Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author ; Dr. Grigori B. Nikiforov, Chemistry Department, University of New Brunswick, E3B 6E2 Fredericton, N.B., Canada ; _publ_contact_author_phone '1-(506) 453-48-21' _publ_contact_author_fax '1-(506) 453-48-21' _publ_contact_author_email grigori@unb.ca _publ_contact_letter ; ? ; #============================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Hexafluoroantimony (V) salts of the cationic Ti(IV) fluoride non metallocene complexes [TiF3L3]+ and [TiF2L]2+ supported by the molecular ligand L. Preparation, characterization and stability. ; _publ_author_address ; Prof. Jack Passmore, Dr. Grigori B. Nikiforov, Dr. Andreas Decken Chemistry Department, University of New Brunswick, E3B 6E2 Fredericton, N.B., Canada Pof. Evgeny G. Ilyin N.S. Kurnakov Institute of General and Inorganic Chemistry of Russian Academy of Sciences. 117907 Moscow GSP-1, Leninsky Prospect 31, Russia Prof H. Donald Brooke Jenkins, Department of Chemistry, University of Warwick, Coventry, CV4 7AL, West Midlands, United Kingdom ; _publ_contact_author_name 'Dr. Grigori B. Nikiforov,' loop_ _publ_author_name 'Andreas Decken' 'Evgeny G. Ilyin' 'H.D.Brooke Jenkins' 'Grigori B. Nikiforov' 'Jack Passmore' #============================================================= data_jp_1 _database_code_depnum_ccdc_archive 'CCDC 250627' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H12 F9 N4 Sb Ti' _chemical_formula_weight 504.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ti Ti 0.2776 0.4457 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.7491(18) _cell_length_b 23.322(5) _cell_length_c 8.8016(19) _cell_angle_alpha 90.00 _cell_angle_beta 96.995(4) _cell_angle_gamma 90.00 _cell_volume 1782.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 198(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Irregular _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.881 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 2.047 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(1) _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8670 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3021 _reflns_number_gt 2272 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+3.8271P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3021 _refine_ls_number_parameters 212 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0781 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1820 _refine_ls_wR_factor_gt 0.1679 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _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 Ti Ti -0.13867(12) 0.10901(5) 0.60107(13) 0.0319(3) Uani 1 1 d . . . F1 F -0.1988(5) 0.04068(17) 0.5390(5) 0.0547(11) Uani 1 1 d . . . F2 F -0.3154(4) 0.14061(16) 0.6243(4) 0.0453(9) Uani 1 1 d . . . F3 F -0.1080(4) 0.14020(17) 0.4274(4) 0.0479(10) Uani 1 1 d . . . N1 N -0.0254(6) 0.1821(2) 0.7190(6) 0.0385(12) Uani 1 1 d . . . N2 N 0.0973(6) 0.0800(2) 0.6251(6) 0.0392(12) Uani 1 1 d . . . N3 N -0.1293(6) 0.0803(2) 0.8360(6) 0.0384(12) Uani 1 1 d . . . C1 C 0.0451(7) 0.2153(3) 0.7918(7) 0.0325(13) Uani 1 1 d . . . C2 C 0.1337(8) 0.2571(3) 0.8846(8) 0.048(2) Uani 1 1 d . . . H2A H 0.1961 0.2786 0.8223 0.073 Uiso 1 1 calc R . . H2B H 0.1988 0.2380 0.9647 0.073 Uiso 1 1 calc R . . H2C H 0.0654 0.2827 0.9289 0.073 Uiso 1 1 calc R . . C3 C 0.2240(8) 0.0706(3) 0.6316(7) 0.0388(15) Uani 1 1 d . . . C4 C 0.3877(7) 0.0585(4) 0.6386(8) 0.052(2) Uani 1 1 d . . . H4A H 0.4138 0.0268 0.7066 0.079 Uiso 1 1 calc R . . H4B H 0.4455 0.0917 0.6755 0.079 Uiso 1 1 calc R . . H4C H 0.4120 0.0489 0.5381 0.079 Uiso 1 1 calc R . . C5 C -0.1312(7) 0.0707(3) 0.9599(8) 0.0392(15) Uani 1 1 d . . . C6 C -0.1340(9) 0.0579(5) 1.1210(8) 0.062(2) Uani 1 1 d . . . H6A H -0.2060 0.0828 1.1622 0.093 Uiso 1 1 calc R . . H6B H -0.0332 0.0636 1.1753 0.093 Uiso 1 1 calc R . . H6C H -0.1646 0.0187 1.1321 0.093 Uiso 1 1 calc R . . Sb Sb 