# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1348 data_hanks _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20 H36 P6 Ti' _chemical_formula_weight 510.21 _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' 0.0033 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' '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, -z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 11.632(6) _cell_length_b 16.114(5) _cell_length_c 13.920(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2609.1(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method ? _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.701 _exptl_absorpt_correction_type psiscan _exptl_absorpt_correction_T_min 0.95 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device CAD4 _diffrn_measurement_method 'omega-2theta scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2112 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 29.96 _reflns_number_total 2112 _reflns_number_observed 2036 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 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^)+(0.0211P)^2^+1.6906P] 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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.12(3) _refine_ls_number_reflns 2112 _refine_ls_number_parameters 195 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0260 _refine_ls_R_factor_obs 0.0245 _refine_ls_wR_factor_all 0.0630 _refine_ls_wR_factor_obs 0.0619 _refine_ls_goodness_of_fit_all 1.063 _refine_ls_goodness_of_fit_obs 1.066 _refine_ls_restrained_S_all 1.063 _refine_ls_restrained_S_obs 1.066 _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 0.33236(3) 0.2500 0.01765(10) Uani 1 d S . M1 C 0.1246 0.3260 0.3426 0.000 Uiso 0.00 d P 1 P1 P 0.10839(5) 0.22204(3) 0.33459(4) 0.02131(11) Uani 1 d . 2 P2 P 0.21487(4) 0.30608(3) 0.25184(5) 0.02188(11) Uani 1 d . 2 P3 P 0.08194(4) 0.40310(3) 0.40648(4) 0.01955(11) Uani 1 d . 2 C1 C 0.0417(2) 0.29763(12) 0.41054(15) 0.0191(3) Uani 1 d . 2 C2 C 0.1761(2) 0.40090(12) 0.30948(14) 0.0191(3) Uani 1 d . 2 C3 C -0.0332(2) 0.26710(13) 0.4950(2) 0.0240(4) Uani 1 d . 2 C4 C -0.1110(3) 0.3359(2) 0.5329(2) 0.0377(6) Uani 1 d . 2 H4C H -0.1498(31) 0.3135(22) 0.5893(30) 0.046(9) Uiso 1 d . 2 H4B H -0.0683(31) 0.3806(23) 0.5619(27) 0.050(10) Uiso 1 d . 2 H4A H -0.1619(28) 0.3545(20) 0.4826(25) 0.035(8) Uiso 1 d . 2 C5 C 0.0485(2) 0.2399(2) 0.5761(2) 0.0342(5) Uani 1 d . 2 H5C H 0.0075(30) 0.2249(18) 0.6309(23) 0.035(7) Uiso 1 d . 2 H5B H 0.0924(28) 0.1922(22) 0.5559(24) 0.037(8) Uiso 1 d . 2 H5A H 0.0872(30) 0.2842(24) 0.5902(26) 0.049(10) Uiso 1 d . 2 C6 C -0.1076(3) 0.1925(2) 0.4672(2) 0.0350(6) Uani 1 d . 2 H6C H -0.0609(27) 0.1471(21) 0.4472(24) 0.037(9) Uiso 1 d . 2 H6B H -0.1512(31) 0.1737(22) 0.5244(28) 0.047(10) Uiso 1 d . 2 H6A H -0.1477(32) 0.2043(23) 0.4195(31) 0.048(10) Uiso 1 d . 