Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Parkin, I.' 'Apostolico, Leonardo' 'Blackman, C.' 'Carmalt, Claire J.' 'Molloy, K.' 'White, Andrew J. P.' 'Williams, David J.' _publ_contact_author_name 'Prof I Parkin' _publ_contact_author_address ; Prof I Parkin Department of Chemistry University College London 20 Gordon Street London WCIH OAJ UNITED KINGDOM ; _publ_contact_author_email 'I.P.PARKIN@UCL.AC.UK' _publ_section_title ; Single-Source CVD Routes to Titanium Phosphide ; data_IP0101 _database_code_CSD 185882 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H46 P2 Cl4 Ti' _chemical_formula_weight 586.25 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2191 1.8069 '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 10.9819(5) _cell_length_b 10.1691(3) _cell_length_c 13.3319(11) _cell_angle_alpha 90.00 _cell_angle_beta 103.415(5) _cell_angle_gamma 90.00 _cell_volume 1448.23(14) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 54 _cell_measurement_theta_min 10.59 _cell_measurement_theta_max 24.78 _exptl_crystal_description plates _exptl_crystal_colour Orange/red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method ? _exptl_crystal_F_000 620 _exptl_absorpt_coefficient_mu 7.017 _exptl_absorpt_correction_type Ellipsoidal _exptl_absorpt_correction_T_min 0.2031 _exptl_absorpt_correction_T_max 0.5376 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2279 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.14 _diffrn_reflns_theta_max 60.00 _reflns_number_total 2153 _reflns_number_observed 1899 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 62 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0874P)^2^+0.4822P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0010(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2091 _refine_ls_number_parameters 147 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_obs 0.0475 _refine_ls_wR_factor_all 0.1322 _refine_ls_wR_factor_obs 0.1238 _refine_ls_goodness_of_fit_all 1.060 _refine_ls_goodness_of_fit_obs 1.087 _refine_ls_restrained_S_all 1.086 _refine_ls_restrained_S_obs 1.086 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ti Ti 0.0000 0.5000 0.5000 0.0228(3) Uani 1 d S . Cl1 Cl 0.06184(8) 0.66135(8) 0.62083(6) 0.0326(3) Uani 1 d . . Cl2 Cl 0.16189(8) 0.37261(9) 0.58638(7) 0.0370(3) Uani 1 d . . P P 0.14101(7) 0.59509(8) 0.38168(6) 0.0230(3) Uani 1 d D . H H 0.0791(37) 0.5900(42) 0.2877(13) 0.043(12) Uiso 1 d D . C1 C 0.2459(3) 0.3591(3) 0.3345(3) 0.0316(8) Uani 1 d . . H1A H 0.1956(3) 0.3167(3) 0.3772(3) 0.038 Uiso 1 calc R . H1B H 0.1952(3) 0.3637(3) 0.2636(3) 0.038 Uiso 1 calc R . C2 C 0.3635(4) 0.2769(4) 0.3369(3) 0.0369(8) Uani 1 d . . H2A H 0.4099(4) 0.2654(4) 0.4086(3) 0.044 Uiso 1 calc R . H2B H 