0.36772(6) 0.10457(2) 0.13517(6) 0.0503(3) Uani 1 1 d . . . F4 F 0.2354(9) 0.0986(5) 0.2780(11) 0.164(4) Uani 1 1 d . . . F5 F 0.5141(10) 0.1084(4) -0.0041(9) 0.131(3) Uani 1 1 d . . . F6 F 0.2093(11) 0.1133(4) -0.0166(12) 0.171(4) Uani 1 1 d . . . F7 F 0.3852(9) 0.1827(3) 0.1562(9) 0.127(3) Uani 1 1 d . . . F8 F 0.5337(8) 0.0948(3) 0.2865(8) 0.108(2) Uani 1 1 d . . . F9 F 0.3602(13) 0.0265(4) 0.1083(14) 0.201(5) Uani 1 1 d . . . C20 C 0.1037(10) 0.2532(4) 0.3578(10) 0.068(3) Uani 1 1 d . . . H20A H 0.0078 0.2525 0.4005 0.103 Uiso 1 1 calc R . . H20B H 0.1115 0.2197 0.2960 0.103 Uiso 1 1 calc R . . H20C H 0.1079 0.2869 0.2957 0.103 Uiso 1 1 calc R . . C21 C 0.2250(13) 0.2541(7) 0.4753(13) 0.131(7) Uani 1 1 d . . . N22 N 0.3209(13) 0.2551(11) 0.5699(13) 0.279(15) 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 Ti 0.0351(6) 0.0306(7) 0.0297(6) -0.0029(4) 0.0034(4) -0.0017(4) F1 0.066(3) 0.035(2) 0.061(3) -0.0118(19) -0.003(2) -0.0068(19) F2 0.0327(18) 0.050(2) 0.053(2) -0.0004(18) 0.0055(16) 0.0032(16) F3 0.060(2) 0.054(3) 0.030(2) 0.0061(17) 0.0054(17) -0.0005(19) N1 0.046(3) 0.031(3) 0.040(3) -0.004(2) 0.011(2) -0.004(2) N2 0.036(3) 0.045(3) 0.038(3) 0.001(2) 0.009(2) 0.006(2) N3 0.047(3) 0.037(3) 0.032(3) 0.000(2) 0.008(2) -0.005(2) C1 0.036(3) 0.030(3) 0.033(3) 0.002(3) 0.009(3) 0.002(3) C2 0.048(5) 0.047(5) 0.048(5) -0.013(3) 0.001(4) -0.009(3) C3 0.052(4) 0.036(4) 0.029(3) -0.004(3) 0.006(3) -0.005(3) C4 0.039(4) 0.066(6) 0.052(5) -0.006(4) 0.002(3) 0.004(3) C5 0.035(3) 0.039(4) 0.044(4) -0.002(3) 0.008(3) -0.001(3) C6 0.070(5) 0.080(7) 0.037(4) 0.010(4) 0.011(4) 0.006(4) Sb 0.0568(4) 0.0452(4) 0.0462(4) 0.0011(2) -0.0045(2) -0.0072(2) F4 0.090(5) 0.295(13) 0.120(7) 0.057(6) 0.062(5) 0.024(6) F5 0.128(6) 0.180(9) 0.092(5) 0.006(5) 0.041(5) -0.003(5) F6 0.134(7) 0.200(10) 0.152(8) 0.034(6) -0.095(6) -0.032(6) F7 0.148(7) 0.064(4) 0.157(7) -0.015(4) -0.027(6) 0.001(4) F8 0.082(4) 0.136(6) 0.101(5) 0.024(4) -0.016(4) 0.022(4) F9 0.263(14) 0.058(5) 0.283(14) -0.030(6) 0.030(11) -0.045(6) C20 0.064(6) 0.080(7) 0.061(6) 0.016(4) 0.003(5) -0.016(4) C21 0.052(6) 0.30(2) 0.051(6) 0.001(8) 0.025(5) -0.018(8) N22 0.057(6) 0.73(5) 0.050(6) -0.021(12) 0.001(6) 0.004(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti F3 1.743(4) . ? Ti F1 1.745(4) . ? Ti F2 1.747(3) . ? Ti N2 2.159(5) . ? Ti N3 2.166(6) . ? Ti N1 2.171(6) . ? N1 C1 1.137(8) . ? N2 C3 1.124(8) . ? N3 C5 1.115(8) . ? C1 C2 1.438(9) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.454(9) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.453(10) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? Sb F4 1.815(7) . ? Sb F6 1.815(7) . ? Sb F9 1.835(9) . ? Sb F7 1.836(7) . ? Sb F8 1.861(6) . ? Sb F5 1.880(7) . ? C20 C21 1.389(14) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 N22 1.108(15) . ? 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 F3 Ti F1 100.3(2) . . ? F3 Ti F2 99.20(19) . . ? F1 Ti F2 100.6(2) . . ? F3 Ti N2 88.24(19) . . ? F1 Ti N2 89.6(2) . . ? F2 Ti N2 166.0(2) . . ? F3 Ti N3 167.02(19) . . ? F1 Ti N3 89.5(2) . . ? F2 Ti N3 87.11(19) . . ? N2 Ti N3 83.4(2) . . ? F3 Ti N1 88.95(19) . . ? F1 Ti N1 165.8(2) . . ? F2 Ti N1 88.39(19) . . ? N2 Ti N1 79.8(2) . . ? N3 Ti N1 79.9(2) . . ? C1 N1 Ti 171.2(5) . . ? C3 N2 Ti 172.4(6) . . ? C5 N3 Ti 173.0(6) . . ? N1 C1 C2 179.6(7) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 C4 179.5(8) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 C6 179.7(9) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? F4 Sb F6 91.4(5) . . ? F4 Sb F9 89.9(5) . . ? F6 Sb F9 90.2(5) . . ? F4 Sb F7 93.4(4) . . ? F6 Sb F7 90.6(4) . . ? F9 Sb F7 176.7(4) . . ? F4 Sb F8 90.2(4) . . ? F6 Sb F8 178.3(4) . . ? F9 Sb F8 89.0(4) . . ? F7 Sb F8 90.1(3) . . ? F4 Sb F5 176.4(3) . . ? F6 Sb F5 92.0(5) . . ? F9 Sb F5 88.8(4) . . ? F7 Sb F5 87.9(4) . . ? F8 Sb F5 86.4(4) . . ? C21 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C21 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N22 C21 C20 179.3(19) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 1.628 _refine_diff_density_min -1.581 _refine_diff_density_rms 0.153 data_jp_2 _database_code_depnum_ccdc_archive 'CCDC 250628' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H20 F14 O5 Sb2 Ti' _chemical_formula_weight 777.