# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _audit_creation_date 10-05-05 _publ_contact_author_name 'J. Nierengarten' _publ_contact_author_address ; Groupe de Chimie des Fullerenes et des Systemes Conjugues Laboratoire de Chimie de Coordination du CNRS 205 205 route de Narbonne Toulouse Cedex 4 31077 FRANCE ; _publ_contact_author_email JFNIERENGARTEN@LCC-TOULOUSE.FR _publ_section_title ; Changes in electronic couplings of mixed-valence systems due to through-space intramolecular interactions ; _publ_section_references ; Blessing, R.H. (1987). Crystallogr. Rev. 1, 3-58. Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. A.L. Spek, PLATON 98, Utrecht University, The Netherland, 1998. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. Sheldrick, G.M. (1997). SHELXL97. Program for the refinement of crystal structures. University of Gottingen. Germany. ; loop_ _publ_author_name 'J. Nierengarten' 'Beatrice Delavaux-Nicot' 'Teresa M. Figueira-Duarte' 'Aline Gegout' ; V.Lloveras ; 'Concepcio Rovira' 'Jaume Veciana' 'Jose Vidal-Gancedo' 'Richard Welter' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 624690' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H28 Fe2 O4' _chemical_formula_sum 'C32 H28 Fe2 O4' _chemical_formula_weight 588.24 _chemical_absolute_configuration . 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6870(3) _cell_length_b 11.4770(4) _cell_length_c 12.5620(5) _cell_angle_alpha 108.25(5) _cell_angle_beta 93.06(5) _cell_angle_gamma 93.80(5) _cell_volume 1319.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4852 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 1.136 _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 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 KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean . _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 11644 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.1021 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 30.12 _reflns_number_total 7706 _reflns_number_gt 4332 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _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. A structural disorder has been considered for the ester group C30-O3-C31-O5-C33. This explains the alert B in the checkcif process. ; _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^)+(0.0792P)^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 7706 _refine_ls_number_parameters 332 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1234 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1594 _refine_ls_wR_factor_gt 