# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Isabelle Artaud' _publ_contact_author_email ISABELLE.ARTAUD@UNIV-PARIS5.FR _publ_section_title ; Synthesis and characterization of mononuclear hydroxamato and hydroximato complexes of iron(III) based on the tris-(2-pyridylmethyl)amine ligand ; _publ_contact_author_address ; Laboratoire de Chimie et Biochimie Toxicologiques et Pharmacologiques, UMR8601 CNRS, Universit\'e Paris-Descartes, 45 rue des St-P\'eres, 75270 Paris Cedex 06, France. ; _publ_contact_author_phone 33142862189 loop_ _publ_author_name 'Isabelle Artaud' 'Erwan Galardon' 'Pascal Roussel' 'Mohamed Selkti' 'Alain Tomas' # Attachment 'complex1a.cif' data_complex1a _database_code_depnum_ccdc_archive 'CCDC 689687' _audit_creation_method 'WinGX routine CIF_UPDATE' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H22 Cl2 Fe N5 O10' _chemical_formula_sum 'C20 H22 Cl2 Fe N5 O10' _chemical_formula_weight 619.18 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 triclinic _symmetry_space_group_name_H-M ' p_-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.098(4) _cell_length_b 12.376(4) _cell_length_c 13.055(5) _cell_angle_alpha 83.11(5) _cell_angle_beta 75.24(3) _cell_angle_gamma 71.67(4) _cell_volume 1644.4(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8056 _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 23.01 _exptl_crystal_description parallepiped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.075 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 634 _exptl_absorpt_coefficient_mu 0.670 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8056 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0778 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 23.01 _reflns_number_total 4553 _reflns_number_gt 2915 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep (C.K.Johnson, 1976)' _computing_publication_material ? _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^)+(0.1334P)^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 4553 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1058 _refine_ls_R_factor_gt 0.0748 _refine_ls_wR_factor_ref 0.2273 _refine_ls_wR_factor_gt 0.2094 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 0.21831(8) 0.21693(7) 0.82318(6) 0.0411(3) Uani 1 1 d . . . O1 O 0.3227(4) 0.1224(3) 0.9042(3) 0.0525(11) Uani 1 1 d . . . O2 O 0.0752(4) 0.1949(3) 0.9388(3) 0.0496(11) Uani 1 1 d . . . N1 N 0.2062(5) 0.0945(4) 0.7459(4) 0.0528(14) Uani 1 1 d . . . N2 N 0.3612(5) 0.2432(4) 0.7166(4) 0.0432(12) Uani 1 1 d . . . N3 N 0.1963(5) 0.3617(4) 0.8807(4) 0.0436(12) Uani 1 1 d . . . N4 N 0.1059(5) 0.3126(4) 0.7300(4) 0.0445(12) Uani 1 1 d . . . N5 N 0.2501(6) 0.0826(5) 0.9915(5) 0.0662(16) Uani 1 1 d . . . H5 H 0.2864 0.0338 1.0356 0.079 Uiso 1 1 calc R . . C1 C 0.2897(8) -0.0120(6) 0.7397(6) 0.066(2) Uani 1 1 d . . . H1 H 0.3595 -0.0324 0.7724 0.080 Uiso 1 1 calc R . . C2 C 0.2692(11) -0.0899(7) 0.6838(6) 0.087(3) Uani 1 1 d . . . H2 H 0.3245 -0.1642 0.6802 0.105 Uiso 1 1 calc R . . C3 C 0.1702(12) -0.0596(9) 0.6347(7) 0.094(3) Uani 1 1 d . . . H3 H 0.1578 -0.1128 0.5968 0.113 Uiso 1 1 calc R . . C4 C 0.0848(10) 0.0524(8) 0.6402(7) 0.086(3) Uani 1 1 d . . . H4 H 0.0176 0.0751 0.6046 0.103 Uiso 1 1 calc R . . C5 C 0.1038(7) 0.1249(6) 0.6983(5) 0.0587(18) Uani 1 1 d . . . C6 C 0.0211(6) 0.2465(5) 0.7140(5) 