# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1626 data_global #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name 'Mark Thornton-Pett' _publ_contact_author_address ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; _publ_contact_author_phone '+44 (0)113 2336423' _publ_contact_author_fax '+44 (0)113 2336565' _publ_contact_author_email marktp@chem.leeds.ac.uk _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_contact_letter ; The following set of data is for the a compound included in the paper below which we have just submitted to you as a communication. ; #======================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; Facile formation of a titanium-carbon bond from TiCl4 by HCl elimination: The synthesis and structure of TiCl3[Me3SiNP(Ph)2CHCH2P(Ph)2NSiMe3] ; loop_ _publ_author_name _publ_author_address 'Mark J. Sarsfield' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Mark Thornton-Pett' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Manfred Bochmann' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; #================================================================= data_mb62 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H45 Cl7 N2 P2 Si2 Ti' _chemical_formula_weight 895.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 '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' '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 Monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 22.4593(7) _cell_length_b 9.4978(3) _cell_length_c 21.4978(6) _cell_angle_alpha 90.00 _cell_angle_beta 113.0940(14) _cell_angle_gamma 90.00 _cell_volume 4218.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 76650 _cell_measurement_theta_min 1.88 _cell_measurement_theta_max 32.33 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 0.806 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6433 _exptl_absorpt_correction_T_max 0.7939 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean '9.091 pixels/mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33497 _diffrn_reflns_av_R_equivalents 0.0608 _diffrn_reflns_av_sigmaI/netI 0.0404 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8233 _reflns_number_gt 7749 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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^)+(0.0482P)^2^+13.0030P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.42(4) _refine_ls_number_reflns 8233 _refine_ls_number_parameters 444 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1201 _refine_ls_wR_factor_gt 0.1176 