Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Gerhard Erker' _publ_contact_author_address ; Organisch-Chemisches Institut Universitaet Muenster Corrensstrasse 40 Muenster 48149 GERMANY ; _publ_contact_author_email ERKER@UNI-MUENSTER.DE _publ_section_title ; Development of a Convenient New Synthetic Route to [3]Ferrocenophanones ; loop_ _publ_author_name 'G. Erker' 'Roland Frohlich' 'Gerald Kehr' 'Serena Losi' 'Markus Neumann' 'Ludger Tebben' 'Piero Zanello' # Attachment 'ERK2718.CIF' data_erk2718 _database_code_depnum_ccdc_archive 'CCDC 287243' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H14 Fe O' _chemical_formula_weight 254.10 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 5.740(1) _cell_length_b 13.703(1) _cell_length_c 13.774(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1083.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used 9884 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 1.363 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6852 _exptl_absorpt_correction_T_max 0.8216 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8802 _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 27.86 _reflns_number_total 2581 _reflns_number_gt 2400 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Shedlrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0208P)^2^+0.3261P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.011(16) _refine_ls_number_reflns 2581 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0296 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_ref 0.0543 _refine_ls_wR_factor_gt 0.0525 _refine_ls_goodness_of_fit_ref 1.036 _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 Fe Fe 0.16123(4) 0.988227(16) 0.465012(18) 0.01888(7) Uani 1 1 d . . . C1 C 0.1888(3) 0.85247(12) 0.40582(14) 0.0197(4) Uani 1 1 d . . . C2 C 0.4124(3) 0.88748(13) 0.43478(14) 0.0204(4) Uani 1 1 d . . . H2 H 0.5428 0.8965 0.3932 0.024 Uiso 1 1 calc R . . C3 C 0.4074(3) 0.90673(12) 0.53671(16) 0.0239(4) Uani 1 1 d . . . H3 H 0.5328 0.9310 0.5747 0.029 Uiso 1 1 calc R . . C4 C 0.1808(4) 0.88301(13) 0.57109(14) 0.0266(4) Uani 1 1 d . . . H4 H 0.1276 0.8891 0.6361 0.032 Uiso 1 1 calc R . . C5 C 0.0483(4) 0.84868(13) 0.49127(15) 0.0244(4) Uani 1 1 d . . . H5 H -0.1085 0.8267 0.4942 0.029 Uiso 1 1 calc R . . C6 C 0.1148(3) 0.82877(13) 0.30300(15) 0.0245(4) Uani 1 1 d . . . H6 H -0.0459 0.8007 0.3054 0.029 Uiso 1 1 calc R . . C7 C 0.2767(4) 0.75233(15) 0.25827(17) 0.0359(5) Uani 1 1 d . . . H7A H 0.4362 0.7778 0.2566 0.054 Uiso 1 1 calc R . . H7B H 0.2252 0.7376 0.1920 0.054 Uiso 1 1 calc R . . H7C H 