data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Douglas Stephan' _publ_contact_author_email dstephan@chem.utoronto.ca _publ_author_name 'Douglas Stephan' data_(C5Me4HSiMe2N(H)C6H4Ph) _database_code_depnum_ccdc_archive 'CCDC 808875' #TrackingRef '- all-cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H29 N Si' _chemical_formula_weight 347.56 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3969(19) _cell_length_b 10.297(2) _cell_length_c 12.440(3) _cell_angle_alpha 68.91(3) _cell_angle_beta 82.78(3) _cell_angle_gamma 64.73(3) _cell_volume 1015.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5043 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colour _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.137 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 376 _exptl_absorpt_coefficient_mu 0.121 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.845 _exptl_absorpt_correction_T_max 0.993 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10726 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0555 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 27.51 _reflns_number_total 4542 _reflns_number_gt 3144 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1026P)^2^+0.2068P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4542 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0929 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1891 _refine_ls_wR_factor_gt 0.1644 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _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 Si1 Si 0.27301(7) 0.06069(7) 0.29135(5) 0.0338(2) Uani 1 1 d . . . N1 N 0.1094(2) 0.05776(19) 0.24379(17) 0.0344(4) Uani 1 1 d . . . H1A H 0.1112 -0.0340 0.2630 0.041 Uiso 1 1 calc R . . C1 C -0.0243(2) 0.1753(2) 0.18061(19) 0.0294(5) Uani 1 1 d . . . C2 C -0.1391(2) 0.1457(2) 0.14173(18) 0.0287(5) Uani 1 1 d . . . C7 C -0.1257(2) -0.0130(2) 0.17095(19) 0.0286(5) Uani 1 1 d . . . C12 C -0.1237(2) -0.0709(2) 0.0852(2) 0.0323(5) Uani 1 1 d . . . H12A H -0.1311 -0.0082 0.0066 0.039 Uiso 1 1 calc R . . C6 C -0.0462(2) 0.3277(2) 0.1497(2) 0.0328(5) Uani 1 1 d . . . H6A H 0.0285 0.3499 0.1763 0.039 Uiso 1 1 calc R . . C5 C -0.1733(3) 0.4462(2) 0.0819(2) 0.0354(5) Uani 1 1 d . . . H5A H -0.1856 0.5485 0.0629 0.043 Uiso 1 1 calc R . . C3 C -0.2651(2) 0.2682(2) 0.0716(2) 0.0351(5) Uani 1 1 d . . . H3A H -0.3406 0.2482 0.0439 0.042 Uiso 1 1 calc R . . C13 C 0.4046(3) -0.1499(2) 0.3585(2) 0.0352(5) Uani 1 1 d . . . H13A H 0.5109 -0.1629 0.3782 0.042 Uiso 1 1 calc R . . C11 C -0.1110(3) -0.2184(3) 0.1126(2) 0.0391(6) Uani 1 1 d . . . H11A H -0.1074 -0.2564 0.0527 0.047 Uiso 1 1 calc R . . C4 C -0.2836(3) 0.4174(2) 0.0410(2) 0.0389(6) Uani 1 1 d . . . H4A H -0.3702 0.4989 -0.0071 0.047 Uiso 1 1 calc R . . C17 C 0.4199(2) -0.2332(3) 0.2770(2) 0.0380(5) Uani 1 1 d . . . C10 C -0.1035(3) -0.3105(2) 0.2261(2) 0.0381(5) Uani 1 1 d . . . H10A H -0.0950 -0.4115 0.2445 0.046 Uiso 1 1 calc R . . C8 C -0.1161(3) -0.1083(2) 0.2857(2) 0.0358(5) Uani 1 1 d . . . H8A H -0.1147 -0.0726 0.3460 0.043 Uiso 1 1 calc R . . C16 C 0.3592(3) -0.3374(3) 0.3256(2) 0.0424(6) Uani 1 1 d . . . C9 C -0.1085(3) -0.2543(3) 0.3127(2) 0.0398(5) Uani 1 1 d . . . H9A H -0.1067 -0.3158 0.3911 0.048 Uiso 1 1 calc R . . C14 C 0.3371(3) -0.2310(3) 0.4637(2) 0.0396(6) Uani 1 1 d . . . C15 C 0.3089(3) -0.3368(3) 0.4417(2) 0.0427(6) Uani 1 1 d . . . C22 C 0.3738(3) 0.1573(3) 0.1729(3) 0.0553(7) Uani 1 1 d . . . H22A H 0.3038 0.2657 0.1392 0.083 Uiso 1 1 calc R . . H22B H 0.4005 0.1096 0.1135 0.083 Uiso 1 1 calc R . . H22C H 0.4704 0.1474 0.2037 0.083 Uiso 1 1 calc R . . C21 C 0.4857(3) -0.1967(3) 0.1592(2) 0.0517(7) Uani 1 1 d . . . H21A H 0.4846 -0.2657 0.1222 0.078 Uiso 1 1 calc R . . H21B H 0.5942 -0.2096 0.1658 0.078 Uiso 1 1 calc R . . H21C H 0.4214 -0.0908 0.1126 0.078 Uiso 1 1 calc R . . C18 C 0.3069(4) -0.1965(3) 0.5735(2) 0.0611(8) Uani 1 1 d . . . H18A H 0.2631 -0.2641 0.6292 0.092 Uiso 1 1 calc R . . H18B H 0.2319 -0.0899 0.5581 0.092 Uiso 1 1 calc R . . H18C H 0.4060 -0.2128 0.6052 0.092 Uiso 1 1 calc R . . C20 C 0.3445(3) -0.4412(3) 0.2729(3) 0.0631(8) Uani 1 1 d . . . H20A H 0.3859 -0.4219 0.1951 0.095 Uiso 1 1 calc R . . H20B H 0.2333 -0.4217 0.2687 0.095 Uiso 1 1 calc R . . H20C H 0.4044 -0.5477 0.3204 0.095 Uiso 1 1 calc R . . C19 C 0.2428(3) -0.4435(3) 0.5221(3) 0.0620(8) Uani 1 1 d . . . H19A H 0.2171 -0.4222 0.5946 0.093 Uiso 1 1 calc R . . H19B H 0.3208 -0.5491 0.5377 0.093 Uiso 1 1 calc R . . H19C H 0.1472 -0.4293 0.4869 0.093 Uiso 1 1 calc R . . C23 C 0.2187(3) 0.1654(3) 0.3958(2) 0.0524(7) Uani 1 1 d . . . H23A H 0.1506 0.2732 0.3566 0.079 Uiso 1 1 calc R . . H23B H 0.3144 0.1578 0.4261 0.079 Uiso 1 1 calc R . . H23C H 0.1626 0.1204 0.4595 0.079 Uiso 1 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 Si1 0.0372(4) 0.0320(3) 0.0316(4) -0.0044(3) -0.0034(3) -0.0179(3) N1 0.0356(10) 0.0241(9) 0.0430(12) -0.0081(8) -0.0062(8) -0.0127(7) C1 0.0309(10) 0.0275(10) 0.0305(12) -0.0112(9) 0.0041(8) -0.0123(8) C2 0.0308(10) 0.0279(10) 0.0306(12) -0.0120(9) 0.0067(8) -0.0150(8) C7 0.0271(10) 0.0287(10) 0.0321(12) -0.0109(9) 0.0043(8) -0.0140(8) C12 0.0336(11) 0.0358(11) 0.0346(12) -0.0131(10) 0.0068(9) -0.0213(9) C6 0.0350(11) 0.0308(11) 0.0380(13) -0.0147(10) 0.0016(9) -0.0163(9) C5 0.0394(12) 0.0228(10) 0.0439(14) -0.0107(9) 0.0025(10) -0.0135(9) C3 0.0309(11) 0.0348(11) 0.0412(14) -0.0113(10) 0.0002(9) -0.0161(9) C13 0.0341(11) 0.0356(11) 0.0312(12) -0.0063(10) -0.0008(9) -0.0138(9) C11 0.0441(13) 0.0430(13) 0.0460(15) -0.0244(12) 0.0117(10) -0.0274(10) C4 0.0330(11) 0.0292(11) 0.0509(16) -0.0098(10) -0.0018(10) -0.0119(9) C17 0.0277(11) 0.0390(12) 0.0387(14) -0.0124(10) -0.0017(9) -0.0061(9) C10 0.0398(12) 0.0279(11) 0.0518(16) -0.0146(10) 0.0065(10) -0.0192(9) C8 0.0472(13) 0.0316(11) 0.0334(13) -0.0118(10) 0.0050(10) -0.0209(10) C16 0.0308(11) 0.0339(12) 0.0559(17) -0.0139(11) -0.0032(10) -0.0073(9) C9 0.0484(13) 0.0343(12) 0.0379(14) -0.0062(10) 0.0012(10) -0.0231(10) C14 0.0426(13) 0.0319(11) 0.0291(13) -0.0016(10) 0.0018(10) -0.0091(9) C15 0.0342(12) 0.0287(11) 0.0498(16) -0.0017(10) -0.0007(10) -0.0082(9) C22 0.0526(15) 0.0494(15) 0.0562(18) 0.0030(13) -0.0008(13) -0.0306(13) C21 0.0397(14) 0.0643(17) 0.0420(16) -0.0202(13) 0.0066(11) -0.0130(12) C18 0.080(2) 0.0478(15) 0.0346(16) -0.0056(12) 0.0043(14) -0.0151(14) C20 0.0551(17) 0.0497(16) 0.088(2) -0.0333(16) -0.0062(15) -0.0141(13) C19 0.0479(15) 0.0399(14) 0.076(2) 0.0050(14) 0.0038(14) -0.0189(12) C23 0.0757(18) 0.0361(13) 0.0447(16) -0.0093(12) -0.0152(13) -0.0214(12) _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 Si1 N1 1.7312(19) . ? Si1 C22 1.859(3) . ? Si1 C23 1.867(3) . ? Si1 C13 1.896(2) . ? N1 C1 1.388(3) . ? C1 C6 1.401(3) . ? C1 C2 1.418(3) . ? C2 C3 1.395(3) . ? C2 C7 1.492(3) . ? C7 C12 1.391(3) . ? C7 C8 1.399(3) . ? C12 C11 1.386(3) . ? C6 C5 1.377(3) . ? C5 C4 1.387(3) . ? C3 C4 1.380(3) . ? C13 C14 1.506(3) . ? C13 C17 1.507(3) . ? C11 C10 1.379(3) . ? C17 C16 1.345(3) . ? C17 C21 1.499(4) . ? C10 C9 1.383(3) . ? C8 C9 1.389(3) . ? C16 C15 1.463(4) . ? C16 C20 1.499(4) . ? C14 C15 1.347(3) . ? C14 C18 1.497(4) . ? C15 C19 1.493(3) . ? 