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 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 0.29417(5) 0.10374(6) 0.40801(5) 0.02554(13) Uani 1 1 d . . . Cl1 Cl 0.34689(5) 0.12622(15) 0.33222(6) 0.0431(3) Uani 1 1 d . . . Cl2 Cl 0.29088(8) 0.35103(9) 0.41113(9) 0.0450(2) Uani 1 1 d . . . Cl3 Cl 0.23880(5) 0.09164(16) 0.48118(6) 0.0449(3) Uani 1 1 d . . . N1 N 0.37965(19) 0.0580(4) 0.4900(2) 0.0327(8) Uani 1 1 d . . . Si1 Si 0.43829(6) 0.17680(14) 0.54351(7) 0.0354(3) Uani 1 1 d . . . C11 C 0.4005(3) 0.2942(5) 0.5879(3) 0.0460(13) Uani 1 1 d . . . H11A H 0.3564 0.3184 0.5570 0.069 Uiso 1 1 calc R . . H11B H 0.4262 0.3804 0.6026 0.069 Uiso 1 1 calc R . . H11C H 0.3992 0.2451 0.6275 0.069 Uiso 1 1 calc R . . C12 C 0.4709(3) 0.2830(6) 0.4903(3) 0.0486(14) Uani 1 1 d . . . H12A H 0.4788 0.2211 0.4579 0.073 Uiso 1 1 calc R . . H12B H 0.5116 0.3280 0.5195 0.073 Uiso 1 1 calc R . . H12C H 0.4394 0.3555 0.4658 0.073 Uiso 1 1 calc R . . C13 C 0.5049(3) 0.0749(6) 0.6086(3) 0.0459(12) Uani 1 1 d . . . H13A H 0.4871 0.0177 0.6352 0.069 Uiso 1 1 calc R . . H13B H 0.5372 0.1403 0.6386 0.069 Uiso 1 1 calc R . . H13C H 0.5254 0.0133 0.5862 0.069 Uiso 1 1 calc R . . P1 P 0.38086(5) -0.11083(12) 0.49182(5) 0.0271(2) Uani 1 1 d . . . C111 C 0.4576(2) -0.1777(4) 0.4959(2) 0.0257(8) Uani 1 1 d . . . C112 C 0.4793(2) -0.1231(5) 0.4479(2) 0.0328(10) Uani 1 1 d . . . H112 H 0.4535 -0.0566 0.4155 0.039 Uiso 1 1 calc R . . C113 C 0.5381(2) -0.1656(6) 0.4475(3) 0.0376(11) Uani 1 1 d . . . H113 H 0.5533 -0.1269 0.4157 0.045 Uiso 1 1 calc R . . C114 C 0.5747(3) -0.2658(6) 0.4941(3) 0.0453(12) Uani 1 1 d . . . H114 H 0.6153 -0.2946 0.4943 0.054 Uiso 1 1 calc R . . C115 C 0.5526(3) -0.3240(6) 0.5404(3) 0.0501(13) Uani 1 1 d . . . H115 H 0.5773 -0.3947 0.5709 0.060 Uiso 1 1 calc R . . C116 C 0.4945(2) -0.2789(5) 0.5422(3) 0.0402(12) Uani 1 1 d . . . H116 H 0.4799 -0.3166 0.5746 0.048 Uiso 1 1 calc R . . C121 C 0.36427(19) -0.1851(5) 0.5620(2) 0.0269(8) Uani 1 1 d . . . C122 C 0.3583(2) -0.0931(5) 0.6108(2) 0.0303(10) Uani 1 1 d . . . H122 H 0.3619 0.0057 0.6063 0.036 Uiso 1 1 calc R . . C123 C 0.3470(2) -0.1470(5) 0.6658(2) 0.0320(9) Uani 1 1 d . . . H123 H 0.3448 -0.0850 0.6995 0.038 Uiso 1 1 calc R . . C124 C 0.3391(2) -0.2912(5) 0.6712(3) 0.0363(10) Uani 1 1 d . . . H124 H 0.3312 -0.3283 0.7083 0.044 Uiso 1 1 calc R . . C125 C 0.3430(3) -0.3799(5) 0.6216(3) 0.0443(13) Uani 1 1 d . . . H125 H 0.3375 -0.4784 0.6249 0.053 Uiso 1 1 calc R . . C126 C 0.3549(2) -0.3267(5) 0.5662(3) 0.0371(10) Uani 1 1 d . . . H126 H 0.3565 -0.3885 0.5321 0.045 Uiso 1 1 calc R . . C1 C 0.31790(18) -0.1296(5) 0.41048(19) 0.0328(9) Uani 1 1 d . . . H1 H 0.338(2) -0.145(4) 0.375(2) 0.026(10) Uiso 1 1 d . . . C2 C 0.2584(2) -0.2164(5) 0.3965(2) 0.0352(9) Uani 1 1 d . . . H2A H 0.2441 -0.2126 0.4346 0.042 Uiso 1 1 calc R . . H2B H 0.2653 -0.3157 0.3870 0.042 Uiso 1 1 calc R . . P2 P 0.20047(5) -0.12812(12) 0.32102(5) 0.0262(2) Uani 1 1 d . . . C211 C 0.2160(2) -0.1948(5) 0.2495(2) 0.0282(9) Uani 1 1 d . . . C212 C 0.2249(2) -0.1013(4) 0.2036(2) 0.0280(9) Uani 1 1 d . . . H212 H 0.2236 -0.0028 0.2105 0.034 Uiso 1 1 calc R . . C213 C 0.2358(2) -0.1508(5) 0.1472(2) 0.0328(9) Uani 1 1 d . . . H213 H 0.2417 -0.0858 0.1165 0.039 Uiso 1 1 calc R . . C214 C 0.2377(2) -0.2922(5) 0.1366(3) 0.0357(10) Uani 1 1 d . . . H214 H 0.2439 -0.3256 0.0979 0.043 Uiso 1 1 calc R . . C215 C 0.2308(3) -0.3883(5) 0.1827(3) 0.0438(13) Uani 1 1 d . . . H215 H 0.2342 -0.4865 0.1765 0.053 Uiso 1 1 calc R . . C216 C 0.2188(3) -0.3394(5) 0.2375(3) 0.0417(11) Uani 1 1 d . . . H216 H 0.2123 -0.4052 0.2676 0.050 Uiso 1 1 calc R . . C221 C 0.1218(2) -0.1880(5) 0.3146(2) 0.0284(9) Uani 1 1 d . . . C222 C 0.1010(2) -0.1267(5) 0.3627(2) 0.0318(10) Uani 1 1 d . . . H222 H 0.1276 -0.0600 0.3945 0.038 Uiso 1 1 calc R . . C223 C 0.0410(2) -0.1654(6) 0.3629(3) 0.0414(12) Uani 1 1 d . . . H223 H 0.0267 -0.1261 0.3954 0.050 Uiso 1 1 calc R . . C224 C 0.0026(3) -0.2609(7) 0.3159(3) 0.0488(13) Uani 1 1 d . . . H224 H -0.0381 -0.2877 0.3163 0.059 Uiso 1 1 calc R . . C225 C 0.0230(3) -0.3182(7) 0.2681(3) 0.0537(15) Uani 1 1 d . . . H225 H -0.0042 -0.3824 0.2354 0.064 Uiso 1 1 calc R . . C226 C 0.0827(3) -0.2830(5) 0.2673(3) 0.0411(12) Uani 1 1 d . . . H226 H 0.0965 -0.3233 0.2347 0.049 Uiso 1 1 calc R . . N2 N 0.20816(19) 0.0407(4) 0.3277(2) 0.0348(9) Uani 1 1 d . . . Si2 Si 0.15007(6) 0.15984(14) 0.27540(7) 0.0352(3) Uani 1 1 d . . . C21 C 0.1870(3) 0.2828(5) 0.2324(3) 0.0460(12) Uani 1 1 d . . . H21A H 0.2221 0.3359 0.2665 0.069 Uiso 1 1 calc R . . H21B H 0.1539 0.3483 0.2037 0.069 Uiso 1 1 calc R . . H21C H 0.2043 0.2285 0.2045 0.069 Uiso 1 1 calc R . . C22 C 0.1152(3) 0.2616(7) 0.3272(3) 0.0489(13) Uani 1 1 d . . . H22A H 0.0930 0.1971 0.3465 0.073 Uiso 1 1 calc R . . H22B H 0.0842 0.3308 0.2985 0.073 Uiso 1 1 calc R . . H22C H 0.1500 0.3103 0.3637 0.073 Uiso 1 1 calc R . . C23 C 0.0813(3) 0.0664(6) 0.2057(3) 0.0427(12) Uani 1 1 d . . . H23A H 0.0983 -0.0157 0.1904 0.064 Uiso 1 1 calc R . . H23B H 0.0610 0.1310 0.1677 0.064 Uiso 1 1 calc R . . H23C H 0.0491 0.0355 0.2231 0.064 Uiso 1 1 calc R . . C1S C 0.4335(4) 0.6273(7) 0.2944(5) 0.073(2) Uani 