# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_fcc20a _database_code_depnum_ccdc_archive 'CCDC 869094' #TrackingRef '- compound3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H18 Fe' _chemical_formula_weight 434.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 22.011(5) _cell_length_b 43.742(9) _cell_length_c 8.1622(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7858(3) _cell_formula_units_Z 16 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 976 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 27.9 _exptl_crystal_description platelett _exptl_crystal_colour orange _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3584 _exptl_absorpt_coefficient_mu 0.783 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.744 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS SMART CCD' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25166 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -62 _diffrn_reflns_limit_k_max 62 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 30.57 _reflns_number_total 5905 _reflns_number_gt 5031 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker-AXS)' _computing_cell_refinement 'SAINT (Bruker-AXS)' _computing_data_reduction 'SAINT (Bruker-AXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+4.3761P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.045(13) _refine_ls_number_reflns 5905 _refine_ls_number_parameters 280 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.0978 _refine_ls_wR_factor_gt 0.0925 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 0.913442(14) 0.209936(7) 0.68690(4) 0.01510(8) Uani 1 1 d . . . C1 C 0.82662(11) 0.19678(5) 0.7418(3) 0.0216(5) Uani 1 1 d . . . H1 H 0.7962 0.1909 0.6656 0.026 Uiso 1 1 calc R . . C2 C 0.86924(12) 0.17697(6) 0.8175(3) 0.0242(5) Uani 1 1 d . . . H2 H 0.8722 0.1555 0.8009 0.029 Uiso 1 1 calc R . . C3 C 0.90668(11) 0.19474(6) 0.9222(3) 0.0236(5) Uani 1 1 d . . . H3 H 0.9392 0.1873 0.9876 0.028 Uiso 1 1 calc R . . C4 C 0.88685(11) 0.22568(6) 0.9117(3) 0.0219(5) Uani 1 1 d . . . H4 H 0.9037 0.2425 0.9694 0.026 Uiso 1 1 calc R . . C5 C 0.83712(11) 0.22686(5) 0.7990(3) 0.0199(5) Uani 1 1 d . . . H5 H 0.8151 0.2446 0.7682 0.024 Uiso 1 1 calc R . . C6 C 0.92116(11) 0.20844(5) 0.4394(3) 0.0193(5) Uani 1 1 d . . . H6 H 0.8899 0.2032 0.3644 0.023 Uiso 1 1 calc R . . C7 C 0.96279(12) 0.18762(5) 0.5127(3) 0.0215(5) Uani 1 1 d . . . H7 H 0.9640 0.1662 0.4951 0.026 Uiso 1 1 calc R . . C8 C 1.00209(12) 0.20441(6) 0.6159(3) 0.0212(5) Uani 1 1 d . . . H8 H 1.0343 0.1962 0.6796 0.025 Uiso 1 1 calc R . . C9 C 0.98481(11) 0.23596(5) 0.6079(3) 0.0177(5) Uani 1 1 d . . . H9 H 1.0036 0.2523 0.6656 0.021 Uiso 1 1 calc R . . C10 C 0.93417(11) 0.23868(5) 0.4974(3) 0.0174(4) Uani 1 1 d . . . C11 C 0.90079(10) 0.26671(5) 0.4508(3) 0.0173(4) Uani 1 1 d . . . C12 C 0.89846(11) 0.29374(5) 0.5572(3) 0.0163(4) Uani 1 1 d . . . C13 C 0.91135(11) 0.29702(5) 0.7299(3) 0.0175(5) Uani 1 1 d . . . H13 H 0.9376 0.2827 0.7812 0.021 Uiso 1 1 calc R . . C14 C 0.88639(11) 0.32062(5) 0.8240(3) 0.0204(5) Uani 1 1 d . . . H14 H 0.8959 0.3216 0.9374 0.025 Uiso 1 1 calc R . . C15 C 0.84713(11) 0.34332(5) 0.7555(3) 0.0192(5) Uani 1 1 d . . . C16 C 0.80199(12) 0.36257(5) 0.8335(3) 0.0224(5) Uani 1 1 d . . . H16 H 0.8049 0.3662 0.9480 0.027 Uiso 1 1 calc R . . C17 C 0.75463(12) 0.37585(5) 0.7467(3) 0.0238(5) Uani 1 1 d . . . H17 H 0.7262 0.3884 0.8028 0.029 Uiso 1 1 calc R . . C18 C 0.74772(11) 0.37096(5) 0.5714(3) 0.0220(5) Uani 1 1 d . . . C19 C 0.69356(12) 0.37329(5) 0.4709(3) 0.0264(6) Uani 1 1 d . . . H19 H 0.6607 0.3856 0.5073 0.032 Uiso 1 1 calc R . . C20 C 0.68871(12) 0.35792(6) 0.3226(4) 0.0282(6) Uani 1 1 d . . . H20 H 0.6525 0.3601 0.2604 0.034 Uiso 1 1 calc R . . C21 C 0.73670(12) 0.33884(6) 0.2599(3) 0.0238(5) Uani 1 1 d . . . C22 C 0.73445(12) 0.31399(6) 0.1441(3) 0.0273(6) Uani 1 1 d . . . H22 H 0.7018 0.3131 0.0681 0.033 Uiso 1 1 calc R . . C23 C 0.77847(14) 0.29122(6) 0.1399(3) 0.0258(6) Uani 1 1 d . . . H23 H 0.7751 0.2753 0.0610 0.031 Uiso 1 1 calc R . . C24 C 0.82914(11) 0.29097(5) 0.2518(3) 0.0195(5) Uani 1 1 d . . . C25 C 0.86652(11) 0.26612(5) 0.3057(3) 0.0194(5) Uani 1 1 d . . . H25 H 0.8682 0.2483 0.2396 0.023 Uiso 1 1 calc R . . C26 C 0.86886(11) 0.31855(5) 0.4901(3) 0.0176(5) Uani 1 1 d . . . C27 C 0.84405(11) 0.34275(5) 0.5867(3) 0.0182(5) Uani 1 1 d . . . C28 C 0.79572(11) 0.35614(5) 0.4972(3) 0.0196(5) Uani 1 1 d . . . C29 C 0.79065(11) 0.34089(5) 0.3462(3) 0.0197(5) Uani 1 1 d . . . C30 C 0.83555(11) 0.31762(5) 0.3422(3) 0.0190(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 Fe1 0.01609(14) 0.01426(13) 0.01494(14) -0.00032(13) 0.00366(13) 0.00101(13) C1 0.0193(11) 0.0193(11) 0.0260(13) -0.0038(10) 0.0072(10) -0.0031(9) C2 0.0251(12) 0.0167(10) 0.0309(14) 0.0025(10) 0.0126(11) 0.0027(9) C3 0.0248(12) 0.0282(12) 0.0179(12) 0.0074(11) 0.0050(11) 0.0050(10) C4 0.0263(12) 0.0241(11) 0.0154(13) -0.0017(9) 0.0067(10) -0.0029(10) C5 0.0213(12) 0.0167(10) 0.0216(12) -0.0001(9) 0.0051(10) 0.0030(9) C6 0.0231(11) 0.0198(11) 0.0150(11) -0.0024(10) 0.0019(10) -0.0002(8) C7 0.0256(12) 0.0164(10) 0.0227(12) -0.0029(9) 0.0076(10) 0.0023(9) C8 0.0194(12) 0.0234(12) 0.0209(12) 0.0009(9) 0.0067(10) 0.0051(9) C9 0.0163(11) 0.0192(11) 0.0177(11) -0.0005(9) 0.0039(9) 