Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'David Richens' _publ_contact_author_address ; School of Chemistry University of St Andrews North Haugh St Andrews Fife KY16 9ST UNITED KINGDOM ; _publ_contact_author_email DTR@ST-ANDREWS.AC.UK _publ_section_title ; High Spin d5 Complexes of Tris(6-hydroxymethyl-2-pyridylmethyl)amine (H3L): Hepta-coordinated [Mn(H3L)]Cl2 and [Fe3L2](ClO4)3; an Unusual Weakly Antiferromagnetically-Coupled Alkoxide-Bridged Linear Triiron(III) Complex with a Tight Fe-O-Fe Angle ; loop_ _publ_author_name 'D. Richens' 'Euan Brechin' 'Ian A. Gass' 'Gregorio Guisado-Barrios' 'Yang Li.' ; P.R.Murray ; 'A. Slawin' 'Lesley Yellowlees' data_Mn _database_code_depnum_ccdc_archive 'CCDC 663306' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H30 Cl2 Mn N4 O6' _chemical_formula_weight 560.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 13.0657(18) _cell_length_b 13.0657(18) _cell_length_c 54.299(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 8028(2) _cell_formula_units_Z 12 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 7046 _cell_measurement_theta_min 1.89 _cell_measurement_theta_max 27.62 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.391 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3492 _exptl_absorpt_coefficient_mu 0.734 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.860 _exptl_absorpt_correction_T_max 0.929 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type ? _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13439 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0218 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -65 _diffrn_reflns_limit_l_max 57 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 25.31 _reflns_number_total 1566 _reflns_number_gt 1266 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _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. A twin instruction was utilsed, as the crystals were poor quality. Dfix constraints are used for the hydroxyl groups. ; _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^)+(0.1017P)^2^+97.4248P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1566 _refine_ls_number_parameters 119 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0934 _refine_ls_R_factor_gt 0.0781 _refine_ls_wR_factor_ref 0.2079 _refine_ls_wR_factor_gt 0.1930 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.6667 0.3333 0.194190(19) 0.0248(4) Uani 1 3 d S . . N1 N 0.6667 0.3333 0.14926(12) 0.0259(14) Uani 1 3 d S . . C2 C 0.5425(4) 0.2712(4) 0.14085(8) 0.0324(11) Uani 1 1 d . . . H2A H 0.5093 0.1847 0.1423 0.039 Uiso 1 1 calc R . . H2B H 0.5387 0.2901 0.1233 0.039 Uiso 1 1 calc R . . C3 C 0.4712(4) 0.3086(4) 0.15630(8) 0.0300(10) Uani 1 1 d . . . N4 N 0.5031(3) 0.3326(3) 0.17992(7) 0.0278(9) Uani 1 1 d . . . C5 C 0.4440(4) 0.3669(4) 0.19486(9) 0.0342(11) Uani 1 1 d . . . C6 C 0.3486(4) 0.3767(5) 0.18633(11) 0.0436(13) Uani 1 1 d . . . H6A H 0.3063 0.3996 0.1971 0.052 Uiso 1 1 calc R . . C7 C 0.3172(4) 0.3526(5) 0.16218(11) 0.0470(14) Uani 1 1 d . . . H7A H 0.2530 0.3596 0.1560 0.056 Uiso 1 1 calc R . . C8 C 0.3781(4) 0.3181(5) 0.14656(10) 0.0394(12) Uani 1 1 d . . . H8A H 0.3568 0.3015 0.1297 0.047 Uiso 1 1 calc R . . C9 C 0.4876(5) 0.3965(5) 0.22090(9) 0.0407(12) Uani 1 1 d . . . H9A H 0.4828 0.4659 0.2266 0.049 Uiso 1 1 calc R . . H9B H 0.4382 0.3290 0.2319 0.049 Uiso 1 1 calc R . . O9 O 0.6067(3) 0.4219(3) 0.22156(6) 0.0405(9) Uani 1 1 d D . . H9O H 0.620(11) 0.457(10) 0.2380(9) 0.14(4) Uiso 1 1 d D . . Cl1 Cl 0.8767(3) 0.7379(3) 0.25712(5) 0.0471(7) Uani 0.50 1 d P . . Cl2 Cl 0.6667 0.3333 0.30833(18) 0.084(2) Uani 0.50 3 d SP . . O21 O 0.6825(4) 0.5024(5) 0.26927(9) 0.0713(15) Uani 1 1 d D . . H21A H 0.687(8) 0.446(6) 0.2806(12) 0.086 Uiso 1 1 d D . . H21B H 0.746(5) 0.582(3) 0.2652(15) 0.086 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0279(5) 0.0279(5) 0.0185(6) 0.000 0.000 0.0140(2) N1 0.023(2) 0.023(2) 0.032(3) 0.000 0.000 0.0115(10) C2 0.034(3) 0.037(3) 0.025(2) -0.002(2) -0.0083(19) 0.017(2) C3 0.027(2) 0.023(2) 0.031(2) 0.0074(18) 0.0008(19) 0.0061(18) N4 0.0257(19) 0.0252(19) 0.030(2) 0.0064(15) 0.0050(15) 0.0113(16) C5 0.033(3) 0.027(2) 