1 1 d . . . H1SA H 0.4297 0.5733 0.2536 0.088 Uiso 1 1 calc R . . H1SB H 0.4797 0.6281 0.3256 0.088 Uiso 1 1 calc R . . Cl1S Cl 0.40747(10) 0.80252(19) 0.27072(9) 0.0690(5) Uani 1 1 d . . . Cl2S Cl 0.38834(9) 0.54275(19) 0.33402(9) 0.0673(4) Uani 1 1 d . . . C2S C 0.1403(4) 0.3739(7) 0.0154(5) 0.0668(18) Uani 1 1 d . . . H2SA H 0.1397 0.4291 0.0543 0.080 Uiso 1 1 calc R . . H2SB H 0.0951 0.3666 -0.0182 0.080 Uiso 1 1 calc R . . Cl3S Cl 0.18690(7) 0.46524(17) -0.02150(8) 0.0592(4) Uani 1 1 d . . . Cl4S Cl 0.16930(9) 0.20552(19) 0.04320(8) 0.0670(4) 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 0.0365(3) 0.0222(3) 0.0204(2) -0.0008(3) 0.0138(2) -0.0001(3) Cl1 0.0329(6) 0.0759(8) 0.0235(6) 0.0008(5) 0.0143(5) 0.0107(5) Cl2 0.0472(5) 0.0247(4) 0.0664(6) -0.0010(6) 0.0257(5) 0.0004(6) Cl3 0.0312(5) 0.0835(9) 0.0223(6) 0.0001(5) 0.0128(4) -0.0126(5) N1 0.0349(18) 0.045(2) 0.0202(18) 0.0054(16) 0.0126(15) 0.0148(17) Si1 0.0387(7) 0.0377(7) 0.0335(7) 0.0061(5) 0.0182(5) 0.0065(5) C11 0.060(3) 0.036(2) 0.054(3) -0.005(2) 0.034(3) 0.001(2) C12 0.048(3) 0.052(3) 0.055(4) 0.013(2) 0.029(3) 0.002(2) C13 0.046(3) 0.043(3) 0.038(3) 0.000(2) 0.006(2) 0.002(2) P1 0.0213(5) 0.0417(6) 0.0188(5) -0.0032(4) 0.0085(4) -0.0020(4) C111 0.0204(18) 0.033(2) 0.024(2) -0.0038(16) 0.0082(16) 0.0006(16) C112 0.026(2) 0.047(3) 0.024(2) -0.0010(18) 0.0092(19) 0.0011(18) C113 0.028(2) 0.054(3) 0.036(3) 0.002(2) 0.017(2) 0.000(2) C114 0.031(2) 0.063(3) 0.048(3) -0.003(2) 0.022(2) 0.010(2) C115 0.039(3) 0.061(3) 0.055(3) 0.012(3) 0.023(3) 0.012(2) C116 0.034(3) 0.042(3) 0.047(3) 0.007(2) 0.019(2) 0.002(2) C121 0.0219(19) 0.039(2) 0.021(2) -0.0005(17) 0.0098(16) -0.0025(16) C122 0.030(2) 0.038(2) 0.024(2) -0.0006(17) 0.0114(19) -0.0003(18) C123 0.035(2) 0.039(2) 0.025(2) -0.0015(19) 0.0147(19) 0.0037(19) C124 0.029(2) 0.047(3) 0.035(3) 0.009(2) 0.0160(19) 0.0029(19) C125 0.051(3) 0.033(3) 0.064(4) 0.000(2) 0.038(3) -0.005(2) C126 0.039(2) 0.040(3) 0.042(3) -0.008(2) 0.026(2) -0.0052(19) C1 0.0234(17) 0.053(3) 0.0205(18) -0.0036(17) 0.0075(15) -0.0033(17) C2 0.032(2) 0.051(3) 0.0235(19) 0.0041(18) 0.0117(16) 0.0003(18) P2 0.0209(5) 0.0384(6) 0.0197(5) 0.0027(4) 0.0086(4) 0.0006(4) C211 0.024(2) 0.034(2) 0.028(2) 0.0015(17) 0.0108(17) 0.0010(16) C212 0.033(2) 0.024(2) 0.027(2) -0.0036(15) 0.0118(19) -0.0037(16) C213 0.037(2) 0.040(2) 0.022(2) -0.0013(19) 0.0129(19) -0.001(2) C214 0.038(2) 0.045(3) 0.029(2) -0.0064(19) 0.0183(19) 0.001(2) C215 0.052(3) 0.036(3) 0.055(3) -0.002(2) 0.034(3) 0.004(2) C216 0.049(3) 0.035(2) 0.051(3) 0.014(2) 0.030(2) 