0.2723 0.6927 0.2975 0.054 Uiso 1 1 calc R . . C8 C 0.1087(3) 0.92038(14) 0.23718(14) 0.0268(4) Uani 1 1 d . . . H8A H 0.2648 0.9511 0.2355 0.032 Uiso 1 1 calc R . . H8B H 0.0666 0.9013 0.1701 0.032 Uiso 1 1 calc R . . C9 C -0.0682(3) 0.99258(15) 0.27595(13) 0.0240(4) Uani 1 1 d . . . O1 O -0.2710(2) 0.98982(13) 0.24867(10) 0.0345(3) Uani 1 1 d . . . C10 C 0.0051(3) 1.05812(13) 0.35502(15) 0.0232(4) Uani 1 1 d . . . C11 C 0.2344(4) 1.09727(13) 0.37183(15) 0.0252(4) Uani 1 1 d . . . H11 H 0.3602 1.0976 0.3270 0.030 Uiso 1 1 calc R . . C12 C 0.2383(3) 1.13550(13) 0.46809(18) 0.0291(4) Uani 1 1 d . . . H12 H 0.3672 1.1666 0.4983 0.035 Uiso 1 1 calc R . . C13 C 0.0162(4) 1.11917(13) 0.51121(17) 0.0284(5) Uani 1 1 d . . . H13 H -0.0274 1.1363 0.5755 0.034 Uiso 1 1 calc R . . C14 C -0.1280(3) 1.07315(12) 0.44207(14) 0.0251(4) Uani 1 1 d . . . H14 H -0.2862 1.0552 0.4515 0.030 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 Fe 0.01979(12) 0.01590(11) 0.02096(13) 0.00222(10) -0.00018(11) 0.00025(10) C1 0.0230(9) 0.0119(7) 0.0242(10) 0.0014(7) -0.0005(9) 0.0013(8) C2 0.0190(9) 0.0179(8) 0.0242(10) 0.0017(7) -0.0015(7) 0.0033(7) C3 0.0273(9) 0.0204(8) 0.0239(10) 0.0015(9) -0.0066(9) 0.0044(7) C4 0.0362(11) 0.0228(9) 0.0208(10) 0.0073(7) 0.0024(9) 0.0017(9) C5 0.0274(10) 0.0163(8) 0.0296(12) 0.0050(7) 0.0029(8) -0.0031(8) C6 0.0263(11) 0.0204(8) 0.0269(10) -0.0004(8) -0.0039(8) -0.0033(7) C7 0.0477(13) 0.0269(10) 0.0330(12) -0.0097(9) -0.0042(10) 0.0038(10) C8 0.0323(11) 0.0280(10) 0.0203(10) 0.0015(8) -0.0001(8) 0.0004(8) C9 0.0270(9) 0.0247(10) 0.0204(9) 0.0093(9) -0.0024(7) -0.0003(9) O1 0.0282(7) 0.0440(9) 0.0313(7) 0.0030(8) -0.0071(6) 0.0015(7) C10 0.0237(9) 0.0189(9) 0.0270(11) 0.0058(8) -0.0034(8) 0.0033(8) C11 0.0274(10) 0.0186(9) 0.0297(11) 0.0088(8) -0.0003(8) -0.0025(8) C12 0.0330(10) 0.0149(8) 0.0395(12) 0.0004(10) -0.0067(10) -0.0014(7) C13 0.0332(11) 0.0178(9) 0.0342(13) -0.0048(8) -0.0008(9) 0.0074(8) C14 0.0233(10) 0.0210(8) 0.0310(11) 0.0020(7) 0.0009(8) 0.0057(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 Fe C10 2.0040(19) . ? Fe C11 2.0140(19) . ? Fe C1 2.0373(17) . ? Fe C2 2.0390(18) . ? Fe C5 2.0512(18) . ? Fe C14 2.0519(18) . ? Fe C3 2.0539(18) . ? Fe C4 2.0558(18) . ? Fe C12 2.0664(18) . ? Fe C13 2.0779(19) . ? C1 C2 1.427(3) . ? C1 C5 1.428(3) . ? C1 C6 1.514(3) . ? C2 C3 1.429(3) . ? C3 C4 1.422(3) . ? C4 C5 1.417(3) . ? C6 C7 1.530(3) . ? C6 C8 1.549(3) . ? C8 C9 1.515(3) . ? C9 O1 1.224(2) . ? C9 C10 1.473(3) . ? C10 C14 1.436(3) . ? C10 C11 1.440(3) . ? C11 C12 1.426(3) . ? C12 C13 1.424(3) . ? C13 C14 