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 9.8690(5) _cell_length_b 10.4615(5) _cell_length_c 11.9993(6) _cell_angle_alpha 80.1080(10) _cell_angle_beta 76.8470(10) _cell_angle_gamma 64.5190(10) _cell_volume 1085.16(9) _cell_formula_units_Z 2 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used 6066 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 28.29 _exptl_crystal_description Irregular _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 2.969 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7469 _diffrn_reflns_av_R_equivalents 0.0175 _diffrn_reflns_av_sigmaI/netI 0.0234 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4700 _reflns_number_gt 4393 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+1.9601P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4700 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0328 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0823 _refine_ls_wR_factor_gt 0.0810 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.49038(6) 0.51508(6) 0.25607(5) 0.02505(12) Uani 1 1 d . . . F1 F 0.4050(2) 0.4860(2) 0.40142(16) 0.0355(4) Uani 1 1 d . . . F2 F 0.5596(2) 0.5544(2) 0.10873(17) 0.0375(4) Uani 1 1 d . . . O1 O 0.6547(3) 0.5458(3) 0.3135(2) 0.0364(5) Uani 1 1 d . . . C2 C 0.6362(5) 0.6842(5) 0.3368(4) 0.0475(10) Uani 1 1 d . . . H2A H 0.7350 0.6930 0.3181 0.057 Uiso 1 1 calc R . . H2B H 0.5925 0.7012 0.4185 0.057 Uiso 1 1 calc R . . C3 C 0.5309(6) 0.7841(4) 0.2616(4) 0.0533(11) Uani 1 1 d . . . H3A H 0.4881 0.8821 0.2850 0.064 Uiso 1 1 calc R . . H3B H 0.5827 0.7830 0.1806 0.064 Uiso 1 1 calc R . . O4 O 0.4117(3) 0.7317(3) 0.2772(2) 0.0428(6) Uani 1 1 d . . . C5 C 0.2814(7) 0.8289(5) 0.2269(5) 0.0761(19) Uani 1 1 d . . . H5A H 0.3103 0.8452 0.1428 0.091 Uiso 1 1 calc R . . H5B H 0.2344 0.9212 0.2610 0.091 Uiso 1 1 calc R . . C6 C 0.1769(6) 0.7572(7) 0.2541(5) 0.084(2) Uani 1 1 d . . . H6A H 0.1363 0.7536 0.3374 0.101 Uiso 1 1 calc R . . H6B H 0.0906 0.8068 0.2117 0.101 Uiso 1 1 calc R . . O7 O 0.2703(3) 0.6142(3) 0.2175(2) 0.0464(7) Uani 1 1 d . . . C8 C 0.1906(5) 0.5229(7) 0.2290(4) 0.0673(16) Uani 1 1 d . . . H8A H 0.0952 0.5726 0.1969 0.081 Uiso 1 1 calc R . . H8B H 0.1660 0.4902 0.3105 0.081 Uiso 1 1 calc R . . C9 C 0.3003(6) 0.4035(6) 0.1623(4) 0.0606(14) Uani 1 1 d . . . H9A H 0.2672 0.3244 0.1752 0.073 Uiso 1 1 calc R . . H9B H 0.3135 0.4337 0.0792 0.073 Uiso 1 1 calc R . . O10 O 0.4409(3) 0.3618(3) 0.2067(2) 0.0400(6) Uani 1 1 d . . . C11 C 0.5690(6) 0.2409(5) 0.1573(4) 0.0545(11) Uani 1 1 d . . . H11A H 0.6188 0.2690 0.0817 0.065 Uiso 1 1 calc R . . H11B H 0.5373 0.1660 0.1481 0.065 Uiso 1 1 calc R . . C12 C 0.6705(5) 0.1928(4) 0.2432(4) 0.0499(10) Uani 1 1 d . . . H12A H 0.6277 0.1496 0.3144 0.060 Uiso 1 1 calc R . . H12B H 0.7728 0.1225 0.2126 0.060 Uiso 1 1 calc R . . O13 O 0.6779(3) 0.3231(2) 0.2647(2) 0.0340(5) Uani 1 1 d . . . C14 C 0.7660(5) 0.3014(5) 0.3537(4) 0.0474(10) Uani 1 1 d . . . H14A H 0.8625 0.2154 0.3432 0.057 Uiso 1 1 calc R . . H14B H 0.7072 0.2916 0.4310 0.057 Uiso 1 1 calc R . . C15 C 0.7956(4) 0.4310(5) 0.3384(4) 0.0457(9) Uani 1 1 d . . . H15A H 0.8214 0.4448 0.4093 0.055 Uiso 1 1 calc R . . H15B H 0.8806 0.4251 0.2741 0.055 Uiso 1 1 calc R . . Sb1 Sb 0.09269(3) 0.19776(2) 0.01778(2) 0.03353(8) Uani 1 1 d . . . Sb2 Sb 0.20501(3) 0.14233(3) 0.47570(2) 0.03612(8) Uani 1 1 d . . . F3 F 0.2932(3) 0.1353(4) 0.0424(3) 0.0684(8) Uani 1 1 d . . . F4 F 0.0376(3) 0.3532(3) 0.0998(3) 0.0598(7) Uani 1 1 d . . . F5 F -0.1074(3) 0.2636(3) -0.0078(2) 0.0557(7) Uani 1 1 d . . . F6 F 0.1530(5) 0.0416(4) -0.0632(4) 