# 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 2011 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Dr F Gabbai' _publ_contact_author_email 'francois@tamu.edu, gabbai@chem.tamu.edu' loop_ _publ_author_name 'Duxia Cao' 'Haiyan Zhao' F.Gabbai # Attachment '- 1-PF6.cif' data_mm _database_code_depnum_ccdc_archive 'CCDC 817396' #TrackingRef '- 1-PF6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H38 B F6 Fe P' _chemical_formula_weight 634.25 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 20.827(2) _cell_length_b 8.7404(10) _cell_length_c 16.2270(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2953.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.624 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8854 _exptl_absorpt_correction_T_max 0.9695 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24879 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_sigmaI/netI 0.0481 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 24.00 _reflns_number_total 4636 _reflns_number_gt 4011 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker APEX' _computing_data_reduction 'Bruker APEX' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0513P)^2^+3.2170P] 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 constra _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 0.01(2) _refine_ls_number_reflns 4636 _refine_ls_number_parameters 379 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1107 _refine_ls_wR_factor_gt 0.1041 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 0.06726(3) 0.03027(6) 0.30605(4) 0.02393(16) Uani 1 1 d . . . C1 C 0.0147(2) -0.0639(6) 0.4011(3) 0.0308(11) Uani 1 1 d . . . H1A H 0.0330 -0.1133 0.4515 0.037 Uiso 1 1 calc R . . B1 B 0.2146(2) 0.0577(5) 0.4229(3) 0.0231(11) Uani 1 1 d . . . P1 P 0.00239(7) 0.55187(16) 0.12028(9) 0.0431(4) Uani 1 1 d . . . F1 F 0.0417(3) 0.4306(6) 0.0758(4) 0.145(3) Uani 1 1 d . . . C2 C 0.0008(2) -0.1382(6) 0.3271(3) 0.0331(12) Uani 1 1 d . . . H2A H 0.0068 -0.2497 0.3158 0.040 Uiso 1 1 calc R . . F2 F -0.0515(3) 0.5446(6) 0.0535(4) 0.117(2) Uani 1 1 d . . . C3 C -0.0240(2) -0.0282(6) 0.2711(3) 0.0312(11) Uani 1 1 d . . . H3A H -0.0386 -0.0492 0.2135 0.037 Uiso 1 1 calc R . . F3 F -0.02865(19) 0.4147(4) 0.1707(2) 0.0713(10) Uani 1 1 d . . . C4 C -0.0248(2) 0.1144(5) 0.3104(3) 0.0346(10) Uani 1 1 d . . . H4A H -0.0400 0.2130 0.2859 0.042 Uiso 1 1 calc R . . F4 F -0.0378(2) 0.6699(4) 0.1690(2) 0.0831(13) Uani 1 1 d . . . C5 C -0.0008(2) 0.0936(6) 0.3929(3) 0.0354(12) Uani 1 1 d . . . H5A H 0.0041 0.1744 0.4361 0.042 Uiso 1 1 calc R . . F5 F 0.0550(2) 0.5638(5) 0.1938(3) 0.1024(17) Uani 1 1 d . . . C6 C 0.1057(2) 0.0666(5) 0.1876(3) 0.0290(11) Uani 1 1 d . . . F6 F 0.0344(2) 0.6856(5) 0.0706(3) 0.0983(15) Uani 1 1 d . . . C7 C 0.1112(2) 0.1992(5) 0.2349(3) 0.0273(10) Uani 1 1 d . . . H7A H 0.0856 0.2911 0.2187 0.033 Uiso 1 1 calc R . . C8 C 0.14089(19) 0.1963(5) 0.3152(3) 0.0248(9) Uani 1 1 d . . . C9 C 0.1653(2) 0.0564(5) 0.3478(3) 0.0237(10) Uani 1 1 d . . . C10 C 0.15504(18) -0.0818(4) 0.2999(3) 0.0248(9) Uani 1 1 d . . . C11 C 0.1275(2) -0.0735(5) 0.2212(3) 0.0294(11) Uani 1 1 d . . . H11A H 0.1128 -0.1707 0.1947 0.035 Uiso 1 1 calc R . . C12 C 0.0741(2) 0.0711(6) 0.1031(3) 0.0395(13) Uani 1 1 d . . . H12A H 0.1045 0.1122 0.0627 0.059 Uiso 1 1 calc R . . H12B H 0.0360 0.1367 0.1053 0.059 Uiso 1 1 calc R . . H12C H 0.0615 -0.0326 0.0870 0.059 Uiso 1 1 calc R . . C13 C 0.1440(2) 0.3434(5) 0.3617(3) 0.0324(11) Uani 1 1 d . . . H13A H 0.1841 0.3966 0.3482 0.049 Uiso 1 1 calc R . . H13B H 0.1426 0.3224 0.4210 0.049 Uiso 1 1 calc R . . H13C H 0.1074 0.4079 0.3463 0.049 Uiso 1 1 calc R . . C14 C 0.1721(2) -0.2379(5) 0.3331(3) 0.0327(12) Uani 1 1 d . . . H14A H 0.2185 -0.2543 0.3278 0.049 Uiso 1 1 calc R . . H14B H 0.1492 -0.3165 0.3017 0.049 Uiso 1 1 calc R . . H14C H 0.1599 -0.2443 0.3913 0.049 Uiso 1 1 calc R . . C15 C 0.2719(2) 0.1733(5) 0.4113(3) 0.0221(9) Uani 1 1 d . . . C16 C 0.3061(2) 0.1844(5) 0.3356(3) 0.0239(10) Uani 1 1 d . . . C17 C 0.3543(2) 0.2921(5) 0.3260(3) 0.0271(11) Uani 1 1 d . . . H17A H 0.3761 0.2982 0.2747 0.032 Uiso 1 1 calc R . . C18 C 0.3721(2) 0.3916(5) 0.3890(3) 0.0299(11) Uani 1 1 d . . . C19 C 0.3385(2) 0.3800(5) 0.4631(3) 0.0287(10) Uani 1 1 d . . . H19A H 0.3490 0.4479 0.5068 0.034 Uiso 1 1 calc R . . C20 C 0.2903(2) 0.2736(5) 0.4754(3) 0.0266(10) Uani 1 1 d . . . C22 C 0.2941(2) 0.0779(6) 0.2636(3) 0.0319(11) Uani 1 1 d . . . H22A H 0.3310 0.0813 0.2261 0.048 Uiso 1 1 calc R . . H22B H 0.2553 0.1102 0.2343 0.048 Uiso 1 1 calc R . . H22C H 0.2884 -0.0268 0.2840 0.048 Uiso 1 1 calc R . . C23 C 0.4257(2) 0.5049(6) 0.3782(4) 0.0427(13) Uani 1 1 d . . . H23A H 0.4093 0.6086 0.3876 0.064 Uiso 1 1 calc R . . H23B H 0.4427 0.4973 0.3220 0.064 Uiso 1 1 calc R . . H23C H 0.4599 0.4828 0.4178 0.064 Uiso 1 1 calc R . . C21 C 0.2574(3) 0.2709(5) 0.5589(3) 0.0392(12) Uani 1 1 d . . . H21A H 0.2805 0.3379 0.5972 0.059 Uiso 1 1 calc R . . H21B H 0.2573 0.1661 0.5805 0.059 Uiso 1 1 calc R . . H21C H 0.2131 0.3069 0.5531 0.059 Uiso 1 1 calc R . . C24 C 0.2111(2) -0.0562(5) 0.4987(3) 0.0238(10) Uani 1 1 d . . . C25 C 0.2604(2) -0.1627(5) 0.5127(3) 0.0258(10) Uani 1 1 d . . . C26 C 0.2547(2) -0.2704(5) 0.5762(3) 0.0316(11) Uani 1 1 d . . . H26A H 0.2891 -0.3395 0.5862 0.038 Uiso 1 1 calc R . . C27 C 0.2000(2) -0.2786(5) 0.6249(3) 0.0315(11) Uani 1 1 d . . . C28 C 0.1526(2) -0.1703(5) 0.6121(3) 0.0297(11) Uani 1 1 d . . . H28A H 0.1154 -0.1729 0.6458 0.036 Uiso 1 1 calc R . . C29 C 0.1572(2) -0.0582(5) 0.5519(3) 0.0246(10) Uani 1 1 d . . . C31 C 0.3205(2) -0.1703(6) 0.4595(3) 0.0356(12) Uani 1 1 d . . . H31A H 0.3313 -0.0675 0.4398 0.053 Uiso 1 1 calc R . . H31B H 0.3126 -0.2375 0.4122 0.053 Uiso 1 1 calc R . . H31C H 0.3562 -0.2109 0.4921 0.053 Uiso 1 1 calc R . . C32 C 0.1928(3) -0.4009(6) 0.6908(3) 0.0441(14) Uani 1 1 d . . . H32A H 0.2347 -0.4476 0.7018 0.066 Uiso 1 1 calc R . . H32B H 0.1628 -0.4796 0.6716 0.066 Uiso 1 1 calc R . . H32C H 0.1763 -0.3544 0.7415 0.066 Uiso 1 1 calc R . . C30 C 0.1089(2) 0.0678(5) 0.5500(3) 0.0310(11) Uani 1 1 d . . . H30C H 0.0668 0.0277 0.5661 0.046 Uiso 1 1 calc R . . H30B H 0.1064 0.1099 0.4941 0.046 Uiso 1 1 calc R . . H30D H 0.1218 0.1486 0.5884 0.046 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 0.0221(3) 0.0263(3) 0.0234(3) -0.0008(4) -0.0003(3) 0.0012(3) C1 0.025(3) 0.042(3) 0.026(2) 0.005(2) 0.004(2) -0.002(2) B1 0.026(3) 0.020(3) 0.023(3) -0.006(2) 0.003(2) 0.004(2) P1 0.0441(8) 0.0406(8) 0.0444(8) 0.0071(7) 0.0105(6) 0.0097(7) F1 0.213(6) 0.090(4) 0.132(5) 0.030(3) 0.100(5) 0.084(4) C2 0.026(2) 0.036(3) 0.036(3) 0.005(2) 0.003(2) -0.006(2) F2 0.154(5) 0.089(4) 0.106(4) 0.007(3) -0.073(4) 0.002(3) C3 0.021(2) 0.042(3) 0.030(2) 0.002(2) -0.0042(19) -0.002(2) F3 0.084(3) 0.059(2) 0.071(2) 0.0102(19) 0.007(2) -0.010(2) C4 0.027(2) 0.042(3) 0.035(2) 0.005(3) -0.001(3) 0.008(2) F4 0.140(4) 0.064(2) 0.046(2) -0.0011(18) 0.025(2) 0.036(2) C5 0.023(3) 0.043(3) 0.040(3) -0.005(3) 0.004(2) 0.006(2) F5 0.091(3) 0.063(3) 0.154(5) 0.021(3) -0.058(3) -0.010(2) C6 0.023(2) 0.036(3) 0.028(3) 0.002(2) -0.002(2) -0.002(2) F6 0.117(3) 0.065(3) 0.113(4) 0.029(2) 0.062(3) -0.007(2) C7 0.025(2) 0.035(3) 0.023(2) 0.005(2) -0.0048(19) -0.002(2) C8 0.024(2) 0.026(2) 0.025(2) 0.003(2) -0.004(2) 0.0003(17) C9 0.023(2) 0.024(2) 0.023(2) -0.0008(18) 0.004(2) -0.0030(18) C10 0.022(2) 0.027(2) 0.026(2) -0.006(2) 0.000(2) -0.0004(16) C11 0.027(2) 0.032(3) 0.030(3) -0.006(2) 0.005(2) -0.005(2) C12 0.042(3) 0.053(3) 0.024(3) 0.004(2) -0.007(2) -0.010(3) C13 0.034(3) 0.023(2) 0.040(3) 0.003(2) -0.006(2) 0.004(2) C14 0.037(3) 0.024(2) 0.038(3) -0.005(2) -0.004(2) 0.003(2) C15 0.023(2) 0.023(2) 0.020(2) 0.0015(18) -0.0034(17) 0.0010(19) C16 0.021(2) 0.028(2) 0.022(2) -0.0014(18) -0.0009(17) 0.0033(19) C17 0.023(2) 0.030(2) 0.028(3) 0.0045(19) 0.0059(18) 0.0041(19) C18 0.027(3) 0.023(2) 0.039(3) 0.003(2) 0.002(2) 0.001(2) C19 0.034(3) 0.022(2) 0.030(3) -0.006(2) 0.003(2) -0.005(2) C20 0.029(2) 0.030(3) 0.021(2) -0.001(2) 0.001(2) -0.002(2) C22 0.028(3) 0.049(3) 0.019(2) 0.000(2) 0.003(2) -0.007(2) C23 0.043(3) 0.032(3) 0.053(3) -0.006(2) 0.014(3) -0.008(2) C21 0.055(3) 0.038(3) 0.024(2) -0.013(3) 0.006(2) -0.012(3) C24 0.026(2) 0.022(2) 0.023(2) -0.0021(18) -0.0010(19) -0.0018(19) C25 0.031(2) 0.022(2) 0.024(2) 0.001(2) 0.001(2) 0.000(2) C26 0.036(3) 0.025(2) 0.034(3) 0.000(2) -0.007(2) 0.001(2) C27 0.046(3) 0.023(2) 0.025(2) 0.004(2) 0.000(2) -0.007(2) C28 0.038(3) 0.025(2) 0.026(3) -0.004(2) 0.006(2) -0.006(2) C29 0.025(2) 0.027(3) 0.022(2) -0.0034(19) -0.0032(19) -0.003(2) C31 0.026(3) 0.039(3) 0.042(3) 0.009(2) 0.005(2) 0.008(2) C32 0.072(4) 0.028(3) 0.033(3) 0.004(2) 0.004(3) -0.002(3) C30 0.028(3) 0.042(3) 0.023(2) -0.001(2) 0.002(2) -0.001(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 C3 2.049(4) . ? Fe1 C2 2.049(5) . ? Fe1 C4 2.055(4) . ? Fe1 C1 2.062(5) . ? Fe1 C11 2.072(4) . ? Fe1 C5 2.073(5) . ? Fe1 C10 2.077(4) . ? Fe1 C7 2.086(4) . ? Fe1 C6 2.107(5) . ? Fe1 C8 2.116(4) . ? Fe1 C9 2.163(4) . ? C1 C2 1.394(7) . ? C1 C5 1.420(7) . ? C1 H1A 1.0000 . ? B1 C15 1.575(6) . ? B1 C24 1.584(7) . ? B1 C9 1.593(7) . ? P1 F1 1.522(5) . ? P1 F4 1.545(4) . ? P1 F2 1.562(5) . ? P1 F6 1.568(4) . ? P1 F3 1.589(4) . ? P1 F5 1.624(5) . ? C2 C3 1.421(6) . ? C2 H2A 1.0000 . ? C3 C4 1.401(6) . ? C3 H3A 1.0000 . ? C4 C5 1.440(8) . ? C4 H4A 1.0000 . ? C5 H5A 1.0000 . ? C6 C7 1.394(7) . ? C6 C11 1.415(7) . ? C6 C12 1.521(6) . ? C7 C8 1.443(6) . ? C7 H7A 1.0000 . ? C8 C9 1.426(6) . ? C8 C13 1.492(6) . ? C9 C10 1.452(6) . ? C10 C11 1.403(7) . ? C10 C14 1.509(6) . ? C11 H11A 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C20 1.414(6) . ? C15 C16 1.423(6) . ? C16 C17 1.386(6) . ? C16 C22 1.514(6) . ? C17 C18 1.393(6) . ? C17 H17A 0.9500 . ? C18 C19 1.396(6) . ? C18 C23 1.502(6) . ? C19 C20 1.382(6) . ? C19 H19A 0.9500 . ? C20 C21 1.520(7) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C24 C25 1.405(6) . ? C24 C29 1.416(6) . ? C25 C26 1.400(6) . ? C25 C31 1.522(6) . ? C26 C27 1.389(7) . ? C26 H26A 0.9500 . ? C27 C28 1.384(7) . ? C27 C32 1.519(6) . ? C28 C29 1.386(6) . ? C28 H28A 0.9500 . ? C29 C30 1.491(6) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C30 H30C 0.9800 . ? C30 H30B 0.9800 . ? C30 H30D 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Fe1 C2 40.57(18) . . ? C3 Fe1 C4 39.92(18) . . ? C2 Fe1 