1.411(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 Fe C11 42.02(8) . . ? C10 Fe C1 99.70(8) . . ? C11 Fe C1 113.97(8) . . ? C10 Fe C2 119.04(8) . . ? C11 Fe C2 102.98(8) . . ? C1 Fe C2 40.99(8) . . ? C10 Fe C5 115.94(8) . . ? C11 Fe C5 150.45(8) . . ? C1 Fe C5 40.87(8) . . ? C2 Fe C5 68.18(8) . . ? C10 Fe C14 41.46(8) . . ? C11 Fe C14 69.51(8) . . ? C1 Fe C14 121.27(8) . . ? C2 Fe C14 157.60(8) . . ? C5 Fe C14 107.47(8) . . ? C10 Fe C3 158.60(8) . . ? C11 Fe C3 124.49(8) . . ? C1 Fe C3 69.05(8) . . ? C2 Fe C3 40.86(8) . . ? C5 Fe C3 68.02(8) . . ? C14 Fe C3 159.88(8) . . ? C10 Fe C4 153.76(8) . . ? C11 Fe C4 164.11(9) . . ? C1 Fe C4 68.89(8) . . ? C2 Fe C4 68.39(8) . . ? C5 Fe C4 40.37(8) . . ? C14 Fe C4 123.47(8) . . ? C3 Fe C4 40.48(8) . . ? C10 Fe C12 69.18(8) . . ? C11 Fe C12 40.88(9) . . ? C1 Fe C12 152.05(9) . . ? C2 Fe C12 120.94(8) . . ? C5 Fe C12 167.02(9) . . ? C14 Fe C12 67.82(7) . . ? C3 Fe C12 111.96(8) . . ? C4 Fe C12 131.19(9) . . ? C10 Fe C13 68.88(8) . . ? C11 Fe C13 68.78(9) . . ? C1 Fe C13 160.42(8) . . ? C2 Fe C13 158.51(8) . . ? C5 Fe C13 128.64(9) . . ? C14 Fe C13 39.94(8) . . ? C3 Fe C13 126.72(8) . . ? C4 Fe C13 114.20(8) . . ? C12 Fe C13 40.19(8) . . ? C2 C1 C5 106.84(17) . . ? C2 C1 C6 125.87(18) . . ? C5 C1 C6 127.23(17) . . ? C2 C1 Fe 69.57(9) . . ? C5 C1 Fe 70.09(10) . . ? C6 C1 Fe 123.26(12) . . ? C1 C2 C3 108.57(17) . . ? C1 C2 Fe 69.44(10) . . ? C3 C2 Fe 70.13(10) . . ? C4 C3 C2 107.68(17) . . ? C4 C3 Fe 69.84(10) . . ? C2 C3 Fe 69.01(11) . . ? C5 C4 C3 107.96(18) . . ? C5 C4 Fe 69.64(11) . . ? C3 C4 Fe 69.69(10) . . ? C4 C5 C1 108.93(17) . . ? C4 C5 Fe 69.99(10) . . ? C1 C5 Fe 69.04(10) . . ? C1 C6 C7 110.68(17) . . ? C1 C6 C8 112.33(15) . . ? C7 C6 C8 109.44(17) . . ? C9 C8 C6 109.75(16) . . ? O1 C9 C10 121.17(19) . . ? O1 C9 C8 120.6(2) . . ? C10 C9 C8 117.86(16) . . ? C14 C10 C11 107.36(17) . . ? C14 C10 C9 123.56(16) . . ? C11 C10 C9 127.37(18) . . ? C14 C10 Fe 71.06(11) . . ? C11 C10 Fe 69.37(11) . . ? C9 C10 Fe 113.29(12) . . ? C12 C11 C10 107.49(18) . . ? C12 C11 Fe 71.53(11) . . ? C10 C11 Fe 68.62(11) . . ? C13 C12 C11 108.43(18) . . ? C13 C12 Fe 70.34(11) . . ? C11 C12 Fe 67.59(10) . . ? C14 C13 C12 108.29(18) . . ? C14 C13 Fe 69.04(11) . . ? C12 C13 Fe 69.47(11) . . ? C13 C14 C10 108.40(17) . . ? C13 C14 Fe 71.03(11) . . ? C10 C14 Fe 67.48(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 Fe C1 C2 123.65(12) . . . . ? C11 Fe C1 C2 82.14(12) . . . . ? C5 Fe C1 C2 -117.63(16) . . . . ? C14 Fe C1 C2 161.87(11) . . . . ? C3 Fe C1 C2 -37.43(12) . . . . ? C4 Fe C1 C2 -80.93(12) . . . . ? C12 