0.0006(9) C10 0.0179(10) 0.0191(10) 0.0152(10) 0.0001(9) 0.0042(9) 0.0016(9) C11 0.0170(10) 0.0183(10) 0.0166(11) 0.0010(9) 0.0031(9) 0.0003(8) C12 0.0165(10) 0.0144(10) 0.0180(12) 0.0003(8) -0.0006(9) -0.0038(8) C13 0.0184(11) 0.0168(10) 0.0172(13) 0.0016(8) -0.0037(9) 0.0022(9) C14 0.0245(12) 0.0203(11) 0.0164(12) -0.0013(9) -0.0049(10) -0.0032(9) C15 0.0182(11) 0.0139(10) 0.0255(13) -0.0024(9) -0.0025(10) -0.0043(8) C16 0.0261(13) 0.0168(11) 0.0242(13) -0.0063(9) -0.0014(10) -0.0041(9) C17 0.0251(13) 0.0147(10) 0.0315(14) -0.0050(10) 0.0040(11) 0.0018(9) C18 0.0210(12) 0.0141(10) 0.0307(14) 0.0043(9) -0.0012(11) -0.0029(9) C19 0.0211(12) 0.0191(11) 0.0391(18) 0.0065(10) -0.0029(11) 0.0020(9) C20 0.0222(12) 0.0262(12) 0.0362(16) 0.0108(11) -0.0112(12) 0.0006(10) C21 0.0265(13) 0.0211(11) 0.0239(13) 0.0074(10) -0.0066(10) -0.0035(10) C22 0.0241(13) 0.0326(14) 0.0253(14) 0.0060(11) -0.0119(10) -0.0056(10) C23 0.0328(14) 0.0289(13) 0.0158(12) -0.0003(10) -0.0058(10) -0.0063(11) C24 0.0212(12) 0.0244(12) 0.0127(10) 0.0017(9) 0.0012(9) -0.0009(9) C25 0.0227(12) 0.0211(11) 0.0145(11) -0.0028(9) 0.0036(9) -0.0035(9) C26 0.0173(11) 0.0174(10) 0.0180(11) 0.0023(9) 0.0010(9) -0.0041(8) C27 0.0161(11) 0.0137(10) 0.0247(13) 0.0017(9) -0.0020(9) -0.0057(9) C28 0.0185(11) 0.0136(10) 0.0268(12) 0.0048(9) -0.0013(9) -0.0031(9) C29 0.0199(12) 0.0203(11) 0.0190(12) 0.0080(9) -0.0024(10) -0.0039(9) C30 0.0202(11) 0.0192(11) 0.0174(12) 0.0043(9) 0.0007(9) -0.0056(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C6 2.028(3) . ? Fe1 C3 2.038(3) . ? Fe1 C7 2.038(2) . ? Fe1 C2 2.040(2) . ? Fe1 C10 2.044(2) . ? Fe1 C9 2.045(2) . ? Fe1 C1 2.045(2) . ? Fe1 C4 2.045(2) . ? Fe1 C8 2.050(2) . ? Fe1 C5 2.051(2) . ? C1 C5 1.415(3) . ? C1 C2 1.419(4) . ? C2 C3 1.419(4) . ? C3 C4 1.425(4) . ? C4 C5 1.431(4) . ? C6 C7 1.424(3) . ? C6 C10 1.434(3) . ? C7 C8 1.414(4) . ? C8 C9 1.433(3) . ? C9 C10 1.438(3) . ? C10 C11 1.479(3) . ? C11 C25 1.405(3) . ? C11 C12 1.468(3) . ? C12 C26 1.379(3) . ? C12 C13 1.445(4) . ? C13 C14 1.399(3) . ? C14 C15 1.430(3) . ? C15 C27 1.379(4) . ? C15 C16 1.450(3) . ? C16 C17 1.388(4) . ? C17 C18 1.454(4) . ? C18 C28 1.380(4) . ? C18 C19 1.451(4) . ? C19 C20 1.389(4) . ? C20 C21 1.440(4) . ? C21 C29 1.384(3) . ? C21 C22 1.441(4) . ? C22 C23 1.390(4) . ? C23 C24 1.442(4) . ? C24 C30 1.387(3) . ? C24 C25 1.433(3) . ? C26 C30 1.413(3) . ? C26 C27 1.428(3) . ? C27 C28 1.417(3) . ? C28 C29 1.406(4) . ? C29 C30 1.419(3) . ? 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 C6 Fe1 C3 159.11(10) . . ? C6 Fe1 C7 40.98(10) . . ? C3 Fe1 C7 122.70(10) . . ? C6 Fe1 C2 122.52(10) . . ? C3 Fe1 C2 40.72(11) . . ? C7 Fe1 C2 106.28(11) . . ? C6 Fe1 C10 41.22(9) . . ? C3 Fe1 C10 158.40(10) . . ? C7 Fe1 C10 69.38(10) . . ? C2 Fe1 C10 159.43(11) . . ? C6 Fe1 C9 68.86(10) . . ? C3 Fe1 C9 122.35(11) . . ? C7 Fe1 C9 68.72(10) . . ? C2 Fe1 C9 157.65(10) . . ? C10 Fe1 C9 41.19(10) . . ? C6 Fe1 C1 106.69(10) . . ? C3 Fe1 C1 68.51(11) . . ? C7 Fe1 C1 121.06(10) . . ? C2 Fe1 C1 40.65(10) . . ? C10 Fe1 C1 123.17(10) . . ? C9 Fe1 C1 160.66(9) . . ? C6 Fe1 C4 158.17(10) . . ? C3 Fe1 C4 40.84(10) . . ? C7 Fe1 C4 159.98(10) . . ? C2 Fe1 C4 68.45(10) . . ? C10 Fe1 C4 122.37(10) . . ? C9 Fe1 C4 108.39(10) . . ? C1 Fe1 C4 68.34(10) . . ? C6 Fe1 C8 68.60(10) . . ? C3 Fe1 C8 107.30(10) . . ? C7 Fe1 C8 40.46(11) . . ? C2 Fe1 C8 121.22(10) . . ? C10 Fe1 C8 69.28(10) . . ? C9 Fe1 C8 40.97(9) . . ? C1 Fe1 C8 156.66(10) . . ? C4 Fe1 C8 124.44(11) . . ? C6 Fe1 C5 121.63(10) . . ? C3 Fe1 C5 68.75(10) . . ? C7 Fe1 C5 156.99(11) . . ? C2 Fe1 C5 68.37(10) . . ? C10 Fe1 C5 107.36(10) . . ? C9 Fe1 C5 124.69(10) . . ? C1 Fe1 C5 40.41(9) . . ? C4 Fe1 C5 40.89(10) . . ? C8 Fe1 C5 161.49(10) . . ? C5 C1 C2 108.4(2) . . ? C5 C1 Fe1 70.02(14) . . ? C2 C1 Fe1 69.47(14) . . ? C3 C2 C1 108.2(2) . . ? C3 C2 Fe1 69.55(14) . . ? C1 C2 Fe1 69.89(14) . . ? C2 C3 C4 107.8(2) . . ? C2 C3 Fe1 69.73(15) . . ? C4 C3 Fe1 69.88(14) . . ? C3 C4 C5 107.9(2) . . ? C3 C4 Fe1 69.28(15) . . ? C5 C4 Fe1 69.77(14) . . ? C1 C5 C4 107.7(2) . . ? C1 C5 Fe1 69.57(14) . . ? C4 C5 Fe1 69.34(13) . . ? C7 C6 C10 108.8(2) . . ? C7 C6 Fe1 69.89(15) . . ? C10 C6 Fe1 70.00(14) . . ? C8 C7 C6 108.2(2) . . ? C8 C7 Fe1 70.19(14) . . ? C6 C7 Fe1 69.12(14) . . ? C7 C8 C9 108.1(2) . . ? C7 C8 Fe1 69.35(14) . . ? C9 C8 Fe1 69.33(13) . . ? C8 C9 C10 108.3(2) . . ? C8 C9 Fe1 69.70(14) . . ? C10 C9 Fe1 69.40(13) . . ? C6 C10 C9 106.6(2) . . ? C6 C10 C11 125.5(2) . . ? C9 C10 C11 127.9(2) . . ? C6 C10 Fe1 68.78(14) . . ? C9 C10 Fe1 69.41(14) . . ? C11 C10 Fe1 126.40(17) . . ? C25 C11 C12 119.7(2) . . ? C25 C11 C10 117.9(2) . . ? C12 C11 C10 122.2(2) . . ? C26 C12 C13 113.7(2) . . ? C26 C12 C11 114.6(2) . . ? C13 C12 C11 130.5(2) . . ? C14 C13 C12 122.1(2) . . ? C13 C14 C15 122.3(2) . . ? C27 C15 C14 114.1(2) . . ? C27 C15 C16 114.6(2) . . ? C14 C15 C16 130.2(2) . . ? C17 C16 C15 122.2(2) . . ? C16 C17 C18 121.3(2) . . ? C28 C18 C19 114.5(3) . . ? C28 C18 C17 114.9(2) . . ? C19 C18 C17 129.2(3) . . ? C20 C19 C18 121.5(2) . . ? C19 C20 C21 122.3(2) . . ? C29 C21 C20 114.3(2) . . ? C29 C21 C22 114.3(2) . . ? C20 C21 C22 130.2(2) . . ? C23 C22 C21 122.2(2) . . ? C22 C23 C24 121.9(2) . . ? C30 C24 C25 114.6(2) . . ? C30 C24 C23 114.2(2) . . ? C25 C24 C23 130.1(2) . . ? C11 C25 C24 123.6(2) . . ? C12 C26 C30 124.2(2) . . ? C12 C26 C27 123.0(2) . . ? C30 C26 C27 107.1(2) . . ? C15 C27 C28 123.0(2) . . ? C15 C27 C26 123.1(2) . . ? C28 C27 C26 108.0(2) . . ? C18 C28 C29 123.2(2) . . ? C18 C28 C27 122.9(3) . . ? C29 C28 C27 108.4(2) . . ? C21 C29 C28 123.0(2) . . ? C21 C29 C30 122.7(2) . . ? C28 C29 C30 107.8(2) . . ? C24 C30 C26 122.1(2) . . ? C24 C30 C29 123.0(2) . . ? C26 C30 C29 108.7(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.57 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.950 _refine_diff_density_min -0.290 _refine_diff_density_rms 0.085 data_corfe2 _database_code_depnum_ccdc_archive 'CCDC 881577' #TrackingRef '4-new.