0.0498(16) Uani 1 1 d . . . H6A H -0.0143 0.2771 0.6523 0.060 Uiso 1 1 calc R . . H6B H -0.0509 0.2509 0.7754 0.060 Uiso 1 1 calc R . . C7 C 0.1865(6) 0.3353(6) 0.6284(5) 0.0522(16) Uani 1 1 d . . . H7A H 0.1542 0.4152 0.6076 0.063 Uiso 1 1 calc R . . H7B H 0.1788 0.2907 0.5755 0.063 Uiso 1 1 calc R . . C8 C 0.3299(6) 0.3077(5) 0.6297(5) 0.0480(16) Uani 1 1 d . . . C9 C 0.4188(8) 0.3457(6) 0.5528(6) 0.069(2) Uani 1 1 d . . . H9 H 0.3943 0.3926 0.4958 0.083 Uiso 1 1 calc R . . C10 C 0.5474(8) 0.3109(7) 0.5636(7) 0.075(2) Uani 1 1 d . . . H10 H 0.6110 0.3332 0.5118 0.090 Uiso 1 1 calc R . . C11 C 0.5808(7) 0.2454(7) 0.6478(7) 0.075(2) Uani 1 1 d . . . H11 H 0.6670 0.2227 0.6539 0.090 Uiso 1 1 calc R . . C12 C 0.4890(7) 0.2123(6) 0.7240(6) 0.0592(18) Uani 1 1 d . . . H12 H 0.5131 0.1677 0.7823 0.071 Uiso 1 1 calc R . . C13 C 0.0259(6) 0.4203(6) 0.7859(5) 0.0568(18) Uani 1 1 d . . . H13A H -0.0525 0.4089 0.8333 0.068 Uiso 1 1 calc R . . H13B H 0.0001 0.4811 0.7345 0.068 Uiso 1 1 calc R . . C14 C 0.1061(6) 0.4523(5) 0.8483(5) 0.0499(16) Uani 1 1 d . . . C15 C 0.0860(7) 0.5607(6) 0.8759(5) 0.0583(18) Uani 1 1 d . . . H15 H 0.0235 0.6216 0.8526 0.070 Uiso 1 1 calc R . . C16 C 0.1603(8) 0.5779(6) 0.9390(6) 0.065(2) Uani 1 1 d . . . H16 H 0.1472 0.6508 0.9597 0.078 Uiso 1 1 calc R . . C17 C 0.2516(8) 0.4890(7) 0.9706(6) 0.067(2) Uani 1 1 d . . . H17 H 0.3034 0.5008 1.0116 0.080 Uiso 1 1 calc R . . C18 C 0.2685(7) 0.3804(6) 0.9424(5) 0.0530(17) Uani 1 1 d . . . H18 H 0.3304 0.3192 0.9660 0.064 Uiso 1 1 calc R . . C19 C 0.1202(7) 0.1215(6) 1.0069(5) 0.0517(17) Uani 1 1 d . . . C20 C 0.0396(8) 0.0826(7) 1.1001(6) 0.078(2) Uani 1 1 d . . . H20A H 0.0941 0.0271 1.1399 0.117 Uiso 1 1 calc R . . H20B H -0.0167 0.0488 1.0791 0.117 Uiso 1 1 calc R . . H20C H -0.0121 0.1460 1.1433 0.117 Uiso 1 1 calc R . . Cl1 Cl 0.07377(19) 0.68231(16) 0.57857(16) 0.0672(6) Uani 1 1 d . . . O11 O 0.1850(6) 0.6127(6) 0.6075(6) 0.118(2) Uani 1 1 d . . . O12 O 0.1013(11) 0.7623(7) 0.4985(6) 0.154(4) Uani 1 1 d . . . O13 O 0.0015(9) 0.6225(8) 0.5533(7) 0.151(3) Uani 1 1 d . . . O14 O 0.0053(10) 0.7486(9) 0.6689(7) 0.179(4) Uani 1 1 d . . . Cl2 Cl 0.66412(19) 0.22600(16) 0.95909(18) 0.0725(6) Uani 1 1 d . . . O21 O 0.7290(9) 0.1840(6) 1.0404(7) 0.146(3) Uani 1 1 d . . . O22 O 0.6278(11) 0.1409(6) 0.9273(8) 0.187(5) Uani 1 1 d . . . O23 O 0.5568(8) 0.3173(9) 0.9880(10) 0.202(5) Uani 1 1 d . . . O24 O 0.7490(11) 0.2802(12) 0.8802(9) 0.228(6) 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 0.0397(6) 0.0458(6) 0.0392(6) 0.0028(4) -0.0128(4) -0.0133(4) O1 0.053(3) 0.050(2) 0.056(3) 0.014(2) -0.023(2) -0.015(2) O2 0.053(3) 0.056(3) 0.039(2) 0.007(2) -0.009(2) -0.019(2) N1 0.060(4) 0.053(3) 0.047(3) 0.001(3) -0.009(3) -0.022(3) N2 0.038(3) 0.050(3) 0.040(3) -0.006(2) -0.007(2) -0.012(2) N3 0.045(3) 0.048(3) 0.037(3) -0.002(2) -0.011(2) -0.012(2) N4 0.035(3) 0.052(3) 0.048(3) -0.007(2) -0.015(2) -0.009(2) N5 0.064(4) 0.056(3) 0.082(4) 0.025(3) -0.029(4) -0.022(3) C1 0.078(5) 0.045(4) 0.071(5) -0.005(4) -0.011(4) -0.015(4) C2 0.128(8) 0.057(5) 0.064(5) -0.007(4) -0.001(6) -0.025(5) C3 0.143(9) 0.099(7) 0.075(6) -0.002(5) -0.029(6) -0.080(7) C4 0.122(8) 0.086(6) 0.079(6) 0.022(5) -0.044(6) -0.065(6) C5 0.071(5) 0.072(5) 0.047(4) -0.003(3) -0.019(4) -0.037(4) C6 0.047(4) 0.062(4) 0.047(4) 0.004(3) -0.023(3) -0.017(3) C7 