# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_rm007 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H26 Fe2' _chemical_formula_weight 570.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.9624(2) _cell_length_b 13.0786(7) _cell_length_c 19.7678(10) _cell_angle_alpha 92.174(4) _cell_angle_beta 95.890(4) _cell_angle_gamma 90.352(4) _cell_volume 1532.17(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5025 _cell_measurement_theta_min 3.1113 _cell_measurement_theta_max 32.3283 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 0.967 _exptl_absorpt_correction_T_min 0.7734 _exptl_absorpt_correction_T_max 0.8451 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Micro-Focus (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION SUPER NOVA' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10430 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5374 _reflns_number_gt 4325 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.0426P)^2^+0.0890P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5374 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0953 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.73245(5) 0.52776(2) 0.375060(15) 0.02184(11) Uani 1 1 d . . . Fe2 Fe 0.21926(5) 0.02101(2) 0.372084(15) 0.02078(11) Uani 1 1 d . . . C1 C 0.9312(4) 0.4855(2) 0.02429(12) 0.0337(6) Uani 1 1 d . . . C2 C 0.8128(4) 0.46075(19) 0.06626(12) 0.0313(6) Uani 1 1 d . . . C3 C 0.6761(4) 0.42929(18) 0.11760(11) 0.0264(5) Uani 1 1 d . . . C4 C 0.4597(4) 0.39026(18) 0.09983(12) 0.0297(6) Uani 1 1 d . . . H4 H 0.3971 0.3873 0.0536 0.036 Uiso 1 1 calc R . . C5 C 0.3368(4) 0.35577(18) 0.15030(12) 0.0295(6) Uani 1 1 d . . . H5 H 0.1895 0.3282 0.1385 0.035 Uiso 1 1 calc R . . C6 C 0.4259(4) 0.36103(17) 0.21734(11) 0.0243(5) Uani 1 1 d . . . H6 H 0.3386 0.3369 0.2511 0.029 Uiso 1 1 calc R . . C7 C 0.6407(4) 0.40077(16) 0.23689(11) 0.0205(5) Uani 1 1 d . . . C8 C 0.7655(4) 0.43562(17) 0.18579(11) 0.0236(5) Uani 1 1 d . . . H8 H 0.9122 0.4638 0.1976 0.028 Uiso 1 1 calc R . . C9 C 0.7397(4) 0.40437(16) 0.30821(11) 0.0205(5) Uani 1 1 d . . . C10 C 0.6258(4) 0.37813(16) 0.36658(11) 0.0239(5) Uani 1 1 d . . . H10 H 0.4746 0.3543 0.3655 0.029 Uiso 1 1 calc R . . C11 C 0.7807(4) 0.39446(18) 0.42577(12) 0.0300(6) Uani 1 1 d . . . H11 H 0.7502 0.3832 0.4711 0.036 Uiso 1 1 calc R . . C12 C 0.9877(4) 0.43022(17) 0.40591(11) 0.0284(5) Uani 1 1 d . . . H12 H 1.1197 0.4471 0.4355 0.034 Uiso 1 1 calc R . . C13 C 0.9634(4) 0.43638(17) 0.33409(11) 0.0246(5) Uani 1 1 d . . . H13 H 1.0772 0.4582 0.3074 0.030 Uiso 1 1 calc R . . C14 C 0.5513(5) 0.63638(19) 0.32231(14) 0.0425(7) Uani 1 1 d . . . H14 H 0.4773 0.6278 0.2775 0.051 Uiso 1 1 calc R . . C15 C 0.7778(5) 0.67039(19) 0.33979(16) 0.0472(8) Uani 1 1 d . . . H15 H 0.8820 0.6881 0.3088 0.057 Uiso 1 1 calc R . . C16 C 0.8204(5) 0.67315(19) 0.41184(16) 0.0421(7) Uani 1 1 d . . . H16 H 0.9578 0.6934 0.4376 0.050 Uiso 1 1 calc R . . C17 C 0.6224(4) 0.64049(19) 0.43828(13) 0.0350(6) Uani 1 1 d . . . H17 H 0.6034 0.6347 0.4851 0.042 Uiso 1 1 calc R . . C18 C 0.4561(4) 0.61770(18) 0.38302(13) 0.0341(6) Uani 1 1 d . . . H18 H 0.3069 0.5940 0.3864 0.041 Uiso 1 1 calc R . . C19 C 0.4304(4) 0.0178(2) 0.02354(12) 0.0329(6) Uani 1 1 d . . . C20 C 0.3110(4) 0.0494(2) 0.06492(12) 0.0322(6) Uani 1 1 d . . . C21 C 0.1735(4) 0.08803(18) 0.11532(11) 0.0269(5) Uani 1 1 d . . . C22 C -0.0412(4) 0.12552(18) 0.09653(12) 0.0298(6) Uani 1 1 d . . . H22 H -0.1005 0.1236 0.0500 0.036 Uiso 1 1 calc R . . C23 C -0.1681(4) 0.16571(18) 0.14608(12) 0.0293(6) Uani 1 1 d . . . H23 H -0.3150 0.1909 0.1334 0.035 Uiso 1 1 calc R . . C24 C -0.0817(4) 0.16926(17) 0.21376(11) 0.0240(5) Uani 1 1 d . . . H24 H -0.1695 0.1978 0.2471 0.029 Uiso 1 1 calc R . . C25 C 0.1321(4) 0.13160(15) 0.23396(10) 0.0198(5) Uani 1 1 d . . . C26 C 0.2585(4) 0.09099(17) 0.18413(11) 0.0241(5) Uani 1 1 d . . . H26 H 0.4044 0.0649 0.1970 0.029 Uiso 1 1 calc R . . C27 C 0.2258(4) 0.13726(16) 0.30603(11) 0.0201(5) Uani 1 1 d . . . C28 C 0.1089(4) 0.16844(16) 0.36341(11) 0.0227(5) Uani 1 1 d . . . H28 H -0.0431 0.1905 0.3616 0.027 Uiso 1 1 calc R . . C29 C 0.2607(4) 0.16054(17) 0.42334(12) 0.0270(5) Uani 1 1 d . . . H29 H 0.2271 0.1762 0.4685 0.032 Uiso 1 1 calc R . . C30 C 0.4697(4) 0.12552(18) 0.40448(11) 0.0280(6) Uani 1 1 d . . . H30 H 0.6010 0.1140 0.4346 0.034 Uiso 1 1 calc R . . C31 C 0.4495(4) 0.11051(17) 0.33237(11) 0.0256(5) Uani 1 1 d . . . H31 H 0.5650 0.0867 0.3062 0.031 Uiso 1 1 calc R . . C32 C 0.0395(5) -0.09433(19) 0.31864(14) 0.0418(7) Uani 1 1 d . . . H32 H -0.0346 -0.0904 0.2739 0.050 Uiso 1 1 calc R . . C33 C -0.0558(4) -0.07047(19) 0.37931(13) 0.0353(6) Uani 1 1 d . . . H33 H -0.2052 -0.0476 0.3829 0.042 Uiso 1 1 calc R . . C34 C 0.1101(4) -0.08651(18) 0.43411(13) 0.0324(6) Uani 1 1 d . . . H34 H 0.0912 -0.0763 0.4810 0.039 Uiso 1 1 calc R . . C35 C 0.3088(5) -0.12037(18) 0.40739(14) 0.0371(6) Uani 1 1 d . . . H35 H 0.4467 -0.1369 0.4329 0.044 Uiso 1 1 calc R . . C36 C 0.2646(5) -0.12516(19) 0.33549(15) 0.0451(8) Uani 1 1 d . . . H36 H 0.3680 -0.1455 0.3041 0.054 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 0.0262(2) 0.01595(18) 0.02432(19) -0.00180(13) 0.00834(15) -0.00018(14) Fe2 0.0256(2) 0.01580(18) 0.02172(19) 0.00015(13) 0.00659(14) -0.00025(14) C1 0.0298(14) 0.0489(17) 0.0235(12) 0.0113(11) 0.0034(11) 0.0035(12) C2 0.0323(14) 0.0374(15) 0.0241(12) 0.0066(11) 0.0006(11) 0.0033(11) C3 0.0280(13) 0.0271(13) 0.0253(12) 0.0060(10) 0.0067(10) 0.0047(10) C4 0.0302(13) 0.0344(14) 0.0243(12) 0.0023(10) 0.0015(10) 0.0038(11) C5 0.0236(13) 0.0306(14) 0.0341(14) -0.0008(11) 0.0029(11) -0.0016(10) C6 0.0263(13) 0.0208(12) 0.0274(12) 0.0004(10) 0.0106(10) -0.0010(10) C7 0.0251(12) 0.0135(11) 0.0242(12) 0.0006(9) 0.0080(10) 0.0033(9) C8 0.0233(12) 0.0236(12) 0.0245(12) 0.0012(9) 0.0048(10) -0.0007(9) C9 0.0271(13) 0.0130(11) 0.0224(11) -0.0020(9) 0.0090(10) 0.0010(9) C10 0.0309(13) 0.0167(11) 0.0256(12) 0.0010(9) 0.0102(10) -0.0006(10) C11 0.0441(16) 0.0231(13) 0.0239(12) 0.0040(10) 0.0074(11) -0.0003(11) C12 0.0357(14) 0.0224(13) 0.0266(12) -0.0017(10) 0.0013(11) 0.0039(10) C13 0.0259(13) 0.0210(12) 0.0280(12) -0.0010(10) 0.0090(10) 0.0029(10) C14 0.065(2) 0.0226(14) 0.0382(15) 0.0010(11) -0.0030(14) 0.0141(13) C15 0.059(2) 0.0154(13) 0.072(2) 0.0073(13) 0.0301(17) 0.0037(12) C16 0.0357(16) 0.0193(13) 0.069(2) -0.0158(13) 0.0000(14) -0.0025(11) C17 0.0394(16) 0.0309(14) 0.0346(14) -0.0113(11) 0.0079(12) 0.0091(11) C18 0.0317(14) 0.0240(13) 0.0459(16) -0.0059(11) 0.0028(12) 0.0055(11) C19 0.0326(15) 0.0435(16) 0.0219(12) -0.0079(11) 0.0035(11) -0.0033(12) C20 0.0309(14) 0.0406(15) 0.0239(12) -0.0055(11) -0.0003(11) -0.0029(11) C21 0.0291(13) 0.0285(13) 0.0237(12) -0.0038(10) 0.0076(10) -0.0035(10) C22 0.0299(14) 0.0354(14) 0.0232(12) -0.0016(10) -0.0003(10) -0.0045(11) C23 0.0223(13) 0.0319(14) 0.0337(14) 0.0024(11) 0.0027(11) 0.0000(10) C24 0.0260(13) 0.0202(12) 0.0275(12) 0.0002(9) 0.0108(10) 0.0005(10) C25 0.0243(12) 0.0125(11) 0.0235(11) -0.0007(9) 0.0069(9) -0.0030(9) C26 0.0237(12) 0.0233(12) 0.0252(12) -0.0022(9) 0.0034(10) -0.0003(9) C27 0.0243(12) 0.0140(11) 0.0231(11) 0.0019(9) 0.0066(9) -0.0019(9) C28 0.0280(13) 0.0152(11) 0.0260(12) -0.0024(9) 0.0096(10) -0.0010(9) C29 0.0379(15) 0.0216(12) 0.0218(12) -0.0030(9) 0.0067(11) -0.0052(10) C30 0.0309(14) 0.0279(13) 0.0244(12) -0.0016(10) 0.0001(10) -0.0077(11) C31 0.0266(13) 0.0240(13) 0.0274(12) 0.0015(10) 0.0082(10) -0.0046(10) C32 0.066(2) 0.0178(13) 0.0389(15) -0.0032(11) -0.0039(14) -0.0139(13) C33 0.0308(14) 0.0240(13) 0.0515(17) 0.0072(12) 0.0047(12) -0.0070(11) C34 0.0386(15) 0.0243(13) 0.0371(14) 0.0070(11) 0.0149(12) -0.0012(11) C35 0.0404(16) 0.0228(13) 0.0502(17) 0.0111(12) 0.0111(13) 0.0071(11) C36 0.071(2) 0.0167(13) 0.0524(18) -0.0026(12) 0.0309(16) 0.0028(13) _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 C13 2.039(2) . ? Fe1 C15 2.042(2) . ? Fe1 C14 2.043(3) . ? Fe1 C18 2.046(3) . ? Fe1 C10 2.049(2) . ? Fe1 C9 2.050(2) . ? Fe1 C11 2.051(2) . ? Fe1 C17 2.051(2) . ? Fe1 C12 2.052(2) . ? Fe1 C16 2.055(2) . ? Fe2 C31 2.035(2) . ? Fe2 C32 2.041(2) . ? Fe2 C33 2.044(2) . ? Fe2 C27 2.044(2) . ? Fe2 C34 2.046(2) . ? Fe2 C36 2.048(3) . ? Fe2 C28 2.049(2) . ? Fe2 C29 2.054(2) . ? Fe2 C30 2.054(2) . ? Fe2 C35 2.055(2) . ? C1 C2 1.196(3) . ? C1 C1 1.387(4) 2_765 ? C2 C3 1.436(3) . ? C3 C4 1.390(3) . ? C3 C8 1.397(3) . ? C4 C5 1.385(3) . ? C4 H4 0.9500 . ? C5 C6 1.375(3) . ? C5 H5 0.9500 . ? C6 C7 1.391(3) . ? C6 H6 0.9500 . ? C7 C8 1.403(3) . ? C7 C9 1.471(3) . ? C8 H8 0.9500 . ? C9 C13 1.432(3) . ? C9 C10 1.449(3) . ? C10 C11 1.423(3) . ? C10 H10 0.9500 . ? C11 C12 1.415(3) . ? C11 H11 0.9500 . ? C12 C13 1.418(3) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C18 1.408(4) . ? C14 C15 1.424(4) . ? C14 H14 0.9500 . ? C15 C16 1.420(4) . ? C15 H15 0.9500 . ? C16 C17 1.410(4) . ? C16 H16 0.9500 . ? C17 C18 1.419(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.202(3) . ? C19 C19 1.379(5) 2_655 ? C20 C21 1.433(3) . ? C21 C22 1.393(3) . ? C21 C26 1.401(3) . ? C22 C23 1.388(3) . ? C22 H22 0.9500 . ? C23 C24 1.382(3) . ? C23 H23 0.9500 . ? C24 C25 1.395(3) . ? C24 H24 0.9500 . ? C25 C26 1.392(3) . ? C25 C27 1.475(3) . ? C26 H26 0.9500 . ? C27 C31 1.432(3) . ? C27 C28 1.438(3) . ? C28 C29 1.423(3) . ? C28 H28 0.9500 . ? C29 C30 1.411(3) . ? C29 H29 0.9500 . ? C30 C31 1.424(3) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.404(4) . ? C32 C36 1.414(4) . ? C32 H32 0.9500 . ? C33 C34 1.413(4) . ? C33 H33 0.9500 . ? C34 C35 1.413(4) . ? C34 H34 0.9500 . ? C35 C36 1.418(4) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? 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 C13 Fe1 C15 106.17(10) . . ? C13 Fe1 C14 123.64(10) . . ? C15 Fe1 C14 40.80(11) . . ? C13 Fe1 C18 160.84(10) . . ? C15 Fe1 C18 68.18(11) . . ? C14 Fe1 C18 40.29(10) . . ? C13 Fe1 C10 68.76(9) . . ? C15 Fe1 C10 154.45(12) . . ? C14 Fe1 C10 119.80(11) . . ? C18 Fe1 C10 107.97(10) . . ? C13 Fe1 C9 41.01(9) . . ? C15 Fe1 C9 118.29(10) . . ? C14 Fe1 C9 105.33(10) . . ? C18 Fe1 C9 124.07(10) . . ? C10 Fe1 C9 41.39(8) . . ? C13 Fe1 C11 68.10(9) . . ? C15 Fe1 C11 162.65(12) . . ? C14 Fe1 C11 156.02(11) . . ? C18 Fe1 C11 122.53(10) . . ? C10 Fe1 C11 40.62(9) . . ? C9 Fe1 C11 68.91(9) . . ? C13 Fe1 C17 156.16(10) . . ? C15 Fe1 C17 67.91(11) . . ? C14 Fe1 C17 67.92(11) . . ? C18 Fe1 C17 40.53(10) . . ? C10 Fe1 C17 126.61(9) . . ? C9 Fe1 C17 162.49(10) . . ? C11 Fe1 C17 110.29(10) . . ? C13 Fe1 C12 40.56(9) . . ? C15 Fe1 C12 124.84(11) . . ? C14 Fe1 C12 161.21(10) . . ? C18 Fe1 C12 157.49(10) . . ? C10 Fe1 C12 68.48(9) . . ? C9 Fe1 C12 68.94(9) . . ? C11 Fe1 C12 40.35(9) . . ? C17 Fe1 C12 122.56(10) . . ? C13 Fe1 C16 120.38(10) . . ? C15 Fe1 C16 40.55(12) . . ? C14 Fe1 C16 68.23(11) . . ? C18 Fe1 C16 68.04(10) . . ? C10 Fe1 C16 163.58(11) . . ? C9 Fe1 C16 154.22(10) . . ? C11 Fe1 C16 126.93(11) . . ? C17 Fe1 C16 40.16(10) . . ? C12 Fe1 C16 108.71(11) . . ? C31 Fe2 C32 123.99(10) . . ? C31 Fe2 C33 161.12(10) . . ? C32 Fe2 C33 40.21(10) . . ? C31 Fe2 C27 41.10(9) . . ? C32 Fe2 C27 105.26(10) . . ? C33 Fe2 C27 124.08(9) . . ? C31 Fe2 C34 156.07(10) . . ? C32 Fe2 C34 67.68(10) . . ? C33 Fe2 C34 40.41(10) . . ? C27 Fe2 C34 162.54(10) . . ? C31 Fe2 C36 106.53(10) . . ? C32 Fe2 C36 40.47(11) . . ? C33 Fe2 C36 67.89(11) . . ? C27 Fe2 C36 118.03(10) . . ? C34 Fe2 C36 67.73(10) . . ? C31 Fe2 C28 68.73(9) . . ? C32 Fe2 C28 119.17(11) . . ? C33 Fe2 C28 107.73(10) . . ? C27 Fe2 C28 41.15(8) . . ? C34 Fe2 C28 126.93(9) . . ? C36 Fe2 C28 153.50(11) . . ? C31 Fe2 C29 68.25(9) . . ? C32 Fe2 C29 155.12(11) . . ? C33 Fe2 C29 121.93(10) . . ? C27 Fe2 C29 68.79(9) . . ? C34 Fe2 C29 110.46(10) . . ? C36 Fe2 C29 163.87(12) . . ? C28 Fe2 C29 40.58(9) . . ? C31 Fe2 C30 40.75(9) . . ? C32 Fe2 C30 162.16(11) . . ? C33 Fe2 C30 156.83(10) . . ? C27 Fe2 C30 68.87(9) . . ? C34 Fe2 C30 122.60(10) . . ? C36 Fe2 C30 126.12(12) . . ? C28 Fe2 C30 68.21(10) . . ? C29 Fe2 C30 40.17(10) . . ? C31 Fe2 C35 120.27(10) . . ? C32 Fe2 C35 67.98(11) . . ? C33 Fe2 C35 68.01(11) . . ? C27 Fe2 C35 153.79(10) . . ? C34 Fe2 C35 40.30(10) . . ? C36 Fe2 C35 40.43(11) . . ? C28 Fe2 C35 164.43(10) . . ? C29 Fe2 C35 127.81(10) . . ? C30 Fe2 C35 109.42(11) . . ? C2 C1 C1 179.8(4) . 2_765 ? C1 C2 C3 178.3(3) . . ? C4 C3 C8 120.20(19) . . ? C4 C3 C2 120.7(2) . . ? C8 C3 C2 119.1(2) . . ? C5 C4 C3 119.2(2) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C6 C5 C4 120.6(2) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C7 121.65(19) . . ? C5 C6 H6 119.2 . . ? C7 C6 H6 119.2 . . ? C6 C7 C8 117.8(2) . . ? C6 C7 C9 122.08(18) . . ? C8 C7 C9 120.07(19) . . ? C3 C8 C7 120.6(2) . . ? C3 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C13 C9 C10 106.48(19) . . ? C13 C9 C7 127.41(18) . . ? C10 C9 C7 126.1(2) . . ? C13 C9 Fe1 69.06(12) . . ? C10 C9 Fe1 69.28(12) . . ? C7 C9 Fe1 125.36(15) . . ? C11 C10 C9 107.79(19) . . ? C11 C10 Fe1 69.75(12) . . ? C9 C10 Fe1 69.33(11) . . ? C11 C10 H10 126.1 . . ? C9 C10 H10 126.1 . . ? Fe1 C10 H10 126.4 . . ? C12 C11 C10 108.8(2) . . ? C12 C11 Fe1 69.84(13) . . ? C10 C11 Fe1 69.63(13) . . ? C12 C11 H11 125.6 . . ? C10 C11 H11 125.6 . . ? Fe1 C11 H11 126.5 . . ? C11 C12 C13 107.9(2) . . ? C11 C12 Fe1 69.80(14) . . ? C13 C12 Fe1 69.23(13) . . ? C11 C12 H12 126.1 . . ? C13 C12 H12 126.1 . . ? Fe1 C12 H12 126.5 . . ? C12 C13 C9 109.08(19) . . ? C12 C13 Fe1 70.21(14) . . ? C9 C13 Fe1 69.93(12) . . ? C12 C13 H13 125.5 . . ? C9 C13 H13 125.5 . . ? Fe1 C13 H13 126.0 . . ? C18 C14 C15 108.0(2) . . ? C18 C14 Fe1 69.99(14) . . ? C15 C14 Fe1 69.58(15) . . ? C18 C14 H14 126.0 . . ? C15 C14 H14 126.0 . . ? Fe1 C14 H14 126.0 . . ? C16 C15 C14 107.8(2) . . ? C16 C15 Fe1 70.22(14) . . ? C14 C15 Fe1 69.62(14) . . ? C16 C15 H15 126.1 . . ? C14 C15 H15 126.1 . . ? Fe1 C15 H15 125.7 . . ? C17 C16 C15 107.8(2) . . ? C17 C16 Fe1 69.76(14) . . ? C15 C16 Fe1 69.23(15) . . ? C17 C16 H16 126.1 . . ? C15 C16 H16 126.1 . . ? Fe1 C16 H16 126.5 . . ? C16 C17 C18 108.4(2) . . ? C16 C17 Fe1 70.07(14) . . ? C18 C17 Fe1 69.54(14) . . ? C16 C17 H17 125.8 . . ? C18 C17 H17 125.8 . . ? Fe1 C17 H17 126.2 . . ? C14 C18 C17 108.0(2) . . ? C14 C18 Fe1 69.72(15) . . ? C17 C18 Fe1 69.92(14) . . ? C14 C18 H18 126.0 . . ? C17 C18 H18 126.0 . . ? Fe1 C18 H18 125.9 . . ? C20 C19 C19 179.3(4) . 2_655 ? C19 C20 C21 178.6(3) . . ? C22 C21 C26 119.6(2) . . ? C22 C21 C20 120.8(2) . . ? C26 C21 C20 119.6(2) . . ? C23 C22 C21 119.7(2) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.2 . . ? C24 C23 C22 120.3(2) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C25 121.2(2) . . ? C23 C24 H24 119.4 . . ? C25 C24 H24 119.4 . . ? C26 C25 C24 118.4(2) . . ? C26 C25 C27 120.5(2) . . ? C24 C25 C27 121.1(2) . . ? C25 C26 C21 120.9(2) . . ? C25 C26 H26 119.5 . . ? C21 C26 H26 119.5 . . ? C31 C27 C28 106.86(19) . . ? C31 C27 C25 126.4(2) . . ? C28 C27 C25 126.7(2) . . ? C31 C27 Fe2 69.12(12) . . ? C28 C27 Fe2 69.60(12) . . ? C25 C27 Fe2 125.27(14) . . ? C29 C28 C27 108.0(2) . . ? C29 C28 Fe2 69.92(13) . . ? C27 C28 Fe2 69.25(12) . . ? C29 C28 H28 126.0 . . ? C27 C28 H28 126.0 . . ? Fe2 C28 H28 126.4 . . ? C30 C29 C28 108.6(2) . . ? C30 C29 Fe2 69.92(13) . . ? C28 C29 Fe2 69.50(13) . . ? C30 C29 H29 125.7 . . ? C28 C29 H29 125.7 . . ? Fe2 C29 H29 126.4 . . ? C29 C30 C31 108.0(2) . . ? C29 C30 Fe2 69.91(13) . . ? C31 C30 Fe2 68.90(12) . . ? C29 C30 H30 126.0 . . ? C31 C30 H30 126.0 . . ? Fe2 C30 H30 126.8 . . ? C30 C31 C27 108.5(2) . . ? C30 C31 Fe2 70.35(12) . . ? C27 C31 Fe2 69.79(11) . . ? C30 C31 H31 125.8 . . ? C27 C31 H31 125.8 . . ? Fe2 C31 H31 125.7 . . ? C33 C32 C36 108.3(2) . . ? C33 C32 Fe2 69.99(14) . . ? C36 C32 Fe2 70.01(15) . . ? C33 C32 H32 125.8 . . ? C36 C32 H32 125.8 . . ? Fe2 C32 H32 125.7 . . ? C32 C33 C34 107.8(2) . . ? C32 C33 Fe2 69.80(13) . . ? C34 C33 Fe2 69.90(13) . . ? C32 C33 H33 126.1 . . ? C34 C33 H33 126.1 . . ? Fe2 C33 H33 125.8 . . ? C35 C34 C33 108.5(2) . . ? C35 C34 Fe2 70.19(12) . . ? C33 C34 Fe2 69.70(13) . . ? C35 C34 H34 125.8 . . ? C33 C34 H34 125.8 . . ? Fe2 C34 H34 125.9 . . ? C34 C35 C36 107.4(3) . . ? C34 C35 Fe2 69.51(14) . . ? C36 C35 Fe2 69.49(14) . . ? C34 C35 H35 126.3 . . ? C36 C35 H35 126.3 . . ? Fe2 C35 H35 126.3 . . ? C32 C36 C35 108.0(2) . . ? C32 C36 Fe2 69.52(15) . . ? C35 C36 Fe2 70.08(15) . . ? C32 C36 H36 126.0 . . ? C35 C36 H36 126.0 . . ? Fe2 C36 H36 125.9 . . ? 