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H26 Fe' _chemical_formula_weight 682.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0056 0.0026 '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 0.3418 1.2585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 37.1090(10) _cell_length_b 23.2570(10) _cell_length_c 7.4300(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6412.4(9) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 38000 _cell_measurement_theta_min 5 _cell_measurement_theta_max 32 _exptl_crystal_description platelett _exptl_crystal_colour red _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2816 _exptl_absorpt_coefficient_mu 0.868 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.88561 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'BL 14.1, PSF, BESSY, Berlin, Germany' _diffrn_radiation_monochromator Si(111) _diffrn_measurement_device_type MAR225_CCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49378 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 33.61 _reflns_number_total 12181 _reflns_number_gt 10918 _reflns_threshold_expression >2sigma(I) _computing_data_collection XDS _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0799P)^2^+1.4867P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.062(8) _refine_ls_number_reflns 12181 _refine_ls_number_parameters 919 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1187 _refine_ls_wR_factor_gt 0.1108 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.003 _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 0.876330(10) 0.610061(16) 0.15625(7) 0.02494(10) Uani 1 1 d . . . Fe2 Fe 0.741074(9) 0.573439(16) 0.66051(7) 0.02319(10) Uani 1 1 d . . . C1 C 0.82423(8) 0.62307(14) 0.2368(5) 0.0302(7) Uani 1 1 d . . . H1 H 0.8064 0.6440 0.1723 0.036 Uiso 1 1 calc R . . C2 C 0.83160(8) 0.56356(14) 0.2173(4) 0.0306(7) Uani 1 1 d . . . H2 H 0.8194 0.5379 0.1386 0.037 Uiso 1 1 calc R . . C3 C 0.86016(9) 0.54878(14) 0.3350(5) 0.0307(7) Uani 1 1 d . . . H3 H 0.8705 0.5117 0.3491 0.037 Uiso 1 1 calc R . . C4 C 0.87060(9) 0.59956(15) 0.4286(5) 0.0302(7) Uani 1 1 d . . . H4 H 0.8893 0.6021 0.5155 0.036 Uiso 1 1 calc R . . C5 C 0.84811(8) 0.64659(13) 0.3698(4) 0.0270(6) Uani 1 1 d . . . C6 C 0.84804(8) 0.70578(14) 0.4386(5) 0.0289(7) Uani 1 1 d . . . C7 C 0.87922(8) 0.72958(14) 0.5332(5) 0.0291(7) Uani 1 1 d . . . C8 C 0.91676(8) 0.71313(14) 0.5249(5) 0.0293(7) Uani 1 1 d . . . H8 H 0.9228 0.6760 0.4812 0.035 Uiso 1 1 calc R . . C9 C 0.94432(8) 0.74975(14) 0.5786(5) 0.0306(7) Uani 1 1 d . . . H9 H 0.9685 0.7364 0.5726 0.037 Uiso 1 1 calc R . . C10 C 0.93775(7) 0.80682(13) 0.6426(5) 0.0302(6) Uani 1 1 d . . . C11 C 0.96043(7) 0.85666(13) 0.6466(5) 0.0296(6) Uani 1 1 d . . . H11 H 0.9858 0.8513 0.6457 0.036 Uiso 1 1 calc R . . C12 C 0.94713(8) 0.91197(14) 0.6516(6) 0.0357(7) Uani 1 1 d . . . H12 H 0.9635 0.9433 0.6525 0.043 Uiso 1 1 calc R . . C13 C 0.90882(8) 0.92353(13) 0.6557(6) 0.0341(6) Uani 1 1 d . . . C14 C 0.88887(9) 0.97471(14) 0.6075(5) 0.0346(8) Uani 1 1 d . . . H14 H 0.9008 1.0108 0.6087 0.041 Uiso 1 1 calc R . . C15 C 0.85280(10) 0.97247(16) 0.5596(5) 0.0402(8) Uani 1 1 d . . . H15 H 0.8408 1.0072 0.5284 0.048 Uiso 1 1 calc R . . C16 C 0.83295(9) 0.91951(15) 0.5555(5) 0.0344(7) Uani 1 1 d . . . C17 C 0.80121(8) 0.90372(15) 0.4551(5) 0.0334(7) Uani 1 1 d . . . H17 H 0.7855 0.9332 0.4148 0.040 Uiso 1 1 calc R . . C18 C 0.79275(8) 0.84648(16) 0.4148(5) 0.0344(8) Uani 1 1 d . . . H18 H 0.7717 0.8385 0.3463 0.041 Uiso 1 1 calc R . . C19 C 0.81492(8) 0.79937(15) 0.4739(5) 0.0299(7) Uani 1 1 d . . . C20 C 0.81717(8) 0.74129(15) 0.4109(4) 0.0300(7) Uani 1 1 d . . . H20 H 0.7972 0.7257 0.3476 0.036 Uiso 1 1 calc R . . C21 C 0.87337(8) 0.78151(14) 0.6172(4) 0.0284(7) Uani 1 1 d . . . C22 C 0.90144(7) 0.81870(13) 0.6709(5) 0.0294(6) Uani 1 1 d . . . C23 C 0.88795(8) 0.87449(14) 0.6774(5) 0.0300(6) Uani 1 1 d . . . C24 C 0.85115(8) 0.87297(14) 0.6292(4) 0.0294(7) Uani 1 1 d . . . C25 C 0.84225(8) 0.81532(15) 0.5917(4) 0.0313(7) Uani 1 1 d . . . C26 C 0.88112(8) 0.64822(14) -0.0903(4) 0.0296(7) Uani 1 1 d . . . H26 H 0.8627 0.6697 -0.1481 0.035 Uiso 1 1 calc R . . C27 C 0.88649(9) 0.58748(16) -0.1038(5) 0.0342(7) Uani 1 1 d . . . H27 H 0.8724 0.5617 -0.1737 0.041 Uiso 1 1 calc R . . C28 C 0.91600(9) 0.57261(15) 0.0036(5) 0.0346(8) Uani 1 1 d . . . H28 H 0.9255 0.5350 0.0188 0.041 Uiso 1 1 calc R . . C29 C 0.92938(8) 0.62331(14) 0.0861(5) 0.0292(7) Uani 1 1 d . . . H29 H 0.9490 0.6252 0.1680 0.035 Uiso 1 1 calc R . . C30 C 0.90846(8) 0.67109(14) 0.0254(5) 0.0291(7) Uani 1 1 d . . . C31 C 0.91472(8) 