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 Si1 C22 113.10(12) . . ? N1 Si1 C23 111.32(11) . . ? C22 Si1 C23 106.10(14) . . ? N1 Si1 C13 102.74(10) . . ? C22 Si1 C13 110.75(12) . . ? C23 Si1 C13 113.01(11) . . ? C1 N1 Si1 131.04(14) . . ? N1 C1 C6 120.35(19) . . ? N1 C1 C2 121.57(18) . . ? C6 C1 C2 118.04(19) . . ? C3 C2 C1 118.82(19) . . ? C3 C2 C7 119.47(18) . . ? C1 C2 C7 121.69(19) . . ? C12 C7 C8 117.74(19) . . ? C12 C7 C2 121.2(2) . . ? C8 C7 C2 121.0(2) . . ? C11 C12 C7 121.1(2) . . ? C5 C6 C1 121.6(2) . . ? C6 C5 C4 120.50(19) . . ? C4 C3 C2 122.2(2) . . ? C14 C13 C17 103.10(19) . . ? C14 C13 Si1 113.33(16) . . ? C17 C13 Si1 110.41(15) . . ? C10 C11 C12 120.6(2) . . ? C3 C4 C5 118.8(2) . . ? C16 C17 C21 127.2(2) . . ? C16 C17 C13 108.9(2) . . ? C21 C17 C13 123.9(2) . . ? C11 C10 C9 119.3(2) . . ? C9 C8 C7 120.9(2) . . ? C17 C16 C15 109.5(2) . . ? C17 C16 C20 126.9(3) . . ? C15 C16 C20 123.6(2) . . ? C10 C9 C8 120.3(2) . . ? C15 C14 C18 126.6(2) . . ? C15 C14 C13 108.9(2) . . ? C18 C14 C13 124.5(2) . . ? C14 C15 C16 109.4(2) . . ? C14 C15 C19 126.8(3) . . ? C16 C15 C19 123.7(2) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.396 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.059 #===end data_C5Me4(SiMe2NCMe2Ph)Ti(NMe2)2 _database_code_depnum_ccdc_archive 'CCDC 808876' #TrackingRef '- all-cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H41 N3 Si Ti' _chemical_formula_weight 447.59 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' 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 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 8.9918(18) _cell_length_b 32.057(6) _cell_length_c 9.6600(19) _cell_angle_alpha 90.00 _cell_angle_beta 117.73(3) _cell_angle_gamma 90.00 _cell_volume 2464.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.206 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 0.411 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.801 _exptl_absorpt_correction_T_max 0.978 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22417 _diffrn_reflns_av_R_equivalents 0.0799 _diffrn_reflns_av_sigmaI/netI 0.0947 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5597 _reflns_number_gt 3256 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0811P)^2^+0.0073P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5597 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1204 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1575 _refine_ls_wR_factor_gt 0.1273 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.17995(6) 0.110881(16) 0.66145(6) 0.02751(17) Uani 1 1 d . . . Si2 Si 0.16279(10) 0.09453(3) 0.35824(9) 0.0304(2) Uani 1 1 d . . . N2 N 0.0680(3) 0.14677(7) 0.7460(3) 0.0325(6) Uani 1 1 d . . . N1 N 0.1849(3) 0.13691(7) 0.4772(3) 0.0292(6) Uani 1 1 d . . . N3 N 0.4094(3) 0.11843(7) 0.8150(3) 0.0341(6) Uani 1 1 d . . . C13 C 0.2315(3) 0.03943(9) 0.6258(3) 0.0302(7) Uani 1 1 d . . . C14 C 0.1584(4) 0.03660(9) 0.7258(3) 0.0314(7) Uani 1 1 d . . . C12 C 0.1119(3) 0.05788(9) 0.4796(3) 0.0281(7) Uani 1 1 d . . . C23 C 0.4618(4) 0.10530(10) 0.9767(4) 0.0459(9) Uani 1 1 d . . . H23A H 0.5273 0.1270 1.0472 0.069 Uiso 1 1 calc R . . H23B H 0.5280 0.0804 0.9988 0.069 Uiso 1 1 calc R . . H23C H 0.3641 0.0999 0.9901 0.069 Uiso 1 1 calc R . . C4 C 0.0148(4) 0.19496(9) 0.3110(3) 0.0351(7) Uani 1 1 d . . . C1 C 0.1916(4) 0.18131(9) 0.4332(3) 0.0331(7) Uani 1 1 d . . . C16 C -0.0401(3) 0.06390(9) 0.4944(3) 0.0307(7) Uani 1 1 d . . . C21 C 0.1582(4) 0.17672(10) 0.8719(4) 0.0423(8) Uani 1 1 d . . . H21A H 0.1113 0.2040 0.8387 0.063 Uiso 1 1 calc R . . H21B H 0.2747 0.1770 0.8968 0.063 Uiso 1 1 calc R . . H21C H 0.1477 0.1688 0.9628 0.063 Uiso 1 1 calc R . . C11 C 0.3570(4) 0.07923(11) 0.3447(4) 0.0444(8) Uani 1 1 d . . . H11A H 0.3677 0.0964 0.2683 0.067 Uiso 1 1 calc R . . H11B H 0.3491 0.0505 0.3142 0.067 Uiso 1 1 calc R . . H11C H 0.4537 0.0830 0.4447 0.067 Uiso 1 1 calc R . . C15 C -0.0104(4) 0.05102(9) 0.6439(3) 0.0310(7) Uani 1 1 d . . . C18 C 0.2309(4) 0.01683(10) 0.8857(4) 0.0424(8) Uani 1 1 d . . . H18A H 0.1845 -0.0106 0.8772 0.064 Uiso 1 1 calc R . . H18B H 0.2037 0.0336 0.9530 0.064 Uiso 1 1 calc R . . H18C H 0.3508 0.0149 0.9286 0.064 Uiso 1 1 calc R . . C17 C 0.4066(4) 0.02452(10) 0.6654(4) 0.0390(8) Uani 1 1 d . . . H17A H 0.3991 0.0002 0.6047 0.059 Uiso 1 1 calc R . . H17B H 0.4664 0.0178 0.7747 0.059 Uiso 1 1 calc R . . H17C H 0.4653 0.0462 0.6420 0.059 Uiso 1 1 calc R . . C9 C -0.0226(4) 0.21044(9) 0.1641(4) 0.0439(8) Uani 1 1 d . . . H9A H 0.0624 0.2133 0.1357 0.053 Uiso 1 1 calc R . . C5 C -0.1175(4) 0.19152(10) 0.3476(4) 0.0410(8) Uani 1 1 d . . . H5A H -0.0960 0.1813 0.4452 0.049 Uiso 1 1 calc R . . C19 C -0.1338(4) 0.04658(10) 0.7069(4) 0.0404(8) Uani 1 1 d . . . H19A H -0.1572 0.0176 0.7121 0.061 Uiso 1 1 calc R . . H19B H -0.2360 0.0608 0.6393 0.061 Uiso 1 1 calc R . . H19C H -0.0873 0.0585 0.8098 0.061 Uiso 1 1 calc R . . C24 C 0.5565(4) 0.12699(11) 0.7947(4) 0.0431(8) Uani 1 1 d . . . H24A H 0.6194 0.1494 0.8627 0.065 Uiso 1 1 calc R . . H24B H 0.5219 0.1348 0.6881 0.065 Uiso 1 1 calc R . . H24C H 0.6255 0.1025 0.8199 0.065 Uiso 1 1 calc R . . C10 C -0.0022(4) 0.09843(10) 0.1493(3) 0.0407(8) Uani 1 1 d . . . H10A H 0.0338 0.1177 0.0949 0.061 Uiso 1 1 calc R . . H10B H -0.1053 0.1081 0.1450 0.061 Uiso 1 1 calc R . . H10C H -0.0198 0.0715 0.1009 0.061 Uiso 1 1 calc R . . C2 C 0.2509(4) 0.20984(9) 0.5770(4) 0.0403(8) Uani 1 1 d . . . H2A H 0.1742 0.2078 0.6201 0.061 Uiso 1 1 calc R . . H2B H 0.2548 0.2382 0.5466 0.061 Uiso 1 1 calc R . . H2C H 0.3610 0.2014 0.6542 0.061 Uiso 1 1 calc R . . C20 C -0.2042(3) 0.08002(10) 0.3672(3) 0.0365(7) Uani 1 1 d . . . H20A H -0.2435 0.0617 0.2784 0.055 Uiso 1 1 calc R . . H20B H -0.1880 0.1075 0.3370 0.055 Uiso 1 1 calc R . . H20C H -0.2857 0.0811 0.4051 0.055 Uiso 1 1 calc R . . C3 C 0.3193(4) 0.18562(10) 0.3691(4) 0.0434(8) Uani 1 1 d . . . H3A H 0.4279 0.1765 0.4471 0.065 Uiso 1 1 calc R . . H3B H 0.3254 0.2143 0.3433 0.065 Uiso 1 1 calc R . . H3C H 0.2839 0.1687 0.2771 0.065 Uiso 1 1 calc R . . C22 C -0.1105(4) 0.14958(10) 0.7030(4) 0.0435(8) Uani 1 1 d . . . H22A H -0.1488 0.1776 0.6719 0.065 Uiso 1 1 calc R . . H22B H -0.1269 0.1420 0.7911 0.065 Uiso 1 1 calc R . . H22C H -0.1732 0.1309 0.6177 0.065 Uiso 1 1 calc R . . C6 C -0.2806(4) 0.20297(10) 0.2424(4) 0.0505(9) Uani 1 1 d . . . H6A H -0.3663 0.2004 0.2701 0.061 Uiso 1 1 calc R . . C8 C -0.1877(5) 0.22180(10) 0.0583(4) 0.0593(11) Uani 1 1 d . . . H8A H -0.2107 0.2320 -0.0398 0.071 Uiso 1 1 calc R . . C7 C -0.3150(5) 0.21812(11) 0.0968(4) 0.0580(11) Uani 1 1 d . . . H7A H -0.4239 0.2257 0.0257 0.070 Uiso 1 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 Ti1 0.0259(3) 0.0321(3) 0.0243(3) -0.0010(2) 0.0114(2) -0.0001(2) Si2 0.0303(4) 0.0352(5) 0.0272(4) -0.0012(4) 0.0147(4) 0.0011(4) N2 0.0354(13) 0.0352(14) 0.0312(14) -0.0022(11) 0.0191(11) -0.0011(11) N1 0.0281(12) 0.0331(14) 0.0265(13) 0.0030(10) 0.0128(10) 0.0012(11) N3 0.0277(12) 0.0402(15) 0.0303(14) -0.0003(11) 0.0099(11) 0.0015(11) C13 0.0310(15) 0.0270(16) 0.0308(16) 0.0021(13) 0.0129(13) 0.0012(13) C14 0.0350(16) 0.0275(16) 0.0312(16) 0.0030(13) 0.0149(13) -0.0003(13) C12 0.0307(15) 0.0297(16) 0.0265(15) -0.0031(12) 0.0154(13) -0.0009(13) C23 0.0382(18) 0.055(2) 0.0318(18) 0.0014(15) 0.0055(14) -0.0056(16) C4 0.0453(18) 0.0267(16) 0.0309(17) -0.0004(13) 0.0158(14) 0.0020(14) C1 0.0406(17) 0.0327(17) 0.0308(16) 0.0001(13) 0.0208(14) -0.0010(14) C16 0.0297(15) 0.0304(16) 0.0293(16) -0.0038(13) 0.0116(13) -0.0030(13) C21 0.052(2) 0.0445(19) 0.0370(18) -0.0045(15) 0.0263(16) -0.0018(16) C11 0.0469(19) 0.050(2) 0.045(2) 0.0043(16) 0.0291(17) 0.0054(16) C15 0.0317(15) 0.0332(17) 0.0286(16) -0.0059(13) 0.0147(13) -0.0052(13) C18 0.0458(19) 0.0407(19) 0.0417(19) 0.0075(15) 0.0211(16) 0.0028(16) C17 0.0369(17) 0.0387(18) 0.0431(19) 0.0044(15) 0.0200(15) 0.0064(15) C9 0.058(2) 0.0370(18) 0.0342(19) 