# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Simon Aldridge' 'Natalie R. Bunn' 'Deborah L. Coombs' 'Cameron Jones' 'Li-ling Ooi' 'Andrea Rossin' 'David J. Willock' _publ_contact_author_name 'Dr Simon Aldridge' _publ_contact_author_address ; School of Chemistry Cardiff University PO Box 912 Park Place Cardiff CF10 3TB UNITED KINGDOM ; _publ_contact_author_email ALDRIDGES@CF.AC.UK _publ_requested_journal 'Chemical Communications' _publ_section_title ; Fe-Ga multiple bonding? Synthesis, spectroscopic and structural characterization of a transition metal complex containing a cationic two-coordinate gallium centre ; data_sa0401 _database_code_depnum_ccdc_archive 'CCDC 237193' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common sa0401 _chemical_melting_point ? _chemical_formula_moiety 'C24 H30 Cl Fe2 Ga O4' _chemical_formula_sum ' C24 H30 Cl Fe2 Ga O4' _chemical_formula_weight 599.34 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' 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' Ga Ga 0.2307 1.6083 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P cnb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x, -y+1/2, z' '-x, -y, -z' 'x-1/2, -y, -z-1/2' '-x-1/2, y-1/2, -z-1/2' 'x, y-1/2, -z' _cell_length_a 11.1946(2) _cell_length_b 12.9307(3) _cell_length_c 16.9269(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2450.24(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 29438 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 2.397 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5856 _exptl_absorpt_correction_T_max 0.7458 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29314 _diffrn_reflns_av_R_equivalents 0.1124 _diffrn_reflns_av_sigmaI/netI 0.0535 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.64 _diffrn_reflns_theta_max 30.02 _reflns_number_total 3574 _reflns_number_gt 2889 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'Dirdif-99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0363P)^2^+4.2544P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3574 _refine_ls_number_parameters 151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0678 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1050 _refine_ls_wR_factor_gt 0.0981 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1351(3) 0.0652(2) 0.15629(17) 0.0214(6) Uani 1 1 d . . . C2 C 0.0984(3) 0.1373(3) 0.01400(18) 0.0224(6) Uani 1 1 d . . . C3 C 0.2066(3) 0.4194(2) 0.15421(19) 0.0258(7) Uani 1 1 d . . . H3A H 0.1757 0.4107 0.2080 0.039 Uiso 1 1 calc R . . H3B H 0.1416 0.4415 0.1192 0.039 Uiso 1 1 calc R . . H3C H 0.2697 0.4719 0.1542 0.039 Uiso 1 1 calc R . . C4 C 0.2445(3) 0.3543(3) -0.02660(18) 0.0265(7) Uani 1 1 d . . . H4A H 0.1874 0.4081 -0.0112 0.040 Uiso 1 1 calc R . . H4B H 0.2086 0.3099 -0.0671 0.040 Uiso 1 1 calc R . . H4C H 0.3169 0.3867 -0.0478 0.040 Uiso 1 1 calc R . . C5 C 0.3866(3) 0.1398(3) -0.02914(18) 0.0265(7) Uani 1 1 d . . . H5A H 0.4691 0.1610 -0.0400 0.040 Uiso 1 1 calc R . . H5B H 0.3359 0.1576 -0.0743 0.040 Uiso 1 1 calc R . . H5C H 0.3840 0.0649 -0.0204 0.040 Uiso 1 1 calc R . . C6 C 0.4330(3) 0.0713(3) 0.14897(19) 0.0256(7) Uani 1 1 d . . . H6A H 0.4256 0.0159 0.1097 0.038 Uiso 1 1 calc R . . H6B H 0.4028 0.0469 0.2000 0.038 Uiso 1 1 calc R . . H6C H 0.5172 0.0909 0.1543 0.038 Uiso 1 1 calc R . . C7 C 0.3168(3) 0.2392(3) 0.26252(17) 0.0276(7) Uani 1 1 d . . . H7A H 0.3882 0.2776 0.2785 0.041 Uiso 1 1 calc R . . H7B H 0.3223 0.1679 0.2818 0.041 Uiso 1 1 calc R . . H7C H 0.2458 0.2724 0.2850 0.041 Uiso 1 1 calc R . . C8 C 0.2568(3) 0.3180(2) 0.12524(17) 0.0174(5) Uani 1 1 d . . . C9 C 0.2763(3) 0.2902(2) 0.04442(16) 0.0179(6) Uani 1 1 d . . . C10 C 0.3421(3) 0.1948(2) 0.04336(17) 0.0189(6) Uani 1 1 d . . . C11 C 0.3619(3) 0.1631(2) 0.12273(17) 0.0191(6) Uani 1 1 d . . . C12 C 0.3075(3) 0.2388(2) 0.17366(16) 0.0183(6) Uani 1 1 d . . . Cl1 Cl 0.0000 0.2500 0.28327(6) 0.0400(3) Uani 1 2 d S . . Fe1 Fe 0.17593(3) 0.17371(3) 0.09962(2) 0.01461(11) Uani 1 1 d . . . Ga1 Ga 0.0000 0.2500 0.14840(2) 0.01658(12) Uani 1 2 d S . . O1 O 0.1128(2) -0.0068(2) 0.19262(15) 0.0379(6) Uani 1 1 d . . . O2 O 0.0529(2) 0.1143(2) -0.04436(13) 0.0367(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0163(14) 0.0252(15) 0.0226(14) 0.0014(12) -0.0008(11) 0.0017(12) C2 0.0175(14) 0.0268(15) 0.0230(14) -0.0023(12) 0.0038(12) -0.0005(12) C3 0.0268(16) 0.0207(15) 0.0299(15) -0.0040(13) -0.0009(13) 0.0026(12) C4 0.0265(17) 0.0282(17) 0.0247(15) 0.0088(13) 0.0010(13) -0.0007(13) C5 0.0263(17) 0.0280(16) 0.0252(15) -0.0046(13) 0.0126(13) -0.0004(13) C6 0.0202(16) 0.0243(16) 0.0324(16) 0.0030(13) -0.0049(13) 0.0018(12) C7 0.0257(16) 0.0388(19) 0.0183(13) -0.0032(13) -0.0037(12) -0.0005(14) C8 0.0163(14) 0.0171(14) 0.0188(12) -0.0008(11) 0.0004(10) -0.0001(11) C9 0.0175(14) 0.0192(13) 0.0172(12) 0.0000(11) 0.0018(11) -0.0024(11) C10 0.0142(13) 0.0238(15) 0.0188(12) -0.0009(11) 0.0055(10) -0.0017(11) C11 0.0146(13) 0.0213(14) 0.0212(13) 0.0010(11) -0.0007(11) 0.0002(11) C12 