Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Cameron Jones' _publ_contact_author_name 'Cameron Jones' _publ_contact_author_address ; Chemistry Department Cardiff University PO Box 912 Park Place Cardiff CF10 3TB UNITED KINGDOM ; _publ_contact_author_email JONESCA6@CARDIFF.AC.UK _publ_section_title ; Synthesis and Characterisation of Complexes of Group 13 Metal Amidinate Heterocycles with the CpFe(CO)2 Fragment ; data_compound2a _database_code_depnum_ccdc_archive 'CCDC 617851' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H36 Al Cl Fe N2 O2' _chemical_formula_weight 502.83 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' N N 0.0061 0.0033 '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' Al Al 0.0645 0.0514 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.7688(18) _cell_length_b 15.849(3) _cell_length_c 17.550(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2438.9(9) _cell_formula_units_Z 4 _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 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 0.787 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.725 _exptl_absorpt_correction_T_max 0.858 _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 32614 _diffrn_reflns_av_R_equivalents 0.1256 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 26.50 _reflns_number_total 5035 _reflns_number_gt 4431 _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^)+(0.0188P)^2^+0.8421P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.001(14) _refine_ls_number_reflns 5035 _refine_ls_number_parameters 283 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0765 _refine_ls_wR_factor_gt 0.0726 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 0.30500(4) 0.46515(2) 0.09485(2) 0.01837(10) Uani 1 1 d . . . Cl1 Cl 0.03008(8) 0.42944(4) 0.26025(4) 0.02529(15) Uani 1 1 d . . . Al1 Al 0.20384(9) 0.51133(4) 0.21292(4) 0.01532(16) Uani 1 1 d . . . O1 O -0.0179(2) 0.45552(15) 0.06035(10) 0.0352(5) Uani 1 1 d . . . O2 O 0.3039(3) 0.29473(12) 0.15547(12) 0.0356(5) Uani 1 1 d . . . N1 N 0.1446(2) 0.62529(13) 0.23091(11) 0.0173(5) Uani 1 1 d . . . N2 N 0.3145(2) 0.55733(12) 0.29707(11) 0.0180(4) Uani 1 1 d . . . C1 C 0.2365(3) 0.63061(15) 0.29266(13) 0.0162(5) Uani 1 1 d . . . C2 C 0.0357(3) 0.68585(16) 0.19899(13) 0.0170(5) Uani 1 1 d . . . H2 H 0.0449 0.7406 0.2270 0.020 Uiso 1 1 calc R . . C3 C -0.1272(3) 0.65219(17) 0.20780(15) 0.0228(6) Uani 1 1 d . . . H3A H -0.1345 0.5957 0.1841 0.027 Uiso 1 1 calc R . . H3B H -0.1516 0.6463 0.2626 0.027 Uiso 1 1 calc R . . C4 C -0.2422(3) 0.71109(18) 0.17058(15) 0.0263(6) Uani 1 1 d . . . H4A H -0.2402 0.7664 0.1967 0.032 Uiso 1 1 calc R . . H4B H -0.3460 0.6872 0.1761 0.032 Uiso 1 1 calc R . . C5 C -0.2061(3) 0.72324(17) 0.08628(14) 0.0262(6) Uani 1 1 d . . . H5A H -0.2149 0.6685 0.0594 0.031 Uiso 1 1 calc R . . H5B H -0.2806 0.7629 0.0635 0.031 Uiso 1 1 calc R . . C6 C -0.0459(3) 0.75789(18) 0.07659(14) 0.0236(6) Uani 1 1 d . . . H6A H -0.0402 0.8150 0.0992 0.028 Uiso 1 1 calc R . . H6B H -0.0220 0.7627 0.0216 0.028 Uiso 1 1 calc R . . C7 C 0.0718(3) 0.70037(17) 0.11505(13) 0.0217(6) Uani 1 1 d . . . H7A H 0.0741 0.6454 0.0883 0.026 Uiso 1 1 calc R . . H7B H 0.1742 0.7262 0.1105 0.026 Uiso 1 1 calc R . . C8 C 0.4314(3) 0.52691(16) 0.35003(13) 0.0166(5) Uani 1 1 d . . . H8 H 0.4075 0.5480 0.4024 0.020 Uiso 1 1 calc R . . C9 C 0.5909(3) 0.55652(17) 0.32759(14) 0.0214(6) Uani 1 1 d . . . H9A H 0.5938 0.6190 0.3270 0.026 Uiso 1 1 calc R . . H9B H 0.6152 0.5361 0.2757 0.026 Uiso 1 1 calc R . . C10 C 0.7100(3) 0.52319(16) 0.38386(14) 0.0235(6) Uani 1 1 d . . . H10A H 0.8128 0.5418 0.3677 0.028 Uiso 1 1 calc R . . H10B H 0.6898 0.5468 0.4351 0.028 Uiso 1 1 calc R . . C11 C 0.7056(3) 0.42731(17) 0.38757(15) 0.0257(6) Uani 1 1 d . . . H11A H 0.7766 0.4077 0.4277 0.031 Uiso 1 1 calc R . . H11B H 0.7409 0.4039 0.3383 0.031 Uiso 1 1 calc R . . C12 C 0.5464(3) 0.39398(17) 0.40459(16) 0.0239(6) Uani 1 1 d . . . H12A H 0.5187 0.4084 0.4577 0.029 Uiso 1 1 calc R . . H12B H 0.5465 0.3317 0.4000 0.029 Uiso 1 1 calc R . . C13 C 0.4268(3) 0.43078(16) 0.35029(14) 0.0195(6) Uani 1 1 d . . . H13A H 0.4458 0.4096 0.2981 0.023 Uiso 1 1 calc R . . H13B H 0.3241 0.4116 0.3661 0.023 Uiso 1 1 calc R . . C14 C 0.2427(3) 0.70823(15) 0.34538(15) 0.0211(6) Uani 1 1 d . . . C15 C 0.3068(4) 0.78212(17) 0.29813(16) 0.0299(6) Uani 1 1 d . . . H15A H 0.4106 0.7686 0.2814 0.045 Uiso 1 1 calc R . . H15B H 0.3087 0.8333 0.3294 0.045 Uiso 1 1 calc R . . H15C H 0.2419 0.7915 0.2535 0.045 Uiso 1 1 calc R . . C16 C 0.3446(3) 0.69880(18) 0.41589(15) 0.0277(7) Uani 1 1 d . . . H16A H 0.3089 0.6511 0.4466 0.042 Uiso 1 1 calc R . . H16B H 0.3398 0.7506 0.4463 0.042 Uiso 1 1 calc R . . H16C H 0.4500 0.6887 0.3998 0.042 Uiso 1 1 calc R . . C17 C 0.0818(3) 0.72736(19) 0.37585(15) 0.0285(7) Uani 1 1 d . . . H17A H 0.0158 0.7446 0.3336 0.043 Uiso 1 1 calc R . . H17B H 0.0874 0.7730 0.4134 0.043 Uiso 1 1 calc R . . H17C H 0.0397 0.6767 0.3999 0.043 Uiso 1 1 calc R . . C18 C 0.3600(3) 0.57194(18) 0.03054(16) 0.0284(7) Uani 1 1 d . . . H18 H 0.2873 0.6114 0.0122 0.034 Uiso 1 1 calc R . . C19 C 0.4130(3) 0.49971(19) -0.00915(15) 0.0274(6) Uani 1 1 d . . . H19 H 0.3828 0.4828 -0.0588 0.033 Uiso 1 1 calc R . . C20 C 0.5177(3) 0.4577(2) 0.03777(15) 0.0274(6) Uani 1 1 d . . . H20 H 0.5702 0.4071 0.0256 0.033 Uiso 1 1 calc R . . C21 C 0.5316(3) 0.5044(2) 0.10701(15) 0.0294(6) Uani 1 1 d . . . H21 H 0.5953 0.4903 0.1489 0.035 Uiso 1 1 calc R . . C22 C 0.4342(3) 0.57508(18) 0.10234(17) 0.0298(7) Uani 1 1 d . . . H22 H 0.4208 0.6171 0.1403 0.036 Uiso 1 1 calc R . . C23 C 0.1103(3) 0.46008(19) 0.07442(13) 0.0244(6) Uani 1 1 d . . . C24 C 0.3045(3) 0.36348(18) 0.13330(14) 0.0244(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01967(18) 0.01875(19) 0.01670(17) 0.00128(15) 0.00191(16) -0.00058(17) Cl1 0.0245(3) 0.0234(4) 0.0280(3) 0.0019(3) 0.0063(3) -0.0054(3) Al1 0.0151(4) 0.0156(4) 0.0152(3) 0.0013(3) 0.0000(3) -0.0008(3) O1 0.0248(11) 0.0513(14) 0.0293(10) 0.0064(10) -0.0098(9) -0.0055(11) O2 0.0379(12) 0.0208(10) 0.0481(12) 0.0117(9) 0.0107(11) 0.0040(10) N1 0.0175(11) 0.0163(11) 0.0180(11) 0.0006(8) -0.0024(8) 0.0002(9) N2 0.0176(11) 0.0170(11) 0.0195(10) 0.0007(8) -0.0023(9) 0.0017(9) C1 0.0139(12) 0.0184(13) 0.0163(12) 0.0044(10) 0.0006(10) -0.0036(10) C2 0.0158(13) 0.0162(13) 0.0191(12) 0.0011(10) -0.0023(10) 0.0013(11) C3 0.0189(14) 0.0231(15) 0.0263(14) 0.0044(11) 0.0012(11) 0.0009(12) C4 0.0188(14) 0.0298(16) 0.0301(15) 0.0024(12) -0.0021(11) -0.0010(12) C5 0.0284(15) 0.0266(14) 0.0237(14) -0.0006(11) -0.0104(13) 0.0077(13) C6 0.0282(15) 0.0233(15) 0.0192(14) 0.0011(11) -0.0003(11) 0.0096(12) C7 0.0222(15) 0.0224(15) 0.0205(14) 0.0039(11) 0.0014(10) 0.0036(11) C8 0.0179(13) 0.0174(14) 0.0146(11) 0.0010(10) -0.0015(10) 0.0023(10) C9 0.0202(13) 0.0210(15) 0.0230(13) 0.0030(11) -0.0019(11) -0.0028(11) C10 0.0154(12) 0.0322(16) 0.0230(13) 0.0008(11) 0.0003(10) 0.0019(12) C11 0.0193(13) 0.0315(15) 0.0264(15) 0.0021(11) -0.0019(11) 0.0079(13) C12 0.0249(14) 0.0189(14) 0.0278(14) 0.0067(12) -0.0035(13) 0.0039(11) C13 0.0197(13) 0.0186(13) 0.0202(13) 0.0016(11) 0.0005(10) 0.0003(11) C14 0.0244(15) 0.0161(13) 0.0229(14) -0.0005(11) -0.0056(11) 0.0013(11) C15 0.0374(17) 0.0199(14) 0.0324(15) 0.0025(11) -0.0108(14) -0.0055(14) C16 0.0381(17) 0.0225(15) 0.0225(15) -0.0022(11) -0.0066(12) 0.0012(12) C17 0.0350(17) 0.0277(17) 0.0228(14) -0.0055(12) -0.0008(12) 0.0054(14) C18 0.0295(15) 0.0237(15) 0.0321(16) 0.0082(13) 0.0128(13) -0.0034(12) C19 0.0272(14) 0.0334(16) 0.0215(13) 0.0035(12) 0.0070(11) -0.0033(13) C20 0.0203(14) 0.0295(16) 0.0324(15) 0.0036(13) 0.0108(12) 0.0009(13) C21 0.0213(13) 0.0416(17) 0.0253(15) 0.0005(13) 0.0031(12) -0.0064(13) C22 0.0253(15) 0.0273(16) 0.0370(16) -0.0031(13) 0.0099(13) -0.0093(12) C23 0.0317(17) 0.0236(15) 0.0178(13) 0.0044(11) -0.0017(11) -0.0015(13) C24 0.0201(14) 0.0309(16) 0.0221(13) -0.0010(11) 0.0054(12) 0.0010(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C23 1.747(3) . ? Fe1 C24 1.747(3) . ? Fe1 C22 2.082(3) . ? Fe1 C18 2.091(3) . ? Fe1 C21 2.093(3) . ? Fe1 C20 2.120(3) . ? Fe1 C19 2.128(3) . ? Fe1 Al1 2.3699(8) . ? Cl1 Al1 2.1670(10) . ? Al1 N1 1.906(2) . ? Al1 N2 1.912(2) . ? O1 C23 1.153(3) . ? O2 C24 1.157(3) . ? N1 C1 1.353(3) . ? N1 C2 1.465(3) . ? N2 C1 1.350(3) . ? N2 C8 1.465(3) . ? C1 C14 1.540(3) . ? C2 C7 1.524(3) . ? C2 C3 1.533(4) . ? C3 C4 1.521(4) . ? C4 C5 1.525(4) . ? C5 C6 1.518(4) . ? C6 C7 1.533(4) . ? C8 C13 1.524(4) . ? C8 C9 1.527(3) . ? C9 C10 1.531(3) . ? C10 C11 1.521(4) . ? C11 C12 1.522(4) . ? C12 C13 1.533(3) . ? C14 C16 1.533(4) . ? C14 C17 1.539(4) . ? C14 C15 1.541(4) . ? C18 C19 1.418(4) . ? C18 C22 1.419(4) . ? C19 C20 1.401(4) . ? C20 C21 1.428(4) . ? C21 C22 1.411(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 C23 Fe1 C24 91.97(14) . . ? C23 Fe1 C22 125.70(13) . . ? C24 Fe1 C22 138.47(13) . . ? C23 Fe1 C18 98.75(12) . . ? C24 Fe1 C18 162.90(12) . . ? C22 Fe1 C18 39.76(11) . . ? C23 Fe1 C21 164.31(13) . . ? C24 Fe1 C21 103.72(13) . . ? C22 Fe1 C21 39.49(11) . . ? C18 Fe1 C21 66.13(12) . . ? C23 Fe1 C20 139.50(11) . . ? C24 Fe1 C20 97.68(13) . . ? C22 Fe1 C20 66.27(11) . . ? C18 Fe1 C20 65.60(11) . . ? C21 Fe1 C20 39.61(11) . . ? C23 Fe1 C19 105.72(11) . . ? C24 Fe1 C19 124.74(12) . . ? C22 Fe1 C19 66.21(12) . . ? C18 Fe1 C19 39.28(11) . . ? C21 Fe1 C19 65.70(11) . . ? C20 Fe1 C19 38.51(11) . . ? C23 Fe1 Al1 80.08(9) . . ? C24 Fe1 Al1 86.91(9) . . ? C22 Fe1 Al1 83.69(8) . . ? C18 Fe1 Al1 107.96(8) . . ? C21 Fe1 Al1 100.04(8) . . ? C20 Fe1 Al1 139.42(8) . . ? C19 Fe1 Al1 146.83(9) . . ? N1 Al1 N2 69.45(9) . . ? N1 Al1 Cl1 108.21(7) . . ? N2 Al1 Cl1 106.81(7) . . ? N1 Al1 Fe1 122.65(7) . . ? N2 Al1 Fe1 127.11(7) . . ? Cl1 Al1 Fe1 114.42(4) . . ? C1 N1 C2 130.8(2) . . ? C1 N1 Al1 91.68(15) . . ? C2 N1 Al1 137.32(16) . . ? C1 N2 C8 132.4(2) . . ? C1 N2 Al1 91.53(15) . . ? C8 N2 Al1 136.03(16) . . ? N2 C1 N1 107.1(2) . . ? N2 C1 C14 129.4(2) . . ? N1 C1 C14 123.5(2) . . ? N1 C2 C7 109.5(2) . . ? N1 C2 C3 109.9(2) . . ? C7 C2 C3 110.1(2) . . ? C4 C3 C2 111.2(2) . . ? C3 C4 C5 110.9(2) . . ? C6 C5 C4 110.3(2) . . ? C5 C6 C7 111.0(2) . . ? C2 C7 C6 112.1(2) . . ? N2 C8 C13 108.2(2) . . ? N2 C8 C9 112.09(19) . . ? C13 C8 C9 109.4(2) . . ? C8 C9 C10 110.6(2) . . ? C11 C10 C9 110.8(2) . . ? C10 C11 C12 112.2(2) . . ? C11 C12 C13 111.9(2) . . ? C8 C13 C12 111.4(2) . . ? C16 C14 C17 105.8(2) . . ? C16 C14 C1 115.3(2) . . ? C17 C14 C1 109.5(2) . . ? C16 C14 C15 107.2(2) . . ? C17 C14 C15 111.8(2) . . ? C1 C14 C15 107.3(2) . . ? C19 C18 C22 108.3(3) . . ? C19 C18 Fe1 71.78(16) . . ? C22 C18 Fe1 69.81(15) . . ? C20 C19 C18 108.0(3) . . ? C20 C19 Fe1 70.45(15) . . ? C18 C19 Fe1 68.94(14) . . ? C19 C20 C21 108.1(3) . . ? C19 C20 Fe1 71.04(15) . . ? C21 C20 Fe1 69.17(15) . . ? C22 C21 C20 108.1(2) . . ? C22 C21 Fe1 69.84(16) . . ? C20 C21 Fe1 71.21(15) . . ? C21 C22 C18 107.5(2) . . ? C21 C22 Fe1 70.67(16) . . ? C18 C22 Fe1 70.43(16) . . ? O1 C23 Fe1 178.9(3) . . ? O2 C24 Fe1 176.9(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.276 _refine_diff_density_min -0.274 _refine_diff_density_rms 0.054 # Attachment 'cmpd2b.cif' data_compound2b _database_code_depnum_ccdc_archive 'CCDC 617852' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H36 Cl Fe Ga N2 O2' _chemical_formula_weight 545.57 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' N N 0.0061 0.0033 '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' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.7580(18) _cell_length_b 15.865(3) _cell_length_c 17.650(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2452.4(9) _cell_formula_units_Z 4 _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 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 1.822 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.605 _exptl_absorpt_correction_T_max 0.771 _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 8770 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 26.38 _reflns_number_total 4965 _reflns_number_gt 4590 _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^)+(0.0192P)^2^+1.2138P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.005(10) _refine_ls_number_reflns 4965 _refine_ls_number_parameters 283 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0673 _refine_ls_wR_factor_gt 0.0656 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 0.20722(4) 0.488934(17) 0.789013(17) 0.01433(8) Uani 1 1 d . . . Fe1 Fe 0.30543(5) 0.53442(2) 0.90624(2) 0.01629(10) Uani 1 1 d . . . Cl1 Cl 0.02549(9) 0.57062(5) 0.73970(4) 0.02469(18) Uani 1 1 d . . . O1 O -0.0176(3) 0.54644(15) 0.94237(13) 0.0323(6) Uani 1 1 d . . . O2 O 0.3050(3) 0.70612(12) 0.84915(14) 0.0338(6) Uani 1 1 d . . . N1 N 0.1466(3) 0.37090(13) 0.76635(14) 0.0171(5) Uani 1 1 d . . . N2 N 0.3132(3) 0.44042(13) 0.69974(13) 0.0171(5) Uani 1 1 d . . . C1 C 0.2367(3) 0.36703(15) 0.70502(16) 0.0162(6) Uani 1 1 d . . . C2 C 0.0362(3) 0.31177(17) 0.79855(17) 0.0162(6) Uani 1 1 d . . . H2 H 0.0451 0.2564 0.7719 0.019 Uiso 1 1 calc R . . C3 C 0.0726(4) 0.29939(18) 0.88325(17) 0.0205(7) Uani 1 1 d . . . H3A H 0.1752 0.2739 0.8885 0.025 Uiso 1 1 calc R . . H3B H 0.0740 0.3549 0.9088 0.025 Uiso 1 1 calc R . . C4 C -0.0451(4) 0.24269(18) 0.92175(17) 0.0216(7) Uani 1 1 d . . . H4A H -0.0214 0.2385 0.9765 0.026 Uiso 1 1 calc R . . H4B H -0.0393 0.1854 0.8998 0.026 Uiso 1 1 calc R . . C5 C -0.2067(4) 0.27749(18) 0.91156(18) 0.0249(7) Uani 1 1 d . . . H5A H -0.2812 0.2385 0.9351 0.030 Uiso 1 1 calc R . . H5B H -0.2152 0.3327 0.9373 0.030 Uiso 1 1 calc R . . C6 C -0.2433(3) 0.28777(18) 0.82777(18) 0.0233(7) Uani 1 1 d . . . H6A H -0.3466 0.3123 0.8220 0.028 Uiso 1 1 calc R . . H6B H -0.2428 0.2318 0.8029 0.028 Uiso 1 1 calc R . . C7 C -0.1258(3) 0.34535(17) 0.78924(19) 0.0212(6) Uani 1 1 d . . . H7A H -0.1501 0.3499 0.7346 0.025 Uiso 1 1 calc R . . H7B H -0.1322 0.4025 0.8115 0.025 Uiso 1 1 calc R . . C8 C 0.4314(3) 0.47155(16) 0.64836(16) 0.0158(6) Uani 1 1 d . . . H8 H 0.4092 0.4508 0.5960 0.019 Uiso 1 1 calc R . . C9 C 0.4251(3) 0.56775(17) 0.64867(17) 0.0177(6) Uani 1 1 d . . . H9A H 0.4433 0.5886 0.7008 0.021 Uiso 1 1 calc R . . H9B H 0.3222 0.5865 0.6328 0.021 Uiso 1 1 calc R . . C10 C 0.5447(3) 0.60533(18) 0.59527(19) 0.0220(7) Uani 1 1 d . . . H10A H 0.5185 0.5904 0.5424 0.026 Uiso 1 1 calc R . . H10B H 0.5427 0.6675 0.5996 0.026 Uiso 1 1 calc R . . C11 C 0.7047(4) 0.57366(17) 0.61316(17) 0.0232(7) Uani 1 1 d . . . H11A H 0.7379 0.5972 0.6624 0.028 Uiso 1 1 calc R . . H11B H 0.7762 0.5941 0.5738 0.028 Uiso 1 1 calc R . . C12 C 0.7119(3) 0.47741(17) 0.61661(16) 0.0221(6) Uani 1 1 d . . . H12A H 0.6940 0.4539 0.5654 0.027 Uiso 1 1 calc R . . H12B H 0.8148 0.4597 0.6334 0.027 Uiso 1 1 calc R . . C13 C 0.5925(3) 0.44310(18) 0.67119(17) 0.0202(7) Uani 1 1 d . . . H13A H 0.6152 0.4632 0.7231 0.024 Uiso 1 1 calc R . . H13B H 0.5971 0.3807 0.6715 0.024 Uiso 1 1 calc R . . C14 C 0.2439(3) 0.28964(16) 0.65255(17) 0.0190(7) Uani 1 1 d . . . C15 C 0.3454(4) 0.30017(18) 0.58204(18) 0.0251(8) Uani 1 1 d . . . H15A H 0.3463 0.2474 0.5531 0.038 Uiso 1 1 calc R . . H15B H 0.4497 0.3141 0.5978 0.038 Uiso 1 1 calc R . . H15C H 0.3049 0.3456 0.5503 0.038 Uiso 1 1 calc R . . C16 C 0.0823(4) 0.26960(19) 0.62244(19) 0.0277(8) Uani 1 1 d . . . H16A H 0.0889 0.2256 0.5836 0.041 Uiso 1 1 calc R . . H16B H 0.0375 0.3206 0.6004 0.041 Uiso 1 1 calc R . . H16C H 0.0180 0.2499 0.6643 0.041 Uiso 1 1 calc R . . C17 C 0.3092(4) 0.21571(17) 0.69920(18) 0.0265(7) Uani 1 1 d . . . H17A H 0.2455 0.2065 0.7441 0.040 Uiso 1 1 calc R . . H17B H 0.4137 0.2291 0.7151 0.040 Uiso 1 1 calc R . . H17C H 0.3100 0.1645 0.6681 0.040 Uiso 1 1 calc R . . C18 C 0.4349(4) 0.42412(19) 0.9011(2) 0.0287(8) Uani 1 1 d . . . H18 H 0.4224 0.3811 0.8641 0.034 Uiso 1 1 calc R . . C19 C 0.3589(4) 0.42881(19) 0.97124(18) 0.0243(7) Uani 1 1 d . . . H19 H 0.2853 0.3897 0.9895 0.029 Uiso 1 1 calc R . . C20 C 0.4100(4) 0.5011(2) 1.00989(17) 0.0259(7) Uani 1 1 d . . . H20 H 0.3780 0.5190 1.0587 0.031 Uiso 1 1 calc R . . C21 C 0.5170(4) 0.5420(2) 0.96325(18) 0.0260(7) Uani 1 1 d . . . H21 H 0.5697 0.5927 0.9751 0.031 Uiso 1 1 calc R . . C22 C 0.5329(3) 0.4946(2) 0.89522(18) 0.0254(7) Uani 1 1 d . . . H22 H 0.5974 0.5079 0.8536 0.030 Uiso 1 1 calc R . . C23 C 0.1108(4) 0.54111(18) 0.92825(17) 0.0210(7) Uani 1 1 d . . . C24 