0.0013(14) 0.0195(16) -0.0039(16) C5 0.0454(18) 0.0405(19) 0.0360(18) -0.0001(15) 0.0180(15) 0.0060(16) C19 0.0409(18) 0.0460(19) 0.0372(18) -0.0029(15) 0.0207(15) -0.0059(15) C24 0.0285(16) 0.057(2) 0.043(2) -0.0046(17) 0.0157(15) -0.0028(15) C10 0.0503(19) 0.0441(19) 0.0300(17) 0.0008(14) 0.0206(15) -0.0032(16) C2 0.0484(19) 0.0366(18) 0.0347(18) -0.0007(14) 0.0182(15) -0.0040(15) C20 0.0285(15) 0.0457(19) 0.0321(17) -0.0059(14) 0.0114(13) -0.0025(14) C3 0.050(2) 0.043(2) 0.0444(19) -0.0002(16) 0.0279(16) -0.0070(16) C22 0.0486(19) 0.0430(19) 0.049(2) 0.0025(16) 0.0307(17) 0.0062(16) C6 0.045(2) 0.048(2) 0.053(2) -0.0062(18) 0.0180(17) 0.0050(17) C8 0.082(3) 0.041(2) 0.035(2) 0.0068(17) 0.010(2) -0.003(2) C7 0.053(2) 0.047(2) 0.049(2) 0.0025(18) 0.0034(19) 0.0115(18) _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 N3 1.915(2) . ? Ti1 N2 1.942(2) . ? Ti1 N1 1.985(2) . ? Ti1 C12 2.312(3) . ? Ti1 C13 2.393(3) . ? Ti1 C16 2.412(3) . ? Ti1 C14 2.491(3) . ? Ti1 C15 2.524(3) . ? Ti1 Si2 2.9082(11) . ? Si2 N1 1.730(2) . ? Si2 C12 1.861(3) . ? Si2 C10 1.872(3) . ? Si2 C11 1.876(3) . ? N2 C22 1.462(4) . ? N2 C21 1.463(4) . ? N1 C1 1.494(4) . ? N3 C24 1.451(4) . ? N3 C23 1.468(4) . ? C13 C14 1.401(4) . ? C13 C12 1.444(4) . ? C13 C17 1.514(4) . ? C14 C15 1.423(4) . ? C14 C18 1.509(4) . ? C12 C16 1.452(4) . ? C4 C9 1.388(4) . ? C4 C5 1.394(4) . ? C4 C1 1.538(4) . ? C1 C2 1.537(4) . ? C1 C3 1.543(4) . ? C16 C15 1.403(4) . ? C16 C20 1.506(4) . ? C15 C19 1.501(4) . ? C9 C8 1.404(5) . ? C5 C6 1.389(4) . ? C6 C7 1.381(5) . ? C8 C7 1.363(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 N3 Ti1 N2 100.48(10) . . ? N3 Ti1 N1 100.13(10) . . ? N2 Ti1 N1 111.14(10) . . ? N3 Ti1 C12 119.35(10) . . ? N2 Ti1 C12 138.53(10) . . ? N1 Ti1 C12 74.69(10) . . ? N3 Ti1 C13 91.23(10) . . ? N2 Ti1 C13 143.19(10) . . ? N1 Ti1 C13 100.75(10) . . ? C12 Ti1 C13 35.70(9) . . ? N3 Ti1 C16 148.21(10) . . ? N2 Ti1 C16 103.11(10) . . ? N1 Ti1 C16 90.94(10) . . ? C12 Ti1 C16 35.73(10) . . ? C13 Ti1 C16 57.28(9) . . ? N3 Ti1 C14 96.22(10) . . ? N2 Ti1 C14 110.23(10) . . ? N1 Ti1 C14 131.47(10) . . ? C12 Ti1 C14 57.54(10) . . ? C13 Ti1 C14 33.26(10) . . ? C16 Ti1 C14 55.60(10) . . ? N3 Ti1 C15 126.91(10) . . ? N2 Ti1 C15 90.61(10) . . ? N1 Ti1 C15 123.83(9) . . ? C12 Ti1 C15 57.24(10) . . ? C13 Ti1 C15 55.48(10) . . ? C16 Ti1 C15 32.92(9) . . ? C14 Ti1 C15 32.96(9) . . ? N3 Ti1 Si2 109.64(8) . . ? N2 Ti1 Si2 137.36(7) . . ? N1 Ti1 Si2 35.46(7) . . ? C12 Ti1 Si2 39.74(7) . . ? C13 Ti1 Si2 66.77(7) . . ? C16 Ti1 Si2 64.60(7) . . ? C14 Ti1 Si2 96.03(7) . . ? C15 Ti1 Si2 94.51(7) . . ? N1 Si2 C12 93.63(12) . . ? N1 Si2 C10 116.88(13) . . ? C12 Si2 C10 114.68(14) . . ? N1 Si2 C11 115.36(14) . . ? C12 Si2 C11 112.86(14) . . ? C10 Si2 C11 103.83(15) . . ? N1 Si2 Ti1 41.73(8) . . ? C12 Si2 Ti1 52.60(9) . . ? C10 Si2 Ti1 135.87(11) . . ? C11 Si2 Ti1 120.16(11) . . ? C22 N2 C21 107.8(2) . . ? C22 N2 Ti1 129.3(2) . . ? C21 N2 Ti1 122.88(19) . . ? C1 N1 Si2 124.51(18) . . ? C1 N1 Ti1 132.52(18) . . ? Si2 N1 Ti1 102.82(11) . . ? C24 N3 C23 109.7(2) . . ? C24 N3 Ti1 129.8(2) . . ? C23 N3 Ti1 119.0(2) . . ? C14 C13 C12 109.0(2) . . ? C14 C13 C17 124.8(3) . . ? C12 C13 C17 126.1(3) . . ? C14 C13 Ti1 77.20(17) . . ? C12 C13 Ti1 69.09(15) . . ? C17 C13 Ti1 120.91(19) . . ? C13 C14 C15 108.5(3) . . ? C13 C14 C18 128.0(3) . . ? C15 C14 C18 123.1(3) . . ? C13 C14 Ti1 69.54(16) . . ? C15 C14 Ti1 74.78(16) . . ? C18 C14 Ti1 127.6(2) . . ? C13 C12 C16 105.3(2) . . ? C13 C12 Si2 125.8(2) . . ? C16 C12 Si2 119.8(2) . . ? C13 C12 Ti1 75.22(16) . . ? C16 C12 Ti1 75.87(16) . . ? Si2 C12 Ti1 87.66(11) . . ? C9 C4 C5 117.2(3) . . ? C9 C4 C1 124.0(3) . . ? C5 C4 C1 118.8(3) . . ? N1 C1 C2 110.7(2) . . ? N1 C1 C4 109.0(2) . . ? C2 C1 C4 109.0(2) . . ? N1 C1 C3 109.6(2) . . ? C2 C1 C3 107.4(2) . . ? C4 C1 C3 111.3(2) . . ? C15 C16 C12 109.0(2) . . ? C15 C16 C20 125.9(3) . . ? C12 C16 C20 125.1(3) . . ? C15 C16 Ti1 77.94(17) . . ? C12 C16 Ti1 68.40(15) . . ? C20 C16 Ti1 121.27(19) . . ? C16 C15 C14 108.1(3) . . ? C16 C15 C19 128.5(3) . . ? C14 C15 C19 122.9(3) . . ? C16 C15 Ti1 69.14(16) . . ? C14 C15 Ti1 72.26(16) . . ? C19 C15 Ti1 130.6(2) . . ? C4 C9 C8 120.6(4) . . ? C6 C5 C4 121.9(3) . . ? C7 C6 C5 119.8(4) . . ? C7 C8 C9 121.1(3) . . ? C8 C7 C6 119.4(3) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.407 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.071 #===end data_C5Me4(SiMe2NC6H4Ph)Ti(NMe2)2 _database_code_depnum_ccdc_archive 'CCDC 808877' #TrackingRef '- all-cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H39 N3 Si Ti' _chemical_formula_weight 481.60 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7355(17) _cell_length_b 12.022(2) _cell_length_c 12.655(3) _cell_angle_alpha 85.17(3) _cell_angle_beta 82.55(3) _cell_angle_gamma 79.94(3) _cell_volume 1295.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max .1 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 516 _exptl_absorpt_coefficient_mu 0.396 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.871 _exptl_absorpt_correction_T_max 0.974 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12539 _diffrn_reflns_av_R_equivalents 0.0586 _diffrn_reflns_av_sigmaI/netI 0.0917 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 27.56 _reflns_number_total 5897 _reflns_number_gt 3687 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0760P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5897 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1073 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1551 _refine_ls_wR_factor_gt 0.1289 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.27860(6) 0.31277(4) 0.29884(4) 0.02418(16) Uani 1 1 d . . . Si1 Si 0.58430(9) 0.16362(6) 0.25647(6) 0.0265(2) Uani 1 1 d . . . N1 N 0.3919(3) 0.17003(17) 0.23305(16) 0.0244(5) Uani 1 1 d . . . N2 N 0.1408(3) 0.38982(19) 0.19923(18) 0.0335(6) Uani 1 1 d . . . N3 N 0.1265(3) 0.26829(18) 0.41121(18) 0.0308(6) Uani 1 1 d . . . C14 C 0.4660(3) 0.3227(2) 0.4201(2) 0.0258(6) Uani 1 1 d . . . C1 C 0.3119(3) 0.0783(2) 0.2285(2) 0.0238(6) Uani 1 1 d . . . C2 C 0.2435(3) 0.0611(2) 0.1368(2) 0.0247(6) Uani 1 1 d . . . C8 C 0.4173(3) 0.1403(2) -0.0137(2) 0.0293(6) Uani 1 1 d . . . H8A H 0.5055 0.1085 0.0220 0.035 Uiso 1 1 calc R . . C13 C 0.5435(3) 0.3053(2) 0.3143(2) 0.0251(6) Uani 1 1 d . . . C15 C 0.3689(3) 0.4302(2) 0.4197(2) 0.0287(6) Uani 1 1 d . . . C12 C 0.1407(4) 0.1748(2) -0.0217(2) 0.0329(7) Uani 1 1 d . . . H12A H 0.0378 0.1652 0.0079 0.039 Uiso 1 1 calc R . . C16 C 0.3868(4) 0.4812(2) 0.3142(2) 0.0302(7) Uani 1 1 d . . . C17 C 0.4954(3) 0.4071(2) 0.2504(2) 0.0273(6) Uani 1 1 d . . . C6 C 0.2857(3) 0.0072(2) 0.3195(2) 0.0304(7) Uani 1 1 d . . . H6A H 0.3318 0.0170 0.3814 0.037 Uiso 1 1 calc R . . C7 C 0.2687(3) 0.1280(2) 0.0338(2) 0.0278(6) Uani 1 1 d . . . C5 C 0.1955(4) -0.0769(2) 0.3232(2) 0.0352(7) Uani 1 1 d . . . H5A H 0.1819 -0.1245 0.3864 0.042 Uiso 1 1 calc R . . C4 C 0.1248(4) -0.0918(2) 0.2348(2) 0.0342(7) Uani 1 1 d . . . H4A H 0.0601 -0.1480 0.2371 0.041 Uiso 1 1 calc R . . C20 C 0.3066(4) 0.5992(2) 0.2808(3) 0.0433(8) Uani 1 1 d . . . H20A H 0.3653 0.6554 0.3000 0.065 Uiso 1 1 calc R . . H20B H 0.1998 0.6128 0.3175 0.065 Uiso 1 1 calc R . . H20C H 0.3030 0.6055 0.2035 0.065 Uiso 1 1 calc R . . C3 C 0.1501(3) -0.0237(2) 0.1432(2) 0.0314(7) Uani 1 1 d . . . H3A H 0.1026 -0.0345 0.0823 0.038 Uiso 1 1 calc R . . C11 C 0.1637(4) 0.2348(3) -0.1193(2) 0.0401(8) Uani 1 1 d . . . H11A H 0.0762 0.2682 -0.1551 0.048 Uiso 1 1 calc R . . C22 C 0.6603(4) 0.0417(2) 