0.0161(13) 0.0218(14) 0.0169(12) 0.0003(11) 0.0010(10) -0.0008(11) Cl1 0.0260(6) 0.0807(10) 0.0134(4) 0.000 0.000 0.0135(6) Fe1 0.0129(2) 0.0175(2) 0.01344(17) 0.00051(15) 0.00062(14) 0.00065(15) Ga1 0.0139(2) 0.0230(2) 0.01292(19) 0.000 0.000 0.00294(18) O1 0.0380(15) 0.0327(14) 0.0430(14) 0.0176(12) 0.0030(12) -0.0026(12) O2 0.0341(14) 0.0511(17) 0.0249(11) -0.0137(11) -0.0065(10) 0.0011(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.143(4) . ? C1 Fe1 1.760(3) . ? C2 O2 1.150(4) . ? C2 Fe1 1.754(3) . ? C3 C8 1.508(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C9 1.502(4) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C10 1.503(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C11 1.496(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C12 1.508(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C12 1.429(4) . ? C8 C9 1.431(4) . ? C8 Fe1 2.119(3) . ? C9 C10 1.438(4) . ? C9 Fe1 2.099(3) . ? C10 C11 1.422(4) . ? C10 Fe1 2.108(3) . ? C11 C12 1.440(4) . ? C11 Fe1 2.123(3) . ? C12 Fe1 2.109(3) . ? Cl1 Ga1 2.2829(11) . ? Fe1 Ga1 2.3524(4) . ? Ga1 Fe1 2.3524(4) 4 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 Fe1 177.4(3) . . ? O2 C2 Fe1 176.4(3) . . ? C8 C3 H3A 109.5 . . ? C8 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C8 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C9 C4 H4A 109.5 . . ? C9 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C9 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C10 C5 H5A 109.5 . . ? C10 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C10 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 H6A 109.5 . . ? C11 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C11 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 C7 H7A 109.5 . . ? C12 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C12 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C12 C8 C9 107.9(3) . . ? C12 C8 C3 125.8(3) . . ? C9 C8 C3 125.9(3) . . ? C12 C8 Fe1 69.87(17) . . ? C9 C8 Fe1 69.40(16) . . ? C3 C8 Fe1 132.2(2) . . ? C8 C9 C10 107.8(2) . . ? C8 C9 C4 126.2(3) . . ? C10 C9 C4 125.8(3) . . ? C8 C9 Fe1 70.94(16) . . ? C10 C9 Fe1 70.34(16) . . ? C4 C9 Fe1 128.7(2) . . ? C11 C10 C9 108.4(2) . . ? C11 C10 C5 125.7(3) . . ? C9 C10 C5 125.9(3) . . ? C11 C10 Fe1 70.92(16) . . ? C9 C10 Fe1 69.68(16) . . ? C5 C10 Fe1 126.9(2) . . ? C10 C11 C12 107.7(3) . . ? C10 C11 C6 126.3(3) . . ? C12 C11 C6 125.9(3) . . ? C10 C11 Fe1 69.79(16) . . ? C12 C11 Fe1 69.61(17) . . ? C6 C11 Fe1 128.9(2) . . ? C8 C12 C11 108.2(2) . . ? C8 C12 C7 126.6(3) . . ? C11 C12 C7 124.8(3) . . ? C8 C12 Fe1 70.62(17) . . ? C11 C12 Fe1 70.61(17) . . ? C7 C12 Fe1 129.9(2) . . ? C2 Fe1 C1 96.20(14) . . ? C2 Fe1 C9 95.15(13) . . ? C1 Fe1 C9 162.55(13) . . ? C2 Fe1 C10 95.65(12) . . ? C1 Fe1 C10 125.35(13) . . ? C9 Fe1 C10 39.98(11) . . ? C2 Fe1 C12 160.71(13) . . ? C1 Fe1 C12 100.12(13) . . ? C9 Fe1 C12 66.69(11) . . ? C10 Fe1 C12 66.45(11) . . ? C2 Fe1 C8 128.10(13) . . ? C1 Fe1 C8 134.54(13) . . ? C9 Fe1 C8 39.66(11) . . ? C10 Fe1 C8 66.52(11) . . ? C12 Fe1 C8 39.51(11) . . ? C2 Fe1 C11 128.35(13) . . ? C1 Fe1 C11 95.89(13) . . ? C9 Fe1 C11 66.66(11) . . ? C10 Fe1 C11 39.28(11) . . ? C12 Fe1 C11 39.78(11) . . ? C8 Fe1 C11 66.44(11) . . ? C2 Fe1 Ga1 89.31(10) . . ? C1 Fe1 Ga1 85.72(10) . . ? C9 Fe1 Ga1 107.65(8) . . ? C10 Fe1 Ga1 147.51(8) . . ? C12 Fe1 Ga1 102.05(8) . . ? C8 Fe1 Ga1 85.22(8) . . ? C11 Fe1 Ga1 141.59(8) . . ? Cl1 Ga1 Fe1 110.549(13) . 4 ? Cl1 Ga1 Fe1 110.549(13) . . ? Fe1 Ga1 Fe1 138.90(3) 4 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 C8 C9 C10 -1.5(3) . . . . ? C3 C8 C9 C10 171.1(3) . . . . ? Fe1 C8 C9 C10 -61.0(2) . . . . ? C12 C8 C9 C4 -176.0(3) . . . . ? C3 C8 C9 C4 -3.4(5) . . . . ? Fe1 C8 C9 C4 124.5(3) . . . . ? C12 C8 C9 Fe1 59.5(2) . . . . ? C3 C8 C9 Fe1 -127.9(3) . . . . ? C8 C9 C10 C11 0.8(3) . . . . ? C4 C9 C10 C11 175.2(3) . . . . ? Fe1 C9 C10 C11 -60.6(2) . . . . ? C8 C9 C10 C5 -177.1(3) . . . . ? C4 C9 C10 C5 -2.6(5) . . . . ? Fe1 C9 C10 C5 121.5(3) . . . . ? C8 C9 C10 Fe1 61.4(2) . . . . ? C4 C9 C10 Fe1 -124.1(3) . . . . ? C9 C10 C11 C12 0.3(3) . . . . ? C5 C10 C11 C12 178.2(3) . . . . ? Fe1 C10 C11 C12 -59.5(2) . . . . ? C9 C10 C11 C6 -176.1(3) . . . . ? C5 C10 C11 C6 1.8(5) . . . . ? Fe1 C10 C11 C6 124.0(3) . . . . ? C9 C10 C11 Fe1 59.9(2) . . . . ? C5 C10 C11 Fe1 -122.3(3) . . . . ? C9 C8 C12 C11 1.7(3) . . . . ? C3 C8 C12 C11 -170.9(3) . . . . ? Fe1 C8 C12 C11 60.9(2) . . . . ? C9 C8 C12 C7 174.9(3) . . . . ? C3 C8 C12 C7 2.3(5) . . . . ? Fe1 C8 C12 C7 -125.9(3) . . . . ? C9 C8 C12 Fe1 -59.2(2) . . . . ? C3 C8 C12 Fe1 128.2(3) . . . . ? C10 C11 C12 C8 -1.3(3) . . . . ? C6 C11 C12 C8 175.2(3) . . . . ? Fe1 C11 C12 C8 -60.9(2) . . . . ? C10 C11 C12 C7 -174.6(3) . . . . ? C6 C11 C12 C7 1.8(5) . . . . ? Fe1 C11 C12 C7 125.8(3) . . . . ? C10 C11 C12 Fe1 59.7(2) . . . . ? C6 C11 C12 Fe1 -123.9(3) . . . . ? O2 C2 Fe1 C1 -129(5) . . . . ? O2 C2 Fe1 C9 38(5) . . . . ? O2 C2 Fe1 C10 -3(5) . . . . ? O2 C2 Fe1 C12 19(5) . . . . ? O2 