0.0951(13) Uani 1 1 d . . . F7 F 0.1350(3) 0.3016(4) -0.1186(2) 0.0661(8) Uani 1 1 d . . . F8 F 0.0436(3) 0.0970(3) 0.1531(2) 0.0577(7) Uani 1 1 d . . . F9 F 0.3885(4) 0.1540(5) 0.4341(4) 0.1094(15) Uani 1 1 d . . . F10 F 0.0132(4) 0.1400(6) 0.5098(5) 0.1213(19) Uani 1 1 d . . . F11 F 0.1896(7) 0.1707(5) 0.3214(3) 0.1251(19) Uani 1 1 d . . . F12 F 0.2952(4) -0.0544(3) 0.4647(3) 0.0683(8) Uani 1 1 d . . . F13 F 0.2162(5) 0.1182(4) 0.6289(2) 0.0859(12) Uani 1 1 d . . . F14 F 0.1143(5) 0.3373(3) 0.4875(4) 0.0931(12) 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 Ti1 0.0234(3) 0.0291(3) 0.0209(3) -0.0009(2) -0.00335(19) -0.0097(2) F1 0.0350(10) 0.0468(12) 0.0230(9) 0.0013(8) -0.0030(8) -0.0176(9) F2 0.0416(11) 0.0439(11) 0.0247(9) -0.0009(8) 0.0002(8) -0.0190(9) O1 0.0366(13) 0.0408(14) 0.0395(13) -0.0066(11) -0.0088(10) -0.0207(11) C2 0.060(2) 0.053(2) 0.043(2) -0.0165(18) 0.0086(18) -0.041(2) C3 0.076(3) 0.038(2) 0.047(2) -0.0070(17) 0.010(2) -0.032(2) O4 0.0480(15) 0.0300(12) 0.0370(14) -0.0026(10) -0.0055(11) -0.0043(11) C5 0.089(4) 0.041(2) 0.063(3) -0.014(2) -0.042(3) 0.023(3) C6 0.040(2) 0.114(5) 0.052(3) -0.036(3) -0.021(2) 0.029(3) O7 0.0275(12) 0.0670(19) 0.0345(14) 0.0049(12) -0.0090(10) -0.0113(12) C8 0.041(2) 0.123(5) 0.046(2) 0.033(3) -0.022(2) -0.049(3) C9 0.075(3) 0.105(4) 0.038(2) 0.020(2) -0.027(2) -0.071(3) O10 0.0472(15) 0.0544(16) 0.0334(13) -0.0011(11) -0.0100(11) -0.0340(13) C11 0.073(3) 0.052(2) 0.052(2) -0.021(2) 0.007(2) -0.040(2) C12 0.054(2) 0.0292(18) 0.062(3) -0.0108(17) 0.006(2) -0.0175(17) O13 0.0325(12) 0.0282(11) 0.0371(13) -0.0052(10) -0.0055(10) -0.0079(9) C14 0.0377(19) 0.050(2) 0.041(2) 0.0018(17) -0.0154(16) -0.0029(17) C15 0.0275(17) 0.067(3) 0.043(2) -0.0148(19) -0.0093(15) -0.0147(17) Sb1 0.03024(13) 0.03512(13) 0.03259(13) -0.00645(9) -0.00646(9) -0.00904(10) Sb2 0.03678(14) 0.04243(15) 0.03112(13) -0.00462(10) -0.00545(10) -0.01763(11) F3 0.0333(12) 0.083(2) 0.078(2) -0.0052(16) -0.0143(13) -0.0123(13) F4 0.0674(17) 0.0536(15) 0.0627(17) -0.0250(13) -0.0029(13) -0.0254(13) F5 0.0384(12) 0.0806(18) 0.0480(14) 0.0077(12) -0.0194(10) -0.0231(12) F6 0.095(3) 0.081(2) 0.113(3) -0.065(2) 0.011(2) -0.033(2) F7 0.0493(14) 0.090(2) 0.0432(14) 0.0120(14) 0.0004(11) -0.0247(14) F8 0.0522(14) 0.0581(15) 0.0569(15) 0.0223(12) -0.0199(12) -0.0219(12) F9 0.067(2) 0.109(3) 0.158(4) -0.025(3) 0.030(2) -0.061(2) F10 0.062(2) 0.169(5) 0.161(5) -0.085(4) 0.017(2) -0.065(3) F11 0.240(6) 0.106(3) 0.048(2) 0.0068(19) -0.056(3) -0.077(4) F12 0.093(2) 0.0443(14) 0.0665(18) -0.0091(13) -0.0051(16) -0.0298(15) F13 0.172(4) 0.072(2) 0.0401(15) 0.0091(13) -0.0417(19) -0.067(2) F14 0.116(3) 0.0414(16) 0.100(3) -0.0127(16) -0.039(2) 0.0003(17) _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 Ti1 F2 1.790(2) . ? Ti1 F1 1.793(2) . ? Ti1 O1 2.059(2) . ? Ti1 O13 2.071(2) . ? Ti1 O10 2.072(3) . ? Ti1 O7 2.089(3) . ? Ti1 O4 2.097(3) . ? O1 C15 1.447(5) . ? O1 C2 1.448(5) . ? C2 C3 1.468(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O4 1.463(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? O4 C5 1.438(5) . ? C5 C6 1.470(10) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O7 1.461(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O7 C8 1.450(6) . ? C8 C9 1.470(8) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O10 1.461(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? O10 C11 1.446(5) . ? C11 C12 1.476(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O13 1.466(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? O13 C14 1.454(5) . ? C14 C15 1.480(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? Sb1 F6 1.847(3) . ? Sb1 F4 1.859(2) . ? Sb1 F8 1.865(2) . ? Sb1 F5 1.871(2) . ? Sb1 F7 1.871(3) . ? Sb1 F3 1.875(3) . ? Sb2 F9 1.816(3) . ? Sb2 F13 1.834(3) . ? Sb2 F10 1.853(3) . ? Sb2 F11 1.854(3) . ? Sb2 F14 1.858(3) . ? Sb2 F12 1.873(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 F2 Ti1 