0.041(3) 0.010(2) 0.013(2) 0.014(2) C6 0.025(2) 0.038(3) 0.065(4) 0.013(3) 0.017(2) 0.014(2) C7 0.020(2) 0.047(3) 0.071(4) 0.008(3) -0.004(2) 0.014(2) C8 0.024(2) 0.039(3) 0.046(3) 0.009(2) -0.006(2) 0.008(2) C9 0.049(3) 0.044(3) 0.037(3) 0.005(2) 0.015(2) 0.029(3) O9 0.044(2) 0.049(2) 0.0303(17) -0.0070(16) 0.0042(15) 0.0247(18) Cl1 0.0661(18) 0.0510(16) 0.0318(12) -0.0016(11) 0.0008(12) 0.0351(14) Cl2 0.067(3) 0.067(3) 0.117(6) 0.000 0.000 0.0335(13) O21 0.061(3) 0.069(3) 0.072(3) -0.026(2) 0.031(3) 0.023(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O9 2.251(4) 3_665 ? Mn1 O9 2.251(4) 2_655 ? Mn1 O9 2.251(4) . ? Mn1 N4 2.269(4) 2_655 ? Mn1 N4 2.269(4) . ? Mn1 N4 2.269(4) 3_665 ? Mn1 N1 2.440(7) . ? N1 C2 1.477(5) 2_655 ? N1 C2 1.477(5) . ? N1 C2 1.477(5) 3_665 ? C2 C3 1.506(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N4 1.337(6) . ? C3 C8 1.388(7) . ? N4 C5 1.342(6) . ? C5 C6 1.395(8) . ? C5 C9 1.501(7) . ? C6 C7 1.363(9) . ? C6 H6A 0.9500 . ? C7 C8 1.383(8) . ? C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? C9 O9 1.420(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? O9 H9O 0.980(5) . ? O21 H21A 0.979(5) . ? O21 H21B 0.980(5) . ? 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 O9 Mn1 O9 81.15(15) 3_665 2_655 ? O9 Mn1 O9 81.15(15) 3_665 . ? O9 Mn1 O9 81.15(15) 2_655 . ? O9 Mn1 N4 98.34(13) 3_665 2_655 ? O9 Mn1 N4 70.04(13) 2_655 2_655 ? O9 Mn1 N4 150.83(14) . 2_655 ? O9 Mn1 N4 150.82(14) 3_665 . ? O9 Mn1 N4 98.33(13) 2_655 . ? O9 Mn1 N4 70.03(13) . . ? N4 Mn1 N4 108.96(10) 2_655 . ? O9 Mn1 N4 70.04(13) 3_665 3_665 ? O9 Mn1 N4 150.83(14) 2_655 3_665 ? O9 Mn1 N4 98.34(13) . 3_665 ? N4 Mn1 N4 108.96(10) 2_655 3_665 ? N4 Mn1 N4 108.96(10) . 3_665 ? O9 Mn1 N1 131.32(10) 3_665 . ? O9 Mn1 N1 131.32(10) 2_655 . ? O9 Mn1 N1 131.32(10) . . ? N4 Mn1 N1 70.02(9) 2_655 . ? N4 Mn1 N1 70.03(9) . . ? N4 Mn1 N1 70.02(9) 3_665 . ? C2 N1 C2 110.9(3) 2_655 . ? C2 N1 C2 110.9(3) 2_655 3_665 ? C2 N1 C2 110.9(3) . 3_665 ? C2 N1 Mn1 108.0(3) 2_655 . ? C2 N1 Mn1 108.0(3) . . ? C2 N1 Mn1 108.0(3) 3_665 . ? N1 C2 C3 109.7(4) . . ? N1 C2 H2A 109.7 . . ? C3 C2 H2A 109.7 . . ? N1 C2 H2B 109.7 . . ? C3 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? N4 C3 C8 122.0(5) . . ? N4 C3 C2 116.1(4) . . ? C8 C3 C2 122.0(4) . . ? C3 N4 C5 119.6(4) . . ? C3 N4 Mn1 120.8(3) . . ? C5 N4 Mn1 119.3(3) . . ? N4 C5 C6 121.3(5) . . ? N4 C5 C9 116.6(4) . . ? C6 C5 C9 122.0(5) . . ? C7 C6 C5 118.5(5) . . ? C7 C6 H6A 120.7 . . ? C5 C6 H6A 120.7 . . ? C6 C7 C8 120.7(5) . . ? C6 C7 H7A 119.7 . . ? C8 C7 H7A 119.7 . . ? C7 C8 C3 117.9(5) . . ? C7 C8 H8A 121.0 . . ? C3 C8 H8A 121.0 . . ? O9 C9 C5 108.3(4) . . ? O9 C9 H9A 110.0 . . ? C5 C9 H9A 110.0 . . ? O9 C9 H9B 110.0 . . ? C5 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? C9 O9 Mn1 119.1(3) . . ? C9 O9 H9O 93(8) . . ? Mn1 O9 H9O 145(8) . . ? H21A O21 H21B 128(8) . . ? 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 O9 Mn1 N1 C2 53.6(2) 3_665 . . 2_655 ? O9 Mn1 N1 C2 -66.4(2) 2_655 . . 2_655 ? O9 Mn1 N1 C2 173.6(2) . . . 2_655 ? N4 Mn1 N1 C2 -29.8(2) 2_655 . . 2_655 ? N4 Mn1 N1 C2 -149.8(2) . . . 2_655 ? N4 Mn1 N1 C2 90.2(2) 3_665 . . 2_655 ? O9 Mn1 N1 C2 173.6(2) 3_665 . . . ? O9 Mn1 N1 C2 53.6(2) 2_655 . . . ? O9 Mn1 N1 C2 -66.4(2) . . . . ? N4 Mn1 N1 C2 90.2(2) 2_655 . . . ? N4 Mn1 N1 C2 -29.8(2) . . . . ? N4 Mn1 N1 C2 -149.8(2) 3_665 . . . ? O9 Mn1 N1 C2 -66.4(2) 3_665 . . 3_665 ? O9 Mn1 N1 C2 173.6(2) 2_655 . . 3_665 ? O9 Mn1 N1 C2 53.6(2) . . . 3_665 ? N4 Mn1 N1 C2 -149.8(2) 2_655 . . 3_665 ? N4 Mn1 N1 C2 90.2(2) . . . 3_665 ? N4 Mn1 N1 C2 -29.8(2) 3_665 . . 