2 C7 C 0.2369(2) 0.48090(13) 0.27602(15) 0.0229(4) Uani 1 d . 2 C8 C 0.1733(3) 0.5590(2) 0.3082(2) 0.0376(6) Uani 1 d . 2 H8C H 0.2146(30) 0.6049(21) 0.2859(24) 0.047(10) Uiso 1 d . 2 H8B H 0.0947(31) 0.5582(20) 0.2761(26) 0.050(10) Uiso 1 d . 2 H8A H 0.1589(31) 0.5630(22) 0.3786(29) 0.048(10) Uiso 1 d . 2 C9 C 0.3559(2) 0.4823(2) 0.3232(3) 0.0428(7) Uani 1 d . 2 H9C H 0.3973(29) 0.5332(20) 0.3018(25) 0.041(9) Uiso 1 d . 2 H9B H 0.3521(30) 0.4812(23) 0.3858(30) 0.046(10) Uiso 1 d . 2 H9A H 0.3958(36) 0.4270(26) 0.3081(33) 0.069(13) Uiso 1 d . 2 C10 C 0.2499(3) 0.4833(2) 0.1671(2) 0.0419(7) Uani 1 d . 2 H10C H 0.1823(41) 0.4817(33) 0.1297(40) 0.090(17) Uiso 1 d . 2 H10B H 0.2924(39) 0.5267(28) 0.1494(34) 0.070(13) Uiso 1 d . 2 H10A H 0.2989(39) 0.4401(28) 0.1448(35) 0.068(13) Uiso 1 d . 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 Ti 0.0183(2) 0.0183(2) 0.0164(2) 0.000 -0.0031(2) 0.000 P1 0.0224(2) 0.0165(2) 0.0250(2) 0.0007(2) -0.0023(2) 0.0025(2) P2 0.0199(2) 0.0215(2) 0.0243(2) -0.0020(2) 0.0027(2) 0.0021(2) P3 0.0218(2) 0.0193(2) 0.0175(2) -0.0027(2) 0.0020(2) -0.0036(2) C1 0.0195(8) 0.0189(8) 0.0190(8) 0.0008(7) -0.0017(7) -0.0019(7) C2 0.0196(8) 0.0186(8) 0.0190(8) -0.0006(7) -0.0002(7) -0.0012(7) C3 0.0249(9) 0.0272(10) 0.0199(8) 0.0048(8) -0.0013(8) -0.0071(8) C4 0.0372(13) 0.0407(13) 0.0351(12) 0.0056(11) 0.0174(11) 0.0024(12) C5 0.0386(13) 0.0409(13) 0.0231(10) 0.0110(10) -0.0067(10) -0.0090(11) C6 0.0399(13) 0.0378(13) 0.0272(10) 0.0074(10) -0.0033(11) -0.0192(12) C7 0.0234(9) 0.0228(9) 0.0224(9) -0.0005(7) 0.0035(7) -0.0066(8) C8 0.0427(14) 0.0206(10) 0.049(2) -0.0005(10) 0.0135(12) -0.0044(10) C9 0.0308(12) 0.0393(15) 0.058(2) 0.0060(13) -0.0064(13) -0.0151(11) C10 0.064(2) 0.0318(13) 0.0300(12) 0.0009(10) 0.0118(13) -0.0168(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 M1 1.9423(6) 4 ? Ti M1 1.9423(6) . ? Ti C1 2.354(2) 4 ? Ti C1 2.354(2) . ? Ti C2 2.470(2) . ? Ti C2 2.470(2) 4 ? Ti P1 2.4771(8) 4 ? Ti P1 2.4771(8) . ? Ti P2 2.5351(14) 4 ? Ti P2 2.5351(14) . ? Ti P3 2.6368(8) . ? Ti P3 2.6368(8) 4 ? P1 C1 1.790(2) . ? P1 P2 2.1668(9) . ? P2 C2 1.784(2) . ? P3 C2 1.739(2) . ? P3 C1 1.764(2) . ? C1 C3 1.544(3) . ? C2 C7 1.542(3) . ? C3 C4 1.526(4) . ? C3 C6 1.531(3) . ? C3 C5 1.539(3) . ? C7 C10 1.524(4) . ? C7 C8 1.527(3) . ? C7 C9 1.533(4) . ? 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 M1 Ti M1 173.91(3) 4 . ? C1 Ti C1 152.50(10) 4 . ? C1 Ti C2 126.55(7) 4 . ? C1 Ti C2 67.49(7) . . ? C1 Ti C2 67.49(7) 4 4 ? C1 Ti C2 126.55(7) . 4 ? C2 Ti C2 126.87(10) . 4 ? C1 Ti P1 43.39(5) 4 4 ? C1 Ti P1 112.68(5) . 4 ? C2 Ti P1 154.47(5) . 4 ? C2 Ti P1 74.90(5) 4 4 ? C1 Ti P1 112.68(5) 4 . ? C1 Ti P1 43.39(5) . . ? C2 Ti P1 74.90(5) . . ? C2 Ti P1 154.47(5) 4 . ? P1 Ti P1 88.28(4) 4 . ? C1 Ti P2 75.37(5) 4 4 ? C1 Ti P2 99.97(5) . 