# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Florence Mongin' _publ_contact_author_email FLORENCE.MONGIN@UNIV-RENNES1.FR _publ_section_title ; Deprotonative metallation of ferrocenes using mixed lithium-zinc and lithium-cadmium combinations ; _publ_requested_category FM loop_ _publ_author_name 'Florence Mongin' 'Floris Chevallier' 'Gandrath Dayaker' 'Palakodety Radha Krishna' 'Thierry Roisnel' ; A.Sreeshailam ; # Attachment 'CIF_Mongin.cif' # # CCDC ELECTRONIC DATA DEPOSITION FORM (CIF) # # This electronic data deposition form can be used: # # (a) WHEN SUBMITTING A PAPER TO A JOURNAL FOR PUBLICATION or # (b) WHEN SUBMITTING A PRIVATE COMMUNICATION TO THE CCDC # # A comprehensive archive of CIF resources is maintained by the IUCr # at its Chester office. This can be accessed # by anonymous ftp to ftp.iucr.org # or via the WWW at http://www.iucr.org/cif/home.html # If data items in this form are not available or not applicable # then ignore these items # A few items specific to CCDC input are indicated by _ccdc_ # # Submission and help information is provided at the end of this form #------------------------------------------------------------------------- #1 Global data block identification for start of deposition data_10b _database_code_depnum_ccdc_archive 'CCDC 755178' #TrackingRef 'CIF_Mongin.cif' _audit_creation_date 2009-01-06T17:38:48-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C12 H10 Fe1 I2 O2)' _chemical_formula_sum 'C24 H20 Fe2 I4 O4' _chemical_formula_weight 991.7 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 14.781(2) _cell_length_b 8.0884(14) _cell_length_c 22.871(4) _cell_angle_alpha 90 _cell_angle_beta 101.820(5) _cell_angle_gamma 90 _cell_volume 2676.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5195 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 27.42 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 2.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1840 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.727 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.175 _exptl_absorpt_correction_T_max 0.751 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0522 _diffrn_reflns_av_unetI/netI 0.0622 _diffrn_reflns_number 16591 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 6132 _reflns_number_gt 5085 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SAINT' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0466P)^2^+6.3255P] 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_number_reflns 6132 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.059 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1165 _refine_ls_wR_factor_gt 0.1091 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.544 _refine_diff_density_min -1.639 _refine_diff_density_rms 0.248 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe -0.15135(6) 0.42507(11) 0.86435(4) 0.0144(2) Uani 1 d . . . C1 C -0.0865(4) 0.6340(8) 0.8443(3) 0.0173(14) Uani 1 d . . . I1 I 0.03966(3) 0.74386(5) 0.88061(2) 0.01862(12) Uani 1 d . . . C2 C -0.0955(5) 0.5215(8) 0.7961(3) 0.0199(15) Uani 1 d . . . H2 H -0.0459 0.4776 0.7803 0.024 Uiso 1 calc R . . C3 C -0.1912(4) 0.4841(8) 0.7749(3) 0.0177(14) Uani 1 d . . . H3 H -0.216 0.4118 0.7429 0.021 Uiso 1 calc R . . C4 C -0.2422(4) 0.5746(8) 0.8103(3) 0.0186(14) Uani 1 d . . . I4 I -0.38584(3) 0.56053(6) 0.79502(2) 0.02328(13) Uani 1 d . . . C5 C -0.1784(4) 0.6690(8) 0.8542(3) 0.0167(13) Uani 1 d . . . C6 C -0.2039(4) 0.7694(8) 0.9030(3) 0.0162(13) Uani 1 d . . . O7 O -0.2819(3) 0.8181(6) 0.9026(3) 0.0268(12) Uani 1 d . . . O8 O -0.1316(3) 0.7996(6) 0.9466(2) 0.0204(10) Uani 1 d . . . C9 C -0.1501(5) 0.8989(9) 0.9953(3) 0.0244(16) Uani 1 d . . . H9A H -0.1775 1.0045 0.9797 0.037 Uiso 1 calc R . . H9B H -0.0922 0.9196 1.0239 0.037 Uiso 1 calc R . . H9C H -0.1932 0.8401 1.0152 0.037 Uiso 1 calc R . . C10 C -0.1873(6) 0.1831(9) 0.8716(4) 0.0304(18) Uani 1 d . . . H10 H -0.2183 0.116 0.8397 0.036 Uiso 1 calc R . . C11 C -0.0912(6) 0.2017(9) 0.8906(4) 0.0328(19) Uani 1 d . . . H11 H -0.0455 0.1469 0.874 0.039 Uiso 1 calc R . . C12 C -0.0735(5) 0.3157(10) 0.9388(4) 0.0330(19) Uani 1 d . . . H12 H -0.0147 0.3527 0.9597 0.04 Uiso 1 calc R . . C13 C -0.1605(5) 0.3633(9) 0.9495(3) 0.0275(17) Uani 1 d . . . H13 H -0.1702 0.4382 0.9797 0.033 Uiso 1 calc R . . C14 C -0.2291(5) 0.2842(10) 0.9095(4) 0.0317(19) Uani 1 d . . . H14 H -0.2936 0.2954 0.9075 0.038 Uiso 1 calc R . . Fe2 Fe 0.35174(6) 0.33278(11) 0.85559(4) 0.0150(2) Uani 1 d . . . C21 C 0.4097(4) 0.1236(8) 0.8289(3) 0.0151(13) Uani 1 d . . . I21 I 0.53618(3) 0.00623(5) 0.85837(2) 0.01822(12) Uani 1 d . . . C22 C 0.3955(4) 0.2419(8) 0.7819(3) 0.0188(14) Uani 1 d . . . H22 H 0.442 0.2868 0.7634 0.023 Uiso 1 calc R . . C23 C 0.2995(4) 0.2817(8) 0.7672(3) 0.0173(13) Uani 1 d . . . H23 H 0.2711 0.3569 0.7371 0.021 Uiso 1 calc R . . C24 C 0.2540(4) 0.1897(8) 0.8053(3) 0.0151(13) Uani 1 d . . . I24 I 0.11224(3) 0.20550(6) 0.80044(2) 0.02668(14) Uani 1 d . . . C25 C 0.3211(4) 0.0895(7) 0.8453(3) 0.0120(12) Uani 1 d . . . C26 C 0.3021(4) -0.0137(8) 0.8941(3) 0.0150(13) Uani 1 d . . . O27 O 0.2261(3) -0.0584(6) 0.8991(2) 0.0235(11) Uani 1 d . . . O28 O 0.3795(3) -0.0495(6) 0.9340(2) 0.0204(10) Uani 1 d . . . C29 C 0.3675(5) -0.1460(9) 0.9852(3) 0.0262(16) Uani 1 d . . . H29A H 0.3343 -0.0801 1.01 0.039 Uiso 1 calc R . . H29B H 0.4282 -0.1773 1.0088 0.039 Uiso 1 calc R . . H29C H 0.3319 -0.246 0.9716 0.039 Uiso 1 calc R . . C30 C 0.3771(6) 0.3881(9) 0.9452(3) 0.0275(17) Uani 1 d . . . H30 H 0.3886 0.3116 0.9774 0.033 Uiso 1 calc R . . C31 C 0.4454(5) 0.4614(9) 0.9180(4) 0.0267(17) Uani 1 d . . . H31 H 0.51 0.4411 0.9279 0.032 Uiso 1 calc R . . C32 C 0.3993(5) 0.5703(9) 0.8732(4) 0.0256(17) Uani 1 d . . . H32 H 0.4276 0.6387 0.8483 0.031 Uiso 1 calc R . . C33 C 0.3026(5) 0.5590(9) 0.8721(4) 0.0273(17) Uani 1 d . . . H33 H 0.2551 0.617 0.8457 0.033 Uiso 1 calc R . . C34 C 0.2897(5) 0.4471(9) 0.9168(4) 0.0245(16) Uani 1 d . . . H34 H 0.2322 0.4169 0.9261 0.029 Uiso 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 0.0131(4) 0.0099(4) 0.0219(5) 0.0014(4) 0.0072(4) 0.0009(3) C1 0.015(3) 0.016(3) 0.022(4) 0.002(3) 0.008(3) -0.003(2) I1 0.0123(2) 0.0185(2) 0.0268(3) -0.00238(19) 0.00785(17) -0.00237(15) C2 0.023(3) 0.009(3) 0.029(4) 0.002(3) 0.009(3) 0.002(3) C3 0.025(3) 0.014(3) 0.015(3) 0.000(3) 0.005(3) 0.002(3) C4 0.013(3) 0.017(3) 0.027(4) 0.004(3) 0.007(3) 0.004(2) I4 0.0116(2) 0.0194(2) 0.0381(3) 0.0000(2) 0.00323(18) -0.00048(16) C5 0.016(3) 0.013(3) 0.022(4) 0.002(3) 0.008(3) 0.001(2) C6 0.018(3) 0.012(3) 0.019(3) 0.003(3) 0.006(3) 0.001(2) O7 0.015(2) 0.023(3) 0.044(3) -0.006(2) 0.009(2) 0.005(2) O8 0.019(2) 0.022(3) 0.020(3) -0.004(2) 0.0041(19) 0.0048(19) C9 0.034(4) 0.016(4) 0.026(4) -0.003(3) 0.013(3) 0.007(3) C10 0.049(5) 0.012(3) 0.029(4) 0.005(3) 0.003(4) -0.006(3) C11 0.045(5) 0.021(4) 0.038(5) 0.011(4) 0.020(4) 0.021(3) C12 0.023(4) 0.034(5) 0.037(5) 0.015(4) -0.006(3) 0.001(3) C13 0.042(4) 0.025(4) 0.019(4) 0.003(3) 0.015(3) 0.008(3) C14 0.023(4) 0.036(5) 0.037(5) 0.025(4) 0.009(3) -0.002(3) Fe2 0.0144(4) 0.0101(4) 0.0219(5) -0.0017(4) 0.0067(4) 0.0000(3) C21 0.012(3) 0.009(3) 0.026(4) -0.004(3) 0.008(3) 0.001(2) I21 0.0116(2) 0.0188(2) 0.0258(3) -0.00345(19) 0.00749(16) 0.00179(16) C22 0.017(3) 0.019(3) 0.024(4) 0.000(3) 0.012(3) -0.005(3) C23 0.021(3) 0.010(3) 0.020(4) 0.000(3) 0.003(3) 0.001(2) C24 0.010(3) 0.011(3) 0.024(4) -0.002(3) 0.003(2) -0.002(2) I24 0.0124(2) 0.0222(3) 0.0441(3) -0.0037(2) 0.00239(19) 0.00379(16) C25 0.010(3) 0.008(3) 0.019(3) -0.005(2) 0.003(2) 0.002(2) C26 0.019(3) 0.008(3) 0.019(3) -0.002(3) 0.008(3) 0.002(2) O27 0.014(2) 0.024(3) 0.035(3) -0.001(2) 0.011(2) -0.0045(19) O28 0.020(2) 0.020(3) 0.022(3) 0.004(2) 0.0057(19) 0.0022(19) C29 0.036(4) 0.020(4) 0.024(4) 0.008(3) 0.010(3) 0.006(3) C30 0.050(5) 0.012(3) 0.020(4) -0.004(3) 0.005(3) 0.000(3) C31 0.027(4) 0.019(4) 0.030(4) -0.013(3) -0.002(3) 0.003(3) C32 0.032(4) 0.015(4) 0.034(5) -0.010(3) 0.017(3) -0.007(3) C33 0.037(4) 0.013(3) 0.032(4) -0.005(3) 0.008(3) 0.006(3) C34 0.029(4) 0.018(4) 0.033(4) -0.004(3) 0.022(3) -0.001(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C5 2.017(7) . ? Fe1 C4 2.028(7) . ? Fe1 C1 2.042(6) . ? Fe1 C14 2.042(7) . ? Fe1 C13 2.043(7) . ? Fe1 C10 2.043(7) . ? Fe1 C11 2.049(7) . ? Fe1 C12 2.050(8) . ? Fe1 C2 2.063(7) . ? Fe1 C3 2.065(7) . ? C1 C2 1.414(10) . ? C1 C5 1.451(8) . ? C1 I1 2.079(6) . ? C2 C3 1.430(9) . ? C2 H2 0.95 . ? C3 C4 1.418(9) . ? C3 H3 0.95 . ? C4 C5 1.446(10) . ? C4 I4 2.084(6) . ? C5 C6 1.489(9) . ? C6 O7 1.217(8) . ? C6 O8 1.327(8) . ? O8 C9 1.444(8) . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 C11 1.406(11) . ? C10 C14 1.421(12) . ? C10 H10 0.95 . ? C11 C12 1.419(12) . ? C11 H11 0.95 . ? C12 C13 1.411(11) . ? C12 H12 0.95 . ? C13 C14 1.377(11) . ? C13 H13 0.95 . ? C14 H14 0.95 . ? Fe2 C24 2.017(6) . ? Fe2 C25 2.022(6) . ? Fe2 C33 2.032(7) . ? Fe2 C34 2.045(7) . ? Fe2 C21 2.046(6) . ? Fe2 C23 2.052(7) . ? Fe2 C31 2.055(7) . ? Fe2 C30 2.056(8) . ? Fe2 C32 2.057(7) . ? Fe2 C22 2.061(7) . ? C21 C22 1.422(10) . ? C21 C25 1.461(8) . ? C21 I21 2.082(6) . ? C22 C23 1.426(9) . ? C22 H22 0.95 . ? C23 C24 1.417(9) . ? C23 H23 0.95 . ? C24 C25 1.451(9) . ? C24 I24 2.079(6) . ? C25 C26 1.466(9) . ? C26 O27 1.208(7) . ? C26 O28 1.340(8) . ? O28 C29 1.450(8) . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C30 C34 1.405(11) . ? C30 C31 1.420(11) . ? C30 H30 0.95 . ? C31 C32 1.415(11) . ? C31 H31 0.95 . ? C32 C33 1.427(10) . ? C32 H32 0.95 . ? C33 C34 1.407(11) . ? C33 H33 0.95 . ? C34 H34 0.95 . ? 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 C5 Fe1 C4 41.9(3) . . ? C5 Fe1 C1 41.9(2) . . ? C4 Fe1 C1 69.6(3) . . ? C5 Fe1 C14 119.0(3) . . ? C4 Fe1 C14 105.7(3) . . ? C1 Fe1 C14 156.1(3) . . ? C5 Fe1 C13 107.4(3) . . ? C4 Fe1 C13 124.2(3) . . ? C1 Fe1 C13 122.9(3) . . ? C14 Fe1 C13 39.4(3) . . ? C5 Fe1 C10 153.8(3) . . ? C4 Fe1 C10 118.1(3) . . ? C1 Fe1 C10 162.4(3) . . ? C14 Fe1 C10 40.7(3) . . ? C13 Fe1 C10 67.6(3) . . ? C5 Fe1 C11 163.8(3) . . ? C4 Fe1 C11 153.9(3) . . ? C1 Fe1 C11 126.9(3) . . ? C14 Fe1 C11 67.4(3) . . ? C13 Fe1 C11 67.3(3) . . ? C10 Fe1 C11 40.2(3) . . ? C5 Fe1 C12 125.6(3) . . ? C4 Fe1 C12 162.2(3) . . ? C1 Fe1 C12 109.5(3) . . ? C14 Fe1 C12 67.5(3) . . ? C13 Fe1 C12 40.3(3) . . ? C10 Fe1 C12 68.3(3) . . ? C11 Fe1 C12 40.5(3) . . ? C5 Fe1 C2 69.1(3) . . ? C4 Fe1 C2 68.3(3) . . ? C1 Fe1 C2 40.3(3) . . ? C14 Fe1 C2 161.3(3) . . ? C13 Fe1 C2 158.3(3) . . ? C10 Fe1 C2 125.1(3) . . ? C11 Fe1 C2 109.8(3) . . ? C12 Fe1 C2 123.2(3) . . ? C5 Fe1 C3 69.5(3) . . ? C4 Fe1 C3 40.5(3) . . ? C1 Fe1 C3 68.7(3) . . ? C14 Fe1 C3 123.6(3) . . ? C13 Fe1 C3 160.1(3) . . ? C10 Fe1 C3 106.0(3) . . ? C11 Fe1 C3 120.9(3) . . ? C12 Fe1 C3 156.9(3) . . ? C2 Fe1 C3 40.5(3) . . ? C2 C1 C5 107.8(6) . . ? C2 C1 Fe1 70.7(4) . . ? C5 C1 Fe1 68.2(4) . . ? C2 C1 I1 121.4(5) . . ? C5 C1 I1 130.2(5) . . ? Fe1 C1 I1 133.5(4) . . ? C1 C2 C3 109.2(6) . . ? C1 C2 Fe1 69.0(4) . . ? C3 C2 Fe1 69.8(4) . . ? C1 C2 H2 125.4 . . ? C3 C2 H2 125.4 . . ? Fe1 C2 H2 127.3 . . ? C4 C3 C2 107.6(6) . . ? C4 C3 Fe1 68.3(4) . . ? C2 C3 Fe1 69.6(4) . . ? C4 C3 H3 126.2 . . ? C2 C3 H3 126.2 . . ? Fe1 C3 H3 127.4 . . ? C3 C4 C5 108.8(5) . . ? C3 C4 Fe1 71.2(4) . . ? C5 C4 Fe1 68.7(4) . . ? C3 C4 I4 121.3(5) . . ? C5 C4 I4 129.9(5) . . ? Fe1 C4 I4 126.5(3) . . ? C4 C5 C1 106.6(6) . . ? C4 C5 C6 125.4(6) . . ? C1 C5 C6 127.8(6) . . ? C4 C5 Fe1 69.5(4) . . ? C1 C5 Fe1 