0.057(4) 0.055(4) 0.046(4) 0.010(3) -0.017(3) -0.018(3) C8 0.059(4) 0.043(3) 0.038(4) -0.007(3) -0.010(3) -0.009(3) C9 0.064(5) 0.077(5) 0.052(4) 0.014(4) 0.007(4) -0.025(4) C10 0.055(5) 0.094(6) 0.074(6) 0.015(5) -0.006(4) -0.032(4) C11 0.036(4) 0.097(6) 0.084(6) 0.009(5) -0.006(4) -0.019(4) C12 0.057(5) 0.069(4) 0.052(4) 0.004(3) -0.013(4) -0.021(4) C13 0.048(4) 0.062(4) 0.056(4) -0.004(3) -0.020(3) -0.002(3) C14 0.040(4) 0.048(4) 0.056(4) -0.006(3) -0.008(3) -0.007(3) C15 0.058(4) 0.059(4) 0.045(4) -0.005(3) -0.003(3) -0.007(3) C16 0.075(5) 0.053(4) 0.064(5) -0.001(4) -0.004(4) -0.025(4) C17 0.074(5) 0.093(6) 0.050(4) -0.007(4) -0.020(4) -0.041(5) C18 0.059(4) 0.057(4) 0.048(4) 0.001(3) -0.016(3) -0.022(3) C19 0.055(5) 0.067(4) 0.037(4) -0.003(3) 0.002(3) -0.032(4) C20 0.075(6) 0.096(6) 0.059(5) 0.009(4) -0.017(4) -0.021(5) Cl1 0.0704(13) 0.0660(11) 0.0720(13) 0.0128(10) -0.0254(10) -0.0280(10) O11 0.079(4) 0.136(5) 0.136(6) 0.038(5) -0.051(4) -0.022(4) O12 0.294(12) 0.140(6) 0.103(5) 0.060(5) -0.118(7) -0.137(7) O13 0.174(8) 0.175(7) 0.178(8) 0.025(6) -0.104(7) -0.116(6) O14 0.202(10) 0.209(10) 0.103(6) -0.045(6) -0.016(6) -0.033(8) Cl2 0.0623(12) 0.0638(11) 0.0985(15) 0.0122(10) -0.0386(11) -0.0186(9) O21 0.209(9) 0.120(6) 0.168(7) 0.046(5) -0.152(7) -0.061(5) O22 0.305(13) 0.096(5) 0.256(10) 0.066(6) -0.243(11) -0.079(6) O23 0.109(7) 0.177(9) 0.288(13) -0.070(9) -0.074(8) 0.045(6) O24 0.161(9) 0.292(14) 0.164(9) 0.063(9) 0.034(8) -0.058(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.818(4) . ? Fe1 N2 1.910(5) . ? Fe1 N3 1.946(5) . ? Fe1 O2 1.957(4) . ? Fe1 N1 1.974(5) . ? Fe1 N4 1.984(5) . ? O1 N5 1.355(7) . ? O2 C19 1.269(8) . ? N1 C1 1.350(8) . ? N1 C5 1.361(9) . ? N2 C8 1.361(8) . ? N2 C12 1.373(8) . ? N3 C14 1.354(8) . ? N3 C18 1.354(8) . ? N4 C7 1.450(8) . ? N4 C6 1.492(7) . ? N4 C13 1.503(7) . ? N5 C19 1.338(9) . ? C1 C2 1.381(10) . ? C2 C3 1.342(13) . ? C3 C4 1.410(13) . ? C4 C5 1.338(10) . ? C5 C6 1.503(9) . ? C7 C8 1.523(9) . ? C8 C9 1.370(9) . ? C9 C10 1.395(11) . ? C10 C11 1.344(11) . ? C11 C12 1.358(10) . ? C13 C14 1.510(9) . ? C14 C15 1.366(9) . ? C15 C16 1.379(10) . ? C16 C17 1.346(10) . ? C17 C18 1.379(9) . ? C19 C20 1.445(10) . ? Cl1 O13 1.366(6) . ? Cl1 O11 1.379(6) . ? Cl1 O12 1.395(7) . ? Cl1 O14 1.422(8) . ? Cl2 O23 1.366(8) . ? Cl2 O22 1.379(7) . ? Cl2 O21 1.391(6) . ? Cl2 O24 1.461(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 O1 Fe1 N2 93.8(2) . . ? O1 Fe1 N3 99.2(2) . . ? N2 Fe1 N3 87.9(2) . . ? O1 Fe1 O2 84.6(2) . . ? N2 Fe1 O2 176.27(18) . . ? N3 Fe1 O2 89.09(19) . . ? O1 Fe1 N1 95.4(2) . . ? N2 Fe1 N1 93.3(2) . . ? N3 Fe1 N1 165.3(2) . . ? O2 Fe1 N1 90.2(2) . . ? O1 Fe1 N4 176.75(18) . . ? N2 Fe1 N4 85.9(2) . . ? N3 Fe1 N4 84.05(19) . . ? O2 Fe1 N4 95.9(2) . . ? N1 Fe1 N4 81.4(2) . . ? N5 O1 Fe1 110.5(4) . . ? C19 O2 Fe1 109.9(4) . . ? C1 N1 C5 121.0(6) . . ? C1 N1 Fe1 124.4(5) . . ? C5 N1 Fe1 114.6(4) . . ? C8 N2 C12 117.6(6) . . ? C8 N2 Fe1 115.9(4) . . ? C12 N2 Fe1 126.2(5) . . ? C14 N3 C18 118.3(5) . . ? C14 N3 Fe1 115.3(4) . . ? C18 N3 Fe1 126.1(4) . . ? C7 N4 C6 109.3(5) . . ? C7 N4 C13 111.9(5) . . ? C6 N4 C13 111.1(5) . . ? C7 N4 Fe1 109.7(4) . . ? C6 N4 Fe1 107.3(4) . . ? C13 N4 Fe1 107.5(3) . . ? C19 N5 O1 117.9(6) . . ? N1 C1 C2 118.5(8) . . ? C3 C2 C1 120.7(8) . . ? C2 C3 C4 120.3(8) . . ? C5 C4 C3 117.7(8) . . ? C4 