4 ? C2 Ti P2 153.59(5) . 4 ? C2 Ti P2 41.74(5) 4 4 ? P1 Ti P2 51.21(2) 4 4 ? P1 Ti P2 112.75(3) . 4 ? C1 Ti P2 99.97(5) 4 . ? C1 Ti P2 75.37(5) . . ? C2 Ti P2 41.74(5) . . ? C2 Ti P2 153.59(5) 4 . ? P1 Ti P2 112.75(3) 4 . ? P1 Ti P2 51.21(2) . . ? P2 Ti P2 160.77(3) 4 . ? C1 Ti P3 164.03(5) 4 . ? C1 Ti P3 40.90(5) . . ? C2 Ti P3 39.64(5) . . ? C2 Ti P3 112.54(5) 4 . ? P1 Ti P3 152.49(2) 4 . ? P1 Ti P3 74.55(3) . . ? P2 Ti P3 115.91(2) 4 . ? P2 Ti P3 72.99(2) . . ? C1 Ti P3 40.90(5) 4 4 ? C1 Ti P3 164.03(5) . 4 ? C2 Ti P3 112.54(5) . 4 ? C2 Ti P3 39.64(5) 4 4 ? P1 Ti P3 74.55(3) 4 4 ? P1 Ti P3 152.49(2) . 4 ? P2 Ti P3 72.99(2) 4 4 ? P2 Ti P3 115.91(2) . 4 ? P3 Ti P3 128.77(3) . 4 ? C1 P1 P2 97.84(7) . . ? C1 P1 Ti 64.65(7) . . ? P2 P1 Ti 65.78(4) . . ? C2 P2 P1 98.72(7) . . ? C2 P2 Ti 67.17(7) . . ? P1 P2 Ti 63.01(3) . . ? C2 P3 C1 99.92(10) . . ? C2 P3 Ti 64.99(7) . . ? C1 P3 Ti 60.92(7) . . ? C3 C1 P3 118.76(14) . . ? C3 C1 P1 118.53(14) . . ? P3 C1 P1 121.47(12) . . ? C3 C1 Ti 133.03(14) . . ? P3 C1 Ti 78.18(8) . . ? P1 C1 Ti 71.96(7) . . ? C7 C2 P3 120.42(14) . . ? C7 C2 P2 117.64(14) . . ? P3 C2 P2 121.74(12) . . ? C7 C2 Ti 130.76(14) . . ? P3 C2 Ti 75.37(8) . . ? P2 C2 Ti 71.10(7) . . ? C4 C3 C6 108.8(2) . . ? C4 C3 C5 108.6(2) . . ? C6 C3 C5 108.1(2) . . ? C4 C3 C1 111.5(2) . . ? C6 C3 C1 112.1(2) . . ? C5 C3 C1 107.5(2) . . ? C10 C7 C8 108.6(2) . . ? C10 C7 C9 109.6(2) . . ? C8 C7 C9 107.4(2) . . ? C10 C7 C2 111.6(2) . . ? C8 C7 C2 112.2(2) . . ? C9 C7 C2 107.3(2) . . ? _refine_diff_density_max 0.556 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.055 #===END # CIF produced by WinGX routine CIF_UPDATE # Created on 1999-05-04 at 13:10:04 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.1beta3 # Request file : c:\wingx\files\archive.dat # CIF files read : may899 dreduc struct difabs data_may899 _audit_creation_date 1999-05-04T13:10:04-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta3 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C25 H39 P7 Ti1' _chemical_formula_structural 'C25 H39 P7 TI' _chemical_formula_sum 'C25 H45 P7 Ti' _chemical_formula_weight 610.3 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.299(5) _cell_length_b 11.910(6) _cell_length_c 14.230(10) _cell_angle_alpha 86.48(5) _cell_angle_beta 71.00(5) _cell_angle_gamma 68.75(4) _cell_volume 1535.1(16) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.4 _cell_measurement_theta_max 8.7 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.32 _exptl_crystal_density_method none _exptl_crystal_F_000 644 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.657 _exptl_absorpt_factor_muR 0.099 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; Walker, N. & Stuart, D (1983) Acta. Cryst. A39, 158-166 ; _exptl_absorpt_correction_T_min 0.2065 _exptl_absorpt_correction_T_max 0.9054 