69.9(4) . . ? C6 C5 Fe1 121.4(5) . . ? O7 C6 O8 124.1(6) . . ? O7 C6 C5 123.9(6) . . ? O8 C6 C5 112.0(5) . . ? C6 O8 C9 115.6(5) . . ? O8 C9 H9A 109.5 . . ? O8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C14 106.7(7) . . ? C11 C10 Fe1 70.1(4) . . ? C14 C10 Fe1 69.6(4) . . ? C11 C10 H10 126.6 . . ? C14 C10 H10 126.6 . . ? Fe1 C10 H10 125.3 . . ? C10 C11 C12 108.9(7) . . ? C10 C11 Fe1 69.7(4) . . ? C12 C11 Fe1 69.8(4) . . ? C10 C11 H11 125.6 . . ? C12 C11 H11 125.6 . . ? Fe1 C11 H11 126.5 . . ? C13 C12 C11 106.4(7) . . ? C13 C12 Fe1 69.5(4) . . ? C11 C12 Fe1 69.7(5) . . ? C13 C12 H12 126.8 . . ? C11 C12 H12 126.8 . . ? Fe1 C12 H12 125.6 . . ? C14 C13 C12 109.3(7) . . ? C14 C13 Fe1 70.3(4) . . ? C12 C13 Fe1 70.1(5) . . ? C14 C13 H13 125.4 . . ? C12 C13 H13 125.4 . . ? Fe1 C13 H13 125.8 . . ? C13 C14 C10 108.7(7) . . ? C13 C14 Fe1 70.3(4) . . ? C10 C14 Fe1 69.7(4) . . ? C13 C14 H14 125.7 . . ? C10 C14 H14 125.7 . . ? Fe1 C14 H14 125.9 . . ? C24 Fe2 C25 42.1(2) . . ? C24 Fe2 C33 112.4(3) . . ? C25 Fe2 C33 144.9(3) . . ? C24 Fe2 C34 106.3(3) . . ? C25 Fe2 C34 113.5(3) . . ? C33 Fe2 C34 40.4(3) . . ? C24 Fe2 C21 69.5(2) . . ? C25 Fe2 C21 42.1(2) . . ? C33 Fe2 C21 171.0(3) . . ? C34 Fe2 C21 148.5(3) . . ? C24 Fe2 C23 40.7(3) . . ? C25 Fe2 C23 70.1(3) . . ? C33 Fe2 C23 106.7(3) . . ? C34 Fe2 C23 129.4(3) . . ? C21 Fe2 C23 68.6(3) . . ? C24 Fe2 C31 171.1(3) . . ? C25 Fe2 C31 132.6(3) . . ? C33 Fe2 C31 68.3(3) . . ? C34 Fe2 C31 68.2(3) . . ? C21 Fe2 C31 111.2(3) . . ? C23 Fe2 C31 148.1(3) . . ? C24 Fe2 C30 131.0(3) . . ? C25 Fe2 C30 108.6(3) . . ? C33 Fe2 C30 67.5(3) . . ? C34 Fe2 C30 40.1(3) . . ? C21 Fe2 C30 118.4(3) . . ? C23 Fe2 C30 168.7(3) . . ? C31 Fe2 C30 40.4(3) . . ? C24 Fe2 C32 145.5(3) . . ? C25 Fe2 C32 172.3(3) . . ? C33 Fe2 C32 40.8(3) . . ? C34 Fe2 C32 68.1(3) . . ? C21 Fe2 C32 133.1(3) . . ? C23 Fe2 C32 115.2(3) . . ? C31 Fe2 C32 40.3(3) . . ? C30 Fe2 C32 67.4(3) . . ? C24 Fe2 C22 68.7(3) . . ? C25 Fe2 C22 70.0(3) . . ? C33 Fe2 C22 131.1(3) . . ? C34 Fe2 C22 168.9(3) . . ? C21 Fe2 C22 40.5(3) . . ? C23 Fe2 C22 40.6(3) . . ? C31 Fe2 C22 117.9(3) . . ? C30 Fe2 C22 150.4(3) . . ? C32 Fe2 C22 110.0(3) . . ? C22 C21 C25 108.7(5) . . ? C22 C21 Fe2 70.3(4) . . ? C25 C21 Fe2 68.1(3) . . ? C22 C21 I21 122.4(4) . . ? C25 C21 I21 128.5(5) . . ? Fe2 C21 I21 133.1(3) . . ? C21 C22 C23 108.4(6) . . ? C21 C22 Fe2 69.2(4) . . ? C23 C22 Fe2 69.4(4) . . ? C21 C22 H22 125.8 . . ? C23 C22 H22 125.8 . . ? Fe2 C22 H22 127.2 . . ? C24 C23 C22 108.2(6) . . ? C24 C23 Fe2 68.3(4) . . ? C22 C23 Fe2 70.1(4) . . ? C24 C23 H23 125.9 . . ? C22 C23 H23 125.9 . . ? Fe2 C23 H23 127.3 . . ? C23 C24 C25 109.3(5) . . ? C23 C24 Fe2 71.0(4) . . ? C25 C24 Fe2 69.1(3) . . ? C23 C24 I24 122.4(5) . . ? C25 C24 I24 128.3(5) . . ? Fe2 C24 I24 126.3(3) . . ? C24 C25 C21 105.4(6) . . ? C24 C25 C26 125.8(5) . . ? C21 C25 C26 128.7(6) . . ? C24 C25 Fe2 68.8(3) . . ? C21 C25 Fe2 69.8(3) . . ? C26 C25 Fe2 122.6(5) . . ? O27 C26 O28 123.5(6) . . ? O27 C26 C25 124.7(6) . . ? O28 C26 C25 111.8(5) . . ? C26 O28 C29 116.0(5) . . ? O28 C29 H29A 109.5 . . ? O28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C34 C30 C31 108.9(7) . . ? C34 C30 Fe2 69.6(4) . . ? C31 C30 Fe2 69.8(4) . . ? C34 C30 H30 125.5 . . ? C31 C30 H30 125.5 . . ? Fe2 C30 H30 126.7 . . ? C32 C31 C30 107.3(6) . . ? C32 C31 Fe2 69.9(4) . . ? C30 C31 Fe2 69.8(4) . . ? C32 C31 H31 126.4 . . ? C30 C31 H31 126.4 . . ? Fe2 C31 H31 125.5 . . ? C31 C32 C33 107.8(7) . . ? C31 C32 Fe2 69.8(4) . . ? C33 C32 Fe2 68.7(4) . . ? C31 C32 H32 126.1 . . ? C33 C32 H32 126.1 . . ? Fe2 C32 H32 127 . . ? C34 C33 C32 108.2(7) . . ? C34 C33 Fe2 70.3(4) . . ? C32 C33 Fe2 70.5(4) . . ? C34 C33 H33 125.9 . . ? C32 C33 H33 125.9 . . ? Fe2 C33 H33 124.9 . . ? C30 C34 C33 107.8(6) . . ? C30 C34 Fe2 70.4(4) . . ? C33 C34 Fe2 69.3(4) . . ? C30 C34 H34 126.1 . . ? C33 C34 H34 126.1 . . ? Fe2 C34 H34 125.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 Fe1 C1 C2 -119.3(6) . . . . ? C4 Fe1 C1 C2 -80.2(4) . . . . ? C14 Fe1 C1 C2 -162.9(7) . . . . ? C13 Fe1 C1 C2 161.5(4) . . . . ? C10 Fe1 C1 C2 39.0(11) . . . . ? C11 Fe1 C1 C2 76.7(5) . . . . ? C12 Fe1 C1 C2 118.7(4) . . . . ? C3 Fe1 C1 C2 -36.7(4) . . . . ? C4 Fe1 C1 C5 39.2(4) . . . . ? C14 Fe1 C1 C5 -43.5(9) . . . . ? C13 Fe1 C1 C5 -79.2(5) . . . . ? C10 Fe1 C1 C5 158.4(9) . . . . ? C11 Fe1 C1 C5 -164.0(4) . . . . ? C12 Fe1 C1 C5 -121.9(5) . . . . ? C2 Fe1 C1 C5 119.3(6) . . . . ? C3 Fe1 C1 C5 82.6(4) . . . . ? C5 Fe1 C1 I1 125.4(7) . . . . ? C4 Fe1 C1 I1 164.6(5) . . . . ? C14 Fe1 C1 I1 81.8(8) . . . . ? C13 Fe1 C1 I1 46.2(6) . . . . ? C10 Fe1 C1 I1 -76.3(11) . . . . ? C11 Fe1 C1 I1 -38.6(6) . . . . ? C12 Fe1 C1 I1 3.4(6) . . . . ? C2 Fe1 C1 I1 -115.3(6) . . . . ? C3 Fe1 C1 I1 -152.0(5) . . . . ? C5 C1 C2 C3 0.2(8) . . . . ? Fe1 C1 C2 C3 58.4(5) . . . . ? I1 C1 C2 C3 -171.8(5) . . . . ? C5 C1 C2 Fe1 -58.2(5) . . . . ? I1 C1 C2 Fe1 129.8(5) . . . . ? C5 Fe1 C2 C1 38.5(4) . . . . ? C4 Fe1 C2 C1 83.6(4) . . . . ? C14 Fe1 C2 C1 158.1(8) . . . . ? C13 Fe1 C2 C1 -46.1(9) . . . . ? C10 Fe1 C2 C1 -166.5(4) . . . . ? C11 Fe1 C2 C1 -124.2(4) . . . . ? C12 Fe1 C2 C1 -81.1(5) . . . . ? C3 Fe1 C2 C1 121.1(6) . . . . ? C5 Fe1 C2 C3 -82.5(4) . . . . ? C4 Fe1 C2 C3 -37.4(4) . . . . ? C1 Fe1 C2 C3 -121.1(6) . . . . ? C14 Fe1 C2 C3 37.1(10) . . . . ? C13 Fe1 C2 C3 -167.1(7) . . . . ? C10 Fe1 C2 C3 72.4(5) . . . . ? C11 Fe1 C2 C3 114.7(4) . . . . ? C12 Fe1 C2 C3 157.8(4) . . . . ? C1 C2 C3 C4 0.0(8) . . . . ? Fe1 C2 C3 C4 57.9(5) . . . . ? C1 C2 C3 Fe1 -57.9(5) . . . . ? C5 Fe1 C3 C4 -38.1(4) . . . . ? C1 Fe1 C3 C4 -83.1(4) . . . . ? C14 Fe1 C3 C4 73.8(5) . . . . ? C13 Fe1 C3 C4 46.4(10) . . . . ? C10 Fe1 C3 C4 114.7(4) . . . . ? C11 Fe1 C3 C4 155.7(4) . . . . ? C12 Fe1 C3 C4 -173.3(7) . . . . ? C2 Fe1 C3 C4 -119.6(5) . . . . ? C5 Fe1 C3 C2 81.5(4) . . . . ? C4 Fe1 C3 C2 119.6(6) . . . . ? C1 Fe1 C3 C2 36.5(4) . . . . ? C14 Fe1 C3 C2 -166.6(4) . . . . ? C13 Fe1 C3 C2 166.0(8) . . . . ? C10 Fe1 C3 C2 -125.7(4) . . . . ? C11 Fe1 C3 C2 -84.7(5) . . . . ? C12 Fe1 C3 C2 -53.6(9) . . . . ? C2 C3 C4 C5 -0.2(8) . . . . ? Fe1 C3 C4 C5 58.5(5) . . . . ? C2 C3 C4 Fe1 -58.7(5) . . . . ? C2 C3 C4 I4 179.4(5) . . . . ? Fe1 C3 C4 I4 -121.8(5) . . . . ? C5 Fe1 C4 C3 119.9(5) . . . . ? C1 Fe1 C4 C3 80.7(4) . . . . ? C14 Fe1 C4 C3 -123.9(4) . . . . ? C13 Fe1 C4 C3 -162.6(4) . . . . ? C10 Fe1 C4 C3 -81.8(5) . . . . ? C11 Fe1 C4 C3 -53.5(8) . . . . ? C12 Fe1 C4 C3 171.3(9) . . . . ? C2 Fe1 C4 C3 37.4(4) . . . . ? C1 Fe1 C4 C5 -39.2(4) . . . . ? C14 Fe1 C4 C5 116.2(4) . . . . ? C13 Fe1 C4 C5 77.4(5) . . . . ? C10 Fe1 C4 C5 158.3(4) . . . . ? C11 Fe1 C4 C5 -173.4(6) . . . . ? C12 Fe1 C4 C5 51.4(11) . . . . ? C2 Fe1 C4 C5 -82.5(4) . . . . ? C3 Fe1 C4 C5 -119.9(5) . . . . ? C5 Fe1 C4 I4 -124.6(6) . . . . ? C1 Fe1 C4 I4 -163.8(5) . . . . ? C14 Fe1 C4 I4 -8.4(5) . . . . ? C13 Fe1 C4 I4 -47.2(6) . . . . ? C10 Fe1 C4 I4 33.6(6) . . . . ? C11 Fe1 C4 I4 61.9(9) . . . . ? C12 Fe1 C4 I4 -73.2(11) . . . . ? C2 Fe1 C4 I4 152.9(5) . . . . ? C3 Fe1 C4 I4 115.4(6) . . . . ? C3 C4 C5 C1 0.3(8) . . . . ? Fe1 C4 C5 C1 60.4(5) . . . . ? I4 C4 C5 C1 -179.3(5) . . . . ? C3 C4 C5 C6 -174.7(6) . . . . ? Fe1 C4 C5 C6 -114.6(7) . . . . ? I4 C4 C5 C6 5.7(10) . . . . ? C3 C4 C5 Fe1 -60.1(5) . . . . ? I4 C4 C5 Fe1 120.3(6) . . . . ? C2 C1 C5 C4 -0.3(8) . . . . ? Fe1 C1 C5 C4 -60.1(5) . . . . ? I1 C1 C5 C4 170.7(5) . . . . ? C2 C1 C5 C6 174.6(6) . . . . ? Fe1 C1 C5 C6 114.8(7) . . . . ? I1 C1 C5 C6 -14.4(11) . . . . ? C2 C1 C5 Fe1 59.8(5) . . . . ? I1 C1 C5 Fe1 -129.2(6) . . . . ? C1 Fe1 C5 C4 117.5(6) . . . . ? C14 Fe1 C5 C4 -81.0(5) . . . . ? C13 Fe1 C5 C4 -122.3(4) . . . . ? C10 Fe1 C5 C4 -47.8(8) . . . . ? C11 Fe1 C5 C4 169.6(10) . . . . ? C12 Fe1 C5 C4 -162.9(4) . . . . ? C2 Fe1 C5 C4 80.4(4) . . . . ? C3 Fe1 C5 C4 36.9(4) . . . . ? C4 Fe1 C5 C1 -117.5(6) . . . . ? C14 Fe1 C5 C1 161.4(4) . . . . ? C13 Fe1 C5 C1 120.2(4) . . . . ? C10 Fe1 C5 C1 -165.3(6) . . . . ? C11 Fe1 C5 C1 52.1(12) . . . . ? C12 Fe1 C5 C1 79.5(5) . . . . ? C2 Fe1 C5 C1 -37.1(4) . . . . ? C3 Fe1 C5 C1 -80.6(4) . . . . ? C4 Fe1 C5 C6 119.7(7) . . . . ? C1 Fe1 C5 C6 -122.8(7) . . . . ? C14 Fe1 C5 C6 38.7(6) . . . . ? C13 Fe1 C5 C6 -2.5(6) . . . . ? C10 Fe1 C5 C6 71.9(9) . . . . ? C11 Fe1 C5 C6 -70.7(12) . . . . ? C12 Fe1 C5 C6 -43.2(6) . . . . ? C2 Fe1 C5 C6 -159.9(6) . . . . ? C3 Fe1 C5 C6 156.6(6) . . . . ? C4 C5 C6 O7 -19.8(11) . . . . ? C1 C5 C6 O7 166.2(7) . . . . ? Fe1 C5 C6 O7 -105.8(7) . . . . ? C4 C5 C6 O8 160.4(6) . . . . ? C1 C5 C6 O8 -13.6(10) . . . . ? Fe1 C5 C6 O8 74.4(7) . . . . ? O7 C6 O8 C9 -0.8(10) . . . . ? C5 C6 O8 C9 179.0(6) . . . . ? C5 Fe1 C10 C11 -164.8(6) . . . . ? C4 Fe1 C10 C11 161.1(5) . . . . ? C1 Fe1 C10 C11 49.2(12) . . . . ? C14 Fe1 C10 C11 -117.5(7) . . . . ? C13 Fe1 C10 C11 -80.8(5) . . . . ? C12 Fe1 C10 C11 -37.2(5) . . . . ? C2 Fe1 C10 C11 79.0(5) . . . . ? C3 Fe1 C10 C11 119.2(5) . . . . ? C5 Fe1 C10 C14 -47.3(9) . . . . ? C4 Fe1 C10 C14 -81.4(5) . . . . ? C1 Fe1 C10 C14 166.6(9) . . . . ? C13 Fe1 C10 C14 36.6(4) . . . . ? C11 Fe1 C10 C14 117.5(7) . . . . ? C12 Fe1 C10 C14 80.3(5) . . . . ? C2 Fe1 C10 C14 -163.5(4) . . . . ? C3 Fe1 C10 C14 -123.4(5) . . . . ? C14 C10 C11 C12 -1.3(9) . . . . ? Fe1 C10 C11 C12 59.0(6) . . . . ? C14 C10 C11 Fe1 -60.3(5) . . . . ? C5 Fe1 C11 C10 155.5(10) . . . . ? C4 Fe1 C11 C10 -40.5(9) . . . . ? C1 Fe1 C11 C10 -163.3(5) . . . . ? C14 Fe1 C11 C10 38.8(5) . . . . ? C13 Fe1 C11 C10 81.7(5) . . . . ? C12 Fe1 C11 C10 120.2(7) . . . . ? C2 Fe1 C11 C10 -121.4(5) . . . . ? C3 Fe1 C11 C10 -77.9(5) . . . . ? C5 Fe1 C11 C12 35.3(13) . . . . ? C4 Fe1 C11 C12 -160.7(6) . . . . ? C1 Fe1 C11 C12 76.4(6) . . . . ? C14 Fe1 C11 C12 -81.4(5) . . . . ? C13 Fe1 C11 C12 -38.5(5) . . . . ? C10 Fe1 C11 C12 -120.2(7) . . . . ? C2 Fe1 C11 C12 118.4(5) . . . . ? C3 Fe1 C11 C12 161.9(4) . . . . ? C10 C11 C12 C13 1.2(9) . . . . ? Fe1 C11 C12 C13 60.1(5) . . . . ? C10 C11 C12 Fe1 -58.9(5) . . . . ? C5 Fe1 C12 C13 74.0(5) . . . . ? C4 Fe1 C12 C13 34.1(12) . . . . ? C1 Fe1 C12 C13 118.2(5) . . . . ? C14 Fe1 C12 C13 -36.4(5) . . . . ? C10 Fe1 C12 C13 -80.5(5) . . . . ? C11 Fe1 C12 C13 -117.4(7) . . . . ? C2 Fe1 C12 C13 160.9(4) . . . . ? C3 Fe1 C12 C13 -160.4(7) . . . . ? C5 Fe1 C12 C11 -168.6(4) . . . . ? C4 Fe1 C12 C11 151.5(9) . . . . ? C1 Fe1 C12 C11 -124.4(5) . . . . ? C14 Fe1 C12 C11 81.0(5) . . . . ? C13 Fe1 C12 C11 117.4(7) . . . . ? C10 Fe1 C12 C11 36.9(5) . . . . ? C2 Fe1 C12 C11 -81.7(5) . . . . ? C3 Fe1 C12 C11 -43.0(10) . . . . ? C11 C12 C13 C14 -0.7(9) . . . . ? Fe1 C12 C13 C14 59.5(6) . . . . ? C11 C12 C13 Fe1 -60.2(6) . . . . ? C5 Fe1 C13 C14 114.8(5) . . . . ? C4 Fe1 C13 C14 71.8(5) . . . . ? C1 Fe1 C13 C14 158.2(4) . . . . ? C10 Fe1 C13 C14 -37.8(5) . . . . ? C11 Fe1 C13 C14 -81.5(5) . . . . ? C12 Fe1 C13 C14 -120.2(7) . . . . ? C2 Fe1 C13 C14 -168.1(7) . . . . ? C3 Fe1 C13 C14 37.1(11) . . . . ? C5 Fe1 C13 C12 -125.0(5) . . . . ? C4 Fe1 C13 C12 -168.1(5) . . . . ? C1 Fe1 C13 C12 -81.6(5) . . . . ? C14 Fe1 C13 C12 120.2(7) . . . . ? C10 Fe1 C13 C12 82.4(5) . . . . ? C11 Fe1 C13 C12 38.7(5) . . . . ? C2 Fe1 C13 C12 -47.9(10) . . . . ? C3 Fe1 C13 C12 157.3(8) . . . . ? C12 C13 C14 C10 -0.1(9) . . . . ? Fe1 C13 C14 C10 59.4(5) . . . . ? C12 C13 C14 Fe1 -59.5(6) . . . . ? C11 C10 C14 C13 0.9(8) . . . . ? Fe1 C10 C14 C13 -59.7(5) . . . . ? C11 C10 C14 Fe1 60.6(5) . . . . ? C5 Fe1 C14 C13 -82.1(5) . . . . ? C4 Fe1 C14 C13 -125.3(5) . . . . ? C1 Fe1 C14 C13 -50.4(9) . . . . ? C10 Fe1 C14 C13 