C5 N1 121.6(7) . . ? C4 C5 C6 124.7(7) . . ? N1 C5 C6 113.6(5) . . ? N4 C6 C5 107.6(5) . . ? N4 C7 C8 113.2(5) . . ? N2 C8 C9 122.9(6) . . ? N2 C8 C7 113.4(5) . . ? C9 C8 C7 123.7(6) . . ? C8 C9 C10 117.1(7) . . ? C11 C10 C9 120.8(7) . . ? C10 C11 C12 120.2(7) . . ? C11 C12 N2 121.3(7) . . ? N4 C13 C14 109.0(5) . . ? N3 C14 C15 122.1(6) . . ? N3 C14 C13 113.6(5) . . ? C15 C14 C13 124.2(6) . . ? C14 C15 C16 118.7(7) . . ? C17 C16 C15 119.9(7) . . ? C16 C17 C18 120.1(7) . . ? N3 C18 C17 120.9(7) . . ? O2 C19 N5 116.7(6) . . ? O2 C19 C20 123.8(7) . . ? N5 C19 C20 119.5(7) . . ? O13 Cl1 O11 112.7(5) . . ? O13 Cl1 O12 111.9(5) . . ? O11 Cl1 O12 111.9(6) . . ? O13 Cl1 O14 112.1(6) . . ? O11 Cl1 O14 103.6(5) . . ? O12 Cl1 O14 104.0(6) . . ? O23 Cl2 O22 109.6(7) . . ? O23 Cl2 O21 112.5(7) . . ? O22 Cl2 O21 109.8(4) . . ? O23 Cl2 O24 100.8(8) . . ? O22 Cl2 O24 118.3(7) . . ? O21 Cl2 O24 105.7(7) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 23.01 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.467 _refine_diff_density_min -0.355 _refine_diff_density_rms 0.085 # Attachment 'complex2b.cif' data_complex2b _database_code_depnum_ccdc_archive 'CCDC 689688' _audit_creation_method 'WinGX routine CIF_UPDATE' loop_ _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H43 B Fe N5 O2.5' _chemical_formula_weight 808.6 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 13.052(2) _cell_length_b 11.580(2) _cell_length_c 27.714(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.54(4) _cell_angle_gamma 90.00 _cell_volume 4142.2(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 69025 _cell_measurement_theta_min 1.91 _cell_measurement_theta_max 20.84 _exptl_crystal_description parallepiped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.095 _exptl_crystal_size_mid 0.085 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1692 _exptl_absorpt_coefficient_mu 0.412 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method \f _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69025 _diffrn_reflns_av_R_equivalents 0.1332 _diffrn_reflns_av_sigmaI/netI 0.0613 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 20.84 _reflns_number_total 4346 _reflns_number_gt 3129 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep (C.K.Johnson, 1976)' _computing_publication_material ? _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^)+(0.0722P)^2^+10.1904P] 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 4346 _refine_ls_number_parameters 527 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1161 _refine_ls_R_factor_gt 0.0823 _refine_ls_wR_factor_ref 0.2001 _refine_ls_wR_factor_gt 0.1824 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.142 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.83661(9) 0.53412(9) 0.07187(4) 0.0563(4) Uani 1 1 d . . . O1 O 0.8739(4) 0.4846(4) 0.01523(17) 0.0634(14) Uani 1 1 d . . . O2 O 0.7866(4) 0.3806(4) 0.07677(18) 0.0546(13) Uani 1 1 d . . . N1 N 0.9667(6) 0.5029(5) 0.1157(2) 0.0573(17) Uani 1 1 d . . . N2 N 0.8852(4) 0.6922(5) 0.0682(2) 0.0459(15) Uani 1 1 d . . . N3 N 0.6981(5) 0.5831(6) 0.0434(3) 0.0693(19) Uani 1 1 d . . . N4 N 0.7886(5) 0.5841(5) 0.1338(2) 0.0601(17) Uani 1 1 d . . . N5 N 0.8372(5) 0.3722(5) 0.0013(2) 0.0644(18) Uani 1 1 d . . . C1 C 1.0607(8) 0.4950(6) 0.1033(4) 0.075(3) Uani 1 1 d . . . H1 H 1.0690 0.5039 