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 C1 C1 C2 C3 -108(100) 2_765 . . . ? C1 C2 C3 C4 -131(10) . . . . ? C1 C2 C3 C8 47(10) . . . . ? C8 C3 C4 C5 -1.4(4) . . . . ? C2 C3 C4 C5 176.7(2) . . . . ? C3 C4 C5 C6 0.7(4) . . . . ? C4 C5 C6 C7 0.0(4) . . . . ? C5 C6 C7 C8 -0.1(3) . . . . ? C5 C6 C7 C9 -178.4(2) . . . . ? C4 C3 C8 C7 1.4(4) . . . . ? C2 C3 C8 C7 -176.8(2) . . . . ? C6 C7 C8 C3 -0.6(3) . . . . ? C9 C7 C8 C3 177.8(2) . . . . ? C6 C7 C9 C13 175.2(2) . . . . ? C8 C7 C9 C13 -3.1(3) . . . . ? C6 C7 C9 C10 -6.5(3) . . . . ? C8 C7 C9 C10 175.2(2) . . . . ? C6 C7 C9 Fe1 -95.3(2) . . . . ? C8 C7 C9 Fe1 86.4(2) . . . . ? C15 Fe1 C9 C13 82.13(16) . . . . ? C14 Fe1 C9 C13 124.07(14) . . . . ? C18 Fe1 C9 C13 163.76(13) . . . . ? C10 Fe1 C9 C13 -118.01(18) . . . . ? C11 Fe1 C9 C13 -80.46(14) . . . . ? C17 Fe1 C9 C13 -171.2(3) . . . . ? C12 Fe1 C9 C13 -37.08(12) . . . . ? C16 Fe1 C9 C13 52.5(3) . . . . ? C13 Fe1 C9 C10 118.01(18) . . . . ? C15 Fe1 C9 C10 -159.86(15) . . . . ? C14 Fe1 C9 C10 -117.93(15) . . . . ? C18 Fe1 C9 C10 -78.23(16) . . . . ? C11 Fe1 C9 C10 37.54(14) . . . . ? C17 Fe1 C9 C10 -53.2(3) . . . . ? C12 Fe1 C9 C10 80.93(14) . . . . ? C16 Fe1 C9 C10 170.5(2) . . . . ? C13 Fe1 C9 C7 -121.7(2) . . . . ? C15 Fe1 C9 C7 -39.6(2) . . . . ? C14 Fe1 C9 C7 2.3(2) . . . . ? C18 Fe1 C9 C7 42.0(2) . . . . ? C10 Fe1 C9 C7 120.3(2) . . . . ? C11 Fe1 C9 C7 157.8(2) . . . . ? C17 Fe1 C9 C7 67.1(4) . . . . ? C12 Fe1 C9 C7 -158.8(2) . . . . ? C16 Fe1 C9 C7 -69.2(3) . . . . ? C13 C9 C10 C11 -0.1(2) . . . . ? C7 C9 C10 C11 -178.7(2) . . . . ? Fe1 C9 C10 C11 -59.37(16) . . . . ? C13 C9 C10 Fe1 59.30(15) . . . . ? C7 C9 C10 Fe1 -119.3(2) . . . . ? C13 Fe1 C10 C11 80.71(15) . . . . ? C15 Fe1 C10 C11 163.8(2) . . . . ? C14 Fe1 C10 C11 -161.75(15) . . . . ? C18 Fe1 C10 C11 -119.34(15) . . . . ? C9 Fe1 C10 C11 119.2(2) . . . . ? C17 Fe1 C10 C11 -78.31(17) . . . . ? C12 Fe1 C10 C11 37.01(14) . . . . ? C16 Fe1 C10 C11 -46.2(4) . . . . ? C13 Fe1 C10 C9 -38.44(13) . . . . ? C15 Fe1 C10 C9 44.7(3) . . . . ? C14 Fe1 C10 C9 79.10(16) . . . . ? C18 Fe1 C10 C9 121.51(14) . . . . ? C11 Fe1 C10 C9 -119.2(2) . . . . ? C17 Fe1 C10 C9 162.54(14) . . . . ? C12 Fe1 C10 C9 -82.14(14) . . . . ? C16 Fe1 C10 C9 -165.4(3) . . . . ? C9 C10 C11 C12 0.1(3) . . . . ? Fe1 C10 C11 C12 -59.04(16) . . . . ? C9 C10 C11 Fe1 59.11(15) . . . . ? C13 Fe1 C11 C12 37.67(13) . . . . ? C15 Fe1 C11 C12 -36.1(4) . . . . ? C14 Fe1 C11 C12 162.1(2) . . . . ? C18 Fe1 C11 C12 -160.32(14) . . . . ? C10 Fe1 C11 C12 120.1(2) . . . . ? C9 Fe1 C11 C12 81.90(14) . . . . ? C17 Fe1 C11 C12 -116.81(15) . . . . ? C16 Fe1 C11 C12 -74.65(18) . . . . ? C13 Fe1 C11 C10 -82.46(15) . . . . ? C15 Fe1 C11 C10 -156.2(3) . . . . ? C14 Fe1 C11 C10 42.0(3) . . . . ? C18 Fe1 C11 C10 79.55(17) . . . . ? C9 Fe1 C11 C10 -38.24(13) . . . . ? C17 Fe1 C11 C10 123.06(14) . . . . ? C12 Fe1 C11 C10 -120.1(2) . . . . ? C16 Fe1 C11 C10 165.21(14) . . . . ? C10 C11 C12 C13 0.0(3) . . . . ? Fe1 C11 C12 C13 -58.96(16) . . . . ? C10 C11 C12 Fe1 58.91(17) . . . . ? C13 Fe1 C12 C11 -119.3(2) . . . . ? C15 Fe1 C12 C11 167.65(16) . . . . ? C14 Fe1 C12 C11 -157.2(3) . . . . ? C18 Fe1 C12 C11 47.9(3) . . . . ? C10 Fe1 C12 C11 -37.24(14) . . . . ? C9 Fe1 C12 C11 -81.82(14) . . . . ? C17 Fe1 C12 C11 83.34(16) . . . . ? C16 Fe1 C12 C11 125.52(15) . . . . ? C15 Fe1 C12 C13 -73.05(18) . . . . ? C14 Fe1 C12 C13 -37.9(4) . . . . ? C18 Fe1 C12 C13 167.2(2) . . . . ? C10 Fe1 C12 C13 82.05(14) . . . . ? C9 Fe1 C12 C13 37.48(12) . . . . ? C11 Fe1 C12 C13 119.3(2) . . . . ? C17 Fe1 C12 C13 -157.37(13) . . . . ? C16 Fe1 C12 C13 -115.18(15) . . . . ? C11 C12 C13 C9 0.0(3) . . . . ? Fe1 C12 C13 C9 -59.31(16) . . . . ? C11 C12 C13 Fe1 59.32(17) . . . . ? C10 C9 C13 C12 0.0(3) . . . . ? C7 C9 C13 C12 178.7(2) . . . . ? Fe1 C9 C13 C12 59.49(16) . . . . ? C10 C9 C13 Fe1 -59.44(15) . . . . ? C7 C9 C13 Fe1 119.2(2) . . . . ? C15 Fe1 C13 C12 125.17(15) . . . . ? C14 Fe1 C13 C12 166.25(14) . . . . ? C18 Fe1 C13 C12 -165.0(3) . . . . ? C10 Fe1 C13 C12 -81.31(14) . . . . ? C9 Fe1 C13 C12 -120.09(18) . . . . ? C11 Fe1 C13 C12 -37.49(14) . . . . ? C17 Fe1 C13 C12 53.4(3) . . . . ? C16 Fe1 C13 C12 83.51(16) . . . . ? C15 Fe1 C13 C9 -114.74(14) . . . . ? C14 Fe1 C13 C9 -73.66(16) . . . . ? C18 Fe1 C13 C9 -44.9(3) . . . . ? C10 Fe1 C13 C9 38.78(12) . . . . ? C11 Fe1 C13 C9 82.60(13) . . . . ? C17 Fe1 C13 C9 173.5(2) . . . . ? C12 Fe1 C13 C9 120.09(18) . . . . ? C16 Fe1 C13 C9 -156.41(14) . . . . ? C13 Fe1 C14 C18 165.86(14) . . . . ? C15 Fe1 C14 C18 -119.1(2) . . . . ? C10 Fe1 C14 C18 82.78(17) . . . . ? C9 Fe1 C14 C18 125.10(15) . . . . ? C11 Fe1 C14 C18 52.7(3) . . . . ? C17 Fe1 C14 C18 -37.83(14) . . . . ? C12 Fe1 C14 C18 -165.5(3) . . . . ? C16 Fe1 C14 C18 -81.28(17) . . . . ? C13 Fe1 C14 C15 -74.99(19) . . . . ? C18 Fe1 C14 C15 119.1(2) . . . . ? C10 Fe1 C14 C15 -158.07(16) . . . . ? C9 Fe1 C14 C15 -115.76(16) . . . . ? C11 Fe1 C14 C15 171.8(2) . . . . ? C17 Fe1 C14 C15 81.31(17) . . . . ? C12 Fe1 C14 C15 -46.3(4) . . . . ? C16 Fe1 C14 C15 37.87(16) . . . . ? C18 C14 C15 C16 -0.4(3) . . . . ? Fe1 C14 C15 C16 -60.08(18) . . . . ? C18 C14 C15 Fe1 59.66(17) . . . . ? C13 Fe1 C15 C16 -118.11(16) . . . . ? C14 Fe1 C15 C16 118.7(2) . . . . ? C18 Fe1 C15 C16 81.28(17) . . . . ? C10 Fe1 C15 C16 167.4(2) . . . . ? C9 Fe1 C15 C16 -160.70(16) . . . . ? C11 Fe1 C15 C16 -50.1(4) . . . . ? C17 Fe1 C15 C16 37.42(16) . . . . ? C12 Fe1 C15 C16 -77.74(19) . . . . ? C13 Fe1 C15 C14 123.15(16) . . . . ? C18 Fe1 C15 C14 -37.47(16) . . . . ? C10 Fe1 C15 C14 48.7(3) . . . . ? C9 Fe1 C15 C14 80.55(18) . . . . ? C11 Fe1 C15 C14 -168.8(3) . . . . ? C17 Fe1 C15 C14 -81.33(17) . . . . ? C12 Fe1 C15 C14 163.51(15) . . . . ? C16 Fe1 C15 C14 -118.7(2) . . . . ? C14 C15 C16 C17 0.4(3) . . . . ? Fe1 C15 C16 C17 -59.33(18) . . . . ? C14 C15 C16 Fe1 59.70(18) . . . . ? C13 Fe1 C16 C17 -161.67(15) . . . . ? C15 Fe1 C16 C17 119.2(2) . . . . ? C14 Fe1 C16 C17 81.12(17) . . . . ? C18 Fe1 C16 C17 37.56(16) . . . . ? C10 Fe1 C16 C17 -41.4(4) . . . . ? C9 Fe1 C16 C17 161.2(2) . . . . ? C11 Fe1 C16 C17 -77.41(19) . . . . ? C12 Fe1 C16 C17 -118.66(16) . . . . ? C13 Fe1 C16 C15 79.13(19) . . . . ? C14 Fe1 C16 C15 -38.09(17) . . . . ? C18 Fe1 C16 C15 -81.65(18) . . . . ? C10 Fe1 C16 C15 -160.6(3) . . . . ? C9 Fe1 C16 C15 42.0(3) . . . . ? C11 Fe1 C16 C15 163.38(16) . . . . ? C17 Fe1 C16 C15 -119.2(2) . . . . ? C12 Fe1 C16 C15 122.14(17) . . . . ? C15 C16 C17 C18 -0.2(3) . . . . ? Fe1 C16 C17 C18 -59.18(17) . . . . ? C15 C16 C17 Fe1 58.99(18) . . . . ? C13 Fe1 C17 C16 42.2(3) . . . . ? C15 Fe1 C17 C16 -37.77(17) . . . . ? C14 Fe1 C17 C16 -81.96(18) . . . . ? C18 Fe1 C17 C16 -119.6(2) . . . . ? C10 Fe1 C17 C16 166.53(16) . . . . ? C9 Fe1 C17 C16 -152.2(3) . . . . ? C11 Fe1 C17 C16 123.72(17) . . . . ? C12 Fe1 C17 C16 80.43(18) . . . . ? C13 Fe1 C17 C18 161.7(2) . . . . ? C15 Fe1 C17 C18 81.79(17) . . . . ? C14 Fe1 C17 C18 37.61(15) . . . . ? C10 Fe1 C17 C18 -73.91(18) . . . . ? C9 Fe1 C17 C18 -32.6(4) . . . . ? C11 Fe1 C17 C18 -116.72(15) . . . . ? C12 Fe1 C17 C18 -160.01(14) . . . . ? C16 Fe1 C17 C18 119.6(2) . . . . ? C15 C14 C18 C17 0.3(3) . . . . ? Fe1 C14 C18 C17 59.70(18) . . . . ? C15 C14 C18 Fe1 -59.41(18) . . . . ? C16 C17 C18 C14 -0.1(3) . . . . ? Fe1 C17 C18 C14 -59.58(17) . . . . ? C16 C17 C18 Fe1 59.51(18) . . . . ? C13 Fe1 C18 C14 -38.3(3) . . . . ? C15 Fe1 C18 C14 37.93(16) . . . . ? C10 Fe1 C18 C14 -115.17(16) . . . . ? C9 Fe1 C18 C14 -72.28(17) . . . . ? C11 Fe1 C18 C14 -157.47(15) . . . . ? C17 Fe1 C18 C14 119.0(2) . . . . ? C12 Fe1 C18 C14 167.8(2) . . . . ? C16 Fe1 C18 C14 81.79(17) . . . . ? C13 Fe1 C18 C17 -157.3(2) . . . . ? C15 Fe1 C18 C17 -81.08(17) . . . . ? C14 Fe1 C18 C17 -119.0(2) . . . . ? C10 Fe1 C18 C17 125.82(15) . . . . ? C9 Fe1 C18 C17 168.70(13) . . . . ? C11 Fe1 C18 C17 83.52(17) . . . . ? C12 Fe1 C18 C17 48.8(3) . . . . ? C16 Fe1 C18 C17 -37.22(15) . . . . ? C19 C19 C20 C21 -10(44) 2_655 . . . ? C19 C20 C21 C22 146(11) . . . . ? C19 C20 C21 C26 -32(11) . . . . ? C26 C21 C22 C23 0.3(3) . . . . ? C20 C21 C22 C23 -177.8(2) . . . . ? C21 C22 C23 C24 0.4(3) . . . . ? C22 C23 C24 C25 -0.9(3) . . . . ? C23 C24 C25 C26 0.6(3) . . . . ? C23 C24 C25 C27 178.81(19) . . . . ? C24 C25 C26 C21 0.1(3) . . . . ? C27 C25 C26 C21 -178.13(19) . . . . ? C22 C21 C26 C25 -0.5(3) . . . . ? C20 C21 C26 C25 177.6(2) . . . . ? C26 C25 C27 C31 4.5(3) . . . . ? C24 C25 C27 C31 -173.66(19) . . . . ? C26 C25 C27 C28 -174.02(19) . . . . ? C24 C25 C27 C28 7.8(3) . . . . ? C26 C25 C27 Fe2 -84.3(2) . . . . ? C24 C25 C27 Fe2 97.5(2) . . . . ? C32 Fe2 C27 C31 -124.67(15) . . . . ? C33 Fe2 C27 C31 -164.21(15) . . . . ? C34 Fe2 C27 C31 171.7(3) . . . . ? C36 Fe2 C27 C31 -83.10(17) . . . . ? C28 Fe2 C27 C31 118.23(18) . . . . ? C29 Fe2 C27 C31 80.80(14) . . . . ? C30 Fe2 C27 C31 37.58(13) . . . . ? C35 Fe2 C27 C31 -53.7(3) . . . . ? C31 Fe2 C27 C28 -118.23(18) . . . . ? C32 Fe2 C27 C28 117.10(15) . . . . ? C33 Fe2 C27 C28 77.56(16) . . . . ? C34 Fe2 C27 C28 53.5(4) . . . . ? C36 Fe2 C27 C28 158.67(15) . . . . ? C29 Fe2 C27 C28 -37.43(13) . . . . ? C30 Fe2 C27 C28 -80.65(14) . . . . ? C35 Fe2 C27 C28 -171.9(2) . . . . ? C31 Fe2 C27 C25 120.6(2) . . . . ? C32 Fe2 C27 C25 -4.1(2) . . . . ? C33 Fe2 C27 C25 -43.6(2) . . . . ? C34 Fe2 C27 C25 -67.7(4) . . . . ? C36 Fe2 C27 C25 37.5(2) . . . . ? C28 Fe2 C27 C25 -121.2(2) . . . . ? C29 Fe2 C27 C25 -158.6(2) . . . . ? C30 Fe2 C27 C25 158.2(2) . . . . ? C35 Fe2 C27 C25 66.9(3) . . . . ? C31 C27 C28 C29 0.0(2) . . . . ? C25 C27 C28 C29 178.79(19) . . . . ? Fe2 C27 C28 C29 59.37(15) . . . . ? C31 C27 C28 Fe2 -59.33(14) . . . . ? C25 C27 C28 Fe2 119.4(2) . . . . ? C31 Fe2 C28 C29 -80.98(14) . . . . ? C32 Fe2 C28 C29 161.00(14) . . . . ? C33 Fe2 C28 C29 118.71(14) . . . . ? C27 Fe2 C28 C29 -119.41(18) . . . . ? C34 Fe2 C28 C29 78.15(16) . . . . ? C36 Fe2 C28 C29 -165.4(2) . . . . ? C30 Fe2 C28 C29 -37.03(13) . . . . ? C35 Fe2 C28 C29 47.2(4) . . . . ? C31 Fe2 C28 C27 38.43(12) . . . . ? C32 Fe2 C28 C27 -79.59(15) . . . . ? C33 Fe2 C28 C27 -121.88(14) . . . . ? C34 Fe2 C28 C27 -162.44(13) . . . . ? C36 Fe2 C28 C27 -46.0(3) . . . . ? C29 Fe2 C28 C27 119.41(18) . . . . ? C30 Fe2 C28 C27 82.39(13) . . . . ? C35 Fe2 C28 C27 166.6(3) . . . . ? C27 C28 C29 C30 0.2(2) . . . . ? Fe2 C28 C29 C30 59.18(16) . . . . ? C27 C28 C29 Fe2 -58.95(14) . . . . ? C31 Fe2 C29 C30 -37.65(13) . . . . ? C32 Fe2 C29 C30 -162.4(2) . . . . ? C33 Fe2 C29 C30 160.23(14) . . . . ? C27 Fe2 C29 C30 -81.97(14) . . . . ? C34 Fe2 C29 C30 116.71(14) . . . . ? C36 Fe2 C29 C30 36.3(4) . . . . ? C28 Fe2 C29 C30 -119.91(18) . . . . ? C35 Fe2 C29 C30 74.52(16) . . . . ? C31 Fe2 C29 C28 82.26(14) . . . . ? C32 Fe2 C29 C28 -42.5(3) . . . . ? C33 Fe2 C29 C28 -79.86(15) . . . . ? C27 Fe2 C29 C28 37.94(12) . . . . ? C34 Fe2 C29 C28 -123.38(14) . . . . ? C36 Fe2 C29 C28 156.2(3) . . . . ? C30 Fe2 C29 C28 119.91(18) . . . . ? C35 Fe2 C29 C28 -165.57(13) . . . . ? C28 C29 C30 C31 -0.4(2) . . . . ? Fe2 C29 C30 C31 58.51(15) . . . . ? C28 C29 C30 Fe2 -58.93(15) . . . . ? C31 Fe2 C30 C29 119.6(2) . . . . ? C32 Fe2 C30 C29 155.5(3) . . . . ? C33 Fe2 C30 C29 -46.8(3) . . . . ? C27 Fe2 C30 C29 81.75(14) . . . . ? C34 Fe2 C30 C29 -83.43(16) . . . . ? C36 Fe2 C30 C29 -168.26(14) . . . . ? C28 Fe2 C30 C29 37.39(13) . . . . ? C35 Fe2 C30 C29 -126.16(14) . . . . ? C32 Fe2 C30 C31 35.9(4) . . . . ? C33 Fe2 C30 C31 -166.5(2) . . . . ? C27 Fe2 C30 C31 -37.89(14) . . . . ? C34 Fe2 C30 C31 156.92(15) . . . . ? C36 Fe2 C30 C31 72.09(18) . . . . ? C28 Fe2 C30 C31 -82.26(15) . . . . ? C29 Fe2 C30 C31 -119.6(2) . . . . ? C35 Fe2 C30 C31 114.19(15) . . . . ? C29 C30 C31 C27 0.4(2) . . . . ? Fe2 C30 C31 C27 59.58(15) . . . . ? C29 C30 C31 Fe2 -59.14(15) . . . . ? C28 C27 C31 C30 -0.3(2) . . . . ? C25 C27 C31 C30 -179.05(19) . . . . ? Fe2 C27 C31 C30 -59.94(15) . . . . ? C28 C27 C31 Fe2 59.64(14) . . . . ? C25 C27 C31 Fe2 -119.1(2) . . . . ? C32 Fe2 C31 C30 -167.50(15) . . . . ? C33 Fe2 C31 C30 163.5(3) . . . . ? C27 Fe2 C31 C30 119.4(2) . . . . ? C34 Fe2 C31 C30 -54.5(3) . . . . ? C36 Fe2 C31 C30 -126.71(16) . . . . ? C28 Fe2 C31 C30 80.89(15) . . . . ? C29 Fe2 C31 C30 37.13(15) . . . . ? C35 Fe2 C31 C30 -84.97(17) . . . . ? C32 Fe2 C31 C27 73.13(17) . . . . ? C33 Fe2 C31 C27 44.1(4) . . . . ? C34 Fe2 C31 C27 -173.9(2) . . . . ? C36 Fe2 C31 C27 113.93(15) . . . . ? C28 Fe2 C31 C27 -38.47(13) . . . . ? C29 Fe2 C31 C27 -82.24(14) . . . . ? C30 Fe2 C31 C27 -119.4(2) . . . . ? C35 Fe2 C31 C27 155.67(14) . . . . ? C31 Fe2 C32 C33 -165.94(15) . . . . ? C27 Fe2 C32 C33 -125.24(15) . . . . ? C34 Fe2 C32 C33 37.86(15) . . . . ? C36 Fe2 C32 C33 119.2(2) . . . . ? C28 Fe2 C32 C33 -83.11(17) . . . . ? C29 Fe2 C32 C33 -52.9(3) . . . . ? C30 Fe2 C32 C33 166.6(3) . . . . ? C35 Fe2 C32 C33 81.53(16) . . . . ? C31 Fe2 C32 C36 74.82(18) . . . . ? C33 Fe2 C32 C36 -119.2(2) . . . . ? C27 Fe2 C32 C36 115.52(15) . . . . ? C34 Fe2 C32 C36 -81.37(16) . . . . ? C28 Fe2 C32 C36 157.65(14) . . . . ? C29 Fe2 C32 C36 -172.12(19) . . . . ? C30 Fe2 C32 C36 47.4(4) . . . . ? C35 Fe2 C32 C36 -37.71(15) . . . . ? C36 C32 C33 C34 0.0(3) . . . . ? Fe2 C32 C33 C34 -59.79(16) . . . . ? C36 C32 C33 Fe2 59.74(17) . . . . ? C31 Fe2 C33 C32 38.5(4) . . . . ? C27 Fe2 C33 C32 72.05(19) . . . . ? C34 Fe2 C33 C32 -118.8(2) . . . . ? C36 Fe2 C33 C32 -37.68(16) . . . . ? C28 Fe2 C33 C32 114.48(16) . . . . ? C29 Fe2 C33 C32 156.72(16) . . . . ? C30 Fe2 C33 C32 -169.6(2) . . . . ? C35 Fe2 C33 C32 -81.46(17) . . . . ? C31 Fe2 C33 C34 157.3(3) . . . . ? C32 Fe2 C33 C34 118.8(2) . . . . ? C27 Fe2 C33 C34 -169.11(14) . . . . ? C36 Fe2 C33 C34 81.15(17) . . . . ? C28 Fe2 C33 C34 -126.69(15) . . . . ? C29 Fe2 C33 C34 -84.45(17) . . . . ? C30 Fe2 C33 C34 -50.8(3) . . . . ? C35 Fe2 C33 C34 37.38(16) . . . . ? C32 C33 C34 C35 0.0(3) . . . . ? Fe2 C33 C34 C35 -59.70(16) . . . . ? C32 C33 C34 Fe2 59.73(16) . . . . ? C31 Fe2 C34 C35 -42.6(3) . . . . ? C32 Fe2 C34 C35 81.81(18) . . . . ? C33 Fe2 C34 C35 119.5(2) . . . . ? C27 Fe2 C34 C35 150.9(3) . . . . ? C36 Fe2 C34 C35 37.91(17) . . . . ? C28 Fe2 C34 C35 -167.67(15) . . . . ? C29 Fe2 C34 C35 -124.87(17) . . . . ? C30 Fe2 C34 C35 -81.72(19) . . . . ? C31 Fe2 C34 C33 -162.1(2) . . . . ? C32 Fe2 C34 C33 -37.68(16) . . . . ? C27 Fe2 C34 C33 31.4(4) . . . . ? C36 Fe2 C34 C33 -81.58(18) . . . . ? C28 Fe2 C34 C33 72.84(19) . . . . ? C29 Fe2 C34 C33 115.64(16) . . . . ? C30 Fe2 C34 C33 158.79(16) . . . . ? C35 Fe2 C34 C33 -119.5(2) . . . . ? C33 C34 C35 C36 0.0(3) . . . . ? Fe2 C34 C35 C36 -59.39(17) . . . . ? C33 C34 C35 Fe2 59.40(16) . . . . ? C31 Fe2 C35 C34 161.47(15) . . . . ? C32 Fe2 C35 C34 -81.00(17) . . . . ? C33 Fe2 C35 C34 -37.48(16) . . . . ? C27 Fe2 C35 C34 -160.71(19) . . . . ? C36 Fe2 C35 C34 -118.7(2) . . . . ? C28 Fe2 C35 C34 39.5(4) . . . . ? C29 Fe2 C35 C34 76.64(19) . . . . ? C30 Fe2 C35 C34 117.88(16) . . . . ? C31 Fe2 C35 C36 -79.79(19) . . . . ? C32 Fe2 C35 C36 37.75(17) . . . . ? C33 Fe2 C35 C36 81.27(18) . . . . ? C27 Fe2 C35 C36 -42.0(3) . . . . ? C34 Fe2 C35 C36 118.7(2) . . . . ? C28 Fe2 C35 C36 158.2(3) . . . . ? C29 Fe2 C35 C36 -164.61(16) . . . . ? C30 Fe2 C35 C36 -123.38(17) . . . . ? C33 C32 C36 C35 0.0(3) . . . . ? Fe2 C32 C36 C35 59.78(17) . . . . ? C33 C32 C36 Fe2 -59.74(16) . . . . ? C34 C35 C36 C32 0.0(3) . . . . ? Fe2 C35 C36 C32 -59.43(17) . . . . ? C34 C35 C36 Fe2 59.40(17) . . . . ? C31 Fe2 C36 C32 -123.42(15) . . . . ? C33 Fe2 C36 C32 37.44(15) . . . . ? C27 Fe2 C36 C32 -80.52(17) . . . . ? C34 Fe2 C36 C32 81.24(16) . . . . ? C28 Fe2 C36 C32 -48.1(3) . . . . ? C29 Fe2 C36 C32 168.0(3) . . . . ? C30 Fe2 C36 C32 -163.80(14) . . . . ? C35 Fe2 C36 C32 119.0(2) . . . . ? C31 Fe2 C36 C35 117.55(16) . . . . ? C32 Fe2 C36 C35 -119.0(2) . . . . ? C33 Fe2 C36 C35 -81.58(17) . . . . ? C27 Fe2 C36 C35 160.45(15) . . . . ? C34 Fe2 C36 C35 -37.79(16) . . . . ? C28 Fe2 C36 C35 -167.11(19) . . . . ? C29 Fe2 C36 C35 49.0(4) . . . . ? C30 Fe2 C36 C35 77.17(18) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.303 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.062 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.018 0.241 0.878 164 10 ' ' 2 -0.042 0.759 0.122 164 10 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 942658' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_rm053 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H22 Fe2' _chemical_formula_weight 470.