119.6(6) . . . . ? C11 Fe1 C14 C13 81.3(5) . . . . ? C12 Fe1 C14 C13 37.3(5) . . . . ? C2 Fe1 C14 C13 166.2(8) . . . . ? C3 Fe1 C14 C13 -165.7(4) . . . . ? C5 Fe1 C14 C10 158.2(4) . . . . ? C4 Fe1 C14 C10 115.0(5) . . . . ? C1 Fe1 C14 C10 -170.0(6) . . . . ? C13 Fe1 C14 C10 -119.6(6) . . . . ? C11 Fe1 C14 C10 -38.3(5) . . . . ? C12 Fe1 C14 C10 -82.4(5) . . . . ? C2 Fe1 C14 C10 46.5(11) . . . . ? C3 Fe1 C14 C10 74.6(5) . . . . ? C24 Fe2 C21 C22 80.9(4) . . . . ? C25 Fe2 C21 C22 120.7(5) . . . . ? C34 Fe2 C21 C22 168.8(5) . . . . ? C23 Fe2 C21 C22 37.1(4) . . . . ? C31 Fe2 C21 C22 -108.6(4) . . . . ? C30 Fe2 C21 C22 -152.7(4) . . . . ? C32 Fe2 C21 C22 -67.9(5) . . . . ? C24 Fe2 C21 C25 -39.8(4) . . . . ? C34 Fe2 C21 C25 48.1(7) . . . . ? C23 Fe2 C21 C25 -83.5(4) . . . . ? C31 Fe2 C21 C25 130.7(4) . . . . ? C30 Fe2 C21 C25 86.6(4) . . . . ? C32 Fe2 C21 C25 171.4(4) . . . . ? C22 Fe2 C21 C25 -120.7(5) . . . . ? C24 Fe2 C21 I21 -162.7(5) . . . . ? C25 Fe2 C21 I21 -122.9(7) . . . . ? C34 Fe2 C21 I21 -74.8(7) . . . . ? C23 Fe2 C21 I21 153.5(5) . . . . ? C31 Fe2 C21 I21 7.8(6) . . . . ? C30 Fe2 C21 I21 -36.3(6) . . . . ? C32 Fe2 C21 I21 48.5(7) . . . . ? C22 Fe2 C21 I21 116.4(6) . . . . ? C25 C21 C22 C23 -1.0(8) . . . . ? Fe2 C21 C22 C23 -58.4(5) . . . . ? I21 C21 C22 C23 172.3(4) . . . . ? C25 C21 C22 Fe2 57.4(4) . . . . ? I21 C21 C22 Fe2 -129.3(5) . . . . ? C24 Fe2 C22 C21 -83.0(4) . . . . ? C25 Fe2 C22 C21 -37.9(4) . . . . ? C33 Fe2 C22 C21 175.3(4) . . . . ? C34 Fe2 C22 C21 -148.2(13) . . . . ? C23 Fe2 C22 C21 -120.2(5) . . . . ? C31 Fe2 C22 C21 90.6(4) . . . . ? C30 Fe2 C22 C21 54.8(7) . . . . ? C32 Fe2 C22 C21 134.0(4) . . . . ? C24 Fe2 C22 C23 37.3(4) . . . . ? C25 Fe2 C22 C23 82.4(4) . . . . ? C33 Fe2 C22 C23 -64.4(5) . . . . ? C34 Fe2 C22 C23 -28.0(16) . . . . ? C21 Fe2 C22 C23 120.2(5) . . . . ? C31 Fe2 C22 C23 -149.2(4) . . . . ? C30 Fe2 C22 C23 175.0(5) . . . . ? C32 Fe2 C22 C23 -105.8(4) . . . . ? C21 C22 C23 C24 0.5(8) . . . . ? Fe2 C22 C23 C24 -57.8(5) . . . . ? C21 C22 C23 Fe2 58.3(5) . . . . ? C25 Fe2 C23 C24 37.9(4) . . . . ? C33 Fe2 C23 C24 -105.1(4) . . . . ? C34 Fe2 C23 C24 -66.6(5) . . . . ? C21 Fe2 C23 C24 83.1(4) . . . . ? C31 Fe2 C23 C24 179.2(5) . . . . ? C30 Fe2 C23 C24 -47.2(15) . . . . ? C32 Fe2 C23 C24 -148.1(4) . . . . ? C22 Fe2 C23 C24 120.1(5) . . . . ? C24 Fe2 C23 C22 -120.1(5) . . . . ? C25 Fe2 C23 C22 -82.2(4) . . . . ? C33 Fe2 C23 C22 134.8(4) . . . . ? C34 Fe2 C23 C22 173.3(4) . . . . ? C21 Fe2 C23 C22 -37.1(4) . . . . ? C31 Fe2 C23 C22 59.0(6) . . . . ? C30 Fe2 C23 C22 -167.3(13) . . . . ? C32 Fe2 C23 C22 91.8(4) . . . . ? C22 C23 C24 C25 0.2(8) . . . . ? Fe2 C23 C24 C25 -58.7(4) . . . . ? C22 C23 C24 Fe2 58.9(5) . . . . ? C22 C23 C24 I24 -179.7(5) . . . . ? Fe2 C23 C24 I24 121.5(5) . . . . ? C25 Fe2 C24 C23 -120.4(5) . . . . ? C33 Fe2 C24 C23 89.9(4) . . . . ? C34 Fe2 C24 C23 132.4(4) . . . . ? C21 Fe2 C24 C23 -80.6(4) . . . . ? C30 Fe2 C24 C23 169.0(4) . . . . ? C32 Fe2 C24 C23 57.5(6) . . . . ? C22 Fe2 C24 C23 -37.1(4) . . . . ? C33 Fe2 C24 C25 -149.7(4) . . . . ? C34 Fe2 C24 C25 -107.2(4) . . . . ? C21 Fe2 C24 C25 39.8(4) . . . . ? C23 Fe2 C24 C25 120.4(5) . . . . ? C30 Fe2 C24 C25 -70.6(5) . . . . ? C32 Fe2 C24 C25 177.9(5) . . . . ? C22 Fe2 C24 C25 83.3(4) . . . . ? C25 Fe2 C24 I24 122.9(6) . . . . ? C33 Fe2 C24 I24 -26.8(5) . . . . ? C34 Fe2 C24 I24 15.7(5) . . . . ? C21 Fe2 C24 I24 162.7(5) . . . . ? C23 Fe2 C24 I24 -116.7(6) . . . . ? C30 Fe2 C24 I24 52.3(6) . . . . ? C32 Fe2 C24 I24 -59.2(7) . . . . ? C22 Fe2 C24 I24 -153.8(5) . . . . ? C23 C24 C25 C21 -0.8(7) . . . . ? Fe2 C24 C25 C21 -60.6(4) . . . . ? I24 C24 C25 C21 179.0(5) . . . . ? C23 C24 C25 C26 175.4(6) . . . . ? Fe2 C24 C25 C26 115.6(6) . . . . ? I24 C24 C25 C26 -4.8(10) . . . . ? C23 C24 C25 Fe2 59.8(5) . . . . ? I24 C24 C25 Fe2 -120.4(5) . . . . ? C22 C21 C25 C24 1.1(7) . . . . ? Fe2 C21 C25 C24 59.9(4) . . . . ? I21 C21 C25 C24 -171.7(5) . . . . ? C22 C21 C25 C26 -174.9(6) . . . . ? Fe2 C21 C25 C26 -116.1(7) . . . . ? I21 C21 C25 C26 12.3(10) . . . . ? C22 C21 C25 Fe2 -58.8(5) . . . . ? I21 C21 C25 Fe2 128.4(5) . . . . ? C33 Fe2 C25 C24 54.2(7) . . . . ? C34 Fe2 C25 C24 88.6(4) . . . . ? C21 Fe2 C25 C24 -116.5(5) . . . . ? C23 Fe2 C25 C24 -36.8(4) . . . . ? C31 Fe2 C25 C24 169.9(4) . . . . ? C30 Fe2 C25 C24 131.3(4) . . . . ? C22 Fe2 C25 C24 -80.1(4) . . . . ? C24 Fe2 C25 C21 116.5(5) . . . . ? C33 Fe2 C25 C21 170.7(5) . . . . ? C34 Fe2 C25 C21 -154.9(4) . . . . ? C23 Fe2 C25 C21 79.8(4) . . . . ? C31 Fe2 C25 C21 -73.6(5) . . . . ? C30 Fe2 C25 C21 -112.1(4) . . . . ? C22 Fe2 C25 C21 36.5(4) . . . . ? C24 Fe2 C25 C26 -119.8(6) . . . . ? C33 Fe2 C25 C26 -65.6(7) . . . . ? C34 Fe2 C25 C26 -31.2(6) . . . . ? C21 Fe2 C25 C26 123.7(7) . . . . ? C23 Fe2 C25 C26 -156.5(5) . . . . ? C31 Fe2 C25 C26 50.1(6) . . . . ? C30 Fe2 C25 C26 11.6(6) . . . . ? C22 Fe2 C25 C26 160.2(6) . . . . ? C24 C25 C26 O27 17.7(11) . . . . ? C21 C25 C26 O27 -167.1(7) . . . . ? Fe2 C25 C26 O27 103.7(7) . . . . ? C24 C25 C26 O28 -160.6(6) . . . . ? C21 C25 C26 O28 14.7(9) . . . . ? Fe2 C25 C26 O28 -74.5(6) . . . . ? O27 C26 O28 C29 -0.5(9) . . . . ? C25 C26 O28 C29 177.7(5) . . . . ? C24 Fe2 C30 C34 -62.9(5) . . . . ? C25 Fe2 C30 C34 -104.7(4) . . . . ? C33 Fe2 C30 C34 37.9(4) . . . . ? C21 Fe2 C30 C34 -149.6(4) . . . . ? C23 Fe2 C30 C34 -23.5(16) . . . . ? C31 Fe2 C30 C34 120.4(6) . . . . ? C32 Fe2 C30 C34 82.3(4) . . . . ? C22 Fe2 C30 C34 173.3(5) . . . . ? C24 Fe2 C30 C31 176.7(4) . . . . ? C25 Fe2 C30 C31 134.9(4) . . . . ? C33 Fe2 C30 C31 -82.5(5) . . . . ? C34 Fe2 C30 C31 -120.4(6) . . . . ? C21 Fe2 C30 C31 90.0(4) . . . . ? C23 Fe2 C30 C31 -143.9(13) . . . . ? C32 Fe2 C30 C31 -38.1(4) . . . . ? C22 Fe2 C30 C31 52.9(7) . . . . ? C34 C30 C31 C32 1.5(8) . . . . ? Fe2 C30 C31 C32 60.2(5) . . . . ? C34 C30 C31 Fe2 -58.7(5) . . . . ? C25 Fe2 C31 C32 176.2(4) . . . . ? C33 Fe2 C31 C32 -37.8(4) . . . . ? C34 Fe2 C31 C32 -81.4(5) . . . . ? C21 Fe2 C31 C32 132.6(4) . . . . ? C23 Fe2 C31 C32 49.2(7) . . . . ? C30 Fe2 C31 C32 -118.1(6) . . . . ? C22 Fe2 C31 C32 88.4(5) . . . . ? C25 Fe2 C31 C30 -65.7(5) . . . . ? C33 Fe2 C31 C30 80.3(5) . . . . ? C34 Fe2 C31 C30 36.7(4) . . . . ? C21 Fe2 C31 C30 -109.4(4) . . . . ? C23 Fe2 C31 C30 167.3(5) . . . . ? C32 Fe2 C31 C30 118.1(6) . . . . ? C22 Fe2 C31 C30 -153.5(4) . . . . ? C30 C31 C32 C33 -1.8(8) . . . . ? Fe2 C31 C32 C33 58.3(5) . . . . ? C30 C31 C32 Fe2 -60.1(5) . . . . ? C24 Fe2 C32 C31 168.7(5) . . . . ? C33 Fe2 C32 C31 119.5(7) . . . . ? C34 Fe2 C32 C31 81.7(5) . . . . ? C21 Fe2 C32 C31 -70.2(6) . . . . ? C23 Fe2 C32 C31 -153.8(4) . . . . ? C30 Fe2 C32 C31 38.3(5) . . . . ? C22 Fe2 C32 C31 -110.0(5) . . . . ? C24 Fe2 C32 C33 49.2(7) . . . . ? C34 Fe2 C32 C33 -37.8(5) . . . . ? C21 Fe2 C32 C33 170.3(5) . . . . ? C23 Fe2 C32 C33 86.7(5) . . . . ? C31 Fe2 C32 C33 -119.5(7) . . . . ? C30 Fe2 C32 C33 -81.2(5) . . . . ? C22 Fe2 C32 C33 130.5(5) . . . . ? C31 C32 C33 C34 1.4(9) . . . . ? Fe2 C32 C33 C34 60.5(5) . . . . ? C31 C32 C33 Fe2 -59.1(5) . . . . ? C24 Fe2 C33 C34 89.1(5) . . . . ? C25 Fe2 C33 C34 53.0(7) . . . . ? C23 Fe2 C33 C34 132.0(5) . . . . ? C31 Fe2 C33 C34 -81.4(5) . . . . ? C30 Fe2 C33 C34 -37.6(5) . . . . ? C32 Fe2 C33 C34 -118.6(7) . . . . ? C22 Fe2 C33 C34 169.8(4) . . . . ? C24 Fe2 C33 C32 -152.3(5) . . . . ? C25 Fe2 C33 C32 171.7(5) . . . . ? C34 Fe2 C33 C32 118.6(7) . . . . ? C23 Fe2 C33 C32 -109.4(5) . . . . ? C31 Fe2 C33 C32 37.2(5) . . . . ? C30 Fe2 C33 C32 81.0(5) . . . . ? C22 Fe2 C33 C32 -71.6(6) . . . . ? C31 C30 C34 C33 -0.6(8) . . . . ? Fe2 C30 C34 C33 -59.4(5) . . . . ? C31 C30 C34 Fe2 58.8(5) . . . . ? C32 C33 C34 C30 -0.5(8) . . . . ? Fe2 C33 C34 C30 60.1(5) . . . . ? C32 C33 C34 Fe2 -60.6(5) . . . . ? C24 Fe2 C34 C30 135.6(4) . . . . ? C25 Fe2 C34 C30 91.3(5) . . . . ? C33 Fe2 C34 C30 -118.8(6) . . . . ? C21 Fe2 C34 C30 58.3(7) . . . . ? C23 Fe2 C34 C30 174.2(4) . . . . ? C31 Fe2 C34 C30 -37.0(4) . . . . ? C32 Fe2 C34 C30 -80.6(5) . . . . ? C22 Fe2 C34 C30 -162.6(13) . . . . ? C24 Fe2 C34 C33 -105.6(5) . . . . ? C25 Fe2 C34 C33 -149.9(4) . . . . ? C21 Fe2 C34 C33 177.1(5) . . . . ? C23 Fe2 C34 C33 -67.0(6) . . . . ? C31 Fe2 C34 C33 81.8(5) . . . . ? C30 Fe2 C34 C33 118.8(6) . . . . ? C32 Fe2 C34 C33 38.2(5) . . . . ? C22 Fe2 C34 C33 -43.8(16) . . . . ? data_15c _database_code_depnum_ccdc_archive 'CCDC 755179' #TrackingRef 'CIF_Mongin.cif' _audit_creation_date 2009-11-06T13:44:43-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C16 H12 Fe N2)' _chemical_formula_sum 'C32 H24 Fe2 N4' _chemical_formula_weight 576.25 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.3522(6) _cell_length_b 8.7529(4) _cell_length_c 17.9951(6) _cell_angle_alpha 90 _cell_angle_beta 102.168(3) _cell_angle_gamma 90 _cell_volume 2517.76(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 24751 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.32 _exptl_crystal_density_diffrn 1.52 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.182 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.582 _exptl_absorpt_correction_T_max 0.685 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.620951E-1 _diffrn_orient_matrix_ub_12 -0.131974E-1 _diffrn_orient_matrix_ub_13 -0.85813E-2 _diffrn_orient_matrix_ub_21 -0.71894E-2 _diffrn_orient_matrix_ub_22 0.647457E-1 _diffrn_orient_matrix_ub_23 -0.466868E-1 _diffrn_orient_matrix_ub_31 0.38061E-2 _diffrn_orient_matrix_ub_32 -0.930122E-1 _diffrn_orient_matrix_ub_33 -0.31281E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_unetI/netI 0.0364 _diffrn_reflns_number 34649 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 5773 _reflns_number_gt 4303 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0412P)^2^+1.0018P] 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_number_reflns 5773 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0834 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.414 _refine_diff_density_min -0.611 _refine_diff_density_rms 0.075 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.302989(16) -0.69707(3) 0.192625(15) 0.01946(8) Uani 1 1 d . . . C1 C 0.39802(13) -0.8346(3) 0.17352(13) 0.0318(5) Uani 1 1 d . . . H1 H 0.3985 -0.9431 0.1732 0.038 Uiso 1 1 calc R . . C2 C 0.42728(13) -0.7410(3) 0.23752(13) 0.0326(5) Uani 1 1 d . . . H2 H 0.4504 -0.7755 0.2876 0.039 Uiso 1 1 calc R . . C3 C 0.41604(12) -0.5861(3) 0.21384(12) 0.0290(5) Uani 1 1 d . . . H3 H 0.4306 -0.4987 0.2452 0.035 Uiso 1 1 calc R . . C4 C 0.37912(12) -0.5853(2) 0.13479(11) 0.0260(4) Uani 1 1 d . . . H4 H 0.3645 -0.4972 0.104 0.031 Uiso 1 1 calc R . . C5 C 0.36790(13) -0.7396(3) 0.10996(12) 0.0287(5) Uani 1 1 d . . . H5 H 0.3444 -0.7729 0.0598 0.034 Uiso 1 1 calc R . . C11 C 0.21000(12) -0.8349(2) 0.21554(11) 0.0241(4) Uani 1 1 d . . . H11 H 0.2117 -0.9429 0.2206 0.029 Uiso 1 1 calc R . . C12 C 0.23521(12) -0.7281(2) 0.27581(11) 0.0258(4) Uani 1 1 d . . . H12 H 0.2565 -0.753 0.3277 0.031 Uiso 1 1 calc R . . C13 C 0.22316(12) -0.5782(2) 0.24525(11) 0.0244(4) Uani 1 1 d . . . H13 H 0.2348 -0.4854 0.2729 0.029 Uiso 1 1 calc R . . C14 C 0.19018(11) -0.5922(2) 0.16500(10) 0.0214(4) Uani 1 1 d . . . C15 C 0.16842(12) -0.4644(2) 0.11524(11) 0.0239(4) Uani 1 1 d . . . N36 N 0.14926(13) -0.3576(2) 0.07900(11) 0.0388(5) Uani 1 1 d . . . C17 C 0.18162(11) -0.7524(2) 0.14587(11) 0.0208(4) Uani 1 1 d . . . C18 C 0.15027(11) -0.8200(2) 0.07017(11) 0.0214(4) Uani 1 1 d . . . N19 N 0.13940(13) -0.7246(2) 0.01060(10) 0.0340(4) Uani 1 1 d . . . C20 C 