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_ub_11 -0.14476E-1 _diffrn_orient_matrix_ub_12 0.76409E-1 _diffrn_orient_matrix_ub_13 -0.03562 _diffrn_orient_matrix_ub_21 -0.101788 _diffrn_orient_matrix_ub_22 0.5963E-2 _diffrn_orient_matrix_ub_23 0.5872E-2 _diffrn_orient_matrix_ub_31 -0.40129E-1 _diffrn_orient_matrix_ub_32 0.47755E-1 _diffrn_orient_matrix_ub_33 0.65298E-1 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius TurboCAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 2 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_standards_decay_corr_max 1.051 _diffrn_standards_decay_corr_min 0.993 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 -2 4 -2 -2 4 _diffrn_reflns_number 5362 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_sigmaI/netI 0.061 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 24.99 _reflns_number_total 5362 _reflns_number_gt 4021 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1998)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 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^)+(0.1512P)^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_extinction_method none _refine_ls_number_reflns 5362 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0992 _refine_ls_R_factor_gt 0.0765 _refine_ls_wR_factor_gt 0.1964 _refine_ls_wR_factor_all 0.212 _refine_ls_goodness_of_fit_gt 1.081 _refine_ls_goodness_of_fit_all 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_restrained_S_obs 1.081 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.306 _refine_diff_density_min -1.023 _refine_diff_density_rms 0.15 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ti Ti 0.49974(10) 1.16181(8) 0.23588(7) 0.0194(3) Uani 1 d . . P1 P 0.55646(15) 0.94169(12) 0.30704(10) 0.0204(3) Uani 1 d . . P2 P 0.4885(2) 1.10271(12) 0.40712(10) 0.0212(3) Uani 1 d . . P3 P 0.2527(2) 1.11591(13) 0.31229(10) 0.0223(3) Uani 1 d . . P4 P 0.4723(2) 0.99568(13) 0.14469(10) 0.0229(3) Uani 1 d . . P5 P 0.7159(2) 1.21984(13) 0.11744(10) 0.0254(4) Uani 1 d . . P6 P 0.5421(2) 1.25433(13) 0.05728(10) 0.0262(4) Uani 1 d . . P7 P 0.4307(2) 1.40337(13) 0.25391(11) 0.0244(3) Uani 1 d . . C1 C 0.3847(6) 0.9610(5) 0.2780(4) 0.0225(11) Uani 1 d . . C2 C 0.3064(6) 1.1702(5) 0.3995(4) 0.0211(11) Uani 1 d . . C3 C 0.3228(6) 0.8600(5) 0.3018(4) 0.0278(12) Uani 1 d . . C4 C 0.2031(7) 0.8815(6) 0.2527(5) 0.0371(15) Uani 1 d . . H4C H 0.1239(7) 0.9596(6) 0.2783(5) 0.056 Uiso 1 calc R . H4B H 0.1628(7) 0.8171(6) 0.2684(5) 0.056 Uiso 1 calc R . H4A H 0.2465(7) 0.8816(6) 0.1804(5) 0.056 Uiso 1 calc R . C5 C 0.2574(7) 0.8580(6) 0.4145(4) 0.0367(15) Uani 1 d . . H5C H 0.1791(7) 0.9361(6) 0.4413(4) 0.055 Uiso 1 calc R . H5B H 0.3347(7) 0.8427(6) 0.4447(4) 0.055 Uiso 1 calc R . H5A H 0.2165(7) 0.7939(6) 0.4298(4) 0.055 Uiso 1 calc R . C6 C 0.4440(7) 0.7386(5) 0.2610(6) 0.042(2) Uani 1 