F1 175.09(10) . . ? F2 Ti1 O1 92.99(10) . . ? F1 Ti1 O1 90.28(10) . . ? F2 Ti1 O13 91.84(10) . . ? F1 Ti1 O13 92.68(10) . . ? O1 Ti1 O13 71.11(10) . . ? F2 Ti1 O10 89.27(10) . . ? F1 Ti1 O10 90.29(10) . . ? O1 Ti1 O10 143.26(11) . . ? O13 Ti1 O10 72.16(11) . . ? F2 Ti1 O7 87.90(10) . . ? F1 Ti1 O7 87.31(10) . . ? O1 Ti1 O7 144.44(12) . . ? O13 Ti1 O7 144.43(12) . . ? O10 Ti1 O7 72.27(12) . . ? F2 Ti1 O4 87.53(10) . . ? F1 Ti1 O4 90.05(11) . . ? O1 Ti1 O4 71.49(11) . . ? O13 Ti1 O4 142.51(11) . . ? O10 Ti1 O4 145.24(12) . . ? O7 Ti1 O4 73.03(12) . . ? C15 O1 C2 114.1(3) . . ? C15 O1 Ti1 123.3(2) . . ? C2 O1 Ti1 122.6(2) . . ? O1 C2 C3 104.1(3) . . ? O1 C2 H2A 110.9 . . ? C3 C2 H2A 110.9 . . ? O1 C2 H2B 110.9 . . ? C3 C2 H2B 110.9 . . ? H2A C2 H2B 109.0 . . ? O4 C3 C2 103.8(3) . . ? O4 C3 H3A 111.0 . . ? C2 C3 H3A 111.0 . . ? O4 C3 H3B 111.0 . . ? C2 C3 H3B 111.0 . . ? H3A C3 H3B 109.0 . . ? C5 O4 C3 113.1(4) . . ? C5 O4 Ti1 117.6(3) . . ? C3 O4 Ti1 115.0(2) . . ? O4 C5 C6 104.0(4) . . ? O4 C5 H5A 111.0 . . ? C6 C5 H5A 111.0 . . ? O4 C5 H5B 111.0 . . ? C6 C5 H5B 111.0 . . ? H5A C5 H5B 109.0 . . ? O7 C6 C5 104.5(4) . . ? O7 C6 H6A 110.8 . . ? C5 C6 H6A 110.8 . . ? O7 C6 H6B 110.8 . . ? C5 C6 H6B 110.8 . . ? H6A C6 H6B 108.9 . . ? C8 O7 C6 115.6(4) . . ? C8 O7 Ti1 115.6(3) . . ? C6 O7 Ti1 116.9(3) . . ? O7 C8 C9 103.2(3) . . ? O7 C8 H8A 111.1 . . ? C9 C8 H8A 111.1 . . ? O7 C8 H8B 111.1 . . ? C9 C8 H8B 111.1 . . ? H8A C8 H8B 109.1 . . ? O10 C9 C8 103.4(3) . . ? O10 C9 H9A 111.1 . . ? C8 C9 H9A 111.1 . . ? O10 C9 H9B 111.1 . . ? C8 C9 H9B 111.1 . . ? H9A C9 H9B 109.1 . . ? C11 O10 C9 115.0(4) . . ? C11 O10 Ti1 116.6(2) . . ? C9 O10 Ti1 119.9(3) . . ? O10 C11 C12 102.5(3) . . ? O10 C11 H11A 111.3 . . ? C12 C11 H11A 111.3 . . ? O10 C11 H11B 111.3 . . ? C12 C11 H11B 111.3 . . ? H11A C11 H11B 109.2 . . ? O13 C12 C11 103.9(3) . . ? O13 C12 H12A 111.0 . . ? C11 C12 H12A 111.0 . . ? O13 C12 H12B 111.0 . . ? C11 C12 H12B 111.0 . . ? H12A C12 H12B 109.0 . . ? C14 O13 C12 113.2(3) . . ? C14 O13 Ti1 116.5(2) . . ? C12 O13 Ti1 119.8(2) . . ? O13 C14 C15 104.0(3) . . ? O13 C14 H14A 111.0 . . ? C15 C14 H14A 111.0 . . ? O13 C14 H14B 111.0 . . ? C15 C14 H14B 111.0 . . ? H14A C14 H14B 109.0 . . ? O1 C15 C14 104.8(3) . . ? O1 C15 H15A 110.8 . . ? C14 C15 H15A 110.8 . . ? O1 C15 H15B 110.8 . . ? C14 C15 H15B 110.8 . . ? H15A C15 H15B 108.9 . . ? F6 Sb1 F4 178.39(16) . . ? F6 Sb1 F8 90.43(17) . . ? F4 Sb1 F8 89.65(14) . . ? F6 Sb1 F5 91.21(16) . . ? F4 Sb1 F5 90.40(13) . . ? F8 Sb1 F5 89.40(11) . . ? F6 Sb1 F7 89.80(18) . . ? F4 Sb1 F7 90.17(14) . . ? F8 Sb1 F7 178.03(11) . . ? F5 Sb1 F7 88.64(12) . . ? F6 Sb1 F3 89.51(17) . . ? F4 Sb1 F3 88.88(14) . . ? F8 Sb1 F3 91.47(13) . . ? F5 Sb1 F3 178.87(14) . . ? F7 Sb1 F3 90.49(14) . . ? F9 Sb2 F13 92.3(2) . . ? F9 Sb2 F10 176.0(3) . . ? F13 Sb2 F10 90.9(2) . . ? F9 Sb2 F11 88.3(3) . . ? F13 Sb2 F11 178.6(2) . . ? F10 Sb2 F11 88.4(3) . . ? F9 Sb2 F14 88.5(2) . . ? F13 Sb2 F14 88.17(16) . . ? F10 Sb2 F14 89.2(2) . . ? F11 Sb2 F14 90.63(19) . . ? F9 Sb2 F12 91.87(17) . . ? F13 Sb2 F12 91.59(15) . . ? F10 Sb2 F12 90.44(19) . . ? F11 Sb2 F12 89.60(17) . . ? F14 Sb2 F12 179.54(18) . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 1.354 _refine_diff_density_min -0.973 _refine_diff_density_rms 0.111 data_jp_3 _database_code_depnum_ccdc_archive 'CCDC 250629' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H24 F14 O6 Sb2 Ti' _chemical_formula_weight 821.