0.10968(16) -0.7846(3) -0.05830(13) 0.0400(6) Uani 1 1 d . . . H20 H 0.1023 -0.7181 -0.1009 0.048 Uiso 1 1 calc R . . C21 C 0.08908(14) -0.9360(2) -0.07137(12) 0.0339(5) Uani 1 1 d . . . H21 H 0.0673 -0.9725 -0.1214 0.041 Uiso 1 1 calc R . . C22 C 0.10093(14) -1.0332(2) -0.00982(12) 0.0343(5) Uani 1 1 d . . . H22 H 0.088 -1.1388 -0.0166 0.041 Uiso 1 1 calc R . . C23 C 0.13186(13) -0.9748(2) 0.06194(12) 0.0285(5) Uani 1 1 d . . . H23 H 0.1404 -1.0398 0.1052 0.034 Uiso 1 1 calc R . . Fe2 Fe 0.354724(16) -0.20504(3) 0.435826(14) 0.01940(8) Uani 1 1 d . . . C31 C 0.33117(14) -0.3418(2) 0.52191(12) 0.0317(5) Uani 1 1 d . . . H31 H 0.2944 -0.3196 0.5549 0.038 Uiso 1 1 calc R . . C32 C 0.41740(15) -0.3040(2) 0.53456(12) 0.0345(5) Uani 1 1 d . . . H32 H 0.4485 -0.252 0.5777 0.041 Uiso 1 1 calc R . . C33 C 0.44905(13) -0.3573(3) 0.47165(13) 0.0344(5) Uani 1 1 d . . . H33 H 0.5049 -0.3465 0.4651 0.041 Uiso 1 1 calc R . . C34 C 0.38261(14) -0.4293(2) 0.42048(12) 0.0315(5) Uani 1 1 d . . . H34 H 0.3862 -0.4764 0.3737 0.038 Uiso 1 1 calc R . . C35 C 0.30984(14) -0.4190(2) 0.45105(12) 0.0312(5) Uani 1 1 d . . . H35 H 0.256 -0.457 0.4281 0.037 Uiso 1 1 calc R . . C41 C 0.29272(12) -0.0016(2) 0.43833(11) 0.0231(4) Uani 1 1 d . . . H41 H 0.2616 0.0292 0.4748 0.028 Uiso 1 1 calc R . . C42 C 0.37968(12) 0.0257(2) 0.44317(11) 0.0255(4) Uani 1 1 d . . . H42 H 0.416 0.0781 0.4833 0.031 Uiso 1 1 calc R . . C43 C 0.40291(12) -0.0383(2) 0.37826(11) 0.0238(4) Uani 1 1 d . . . H43 H 0.4573 -0.037 0.3674 0.029 Uiso 1 1 calc R . . C44 C 0.32917(11) -0.1057(2) 0.33180(10) 0.0208(4) Uani 1 1 d . . . C45 C 0.33084(12) -0.1815(2) 0.26153(11) 0.0235(4) Uani 1 1 d . . . N46 N 0.33892(12) -0.2367(2) 0.20571(10) 0.0336(4) Uani 1 1 d . . . C47 C 0.26007(11) -0.0829(2) 0.36945(10) 0.0207(4) Uani 1 1 d . . . C48 C 0.17255(11) -0.1310(2) 0.34198(10) 0.0205(4) Uani 1 1 d . . . N49 N 0.15445(11) -0.1957(2) 0.27257(10) 0.0301(4) Uani 1 1 d . . . C50 C 0.07500(14) -0.2374(3) 0.24535(13) 0.0386(5) Uani 1 1 d . . . H50 H 0.0615 -0.2835 0.1965 0.046 Uiso 1 1 calc R . . C51 C 0.01115(14) -0.2168(3) 0.28471(13) 0.0370(5) Uani 1 1 d . . . H51 H -0.0445 -0.2475 0.2632 0.044 Uiso 1 1 calc R . . C52 C 0.03077(13) -0.1506(3) 0.35590(12) 0.0333(5) Uani 1 1 d . . . H52 H -0.0113 -0.1356 0.3845 0.04 Uiso 1 1 calc R . . C53 C 0.11221(12) -0.1065(2) 0.38499(11) 0.0265(4) Uani 1 1 d . . . H53 H 0.1269 -0.06 0.4337 0.032 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 0.01562(14) 0.02294(15) 0.01991(15) 0.00348(11) 0.00393(10) 0.00050(10) C1 0.0222(10) 0.0315(11) 0.0445(13) 0.0069(10) 0.0133(9) 0.0069(9) C2 0.0171(10) 0.0454(13) 0.0338(12) 0.0123(10) 0.0018(8) 0.0043(9) C3 0.0175(9) 0.0371(12) 0.0332(11) -0.0013(9) 0.0071(8) -0.0058(9) C4 0.0213(10) 0.0303(11) 0.0285(10) 0.0063(9) 0.0100(8) -0.0013(8) C5 0.0222(10) 0.0375(12) 0.0291(11) -0.0029(9) 0.0113(8) 0.0000(9) C11 0.0203(9) 0.0251(10) 0.0275(10) 0.0097(8) 0.0061(8) 0.0015(8) C12 0.0227(10) 0.0339(11) 0.0217(10) 0.0050(8) 0.0066(8) 0.0001(8) C13 0.0235(10) 0.0283(10) 0.0225(10) -0.0011(8) 0.0076(8) 0.0009(8) C14 0.0177(9) 0.0240(10) 0.0229(9) 0.0042(8) 0.0054(7) 0.0018(8) C15 0.0249(10) 0.0233(10) 0.0233(10) -0.0016(8) 0.0046(8) 0.0009(8) N36 0.0587(13) 0.0251(10) 0.0307(10) 0.0026(8) 0.0053(9) 0.0057(9) C17 0.0164(9) 0.0220(9) 0.0247(10) 0.0035(8) 0.0055(7) 0.0000(7) C18 0.0160(9) 0.0227(10) 0.0257(10) 0.0015(8) 0.0045(7) 0.0006(7) N19 0.0475(12) 0.0242(9) 0.0263(9) 0.0038(8) -0.0017(8) -0.0049(8) C20 0.0546(15) 0.0333(13) 0.0275(11) 0.0043(10) -0.0023(10) -0.0032(11) C21 0.0368(12) 0.0318(12) 0.0299(11) -0.0043(9) -0.0002(9) 0.0012(9) C22 0.0398(13) 0.0228(11) 0.0390(13) -0.0051(9) 0.0053(10) -0.0002(9) C23 0.0328(11) 0.0224(10) 0.0306(11) 0.0035(9) 0.0074(9) 0.0014(8) Fe2 0.01755(14) 0.02327(15) 0.01732(14) 0.00251(11) 0.00356(10) 0.00276(11) C31 0.0405(13) 0.0320(11) 0.0258(11) 0.0095(9) 0.0139(9) 0.0043(10) C32 0.0407(13) 0.0323(12) 0.0244(11) 0.0053(9) -0.0067(9) 0.0041(10) C33 0.0270(11) 0.0303(11) 0.0454(13) 0.0142(10) 0.0063(10) 0.0095(9) C34 0.0428(13) 0.0249(11) 0.0272(11) 0.0059(9) 0.0080(9) 0.0074(9) C35 0.0355(12) 0.0275(11) 0.0293(11) 0.0080(9) 0.0038(9) -0.0023(9) C41 0.0228(10) 0.0246(10) 0.0224(10) -0.0005(8) 0.0056(8) 0.0040(8) C42 0.0251(10) 0.0245(10) 0.0259(10) -0.0018(8) 0.0030(8) -0.0020(8) C43 0.0212(10) 0.0253(10) 0.0251(10) 0.0037(8) 0.0052(8) -0.0005(8) C44 0.0204(9) 0.0222(9) 0.0203(9) 0.0031(8) 0.0052(7) 0.0022(8) C45 0.0221(10) 0.0254(10) 0.0232(10) 0.0064(8) 0.0054(8) 0.0014(8) N46 0.0404(11) 0.0353(10) 0.0273(10) -0.0018(8) 0.0124(8) -0.0001(8) C47 0.0207(9) 0.0213(9) 0.0205(9) 0.0032(8) 0.0055(7) 0.0031(8) C48 0.0204(9) 0.0190(9) 0.0215(9) 0.0040(8) 0.0029(7) 0.0026(7) N49 0.0212(9) 0.0405(10) 0.0284(9) -0.0074(8) 0.0050(7) -0.0011(8) C50 0.0254(11) 0.0537(14) 0.0343(12) -0.0115(11) 0.0009(9) -0.0050(10) C51 0.0209(11) 0.0495(14) 0.0391(13) 0.0016(11) 0.0025(9) -0.0045(10) C52 0.0213(10) 0.0447(13) 0.0361(12) 0.0058(10) 0.0109(9) 0.0027(9) C53 0.0235(10) 0.0326(11) 0.0236(10) 0.0018(9) 0.0056(8) 0.0023(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C14 2.0263(18) . ? Fe1 C4 2.0336(19) . ? Fe1 C5 2.036(2) . ? Fe1 C17 2.0438(18) . ? Fe1 C11 2.0497(19) . ? Fe1 C13 2.0506(19) . ? Fe1 C1 2.051(2) . ? Fe1 C3 2.0517(19) . ? Fe1 C2 2.059(2) . ? Fe1 C12 2.060(2) . ? C1 C2 1.412(3) . ? C1 C5 1.416(3) . ? C1 H1 0.95 . ? C2 C3 1.422(3) . ? C2 H2 0.95 . ? C3 C4 1.424(3) . ? C3 H3 0.95 . ? C4 C5 1.422(3) . ? C4 H4 0.95 . ? C5 H5 0.95 . ? C11 C12 1.425(3) . ? C11 C17 1.436(3) . ? C11 H11 0.95 . ? C12 C13 1.421(3) . ? C12 H12 0.95 . ? C13 C14 1.436(3) . ? C13 H13 0.95 . ? C14 C15 1.430(3) . ? C14 C17 1.444(3) . ? C15 N36 1.145(3) . ? C17 C18 1.474(3) . ? C18 N19 1.341(3) . ? C18 C23 1.390(3) . ? N19 C20 1.340(3) . ? C20 C21 1.376(3) . ? C20 H20 0.95 . ? C21 C22 1.377(3) . ? C21 H21 0.95 . ? C22 C23 1.382(3) . ? C22 H22 0.95 . ? C23 H23 0.95 . ? Fe2 C44 2.0263(18) . ? Fe2 C33 2.037(2) . ? Fe2 C43 2.0415(19) . ? Fe2 C47 2.0458(18) . ? Fe2 C32 2.047(2) . ? Fe2 C34 2.047(2) . ? Fe2 C35 2.050(2) . ? Fe2 C41 2.0546(19) . ? Fe2 C31 2.057(2) . ? Fe2 C42 2.059(2) . ? C31 C35 1.420(3) . ? C31 C32 1.419(3) . ? C31 H31 0.95 . ? C32 C33 1.419(3) . ? C32 H32 0.95 . ? C33 C34 1.416(3) . ? C33 H33 0.95 . ? C34 C35 1.415(3) . ? C34 H34 0.95 . ? C35 H35 0.95 . ? C41 C42 1.426(3) . ? C41 C47 1.432(3) . ? C41 H41 0.95 . ? C42 C43 1.418(3) . ? C42 H42 0.95 . ? C43 C44 1.441(3) . ? C43 H43 0.95 . ? C44 C45 1.433(3) . ? C44 C47 1.448(3) . ? C45 N46 1.147(3) . ? C47 C48 1.473(3) . ? C48 N49 1.346(3) . ? C48 C53 1.393(3) . ? N49 C50 1.339(3) . ? C50 C51 1.391(3) . ? C50 H50 0.95 . ? C51 C52 1.381(3) . ? C51 H51 0.95 . ? C52 C53 1.379(3) . ? C52 H52 0.95 . ? C53 H53 0.95 . ? 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 C14 Fe1 C4 106.29(8) . . ? C14 Fe1 C5 119.44(8) . . ? C4 Fe1 C5 40.90(9) . . ? C14 Fe1 C17 41.55(8) . . ? C4 Fe1 C17 123.32(8) . . ? C5 Fe1 C17 105.46(8) . . ? C14 Fe1 C11 68.92(8) . . ? C4 Fe1 C11 161.09(8) . . ? C5 Fe1 C11 124.24(8) . . ? C17 Fe1 C11 41.08(7) . . ? C14 Fe1 C13 41.25(7) . . ? C4 Fe1 C13 120.68(8) . . ? C5 Fe1 C13 155.64(8) . . ? C17 Fe1 C13 69.69(8) . . ? C11 Fe1 C13 68.55(8) . . ? C14 Fe1 C1 155.15(9) . . ? C4 Fe1 C1 68.24(9) . . ? C5 Fe1 C1 40.54(9) . . ? C17 Fe1 C1 119.75(9) . . ? C11 Fe1 C1 107.98(9) . . ? C13 Fe1 C1 162.51(8) . . ? C14 Fe1 C3 124.69(8) . . ? C4 Fe1 C3 40.78(8) . . ? C5 Fe1 C3 68.56(9) . . ? C17 Fe1 C3 161.35(8) . . ? C11 Fe1 C3 156.74(8) . . ? C13 Fe1 C3 108.07(8) . . ? C1 Fe1 C3 67.93(9) . . ? C14 Fe1 C2 162.40(9) . . ? C4 Fe1 C2 68.32(8) . . ? C5 Fe1 C2 68.22(9) . . ? C17 Fe1 C2 155.47(9) . . ? C11 Fe1 C2 121.59(8) . . ? C13 Fe1 C2 125.84(9) . . ? C1 Fe1 C2 40.18(9) . . ? C3 Fe1 C2 40.47(9) . . ? C14 Fe1 C12 68.69(8) . . ? C4 Fe1 C12 156.44(8) . . ? C5 Fe1 C12 161.86(9) . . ? C17 Fe1 C12 69.10(8) . . ? C11 Fe1 C12 40.58(8) . . ? C13 Fe1 C12 40.44(8) . . ? C1 Fe1 C12 125.95(8) . . ? C3 Fe1 C12 121.94(8) . . ? C2 Fe1 C12 109.15(8) . . ? C2 C1 C5 108.58(19) . . ? C2 C1 Fe1 70.20(12) . . ? C5 C1 Fe1 69.14(11) . . ? C2 C1 H1 125.7 . . ? C5 C1 H1 125.7 . . ? Fe1 C1 H1 126.5 . . ? C1 C2 C3 107.98(18) . . ? C1 C2 Fe1 69.61(12) . . ? C3 C2 Fe1 69.49(11) . . ? C1 C2 H2 126 . . ? C3 C2 H2 126 . . ? Fe1 C2 H2 126.5 . . ? C2 C3 C4 107.74(19) . . ? C2 C3 Fe1 70.04(12) . . ? C4 C3 Fe1 68.93(11) . . ? C2 C3 H3 126.1 . . ? C4 C3 H3 126.1 . . ? Fe1 C3 H3 126.5 . . ? C5 C4 C3 108.01(19) . . ? C5 C4 Fe1 69.62(11) . . ? C3 C4 Fe1 70.29(11) . . ? C5 C4 H4 126 . . ? C3 C4 H4 126 . . ? Fe1 C4 H4 125.7 . . ? C1 C5 C4 107.70(19) . . ? C1 C5 Fe1 70.32(12) . . ? C4 C5 Fe1 69.48(11) . . ? C1 C5 H5 126.2 . . ? C4 C5 H5 126.2 . . ? Fe1 C5 H5 125.6 . . ? C12 C11 C17 108.86(17) . . ? C12 C11 Fe1 70.09(11) . . ? C17 C11 Fe1 69.24(11) . . ? C12 C11 H11 125.6 . . ? C17 C11 H11 125.6 . . ? Fe1 C11 H11 126.7 . . ? C13 C12 C11 108.47(17) . . ? C13 C12 Fe1 69.43(11) . . ? C11 C12 Fe1 69.33(11) . . ? C13 C12 H12 125.8 . . ? C11 C12 H12 125.8 . . ? Fe1 C12 H12 127 . . ? C12 C13 C14 107.60(17) . . ? C12 C13 Fe1 70.13(11) . . ? C14 C13 Fe1 68.47(11) . . ? C12 C13 H13 126.2 . . ? C14 C13 H13 126.2 . . ? Fe1 C13 H13 126.8 . . ? C15 C14 C13 123.64(18) . . ? C15 C14 C17 127.70(17) . . ? C13 C14 C17 108.64(17) . . ? C15 C14 Fe1 126.97(14) . . ? C13 C14 Fe1 70.28(11) . . ? C17 C14 Fe1 69.88(10) . . ? N36 C15 C14 175.7(2) . . ? C11 C17 C14 106.43(16) . . ? C11 C17 C18 126.18(18) . . ? C14 C17 C18 127.39(17) . . ? C11 C17 Fe1 69.68(11) . . ? C14 C17 Fe1 68.58(10) . . ? C18 C17 Fe1 126.42(13) . . ? N19 C18 C23 122.21(18) . . ? N19 C18 C17 116.78(17) . . ? C23 C18 C17 121.00(18) . . ? C20 N19 C18 117.18(18) . . ? N19 C20 C21 124.3(2) . . ? N19 C20 H20 117.8 . . ? C21 C20 H20 117.8 . . ? C22 C21 C20 118.0(2) . . ? C22 C21 H21 121 . . ? C20 C21 H21 121 . . ? C21 C22 C23 119.0(2) . . ? C21 C22 H22 120.5 . . ? C23 C22 H22 120.5 . . ? C22 C23 C18 119.26(19) . . ? C22 C23 H23 120.4 . . ? C18 C23 H23 120.4 . . ? C44 Fe2 C33 124.62(9) . . ? C44 Fe2 C43 41.48(7) . . ? C33 Fe2 C43 106.30(9) . . ? C44 Fe2 C47 41.67(7) . . ? C33 Fe2 C47 162.85(9) . . ? C43 Fe2 C47 69.87(7) . . ? C44 Fe2 C32 162.10(9) . . ? C33 Fe2 C32 40.66(9) . . ? C43 Fe2 C32 124.52(9) . . ? C47 Fe2 C32 155.05(9) . . ? C44 Fe2 C34 107.19(8) . . ? C33 Fe2 C34 40.56(9) . . ? C43 Fe2 C34 119.75(8) . . ? C47 Fe2 C34 125.79(8) . . ? C32 Fe2 C34 68.06(9) . . ? C44 Fe2 C35 120.36(8) . . ? C33 Fe2 C35 68.22(9) . . ? C43 Fe2 C35 155.21(8) . . ? C47 Fe2 C35 107.87(8) . . ? C32 Fe2 C35 68.01(9) . . ? C34 Fe2 C35 40.41(9) . . ? C44 Fe2 C41 68.99(8) . . ? C33 Fe2 C41 154.71(9) . . ? C43 Fe2 C41 68.69(8) . . ? C47 Fe2 C41 40.88(7) . . ? C32 Fe2 C41 120.45(8) . . ? C34 Fe2 C41 163.57(8) . . ? C35 Fe2 C41 126.61(8) . . ? C44 Fe2 C31 155.58(8) . . ? C33 Fe2 C31 68.32(9) . . ? C43 Fe2 C31 162.10(8) . . ? C47 Fe2 C31 120.33(8) . . ? C32 Fe2 C31 40.46(9) . . ? C34 Fe2 C31 68.03(9) . . ? C35 Fe2 C31 40.44(9) . . ? C41 Fe2 C31 108.44(8) . . ? C44 Fe2 C42 68.76(8) . . ? C33 Fe2 C42 119.64(9) . . ? C43 Fe2 C42 40.45(8) . . ? C47 Fe2 C42 68.93(8) . . ? C32 Fe2 C42 107.64(8) . . ? C34 Fe2 C42 154.48(9) . . ? C35 Fe2 C42 163.48(9) . . ? C41 Fe2 C42 40.57(8) . . ? C31 Fe2 C42 126.04(9) . . ? C35 C31 C32 107.62(19) . . ? C35 C31 Fe2 69.52(12) . . ? C32 C31 Fe2 69.37(12) . . ? C35 C31 H31 126.2 . . ? C32 C31 H31 126.2 . . ? Fe2 C31 H31 126.5 . . ? C33 C32 C31 108.20(19) . . ? C33 C32 Fe2 69.31(12) . . ? C31 C32 Fe2 70.17(12) . . ? C33 C32 H32 125.9 . . ? C31 