d . . H6C H 0.4865(7) 0.7393(5) 0.1886(6) 0.062 Uiso 1 calc R . H6B H 0.4028(7) 0.6747(5) 0.2766(6) 0.062 Uiso 1 calc R . H6A H 0.5211(7) 0.7234(5) 0.2914(6) 0.062 Uiso 1 calc R . C7 C 0.1882(6) 1.2652(5) 0.4812(4) 0.0271(12) Uani 1 d . . C8 C 0.1281(7) 1.1928(6) 0.5654(4) 0.042(2) Uani 1 d . . H8C H 0.2083(7) 1.1401(6) 0.5886(4) 0.062 Uiso 1 calc R . H8B H 0.0860(7) 1.1436(6) 0.5410(4) 0.062 Uiso 1 calc R . H8A H 0.0515(7) 1.2483(6) 0.6207(4) 0.062 Uiso 1 calc R . C9 C 0.2481(7) 1.3443(6) 0.5221(5) 0.0366(15) Uani 1 d . . H9C H 0.3295(7) 1.2929(6) 0.5447(5) 0.055 Uiso 1 calc R . H9B H 0.1695(7) 1.3971(6) 0.5782(5) 0.055 Uiso 1 calc R . H9A H 0.2837(7) 1.3935(6) 0.4697(5) 0.055 Uiso 1 calc R . C10 C 0.0618(7) 1.3464(6) 0.4464(5) 0.043(2) Uani 1 d . . H10C H 0.0224(7) 1.2965(6) 0.4200(5) 0.064 Uiso 1 calc R . H10B H 0.0979(7) 1.3957(6) 0.3942(5) 0.064 Uiso 1 calc R . H10A H -0.0163(7) 1.3992(6) 0.5028(5) 0.064 Uiso 1 calc R . C11 C 0.6340(6) 0.9822(5) 0.1782(4) 0.0229(11) Uani 1 d . . C12 C 0.7911(6) 0.9034(5) 0.1146(4) 0.0243(12) Uani 1 d . . C13 C 0.9073(6) 0.9145(5) 0.1546(4) 0.0313(13) Uani 1 d . . H13C H 0.8873(6) 0.8921(5) 0.2239(4) 0.047 Uiso 1 calc R . H13B H 0.9036(6) 0.9980(5) 0.1515(4) 0.047 Uiso 1 calc R . H13A H 1.0053(6) 0.8605(5) 0.1142(4) 0.047 Uiso 1 calc R . C14 C 0.8205(7) 0.9382(6) 0.0062(4) 0.0316(13) Uani 1 d . . H14C H 0.7455(7) 0.9307(6) -0.0186(4) 0.047 Uiso 1 calc R . H14B H 0.9183(7) 0.8843(6) -0.0347(4) 0.047 Uiso 1 calc R . H14A H 0.8166(7) 1.0217(6) 0.0026(4) 0.047 Uiso 1 calc R . C15 C 0.8060(7) 0.7694(5) 0.1171(5) 0.0348(14) Uani 1 d . . H15C H 0.7329(7) 0.7591(5) 0.0919(5) 0.052 Uiso 1 calc R . H15B H 0.7893(7) 0.7451(5) 0.1858(5) 0.052 Uiso 1 calc R . H15A H 0.9052(7) 0.7192(5) 0.0754(5) 0.052 Uiso 1 calc R . C16 C 0.6163(6) 1.3115(5) 0.2285(4) 0.0220(11) Uani 1 d . . C17 C 0.4043(6) 1.3645(5) 0.1474(4) 0.0250(12) Uani 1 d . . C18 C 0.7070(6) 1.3287(5) 0.2913(4) 0.0294(13) Uani 1 d . . C19 C 0.7742(8) 1.4208(6) 0.2405(5) 0.043(2) Uani 1 d . . H19C H 0.8380(8) 1.3899(6) 0.1724(5) 0.064 Uiso 1 calc R . H19B H 0.8324(8) 1.4347(6) 0.2779(5) 0.064 Uiso 1 calc R . H19A H 0.6952(8) 1.4969(6) 0.2386(5) 0.064 Uiso 1 calc R . C20 C 0.6081(7) 1.3795(6) 0.3974(5) 0.0364(14) Uani 1 d . . H20C H 0.5639(7) 1.3215(6) 0.4313(5) 0.055 Uiso 1 calc R . H20B H 0.5300(7) 1.4558(6) 0.3947(5) 0.055 Uiso 1 calc R . H20A H 0.6671(7) 1.3936(6) 0.4340(5) 0.055 Uiso 1 calc R . C21 C 0.8290(7) 1.2103(6) 0.2980(5) 0.0371(15) Uani 1 d . . H21C H 0.7848(7) 1.1519(6) 0.3307(5) 0.056 Uiso 1 calc R . H21B H 0.8847(7) 1.2257(6) 0.3367(5) 0.056 Uiso 1 calc R . H21A H 0.8954(7) 1.1778(6) 0.2308(5) 0.056 Uiso 1 calc R . C22 C 0.2575(6) 1.4324(5) 0.1268(4) 0.0270(12) Uani 1 d . . C23 C 0.1757(8) 1.3475(7) 0.1284(6) 0.050(2) Uani 1 d . . H23C H 0.1525(8) 1.3152(7) 0.1943(6) 0.075 Uiso 1 