# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dieter Lentz' _publ_contact_author_email LENTZ@CHEMIE.FU-BERLIN.DE _publ_section_title ; Synthesis and Reactions of Hydroxobis(?5-pentamethylcyclopenta-dienyl) (trifluoroethenyl)titanium(IV) ; loop_ _publ_author_name 'Dieter Lentz' 'Rainer Kickbusch' # Attachment '1b.CIF' data_rk6m _database_code_depnum_ccdc_archive 'CCDC 757334' #TrackingRef '1b.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Chloro-bis(ethyltetramethylcyclopentadienyl)(trifluoro- ethenyl)titanium(IV) ; _chemical_name_common ;Chloro-bis(ethyltetramethylcyclopentadienyl)(trifluoro- ethenyl)titanium(IV) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H34 Cl F3 Ti' _chemical_formula_weight 462.86 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' F F 0.0171 0.0103 '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' Ti Ti 0.2776 0.4457 '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 8.4533(17) _cell_length_b 9.1295(18) _cell_length_c 15.551(3) _cell_angle_alpha 77.122(4) _cell_angle_beta 82.512(4) _cell_angle_gamma 74.816(4) _cell_volume 1125.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 971 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 30.44 _exptl_crystal_description platelett _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 0.531 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.847 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_special_details ; the ratio of the minimum to maximum transmission is given by the program ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER-AXS SMART CCD' _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 14011 _diffrn_reflns_av_R_equivalents 0.0180 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 30.54 _reflns_number_total 6657 _reflns_number_gt 5453 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker-AXS)' _computing_cell_refinement 'SAINT (Bruker-AXS)' _computing_data_reduction 'SAINT (Bruker-AXS)' _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^)+(0.0452P)^2^+0.3771P] 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 6657 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0925 _refine_ls_wR_factor_gt 0.0864 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.002 _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 0.78178(3) 0.86726(3) 0.764140(15) 0.01624(6) Uani 1 1 d . . . Cl2 Cl 1.05331(4) 0.86927(4) 0.70908(2) 0.02691(9) Uani 1 1 d . . . C1 C 0.82271(16) 0.85434(16) 0.90106(9) 0.0209(3) Uani 1 1 d . . . C2 C 0.94955(17) 0.84501(17) 0.94501(9) 0.0239(3) Uani 1 1 d . . . C1R C 0.70804(17) 1.10043(16) 0.65534(10) 0.0246(3) Uani 1 1 d . . . C2R C 0.76960(18) 1.14323(16) 0.72485(11) 0.0279(3) Uani 1 1 d . . . C3R C 0.65943(18) 1.12565(16) 0.80081(10) 0.0260(3) Uani 1 1 d . . . C4R C 0.53110(16) 1.06989(15) 0.77989(9) 0.0206(3) Uani 1 1 d . . . C5R C 0.55778(16) 1.05964(15) 0.68912(9) 0.0193(2) Uani 1 1 d . . . C6R C 0.84604(17) 0.64132(16) 0.69714(9) 0.0219(3) Uani 1 1 d . . . C7R C 0.90547(16) 0.58939(15) 0.78281(9) 0.0212(3) Uani 1 1 d . . . C8R C 0.76871(16) 0.60515(15) 0.84597(9) 0.0199(3) Uani 1 1 d . . . C9R C 0.62439(16) 0.67093(15) 0.79995(9) 0.0205(3) Uani 1 1 d . . . C10R C 0.67231(17) 0.69016(15) 0.70752(9) 0.0214(3) Uani 1 1 d . . . C11R C 0.7789(2) 1.1133(2) 0.56097(11) 0.0409(4) Uani 1 1 d . . . H11A H 0.7484 1.0401 0.5346 0.061 Uiso 1 1 calc R . . H11B H 0.8965 1.0919 0.5593 0.061 Uiso 1 1 calc R . . H11C H 0.7370 1.2162 0.5287 0.061 Uiso 1 1 calc R . . C12R C 0.9115(2) 1.2151(2) 0.71831(16) 0.0473(5) Uani 1 1 d . . . H12A H 0.8714 1.3224 0.7216 0.071 Uiso 1 1 calc R . . H12B H 0.9748 1.2063 0.6630 0.071 Uiso 1 1 calc R . . H12C H 0.9796 1.1627 0.7661 0.071 Uiso 1 1 calc R . . C13R C 0.6600(2) 1.1880(2) 0.88273(13) 0.0415(4) Uani 1 1 d . . . H13A H 0.6172 1.2982 0.8707 0.062 Uiso 1 1 calc R . . H13B H 0.7705 1.1640 0.8998 0.062 Uiso 1 1 calc R . . H13C H 0.5926 1.1414 0.9299 0.062 Uiso 1 1 calc R . . C14R C 0.37523(18) 1.0613(2) 0.83816(10) 0.0313(3) Uani 1 1 d . . . H14A H 0.4021 0.9962 0.8945 0.047 Uiso 1 1 calc R . . H14B H 0.3069 1.0191 0.8106 0.047 Uiso 1 1 calc R . . H14C H 0.3175 1.1634 0.8465 0.047 Uiso 1 1 calc R . . C15R C 0.42289(17) 1.06460(17) 0.63358(10) 0.0242(3) Uani 1 1 d . . . H15A H 0.3514 1.0004 0.6664 0.029 Uiso 1 1 calc R . . H15B H 0.4695 1.0256 0.5803 0.029 Uiso 1 1 calc R . . C16R C 0.32440(19) 1.23347(19) 0.60925(11) 0.0321(3) Uani 1 1 d . . . H16A H 0.2780 1.2708 0.6623 0.048 Uiso 1 1 calc R . . H16B H 0.2377 1.2389 0.5736 0.048 Uiso 1 1 calc R . . H16C H 0.3960 1.2961 0.5767 0.048 Uiso 1 1 calc R . . C17R C 0.9481(2) 0.6324(2) 0.61065(11) 0.0337(3) Uani 1 1 d . . . H17A H 1.0599 0.6291 0.6185 0.051 Uiso 1 1 calc R . . H17B H 0.9053 0.7217 0.5669 0.051 Uiso 1 1 calc R . . H17C H 0.9443 0.5405 0.5915 0.051 Uiso 1 1 calc R . . C18R C 1.07991(18) 0.51472(18) 0.80492(12) 0.0310(3) Uani 1 1 d . . . H18A H 1.0922 0.4054 0.8256 0.046 Uiso 1 1 calc R . . H18B H 1.1062 0.5587 0.8503 0.046 Uiso 1 1 calc R . . H18C H 1.1528 0.5323 0.7530 0.046 Uiso 1 1 calc R . . C19R C 0.7730(2) 0.53520(18) 0.94287(10) 0.0293(3) Uani 1 1 d . . . H19A H 0.6745 0.5836 0.9741 0.044 Uiso 1 1 calc R . . H19B H 0.8668 0.5511 0.9650 0.044 Uiso 1 1 calc R . . H19C H 0.7805 0.4262 0.9515 0.044 Uiso 1 1 calc R . . C20R C 0.45239(18) 0.68256(19) 0.84205(11) 0.0314(3) Uani 1 1 d . . . H20A H 0.4299 0.5818 0.8562 0.047 Uiso 1 1 calc R . . H20B H 0.3758 0.7508 0.8017 0.047 Uiso 1 1 calc R . . H20C H 0.4415 0.7225 0.8952 0.047 Uiso 1 1 calc R . . C21R C 0.5592(2) 0.70784(17) 0.63681(11) 0.0294(3) Uani 1 1 d . . . H21A H 0.6003 0.7632 0.5813 0.035 Uiso 1 1 calc R . . H21B H 0.4507 0.7676 0.6529 0.035 Uiso 1 1 calc R . . C22R C 0.5480(3) 0.5484(2) 0.62552(14) 0.0457(5) Uani 1 1 d . . . H22A H 0.6532 0.4936 0.6036 0.068 Uiso 1 1 calc R . . H22B H 0.4679 0.5611 0.5843 0.068 Uiso 1 1 calc R . . H22C H 0.5158 0.4906 0.6816 0.068 Uiso 1 1 calc R . . F1 F 0.67987(10) 0.85774(11) 0.95777(6) 0.0292(2) Uani 1 1 d . . . F2 F 0.94560(11) 0.84068(12) 1.03210(6) 0.0335(2) Uani 1 1 d . . . F3 F 1.10238(11) 0.83947(13) 0.91025(7) 0.0366(2) 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 0.01466(11) 0.01671(11) 0.01784(11) -0.00339(8) -0.00216(8) -0.00418(8) Cl2 0.01792(15) 0.02733(17) 0.03504(19) -0.00507(14) 0.00182(13) -0.00744(12) C1 0.0195(6) 0.0213(6) 0.0221(6) -0.0058(5) -0.0012(5) -0.0039(5) C2 0.0233(6) 0.0261(7) 0.0231(7) -0.0074(5) -0.0042(5) -0.0039(5) C1R 0.0213(6) 0.0206(6) 0.0273(7) 0.0029(5) -0.0012(5) -0.0037(5) C2R 0.0225(6) 0.0162(6) 0.0454(9) -0.0020(6) -0.0095(6) -0.0053(5) C3R 0.0278(7) 0.0175(6) 0.0338(8) -0.0084(5) -0.0117(6) -0.0002(5) C4R 0.0186(6) 0.0191(6) 0.0227(6) -0.0047(5) -0.0036(5) -0.0004(5) C5R 0.0184(6) 0.0172(6) 0.0216(6) -0.0024(5) -0.0041(5) -0.0031(5) C6R 0.0262(7) 0.0187(6) 0.0219(6) -0.0065(5) -0.0002(5) -0.0062(5) C7R 0.0209(6) 0.0163(6) 0.0262(7) -0.0036(5) -0.0042(5) -0.0033(5) C8R 0.0227(6) 0.0171(6) 0.0211(6) -0.0019(5) -0.0040(5) -0.0071(5) C9R 0.0190(6) 0.0190(6) 0.0249(6) -0.0039(5) -0.0022(5) -0.0069(5) C10R 0.0256(6) 0.0180(6) 0.0228(6) -0.0042(5) -0.0068(5) -0.0064(5) C11R 0.0318(8) 0.0460(10) 0.0315(8) 0.0097(7) 0.0054(7) -0.0043(7) C12R 0.0308(8) 0.0257(8) 0.0882(16) -0.0025(9) -0.0159(9) -0.0134(7) C13R 0.0499(10) 0.0306(8) 0.0480(11) -0.0211(8) -0.0239(9) 0.0041(7) C14R 0.0227(7) 0.0369(8) 0.0275(7) -0.0058(6) 0.0022(6) 0.0020(6) C15R 0.0242(7) 0.0256(7) 0.0235(7) -0.0057(5) -0.0066(5) -0.0039(5) C16R 0.0290(7) 0.0318(8) 0.0322(8) -0.0045(6) -0.0107(6) 0.0011(6) C17R 0.0411(9) 0.0352(8) 0.0265(8) -0.0121(6) 0.0068(7) -0.0118(7) C18R 0.0206(7) 0.0255(7) 0.0437(9) -0.0037(6) -0.0060(6) -0.0008(5) C19R 0.0381(8) 0.0279(7) 0.0220(7) 0.0012(6) -0.0068(6) -0.0111(6) C20R 0.0209(7) 0.0338(8) 0.0399(9) -0.0060(7) 0.0005(6) -0.0100(6) C21R 0.0375(8) 0.0229(7) 0.0310(8) -0.0041(6) -0.0167(6) -0.0068(6) C22R 0.0630(12) 0.0289(8) 0.0535(11) -0.0078(8) -0.0321(10) -0.0126(8) F1 0.0218(4) 0.0418(5) 0.0245(4) -0.0102(4) 0.0012(3) -0.0068(4) F2 0.0336(5) 0.0457(6) 0.0240(4) -0.0106(4) -0.0101(4) -0.0073(4) F3 0.0211(4) 0.0546(6) 0.0366(5) -0.0107(5) -0.0048(4) -0.0106(4) _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 C1 2.1739(15) . ? Ti1 Cl2 2.3462(6) . ? Ti1 C1R 2.3993(14) . ? Ti1 C6R 2.4205(15) . ? Ti1 C10R 2.4241(14) . ? Ti1 C9R 2.4298(14) . ? Ti1 C2R 2.4344(15) . ? Ti1 C5R 2.4396(13) . ? Ti1 C7R 2.4442(14) . ? Ti1 C4R 2.4466(14) . ? Ti1 C8R 2.4703(14) . ? Ti1 C3R 2.4754(15) . ? C1 C2 1.3195(19) . ? C1 F1 1.3970(16) . ? C2 F3 1.3266(17) . ? C2 F2 1.3422(17) . ? C1R C5R 1.4193(19) . ? C1R C2R 1.426(2) . ? C1R C11R 1.502(2) . ? C2R C3R 1.413(2) . ? C2R C12R 1.493(2) . ? C3R C4R 1.413(2) . ? C3R C13R 1.508(2) . ? C4R C5R 1.4202(19) . ? C4R C14R 1.508(2) . ? C5R C15R 1.5035(19) . ? C6R C10R 1.417(2) . ? C6R C7R 1.4213(19) . ? C6R C17R 1.507(2) . ? C7R C8R 1.415(2) . ? C7R C18R 1.5028(19) . ? C8R C9R 1.4189(18) . ? C8R C19R 1.5010(19) . ? C9R C10R 1.426(2) . ? C9R C20R 1.502(2) . ? C10R C21R 1.5042(19) . ? C11R H11A 0.9600 . ? C11R H11B 0.9600 . ? C11R H11C 0.9600 . ? C12R H12A 0.9600 . ? C12R H12B 0.9600 . ? C12R H12C 0.9600 . ? C13R H13A 0.9600 . ? C13R H13B 0.9600 . ? C13R H13C 0.9600 . ? C14R H14A 0.9600 . ? C14R H14B 0.9600 . ? C14R H14C 0.9600 . ? C15R C16R 1.537(2) . ? C15R H15A 0.9700 . ? C15R H15B 0.9700 . ? C16R H16A 0.9600 . ? C16R H16B 0.9600 . ? C16R H16C 0.9600 . ? C17R H17A 0.9600 . ? C17R H17B 0.9600 . ? C17R H17C 0.9600 . ? C18R H18A 0.9600 . ? C18R H18B 0.9600 . ? C18R H18C 0.9600 . ? C19R H19A 0.9600 . ? C19R H19B 0.9600 . ? C19R H19C 0.9600 . ? C20R H20A 0.9600 . ? C20R H20B 0.9600 . ? C20R H20C 0.9600 . ? C21R C22R 1.533(2) . ? C21R H21A 0.9700 . ? C21R H21B 0.9700 . ? C22R H22A 0.9600 . ? C22R H22B 0.9600 . ? C22R H22C 0.9600 . ? 