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.6452(3) _cell_length_b 10.2825(2) _cell_length_c 14.8003(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.902(2) _cell_angle_gamma 90.00 _cell_volume 2067.90(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8946 _cell_measurement_theta_min 2.9610 _cell_measurement_theta_max 32.3748 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 1.415 _exptl_absorpt_correction_T_min 0.7367 _exptl_absorpt_correction_T_max 0.8374 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Micro-Focus (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION SUPER NOVA' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16462 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0212 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3642 _reflns_number_gt 3247 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.0713P)^2^+8.9558P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3642 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1592 _refine_ls_wR_factor_gt 0.1534 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.87128(5) 0.48266(7) 0.67323(5) 0.0321(2) Uani 1 1 d . . . Fe2 Fe 0.29377(4) 0.53565(6) 0.88590(4) 0.0225(2) Uani 1 1 d . . . C1 C 0.6816(4) 0.3573(5) 0.6737(4) 0.0438(12) Uani 1 1 d . . . C2 C 0.6164(4) 0.4180(5) 0.7088(4) 0.0422(12) Uani 1 1 d . . . H2 H 0.6413 0.4679 0.7669 0.051 Uiso 1 1 calc R . . C3 C 0.5129(4) 0.4060(5) 0.6585(4) 0.0385(11) Uani 1 1 d . . . C4 C 0.4751(4) 0.3247(5) 0.5780(4) 0.0382(11) Uani 1 1 d . . . H4 H 0.4065 0.3072 0.5504 0.046 Uiso 1 1 calc R . . C5 C 0.5379(5) 0.2694(6) 0.5383(5) 0.0569(16) Uani 1 1 d . . . H5 H 0.5121 0.2234 0.4784 0.068 Uiso 1 1 calc R . . C6 C 0.6421(5) 0.2823(6) 0.5883(5) 0.0564(15) Uani 1 1 d . . . H6 H 0.6853 0.2395 0.5634 0.068 Uiso 1 1 calc R . . C7 C 0.7901(4) 0.3733(5) 0.7244(4) 0.0457(13) Uani 1 1 d . . . C8 C 0.8387(4) 0.4728(6) 0.7932(4) 0.0485(14) Uani 1 1 d . . . H8 H 0.8063 0.5350 0.8181 0.058 Uiso 1 1 calc R . . C9 C 0.9437(4) 0.4653(6) 0.8193(4) 0.0451(13) Uani 1 1 d . . . H9 H 0.9920 0.5222 0.8613 0.054 Uiso 1 1 calc R . . C10 C 0.9603(5) 0.3532(7) 0.7684(4) 0.0609(19) Uani 1 1 d . . . H10 H 1.0226 0.3225 0.7716 0.073 Uiso 1 1 calc R . . C11 C 0.8683(5) 0.2970(5) 0.7129(4) 0.0507(14) Uani 1 1 d . . . H11 H 0.8592 0.2209 0.6741 0.061 Uiso 1 1 calc R . . C12 C 0.8042(5) 0.6451(6) 0.5982(4) 0.0575(16) Uani 1 1 d . . . H12 H 0.7592 0.6975 0.6146 0.069 Uiso 1 1 calc R . . C13 C 0.9030(5) 0.6616(6) 0.6292(4) 0.0523(15) Uani 1 1 d . . . H13 H 0.9391 0.7288 0.6715 0.063 Uiso 1 1 calc R . . C14 C 0.9451(5) 0.5618(6) 0.5883(5) 0.0579(16) Uani 1 1 d . . . H14 H 1.0126 0.5507 0.5986 0.070 Uiso 1 1 calc R . . C15 C 0.8682(5) 0.4863(7) 0.5319(4) 0.0582(16) Uani 1 1 d . . . H15 H 0.8744 0.4129 0.4957 0.070 Uiso 1 1 calc R . . C16 C 0.7805(5) 0.5310(7) 0.5345(4) 0.0599(18) Uani 1 1 d . . . H16 H 0.7170 0.4948 0.5014 0.072 Uiso 1 1 calc R . . C17 C 0.4504(3) 0.4683(4) 0.7000(3) 0.0311(10) Uani 1 1 d . . . C18 C 0.3984(3) 0.5197(4) 0.7351(3) 0.0284(9) Uani 1 1 d . . . C19 C 0.3341(3) 0.5858(4) 0.7718(3) 0.0260(9) Uani 1 1 d . . . C20 C 0.2294(3) 0.5671(5) 0.7391(3) 0.0294(10) Uani 1 1 d . . . H20 H 0.1920 0.5055 0.6921 0.035 Uiso 1 1 calc R . . C21 C 0.1919(4) 0.6564(5) 0.7893(3) 0.0334(10) Uani 1 1 d . . . H21 H 0.1247 0.6656 0.7814 0.040 Uiso 1 1 calc R . . C22 C 0.2717(4) 0.7298(4) 0.8535(3) 0.0335(10) Uani 1 1 d . . . H22 H 0.2670 0.7966 0.8958 0.040 Uiso 1 1 calc R . . C23 C 0.3597(3) 0.6871(4) 0.8441(3) 0.0296(9) Uani 1 1 d . . . H23 H 0.4241 0.7194 0.8791 0.036 Uiso 1 1 calc R . . C24 C 0.3668(4) 0.3696(5) 0.9490(3) 0.0355(11) Uani 1 1 d . . . H24 H 0.4141 0.3246 0.9310 0.043 Uiso 1 1 calc R . . C25 C 0.2634(4) 0.3484(5) 0.9097(3) 0.0355(11) Uani 1 1 d . . . H25 H 0.2295 0.2867 0.8610 0.043 Uiso 1 1 calc R . . C26 C 0.2201(3) 0.4357(5) 0.9560(3) 0.0343(10) Uani 1 1 d . . . H26 H 0.1518 0.4428 0.9439 0.041 Uiso 1 1 calc R . . C27 C 0.2959(4) 0.5104(5) 1.0233(3) 0.0349(11) Uani 1 1 d . . . H27 H 0.2876 0.5768 1.0642 0.042 Uiso 1 1 calc R . . C28 C 0.3869(4) 0.4694(5) 1.0194(3) 0.0368(11) Uani 1 1 d . . . H28 H 0.4500 0.5030 1.0574 0.044 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 0.0275(4) 0.0335(4) 0.0313(4) -0.0018(3) 0.0062(3) 0.0069(3) Fe2 0.0253(4) 0.0237(4) 0.0189(3) 0.0013(2) 0.0086(3) 0.0002(2) C1 0.052(3) 0.042(3) 0.042(3) 0.001(2) 0.023(3) 0.002(2) C2 0.056(3) 0.042(3) 0.034(3) 0.003(2) 0.023(2) 0.003(2) C3 0.034(3) 0.042(3) 0.044(3) -0.013(2) 0.020(2) -0.004(2) C4 0.036(3) 0.042(3) 0.037(3) -0.007(2) 0.014(2) -0.002(2) C5 0.069(4) 0.052(3) 0.062(4) -0.030(3) 0.038(3) -0.015(3) C6 0.057(4) 0.060(4) 0.063(4) -0.018(3) 0.035(3) -0.001(3) C7 0.054(3) 0.047(3) 0.046(3) 0.001(2) 0.030(3) 0.002(3) C8 0.053(3) 0.058(4) 0.046(3) -0.010(3) 0.032(3) -0.007(3) C9 0.052(3) 0.055(3) 0.028(3) 0.010(2) 0.013(2) 0.017(3) C10 0.070(4) 0.080(4) 0.033(3) 0.024(3) 0.020(3) 0.052(4) C11 0.077(4) 0.036(3) 0.048(3) 0.010(2) 0.033(3) 0.011(3) C12 0.072(4) 0.036(3) 0.051(3) 0.002(3) 0.008(3) 0.013(3) C13 0.079(4) 0.041(3) 0.036(3) 0.001(2) 0.019(3) 0.003(3) C14 0.073(4) 0.059(4) 0.052(4) 0.006(3) 0.034(3) 0.003(3) C15 0.074(4) 0.065(4) 0.043(3) 0.014(3) 0.031(3) 0.003(3) C16 0.053(4) 0.087(5) 0.030(3) 0.009(3) 0.004(3) -0.019(3) C17 0.031(2) 0.035(2) 0.027(2) -0.0003(18) 0.011(2) 0.0020(19) C18 0.032(2) 0.030(2) 0.022(2) 0.0044(17) 0.0096(19) 0.0017(18) C19 0.032(2) 0.027(2) 0.020(2) 0.0067(17) 0.0117(18) 0.0053(18) C20 0.033(2) 0.036(2) 0.018(2) 0.0050(18) 0.0084(18) 0.0058(19) C21 0.037(3) 0.038(3) 0.027(2) 0.0094(19) 0.015(2) 0.014(2) C22 0.051(3) 0.027(2) 0.028(2) 0.0049(18) 0.021(2) 0.010(2) C23 0.038(2) 0.026(2) 0.025(2) 0.0049(18) 0.0130(19) -0.0021(19) C24 0.040(3) 0.032(2) 0.041(3) 0.015(2) 0.021(2) 0.008(2) C25 0.047(3) 0.027(2) 0.031(2) 0.0021(19) 0.011(2) -0.009(2) C26 0.030(2) 0.041(3) 0.034(2) 0.010(2) 0.015(2) -0.002(2) C27 0.054(3) 0.033(2) 0.022(2) 0.0017(18) 0.020(2) -0.006(2) C28 0.033(2) 0.043(3) 0.026(2) 0.012(2) 0.002(2) -0.010(2) _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 C7 1.981(5) . ? Fe1 C11 2.003(5) . ? Fe1 C8 2.005(5) . ? Fe1 C10 2.021(5) . ? Fe1 C9 2.030(5) . ? Fe1 C12 2.043(6) . ? Fe1 C16 2.048(6) . ? Fe1 C13 2.062(6) . ? Fe1 C15 2.075(6) . ? Fe1 C14 2.103(6) . ? Fe2 C26 2.033(4) . ? Fe2 C25 2.035(5) . ? Fe2 C27 2.039(4) . ? Fe2 C20 2.045(4) . ? Fe2 C24 2.046(5) . ? Fe2 C23 2.046(4) . ? Fe2 C22 2.050(5) . ? Fe2 C19 2.052(4) . ? Fe2 C28 2.054(5) . ? Fe2 C21 2.054(4) . ? C1 C2 1.392(7) . ? C1 C6 1.408(8) . ? C1 C7 1.492(8) . ? C2 C3 1.423(7) . ? C2 H2 0.9500 . ? C3 C4 1.389(7) . ? C3 C17 1.430(6) . ? C4 C5 1.386(7) . ? C4 H4 0.9500 . ? C5 C6 1.432(9) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.431(8) . ? C7 C11 1.450(8) . ? C8 C9 1.440(8) . ? C8 H8 0.9500 . ? C9 C10 1.446(8) . ? C9 H9 0.9500 . ? C10 C11 1.413(9) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.356(9) . ? C12 C16 1.464(9) . ? C12 H12 0.9500 . ? C13 C14 1.441(8) . ? C13 H13 0.9500 . ? C14 C15 1.366(10) . ? C14 H14 0.9500 . ? C15 C16 1.378(9) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.194(7) . ? C18 C19 1.423(6) . ? C19 C23 1.438(6) . ? C19 C20 1.439(6) . ? C20 C21 1.415(6) . ? C20 H20 0.9500 . ? C21 C22 1.418(7) . ? C21 H21 0.9500 . ? C22 C23 1.418(6) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C28 1.413(7) . ? C24 C25 1.421(7) . ? C24 H24 0.9500 . ? C25 C26 1.416(7) . ? C25 H25 0.9500 . ? C26 C27 1.411(7) . ? C26 H26 0.9500 . ? C27 C28 1.419(7) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? 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 C7 Fe1 C11 42.7(2) . . ? C7 Fe1 C8 42.1(2) . . ? C11 Fe1 C8 69.7(2) . . ? C7 Fe1 C10 71.5(3) . . ? C11 Fe1 C10 41.1(3) . . ? C8 Fe1 C10 69.8(2) . . ? C7 Fe1 C9 72.1(2) . . ? C11 Fe1 C9 70.3(2) . . ? C8 Fe1 C9 41.8(2) . . ? C10 Fe1 C9 41.8(2) . . ? C7 Fe1 C12 115.9(3) . . ? C11 Fe1 C12 151.7(3) . . ? C8 Fe1 C12 107.3(3) . . ? C10 Fe1 C12 166.3(3) . . ? C9 Fe1 C12 127.2(2) . . ? C7 Fe1 C16 105.3(2) . . ? C11 Fe1 C16 116.6(3) . . ? C8 Fe1 C16 128.3(3) . . ? C10 Fe1 C16 150.1(3) . . ? C9 Fe1 C16 167.2(3) . . ? C12 Fe1 C16 41.9(3) . . ? C7 Fe1 C13 149.9(2) . . ? C11 Fe1 C13 167.3(3) . . ? C8 Fe1 C13 118.8(2) . . ? C10 Fe1 C13 130.2(3) . . ? C9 Fe1 C13 109.0(2) . . ? C12 Fe1 C13 38.6(3) . . ? C16 Fe1 C13 66.8(2) . . ? C7 Fe1 C15 127.2(3) . . ? C11 Fe1 C15 108.6(3) . . ? C8 Fe1 C15 166.0(3) . . ? C10 Fe1 C15 118.7(2) . . ? C9 Fe1 C15 151.8(3) . . ? C12 Fe1 C15 67.2(3) . . ? C16 Fe1 C15 39.0(3) . . ? C13 Fe1 C15 65.7(2) . . ? C7 Fe1 C14 164.5(2) . . ? C11 Fe1 C14 128.1(2) . . ? C8 Fe1 C14 153.3(3) . . ? C10 Fe1 C14 109.2(3) . . ? C9 Fe1 C14 119.3(3) . . ? C12 Fe1 C14 67.0(3) . . ? C16 Fe1 C14 66.0(3) . . ? C13 Fe1 C14 40.5(2) . . ? C15 Fe1 C14 38.2(3) . . ? C26 Fe2 C25 40.7(2) . . ? C26 Fe2 C27 40.6(2) . . ? C25 Fe2 C27 68.31(19) . . ? C26 Fe2 C20 119.98(19) . . ? C25 Fe2 C20 106.81(19) . . ? C27 Fe2 C20 155.4(2) . . ? C26 Fe2 C24 68.41(19) . . ? C25 Fe2 C24 40.76(19) . . ? C27 Fe2 C24 68.1(2) . . ? C20 Fe2 C24 124.89(19) . . ? C26 Fe2 C23 159.97(19) . . ? C25 Fe2 C23 158.4(2) . . ? C27 Fe2 C23 124.42(19) . . ? C20 Fe2 C23 68.96(19) . . ? C24 Fe2 C23 123.20(19) . . ? C26 Fe2 C22 122.96(19) . . ? C25 Fe2 C22 159.3(2) . . ? C27 Fe2 C22 107.44(19) . . ? C20 Fe2 C22 68.14(19) . . ? C24 Fe2 C22 158.3(2) . . ? C23 Fe2 C22 40.50(18) . . ? C26 Fe2 C19 156.6(2) . . ? C25 Fe2 C19 121.90(19) . . ? C27 Fe2 C19 161.9(2) . . ? C20 Fe2 C19 41.11(17) . . ? C24 Fe2 C19 108.87(18) . . ? C23 Fe2 C19 41.08(17) . . ? C22 Fe2 C19 68.37(17) . . ? C26 Fe2 C28 68.25(19) . . ? C25 Fe2 C28 68.24(19) . . ? C27 Fe2 C28 40.6(2) . . ? C20 Fe2 C28 162.1(2) . . ? C24 Fe2 C28 40.3(2) . . ? C23 Fe2 C28 108.95(19) . . ? C22 Fe2 C28 122.6(2) . . ? C19 Fe2 C28 125.71(19) . . ? C26 Fe2 C21 105.91(19) . . ? C25 Fe2 C21 122.9(2) . . ? C27 Fe2 C21 120.52(19) . . ? C20 Fe2 C21 40.38(18) . . ? C24 Fe2 C21 160.4(2) . . ? C23 Fe2 C21 68.43(19) . . ? C22 Fe2 C21 40.4(2) . . ? C19 Fe2 C21 68.47(17) . . ? C28 Fe2 C21 156.8(2) . . ? C2 C1 C6 118.1(5) . . ? C2 C1 C7 120.9(5) . . ? C6 C1 C7 121.0(5) . . ? C1 C2 C3 120.7(5) . . ? C1 C2 H2 119.6 . . ? C3 C2 H2 119.6 . . ? C4 C3 C2 120.4(4) . . ? C4 C3 C17 121.6(4) . . ? C2 C3 C17 117.7(4) . . ? C5 C4 C3 119.7(5) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 119.4(5) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C1 C6 C5 121.1(5) . . ? C1 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C8 C7 C11 105.3(5) . . ? C8 C7 C1 126.2(5) . . ? C11 C7 C1 128.5(5) . . ? C8 C7 Fe1 69.9(3) . . ? C11 C7 Fe1 69.4(3) . . ? C1 C7 Fe1 123.3(4) . . ? C7 C8 C9 110.5(5) . . ? C7 C8 Fe1 68.1(3) . . ? C9 C8 Fe1 70.0(3) . . ? C7 C8 H8 124.7 . . ? C9 C8 H8 124.7 . . ? Fe1 C8 H8 128.9 . . ? C8 C9 C10 105.8(5) . . ? C8 C9 Fe1 68.2(3) . . ? C10 C9 Fe1 68.7(3) . . ? C8 C9 H9 127.1 . . ? C10 C9 H9 127.1 . . ? Fe1 C9 H9 127.5 . . ? C11 C10 C9 108.6(5) . . ? C11 C10 Fe1 68.8(3) . . ? C9 C10 Fe1 69.4(3) . . ? C11 C10 H10 125.7 . . ? C9 C10 H10 125.7 . . ? Fe1 C10 H10 127.7 . . ? C10 C11 C7 109.5(5) . . ? C10 C11 Fe1 70.1(3) . . ? C7 C11 Fe1 67.9(3) . . ? C10 C11 H11 125.2 . . ? C7 C11 H11 125.2 . . ? Fe1 C11 H11 128.4 . . ? C13 C12 C16 106.6(6) . . ? C13 C12 Fe1 71.5(3) . . ? C16 C12 Fe1 69.2(3) . . ? C13 C12 H12 126.7 . . ? C16 C12 H12 126.7 . . ? Fe1 C12 H12 124.2 . . ? C12 C13 C14 109.8(6) . . ? C12 C13 Fe1 70.0(4) . . ? C14 C13 Fe1 71.3(3) . . ? C12 C13 H13 125.1 . . ? C14 C13 H13 125.1 . . ? Fe1 C13 H13 125.2 . . ? C15 C14 C13 106.1(6) . . ? C15 C14 Fe1 69.8(4) . . ? C13 C14 Fe1 68.3(3) . . ? C15 C14 H14 127.0 . . ? C13 C14 H14 127.0 . . ? Fe1 C14 H14 126.5 . . ? C14 C15 C16 111.0(6) . . ? C14 C15 Fe1 72.0(4) . . ? C16 C15 Fe1 69.4(3) . . ? C14 C15 H15 124.5 . . ? C16 C15 H15 124.5 . . ? Fe1 C15 H15 125.7 . . ? C15 C16 C12 106.5(6) . . ? C15 C16 Fe1 71.5(4) . . ? C12 C16 Fe1 68.8(3) . . ? C15 C16 H16 126.7 . . ? C12 C16 H16 126.7 . . ? Fe1 C16 H16 124.5 . . ? C18 C17 C3 179.6(5) . . ? C17 C18 C19 176.5(5) . . ? C18 C19 C23 127.1(4) . . ? C18 C19 C20 125.6(4) . . ? C23 C19 C20 107.3(4) . . ? C18 C19 Fe2 128.9(3) . . ? C23 C19 Fe2 69.2(2) . . ? C20 C19 Fe2 69.2(2) . . ? C21 C20 C19 108.1(4) . . ? C21 C20 Fe2 70.2(2) . . ? C19 C20 Fe2 69.7(2) . . ? C21 C20 H20 125.9 . . ? C19 C20 H20 125.9 . . ? Fe2 C20 H20 125.8 . . ? C20 C21 C22 108.2(4) . . ? C20 C21 Fe2 69.5(2) . . ? C22 C21 Fe2 69.6(3) . . ? C20 C21 H21 125.9 . . ? C22 C21 H21 125.9 . . ? Fe2 C21 H21 126.6 . . ? C23 C22 C21 108.8(4) . . ? C23 C22 Fe2 69.6(3) . . ? C21 C22 Fe2 69.9(3) . . ? C23 C22 H22 125.6 . . ? C21 C22 H22 125.6 . . ? Fe2 C22 H22 126.4 . . ? C22 C23 C19 107.6(4) . . ? C22 C23 Fe2 69.9(3) . . ? C19 C23 Fe2 69.7(2) . . ? C22 C23 H23 126.2 . . ? C19 C23 H23 126.2 . . ? Fe2 C23 H23 125.8 . . ? C28 C24 C25 108.1(4) . . ? C28 C24 Fe2 70.2(3) . . ? C25 C24 Fe2 69.2(3) . . ? C28 C24 H24 126.0 . . ? C25 C24 H24 126.0 . . ? Fe2 C24 H24 126.2 . . ? C26 C25 C24 107.8(4) . . ? C26 C25 Fe2 69.6(3) . . ? C24 C25 Fe2 70.0(3) . . ? C26 C25 H25 126.1 . . ? C24 C25 H25 126.1 . . ? Fe2 C25 H25 125.9 . . ? C27 C26 C25 108.0(4) . . ? C27 C26 Fe2 69.9(3) . . ? C25 C26 Fe2 69.7(3) . . ? C27 C26 H26 126.0 . . ? C25 C26 H26 126.0 . . ? Fe2 C26 H26 125.9 . . ? C26 C27 C28 108.2(4) . . ? C26 C27 Fe2 69.5(3) . . ? C28 C27 Fe2 70.3(3) . . ? C26 C27 H27 125.9 . . ? C28 C27 H27 125.9 . . ? Fe2 C27 H27 125.9 . . ? C24 C28 C27 107.8(4) . . ? C24 C28 Fe2 69.5(3) . . ? C27 C28 Fe2 69.2(3) . . ? C24 C28 H28 126.1 . . ? C27 C28 H28 126.1 . . ? Fe2 C28 H28 126.8 . . ? 