C4 67.76(19) . . ? C3 Fe1 C1 67.33(18) . . ? C2 Fe1 C1 39.64(19) . . ? C4 Fe1 C1 67.8(2) . . ? C3 Fe1 C11 105.57(18) . . ? C2 Fe1 C11 101.84(19) . . ? C4 Fe1 C11 138.1(2) . . ? C1 Fe1 C11 130.06(18) . . ? C3 Fe1 C5 67.7(2) . . ? C2 Fe1 C5 67.5(2) . . ? C4 Fe1 C5 40.8(2) . . ? C1 Fe1 C5 40.2(2) . . ? C11 Fe1 C5 169.2(2) . . ? C3 Fe1 C10 133.31(18) . . ? C2 Fe1 C10 105.26(18) . . ? C4 Fe1 C10 172.77(17) . . ? C1 Fe1 C10 108.34(19) . . ? C11 Fe1 C10 39.55(19) . . ? C5 Fe1 C10 139.5(2) . . ? C3 Fe1 C7 115.51(18) . . ? C2 Fe1 C7 153.81(18) . . ? C4 Fe1 C7 100.10(19) . . ? C1 Fe1 C7 158.35(19) . . ? C11 Fe1 C7 71.09(19) . . ? C5 Fe1 C7 119.2(2) . . ? C10 Fe1 C7 85.47(18) . . ? C3 Fe1 C6 97.92(18) . . ? C2 Fe1 C6 121.16(18) . . ? C4 Fe1 C6 109.4(2) . . ? C1 Fe1 C6 160.77(19) . . ? C11 Fe1 C6 39.58(18) . . ? C5 Fe1 C6 147.09(19) . . ? C10 Fe1 C6 72.13(19) . . ? C7 Fe1 C6 38.84(18) . . ? C3 Fe1 C8 149.65(17) . . ? C2 Fe1 C8 165.95(18) . . ? C4 Fe1 C8 115.36(17) . . ? C1 Fe1 C8 127.29(19) . . ? C11 Fe1 C8 84.73(18) . . ? C5 Fe1 C8 105.32(19) . . ? C10 Fe1 C8 71.88(16) . . ? C7 Fe1 C8 40.16(17) . . ? C6 Fe1 C8 71.66(18) . . ? C3 Fe1 C9 171.44(18) . . ? C2 Fe1 C9 131.36(17) . . ? C4 Fe1 C9 146.30(19) . . ? C1 Fe1 C9 108.00(18) . . ? C11 Fe1 C9 71.53(17) . . ? C5 Fe1 C9 113.81(18) . . ? C10 Fe1 C9 40.00(16) . . ? C7 Fe1 C9 71.60(17) . . ? C6 Fe1 C9 84.91(17) . . ? C8 Fe1 C9 38.89(16) . . ? C2 C1 C5 108.9(5) . . ? C2 C1 Fe1 69.7(3) . . ? C5 C1 Fe1 70.3(3) . . ? C2 C1 H1A 125.5 . . ? C5 C1 H1A 125.5 . . ? Fe1 C1 H1A 125.5 . . ? C15 B1 C24 122.0(4) . . ? C15 B1 C9 113.7(4) . . ? C24 B1 C9 124.1(4) . . ? F1 P1 F4 177.3(3) . . ? F1 P1 F2 91.6(4) . . ? F4 P1 F2 89.6(3) . . ? F1 P1 F6 92.7(3) . . ? F4 P1 F6 89.7(2) . . ? F2 P1 F6 88.8(3) . . ? F1 P1 F3 86.4(3) . . ? F4 P1 F3 91.1(2) . . ? F2 P1 F3 92.0(3) . . ? F6 P1 F3 178.9(2) . . ? F1 P1 F5 91.8(3) . . ? F4 P1 F5 86.9(3) . . ? F2 P1 F5 176.3(3) . . ? F6 P1 F5 92.5(3) . . ? F3 P1 F5 86.8(2) . . ? C1 C2 C3 108.1(4) . . ? C1 C2 Fe1 70.7(3) . . ? C3 C2 Fe1 69.7(3) . . ? C1 C2 H2A 125.9 . . ? C3 C2 H2A 125.9 . . ? Fe1 C2 H2A 125.9 . . ? C4 C3 C2 108.4(4) . . ? C4 C3 Fe1 70.3(3) . . ? C2 C3 Fe1 69.7(3) . . ? C4 C3 H3A 125.8 . . ? C2 C3 H3A 125.8 . . ? Fe1 C3 H3A 125.8 . . ? C3 C4 C5 107.8(4) . . ? C3 C4 Fe1 69.8(3) . . ? C5 C4 Fe1 70.2(3) . . ? C3 C4 H4A 126.1 . . ? C5 C4 H4A 126.1 . . ? Fe1 C4 H4A 126.1 . . ? C1 C5 C4 106.8(5) . . ? C1 C5 Fe1 69.5(3) . . ? C4 C5 Fe1 68.9(3) . . ? C1 C5 H5A 126.6 . . ? C4 C5 H5A 126.6 . . ? Fe1 C5 H5A 126.6 . . ? C7 C6 C11 118.7(4) . . ? C7 C6 C12 120.7(4) . . ? C11 C6 C12 120.5(4) . . ? C7 C6 Fe1 69.8(3) . . ? C11 C6 Fe1 68.9(3) . . ? C12 C6 Fe1 131.4(3) . . ? C6 C7 C8 121.2(4) . . ? C6 C7 Fe1 71.4(3) . . ? C8 C7 Fe1 71.0(2) . . ? C6 C7 H7A 118.6 . . ? C8 C7 H7A 118.6 . . ? Fe1 C7 H7A 118.6 . . ? C9 C8 C7 120.2(4) . . ? C9 C8 C13 122.4(4) . . ? C7 C8 C13 117.4(4) . . ? C9 C8 Fe1 72.3(2) . . ? C7 C8 Fe1 68.8(2) . . ? C13 C8 Fe1 131.2(3) . . ? C8 C9 C10 117.6(4) . . ? C8 C9 B1 120.5(4) . . ? C10 C9 B1 120.6(4) . . ? C8 C9 Fe1 68.8(2) . . ? C10 C9 Fe1 66.8(2) . . ? B1 C9 Fe1 148.0(3) . . ? C11 C10 C9 120.3(4) . . ? C11 C10 C14 117.9(4) . . ? C9 C10 C14 121.8(4) . . ? C11 C10 Fe1 70.0(3) . . ? C9 C10 Fe1 73.2(2) . . ? C14 C10 Fe1 128.1(3) . . ? C10 C11 C6 121.8(4) . . ? C10 C11 Fe1 70.4(2) . . ? C6 C11 Fe1 71.5(3) . . ? C10 C11 H11A 118.2 . . ? C6 C11 H11A 118.2 . . ? Fe1 C11 H11A 118.2 . . ? C6 C12 H12A 109.5 . . ? C6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C10 C14 H14A 109.5 . . ? C10 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C10 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C15 C16 117.2(4) . . ? C20 C15 B1 121.1(4) . . ? C16 C15 B1 121.7(4) . . ? C17 C16 C15 120.4(4) . . ? C17 C16 C22 116.7(4) . . ? C15 C16 C22 122.8(4) . . ? C16 C17 C18 122.4(4) . . ? C16 C17 H17A 118.8 . . ? C18 C17 H17A 118.8 . . ? C17 C18 C19 117.0(4) . . ? C17 C18 C23 121.6(4) . . ? C19 C18 C23 121.5(4) . . ? C20 C19 C18 122.5(4) . . ? C20 C19 H19A 118.8 . . ? C18 C19 H19A 118.8 . . ? C19 C20 C15 120.6(4) . . ? C19 C20 C21 117.8(4) . . ? C15 C20 C21 121.6(4) . . ? C16 C22 H22A 109.5 . . ? C16 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C16 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C25 C24 C29 118.2(4) . . ? C25 C24 B1 120.6(4) . . ? C29 C24 B1 121.2(4) . . ? C26 C25 C24 120.2(4) . . ? C26 C25 C31 117.2(4) . . ? C24 C25 C31 122.5(4) . . ? C27 C26 C25 121.5(4) . . ? C27 C26 H26A 119.3 . . ? C25 C26 H26A 119.3 . . ? C28 C27 C26 117.7(4) . . ? C28 C27 C32 121.2(4) . . ? C26 C27 C32 121.2(5) . . ? C27 C28 C29 122.7(4) . . ? C27 C28 H28A 118.6 . . ? C29 C28 H28A 118.6 . . ? C28 C29 C24 119.5(4) . . ? C28 C29 C30 119.4(4) . . ? C24 C29 C30 120.8(4) . . ? C25 C31 H31A 109.5 . . ? C25 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C25 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C30 H30C 109.5 . . ? C29 C30 H30B 109.5 . . ? H30C C30 H30B 109.5 . . ? C29 C30 H30D 109.5 . . ? H30C C30 H30D 109.5 . . ? H30B C30 H30D 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 Fe1 C1 C2 38.2(3) . . . . ? C4 Fe1 C1 C2 81.5(3) . . . . ? C11 Fe1 C1 C2 -53.5(4) . . . . ? C5 Fe1 C1 C2 120.0(4) . . . . ? C10 Fe1 C1 C2 -92.0(3) . . . . ? C7 Fe1 C1 C2 140.5(5) . . . . ? C6 Fe1 C1 C2 -3.8(7) . . . . ? C8 Fe1 C1 C2 -172.8(3) . . . . ? C9 Fe1 C1 C2 -134.2(3) . . . . ? C3 Fe1 C1 C5 -81.8(3) . . . . ? C2 Fe1 C1 C5 -120.0(4) . . . . ? C4 Fe1 C1 C5 -38.5(3) . . . . ? C11 Fe1 C1 C5 -173.5(3) . . . . ? C10 Fe1 C1 C5 148.0(3) . . . . ? C7 Fe1 C1 C5 20.5(6) . . . . ? C6 Fe1 C1 C5 -123.8(6) . . . . ? C8 Fe1 C1 C5 67.2(3) . . . . ? C9 Fe1 C1 C5 105.9(3) . . . . ? C5 C1 C2 C3 -0.4(5) . . . . ? Fe1 C1 C2 C3 -59.9(3) . . . . ? C5 C1 C2 Fe1 59.6(3) . . . . ? C3 Fe1 C2 C1 -118.8(4) . . . . ? C4 Fe1 C2 C1 -81.6(3) . . . . ? C11 Fe1 C2 C1 141.1(3) . . . . ? C5 Fe1 C2 C1 -37.2(3) . . . . ? C10 Fe1 C2 C1 100.5(3) . . . . ? C7 Fe1 C2 C1 -147.9(4) . . . . ? C6 Fe1 C2 C1 178.5(3) . . . . ? C8 Fe1 C2 C1 24.2(9) . . . . ? C9 Fe1 C2 C1 65.3(4) . . . . ? C4 Fe1 C2 C3 37.2(3) . . . . ? C1 Fe1 C2 C3 118.8(4) . . . . ? C11 Fe1 C2 C3 -100.2(3) . . . . ? C5 Fe1 C2 C3 81.5(3) . . . . ? C10 Fe1 C2 C3 -140.8(3) . . . . ? C7 Fe1 C2 C3 -29.1(6) . . . . ? C6 Fe1 C2 C3 -62.7(3) . . . . ? C8 Fe1 C2 C3 143.0(7) . . . . ? C9 Fe1 C2 C3 -175.9(3) . . . . ? C1 C2 C3 C4 0.6(5) . . . . ? Fe1 C2 C3 C4 -59.9(3) . . . . ? C1 C2 C3 Fe1 60.5(3) . . . . ? C2 Fe1 C3 C4 119.3(4) . . . . ? C1 Fe1 C3 C4 82.0(3) . . . . ? C11 Fe1 C3 C4 -150.6(3) . . . . ? C5 Fe1 C3 C4 38.3(3) . . . . ? C10 Fe1 C3 C4 176.3(3) . . . . ? C7 Fe1 C3 C4 -74.5(3) . . . . ? C6 Fe1 C3 C4 -110.9(3) . . . . ? C8 Fe1 C3 C4 -43.9(5) . . . . ? C9 Fe1 C3 C4 140.4(11) . . . . ? C4 Fe1 C3 C2 -119.3(4) . . . . ? C1 Fe1 C3 C2 -37.3(3) . . . . ? C11 Fe1 C3 C2 90.1(3) . . . . ? C5 Fe1 C3 C2 -80.9(3) . . . . ? C10 Fe1 C3 C2 57.0(4) . . . . ? C7 Fe1 C3 C2 166.2(3) . . . . ? C6 Fe1 C3 C2 129.9(3) . . . . ? C8 Fe1 C3 C2 -163.2(3) . . . . ? C9 Fe1 C3 C2 21.1(13) . . . . ? C2 C3 C4 C5 -0.7(5) . . . . ? Fe1 C3 C4 C5 -60.2(3) . . . . ? C2 C3 C4 Fe1 59.5(3) . . . . ? C2 Fe1 C4 C3 -37.8(3) . . . . ? C1 Fe1 C4 C3 -80.8(3) . . . . ? C11 Fe1 C4 C3 45.1(4) . . . . ? C5 Fe1 C4 C3 -118.6(4) . . . . ? C10 Fe1 C4 C3 -22.1(19) . . . . ? C7 Fe1 C4 C3 118.0(3) . . . . ? C6 Fe1 C4 C3 78.9(3) . . . . ? C8 Fe1 C4 C3 157.2(3) . . . . ? C9 Fe1 C4 C3 -170.1(3) . . . . ? C3 Fe1 C4 C5 118.6(4) . . . . ? C2 Fe1 C4 C5 80.8(3) . . . . ? C1 Fe1 C4 C5 37.8(3) . . . . ? C11 Fe1 C4 C5 163.7(3) . . . . ? C10 Fe1 C4 C5 96.5(18) . . . . ? C7 Fe1 C4 C5 -123.4(3) . . . . ? C6 Fe1 C4 C5 -162.5(3) . . . . ? C8 Fe1 C4 C5 -84.2(3) . . . . ? C9 Fe1 C4 C5 -51.5(5) . . . . ? C2 C1 C5 C4 -0.1(5) . . . . ? Fe1 C1 C5 C4 59.1(3) . . . . ? C2 C1 C5 Fe1 -59.2(3) . . . . ? C3 C4 C5 C1 0.5(5) . . . . ? Fe1 C4 C5 C1 -59.5(3) . . . . ? C3 C4 C5 Fe1 59.9(3) . . . . ? C3 Fe1 C5 C1 80.8(3) . . . . ? C2 Fe1 C5 C1 36.7(3) . . . . ? C4 Fe1 C5 C1 118.3(4) . . . . ? C11 Fe1 C5 C1 27.7(12) . . . . ? C10 Fe1 C5 C1 -50.6(4) . . . . ? C7 Fe1 C5 C1 -171.5(3) . . . . ? C6 Fe1 C5 C1 149.7(3) . . . . ? C8 Fe1 C5 C1 -130.5(3) . . . . ? C9 Fe1 C5 C1 -90.0(3) . . . . ? C3 Fe1 C5 C4 -37.5(3) . . . . ? C2 Fe1 C5 C4 -81.6(3) . . . . ? C1 Fe1 C5 C4 -118.3(4) . . . . ? C11 Fe1 C5 C4 -90.6(11) . . . . ? C10 Fe1 C5 C4 -168.9(3) . . . . ? C7 Fe1 C5 C4 70.2(3) . . . . ? C6 Fe1 C5 C4 31.4(5) . . . . ? C8 Fe1 C5 C4 111.2(3) . . . . ? C9 Fe1 C5 C4 151.7(3) . . . . ? C3 Fe1 C6 C7 121.4(3) . . . . ? C2 Fe1 C6 C7 157.1(3) . . . . ? C4 Fe1 C6 C7 81.9(3) . . . . ? C1 Fe1 C6 C7 159.9(5) . . . . ? C11 Fe1 C6 C7 -133.7(4) . . . . ? C5 Fe1 C6 C7 60.7(4) . . . . ? C10 Fe1 C6 C7 -105.6(3) . . . . ? C8 Fe1 C6 C7 -29.3(3) . . . . ? C9 Fe1 C6 C7 -66.8(3) . . . . ? C3 Fe1 C6 C11 -104.9(3) . . . . ? C2 Fe1 C6 C11 -69.2(3) . . . . ? C4 Fe1 C6 C11 -144.4(3) . . . . ? C1 Fe1 C6 C11 -66.4(6) . . . . ? C5 Fe1 C6 C11 -165.6(3) . . . . ? C10 Fe1 C6 C11 28.2(3) . . . . ? C7 Fe1 C6 C11 133.7(4) . . . . ? C8 Fe1 C6 C11 104.4(3) . . . . ? C9 Fe1 C6 C11 67.0(3) . . . . ? C3 Fe1 C6 C12 7.8(5) . . . . ? C2 Fe1 C6 C12 43.5(5) . . . . ? C4 Fe1 C6 C12 -31.7(5) . . . . ? C1 Fe1 C6 C12 46.3(8) . . . . ? C11 Fe1 C6 C12 112.7(5) . . . . ? C5 Fe1 C6 C12 -52.9(6) . . . . ? C10 Fe1 C6 C12 140.8(5) . . . . ? C7 Fe1 C6 C12 -113.6(5) . . . . ? C8 Fe1 C6 C12 -142.9(5) . . . . ? C9 Fe1 C6 C12 179.6(5) . . . . ? C11 C6 C7 C8 2.5(6) . . . . ? C12 C6 C7 C8 179.8(4) . . . . ? Fe1 C6 C7 C8 52.8(4) . . . . ? C11 C6 C7 Fe1 -50.2(4) . . . . ? C12 C6 C7 Fe1 127.0(4) . . . . ? C3 Fe1 C7 C6 -69.6(3) . . . . ? C2 Fe1 C7 C6 -49.0(5) . . . . ? C4 Fe1 C7 C6 -108.5(3) . . . . ? C1 Fe1 C7 C6 -162.1(5) . . . . ? C11 Fe1 C7 C6 29.1(3) . . . . ? C5 Fe1 C7 C6 -147.1(3) . . . . ? C10 Fe1 C7 C6 66.9(3) . . . . ? C8 Fe1 C7 C6 133.9(4) . . . . ? C9 Fe1 C7 C6 105.3(3) . . . . ? C3 Fe1 C7 C8 156.5(3) . . . . ? C2 Fe1 C7 C8 177.0(4) . . . . ? C4 Fe1 C7 C8 117.6(3) . . . . ? C1 Fe1 C7 C8 63.9(6) . . . . ? C11 Fe1 C7 C8 -104.8(3) . . . . ? C5 Fe1 C7 C8 78.9(3) . . . . ? C10 Fe1 C7 C8 -67.0(3) . . . . ? C6 Fe1 C7 C8 -133.9(4) . . . . ? C9 Fe1 C7 C8 -28.6(2) . . . . ? C6 C7 C8 C9 0.1(6) . . . . ? Fe1 C7 C8 C9 53.0(4) . . . . ? C6 C7 C8 C13 -179.4(4) . . . . ? Fe1 C7 C8 C13 -126.4(4) . . . . ? C6 C7 C8 Fe1 -52.9(4) . . . . ? C3 Fe1 C8 C9 -179.0(3) . . . . ? C2 Fe1 C8 C9 51.8(8) . . . . ? C4 Fe1 C8 C9 151.5(3) . . . . ? C1 