Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Manfred Bochmann' 'David L. Hughes' 'Musa Said' _publ_contact_author_name 'Prof Manfred Bochmann' _publ_contact_author_address ; School of Chemical Sciences University of East Anglia Wolfson Materials and Catalysis Cen Norwich NR4 7TJ UNITED KINGDOM ; _publ_contact_author_email M.BOCHMANN@UEA.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis and Catalytic Activity of Binuclear Titanium Imido Complexes ; data_musa13a _database_code_depnum_ccdc_archive 'CCDC 225816' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'complex 5' _chemical_melting_point ? _chemical_formula_moiety 'C56 H48 F24 N2 O2 P2 Ti2' _chemical_formula_structural [{TiMe2(thf)(NC6H4P{C6H3(CF3)2})}2] _chemical_formula_sum 'C56 H48 F24 N2 O2 P2 Ti2' _chemical_formula_weight 1394.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.572(4) _cell_length_b 9.754(10) _cell_length_c 16.736(14) _cell_angle_alpha 77.03(7) _cell_angle_beta 86.91(2) _cell_angle_gamma 87.63(1) _cell_volume 1520(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plates _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 0.431 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku R-Axis-IIc' _diffrn_measurement_method 'image-plate oscillation photos' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7860 _diffrn_reflns_av_R_equivalents 0.1436 _diffrn_reflns_av_sigmaI/netI 0.1572 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 25.43 _reflns_number_total 4957 _reflns_number_gt 2758 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'MSC R-Axis-II control software' _computing_cell_refinement 'DENZO/CELL (Otwinowski and Minor, 1985)' _computing_data_reduction 'DENZO, SCALEPACK (Otwinowski and Minor, 1985)' _computing_structure_solution 'SHELXS (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1922P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4957 _refine_ls_number_parameters 412 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1641 _refine_ls_R_factor_gt 0.1191 _refine_ls_wR_factor_ref 0.3007 _refine_ls_wR_factor_gt 0.2760 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.981 _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 Ti Ti 0.09698(13) 0.40245(13) 0.04957(8) 0.0512(4) Uani 1 1 d . . . O2 O 0.2551(5) 0.4473(5) 0.1292(3) 0.0564(12) Uani 1 1 d . . . C21 C 0.3753(8) 0.5358(9) 0.0971(5) 0.067(2) Uani 1 1 d . . . H21A H 0.3443 0.6243 0.0625 0.080 Uiso 1 1 calc R . . H21B H 0.4403 0.4881 0.0652 0.080 Uiso 1 1 calc R . . C22 C 0.4438(10) 0.5611(11) 0.1717(6) 0.083(3) Uani 1 1 d . . . H22A H 0.5266 0.5005 0.1834 0.100 Uiso 1 1 calc R . . H22B H 