C2 Fe1 C8 62(5) . . . . ? O2 C2 Fe1 C11 -27(5) . . . . ? O2 C2 Fe1 Ga1 145(5) . . . . ? O1 C1 Fe1 C2 103(6) . . . . ? O1 C1 Fe1 C9 -27(7) . . . . ? O1 C1 Fe1 C10 1(7) . . . . ? O1 C1 Fe1 C12 -67(6) . . . . ? O1 C1 Fe1 C8 -89(6) . . . . ? O1 C1 Fe1 C11 -27(6) . . . . ? O1 C1 Fe1 Ga1 -168(6) . . . . ? C8 C9 Fe1 C2 149.53(19) . . . . ? C10 C9 Fe1 C2 -92.65(18) . . . . ? C4 C9 Fe1 C2 27.9(3) . . . . ? C8 C9 Fe1 C1 -80.1(5) . . . . ? C10 C9 Fe1 C1 37.7(5) . . . . ? C4 C9 Fe1 C1 158.3(4) . . . . ? C8 C9 Fe1 C10 -117.8(2) . . . . ? C4 C9 Fe1 C10 120.6(3) . . . . ? C8 C9 Fe1 C12 -37.21(17) . . . . ? C10 C9 Fe1 C12 80.61(17) . . . . ? C4 C9 Fe1 C12 -158.8(3) . . . . ? C10 C9 Fe1 C8 117.8(2) . . . . ? C4 C9 Fe1 C8 -121.6(3) . . . . ? C8 C9 Fe1 C11 -80.70(18) . . . . ? C10 C9 Fe1 C11 37.12(16) . . . . ? C4 C9 Fe1 C11 157.7(3) . . . . ? C8 C9 Fe1 Ga1 58.61(17) . . . . ? C10 C9 Fe1 Ga1 176.43(14) . . . . ? C4 C9 Fe1 Ga1 -63.0(3) . . . . ? C11 C10 Fe1 C2 -149.76(19) . . . . ? C9 C10 Fe1 C2 91.29(19) . . . . ? C5 C10 Fe1 C2 -28.9(3) . . . . ? C11 C10 Fe1 C1 -48.0(2) . . . . ? C9 C10 Fe1 C1 -166.99(18) . . . . ? C5 C10 Fe1 C1 72.8(3) . . . . ? C11 C10 Fe1 C9 118.9(2) . . . . ? C5 C10 Fe1 C9 -120.2(3) . . . . ? C11 C10 Fe1 C12 37.70(17) . . . . ? C9 C10 Fe1 C12 -81.25(18) . . . . ? C5 C10 Fe1 C12 158.5(3) . . . . ? C11 C10 Fe1 C8 80.96(18) . . . . ? C9 C10 Fe1 C8 -37.98(16) . . . . ? C5 C10 Fe1 C8 -158.2(3) . . . . ? C9 C10 Fe1 C11 -118.9(2) . . . . ? C5 C10 Fe1 C11 120.8(3) . . . . ? C11 C10 Fe1 Ga1 112.61(19) . . . . ? C9 C10 Fe1 Ga1 -6.3(3) . . . . ? C5 C10 Fe1 Ga1 -126.6(2) . . . . ? C8 C12 Fe1 C2 58.1(5) . . . . ? C11 C12 Fe1 C2 -60.3(5) . . . . ? C7 C12 Fe1 C2 -179.9(4) . . . . ? C8 C12 Fe1 C1 -154.62(18) . . . . ? C11 C12 Fe1 C1 87.05(19) . . . . ? C7 C12 Fe1 C1 -32.6(3) . . . . ? C8 C12 Fe1 C9 37.35(16) . . . . ? C11 C12 Fe1 C9 -80.99(18) . . . . ? C7 C12 Fe1 C9 159.4(3) . . . . ? C8 C12 Fe1 C10 81.10(18) . . . . ? C11 C12 Fe1 C10 -37.24(17) . . . . ? C7 C12 Fe1 C10 -156.9(3) . . . . ? C11 C12 Fe1 C8 -118.3(2) . . . . ? C7 C12 Fe1 C8 122.0(4) . . . . ? C8 C12 Fe1 C11 118.3(2) . . . . ? C7 C12 Fe1 C11 -119.6(4) . . . . ? C8 C12 Fe1 Ga1 -66.87(16) . . . . ? C11 C12 Fe1 Ga1 174.79(15) . . . . ? C7 C12 Fe1 Ga1 55.2(3) . . . . ? C12 C8 Fe1 C2 -159.13(18) . . . . ? C9 C8 Fe1 C2 -39.9(2) . . . . ? C3 C8 Fe1 C2 80.3(3) . . . . ? C12 C8 Fe1 C1 36.3(2) . . . . ? C9 C8 Fe1 C1 155.51(19) . . . . ? C3 C8 Fe1 C1 -84.2(3) . . . . ? C12 C8 Fe1 C9 -119.2(2) . . . . ? C3 C8 Fe1 C9 120.3(4) . . . . ? C12 C8 Fe1 C10 -80.92(18) . . . . ? C9 C8 Fe1 C10 38.29(17) . . . . ? C3 C8 Fe1 C10 158.5(3) . . . . ? C9 C8 Fe1 C12 119.2(2) . . . . ? C3 C8 Fe1 C12 -120.5(3) . . . . ? C12 C8 Fe1 C11 -37.91(16) . . . . ? C9 C8 Fe1 C11 81.30(18) . . . . ? C3 C8 Fe1 C11 -158.4(3) . . . . ? C12 C8 Fe1 Ga1 115.51(16) . . . . ? C9 C8 Fe1 Ga1 -125.28(16) . . . . ? C3 C8 Fe1 Ga1 -5.0(3) . . . . ? C10 C11 Fe1 C2 39.7(2) . . . . ? C12 C11 Fe1 C2 158.54(19) . . . . ? C6 C11 Fe1 C2 -81.2(3) . . . . ? C10 C11 Fe1 C1 142.43(19) . . . . ? C12 C11 Fe1 C1 -98.75(18) . . . . ? C6 C11 Fe1 C1 21.5(3) . . . . ? C10 C11 Fe1 C9 -37.76(17) . . . . ? C12 C11 Fe1 C9 81.06(18) . . . . ? C6 C11 Fe1 C9 -158.6(3) . . . . ? C12 C11 Fe1 C10 118.8(2) . . . . ? C6 C11 Fe1 C10 -120.9(3) . . . . ? C10 C11 Fe1 C12 -118.8(2) . . . . ? C6 C11 Fe1 C12 120.3(3) . . . . ? C10 C11 Fe1 C8 -81.16(18) . . . . ? C12 C11 Fe1 C8 37.66(17) . . . . ? C6 C11 Fe1 C8 157.9(3) . . . . ? C10 C11 Fe1 Ga1 -127.04(16) . . . . ? C12 C11 Fe1 Ga1 -8.2(2) . . . . ? C6 C11 Fe1 Ga1 112.1(3) . . . . ? C2 Fe1 Ga1 Cl1 152.50(10) . . . . ? C1 Fe1 Ga1 Cl1 56.24(10) . . . . ? C9 Fe1 Ga1 Cl1 -112.31(8) . . . . ? C10 Fe1 Ga1 Cl1 -108.04(15) . . . . ? C12 Fe1 Ga1 Cl1 -43.21(8) . . . . ? C8 Fe1 Ga1 Cl1 -79.17(8) . . . . ? C11 Fe1 Ga1 Cl1 -37.85(13) . . . . ? C2 Fe1 Ga1 Fe1 -27.50(10) . . . 4 ? C1 Fe1 Ga1 Fe1 -123.76(10) . . . 4 ? C9 Fe1 Ga1 Fe1 67.69(8) . . . 4 ? C10 Fe1 Ga1 Fe1 71.96(15) . . . 4 ? C12 Fe1 Ga1 Fe1 136.79(8) . . . 4 ? C8 Fe1 Ga1 Fe1 100.83(8) . . . 4 ? C11 Fe1 Ga1 Fe1 142.15(13) . . . 4 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.310 _refine_diff_density_min -0.761 _refine_diff_density_rms 0.115 data_cj302 _database_code_depnum_ccdc_archive 'CCDC 237194' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H42 B F24 Fe2 Ga O4' _chemical_formula_weight 1427.13 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' O O 0.0106 0.0060 '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' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.442(3) _cell_length_b 15.004(3) _cell_length_c 15.541(3) _cell_angle_alpha 66.25(3) _cell_angle_beta 71.75(3) _cell_angle_gamma 75.17(3) _cell_volume 2894.5(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.637 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1428 _exptl_absorpt_coefficient_mu 1.079 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.552 _exptl_absorpt_correction_T_max 0.810 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43319 _diffrn_reflns_av_R_equivalents 0.0770 _diffrn_reflns_av_sigmaI/netI 0.0552 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.53 _reflns_number_total 13120 _reflns_number_gt 10505 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+3.9021P] 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 'calculated (riding model)' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0033(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 13120 _refine_ls_number_parameters 861 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0599 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1119 _refine_ls_wR_factor_gt 0.1038 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.102 _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 Ga1 Ga 0.84941(2) 0.89372(2) 0.49590(2) 0.02443(9) Uani 1 1 d . . . Fe1 Fe 0.92795(3) 0.79503(3) 0.61520(3) 0.02170(10) Uani 1 1 d . . . Fe2 Fe 0.77271(3) 0.99052(3) 0.37531(3) 0.02249(10) Uani 1 1 d . . . F1 F 0.4847(17) 0.3265(15) 0.3690(15) 0.043(3) Uani 0.63(2) 1 d P A 1 F1A F 0.476(3) 0.313(3) 0.389(3) 0.049(6) Uani 0.37(2) 1 d P A 2 F2 F 0.6271(3) 0.2457(4) 0.3776(9) 0.061(3) Uani 0.63(2) 1 d P A 1 F2A F 0.6243(6) 0.2685(7) 0.3138(14) 0.060(4) Uani 0.37(2) 1 d P A 2 F3 F 0.5279(7) 0.2654(7) 0.5057(4) 0.060(2) Uani 0.63(2) 1 d P A 1 F3A F 0.5848(14) 0.2310(7) 0.4671(12) 0.073(6) Uani 0.37(2) 1 d P A 2 F4 F 0.7865(9) 0.4302(9) 0.5250(9) 0.053(3) Uani 0.46(3) 1 d P B 1 F4A F 0.7729(10) 0.4230(7) 0.5361(8) 0.072(4) Uani 0.54(3) 1 d P B 2 F5 F 0.6490(8) 0.4988(14) 0.5817(6) 0.071(4) Uani 0.46(3) 1 d P B 1 F5A F 0.6681(9) 0.5474(13) 0.5497(14) 0.086(4) Uani 0.54(3) 1 d PU B 2 F6 F 0.7494(17) 0.5871(7) 0.4678(10) 0.069(4) Uani 0.46(3) 1 d PU B 1 F6A F 0.7989(10) 0.5649(9) 0.4395(7) 0.064(3) Uani 0.54(3) 1 d P B 2 F7 F 0.2942(2) 0.85813(18) 0.42600(16) 0.0631(6) Uani 1 1 d . . . F8 F 0.39284(16) 0.94519(16) 0.3046(2) 0.0643(7) Uani 1 1 d . . . F9 F 0.24321(16) 0.95547(15) 0.30208(18) 0.0564(6) Uani 1 1 d . . . F10 F 0.13768(15) 0.68054(19) 0.2783(2) 0.0679(7) Uani 1 1 d . . . F11 F 0.2213(2) 0.6971(2) 0.13383(17) 0.0816(9) Uani 1 1 d . . . F12 F 0.24541(15) 0.56401(15) 0.24915(17) 0.0518(5) Uani 1 1 d . . . F13 F 0.41868(14) 0.6567(2) -0.06896(15) 0.0595(6) Uani 1 1 d . . . F14 F 0.52163(19) 0.57710(16) -0.15533(17) 0.0602(6) Uani 1 1 d . . . F15 F 0.52677(15) 0.72852(14) -0.19013(14) 0.0488(5) Uani 1 1 d . . . F16 F 0.86294(17) 0.46473(19) -0.11508(18) 0.0680(7) Uani 1 1 d . . . F17 F 0.8201(2) 0.36997(17) 0.0278(2) 0.1022(12) Uani 1 1 d U . . F18 F 0.90089(17) 0.4849(2) -0.0065(3) 0.0905(10) Uani 1 1 d . . . F19 F 0.6341(3) 1.0288(2) -0.0848(2) 0.1159(13) Uani 1 1 d . . . F20 F 0.5742(3) 1.05620(19) 0.0392(2) 0.1021(11) Uani 1 1 d . . . F21 F 0.7188(3) 1.0836(2) -0.0327(4) 0.1587(18) Uani 1 1 d U . . F22 F 0.99204(16) 0.7523(2) 0.01270(17) 0.0763(8) Uani 1 1 d . . . F23 F 0.95852(15) 0.67860(17) 0.16634(18) 0.0571(6) Uani 1 1 d . . . F24 F 0.97752(16) 0.82966(18) 0.10625(19) 0.0631(6) Uani 1 1 d . . . O1 O 0.96304(16) 0.97632(15) 0.61852(16) 0.0350(5) Uani 1 1 d . . . O2 O 1.10738(19) 0.77314(19) 0.46982(19) 0.0535(7) Uani 1 1 d . . . O3 O 0.83777(17) 1.16591(16) 0.36009(18) 0.0421(6) Uani 1 1 d . . . O4 O 0.59004(18) 1.0065(2) 0.5202(2) 0.0582(7) Uani 1 1 d . . . C1 C 0.9475(2) 0.9054(2) 0.61742(19) 0.0250(6) Uani 1 1 d . . . C2 C 1.0363(2) 0.7842(2) 0.5254(2) 0.0325(6) Uani 1 1 d . . . C3 C 0.8129(2) 1.0954(2) 0.3691(2) 0.0288(6) Uani 1 1 d . . . C4 C 0.6623(2) 1.0000(2) 0.4642(2) 0.0346(7) Uani 1 1 d . . . C5 C 0.8158(2) 0.70437(19) 0.6765(2) 0.0259(6) Uani 1 1 d . . . C6 C 0.8145(2) 0.7517(2) 0.7409(2) 0.0280(6) Uani 1 1 d . . . C7 C 0.9082(2) 0.7202(2) 0.7661(2) 0.0306(6) Uani 1 1 d . . . C8 C 0.9673(2) 0.6558(2) 0.7174(2) 0.0309(6) Uani 1 1 d . . . C9 C 0.9102(2) 0.64659(19) 0.6610(2) 0.0280(6) Uani 1 1 d . . . C10 C 0.7292(2) 0.7055(2) 0.6416(2) 0.0354(7) Uani 1 1 d . . . H10A H 0.7529 0.6957 0.5792 0.053 Uiso 1 1 calc R . . H10B H 0.6862 0.7689 0.6341 0.053 Uiso 1 1 calc R . . H10C H 0.6922 0.6524 0.6889 0.053 Uiso 1 1 calc R . . C11 C 0.7283(3) 0.8134(2) 0.7838(3) 0.0426(8) Uani 1 1 d . . . H11A H 0.6923 0.7713 0.8458 0.064 Uiso 1 1 calc R . . H11B H 0.6844 0.8461 0.7395 0.064 Uiso 1 1 calc R . . H11C H 0.7518 0.8631 0.7944 0.064 Uiso 1 1 calc R . . C12 C 0.9353(3) 0.7449(3) 0.8390(2) 0.0502(10) Uani 1 1 d . . . H12A H 0.9010 0.8104 0.8388 0.075 Uiso 1 1 calc R . . H12B H 1.0067 0.7445 0.8220 0.075 Uiso 1 1 calc R . . H12C H 0.9158 0.6959 0.9035 0.075 Uiso 1 1 calc R . . C13 C 1.0682(3) 0.6007(3) 0.7276(3) 0.0494(9) Uani 1 1 d . . . H13A H 1.1027 0.6387 0.7429 0.074 Uiso 1 1 calc R . . H13B H 1.1055 0.5908 0.6667 0.074 Uiso 1 1 calc R . . H13C H 1.0621 0.5366 0.7798 0.074 Uiso 1 1 calc R . . C14 C 0.9421(3) 0.5779(2) 0.6050(3) 0.0410(8) Uani 1 1 d . . . H14A H 0.9359 0.5103 0.6499 0.061 Uiso 1 1 calc R . . H14B H 1.0109 0.5817 0.5689 0.061 Uiso 1 1 calc R . . H14C H 0.9002 0.5969 0.5596 0.061 Uiso 1 1 calc R . . C15 C 0.7281(2) 