# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. #==================================== _journal_coden_Cambridge 0182 _journal_volume ? _journal_year ? _journal_page_first ? # 1. SUBMISSION DETAILS _publ_contact_author_name 'Roland Kraemer' _publ_contact_author_address ; Prof Roland Kraemer Universitaet Heidelberg Anorganisch-Chemisches Institut Im Neuenheimer Feld 270 Heidelberg 69120 GERMANY =20 ; _publ_contact_author_email ROLAND.KRAEMER@URZ.UNI-HEIDELBERG.DE _publ_requested_coeditor_name ? #=========================================================================== #========================================================================== #======= # 2. TITLE AND AUTHOR LIST _publ_section_title ; Redox- triggered on/off coordination of a bridgehead nitrogen donor=20 in a tripodal iron complex ; loop_ _publ_author_name _publ_author_address S.Worl ; Anorganisch-Chemisches Institut Universitaet Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg ; D.Hellwinkel ; Organisch-Chemisches Institut Universitaet Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg ; H.Pritzkow ; Anorganisch-Chemisches Institut Universitaet Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg ; R.Kramer ; Anorganisch-Chemisches Institut Universitaet Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg ; #=========================================================================== #========================================================================== #======= data_sw08 _database_code_CSD 200179 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H18 Fe N O9, 5(H2 O)' _chemical_formula_sum 'C21 H28 Fe N O14' _chemical_formula_weight 574.29 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 8.5867(10) _cell_length_b 10.2031(12) _cell_length_c 15.4545(18) _cell_angle_alpha 74.869(2) _cell_angle_beta 81.900(2) _cell_angle_gamma 75.801(2) _cell_volume 1262.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 190(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 598 _exptl_absorpt_coefficient_mu 0.669 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8482 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 190(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22077 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0353 _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 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 32.05 _reflns_number_total 8334 _reflns_number_gt 7092 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0467P)^2^+0.5263P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8334 _refine_ls_number_parameters 446 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0443 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0990 _refine_ls_wR_factor_gt 0.0929 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.008 _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 0.23683(2) 0.065498(19) 0.365771(12) 0.01469(6) Uani 1 1 d . . . O1 O 0.36597(12) -0.00511(10) 0.26968(7) 0.01845(18) Uani 1 1 d . . . O2 O 0.48973(16) -0.18024(14) 0.20888(10) 0.0390(3) Uani 1 1 d . . . O3 O 0.18821(12) 0.26299(10) 0.30939(7) 0.01921(19) Uani 1 1 d . . . O4 O 0.23894(16) 0.47010(11) 0.24712(8) 0.0295(2) Uani 1 1 d . . . O5 O 0.02868(11) 0.03298(10) 0.34855(7) 0.01900(19) Uani 1 1 d . . . O6 O -0.22966(12) 0.04187(11) 0.35082(7) 0.0216(2) Uani 1 1 d . . . O7 O 0.44945(12) 0.08048(12) 0.40449(7) 0.0225(2) Uani 1 1 d . . . O8 O 0.26808(14) -0.13324(12) 0.44892(8) 0.0255(2) Uani 1 1 d . . . O9 O 0.14980(14) 0.12407(12) 