C 0.3064(4) 0.63727(18) 0.87021(17) 0.0224(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 0.01538(16) 0.01409(14) 0.01351(15) 0.00041(11) 0.00026(13) 0.00024(13) Fe1 0.0175(2) 0.01663(19) 0.0147(2) 0.00049(16) -0.0017(2) 0.00061(18) Cl1 0.0242(4) 0.0223(3) 0.0276(4) 0.0018(3) -0.0075(3) 0.0065(3) O1 0.0244(14) 0.0471(14) 0.0253(13) 0.0048(11) 0.0052(11) 0.0032(11) O2 0.0326(14) 0.0192(10) 0.0496(16) 0.0107(10) -0.0081(13) -0.0036(11) N1 0.0210(13) 0.0122(11) 0.0181(13) -0.0005(10) 0.0042(10) -0.0035(10) N2 0.0209(13) 0.0160(10) 0.0143(13) -0.0002(9) 0.0059(11) -0.0024(10) C1 0.0178(15) 0.0146(12) 0.0161(15) 0.0032(11) -0.0020(12) 0.0015(11) C2 0.0151(14) 0.0139(12) 0.0196(16) -0.0008(12) 0.0025(13) -0.0003(11) C3 0.0216(18) 0.0217(15) 0.0181(17) 0.0037(12) 0.0010(13) -0.0035(13) C4 0.0249(17) 0.0231(15) 0.0169(17) 0.0010(12) 0.0030(13) -0.0082(13) C5 0.0223(17) 0.0261(14) 0.0261(18) -0.0024(13) 0.0102(16) -0.0082(15) C6 0.0153(16) 0.0264(14) 0.0282(18) 0.0003(13) 0.0032(13) -0.0008(12) C7 0.0201(16) 0.0219(14) 0.0217(16) 0.0038(13) 0.0015(14) 0.0006(12) C8 0.0143(15) 0.0189(14) 0.0143(15) 0.0000(12) 0.0050(12) -0.0036(11) C9 0.0192(16) 0.0181(13) 0.0160(16) 0.0024(12) -0.0014(13) -0.0017(12) C10 0.0218(16) 0.0208(14) 0.0235(17) 0.0067(13) 0.0001(15) -0.0038(13) C11 0.0204(16) 0.0289(15) 0.0204(17) 0.0024(12) 0.0036(14) -0.0042(15) C12 0.0143(14) 0.0303(15) 0.0218(16) -0.0004(12) 0.0026(13) -0.0017(14) C13 0.0215(16) 0.0216(14) 0.0176(16) 0.0004(13) -0.0012(13) 0.0031(13) C14 0.0201(17) 0.0149(12) 0.0220(17) -0.0029(12) 0.0043(13) 0.0007(11) C15 0.036(2) 0.0179(14) 0.0209(18) -0.0050(13) 0.0086(14) -0.0007(13) C16 0.034(2) 0.0249(16) 0.0245(18) -0.0048(14) -0.0004(15) -0.0075(15) C17 0.0321(18) 0.0201(13) 0.0273(18) 0.0016(12) 0.0087(16) 0.0071(15) C18 0.0286(18) 0.0223(16) 0.035(2) -0.0043(15) -0.0125(16) 0.0114(14) C19 0.0253(18) 0.0234(15) 0.0242(18) 0.0105(14) -0.0059(14) 0.0001(13) C20 0.0258(17) 0.0337(17) 0.0182(16) 0.0033(15) -0.0065(13) 0.0023(16) C21 0.0185(17) 0.0333(17) 0.0261(18) 0.0033(14) -0.0107(14) -0.0036(14) C22 0.0158(14) 0.0376(17) 0.0227(16) 0.0013(15) 0.0006(13) 0.0051(15) C23 0.0291(19) 0.0199(14) 0.0139(16) 0.0050(13) -0.0007(14) 0.0005(14) C24 0.0155(15) 0.0274(16) 0.0242(17) -0.0045(13) -0.0014(14) -0.0017(15) _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 N2 1.984(2) . ? Ga1 N1 1.987(2) . ? Ga1 Cl1 2.2294(8) . ? Ga1 Fe1 2.3540(6) . ? Fe1 C24 1.751(3) . ? Fe1 C23 1.751(4) . ? Fe1 C19 2.084(3) . ? Fe1 C18 2.087(3) . ? Fe1 C22 2.099(3) . ? Fe1 C21 2.112(3) . ? Fe1 C20 2.113(3) . ? O1 C23 1.155(4) . ? O2 C24 1.154(3) . ? N1 C1 1.341(4) . ? N1 C2 1.462(3) . ? N2 C1 1.347(3) . ? N2 C8 1.462(3) . ? C1 C14 1.539(4) . ? C2 C7 1.524(4) . ? C2 C3 1.541(4) . ? C3 C4 1.527(4) . ? C4 C5 1.530(5) . ? C5 C6 1.522(5) . ? C6 C7 1.535(4) . ? C8 C9 1.527(4) . ? C8 C13 1.536(4) . ? C9 C10 1.530(4) . ? C10 C11 1.522(4) . ? C11 C12 1.529(4) . ? C12 C13 1.522(4) . ? C14 C15 1.538(4) . ? C14 C17 1.543(4) . ? C14 C16 1.545(4) . ? C18 C19 1.408(5) . ? C18 C22 1.414(4) . ? C19 C20 1.407(4) . ? C20 C21 1.407(4) . ? C21 C22 1.424(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 N2 Ga1 N1 66.39(9) . . ? N2 Ga1 Cl1 104.45(7) . . ? N1 Ga1 Cl1 106.18(8) . . ? N2 Ga1 Fe1 130.24(8) . . ? N1 Ga1 Fe1 124.29(7) . . ? Cl1 Ga1 Fe1 115.20(3) . . ? C24 Fe1 C23 91.64(14) . . ? C24 Fe1 C19 161.44(14) . . ? C23 Fe1 C19 98.34(13) . . ? C24 Fe1 C18 139.71(15) . . ? C23 Fe1 C18 126.09(14) . . ? C19 Fe1 C18 39.47(13) . . ? C24 Fe1 C22 104.01(14) . . ? C23 Fe1 C22 164.27(13) . . ? C19 Fe1 C22 66.18(13) . . ? C18 Fe1 C22 39.49(12) . . ? C24 Fe1 C21 96.63(14) . . ? C23 Fe1 C21 138.13(14) . . ? C19 Fe1 C21 65.59(12) . . ? C18 Fe1 C21 65.95(13) . . ? C22 Fe1 C21 39.52(12) . . ? C24 Fe1 C20 123.06(14) . . ? C23 Fe1 C20 104.17(13) . . ? C19 Fe1 C20 39.18(12) . . ? C18 Fe1 C20 65.97(13) . . ? C22 Fe1 C20 66.03(13) . . ? C21 Fe1 C20 38.89(12) . . ? C24 Fe1 Ga1 88.18(10) . . ? C23 Fe1 Ga1 81.84(10) . . ? C19 Fe1 Ga1 108.63(9) . . ? C18 Fe1 Ga1 84.42(10) . . ? C22 Fe1 Ga1 99.97(9) . . ? C21 Fe1 Ga1 139.19(9) . . ? C20 Fe1 Ga1 147.41(9) . . ? C1 N1 C2 132.3(2) . . ? C1 N1 Ga1 92.79(16) . . ? C2 N1 Ga1 134.66(19) . . ? C1 N2 C8 133.4(2) . . ? C1 N2 Ga1 92.73(17) . . ? C8 N2 Ga1 133.85(17) . . ? N1 C1 N2 108.0(2) . . ? N1 C1 C14 123.1(2) . . ? N2 C1 C14 128.9(3) . . ? N1 C2 C7 110.4(2) . . ? N1 C2 C3 108.8(2) . . ? C7 C2 C3 110.0(3) . . ? C4 C3 C2 111.6(2) . . ? C3 C4 C5 111.1(2) . . ? C6 C5 C4 110.4(3) . . ? C5 C6 C7 110.7(3) . . ? C2 C7 C6 111.6(2) . . ? N2 C8 C9 108.1(2) . . ? N2 C8 C13 112.9(2) . . ? C9 C8 C13 109.0(2) . . ? C8 C9 C10 111.3(2) . . ? C11 C10 C9 111.9(2) . . ? C10 C11 C12 112.1(3) . . ? C13 C12 C11 110.7(2) . . ? C12 C13 C8 111.1(2) . . ? C15 C14 C1 115.1(2) . . ? C15 C14 C17 107.5(2) . . ? C1 C14 C17 107.5(2) . . ? C15 C14 C16 105.9(3) . . ? C1 C14 C16 109.5(2) . . ? C17 C14 C16 111.5(2) . . ? C19 C18 C22 108.0(3) . . ? C19 C18 Fe1 70.15(18) . . ? C22 C18 Fe1 70.71(17) . . ? C18 C19 C20 108.6(3) . . ? C18 C19 Fe1 70.39(18) . . ? C20 C19 Fe1 71.53(17) . . ? C21 C20 C19 107.7(3) . . ? C21 C20 Fe1 70.52(17) . . ? C19 C20 Fe1 69.29(17) . . ? C20 C21 C22 108.3(3) . . ? C20 C21 Fe1 70.59(17) . . ? C22 C21 Fe1 69.74(17) . . ? C18 C22 C21 107.3(3) . . ? C18 C22 Fe1 69.80(17) . . ? C21 C22 Fe1 70.74(18) . . ? O1 C23 Fe1 179.2(3) . . ? O2 C24 Fe1 177.4(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.500 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.067 # Attachment 'cmpd2c.cif' data_compound2c _database_code_depnum_ccdc_archive 'CCDC 617853' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H28 Cl Fe Ga N2 O2' _chemical_formula_weight 465.44 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' N N 0.0061 0.0033 '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' 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' _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 16.618(3) _cell_length_b 9.4461(19) _cell_length_c 13.563(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.57(3) _cell_angle_gamma 90.00 _cell_volume 2126.8(7) _cell_formula_units_Z 4 _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 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 2.087 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.680 _exptl_absorpt_correction_T_max 0.818 _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 7968 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4176 _reflns_number_gt 3638 _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^)+(0.0196P)^2^+0.9276P] 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 4176 _refine_ls_number_parameters 233 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0601 _refine_ls_wR_factor_gt 0.0574 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 0.731437(12) 0.81712(2) 0.968569(15) 0.02047(7) Uani 1 1 d . . . Fe1 Fe 0.602866(16) 0.71766(3) 0.94567(2) 0.02319(8) Uani 1 1 d . . . Cl1 Cl 0.78407(3) 0.82202(6) 1.12340(4) 0.03500(13) Uani 1 1 d . . . O1 O 0.55551(10) 0.92934(18) 1.08731(11) 0.0453(4) Uani 1 1 d . . . N1 N 0.82429(9) 0.78971(15) 0.88372(11) 0.0209(3) Uani 1 1 d . . . C1 C 0.82804(11) 0.92853(19) 0.86287(13) 0.0204(4) Uani 1 1 d . . . O2 O 0.65597(9) 0.51199(16) 1.09342(12) 0.0417(4) Uani 1 1 d . . . N2 N 0.76776(9) 0.99359(15) 0.90628(12) 0.0245(4) Uani 1 1 d . . . C2 C 0.88898(12) 1.0061(2) 0.79984(14) 0.0262(4) Uani 1 1 d . . . C3 C 0.94817(12) 0.9093(2) 0.74823(15) 0.0329(5) Uani 1 1 d . . . H3A H 0.9823 0.9665 0.7066 0.049 Uiso 1 1 calc R . . H3B H 0.9180 0.8404 0.7072 0.049 Uiso 1 1 calc R . . H3C H 0.9820 0.8593 0.7979 0.049 Uiso 1 1 calc R . . C4 C 0.93913(13) 1.1058(2) 0.86833(17) 0.0380(5) Uani 1 1 d . . . H4A H 0.9033 1.1729 0.8996 0.057 Uiso 1 1 calc R . . H4B H 0.9778 1.1579 0.8296 0.057 Uiso 1 1 calc R . . H4C H 0.9683 1.0500 0.9193 0.057 Uiso 1 1 calc R . . C5 C 0.84309(13) 1.0876(2) 0.71620(16) 0.0395(5) Uani 1 1 d . . . H5A H 0.8074 1.1576 0.7448 0.059 Uiso 1 1 calc R . . H5B H 0.8110 1.0209 0.6754 0.059 Uiso 1 1 calc R . . H5C H 0.8817 1.1359 0.6753 0.059 Uiso 1 1 calc R . . C6 C 0.88234(11) 0.67413(19) 0.87420(14) 0.0232(4) Uani 1 1 d . . . H6 H 0.9052 0.6781 0.8073 0.028 Uiso 1 1 calc R . . C7 C 0.83712(13) 0.5355(2) 0.88510(18) 0.0378(5) Uani 1 1 d . . . H7A H 0.8119 0.5337 0.9491 0.057 Uiso 1 1 calc R . . H7B H 0.8749 0.4562 0.8813 0.057 Uiso 1 1 calc R . . H7C H 0.7954 0.5272 0.8320 0.057 Uiso 1 1 calc R . . C8 C 0.95029(13) 0.6866(2) 0.95263(16) 0.0335(5) Uani 1 1 d . . . H8A H 0.9769 0.7786 0.9466 0.050 Uiso 1 1 calc R . . H8B H 0.9895 0.6107 0.9436 0.050 Uiso 1 1 calc R . . H8C H 0.9283 0.6785 1.0182 0.050 Uiso 1 1 calc R . . C9 C 0.74463(13) 1.1432(2) 0.91226(17) 0.0347(5) Uani 1 1 d . . . H9 H 0.7847 1.2021 0.8778 0.042 Uiso 1 1 calc R . . C10 C 0.66172(15) 1.1647(3) 0.8628(2) 0.0591(8) Uani 1 1 d . . . H10A H 0.6631 1.1385 0.7930 0.089 Uiso 1 1 calc R . . H10B H 0.6461 1.2644 0.8682 0.089 Uiso 1 1 calc R . . H10C H 0.6225 1.1052 0.8953 0.089 Uiso 1 1 calc R . . C11 C 0.7457(2) 1.1849(3) 1.0203(2) 0.0647(8) Uani 1 1 d . . . H11A H 0.7076 1.1256 1.0548 0.097 Uiso 1 1 calc R . . H11B H 0.7300 1.2845 1.0259 0.097 Uiso 1 1 calc R . . H11C H 0.8000 1.1716 1.0499 0.097 Uiso 1 1 calc R . . C12 C 0.55061(13) 0.8129(2) 0.81888(15) 0.0347(5) Uani 1 1 d . . . H12 H 0.5403 0.9114 0.8119 0.042 Uiso 1 1 calc R . . C13 C 0.49669(13) 0.7109(3) 0.85529(16) 0.0384(5) Uani 1 1 d . . . H13 H 0.4440 0.7291 0.8766 0.046 Uiso 1 1 calc R . . C14 C 0.53465(13) 0.5790(3) 0.85431(17) 0.0397(5) Uani 1 1 d . . . H14 H 0.5124 0.4919 0.8751 0.048 Uiso 1 1 calc R . . C15 C 0.61258(13) 0.5983(2) 0.81669(16) 0.0358(5) Uani 1 1 d . . . H15 H 0.6514 0.5260 0.8079 0.043 Uiso 1 1 calc R . . C16 C 0.62227(13) 0.7429(2) 0.79474(15) 0.0321(5) Uani 1 1 d . . . H16 H 0.6685 0.7855 0.7685 0.039 Uiso 1 1 calc R . . C17 C 0.57467(12) 0.8446(2) 1.03204(15) 0.0305(5) Uani 1 1 d . . . C18 C 0.63564(12) 0.5949(2) 1.03477(16) 0.0294(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.02046(12) 0.02140(12) 0.01977(12) -0.00003(8) 0.00328(8) -0.00013(8) Fe1 0.02004(15) 0.02689(16) 0.02281(16) -0.00055(11) 0.00297(11) 0.00010(11) Cl1 0.0331(3) 0.0508(3) 0.0209(3) 0.0004(2) -0.0010(2) -0.0023(2) O1 0.0501(10) 0.0555(10) 0.0303(9) -0.0099(8) 0.0015(7) 0.0252(8) N1 0.0210(8) 0.0189(8) 0.0230(9) 0.0004(6) 0.0045(7) 0.0003(6) C1 0.0208(9) 0.0209(9) 0.0191(9) 0.0000(7) -0.0022(7) -0.0032(7) O2 0.0409(9) 0.0357(9) 0.0484(10) 0.0146(8) 0.0020(8) -0.0001(7) N2 0.0263(9) 0.0183(8) 0.0291(9) 0.0009(7) 0.0038(7) -0.0007(7) C2 0.0257(10) 0.0269(10) 0.0261(10) 0.0054(8) 0.0007(8) -0.0059(8) C3 0.0302(11) 0.0403(12) 0.0287(12) 0.0070(9) 0.0088(9) -0.0072(9) C4 0.0356(12) 0.0318(12) 0.0464(14) -0.0001(10) -0.0005(10) -0.0121(10) C5 0.0386(13) 0.0442(13) 0.0358(13) 0.0160(11) 0.0025(10) -0.0031(11) C6 0.0225(10) 0.0228(10) 0.0245(10) -0.0017(8) 0.0045(8) 0.0053(8) C7 0.0373(13) 0.0223(11) 0.0548(15) 0.0012(10) 0.0140(11) 0.0031(9) C8 0.0321(12) 0.0383(12) 0.0300(12) 0.0015(9) 0.0014(9) 0.0117(10) C9 0.0382(12) 0.0187(10) 0.0476(14) 0.0003(9) 0.0053(10) 0.0028(9) C10 0.0432(15) 0.0323(13) 0.101(2) 0.0080(14) -0.0039(15) 0.0126(11) C11 0.100(2) 0.0327(14) 0.0621(19) -0.0206(13) 0.0132(17) 0.0145(14) C12 0.0375(13) 0.0421(13) 0.0237(11) -0.0002(9) -0.0078(9) 0.0051(10) C13 0.0205(11) 0.0620(16) 0.0322(13) -0.0066(11) -0.0045(9) -0.0010(10) C14 0.0351(12) 0.0436(13) 0.0400(13) -0.0081(11) -0.0010(10) -0.0144(11) C15 0.0362(12) 0.0402(13) 0.0310(12) -0.0130(10) 0.0005(10) 0.0021(10) C16 0.0303(12) 0.0462(13) 0.0199(11) -0.0029(9) 0.0010(9) -0.0033(10) C17 0.0251(11) 0.0398(12) 0.0265(11) 0.0057(10) -0.0011(9) 0.0063(9) C18 0.0231(10) 0.0302(11) 0.0354(12) -0.0014(10) 0.0055(9) -0.0033(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 N2 1.9755(15) . ? Ga1 N1 1.9829(16) . ? Ga1 Cl1 2.2387(8) . ? Ga1 Fe1 2.3419(5) . ? Fe1 C18 1.744(2) . ? Fe1 C17 1.755(2) . ? Fe1 C15 2.093(2) . ? Fe1 C12 2.094(2) . ? Fe1 C14 2.100(2) . ? Fe1 C16 2.100(2) . ? Fe1 C13 2.104(2) . ? O1 C17 1.151(2) . ? N1 C1 1.343(2) . ? N1 C6 1.466(2) . ? C1 N2 1.334(2) . ? C1 C2 1.540(3) . ? O2 C18 1.156(2) . ? N2 C9 1.468(2) . ? C2 C3 1.535(3) . ? C2 C4 1.541(3) . ? C2 C5 1.544(3) . ? C6 C7 1.520(3) . ? C6 C8 1.521(3) . ? C9 C11 1.517(4) . ? C9 C10 1.519(3) . ? C12 C16 1.413(3) . ? C12 C13 1.420(3) . ? C13 C14 1.396(3) . ? C14 C15 1.425(3) . ? C15 C16 1.408(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 N2 Ga1 N1 66.51(6) . . ? N2 Ga1 Cl1 105.64(5) . . ? N1 Ga1 Cl1 105.41(5) . . ? N2 Ga1 Fe1 125.19(5) . . ? N1 Ga1 Fe1 126.85(5) . . ? Cl1 Ga1 Fe1 116.64(3) . . ? C18 Fe1 C17 94.38(10) . . ? C18 Fe1 C15 100.80(10) . . ? C17 Fe1 C15 163.49(9) . . ? C18 Fe1 C12 163.63(9) . . ? C17 Fe1 C12 98.12(9) . . ? C15 Fe1 C12 65.79(9) . . ? C18 Fe1 C14 97.91(10) . . ? C17 Fe1 C14 131.83(9) . . ? C15 Fe1 C14 39.72(8) . . ? C12 Fe1 C14 65.82(9) . . ? C18 Fe1 C16 133.93(9) . . ? C17 Fe1 C16 129.08(9) . . ? C15 Fe1 C16 39.25(9) . . ? C12 Fe1 C16 39.39(8) . . ? C14 Fe1 C16 66.29(9) . . ? C18 Fe1 C13 127.66(10) . . ? C17 Fe1 C13 99.66(9) . . ? C15 Fe1 C13 65.84(9) . . ? C12 Fe1 C13 39.53(9) . . ? C14 Fe1 C13 38.80(9) . . ? C16 Fe1 C13 66.23(9) . . ? C18 Fe1 Ga1 85.42(7) . . ? C17 Fe1 Ga1 84.64(7) . . ? C15 Fe1 Ga1 102.87(7) . . ? C12 Fe1 Ga1 106.19(7) . . ? C14 Fe1 Ga1 142.52(6) . . ? C16 Fe1 Ga1 84.53(7) . . ? C13 Fe1 Ga1 145.68(7) . . ? C1 N1 C6 132.17(16) . . ? C1 N1 Ga1 92.25(11) . . ? C6 N1 Ga1 132.87(12) . . ? N2 C1 N1 108.29(16) . . ? N2 C1 C2 123.44(16) . . ? N1 C1 C2 128.26(16) . . ? C1 N2 C9 132.18(16) . . ? C1 N2 Ga1 92.86(11) . . ? C9 N2 Ga1 134.68(13) . . ? C3 C2 C1 114.87(16) . . ? C3 C2 C4 107.38(17) . . ? C1 C2 C4 107.91(16) . . ? C3 C2 C5 105.51(17) . . ? C1 C2 C5 109.25(16) . . ? C4 C2 C5 111.99(17) . . ? N1 C6 C7 107.63(15) . . ? N1 C6 C8 110.58(15) . . ? C7 C6 C8 110.70(17) . . ? N2 C9 C11 108.18(19) . . ? N2 C9 C10 109.82(18) . . ? C11 C9 C10 111.3(2) . . ? C16 C12 C13 108.3(2) . . ? C16 C12 Fe1 70.52(12) . . ? C13 C12 Fe1 70.59(12) . . ? C14 C13 C12 108.04(19) . . ? C14 C13 Fe1 70.45(12) . . ? C12 C13 Fe1 69.88(12) . . ? C13 C14 C15 107.9(2) . . ? C13 C14 Fe1 70.75(12) . . ? C15 C14 Fe1 69.90(12) . . ? C16 C15 C14 108.3(2) . . ? C16 C15 Fe1 70.63(12) . . ? C14 C15 Fe1 70.38(12) . . ? C15 C16 C12 107.41(19) . . ? C15 C16 Fe1 70.12(12) . . ? C12 C16 Fe1 70.09(12) . . ? O1 C17 Fe1 178.74(19) . . ? O2 C18 Fe1 178.62(19) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.381 _refine_diff_density_min -0.301 _refine_diff_density_rms 0.055 # Attachment 'cmpd2d.cif' data_compound2d _database_code_depnum_ccdc_archive 'CCDC 617854' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H36 Br Fe In N2 O2' _chemical_formula_weight 635.13 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' N N 0.0061 0.0033 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 '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 9.3802(19) _cell_length_b 10.710(2) _cell_length_c 15.261(3) _cell_angle_alpha 109.94(3) _cell_angle_beta 92.94(3) _cell_angle_gamma 91.50(3) _cell_volume 1437.9(5) _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 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 2.715 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.531 _exptl_absorpt_correction_T_max 0.612 _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 11354 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.00 _reflns_number_total 6198 _reflns_number_gt 5281 _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^)+(0.0265P)^2^+0.8126P] 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 6198 _refine_ls_number_parameters 283 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0742 _refine_ls_wR_factor_gt 0.0712 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 In1 In 0.469602(19) 0.534532(19) 0.220620(13) 0.01951(7) Uani 1 1 d . . . Br1 Br 0.60525(3) 0.36314(3) 0.09638(2) 0.03421(9) Uani 1 1 d . . . Fe1 Fe 0.20122(4) 0.50942(4) 0.20564(3) 0.02378(11) Uani 1 1 d . . . O1 O 0.2143(3) 0.7462(3) 0.37114(18) 0.0573(8) Uani 1 1 d . . . O2 O 0.2214(3) 0.3267(3) 0.3084(2) 0.0683(9) Uani 1 1 d . . . N1 N 0.5940(2) 0.7240(2) 0.26655(15) 0.0201(5) Uani 1 1 d . . . N2 N 0.6133(2) 0.5876(2) 0.34575(15) 0.0202(5) Uani 1 1 d . . . C1 C 0.6551(3) 0.7058(3) 0.34210(19) 0.0193(6) Uani 1 1 d . . . C2 C 0.7534(3) 0.8145(3) 0.41523(19) 0.0231(6) Uani 1 1 d . . . C3 C 