# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2202 data_global _publ_contact_autor ; Fausto Calderazzo Dipartimento di Chimica e Chimica Industriale Universita' di Pisa Via Risorgimento, 35 56126 Pisa Italy ; _publ_contact_author_phone '+39 050 918218' _publ_contact_author_fax '+39 050 20237' _publ_contact_author_email 'facal@dcci.unipi.it' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Stepwise substitution of N,N-di-isopropylcarbamato groups of Ti(O2CNiPr2)4 by triphenylsilanol leading from octacoordinated to hexacoordinated and tetracoordinated titanium(IV) ; loop_ _publ_author_name _publ_author_address 'Belli Dell' Amico, Daniela' ; Dipartimento di Chimica e Chimica Industriale Universita'' di Pisa Via Risorgimento, 35 I-56126 Pisa Italy ; 'Calderazzo, Fausto' ; Dipartimento di Chimica e Chimica Industriale Universita'' di Pisa Via Risorgimento, 35 56126 Pisa Italy ; 'Ianelli, Sandra' ; Dipartimento di Chimica Generale ed Inorganica Chimica Analitica e Chimica Fisica Universita'' di Parma Parco Area delle Scienze I-43100 Parma Italy ; 'Labella, Luca' ; Dipartimento di Chimica e Chimica Industriale Universita'' di Pisa Via Risorgimento, 35 56126 Pisa Italy ; 'Marchetti, Fabio' ; Dipartimento di Ingegneria Chimica, dei Materiali e delle Materie Prime e Metallurgia Universita'' "La Sapienza" di Roma Via del Castro Laurenziano, 7 I-00161 Roma Italy ; 'Pelizzi, Giancarlo' ; Dipartimento di Chimica Generale ed Inorganica Chimica Analitica e Chimica Fisica Universita'' di Parma Parco Area delle Scienze I-43100 Parma Italy ; #======================================================================= data_ti4carbs1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetrakis-(N,N-diisopropylcarbamato)titanium(iv) ; _chemical_name_common ? _chemical_formula_moiety '(iPr2NCOO)4Ti' _chemical_formula_sum 'C28 H56 N4 O8 Ti' _chemical_formula_weight 624.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, z+1/2' '-x, -y, -z' '-x, y-1/2, -z-1/2' _cell_length_a 12.589(2) _cell_length_b 21.768(4) _cell_length_c 14.617(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.67(2) _cell_angle_gamma 90.00 _cell_volume 3696(1) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10.99 _cell_measurement_theta_max 18.85 _exptl_crystal_description Prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.123 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 0.277 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 1.05 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius CAD4 diffractometer' _diffrn_measurement_method '\w/2\q scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2100 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.1056 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 24.48 _reflns_number_total 6934 _reflns_number_gt 1999 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'molecular replacement' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F against observed reflections, with I>2sigma(I) ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme ? _atom_sites_solution_primary 'molecular replacement' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1999 _refine_ls_number_parameters 386 _refine_ls_number_restraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1052 _refine_ls_wR_factor_gt 0.1052 _refine_ls_goodness_of_fit_ref 0.631 _refine_ls_restrained_S_all 0.631 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti 0.28669(9) 0.36907(5) 0.23111(9) 0.0453(4) Uani 1 d . . . O1 O 0.1766(4) 0.41772(19) 0.2769(3) 0.0535(12) Uani 1 d . . . O2 O 0.3543(4) 0.40608(19) 0.3757(3) 0.0520(12) Uani 1 d . . . O3 O 0.2714(4) 0.29446(18) 0.3088(3) 0.0542(12) Uani 1 d . . . O4 O 0.1389(3) 0.3158(2) 0.1665(3) 0.0527(12) Uani 1 d . . . O5 O 0.4580(3) 0.33992(19) 0.2823(4) 0.0552(12) Uani 1 d . . . O6 O 0.3334(4) 0.3192(2) 0.1350(3) 0.0598(13) Uani 1 d . . . O7 O 0.1944(3) 0.41867(19) 0.1009(3) 0.0525(12) Uani 1 d . . . O8 O 0.3609(4) 0.44679(19) 0.2056(3) 0.0586(13) Uani 1 d . . . N1 N 0.2370(5) 0.4623(3) 0.4305(4) 0.0624(17) Uani 1 d . . . N2 N 0.1107(5) 0.2335(3) 0.2555(4) 0.0604(16) Uani 1 d . . . N3 N 0.5214(5) 0.2891(3) 0.1727(4) 0.0633(17) Uani 