# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_mait3 _database_code_depnum_ccdc_archive 'CCDC 906827' #TrackingRef 'web_deposit_cif_file_0_OlafWalter_1357832893.mait3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H35 Fe N9 O5' _chemical_formula_weight 645.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6875(7) _cell_length_b 10.7398(8) _cell_length_c 15.2491(11) _cell_angle_alpha 100.4530(10) _cell_angle_beta 97.6860(10) _cell_angle_gamma 91.2450(10) _cell_volume 1544.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6499 _cell_measurement_theta_min 2.567 _cell_measurement_theta_max 28.115 _exptl_crystal_description quader _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 676 _exptl_absorpt_coefficient_mu 0.542 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8453 _exptl_absorpt_correction_T_max 0.9656 _exptl_absorpt_process_details (sadabs) _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex II Quazar' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23122 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_unetI/netI 0.0342 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 28.58 _reflns_number_total 7165 _reflns_number_gt 5947 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II (Bruker, 2007)' _computing_cell_refinement 'APEX II (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'WINRAY (Soltek, 1997), ORTEP (Farrugia, 1997)' _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^)+(0.0635P)^2^+0.8614P] 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 7165 _refine_ls_number_parameters 413 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.1159 _refine_ls_wR_factor_gt 0.1094 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _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 0.06233(3) 0.28523(2) 0.315807(18) 0.01904(9) Uani 1 1 d . . . O1 O 0.03095(14) 0.22673(12) 0.43371(9) 0.0238(3) Uani 1 1 d . . . O2 O 0.07647(15) 0.15473(13) 0.56319(9) 0.0250(3) Uani 1 1 d . . . O3 O -0.09674(15) 0.40520(12) 0.28654(9) 0.0249(3) Uani 1 1 d . . . O4 O -0.21604(16) 0.54895(13) 0.22122(10) 0.0306(3) Uani 1 1 d . . . O5 O 0.6347(2) 0.3155(2) -0.20692(14) 0.0638(6) Uani 1 1 d . . . N1 N 0.24601(16) 0.17996(14) 0.31892(11) 0.0205(3) Uani 1 1 d . . . N2 N 0.14260(17) 0.32222(14) 0.20079(11) 0.0202(3) Uani 1 1 d . . . N3 N 0.3737(2) 0.00405(19) 0.57998(13) 0.0342(4) Uani 1 1 d . . . N4 N -0.0605(2) 0.64997(17) 0.06481(12) 0.0345(4) Uani 1 1 d . . . N5 N -0.06667(18) 0.12271(15) 0.23844(11) 0.0249(4) Uani 1 1 d . . . N6 N -0.20071(18) -0.05250(15) 0.20109(12) 0.0265(4) Uani 1 1 d . . . N7 N 0.17886(18) 0.45437(15) 0.40138(12) 0.0258(4) Uani 1 1 d . . . N8 N 0.33387(19) 0.61663(16) 0.44303(12) 0.0300(4) Uani 1 1 d . . . N9 N 0.6964(2) 0.2783(2) -0.06516(15) 0.0432(5) Uani 1 1 d . . . C1 C 0.1102(2) 0.17112(17) 0.48316(13) 0.0214(4) Uani 1 1 d . . . C2 C 0.2399(2) 0.12002(17) 0.46397(13) 0.0211(4) Uani 