0.0708 0.090 Uiso 1 1 calc R . . C2 C 1.1464(9) 0.4738(8) 0.1376(5) 0.105(4) Uani 1 1 d . . . H2 H 1.2116 0.4681 0.1281 0.126 Uiso 1 1 calc R . . C3 C 1.1350(11) 0.4612(8) 0.1852(5) 0.108(4) Uani 1 1 d . . . H3 H 1.1921 0.4441 0.2084 0.129 Uiso 1 1 calc R . . C4 C 1.0381(12) 0.4740(8) 0.1993(4) 0.095(3) Uani 1 1 d . . . H4 H 1.0287 0.4684 0.2318 0.114 Uiso 1 1 calc R . . C5 C 0.9556(9) 0.4955(6) 0.1625(4) 0.071(2) Uani 1 1 d . . . C6 C 0.8478(8) 0.5095(7) 0.1724(3) 0.082(3) Uani 1 1 d . . . H6A H 0.8482 0.5447 0.2042 0.099 Uiso 1 1 calc R . . H6B H 0.8148 0.4345 0.1726 0.099 Uiso 1 1 calc R . . C7 C 0.8118(7) 0.7094(6) 0.1427(3) 0.076(3) Uani 1 1 d . . . H7A H 0.7475 0.7506 0.1439 0.091 Uiso 1 1 calc R . . H7B H 0.8548 0.7182 0.1742 0.091 Uiso 1 1 calc R . . C8 C 0.8657(6) 0.7615(6) 0.1045(3) 0.056(2) Uani 1 1 d . . . C9 C 0.8981(7) 0.8763(7) 0.1064(3) 0.070(2) Uani 1 1 d . . . H9 H 0.8836 0.9247 0.1313 0.084 Uiso 1 1 calc R . . C10 C 0.9515(8) 0.9162(8) 0.0712(3) 0.087(3) Uani 1 1 d . . . H10 H 0.9733 0.9927 0.0720 0.105 Uiso 1 1 calc R . . C11 C 0.9736(7) 0.8451(8) 0.0345(3) 0.086(3) Uani 1 1 d . . . H11 H 1.0111 0.8715 0.0107 0.103 Uiso 1 1 calc R . . C12 C 0.9377(6) 0.7321(7) 0.0342(3) 0.062(2) Uani 1 1 d . . . H12 H 0.9510 0.6828 0.0094 0.075 Uiso 1 1 calc R . . C13 C 0.6782(8) 0.5601(8) 0.1273(3) 0.084(3) Uani 1 1 d . . . H13A H 0.6455 0.6032 0.1509 0.101 Uiso 1 1 calc R . . H13B H 0.6663 0.4784 0.1319 0.101 Uiso 1 1 calc R . . C14 C 0.6335(8) 0.5958(7) 0.0763(4) 0.082(3) Uani 1 1 d . . . C15 C 0.5339(11) 0.6354(10) 0.0642(6) 0.120(4) Uani 1 1 d . . . H15 H 0.4901 0.6426 0.0876 0.144 Uiso 1 1 calc R . . C16 C 0.5011(11) 0.6641(11) 0.0163(7) 0.137(5) Uani 1 1 d . . . H16 H 0.4351 0.6943 0.0072 0.165 Uiso 1 1 calc R . . C17 C 0.5636(11) 0.6489(10) -0.0176(5) 0.118(4) Uani 1 1 d . . . H17 H 0.5394 0.6639 -0.0503 0.141 Uiso 1 1 calc R . . C18 C 0.6656(9) 0.6103(8) -0.0035(4) 0.090(3) Uani 1 1 d . . . H18 H 0.7105 0.6036 -0.0264 0.109 Uiso 1 1 calc R . . C19 C 0.7953(6) 0.3267(6) 0.0362(3) 0.052(2) Uani 1 1 d . . . C20 C 0.7516(6) 0.2075(7) 0.0312(3) 0.061(2) Uani 1 1 d . . . C21 C 0.7530(7) 0.1451(8) -0.0115(3) 0.085(3) Uani 1 1 d . . . H21 H 0.7820 0.1770 -0.0371 0.102 Uiso 1 1 calc R . . C22 C 0.7100(9) 0.0330(9) -0.0156(4) 0.110(4) Uani 1 1 d . . . H22 H 0.7114 -0.0104 -0.0438 0.132 Uiso 1 1 calc R . . C23 C 0.6661(10) -0.0107(9) 0.0224(5) 0.123(4) Uani 1 1 d . . . H23 H 0.6362 -0.0838 0.0194 0.148 Uiso 1 1 calc R . . C24 C 0.6649(9) 0.0483(9) 0.0640(4) 0.108(4) Uani 1 1 d . . . H24 H 0.6348 0.0165 0.0893 0.129 Uiso 1 1 calc R . . C25 C 0.7096(7) 0.1584(7) 0.0688(3) 0.077(3) Uani 1 1 d . . . H25 H 0.7109 0.1988 0.0979 0.093 Uiso 1 1 calc R . . B1 B 0.9992(7) 0.1062(7) 0.2359(3) 0.053(2) Uani 1 1 d . . . C26 C 1.0444(6) 0.1328(6) 0.1844(3) 0.0501(19) Uani 1 1 d . . . C27 C 1.1443(7) 0.1016(7) 0.1780(3) 0.065(2) Uani 1 1 d . . . H27 H 1.1853 0.0630 0.2033 0.078 Uiso 1 1 calc R . . C28 C 1.1861(7) 0.1251(7) 0.1358(3) 0.069(2) Uani 1 1 d . . . H28 H 1.2538 0.1034 0.1335 0.083 Uiso 1 1 calc R . . C29 C 1.1274(7) 0.1805(7) 0.0974(3) 0.064(2) Uani 1 1 d . . . H29 H 1.1548 0.1974 0.0691 0.077 Uiso 1 1 calc R . . C30 C 1.0274(7) 0.2103(6) 0.1017(3) 0.059(2) Uani 1 1 d . . . H30 H 0.9857 0.2460 0.0759 0.070 Uiso 1 1 calc R . . C31 C 0.9886(6) 0.1875(6) 0.1443(3) 0.055(2) Uani 1 