0.3472(3) 0.0401(8) Uani 1 1 d . . . H22A H 0.7665 0.0479 0.3604 0.060 Uiso 1 1 calc R . . H22B H 0.6624 -0.0293 0.3138 0.060 Uiso 1 1 calc R . . H22C H 0.5919 0.0425 0.4151 0.060 Uiso 1 1 calc R . . C10 C 0.3124(4) 0.2462(3) -0.1646(2) 0.0462(9) Uani 1 1 d . . . H10A H 0.3278 0.2869 -0.2317 0.055 Uiso 1 1 calc R . . C18 C 0.4928(4) 0.2434(3) 0.5164(2) 0.0384(8) Uani 1 1 d . . . H18A H 0.6044 0.2115 0.5136 0.058 Uiso 1 1 calc R . . H18B H 0.4320 0.1821 0.5173 0.058 Uiso 1 1 calc R . . H18C H 0.4597 0.2848 0.5812 0.058 Uiso 1 1 calc R . . C21 C 0.5541(4) 0.4318(3) 0.1346(2) 0.0415(8) Uani 1 1 d . . . H21A H 0.6676 0.4299 0.1272 0.062 Uiso 1 1 calc R . . H21B H 0.5026 0.5069 0.1101 0.062 Uiso 1 1 calc R . . H21C H 0.5303 0.3745 0.0913 0.062 Uiso 1 1 calc R . . C26 C 0.0024(4) 0.2174(3) 0.3738(3) 0.0436(8) Uani 1 1 d . . . H26A H -0.1003 0.2599 0.3987 0.065 Uiso 1 1 calc R . . H26B H 0.0093 0.1385 0.4022 0.065 Uiso 1 1 calc R . . H26C H 0.0162 0.2200 0.2955 0.065 Uiso 1 1 calc R . . C19 C 0.2761(4) 0.4902(2) 0.5129(2) 0.0399(8) Uani 1 1 d . . . H19A H 0.3071 0.5644 0.5149 0.060 Uiso 1 1 calc R . . H19B H 0.2964 0.4451 0.5793 0.060 Uiso 1 1 calc R . . H19C H 0.1642 0.5002 0.5051 0.060 Uiso 1 1 calc R . . C9 C 0.4395(4) 0.1981(3) -0.1122(2) 0.0402(8) Uani 1 1 d . . . H9A H 0.5424 0.2047 -0.1439 0.048 Uiso 1 1 calc R . . C23 C 0.7340(4) 0.1534(3) 0.1367(2) 0.0414(8) Uani 1 1 d . . . H23A H 0.7534 0.0761 0.1131 0.062 Uiso 1 1 calc R . . H23B H 0.8316 0.1724 0.1550 0.062 Uiso 1 1 calc R . . H23C H 0.6957 0.2063 0.0791 0.062 Uiso 1 1 calc R . . C27 C 0.1063(4) 0.2573(3) 0.5270(2) 0.0418(8) Uani 1 1 d . . . H27A H -0.0009 0.2908 0.5535 0.063 Uiso 1 1 calc R . . H27B H 0.1805 0.2968 0.5545 0.063 Uiso 1 1 calc R . . H27C H 0.1256 0.1770 0.5511 0.063 Uiso 1 1 calc R . . C24 C 0.1854(4) 0.4160(3) 0.0856(2) 0.0422(8) Uani 1 1 d . . . H24A H 0.1015 0.4053 0.0449 0.063 Uiso 1 1 calc R . . H24B H 0.2820 0.3655 0.0613 0.063 Uiso 1 1 calc R . . H24C H 0.2025 0.4948 0.0745 0.063 Uiso 1 1 calc R . . C25 C -0.0103(4) 0.4567(3) 0.2341(3) 0.0565(10) Uani 1 1 d . . . H25A H -0.0926 0.4302 0.2020 0.085 Uiso 1 1 calc R . . H25B H -0.0088 0.5365 0.2117 0.085 Uiso 1 1 calc R . . H25C H -0.0312 0.4482 0.3121 0.085 Uiso 1 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 Ti1 0.0237(3) 0.0248(3) 0.0233(3) -0.0015(2) -0.0014(2) -0.0031(2) Si1 0.0223(5) 0.0287(4) 0.0280(4) -0.0041(3) -0.0010(3) -0.0035(3) N1 0.0254(13) 0.0263(11) 0.0214(11) -0.0028(9) 0.0006(10) -0.0056(10) N2 0.0308(15) 0.0331(13) 0.0350(13) -0.0066(11) -0.0067(11) 0.0031(11) N3 0.0266(14) 0.0311(13) 0.0337(13) -0.0031(11) 0.0046(11) -0.0074(11) C14 0.0237(16) 0.0313(15) 0.0247(14) -0.0024(12) -0.0046(12) -0.0098(12) C1 0.0181(15) 0.0235(13) 0.0284(14) -0.0058(11) 0.0008(11) -0.0002(11) C2 0.0228(16) 0.0258(14) 0.0240(13) -0.0044(11) 0.0023(11) -0.0020(11) C8 0.0280(17) 0.0315(15) 0.0279(14) -0.0046(12) -0.0006(12) -0.0041(12) C13 0.0246(16) 0.0289(14) 0.0232(13) -0.0003(11) -0.0034(12) -0.0081(12) C15 0.0292(17) 0.0289(15) 0.0298(14) -0.0064(12) -0.0019(12) -0.0087(13) C12 0.0286(18) 0.0349(16) 0.0370(16) -0.0047(13) -0.0052(13) -0.0081(13) C16 0.0324(18) 0.0220(14) 0.0371(16) 0.0015(12) -0.0032(13) -0.0090(12) C17 0.0283(17) 0.0302(15) 0.0254(14) 0.0015(12) -0.0025(12) -0.0120(13) C6 0.0284(17) 0.0348(16) 0.0274(14) 0.0014(12) -0.0042(12) -0.0044(13) C7 0.0302(17) 0.0251(14) 0.0290(14) -0.0078(12) -0.0006(13) -0.0059(12) C5 0.0330(19) 0.0322(16) 0.0387(17) 0.0074(13) -0.0014(14) -0.0075(14) C4 0.0310(18) 0.0287(15) 0.0445(17) 0.0013(13) -0.0033(14) -0.0115(13) C20 0.047(2) 0.0293(16) 0.0525(19) -0.0012(15) 0.0010(16) -0.0105(15) C3 0.0307(18) 0.0332(15) 0.0320(15) -0.0057(13) -0.0037(13) -0.0087(13) C11 0.047(2) 0.0449(18) 0.0310(16) 0.0025(14) -0.0162(15) -0.0075(16) C22 0.0332(19) 0.0347(16) 0.0527(19) -0.0004(15) -0.0137(15) -0.0015(14) C10 0.061(3) 0.050(2) 0.0266(16) 0.0050(15) -0.0038(16) -0.0129(18) C18 0.039(2) 0.0473(18) 0.0268(15) -0.0014(14) -0.0037(14) -0.0032(15) C21 0.039(2) 0.0509(19) 0.0313(16) 0.0125(14) 0.0038(14) -0.0117(16) C26 0.0295(19) 0.0444(18) 0.058(2) -0.0092(16) 0.0053(15) -0.0130(15) C19 0.042(2) 0.0373(17) 0.0412(17) -0.0108(14) 0.0005(15) -0.0085(15) C9 0.038(2) 0.0472(19) 0.0325(16) -0.0027(15) 0.0101(14) -0.0101(16) C23 0.0232(18) 0.060(2) 0.0408(18) -0.0157(16) 0.0042(14) -0.0061(15) C27 0.035(2) 0.0494(19) 0.0362(17) 0.0021(15) 0.0084(14) -0.0063(15) C24 0.055(2) 0.0366(17) 0.0344(16) 0.0000(14) -0.0141(16) -0.0014(16) C25 0.043(2) 0.061(2) 0.057(2) -0.0004(19) -0.0079(18) 0.0152(18) _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 N2 1.925(2) . ? Ti1 N3 1.925(2) . ? Ti1 N1 2.013(2) . ? Ti1 C13 2.333(3) . ? Ti1 C17 2.362(3) . ? Ti1 C14 2.408(3) . ? Ti1 C16 2.411(3) . ? Ti1 C15 2.453(3) . ? Ti1 Si1 2.9584(13) . ? Si1 N1 1.732(2) . ? Si1 C22 1.866(3) . ? Si1 C23 1.867(3) . ? Si1 C13 1.869(3) . ? N1 C1 1.413(3) . ? N2 C25 1.456(4) . ? N2 C24 1.463(4) . ? N3 C27 1.450(3) . ? N3 C26 1.479(4) . ? C14 C15 1.416(4) . ? C14 C13 1.433(4) . ? C14 C18 1.500(4) . ? C1 C6 1.394(4) . ? C1 C2 1.418(3) . ? C2 C3 1.404(4) . ? C2 C7 1.486(4) . ? C8 C9 1.382(4) . ? C8 C7 1.384(4) . ? C13 C17 1.439(4) . ? C15 C16 1.423(4) . ? C15 C19 1.503(4) . ? C12 C11 1.387(4) . ? C12 C7 1.406(4) . ? C16 C17 1.404(4) . ? C16 C20 1.520(4) . ? C17 C21 1.512(4) . ? C6 C5 1.380(4) . ? C5 C4 1.385(4) . ? C4 C3 1.377(4) . ? C11 C10 1.375(5) . ? C10 C9 1.381(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 N2 Ti1 N3 99.76(11) . . ? N2 Ti1 N1 106.88(9) . . ? N3 Ti1 N1 106.76(10) . . ? N2 Ti1 C13 133.79(11) . . ? N3 Ti1 C13 124.92(10) . . ? N1 Ti1 C13 73.61(9) . . ? N2 Ti1 C17 99.75(10) . . ? N3 Ti1 C17 147.10(9) . . ? N1 Ti1 C17 92.50(10) . . ? C13 Ti1 C17 35.70(9) . . ? N2 Ti1 C14 148.58(10) . . ? N3 Ti1 C14 93.17(10) . . ? N1 Ti1 C14 96.42(9) . . ? C13 Ti1 C14 35.15(9) . . ? C17 Ti1 C14 57.63(9) . . ? N2 Ti1 C16 92.02(10) . . ? N3 Ti1 C16 118.96(10) . . ? N1 Ti1 C16 126.43(10) . . ? C13 Ti1 C16 58.25(10) . . ? C17 Ti1 C16 34.20(10) . . ? C14 Ti1 C16 56.82(9) . . ? N2 Ti1 C15 116.92(9) . . ? N3 Ti1 C15 90.58(10) . . ? N1 Ti1 C15 129.13(9) . . ? C13 Ti1 C15 57.83(9) . . ? C17 Ti1 C15 56.89(9) . . ? C14 Ti1 C15 33.86(9) . . ? C16 Ti1 C15 34.01(9) . . ? N2 Ti1 Si1 129.16(8) . . ? N3 Ti1 Si1 119.36(8) . . ? N1 Ti1 Si1 34.60(7) . . ? C13 Ti1 Si1 39.17(6) . . ? C17 Ti1 Si1 64.71(7) . . ? C14 Ti1 Si1 64.57(7) . . ? C16 Ti1 Si1 95.49(8) . . ? C15 Ti1 Si1 95.16(7) . . ? N1 Si1 C22 114.93(13) . . ? N1 Si1 C23 116.29(12) . . ? C22 Si1 C23 103.30(16) . . ? N1 Si1 C13 93.10(11) . . ? C22 Si1 C13 115.80(13) . . ? C23 Si1 C13 114.01(14) . . ? N1 Si1 Ti1 41.28(7) . . ? C22 Si1 Ti1 124.64(12) . . ? C23 Si1 Ti1 131.76(11) . . ? C13 Si1 Ti1 52.04(9) . . ? C1 N1 Si1 127.40(18) . . ? C1 N1 Ti1 120.00(17) . . ? Si1 N1 Ti1 104.12(10) . . ? C25 N2 C24 110.0(2) . . ? C25 N2 Ti1 122.1(2) . . ? C24 N2 Ti1 125.8(2) . . ? C27 N3 C26 107.5(2) . . ? C27 N3 Ti1 137.8(2) . . ? C26 N3 Ti1 114.20(18) . . ? C15 C14 C13 108.8(2) . . ? C15 C14 C18 125.8(2) . . ? C13 C14 C18 125.3(2) . . ? C15 C14 Ti1 74.81(15) . . ? C13 C14 Ti1 69.57(14) . . ? C18 C14 Ti1 124.90(19) . . ? C6 C1 N1 119.8(2) . . ? C6 C1 C2 117.6(2) . . ? N1 C1 C2 122.3(2) . . ? C3 C2 C1 118.7(3) . . ? C3 C2 C7 118.7(2) . . ? C1 C2 C7 122.6(2) . . ? C9 C8 C7 121.1(3) . . ? C14 C13 C17 106.3(2) . . ? C14 C13 Si1 122.6(2) . . ? C17 C13 Si1 121.29(18) . . ? C14 C13 Ti1 75.28(16) . . ? C17 C13 Ti1 73.24(16) . . ? Si1 C13 Ti1 88.78(11) . . ? C14 C15 C16 107.7(2) . . ? C14 C15 C19 128.4(3) . . ? C16 