0.73161(13) 0.0748(4) 0.0266(6) Uani 1 1 d . . . C32 C 0.88611(8) 0.77014(13) 0.1001(4) 0.0265(6) Uani 1 1 d . . . H32 H 0.8622 0.7563 0.0884 0.032 Uiso 1 1 calc R . . C33 C 0.89150(7) 0.82948(13) 0.1428(5) 0.0289(6) Uani 1 1 d . . . C34 C 0.86732(8) 0.87771(15) 0.1182(5) 0.0338(8) Uani 1 1 d . . . H34 H 0.8422 0.8705 0.1095 0.041 Uiso 1 1 calc R . . C35 C 0.87955(9) 0.93416(15) 0.1069(5) 0.0347(8) Uani 1 1 d . . . H35 H 0.8627 0.9645 0.0918 0.042 Uiso 1 1 calc R . . C36 C 0.91765(9) 0.94723(14) 0.1178(4) 0.0322(7) Uani 1 1 d . . . C37 C 0.93694(10) 0.99641(14) 0.0488(5) 0.0358(8) Uani 1 1 d . . . H37 H 0.9241 1.0311 0.0280 0.043 Uiso 1 1 calc R . . C38 C 0.97328(9) 0.99476(14) 0.0121(5) 0.0350(7) Uani 1 1 d . . . H38 H 0.9847 1.0284 -0.0322 0.042 Uiso 1 1 calc R . . C39 C 0.99457(9) 0.94346(14) 0.0387(5) 0.0322(7) Uani 1 1 d . . . C40 C 1.02778(8) 0.92590(15) -0.0450(5) 0.0340(7) Uani 1 1 d . . . H40 H 1.0433 0.9545 -0.0928 0.041 Uiso 1 1 calc R . . C41 C 1.03778(8) 0.86876(15) -0.0579(5) 0.0311(7) Uani 1 1 d . . . H41 H 1.0600 0.8594 -0.1146 0.037 Uiso 1 1 calc R . . C42 C 1.01552(7) 0.82286(14) 0.0121(4) 0.0277(6) Uani 1 1 d . . . C43 C 1.01397(7) 0.76340(14) -0.0397(5) 0.0282(6) Uani 1 1 d . . . H43 H 1.0340 0.7466 -0.0993 0.034 Uiso 1 1 calc R . . C44 C 0.98352(8) 0.72958(14) -0.0042(5) 0.0278(6) Uani 1 1 d . . . H44 H 0.9837 0.6902 -0.0384 0.033 Uiso 1 1 calc R . . C45 C 0.95187(8) 0.75258(13) 0.0826(4) 0.0270(6) Uani 1 1 d . . . C46 C 0.92661(8) 0.84496(13) 0.1819(4) 0.0274(6) Uani 1 1 d . . . C47 C 0.93936(8) 0.90210(12) 0.1689(5) 0.0291(6) Uani 1 1 d . . . C48 C 0.97669(8) 0.89972(13) 0.1304(4) 0.0280(7) Uani 1 1 d . . . C49 C 0.98685(8) 0.84181(14) 0.1178(4) 0.0274(7) Uani 1 1 d . . . C50 C 0.95601(7) 0.80741(11) 0.1502(5) 0.0247(5) Uani 1 1 d . . . C51 C 0.75045(8) 0.56308(14) 0.9306(5) 0.0269(6) Uani 1 1 d . . . H51 H 0.7331 0.5529 1.0188 0.032 Uiso 1 1 calc R . . C52 C 0.77187(7) 0.52418(13) 0.8277(4) 0.0270(6) Uani 1 1 d . . . H52 H 0.7712 0.4834 0.8356 0.032 Uiso 1 1 calc R . . C53 C 0.79419(7) 0.55659(14) 0.7124(4) 0.0281(7) Uani 1 1 d . . . H53 H 0.8114 0.5414 0.6306 0.034 Uiso 1 1 calc R . . C54 C 0.78669(7) 0.61543(14) 0.7389(5) 0.0281(7) Uani 1 1 d . . . H54 H 0.7976 0.6464 0.6759 0.034 Uiso 1 1 calc R . . C55 C 0.75989(7) 0.62061(14) 0.8769(5) 0.0257(6) Uani 1 1 d . . . C56 C 0.74670(8) 0.67558(14) 0.9509(5) 0.0270(6) Uani 1 1 d . . . C57 C 0.76769(8) 0.72508(14) 0.9290(5) 0.0301(7) Uani 1 1 d . . . H57 H 0.7905 0.7216 0.8716 0.036 Uiso 1 1 calc R . . C58 C 0.75640(8) 0.78108(14) 0.9894(5) 0.0286(7) Uani 1 1 d . . . C59 C 0.76732(9) 0.83681(15) 0.9271(5) 0.0341(7) Uani 1 1 d . . . H59 H 0.7898 0.8410 0.8674 0.041 Uiso 1 1 calc R . . C60 C 0.74564(9) 0.88468(14) 0.9525(5) 0.0349(8) Uani 1 1 d . . . H60 H 0.7535 0.9208 0.9073 0.042 Uiso 1 1 calc R . . C61 C 0.71178(9) 0.88160(13) 1.0445(5) 0.0317(7) Uani 1 1 d . . . C62 C 0.68087(10) 0.91959(14) 1.0313(5) 0.0361(8) Uani 1 1 d . . . H62 H 0.6843 0.9580 0.9915 0.043 Uiso 1 1 calc R . . C63 C 0.64624(10) 0.90100(15) 1.0758(5) 0.0352(7) Uani 1 1 d . . . H63 H 0.6268 0.9275 1.0683 0.042 Uiso 1 1 calc R . . C64 C 0.63909(8) 0.84321(14) 1.1325(5) 0.0323(7) Uani 1 1 d . . . C65 C 0.60620(8) 0.81081(15) 1.1235(5) 0.0346(8) Uani 1 1 d . . . H65 H 0.5839 0.8307 1.1176 0.042 Uiso 1 1 calc R . . C66 C 0.60616(8) 0.75075(14) 1.1234(4) 0.0306(7) Uani 1 1 d . . . H66 H 0.5838 0.7310 1.1170 0.037 Uiso 1 1 calc R . . C67 C 0.63912(8) 0.71782(13) 1.1328(5) 0.0287(7) Uani 1 1 d . . . C68 C 0.64612(8) 0.66057(14) 1.0704(5) 0.0292(7) Uani 1 1 d . . . H68 H 0.6265 0.6345 1.0587 0.035 Uiso 1 1 calc R . . C69 C 0.68067(8) 0.64195(13) 1.0263(4) 0.0270(6) Uani 1 1 d . . . H69 H 0.6840 0.6035 0.9863 0.032 Uiso 1 1 calc R . . C70 C 0.71154(8) 0.67940(13) 1.0397(4) 0.0266(6) Uani 1 1 d . . . C71 C 0.72638(8) 0.78036(14) 1.0986(4) 0.0289(7) Uani 1 1 d . . . C72 C 0.70484(8) 0.82956(13) 1.1268(4) 0.0295(7) Uani 1 1 d . . . C73 C 0.66952(8) 0.81075(13) 1.1689(5) 0.0290(6) Uani 1 1 d . . . C74 C 0.66963(7) 0.75012(12) 1.1664(5) 0.0278(6) Uani 1 1 d . . . C75 C 0.70474(8) 0.73145(13) 1.1223(4) 0.0260(7) Uani 1 1 d . . . C76 C 0.68747(7) 0.56138(13) 0.5993(4) 0.0260(6) Uani 1 1 d . . . H76 H 0.6687 0.5549 0.6836 0.031 Uiso 1 1 calc R . . C77 C 0.70902(8) 0.51849(14) 0.5170(5) 0.0298(7) Uani 1 1 d . . . H77 H 0.7069 0.4782 0.5352 0.036 Uiso 1 1 calc R . . C78 C 0.73423(8) 0.54593(15) 0.4033(5) 0.0305(7) Uani 1 1 d . . . H78 H 0.7520 0.5273 0.3319 0.037 Uiso 1 1 calc R . . C79 C 0.72843(8) 0.60640(14) 0.4142(4) 0.0284(7) Uani 1 1 d . . . H79 H 0.7419 0.6351 0.3526 0.034 Uiso 1 1 calc R . . C80 C 0.69903(8) 0.61638(14) 0.5333(5) 0.0277(7) Uani 1 1 d . . . C81 C 0.68213(8) 0.67272(14) 0.5779(4) 0.0278(6) Uani 1 1 d . . . C82 C 0.70309(8) 0.72256(14) 0.5956(4) 0.0260(6) Uani 1 1 d . . . H82 H 0.7285 0.7196 0.5841 0.031 Uiso 1 1 calc R . . C83 C 0.68758(8) 0.77769(13) 0.6302(5) 0.0280(7) Uani 1 1 d . . . C84 C 0.70199(8) 0.83437(14) 0.5973(4) 0.0302(7) Uani 1 1 d . . . H84 H 0.7273 0.8388 0.5867 0.036 Uiso 1 1 calc R . . C85 C 0.68024(9) 0.88261(14) 0.5807(5) 0.0310(7) Uani 1 1 d . . . H85 H 0.6910 0.9189 0.5574 0.037 Uiso 1 1 calc R . . C86 C 0.64142(9) 0.87879(14) 0.5980(4) 0.0304(7) Uani 1 1 d . . . C87 C 0.61406(9) 0.91654(14) 0.5294(5) 