0.8812(3) 0.8483(3) 0.3665(2) 0.0364(8) Uani 1 1 d . . . H3A H 0.8462 0.8805 0.3168 0.055 Uiso 1 1 calc R . . H3B H 0.9350 0.7684 0.3395 0.055 Uiso 1 1 calc R . . H3C H 0.9436 0.9174 0.4122 0.055 Uiso 1 1 calc R . . C4 C 0.6655(3) 0.9355(3) 0.4606(2) 0.0272(6) Uani 1 1 d . . . H4A H 0.7262 1.0044 0.5078 0.041 Uiso 1 1 calc R . . H4B H 0.5855 0.9092 0.4904 0.041 Uiso 1 1 calc R . . H4C H 0.6285 0.9704 0.4127 0.041 Uiso 1 1 calc R . . C5 C 0.8143(4) 0.7763(3) 0.4978(2) 0.0389(9) Uani 1 1 d . . . H5A H 0.8735 0.8511 0.5409 0.058 Uiso 1 1 calc R . . H5B H 0.8727 0.6987 0.4744 0.058 Uiso 1 1 calc R . . H5C H 0.7355 0.7549 0.5308 0.058 Uiso 1 1 calc R . . C6 C 0.5876(3) 0.8429(3) 0.24017(19) 0.0231(6) Uani 1 1 d . . . H6 H 0.6566 0.9129 0.2825 0.028 Uiso 1 1 calc R . . C7 C 0.4377(3) 0.8963(3) 0.2492(2) 0.0314(7) Uani 1 1 d . . . H7A H 0.4125 0.9215 0.3150 0.038 Uiso 1 1 calc R . . H7B H 0.3677 0.8259 0.2104 0.038 Uiso 1 1 calc R . . C8 C 0.4301(4) 1.0175(3) 0.2180(2) 0.0410(9) Uani 1 1 d . . . H8A H 0.4936 1.0906 0.2606 0.049 Uiso 1 1 calc R . . H8B H 0.3312 1.0482 0.2219 0.049 Uiso 1 1 calc R . . C9 C 0.4747(4) 0.9852(4) 0.1179(2) 0.0466(10) Uani 1 1 d . . . H9A H 0.4042 0.9202 0.0742 0.056 Uiso 1 1 calc R . . H9B H 0.4757 1.0671 0.1016 0.056 Uiso 1 1 calc R . . C10 C 0.6200(4) 0.9289(4) 0.1075(2) 0.0461(9) Uani 1 1 d . . . H10A H 0.6920 0.9988 0.1443 0.055 Uiso 1 1 calc R . . H10B H 0.6425 0.9016 0.0411 0.055 Uiso 1 1 calc R . . C11 C 0.6304(4) 0.8094(3) 0.1400(2) 0.0327(7) Uani 1 1 d . . . H11A H 0.5672 0.7353 0.0983 0.039 Uiso 1 1 calc R . . H11B H 0.7297 0.7798 0.1358 0.039 Uiso 1 1 calc R . . C12 C 0.6782(3) 0.5032(3) 0.39338(19) 0.0202(6) Uani 1 1 d . . . H12 H 0.6995 0.5573 0.4608 0.024 Uiso 1 1 calc R . . C13 C 0.8163(3) 0.4444(3) 0.3513(2) 0.0259(6) Uani 1 1 d . . . H13A H 0.7966 0.3929 0.2841 0.031 Uiso 1 1 calc R . . H13B H 0.8872 0.5173 0.3570 0.031 Uiso 1 1 calc R . . C14 C 0.8777(3) 0.3540(3) 0.4009(2) 0.0308(7) Uani 1 1 d . . . H14A H 0.9041 0.4070 0.4671 0.037 Uiso 1 1 calc R . . H14B H 0.9653 0.3151 0.3714 0.037 Uiso 1 1 calc R . . C15 C 0.7695(3) 0.2424(3) 0.3961(2) 0.0324(7) Uani 1 1 d . . . H15A H 0.7524 0.1827 0.3304 0.039 Uiso 1 1 calc R . . H15B H 0.8090 0.1894 0.4328 0.039 Uiso 1 1 calc R . . C16 C 0.6290(3) 0.2973(3) 0.4338(2) 0.0295(7) Uani 1 1 d . . . H16A H 0.6436 0.3459 0.5018 0.035 Uiso 1 1 calc R . . H16B H 0.5585 0.2227 0.4242 0.035 Uiso 1 1 calc R . . C17 C 0.5702(3) 0.3908(3) 0.3859(2) 0.0225(6) Uani 1 1 d . . . H17A H 0.5450 0.3397 0.3192 0.027 Uiso 1 1 calc R . . H17B H 0.4819 0.4288 0.4150 0.027 Uiso 1 1 calc R . . C18 C 0.2215(4) 0.4917(6) 0.0660(3) 0.0649(15) Uani 1 1 d . . . H18 H 0.3085 0.5021 0.0395 0.078 Uiso 1 1 calc R . . C19 C 0.1284(5) 0.5931(5) 0.1075(3) 0.0680(15) Uani 1 1 d . . . H19 H 0.1422 0.6843 0.1145 0.082 Uiso 1 1 calc R . . C20 C 0.0098(4) 0.5353(5) 0.1374(3) 0.0523(11) Uani 1 1 d . . . H20 H -0.0695 0.5803 0.1678 0.063 Uiso 1 1 calc R . . C21 C 0.0324(4) 0.4025(4) 0.1137(2) 0.0474(10) Uani 1 1 d . . . H21 H -0.0303 0.3388 0.1244 0.057 Uiso 1 1 calc R . . C22 C 0.1639(4) 0.3749(5) 0.0708(2) 0.0554(11) Uani 1 1 d . . . H22 H 0.2051 0.2905 0.0491 0.066 Uiso 1 1 calc R . . C23 C 0.2103(3) 0.6515(4) 0.3055(2) 0.0349(8) Uani 1 1 d . . . C24 C 0.2168(3) 0.4004(4) 0.2680(2) 0.0374(8) 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 In1 0.02120(11) 0.01806(11) 0.01826(11) 0.00560(8) -0.00177(7) -0.00260(8) Br1 0.03808(18) 0.03293(19) 0.02391(17) -0.00068(14) 0.00604(13) 0.00004(14) Fe1 0.0219(2) 0.0291(2) 0.0196(2) 0.00824(18) -0.00279(16) -0.00271(18) O1 0.0449(15) 0.0592(18) 0.0430(15) -0.0145(14) -0.0042(12) 0.0176(13) O2 0.0426(15) 0.090(2) 0.107(2) 0.079(2) 0.0048(15) -0.0043(15) N1 0.0260(12) 0.0151(12) 0.0189(12) 0.0065(10) -0.0045(9) -0.0048(9) N2 0.0247(12) 0.0181(12) 0.0183(12) 0.0078(10) -0.0044(9) 0.0003(10) C1 0.0189(13) 0.0174(14) 0.0216(14) 0.0066(11) 0.0012(11) 0.0033(11) C2 0.0252(14) 0.0183(15) 0.0217(14) 0.0031(12) -0.0066(11) -0.0020(12) C3 0.0261(16) 0.0325(19) 0.044(2) 0.0059(16) -0.0044(14) -0.0048(14) C4 0.0413(17) 0.0176(15) 0.0199(14) 0.0029(12) 0.0013(13) 0.0002(13) C5 0.057(2) 0.0221(16) 0.0330(18) 0.0079(14) -0.0266(16) -0.0069(15) C6 0.0321(15) 0.0200(15) 0.0182(14) 0.0090(12) -0.0045(12) -0.0031(12) C7 0.0353(17) 0.0252(17) 0.0347(17) 0.0123(14) -0.0043(14) 0.0022(13) C8 0.053(2) 0.0272(18) 0.043(2) 0.0137(16) -0.0125(17) 0.0086(16) C9 0.077(3) 0.0286(19) 0.037(2) 0.0177(16) -0.0170(19) 0.0000(18) C10 0.074(3) 0.044(2) 0.0286(18) 0.0229(17) 0.0018(17) -0.0038(19) C11 0.0461(19) 0.0306(18) 0.0239(16) 0.0130(14) 0.0005(14) -0.0005(15) C12 0.0251(14) 0.0162(14) 0.0207(14) 0.0083(12) -0.0010(11) 0.0038(11) C13 0.0265(15) 0.0211(15) 0.0326(17) 0.0127(13) 0.0003(12) -0.0010(12) C14 0.0276(16) 0.0281(17) 0.0419(19) 0.0183(15) 0.0014(13) 0.0096(13) C15 0.0392(18) 0.0234(16) 0.0392(18) 0.0163(15) 0.0028(14) 0.0071(14) C16 0.0329(16) 0.0258(17) 0.0356(17) 0.0180(14) 0.0022(13) -0.0005(13) C17 0.0237(14) 0.0195(15) 0.0245(15) 0.0074(12) 0.0027(11) 0.0004(11) C18 0.036(2) 0.138(5) 0.033(2) 0.049(3) -0.0119(17) -0.025(3) C19 0.076(3) 0.074(3) 0.067(3) 0.051(3) -0.053(3) -0.024(3) C20 0.036(2) 0.077(3) 0.035(2) 0.010(2) -0.0181(16) 0.006(2) C21 0.0317(18) 0.066(3) 0.0326(19) 0.0043(19) -0.0080(15) -0.0193(18) C22 0.048(2) 0.071(3) 0.0249(18) -0.0113(19) -0.0050(16) 0.001(2) C23 0.0221(15) 0.048(2) 0.0307(18) 0.0086(16) -0.0031(13) 0.0088(14) C24 0.0219(15) 0.050(2) 0.047(2) 0.0255(18) 0.0035(14) -0.0027(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag In1 N2 2.178(2) . ? In1 N1 2.190(2) . ? In1 Fe1 2.5151(7) . ? In1 Br1 2.5652(11) . ? Fe1 C24 1.744(3) . ? Fe1 C23 1.745(4) . ? Fe1 C22 2.076(3) . ? Fe1 C19 2.087(3) . ? Fe1 C21 2.090(3) . ? Fe1 C18 2.093(4) . ? Fe1 C20 2.102(3) . ? O1 C23 1.155(4) . ? O2 C24 1.156(4) . ? N1 C1 1.337(3) . ? N1 C6 1.462(3) . ? N2 C1 1.336(3) . ? N2 C12 1.465(3) . ? C1 C2 1.551(4) . ? C2 C4 1.530(4) . ? C2 C3 1.540(4) . ? C2 C5 1.541(4) . ? C6 C11 1.524(4) . ? C6 C7 1.527(4) . ? C7 C8 1.530(4) . ? C8 C9 1.530(5) . ? C9 C10 1.499(6) . ? C10 C11 1.525(4) . ? C12 C17 1.524(4) . ? C12 C13 1.529(4) . ? C13 C14 1.526(4) . ? C14 C15 1.527(4) . ? C15 C16 1.517(4) . ? C16 C17 1.526(4) . ? C18 C22 1.376(6) . ? C18 C19 1.407(7) . ? C19 C20 1.427(6) . ? C20 C21 1.368(6) . ? C21 C22 1.417(5) . ? 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 N2 In1 N1 60.40(8) . . ? N2 In1 Fe1 129.09(7) . . ? N1 In1 Fe1 125.21(7) . . ? N2 In1 Br1 103.81(7) . . ? N1 In1 Br1 108.29(7) . . ? Fe1 In1 Br1 117.06(3) . . ? C24 Fe1 C23 94.18(17) . . ? C24 Fe1 C22 100.36(18) . . ? C23 Fe1 C22 164.35(17) . . ? C24 Fe1 C19 160.83(16) . . ? C23 Fe1 C19 99.14(18) . . ? C22 Fe1 C19 65.37(19) . . ? C24 Fe1 C21 95.87(16) . . ? C23 Fe1 C21 133.21(15) . . ? C22 Fe1 C21 39.76(15) . . ? C19 Fe1 C21 64.96(16) . . ? C24 Fe1 C18 134.3(2) . . ? C23 Fe1 C18 129.6(2) . . ? C22 Fe1 C18 38.54(17) . . ? C19 Fe1 C18 39.35(19) . . ? C21 Fe1 C18 65.40(15) . . ? C24 Fe1 C20 123.88(16) . . ? C23 Fe1 C20 101.11(16) . . ? C22 Fe1 C20 65.89(16) . . ? C19 Fe1 C20 39.84(17) . . ? C21 Fe1 C20 38.09(16) . . ? C18 Fe1 C20 66.36(16) . . ? C24 Fe1 In1 87.03(10) . . ? C23 Fe1 In1 84.57(11) . . ? C22 Fe1 In1 101.83(12) . . ? C19 Fe1 In1 107.82(14) . . ? C21 Fe1 In1 141.44(11) . . ? C18 Fe1 In1 85.26(11) . . ? C20 Fe1 In1 147.53(12) . . ? C1 N1 C6 130.9(2) . . ? C1 N1 In1 94.20(16) . . ? C6 N1 In1 133.31(16) . . ? C1 N2 C12 131.6(2) . . ? C1 N2 In1 94.78(16) . . ? C12 N2 In1 130.14(17) . . ? N2 C1 N1 110.6(2) . . ? N2 C1 C2 127.2(2) . . ? N1 C1 C2 122.2(2) . . ? C4 C2 C3 112.4(3) . . ? C4 C2 C5 104.3(2) . . ? C3 C2 C5 107.4(2) . . ? C4 C2 C1 108.7(2) . . ? C3 C2 C1 108.9(2) . . ? C5 C2 C1 115.1(2) . . ? N1 C6 C11 109.4(2) . . ? N1 C6 C7 110.9(2) . . ? C11 C6 C7 110.0(2) . . ? C6 C7 C8 110.7(3) . . ? C7 C8 C9 111.5(3) . . ? C10 C9 C8 110.9(3) . . ? C9 C10 C11 112.4(3) . . ? C6 C11 C10 111.6(3) . . ? N2 C12 C17 107.9(2) . . ? N2 C12 C13 112.6(2) . . ? C17 C12 C13 109.3(2) . . ? C14 C13 C12 110.9(2) . . ? C13 C14 C15 111.0(2) . . ? C16 C15 C14 111.3(2) . . ? C15 C16 C17 111.7(2) . . ? C12 C17 C16 111.6(2) . . ? C22 C18 C19 107.7(4) . . ? C22 C18 Fe1 70.1(2) . . ? C19 C18 Fe1 70.1(2) . . ? C18 C19 C20 108.2(4) . . ? C18 C19 Fe1 70.5(2) . . ? C20 C19 Fe1 70.6(2) . . ? C21 C20 C19 106.7(4) . . ? C21 C20 Fe1 70.5(2) . . ? C19 C20 Fe1 69.52(19) . . ? C20 C21 C22 109.3(4) . . ? C20 C21 Fe1 71.4(2) . . ? C22 C21 Fe1 69.58(19) . . ? C18 C22 C21 108.0(4) . . ? C18 C22 Fe1 71.4(2) . . ? C21 C22 Fe1 70.7(2) . . ? O1 C23 Fe1 178.9(3) . . ? O2 C24 Fe1 177.3(3) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.416 _refine_diff_density_min -0.547 _refine_diff_density_rms 0.090 # Attachment 'cmpd3.cif' data_compound3 _database_code_depnum_ccdc_archive 'CCDC 617855' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H58 B F24 Fe Ga N2 O3' _chemical_formula_weight 1447.46 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' N N 0.0061 0.0033 '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 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 30.023(5) _cell_length_b 17.780(5) _cell_length_c 26.410(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 115.322(5) _cell_angle_gamma 90.000(5) _cell_volume 12743(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5872 _exptl_absorpt_coefficient_mu 0.766 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.861 _exptl_absorpt_correction_T_max 0.927 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _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 44400 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0704 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 25.33 _reflns_number_total 23061 _reflns_number_gt 15498 _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. During the course of refinement 2 crystallographically independent ion pairs were located in the asymmetric unit that exhibited no significant geometric differences. The tert-butyl groups of both cations were found to be disordered over 2 sites. This disorder was successfully modelled. One CF3 group of one of the anions was found to be disordered over 2 sites. This disorder was successfully modelled. The other anion displayed several CF3 groups disordered over 2 sites which was modelled. In addition, 2 of the pheny rings were found to be disordered over two sites and this disorder was adequately modelled. The disorder displayed by this anion led to the high r-factors for this structure, though the molecular connectivity of the cations is unambiguous. The highest residual electron density peak (2.296 e-/ang.3) seen in the final difference map was located close to Ga(2). ; _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^)+(0.1602P)^2^+66.6504P] 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 23061 _refine_ls_number_parameters 1942 _refine_ls_number_restraints 498 _refine_ls_R_factor_all 0.1611 _refine_ls_R_factor_gt 0.1188 _refine_ls_wR_factor_ref 0.3302 _refine_ls_wR_factor_gt 0.3001 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.185 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.002 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 0.35456(3) -0.23605(5) 0.81707(3) 0.0330(2) Uani 1 1 d . . . Ga2 Ga 0.09716(3) 0.21811(6) 0.95017(4) 0.0442(3) Uani 1 1 d . . . Fe1 Fe 0.29696(5) -0.14341(7) 0.77138(5) 0.0469(3) Uani 1 1 d . . . Fe2 Fe 0.07562(5) 0.11471(8) 0.98938(6) 0.0519(4) Uani 1 1 d . . . F1 F 0.2122(3) 0.0907(4) 0.6623(3) 0.086(2) Uani 1 1 d U . . F2 F 0.1933(2) 0.0870(3) 0.7304(3) 0.0797(18) Uani 1 1 d U . . F3 F 0.1486(2) 0.1490(4) 0.6585(4) 0.105(2) Uani 1 1 d U . . F4 F 0.2155(4) 0.4381(5) 0.6673(4) 0.081(3) Uani 0.724(13) 1 d PU A 1 F5 F 0.2328(3) 0.4591(4) 0.7526(3) 0.067(3) Uani 0.724(13) 1 d PU A 1 F6 F 0.1644(3) 0.4119(4) 0.6999(4) 0.062(3) Uani 0.724(13) 1 d PU A 1 F7 F 0.4920(4) 0.4672(7) 0.9433(5) 0.147(4) Uani 1 1 d U . . F8 F 0.5360(4) 0.3933(7) 0.9331(5) 0.145(4) Uani 1 1 d U . . F9 F 0.5258(5) 0.4990(7) 0.8987(4) 0.156(4) Uani 1 1 d U . . F10 F 0.4382(5) 0.4962(9) 0.6997(5) 0.087(5) Uani 0.506(16) 1 d PU B 1 F11 F 0.4016(5) 0.3911(7) 0.6641(4) 0.062(4) Uani 0.506(16) 1 d PU B 1 F12 F 0.3616(6) 0.4798(12) 0.6766(7) 0.094(5) Uani 0.506(16) 1 d PU B 1 F13 F 0.3692(6) 0.0475(8) 0.9616(6) 0.100(5) Uani 0.62(2) 1 d PU C 1 F14 F 0.3618(5) 0.0994(7) 1.0243(5) 0.082(4) Uani 0.62(2) 1 d PU C 1 F15 F 0.2968(6) 0.0761(11) 0.9446(8) 0.118(6) Uani 0.62(2) 1 d PU C 1 F16 F 0.3080(4) 0.4208(7) 0.9461(5) 0.161(4) Uani 1 1 d U . . F17 F 0.3758(4) 0.4310(6) 0.9810(5) 0.137(3) Uani 1 1 d U . . F18 F 0.3584(5) 0.3730(8) 1.0313(6) 0.175(5) Uani 1 1 d U . . F19 F 0.3695(4) 0.0837(7) 0.6535(4) 0.155(4) Uani 1 1 d U . . F20 F 0.4473(4) 0.0882(6) 0.6801(4) 0.128(3) Uani 1 1 d U . . F21 F 0.4058(5) 0.0003(8) 0.6823(5) 0.166(4) Uani 1 1 d U . . F22 F 0.5237(6) -0.0090(10) 0.8871(6) 0.093(5) Uani 0.54(2) 1 d PU D 1 F23 F 0.5304(5) 0.0976(9) 0.9282(6) 0.095(6) Uani 0.54(2) 1 d PU D 1 F24 F 0.4805(7) 0.0135(11) 0.9271(7) 0.106(6) Uani 0.54(2) 1 d PU D 1 F25 F 0.1269(4) -0.4628(5) 1.1204(4) 0.132(3) Uani 1 1 d U . . F26 F 0.0893(3) -0.4120(5) 1.1595(4) 0.116(3) Uani 1 1 d U . . F27 F 0.1630(4) -0.4174(5) 1.1993(4) 0.134(3) Uani 1 1 d U . . F28 F 0.0921(3) -0.1007(4) 1.1481(4) 0.103(2) Uani 1 1 d U . . F29 F 0.1569(3) -0.1349(5) 1.2148(3) 0.104(2) Uani 1 1 d U . . F30 F 0.1587(3) -0.0732(4) 1.1496(3) 0.100(2) Uani 1 1 d U . . F33 F 0.1417(9) -0.4762(15) 0.8422(10) 0.159(9) Uani 0.57(2) 1 d PU E 1 F34 F 0.3110(2) -0.3904(4) 1.1022(3) 0.0776(18) Uani 1 1 d U . . F35 F 0.2673(3) -0.4852(4) 1.0986(3) 0.089(2) Uani 1 1 d U . . F36 F 0.3131(2) -0.4858(4) 1.0556(2) 0.0789(18) Uani 1 1 d U . . F37 F -0.0220(5) -0.4501(7) 0.9095(6) 0.165(4) Uani 1 1 d U . . F38 F 0.0139(3) -0.4651(5) 0.8633(4) 0.119(3) Uani 1 1 d U . . F39 F -0.0552(3) -0.4189(6) 0.8248(4) 0.139(3) Uani 1 1 d U . . F40 F -0.0062(2) -0.0901(4) 0.8376(3) 0.0772(17) Uani 1 1 d U . . F41 F -0.0370(2) -0.0987(4) 0.8955(3) 0.0833(19) Uani 1 1 d U . . F42 F -0.0721(2) -0.1519(4) 0.8149(3) 0.088(2) Uani 1 1 d U . . F43 F 0.3049(2) -0.0160(4) 1.0503(3) 0.0822(19) Uani 1 1 d U . . F44 F 0.3054(2) -0.1136(3) 1.0976(2) 0.0670(15) Uani 1 1 d U . . F45 F 0.2599(2) -0.0193(3) 1.0954(3) 0.0707(16) Uani 1 1 d U . . F46 F 0.1468(3) -0.1097(5) 0.8192(3) 0.104(2) Uani 1 1 d U . . F47 F 0.1337(4) -0.0099(7) 0.8460(4) 0.141(3) Uani 1 1 d U . . F48 F 0.2029(3) -0.0367(6) 0.8505(3) 0.121(3) Uani 1 1 d U . . O1 O 0.3317(2) -0.3454(3) 0.8040(3) 0.0541(16) Uani 1 1 d . . . O2 O 0.2643(3) -0.2227(5) 0.6647(3) 0.074(2) Uani 1 1 d . . . O3 O 0.2288(3) -0.2146(5) 0.8085(4) 0.082(2) Uani 1 1 d . . . O4 O 0.0823(3) 0.3216(4) 0.9738(3) 0.071(2) Uani 1 1 d . . . O5 O 0.1134(4) 0.2028(7) 1.0921(3) 0.111(4) Uani 1 1 d . . . O6 O -0.0232(3) 0.1725(7) 0.9568(5) 0.118(4) Uani 1 1 d . . . N1 N 0.4011(3) -0.2449(4) 0.8961(3) 0.0386(15) Uani 1 1 d . . . N2 N 0.4231(2) -0.2483(4) 0.8283(3) 0.0413(16) Uani 1 1 d . . . N3 N 0.1600(3) 0.2404(4) 0.9475(3) 0.0448(17) Uani 1 1 d . . . N4 N 0.0904(3) 0.2387(5) 0.8740(3) 0.057(2) Uani 1 1 d . . . C1 C 0.4401(3) -0.2470(4) 0.8840(3) 0.0346(17) Uani 1 1 d . F . C2 C 0.4942(3) -0.2523(6) 0.9267(4) 0.058(3) Uani 1 1 d . . . C3 C 0.5030(7) -0.1803(12) 0.9671(8) 0.073(6) Uani 0.63(2) 1 d P F 1 H3A H 0.4824 -0.1848 0.9874 0.109 Uiso 0.63(2) 1 calc PR F 1 H3B H 0.4942 -0.1343 0.9445 0.109 Uiso 0.63(2) 1 calc PR F 1 H3C H 0.5378 -0.1781 0.9939 0.109 Uiso 0.63(2) 1 calc PR F 1 C4 C 0.5327(7) -0.2531(13) 0.9072(9) 0.076(6) Uani 0.63(2) 1 d PU F 1 H4A H 0.5647 -0.2447 0.9390 0.113 Uiso 0.63(2) 1 calc PR F 1 H4B H 0.5265 -0.2131 0.8794 0.113 Uiso 0.63(2) 1 calc PR F 1 H4C H 0.5329 -0.3019 0.8901 0.113 Uiso 0.63(2) 1 calc PR F 1 C5 C 0.4992(7) -0.3236(14) 0.9645(10) 0.097(9) Uani 0.63(2) 1 d P F 1 H5A H 0.5315 -0.3231 0.9967 0.146 Uiso 0.63(2) 1 calc PR F 1 H5B H 0.4959 -0.3694 0.9425 0.146 Uiso 0.63(2) 1 calc PR F 1 H5C H 0.4732 -0.3226 0.9776 0.146 Uiso 0.63(2) 1 calc PR F 1 C6 C 0.3961(3) -0.2446(5) 0.9493(3) 0.044(2) Uani 1 1 d . . . H6 H 0.4294 -0.2479 0.9815 0.053 Uiso 1 1 calc R . . C7 C 0.3654(5) -0.3112(7) 0.9500(5) 0.080(4) Uani 1 1 d . . . H7A H 0.3834 -0.3581 0.9506 0.096 Uiso 1 1 calc R . . H7B H 0.3342 -0.3111 0.9154 0.096 Uiso 1 1 calc R . . C8 C 0.3536(6) -0.3095(8) 1.0015(6) 0.092(4) Uani 1 1 d . . . H8A H 0.3330 -0.3537 1.0000 