C15 C19 123.5(3) . . ? C14 C15 Ti1 71.32(14) . . ? C16 C15 Ti1 71.38(15) . . ? C19 C15 Ti1 128.1(2) . . ? C11 C12 C7 120.4(3) . . ? C17 C16 C15 108.5(2) . . ? C17 C16 C20 127.1(3) . . ? C15 C16 C20 124.3(3) . . ? C17 C16 Ti1 70.98(15) . . ? C15 C16 Ti1 74.61(15) . . ? C20 C16 Ti1 123.0(2) . . ? C16 C17 C13 108.6(2) . . ? C16 C17 C21 125.4(3) . . ? C13 C17 C21 125.9(3) . . ? C16 C17 Ti1 74.82(17) . . ? C13 C17 Ti1 71.06(15) . . ? C21 C17 Ti1 121.24(18) . . ? C5 C6 C1 122.6(3) . . ? C8 C7 C12 118.1(3) . . ? C8 C7 C2 121.8(3) . . ? C12 C7 C2 120.0(3) . . ? C6 C5 C4 119.9(3) . . ? C3 C4 C5 118.8(3) . . ? C4 C3 C2 122.3(3) . . ? C10 C11 C12 120.4(3) . . ? C11 C10 C9 119.8(3) . . ? C10 C9 C8 120.2(3) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.578 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.076 #===end data_C5Me4(SiMe2NCMe2Ph)TiI2 _database_code_depnum_ccdc_archive 'CCDC 808878' #TrackingRef '- all-cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H29 I2 N Si Ti' _chemical_formula_weight 613.23 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' 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc 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 19.434(4) _cell_length_b 8.4193(17) _cell_length_c 14.943(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.49(3) _cell_angle_gamma 90.00 _cell_volume 2275.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5380 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.790 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 3.147 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.849 _exptl_absorpt_correction_T_max 0.990 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7355 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3837 _reflns_number_gt 3522 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0273P)^2^+7.1632P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(3) _refine_ls_number_reflns 3837 _refine_ls_number_parameters 226 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0775 _refine_ls_wR_factor_gt 0.0728 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I -0.45845(2) -0.11760(5) -0.23185(3) 0.02637(12) Uani 1 1 d . . . I2 I -0.54135(2) 0.35507(5) -0.26826(3) 0.03013(13) Uani 1 1 d . . . Ti1 Ti -0.47623(6) 0.13363(12) -0.13517(8) 0.0169(2) Uani 1 1 d . . . Si1 Si -0.37424(10) 0.2042(2) 0.05892(13) 0.0196(4) Uani 1 1 d . . . N1 N -0.3785(3) 0.2078(6) -0.0610(4) 0.0194(11) Uani 1 1 d . . . C17 C -0.5432(5) 0.4013(8) -0.0184(6) 0.0275(18) Uani 1 1 d . . . H17A H -0.5683 0.4146 0.0272 0.041 Uiso 1 1 calc R . . H17B H -0.5728 0.4503 -0.0800 0.041 Uiso 1 1 calc R . . H17C H -0.4945 0.4525 0.0072 0.041 Uiso 1 1 calc R . . C12 C -0.4723(4) 0.1279(7) 0.0185(5) 0.0202(16) Uani 1 1 d . . . C5 C -0.2028(4) 0.3858(8) 0.0302(5) 0.0249(16) Uani 1 1 d . . . H5A H -0.1761 0.2887 0.0441 0.030 Uiso 1 1 calc R . . C4 C -0.2748(4) 0.3898(7) -0.0370(5) 0.0203(15) Uani 1 1 d . . . C1 C -0.3142(4) 0.2422(7) -0.0906(5) 0.0205(14) Uani 1 1 d . . . C7 C -0.2078(5) 0.6700(9) 0.0579(6) 0.0324(18) Uani 1 1 d . . . H7A H -0.1845 0.7645 0.0893 0.039 Uiso 1 1 calc R . . C8 C -0.2791(5) 0.6735(9) -0.0073(6) 0.0300(18) Uani 1 1 d . . . H8A H -0.3058 0.7708 -0.0202 0.036 Uiso 1 1 calc R . . C11 C -0.3613(5) 0.4008(8) 0.1217(6) 0.0309(17) Uani 1 1 d . . . H11A H -0.3235 0.3910 0.1863 0.046 Uiso 1 1 calc R . . H11B H -0.4081 0.4343 0.1265 0.046 Uiso 1 1 calc R . . H11C H -0.3456 0.4800 0.0850 0.046 Uiso 1 1 calc R . . C14 C -0.5900(4) 0.1306(7) -0.0995(5) 0.0230(14) Uani 1 1 d . . . C6 C -0.1700(4) 0.5269(9) 0.0774(5) 0.0342(19) Uani 1 1 d . . . H6A H -0.1210 0.5237 0.1236 0.041 Uiso 1 1 calc R . . C9 C -0.3124(4) 0.5370(7) -0.0542(5) 0.0261(16) Uani 1 1 d . . . H9A H -0.3618 0.5419 -0.0992 0.031 Uiso 1 1 calc R . . C3 C -0.2632(4) 0.0958(7) -0.0690(5) 0.0247(15) Uani 1 1 d . . . H3A H -0.2908 0.0043 -0.1053 0.037 Uiso 1 1 calc R . . H3B H -0.2455 0.0723 0.0000 0.037 Uiso 1 1 calc R . . H3C H -0.2209 0.1175 -0.0880 0.037 Uiso 1 1 calc R . . C10 C -0.3008(4) 0.0736(8) 0.1424(5) 0.0295(16) Uani 1 1 d . . . H10A H -0.2754 0.1301 0.2029 0.044 Uiso 1 1 calc R . . H10B H -0.2651 0.0456 0.1127 0.044 Uiso 1 1 calc R . . H10C H -0.3235 -0.0234 0.1554 0.044 Uiso 1 1 calc R . . C2 C -0.3395(4) 0.2754(8) -0.1996(5) 0.0255(15) Uani 1 1 d . . . H2A H -0.3722 0.3683 -0.2159 0.038 Uiso 1 1 calc R . . H2B H -0.3662 0.1829 -0.2355 0.038 Uiso 1 1 calc R . . H2C H -0.2962 0.2962 -0.2166 0.038 Uiso 1 1 calc R . . C13 C -0.5338(4) 0.2288(8) -0.0332(5) 0.0258(15) Uani 1 1 d . . . C16 C -0.4922(4) -0.0306(7) -0.0163(4) 0.0218(14) Uani 1 1 d . . . C15 C -0.5633(4) -0.0278(8) -0.0886(5) 0.0253(15) Uani 1 1 d . . . C18 C -0.6655(4) 0.1794(10) -0.1638(6) 0.0349(18) Uani 1 1 d . . . H18A H -0.7000 0.1645 -0.1304 0.052 Uiso 1 1 calc R . . H18B H -0.6812 0.1142 -0.2222 0.052 Uiso 1 1 calc R . . H18C H -0.6649 0.2915 -0.1811 0.052 Uiso 1 1 calc R . . C20 C -0.4502(4) -0.1805(8) 0.0225(5) 0.0290(17) Uani 1 1 d . . . H20A H -0.4671 -0.2258 0.0713 0.043 Uiso 1 1 calc R . . H20B H -0.3973 -0.1568 0.0514 0.043 Uiso 1 1 calc R . . H20C H -0.4590 -0.2570 -0.0300 0.043 Uiso 1 1 calc R . . C19 C -0.6077(4) -0.1691(8) -0.1406(5) 0.0318(17) Uani 1 1 d . . . H19A H -0.6375 -0.2093 -0.1049 0.048 Uiso 1 1 calc R . . H19B H -0.5741 -0.2527 -0.1453 0.048 Uiso 1 1 calc R . . H19C H -0.6403 -0.1372 -0.2053 0.048 Uiso 1 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 I1 0.0293(3) 0.0279(2) 0.0235(2) -0.00576(19) 0.0115(2) -0.0026(2) I2 0.0302(3) 0.0327(2) 0.0251(2) 0.0097(2) 0.0073(2) 0.0023(2) Ti1 0.0184(6) 0.0186(6) 0.0133(5) -0.0001(4) 0.0055(5) -0.0016(4) Si1 0.0241(10) 0.0171(8) 0.0165(8) -0.0012(7) 0.0062(8) -0.0021(7) N1 0.024(3) 0.016(3) 0.019(3) -0.003(2) 0.010(2) -0.006(2) C17 0.030(4) 0.022(3) 0.029(4) -0.008(3) 0.010(3) 0.011(3) C12 0.020(4) 0.028(4) 0.011(3) -0.002(3) 0.004(3) -0.003(3) C5 0.024(4) 0.026(4) 0.023(4) 0.000(3) 0.008(3) -0.004(3) C4 0.021(4) 0.022(3) 0.021(4) 0.000(2) 0.011(3) -0.003(3) C1 0.023(4) 0.015(3) 0.024(3) 0.000(2) 0.009(3) -0.004(3) C7 0.036(5) 0.024(4) 0.040(5) -0.007(3) 0.018(4) -0.015(3) C8 0.041(5) 0.018(3) 0.045(5) 0.000(3) 0.032(4) -0.005(3) C11 0.046(5) 0.021(3) 0.035(5) -0.006(3) 0.026(4) -0.006(3) C14 0.023(4) 0.024(3) 0.025(4) 0.004(3) 0.012(3) 0.000(3) C6 0.030(5) 0.038(4) 0.030(4) -0.005(3) 0.006(4) -0.012(3) C9 0.024(4) 0.017(3) 0.034(4) 0.007(3) 0.006(3) -0.003(3) C3 0.023(4) 0.021(3) 0.037(4) 0.001(3) 0.019(3) 0.002(3) C10 0.033(4) 0.031(4) 0.022(3) 0.000(3) 0.006(3) 0.001(3) C2 0.025(4) 0.028(3) 0.024(4) 0.002(3) 0.010(3) -0.006(3) C13 0.032(4) 0.026(4) 0.027(4) 0.000(3) 0.020(3) 0.003(3) C16 0.032(4) 0.018(3) 0.020(3) 0.001(2) 0.015(3) -0.001(3) C15 0.030(4) 0.026(3) 0.021(4) -0.003(3) 0.011(3) -0.007(3) C18 0.028(4) 0.041(4) 0.033(4) 0.000(3) 0.009(4) 0.001(3) C20 0.036(4) 0.024(4) 0.026(4) 0.008(3) 0.010(3) -0.002(3) C19 0.031(4) 0.032(4) 0.033(4) -0.005(3) 0.012(3) -0.010(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 I1 Ti1 2.6544(12) . ? I2 Ti1 2.6812(13) . ? Ti1 N1 1.919(5) . ? Ti1 C12 2.270(7) . ? Ti1 C13 2.338(7) . ? Ti1 C16 2.359(6) . ? Ti1 C14 2.458(7) . ? Ti1 C15 2.461(7) . ? Ti1 Si1 2.912(2) . ? Si1 N1 1.764(5) . ? Si1 C10 1.870(7) . ? Si1 C11 1.873(6) . ? Si1 C12 1.889(8) . ? N1 C1 1.499(9) . ? C17 C13 1.490(9) . ? C12 C16 1.433(8) . ? C12 C13 1.438(10) . ? C5 C4 1.392(10) . ? C5 C6 1.409(10) . ? C4 C9 1.413(9) . ? C4 C1 1.525(9) . ? C1 C3 1.540(9) . ? C1 C2 1.545(9) . ? C7 C8 1.373(11) . ? C7 C6 1.385(11) . ? C8 C9 1.378(10) . ? C14 C15 1.419(9) . ? C14 C13 