calc R . H23B H 0.2379(8) 1.2808(7) 0.0778(6) 0.075 Uiso 1 calc R . H23A H 0.0841(8) 1.3921(7) 0.1142(6) 0.075 Uiso 1 calc R . C24 C 0.1550(9) 1.5395(7) 0.2023(6) 0.062(2) Uani 1 d . . H24C H 0.2061(9) 1.5948(7) 0.2021(6) 0.094 Uiso 1 calc R . H24B H 0.1271(9) 1.5100(7) 0.2689(6) 0.094 Uiso 1 calc R . H24A H 0.0663(9) 1.5821(7) 0.1841(6) 0.094 Uiso 1 calc R . C25 C 0.2928(8) 1.4818(8) 0.0235(6) 0.057(2) Uani 1 d . . H25C H 0.3454(8) 1.5364(8) 0.0216(6) 0.086 Uiso 1 calc R . H25B H 0.2009(8) 1.5260(8) 0.0095(6) 0.086 Uiso 1 calc R . H25A H 0.3547(8) 1.4148(8) -0.0268(6) 0.086 Uiso 1 calc R . M1 C 0.5419(8) 1.3107(8) 0.1609(6) 0 Uiso 0 d PR . 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 0.0189(5) 0.0196(5) 0.0197(5) 0.0021(4) -0.0043(4) -0.0090(4) P1 0.0202(7) 0.0217(7) 0.0186(7) 0.0015(5) -0.0044(6) -0.0086(6) P2 0.0216(8) 0.0231(7) 0.0188(7) -0.0011(5) -0.0056(6) -0.0085(6) P3 0.0199(7) 0.0245(7) 0.0236(7) 0.0002(6) -0.0060(6) -0.0099(6) P4 0.0228(8) 0.0263(8) 0.0206(7) -0.0007(6) -0.0056(6) -0.0110(6) P5 0.0223(8) 0.0284(8) 0.0233(7) 0.0010(6) -0.0016(6) -0.0118(7) P6 0.0291(8) 0.0275(8) 0.0208(7) 0.0020(6) -0.0061(6) -0.0106(7) P7 0.0247(8) 0.0197(7) 0.0282(8) -0.0016(6) -0.0079(6) -0.0076(6) C1 0.024(3) 0.027(3) 0.019(3) 0.001(2) -0.004(2) -0.015(3) C2 0.020(3) 0.018(3) 0.024(3) 0.003(2) -0.005(2) -0.007(2) C3 0.025(3) 0.030(3) 0.028(3) -0.001(2) -0.004(2) -0.014(3) C4 0.042(4) 0.042(4) 0.039(4) -0.001(3) -0.013(3) -0.028(3) C5 0.044(4) 0.035(4) 0.037(3) 0.009(3) -0.010(3) -0.025(3) C6 0.037(4) 0.017(3) 0.066(5) -0.003(3) -0.009(3) -0.011(3) C7 0.018(3) 0.028(3) 0.029(3) -0.006(2) -0.004(2) -0.003(2) C8 0.036(4) 0.055(4) 0.027(3) -0.009(3) 0.008(3) -0.022(4) C9 0.034(4) 0.034(3) 0.038(3) -0.019(3) -0.006(3) -0.010(3) C10 0.033(4) 0.036(4) 0.049(4) -0.018(3) -0.018(3) 0.006(3) C11 0.028(3) 0.022(3) 0.020(3) 0.003(2) -0.006(2) -0.011(3) C12 0.021(3) 0.030(3) 0.020(3) -0.003(2) -0.001(2) -0.010(3) C13 0.023(3) 0.033(3) 0.032(3) -0.001(3) -0.009(3) -0.003(3) C14 0.033(3) 0.038(3) 0.024(3) -0.004(3) -0.005(3) -0.016(3) C15 0.030(3) 0.028(3) 0.034(3) -0.008(3) 0.001(3) -0.004(3) C16 0.016(3) 0.022(3) 0.025(3) -0.001(2) -0.003(2) -0.005(2) C17 0.022(3) 0.022(3) 0.027(3) 0.002(2) -0.005(2) -0.006(2) C18 0.029(3) 0.031(3) 0.030(3) -0.004(2) -0.007(3) -0.015(3) C19 0.044(4) 0.052(4) 0.049(4) 0.008(3) -0.014(3) -0.036(4) C20 0.030(3) 0.043(4) 0.038(3) -0.008(3) -0.009(3) -0.015(3) C21 0.026(3) 0.042(4) 0.043(4) -0.008(3) -0.018(3) -0.006(3) C22 0.024(3) 0.026(3) 0.032(3) 0.010(2) -0.014(3) -0.007(3) C23 0.043(4) 0.049(4) 0.067(5) 0.015(4) -0.030(4) -0.017(4) C24 0.057(5) 0.046(5) 0.068(5) -0.012(4) -0.035(4) 0.014(4) C25 0.046(5) 0.076(6) 0.054(5) 0.038(4) -0.024(4) -0.024(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C11 2.120(6) . ? Ti M1 2.120(7) . ? Ti C16 2.465(5) . ? Ti