0.3388(4) 0.1897(4) 0.3080(3) 0.044 Uiso 1 calc R . C3 C 0.4479(4) 0.3415(4) 0.2760(3) 0.0405(9) Uani 1 d . . H3A H 0.4058(4) 0.3419(4) 0.2027(3) 0.049 Uiso 1 calc R . H3B H 0.5251(4) 0.2901(4) 0.2842(3) 0.049 Uiso 1 calc R . C4 C 0.4804(4) 0.4814(4) 0.3116(3) 0.0412(9) Uani 1 d . . H4A H 0.5282(4) 0.5224(4) 0.2663(3) 0.049 Uiso 1 calc R . H4B H 0.5335(4) 0.4799(4) 0.3816(3) 0.049 Uiso 1 calc R . C5 C 0.3637(3) 0.5642(4) 0.3107(3) 0.0329(8) Uani 1 d . . H5A H 0.3155(3) 0.5751(4) 0.2395(3) 0.039 Uiso 1 calc R . H5B H 0.3891(3) 0.6517(4) 0.3387(3) 0.039 Uiso 1 calc R . C6 C 0.2810(3) 0.4989(3) 0.3748(3) 0.0257(7) Uani 1 d . . H6A H 0.3323(3) 0.4903(3) 0.4461(3) 0.031 Uiso 1 calc R . C7 C 0.2947(3) 0.7899(3) 0.4954(3) 0.0294(8) Uani 1 d . . H7A H 0.3660(3) 0.7322(3) 0.4945(3) 0.035 Uiso 1 calc R . H7B H 0.2626(3) 0.7674(3) 0.5560(3) 0.035 Uiso 1 calc R . C8 C 0.3378(4) 0.9340(4) 0.5026(3) 0.0395(9) Uani 1 d . . H8A H 0.4005(4) 0.9476(4) 0.5672(3) 0.047 Uiso 1 calc R . H8B H 0.3770(4) 0.9539(4) 0.4453(3) 0.047 Uiso 1 calc R . C9 C 0.2279(4) 1.0266(4) 0.4986(3) 0.0411(9) Uani 1 d . . H9A H 0.2571(4) 1.1178(4) 0.5000(3) 0.049 Uiso 1 calc R . H9B H 0.1938(4) 1.0124(4) 0.5594(3) 0.049 Uiso 1 calc R . C10 C 0.1254(4) 1.0042(3) 0.4014(3) 0.0356(9) Uani 1 d . . H10A H 0.1572(4) 1.0265(3) 0.3407(3) 0.043 Uiso 1 calc R . H10B H 0.0544(4) 1.0622(3) 0.4024(3) 0.043 Uiso 1 calc R . C11 C 0.0812(3) 0.8615(3) 0.3937(3) 0.0289(7) Uani 1 d . . H11A H 0.0183(3) 0.8485(3) 0.3291(3) 0.035 Uiso 1 calc R . H11B H 0.0423(3) 0.8413(3) 0.4510(3) 0.035 Uiso 1 calc R . C12 C 0.1918(3) 0.7686(3) 0.3970(3) 0.0245(7) Uani 1 d . . H12A H 0.2279(3) 0.7910(3) 0.3377(3) 0.029 Uiso 1 calc R . 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 0.0245(4) 0.0231(5) 0.0224(5) 0.0006(3) 0.0088(3) -0.0009(3) Cl1 0.0399(5) 0.0319(5) 0.0277(5) -0.0069(3) 0.0115(3) -0.0060(3) Cl2 0.0344(5) 0.0380(5) 0.0371(5) 0.0051(4) 0.0050(4) 0.0072(4) P 0.0244(4) 0.0234(5) 0.0220(4) -0.0008(3) 0.0071(3) -0.0009(3) C1 0.030(2) 0.031(2) 0.036(2) -0.0026(15) 0.0117(15) -0.0014(15) C2 0.034(2) 0.028(2) 0.049(2) -0.004(2) 0.011(2) 0.004(2) C3 0.037(2) 0.043(2) 0.045(2) -0.002(2) 0.018(2) 0.008(2) C4 0.034(2) 0.047(2) 0.048(2) -0.003(2) 0.020(2) -0.003(2) C5 0.034(2) 0.032(2) 0.038(2) -0.001(2) 0.018(2) -0.0011(15) C6 0.026(2) 0.025(2) 0.028(2) -0.0002(13) 0.0114(14) -0.0013(13) C7 0.026(2) 0.030(2) 0.032(2) 0.0008(14) 0.0056(14) -0.0013(14) C8 0.039(2) 0.034(2) 0.044(2) -0.005(2) 0.007(2) -0.012(2) C9 0.053(2) 0.026(2) 0.044(2) -0.007(2) 0.011(2) -0.004(2) C10 0.046(2) 0.027(2) 0.035(2) 0.0035(15) 0.012(2) 0.004(2) C11 0.029(2) 0.029(2) 0.028(2) 0.0018(13) 0.0053(13) 0.0031(14) C12 0.028(2) 0.022(2) 0.025(2) 0.0011(12) 0.0098(13) -0.0011(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti Cl2 2.2837(8) . ? Ti Cl2 2.2837(8) 3_566 ? Ti Cl1 2.2892(8) . ? Ti Cl1 2.2892(8) 3_566 ? Ti P 2.6372(8) . ? Ti P 2.6372(8) 3_566 ? P C6 1.842(3) . ? P C12 1.848(3) . ? C1 C2 1.533(5) . ? C1 C6 1.538(5) . ? C2 C3 1.515(6) . ? C3 C4 1.516(6) . ? C4 C5 1.531(5) . ? C5 C6 1.535(5) . ? C7 C12 1.536(5) . ? C7 C8 1.536(5) . ? C8 C9 1.522(6) . ? C9 C10 1.524(6) . ? C10 C11 1.526(5) . ? C11 C12 1.531(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 Ti Cl2 180.0 . 3_566 ? Cl2 Ti Cl1 89.00(3) . . ? Cl2 Ti Cl1 91.00(3) 3_566 . ? Cl2 Ti Cl1 91.00(3) . 3_566 ? Cl2 Ti Cl1 89.00(3) 3_566 3_566 ? Cl1 Ti Cl1 180.0 . 3_566 ? Cl2 Ti P 90.75(3) . . ? Cl2 Ti P 89.25(3) 3_566 . ? Cl1 Ti P 92.21(3) . . ? Cl1 Ti P 87.79(3) 3_566 . ? Cl2 Ti P 89.25(3) . 3_566 ? Cl2 Ti P 90.75(3) 3_566 3_566 ? Cl1 Ti P 87.79(3) . 3_566 ? Cl1 Ti P 92.21(3) 3_566 3_566 ? P Ti P 180.0 . 3_566 ? C6 P C12 106.17(15) . . ? C6 P Ti 116.60(11) . . ? C12 P Ti 119.21(11) . . ? C2 C1 C6 110.8(3) . . ? C3 C2 C1 111.7(3) . . ? C2 C3 C4 111.6(3) . . ? C3 C4 C5 112.2(3) . . ? C4 C5 C6 111.1(3) . . ? C5 C6 C1 109.8(3) . . ? C5 C6 P 114.0(2) . . ? C1 C6 P 111.3(2) . . ? C12 C7 C8 110.0(3) . . ? C9 C8 C7 111.0(3) . . ? C8 C9 C10 111.2(3) . . ? C9 C10 C11 111.1(3) . . ? C10 C11 C12 110.3(3) . . ? C11 C12 C7 111.1(3) . . ? C11 C12 P 111.7(2) . . ? C7 C12 P 111.9(2) . . ? _refine_diff_density_max 0.634 _refine_diff_density_min -0.529 _refine_diff_density_rms 0.083 data_IP0104 _database_code_CSD 185883 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H24 P2 Cl4 Ti' _chemical_formula_weight 588.09 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2191 1.8069 '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 12.2287(15) _cell_length_b 14.560(2) _cell_length_c 16.047(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.254(12) _cell_angle_gamma 90.00 _cell_volume 2662.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 10.77 _cell_measurement_theta_max 22.43 _exptl_crystal_description 'platy needles' _exptl_crystal_colour Orange _exptl_crystal_size_max 0.90 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method ? _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 7.657 _exptl_absorpt_correction_type 'Lamina [0 1 0]' _exptl_absorpt_correction_T_min 0.2124 _exptl_absorpt_correction_T_max 0.7627 _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3479 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0617 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.88 _diffrn_reflns_theta_max 57.20 _reflns_number_total 3294 _reflns_number_observed 2429 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 250 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0913P)^2^+0.0000P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0004(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3044 _refine_ls_number_parameters 251 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0848 _refine_ls_R_factor_obs 0.0550 _refine_ls_wR_factor_all 0.1594 _refine_ls_wR_factor_obs 0.1306 _refine_ls_goodness_of_fit_all 1.022 _refine_ls_goodness_of_fit_obs 1.073 _refine_ls_restrained_S_all 1.113 _refine_ls_restrained_S_obs 1.073 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ti Ti 0.69152(8) 0.64753(7) 0.11808(7) 0.0246(3) Uani 1 d . . Cl1 Cl 0.65776(12) 0.50615(10) 0.16255(11) 0.0367(4) Uani 1 d . . Cl2 Cl 0.72537(12) 0.80254(10) 0.11691(11) 0.0357(4) Uani 1 d . . Cl3 Cl 0.86101(12) 0.61173(12) 0.09878(11) 0.0386(4) Uani 1 d . . Cl4 Cl 0.54635(13) 0.64420(12) -0.01705(10) 0.0404(4) Uani 1 d . . P1 P 0.53398(11) 0.71399(10) 0.18092(10) 0.0264(4) Uani 1 d . . P2 P 0.80921(11) 0.65862(10) 0.29195(9) 0.0246(4) Uani 1 d . . C1 C 0.6151(5) 0.7497(5) 0.2972(4) 0.0322(13) Uani 1 d . . H1A H 0.6593(5) 0.8069(5) 0.2981(4) 0.039 Uiso 1 calc R . H1B H 0.5599(5) 0.7613(5) 0.3283(4) 0.039 Uiso 1 calc R . C2 C 0.6993(5) 0.6729(4) 0.3435(4) 0.0297(13) Uani 1 d . . H2A H 0.6552(5) 0.6148(4) 0.3386(4) 0.036 Uiso 1 calc R . H2B H 0.7385(5) 0.6876(4) 0.4077(4) 0.036 Uiso 1 calc R . C3 C 0.5038(3) 0.9035(3) 0.1445(2) 0.041(2) Uani 1 d G . H3A H 0.5701(3) 0.9127(3) 0.1977(2) 0.049 Uiso 1 calc R . C4 C 0.4519(4) 0.9779(2) 0.0903(3) 0.048(2) Uani 1 d G . H4A H 0.4828(5) 1.0379(2) 0.1065(4) 0.058 Uiso 1 calc R . C5 C 0.3548(4) 0.9645(3) 0.0125(3) 0.053(2) Uani 1 d G . H5A H 0.3194(5) 1.0153(3) -0.0246(4) 0.063 Uiso 1 calc R . C6 C 0.3096(3) 0.8767(3) -0.0112(2) 0.051(2) Uani 1 d G . H6A H 0.2433(4) 0.8675(4) -0.0643(3) 0.062 Uiso 1 calc R . C7 C 0.3615(3) 0.8023(2) 0.0430(3) 0.0386(15) Uani 1 d G . H7A H 0.3306(5) 0.7423(3) 0.0269(4) 0.046 Uiso 1 calc R . C8 C 0.4586(3) 0.8157(2) 0.1209(2) 0.0349(14) Uani 1 d G . C9 C 0.3785(3) 0.5643(3) 0.1307(3) 0.0339(14) Uani 1 d G . H9A H 0.4215(3) 0.5462(3) 0.0946(3) 0.041 Uiso 1 calc R . C10 C 0.2816(3) 0.5136(3) 0.1293(3) 0.042(2) Uani 1 d G . H10A H 0.2583(5) 0.4608(3) 0.0923(4) 0.051 Uiso 1 calc R . C11 C 0.2187(3) 0.5402(3) 0.1821(3) 0.051(2) Uani 1 d G . H11A H 0.1524(4) 0.5055(5) 0.1812(5) 0.061 Uiso 1 calc R . C12 C 0.2528(4) 0.6174(4) 0.2363(3) 0.070(3) Uani 1 d G . H12A H 0.2098(5) 0.6356(5) 0.2724(5) 0.084 Uiso 1 calc R . C13 C 0.3497(4) 0.6681(3) 0.2377(3) 0.052(2) Uani 1 d G . H13A H 0.3730(5) 0.7209(4) 0.2747(4) 0.063 Uiso 1 calc R . C14 C 0.4126(3) 0.6416(3) 0.1849(3) 0.0325(14) Uani 1 d G . C15 C 0.8504(3) 0.4891(3) 0.3831(3) 0.042(2) Uani 1 d G . H15A H 0.7780(3) 0.4982(3) 0.3913(3) 0.051 Uiso 1 calc R . C16 C 0.9149(3) 0.4095(3) 0.4148(3) 0.045(2) Uani 1 d G . H16A