0.111 Uiso 1 1 calc R . . H8B H 0.3848 -0.3137 1.0359 0.111 Uiso 1 1 calc R . . C9 C 0.3282(6) -0.2421(9) 1.0050(6) 0.094(5) Uani 1 1 d . . . H9A H 0.3230 -0.2431 1.0395 0.113 Uiso 1 1 calc R . . H9B H 0.2956 -0.2393 0.9724 0.113 Uiso 1 1 calc R . . C10 C 0.3587(6) -0.1750(9) 1.0056(6) 0.103(4) Uani 1 1 d U . . H10A H 0.3899 -0.1759 1.0402 0.123 Uiso 1 1 calc R . . H10B H 0.3407 -0.1286 1.0060 0.123 Uiso 1 1 calc R . . C11 C 0.3706(6) -0.1738(6) 0.9541(5) 0.091(5) Uani 1 1 d . . . H11A H 0.3396 -0.1676 0.9198 0.110 Uiso 1 1 calc R . . H11B H 0.3919 -0.1300 0.9570 0.110 Uiso 1 1 calc R . . C12 C 0.4470(3) -0.2504(6) 0.7890(3) 0.048(2) Uani 1 1 d . . . H12 H 0.4830 -0.2600 0.8113 0.058 Uiso 1 1 calc R . . C13 C 0.4411(7) -0.1790(11) 0.7606(7) 0.122(5) Uani 1 1 d U . . H13A H 0.4604 -0.1404 0.7884 0.146 Uiso 1 1 calc R . . H13B H 0.4060 -0.1642 0.7450 0.146 Uiso 1 1 calc R . . C14 C 0.4579(8) -0.1795(12) 0.7124(8) 0.130(6) Uani 1 1 d U . . H14A H 0.4464 -0.1324 0.6906 0.156 Uiso 1 1 calc R . . H14B H 0.4943 -0.1795 0.7291 0.156 Uiso 1 1 calc R . . C15 C 0.4406(4) -0.2407(9) 0.6756(5) 0.082(4) Uani 1 1 d . . . H15A H 0.4590 -0.2427 0.6523 0.098 Uiso 1 1 calc R . . H15B H 0.4054 -0.2320 0.6502 0.098 Uiso 1 1 calc R . . C16 C 0.4450(7) -0.3119(10) 0.7025(7) 0.112(5) Uani 1 1 d U . . H16A H 0.4801 -0.3272 0.7193 0.134 Uiso 1 1 calc R . . H16B H 0.4263 -0.3498 0.6739 0.134 Uiso 1 1 calc R . . C17 C 0.4261(7) -0.3124(10) 0.7492(6) 0.106(5) Uani 1 1 d U . . H17A H 0.3898 -0.3084 0.7316 0.127 Uiso 1 1 calc R . . H17B H 0.4351 -0.3608 0.7696 0.127 Uiso 1 1 calc R . . C18 C 0.3355(4) -0.0589(6) 0.7520(6) 0.074(3) Uani 1 1 d . . . H18 H 0.3519 -0.0648 0.7284 0.089 Uiso 1 1 calc R . . C19 C 0.2856(4) -0.0365(6) 0.7349(5) 0.069(3) Uani 1 1 d . . . H19 H 0.2625 -0.0258 0.6976 0.083 Uiso 1 1 calc R . . C20 C 0.2769(5) -0.0332(6) 0.7812(5) 0.076(3) Uani 1 1 d . . . H20 H 0.2467 -0.0187 0.7819 0.091 Uiso 1 1 calc R . . C21 C 0.3204(5) -0.0548(6) 0.8285(5) 0.079(4) Uani 1 1 d . . . H21 H 0.3242 -0.0577 0.8660 0.095 Uiso 1 1 calc R . . C22 C 0.3563(5) -0.0707(6) 0.8106(5) 0.074(3) Uani 1 1 d . . . H22 H 0.3890 -0.0867 0.8335 0.088 Uiso 1 1 calc R . . C23 C 0.2769(4) -0.1940(6) 0.7072(4) 0.057(3) Uani 1 1 d . . . C24 C 0.2555(4) -0.1892(6) 0.7941(5) 0.060(3) Uani 1 1 d . . . C25 C 0.2834(3) -0.3674(5) 0.7623(4) 0.050(2) Uani 1 1 d . . . H25A H 0.2611 -0.3234 0.7511 0.060 Uiso 1 1 calc R . . H25B H 0.2690 -0.4060 0.7780 0.060 Uiso 1 1 calc R . . C26 C 0.2887(6) -0.3982(10) 0.7128(6) 0.109(5) Uani 1 1 d . . . H26A H 0.3098 -0.3649 0.7031 0.164 Uiso 1 1 calc R . . H26B H 0.2562 -0.4016 0.6810 0.164 Uiso 1 1 calc R . . H26C H 0.3036 -0.4483 0.7217 0.164 Uiso 1 1 calc R . . C27 C 0.3673(3) -0.4061(5) 0.8273(5) 0.060(3) Uani 1 1 d . . . H27A H 0.3983 -0.3858 0.8566 0.072 Uiso 1 1 calc R . . H27B H 0.3747 -0.4283 0.7974 0.072 Uiso 1 1 calc R . . C28 C 0.3462(5) -0.4684(8) 0.8532(7) 0.101(5) Uani 1 1 d . . . H28A H 0.3329 -0.4447 0.8774 0.151 Uiso 1 1 calc R . . H28B H 0.3726 -0.5033 0.8754 0.151 Uiso 1 1 calc R . . H28C H 0.3199 -0.4960 0.8230 0.151 Uiso 1 1 calc R . . C29 C 0.1398(3) 0.2439(6) 0.8918(4) 0.050(2) Uani 1 1 d . G . C30 C 0.1668(4) 0.2527(7) 0.8547(5) 0.070(3) Uani 1 1 d . . . C31 C 0.1972(12) 0.3250(19) 0.8744(11) 0.119(13) Uani 0.58(2) 1 d P G 1 H31A H 0.2323 0.3124 0.8930 0.179 Uiso 0.58(2) 1 calc PR G 1 H31B H 0.1877 0.3515 0.9008 0.179 Uiso 0.58(2) 1 calc PR G 1 H31C H 0.1910 0.3574 0.8421 0.179 Uiso 0.58(2) 1 calc PR G 1 C32 C 0.1427(11) 0.2507(18) 0.7968(12) 0.097(9) Uani 0.58(2) 1 d PU G 1 H32A H 0.1575 0.2877 0.7810 0.146 Uiso 0.58(2) 1 calc PR G 1 H32B H 0.1078 0.2626 0.7848 0.146 Uiso 0.58(2) 1 calc PR G 1 H32C H 0.1457 0.2003 0.7835 0.146 Uiso 0.58(2) 1 calc PR G 1 C33 C 0.2105(8) 0.1932(14) 0.8732(9) 0.074(6) Uani 0.58(2) 1 d PU G 1 H33A H 0.2337 0.2080 0.8580 0.111 Uiso 0.58(2) 1 calc PR G 1 H33B H 0.1970 0.1433 0.8590 0.111 Uiso 0.58(2) 1 calc PR G 1 H33C H 0.2276 0.1916 0.9142 0.111 Uiso 0.58(2) 1 calc PR G 1 C34 C 0.2117(3) 0.2439(6) 0.9915(4) 0.055(2) Uani 1 1 d . . . H34 H 0.2351 0.2503 0.9740 0.066 Uiso 1 1 calc R . . C35 C 0.2147(4) 0.3120(6) 1.0293(5) 0.076(3) Uani 1 1 d . . . H35A H 0.1883 0.3087 1.0421 0.091 Uiso 1 1 calc R . . H35B H 0.2102 0.3592 1.0079 0.091 Uiso 1 1 calc R . . C36 C 0.2659(6) 0.3123(9) 1.0808(6) 0.111(5) Uani 1 1 d . . . H36A H 0.2915 0.3243 1.0677 0.133 Uiso 1 1 calc R . . H36B H 0.2663 0.3527 1.1067 0.133 Uiso 1 1 calc R . . C37 C 0.2789(6) 0.2415(8) 1.1116(5) 0.102(5) Uani 1 1 d . . . H37A H 0.3132 0.2448 1.1407 0.123 Uiso 1 1 calc R . . H37B H 0.2572 0.2342 1.1308 0.123 Uiso 1 1 calc R . . C38 C 0.2744(4) 0.1774(8) 1.0767(5) 0.079(4) Uani 1 1 d . . . H38A H 0.2795 0.1309 1.0992 0.095 Uiso 1 1 calc R . . H38B H 0.3004 0.1796 1.0631 0.095 Uiso 1 1 calc R . . C39 C 0.2235(4) 0.1744(7) 1.0262(5) 0.079(4) Uani 1 1 d . . . H39A H 0.2226 0.1308 1.0024 0.095 Uiso 1 1 calc R . . H39B H 0.1980 0.1664 1.0399 0.095 Uiso 1 1 calc R . . C40 C 0.0490(4) 0.2391(8) 0.8188(4) 0.072(3) Uani 1 1 d . . . H40 H 0.0611 0.2418 0.7889 0.086 Uiso 1 1 calc R . . C41 C 0.0171(5) 0.3119(10) 0.8166(7) 0.126(7) Uani 1 1 d . . . H41A H 0.0360 0.3583 0.8185 0.151 Uiso 1 1 calc R . . H41B H 0.0077 0.3118 0.8483 0.151 Uiso 1 1 calc R . . C42 C -0.0309(7) 0.3071(11) 0.7581(7) 0.125(6) Uani 1 1 d U . . H42A H -0.0535 0.3486 0.7562 0.150 Uiso 1 1 calc R . . H42B H -0.0209 0.3142 0.7272 0.150 Uiso 1 1 calc R . . C43 C -0.0564(6) 0.2380(10) 0.7501(7) 0.106(5) Uani 1 1 d U . . H43A H -0.0691 0.2339 0.7790 0.128 Uiso 1 1 calc R . . H43B H -0.0853 0.2397 0.7132 0.128 Uiso 1 1 calc R . . C44 C -0.0297(6) 0.1729(11) 0.7522(7) 0.111(5) Uani 1 1 d U . . H44A H -0.0194 0.1732 0.7212 0.133 Uiso 1 1 calc R . . H44B H -0.0505 0.1280 0.7478 0.133 Uiso 1 1 calc R . . C45 C 0.0174(6) 0.1698(11) 0.8107(7) 0.120(6) Uani 1 1 d . . . H45A H 0.0068 0.1666 0.8414 0.144 Uiso 1 1 calc R . . H45B H 0.0370 0.1243 0.8123 0.144 Uiso 1 1 calc R . . C46 C 0.0538(7) 0.0019(7) 0.9750(8) 0.109(6) Uani 1 1 d . . . H46 H 0.0226 -0.0173 0.9696 0.131 Uiso 1 1 calc R . . C47 C 0.0942(7) 0.0069(10) 1.0253(8) 0.110(5) Uani 1 1 d U . . H47 H 0.0958 -0.0055 1.0610 0.132 Uiso 1 1 calc R . . C48 C 0.1315(6) 0.0331(8) 1.0142(8) 0.103(5) Uani 1 1 d . . . H48 H 0.1644 0.0393 1.0417 0.123 Uiso 1 1 calc R . . C49 C 0.1168(6) 0.0491(7) 0.9603(7) 0.087(4) Uani 1 1 d . . . H49 H 0.1369 0.0695 0.9440 0.105 Uiso 1 1 calc R . . C50 C 0.0663(7) 0.0308(8) 0.9310(7) 0.109(5) Uani 1 1 d . . . H50 H 0.0455 0.0360 0.8922 0.131 Uiso 1 1 calc R . . C51 C 0.0993(4) 0.1656(7) 1.0515(4) 0.065(3) Uani 1 1 d . . . C52 C 0.0164(5) 0.1489(7) 0.9693(5) 0.071(3) Uani 1 1 d . . . C53 C 0.0954(5) 0.3918(6) 0.9519(5) 0.072(3) Uani 1 1 d . . . H53A H 0.1190 0.3795 0.9361 0.087 Uiso 1 1 calc R . . H53B H 0.0654 0.4129 0.9215 0.087 Uiso 1 1 calc R . . C54 C 0.1175(5) 0.4486(7) 0.9970(7) 0.094(4) Uani 1 1 d . . . H54A H 0.0912 0.4758 1.0020 0.141 Uiso 1 1 calc R . . H54B H 0.1372 0.4842 0.9868 0.141 Uiso 1 1 calc R . . H54C H 0.1387 0.4233 1.0321 0.141 Uiso 1 1 calc R . . C55 C 0.0511(5) 0.3311(9) 1.0011(5) 0.091(4) Uani 1 1 d . . . H55A H 0.0658 0.3687 1.0315 0.109 Uiso 1 1 calc R . . H55B H 0.0483 0.2829 1.0182 0.109 Uiso 1 1 calc R . . C56 C 0.0026(7) 0.3560(12) 0.9623(10) 0.155(8) Uani 1 1 d . . . H56A H 0.0052 0.4046 0.9463 0.232 Uiso 1 1 calc R . . H56B H -0.0184 0.3611 0.9821 0.232 Uiso 1 1 calc R . . H56C H -0.0119 0.3189 0.9321 0.232 Uiso 1 1 calc R . . C57 C 0.3066(3) 0.2550(4) 0.7722(3) 0.0390(19) Uani 1 1 d . . . C58 C 0.2766(3) 0.1936(5) 0.7491(4) 0.051(2) Uani 1 1 d . . . H58 H 0.2910 0.1449 0.7559 0.061 Uiso 1 1 calc R . . C59 C 0.2259(3) 0.2005(5) 0.7161(4) 0.048(2) Uani 1 1 d . . . C60 C 0.2039(3) 0.2714(4) 0.7049(3) 0.0381(18) Uani 1 1 d . . . H60 H 0.1694 0.2766 0.6832 0.046 Uiso 1 1 calc R . . C61 C 0.2332(3) 0.3335(4) 0.7259(3) 0.0332(17) Uani 1 1 d . A . C62 C 0.2836(3) 0.3252(4) 0.7595(3) 0.0326(16) Uani 1 1 d . . . H62 H 0.3030 0.3689 0.7743 0.039 Uiso 1 1 calc R . . C63 C 0.1948(3) 0.1323(6) 0.6926(5) 0.064(3) Uani 1 1 d . . . C64 C 0.2120(3) 0.4094(5) 0.7113(4) 0.045(2) Uani 1 1 d . . . C65 C 0.3979(3) 0.3224(6) 0.8127(4) 0.031(2) Uani 0.751(7) 1 d P B 3 C66 C 0.4361(7) 0.3547(13) 0.8595(8) 0.032(4) Uani 0.751(7) 1 d P B 3 H66 H 0.4431 0.3353 0.8956 0.039 Uiso 1 1 calc R B 3 C67 C 0.4646(4) 0.4146(6) 0.8548(4) 0.036(2) Uani 0.751(7) 1 d P B 3 C68 C 0.4544(4) 0.4463(7) 0.8033(4) 0.041(3) Uani 0.751(7) 1 d P B 3 H68 H 0.4727 0.4882 0.8002 0.049 Uiso 1 1 calc R B 3 C69 C 0.4167(4) 0.4152(6) 0.7560(4) 0.037(2) Uani 0.751(7) 1 d P B 3 C70 C 0.3894(4) 0.3544(6) 0.7606(4) 0.031(2) Uani 0.751(7) 1 d P B 3 H70 H 0.3643 0.3338 0.7275 0.037 Uiso 1 1 calc R B 3 C71 C 0.5017(4) 0.4462(7) 0.9064(4) 0.062(3) Uani 1 1 d . . . C72 C 0.4054(5) 0.4442(8) 0.6974(6) 0.077(3) Uani 1 1 d . . . C73 C 0.3614(3) 0.2447(6) 0.8757(4) 0.029(2) Uani 0.751(7) 1 d P C 3 C74 C 0.3549(4) 0.1802(8) 0.8990(5) 0.041(3) Uani 0.751(7) 1 d P C 3 H74 H 0.3555 0.1347 0.8805 0.049 Uiso 1 1 calc R C 3 C75 C 0.3474(4) 0.1738(6) 0.9468(4) 0.035(2) Uani 0.751(7) 1 d P C 3 C76 C 0.3445(4) 0.2376(6) 0.9734(4) 0.038(3) Uani 0.751(7) 1 d P C 3 H76 H 0.3394 0.2353 1.0065 0.046 Uiso 1 1 calc R C 3 C77 C 0.3493(3) 0.3072(6) 0.9510(4) 0.033(2) Uani 0.751(7) 1 d P C 3 C78 C 0.3581(3) 0.3099(6) 0.9038(4) 0.030(2) Uani 0.751(7) 1 d PU C 3 H78 H 0.3621 0.3575 0.8899 0.036 Uiso 1 1 calc R C 3 C79 C 0.3418(4) 0.1003(8) 0.9690(5) 0.074(3) Uani 1 1 d U . . C80 C 0.3454(4) 0.3807(6) 0.9796(4) 0.054(2) Uani 1 1 d . . . C81 C 0.3950(3) 0.1766(6) 0.8074(4) 0.031(2) Uani 0.751(7) 1 d P B 3 C82 C 0.3881(4) 0.1495(8) 0.7552(5) 0.035(3) Uani 0.751(7) 1 d P B 3 H82 H 0.3618 0.1698 0.7231 0.042 Uiso 1 1 calc R B 3 C83 C 0.4177(4) 0.0941(6) 0.7472(4) 0.037(2) Uani 0.751(7) 1 d P B 3 C84 C 0.4530(4) 0.0584(7) 0.7918(4) 0.043(3) Uani 0.751(7) 1 d P B 3 H84 H 0.4715 0.0182 0.7866 0.052 Uiso 1 1 calc R B 3 C85 C 0.4615(4) 0.0827(6) 0.8466(4) 0.041(3) Uani 0.751(7) 1 d P B 3 C86 C 0.4340(4) 0.1404(7) 0.8526(5) 0.036(3) Uani 0.751(7) 1 d P B 3 H86 H 0.4415 0.1575 0.8894 0.043 Uiso 1 1 calc R B 3 C87 C 0.4115(4) 0.0763(7) 0.6896(5) 0.070(3) Uani 1 1 d U . . C88 C 0.4994(5) 0.0460(8) 0.8954(5) 0.080(3) Uani 1 1 d U . . C89 C 0.1372(2) -0.2602(4) 1.0478(3) 0.0293(15) Uani 1 1 d . . . C90 C 0.1368(3) -0.1953(4) 1.0779(3) 0.0307(16) Uani 1 1 d . . . H90 H 0.1373 -0.1474 1.0621 0.037 Uiso 1 1 calc R . . C91 C 0.1356(3) -0.1988(4) 1.1304(3) 0.0322(16) Uani 1 1 d . . . C92 C 0.1337(3) -0.2668(5) 1.1539(4) 0.0408(19) Uani 1 1 d . . . H92 H 0.1334 -0.2693 1.1897 0.049 Uiso 1 1 calc R . . C93 C 0.1324(3) -0.3319(5) 1.1243(3) 0.0382(18) Uani 1 1 d . . . C94 C 0.1342(3) -0.3284(4) 1.0728(3) 0.0361(17) Uani 1 1 d . . . H94 H 0.1335 -0.3741 1.0538 0.043 Uiso 1 1 calc R . . C95 C 0.1354(3) -0.1276(5) 1.1601(4) 0.045(2) Uani 1 1 d . . . C96 C 0.1291(4) -0.4046(5) 1.1488(4) 0.051(2) Uani 1 1 d . . . C97 C 0.1712(3) -0.3270(4) 0.9790(3) 0.0309(16) Uani 1 1 d . . . C98 C 0.1640(4) -0.3530(5) 0.9257(4) 0.054(2) Uani 1 1 d . . . H98 H 0.1377 -0.3331 0.8934 0.065 Uiso 1 1 calc R . . C99 C 0.1946(4) -0.4071(6) 0.9193(3) 0.061(3) Uani 1 1 d . E . C100 C 0.2324(4) -0.4384(6) 0.9648(4) 0.059(3) Uani 1 1 d . . . H100 H 0.2521 -0.4776 0.9606 0.071 Uiso 1 1 calc R . . C101 C 0.2409(3) -0.4110(5) 1.0166(3) 0.0392(18) Uani 1 1 d . . . C102 C 0.2117(3) -0.3576(4) 1.0237(3) 0.0329(16) Uani 1 1 d . . . H102 H 0.2192 -0.3404 1.0606 0.039 Uiso 1 1 calc R . . F31A F 0.2241(10) -0.3910(15) 0.8453(10) 0.134(10) Uani 0.43(2) 1 d PU E 2 C104 C 0.2837(4) -0.4439(6) 1.0681(4) 0.052(2) Uani 1 1 d . . . C105 C 0.0799(3) -0.2629(5) 0.9401(3) 0.0391(18) Uani 1 1 d . . . C106 C 0.0573(3) -0.3331(5) 0.9231(4) 0.053(2) Uani 1 1 d . . . H106 H 0.0763 -0.3775 0.9368 0.063 Uiso 1 1 calc R . . C107 C 0.0072(3) -0.3392(6) 0.8862(5) 0.064(3) Uani 1 1 d . . . C108 C -0.0212(3) -0.2770(6) 0.8650(4) 0.056(2) Uani 1 1 d . . . H108 H -0.0550 -0.2817 0.8398 0.067 Uiso 1 1 calc R . . C109 C 0.0000(3) -0.2072(5) 0.8804(3) 0.044(2) Uani 1 1 d . . . C110 C 0.0500(3) -0.1996(5) 0.9186(3) 0.0361(17) Uani 1 1 d . . . H110 H 0.0635 -0.1508 0.9298 0.043 Uiso 1 1 calc R . . C111 C -0.0147(4) -0.4152(8) 0.8686(7) 0.093(5) Uani 1 1 d . . . C112 C -0.0294(3) -0.1378(7) 0.8569(4) 0.059(3) Uani 1 1 d . . . C113 C 0.1660(3) -0.1820(4) 0.9774(3) 0.0327(16) Uani 1 1 d . . . C114 C 0.1544(3) -0.1516(5) 0.9244(4) 0.0410(19) Uani 1 1 d . . . H114 H 0.1276 -0.1723 0.8928 0.049 Uiso 1 1 calc R . . C115 C 0.1807(3) -0.0919(5) 0.9163(4) 0.046(2) Uani 1 1 d . . . C116 C 0.2212(3) -0.0631(5) 0.9621(4) 0.047(2) Uani 1 1 d . . . H116 H 0.2397 -0.0226 0.9572 0.056 Uiso 1 1 calc R . . C117 C 0.2340(3) -0.0930(5) 1.0135(4) 0.043(2) Uani 1 1 d . . . C118 C 0.2075(3) -0.1518(5) 1.0218(3) 0.0363(17) Uani 1 1 d . . . H118 H 0.2176 -0.1720 1.0584 0.044 Uiso 1 1 calc R . . C119 C 0.1671(4) -0.0612(6) 0.8604(5) 0.061(3) Uani 1 1 d . . . C120 C 0.2762(4) -0.0610(5) 1.0644(4) 0.055(2) Uani 1 1 d . . . B1 B 0.3651(3) 0.2485(5) 0.8155(3) 0.0302(18) Uani 1 1 d . . . B2 B 0.1382(3) -0.2573(5) 0.9863(4) 0.0340(19) Uani 1 1 d . . . C4A C 0.5156(14) -0.326(2) 0.9120(16) 0.091(12) Uani 0.37(2) 1 d PU F 2 H4A1 H 0.5514 -0.3279 0.9341 0.136 Uiso 0.37(2) 1 calc PR F 2 H4A2 H 0.5079 -0.3266 0.8720 0.136 Uiso 0.37(2) 1 calc PR F 2 H4A3 H 0.5007 -0.3706 0.9208 0.136 Uiso 0.37(2) 1 calc PR F 2 C5A C 0.5110(11) -0.248(2) 0.9846(9) 0.066(11) Uani 0.37(2) 1 d P F 2 H5A1 H 0.4968 -0.2043 0.9943 0.099 Uiso 0.37(2) 1 calc PR F 2 H5A2 H 0.5471 -0.2443 1.0021 0.099 Uiso 0.37(2) 1 calc PR F 2 H5A3 H 0.5012 -0.2940 0.9980 0.099 Uiso 0.37(2) 1 calc PR F 2 C3A C 0.5252(15) -0.190(3) 0.9107(17) 0.097(13) Uani 0.37(2) 1 d PU F 2 H3A1 H 0.5182 -0.1401 0.9211 0.145 Uiso 0.37(2) 1 calc PR F 2 H3A2 H 0.5156 -0.1918 0.8703 0.145 Uiso 0.37(2) 1 calc PR F 2 H3A3 H 0.5604 -0.2009 0.9310 0.145 Uiso 0.37(2) 1 calc PR F 2 C31A C 0.1455(11) 0.3310(17) 0.8198(12) 0.072(9) Uani 0.42(2) 1 d PU G 2 H31D H 0.1595 0.3741 0.8447 0.109 Uiso 0.42(2) 1 calc PR G 2 H31E H 0.1095 0.3320 0.8053 0.109 Uiso 0.42(2) 1 calc PR G 2 H31F H 0.1547 0.3338 0.7885 0.109 Uiso 0.42(2) 1 calc PR G 2 C33A C 0.2160(12) 0.258(2) 0.8770(14) 0.080(9) Uani 0.42(2) 1 d PU G 2 H33D H 0.2267 0.2661 0.8471 0.120 Uiso 0.42(2) 1 calc PR G 2 H33E H 0.2306 0.2112 0.8969 0.120 Uiso 0.42(2) 1 calc PR G 2 H33F H 0.2269 0.3002 0.9033 0.120 Uiso 0.42(2) 1 calc PR G 2 C32A C 0.1420(12) 0.196(2) 0.8017(12) 0.081(11) Uani 0.42(2) 1 d P G 2 H32D H 0.1256 0.2253 0.7672 0.122 Uiso 0.42(2) 1 calc PR G 2 H32E H 0.1178 0.1639 0.8070 0.122 Uiso 0.42(2) 1 calc PR G 2 H32F H 0.1676 0.1645 0.7989 0.122 Uiso 0.42(2) 1 calc PR G 2 F12A F 0.3684(6) 0.4248(10) 0.6614(6) 0.078(5) Uani 0.494(16) 1 d PU B 2 F10A F 0.3940(12) 0.5202(17) 0.6956(12) 0.168(10) Uani 0.494(16) 1 d PU B 2 F5A F 0.1910(14) 0.4389(19) 0.7416(14) 0.107(11) Uani 0.276(13) 1 d PU A 2 F11A F 0.4451(7) 0.4162(11) 0.6872(7) 0.105(6) Uani 0.494(16) 1 d PU B 2 F6A F 0.1699(8) 0.4101(12) 0.6623(11) 0.067(7) Uani 0.276(13) 1 d PU A 2 F7A F 0.2407(7) 0.4589(10) 0.7056(9) 0.052(6) Uani 0.276(13) 1 d PU A 2 F14A F 0.3120(12) 0.0973(17) 0.9902(14) 0.138(12) Uani 0.38(2) 1 d PU C 2 F22A F 0.4864(10) -0.0261(14) 0.8890(10) 0.132(9) Uani 0.46(2) 1 d PU D 2 F23A F 0.5422(9) 0.0413(16) 0.8931(10) 0.129(9) Uani 0.46(2) 1 d PU D 2 F24A F 0.5071(9) 0.0588(14) 0.9442(9) 0.111(7) Uani 0.46(2) 1 d PU D 2 F15A F 0.3081(7) 0.0465(11) 0.9266(8) 0.071(6) Uani 0.38(2) 1 d PU C 2 F13A F 0.3764(11) 0.052(2) 1.0034(15) 0.142(11) Uani 0.38(2) 1 d PU C 2 C103 C 0.1822(9) -0.4335(12) 0.8582(8) 0.127(7) Uani 1 1 d . . . F31 F 0.1677(7) -0.3758(11) 0.8231(6) 0.101(6) Uani 0.57(2) 1 d PU E 1 F33A F 0.1473(5) -0.4180(10) 0.8229(5) 0.056(5) Uani 0.43(2) 1 d PU E 2 F32 F 0.2207(7) -0.4733(11) 0.8591(6) 0.096(5) Uani 0.57(2) 1 d PU E 1 F32A F 0.1995(7) -0.4969(9) 0.8576(6) 0.058(5) Uani 0.43(2) 1 d PU E 2 C65A C 0.3816(10) 0.2440(15) 0.7644(11) 0.025(6) Uiso 0.249(7) 1 d P B 4 C69A C 0.3978(10) 0.1762(15) 0.6952(11) 0.025(6) Uiso 0.249(7) 1 d P B 4 C68A C 0.4025(13) 0.241(2) 0.6720(15) 0.045(8) Uiso 0.249(7) 1 d P B 4 C67A C 0.3983(10) 0.3104(16) 0.6933(11) 0.026(6) Uiso 0.249(7) 1 d P B 4 C66A C 0.3893(10) 0.3143(17) 0.7409(11) 0.022(6) Uiso 0.249(7) 1 d P B 4 C70A C 0.3848(12) 0.1749(18) 0.7423(13) 0.015(8) Uiso 0.249(7) 1 d P B 4 C73A C 0.3870(9) 0.3238(14) 