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 C1 Ti1 Cl2 95.30(4) . . ? C1 Ti1 C1R 125.81(5) . . ? Cl2 Ti1 C1R 85.07(4) . . ? C1 Ti1 C6R 122.65(5) . . ? Cl2 Ti1 C6R 81.08(4) . . ? C1R Ti1 C6R 110.97(5) . . ? C1 Ti1 C10R 126.88(5) . . ? Cl2 Ti1 C10R 113.10(4) . . ? C1R Ti1 C10R 101.50(5) . . ? C6R Ti1 C10R 34.02(5) . . ? C1 Ti1 C9R 94.27(5) . . ? Cl2 Ti1 C9R 134.39(4) . . ? C1R Ti1 C9R 123.16(5) . . ? C6R Ti1 C9R 56.59(5) . . ? C10R Ti1 C9R 34.17(5) . . ? C1 Ti1 C2R 92.67(6) . . ? Cl2 Ti1 C2R 77.95(4) . . ? C1R Ti1 C2R 34.31(5) . . ? C6R Ti1 C2R 140.33(5) . . ? C10R Ti1 C2R 135.32(5) . . ? C9R Ti1 C2R 145.82(5) . . ? C1 Ti1 C5R 122.41(5) . . ? Cl2 Ti1 C5R 118.67(4) . . ? C1R Ti1 C5R 34.10(5) . . ? C6R Ti1 C5R 108.36(5) . . ? C10R Ti1 C5R 82.72(5) . . ? C9R Ti1 C5R 92.44(5) . . ? C2R Ti1 C5R 56.15(5) . . ? C1 Ti1 C7R 88.83(5) . . ? Cl2 Ti1 C7R 79.55(4) . . ? C1R Ti1 C7R 143.36(5) . . ? C6R Ti1 C7R 33.97(5) . . ? C10R Ti1 C7R 56.29(5) . . ? C9R Ti1 C7R 56.18(5) . . ? C2R Ti1 C7R 157.49(5) . . ? C5R Ti1 C7R 138.88(5) . . ? C1 Ti1 C4R 88.95(5) . . ? Cl2 Ti1 C4R 133.90(4) . . ? C1R Ti1 C4R 56.65(5) . . ? C6R Ti1 C4R 133.16(5) . . ? C10R Ti1 C4R 100.04(5) . . ? C9R Ti1 C4R 90.72(5) . . ? C2R Ti1 C4R 55.98(5) . . ? C5R Ti1 C4R 33.80(5) . . ? C7R Ti1 C4R 146.53(5) . . ? C1 Ti1 C8R 72.69(5) . . ? Cl2 Ti1 C8R 109.89(3) . . ? C1R Ti1 C8R 156.17(5) . . ? C6R Ti1 C8R 55.98(5) . . ? C10R Ti1 C8R 56.01(5) . . ? C9R Ti1 C8R 33.65(4) . . ? C2R Ti1 C8R 163.69(5) . . ? C5R Ti1 C8R 125.73(5) . . ? C7R Ti1 C8R 33.46(5) . . ? C4R Ti1 C8R 115.14(5) . . ? C1 Ti1 C3R 71.95(5) . . ? Cl2 Ti1 C3R 105.66(4) . . ? C1R Ti1 C3R 56.22(5) . . ? C6R Ti1 C3R 163.89(5) . . ? C10R Ti1 C3R 133.25(5) . . ? C9R Ti1 C3R 119.70(5) . . ? C2R Ti1 C3R 33.43(5) . . ? C5R Ti1 C3R 55.54(5) . . ? C7R Ti1 C3R 160.35(5) . . ? C4R Ti1 C3R 33.36(5) . . ? C8R Ti1 C3R 131.35(5) . . ? C2 C1 F1 110.83(12) . . ? C2 C1 Ti1 136.05(11) . . ? F1 C1 Ti1 113.12(9) . . ? C1 C2 F3 125.61(13) . . ? C1 C2 F2 125.85(13) . . ? F3 C2 F2 108.54(11) . . ? C5R C1R C2R 107.45(13) . . ? C5R C1R C11R 126.01(14) . . ? C2R C1R C11R 126.21(15) . . ? C5R C1R Ti1 74.50(7) . . ? C2R C1R Ti1 74.19(8) . . ? C11R C1R Ti1 122.22(10) . . ? C3R C2R C1R 108.08(13) . . ? C3R C2R C12R 124.01(16) . . ? C1R C2R C12R 127.42(17) . . ? C3R C2R Ti1 74.88(8) . . ? C1R C2R Ti1 71.50(8) . . ? C12R C2R Ti1 125.76(10) . . ? C2R C3R C4R 108.33(13) . . ? C2R C3R C13R 124.96(15) . . ? C4R C3R C13R 125.52(15) . . ? C2R C3R Ti1 71.69(8) . . ? C4R C3R Ti1 72.20(8) . . ? C13R C3R Ti1 131.72(10) . . ? C3R C4R C5R 107.86(12) . . ? C3R C4R C14R 124.36(14) . . ? C5R C4R C14R 126.26(13) . . ? C3R C4R Ti1 74.44(8) . . ? C5R C4R Ti1 72.83(7) . . ? C14R C4R Ti1 129.60(10) . . ? C1R C5R C4R 108.17(12) . . ? C1R C5R C15R 124.73(13) . . ? C4R C5R C15R 123.43(12) . . ? C1R C5R Ti1 71.40(7) . . ? C4R C5R Ti1 73.37(7) . . ? C15R C5R Ti1 138.24(10) . . ? C10R C6R C7R 107.99(12) . . ? C10R C6R C17R 125.82(13) . . ? C7R C6R C17R 125.97(13) . . ? C10R C6R Ti1 73.13(8) . . ? C7R C6R Ti1 73.93(8) . . ? C17R C6R Ti1 122.99(10) . . ? C8R C7R C6R 108.09(12) . . ? C8R C7R C18R 124.51(13) . . ? C6R C7R C18R 127.12(14) . . ? C8R C7R Ti1 74.28(8) . . ? C6R C7R Ti1 72.10(8) . . ? C18R C7R Ti1 124.27(10) . . ? C7R C8R C9R 108.18(12) . . ? C7R C8R C19R 125.29(12) . . ? C9R C8R C19R 125.47(13) . . ? C7R C8R Ti1 72.26(7) . . ? C9R C8R Ti1 71.61(8) . . ? C19R C8R Ti1 131.09(10) . . ? C8R C9R C10R 107.78(12) . . ? C8R C9R C20R 124.55(13) . . ? C10R C9R C20R 126.30(13) . . ? C8R C9R Ti1 74.74(8) . . ? C10R C9R Ti1 72.70(8) . . ? C20R C9R Ti1 128.80(10) . . ? C6R C10R C9R 107.91(12) . . ? C6R C10R C21R 124.62(14) . . ? C9R C10R C21R 124.70(13) . . ? C6R C10R Ti1 72.85(8) . . ? C9R C10R Ti1 73.13(8) . . ? C21R C10R Ti1 134.68(10) . . ? C1R C11R H11A 109.5 . . ? C1R C11R H11B 109.5 . . ? H11A C11R H11B 109.5 . . ? C1R C11R H11C 109.5 . . ? H11A C11R H11C 109.5 . . ? H11B C11R H11C 109.5 . . ? C2R C12R H12A 109.5 . . ? C2R C12R H12B 109.5 . . ? H12A C12R H12B 109.5 . . ? C2R C12R H12C 109.5 . . ? H12A C12R H12C 109.5 . . ? H12B C12R H12C 109.5 . . ? C3R C13R H13A 109.5 . . ? C3R C13R H13B 109.5 . . ? H13A C13R H13B 109.5 . . ? C3R C13R H13C 109.5 . . ? H13A C13R H13C 109.5 . . ? H13B C13R H13C 109.5 . . ? C4R C14R H14A 109.5 . . ? C4R C14R H14B 109.5 . . ? H14A C14R H14B 109.5 . . ? C4R C14R H14C 109.5 . . ? H14A C14R H14C 109.5 . . ? H14B C14R H14C 109.5 . . ? C5R C15R C16R 108.28(12) . . ? C5R C15R H15A 110.0 . . ? C16R C15R H15A 110.0 . . ? C5R C15R H15B 110.0 . . ? C16R C15R H15B 110.0 . . ? H15A C15R H15B 108.4 . . ? C15R C16R H16A 109.5 . . ? C15R C16R H16B 109.5 . . ? H16A C16R H16B 109.5 . . ? C15R C16R H16C 109.5 . . ? H16A C16R H16C 109.5 . . ? H16B C16R H16C 109.5 . . ? C6R C17R H17A 109.5 . . ? C6R C17R H17B 109.5 . . ? H17A C17R H17B 109.5 . . ? C6R C17R H17C 109.5 . . ? H17A C17R H17C 109.5 . . ? H17B C17R H17C 109.5 . . ? C7R C18R H18A 109.5 . . ? C7R C18R H18B 109.5 . . ? H18A C18R H18B 109.5 . . ? C7R C18R H18C 109.5 . . ? H18A C18R H18C 109.5 . . ? H18B C18R H18C 109.5 . . ? C8R C19R H19A 109.5 . . ? C8R C19R H19B 109.5 . . ? H19A C19R H19B 109.5 . . ? C8R C19R H19C 109.5 . . ? H19A C19R H19C 109.5 . . ? H19B C19R H19C 109.5 . . ? C9R C20R H20A 109.5 . . ? C9R C20R H20B 109.5 . . ? H20A C20R H20B 109.5 . . ? C9R C20R H20C 109.5 . . ? H20A C20R H20C 109.5 . . ? H20B C20R H20C 109.5 . . ? C10R C21R C22R 110.18(12) . . ? C10R C21R H21A 109.6 . . ? C22R C21R H21A 109.6 . . ? C10R C21R H21B 109.6 . . ? C22R C21R H21B 109.6 . . ? H21A C21R H21B 108.1 . . ? C21R C22R H22A 109.5 . . ? C21R C22R H22B 109.5 . . ? H22A C22R H22B 109.5 . . ? C21R C22R H22C 109.5 . . ? H22A C22R H22C 109.5 . . ? H22B C22R H22C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 30.54 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.449 _refine_diff_density_min -0.307 _refine_diff_density_rms 0.061 # Attachment '2b.CIF' data_cp0tioha _database_code_depnum_ccdc_archive 'CCDC 757335' #TrackingRef '2b.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(ethyltetramethylcyclopentadienyl)(hydroxo)- (trifluoroethenyl)titanium(IV) ; _chemical_name_common ;Bis(ethyltetramethylcyclopentadienyl)(hydroxo)- (trifluoroethenyl)titanium(IV) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H35 F3 O Ti' _chemical_formula_weight 444.42 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.138(5) _cell_length_b 10.007(4) _cell_length_c 16.696(6) _cell_angle_alpha 90.00 _cell_angle_beta 108.655(7) _cell_angle_gamma 90.00 _cell_volume 2238.2(13) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 937 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 30.4 _exptl_crystal_description platelett _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.319 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 0.419 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD (Bruker-AXS)' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28339 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 30.54 _reflns_number_total 6542 _reflns_number_gt 4675 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker-AXS)' _computing_cell_refinement 'SAINT (Bruker-AXS)' _computing_data_reduction 'SAINT (Bruker-AXS)' _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. A disordered modell (Ti1, C2F3, OH) with a 0.818 and 0.182 population was refined. The hydrogen atom of the hydroxo ligand could not be detected unambiguously and is missing. Peak Q2 in in the difference fourier map is located 0.97 Angstr. from O1 with angle Ti1-O1-Q2 of 119 \%. All atoms of the minor part have been refined with isotropic displacement parameters. The distances C1F-C2F, C1F-F1F, C2F-F2F and C2F-F3F have been restrained using the SADI Command in SHELXL97. ; _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^)+(0.0440P)^2^+3.4822P] 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 6542 _refine_ls_number_parameters 301 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0920 _refine_ls_R_factor_gt 0.0626 _refine_ls_wR_factor_ref 0.1550 _refine_ls_wR_factor_gt 0.1404 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 C1A C 0.73721(17) 0.1570(2) 0.63762(16) 0.0249(5) Uani 1 1 d . . . C2A C 0.71596(18) 0.0249(3) 0.60635(16) 0.0266(5) Uani 1 1 d . A . C3A C 0.62223(18) -0.0115(2) 0.61401(16) 0.0260(5) Uani 1 1 d . . . C4A C 0.58488(18) 0.0978(3) 0.64808(16) 0.0261(5) Uani 1 1 d . A . C5A C 0.65605(18) 0.2028(2) 0.66323(15) 0.0239(5) Uani 1 1 d . A . C6A C 0.8232(2) 0.2398(3) 0.62917(19) 0.0373(7) Uani 1 1 d . A . H6A1 H 0.8852 0.2016 0.6635 0.056 Uiso 1 1 calc R . . H6A2 H 0.8177 0.3295 0.6475 0.056 Uiso 1 1 calc R . . H6A3 H 0.8211 0.2407 0.5711 0.056 Uiso 1 1 calc R . . C7A C 0.7733(2) -0.0524(3) 0.5600(2) 0.0395(7) Uani 1 1 d . . . H7A1 H 0.7462 -0.0343 0.5005 0.059 Uiso 1 1 calc R A . H7A2 H 0.7683 -0.1462 0.5698 0.059 Uiso 1 1 calc R . . H7A3 H 0.8422 -0.0259 0.5800 0.059 Uiso 1 1 calc R . . C8A C 0.5679(2) -0.1422(3) 0.58592(19) 0.0367(6) Uani 1 1 d . A . H8A1 H 0.5449 -0.1764 0.6302 0.055 Uiso 1 1 calc R . . H8A2 H 0.6124 -0.2055 0.5737 0.055 Uiso 1 1 calc R . . H8A3 H 0.5117 -0.1275 0.5361 0.055 Uiso 1 1 calc R . . C9A C 0.4837(2) 0.1038(3) 0.6607(2) 0.0413(7) Uani 1 1 d . . . H9A1 H 0.4334 0.1223 0.6076 0.062 Uiso 1 1 calc R A . H9A2 H 0.4837 0.1732 0.7004 0.062 Uiso 1 1 calc R . . H9A3 H 0.4697 0.0196 0.6821 0.062 Uiso 1 1 calc R . . C10A C 0.6330(2) 0.3456(3) 0.67874(18) 0.0325(6) Uani 1 1 d . . . H10A H 0.6948 0.3952 0.7010 0.039 Uiso 1 1 calc R A . H10B H 0.5986 0.3481 0.7205 0.039 Uiso 1 1 calc R . . C11A C 0.5681(2) 0.4109(3) 0.59725(18) 0.0353(6) Uani 1 1 d . A . H11A H 0.6035 0.4122 0.5568 0.053 Uiso 1 1 calc R . . H11B H 0.5525 0.5007 0.6088 0.053 Uiso 1 1 calc R . . H11C H 0.5074 0.3609 0.5747 0.053 Uiso 1 1 calc R . . C1B C 0.89633(18) 0.0902(3) 0.85170(17) 0.0273(5) Uani 1 1 d . . . C2B C 0.86868(17) -0.0221(3) 0.89135(16) 0.0252(5) Uani 1 1 d . A . C3B C 0.78185(17) 0.0122(2) 0.91160(16) 0.0258(5) Uani 1 1 d . . . C4B C 0.75568(17) 0.1459(3) 0.88422(16) 0.0267(5) Uani 1 1 d . A . C5B C 0.82897(18) 0.1957(2) 0.85044(16) 0.0248(5) Uani 1 1 d . A . C6B C 0.9905(2) 0.0997(3) 0.8294(2) 0.0426(7) Uani 1 1 d . A . H6B1 H 0.9955 0.1871 0.8073 0.064 Uiso 1 1 calc R . . H6B2 H 0.9896 0.0336 0.7874 0.064 Uiso 1 1 calc R . . H6B3 H 1.0468 0.0844 0.8790 0.064 Uiso 1 1 calc R . . C7B C 0.9296(2) -0.1467(3) 0.91843(19) 0.0359(6) Uani 1 1 d . . . H7B1 H 0.9788 -0.1325 0.9727 0.054 Uiso 1 1 calc R A . H7B2 H 0.9623 -0.1683 0.8778 0.054 Uiso 1 1 calc R . . H7B3 H 0.8867 -0.2192 0.9222 0.054 Uiso 1 1 calc R . . C8B C 0.7332(2) -0.0727(3) 0.96104(19) 0.0381(7) Uani 1 1 d . A . H8B1 H 0.7345 -0.1645 0.9448 0.057 Uiso 1 1 calc R . . H8B2 H 0.6653 -0.0446 0.9498 0.057 Uiso 1 1 calc R . . H8B3 H 0.7686 -0.0634 1.0203 0.057 Uiso 1 1 calc R . . C9B C 0.6691(2) 0.2220(3) 0.8967(2) 0.0387(7) Uani 1 1 d . . . H9B1 H 0.6821 0.2387 0.9558 0.058 Uiso 1 1 calc R A . H9B2 H 0.6092 0.1701 0.8752 0.058 Uiso 1 1 calc R . . H9B3 H 0.6611 0.3054 0.8669 0.058 Uiso 1 1 calc R . . C10B C 0.8475(2) 0.3409(3) 0.83760(18) 0.0359(7) Uani 1 1 d . . . H10C H 0.7854 0.3902 0.8259 0.043 Uiso 1 1 calc R A . H10D H 0.8708 0.3503 0.7892 0.043 Uiso 1 1 calc R . . C11B C 0.9253(2) 0.3995(3) 0.91613(19) 0.0384(7) Uani 1 1 d . A . H11D H 0.9046 0.3842 0.9648 0.058 Uiso 1 1 calc R . . H11E H 0.9314 0.4938 0.9085 0.058 Uiso 1 1 calc R . . H11F H 0.9886 0.3572 0.9242 0.058 Uiso 1 1 calc R . . Ti1 Ti 0.72739(4) 0.02010(4) 0.75914(3) 0.01453(14) Uani 0.818(2) 1 d P A 1 C1 C 0.7981(2) -0.1639(3) 0.73841(19) 0.0212(6) Uani 0.818(2) 1 d PD A 1 C2 C 0.7707(3) -0.2913(3) 0.7374(2) 0.0288(7) Uani 0.818(2) 1 d PD A 1 F1 F 0.88991(13) -0.15401(19) 0.72434(13) 0.0303(4) Uani 0.818(2) 1 d PD A 1 F2 F 0.82231(17) -0.3969(2) 0.72387(17) 0.0457(6) Uani 0.818(2) 1 d PD A 1 F3 F 0.68868(16) -0.3346(2) 0.75167(16) 0.0421(6) Uani 0.818(2) 1 d PD A 1 O1 O 0.62149(14) -0.0723(2) 0.77839(13) 0.0225(4) Uani 0.818(2) 1 d P A 1 Ti1C Ti 0.7721(3) 0.0231(3) 0.74828(18) 0.0278(8) Uiso 0.182(2) 1 d P A 2 C1F C 0.7041(9) -0.1625(13) 0.7687(10) 0.037(3) Uiso 0.182(2) 1 d PD A 2 C2F C 0.7373(12) -0.2874(13) 0.7700(13) 0.046(4) Uiso 0.182(2) 1 d PD A 2 F1F F 0.6131(7) -0.1541(11) 0.7834(6) 0.043(2) Uiso 0.182(2) 1 d PD A 2 F2F F 0.6840(10) -0.3942(15) 0.7773(9) 0.068(4) Uiso 0.182(2) 1 d PD A 2 F3F F 0.8166(10) -0.3334(15) 0.7529(9) 0.057(3) Uiso 0.182(2) 1 d PD A 2 O1F O 0.8797(9) -0.0678(14) 0.7273(8) 0.041(3) Uiso 0.182(2) 1 d P 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 C1A 0.0234(10) 0.0231(11) 0.0242(13) 0.0038(9) 0.0021(9) -0.0036(9) C2A 0.0273(11) 0.0256(11) 0.0253(13) 0.0002(10) 0.0062(10) -0.0009(10) C3A 0.0308(11) 0.0222(11) 0.0218(13) -0.0011(9) 0.0039(10) -0.0074(9) C4A 0.0275(11) 0.0272(12) 0.0232(13) 0.0016(10) 0.0075(10) -0.0024(9) C5A 0.0280(11) 0.0193(11) 0.0186(13) 0.0014(9) -0.0006(9) -0.0001(9) C6A 0.0316(13) 0.0399(16) 0.0366(17) 0.0060(12) 0.0054(12) -0.0122(12) C7A 0.0437(16) 0.0396(16) 0.0386(18) -0.0024(13) 0.0179(14) 0.0037(12) C8A 0.0403(15) 0.0293(14) 0.0343(17) -0.0073(11) 0.0033(12) -0.0136(11) C9A 0.0317(13) 0.0437(17) 0.051(2) 0.0050(14) 0.0169(13) -0.0005(12) C10A 0.0380(14) 