1 1 d . . . C3 C 0.2989(2) 0.12549(17) 0.38496(13) 0.0210(4) Uani 1 1 d . . . H3 H 0.3848 0.0860 0.3792 0.031(4) Uiso 1 1 calc R . . C4 C 0.3132(2) 0.05648(18) 0.52864(13) 0.0247(4) Uani 1 1 d . . . C5 C -0.0540(2) 0.2071(2) 0.58596(14) 0.0280(4) Uani 1 1 d . . . H5A H -0.1325 0.1674 0.5404 0.038(3) Uiso 1 1 calc R . . H5B H -0.0511 0.2996 0.5871 0.038(3) Uiso 1 1 calc R . . C6 C -0.0736(2) 0.1808(2) 0.67701(14) 0.0318(5) Uani 1 1 d . . . H6A H -0.0764 0.0891 0.6752 0.053(3) Uiso 1 1 calc R . . H6B H -0.1614 0.2151 0.6936 0.053(3) Uiso 1 1 calc R . . H6C H 0.0042 0.2211 0.7217 0.053(3) Uiso 1 1 calc R . . C7 C 0.3116(2) 0.17300(17) 0.24053(13) 0.0217(4) Uani 1 1 d . . . C8 C 0.4230(2) 0.0970(2) 0.22024(14) 0.0296(5) Uani 1 1 d . . . H8 H 0.4640 0.0491 0.2627 0.032(3) Uiso 1 1 calc R . . C9 C 0.4738(2) 0.0909(2) 0.13915(15) 0.0336(5) Uani 1 1 d . . . H9 H 0.5507 0.0402 0.1269 0.032(3) Uiso 1 1 calc R . . C10 C 0.4138(2) 0.1579(2) 0.07574(14) 0.0304(5) Uani 1 1 d . . . H10 H 0.4475 0.1512 0.0194 0.032(3) Uiso 1 1 calc R . . C11 C 0.3045(2) 0.23473(18) 0.09450(13) 0.0250(4) Uani 1 1 d . . . H11 H 0.2630 0.2802 0.0506 0.032(3) Uiso 1 1 calc R . . C12 C 0.2546(2) 0.24611(17) 0.17702(13) 0.0204(4) Uani 1 1 d . . . C13 C -0.1067(2) 0.47501(17) 0.22983(13) 0.0226(4) Uani 1 1 d . . . C14 C -0.0109(2) 0.48738(17) 0.16842(13) 0.0220(4) Uani 1 1 d . . . C15 C 0.1054(2) 0.41180(17) 0.15618(13) 0.0210(4) Uani 1 1 d . . . H15 H 0.1608 0.4275 0.1120 0.031(4) Uiso 1 1 calc R . . C16 C -0.0379(2) 0.57784(18) 0.11138(13) 0.0254(4) Uani 1 1 d . . . C17 C -0.3215(2) 0.5415(2) 0.27935(16) 0.0331(5) Uani 1 1 d . . . H17A H -0.3771 0.6180 0.2818 0.038(3) Uiso 1 1 calc R . . H17B H -0.2755 0.5399 0.3411 0.038(3) Uiso 1 1 calc R . . C18 C -0.4160(3) 0.4262(3) 0.2467(2) 0.0505(7) Uani 1 1 d . . . H18A H -0.4613 0.4275 0.1854 0.053(3) Uiso 1 1 calc R . . H18B H -0.4871 0.4252 0.2866 0.053(3) Uiso 1 1 calc R . . H18C H -0.3617 0.3503 0.2466 0.053(3) Uiso 1 1 calc R . . C19 C -0.1615(2) 0.05262(18) 0.26357(14) 0.0263(4) Uani 1 1 d . . . H19 H -0.1980 0.0734 0.3189 0.041(4) Uiso 1 1 calc R . . C20 C -0.1260(2) -0.0501(2) 0.13161(15) 0.0341(5) Uani 1 1 d . . . H20 H -0.1305 -0.1115 0.0778 0.041(4) Uiso 1 1 calc R . . C21 C -0.0440(2) 0.0579(2) 0.15514(15) 0.0330(5) Uani 1 1 d . . . H21 H 0.0198 0.0851 0.1195 0.041(4) Uiso 1 1 calc R . . C22 C -0.2985(2) -0.1543(2) 0.20833(18) 0.0378(5) Uani 1 1 d . . . H22A H -0.3221 -0.1419 0.2697 0.063(5) Uiso 1 1 calc R . . H22B H -0.2555 -0.2360 0.1945 0.063(5) Uiso 1 1 calc R . . H22C H -0.3834 -0.1533 0.1656 0.063(5) Uiso 1 1 calc R . . C23 C 0.2679(2) 0.52785(19) 0.37629(15) 0.0304(5) Uani 1 1 d . . . H23 H 0.2851 0.5195 0.3156 0.056(5) Uiso 1 1 calc R . . C24 C 0.2809(4) 0.6020(3) 0.5196(2) 0.0577(8) Uani 1 1 d . . . H24 H 0.3057 0.6491 0.5789 0.056(5) Uiso 1 1 calc R . . C25 C 0.1797(3) 0.4991(3) 0.4894(2) 0.0538(7) Uani 1 1 d . . . H25 H 0.1214 0.4671 0.5263 0.056(5) Uiso 1 1 calc R . . C26 C 0.4392(3) 0.7086(2) 0.4334(2) 0.0502(7) Uani 1 1 d . . . H26A H 0.5312 0.6840 0.4580 0.062(5) Uiso 1 1 calc R . . H26B H 0.4202 0.7922 0.4662 0.062(5) Uiso 1 1 calc R . . H26C H 0.4378 0.7119 0.3695 0.062(5) Uiso 1 1 calc R . . C27 C 0.6921(3) 0.2533(3) -0.1537(2) 0.0512(7) Uani 1 1 d . . . H27 H 0.7377 0.1804 -0.1784 0.066(10) Uiso 1 1 calc R . . C28 C 0.6336(4) 0.3906(3) -0.0230(2) 0.0630(8) Uani 1 1 d . . . H28A H 0.7067 0.4503 0.0128 0.098(5) Uiso 1 1 calc R . . H28B H 0.5691 0.3671 0.0162 0.098(5) Uiso 1 1 calc R . . H28C H 0.5824 0.4307 -0.0696 0.098(5) Uiso 1 1 calc R . . C29 C 0.7761(3) 0.2045(3) -0.0062(2) 0.0640(9) Uani 1 1 d . . . H29A H 0.8079 0.1286 -0.0427 0.098(5) Uiso 1 1 calc R . . H29B H 0.7170 0.1793 0.0355 0.098(5) Uiso 1 1 calc R . . H29C H 0.8571 0.2560 0.0280 0.098(5) 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 0.01954(15) 0.01904(14) 0.02033(15) 0.00715(10) 0.00396(11) 0.00427(10) O1 0.0223(7) 0.0284(7) 0.0239(7) 0.0110(5) 0.0055(6) 0.0074(5) O2 0.0229(7) 0.0330(7) 0.0234(7) 0.0123(6) 0.0081(6) 0.0087(6) O3 0.0261(7) 0.0244(7) 0.0286(7) 0.0120(6) 0.0087(6) 0.0076(5) O4 0.0310(8) 0.0315(7) 0.0375(8) 0.0182(6) 0.0154(7) 0.0156(6) O5 0.0666(14) 0.0835(15) 0.0480(12) 0.0263(11) 0.0117(11) 0.0146(12) N1 0.0203(8) 0.0211(7) 0.0220(8) 0.0069(6) 0.0049(6) 0.0042(6) N2 0.0205(8) 0.0193(7) 0.0217(8) 0.0053(6) 0.0038(6) 0.0049(6) N3 0.0289(10) 0.0478(11) 0.0324(10) 0.0191(8) 0.0098(8) 0.0147(8) N4 0.0478(12) 0.0311(9) 0.0289(10) 0.0124(8) 0.0100(9) 0.0151(8) N5 0.0258(9) 0.0233(8) 0.0263(9) 0.0068(6) 0.0022(7) 0.0018(6) N6 0.0237(9) 0.0209(8) 0.0340(9) 0.0059(7) -0.0002(7) 0.0017(6) N7 0.0262(9) 0.0231(8) 0.0276(9) 0.0024(6) 0.0051(7) 0.0008(6) N8 0.0283(10) 0.0288(9) 0.0300(9) 0.0000(7) 0.0017(8) -0.0005(7) N9 0.0392(12) 0.0530(12) 0.0408(12) 0.0144(10) 0.0098(10) 0.0028(9) C1 0.0232(10) 0.0201(8) 0.0216(9) 0.0051(7) 0.0042(8) 0.0003(7) C2 0.0213(10) 0.0217(8) 0.0214(9) 0.0070(7) 0.0024(7) 0.0030(7) C3 0.0182(9) 0.0208(8) 0.0247(9) 0.0049(7) 0.0034(7) 0.0036(7) C4 0.0236(10) 0.0284(10) 0.0244(10) 0.0076(8) 0.0073(8) 0.0048(8) C5 0.0240(11) 0.0348(11) 0.0290(11) 0.0103(8) 0.0100(9) 0.0104(8) C6 0.0312(12) 0.0391(11) 0.0288(11) 0.0108(9) 0.0106(9) 0.0103(9) C7 0.0205(9) 0.0223(9) 0.0234(9) 0.0053(7) 0.0045(8) 0.0034(7) C8 0.0293(11) 0.0352(11) 0.0292(11) 0.0134(9) 0.0095(9) 0.0156(9) C9 0.0333(12) 0.0390(12) 0.0330(12) 0.0105(9) 0.0129(10) 0.0196(9) C10 0.0332(12) 0.0370(11) 0.0237(10) 0.0062(8) 0.0109(9) 0.0111(9) C11 0.0268(10) 0.0283(10) 0.0215(9) 0.0077(7) 0.0045(8) 0.0053(8) C12 0.0196(9) 0.0201(8) 0.0221(9) 0.0041(7) 0.0044(7) 0.0023(7) C13 0.0232(10) 0.0195(8) 0.0253(10) 0.0046(7) 0.0033(8) 0.0044(7) C14 0.0261(10) 0.0202(8) 0.0216(9) 0.0075(7) 0.0044(8) 0.0053(7) C15 0.0228(10) 0.0217(8) 0.0195(9) 0.0052(7) 0.0047(7) 0.0026(7) C16 0.0292(11) 0.0249(9) 