1 d . . . N4 N 0.2649(5) 0.5127(3) 0.0794(4) 0.0595(16) Uani 1 d . . . C1 C 0.2564(6) 0.4286(3) 0.3610(6) 0.0520(18) Uani 1 d . . . C2 C 0.1228(7) 0.4893(4) 0.4092(6) 0.084(3) Uani 1 d . . . H2 H 0.1290 0.5128 0.4683 0.100 Uiso 1 calc R . . C3 C 0.0882(8) 0.5345(4) 0.3246(7) 0.120(4) Uani 1 d . . . H3A H 0.1465 0.5656 0.3383 0.181 Uiso 1 calc R . . H3B H 0.0164 0.5534 0.3172 0.181 Uiso 1 calc R . . H3C H 0.0798 0.5134 0.2646 0.181 Uiso 1 calc R . . C4 C 0.0325(7) 0.4404(4) 0.3955(6) 0.111(3) Uani 1 d . . . H4A H 0.0235 0.4161 0.3381 0.167 Uiso 1 calc R . . H4B H -0.0395 0.4596 0.3865 0.167 Uiso 1 calc R . . H4C H 0.0562 0.4145 0.4530 0.167 Uiso 1 calc R . . C5 C 0.3322(7) 0.4746(5) 0.5261(6) 0.105(3) Uani 1 d . . . H5 H 0.3993 0.4512 0.5275 0.126 Uiso 1 calc R . . C6 C 0.3637(8) 0.5418(6) 0.5335(9) 0.203(7) Uani 1 d . . . H6A H 0.3740 0.5543 0.4745 0.304 Uiso 1 calc R . . H6B H 0.4340 0.5483 0.5901 0.304 Uiso 1 calc R . . H6C H 0.3032 0.5656 0.5407 0.304 Uiso 1 calc R . . C7 C 0.3018(8) 0.4524(7) 0.6117(6) 0.199(7) Uani 1 d . . . H7A H 0.2320 0.4718 0.6083 0.299 Uiso 1 calc R . . H7B H 0.3631 0.4626 0.6734 0.299 Uiso 1 calc R . . H7C H 0.2913 0.4086 0.6073 0.299 Uiso 1 calc R . . C8 C 0.1725(7) 0.2806(3) 0.2431(6) 0.0528(19) Uani 1 d . . . C9 C 0.0015(7) 0.2176(4) 0.1785(7) 0.088(3) Uani 1 d . . . H9 H -0.0253 0.1829 0.2066 0.106 Uiso 1 calc R . . C10 C 0.0130(8) 0.1908(4) 0.0879(6) 0.128(4) Uani 1 d . . . H10A H 0.0311 0.2229 0.0512 0.192 Uiso 1 calc R . . H10B H -0.0583 0.1717 0.0469 0.192 Uiso 1 calc R . . H10C H 0.0734 0.1607 0.1076 0.192 Uiso 1 calc R . . C11 C -0.0894(7) 0.2632(5) 0.1590(8) 0.141(4) Uani 1 d . . . H11A H -0.0849 0.2810 0.2205 0.212 Uiso 1 calc R . . H11B H -0.1630 0.2438 0.1268 0.212 Uiso 1 calc R . . H11C H -0.0802 0.2948 0.1168 0.212 Uiso 1 calc R . . C12 C 0.1547(7) 0.1995(4) 0.3537(6) 0.089(3) Uani 1 d . . . H12 H 0.2224 0.2228 0.3960 0.106 Uiso 1 calc R . . C13 C 0.1998(9) 0.1396(4) 0.3421(8) 0.168(5) Uani 1 d . . . H13A H 0.2416 0.1221 0.4062 0.252 Uiso 1 calc R . . H13B H 0.2503 0.1443 0.3073 0.252 Uiso 1 calc R . . H13C H 0.1371 0.1130 0.3050 0.252 Uiso 1 calc R . . C14 C 0.0755(10) 0.2027(7) 0.4040(7) 0.196(6) Uani 1 d . . . H14A H 0.0019 0.1868 0.3613 0.293 Uiso 1 calc R . . H14B H 0.0673 0.2446 0.4203 0.293 Uiso 1 calc R . . H14C H 0.1050 0.1787 0.4636 0.293 Uiso 1 calc R . . C15 C 0.4385(7) 0.3160(3) 0.1969(6) 0.060(2) Uani 1 d . . . C16 C 0.6403(7) 0.2951(4) 0.2393(7) 0.082(2) Uani 1 d . . . H16 H 0.6830 0.2740 0.2050 0.099 Uiso 1 calc R . . C17 C 0.6879(8) 0.3592(4) 0.2543(7) 0.124(4) Uani 1 d . . . H17A H 0.6709 0.3782 0.1910 0.187 Uiso 1 calc R . . H17B H 0.7697 0.3577 0.2901 0.187 Uiso 1 calc R . . H17C H 0.6534 0.3826 0.2913 0.187 Uiso 1 calc R . . C18 C 0.6710(7) 0.2607(5) 0.3341(6) 0.125(4) Uani 1 d . . . H18A H 0.6476 0.2839 0.3790 0.188 Uiso 1 calc R . . H18B H 0.7527 0.2543 0.3631 0.188 Uiso 1 calc R . . H18C H 0.6324 0.2217 0.3213 0.188 Uiso 1 calc R . . C19 C 0.4870(7) 0.2634(4) 0.0700(6) 0.078(2) Uani 1 d . . . H19 H 0.4027 0.2626 0.0416 0.094 Uiso 1 calc R . . C20 C 0.5225(9) 0.3070(5) 0.0053(7) 0.137(4) Uani 1 d . . . H20A H 0.6049 0.3097 0.0305 0.206 Uiso 1 calc R . . H20B H 0.4907 0.3470 0.0062 0.206 Uiso 1 calc R . . H20C H 0.4942 0.2918 -0.0615 0.206 Uiso 1 calc R . . C21 C 0.5235(9) 0.2005(4) 0.0700(7) 0.148(4) Uani 1 d . . . H21A H 0.6052 0.1976 0.1061 0.222 Uiso 1 calc R . . H21B H 0.5046 0.1871 0.0029 0.222 Uiso 1 calc R . . H21C H 0.4849 0.1748 0.1009 0.222 Uiso 1 calc R . . C22 C 0.2723(6) 0.4589(3) 0.1277(5) 0.0536(19) Uani 1 d . . . C23 C 0.3567(7) 0.5594(3) 0.1169(6) 0.074(2) Uani 1 d . . . H23 H 0.3315 0.5948 0.0723 0.088 Uiso 1 calc R . . C24 C 0.4669(7) 0.5372(4) 0.1116(6) 0.107(3) Uani 1 d . . . H24A H 0.4979 0.5044 0.1583 0.160 Uiso 1 calc R . . H24B H 0.5212 0.5704 0.1272 0.160 Uiso 1 calc R . . H24C H 0.4522 0.5225 0.0459 0.160 Uiso 1 calc R . . C25 C 0.3735(7) 0.5819(4) 0.2195(7) 0.112(3) Uani 1 d . . . H25A H 0.3012 0.5958 0.2196 0.169 Uiso 1 calc R . . H25B H 0.4276 0.6152 0.2378 0.169 Uiso 1 calc R . . H25C H 0.4024 0.5489 0.2663 0.169 Uiso 1 calc R . . C26 C 0.1594(7) 0.5285(4) -0.0067(6) 