Fe1 C8 C9 71.0(3) . . . . ? C11 Fe1 C8 C9 -66.9(3) . . . . ? C5 Fe1 C8 C9 109.1(3) . . . . ? C10 Fe1 C8 C9 -28.6(3) . . . . ? C7 Fe1 C8 C9 -133.6(4) . . . . ? C6 Fe1 C8 C9 -105.2(3) . . . . ? C3 Fe1 C8 C7 -45.4(5) . . . . ? C2 Fe1 C8 C7 -174.6(7) . . . . ? C4 Fe1 C8 C7 -74.9(3) . . . . ? C1 Fe1 C8 C7 -155.4(3) . . . . ? C11 Fe1 C8 C7 66.7(3) . . . . ? C5 Fe1 C8 C7 -117.3(3) . . . . ? C10 Fe1 C8 C7 105.0(3) . . . . ? C6 Fe1 C8 C7 28.4(3) . . . . ? C9 Fe1 C8 C7 133.6(4) . . . . ? C3 Fe1 C8 C13 63.1(6) . . . . ? C2 Fe1 C8 C13 -66.1(9) . . . . ? C4 Fe1 C8 C13 33.6(5) . . . . ? C1 Fe1 C8 C13 -46.9(5) . . . . ? C11 Fe1 C8 C13 175.1(4) . . . . ? C5 Fe1 C8 C13 -8.9(4) . . . . ? C10 Fe1 C8 C13 -146.5(5) . . . . ? C7 Fe1 C8 C13 108.5(5) . . . . ? C6 Fe1 C8 C13 136.9(4) . . . . ? C9 Fe1 C8 C13 -118.0(5) . . . . ? C7 C8 C9 C10 -4.2(6) . . . . ? C13 C8 C9 C10 175.2(4) . . . . ? Fe1 C8 C9 C10 47.2(3) . . . . ? C7 C8 C9 B1 162.8(4) . . . . ? C13 C8 C9 B1 -17.8(6) . . . . ? Fe1 C8 C9 B1 -145.8(4) . . . . ? C7 C8 C9 Fe1 -51.4(4) . . . . ? C13 C8 C9 Fe1 128.0(4) . . . . ? C15 B1 C9 C8 -48.1(5) . . . . ? C24 B1 C9 C8 137.5(4) . . . . ? C15 B1 C9 C10 118.6(4) . . . . ? C24 B1 C9 C10 -55.9(6) . . . . ? C15 B1 C9 Fe1 -146.7(5) . . . . ? C24 B1 C9 Fe1 38.9(8) . . . . ? C3 Fe1 C9 C8 176.6(11) . . . . ? C2 Fe1 C9 C8 -165.3(3) . . . . ? C4 Fe1 C9 C8 -51.0(4) . . . . ? C1 Fe1 C9 C8 -127.7(3) . . . . ? C11 Fe1 C9 C8 105.1(3) . . . . ? C5 Fe1 C9 C8 -85.0(3) . . . . ? C10 Fe1 C9 C8 135.0(4) . . . . ? C7 Fe1 C9 C8 29.5(3) . . . . ? C6 Fe1 C9 C8 66.9(3) . . . . ? C3 Fe1 C9 C10 41.6(13) . . . . ? C2 Fe1 C9 C10 59.8(3) . . . . ? C4 Fe1 C9 C10 174.0(4) . . . . ? C1 Fe1 C9 C10 97.3(3) . . . . ? C11 Fe1 C9 C10 -29.9(3) . . . . ? C5 Fe1 C9 C10 140.0(3) . . . . ? C7 Fe1 C9 C10 -105.5(3) . . . . ? C6 Fe1 C9 C10 -68.1(3) . . . . ? C8 Fe1 C9 C10 -135.0(4) . . . . ? C3 Fe1 C9 B1 -69.5(14) . . . . ? C2 Fe1 C9 B1 -51.3(6) . . . . ? C4 Fe1 C9 B1 63.0(7) . . . . ? C1 Fe1 C9 B1 -13.8(6) . . . . ? C11 Fe1 C9 B1 -141.0(6) . . . . ? C5 Fe1 C9 B1 28.9(6) . . . . ? C10 Fe1 C9 B1 -111.1(6) . . . . ? C7 Fe1 C9 B1 143.4(6) . . . . ? C6 Fe1 C9 B1 -179.2(6) . . . . ? C8 Fe1 C9 B1 113.9(7) . . . . ? C8 C9 C10 C11 5.9(6) . . . . ? B1 C9 C10 C11 -161.1(4) . . . . ? Fe1 C9 C10 C11 53.9(4) . . . . ? C8 C9 C10 C14 -172.9(4) . . . . ? B1 C9 C10 C14 20.1(6) . . . . ? Fe1 C9 C10 C14 -124.9(4) . . . . ? C8 C9 C10 Fe1 -48.1(4) . . . . ? B1 C9 C10 Fe1 144.9(4) . . . . ? C3 Fe1 C10 C11 55.8(4) . . . . ? C2 Fe1 C10 C11 90.2(3) . . . . ? C4 Fe1 C10 C11 75.2(18) . . . . ? C1 Fe1 C10 C11 131.6(3) . . . . ? C5 Fe1 C10 C11 163.2(3) . . . . ? C7 Fe1 C10 C11 -65.5(3) . . . . ? C6 Fe1 C10 C11 -28.2(3) . . . . ? C8 Fe1 C10 C11 -104.2(3) . . . . ? C9 Fe1 C10 C11 -132.0(4) . . . . ? C3 Fe1 C10 C9 -172.2(3) . . . . ? C2 Fe1 C10 C9 -137.8(3) . . . . ? C4 Fe1 C10 C9 -152.8(17) . . . . ? C1 Fe1 C10 C9 -96.4(3) . . . . ? C11 Fe1 C10 C9 132.0(4) . . . . ? C5 Fe1 C10 C9 -64.7(4) . . . . ? C7 Fe1 C10 C9 66.5(3) . . . . ? C6 Fe1 C10 C9 103.8(3) . . . . ? C8 Fe1 C10 C9 27.9(3) . . . . ? C3 Fe1 C10 C14 -54.6(5) . . . . ? C2 Fe1 C10 C14 -20.2(5) . . . . ? C4 Fe1 C10 C14 -35(2) . . . . ? C1 Fe1 C10 C14 21.2(5) . . . . ? C11 Fe1 C10 C14 -110.4(5) . . . . ? C5 Fe1 C10 C14 52.9(5) . . . . ? C7 Fe1 C10 C14 -175.9(4) . . . . ? C6 Fe1 C10 C14 -138.6(4) . . . . ? C8 Fe1 C10 C14 145.4(5) . . . . ? C9 Fe1 C10 C14 117.6(5) . . . . ? C9 C10 C11 C6 -3.5(6) . . . . ? C14 C10 C11 C6 175.4(4) . . . . ? Fe1 C10 C11 C6 52.0(4) . . . . ? C9 C10 C11 Fe1 -55.4(4) . . . . ? C14 C10 C11 Fe1 123.4(4) . . . . ? C7 C6 C11 C10 -0.8(7) . . . . ? C12 C6 C11 C10 -178.0(4) . . . . ? Fe1 C6 C11 C10 -51.5(4) . . . . ? C7 C6 C11 Fe1 50.7(4) . . . . ? C12 C6 C11 Fe1 -126.6(4) . . . . ? C3 Fe1 C11 C10 -141.3(3) . . . . ? C2 Fe1 C11 C10 -99.7(3) . . . . ? C4 Fe1 C11 C10 -169.5(3) . . . . ? C1 Fe1 C11 C10 -68.1(3) . . . . ? C5 Fe1 C11 C10 -91.2(11) . . . . ? C7 Fe1 C11 C10 106.5(3) . . . . ? C6 Fe1 C11 C10 135.1(4) . . . . ? C8 Fe1 C11 C10 67.7(3) . . . . ? C9 Fe1 C11 C10 30.2(2) . . . . ? C3 Fe1 C11 C6 83.5(3) . . . . ? C2 Fe1 C11 C6 125.2(3) . . . . ? C4 Fe1 C11 C6 55.4(4) . . . . ? C1 Fe1 C11 C6 156.8(3) . . . . ? C5 Fe1 C11 C6 133.7(10) . . . . ? C10 Fe1 C11 C6 -135.1(4) . . . . ? C7 Fe1 C11 C6 -28.6(3) . . . . ? C8 Fe1 C11 C6 -67.4(3) . . . . ? C9 Fe1 C11 C6 -104.9(3) . . . . ? C24 B1 C15 C20 -52.4(6) . . . . ? C9 B1 C15 C20 133.0(4) . . . . ? C24 B1 C15 C16 129.4(4) . . . . ? C9 B1 C15 C16 -45.2(6) . . . . ? C20 C15 C16 C17 -1.3(6) . . . . ? B1 C15 C16 C17 177.0(4) . . . . ? C20 C15 C16 C22 176.2(4) . . . . ? B1 C15 C16 C22 -5.5(6) . . . . ? C15 C16 C17 C18 0.8(6) . . . . ? C22 C16 C17 C18 -176.8(4) . . . . ? C16 C17 C18 C19 -0.8(6) . . . . ? C16 C17 C18 C23 178.5(4) . . . . ? C17 C18 C19 C20 1.2(7) . . . . ? C23 C18 C19 C20 -178.0(5) . . . . ? C18 C19 C20 C15 -1.7(7) . . . . ? C18 C19 C20 C21 179.5(5) . . . . ? C16 C15 C20 C19 1.7(6) . . . . ? B1 C15 C20 C19 -176.6(4) . . . . ? C16 C15 C20 C21 -179.6(4) . . . . ? B1 C15 C20 C21 2.1(7) . . . . ? C15 B1 C24 C25 -58.7(6) . . . . ? C9 B1 C24 C25 115.3(5) . . . . ? C15 B1 C24 C29 124.1(5) . . . . ? C9 B1 C24 C29 -61.9(6) . . . . ? C29 C24 C25 C26 2.0(6) . . . . ? B1 C24 C25 C26 -175.3(4) . . . . ? C29 C24 C25 C31 -179.8(4) . . . . ? B1 C24 C25 C31 2.9(6) . . . . ? C24 C25 C26 C27 2.1(6) . . . . ? C31 C25 C26 C27 -176.1(4) . . . . ? C25 C26 C27 C28 -3.9(7) . . . . ? C25 C26 C27 C32 176.9(4) . . . . ? C26 C27 C28 C29 1.5(7) . . . . ? C32 C27 C28 C29 -179.2(4) . . . . ? C27 C28 C29 C24 2.6(6) . . . . ? C27 C28 C29 C30 -171.1(4) . . . . ? C25 C24 C29 C28 -4.3(6) . . . . ? B1 C24 C29 C28 173.0(4) . . . . ? C25 C24 C29 C30 169.2(4) . . . . ? B1 C24 C29 C30 -13.5(6) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.716 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.062 # Attachment '- 1-F.cif' data_caof _database_code_depnum_ccdc_archive 'CCDC 817397' #TrackingRef '- 1-F.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H38 B F Fe' _chemical_formula_weight 508.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 17.1967(10) _cell_length_b 17.6328(10) _cell_length_c 8.5350(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2588.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 0.609 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8151 _exptl_absorpt_correction_T_max 0.9586 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 31109 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_sigmaI/netI 0.0711 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 28.35 _reflns_number_total 6449 _reflns_number_gt 4877 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker APEX' _computing_data_reduction 'Bruker APEX' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. This crystal proved to be a racemic twin. To account for this situtaion, the TWIN card was added to the ins file. ; _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^)+(0.0214P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constra _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 0.676(11) _refine_ls_number_reflns 6449 _refine_ls_number_parameters 326 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0618 _refine_ls_wR_factor_gt 0.0581 _refine_ls_goodness_of_fit_ref 0.863 _refine_ls_restrained_S_all 0.863 _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 0.124105(16) -0.151082(15) 0.91804(4) 0.01860(7) Uani 1 1 d . . . F1 F 0.12598(6) 0.01836(6) 0.67504(13) 0.0207(3) Uani 1 1 d . . . C1 C 0.12929(15) -0.26198(13) 0.8415(3) 0.0312(6) Uani 1 1 d . . . H1A H 0.1622 -0.3029 0.8881 0.037 Uiso 1 1 calc R . . B1 B 0.18675(14) 0.03338(14) 0.7908(3) 0.0189(5) Uani 1 1 d . . . C2 C 0.15179(14) -0.21270(13) 0.7207(3) 0.0273(6) Uani 1 1 d . . . H2A H 0.2031 -0.2127 0.6654 0.033 Uiso 1 1 calc R . . C3 C 0.08809(14) -0.16275(13) 0.6899(3) 0.0262(6) Uani 1 1 d . . . H3A H 0.0866 -0.1218 0.6089 0.031 Uiso 1 1 calc R . . C4 C 0.02753(15) -0.18188(14) 0.7947(3) 0.0320(6) Uani 1 1 d . . . H4A H -0.0245 -0.1568 0.8005 0.038 Uiso 1 1 calc R . . C5 C 0.05295(14) -0.24288(12) 0.8891(3) 0.0335(6) Uani 1 1 d . . . H5A H 0.0221 -0.2686 0.9731 0.040 Uiso 1 1 calc R . . C6 C 0.13628(14) -0.14950(12) 1.1624(3) 0.0244(5) Uani 1 1 d . . . C7 C 0.20900(13) -0.14699(12) 1.0880(3) 0.0220(5) Uani 1 1 d . . . H7A H 0.2440 -0.1919 1.0994 0.026 Uiso 1 1 calc R . . C8 C 0.22686(12) -0.09340(12) 0.9695(2) 0.0203(5) Uani 1 1 d . . . C9 C 0.17185(10) -0.03629(10) 0.9225(3) 0.0168(4) Uani 1 1 d . . . C10 C 0.09612(13) -0.04232(12) 0.9951(2) 0.0195(5) Uani 1 1 d . . . C11 C 0.08014(13) -0.09602(12) 1.1127(3) 0.0228(5) Uani 1 1 d . . . H11A H 0.0246 -0.1052 1.1415 0.027 Uiso 1 1 calc R . . C12 C 0.11716(15) -0.21034(13) 1.2797(3) 0.0334(6) Uani 1 1 d . . . H12C H 0.1443 -0.1999 1.3783 0.050 Uiso 1 1 calc R . . H12B H 0.1338 -0.2597 1.2389 0.050 Uiso 1 1 calc R . . H12A H 0.0609 -0.2111 1.2983 0.050 Uiso 1 1 calc R . . C13 C 0.30533(11) -0.10245(12) 0.8925(3) 0.0299(6) Uani 1 1 d . . . H13C H 0.3414 -0.0646 0.9349 0.045 Uiso 1 1 calc R . . H13B H 0.3001 -0.0951 0.7792 0.045 Uiso 1 1 calc R . . H13A H 0.3255 -0.1535 0.9134 0.045 Uiso 1 1 calc R . . C14 C 0.02779(11) 0.00666(11) 0.9439(3) 0.0271(6) Uani 1 1 d . . . H14C H 0.0363 0.0590 0.9783 0.041 Uiso 1 1 calc R . . H14B H -0.0202 -0.0128 0.9910 0.041 Uiso 1 1 calc R . . H14A H 0.0233 0.0053 0.8295 0.041 Uiso 1 1 calc R . . C15 C 0.16475(13) 0.11918(12) 0.8633(3) 0.0174(5) Uani 1 1 d . . . C16 C 0.14409(13) 0.17631(13) 0.7533(3) 0.0205(5) Uani 1 1 d . . . C17 C 0.11571(12) 0.24669(14) 0.8026(3) 0.0244(6) Uani 1 1 d . . . H17A H 0.1010 0.2829 0.7257 0.029 Uiso 1 1 calc R . . C18 C 0.10833(13) 0.26558(12) 0.9583(3) 0.0240(6) Uani 1 1 d . . . C19 C 0.13453(13) 0.21254(13) 1.0658(3) 0.0227(6) Uani 1 1 d . . . H19A H 0.1340 0.2255 1.1738 0.027 Uiso 1 1 calc R . . C20 C 0.16167(13) 0.14104(12) 1.0226(3) 0.0192(5) Uani 1 1 d . . . C21 C 0.18405(14) 0.09040(12) 1.1592(3) 0.0282(6) Uani 1 1 d . . . H21C H 0.2115 0.1205 1.2384 0.042 Uiso 1 1 calc R . . H21B H 0.2181 0.0497 1.1219 0.042 Uiso 1 1 calc R . . H21A H 0.1370 0.0684 1.2054 0.042 Uiso 1 1 calc R . . C22 C 0.15107(13) 0.16557(13) 0.5775(3) 0.0271(6) Uani 1 1 d . . . H22C H 0.1420 0.2141 0.5247 0.041 Uiso 1 1 calc R . . H22B H 0.1124 0.1285 0.5422 0.041 Uiso 1 1 calc R . . H22A H 0.2033 0.1471 0.5520 0.041 Uiso 1 1 calc R . . C23 C 0.07274(15) 