0.0234(12) 0.0283(15) 0.0015(10) -0.0005(11) 0.0051(10) C11A 0.0359(14) 0.0299(14) 0.0329(16) 0.0081(11) 0.0011(12) 0.0082(11) C1B 0.0267(11) 0.0262(12) 0.0284(14) 0.0036(10) 0.0082(10) 0.0011(9) C2B 0.0252(10) 0.0229(11) 0.0243(13) 0.0035(10) 0.0034(9) 0.0051(9) C3B 0.0247(10) 0.0246(12) 0.0253(13) 0.0007(10) 0.0040(9) 0.0023(9) C4B 0.0214(10) 0.0261(12) 0.0261(14) -0.0058(10) -0.0014(9) 0.0050(9) C5B 0.0280(11) 0.0182(11) 0.0204(13) 0.0002(9) -0.0035(9) -0.0004(9) C6B 0.0336(14) 0.0485(18) 0.051(2) 0.0057(15) 0.0203(14) 0.0003(13) C7B 0.0346(14) 0.0310(14) 0.0357(17) 0.0075(12) 0.0021(12) 0.0138(11) C8B 0.0357(14) 0.0439(16) 0.0343(17) 0.0044(13) 0.0106(12) -0.0046(12) C9B 0.0329(13) 0.0386(16) 0.0396(17) -0.0078(13) 0.0047(12) 0.0134(12) C10B 0.0431(15) 0.0209(12) 0.0312(16) 0.0004(10) -0.0057(12) -0.0077(11) C11B 0.0392(15) 0.0291(14) 0.0355(17) -0.0044(12) -0.0040(13) -0.0093(11) Ti1 0.0138(2) 0.01152(19) 0.0180(3) 0.00017(18) 0.00472(17) -0.00029(16) C1 0.0200(12) 0.0190(12) 0.0270(16) -0.0009(11) 0.0110(11) 0.0026(10) C2 0.0324(16) 0.0181(13) 0.041(2) 0.0016(13) 0.0195(15) 0.0022(13) F1 0.0251(8) 0.0225(9) 0.0484(12) 0.0003(8) 0.0189(8) 0.0022(7) F2 0.0545(13) 0.0151(9) 0.0824(18) -0.0014(10) 0.0428(13) 0.0035(9) F3 0.0445(12) 0.0211(10) 0.0742(17) 0.0004(11) 0.0379(12) -0.0049(9) O1 0.0209(9) 0.0219(10) 0.0263(12) 0.0007(8) 0.0098(8) -0.0054(8) _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 C1A C2A 1.418(4) . ? C1A C5A 1.423(3) . ? C1A C6A 1.515(3) . ? C1A Ti1C 2.207(4) . ? C1A Ti1 2.488(3) . ? C2A C3A 1.419(3) . ? C2A C7A 1.502(4) . ? C2A Ti1C 2.246(4) . ? C2A Ti1 2.504(3) . ? C3A C4A 1.411(4) . ? C3A C8A 1.513(3) . ? C3A Ti1 2.424(3) . ? C3A Ti1C 2.568(4) . ? C4A C5A 1.420(3) . ? C4A C9A 1.513(4) . ? C4A Ti1 2.390(3) . ? C5A C10A 1.507(3) . ? C5A Ti1 2.427(2) . ? C5A Ti1C 2.540(4) . ? C6A H6A1 0.9600 . ? C6A H6A2 0.9600 . ? C6A H6A3 0.9600 . ? C7A H7A1 0.9600 . ? C7A H7A2 0.9600 . ? C7A H7A3 0.9600 . ? C8A H8A1 0.9600 . ? C8A H8A2 0.9600 . ? C8A H8A3 0.9600 . ? C9A H9A1 0.9600 . ? C9A H9A2 0.9600 . ? C9A H9A3 0.9600 . ? C10A C11A 1.524(4) . ? C10A H10A 0.9700 . ? C10A H10B 0.9700 . ? C11A H11A 0.9600 . ? C11A H11B 0.9600 . ? C11A H11C 0.9600 . ? C1B C5B 1.417(3) . ? C1B C2B 1.421(3) . ? C1B C6B 1.496(4) . ? C1B Ti1C 2.139(4) . ? C1B Ti1 2.495(3) . ? C2B C3B 1.416(3) . ? C2B C7B 1.502(3) . ? C2B Ti1C 2.385(4) . ? C2B Ti1 2.494(2) . ? C3B C4B 1.425(3) . ? C3B C8B 1.496(4) . ? C3B Ti1 2.414(3) . ? C3B Ti1C 2.688(4) . ? C4B C5B 1.419(4) . ? C4B C9B 1.511(3) . ? C4B Ti1 2.361(3) . ? C4B Ti1C 2.656(4) . ? C5B C10B 1.505(3) . ? C5B Ti1C 2.379(4) . ? C5B Ti1 2.464(2) . ? C6B H6B1 0.9600 . ? C6B H6B2 0.9600 . ? C6B H6B3 0.9600 . ? C7B H7B1 0.9600 . ? C7B H7B2 0.9600 . ? C7B H7B3 0.9600 . ? C8B H8B1 0.9600 . ? C8B H8B2 0.9600 . ? C8B H8B3 0.9600 . ? C9B H9B1 0.9600 . ? C9B H9B2 0.9600 . ? C9B H9B3 0.9600 . ? C10B C11B 1.533(4) . ? C10B H10C 0.9700 . ? C10B H10D 0.9700 . ? C11B H11D 0.9600 . ? C11B H11E 0.9600 . ? C11B H11F 0.9600 . ? Ti1 O1 1.873(2) . ? Ti1 C1 2.175(3) . ? C1 C2 1.331(4) . ? C1 F1 1.395(3) . ? C2 F3 1.329(4) . ? C2 F2 1.344(4) . ? Ti1C O1F 1.899(13) . ? Ti1C C1F 2.168(14) . ? C1F C2F 1.333(10) . ? C1F F1F 1.387(9) . ? C2F F3F 1.325(10) . ? C2F F2F 1.337(10) . ? 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 C2A C1A C5A 108.4(2) . . ? C2A C1A C6A 123.9(2) . . ? C5A C1A C6A 126.9(2) . . ? C2A C1A Ti1C 72.93(16) . . ? C5A C1A Ti1C 85.97(18) . . ? C6A C1A Ti1C 116.05(19) . . ? C2A C1A Ti1 74.12(15) . . ? C5A C1A Ti1 70.83(14) . . ? C6A C1A Ti1 129.27(17) . . ? Ti1C C1A Ti1 16.04(9) . . ? C1A C2A C3A 107.5(2) . . ? C1A C2A C7A 125.7(2) . . ? C3A C2A C7A 126.0(2) . . ? C1A C2A Ti1C 69.94(16) . . ? C3A C2A Ti1C 85.87(18) . . ? C7A C2A Ti1C 118.2(2) . . ? C1A C2A Ti1 72.88(15) . . ? C3A C2A Ti1 70.20(14) . . ? C7A C2A Ti1 130.21(19) . . ? Ti1C C2A Ti1 16.07(9) . . ? C4A C3A C2A 108.5(2) . . ? C4A C3A C8A 125.2(2) . . ? C2A C3A C8A 126.2(2) . . ? C4A C3A Ti1 71.63(14) . . ? C2A C3A Ti1 76.39(15) . . ? C8A C3A Ti1 120.72(18) . . ? C4A C3A Ti1C 81.61(17) . . ? C2A C3A Ti1C 60.69(16) . . ? C8A C3A Ti1C 125.63(19) . . ? Ti1 C3A Ti1C 16.06(8) . . ? C3A C4A C5A 108.1(2) . . ? C3A C4A C9A 125.4(2) . . ? C5A C4A C9A 126.4(2) . . ? C3A C4A Ti1 74.29(15) . . ? C5A C4A Ti1 74.28(14) . . ? C9A C4A Ti1 120.34(19) . . ? C4A C5A C1A 107.6(2) . . ? C4A C5A C10A 123.5(2) . . ? C1A C5A C10A 126.6(2) . . ? C4A C5A Ti1 71.43(14) . . ? C1A C5A Ti1 75.56(14) . . ? C10A C5A Ti1 131.94(18) . . ? C4A C5A Ti1C 82.53(16) . . ? C1A C5A Ti1C 60.06(15) . . ? C10A C5A Ti1C 135.40(18) . . ? Ti1 C5A Ti1C 16.27(8) . . ? C1A C6A H6A1 109.5 . . ? C1A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? C1A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C2A C7A H7A1 109.5 . . ? C2A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? C2A C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C3A C8A H8A1 109.5 . . ? C3A C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? C3A C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? C4A C9A H9A1 109.5 . . ? C4A C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? C4A C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? C5A C10A C11A 110.8(2) . . ? C5A C10A H10A 109.5 . . ? C11A C10A H10A 109.5 . . ? C5A C10A H10B 109.5 . . ? C11A C10A H10B 109.5 . . ? H10A C10A H10B 108.1 . . ? C10A C11A H11A 109.5 . . ? C10A C11A H11B 109.5 . . ? H11A C11A H11B 109.5 . . ? C10A C11A H11C 109.5 . . ? H11A C11A H11C 109.5 . . ? H11B C11A H11C 109.5 . . ? C5B C1B C2B 108.2(2) . . ? C5B C1B C6B 126.6(2) . . ? C2B C1B C6B 124.4(2) . . ? C5B C1B Ti1C 81.23(17) . . ? C2B C1B Ti1C 81.41(17) . . ? C6B C1B Ti1C 112.6(2) . . ? C5B C1B Ti1 72.22(14) . . ? C2B C1B Ti1 73.42(14) . . ? C6B C1B Ti1 128.0(2) . . ? Ti1C C1B Ti1 15.34(9) . . ? C3B C2B C1B 108.0(2) . . ? C3B C2B C7B 126.0(2) . . ? C1B C2B C7B 125.5(2) . . ? C3B C2B Ti1C 86.04(17) . . ? C1B C2B Ti1C 62.50(16) . . ? C7B C2B Ti1C 123.3(2) . . ? C3B C2B Ti1 70.14(14) . . ? C1B C2B Ti1 73.48(14) . . ? C7B C2B Ti1 128.84(19) . . ? Ti1C C2B Ti1 16.58(8) . . ? C2B C3B C4B 107.9(2) . . ? C2B C3B C8B 125.5(2) . . ? C4B C3B C8B 126.3(2) . . ? C2B C3B Ti1 76.38(15) . . ? C4B C3B Ti1 70.62(15) . . ? C8B C3B Ti1 123.55(18) . . ? C2B C3B Ti1C 62.26(15) . . ? C4B C3B Ti1C 73.29(16) . . ? C8B C3B Ti1C 134.4(2) . . ? Ti1 C3B Ti1C 14.81(7) . . ? C5B C4B C3B 108.0(2) . . ? C5B C4B C9B 127.2(2) . . ? C3B C4B C9B 124.6(3) . . ? C5B C4B Ti1 76.94(15) . . ? C3B C4B Ti1 74.68(15) . . ? C9B C4B Ti1 118.36(17) . . ? C5B C4B Ti1C 63.13(15) . . ? C3B C4B Ti1C 75.79(16) . . ? C9B C4B Ti1C 130.31(19) . . ? Ti1 C4B Ti1C 14.86(7) . . ? C1B C5B C4B 107.8(2) . . ? C1B C5B C10B 125.1(2) . . ? C4B C5B C10B 125.3(2) . . ? C1B C5B Ti1C 62.71(16) . . ? C4B C5B Ti1C 84.73(17) . . ? C10B C5B Ti1C 129.3(2) . . ? C1B C5B Ti1 74.59(14) . . ? C4B C5B Ti1 68.94(14) . . ? C10B C5B Ti1 133.97(18) . . ? Ti1C C5B Ti1 16.78(8) . . ? C1B C6B H6B1 109.5 . . ? C1B C6B H6B2 109.5 . . ? H6B1 C6B H6B2 109.5 . . ? C1B C6B H6B3 109.5 . . ? H6B1 C6B H6B3 109.5 . . ? H6B2 C6B H6B3 109.5 . . ? C2B C7B H7B1 109.5 . . ? C2B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? C2B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? C3B C8B H8B1 109.5 . . ? C3B C8B H8B2 109.5 . . ? H8B1 C8B H8B2 109.5 . . ? C3B C8B H8B3 109.5 . . ? H8B1 C8B H8B3 109.5 . . ? H8B2 C8B H8B3 109.5 . . ? C4B C9B H9B1 109.5 . . ? C4B C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? C4B C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? C5B C10B C11B 110.9(2) . . ? C5B C10B H10C 109.5 . . ? C11B C10B H10C 109.5 . . ? C5B C10B H10D 109.5 . . ? C11B C10B H10D 109.5 . . ? H10C C10B H10D 108.0 . . ? C10B C11B H11D 109.5 . . ? C10B C11B H11E 109.5 . . ? H11D C11B H11E 109.5 . . ? C10B C11B H11F 109.5 . . ? H11D C11B H11F 109.5 . . ? H11E C11B H11F 109.5 . . ? O1 Ti1 C1 92.44(10) . . ? O1 Ti1 C4B 91.72(9) . . ? C1 Ti1 C4B 129.49(10) . . ? O1 Ti1 C4A 76.82(9) . . ? C1 Ti1 C4A 117.92(10) . . ? C4B Ti1 C4A 112.02(9) . . ? O1 Ti1 C3B 78.79(9) . . ? C1 Ti1 C3B 97.59(10) . . ? C4B Ti1 C3B 34.70(8) . . ? C4A Ti1 C3B 137.25(9) . . ? O1 Ti1 C3A 80.72(9) . . ? C1 Ti1 C3A 84.06(10) . . ? C4B Ti1 C3A 146.10(9) . . ? C4A Ti1 C3A 34.08(9) . . ? C3B Ti1 C3A 159.49(9) . . ? O1 Ti1 C5A 107.38(9) . . ? C1 Ti1 C5A 130.39(10) . . ? C4B Ti1 C5A 95.67(9) . . ? C4A Ti1 C5A 34.29(8) . . ? C3B Ti1 C5A 130.21(9) . . ? C3A Ti1 C5A 56.38(8) . . ? O1 Ti1 C5B 125.84(9) . . ? C1 Ti1 C5B 119.71(10) . . ? C4B Ti1 C5B 34.12(9) . . ? C4A Ti1 C5B 115.33(9) . . ? C3B Ti1 C5B 56.28(9) . . ? C3A Ti1 C5B 139.56(8) . . ? C5A Ti1 C5B 84.72(8) . . ? O1 Ti1 C1A 131.90(9) . . ? C1 Ti1 C1A 100.84(10) . . ? C4B Ti1 C1A 112.94(9) . . ? C4A Ti1 C1A 56.04(8) . . ? C3B Ti1 C1A 142.73(9) . . ? C3A Ti1 C1A 55.48(8) . . ? C5A Ti1 C1A 33.61(8) . . ? C5B Ti1 C1A 86.47(9) . . ? O1 Ti1 C2B 102.86(9) . . ? C1 Ti1 C2B 73.68(10) . . ? C4B Ti1 C2B 56.37(8) . . ? C4A Ti1 C2B 168.37(9) . . ? C3B Ti1 C2B 33.48(8) . . ? C3A Ti1 C2B 157.53(9) . . ? C5A Ti1 C2B 139.25(8) . . ? C5B Ti1 C2B 55.24(8) . . ? C1A Ti1 C2B 125.24(8) . . ? O1 Ti1 C1B 133.79(9) . . ? C1 Ti1 C1B 86.52(10) . . ? C4B Ti1 C1B 56.24(8) . . ? C4A Ti1 C1B 142.33(9) . . ? C3B Ti1 C1B 55.71(8) . . ? C3A Ti1 C1B 144.63(9) . . ? C5A Ti1 C1B 108.08(8) . . ? C5B Ti1 C1B 33.20(8) . . ? C1A Ti1 C1B 93.34(8) . . ? C2B Ti1 C1B 33.10(8) . . ? O1 Ti1 C2A 112.93(9) . . ? C1 Ti1 C2A 74.77(10) . . ? C4B Ti1 C2A 145.94(9) . . ? C4A Ti1 C2A 55.93(8) . . ? C3B Ti1 C2A 165.89(8) . . ? C3A Ti1 C2A 33.41(8) . . ? C5A Ti1 C2A 55.66(8) . . ? C5B Ti1 C2A 116.84(9) . . ? C1A Ti1 C2A 33.00(8) . . ? C2B Ti1 C2A 132.63(8) . . ? C1B Ti1 C2A 111.27(9) . . ? C2 C1 F1 110.4(2) . . ? C2 C1 Ti1 131.8(2) . . ? F1 C1 Ti1 117.79(18) . . ? F3 C2 C1 125.2(3) . . ? F3 C2 F2 109.0(2) . . ? C1 C2 F2 125.7(3) . . ? O1F Ti1C C1B 78.5(4) . . ? O1F Ti1C C1F 92.3(5) . . ? C1B Ti1C C1F 115.7(5) . . ? O1F Ti1C C1A 96.5(4) . . ? C1B Ti1C C1A 113.02(17) . . ? C1F Ti1C C1A 131.3(5) . . ? O1F Ti1C C2A 80.9(4) . . ? C1B Ti1C C2A 140.5(2) . . ? C1F Ti1C C2A 98.5(5) . . ? C1A Ti1C C2A 37.13(10) . . ? O1F Ti1C C5B 111.9(4) . . ? C1B Ti1C C5B 36.06(10) . . ? C1F Ti1C C5B 125.1(4) . . ? C1A Ti1C C5B 95.35(14) . . ? C2A Ti1C C5B 132.47(16) . . ? O1F Ti1C C2B 81.9(4) . . ? C1B Ti1C C2B 36.09(10) . . ? C1F Ti1C C2B 79.7(5) . . ? C1A Ti1C C2B 148.95(17) . . ? C2A Ti1C C2B 162.61(19) . . ? C5B Ti1C C2B 57.70(11) . . ? O1F Ti1C C5A 130.4(4) . . ? C1B Ti1C C5A 116.47(15) . . ? C1F Ti1C C5A 117.0(4) . . ? C1A Ti1C C5A 33.96(9) . . ? C2A Ti1C C5A 57.14(11) . . ? C5B Ti1C C5A 84.07(12) . . ? C2B Ti1C C5A 138.99(15) . . ? O1F Ti1C C3A 105.1(4) . . ? C1B Ti1C C3A 169.08(16) . . ? C1F Ti1C C3A 74.8(4) . . ? C1A Ti1C C3A 56.63(10) . . ? C2A Ti1C C3A 33.44(9) . . ? C5B Ti1C C3A 135.97(15) . . ? C2B Ti1C C3A 153.74(17) . . ? C5A Ti1C C3A 53.31(10) . . ? O1F Ti1C C4B 132.4(4) . . ? C1B Ti1C C4B 55.85(11) . . ? C1F Ti1C C4B 95.6(4) . . ? C1A Ti1C C4B 112.16(15) . . ? C2A Ti1C C4B 143.14(16) . . ? C5B Ti1C C4B 32.14(9) . . ? C2B Ti1C C4B 53.87(10) . . ? C5A Ti1C C4B 86.13(12) . . ? C3A Ti1C C4B 122.35(16) . . ? O1F Ti1C C3B 112.6(4) . . ? C1B Ti1C C3B 55.36(11) . . ? C1F Ti1C C3B 71.8(4) . . ? C1A Ti1C C3B 143.06(16) . . ? C2A Ti1C C3B 163.12(19) . . ? C5B Ti1C C3B 53.59(10) . . ? C2B Ti1C C3B 31.69(8) . . ? C5A Ti1C C3B 114.22(14) . . ? C3A Ti1C C3B 129.81(17) . . ? C4B Ti1C C3B 30.92(8) . . ? C2F C1F F1F 113.3(12) . . ? C2F C1F Ti1C 129.4(10) . . ? F1F C1F Ti1C 117.3(9) . . ? F3F C2F C1F 129.8(15) . . ? F3F C2F F2F 106.4(12) . . ? C1F C2F F2F 123.0(14) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 30.54 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.550 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.081 # Attachment '3b.CIF' data_cp0tif2 _database_code_depnum_ccdc_archive 'CCDC 757336' #TrackingRef '3b.