0.095(3) Uani 1 d . . . H26 H 0.1085 0.4927 -0.0209 0.114 Uiso 1 calc R . . C27 C 0.1830(11) 0.5412(5) -0.0987(6) 0.182(6) Uani 1 d . . . H27A H 0.2320 0.5765 -0.0877 0.273 Uiso 1 calc R . . H27B H 0.1116 0.5490 -0.1534 0.273 Uiso 1 calc R . . H27C H 0.2202 0.5063 -0.1133 0.273 Uiso 1 calc R . . C28 C 0.0967(7) 0.5819(4) 0.0212(8) 0.148(5) Uani 1 d . . . H28A H 0.0811 0.5707 0.0783 0.223 Uiso 1 calc R . . H28B H 0.0255 0.5904 -0.0334 0.223 Uiso 1 calc R . . H28C H 0.1445 0.6179 0.0360 0.223 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti 0.0471(7) 0.0432(7) 0.0468(7) 0.0007(7) 0.0196(6) -0.0019(7) O1 0.043(3) 0.065(3) 0.046(3) -0.002(3) 0.010(2) 0.008(2) O2 0.049(3) 0.056(3) 0.047(3) -0.006(2) 0.015(2) 0.001(2) O3 0.049(3) 0.050(3) 0.059(3) 0.009(2) 0.015(3) -0.004(2) O4 0.046(3) 0.058(3) 0.052(3) -0.003(3) 0.017(2) -0.003(2) O5 0.048(3) 0.055(3) 0.063(3) 0.001(3) 0.021(3) -0.001(2) O6 0.057(3) 0.069(3) 0.057(3) -0.007(3) 0.026(3) 0.003(3) O7 0.053(3) 0.046(3) 0.050(3) 0.004(2) 0.011(2) -0.008(2) O8 0.050(3) 0.060(3) 0.058(3) 0.011(3) 0.011(3) -0.006(2) N1 0.046(4) 0.082(5) 0.058(4) -0.014(4) 0.019(3) 0.016(3) N2 0.057(4) 0.050(4) 0.075(5) -0.007(3) 0.026(4) -0.019(3) N3 0.045(4) 0.065(4) 0.081(5) 0.000(4) 0.026(4) 0.003(3) N4 0.055(4) 0.054(4) 0.060(4) 0.010(3) 0.011(3) -0.016(3) C1 0.044(4) 0.050(5) 0.062(5) 0.011(4) 0.021(4) 0.006(4) C2 0.072(6) 0.109(7) 0.072(6) -0.027(6) 0.029(5) 0.015(6) C3 0.119(8) 0.085(7) 0.144(9) 0.002(7) 0.036(7) 0.049(6) C4 0.073(6) 0.178(10) 0.098(7) -0.002(7) 0.050(5) 0.001(7) C5 0.059(5) 0.166(10) 0.075(6) -0.054(7) 0.008(5) 0.004(6) C6 0.104(8) 0.245(15) 0.240(15) -0.179(13) 0.046(9) -0.058(9) C7 0.120(9) 0.42(2) 0.050(6) 0.000(10) 0.025(6) 0.051(11) C8 0.054(5) 0.048(5) 0.059(6) -0.005(4) 0.024(4) 0.004(4) C9 0.072(6) 0.081(6) 0.111(8) -0.007(6) 0.035(6) -0.020(5) C10 0.191(11) 0.128(9) 0.066(6) -0.011(7) 0.050(7) -0.032(8) C11 0.070(6) 0.188(11) 0.150(10) 0.033(9) 0.025(7) 0.020(7) C12 0.098(7) 0.076(7) 0.079(6) 0.036(5) 0.020(5) -0.015(5) C13 0.202(12) 0.082(8) 0.148(10) 0.006(7) -0.012(9) 0.042(8) C14 0.217(13) 0.309(18) 0.084(8) 0.063(10) 0.084(9) 0.057(12) C15 0.075(6) 0.046(5) 0.065(6) 0.012(4) 0.034(5) 0.002(5) C16 0.067(6) 0.079(7) 0.108(7) -0.012(6) 0.042(5) 0.002(5) C17 0.141(8) 0.111(8) 0.152(9) -0.053(7) 0.091(7) -0.070(7) C18 0.110(7) 0.153(9) 0.078(7) -0.007(7) -0.002(6) 0.004(7) C19 0.090(6) 0.086(7) 0.066(6) -0.017(5) 0.038(5) 0.019(5) C20 0.178(10) 0.147(10) 0.106(7) 0.036(8) 0.076(8) -0.005(8) C21 0.226(12) 0.079(7) 0.106(8) -0.015(6) 0.027(8) 0.004(8) C22 0.057(5) 0.053(5) 0.056(5) -0.006(4) 0.028(4) -0.012(4) C23 0.081(6) 0.052(5) 0.082(6) 0.008(5) 0.025(5) -0.014(5) C24 0.087(6) 0.127(8) 0.115(8) 0.015(6) 0.049(6) -0.025(6) C25 0.139(8) 0.067(6) 0.119(8) -0.021(6) 0.036(7) -0.010(6) C26 0.085(6) 0.078(7) 0.093(7) 0.020(6) 0.001(6) -0.034(5) C27 0.256(14) 0.183(11) 0.056(6) 0.040(7) 0.005(8) -0.093(10) C28 0.086(7) 0.120(9) 0.210(12) 0.061(9) 0.025(8) 0.029(7) _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 O8 2.035(4) . ? Ti O6 2.034(4) . ? Ti O3 2.033(4) . ? Ti O1 2.051(4) . ? Ti O4 2.084(4) . ? Ti O5 2.090(4) . ? Ti O7 2.106(4) . ? Ti O2 2.110(4) . ? Ti C22 2.435(8) . ? Ti C1 2.447(8) . ? Ti C15 2.444(8) . ? Ti C8 2.449(8) . ? O1 C1 1.274(7) . ? O2 C1 1.266(7) . ? O3 C8 1.281(7) . ? O4 C8 1.285(7) . ? O5 C15 1.285(8) . ? O6 C15 1.285(8) . ? O7 C22 1.260(7) . ? O8 C22 1.277(7) . ? N1 C1 1.349(8) . ? N1 C5 1.473(8) . ? N1 C2 1.471(8) . ? N2 C8 1.341(8) . ? N2 C9 1.444(8) . ? N2 C12 1.517(8) . ? N3 C15 1.357(8) . ? N3 C16 1.442(9) . ? N3 C19 1.501(8) . ? N4 C22 1.352(8) . ? N4 C23 1.476(8) . ? N4 C26 1.476(8) . ? C2 C4 1.514(10) . ? C2 C3 1.507(10) . ? C5 C6 1.508(13) . ? C5 C7 1.521(12) . ? C9 C11 1.458(10) . ? C9 C10 1.505(10) . ? C12 C13 1.457(11) . ? C12 C14 1.450(11) . ? C16 C18 1.489(10) . ? C16 C17 1.501(9) . ? C19 C21 1.444(10) . ? C19 C20 1.523(10) . ? C23 C25 1.514(9) . ? C23 C24 1.499(10) . ? C26 C27 1.509(11) . ? C26 C28 1.547(11) . ? 