0.009(2) C221 0.022(2) 0.035(2) 0.029(2) 0.0063(17) 0.0108(17) 0.0004(16) C222 0.031(2) 0.038(3) 0.028(2) 0.0026(18) 0.0130(19) -0.0007(18) C223 0.033(3) 0.061(3) 0.036(3) 0.006(2) 0.020(2) -0.001(2) C224 0.028(2) 0.064(4) 0.057(4) -0.006(3) 0.020(2) -0.013(2) C225 0.039(3) 0.066(4) 0.057(4) -0.022(3) 0.020(3) -0.024(3) C226 0.039(3) 0.050(3) 0.040(3) -0.009(2) 0.021(2) -0.008(2) N2 0.035(2) 0.047(2) 0.028(2) -0.0104(16) 0.0182(16) -0.0129(17) Si2 0.0388(7) 0.0387(7) 0.0319(6) -0.0068(5) 0.0179(5) -0.0065(5) C21 0.054(3) 0.038(3) 0.047(3) 0.004(2) 0.022(3) 0.005(2) C22 0.040(3) 0.061(3) 0.050(3) -0.015(3) 0.022(2) -0.001(2) C23 0.043(3) 0.041(3) 0.032(3) 0.005(2) 0.001(2) -0.002(2) C1S 0.066(4) 0.065(4) 0.091(6) -0.007(4) 0.034(4) -0.001(3) Cl1S 0.0845(12) 0.0646(9) 0.0448(9) 0.0048(7) 0.0111(8) 0.0146(8) Cl2S 0.0645(9) 0.0709(10) 0.0600(10) 0.0034(7) 0.0174(8) -0.0017(8) C2S 0.056(4) 0.058(4) 0.087(5) -0.012(3) 0.029(4) -0.003(3) Cl3S 0.0574(8) 0.0634(9) 0.0569(9) -0.0037(7) 0.0225(7) 0.0048(6) Cl4S 0.0750(11) 0.0678(10) 0.0457(9) 0.0044(7) 0.0103(7) 0.0088(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 Ti1 N1 2.080(4) . ? Ti1 N2 2.111(4) . ? Ti1 C1 2.275(5) . ? Ti1 Cl2 2.3517(10) . ? Ti1 Cl3 2.3597(15) . ? Ti1 Cl1 2.3698(15) . ? Ti1 P1 2.9049(14) . ? N1 P1 1.604(4) . ? N1 Si1 1.772(4) . ? Si1 C13 1.869(6) . ? Si1 C11 1.873(5) . ? Si1 C12 1.876(5) . ? P1 C1 1.775(4) . ? P1 C111 1.807(4) . ? P1 C121 1.831(4) . ? C111 C116 1.397(7) . ? C111 C112 1.401(6) . ? C112 C113 1.384(7) . ? C113 C114 1.393(8) . ? C114 C115 1.389(8) . ? C115 C116 1.389(7) . ? C121 C126 1.369(7) . ? C121 C122 1.411(6) . ? C122 C123 1.399(7) . ? C123 C124 1.392(7) . ? C124 C125 1.389(8) . ? C125 C126 1.414(7) . ? C1 C2 1.497(5) . ? C1 H1 1.04(4) . ? C2 P2 1.836(4) . ? P2 N2 1.614(4) . ? P2 C221 1.809(4) . ? P2 C211 1.818(5) . ? C211 C212 1.400(6) . ? C211 C216 1.403(7) . ? C212 C213 1.408(6) . ? C213 C214 1.366(7) . ? C214 C215 1.401(7) . ? C215 C216 1.388(8) . ? C221 C226 1.386(7) . ? C221 C222 1.415(6) . ? C222 C223 1.400(7) . ? C223 C224 1.380(8) . ? C224 C225 1.392(8) . ? C225 C226 1.387(7) . ? N2 Si2 1.759(5) . ? Si2 C22 1.863(5) . ? Si2 C21 1.873(6) . ? Si2 C23 1.898(5) . ? C1S Cl2S 1.753(8) . ? C1S Cl1S 1.771(8) . ? C2S Cl4S 1.742(8) . ? C2S Cl3S 1.770(8) . ? 