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Fluoro-bis(ethyltetramethylcyclopentadienyl)(trifluoro- ethenyl)titanium(VI) ; _chemical_name_common ;Fluoro-bis(ethyltetramethylcyclopentadienyl)(trifluoro- ethenyl)titanium(VI) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H34 F4 Ti' _chemical_formula_weight 446.41 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.102(3) _cell_length_b 9.979(2) _cell_length_c 16.560(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.593(4) _cell_angle_gamma 90.00 _cell_volume 2208.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 1004 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 26.3 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.342 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 0.428 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.62 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_process_details 'Sadabs (Bruker-AXS)' _exptl_special_details ; A diordered modell for the fluoro ligand the Ti atom and the the trifluoroethenyl ligand has been refined with a population of 0.816 and 0.184. ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD (Bruker-AXS)' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25489 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0217 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 26.39 _reflns_number_total 4532 _reflns_number_gt 3818 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker-AXS)' _computing_cell_refinement 'SAINT (Bruker-AXS)' _computing_data_reduction 'SAINT (Bruker-AXS)' _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. The structure has been refined with a disorder of the Ti(F)CF=CF2 group. with an occupancy of 0.816(2) for the major part. All atoms of the minor part have been refined with isotropic displacement parameters and the C-C and C-F distances of similar bonds in the minor component were restrained to be equal to the ones in the major part using the SADI command of SHELXL97. Although this model converges well it can not be ruled out that the disorder problem might be due to unrecognized twinning or a small disorder of the Cp* ligands, which is not included in the model, causes the unusual distances of the minor part to the Cp* ligands. ; _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^)+(0.0535P)^2^+2.1346P] 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 4532 _refine_ls_number_parameters 301 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1198 _refine_ls_wR_factor_gt 0.1103 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 C1A C 0.60399(15) 0.4084(2) 0.14822(13) 0.0243(4) Uani 1 1 d . . . C2A C 0.63201(15) 0.5216(2) 0.10953(13) 0.0232(4) Uani 1 1 d . A . C3A C 0.71904(15) 0.4887(2) 0.08915(12) 0.0224(4) Uani 1 1 d . . . C4A C 0.74565(14) 0.3552(2) 0.11584(13) 0.0235(4) Uani 1 1 d . A . C5A C 0.67167(14) 0.3035(2) 0.14949(12) 0.0224(4) Uani 1 1 d . A . C6A C 0.50936(17) 0.3974(3) 0.17056(16) 0.0357(5) Uani 1 1 d . A . H6A1 H 0.4518 0.4115 0.1193 0.054 Uiso 1 1 calc R . . H6A2 H 0.5093 0.4653 0.2133 0.054 Uiso 1 1 calc R . . H6A3 H 0.5052 0.3080 0.1937 0.054 Uiso 1 1 calc R . . C7A C 0.57047(17) 0.6466(2) 0.08259(15) 0.0328(5) Uani 1 1 d . . . H7A1 H 0.6139 0.7206 0.0776 0.049 Uiso 1 1 calc R A . H7A2 H 0.5382 0.6691 0.1252 0.049 Uiso 1 1 calc R . . H7A3 H 0.5192 0.6314 0.0274 0.049 Uiso 1 1 calc R . . C8A C 0.77127(17) 0.5780(3) 0.04435(14) 0.0337(5) Uani 1 1 d . A . H8A1 H 0.7368 0.5743 -0.0172 0.050 Uiso 1 1 calc R . . H8A2 H 0.8406 0.5480 0.0565 0.050 Uiso 1 1 calc R . . H8A3 H 0.7707 0.6703 0.0644 0.050 Uiso 1 1 calc R . . C9A C 0.83349(16) 0.2805(2) 0.10434(15) 0.0334(5) Uani 1 1 d . . . H9A1 H 0.8230 0.2678 0.0434 0.050 Uiso 1 1 calc R A . H9A2 H 0.8396 0.1929 0.1323 0.050 Uiso 1 1 calc R . . H9A3 H 0.8949 0.3322 0.1298 0.050 Uiso 1 1 calc R . . C10A C 0.65362(17) 0.1572(2) 0.16177(14) 0.0314(5) Uani 1 1 d . . . H10A H 0.6312 0.1464 0.2123 0.038 Uiso 1 1 calc R A . H10B H 0.7169 0.1069 0.1722 0.038 Uiso 1 1 calc R . . C11A C 0.57418(17) 0.1000(2) 0.08322(14) 0.0322(5) Uani 1 1 d . A . H11A H 0.5101 0.1449 0.0756 0.048 Uiso 1 1 calc R . . H11B H 0.5668 0.0036 0.0911 0.048 Uiso 1 1 calc R . . H11C H 0.5948 0.1147 0.0327 0.048 Uiso 1 1 calc R . . C1B C 0.76262(14) 0.3415(2) 0.36308(13) 0.0233(4) Uani 1 1 d . . . C2B C 0.78511(15) 0.4733(2) 0.39488(13) 0.0243(4) Uani 1 1 d . A . C3B C 0.87873(15) 0.5100(2) 0.38623(12) 0.0238(4) Uani 1 1 d . . . C4B C 0.91533(15) 0.3999(2) 0.35150(13) 0.0246(4) Uani 1 1 d . A . C5B C 0.84412(14) 0.2951(2) 0.33705(12) 0.0221(4) Uani 1 1 d . A . C6B C 0.67665(16) 0.2595(3) 0.37204(15) 0.0332(5) Uani 1 1 d . A . H6B1 H 0.6800 0.2570 0.4320 0.050 Uiso 1 1 calc R . . H6B2 H 0.6809 0.1681 0.3519 0.050 Uiso 1 1 calc R . . H6B3 H 0.6132 0.3002 0.3380 0.050 Uiso 1 1 calc R . . C7B C 0.72798(18) 0.5509(3) 0.44141(15) 0.0361(6) Uani 1 1 d . . . H7B1 H 0.6572 0.5253 0.4202 0.054 Uiso 1 1 calc R A . H7B2 H 0.7344 0.6470 0.4321 0.054 Uiso 1 1 calc R . . H7B3 H 0.7549 0.5313 0.5025 0.054 Uiso 1 1 calc R . . C8B C 0.93284(17) 0.6402(2) 0.41288(15) 0.0343(5) Uani 1 1 d . A . H8B1 H 0.9910 0.6258 0.4636 0.051 Uiso 1 1 calc R . . H8B2 H 0.8877 0.7053 0.4260 0.051 Uiso 1 1 calc R . . H8B3 H 0.9551 0.6747 0.3665 0.051 Uiso 1 1 calc R . . C9B C 1.01531(17) 0.3939(3) 0.33687(16) 0.0377(6) Uani 1 1 d . . . H9B1 H 1.0216 0.4699 0.3014 0.057 Uiso 1 1 calc R A . H9B2 H 1.0205 0.3099 0.3079 0.057 Uiso 1 1 calc R . . H9B3 H 1.0689 0.3979 0.3918 0.057 Uiso 1 1 calc R . . C10B C 0.86634(17) 0.1515(2) 0.32141(14) 0.0301(5) Uani 1 1 d . . . H10C H 0.9011 0.1483 0.2781 0.036 Uiso 1 1 calc R A . H10D H 0.8028 0.1012 0.2990 0.036 Uiso 1 1 calc R . . C11B C 0.93168(16) 0.0861(2) 0.40349(14) 0.0319(5) Uani 1 1 d . A . H11D H 0.9950 0.1350 0.4251 0.048 Uiso 1 1 calc R . . H11E H 0.9452 -0.0072 0.3920 0.048 Uiso 1 1 calc R . . H11F H 0.8969 0.0883 0.4461 0.048 Uiso 1 1 calc R . . C1 C 0.70214(16) 0.6623(2) 0.26332(15) 0.0176(5) Uani 0.816(2) 1 d PD A 1 C2 C 0.7296(2) 0.7887(3) 0.26351(17) 0.0243(6) Uani 0.816(2) 1 d PD A 1 F1 F 0.61003(10) 0.65239(15) 0.27760(10) 0.0241(3) Uani 0.816(2) 1 d PD A 1 F2 F 0.67884(13) 0.89572(17) 0.27629(13) 0.0383(4) Uani 0.816(2) 1 d PD A 1 F3 F 0.81257(13) 0.83036(18) 0.24915(12) 0.0337(4) Uani 0.816(2) 1 d PD A 1 F4 F 0.87391(9) 0.56885(16) 0.21841(8) 0.0192(3) Uani 0.816(2) 1 d P A 1 Ti1 Ti 0.77198(4) 0.47800(4) 0.24174(3) 0.01142(15) Uani 0.816(2) 1 d P A 1 C1F C 0.7984(8) 0.6619(12) 0.2332(8) 0.035(3) Uiso 0.184(2) 1 d PD A 2 C2F C 0.7672(11) 0.7869(12) 0.2333(12) 0.049(4) Uiso 0.184(2) 1 d PD A 2 F1F F 0.8893(6) 0.6540(10) 0.2177(5) 0.042(2) Uiso 0.184(2) 1 d PD A 2 F2F F 0.8170(8) 0.8931(12) 0.2212(7) 0.061(3) Uiso 0.184(2) 1 d PD A 2 F3F F 0.6841(8) 0.8269(13) 0.2468(7) 0.055(3) Uiso 0.184(2) 1 d PD A 2 F4F F 0.6263(6) 0.5660(9) 0.2760(5) 0.0359(18) Uiso 0.184(2) 1 d P A 2 Ti1F Ti 0.7293(3) 0.4754(3) 0.25242(16) 0.0311(8) Uiso 0.184(2) 1 d P 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 C1A 0.0212(9) 0.0268(12) 0.0224(10) -0.0009(8) 0.0036(8) 0.0015(8) C2A 0.0227(9) 0.0230(11) 0.0205(10) 0.0013(8) 0.0022(8) 0.0050(8) C3A 0.0208(9) 0.0238(11) 0.0190(9) -0.0019(8) 0.0011(7) 0.0028(8) C4A 0.0186(9) 0.0251(11) 0.0211(10) -0.0052(8) -0.0014(7) 0.0036(8) C5A 0.0238(9) 0.0191(10) 0.0167(9) -0.0016(8) -0.0042(7) 0.0001(8) C6A 0.0293(11) 0.0413(15) 0.0387(13) 0.0005(11) 0.0139(10) 0.0001(10) C7A 0.0315(11) 0.0297(13) 0.0303(12) 0.0043(10) 0.0004(9) 0.0118(10) C8A 0.0345(12) 0.0409(14) 0.0264(11) 0.0040(10) 0.0110(9) -0.0012(10) C9A 0.0285(11) 0.0346(13) 0.0328(12) -0.0079(10) 0.0036(9) 0.0096(10) C10A 0.0347(12) 0.0210(12) 0.0268(11) -0.0013(9) -0.0067(9) -0.0043(9) C11A 0.0327(11) 0.0255(12) 0.0297(12) -0.0048(9) -0.0022(9) -0.0068(9) C1B 0.0212(9) 0.0220(11) 0.0218(10) 0.0048(8) 0.0000(8) -0.0037(8) C2B 0.0237(10) 0.0251(11) 0.0213(10) 0.0026(8) 0.0033(8) -0.0006(8) C3B 0.0277(10) 0.0230(11) 0.0171(9) -0.0001(8) 0.0023(8) -0.0091(8) C4B 0.0239(10) 0.0280(12) 0.0201(10) 0.0032(8) 0.0047(8) -0.0026(8) C5B 0.0237(9) 0.0216(11) 0.0157(9) 0.0039(8) -0.0011(7) -0.0004(8) C6B 0.0280(11) 0.0356(13) 0.0317(12) 0.0065(10) 0.0035(9) -0.0123(10) C7B 0.0411(13) 0.0397(15) 0.0296(12) 0.0006(10) 0.0142(10) 0.0040(11) C8B 0.0367(12) 0.0296(13) 0.0291(12) -0.0035(10) 0.0000(10) -0.0152(10) C9B 0.0292(11) 0.0448(15) 0.0411(14) 0.0065(11) 0.0140(10) -0.0007(10) C10B 0.0353(11) 0.0208(11) 0.0254(11) 0.0029(9) -0.0029(9) 0.0047(9) C11B 0.0309(11) 0.0297(13) 0.0293(11) 0.0078(10) 0.0014(9) 0.0083(9) C1 0.0151(10) 0.0178(12) 0.0228(12) -0.0004(9) 0.0101(9) 0.0019(9) C2 0.0246(13) 0.0180(14) 0.0345(15) 0.0012(11) 0.0155(12) 0.0013(11) F1 0.0204(7) 0.0177(8) 0.0398(9) 0.0002(6) 0.0174(6) 0.0018(6) F2 0.0447(10) 0.0137(8) 0.0687(12) -0.0022(8) 0.0352(9) 0.0032(7) F3 0.0338(9) 0.0196(9) 0.0578(11) 0.0019(8) 0.0290(8) -0.0031(7) F4 0.0160(6) 0.0209(8) 0.0215(7) 0.0023(6) 0.0072(5) -0.0043(5) Ti1 0.0098(2) 0.0103(2) 0.0143(2) 0.00042(15) 0.00392(15) -0.00045(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 C1A C5A 1.413(3) . ? C1A C2A 1.415(3) . ? C1A C6A 1.498(3) . ? C1A Ti1F 2.145(3) . ? C1A Ti1 2.481(2) . ? C2A C3A 1.411(3) . ? C2A C7A 1.504(3) . ? C2A Ti1F 2.371(3) . ? C2A Ti1 2.474(2) . ? C3A C4A 1.416(3) . ? C3A C8A 1.495(3) . ? C3A Ti1 2.398(2) . ? C3A Ti1F 2.664(4) . ? C4A C5A 1.427(3) . ? C4A C9A 1.509(3) . ? C4A Ti1 2.344(2) . ? C4A Ti1F 2.635(4) . ? C5A C10A 1.506(3) . ? C5A Ti1F 2.372(3) . ? C5A Ti1 2.447(2) . ? C6A H6A1 0.9800 . ? C6A H6A2 0.9800 . ? C6A H6A3 0.9800 . ? C7A H7A1 0.9800 . ? C7A H7A2 0.9800 . ? C7A H7A3 0.9800 . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? C9A H9A1 0.9800 . ? C9A H9A2 0.9800 . ? C9A H9A3 0.9800 . ? C10A C11A 1.531(3) . ? C10A H10A 0.9900 . ? C10A H10B 0.9900 . ? C11A H11A 0.9800 . ? C11A H11B 0.9800 . ? C11A H11C 0.9800 . ? C1B C2B 1.415(3) . ? C1B C5B 1.427(3) . ? C1B C6B 1.509(3) . ? C1B Ti1F 2.195(3) . ? C1B Ti1 2.466(2) . ? C2B C3B 1.421(3) . ? C2B C7B 1.496(3) . ? C2B Ti1F 2.236(3) . ? C2B Ti1 2.484(2) . ? C3B C4B 1.412(3) . ? C3B C8B 1.500(3) . ? C3B Ti1 2.408(2) . ? C3B Ti1F 2.548(3) . ? C4B C5B 1.417(3) . ? C4B C9B 1.506(3) . ? C4B Ti1 2.378(2) . ? C4B Ti1F 2.720(4) . ? C5B C10B 1.506(3) . ? C5B Ti1 2.416(2) . ? C5B Ti1F 2.526(3) . ? C6B H6B1 0.9800 . ? C6B H6B2 0.9800 . ? C6B H6B3 0.9800 . ? C7B H7B1 0.9800 . ? C7B H7B2 0.9800 . ? C7B H7B3 0.9800 . ? C8B H8B1 0.9800 . ? C8B H8B2 0.9800 . ? C8B H8B3 0.9800 . ? C9B H9B1 0.9800 . ? C9B H9B2 0.9800 . ? C9B H9B3 0.9800 . ? C10B C11B 1.525(3) . ? C10B H10C 0.9900 . ? C10B H10D 0.9900 . ? C11B H11D 0.9800 . ? C11B H11E 0.9800 . ? C11B H11F 0.9800 . ? C1 C2 1.318(4) . ? C1 F1 1.396(2) . ? C1 Ti1 2.169(2) . ? C2 F3 1.333(3) . ? C2 F2 1.339(3) . ? F4 Ti1 1.8416(15) . ? C1F C2F 1.323(10) . ? C1F F1F 1.387(9) . ? C1F Ti1F 2.171(12) . ? C2F F2F 1.321(9) . ? C2F F3F 1.322(10) . ? F4F Ti1F 1.855(9) . ? 