0.0343(7) Uani 1 1 d . . . H87 H 0.6201 0.9554 0.5035 0.041 Uiso 1 1 calc R . . C88 C 0.57893(9) 0.89791(14) 0.4998(5) 0.0343(7) Uani 1 1 d . . . H88 H 0.5615 0.9245 0.4565 0.041 Uiso 1 1 calc R . . C89 C 0.56832(8) 0.83956(14) 0.5330(5) 0.0288(7) Uani 1 1 d . . . C90 C 0.53932(8) 0.80688(15) 0.4562(5) 0.0333(7) Uani 1 1 d . . . H90 H 0.5192 0.8267 0.4074 0.040 Uiso 1 1 calc R . . C91 C 0.53985(8) 0.74702(14) 0.4512(5) 0.0303(7) Uani 1 1 d . . . H91 H 0.5201 0.7272 0.3983 0.036 Uiso 1 1 calc R . . C92 C 0.56925(8) 0.71430(14) 0.5235(5) 0.0279(7) Uani 1 1 d . . . C93 C 0.58104(8) 0.65713(14) 0.4785(5) 0.0294(7) Uani 1 1 d . . . H93 H 0.5643 0.6311 0.4261 0.035 Uiso 1 1 calc R . . C94 C 0.61602(8) 0.63908(13) 0.5094(5) 0.0286(7) Uani 1 1 d . . . H94 H 0.6226 0.6010 0.4767 0.034 Uiso 1 1 calc R . . C95 C 0.64291(8) 0.67588(13) 0.5896(4) 0.0271(6) Uani 1 1 d . . . C96 C 0.65123(7) 0.77724(13) 0.6747(5) 0.0271(6) Uani 1 1 d . . . C97 C 0.62890(7) 0.82605(12) 0.6585(5) 0.0279(6) Uani 1 1 d . . . C98 C 0.59333(7) 0.80677(13) 0.6241(4) 0.0265(7) Uani 1 1 d . . . C99 C 0.59383(8) 0.74622(13) 0.6196(4) 0.0274(7) Uani 1 1 d . . . C100 C 0.62977(7) 0.72775(11) 0.6496(5) 0.0262(6) 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 Fe1 0.02328(18) 0.02657(19) 0.0250(2) 0.0045(2) 0.00109(19) -0.00598(14) Fe2 0.01824(17) 0.02712(18) 0.0242(2) 0.0028(2) 0.00076(18) 0.00230(13) C1 0.0216(13) 0.0376(17) 0.0315(18) 0.0058(13) 0.0045(12) -0.0072(12) C2 0.0280(14) 0.0367(17) 0.0271(19) 0.0022(12) 0.0063(12) -0.0142(12) C3 0.0363(16) 0.0242(14) 0.032(2) 0.0102(12) 0.0071(13) -0.0065(12) C4 0.0303(15) 0.0382(18) 0.0221(18) 0.0057(13) 0.0045(13) -0.0090(13) C5 0.0275(14) 0.0324(15) 0.0209(16) 0.0053(12) 0.0060(12) -0.0066(12) C6 0.0249(14) 0.0348(16) 0.0269(18) 0.0049(13) 0.0055(12) -0.0086(12) C7 0.0280(14) 0.0384(17) 0.0210(18) 0.0101(12) 0.0014(12) -0.0033(12) C8 0.0316(15) 0.0317(16) 0.0245(18) 0.0076(12) 0.0006(13) 0.0030(12) C9 0.0205(13) 0.0425(18) 0.0288(18) 0.0096(14) -0.0008(12) 0.0006(12) C10 0.0253(12) 0.0411(16) 0.0243(18) 0.0058(15) -0.0056(14) -0.0065(11) C11 0.0203(11) 0.0492(17) 0.0193(16) -0.0008(15) -0.0078(13) -0.0048(11) C12 0.0318(14) 0.0433(16) 0.0320(18) -0.0039(18) -0.0001(16) -0.0148(12) C13 0.0350(14) 0.0408(16) 0.0265(17) -0.0041(16) 0.0017(16) -0.0053(12) C14 0.0380(16) 0.0316(16) 0.034(2) -0.0044(13) 0.0028(13) -0.0049(12) C15 0.0463(19) 0.0368(18) 0.038(2) -0.0039(15) 0.0016(16) 0.0041(14) C16 0.0296(15) 0.0416(18) 0.032(2) -0.0033(14) 0.0039(14) 0.0035(13) C17 0.0231(14) 0.0443(18) 0.0328(19) 0.0015(15) 0.0035(13) 0.0082(13) C18 0.0198(14) 0.051(2) 0.032(2) -0.0006(15) 0.0043(13) 0.0017(13) C19 0.0186(12) 0.0436(18) 0.0275(19) 0.0041(14) 0.0030(12) -0.0034(12) C20 0.0221(13) 0.0430(18) 0.0248(19) 0.0006(13) 0.0040(12) -0.0106(12) C21 0.0248(13) 0.0379(16) 0.023(2) 0.0056(12) 0.0020(12) -0.0034(11) C22 0.0269(13) 0.0420(16) 0.0193(17) 0.0049(15) -0.0015(14) -0.0023(11) C23 0.0294(13) 0.0399(16) 0.0208(18) -0.0042(14) 0.0000(14) -0.0058(11) C24 0.0288(14) 0.0385(16) 0.021(2) 0.0026(13) 0.0063(13) 0.0036(11) C25 0.0241(14) 0.0484(19) 0.0213(17) 0.0017(13) 0.0059(11) -0.0124(13) C26 0.0312(15) 0.0368(17) 0.0207(18) 0.0072(12) 0.0011(12) -0.0083(13) C27 0.0350(17) 0.0387(18) 0.029(2) -0.0026(14) 0.0064(14) -0.0124(14) C28 0.0321(16) 0.0342(17) 0.037(2) -0.0004(14) 0.0096(14) -0.0012(13) C29 0.0208(13) 0.0334(15) 0.0333(19) 0.0056(13) 0.0036(12) -0.0045(11) C30 0.0234(13) 0.0363(17) 0.0276(18) 0.0063(13) 0.0069(13) -0.0091(12) C31 0.0272(14) 0.0337(16) 0.0191(16) 0.0081(12) 0.0000(12) -0.0055(12) C32 0.0229(13) 0.0368(16) 0.0198(17) 0.0034(11) 0.0046(11) -0.0060(11) C33 0.0248(12) 0.0367(15) 0.0252(17) 0.0041(14) 0.0066(14) -0.0003(10) C34 0.0257(14) 0.0429(17) 0.033(2) -0.0005(14) 0.0073(13) 0.0022(12) C35 0.0361(16) 0.0346(16) 0.033(2) -0.0054(13) 0.0044(13) 0.0090(13) C36 0.0366(16) 0.0341(16) 0.026(2) -0.0049(12) 0.0004(13) 0.0009(12) C37 0.0487(19) 0.0242(15) 0.035(2) -0.0044(13) -0.0070(15) -0.0010(13) C38 0.0458(18) 0.0268(16) 0.032(2) -0.0009(13) -0.0059(15) -0.0097(13) C39 0.0354(16) 0.0329(16) 0.0282(19) -0.0028(13) -0.0072(14) -0.0099(13) C40 0.0267(14) 0.0411(18) 0.034(2) 0.0036(14) -0.0058(13) -0.0131(13) C41 0.0203(13) 0.0446(18) 0.0285(18) 0.0009(14) -0.0033(12) -0.0054(12) C42 0.0178(12) 0.0408(17) 0.0244(17) 0.0043(13) -0.0069(11) -0.0038(11) C43 0.0194(13) 0.0382(16) 0.0269(18) 0.0049(13) 0.0008(12) 0.0030(12) C44 0.0251(13) 0.0315(16) 0.0269(18) 0.0024(12) -0.0023(12) 0.0001(11) C45 0.0244(14) 0.0331(16) 0.0236(16) 0.0063(12) -0.0036(11) -0.0013(11) C46 0.0281(13) 0.0382(15) 0.0157(17) 0.0006(13) 0.0023(12) -0.0019(11) C47 0.0321(13) 0.0340(14) 0.0212(17) -0.0036(15) 0.0016(15) 0.0000(11) C48 0.0308(13) 0.0378(15) 0.0154(18) -0.0022(12) -0.0055(12) -0.0069(11) C49 0.0262(13) 0.0352(15) 0.0209(19) 0.0058(11) -0.0065(11) -0.0027(11) C50 0.0269(12) 0.0318(13) 0.0154(15) 0.0068(13) -0.0021(14) -0.0002(10) C51 0.0246(13) 0.0316(16) 0.0245(18) 0.0056(12) -0.0057(12) 0.0042(12) C52 0.0229(13) 0.0284(15) 0.0298(19) 0.0037(12) -0.0052(12) 0.0067(11) C53 0.0169(12) 0.0405(17) 0.0269(19) -0.0026(12) -0.0012(11) 0.0035(11) C54 0.0169(12) 0.0386(17) 0.0286(18) 0.0020(13) 0.0003(11) -0.0025(11) C55 0.0221(13) 0.0323(15) 0.0228(17) 0.0006(12) -0.0051(11) 