1.438(10) . ? C14 C18 1.486(10) . ? C16 C15 1.408(10) . ? C16 C20 1.499(9) . ? C15 C19 1.507(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 N1 Ti1 C12 76.3(2) . . ? N1 Ti1 C13 96.9(2) . . ? C12 Ti1 C13 36.3(2) . . ? N1 Ti1 C16 97.5(2) . . ? C12 Ti1 C16 36.0(2) . . ? C13 Ti1 C16 58.9(2) . . ? N1 Ti1 C14 131.1(2) . . ? C12 Ti1 C14 58.6(3) . . ? C13 Ti1 C14 34.8(2) . . ? C16 Ti1 C14 56.9(2) . . ? N1 Ti1 C15 130.8(2) . . ? C12 Ti1 C15 58.3(2) . . ? C13 Ti1 C15 57.5(2) . . ? C16 Ti1 C15 33.9(2) . . ? C14 Ti1 C15 33.5(2) . . ? N1 Ti1 I1 105.97(17) . . ? C12 Ti1 I1 124.80(17) . . ? C13 Ti1 I1 144.76(18) . . ? C16 Ti1 I1 91.25(16) . . ? C14 Ti1 I1 114.62(16) . . ? C15 Ti1 I1 87.35(16) . . ? N1 Ti1 I2 107.47(16) . . ? C12 Ti1 I2 126.65(18) . . ? C13 Ti1 I2 92.10(17) . . ? C16 Ti1 I2 144.05(18) . . ? C14 Ti1 I2 87.16(16) . . ? C15 Ti1 I2 114.03(17) . . ? I1 Ti1 I2 105.70(4) . . ? N1 Ti1 Si1 35.91(16) . . ? C12 Ti1 Si1 40.41(19) . . ? C13 Ti1 Si1 66.06(18) . . ? C16 Ti1 Si1 66.36(17) . . ? C14 Ti1 Si1 97.14(17) . . ? C15 Ti1 Si1 96.82(16) . . ? I1 Ti1 Si1 121.86(5) . . ? I2 Ti1 Si1 124.11(5) . . ? N1 Si1 C10 115.4(3) . . ? N1 Si1 C11 116.2(3) . . ? C10 Si1 C11 104.8(4) . . ? N1 Si1 C12 90.8(3) . . ? C10 Si1 C12 116.5(3) . . ? C11 Si1 C12 113.3(3) . . ? N1 Si1 Ti1 39.64(17) . . ? C10 Si1 Ti1 128.2(2) . . ? C11 Si1 Ti1 126.6(3) . . ? C12 Si1 Ti1 51.2(2) . . ? C1 N1 Si1 124.7(4) . . ? C1 N1 Ti1 130.4(4) . . ? Si1 N1 Ti1 104.5(3) . . ? C16 C12 C13 107.2(6) . . ? C16 C12 Si1 122.6(5) . . ? C13 C12 Si1 120.8(5) . . ? C16 C12 Ti1 75.4(4) . . ? C13 C12 Ti1 74.4(4) . . ? Si1 C12 Ti1 88.4(3) . . ? C4 C5 C6 119.4(7) . . ? C5 C4 C9 118.0(6) . . ? C5 C4 C1 122.5(6) . . ? C9 C4 C1 119.5(6) . . ? N1 C1 C4 108.3(5) . . ? N1 C1 C3 109.0(5) . . ? C4 C1 C3 112.5(6) . . ? N1 C1 C2 111.6(5) . . ? C4 C1 C2 108.1(5) . . ? C3 C1 C2 107.3(6) . . ? C8 C7 C6 119.2(7) . . ? C7 C8 C9 120.4(7) . . ? C15 C14 C13 107.9(6) . . ? C15 C14 C18 124.5(6) . . ? C13 C14 C18 127.4(6) . . ? C15 C14 Ti1 73.4(4) . . ? C13 C14 Ti1 68.0(4) . . ? C18 C14 Ti1 127.6(5) . . ? C7 C6 C5 121.3(7) . . ? C8 C9 C4 121.6(7) . . ? C14 C13 C12 107.6(6) . . ? C14 C13 C17 124.0(6) . . ? C12 C13 C17 128.2(7) . . ? C14 C13 Ti1 77.2(4) . . ? C12 C13 Ti1 69.3(4) . . ? C17 C13 Ti1 123.0(5) . . ? C15 C16 C12 108.7(6) . . ? C15 C16 C20 123.5(6) . . ? C12 C16 C20 127.4(6) . . ? C15 C16 Ti1 77.0(4) . . ? C12 C16 Ti1 68.6(4) . . ? C20 C16 Ti1 125.6(5) . . ? C16 C15 C14 108.6(6) . . ? C16 C15 C19 126.7(6) . . ? C14 C15 C19 124.5(6) . . ? C16 C15 Ti1 69.1(4) . . ? C14 C15 Ti1 73.1(4) . . ? C19 C15 Ti1 127.8(5) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.426 _refine_diff_density_min -0.841 _refine_diff_density_rms 0.137 #===end data_C5Me4(SiMe2NC6H4Ph)TiI2 _database_code_depnum_ccdc_archive 'CCDC 808879' #TrackingRef '- all-cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H27 I2 N Si Ti' _chemical_formula_weight 647.25 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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' _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 15.316(3) _cell_length_b 7.7666(16) _cell_length_c 21.150(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.64(3) _cell_angle_gamma 90.00 _cell_volume 2383.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6184 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.803 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 3.009 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.662 _exptl_absorpt_correction_T_max 0.916 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16159 _diffrn_reflns_av_R_equivalents 0.0929 _diffrn_reflns_av_sigmaI/netI 0.1226 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 27.52 _reflns_number_total 5413 _reflns_number_gt 2956 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0749P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5413 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1364 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1655 _refine_ls_wR_factor_gt 0.1287 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 I1 I 0.34023(4) 0.10481(7) 0.13453(3) 0.0294(2) Uani 1 1 d . . . I2 I 0.11397(4) 0.29971(7) -0.00645(3) 0.0319(2) Uani 1 1 d . . . Ti1 Ti 0.24929(10) 0.39706(17) 0.10098(7) 0.0205(4) Uani 1 1 d . . . Si1 Si 0.22574(18) 0.6791(3) 0.18717(12) 0.0245(6) Uani 1 1 d . . . N1 N 0.2015(5) 0.4566(8) 0.1731(3) 0.0236(16) Uani 1 1 d . . . C9 C 0.4198(6) 0.3366(11) 0.3612(4) 0.031(2) Uani 1 1 d . . . H9A H 0.4786 0.3138 0.3569 0.037 Uiso 1 1 calc R . . C1 C 0.1415(6) 0.3531(10) 0.1968(4) 0.0220(19) Uani 1 1 d . . . C3 C 0.1007(6) 0.1901(10) 0.2802(4) 0.027(2) Uani 1 1 d . . . H3A H 0.1159 0.1474 0.3245 0.032 Uiso 1 1 calc R . . C17 C 0.2522(6) 0.6731(10) 0.0564(4) 0.0221(19) Uani 1 1 d . . . C7 C 0.2518(6) 0.3337(10) 0.3153(4) 0.023(2) Uani 1 1 d . . . C21 C 0.1679(6) 0.7744(10) 0.0158(4) 0.028(2) Uani 1 1 d . . . H21A H 0.1874 0.8854 0.0028 0.042 Uiso 1 1 calc R . . H21B H 0.1272 0.7938 0.0427 0.042 Uiso 1 1 calc R . . H21C H 0.1347 0.7091 -0.0244 0.042 Uiso 1 1 calc R . . C13 C 0.2927(6) 0.6724(10) 0.1274(4) 0.025(2) Uani 1 1 d . . . C18 C 0.4470(6) 0.5421(11) 0.2093(4) 0.031(2) Uani 1 1 d . . . H18A H 0.4954 0.6298 0.2179 0.046 Uiso 1 1 calc R . . H18B H 0.4742 0.4277 0.2097 0.046 Uiso 1 1 calc R . . H18C H 0.4172 0.5479 0.2439 0.046 Uiso 1 1 calc R . . C8 C 0.3378(6) 0.2958(10) 0.3084(4) 0.028(2) Uani 1 1 d . . . H8A H 0.3414 0.2434 0.2687 0.033 Uiso 1 1 calc R . . C2 C 0.1641(6) 0.2917(9) 0.2625(4) 0.024(2) Uani 1 1 d . . . C15 C 0.3857(6) 0.5127(10) 0.0808(4) 0.0214(18) Uani 1 1 d . . . C10 C 0.4126(8) 0.4093(11) 0.4185(5) 0.041(3) Uani 1 1 d . . . H10A H 0.4673 0.4375 0.4535 0.050 Uiso 1 1 calc R . . C19 C 0.4658(6) 0.4166(11) 0.0730(4) 0.031(2) Uani 1 1 d . . . H19A H 0.5101 0.4983 0.0651 0.046 Uiso 1 1 calc R . . H19B H 0.4445 0.3377 0.0350 0.046 Uiso 1 1 calc R . . H19C H 0.4956 0.3507 0.1137 0.046 Uiso 1 1 calc R . . C4 C 0.0170(6) 0.1506(11) 0.2351(5) 0.033(2) Uani 1 1 d . . . H4A H -0.0242 0.0782 0.2482 0.040 Uiso 1 1 calc R . . C11 C 0.3304(8) 0.4422(12) 0.4266(4) 0.039(3) Uani 1 1 d . . . H11A H 0.3279 0.4898 0.4674 0.047 Uiso 1 1 calc R . . C12 C 0.2486(7) 0.4060(11) 0.3750(4) 0.034(2) Uani 1 1 d . . . H12A H 0.1908 0.4309 0.3806 0.040 Uiso 1 1 calc R . . C16 C 0.3084(6) 0.5752(10) 0.0282(4) 0.025(2) Uani 1 1 d . . . C22 C 0.2905(7) 0.7449(11) 0.2734(5) 0.034(2) Uani 1 1 d . . . H22A H 0.2616 0.8471 0.2853 0.052 Uiso 1 1 calc R . . H22B H 0.3542 0.7717 0.2765 0.052 Uiso 1 1 calc R . . H22C H 0.2900 0.6508 0.3041 0.052 Uiso 1 1 calc R . . C20 C 0.2943(6) 0.5517(11) -0.0456(4) 0.033(2) Uani 1 1 d . . . H20A H 0.3271 0.6427 -0.0609 0.050 Uiso 1 1 calc R . . H20B H 0.2284 0.5580 -0.0707 0.050 Uiso 1 1 calc R . . H20C H 0.3183 0.4391 -0.0530 0.050 Uiso 1 1 calc R . . C14 C 0.3759(6) 0.5742(10) 0.1415(4) 0.025(2) Uani 1 1 d . . . C6 C 0.0535(6) 0.3137(10) 0.1523(4) 0.028(2) Uani 1 1 d . . . H6A H 0.0368 0.3575 0.1081 0.034 Uiso 1 1 calc R . . C5 C -0.0091(7) 0.2148(11) 0.1701(5) 0.033(2) Uani 1 1 d . . . H5A H -0.0682 0.1909 0.1392 0.040 Uiso 1 1 calc R . . C23 C 0.1197(7) 0.8115(12) 0.1614(5) 0.039(2) Uani 1 1 d . . . H23A H 0.1231 0.8989 0.1956 0.058 Uiso 1 1 calc R . . H23B H 0.0660 0.7376 0.1562 0.058 Uiso 1 1 calc R . . H23C H 0.1140 0.8682 0.1189 0.058 Uiso 1 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 I1 0.0315(4) 0.0221(3) 0.0333(4) 0.0006(2) 0.0084(3) 0.0013(3) I2 0.0264(4) 0.0357(4) 0.0315(4) -0.0040(3) 0.0062(3) -0.0036(3) Ti1 0.0202(9) 0.0170(7) 0.0250(8) 