0.8583(10) 0.019(5) Uiso 0.249(7) 1 d P B 4 C75A C 0.3814(9) 0.4102(14) 0.9252(10) 0.021(6) Uiso 0.249(7) 1 d P B 4 C77A C 0.4525(11) 0.4119(17) 0.9046(12) 0.034(7) Uiso 0.249(7) 1 d P B 4 C76A C 0.4278(12) 0.4374(18) 0.9373(13) 0.038(7) Uiso 0.249(7) 1 d P B 4 C74A C 0.3620(11) 0.3521(19) 0.8863(13) 0.033(7) Uiso 0.249(7) 1 d P B 4 C78A C 0.431(3) 0.346(4) 0.867(3) 0.028(16) Uiso 0.249(7) 1 d P B 4 C81A C 0.3816(9) 0.1744(14) 0.8581(10) 0.018(5) Uiso 0.249(7) 1 d P B 4 C83A C 0.3755(10) 0.0934(15) 0.9283(11) 0.025(6) Uiso 0.249(7) 1 d P B 4 C84A C 0.4202(12) 0.0589(19) 0.9384(13) 0.039(7) Uiso 0.249(7) 1 d P B 4 C85A C 0.4448(11) 0.0836(18) 0.9077(13) 0.036(7) Uiso 0.249(7) 1 d P B 4 C82A C 0.3577(10) 0.1535(16) 0.8899(11) 0.005(6) Uiso 0.249(7) 1 d P B 4 C86A C 0.4265(13) 0.139(2) 0.8677(15) 0.022(9) Uiso 0.249(7) 1 d P B 4 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 0.0313(4) 0.0348(5) 0.0337(4) 0.0026(4) 0.0146(4) 0.0020(3) Ga2 0.0380(5) 0.0578(6) 0.0423(5) -0.0001(4) 0.0224(4) -0.0003(4) Fe1 0.0445(7) 0.0406(7) 0.0557(8) 0.0139(6) 0.0217(6) 0.0074(6) Fe2 0.0548(8) 0.0514(8) 0.0587(8) -0.0043(6) 0.0330(7) -0.0064(6) F1 0.095(4) 0.055(3) 0.086(4) -0.026(3) 0.018(3) -0.015(3) F2 0.070(3) 0.048(3) 0.113(4) 0.005(3) 0.031(3) -0.014(3) F3 0.061(3) 0.055(3) 0.136(5) 0.001(3) -0.019(3) -0.006(3) F4 0.110(6) 0.057(5) 0.083(5) 0.029(4) 0.048(4) 0.024(4) F5 0.059(4) 0.036(4) 0.076(5) -0.016(3) 0.000(3) 0.004(3) F6 0.036(4) 0.048(4) 0.096(6) 0.003(4) 0.024(3) 0.005(3) F7 0.173(6) 0.147(6) 0.126(5) -0.031(5) 0.067(5) -0.014(5) F8 0.097(5) 0.138(6) 0.163(6) -0.015(5) 0.021(4) -0.012(5) F9 0.183(6) 0.161(6) 0.125(5) 0.008(5) 0.068(5) -0.063(5) F10 0.090(7) 0.093(7) 0.072(6) 0.028(5) 0.028(5) -0.037(5) F11 0.089(7) 0.065(6) 0.039(5) -0.002(4) 0.034(4) 0.010(5) F12 0.089(7) 0.107(8) 0.086(7) 0.023(5) 0.038(5) 0.009(6) F13 0.132(8) 0.083(7) 0.095(7) 0.010(5) 0.058(5) 0.000(5) F14 0.096(7) 0.071(6) 0.079(6) 0.006(4) 0.036(5) 0.001(4) F15 0.113(7) 0.110(8) 0.124(8) 0.019(6) 0.044(6) -0.024(5) F16 0.144(6) 0.136(6) 0.170(6) -0.059(5) 0.036(5) 0.036(5) F17 0.137(6) 0.126(6) 0.170(6) -0.023(5) 0.086(5) -0.020(5) F18 0.214(7) 0.157(7) 0.155(6) -0.025(5) 0.082(5) 0.020(5) F19 0.148(6) 0.199(7) 0.113(5) -0.047(5) 0.051(5) 0.058(5) F20 0.139(5) 0.152(6) 0.128(5) -0.025(4) 0.089(5) -0.016(5) F21 0.206(7) 0.164(7) 0.134(6) -0.013(5) 0.078(5) -0.018(5) F22 0.097(7) 0.099(7) 0.085(7) -0.002(5) 0.041(5) 0.030(5) F23 0.077(7) 0.087(7) 0.099(7) 0.010(5) 0.017(5) 0.014(5) F24 0.106(8) 0.120(8) 0.101(8) 0.015(6) 0.052(6) 0.019(6) F25 0.224(6) 0.085(5) 0.120(5) 0.023(4) 0.107(5) -0.015(4) F26 0.117(5) 0.093(5) 0.161(6) 0.032(4) 0.082(4) -0.009(4) F27 0.142(6) 0.096(5) 0.128(5) 0.044(4) 0.023(4) -0.027(4) F28 0.085(4) 0.094(4) 0.122(5) -0.039(4) 0.038(4) 0.023(3) F29 0.135(5) 0.092(4) 0.070(4) -0.024(3) 0.028(4) 0.013(4) F30 0.135(5) 0.071(4) 0.122(5) -0.038(3) 0.082(4) -0.027(4) F33 0.157(11) 0.150(11) 0.151(11) -0.027(6) 0.049(7) 0.011(6) F34 0.068(3) 0.075(4) 0.065(3) -0.007(3) 0.004(3) 0.017(3) F35 0.088(4) 0.098(4) 0.084(4) 0.044(3) 0.041(3) 0.018(3) F36 0.079(4) 0.090(4) 0.064(3) 0.007(3) 0.028(3) 0.049(3) F37 0.178(7) 0.134(6) 0.178(7) 0.000(5) 0.074(5) -0.054(5) F38 0.105(5) 0.086(4) 0.144(5) -0.035(4) 0.032(4) -0.013(4) F39 0.097(5) 0.111(5) 0.152(6) -0.018(5) 0.000(4) -0.024(4) F40 0.080(4) 0.080(4) 0.072(3) 0.026(3) 0.032(3) 0.020(3) F41 0.080(4) 0.097(4) 0.075(4) -0.003(3) 0.036(3) 0.029(3) F42 0.059(3) 0.098(4) 0.081(4) 0.007(3) 0.004(3) 0.020(3) F43 0.073(3) 0.084(4) 0.091(4) -0.017(3) 0.037(3) -0.042(3) F44 0.051(3) 0.064(3) 0.070(3) -0.008(3) 0.011(3) -0.001(3) F45 0.070(3) 0.063(3) 0.078(3) -0.025(3) 0.030(3) -0.001(3) F46 0.125(5) 0.109(5) 0.075(4) 0.004(4) 0.040(4) -0.017(4) F47 0.179(6) 0.154(6) 0.111(5) 0.038(4) 0.083(5) 0.056(5) F48 0.125(5) 0.154(6) 0.099(4) 0.020(4) 0.063(4) -0.040(4) O1 0.043(3) 0.035(3) 0.068(4) -0.006(3) 0.007(3) -0.003(3) O2 0.074(5) 0.090(6) 0.040(4) 0.005(4) 0.007(3) -0.012(4) O3 0.073(5) 0.086(6) 0.115(7) 0.008(5) 0.067(5) 0.004(4) O4 0.080(5) 0.056(4) 0.101(6) 0.004(4) 0.062(5) 0.005(4) O5 0.100(7) 0.155(10) 0.038(4) -0.017(5) -0.008(4) -0.009(7) O6 0.029(4) 0.181(11) 0.132(8) -0.026(8) 0.022(5) 0.000(5) N1 0.048(4) 0.033(4) 0.034(3) 0.004(3) 0.016(3) 0.003(3) N2 0.030(3) 0.062(5) 0.037(4) -0.002(3) 0.019(3) 0.001(3) N3 0.034(4) 0.063(5) 0.042(4) 0.003(3) 0.021(3) 0.000(3) N4 0.047(4) 0.084(6) 0.043(4) 0.013(4) 0.021(4) -0.008(4) C1 0.036(4) 0.030(4) 0.037(4) 0.000(3) 0.015(3) -0.003(3) C2 0.040(5) 0.069(7) 0.047(5) 0.000(5) 0.003(4) -0.005(4) C3 0.066(11) 0.070(14) 0.066(11) -0.015(10) 0.014(9) -0.018(9) C4 0.069(8) 0.090(9) 0.073(8) -0.007(6) 0.035(6) 0.008(6) C5 0.059(12) 0.100(18) 0.101(17) 0.037(14) 0.004(11) 0.030(12) C6 0.042(5) 0.053(5) 0.036(4) 0.003(4) 0.016(4) 0.005(4) C7 0.115(10) 0.062(7) 0.092(9) -0.005(6) 0.072(8) -0.012(7) C8 0.138(12) 0.091(9) 0.096(9) -0.007(8) 0.096(10) -0.016(9) C9 0.101(10) 0.146(14) 0.065(7) 0.008(8) 0.063(8) 0.020(9) C10 0.135(8) 0.105(7) 0.092(7) -0.012(6) 0.070(6) 0.012(6) C11 0.188(15) 0.042(6) 0.085(8) 0.004(6) 0.097(10) 0.013(7) C12 0.032(4) 0.078(7) 0.032(4) -0.006(4) 0.012(4) -0.004(4) C13 0.151(8) 0.129(9) 0.126(8) -0.001(6) 0.099(7) -0.010(6) C14 0.154(9) 0.144(9) 0.129(8) 0.007(6) 0.097(7) -0.009(7) C15 0.058(7) 0.141(13) 0.048(6) 0.011(7) 0.024(5) 0.007(7) C16 0.132(8) 0.121(8) 0.108(7) -0.019(6) 0.076(6) -0.011(6) C17 0.133(8) 0.115(8) 0.103(7) -0.008(6) 0.082(6) -0.004(6) C18 0.078(8) 0.051(6) 0.098(9) 0.017(6) 0.042(7) -0.005(6) C19 0.071(7) 0.053(6) 0.077(7) 0.026(6) 0.024(6) 0.013(5) C20 0.092(9) 0.051(6) 0.087(8) 0.026(6) 0.041(7) 0.029(6) C21 0.123(11) 0.031(5) 0.074(7) 0.003(5) 0.033(8) 0.011(6) C22 0.075(8) 0.039(6) 0.091(9) 0.001(6) 0.020(7) -0.011(5) C23 0.046(5) 0.059(6) 0.057(6) 0.023(5) 0.014(5) 0.005(5) C24 0.054(6) 0.060(6) 0.076(7) 0.018(5) 0.037(5) 0.015(5) C25 0.041(5) 0.049(5) 0.052(5) -0.004(4) 0.013(4) 0.004(4) C26 0.098(11) 0.112(12) 0.092(10) -0.025(9) 0.016(8) -0.021(9) C27 0.046(5) 0.037(5) 0.075(7) 0.003(5) 0.006(5) 0.003(4) C28 0.077(9) 0.070(9) 0.125(12) 0.006(8) 0.014(8) -0.002(7) C29 0.045(5) 0.064(6) 0.043(5) 0.007(4) 0.021(4) 0.000(4) C30 0.058(6) 0.099(9) 0.065(7) 0.009(6) 0.038(6) -0.006(6) C31 0.15(3) 0.14(3) 0.093(18) -0.003(17) 0.068(18) -0.08(2) C32 0.094(11) 0.107(11) 0.093(11) 0.004(7) 0.043(7) -0.008(7) C33 0.070(8) 0.090(10) 0.070(8) 0.004(6) 0.038(6) 0.011(6) C34 0.036(5) 0.087(8) 0.045(5) 0.001(5) 0.021(4) -0.005(5) C35 0.067(7) 0.046(6) 0.086(8) -0.016(6) 0.006(6) -0.010(5) C36 0.095(10) 0.092(11) 0.092(10) -0.023(9) -0.010(8) -0.014(8) C37 0.130(13) 0.088(10) 0.047(6) 0.002(7) -0.003(7) -0.018(9) C38 0.061(7) 0.087(9) 0.068(7) 0.022(7) 0.007(6) -0.001(6) C39 0.069(7) 0.067(7) 0.070(7) 0.013(6) 0.000(6) -0.010(6) C40 0.046(6) 0.132(11) 0.039(5) 0.006(6) 0.020(4) -0.016(6) C41 0.071(9) 0.120(13) 0.117(12) 0.048(10) -0.027(8) 0.005(9) C42 0.120(8) 0.125(8) 0.115(8) 0.012(6) 0.038(6) 0.004(7) C43 0.102(7) 0.130(8) 0.091(7) 0.007(6) 0.046(6) -0.008(6) C44 0.102(7) 0.120(8) 0.102(7) -0.012(6) 0.035(6) -0.017(6) C45 0.080(10) 0.143(15) 0.105(11) -0.039(11) 0.008(8) -0.025(10) C46 0.170(16) 0.049(7) 0.179(17) -0.015(9) 0.140(15) -0.031(8) C47 0.123(8) 0.099(8) 0.116(8) 0.004(6) 0.060(6) -0.002(6) C48 0.103(11) 0.083(10) 0.158(15) 0.041(10) 0.089(11) 0.035(8) C49 0.121(11) 0.051(7) 0.138(12) -0.022(8) 0.101(11) -0.005(7) C50 0.161(16) 0.066(8) 0.126(12) -0.059(9) 0.086(12) -0.036(9) C51 0.054(6) 0.078(7) 0.048(6) 0.013(5) 0.006(5) 0.000(5) C52 0.071(8) 0.082(8) 0.060(6) -0.015(6) 0.027(6) -0.018(6) C53 0.083(8) 0.047(6) 0.096(9) 0.007(6) 0.046(7) 0.005(5) C54 0.104(10) 0.060(8) 0.141(12) -0.025(8) 0.075(10) -0.006(7) C55 0.077(8) 0.122(12) 0.067(7) 0.001(8) 0.026(6) 0.030(8) C56 0.103(13) 0.148(18) 0.22(2) 0.041(17) 0.071(15) 0.043(12) C57 0.033(4) 0.026(4) 0.043(4) 0.003(3) 0.003(4) 0.002(3) C58 0.035(4) 0.024(4) 0.067(6) 0.005(4) -0.003(4) -0.003(3) C59 0.041(5) 0.027(4) 0.054(5) 0.000(4) 0.000(4) -0.002(4) C60 0.032(4) 0.034(4) 0.037(4) 0.009(3) 0.004(3) -0.004(3) C61 0.038(4) 0.022(4) 0.031(4) 0.001(3) 0.006(3) 0.001(3) C62 0.034(4) 0.026(4) 0.032(4) -0.003(3) 0.008(3) -0.006(3) C63 0.036(5) 0.042(5) 0.079(7) 0.007(5) -0.010(5) -0.007(4) C64 0.042(5) 0.046(5) 0.044(5) -0.005(4) 0.015(4) -0.003(4) C65 0.030(5) 0.032(5) 0.032(5) 0.002(4) 0.015(4) 0.001(4) C66 0.032(8) 0.041(9) 0.027(8) -0.004(6) 0.016(6) -0.008(6) C67 0.038(6) 0.045(6) 0.026(5) -0.005(4) 0.014(4) -0.006(5) C68 0.039(6) 0.048(7) 0.043(6) 0.002(5) 0.025(5) -0.007(5) C69 0.033(5) 0.042(6) 0.037(5) 0.011(5) 0.015(5) 0.001(5) C70 0.031(5) 0.033(6) 0.031(5) -0.001(5) 0.015(4) 0.001(4) C71 0.057(6) 0.074(7) 0.054(6) -0.014(5) 0.024(5) -0.030(6) C72 0.073(8) 0.077(9) 0.089(9) 0.020(7) 0.042(7) -0.008(7) C73 0.019(4) 0.036(6) 0.028(5) 0.004(4) 0.007(4) 0.000(4) C74 0.039(7) 0.034(7) 0.052(8) -0.014(6) 0.022(6) 0.001(5) C75 0.032(5) 0.038(6) 0.028(5) 0.001(4) 0.006(4) -0.010(4) C76 0.028(5) 0.057(7) 0.031(5) 0.005(5) 0.013(4) 0.003(5) C77 0.024(5) 0.036(6) 0.038(5) -0.002(4) 0.011(4) 0.000(4) C78 0.026(4) 0.032(5) 0.032(4) 0.002(4) 0.012(4) -0.004(4) C79 0.060(5) 0.097(6) 0.068(5) 0.032(5) 0.031(4) -0.012(5) C80 0.070(6) 0.061(6) 0.051(5) 0.023(5) 0.045(5) 0.016(5) C81 0.027(5) 0.042(6) 0.025(5) 0.000(4) 0.013(4) -0.001(4) C82 0.039(7) 0.032(7) 0.029(6) 0.002(6) 0.011(5) 0.001(5) C83 0.037(6) 0.047(6) 0.025(5) 0.007(5) 0.011(4) 0.005(5) C84 0.036(6) 0.054(7) 0.047(6) 0.000(5) 0.026(5) 0.014(5) C85 0.043(6) 0.042(6) 0.038(6) -0.002(5) 0.019(5) 0.003(5) C86 0.034(6) 0.051(8) 0.023(6) 0.008(5) 0.013(5) 0.007(5) C87 0.056(5) 0.082(6) 0.080(6) -0.035(5) 0.037(5) 0.001(4) C88 0.067(6) 0.084(6) 0.078(6) 0.002(5) 0.019(5) 0.037(5) C89 0.020(3) 0.027(4) 0.036(4) 0.001(3) 0.007(3) -0.003(3) C90 0.030(4) 0.024(4) 0.041(4) 0.004(3) 0.018(3) 0.003(3) C91 0.025(4) 0.028(4) 0.046(4) 0.003(3) 0.017(3) 0.001(3) C92 0.028(4) 0.049(5) 0.049(5) 0.005(4) 0.019(4) 0.002(4) C93 0.032(4) 0.035(4) 0.048(5) 0.004(4) 0.018(4) 0.002(3) C94 0.032(4) 0.029(4) 0.051(5) -0.004(4) 0.021(4) -0.001(3) C95 0.049(5) 0.049(5) 0.046(5) -0.005(4) 0.028(4) -0.008(4) C96 0.069(6) 0.043(5) 0.054(5) -0.010(4) 0.037(5) -0.005(5) C97 0.032(4) 0.024(4) 0.035(4) -0.001(3) 0.012(3) 0.000(3) C98 0.061(6) 0.045(5) 0.043(5) -0.012(4) 0.009(4) 0.013(4) C99 0.086(7) 0.060(6) 0.029(4) -0.006(4) 0.016(5) 0.032(6) C100 0.073(7) 0.057(6) 0.057(6) -0.008(5) 0.037(5) 0.021(5) C101 0.044(5) 0.037(4) 0.035(4) 0.007(3) 0.016(4) 0.008(4) C102 0.040(4) 0.029(4) 0.035(4) -0.003(3) 0.020(3) -0.002(3) F31A 0.145(12) 0.147(12) 0.124(11) 0.001(6) 0.070(7) -0.017(6) C104 0.056(6) 0.061(6) 0.047(5) 0.009(5) 0.028(5) 0.020(5) C105 0.035(4) 0.042(5) 0.040(4) 0.002(4) 0.016(4) -0.004(4) C106 0.040(5) 0.043(5) 0.056(5) -0.003(4) 0.004(4) -0.008(4) C107 0.036(5) 0.055(6) 0.088(8) -0.019(6) 0.013(5) -0.020(5) C108 0.032(5) 0.078(7) 0.049(5) -0.010(5) 0.010(4) -0.009(5) C109 0.035(4) 0.061(6) 0.038(4) 0.005(4) 0.019(4) 0.008(4) C110 0.033(4) 0.042(5) 0.032(4) 0.002(3) 0.013(3) 0.001(3) C111 0.049(7) 0.073(9) 0.116(11) 0.004(8) -0.005(7) -0.018(6) C112 0.034(5) 0.097(8) 0.041(5) 0.008(5) 0.013(4) 0.014(5) C113 0.028(4) 0.030(4) 0.043(4) 0.002(3) 0.017(3) 0.002(3) C114 0.044(5) 0.035(4) 0.051(5) -0.001(4) 0.026(4) 0.002(4) C115 0.051(5) 0.039(5) 0.062(5) 0.009(4) 0.037(5) 0.002(4) C116 0.048(5) 0.041(5) 0.073(6) 0.004(4) 0.047(5) -0.003(4) C117 0.033(4) 0.036(4) 0.066(6) -0.013(4) 0.027(4) -0.005(3) C118 0.029(4) 0.041(4) 0.043(4) 0.001(4) 0.020(3) 0.001(3) C119 0.071(7) 0.053(6) 0.068(7) 0.014(5) 0.038(6) 0.005(5) C120 0.057(6) 0.046(5) 0.073(6) -0.016(5) 0.039(5) -0.018(5) B1 0.039(5) 0.027(4) 0.022(4) -0.001(3) 0.011(4) -0.001(3) B2 0.030(4) 0.032(5) 0.038(5) -0.002(4) 0.013(4) 0.000(4) C4A 0.086(13) 0.090(14) 0.091(13) -0.007(7) 0.033(8) 0.012(7) C5A 0.062(18) 0.10(3) 0.020(11) -0.009(13) -0.001(11) -0.011(16) C3A 0.095(14) 0.098(15) 0.096(14) 0.004(7) 0.040(9) -0.010(7) C31A 0.075(11) 0.080(11) 0.072(10) 0.013(7) 0.040(7) -0.010(7) C33A 0.081(11) 0.093(12) 0.077(11) 0.003(7) 0.044(8) 0.002(7) C32A 0.11(2) 0.11(3) 0.070(18) -0.038(18) 0.074(18) -0.01(2) F12A 0.079(7) 0.084(7) 0.064(6) 0.019(5) 0.023(5) -0.017(5) F10A 0.180(12) 0.160(12) 0.161(12) 0.005(6) 0.069(7) -0.001(6) F5A 0.112(12) 0.105(12) 0.108(12) 0.006(6) 0.052(8) 0.009(6) F11A 0.112(8) 0.121(9) 0.096(8) 0.014(5) 0.059(6) -0.004(6) F6A 0.062(9) 0.051(8) 0.070(9) 0.002(6) 0.010(6) 0.012(6) F7A 0.047(8) 0.040(7) 0.062(8) 0.010(5) 0.017(6) -0.003(5) F14A 0.146(13) 0.133(13) 0.140(13) -0.007(6) 0.066(8) 0.004(6) F22A 0.130(11) 0.123(11) 0.131(11) 0.001(6) 0.045(7) 0.002(6) F23A 0.123(10) 0.132(11) 0.126(10) 0.007(6) 0.047(6) -0.001(6) F24A 0.114(9) 0.125(10) 0.107(9) -0.013(6) 0.061(6) 0.012(6) F15A 0.081(8) 0.070(8) 0.068(8) -0.005(5) 0.037(6) -0.015(5) F13A 0.137(12) 0.146(13) 0.139(13) 0.003(7) 0.057(7) 0.010(6) C103 0.154(18) 0.134(16) 0.105(12) 0.036(11) 0.068(13) 0.087(15) F31 0.122(8) 0.107(8) 0.078(7) 0.000(5) 0.049(5) 0.014(6) F33A 0.052(6) 0.076(7) 0.038(6) -0.009(5) 0.018(5) 0.015(5) F32 0.101(7) 0.108(8) 0.087(7) -0.020(5) 0.047(5) 0.014(6) F32A 0.071(7) 0.053(7) 0.058(6) -0.020(5) 0.036(5) 0.000(5) _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 N1 1.958(7) . ? Ga1 N2 1.963(6) . ? Ga1 O1 2.042(6) . ? Ga1 Fe1 2.3183(15) . ? Ga2 N3 1.960(7) . ? Ga2 N4 1.969(7) . ? Ga2 O4 2.052(7) . ? Ga2 Fe2 2.3331(17) . ? Fe1 C23 1.781(12) . ? Fe1 C24 1.792(11) . ? Fe1 C22 2.083(11) . ? Fe1 C21 2.084(11) . ? Fe1 C18 2.090(11) . ? Fe1 C19 2.092(10) . ? Fe1 C20 2.099(11) . ? Fe2 C52 1.733(13) . ? Fe2 C51 1.737(12) . ? Fe2 C49 2.072(11) . ? Fe2 C50 2.076(12) . ? Fe2 C46 2.093(12) . ? Fe2 C48 2.100(13) . ? Fe2 C47 2.105(17) . ? F1 C63 1.349(14) . ? F2 C63 1.297(13) . ? F3 C63 1.325(11) . ? F4 C64 1.312(12) . ? F5 C64 1.333(11) . ? F6 C64 1.329(11) . ? F7 C71 1.189(13) . ? F8 C71 1.350(15) . ? F9 C71 1.254(13) . ? F10 C72 1.333(17) . ? F11 C72 1.262(17) . ? F12 C72 1.35(2) . ? F13 C79 1.315(18) . ? F14 C79 1.321(16) . ? F15 C79 1.297(19) . ? F16 C80 1.305(14) . ? F17 C80 1.269(13) . ? F18 C80 1.258(14) . ? F19 C87 1.220(14) . ? F20 C87 1.222(13) . ? F21 C87 1.366(17) . ? F22 C88 1.293(18) . ? F23 C88 1.33(2) . ? F24 C88 1.33(2) . ? F25 C96 1.265(12) . ? F26 C96 1.347(12) . ? F27 C96 1.304(13) . ? F28 C95 1.292(11) . ? F29 C95 1.311(11) . ? F30 C95 1.292(11) . ? F33 C103 1.34(3) . ? F34 C104 1.324(12) . ? F35 C104 1.332(11) . ? F36 C104 1.300(10) . ? F37 C111 1.344(18) . ? F38 C111 1.283(16) . ? F39 C111 1.272(14) . ? F40 C112 1.330(12) . ? F41 C112 1.331(11) . ? F42 C112 1.312(11) . ? F43 C120 1.340(11) . ? F44 C120 1.324(12) . ? F45 C120 1.343(11) . ? F46 C119 1.315(13) . ? F47 C119 1.286(13) . ? F48 C119 1.286(12) . ? O1 C25 1.450(10) . ? O1 C27 1.457(11) . ? O2 C23 1.140(12) . ? O3 C24 1.118(12) . ? O4 C55 1.414(14) . ? O4 C53 1.496(13) . ? O5 C51 1.175(14) . ? O6 C52 1.168(14) . ? N1 C1 1.340(11) . ? N1 C6 1.475(11) . ? N2 C1 1.335(10) . ? N2 C12 1.492(10) . ? N3 C29 1.331(11) . ? N3 C34 1.488(11) . ? N4 C29 1.354(12) . ? N4 C40 1.455(12) . ? C1 C2 1.534(12) . ? C2 C5A 1.39(2) . ? C2 C4 1.45(2) . ? C2 C5 1.58(2) . ? C2 C4A 1.59(4) . ? C2 C3A 1.61(4) . ? C2 C3 1.61(2) . ? C6 C7 1.505(14) . ? C6 C11 1.507(14) . ? C7 C8 1.547(14) . ? C8 C9 1.443(19) . ? C9 C10 1.50(2) . ? C10 C11 1.544(16) . ? C12 C13 1.45(2) . ? C12 C17 1.467(18) . ? C13 C14 1.55(2) . ? C14 C15 1.40(2) . ? C15 C16 1.43(2) . ? C16 C17 1.561(18) . ? C18 C22 1.416(17) . ? C18 C19 1.423(16) . ? C19 C20 1.358(16) . ? C20 C21 1.421(17) . ? C21 C22 1.375(18) . ? C25 C26 1.486(17) . ? C27 C28 1.571(17) . ? C29 C30 1.523(14) . ? C30 C33A 1.34(3) . ? C30 C32 1.38(3) . ? C30 C31 1.53(3) . ? C30 C33 1.59(2) . ? C30 C32A 1.62(3) . ? C30 C31A 1.64(3) . ? C34 C39 1.488(15) . ? C34 C35 1.547(15) . ? C35 C36 1.557(16) . ? C36 C37 1.46(2) . ? C37 C38 1.436(19) . ? C38 C39 1.541(15) . ? C40 C45 1.51(2) . ? C40 C41 1.60(2) . ? C41 C42 1.60(2) . ? C42 C43 1.41(2) . ? C43 C44 1.40(2) . ? C44 C45 1.59(2) . ? C46 C47 1.36(2) . ? C46 C50 1.46(2) . ? C47 C48 1.36(2) . ? C48 C49 1.33(2) . ? C49 C50 1.41(2) . ? C53 C54 1.485(17) . ? C55 C56 1.45(2) . ? C57 C58 1.379(11) . ? C57 C62 1.395(11) . ? C57 B1 1.640(11) . ? C58 C59 1.400(12) . ? C59 C60 1.395(12) . ? C59 C63 1.494(12) . ? C60 C61 1.372(11) . ? C61 C62 1.397(10) . ? C61 C64 1.471(12) . ? C64 F7A 1.28(2) . ? C64 F5A 1.32(3) . ? C64 F6A 1.37(2) . ? C65 C66 1.40(2) . ? C65 C70 1.408(14) . ? C65 B1 1.663(13) . ? C66 C67 1.40(2) . ? C67 C68 1.381(14) . ? C67 C71 1.453(14) . ? C68 C69 1.391(15) . ? C69 C70 1.394(15) . ? C69 C72 1.524(16) . ? C72 F12A 1.164(18) . ? C72 F10A 1.39(3) . ? C72 F11A 1.42(2) . ? C73 C74 1.355(17) . ? C73 C78 1.401(14) . ? C73 B1 1.642(12) . ? C74 C75 1.377(16) . ? C75 C76 1.357(16) . ? C75 C79 1.473(15) . ? C76 C77 1.406(15) . ? C77 C78 1.382(14) . ? C77 C80 1.539(14) . ? C79 F14A 1.24(3) . ? C79 F13A 1.36(4) . ? C79 F15A 1.49(2) . ? C81 C82 1.388(15) . ? C81 C86 1.419(15) . ? C81 B1 1.629(13) . ? C82 C83 1.404(17) . ? C83 C84 1.358(15) . ? C83 C87 1.484(15) . ? C84 C85 1.426(15) . ? C85 C86 1.368(17) . ? C85 C88 1.458(16) . ? C88 F24A 1.23(2) . ? C88 F23A 1.32(3) . ? C88 F22A 1.33(3) . ? C89 C94 1.402(11) . ? C89 C90 1.403(10) . ? C89 B2 1.639(12) . ? C90 C91 1.403(10) . ? C91 C92 1.372(11) . ? C91 C95 1.491(12) . ? C92 C93 1.388(12) . ? C93 C94 1.385(11) . ? C93 C96 1.468(12) . ? C97 C102 1.394(11) . ? C97 C98 1.408(11) . ? C97 B2 1.648(11) . ? C98 C99 1.389(13) . ? C99 C100 1.370(13) . ? C99 C103 1.56(2) . ? C100 C101 1.369(12) . ? C101 C102 1.359(11) . ? C101 C104 1.533(12) . ? F31A C103 1.62(3) . ? C105 C110 1.400(12) . ? C105 C106 1.400(12) . ? C105 B2 1.654(12) . ? C106 C107 1.405(13) . ? C107 C108 1.362(15) . ? C107 C111 1.487(16) . ? C108 C109 1.374(14) . ? C109 C110 1.412(11) . ? C109 C112 1.488(14) . ? C113 C114 1.399(11) . ? C113 C118 1.402(11) . ? C113 B2 1.646(11) . ? C114 C115 1.392(12) . ? C115 C116 1.395(13) . ? C115 C119 1.460(13) . ? C116 C117 1.354(13) . ? C117 C118 1.386(11) . ? C117 C120 1.511(13) . ? B1 C65A 1.63(3) . ? B1 C81A 1.66(3) . ? B1 C73A 1.69(3) . ? C103 F33A 1.10(2) . ? C103 F32A 1.24(2) . ? C103 F31 1.33(2) . ? C103 F32 1.35(2) . ? C65A C70A 1.38(4) . ? C65A C66A 1.46(4) . ? C69A C68A 1.34(5) . ? C69A C70A 1.45(4) . ? C68A C67A 1.39(5) . ? C67A C66A 1.40(4) . ? C73A C78A 1.30(7) . ? C73A C74A 1.36(4) . ? C75A C76A 1.38(4) . ? C75A C74A 1.40(4) . ? C77A C76A 1.43(4) . ? C77A C78A 1.48(8) . ? C81A C82A 1.37(4) . ? C81A C86A 1.41(4) . ? C83A C84A 1.39(4) . ? C83A C82A 1.41(4) . ? C84A C85A 1.38(4) . ? C85A C86A 1.38(5) . ? 