0.0009(11) C56 0.0220(13) 0.0340(16) 0.0250(17) -0.0003(13) -0.0060(12) 0.0041(11) C57 0.0178(12) 0.0418(18) 0.0308(19) 0.0042(14) -0.0047(12) 0.0001(12) C58 0.0231(13) 0.0338(17) 0.029(2) -0.0007(13) -0.0063(12) -0.0024(11) C59 0.0277(15) 0.0421(19) 0.033(2) -0.0028(14) -0.0043(13) -0.0114(13) C60 0.0381(17) 0.0285(16) 0.038(2) 0.0002(14) -0.0096(15) -0.0115(13) C61 0.0437(17) 0.0246(15) 0.027(2) -0.0059(12) -0.0079(14) -0.0041(12) C62 0.0508(19) 0.0271(16) 0.030(2) -0.0060(13) -0.0072(15) -0.0013(14) C63 0.0413(18) 0.0369(17) 0.0274(19) -0.0047(14) -0.0029(14) 0.0109(14) C64 0.0355(15) 0.0381(16) 0.023(2) -0.0046(13) 0.0021(14) 0.0071(12) C65 0.0278(14) 0.0471(18) 0.029(2) -0.0014(14) 0.0074(13) 0.0093(13) C66 0.0211(12) 0.0448(17) 0.026(2) 0.0006(13) 0.0027(12) 0.0014(11) C67 0.0269(13) 0.0381(15) 0.0211(19) 0.0031(13) 0.0050(13) 0.0008(11) C68 0.0264(14) 0.0320(15) 0.0291(18) 0.0037(13) 0.0015(12) -0.0055(12) C69 0.0332(15) 0.0263(14) 0.0215(17) 0.0040(11) -0.0009(12) 0.0019(11) C70 0.0243(13) 0.0305(15) 0.0249(18) 0.0038(12) -0.0033(12) 0.0016(11) C71 0.0256(14) 0.0368(16) 0.0243(18) -0.0028(12) -0.0117(12) -0.0002(12) C72 0.0363(15) 0.0309(15) 0.0212(19) -0.0052(12) -0.0096(13) -0.0030(11) C73 0.0326(13) 0.0372(15) 0.0173(16) -0.0034(15) -0.0020(14) 0.0055(11) C74 0.0308(13) 0.0335(14) 0.0191(15) 0.0021(15) -0.0016(14) -0.0001(11) C75 0.0275(13) 0.0335(15) 0.0169(18) 0.0036(11) -0.0055(11) 0.0025(11) C76 0.0197(13) 0.0348(15) 0.0234(18) 0.0018(11) -0.0030(10) 0.0029(11) C77 0.0261(14) 0.0295(15) 0.0339(19) -0.0022(13) -0.0084(13) 0.0022(11) C78 0.0264(14) 0.0394(18) 0.0257(19) -0.0021(13) -0.0024(12) 0.0064(13) C79 0.0273(14) 0.0353(17) 0.0226(18) 0.0059(12) -0.0017(12) 0.0067(12) C80 0.0230(13) 0.0327(16) 0.0273(18) 0.0045(12) -0.0063(12) 0.0006(11) C81 0.0243(14) 0.0351(16) 0.0239(17) 0.0065(13) -0.0028(12) 0.0014(11) C82 0.0196(12) 0.0380(16) 0.0204(17) 0.0035(11) -0.0012(10) 0.0005(11) C83 0.0256(13) 0.0385(16) 0.0201(19) 0.0009(12) -0.0032(12) -0.0040(11) C84 0.0224(13) 0.0409(17) 0.0272(18) -0.0049(13) 0.0016(11) -0.0060(12) C85 0.0322(15) 0.0341(16) 0.0268(18) -0.0042(13) -0.0010(13) -0.0116(12) C86 0.0342(16) 0.0329(16) 0.0241(19) -0.0076(12) 0.0007(12) -0.0016(12) C87 0.0380(17) 0.0275(16) 0.037(2) -0.0042(13) 0.0043(15) 0.0006(13) C88 0.0346(16) 0.0328(17) 0.036(2) -0.0022(14) 0.0047(14) 0.0089(13) C89 0.0258(14) 0.0334(16) 0.0271(18) -0.0044(12) 0.0058(12) 0.0044(12) C90 0.0200(13) 0.0389(18) 0.041(2) 0.0019(15) 0.0044(13) 0.0061(12) C91 0.0190(12) 0.0392(17) 0.0326(19) -0.0041(14) 0.0022(12) -0.0039(12) C92 0.0195(12) 0.0339(16) 0.0302(18) 0.0030(13) 0.0029(12) -0.0016(11) C93 0.0258(14) 0.0310(16) 0.0315(19) 0.0012(13) 0.0031(12) -0.0062(11) C94 0.0274(14) 0.0279(15) 0.0305(18) 0.0027(12) 0.0072(13) -0.0010(11) C95 0.0261(14) 0.0307(15) 0.0244(17) 0.0070(12) 0.0028(11) 0.0003(11) C96 0.0248(13) 0.0425(16) 0.0141(16) -0.0013(14) -0.0035(12) -0.0029(11) C97 0.0330(13) 0.0332(14) 0.0173(15) -0.0061(15) 0.0039(15) -0.0038(11) C98 0.0246(13) 0.0332(15) 0.0216(19) -0.0038(12) 0.0076(12) 0.0037(11) C99 0.0253(13) 0.0359(15) 0.0211(19) 0.0012(12) 0.0062(11) -0.0054(11) C100 0.0318(13) 0.0285(13) 0.0183(15) 0.0033(14) 0.0037(14) -0.0022(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C2 2.033(3) . ? Fe1 C27 2.038(4) . ? Fe1 C3 2.039(3) . ? Fe1 C26 2.044(3) . ? Fe1 C1 2.046(3) . ? Fe1 C4 2.049(3) . ? Fe1 C28 2.052(3) . ? Fe1 C29 2.060(3) . ? Fe1 C5 2.082(3) . ? Fe1 C30 2.093(3) . ? Fe2 C78 2.031(3) . ? Fe2 C79 2.039(3) . ? Fe2 C54 2.039(3) . ? Fe2 C52 2.040(3) . ? Fe2 C77 2.046(3) . ? Fe2 C53 2.046(3) . ? Fe2 C51 2.051(3) . ? Fe2 C76 2.059(3) . ? Fe2 C55 2.068(3) . ? Fe2 C80 2.080(3) . ? C1 C2 1.418(5) . ? C1 C5 1.436(5) . ? C2 C3 1.417(5) . ? C3 C4 1.424(5) . ? C4 C5 1.444(5) . ? C5 C6 1.468(5) . ? C6 C20 1.427(5) . ? C6 C7 1.462(4) . ? C7 C21 1.376(5) . ? C7 C8 1.446(4) . ? C8 C9 1.390(5) . ? C9 C10 1.431(5) . ? C10 C22 1.391(4) . ? C10 C11 1.433(4) . ? C11 C12 1.378(4) . ? C12 C13 1.447(4) . ? C13 C23 1.388(4) . ? C13 C14 1.447(5) . ? C14 C15 1.386(5) . ? C15 C16 1.435(5) . ? C16 C24 1.388(5) . ? C16 C17 1.442(5) . ? C17 C18 1.400(5) . ? C18 C19 1.439(5) . ? C19 C25 1.390(5) . ? C19 C20 1.432(5) . ? C21 C25 1.410(5) . ? C21 C22 1.411(4) . ? C22 C23 1.392(4) . ? C23 C24 1.412(4) . ? C24 C25 1.409(5) . ? C26 C27 1.430(5) . ? C26 C30 1.432(4) . ? C27 C28 1.398(5) . ? C28 C29 1.419(5) . ? C29 C30 1.429(5) . ? C30 C31 1.473(4) . ? C31 C32 1.402(4) . ? C31 C45 1.463(4) . ? C32 C33 1.430(4) . ? C33 C46 1.383(4) . ? C33 C34 1.448(4) . ? C34 C35 1.392(5) . ? C35 C36 1.448(5) . ? C36 C47 1.377(4) . ? C36 C37 1.444(5) . ? C37 C38 1.376(5) . ? C38 C39 1.445(5) . ? C39 C48 1.393(5) . ? C39 C40 1.439(5) . ? C40 C41 1.383(5) . ? C41 C42 1.447(4) . ? C42 C49 1.394(4) . ? C42 C43 1.437(5) . ? C43 C44 1.402(4) . ? C44 C45 1.443(4) . ? C45 C50 1.379(4) . ? C46 C47 1.414(4) . ? C46 C50 1.417(4) . ? C47 C48 1.416(4) . ? C48 C49 1.402(4) . ? C49 C50 1.417(4) . ? C51 C52 1.426(5) . ? C51 C55 1.440(4) . ? C52 C53 1.410(5) . ? C53 C54 1.410(5) . ? C54 C55 1.433(4) . ? C55 C56 1.475(4) . ? C56 C57 1.399(4) . ? C56 C70 1.465(4) . ? C57 C58 1.440(5) . ? C58 C71 1.378(5) . ? C58 C59 1.435(5) . ? C59 C60 1.387(5) . ? C60 C61 1.432(5) . ? C61 C72 1.380(5) . ? C61 C62 1.451(5) . ? C62 