0.9011(2) 0.3258(2) 0.0294(6) Uani 1 1 d . . . C16 C 0.8324(2) 0.8791(2) 0.3138(2) 0.0304(6) Uani 1 1 d . . . C17 C 0.8719(2) 0.9684(2) 0.2515(2) 0.0323(6) Uani 1 1 d . . . C18 C 0.7914(3) 1.0434(2) 0.2234(2) 0.0346(7) Uani 1 1 d . . . C19 C 0.7030(2) 1.0025(2) 0.2695(2) 0.0326(7) Uani 1 1 d . . . C20 C 0.6552(3) 0.8294(3) 0.3795(3) 0.0429(8) Uani 1 1 d . . . H20A H 0.5923 0.8629 0.4075 0.064 Uiso 1 1 calc R . . H20B H 0.6808 0.7746 0.4313 0.064 Uiso 1 1 calc R . . H20C H 0.6449 0.8040 0.3346 0.064 Uiso 1 1 calc R . . C21 C 0.8903(3) 0.7790(2) 0.3502(3) 0.0440(8) Uani 1 1 d . . . H21A H 0.8544 0.7417 0.4148 0.066 Uiso 1 1 calc R . . H21B H 0.9547 0.7857 0.3536 0.066 Uiso 1 1 calc R . . H21C H 0.8998 0.7440 0.3060 0.066 Uiso 1 1 calc R . . C22 C 0.9790(3) 0.9787(3) 0.2129(3) 0.0480(9) Uani 1 1 d . . . H22A H 1.0030 0.9686 0.1506 0.072 Uiso 1 1 calc R . . H22B H 1.0164 0.9294 0.2588 0.072 Uiso 1 1 calc R . . H22C H 0.9877 1.0448 0.2039 0.072 Uiso 1 1 calc R . . C23 C 0.8000(3) 1.1470(3) 0.1529(3) 0.0549(10) Uani 1 1 d . . . H23A H 0.8089 1.1487 0.0871 0.082 Uiso 1 1 calc R . . H23B H 0.8569 1.1685 0.1565 0.082 Uiso 1 1 calc R . . H23C H 0.7399 1.1911 0.1693 0.082 Uiso 1 1 calc R . . C24 C 0.6008(3) 1.0536(3) 0.2592(3) 0.0541(10) Uani 1 1 d . . . H24A H 0.5968 1.1242 0.2446 0.081 Uiso 1 1 calc R . . H24B H 0.5529 1.0262 0.3198 0.081 Uiso 1 1 calc R . . H24C H 0.5860 1.0437 0.2065 0.081 Uiso 1 1 calc R . . C25 C 0.62012(19) 0.57072(19) 0.27313(19) 0.0235(5) Uani 1 1 d . . . C26 C 0.5896(2) 0.4803(2) 0.2967(2) 0.0295(6) Uani 1 1 d . . . H26 H 0.5612 0.4728 0.2530 0.035 Uiso 1 1 calc R . . C27 C 0.5994(2) 0.4017(2) 0.3813(2) 0.0328(7) Uani 1 1 d . A . C28 C 0.6427(2) 0.4078(2) 0.4462(2) 0.0338(7) Uani 1 1 d . . . H28 H 0.6507 0.3534 0.5035 0.041 Uiso 1 1 calc R . . C29 C 0.6741(2) 0.4964(2) 0.4247(2) 0.0293(6) Uani 1 1 d . B . C30 C 0.6616(2) 0.57585(19) 0.34038(19) 0.0250(6) Uani 1 1 d . . . H30 H 0.6823 0.6359 0.3284 0.030 Uiso 1 1 calc R . . C31 C 0.5634(3) 0.3082(2) 0.4021(3) 0.0517(10) Uani 1 1 d . . . C32 C 0.7212(3) 0.5053(2) 0.4930(2) 0.0422(8) Uani 1 1 d . . . C33 C 0.47961(19) 0.70624(18) 0.21194(18) 0.0210(5) Uani 1 1 d . . . C34 C 0.4495(2) 0.77892(18) 0.25488(19) 0.0226(5) Uani 1 1 d . . . H34 H 0.4983 0.8056 0.2624 0.027 Uiso 1 1 calc R . . C35 C 0.3509(2) 0.81267(19) 0.28650(19) 0.0241(5) Uani 1 1 d . . . C36 C 0.2768(2) 0.77610(19) 0.27766(19) 0.0247(6) Uani 1 1 d . . . H36 H 0.2093 0.8009 0.2976 0.030 Uiso 1 1 calc R . . C37 C 0.3045(2) 0.7020(2) 0.23862(19) 0.0242(5) Uani 1 1 d . . . C38 C 0.4031(2) 0.66766(19) 0.20805(19) 0.0241(5) Uani 1 1 d . . . H38 H 0.4196 0.6156 0.1834 0.029 Uiso 1 1 calc R . . C39 C 0.3217(2) 0.8924(2) 0.3287(2) 0.0351(7) Uani 1 1 d . . . C40 C 0.2271(2) 0.6622(2) 0.2252(2) 0.0341(7) Uani 1 1 d . . . C41 C 0.61928(19) 0.62557(18) 0.08649(19) 0.0229(5) Uani 1 1 d . . . C42 C 0.5593(2) 0.65328(19) 0.02192(19) 0.0241(5) Uani 1 1 d . . . H42 H 0.5007 0.6990 0.0289 0.029 Uiso 1 1 calc R . . C43 C 0.5829(2) 0.6158(2) -0.0524(2) 0.0261(6) Uani 1 1 d . . . C44 C 0.6699(2) 0.5532(2) -0.0689(2) 0.0278(6) Uani 1 1 d . . . H44 H 0.6859 0.5278 -0.1196 0.033 Uiso 1 1 calc R . . C45 C 0.7331(2) 0.5287(2) -0.0087(2) 0.0282(6) Uani 1 1 d . . . C46 C 0.7072(2) 0.5623(2) 0.0683(2) 0.0264(6) Uani 1 1 d . . . H46 H 0.7505 0.5415 0.1101 0.032 Uiso 1 1 calc R . . C47 C 0.5128(2) 0.6442(2) -0.1156(2) 0.0332(7) Uani 1 1 d . . . C48 C 0.8280(2) 0.4607(2) -0.0231(2) 0.0367(7) Uani 1 1 d . . . C49 C 0.6679(2) 0.74840(19) 0.13739(18) 0.0226(5) Uani 1 1 d . . . C50 C 0.6366(2) 0.8472(2) 0.0882(2) 0.0300(6) Uani 1 1 d . . . H50 H 0.5698 0.8673 0.0838 0.036 Uiso 1 1 calc R . . C51 C 0.7004(3) 0.9176(2) 0.0454(2) 0.0372(7) Uani 1 1 d . . . C52 C 0.7981(3) 0.8919(2) 0.0500(2) 0.0378(7) Uani 1 1 d . . . H52 H 0.8410 0.9400 0.0217 0.045 Uiso 1 1 calc R . . C53 C 0.8318(2) 0.7940(2) 0.0970(2) 0.0299(6) Uani 1 1 d . . . C54 C 0.7681(2) 0.7243(2) 0.13970(19) 0.0242(5) Uani 1 1 d . . . H54 H 0.7932 0.6577 0.1717 0.029 Uiso 1 1 calc R . . C55 C 0.6625(4) 1.0209(3) -0.0097(3) 0.0620(12) Uani 1 1 d . . . C56 C 0.9386(2) 0.7640(3) 0.0955(2) 0.0390(8) Uani 1 1 d . . . B1 B 0.5963(2) 0.6640(2) 0.1775(2) 0.0222(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.02836(17) 0.02351(16) 0.02159(16) -0.00562(12) -0.00759(12) -0.00593(12) Fe1 0.0239(2) 0.02058(19) 0.01933(19) -0.00439(15) -0.00405(15) -0.00685(15) Fe2 0.0234(2) 0.02220(19) 0.0228(2) -0.00732(15) -0.00636(16) -0.00483(15) F1 0.048(6) 0.031(4) 0.053(6) 0.001(4) -0.025(5) -0.019(3) F1A 0.034(5) 0.035(9) 0.071(16) 0.000(9) -0.019(8) -0.016(6) F2 0.046(2) 0.025(2) 0.104(9) -0.023(4) -0.011(3) -0.0036(17) F2A 0.062(4) 0.032(4) 0.087(9) -0.024(5) -0.014(5) -0.009(3) F3 0.079(4) 0.053(4) 0.042(3) 0.012(2) -0.017(3) -0.045(3) F3A 0.115(13) 0.032(4) 0.075(10) 0.019(5) -0.057(11) -0.033(6) F4 0.036(4) 0.071(7) 0.076(6) -0.054(6) -0.028(4) 0.015(3) F4A 0.129(9) 0.028(3) 0.068(5) 0.012(3) -0.079(6) -0.002(4) F5 0.073(5) 0.108(8) 0.024(4) -0.030(4) -0.005(3) 