0.0006(6) 0.0082(7) -0.0010(6) Si1 0.0287(15) 0.0198(11) 0.0276(14) -0.0009(10) 0.0125(11) -0.0039(10) N1 0.018(4) 0.029(4) 0.027(4) 0.001(3) 0.011(3) -0.001(3) C9 0.018(5) 0.035(5) 0.041(6) 0.014(4) 0.012(4) 0.012(4) C1 0.017(5) 0.024(4) 0.025(5) 0.000(3) 0.007(4) -0.002(4) C3 0.026(5) 0.029(5) 0.029(5) 0.005(4) 0.015(4) 0.002(4) C17 0.017(5) 0.029(4) 0.023(5) 0.003(4) 0.012(4) -0.008(4) C7 0.033(5) 0.020(4) 0.022(5) 0.005(3) 0.016(4) 0.001(4) C21 0.029(5) 0.025(4) 0.028(5) 0.003(4) 0.007(4) 0.005(4) C13 0.034(6) 0.021(4) 0.025(5) 0.001(3) 0.015(4) -0.007(4) C18 0.031(6) 0.033(5) 0.026(5) -0.011(4) 0.006(4) 0.006(4) C8 0.032(6) 0.021(4) 0.030(5) 0.002(4) 0.009(4) 0.003(4) C2 0.033(5) 0.018(4) 0.023(5) -0.004(3) 0.010(4) 0.004(4) C15 0.019(5) 0.021(4) 0.026(5) 0.002(4) 0.009(4) -0.006(4) C10 0.048(7) 0.037(6) 0.031(6) 0.000(4) 0.000(5) 0.000(5) C19 0.023(5) 0.032(5) 0.037(6) 0.008(4) 0.009(4) 0.004(4) C4 0.027(6) 0.040(5) 0.042(6) 0.013(4) 0.024(5) -0.002(4) C11 0.052(7) 0.048(6) 0.015(5) -0.002(4) 0.007(5) 0.000(5) C12 0.040(6) 0.038(5) 0.029(5) 0.006(4) 0.018(5) 0.008(5) C16 0.030(5) 0.023(4) 0.024(5) 0.006(3) 0.009(4) -0.009(4) C22 0.030(6) 0.030(5) 0.043(6) 0.000(4) 0.010(5) -0.002(4) C20 0.022(5) 0.044(5) 0.030(5) 0.002(4) 0.000(4) -0.005(4) C14 0.030(5) 0.026(4) 0.020(5) 0.006(3) 0.009(4) 0.011(4) C6 0.033(6) 0.031(5) 0.030(5) -0.002(4) 0.025(5) 0.006(4) C5 0.026(5) 0.039(5) 0.033(5) 0.001(4) 0.007(4) 0.002(4) C23 0.034(6) 0.045(6) 0.045(6) -0.003(5) 0.024(5) 0.003(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Ti1 2.6390(16) . ? I2 Ti1 2.6495(18) . ? Ti1 N1 1.946(7) . ? Ti1 C13 2.256(8) . ? Ti1 C14 2.308(9) . ? Ti1 C17 2.348(8) . ? Ti1 C15 2.434(8) . ? Ti1 C16 2.449(8) . ? Ti1 Si1 2.945(3) . ? Si1 N1 1.773(7) . ? Si1 C22 1.847(9) . ? Si1 C23 1.850(9) . ? Si1 C13 1.866(9) . ? N1 C1 1.427(10) . ? C9 C10 1.372(13) . ? C9 C8 1.425(12) . ? C1 C2 1.403(11) . ? C1 C6 1.409(12) . ? C3 C4 1.366(12) . ? C3 C2 1.392(12) . ? C17 C16 1.417(12) . ? C17 C13 1.430(11) . ? C17 C21 1.522(11) . ? C7 C12 1.396(11) . ? C7 C8 1.403(12) . ? C7 C2 1.483(12) . ? C13 C14 1.432(12) . ? C18 C14 1.518(12) . ? C15 C14 1.422(11) . ? C15 C16 1.425(11) . ? C15 C19 1.491(12) . ? C10 C11 1.349(15) . ? C4 C5 1.395(12) . ? C11 C12 1.402(13) . ? C16 C20 1.516(12) . ? C6 C5 1.372(12) . ? 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 C13 74.7(3) . . ? N1 Ti1 C14 92.8(3) . . ? C13 Ti1 C14 36.6(3) . . ? N1 Ti1 C17 99.1(3) . . ? C13 Ti1 C17 36.1(3) . . ? C14 Ti1 C17 58.9(3) . . ? N1 Ti1 C15 127.5(3) . . ? C13 Ti1 C15 59.5(3) . . ? C14 Ti1 C15 34.8(3) . . ? C17 Ti1 C15 57.7(3) . . ? N1 Ti1 C16 131.7(3) . . ? C13 Ti1 C16 58.8(3) . . ? C14 Ti1 C16 57.4(3) . . ? C17 Ti1 C16 34.3(3) . . ? C15 Ti1 C16 33.9(3) . . ? N1 Ti1 I1 107.0(2) . . ? C13 Ti1 I1 131.3(2) . . ? C14 Ti1 I1 96.0(2) . . ? C17 Ti1 I1 144.8(2) . . ? C15 Ti1 I1 87.47(19) . . ? C16 Ti1 I1 112.7(2) . . ? N1 Ti1 I2 110.6(2) . . ? C13 Ti1 I2 124.8(2) . . ? C14 Ti1 I2 145.4(2) . . ? C17 Ti1 I2 91.5(2) . . ? C15 Ti1 I2 115.76(19) . . ? C16 Ti1 I2 88.1(2) . . ? I1 Ti1 I2 100.73(5) . . ? N1 Ti1 Si1 35.6(2) . . ? C13 Ti1 Si1 39.3(2) . . ? C14 Ti1 Si1 65.3(2) . . ? C17 Ti1 Si1 65.9(2) . . ? C15 Ti1 Si1 96.7(2) . . ? C16 Ti1 Si1 96.4(2) . . ? I1 Ti1 Si1 129.20(7) . . ? I2 Ti1 Si1 121.75(7) . . ? N1 Si1 C22 117.0(4) . . ? N1 Si1 C23 112.0(4) . . ? C22 Si1 C23 106.3(4) . . ? N1 Si1 C13 89.4(3) . . ? C22 Si1 C13 116.0(4) . . ? C23 Si1 C13 115.9(4) . . ? N1 Si1 Ti1 39.8(2) . . ? C22 Si1 Ti1 133.1(3) . . ? C23 Si1 Ti1 120.0(3) . . ? C13 Si1 Ti1 50.0(2) . . ? C1 N1 Si1 127.9(6) . . ? C1 N1 Ti1 126.0(5) . . ? Si1 N1 Ti1 104.6(3) . . ? C10 C9 C8 119.0(9) . . ? C2 C1 C6 117.9(8) . . ? C2 C1 N1 123.9(8) . . ? C6 C1 N1 118.2(7) . . ? C4 C3 C2 121.3(8) . . ? C16 C17 C13 108.8(7) . . ? C16 C17 C21 124.0(7) . . ? C13 C17 C21 126.9(8) . . ? C16 C17 Ti1 76.8(5) . . ? C13 C17 Ti1 68.4(4) . . ? C21 C17 Ti1 125.2(5) . . ? C12 C7 C8 118.9(8) . . ? C12 C7 C2 119.0(8) . . ? C8 C7 C2 122.0(7) . . ? C17 C13 C14 106.2(7) . . ? C17 C13 Si1 124.3(7) . . ? C14 C13 Si1 121.3(6) . . ? C17 C13 Ti1 75.4(5) . . ? C14 C13 Ti1 73.7(5) . . ? Si1 C13 Ti1 90.7(3) . . ? C7 C8 C9 119.6(8) . . ? C3 C2 C1 119.1(8) . . ? C3 C2 C7 117.7(7) . . ? C1 C2 C7 123.2(8) . . ? C14 C15 C16 106.9(7) . . ? C14 C15 C19 126.6(8) . . ? C16 C15 C19 126.3(7) . . ? C14 C15 Ti1 67.8(5) . . ? C16 C15 Ti1 73.6(5) . . ? C19 C15 Ti1 128.2(5) . . ? C11 C10 C9 122.2(10) . . ? C3 C4 C5 121.2(8) . . ? C10 C11 C12 120.0(9) . . ? C7 C12 C11 120.3(9) . . ? C17 C16 C15 108.6(7) . . ? C17 C16 C20 126.4(8) . . ? C15 C16 C20 124.9(8) . . ? C17 C16 Ti1 69.0(4) . . ? C15 C16 Ti1 72.4(4) . . ? C20 C16 Ti1 128.3(5) . . ? C15 C14 C13 109.5(7) . . ? C15 C14 C18 123.2(8) . . ? C13 C14 C18 127.3(7) . . ? C15 C14 Ti1 77.5(5) . . ? C13 C14 Ti1 69.8(5) . . ? C18 C14 Ti1 121.1(6) . . ? C5 C6 C1 122.8(8) . . ? C6 C5 C4 117.7(9) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.345 _refine_diff_density_min -1.442 _refine_diff_density_rms 0.247 #===end data_C5Me4SiMe2N(C6H4Ph)TiMe2 _database_code_depnum_ccdc_archive 'CCDC 808880' #TrackingRef '- all-cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H33 N Si Ti' _chemical_formula_weight 423.51 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.5742(15) _cell_length_b 11.756(2) _cell_length_c 13.062(3) _cell_angle_alpha 80.73(3) _cell_angle_beta 85.90(3) _cell_angle_gamma 83.85(3) _cell_volume 1139.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 452 _exptl_absorpt_coefficient_mu 0.438 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.801 _exptl_absorpt_correction_T_max 0.979 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10685 _diffrn_reflns_av_R_equivalents 0.1237 _diffrn_reflns_av_sigmaI/netI 0.2222 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 27.69 _reflns_number_total 5127 _reflns_number_gt 2277 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1055P)^2^+8.2711P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5127 _refine_ls_number_parameters 261 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2394 _refine_ls_R_factor_gt 0.1179 _refine_ls_wR_factor_ref 0.3469 _refine_ls_wR_factor_gt 0.2902 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.76565(19) 0.72545(14) 0.66398(12) 0.0296(5) Uani 1 1 d . . . Si1 Si 0.4468(3) 0.7875(2) 0.7908(2) 0.0335(6) Uani 1 1 d . . . N1 N 0.6668(9) 0.8228(6) 0.7654(5) 0.0286(16) Uani 1 1 d . . . C19 C 0.6227(11) 0.6213(8) 0.5512(7) 0.034(2) Uani 1 1 d . . . C3 C 0.7367(10) 0.9221(7) 0.7903(6) 0.0282(19) Uani 1 1 d . . . C17 C 0.4824(11) 0.6748(8) 0.7024(6) 0.032(2) Uani 1 1 d . . . C8 C 0.7678(11) 1.0144(7) 0.7110(7) 0.035(2) Uani 1 1 d . . . H8A H 0.7451 1.0076 0.6418 0.042 Uiso 1 1 calc R . . C14 C 0.8509(12) 0.7284(8) 0.9785(7) 0.036(2) Uani 1 1 d . . . H14A H 0.9179 0.7138 0.9169 0.043 Uiso 1 1 calc R . . C10 C 0.6589(12) 0.8568(9) 1.0720(7) 0.041(2) Uani 1 1 d . . . H10A H 0.5945 0.9303 1.0748 0.049 Uiso 1 1 calc R . . C18 C 0.4992(11) 0.7035(8) 0.5916(7) 0.032(2) Uani 1 1 d . . . C9 C 0.7584(11) 0.8369(8) 0.9817(7) 0.033(2) Uani 1 1 d . . . C21 C 0.5987(12) 0.5711(8) 0.7284(7) 0.035(2) Uani 1 1 d . . . C20 C 0.6850(11) 0.5393(8) 0.6378(7) 0.036(2) Uani 1 1 d . . . C5 C 0.8334(11) 1.0368(8) 0.9097(7) 0.037(2) Uani 1 1 d . . . H5A H 0.8536 1.0457 0.9788 0.044 Uiso 1 1 calc R . . C4 C 0.7752(10) 0.9330(7) 0.8918(7) 0.031(2) Uani 1 1 d . . . C6 C 0.8625(12) 1.1272(8) 0.8297(8) 0.038(2) Uani 1 1 d . . . H6A H 0.9041 1.1963 0.8436 0.045 Uiso 1 1 calc R . . C1 C 1.0053(11) 0.6375(8) 0.7180(8) 