H 0.8866(5) 0.3643(3) 0.4446(4) 0.054 Uiso 1 calc R . C17 C 1.0208(3) 0.3961(2) 0.4028(3) 0.039(2) Uani 1 d G . H17A H 1.0648(4) 0.3417(3) 0.4244(4) 0.047 Uiso 1 calc R . C18 C 1.0621(3) 0.4622(3) 0.3591(3) 0.040(2) Uani 1 d G . H18A H 1.1345(4) 0.4531(4) 0.3509(5) 0.048 Uiso 1 calc R . C19 C 0.9977(3) 0.5418(2) 0.3275(3) 0.0352(14) Uani 1 d G . H19A H 1.0259(4) 0.5870(3) 0.2976(4) 0.042 Uiso 1 calc R . C20 C 0.8918(3) 0.5552(2) 0.3395(3) 0.0278(12) Uani 1 d G . C21 C 0.9379(3) 0.7892(3) 0.4186(2) 0.0380(15) Uani 1 d G . H21A H 0.8876(3) 0.7750(3) 0.4501(2) 0.046 Uiso 1 calc R . C22 C 1.0314(4) 0.8493(3) 0.4556(2) 0.048(2) Uani 1 d G . H22A H 1.0449(5) 0.8761(5) 0.5125(3) 0.057 Uiso 1 calc R . C23 C 1.1050(3) 0.8701(3) 0.4095(3) 0.044(2) Uani 1 d G . H23A H 1.1689(4) 0.9111(4) 0.4349(4) 0.053 Uiso 1 calc R . C24 C 1.0852(3) 0.8308(3) 0.3264(3) 0.043(2) Uani 1 d G . H24A H 1.1355(4) 0.8450(5) 0.2949(3) 0.051 Uiso 1 calc R . C25 C 0.9918(3) 0.7707(3) 0.2893(2) 0.0362(14) Uani 1 d G . H25A H 0.9782(5) 0.7438(4) 0.2325(3) 0.043 Uiso 1 calc R . C26 C 0.9181(3) 0.7499(3) 0.3354(2) 0.0260(12) Uani 1 d G . 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 0.0156(5) 0.0294(5) 0.0280(6) -0.0036(4) 0.0070(4) -0.0010(4) Cl1 0.0257(7) 0.0294(7) 0.0488(9) -0.0010(7) 0.0059(6) -0.0043(6) Cl2 0.0214(6) 0.0306(7) 0.0544(9) 0.0039(7) 0.0130(6) -0.0016(6) Cl3 0.0252(7) 0.0486(9) 0.0471(9) -0.0068(7) 0.0191(6) 0.0026(7) Cl4 0.0316(7) 0.0537(9) 0.0289(7) -0.0052(7) 0.0027(6) -0.0026(7) P1 0.0148(6) 0.0315(7) 0.0313(8) -0.0052(6) 0.0062(5) 0.0000(6) P2 0.0139(6) 0.0292(7) 0.0293(7) -0.0009(6) 0.0060(5) -0.0008(6) C1 0.015(2) 0.044(3) 0.035(3) -0.012(3) 0.006(2) 0.000(3) C2 0.020(3) 0.041(3) 0.026(3) -0.001(3) 0.005(2) -0.003(3) C3 0.027(3) 0.041(4) 0.058(4) -0.005(3) 0.022(3) 0.006(3) C4 0.043(4) 0.035(3) 0.081(5) 0.006(4) 0.041(4) 0.013(3) C5 0.054(4) 0.051(4) 0.065(5) 0.017(4) 0.035(4) 0.029(4) C6 0.041(4) 0.071(5) 0.041(4) 0.011(4) 0.014(3) 0.028(4) C7 0.029(3) 0.049(4) 0.036(3) 0.000(3) 0.010(3) 0.009(3) C8 0.021(3) 0.037(3) 0.047(4) -0.005(3) 0.012(3) 0.005(3) C9 0.019(3) 0.044(4) 0.038(3) 0.006(3) 0.010(2) -0.001(3) C10 0.025(3) 0.053(4) 0.041(4) 0.012(3) 0.002(3) -0.010(3) C11 0.024(3) 0.075(5) 0.051(4) 0.013(4) 0.010(3) -0.018(4) C12 0.043(4) 0.120(8) 0.061(5) -0.020(6) 0.033(4) -0.028(5) C13 0.038(4) 0.078(5) 0.050(4) -0.019(4) 0.027(3) -0.012(4) C14 0.019(3) 0.044(3) 0.033(3) 0.006(3) 0.007(2) 0.000(3) C15 0.027(3) 0.051(4) 0.052(4) 0.014(4) 0.018(3) 0.011(3) C16 0.046(4) 0.044(4) 0.051(4) 0.016(3) 0.025(3) 0.006(3) C17 0.028(3) 0.043(3) 0.042(4) 0.005(3) 0.005(3) 0.009(3) C18 0.024(3) 0.041(4) 0.055(4) 0.004(3) 0.013(3) 0.008(3) C19 0.023(3) 0.039(3) 0.046(4) 0.004(3) 0.014(3) -0.004(3) C20 0.015(2) 