0.48284(7) 0.0233(2) Uani 1 1 d . . . O10 O 0.71888(14) -0.21878(13) 0.32512(8) 0.0272(2) Uani 1 1 d . . . O11 O 0.55799(14) -0.26393(14) 0.49334(9) 0.0292(2) Uani 1 1 d . . . O12 O -0.02599(16) 0.55849(13) 0.36804(8) 0.0289(2) Uani 1 1 d . . . O13 O -0.08546(15) 0.34080(13) 0.50902(9) 0.0290(2) Uani 1 1 d . . . O14 O 0.38653(19) 0.51187(17) 0.38713(12) 0.0432(3) Uani 1 1 d . . . N1 N 0.11215(14) 0.16877(12) 0.16204(8) 0.0172(2) Uani 1 1 d . . . C1 C 0.09339(16) 0.03602(14) 0.15788(9) 0.0176(2) Uani 1 1 d . . . C2 C 0.21507(17) -0.08473(14) 0.18158(9) 0.0182(2) Uani 1 1 d . . . C3 C 0.1928(2) -0.21097(15) 0.17113(10) 0.0242(3) Uani 1 1 d . . . C4 C 0.0505(2) -0.22062(18) 0.14288(11) 0.0307(3) Uani 1 1 d . . . C5 C -0.0707(2) -0.10227(19) 0.12257(11) 0.0304(3) Uani 1 1 d . . . C6 C -0.04903(19) 0.02593(17) 0.12829(10) 0.0239(3) Uani 1 1 d . . . C7 C 0.36742(18) -0.09152(14) 0.22171(9) 0.0204(3) Uani 1 1 d . . . C8 C 0.25577(16) 0.21313(13) 0.12332(9) 0.0173(2) Uani 1 1 d . . . C9 C 0.31492(16) 0.30349(14) 0.15867(9) 0.0179(2) Uani 1 1 d . . . C10 C 0.45104(18) 0.35197(16) 0.11487(10) 0.0236(3) Uani 1 1 d . . . C11 C 0.5341(2) 0.30638(18) 0.04058(11) 0.0289(3) Uani 1 1 d . . . C12 C 0.4779(2) 0.21395(17) 0.00737(10) 0.0277(3) Uani 1 1 d . . . C13 C 0.33842(19) 0.16977(16) 0.04758(9) 0.0228(3) Uani 1 1 d . . . C14 C 0.24250(16) 0.34949(14) 0.24293(9) 0.0187(2) Uani 1 1 d . . . C15 C -0.02571(16) 0.26911(14) 0.18297(9) 0.0190(2) Uani 1 1 d . . . C16 C -0.13292(16) 0.23610(14) 0.25850(9) 0.0186(2) Uani 1 1 d . . . C17 C -0.26546(18) 0.33906(16) 0.27783(12) 0.0264(3) Uani 1 1 d . . . C18 C -0.2901(2) 0.47342(17) 0.22464(14) 0.0334(4) Uani 1 1 d . . . C19 C -0.1857(2) 0.50494(16) 0.14902(14) 0.0339(4) Uani 1 1 d . . . C20 C -0.0560(2) 0.40382(16) 0.12803(12) 0.0274(3) Uani 1 1 d . . . C21 C -0.11040(15) 0.09562(14) 0.32226(9) 0.0167(2) Uani 1 1 d . . . H3 H 0.273(2) -0.292(2) 0.1868(13) 0.025(5) Uiso 1 1 d . . . H4 H 0.037(3) -0.308(2) 0.1375(14) 0.032(5) Uiso 1 1 d . . . H5 H -0.168(3) -0.106(2) 0.1058(15) 0.034(5) Uiso 1 1 d . . . H6 H -0.128(2) 0.107(2) 0.1092(13) 0.026(5) Uiso 1 1 d . . . H10 H 0.488(2) 0.413(2) 0.1375(13) 0.024(5) Uiso 1 1 d . . . H11 H 0.629(3) 0.335(2) 0.0125(15) 0.035(5) Uiso 1 1 d . . . H12 H 0.536(3) 0.183(2) -0.0441(15) 0.033(5) Uiso 1 1 d . . . H13 H 0.299(3) 0.112(2) 0.0250(15) 0.033(5) Uiso 1 1 d . . . H17 H -0.336(3) 0.315(2) 0.3291(15) 0.031(5) Uiso 1 1 d . . . H18 H -0.374(3) 0.542(2) 0.2372(16) 0.044(6) Uiso 1 1 d . . . H19 H -0.205(3) 0.595(2) 0.1106(15) 0.037(6) Uiso 1 1 d . . . H20 H 0.012(3) 0.423(2) 0.0790(15) 0.037(6) Uiso 1 1 d . . . H71 H 0.542(3) 0.073(3) 0.3761(17) 0.046(7) Uiso 1 1 d . . . H72 H 0.443(3) 0.131(2) 0.4379(16) 0.039(6) Uiso 1 1 d . . . H81 H 0.212(3) -0.189(2) 0.4552(15) 0.033(5) Uiso 1 1 d . . . H82 H 0.360(3) -0.181(3) 0.4622(17) 0.044(6) Uiso 1 1 d . . . H91 H 0.081(3) 0.195(3) 0.4876(17) 0.048(7) Uiso 1 1 d . . . H92 H 0.160(3) 0.073(3) 0.5330(18) 0.045(7) Uiso 1 1 d . . . H101 H 0.656(3) -0.204(3) 0.2876(18) 0.049(7) Uiso 1 1 d . . . H102 H 0.744(3) -0.146(3) 0.3182(17) 0.044(7) Uiso 1 1 d . . . H111 H 0.574(3) -0.346(3) 0.519(2) 0.060(8) Uiso 1 1 d . . . H112 H 0.615(4) -0.248(3) 0.440(2) 0.067(9) Uiso 1 1 d . . . H121 H -0.096(3) 0.613(3) 0.3443(17) 0.045(7) Uiso 1 1 d . . . H122 H 0.047(4) 0.536(3) 0.330(2) 0.063(9) Uiso 1 1 d . . . H131 H -0.056(3) 0.370(3) 0.548(2) 0.060(8) Uiso 1 1 d . . . H132 H -0.075(3) 0.401(3) 0.4606(18) 0.046(7) Uiso 1 1 d . . . H141 H 