C32 H32 125.9 . . ? Fe2 C32 H32 126.2 . . ? C34 C33 C32 107.8(2) . . ? C34 C33 Fe2 70.09(12) . . ? C32 C33 Fe2 70.02(12) . . ? C34 C33 H33 126.1 . . ? C32 C33 H33 126.1 . . ? Fe2 C33 H33 125.4 . . ? C35 C34 C33 108.2(2) . . ? C35 C34 Fe2 69.93(12) . . ? C33 C34 Fe2 69.36(12) . . ? C35 C34 H34 125.9 . . ? C33 C34 H34 125.9 . . ? Fe2 C34 H34 126.4 . . ? C34 C35 C31 108.17(19) . . ? C34 C35 Fe2 69.67(12) . . ? C31 C35 Fe2 70.04(12) . . ? C34 C35 H35 125.9 . . ? C31 C35 H35 125.9 . . ? Fe2 C35 H35 126 . . ? C42 C41 C47 108.73(17) . . ? C42 C41 Fe2 69.88(11) . . ? C47 C41 Fe2 69.23(11) . . ? C42 C41 H41 125.6 . . ? C47 C41 H41 125.6 . . ? Fe2 C41 H41 126.8 . . ? C43 C42 C41 108.69(17) . . ? C43 C42 Fe2 69.11(11) . . ? C41 C42 Fe2 69.54(11) . . ? C43 C42 H42 125.7 . . ? C41 C42 H42 125.7 . . ? Fe2 C42 H42 127.3 . . ? C42 C43 C44 107.63(17) . . ? C42 C43 Fe2 70.44(11) . . ? C44 C43 Fe2 68.69(10) . . ? C42 C43 H43 126.2 . . ? C44 C43 H43 126.2 . . ? Fe2 C43 H43 126.2 . . ? C45 C44 C43 122.14(17) . . ? C45 C44 C47 129.64(17) . . ? C43 C44 C47 108.21(16) . . ? C45 C44 Fe2 125.29(14) . . ? C43 C44 Fe2 69.83(10) . . ? C47 C44 Fe2 69.89(10) . . ? N46 C45 C44 174.1(2) . . ? C41 C47 C44 106.73(16) . . ? C41 C47 C48 126.23(17) . . ? C44 C47 C48 127.02(17) . . ? C41 C47 Fe2 69.89(10) . . ? C44 C47 Fe2 68.44(10) . . ? C48 C47 Fe2 127.48(13) . . ? N49 C48 C53 122.50(17) . . ? N49 C48 C47 116.07(16) . . ? C53 C48 C47 121.41(17) . . ? C50 N49 C48 117.42(18) . . ? N49 C50 C51 123.6(2) . . ? N49 C50 H50 118.2 . . ? C51 C50 H50 118.2 . . ? C52 C51 C50 118.3(2) . . ? C52 C51 H51 120.8 . . ? C50 C51 H51 120.8 . . ? C53 C52 C51 119.1(2) . . ? C53 C52 H52 120.4 . . ? C51 C52 H52 120.4 . . ? C52 C53 C48 119.09(19) . . ? C52 C53 H53 120.5 . . ? C48 C53 H53 120.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C14 Fe1 C1 C2 163.49(18) . . . . ? C4 Fe1 C1 C2 81.73(13) . . . . ? C5 Fe1 C1 C2 119.97(18) . . . . ? C17 Fe1 C1 C2 -161.32(12) . . . . ? C11 Fe1 C1 C2 -117.99(13) . . . . ? C13 Fe1 C1 C2 -42.4(3) . . . . ? C3 Fe1 C1 C2 37.61(12) . . . . ? C12 Fe1 C1 C2 -76.67(15) . . . . ? C14 Fe1 C1 C5 43.5(2) . . . . ? C4 Fe1 C1 C5 -38.24(12) . . . . ? C17 Fe1 C1 C5 78.70(14) . . . . ? C11 Fe1 C1 C5 122.04(13) . . . . ? C13 Fe1 C1 C5 -162.4(2) . . . . ? C3 Fe1 C1 C5 -82.36(13) . . . . ? C2 Fe1 C1 C5 -119.97(18) . . . . ? C12 Fe1 C1 C5 163.36(12) . . . . ? C5 C1 C2 C3 -0.5(2) . . . . ? Fe1 C1 C2 C3 -59.10(14) . . . . ? C5 C1 C2 Fe1 58.65(14) . . . . ? C14 Fe1 C2 C1 -156.7(2) . . . . ? C4 Fe1 C2 C1 -81.51(14) . . . . ? C5 Fe1 C2 C1 -37.33(13) . . . . ? C17 Fe1 C2 C1 42.1(2) . . . . ? C11 Fe1 C2 C1 80.42(15) . . . . ? C13 Fe1 C2 C1 165.51(12) . . . . ? C3 Fe1 C2 C1 -119.38(18) . . . . ? C12 Fe1 C2 C1 123.50(13) . . . . ? C14 Fe1 C2 C3 -37.4(3) . . . . ? C4 Fe1 C2 C3 37.86(13) . . . . ? C5 Fe1 C2 C3 82.05(14) . . . . ? C17 Fe1 C2 C3 161.43(17) . . . . ? C11 Fe1 C2 C3 -160.20(12) . . . . ? C13 Fe1 C2 C3 -75.11(15) . . . . ? C1 Fe1 C2 C3 119.38(18) . . . . ? C12 Fe1 C2 C3 -117.12(13) . . . . ? C1 C2 C3 C4 0.4(2) . . . . ? Fe1 C2 C3 C4 -58.81(13) . . . . ? C1 C2 C3 Fe1 59.17(14) . . . . ? C14 Fe1 C3 C2 167.11(12) . . . . ? C4 Fe1 C3 C2 -119.16(18) . . . . ? C5 Fe1 C3 C2 -81.15(14) . . . . ? C17 Fe1 C3 C2 -155.6(2) . . . . ? C11 Fe1 C3 C2 46.9(3) . . . . ? C13 Fe1 C3 C2 124.50(13) . . . . ? C1 Fe1 C3 C2 -37.35(13) . . . . ? C12 Fe1 C3 C2 82.24(15) . . . . ? C14 Fe1 C3 C4 -73.73(15) . . . . ? C5 Fe1 C3 C4 38.01(13) . . . . ? C17 Fe1 C3 C4 -36.4(3) . . . . ? C11 Fe1 C3 C4 166.10(19) . . . . ? C13 Fe1 C3 C4 -116.33(13) . . . . ? C1 Fe1 C3 C4 81.81(14) . . . . ? C2 Fe1 C3 C4 119.16(18) . . . . ? C12 Fe1 C3 C4 -158.60(12) . . . . ? C2 C3 C4 C5 -0.1(2) . . . . ? Fe1 C3 C4 C5 -59.64(14) . . . . ? C2 C3 C4 Fe1 59.51(14) . . . . ? C14 Fe1 C4 C5 -116.41(12) . . . . ? C17 Fe1 C4 C5 -74.23(14) . . . . ? C11 Fe1 C4 C5 -44.1(3) . . . . ? C13 Fe1 C4 C5 -158.89(12) . . . . ? C1 Fe1 C4 C5 37.92(12) . . . . ? C3 Fe1 C4 C5 118.91(18) . . . . ? C2 Fe1 C4 C5 81.32(13) . . . . ? C12 Fe1 C4 C5 169.69(18) . . . . ? C14 Fe1 C4 C3 124.68(13) . . . . ? C5 Fe1 C4 C3 -118.91(18) . . . . ? C17 Fe1 C4 C3 166.87(12) . . . . ? C11 Fe1 C4 C3 -163.0(2) . . . . ? C13 Fe1 C4 C3 82.20(14) . . . . ? C1 Fe1 C4 C3 -80.99(14) . . . . ? C2 Fe1 C4 C3 -37.59(13) . . . . ? C12 Fe1 C4 C3 50.8(2) . . . . ? C2 C1 C5 C4 0.4(2) . . . . ? Fe1 C1 C5 C4 59.67(14) . . . . ? C2 C1 C5 Fe1 -59.30(14) . . . . ? C3 C4 C5 C1 -0.1(2) . . . . ? Fe1 C4 C5 C1 -60.21(14) . . . . ? C3 C4 C5 Fe1 60.06(14) . . . . ? C14 Fe1 C5 C1 -160.60(12) . . . . ? C4 Fe1 C5 C1 118.59(18) . . . . ? C17 Fe1 C5 C1 -117.95(13) . . . . ? C11 Fe1 C5 C1 -77.23(15) . . . . ? C13 Fe1 C5 C1 167.27(18) . . . . ? C3 Fe1 C5 C1 80.69(14) . . . . ? C2 Fe1 C5 C1 37.01(13) . . . . ? C12 Fe1 C5 C1 -48.1(3) . . . . ? C14 Fe1 C5 C4 80.81(13) . . . . ? C17 Fe1 C5 C4 123.46(12) . . . . ? C11 Fe1 C5 C4 164.18(11) . . . . ? C13 Fe1 C5 C4 48.7(2) . . . . ? C1 Fe1 C5 C4 -118.59(18) . . . . ? C3 Fe1 C5 C4 -37.90(12) . . . . ? C2 Fe1 C5 C4 -81.59(13) . . . . ? C12 Fe1 C5 C4 -166.7(2) . . . . ? C14 Fe1 C11 C12 -81.45(12) . . . . ? C4 Fe1 C11 C12 -160.0(2) . . . . ? C5 Fe1 C11 C12 166.54(12) . . . . ? C17 Fe1 C11 C12 -120.33(16) . . . . ? C13 Fe1 C11 C12 -37.03(11) . . . . ? C1 Fe1 C11 C12 124.74(12) . . . . ? C3 Fe1 C11 C12 48.9(3) . . . . ? C2 Fe1 C11 C12 82.76(14) . . . . ? C14 Fe1 C11 C17 38.88(11) . . . . ? C4 Fe1 C11 C17 -39.7(3) . . . . ? C5 Fe1 C11 C17 -73.13(14) . . . . ? C13 Fe1 C11 C17 83.30(12) . . . . ? C1 Fe1 C11 C17 -114.93(12) . . . . ? C3 Fe1 C11 C17 169.26(19) . . . . ? C2 Fe1 C11 C17 -156.91(12) . . . . ? C12 Fe1 C11 C17 120.33(16) . . . . ? C17 C11 C12 C13 0.0(2) . . . . ? Fe1 C11 C12 C13 58.54(14) . . . . ? C17 C11 C12 Fe1 -58.53(13) . . . . ? C14 Fe1 C12 C13 -38.14(11) . . . . ? C4 Fe1 C12 C13 43.7(2) . . . . ? C5 Fe1 C12 C13 -158.4(2) . . . . ? C17 Fe1 C12 C13 -82.83(12) . . . . ? C11 Fe1 C12 C13 -120.21(16) . . . . ? C1 Fe1 C12 C13 164.89(12) . . . . ? C3 Fe1 C12 C13 80.33(13) . . . . ? C2 Fe1 C12 C13 123.23(12) . . . . ? C14 Fe1 C12 C11 82.07(12) . . . . ? C4 Fe1 C12 C11 163.93(18) . . . . ? C5 Fe1 C12 C11 -38.2(3) . . . . ? C17 Fe1 C12 C11 37.38(11) . . . . ? C13 Fe1 C12 C11 120.21(16) . . . . ? C1 Fe1 C12 C11 -74.90(14) . . . . ? C3 Fe1 C12 C11 -159.46(11) . . . . ? C2 Fe1 C12 C11 -116.56(12) . . . . ? C11 C12 C13 C14 -0.1(2) . . . . ? Fe1 C12 C13 C14 58.40(13) . . . . ? C11 C12 C13 Fe1 -58.48(14) . . . . ? C14 Fe1 C13 C12 119.22(16) . . . . ? C4 Fe1 C13 C12 -161.27(11) . . . . ? C5 Fe1 C13 C12 163.86(18) . . . . ? C17 Fe1 C13 C12 81.25(12) . . . . ? C11 Fe1 C13 C12 37.15(11) . . . . ? C1 Fe1 C13 C12 -44.6(3) . . . . ? C3 Fe1 C13 C12 -118.37(12) . . . . ? C2 Fe1 C13 C12 -77.08(14) . . . . ? C4 Fe1 C13 C14 79.51(13) . . . . ? C5 Fe1 C13 C14 44.6(2) . . . . ? C17 Fe1 C13 C14 -37.97(11) . . . . ? C11 Fe1 C13 C14 -82.07(12) . . . . ? C1 Fe1 C13 C14 -163.8(3) . . . . ? C3 Fe1 C13 C14 122.41(12) . . . . ? C2 Fe1 C13 C14 163.70(12) . . . . ? C12 Fe1 C13 C14 -119.22(16) . . . . ? C12 C13 C14 C15 178.63(17) . . . . ? Fe1 C13 C14 C15 -121.93(19) . . . . ? C12 C13 C14 C17 0.1(2) . . . . ? Fe1 C13 C14 C17 59.56(13) . . . . ? C12 C13 C14 Fe1 -59.43(13) . . . . ? C4 Fe1 C14 C15 -0.42(19) . . . . ? C5 Fe1 C14 C15 -42.7(2) . . . . ? C17 Fe1 C14 C15 -122.6(2) . . . . ? C11 Fe1 C14 C15 -161.09(19) . . . . ? C13 Fe1 C14 C15 117.8(2) . . . . ? C1 Fe1 C14 C15 -73.7(3) . . . . ? C3 Fe1 C14 C15 40.4(2) . . . . ? C2 Fe1 C14 C15 69.0(3) . . . . ? C12 Fe1 C14 C15 155.24(19) . . . . ? C4 Fe1 C14 C13 -118.24(12) . . . . ? C5 Fe1 C14 C13 -160.57(12) . . . . ? C17 Fe1 C14 C13 119.54(16) . . . . ? C11 Fe1 C14 C13 81.08(12) . . . . ? C1 Fe1 C14 C13 168.51(18) . . . . ? C3 Fe1 C14 C13 -77.45(14) . . . . ? C2 Fe1 C14 C13 -48.8(3) . . . . ? C12 Fe1 C14 C13 37.42(12) . . . . ? C4 Fe1 C14 C17 122.22(11) . . . . ? C5 Fe1 C14 C17 79.90(13) . . . . ? C11 Fe1 C14 C17 -38.45(11) . . . . ? C13 Fe1 C14 C17 -119.54(16) . . . . ? C1 Fe1 C14 C17 49.0(2) . . . . ? C3 Fe1 C14 C17 163.01(11) . . . . ? C2 Fe1 C14 C17 -168.4(2) . . . . ? C12 Fe1 C14 C17 -82.12(12) . . . . ? C12 C11 C17 C14 0.1(2) . . . . ? Fe1 C11 C17 C14 -58.99(12) . . . . ? C12 C11 C17 C18 179.95(18) . . . . ? Fe1 C11 C17 C18 120.90(19) . . . . ? C12 C11 C17 Fe1 59.05(13) . . . . ? C15 C14 C17 C11 -178.54(18) . . . . ? C13 C14 C17 C11 -0.1(2) . . . . ? Fe1 C14 C17 C11 59.70(12) . . . . ? C15 C14 C17 C18 1.6(3) . . . . ? C13 C14 C17 C18 180.00(18) . . . . ? Fe1 C14 C17 C18 -120.19(19) . . . . ? C15 C14 C17 Fe1 121.8(2) . . . . ? C13 C14 C17 Fe1 -59.81(13) . . . . ? C14 Fe1 C17 C11 -117.98(16) . . . . ? C4 Fe1 C17 C11 165.66(12) . . . . ? C5 Fe1 C17 C11 124.83(12) . . . . ? C13 Fe1 C17 C11 -80.27(12) . . . . ? C1 Fe1 C17 C11 83.43(14) . . . . ? C3 Fe1 C17 C11 -166.7(2) . . . . ? C2 Fe1 C17 C11 53.6(2) . . . . ? C12 Fe1 C17 C11 -36.94(12) . . . . ? C4 Fe1 C17 C14 -76.36(13) . . . . ? C5 Fe1 C17 C14 -117.18(12) . . . . ? C11 Fe1 C17 C14 117.98(16) . . . . ? C13 Fe1 C17 C14 37.71(11) . . . . ? C1 Fe1 C17 C14 -158.59(11) . . . . ? C3 Fe1 C17 C14 -48.7(3) . . . . ? C2 Fe1 C17 C14 171.56(18) . . . . ? C12 Fe1 C17 C14 81.04(12) . . . . ? C14 Fe1 C17 C18 121.4(2) . . . . ? C4 Fe1 C17 C18 45.1(2) . . . . ? C5 Fe1 C17 C18 4.23(19) . . . . ? C11 Fe1 C17 C18 -120.6(2) . . . . ? C13 Fe1 C17 C18 159.12(18) . . . . ? C1 Fe1 C17 C18 -37.2(2) . . . . ? C3 Fe1 C17 C18 72.7(3) . . . . ? C2 Fe1 C17 C18 -67.0(3) . . . . ? C12 Fe1 C17 C18 -157.54(19) . . . . ? C11 C17 C18 N19 -169.67(19) . . . . ? C14 C17 C18 N19 10.2(3) . . . . ? Fe1 C17 C18 N19 -79.4(2) . . . . ? C11 C17 C18 C23 11.3(3) . . . . ? C14 C17 C18 C23 -168.79(19) . . . . ? Fe1 C17 C18 C23 101.6(2) . . . . ? C23 C18 N19 C20 0.0(3) . . . . ? C17 C18 N19 C20 -179.0(2) . . . . ? C18 N19 C20 C21 0.7(4) . . . . ? N19 C20 C21 C22 -1.1(4) . . . . ? C20 C21 C22 C23 0.7(3) . . . . ? C21 C22 C23 C18 -0.1(3) . . . . ? N19 C18 C23 C22 -0.3(3) . . . . ? C17 C18 C23 C22 178.64(19) . . . . ? C44 Fe2 C31 C35 45.7(3) . . . . ? C33 Fe2 C31 C35 -81.43(14) . . . . ? C43 Fe2 C31 C35 -157.0(2) . . . . ? C47 Fe2 C31 C35 82.06(14) . . . . ? C32 Fe2 C31 C35 -119.08(19) . . . . ? C34 Fe2 C31 C35 -37.58(13) . . . . ? C41 Fe2 C31 C35 125.31(13) . . . . ? C42 Fe2 C31 C35 166.92(12) . . . . ? C44 Fe2 C31 C32 164.73(18) . . . . ? C33 Fe2 C31 C32 37.65(13) . . . . ? C43 Fe2 C31 C32 -38.0(3) . . . . ? C47 Fe2 C31 C32 -158.87(12) . . . . ? C34 Fe2 C31 C32 81.49(14) . . . . ? C35 Fe2 C31 C32 119.08(19) . . . . ? C41 Fe2 C31 C32 -115.62(13) . . . . ? C42 Fe2 C31 C32 -74.00(15) . . . . ? C35 C31 C32 C33 0.1(2) . . . . ? Fe2 C31 C32 C33 -59.08(15) . . . . ? C35 C31 C32 Fe2 59.21(14) . . . . ? C44 Fe2 C32 C33 -39.8(3) . . . . ? C43 Fe2 C32 C33 -73.86(16) . . . . ? C47 Fe2 C32 C33 166.94(18) . . . . ? C34 Fe2 C32 C33 37.99(13) . . . . ? C35 Fe2 C32 C33 81.72(14) . . . . ? C41 Fe2 C32 C33 -157.70(13) . . . . ? C31 Fe2 C32 C33 119.41(19) . . . . ? C42 Fe2 C32 C33 -115.23(14) . . . . ? C44 Fe2 C32 C31 -159.2(2) . . . . ? C33 Fe2 C32 C31 -119.41(19) . . . . ? C43 Fe2 C32 C31 166.73(12) . . . . ? C47 Fe2 C32 C31 47.5(2) . . . . ? C34 Fe2 C32 C31 -81.42(14) . . . . ? C35 Fe2 C32 C31 -37.69(13) . . . . ? C41 Fe2 C32 C31 82.89(14) . . . . ? C42 Fe2 C32 C31 125.35(13) . . . . ? C31 C32 C33 C34 -0.5(2) . . . . ? Fe2 C32 C33 C34 -60.15(14) . . . . ? C31 C32 C33 Fe2 59.61(15) . . . . ? C44 Fe2 C33 C34 -75.26(15) . . . . ? C43 Fe2 C33 C34 -116.97(13) . . . . ? C47 Fe2 C33 C34 -42.6(3) . . . . ? C32 Fe2 C33 C34 