0.4706 0.6583 0.1630 0.100 Uiso 1 1 calc R . . C23 C 0.3347(9) 0.5267(10) 0.2412(6) 0.075(2) Uani 1 1 d . . . H23A H 0.2731 0.6074 0.2433 0.090 Uiso 1 1 calc R . . H23B H 0.3777 0.4951 0.2936 0.090 Uiso 1 1 calc R . . C24 C 0.2565(8) 0.4094(9) 0.2192(5) 0.066(2) Uani 1 1 d . . . H24A H 0.3044 0.3192 0.2379 0.079 Uiso 1 1 calc R . . H24B H 0.1620 0.4048 0.2435 0.079 Uiso 1 1 calc R . . C3 C 0.2680(7) 0.3335(9) -0.0216(5) 0.0637(19) Uani 1 1 d . . . H3A H 0.2454 0.2465 -0.0350 0.096 Uiso 1 1 calc R . . H3B H 0.3507 0.3195 0.0095 0.096 Uiso 1 1 calc R . . H3C H 0.2843 0.4035 -0.0713 0.096 Uiso 1 1 calc R . . C4 C 0.0142(8) 0.2522(8) 0.1516(5) 0.0615(18) Uani 1 1 d . . . H4A H -0.0356 0.3001 0.1891 0.092 Uiso 1 1 calc R . . H4B H 0.0894 0.1955 0.1789 0.092 Uiso 1 1 calc R . . H4C H -0.0485 0.1931 0.1328 0.092 Uiso 1 1 calc R . . N1 N 0.0345(5) 0.6016(6) 0.0325(4) 0.0511(13) Uani 1 1 d . . . C11 C 0.0396(7) 0.6912(7) 0.0863(4) 0.0496(15) Uani 1 1 d . . . C12 C -0.0244(6) 0.6551(7) 0.1666(4) 0.0472(15) Uani 1 1 d . . . H12 H -0.0728 0.5720 0.1827 0.057 Uiso 1 1 calc R . . C13 C -0.0157(6) 0.7430(7) 0.2220(4) 0.0488(15) Uani 1 1 d . . . C14 C 0.0549(7) 0.8714(7) 0.1963(5) 0.0531(17) Uani 1 1 d . . . H14 H 0.0610 0.9309 0.2322 0.064 Uiso 1 1 calc R . . C15 C 0.1145(7) 0.9083(7) 0.1177(5) 0.0610(19) Uani 1 1 d . . . H15 H 0.1595 0.9934 0.1010 0.073 Uiso 1 1 calc R . . C16 C 0.1083(7) 0.8207(7) 0.0634(4) 0.0554(17) Uani 1 1 d . . . H16 H 0.1501 0.8476 0.0111 0.067 Uiso 1 1 calc R . . P P -0.10121(18) 0.70624(19) 0.32474(12) 0.0503(5) Uani 1 1 d . . . C51 C -0.2819(7) 0.7634(7) 0.3023(4) 0.0507(16) Uani 1 1 d . . . C52 C -0.3180(7) 0.8568(7) 0.2290(5) 0.0535(17) Uani 1 1 d . . . H52 H -0.2498 0.8817 0.1871 0.064 Uiso 1 1 calc R . . C53 C -0.4541(7) 0.9135(8) 0.2175(5) 0.0546(17) Uani 1 1 d . . . C54 C -0.5579(7) 0.8756(8) 0.2789(5) 0.0535(16) Uani 1 1 d . . . H54 H -0.6485 0.9129 0.2716 0.064 Uiso 1 1 calc R . . C55 C -0.5247(7) 0.7806(8) 0.3521(5) 0.0537(17) Uani 1 1 d . . . C56 C -0.3884(7) 0.7265(7) 0.3643(4) 0.0540(17) Uani 1 1 d . . . H56 H -0.3674 0.6658 0.4138 0.065 Uiso 1 1 calc R . . C530 C -0.4905(8) 1.0141(10) 0.1398(5) 0.068(2) Uani 1 1 d . . . F531 F -0.5437(5) 0.9455(6) 0.0877(3) 0.0855(14) Uani 1 1 d . . . F532 F -0.5874(5) 1.1113(6) 0.1507(3) 0.0860(15) Uani 1 1 d . . . F533 F -0.3790(5) 1.0813(6) 0.0999(3) 0.0874(15) Uani 1 1 d . . . C550 C -0.6345(8) 0.7391(9) 0.4210(5) 0.065(2) Uani 1 1 d . . . F551 F -0.6413(8) 0.8298(9) 0.4702(4) 0.107(3) Uani 0.879(14) 1 d P . . F552 F -0.6167(9) 0.6145(8) 0.4652(6) 0.133(5) Uani 0.879(14) 1 d P . . F553 F -0.7645(6) 0.7495(13) 