0.0236(10) 0.0047(8) 0.0070(8) 0.0094(8) C17 0.0314(12) 0.0362(11) 0.0390(12) 0.0154(9) 0.0168(10) 0.0156(9) C18 0.0313(14) 0.0672(18) 0.0540(17) 0.0139(14) 0.0067(12) -0.0024(12) C19 0.0254(10) 0.0228(9) 0.0314(11) 0.0063(8) 0.0051(9) 0.0035(7) C20 0.0372(13) 0.0318(11) 0.0312(11) 0.0014(9) 0.0033(10) 0.0000(9) C21 0.0379(13) 0.0315(11) 0.0291(11) 0.0032(9) 0.0068(10) -0.0031(9) C22 0.0340(12) 0.0230(10) 0.0562(15) 0.0090(10) 0.0037(11) -0.0028(9) C23 0.0262(11) 0.0272(10) 0.0351(12) 0.0008(8) 0.0018(9) -0.0010(8) C24 0.083(2) 0.0520(16) 0.0433(16) 0.0151(13) 0.0172(15) 0.0181(15) C25 0.066(2) 0.0501(15) 0.0462(16) 0.0093(12) 0.0105(14) -0.0040(14) C26 0.0337(14) 0.0413(13) 0.0704(19) -0.0067(13) 0.0144(13) -0.0108(11) C27 0.0487(17) 0.0542(16) 0.0548(17) 0.0108(13) 0.0211(14) 0.0058(13) C28 0.083(2) 0.0531(17) 0.0548(18) 0.0032(14) 0.0272(17) 0.0001(16) C29 0.0485(18) 0.083(2) 0.070(2) 0.0430(18) 0.0061(16) 0.0008(16) _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 2.0657(14) . ? Fe1 O3 2.0845(13) . ? Fe1 N2 2.1078(16) . ? Fe1 N1 2.1286(16) . ? Fe1 N5 2.1826(16) . ? Fe1 N7 2.2213(16) . ? O1 C1 1.243(2) . ? O2 C1 1.345(2) . ? O2 C5 1.453(2) . ? O3 C13 1.239(2) . ? O4 C13 1.344(2) . ? O4 C17 1.449(3) . ? O5 C27 1.227(3) . ? N1 C3 1.307(2) . ? N1 C7 1.418(2) . ? N2 C15 1.306(2) . ? N2 C12 1.419(2) . ? N3 C4 1.151(3) . ? N4 C16 1.148(3) . ? N5 C19 1.314(3) . ? N5 C21 1.381(3) . ? N6 C19 1.349(3) . ? N6 C20 1.364(3) . ? N6 C22 1.460(3) . ? N7 C23 1.297(3) . ? N7 C25 1.339(3) . ? N8 C23 1.342(3) . ? N8 C24 1.369(3) . ? N8 C26 1.445(3) . ? N9 C27 1.323(4) . ? N9 C28 1.447(4) . ? N9 C29 1.460(4) . ? C1 C2 1.426(3) . ? C2 C3 1.411(3) . ? C2 C4 1.421(3) . ? C3 H3 0.9500 . ? C5 C6 1.501(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.401(3) . ? C7 C12 1.418(3) . ? C8 C9 1.382(3) . ? C8 H8 0.9500 . ? C9 C10 1.382(3) . ? C9 H9 0.9500 . ? C10 C11 1.385(3) . ? C10 H10 0.9500 . ? C11 C12 1.393(3) . ? C11 H11 0.9500 . ? C13 C14 1.424(3) . ? C14 C15 1.416(3) . ? C14 C16 1.423(3) . ? C15 H15 0.9500 . ? C17 C18 1.492(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19 0.9500 . ? C20 C21 1.356(3) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23 0.9500 . ? C24 C25 1.429(4) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 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 O1 Fe1 O3 107.22(5) . . ? O1 Fe1 N2 165.41(6) . . ? O3 Fe1 N2 87.19(6) . . ? O1 Fe1 N1 87.13(6) . . ? O3 Fe1 N1 165.42(6) . . ? N2 Fe1 N1 78.37(6) . . ? O1 Fe1 N5 89.82(6) . . ? O3 Fe1 N5 90.04(6) . . ? N2 Fe1 N5 92.45(6) . . ? N1 Fe1 N5 92.57(6) . . ? O1 Fe1 N7 87.17(6) . . ? O3 Fe1 N7 87.20(6) . . ? N2 Fe1 N7 91.42(6) . . ? N1 Fe1 N7 91.10(6) . . ? N5 Fe1 N7 175.13(6) . . ? C1 O1 Fe1 129.45(13) . . ? C1 O2 C5 115.64(15) . . ? C13 O3 Fe1 128.49(13) . . ? C13 O4 C17 117.39(16) . . ? C3 N1 C7 120.59(16) . . ? C3 N1 Fe1 125.73(13) . . ? C7 N1 Fe1 113.68(12) . . ? C15 