1 d . . . H31 H 0.9209 0.2100 0.1463 0.066 Uiso 1 1 calc R . . C32 C 1.0395(6) -0.0211(7) 0.2580(3) 0.060(2) Uani 1 1 d . . . C33 C 1.0558(6) -0.0454(8) 0.3067(3) 0.078(3) Uani 1 1 d . . . H33 H 1.0509 0.0141 0.3287 0.094 Uiso 1 1 calc R . . C34 C 1.0802(8) -0.1586(12) 0.3249(4) 0.114(4) Uani 1 1 d . . . H34 H 1.0881 -0.1732 0.3583 0.137 Uiso 1 1 calc R . . C35 C 1.0918(8) -0.2456(10) 0.2927(6) 0.109(4) Uani 1 1 d . . . H35 H 1.1110 -0.3190 0.3043 0.131 Uiso 1 1 calc R . . C36 C 1.0757(7) -0.2256(9) 0.2446(5) 0.100(3) Uani 1 1 d . . . H36 H 1.0802 -0.2857 0.2227 0.120 Uiso 1 1 calc R . . C37 C 1.0520(6) -0.1137(7) 0.2275(3) 0.076(3) Uani 1 1 d . . . H37 H 1.0442 -0.1006 0.1940 0.091 Uiso 1 1 calc R . . C38 C 0.8734(6) 0.1059(6) 0.2261(2) 0.0501(19) Uani 1 1 d . . . C39 C 0.8135(7) 0.2073(6) 0.2196(3) 0.060(2) Uani 1 1 d . . . H39 H 0.8476 0.2778 0.2244 0.072 Uiso 1 1 calc R . . C40 C 0.7077(7) 0.2087(8) 0.2067(3) 0.071(2) Uani 1 1 d . . . H40 H 0.6726 0.2787 0.2031 0.085 Uiso 1 1 calc R . . C41 C 0.6533(7) 0.1060(9) 0.1990(3) 0.069(2) Uani 1 1 d . . . H41 H 0.5819 0.1058 0.1897 0.083 Uiso 1 1 calc R . . C42 C 0.7087(7) 0.0034(7) 0.2057(3) 0.067(2) Uani 1 1 d . . . H42 H 0.6740 -0.0667 0.2011 0.080 Uiso 1 1 calc R . . C43 C 0.8148(7) 0.0046(6) 0.2191(3) 0.055(2) Uani 1 1 d . . . H43 H 0.8491 -0.0658 0.2236 0.066 Uiso 1 1 calc R . . C44 C 1.0451(6) 0.2061(6) 0.2767(3) 0.055(2) Uani 1 1 d . . . C45 C 0.9886(7) 0.2588(7) 0.3084(3) 0.068(2) Uani 1 1 d . . . H45 H 0.9183 0.2422 0.3058 0.081 Uiso 1 1 calc R . . C46 C 1.0316(9) 0.3364(7) 0.3446(3) 0.081(3) Uani 1 1 d . . . H46 H 0.9896 0.3691 0.3652 0.097 Uiso 1 1 calc R . . C47 C 1.1323(10) 0.3644(8) 0.3498(4) 0.094(3) Uani 1 1 d . . . H47 H 1.1606 0.4162 0.3738 0.113 Uiso 1 1 calc R . . C48 C 1.1919(8) 0.3152(10) 0.3193(4) 0.114(4) Uani 1 1 d . . . H48 H 1.2621 0.3328 0.3225 0.137 Uiso 1 1 calc R . . C49 C 1.1486(8) 0.2384(8) 0.2832(3) 0.085(3) Uani 1 1 d . . . H49 H 1.1912 0.2074 0.2624 0.102 Uiso 1 1 calc R . . OW1 O 0.6939(15) 0.3971(17) -0.0883(7) 0.173(7) Uiso 0.50 1 d P . . 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 0.0700(8) 0.0365(7) 0.0642(7) -0.0029(5) 0.0156(5) -0.0006(6) O1 0.078(4) 0.044(3) 0.069(3) -0.005(3) 0.014(3) -0.009(3) O2 0.060(3) 0.034(3) 0.072(3) -0.006(3) 0.014(3) -0.016(2) N1 0.074(5) 0.028(4) 0.071(5) -0.006(3) 0.015(4) -0.006(3) N2 0.051(4) 0.034(4) 0.052(4) 0.000(3) 0.006(3) 0.002(3) N3 0.065(5) 0.055(4) 0.090(6) -0.017(4) 0.019(5) -0.005(4) N4 0.069(5) 0.038(4) 0.077(4) -0.008(3) 0.023(4) -0.001(4) N5 0.088(5) 0.045(4) 0.062(4) -0.011(3) 0.015(4) -0.002(4) C1 0.084(7) 0.037(5) 0.106(7) -0.011(4) 0.017(7) 0.002(5) C2 0.100(9) 0.065(7) 0.136(10) -0.011(7) -0.027(8) 0.007(6) C3 0.135(12) 0.050(6) 0.122(11) -0.008(7) -0.037(9) 0.007(7) C4 0.157(11) 0.038(5) 0.079(7) -0.004(5) -0.015(8) -0.010(7) C5 0.112(9) 0.031(5) 0.067(7) -0.003(4) 0.007(6) -0.008(5) C6 0.136(10) 0.048(6) 0.066(6) 0.002(4) 0.026(6) -0.012(6) C7 0.117(8) 0.047(5) 0.071(6) -0.008(4) 0.037(5) -0.005(5) C8 0.067(6) 0.044(5) 0.055(5) -0.007(4) 0.004(4) 0.011(4) C9 0.102(7) 0.042(6) 0.068(6) -0.005(4) 0.014(5) -0.005(5) C10 0.125(9) 0.049(6) 0.090(7) -0.005(5) 0.023(6) -0.018(6) C11 0.120(8) 0.064(7) 0.079(6) -0.005(5) 0.034(5) -0.020(6) C12 0.078(6) 0.044(5) 0.069(5) -0.003(4) 0.021(5) 0.001(5) C13 0.100(9) 0.066(6) 0.095(7) -0.009(5) 