0.33955(12) 1.0127(3) 0.0358(6) Uani 1 1 d . . . H23C H 0.1089 0.3654 1.0835 0.054 Uiso 1 1 calc R . . H23B H 0.0239 0.3292 1.0680 0.054 Uiso 1 1 calc R . . H23A H 0.0623 0.3719 0.9217 0.054 Uiso 1 1 calc R . . C24 C 0.27169(12) 0.03691(11) 0.6980(2) 0.0196(5) Uani 1 1 d . . . C25 C 0.28066(12) 0.00775(12) 0.5442(3) 0.0217(5) Uani 1 1 d . . . C26 C 0.34864(12) 0.01973(12) 0.4579(3) 0.0266(6) Uani 1 1 d . . . H26A H 0.3515 0.0013 0.3535 0.032 Uiso 1 1 calc R . . C27 C 0.41212(14) 0.05791(12) 0.5207(3) 0.0286(6) Uani 1 1 d . . . C28 C 0.40552(13) 0.08334(12) 0.6712(3) 0.0271(6) Uani 1 1 d . . . H28A H 0.4487 0.1084 0.7175 0.033 Uiso 1 1 calc R . . C29 C 0.33756(13) 0.07401(12) 0.7603(3) 0.0227(5) Uani 1 1 d . . . C30 C 0.34146(11) 0.10207(12) 0.9281(3) 0.0302(5) Uani 1 1 d . . . H30C H 0.3226 0.0623 0.9988 0.045 Uiso 1 1 calc R . . H30B H 0.3089 0.1474 0.9394 0.045 Uiso 1 1 calc R . . H30A H 0.3954 0.1146 0.9546 0.045 Uiso 1 1 calc R . . C31 C 0.22157(13) -0.04324(13) 0.4658(2) 0.0304(6) Uani 1 1 d . . . H31C H 0.2058 -0.0833 0.5387 0.046 Uiso 1 1 calc R . . H31B H 0.2447 -0.0662 0.3721 0.046 Uiso 1 1 calc R . . H31A H 0.1760 -0.0133 0.4356 0.046 Uiso 1 1 calc R . . C32 C 0.48678(12) 0.06498(13) 0.4279(4) 0.0464(7) Uani 1 1 d . . . H32C H 0.5202 0.1034 0.4764 0.070 Uiso 1 1 calc R . . H32B H 0.4747 0.0800 0.3201 0.070 Uiso 1 1 calc R . . H32A H 0.5138 0.0161 0.4273 0.070 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 0.02157(14) 0.01644(13) 0.01779(14) -0.00036(17) 0.00037(17) -0.00184(13) F1 0.0197(6) 0.0222(7) 0.0202(7) 0.0014(6) -0.0030(6) -0.0027(5) C1 0.0478(17) 0.0202(13) 0.0257(13) -0.0059(10) -0.0073(13) -0.0020(12) B1 0.0175(13) 0.0211(14) 0.0181(13) -0.0003(11) -0.0033(11) -0.0018(11) C2 0.0353(14) 0.0257(13) 0.0211(13) -0.0070(11) 0.0014(11) -0.0008(11) C3 0.0338(15) 0.0257(14) 0.0190(13) -0.0031(10) -0.0074(11) -0.0038(11) C4 0.0260(14) 0.0358(14) 0.0342(15) -0.0074(12) -0.0021(11) -0.0064(12) C5 0.0415(15) 0.0279(13) 0.0310(17) -0.0030(12) 0.0027(13) -0.0163(11) C6 0.0408(15) 0.0188(12) 0.0137(11) 0.0004(10) -0.0014(11) -0.0084(11) C7 0.0272(13) 0.0158(11) 0.0229(13) 0.0003(10) -0.0050(10) -0.0005(10) C8 0.0213(12) 0.0190(11) 0.0206(12) -0.0002(9) -0.0046(9) -0.0025(9) C9 0.0177(9) 0.0147(9) 0.0181(10) -0.0027(12) -0.0010(12) -0.0014(8) C10 0.0215(12) 0.0159(12) 0.0210(12) -0.0045(9) 0.0020(9) -0.0025(9) C11 0.0273(13) 0.0193(12) 0.0219(12) -0.0052(10) 0.0050(10) -0.0046(10) C12 0.0530(18) 0.0252(13) 0.0220(13) 0.0040(10) 0.0011(13) -0.0075(12) C13 0.0197(11) 0.0241(12) 0.0461(18) 0.0117(12) 0.0017(12) 0.0053(9) C14 0.0202(11) 0.0236(11) 0.0374(17) 0.0054(11) 0.0055(12) 0.0032(9) C15 0.0141(11) 0.0176(12) 0.0204(12) 0.0017(9) 0.0009(9) -0.0013(9) C16 0.0179(13) 0.0203(12) 0.0233(13) 0.0016(11) -0.0016(10) -0.0034(10) C17 0.0198(14) 0.0162(12) 0.0371(16) 0.0108(11) -0.0029(11) -0.0009(11) C18 0.0192(13) 0.0184(12) 0.0343(17) -0.0035(10) 0.0007(10) -0.0021(9) C19 0.0216(14) 0.0219(13) 0.0247(14) -0.0066(11) 0.0046(10) -0.0051(10) C20 0.0190(12) 0.0183(12) 0.0204(13) 0.0037(10) -0.0013(10) -0.0049(10) C21 0.0422(15) 0.0221(13) 0.0204(13) -0.0006(10) -0.0029(11) -0.0015(11) C22 0.0276(13) 0.0277(14) 0.0260(14) 0.0063(11) -0.0024(10) -0.0012(10) C23 0.0385(15) 0.0249(14) 0.0441(16) -0.0058(12) -0.0030(13) 0.0026(11) C24 0.0207(12) 0.0138(11) 0.0241(13) 0.0041(9) -0.0001(10) 0.0014(9) C25 0.0221(12) 0.0185(11) 0.0246(13) 0.0053(10) 0.0040(11) 0.0007(9) C26 0.0284(13) 0.0220(12) 0.0293(16) 0.0046(10) 0.0091(10) 0.0057(10) C27 0.0217(13) 0.0161(12) 0.0479(17) 0.0080(12) 0.0127(12) 0.0046(10) C28 0.0175(12) 0.0174(12) 0.0464(16) 0.0064(11) 0.0001(12) -0.0009(10) C29 0.0218(12) 0.0153(11) 0.0311(14) 0.0065(10) -0.0011(11) 0.0010(10) C30 0.0240(11) 0.0309(12) 0.0358(14) 0.0002(14) -0.0058(14) -0.0059(9) C31 0.0333(14) 0.0355(15) 0.0225(14) -0.0043(10) 0.0053(10) -0.0023(11) C32 0.0298(13) 0.0319(13) 0.077(2) -0.0034(18) 0.0280(19) 0.0018(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 C4 2.040(2) . ? Fe1 C5 2.044(2) . ? Fe1 C3 2.053(2) . ? Fe1 C7 2.059(2) . ? Fe1 C2 2.060(2) . ? Fe1 C1 2.064(2) . ? Fe1 C11 2.068(2) . ? Fe1 C10 2.084(2) . ? Fe1 C8 2.086(2) . ? Fe1 C6 2.096(2) . ? Fe1 C9 2.1847(17) . ? F1 B1 1.462(3) . ? C1 C2 1.403(3) . ? C1 C5 1.415(3) . ? C1 H1A 1.0000 . ? B1 C24 1.663(3) . ? B1 C15 1.678(3) . ? B1 C9 1.685(3) . ? C2 C3 1.430(3) . ? C2 H2A 1.0000 . ? C3 C4 1.413(3) . ? C3 H3A 1.0000 . ? C4 C5 1.413(3) . ? C4 H4A 1.0000 . ? C5 H5A 1.0000 . ? C6 C7 1.403(3) . ? C6 C11 1.414(3) . ? C6 C12 1.504(3) . ? C7 C8 1.418(3) . ? C7 H7A 1.0000 . ? C8 C9 1.439(3) . ? C8 C13 1.510(3) . ? C9 C10 1.446(3) . ? C10 C11 1.407(3) . ? C10 C14 1.522(3) . ? C11 H11A 1.0000 . ? C12 H12C 0.9800 . ? C12 H12B 0.9800 . ? C12 H12A 0.9800 . ? C13 H13C 0.9800 . ? C13 H13B 0.9800 . ? C13 H13A 0.9800 . ? C14 H14C 0.9800 . ? C14 H14B 0.9800 . ? C14 H14A 0.9800 . ? C15 C20 1.415(3) . ? C15 C16 1.422(3) . ? C16 C17 1.398(3) . ? C16 C22 1.518(3) . ? C17 C18 1.376(4) . ? C17 H17A 0.9500 . ? C18 C19 1.385(3) . ? C18 C23 1.513(3) . ? C19 C20 1.394(3) . ? C19 H19A 0.9500 . ? C20 C21 1.518(3) . ? C21 H21C 0.9800 . ? C21 H21B 0.9800 . ? C21 H21A 0.9800 . ? C22 H22C 0.9800 . ? C22 H22B 0.9800 . ? C22 H22A 0.9800 . ? C23 H23C 0.9800 . ? C23 H23B 0.9800 . ? C23 H23A 0.9800 . ? C24 C29 1.412(3) . ? C24 C25 1.418(3) . ? C25 C26 1.398(3) . ? C25 C31 1.513(3) . ? C26 C27 1.390(3) . ? C26 H26A 0.9500 . ? C27 C28 1.366(3) . ? C27 C32 1.513(3) . ? C28 C29 1.404(3) . ? C28 H28A 0.9500 . ? C29 C30 1.516(4) . ? C30 H30C 0.9800 . ? C30 H30B 0.9800 . ? C30 H30A 0.9800 . ? C31 H31C 0.9800 . ? C31 H31B 0.9800 . ? C31 H31A 0.9800 . ? C32 H32C 0.9800 . ? C32 H32B 0.9800 . ? C32 H32A 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Fe1 C5 40.49(9) . . ? C4 Fe1 C3 40.39(9) . . ? C5 Fe1 C3 68.01(10) . . ? C4 Fe1 C7 161.81(10) . . ? C5 Fe1 C7 122.49(9) . . ? C3 Fe1 C7 152.28(10) . . ? C4 Fe1 C2 68.02(10) . . ? C5 Fe1 C2 67.79(9) . . ? C3 Fe1 C2 40.68(9) . . ? C7 Fe1 C2 115.51(9) . . ? C4 Fe1 C1 67.64(10) . . ? C5 Fe1 C1 40.29(9) . . ? C3 Fe1 C1 67.55(9) . . ? C7 Fe1 C1 103.03(9) . . ? C2 Fe1 C1 39.78(9) . . ? C4 Fe1 C11 104.01(10) . . ? C5 Fe1 C11 104.48(9) . . ? C3 Fe1 C11 134.33(9) . . ? C7 Fe1 C11 71.13(9) . . ? C2 Fe1 C11 171.56(9) . . ? C1 Fe1 C11 135.65(9) . . ? C4 Fe1 C10 102.71(9) . . ? C5 Fe1 C10 128.95(9) . . ? C3 Fe1 C10 108.78(9) . . ? C7 Fe1 C10 84.78(9) . . ? C2 Fe1 C10 142.83(9) . . ? C1 Fe1 C10 169.11(10) . . ? C11 Fe1 C10 39.62(8) . . ? C4 Fe1 C8 158.17(9) . . ? C5 Fe1 C8 156.75(9) . . ? C3 Fe1 C8 120.28(9) . . ? C7 Fe1 C8 39.99(8) . . ? C2 Fe1 C8 103.52(9) . . ? C1 Fe1 C8 119.49(9) . . ? C11 Fe1 C8 84.92(9) . . ? C10 Fe1 C8 71.35(8) . . ? C4 Fe1 C6 126.76(10) . . ? C5 Fe1 C6 100.98(10) . . ? C3 Fe1 C6 167.11(11) . . ? C7 Fe1 C6 39.45(8) . . ? C2 Fe1 C6 142.88(10) . . ? C1 Fe1 C6 108.85(9) . . ? C11 Fe1 C6 39.71(9) . . ? C10 Fe1 C6 72.34(9) . . ? C8 Fe1 C6 72.50(8) . . ? C4 Fe1 C9 124.17(9) . . ? C5 Fe1 C9 163.90(9) . . ? C3 Fe1 C9 102.87(9) . . ? C7 Fe1 C9 71.86(8) . . ? C2 Fe1 C9 114.59(9) . . ? C1 Fe1 C9 150.14(9) . . ? C11 Fe1 C9 71.84(9) . . ? C10 Fe1 C9 39.52(7) . . ? C8 Fe1 C9 39.29(7) . . ? C6 Fe1 C9 86.14(9) . . ? C2 C1 C5 108.6(2) . . ? C2 C1 Fe1 69.98(13) . . ? C5 C1 Fe1 69.11(13) . . ? C2 C1 H1A 125.7 . . ? C5 C1 H1A 125.7 . . ? Fe1 C1 H1A 125.7 . . ? F1 B1 C24 108.22(17) . . ? F1 B1 C15 104.55(17) . . ? C24 B1 C15 109.87(17) . . ? F1 B1 C9 102.13(16) . . ? C24 B1 C9 118.60(17) . . ? C15 B1 C9 112.17(18) . . ? C1 C2 C3 107.8(2) . . ? C1 C2 Fe1 70.23(13) . . ? C3 C2 Fe1 69.40(13) . . ? C1 C2 H2A 126.1 . . ? C3 C2 H2A 126.1 . . ? Fe1 C2 H2A 126.1 . . ? C4 C3 C2 107.5(2) . . ? C4 C3 Fe1 69.29(14) . . ? C2 C3 Fe1 69.92(13) . . ? C4 C3 H3A 126.2 . . ? C2 C3 H3A 126.2 . . ? Fe1 C3 H3A 126.2 . . ? C5 C4 C3 108.3(2) . . ? C5 C4 Fe1 69.91(14) . . ? C3 C4 Fe1 70.31(14) . . ? C5 C4 H4A 125.8 . . ? C3 C4 H4A 125.8 . . ? Fe1 C4 H4A 125.8 . . ? C4 C5 C1 107.7(2) . . ? C4 C5 Fe1 69.60(13) . . ? C1 C5 Fe1 70.60(13) . . ? C4 C5 H5A 126.1 . . ? C1 C5 H5A 126.1 . . ? Fe1 C5 H5A 126.1 . . ? C7 C6 C11 116.9(2) . . ? C7 C6 C12 121.2(2) . . ? C11 C6 C12 121.7(2) . . ? C7 C6 Fe1 68.86(13) . . ? C11 C6 Fe1 69.07(13) . . ? C12 C6 Fe1 129.13(16) . . ? C6 C7 C8 122.5(2) . . ? C6 C7 Fe1 71.68(13) . . ? C8 C7 Fe1 71.01(12) . . ? C6 C7 H7A 117.9 . . ? C8 C7 H7A 117.9 . . ? Fe1 C7 H7A 117.9 . . ? C7 C8 C9 121.5(2) . . ? C7 C8 C13 115.71(19) . . ? C9 C8 C13 122.71(19) . . ? C7 C8 Fe1 69.00(12) . . ? C9 C8 Fe1 74.07(11) . . ? C13 C8 Fe1 127.88(15) . . ? C8 C9 C10 114.90(19) . . ? C8 C9 B1 126.62(18) . . ? C10 C9 B1 118.46(17) . . ? C8 C9 Fe1 66.64(11) . . ? C10 C9 Fe1 66.48(10) . . ? B1 C9 Fe1 136.14(16) . . ? C11 C10 C9 122.1(2) . . ? C11 C10 C14 115.83(19) . . ? C9 C10 C14 122.03(19) . . ? C11 C10 Fe1 69.58(12) . . ? C9 C10 Fe1 74.00(11) . . ? C14 C10 Fe1 127.56(15) . . ? C10 C11 C6 121.9(2) . . ? C10 C11 Fe1 70.80(13) . . ? C6 C11 Fe1 71.21(13) . . ? C10 C11 H11A 118.1 . . ? C6 C11 H11A 118.1 . . ? Fe1 C11 H11A 118.1 . . ? C6 C12 H12C 109.5 . . ? C6 C12 H12B 109.5 . . ? H12C C12 H12B 109.5 . . ? C6 C12 H12A 109.5 . . ? H12C C12 H12A 109.5 . . ? H12B C12 H12A 109.5 . . ? C8 C13 H13C 109.5 . . ? C8 C13 H13B 109.5 . . ? H13C C13 H13B 109.5 . . ? C8 C13 H13A 109.5 . . ? H13C C13 H13A 109.5 . . ? H13B C13 H13A 109.5 . . ? C10 C14 H14C 109.5 . . ? C10 C14 H14B 109.5 . . ? H14C C14 H14B 109.5 . . ? C10 C14 H14A 109.5 . . ? H14C C14 H14A 109.5 . . ? H14B C14 H14A 109.5 . . ? C20 C15 C16 115.6(2) . . ? C20 C15 B1 127.49(19) . . ? C16 C15 B1 116.88(19) . . ? C17 C16 C15 121.2(2) . . ? C17 C16 C22 115.8(2) . . ? C15 C16 C22 123.0(2) . . ? C18 C17 C16 122.5(2) . . ? C18 C17 H17A 118.7 . . ? C16 C17 H17A 118.7 . . ? C17 C18 C19 116.5(2) . . ? C17 C18 C23 122.8(2) . . ? C19 C18 C23 120.7(2) . . ? C18 C19 C20 123.0(2) . . ? C18 C19 H19A 118.5 . . ? C20 C19 H19A 118.5 . . ? C19 C20 C15 120.8(2) . . ? C19 C20 C21 114.5(2) . . ? C15 C20 C21 124.64(19) . . ? C20 C21 H21C 109.5 . . ? C20 C21 H21B 109.5 . . ? H21C C21 H21B 109.5 . . ? C20 C21 H21A 109.5 . . ? H21C C21 H21A 109.5 . . ? H21B C21 H21A 109.5 . . ? C16 C22 H22C 109.5 . . ? C16 C22 H22B 109.5 . . ? H22C C22 H22B 109.5 . . ? C16 C22 H22A 109.5 . . ? H22C C22 H22A 109.5 . . ? H22B C22 H22A 109.5 . . ? C18 C23 H23C 109.5 . . ? C18 C23 H23B 109.5 . . ? H23C C23 H23B 109.5 . . ? C18 C23 H23A 109.5 . . ? H23C C23 H23A 109.5 . . ? H23B C23 H23A 109.5 . . ? C29 C24 C25 115.4(2) . . ? C29 C24 B1 122.87(19) . . ? C25 C24 B1 121.52(19) . . ? C26 C25 C24 121.6(2) . . ? C26 C25 C31 114.7(2) . . ? C24 C25 C31 123.52(19) . . ? C27 C26 C25 121.8(2) . . ? C27 C26 H26A 119.1 . . ? C25 C26 H26A 119.1 . . ? C28 C27 C26 117.2(2) . . ? C28 C27 C32 122.4(2) . . ? C26 C27 C32 120.3(2) . . ? C27 C28 C29 122.7(2) . . ? C27 C28 H28A 118.6 . . ? C29 C28 H28A 118.6 . . ? C28 C29 C24 121.2(2) . . ? C28 C29 C30 115.9(2) . . ? C24 C29 C30 122.8(2) . . ? C29 C30 H30C 109.5 . . ? C29 C30 H30B 109.5 . . ? H30C C30 H30B 109.5 . . ? C29 C30 H30A 109.5 . . ? H30C C30 H30A 109.5 . . ? H30B C30 H30A 109.5 . . ? C25 C31 H31C 109.5 . . ? C25 C31 H31B 109.5 . . ? H31C C31 H31B 109.5 . . ? C25 C31 H31A 109.5 . . ? H31C C31 H31A 109.5 . . ? H31B C31 H31A 109.5 . . ? C27 C32 H32C 109.5 . . ? C27 C32 H32B 109.5 . . ? H32C C32 H32B 109.5 . . ? C27 C32 H32A 109.5 . . ? H32C C32 H32A 109.5 . . ? H32B C32 H32A 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 Fe1 C1 C2 82.04(15) . . . . ? C5 Fe1 C1 C2 120.2(2) . . . . ? C3 Fe1 C1 C2 38.18(14) . . . . ? C7 Fe1 C1 C2 -114.38(15) . . . . ? C11 Fe1 C1 C2 169.39(15) . . . . ? C10 Fe1 C1 C2 110.5(5) . . . . ? C8 Fe1 C1 C2 -74.96(16) . . . . ? C6 Fe1 C1 C2 -155.06(15) . . . . ? C9 Fe1 C1 C2 -38.2(3) . . . . ? C4 Fe1 C1 C5 -38.16(14) . . . . ? C3 Fe1 C1 C5 -82.01(16) . . . . ? C7 Fe1 C1 C5 125.42(15) . . . . ? C2 Fe1 C1 C5 -120.2(2) . . . . ? C11 Fe1 C1 C5 49.2(2) . . . . ? C10 Fe1 C1 C5 -9.7(6) . . . . ? C8 Fe1 C1 C5 164.84(14) . . . . ? C6 Fe1 C1 C5 84.75(16) . . . . ? C9 Fe1 C1 C5 -158.37(17) . . . . ? C5 C1 C2 C3 -1.0(3) . . . . ? Fe1 C1 C2 C3 -59.48(15) . . . . ? C5 C1 C2 Fe1 58.45(16) . . . . ? C4 Fe1 C2 C1 -81.00(16) . . . . ? C5 Fe1 C2 C1 -37.14(14) . . . . ? C3 Fe1 C2 C1 -118.8(2) . . . . ? C7 Fe1 C2 C1 79.48(16) . . . . ? C11 Fe1 C2 C1 -61.3(7) . . . . ? C10 Fe1 C2 C1 -162.97(16) . . . . ? C8 Fe1 C2 C1 120.16(15) . . . . ? C6 Fe1 C2 C1 41.4(2) . . . . ? C9 Fe1 C2 C1 160.22(14) . . . . ? C4 Fe1 C2 C3 37.78(14) . . . . ? C5 Fe1 C2 C3 81.65(15) . . . . ? C7 Fe1 C2 C3 -161.73(13) . . . . ? C1 Fe1 C2 C3 118.8(2) . . . . ? C11 Fe1 C2 C3 57.5(7) . . . . ? C10 Fe1 C2 C3 -44.2(2) . . . . ? C8 Fe1 C2 C3 -121.05(14) . . . . ? C6 Fe1 C2 C3 160.19(17) . . . . ? C9 Fe1 C2 C3 -81.00(15) . . . . ? C1 C2 C3 C4 0.7(3) . . . . ? Fe1 C2 C3 C4 -59.31(16) . . . . ? C1 C2 C3 Fe1 60.01(16) . . . . ? C5 Fe1 C3 C4 37.72(14) . . . . ? C7 Fe1 C3 C4 156.21(18) . . . . ? C2 Fe1 C3 C4 118.8(2) . . . . ? C1 Fe1 C3 C4 81.40(16) . . . . ? C11 Fe1 C3 C4 -51.28(19) . . . . ? C10 Fe1 C3 C4 -87.65(15) . . . . ? C8 Fe1 C3 C4 -166.55(14) . . . . ? C6 Fe1 C3 C4 5.2(5) . . . . ? C9 Fe1 C3 C4 -128.35(14) . . . . ? C4 Fe1 C3 C2 -118.8(2) . . . . ? C5 Fe1 C3 C2 -81.04(15) . . . . ? C7 Fe1 C3 C2 37.5(2) . . . . ? C1 Fe1 C3 C2 -37.36(13) . . . . ? C11 Fe1 C3 C2 -170.04(14) . . . . ? C10 Fe1 C3 C2 153.59(13) . . . . ? C8 Fe1 C3 C2 74.69(16) . . . . ? C6 Fe1 C3 C2 -113.6(4) . . . . ? C9 Fe1 C3 C2 112.89(14) . . . . ? C2 C3 C4 C5 -0.1(3) . . . . ? Fe1 C3 C4 C5 -59.80(16) . . . . ? C2 C3 C4 Fe1 59.71(15) . . . . ? C3 Fe1 C4 C5 119.1(2) . . . . ? C7 Fe1 C4 C5 -23.9(4) . . . . ? C2 Fe1 C4 C5 81.08(15) . . . . ? C1 Fe1 C4 C5 37.97(14) . . . . ? C11 Fe1 C4 C5 -96.00(15) . . . . ? C10 Fe1 C4 C5 -136.74(14) . . . . ? C8 Fe1 C4 C5 151.8(2) . . . . ? C6 Fe1 C4 C5 -59.43(18) . . . . ? C9 Fe1 C4 C5 -173.36(14) . . . . ? C5 Fe1 C4 C3 -119.1(2) . . . . ? C7 Fe1 C4 C3 -143.1(3) . . . . ? C2 Fe1 C4 C3 -38.04(13) . . . . ? C1 Fe1 C4 C3 -81.15(15) . . . . ? C11 Fe1 C4 C3 144.88(14) . . . . ? C10 Fe1 C4 C3 104.14(14) . . . . ? C8 Fe1 C4 C3 32.7(3) . . . . ? C6 Fe1 C4 C3 -178.55(13) . . . . ? C9 Fe1 C4 C3 67.52(17) . . . . ? C3 C4 C5 C1 -0.5(3) . . . . ? Fe1 C4 C5 C1 -60.60(16) . . . . ? C3 C4 C5 Fe1 60.06(16) . . . . ? C2 C1 C5 C4 1.0(3) . . . . ? Fe1 C1 C5 C4 59.96(16) . . . . ? C2 C1 C5 Fe1 -58.99(16) . . . . ? C3 Fe1 C5 C4 -37.63(14) . . . . ? C7 Fe1 C5 C4 171.36(14) . . . . ? C2 Fe1 C5 C4 -81.69(15) . . . . ? C1 Fe1 C5 C4 -118.4(2) . . . . ? C11 Fe1 C5 C4 94.75(16) . . . . ? C10 Fe1 C5 C4 59.27(18) . . . . ? C8 Fe1 C5 C4 -153.6(2) . . . . ? C6 Fe1 C5 C4 135.35(15) . . . . ? C9 Fe1 C5 C4 20.2(4) . . . . ? C4 Fe1 C5 C1 118.4(2) . . . . ? C3 Fe1 C5 C1 80.75(16) . . . . ? C7 Fe1 C5 C1 -70.26(17) . . . . ? C2 Fe1 C5 C1 36.69(14) . . . . ? C11 Fe1 C5 C1 -146.87(14) . . . . ? C10 Fe1 C5 C1 177.65(14) . . . . ? C8 Fe1 C5 C1 -35.2(3) . . . . ? C6 Fe1 C5 C1 -106.27(15) . . . . ? C9 Fe1 C5 C1 138.6(3) . . . . ? C4 Fe1 C6 C7 163.43(14) . . . . ? C5 Fe1 C6 C7 128.71(14) . . . . ? C3 Fe1 C6 C7 159.2(4) . . . . ? C2 Fe1 C6 C7 61.2(2) . . . . ? C1 Fe1 C6 C7 87.71(14) . . . . ? C11 Fe1 C6 C7 -131.80(19) . . . . ? C10 Fe1 C6 C7 -103.68(14) . . . . ? C8 Fe1 C6 C7 -28.24(12) . . . . ? C9 Fe1 C6 C7 -65.86(13) . . . . ? C4 Fe1 C6 C11 -64.78(17) . . . . ? C5 Fe1 C6 C11 -99.50(14) . . . . ? C3 Fe1 C6 C11 -69.0(4) . . . . ? C7 Fe1 C6 C11 131.80(19) . . . . ? C2 Fe1 C6 C11 -167.05(15) . . . . ? C1 Fe1 C6 C11 -140.49(14) . . . . ? C10 Fe1 C6 C11 28.12(13) . . . . ? C8 Fe1 C6 C11 103.55(14) . . . . ? C9 Fe1 C6 C11 65.94(13) . . . . ? C4 Fe1 C6 C12 49.7(3) . . . . ? C5 Fe1 C6 C12 15.0(2) . . . . ? C3 Fe1 C6 C12 45.5(5) . . . . ? C7 Fe1 C6 C12 -113.7(3) . . . . ? C2 Fe1 C6 C12 -52.6(3) . . . . ? C1 Fe1 C6 C12 -26.0(3) . . . . ? C11 Fe1 C6 C12 114.5(3) . . . . ? C10 Fe1 C6 C12 142.6(2) . . . . ? C8 Fe1 C6 C12 -142.0(2) . . . . ? C9 Fe1 C6 C12 -179.6(2) . . . . ? C11 C6 C7 C8 0.6(3) . . . . ? C12 C6 C7 C8 175.7(2) . . . . ? Fe1 C6 C7 C8 51.90(18) . . . . ? C11 C6 C7 Fe1 -51.31(18) . . . . ? C12 C6 C7 Fe1 123.8(2) . . . . ? C4 Fe1 C7 C6 -47.1(4) . . . . ? C5 Fe1 C7 C6 -65.26(16) . . . . ? C3 Fe1 C7 C6 -170.20(17) . . . . ? C2 Fe1 C7 C6 -144.15(14) . . . . ? C1 Fe1 C7 C6 -103.93(14) . . . . ? C11 Fe1 C7 C6 30.22(13) . . . . ? C10 Fe1 C7 C6 68.39(13) . . . . ? C8 Fe1 C7 C6 135.40(19) . . . . ? C9 Fe1 C7 C6 106.65(14) . . . . ? C4 Fe1 C7 C8 177.5(3) . . . . ? C5 Fe1 C7 C8 159.34(13) . . . . ? C3 Fe1 C7 C8 54.4(2) . . . . ? C2 Fe1 C7 C8 80.45(14) . . . . ? C1 Fe1 C7 C8 120.68(13) . . . . ? C11 Fe1 C7 C8 -105.17(14) . . . . ? C10 Fe1 C7 C8 -67.01(13) . . . . ? C6 Fe1 C7 C8 -135.40(19) . . . . ? C9 Fe1 C7 C8 -28.75(12) . . . . ? C6 C7 C8 C9 2.3(3) . . . . ? Fe1 C7 C8 C9 54.51(18) . . . . ? C6 C7 C8 C13 -175.2(2) . . . . ? Fe1 C7 C8 C13 -123.04(18) . . . . ? C6 C7 C8 Fe1 -52.20(19) . . . . ? C4 Fe1 C8 C7 -177.9(2) . . . . ? C5 Fe1 C8 C7 -48.9(3) . . . . ? C3 Fe1 C8 C7 -154.03(13) . . . . ? C2 Fe1 C8 C7 -113.74(13) . . . . ? C1 Fe1 C8 C7 -74.28(15) . . . . ? C11 Fe1 C8 C7 66.47(13) . . . . ? C10 Fe1 C8 C7 104.64(14) . . . . ? C6 Fe1 C8 C7 27.90(12) . . . . ? C9 Fe1 C8 C7 133.80(19) . . . . ? C4 Fe1 C8 C9 48.3(3) . . . . ? C5 Fe1 C8 C9 177.3(2) . . . . ? C3 Fe1 C8 C9 72.17(16) . . . . ? C7 Fe1 C8 C9 -133.80(19) . . . . ? C2 Fe1 C8 C9 112.45(14) . . . . ? C1 Fe1 C8 C9 151.92(14) . . . . ? C11 Fe1 C8 C9 -67.33(14) . . . . ? C10 Fe1 C8 C9 -29.16(14) . . . . ? C6 Fe1 C8 C9 -105.91(15) . . . . ? C4 Fe1 C8 C13 -71.1(3) . . . . ? C5 Fe1 C8 C13 57.9(3) . . . . ? C3 Fe1 C8 C13 -47.2(2) . . . . ? C7 Fe1 C8 C13 106.9(2) . . . . ? C2 Fe1 C8 C13 -6.9(2) . . . . ? C1 Fe1 C8 C13 32.6(2) . . . . ? C11 Fe1 C8 C13 173.34(19) . . . . ? C10 Fe1 C8 C13 -148.5(2) . . . . ? C6 Fe1 C8 C13 134.8(2) . . . . ? C9 Fe1 C8 C13 -119.3(2) . . . . ? C7 C8 C9 C10 -5.1(3) . . . . ? C13 C8 C9 C10 172.3(2) . . . . ? Fe1 C8 C9 C10 47.17(17) . . . . ? C7 C8 C9 B1 176.6(2) . . . . ? C13 C8 C9 B1 -6.0(3) . . . . ? Fe1 C8 C9 B1 -131.1(2) . . . . ? C7 C8 C9 Fe1 -52.24(18) . . . . ? C13 C8 C9 Fe1 125.1(2) . . . . ? F1 B1 C9 C8 121.2(2) . . . . ? C24 B1 C9 C8 2.4(3) . . . . ? C15 B1 C9 C8 -127.4(2) . . . . ? F1 B1 C9 C10 -57.1(2) . . . . ? C24 B1 C9 C10 -175.85(19) . . . . ? C15 B1 C9 C10 54.4(3) . . . . ? F1 B1 C9 Fe1 27.7(3) . . . . ? C24 B1 C9 Fe1 -91.1(2) . . . . ? C15 B1 C9 Fe1 139.12(16) . . . . ? C4 Fe1 C9 C8 -160.41(13) . . . . ? C5 Fe1 C9 C8 -176.1(3) . . . . ? C3 Fe1 C9 C8 -122.51(14) . . . . ? C7 Fe1 C9 C8 29.21(13) . . . . ? C2 Fe1 C9 C8 -81.18(15) . . . . ? C1 Fe1 C9 C8 -55.4(2) . . . . ? C11 Fe1 C9 C8 104.70(15) . . . . ? C10 Fe1 C9 C8 133.5(2) . . . . ? C6 Fe1 C9 C8 66.82(14) . . . . ? C4 Fe1 C9 C10 66.11(17) . . . . ? C5 Fe1 C9 C10 50.4(4) . . . . ? C3 Fe1 C9 C10 104.01(14) . . . . ? C7 Fe1 C9 C10 -104.27(15) . . . . ? C2 Fe1 C9 C10 145.33(14) . . . . ? C1 Fe1 C9 C10 171.12(18) . . . . ? C11 Fe1 C9 C10 -28.79(13) . . . . ? C8 Fe1 C9 C10 -133.5(2) . . . . ? C6 Fe1 C9 C10 -66.67(14) . . . . ? C4 Fe1 C9 B1 -41.2(2) . . . . ? C5 Fe1 C9 B1 -56.9(4) . . . . ? C3 Fe1 C9 B1 -3.3(2) . . . . ? C7 Fe1 C9 B1 148.4(2) . . . . ? C2 Fe1 C9 B1 38.1(2) . . . . ? C1 Fe1 C9 B1 63.8(3) . . . . ? C11 Fe1 C9 B1 -136.1(2) . . . . ? C10 Fe1 C9 B1 -107.3(2) . . . . ? C8 Fe1 C9 B1 119.2(2) . . . . ? C6 Fe1 C9 B1 -173.9(2) . . . . ? C8 C9 C10 C11 5.3(3) . . . . ? B1 C9 C10 C11 -176.27(19) . . . . ? Fe1 C9 C10 C11 52.54(19) . . . . ? C8 C9 C10 C14 -171.91(19) . . . . ? B1 C9 C10 C14 6.5(3) . . . . ? Fe1 C9 C10 C14 -124.7(2) . . . . ? C8 C9 C10 Fe1 -47.25(17) . . . . ? B1 C9 C10 Fe1 131.19(18) . . . . ? C4 Fe1 C10 C11 96.71(15) . . . . ? C5 Fe1 C10 C11 61.80(17) . . . . ? C3 Fe1 C10 C11 138.30(14) . . . . ? C7 Fe1 C10 C11 -66.49(14) . . . . ? C2 Fe1 C10 C11 166.97(16) . . . . ? C1 Fe1 C10 C11 69.9(5) . . . . ? C8 Fe1 C10 C11 -105.13(14) . . . . ? C6 Fe1 C10 C11 -28.18(13) . . . . ? C9 Fe1 C10 C11 -134.1(2) . . . . ? C4 Fe1 C10 C9 -129.15(14) . . . . ? C5 Fe1 C10 C9 -164.06(14) . . . . ? C3 Fe1 C10 C9 -87.56(15) . . . . ? C7 Fe1 C10 C9 67.64(14) . . . . ? C2 Fe1 C10 C9 -58.9(2) . . . . ? C1 Fe1 C10 C9 -156.0(5) . . . . ? C11 Fe1 C10 C9 134.1(2) . . . . ? C8 Fe1 C10 C9 29.01(13) . . . . ? C6 Fe1 C10 C9 105.96(15) . . . . ? C4 Fe1 C10 C14 -10.8(2) . . . . ? C5 Fe1 C10 C14 -45.7(2) . . . . ? C3 Fe1 C10 C14 30.8(2) . . . . ? C7 Fe1 C10 C14 -173.97(19) . . . . ? C2 Fe1 C10 C14 59.5(2) . . . . ? C1 Fe1 C10 C14 -37.6(6) . . . . ? C11 Fe1 C10 C14 -107.5(2) . . . . ? C8 Fe1 C10 C14 147.4(2) . . . . ? C6 Fe1 C10 C14 -135.6(2) . . . . ? C9 Fe1 C10 C14 118.4(2) . . . . ? C9 C10 C11 C6 -2.7(3) . . . . ? C14 C10 C11 C6 174.63(19) . . . . ? Fe1 C10 C11 C6 51.78(19) . . . . ? C9 C10 C11 Fe1 -54.51(19) . . . . ? C14 C10 C11 Fe1 122.85(18) . . . . ? C7 C6 C11 C10 -0.4(3) . . . . ? C12 C6 C11 C10 -175.5(2) . . . . ? Fe1 