0.3935(4) 0.113(3) Uani 0.879(14) 1 d P . . F554 F -0.589(3) 0.720(5) 0.496(2) 0.057(12) Uiso 0.121(14) 1 d P . . F555 F -0.694(5) 0.626(6) 0.420(3) 0.073(14) Uiso 0.121(14) 1 d P . . F556 F -0.750(4) 0.824(5) 0.421(3) 0.065(13) Uiso 0.121(14) 1 d P . . C61 C -0.1113(7) 0.5106(7) 0.3480(4) 0.0497(16) Uani 1 1 d . . . C62 C -0.2223(7) 0.4353(7) 0.3307(4) 0.0523(16) Uani 1 1 d . . . H62 H -0.3014 0.4833 0.3075 0.063 Uiso 1 1 calc R . . C63 C -0.2157(7) 0.2878(7) 0.3481(4) 0.0530(16) Uani 1 1 d . . . C64 C -0.0980(7) 0.2138(8) 0.3820(4) 0.0552(17) Uani 1 1 d . . . H64 H -0.0934 0.1160 0.3927 0.066 Uiso 1 1 calc R . . C65 C 0.0138(7) 0.2890(8) 0.3998(5) 0.0567(17) Uani 1 1 d . . . C66 C 0.0058(7) 0.4369(7) 0.3841(4) 0.0519(16) Uani 1 1 d . . . H66 H 0.0790 0.4859 0.3977 0.062 Uiso 1 1 calc R . . C630 C -0.3366(8) 0.2104(8) 0.3284(5) 0.0634(19) Uani 1 1 d . . . F631 F -0.4605(5) 0.2609(5) 0.3521(3) 0.0826(14) Uani 1 1 d . . . F632 F -0.3322(5) 0.0726(5) 0.3637(4) 0.0873(15) Uani 1 1 d . . . F633 F -0.3419(6) 0.2193(6) 0.2487(3) 0.0942(17) Uani 1 1 d . . . C650 C 0.1417(8) 0.2076(9) 0.4338(5) 0.070(2) Uani 1 1 d . . . F651 F 0.1161(5) 0.1152(5) 0.5039(3) 0.0852(14) Uani 1 1 d . . . F652 F 0.2021(6) 0.1338(7) 0.3831(4) 0.1062(19) Uani 1 1 d . . . F653 F 0.2409(5) 0.2903(6) 0.4481(4) 0.1005(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti 0.0622(8) 0.0388(7) 0.0520(8) -0.0098(5) 0.0036(5) -0.0024(5) O2 0.061(3) 0.057(3) 0.051(3) -0.010(2) 0.003(2) -0.006(2) C21 0.066(4) 0.062(5) 0.074(6) -0.017(4) 0.007(4) -0.013(4) C22 0.092(6) 0.088(7) 0.076(6) -0.028(5) 0.005(5) -0.029(5) C23 0.083(5) 0.077(6) 0.077(6) -0.038(5) -0.013(4) -0.004(4) C24 0.084(5) 0.066(5) 0.047(4) -0.014(4) -0.006(4) -0.005(4) C3 0.066(4) 0.071(5) 0.057(5) -0.024(4) 0.003(3) 0.006(4) C4 0.082(5) 0.041(4) 0.061(5) -0.012(3) 0.000(3) 0.001(3) N1 0.052(3) 0.048(3) 0.057(4) -0.021(3) 0.006(2) -0.007(2) C11 0.059(4) 0.034(3) 0.057(4) -0.012(3) 0.001(3) -0.007(3) C12 0.050(4) 0.034(3) 0.057(4) -0.008(3) 0.001(3) -0.006(3) C13 0.051(4) 0.038(3) 0.059(4) -0.015(3) 0.001(3) -0.009(3) C14 0.056(4) 0.039(4) 0.069(5) -0.020(3) 0.002(3) -0.010(3) C15 0.070(4) 0.036(4) 0.077(6) -0.015(3) 0.013(4) -0.015(3) C16 0.071(4) 0.043(4) 0.050(4) -0.008(3) 0.011(3) -0.012(3) P 0.0557(10) 0.0422(10) 0.0562(11) -0.0167(8) -0.0018(7) -0.0072(7) C51 0.062(4) 0.043(4) 0.049(4) -0.016(3) 0.006(3) -0.015(3) C52 0.063(4) 0.044(4) 0.057(4) -0.019(3) 0.001(3) -0.009(3) C53 0.051(4) 0.051(4) 0.064(5) -0.019(3) -0.004(3) 0.001(3) C54 0.052(4) 0.049(4) 0.061(5) -0.015(3) -0.001(3) -0.003(3) C55 0.054(4) 0.049(4) 0.061(5) -0.020(3) 0.008(3) -0.011(3) C56 