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 10.0613(6) _cell_length_b 10.3710(6) _cell_length_c 12.4456(7) _cell_angle_alpha 84.0980(10) _cell_angle_beta 77.8200(10) _cell_angle_gamma 67.2570(10) _cell_volume 1170.39(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6596 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 28.35 _exptl_crystal_description Irregular _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.375 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.125 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.332 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_absorpt_coefficient_mu 2.763 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8094 _diffrn_reflns_av_R_equivalents 0.0177 _diffrn_reflns_av_sigmaI/netI 0.0249 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5082 _reflns_number_gt 4786 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+2.6488P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5082 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0280 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0701 _refine_ls_wR_factor_gt 0.0694 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _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 Ti Ti 1.02544(5) 0.91131(5) 0.24550(4) 0.01446(11) Uani 1 1 d . . . F1 F 1.11738(19) 0.9315(2) 0.10839(14) 0.0228(4) Uani 1 1 d . . . F2 F 0.93297(19) 0.89135(19) 0.38275(14) 0.0212(4) Uani 1 1 d . . . O1 O 1.1101(2) 0.6932(2) 0.23755(18) 0.0190(4) Uani 1 1 d . . . C2 C 1.0038(3) 0.6265(3) 0.2522(3) 0.0226(6) Uani 1 1 d . . . H2A H 0.9469 0.6367 0.3283 0.027 Uiso 1 1 calc R . . H2B H 1.0527 0.5258 0.2353 0.027 Uiso 1 1 calc R . . C3 C 0.9076(4) 0.7039(3) 0.1718(3) 0.0239(6) Uani 1 1 d . . . H3A H 0.9582 0.6763 0.0955 0.029 Uiso 1 1 calc R . . H3B H 0.8153 0.6864 0.1873 0.029 Uiso 1 1 calc R . . O4 O 0.8790(2) 0.8502(2) 0.18810(18) 0.0205(4) Uani 1 1 d . . . C5 C 0.7470(3) 0.9528(3) 0.1546(3) 0.0211(6) Uani 1 1 d . . . H5A H 0.6664 0.9175 0.1689 0.025 Uiso 1 1 calc R . . H5B H 0.7659 0.9790 0.0757 0.025 Uiso 1 1 calc R . . C6 C 0.7124(3) 1.0738(3) 0.2262(3) 0.0220(6) Uani 1 1 d . . . H6A H 0.6374 1.1591 0.2008 0.026 Uiso 1 1 calc R . . H6B H 0.6761 1.0527 0.3036 0.026 Uiso 1 1 calc R . . O7 O 0.8518(2) 1.0918(2) 0.21506(17) 0.0176(4) Uani 1 1 d . . . C8 C 0.8635(4) 1.2111(3) 0.1436(3) 0.0222(6) Uani 1 1 d . . . H8A H 0.8071 1.2245 0.0843 0.027 Uiso 1 1 calc R . . H8B H 0.9675 1.1894 0.1089 0.027 Uiso 1 1 calc R . . C9 C 0.8064(4) 1.3458(3) 0.2065(3) 0.0254(7) Uani 1 1 d . . . H9A H 0.7684 1.4261 0.1561 0.030 Uiso 1 1 calc R . . H9B H 0.7238 1.3460 0.2661 0.030 Uiso 1 1 calc R . . O10 O 0.9162(3) 1.3630(3) 0.2529(2) 0.0280(5) Uani 1 1 d . . . C11 C 0.9183(4) 1.3214(4) 0.3650(3) 0.0283(7) Uani 1 1 d . . . H11B H 0.8260 1.3824 0.4104 0.034 Uiso 1 1 calc R . . H11A H 1.0003 1.3362 0.3870 0.034 Uiso 1 1 calc R . . C12 C 0.9351(3) 1.1712(3) 0.3897(3) 0.0208(6) Uani 1 1 d . . . H12A H 0.9565 1.1445 0.4647 0.025 Uiso 1 1 calc R . . H12B H 0.8419 1.1609 0.3875 0.025 Uiso 1 1 calc R . . O13 O 1.0538(2) 1.0775(2) 0.31001(17) 0.0181(4) Uani 1 1 d . . . C14 C 1.1981(3) 1.0619(3) 0.3290(3) 0.0223(6) Uani 1 1 d . . . H14A H 1.2034 1.0437 0.4079 0.027 Uiso 1 1 calc R . . H14B H 1.2188 1.1472 0.3045 0.027 Uiso 1 1 calc R . . C15 C 1.3039(3) 0.9400(3) 0.2625(3) 0.0233(6) Uani 1 1 d . . . H15A H 1.3171 0.9652 0.1831 0.028 Uiso 1 1 calc R . . H15B H 1.4005 0.9038 0.2854 0.028 Uiso 1 1 calc R . . O16 O 1.2339(2) 0.8378(2) 0.28655(18) 0.0201(4) Uani 1 1 d . . . C17 C 1.3320(3) 0.6942(3) 0.2584(3) 0.0272(7) Uani 1 1 d . . . H17A H 1.4135 0.6605 0.2998 0.033 Uiso 1 1 calc R . . H17B H 1.3730 0.6864 0.1787 0.033 Uiso 1 1 calc R . . C18 C 1.2338(4) 0.6154(3) 0.2918(3) 0.0255(7) Uani 1 1 d . . . H18A H 1.2829 0.5179 0.2664 0.031 Uiso 1 1 calc R . . H18B H 1.2019 0.6142 0.3727 0.031 Uiso 1 1 calc R . . Sb1 Sb 0.58783(2) 0.72814(2) 0.503039(17) 0.01962(7) Uani 1 1 d . . . F3 F 0.5771(2) 0.8746(2) 0.58409(19) 0.0344(5) Uani 1 1 d . . . F4 F 0.6409(2) 0.8169(2) 0.37146(18) 0.0384(5) Uani 1 1 d . . . F5 F 0.5985(3) 0.5826(2) 0.4199(2) 0.0429(6) Uani 1 1 d . . . F6 F 0.5315(2) 0.6378(2) 0.63265(18) 0.0340(5) Uani 1 1 d . . . F7 F 0.7863(2) 0.6335(2) 0.51353(19) 0.0358(5) Uani 1 1 d . . . F8 F 0.3888(2) 0.8197(2) 0.49282(18) 0.0319(5) Uani 1 1 d . . . Sb2 Sb 0.64994(2) 0.71118(2) 0.945345(18) 0.02424(7) Uani 1 1 d . . . F9 F 0.7786(4) 0.5303(3) 