0.344(4) 0.501(4) 0.342(3) 0.090(12) Uiso 1 1 d . . . H142 H 0.331(5) 0.562(4) 0.408(3) 0.112(16) Uiso 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 0.01262(9) 0.01598(9) 0.01495(9) -0.00342(6) -0.00155(6) -0.00218(6) O1 0.0193(4) 0.0190(4) 0.0182(4) -0.0079(4) -0.0011(3) -0.0029(4) O2 0.0340(7) 0.0379(7) 0.0493(8) -0.0294(6) -0.0187(6) 0.0136(5) O3 0.0233(5) 0.0160(4) 0.0176(4) -0.0036(3) -0.0007(4) -0.0038(4) O4 0.0432(7) 0.0167(5) 0.0298(6) -0.0076(4) 0.0033(5) -0.0099(5) O5 0.0143(4) 0.0194(4) 0.0214(5) -0.0005(4) -0.0045(3) -0.0030(3) O6 0.0141(4) 0.0256(5) 0.0232(5) -0.0030(4) 0.0001(4) -0.0047(4) O7 0.0134(4) 0.0343(6) 0.0246(5) -0.0162(4) 0.0001(4) -0.0049(4) O8 0.0175(5) 0.0216(5) 0.0333(6) 0.0049(4) -0.0082(4) -0.0055(4) O9 0.0244(5) 0.0248(5) 0.0155(5) -0.0034(4) 0.0014(4) 0.0011(4) O10 0.0232(5) 0.0262(6) 0.0320(6) -0.0078(5) -0.0063(4) -0.0017(4) O11 0.0219(5) 0.0347(6) 0.0321(6) -0.0139(5) -0.0038(4) -0.0012(5) O12 0.0278(6) 0.0288(6) 0.0267(6) -0.0083(5) -0.0024(5) 0.0020(5) O13 0.0300(6) 0.0254(5) 0.0310(6) -0.0055(5) -0.0020(5) -0.0064(5) O14 0.0375(8) 0.0410(8) 0.0521(9) -0.0190(7) -0.0075(7) 0.0007(6) N1 0.0175(5) 0.0154(5) 0.0183(5) -0.0024(4) -0.0025(4) -0.0039(4) C1 0.0219(6) 0.0181(6) 0.0142(5) -0.0028(4) -0.0028(4) -0.0071(5) C2 0.0238(6) 0.0174(6) 0.0145(5) -0.0035(4) -0.0019(5) -0.0068(5) C3 0.0343(8) 0.0189(6) 0.0209(6) -0.0052(5) -0.0005(5) -0.0092(6) C4 0.0427(9) 0.0283(8) 0.0291(8) -0.0104(6) -0.0010(7) -0.0196(7) C5 0.0340(8) 0.0383(9) 0.0271(7) -0.0103(6) -0.0062(6) -0.0186(7) C6 0.0254(7) 0.0283(7) 0.0208(6) -0.0054(5) -0.0074(5) -0.0082(6) C7 0.0244(7) 0.0190(6) 0.0178(6) -0.0055(5) -0.0045(5) -0.0020(5) C8 0.0195(6) 0.0166(5) 0.0150(5) -0.0005(4) -0.0021(4) -0.0052(5) C9 0.0203(6) 0.0158(5) 0.0166(6) -0.0012(4) -0.0020(4) -0.0049(5) C10 0.0232(7) 0.0229(6) 0.0249(7) -0.0027(5) -0.0010(5) -0.0094(5) C11 0.0261(7) 0.0316(8) 0.0278(7) -0.0037(6) 0.0049(6) -0.0113(6) C12 0.0311(8) 0.0301(7) 0.0199(7) -0.0050(6) 0.0058(6) -0.0084(6) C13 0.0292(7) 0.0244(7) 0.0158(6) -0.0046(5) -0.0002(5) -0.0085(6) C14 0.0197(6) 0.0161(6) 0.0201(6) -0.0040(5) -0.0028(5) -0.0032(5) C15 0.0179(6) 0.0160(5) 0.0223(6) -0.0013(5) -0.0072(5) -0.0025(5) C16 0.0150(6) 0.0173(6) 0.0235(6) -0.0037(5) -0.0055(5) -0.0025(5) C17 0.0163(6) 0.0236(7) 0.0394(9) -0.0099(6) -0.0052(6) -0.0001(5) C18 0.0199(7) 0.0200(7) 0.0602(12) -0.0105(7) -0.0132(7) 0.0024(6) C19 0.0268(8) 0.0164(6) 0.0551(11) 0.0034(7) -0.0187(7) -0.0023(6) C20 0.0254(7) 0.0205(6) 0.0321(8) 0.0053(6) -0.0102(6) -0.0047(6) C21 0.0146(5) 0.0190(6) 0.0171(6) -0.0060(5) -0.0010(4) -0.0029(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic= ) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.9122(10) . ? Fe1 O3 1.9409(10) . ? Fe1 O5 1.9612(10) . ? Fe1 O9 2.0380(11) . ? Fe1 O7 2.0511(10) . ? Fe1 O8 2.0748(11) . ? O1 C7 1.2884(16) . ? O2 C7 1.2370(18) . ? O3 C14 1.2825(16) . ? O4 C14 1.2418(16) . ? O5 C21 1.2754(16) . ? O6 C21 1.2514(16) . ? O7 H71 0.85(3) . ? O7 H72 0.81(2) . ? O8 H81 0.81(2) . ? O8 H82 0.84(3) . ? O9 H91 0.83(3) . ? O9 H92 0.82(3) . ? O10 H101 0.81(3) . ? O10 H102 0.80(3) . ? O11 H111 0.81(3) . ? O11 H112 0.89(3) . ? O12 H121 0.77(3) . ? O12 H122 0.83(3) . ? O13 H131 0.83(3) . ? O13 H132 0.84(3) . ? O14 H141 0.87(4) . ? O14 H142 0.72(4) . ? N1 C8 1.4171(17) . ? N1 C1 1.4213(16) . ? N1 C15 1.4229(18) . ? C1 C6 1.3997(19) . ? C1 C2 1.409(2) . ? C2 C3 1.3999(18) . ? C2 C7 1.5042(19) . ? C3 C4 1.388(2) . ? C3 H3 0.94(2) . ? C4 C5 