C6 C11 C10 -51.60(19) . . . . ? C7 C6 C11 Fe1 51.21(18) . . . . ? C12 C6 C11 Fe1 -123.9(2) . . . . ? C4 Fe1 C11 C10 -93.10(14) . . . . ? C5 Fe1 C11 C10 -134.94(13) . . . . ? C3 Fe1 C11 C10 -61.69(18) . . . . ? C7 Fe1 C11 C10 105.19(14) . . . . ? C2 Fe1 C11 C10 -111.9(6) . . . . ? C1 Fe1 C11 C10 -165.31(14) . . . . ? C8 Fe1 C11 C10 66.67(13) . . . . ? C6 Fe1 C11 C10 135.2(2) . . . . ? C9 Fe1 C11 C10 28.73(12) . . . . ? C4 Fe1 C11 C6 131.67(14) . . . . ? C5 Fe1 C11 C6 89.83(15) . . . . ? C3 Fe1 C11 C6 163.07(15) . . . . ? C7 Fe1 C11 C6 -30.04(13) . . . . ? C2 Fe1 C11 C6 112.9(6) . . . . ? C1 Fe1 C11 C6 59.46(19) . . . . ? C10 Fe1 C11 C6 -135.2(2) . . . . ? C8 Fe1 C11 C6 -68.56(14) . . . . ? C9 Fe1 C11 C6 -106.51(14) . . . . ? F1 B1 C15 C20 132.5(2) . . . . ? C24 B1 C15 C20 -111.5(3) . . . . ? C9 B1 C15 C20 22.7(3) . . . . ? F1 B1 C15 C16 -45.1(2) . . . . ? C24 B1 C15 C16 70.9(2) . . . . ? C9 B1 C15 C16 -154.96(19) . . . . ? C20 C15 C16 C17 -5.8(3) . . . . ? B1 C15 C16 C17 172.11(19) . . . . ? C20 C15 C16 C22 174.2(2) . . . . ? B1 C15 C16 C22 -7.9(3) . . . . ? C15 C16 C17 C18 2.0(4) . . . . ? C22 C16 C17 C18 -178.0(2) . . . . ? C16 C17 C18 C19 3.4(4) . . . . ? C16 C17 C18 C23 -175.8(2) . . . . ? C17 C18 C19 C20 -4.8(3) . . . . ? C23 C18 C19 C20 174.4(2) . . . . ? C18 C19 C20 C15 0.9(4) . . . . ? C18 C19 C20 C21 -177.3(2) . . . . ? C16 C15 C20 C19 4.4(4) . . . . ? B1 C15 C20 C19 -173.22(19) . . . . ? C16 C15 C20 C21 -177.6(2) . . . . ? B1 C15 C20 C21 4.7(4) . . . . ? F1 B1 C24 C29 158.43(18) . . . . ? C15 B1 C24 C29 44.8(3) . . . . ? C9 B1 C24 C29 -86.0(3) . . . . ? F1 B1 C24 C25 -16.4(3) . . . . ? C15 B1 C24 C25 -130.0(2) . . . . ? C9 B1 C24 C25 99.2(2) . . . . ? C29 C24 C25 C26 -4.0(3) . . . . ? B1 C24 C25 C26 171.16(19) . . . . ? C29 C24 C25 C31 171.0(2) . . . . ? B1 C24 C25 C31 -13.9(3) . . . . ? C24 C25 C26 C27 2.8(3) . . . . ? C31 C25 C26 C27 -172.5(2) . . . . ? C25 C26 C27 C28 0.1(3) . . . . ? C25 C26 C27 C32 175.7(2) . . . . ? C26 C27 C28 C29 -1.7(3) . . . . ? C32 C27 C28 C29 -177.1(2) . . . . ? C27 C28 C29 C24 0.3(3) . . . . ? C27 C28 C29 C30 177.0(2) . . . . ? C25 C24 C29 C28 2.5(3) . . . . ? B1 C24 C29 C28 -172.61(19) . . . . ? C25 C24 C29 C30 -173.99(19) . . . . ? B1 C24 C29 C30 10.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.309 _refine_diff_density_min -0.355 _refine_diff_density_rms 0.047 _vrf_STRVA01_caof ; PROBLEM: Flack test results are ambiguous. From the CIF: _refine_ls_abs_structure_Flack 0.676 From the CIF: _refine_ls_abs_structure_Flack_su 0.011 RESPONSE: This ambiguity arises from the fact that the crystal is a racemic twin which was refined using the TWIN card. ; data_1 _database_code_depnum_ccdc_archive 'CCDC 817398' #TrackingRef '- 1-CN.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H39 B Cl3 Fe N' _chemical_formula_weight 634.67 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 14.5594(7) _cell_length_b 13.9523(6) _cell_length_c 15.6438(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.5310(10) _cell_angle_gamma 90.00 _cell_volume 3157.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 7957 _cell_measurement_theta_min 4.652 _cell_measurement_theta_max 55.464 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.756 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8635 _exptl_absorpt_correction_T_max 0.9420 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38288 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_sigmaI/netI 0.0350 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 28.31 _reflns_number_total 7834 _reflns_number_gt 6249 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker APEX' _computing_data_reduction 'Bruker APEX' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. The bond distances of Cl1 and C34, Cl2 and C34, Cl3 and C34, Cl11 and C134, Cl12 and C134, Cl13 and C134 are fixed because of the disorder of the solvent. ; _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^)+(0.0509P)^2^+1.8519P] 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 constra _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7834 _refine_ls_number_parameters 409 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0544 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.1077 _refine_ls_wR_factor_gt 0.0988 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.036 _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 0.917478(17) 0.224167(18) 0.370066(16) 0.01559(8) Uani 1 1 d . . . N1 N 0.94311(11) 0.43652(12) 0.16739(11) 0.0253(4) Uani 1 1 d . . . C1 C 1.00574(14) 0.22122(15) 0.48255(12) 0.0256(4) Uani 1 1 d . . . H1 H 0.9898 0.1991 0.5399 0.031 Uiso 1 1 calc R . . C2 C 1.04095(13) 0.16309(15) 0.41940(12) 0.0235(4) Uani 1 1 d . . . H2 H 1.0543 0.0929 0.4244 0.028 Uiso 1 1 calc R . . C3 C 1.05443(13) 0.22233(15) 0.34818(13) 0.0247(4) Uani 1 1 d . . . H3 H 1.0786 0.2008 0.2940 0.030 Uiso 1 1 calc R . . C4 C 1.02683(13) 0.31660(16) 0.36627(14) 0.0270(4) Uani 1 1 d . . . H4 H 1.0287 0.3736 0.3277 0.032 Uiso 1 1 calc R . . C5 C 0.99607(14) 0.31579(16) 0.44996(14) 0.0285(4) Uani 1 1 d . . . H5 H 0.9728 0.3723 0.4804 0.034 Uiso 1 1 calc R . . C6 C 0.79406(12) 0.18201(13) 0.41331(11) 0.0182(4) Uani 1 1 d . . . H6 H 0.7770 0.1731 0.4696 0.022 Uiso 1 1 calc R . . C7 C 0.83078(12) 0.10390(13) 0.37151(12) 0.0191(4) Uani 1 1 d . . . C8 C 0.85661(12) 0.12066(13) 0.28884(11) 0.0177(4) Uani 1 1 d . . . H8 H 0.8831 0.0697 0.2596 0.021 Uiso 1 1 calc R . . C9 C 0.84446(12) 0.21106(12) 0.24764(11) 0.0148(3) Uani 1 1 d . . . C10 C 0.80253(12) 0.29050(12) 0.28743(11) 0.0147(3) Uani 1 1 d . . . C11 C 0.78156(12) 0.27412(13) 0.37415(11) 0.0162(3) Uani 1 1 d . . . C12 C 0.84824(15) 0.00887(14) 0.41609(13) 0.0265(4) Uani 1 1 d . . . H12A H 0.7939 -0.0324 0.4034 0.040 Uiso 1 1 calc R . . H12B H 0.8601 0.0191 0.4783 0.040 Uiso 1 1 calc R . . H12C H 0.9021 -0.0219 0.3955 0.040 Uiso 1 1 calc R . . C13 C 0.87929(13) 0.21725(13) 0.16009(11) 0.0183(4) Uani 1 1 d . . . H13A H 0.9408 0.2467 0.1661 0.027 Uiso 1 1 calc R . . H13B H 0.8367 0.2563 0.1216 0.027 Uiso 1 1 calc R . . H13C H 0.8829 0.1527 0.1360 0.027 Uiso 1 1 calc R . . C14 C 0.74744(13) 0.35070(13) 0.43076(11) 0.0201(4) Uani 1 1 d . . . H14A H 0.6827 0.3654 0.4111 0.030 Uiso 1 1 calc R . . H14B H 0.7849 0.4087 0.4277 0.030 Uiso 1 1 calc R . . H14C H 0.7526 0.3278 0.4903 0.030 Uiso 1 1 calc R . . C15 C 0.70495(11) 0.37820(12) 0.14171(11) 0.0150(3) Uani 1 1 d . . . C16 C 0.65092(12) 0.29570(13) 0.11778(12) 0.0182(4) Uani 1 1 d . . . C17 C 0.59363(13) 0.29158(14) 0.03921(12) 0.0208(4) Uani 1 1 d . . . H17 H 0.5599 0.2344 0.0249 0.025 Uiso 1 1 calc R . . C18 C 0.58447(13) 0.36756(15) -0.01815(12) 0.0231(4) Uani 1 1 d . . . C19 C 0.63258(13) 0.45027(14) 0.00664(12) 0.0211(4) Uani 1 1 d . . . H19 H 0.6252 0.5047 -0.0300 0.025 Uiso 1 1 calc R . . C20 C 0.69173(12) 0.45716(13) 0.08351(11) 0.0176(4) Uani 1 1 d . . . C21 C 0.64471(13) 0.20708(14) 0.17309(13) 0.0239(4) Uani 1 1 d . . . H21A H 0.5854 0.1750 0.1570 0.036 Uiso 1 1 calc R . . H21B H 0.6495 0.2258 0.2338 0.036 Uiso 1 1 calc R . . H21C H 0.6953 0.1632 0.1641 0.036 Uiso 1 1 calc R . . C22 C 0.52461(15) 0.36108(18) -0.10319(13) 0.0324(5) Uani 1 1 d . . . H22A H 0.4741 0.4076 -0.1043 0.049 Uiso 1 1 calc R . . H22B H 0.4990 0.2963 -0.1106 0.049 Uiso 1 1 calc R . . H22C H 0.5619 0.3752 -0.1500 0.049 Uiso 1 1 calc R . . C23 C 0.73459(13) 0.55551(13) 0.10101(12) 0.0201(4) Uani 1 1 d . . . H23A H 0.7331 0.5911 0.0468 0.030 Uiso 1 1 calc R . . H23B H 0.7988 0.5482 0.1267 0.030 Uiso 1 1 calc R . . H23C H 0.6995 0.5907 0.1407 0.030 Uiso 1 1 calc R . . C24 C 0.87516(12) 0.42046(13) 0.19573(11) 0.0173(3) Uani 1 1 d . . . C25 C 0.74213(12) 0.48726(12) 0.28400(11) 0.0165(3) Uani 1 1 d . . . C26 C 0.64651(13) 0.50634(13) 0.28376(11) 0.0190(4) Uani 1 1 d . . . C27 C 0.61536(14) 0.59688(15) 0.30577(13) 0.0254(4) Uani 1 1 d . . . H27 H 0.5507 0.6073 0.3041 0.030 Uiso 1 1 calc R . . C28 C 0.67505(16) 0.67202(15) 0.32993(14) 0.0308(5) Uani 1 1 d . . . C29 C 0.76868(15) 0.65056(14) 0.33994(13) 0.0267(4) Uani 1 1 d . . . H29 H 0.8115 0.6987 0.3610 0.032 Uiso 1 1 calc R . . C30 C 0.80208(13) 0.56005(13) 0.32001(12) 0.0203(4) Uani 1 1 d . . . C31 C 0.90527(14) 0.54400(15) 0.34346(14) 0.0281(4) Uani 1 1 d . . . H31A H 0.9385 0.5633 0.2951 0.042 Uiso 1 1 calc R . . H31B H 0.9168 0.4760 0.3561 0.042 Uiso 1 1 calc R . . H31C H 0.9270 0.5824 0.3942 0.042 Uiso 1 1 calc R . . C32 C 0.57188(13) 0.43198(15) 0.26169(13) 0.0250(4) Uani 1 1 d . . . H32A H 0.5203 0.4440 0.2954 0.038 Uiso 1 1 calc R . . H32B H 0.5972 0.3679 0.2751 0.038 Uiso 1 1 calc R . . H32C H 0.5498 0.4358 0.2002 0.038 Uiso 1 1 calc R . . C33 C 0.6397(2) 0.77175(18) 0.3467(2) 0.0534(8) Uani 1 1 d . . . H33A H 0.6201 0.8035 0.2918 0.080 Uiso 1 1 calc R . . H33B H 0.6892 0.8091 0.3789 0.080 Uiso 1 1 calc R . . H33C H 0.5871 0.7671 0.3804 0.080 Uiso 1 1 calc R . . B1 B 0.77822(13) 0.39248(14) 0.23212(12) 0.0150(4) Uani 1 1 d . . . Cl1 Cl 0.79133(19) 0.9791(2) 0.10286(13) 0.0401(6) Uani 0.582(9) 1 d PD A 1 Cl2 Cl 0.5970(3) 0.9580(4) 0.0507(3) 0.1023(16) Uani 0.582(9) 1 d PD A 1 Cl3 Cl 0.70876(17) 0.79222(13) 0.06973(13) 0.0545(8) Uani 0.582(9) 1 d PD A 1 C34 C 0.7055(8) 0.9127(7) 0.0395(8) 0.029(2) Uani 0.582(9) 1 d PD A 1 H34A H 0.7166 0.9175 -0.0222 0.023(10) Uiso 0.582(9) 1 calc PR A 1 Cl1' Cl 0.7854(5) 0.9685(5) 0.1074(5) 0.115(3) Uani 0.418(9) 1 d P A 2 Cl2' Cl 0.5954(2) 0.9629(2) 0.0468(2) 0.0341(8) Uani 0.418(9) 1 d P A 2 Cl3' Cl 0.7022(4) 0.7986(4) 0.1195(12) 0.187(4) Uani 0.418(9) 1 d P A 2 C34' C 0.7030(14) 0.9006(14) 0.0567(14) 0.059(5) Uani 0.418(9) 1 d P A 2 H34B H 0.7195 0.8834 -0.0017 0.11(4) Uiso 0.418(9) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01459(13) 0.01903(14) 0.01309(13) 0.00096(10) 0.00137(9) 0.00165(10) N1 0.0211(8) 0.0236(8) 0.0319(9) 0.0056(7) 0.0057(7) -0.0013(7) C1 0.0211(9) 0.0387(12) 0.0159(9) -0.0009(8) -0.0035(7) 0.0060(8) C2 0.0174(9) 0.0294(10) 0.0226(9) 0.0005(8) -0.0029(7) 0.0062(8) C3 0.0153(9) 0.0365(11) 0.0220(9) -0.0010(8) 0.0012(7) 0.0006(8) C4 0.0179(9) 0.0299(11) 0.0313(11) 0.0044(9) -0.0053(8) -0.0056(8) C5 0.0215(10) 0.0308(11) 0.0309(11) -0.0104(9) -0.0070(8) 0.0023(8) C6 0.0170(8) 0.0219(9) 0.0163(8) 0.0053(7) 0.0040(7) 0.0016(7) C7 0.0166(8) 0.0187(9) 0.0224(9) 0.0056(7) 0.0036(7) 0.0013(7) C8 0.0171(8) 0.0174(8) 0.0184(9) -0.0020(7) 0.0018(7) 0.0008(7) C9 0.0131(8) 0.0176(8) 