P2 2.472(2) . ? Ti C2 2.503(6) . ? Ti P4 2.577(2) . ? Ti P5 2.609(2) . ? Ti P3 2.662(2) . ? Ti C17 2.663(6) . ? Ti P6 2.673(3) . ? Ti P1 2.681(2) . ? Ti P7 2.709(2) . ? P1 C11 1.858(5) . ? P1 C1 1.876(5) . ? P1 P2 2.216(2) . ? P1 P4 2.687(3) . ? P2 C2 1.790(5) . ? P3 C2 1.752(5) . ? P3 C1 1.831(6) . ? P4 C11 1.828(5) . ? P4 C1 1.909(5) . ? P5 M1 1.650(8) . ? P5 C16 1.757(6) . ? P5 P6 2.129(2) . ? P6 M1 1.657(8) . ? P6 C17 1.747(6) . ? P7 M1 1.599(9) . ? P7 C17 1.741(6) . ? P7 C16 1.751(6) . ? C1 C3 1.528(7) . ? C2 C7 1.534(8) . ? C3 C6 1.520(8) . ? C3 C5 1.526(8) . ? C3 C4 1.544(8) . ? C7 C10 1.524(8) . ? C7 C9 1.527(7) . ? C7 C8 1.529(8) . ? C11 C12 1.539(8) . ? C12 C13 1.530(7) . ? C12 C14 1.533(8) . ? C12 C15 1.547(8) . ? C16 M1 1.414(9) . ? C16 C18 1.555(7) . ? C17 M1 1.400(9) . ? C17 C22 1.549(7) . ? C18 C19 1.527(8) . ? C18 C20 1.532(8) . ? C18 C21 1.534(8) . ? C22 C23 1.528(8) . ? C22 C25 1.530(8) . ? C22 C24 1.533(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 C11 Ti M1 120.9(3) . . ? C11 Ti C16 119.2(2) . . ? M1 Ti C16 34.9(2) . . ? C11 Ti P2 90.8(2) . . ? M1 Ti P2 130.3(2) . . ? C16 Ti P2 97.58(13) . . ? C11 Ti C2 112.3(2) . . ? M1 Ti C2 126.6(3) . . ? C16 Ti C2 113.6(2) . . ? P2 Ti C2 42.17(12) . . ? C11 Ti P4 44.51(14) . . ? M1 Ti P4 121.3(2) . . ? C16 Ti P4 148.25(14) . . ? P2 Ti P4 108.27(7) . . ? C2 Ti P4 98.06(13) . . ? C11 Ti P5 85.5(2) . . ? M1 Ti P5 39.1(2) . . ? C16 Ti P5 40.39(13) . . ? P2 Ti P5 122.26(7) . . ? C2 Ti P5 153.41(12) . . ? P4 Ti P5 108.33(8) . . ? C11 Ti P3 95.0(2) . . ? M1 Ti P3 131.8(2) . . ? C16 Ti P3 145.22(14) . . ? P2 Ti P3 74.01(7) . . ? C2 Ti P3 39.52(12) . . ? P4 Ti P3 62.60(7) . . ? P5 Ti P3 163.73(6) . . ? C11 Ti C17 132.0(2) . . ? M1 Ti C17 31.5(2) . . ? C16 Ti C17 62.2(2) . . ? P2 Ti C17 137.08(14) . . ? C2 Ti C17 108.4(2) . . ? P4 Ti C17 106.20(13) . . ? P5 Ti C17 67.79(13) . . ? P3 Ti C17 100.72(13) . . ? C11 Ti P6 94.4(2) . . ? M1 Ti P6 38.3(2) . . ? C16 Ti P6 70.29(13) . . ? P2 Ti P6 167.84(6) . . ? C2 Ti P6 142.89(13) . . ? P4 Ti P6 82.99(7) . . ? P5 Ti P6 47.51(6) . . ? P3 Ti P6 116.35(7) . . ? C17 Ti P6 38.22(13) . . ? C11 Ti P1 43.60(14) . . ? M1 Ti P1 158.5(2) . . ? C16 Ti P1 131.03(13) . . ? P2 Ti P1 50.73(6) . . ? C2 Ti P1 70.29(13) . . ? P4 Ti P1 61.43(6) . . ? P5 Ti P1 119.64(7) . . ? P3 Ti P1 69.43(6) . . ? C17 Ti P1 166.52(12) . . ? P6 Ti P1 137.10(7) . . ? C11 Ti P7 155.55(15) . . ? M1 Ti P7 36.2(2) . . ? C16 Ti P7 39.19(13) . . ? P2 Ti P7 102.16(8) . . ? C2 Ti P7 90.78(14) . . ? P4 Ti P7 143.26(6) . . ? P5 Ti P7 70.10(7) . . ? P3 Ti P7 108.41(7) . . ? C17 Ti P7 37.82(12) . . ? P6 Ti P7 69.20(7) . . ? P1 Ti P7 152.83(6) . . ? C11 P1 C1 88.0(2) . . ? C11 P1 P2 106.9(2) . . ? C1 P1 P2 103.2(2) . . ? C11 P1 Ti 51.9(2) . . ? C1 P1 Ti 79.6(2) . . ? P2 P1 Ti 59.74(7) . . ? C11 P1 P4 42.8(2) . . ? C1 P1 P4 45.3(2) . . ? P2 