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 C6 C1 C2 C3 -1.1(8) . . . . ? C7 C1 C2 C3 177.9(5) . . . . ? C1 C2 C3 C4 5.4(8) . . . . ? C1 C2 C3 C17 178.5(5) . . . . ? C2 C3 C4 C5 -9.1(8) . . . . ? C17 C3 C4 C5 178.1(5) . . . . ? C3 C4 C5 C6 8.5(9) . . . . ? C2 C1 C6 C5 0.5(9) . . . . ? C7 C1 C6 C5 -178.5(6) . . . . ? C4 C5 C6 C1 -4.2(10) . . . . ? C2 C1 C7 C8 -17.9(8) . . . . ? C6 C1 C7 C8 161.1(6) . . . . ? C2 C1 C7 C11 164.7(5) . . . . ? C6 C1 C7 C11 -16.3(9) . . . . ? C2 C1 C7 Fe1 -106.1(5) . . . . ? C6 C1 C7 Fe1 72.9(7) . . . . ? C11 Fe1 C7 C8 116.0(5) . . . . ? C10 Fe1 C7 C8 80.0(4) . . . . ? C9 Fe1 C7 C8 35.9(3) . . . . ? C12 Fe1 C7 C8 -87.5(4) . . . . ? C16 Fe1 C7 C8 -131.1(4) . . . . ? C13 Fe1 C7 C8 -61.3(6) . . . . ? C15 Fe1 C7 C8 -167.5(4) . . . . ? C14 Fe1 C7 C8 175.4(9) . . . . ? C8 Fe1 C7 C11 -116.0(5) . . . . ? C10 Fe1 C7 C11 -36.0(3) . . . . ? C9 Fe1 C7 C11 -80.1(4) . . . . ? C12 Fe1 C7 C11 156.5(3) . . . . ? C16 Fe1 C7 C11 112.9(4) . . . . ? C13 Fe1 C7 C11 -177.3(4) . . . . ? C15 Fe1 C7 C11 76.5(4) . . . . ? C14 Fe1 C7 C11 59.4(10) . . . . ? C11 Fe1 C7 C1 -123.3(6) . . . . ? C8 Fe1 C7 C1 120.8(6) . . . . ? C10 Fe1 C7 C1 -159.2(5) . . . . ? C9 Fe1 C7 C1 156.6(5) . . . . ? C12 Fe1 C7 C1 33.2(5) . . . . ? C16 Fe1 C7 C1 -10.3(5) . . . . ? C13 Fe1 C7 C1 59.5(7) . . . . ? C15 Fe1 C7 C1 -46.8(6) . . . . ? C14 Fe1 C7 C1 -63.8(11) . . . . ? C11 C7 C8 C9 3.8(6) . . . . ? C1 C7 C8 C9 -174.1(5) . . . . ? Fe1 C7 C8 C9 -57.0(4) . . . . ? C11 C7 C8 Fe1 60.8(4) . . . . ? C1 C7 C8 Fe1 -117.1(5) . . . . ? C11 Fe1 C8 C7 -40.5(4) . . . . ? C10 Fe1 C8 C7 -84.5(4) . . . . ? C9 Fe1 C8 C7 -123.3(5) . . . . ? C12 Fe1 C8 C7 109.7(4) . . . . ? C16 Fe1 C8 C7 68.0(5) . . . . ? C13 Fe1 C8 C7 149.9(3) . . . . ? C15 Fe1 C8 C7 45.0(12) . . . . ? C14 Fe1 C8 C7 -177.3(5) . . . . ? C7 Fe1 C8 C9 123.3(5) . . . . ? C11 Fe1 C8 C9 82.8(4) . . . . ? C10 Fe1 C8 C9 38.8(4) . . . . ? C12 Fe1 C8 C9 -127.0(4) . . . . ? C16 Fe1 C8 C9 -168.7(4) . . . . ? C13 Fe1 C8 C9 -86.7(4) . . . . ? C15 Fe1 C8 C9 168.3(10) . . . . ? C14 Fe1 C8 C9 -54.0(7) . . . . ? C7 C8 C9 C10 -2.8(6) . . . . ? Fe1 C8 C9 C10 -58.7(4) . . . . ? C7 C8 C9 Fe1 55.9(4) . . . . ? C7 Fe1 C9 C8 -36.1(3) . . . . ? C11 Fe1 C9 C8 -81.2(4) . . . . ? C10 Fe1 C9 C8 -118.1(5) . . . . ? C12 Fe1 C9 C8 73.2(5) . . . . ? C16 Fe1 C9 C8 43.9(12) . . . . ? C13 Fe1 C9 C8 112.2(4) . . . . ? C15 Fe1 C9 C8 -174.0(5) . . . . ? C14 Fe1 C9 C8 155.4(3) . . . . ? C7 Fe1 C9 C10 82.0(4) . . . . ? C11 Fe1 C9 C10 36.8(4) . . . . ? C8 Fe1 C9 C10 118.1(5) . . . . ? C12 Fe1 C9 C10 -168.7(4) . . . . ? C16 Fe1 C9 C10 161.9(10) . . . . ? C13 Fe1 C9 C10 -129.7(4) . . . . ? C15 Fe1 C9 C10 -55.9(7) . . . . ? C14 Fe1 C9 C10 -86.5(4) . . . . ? C8 C9 C10 C11 0.7(6) . . . . ? Fe1 C9 C10 C11 -57.6(4) . . . . ? C8 C9 C10 Fe1 58.3(4) . . . . ? C7 Fe1 C10 C11 37.3(3) . . . . ? C8 Fe1 C10 C11 82.0(4) . . . . ? C9 Fe1 C10 C11 120.8(5) . . . . ? C12 Fe1 C10 C11 162.1(10) . . . . ? C16 Fe1 C10 C11 -51.2(6) . . . . ? C13 Fe1 C10 C11 -166.9(3) . . . . ? C15 Fe1 C10 C11 -85.7(4) . . . . ? C14 Fe1 C10 C11 -126.4(4) . . . . ? C7 Fe1 C10 C9 -83.5(4) . . . . ? C11 Fe1 C10 C9 -120.8(5) . . . . ? C8 Fe1 C10 C9 -38.8(4) . . . . ? C12 Fe1 C10 C9 41.3(13) . . . . ? C16 Fe1 C10 C9 -172.1(5) . . . . ? C13 Fe1 C10 C9 72.3(4) . . . . ? C15 Fe1 C10 C9 153.5(4) . . . . ? C14 Fe1 C10 C9 112.8(4) . . . . ? C9 C10 C11 C7 1.6(6) . . . . ? Fe1 C10 C11 C7 -56.4(4) . . . . ? C9 C10 C11 Fe1 58.0(4) . . . . ? C8 C7 C11 C10 -3.3(6) . . . . ? C1 C7 C11 C10 174.6(5) . . . . ? Fe1 C7 C11 C10 57.7(4) . . . . ? C8 C7 C11 Fe1 -61.0(4) . . . . ? C1 C7 C11 Fe1 116.8(6) . . . . ? C7 Fe1 C11 C10 -122.1(5) . . . . ? C8 Fe1 C11 C10 -82.1(4) . . . . ? C9 Fe1 C11 C10 -37.5(3) . . . . ? C12 Fe1 C11 C10 -171.2(5) . . . . ? C16 Fe1 C11 C10 154.2(3) . . . . ? C13 Fe1 C11 C10 51.7(12) . . . . ? C15 Fe1 C11 C10 112.7(4) . . . . ? C14 Fe1 C11 C10 74.9(4) . . . . ? C8 Fe1 C11 C7 40.0(3) . . . . ? C10 Fe1 C11 C7 122.1(5) . . . . ? C9 Fe1 C11 C7 84.6(4) . . . . ? C12 Fe1 C11 C7 -49.1(6) . . . . ? C16 Fe1 C11 C7 -83.7(4) . . . . ? C13 Fe1 C11 C7 173.8(10) . . . . ? C15 Fe1 C11 C7 -125.3(4) . . . . ? C14 Fe1 C11 C7 -163.0(4) . . . . ? C7 Fe1 C12 C13 159.2(3) . . . . ? C11 Fe1 C12 C13 -166.1(4) . . . . ? C8 Fe1 C12 C13 114.6(4) . . . . ? C10 Fe1 C12 C13 39.1(13) . . . . ? C9 Fe1 C12 C13 72.7(5) . . . . ? C16 Fe1 C12 C13 -116.7(5) . . . . ? C15 Fe1 C12 C13 -79.1(4) . . . . ? C14 Fe1 C12 C13 -37.5(4) . . . . ? C7 Fe1 C12 C16 -84.1(4) . . . . ? C11 Fe1 C12 C16 -49.4(7) . . . . ? C8 Fe1 C12 C16 -128.6(4) . . . . ? C10 Fe1 C12 C16 155.8(10) . . . . ? C9 Fe1 C12 C16 -170.6(4) . . . . ? C13 Fe1 C12 C16 116.7(5) . . . . ? C15 Fe1 C12 C16 37.6(4) . . . . ? C14 Fe1 C12 C16 79.2(4) . . . . ? C16 C12 C13 C14 -0.2(7) . . . . ? Fe1 C12 C13 C14 60.4(4) . . . . ? C16 C12 C13 Fe1 -60.6(4) . . . . ? C7 Fe1 C13 C12 -39.7(6) . . . . ? C11 Fe1 C13 C12 148.8(10) . . . . ? C8 Fe1 C13 C12 -81.8(4) . . . . ? C10 Fe1 C13 C12 -168.7(4) . . . . ? C9 Fe1 C13 C12 -126.5(4) . . . . ? C16 Fe1 C13 C12 40.5(4) . . . . ? C15 Fe1 C13 C12 83.3(4) . . . . ? C14 Fe1 C13 C12 120.2(5) . . . . ? C7 Fe1 C13 C14 -159.9(5) . . . . ? C11 Fe1 C13 C14 28.6(13) . . . . ? C8 Fe1 C13 C14 158.0(4) . . . . ? C10 Fe1 C13 C14 71.1(5) . . . . ? C9 Fe1 C13 C14 113.3(4) . . . . ? C12 Fe1 C13 C14 -120.2(5) . . . . ? C16 Fe1 C13 C14 -79.7(4) . . . . ? C15 Fe1 C13 C14 -36.9(4) . . . . ? C12 C13 C14 C15 0.3(7) . . . . ? Fe1 C13 C14 C15 59.9(4) . . . . ? C12 C13 C14 Fe1 -59.6(4) . . . . ? C7 Fe1 C14 C15 22.2(11) . . . . ? C11 Fe1 C14 C15 70.0(5) . . . . ? C8 Fe1 C14 C15 -164.7(5) . . . . ? C10 Fe1 C14 C15 112.3(4) . . . . ? C9 Fe1 C14 C15 157.1(4) . . . . ? C12 Fe1 C14 C15 -81.9(4) . . . . ? C16 Fe1 C14 C15 -35.9(4) . . . . ? C13 Fe1 C14 C15 -117.7(6) . . . . ? C7 Fe1 C14 C13 139.9(9) . . . . ? C11 Fe1 C14 C13 -172.3(4) . . . . ? C8 Fe1 C14 C13 -47.0(7) . . . . ? C10 Fe1 C14 C13 -130.0(4) . . . . ? C9 Fe1 C14 C13 -85.2(4) . . . . ? C12 Fe1 C14 C13 35.8(4) . . . . ? C16 Fe1 C14 C13 81.7(4) . . . . ? C15 Fe1 C14 C13 117.7(6) . . . . ? C13 C14 C15 C16 -0.2(7) . . . . ? Fe1 C14 C15 C16 58.6(4) . . . . ? C13 C14 C15 Fe1 -58.9(4) . . . . ? C7 Fe1 C15 C14 -172.7(4) . . . . ? C11 Fe1 C15 C14 -128.7(4) . . . . ? C8 Fe1 C15 C14 150.7(10) . . . . ? C10 Fe1 C15 C14 -84.9(5) . . . . ? C9 Fe1 C15 C14 -45.9(7) . . . . ? C12 Fe1 C15 C14 81.3(4) . . . . ? C16 Fe1 C15 C14 121.6(6) . . . . ? C13 Fe1 C15 C14 39.1(4) . . . . ? C7 Fe1 C15 C16 65.6(5) . . . . ? C11 Fe1 C15 C16 109.7(4) . . . . ? C8 Fe1 C15 C16 29.1(13) . . . . ? C10 Fe1 C15 C16 153.4(4) . . . . ? C9 Fe1 C15 C16 -167.5(5) . . . . ? C12 Fe1 C15 C16 -40.3(4) . . . . ? C13 Fe1 C15 C16 -82.5(4) . . . . ? C14 Fe1 C15 C16 -121.6(6) . . . . ? C14 C15 C16 C12 0.1(7) . . . . ? Fe1 C15 C16 C12 60.3(4) . . . . ? C14 C15 C16 Fe1 -60.2(5) . . . . ? C13 C12 C16 C15 0.1(7) . . . . ? Fe1 C12 C16 C15 -62.0(4) . . . . ? C13 C12 C16 Fe1 62.1(4) . . . . ? C7 Fe1 C16 C15 -131.3(4) . . . . ? C11 Fe1 C16 C15 -87.0(4) . . . . ? C8 Fe1 C16 C15 -171.4(4) . . . . ? C10 Fe1 C16 C15 -52.0(7) . . . . ? C9 Fe1 C16 C15 152.6(10) . . . . ? C12 Fe1 C16 C15 116.8(6) . . . . ? C13 Fe1 C16 C15 79.5(4) . . . . ? C14 Fe1 C16 C15 35.2(4) . . . . ? C7 Fe1 C16 C12 111.9(4) . . . . ? C11 Fe1 C16 C12 156.2(4) . . . . ? C8 Fe1 C16 C12 71.9(5) . . . . ? C10 Fe1 C16 C12 -168.7(5) . . . . ? C9 Fe1 C16 C12 35.8(13) . . . . ? C13 Fe1 C16 C12 -37.3(4) . . . . ? C15 Fe1 C16 C12 -116.8(6) . . . . ? C14 Fe1 C16 C12 -81.6(4) . . . . ? C4 C3 C17 C18 99(86) . . . . ? C2 C3 C17 C18 -74(86) . . . . ? C3 C17 C18 C19 -169(100) . . . . ? C17 C18 C19 C23 -102(8) . . . . ? C17 C18 C19 C20 75(8) . . . . ? C17 C18 C19 Fe2 166(8) . . . . ? C26 Fe2 C19 C18 -76.8(6) . . . . ? C25 Fe2 C19 C18 -40.8(5) . . . . ? C27 Fe2 C19 C18 79.5(7) . . . . ? C20 Fe2 C19 C18 -119.6(5) . . . . ? C24 Fe2 C19 C18 2.3(5) . . . . ? C23 Fe2 C19 C18 121.5(5) . . . . ? C22 Fe2 C19 C18 159.3(5) . . . . ? C28 Fe2 C19 C18 44.0(5) . . . . ? C21 Fe2 C19 C18 -157.0(5) . . . . ? C26 Fe2 C19 C23 161.7(4) . . . . ? C25 Fe2 C19 C23 -162.3(3) . . . . ? C27 Fe2 C19 C23 -42.0(7) . . . . ? C20 Fe2 C19 C23 118.9(4) . . . . ? C24 Fe2 C19 C23 -119.2(3) . . . . ? C22 Fe2 C19 C23 37.8(3) . . . . ? C28 Fe2 C19 C23 -77.5(3) . . . . ? C21 Fe2 C19 C23 81.4(3) . . . . ? C26 Fe2 C19 C20 42.8(6) . . . . ? C25 Fe2 C19 C20 78.7(3) . . . . ? C27 Fe2 C19 C20 -160.9(6) . . . . ? C24 Fe2 C19 C20 121.8(3) . . . . ? C23 Fe2 C19 C20 -118.9(4) . . . . ? C22 Fe2 C19 C20 -81.1(3) . . . . ? C28 Fe2 C19 C20 163.6(3) . . . . ? C21 Fe2 C19 C20 -37.5(3) . . . . ? C18 C19 C20 C21 -176.4(4) . . . . ? C23 C19 C20 C21 0.9(5) . . . . ? Fe2 C19 C20 C21 59.9(3) . . . . ? C18 C19 C20 Fe2 123.7(4) . . . . ? C23 C19 C20 Fe2 -59.0(3) . . . . ? C26 Fe2 C20 C21 79.1(3) . . . . ? C25 Fe2 C20 C21 121.4(3) . . . . ? C27 Fe2 C20 C21 46.9(6) . . . . ? C24 Fe2 C20 C21 162.4(3) . . . . ? C23 Fe2 C20 C21 -81.0(3) . . . . ? C22 Fe2 C20 C21 -37.4(3) . . . . ? C19 Fe2 C20 C21 -119.1(4) . . . . ? C28 Fe2 C20 C21 -167.6(6) . . . . ? C26 Fe2 C20 C19 -161.9(3) . . . . ? C25 Fe2 C20 C19 -119.6(3) . . . . ? C27 Fe2 C20 C19 165.9(4) . . . . ? C24 Fe2 C20 C19 -78.5(3) . . . . ? C23 Fe2 C20 C19 38.0(3) . . . . ? C22 Fe2 C20 C19 81.7(3) . . . . ? C28 Fe2 C20 C19 -48.5(7) . . . . ? C21 Fe2 C20 C19 119.1(4) . . . . ? C19 C20 C21 C22 -0.5(5) . . . . ? Fe2 C20 C21 C22 59.1(3) . . . . ? C19 C20 C21 Fe2 -59.6(3) . . . . ? C26 Fe2 C21 C20 -117.8(3) . . . . ? C25 Fe2 C21 C20 -76.8(3) . . . . ? C27 Fe2 C21 C20 -159.3(3) . . . . ? C24 Fe2 C21 C20 -47.7(6) . . . . ? C23 Fe2 C21 C20 82.5(3) . . . . ? C22 Fe2 C21 C20 119.6(4) . . . . ? C19 Fe2 C21 C20 38.1(3) . . . . ? C28 Fe2 C21 C20 170.4(4) . . . . ? C26 Fe2 C21 C22 122.5(3) . . . . ? C25 Fe2 C21 C22 163.6(3) . . . . ? C27 Fe2 C21 C22 81.0(3) . . . . ? C20 Fe2 C21 C22 -119.6(4) . . . . ? C24 Fe2 C21 C22 -167.4(5) . . . . ? C23 Fe2 C21 C22 -37.2(3) . . . . ? C19 Fe2 C21 C22 -81.5(3) . . . . ? C28 Fe2 C21 C22 50.8(6) . . . . ? C20 C21 C22 C23 0.0(5) . . . . ? Fe2 C21 C22 C23 58.9(3) . . . . ? C20 C21 C22 Fe2 -59.0(3) . . . . ? C26 Fe2 C22 C23 164.8(3) . . . . ? C25 Fe2 C22 C23 -162.4(5) . . . . ? C27 Fe2 C22 C23 123.0(3) . . . . ? C20 Fe2 C22 C23 -82.8(3) . . . . ? C24 Fe2 C22 C23 48.5(6) . . . . ? C19 Fe2 C22 C23 -38.4(3) . . . . ? C28 Fe2 C22 C23 81.1(3) . . . . ? C21 Fe2 C22 C23 -120.1(4) . . . . ? C26 Fe2 C22 C21 -75.1(3) . . . . ? C25 Fe2 C22 C21 -42.2(6) . . . . ? C27 Fe2 C22 C21 -116.9(3) . . . . ? C20 Fe2 C22 C21 37.3(3) . . . . ? C24 Fe2 C22 C21 168.6(4) . . . . ? C23 Fe2 C22 C21 120.1(4) . . . . ? C19 Fe2 C22 C21 81.8(3) . . . . ? C28 Fe2 C22 C21 -158.8(3) . . . . ? C21 C22 C23 C19 0.6(5) . . . . ? Fe2 C22 C23 C19 59.7(3) . . . . ? C21 C22 C23 Fe2 -59.1(3) . . . . ? C18 C19 C23 C22 176.4(4) . . . . ? C20 C19 C23 C22 -0.9(5) . . . . ? Fe2 C19 C23 C22 -59.9(3) . . . . ? C18 C19 C23 Fe2 -123.8(4) . . . . ? C20 C19 C23 Fe2 59.0(3) . . . . ? C26 Fe2 C23 C22 -40.0(7) . . . . ? C25 Fe2 C23 C22 163.1(5) . . . . ? C27 Fe2 C23 C22 -75.9(3) . . . . ? C20 Fe2 C23 C22 80.6(3) . . . . ? C24 Fe2 C23 C22 -160.7(3) . . . . ? C19 Fe2 C23 C22 118.6(4) . . . . ? C28 Fe2 C23 C22 -118.3(3) . . . . ? C21 Fe2 C23 C22 37.1(3) . . . . ? C26 Fe2 C23 C19 -158.6(5) . . . . ? C25 Fe2 C23 C19 44.5(6) . . . . ? C27 Fe2 C23 C19 165.4(3) . . . . ? C20 Fe2 C23 C19 -38.1(3) . . . . ? C24 Fe2 C23 C19 80.7(3) . . . . ? C22 Fe2 C23 C19 -118.6(4) . . . . ? C28 Fe2 C23 C19 123.0(3) . . . . ? C21 Fe2 C23 C19 -81.5(3) . . . . ? C26 Fe2 C24 C28 -81.4(3) . . . . ? C25 Fe2 C24 C28 -119.3(4) . . . . ? C27 Fe2 C24 C28 -37.6(3) . . . . ? C20 Fe2 C24 C28 166.3(3) . . . . ? C23 Fe2 C24 C28 80.1(3) . . . . ? C22 Fe2 C24 C28 44.6(6) . . . . ? C19 Fe2 C24 C28 123.4(3) . . . . ? C21 Fe2 C24 C28 -157.9(5) . . . . ? C26 Fe2 C24 C25 37.9(3) . . . . ? C27 Fe2 C24 C25 81.7(3) . . . . ? C20 Fe2 C24 C25 -74.4(3) . . . . ? C23 Fe2 C24 C25 -160.6(3) . . . . ? C22 Fe2 C24 C25 163.9(4) . . . . ? C19 Fe2 C24 C25 -117.3(3) . . . . ? C28 Fe2 C24 C25 119.3(4) . . . . ? C21 Fe2 C24 C25 -38.6(7) . . . . ? C28 C24 C25 C26 0.1(5) . . . . ? Fe2 C24 C25 C26 -59.5(3) . . . . ? C28 C24 C25 Fe2 59.6(3) . . . . ? C27 Fe2 C25 C26 37.7(3) . . . . ? C20 Fe2 C25 C26 -116.7(3) . . . . ? C24 Fe2 C25 C26 118.9(4) . . . . ? C23 Fe2 C25 C26 168.1(5) . . . . ? C22 Fe2 C25 C26 -44.2(6) . . . . ? C19 Fe2 C25 C26 -159.0(3) . . . . ? C28 Fe2 C25 C26 81.5(3) . . . . ? C21 Fe2 C25 C26 -75.5(3) . . . . ? C26 Fe2 C25 C24 -118.9(4) . . . . ? C27 Fe2 C25 C24 -81.2(3) . . . . ? C20 Fe2 C25 C24 124.4(3) . . . . ? C23 Fe2 C25 C24 49.2(6) . . . . ? C22 Fe2 C25 C24 -163.1(5) . . . . ? C19 Fe2 C25 C24 82.0(3) . . . . ? C28 Fe2 C25 C24 -37.4(3) . . . . ? C21 Fe2 C25 C24 165.6(3) . . . . ? C24 C25 C26 C27 0.1(5) . . . . ? Fe2 C25 C26 C27 -59.7(3) . . . . ? C24 C25 C26 Fe2 59.8(3) . . . . ? C25 Fe2 C26 C27 119.1(4) . . . . ? C20 Fe2 C26 C27 -160.0(3) . . . . ? C24 Fe2 C26 C27 81.2(3) . . . . ? C23 Fe2 C26 C27 -48.1(7) . . . . ? C22 Fe2 C26 C27 -78.0(3) . . . . ? C19 Fe2 C26 C27 169.0(4) . . . . ? C28 Fe2 C26 C27 37.6(3) . . . . ? C21 Fe2 C26 C27 -118.6(3) . . . . ? C27 Fe2 C26 C25 -119.1(4) . . . . ? C20 Fe2 C26 C25 80.9(3) . . . . ? C24 Fe2 C26 C25 -37.9(3) . . . . ? C23 Fe2 C26 C25 -167.2(5) . . . . ? C22 Fe2 C26 C25 162.9(3) . . . . ? C19 Fe2 C26 C25 49.9(6) . . . . ? C28 Fe2 C26 C25 -81.5(3) . . . . ? C21 Fe2 C26 C25 122.3(3) . . . . ? C25 C26 C27 C28 -0.3(5) . . . . ? Fe2 C26 C27 C28 -59.8(3) . . . . ? C25 C26 C27 Fe2 59.5(3) . . . . ? C25 Fe2 C27 C26 -37.9(3) . . . . ? C20 Fe2 C27 C26 45.2(6) . . . . ? C24 Fe2 C27 C26 -81.9(3) . . . . ? C23 Fe2 C27 C26 162.0(3) . . . . ? C22 Fe2 C27 C26 120.7(3) . . . . ? C19 Fe2 C27 C26 -165.8(5) . . . . ? C28 Fe2 C27 C26 -119.3(4) . . . . ? C21 Fe2 C27 C26 78.5(3) . . . . ? C26 Fe2 C27 C28 119.3(4) . . . . ? C25 Fe2 C27 C28 81.4(3) . . . . ? C20 Fe2 C27 C28 164.5(4) . . . . ? C24 Fe2 C27 C28 37.4(3) . . . . ? C23 Fe2 C27 C28 -78.7(3) . . . . ? C22 Fe2 C27 C28 -120.0(3) . . . . ? C19 Fe2 C27 C28 -46.5(7) . . . . ? C21 Fe2 C27 C28 -162.2(3) . . . . ? C25 C24 C28 C27 -0.3(5) . . . . ? Fe2 C24 C28 C27 58.7(3) . . . . ? C25 C24 C28 Fe2 -59.1(3) . . . . ? C26 C27 C28 C24 0.4(5) . . . . ? Fe2 C27 C28 C24 -59.0(3) . . . . ? C26 C27 C28 Fe2 59.3(3) . . . . ? C26 Fe2 C28 C24 81.8(3) . . . . ? C25 Fe2 C28 C24 37.8(3) . . . . ? C27 Fe2 C28 C24 119.4(4) . . . . ? C20 Fe2 C28 C24 -39.3(7) . . . . ? C23 Fe2 C28 C24 -119.3(3) . . . . ? C22 Fe2 C28 C24 -162.1(3) . . . . ? C19 Fe2 C28 C24 -76.6(3) . . . . ? C21 Fe2 C28 C24 161.4(4) . . . . ? C26 Fe2 C28 C27 -37.6(3) . . . . ? C25 Fe2 C28 C27 -81.6(3) . . . . ? C20 Fe2 C28 C27 -158.7(6) . . . . ? C24 Fe2 C28 C27 -119.4(4) . . . . ? C23 Fe2 C28 C27 121.2(3) . . . . ? C22 Fe2 C28 C27 78.5(3) . . . . ? C19 Fe2 C28 C27 163.9(3) . . . . ? C21 Fe2 C28 C27 41.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.647 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.108 _database_code_depnum_ccdc_archive 'CCDC 942659' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_rm063 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H26 Fe2' _chemical_formula_weight 546.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' 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 10.1907(12) _cell_length_b 7.5711(3) _cell_length_c 20.759(3) _cell_angle_alpha 90.00 _cell_angle_beta 126.477(19) _cell_angle_gamma 90.00 _cell_volume 1287.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3625 _cell_measurement_theta_min 3.4760 _cell_measurement_theta_max 26.9950 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 564 _exptl_absorpt_coefficient_mu 1.147 _exptl_absorpt_correction_T_min 0.7783 _exptl_absorpt_correction_T_max 0.8652 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Micro-Focus (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION SUPER NOVA' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9242 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2255 _reflns_number_gt 1958 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.1068P)^2^+12.2628P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2255 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1058 _refine_ls_R_factor_gt 0.0987 _refine_ls_wR_factor_ref 0.2822 _refine_ls_wR_factor_gt 0.2776 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.34767(14) 0.95434(16) 0.32802(7) 0.0469(5) Uani 1 1 d . . . C1 C -0.0113(14) 1.4375(17) 0.0141(6) 0.076(3) Uani 1 1 d . . . C2 C -0.0282(13) 1.2917(15) 0.0520(6) 0.064(3) Uani 1 1 d . . . C3 C -0.1460(17) 1.165(2) 0.0085(7) 0.098(4) Uani 1 1 d . . . H3 H -0.2153 1.1719 -0.0484 0.117 Uiso 1 1 calc R . . C4 C -0.1650(17) 1.028(2) 0.0467(8) 0.101(5) Uani 1 1 d . . . H4 H -0.2476 0.9416 0.0161 0.122 Uiso 1 1 calc R . . C5 C -0.0638(14) 1.0169(15) 0.1289(7) 0.073(3) Uani 1 1 d . . . H5 H -0.0769 0.9223 0.1547 0.088 Uiso 1 1 calc R . . C6 C 0.0568(10) 1.1412(11) 0.1747(5) 0.0443(18) Uani 1 1 d . . . C7 C 0.0750(10) 1.2786(12) 0.1359(5) 0.050(2) Uani 1 1 d . . . H7 H 0.1581 1.3644 0.1665 0.060 Uiso 1 1 calc R . . C8 C 0.1644(10) 1.1318(10) 0.2626(5) 0.0432(18) Uani 1 1 d . . . C9 C 0.1388(12) 1.0262(14) 0.3121(6) 0.060(2) Uani 1 1 d . . . H9 H 0.0479 0.9516 0.2937 0.072 Uiso 1 1 calc R . . C10 C 0.2730(15) 1.0536(16) 0.3926(6) 0.073(3) Uani 1 1 d . . . H10 H 0.2868 1.0014 0.4379 0.087 Uiso 1 1 calc R . . C11 C 0.3836(14) 1.1712(14) 0.3950(6) 0.068(3) Uani 1 1 d . . . H11 H 0.4852 1.2089 0.4419 0.082 Uiso 1 1 calc R . . C12 C 0.3161(11) 1.2233(10) 0.3150(5) 0.049(2) Uani 1 1 d . . . H12 H 0.3632 1.3043 0.2992 0.059 Uiso 1 1 calc R . . C13 C 0.3192(18) 0.6984(17) 0.2939(12) 0.101(5) Uani 1 1 d . . . H13 H 0.2244 0.6293 0.2740 0.122 Uiso 1 1 calc R . . C14 C 0.4506(17) 0.7116(17) 0.3711(10) 0.092(4) Uani 1 1 d . . . H14 H 0.4631 0.6517 0.4146 0.111 Uiso 1 1 calc R . . C15 C 0.5622(15) 0.8228(19) 0.3775(10) 0.097(4) Uani 1 1 d . . . H15 H 0.6651 0.8497 0.4262 0.116 Uiso 1 1 calc R . . C16 C 0.507(2) 0.890(2) 0.3046(12) 0.104(5) Uani 1 1 d . . . H16 H 0.5587 0.9742 0.2927 0.124 Uiso 1 1 calc R . . C17 C 0.349(2) 0.805(2) 0.2489(9) 0.115(6) Uani 1 1 d . . . H17 H 0.2785 0.8199 0.1924 0.138 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 0.0493(8) 0.0394(8) 0.0529(8) 0.0075(5) 0.0309(6) 0.0074(5) C1 0.070(6) 0.114(10) 0.049(6) 0.035(6) 0.037(5) 0.033(7) C2 0.063(6) 0.082(7) 0.045(5) 0.015(5) 0.030(5) 0.017(5) C3 0.085(9) 0.135(13) 0.050(6) -0.004(7) 0.028(6) -0.004(9) C4 0.088(9) 0.101(10) 0.070(8) -0.011(7) 0.023(7) -0.030(8) C5 0.074(7) 0.065(6) 0.069(7) -0.004(5) 0.036(6) -0.019(5) C6 0.042(4) 0.048(5) 0.045(4) 0.005(4) 0.027(4) 0.003(4) C7 0.048(5) 0.054(5) 0.049(5) 0.008(4) 0.029(4) 0.010(4) C8 0.057(5) 0.033(4) 0.047(4) 0.005(3) 0.035(4) 0.008(3) C9 0.057(5) 0.069(6) 0.070(6) 0.016(5) 0.046(5) 0.012(5) C10 0.095(8) 0.081(8) 0.057(6) 0.025(5) 0.054(6) 0.028(6) C11 0.087(7) 0.060(6) 0.046(5) 0.000(4) 0.033(5) 0.011(5) C12 0.064(5) 0.026(4) 0.057(5) 0.008(3) 0.035(4) 0.004(4) C13 0.087(9) 0.055(7) 0.145(14) -0.020(8) 0.060(10) 0.003(6) C14 0.084(9) 0.066(7) 0.122(11) 0.032(8) 0.059(9) 0.030(7) C15 0.062(7) 0.079(8) 0.123(12) -0.004(8) 0.040(8) 0.018(6) C16 0.118(12) 0.093(10) 0.164(15) 0.043(10) 0.119(13) 0.043(9) C17 0.138(14) 0.122(13) 0.080(9) -0.004(9) 0.063(10) 0.073(12) _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 C17 1.997(12) . ? Fe1 C16 2.006(12) . ? Fe1 C13 2.024(12) . ? Fe1 C9 2.025(9) . ? Fe1 C8 2.030(8) . ? Fe1 C10 2.038(10) . ? Fe1 C15 2.039(12) . ? Fe1 C11 2.039(10) . ? Fe1 C14 2.040(11) . ? Fe1 C12 2.054(8) . ? C1 C1 1.20(2) 3_585 ? C1 C2 1.425(15) . ? C2 C3 1.372(17) . ? C2 C7 1.405(12) . ? C3 C4 1.391(19) . ? C3 H3 0.9500 . ? C4 C5 1.375(17) . ? C4 H4 0.9500 . ? C5 C6 1.382(13) . ? C5 H5 0.9500 . ? C6 C7 1.393(12) . ? C6 C8 1.470(11) . ? C7 H7 0.9500 . ? C8 C12 1.433(12) . ? C8 C9 1.443(12) . ? C9 C10 1.410(15) . ? C9 H9 0.9500 . ? C10 C11 1.413(16) . ? C10 H10 0.9500 . ? C11 C12 1.425(12) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.35(2) . ? C13 C17 1.40(2) . ? C13 H13 0.9500 . ? C14 C15 1.357(18) . ? C14 H14 0.9500 . ? C15 C16 1.36(2) . ? C15 H15 0.9500 . ? C16 C17 1.46(2) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? 