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 O8 Ti O6 92.37(18) . . ? O8 Ti O3 156.26(19) . . ? O6 Ti O3 94.29(18) . . ? O8 Ti O1 92.65(18) . . ? O6 Ti O1 155.94(19) . . ? O3 Ti O1 90.50(17) . . ? O8 Ti O4 140.56(19) . . ? O6 Ti O4 80.56(17) . . ? O3 Ti O4 63.14(17) . . ? O1 Ti O4 80.65(17) . . ? O8 Ti O5 80.49(17) . . ? O6 Ti O5 63.38(18) . . ? O3 Ti O5 82.21(16) . . ? O1 Ti O5 140.7(2) . . ? O4 Ti O5 127.66(18) . . ? O8 Ti O7 62.66(17) . . ? O6 Ti O7 81.65(18) . . ? O3 Ti O7 140.93(18) . . ? O1 Ti O7 79.83(17) . . ? O4 Ti O7 77.91(18) . . ? O5 Ti O7 127.80(17) . . ? O8 Ti O2 80.19(17) . . ? O6 Ti O2 141.55(19) . . ? O3 Ti O2 80.45(17) . . ? O1 Ti O2 62.51(17) . . ? O4 Ti O2 127.67(17) . . ? O5 Ti O2 78.18(19) . . ? O7 Ti O2 125.35(17) . . ? O8 Ti C22 31.62(18) . . ? O6 Ti C22 88.4(2) . . ? O3 Ti C22 171.0(2) . . ? O1 Ti C22 83.68(19) . . ? O4 Ti C22 109.0(2) . . ? O5 Ti C22 106.6(2) . . ? O7 Ti C22 31.15(17) . . ? O2 Ti C22 102.7(2) . . ? O8 Ti C1 85.51(19) . . ? O6 Ti C1 172.7(2) . . ? O3 Ti C1 85.00(19) . . ? O1 Ti C1 31.36(17) . . ? O4 Ti C1 105.5(2) . . ? O5 Ti C1 109.3(2) . . ? O7 Ti C1 103.5(2) . . ? O2 Ti C1 31.15(16) . . ? C22 Ti C1 93.4(2) . . ? O8 Ti C15 84.5(2) . . ? O6 Ti C15 31.71(19) . . ? O3 Ti C15 89.23(19) . . ? O1 Ti C15 172.3(3) . . ? O4 Ti C15 106.1(2) . . ? O5 Ti C15 31.72(19) . . ? O7 Ti C15 105.1(2) . . ? O2 Ti C15 109.8(2) . . ? C22 Ti C15 97.5(2) . . ? C1 Ti C15 141.0(3) . . ? O8 Ti C8 171.9(2) . . ? O6 Ti C8 88.0(2) . . ? O3 Ti C8 31.52(18) . . ? O1 Ti C8 83.87(19) . . ? O4 Ti C8 31.65(18) . . ? O5 Ti C8 106.8(2) . . ? O7 Ti C8 109.4(2) . . ? O2 Ti C8 104.5(2) . . ? C22 Ti C8 140.4(3) . . ? C1 Ti C8 95.1(2) . . ? C15 Ti C8 99.8(2) . . ? C1 O1 Ti 91.7(4) . . ? C1 O2 Ti 89.3(4) . . ? C8 O3 Ti 92.5(4) . . ? C8 O4 Ti 90.0(4) . . ? C15 O5 Ti 89.5(4) . . ? C15 O6 Ti 92.0(4) . . ? C22 O7 Ti 89.0(4) . . ? C22 O8 Ti 91.7(4) . . ? C1 N1 C5 119.7(6) . . ? C1 N1 C2 120.3(6) . . ? C5 N1 C2 119.9(6) . . ? C8 N2 C9 120.3(6) . . ? C8 N2 C12 118.9(6) . . ? C9 N2 C12 120.8(6) . . ? C15 N3 C16 119.1(7) . . ? C15 N3 C19 117.9(6) . . ? C16 N3 C19 122.2(6) . . ? C22 N4 C23 121.1(6) . . ? C22 N4 C26 120.4(6) . . ? C23 N4 C26 118.3(6) . . ? O2 C1 O1 116.5(7) . . ? O2 C1 N1 122.0(7) . . ? O1 C1 N1 121.5(6) . . ? O2 C1 Ti 59.6(4) . . ? O1 C1 Ti 56.9(4) . . ? N1 C1 Ti 178.3(5) . . ? N1 C2 C4 111.7(7) . . ? N1 C2 C3 112.6(7) . . ? C4 C2 C3 112.7(7) . . ? N1 C5 C6 109.9(9) . . ? N1 C5 C7 110.5(8) . . ? C6 C5 C7 113.1(9) . . ? O3 C8 O4 114.3(7) . . ? O3 C8 N2 121.6(7) . . ? O4 C8 N2 124.1(7) . . ? O3 C8 Ti 56.0(4) . . ? O4 C8 Ti 58.3(4) . . ? N2 C8 Ti 176.3(5) . . ? N2 C9 C11 115.4(8) . . ? N2 C9 C10 113.2(7) . . ? C11 C9 C10 115.2(9) . . ? C13 C12 C14 118.5(9) . . ? C13 C12 N2 110.0(8) . . ? C14 C12 N2 112.6(7) . . ? O5 C15 O6 114.9(7) . . ? O5 C15 N3 123.4(7) . . ? O6 C15 N3 121.7(7) . . ? O5 C15 Ti 58.8(4) . . ? O6 C15 Ti 56.2(4) . . ? N3 C15 Ti 176.2(5) . . ? N3 C16 C18 114.4(7) . . ? N3 C16 C17 115.7(7) . . ? C18 C16 C17 112.7(8) . . ? C21 C19 N3 112.6(7) . . ? C21 C19 C20 115.0(8) . . ? N3 C19 C20 110.3(7) . . ? O7 C22 O8 116.2(7) . . ? O7 C22 N4 123.5(7) . . ? O8 C22 N4 120.3(6) . . ? O7 C22 Ti 59.8(4) . . ? O8 C22 Ti 56.7(4) . . ? N4 C22 Ti 173.4(5) . . ? N4 C23 C25 112.4(6) . . ? N4 C23 C24 111.5(7) . . ? C25 C23 C24 112.1(7) . . ? N4 C26 C27 112.5(8) . . ? N4 C26 C28 109.5(7) . . ? C27 C26 C28 113.1(8) . . ? _diffrn_measured_fraction_theta_max 0.323 _diffrn_reflns_theta_full 24.48 _diffrn_measured_fraction_theta_full 0.323 _refine_diff_density_max 0.160 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.040 #===END data_carbati _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-(N,N-diisopropylcarbamato)bis(triphenylsilanolato)titanium(iv) ; _chemical_name_common ? _chemical_formula_moiety '(iPr2NCOO)2(Ph3SiO)2Ti' _chemical_formula_sum 'C50 H58 N2 O6 Si2 Ti' _chemical_formula_weight 887.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 11.0030(10) _cell_length_b 13.298(2) _cell_length_c 18.403(3) _cell_angle_alpha 83.630(10) _cell_angle_beta 84.050(10) _cell_angle_gamma 66.800(10) _cell_volume 2454.