1.385(3) . ? C4 H4 0.95(2) . ? C5 C6 1.392(2) . ? C5 H5 0.92(2) . ? C6 H6 0.94(2) . ? C8 C13 1.397(2) . ? C8 C9 1.4061(18) . ? C9 C10 1.3982(19) . ? C9 C14 1.5001(19) . ? C10 C11 1.389(2) . ? C10 H10 0.926(19) . ? C11 C12 1.390(2) . ? C11 H11 0.94(2) . ? C12 C13 1.390(2) . ? C12 H12 0.96(2) . ? C13 H13 0.91(2) . ? C15 C20 1.3984(19) . ? C15 C16 1.403(2) . ? C16 C17 1.403(2) . ? C16 C21 1.4978(19) . ? C17 C18 1.385(2) . ? C17 H17 0.95(2) . ? C18 C19 1.386(3) . ? C18 H18 0.91(2) . ? C19 C20 1.385(2) . ? C19 H19 0.94(2) . ? C20 H20 0.90(2) . ? 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 100.32(4) . . ? O1 Fe1 O5 99.38(4) . . ? O3 Fe1 O5 95.57(4) . . ? O1 Fe1 O9 166.18(4) . . ? O3 Fe1 O9 85.50(4) . . ? O5 Fe1 O9 92.45(5) . . ? O1 Fe1 O7 85.84(4) . . ? O3 Fe1 O7 90.98(4) . . ? O5 Fe1 O7 170.73(4) . . ? O9 Fe1 O7 81.51(5) . . ? O1 Fe1 O8 90.86(5) . . ? O3 Fe1 O8 168.69(5) . . ? O5 Fe1 O8 84.16(4) . . ? O9 Fe1 O8 83.22(5) . . ? O7 Fe1 O8 88.13(5) . . ? C7 O1 Fe1 139.40(10) . . ? C14 O3 Fe1 139.08(9) . . ? C21 O5 Fe1 142.54(9) . . ? Fe1 O7 H71 129.1(17) . . ? Fe1 O7 H72 116.7(17) . . ? H71 O7 H72 108(2) . . ? Fe1 O8 H81 127.6(16) . . ? Fe1 O8 H82 121.9(17) . . ? H81 O8 H82 105(2) . . ? Fe1 O9 H91 125.7(18) . . ? Fe1 O9 H92 124.7(17) . . ? H91 O9 H92 108(2) . . ? H101 O10 H102 104(2) . . ? H111 O11 H112 113(3) . . ? H121 O12 H122 110(3) . . ? H131 O13 H132 105(2) . . ? H141 O14 H142 110(4) . . ? C8 N1 C1 119.59(11) . . ? C8 N1 C15 118.99(11) . . ? C1 N1 C15 119.38(11) . . ? C6 C1 C2 119.42(12) . . ? C6 C1 N1 118.89(13) . . ? C2 C1 N1 121.69(11) . . ? C3 C2 C1 118.82(13) . . ? C3 C2 C7 116.01(13) . . ? C1 C2 C7 125.12(12) . . ? C4 C3 C2 121.41(15) . . ? C4 C3 H3 118.8(12) . . ? C2 C3 H3 119.6(12) . . ? C5 C4 C3 119.35(14) . . ? C5 C4 H4 120.4(13) . . ? C3 C4 H4 120.2(13) . . ? C4 C5 C6 120.50(14) . . ? C4 C5 H5 121.3(14) . . ? C6 C5 H5 118.2(14) . . ? C5 C6 C1 120.39(15) . . ? C5 C6 H6 119.5(12) . . ? C1 C6 H6 120.0(12) . . ? O2 C7 O1 121.76(13) . . ? O2 C7 C2 119.54(12) . . ? O1 C7 C2 118.69(12) . . ? C13 C8 C9 119.10(12) . . ? C13 C8 N1 119.93(12) . . ? C9 C8 N1 120.95(12) . . ? C10 C9 C8 119.06(13) . . ? C10 C9 C14 117.18(12) . . ? C8 C9 C14 123.74(12) . . ? C11 C10 C9 121.38(14) . . ? C11 C10 H10 119.8(12) . . ? C9 C10 H10 118.8(12) . . ? C10 C11 C12 119.30(14) . . ? C10 C11 H11 121.8(13) . . ? C12 C11 H11 118.9(13) . . ? C11 C12 C13 120.02(14) . . ? C11 C12 H12 119.0(13) . . ? C13 C12 H12 120.9(13) . . ? C12 C13 C8 121.02(14) . . ? C12 C13 H13 120.6(14) . . ? C8 C13 H13 118.4(14) . . ? O4 C14 O3 121.54(13) . . ? O4 C14 C9 119.06(12) . . ? O3 C14 C9 119.40(11) . . ? C20 C15 C16 118.72(14) . . ? C20 C15 N1 120.00(13) . . ? C16 C15 N1 121.27(12) . . ? C15 C16 C17 119.44(13) . . ? C15 C16 C21 122.97(12) . . ? C17 C16 C21 117.57(13) . . ? C18 C17 C16 121.04(16) . . ? C18 C17 H17 120.9(13) . . ? C16 C17 H17 118.1(13) . . ? C17 C18 C19 119.34(15) . . ? C17 C18 H18 122.0(15) . . ? C19 C18 H18 118.7(15) . . ? C20 C19 C18 120.32(15) . . ? C20 C19 H19 119.6(14) . . ? C18 C19 H19 120.1(14) . . ? C19 C20 C15 121.08(16) . . ? C19 C20 H20 121.2(14) . . ? C15 C20 H20 117.7(14) . . ? O6 C21 O5 120.47(12) . . ? O6 C21 C16 119.42(12) . . ? O5 C21 C16 120.09(11) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 32.05 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 0.819 _refine_diff_density_min -0.450 _refine_diff_density_rms 0.067 #=========================================================================== #================================= data_sw31 _database_code_CSD 200180 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H24 Fe2 N2 O12, 2(C6 H16 N), 2(C2H3N)' _chemical_formula_sum 'C58 H62 Fe2 N6 O12' _chemical_formula_weight 1146.84 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' 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 10.5263(6) _cell_length_b 11.9071(7) _cell_length_c 12.9073(7) _cell_angle_alpha 95.2450(10) _cell_angle_beta 110.6550(10) _cell_angle_gamma 113.0040(10) _cell_volume 1343.13(13) _cell_formula_units_Z 1 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 600 _exptl_absorpt_coefficient_mu 0.610 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8615 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20922 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 32.04 _reflns_number_total 8868 _reflns_number_gt 7111 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; disordered acetonitrile solvent molecule 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^)+(0.0512P)^2^+1.5710P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8868 _refine_ls_number_parameters 465 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0639 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1238 _refine_ls_wR_factor_gt 0.1143 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 0.33591(3) 0.32198(2) 0.86593(2) 0.01131(7) Uani 1 1 d . . . O5 O 0.34372(14) 0.45762(12) 0.97553(11) 0.0126(2) Uani 1 1 d . . . O6 O 0.46132(15) 0.66762(12) 1.01914(12) 0.0167(3) Uani 1 1 d . . . O3 O 0.20660(14) 0.13934(12) 0.82402(12) 0.0143(2) Uani 1 1 d . . . O4 O -0.00096(17) -0.03146(13) 0.80211(14) 0.0217(3) Uani 1 1 d . . . O1 O 0.37557(15) 0.38281(13) 0.73528(12) 0.0166(3) Uani 1 1 d . . . O2 O 0.32307(16) 0.42068(13) 0.56366(12) 0.0176(3) Uani 1 1 d . . . N1 N 0.09641(16) 0.32707(13) 0.76225(13) 0.0101(3) Uani 1 1 d . . . N2 N 0.41598(18) 0.34928(15) 0.31768(14) 0.0143(3) Uani 1 1 d . . . C1 C 0.03395(19) 0.24002(16) 0.65027(15) 0.0106(3) Uani 1 1 d . . . C2 C 0.12237(19) 0.25954(16) 0.58692(15) 0.0108(3) Uani 1 1 d . . . C3 C 0.0578(2) 0.17946(17) 0.47685(16) 0.0134(3) Uani 1 1 d . . . C4 C -0.0882(2) 0.07931(17) 0.43075(17) 0.0156(3) Uani 1 1 d . . . C5 C -0.1733(2) 0.06103(18) 0.49442(17) 0.0167(3) Uani 1 1 d . . . C6 C -0.1140(2) 0.14157(17) 0.60287(16) 0.0138(3) Uani 1 1 d . . . C7 C 0.2840(2) 0.36246(16) 0.63204(16) 0.0130(3) Uani 1 1 d . . . C8 C 0.02285(18) 0.28043(16) 0.83656(15) 0.0108(3) Uani 1 1 d . . . C9 C 0.01483(19) 0.16809(16) 0.86735(16) 0.0117(3) Uani 1 1 d . . . C10 C -0.0544(2) 0.12896(18) 0.94119(17) 0.0152(3) Uani 1 1 d . . . C11 C -0.1124(2) 0.19750(19) 0.98577(18) 0.0178(4) Uani 1 1 d . . . C12 C -0.1068(2) 0.30620(18) 0.95274(18) 0.0170(3) Uani 1 1 d . . . C13 C -0.0417(2) 0.34641(17) 0.87756(17) 0.0140(3) Uani 1 1 d . . . C14 C 0.0750(2) 0.08397(16) 0.82693(16) 0.0133(3) Uani 1 1 d . . . C15 C 0.12176(18) 0.45539(16) 0.75609(15) 0.0102(3) Uani 1 1 d . . . C16 C 0.23743(18) 0.56345(16) 0.84574(15) 0.0105(3) Uani 1 1 d . . . C17 C 0.2485(2) 0.68277(17) 0.83393(16) 0.0134(3) Uani 1 1 d . . . C18 C 0.1488(2) 0.69640(18) 0.73753(17) 0.0162(3) Uani 1 1 d . . . C19 C 0.0363(2) 0.58962(18) 0.64886(17) 0.0165(3) Uani 1 1 d . . . C20 C 0.0237(2) 0.47063(17) 0.65844(16) 0.0141(3) Uani 1 1 d . . . C21 C 0.35463(19) 0.56203(16) 0.95401(15) 0.0112(3) Uani 1 1 d . . . C22 C 0.4327(2) 0.2678(2) 0.39967(19) 0.0205(4) Uani 1 1 d . . . C23 C 0.5884(3) 0.2721(3) 0.4459(3) 0.0368(6) Uani 1 1 d . . . C24 C 0.4446(2) 0.31511(19) 