3_665 ? C2 N1 C2 C3 160.6(4) 2_655 . . . ? C2 N1 C2 C3 -75.8(6) 3_665 . . . ? Mn1 N1 C2 C3 42.4(4) . . . . ? N1 C2 C3 N4 -33.9(5) . . . . ? N1 C2 C3 C8 145.8(4) . . . . ? C8 C3 N4 C5 0.0(7) . . . . ? C2 C3 N4 C5 179.8(4) . . . . ? C8 C3 N4 Mn1 -174.0(3) . . . . ? C2 C3 N4 Mn1 5.8(5) . . . . ? O9 Mn1 N4 C3 155.8(3) 3_665 . . . ? O9 Mn1 N4 C3 -117.4(3) 2_655 . . . ? O9 Mn1 N4 C3 165.2(4) . . . . ? N4 Mn1 N4 C3 -45.8(3) 2_655 . . . ? N4 Mn1 N4 C3 73.0(3) 3_665 . . . ? N1 Mn1 N4 C3 13.6(3) . . . . ? O9 Mn1 N4 C5 -18.2(5) 3_665 . . . ? O9 Mn1 N4 C5 68.5(3) 2_655 . . . ? O9 Mn1 N4 C5 -8.8(3) . . . . ? N4 Mn1 N4 C5 140.2(3) 2_655 . . . ? N4 Mn1 N4 C5 -101.0(4) 3_665 . . . ? N1 Mn1 N4 C5 -160.4(3) . . . . ? C3 N4 C5 C6 0.9(7) . . . . ? Mn1 N4 C5 C6 174.9(4) . . . . ? C3 N4 C5 C9 -177.8(4) . . . . ? Mn1 N4 C5 C9 -3.8(5) . . . . ? N4 C5 C6 C7 -1.2(7) . . . . ? C9 C5 C6 C7 177.4(5) . . . . ? C5 C6 C7 C8 0.6(8) . . . . ? C6 C7 C8 C3 0.2(8) . . . . ? N4 C3 C8 C7 -0.6(7) . . . . ? C2 C3 C8 C7 179.7(5) . . . . ? N4 C5 C9 O9 20.7(6) . . . . ? C6 C5 C9 O9 -158.0(4) . . . . ? C5 C9 O9 Mn1 -29.5(5) . . . . ? O9 Mn1 O9 C9 -163.0(4) 3_665 . . . ? O9 Mn1 O9 C9 -80.7(4) 2_655 . . . ? N4 Mn1 O9 C9 -71.7(5) 2_655 . . . ? N4 Mn1 O9 C9 21.6(3) . . . . ? N4 Mn1 O9 C9 128.8(3) 3_665 . . . ? N1 Mn1 O9 C9 58.2(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 O9 H9O O21 0.980(5) 1.85(5) 2.785(6) 159(11) . O21 H21B Cl1 0.980(5) 1.943(10) 2.922(6) 177(8) . O21 H21A Cl2 0.979(5) 2.03(2) 2.993(9) 167(8) . _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.561 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.113 # Attachment 'Richens_et_al_2.cif' data_Fe _database_code_depnum_ccdc_archive 'CCDC 663307' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H48 Cl3 Fe3 N10 O18' _chemical_formula_weight 1302.84 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.4533(19) _cell_length_b 20.826(3) _cell_length_c 11.5573(19) _cell_angle_alpha 90.00 _cell_angle_beta 108.114(4) _cell_angle_gamma 90.00 _cell_volume 2620.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 8082 _cell_measurement_theta_min 1.9556 _cell_measurement_theta_max 28.4925 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.1500 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.651 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1334 _exptl_absorpt_coefficient_mu 1.057 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8640 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type ? _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16517 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0792 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.33 _reflns_number_total 4700 _reflns_number_gt 3629 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _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^)+(0.1100P)^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 4700 _refine_ls_number_parameters 383 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0766 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1701 _refine_ls_wR_factor_gt 0.1469 _refine_ls_goodness_of_fit_ref 0.932 _refine_ls_restrained_S_all 0.932 _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 0.13273(4) 0.94588(2) 0.85386(4) 0.0212(2) Uani 1 1 d . . . Fe2 Fe 0.0000 1.0000 1.0000 0.0232(2) Uani 1 2 d S . . N1 N 0.2467(3) 0.90103(14) 0.7340(3) 0.0259(7) Uani 1 1 d . . . C2 C 0.3769(3) 0.92174(18) 0.7863(4) 0.0319(9) Uani 1 1 d . . . H2A H 0.3872 0.9655 0.7576 0.038 Uiso 1 1 calc R . . H2B H 0.4312 0.8923 0.7594 0.038 Uiso 1 1 calc R . . C3 C 0.4106(3) 0.92106(16) 0.9220(4) 0.0310(9) Uani 1 1 d . . . N4 N 0.3152(3) 0.92607(13) 0.9672(3) 0.0282(7) Uani 1 1 d . . . C5 C 0.3351(3) 0.92256(16) 1.0881(4) 0.0284(9) Uani 1 1 d . . . C6 C 0.4540(4) 0.91764(17) 1.1697(4) 0.0390(11) Uani 1 1 d . . . H6A H 0.4678 0.9166 1.2551 0.047 Uiso 1 1 calc R . . C7 C 0.5511(4) 0.91428(18) 1.1223(4) 0.0416(12) Uani 1 1 d . . . H7A H 0.6329 0.9111 1.1757 0.050 Uiso 1 1 calc R . . C8 C 0.5299(4) 0.91556(18) 0.9993(4) 0.0394(11) Uani 1 1 d . . . H8A H 0.5965 0.9127 0.9670 0.047 Uiso 1 1 calc R . . O9 O 0.1153(2) 0.92604(11) 1.0242(2) 0.0246(6) Uani 1 1 d . . . C9 C 0.2216(4) 0.92130(18) 1.1265(3) 0.0329(9) Uani 1 1 d . . . H9A H 0.2190 0.8808 1.1705 0.040 Uiso 1 1 calc R . . H9B H 0.2237 0.9575 1.1826 0.040 Uiso 1 1 calc R . . C12 C 0.2339(3) 0.83060(17) 0.7411(4) 0.0290(9) Uani 1 1 d . . . H12A H 0.2878 0.8145 0.8204 0.035 Uiso 1 1 calc R . . H12B H 0.2583 0.8095 0.6755 0.035 Uiso 1 1 calc R . . C13 C 0.1024(3) 0.81551(15) 0.7279(3) 0.0222(8) Uani 1 1 d . . . N14 N 0.0429(3) 0.86132(13) 0.7699(3) 0.0223(6) Uani 1 1 d . . . C15 C -0.0749(3) 0.85194(16) 0.7646(3) 0.0218(8) Uani 1 1 d . . . C16 C -0.1367(3) 0.79598(17) 0.7183(3) 