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 26 _cell_measurement_theta_min 5.72 _cell_measurement_theta_max 12.25 _exptl_crystal_description 'Plate' _exptl_crystal_colour 'Colourless' _exptl_crystal_size_max 0.86 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.200 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 940 _exptl_absorpt_coefficient_mu 0.271 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.8321 _exptl_absorpt_correction_T_max 0.8661 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6801 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.1024 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 22.50 _reflns_number_total 6398 _reflns_number_gt 3358 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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 w=1/[\s^2^(Fo^2^)+(0.0545P)^2^+0.1784P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6398 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1439 _refine_ls_R_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.1508 _refine_ls_wR_factor_gt 0.1191 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.002 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti 0.01007(11) 0.63452(8) 0.26498(6) 0.0529(3) Uani 1 d . . . Si1 Si -0.26476(16) 0.86231(12) 0.29579(8) 0.0483(4) Uani 1 d . . . Si2 Si 0.00152(17) 0.40226(13) 0.21762(9) 0.0556(5) Uani 1 d . . . O1 O 0.1013(4) 0.7492(3) 0.2468(2) 0.0712(12) Uani 1 d . . . O2 O 0.0699(4) 0.6625(3) 0.1618(2) 0.0679(12) Uani 1 d . . . O3 O 0.2042(4) 0.5256(3) 0.2892(2) 0.0633(11) Uani 1 d . . . O4 O 0.0483(4) 0.6063(3) 0.37121(19) 0.0582(11) Uani 1 d . . . O5 O -0.1516(4) 0.7414(3) 0.28018(19) 0.0578(11) Uani 1 d . . . O6 O -0.0318(4) 0.5240(3) 0.2449(2) 0.0622(11) Uani 1 d . . . C1 C 0.1152(7) 0.7327(5) 0.1791(4) 0.0685(19) Uani 1 d . . . N1 N 0.1728(6) 0.7823(5) 0.1287(3) 0.0897(19) Uani 1 d . . . C2 C 0.2149(13) 0.8664(9) 0.1502(7) 0.157(5) Uani 1 d . . . H2 H 0.2365 0.8866 0.0991 0.204 Uiso 1 calc R . . C3 C 0.3407(17) 0.8333(12) 0.1672(9) 0.283(11) Uani 1 d . . . H3A H 0.3907 0.7613 0.1511 0.368 Uiso 1 calc R . . H3B H 0.3437 0.8314 0.2193 0.368 Uiso 1 calc R . . H3C H 0.3782 0.8836 0.1434 0.368 Uiso 1 calc R . . C4 C 0.1066(14) 0.9726(8) 0.1579(6) 0.214(7) Uani 1 d . . . H4A H 0.0304 0.9738 0.1361 0.279 Uiso 1 calc R . . H4B H 0.1328 1.0293 0.1337 0.279 Uiso 1 calc R . . H4C H 0.0850 0.9847 0.2089 0.279 Uiso 1 calc R . . C5 C 0.1898(10) 0.7596(8) 0.0510(4) 0.126(4) Uani 1 d . . . H5 H 0.1472 0.7070 0.0625 0.164 Uiso 1 calc R . . C6 C 0.3079(10) 0.6750(9) 0.0309(5) 0.167(5) Uani 1 d . . . H6A H 0.3567 0.6419 0.0735 0.217 Uiso 1 calc R . . H6B H 0.3596 0.7038 -0.0039 0.217 Uiso 1 calc R . . H6C H 0.2889 0.6209 0.0091 0.217 Uiso 1 calc R . . C7 C 0.0849(9) 0.8265(8) 0.0068(5) 0.147(4) Uani 1 d . . . H7A H 0.0138 0.8747 0.0368 0.191 Uiso 1 calc R . . H7B H 0.0534 0.7809 -0.0164 0.191 Uiso 1 calc R . . H7C H 0.1163 0.8692 -0.0300 0.191 Uiso 1 calc R . . C8 C 0.1718(6) 0.5420(4) 0.3570(3) 0.0552(15) Uani 1 d . . . N2 N 0.2540(4) 0.4955(4) 0.4105(3) 0.0554(13) Uani 1 d . . . C9 C 0.2067(6) 0.5211(4) 0.4869(3) 0.0576(16) Uani 1 d . . . H9 H 0.1097 0.5552 0.4881 0.075 Uiso 1 calc R . . C10 C 0.2533(8) 0.6059(6) 0.5092(4) 0.102(3) Uani 1 d . . . H10A H 0.2264 0.6690 0.4747 0.133 Uiso 1 calc R . . H10B H 0.3482 0.5750 0.5098 0.133 Uiso 1 calc R . . H10C H 0.2149 0.6272 0.5571 0.133 Uiso 1 calc R . . C11 C 0.2419(7) 0.4199(5) 0.5392(4) 0.091(2) Uani 1 d . . . H11A H 0.2071 0.3706 0.5236 0.118 Uiso 1 calc R . . H11B H 0.2046 0.4402 0.5875 0.118 Uiso 1 calc R . . H11C H 0.3366 0.3843 0.5400 0.118 Uiso 1 calc R . . C12 C 0.3952(6) 0.4285(5) 0.3927(4) 0.0709(19) Uani 1 d . . . H12 H 0.4368 0.4028 0.4395 0.092 Uiso 1 calc R . . C13 C 0.4662(7) 0.4954(7) 0.3498(4) 0.103(3) Uani 1 d . . . H13A H 0.4530 0.5581 0.3757 0.134 Uiso 1 calc R . . H13B H 0.4313 0.5194 0.3024 0.134 Uiso 1 calc R . . H13C H 0.5592 0.4511 0.3442 0.134 Uiso 1 calc R . . C14 C 0.4145(6) 0.3271(5) 0.3552(4) 0.086(2) Uani 1 d . . . H14A H 0.3703 0.2857 0.3847 0.112 Uiso 1 calc R . . H14B H 0.5074 0.2827 0.3491 0.112 Uiso 1 calc R . . H14C H 0.3780 0.3485 0.3081 0.112 Uiso 1 calc R . . C1S C -0.1585(7) 0.3933(6) 0.2015(3) 0.0715(19) Uani 1 d . . . C2S C -0.2689(9) 0.4876(8) 0.1865(5) 0.118(3) Uani 1 d . . . H2S H -0.2633 0.5556 0.1864 0.154 Uiso 1 calc R . . C3S