Fe C1 C2 60.2(2) . . . . ? C13 Fe C1 C2 176.0(2) . . . . ? C10 Fe C1 C5 -118.72(12) . . . . ? C11 Fe C1 C5 -160.23(12) . . . . ? C2 Fe C1 C5 117.63(16) . . . . ? C14 Fe C1 C5 -80.50(13) . . . . ? C3 Fe C1 C5 80.20(12) . . . . ? C4 Fe C1 C5 36.70(12) . . . . ? C12 Fe C1 C5 177.83(17) . . . . ? C13 Fe C1 C5 -66.3(3) . . . . ? C10 Fe C1 C6 3.41(17) . . . . ? C11 Fe C1 C6 -38.09(18) . . . . ? C2 Fe C1 C6 -120.2(2) . . . . ? C5 Fe C1 C6 122.1(2) . . . . ? C14 Fe C1 C6 41.64(19) . . . . ? C3 Fe C1 C6 -157.66(18) . . . . ? C4 Fe C1 C6 158.84(19) . . . . ? C12 Fe C1 C6 -60.0(3) . . . . ? C13 Fe C1 C6 55.8(3) . . . . ? C5 C1 C2 C3 -1.10(19) . . . . ? C6 C1 C2 C3 176.33(16) . . . . ? Fe C1 C2 C3 59.40(12) . . . . ? C5 C1 C2 Fe -60.50(12) . . . . ? C6 C1 C2 Fe 116.93(16) . . . . ? C10 Fe C2 C1 -69.81(13) . . . . ? C11 Fe C2 C1 -111.73(12) . . . . ? C5 Fe C2 C1 38.65(11) . . . . ? C14 Fe C2 C1 -44.3(2) . . . . ? C3 Fe C2 C1 119.82(16) . . . . ? C4 Fe C2 C1 82.26(12) . . . . ? C12 Fe C2 C1 -151.70(12) . . . . ? C13 Fe C2 C1 -176.4(2) . . . . ? C10 Fe C2 C3 170.36(11) . . . . ? C11 Fe C2 C3 128.44(11) . . . . ? C1 Fe C2 C3 -119.82(16) . . . . ? C5 Fe C2 C3 -81.18(12) . . . . ? C14 Fe C2 C3 -164.11(18) . . . . ? C4 Fe C2 C3 -37.57(11) . . . . ? C12 Fe C2 C3 88.48(14) . . . . ? C13 Fe C2 C3 63.8(3) . . . . ? C1 C2 C3 C4 0.4(2) . . . . ? Fe C2 C3 C4 59.35(12) . . . . ? C1 C2 C3 Fe -58.97(12) . . . . ? C10 Fe C3 C4 -142.8(2) . . . . ? C11 Fe C3 C4 173.02(12) . . . . ? C1 Fe C3 C4 -81.63(13) . . . . ? C2 Fe C3 C4 -119.16(16) . . . . ? C5 Fe C3 C4 -37.57(12) . . . . ? C14 Fe C3 C4 43.2(3) . . . . ? C12 Fe C3 C4 128.43(12) . . . . ? C13 Fe C3 C4 85.04(14) . . . . ? C10 Fe C3 C2 -23.6(3) . . . . ? C11 Fe C3 C2 -67.81(13) . . . . ? C1 Fe C3 C2 37.54(11) . . . . ? C5 Fe C3 C2 81.60(12) . . . . ? C14 Fe C3 C2 162.34(19) . . . . ? C4 Fe C3 C2 119.16(16) . . . . ? C12 Fe C3 C2 -112.41(12) . . . . ? C13 Fe C3 C2 -155.79(12) . . . . ? C2 C3 C4 C5 0.5(2) . . . . ? Fe C3 C4 C5 59.34(13) . . . . ? C2 C3 C4 Fe -58.84(13) . . . . ? C10 Fe C4 C5 30.9(2) . . . . ? C11 Fe C4 C5 -140.7(3) . . . . ? C1 Fe C4 C5 -37.13(12) . . . . ? C2 Fe C4 C5 -81.30(13) . . . . ? C14 Fe C4 C5 77.18(14) . . . . ? C3 Fe C4 C5 -119.21(17) . . . . ? C12 Fe C4 C5 165.87(12) . . . . ? C13 Fe C4 C5 121.89(12) . . . . ? C10 Fe C4 C3 150.08(17) . . . . ? C11 Fe C4 C3 -21.5(4) . . . . ? C1 Fe C4 C3 82.08(13) . . . . ? C2 Fe C4 C3 37.92(12) . . . . ? C5 Fe C4 C3 119.21(17) . . . . ? C14 Fe C4 C3 -163.61(11) . . . . ? C12 Fe C4 C3 -74.92(15) . . . . ? C13 Fe C4 C3 -118.90(13) . . . . ? C3 C4 C5 C1 -1.2(2) . . . . ? Fe C4 C5 C1 58.17(12) . . . . ? C3 C4 C5 Fe -59.37(12) . . . . ? C2 C1 C5 C4 1.41(19) . . . . ? C6 C1 C5 C4 -175.97(16) . . . . ? Fe C1 C5 C4 -58.75(13) . . . . ? C2 C1 C5 Fe 60.16(11) . . . . ? C6 C1 C5 Fe -117.22(17) . . . . ? C10 Fe C5 C4 -165.39(12) . . . . ? C11 Fe C5 C4 159.41(16) . . . . ? C1 Fe C5 C4 120.61(17) . . . . ? C2 Fe C5 C4 81.86(13) . . . . ? C14 Fe C5 C4 -121.49(13) . . . . ? C3 Fe C5 C4 37.66(12) . . . . ? C12 Fe C5 C4 -54.9(4) . . . . ? C13 Fe C5 C4 -82.52(14) . . . . ? C10 Fe C5 C1 74.00(13) . . . . ? C11 Fe C5 C1 38.8(2) . . . . ? C2 Fe C5 C1 -38.75(11) . . . . ? C14 Fe C5 C1 117.90(12) . . . . ? C3 Fe C5 C1 -82.95(12) . . . . ? C4 Fe C5 C1 -120.61(17) . . . . ? C12 Fe C5 C1 -175.5(3) . . . . ? C13 Fe C5 C1 156.86(12) . . . . ? C2 C1 C6 C7 57.2(2) . . . . ? C5 C1 C6 C7 -125.9(2) . . . . ? Fe C1 C6 C7 144.87(15) . . . . ? C2 C1 C6 C8 -65.5(2) . . . . ? C5 C1 C6 C8 111.46(19) . . . . ? Fe C1 C6 C8 22.2(2) . . . . ? C1 C6 C8 C9 -61.9(2) . . . . ? C7 C6 C8 C9 174.74(16) . . . . ? C6 C8 C9 O1 -90.3(2) . . . . ? C6 C8 C9 C10 82.9(2) . . . . ? O1 C9 C10 C14 41.9(3) . . . . ? C8 C9 C10 C14 -131.27(18) . . . . ? O1 C9 C10 C11 -155.0(2) . . . . ? C8 C9 C10 C11 31.9(3) . . . . ? O1 C9 C10 Fe 123.89(18) . . . . ? C8 C9 C10 Fe -49.2(2) . . . . ? C11 Fe C10 C14 -117.80(15) . . . . ? C1 Fe C10 C14 126.99(11) . . . . ? C2 Fe C10 C14 165.64(10) . . . . ? C5 Fe C10 C14 87.34(12) . . . . ? C3 Fe C10 C14 -176.89(18) . . . . ? C4 Fe C10 C14 65.7(2) . . . . ? C12 Fe C10 C14 -79.66(12) . . . . ? C13 Fe C10 C14 -36.47(11) . . . . ? C1 Fe C10 C11 -115.21(12) . . . . ? C2 Fe C10 C11 -76.56(13) . . . . ? C5 Fe C10 C11 -154.86(12) . . . . ? C14 Fe C10 C11 117.80(15) . . . . ? C3 Fe C10 C11 -59.1(2) . . . . ? C4 Fe C10 C11 -176.55(17) . . . . ? C12 Fe C10 C11 38.15(12) . . . . ? C13 Fe C10 C11 81.33(13) . . . . ? C11 Fe C10 C9 123.0(2) . . . . ? C1 Fe C10 C9 7.75(15) . . . . ? C2 Fe C10 C9 46.40(16) . . . . ? C5 Fe C10 C9 -31.91(17) . . . . ? C14 Fe C10 C9 -119.24(18) . . . . ? C3 Fe C10 C9 63.9(3) . . . . ? C4 Fe C10 C9 -53.6(2) . . . . ? C12 Fe C10 C9 161.10(16) . . . . ? C13 Fe C10 C9 -155.72(16) . . . . ? C14 C10 C11 C12 -0.1(2) . . . . ? C9 C10 C11 C12 -165.43(18) . . . . ? Fe C10 C11 C12 -61.31(13) . . . . ? C14 C10 C11 Fe 61.24(12) . . . . ? C9 C10 C11 Fe -104.12(19) . . . . ? C10 Fe C11 C12 118.10(17) . . . . ? C1 Fe C11 C12 -164.48(12) . . . . ? C2 Fe C11 C12 -122.67(12) . . . . ? C5 Fe C11 C12 168.86(15) . . . . ? C14 Fe C11 C12 79.40(12) . . . . ? C3 Fe C11 C12 -84.23(14) . . . . ? C4 Fe C11 C12 -67.5(3) . . . . ? C13 Fe