0.042(6) -0.008(6) C14 0.055(7) 0.051(6) 0.141(10) -0.018(6) 0.016(7) 0.001(5) C15 0.097(11) 0.105(10) 0.157(12) -0.037(9) 0.020(8) -0.005(8) C16 0.091(10) 0.101(10) 0.208(17) -0.044(11) -0.018(11) 0.037(8) C17 0.109(11) 0.099(9) 0.131(10) -0.016(7) -0.030(9) 0.033(8) C18 0.101(9) 0.071(7) 0.096(8) -0.010(6) 0.004(6) -0.005(6) C19 0.055(5) 0.045(5) 0.051(5) -0.019(4) -0.003(4) -0.001(4) C20 0.064(6) 0.046(5) 0.068(6) -0.007(5) -0.005(4) 0.004(4) C21 0.114(8) 0.060(6) 0.075(6) -0.010(5) -0.007(5) 0.001(6) C22 0.184(12) 0.061(7) 0.080(7) -0.031(6) 0.000(7) -0.014(7) C23 0.192(13) 0.058(7) 0.108(9) -0.006(7) -0.014(9) -0.034(7) C24 0.153(10) 0.072(7) 0.096(8) -0.018(6) 0.013(7) -0.047(7) C25 0.104(7) 0.054(6) 0.069(6) -0.010(5) -0.001(5) -0.009(5) B1 0.052(6) 0.033(5) 0.074(6) -0.004(4) 0.007(4) -0.001(5) C26 0.053(5) 0.024(4) 0.071(5) -0.004(4) 0.004(4) 0.004(4) C27 0.067(7) 0.060(5) 0.064(6) -0.001(4) -0.001(5) 0.011(5) C28 0.063(6) 0.061(6) 0.083(6) -0.013(5) 0.014(5) 0.000(5) C29 0.072(7) 0.048(5) 0.071(6) -0.004(4) 0.011(5) -0.006(5) C30 0.062(6) 0.037(5) 0.073(6) 0.003(4) 0.001(4) -0.003(4) C31 0.059(5) 0.030(4) 0.073(6) -0.003(4) 0.002(5) 0.003(4) C32 0.052(5) 0.042(5) 0.082(6) 0.011(5) 0.000(4) 0.009(4) C33 0.073(6) 0.065(6) 0.098(7) 0.018(5) 0.014(5) 0.016(5) C34 0.105(9) 0.110(10) 0.122(9) 0.066(9) 0.003(7) 0.007(8) C35 0.067(8) 0.060(8) 0.197(14) 0.040(9) 0.004(8) 0.000(6) C36 0.069(7) 0.052(7) 0.173(12) 0.005(7) 0.004(7) -0.002(5) C37 0.075(7) 0.038(5) 0.112(7) 0.007(5) 0.003(5) 0.003(5) C38 0.052(5) 0.040(5) 0.058(5) 0.004(4) 0.009(4) 0.008(4) C39 0.054(6) 0.040(5) 0.082(6) 0.005(4) -0.001(4) -0.006(5) C40 0.081(8) 0.059(6) 0.072(6) -0.001(4) 0.008(5) 0.014(6) C41 0.057(6) 0.083(7) 0.065(5) 0.000(5) 0.002(4) -0.001(6) C42 0.073(7) 0.053(6) 0.075(6) 0.000(4) 0.013(5) -0.015(5) C43 0.058(6) 0.038(5) 0.070(5) -0.004(4) 0.014(4) -0.005(4) C44 0.051(6) 0.040(5) 0.076(5) 0.002(4) 0.013(4) 0.001(4) C45 0.081(6) 0.046(5) 0.077(6) 0.003(5) 0.012(5) -0.008(5) C46 0.116(9) 0.053(6) 0.072(6) -0.015(5) 0.010(5) -0.011(6) C47 0.108(9) 0.076(7) 0.095(7) -0.026(6) 0.000(7) -0.049(7) C48 0.082(8) 0.137(10) 0.125(9) -0.042(8) 0.023(7) -0.044(7) C49 0.077(8) 0.083(7) 0.097(7) -0.026(6) 0.016(5) -0.015(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.804(5) . ? Fe1 O2 1.905(4) . ? Fe1 N2 1.944(5) . ? Fe1 N3 1.946(7) . ? Fe1 N1 1.968(7) . ? Fe1 N4 1.999(6) . ? O1 N5 1.421(7) . ? O2 C19 1.306(8) . ? N1 C1 1.325(10) . ? N1 C5 1.330(10) . ? N2 C12 1.328(9) . ? N2 C8 1.339(8) . ? N3 C14 1.338(11) . ? N3 C18 1.343(11) . ? N4 C13 1.452(10) . ? N4 C7 1.495(9) . ? N4 C6 1.497(10) . ? N5 C19 1.291(9) . ? C1 C2 1.377(12) . ? C2 C3 1.359(14) . ? C3 C4 1.385(14) . ? C4 C5 1.391(13) . ? C5 C6 1.481(12) . ? C7 C8 1.485(10) . ? C8 C9 1.393(10) . ? C9 C10 1.362(11) . ? C10 C11 1.372(11) . ? C11 C12 1.389(11) . ? C13 C14 1.505(12) . ? C14 C15 1.373(14) . ? C15 C16 1.374(16) . ? C16 C17 1.344(16) . ? C17 C18 1.404(14) . ? C19 C20 1.493(10) . ? C20 C25 1.371(10) . ? C20 C21 1.387(10) . ? C21 C22 1.413(12) . ? C22 C23 1.370(13) . ? C23 C24 1.342(13) . ? C24 C25 1.400(12) . ? B1 C38 1.624(11) . ? B1 C26 1.652(11) . ? B1 C32 1.652(11) . ? B1 C44 1.666(11) . ? C26 C27 1.390(10) . ? C26 C31 1.388(9) . ? C27 C28 1.390(10) . ? C28 C29 1.373(10) . ? C29 C30 1.372(10) . ? C30 C31 1.377(9) . ? C32 C33 