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 C17 Fe1 C16 42.8(7) . . ? C17 Fe1 C13 40.6(6) . . ? C16 Fe1 C13 69.7(7) . . ? C17 Fe1 C9 122.4(6) . . ? C16 Fe1 C9 161.2(6) . . ? C13 Fe1 C9 106.4(5) . . ? C17 Fe1 C8 106.0(5) . . ? C16 Fe1 C8 123.5(5) . . ? C13 Fe1 C8 121.1(5) . . ? C9 Fe1 C8 41.7(3) . . ? C17 Fe1 C10 159.3(8) . . ? C16 Fe1 C10 156.7(7) . . ? C13 Fe1 C10 123.4(7) . . ? C9 Fe1 C10 40.6(4) . . ? C8 Fe1 C10 69.0(4) . . ? C17 Fe1 C15 67.1(6) . . ? C16 Fe1 C15 39.3(6) . . ? C13 Fe1 C15 66.2(6) . . ? C9 Fe1 C15 157.2(6) . . ? C8 Fe1 C15 160.9(5) . . ? C10 Fe1 C15 123.8(6) . . ? C17 Fe1 C11 158.3(7) . . ? C16 Fe1 C11 121.1(7) . . ? C13 Fe1 C11 160.0(7) . . ? C9 Fe1 C11 68.9(5) . . ? C8 Fe1 C11 69.2(4) . . ? C10 Fe1 C11 40.6(5) . . ? C15 Fe1 C11 110.2(5) . . ? C17 Fe1 C14 66.3(6) . . ? C16 Fe1 C14 67.1(6) . . ? C13 Fe1 C14 38.7(6) . . ? C9 Fe1 C14 122.0(5) . . ? C8 Fe1 C14 156.7(5) . . ? C10 Fe1 C14 109.9(5) . . ? C15 Fe1 C14 38.9(5) . . ? C11 Fe1 C14 126.1(6) . . ? C17 Fe1 C12 121.9(6) . . ? C16 Fe1 C12 107.0(5) . . ? C13 Fe1 C12 157.6(6) . . ? C9 Fe1 C12 69.2(4) . . ? C8 Fe1 C12 41.1(3) . . ? C10 Fe1 C12 68.3(4) . . ? C15 Fe1 C12 126.0(5) . . ? C11 Fe1 C12 40.7(4) . . ? C14 Fe1 C12 161.8(5) . . ? C1 C1 C2 176.4(17) 3_585 . ? C3 C2 C7 119.0(10) . . ? C3 C2 C1 121.5(10) . . ? C7 C2 C1 119.5(10) . . ? C2 C3 C4 120.7(11) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 119.8(12) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 121.1(11) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C7 118.8(8) . . ? C5 C6 C8 121.5(8) . . ? C7 C6 C8 119.8(8) . . ? C6 C7 C2 120.7(9) . . ? C6 C7 H7 119.7 . . ? C2 C7 H7 119.7 . . ? C12 C8 C9 107.3(8) . . ? C12 C8 C6 126.3(7) . . ? C9 C8 C6 126.4(8) . . ? C12 C8 Fe1 70.4(5) . . ? C9 C8 Fe1 69.0(5) . . ? C6 C8 Fe1 125.0(6) . . ? C10 C9 C8 107.7(9) . . ? C10 C9 Fe1 70.2(6) . . ? C8 C9 Fe1 69.3(5) . . ? C10 C9 H9 126.2 . . ? C8 C9 H9 126.2 . . ? Fe1 C9 H9 125.9 . . ? C9 C10 C11 109.0(9) . . ? C9 C10 Fe1 69.2(5) . . ? C11 C10 Fe1 69.8(6) . . ? C9 C10 H10 125.5 . . ? C11 C10 H10 125.5 . . ? Fe1 C10 H10 127.1 . . ? C10 C11 C12 108.1(9) . . ? C10 C11 Fe1 69.7(6) . . ? C12 C11 Fe1 70.2(5) . . ? C10 C11 H11 126.0 . . ? C12 C11 H11 126.0 . . ? Fe1 C11 H11 125.8 . . ? C11 C12 C8 107.9(8) . . ? C11 C12 Fe1 69.1(5) . . ? C8 C12 Fe1 68.6(4) . . ? C11 C12 H12 126.1 . . ? C8 C12 H12 126.1 . . ? Fe1 C12 H12 127.9 . . ? C14 C13 C17 107.2(14) . . ? C14 C13 Fe1 71.3(8) . . ? C17 C13 Fe1 68.6(7) . . ? C14 C13 H13 126.4 . . ? C17 C13 H13 126.4 . . ? Fe1 C13 H13 125.3 . . ? C13 C14 C15 110.2(14) . . ? C13 C14 Fe1 70.0(7) . . ? C15 C14 Fe1 70.5(7) . . ? C13 C14 H14 124.9 . . ? C15 C14 H14 124.9 . . ? Fe1 C14 H14 126.2 . . ? C14 C15 C16 110.7(14) . . ? C14 C15 Fe1 70.6(7) . . ? C16 C15 Fe1 69.1(7) . . ? C14 C15 H15 124.7 . . ? C16 C15 H15 124.7 . . ? Fe1 C15 H15 127.3 . . ? C15 C16 C17 104.4(13) . . ? C15 C16 Fe1 71.6(7) . . ? C17 C16 Fe1 68.3(7) . . ? C15 C16 H16 127.8 . . ? C17 C16 H16 127.8 . . ? Fe1 C16 H16 124.0 . . ? C13 C17 C16 107.4(13) . . ? C13 C17 Fe1 70.7(8) . . ? C16 C17 Fe1 68.9(7) . . ? C13 C17 H17 126.3 . . ? C16 C17 H17 126.3 . . ? Fe1 C17 H17 125.6 . . ? 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 C1 C1 C2 C3 -166(26) 3_585 . . . ? C1 C1 C2 C7 16(27) 3_585 . . . ? C7 C2 C3 C4 1(2) . . . . ? C1 C2 C3 C4 -177.4(13) . . . . ? C2 C3 C4 C5 -1(2) . . . . ? C3 C4 C5 C6 0(2) . . . . ? C4 C5 C6 C7 -0.3(17) . . . . ? C4 C5 C6 C8 179.4(11) . . . . ? C5 C6 C7 C2 0.6(13) . . . . ? C8 C6 C7 C2 -179.0(8) . . . . ? C3 C2 C7 C6 -1.0(15) . . . . ? C1 C2 C7 C6 177.4(9) . . . . ? C5 C6 C8 C12 163.5(9) . . . . ? C7 C6 C8 C12 -16.9(12) . . . . ? C5 C6 C8 C9 -15.3(14) . . . . ? C7 C6 C8 C9 164.4(8) . . . . ? C5 C6 C8 Fe1 73.2(11) . . . . ? C7 C6 C8 Fe1 -107.2(8) . . . . ? C17 Fe1 C8 C12 -120.6(8) . . . . ? C16 Fe1 C8 C12 -77.1(8) . . . . ? C13 Fe1 C8 C12 -162.1(8) . . . . ? C9 Fe1 C8 C12 118.4(7) . . . . ? C10 Fe1 C8 C12 80.7(6) . . . . ? C15 Fe1 C8 C12 -54.7(16) . . . . ? C11 Fe1 C8 C12 37.1(5) . . . . ? C14 Fe1 C8 C12 172.3(12) . . . . ? C17 Fe1 C8 C9 121.0(9) . . . . ? C16 Fe1 C8 C9 164.5(8) . . . . ? C13 Fe1 C8 C9 79.5(9) . . . . ? C10 Fe1 C8 C9 -37.7(6) . . . . ? C15 Fe1 C8 C9 -173.1(14) . . . . ? C11 Fe1 C8 C9 -81.3(6) . . . . ? C14 Fe1 C8 C9 53.9(14) . . . . ? C12 Fe1 C8 C9 -118.4(7) . . . . ? C17 Fe1 C8 C6 0.5(10) . . . . ? C16 Fe1 C8 C6 44.0(10) . . . . ? C13 Fe1 C8 C6 -41.0(10) . . . . ? C9 Fe1 C8 C6 -120.5(10) . . . . ? C10 Fe1 C8 C6 -158.2(9) . . . . ? C15 Fe1 C8 C6 66.4(17) . . . . ? C11 Fe1 C8 C6 158.2(8) . . . . ? C14 Fe1 C8 C6 -66.6(15) . . . . ? C12 Fe1 C8 C6 121.1(9) . . . . ? C12 C8 C9 C10 -0.2(10) . . . . ? C6 C8 C9 C10 178.7(8) . . . . ? Fe1 C8 C9 C10 60.0(7) . . . . ? C12 C8 C9 Fe1 -60.2(6) . . . . ? C6 C8 C9 Fe1 118.7(8) . . . . ? C17 Fe1 C9 C10 164.0(9) . . . . ? C16 Fe1 C9 C10 -162.3(16) . . . . ? C13 Fe1 C9 C10 122.7(9) . . . . ? C8 Fe1 C9 C10 -118.7(9) . . . . ? C15 Fe1 C9 C10 55.4(15) . . . . ? C11 Fe1 C9 C10 -36.8(6) . . . . ? C14 Fe1 C9 C10 83.5(9) . . . . ? C12 Fe1 C9 C10 -80.5(7) . . . . ? C17 Fe1 C9 C8 -77.2(9) . . . . ? C16 Fe1 C9 C8 -43.6(19) . . . . ? C13 Fe1 C9 C8 -118.6(8) . . . . ? C10 Fe1 C9 C8 118.7(9) . . . . ? C15 Fe1 C9 C8 174.2(12) . . . . ? C11 Fe1 C9 C8 82.0(6) . . . . ? C14 Fe1 C9 C8 -157.8(7) . . . . ? C12 Fe1 C9 C8 38.2(5) . . . . ? C8 C9 C10 C11 -0.9(12) . . . . ? Fe1 C9 C10 C11 58.5(8) . . . . ? C8 C9 C10 Fe1 -59.5(6) . . . . ? C17 Fe1 C10 C9 -40.9(17) . . . . ? C16 Fe1 C10 C9 165.6(12) . . . . ? C13 Fe1 C10 C9 -75.5(8) . . . . ? C8 Fe1 C10 C9 38.7(6) . . . . ? C15 Fe1 C10 C9 -157.4(7) . . . . ? C11 Fe1 C10 C9 120.8(9) . . . . ? C14 Fe1 C10 C9 -116.4(7) . . . . ? C12 Fe1 C10 C9 82.9(6) . . . . ? C17 Fe1 C10 C11 -161.7(14) . . . . ? C16 Fe1 C10 C11 44.8(15) . . . . ? C13 Fe1 C10 C11 163.7(7) . . . . ? C9 Fe1 C10 C11 -120.8(9) . . . . ? C8 Fe1 C10 C11 -82.1(6) . . . . ? C15 Fe1 C10 C11 81.8(8) . . . . ? C14 Fe1 C10 C11 122.8(7) . . . . ? C12 Fe1 C10 C11 -37.9(6) . . . . ? C9 C10 C11 C12 1.8(12) . . . . ? Fe1 C10 C11 C12 59.9(7) . . . . ? C9 C10 C11 Fe1 -58.2(7) . . . . ? C17 Fe1 C11 C10 162.5(13) . . . . ? C16 Fe1 C11 C10 -161.0(7) . . . . ? C13 Fe1 C11 C10 -43.0(17) . . . . ? C9 Fe1 C11 C10 36.8(6) . . . . ? C8 Fe1 C11 C10 81.6(6) . . . . ? C15 Fe1 C11 C10 -118.8(8) . . . . ? C14 Fe1 C11 C10 -78.1(8) . . . . ? C12 Fe1 C11 C10 119.0(9) . . . . ? C17 Fe1 C11 C12 43.5(17) . . . . ? C16 Fe1 C11 C12 79.9(8) . . . . ? C13 Fe1 C11 C12 -162.0(14) . . . . ? C9 Fe1 C11 C12 -82.2(6) . . . . ? C8 Fe1 C11 C12 -37.4(6) . . . . ? C10 Fe1 C11 C12 -119.0(9) . . . . ? C15 Fe1 C11 C12 122.1(7) . . . . ? C14 Fe1 C11 C12 162.8(7) . . . . ? C10 C11 C12 C8 -1.9(11) . . . . ? Fe1 C11 C12 C8 57.7(6) . . . . ? C10 C11 C12 Fe1 -59.6(7) . . . . ? C9 C8 C12 C11 1.3(10) . . . . ? C6 C8 C12 C11 -177.6(8) . . . . ? Fe1 C8 C12 C11 -58.0(6) . . . . ? C9 C8 C12 Fe1 59.3(6) . . . . ? C6 C8 C12 Fe1 -119.6(8) . . . . ? C17 Fe1 C12 C11 -162.6(9) . . . . ? C16 Fe1 C12 C11 -118.1(9) . . . . ? C13 Fe1 C12 C11 163.9(14) . . . . ? C9 Fe1 C12 C11 81.4(7) . . . . ? C8 Fe1 C12 C11 120.2(8) . . . . ? C10 Fe1 C12 C11 37.7(7) . . . . ? C15 Fe1 C12 C11 -79.1(9) . . . . ? C14 Fe1 C12 C11 -50.0(18) . . . . ? C17 Fe1 C12 C8 77.2(8) . . . . ? C16 Fe1 C12 C8 121.7(7) . . . . ? C13 Fe1 C12 C8 43.7(15) . . . . ? C9 Fe1 C12 C8 -38.8(5) . . . . ? C10 Fe1 C12 C8 -82.5(6) . . . . ? C15 Fe1 C12 C8 160.7(7) . . . . ? C11 Fe1 C12 C8 -120.2(8) . . . . ? C14 Fe1 C12 C8 -170.2(15) . . . . ? C17 Fe1 C13 C14 117.9(13) . . . . ? C16 Fe1 C13 C14 78.3(10) . . . . ? C9 Fe1 C13 C14 -121.1(9) . . . . ? C8 Fe1 C13 C14 -164.1(8) . . . . ? C10 Fe1 C13 C14 -80.1(10) . . . . ? C15 Fe1 C13 C14 35.9(9) . . . . ? C11 Fe1 C13 C14 -48.0(19) . . . . ? C12 Fe1 C13 C14 163.9(11) . . . . ? C16 Fe1 C13 C17 -39.6(9) . . . . ? C9 Fe1 C13 C17 121.0(9) . . . . ? C8 Fe1 C13 C17 78.0(10) . . . . ? C10 Fe1 C13 C17 162.0(9) . . . . ? C15 Fe1 C13 C17 -82.0(10) . . . . ? C11 Fe1 C13 C17 -165.9(14) . . . . ? C14 Fe1 C13 C17 -117.9(13) . . . . ? C12 Fe1 C13 C17 46.0(18) . . . . ? C17 C13 C14 C15 0.3(15) . . . . ? Fe1 C13 C14 C15 -59.2(10) . . . . ? C17 C13 C14 Fe1 59.5(9) . . . . ? C17 Fe1 C14 C13 -39.0(10) . . . . ? C16 Fe1 C14 C13 -85.7(11) . . . . ? C9 Fe1 C14 C13 75.6(11) . . . . ? C8 Fe1 C14 C13 36.3(18) . . . . ? C10 Fe1 C14 C13 119.1(10) . . . . ? C15 Fe1 C14 C13 -121.2(15) . . . . ? C11 Fe1 C14 C13 161.6(10) . . . . ? C12 Fe1 C14 C13 -160.2(14) . . . . ? C17 Fe1 C14 C15 82.3(11) . . . . ? C16 Fe1 C14 C15 35.5(10) . . . . ? C13 Fe1 C14 C15 121.2(15) . . . . ? C9 Fe1 C14 C15 -163.1(9) . . . . ? C8 Fe1 C14 C15 157.5(11) . . . . ? C10 Fe1 C14 C15 -119.7(10) . . . . ? C11 Fe1 C14 C15 -77.1(11) . . . . ? C12 Fe1 C14 C15 -39(2) . . . . ? C13 C14 C15 C16 1.4(16) . . . . ? Fe1 C14 C15 C16 -57.5(10) . . . . ? C13 C14 C15 Fe1 58.9(9) . . . . ? C17 Fe1 C15 C14 -80.2(11) . . . . ? C16 Fe1 C15 C14 -122.4(14) . . . . ? C13 Fe1 C15 C14 -35.8(10) . . . . ? C9 Fe1 C15 C14 39.4(18) . . . . ? C8 Fe1 C15 C14 -152.5(13) . . . . ? C10 Fe1 C15 C14 79.6(11) . . . . ? C11 Fe1 C15 C14 122.9(10) . . . . ? C12 Fe1 C15 C14 166.0(9) . . . . ? C17 Fe1 C15 C16 42.2(11) . . . . ? C13 Fe1 C15 C16 86.6(11) . . . . ? C9 Fe1 C15 C16 161.8(13) . . . . ? C8 Fe1 C15 C16 -30(2) . . . . ? C10 Fe1 C15 C16 -158.0(10) . . . . ? C11 Fe1 C15 C16 -114.7(10) . . . . ? C14 Fe1 C15 C16 122.4(14) . . . . ? C12 Fe1 C15 C16 -71.6(11) . . . . ? C14 C15 C16 C17 -2.4(15) . . . . ? Fe1 C15 C16 C17 -60.8(8) . . . . ? C14 C15 C16 Fe1 58.4(10) . . . . ? C17 Fe1 C16 C15 -114.5(13) . . . . ? C13 Fe1 C16 C15 -76.8(10) . . . . ? C9 Fe1 C16 C15 -158.0(14) . . . . ? C8 Fe1 C16 C15 168.6(8) . . . . ? C10 Fe1 C16 C15 52.0(18) . . . . ? C11 Fe1 C16 C15 84.4(10) . . . . ? C14 Fe1 C16 C15 -35.1(9) . . . . ? C12 Fe1 C16 C15 126.6(9) . . . . ? C13 Fe1 C16 C17 37.7(9) . . . . ? C9 Fe1 C16 C17 -44(2) . . . . ? C8 Fe1 C16 C17 -76.9(10) . . . . ? C10 Fe1 C16 C17 166.5(12) . . . . ? C15 Fe1 C16 C17 114.5(13) . . . . ? C11 Fe1 C16 C17 -161.1(9) . . . . ? C14 Fe1 C16 C17 79.4(10) . . . . ? C12 Fe1 C16 C17 -118.9(9) . . . . ? C14 C13 C17 C16 -1.8(14) . . . . ? Fe1 C13 C17 C16 59.4(9) . . . . ? C14 C13 C17 Fe1 -61.2(9) . . . . ? C15 C16 C17 C13 2.6(14) . . . . ? Fe1 C16 C17 C13 -60.5(9) . . . . ? C15 C16 C17 Fe1 63.1(9) . . . . ? C16 Fe1 C17 C13 118.4(12) . . . . ? C9 Fe1 C17 C13 -76.9(10) . . . . ? C8 Fe1 C17 C13 -119.3(9) . . . . ? C10 Fe1 C17 C13 -46.6(18) . . . . ? C15 Fe1 C17 C13 79.6(10) . . . . ? C11 Fe1 C17 C13 166.9(12) . . . . ? C14 Fe1 C17 C13 37.2(8) . . . . ? C12 Fe1 C17 C13 -161.1(8) . . . . ? C13 Fe1 C17 C16 -118.4(12) . . . . ? C9 Fe1 C17 C16 164.7(7) . . . . ? C8 Fe1 C17 C16 122.3(8) . . . . ? C10 Fe1 C17 C16 -164.9(12) . . . . ? C15 Fe1 C17 C16 -38.7(8) . . . . ? C11 Fe1 C17 C16 48.6(17) . . . . ? C14 Fe1 C17 C16 -81.2(9) . . . . ? C12 Fe1 C17 C16 80.5(9) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.267 _refine_diff_density_min -0.817 _refine_diff_density_rms 0.138 _database_code_depnum_ccdc_archive 'CCDC 942660' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_rm066 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H22 Fe Si' _chemical_formula_weight 358.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.0972(4) _cell_length_b 13.1305(3) _cell_length_c 13.4256(4) _cell_angle_alpha 90.00 _cell_angle_beta 112.670(4) _cell_angle_gamma 90.00 _cell_volume 1805.13(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10405 _cell_measurement_theta_min 3.3980 _cell_measurement_theta_max 32.1010 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 0.899 _exptl_absorpt_correction_T_min 0.8200 _exptl_absorpt_correction_T_max 0.8921 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Micro-Focus (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION SUPER NOVA' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13235 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3174 _reflns_number_gt 2904 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.0388P)^2^+0.9712P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3174 _refine_ls_number_parameters 211 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0841 _refine_ls_wR_factor_gt 0.0803 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.75427(3) 0.08280(2) 0.14832(2) 0.02506(12) Uani 1 1 d . . . Si1 Si 0.76575(6) 0.50099(4) 0.79520(5) 0.02838(16) Uani 1 1 d . . . C1 C 0.9257(2) 0.56707(19) 0.8440(2) 0.0449(6) Uani 1 1 d . . . H1A H 0.9954 0.5181 0.8805 0.067 Uiso 1 1 calc R . . H1B H 0.9264 0.6209 0.8948 0.067 Uiso 1 1 calc R . . H1C H 0.9399 0.5972 0.7826 0.067 Uiso 1 1 calc R . . C2 C 0.7610(2) 0.40716(15) 0.69128(17) 0.0277(5) Uani 1 1 d . . . C3 C 0.75258(19) 0.34801(15) 0.62020(17) 0.0256(4) Uani 1 1 d . . . C4 C 0.74358(19) 0.27767(14) 0.53541(15) 0.0236(4) Uani 1 1 d . . . C5 C 0.8558(2) 0.23654(16) 0.52752(17) 0.0287(5) Uani 1 1 d . . . H5 H 0.9393 0.2553 0.5788 0.034 Uiso 1 1 calc R . . C6 C 0.8466(2) 0.16922(15) 0.44625(17) 0.0281(4) Uani 1 1 d . . . H6 H 0.9242 0.1424 0.4424 0.034 Uiso 1 1 calc R . . C7 C 0.72517(19) 0.13946(14) 0.36901(15) 0.0230(4) Uani 1 1 d . . . C8 C 0.61364(19) 0.18139(14) 0.37662(16) 0.0235(4) Uani 1 1 d . . . H8 H 0.5301 0.1632 0.3248 0.028 Uiso 1 1 calc R . . C9 C 0.62211(19) 0.24905(14) 0.45824(16) 0.0242(4) Uani 1 1 d . . . H9 H 0.5446 0.2763 0.4618 0.029 Uiso 1 1 calc R . . C10 C 0.7162(2) 0.06361(14) 0.28548(16) 0.0235(4) Uani 1 1 d . . . C11 C 0.8184(2) -0.00327(14) 0.28575(17) 0.0271(4) Uani 1 1 d . . . H11 H 0.9050 -0.0047 0.3387 0.032 Uiso 1 1 calc R . . C12 C 0.7678(2) -0.06714(15) 0.19311(18) 0.0306(5) Uani 1 1 d . . . H12 H 0.8146 -0.1189 0.1738 0.037 Uiso 1 1 calc R . . C13 C 0.6353(2) -0.04007(15) 0.13467(17) 0.0303(5) Uani 1 1 d . . . H13 H 0.5781 -0.0703 0.0692 0.036 Uiso 1 1 calc R . . C14 C 0.6032(2) 0.04023(15) 0.19124(16) 0.0259(4) Uani 1 1 d . . . H14 H 0.5206 0.0728 0.1700 0.031 Uiso 1 1 calc R . . C15 C 0.8106(3) 0.22952(18) 0.1404(3) 0.0553(8) Uani 1 1 d . . . H15 H 0.8175 0.2815 