0.1263 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _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 0.48450(4) 0.74546(4) -0.03538(4) 0.02719(14) Uani 1 1 d . . . Fe2 Fe 1.01482(4) 0.09885(4) 0.30201(4) 0.03116(15) Uani 1 1 d . . . O1 O 0.9125(3) 0.6353(2) 0.2229(2) 0.0439(6) Uani 1 1 d . . . O2 O 0.9251(3) 0.4593(2) 0.2614(3) 0.0708(9) Uani 1 1 d . . . C1 C 0.4698(4) 0.6894(3) 0.1034(3) 0.0431(9) Uani 1 1 d . . . H1 H 0.5418 0.6579 0.1379 0.052 Uiso 1 1 calc . . . C2 C 0.3699(4) 0.6193(3) 0.0167(3) 0.0414(9) Uani 1 1 d . . . H2 H 0.3626 0.5324 -0.0171 0.050 Uiso 1 1 calc . . . C3 C 0.2822(3) 0.7023(3) -0.0107(3) 0.0415(9) Uani 1 1 d . . . H3 H 0.2062 0.6805 -0.0662 0.050 Uiso 1 1 calc . . . C4 C 0.3282(3) 0.8227(3) 0.0592(3) 0.0380(8) Uani 1 1 d . . . H4 H 0.2885 0.8961 0.0589 0.046 Uiso 1 1 calc . . . C5 C 0.4432(4) 0.8152(3) 0.1294(3) 0.0408(8) Uani 1 1 d . . . H5 H 0.4942 0.8826 0.1848 0.049 Uiso 1 1 calc . . . C6 C 0.6808(3) 0.7217(3) -0.0865(3) 0.0299(7) Uani 1 1 d . . . C7 C 0.6542(3) 0.8490(3) -0.0559(3) 0.0328(8) Uani 1 1 d . . . H7 H 0.7051 0.9150 0.0011 0.039 Uiso 1 1 calc . . . C8 C 0.5392(3) 0.8587(3) -0.1255(3) 0.0351(8) Uani 1 1 d . . . H8 H 0.4990 0.9328 -0.1227 0.042 Uiso 1 1 calc . . . C9 C 0.4936(3) 0.7402(3) -0.2000(3) 0.0377(8) Uani 1 1 d . . . H9 H 0.4188 0.7212 -0.2564 0.045 Uiso 1 1 calc . . . C10 C 0.5790(3) 0.6549(3) -0.1756(3) 0.0332(7) Uani 1 1 d . . . H10 H 0.5704 0.5683 -0.2120 0.040 Uiso 1 1 calc . . . C11 C 0.7894(3) 0.6689(3) -0.0414(3) 0.0311(7) Uani 1 1 d . . . C12 C 0.8776(3) 0.6164(3) -0.0100(3) 0.0314(7) Uani 1 1 d . . . C13 C 0.9776(3) 0.5536(2) 0.0322(3) 0.0278(7) Uani 1 1 d . . . C14 C 1.0298(3) 0.6106(3) 0.1537(3) 0.0399(9) Uani 1 1 d . . . H14A H 1.0882 0.5540 0.1772 0.048 Uiso 1 1 calc . . . H14B H 1.0874 0.6884 0.1637 0.048 Uiso 1 1 calc . . . C15 C 0.8669(4) 0.5493(3) 0.2665(3) 0.0414(9) Uani 1 1 d . . . C16 C 0.7352(4) 0.5793(4) 0.3204(4) 0.0545(10) Uani 1 1 d . . . H16A H 0.6625 0.5129 0.2843 0.082 Uiso 1 1 calc . . . H16B H 0.7074 0.6567 0.3121 0.082 Uiso 1 1 calc . . . H16C H 0.7489 0.5880 0.4005 0.082 Uiso 1 1 calc . . . C17 C 0.8509(3) 0.1342(3) 0.2135(3) 0.0385(8) Uani 1 1 d . . . H17 H 0.8144 0.2119 0.2264 0.046 Uiso 1 1 calc . . . C18 C 0.9561(4) 0.0893(4) 0.1416(3) 0.0473(10) Uani 1 1 d . . . H18 H 1.0021 0.1312 0.0974 0.057 Uiso 1 1 calc . . . C19 C 0.9809(4) -0.0291(4) 0.1468(3) 0.0499(10) Uani 1 1 d . . . H19 H 1.0470 -0.0801 0.1071 0.060 Uiso 1 1 calc . . . C20 C 0.8905(3) -0.0586(3) 0.2214(3) 0.0391(8) Uani 1 1 d . . . H20 H 0.8851 -0.1327 0.2402 0.047 Uiso 1 1 calc . . . C21 C 0.8086(3) 0.0431(3) 0.2636(3) 0.0299(7) Uani 1 1 d . . . C22 C 1.0862(5) 0.2622(4) 0.4166(4) 0.0628(12) Uani 1 1 d . . . H22 H 1.0471 0.3382 0.4260 0.075 Uiso 1 1 calc . . . C23 C 1.0499(4) 0.1779(5) 0.4723(3) 0.0605(12) Uani 1 1 d . . . H23 H 0.9831 0.1868 0.5264 0.073 Uiso 1 1 calc . . . C24 C 1.1308(4) 0.0771(5) 0.4336(4) 0.0697(14) Uani 1 1 d . . . H24 H 1.1275 0.0058 0.4567 0.084 Uiso 1 1 calc . . . C25 C 1.2186(4) 0.1013(5) 0.3533(4) 0.0648(13) Uani 1 1 d . . . H25 H 1.2838 0.0492 0.3136 0.078 Uiso 1 1 calc . . . C26 C 1.1902(4) 0.2163(4) 0.3442(4) 0.0586(12) Uani 1 1 d . . . H26 H 1.2335 0.2563 0.2974 0.070 Uiso 1 1 calc . . . C27 C 0.7072(3) 0.0491(3) 0.3425(3) 0.0278(7) Uani 1 1 d . . . C28 C 0.6221(3) 0.0489(3) 0.4087(3) 0.0301(7) Uani 1 1 d . . . C29 C 0.5271(3) 0.0520(3) 0.4921(3) 0.0287(7) Uani 1 1 d . . . C30 C 0.4894(3) 0.1756(3) 0.5643(3) 0.0401(9) Uani 1 1 d . . . H30A H 0.4156 0.2041 0.5232 0.048 Uiso 1 1 calc . A 1 H30B H 0.4523 0.1674 0.6338 0.048 Uiso 1 1 calc . B 1 O3 O 0.6089(10) 0.2667(8) 0.5941(9) 0.0532(5) Uiso 0.30 1 d P C 1 C31 C 0.6332(15) 0.3526(12) 0.5462(13) 0.0532(5) Uiso 0.30 1 d P C 1 O5 O 0.5467(9) 0.3713(8) 0.4818(8) 0.0532(5) Uiso 0.30 1 d P C 1 C33 C 0.7863(15) 0.4155(13) 0.5863(14) 0.0532(5) Uiso 0.30 1 d P C 1 H33A H 0.8431 0.3977 0.5218 0.080 Uiso 0.30 1 calc P D 1 H33B H 0.8268 0.3828 0.6430 0.080 Uiso 0.30 1 calc P E 1 H33C H 0.7834 0.5048 0.6188 0.080 Uiso 0.30 1 calc P F 1 O4 O 0.5527(4) 0.2760(3) 0.5409(4) 0.0532(5) Uiso 0.70 1 d P C 2 C32 C 0.6849(6) 0.3091(6) 0.5828(6) 0.0532(5) Uiso 0.70 1 d P C 2 O6 O 0.7463(4) 0.2574(3) 0.6365(3) 0.0532(5) Uiso 0.70 1 d P C 2 C34 C 0.7434(6) 0.4189(6) 0.5497(6) 0.0532(5) Uiso 0.70 1 d P C 2 H34A H 0.7690 0.4892 0.6177 0.080 Uiso 0.70 1 calc P G 2 H34B H 0.6729 0.4410 0.5022 0.080 Uiso 0.70 1 calc P H 2 H34C H 0.8256 0.3969 0.5081 0.080 Uiso 0.70 1 calc P I 2 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 0.0211(2) 0.0275(2) 0.0351(3) 0.0123(2) 0.00373(18) 0.00387(16) Fe2 0.0231(2) 0.0426(3) 0.0310(3) 0.0165(2) 0.00356(19) 0.00048(18) O1 0.0565(15) 0.0404(13) 0.0401(16) 0.0158(11) 0.0124(12) 0.0206(11) O2 0.072(2) 0.0495(16) 0.104(3) 0.0391(17) 0.0181(18) 0.0177(14) C1 0.048(2) 0.050(2) 0.042(2) 0.0257(18) 0.0089(17) 0.0145(17) C2 0.046(2) 0.0320(17) 0.052(2) 0.0191(17) 0.0180(18) 0.0027(15) C3 0.0237(16) 0.049(2) 0.056(3) 0.0215(18) 0.0114(15) -0.0009(14) C4 0.0312(17) 0.0365(17) 0.050(2) 0.0148(16) 0.0168(16) 0.0115(14) C5 0.046(2) 0.0403(18) 0.037(2) 0.0124(16) 0.0097(17) 0.0039(15) C6 