0.9674(2) 0.0665(9) Uani 1 1 d . . . F10 F 0.4979(4) 0.6508(4) 0.9457(3) 0.0706(9) Uani 1 1 d . . . F11 F 0.5237(3) 0.8923(3) 0.9174(3) 0.0607(8) Uani 1 1 d . . . F12 F 0.7951(3) 0.7819(3) 0.94337(19) 0.0460(6) Uani 1 1 d . . . F13 F 0.5952(3) 0.7342(3) 1.09797(19) 0.0464(6) Uani 1 1 d . . . F14 F 0.7111(3) 0.6851(2) 0.79301(18) 0.0445(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 Ti 0.0140(2) 0.0146(2) 0.0149(2) -0.00029(18) -0.00409(18) -0.00484(19) F1 0.0219(9) 0.0252(10) 0.0185(9) 0.0011(7) -0.0018(7) -0.0074(7) F2 0.0234(9) 0.0234(9) 0.0174(8) 0.0000(7) -0.0022(7) -0.0103(7) O1 0.0171(10) 0.0139(10) 0.0253(11) -0.0005(8) -0.0061(8) -0.0039(8) C2 0.0209(14) 0.0174(15) 0.0296(16) -0.0020(12) -0.0029(12) -0.0076(12) C3 0.0229(15) 0.0169(15) 0.0341(17) -0.0063(13) -0.0079(13) -0.0071(12) O4 0.0184(10) 0.0165(10) 0.0285(11) -0.0022(9) -0.0101(9) -0.0052(8) C5 0.0167(13) 0.0209(15) 0.0268(15) -0.0005(12) -0.0102(12) -0.0050(12) C6 0.0144(13) 0.0232(16) 0.0278(16) -0.0010(12) -0.0055(11) -0.0053(12) O7 0.0155(9) 0.0161(10) 0.0226(10) 0.0029(8) -0.0075(8) -0.0063(8) C8 0.0266(15) 0.0200(15) 0.0204(14) 0.0054(12) -0.0075(12) -0.0090(13) C9 0.0276(16) 0.0172(15) 0.0318(17) 0.0063(13) -0.0113(13) -0.0076(13) O10 0.0333(13) 0.0237(12) 0.0319(13) 0.0035(10) -0.0105(10) -0.0148(10) C11 0.0328(17) 0.0206(16) 0.0324(18) -0.0062(13) -0.0109(14) -0.0071(14) C12 0.0235(14) 0.0179(15) 0.0201(14) -0.0043(11) -0.0050(12) -0.0053(12) O13 0.0174(10) 0.0165(10) 0.0214(10) -0.0029(8) -0.0061(8) -0.0056(8) C14 0.0201(14) 0.0231(16) 0.0292(16) 0.0026(13) -0.0118(12) -0.0112(12) C15 0.0174(14) 0.0238(16) 0.0305(17) 0.0028(13) -0.0076(12) -0.0091(12) O16 0.0167(10) 0.0167(10) 0.0275(11) 0.0020(8) -0.0088(8) -0.0052(8) C17 0.0186(14) 0.0207(16) 0.0392(19) -0.0055(14) -0.0116(13) 0.0002(12) C18 0.0268(16) 0.0170(15) 0.0314(17) 0.0011(12) -0.0153(13) -0.0022(12) Sb1 0.01562(10) 0.01887(11) 0.02224(11) 0.00005(8) -0.00402(7) -0.00405(8) F3 0.0346(11) 0.0286(11) 0.0431(12) -0.0101(9) -0.0092(9) -0.0120(9) F4 0.0350(11) 0.0424(13) 0.0296(11) 0.0097(9) 0.0008(9) -0.0119(10) F5 0.0449(13) 0.0320(12) 0.0519(14) -0.0176(11) -0.0127(11) -0.0086(10) F6 0.0307(10) 0.0360(12) 0.0341(11) 0.0130(9) -0.0080(9) -0.0135(9) F7 0.0176(9) 0.0371(12) 0.0454(13) 0.0025(10) -0.0078(9) -0.0022(8) F8 0.0182(9) 0.0374(12) 0.0355(11) 0.0024(9) -0.0083(8) -0.0045(8) Sb2 0.02589(12) 0.02264(12) 0.02559(12) -0.00181(8) -0.00922(9) -0.00804(9) F9 0.079(2) 0.0361(14) 0.0439(15) 0.0132(12) -0.0052(14) 0.0152(14) F10 0.082(2) 0.089(2) 0.080(2) 0.0110(18) -0.0313(18) -0.070(2) F11 0.0447(15) 0.0324(14) 0.097(2) -0.0024(14) -0.0310(15) 0.0037(11) F12 0.0367(12) 0.0817(19) 0.0337(12) -0.0071(12) -0.0047(10) -0.0371(13) F13 0.0404(13) 0.0730(18) 0.0304(12) -0.0186(12) 0.0087(10) -0.0299(13) F14 0.0843(19) 0.0358(13) 0.0231(10) 0.0008(9) -0.0174(11) -0.0295(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 Ti F1 1.7949(18) . ? Ti F2 1.7978(18) . ? Ti O7 2.075(2) . ? Ti O4 2.084(2) . ? Ti O1 2.091(2) . ? Ti O16 2.092(2) . ? Ti O13 2.112(2) . ? O1 C2 1.456(4) . ? O1 C18 1.457(4) . ? C2 C3 1.492(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O4 1.459(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? O4 C5 1.455(3) . ? C5 C6 1.500(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O7 1.461(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O7 C8 1.475(4) . ? C8 C9 1.519(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O10 1.425(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? O10 C11 1.419(4) . ? C11 C12 1.507(5) . ? C11 H11B 0.9900 . ? C11 H11A 0.9900 . ? C12 O13 1.468(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? O13 C14 1.464(3) . ? C14 C15 1.490(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O16 1.460(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? O16 C17 1.463(4) . ? C17 C18 1.482(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? Sb1 F3 1.865(2) . ? Sb1 F5 1.873(2) . ? Sb1 F6 1.875(2) . ? Sb1 F4 1.875(2) . ? Sb1 F7 1.8809(19) . ? Sb1 F8 1.8819(19) . ? Sb2 F9 1.854(2) . ? Sb2 F10 1.862(3) . ? Sb2 F11 1.863(2) . ? Sb2 F12 1.866(2) . ? Sb2 F13 1.876(2) . ? Sb2 F14 1.879(2) . ? 