0.0132(8) 0.0008(6) -0.0001(6) -0.0001(6) C10 0.0117(8) 0.0180(8) 0.0141(8) 0.0004(6) 0.0007(6) -0.0016(6) C11 0.0145(8) 0.0185(8) 0.0157(8) 0.0014(7) 0.0022(6) 0.0003(7) C12 0.0312(11) 0.0218(10) 0.0283(10) 0.0087(8) 0.0114(8) 0.0067(8) C13 0.0212(9) 0.0196(9) 0.0145(8) -0.0009(7) 0.0039(7) 0.0019(7) C14 0.0251(9) 0.0199(9) 0.0161(8) 0.0019(7) 0.0060(7) 0.0046(7) C15 0.0127(8) 0.0165(8) 0.0160(8) -0.0001(6) 0.0025(6) 0.0013(6) C16 0.0142(8) 0.0197(9) 0.0208(9) -0.0016(7) 0.0031(7) 0.0008(7) C17 0.0157(9) 0.0228(9) 0.0238(9) -0.0060(7) 0.0015(7) 0.0001(7) C18 0.0165(9) 0.0338(11) 0.0185(9) -0.0034(8) 0.0000(7) 0.0051(8) C19 0.0214(9) 0.0247(9) 0.0172(9) 0.0043(7) 0.0024(7) 0.0071(7) C20 0.0160(8) 0.0210(9) 0.0163(8) 0.0001(7) 0.0044(7) 0.0025(7) C21 0.0193(9) 0.0210(9) 0.0304(10) 0.0019(8) -0.0015(8) -0.0053(7) C22 0.0262(11) 0.0464(13) 0.0227(10) -0.0046(9) -0.0059(8) 0.0057(10) C23 0.0234(9) 0.0175(9) 0.0196(9) 0.0040(7) 0.0033(7) 0.0021(7) C24 0.0183(9) 0.0161(8) 0.0169(8) 0.0026(7) -0.0005(7) 0.0004(7) C25 0.0182(8) 0.0162(8) 0.0152(8) 0.0021(6) 0.0024(7) 0.0008(7) C26 0.0222(9) 0.0206(9) 0.0147(8) 0.0006(7) 0.0038(7) 0.0011(7) C27 0.0242(10) 0.0281(10) 0.0239(10) -0.0024(8) 0.0029(8) 0.0082(8) C28 0.0362(12) 0.0222(10) 0.0342(12) -0.0055(9) 0.0049(9) 0.0073(9) C29 0.0313(11) 0.0184(9) 0.0302(11) -0.0052(8) 0.0031(8) -0.0028(8) C30 0.0226(9) 0.0200(9) 0.0184(9) 0.0004(7) 0.0023(7) -0.0010(7) C31 0.0236(10) 0.0273(10) 0.0317(11) -0.0080(9) -0.0039(8) -0.0021(8) C32 0.0175(9) 0.0307(11) 0.0280(10) -0.0044(8) 0.0073(8) -0.0011(8) C33 0.0502(16) 0.0262(12) 0.083(2) -0.0172(13) 0.0039(15) 0.0106(11) B1 0.0152(9) 0.0159(9) 0.0141(9) 0.0021(7) 0.0020(7) -0.0002(7) Cl1 0.0422(10) 0.0183(7) 0.0530(11) 0.0028(6) -0.0242(7) -0.0030(6) Cl2 0.066(2) 0.140(4) 0.102(3) 0.006(2) 0.016(2) 0.024(2) Cl3 0.0588(11) 0.0213(6) 0.0807(15) 0.0027(6) -0.0039(9) -0.0079(6) C34 0.034(4) 0.017(2) 0.037(4) 0.002(3) 0.002(3) 0.002(2) Cl1' 0.090(3) 0.043(2) 0.197(6) 0.003(2) -0.043(3) -0.005(2) Cl2' 0.0186(13) 0.0448(14) 0.0392(15) -0.0027(10) 0.0046(10) 0.0115(10) Cl3' 0.104(3) 0.051(2) 0.425(13) 0.080(4) 0.112(5) 0.0125(17) C34' 0.037(6) 0.077(12) 0.065(11) -0.033(8) 0.022(6) -0.014(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C5 2.045(2) . ? Fe1 C4 2.055(2) . ? Fe1 C8 2.0566(18) . ? Fe1 C1 2.0580(19) . ? Fe1 C2 2.0586(18) . ? Fe1 C3 2.0613(19) . ? Fe1 C6 2.0757(18) . ? Fe1 C9 2.0901(17) . ? Fe1 C7 2.1015(18) . ? Fe1 C11 2.1058(17) . ? Fe1 C10 2.1992(17) . ? N1 C24 1.151(2) . ? C1 C5 1.416(3) . ? C1 C2 1.418(3) . ? C1 H1 1.0000 . ? C2 C3 1.419(3) . ? C2 H2 1.0000 . ? C3 C4 1.413(3) . ? C3 H3 1.0000 . ? C4 C5 1.431(3) . ? C4 H4 1.0000 . ? C5 H5 1.0000 . ? C6 C7 1.407(3) . ? C6 C11 1.426(2) . ? C6 H6 0.9500 . ? C7 C8 1.407(3) . ? C7 C12 1.506(3) . ? C8 C9 1.418(2) . ? C8 H8 0.9500 . ? C9 C10 1.441(2) . ? C9 C13 1.516(2) . ? C10 C11 1.442(2) . ? C10 B1 1.682(3) . ? C11 C14 1.507(2) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.420(2) . ? C15 C20 1.428(2) . ? C15 B1 1.684(3) . ? C16 C17 1.406(3) . ? C16 C21 1.518(3) . ? C17 C18 1.386(3) . ? C17 H17 0.9500 . ? C18 C19 1.382(3) . ? C18 C22 1.508(3) . ? C19 C20 1.401(3) . ? C19 H19 0.9500 . ? C20 C23 1.519(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 B1 1.628(3) . ? C25 C30 1.414(3) . ? C25 C26 1.417(3) . ? C25 B1 1.668(3) . ? C26 C27 1.398(3) . ? C26 C32 1.514(3) . ? C27 C28 1.386(3) . ? C27 H27 0.9500 . ? C28 C29 1.387(3) . ? C28 C33 1.517(3) . ? C29 C30 1.401(3) . ? C29 H29 0.9500 . ? C30 C31 1.522(3) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? Cl1 C34 1.767(13) . ? Cl2 C34 1.728(12) . ? Cl3 C34 1.745(9) . ? C34 H34A 1.0000 . ? Cl1' C34' 1.66(2) . ? Cl2' C34' 1.78(2) . ? Cl3' C34' 1.730(17) . ? C34' H34B 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Fe1 C4 40.86(9) . . ? C5 Fe1 C8 171.35(8) . . ? C4 Fe1 C8 134.72(8) . . ? C5 Fe1 C1 40.37(9) . . ? C4 Fe1 C1 68.09(8) . . ? C8 Fe1 C1 134.23(8) . . ? C5 Fe1 C2 68.01(8) . . ? C4 Fe1 C2 67.93(8) . . ? C8 Fe1 C2 103.74(8) . . ? C1 Fe1 C2 40.31(8) . . ? C5 Fe1 C3 67.95(8) . . ? C4 Fe1 C3 40.16(8) . . ? C8 Fe1 C3 104.22(8) . . ? C1 Fe1 C3 67.67(8) . . ? C2 Fe1 C3 40.29(8) . . ? C5 Fe1 C6 115.02(8) . . ? C4 Fe1 C6 152.80(8) . . ? C8 Fe1 C6 70.99(7) . . ? C1 Fe1 C6 101.25(8) . . ? C2 Fe1 C6 120.79(8) . . ? C3 Fe1 C6 160.08(8) . . ? C5 Fe1 C9 143.69(8) . . ? C4 Fe1 C9 110.09(8) . . ? C8 Fe1 C9 39.99(7) . . ? C1 Fe1 C9 170.01(7) . . ? C2 Fe1 C9 129.70(7) . . ? C3 Fe1 C9 104.33(7) . . ? C6 Fe1 C9 84.54(7) . . ? C5 Fe1 C7 141.98(8) . . ? C4 Fe1 C7 165.87(8) . . ? C8 Fe1 C7 39.54(7) . . ? C1 Fe1 C7 106.99(8) . . ? C2 Fe1 C7 99.52(8) . . ? C3 Fe1 C7 125.84(8) . . ? C6 Fe1 C7 39.37(7) . . ? C9 Fe1 C7 72.33(7) . . ? C5 Fe1 C11 103.71(8) . . ? C4 Fe1 C11 121.80(8) . . ? C8 Fe1 C11 84.88(7) . . ? C1 Fe1 C11 118.57(7) . . ? C2 Fe1 C11 155.39(7) . . ? C3 Fe1 C11 159.92(8) . . ? C6 Fe1 C11 39.88(7) . . ? C9 Fe1 C11 71.04(7) . . ? C7 Fe1 C11 72.32(7) . . ? C5 Fe1 C10 115.58(8) . . ? C4 Fe1 C10 105.02(7) . . ? C8 Fe1 C10 71.74(7) . . ? C1 Fe1 C10 150.51(7) . . ? C2 Fe1 C10 165.54(7) . . ? C3 Fe1 C10 126.40(7) . . ? C6 Fe1 C10 71.44(7) . . ? C9 Fe1 C10 39.15(6) . . ? C7 Fe1 C10 85.67(7) . . ? C11 Fe1 C10 39.07(6) . . ? C5 C1 C2 108.13(18) . . ? C5 C1 Fe1 69.30(11) . . ? C2 C1 Fe1 69.87(11) . . ? C5 C1 H1 125.9 . . ? C2 C1 H1 125.9 . . ? Fe1 C1 H1 125.9 . . ? C3 C2 C1 107.88(18) . . ? C3 C2 Fe1 69.96(11) . . ? C1 C2 Fe1 69.82(11) . . ? C3 C2 H2 126.1 . . ? C1 C2 H2 126.1 . . ? Fe1 C2 H2 126.1 . . ? C4 C3 C2 108.48(18) . . ? C4 C3 Fe1 69.68(11) . . ? C2 C3 Fe1 69.75(11) . . ? C4 C3 H3 125.8 . . ? C2 C3 H3 125.8 . . ? Fe1 C3 H3 125.8 . . ? C3 C4 C5 107.55(18) . . ? C3 C4 Fe1 70.16(11) . . ? C5 C4 Fe1 69.18(12) . . ? C3 C4 H4 126.2 . . ? C5 C4 H4 126.2 . . ? Fe1 C4 H4 126.2 . . ? C1 C5 C4 107.95(18) . . ? C1 C5 Fe1 70.32(12) . . ? C4 C5 Fe1 69.96(11) . . ? C1 C5 H5 126.0 . . ? C4 C5 H5 126.0 . . ? Fe1 C5 H5 126.0 . . ? C7 C6 C11 122.34(16) . . ? C7 C6 Fe1 71.30(10) . . ? C11 C6 Fe1 71.19(10) . . ? C7 C6 H6 118.8 . . ? C11 C6 H6 118.8 . . ? Fe1 C6 H6 131.8 . . ? C8 C7 C6 116.98(16) . . ? C8 C7 C12 121.55(17) . . ? C6 C7 C12 121.31(16) . . ? C8 C7 Fe1 68.51(10) . . ? C6 C7 Fe1 69.33(10) . . ? C12 C7 Fe1 129.64(14) . . ? C7 C8 C9 122.20(16) . . ? C7 C8 Fe1 71.95(11) . . ? C9 C8 Fe1 71.27(10) . . ? C7 C8 H8 118.9 . . ? C9 C8 H8 118.9 . . ? Fe1 C8 H8 130.7 . . ? C8 C9 C10 121.67(15) . . ? C8 C9 C13 115.08(15) . . ? C10 C9 C13 123.25(15) . . ? C8 C9 Fe1 68.74(10) . . ? C10 C9 Fe1 74.52(10) . . ? C13 C9 Fe1 129.44(12) . . ? C9 C10 C11 115.47(15) . . ? C9 C10 B1 120.22(14) . . ? C11 C10 B1 124.29(15) . . ? C9 C10 Fe1 66.33(9) . . ? C11 C10 Fe1 66.97(9) . . ? B1 C10 Fe1 139.46(12) . . ? C6 C11 C10 121.09(16) . . ? C6 C11 C14 114.89(15) . . ? C10 C11 C14 124.01(15) . . ? C6 C11 Fe1 68.92(10) . . ? C10 C11 Fe1 73.96(10) . . ? C14 C11 Fe1 128.76(13) . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C20 115.26(16) . . ? C16 C15 B1 126.61(15) . . ? C20 C15 B1 118.08(15) . . ? C17 C16 C15 121.29(17) . . ? C17 C16 C21 113.41(16) . . ? C15 C16 C21 125.25(16) . . ? C18 C17 C16 122.60(18) . . ? C18 C17 H17 118.7 . . ? C16 C17 H17 118.7 . . ? C19 C18 C17 116.66(17) . . ? C19 C18 C22 121.41(19) . . ? C17 C18 C22 121.93(19) . . ? C18 C19 C20 122.73(18) . . ? C18 C19 H19 118.6 . . ? C20 C19 H19 118.6 . . ? C19 C20 C15 121.29(17) . . ? C19 C20 C23 114.62(16) . . ? C15 C20 C23 123.99(16) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N1 C24 B1 176.71(19) . . ? C30 C25 C26 115.34(16) . . ? C30 C25 B1 123.31(15) . . ? C26 C25 B1 120.77(15) . . ? C27 C26 C25 121.00(18) . . ? C27 C26 C32 115.53(17) . . ? C25 C26 C32 123.47(17) . . ? C28 C27 C26 122.65(19) . . ? C28 C27 H27 118.7 . . ? C26 C27 H27 118.7 . . ? C27 C28 C29 116.43(18) . . ? C27 C28 C33 121.8(2) . . ? C29 C28 C33 121.8(2) . . ? C28 C29 C30 122.06(19) . . ? C28 C29 H29 119.0 . . ? C30 C29 H29 119.0 . . ? C29 C30 C25 121.47(18) . . ? C29 C30 C31 115.91(17) . . ? C25 C30 C31 122.56(17) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C26 C32 H32A 109.5 . . ? C26 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C26 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C24 B1 C25 108.28(14) . . ? C24 B1 C10 104.05(14) . . ? C25 B1 C10 118.68(14) . . ? C24 B1 C15 103.08(13) . . ? C25 B1 C15 107.34(14) . . ? C10 B1 C15 114.09(14) . . ? Cl2 C34 Cl1 110.3(7) . . ? Cl2 C34 Cl3 108.8(7) . . ? Cl1 C34 Cl3 110.9(6) . . ? Cl2 C34 H34A 108.9 . . ? Cl1 C34 H34A 108.9 . . ? Cl3 C34 H34A 108.9 . . ? Cl1' C34' Cl2' 110.1(12) . . ? Cl1' C34' Cl3' 104.5(11) . . ? Cl2' C34' Cl3' 112.8(12) . . ? Cl1' C34' H34B 109.8 . . ? Cl2' C34' H34B 109.8 . . ? Cl3' C34' H34B 109.8 . . ? 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 C4 Fe1 C1 C5 38.25(13) . . . . ? C8 Fe1 C1 C5 170.08(12) . . . . ? C2 Fe1 C1 C5 119.52(18) . . . . ? C3 Fe1 C1 C5 81.76(13) . . . . ? C6 Fe1 C1 C5 -115.58(13) . . . . ? C9 Fe1 C1 C5 119.6(4) . . . . ? C7 Fe1 C1 C5 -155.81(12) . . . . ? C11 Fe1 C1 C5 -77.07(14) . . . . ? C10 Fe1 C1 C5 -43.5(2) . . . . ? C5 Fe1 C1 C2 -119.52(18) . . . . ? C4 Fe1 C1 C2 -81.27(13) . . . . ? C8 Fe1 C1 C2 50.56(16) . . . . ? C3 Fe1 C1 C2 -37.76(12) . . . . ? C6 Fe1 C1 C2 124.90(12) . . . . ? C9 Fe1 C1 C2 0.1(5) . . . . ? C7 Fe1 C1 C2 84.67(13) . . . . ? C11 Fe1 C1 C2 163.41(11) . . . . ? C10 Fe1 C1 C2 -163.00(14) . . . . ? C5 C1 C2 C3 0.9(2) . . . . ? Fe1 C1 C2 C3 59.85(13) . . . . ? C5 C1 C2 Fe1 -58.93(14) . . . . ? C5 Fe1 C2 C3 -81.40(13) . . . . ? C4 Fe1 C2 C3 -37.15(12) . . . . ? C8 Fe1 C2 C3 95.89(12) . . . . ? C1 Fe1 C2 C3 -118.84(18) . . . . ? C6 Fe1 C2 C3 171.72(11) . . . . ? C9 Fe1 C2 C3 61.19(15) . . . . ? C7 Fe1 C2 C3 136.07(12) . . . . ? C11 Fe1 C2 C3 -155.85(17) . . . . ? C10 Fe1 C2 C3 26.0(4) . . . . ? C5 Fe1 C2 C1 37.44(13) . . . . ? C4 Fe1 C2 C1 81.68(13) . . . . ? C8 Fe1 C2 C1 -145.27(12) . . . . ? C3 Fe1 C2 C1 118.84(18) . . . . ? C6 Fe1 C2 C1 -69.44(14) . . . . ? C9 Fe1 C2 C1 -179.98(12) . . . . ? C7 Fe1 C2 C1 -105.09(13) . . . . ? C11 Fe1 C2 C1 -37.0(2) . . . . ? C10 Fe1 C2 C1 144.8(3) . . . . ? C1 C2 C3 C4 -0.7(2) . . . . ? Fe1 C2 C3 C4 59.10(13) . . . . ? C1 C2 C3 Fe1 -59.77(13) . . . . ? C5 Fe1 C3 C4 -38.25(12) . . . . ? C8 Fe1 C3 C4 145.62(12) . . . . ? C1 Fe1 C3 C4 -82.02(13) . . . . ? C2 Fe1 C3 C4 -119.79(17) . . . . ? C6 Fe1 C3 C4 -141.1(2) . . . . ? C9 Fe1 C3 C4 104.30(12) . . . . ? C7 Fe1 