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 C5A C1A C2A 108.28(18) . . ? C5A C1A C6A 126.3(2) . . ? C2A C1A C6A 124.7(2) . . ? C5A C1A Ti1F 80.78(14) . . ? C2A C1A Ti1F 80.68(15) . . ? C6A C1A Ti1F 113.23(18) . . ? C5A C1A Ti1 72.06(11) . . ? C2A C1A Ti1 73.17(11) . . ? C6A C1A Ti1 127.96(15) . . ? Ti1F C1A Ti1 14.73(9) . . ? C3A C2A C1A 108.18(18) . . ? C3A C2A C7A 125.9(2) . . ? C1A C2A C7A 125.31(19) . . ? C3A C2A Ti1F 85.57(15) . . ? C1A C2A Ti1F 63.23(13) . . ? C7A C2A Ti1F 123.56(16) . . ? C3A C2A Ti1 70.21(11) . . ? C1A C2A Ti1 73.64(11) . . ? C7A C2A Ti1 129.09(15) . . ? Ti1F C2A Ti1 15.94(9) . . ? C2A C3A C4A 107.96(18) . . ? C2A C3A C8A 125.7(2) . . ? C4A C3A C8A 126.33(19) . . ? C2A C3A Ti1 76.16(12) . . ? C4A C3A Ti1 70.54(11) . . ? C8A C3A Ti1 120.81(14) . . ? C2A C3A Ti1F 62.54(13) . . ? C4A C3A Ti1F 73.35(13) . . ? C8A C3A Ti1F 131.07(16) . . ? Ti1 C3A Ti1F 14.21(7) . . ? C3A C4A C5A 107.94(17) . . ? C3A C4A C9A 124.9(2) . . ? C5A C4A C9A 127.1(2) . . ? C3A C4A Ti1 74.73(12) . . ? C5A C4A Ti1 76.70(12) . . ? C9A C4A Ti1 117.84(13) . . ? C3A C4A Ti1F 75.66(13) . . ? C5A C4A Ti1F 63.54(13) . . ? C9A C4A Ti1F 129.30(15) . . ? Ti1 C4A Ti1F 14.20(7) . . ? C1A C5A C4A 107.51(18) . . ? C1A C5A C10A 125.3(2) . . ? C4A C5A C10A 125.4(2) . . ? C1A C5A Ti1F 63.22(13) . . ? C4A C5A Ti1F 83.88(15) . . ? C10A C5A Ti1F 129.63(16) . . ? C1A C5A Ti1 74.63(12) . . ? C4A C5A Ti1 68.74(11) . . ? C10A C5A Ti1 133.96(14) . . ? Ti1F C5A Ti1 16.12(9) . . ? C1A C6A H6A1 109.5 . . ? C1A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? C1A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C2A C7A H7A1 109.5 . . ? C2A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? C2A C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C3A C8A H8A1 109.5 . . ? C3A C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? C3A C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? C4A C9A H9A1 109.5 . . ? C4A C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? C4A C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? C5A C10A C11A 110.89(18) . . ? C5A C10A H10A 109.5 . . ? C11A C10A H10A 109.5 . . ? C5A C10A H10B 109.5 . . ? C11A C10A H10B 109.5 . . ? H10A C10A H10B 108.1 . . ? C10A C11A H11A 109.5 . . ? C10A C11A H11B 109.5 . . ? H11A C11A H11B 109.5 . . ? C10A C11A H11C 109.5 . . ? H11A C11A H11C 109.5 . . ? H11B C11A H11C 109.5 . . ? C2B C1B C5B 107.92(18) . . ? C2B C1B C6B 124.0(2) . . ? C5B C1B C6B 127.1(2) . . ? C2B C1B Ti1F 72.98(14) . . ? C5B C1B Ti1F 85.65(15) . . ? C6B C1B Ti1F 116.59(16) . . ? C2B C1B Ti1 74.08(12) . . ? C5B C1B Ti1 71.08(11) . . ? C6B C1B Ti1 129.29(14) . . ? Ti1F C1B Ti1 15.40(9) . . ? C1B C2B C3B 107.91(19) . . ? C1B C2B C7B 125.4(2) . . ? C3B C2B C7B 126.1(2) . . ? C1B C2B Ti1F 69.79(13) . . ? C3B C2B Ti1F 85.24(16) . . ? C7B C2B Ti1F 118.18(17) . . ? C1B C2B Ti1 72.70(12) . . ? C3B C2B Ti1 70.21(11) . . ? C7B C2B Ti1 129.72(15) . . ? Ti1F C2B Ti1 15.44(9) . . ? C4B C3B C2B 108.20(18) . . ? C4B C3B C8B 125.2(2) . . ? C2B C3B C8B 126.6(2) . . ? C4B C3B Ti1 71.69(11) . . ? C2B C3B Ti1 76.07(12) . . ? C8B C3B Ti1 120.37(14) . . ? C4B C3B Ti1F 81.30(14) . . ? C2B C3B Ti1F 61.00(13) . . ? C8B C3B Ti1F 125.12(16) . . ? Ti1 C3B Ti1F 15.43(8) . . ? C3B C4B C5B 108.19(18) . . ? C3B C4B C9B 125.4(2) . . ? C5B C4B C9B 126.4(2) . . ? C3B C4B Ti1 73.99(12) . . ? C5B C4B Ti1 74.27(11) . . ? C9B C4B Ti1 120.09(14) . . ? C3B C4B Ti1F 67.82(13) . . ? C5B C4B Ti1F 66.88(12) . . ? C9B C4B Ti1F 133.34(16) . . ? Ti1 C4B Ti1F 13.27(7) . . ? C4B C5B C1B 107.76(18) . . ? C4B C5B C10B 123.79(19) . . ? C1B C5B C10B 126.32(19) . . ? C4B C5B Ti1 71.37(12) . . ? C1B C5B Ti1 74.94(12) . . ? C10B C5B Ti1 132.36(14) . . ? C4B C5B Ti1F 82.07(14) . . ? C1B C5B Ti1F 60.05(13) . . ? C10B C5B Ti1F 135.57(15) . . ? Ti1 C5B Ti1F 15.61(8) . . ? C1B C6B H6B1 109.5 . . ? C1B C6B H6B2 109.5 . . ? H6B1 C6B H6B2 109.5 . . ? C1B C6B H6B3 109.5 . . ? H6B1 C6B H6B3 109.5 . . ? H6B2 C6B H6B3 109.5 . . ? C2B C7B H7B1 109.5 . . ? C2B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? C2B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? C3B C8B H8B1 109.5 . . ? C3B C8B H8B2 109.5 . . ? H8B1 C8B H8B2 109.5 . . ? C3B C8B H8B3 109.5 . . ? H8B1 C8B H8B3 109.5 . . ? H8B2 C8B H8B3 109.5 . . ? C4B C9B H9B1 109.5 . . ? C4B C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? C4B C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? C5B C10B C11B 110.72(18) . . ? C5B C10B H10C 109.5 . . ? C11B C10B H10C 109.5 . . ? C5B C10B H10D 109.5 . . ? C11B C10B H10D 109.5 . . ? H10C C10B H10D 108.1 . . ? C10B C11B H11D 109.5 . . ? C10B C11B H11E 109.5 . . ? H11D C11B H11E 109.5 . . ? C10B C11B H11F 109.5 . . ? H11D C11B H11F 109.5 . . ? H11E C11B H11F 109.5 . . ? C2 C1 F1 110.8(2) . . ? C2 C1 Ti1 131.54(18) . . ? F1 C1 Ti1 117.61(15) . . ? C1 C2 F3 124.8(3) . . ? C1 C2 F2 126.3(2) . . ? F3 C2 F2 108.8(2) . . ? F4 Ti1 C1 92.46(8) . . ? F4 Ti1 C4A 89.07(7) . . ? C1 Ti1 C4A 129.68(8) . . ? F4 Ti1 C4B 77.97(7) . . ? C1 Ti1 C4B 118.16(8) . . ? C4A Ti1 C4B 111.31(7) . . ? F4 Ti1 C3A 76.04(7) . . ? C1 Ti1 C3A 97.51(8) . . ? C4A Ti1 C3A 34.73(7) . . ? C4B Ti1 C3A 136.31(7) . . ? F4 Ti1 C3B 81.99(7) . . ? C1 Ti1 C3B 84.06(8) . . ? C4A Ti1 C3B 145.59(7) . . ? C4B Ti1 C3B 34.32(7) . . ? C3A Ti1 C3B 158.01(7) . . ? F4 Ti1 C5B 108.35(7) . . ? C1 Ti1 C5B 130.69(8) . . ? C4A Ti1 C5B 95.75(7) . . ? C4B Ti1 C5B 34.37(7) . . ? C3A Ti1 C5B 130.30(7) . . ? C3B Ti1 C5B 56.73(7) . . ? F4 Ti1 C5A 123.63(7) . . ? C1 Ti1 C5A 120.25(8) . . ? C4A Ti1 C5A 34.56(7) . . ? C4B Ti1 C5A 115.16(7) . . ? C3A Ti1 C5A 56.64(7) . . ? C3B Ti1 C5A 140.23(7) . . ? C5B Ti1 C5A 84.79(7) . . ? F4 Ti1 C1B 133.72(6) . . ? C1 Ti1 C1B 100.90(8) . . ? C4A Ti1 C1B 113.67(8) . . ? C4B Ti1 C1B 56.59(7) . . ? C3A Ti1 C1B 143.48(7) . . ? C3B Ti1 C1B 56.12(7) . . ? C5B Ti1 C1B 33.99(7) . . ? C5A Ti1 C1B 86.84(7) . . ? F4 Ti1 C2A 100.58(7) . . ? C1 Ti1 C2A 73.78(8) . . ? C4A Ti1 C2A 56.60(7) . . ? C4B Ti1 C2A 167.91(7) . . ? C3A Ti1 C2A 33.63(7) . . ? C3B Ti1 C2A 157.75(8) . . ? C5B Ti1 C2A 139.64(7) . . ? C5A Ti1 C2A 55.50(7) . . ? C1B Ti1 C2A 125.68(7) . . ? F4 Ti1 C1A 131.36(7) . . ? C1 Ti1 C1A 86.95(8) . . ? C4A Ti1 C1A 56.59(7) . . ? C4B Ti1 C1A 142.69(8) . . ? C3A Ti1 C1A 55.95(7) . . ? C3B Ti1 C1A 145.86(7) . . ? C5B Ti1 C1A 108.41(7) . . ? C5A Ti1 C1A 33.31(7) . . ? C1B Ti1 C1A 93.75(7) . . ? C2A Ti1 C1A 33.20(7) . . ? F4 Ti1 C2B 114.48(7) . . ? C1 Ti1 C2B 74.79(8) . . ? C4A Ti1 C2B 146.88(8) . . ? C4B Ti1 C2B 56.29(7) . . ? C3A Ti1 C2B 166.80(7) . . ? C3B Ti1 C2B 33.73(7) . . ? C5B Ti1 C2B 55.94(7) . . ? C5A Ti1 C2B 117.64(7) . . ? C1B Ti1 C2B 33.22(7) . . ? C2A Ti1 C2B 133.27(7) . . ? C1A Ti1 C2B 112.19(7) . . ? C2F C1F F1F 112.4(11) . . ? C2F C1F Ti1F 130.0(8) . . ? F1F C1F Ti1F 117.6(8) . . ? F2F C2F F3F 109.0(11) . . ? F2F C2F C1F 124.2(12) . . ? F3F C2F C1F 126.8(13) . . ? F4F Ti1F C1A 79.7(3) . . ? F4F Ti1F C1F 91.8(4) . . ? C1A Ti1F C1F 116.3(4) . . ? F4F Ti1F C1B 95.4(3) . . ? C1A Ti1F C1B 112.57(16) . . ? C1F Ti1F C1B 131.1(4) . . ? F4F Ti1F C2B 79.5(3) . . ? C1A Ti1F C2B 140.2(2) . . ? C1F Ti1F C2B 98.0(4) . . ? C1B Ti1F C2B 37.23(9) . . ? F4F Ti1F C2A 82.7(3) . . ? C1A Ti1F C2A 36.09(9) . . ? C1F Ti1F C2A 80.3(4) . . ? C1B Ti1F C2A 148.56(16) . . ? C2B Ti1F C2A 162.08(18) . . ? F4F Ti1F C5A 113.1(3) . . ? C1A Ti1F C5A 36.00(8) . . ? C1F Ti1F C5A 125.6(4) . . ? C1B Ti1F C5A 95.30(13) . . ? C2B Ti1F C5A 132.52(14) . . ? C2A Ti1F C5A 57.79(9) . . ? F4F Ti1F C5B 129.6(3) . . ? C1A Ti1F C5B 116.23(13) . . ? C1F Ti1F C5B 117.0(3) . . ? C1B Ti1F C5B 34.30(8) . . ? C2B Ti1F C5B 57.33(9) . . ? C2A Ti1F C5B 139.17(14) . . ? C5A Ti1F C5B 83.99(11) . . ? F4F Ti1F C3B 103.7(3) . . ? C1A Ti1F C3B 169.24(15) . . ? C1F Ti1F C3B 74.1(4) . . ? C1B Ti1F C3B 57.24(9) . . ? C2B Ti1F C3B 33.76(8) . . ? C2A Ti1F C3B 153.69(17) . . ? C5A Ti1F C3B 136.20(14) . . ? C5B Ti1F C3B 53.69(9) . . ? F4F Ti1F C4A 133.7(3) . . ? C1A Ti1F C4A 56.13(9) . . ? C1F Ti1F C4A 95.6(3) . . ? C1B Ti1F C4A 112.66(13) . . ? C2B Ti1F C4A 143.47(15) . . ? C2A Ti1F C4A 54.06(9) . . ? C5A Ti1F C4A 32.58(8) . . ? C5B Ti1F C4A 86.30(11) . . ? C3B Ti1F C4A 122.26(16) . . ? F4F Ti1F C3A 113.4(3) . . ? C1A Ti1F C3A 55.60(9) . . ? C1F Ti1F C3A 72.0(4) . . ? C1B Ti1F C3A 143.65(15) . . ? C2B Ti1F C3A 163.32(19) . . ? C2A Ti1F C3A 31.88(7) . . ? C5A Ti1F C3A 53.95(9) . . ? C5B Ti1F C3A 114.59(14) . . ? C3B Ti1F C3A 129.64(17) . . ? C4A Ti1F C3A 31.00(7) . . ? F4F Ti1F C4B 132.6(3) . . ? C1A Ti1F C4B 141.95(15) . . ? C1F Ti1F C4B 86.2(3) . . ? C1B Ti1F C4B 54.48(9) . . ? C2B Ti1F C4B 54.11(9) . . ? C2A Ti1F C4B 142.72(17) . . ? C5A Ti1F C4B 106.05(13) . . ? C5B Ti1F C4B 31.05(7) . . ? C3B Ti1F C4B 30.88(8) . . ? C4A Ti1F C4B 93.44(13) . . ? C3A Ti1F C4B 110.84(15) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.504 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.067 # Attachment '4a.CIF' data_rktioh _database_code_depnum_ccdc_archive 'CCDC 757337' #TrackingRef '4a.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Sodium-oxo-bis(pentamethylcylopentadienyl)- (trifluoroethenyl)titanate(IV) ; _chemical_name_common ;Sodium-oxo-bis(pentamethylcylopentadienyl)- (trifluoroethenyl)titanate(IV) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H54 F3 Na O4 Ti' _chemical_formula_weight 654.66 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' Na Na 0.0362 0.0249 '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 9.0526(17) _cell_length_b 14.710(3) _cell_length_c 26.010(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.099(4) _cell_angle_gamma 90.00 _cell_volume 3458.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 29.7 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 0.311 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.915 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'SADABS (Brukler-AXS)' _exptl_special_details ; The ration Tmin/Tmax is provided by the program ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD Bruker-AXS' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40911 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 30.57 _reflns_number_total 10352 _reflns_number_gt 7481 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker-AXS)' _computing_cell_refinement 'SAINT (Bruker-AXS)' _computing_data_reduction 'SAINT (Bruker-AXS)' _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^)+(0.0634P)^2^+1.3179P] 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 10352 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1306 _refine_ls_wR_factor_gt 0.1136 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 Ti1 Ti 0.25516(3) 0.751645(17) 0.403233(10) 0.02197(7) Uani 1 1 d . . . Na1 Na 0.32866(7) 0.97827(4) 0.34142(3) 0.03264(15) Uani 1 1 d . . . C1 C 0.04405(17) 0.77903(12) 0.36029(6) 0.0312(3) Uani 1 1 d . . . C2 C 0.00122(18) 0.84530(13) 0.32900(7) 0.0361(4) Uani 1 1 d . . . C10C C 0.32534(18) 0.81206(11) 0.48814(6) 0.0301(3) Uani 1 1 d . . . C1CP C 0.4238(2) 0.68146(12) 0.34301(7) 0.0416(4) Uani 1 1 d . . . C2CP C 0.2813(3) 0.65876(14) 0.32423(7) 0.0498(5) Uani 1 1 d . . . C3CP C 0.2205(2) 0.59643(13) 0.35905(8) 0.0435(5) Uani 1 1 d . . . C4CP C 0.32536(18) 0.58187(10) 0.39941(6) 0.0312(3) Uani 1 1 d . . . C5CP C 0.44991(18) 0.63745(11) 0.39068(6) 0.0308(3) Uani 1 1 d . . . C6CP C 0.19599(18) 0.85908(10) 0.47161(6) 0.0279(3) Uani 1 1 d . . . C7CP C 0.07676(18) 0.79744(12) 0.47086(6) 0.0323(3) Uani 1 1 d . . . C8CP C 0.1310(2) 0.71204(12) 0.48839(7) 0.0363(4) Uani 1 1 d . . . C9CP C 0.2839(2) 0.72114(12) 0.49958(6) 0.0348(4) Uani 1 1 d . . . C1L C 0.5198(3) 0.96630(18) 0.23414(11) 0.0643(7) Uani 1 1 d . . . H1L1 H 0.5869 0.9336 0.2591 0.077 Uiso 1 1 calc R . . H1L2 H 0.5670 1.0243 0.2248 0.077 Uiso 1 1 calc R . . C2L C 0.4865(5) 0.9093(2) 0.18718(13) 0.0992(12) Uani 1 1 d . . . H2L1 H 0.5460 0.9295 0.1584 0.119 Uiso 1 1 calc R . . H2L2 H 0.5082 0.8444 0.1945 0.119 Uiso 1 1 calc R . . C3L C 0.3255(5) 0.9231(3) 0.17428(12) 0.1006(12) Uani 1 1 d . . . H3L1 H 0.3091 0.9478 0.1390 0.121 Uiso 1 1 calc R . . H3L2 H 0.2709 0.8650 0.1766 0.121 Uiso 1 1 calc R . . C4L C 0.2769(3) 0.9880(2) 0.21250(9) 0.0727(8) Uani 1 1 d . . . H4L1 H 0.2744 1.0503 0.1981 0.087 Uiso 1 1 calc R . . H4L2 H 0.1766 0.9723 0.2230 0.087 Uiso 1 1 calc R . . C5L C 0.1771(4) 1.17566(19) 0.30196(9) 0.0788(9) Uani 1 1 d . . . H5L1 H 0.0981 1.1467 0.2798 0.095 Uiso 1 1 calc R . . H5L2 H 0.2657 1.1827 0.2816 0.095 Uiso 1 1 calc R . . C6L C 0.1270(3) 1.26592(15) 0.31931(10) 0.0601(6) Uani 1 1 d . . . H6L1 H 0.0180 1.2714 0.3151 0.072 Uiso 1 1 calc R . . H6L2 H 0.1728 1.3154 0.2998 0.072 Uiso 1 1 calc R . . C7L C 0.1779(4) 1.26866(15) 0.37482(10) 0.0669(7) Uani 1 1 d . . . H7L1 H 0.1072 1.3028 0.3952 0.080 Uiso 1 1 calc R . . H7L2 H 0.2766 1.2974 0.3794 0.080 Uiso 1 1 calc R . . C8L C 0.1843(2) 1.17048(13) 0.39062(8) 0.0443(4) Uani 1 1 d . . . H8L1 H 0.2650 1.1604 0.4172 0.053 Uiso 1 1 calc R . . H8L2 H 0.0896 1.1515 0.4047 0.053 Uiso 1 1 calc R . . C9L C 0.5862(2) 1.13939(13) 0.36014(9) 0.0458(4) Uani 1 1 d . . . H9L1 H 0.5285 1.1836 0.3796 0.055 Uiso 1 1 calc R . . H9L2 H 0.5673 1.1511 0.3229 0.055 Uiso 1 1 calc R . . C10L C 0.7495(2) 1.14832(14) 0.37493(8) 0.0429(4) Uani 1 1 d . . . H10D H 0.7660 1.1722 0.4104 0.052 Uiso 1 1 calc R . . H10E H 0.7995 1.1884 0.3507 0.052 Uiso 1 1 calc R . . C11L C 0.8023(2) 1.05108(16) 0.37112(11) 0.0609(6) Uani 1 1 d . . . H11A H 0.8234 1.0353 0.3353 0.073 Uiso 1 1 calc R . . H11B H 0.8922 1.0405 0.3937 0.073 Uiso 1 1 calc R . . C12L C 0.6741(2) 0.99782(14) 0.38890(9) 0.0509(5) Uani 1 1 d . . . H12A H 0.6717 0.9364 0.3733 0.061 Uiso 1 1 calc R . . H12B H 0.6807 0.9915 0.4268 0.061 Uiso 1 1 calc R . . C1M C 0.5316(4) 0.74179(16) 0.31763(12) 0.0831(10) Uani 1 1 d . . . H1M1 H 0.5682 0.7108 0.2875 0.125 Uiso 1 1 calc R . . H1M2 H 0.6149 0.7556 0.3420 0.125 Uiso 1 1 calc R . . H1M3 H 0.4823 0.7985 0.3068 0.125 Uiso 1 1 calc R . . C2M C 0.2130(4) 0.6875(3) 0.27285(9) 0.1111(15) Uani 1 1 d . . . H2M1 H 0.2375 0.7513 0.2665 0.167 Uiso 1 1 calc R . . H2M2 H 0.1053 0.6806 0.2728 0.167 Uiso 1 1 calc R . . H2M3 H 0.2517 0.6495 0.2457 0.167 Uiso 1 1 calc R . . C3M C 0.0806(3) 0.54179(18) 0.34993(15) 0.0917(12) Uani 1 1 d . . . H3M1 H 0.1053 0.4811 0.3375 0.137 Uiso 1 1 calc R . . H3M2 H 0.0152 0.5724 0.3241 0.137 Uiso 1 1 calc R . . H3M3 H 0.0304 0.5363 0.3822 0.137 Uiso 1 1 calc R . . C4M C 0.3185(3) 0.50678(13) 0.43808(9) 0.0552(6) Uani 1 1 d . . . H4M1 H 0.2251 0.5106 0.4553 0.083 Uiso 1 1 calc R . . H4M2 H 0.4015 0.5126 0.4636 0.083 Uiso 1 1 calc R . . H4M3 H 0.3243 0.4480 0.4206 0.083 Uiso 1 1 calc R . . C5M C 0.5970(2) 0.63576(16) 0.42078(10) 0.0549(6) Uani 1 1 d . . . H5M1 H 0.6761 0.6246 0.3973 0.082 Uiso 1 1 calc R . . H5M2 H 0.5969 0.5872 0.4466 0.082 Uiso 1 1 calc R . . H5M3 H 0.6137 0.6944 0.4381 0.082 Uiso 1 1 calc R . . C6M C 0.1861(2) 0.95751(11) 0.45735(7) 0.0407(4) Uani 1 1 d . . . H6M1 H 0.1472 0.9921 0.4859 0.061 Uiso 1 1 calc R . . H6M2 H 0.1199 0.9647 0.4265 0.061 Uiso 1 1 calc R . . H6M3 H 0.2847 0.9802 0.4503 0.061 Uiso 1 1 calc R . . C7M C -0.0838(2) 0.82250(16) 0.46215(8) 0.0495(5) Uani 1 1 d . . . H7M1 H -0.1396 0.7696 0.4489 0.074 Uiso 1 1 calc R . . H7M2 H -0.0935 0.8722 0.4371 0.074 Uiso 1 1 calc R . . H7M3 H -0.1230 0.8421 0.4948 0.074 Uiso 1 1 calc R . . C8M C 0.0342(3) 0.63101(15) 0.49778(10) 0.0648(7) Uani 1 1 d . . . H8M1 H -0.0506 0.6502 0.5170 0.097 Uiso 1 1 calc R . . H8M2 H 0.0914 0.5853 0.5178 0.097 Uiso 1 1 calc R . . H8M3 H -0.0010 0.6048 0.4647 0.097 Uiso 1 1 calc R . . C9M C 0.3826(3) 0.65741(15) 0.53101(8) 0.0583(6) Uani 1 1 d . . . H9M1 H 0.3985 0.6814 0.5660 0.087 Uiso 1 1 calc R . . H9M2 H 0.4779 0.6519 0.5151 0.087 Uiso 1 1 calc R . . H9M3 H 0.3357 0.5975 0.5323 0.087 Uiso 1 1 calc R . . C10M C 0.4767(2) 0.85282(15) 0.49575(8) 0.0458(5) Uani 1 1 d . . . H10A H 0.4971 0.8907 0.4660 0.069 Uiso 1 1 calc R . . H10B H 0.5505 0.8041 0.4993 0.069 Uiso 1 1 calc R . . H10C H 0.4815 0.8903 0.5270 0.069 Uiso 1 1 calc R . . F1 F -0.07233(11) 0.71701(8) 0.36417(5) 0.0453(3) Uani 1 1 d . . . F2 F -0.13089(12) 0.85449(9) 0.30345(5) 0.0516(3) Uani 1 1 d . . . F3 F 0.08500(12) 0.91605(8) 0.31618(5) 0.0507(3) Uani 1 1 d . . . O1 O 0.33641(12) 0.84474(7) 0.37963(4) 0.0290(2) Uani 1 1 d . . . O1L O 0.38094(16) 0.98270(11) 0.25538(5) 0.0521(4) Uani 1 1 d . . . O2L O 0.21102(17) 1.12091(9) 0.34527(5) 0.0498(3) Uani 1 1 d . . . O3L O 0.54484(14) 1.04827(9) 0.37245(6) 0.0441(3) 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 0.02403(12) 0.01922(12) 0.02252(12) -0.00075(9) 0.00010(8) 0.00008(10) Na1 0.0386(3) 0.0251(3) 0.0342(3) 0.0019(3) 0.0011(3) -0.0018(3) C1 0.0249(7) 0.0355(8) 0.0331(8) -0.0059(6) 0.0011(6) 0.0011(6) C2 0.0263(7) 0.0470(10) 0.0345(9) -0.0024(7) -0.0029(6) 0.0073(7) C10C 0.0368(8) 0.0312(8) 0.0219(7) -0.0024(6) -0.0024(6) -0.0009(6) C1CP 0.0591(11) 0.0305(8) 0.0372(9) 0.0012(7) 0.0208(8) 0.0133(8) C2CP 0.0735(14) 0.0467(11) 0.0278(9) -0.0132(8) -0.0101(9) 0.0319(10) C3CP 0.0373(9) 0.0326(9) 0.0590(12) -0.0224(8) -0.0137(8) 0.0064(7) C4CP 0.0359(8) 0.0195(7) 0.0380(8) -0.0036(6) 0.0022(6) 0.0014(6) C5CP 0.0306(8) 0.0250(7) 0.0368(8) -0.0050(6) 0.0009(6) 0.0016(6) C6CP 0.0380(8) 0.0224(7) 0.0233(7) -0.0030(5) 0.0024(6) 0.0003(6) C7CP 0.0353(8) 0.0336(8) 0.0288(8) -0.0076(6) 0.0083(6) -0.0010(7) C8CP 0.0514(10) 0.0276(8) 0.0314(8) -0.0032(6) 0.0149(7) -0.0063(7) C9CP 0.0542(10) 0.0280(7) 0.0222(7) 0.0016(6) 0.0033(7) 0.0069(7) C1L 0.0548(13) 0.0604(14) 0.0798(17) 0.0230(13) 0.0244(12) -0.0013(11) C2L 0.142(3) 0.076(2) 0.087(2) -0.0023(17) 0.070(2) 0.019(2) C3L 0.157(4) 0.084(2) 0.0601(18) -0.0220(16) -0.001(2) -0.002(2) C4L 0.0702(16) 0.109(2) 0.0383(12) -0.0004(13) -0.0030(11) 0.0117(15) C5L 0.120(2) 0.0738(18) 0.0411(12) -0.0049(11) -0.0142(13) 0.0484(17) C6L 0.0795(16) 0.0410(11) 0.0595(14) 0.0114(10) 0.0014(12) 0.0085(11) C7L 0.111(2) 0.0334(11) 0.0569(14) -0.0060(9) 0.0099(14) -0.0007(12) C8L 0.0503(11) 0.0409(10) 0.0416(10) 0.0009(8) 0.0016(8) -0.0011(8) C9L 0.0423(10) 0.0336(9) 0.0612(12) 0.0071(8) -0.0006(9) -0.0014(8) C10L 0.0413(10) 0.0418(10) 0.0459(10) 0.0007(8) 0.0039(8) -0.0081(8) C11L 0.0402(11) 0.0507(13) 0.0921(18) 0.0087(12) 0.0061(11) 0.0039(9) C12L 0.0438(11) 0.0399(10) 0.0680(14) 0.0109(9) -0.0064(10) 0.0005(8) C1M 0.111(2) 0.0456(13) 0.101(2) 0.0211(13) 0.0783(19) 0.0227(14) C2M 0.166(3) 0.134(3) 0.0302(11) -0.0225(14) -0.0236(15) 0.107(3) C3M 0.0462(13) 0.0549(15) 0.170(3) -0.0595(18) -0.0331(16) 0.0027(11) C4M 0.0817(16) 0.0236(8) 0.0621(13) 0.0060(8) 0.0214(12) 0.0032(9) C5M 0.0322(9) 0.0584(13) 0.0727(15) -0.0200(11) -0.0093(9) 0.0056(9) C6M 0.0630(12) 0.0231(7) 0.0362(9) -0.0027(6) 0.0041(8) 0.0048(8) C7M 0.0342(9) 0.0631(13) 0.0524(12) -0.0195(10) 0.0125(8) 0.0031(9) C8M 0.0883(18) 0.0403(11) 0.0702(15) -0.0049(10) 0.0439(14) -0.0213(11) C9M 0.0978(18) 0.0440(11) 0.0320(10) 0.0062(8) -0.0061(10) 0.0243(11) C10M 0.0404(10) 0.0559(12) 0.0400(10) -0.0117(9) -0.0074(8) -0.0065(9) F1 0.0296(5) 0.0430(6) 0.0629(7) -0.0051(5) -0.0012(5) -0.0064(4) F2 0.0375(6) 0.0663(8) 0.0490(7) -0.0018(6) -0.0159(5) 0.0143(5) F3 0.0425(6) 0.0550(7) 0.0542(7) 0.0231(6) -0.0020(5) 0.0029(5) O1 0.0339(6) 0.0246(5) 0.0289(5) 0.0006(4) 0.0044(4) -0.0026(4) O1L 0.0510(8) 0.0709(10) 0.0346(7) 0.0005(7) 0.0050(6) 0.0092(7) O2L 0.0665(9) 0.0349(7) 0.0474(8) -0.0031(6) -0.0018(7) 0.0115(6) O3L 0.0379(7) 0.0346(7) 0.0588(8) 0.0060(6) -0.0062(6) -0.0051(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 Ti1 O1 1.6859(11) . ? Ti1 C1 2.1980(16) . ? Ti1 C10C 2.4329(16) . ? Ti1 C6CP 2.4597(15) . ? Ti1 C5CP 2.4695(16) . ? Ti1 C1CP 2.4716(17) . ? Ti1 C2CP 2.4896(18) . ? Ti1 C7CP 2.5423(16) . ? Ti1 C9CP 2.5453(17) . ? Ti1 C3CP 2.5677(17) . ? Ti1 C4CP 2.5802(16) . ? Ti1 C8CP 2.6037(17) . ? Na1 O1 2.2007(13) . ? Na1 O1L 2.3133(15) . ? Na1 O3L 2.3174(15) . ? Na1 O2L 2.3576(15) . ? Na1 F3 2.4449(14) . ? C1 C2 1.315(2) . ? C1 F1 1.4014(19) . ? C2 F3 1.341(2) . ? C2 F2 1.3432(19) . ? C10C C6CP 1.407(2) . ? C10C C9CP 1.425(2) . ? C10C C10M 1.499(2) . ? C1CP C2CP 1.395(3) . ? C1CP C5CP 1.407(2) . ? C1CP C1M 1.499(3) . ? C2CP C3CP 1.420(3) . ? C2CP C2M 1.503(3) . ? C3CP C4CP 1.393(2) . ? C3CP C3M 1.508(3) . ? C4CP C5CP 1.421(2) . ? C4CP C4M 1.498(3) . ? C5CP C5M 1.508(3) . ? C6CP C7CP 1.409(2) . ? C6CP C6M 1.496(2) . ? C7CP C8CP 1.415(3) . ? C7CP C7M 1.505(3) . ? C8CP C9CP 1.406(3) . ? C8CP C8M 1.507(3) . ? C9CP C9M 1.506(3) . ? C1L O1L 1.420(3) . ? C1L C2L 1.499(4) . ? C1L H1L1 0.9900 . ? C1L H1L2 0.9900 . ? C2L C3L 1.492(5) . ? C2L H2L1 0.9900 . ? C2L H2L2 0.9900 . ? C3L C4L 1.463(4) . ? C3L H3L1 0.9900 . ? C3L H3L2 0.9900 . ? C4L O1L 1.423(3) . ? C4L H4L1 0.9900 . ? C4L H4L2 0.9900 . ? C5L O2L 1.405(3) . ? C5L C6L 1.481(3) . ? C5L H5L1 0.9900 . ? C5L H5L2 0.9900 . ? C6L C7L 1.492(4) . ? C6L H6L1 0.9900 . ? C6L H6L2 0.9900 . ? C7L C8L 1.502(3) . ? C7L H7L1 0.9900 . ? C7L H7L2 0.9900 . ? C8L O2L 1.419(2) . ? C8L H8L1 0.9900 . ? C8L H8L2 0.9900 . ? C9L O3L 1.433(2) . ? C9L C10L 1.513(3) . ? C9L H9L1 0.9900 . ? C9L H9L2 0.9900 . ? C10L C11L 1.513(3) . ? C10L H10D 0.9900 . ? C10L H10E 0.9900 . ? C11L C12L 1.494(3) . ? C11L H11A 0.9900 . ? C11L H11B 0.9900 . ? C12L O3L 1.431(2) . ? C12L H12A 0.9900 . ? C12L H12B 0.9900 . ? C1M H1M1 0.9800 . ? C1M H1M2 0.9800 . ? C1M H1M3 0.9800 . ? C2M H2M1 0.9800 . ? C2M H2M2 0.9800 . ? C2M H2M3 0.9800 . ? C3M H3M1 0.9800 . ? C3M H3M2 0.9800 . ? C3M H3M3 0.9800 . ? C4M H4M1 0.9800 . ? C4M H4M2 0.9800 . ? C4M H4M3 0.9800 . ? C5M H5M1 0.9800 . ? C5M H5M2 0.9800 . ? C5M H5M3 0.9800 . ? C6M H6M1 0.9800 . ? C6M H6M2 0.9800 . ? C6M H6M3 0.9800 . ? C7M H7M1 0.9800 . ? C7M H7M2 0.9800 . ? C7M H7M3 0.9800 . ? C8M H8M1 0.9800 . ? C8M H8M2 0.9800 . ? C8M H8M3 0.9800 . ? C9M H9M1 0.9800 . ? C9M H9M2 0.9800 . ? C9M H9M3 0.9800 . ? C10M H10A 0.9800 . ? C10M H10B 0.9800 . ? C10M H10C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ti1 C1 92.90(6) . . ? O1 Ti1 C10C 86.34(6) . . ? C1 Ti1 C10C 124.85(6) . . ? O1 Ti1 C6CP 81.82(5) . . ? C1 Ti1 C6CP 91.85(6) . . ? C10C Ti1 C6CP 33.42(5) . . ? O1 Ti1 C5CP 100.12(6) . . ? C1 Ti1 C5CP 131.67(6) . . ? C10C Ti1 C5CP 102.43(6) . . ? C6CP Ti1 C5CP 135.85(5) . . ? O1 Ti1 C1CP 79.16(6) . . ? C1 Ti1 C1CP 107.72(7) . . ? C10C Ti1 C1CP 126.01(7) . . ? C6CP Ti1 C1CP 153.22(7) . . ? C5CP Ti1 C1CP 33.10(6) . . ? O1 Ti1 C2CP 94.73(7) . . ? C1 Ti1 C2CP 78.46(6) . . ? C10C Ti1 C2CP 156.63(6) . . ? C6CP Ti1 C2CP 169.58(6) . . ? C5CP Ti1 C2CP 54.36(6) . . ? C1CP Ti1 C2CP 32.67(7) . . ? O1 Ti1 C7CP 110.04(6) . . ? C1 Ti1 C7CP 74.67(6) . . ? C10C Ti1 C7CP 54.52(6) . . ? C6CP Ti1 C7CP 32.67(5) . . ? C5CP Ti1 C7CP 139.15(6) . . ? C1CP Ti1 C7CP 170.55(6) . . ? C2CP Ti1 C7CP 143.97(7) . . ? O1 Ti1 C9CP 118.58(6) . . ? C1 Ti1 C9CP 124.92(6) . . ? C10C Ti1 C9CP 33.16(6) . . ? C6CP Ti1 C9CP 54.27(5) . . ? C5CP Ti1 C9CP 88.54(6) . . ? C1CP Ti1 C9CP 121.10(6) . . ? C2CP Ti1 C9CP 134.97(6) . . ? C7CP Ti1 C9CP 53.16(6) . . ? O1 Ti1 C3CP 127.19(7) . . ? C1 Ti1 C3CP 81.59(6) . . ? C10C Ti1 C3CP 138.65(6) . . ? C6CP Ti1 C3CP 150.32(6) . . ? C5CP Ti1 C3CP 53.61(6) . . ? C1CP Ti1 C3CP 53.81(7) . . ? C2CP Ti1 C3CP 32.58(8) . . ? C7CP Ti1 C3CP 118.59(6) . . ? C9CP Ti1 C3CP 106.70(7) . . ? O1 Ti1 C4CP 131.22(5) . . ? C1 Ti1 C4CP 111.53(6) . . ? C10C Ti1 C4CP 