0.0257(8) Uani 1 1 d . . . H16A H -0.2193 0.7897 0.7169 0.031 Uiso 1 1 calc R . . C17 C -0.0760(4) 0.74933(17) 0.6742(4) 0.0286(9) Uani 1 1 d . . . H17A H -0.1168 0.7106 0.6412 0.034 Uiso 1 1 calc R . . C18 C 0.0450(4) 0.75952(17) 0.6786(3) 0.0277(9) Uani 1 1 d . . . H18A H 0.0877 0.7281 0.6479 0.033 Uiso 1 1 calc R . . O19 O -0.0538(2) 0.96137(11) 0.8328(2) 0.0231(6) Uani 1 1 d . . . C19 C -0.1345(3) 0.90773(17) 0.8078(3) 0.0258(8) Uani 1 1 d . . . H19A H -0.2121 0.9193 0.7444 0.031 Uiso 1 1 calc R . . H19B H -0.1542 0.8954 0.8823 0.031 Uiso 1 1 calc R . . C22 C 0.1927(4) 0.92515(18) 0.6082(3) 0.0315(9) Uani 1 1 d . . . H22A H 0.1163 0.9014 0.5665 0.038 Uiso 1 1 calc R . . H22B H 0.2513 0.9191 0.5616 0.038 Uiso 1 1 calc R . . C23 C 0.1652(4) 0.99580(17) 0.6158(4) 0.0286(9) Uani 1 1 d . . . N24 N 0.1398(3) 1.01396(13) 0.7169(3) 0.0248(7) Uani 1 1 d . . . C25 C 0.1183(3) 1.07636(17) 0.7354(3) 0.0270(8) Uani 1 1 d . . . C26 C 0.1212(4) 1.12297(18) 0.6491(4) 0.0330(9) Uani 1 1 d . . . H26A H 0.1062 1.1668 0.6621 0.040 Uiso 1 1 calc R . . C27 C 0.1460(4) 1.1042(2) 0.5455(4) 0.0402(10) Uani 1 1 d . . . H27A H 0.1482 1.1354 0.4863 0.048 Uiso 1 1 calc R . . C28 C 0.1681(4) 1.0400(2) 0.5261(4) 0.0400(10) Uani 1 1 d . . . H28A H 0.1846 1.0267 0.4541 0.048 Uiso 1 1 calc R . . O29 O 0.1269(2) 1.03673(11) 0.9311(2) 0.0249(6) Uani 1 1 d . . . C29 C 0.0995(4) 1.09126(17) 0.8542(4) 0.0302(9) Uani 1 1 d . . . H29A H 0.1534 1.1274 0.8936 0.036 Uiso 1 1 calc R . . H29B H 0.0132 1.1044 0.8407 0.036 Uiso 1 1 calc R . . Cl1 Cl 0.61684(9) 0.76801(5) 0.87902(9) 0.0347(3) Uani 1 1 d . . . O31 O 0.7076(3) 0.77960(16) 0.9956(3) 0.0518(8) Uani 1 1 d . . . O32 O 0.6422(3) 0.71140(15) 0.8255(4) 0.0635(10) Uani 1 1 d . . . O33 O 0.4966(3) 0.76647(13) 0.8923(3) 0.0435(8) Uani 1 1 d . . . O34 O 0.6211(3) 0.82265(15) 0.8015(3) 0.0570(9) Uani 1 1 d . . . Cl2A Cl 0.5000 1.0000 0.5000 0.0500(5) Uani 0.50 2 d SP . 1 O35 O 0.5420(7) 1.0253(3) 0.4186(6) 0.0514(17) Uani 0.50 1 d P . 1 O36 O 0.4291(6) 1.0527(4) 0.5508(6) 0.063(2) Uani 0.50 1 d P . 1 Cl2B Cl 0.5000 1.0000 0.5000 0.0500(5) Uani 0.50 2 d SP . 2 O37 O 0.6104(7) 1.0428(4) 0.5554(7) 0.065(2) Uani 0.50 1 d P . 2 O38 O 0.4225(9) 1.0283(5) 0.3931(7) 0.089(3) Uani 0.50 1 d P . 2 C31 C 0.0704(5) 0.7358(3) 0.9976(5) 0.0581(14) Uani 1 1 d . . . N31 N 0.1539(5) 0.7645(3) 0.9883(5) 0.0887(19) Uani 1 1 d . . . C30 C -0.0316(5) 0.7018(3) 1.0128(5) 0.0627(14) Uani 1 1 d . . . H30A H -0.0109 0.6561 1.0259 0.094 Uiso 1 1 calc R . . H30B H -0.1027 0.7068 0.9397 0.094 Uiso 1 1 calc R . . H30C H -0.0515 0.7189 1.0834 0.094 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 0.0229(3) 0.0167(3) 0.0238(3) -0.00286(19) 0.0072(2) -0.00068(19) Fe2 0.0266(4) 0.0205(4) 0.0226(4) -0.0043(3) 0.0077(3) 0.0011(3) N1 0.0247(16) 0.0192(15) 0.0350(17) -0.0062(13) 0.0110(14) -0.0024(12) C2 0.025(2) 0.0262(19) 0.048(2) -0.0115(18) 0.0172(18) -0.0050(16) C3 0.027(2) 0.0113(16) 0.054(2) -0.0098(17) 0.0118(18) -0.0019(15) N4 0.0267(16) 0.0142(14) 0.0396(19) -0.0036(13) 0.0045(15) -0.0009(13) C5 0.033(2) 0.0139(17) 0.034(2) -0.0040(15) 0.0034(17) 0.0026(15) C6 0.041(2) 0.0162(18) 0.045(2) -0.0054(17) -0.008(2) 0.0015(17) C7 0.027(2) 0.0204(19) 0.063(3) -0.0094(19) -0.007(2) 0.0018(17) C8 0.027(2) 0.0208(19) 0.068(3) -0.0090(19) 0.012(2) -0.0007(17) O9 0.0246(13) 0.0236(13) 0.0237(13) -0.0025(10) 0.0048(11) 0.0024(10) C9 0.040(2) 0.0268(19) 0.0258(19) -0.0035(16) 0.0008(18) 0.0085(18) C12 0.0287(19) 0.0214(18) 0.041(2) -0.0078(16) 0.0163(17) -0.0034(15) C13 0.0290(19) 0.0166(16) 0.0225(17) -0.0004(14) 0.0103(15) 0.0012(15) N14 0.0256(15) 0.0210(15) 0.0228(15) -0.0033(12) 0.0108(13) -0.0030(13) C15 0.0254(19) 0.0235(17) 0.0161(16) 0.0000(14) 0.0057(15) -0.0024(15) C16 0.0292(19) 0.0252(18) 0.0247(18) -0.0034(15) 0.0114(15) -0.0070(16) C17 0.035(2) 0.0173(18) 0.034(2) -0.0046(15) 0.0116(18) -0.0084(16) C18 0.035(2) 0.0224(18) 0.0270(19) -0.0061(15) 0.0120(17) -0.0024(16) O19 0.0248(13) 0.0186(11) 0.0272(13) -0.0055(10) 0.0098(11) -0.0043(10) C19 0.0244(18) 0.0267(18) 0.0272(19) -0.0059(15) 0.0092(16) -0.0031(16) C22 0.036(2) 0.034(2) 0.029(2) -0.0075(17) 0.0173(18) -0.0062(18) C23 0.029(2) 0.0251(19) 