P1 P4 112.80(8) . . ? Ti P1 P4 57.37(6) . . ? C2 P2 P1 95.9(2) . . ? C2 P2 Ti 69.8(2) . . ? P1 P2 Ti 69.53(7) . . ? C2 P3 C1 104.4(2) . . ? C2 P3 Ti 65.3(2) . . ? C1 P3 Ti 80.9(2) . . ? C11 P4 C1 87.9(2) . . ? C11 P4 Ti 54.4(2) . . ? C1 P4 Ti 81.9(2) . . ? C11 P4 P1 43.6(2) . . ? C1 P4 P1 44.3(2) . . ? Ti P4 P1 61.20(6) . . ? M1 P5 C16 48.9(3) . . ? M1 P5 P6 50.1(3) . . ? C16 P5 P6 98.9(2) . . ? M1 P5 Ti 54.2(2) . . ? C16 P5 Ti 65.4(2) . . ? P6 P5 Ti 67.84(7) . . ? M1 P6 C17 48.5(3) . . ? M1 P6 P5 49.8(3) . . ? C17 P6 P5 98.2(2) . . ? M1 P6 Ti 52.5(2) . . ? C17 P6 Ti 70.6(2) . . ? P5 P6 Ti 64.65(7) . . ? M1 P7 C17 49.3(3) . . ? M1 P7 C16 49.7(3) . . ? C17 P7 C16 99.0(3) . . ? M1 P7 Ti 51.5(3) . . ? C17 P7 Ti 69.7(2) . . ? C16 P7 Ti 62.9(2) . . ? C3 C1 P3 117.0(4) . . ? C3 C1 P1 118.3(4) . . ? P3 C1 P1 110.4(3) . . ? C3 C1 P4 122.3(4) . . ? P3 C1 P4 93.4(2) . . ? P1 C1 P4 90.5(2) . . ? C7 C2 P3 118.7(4) . . ? C7 C2 P2 118.9(4) . . ? P3 C2 P2 121.7(3) . . ? C7 C2 Ti 138.5(3) . . ? P3 C2 Ti 75.2(2) . . ? P2 C2 Ti 68.0(2) . . ? C6 C3 C5 109.1(5) . . ? C6 C3 C1 110.3(5) . . ? C5 C3 C1 109.4(4) . . ? C6 C3 C4 108.4(5) . . ? C5 C3 C4 110.2(5) . . ? C1 C3 C4 109.5(5) . . ? C10 C7 C9 108.8(5) . . ? C10 C7 C8 108.6(5) . . ? C9 C7 C8 108.4(5) . . ? C10 C7 C2 112.2(5) . . ? C9 C7 C2 113.6(4) . . ? C8 C7 C2 105.1(5) . . ? C12 C11 P4 122.1(4) . . ? C12 C11 P1 119.1(4) . . ? P4 C11 P1 93.6(2) . . ? C12 C11 Ti 142.5(4) . . ? P4 C11 Ti 81.1(2) . . ? P1 C11 Ti 84.5(2) . . ? C13 C12 C14 110.2(4) . . ? C13 C12 C11 111.8(4) . . ? C14 C12 C11 109.9(5) . . ? C13 C12 C15 107.3(5) . . ? C14 C12 C15 108.3(4) . . ? C11 C12 C15 109.3(4) . . ? M1 C16 C18 170.1(5) . . ? M1 C16 P7 59.6(4) . . ? C18 C16 P7 120.7(4) . . ? M1 C16 P5 61.6(4) . . ? C18 C16 P5 116.8(4) . . ? P7 C16 P5 121.1(3) . . ? M1 C16 Ti 59.1(3) . . ? C18 C16 Ti 130.7(4) . . ? P7 C16 Ti 77.9(2) . . ? P5 C16 Ti 74.2(2) . . ? M1 C17 C22 174.8(5) . . ? M1 C17 P7 60.0(4) . . ? C22 C17 P7 120.3(4) . . ? M1 C17 P6 62.4(4) . . ? C22 C17 P6 117.2(4) . . ? P7 C17 P6 122.4(3) . . ? M1 C17 Ti 52.3(3) . . ? C22 C17 Ti 132.9(3) . . ? P7 C17 Ti 72.5(2) . . ? P6 C17 Ti 71.2(2) . . ? C19 C18 C20 108.2(5) . . ? C19 C18 C21 110.1(5) . . ? C20 C18 C21 108.2(5) . . ? C19 C18 C16 106.6(5) . . ? C20 C18 C16 111.3(5) . . ? C21 C18 C16 112.3(4) . . ? C23 C22 C25 108.8(5) . . ? C23 C22 C24 108.5(6) . . ? C25 C22 C24 107.7(6) . . ? C23 C22 C17 110.9(5) . . ? C25 C22 C17 108.4(5) . . ? C24 C22 C17 112.4(5) . . ? C17 M1 C16 141.3(8) . . ? C17 M1 P7 70.6(4) . . ? C16 M1 P7 70.7(4) . . ? C17 M1 P5 149.1(6) . . ? C16 M1 P5 69.5(4) . . ? P7 M1 P5 140.2(5) . . ? C17 M1 P6 69.1(4) . . ? C16 M1 P6 149.5(7) . . ? P7 M1 P6 139.7(5) . . ? P5 M1 P6 80.1(4) . . ? C17 M1 Ti 96.1(4) . . ? C16 M1 Ti 86.0(4) . . ? P7 M1 Ti 92.4(3) . . ? P5 M1 Ti 86.6(3) . . ? P6 M1 Ti 89.2(4) . . ?