? C16 C17 C18 C31 -176.0(5) . . . . ? O1 C13 C18 C17 176.0(4) . . . . ? C14 C13 C18 C17 -1.2(6) . . . . ? O1 C13 C18 C31 -7.9(7) . . . . ? C14 C13 C18 C31 174.8(4) . . . . ? Fe1 O3 C20 O4 -5.6(7) . . . . ? Fe1 O3 C20 C21 174.1(3) . . . . ? Fe2 O4 C20 O3 2.8(7) . . . . ? Fe2 O4 C20 C21 -176.9(3) . . . . ? O3 C20 C21 C22 30.8(7) . . . . ? O4 C20 C21 C22 -149.4(5) . . . . ? O3 C20 C21 C26 -149.7(5) . . . . ? O4 C20 C21 C26 30.1(6) . . . . ? C26 C21 C22 C23 -0.8(7) . . . . ? C20 C21 C22 C23 178.8(5) . . . . ? C21 C22 C23 C24 0.7(10) . . . . ? C22 C23 C24 C25 0.1(15) . . . . ? C23 C24 C25 C26 -0.8(14) . . . . ? C22 C21 C26 C25 0.1(8) . . . . ? C20 C21 C26 C25 -179.4(5) . . . . ? C24 C25 C26 C21 0.7(11) . . . . ? C30 N3 C27 C28 -175.1(6) . . . . ? Fe2 N3 C27 C28 18.5(7) . . . . ? C30 N3 C27 C28' 128.9(16) . . . . ? Fe2 N3 C27 C28' -37.5(17) . . . . ? N3 C27 C28 C29 -61.9(8) . . . . ? C28' C27 C28 C29 27.7(16) . . . . ? C28 C27 C28' C29 -34(2) . . . . ? N3 C27 C28' C29 78(3) . . . . ? C27 C28' C29 N4 -66(3) . . . . ? C27 C28' C29 C28 29.0(16) . . . . ? C31 N4 C29 C28' -171(2) . . . . ? Fe2 N4 C29 C28' 13(2) . . . . ? C31 N4 C29 C28 122.8(5) . . . . ? Fe2 N4 C29 C28 -52.5(5) . . . . ? C27 C28 C29 C28' -35(2) . . . . ? C27 C28 C29 N4 82.1(6) . . . . ? C27 N3 C30 C10 179.0(5) . . . . ? Fe2 N3 C30 C10 -14.4(7) . . . . ? C9 C10 C30 N3 174.2(5) . . . . ? C5 C10 C30 N3 -12.1(8) . . . . ? C29 N4 C31 C18 -172.1(5) . . . . ? Fe2 N4 C31 C18 2.7(7) . . . . ? C17 C18 C31 N4 167.5(5) . . . . ? C13 C18 C31 N4 -8.7(8) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.317 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.069