0.033(2) -0.0017(16) 0.0110(17) -0.0037(15) N24 0.0307(17) 0.0204(14) 0.0260(16) 0.0005(12) 0.0127(14) -0.0030(13) C25 0.0227(18) 0.0268(19) 0.031(2) -0.0007(16) 0.0068(16) -0.0030(16) C26 0.035(2) 0.0224(19) 0.039(2) 0.0084(16) 0.0077(18) 0.0009(17) C27 0.047(3) 0.038(2) 0.036(2) 0.0125(19) 0.014(2) -0.004(2) C28 0.052(3) 0.043(2) 0.030(2) 0.0051(19) 0.019(2) -0.005(2) O29 0.0270(13) 0.0189(12) 0.0277(14) -0.0028(10) 0.0067(11) 0.0020(11) C29 0.032(2) 0.0201(18) 0.040(2) -0.0009(15) 0.0139(18) 0.0015(16) Cl1 0.0333(6) 0.0359(5) 0.0387(6) 0.0022(4) 0.0166(5) 0.0010(4) O31 0.0386(17) 0.064(2) 0.052(2) -0.0057(17) 0.0132(15) -0.0057(15) O32 0.063(2) 0.0363(18) 0.095(3) -0.0165(18) 0.030(2) -0.0019(16) O33 0.0333(16) 0.0293(15) 0.070(2) -0.0023(14) 0.0184(16) -0.0016(12) O34 0.073(2) 0.0465(19) 0.068(2) 0.0173(17) 0.0461(19) 0.0122(16) Cl2A 0.0611(11) 0.0454(9) 0.0367(9) -0.0021(7) 0.0053(8) -0.0106(8) O35 0.066(5) 0.058(4) 0.044(4) 0.007(3) 0.037(4) -0.017(4) O36 0.041(4) 0.089(6) 0.054(4) -0.036(4) 0.007(3) 0.010(3) Cl2B 0.0611(11) 0.0454(9) 0.0367(9) -0.0021(7) 0.0053(8) -0.0106(8) O37 0.058(4) 0.074(5) 0.076(5) -0.033(4) 0.038(4) -0.037(4) O38 0.089(7) 0.122(8) 0.058(5) 0.028(5) 0.023(5) 0.042(6) C31 0.049(3) 0.073(4) 0.044(3) 0.024(3) 0.002(2) 0.004(3) N31 0.060(3) 0.127(5) 0.061(3) 0.051(3) -0.007(3) -0.002(3) C30 0.052(3) 0.084(4) 0.053(3) 0.014(3) 0.017(2) 0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O9 2.081(3) . ? Fe1 O19 2.099(2) . ? Fe1 O29 2.102(2) . ? Fe1 N14 2.117(3) . ? Fe1 N4 2.133(3) . ? Fe1 N24 2.145(3) . ? Fe1 N1 2.370(3) . ? Fe1 Fe2 2.8339(6) . ? Fe2 O9 1.991(2) 3_577 ? Fe2 O9 1.991(2) . ? Fe2 O19 2.005(2) . ? Fe2 O19 2.005(2) 3_577 ? Fe2 O29 2.013(3) . ? Fe2 O29 2.013(3) 3_577 ? Fe2 Fe1 2.8339(6) 3_577 ? N1 C2 1.488(5) . ? N1 C12 1.479(5) . ? N1 C22 1.480(5) . ? C2 C3 1.495(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N4 1.354(5) . ? C3 C8 1.385(5) . ? N4 C5 1.346(5) . ? C5 C6 1.399(5) . ? C5 C9 1.499(6) . ? C6 C7 1.386(7) . ? C6 H6A 0.9500 . ? C7 C8 1.366(7) . ? C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? O9 C9 1.412(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C12 C13 1.498(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N14 1.348(4) . ? C13 C18 1.372(5) . ? N14 C15 1.346(5) . ? C15 C16 1.382(5) . ? C15 C19 1.510(5) . ? C16 C17 1.381(5) . ? C16 H16A 0.9500 . ? C17 C18 1.388(6) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? O19 C19 1.421(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C22 C23 1.513(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 N24 1.344(5) . ? C23 C28 1.394(6) . ? N24 C25 1.352(5) . ? C25 C26 1.399(5) . ? C25 C29 1.487(6) . ? C26 C27 1.371(6) . ? C26 H26A 0.9500 . ? C27 C28 1.392(6) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? O29 C29 1.416(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? Cl1 O32 1.403(3) . ? Cl1 O33 1.433(3) . ? Cl1 O31 1.444(3) . ? Cl1 O34 1.458(3) . ? Cl2A O35 1.294(6) . ? Cl2A O35 1.294(6) 3_676 ? Cl2A O36 1.583(6) 3_676 ? Cl2A O36 1.583(6) . ? O35 O36 1.672(10) 3_676 ? O36 O35 1.672(10) 3_676 ? Cl2B O38 1.407(8) . ? Cl2B O38 1.408(8) 3_676 ? Cl2B O37 1.517(6) . ? Cl2B O37 1.517(6) 3_676 ? O37 O38 1.683(13) 3_676 ? O38 O37 1.683(13) 3_676 ? C31 N31 1.161(7) . ? C31 C30 1.424(8) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Fe1 O19 75.32(10) . . ? O9 Fe1 O29 75.63(10) . . ? O19 Fe1 O29 75.25(9) . . ? O9 Fe1 N14 95.32(11) . . ? O19 Fe1 N14 75.10(10) . . ? O29 Fe1 N14 150.31(11) . . ? O9 Fe1 N4 75.20(12) . . ? O19 Fe1 N4 150.29(12) . . ? O29 Fe1 N4 93.87(10) . . ? N14 Fe1 N4 111.35(11) . . ? O9 Fe1 N24 149.98(11) . . ? O19 Fe1 N24 94.79(11) . . ? O29 Fe1 N24 74.44(10) . . ? N14 Fe1 N24 109.65(11) . . ? N4 Fe1 N24 109.04(13) . . ? O9 Fe1 N1 134.97(10) . . ? O19 Fe1 N1 135.93(10) . . ? O29 Fe1 N1 134.33(10) . . ? N14 Fe1 N1 71.43(11) . . ? N4 Fe1 N1 70.75(12) . . ? N24 Fe1 N1 71.06(11) . . ? O9 Fe1 Fe2 44.61(7) . . ? O19 Fe1 Fe2 44.97(6) . . ? O29 Fe1 Fe2 45.18(7) . . ? N14 Fe1 Fe2 109.27(8) . . ? N4 Fe1 Fe2 108.40(9) . . ? N24 Fe1 Fe2 109.10(8) . . ? N1 Fe1 Fe2 179.10(7) . . ? O9 Fe2 O9 180.00(8) 3_577 . ? O9 Fe2 O19 100.55(9) 3_577 . ? O9 Fe2 O19 79.45(9) . . ? O9 Fe2 O19 79.45(9) 3_577 3_577 ? O9 Fe2 O19 100.55(9) . 