118.58(19) . . . . ? C35 Fe2 C33 C34 37.42(13) . . . . ? C41 Fe2 C33 C34 168.55(17) . . . . ? C31 Fe2 C33 C34 81.11(14) . . . . ? C42 Fe2 C33 C34 -158.74(13) . . . . ? C44 Fe2 C33 C32 166.16(12) . . . . ? C43 Fe2 C33 C32 124.45(13) . . . . ? C47 Fe2 C33 C32 -161.1(3) . . . . ? C34 Fe2 C33 C32 -118.58(19) . . . . ? C35 Fe2 C33 C32 -81.16(14) . . . . ? C41 Fe2 C33 C32 50.0(3) . . . . ? C31 Fe2 C33 C32 -37.47(13) . . . . ? C42 Fe2 C33 C32 82.68(15) . . . . ? C32 C33 C34 C35 0.7(2) . . . . ? Fe2 C33 C34 C35 -59.37(14) . . . . ? C32 C33 C34 Fe2 60.11(14) . . . . ? C44 Fe2 C34 C35 -116.93(12) . . . . ? C33 Fe2 C34 C35 119.49(18) . . . . ? C43 Fe2 C34 C35 -160.34(12) . . . . ? C47 Fe2 C34 C35 -74.74(14) . . . . ? C32 Fe2 C34 C35 81.40(14) . . . . ? C41 Fe2 C34 C35 -43.1(3) . . . . ? C31 Fe2 C34 C35 37.62(12) . . . . ? C42 Fe2 C34 C35 166.50(17) . . . . ? C44 Fe2 C34 C33 123.58(13) . . . . ? C43 Fe2 C34 C33 80.17(15) . . . . ? C47 Fe2 C34 C33 165.77(12) . . . . ? C32 Fe2 C34 C33 -38.09(14) . . . . ? C35 Fe2 C34 C33 -119.49(18) . . . . ? C41 Fe2 C34 C33 -162.5(3) . . . . ? C31 Fe2 C34 C33 -81.87(14) . . . . ? C42 Fe2 C34 C33 47.0(2) . . . . ? C33 C34 C35 C31 -0.7(2) . . . . ? Fe2 C34 C35 C31 -59.68(14) . . . . ? C33 C34 C35 Fe2 59.01(14) . . . . ? C32 C31 C35 C34 0.3(2) . . . . ? Fe2 C31 C35 C34 59.45(14) . . . . ? C32 C31 C35 Fe2 -59.12(14) . . . . ? C44 Fe2 C35 C34 80.80(14) . . . . ? C33 Fe2 C35 C34 -37.55(13) . . . . ? C43 Fe2 C35 C34 44.1(2) . . . . ? C47 Fe2 C35 C34 124.69(12) . . . . ? C32 Fe2 C35 C34 -81.53(14) . . . . ? C41 Fe2 C35 C34 166.08(12) . . . . ? C31 Fe2 C35 C34 -119.24(18) . . . . ? C42 Fe2 C35 C34 -159.3(3) . . . . ? C44 Fe2 C35 C31 -159.96(12) . . . . ? C33 Fe2 C35 C31 81.69(14) . . . . ? C43 Fe2 C35 C31 163.39(17) . . . . ? C47 Fe2 C35 C31 -116.07(13) . . . . ? C32 Fe2 C35 C31 37.71(13) . . . . ? C34 Fe2 C35 C31 119.24(18) . . . . ? C41 Fe2 C35 C31 -74.68(15) . . . . ? C42 Fe2 C35 C31 -40.0(3) . . . . ? C44 Fe2 C41 C42 -81.48(12) . . . . ? C33 Fe2 C41 C42 46.2(2) . . . . ? C43 Fe2 C41 C42 -36.85(11) . . . . ? C47 Fe2 C41 C42 -120.31(16) . . . . ? C32 Fe2 C41 C42 81.60(14) . . . . ? C34 Fe2 C41 C42 -160.9(3) . . . . ? C35 Fe2 C41 C42 165.61(12) . . . . ? C31 Fe2 C41 C42 124.35(12) . . . . ? C44 Fe2 C41 C47 38.83(11) . . . . ? C33 Fe2 C41 C47 166.54(18) . . . . ? C43 Fe2 C41 C47 83.46(12) . . . . ? C32 Fe2 C41 C47 -158.09(12) . . . . ? C34 Fe2 C41 C47 -40.6(3) . . . . ? C35 Fe2 C41 C47 -74.08(14) . . . . ? C31 Fe2 C41 C47 -115.34(12) . . . . ? C42 Fe2 C41 C47 120.31(16) . . . . ? C47 C41 C42 C43 -0.3(2) . . . . ? Fe2 C41 C42 C43 58.13(14) . . . . ? C47 C41 C42 Fe2 -58.47(13) . . . . ? C44 Fe2 C42 C43 -38.46(11) . . . . ? C33 Fe2 C42 C43 80.23(14) . . . . ? C47 Fe2 C42 C43 -83.30(12) . . . . ? C32 Fe2 C42 C43 122.93(12) . . . . ? C34 Fe2 C42 C43 47.1(2) . . . . ? C35 Fe2 C42 C43 -165.1(3) . . . . ? C41 Fe2 C42 C43 -120.56(16) . . . . ? C31 Fe2 C42 C43 163.82(12) . . . . ? C44 Fe2 C42 C41 82.10(12) . . . . ? C33 Fe2 C42 C41 -159.21(12) . . . . ? C43 Fe2 C42 C41 120.56(16) . . . . ? C47 Fe2 C42 C41 37.26(11) . . . . ? C32 Fe2 C42 C41 -116.51(13) . . . . ? C34 Fe2 C42 C41 167.62(17) . . . . ? C35 Fe2 C42 C41 -44.5(3) . . . . ? C31 Fe2 C42 C41 -75.62(14) . . . . ? C41 C42 C43 C44 0.4(2) . . . . ? Fe2 C42 C43 C44 58.83(13) . . . . ? C41 C42 C43 Fe2 -58.39(14) . . . . ? C44 Fe2 C43 C42 118.92(16) . . . . ? C33 Fe2 C43 C42 -116.83(12) . . . . ? C47 Fe2 C43 C42 80.78(12) . . . . ? C32 Fe2 C43 C42 -76.12(14) . . . . ? C34 Fe2 C43 C42 -158.70(12) . . . . ? C35 Fe2 C43 C42 169.97(18) . . . . ? C41 Fe2 C43 C42 36.95(11) . . . . ? C31 Fe2 C43 C42 -47.1(3) . . . . ? C33 Fe2 C43 C44 124.25(12) . . . . ? C47 Fe2 C43 C44 -38.14(11) . . . . ? C32 Fe2 C43 C44 164.95(12) . . . . ? C34 Fe2 C43 C44 82.38(13) . . . . ? C35 Fe2 C43 C44 51.0(2) . . . . ? C41 Fe2 C43 C44 -81.97(12) . . . . ? C31 Fe2 C43 C44 -166.1(2) . . . . ? C42 Fe2 C43 C44 -118.92(16) . . . . ? C42 C43 C44 C45 -179.67(17) . . . . ? Fe2 C43 C44 C45 -119.74(18) . . . . ? C42 C43 C44 C47 -0.4(2) . . . . ? Fe2 C43 C44 C47 59.57(13) . . . . ? C42 C43 C44 Fe2 -59.93(14) . . . . ? C33 Fe2 C44 C45 41.2(2) . . . . ? C43 Fe2 C44 C45 115.7(2) . . . . ? C47 Fe2 C44 C45 -125.0(2) . . . . ? C32 Fe2 C44 C45 71.6(3) . . . . ? C34 Fe2 C44 C45 0.00(18) . . . . ? C35 Fe2 C44 C45 -42.05(19) . . . . ? C41 Fe2 C44 C45 -163.08(18) . . . . ? C31 Fe2 C44 C45 -74.6(3) . . . . ? C42 Fe2 C44 C45 153.28(18) . . . . ? C33 Fe2 C44 C43 -74.58(14) . . . . ? C47 Fe2 C44 C43 119.28(16) . . . . ? C32 Fe2 C44 C43 -44.1(3) . . . . ? C34 Fe2 C44 C43 -115.75(12) . . . . ? C35 Fe2 C44 C43 -157.80(12) . . . . ? C41 Fe2 C44 C43 81.17(12) . . . . ? C31 Fe2 C44 C43 169.68(18) . . . . ? C42 Fe2 C44 C43 37.53(11) . . . . ? C33 Fe2 C44 C47 166.13(12) . . . . ? C43 Fe2 C44 C47 -119.28(16) . . . . ? C32 Fe2 C44 C47 -163.4(2) . . . . ? C34 Fe2 C44 C47 124.97(12) . . . . ? C35 Fe2 C44 C47 82.92(13) . . . . ? C41 Fe2 C44 C47 -38.11(11) . . . . ? C31 Fe2 C44 C47 50.4(2) . . . . ? C42 Fe2 C44 C47 -81.75(12) . . . . ? C42 C41 C47 C44 0.1(2) . . . . ? Fe2 C41 C47 C44 -58.76(12) . . . . ? C42 C41 C47 C48 -178.78(17) . . . . ? Fe2 C41 C47 C48 122.34(19) . . . . ? C42 C41 C47 Fe2 58.87(14) . . . . ? C45 C44 C47 C41 179.39(19) . . . . ? C43 C44 C47 C41 0.2(2) . . . . ? Fe2 C44 C47 C41 59.68(13) . . . . ? C45 C44 C47 C48 -1.7(3) . . . . ? C43 C44 C47 C48 179.04(17) . . . . ? Fe2 C44 C47 C48 -121.43(19) . . . . ? C45 C44 C47 Fe2 119.7(2) . . . . ? C43 C44 C47 Fe2 -59.53(12) . . . . ? C44 Fe2 C47 C41 -118.31(16) . . . . ? C33 Fe2 C47 C41 -160.3(3) . . . . ? C43 Fe2 C47 C41 -80.33(12) . . . . ? C32 Fe2 C47 C41 49.7(2) . . . . ? C34 Fe2 C47 C41 166.88(12) . . . . ? C35 Fe2 C47 C41 125.80(12) . . . . ? C31 Fe2 C47 C41 83.35(13) . . . . ? C42 Fe2 C47 C41 -37.00(11) . . . . ? C33 Fe2 C47 C44 -42.0(3) . . . . ? C43 Fe2 C47 C44 37.98(11) . . . . ? C32 Fe2 C47 C44 167.98(18) . . . . ? C34 Fe2 C47 C44 -74.81(14) . . . . ? C35 Fe2 C47 C44 -115.88(12) . . . . ? C41 Fe2 C47 C44 118.31(16) . . . . ? C31 Fe2 C47 C44 -158.34(11) . . . . ? C42 Fe2 C47 C44 81.32(12) . . . . ? C44 Fe2 C47 C48 120.9(2) . . . . ? C33 Fe2 C47 C48 78.9(3) . . . . ? C43 Fe2 C47 C48 158.84(19) . . . . ? C32 Fe2 C47 C48 -71.2(3) . . . . ? C34 Fe2 C47 C48 46.1(2) . . . . ? C35 Fe2 C47 C48 4.98(19) . . . . ? C41 Fe2 C47 C48 -120.8(2) . . . . ? C31 Fe2 C47 C48 -37.5(2) . . . . ? C42 Fe2 C47 C48 -157.82(19) . . . . ? C41 C47 C48 N49 174.88(18) . . . . ? C44 C47 C48 N49 -3.8(3) . . . . ? Fe2 C47 C48 N49 -93.7(2) . . . . ? C41 C47 C48 C53 -3.4(3) . . . . ? C44 C47 C48 C53 177.91(18) . . . . ? Fe2 C47 C48 C53 88.0(2) . . . . ? C53 C48 N49 C50 -0.2(3) . . . . ? C47 C48 N49 C50 -178.50(19) . . . . ? C48 N49 C50 C51 0.2(4) . . . . ? N49 C50 C51 C52 -0.4(4) . . . . ? C50 C51 C52 C53 0.5(3) . . . . ? C51 C52 C53 C48 -0.5(3) . . . . ? N49 C48 C53 C52 0.4(3) . . . . ? C47 C48 C53 C52 178.54(19) . . . . ? data_20a _database_code_depnum_ccdc_archive 'CCDC 755180' #TrackingRef 'CIF_Mongin.cif' _audit_creation_date 2009-10-20T09:07:45-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C10 H8 Br Fe I, C10 H8 Br Fe I' _chemical_formula_sum 'C20 H16 Br2 Fe2 I2' _chemical_formula_weight 781.65 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8917(4) _cell_length_b 10.0527(5) _cell_length_c 10.8535(5) _cell_angle_alpha 81.390(2) _cell_angle_beta 82.628(2) _cell_angle_gamma 84.345(2) _cell_volume 1054.80(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9204 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 27.52 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.17 _exptl_crystal_density_diffrn 2.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 8.093 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.109 _exptl_absorpt_correction_T_max 0.253 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_unetI/netI 0.0422 _diffrn_reflns_number 15292 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.98 _diffrn_measured_fraction_theta_max 0.98 _reflns_number_total 4746 _reflns_number_gt 4184 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SAINT (Bruker, 2002)' _computing_cell_refinement 'Bruker SMART (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT (Bruker, 2002)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0466P)^2^+6.9479P] 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_number_reflns 4746 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.051 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1217 _refine_ls_wR_factor_gt 0.1182 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.002 _refine_diff_density_max 4.35 _refine_diff_density_min -1.548 _refine_diff_density_rms 0.18 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.60823(9) -0.25949(9) 0.21036(8) 0.0272(2) Uani 1 1 d . . . C1 C 0.4489(7) -0.3212(7) 0.3345(6) 0.0282(13) Uani 1 1 d . . . I1 I 0.29397(4) -0.43306(5) 0.30944(4) 0.03490(13) Uani 1 1 d . . . C2 C 0.4503(7) -0.1790(7) 0.3168(6) 0.0309(13) Uani 1 1 d . . . Br2 Br 0.30518(8) -0.05335(7) 0.26533(7) 0.04030(19) Uani 1 1 d . . . C3 C 0.5718(8) -0.1440(8) 0.3533(6) 0.0374(16) Uani 1 1 d . . . H3 H 0.597 -0.055 0.3524 0.045 Uiso 1 1 calc R . . C4 C 0.6502(8) -0.2658(8) 0.3917(6) 0.0393(16) Uani 1 1 d . . . H4 H 0.7385 -0.2725 0.4189 0.047 Uiso 1 1 calc R . . C5 C 0.5744(7) -0.3754(7) 0.3824(6) 0.0334(14) Uani 1 1 d . . . H5 H 0.6018 -0.4684 0.4041 0.04 Uiso 1 1 calc R . . C6 C 0.5955(7) -0.3325(7) 0.0477(6) 0.0319(14) Uani 1 1 d . . . H6 H 0.5273 -0.3875 0.0347 0.038 Uiso 1 1 calc R . . C7 C 0.5886(7) -0.1899(7) 0.0247(6) 0.0314(14) Uani 1 1 d . . . H7 H 0.5159 -0.1325 -0.0085 0.038 Uiso 1 1 calc R . . C8 C 0.7077(8) -0.1478(8) 0.0595(7) 0.0421(17) Uani 1 1 d . . . H8 H 0.7292 -0.0571 0.0557 0.05 Uiso 1 1 calc R . . C9 C 0.7912(8) -0.2667(9) 0.1019(7) 0.0455(19) Uani 1 1 d . . . H9 H 0.8782 -0.2686 0.1306 0.055 Uiso 1 1 calc R . . C10 C 0.7220(8) -0.3792(8) 0.0936(7) 0.0411(17) Uani 1 1 d . . . H10 H 0.7543 -0.4709 0.1149 0.049 Uiso 1 1 calc R . . Fe2 Fe 0.95503(9) -0.78382(9) 0.29004(8) 0.02429(19) Uani 1 1 d . . . C21 C 0.8489(7) -0.8449(6) 0.1635(6) 0.0278(13) Uani 1 1 d . . . I21 I 0.81194(5) -0.75350(6) -0.00509(5) 0.03405(14) Uani 0.5 1 d P . . Br21 Br 0.81194(5) -0.75350(6) -0.00509(5) 0.03405(14) Uani 0.5 1 d P . . C22 C 0.7618(7) -0.8306(7) 0.2773(6) 0.0305(13) Uani 1 1 d . . . Br22 Br 0.58223(6) -0.72409(6) 0.29180(6) 0.04376(17) Uani 0.5 1 d P . . I22 I 0.58223(6) -0.72409(6) 0.29180(6) 0.04376(17) Uani 0.5 1 d P . . C23 C 0.8197(8) -0.9193(8) 0.3766(7) 0.0423(18) Uani 1 1 d . . . H23 H 0.784 -0.9294 0.4627 0.051 Uiso 1 1 calc R . . C24 C 0.9393(8) -0.9891(7) 0.3238(8) 0.0432(18) Uani 1 1 d . . . H24 H 0.9973 -1.0552 0.3682 0.052 Uiso 1 1 calc R . . C25 C 0.9576(7) -0.9433(7) 0.1935(7) 0.0346(15) Uani 1 1 d . . . H25 H 1.0303 -0.9734 0.1356 0.042 Uiso 1 1 calc R . . C26 C 1.0304(7) -0.6041(7) 0.2113(6) 0.0339(14) Uani 1 1 d . . . H26 H 1.0152 -0.5572 0.131 0.041 Uiso 1 1 calc R . . C27 C 0.9475(7) -0.5878(7) 0.3263(7) 0.0362(15) Uani 1 1 d . . . H27 H 0.8678 -0.5277 0.3364 0.043 Uiso 1 1 calc R . . C28 C 1.0053(7) -0.6769(8) 0.4224(7) 0.0360(15) Uani 1 1 d . . . H28 H 0.9711 -0.6872 0.5089 0.043 Uiso 1 1 calc R . . C29 C 1.1232(7) -0.7486(7) 0.3679(6) 0.0320(14) Uani 1 1 d . . . H29 H 1.181 -0.8156 0.4114 0.038 Uiso 1 1 calc R . . C30 C 1.1395(7) -0.7028(7) 0.2376(6) 0.0305(14) Uani 1 1 d . . . H30 H 1.2109 -0.7327 0.1783 0.037 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 0.0304(5) 0.0286(5) 