109.62(6) . . ? C6CP Ti1 C4CP 135.52(5) . . ? C5CP Ti1 C4CP 32.59(5) . . ? C1CP Ti1 C4CP 53.80(6) . . ? C2CP Ti1 C4CP 53.30(6) . . ? C7CP Ti1 C4CP 116.75(6) . . ? C9CP Ti1 C4CP 81.67(5) . . ? C3CP Ti1 C4CP 31.40(6) . . ? O1 Ti1 C8CP 135.12(5) . . ? C1 Ti1 C8CP 94.00(6) . . ? C10C Ti1 C8CP 54.06(6) . . ? C6CP Ti1 C8CP 53.68(5) . . ? C5CP Ti1 C8CP 107.73(6) . . ? C1CP Ti1 C8CP 139.08(6) . . ? C2CP Ti1 C8CP 130.09(7) . . ? C7CP Ti1 C8CP 31.90(6) . . ? C9CP Ti1 C8CP 31.66(6) . . ? C3CP Ti1 C8CP 97.69(7) . . ? C4CP Ti1 C8CP 86.26(5) . . ? O1 Na1 O1L 117.31(6) . . ? O1 Na1 O3L 103.51(5) . . ? O1L Na1 O3L 96.39(6) . . ? O1 Na1 O2L 141.13(6) . . ? O1L Na1 O2L 97.62(6) . . ? O3L Na1 O2L 87.98(6) . . ? O1 Na1 F3 78.07(4) . . ? O1L Na1 F3 88.83(5) . . ? O3L Na1 F3 172.96(6) . . ? O2L Na1 F3 86.65(5) . . ? O1 Na1 Ti1 11.97(3) . . ? O1L Na1 Ti1 119.13(5) . . ? O3L Na1 Ti1 114.14(4) . . ? O2L Na1 Ti1 132.63(5) . . ? F3 Na1 Ti1 66.83(3) . . ? C2 C1 F1 109.24(14) . . ? C2 C1 Ti1 132.04(13) . . ? F1 C1 Ti1 118.72(11) . . ? C1 C2 F3 125.28(15) . . ? C1 C2 F2 127.29(17) . . ? F3 C2 F2 107.42(15) . . ? C6CP C10C C9CP 107.53(15) . . ? C6CP C10C C10M 125.69(16) . . ? C9CP C10C C10M 126.65(16) . . ? C6CP C10C Ti1 74.33(9) . . ? C9CP C10C Ti1 77.76(9) . . ? C10M C10C Ti1 117.25(11) . . ? C2CP C1CP C5CP 107.85(17) . . ? C2CP C1CP C1M 126.8(2) . . ? C5CP C1CP C1M 125.3(2) . . ? C2CP C1CP Ti1 74.37(10) . . ? C5CP C1CP Ti1 73.37(9) . . ? C1M C1CP Ti1 118.11(13) . . ? C1CP C2CP C3CP 108.28(16) . . ? C1CP C2CP C2M 124.9(3) . . ? C3CP C2CP C2M 126.5(3) . . ? C1CP C2CP Ti1 72.96(10) . . ? C3CP C2CP Ti1 76.74(10) . . ? C2M C2CP Ti1 121.78(14) . . ? C4CP C3CP C2CP 107.96(17) . . ? C4CP C3CP C3M 124.7(2) . . ? C2CP C3CP C3M 126.5(2) . . ? C4CP C3CP Ti1 74.79(9) . . ? C2CP C3CP Ti1 70.69(10) . . ? C3M C3CP Ti1 128.72(14) . . ? C3CP C4CP C5CP 107.79(16) . . ? C3CP C4CP C4M 124.62(18) . . ? C5CP C4CP C4M 126.43(17) . . ? C3CP C4CP Ti1 73.81(10) . . ? C5CP C4CP Ti1 69.42(9) . . ? C4M C4CP Ti1 131.97(12) . . ? C1CP C5CP C4CP 107.96(15) . . ? C1CP C5CP C5M 124.50(18) . . ? C4CP C5CP C5M 126.43(17) . . ? C1CP C5CP Ti1 73.53(9) . . ? C4CP C5CP Ti1 77.99(9) . . ? C5M C5CP Ti1 124.01(12) . . ? C10C C6CP C7CP 108.19(14) . . ? C10C C6CP C6M 126.10(16) . . ? C7CP C6CP C6M 125.71(16) . . ? C10C C6CP Ti1 72.24(9) . . ? C7CP C6CP Ti1 76.89(9) . . ? C6M C6CP Ti1 117.06(11) . . ? C6CP C7CP C8CP 108.35(15) . . ? C6CP C7CP C7M 125.28(17) . . ? C8CP C7CP C7M 125.53(17) . . ? C6CP C7CP Ti1 70.44(9) . . ? C8CP C7CP Ti1 76.44(9) . . ? C7M C7CP Ti1 127.25(12) . . ? C9CP C8CP C7CP 107.61(15) . . ? C9CP C8CP C8M 128.05(19) . . ? C7CP C8CP C8M 124.06(19) . . ? C9CP C8CP Ti1 71.88(9) . . ? C7CP C8CP Ti1 71.66(9) . . ? C8M C8CP Ti1 126.62(13) . . ? C8CP C9CP C10C 108.28(15) . . ? C8CP C9CP C9M 127.02(18) . . ? C10C C9CP C9M 122.87(18) . . ? C8CP C9CP Ti1 76.46(10) . . ? C10C C9CP Ti1 69.08(9) . . ? C9M C9CP Ti1 132.10(13) . . ? O1L C1L C2L 105.6(2) . . ? O1L C1L H1L1 110.6 . . ? C2L C1L H1L1 110.6 . . ? O1L C1L H1L2 110.6 . . ? C2L C1L H1L2 110.6 . . ? H1L1 C1L H1L2 108.7 . . ? C3L C2L C1L 104.9(2) . . ? C3L C2L H2L1 110.8 . . ? C1L C2L H2L1 110.8 . . ? C3L C2L H2L2 110.8 . . ? C1L C2L H2L2 110.8 . . ? H2L1 C2L H2L2 108.8 . . ? C4L C3L C2L 105.2(3) . . ? C4L C3L H3L1 110.7 . . ? C2L C3L H3L1 110.7 . . ? C4L C3L H3L2 110.7 . . ? C2L C3L H3L2 110.7 . . ? H3L1 C3L H3L2 108.8 . . ? O1L C4L C3L 106.6(3) . . ? O1L C4L H4L1 110.4 . . ? C3L C4L H4L1 110.4 . . ? O1L C4L H4L2 110.4 . . ? C3L C4L H4L2 110.4 . . ? H4L1 C4L H4L2 108.6 . . ? O2L C5L C6L 109.06(19) . . ? O2L C5L H5L1 109.9 . . ? C6L C5L H5L1 109.9 . . ? O2L C5L H5L2 109.9 . . ? C6L C5L H5L2 109.9 . . ? H5L1 C5L H5L2 108.3 . . ? C5L C6L C7L 103.60(19) . . ? C5L C6L H6L1 111.0 . . ? C7L C6L H6L1 111.0 . . ? C5L C6L H6L2 111.0 . . ? C7L C6L H6L2 111.0 . . ? H6L1 C6L H6L2 109.0 . . ? C6L C7L C8L 104.14(18) . . ? C6L C7L H7L1 110.9 . . ? C8L C7L H7L1 110.9 . . ? C6L C7L H7L2 110.9 . . ? C8L C7L H7L2 110.9 . . ? H7L1 C7L H7L2 108.9 . . ? O2L C8L C7L 105.81(17) . . ? O2L C8L H8L1 110.6 . . ? C7L C8L H8L1 110.6 . . ? O2L C8L H8L2 110.6 . . ? C7L C8L H8L2 110.6 . . ? H8L1 C8L H8L2 108.7 . . ? O3L C9L C10L 106.74(15) . . ? O3L C9L H9L1 110.4 . . ? C10L C9L H9L1 110.4 . . ? O3L C9L H9L2 110.4 . . ? C10L C9L H9L2 110.4 . . ? H9L1 C9L H9L2 108.6 . . ? C9L C10L C11L 102.05(16) . . ? C9L C10L H10D 111.4 . . ? C11L C10L H10D 111.4 . . ? C9L C10L H10E 111.4 . . ? C11L C10L H10E 111.4 . . ? H10D C10L H10E 109.2 . . ? C12L C11L C10L 102.83(17) . . ? C12L C11L H11A 111.2 . . ? C10L C11L H11A 111.2 . . ? C12L C11L H11B 111.2 . . ? C10L C11L H11B 111.2 . . ? H11A C11L H11B 109.1 . . ? O3L C12L C11L 105.77(17) . . ? O3L C12L H12A 110.6 . . ? C11L C12L H12A 110.6 . . ? O3L C12L H12B 110.6 . . ? C11L C12L H12B 110.6 . . ? H12A C12L H12B 108.7 . . ? C1CP C1M H1M1 109.5 . . ? C1CP C1M H1M2 109.5 . . ? H1M1 C1M H1M2 109.5 . . ? C1CP C1M H1M3 109.5 . . ? H1M1 C1M H1M3 109.5 . . ? H1M2 C1M H1M3 109.5 . . ? C2CP C2M H2M1 109.5 . . ? C2CP C2M H2M2 109.5 . . ? H2M1 C2M H2M2 109.5 . . ? C2CP C2M H2M3 109.5 . . ? H2M1 C2M H2M3 109.5 . . ? H2M2 C2M H2M3 109.5 . . ? C3CP C3M H3M1 109.5 . . ? C3CP C3M H3M2 109.5 . . ? H3M1 C3M H3M2 109.5 . . ? C3CP C3M H3M3 109.5 . . ? H3M1 C3M H3M3 109.5 . . ? H3M2 C3M H3M3 109.5 . . ? C4CP C4M H4M1 109.5 . . ? C4CP C4M H4M2 109.5 . . ? H4M1 C4M H4M2 109.5 . . ? C4CP C4M H4M3 109.5 . . ? H4M1 C4M H4M3 109.5 . . ? H4M2 C4M H4M3 109.5 . . ? C5CP C5M H5M1 109.5 . . ? C5CP C5M H5M2 109.5 . . ? H5M1 C5M H5M2 109.5 . . ? C5CP C5M H5M3 109.5 . . ? H5M1 C5M H5M3 109.5 . . ? H5M2 C5M H5M3 109.5 . . ? C6CP C6M H6M1 109.5 . . ? C6CP C6M H6M2 109.5 . . ? H6M1 C6M H6M2 109.5 . . ? C6CP C6M H6M3 109.5 . . ? H6M1 C6M H6M3 109.5 . . ? H6M2 C6M H6M3 109.5 . . ? C7CP C7M H7M1 109.5 . . ? C7CP C7M H7M2 109.5 . . ? H7M1 C7M H7M2 109.5 . . ? C7CP C7M H7M3 109.5 . . ? H7M1 C7M H7M3 109.5 . . ? H7M2 C7M H7M3 109.5 . . ? C8CP C8M H8M1 109.5 . . ? C8CP C8M H8M2 109.5 . . ? H8M1 C8M H8M2 109.5 . . ? C8CP C8M H8M3 109.5 . . ? H8M1 C8M H8M3 109.5 . . ? H8M2 C8M H8M3 109.5 . . ? C9CP C9M H9M1 109.5 . . ? C9CP C9M H9M2 109.5 . . ? H9M1 C9M H9M2 109.5 . . ? C9CP C9M H9M3 109.5 . . ? H9M1 C9M H9M3 109.5 . . ? H9M2 C9M H9M3 109.5 . . ? C10C C10M H10A 109.5 . . ? C10C C10M H10B 109.5 . . ? H10A C10M H10B 109.5 . . ? C10C C10M H10C 109.5 . . ? H10A C10M H10C 109.5 . . ? H10B C10M H10C 109.5 . . ? C2 F3 Na1 137.58(10) . . ? Ti1 O1 Na1 152.32(7) . . ? C1L O1L C4L 105.46(18) . . ? C1L O1L Na1 127.09(14) . . ? C4L O1L Na1 126.78(14) . . ? C5L O2L C8L 109.41(16) . . ? C5L O2L Na1 123.75(13) . . ? C8L O2L Na1 126.20(12) . . ? C12L O3L C9L 109.43(14) . . ? C12L O3L Na1 122.34(12) . . ? C9L O3L Na1 124.32(11) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 30.57 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.489 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.057 # Attachment '5a.CIF' data_rainer2 _database_code_depnum_ccdc_archive 'CCDC 757338' #TrackingRef '5a.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(pentamethylcyclopentadienyl)(trifluorethenyl)(trimethyl- siloxo)titatnium(IV) ; _chemical_name_common ; Bis(pentamethylcyclopentadienyl)(trifluorethenyl)(trimethyl- siloxo)titatnium(IV) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H39 F3 O Si Ti' _chemical_formula_weight 488.55 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' Si Si 0.0817 0.0704 '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' _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 8.996(2) _cell_length_b 9.886(3) _cell_length_c 14.979(4) _cell_angle_alpha 86.164(6) _cell_angle_beta 88.270(6) _cell_angle_gamma 73.370(6) _cell_volume 1273.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 914 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 30.3 _exptl_crystal_description platelett _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.274 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 0.419 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.725 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'SADABS (BRUKER-AXS)' _exptl_special_details ; The program SADABS provides the ratio of T_min/T_max ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER-AXS SMART CCD' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15049 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 30.56 _reflns_number_total 7502 _reflns_number_gt 5826 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER-AXS)' _computing_cell_refinement 'SAINT (BRUKER-AXS)' _computing_data_reduction 'SAINT (BRUKER-AXS)' _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^)+(0.0643P)^2^+0.2857P] 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 7502 _refine_ls_number_parameters 293 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.1228 _refine_ls_wR_factor_gt 0.1119 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 0.38029(3) 0.23450(3) 0.246659(18) 0.01942(8) Uani 1 1 d . . . Si1 Si 0.07717(6) 0.54074(5) 0.28017(4) 0.03127(13) Uani 1 1 d . . . C1 C 0.5445(2) 0.35849(18) 0.22097(11) 0.0267(3) Uani 1 1 d . . . C2 C 0.5246(2) 0.4951(2) 0.20518(13) 0.0331(4) Uani 1 1 d . . . C1A C 0.3253(2) 0.1114(2) 0.38261(12) 0.0341(4) Uani 1 1 d . . . C2A C 0.4611(2) 0.01584(19) 0.34766(12) 0.0322(4) Uani 1 1 d . . . C3A C 0.5823(2) 0.0797(2) 0.34795(12) 0.0316(4) Uani 1 1 d . . . C4A C 0.5235(2) 0.2118(2) 0.38837(12) 0.0325(4) Uani 1 1 d . . . C5A C 0.3674(2) 0.2281(2) 0.41103(12) 0.0329(4) Uani 1 1 d . . . C6A C 0.1704(3) 0.0833(3) 0.40171(16) 0.0523(6) Uani 1 1 d . . . H6A1 H 0.1399 0.1016 0.4641 0.079 Uiso 1 1 calc R . . H6A2 H 0.1790 -0.0155 0.3915 0.079 Uiso 1 1 calc R . . H6A3 H 0.0919 0.1457 0.3619 0.079 Uiso 1 1 calc R . . C7A C 0.4801(3) -0.1392(2) 0.33811(17) 0.0517(6) Uani 1 1 d . . . H7A1 H 0.5776 -0.1809 0.3062 0.078 Uiso 1 1 calc R . . H7A2 H 0.3930 -0.1499 0.3043 0.078 Uiso 1 1 calc R . . H7A3 H 0.4822 -0.1874 0.3976 0.078 Uiso 1 1 calc R . . C8A C 0.7503(2) 0.0092(3) 0.32677(16) 0.0468(5) Uani 1 1 d . . . H8A1 H 0.7710 -0.0936 0.3353 0.070 Uiso 1 1 calc R . . H8A2 H 0.8162 0.0410 0.3667 0.070 Uiso 1 1 calc R . . H8A3 H 0.7730 0.0344 0.2645 0.070 Uiso 1 1 calc R . . C9A C 0.6185(3) 0.3032(3) 0.41749(15) 0.0481(5) Uani 1 1 d . . . H9A1 H 0.5628 0.4029 0.4040 0.072 Uiso 1 1 calc R . . H9A2 H 0.7184 0.2799 0.3855 0.072 Uiso 1 1 calc R . . H9A3 H 0.6363 0.2864 0.4820 0.072 Uiso 1 1 calc R . . C10A C 0.2666(3) 0.3385(3) 0.46680(14) 0.0532(6) Uani 1 1 d . . . H10A H 0.1624 0.3713 0.4414 0.080 Uiso 1 1 calc R . . H10B H 0.3106 0.4183 0.4677 0.080 Uiso 1 1 calc R . . H10C H 0.2606 0.2984 0.5280 0.080 Uiso 1 1 calc R . . C1B C 0.2213(2) 0.21939(18) 0.12059(11) 0.0265(3) Uani 1 1 d . . . C2B C 0.3002(2) 0.07801(17) 0.15112(11) 0.0266(3) Uani 1 1 d . . . C3B C 0.4612(2) 0.05605(18) 0.13182(12) 0.0281(3) Uani 1 1 d . . . C4B C 0.4804(2) 0.18461(19) 0.09315(11) 0.0279(3) Uani 1 1 d . . . C5B C 0.3319(2) 0.28475(18) 0.08583(11) 0.0273(3) Uani 1 1 d . . . C6B C 0.0485(2) 0.2787(2) 0.11873(15) 0.0418(5) Uani 1 1 d . . . H6B1 H 0.0212 0.3816 0.1075 0.063 Uiso 1 1 calc R . . H6B2 H 0.0044 0.2559 0.1765 0.063 Uiso 1 1 calc R . . H6B3 H 0.0068 0.2374 0.0711 0.063 Uiso 1 1 calc R . . C7B C 0.2167(3) -0.0319(2) 0.17349(15) 0.0416(5) Uani 1 1 d . . . H7B1 H 0.1514 -0.0068 0.2269 0.062 Uiso 1 1 calc R . . H7B2 H 0.2927 -0.1244 0.1851 0.062 Uiso 1 1 calc R . . H7B3 H 0.1515 -0.0363 0.1231 0.062 Uiso 1 1 calc R . . C8B C 0.5858(3) -0.0820(2) 0.13003(15) 0.0443(5) Uani 1 1 d . . . H8B1 