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 N1 Ga1 N2 66.8(3) . . ? N1 Ga1 O1 98.0(3) . . ? N2 Ga1 O1 100.1(3) . . ? N1 Ga1 Fe1 130.1(2) . . ? N2 Ga1 Fe1 131.1(2) . . ? O1 Ga1 Fe1 117.78(17) . . ? N3 Ga2 N4 66.8(3) . . ? N3 Ga2 O4 99.7(3) . . ? N4 Ga2 O4 101.7(4) . . ? N3 Ga2 Fe2 129.0(2) . . ? N4 Ga2 Fe2 132.3(3) . . ? O4 Ga2 Fe2 115.7(2) . . ? C23 Fe1 C24 95.1(5) . . ? C23 Fe1 C22 131.1(5) . . ? C24 Fe1 C22 133.1(5) . . ? C23 Fe1 C21 160.5(5) . . ? C24 Fe1 C21 99.8(6) . . ? C22 Fe1 C21 38.5(5) . . ? C23 Fe1 C18 97.4(5) . . ? C24 Fe1 C18 161.0(5) . . ? C22 Fe1 C18 39.7(5) . . ? C21 Fe1 C18 65.3(5) . . ? C23 Fe1 C19 95.7(5) . . ? C24 Fe1 C19 124.6(5) . . ? C22 Fe1 C19 66.5(5) . . ? C21 Fe1 C19 65.4(5) . . ? C18 Fe1 C19 39.8(4) . . ? C23 Fe1 C20 126.2(5) . . ? C24 Fe1 C20 96.1(5) . . ? C22 Fe1 C20 65.7(5) . . ? C21 Fe1 C20 39.7(5) . . ? C18 Fe1 C20 65.0(5) . . ? C19 Fe1 C20 37.8(4) . . ? C23 Fe1 Ga1 90.6(3) . . ? C24 Fe1 Ga1 88.4(3) . . ? C22 Fe1 Ga1 83.9(3) . . ? C21 Fe1 Ga1 102.4(3) . . ? C18 Fe1 Ga1 105.7(3) . . ? C19 Fe1 Ga1 145.4(3) . . ? C20 Fe1 Ga1 142.1(4) . . ? C52 Fe2 C51 93.4(5) . . ? C52 Fe2 C49 141.3(6) . . ? C51 Fe2 C49 125.1(6) . . ? C52 Fe2 C50 103.2(7) . . ? C51 Fe2 C50 161.1(7) . . ? C49 Fe2 C50 39.9(6) . . ? C52 Fe2 C46 94.6(7) . . ? C51 Fe2 C46 129.8(6) . . ? C49 Fe2 C46 65.4(5) . . ? C50 Fe2 C46 40.9(6) . . ? C52 Fe2 C48 156.4(6) . . ? C51 Fe2 C48 96.6(7) . . ? C49 Fe2 C48 37.1(6) . . ? C50 Fe2 C48 64.6(7) . . ? C46 Fe2 C48 62.7(7) . . ? C52 Fe2 C47 119.8(7) . . ? C51 Fe2 C47 97.3(6) . . ? C49 Fe2 C47 64.5(6) . . ? C50 Fe2 C47 66.8(7) . . ? C46 Fe2 C47 37.9(6) . . ? C48 Fe2 C47 37.7(6) . . ? C52 Fe2 Ga2 91.7(4) . . ? C51 Fe2 Ga2 85.9(4) . . ? C49 Fe2 Ga2 87.5(4) . . ? C50 Fe2 Ga2 102.2(5) . . ? C46 Fe2 Ga2 143.0(4) . . ? C48 Fe2 Ga2 110.3(4) . . ? C47 Fe2 Ga2 147.9(5) . . ? C25 O1 C27 115.8(7) . . ? C25 O1 Ga1 122.8(5) . . ? C27 O1 Ga1 120.0(5) . . ? C55 O4 C53 115.9(10) . . ? C55 O4 Ga2 122.7(8) . . ? C53 O4 Ga2 120.2(6) . . ? C1 N1 C6 133.0(7) . . ? C1 N1 Ga1 92.6(5) . . ? C6 N1 Ga1 134.3(6) . . ? C1 N2 C12 134.1(7) . . ? C1 N2 Ga1 92.6(5) . . ? C12 N2 Ga1 133.0(5) . . ? C29 N3 C34 133.7(7) . . ? C29 N3 Ga2 93.3(5) . . ? C34 N3 Ga2 132.7(6) . . ? C29 N4 C40 133.4(8) . . ? C29 N4 Ga2 92.2(6) . . ? C40 N4 Ga2 134.1(6) . . ? N2 C1 N1 107.7(7) . . ? N2 C1 C2 126.4(8) . . ? N1 C1 C2 125.8(7) . . ? C5A C2 C4 114.7(17) . . ? C5A C2 C1 125.4(16) . . ? C4 C2 C1 119.5(11) . . ? C5A C2 C5 56.9(17) . . ? C4 C2 C5 109.9(14) . . ? C1 C2 C5 107.3(10) . . ? C5A C2 C4A 108(2) . . ? C4 C2 C4A 55.8(17) . . ? C1 C2 C4A 106.5(16) . . ? C5 C2 C4A 63.1(18) . . ? C5A C2 C3A 106(2) . . ? C4 C2 C3A 43.8(17) . . ? C1 C2 C3A 108.3(16) . . ? C5 C2 C3A 143.6(18) . . ? C4A C2 C3A 100(2) . . ? C5A C2 C3 49.8(15) . . ? C4 C2 C3 108.1(13) . . ? C1 C2 C3 105.1(10) . . ? C5 C2 C3 105.9(15) . . ? C4A C2 C3 148.4(17) . . ? C3A C2 C3 71.3(18) . . ? N1 C6 C7 108.6(8) . . ? N1 C6 C11 110.2(7) . . ? C7 C6 C11 108.6(10) . . ? C6 C7 C8 111.5(10) . . ? C9 C8 C7 113.5(11) . . ? C8 C9 C10 108.9(12) . . ? C9 C10 C11 111.8(12) . . ? C6 C11 C10 112.3(10) . . ? C13 C12 C17 111.6(12) . . ? C13 C12 N2 110.5(9) . . ? C17 C12 N2 109.4(8) . . ? C12 C13 C14 114.2(15) . . ? C15 C14 C13 114.8(15) . . ? C14 C15 C16 114.4(13) . . ? C15 C16 C17 114.1(14) . . ? C12 C17 C16 112.0(13) . . ? C22 C18 C19 107.4(11) . . ? C22 C18 Fe1 69.9(6) . . ? C19 C18 Fe1 70.2(6) . . ? C20 C19 C18 108.0(11) . . ? C20 C19 Fe1 71.4(6) . . ? C18 C19 Fe1 70.0(6) . . ? C19 C20 C21 108.6(11) . . ? C19 C20 Fe1 70.8(7) . . ? C21 C20 Fe1 69.6(6) . . ? C22 C21 C20 108.4(11) . . ? C22 C21 Fe1 70.7(7) . . ? C20 C21 Fe1 70.7(7) . . ? C21 C22 C18 107.5(11) . . ? C21 C22 Fe1 70.8(7) . . ? C18 C22 Fe1 70.4(6) . . ? O2 C23 Fe1 176.1(9) . . ? O3 C24 Fe1 176.8(10) . . ? O1 C25 C26 108.6(9) . . ? O1 C27 C28 110.3(9) . . ? N3 C29 N4 107.2(8) . . ? N3 C29 C30 126.8(9) . . ? N4 C29 C30 126.1(8) . . ? C33A C30 C32 116(2) . . ? C33A C30 C29 121.0(16) . . ? C32 C30 C29 122.5(15) . . ? C33A C30 C31 53.8(18) . . ? C32 C30 C31 110.5(18) . . ? C29 C30 C31 105.7(14) . . ? C33A C30 C33 45.7(17) . . ? C32 C30 C33 107.2(17) . . ? C29 C30 C33 109.2(11) . . ? C31 C30 C33 99.3(18) . . ? C33A C30 C32A 116(2) . . ? C32 C30 C32A 37.0(15) . . ? C29 C30 C32A 108.4(13) . . ? C31 C30 C32A 143.2(17) . . ? C33 C30 C32A 82.3(17) . . ? C33A C30 C31A 106(2) . . ? C32 C30 C31A 60.5(16) . . ? C29 C30 C31A 105.1(12) . . ? C31 C30 C31A 60.7(17) . . ? C33 C30 C31A 144.0(14) . . ? C32A C30 C31A 96.8(18) . . ? C39 C34 N3 110.0(8) . . ? C39 C34 C35 108.7(9) . . ? N3 C34 C35 107.0(8) . . ? C34 C35 C36 109.3(10) . . ? C37 C36 C35 114.4(12) . . ? C38 C37 C36 113.5(12) . . ? C37 C38 C39 111.6(12) . . ? C34 C39 C38 113.1(10) . . ? N4 C40 C45 110.6(10) . . ? N4 C40 C41 106.3(10) . . ? C45 C40 C41 108.9(12) . . ? C40 C41 C42 105.6(14) . . ? C43 C42 C41 113.4(15) . . ? C44 C43 C42 116.6(17) . . ? C43 C44 C45 108.9(15) . . ? C40 C45 C44 110.6(14) . . ? C47 C46 C50 109.2(15) . . ? C47 C46 Fe2 71.5(10) . . ? C50 C46 Fe2 68.9(6) . . ? C48 C47 C46 106.5(16) . . ? C48 C47 Fe2 71.0(9) . . ? C46 C47 Fe2 70.6(9) . . ? C49 C48 C47 112.2(17) . . ? C49 C48 Fe2 70.3(8) . . ? C47 C48 Fe2 71.3(9) . . ? C48 C49 C50 108.9(13) . . ? C48 C49 Fe2 72.6(7) . . ? C50 C49 Fe2 70.2(7) . . ? C49 C50 C46 103.1(15) . . ? C49 C50 Fe2 69.9(7) . . ? C46 C50 Fe2 70.2(7) . . ? O5 C51 Fe2 176.5(11) . . ? O6 C52 Fe2 178.6(11) . . ? C54 C53 O4 111.0(10) . . ? O4 C55 C56 111.2(13) . . ? C58 C57 C62 116.1(7) . . ? C58 C57 B1 123.6(7) . . ? C62 C57 B1 120.1(7) . . ? C57 C58 C59 122.4(8) . . ? C60 C59 C58 120.0(8) . . ? C60 C59 C63 119.5(8) . . ? C58 C59 C63 120.6(8) . . ? C61 C60 C59 118.7(7) . . ? C60 C61 C62 120.2(7) . . ? C60 C61 C64 120.1(7) . . ? C62 C61 C64 119.6(7) . . ? C57 C62 C61 122.5(7) . . ? F2 C63 F3 106.9(9) . . ? F2 C63 F1 105.5(8) . . ? F3 C63 F1 106.1(9) . . ? F2 C63 C59 113.9(9) . . ? F3 C63 C59 112.8(8) . . ? F1 C63 C59 111.1(9) . . ? F7A C64 F4 47.1(10) . . ? F7A C64 F5A 109(2) . . ? F4 C64 F5A 128.4(16) . . ? F7A C64 F6 131.4(12) . . ? F4 C64 F6 105.7(9) . . ? F5A C64 F6 51.5(16) . . ? F7A C64 F5 62.6(11) . . ? F4 C64 F5 106.3(9) . . ? F5A C64 F5 54.5(17) . . ? F6 C64 F5 104.2(8) . . ? F7A C64 F6A 106.1(16) . . ? F4 C64 F6A 63.3(13) . . ? F5A C64 F6A 95(2) . . ? F6 C64 F6A 46.9(11) . . ? F5 C64 F6A 133.4(12) . . ? F7A C64 C61 115.0(11) . . ? F4 C64 C61 113.6(8) . . ? F5A C64 C61 118.0(16) . . ? F6 C64 C61 113.0(8) . . ? F5 C64 C61 113.2(7) . . ? F6A C64 C61 112.2(11) . . ? C66 C65 C70 115.8(12) . . ? C66 C65 B1 124.1(11) . . ? C70 C65 B1 120.0(8) . . ? C65 C66 C67 122.2(16) . . ? C68 C67 C66 120.6(12) . . ? C68 C67 C71 121.6(10) . . ? C66 C67 C71 117.5(11) . . ? C67 C68 C69 118.4(10) . . ? C68 C69 C70 120.9(9) . . ? C68 C69 C72 121.3(10) . . ? C70 C69 C72 117.8(10) . . ? C69 C70 C65 122.0(10) . . ? F7 C71 F9 105.0(12) . . ? F7 C71 F8 101.1(11) . . ? F9 C71 F8 103.9(11) . . ? F7 C71 C67 122.1(11) . . ? F9 C71 C67 113.6(10) . . ? F8 C71 C67 109.1(10) . . ? F12A C72 F11 55.8(12) . . ? F12A C72 F10 132.2(13) . . ? F11 C72 F10 113.3(13) . . ? F12A C72 F12 51.8(12) . . ? F11 C72 F12 106.6(15) . . ? F10 C72 F12 105.3(14) . . ? F12A C72 F10A 97.2(18) . . ? F11 C72 F10A 139.0(17) . . ? F10 C72 F10A 59.5(15) . . ? F12 C72 F10A 49.1(14) . . ? F12A C72 F11A 109.1(17) . . ? F11 C72 F11A 55.8(11) . . ? F10 C72 F11A 65.7(11) . . ? F12 C72 F11A 147.1(14) . . ? F10A C72 F11A 123.2(18) . . ? F12A C72 C69 116.7(11) . . ? F11 C72 C69 111.7(11) . . ? F10 C72 C69 110.4(12) . . ? F12 C72 C69 109.2(11) . . ? F10A C72 C69 108.0(16) . . ? F11A C72 C69 103.5(11) . . ? C74 C73 C78 113.8(10) . . ? C74 C73 B1 123.8(9) . . ? C78 C73 B1 121.9(8) . . ? C73 C74 C75 126.7(13) . . ? C76 C75 C74 118.6(11) . . ? C76 C75 C79 119.4(10) . . ? C74 C75 C79 122.0(11) . . ? C75 C76 C77 118.4(9) . . ? C78 C77 C76 120.3(10) . . ? C78 C77 C80 119.9(9) . . ? C76 C77 C80 119.8(9) . . ? C77 C78 C73 122.2(9) . . ? F14A C79 F15 53.9(16) . . ? F14A C79 F13 130.7(18) . . ? F15 C79 F13 105.9(17) . . ? F14A C79 F14 64.9(17) . . ? F15 C79 F14 115.5(13) . . ? F13 C79 F14 98.0(12) . . ? F14A C79 F13A 99(2) . . ? F15 C79 F13A 117.2(19) . . ? F13 C79 F13A 45.4(15) . . ? F14 C79 F13A 52.9(15) . . ? F14A C79 C75 116.4(19) . . ? F15 C79 C75 111.6(12) . . ? F13 C79 C75 112.9(10) . . ? F14 C79 C75 112.1(12) . . ? F13A C79 C75 130.4(17) . . ? F14A C79 F15A 85.6(18) . . ? F15 C79 F15A 35.6(10) . . ? F13 C79 F15A 72.3(13) . . ? F14 C79 F15A 131.7(12) . . ? F13A C79 F15A 100(2) . . ? C75 C79 F15A 115.1(11) . . ? F18 C80 F17 99.3(12) . . ? F18 C80 F16 125.0(11) . . ? F17 C80 F16 92.0(10) . . ? F18 C80 C77 112.8(10) . . ? F17 C80 C77 114.1(9) . . ? F16 C80 C77 110.7(9) . . ? C82 C81 C86 113.4(11) . . ? C82 C81 B1 123.1(9) . . ? C86 C81 B1 123.2(9) . . ? C81 C82 C83 124.0(11) . . ? C84 C83 C82 120.4(10) . . ? C84 C83 C87 120.0(10) . . ? C82 C83 C87 119.6(10) . . ? C83 C84 C85 118.3(10) . . ? C86 C85 C84 119.3(10) . . ? C86 C85 C88 121.1(10) . . ? C84 C85 C88 119.7(10) . . ? C85 C86 C81 124.4(11) . . ? F19 C87 F20 121.7(14) . . ? F19 C87 F21 88.3(11) . . ? F20 C87 F21 102.2(10) . . ? F19 C87 C83 114.4(10) . . ? F20 C87 C83 116.0(10) . . ? F21 C87 C83 108.0(12) . . ? F24A C88 F22 116.8(15) . . ? F24A C88 F23A 108.1(18) . . ? F22 C88 F23A 46.5(12) . . ? F24A C88 F24 50.1(13) . . ? F22 C88 F24 101.7(15) . . ? F23A C88 F24 133.8(16) . . ? F24A C88 F22A 103(2) . . ? F22 C88 F22A 53.5(13) . . ? F23A C88 F22A 99.9(19) . . ? F24 C88 F22A 58.7(15) . . ? F24A C88 F23 54.9(14) . . ? F22 C88 F23 110.0(14) . . ? F23A C88 F23 69.3(15) . . ? F24 C88 F23 105.0(15) . . ? F22A C88 F23 146.5(16) . . ? F24A C88 C85 124.7(14) . . ? F22 C88 C85 118.2(12) . . ? F23A C88 C85 113.3(15) . . ? F24 C88 C85 111.6(13) . . ? F22A C88 C85 104.0(15) . . ? F23 C88 C85 109.4(12) . . ? C94 C89 C90 115.3(7) . . ? C94 C89 B2 121.7(7) . . ? C90 C89 B2 122.9(6) . . ? C91 C90 C89 122.1(7) . . ? C92 C91 C90 120.7(7) . . ? C92 C91 C95 120.0(7) . . ? C90 C91 C95 119.3(7) . . ? C91 C92 C93 118.5(8) . . ? C94 C93 C92 120.8(7) . . ? C94 C93 C96 120.7(7) . . ? C92 C93 C96 118.4(7) . . ? C93 C94 C89 122.5(7) . . ? F28 C95 F30 104.5(9) . . ? F28 C95 F29 106.0(8) . . ? F30 C95 F29 104.8(8) . . ? F28 C95 C91 114.6(7) . . ? F30 C95 C91 113.5(7) . . ? F29 C95 C91 112.6(8) . . ? F25 C96 F27 106.5(10) . . ? F25 C96 F26 102.6(9) . . ? F27 C96 F26 98.2(9) . . ? F25 C96 C93 117.0(8) . . ? F27 C96 C93 115.8(8) . . ? F26 C96 C93 114.3(8) . . ? C102 C97 C98 115.1(7) . . ? C102 C97 B2 122.9(7) . . ? C98 C97 B2 121.5(7) . . ? C99 C98 C97 121.6(8) . . ? C100 C99 C98 121.1(8) . . ? C100 C99 C103 121.7(9) . . ? C98 C99 C103 117.1(9) . . ? C101 C100 C99 117.6(8) . . ? C102 C101 C100 122.2(8) . . ? C102 C101 C104 119.3(7) . . ? C100 C101 C104 118.5(8) . . ? C101 C102 C97 122.3(7) . . ? F36 C104 F34 107.1(8) . . ? F36 C104 F35 107.7(8) . . ? F34 C104 F35 105.4(8) . . ? F36 C104 C101 113.4(7) . . ? F34 C104 C101 111.7(8) . . ? F35 C104 C101 111.1(8) . . ? C110 C105 C106 116.5(8) . . ? C110 C105 B2 123.1(7) . . ? C106 C105 B2 120.3(7) . . ? C105 C106 C107 121.4(9) . . ? C108 C107 C106 121.2(9) . . ? C108 C107 C111 119.6(9) . . ? C106 C107 C111 119.2(10) . . ? C107 C108 C109 119.0(8) . . ? C108 C109 C110 120.9(8) . . ? C108 C109 C112 120.6(8) . . ? C110 C109 C112 118.5(8) . . ? C105 C110 C109 121.1(8) . . ? F39 C111 F38 106.9(14) . . ? F39 C111 F37 106.6(12) . . ? F38 C111 F37 96.6(12) . . ? F39 C111 C107 117.0(12) . . ? F38 C111 C107 115.8(11) . . ? F37 C111 C107 111.6(14) . . ? F42 C112 F40 106.2(8) . . ? F42 C112 F41 108.7(8) . . ? F40 C112 F41 104.5(10) . . ? F42 C112 C109 112.6(10) . . ? F40 C112 C109 112.0(7) . . ? F41 C112 C109 112.3(8) . . ? C114 C113 C118 116.2(7) . . ? C114 C113 B2 122.2(7) . . ? C118 C113 B2 121.0(7) . . ? C115 C114 C113 122.2(8) . . ? C114 C115 C116 119.3(8) . . ? C114 C115 C119 120.6(9) . . ? C116 C115 C119 120.1(8) . . ? C117 C116 C115 119.5(8) . . ? C116 C117 C118 121.4(8) . . ? C116 C117 C120 121.0(8) . . ? C118 C117 C120 117.6(8) . . ? C117 C118 C113 121.4(8) . . ? F47 C119 F48 108.2(10) . . ? F47 C119 F46 101.2(10) . . ? F48 C119 F46 100.8(9) . . ? F47 C119 C115 114.1(9) . . ? F48 C119 C115 115.9(10) . . ? F46 C119 C115 114.8(9) . . ? F44 C120 F43 106.6(8) . . ? F44 C120 F45 107.3(8) . . ? F43 C120 F45 106.6(8) . . ? F44 C120 C117 112.9(8) . . ? F43 C120 C117 111.8(8) . . ? F45 C120 C117 111.3(8) . . ? C65A B1 C81 58.1(10) . . ? C65A B1 C57 92.3(11) . . ? C81 B1 C57 116.7(6) . . ? C65A B1 C73 166.5(12) . . ? C81 B1 C73 111.5(7) . . ? C57 B1 C73 100.5(7) . . ? C65A B1 C81A 114.4(14) . . ? C81 B1 C81A 56.4(9) . . ? C57 B1 C81A 116.6(10) . . ? C73 B1 C81A 55.8(9) . . ? C65A B1 C65 66.8(11) . . ? C81 B1 C65 104.2(7) . . ? C57 B1 C65 113.0(6) . . ? C73 B1 C65 111.2(7) . . ? C81A B1 C65 130.2(11) . . ? C65A B1 C73A 115.0(14) . . ? C81 B1 C73A 129.1(11) . . ? C57 B1 C73A 113.8(10) . . ? C73 B1 C73A 63.5(9) . . ? C81A B1 C73A 104.9(13) . . ? C65 B1 C73A 48.4(9) . . ? C89 B2 C113 113.1(6) . . ? C89 B2 C97 111.1(6) . . ? C113 B2 C97 103.2(6) . . ? C89 B2 C105 105.4(6) . . ? C113 B2 C105 112.6(6) . . ? C97 B2 C105 111.5(6) . . ? F33A C103 F32A 118(2) . . ? F33A C103 F31 45.9(11) . . ? F32A C103 F31 135.0(17) . . ? F33A C103 F33 57.8(19) . . ? F32A C103 F33 79(2) . . ? F31 C103 F33 104(2) . . ? F33A C103 F32 130.3(18) . . ? F32A C103 F32 33.3(9) . . ? F31 C103 F32 116.2(19) . . ? F33 C103 F32 111(2) . . ? F33A C103 C99 121.3(14) . . ? F32A C103 C99 111.6(14) . . ? F31 C103 C99 110.5(15) . . ? F33 C103 C99 106.2(17) . . ? F32 C103 C99 108.4(15) . . ? F33A C103 F31A 104.4(19) . . ? F32A C103 F31A 93.1(17) . . ? F31 C103 F31A 62.9(16) . . ? F33 C103 F31A 151(2) . . ? F32 C103 F31A 60.8(16) . . ? C99 C103 F31A 102.3(18) . . ? C70A C65A C66A 122(3) . . ? C70A C65A B1 120(2) . . ? C66A C65A B1 118(2) . . ? C68A C69A C70A 122(3) . . ? C69A C68A C67A 122(3) . . ? C68A C67A C66A 120(3) . . ? C67A C66A C65A 118(3) . . ? C65A C70A C69A 116(3) . . ? C78A C73A C74A 123(4) . . ? C78A C73A B1 116(4) . . ? C74A C73A B1 121(2) . . ? C76A C75A C74A 120(3) . . ? C76A C77A C78A 117(3) . . ? C75A C76A C77A 119(3) . . ? C73A C74A C75A 