0.1916 0.066 Uiso 1 1 calc R . . C16 C 0.6318(2) 0.59304(17) 0.72928(19) 0.0393(6) Uani 1 1 d . . . H16A H 0.6492 0.6304 0.6731 0.059 Uiso 1 1 calc R . . H16B H 0.6263 0.6411 0.7832 0.059 Uiso 1 1 calc R . . H16C H 0.5489 0.5562 0.6967 0.059 Uiso 1 1 calc R . . C17 C 0.7392(3) 0.4316(2) 0.9059(2) 0.0488(7) Uani 1 1 d . . . H17A H 0.6532 0.3987 0.8774 0.073 Uiso 1 1 calc R . . H17B H 0.7431 0.4798 0.9628 0.073 Uiso 1 1 calc R . . H17C H 0.8071 0.3797 0.9358 0.073 Uiso 1 1 calc R . . C18 C 0.9091(2) 0.16219(18) 0.1411(2) 0.0425(6) Uani 1 1 d . . . H18 H 0.9960 0.1606 0.1936 0.051 Uiso 1 1 calc R . . C19 C 0.8587(3) 0.0985(2) 0.0523(2) 0.0451(6) Uani 1 1 d . . . H19 H 0.9058 0.0462 0.0341 0.054 Uiso 1 1 calc R . . C20 C 0.7300(3) 0.1227(2) -0.0054(2) 0.0514(7) Uani 1 1 d . . . H20 H 0.6735 0.0899 -0.0694 0.062 Uiso 1 1 calc R . . C21 C 0.6966(3) 0.2034(2) 0.0459(3) 0.0615(9) Uani 1 1 d . . . H21 H 0.6137 0.2357 0.0230 0.074 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 0.0282(2) 0.02701(18) 0.02319(19) 0.00098(11) 0.01343(14) -0.00012(11) Si1 0.0291(3) 0.0320(3) 0.0224(3) -0.0070(2) 0.0081(3) 0.0009(2) C1 0.0362(14) 0.0473(14) 0.0482(15) -0.0234(12) 0.0130(12) -0.0023(11) C2 0.0259(11) 0.0314(11) 0.0248(11) -0.0032(9) 0.0087(9) -0.0014(8) C3 0.0245(11) 0.0271(10) 0.0255(11) 0.0005(9) 0.0099(9) -0.0006(8) C4 0.0314(11) 0.0219(9) 0.0192(10) 0.0001(8) 0.0117(9) -0.0030(8) C5 0.0249(11) 0.0328(11) 0.0271(11) -0.0058(9) 0.0085(9) -0.0057(8) C6 0.0262(11) 0.0312(11) 0.0298(11) -0.0050(9) 0.0139(9) -0.0025(9) C7 0.0303(11) 0.0217(9) 0.0194(10) 0.0022(8) 0.0122(9) -0.0023(8) C8 0.0259(10) 0.0231(9) 0.0211(10) 0.0013(8) 0.0087(8) -0.0020(8) C9 0.0276(11) 0.0236(9) 0.0235(10) 0.0018(8) 0.0122(9) 0.0011(8) C10 0.0300(11) 0.0205(9) 0.0228(10) 0.0017(8) 0.0134(9) -0.0015(8) C11 0.0321(11) 0.0246(10) 0.0252(11) 0.0006(8) 0.0119(9) 0.0022(8) C12 0.0409(13) 0.0222(10) 0.0327(12) -0.0022(9) 0.0187(10) 0.0018(9) C13 0.0365(12) 0.0290(11) 0.0272(11) -0.0071(9) 0.0141(10) -0.0087(9) C14 0.0292(11) 0.0259(10) 0.0255(11) -0.0004(8) 0.0137(9) -0.0036(8) C15 0.097(2) 0.0256(12) 0.074(2) -0.0005(12) 0.067(2) -0.0095(13) C16 0.0381(14) 0.0418(13) 0.0345(13) -0.0079(10) 0.0103(11) 0.0082(10) C17 0.0642(18) 0.0554(16) 0.0278(13) -0.0014(11) 0.0187(13) 0.0001(13) C18 0.0346(13) 0.0481(14) 0.0471(15) 0.0119(12) 0.0182(11) -0.0072(11) C19 0.0534(16) 0.0504(14) 0.0454(15) 0.0049(12) 0.0344(14) 0.0018(12) C20 0.0561(18) 0.0677(18) 0.0333(14) 0.0115(13) 0.0204(13) -0.0068(14) C21 0.0415(16) 0.0677(19) 0.087(2) 0.0556(18) 0.0378(16) 0.0204(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C21 2.032(2) . ? Fe1 C15 2.041(2) . ? Fe1 C11 2.043(2) . ? Fe1 C20 2.043(2) . ? Fe1 C18 2.044(2) . ? Fe1 C13 2.047(2) . ? Fe1 C12 2.047(2) . ? Fe1 C19 2.049(2) . ? Fe1 C14 2.0491(19) . ? Fe1 C10 2.0575(19) . ? Si1 C2 1.847(2) . ? Si1 C1 1.854(2) . ? Si1 C16 1.855(2) . ? Si1 C17 1.862(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.206(3) . ? C3 C4 1.439(3) . ? C4 C5 1.398(3) . ? C4 C9 1.398(3) . ? C5 C6 1.377(3) . ? C5 H5 0.9500 . ? C6 C7 1.402(3) . ? C6 H6 0.9500 . ? C7 C8 1.394(3) . ? C7 C10 1.474(3) . ? C8 C9 1.385(3) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C14 1.429(3) . ? C10 C11 1.433(3) . ? C11 C12 1.424(3) . ? C11 H11 0.9500 . ? C12 C13 1.419(3) . ? C12 H12 0.9500 . ? C13 C14 1.423(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C18 1.404(4) . ? C15 C21 1.446(4) . ? C15 H15 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.385(4) . ? C18 H18 0.9500 . ? C19 C20 1.374(4) . ? C19 H19 0.9500 . ? C20 C21 1.390(4) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? 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 C21 Fe1 C15 41.58(12) . . ? C21 Fe1 C11 162.00(12) . . ? C15 Fe1 C11 124.19(11) . . ? C21 Fe1 C20 39.89(12) . . ? C15 Fe1 C20 68.24(12) . . ? C11 Fe1 C20 156.63(10) . . ? C21 Fe1 C18 67.77(10) . . ? C15 Fe1 C18 40.19(10) . . ? C11 Fe1 C18 108.58(9) . . ? C20 Fe1 C18 66.86(11) . . ? C21 Fe1 C13 121.97(11) . . ? C15 Fe1 C13 159.89(11) . . ? C11 Fe1 C13 68.48(9) . . ? C20 Fe1 C13 106.39(10) . . ? C18 Fe1 C13 157.27(10) . . ? C21 Fe1 C12 156.44(13) . . ? C15 Fe1 C12 159.05(12) . . ? C11 Fe1 C12 40.74(8) . . ? C20 Fe1 C12 120.62(11) . . ? C18 Fe1 C12 122.45(10) . . ? C13 Fe1 C12 40.56(9) . . ? C21 Fe1 C19 66.62(11) . . ? C15 Fe1 C19 67.26(10) . . ? C11 Fe1 C19 122.63(10) . . ? C20 Fe1 C19 39.23(11) . . ? C18 Fe1 C19 39.55(10) . . ? C13 Fe1 C19 121.63(10) . . ? C12 Fe1 C19 106.64(9) . . ? C21 Fe1 C14 108.92(9) . . ? C15 Fe1 C14 124.92(9) . . ? C11 Fe1 C14 68.47(8) . . ? C20 Fe1 C14 123.38(10) . . ? C18 Fe1 C14 161.16(9) . . ? C13 Fe1 C14 40.64(8) . . ? C12 Fe1 C14 68.31(8) . . ? C19 Fe1 C14 157.92(10) . . ? C21 Fe1 C10 125.52(11) . . ? C15 Fe1 C10 109.56(9) . . ? C11 Fe1 C10 40.91(8) . . ? C20 Fe1 C10 160.48(10) . . ? C18 Fe1 C10 124.87(9) . . ? C13 Fe1 C10 68.64(8) . . ? C12 Fe1 C10 68.68(8) . . ? C19 Fe1 C10 159.47(10) . . ? C14 Fe1 C10 40.74(8) . . ? C2 Si1 C1 108.92(10) . . ? C2 Si1 C16 106.85(10) . . ? C1 Si1 C16 110.24(12) . . ? C2 Si1 C17 108.03(11) . . ? C1 Si1 C17 111.81(13) . . ? C16 Si1 C17 110.81(12) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 Si1 176.95(19) . . ? C2 C3 C4 179.5(2) . . ? C5 C4 C9 118.19(18) . . ? C5 C4 C3 121.03(18) . . ? C9 C4 C3 120.78(18) . . ? C6 C5 C4 120.79(19) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 121.42(19) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C8 C7 C6 117.58(18) . . ? C8 C7 C10 121.38(18) . . ? C6 C7 C10 121.00(18) . . ? C9 C8 C7 121.31(18) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C8 C9 C4 120.70(18) . . ? C8 C9 H9 119.6 . . ? C4 C9 H9 119.6 . . ? C14 C10 C11 107.08(17) . . ? C14 C10 C7 126.70(18) . . ? C11 C10 C7 126.19(18) . . ? C14 C10 Fe1 69.31(11) . . ? C11 C10 Fe1 69.02(11) . . ? C7 C10 Fe1 128.39(13) . . ? C12 C11 C10 108.28(18) . . ? C12 C11 Fe1 69.77(12) . . ? C10 C11 Fe1 70.07(11) . . ? C12 C11 H11 125.9 . . ? C10 C11 H11 125.9 . . ? Fe1 C11 H11 125.9 . . ? C13 C12 C11 108.11(18) . . ? C13 C12 Fe1 69.73(12) . . ? C11 C12 Fe1 69.49(11) . . ? C13 C12 H12 125.9 . . ? C11 C12 H12 125.9 . . ? Fe1 C12 H12 126.4 . . ? C12 C13 C14 108.04(19) . . ? C12 C13 Fe1 69.71(11) . . ? C14 C13 Fe1 69.74(11) . . ? C12 C13 H13 126.0 . . ? C14 C13 H13 126.0 . . ? Fe1 C13 H13 126.2 . . ? C13 C14 C10 108.49(18) . . ? C13 C14 Fe1 69.62(11) . . ? C10 C14 Fe1 69.95(11) . . ? C13 C14 H14 125.8 . . ? C10 C14 H14 125.8 . . ? Fe1 C14 H14 126.3 . . ? C18 C15 C21 105.8(2) . . ? C18 C15 Fe1 70.04(13) . . ? C21 C15 Fe1 68.89(14) . . ? C18 C15 H15 127.1 . . ? C21 C15 H15 127.1 . . ? Fe1 C15 H15 125.6 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si1 C17 H17A 109.5 . . ? Si1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C15 108.6(2) . . ? C19 C18 Fe1 70.40(14) . . ? C15 C18 Fe1 69.77(13) . . ? C19 C18 H18 125.7 . . ? C15 C18 H18 125.7 . . ? Fe1 C18 H18 125.7 . . ? C20 C19 C18 109.4(2) . . ? C20 C19 Fe1 70.17(15) . . ? C18 C19 Fe1 70.05(14) . . ? C20 C19 H19 125.3 . . ? C18 C19 H19 125.3 . . ? Fe1 C19 H19 126.1 . . ? C19 C20 C21 108.4(3) . . ? C19 C20 Fe1 70.60(15) . . ? C21 C20 Fe1 69.63(15) . . ? C19 C20 H20 125.8 . . ? C21 C20 H20 125.8 . . ? Fe1 C20 H20 125.5 . . ? C20 C21 C15 107.7(2) . . ? C20 C21 Fe1 70.48(15) . . ? C15 C21 Fe1 69.52(14) . . ? C20 C21 H21 126.1 . . ? C15 C21 H21 126.1 . . ? Fe1 C21 H21 125.4 . . ? 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 C1 Si1 C2 C3 -125(4) . . . . ? C16 Si1 C2 C3 -6(4) . . . . ? C17 Si1 C2 C3 113(4) . . . . ? Si1 C2 C3 C4 122(31) . . . . ? C2 C3 C4 C5 27(32) . . . . ? C2 C3 C4 C9 -153(100) . . . . ? C9 C4 C5 C6 -0.4(3) . . . . ? C3 C4 C5 C6 179.97(19) . . . . ? C4 C5 C6 C7 -0.1(3) . . . . ? C5 C6 C7 C8 0.7(3) . . . . ? C5 C6 C7 C10 -177.03(18) . . . . ? C6 C7 C8 C9 -0.8(3) . . . . ? C10 C7 C8 C9 176.93(17) . . . . ? C7 C8 C9 C4 0.3(3) . . . . ? C5 C4 C9 C8 0.3(3) . . . . ? C3 C4 C9 C8 179.94(18) . . . . ? C8 C7 C10 C14 14.7(3) . . . . ? C6 C7 C10 C14 -167.64(19) . . . . ? C8 C7 C10 C11 -162.87(18) . . . . ? C6 C7 C10 C11 14.8(3) . . . . ? C8 C7 C10 Fe1 106.4(2) . . . . ? C6 C7 C10 Fe1 -76.0(2) . . . . ? C21 Fe1 C10 C14 77.40(16) . . . . ? C15 Fe1 C10 C14 121.21(14) . . . . ? C11 Fe1 C10 C14 -118.75(16) . . . . ? C20 Fe1 C10 C14 41.3(3) . . . . ? C18 Fe1 C10 C14 163.43(12) . . . . ? C13 Fe1 C10 C14 -37.40(12) . . . . ? C12 Fe1 C10 C14 -81.09(13) . . . . ? C19 Fe1 C10 C14 -161.5(2) . . . . ? C21 Fe1 C10 C11 -163.85(15) . . . . ? C15 Fe1 C10 C11 -120.04(14) . . . . ? C20 Fe1 C10 C11 160.0(3) . . . . ? C18 Fe1 C10 C11 -77.81(15) . . . . ? C13 Fe1 C10 C11 81.36(12) . . . . ? C12 Fe1 C10 C11 37.66(12) . . . . ? C19 Fe1 C10 C11 -42.8(3) . . . . ? C14 Fe1 C10 C11 118.75(16) . . . . ? C21 Fe1 C10 C7 -43.7(2) . . . . ? C15 Fe1 C10 C7 0.2(2) . . . . ? C11 Fe1 C10 C7 120.2(2) . . . . ? C20 Fe1 C10 C7 -79.8(4) . . . . ? C18 Fe1 C10 C7 42.4(2) . . . . ? C13 Fe1 C10 C7 -158.5(2) . . . . ? C12 Fe1 C10 C7 157.9(2) . . . . ? C19 Fe1 C10 C7 77.4(3) . . . . ? C14 Fe1 C10 C7 -121.1(2) . . . . ? C14 C10 C11 C12 -0.4(2) . . . . ? C7 C10 C11 C12 177.55(18) . . . . ? Fe1 C10 C11 C12 -59.53(14) . . . . ? C14 C10 C11 Fe1 59.09(13) . . . . ? C7 C10 C11 Fe1 -122.92(19) . . . . ? C21 Fe1 C11 C12 166.4(3) . . . . ? C15 Fe1 C11 C12 -160.26(14) . . . . ? C20 Fe1 C11 C12 -44.0(3) . . . . ? C18 Fe1 C11 C12 -118.50(14) . . . . ? C13 Fe1 C11 C12 37.49(12) . . . . ? C19 Fe1 C11 C12 -77.15(16) . . . . ? C14 Fe1 C11 C12 81.33(13) . . . . ? C10 Fe1 C11 C12 119.28(17) . . . . ? C21 Fe1 C11 C10 47.1(3) . . . . ? C15 Fe1 C11 C10 80.46(15) . . . . ? C20 Fe1 C11 C10 -163.3(2) . . . . ? C18 Fe1 C11 C10 122.21(13) . . . . ? C13 Fe1 C11 C10 -81.80(12) . . . . ? C12 Fe1 C11 C10 -119.28(17) . . . . ? C19 Fe1 C11 C10 163.57(13) . . . . ? C14 Fe1 C11 C10 -37.96(11) . . . . ? C10 C11 C12 C13 0.5(2) . . . . ? Fe1 C11 C12 C13 -59.24(14) . . . . ? C10 C11 C12 Fe1 59.72(13) . . . . ? C21 Fe1 C12 C13 -50.0(3) . . . . ? C15 Fe1 C12 C13 170.9(2) . . . . ? C11 Fe1 C12 C13 119.47(18) . . . . ? C20 Fe1 C12 C13 -79.21(16) . . . . ? C18 Fe1 C12 C13 -159.72(13) . . . . ? C19 Fe1 C12 C13 -119.51(14) . . . . ? C14 Fe1 C12 C13 37.71(12) . . . . ? C10 Fe1 C12 C13 81.65(13) . . . . ? C21 Fe1 C12 C11 -169.5(2) . . . . ? C15 Fe1 C12 C11 51.4(3) . . . . ? C20 Fe1 C12 C11 161.33(14) . . . . ? C18 Fe1 C12 C11 80.81(15) . . . . ? C13 Fe1 C12 C11 -119.47(18) . . . . ? C19 Fe1 C12 C11 121.02(14) . . . . ? C14 Fe1 C12 C11 -81.76(13) . . . . ? C10 Fe1 C12 C11 -37.82(12) . . . . ? C11 C12 C13 C14 -0.3(2) . . . . ? Fe1 C12 C13 C14 -59.42(14) . . . . ? C11 C12 C13 Fe1 59.09(14) . . . . ? C21 Fe1 C13 C12 158.83(15) . . . . ? C15 Fe1 C13 C12 -170.5(3) . . . . ? C11 Fe1 C13 C12 -37.65(12) . . . . ? C20 Fe1 C13 C12 118.22(14) . . . . ? C18 Fe1 C13 C12 49.2(3) . . . . ? C19 Fe1 C13 C12 78.32(16) . . . . ? C14 Fe1 C13 C12 -119.24(18) . . . . ? C10 Fe1 C13 C12 -81.75(13) . . . . ? C21 Fe1 C13 C14 -81.93(17) . . . . ? C15 Fe1 C13 C14 -51.2(3) . . . . ? C11 Fe1 C13 C14 81.59(13) . . . . ? C20 Fe1 C13 C14 -122.54(14) . . . . ? C18 Fe1 C13 C14 168.4(2) . . . . ? C12 Fe1 C13 C14 119.24(18) . . . . ? C19 Fe1 C13 C14 -162.44(13) . . . . ? C10 Fe1 C13 C14 37.49(12) . . . . ? C12 C13 C14 C10 0.1(2) . . . . ? Fe1 C13 C14 C10 -59.34(13) . . . . ? C12 C13 C14 Fe1 59.40(14) . . . . ? C11 C10 C14 C13 0.2(2) . . . . ? C7 C10 C14 C13 -177.74(18) . . . . ? Fe1 C10 C14 C13 59.14(14) . . . . ? C11 C10 C14 Fe1 -58.91(13) . . . . ? C7 C10 C14 Fe1 123.12(19) . . . . ? C21 Fe1 C14 C13 117.39(16) . . . . ? C15 Fe1 C14 C13 160.92(15) . . . . ? C11 Fe1 C14 C13 -81.61(13) . . . . ? C20 Fe1 C14 C13 75.59(17) . . . . ? C18 Fe1 C14 C13 -166.1(3) . . . . ? C12 Fe1 C14 C13 -37.64(13) . . . . ? C19 Fe1 C14 C13 43.1(3) . . . . ? C10 Fe1 C14 C13 -119.72(17) . . . . ? C21 Fe1 C14 C10 -122.89(15) . . . . ? C15 Fe1 C14 C10 -79.36(17) . . . . ? C11 Fe1 C14 C10 38.11(11) . . . . ? C20 Fe1 C14 C10 -164.69(14) . . . . ? C18 Fe1 C14 C10 -46.4(3) . . . . ? C13 Fe1 C14 C10 119.72(17) . . . . ? C12 Fe1 C14 C10 82.09(12) . . . . ? C19 Fe1 C14 C10 162.8(2) . . . . ? C21 Fe1 C15 C18 -116.8(2) . . . . ? C11 Fe1 C15 C18 78.03(18) . . . . ? C20 Fe1 C15 C18 -79.45(17) . . . . ? C13 Fe1 C15 C18 -157.5(2) . . . . ? C12 Fe1 C15 C18 40.0(3) . . . . ? C19 Fe1 C15 C18 -36.93(16) . . . . ? C14 Fe1 C15 C18 164.20(14) . . . . ? C10 Fe1 C15 C18 121.30(16) . . . . ? C11 Fe1 C15 C21 -165.16(15) . . . . ? C20 Fe1 C15 C21 37.36(16) . . . . ? C18 Fe1 C15 C21 116.8(2) . . . . ? C13 Fe1 C15 C21 -40.7(3) . . . . ? C12 Fe1 C15 C21 156.8(2) . . . . ? C19 Fe1 C15 C21 79.87(17) . . . . ? C14 Fe1 C15 C21 -78.99(18) . . . . ? C10 Fe1 C15 C21 -121.90(16) . . . . ? C21 C15 C18 C19 0.0(3) . . . . ? Fe1 C15 C18 C19 59.90(17) . . . . ? C21 C15 C18 Fe1 -59.93(15) . . . . ? C21 Fe1 C18 C19 -79.73(18) . . . . ? C15 Fe1 C18 C19 -119.5(2) . . . . ? C11 Fe1 C18 C19 119.10(15) . . . . ? C20 Fe1 C18 C19 -36.34(16) . . . . ? C13 Fe1 C18 C19 40.6(3) . . . . ? C12 Fe1 C18 C19 76.28(17) . . . . ? C14 Fe1 C18 C19 -163.2(3) . . . . ? C10 Fe1 C18 C19 161.58(14) . . . . ? C21 Fe1 C18 C15 39.79(18) . . . . ? C11 Fe1 C18 C15 -121.39(17) . . . . ? C20 Fe1 C18 C15 83.17(19) . . . . ? C13 Fe1 C18 C15 160.1(2) . . . . ? C12 Fe1 C18 C15 -164.20(16) . . . . ? C19 Fe1 C18 C15 119.5(2) . . . . ? C14 Fe1 C18 C15 -43.7(4) . . . . ? C10 Fe1 C18 C15 -78.90(19) . . . . ? C15 C18 C19 C20 -0.2(3) . . . . ? Fe1 C18 C19 C20 59.28(18) . . . . ? C15 C18 C19 Fe1 -59.51(16) . . . . ? C21 Fe1 C19 C20 -37.60(18) . . . . ? C15 Fe1 C19 C20 -82.98(19) . . . . ? C11 Fe1 C19 C20 159.94(16) . . . . ? C18 Fe1 C19 C20 -120.5(2) . . . . ? C13 Fe1 C19 C20 76.68(19) . . . . ? C12 Fe1 C19 C20 118.33(17) . . . . ? C14 Fe1 C19 C20 45.2(3) . . . . ? C10 Fe1 C19 C20 -168.2(2) . . . . ? C21 Fe1 C19 C18 82.89(18) . . . . ? C15 Fe1 C19 C18 37.51(16) . . . . ? C11 Fe1 C19 C18 -79.57(17) . . . . ? C20 Fe1 C19 C18 120.5(2) . . . . ? C13 Fe1 C19 C18 -162.83(14) . . . . ? C12 Fe1 C19 C18 -121.18(15) . . . . ? C14 Fe1 C19 C18 165.7(2) . . . . ? C10 Fe1 C19 C18 -47.7(3) . . . . ? C18 C19 C20 C21 0.4(3) . . . . ? Fe1 C19 C20 C21 59.61(17) . . . . ? C18 C19 C20 Fe1 -59.20(17) . . . . ? C21 Fe1 C20 C19 119.2(2) . . . . ? C15 Fe1 C20 C19 80.26(18) . . . . ? C11 Fe1 C20 C19 -46.7(3) . . . . ? C18 Fe1 C20 C19 36.64(16) . . . . ? C13 Fe1 C20 C19 -120.27(16) . . . . ? C12 Fe1 C20 C19 -78.53(18) . . . . ? C14 Fe1 C20 C19 -161.38(15) . . . . ? C10 Fe1 C20 C19 167.6(2) . . . . ? C15 Fe1 C20 C21 -38.90(17) . . . . ? C11 Fe1 C20 C21 -165.9(2) . . . . ? C18 Fe1 C20 C21 -82.52(18) . . . . ? C13 Fe1 C20 C21 120.58(17) . . . . ? C12 Fe1 C20 C21 162.32(16) . . . . ? C19 Fe1 C20 C21 -119.2(2) . . . . ? C14 Fe1 C20 C21 79.46(19) . . . . ? C10 Fe1 C20 C21 48.4(4) . . . . ? C19 C20 C21 C15 -0.4(3) . . . . ? Fe1 C20 C21 C15 59.80(16) . . . . ? C19 C20 C21 Fe1 -60.22(18) . . . . ? C18 C15 C21 C20 0.3(3) . . . . ? Fe1 C15 C21 C20 -60.41(17) . . . . ? C18 C15 C21 Fe1 60.69(16) . . . . ? C15 Fe1 C21 C20 118.5(2) . . . . ? C11 Fe1 C21 C20 161.8(3) . . . . ? C18 Fe1 C21 C20 80.04(17) . . . . ? C13 Fe1 C21 C20 -76.82(18) . . . . ? C12 Fe1 C21 C20 -40.8(3) . . . . ? C19 Fe1 C21 C20 36.99(16) . . . . ? C14 Fe1 C21 C20 -119.79(16) . . . . ? C10 Fe1 C21 C20 -162.12(15) . . . . ? C11 Fe1 C21 C15 43.3(4) . . . . ? C20 Fe1 C21 C15 -118.5(2) . . . . ? C18 Fe1 C21 C15 -38.48(15) . . . . ? C13 Fe1 C21 C15 164.67(13) . . . . ? C12 Fe1 C21 C15 -159.3(2) . . . . ? C19 Fe1 C21 C15 -81.53(16) . . . . ? C14 Fe1 C21 C15 121.69(14) . . . . ? C10 Fe1 C21 C15 79.37(16) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.448 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.056 _database_code_depnum_ccdc_archive 'CCDC 942661' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_rm049 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H13 Fe I' _chemical_formula_weight 412.