0.062(4) 0.046(4) 0.055(4) -0.012(3) -0.002(3) -0.010(3) C530 0.058(4) 0.075(6) 0.073(6) -0.020(4) -0.003(4) 0.001(4) F531 0.103(3) 0.095(4) 0.062(3) -0.021(3) -0.015(2) -0.010(3) F532 0.092(3) 0.077(3) 0.081(4) -0.006(3) -0.005(2) 0.023(3) F533 0.072(3) 0.086(4) 0.086(4) 0.020(3) -0.003(2) -0.011(2) C550 0.063(5) 0.067(5) 0.063(5) -0.011(4) 0.004(3) -0.011(4) F551 0.125(6) 0.118(7) 0.091(5) -0.055(5) 0.048(4) -0.039(5) F552 0.122(7) 0.081(5) 0.151(8) 0.048(5) 0.074(6) 0.029(4) F553 0.065(4) 0.186(10) 0.084(5) -0.015(5) 0.006(3) -0.032(5) C61 0.055(4) 0.049(4) 0.047(4) -0.015(3) 0.005(3) -0.010(3) C62 0.061(4) 0.051(4) 0.048(4) -0.016(3) -0.007(3) -0.001(3) C63 0.064(4) 0.048(4) 0.050(4) -0.015(3) -0.001(3) -0.007(3) C64 0.069(4) 0.043(4) 0.051(4) -0.007(3) 0.004(3) -0.004(3) C65 0.063(4) 0.047(4) 0.055(4) -0.002(3) -0.006(3) -0.002(3) C66 0.061(4) 0.044(4) 0.053(4) -0.014(3) -0.004(3) -0.006(3) C630 0.072(5) 0.045(4) 0.075(6) -0.015(4) -0.007(4) -0.006(3) F631 0.066(3) 0.072(3) 0.115(4) -0.030(3) -0.005(2) -0.016(2) F632 0.099(3) 0.047(3) 0.117(4) -0.014(3) -0.024(3) -0.016(2) F633 0.117(4) 0.106(4) 0.070(4) -0.033(3) -0.013(3) -0.041(3) C650 0.072(5) 0.062(5) 0.072(6) -0.005(4) -0.011(4) -0.001(4) F651 0.096(3) 0.070(3) 0.076(3) 0.015(3) -0.014(2) -0.004(2) F652 0.115(4) 0.115(5) 0.090(4) -0.030(4) -0.013(3) 0.048(3) F653 0.079(3) 0.065(3) 0.151(6) 0.001(3) -0.039(3) -0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti N1 1.921(6) 2_565 ? Ti N1 1.971(6) . ? Ti C4 2.125(8) . ? Ti C3 2.147(7) . ? Ti O2 2.188(5) . ? Ti Ti 2.906(3) 2_565 ? O2 C24 1.470(9) . ? O2 C21 1.472(8) . ? C21 C22 1.513(12) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.510(12) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.514(11) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? N1 C11 1.391(8) . ? N1 Ti 1.921(6) 2_565 ? C11 C16 1.414(9) . ? C11 C12 1.422(9) . ? C12 C13 1.405(9) . ? C12 H12 0.9300 . ? C13 C14 1.417(9) . ? C13 P 1.830(7) . ? C14 C15 1.381(10) . ? C14 H14 0.9300 . ? C15 C16 1.384(10) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? P C51 1.828(7) . ? P C61 1.866(7) . ? C51 C52 1.404(10) . ? C51 C56 1.412(9) . ? C52 C53 1.400(10) . ? C52 H52 0.9300 . ? C53 C54 1.389(10) . ? C53 C530 1.491(12) . ? C54 C55 1.402(11) . ? C54 H54 0.9300 . ? C55 C56 1.395(10) . ? C55 C550 1.514(10) . ? C56 H56 0.9300 . ? C530 F532 1.334(9) . ? C530 F533 1.341(9) . ? C530 F531 1.344(9) . ? C550 F555 1.27(4) . ? C550 F552 1.284(11) . ? C550 F554 1.32(4) . ? C550 F551 1.334(10) . ? C550 F553 1.342(10) . ? C550 F556 1.35(4) . ? F551 F554 1.16(4) . ? F551 F556 1.37(5) . ? F552 F555 