0.0203(14) 0.0331(16) 0.042(2) 0.0182(14) 0.0077(13) 0.0070(12) C7 0.0200(14) 0.0339(16) 0.047(2) 0.0165(15) 0.0026(14) 0.0018(12) C8 0.0269(16) 0.0387(17) 0.050(2) 0.0264(16) 0.0081(15) 0.0083(13) C9 0.0269(16) 0.059(2) 0.035(2) 0.0244(17) 0.0031(14) 0.0100(15) C10 0.0269(16) 0.0379(17) 0.035(2) 0.0105(15) 0.0074(14) 0.0069(13) C11 0.0236(15) 0.0296(15) 0.041(2) 0.0111(14) 0.0054(14) 0.0029(12) C12 0.0244(15) 0.0299(15) 0.040(2) 0.0113(14) 0.0039(14) 0.0024(12) C13 0.0197(13) 0.0287(14) 0.037(2) 0.0139(13) 0.0006(13) 0.0011(11) C14 0.0354(18) 0.0408(18) 0.040(2) 0.0076(16) 0.0003(16) 0.0071(15) C15 0.045(2) 0.0369(19) 0.038(2) 0.0074(16) -0.0051(16) 0.0013(16) C16 0.048(2) 0.069(3) 0.039(2) 0.0078(19) 0.0009(18) 0.0017(19) C17 0.0303(16) 0.054(2) 0.040(2) 0.0273(17) 0.0038(15) 0.0060(15) C18 0.0330(18) 0.083(3) 0.031(2) 0.026(2) 0.0049(15) -0.0009(18) C19 0.0365(19) 0.063(2) 0.041(2) 0.0003(19) 0.0138(17) 0.0109(17) C20 0.0320(17) 0.0360(17) 0.044(2) 0.0037(16) 0.0085(15) 0.0043(14) C21 0.0243(14) 0.0389(17) 0.0250(18) 0.0083(14) 0.0029(13) -0.0001(12) C22 0.065(3) 0.060(2) 0.051(3) 0.008(2) 0.000(2) -0.026(2) C23 0.050(2) 0.094(3) 0.031(2) 0.019(2) -0.0047(18) -0.030(2) C24 0.042(2) 0.109(4) 0.074(4) 0.060(3) -0.021(2) -0.015(2) C25 0.0279(19) 0.108(4) 0.062(3) 0.037(3) -0.0101(19) -0.003(2) C26 0.039(2) 0.084(3) 0.051(3) 0.026(2) 0.0025(19) -0.025(2) C27 0.0230(14) 0.0313(15) 0.0287(18) 0.0099(13) -0.0008(13) 0.0005(12) C28 0.0281(15) 0.0293(15) 0.0317(19) 0.0083(14) 0.0008(14) 0.0009(12) C29 0.0208(14) 0.0338(16) 0.0302(19) 0.0086(14) 0.0028(13) 0.0017(12) C30 0.0387(18) 0.0343(17) 0.048(2) 0.0131(16) 0.0155(17) 0.0009(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C8 2.036(3) . ? Fe1 C7 2.040(3) . ? Fe1 C10 2.043(3) . ? Fe1 C5 2.045(4) . ? Fe1 C6 2.047(3) . ? Fe1 C1 2.047(4) . ? Fe1 C4 2.049(3) . ? Fe1 C3 2.053(3) . ? Fe1 C2 2.053(3) . ? Fe1 C9 2.056(4) . ? Fe2 C22 2.024(4) . ? Fe2 C17 2.026(4) . ? Fe2 C18 2.032(4) . ? Fe2 C26 2.034(4) . ? Fe2 C19 2.034(4) . ? Fe2 C24 2.038(4) . ? Fe2 C25 2.039(4) . ? Fe2 C21 2.041(3) . ? Fe2 C20 2.043(3) . ? Fe2 C23 2.045(4) . ? O1 C15 1.333(4) . ? O1 C14 1.456(4) . ? O2 C15 1.195(4) . ? C1 C2 1.416(5) . ? C1 C5 1.422(5) . ? C1 H1 0.9500 . ? C2 C3 1.424(5) . ? C2 H2 0.9500 . ? C3 C4 1.413(5) . ? C3 H3 0.9500 . ? C4 C5 1.407(5) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C11 1.425(4) . ? C6 C10 1.434(5) . ? C6 C7 1.434(4) . ? C7 C8 1.411(5) . ? C7 H7 0.9500 . ? C8 C9 1.414(5) . ? C8 H8 0.9500 . ? C9 C10 1.417(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.196(4) . ? C12 