C11 C12 36.53(12) . . . . ? C1 Fe C11 C10 77.42(13) . . . . ? C2 Fe C11 C10 119.23(12) . . . . ? C5 Fe C11 C10 50.8(2) . . . . ? C14 Fe C11 C10 -38.70(11) . . . . ? C3 Fe C11 C10 157.67(11) . . . . ? C4 Fe C11 C10 174.4(3) . . . . ? C12 Fe C11 C10 -118.10(17) . . . . ? C13 Fe C11 C10 -81.57(12) . . . . ? C10 C11 C12 C13 0.9(2) . . . . ? Fe C11 C12 C13 -58.59(13) . . . . ? C10 C11 C12 Fe 59.46(12) . . . . ? C10 Fe C12 C13 81.53(13) . . . . ? C11 Fe C12 C13 120.70(17) . . . . ? C1 Fe C12 C13 152.14(16) . . . . ? C2 Fe C12 C13 -166.29(12) . . . . ? C5 Fe C12 C13 -34.2(4) . . . . ? C14 Fe C12 C13 36.83(12) . . . . ? C3 Fe C12 C13 -121.45(13) . . . . ? C4 Fe C12 C13 -78.93(15) . . . . ? C10 Fe C12 C11 -39.17(12) . . . . ? C1 Fe C12 C11 31.4(2) . . . . ? C2 Fe C12 C11 73.01(14) . . . . ? C5 Fe C12 C11 -154.9(3) . . . . ? C14 Fe C12 C11 -83.87(13) . . . . ? C3 Fe C12 C11 117.85(13) . . . . ? C4 Fe C12 C11 160.37(13) . . . . ? C13 Fe C12 C11 -120.70(17) . . . . ? C11 C12 C13 C14 -1.3(2) . . . . ? Fe C12 C13 C14 -58.25(13) . . . . ? C11 C12 C13 Fe 56.92(13) . . . . ? C10 Fe C13 C14 37.81(12) . . . . ? C11 Fe C13 C14 83.03(13) . . . . ? C1 Fe C13 C14 -19.0(3) . . . . ? C2 Fe C13 C14 153.9(2) . . . . ? C5 Fe C13 C14 -69.14(15) . . . . ? C3 Fe C13 C14 -159.05(12) . . . . ? C4 Fe C13 C14 -113.90(13) . . . . ? C12 Fe C13 C14 120.16(17) . . . . ? C10 Fe C13 C12 -82.35(13) . . . . ? C11 Fe C13 C12 -37.13(13) . . . . ? C1 Fe C13 C12 -139.2(2) . . . . ? C2 Fe C13 C12 33.7(3) . . . . ? C5 Fe C13 C12 170.70(13) . . . . ? C14 Fe C13 C12 -120.16(17) . . . . ? C3 Fe C13 C12 80.79(14) . . . . ? C4 Fe C13 C12 125.94(13) . . . . ? C12 C13 C14 C10 1.3(2) . . . . ? Fe C13 C14 C10 -57.23(12) . . . . ? C12 C13 C14 Fe 58.52(13) . . . . ? C11 C10 C14 C13 -0.7(2) . . . . ? C9 C10 C14 C13 165.30(17) . . . . ? Fe C10 C14 C13 59.41(13) . . . . ? C11 C10 C14 Fe -60.15(12) . . . . ? C9 C10 C14 Fe 105.90(17) . . . . ? C10 Fe C14 C13 -120.26(17) . . . . ? C11 Fe C14 C13 -81.06(13) . . . . ? C1 Fe C14 C13 172.66(12) . . . . ? C2 Fe C14 C13 -154.95(19) . . . . ? C5 Fe C14 C13 130.08(13) . . . . ? C3 Fe C14 C13 56.4(3) . . . . ? C4 Fe C14 C13 88.61(14) . . . . ? C12 Fe C14 C13 -37.06(12) . . . . ? C11 Fe C14 C10 39.20(11) . . . . ? C1 Fe C14 C10 -67.08(13) . . . . ? C2 Fe C14 C10 -34.7(2) . . . . ? C5 Fe C14 C10 -109.66(12) . . . . ? C3 Fe C14 C10 176.7(2) . . . . ? C4 Fe C14 C10 -151.13(11) . . . . ? C12 Fe C14 C10 83.21(13) . . . . ? C13 Fe C14 C10 120.26(17) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.236 _refine_diff_density_min -0.280 _refine_diff_density_rms 0.048