0.042(2) Uani 1 1 d . . . H1A H 1.0619 0.5919 0.6659 0.062 Uiso 1 1 calc R . . H1B H 0.9810 0.5857 0.7830 0.062 Uiso 1 1 calc R . . H1C H 1.0850 0.6937 0.7303 0.062 Uiso 1 1 calc R . . C13 C 0.8467(12) 0.6410(8) 1.0640(8) 0.040(2) Uani 1 1 d . . . H13A H 0.9103 0.5673 1.0611 0.048 Uiso 1 1 calc R . . C11 C 0.6526(12) 0.7707(9) 1.1578(7) 0.042(2) Uani 1 1 d . . . H11A H 0.5835 0.7852 1.2188 0.050 Uiso 1 1 calc R . . C15 C 0.3805(13) 0.7276(10) 0.9270(7) 0.047(3) Uani 1 1 d . . . H15A H 0.3600 0.7906 0.9686 0.071 Uiso 1 1 calc R . . H15B H 0.4756 0.6710 0.9560 0.071 Uiso 1 1 calc R . . H15C H 0.2711 0.6898 0.9281 0.071 Uiso 1 1 calc R . . C2 C 0.8631(13) 0.8254(9) 0.5273(8) 0.045(2) Uani 1 1 d . . . H2A H 0.9336 0.7745 0.4840 0.067 Uiso 1 1 calc R . . H2B H 0.9379 0.8814 0.5454 0.067 Uiso 1 1 calc R . . H2C H 0.7630 0.8668 0.4888 0.067 Uiso 1 1 calc R . . C12 C 0.7466(13) 0.6638(9) 1.1548(7) 0.045(2) Uani 1 1 d . . . H12A H 0.7437 0.6054 1.2141 0.054 Uiso 1 1 calc R . . C24 C 0.8074(13) 0.4315(8) 0.6271(9) 0.052(3) Uani 1 1 d . . . H24A H 0.7366 0.3676 0.6226 0.078 Uiso 1 1 calc R . . H24B H 0.8800 0.4113 0.6878 0.078 Uiso 1 1 calc R . . H24C H 0.8851 0.4455 0.5640 0.078 Uiso 1 1 calc R . . C16 C 0.2850(13) 0.9144(9) 0.7498(8) 0.047(3) Uani 1 1 d . . . H16A H 0.2567 0.9584 0.8075 0.071 Uiso 1 1 calc R . . H16B H 0.1760 0.8875 0.7301 0.071 Uiso 1 1 calc R . . H16C H 0.3369 0.9641 0.6903 0.071 Uiso 1 1 calc R . . C23 C 0.6721(13) 0.6149(9) 0.4403(7) 0.046(2) Uani 1 1 d . . . H23A H 0.5970 0.5636 0.4151 0.068 Uiso 1 1 calc R . . H23B H 0.7972 0.5845 0.4329 0.068 Uiso 1 1 calc R . . H23C H 0.6548 0.6925 0.3996 0.068 Uiso 1 1 calc R . . C7 C 0.8299(13) 1.1148(8) 0.7295(8) 0.044(2) Uani 1 1 d . . . H7A H 0.8502 1.1752 0.6736 0.053 Uiso 1 1 calc R . . C25 C 0.6291(14) 0.5055(9) 0.8375(8) 0.049(3) Uani 1 1 d . . . H25A H 0.5144 0.4887 0.8732 0.073 Uiso 1 1 calc R . . H25B H 0.6892 0.5530 0.8766 0.073 Uiso 1 1 calc R . . H25C H 0.7033 0.4328 0.8326 0.073 Uiso 1 1 calc R . . C22 C 0.4043(14) 0.8077(9) 0.5270(7) 0.049(3) Uani 1 1 d . . . H22A H 0.2755 0.8055 0.5392 0.074 Uiso 1 1 calc R . . H22B H 0.4370 0.8062 0.4532 0.074 Uiso 1 1 calc R . . H22C H 0.4392 0.8788 0.5467 0.074 Uiso 1 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 Ti1 0.0259(8) 0.0310(9) 0.0311(9) -0.0033(7) -0.0019(7) -0.0007(6) Si1 0.0262(12) 0.0390(16) 0.0358(14) -0.0071(12) -0.0036(11) -0.0014(10) N1 0.032(4) 0.027(4) 0.024(4) 0.004(3) -0.006(3) -0.004(3) C19 0.029(4) 0.039(5) 0.038(5) -0.017(4) -0.005(4) -0.002(4) C3 0.029(4) 0.026(5) 0.030(5) -0.004(4) -0.006(4) 0.002(3) C17 0.029(4) 0.042(5) 0.025(4) -0.002(4) -0.002(4) -0.004(4) C8 0.037(5) 0.028(5) 0.036(5) 0.001(4) -0.004(4) 0.003(4) C14 0.037(5) 0.040(6) 0.031(5) -0.007(4) -0.010(4) 0.005(4) C10 0.039(5) 0.049(6) 0.033(5) -0.007(4) -0.007(4) 0.006(4) C18 0.027(4) 0.037(5) 0.033(5) -0.006(4) -0.002(4) -0.006(4) C9 0.034(5) 0.032(5) 0.030(5) -0.001(4) -0.010(4) 0.001(4) C21 0.037(5) 0.034(5) 0.034(5) -0.003(4) -0.008(4) -0.008(4) C20 0.032(5) 0.026(5) 0.048(6) -0.006(4) -0.004(4) 0.005(4) C5 0.028(4) 0.041(6) 0.044(6) -0.012(5) -0.010(4) 0.002(4) C4 0.024(4) 0.030(5) 0.037(5) -0.002(4) -0.002(4) -0.001(3) C6 0.041(5) 0.022(5) 0.052(6) -0.011(4) -0.010(5) -0.002(4) C1 0.028(5) 0.043(6) 0.055(6) -0.013(5) 0.000(4) 0.003(4) C13 0.041(5) 0.030(5) 0.049(6) -0.002(4) -0.010(5) 0.004(4) C11 0.038(5) 0.058(7) 0.027(5) -0.006(5) 0.000(4) 0.004(5) C15 0.039(5) 0.069(8) 0.039(6) -0.019(5) 0.000(5) -0.007(5) C2 0.041(5) 0.043(6) 0.049(6) -0.007(5) 0.012(5) -0.011(4) C12 0.052(6) 0.049(7) 0.031(5) 0.000(5) -0.004(5) -0.003(5) C24 0.041(6) 0.036(6) 0.081(8) -0.015(5) -0.017(6) 0.004(4) C16 0.041(5) 0.052(7) 0.051(6) -0.020(5) -0.007(5) 0.009(5) C23 0.045(6) 0.059(7) 0.034(5) -0.013(5) 0.004(4) -0.005(5) C7 0.050(6) 0.036(6) 0.043(6) 0.004(5) 0.004(5) -0.004(4) C25 0.054(6) 0.039(6) 0.048(6) 0.009(5) -0.008(5) -0.002(5) C22 0.054(6) 0.054(7) 0.034(5) -0.005(5) -0.003(5) 0.023(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 N1 1.947(7) . ? Ti1 C1 2.100(9) . ? Ti1 C2 2.106(10) . ? Ti1 C17 2.287(8) . ? Ti1 C21 2.334(9) . ? Ti1 C18 2.344(8) . ? Ti1 C20 2.416(9) . ? Ti1 C19 2.436(8) . ? Ti1 Si1 2.924(3) . ? Si1 N1 1.756(7) . ? Si1 C15 1.859(10) . ? Si1 C16 1.860(10) . ? Si1 C17 1.879(10) . ? N1 C3 1.424(10) . ? C19 C18 1.410(12) . ? C19 C20 1.435(12) . ? C19 C23 1.482(13) . ? C3 C8 1.402(12) . ? C3 C4 1.406(12) . ? C17 C18 1.432(12) . ? C17 C21 1.434(12) . ? C8 C7 1.378(13) . ? C14 C13 1.391(12) . ? C14 C9 1.394(12) . ? C10 C11 1.386(13) . ? C10 C9 1.392(13) . ? C18 C22 1.515(12) . ? C9 C4 1.501(12) . ? C21 C20 1.396(13) . ? C21 C25 1.527(12) . ? C20 C24 1.507(12) . ? C5 C6 1.389(13) . ? C5 C4 1.400(12) . ? C6 C7 1.383(13) . ? C13 C12 1.408(14) . ? C11 C12 1.382(14) . ? 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 C1 107.9(3) . . ? N1 Ti1 C2 111.3(4) . . ? C1 Ti1 C2 99.8(4) . . ? N1 Ti1 C17 75.6(3) . . ? C1 Ti1 C17 128.6(4) . . ? C2 Ti1 C17 127.5(3) . . ? N1 Ti1 C21 95.3(3) . . ? C1 Ti1 C21 94.0(3) . . ? C2 Ti1 C21 144.1(4) . . ? C17 Ti1 C21 36.1(3) . . ? N1 Ti1 C18 98.0(3) . . ? C1 Ti1 C18 144.1(4) . . ? C2 Ti1 C18 93.2(4) . . ? C17 Ti1 C18 36.0(3) . . ? C21 Ti1 C18 58.5(3) . . ? N1 Ti1 C20 129.2(3) . . ? C1 Ti1 C20 86.7(3) . . ? C2 Ti1 C20 113.6(4) . . ? C17 Ti1 C20 58.7(3) . . ? C21 Ti1 C20 34.1(3) . . ? C18 Ti1 C20 57.4(3) . . ? N1 Ti1 C19 131.4(3) . . ? C1 Ti1 C19 113.0(3) . . ? C2 Ti1 C19 86.7(4) . . ? C17 Ti1 C19 58.7(3) . . ? C21 Ti1 C19 57.4(3) . . ? C18 Ti1 C19 34.2(3) . . ? C20 Ti1 C19 34.4(3) . . ? N1 Ti1 Si1 35.6(2) . . ? C1 Ti1 Si1 126.6(3) . . ? C2 Ti1 Si1 126.1(3) . . ? C17 Ti1 Si1 40.0(2) . . ? C21 Ti1 Si1 65.6(2) . . ? C18 Ti1 Si1 66.1(2) . . ? C20 Ti1 Si1 96.6(2) . . ? C19 Ti1 Si1 96.9(2) . . ? N1 Si1 C15 117.1(4) . . ? N1 Si1 C16 111.3(4) . . ? C15 Si1 C16 107.2(5) . . ? N1 Si1 C17 91.6(4) . . ? C15 Si1 C17 113.2(4) . . ? C16 Si1 C17 116.2(4) . . ? N1 Si1 Ti1 40.2(2) . . ? C15 Si1 Ti1 129.3(3) . . ? C16 Si1 Ti1 123.0(4) . . ? C17 Si1 Ti1 51.5(3) . . ? C3 N1 Si1 126.2(6) . . ? C3 N1 Ti1 127.4(6) . . ? Si1 N1 Ti1 104.2(3) . . ? C18 C19 C20 107.1(8) . . ? C18 C19 C23 127.2(8) . . ? C20 C19 C23 125.7(9) . . ? C18 C19 Ti1 69.3(5) . . ? C20 C19 Ti1 72.0(5) . . ? C23 C19 Ti1 126.7(6) . . ? C8 C3 C4 117.7(8) . . ? C8 C3 N1 119.2(7) . . ? C4 C3 N1 123.1(7) . . ? C18 C17 C21 105.9(8) . . ? C18 C17 Si1 122.8(7) . . ? C21 C17 Si1 121.0(6) . . ? C18 C17 Ti1 74.2(5) . . ? C21 C17 Ti1 73.7(5) . . ? Si1 C17 Ti1 88.6(3) . . ? C7 C8 C3 122.6(9) . . ? C13 C14 C9 121.2(9) . . ? C11 C10 C9 120.8(9) . . ? C19 C18 C17 109.5(8) . . ? C19 C18 C22 124.7(8) . . ? C17 C18 C22 125.9(8) . . ? C19 C18 Ti1 76.5(5) . . ? C17 C18 Ti1 69.8(5) . . ? C22 C18 Ti1 118.7(6) . . ? C10 C9 C14 118.9(8) . . ? C10 C9 C4 120.5(8) . . ? C14 C9 C4 120.5(8) . . ? C20 C21 C17 109.3(8) . . ? C20 C21 C25 124.3(8) . . ? C17 C21 C25 126.3(9) . . ? C20 C21 Ti1 76.1(5) . . ? C17 C21 Ti1 70.1(5) . . ? C25 C21 Ti1 119.0(6) . . ? C21 C20 C19 108.3(8) . . ? C21 C20 C24 127.6(9) . . ? C19 C20 C24 123.8(9) . . ? C21 C20 Ti1 69.7(5) . . ? C19 C20 Ti1 73.6(5) . . ? C24 C20 Ti1 127.6(6) . . ? C6 C5 C4 122.1(9) . . ? C5 C4 C3 118.9(8) . . ? C5 C4 C9 118.6(8) . . ? C3 C4 C9 122.5(8) . . ? C7 C6 C5 118.8(9) . . ? C14 C13 C12 118.8(9) . . ? C12 C11 C10 120.1(9) . . ? C11 C12 C13 120.3(9) . . ? C8 C7 C6 119.8(9) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 27.69 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 1.413 _refine_diff_density_min -0.799 _refine_diff_density_rms 0.138 #===end