C -0.3881(12) 0.4832(14) 0.1714(7) 0.174(6) Uani 1 d . . . H3S H -0.4620 0.5470 0.1618 0.227 Uiso 1 calc R . . C4S C -0.3932(15) 0.3804(16) 0.1712(6) 0.175(8) Uani 1 d . . . H4S H -0.4709 0.3760 0.1592 0.227 Uiso 1 calc R . . C5S C -0.2887(14) 0.2864(13) 0.1879(5) 0.156(5) Uani 1 d . . . H5S H -0.2951 0.2184 0.1905 0.203 Uiso 1 calc R . . C6S C -0.1722(9) 0.2956(8) 0.2008(4) 0.102(3) Uani 1 d . . . H6S H -0.0985 0.2313 0.2095 0.133 Uiso 1 calc R . . C7S C 0.1075(6) 0.3814(5) 0.1307(3) 0.0596(16) Uani 1 d . . . C8S C 0.0664(8) 0.3640(7) 0.0671(4) 0.103(3) Uani 1 d . . . H8S H -0.0164 0.3604 0.0679 0.134 Uiso 1 calc R . . C9S C 0.1433(11) 0.3518(9) 0.0020(5) 0.135(4) Uani 1 d . . . H9S H 0.1112 0.3424 -0.0405 0.175 Uiso 1 calc R . . C10S C 0.2672(10) 0.3535(7) 0.0002(5) 0.110(3) Uani 1 d . . . H10S H 0.3213 0.3417 -0.0429 0.143 Uiso 1 calc R . . C11S C 0.3109(8) 0.3725(7) 0.0618(5) 0.100(3) Uani 1 d . . . H11S H 0.3941 0.3756 0.0607 0.130 Uiso 1 calc R . . C12S C 0.2313(7) 0.3872(6) 0.1258(4) 0.080(2) Uani 1 d . . . H12S H 0.2616 0.4016 0.1673 0.105 Uiso 1 calc R . . C13S C 0.0876(6) 0.2972(4) 0.2913(3) 0.0551(16) Uani 1 d . . . C14S C 0.1732(7) 0.1914(5) 0.2772(4) 0.077(2) Uani 1 d . . . H14S H 0.1921 0.1717 0.2291 0.100 Uiso 1 calc R . . C15S C 0.2315(7) 0.1138(5) 0.3342(5) 0.094(2) Uani 1 d . . . H15S H 0.2906 0.0438 0.3237 0.122 Uiso 1 calc R . . C16S C 0.2023(7) 0.1399(6) 0.4049(5) 0.087(2) Uani 1 d . . . H16S H 0.2395 0.0870 0.4425 0.113 Uiso 1 calc R . . C17S C 0.1187(7) 0.2434(6) 0.4212(4) 0.079(2) Uani 1 d . . . H17S H 0.0998 0.2620 0.4695 0.102 Uiso 1 calc R . . C18S C 0.0621(6) 0.3205(5) 0.3636(4) 0.0661(18) Uani 1 d . . . H18S H 0.0047 0.3908 0.3747 0.086 Uiso 1 calc R . . C19S C -0.3324(6) 0.9334(4) 0.2070(3) 0.0521(15) Uani 1 d . . . C20S C -0.4480(6) 1.0269(5) 0.2042(4) 0.077(2) Uani 1 d . . . H20S H -0.4946 1.0530 0.2479 0.101 Uiso 1 calc R . . C21S C -0.4963(8) 1.0828(6) 0.1387(5) 0.102(3) Uani 1 d . . . H21S H -0.5725 1.1468 0.1387 0.133 Uiso 1 calc R . . C22S C -0.4328(9) 1.0442(8) 0.0745(5) 0.109(3) Uani 1 d . . . H22S H -0.4665 1.0810 0.0305 0.141 Uiso 1 calc R . . C23S C -0.3184(9) 0.9509(8) 0.0741(4) 0.120(3) Uani 1 d . . . H23S H -0.2740 0.9244 0.0301 0.155 Uiso 1 calc R . . C24S C -0.2702(7) 0.8966(6) 0.1408(4) 0.091(2) Uani 1 d . . . H24S H -0.1932 0.8333 0.1404 0.118 Uiso 1 calc R . . C25S C -0.1903(6) 0.9438(5) 0.3383(3) 0.0516(15) Uani 1 d . . . C26S C -0.2456(7) 1.0576(5) 0.3323(4) 0.080(2) Uani 1 d . . . H26S H -0.3218 1.0935 0.3069 0.104 Uiso 1 calc R . . C27S C -0.1909(9) 1.1195(6) 0.3628(5) 0.098(3) Uani 1 d . . . H27S H -0.2306 1.1957 0.3580 0.127 Uiso 1 calc R . . C28S C -0.0817(9) 1.0698(8) 0.3988(5) 0.102(3) Uani 1 d . . . H28S H -0.0436 1.1114 0.4181 0.133 Uiso 1 calc R . . C29S C -0.0247(7) 0.9577(8) 0.4076(5) 0.109(3) Uani 1 d . . . H29S H 0.0508 0.9233 0.4338 0.141 Uiso 1 calc R . . C30S C -0.0795(7) 0.8958(6) 0.3777(4) 0.089(2) Uani 1 d . . . H30S H -0.0405 0.8196 0.3843 0.116 Uiso 1 calc R . . C31S C -0.4027(6) 0.8479(4) 0.3580(3) 0.0507(15) Uani 1 d . . . C32S C -0.4888(7) 0.8056(5) 0.3343(4) 0.0711(18) Uani 1 d . . . H32S H -0.4759 0.7831 0.2871 0.092 Uiso 1 calc R . . C33S C -0.5933(8) 0.7969(6) 0.3804(5) 0.086(2) Uani 1 d . . . H33S H -0.6500 0.7694 0.3636 0.112 Uiso 1 calc R . . C34S C -0.6129(7) 0.8282(6) 0.4495(5) 0.084(2) Uani 1 d . . . H34S H -0.6835 0.8222 0.4795 0.110 Uiso 1 calc R . . C35S C -0.5315(8) 0.8684(5) 0.4761(4) 0.077(2) Uani 1 d . . . H35S H -0.5446 0.8888 0.5240 0.100 Uiso 1 calc R . . C36S C -0.4283(6) 0.8780(4) 0.4295(3) 0.0591(16) Uani 1 d . . . H36S H -0.3731 0.9063 0.4473 0.077 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti 0.0592(7) 0.0381(6) 0.0504(7) -0.0023(5) -0.0037(5) -0.0073(5) Si1 0.0518(10) 0.0372(8) 0.0481(10) -0.0014(7) -0.0107(8) -0.0077(8) Si2 0.0549(11) 0.0482(9) 0.0606(11) -0.0079(8) 0.0014(9) -0.0169(8) O1 0.098(3) 0.062(3) 0.057(3) -0.009(2) 0.007(2) -0.036(2) O2 0.090(3) 0.055(3) 0.050(3) -0.006(2) -0.002(2) -0.019(2) O3 0.060(3) 0.056(2) 0.055(3) -0.005(2) 0.001(2) -0.003(2) O4 0.049(3) 0.055(2) 0.052(2) -0.0003(19) -0.0015(19) -0.001(2) O5 0.062(3) 0.042(2) 