0.002(5) F5A 0.080(5) 0.120(8) 0.094(8) -0.086(6) -0.031(5) 0.020(5) F6 0.132(9) 0.038(3) 0.055(5) 0.004(3) -0.058(6) -0.032(5) F6A 0.081(6) 0.071(5) 0.049(4) 0.001(3) -0.037(4) -0.038(4) F7 0.0854(18) 0.0659(15) 0.0458(13) -0.0377(12) -0.0024(12) -0.0105(13) F8 0.0406(12) 0.0563(13) 0.114(2) -0.0612(14) 0.0049(12) -0.0151(10) F9 0.0455(12) 0.0360(10) 0.0919(17) -0.0356(11) -0.0205(12) 0.0140(9) F10 0.0239(10) 0.0878(17) 0.115(2) -0.0687(17) 0.0012(11) -0.0123(11) F11 0.104(2) 0.107(2) 0.0507(14) 0.0028(14) -0.0430(14) -0.0640(18) F12 0.0461(12) 0.0454(11) 0.0760(15) -0.0278(11) -0.0127(11) -0.0183(9) F13 0.0293(10) 0.1114(19) 0.0386(11) -0.0226(12) -0.0089(9) -0.0169(11) F14 0.0854(17) 0.0536(13) 0.0655(15) -0.0284(11) -0.0486(13) 0.0007(12) F15 0.0479(12) 0.0436(11) 0.0409(11) 0.0099(9) -0.0230(9) -0.0093(9) F16 0.0506(13) 0.0808(17) 0.0615(15) -0.0384(13) -0.0016(11) 0.0161(12) F17 0.0659(16) 0.0332(12) 0.124(2) 0.0063(13) 0.0242(16) 0.0169(11) F18 0.0362(12) 0.122(2) 0.162(3) -0.111(2) -0.0395(16) 0.0288(14) F19 0.186(4) 0.0684(19) 0.071(2) 0.0176(15) -0.073(2) 0.002(2) F20 0.135(3) 0.0380(13) 0.104(2) 0.0000(14) -0.048(2) 0.0190(16) F21 0.130(3) 0.0478(15) 0.261(4) 0.053(2) -0.110(3) -0.0484(17) F22 0.0328(11) 0.160(3) 0.0572(14) -0.0725(17) 0.0037(10) -0.0097(14) F23 0.0305(10) 0.0663(14) 0.0732(15) -0.0239(13) -0.0165(10) -0.0010(10) F24 0.0447(12) 0.0785(16) 0.0900(18) -0.0437(14) -0.0190(12) -0.0216(12) O1 0.0370(12) 0.0276(10) 0.0448(13) -0.0148(9) -0.0104(10) -0.0078(9) O2 0.0470(15) 0.0494(15) 0.0488(15) -0.0209(12) 0.0138(12) -0.0073(12) O3 0.0409(13) 0.0289(11) 0.0639(16) -0.0176(11) -0.0191(12) -0.0070(10) O4 0.0311(13) 0.098(2) 0.0608(17) -0.0502(17) 0.0059(12) -0.0186(14) C1 0.0239(13) 0.0248(13) 0.0227(13) -0.0053(11) -0.0051(11) -0.0035(11) C2 0.0375(17) 0.0262(14) 0.0291(15) -0.0075(12) -0.0021(13) -0.0080(12) C3 0.0255(14) 0.0264(14) 0.0336(16) -0.0094(12) -0.0103(12) -0.0003(11) C4 0.0273(15) 0.0466(18) 0.0390(17) -0.0220(15) -0.0067(14) -0.0105(13) C5 0.0294(14) 0.0234(13) 0.0228(13) -0.0038(11) -0.0033(11) -0.0113(11) C6 0.0353(15) 0.0242(13) 0.0214(14) -0.0041(11) -0.0010(12) -0.0133(12) C7 0.0427(17) 0.0286(14) 0.0195(13) 0.0005(11) -0.0083(12) -0.0177(13) C8 0.0332(15) 0.0242(13) 0.0295(15) 0.0024(12) -0.0116(13) -0.0090(12) C9 0.0337(15) 0.0204(12) 0.0264(14) -0.0036(11) -0.0042(12) -0.0095(11) C10 0.0317(16) 0.0417(17) 0.0351(17) -0.0108(14) -0.0063(13) -0.0158(14) C11 0.0453(19) 0.0354(17) 0.0420(19) -0.0169(15) 0.0111(15) -0.0185(15) C12 0.078(3) 0.052(2) 0.0275(17) -0.0047(15) -0.0177(18) -0.031(2) C13 0.0425(19) 0.0353(17) 0.059(2) 0.0036(16) -0.0254(18) -0.0042(15) C14 0.0456(19) 0.0281(15) 0.048(2) -0.0181(14) -0.0011(16) -0.0091(14) C15 0.0372(16) 0.0307(14) 0.0257(14) -0.0105(12) -0.0092(12) -0.0109(13) C16 0.0402(17) 0.0306(14) 0.0222(14) -0.0121(12) -0.0053(12) -0.0061(13) C17 0.0362(16) 0.0413(16) 0.0231(14) -0.0153(13) -0.0021(12) -0.0118(14) C18 0.0484(19) 0.0336(15) 0.0217(14) -0.0038(12) -0.0092(13) -0.0144(14) C19 0.0396(17) 0.0355(16) 0.0257(15) -0.0071(12) -0.0145(13) -0.0080(13) C20 0.053(2) 0.0404(18) 0.0442(19) -0.0140(15) -0.0112(16) -0.0240(16) C21 0.058(2) 0.0356(17) 0.0383(18) -0.0216(15) -0.0109(16) 0.0060(16) C22 0.0411(19) 0.066(2) 0.044(2) -0.0306(19) 0.0062(16) -0.0201(18) C23 0.079(3) 0.043(2) 0.0356(19) 0.0049(16) -0.0139(19) -0.027(2) C24 0.051(2) 0.059(2) 0.054(2) -0.0108(19) -0.0335(19) -0.0020(19) C25 0.0187(12) 0.0204(12) 0.0249(14) -0.0040(10) -0.0043(10) 0.0002(10) C26 0.0257(14) 0.0241(13) 0.0364(16) -0.0032(12) -0.0141(12) -0.0038(11) C27 0.0263(14) 0.0222(13) 0.0421(17) 0.0013(12) -0.0122(13) -0.0067(11) C28 0.0332(16) 0.0244(14) 0.0297(15) 0.0057(12) -0.0104(13) -0.0023(12) C29 0.0330(15) 0.0239(13) 0.0260(14) -0.0067(11) -0.0081(12) 0.0020(12) C30 0.0293(14) 0.0190(12) 0.0228(13) -0.0061(10) -0.0070(11) 0.0017(11) C31 0.046(2) 0.0272(16) 0.073(3) 0.0112(17) -0.034(2) -0.0139(16) C32 0.066(2) 0.0293(16) 0.0318(17) -0.0092(14) -0.0229(17) 0.0043(16) C33 0.0238(13) 0.0160(11) 0.0181(12) -0.0004(9) -0.0075(10) -0.0005(10) C34 0.0243(13) 0.0184(12) 0.0239(13) -0.0036(10) -0.0093(11) -0.0030(10) C35 0.0277(14) 0.0196(12) 0.0213(13) -0.0052(10) -0.0049(11) -0.0017(11) C36 0.0210(13) 0.0248(13) 0.0216(13) -0.0037(11) -0.0031(11) -0.0020(10) C37 0.0231(13) 0.0256(13) 0.0210(13) -0.0036(11) -0.0054(11) -0.0058(11) C38 0.0269(14) 0.0210(12) 0.0226(13) -0.0061(10) -0.0045(11) -0.0050(11) C39 0.0281(15) 0.0328(15) 0.0444(19) -0.0200(14) -0.0023(13) -0.0019(13) C40 0.0287(15) 0.0421(17) 0.0352(17) -0.0151(14) -0.0060(13) -0.0105(13) C41 0.0216(13) 0.0180(12) 0.0252(13) -0.0043(10) -0.0045(11) -0.0032(10) C42 0.0234(13) 0.0208(12) 0.0227(13) -0.0026(10) -0.0052(11) -0.0030(10) C43 0.0262(14) 0.0255(13) 0.0232(14) -0.0038(11) -0.0052(11) -0.0071(11) C44 0.0313(15) 0.0251(13) 0.0259(14) -0.0102(11) -0.0025(12) -0.0057(12) C45 0.0260(14) 0.0249(13) 0.0322(15) -0.0116(12) -0.0042(12) -0.0025(11) C46 0.0255(14) 0.0243(13) 