3_577 ? O19 Fe2 O19 179.997(1) . 3_577 ? O9 Fe2 O29 100.33(10) 3_577 . ? O9 Fe2 O29 79.67(10) . . ? O19 Fe2 O29 79.33(10) . . ? O19 Fe2 O29 100.68(10) 3_577 . ? O9 Fe2 O29 79.67(10) 3_577 3_577 ? O9 Fe2 O29 100.33(10) . 3_577 ? O19 Fe2 O29 100.68(10) . 3_577 ? O19 Fe2 O29 79.32(10) 3_577 3_577 ? O29 Fe2 O29 179.999(1) . 3_577 ? O9 Fe2 Fe1 132.77(7) 3_577 . ? O9 Fe2 Fe1 47.23(7) . . ? O19 Fe2 Fe1 47.72(7) . . ? O19 Fe2 Fe1 132.28(7) 3_577 . ? O29 Fe2 Fe1 47.79(7) . . ? O29 Fe2 Fe1 132.21(7) 3_577 . ? O9 Fe2 Fe1 47.23(7) 3_577 3_577 ? O9 Fe2 Fe1 132.77(7) . 3_577 ? O19 Fe2 Fe1 132.28(7) . 3_577 ? O19 Fe2 Fe1 47.72(7) 3_577 3_577 ? O29 Fe2 Fe1 132.21(7) . 3_577 ? O29 Fe2 Fe1 47.79(7) 3_577 3_577 ? Fe1 Fe2 Fe1 180.00(2) . 3_577 ? C2 N1 C12 111.7(3) . . ? C2 N1 C22 111.1(3) . . ? C12 N1 C22 111.9(3) . . ? C2 N1 Fe1 108.3(2) . . ? C12 N1 Fe1 106.0(2) . . ? C22 N1 Fe1 107.6(2) . . ? N1 C2 C3 108.8(3) . . ? N1 C2 H2A 109.9 . . ? C3 C2 H2A 109.9 . . ? N1 C2 H2B 109.9 . . ? C3 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? N4 C3 C8 120.7(4) . . ? N4 C3 C2 115.3(3) . . ? C8 C3 C2 124.0(4) . . ? C5 N4 C3 120.0(3) . . ? C5 N4 Fe1 117.7(3) . . ? C3 N4 Fe1 122.2(3) . . ? N4 C5 C6 121.3(4) . . ? N4 C5 C9 115.2(3) . . ? C6 C5 C9 123.5(4) . . ? C7 C6 C5 118.1(4) . . ? C7 C6 H6A 121.0 . . ? C5 C6 H6A 121.0 . . ? C8 C7 C6 120.3(4) . . ? C8 C7 H7A 119.8 . . ? C6 C7 H7A 119.8 . . ? C7 C8 C3 119.6(4) . . ? C7 C8 H8A 120.2 . . ? C3 C8 H8A 120.2 . . ? C9 O9 Fe2 122.2(2) . . ? C9 O9 Fe1 119.6(2) . . ? Fe2 O9 Fe1 88.16(9) . . ? O9 C9 C5 110.6(3) . . ? O9 C9 H9A 109.5 . . ? C5 C9 H9A 109.5 . . ? O9 C9 H9B 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? N1 C12 C13 108.4(3) . . ? N1 C12 H12A 110.0 . . ? C13 C12 H12A 110.0 . . ? N1 C12 H12B 110.0 . . ? C13 C12 H12B 110.0 . . ? H12A C12 H12B 108.4 . . ? N14 C13 C18 121.3(3) . . ? N14 C13 C12 114.8(3) . . ? C18 C13 C12 123.9(3) . . ? C15 N14 C13 119.5(3) . . ? C15 N14 Fe1 118.6(2) . . ? C13 N14 Fe1 121.8(2) . . ? N14 C15 C16 121.7(3) . . ? N14 C15 C19 115.1(3) . . ? C16 C15 C19 123.2(3) . . ? C15 C16 C17 118.7(3) . . ? C15 C16 H16A 120.7 . . ? C17 C16 H16A 120.7 . . ? C16 C17 C18 119.4(3) . . ? C16 C17 H17A 120.3 . . ? C18 C17 H17A 120.3 . . ? C13 C18 C17 119.3(3) . . ? C13 C18 H18A 120.3 . . ? C17 C18 H18A 120.3 . . ? C19 O19 Fe2 119.8(2) . . ? C19 O19 Fe1 118.5(2) . . ? Fe2 O19 Fe1 87.31(9) . . ? O19 C19 C15 109.9(3) . . ? O19 C19 H19A 109.7 . . ? C15 C19 H19A 109.7 . . ? O19 C19 H19B 109.7 . . ? C15 C19 H19B 109.7 . . ? H19A C19 H19B 108.2 . . ? N1 C22 C23 107.7(3) . . ? N1 C22 H22A 110.2 . . ? C23 C22 H22A 110.2 . . ? N1 C22 H22B 110.2 . . ? C23 C22 H22B 110.2 . . ? H22A C22 H22B 108.5 . . ? N24 C23 C28 121.5(4) . . ? N24 C23 C22 115.4(3) . . ? C28 C23 C22 123.1(4) . . ? C23 N24 C25 120.5(3) . . ? C23 N24 Fe1 121.6(2) . . ? C25 N24 Fe1 117.9(3) . . ? N24 C25 C26 120.6(4) . . ? N24 C25 C29 115.6(3) . . ? C26 C25 C29 123.7(3) . . ? C27 C26 C25 118.8(4) . . ? C27 C26 H26A 120.6 . . ? C25 C26 H26A 120.6 . . ? C26 C27 C28 120.8(4) . . ? C26 C27 H27A 119.6 . . ? C28 C27 H27A 119.6 . . ? C23 C28 C27 117.9(4) . . ? C23 C28 H28A 121.1 . . ? C27 C28 H28A 121.1 . . ? C29 O29 Fe2 120.5(2) . . ? C29 O29 Fe1 119.0(2) . . ? Fe2 O29 Fe1 87.02(9) . . ? O29 C29 C25 110.2(3) . . ? O29 C29 H29A 109.6 . . ? C25 C29 H29A 109.6 . . ? O29 C29 H29B 109.6 . . ? C25 C29 H29B 109.6 . . ? H29A C29 H29B 108.1 . . ? O32 Cl1 O33 111.5(2) . . ? O32 Cl1 O31 111.4(2) . . ? O33 Cl1 O31 110.0(2) . . ? O32 Cl1 O34 109.5(2) . . ? O33 Cl1 O34 107.47(19) . . ? O31 Cl1 O34 106.9(2) . . ? O35 Cl2A O35 180.0(5) . 3_676 ? O35 Cl2A O36 70.2(4) . 3_676 ? O35 Cl2A O36 109.8(4) 3_676 3_676 ? O35 Cl2A O36 109.8(4) . . ? O35 Cl2A O36 70.2(4) 3_676 . ? O36 Cl2A O36 180.0(4) 3_676 . ? Cl2A O35 O36 63.0(4) . 3_676 ? Cl2A O36 O35 46.8(3) . 3_676 ? O38 Cl2B O38 180.0(5) . 3_676 ? O38 Cl2B O37 109.9(6) . . ? O38 Cl2B O37 70.1(6) 3_676 . ? O38 Cl2B O37 70.1(6) . 3_676 ? O38 Cl2B O37 109.9(6) 3_676 3_676 ? O37 Cl2B O37 180.0(5) . 3_676 ? Cl2B O37 O38 51.9(4) . 3_676 ? Cl2B O38 O37 58.0(4) . 3_676 ? N31 C31 C30 178.0(7) . . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 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 O9 Fe1 Fe2 O9 180.001(2) . . . 3_577 ? O19 Fe1 Fe2 O9 -59.73(13) . . . 3_577 ? O29 Fe1 Fe2 O9 59.39(13) . . . 3_577 ? N14 Fe1 Fe2 O9 -102.39(13) . . . 3_577 ? N4 Fe1 Fe2 O9 136.09(12) . . . 3_577 ? N24 Fe1 Fe2 O9 17.48(13) . . . 3_577 ? O19 Fe1 Fe2 O9 120.27(13) . . . . ? O29 Fe1 Fe2 O9 -120.61(13) . . . . ? N14 Fe1 Fe2 O9 77.61(13) . . . . ? N4 Fe1 Fe2 O9 -43.91(12) . . . . ? N24 Fe1 Fe2 O9 -162.52(13) . . . . ? O9 Fe1 Fe2 O19 -120.27(13) . . . . ? O29 Fe1 Fe2 O19 119.12(13) . . . . ? N14 Fe1 Fe2 O19 -42.66(12) . . . . ? N4 Fe1 Fe2 O19 -164.18(13) . . . . ? N24 Fe1 Fe2 O19 77.21(12) . . . . ? O9 Fe1 Fe2 O19 59.73(13) . . . 3_577 ? O19 Fe1 Fe2 O19 179.998(1) . . . 3_577 ? O29 Fe1 Fe2 O19 -60.88(13) . . . 3_577 ? N14 Fe1 Fe2 O19 137.34(12) . . . 3_577 ? N4 Fe1 Fe2 O19 15.82(13) . . . 3_577 ? N24 Fe1 Fe2 O19 -102.79(12) . . . 3_577 ? O9 Fe1 Fe2 O29 120.61(13) . . . . ? O19 Fe1 Fe2 O29 -119.12(13) . . . . ? N14 Fe1 Fe2 O29 -161.78(12) . . . . ? N4 Fe1 Fe2 O29 76.70(12) . . . . ? N24 Fe1 Fe2 O29 -41.92(12) . . . . ? O9 Fe1 Fe2 O29 -59.39(13) . . . 3_577 ? O19 Fe1 Fe2 O29 60.88(13) . . . 3_577 ? O29 Fe1 Fe2 O29 180.0 . . . 3_577 ? N14 Fe1 Fe2 O29 18.22(12) . . . 3_577 ? N4 Fe1 Fe2 O29 -103.30(12) . . . 3_577 ? N24 Fe1 Fe2 O29 138.09(12) . . . 3_577 ? O9 Fe1 N1 C2 -75.5(3) . . . . ? O19 Fe1 N1 C2 163.4(2) . . . . ? O29 Fe1 N1 C2 43.6(3) . . . . ? N14 Fe1 N1 C2 -154.1(3) . . . . ? N4 Fe1 N1 C2 -32.5(2) . . . . ? N24 Fe1 N1 C2 86.6(2) . . . . ? O9 Fe1 N1 C12 44.5(3) . . . . ? O19 Fe1 N1 C12 -76.6(3) . . . . ? O29 Fe1 N1 C12 163.5(2) . . . . ? N14 Fe1 N1 C12 -34.1(2) . . . . ? N4 Fe1 N1 C12 87.5(2) . . . . ? N24 Fe1 N1 C12 -153.5(2) . . . . ? O9 Fe1 N1 C22 164.4(2) . . . . ? O19 Fe1 N1 C22 43.3(3) . . . . ? O29 Fe1 N1 C22 -76.6(2) . . . . ? N14 Fe1 N1 C22 85.8(2) . . . . ? N4 Fe1 N1 C22 -152.6(2) . . . . ? N24 Fe1 N1 C22 -33.6(2) . . . . ? C12 N1 C2 C3 -77.6(4) . . . . ? C22 N1 C2 C3 156.7(3) . . . . ? Fe1 N1 C2 C3 38.8(3) . . . . ? N1 C2 C3 N4 -23.2(4) . . . . ? N1 C2 C3 C8 156.6(3) . . . . ? C8 C3 N4 C5 -3.3(5) . . . . ? C2 C3 N4 C5 176.5(3) . . . . ? C8 C3 N4 Fe1 172.5(3) . . . . ? C2 C3 N4 Fe1 -7.7(4) . . . . ? O9 Fe1 N4 C5 -11.4(2) . . . . ? O19 Fe1 N4 C5 -4.0(4) . . . . ? O29 Fe1 N4 C5 62.6(3) . . . . ? N14 Fe1 N4 C5 -101.4(3) . . . . ? N24 Fe1 N4 C5 137.5(2) . . . . ? N1 Fe1 N4 C5 -161.5(3) . . . . ? Fe2 Fe1 N4 C5 18.8(3) . . . . ? O9 Fe1 N4 C3 172.7(3) . . . . ? O19 Fe1 N4 C3 -179.9(2) . . . . ? O29 Fe1 N4 C3 -113.2(3) . . . . ? N14 Fe1 N4 C3 82.8(3) . . . . ? N24 Fe1 N4 C3 -38.4(3) . . . . ? N1 Fe1 N4 C3 22.7(2) . . . . ? Fe2 Fe1 N4 C3 -157.0(2) . . . . ? C3 N4 C5 C6 3.9(5) . . . . ? Fe1 N4 C5 C6 -172.1(2) . . . . ? C3 N4 C5 C9 -173.4(3) . . . . ? Fe1 N4 C5 C9 10.6(4) . . . . ? N4 C5 C6 C7 -2.1(5) . . . . ? C9 C5 C6 C7 175.0(3) . . . . ? C5 C6 C7 C8 -0.2(6) . . . . ? C6 C7 C8 C3 0.8(6) . . . . ? N4 C3 C8 C7 0.9(5) . . . . ? C2 C3 C8 C7 -178.9(4) . . . . ? O19 Fe2 O9 C9 164.9(3) . . . . ? O19 Fe2 O9 C9 -15.1(3) 3_577 . . . ? O29 Fe2 O9 C9 84.0(3) . . . . ? O29 Fe2 O9 C9 -96.0(3) 3_577 . . . ? Fe1 Fe2 O9 C9 124.4(3) . . . . ? Fe1 Fe2 O9 C9 -55.6(3) 3_577 . . . ? O19 Fe2 O9 Fe1 40.54(9) . . . . ? O19 Fe2 O9 Fe1 -139.46(9) 3_577 . . . ? O29 Fe2 O9 Fe1 -40.39(9) . . . . ? O29 Fe2 O9 Fe1 139.61(9) 3_577 . . . ? Fe1 Fe2 O9 Fe1 179.999(1) 3_577 . . . ? O19 Fe1 O9 C9 -165.7(2) . . . . ? O29 Fe1 O9 C9 -87.5(2) . . . . ? N14 Fe1 O9 C9 121.3(2) . . . . ? N4 Fe1 O9 C9 10.6(2) . . . . ? N24 Fe1 O9 C9 -92.0(3) . . . . ? N1 Fe1 O9 C9 52.3(3) . . . . ? Fe2 Fe1 O9 C9 -126.5(3) . . . . ? O19 Fe1 O9 Fe2 -39.13(8) . . . . ? O29 Fe1 O9 Fe2 39.07(8) . . . . ? N14 Fe1 O9 Fe2 -112.18(10) . . . . ? N4 Fe1 O9 Fe2 137.10(11) . . . . ? N24 Fe1 O9 Fe2 34.6(2) . . . . ? N1 Fe1 O9 Fe2 178.86(10) . . . . ? Fe2 O9 C9 C5 -116.7(3) . . . . ? Fe1 O9 C9 C5 -8.3(4) . . . . ? N4 C5 C9 O9 -1.7(4) . . . . ? C6 C5 C9 O9 -179.0(3) . . . . ? C2 N1 C12 C13 161.1(3) . . . . ? C22 N1 C12 C13 -73.7(4) . . . . ? Fe1 N1 C12 C13 43.3(3) . . . . ? N1 C12 C13 N14 -30.2(4) . . . . ? N1 C12 C13 C18 150.6(3) . . . . ? C18 C13 N14 C15 0.5(5) . . . . ? C12 C13 