N2 C12 119.63(16) . . ? C15 N2 Fe1 126.15(13) . . ? C12 N2 Fe1 114.02(12) . . ? C19 N5 C21 104.93(17) . . ? C19 N5 Fe1 129.75(14) . . ? C21 N5 Fe1 124.33(14) . . ? C19 N6 C20 107.36(17) . . ? C19 N6 C22 126.62(19) . . ? C20 N6 C22 125.92(18) . . ? C23 N7 C25 105.0(2) . . ? C23 N7 Fe1 126.20(14) . . ? C25 N7 Fe1 128.71(17) . . ? C23 N8 C24 106.5(2) . . ? C23 N8 C26 125.5(2) . . ? C24 N8 C26 128.0(2) . . ? C27 N9 C28 119.7(3) . . ? C27 N9 C29 122.4(3) . . ? C28 N9 C29 117.6(3) . . ? O1 C1 O2 120.04(17) . . ? O1 C1 C2 126.10(18) . . ? O2 C1 C2 113.86(16) . . ? C3 C2 C4 117.83(17) . . ? C3 C2 C1 124.90(17) . . ? C4 C2 C1 117.26(17) . . ? N1 C3 C2 125.93(18) . . ? N1 C3 H3 117.0 . . ? C2 C3 H3 117.0 . . ? N3 C4 C2 178.9(2) . . ? O2 C5 C6 108.12(16) . . ? O2 C5 H5A 110.1 . . ? C6 C5 H5A 110.1 . . ? O2 C5 H5B 110.1 . . ? C6 C5 H5B 110.1 . . ? H5A C5 H5B 108.4 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 N1 125.26(17) . . ? C8 C7 C12 118.47(18) . . ? N1 C7 C12 116.22(16) . . ? C9 C8 C7 120.75(19) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 120.53(19) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C9 C10 C11 119.85(19) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C10 C11 C12 120.72(19) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C11 C12 C7 119.55(17) . . ? C11 C12 N2 123.92(17) . . ? C7 C12 N2 116.43(16) . . ? O3 C13 O4 120.62(18) . . ? O3 C13 C14 126.46(18) . . ? O4 C13 C14 112.92(17) . . ? C15 C14 C16 117.15(17) . . ? C15 C14 C13 125.01(17) . . ? C16 C14 C13 117.76(17) . . ? N2 C15 C14 125.12(18) . . ? N2 C15 H15 117.4 . . ? C14 C15 H15 117.4 . . ? N4 C16 C14 179.3(2) . . ? O4 C17 C18 111.62(19) . . ? O4 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? O4 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N5 C19 N6 111.71(19) . . ? N5 C19 H19 124.1 . . ? N6 C19 H19 124.1 . . ? C21 C20 N6 105.86(19) . . ? C21 C20 H20 127.1 . . ? N6 C20 H20 127.1 . . ? C20 C21 N5 110.1(2) . . ? C20 C21 H21 124.9 . . ? N5 C21 H21 124.9 . . ? N6 C22 H22A 109.5 . . ? N6 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N6 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N7 C23 N8 114.5(2) . . ? N7 C23 H23 122.8 . . ? N8 C23 H23 122.8 . . ? N8 C24 C25 103.7(2) . . ? N8 C24 H24 128.1 . . ? C25 C24 H24 128.1 . . ? N7 C25 C24 110.2(3) . . ? N7 C25 H25 124.9 . . ? C24 C25 H25 124.9 . . ? N8 C26 H26A 109.5 . . ? N8 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N8 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O5 C27 N9 126.1(3) . . ? O5 C27 H27 117.0 . . ? N9 C27 H27 117.0 . . ? N9 C28 H28A 109.5 . . ? N9 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N9 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N9 C29 H29A 109.5 . . ? N9 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N9 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.798 _refine_diff_density_min -0.580 _refine_diff_density_rms 0.059