0.21556(19) 0.0183(4) Uani 1 1 d . . . C25 C 0.3388(3) 0.1808(2) 0.1426(2) 0.0228(4) Uani 1 1 d . . . C26 C 0.2649(2) 0.35166(19) 0.28568(18) 0.0165(3) Uani 1 1 d . . . C27 C 0.2481(3) 0.4447(2) 0.2162(2) 0.0260(4) Uani 1 1 d . . . N3 N -0.5727(6) -0.0421(5) 0.3458(5) 0.0497(14) Uiso 0.530(5) 1 d P A 1 C28 C -0.5397(6) -0.0635(5) 0.2748(5) 0.0365(12) Uiso 0.530(5) 1 d P A 1 C29 C -0.4895(7) -0.0739(6) 0.1799(6) 0.0408(13) Uiso 0.530(5) 1 d P A 1 H29A H -0.5156 -0.0218 0.1298 0.096(15) Uiso 0.530(5) 1 calc PR A 1 H29B H -0.5412 -0.1624 0.1350 0.096(15) Uiso 0.530(5) 1 calc PR A 1 H29C H -0.3790 -0.0443 0.2133 0.096(15) Uiso 0.530(5) 1 calc PR A 1 N4 N -0.4658(10) -0.0054(8) 0.0597(7) 0.075(2) Uiso 0.470(5) 1 d P . 2 C30 C -0.4802(8) -0.0508(7) 0.1288(7) 0.0431(15) Uiso 0.470(5) 1 d P A 2 C31 C -0.4977(7) -0.1187(6) 0.2145(6) 0.0357(13) Uiso 0.470(5) 1 d P A 2 H31A H -0.5710 -0.2078 0.1763 0.096(15) Uiso 0.470(5) 1 calc PR A 2 H31B H -0.5350 -0.0814 0.2608 0.096(15) Uiso 0.470(5) 1 calc PR A 2 H31C H -0.3991 -0.1127 0.2644 0.096(15) Uiso 0.470(5) 1 calc PR A 2 H2N H 0.488(3) 0.429(3) 0.357(2) 0.023(7) Uiso 1 1 d . . . H3 H 0.116(3) 0.192(2) 0.434(2) 0.017(6) Uiso 1 1 d . . . H4 H -0.124(3) 0.022(2) 0.358(2) 0.016(6) Uiso 1 1 d . . . H5 H -0.274(3) -0.006(3) 0.467(2) 0.026(7) Uiso 1 1 d . . . H6 H -0.174(3) 0.130(3) 0.645(2) 0.025(7) Uiso 1 1 d . . . H10 H -0.064(3) 0.052(3) 0.958(2) 0.023(7) Uiso 1 1 d . . . H11 H -0.155(3) 0.168(3) 1.039(2) 0.022(6) Uiso 1 1 d . . . H12 H -0.146(3) 0.355(3) 0.983(2) 0.022(7) Uiso 1 1 d . . . H13 H -0.041(3) 0.419(2) 0.856(2) 0.019(6) Uiso 1 1 d . . . H17 H 0.329(3) 0.753(2) 0.897(2) 0.011(5) Uiso 1 1 d . . . H18 H 0.155(3) 0.777(2) 0.733(2) 0.020(6) Uiso 1 1 d . . . H19 H -0.036(3) 0.595(3) 0.582(3) 0.028(7) Uiso 1 1 d . . . H20 H -0.054(3) 0.399(2) 0.597(2) 0.012(5) Uiso 1 1 d . . . H22A H 0.415(3) 0.298(2) 0.456(2) 0.019(6) Uiso 1 1 d . . . H22B H 0.352(3) 0.185(3) 0.362(2) 0.022(7) Uiso 1 1 d . . . H23A H 0.598(4) 0.224(3) 0.507(3) 0.048(10) Uiso 1 1 d . . . H23B H 0.603(4) 0.232(3) 0.385(3) 0.042(9) Uiso 1 1 d . . . H23C H 0.667(5) 0.359(5) 0.481(4) 0.082(14) Uiso 1 1 d . . . H24A H 0.553(3) 0.332(3) 0.250(2) 0.026(7) Uiso 1 1 d . . . H24B H 0.433(3) 0.376(2) 0.175(2) 0.019(6) Uiso 1 1 d . . . H25A H 0.358(3) 0.162(3) 0.076(3) 0.030(7) Uiso 1 1 d . . . H25B H 0.239(4) 0.163(3) 0.112(3) 0.032(8) Uiso 1 1 d . . . H25C H 0.352(3) 0.118(3) 0.177(3) 0.035(8) Uiso 1 1 d . . . H26A H 0.261(3) 0.376(2) 0.358(2) 0.012(6) Uiso 1 1 d . . . H26B H 0.188(3) 0.269(3) 0.247(2) 0.023(7) Uiso 1 1 d . . . H27A H 0.158(3) 0.447(3) 0.212(3) 0.031(8) Uiso 1 1 d . . . H27B H 0.334(4) 0.526(3) 0.256(3) 0.039(8) Uiso 1 1 d . . . H27C H 0.243(4) 0.423(3) 0.145(3) 0.045(9) Uiso 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 0.01211(11) 0.01065(11) 0.00935(12) 0.00208(9) 0.00279(9) 0.00514(9) O5 0.0145(5) 0.0136(5) 0.0111(6) 0.0042(5) 0.0055(5) 0.0075(5) O6 0.0144(6) 0.0133(6) 0.0167(7) 0.0002(5) 0.0010(5) 0.0065(5) O3 0.0135(6) 0.0122(5) 0.0172(7) 0.0023(5) 0.0066(5) 0.0059(5) O4 0.0247(7) 0.0113(6) 0.0307(8) 0.0049(6) 0.0162(7) 0.0058(5) O1 0.0120(6) 0.0210(6) 0.0134(6) 0.0063(5) 0.0043(5) 0.0048(5) O2 0.0181(6) 0.0187(6) 0.0127(6) 0.0050(5) 0.0079(5) 0.0037(5) N1 0.0119(6) 0.0091(6) 0.0088(6) 0.0023(5) 0.0047(5) 0.0040(5) N2 0.0134(7) 0.0145(7) 0.0143(7) 0.0037(6) 0.0062(6) 0.0054(6) C1 0.0119(7) 0.0117(7) 0.0080(7) 0.0024(6) 0.0031(6) 0.0061(6) C2 0.0116(7) 0.0111(7) 0.0100(7) 0.0033(6) 0.0044(6) 