1.362(10) . ? C32 C37 1.392(11) . ? C33 C34 1.424(13) . ? C34 C35 1.370(15) . ? C35 C36 1.339(14) . ? C36 C37 1.398(12) . ? C38 C43 1.399(10) . ? C38 C39 1.407(10) . ? C39 C40 1.374(10) . ? C40 C41 1.385(11) . ? C41 C42 1.389(11) . ? C42 C43 1.379(10) . ? C44 C45 1.372(10) . ? C44 C49 1.387(11) . ? C45 C46 1.399(11) . ? C46 C47 1.341(12) . ? C47 C48 1.357(13) . ? C48 C49 1.394(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O2 84.6(2) . . ? O1 Fe1 N2 97.0(2) . . ? O2 Fe1 N2 178.4(2) . . ? O1 Fe1 N3 95.4(3) . . ? O2 Fe1 N3 89.6(2) . . ? N2 Fe1 N3 89.7(2) . . ? O1 Fe1 N1 99.1(3) . . ? O2 Fe1 N1 93.3(2) . . ? N2 Fe1 N1 87.0(2) . . ? N3 Fe1 N1 165.4(3) . . ? O1 Fe1 N4 177.0(3) . . ? O2 Fe1 N4 93.1(2) . . ? N2 Fe1 N4 85.3(2) . . ? N3 Fe1 N4 82.7(3) . . ? N1 Fe1 N4 82.8(3) . . ? N5 O1 Fe1 113.8(4) . . ? C19 O2 Fe1 108.1(4) . . ? C1 N1 C5 119.1(8) . . ? C1 N1 Fe1 126.9(7) . . ? C5 N1 Fe1 113.9(6) . . ? C12 N2 C8 119.9(6) . . ? C12 N2 Fe1 124.8(5) . . ? C8 N2 Fe1 115.2(5) . . ? C14 N3 C18 119.5(9) . . ? C14 N3 Fe1 113.4(7) . . ? C18 N3 Fe1 127.0(7) . . ? C13 N4 C7 112.3(6) . . ? C13 N4 C6 112.1(7) . . ? C7 N4 C6 111.8(6) . . ? C13 N4 Fe1 105.6(5) . . ? C7 N4 Fe1 109.9(4) . . ? C6 N4 Fe1 104.6(5) . . ? C19 N5 O1 109.4(5) . . ? N1 C1 C2 121.5(10) . . ? C3 C2 C1 119.7(12) . . ? C2 C3 C4 119.9(11) . . ? C3 C4 C5 116.9(11) . . ? N1 C5 C4 122.8(10) . . ? N1 C5 C6 114.7(8) . . ? C4 C5 C6 122.5(10) . . ? C5 C6 N4 109.6(7) . . ? C8 C7 N4 112.5(6) . . ? N2 C8 C9 120.7(7) . . ? N2 C8 C7 117.0(7) . . ? C9 C8 C7 122.2(7) . . ? C10 C9 C8 118.7(8) . . ? C9 C10 C11 120.9(8) . . ? C10 C11 C12 117.5(8) . . ? N2 C12 C11 122.2(7) . . ? N4 C13 C14 107.6(7) . . ? N3 C14 C15 122.7(11) . . ? N3 C14 C13 114.4(9) . . ? C15 C14 C13 122.8(11) . . ? C16 C15 C14 117.7(12) . . ? C17 C16 C15 120.6(13) . . ? C16 C17 C18 119.7(12) . . ? N3 C18 C17 119.7(10) . . ? N5 C19 O2 123.4(7) . . ? N5 C19 C20 120.3(7) . . ? O2 C19 C20 116.2(7) . . ? C25 C20 C21 119.3(8) . . ? C25 C20 C19 120.2(7) . . ? C21 C20 C19 120.5(8) . . ? C20 C21 C22 119.6(9) . . ? C23 C22 C21 118.9(9) . . ? C24 C23 C22 122.2(10) . . ? C23 C24 C25 119.2(10) . . ? C20 C25 C24 120.9(8) . . ? C38 B1 C26 109.8(6) . . ? C38 B1 C32 108.5(6) . . ? C26 B1 C32 110.7(6) . . ? C38 B1 C44 111.6(6) . . ? C26 B1 C44 108.5(6) . . ? C32 B1 C44 107.7(6) . . ? C27 C26 C31 114.1(7) . . ? C27 C26 B1 121.6(7) . . ? C31 C26 B1 124.3(7) . . ? C26 C27 C28 123.2(7) . . ? C29 C28 C27 120.0(8) . . ? C30 C29 C28 118.6(8) . . ? C29 C30 C31 120.1(7) . . ? C30 C31 C26 123.9(7) . . ? C33 C32 C37 115.3(7) . . ? C33 C32 B1 123.1(7) . . ? C37 C32 B1 121.4(7) . . ? C32 C33 C34 122.4(9) . . ? C35 C34 C33 119.0(10) . . ? C36 C35 C34 120.4(11) . . ? C35 C36 C37 119.5(11) . . ? C32 C37 C36 123.2(9) . . ? C43 C38 C39 113.6(7) . . ? C43 C38 B1 122.9(7) . . ? C39 C38 B1 123.3(7) . . ? C40 C39 C38 124.1(7) . . ? C39 C40 C41 120.2(8) . . ? C40 C41 C42 118.0(8) . . ? C43 C42 C41 120.6(7) . . ? C42 C43 C38 123.5(7) . . ? C45 C44 C49 113.7(7) . . ? C45 C44 B1 124.8(7) . . ? C49 C44 B1 121.4(7) . . ? C44 C45 C46 123.2(8) . . ? C47 C46 C45 121.0(9) . . ? C46 C47 C48 118.3(9) . . ? C47 C48 C49 120.4(10) . . ? C44 C49 C48 123.3(9) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 20.84 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.359 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.067