121(3) . . ? C73A C78A C77A 119(5) . . ? C82A C81A C86A 119(3) . . ? C82A C81A B1 123(2) . . ? C86A C81A B1 117(2) . . ? C84A C83A C82A 121(3) . . ? C85A C84A C83A 117(3) . . ? C86A C85A C84A 123(3) . . ? C81A C82A C83A 121(2) . . ? C85A C86A C81A 120(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.33 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.296 _refine_diff_density_min -1.234 _refine_diff_density_rms 0.132 # Attachment 'cmpd4.cif' data_compound4 _database_code_depnum_ccdc_archive 'CCDC 617856' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H85 B F24 Fe2 Ga2 N4 O5' _chemical_formula_weight 1900.47 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' N N 0.0061 0.0033 '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 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 13.873(3) _cell_length_b 20.005(4) _cell_length_c 31.856(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.50(3) _cell_angle_gamma 90.00 _cell_volume 8838(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3872 _exptl_absorpt_coefficient_mu 1.025 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.783 _exptl_absorpt_correction_T_max 0.861 _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 52383 _diffrn_reflns_av_R_equivalents 0.0757 _diffrn_reflns_av_sigmaI/netI 0.0670 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 25.36 _reflns_number_total 15894 _reflns_number_gt 12281 _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. During the course of refinement, 1 CF3 group of the anion was found to be disordered over 2 sites. This disorder was successfully modelled. The highest residual electron density peak (2.028 e-/ang.3) seen in the final difference map was located close to Ga(2). ; _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^)+(0.1067P)^2^+31.0962P] 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 15894 _refine_ls_number_parameters 1097 _refine_ls_number_restraints 174 _refine_ls_R_factor_all 0.0976 _refine_ls_R_factor_gt 0.0779 _refine_ls_wR_factor_ref 0.2147 _refine_ls_wR_factor_gt 0.2024 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.130 _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 0.13537(4) 0.23431(3) 0.11765(2) 0.03054(18) Uani 1 1 d . . . Ga2 Ga 0.19667(4) 0.25816(3) 0.23697(2) 0.03128(18) Uani 1 1 d . . . Fe1 Fe -0.02037(6) 0.19523(4) 0.10262(3) 0.0324(2) Uani 1 1 d . . . Fe2 Fe 0.07187(6) 0.31541(5) 0.26773(3) 0.0400(2) Uani 1 1 d . . . F1 F -0.0191(5) 0.0352(3) -0.09910(19) 0.1026(19) Uani 1 1 d U . . F2 F 0.0953(6) 0.0578(4) -0.0571(3) 0.152(3) Uani 1 1 d U . . F3 F -0.0393(5) 0.0351(3) -0.0371(2) 0.0997(18) Uani 1 1 d U . . F4 F 0.0720(4) 0.3649(3) -0.0826(2) 0.0933(18) Uani 1 1 d U . . F5 F 0.1802(3) 0.2933(3) -0.0771(2) 0.0861(16) Uani 1 1 d U . . F6 F 0.1158(5) 0.3265(3) -0.02308(18) 0.1032(19) Uani 1 1 d U . . F7 F -0.6530(4) 0.0910(3) -0.08453(19) 0.102(2) Uani 1 1 d U . . F8 F -0.6311(4) 0.1842(3) -0.1115(2) 0.108(2) Uani 1 1 d U . . F9 F -0.5739(5) 0.1028(4) -0.1390(2) 0.123(2) Uani 1 1 d U . . F10 F -0.4665(3) 0.0591(2) 0.04293(14) 0.0642(12) Uani 1 1 d U . . F11 F -0.3492(4) 0.1247(3) 0.05525(15) 0.0870(17) Uani 1 1 d U . . F12 F -0.3269(4) 0.0326(3) 0.02559(17) 0.0937(18) Uani 1 1 d U . . F13 F -0.2120(5) 0.0990(3) -0.2206(2) 0.113(2) Uani 1 1 d U . . F14 F -0.3541(4) 0.1198(3) -0.2303(2) 0.0990(19) Uani 1 1 d U . . F15 F -0.2554(6) 0.1585(3) -0.2720(2) 0.127(2) Uani 1 1 d U . . F16 F -0.2088(5) 0.3964(3) -0.25403(16) 0.0943(17) Uani 1 1 d U . . F17 F -0.2502(4) 0.4402(2) -0.19652(19) 0.0883(16) Uani 1 1 d U . . F18 F -0.1100(4) 0.4071(3) -0.2032(2) 0.0894(17) Uani 1 1 d U . . F19 F -0.5240(4) 0.4222(3) -0.10948(17) 0.0956(18) Uani 1 1 d U . . F20 F -0.5738(3) 0.4407(3) -0.04819(16) 0.0732(14) Uani 1 1 d U . . F21 F -0.4775(4) 0.5051(3) -0.0747(2) 0.0872(16) Uani 1 1 d U . . F22 F -0.3039(9) 0.4416(6) 0.0665(3) 0.081(4) Uani 0.607(14) 1 d PU A 1 F23 F -0.2759(10) 0.3391(6) 0.0731(3) 0.113(5) Uani 0.607(14) 1 d PU A 1 F24 F -0.1671(8) 0.3999(7) 0.0475(4) 0.093(4) Uani 0.607(14) 1 d PU A 1 O1 O 0.1865(3) 0.2469(2) 0.17543(11) 0.0320(9) Uani 1 1 d . . . H1 H 0.2531 0.2490 0.1695 0.038 Uiso 1 1 calc R . . O2 O 0.0078(4) 0.0949(3) 0.16749(16) 0.0587(13) Uani 1 1 d . . . O3 O -0.0941(4) 0.3045(3) 0.15275(17) 0.0609(14) Uani 1 1 d . . . O4 O -0.0500(3) 0.2153(3) 0.22718(16) 0.0589(14) Uani 1 1 d . . . O5 O 0.0749(4) 0.4060(3) 0.19655(19) 0.0685(16) Uani 1 1 d . . . N1 N 0.2068(4) 0.3025(2) 0.08487(16) 0.0344(11) Uani 1 1 d . . . N2 N 0.2571(3) 0.2006(2) 0.09396(16) 0.0341(11) Uani 1 1 d . . . N3 N 0.3382(3) 0.2728(2) 0.24170(15) 0.0292(10) Uani 1 1 d . . . N4 N 0.2699(3) 0.1785(2) 0.25766(15) 0.0316(11) Uani 1 1 d . . . C1 C 0.2754(4) 0.2584(3) 0.07515(18) 0.0331(13) Uani 1 1 d . . . C2 C 0.3618(5) 0.2680(3) 0.0457(2) 0.0431(15) Uani 1 1 d . . . C3 C 0.3521(6) 0.2166(4) 0.0101(2) 0.0563(19) Uani 1 1 d . . . H3A H 0.4054 0.2222 -0.0092 0.084 Uiso 1 1 calc R . . H3B H 0.2907 0.2235 -0.0053 0.084 Uiso 1 1 calc R . . H3C H 0.3539 0.1714 0.0219 0.084 Uiso 1 1 calc R . . C4 C 0.3673(6) 0.3366(4) 0.0239(2) 0.0554(19) Uani 1 1 d . . . H4A H 0.3677 0.3720 0.0451 0.083 Uiso 1 1 calc R . . H4B H 0.3112 0.3422 0.0049 0.083 Uiso 1 1 calc R . . H4C H 0.4265 0.3391 0.0078 0.083 Uiso 1 1 calc R . . C5 C 0.4558(5) 0.2586(4) 0.0715(3) 0.0554(19) Uani 1 1 d . . . H5A H 0.5110 0.2674 0.0537 0.083 Uiso 1 1 calc R . . H5B H 0.4594 0.2127 0.0821 0.083 Uiso 1 1 calc R . . H5C H 0.4571 0.2898 0.0952 0.083 Uiso 1 1 calc R . . C6 C 0.1924(4) 0.3733(3) 0.0744(2) 0.0357(13) Uani 1 1 d . . . H6 H 0.2153 0.3818 0.0454 0.043 Uiso 1 1 calc R . . C7 C 0.0838(5) 0.3891(3) 0.0762(2) 0.0457(16) Uani 1 1 d . . . H7A H 0.0480 0.3609 0.0555 0.055 Uiso 1 1 calc R . . H7B H 0.0603 0.3783 0.1044 0.055 Uiso 1 1 calc R . . C8 C 0.0640(5) 0.4632(4) 0.0664(3) 0.060(2) Uani 1 1 d . . . H8A H 0.0811 0.4729 0.0371 0.072 Uiso 1 1 calc R . . H8B H -0.0055 0.4726 0.0693 0.072 Uiso 1 1 calc R . . C9 C 0.1216(5) 0.5080(3) 0.0957(3) 0.060(2) Uani 1 1 d . . . H9A H 0.0986 0.5025 0.1246 0.072 Uiso 1 1 calc R . . H9B H 0.1114 0.5552 0.0873 0.072 Uiso 1 1 calc R . . C10 C 0.2290(5) 0.4919(3) 0.0949(3) 0.0499(17) Uani 1 1 d . . . H10A H 0.2643 0.5200 0.1157 0.060 Uiso 1 1 calc R . . H10B H 0.2539 0.5021 0.0668 0.060 Uiso 1 1 calc R . . C11 C 0.2466(5) 0.4181(3) 0.1050(2) 0.0400(14) Uani 1 1 d . . . H11A H 0.3165 0.4084 0.1039 0.048 Uiso 1 1 calc R . . H11B H 0.2256 0.4086 0.1339 0.048 Uiso 1 1 calc R . . C12 C 0.3086(4) 0.1367(3) 0.0966(2) 0.0347(13) Uani 1 1 d . . . H12 H 0.3683 0.1401 0.0798 0.042 Uiso 1 1 calc R . . C13 C 0.2457(5) 0.0814(3) 0.0781(3) 0.0550(19) Uani 1 1 d . . . H13A H 0.2313 0.0911 0.0481 0.066 Uiso 1 1 calc R . . H13B H 0.1838 0.0800 0.0929 0.066 Uiso 1 1 calc R . . C14 C 0.2964(6) 0.0128(4) 0.0821(4) 0.075(3) Uani 1 1 d . . . H14A H 0.2529 -0.0226 0.0711 0.090 Uiso 1 1 calc R . . H14B H 0.3553 0.0129 0.0652 0.090 Uiso 1 1 calc R . . C15 C 0.3236(7) -0.0019(5) 0.1278(4) 0.080(3) Uani 1 1 d U . . H15A H 0.2643 -0.0064 0.1442 0.096 Uiso 1 1 calc R . . H15B H 0.3591 -0.0448 0.1296 0.096 Uiso 1 1 calc R . . C16 C 0.3851(7) 0.0528(4) 0.1462(3) 0.074(3) Uani 1 1 d . . . H16A H 0.4478 0.0533 0.1321 0.089 Uiso 1 1 calc R . . H16B H 0.3978 0.0436 0.1764 0.089 Uiso 1 1 calc R . . C17 C 0.3377(6) 0.1211(4) 0.1415(2) 0.0565(19) Uani 1 1 d . . . H17A H 0.2799 0.1227 0.1590 0.068 Uiso 1 1 calc R . . H17B H 0.3832 0.1558 0.1520 0.068 Uiso 1 1 calc R . . C18 C -0.0015(5) 0.1322(3) 0.0511(2) 0.0453(16) Uani 1 1 d . . . H18 H 0.0401 0.0944 0.0509 0.054 Uiso 1 1 calc R . . C19 C -0.1001(5) 0.1320(4) 0.0620(2) 0.0494(17) Uani 1 1 d . . . H19 H -0.1360 0.0941 0.0703 0.059 Uiso 1 1 calc R . . C20 C -0.1349(5) 0.1969(4) 0.0582(2) 0.0435(16) Uani 1 1 d . . . H20 H -0.1987 0.2110 0.0636 0.052 Uiso 1 1 calc R . . C21 C -0.0591(5) 0.2379(3) 0.0451(2) 0.0446(16) Uani 1 1 d . . . H21 H -0.0630 0.2847 0.0402 0.054 Uiso 1 1 calc R . . C22 C 0.0238(5) 0.1978(4) 0.04048(19) 0.0445(16) Uani 1 1 d . . . H22 H 0.0853 0.2126 0.0318 0.053 Uiso 1 1 calc R . . C23 C -0.0019(5) 0.1357(3) 0.1430(2) 0.0408(15) Uani 1 1 d . . . C24 C -0.0633(5) 0.2611(4) 0.1340(2) 0.0419(15) Uani 1 1 d . . . C25 C 0.3541(4) 0.2107(3) 0.25656(17) 0.0278(12) Uani 1 1 d . . . C26 C 0.4558(4) 0.1855(3) 0.26960(18) 0.0298(12) Uani 1 1 d . . . C27 C 0.4894(4) 0.2245(3) 0.3087(2) 0.0369(14) Uani 1 1 d . . . H27A H 0.4462 0.2152 0.3318 0.055 Uiso 1 1 calc R . . H27B H 0.4884 0.2725 0.3025 0.055 Uiso 1 1 calc R . . H27C H 0.5552 0.2109 0.3168 0.055 Uiso 1 1 calc R . . C28 C 0.5255(4) 0.1933(3) 0.2328(2) 0.0362(14) Uani 1 1 d . . . H28A H 0.5323 0.2408 0.2259 0.054 Uiso 1 1 calc R . . H28B H 0.4996 0.1693 0.2082 0.054 Uiso 1 1 calc R . . H28C H 0.5887 0.1749 0.2409 0.054 Uiso 1 1 calc R . . C29 C 0.4612(4) 0.1107(3) 0.2813(2) 0.0408(15) Uani 1 1 d . . . H29A H 0.5276 0.0991 0.2896 0.061 Uiso 1 1 calc R . . H29B H 0.4407 0.0836 0.2570 0.061 Uiso 1 1 calc R . . H29C H 0.4186 0.1018 0.3047 0.061 Uiso 1 1 calc R . . C30 C 0.4032(4) 0.3268(3) 0.23112(19) 0.0311(12) Uani 1 1 d . . . H30 H 0.4672 0.3187 0.2454 0.037 Uiso 1 1 calc R . . C31 C 0.3629(5) 0.3930(3) 0.2465(2) 0.0390(14) Uani 1 1 d . . . H31A H 0.3556 0.3911 0.2773 0.047 Uiso 1 1 calc R . . H31B H 0.2983 0.4006 0.2334 0.047 Uiso 1 1 calc R . . C32 C 0.4298(5) 0.4511(3) 0.2355(2) 0.0421(15) Uani 1 1 d . . . H32A H 0.4014 0.4937 0.2450 0.051 Uiso 1 1 calc R . . H32B H 0.4928 0.4452 0.2504 0.051 Uiso 1 1 calc R . . C33 C 0.4452(5) 0.4542(3) 0.1881(2) 0.0454(16) Uani 1 1 d . . . H33A H 0.3833 0.4644 0.1733 0.054 Uiso 1 1 calc R . . H33B H 0.4913 0.4904 0.1818 0.054 Uiso 1 1 calc R . . C34 C 0.4840(5) 0.3884(3) 0.1722(2) 0.0429(15) Uani 1 1 d . . . H34A H 0.5491 0.3805 0.1847 0.051 Uiso 1 1 calc R . . H34B H 0.4898 0.3905 0.1413 0.051 Uiso 1 1 calc R . . C35 C 0.4170(4) 0.3303(3) 0.18374(19) 0.0345(13) Uani 1 1 d . . . H35A H 0.3535 0.3364 0.1693 0.041 Uiso 1 1 calc R . . H35B H 0.4448 0.2876 0.1739 0.041 Uiso 1 1 calc R . . C36 C 0.2422(4) 0.1149(3) 0.27721(19) 0.0332(13) Uani 1 1 d . . . H36 H 0.2908 0.0802 0.2698 0.040 Uiso 1 1 calc R . . C37 C 0.1445(5) 0.0936(3) 0.2590(2) 0.0447(16) Uani 1 1 d . . . H37A H 0.0962 0.1287 0.2646 0.054 Uiso 1 1 calc R . . H37B H 0.1487 0.0885 0.2282 0.054 Uiso 1 1 calc R . . C38 C 0.1119(5) 0.0279(4) 0.2780(3) 0.0535(19) Uani 1 1 d . . . H38A H 0.1547 -0.0084 0.2687 0.064 Uiso 1 1 calc R . . H38B H 0.0457 0.0177 0.2676 0.064 Uiso 1 1 calc R . . C39 C 0.1132(5) 0.0298(4) 0.3260(3) 0.060(2) Uani 1 1 d . . . H39A H 0.0631 0.0612 0.3355 0.072 Uiso 1 1 calc R . . H39B H 0.0975 -0.0152 0.3369 0.072 Uiso 1 1 calc R . . C40 C 0.2104(6) 0.0514(4) 0.3439(3) 0.0552(18) Uani 1 1 d . . . H40A H 0.2596 0.0173 0.3374 0.066 Uiso 1 1 calc R . . H40B H 0.2074 0.0555 0.3748 0.066 Uiso 1 1 calc R . . C41 C 0.2387(5) 0.1193(3) 0.3247(2) 0.0415(15) Uani 1 1 d . . . H41A H 0.1912 0.1537 0.3326 0.050 Uiso 1 1 calc R . . H41B H 0.3027 0.1330 0.3362 0.050 Uiso 1 1 calc R . . C42 C 0.0703(5) 0.2778(5) 0.3289(2) 0.057(2) Uani 1 1 d . . . H42 H 0.0632 0.2318 0.3357 0.068 Uiso 1 1 calc R . . C43 C 0.1579(5) 0.3113(5) 0.3223(2) 0.066(2) Uani 1 1 d . . . H43 H 0.2204 0.2920 0.3247 0.079 Uiso 1 1 calc R . . C44 C 0.1371(6) 0.3781(5) 0.3116(3) 0.069(2) Uani 1 1 d . . . H44 H 0.1825 0.4116 0.3045 0.082 Uiso 1 1 calc R . . C45 C 0.0342(6) 0.3864(5) 0.3132(2) 0.066(2) Uani 1 1 d . . . H45 H -0.0006 0.4266 0.3081 0.079 Uiso 1 1 calc R . . C46 C -0.0050(5) 0.3246(5) 0.3236(2) 0.055(2) Uani 1 1 d . . . H46 H -0.0717 0.3155 0.3267 0.066 Uiso 1 1 calc R . . C47 C -0.0019(5) 0.2558(4) 0.2430(2) 0.0441(16) Uani 1 1 d . . . C48 C 0.0735(5) 0.3696(4) 0.2240(2) 0.0498(17) Uani 1 1 d . . . C49 C -0.1472(4) 0.2244(3) -0.07240(17) 0.0277(12) Uani 1 1 d . . . C50 C -0.1160(4) 0.1580(3) -0.07096(19) 0.0322(13) Uani 1 1 d . . . H50 H -0.1624 0.1232 -0.0728 0.039 Uiso 1 1 calc R . . C51 C -0.0186(4) 0.1415(3) -0.06689(19) 0.0348(13) Uani 1 1 d . . . C52 C 0.0512(4) 0.1899(3) -0.06471(18) 0.0355(14) Uani 1 1 d . . . H52 H 0.1176 0.1782 -0.0626 0.043 Uiso 1 1 calc R . . C53 C 0.0225(4) 0.2563(3) -0.06566(18) 0.0342(13) Uani 1 1 d . . . C54 C -0.0754(4) 0.2728(3) -0.06933(17) 0.0295(12) Uani 1 1 d . . . H54 H -0.0934 0.3186 -0.0697 0.035 Uiso 1 1 calc R . . C55 C 0.0082(5) 0.0695(4) -0.0664(3) 0.0532(18) Uani 1 1 d . . . C56 C 0.0958(4) 0.3101(3) -0.0616(2) 0.0422(15) Uani 1 1 d . . . C57 C -0.3389(4) 0.1884(3) -0.06947(18) 0.0295(12) Uani 1 1 d . . . C58 C -0.4247(4) 0.1771(3) -0.09215(19) 0.0327(13) Uani 1 1 d . . . H58 H -0.4342 0.1978 -0.1188 0.039 Uiso 1 1 calc R . . C59 C -0.4972(4) 0.1360(3) -0.0767(2) 0.0372(14) Uani 1 1 d . . . C60 C -0.4864(4) 0.1044(3) -0.0385(2) 0.0372(14) Uani 1 1 d . . . H60 H -0.5352 0.0759 -0.0282 0.045 Uiso 1 1 calc R . . C61 C -0.4020(4) 0.1155(3) -0.01571(19) 0.0350(13) Uani 1 1 d . . . C62 C -0.3297(4) 0.1565(3) -0.03089(18) 0.0320(13) Uani 1 1 d . . . H62 H -0.2724 0.1628 -0.0144 0.038 Uiso 1 1 calc R . . C63 C -0.5883(5) 0.1271(4) -0.1024(2) 0.0522(18) Uani 1 1 d . . . C64 C -0.3868(5) 0.0832(4) 0.0267(2) 0.0454(16) Uani 1 1 d . . . C65 C -0.2592(4) 0.2550(3) -0.13499(18) 0.0277(12) Uani 1 1 d . . . C66 C -0.2694(4) 0.2015(3) -0.16265(19) 0.0309(12) Uani 1 1 d . . . H66 H -0.2837 0.1586 -0.1517 0.037 Uiso 1 1 calc R . . C67 C -0.2595(4) 0.2084(3) -0.20568(19) 0.0347(13) Uani 1 1 d . . . C68 C -0.2379(4) 0.2704(3) -0.22307(19) 0.0345(13) Uani 1 1 d . . . H68 H -0.2319 0.2757 -0.2525 0.041 Uiso 1 1 calc R . . C69 C -0.2254(4) 0.3241(3) -0.19594(18) 0.0301(12) Uani 1 1 d . . . C70 C -0.2361(4) 0.3171(3) -0.15329(18) 0.0285(12) Uani 1 1 d . . . H70 H -0.2277 0.3551 -0.1357 0.034 Uiso 1 1 calc R . . C71 C -0.2698(5) 0.1486(4) -0.2331(2) 0.0450(16) Uani 1 1 d . . . C72 C -0.1991(4) 0.3917(3) -0.2125(2) 0.0395(14) Uani 1 1 d . . . C73 C -0.2963(4) 0.3116(3) -0.05963(17) 0.0275(12) Uani 1 1 d . . . C74 C -0.3740(4) 0.3488(3) -0.07586(18) 0.0306(12) Uani 1 1 d . . . H74 H -0.3993 0.3384 -0.1031 0.037 Uiso 1 1 calc R . . C75 C -0.4159(4) 0.4009(3) -0.05330(19) 0.0331(13) Uani 1 1 d . . . C76 C -0.3803(4) 0.4174(3) -0.0138(2) 0.0404(15) Uani 1 1 d . . . H76 H -0.4083 0.4528 0.0016 0.048 Uiso 1 1 calc R . . C77 C -0.3032(5) 0.3816(3) 0.0032(2) 0.0441(16) Uani 1 1 d . A . C78 C -0.2622(4) 0.3299(3) -0.0198(2) 0.0371(14) Uani 1 1 d . . . H78 H -0.2089 0.3063 -0.0078 0.045 Uiso 1 1 calc R . . C79 C -0.4974(5) 0.4400(3) -0.0719(2) 0.0413(15) Uani 1 1 d . . . C80 C -0.2647(6) 0.3975(5) 0.0468(3) 0.068(2) Uani 1 1 d U . . B1 B -0.2599(5) 0.2444(3) -0.0841(2) 0.0278(13) Uani 1 1 d . . . F23A F -0.3360(12) 0.4041(10) 0.0739(5) 0.081(5) Uani 0.393(14) 1 d PU A 2 F24A F -0.1969(12) 0.3648(9) 0.0600(4) 0.069(5) Uani 0.393(14) 1 d PU A 2 F22A F -0.2392(14) 0.4619(7) 0.0476(5) 0.093(6) Uani 0.393(14) 1 d PU 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 Ga1 0.0295(3) 0.0254(3) 0.0369(4) -0.0013(3) 0.0031(3) -0.0008(3) Ga2 0.0235(3) 0.0333(4) 0.0371(4) 0.0026(3) 0.0013(2) 0.0045(3) Fe1 0.0300(4) 0.0343(5) 0.0328(5) 0.0006(4) -0.0019(3) -0.0014(3) Fe2 0.0288(4) 0.0549(6) 0.0363(5) -0.0024(4) 0.0008(3) 0.0115(4) F1 0.176(5) 0.048(3) 0.084(3) -0.009(3) 0.005(3) 0.028(3) F2 0.112(4) 0.086(4) 0.255(6) 0.005(4) -0.018(4) 0.031(3) F3 0.148(5) 0.051(3) 0.101(4) 0.020(3) 0.019(3) 0.020(3) F4 0.068(3) 0.064(3) 0.147(5) 0.039(3) -0.019(3) -0.023(2) F5 0.049(3) 0.087(3) 0.122(4) -0.007(3) 0.014(3) -0.018(2) F6 0.114(4) 0.117(4) 0.078(3) -0.020(3) 0.003(3) -0.067(3) F7 0.062(3) 0.136(4) 0.107(4) 0.048(3) -0.023(3) -0.051(3) F8 0.071(3) 0.107(4) 0.143(5) 0.036(4) -0.049(3) -0.013(3) F9 0.084(4) 0.185(6) 0.099(4) -0.042(4) -0.027(3) -0.024(4) F10 0.058(2) 0.079(3) 0.055(2) 0.019(2) 0.0091(19) -0.020(2) F11 0.111(4) 0.093(4) 0.056(3) 0.013(3) -0.019(3) -0.049(3) F12 0.101(4) 0.100(4) 0.082(3) 0.046(3) 0.024(3) 0.047(3) F13 0.117(4) 0.090(4) 0.130(5) -0.058(3) -0.033(4) 0.040(3) F14 0.085(3) 0.093(4) 0.119(4) -0.055(3) 0.009(3) -0.031(3) F15 0.215(6) 0.099(4) 0.067(3) -0.040(3) 0.033(4) -0.042(4) F16 0.150(5) 0.075(3) 0.058(3) 0.021(3) 0.004(3) -0.023(3) F17 0.113(4) 0.052(3) 0.102(4) 0.023(3) 0.045(3) 0.019(3) F18 0.067(3) 0.075(3) 0.126(4) 0.032(3) -0.010(3) -0.030(3) F19 0.101(3) 0.110(4) 0.074(3) -0.024(3) -0.029(3) 0.065(3) F20 0.047(2) 0.086(3) 0.088(3) 0.029(3) 0.014(2) 0.023(2) F21 0.072(3) 0.056(3) 0.133(4) 0.029(3) -0.010(3) 0.011(2) F22 0.093(6) 0.083(6) 