C63 1.396(5) . ? C63 C64 1.433(5) . ? C64 C73 1.385(4) . ? C64 C65 1.436(5) . ? C65 C66 1.397(5) . ? C66 C67 1.445(4) . ? C67 C74 1.381(4) . ? C67 C68 1.434(5) . ? C68 C69 1.392(4) . ? C69 C70 1.443(4) . ? C70 C75 1.380(4) . ? C71 C75 1.403(4) . ? C71 C72 1.411(4) . ? C72 C73 1.417(4) . ? C73 C74 1.410(4) . ? C74 C75 1.412(4) . ? C76 C77 1.417(4) . ? C76 C80 1.435(4) . ? C77 C78 1.413(5) . ? C78 C79 1.425(5) . ? C79 C80 1.424(4) . ? C80 C81 1.490(4) . ? C81 C82 1.402(4) . ? C81 C95 1.460(4) . ? C82 C83 1.429(4) . ? C83 C96 1.389(4) . ? C83 C84 1.443(4) . ? C84 C85 1.388(5) . ? C85 C86 1.449(4) . ? C86 C97 1.386(4) . ? C86 C87 1.436(5) . ? C87 C88 1.391(5) . ? C88 C89 1.434(5) . ? C89 C98 1.379(4) . ? C89 C90 1.436(5) . ? C90 C91 1.393(5) . ? C91 C92 1.435(4) . ? C92 C99 1.376(4) . ? C92 C93 1.439(5) . ? C93 C94 1.384(4) . ? C94 C95 1.443(4) . ? C95 C100 1.375(4) . ? C96 C97 1.410(4) . ? C96 C100 1.412(4) . ? C97 C98 1.417(4) . ? C98 C99 1.409(4) . ? C99 C100 1.419(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Fe1 C27 103.05(13) . . ? C2 Fe1 C3 40.72(14) . . ? C27 Fe1 C3 119.49(14) . . ? C2 Fe1 C26 120.16(13) . . ? C27 Fe1 C26 41.03(14) . . ? C3 Fe1 C26 155.99(13) . . ? C2 Fe1 C1 40.69(13) . . ? C27 Fe1 C1 119.35(14) . . ? C3 Fe1 C1 68.58(13) . . ? C26 Fe1 C1 106.27(13) . . ? C2 Fe1 C4 68.37(13) . . ? C27 Fe1 C4 157.65(15) . . ? C3 Fe1 C4 40.77(14) . . ? C26 Fe1 C4 161.10(14) . . ? C1 Fe1 C4 68.35(14) . . ? C2 Fe1 C28 118.91(14) . . ? C27 Fe1 C28 39.99(15) . . ? C3 Fe1 C28 105.94(14) . . ? C26 Fe1 C28 68.06(14) . . ? C1 Fe1 C28 154.43(14) . . ? C4 Fe1 C28 124.71(15) . . ? C2 Fe1 C29 156.45(13) . . ? C27 Fe1 C29 67.76(14) . . ? C3 Fe1 C29 123.43(13) . . ? C26 Fe1 C29 67.96(13) . . ? C1 Fe1 C29 162.73(13) . . ? C4 Fe1 C29 111.53(14) . . ? C28 Fe1 C29 40.36(13) . . ? C2 Fe1 C5 68.67(12) . . ? C27 Fe1 C5 157.05(14) . . ? C3 Fe1 C5 68.94(13) . . ? C26 Fe1 C5 123.35(13) . . ? C1 Fe1 C5 40.69(13) . . ? C4 Fe1 C5 40.90(13) . . ? C28 Fe1 C5 162.74(14) . . ? C29 Fe1 C5 127.78(13) . . ? C2 Fe1 C30 158.39(13) . . ? C27 Fe1 C30 68.22(13) . . ? C3 Fe1 C30 160.80(14) . . ? C26 Fe1 C30 40.49(13) . . ? C1 Fe1 C30 125.00(13) . . ? C4 Fe1 C30 126.76(14) . . ? C28 Fe1 C30 67.83(13) . . ? C29 Fe1 C30 40.23(12) . . ? C5 Fe1 C30 111.32(13) . . ? C78 Fe2 C79 40.98(14) . . ? C78 Fe2 C54 121.57(13) . . ? C79 Fe2 C54 105.52(14) . . ? C78 Fe2 C52 117.79(13) . . ? C79 Fe2 C52 152.46(13) . . ? C54 Fe2 C52 68.28(13) . . ? C78 Fe2 C77 40.55(14) . . ? C79 Fe2 C77 68.49(14) . . ? C54 Fe2 C77 158.55(13) . . ? C52 Fe2 C77 106.99(13) . . ? C78 Fe2 C53 103.74(13) . . ? C79 Fe2 C53 117.56(13) . . ? C54 Fe2 C53 40.38(13) . . ? C52 Fe2 C53 40.38(13) . . ? C77 Fe2 C53 122.59(13) . . ? C78 Fe2 C51 154.80(13) . . ? C79 Fe2 C51 164.05(13) . . ? C54 Fe2 C51 68.64(13) . . ? C52 Fe2 C51 40.81(13) . . ? C77 Fe2 C51 122.36(14) . . ? C53 Fe2 C51 68.27(13) . . ? C78 Fe2 C76 68.20(12) . . ? C79 Fe2 C76 68.34(12) . . ? C54 Fe2 C76 158.42(12) . . ? C52 Fe2 C76 126.79(12) . . ? C77 Fe2 C76 40.40(12) . . ? C53 Fe2 C76 161.05(13) . . ? C51 Fe2 C76 111.33(13) . . ? C78 Fe2 C55 160.19(13) . . ? C79 Fe2 C55 125.18(13) . . ? C54 Fe2 C55 40.84(12) . . ? C52 Fe2 C55 68.61(12) . . ? C77 Fe2 C55 158.91(13) . . ? C53 Fe2 C55 68.27(12) . . ? C51 Fe2 C55 40.91(13) . . ? C76 Fe2 C55 124.75(12) . . ? C78 Fe2 C80 68.27(13) . . ? C79 Fe2 C80 40.44(13) . . ? C54 Fe2 C80 121.51(13) . . ? C52 Fe2 C80 165.17(13) . . ? C77 Fe2 C80 68.10(12) . . ? C53 Fe2 C80 154.19(13) . . ? C51 Fe2 C80 128.93(13) . . ? C76 Fe2 C80 40.58(12) . . ? C55 Fe2 C80 110.60(12) . . ? C2 C1 C5 108.8(3) . . ? C2 C1 Fe1 69.13(17) . . ? C5 C1 Fe1 71.01(17) . . ? C3 C2 C1 108.6(3) . . ? C3 C2 Fe1 69.87(17) . . ? C1 C2 Fe1 70.18(17) . . ? C2 C3 C4 107.7(3) . . ? C2 C3 Fe1 69.41(17) . . ? C4 C3 Fe1 70.01(18) . . ? C3 C4 C5 108.9(3) . . ? C3 C4 Fe1 69.22(19) . . ? C5 C4 Fe1 70.79(19) . . ? C1 C5 C4 106.0(3) . . ? C1 C5 C6 126.6(3) . . ? C4 C5 C6 127.3(3) . . ? C1 C5 Fe1 68.30(18) . . ? C4 C5 Fe1 68.31(19) . . ? C6 C5 Fe1 130.4(2) . . ? C20 C6 C7 119.0(3) . . ? C20 C6 C5 119.6(3) . . ? C7 C6 C5 121.4(3) . . ? C21 C7 C8 113.8(3) . . ? C21 C7 C6 115.2(3) . . ? C8 C7 C6 129.9(3) . . ? C9 C8 C7 122.3(3) . . ? C8 C9 C10 122.6(3) . . ? C22 C10 C9 113.6(3) . . ? C22 C10 C11 113.9(3) . . ? C9 C10 C11 131.1(3) . . ? C12 C11 C10 123.0(3) . . ? C11 C12 C13 121.7(3) . . ? C23 C13 C14 114.8(3) . . ? C23 C13 C12 113.4(3) . . ? C14 C13 C12 130.6(3) . . ? C15 C14 C13 121.8(3) . . ? C14 C15 C16 122.2(3) . . ? C24 C16 C15 114.3(3) . . ? C24 C16 C17 113.8(3) . . ? C15 C16 C17 130.4(3) . . ? C18 C17 C16 122.4(3) . . ? C17 C18 C19 122.0(3) . . ? C25 C19 C20 114.5(3) . . ? C25 C19 C18 114.0(3) . . ? C20 C19 C18 130.7(3) . . ? C6 C20 C19 123.1(3) . . ? C7 C21 C25 123.9(3) . . ? C7 C21 C22 123.3(3) . . ? C25 C21 C22 107.5(3) . . ? C10 C22 C23 122.6(3) . . ? C10 C22 C21 123.4(3) . . ? C23 C22 C21 108.4(3) . . ? C13 C23 C22 124.2(3) . . ? C13 C23 C24 122.0(3) . . ? C22 C23 C24 108.4(3) . . ? C16 C24 C25 123.4(3) . . ? C16 C24 C23 123.4(3) . . ? C25 C24 C23 107.5(3) . . ? C19 C25 C24 123.3(3) . . ? C19 C25 C21 122.2(3) . . ? C24 C25 C21 108.2(3) . . ? C27 C26 C30 108.1(3) . . ? C27 C26 Fe1 69.26(19) . . ? C30 C26 Fe1 71.61(18) . . ? C28 C27 C26 108.3(3) . . ? C28 C27 Fe1 70.6(2) . . ? C26 