C3 C4 -177.36(11) . . . . ? C11 Fe1 C3 C4 30.4(3) . . . . ? C10 Fe1 C3 C4 68.02(14) . . . . ? C5 Fe1 C3 C2 81.54(13) . . . . ? C4 Fe1 C3 C2 119.79(17) . . . . ? C8 Fe1 C3 C2 -94.59(12) . . . . ? C1 Fe1 C3 C2 37.78(12) . . . . ? C6 Fe1 C3 C2 -21.3(3) . . . . ? C9 Fe1 C3 C2 -135.91(12) . . . . ? C7 Fe1 C3 C2 -57.56(14) . . . . ? C11 Fe1 C3 C2 150.24(19) . . . . ? C10 Fe1 C3 C2 -172.19(11) . . . . ? C2 C3 C4 C5 0.2(2) . . . . ? Fe1 C3 C4 C5 59.30(13) . . . . ? C2 C3 C4 Fe1 -59.15(13) . . . . ? C5 Fe1 C4 C3 118.70(17) . . . . ? C8 Fe1 C4 C3 -50.40(16) . . . . ? C1 Fe1 C4 C3 80.89(12) . . . . ? C2 Fe1 C4 C3 37.27(11) . . . . ? C6 Fe1 C4 C3 152.07(15) . . . . ? C9 Fe1 C4 C3 -88.58(12) . . . . ? C7 Fe1 C4 C3 8.8(4) . . . . ? C11 Fe1 C4 C3 -168.19(11) . . . . ? C10 Fe1 C4 C3 -129.40(11) . . . . ? C8 Fe1 C4 C5 -169.09(12) . . . . ? C1 Fe1 C4 C5 -37.80(12) . . . . ? C2 Fe1 C4 C5 -81.43(13) . . . . ? C3 Fe1 C4 C5 -118.70(17) . . . . ? C6 Fe1 C4 C5 33.4(2) . . . . ? C9 Fe1 C4 C5 152.72(12) . . . . ? C7 Fe1 C4 C5 -109.9(3) . . . . ? C11 Fe1 C4 C5 73.11(13) . . . . ? C10 Fe1 C4 C5 111.91(12) . . . . ? C2 C1 C5 C4 -0.8(2) . . . . ? Fe1 C1 C5 C4 -60.11(13) . . . . ? C2 C1 C5 Fe1 59.28(14) . . . . ? C3 C4 C5 C1 0.4(2) . . . . ? Fe1 C4 C5 C1 60.33(14) . . . . ? C3 C4 C5 Fe1 -59.92(13) . . . . ? C4 Fe1 C5 C1 -118.61(17) . . . . ? C8 Fe1 C5 C1 -55.2(6) . . . . ? C2 Fe1 C5 C1 -37.38(12) . . . . ? C3 Fe1 C5 C1 -80.99(13) . . . . ? C6 Fe1 C5 C1 77.50(13) . . . . ? C9 Fe1 C5 C1 -165.25(12) . . . . ? C7 Fe1 C5 C1 39.50(18) . . . . ? C11 Fe1 C5 C1 118.23(12) . . . . ? C10 Fe1 C5 C1 157.94(11) . . . . ? C8 Fe1 C5 C4 63.4(6) . . . . ? C1 Fe1 C5 C4 118.61(17) . . . . ? C2 Fe1 C5 C4 81.23(13) . . . . ? C3 Fe1 C5 C4 37.62(12) . . . . ? C6 Fe1 C5 C4 -163.89(11) . . . . ? C9 Fe1 C5 C4 -46.64(18) . . . . ? C7 Fe1 C5 C4 158.11(12) . . . . ? C11 Fe1 C5 C4 -123.16(12) . . . . ? C10 Fe1 C5 C4 -83.45(13) . . . . ? C5 Fe1 C6 C7 -143.29(11) . . . . ? C4 Fe1 C6 C7 -166.69(15) . . . . ? C8 Fe1 C6 C7 30.00(10) . . . . ? C1 Fe1 C6 C7 -103.14(11) . . . . ? C2 Fe1 C6 C7 -65.00(13) . . . . ? C3 Fe1 C6 C7 -49.1(3) . . . . ? C9 Fe1 C6 C7 68.64(11) . . . . ? C11 Fe1 C6 C7 135.38(15) . . . . ? C10 Fe1 C6 C7 106.48(11) . . . . ? C5 Fe1 C6 C11 81.33(12) . . . . ? C4 Fe1 C6 C11 57.9(2) . . . . ? C8 Fe1 C6 C11 -105.38(11) . . . . ? C1 Fe1 C6 C11 121.48(11) . . . . ? C2 Fe1 C6 C11 159.62(10) . . . . ? C3 Fe1 C6 C11 175.5(2) . . . . ? C9 Fe1 C6 C11 -66.75(11) . . . . ? C7 Fe1 C6 C11 -135.38(15) . . . . ? C10 Fe1 C6 C11 -28.91(10) . . . . ? C11 C6 C7 C8 1.1(3) . . . . ? Fe1 C6 C7 C8 -50.84(15) . . . . ? C11 C6 C7 C12 176.55(17) . . . . ? Fe1 C6 C7 C12 124.65(18) . . . . ? C11 C6 C7 Fe1 51.90(16) . . . . ? C5 Fe1 C7 C8 -166.39(12) . . . . ? C4 Fe1 C7 C8 -73.5(3) . . . . ? C1 Fe1 C7 C8 -140.86(11) . . . . ? C2 Fe1 C7 C8 -100.09(11) . . . . ? C3 Fe1 C7 C8 -66.49(13) . . . . ? C6 Fe1 C7 C8 132.04(15) . . . . ? C9 Fe1 C7 C8 28.69(10) . . . . ? C11 Fe1 C7 C8 103.84(11) . . . . ? C10 Fe1 C7 C8 66.31(11) . . . . ? C5 Fe1 C7 C6 61.57(16) . . . . ? C4 Fe1 C7 C6 154.5(3) . . . . ? C8 Fe1 C7 C6 -132.04(15) . . . . ? C1 Fe1 C7 C6 87.09(11) . . . . ? C2 Fe1 C7 C6 127.87(11) . . . . ? C3 Fe1 C7 C6 161.47(11) . . . . ? C9 Fe1 C7 C6 -103.35(11) . . . . ? C11 Fe1 C7 C6 -28.21(10) . . . . ? C10 Fe1 C7 C6 -65.74(11) . . . . ? C5 Fe1 C7 C12 -52.6(2) . . . . ? C4 Fe1 C7 C12 40.4(4) . . . . ? C8 Fe1 C7 C12 113.8(2) . . . . ? C1 Fe1 C7 C12 -27.03(19) . . . . ? C2 Fe1 C7 C12 13.74(18) . . . . ? C3 Fe1 C7 C12 47.3(2) . . . . ? C6 Fe1 C7 C12 -114.1(2) . . . . ? C9 Fe1 C7 C12 142.53(18) . . . . ? C11 Fe1 C7 C12 -142.33(18) . . . . ? C10 Fe1 C7 C12 -179.86(18) . . . . ? C6 C7 C8 C9 -1.6(3) . . . . ? C12 C7 C8 C9 -177.07(17) . . . . ? Fe1 C7 C8 C9 -52.82(15) . . . . ? C6 C7 C8 Fe1 51.23(15) . . . . ? C12 C7 C8 Fe1 -124.25(18) . . . . ? C5 Fe1 C8 C7 105.3(5) . . . . ? C4 Fe1 C8 C7 160.76(11) . . . . ? C1 Fe1 C8 C7 57.40(15) . . . . ? C2 Fe1 C8 C7 88.35(11) . . . . ? C3 Fe1 C8 C7 129.92(11) . . . . ? C6 Fe1 C8 C7 -29.88(10) . . . . ? C9 Fe1 C8 C7 -134.61(15) . . . . ? C11 Fe1 C8 C7 -68.25(11) . . . . ? C10 Fe1 C8 C7 -105.95(11) . . . . ? C5 Fe1 C8 C9 -120.1(5) . . . . ? C4 Fe1 C8 C9 -64.62(14) . . . . ? C1 Fe1 C8 C9 -167.99(11) . . . . ? C2 Fe1 C8 C9 -137.03(11) . . . . ? C3 Fe1 C8 C9 -95.46(11) . . . . ? C6 Fe1 C8 C9 104.73(11) . . . . ? C7 Fe1 C8 C9 134.61(15) . . . . ? C11 Fe1 C8 C9 66.36(10) . . . . ? C10 Fe1 C8 C9 28.66(10) . . . . ? C7 C8 C9 C10 -1.7(3) . . . . ? Fe1 C8 C9 C10 -54.79(15) . . . . ? C7 C8 C9 C13 177.91(16) . . . . ? Fe1 C8 C9 C13 124.79(14) . . . . ? C7 C8 C9 Fe1 53.12(16) . . . . ? C5 Fe1 C9 C8 167.31(13) . . . . ? C4 Fe1 C9 C8 136.88(11) . . . . ? C1 Fe1 C9 C8 59.3(5) . . . . ? C2 Fe1 C9 C8 59.37(14) . . . . ? C3 Fe1 C9 C8 95.16(11) . . . . ? C6 Fe1 C9 C8 -66.71(11) . . . . ? C7 Fe1 C9 C8 -28.40(10) . . . . ? C11 Fe1 C9 C8 -105.24(11) . . . . ? C10 Fe1 C9 C8 -133.82(15) . . . . ? C5 Fe1 C9 C10 -58.88(16) . . . . ? C4 Fe1 C9 C10 -89.31(11) . . . . ? C8 Fe1 C9 C10 133.82(15) . . . . ? C1 Fe1 C9 C10 -166.9(4) . . . . ? C2 Fe1 C9 C10 -166.81(11) . . . . ? C3 Fe1 C9 C10 -131.02(11) . . . . ? C6 Fe1 C9 C10 67.10(10) . . . . ? C7 Fe1 C9 C10 105.42(11) . . . . ? C11 Fe1 C9 C10 28.57(10) . . . . ? C5 Fe1 C9 C13 61.7(2) . . . . ? C4 Fe1 C9 C13 31.28(18) . . . . ? C8 Fe1 C9 C13 -105.60(19) . . . . ? C1 Fe1 C9 C13 -46.3(5) . . . . ? C2 Fe1 C9 C13 -46.23(19) . . . . ? C3 Fe1 C9 C13 -10.44(17) . . . . ? C6 Fe1 C9 C13 -172.31(16) . . . . ? C7 Fe1 C9 C13 -134.00(17) . . . . ? C11 Fe1 C9 C13 149.16(17) . . . . ? C10 Fe1 C9 C13 120.59(19) . . . . ? C8 C9 C10 C11 5.2(2) . . . . ? C13 C9 C10 C11 -174.36(16) . . . . ? Fe1 C9 C10 C11 -47.01(13) . . . . ? C8 C9 C10 B1 -172.98(15) . . . . ? C13 C9 C10 B1 7.5(2) . . . . ? Fe1 C9 C10 B1 134.83(14) . . . . ? C8 C9 C10 Fe1 52.19(15) . . . . ? C13 C9 C10 Fe1 -127.35(17) . . . . ? C5 Fe1 C10 C9 145.81(11) . . . . ? C4 Fe1 C10 C9 103.51(11) . . . . ? C8 Fe1 C10 C9 -29.23(10) . . . . ? C1 Fe1 C10 C9 175.42(15) . . . . ? C2 Fe1 C10 C9 44.7(3) . . . . ? C3 Fe1 C10 C9 65.25(13) . . . . ? C6 Fe1 C10 C9 -104.68(11) . . . . ? C7 Fe1 C10 C9 -67.10(10) . . . . ? C11 Fe1 C10 C9 -134.14(15) . . . . ? C5 Fe1 C10 C11 -80.05(12) . . . . ? C4 Fe1 C10 C11 -122.35(11) . . . . ? C8 Fe1 C10 C11 104.91(11) . . . . ? C1 Fe1 C10 C11 -50.44(19) . . . . ? C2 Fe1 C10 C11 178.8(3) . . . . ? C3 Fe1 C10 C11 -160.60(11) . . . . ? C6 Fe1 C10 C11 29.46(10) . . . . ? C9 Fe1 C10 C11 134.14(15) . . . . ? C7 Fe1 C10 C11 67.05(11) . . . . ? C5 Fe1 C10 B1 36.4(2) . . . . ? C4 Fe1 C10 B1 -5.94(19) . . . . ? C8 Fe1 C10 B1 -138.68(19) . . . . ? C1 Fe1 C10 B1 66.0(2) . . . . ? C2 Fe1 C10 B1 -64.8(4) . . . . ? C3 Fe1 C10 B1 -44.2(2) . . . . ? C6 Fe1 C10 B1 145.86(19) . . . . ? C9 Fe1 C10 B1 -109.5(2) . . . . ? C7 Fe1 C10 B1 -176.55(18) . . . . ? C11 Fe1 C10 B1 116.4(2) . . . . ? C7 C6 C11 C10 2.7(3) . . . . ? Fe1 C6 C11 C10 54.68(15) . . . . ? C7 C6 C11 C14 -176.06(17) . . . . ? Fe1 C6 C11 C14 -124.11(15) . . . . ? C7 C6 C11 Fe1 -51.94(16) . . . . ? C9 C10 C11 C6 -5.7(2) . . . . ? B1 C10 C11 C6 172.41(16) . . . . ? Fe1 C10 C11 C6 -52.39(15) . . . . ? C9 C10 C11 C14 173.01(16) . . . . ? B1 C10 C11 C14 -8.9(3) . . . . ? Fe1 C10 C11 C14 126.29(18) . . . . ? C9 C10 C11 Fe1 46.72(13) . . . . ? B1 C10 C11 Fe1 -135.20(15) . . . . ? C5 Fe1 C11 C6 -112.77(12) . . . . ? C4 Fe1 C11 C6 -152.89(11) . . . . ? C8 Fe1 C11 C6 66.24(11) . . . . ? C1 Fe1 C11 C6 -72.24(13) . . . . ? C2 Fe1 C11 C6 -45.9(2) . . . . ? C3 Fe1 C11 C6 -175.5(2) . . . . ? C9 Fe1 C11 C6 104.74(11) . . . . ? C7 Fe1 C11 C6 27.88(10) . . . . ? C10 Fe1 C11 C6 133.36(15) . . . . ? C5 Fe1 C11 C10 113.87(11) . . . . ? C4 Fe1 C11 C10 73.75(12) . . . . ? C8 Fe1 C11 C10 -67.12(10) . . . . ? C1 Fe1 C11 C10 154.40(11) . . . . ? C2 Fe1 C11 C10 -179.28(17) . . . . ? C3 Fe1 C11 C10 51.1(2) . . . . ? C6 Fe1 C11 C10 -133.36(15) . . . . ? C9 Fe1 C11 C10 -28.62(10) . . . . ? C7 Fe1 C11 C10 -105.48(11) . . . . ? C5 Fe1 C11 C14 -7.17(17) . . . . ? C4 Fe1 C11 C14 -47.29(18) . . . . ? C8 Fe1 C11 C14 171.84(16) . . . . ? C1 Fe1 C11 C14 33.36(18) . . . . ? C2 Fe1 C11 C14 59.7(3) . . . . ? C3 Fe1 C11 C14 -69.9(3) . . . . ? C6 Fe1 C11 C14 105.60(19) . . . . ? C9 Fe1 C11 C14 -149.66(17) . . . . ? C7 Fe1 C11 C14 133.48(17) . . . . ? C10 Fe1 C11 C14 -121.0(2) . . . . ? C20 C15 C16 C17 4.0(2) . . . . ? B1 C15 C16 C17 -178.47(16) . . . . ? C20 C15 C16 C21 -173.05(17) . . . . ? B1 C15 C16 C21 4.4(3) . . . . ? C15 C16 C17 C18 -1.7(3) . . . . ? C21 C16 C17 C18 175.73(17) . . . . ? C16 C17 C18 C19 -2.0(3) . . . . ? C16 C17 C18 C22 178.40(18) . . . . ? C17 C18 C19 C20 3.2(3) . . . . ? C22 C18 C19 C20 -177.24(18) . . . . ? C18 C19 C20 C15 -0.7(3) . . . . ? C18 C19 C20 C23 -177.25(17) . . . . ? C16 C15 C20 C19 -2.9(2) . . . . ? B1 C15 C20 C19 179.36(15) . . . . ? C16 C15 C20 C23 173.32(16) . . . . ? B1 C15 C20 C23 -4.4(2) . . . . ? C30 C25 C26 C27 9.2(3) . . . . ? B1 C25 C26 C27 -162.32(16) . . . . ? C30 C25 C26 C32 -169.76(17) . . . . ? B1 C25 C26 C32 18.7(3) . . . . ? C25 C26 C27 C28 -0.9(3) . . . . ? C32 C26 C27 C28 178.17(19) . . . . ? C26 C27 C28 C29 -6.4(3) . . . . ? C26 C27 C28 C33 175.1(2) . . . . ? C27 C28 C29 C30 5.1(3) . . . . ? C33 C28 C29 C30 -176.4(2) . . . . ? C28 C29 C30 C25 3.6(3) . . . . ? C28 C29 C30 C31 -173.6(2) . . . . ? C26 C25 C30 C29 -10.5(3) . . . . ? B1 C25 C30 C29 160.77(17) . . . . ? C26 C25 C30 C31 166.44(17) . . . . ? B1 C25 C30 C31 -22.2(3) . . . . ? N1 C24 B1 C25 -163(3) . . . . ? N1 C24 B1 C10 70(3) . . . . ? N1 C24 B1 C15 -50(3) . . . . ? C30 C25 B1 C24 -23.9(2) . . . . ? C26 C25 B1 C24 146.97(16) . . . . ? C30 C25 B1 C10 94.3(2) . . . . ? C26 C25 B1 C10 -94.9(2) . . . . ? C30 C25 B1 C15 -134.54(17) . . . . ? C26 C25 B1 C15 36.3(2) . . . . ? C9 C10 B1 C24 -52.05(19) . . . . ? C11 C10 B1 C24 129.95(17) . . . . ? Fe1 C10 B1 C24 36.0(2) . . . . ? C9 C10 B1 C25 -172.41(15) . . . . ? C11 C10 B1 C25 9.6(2) . . . . ? Fe1 C10 B1 C25 -84.3(2) . . . . ? C9 C10 B1 C15 59.5(2) . . . . ? C11 C10 B1 C15 -118.49(18) . . . . ? Fe1 C10 B1 C15 147.57(14) . . . . ? C16 C15 B1 C24 124.55(18) . . . . ? C20 C15 B1 C24 -58.03(19) . . . . ? C16 C15 B1 C25 -121.25(18) . . . . ? C20 C15 B1 C25 56.17(19) . . . . ? C16 C15 B1 C10 12.4(2) . . . . ? C20 C15 B1 C10 -170.17(14) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.401 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.064