1.07(5) . ? F552 F554 1.29(4) . ? F553 F556 0.97(4) . ? F553 F555 1.36(5) . ? C61 C62 1.394(9) . ? C61 C66 1.396(10) . ? C62 C63 1.402(10) . ? C62 H62 0.9300 . ? C63 C64 1.389(10) . ? C63 C630 1.497(10) . ? C64 C65 1.403(10) . ? C64 H64 0.9300 . ? C65 C66 1.407(10) . ? C65 C650 1.499(11) . ? C66 H66 0.9300 . ? C630 F633 1.321(10) . ? C630 F631 1.339(9) . ? C630 F632 1.341(9) . ? C650 F651 1.327(10) . ? C650 F652 1.328(10) . ? C650 F653 1.335(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 N1 Ti N1 83.4(2) 2_565 . ? N1 Ti C4 101.8(3) 2_565 . ? N1 Ti C4 120.0(3) . . ? N1 Ti C3 92.6(3) 2_565 . ? N1 Ti C3 122.3(3) . . ? C4 Ti C3 117.2(3) . . ? N1 Ti O2 169.1(2) 2_565 . ? N1 Ti O2 87.8(2) . . ? C4 Ti O2 88.3(3) . . ? C3 Ti O2 86.5(2) . . ? N1 Ti Ti 42.37(17) 2_565 2_565 ? N1 Ti Ti 41.05(17) . 2_565 ? C4 Ti Ti 118.3(2) . 2_565 ? C3 Ti Ti 113.1(2) . 2_565 ? O2 Ti Ti 128.56(15) . 2_565 ? C24 O2 C21 108.9(5) . . ? C24 O2 Ti 128.6(4) . . ? C21 O2 Ti 122.3(4) . . ? O2 C21 C22 105.7(7) . . ? O2 C21 H21A 110.6 . . ? C22 C21 H21A 110.6 . . ? O2 C21 H21B 110.6 . . ? C22 C21 H21B 110.6 . . ? H21A C21 H21B 108.7 . . ? C23 C22 C21 105.4(7) . . ? C23 C22 H22A 110.7 . . ? C21 C22 H22A 110.7 . . ? C23 C22 H22B 110.7 . . ? C21 C22 H22B 110.7 . . ? H22A C22 H22B 108.8 . . ? C22 C23 C24 102.6(7) . . ? C22 C23 H23A 111.2 . . ? C24 C23 H23A 111.2 . . ? C22 C23 H23B 111.2 . . ? C24 C23 H23B 111.2 . . ? H23A C23 H23B 109.2 . . ? O2 C24 C23 104.3(7) . . ? O2 C24 H24A 110.9 . . ? C23 C24 H24A 110.9 . . ? O2 C24 H24B 110.9 . . ? C23 C24 H24B 110.9 . . ? H24A C24 H24B 108.9 . . ? Ti C3 H3A 109.5 . . ? Ti C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Ti C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Ti C4 H4A 109.5 . . ? Ti C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Ti C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C11 N1 Ti 130.0(4) . 2_565 ? C11 N1 Ti 128.3(5) . . ? Ti N1 Ti 96.6(2) 2_565 . ? N1 C11 C16 121.5(6) . . ? N1 C11 C12 120.9(6) . . ? C16 C11 C12 117.6(6) . . ? C13 C12 C11 121.1(6) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C12 C13 C14 119.1(6) . . ? C12 C13 P 123.3(5) . . ? C14 C13 P 117.5(5) . . ? C15 C14 C13 120.0(6) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 121.1(6) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C15 C16 C11 121.1(6) . . ? C15 C16 H16 119.4 . . ? C11 C16 H16 119.4 . . ? C51 P C13 101.7(3) . . ? C51 P C61 102.4(3) . . ? C13 P C61 101.9(3) . . ? C52 C51 C56 117.7(6) . . ? C52 C51 P 122.6(5) . . ? C56 C51 P 119.2(6) . . ? C53 C52 C51 121.7(7) . . ? C53 C52 H52 119.2 . . ? C51 C52 H52 119.2 . . ? C54 C53 C52 