0.054(2) -0.0054(17) -0.011(2) -0.0017(19) O6 0.067(3) 0.042(2) 0.069(3) -0.0055(19) -0.002(2) -0.012(2) C1 0.080(5) 0.050(4) 0.052(5) 0.004(3) 0.006(4) -0.005(4) N1 0.114(5) 0.064(4) 0.073(4) 0.016(3) 0.011(4) -0.025(4) C2 0.182(12) 0.096(8) 0.202(13) -0.009(8) 0.068(10) -0.084(9) C3 0.34(2) 0.243(18) 0.32(2) -0.011(14) -0.24(2) -0.117(17) C4 0.35(2) 0.096(8) 0.173(11) -0.031(7) -0.085(12) -0.035(11) C5 0.119(8) 0.135(8) 0.068(6) 0.035(5) 0.024(5) -0.007(6) C6 0.155(10) 0.184(11) 0.117(8) -0.060(8) -0.014(7) -0.004(9) C7 0.147(9) 0.134(8) 0.167(9) -0.023(7) -0.076(8) -0.042(7) C8 0.054(4) 0.045(3) 0.057(4) -0.002(3) 0.005(3) -0.011(3) N2 0.043(3) 0.055(3) 0.054(3) 0.002(2) -0.012(3) -0.003(2) C9 0.069(4) 0.058(4) 0.047(4) 0.001(3) -0.012(3) -0.025(3) C10 0.123(7) 0.108(6) 0.095(6) -0.021(5) 0.000(5) -0.064(6) C11 0.104(6) 0.083(5) 0.074(5) 0.012(4) -0.001(4) -0.029(4) C12 0.048(4) 0.080(5) 0.073(4) 0.000(4) -0.007(3) -0.012(4) C13 0.078(5) 0.118(6) 0.115(6) -0.017(5) 0.018(5) -0.045(5) C14 0.061(5) 0.064(4) 0.107(6) -0.008(4) -0.005(4) 0.006(4) C1S 0.064(5) 0.098(5) 0.063(4) -0.007(4) -0.005(4) -0.041(5) C2S 0.070(6) 0.159(9) 0.114(7) 0.027(6) -0.020(5) -0.038(6) C3S 0.080(8) 0.291(19) 0.143(10) 0.047(11) -0.035(7) -0.072(10) C4S 0.145(12) 0.38(3) 0.059(6) 0.039(10) -0.025(7) -0.176(17) C5S 0.192(13) 0.277(17) 0.092(7) 0.015(9) -0.034(8) -0.191(13) C6S 0.111(7) 0.144(8) 0.090(6) -0.016(5) -0.003(5) -0.089(6) C7S 0.067(5) 0.052(4) 0.064(4) -0.009(3) 0.000(3) -0.026(3) C8S 0.107(6) 0.156(8) 0.076(5) -0.050(5) 0.027(5) -0.080(6) C9S 0.142(9) 0.203(11) 0.077(7) -0.057(6) 0.013(6) -0.079(9) C10S 0.113(8) 0.125(7) 0.073(6) -0.009(5) 0.026(6) -0.032(6) C11S 0.075(6) 0.122(7) 0.091(6) -0.006(5) 0.020(5) -0.032(5) C12S 0.072(5) 0.092(5) 0.074(5) -0.021(4) 0.012(4) -0.029(4) C13S 0.059(4) 0.042(3) 0.067(4) -0.007(3) -0.001(3) -0.024(3) C14S 0.081(5) 0.053(4) 0.086(5) -0.015(4) 0.006(4) -0.016(4) C15S 0.082(6) 0.046(4) 0.128(7) 0.008(5) 0.006(5) -0.003(4) C16S 0.070(5) 0.079(6) 0.110(7) 0.018(5) -0.025(5) -0.029(4) C17S 0.096(6) 0.066(5) 0.079(5) 0.009(4) -0.021(4) -0.037(4) C18S 0.071(5) 0.048(4) 0.076(5) -0.009(3) 0.001(4) -0.019(3) C19S 0.048(4) 0.052(3) 0.053(4) -0.003(3) -0.006(3) -0.015(3) C20S 0.068(5) 0.063(4) 0.080(5) 0.010(4) -0.014(4) -0.004(4) C21S 0.085(6) 0.091(6) 0.106(7) 0.036(5) -0.037(6) -0.013(5) C22S 0.113(8) 0.125(7) 0.078(6) 0.046(6) -0.043(6) -0.041(6) C23S 0.111(7) 0.149(8) 0.060(5) 0.003(5) -0.010(5) -0.011(6) C24S 0.084(5) 0.105(6) 0.053(4) 0.010(4) -0.014(4) -0.006(4) C25S 0.049(4) 0.058(4) 0.044(3) -0.010(3) -0.004(3) -0.014(3) C26S 0.086(5) 0.057(4) 0.103(6) -0.002(4) -0.031(4) -0.027(4) C27S 0.116(7) 0.078(5) 0.125(7) -0.012(5) -0.017(6) -0.061(6) C28S 0.080(6) 0.127(8) 0.132(8) -0.057(6) 0.009(5) -0.065(6) C29S 0.064(5) 0.130(8) 0.126(7) -0.061(6) -0.030(5) -0.012(5) C30S 0.086(6) 0.076(5) 0.088(5) -0.031(4) -0.036(5) 0.000(4) C31S 0.059(4) 0.038(3) 0.050(4) 0.003(3) -0.015(3) -0.011(3) C32S 0.081(5) 0.072(4) 0.067(4) 0.000(3) -0.017(4) -0.036(4) C33S 0.081(6) 0.083(5) 0.105(6) 0.009(5) -0.005(5) -0.049(4) C34S 0.074(5) 0.065(5) 0.102(7) 0.011(4) 0.012(5) -0.022(4) C35S 0.089(6) 0.063(4) 0.067(5) -0.005(3) 0.023(4) -0.024(4) C36S 0.071(5) 0.049(3) 0.058(4) -0.005(3) -0.011(4) -0.022(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti O6 1.788(4) . ? Ti O5 1.804(4) . ? Ti O2 1.988(4) . ? Ti O4 2.006(4) . ? Ti O1 2.114(4) . ? Ti O3 2.115(4) . ? Ti C1 2.428(7) . ? Ti C8 2.447(6) . ? Si1 O5 1.634(4) . ? Si1 C31S 1.863(6) . ? Si1 C19S 1.864(6) . ? Si1 C25S 1.865(6) . ? Si2 O6 1.638(4) . ? Si2 C7S 1.858(6) . ? Si2 C1S 1.866(7) . ? Si2 C13S 1.869(6) . ? O1 C1 1.273(7) . ? O2 C1 1.300(8) . ? O3 C8 1.281(6) . ? O4 C8 1.306(6) . ? C1 N1 1.329(8) . ? N1 C2 1.472(12) . ? N1 C5 1.473(9) . ? C2 C3 1.337(15) . ? C2 C4 1.456(14) . ? C5 C6 1.390(10) . ? C5 C7 1.418(10) . ? C8 N2 1.333(7) . ? N2 C9 1.477(7) . ? N2 C12 1.478(7) . ? C9 C11 1.506(8) . ? C9 C10 1.518(8) . ? C12 C13 1.513(9) . ? C12 C14 1.513(8) . ? C1S C6S 1.368(10) . ? C1S C2S 1.385(10) . ? C2S C3S 1.393(13) . ? C3S C4S 1.391(18) . ? C4S C5S 1.354(18) . ? C5S C6S 1.380(12) . ? C7S C8S 1.373(9) . ? C7S