0.0246(4) -0.0051(3) 0.0001(3) -0.0153(4) C1 0.035(3) 0.031(3) 0.020(3) -0.008(2) 0.003(2) -0.010(3) I1 0.0321(2) 0.0371(3) 0.0367(2) -0.00053(18) -0.00267(17) -0.01727(18) C2 0.037(3) 0.025(3) 0.031(3) -0.006(3) 0.000(3) -0.006(3) Br2 0.0463(4) 0.0329(4) 0.0398(4) -0.0056(3) -0.0049(3) 0.0073(3) C3 0.049(4) 0.037(4) 0.032(3) -0.012(3) -0.005(3) -0.020(3) C4 0.042(4) 0.051(4) 0.030(3) -0.009(3) -0.010(3) -0.018(3) C5 0.035(3) 0.037(4) 0.028(3) -0.004(3) -0.003(3) -0.008(3) C6 0.035(3) 0.037(4) 0.026(3) -0.010(3) 0.002(3) -0.012(3) C7 0.037(3) 0.034(3) 0.020(3) -0.002(2) 0.003(2) -0.001(3) C8 0.053(4) 0.038(4) 0.035(4) -0.004(3) 0.010(3) -0.025(3) C9 0.028(3) 0.069(5) 0.038(4) 0.001(4) 0.004(3) -0.019(3) C10 0.045(4) 0.041(4) 0.034(4) -0.004(3) 0.008(3) 0.000(3) Fe2 0.0267(4) 0.0244(4) 0.0237(4) -0.0015(3) -0.0047(3) -0.0122(3) C21 0.032(3) 0.024(3) 0.030(3) -0.006(2) -0.005(2) -0.013(2) I21 0.0328(3) 0.0439(3) 0.0283(3) -0.0095(2) -0.0050(2) -0.0084(2) Br21 0.0328(3) 0.0439(3) 0.0283(3) -0.0095(2) -0.0050(2) -0.0084(2) C22 0.028(3) 0.031(3) 0.033(3) -0.001(3) -0.001(2) -0.013(3) Br22 0.0397(3) 0.0438(3) 0.0466(3) -0.0109(3) 0.0084(2) -0.0078(2) I22 0.0397(3) 0.0438(3) 0.0466(3) -0.0109(3) 0.0084(2) -0.0078(2) C23 0.047(4) 0.045(4) 0.037(4) 0.011(3) -0.014(3) -0.027(3) C24 0.046(4) 0.023(3) 0.061(5) 0.013(3) -0.023(4) -0.015(3) C25 0.033(3) 0.026(3) 0.050(4) -0.010(3) -0.015(3) -0.008(3) C26 0.042(4) 0.030(3) 0.033(3) -0.002(3) -0.008(3) -0.016(3) C27 0.031(3) 0.031(4) 0.050(4) -0.013(3) -0.007(3) -0.005(3) C28 0.038(4) 0.045(4) 0.030(3) -0.016(3) -0.002(3) -0.015(3) C29 0.036(3) 0.030(3) 0.034(3) -0.008(3) -0.010(3) -0.010(3) C30 0.029(3) 0.035(3) 0.032(3) -0.014(3) 0.002(2) -0.015(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C2 2.000(7) . ? Fe1 C1 2.020(6) . ? Fe1 C9 2.029(7) . ? Fe1 C6 2.033(6) . ? Fe1 C10 2.036(7) . ? Fe1 C8 2.041(7) . ? Fe1 C3 2.049(7) . ? Fe1 C4 2.053(7) . ? Fe1 C5 2.055(7) . ? Fe1 C7 2.059(6) . ? C1 C2 1.415(9) . ? C1 C5 1.434(10) . ? C1 I1 2.055(6) . ? C2 C3 1.405(10) . ? C2 Br2 1.898(7) . ? C3 C4 1.420(11) . ? C3 H3 0.95 . ? C4 C5 1.415(10) . ? C4 H4 0.95 . ? C5 H5 0.95 . ? C6 C7 1.415(10) . ? C6 C10 1.417(11) . ? C6 H6 0.95 . ? C7 C8 1.404(10) . ? C7 H7 0.95 . ? C8 C9 1.436(12) . ? C8 H8 0.95 . ? C9 C10 1.398(11) . ? C9 H9 0.95 . ? C10 H10 0.95 . ? Fe2 C21 2.028(6) . ? Fe2 C25 2.039(7) . ? Fe2 C22 2.039(6) . ? Fe2 C29 2.043(6) . ? Fe2 C23 2.045(7) . ? Fe2 C26 2.046(7) . ? Fe2 C30 2.051(6) . ? Fe2 C28 2.053(7) . ? Fe2 C24 2.059(7) . ? Fe2 C27 2.059(7) . ? C21 C25 1.423(10) . ? C21 C22 1.430(9) . ? C21 I21 1.982(6) . ? C22 C23 1.433(10) . ? C22 Br22 1.982(7) . ? C23 C24 1.416(12) . ? C23 H23 0.95 . ? C24 C25 1.414(11) . ? C24 H24 0.95 . ? C25 H25 0.95 . ? C26 C30 1.419(10) . ? C26 C27 1.424(10) . ? C26 H26 0.95 . ? C27 C28 1.410(11) . ? C27 H27 0.95 . ? C28 C29 1.419(10) . ? C28 H28 0.95 . ? C29 C30 1.413(9) . ? C29 H29 0.95 . ? C30 H30 0.95 . ? 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 C2 Fe1 C1 41.2(3) . . ? C2 Fe1 C9 157.2(3) . . ? C1 Fe1 C9 159.7(3) . . ? C2 Fe1 C6 125.1(3) . . ? C1 Fe1 C6 107.7(3) . . ? C9 Fe1 C6 68.2(3) . . ? C2 Fe1 C10 161.6(3) . . ? C1 Fe1 C10 123.8(3) . . ? C9 Fe1 C10 40.2(3) . . ? C6 Fe1 C10 40.8(3) . . ? C2 Fe1 C8 121.7(3) . . ? C1 Fe1 C8 157.5(3) . . ? C9 Fe1 C8 41.3(3) . . ? C6 Fe1 C8 68.2(3) . . ? C10 Fe1 C8 68.5(3) . . ? C2 Fe1 C3 40.6(3) . . ? C1 Fe1 C3 68.9(3) . . ? C9 Fe1 C3 121.3(3) . . ? C6 Fe1 C3 161.7(3) . . ? C10 Fe1 C3 156.1(3) . . ? C8 Fe1 C3 107.7(3) . . ? C2 Fe1 C4 68.4(3) . . ? C1 Fe1 C4 68.8(3) . . ? C9 Fe1 C4 106.6(3) . . ? C6 Fe1 C4 156.7(3) . . ? C10 Fe1 C4 120.7(3) . . ? C8 Fe1 C4 123.9(3) . . ? C3 Fe1 C4 40.5(3) . . ? C2 Fe1 C5 68.7(3) . . ? C1 Fe1 C5 41.2(3) . . ? C9 Fe1 C5 122.7(3) . . ? C6 Fe1 C5 122.0(3) . . ? C10 Fe1 C5 107.0(3) . . ? C8 Fe1 C5 160.0(3) . . ? C3 Fe1 C5 68.1(3) . . ? C4 Fe1 C5 40.3(3) . . ? C2 Fe1 C7 108.8(3) . . ? C1 Fe1 C7 122.5(3) . . ? C9 Fe1 C7 68.1(3) . . ? C6 Fe1 C7 40.4(3) . . ? C10 Fe1 C7 68.1(3) . . ? C8 Fe1 C7 40.0(3) . . ? C3 Fe1 C7 125.1(3) . . ? C4 Fe1 C7 160.8(3) . . ? C5 Fe1 C7 158.2(3) . . ? C2 C1 C5 106.9(6) . . ? C2 C1 Fe1 68.6(4) . . ? C5 C1 Fe1 70.7(4) . . ? C2 C1 I1 127.8(5) . . ? C5 C1 I1 125.2(5) . . ? Fe1 C1 I1 128.8(3) . . ? C3 C2 C1 109.4(6) . . ? C3 C2 Br2 124.7(5) . . ? C1 C2 Br2 125.8(5) . . ? C3 C2 Fe1 71.6(4) . . ? C1 C2 Fe1 70.2(4) . . ? Br2 C2 Fe1 128.4(4) . . ? C2 C3 C4 107.5(6) . . ? C2 C3 Fe1 67.8(4) . . ? C4 C3 Fe1 69.9(4) . . ? C2 C3 H3 126.2 . . ? C4 C3 H3 126.2 . . ? Fe1 C3 H3 127.6 . . ? C5 C4 C3 108.4(6) . . ? C5 C4 Fe1 69.9(4) . . ? C3 C4 Fe1 69.6(4) . . ? C5 C4 H4 125.8 . . ? C3 C4 H4 125.8 . . ? Fe1 C4 H4 126.2 . . ? C4 C5 C1 107.8(6) . . ? C4 C5 Fe1 69.8(4) . . ? C1 C5 Fe1 68.1(4) . . ? C4 C5 H5 126.1 . . ? C1 C5 H5 126.1 . . ? Fe1 C5 H5 127.6 . . ? C7 C6 C10 108.1(6) . . ? C7 C6 Fe1 70.7(4) . . ? C10 C6 Fe1 69.7(4) . . ? C7 C6 H6 125.9 . . ? C10 C6 H6 125.9 . . ? Fe1 C6 H6 125.2 . . ? C8 C7 C6 108.2(6) . . ? C8 C7 Fe1 69.3(4) . . ? C6 C7 Fe1 68.8(4) . . ? C8 C7 H7 125.9 . . ? C6 C7 H7 125.9 . . ? Fe1 C7 H7 127.6 . . ? C7 C8 C9 107.5(6) . . ? C7 C8 Fe1 70.7(4) . . ? C9 C8 Fe1 68.9(4) . . ? C7 C8 H8 126.2 . . ? C9 C8 H8 126.2 . . ? Fe1 C8 H8 125.7 . . ? C10 C9 C8 108.1(7) . . ? C10 C9 Fe1 70.2(4) . . ? C8 C9 Fe1 69.8(4) . . ? C10 C9 H9 126 . . ? C8 C9 H9 126 . . ? Fe1 C9 H9 125.7 . . ? C9 C10 C6 108.1(7) . . ? C9 C10 Fe1 69.6(4) . . ? C6 C10 Fe1 69.5(4) . . ? C9 C10 H10 126 . . ? C6 C10 H10 126 . . ? Fe1 C10 H10 126.5 . . ? C21 Fe2 C25 40.9(3) . . ? C21 Fe2 C22 41.2(3) . . ? C25 Fe2 C22 68.6(3) . . ? C21 Fe2 C29 157.2(3) . . ? C25 Fe2 C29 121.1(3) . . ? C22 Fe2 C29 159.8(3) . . ? C21 Fe2 C23 69.2(3) . . ? C25 Fe2 C23 68.3(3) . . ? C22 Fe2 C23 41.1(3) . . ? C29 Fe2 C23 122.6(3) . . ? C21 Fe2 C26 107.7(3) . . ? C25 Fe2 C26 123.1(3) . . ? C22 Fe2 C26 123.6(3) . . ? C29 Fe2 C26 68.1(3) . . ? C23 Fe2 C26 160.0(3) . . ? C21 Fe2 C30 121.8(3) . . ? C25 Fe2 C30 106.5(3) . . ? C22 Fe2 C30 158.9(3) . . ? C29 Fe2 C30 40.4(3) . . ? C23 Fe2 C30 158.1(3) . . ? C26 Fe2 C30 40.5(3) . . ? C21 Fe2 C28 160.6(3) . . ? C25 Fe2 C28 157.5(3) . . ? C22 Fe2 C28 124.4(3) . . ? C29 Fe2 C28 40.5(3) . . ? C23 Fe2 C28 108.3(3) . . ? C26 Fe2 C28 67.8(3) . . ? C30 Fe2 C28 67.9(3) . . ? C21 Fe2 C24 68.7(3) . . ? C25 Fe2 C24 40.4(3) . . ? C22 Fe2 C24 68.4(3) . . ? C29 Fe2 C24 106.6(3) . . ? C23 Fe2 C24 40.4(3) . . ? C26 Fe2 C24 158.5(3) . . ? C30 Fe2 C24 122.0(3) . . ? C28 Fe2 C24 122.6(3) . . ? C21 Fe2 C27 124.3(3) . . ? C25 Fe2 C27 160.2(3) . . ? C22 Fe2 C27 109.0(3) . . ? C29 Fe2 C27 68.0(3) . . ? C23 Fe2 C27 123.8(3) . . ? C26 Fe2 C27 40.6(3) . . ? C30 Fe2 C27 68.1(3) . . ? C28 Fe2 C27 40.1(3) . . ? C24 Fe2 C27 158.7(3) . . ? C25 C21 C22 107.4(6) . . ? C25 C21 I21 127.5(5) . . ? C22 C21 I21 124.9(5) . . ? C25 C21 Fe2 69.9(4) . . ? C22 C21 Fe2 69.8(4) . . ? I21 C21 Fe2 129.4(3) . . ? C21 C22 C23 107.7(6) . . ? C21 C22 Br22 126.0(5) . . ? C23 C22 Br22 125.9(5) . . ? C21 C22 Fe2 69.0(3) . . ? C23 C22 Fe2 69.7(4) . . ? Br22 C22 Fe2 132.1(3) . . ? C24 C23 C22 108.0(7) . . ? C24 C23 Fe2 70.3(4) . . ? C22 C23 Fe2 69.2(4) . . ? C24 C23 H23 126 . . ? C22 C23 H23 126 . . ? Fe2 C23 H23 126 . . ? C23 C24 C25 108.1(6) . . ? C23 C24 Fe2 69.3(4) . . ? C25 C24 Fe2 69.1(4) . . ? C23 C24 H24 125.9 . . ? C25 C24 H24 125.9 . . ? Fe2 C24 H24 127.3 . . ? C24 C25 C21 108.7(7) . . ? C24 C25 Fe2 70.6(4) . . ? C21 C25 Fe2 69.1(4) . . ? C24 C25 H25 125.6 . . ? C21 C25 H25 125.6 . . ? Fe2 C25 H25 126.3 . . ? C30 C26 C27 108.2(6) . . ? C30 C26 Fe2 69.9(4) . . ? C27 C26 Fe2 70.2(4) . . ? C30 C26 H26 125.9 . . ? C27 C26 H26 125.9 . . ? Fe2 C26 H26 125.6 . . ? C28 C27 C26 107.6(6) . . ? C28 C27 Fe2 69.7(4) . . ? C26 C27 Fe2 69.2(4) . . ? C28 C27 H27 126.2 . . ? C26 C27 H27 126.2 . . ? Fe2 C27 H27 126.4 . . ? C27 C28 C29 108.4(6) . . ? C27 C28 Fe2 70.2(4) . . ? C29 C28 Fe2 69.3(4) . . ? C27 C28 H28 125.8 . . ? C29 C28 H28 125.8 . . ? Fe2 C28 H28 126.3 . . ? C30 C29 C28 108.1(6) . . ? C30 C29 Fe2 70.1(4) . . ? C28 C29 Fe2 70.1(4) . . ? C30 C29 H29 126 . . ? C28 C29 H29 126 . . ? Fe2 C29 H29 125.4 . . ? C29 C30 C26 107.8(6) . . ? C29 C30 Fe2 69.5(4) . . ? C26 C30 Fe2 69.6(4) . . ? C29 C30 H30 126.1 . . ? C26 C30 H30 126.1 . . ? Fe2 C30 H30 126.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 Fe1 C1 C2 161.5(8) . . . . ? C6 Fe1 C1 C2 -123.5(4) . . . . ? C10 Fe1 C1 C2 -165.5(4) . . . . ? C8 Fe1 C1 C2 -47.9(9) . . . . ? C3 Fe1 C1 C2 37.4(4) . . . . ? C4 Fe1 C1 C2 81.0(4) . . . . ? C5 Fe1 C1 C2 117.9(5) . . . . ? C7 Fe1 C1 C2 -81.6(4) . . . . ? C2 Fe1 C1 C5 -117.9(5) . . . . ? C9 Fe1 C1 C5 43.6(10) . . . . ? C6 Fe1 C1 C5 118.6(4) . . . . ? C10 Fe1 C1 C5 76.6(5) . . . . ? C8 Fe1 C1 C5 -165.8(7) . . . . ? C3 Fe1 C1 C5 -80.5(4) . . . . ? C4 Fe1 C1 C5 -36.9(4) . . . . ? C7 Fe1 C1 C5 160.5(4) . . . . ? C2 Fe1 C1 I1 122.0(6) . . . . ? C9 Fe1 C1 I1 -76.5(10) . . . . ? C6 Fe1 C1 I1 -1.5(5) . . . . ? C10 Fe1 C1 I1 -43.5(6) . . . . ? C8 Fe1 C1 I1 74.1(9) . . . . ? C3 Fe1 C1 I1 159.4(5) . . . . ? C4 Fe1 C1 I1 -157.0(5) . . . . ? C5 Fe1 C1 I1 -120.1(6) . . . . ? C7 Fe1 C1 I1 40.4(6) . . . . ? C5 C1 C2 C3 -0.5(7) . . . . ? Fe1 C1 C2 C3 -61.1(5) . . . . ? I1 C1 C2 C3 175.6(5) . . . . ? C5 C1 C2 Br2 -175.7(5) . . . . ? Fe1 C1 C2 Br2 123.7(5) . . . . ? I1 C1 C2 Br2 0.4(8) . . . . ? C5 C1 C2 Fe1 60.7(4) . . . . ? I1 C1 C2 Fe1 -123.3(5) . . . . ? C1 Fe1 C2 C3 119.5(6) . . . . ? C9 Fe1 C2 C3 -44.0(9) . . . . ? C6 Fe1 C2 C3 -164.3(4) . . . . ? C10 Fe1 C2 C3 160.6(9) . . . . ? C8 Fe1 C2 C3 -80.1(5) . . . . ? C4 Fe1 C2 C3 37.4(4) . . . . ? C5 Fe1 C2 C3 80.8(4) . . . . ? C7 Fe1 C2 C3 -122.3(4) . . . . ? C9 Fe1 C2 C1 -163.5(7) . . . . ? C6 Fe1 C2 C1 76.2(5) . . . . ? C10 Fe1 C2 C1 41.1(11) . . . . ? C8 Fe1 C2 C1 160.5(4) . . . . ? C3 Fe1 C2 C1 -119.5(6) . . . . ? C4 Fe1 C2 C1 -82.1(4) . . . . ? C5 Fe1 C2 C1 -38.7(4) . . . . ? C7 Fe1 C2 C1 118.2(4) . . . . ? C1 Fe1 C2 Br2 -120.5(6) . . . . ? C9 Fe1 C2 Br2 76.0(9) . . . . ? C6 Fe1 C2 Br2 -44.3(6) . . . . ? C10 Fe1 C2 Br2 -79.3(10) . . . . ? C8 Fe1 C2 Br2 40.0(6) . . . . ? C3 Fe1 C2 Br2 120.1(6) . . . . ? C4 Fe1 C2 Br2 157.4(5) . . . . ? C5 Fe1 C2 Br2 -159.1(5) . . . . ? C7 Fe1 C2 Br2 -2.3(5) . . . . ? C1 C2 C3 C4 1.4(8) . . . . ? Br2 C2 C3 C4 176.7(5) . . . . ? Fe1 C2 C3 C4 -58.8(5) . . . . ? C1 C2 C3 Fe1 60.3(5) . . . . ? Br2 C2 C3 Fe1 -124.5(5) . . . . ? C1 Fe1 C3 C2 -38.0(4) . . . . ? C9 Fe1 C3 C2 161.6(4) . . . . ? C6 Fe1 C3 C2 44.7(10) . . . . ? C10 Fe1 C3 C2 -165.0(7) . . . . ? C8 Fe1 C3 C2 118.4(4) . . . . ? C4 Fe1 C3 C2 -119.7(6) . . . . ? C5 Fe1 C3 C2 -82.4(4) . . . . ? C7 Fe1 C3 C2 77.7(5) . . . . ? C2 Fe1 C3 C4 119.7(6) . . . . ? C1 Fe1 C3 C4 81.7(4) . . . . ? C9 Fe1 C3 C4 -78.7(5) . . . . ? C6 Fe1 C3 C4 164.4(8) . . . . ? C10 Fe1 C3 C4 -45.3(9) . . . . ? C8 Fe1 C3 C4 -121.9(5) . . . . ? C5 Fe1 C3 C4 37.3(4) . . . . ? C7 Fe1 C3 C4 -162.6(4) . . . . ? C2 C3 C4 C5 -1.8(8) . . . . ? Fe1 C3 C4 C5 -59.4(5) . . . . ? C2 C3 C4 Fe1 57.5(5) . . . . ? C2 Fe1 C4 C5 82.2(5) . . . . ? C1 Fe1 C4 C5 37.7(4) . . . . ? C9 Fe1 C4 C5 -121.4(5) . . . . ? C6 Fe1 C4 C5 -48.1(9) . . . . ? C10 Fe1 C4 C5 -80.0(5) . . . . ? C8 Fe1 C4 C5 -163.3(4) . . . . ? C3 Fe1 C4 C5 119.6(6) . . . . ? C7 Fe1 C4 C5 167.6(8) . . . . ? C2 Fe1 C4 C3 -37.4(4) . . . . ? C1 Fe1 C4 C3 -81.8(4) . . . . ? C9 Fe1 C4 C3 119.0(5) . . . . ? C6 Fe1 C4 C3 -167.6(6) . . . . ? C10 Fe1 C4 C3 160.5(4) . . . . ? C8 Fe1 C4 C3 77.1(5) . . . . ? C5 Fe1 C4 C3 -119.6(6) . . . . ? C7 Fe1 C4 C3 48.0(10) . . . . ? C3 C4 C5 C1 