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2384(3) _cell_length_b 10.6457(4) _cell_length_c 14.4194(5) _cell_angle_alpha 88.562(3) _cell_angle_beta 78.624(3) _cell_angle_gamma 69.948(3) _cell_volume 1445.82(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11315 _cell_measurement_theta_min 2.9696 _cell_measurement_theta_max 32.6423 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.893 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 3.164 _exptl_absorpt_correction_T_min 0.3955 _exptl_absorpt_correction_T_max 0.4712 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Micro-Focus (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION SUPER NOVA' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10272 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5081 _reflns_number_gt 4816 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.0222P)^2^+0.5292P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5081 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0190 _refine_ls_R_factor_gt 0.0178 _refine_ls_wR_factor_ref 0.0452 _refine_ls_wR_factor_gt 0.0443 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8071(2) 0.6765(2) 0.09940(15) 0.0205(5) Uani 1 1 d . . . C2 C 0.8157(2) 0.5809(2) 0.14762(15) 0.0207(5) Uani 1 1 d . . . C3 C 0.8240(2) 0.4729(2) 0.20991(14) 0.0192(4) Uani 1 1 d . . . C4 C 0.9505(2) 0.3658(2) 0.20773(15) 0.0218(5) Uani 1 1 d . . . H4 H 1.0319 0.3608 0.1609 0.026 Uiso 1 1 calc R . . C5 C 0.9592(2) 0.2666(2) 0.27283(15) 0.0216(5) Uani 1 1 d . . . H5 H 1.0456 0.1941 0.2708 0.026 Uiso 1 1 calc R . . C6 C 0.8400(2) 0.2746(2) 0.34090(14) 0.0179(4) Uani 1 1 d . . . C7 C 0.7122(2) 0.3771(2) 0.34263(15) 0.0224(5) Uani 1 1 d . . . H7 H 0.6304 0.3799 0.3884 0.027 Uiso 1 1 calc R . . C8 C 0.7041(2) 0.4759(2) 0.27712(15) 0.0233(5) Uani 1 1 d . . . H8 H 0.6163 0.5461 0.2780 0.028 Uiso 1 1 calc R . . C9 C 0.8019(2) 0.7863(2) 0.03985(14) 0.0186(4) Uani 1 1 d . . . C10 C 0.9127(2) 0.8409(2) 0.01151(15) 0.0208(4) Uani 1 1 d . . . H10 H 1.0023 0.8109 0.0297 0.025 Uiso 1 1 calc R . . C11 C 0.8656(2) 0.9473(2) -0.04831(15) 0.0236(5) Uani 1 1 d . . . H11 H 0.9185 1.0006 -0.0777 0.028 Uiso 1 1 calc R . . C12 C 0.7256(2) 0.9609(2) -0.05705(14) 0.0243(5) Uani 1 1 d . . . H12 H 0.6689 1.0251 -0.0931 0.029 Uiso 1 1 calc R . . C13 C 0.6848(2) 0.8624(2) -0.00282(15) 0.0211(4) Uani 1 1 d . . . H13 H 0.5963 0.8492 0.0041 0.025 Uiso 1 1 calc R . . C14 C 0.7810(2) 1.0457(2) 0.20068(16) 0.0282(5) Uani 1 1 d . . . H14 H 0.8694 1.0103 0.2203 0.034 Uiso 1 1 calc R . . C15 C 0.7421(2) 1.1545(2) 0.14072(16) 0.0267(5) Uani 1 1 d . . . H15 H 0.7995 1.2048 0.1134 0.032 Uiso 1 1 calc R . . C16 C 0.6021(2) 1.1747(2) 0.12881(16) 0.0262(5) Uani 1 1 d . . . H16 H 0.5494 1.2406 0.0918 0.031 Uiso 1 1 calc R . . C17 C 0.5547(2) 1.0789(2) 0.18200(15) 0.0282(5) Uani 1 1 d . . . H17 H 0.4644 1.0699 0.1871 0.034 Uiso 1 1 calc R . . C18 C 0.6649(3) 0.9992(2) 0.22611(15) 0.0284(5) Uani 1 1 d . . . H18 H 0.6619 0.9272 0.2658 0.034 Uiso 1 1 calc R . . C19 C 0.3030(2) 1.0402(2) 0.38542(15) 0.0200(4) Uani 1 1 d . . . C20 C 0.2946(2) 0.9566(2) 0.33467(14) 0.0208(5) Uani 1 1 d . . . C21 C 0.2879(2) 0.8552(2) 0.27425(14) 0.0188(4) Uani 1 1 d . . . C22 C 0.1586(2) 0.8357(2) 0.27542(15) 0.0238(5) Uani 1 1 d . . . H22 H 0.0757 0.8879 0.3186 0.029 Uiso 1 1 calc R . . C23 C 0.1505(2) 0.7416(2) 0.21444(15) 0.0235(5) Uani 1 1 d . . . H23 H 0.0625 0.7297 0.2152 0.028 Uiso 1 1 calc R . . C24 C 0.2722(2) 0.6647(2) 0.15206(15) 0.0211(4) Uani 1 1 d . . . C25 C 0.4014(2) 0.6795(2) 0.15140(15) 0.0222(5) Uani 1 1 d . . . H25 H 0.4844 0.6249 0.1094 0.027 Uiso 1 1 calc R . . C26 C 0.4090(2) 0.7742(2) 0.21215(15) 0.0212(4) Uani 1 1 d . . . H26 H 0.4979 0.7842 0.2116 0.025 Uiso 1 1 calc R . . C27 C 0.3118(2) 1.1325(2) 0.45159(15) 0.0196(4) Uani 1 1 d . . . C28 C 0.1977(2) 1.2135(2) 0.52367(15) 0.0232(5) Uani 1 1 d . . . H28 H 0.1016 1.2181 0.5339 0.028 Uiso 1 1 calc R . . C29 C 0.2537(2) 1.2855(2) 0.57689(16) 0.0267(5) Uani 1 1 d . . . H29 H 0.2015 1.3464 0.6292 0.032 Uiso 1 1 calc R . . C30 C 0.4014(2) 1.2511(2) 0.53867(16) 0.0274(5) Uani 1 1 d . . . H30 H 0.4647 1.2849 0.5611 0.033 Uiso 1 1 calc R . . C31 C 0.4377(2) 1.1575(2) 0.46124(16) 0.0237(5) Uani 1 1 d . . . H31 H 0.5293 1.1182 0.4226 0.028 Uiso 1 1 calc R . . C32 C 0.1303(2) 1.4547(2) 0.37206(16) 0.0263(5) Uani 1 1 d . . . H32 H 0.0359 1.4551 0.3795 0.032 Uiso 1 1 calc R . . C33 C 0.1778(2) 1.5314(2) 0.42727(16) 0.0267(5) Uani 1 1 d . . . H33 H 0.1208 1.5923 0.4786 0.032 Uiso 1 1 calc R . . C34 C 0.3257(2) 1.5018(2) 0.39296(16) 0.0265(5) Uani 1 1 d . . . H34 H 0.3849 1.5393 0.4170 0.032 Uiso 1 1 calc R . . C35 C 0.3688(2) 1.4059(2) 0.31615(16) 0.0256(5) Uani 1 1 d . . . H35 H 0.4622 1.3680 0.2797 0.031 Uiso 1 1 calc R . . C36 C 0.2490(2) 1.3766(2) 0.30325(16) 0.0248(5) Uani 1 1 d . . . H36 H 0.2478 1.3154 0.2568 0.030 Uiso 1 1 calc R . . Fe1 Fe 0.73320(3) 0.98448(3) 0.08215(2) 0.01654(7) Uani 1 1 d . . . Fe2 Fe 0.28516(3) 1.33109(3) 0.43689(2) 0.01828(7) Uani 1 1 d . . . I1 I 0.845998(14) 0.132840(14) 0.445001(9) 0.02164(5) Uani 1 1 d . . . I2 I 0.255654(15) 0.529870(14) 0.054880(10) 0.02538(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0223(10) 0.0192(11) 0.0200(11) -0.0041(9) -0.0033(8) -0.0074(9) C2 0.0253(11) 0.0200(11) 0.0191(10) -0.0022(9) -0.0048(9) -0.0104(9) C3 0.0281(11) 0.0165(10) 0.0177(10) 0.0005(8) -0.0089(8) -0.0111(9) C4 0.0232(11) 0.0228(12) 0.0207(11) 0.0002(9) -0.0025(9) -0.0105(9) C5 0.0192(10) 0.0202(11) 0.0256(11) 0.0011(9) -0.0052(9) -0.0065(9) C6 0.0247(10) 0.0155(10) 0.0169(10) 0.0006(8) -0.0077(8) -0.0092(9) C7 0.0247(11) 0.0213(11) 0.0193(11) 0.0012(9) -0.0011(9) -0.0074(9) C8 0.0234(11) 0.0209(11) 0.0236(11) 0.0009(9) -0.0059(9) -0.0044(9) C9 0.0253(10) 0.0158(10) 0.0148(10) -0.0010(8) -0.0033(8) -0.0073(9) C10 0.0213(10) 0.0200(11) 0.0195(10) -0.0030(9) -0.0011(8) -0.0064(9) C11 0.0303(11) 0.0200(11) 0.0186(11) -0.0015(9) 0.0039(9) -0.0109(9) C12 0.0357(12) 0.0198(11) 0.0158(10) 0.0010(9) -0.0086(9) -0.0056(10) C13 0.0243(11) 0.0213(11) 0.0197(11) -0.0024(9) -0.0078(8) -0.0082(9) C14 0.0323(12) 0.0289(13) 0.0227(11) -0.0096(10) -0.0087(10) -0.0070(10) C15 0.0313(12) 0.0221(12) 0.0275(12) -0.0094(10) 0.0013(10) -0.0134(10) C16 0.0296(12) 0.0163(11) 0.0276(12) -0.0055(9) -0.0052(9) -0.0016(9) C17 0.0248(11) 0.0297(13) 0.0268(12) -0.0116(10) 0.0045(9) -0.0097(10) C18 0.0429(13) 0.0264(13) 0.0151(11) -0.0043(9) 0.0004(10) -0.0140(11) C19 0.0224(10) 0.0173(11) 0.0201(11) 0.0029(9) -0.0039(8) -0.0071(9) C20 0.0246(11) 0.0184(11) 0.0180(10) 0.0020(9) -0.0030(8) -0.0066(9) C21 0.0273(11) 0.0149(10) 0.0148(10) 0.0019(8) -0.0051(8) -0.0075(9) C22 0.0239(11) 0.0225(12) 0.0204(11) -0.0046(9) 0.0010(9) -0.0046(9) C23 0.0236(11) 0.0229(12) 0.0240(11) -0.0023(9) -0.0054(9) -0.0073(9) C24 0.0307(11) 0.0157(10) 0.0168(10) -0.0006(8) -0.0077(9) -0.0064(9) C25 0.0234(11) 0.0186(11) 0.0211(11) -0.0036(9) -0.0014(9) -0.0040(9) C26 0.0218(10) 0.0189(11) 0.0228(11) 0.0024(9) -0.0054(9) -0.0066(9) C27 0.0261(10) 0.0130(10) 0.0202(10) 0.0017(8) -0.0064(8) -0.0064(9) C28 0.0293(11) 0.0197(11) 0.0214(11) 0.0025(9) -0.0046(9) -0.0096(9) C29 0.0386(13) 0.0214(12) 0.0188(11) -0.0015(9) -0.0046(9) -0.0094(10) C30 0.0354(12) 0.0236(12) 0.0286(12) 0.0010(10) -0.0158(10) -0.0116(10) C31 0.0247(11) 0.0192(11) 0.0272(12) -0.0014(9) -0.0076(9) -0.0060(9) C32 0.0222(11) 0.0224(12) 0.0333(13) 0.0054(10) -0.0081(9) -0.0055(9) C33 0.0298(12) 0.0160(11) 0.0305(12) -0.0014(9) -0.0022(10) -0.0048(9) C34 0.0322(12) 0.0198(11) 0.0302(12) 0.0010(10) -0.0049(10) -0.0129(10) C35 0.0291(11) 0.0218(12) 0.0249(11) 0.0034(9) -0.0019(9) -0.0098(10) C36 0.0311(12) 0.0232(12) 0.0218(11) 0.0025(9) -0.0074(9) -0.0105(10) Fe1 0.02004(15) 0.01453(15) 0.01544(15) -0.00090(12) -0.00302(11) -0.00664(12) Fe2 0.02071(15) 0.01425(15) 0.02006(16) -0.00205(12) -0.00374(12) -0.00627(12) I1 0.02927(8) 0.01801(8) 0.01895(8) 0.00411(6) -0.00645(6) -0.00916(6) I2 0.03034(9) 0.02175(9) 0.02324(8) -0.00786(6) -0.00480(6) -0.00766(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.206(3) . ? C1 C9 1.426(3) . ? C2 C3 1.431(3) . ? C3 C4 1.397(3) . ? C3 C8 1.398(3) . ? C4 C5 1.387(3) . ? C4 H4 0.9500 . ? C5 C6 1.386(3) . ? C5 H5 0.9500 . ? C6 C7 1.383(3) . ? C6 I1 2.096(2) . ? C7 C8 1.388(3) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.432(3) . ? C9 C13 1.439(3) . ? C9 Fe1 2.048(2) . ? C10 C11 1.414(3) . ? C10 Fe1 2.041(2) . ? C10 H10 0.9500 . ? C11 C12 1.421(3) . ? C11 Fe1 2.048(2) . ? C11 H11 0.9500 . ? C12 C13 1.419(3) . ? C12 Fe1 2.049(2) . ? C12 H12 0.9500 . ? C13 Fe1 2.048(2) . ? C13 H13 0.9500 . ? C14 C18 1.420(3) . ? C14 C15 1.420(3) . ? C14 Fe1 2.047(2) . ? C14 H14 0.9500 . ? C15 C16 1.419(3) . ? C15 Fe1 2.054(2) . ? C15 H15 0.9500 . ? C16 C17 1.420(3) . ? C16 Fe1 2.050(2) . ? C16 H16 0.9500 . ? C17 C18 1.413(3) . ? C17 Fe1 2.049(2) . ? C17 H17 0.9500 . ? C18 Fe1 2.047(2) . ? C18 H18 0.9500 . ? C19 C20 1.203(3) . ? C19 C27 1.423(3) . ? C20 C21 1.432(3) . ? C21 C26 1.397(3) . ? C21 C22 1.405(3) . ? C22 C23 1.383(3) . ? C22 H22 0.9500 . ? C23 C24 1.388(3) . ? C23 H23 0.9500 . ? C24 C25 1.383(3) . ? C24 I2 2.101(2) . ? C25 C26 1.384(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C31 1.435(3) . ? C27 C28 1.436(3) . ? C27 Fe2 2.048(2) . ? C28 C29 1.418(3) . ? C28 Fe2 2.045(2) . ? C28 H28 0.9500 . ? C29 C30 1.423(3) . ? C29 Fe2 2.053(2) . ? C29 H29 0.9500 . ? C30 C31 1.420(3) . ? C30 Fe2 2.056(2) . ? C30 H30 0.9500 . ? C31 Fe2 2.045(2) . ? C31 H31 0.9500 . ? C32 C33 1.412(3) . ? C32 C36 1.423(3) . ? C32 Fe2 2.052(2) . ? C32 H32 0.9500 . ? C33 C34 1.422(3) . ? C33 Fe2 2.052(2) . ? C33 H33 0.9500 . ? C34 C35 1.421(3) . ? C34 Fe2 2.057(2) . ? C34 H34 0.9500 . ? C35 C36 1.411(3) . ? C35 Fe2 2.051(2) . ? C35 H35 0.9500 . ? C36 Fe2 2.049(2) . ? C36 H36 0.9500 . ? 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 C1 C9 177.7(2) . . ? C1 C2 C3 176.4(2) . . ? C4 C3 C8 118.59(19) . . ? C4 C3 C2 121.80(19) . . ? C8 C3 C2 119.57(19) . . ? C5 C4 C3 121.07(19) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C6 C5 C4 119.09(19) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C7 C6 C5 121.01(19) . . ? C7 C6 I1 117.46(15) . . ? C5 C6 I1 121.52(15) . . ? C6 C7 C8 119.57(19) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C7 C8 C3 120.59(19) . . ? C7 C8 H8 119.7 . . ? C3 C8 H8 119.7 . . ? C1 C9 C10 126.06(19) . . ? C1 C9 C13 126.4(2) . . ? C10 C9 C13 107.49(18) . . ? C1 C9 Fe1 126.71(15) . . ? C10 C9 Fe1 69.22(12) . . ? C13 C9 Fe1 69.44(12) . . ? C11 C10 C9 108.10(19) . . ? C11 C10 Fe1 70.06(12) . . ? C9 C10 Fe1 69.78(11) . . ? C11 C10 H10 125.9 . . ? C9 C10 H10 125.9 . . ? Fe1 C10 H10 125.8 . . ? C10 C11 C12 108.36(19) . . ? C10 C11 Fe1 69.47(12) . . ? C12 C11 Fe1 69.73(12) . . ? C10 C11 H11 125.8 . . ? C12 C11 H11 125.8 . . ? Fe1 C11 H11 126.6 . . ? C13 C12 C11 108.42(19) . . ? C13 C12 Fe1 69.70(12) . . ? C11 C12 Fe1 69.69(12) . . ? C13 C12 H12 125.8 . . ? C11 C12 H12 125.8 . . ? Fe1 C12 H12 126.4 . . ? C12 C13 C9 107.62(19) . . ? C12 C13 Fe1 69.76(13) . . ? C9 C13 Fe1 69.43(12) . . ? C12 C13 H13 126.2 . . ? C9 C13 H13 126.2 . . ? Fe1 C13 H13 126.2 . . ? C18 C14 C15 108.1(2) . . ? C18 C14 Fe1 69.71(13) . . ? C15 C14 Fe1 69.98(13) . . ? C18 C14 H14 126.0 . . ? C15 C14 H14 126.0 . . ? Fe1 C14 H14 125.9 . . ? C16 C15 C14 107.9(2) . . ? C16 C15 Fe1 69.65(13) . . ? C14 C15 Fe1 69.49(13) . . ? C16 C15 H15 126.1 . . ? C14 C15 H15 126.1 . . ? Fe1 C15 H15 126.4 . . ? C15 C16 C17 107.8(2) . . ? C15 C16 Fe1 69.89(13) . . ? C17 C16 Fe1 69.67(12) . . ? C15 C16 H16 126.1 . . ? C17 C16 H16 126.1 . . ? Fe1 C16 H16 125.9 . . ? C18 C17 C16 108.3(2) . . ? C18 C17 Fe1 69.76(12) . . ? C16 C17 Fe1 69.80(12) . . ? C18 C17 H17 125.8 . . ? C16 C17 H17 125.8 . . ? Fe1 C17 H17 126.2 . . ? C17 C18 C14 107.9(2) . . ? C17 C18 Fe1 69.87(12) . . ? C14 C18 Fe1 69.70(13) . . ? C17 C18 H18 126.1 . . ? C14 C18 H18 126.1 . . ? Fe1 C18 H18 125.9 . . ? C20 C19 C27 175.4(2) . . ? C19 C20 C21 178.7(2) . . ? C26 C21 C22 118.4(2) . . ? C26 C21 C20 120.96(19) . . ? C22 C21 C20 120.65(19) . . ? C23 C22 C21 120.81(19) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C22 C23 C24 119.4(2) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? C25 C24 C23 120.8(2) . . ? C25 C24 I2 120.33(15) . . ? C23 C24 I2 118.85(16) . . ? C24 C25 C26 119.7(2) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C25 C26 C21 120.9(2) . . ? C25 C26 H26 119.6 . . ? C21 C26 H26 119.6 . . ? C19 C27 C31 126.24(19) . . ? C19 C27 C28 126.4(2) . . ? C31 C27 C28 107.34(19) . . ? C19 C27 Fe2 128.49(15) . . ? C31 C27 Fe2 69.36(12) . . ? C28 C27 Fe2 69.34(12) . . ? C29 C28 C27 108.0(2) . . ? C29 C28 Fe2 70.07(13) . . ? C27 C28 Fe2 69.57(12) . . ? C29 C28 H28 126.0 . . ? C27 C28 H28 126.0 . . ? Fe2 C28 H28 125.9 . . ? C28 C29 C30 108.4(2) . . ? C28 C29 Fe2 69.45(13) . . ? C30 C29 Fe2 69.83(13) . . ? C28 C29 H29 125.8 . . ? C30 C29 H29 125.8 . . ? Fe2 C29 H29 126.5 . . ? C31 C30 C29 108.1(2) . . ? C31 C30 Fe2 69.33(13) . . ? C29 C30 Fe2 69.63(13) . . ? C31 C30 H30 125.9 . . ? C29 C30 H30 125.9 . . ? Fe2 C30 H30 126.7 . . ? C30 C31 C27 108.10(19) . . ? C30 C31 Fe2 70.16(13) . . ? C27 C31 Fe2 69.59(12) . . ? C30 C31 H31 126.0 . . ? C27 C31 H31 126.0 . . ? Fe2 C31 H31 125.9 . . ? C33 C32 C36 107.9(2) . . ? C33 C32 Fe2 69.88(13) . . ? C36 C32 Fe2 69.57(12) . . ? C33 C32 H32 126.0 . . ? C36 C32 H32 126.0 . . ? Fe2 C32 H32 126.1 . . ? C32 C33 C34 108.3(2) . . ? C32 C33 Fe2 69.86(13) . . ? C34 C33 Fe2 69.94(13) . . ? C32 C33 H33 125.9 . . ? C34 C33 H33 125.9 . . ? Fe2 C33 H33 125.9 . . ? C35 C34 C33 107.5(2) . . ? C35 C34 Fe2 69.55(13) . . ? C33 C34 Fe2 69.56(13) . . ? C35 C34 H34 126.3 . . ? C33 C34 H34 126.3 . . ? Fe2 C34 H34 126.2 . . ? C36 C35 C34 108.4(2) . . ? C36 C35 Fe2 69.76(12) . . ? C34 C35 Fe2 69.99(13) . . ? C36 C35 H35 125.8 . . ? C34 C35 H35 125.8 . . ? Fe2 C35 H35 126.0 . . ? C35 C36 C32 107.9(2) . . ? C35 C36 Fe2 69.98(13) . . ? C32 C36 Fe2 69.82(13) . . ? C35 C36 H36 126.0 . . ? C32 C36 H36 126.0 . . ? Fe2 C36 H36 125.8 . . ? C10 Fe1 C14 107.33(9) . . ? C10 Fe1 C18 124.46(9) . . ? C14 Fe1 C18 40.58(10) . . ? C10 Fe1 C9 41.00(8) . . ? C14 Fe1 C9 121.54(9) . . ? C18 Fe1 C9 107.83(9) . . ? C10 Fe1 C13 68.97(9) . . ? C14 Fe1 C13 157.49(10) . . ? C18 Fe1 C13 121.99(9) . . ? C9 Fe1 C13 41.13(8) . . ? C10 Fe1 C11 40.47(9) . . ? C14 Fe1 C11 124.01(9) . . ? C18 Fe1 C11 160.81(10) . . ? C9 Fe1 C11 68.46(8) . . ? C13 Fe1 C11 68.45(9) . . ? C10 Fe1 C17 161.38(9) . . ? C14 Fe1 C17 67.99(9) . . ? C18 Fe1 C17 40.37(10) . . ? C9 Fe1 C17 124.74(9) . . ? C13 Fe1 C17 108.03(9) . . ? C11 Fe1 C17 157.11(9) . . ? C10 Fe1 C12 68.41(9) . . ? C14 Fe1 C12 160.57(10) . . ? C18 Fe1 C12 157.36(10) . . ? C9 Fe1 C12 68.54(9) . . ? C13 Fe1 C12 40.54(9) . . ? C11 Fe1 C12 40.58(9) . . ? C17 Fe1 C12 122.05(9) . . ? C10 Fe1 C16 156.33(9) . . ? C14 Fe1 C16 68.14(9) . . ? C18 Fe1 C16 68.19(10) . . ? C9 Fe1 C16 161.35(9) . . ? C13 Fe1 C16 124.22(9) . . ? C11 Fe1 C16 121.38(9) . . ? C17 Fe1 C16 40.54(9) . . ? C12 Fe1 C16 107.70(9) . . ? C10 Fe1 C15 120.98(9) . . ? C14 Fe1 C15 40.52(10) . . ? C18 Fe1 C15 68.19(9) . . ? C9 Fe1 C15 156.78(9) . . ? C13 Fe1 C15 160.58(9) . . ? C11 Fe1 C15 107.36(9) . . ? C17 Fe1 C15 68.02(9) . . ? C12 Fe1 C15 124.08(9) . . ? C16 Fe1 C15 40.47(9) . . ? C31 Fe2 C28 68.89(9) . . ? C31 Fe2 C27 41.06(9) . . ? C28 Fe2 C27 41.09(9) . . ? C31 Fe2 C36 121.38(9) . . ? C28 Fe2 C36 124.13(9) . . ? C27 Fe2 C36 107.09(9) . . ? C31 Fe2 C35 107.36(9) . . ? C28 Fe2 C35 160.53(9) . . ? C27 Fe2 C35 123.63(9) . . ? C36 Fe2 C35 40.26(9) . . ? C31 Fe2 C32 157.22(9) . . ? C28 Fe2 C32 107.71(9) . . ? C27 Fe2 C32 121.56(9) . . ? C36 Fe2 C32 40.61(9) . . ? C35 Fe2 C32 67.92(9) . . ? C31 Fe2 C33 160.70(9) . . ? C28 Fe2 C33 121.88(9) . . ? C27 Fe2 C33 157.23(9) . . ? C36 Fe2 C33 67.98(9) . . ? C35 Fe2 C33 67.92(9) . . ? C32 Fe2 C33 40.26(10) . . ? C31 Fe2 C29 68.36(9) . . ? C28 Fe2 C29 40.48(9) . . ? C27 Fe2 C29 68.53(9) . . ? C36 Fe2 C29 160.90(9) . . ? C35 Fe2 C29 157.60(10) . . ? C32 Fe2 C29 124.57(9) . . ? C33 Fe2 C29 108.43(9) . . ? C31 Fe2 C30 40.52(9) . . ? C28 Fe2 C30 68.38(9) . . ? C27 Fe2 C30 68.56(9) . . ? C36 Fe2 C30 156.97(9) . . ? C35 Fe2 C30 121.99(10) . . ? C32 Fe2 C30 161.01(9) . . ? C33 Fe2 C30 124.75(10) . . ? C29 Fe2 C30 40.53(9) . . ? C31 Fe2 C34 123.85(9) . . ? C28 Fe2 C34 157.40(9) . . ? C27 Fe2 C34 160.35(9) . . ? C36 Fe2 C34 68.02(10) . . ? C35 Fe2 C34 40.46(9) . . ? C32 Fe2 C34 67.99(10) . . ? C33 Fe2 C34 40.50(9) . . ? C29 Fe2 C34 122.32(9) . . ? C30 Fe2 C34 108.05(10) . . ? 