0.0302(15) -0.0097(11) -0.0089(12) -0.0020(11) C47 0.0347(16) 0.0361(16) 0.0259(15) -0.0056(12) -0.0078(13) -0.0088(13) C48 0.0336(16) 0.0337(16) 0.0449(19) -0.0216(14) -0.0080(14) 0.0030(13) C49 0.0251(13) 0.0234(12) 0.0172(12) -0.0048(10) -0.0052(10) -0.0040(11) C50 0.0331(15) 0.0250(13) 0.0271(15) -0.0006(11) -0.0122(12) -0.0041(12) C51 0.0479(19) 0.0285(15) 0.0294(16) 0.0043(12) -0.0145(14) -0.0135(14) C52 0.0433(18) 0.0381(17) 0.0298(16) -0.0024(13) -0.0048(14) -0.0232(15) C53 0.0265(14) 0.0415(16) 0.0251(14) -0.0151(13) -0.0017(12) -0.0108(13) C54 0.0244(13) 0.0260(13) 0.0220(13) -0.0089(11) -0.0047(11) -0.0036(11) C55 0.078(3) 0.0322(19) 0.060(3) 0.0140(18) -0.030(2) -0.015(2) C56 0.0302(16) 0.060(2) 0.0363(17) -0.0272(17) -0.0002(14) -0.0144(15) B1 0.0213(14) 0.0192(13) 0.0235(15) -0.0038(11) -0.0074(12) -0.0022(11) _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 Ga1 Fe2 2.2655(10) . ? Ga1 Fe1 2.2722(10) . ? Fe1 C2 1.763(3) . ? Fe1 C1 1.764(3) . ? Fe1 C9 2.106(3) . ? Fe1 C6 2.107(3) . ? Fe1 C7 2.113(3) . ? Fe1 C8 2.120(3) . ? Fe1 C5 2.121(3) . ? Fe2 C3 1.770(3) . ? Fe2 C4 1.771(3) . ? Fe2 C15 2.096(3) . ? Fe2 C17 2.100(3) . ? Fe2 C19 2.112(3) . ? Fe2 C16 2.117(3) . ? Fe2 C18 2.117(3) . ? F1 C31 1.31(2) . ? F1A C31 1.32(4) . ? F2 C31 1.224(6) . ? F2A C31 1.626(15) . ? F3 C31 1.445(7) . ? F3A C31 1.236(7) . ? F4 C32 1.306(11) . ? F4A C32 1.307(9) . ? F5 C32 1.429(9) . ? F5A C32 1.242(9) . ? F6 C32 1.262(9) . ? F6A C32 1.442(9) . ? F7 C39 1.345(4) . ? F8 C39 1.326(4) . ? F9 C39 1.335(4) . ? F10 C40 1.325(4) . ? F11 C40 1.323(4) . ? F12 C40 1.341(4) . ? F13 C47 1.331(4) . ? F14 C47 1.340(4) . ? F15 C47 1.337(3) . ? F16 C48 1.341(4) . ? F17 C48 1.283(4) . ? F18 C48 1.322(4) . ? F19 C55 1.307(5) . ? F20 C55 1.362(6) . ? F21 C55 1.270(5) . ? F22 C56 1.332(4) . ? F23 C56 1.345(4) . ? F24 C56 1.338(4) . ? O1 C1 1.150(3) . ? O2 C2 1.140(4) . ? O3 C3 1.145(3) . ? O4 C4 1.141(4) . ? C5 C9 1.424(4) . ? C5 C6 1.436(4) . ? C5 C10 1.504(4) . ? C6 C7 1.435(4) . ? C6 C11 1.496(4) . ? C7 C8 1.413(4) . ? C7 C12 1.504(4) . ? C8 C9 1.441(4) . ? C8 C13 1.501(5) . ? C9 C14 1.504(4) . ? C15 C16 1.425(4) . ? C15 C19 1.433(4) . ? C15 C20 1.507(4) . ? C16 C17 1.435(4) . ? C16 C21 1.499(4) . ? C17 C18 1.436(5) . ? C17 C22 1.497(4) . ? C18 C19 1.413(4) . ? C18 C23 1.507(4) . ? C19 C24 1.504(5) . ? C25 C30 1.392(4) . ? C25 C26 1.404(4) . ? C25 B1 1.638(4) . ? C26 C27 1.386(4) . ? C27 C28 1.385(4) . ? C27 C31 1.498(4) . ? C28 C29 1.393(4) . ? C29 C30 1.396(4) . ? C29 C32 1.491(4) . ? C33 C38 1.398(4) . ? C33 C34 1.409(4) . ? C33 B1 1.640(4) . ? C34 C35 1.385(4) . ? C35 C36 1.385(4) . ? C35 C39 1.497(4) . ? C36 C37 1.388(4) . ? C37 C38 1.384(4) . ? C37 C40 1.497(4) . ? C41 C42 1.398(4) . ? C41 C46 1.403(4) . ? C41 B1 1.646(4) . ? C42 C43 1.394(4) . ? C43 C44 1.384(4) . ? C43 C47 1.496(4) . ? C44 C45 1.390(4) . ? C45 C46 1.390(4) . ? C45 C48 1.498(4) . ? C49 C50 1.396(4) . ? C49 C54 1.408(4) . ? C49 B1 1.640(4) . ? C50 C51 1.398(4) . ? C51 C52 1.381(5) . ? C51 C55 1.492(5) . ? C52 C53 1.386(5) . ? C53 C54 1.390(4) . ? C53 C56 1.487(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Fe2 Ga1 Fe1 178.99(2) . . ? C2 Fe1 C1 94.86(13) . . ? C2 Fe1 C9 93.82(13) . . ? C1 Fe1 C9 160.44(12) . . ? C2 Fe1 C6 158.92(12) . . ? C1 Fe1 C6 101.85(12) . . ? C9 Fe1 C6 66.46(12) . . ? C2 Fe1 C7 126.67(14) . . ? C1 Fe1 C7 94.75(12) . . ? C9 Fe1 C7 66.11(11) . . ? C6 Fe1 C7 39.77(12) . . ? C2 Fe1 C8 93.81(14) . . ? C1 Fe1 C8 121.90(12) . . ? C9 Fe1 C8 39.87(11) . . ? C6 Fe1 C8 66.47(12) . . ? C7 Fe1 C8 39.01(12) . . ? C2 Fe1 C5 126.87(13) . . ? C1 Fe1 C5 137.93(12) . . ? C9 Fe1 C5 39.38(11) . . ? C6 Fe1 C5 39.71(11) . . ? C7 Fe1 C5 66.35(11) . . ? C8 Fe1 C5 66.50(11) . . ? C2 Fe1 Ga1 88.71(11) . . ? C1 Fe1 Ga1 85.68(9) . . ? C9 Fe1 Ga1 112.02(9) . . ? C6 Fe1 Ga1 105.15(9) . . ? C7 Fe1 Ga1 144.30(9) . . ? C8 Fe1 Ga1 151.87(8) . . ? C5 Fe1 Ga1 89.71(8) . . ? C3 Fe2 C4 95.23(14) . . ? C3 Fe2 C15 157.45(13) . . ? C4 Fe2 C15 96.03(13) . . ? C3 Fe2 C17 98.93(13) . . ? C4 Fe2 C17 161.10(13) . . ? C15 Fe2 C17 66.54(12) . . ? C3 Fe2 C19 119.52(13) . . ? C4 Fe2 C19 95.53(13) . . ? C15 Fe2 C19 39.83(12) . . ? C17 Fe2 C19 66.56(12) . . ? C3 Fe2 C16 135.64(13) . . ? C4 Fe2 C16 128.91(13) . . ? C15 Fe2 C16 39.54(12) . . ? C17 Fe2 C16 39.79(11) . . ? C19 Fe2 C16 66.68(12) . . ? C3 Fe2 C18 91.60(13) . . ? C4 Fe2 C18 127.70(14) . . ? C15 Fe2 C18 66.10(12) . . ? C17 Fe2 C18 39.82(13) . . ? C19 Fe2 C18 39.04(12) . . ? C16 Fe2 C18 66.50(12) . . ? C3 Fe2 Ga1 90.58(10) . . ? C4 Fe2 Ga1 88.68(11) . . ? C15 Fe2 Ga1 109.13(9) . . ? C17 Fe2 Ga1 103.57(9) . . ? C19 Fe2 Ga1 148.92(9) . . ? C16 Fe2 Ga1 86.78(9) . . ? C18 Fe2 Ga1 143.12(10) . . ? O1 C1 Fe1 178.1(2) . . ? O2 C2 Fe1 177.0(3) . . ? O3 C3 Fe2 176.1(3) . . ? O4 C4 Fe2 178.6(3) . . ? C9 C5 C6 107.6(2) . . ? C9 C5 C10 125.9(3) . . ? C6 C5 C10 126.1(3) . . ? C9 C5 Fe1 69.71(15) . . ? C6 C5 Fe1 69.60(15) . . ? C10 C5 Fe1 131.6(2) . . ? C7 C6 C5 107.6(3) . . ? C7 C6 C11 125.3(3) . . ? C5 C6 C11 