0.0055(6) C3 0.0175(8) 0.0144(7) 0.0100(8) 0.0034(6) 0.0058(6) 0.0088(6) C4 0.0195(8) 0.0139(7) 0.0110(8) 0.0020(6) 0.0045(7) 0.0075(7) C5 0.0130(7) 0.0161(8) 0.0125(8) 0.0018(7) 0.0011(7) 0.0028(6) C6 0.0119(7) 0.0155(7) 0.0117(8) 0.0038(6) 0.0039(6) 0.0048(6) C7 0.0140(7) 0.0125(7) 0.0128(8) 0.0023(6) 0.0063(6) 0.0059(6) C8 0.0103(7) 0.0129(7) 0.0091(7) 0.0032(6) 0.0042(6) 0.0050(6) C9 0.0114(7) 0.0120(7) 0.0117(8) 0.0032(6) 0.0050(6) 0.0051(6) C10 0.0149(7) 0.0156(8) 0.0151(9) 0.0065(7) 0.0070(7) 0.0060(6) C11 0.0176(8) 0.0205(9) 0.0176(9) 0.0077(7) 0.0115(7) 0.0068(7) C12 0.0172(8) 0.0188(8) 0.0181(9) 0.0029(7) 0.0108(7) 0.0086(7) C13 0.0136(7) 0.0145(7) 0.0156(9) 0.0045(7) 0.0075(7) 0.0069(6) C14 0.0164(8) 0.0128(7) 0.0128(8) 0.0049(6) 0.0070(7) 0.0076(6) C15 0.0108(7) 0.0116(7) 0.0097(7) 0.0035(6) 0.0048(6) 0.0060(6) C16 0.0107(7) 0.0125(7) 0.0101(8) 0.0038(6) 0.0051(6) 0.0061(6) C17 0.0145(7) 0.0129(7) 0.0145(8) 0.0036(6) 0.0071(7) 0.0072(6) C18 0.0210(8) 0.0160(8) 0.0165(9) 0.0078(7) 0.0089(7) 0.0115(7) C19 0.0212(8) 0.0188(8) 0.0129(8) 0.0072(7) 0.0059(7) 0.0127(7) C20 0.0145(7) 0.0163(8) 0.0114(8) 0.0041(7) 0.0037(6) 0.0083(6) C21 0.0117(7) 0.0141(7) 0.0098(7) 0.0026(6) 0.0052(6) 0.0072(6) C22 0.0244(9) 0.0235(9) 0.0195(10) 0.0106(8) 0.0111(8) 0.0137(8) C23 0.0288(12) 0.0454(15) 0.0448(17) 0.0236(14) 0.0127(12) 0.0250(12) C24 0.0200(9) 0.0181(8) 0.0201(10) 0.0049(7) 0.0131(8) 0.0078(7) C25 0.0249(10) 0.0209(9) 0.0212(10) 0.0015(8) 0.0111(9) 0.0086(8) C26 0.0138(8) 0.0209(9) 0.0172(9) 0.0059(7) 0.0080(7) 0.0086(7) C27 0.0242(10) 0.0344(12) 0.0294(12) 0.0191(10) 0.0143(9) 0.0180(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 O3 1.9562(13) . ? Fe1 O5 2.0032(13) . ? Fe1 O1 2.0066(14) . ? Fe1 O6 2.0732(14) 2_667 ? Fe1 N1 2.4299(15) . ? O5 C21 1.269(2) . ? O6 C21 1.259(2) . ? O6 Fe1 2.0732(13) 2_667 ? O3 C14 1.297(2) . ? O4 C14 1.229(2) . ? O1 C7 1.271(2) . ? O2 C7 1.255(2) . ? N1 C8 1.454(2) . ? N1 C1 1.456(2) . ? N1 C15 1.460(2) . ? N2 C24 1.507(3) . ? N2 C26 1.508(2) . ? N2 C22 1.511(3) . ? N2 H2N 0.90(3) . ? C1 C6 1.394(2) . ? C1 C2 1.411(2) . ? C2 C3 1.398(3) . ? C2 C7 1.509(2) . ? C3 C4 1.390(3) . ? C3 H3 0.94(3) . ? C4 C5 1.387(3) . ? C4 H4 0.96(3) . ? C5 C6 1.392(3) . ? C5 H5 0.95(3) . ? C6 H6 0.95(3) . ? C8 C13 1.397(2) . ? C8 C9 1.410(2) . ? C9 C10 1.401(2) . ? C9 C14 1.520(2) . ? C10 C11 1.386(3) . ? C10 H10 0.93(3) . ? C11 C12 1.385(3) . ? C11 H11 0.97(3) . ? C12 C13 1.392(3) . ? C12 H12 0.96(3) . ? C13 H13 0.93(3) . ? C15 C20 1.399(2) . ? C15 C16 1.409(2) . ? C16 C17 1.406(2) . ? C16 C21 1.510(2) . ? C17 C18 1.387(3) . ? C17 H17 0.96(2) . ? C18 C19 1.389(3) . ? C18 H18 0.95(3) . ? C19 C20 1.392(2) . ? C19 H19 0.96(3) . ? C20 H20 0.95(2) . ? C22 C23 1.511(3) . ? C22 H22A 0.89(3) . ? C22 H22B 0.95(3) . ? C23 H23A 1.01(4) . ? C23 H23B 0.98(4) . ? C23 H23C 0.97(5) . ? C24 C25 1.509(3) . ? C24 H24A 1.00(3) . ? C24 H24B 0.96(3) . ? C25 H25A 0.97(3) . ? C25 H25B 0.91(3) . ? C25 H25C 0.94(3) . ? C26 C27 1.512(3) . ? C26 H26A 0.97(3) . ? C26 H26B 0.94(3) . ? C27 H27A 0.94(3) . ? C27 H27B 0.96(3) . ? C27 H27C 0.91(4) . ? N3 C28 1.129(8) . ? C28 C29 1.509(8) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? N4 C30 1.109(10) . ? N4 N4 1.496(17) 2_455 ? C30 C31 1.450(9) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 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 O3 Fe1 O5 127.85(5) . . ? O3 Fe1 O1 112.79(6) . . ? O5 Fe1 O1 111.49(6) . . ? O3 Fe1 O6 99.60(5) . 2_667 ? O5 Fe1 O6 93.04(5) . 