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 C1 C2 C3 136(5) . . . . ? C1 C2 C3 C4 -116(4) . . . . ? C1 C2 C3 C8 62(4) . . . . ? C8 C3 C4 C5 -2.3(3) . . . . ? C2 C3 C4 C5 175.6(2) . . . . ? C3 C4 C5 C6 0.0(3) . . . . ? C4 C5 C6 C7 2.3(3) . . . . ? C4 C5 C6 I1 -177.69(16) . . . . ? C5 C6 C7 C8 -2.1(3) . . . . ? I1 C6 C7 C8 177.85(17) . . . . ? C6 C7 C8 C3 -0.3(3) . . . . ? C4 C3 C8 C7 2.5(3) . . . . ? C2 C3 C8 C7 -175.5(2) . . . . ? C2 C1 C9 C10 -56(6) . . . . ? C2 C1 C9 C13 124(6) . . . . ? C2 C1 C9 Fe1 -146(6) . . . . ? C1 C9 C10 C11 179.21(19) . . . . ? C13 C9 C10 C11 -0.7(2) . . . . ? Fe1 C9 C10 C11 -59.81(15) . . . . ? C1 C9 C10 Fe1 -121.0(2) . . . . ? C13 C9 C10 Fe1 59.11(14) . . . . ? C9 C10 C11 C12 0.6(2) . . . . ? Fe1 C10 C11 C12 -59.07(15) . . . . ? C9 C10 C11 Fe1 59.64(14) . . . . ? C10 C11 C12 C13 -0.2(2) . . . . ? Fe1 C11 C12 C13 -59.12(15) . . . . ? C10 C11 C12 Fe1 58.90(15) . . . . ? C11 C12 C13 C9 -0.2(2) . . . . ? Fe1 C12 C13 C9 -59.34(14) . . . . ? C11 C12 C13 Fe1 59.11(15) . . . . ? C1 C9 C13 C12 -179.3(2) . . . . ? C10 C9 C13 C12 0.6(2) . . . . ? Fe1 C9 C13 C12 59.54(15) . . . . ? C1 C9 C13 Fe1 121.1(2) . . . . ? C10 C9 C13 Fe1 -58.97(14) . . . . ? C18 C14 C15 C16 -0.2(3) . . . . ? Fe1 C14 C15 C16 59.28(16) . . . . ? C18 C14 C15 Fe1 -59.52(15) . . . . ? C14 C15 C16 C17 0.4(3) . . . . ? Fe1 C15 C16 C17 59.57(15) . . . . ? C14 C15 C16 Fe1 -59.18(15) . . . . ? C15 C16 C17 C18 -0.4(2) . . . . ? Fe1 C16 C17 C18 59.32(15) . . . . ? C15 C16 C17 Fe1 -59.71(15) . . . . ? C16 C17 C18 C14 0.2(2) . . . . ? Fe1 C17 C18 C14 59.58(15) . . . . ? C16 C17 C18 Fe1 -59.34(15) . . . . ? C15 C14 C18 C17 0.0(3) . . . . ? Fe1 C14 C18 C17 -59.69(15) . . . . ? C15 C14 C18 Fe1 59.69(15) . . . . ? C27 C19 C20 C21 -77(11) . . . . ? C19 C20 C21 C26 -29(10) . . . . ? C19 C20 C21 C22 151(10) . . . . ? C26 C21 C22 C23 -2.0(3) . . . . ? C20 C21 C22 C23 177.3(2) . . . . ? C21 C22 C23 C24 0.6(3) . . . . ? C22 C23 C24 C25 1.1(3) . . . . ? C22 C23 C24 I2 -176.64(16) . . . . ? C23 C24 C25 C26 -1.5(3) . . . . ? I2 C24 C25 C26 176.30(16) . . . . ? C24 C25 C26 C21 0.0(3) . . . . ? C22 C21 C26 C25 1.7(3) . . . . ? C20 C21 C26 C25 -177.6(2) . . . . ? C20 C19 C27 C31 106(3) . . . . ? C20 C19 C27 C28 -71(3) . . . . ? C20 C19 C27 Fe2 -163(3) . . . . ? C19 C27 C28 C29 177.0(2) . . . . ? C31 C27 C28 C29 -0.6(2) . . . . ? Fe2 C27 C28 C29 -59.77(15) . . . . ? C19 C27 C28 Fe2 -123.3(2) . . . . ? C31 C27 C28 Fe2 59.18(14) . . . . ? C27 C28 C29 C30 0.3(3) . . . . ? Fe2 C28 C29 C30 -59.14(16) . . . . ? C27 C28 C29 Fe2 59.46(15) . . . . ? C28 C29 C30 C31 0.1(3) . . . . ? Fe2 C29 C30 C31 -58.81(16) . . . . ? C28 C29 C30 Fe2 58.90(16) . . . . ? C29 C30 C31 C27 -0.5(3) . . . . ? Fe2 C30 C31 C27 -59.46(15) . . . . ? C29 C30 C31 Fe2 59.00(16) . . . . ? C19 C27 C31 C30 -176.9(2) . . . . ? C28 C27 C31 C30 0.7(2) . . . . ? Fe2 C27 C31 C30 59.82(15) . . . . ? C19 C27 C31 Fe2 123.3(2) . . . . ? C28 C27 C31 Fe2 -59.17(14) . . . . ? C36 C32 C33 C34 0.2(3) . . . . ? Fe2 C32 C33 C34 59.60(16) . . . . ? C36 C32 C33 Fe2 -59.40(16) . . . . ? C32 C33 C34 C35 -0.1(3) . . . . ? Fe2 C33 C34 C35 59.46(16) . . . . ? C32 C33 C34 Fe2 -59.55(16) . . . . ? C33 C34 C35 C36 -0.1(3) . . . . ? Fe2 C34 C35 C36 59.41(16) . . . . ? C33 C34 C35 Fe2 -59.47(16) . . . . ? C34 C35 C36 C32 0.2(3) . . . . ? Fe2 C35 C36 C32 59.73(15) . . . . ? C34 C35 C36 Fe2 -59.55(16) . . . . ? C33 C32 C36 C35 -0.2(3) . . . . ? Fe2 C32 C36 C35 -59.83(15) . . . . ? C33 C32 C36 Fe2 59.59(16) . . . . ? C11 C10 Fe1 C14 -122.49(14) . . . . ? C9 C10 Fe1 C14 118.44(13) . . . . ? C11 C10 Fe1 C18 -163.83(14) . . . . ? C9 C10 Fe1 C18 77.10(15) . . . . ? C11 C10 Fe1 C9 119.07(18) . . . . ? C11 C10 Fe1 C13 81.04(14) . . . . ? C9 C10 Fe1 C13 -38.03(12) . . . . ? C9 C10 Fe1 C11 -119.07(18) . . . . ? C11 C10 Fe1 C17 165.2(3) . . . . ? C9 C10 Fe1 C17 46.1(3) . . . . ? C11 C10 Fe1 C12 37.38(13) . . . . ? C9 C10 Fe1 C12 -81.69(13) . . . . ? C11 C10 Fe1 C16 -47.5(3) . . . . ? C9 C10 Fe1 C16 -166.6(2) . . . . ? C11 C10 Fe1 C15 -80.35(15) . . . . ? C9 C10 Fe1 C15 160.58(12) . . . . ? C18 C14 Fe1 C10 -123.15(14) . . . . ? C15 C14 Fe1 C10 117.71(13) . . . . ? C15 C14 Fe1 C18 -119.14(19) . . . . ? C18 C14 Fe1 C9 -80.56(15) . . . . ? C15 C14 Fe1 C9 160.30(13) . . . . ? C18 C14 Fe1 C13 -46.4(3) . . . . ? C15 C14 Fe1 C13 -165.5(2) . . . . ? C18 C14 Fe1 C11 -164.49(13) . . . . ? C15 C14 Fe1 C11 76.37(15) . . . . ? C18 C14 Fe1 C17 37.69(14) . . . . ? C15 C14 Fe1 C17 -81.45(14) . . . . ? C18 C14 Fe1 C12 162.8(2) . . . . ? C15 C14 Fe1 C12 43.6(3) . . . . ? C18 C14 Fe1 C16 81.54(15) . . . . ? C15 C14 Fe1 C16 -37.60(13) . . . . ? C18 C14 Fe1 C15 119.14(19) . . . . ? C17 C18 Fe1 C10 -165.29(14) . . . . ? C14 C18 Fe1 C10 75.77(16) . . . . ? C17 C18 Fe1 C14 118.9(2) . . . . ? C17 C18 Fe1 C9 -123.09(14) . . . . ? C14 C18 Fe1 C9 117.97(14) . . . . ? C17 C18 Fe1 C13 -80.13(16) . . . . ? C14 C18 Fe1 C13 160.92(13) . . . . ? C17 C18 Fe1 C11 161.3(3) . . . . ? C14 C18 Fe1 C11 42.4(3) . . . . ? C14 C18 Fe1 C17 -118.9(2) . . . . ? C17 C18 Fe1 C12 -46.2(3) . . . . ? C14 C18 Fe1 C12 -165.2(2) . . . . ? C17 C18 Fe1 C16 37.53(14) . . . . ? C14 C18 Fe1 C16 -81.42(15) . . . . ? C17 C18 Fe1 C15 81.27(15) . . . . ? C14 C18 Fe1 C15 -37.68(14) . . . . ? C1 C9 Fe1 C10 120.2(2) . . . . ? C13 C9 Fe1 C10 -119.06(17) . . . . ? C1 C9 Fe1 C14 40.1(2) . . . . ? C10 C9 Fe1 C14 -80.02(15) . . . . ? C13 C9 Fe1 C14 160.92(13) . . . . ? C1 C9 Fe1 C18 -2.2(2) . . . . ? C10 C9 Fe1 C18 -122.40(13) . . . . ? C13 C9 Fe1 C18 118.54(13) . . . . ? C1 C9 Fe1 C13 -120.8(2) . . . . ? C10 C9 Fe1 C13 119.06(17) . . . . ? C1 C9 Fe1 C11 157.7(2) . . . . ? C10 C9 Fe1 C11 37.59(13) . . . . ? C13 C9 Fe1 C11 -81.47(13) . . . . ? C1 C9 Fe1 C17 -43.6(2) . . . . ? C10 C9 Fe1 C17 -163.74(13) . . . . ? C13 C9 Fe1 C17 77.20(15) . . . . ? C1 C9 Fe1 C12 -158.5(2) . . . . ? C10 C9 Fe1 C12 81.35(13) . . . . ? C13 C9 Fe1 C12 -37.70(12) . . . . ? C1 C9 Fe1 C16 -76.7(3) . . . . ? C10 C9 Fe1 C16 163.1(3) . . . . ? C13 C9 Fe1 C16 44.0(3) . . . . ? C1 C9 Fe1 C15 73.9(3) . . . . ? C10 C9 Fe1 C15 -46.3(3) . . . . ? C13 C9 Fe1 C15 -165.3(2) . . . . ? C12 C13 Fe1 C10 -80.97(14) . . . . ? C9 C13 Fe1 C10 37.91(12) . . . . ? C12 C13 Fe1 C14 -165.6(2) . . . . ? C9 C13 Fe1 C14 -46.7(3) . . . . ? C12 C13 Fe1 C18 160.70(13) . . . . ? C9 C13 Fe1 C18 -80.42(15) . . . . ? C12 C13 Fe1 C9 -118.88(18) . . . . ? C12 C13 Fe1 C11 -37.39(13) . . . . ? C9 C13 Fe1 C11 81.49(13) . . . . ? C12 C13 Fe1 C17 118.55(13) . . . . ? C9 C13 Fe1 C17 -122.58(13) . . . . ? C9 C13 Fe1 C12 118.88(18) . . . . ? C12 C13 Fe1 C16 76.72(15) . . . . ? C9 C13 Fe1 C16 -164.40(12) . . . . ? C12 C13 Fe1 C15 43.7(3) . . . . ? C9 C13 Fe1 C15 162.5(2) . . . . ? C12 C11 Fe1 C10 119.79(19) . . . . ? C10 C11 Fe1 C14 76.27(16) . . . . ? C12 C11 Fe1 C14 -163.94(14) . . . . ? C10 C11 Fe1 C18 44.3(3) . . . . ? C12 C11 Fe1 C18 164.1(3) . . . . ? C10 C11 Fe1 C9 -38.06(13) . . . . ? C12 C11 Fe1 C9 81.73(14) . . . . ? C10 C11 Fe1 C13 -82.44(14) . . . . ? C12 C11 Fe1 C13 37.35(13) . . . . ? C10 C11 Fe1 C17 -167.9(2) . . . . ? C12 C11 Fe1 C17 -48.1(3) . . . . ? C10 C11 Fe1 C12 -119.79(19) . . . . ? C10 C11 Fe1 C16 159.70(13) . . . . ? C12 C11 Fe1 C16 -80.51(15) . . . . ? C10 C11 Fe1 C15 117.69(14) . . . . ? C12 C11 Fe1 C15 -122.52(14) . . . . ? C18 C17 Fe1 C10 41.0(3) . . . . ? C16 C17 Fe1 C10 160.5(3) . . . . ? C18 C17 Fe1 C14 -37.88(14) . . . . ? C16 C17 Fe1 C14 81.65(15) . . . . ? C16 C17 Fe1 C18 119.5(2) . . . . ? C18 C17 Fe1 C9 76.09(16) . . . . ? C16 C17 Fe1 C9 -164.39(13) . . . . ? C18 C17 Fe1 C13 118.51(14) . . . . ? C16 C17 Fe1 C13 -121.96(14) . . . . ? C18 C17 Fe1 C11 -164.3(2) . . . . ? C16 C17 Fe1 C11 -44.8(3) . . . . ? C18 C17 Fe1 C12 160.86(14) . . . . ? C16 C17 Fe1 C12 -79.61(16) . . . . ? C18 C17 Fe1 C16 -119.5(2) . . . . ? C18 C17 Fe1 C15 -81.74(15) . . . . ? C16 C17 Fe1 C15 37.79(14) . . . . ? C13 C12 Fe1 C10 82.46(14) . . . . ? C11 C12 Fe1 C10 -37.29(13) . . . . ? C13 C12 Fe1 C14 163.3(2) . . . . ? C11 C12 Fe1 C14 43.6(3) . . . . ? C13 C12 Fe1 C18 -46.7(3) . . . . ? C11 C12 Fe1 C18 -166.5(2) . . . . ? C13 C12 Fe1 C9 38.24(12) . . . . ? C11 C12 Fe1 C9 -81.51(14) . . . . ? C11 C12 Fe1 C13 -119.75(18) . . . . ? C13 C12 Fe1 C11 119.75(18) . . . . ? C13 C12 Fe1 C17 -80.21(15) . . . . ? C11 C12 Fe1 C17 160.04(13) . . . . ? C13 C12 Fe1 C16 -122.36(13) . . . . ? C11 C12 Fe1 C16 117.89(14) . . . . ? C13 C12 Fe1 C15 -163.91(13) . . . . ? C11 C12 Fe1 C15 76.34(16) . . . . ? C15 C16 Fe1 C10 -45.7(3) . . . . ? C17 C16 Fe1 C10 -164.6(2) . . . . ? C15 C16 Fe1 C14 37.65(14) . . . . ? C17 C16 Fe1 C14 -81.25(15) . . . . ? C15 C16 Fe1 C18 81.52(15) . . . . ? C17 C16 Fe1 C18 -37.38(14) . . . . ? C15 C16 Fe1 C9 162.7(2) . . . . ? C17 C16 Fe1 C9 43.7(3) . . . . ? C15 C16 Fe1 C13 -163.77(13) . . . . ? C17 C16 Fe1 C13 77.33(16) . . . . ? C15 C16 Fe1 C11 -79.82(16) . . . . ? C17 C16 Fe1 C11 161.28(13) . . . . ? C15 C16 Fe1 C17 118.9(2) . . . . ? C15 C16 Fe1 C12 -122.16(14) . . . . ? C17 C16 Fe1 C12 118.94(14) . . . . ? C17 C16 Fe1 C15 -118.9(2) . . . . ? C16 C15 Fe1 C10 160.42(13) . . . . ? C14 C15 Fe1 C10 -80.34(15) . . . . ? C16 C15 Fe1 C14 -119.24(19) . . . . ? C16 C15 Fe1 C18 -81.51(15) . . . . ? C14 C15 Fe1 C18 37.73(14) . . . . ? C16 C15 Fe1 C9 -166.00(19) . . . . ? C14 C15 Fe1 C9 -46.8(3) . . . . ? C16 C15 Fe1 C13 44.0(3) . . . . ? C14 C15 Fe1 C13 163.3(2) . . . . ? C16 C15 Fe1 C11 118.32(14) . . . . ? C14 C15 Fe1 C11 -122.44(14) . . . . ? C16 C15 Fe1 C17 -37.85(13) . . . . ? C14 C15 Fe1 C17 81.39(15) . . . . ? C16 C15 Fe1 C12 76.84(16) . . . . ? C14 C15 Fe1 C12 -163.91(13) . . . . ? C14 C15 Fe1 C16 119.24(19) . . . . ? C30 C31 Fe2 C28 -81.02(15) . . . . ? C27 C31 Fe2 C28 38.11(13) . . . . ? C30 C31 Fe2 C27 -119.13(19) . . . . ? C30 C31 Fe2 C36 161.01(14) . . . . ? C27 C31 Fe2 C36 -79.86(15) . . . . ? C30 C31 Fe2 C35 119.24(14) . . . . ? C27 C31 Fe2 C35 -121.64(13) . . . . ? C30 C31 Fe2 C32 -166.6(2) . . . . ? C27 C31 Fe2 C32 -47.5(3) . . . . ? C30 C31 Fe2 C33 46.6(3) . . . . ? C27 C31 Fe2 C33 165.8(2) . . . . ? C30 C31 Fe2 C29 -37.41(14) . . . . ? C27 C31 Fe2 C29 81.72(14) . . . . ? C27 C31 Fe2 C30 119.13(19) . . . . ? C30 C31 Fe2 C34 77.84(16) . . . . ? C27 C31 Fe2 C34 -163.03(13) . . . . ? C29 C28 Fe2 C31 80.98(14) . . . . ? C27 C28 Fe2 C31 -38.08(12) . . . . ? C29 C28 Fe2 C27 119.06(18) . . . . ? C29 C28 Fe2 C36 -164.65(13) . . . . ? C27 C28 Fe2 C36 76.29(15) . . . . ? C29 C28 Fe2 C35 163.4(2) . . . . ? C27 C28 Fe2 C35 44.3(3) . . . . ? C29 C28 Fe2 C32 -122.92(14) . . . . ? C27 C28 Fe2 C32 118.02(13) . . . . ? C29 C28 Fe2 C33 -81.07(16) . . . . ? C27 C28 Fe2 C33 159.87(13) . . . . ? C27 C28 Fe2 C29 -119.06(18) . . . . ? C29 C28 Fe2 C30 37.34(13) . . . . ? C27 C28 Fe2 C30 -81.73(14) . . . . ? C29 C28 Fe2 C34 -47.8(3) . . . . ? C27 C28 Fe2 C34 -166.9(2) . . . . ? C19 C27 Fe2 C31 -120.5(2) . . . . ? C28 C27 Fe2 C31 118.84(18) . . . . ? C19 C27 Fe2 C28 120.7(2) . . . . ? C31 C27 Fe2 C28 -118.84(18) . . . . ? C19 C27 Fe2 C36 -2.1(2) . . . . ? C31 C27 Fe2 C36 118.45(13) . . . . ? C28 C27 Fe2 C36 -122.72(13) . . . . ? C19 C27 Fe2 C35 -43.1(2) . . . . ? C31 C27 Fe2 C35 77.41(15) . . . . ? C28 C27 Fe2 C35 -163.76(13) . . . . ? C19 C27 Fe2 C32 39.9(2) . . . . ? C31 C27 Fe2 C32 160.44(13) . . . . ? C28 C27 Fe2 C32 -80.72(15) . . . . ? C19 C27 Fe2 C33 71.6(3) . . . . ? C31 C27 Fe2 C33 -167.9(2) . . . . ? C28 C27 Fe2 C33 -49.0(3) . . . . ? C19 C27 Fe2 C29 158.2(2) . . . . ? C31 C27 Fe2 C29 -81.27(14) . . . . ? C28 C27 Fe2 C29 37.57(13) . . . . ? C19 C27 Fe2 C30 -158.1(2) . . . . ? C31 C27 Fe2 C30 -37.57(13) . . . . ? C28 C27 Fe2 C30 81.27(14) . . . . ? C19 C27 Fe2 C34 -74.4(3) . . . . ? C31 C27 Fe2 C34 46.1(3) . . . . ? C28 C27 Fe2 C34 164.9(2) . . . . ? C35 C36 Fe2 C31 -79.68(16) . . . . ? C32 C36 Fe2 C31 161.42(14) . . . . ? C35 C36 Fe2 C28 -164.16(13) . . . . ? C32 C36 Fe2 C28 76.94(16) . . . . ? C35 C36 Fe2 C27 -122.24(14) . . . . ? C32 C36 Fe2 C27 118.85(14) . . . . ? C32 C36 Fe2 C35 -118.9(2) . . . . ? C35 C36 Fe2 C32 118.9(2) . . . . ? C35 C36 Fe2 C33 81.38(14) . . . . ? C32 C36 Fe2 C33 -37.53(14) . . . . ? C35 C36 Fe2 C29 164.2(3) . . . . ? C32 C36 Fe2 C29 45.3(3) . . . . ? C35 C36 Fe2 C30 -47.0(3) . . . . ? C32 C36 Fe2 C30 -165.9(2) . . . . ? C35 C36 Fe2 C34 37.54(13) . . . . ? C32 C36 Fe2 C34 -81.37(15) . . . . ? C36 C35 Fe2 C31 118.35(14) . . . . ? C34 C35 Fe2 C31 -122.19(14) . . . . ? C36 C35 Fe2 C28 42.7(3) . . . . ? C34 C35 Fe2 C28 162.1(2) . . . . ? C36 C35 Fe2 C27 76.16(16) . . . . ? C34 C35 Fe2 C27 -164.38(13) . . . . ? C34 C35 Fe2 C36 119.46(19) . . . . ? C36 C35 Fe2 C32 -37.95(14) . . . . ? C34 C35 Fe2 C32 81.51(15) . . . . ? C36 C35 Fe2 C33 -81.54(14) . . . . ? C34 C35 Fe2 C33 37.91(14) . . . . ? C36 C35 Fe2 C29 -166.4(2) . . . . ? C34 C35 Fe2 C29 -47.0(3) . . . . ? C36 C35 Fe2 C30 160.30(13) . . . . ? C34 C35 Fe2 C30 -80.25(16) . . . . ? C36 C35 Fe2 C34 -119.46(19) . . . . ? C33 C32 Fe2 C31 -163.7(2) . . . . ? C36 C32 Fe2 C31 -44.6(3) . . . . ? C33 C32 Fe2 C28 118.75(14) . . . . ? C36 C32 Fe2 C28 -122.17(14) . . . . ? C33 C32 Fe2 C27 161.66(13) . . . . ? C36 C32 Fe2 C27 -79.26(15) . . . . ? C33 C32 Fe2 C36 -119.08(19) . . . . ? C33 C32 Fe2 C35 -81.45(14) . . . . ? C36 C32 Fe2 C35 37.63(14) . . . . ? C36 C32 Fe2 C33 119.08(19) . . . . ? C33 C32 Fe2 C29 77.31(16) . . . . ? C36 C32 Fe2 C29 -163.61(14) . . . . ? C33 C32 Fe2 C30 43.9(3) . . . . ? C36 C32 Fe2 C30 162.9(3) . . . . ? C33 C32 Fe2 C34 -37.64(13) . . . . ? C36 C32 Fe2 C34 81.44(15) . . . . ? C32 C33 Fe2 C31 160.8(2) . . . . ? C34 C33 Fe2 C31 41.5(3) . . . . ? C32 C33 Fe2 C28 -79.61(16) . . . . ? C34 C33 Fe2 C28 161.06(13) . . . . ? C32 C33 Fe2 C27 -43.8(3) . . . . ? C34 C33 Fe2 C27 -163.2(2) . . . . ? C32 C33 Fe2 C36 37.85(13) . . . . ? C34 C33 Fe2 C36 -81.48(15) . . . . ? C32 C33 Fe2 C35 81.45(14) . . . . ? C34 C33 Fe2 C35 -37.88(14) . . . . ? C34 C33 Fe2 C32 -119.3(2) . . . . ? C32 C33 Fe2 C29 -122.14(14) . . . . ? C34 C33 Fe2 C29 118.53(14) . . . . ? C32 C33 Fe2 C30 -164.08(13) . . . . ? C34 C33 Fe2 C30 76.59(16) . . . . ? C32 C33 Fe2 C34 119.3(2) . . . . ? C28 C29 Fe2 C31 -82.42(14) . . . . ? C30 C29 Fe2 C31 37.40(14) . . . . ? C30 C29 Fe2 C28 119.82(19) . . . . ? C28 C29 Fe2 C27 -38.12(13) . . . . ? C30 C29 Fe2 C27 81.70(14) . . . . ? C28 C29 Fe2 C36 42.1(3) . . . . ? C30 C29 Fe2 C36 161.9(3) . . . . ? C28 C29 Fe2 C35 -165.5(2) . . . . ? C30 C29 Fe2 C35 -45.7(3) . . . . ? C28 C29 Fe2 C32 76.20(16) . . . . ? C30 C29 Fe2 C32 -163.98(14) . . . . ? C28 C29 Fe2 C33 117.85(14) . . . . ? C30 C29 Fe2 C33 -122.33(14) . . . . ? C28 C29 Fe2 C30 -119.82(19) . . . . ? C28 C29 Fe2 C34 160.32(13) . . . . ? C30 C29 Fe2 C34 -79.87(16) . . . . ? C29 C30 Fe2 C31 -119.7(2) . . . . ? C31 C30 Fe2 C28 82.38(14) . . . . ? C29 C30 Fe2 C28 -37.29(14) . . . . ? C31 C30 Fe2 C27 38.05(13) . . . . ? C29 C30 Fe2 C27 -81.62(14) . . . . ? C31 C30 Fe2 C36 -45.2(3) . . . . ? C29 C30 Fe2 C36 -164.9(2) . . . . ? C31 C30 Fe2 C35 -79.09(16) . . . . ? C29 C30 Fe2 C35 161.24(14) . . . . ? C31 C30 Fe2 C32 164.0(3) . . . . ? C29 C30 Fe2 C32 44.3(3) . . . . ? C31 C30 Fe2 C33 -163.00(13) . . . . ? C29 C30 Fe2 C33 77.33(16) . . . . ? C31 C30 Fe2 C29 119.7(2) . . . . ? C31 C30 Fe2 C34 -121.36(14) . . . . ? C29 C30 Fe2 C34 118.97(14) . . . . ? C35 C34 Fe2 C31 76.55(16) . . . . ? C33 C34 Fe2 C31 -164.71(13) . . . . ? C35 C34 Fe2 C28 -164.6(2) . . . . ? C33 C34 Fe2 C28 -45.8(3) . . . . ? C35 C34 Fe2 C27 41.8(3) . . . . ? C33 C34 Fe2 C27 160.5(2) . . . . ? C35 C34 Fe2 C36 -37.36(13) . . . . ? C33 C34 Fe2 C36 81.38(15) . . . . ? C33 C34 Fe2 C35 118.7(2) . . . . ? C35 C34 Fe2 C32 -81.32(15) . . . . ? C33 C34 Fe2 C32 37.42(14) . . . . ? C35 C34 Fe2 C33 -118.7(2) . . . . ? C35 C34 Fe2 C29 160.74(13) . . . . ? C33 C34 Fe2 C29 -80.52(16) . . . . ? C35 C34 Fe2 C30 118.46(14) . . . . ? C33 C34 Fe2 C30 -122.80(14) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.433 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.068 _database_code_depnum_ccdc_archive 'CCDC 943231'