126.8(3) . . ? C7 C6 Fe1 70.36(16) . . ? C5 C6 Fe1 70.70(16) . . ? C11 C6 Fe1 129.6(2) . . ? C8 C7 C6 108.8(2) . . ? C8 C7 C12 125.7(3) . . ? C6 C7 C12 125.3(3) . . ? C8 C7 Fe1 70.73(16) . . ? C6 C7 Fe1 69.87(16) . . ? C12 C7 Fe1 129.3(2) . . ? C7 C8 C9 107.5(3) . . ? C7 C8 C13 126.8(3) . . ? C9 C8 C13 125.6(3) . . ? C7 C8 Fe1 70.26(16) . . ? C9 C8 Fe1 69.54(15) . . ? C13 C8 Fe1 128.9(2) . . ? C5 C9 C8 108.5(3) . . ? C5 C9 C14 126.2(3) . . ? C8 C9 C14 124.9(3) . . ? C5 C9 Fe1 70.92(15) . . ? C8 C9 Fe1 70.59(15) . . ? C14 C9 Fe1 129.7(2) . . ? C16 C15 C19 108.8(3) . . ? C16 C15 C20 126.8(3) . . ? C19 C15 C20 124.1(3) . . ? C16 C15 Fe2 71.02(16) . . ? C19 C15 Fe2 70.69(16) . . ? C20 C15 Fe2 129.0(2) . . ? C15 C16 C17 107.2(3) . . ? C15 C16 C21 126.0(3) . . ? C17 C16 C21 126.4(3) . . ? C15 C16 Fe2 69.43(16) . . ? C17 C16 Fe2 69.49(16) . . ? C21 C16 Fe2 131.5(2) . . ? C16 C17 C18 107.9(3) . . ? C16 C17 C22 126.0(3) . . ? C18 C17 C22 125.7(3) . . ? C16 C17 Fe2 70.72(17) . . ? C18 C17 Fe2 70.70(18) . . ? C22 C17 Fe2 129.6(2) . . ? C19 C18 C17 108.4(3) . . ? C19 C18 C23 125.7(3) . . ? C17 C18 C23 125.8(3) . . ? C19 C18 Fe2 70.29(17) . . ? C17 C18 Fe2 69.48(17) . . ? C23 C18 Fe2 128.2(2) . . ? C18 C19 C15 107.7(3) . . ? C18 C19 C24 126.8(3) . . ? C15 C19 C24 125.5(3) . . ? C18 C19 Fe2 70.67(17) . . ? C15 C19 Fe2 69.49(16) . . ? C24 C19 Fe2 127.0(2) . . ? C30 C25 C26 115.3(2) . . ? C30 C25 B1 124.5(2) . . ? C26 C25 B1 119.9(2) . . ? C27 C26 C25 122.6(3) . . ? C28 C27 C26 121.1(3) . . ? C28 C27 C31 119.6(3) . . ? C26 C27 C31 119.4(3) . . ? C27 C28 C29 117.7(3) . . ? C28 C29 C30 120.6(3) . . ? C28 C29 C32 119.1(3) . . ? C30 C29 C32 120.3(3) . . ? C25 C30 C29 122.6(3) . . ? F2 C31 F3A 62.9(7) . . ? F2 C31 F1 113.1(11) . . ? F3A C31 F1 123.2(9) . . ? F2 C31 F1A 114.4(18) . . ? F3A C31 F1A 111.2(15) . . ? F1 C31 F1A 13(2) . . ? F2 C31 F3 106.3(4) . . ? F3A C31 F3 43.5(7) . . ? F1 C31 F3 103.8(10) . . ? F1A C31 F3 91.1(16) . . ? F2 C31 C27 114.3(3) . . ? F3A C31 C27 121.9(4) . . ? F1 C31 C27 111.0(9) . . ? F1A C31 C27 119.4(16) . . ? F3 C31 C27 107.5(4) . . ? F2 C31 F2A 34.1(3) . . ? F3A C31 F2A 95.4(8) . . ? F1 C31 F2A 87.4(11) . . ? F1A C31 F2A 94.3(18) . . ? F3 C31 F2A 136.8(4) . . ? C27 C31 F2A 106.9(4) . . ? F5A C32 F6 71.9(6) . . ? F5A C32 F4A 112.5(9) . . ? F6 C32 F4A 120.9(9) . . ? F5A C32 F4 117.8(8) . . ? F6 C32 F4 113.0(10) . . ? F4A C32 F4 10.3(11) . . ? F5A C32 F5 32.2(5) . . ? F6 C32 F5 103.5(6) . . ? F4A C32 F5 91.0(7) . . ? F4 C32 F5 99.6(7) . . ? F5A C32 F6A 103.2(6) . . ? F6 C32 F6A 32.9(6) . . ? F4A C32 F6A 99.5(7) . . ? F4 C32 F6A 89.6(7) . . ? F5 C32 F6A 132.3(5) . . ? F5A C32 C29 116.8(5) . . ? F6 C32 C29 115.5(4) . . ? F4A C32 C29 113.1(6) . . ? F4 C32 C29 114.9(6) . . ? F5 C32 C29 108.3(6) . . ? F6A C32 C29 109.8(4) . . ? C38 C33 C34 115.2(2) . . ? C38 C33 B1 122.7(2) . . ? C34 C33 B1 121.9(2) . . ? C35 C34 C33 122.0(2) . . ? C34 C35 C36 121.4(2) . . ? C34 C35 C39 120.4(3) . . ? C36 C35 C39 118.1(3) . . ? C35 C36 C37 117.7(3) . . ? C38 C37 C36 120.7(2) . . ? C38 C37 C40 119.6(3) . . ? C36 C37 C40 119.6(3) . . ? C37 C38 C33 122.8(2) . . ? F8 C39 F9 106.9(3) . . ? F8 C39 F7 106.5(3) . . ? F9 C39 F7 103.9(3) . . ? F8 C39 C35 113.4(3) . . ? F9 C39 C35 112.4(3) . . ? F7 C39 C35 113.1(3) . . ? F11 C40 F10 107.5(3) . . ? F11 C40 F12 105.1(3) . . ? F10 C40 F12 105.2(3) . . ? F11 C40 C37 111.9(3) . . ? F10 C40 C37 113.8(3) . . ? F12 C40 C37 112.7(3) . . ? C42 C41 C46 115.7(3) . . ? C42 C41 B1 125.3(2) . . ? C46 C41 B1 118.9(2) . . ? C43 C42 C41 121.9(3) . . ? C44 C43 C42 121.3(3) . . ? C44 C43 C47 119.4(3) . . ? C42 C43 C47 119.2(3) . . ? C43 C44 C45 117.7(3) . . ? C46 C45 C44 120.8(3) . . ? C46 C45 C48 119.3(3) . . ? C44 C45 C48 119.8(3) . . ? C45 C46 C41 122.4(3) . . ? F13 C47 F15 105.9(3) . . ? F13 C47 F14 106.3(3) . . ? F15 C47 F14 105.4(2) . . ? F13 C47 C43 113.2(2) . . ? F15 C47 C43 112.8(2) . . ? F14 C47 C43 112.7(3) . . ? F17 C48 F18 109.4(3) . . ? F17 C48 F16 105.8(3) . . ? F18 C48 F16 102.6(3) . . ? F17 C48 C45 113.1(3) . . ? F18 C48 C45 112.7(3) . . ? F16 C48 C45 112.6(3) . . ? C50 C49 C54 115.5(2) . . ? C50 C49 B1 122.0(2) . . ? C54 C49 B1 122.1(2) . . ? C49 C50 C51 122.1(3) . . ? C52 C51 C50 121.0(3) . . ? C52 C51 C55 120.0(3) . . ? C50 C51 C55 118.9(3) . . ? C51 C52 C53 118.3(3) . . ? C52 C53 C54 120.5(3) . . ? C52 C53 C56 118.7(3) . . ? C54 C53 C56 120.6(3) . . ? C53 C54 C49 122.5(3) . . ? F21 C55 F19 110.8(4) . . ? F21 C55 F20 105.4(4) . . ? F19 C55 F20 97.8(4) . . ? F21 C55 C51 115.2(4) . . ? F19 C55 C51 113.2(4) . . ? F20 C55 C51 112.9(3) . . ? F22 C56 F24 106.1(3) . . ? F22 C56 F23 106.2(3) . . ? F24 C56 F23 105.1(3) . . ? F22 C56 C53 112.2(3) . . ? F24 C56 C53 113.1(3) . . ? F23 C56 C53 113.5(3) . . ? C25 B1 C33 104.2(2) . . ? C25 B1 C49 113.7(2) . . ? C33 B1 C49 112.7(2) . . ? C25 B1 C41 109.4(2) . . ? C33 B1 C41 113.1(2) . . ? C49 B1 C41 103.9(2) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.069 _refine_diff_density_min -0.699 _refine_diff_density_rms 0.073