2_667 ? O1 Fe1 O6 106.38(6) . 2_667 ? O3 Fe1 N1 83.64(5) . . ? O5 Fe1 N1 77.26(5) . . ? O1 Fe1 N1 81.18(5) . . ? O6 Fe1 N1 169.53(5) 2_667 . ? C21 O5 Fe1 121.89(12) . . ? C21 O6 Fe1 119.76(11) . 2_667 ? C14 O3 Fe1 126.22(11) . . ? C7 O1 Fe1 130.46(12) . . ? C8 N1 C1 115.56(13) . . ? C8 N1 C15 113.95(13) . . ? C1 N1 C15 113.04(14) . . ? C8 N1 Fe1 98.47(10) . . ? C1 N1 Fe1 103.22(10) . . ? C15 N1 Fe1 110.95(10) . . ? C24 N2 C26 113.60(15) . . ? C24 N2 C22 113.64(15) . . ? C26 N2 C22 109.74(14) . . ? C24 N2 H2N 106.5(18) . . ? C26 N2 H2N 106.1(17) . . ? C22 N2 H2N 106.6(18) . . ? C6 C1 C2 119.76(16) . . ? C6 C1 N1 120.92(15) . . ? C2 C1 N1 119.26(15) . . ? C3 C2 C1 118.65(16) . . ? C3 C2 C7 118.00(15) . . ? C1 C2 C7 123.35(16) . . ? C4 C3 C2 121.59(17) . . ? C4 C3 H3 119.2(16) . . ? C2 C3 H3 119.2(16) . . ? C5 C4 C3 118.99(18) . . ? C5 C4 H4 122.2(15) . . ? C3 C4 H4 118.7(15) . . ? C4 C5 C6 120.78(17) . . ? C4 C5 H5 122.7(17) . . ? C6 C5 H5 116.6(17) . . ? C5 C6 C1 120.18(17) . . ? C5 C6 H6 120.6(17) . . ? C1 C6 H6 119.2(17) . . ? O2 C7 O1 123.04(16) . . ? O2 C7 C2 117.87(16) . . ? O1 C7 C2 119.02(15) . . ? C13 C8 C9 119.35(15) . . ? C13 C8 N1 120.12(15) . . ? C9 C8 N1 120.53(14) . . ? C10 C9 C8 118.13(16) . . ? C10 C9 C14 116.33(15) . . ? C8 C9 C14 125.54(15) . . ? C11 C10 C9 122.43(17) . . ? C11 C10 H10 119.9(17) . . ? C9 C10 H10 117.7(17) . . ? C12 C11 C10 118.78(17) . . ? C12 C11 H11 122.4(16) . . ? C10 C11 H11 118.8(16) . . ? C11 C12 C13 120.30(17) . . ? C11 C12 H12 119.8(16) . . ? C13 C12 H12 119.8(16) . . ? C12 C13 C8 120.93(17) . . ? C12 C13 H13 118.0(16) . . ? C8 C13 H13 121.1(16) . . ? O4 C14 O3 123.98(17) . . ? O4 C14 C9 118.60(16) . . ? O3 C14 C9 117.39(15) . . ? C20 C15 C16 119.04(16) . . ? C20 C15 N1 118.25(15) . . ? C16 C15 N1 122.67(15) . . ? C17 C16 C15 118.46(16) . . ? C17 C16 C21 116.58(15) . . ? C15 C16 C21 124.94(15) . . ? C18 C17 C16 121.92(17) . . ? C18 C17 H17 122.9(14) . . ? C16 C17 H17 115.1(14) . . ? C17 C18 C19 119.31(17) . . ? C17 C18 H18 120.8(17) . . ? C19 C18 H18 119.9(17) . . ? C18 C19 C20 119.75(17) . . ? C18 C19 H19 121.7(17) . . ? C20 C19 H19 118.5(17) . . ? C19 C20 C15 121.50(17) . . ? C19 C20 H20 118.5(15) . . ? C15 C20 H20 119.9(15) . . ? O6 C21 O5 122.94(16) . . ? O6 C21 C16 116.94(15) . . ? O5 C21 C16 120.11(15) . . ? N2 C22 C23 112.89(18) . . ? N2 C22 H22A 105.2(17) . . ? C23 C22 H22A 110.9(17) . . ? N2 C22 H22B 107.9(17) . . ? C23 C22 H22B 113.3(16) . . ? H22A C22 H22B 106(2) . . ? C22 C23 H23A 110(2) . . ? C22 C23 H23B 111(2) . . ? H23A C23 H23B 107(3) . . ? C22 C23 H23C 110(3) . . ? H23A C23 H23C 108(3) . . ? H23B C23 H23C 111(3) . . ? N2 C24 C25 113.91(16) . . ? N2 C24 H24A 104.3(17) . . ? C25 C24 H24A 112.2(16) . . ? N2 C24 H24B 102.9(16) . . ? C25 C24 H24B 112.6(16) . . ? H24A C24 H24B 110(2) . . ? C24 C25 H25A 112.1(17) . . ? C24 C25 H25B 113.5(19) . . ? H25A C25 H25B 104(3) . . ? C24 C25 H25C 115(2) . . ? H25A C25 H25C 100(3) . . ? H25B C25 H25C 111(3) . . ? N2 C26 C27 112.93(16) . . ? N2 C26 H26A 105.9(14) . . ? C27 C26 H26A 109.3(14) . . ? N2 C26 H26B 107.6(17) . . ? C27 C26 H26B 112.5(17) . . ? H26A C26 H26B 108(2) . . ? C26 C27 H27A 104.9(18) . . ? C26 C27 H27B 109(2) . . ? H27A C27 H27B 110(3) . . ? C26 C27 H27C 114(2) . . ? H27A C27 H27C 111(3) . . ? H27B C27 H27C 107(3) . . ? N3 C28 C29 172.4(6) . . ? C30 N4 N4 149.0(11) . 2_455 ? N4 C30 C31 175.2(8) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.078 _refine_diff_density_min -0.587 _refine_diff_density_rms 0.092 #========END