N14 C15 -178.7(3) . . . . ? C18 C13 N14 Fe1 176.9(3) . . . . ? C12 C13 N14 Fe1 -2.2(4) . . . . ? O9 Fe1 N14 C15 61.3(3) . . . . ? O19 Fe1 N14 C15 -11.9(2) . . . . ? O29 Fe1 N14 C15 -8.8(4) . . . . ? N4 Fe1 N14 C15 137.5(2) . . . . ? N24 Fe1 N14 C15 -101.8(3) . . . . ? N1 Fe1 N14 C15 -162.8(3) . . . . ? Fe2 Fe1 N14 C15 17.8(3) . . . . ? O9 Fe1 N14 C13 -115.1(3) . . . . ? O19 Fe1 N14 C13 171.6(3) . . . . ? O29 Fe1 N14 C13 174.7(2) . . . . ? N4 Fe1 N14 C13 -39.0(3) . . . . ? N24 Fe1 N14 C13 81.8(3) . . . . ? N1 Fe1 N14 C13 20.7(3) . . . . ? Fe2 Fe1 N14 C13 -158.7(2) . . . . ? C13 N14 C15 C16 0.8(5) . . . . ? Fe1 N14 C15 C16 -175.7(3) . . . . ? C13 N14 C15 C19 -176.8(3) . . . . ? Fe1 N14 C15 C19 6.6(4) . . . . ? N14 C15 C16 C17 -1.4(5) . . . . ? C19 C15 C16 C17 176.0(3) . . . . ? C15 C16 C17 C18 0.7(5) . . . . ? N14 C13 C18 C17 -1.3(6) . . . . ? C12 C13 C18 C17 177.8(4) . . . . ? C16 C17 C18 C13 0.6(6) . . . . ? O9 Fe2 O19 C19 -98.6(2) 3_577 . . . ? O9 Fe2 O19 C19 81.4(2) . . . . ? O29 Fe2 O19 C19 162.7(2) . . . . ? O29 Fe2 O19 C19 -17.3(2) 3_577 . . . ? Fe1 Fe2 O19 C19 121.6(3) . . . . ? Fe1 Fe2 O19 C19 -58.4(3) 3_577 . . . ? O9 Fe2 O19 Fe1 139.84(9) 3_577 . . . ? O9 Fe2 O19 Fe1 -40.16(9) . . . . ? O29 Fe2 O19 Fe1 41.18(9) . . . . ? O29 Fe2 O19 Fe1 -138.82(9) 3_577 . . . ? Fe1 Fe2 O19 Fe1 180.0 3_577 . . . ? O9 Fe1 O19 C19 -83.9(2) . . . . ? O29 Fe1 O19 C19 -162.6(2) . . . . ? N14 Fe1 O19 C19 15.8(2) . . . . ? N4 Fe1 O19 C19 -91.3(3) . . . . ? N24 Fe1 O19 C19 124.9(2) . . . . ? N1 Fe1 O19 C19 57.3(3) . . . . ? Fe2 Fe1 O19 C19 -122.7(3) . . . . ? O9 Fe1 O19 Fe2 38.83(9) . . . . ? O29 Fe1 O19 Fe2 -39.85(9) . . . . ? N14 Fe1 O19 Fe2 138.55(11) . . . . ? N4 Fe1 O19 Fe2 31.5(2) . . . . ? N24 Fe1 O19 Fe2 -112.37(10) . . . . ? N1 Fe1 O19 Fe2 -179.93(11) . . . . ? Fe2 O19 C19 C15 -121.3(3) . . . . ? Fe1 O19 C19 C15 -16.8(4) . . . . ? N14 C15 C19 O19 6.3(4) . . . . ? C16 C15 C19 O19 -171.3(3) . . . . ? C2 N1 C22 C23 -76.1(4) . . . . ? C12 N1 C22 C23 158.4(3) . . . . ? Fe1 N1 C22 C23 42.3(3) . . . . ? N1 C22 C23 N24 -28.9(4) . . . . ? N1 C22 C23 C28 149.7(4) . . . . ? C28 C23 N24 C25 -1.1(5) . . . . ? C22 C23 N24 C25 177.6(3) . . . . ? C28 C23 N24 Fe1 179.1(3) . . . . ? C22 C23 N24 Fe1 -2.2(4) . . . . ? O9 Fe1 N24 C23 174.2(2) . . . . ? O19 Fe1 N24 C23 -117.1(3) . . . . ? O29 Fe1 N24 C23 169.7(3) . . . . ? N14 Fe1 N24 C23 -41.2(3) . . . . ? N4 Fe1 N24 C23 81.0(3) . . . . ? N1 Fe1 N24 C23 20.1(3) . . . . ? Fe2 Fe1 N24 C23 -160.8(3) . . . . ? O9 Fe1 N24 C25 -5.6(4) . . . . ? O19 Fe1 N24 C25 63.1(3) . . . . ? O29 Fe1 N24 C25 -10.1(2) . . . . ? N14 Fe1 N24 C25 139.0(2) . . . . ? N4 Fe1 N24 C25 -98.8(3) . . . . ? N1 Fe1 N24 C25 -159.7(3) . . . . ? Fe2 Fe1 N24 C25 19.4(3) . . . . ? C23 N24 C25 C26 0.4(5) . . . . ? Fe1 N24 C25 C26 -179.8(3) . . . . ? C23 N24 C25 C29 -176.1(3) . . . . ? Fe1 N24 C25 C29 3.7(4) . . . . ? N24 C25 C26 C27 0.1(6) . . . . ? C29 C25 C26 C27 176.3(4) . . . . ? C25 C26 C27 C28 0.0(6) . . . . ? N24 C23 C28 C27 1.2(6) . . . . ? C22 C23 C28 C27 -177.4(4) . . . . ? C26 C27 C28 C23 -0.6(6) . . . . ? O9 Fe2 O29 C29 -17.8(3) 3_577 . . . ? O9 Fe2 O29 C29 162.2(3) . . . . ? O19 Fe2 O29 C29 81.1(2) . . . . ? O19 Fe2 O29 C29 -98.9(2) 3_577 . . . ? Fe1 Fe2 O29 C29 122.2(3) . . . . ? Fe1 Fe2 O29 C29 -57.8(3) 3_577 . . . ? O9 Fe2 O29 Fe1 -140.04(9) 3_577 . . . ? O9 Fe2 O29 Fe1 39.96(9) . . . . ? O19 Fe2 O29 Fe1 -41.12(9) . . . . ? O19 Fe2 O29 Fe1 138.88(9) 3_577 . . . ? Fe1 Fe2 O29 Fe1 180.0 3_577 . . . ? O9 Fe1 O29 C29 -162.1(3) . . . . ? O19 Fe1 O29 C29 -83.8(2) . . . . ? N14 Fe1 O29 C29 -86.9(3) . . . . ? N4 Fe1 O29 C29 124.3(3) . . . . ? N24 Fe1 O29 C29 15.6(2) . . . . ? N1 Fe1 O29 C29 57.6(3) . . . . ? Fe2 Fe1 O29 C29 -123.5(3) . . . . ? O9 Fe1 O29 Fe2 -38.60(8) . . . . ? O19 Fe1 O29 Fe2 39.68(9) . . . . ? N14 Fe1 O29 Fe2 36.6(2) . . . . ? N4 Fe1 O29 Fe2 -112.25(11) . . . . ? N24 Fe1 O29 Fe2 139.06(12) . . . . ? N1 Fe1 O29 Fe2 -178.93(10) . . . . ? Fe2 O29 C29 C25 -123.0(3) . . . . ? Fe1 O29 C29 C25 -18.1(4) . . . . ? N24 C25 C29 O29 8.7(5) . . . . ? C26 C25 C29 O29 -167.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.815 _refine_diff_density_min -0.743 _refine_diff_density_rms 0.115