C12S 1.387(8) . ? C8S C9S 1.379(11) . ? C9S C10S 1.369(11) . ? C10S C11S 1.361(11) . ? C11S C12S 1.376(9) . ? C13S C18S 1.375(8) . ? C13S C14S 1.386(8) . ? C14S C15S 1.399(9) . ? C15S C16S 1.356(10) . ? C16S C17S 1.366(9) . ? C17S C18S 1.398(8) . ? C19S C24S 1.373(8) . ? C19S C20S 1.386(8) . ? C20S C21S 1.383(9) . ? C21S C22S 1.351(11) . ? C22S C23S 1.376(11) . ? C23S C24S 1.395(9) . ? C25S C30S 1.373(8) . ? C25S C26S 1.387(8) . ? C26S C27S 1.385(9) . ? C27S C28S 1.327(10) . ? C28S C29S 1.368(11) . ? C29S C30S 1.381(10) . ? C31S C36S 1.387(7) . ? C31S C32S 1.400(8) . ? C32S C33S 1.392(9) . ? C33S C34S 1.351(9) . ? C34S C35S 1.362(9) . ? C35S C36S 1.389(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Ti O5 101.62(18) . . ? O6 Ti O2 93.82(19) . . ? O5 Ti O2 105.93(17) . . ? O6 Ti O4 105.40(17) . . ? O5 Ti O4 94.58(16) . . ? O2 Ti O4 148.47(18) . . ? O6 Ti O1 156.58(17) . . ? O5 Ti O1 92.00(17) . . ? O2 Ti O1 63.90(17) . . ? O4 Ti O1 92.24(17) . . ? O6 Ti O3 91.65(17) . . ? O5 Ti O3 157.16(16) . . ? O2 Ti O3 91.45(17) . . ? O4 Ti O3 63.74(15) . . ? O1 Ti O3 82.31(17) . . ? O6 Ti C1 125.8(2) . . ? O5 Ti C1 100.46(19) . . ? O2 Ti C1 32.31(18) . . ? O4 Ti C1 121.3(2) . . ? O1 Ti C1 31.59(19) . . ? O3 Ti C1 86.24(19) . . ? O6 Ti C8 100.79(18) . . ? O5 Ti C8 126.30(19) . . ? O2 Ti C8 120.4(2) . . ? O4 Ti C8 32.22(16) . . ? O1 Ti C8 85.85(18) . . ? O3 Ti C8 31.55(15) . . ? C1 Ti C8 104.6(2) . . ? O5 Si1 C31S 110.1(2) . . ? O5 Si1 C19S 108.5(2) . . ? C31S Si1 C19S 108.6(3) . . ? O5 Si1 C25S 109.8(2) . . ? C31S Si1 C25S 109.7(3) . . ? C19S Si1 C25S 110.1(3) . . ? O6 Si2 C7S 110.7(2) . . ? O6 Si2 C1S 108.0(3) . . ? C7S Si2 C1S 108.9(3) . . ? O6 Si2 C13S 108.2(2) . . ? C7S Si2 C13S 110.4(3) . . ? C1S Si2 C13S 110.6(3) . . ? C1 O1 Ti 88.0(4) . . ? C1 O2 Ti 92.8(4) . . ? C8 O3 Ti 88.7(3) . . ? C8 O4 Ti 92.8(3) . . ? Si1 O5 Ti 159.6(3) . . ? Si2 O6 Ti 154.2(3) . . ? O1 C1 O2 115.3(6) . . ? O1 C1 N1 123.3(7) . . ? O2 C1 N1 121.4(6) . . ? O1 C1 Ti 60.4(3) . . ? O2 C1 Ti 54.9(3) . . ? N1 C1 Ti 176.2(6) . . ? C1 N1 C2 119.4(7) . . ? C1 N1 C5 121.9(7) . . ? C2 N1 C5 118.6(7) . . ? C3 C2 C4 129.0(13) . . ? C3 C2 N1 117.1(11) . . ? C4 C2 N1 113.5(11) . . ? C6 C5 C7 128.7(9) . . ? C6 C5 N1 115.0(8) . . ? C7 C5 N1 116.2(8) . . ? O3 C8 O4 114.7(5) . . ? O3 C8 N2 124.0(5) . . ? O4 C8 N2 121.3(5) . . ? O3 C8 Ti 59.8(3) . . ? O4 C8 Ti 55.0(3) . . ? N2 C8 Ti 176.2(4) . . ? C8 N2 C9 119.5(5) . . ? C8 N2 C12 120.2(5) . . ? C9 N2 C12 119.9(5) . . ? N2 C9 C11 112.6(5) . . ? N2 C9 C10 110.2(5) . . ? C11 C9 C10 113.1(5) . . ? N2 C12 C13 112.1(5) . . ? N2 C12 C14 112.5(5) . . ? C13 C12 C14 111.9(6) . . ? C6S C1S C2S 116.7(7) . . ? C6S C1S Si2 122.8(6) . . ? C2S C1S Si2 120.4(6) . . ? C1S C2S C3S 121.7(11) . . ? C4S C3S C2S 117.9(14) . . ? C5S C4S C3S 122.1(14) . . ? C4S C5S C6S 117.4(13) . . ? C1S C6S C5S 124.1(10) . . ? C8S C7S C12S 116.0(6) . . ? C8S C7S Si2 122.3(5) . . ? C12S C7S Si2 121.7(5) . . ? C7S C8S C9S 122.5(8) . . ? C10S C9S C8S 119.6(8) . . ? C11S C10S C9S 119.8(8) . . ? C10S C11S C12S 119.6(8) . . ? C11S C12S C7S 122.5(7) . . ? C18S C13S C14S 116.7(6) . . ? C18S C13S Si2 120.5(4) . . ? C14S C13S Si2 122.6(5) . . ? C13S C14S C15S 120.8(7) . . ? C16S C15S C14S 120.5(7) . . ? C15S C16S C17S 120.5(7) . . ? C16S C17S C18S 118.5(7) . . ? C13S C18S C17S 122.9(6) . . ? C24S C19S C20S 116.4(6) . . ? C24S C19S Si1 122.0(5) . . ? C20S C19S Si1 121.6(5) . . ? C21S C20S C19S 122.1(7) . . ? C22S C21S C20S 119.9(7) . . ? C21S C22S C23S 120.3(7) . . ? C22S C23S C24S 118.9(8) . . ? C19S C24S C23S 122.3(7) . . ? C30S C25S C26S 116.1(6) . . ? C30S C25S Si1 122.6(5) . . ? C26S C25S Si1 121.3(5) . . ? C27S C26S C25S 122.1(7) . . ? C28S C27S C26S 119.8(7) . . ? C27S C28S C29S 120.4(7) . . ? C28S C29S C30S 119.9(7) . . ? C25S C30S C29S 121.6(7) . . ? C36S C31S C32S 115.5(6) . . ? C36S C31S Si1 123.3(5) . . ? C32S C31S Si1 121.1(5) . . ? C33S C32S C31S 121.0(6) . . ? C34S C33S C32S 120.4(7) . . ? C33S C34S C35S 121.4(7) . . ? C34S C35S C36S 117.8(7) . . ? C31S C36S C35S 123.8(6) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.311 _refine_diff_density_min -0.191 _refine_diff_density_rms 0.046 #===END