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 Ti1 N2 151.47(13) . . ? N1 Ti1 C1 69.33(15) . . ? N2 Ti1 C1 82.75(15) . . ? N1 Ti1 Cl2 102.30(12) . . ? N2 Ti1 Cl2 106.11(13) . . ? C1 Ti1 Cl2 169.08(12) . . ? N1 Ti1 Cl3 88.69(11) . . ? N2 Ti1 Cl3 88.80(11) . . ? C1 Ti1 Cl3 96.71(11) . . ? Cl2 Ti1 Cl3 89.94(6) . . ? N1 Ti1 Cl1 93.31(12) . . ? N2 Ti1 Cl1 90.39(11) . . ? C1 Ti1 Cl1 85.88(11) . . ? Cl2 Ti1 Cl1 87.67(6) . . ? Cl3 Ti1 Cl1 177.17(6) . . ? N1 Ti1 P1 32.51(12) . . ? N2 Ti1 P1 118.97(12) . . ? C1 Ti1 P1 37.65(10) . . ? Cl2 Ti1 P1 134.74(6) . . ? Cl3 Ti1 P1 87.28(5) . . ? Cl1 Ti1 P1 95.48(5) . . ? P1 N1 Si1 128.3(2) . . ? P1 N1 Ti1 103.3(2) . . ? Si1 N1 Ti1 128.4(2) . . ? N1 Si1 C13 109.2(2) . . ? N1 Si1 C11 109.9(2) . . ? C13 Si1 C11 108.4(3) . . ? N1 Si1 C12 108.4(3) . . ? C13 Si1 C12 110.2(3) . . ? C11 Si1 C12 110.7(3) . . ? N1 P1 C1 94.4(2) . . ? N1 P1 C111 111.1(2) . . ? C1 P1 C111 112.87(19) . . ? N1 P1 C121 113.4(2) . . ? C1 P1 C121 115.60(19) . . ? C111 P1 C121 108.9(2) . . ? N1 P1 Ti1 44.18(15) . . ? C1 P1 Ti1 51.54(16) . . ? C111 P1 Ti1 132.16(15) . . ? C121 P1 Ti1 118.54(14) . . ? C116 C111 C112 119.9(4) . . ? C116 C111 P1 124.3(3) . . ? C112 C111 P1 115.8(3) . . ? C113 C112 C111 120.3(4) . . ? C112 C113 C114 119.4(5) . . ? C115 C114 C113 120.7(4) . . ? C114 C115 C116 120.1(5) . . ? C115 C116 C111 119.6(5) . . ? C126 C121 C122 119.9(4) . . ? C126 C121 P1 121.2(3) . . ? C122 C121 P1 118.9(3) . . ? C123 C122 C121 120.2(4) . . ? C124 C123 C122 120.2(4) . . ? C125 C124 C123 118.9(4) . . ? C124 C125 C126 121.3(4) . . ? C121 C126 C125 119.4(4) . . ? C2 C1 P1 123.8(3) . . ? C2 C1 Ti1 110.4(3) . . ? P1 C1 Ti1 90.81(18) . . ? C2 C1 H1 113(2) . . ? P1 C1 H1 109(2) . . ? Ti1 C1 H1 107(2) . . ? C1 C2 P2 101.1(3) . . ? N2 P2 C221 112.7(2) . . ? N2 P2 C211 111.8(2) . . ? C221 P2 C211 109.4(2) . . ? N2 P2 C2 111.2(2) . . ? C221 P2 C2 104.8(2) . . ? C211 P2 C2 106.5(2) . . ? C212 C211 C216 117.6(4) . . ? C212 C211 P2 120.2(3) . . ? C216 C211 P2 122.2(3) . . ? C211 C212 C213 121.1(4) . . ? C214 C213 C212 119.9(4) . . ? C213 C214 C215 120.2(4) . . ? C216 C215 C214 119.8(4) . . ? C215 C216 C211 121.4(4) . . ? C226 C221 C222 120.6(4) . . ? C226 C221 P2 125.4(4) . . ? C222 C221 P2 114.0(3) . . ? C223 C222 C221 119.2(4) . . ? C224 C223 C222 119.8(5) . . ? C223 C224 C225 120.3(5) . . ? C226 C225 C224 121.0(5) . . ? C221 C226 C225 119.0(5) . . ? C221 C226 H226 120.5 . . ? C225 C226 H226 120.5 . . ? P2 N2 Si2 123.8(2) . . ? P2 N2 Ti1 112.7(2) . . ? Si2 N2 Ti1 123.5(2) . . ? N2 Si2 C22 109.4(2) . . ? N2 Si2 C21 110.8(2) . . ? C22 Si2 C21 110.0(3) . . ? N2 Si2 C23 111.9(2) . . ? C22 Si2 C23 108.1(3) . . ? C21 Si2 C23 106.4(3) . . ? Cl2S C1S Cl1S 112.5(4) . . ? Cl4S C2S Cl3S 113.3(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.772 _refine_diff_density_min -0.696 _refine_diff_density_rms 0.062