119.9(7) . . ? C54 C53 C530 119.0(6) . . ? C52 C53 C530 121.1(7) . . ? C53 C54 C55 119.4(6) . . ? C53 C54 H54 120.3 . . ? C55 C54 H54 120.3 . . ? C56 C55 C54 120.7(6) . . ? C56 C55 C550 118.4(7) . . ? C54 C55 C550 120.8(7) . . ? C55 C56 C51 120.6(7) . . ? C55 C56 H56 119.7 . . ? C51 C56 H56 119.7 . . ? F532 C530 F533 107.7(7) . . ? F532 C530 F531 105.9(6) . . ? F533 C530 F531 106.3(7) . . ? F532 C530 C53 113.3(7) . . ? F533 C530 C53 112.7(6) . . ? F531 C530 C53 110.5(7) . . ? F555 C550 F552 49(2) . . ? F555 C550 F554 105(3) . . ? F552 C550 F554 59.6(19) . . ? F555 C550 F551 135(2) . . ? F552 C550 F551 108.4(9) . . ? F554 C550 F551 51.9(19) . . ? F555 C550 F553 63(2) . . ? F552 C550 F553 107.7(8) . . ? F554 C550 F553 131.4(17) . . ? F551 C550 F553 102.3(8) . . ? F555 C550 F556 99(3) . . ? F552 C550 F556 126.8(19) . . ? F554 C550 F556 104(3) . . ? F551 C550 F556 61(2) . . ? F553 C550 F556 42.0(19) . . ? F555 C550 C55 114(2) . . ? F552 C550 C55 114.4(7) . . ? F554 C550 C55 115.5(16) . . ? F551 C550 C55 111.1(7) . . ? F553 C550 C55 112.2(7) . . ? F556 C550 C55 117.8(19) . . ? F554 F551 C550 63.3(19) . . ? F554 F551 F556 113(3) . . ? C550 F551 F556 60.1(18) . . ? F555 F552 C550 65(3) . . ? F555 F552 F554 120(3) . . ? C550 F552 F554 61.5(18) . . ? F556 F553 C550 70(2) . . ? F556 F553 F555 117(3) . . ? C550 F553 F555 56.1(18) . . ? F551 F554 F552 120(3) . . ? F551 F554 C550 65(2) . . ? F552 F554 C550 58.9(17) . . ? F552 F555 C550 66(2) . . ? F552 F555 F553 122(4) . . ? C550 F555 F553 61(2) . . ? F553 F556 C550 68(2) . . ? F553 F556 F551 126(4) . . ? C550 F556 F551 58.7(18) . . ? C62 C61 C66 119.0(6) . . ? C62 C61 P 125.7(5) . . ? C66 C61 P 115.2(5) . . ? C61 C62 C63 120.6(6) . . ? C61 C62 H62 119.7 . . ? C63 C62 H62 119.7 . . ? C64 C63 C62 120.7(6) . . ? C64 C63 C630 120.2(6) . . ? C62 C63 C630 119.1(6) . . ? C63 C64 C65 118.9(7) . . ? C63 C64 H64 120.5 . . ? C65 C64 H64 120.5 . . ? C64 C65 C66 120.3(6) . . ? C64 C65 C650 118.2(7) . . ? C66 C65 C650 121.5(7) . . ? C61 C66 C65 120.3(6) . . ? C61 C66 H66 119.8 . . ? C65 C66 H66 119.8 . . ? F633 C630 F631 106.0(6) . . ? F633 C630 F632 106.1(6) . . ? F631 C630 F632 106.3(7) . . ? F633 C630 C63 111.8(7) . . ? F631 C630 C63 112.8(6) . . ? F632 C630 C63 113.4(6) . . ? F651 C650 F652 105.5(7) . . ? F651 C650 F653 106.5(7) . . ? F652 C650 F653 105.4(7) . . ? F651 C650 C65 113.4(7) . . ? F652 C650 C65 112.5(7) . . ? F653 C650 C65 112.7(7) . . ? _diffrn_measured_fraction_theta_max 0.881 _diffrn_reflns_theta_full 25.43 _diffrn_measured_fraction_theta_full 0.881 _refine_diff_density_max 1.093 _refine_diff_density_min -0.751 _refine_diff_density_rms 0.144