C13 1.421(4) . ? C13 C13 1.356(6) 2_765 ? C13 C14 1.504(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.486(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.413(5) . ? C17 C21 1.428(5) . ? C17 H17 0.9500 . ? C18 C19 1.417(6) . ? C18 H18 0.9500 . ? C19 C20 1.417(5) . ? C19 H19 0.9500 . ? C20 C21 1.432(4) . ? C20 H20 0.9500 . ? C21 C27 1.422(4) . ? C22 C23 1.397(6) . ? C22 C26 1.409(6) . ? C22 H22 0.9500 . ? C23 C24 1.413(6) . ? C23 H23 0.9500 . ? C24 C25 1.433(6) . ? C24 H24 0.9500 . ? C25 C26 1.404(6) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.202(4) . ? C28 C29 1.425(4) . ? C29 C29 1.347(6) 2_656 ? C29 C30 1.506(4) . ? C30 O4 1.388(5) . ? C30 O3 1.457(10) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? O3 C31 1.321(18) . ? C31 O5 1.210(17) . ? C31 C33 1.59(2) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? O4 C32 1.341(7) . ? C32 O6 1.190(7) . ? C32 C34 1.530(9) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 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 C8 Fe1 C7 40.51(13) . . ? C8 Fe1 C10 68.29(13) . . ? C7 Fe1 C10 68.83(13) . . ? C8 Fe1 C5 121.11(14) . . ? C7 Fe1 C5 106.59(15) . . ? C10 Fe1 C5 160.81(14) . . ? C8 Fe1 C6 68.56(13) . . ? C7 Fe1 C6 41.09(12) . . ? C10 Fe1 C6 41.05(13) . . ? C5 Fe1 C6 123.38(15) . . ? C8 Fe1 C1 157.32(15) . . ? C7 Fe1 C1 122.16(15) . . ? C10 Fe1 C1 124.82(14) . . ? C5 Fe1 C1 40.67(14) . . ? C6 Fe1 C1 108.03(14) . . ? C8 Fe1 C4 106.57(14) . . ? C7 Fe1 C4 122.00(13) . . ? C10 Fe1 C4 158.08(15) . . ? C5 Fe1 C4 40.21(15) . . ? C6 Fe1 C4 158.92(13) . . ? C1 Fe1 C4 68.10(15) . . ? C8 Fe1 C3 123.01(15) . . ? C7 Fe1 C3 158.37(14) . . ? C10 Fe1 C3 123.30(15) . . ? C5 Fe1 C3 67.77(16) . . ? C6 Fe1 C3 159.42(13) . . ? C1 Fe1 C3 68.10(16) . . ? C4 Fe1 C3 40.30(14) . . ? C8 Fe1 C2 160.07(16) . . ? C7 Fe1 C2 158.75(15) . . ? C10 Fe1 C2 109.14(14) . . ? C5 Fe1 C2 67.99(15) . . ? C6 Fe1 C2 123.40(13) . . ? C1 Fe1 C2 40.41(15) . . ? C4 Fe1 C2 68.01(13) . . ? C3 Fe1 C2 40.58(14) . . ? C8 Fe1 C9 40.42(14) . . ? C7 Fe1 C9 68.25(15) . . ? C10 Fe1 C9 40.43(13) . . ? C5 Fe1 C9 156.89(14) . . ? C6 Fe1 C9 68.47(14) . . ? C1 Fe1 C9 161.11(14) . . ? C4 Fe1 C9 121.97(15) . . ? C3 Fe1 C9 108.26(15) . . ? C2 Fe1 C9 124.83(16) . . ? C22 Fe2 C17 105.96(18) . . ? C22 Fe2 C18 120.28(19) . . ? C17 Fe2 C18 40.77(14) . . ? C22 Fe2 C26 40.64(17) . . ? C17 Fe2 C26 120.58(18) . . ? C18 Fe2 C26 104.73(17) . . ? C22 Fe2 C19 156.43(18) . . ? C17 Fe2 C19 68.66(16) . . ? C18 Fe2 C19 40.77(16) . . ? C26 Fe2 C19 120.87(17) . . ? C22 Fe2 C24 67.8(2) . . ? C17 Fe2 C24 159.63(18) . . ? C18 