1.6(8) . . . . ? Fe1 C4 C5 C1 -57.6(4) . . . . ? C3 C4 C5 Fe1 59.2(5) . . . . ? C2 C1 C5 C4 -0.7(7) . . . . ? Fe1 C1 C5 C4 58.7(5) . . . . ? I1 C1 C5 C4 -176.9(5) . . . . ? C2 C1 C5 Fe1 -59.3(4) . . . . ? I1 C1 C5 Fe1 124.5(5) . . . . ? C2 Fe1 C5 C4 -81.3(5) . . . . ? C1 Fe1 C5 C4 -119.9(6) . . . . ? C9 Fe1 C5 C4 76.5(6) . . . . ? C6 Fe1 C5 C4 159.7(4) . . . . ? C10 Fe1 C5 C4 117.7(5) . . . . ? C8 Fe1 C5 C4 44.1(11) . . . . ? C3 Fe1 C5 C4 -37.5(5) . . . . ? C7 Fe1 C5 C4 -169.0(7) . . . . ? C2 Fe1 C5 C1 38.7(4) . . . . ? C9 Fe1 C5 C1 -163.5(4) . . . . ? C6 Fe1 C5 C1 -80.4(4) . . . . ? C10 Fe1 C5 C1 -122.4(4) . . . . ? C8 Fe1 C5 C1 164.1(8) . . . . ? C3 Fe1 C5 C1 82.4(4) . . . . ? C4 Fe1 C5 C1 119.9(6) . . . . ? C7 Fe1 C5 C1 -49.1(9) . . . . ? C2 Fe1 C6 C7 77.5(5) . . . . ? C1 Fe1 C6 C7 119.7(4) . . . . ? C9 Fe1 C6 C7 -81.4(5) . . . . ? C10 Fe1 C6 C7 -118.7(6) . . . . ? C8 Fe1 C6 C7 -36.8(4) . . . . ? C3 Fe1 C6 C7 43.4(10) . . . . ? C4 Fe1 C6 C7 -162.8(6) . . . . ? C5 Fe1 C6 C7 162.7(4) . . . . ? C2 Fe1 C6 C10 -163.9(4) . . . . ? C1 Fe1 C6 C10 -121.6(4) . . . . ? C9 Fe1 C6 C10 37.3(5) . . . . ? C8 Fe1 C6 C10 81.9(5) . . . . ? C3 Fe1 C6 C10 162.1(8) . . . . ? C4 Fe1 C6 C10 -44.1(9) . . . . ? C5 Fe1 C6 C10 -78.7(5) . . . . ? C7 Fe1 C6 C10 118.7(6) . . . . ? C10 C6 C7 C8 -1.8(7) . . . . ? Fe1 C6 C7 C8 58.2(5) . . . . ? C10 C6 C7 Fe1 -60.0(5) . . . . ? C2 Fe1 C7 C8 117.2(5) . . . . ? C1 Fe1 C7 C8 160.7(4) . . . . ? C9 Fe1 C7 C8 -38.7(5) . . . . ? C6 Fe1 C7 C8 -120.3(6) . . . . ? C10 Fe1 C7 C8 -82.2(5) . . . . ? C3 Fe1 C7 C8 75.0(5) . . . . ? C4 Fe1 C7 C8 38.9(11) . . . . ? C5 Fe1 C7 C8 -163.1(7) . . . . ? C2 Fe1 C7 C6 -122.5(4) . . . . ? C1 Fe1 C7 C6 -79.0(5) . . . . ? C9 Fe1 C7 C6 81.6(5) . . . . ? C10 Fe1 C7 C6 38.1(4) . . . . ? C8 Fe1 C7 C6 120.3(6) . . . . ? C3 Fe1 C7 C6 -164.7(4) . . . . ? C4 Fe1 C7 C6 159.2(8) . . . . ? C5 Fe1 C7 C6 -42.8(9) . . . . ? C6 C7 C8 C9 1.4(8) . . . . ? Fe1 C7 C8 C9 59.3(5) . . . . ? C6 C7 C8 Fe1 -57.9(5) . . . . ? C2 Fe1 C8 C7 -81.7(5) . . . . ? C1 Fe1 C8 C7 -46.6(9) . . . . ? C9 Fe1 C8 C7 118.5(6) . . . . ? C6 Fe1 C8 C7 37.1(4) . . . . ? C10 Fe1 C8 C7 81.1(5) . . . . ? C3 Fe1 C8 C7 -123.9(4) . . . . ? C4 Fe1 C8 C7 -165.6(4) . . . . ? C5 Fe1 C8 C7 161.6(8) . . . . ? C2 Fe1 C8 C9 159.8(5) . . . . ? C1 Fe1 C8 C9 -165.1(6) . . . . ? C6 Fe1 C8 C9 -81.4(5) . . . . ? C10 Fe1 C8 C9 -37.4(5) . . . . ? C3 Fe1 C8 C9 117.6(5) . . . . ? C4 Fe1 C8 C9 75.9(6) . . . . ? C5 Fe1 C8 C9 43.1(11) . . . . ? C7 Fe1 C8 C9 -118.5(6) . . . . ? C7 C8 C9 C10 -0.5(8) . . . . ? Fe1 C8 C9 C10 59.9(5) . . . . ? C7 C8 C9 Fe1 -60.4(5) . . . . ? C2 Fe1 C9 C10 -168.2(7) . . . . ? C1 Fe1 C9 C10 44.5(10) . . . . ? C6 Fe1 C9 C10 -37.7(5) . . . . ? C8 Fe1 C9 C10 -119.0(7) . . . . ? C3 Fe1 C9 C10 159.8(5) . . . . ? C4 Fe1 C9 C10 118.2(5) . . . . ? C5 Fe1 C9 C10 77.1(5) . . . . ? C7 Fe1 C9 C10 -81.5(5) . . . . ? C2 Fe1 C9 C8 -49.2(10) . . . . ? C1 Fe1 C9 C8 163.5(7) . . . . ? C6 Fe1 C9 C8 81.2(5) . . . . ? C10 Fe1 C9 C8 119.0(7) . . . . ? C3 Fe1 C9 C8 -81.2(5) . . . . ? C4 Fe1 C9 C8 -122.9(5) . . . . ? C5 Fe1 C9 C8 -163.9(4) . . . . ? C7 Fe1 C9 C8 37.5(4) . . . . ? C8 C9 C10 C6 -0.6(8) . . . . ? Fe1 C9 C10 C6 59.1(5) . . . . ? C8 C9 C10 Fe1 -59.7(5) . . . . ? C7 C6 C10 C9 1.5(8) . . . . ? Fe1 C6 C10 C9 -59.1(5) . . . . ? C7 C6 C10 Fe1 60.6(4) . . . . ? C2 Fe1 C10 C9 165.5(8) . . . . ? C1 Fe1 C10 C9 -163.0(4) . . . . ? C6 Fe1 C10 C9 119.5(6) . . . . ? C8 Fe1 C10 C9 38.4(5) . . . . ? C3 Fe1 C10 C9 -46.7(9) . . . . ? C4 Fe1 C10 C9 -79.2(5) . . . . ? C5 Fe1 C10 C9 -121.0(5) . . . . ? C7 Fe1 C10 C9 81.6(5) . . . . ? C2 Fe1 C10 C6 46.0(11) . . . . ? C1 Fe1 C10 C6 77.5(5) . . . . ? C9 Fe1 C10 C6 -119.5(6) . . . . ? C8 Fe1 C10 C6 -81.1(5) . . . . ? C3 Fe1 C10 C6 -166.2(6) . . . . ? C4 Fe1 C10 C6 161.3(4) . . . . ? C5 Fe1 C10 C6 119.6(4) . . . . ? C7 Fe1 C10 C6 -37.8(4) . . . . ? C22 Fe2 C21 C25 -118.3(6) . . . . ? C29 Fe2 C21 C25 45.2(8) . . . . ? C23 Fe2 C21 C25 -80.5(5) . . . . ? C26 Fe2 C21 C25 120.5(4) . . . . ? C30 Fe2 C21 C25 78.3(5) . . . . ? C28 Fe2 C21 C25 -166.4(8) . . . . ? C24 Fe2 C21 C25 -37.1(4) . . . . ? C27 Fe2 C21 C25 162.1(4) . . . . ? C25 Fe2 C21 C22 118.3(6) . . . . ? C29 Fe2 C21 C22 163.5(6) . . . . ? C23 Fe2 C21 C22 37.8(4) . . . . ? C26 Fe2 C21 C22 -121.3(4) . . . . ? C30 Fe2 C21 C22 -163.4(4) . . . . ? C28 Fe2 C21 C22 -48.1(10) . . . . ? C24 Fe2 C21 C22 81.2(4) . . . . ? C27 Fe2 C21 C22 -79.6(5) . . . . ? C25 Fe2 C21 I21 -122.6(6) . . . . ? C22 Fe2 C21 I21 119.1(6) . . . . ? C29 Fe2 C21 I21 -77.4(8) . . . . ? C23 Fe2 C21 I21 157.0(5) . . . . ? C26 Fe2 C21 I21 -2.1(5) . . . . ? C30 Fe2 C21 I21 -44.3(6) . . . . ? C28 Fe2 C21 I21 71.1(10) . . . . ? C24 Fe2 C21 I21 -159.6(5) . . . . ? C27 Fe2 C21 I21 39.5(6) . . . . ? C25 C21 C22 C23 1.0(7) . . . . ? I21 C21 C22 C23 176.2(4) . . . . ? Fe2 C21 C22 C23 -59.2(4) . . . . ? C25 C21 C22 Br22 -172.3(5) . . . . ? I21 C21 C22 Br22 2.9(8) . . . . ? Fe2 C21 C22 Br22 127.5(5) . . . . ? C25 C21 C22 Fe2 60.1(4) . . . . ? I21 C21 C22 Fe2 -124.6(5) . . . . ? C25 Fe2 C22 C21 -38.3(4) . . . . ? C29 Fe2 C22 C21 -161.3(7) . . . . ? C23 Fe2 C22 C21 -119.3(6) . . . . ? C26 Fe2 C22 C21 78.0(5) . . . . ? C30 Fe2 C22 C21 42.2(9) . . . . ? C28 Fe2 C22 C21 162.6(4) . . . . ? C24 Fe2 C22 C21 -81.8(4) . . . . ? C27 Fe2 C22 C21 120.7(4) . . . . ? C21 Fe2 C22 C23 119.3(6) . . . . ? C25 Fe2 C22 C23 81.0(5) . . . . ? C29 Fe2 C22 C23 -42.0(10) . . . . ? C26 Fe2 C22 C23 -162.7(5) . . . . ? C30 Fe2 C22 C23 161.5(7) . . . . ? C28 Fe2 C22 C23 -78.1(5) . . . . ? C24 Fe2 C22 C23 37.5(5) . . . . ? C27 Fe2 C22 C23 -120.0(5) . . . . ? C21 Fe2 C22 Br22 -120.1(6) . . . . ? C25 Fe2 C22 Br22 -158.4(5) . . . . ? C29 Fe2 C22 Br22 78.6(9) . . . . ? C23 Fe2 C22 Br22 120.6(7) . . . . ? C26 Fe2 C22 Br22 -42.0(6) . . . . ? C30 Fe2 C22 Br22 -77.9(9) . . . . ? C28 Fe2 C22 Br22 42.5(6) . . . . ? C24 Fe2 C22 Br22 158.1(6) . . . . ? C27 Fe2 C22 Br22 0.6(5) . . . . ? C21 C22 C23 C24 -1.1(7) . . . . ? Br22 C22 C23 C24 172.2(5) . . . . ? Fe2 C22 C23 C24 -59.9(5) . . . . ? C21 C22 C23 Fe2 58.7(4) . . . . ? Br22 C22 C23 Fe2 -128.0(5) . . . . ? C21 Fe2 C23 C24 81.2(5) . . . . ? C25 Fe2 C23 C24 37.1(4) . . . . ? C22 Fe2 C23 C24 119.1(6) . . . . ? C29 Fe2 C23 C24 -76.8(5) . . . . ? C26 Fe2 C23 C24 165.7(8) . . . . ? C30 Fe2 C23 C24 -43.1(10) . . . . ? C28 Fe2 C23 C24 -119.2(5) . . . . ? C27 Fe2 C23 C24 -160.7(4) . . . . ? C21 Fe2 C23 C22 -37.9(4) . . . . ? C25 Fe2 C23 C22 -82.0(5) . . . . ? C29 Fe2 C23 C22 164.1(4) . . . . ? C26 Fe2 C23 C22 46.5(10) . . . . ? C30 Fe2 C23 C22 -162.2(7) . . . . ? C28 Fe2 C23 C22 121.7(4) . . . . ? C24 Fe2 C23 C22 -119.1(6) . . . . ? C27 Fe2 C23 C22 80.2(5) . . . . ? C22 C23 C24 C25 0.9(8) . . . . ? Fe2 C23 C24 C25 -58.3(5) . . . . ? C22 C23 C24 Fe2 59.2(5) . . . . ? C21 Fe2 C24 C23 -82.5(4) . . . . ? C25 Fe2 C24 C23 -120.1(6) . . . . ? C22 Fe2 C24 C23 -38.1(4) . . . . ? C29 Fe2 C24 C23 121.2(4) . . . . ? C26 Fe2 C24 C23 -166.6(7) . . . . ? C30 Fe2 C24 C23 162.5(4) . . . . ? C28 Fe2 C24 C23 79.8(5) . . . . ? C27 Fe2 C24 C23 49.2(10) . . . . ? C21 Fe2 C24 C25 37.6(4) . . . . ? C22 Fe2 C24 C25 81.9(4) . . . . ? C29 Fe2 C24 C25 -118.8(4) . . . . ? C23 Fe2 C24 C25 120.1(6) . . . . ? C26 Fe2 C24 C25 -46.6(9) . . . . ? C30 Fe2 C24 C25 -77.4(5) . . . . ? C28 Fe2 C24 C25 -160.2(4) . . . . ? C27 Fe2 C24 C25 169.2(7) . . . . ? C23 C24 C25 C21 -0.3(8) . . . . ? Fe2 C24 C25 C21 -58.7(4) . . . . ? C23 C24 C25 Fe2 58.4(5) . . . . ? C22 C21 C25 C24 -0.4(7) . . . . ? I21 C21 C25 C24 -175.5(4) . . . . ? Fe2 C21 C25 C24 59.6(5) . . . . ? C22 C21 C25 Fe2 -60.0(4) . . . . ? I21 C21 C25 Fe2 124.8(5) . . . . ? C21 Fe2 C25 C24 -119.9(6) . . . . ? C22 Fe2 C25 C24 -81.4(5) . . . . ? C29 Fe2 C25 C24 78.8(5) . . . . ? C23 Fe2 C25 C24 -37.1(4) . . . . ? C26 Fe2 C25 C24 161.5(4) . . . . ? C30 Fe2 C25 C24 120.3(4) . . . . ? C28 Fe2 C25 C24 48.3(9) . . . . ? C27 Fe2 C25 C24 -168.5(8) . . . . ? C22 Fe2 C25 C21 38.5(4) . . . . ? C29 Fe2 C25 C21 -161.2(4) . . . . ? C23 Fe2 C25 C21 82.8(4) . . . . ? C26 Fe2 C25 C21 -78.6(5) . . . . ? C30 Fe2 C25 C21 -119.7(4) . . . . ? C28 Fe2 C25 C21 168.2(7) . . . . ? C24 Fe2 C25 C21 119.9(6) . . . . ? C27 Fe2 C25 C21 -48.5(10) . . . . ? C21 Fe2 C26 C30 -118.5(4) . . . . ? C25 Fe2 C26 C30 -76.2(5) . . . . ? C22 Fe2 C26 C30 -161.1(4) . . . . ? C29 Fe2 C26 C30 37.6(4) . . . . ? C23 Fe2 C26 C30 164.0(8) . . . . ? C28 Fe2 C26 C30 81.5(4) . . . . ? C24 Fe2 C26 C30 -42.0(9) . . . . ? C27 Fe2 C26 C30 119.0(6) . . . . ? C21 Fe2 C26 C27 122.5(4) . . . . ? C25 Fe2 C26 C27 164.9(4) . . . . ? C22 Fe2 C26 C27 80.0(5) . . . . ? C29 Fe2 C26 C27 -81.4(4) . . . . ? C23 Fe2 C26 C27 45.0(10) . . . . ? C30 Fe2 C26 C27 -119.0(6) . . . . ? C28 Fe2 C26 C27 -37.5(4) . . . . ? C24 Fe2 C26 C27 -161.0(7) . . . . ? C30 C26 C27 C28 -0.4(7) . . . . ? Fe2 C26 C27 C28 59.4(5) . . . . ? C30 C26 C27 Fe2 -59.8(4) . . . . ? C21 Fe2 C27 C28 164.4(4) . . . . ? C25 Fe2 C27 C28 -159.2(7) . . . . ? C22 Fe2 C27 C28 121.1(4) . . . . ? C29 Fe2 C27 C28 -37.5(4) . . . . ? C23 Fe2 C27 C28 77.9(5) . . . . ? C26 Fe2 C27 C28 -119.0(6) . . . . ? C30 Fe2 C27 C28 -81.2(4) . . . . ? C24 Fe2 C27 C28 41.8(10) . . . . ? C21 Fe2 C27 C26 -76.6(5) . . . . ? C25 Fe2 C27 C26 -40.2(10) . . . . ? C22 Fe2 C27 C26 -119.9(4) . . . . ? C29 Fe2 C27 C26 81.5(4) . . . . ? C23 Fe2 C27 C26 -163.1(4) . . . . ? C30 Fe2 C27 C26 37.8(4) . . . . ? C28 Fe2 C27 C26 119.0(6) . . . . ? C24 Fe2 C27 C26 160.8(7) . . . . ? C26 C27 C28 C29 -0.1(8) . . . . ? Fe2 C27 C28 C29 59.0(5) . . . . ? C26 C27 C28 Fe2 -59.1(5) . . . . ? C21 Fe2 C28 C27 -42.2(10) . . . . ? C25 Fe2 C28 C27 161.6(7) . . . . ? C22 Fe2 C28 C27 -78.6(5) . . . . ? C29 Fe2 C28 C27 119.6(6) . . . . ? C23 Fe2 C28 C27 -121.2(4) . . . . ? C26 Fe2 C28 C27 37.9(4) . . . . ? C30 Fe2 C28 C27 81.8(4) . . . . ? C24 Fe2 C28 C27 -163.3(4) . . . . ? C21 Fe2 C28 C29 -161.8(7) . . . . ? C25 Fe2 C28 C29 42.0(9) . . . . ? C22 Fe2 C28 C29 161.8(4) . . . . ? C23 Fe2 C28 C29 119.2(5) . . . . ? C26 Fe2 C28 C29 -81.7(4) . . . . ? C30 Fe2 C28 C29 -37.8(4) . . . . ? C24 Fe2 C28 C29 77.0(5) . . . . ? C27 Fe2 C28 C29 -119.6(6) . . . . ? C27 C28 C29 C30 0.6(7) . . . . ? Fe2 C28 C29 C30 60.1(4) . . . . ? C27 C28 C29 Fe2 -59.5(5) . . . . ? C21 Fe2 C29 C30 45.8(9) . . . . ? C25 Fe2 C29 C30 78.6(5) . . . . ? C22 Fe2 C29 C30 -167.2(7) . . . . ? C23 Fe2 C29 C30 161.3(4) . . . . ? C26 Fe2 C29 C30 -37.7(4) . . . . ? C28 Fe2 C29 C30 -118.8(6) . . . . ? C24 Fe2 C29 C30 120.2(4) . . . . ? C27 Fe2 C29 C30 -81.6(4) . . . . ? C21 Fe2 C29 C28 164.5(6) . . . . ? C25 Fe2 C29 C28 -162.6(4) . . . . ? C22 Fe2 C29 C28 -48.4(10) . . . . ? C23 Fe2 C29 C28 -79.9(5) . . . . ? C26 Fe2 C29 C28 81.1(5) . . . . ? C30 Fe2 C29 C28 118.8(6) . . . . ? C24 Fe2 C29 C28 -121.0(5) . . . . ? C27 Fe2 C29 C28 37.1(4) . . . . ? C28 C29 C30 C26 -0.9(7) . . . . ? Fe2 C29 C30 C26 59.2(4) . . . . ? C28 C29 C30 Fe2 -60.1(5) . . . . ? C27 C26 C30 C29 0.8(7) . . . . ? Fe2 C26 C30 C29 -59.2(4) . . . . ? C27 C26 C30 Fe2 60.0(5) . . . . ? C21 Fe2 C30 C29 -160.9(4) . . . . ? C25 Fe2 C30 C29 -118.9(4) . . . . ? C22 Fe2 C30 C29 167.7(7) . . . . ? C23 Fe2 C30 C29 -46.2(9) . . . . ? C26 Fe2 C30 C29 119.2(6) . . . . ? C28 Fe2 C30 C29 37.9(4) . . . . ? C24 Fe2 C30 C29 -77.6(5) . . . . ? C27 Fe2 C30 C29 81.3(4) . . . . ? C21 Fe2 C30 C26 79.9(4) . . . . ? C25 Fe2 C30 C26 121.9(4) . . . . ? C22 Fe2 C30 C26 48.6(9) . . . . ? C29 Fe2 C30 C26 -119.2(6) . . . . ? C23 Fe2 C30 C26 -165.4(8) . . . . ? C28 Fe2 C30 C26 -81.2(4) . . . . ? C24 Fe2 C30 C26 163.2(4) . . . . ? C27 Fe2 C30 C26 -37.8(4) . . . . ?