H 0.6210 -0.0995 0.0682 0.066 Uiso 1 1 calc R . . H8B2 H 0.5447 -0.1586 0.1545 0.066 Uiso 1 1 calc R . . H8B3 H 0.6734 -0.0781 0.1662 0.066 Uiso 1 1 calc R . . C9B C 0.6277(3) 0.2004(3) 0.04950(15) 0.0475(5) Uani 1 1 d . . . H9B1 H 0.6317 0.1753 -0.0129 0.071 Uiso 1 1 calc R . . H9B2 H 0.7171 0.1375 0.0815 0.071 Uiso 1 1 calc R . . H9B3 H 0.6303 0.2986 0.0514 0.071 Uiso 1 1 calc R . . C10B C 0.2998(3) 0.4290(2) 0.03860(14) 0.0430(5) Uani 1 1 d . . . H10D H 0.3813 0.4719 0.0527 0.064 Uiso 1 1 calc R . . H10E H 0.1990 0.4887 0.0585 0.064 Uiso 1 1 calc R . . H10F H 0.2982 0.4204 -0.0261 0.064 Uiso 1 1 calc R . . C1C C 0.0088(3) 0.6540(2) 0.17549(17) 0.0503(6) Uani 1 1 d . . . H1C1 H 0.0968 0.6784 0.1455 0.075 Uiso 1 1 calc R . . H1C2 H -0.0701 0.7407 0.1909 0.075 Uiso 1 1 calc R . . H1C3 H -0.0359 0.6019 0.1355 0.075 Uiso 1 1 calc R . . C2C C -0.0929(2) 0.4906(3) 0.33162(16) 0.0452(5) Uani 1 1 d . . . H2C1 H -0.1191 0.4219 0.2953 0.068 Uiso 1 1 calc R . . H2C2 H -0.1819 0.5751 0.3343 0.068 Uiso 1 1 calc R . . H2C3 H -0.0669 0.4484 0.3923 0.068 Uiso 1 1 calc R . . C3C C 0.1365(3) 0.6608(2) 0.35530(17) 0.0479(5) Uani 1 1 d . . . H3C1 H 0.1002 0.6459 0.4165 0.072 Uiso 1 1 calc R . . H3C2 H 0.0903 0.7595 0.3340 0.072 Uiso 1 1 calc R . . H3C3 H 0.2498 0.6397 0.3545 0.072 Uiso 1 1 calc R . . F1 F 0.70259(12) 0.28631(12) 0.21951(8) 0.0364(3) Uani 1 1 d . . . F2 F 0.63666(16) 0.55927(14) 0.18947(9) 0.0489(3) Uani 1 1 d . . . F3 F 0.38875(15) 0.59479(12) 0.20122(9) 0.0475(3) Uani 1 1 d . . . O1 O 0.21626(13) 0.39609(12) 0.26341(8) 0.0259(2) 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 0.01974(14) 0.01971(13) 0.01871(14) -0.00019(9) 0.00008(10) -0.00569(9) Si1 0.0246(2) 0.0279(2) 0.0393(3) -0.0099(2) -0.0004(2) -0.00249(18) C1 0.0257(8) 0.0310(8) 0.0252(8) -0.0005(6) 0.0005(6) -0.0115(6) C2 0.0380(10) 0.0336(9) 0.0333(10) -0.0006(7) 0.0013(8) -0.0194(8) C1A 0.0341(10) 0.0458(10) 0.0230(8) 0.0106(7) -0.0014(7) -0.0151(8) C2A 0.0401(10) 0.0297(8) 0.0266(9) 0.0082(7) -0.0072(7) -0.0114(7) C3A 0.0292(9) 0.0360(9) 0.0261(9) 0.0067(7) -0.0072(7) -0.0051(7) C4A 0.0385(10) 0.0398(10) 0.0216(8) 0.0031(7) -0.0060(7) -0.0153(8) C5A 0.0367(10) 0.0419(10) 0.0186(8) 0.0005(7) -0.0009(7) -0.0091(8) C6A 0.0493(14) 0.0781(17) 0.0383(12) 0.0058(11) 0.0070(10) -0.0349(12) C7A 0.0715(17) 0.0312(10) 0.0517(14) 0.0150(9) -0.0131(12) -0.0164(10) C8A 0.0298(10) 0.0529(13) 0.0501(13) 0.0067(10) -0.0064(9) -0.0011(9) C9A 0.0603(15) 0.0635(14) 0.0324(11) -0.0021(10) -0.0121(10) -0.0358(12) C10A 0.0561(15) 0.0672(15) 0.0269(10) -0.0119(10) 0.0009(10) -0.0004(12) C1B 0.0261(8) 0.0309(8) 0.0229(8) -0.0044(6) -0.0036(6) -0.0076(6) C2B 0.0312(9) 0.0260(8) 0.0249(8) -0.0041(6) -0.0008(7) -0.0114(6) C3B 0.0297(9) 0.0274(8) 0.0261(8) -0.0062(6) -0.0008(7) -0.0055(6) C4B 0.0293(9) 0.0371(9) 0.0200(8) -0.0063(6) 0.0041(6) -0.0132(7) C5B 0.0361(9) 0.0285(8) 0.0178(7) 0.0005(6) -0.0025(7) -0.0104(7) C6B 0.0277(10) 0.0493(12) 0.0473(12) -0.0120(9) -0.0093(9) -0.0063(8) C7B 0.0515(13) 0.0365(10) 0.0450(12) -0.0029(9) -0.0005(10) -0.0254(9) C8B 0.0429(12) 0.0352(10) 0.0470(12) -0.0121(9) -0.0018(9) 0.0034(8) C9B 0.0422(12) 0.0716(15) 0.0362(11) -0.0159(10) 0.0165(9) -0.0269(11) C10B 0.0611(14) 0.0375(10) 0.0299(10) 0.0107(8) -0.0076(9) -0.0154(9) C1C 0.0457(13) 0.0349(10) 0.0595(15) -0.0010(10) -0.0105(11) 0.0062(9) C2C 0.0264(10) 0.0583(13) 0.0509(13) -0.0201(10) 0.0063(9) -0.0092(9) C3C 0.0466(13) 0.0392(11) 0.0609(15) -0.0212(10) 0.0027(11) -0.0131(9) F1 0.0244(5) 0.0436(6) 0.0419(6) -0.0001(5) 0.0004(5) -0.0115(4) F2 0.0579(8) 0.0482(7) 0.0536(8) 0.0054(6) -0.0023(6) -0.0377(6) F3 0.0494(8) 0.0262(5) 0.0654(9) 0.0028(5) 0.0017(6) -0.0102(5) O1 0.0238(6) 0.0253(6) 0.0273(6) -0.0041(5) 0.0009(5) -0.0043(4) _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 O1 1.8639(12) . ? Ti1 C1 2.1842(17) . ? Ti1 C1A 2.4137(18) . ? Ti1 C2B 2.4406(17) . ? Ti1 C1B 2.4408(18) . ? Ti1 C5B 2.4535(18) . ? Ti1 C5A 2.4587(19) . ? Ti1 C4B 2.4728(17) . ? Ti1 C4A 2.4802(19) . ? Ti1 C3B 2.4893(17) . ? Ti1 C3A 2.4922(18) . ? Ti1 C2A 2.4939(18) . ? Si1 O1 1.6366(12) . ? Si1 C2C 1.869(2) . ? Si1 C1C 1.876(2) . ? Si1 C3C 1.881(2) . ? C1 C2 1.317(2) . ? C1 F1 1.397(2) . ? C2 F3 1.332(2) . ? C2 F2 1.344(2) . ? C1A C5A 1.408(3) . ? C1A C2A 1.423(3) . ? C1A C6A 1.512(3) . ? C2A C3A 1.408(3) . ? C2A C7A 1.508(3) . ? C3A C4A 1.429(3) . ? C3A C8A 1.506(3) . ? C4A C5A 1.400(3) . ? C4A C9A 1.501(3) . ? C5A C10A 1.490(3) . ? C6A H6A1 0.9800 . ? C6A H6A2 0.9800 . ? C6A H6A3 0.9800 . ? C7A H7A1 0.9800 . ? C7A H7A2 0.9800 . ? C7A H7A3 0.9800 . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? C9A H9A1 0.9800 . ? C9A H9A2 0.9800 . ? C9A H9A3 0.9800 . ? C10A H10A 0.9800 . ? C10A H10B 0.9800 . ? C10A H10C 0.9800 . ? C1B C5B 1.404(2) . ? C1B C2B 1.426(2) . ? C1B C6B 1.496(3) . ? C2B C3B 1.425(2) . ? C2B C7B 1.504(2) . ? C3B C4B 1.415(3) . ? C3B C8B 1.499(2) . ? C4B C5B 1.419(3) . ? C4B C9B 1.503(3) . ? C5B C10B 1.503(3) . ? C6B H6B1 0.9800 . ? C6B H6B2 0.9800 . ? C6B H6B3 0.9800 . ? C7B H7B1 0.9800 . ? C7B H7B2 0.9800 . ? C7B H7B3 0.9800 . ? C8B H8B1 0.9800 . ? C8B H8B2 0.9800 . ? C8B H8B3 0.9800 . ? C9B H9B1 0.9800 . ? C9B H9B2 0.9800 . ? C9B H9B3 0.9800 . ? C10B H10D 0.9800 . ? C10B H10E 0.9800 . ? C10B H10F 0.9800 . ? C1C H1C1 0.9800 . ? C1C H1C2 0.9800 . ? C1C H1C3 0.9800 . ? C2C H2C1 0.9800 . ? C2C H2C2 0.9800 . ? C2C H2C3 0.9800 . ? C3C H3C1 0.9800 . ? C3C H3C2 0.9800 . ? C3C H3C3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ti1 C1 92.14(6) . . ? O1 Ti1 C1A 93.98(6) . . ? C1 Ti1 C1A 130.16(7) . . ? O1 Ti1 C2B 110.11(6) . . ? C1 Ti1 C2B 130.32(6) . . ? C1A Ti1 C2B 93.13(7) . . ? O1 Ti1 C1B 81.45(6) . . ? C1 Ti1 C1B 116.18(6) . . ? C1A Ti1 C1B 113.65(7) . . ? C2B Ti1 C1B 33.96(6) . . ? O1 Ti1 C5B 86.52(6) . . ? C1 Ti1 C5B 83.17(6) . . ? C1A Ti1 C5B 146.55(6) . . ? C2B Ti1 C5B 55.91(6) . . ? C1B Ti1 C5B 33.33(6) . . ? O1 Ti1 C5A 79.79(6) . . ? C1 Ti1 C5A 100.17(7) . . ? C1A Ti1 C5A 33.57(7) . . ? C2B Ti1 C5A 126.57(6) . . ? C1B Ti1 C5A 139.45(6) . . ? C5B Ti1 C5A 165.99(6) . . ? O1 Ti1 C4B 118.78(6) . . ? C1 Ti1 C4B 74.66(6) . . ? C1A Ti1 C4B 139.86(7) . . ? C2B Ti1 C4B 55.67(6) . . ? C1B Ti1 C4B 55.43(6) . . ? C5B Ti1 C4B 33.49(6) . . ? C5A Ti1 C4B 160.49(6) . . ? O1 Ti1 C4A 101.28(6) . . ? C1 Ti1 C4A 74.72(6) . . ? C1A Ti1 C4A 55.56(7) . . ? C2B Ti1 C4A 137.22(6) . . ? C1B Ti1 C4A 168.82(6) . . ? C5B Ti1 C4A 156.72(6) . . ? C5A Ti1 C4A 32.94(6) . . ? C4B Ti1 C4A 129.70(7) . . ? O1 Ti1 C3B 136.71(6) . . ? C1 Ti1 C3B 101.64(6) . . ? C1A Ti1 C3B 106.93(7) . . ? C2B Ti1 C3B 33.58(6) . . ? C1B Ti1 C3B 55.57(6) . . ? C5B Ti1 C3B 55.36(6) . . ? C5A Ti1 C3B 135.77(6) . . ? C4B Ti1 C3B 33.14(6) . . ? C4A Ti1 C3B 121.88(6) . . ? O1 Ti1 C3A 133.30(6) . . ? C1 Ti1 C3A 85.51(7) . . ? C1A Ti1 C3A 55.66(7) . . ? C2B Ti1 C3A 106.47(6) . . ? C1B Ti1 C3A 140.28(6) . . ? C5B Ti1 C3A 138.97(6) . . ? C5A Ti1 C3A 55.03(6) . . ? C4B Ti1 C3A 105.51(6) . . ? C4A Ti1 C3A 33.41(6) . . ? C3B Ti1 C3A 88.97(6) . . ? O1 Ti1 C2A 127.62(6) . . ? C1 Ti1 C2A 118.25(7) . . ? C1A Ti1 C2A 33.67(7) . . ? C2B Ti1 C2A 82.78(6) . . ? C1B Ti1 C2A 114.96(6) . . ? C5B Ti1 C2A 135.13(6) . . ? C5A Ti1 C2A 54.93(6) . . ? C4B Ti1 C2A 110.35(6) . . ? C4A Ti1 C2A 54.81(6) . . ? C3B Ti1 C2A 80.84(6) . . ? C3A Ti1 C2A 32.81(6) . . ? O1 Si1 C2C 108.58(9) . . ? O1 Si1 C1C 113.97(9) . . ? C2C Si1 C1C 107.56(12) . . ? O1 Si1 C3C 112.84(9) . . ? C2C Si1 C3C 109.09(10) . . ? C1C Si1 C3C 104.57(12) . . ? C2 C1 F1 109.94(15) . . ? C2 C1 Ti1 132.10(14) . . ? F1 C1 Ti1 117.96(11) . . ? C1 C2 F3 125.90(17) . . ? C1 C2 F2 126.47(18) . . ? F3 C2 F2 107.62(15) . . ? C5A C1A C2A 107.59(17) . . ? C5A C1A C6A 124.88(19) . . ? C2A C1A C6A 126.7(2) . . ? C5A C1A Ti1 74.97(11) . . ? C2A C1A Ti1 76.26(10) . . ? C6A C1A Ti1 122.92(14) . . ? C3A C2A C1A 108.04(17) . . ? C3A C2A C7A 125.70(19) . . ? C1A C2A C7A 124.12(19) . . ? C3A C2A Ti1 73.53(10) . . ? C1A C2A Ti1 70.08(10) . . ? C7A C2A Ti1 135.13(14) . . ? C2A C3A C4A 107.57(17) . . ? C2A C3A C8A 125.74(19) . . ? C4A C3A C8A 125.66(19) . . ? C2A C3A Ti1 73.66(10) . . ? C4A C3A Ti1 72.83(10) . . ? C8A C3A Ti1 128.19(14) . . ? C5A C4A C3A 107.88(17) . . ? C5A C4A C9A 125.30(19) . . ? C3A C4A C9A 125.9(2) . . ? C5A C4A Ti1 72.69(10) . . ? C3A C4A Ti1 73.75(10) . . ? C9A C4A Ti1 128.07(14) . . ? C4A C5A C1A 108.70(17) . . ? C4A C5A C10A 126.5(2) . . ? C1A C5A C10A 124.3(2) . . ? C4A C5A Ti1 74.38(10) . . ? C1A C5A Ti1 71.46(10) . . ? C10A C5A Ti1 126.48(14) . . ? C1A C6A H6A1 109.5 . . ? C1A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? C1A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C2A C7A H7A1 109.5 . . ? C2A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? C2A C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C3A C8A H8A1 109.5 . . ? C3A C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? C3A C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? C4A C9A H9A1 109.5 . . ? C4A C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? C4A C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? C5A C10A H10A 109.5 . . ? C5A C10A H10B 109.5 . . ? H10A C10A H10B 109.5 . . ? C5A C10A H10C 109.5 . . ? H10A C10A H10C 109.5 . . ? H10B C10A H10C 109.5 . . ? C5B C1B C2B 108.37(15) . . ? C5B C1B C6B 127.26(17) . . ? C2B C1B C6B 124.10(17) . . ? C5B C1B Ti1 73.83(10) . . ? C2B C1B Ti1 73.01(10) . . ? C6B C1B Ti1 123.78(12) . . ? C3B C2B C1B 107.47(15) . . ? C3B C2B C7B 127.85(16) . . ? C1B C2B C7B 122.47(17) . . ? C3B C2B Ti1 75.08(9) . . ? C1B C2B Ti1 73.02(9) . . ? C7B C2B Ti1 130.72(13) . . ? C4B C3B C2B 107.77(15) . . ? C4B C3B C8B 122.93(17) . . ? C2B C3B C8B 127.78(17) . . ? C4B C3B Ti1 72.79(9) . . ? C2B C3B Ti1 71.33(9) . . ? C8B C3B Ti1 132.48(13) . . ? C3B C4B C5B 108.23(15) . . ? C3B C4B C9B 124.60(18) . . ? C5B C4B C9B 125.90(18) . . ? C3B C4B Ti1 74.07(10) . . ? C5B C4B Ti1 72.51(9) . . ? C9B C4B Ti1 129.44(13) . . ? C1B C5B C4B 108.11(15) . . ? C1B C5B C10B 126.61(18) . . ? C4B C5B C10B 124.88(17) . . ? C1B C5B Ti1 72.84(10) . . ? C4B C5B Ti1 74.00(9) . . ? C10B C5B Ti1 124.65(12) . . ? C1B C6B H6B1 109.5 . . ? C1B C6B H6B2 109.5 . . ? H6B1 C6B H6B2 109.5 . . ? C1B C6B H6B3 109.5 . . ? H6B1 C6B H6B3 109.5 . . ? H6B2 C6B H6B3 109.5 . . ? C2B C7B H7B1 109.5 . . ? C2B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? C2B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? C3B C8B H8B1 109.5 . . ? C3B C8B H8B2 109.5 . . ? H8B1 C8B H8B2 109.5 . . ? C3B C8B H8B3 109.5 . . ? H8B1 C8B H8B3 109.5 . . ? H8B2 C8B H8B3 109.5 . . ? C4B C9B H9B1 109.5 . . ? C4B C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? C4B C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? C5B C10B H10D 109.5 . . ? C5B C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? C5B C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? Si1 C1C H1C1 109.5 . . ? Si1 C1C H1C2 109.5 . . ? H1C1 C1C H1C2 109.5 . . ? Si1 C1C H1C3 109.5 . . ? H1C1 C1C H1C3 109.5 . . ? H1C2 C1C H1C3 109.5 . . ? Si1 C2C H2C1 109.5 . . ? Si1 C2C H2C2 109.5 . . ? H2C1 C2C H2C2 109.5 . . ? Si1 C2C H2C3 109.5 . . ? H2C1 C2C H2C3 109.5 . . ? H2C2 C2C H2C3 109.5 . . ? Si1 C3C H3C1 109.5 . . ? Si1 C3C H3C2 109.5 . . ? H3C1 C3C H3C2 109.5 . . ? Si1 C3C H3C3 109.5 . . ? H3C1 C3C H3C3 109.5 . . ? H3C2 C3C H3C3 109.5 . . ? Si1 O1 Ti1 177.64(8) . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 30.56 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.519 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.066