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 F1 Ti F2 179.87(11) . . ? F1 Ti O7 87.40(9) . . ? F2 Ti O7 92.47(9) . . ? F1 Ti O4 92.09(9) . . ? F2 Ti O4 87.85(9) . . ? O7 Ti O4 72.64(8) . . ? F1 Ti O1 92.89(9) . . ? F2 Ti O1 87.20(9) . . ? O7 Ti O1 143.83(9) . . ? O4 Ti O1 71.21(8) . . ? F1 Ti O16 85.49(9) . . ? F2 Ti O16 94.63(9) . . ? O7 Ti O16 143.31(9) . . ? O4 Ti O16 143.49(9) . . ? O1 Ti O16 72.55(8) . . ? F1 Ti O13 95.09(9) . . ? F2 Ti O13 84.90(8) . . ? O7 Ti O13 73.63(8) . . ? O4 Ti O13 145.10(8) . . ? O1 Ti O13 142.09(8) . . ? O16 Ti O13 71.24(8) . . ? C2 O1 C18 112.6(2) . . ? C2 O1 Ti 116.61(17) . . ? C18 O1 Ti 117.58(18) . . ? O1 C2 C3 103.3(2) . . ? O1 C2 H2A 111.1 . . ? C3 C2 H2A 111.1 . . ? O1 C2 H2B 111.1 . . ? C3 C2 H2B 111.1 . . ? H2A C2 H2B 109.1 . . ? O4 C3 C2 103.7(2) . . ? O4 C3 H3A 111.0 . . ? C2 C3 H3A 111.0 . . ? O4 C3 H3B 111.0 . . ? C2 C3 H3B 111.0 . . ? H3A C3 H3B 109.0 . . ? C5 O4 C3 116.3(2) . . ? C5 O4 Ti 121.34(18) . . ? C3 O4 Ti 122.22(17) . . ? O4 C5 C6 102.3(2) . . ? O4 C5 H5A 111.3 . . ? C6 C5 H5A 111.3 . . ? O4 C5 H5B 111.3 . . ? C6 C5 H5B 111.3 . . ? H5A C5 H5B 109.2 . . ? O7 C6 C5 104.5(2) . . ? O7 C6 H6A 110.8 . . ? C5 C6 H6A 110.8 . . ? O7 C6 H6B 110.8 . . ? C5 C6 H6B 110.8 . . ? H6A C6 H6B 108.9 . . ? C6 O7 C8 114.6(2) . . ? C6 O7 Ti 114.45(17) . . ? C8 O7 Ti 125.92(18) . . ? O7 C8 C9 112.4(3) . . ? O7 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? O7 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.9 . . ? O10 C9 C8 112.7(3) . . ? O10 C9 H9A 109.1 . . ? C8 C9 H9A 109.1 . . ? O10 C9 H9B 109.1 . . ? C8 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? C11 O10 C9 116.3(3) . . ? O10 C11 C12 114.3(3) . . ? O10 C11 H11B 108.7 . . ? C12 C11 H11B 108.7 . . ? O10 C11 H11A 108.7 . . ? C12 C11 H11A 108.7 . . ? H11B C11 H11A 107.6 . . ? O13 C12 C11 111.1(3) . . ? O13 C12 H12A 109.4 . . ? C11 C12 H12A 109.4 . . ? O13 C12 H12B 109.4 . . ? C11 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? C14 O13 C12 111.5(2) . . ? C14 O13 Ti 120.33(18) . . ? C12 O13 Ti 120.10(17) . . ? O13 C14 C15 104.9(2) . . ? O13 C14 H14A 110.8 . . ? C15 C14 H14A 110.8 . . ? O13 C14 H14B 110.8 . . ? C15 C14 H14B 110.8 . . ? H14A C14 H14B 108.8 . . ? O16 C15 C14 103.1(2) . . ? O16 C15 H15A 111.2 . . ? C14 C15 H15A 111.2 . . ? O16 C15 H15B 111.2 . . ? C14 C15 H15B 111.2 . . ? H15A C15 H15B 109.1 . . ? C15 O16 C17 114.5(2) . . ? C15 O16 Ti 112.92(17) . . ? C17 O16 Ti 117.82(18) . . ? O16 C17 C18 102.8(3) . . ? O16 C17 H17A 111.2 . . ? C18 C17 H17A 111.2 . . ? O16 C17 H17B 111.2 . . ? C18 C17 H17B 111.2 . . ? H17A C17 H17B 109.1 . . ? O1 C18 C17 103.3(3) . . ? O1 C18 H18A 111.1 . . ? C17 C18 H18A 111.1 . . ? O1 C18 H18B 111.1 . . ? C17 C18 H18B 111.1 . . ? H18A C18 H18B 109.1 . . ? F3 Sb1 F5 179.23(11) . . ? F3 Sb1 F6 90.49(10) . . ? F5 Sb1 F6 90.24(11) . . ? F3 Sb1 F4 90.76(11) . . ? F5 Sb1 F4 88.50(12) . . ? F6 Sb1 F4 178.38(10) . . ? F3 Sb1 F7 90.34(10) . . ? F5 Sb1 F7 89.89(11) . . ? F6 Sb1 F7 90.34(10) . . ? F4 Sb1 F7 90.67(10) . . ? F3 Sb1 F8 90.48(10) . . ? F5 Sb1 F8 89.29(10) . . ? F6 Sb1 F8 89.02(9) . . ? F4 Sb1 F8 89.95(10) . . ? F7 Sb1 F8 178.96(10) . . ? F9 Sb2 F10 91.89(17) . . ? F9 Sb2 F11 177.79(14) . . ? F10 Sb2 F11 88.42(15) . . ? F9 Sb2 F12 91.35(15) . . ? F10 Sb2 F12 176.76(15) . . ? F11 Sb2 F12 88.34(13) . . ? F9 Sb2 F13 89.90(13) . . ? F10 Sb2 F13 90.71(13) . . ? F11 Sb2 F13 92.28(14) . . ? F12 Sb2 F13 89.44(10) . . ? F9 Sb2 F14 88.71(12) . . ? F10 Sb2 F14 90.57(14) . . ? F11 Sb2 F14 89.10(13) . . ? F12 Sb2 F14 89.35(11) . . ? F13 Sb2 F14 178.14(12) . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 0.941 _refine_diff_density_min -1.023 _refine_diff_density_rms 0.119