C27 Fe1 69.71(19) . . ? C27 C28 C29 108.4(3) . . ? C27 C28 Fe1 69.4(2) . . ? C29 C28 Fe1 70.10(19) . . ? C28 C29 C30 108.7(3) . . ? C28 C29 Fe1 69.54(18) . . ? C30 C29 Fe1 71.14(16) . . ? C29 C30 C26 106.6(3) . . ? C29 C30 C31 125.4(3) . . ? C26 C30 C31 128.0(3) . . ? C29 C30 Fe1 68.63(17) . . ? C26 C30 Fe1 67.90(17) . . ? C31 C30 Fe1 128.5(2) . . ? C32 C31 C45 119.7(3) . . ? C32 C31 C30 121.6(3) . . ? C45 C31 C30 118.5(3) . . ? C31 C32 C33 122.7(3) . . ? C46 C33 C32 115.4(3) . . ? C46 C33 C34 114.1(3) . . ? C32 C33 C34 129.3(3) . . ? C35 C34 C33 122.4(3) . . ? C34 C35 C36 120.8(3) . . ? C47 C36 C37 114.3(3) . . ? C47 C36 C35 115.3(3) . . ? C37 C36 C35 129.1(3) . . ? C38 C37 C36 122.3(3) . . ? C37 C38 C39 122.1(3) . . ? C48 C39 C40 114.3(3) . . ? C48 C39 C38 114.2(3) . . ? C40 C39 C38 130.1(3) . . ? C41 C40 C39 122.2(3) . . ? C40 C41 C42 122.1(3) . . ? C49 C42 C43 115.1(3) . . ? C49 C42 C41 113.9(3) . . ? C43 C42 C41 129.6(3) . . ? C44 C43 C42 121.5(3) . . ? C43 C44 C45 122.2(3) . . ? C50 C45 C44 114.5(3) . . ? C50 C45 C31 115.3(3) . . ? C44 C45 C31 128.7(3) . . ? C33 C46 C47 123.1(3) . . ? C33 C46 C50 122.0(3) . . ? C47 C46 C50 108.1(2) . . ? C36 C47 C46 122.7(3) . . ? C36 C47 C48 123.1(3) . . ? C46 C47 C48 107.7(3) . . ? C39 C48 C49 122.8(3) . . ? C39 C48 C47 122.5(3) . . ? C49 C48 C47 108.3(3) . . ? C42 C49 C48 123.1(3) . . ? C42 C49 C50 122.2(3) . . ? C48 C49 C50 108.3(3) . . ? C45 C50 C49 123.4(3) . . ? C45 C50 C46 123.0(3) . . ? C49 C50 C46 107.6(2) . . ? C52 C51 C55 107.8(3) . . ? C52 C51 Fe2 69.19(19) . . ? C55 C51 Fe2 70.18(19) . . ? C53 C52 C51 108.3(3) . . ? C53 C52 Fe2 70.06(17) . . ? C51 C52 Fe2 70.00(17) . . ? C54 C53 C52 108.5(3) . . ? C54 C53 Fe2 69.53(16) . . ? C52 C53 Fe2 69.57(16) . . ? C53 C54 C55 108.6(3) . . ? C53 C54 Fe2 70.09(17) . . ? C55 C54 Fe2 70.66(17) . . ? C54 C55 C51 106.8(3) . . ? C54 C55 C56 124.7(3) . . ? C51 C55 C56 128.4(3) . . ? C54 C55 Fe2 68.50(18) . . ? C51 C55 Fe2 68.90(18) . . ? C56 C55 Fe2 129.6(2) . . ? C57 C56 C70 119.9(3) . . ? C57 C56 C55 119.0(3) . . ? C70 C56 C55 121.1(3) . . ? C56 C57 C58 123.1(3) . . ? C71 C58 C59 115.4(3) . . ? C71 C58 C57 114.0(3) . . ? C59 C58 C57 129.4(3) . . ? C60 C59 C58 121.2(3) . . ? C59 C60 C61 122.3(3) . . ? C72 C61 C60 114.8(3) . . ? C72 C61 C62 114.6(3) . . ? C60 C61 C62 129.1(3) . . ? C63 C62 C61 121.6(3) . . ? C62 C63 C64 122.0(3) . . ? C73 C64 C63 114.7(3) . . ? C73 C64 C65 114.6(3) . . ? C63 C64 C65 129.5(3) . . ? C66 C65 C64 121.7(3) . . ? C65 C66 C67 121.9(3) . . ? C74 C67 C68 114.5(3) . . ? C74 C67 C66 114.5(3) . . ? C68 C67 C66 129.0(3) . . ? C69 C68 C67 122.1(3) . . ? C68 C69 C70 121.8(3) . . ? C75 C70 C69 114.5(3) . . ? C75 C70 C56 114.6(3) . . ? C69 C70 C56 129.8(3) . . ? C58 C71 C75 123.1(3) . . ? C58 C71 C72 122.4(3) . . ? C75 C71 C72 108.3(3) . . ? C61 C72 C71 122.6(3) . . ? C61 C72 C73 122.8(3) . . ? C71 C72 C73 107.8(3) . . ? C64 C73 C74 123.0(3) . . ? C64 C73 C72 122.9(3) . . ? C74 C73 C72 107.6(2) . . ? C67 C74 C73 122.9(3) . . ? C67 C74 C75 123.2(3) . . ? C73 C74 C75 108.3(3) . . ? C70 C75 C71 123.4(3) . . ? C70 C75 C74 122.8(3) . . ? C71 C75 C74 107.9(3) . . ? C77 C76 C80 108.1(3) . . ? C77 C76 Fe2 69.28(16) . . ? C80 C76 Fe2 70.47(16) . . ? C78 C77 C76 108.3(3) . . ? C78 C77 Fe2 69.18(18) . . ? C76 C77 Fe2 70.33(18) . . ? C77 C78 C79 108.2(3) . . ? C77 C78 Fe2 70.27(19) . . ? C79 C78 Fe2 69.79(19) . . ? C80 C79 C78 108.2(3) . . ? C80 C79 Fe2 71.32(18) . . ? C78 C79 Fe2 69.22(18) . . ? C79 C80 C76 107.2(3) . . ? C79 C80 C81 127.2(3) . . ? C76 C80 C81 125.6(3) . . ? C79 C80 Fe2 68.24(17) . . ? C76 C80 Fe2 68.95(16) . . ? C81 C80 Fe2 129.6(2) . . ? C82 C81 C95 120.4(3) . . ? C82 C81 C80 120.9(3) . . ? C95 C81 C80 118.5(3) . . ? C81 C82 C83 122.4(3) . . ? C96 C83 C82 115.3(3) . . ? C96 C83 C84 114.0(3) . . ? C82 C83 C84 129.8(3) . . ? C85 C84 C83 122.6(3) . . ? C84 C85 C86 121.4(3) . . ? C97 C86 C87 114.8(3) . . ? C97 C86 C85 114.6(3) . . ? C87 C86 C85 129.3(3) . . ? C88 C87 C86 121.9(3) . . ? C87 C88 C89 121.6(3) . . ? C98 C89 C88 115.0(3) . . ? C98 C89 C90 114.0(3) . . ? C88 C89 C90 129.7(3) . . ? C91 C90 C89 121.9(3) . . ? C90 C91 C92 122.1(3) . . ? C99 C92 C91 114.3(3) . . ? C99 C92 C93 114.7(3) . . ? C91 C92 C93 129.4(3) . . ? C94 C93 C92 121.8(3) . . ? C93 C94 C95 122.5(3) . . ? C100 C95 C94 114.1(3) . . ? C100 C95 C81 114.6(3) . . ? C94 C95 C81 129.4(3) . . ? C83 C96 C97 122.9(3) . . ? C83 C96 C100 121.5(3) . . ? C97 C96 C100 108.3(2) . . ? C86 C97 C96 122.9(3) . . ? C86 C97 C98 122.3(3) . . ? C96 C97 C98 107.9(2) . . ? C89 C98 C99 123.4(3) . . ? C89 C98 C97 122.7(3) . . ? C99 C98 C97 107.9(2) . . ? C92 C99 C98 122.9(3) . . ? C92 C99 C100 122.8(3) . . ? C98 C99 C100 108.2(2) . . ? C95 C100 C96 123.9(3) . . ? C95 C100 C99 123.2(3) . . ? C96 C100 C99 107.7(2) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 33.61 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.617 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.074 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 0.000 0.000 -0.034 266 30 ' ' 2 0.500 0.500 -0.029 266 30 ' ' 3 0.106 0.567 0.389 7 1 ' ' 4 0.606 0.933 0.389 7 1 ' ' 5 0.394 0.067 0.889 7 1 ' ' 6 0.894 0.433 0.889 7 1 ' ' _platon_squeeze_details ; The voids are filled with disordered pentane molecules which could not be refined. ;