0.035(3) 0.028(3) -0.002(3) 0.001(2) -0.002(2) C21 0.036(3) 0.039(3) 0.040(4) -0.004(3) 0.014(3) -0.007(3) C22 0.050(4) 0.050(4) 0.039(4) -0.015(3) 0.011(3) -0.019(4) C23 0.032(3) 0.039(4) 0.048(4) -0.002(3) -0.001(3) -0.012(3) C24 0.025(3) 0.046(4) 0.050(4) 0.002(3) 0.005(3) -0.015(3) C25 0.025(3) 0.042(4) 0.037(3) -0.002(3) 0.007(3) -0.009(3) C26 0.019(2) 0.026(3) 0.029(3) 0.001(2) 0.003(2) -0.004(2) _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 Cl4 2.251(2) . ? Ti Cl3 2.265(2) . ? Ti Cl1 2.265(2) . ? Ti Cl2 2.296(2) . ? Ti P2 2.640(2) . ? Ti P1 2.660(2) . ? P1 C8 1.824(3) . ? P1 C14 1.840(3) . ? P1 C1 1.842(6) . ? P2 C20 1.819(3) . ? P2 C2 1.828(6) . ? P2 C26 1.831(3) . ? C1 C2 1.519(9) . ? C3 C4 1.39 . ? C3 C8 1.39 . ? C4 C5 1.39 . ? C5 C6 1.39 . ? C6 C7 1.39 . ? C7 C8 1.39 . ? C9 C10 1.39 . ? C9 C14 1.39 . ? C10 C11 1.39 . ? C11 C12 1.39 . ? C12 C13 1.39 . ? C13 C14 1.39 . ? C15 C16 1.39 . ? C15 C20 1.39 . ? C16 C17 1.39 . ? C17 C18 1.39 . ? C18 C19 1.39 . ? C19 C20 1.39 . ? C21 C22 1.39 . ? C21 C26 1.39 . ? C22 C23 1.39 . ? C23 C24 1.39 . ? C24 C25 1.39 . ? C25 C26 1.39 . ? 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 Cl4 Ti Cl3 107.74(7) . . ? Cl4 Ti Cl1 96.53(7) . . ? Cl3 Ti Cl1 96.57(7) . . ? Cl4 Ti Cl2 95.44(7) . . ? Cl3 Ti Cl2 92.78(7) . . ? Cl1 Ti Cl2 161.79(8) . . ? Cl4 Ti P2 163.12(6) . . ? Cl3 Ti P2 89.05(6) . . ? Cl1 Ti P2 79.31(6) . . ? Cl2 Ti P2 85.28(6) . . ? Cl4 Ti P1 86.92(6) . . ? Cl3 Ti P1 163.79(7) . . ? Cl1 Ti P1 88.36(6) . . ? Cl2 Ti P1 78.63(6) . . ? P2 Ti P1 76.66(5) . . ? C8 P1 C14 102.9(2) . . ? C8 P1 C1 106.8(3) . . ? C14 P1 C1 105.8(2) . . ? C8 P1 Ti 113.08(15) . . ? C14 P1 Ti 120.58(14) . . ? C1 P1 Ti 106.7(2) . . ? C20 P2 C2 107.0(2) . . ? C20 P2 C26 103.0(2) . . ? C2 P2 C26 107.3(2) . . ? C20 P2 Ti 113.54(15) . . ? C2 P2 Ti 106.1(2) . . ? C26 P2 Ti 119.30(13) . . ? C2 C1 P1 108.0(4) . . ? C1 C2 P2 109.9(4) . . ? C4 C3 C8 120.0 . . ? C3 C4 C5 120.0 . . ? C4 C5 C6 120.0 . . ? C7 C6 C5 120.0 . . ? C6 C7 C8 120.0 . . ? C7 C8 C3 120.0 . . ? C7 C8 P1 117.7(2) . . ? C3 C8 P1 121.8(2) . . ? C10 C9 C14 120.0 . . ? C11 C10 C9 120.0 . . ? C12 C11 C10 120.0 . . ? C11 C12 C13 120.0 . . ? C14 C13 C12 120.0 . . ? C13 C14 C9 120.0 . . ? C13 C14 P1 119.6(2) . . ? C9 C14 P1 120.3(2) . . ? C16 C15 C20 120.0 . . ? C15 C16 C17 120.0 . . ? C18 C17 C16 120.0 . . ? C19 C18 C17 120.0 . . ? C18 C19 C20 120.0 . . ? C19 C20 C15 120.0 . . ? C19 C20 P2 117.5(2) . . ? C15 C20 P2 122.4(2) . . ? C22 C21 C26 120.0 . . ? C23 C22 C21 120.0 . . ? C22 C23 C24 120.0 . . ? C25 C24 C23 120.0 . . ? C26 C25 C24 120.0 . . ? C25 C26 C21 120.0 . . ? C25 C26 P2 118.5(2) . . ? C21 C26 P2 120.9(2) . . ? _refine_diff_density_max 0.517 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.093