Fe2 C24 159.31(19) . . ? C26 Fe2 C24 68.22(18) . . ? C19 Fe2 C24 124.8(2) . . ? C22 Fe2 C25 68.2(2) . . ? C17 Fe2 C25 156.59(17) . . ? C18 Fe2 C25 121.04(17) . . ? C26 Fe2 C25 40.33(18) . . ? C19 Fe2 C25 107.13(18) . . ? C24 Fe2 C25 41.16(18) . . ? C22 Fe2 C21 123.10(16) . . ? C17 Fe2 C21 41.12(13) . . ? C18 Fe2 C21 68.94(14) . . ? C26 Fe2 C21 158.05(17) . . ? C19 Fe2 C21 68.83(14) . . ? C24 Fe2 C21 124.72(16) . . ? C25 Fe2 C21 160.84(18) . . ? C22 Fe2 C20 160.82(16) . . ? C17 Fe2 C20 68.91(15) . . ? C18 Fe2 C20 68.67(16) . . ? C26 Fe2 C20 158.03(16) . . ? C19 Fe2 C20 40.66(15) . . ? C24 Fe2 C20 110.20(18) . . ? C25 Fe2 C20 123.83(18) . . ? C21 Fe2 C20 41.05(13) . . ? C22 Fe2 C23 40.17(18) . . ? C17 Fe2 C23 122.39(19) . . ? C18 Fe2 C23 156.8(2) . . ? C26 Fe2 C23 68.18(17) . . ? C19 Fe2 C23 161.8(2) . . ? C24 Fe2 C23 40.50(19) . . ? C25 Fe2 C23 68.68(19) . . ? C21 Fe2 C23 108.96(15) . . ? C20 Fe2 C23 125.86(17) . . ? C15 O1 C14 117.9(3) . . ? C2 C1 C5 107.7(3) . . ? C2 C1 Fe1 70.0(2) . . ? C5 C1 Fe1 69.6(2) . . ? C2 C1 H1 126.2 . . ? C5 C1 H1 126.2 . . ? Fe1 C1 H1 125.8 . . ? C1 C2 C3 107.9(3) . . ? C1 C2 Fe1 69.58(19) . . ? C3 C2 Fe1 69.70(18) . . ? C1 C2 H2 126.1 . . ? C3 C2 H2 126.1 . . ? Fe1 C2 H2 126.2 . . ? C4 C3 C2 107.9(3) . . ? C4 C3 Fe1 69.72(18) . . ? C2 C3 Fe1 69.72(18) . . ? C4 C3 H3 126.0 . . ? C2 C3 H3 126.0 . . ? Fe1 C3 H3 126.1 . . ? C5 C4 C3 108.2(3) . . ? C5 C4 Fe1 69.71(19) . . ? C3 C4 Fe1 69.98(18) . . ? C5 C4 H4 125.9 . . ? C3 C4 H4 125.9 . . ? Fe1 C4 H4 126.0 . . ? C4 C5 C1 108.3(3) . . ? C4 C5 Fe1 70.1(2) . . ? C1 C5 Fe1 69.8(2) . . ? C4 C5 H5 125.8 . . ? C1 C5 H5 125.8 . . ? Fe1 C5 H5 125.9 . . ? C11 C6 C10 125.2(3) . . ? C11 C6 C7 127.7(3) . . ? C10 C6 C7 107.1(3) . . ? C11 C6 Fe1 128.1(2) . . ? C10 C6 Fe1 69.32(17) . . ? C7 C6 Fe1 69.18(17) . . ? C8 C7 C6 107.9(3) . . ? C8 C7 Fe1 69.61(17) . . ? C6 C7 Fe1 69.74(16) . . ? C8 C7 H7 126.1 . . ? C6 C7 H7 126.1 . . ? Fe1 C7 H7 126.2 . . ? C7 C8 C9 108.9(3) . . ? C7 C8 Fe1 69.88(19) . . ? C9 C8 Fe1 70.55(19) . . ? C7 C8 H8 125.6 . . ? C9 C8 H8 125.6 . . ? Fe1 C8 H8 125.6 . . ? C8 C9 C10 108.0(3) . . ? C8 C9 Fe1 69.0(2) . . ? C10 C9 Fe1 69.3(2) . . ? C8 C9 H9 126.0 . . ? C10 C9 H9 126.0 . . ? Fe1 C9 H9 127.2 . . ? C9 C10 C6 108.2(3) . . ? C9 C10 Fe1 70.29(19) . . ? C6 C10 Fe1 69.64(18) . . ? C9 C10 H10 125.9 . . ? C6 C10 H10 125.9 . . ? Fe1 C10 H10 125.7 . . ? C12 C11 C6 175.0(3) . . ? C11 C12 C13 176.7(4) . . ? C13 C13 C12 122.3(4) 2_765 . ? C13 C13 C14 121.3(4) 2_765 . ? C12 C13 C14 116.4(3) . . ? O1 C14 C13 109.6(3) . . ? O1 C14 H14A 109.8 . . ? C13 C14 H14A 109.8 . . ? O1 C14 H14B 109.8 . . ? C13 C14 H14B 109.8 . . ? H14A C14 H14B 108.2 . . ? O2 C15 O1 123.5(3) . . ? O2 C15 C16 124.9(4) . . ? O1 C15 C16 111.5(3) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C21 108.4(3) . . ? C18 C17 Fe2 69.9(2) . . ? C21 C17 Fe2 70.03(19) . . ? C18 C17 H17 125.8 . . ? C21 C17 H17 125.8 . . ? Fe2 C17 H17 125.9 . . ? C17 C18 C19 108.0(3) . . ? C17 C18 Fe2 69.4(2) . . ? C19 C18 Fe2 69.7(2) . . ? C17 C18 H18 126.0 . . ? C19 C18 H18 126.0 . . ? Fe2 C18 H18 126.5 . . ? C18 C19 C20 108.4(3) . . ? C18 C19 Fe2 69.5(2) . . ? C20 C19 Fe2 70.0(2) . . ? C18 C19 H19 125.8 . . ? C20 C19 H19 125.8 . . ? Fe2 C19 H19 126.3 . . ? C19 C20 C21 107.9(3) . . ? C19 C20 Fe2 69.3(2) . . ? C21 C20 Fe2 69.39(17) . . ? C19 C20 H20 126.0 . . ? C21 C20 H20 126.0 . . ? Fe2 C20 H20 126.8 . . ? C27 C21 C17 128.1(3) . . ? C27 C21 C20 124.7(3) . . ? C17 C21 C20 107.2(3) . . ? C27 C21 Fe2 125.7(2) . . ? C17 C21 Fe2 68.85(18) . . ? C20 C21 Fe2 69.55(17) . . ? C23 C22 C26 109.1(4) . . ? C23 C22 Fe2 70.7(2) . . ? C26 C22 Fe2 70.1(2) . . ? C23 C22 H22 125.5 . . ? C26 C22 H22 125.5 . . ? Fe2 C22 H22 125.3 . . ? C22 C23 C24 107.5(4) . . ? C22 C23 Fe2 69.1(2) . . ? C24 C23 Fe2 69.5(3) . . ? C22 C23 H23 126.3 . . ? C24 C23 H23 126.3 . . ? Fe2 C23 H23 126.7 . . ? C23 C24 C25 108.1(4) . . ? C23 C24 Fe2 70.0(2) . . ? C25 C24 Fe2 69.5(2) . . ? C23 C24 H24 126.0 . . ? C25 C24 H24 126.0 . . ? Fe2 C24 H24 126.1 . . ? C26 C25 C24 107.2(4) . . ? C26 C25 Fe2 69.6(2) . . ? C24 C25 Fe2 69.4(2) . . ? C26 C25 H25 126.4 . . ? C24 C25 H25 126.4 . . ? Fe2 C25 H25 126.1 . . ? C25 C26 C22 108.1(4) . . ? C25 C26 Fe2 70.0(2) . . ? C22 C26 Fe2 69.3(2) . . ? C25 C26 H26 125.9 . . ? C22 C26 H26 125.9 . . ? Fe2 C26 H26 126.3 . . ? C28 C27 C21 177.1(3) . . ? C27 C28 C29 176.7(3) . . ? C29 C29 C28 121.6(3) 2_656 . ? C29 C29 C30 120.2(4) 2_656 . ? C28 C29 C30 118.2(3) . . ? O4 C30 O3 35.8(4) . . ? O4 C30 C29 115.0(3) . . ? O3 C30 C29 111.5(4) . . ? O4 C30 H30A 75.1 . . ? O3 C30 H30A 109.3 . . ? C29 C30 H30A 109.3 . . ? O4 C30 H30B 131.6 . . ? O3 C30 H30B 109.3 . . ? C29 C30 H30B 109.3 . . ? H30A C30 H30B 108.0 . . ? C31 O3 C30 124.9(11) . . ? O5 C31 O3 121.1(13) . . ? O5 C31 C33 130.2(14) . . ? O3 C31 C33 108.7(14) . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 O4 C30 115.6(5) . . ? O6 C32 O4 123.5(6) . . ? O6 C32 C34 126.0(6) . . ? O4 C32 C34 110.5(6) . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 30.12 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.778 _refine_diff_density_min -0.632 _refine_diff_density_rms 0.105