0.068(5) -0.039(5) -0.020(4) 0.032(5) F23 0.143(8) 0.115(7) 0.080(6) 0.001(5) -0.023(5) -0.003(6) F24 0.075(5) 0.116(7) 0.086(6) -0.025(5) -0.022(4) -0.006(5) O1 0.0277(19) 0.053(3) 0.0156(18) -0.0069(17) -0.0021(14) -0.0090(18) O2 0.070(3) 0.055(3) 0.051(3) 0.016(3) -0.010(2) -0.013(3) O3 0.059(3) 0.066(4) 0.058(3) -0.022(3) 0.001(2) 0.016(3) O4 0.040(3) 0.092(4) 0.045(3) -0.010(3) 0.006(2) -0.007(3) O5 0.073(4) 0.062(4) 0.071(4) 0.022(3) 0.011(3) 0.024(3) N1 0.039(3) 0.026(3) 0.038(3) 0.003(2) 0.009(2) -0.002(2) N2 0.034(3) 0.026(3) 0.042(3) -0.001(2) 0.008(2) 0.000(2) N3 0.025(2) 0.023(2) 0.040(3) 0.002(2) 0.0018(19) 0.0004(18) N4 0.027(2) 0.028(3) 0.040(3) 0.006(2) 0.001(2) -0.002(2) C1 0.035(3) 0.033(3) 0.031(3) -0.002(2) 0.005(2) -0.002(3) C2 0.041(3) 0.046(4) 0.044(4) -0.002(3) 0.016(3) -0.001(3) C3 0.071(5) 0.053(4) 0.046(4) -0.005(3) 0.016(4) 0.006(4) C4 0.057(4) 0.053(4) 0.058(5) 0.010(4) 0.025(4) -0.005(4) C5 0.040(4) 0.059(5) 0.068(5) -0.004(4) 0.017(3) -0.010(3) C6 0.035(3) 0.027(3) 0.045(4) 0.004(3) 0.004(3) 0.002(2) C7 0.040(3) 0.032(3) 0.065(5) 0.008(3) -0.008(3) -0.004(3) C8 0.047(4) 0.041(4) 0.091(6) 0.012(4) -0.013(4) 0.007(3) C9 0.060(5) 0.028(4) 0.092(6) 0.005(4) -0.008(4) 0.007(3) C10 0.056(4) 0.027(3) 0.066(5) 0.001(3) -0.014(3) -0.005(3) C11 0.039(3) 0.033(3) 0.048(4) 0.005(3) 0.001(3) -0.001(3) C12 0.036(3) 0.022(3) 0.047(4) -0.008(3) 0.011(3) 0.002(2) C13 0.042(4) 0.031(4) 0.092(6) -0.015(4) 0.006(4) 0.000(3) C14 0.053(5) 0.032(4) 0.142(9) -0.030(5) 0.018(5) -0.004(3) C15 0.082(5) 0.051(4) 0.109(6) 0.013(4) 0.030(5) 0.014(4) C16 0.094(7) 0.052(5) 0.076(6) 0.009(4) -0.001(5) 0.028(5) C17 0.075(5) 0.043(4) 0.051(4) 0.000(3) -0.005(4) 0.020(4) C18 0.050(4) 0.043(4) 0.042(4) -0.015(3) -0.008(3) 0.006(3) C19 0.050(4) 0.049(4) 0.049(4) -0.002(3) -0.014(3) -0.013(3) C20 0.034(3) 0.054(4) 0.042(4) 0.001(3) -0.012(3) -0.004(3) C21 0.058(4) 0.042(4) 0.033(3) 0.008(3) -0.015(3) 0.004(3) C22 0.042(4) 0.063(5) 0.027(3) 0.000(3) -0.001(3) -0.003(3) C23 0.041(3) 0.041(4) 0.040(4) -0.001(3) -0.007(3) -0.012(3) C24 0.036(3) 0.051(4) 0.039(4) 0.005(3) -0.003(3) -0.003(3) C25 0.025(3) 0.029(3) 0.029(3) -0.002(2) -0.001(2) 0.004(2) C26 0.026(3) 0.028(3) 0.036(3) 0.005(2) -0.002(2) 0.001(2) C27 0.033(3) 0.039(4) 0.039(3) 0.005(3) -0.004(2) -0.003(3) C28 0.027(3) 0.034(3) 0.047(4) 0.003(3) -0.001(2) 0.007(2) C29 0.032(3) 0.030(3) 0.060(4) 0.009(3) -0.003(3) 0.008(3) C30 0.029(3) 0.024(3) 0.041(3) 0.002(2) -0.004(2) -0.001(2) C31 0.041(3) 0.029(3) 0.047(4) -0.005(3) -0.003(3) 0.001(3) C32 0.053(4) 0.025(3) 0.048(4) -0.004(3) -0.005(3) -0.004(3) C33 0.058(4) 0.025(3) 0.053(4) 0.006(3) -0.010(3) -0.009(3) C34 0.055(4) 0.036(4) 0.038(4) 0.003(3) 0.001(3) -0.009(3) C35 0.041(3) 0.023(3) 0.040(3) 0.001(2) -0.001(3) 0.000(2) C36 0.033(3) 0.026(3) 0.041(3) 0.001(3) 0.002(2) 0.000(2) C37 0.037(3) 0.039(4) 0.058(4) -0.002(3) -0.002(3) -0.005(3) C38 0.043(4) 0.039(4) 0.079(5) -0.006(4) 0.009(3) -0.011(3) C39 0.054(4) 0.044(4) 0.084(6) 0.018(4) 0.019(4) -0.012(3) C40 0.061(5) 0.045(4) 0.060(5) 0.013(4) 0.013(4) 0.000(4) C41 0.044(3) 0.036(3) 0.044(4) 0.011(3) 0.005(3) -0.001(3) C42 0.057(5) 0.085(6) 0.029(4) 0.000(4) -0.003(3) 0.012(4) C43 0.046(4) 0.111(8) 0.040(4) -0.023(4) -0.006(3) 0.029(5) C44 0.057(5) 0.081(6) 0.068(5) -0.035(5) 0.002(4) 0.000(4) C45 0.063(5) 0.088(7) 0.046(4) -0.023(4) 0.003(4) 0.030(5) C46 0.039(4) 0.090(6) 0.038(4) -0.009(4) 0.007(3) 0.010(4) C47 0.034(3) 0.070(5) 0.029(3) 0.006(3) 0.009(3) 0.004(3) C48 0.044(4) 0.052(4) 0.054(4) -0.003(4) 0.004(3) 0.022(3) C49 0.033(3) 0.024(3) 0.026(3) -0.001(2) -0.003(2) 0.000(2) C50 0.035(3) 0.023(3) 0.039(3) 0.000(2) 0.000(2) 0.000(2) C51 0.037(3) 0.028(3) 0.039(3) 0.002(3) 0.002(2) 0.005(3) C52 0.029(3) 0.047(4) 0.030(3) 0.004(3) 0.000(2) 0.010(3) C53 0.037(3) 0.040(3) 0.025(3) 0.002(2) -0.001(2) -0.004(3) C54 0.032(3) 0.028(3) 0.029(3) 0.001(2) -0.001(2) 0.002(2) C55 0.048(4) 0.046(4) 0.066(5) 0.006(4) -0.001(3) 0.015(3) C56 0.036(3) 0.049(4) 0.041(4) 0.002(3) -0.001(3) -0.009(3) C57 0.030(3) 0.019(3) 0.040(3) -0.005(2) 0.003(2) 0.006(2) C58 0.037(3) 0.028(3) 0.033(3) -0.001(2) -0.003(2) 0.002(2) C59 0.031(3) 0.034(3) 0.047(4) -0.005(3) -0.001(3) 0.002(3) C60 0.034(3) 0.030(3) 0.048(4) -0.003(3) 0.006(3) -0.005(3) C61 0.037(3) 0.028(3) 0.040(3) 0.002(3) 0.003(3) 0.001(3) C62 0.035(3) 0.027(3) 0.033(3) -0.001(2) 0.001(2) 0.000(2) C63 0.051(4) 0.057(5) 0.048(4) 0.004(4) -0.009(3) -0.014(4) C64 0.042(4) 0.049(4) 0.046(4) 0.010(3) 0.002(3) -0.011(3) C65 0.024(3) 0.026(3) 0.033(3) -0.001(2) -0.003(2) 0.002(2) C66 0.024(3) 0.026(3) 0.043(3) -0.004(2) 0.000(2) 0.001(2) C67 0.025(3) 0.039(3) 0.041(3) -0.009(3) -0.002(2) 0.005(2) C68 0.024(3) 0.049(4) 0.031(3) 0.001(3) 0.005(2) 0.002(3) C69 0.024(3) 0.032(3) 0.034(3) 0.000(2) -0.002(2) 0.003(2) C70 0.026(3) 0.025(3) 0.034(3) -0.003(2) -0.002(2) 0.002(2) C71 0.034(3) 0.053(4) 0.047(4) -0.020(3) -0.001(3) 0.003(3) C72 0.040(3) 0.043(4) 0.035(3) 0.007(3) 0.005(3) 0.003(3) C73 0.029(3) 0.021(3) 0.032(3) 0.003(2) 0.002(2) -0.001(2) C74 0.032(3) 0.028(3) 0.031(3) -0.002(2) 0.000(2) 0.000(2) C75 0.035(3) 0.027(3) 0.037(3) 0.000(2) 0.004(2) 0.006(2) C76 0.041(3) 0.037(3) 0.043(4) -0.012(3) 0.002(3) 0.010(3) C77 0.045(4) 0.041(4) 0.046(4) -0.016(3) -0.005(3) 0.003(3) C78 0.036(3) 0.033(3) 0.042(4) -0.008(3) -0.005(3) 0.010(3) C79 0.048(4) 0.037(4) 0.039(4) -0.001(3) 0.001(3) 0.009(3) C80 0.066(4) 0.072(5) 0.064(4) -0.024(4) -0.014(4) 0.027(4) B1 0.031(3) 0.023(3) 0.029(3) -0.002(3) -0.002(3) 0.001(3) F23A 0.083(7) 0.100(8) 0.061(7) -0.008(6) 0.006(5) -0.007(6) F24A 0.075(7) 0.076(7) 0.056(6) -0.017(5) -0.025(5) 0.028(6) F22A 0.117(8) 0.072(7) 0.088(8) -0.011(6) -0.025(6) -0.036(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 O1 1.971(3) . ? Ga1 N2 1.986(5) . ? Ga1 N1 1.998(5) . ? Ga1 Fe1 2.3354(11) . ? Ga2 O1 1.975(3) . ? Ga2 N3 1.987(4) . ? Ga2 N4 1.993(5) . ? Ga2 Fe2 2.3148(12) . ? Fe1 C23 1.766(7) . ? Fe1 C24 1.768(8) . ? Fe1 C21 2.079(6) . ? Fe1 C22 2.088(6) . ? Fe1 C18 2.093(6) . ? Fe1 C20 2.099(6) . ? Fe1 C19 2.104(6) . ? Fe2 C47 1.746(8) . ? Fe2 C48 1.767(8) . ? Fe2 C44 2.068(8) . ? Fe2 C43 2.084(7) . ? Fe2 C42 2.089(7) . ? Fe2 C45 2.104(8) . ? Fe2 C46 2.108(7) . ? F1 C55 1.298(10) . ? F2 C55 1.258(10) . ? F3 C55 1.346(9) . ? F4 C56 1.321(8) . ? F5 C56 1.327(8) . ? F6 C56 1.293(8) . ? F7 C63 1.295(9) . ? F8 C63 1.318(10) . ? F9 C63 1.283(10) . ? F10 C64 1.323(7) . ? F11 C64 1.328(8) . ? F12 C64 1.310(9) . ? F13 C71 1.331(9) . ? F14 C71 1.308(8) . ? F15 C71 1.273(9) . ? F16 C72 1.330(8) . ? F17 C72 1.312(8) . ? F18 C72 1.301(8) . ? F19 C79 1.295(8) . ? F20 C79 1.317(8) . ? F21 C79 1.335(8) . ? F22 C80 1.217(11) . ? F23 C80 1.449(15) . ? F24 C80 1.354(13) . ? O2 C23 1.135(8) . ? O3 C24 1.142(8) . ? O4 C47 1.156(9) . ? O5 C48 1.138(9) . ? N1 C1 1.341(8) . ? N1 C6 1.466(7) . ? N2 C1 1.330(8) . ? N2 C12 1.467(7) . ? N3 C25 1.347(7) . ? N3 C30 1.452(7) . ? N4 C25 1.335(7) . ? N4 C36 1.472(7) . ? C1 C2 1.554(8) . ? C2 C3 1.535(10) . ? C2 C5 1.535(10) . ? C2 C4 1.539(10) . ? C6 C11 1.511(9) . ? C6 C7 1.543(9) . ? C7 C8 1.539(9) . ? C8 C9 1.507(11) . ? C9 C10 1.526(10) . ? C10 C11 1.529(9) . ? C12 C17 1.508(10) . ? C12 C13 1.518(9) . ? C13 C14 1.546(10) . ? C14 C15 1.523(14) . ? C15 C16 1.497(14) . ? C16 C17 1.521(10) . ? C18 C22 1.403(10) . ? C18 C19 1.420(10) . ? C19 C20 1.389(10) . ? C20 C21 1.406(10) . ? C21 C22 1.413(10) . ? C25 C26 1.545(7) . ? C26 C27 1.532(8) . ? C26 C29 1.543(8) . ? C26 C28 1.547(8) . ? C30 C31 1.525(8) . ? C30 C35 1.528(8) . ? C31 C32 1.534(9) . ? C32 C33 1.533(10) . ? C33 C34 1.513(9) . ? C34 C35 1.539(8) . ? C36 C41 1.519(9) . ? C36 C37 1.522(8) . ? C37 C38 1.521(10) . ? C38 C39 1.529(12) . ? C39 C40 1.513(11) . ? C40 C41 1.545(9) . ? C42 C43 1.408(12) . ? C42 C46 1.409(11) . ? C43 C44 1.409(13) . ? C44 C45 1.439(11) . ? C45 C46 1.394(13) . ? C49 C54 1.391(8) . ? C49 C50 1.396(8) . ? C49 B1 1.647(8) . ? C50 C51 1.393(8) . ? C51 C52 1.370(9) . ? C51 C55 1.488(9) . ? C52 C53 1.388(9) . ? C53 C54 1.399(8) . ? C53 C56 1.484(9) . ? C57 C62 1.388(8) . ? C57 C58 1.395(8) . ? C57 B1 1.643(8) . ? C58 C59 1.397(9) . ? C59 C60 1.377(9) . ? C59 C63 1.498(9) . ? C60 C61 1.379(8) . ? C61 C62 1.393(8) . ? C61 C64 1.508(9) . ? C65 C66 1.392(8) . ? C65 C70 1.411(8) . ? C65 B1 1.636(8) . ? C66 C67 1.388(9) . ? C67 C68 1.393(9) . ? C67 C71 1.488(9) . ? C68 C69 1.387(8) . ? C69 C70 1.378(8) . ? C69 C72 1.500(9) . ? C73 C78 1.390(8) . ? C73 C74 1.399(8) . ? C73 B1 1.639(8) . ? C74 C75 1.401(8) . ? C75 C76 1.379(9) . ? C75 C79 1.485(8) . ? C76 C77 1.384(9) . ? C77 C78 1.398(9) . ? C77 C80 1.511(10) . ? C80 F24A 1.213(15) . ? C80 F22A 1.335(16) . ? C80 F23A 1.334(17) . ? 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 Ga1 N2 96.29(19) . . ? O1 Ga1 N1 103.29(19) . . ? N2 Ga1 N1 66.1(2) . . ? O1 Ga1 Fe1 122.83(12) . . ? N2 Ga1 Fe1 126.86(15) . . ? N1 Ga1 Fe1 126.20(15) . . ? O1 Ga2 N3 97.90(18) . . ? O1 Ga2 N4 105.04(19) . . ? N3 Ga2 N4 66.37(19) . . ? O1 Ga2 Fe2 116.22(12) . . ? N3 Ga2 Fe2 130.03(14) . . ? N4 Ga2 Fe2 129.49(15) . . ? C23 Fe1 C24 97.8(3) . . ? C23 Fe1 C21 161.4(3) . . ? C24 Fe1 C21 96.3(3) . . ? C23 Fe1 C22 131.8(3) . . ? C24 Fe1 C22 129.0(3) . . ? C21 Fe1 C22 39.6(3) . . ? C23 Fe1 C18 98.4(3) . . ? C24 Fe1 C18 160.8(3) . . ? C21 Fe1 C18 65.8(3) . . ? C22 Fe1 C18 39.2(3) . . ? C23 Fe1 C20 126.4(3) . . ? C24 Fe1 C20 96.3(3) . . ? C21 Fe1 C20 39.3(3) . . ? C22 Fe1 C20 66.2(3) . . ? C18 Fe1 C20 65.7(3) . . ? C23 Fe1 C19 96.1(3) . . ? C24 Fe1 C19 128.1(3) . . ? C21 Fe1 C19 65.5(3) . . ? C22 Fe1 C19 66.0(3) . . ? C18 Fe1 C19 39.5(3) . . ? C20 Fe1 C19 38.6(3) . . ? C23 Fe1 Ga1 87.8(2) . . ? C24 Fe1 Ga1 87.6(2) . . ? C21 Fe1 Ga1 105.0(2) . . ? C22 Fe1 Ga1 83.85(19) . . ? C18 Fe1 Ga1 103.21(19) . . ? C20 Fe1 Ga1 144.3(2) . . ? C19 Fe1 Ga1 142.7(2) . . ? C47 Fe2 C48 94.7(3) . . ? C47 Fe2 C44 163.8(3) . . ? C48 Fe2 C44 98.4(4) . . ? C47 Fe2 C43 131.7(4) . . ? C48 Fe2 C43 131.6(4) . . ? C44 Fe2 C43 39.7(4) . . ? C47 Fe2 C42 98.9(3) . . ? C48 Fe2 C42 163.2(3) . . ? C44 Fe2 C42 66.7(4) . . ? C43 Fe2 C42 39.5(3) . . ? C47 Fe2 C45 128.2(3) . . ? C48 Fe2 C45 97.9(4) . . ? C44 Fe2 C45 40.3(3) . . ? C43 Fe2 C45 66.4(3) . . ? C42 Fe2 C45 65.9(4) . . ? C47 Fe2 C46 97.9(3) . . ? C48 Fe2 C46 129.1(3) . . ? C44 Fe2 C46 66.3(3) . . ? C43 Fe2 C46 65.8(3) . . ? C42 Fe2 C46 39.2(3) . . ? C45 Fe2 C46 38.7(3) . . ? C47 Fe2 Ga2 84.7(2) . . ? C48 Fe2 Ga2 86.8(2) . . ? C44 Fe2 Ga2 105.5(2) . . ? C43 Fe2 Ga2 85.1(2) . . ? C42 Fe2 Ga2 104.1(2) . . ? C45 Fe2 Ga2 145.8(2) . . ? C46 Fe2 Ga2 143.3(2) . . ? Ga1 O1 Ga2 163.0(2) . . ? C1 N1 C6 132.6(5) . . ? C1 N1 Ga1 92.0(4) . . ? C6 N1 Ga1 135.4(4) . . ? C1 N2 C12 133.3(5) . . ? C1 N2 Ga1 92.9(4) . . ? C12 N2 Ga1 133.8(4) . . ? C25 N3 C30 132.1(5) . . ? C25 N3 Ga2 92.4(3) . . ? C30 N3 Ga2 135.3(4) . . ? C25 N4 C36 131.7(5) . . ? C25 N4 Ga2 92.5(3) . . ? C36 N4 Ga2 134.0(4) . . ? N2 C1 N1 108.9(5) . . ? N2 C1 C2 122.7(5) . . ? N1 C1 C2 128.4(5) . . ? C3 C2 C5 111.8(6) . . ? C3 C2 C4 105.5(6) . . ? C5 C2 C4 107.4(6) . . ? C3 C2 C1 108.0(5) . . ? C5 C2 C1 108.6(5) . . ? C4 C2 C1 115.5(5) . . ? N1 C6 C11 111.4(5) . . ? N1 C6 C7 108.5(5) . . ? C11 C6 C7 109.0(5) . . ? C8 C7 C6 111.1(5) . . ? C9 C8 C7 111.1(6) . . ? C8 C9 C10 111.5(7) . . ? C9 C10 C11 110.6(6) . . ? C6 C11 C10 111.2(5) . . ? N2 C12 C17 110.6(5) . . ? N2 C12 C13 109.7(5) . . ? C17 C12 C13 110.8(6) . . ? C12 C13 C14 110.9(6) . . ? C15 C14 C13 110.6(7) . . ? C16 C15 C14 110.8(7) . . ? C15 C16 C17 112.2(8) . . ? C12 C17 C16 112.5(6) . . ? C22 C18 C19 108.0(6) . . ? C22 C18 Fe1 70.2(4) . . ? C19 C18 Fe1 70.6(4) . . ? C20 C19 C18 108.2(6) . . ? C20 C19 Fe1 70.5(4) . . ? C18 C19 Fe1 69.8(4) . . ? C19 C20 C21 108.1(6) . . ? C19 C20 Fe1 70.9(4) . . ? C21 C20 Fe1 69.6(3) . . ? C20 C21 C22 108.4(6) . . ? C20 C21 Fe1 71.1(4) . . ? C22 C21 Fe1 70.5(4) . . ? C18 C22 C21 107.3(6) . . ? C18 C22 Fe1 70.6(4) . . ? C21 C22 Fe1 69.8(4) . . ? O2 C23 Fe1 176.3(6) . . ? O3 C24 Fe1 176.7(6) . . ? N4 C25 N3 108.6(5) . . ? N4 C25 C26 129.0(5) . . ? N3 C25 C26 122.4(5) . . ? C27 C26 C29 106.7(5) . . ? C27 C26 C25 108.0(5) . . ? C29 C26 C25 114.7(5) . . ? C27 C26 C28 112.4(5) . . ? C29 C26 C28 104.7(5) . . ? C25 C26 C28 110.3(4) . . ? N3 C30 C31 109.6(5) . . ? N3 C30 C35 111.0(5) . . ? C31 C30 C35 109.5(5) . . ? C30 C31 C32 110.8(5) . . ? C33 C32 C31 110.9(5) . . ? C34 C33 C32 110.7(5) . . ? C33 C34 C35 110.8(5) . . ? C30 C35 C34 111.2(5) . . ? N4 C36 C41 112.7(5) . . ? N4 C36 C37 108.7(5) . . ? C41 C36 C37 110.2(5) . . ? C38 C37 C36 111.1(6) . . ? C37 C38 C39 112.5(6) . . ? C40 C39 C38 111.7(6) . . ? C39 C40 C41 109.6(6) . . ? C36 C41 C40 110.9(6) . . ? C43 C42 C46 107.9(8) . . ? C43 C42 Fe2 70.1(4) . . ? C46 C42 Fe2 71.1(4) . . ? C42 C43 C44 108.4(7) . . ? C42 C43 Fe2 70.5(4) . . ? C44 C43 Fe2 69.5(4) . . ? C43 C44 C45 107.3(8) . . ? C43 C44 Fe2 70.8(5) . . ? C45 C44 Fe2 71.2(5) . . ? C46 C45 C44 107.5(8) . . ? C46 C45 Fe2 70.8(5) . . ? C44 C45 Fe2 68.5(4) . . ? C45 C46 C42 109.0(7) . . ? C45 C46 Fe2 70.5(4) . . ? C42 C46 Fe2 69.7(4) . . ? O4 C47 Fe2 178.6(7) . . ? O5 C48 Fe2 178.1(7) . . ? C54 C49 C50 116.0(5) . . ? C54 C49 B1 121.3(5) . . ? C50 C49 B1 122.1(5) . . ? C51 C50 C49 121.8(5) . . ? C52 C51 C50 121.4(5) . . ? C52 C51 C55 120.4(6) . . ? C50 C51 C55 118.2(6) . . ? C51 C52 C53 118.2(5) . . ? C52 C53 C54 120.3(5) . . ? C52 C53 C56 119.8(5) . . ? C54 C53 C56 119.9(6) . . ? C49 C54 C53 122.2(5) . . ? F2 C55 F1 110.4(8) . . ? F2 C55 F3 103.1(7) . . ? F1 C55 F3 98.5(7) . . ? F2 C55 C51 114.9(7) . . ? F1 C55 C51 115.9(6) . . ? F3 C55 C51 112.1(6) . . ? F6 C56 F4 108.3(7) . . ? F6 C56 F5 104.4(6) . . ? F4 C56 F5 103.5(6) . . ? F6 C56 C53 113.3(6) . . ? F4 C56 C53 113.3(5) . . ? F5 C56 C53 113.1(6) . . ? C62 C57 C58 116.2(5) . . ? C62 C57 B1 121.2(5) . . ? C58 C57 B1 122.1(5) . . ? C57 C58 C59 121.7(6) . . ? C60 C59 C58 121.2(5) . . ? C60 C59 C63 119.9(6) . . ? C58 C59 C63 118.8(6) . . ? C59 C60 C61 117.6(6) . . ? C60 C61 C62 121.4(6) . . ? C60 C61 C64 120.0(5) . . ? C62 C61 C64 118.6(5) . . ? C57 C62 C61 121.9(5) . . ? F9 C63 F7 108.4(7) . . ? F9 C63 F8 102.0(7) . . ? F7 C63 F8 105.4(7) . . ? F9 C63 C59 113.1(7) . . ? F7 C63 C59 114.2(6) . . ? F8 C63 C59 112.7(6) . . ? F12 C64 F10 105.4(6) . . ? F12 C64 F11 105.3(6) . . ? F10 C64 F11 106.1(6) . . ? F12 C64 C61 112.4(6) . . ? F10 C64 C61 114.0(5) . . ? F11 C64 C61 112.9(6) . . ? C66 C65 C70 115.8(5) . . ? C66 C65 B1 121.6(5) . . ? C70 C65 B1 122.1(5) . . ? C67 C66 C65 122.5(6) . . ? C66 C67 C68 120.7(5) . . ? C66 C67 C71 119.3(6) . . ? C68 C67 C71 120.0(6) . . ? C69 C68 C67 117.8(5) . . ? C70 C69 C68 121.4(5) . . ? C70 C69 C72 118.2(5) . . ? C68 C69 C72 120.4(5) . . ? C69 C70 C65 121.9(5) . . ? F15 C71 F14 107.4(6) . . ? F15 C71 F13 107.4(7) . . ? F14 C71 F13 100.6(7) . . ? F15 C71 C67 115.5(7) . . ? F14 C71 C67 112.7(6) . . ? F13 C71 C67 112.0(6) . . ? F18 C72 F17 104.8(6) . . ? F18 C72 F16 106.4(6) . . ? F17 C72 F16 106.9(6) . . ? F18 C72 C69 111.9(5) . . ? F17 C72 C69 113.0(5) . . ? F16 C72 C69 113.3(6) . . ? C78 C73 C74 116.0(5) . . ? C78 C73 B1 123.2(5) . . ? C74 C73 B1 120.3(5) . . ? C73 C74 C75 122.2(5) . . ? C76 C75 C74 120.1(5) . . ? C76 C75 C79 119.2(5) . . ? C74 C75 C79 120.6(5) . . ? C75 C76 C77 119.2(6) . . ? C76 C77 C78 119.9(6) . . ? C76 C77 C80 120.1(6) . . ? C78 C77 C80 120.0(6) . . ? C73 C78 C77 122.7(6) . . ? F19 C79 F20 108.6(6) . . ? F19 C79 F21 105.1(6) . . ? F20 C79 F21 101.6(6) . . ? F19 C79 C75 114.8(5) . . ? F20 C79 C75 113.1(5) . . ? F21 C79 C75 112.5(6) . . ? F24A C80 F22 124.5(10) . . ? F24A C80 F22A 108.2(14) . . ? F22 C80 F22A 54.1(10) . . ? F24A C80 F23A 114.3(14) . . ? F22 C80 F23A 41.4(8) . . ? F22A C80 F23A 95.4(13) . . ? F24A C80 F24 41.2(9) . . ? F22 C80 F24 115.2(10) . . ? F22A C80 F24 72.6(11) . . ? F23A C80 F24 138.1(11) . . ? F24A C80 F23 57.1(11) . . ? F22 C80 F23 103.4(11) . . ? F22A C80 F23 143.2(10) . . ? F23A C80 F23 67.3(11) . . ? F24 C80 F23 98.1(10) . . ? F24A C80 C77 117.2(9) . . ? F22 C80 C77 118.3(8) . . ? F22A C80 C77 107.9(10) . . ? F23A C80 C77 111.3(9) . . ? F24 C80 C77 110.6(8) . . ? F23 C80 C77 108.7(8) . . ? C65 B1 C73 112.0(5) . . ? C65 B1 C57 113.0(5) . . ? C73 B1 C57 102.0(4) . . ? C65 B1 C49 103.0(4) . . ? C73 B1 C49 113.3(4) . . ? C57 B1 C49 114.0(5) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.028 _refine_diff_density_min -0.809 _refine_diff_density_rms 0.105