# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2004 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Prof Ulrich Schubert' _publ_contact_author_address ; Institute of Materials Chemistry Vienna University of Technology Getreidemarkt 9 Wien A-1060 AUSTRIA ; _publ_contact_author_phone '+43 1 58801 15320' _publ_contact_author_fax '+43 1 58801 15399' _publ_contact_author_email uschuber@mail.zserv.tuwien.ac.at _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #==================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Amine Adducts of Titanium Tetraalkoxides ; loop_ _publ_author_name _publ_author_address 'Helmut Fric' ; Institut fur Materialchemie Technische Universitat Wien Getreidemarkt 9 A-1060 Wien Austria ; 'Ulrich Schubert' ; Institut fur Materialchemie Technische Universitat Wien Getreidemarkt 9 A-1060 Wien Austria ; #============================================================================== data_prnh2 _database_code_depnum_ccdc_archive 'CCDC 245949' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H74 N2 O8 Ti2' _chemical_formula_weight 686.71 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.0686(7) _cell_length_b 17.8421(12) _cell_length_c 12.4515(8) _cell_angle_alpha 90.00 _cell_angle_beta 113.4270(10) _cell_angle_gamma 90.00 _cell_volume 2052.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8535 _cell_measurement_theta_min 4.961 _cell_measurement_theta_max 56.474 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.91 _exptl_crystal_size_mid 0.63 _exptl_crystal_size_min 0.43 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.111 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 0.430 _exptl_absorpt_correction_type ¥SADABS¥ _exptl_absorpt_correction_T_min 0.6958 _exptl_absorpt_correction_T_max 0.8368 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker-AXS APEX CCD Detector' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time 20 _diffrn_standards_decay_% ? _diffrn_reflns_number 10890 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0238 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3585 _reflns_number_gt 3253 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-AXS SMART Software' _computing_cell_refinement 'Bruker-AXS SAINT Software' _computing_data_reduction 'Bruker-AXS SAINT Software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker-AXS SHELXTL Software' _computing_publication_material 'Bruker-AXS SHELXTL Software' _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^)+(0.0742P)^2^+0.6095P] 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 3585 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.1156 _refine_ls_wR_factor_gt 0.1128 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 Ti1 Ti 0.94687(3) 0.989381(17) 0.85614(2) 0.02542(15) Uani 1 1 d . . . O1 O 0.94112(12) 0.94056(6) 1.00317(10) 0.0269(3) Uani 1 1 d . . . O3 O 0.94970(14) 1.05411(7) 0.74567(11) 0.0360(3) Uani 1 1 d . . . O2 O 1.11328(13) 0.93498(7) 0.87477(11) 0.0346(3) Uani 1 1 d . . . N1 N 0.75435(16) 1.05443(9) 0.86743(14) 0.0362(4) Uani 1 1 d . . . H1A H 0.6792 1.0209 0.8497 0.043 Uiso 1 1 calc R . . H1B H 0.7810 1.0676 0.9446 0.043 Uiso 1 1 calc R . . O4 O 0.80822(14) 0.92680(8) 0.75480(11) 0.0367(3) Uani 1 1 d . . . C6 C 0.8780(2) 0.87094(10) 1.01633(16) 0.0347(4) Uani 1 1 d . . . H6 H 0.9155 0.8599 1.1020 0.042 Uiso 1 1 calc R . . C7 C 0.9225(2) 0.80630(11) 0.9591(2) 0.0476(5) Uani 1 1 d . . . H7A H 0.8801 0.8130 0.8740 0.071 Uiso 1 1 calc R . . H7B H 0.8879 0.7591 0.9792 0.071 Uiso 1 1 calc R . . H7C H 1.0282 0.8049 0.9872 0.071 Uiso 1 1 calc R . . C11 C 1.1630(2) 0.90712(12) 0.79091(18) 0.0398(5) Uani 1 1 d . . . H11 H 1.1057 0.9314 0.7139 0.048 Uiso 1 1 calc R . . C1 C 0.6953(2) 1.12151(13) 0.7983(2) 0.0493(5) Uani 1 1 d . . . H1C H 0.6722 1.1101 0.7150 0.059 Uiso 1 1 calc R . . H1D H 0.7703 1.1611 0.8229 0.059 Uiso 1 1 calc R . . C5 C 0.7145(2) 0.87826(13) 0.97234(19) 0.0469(5) Uani 1 1 d . . . H5A H 0.6904 0.9208 1.0110 0.070 Uiso 1 1 calc R . . H5B H 0.6741 0.8322 0.9901 0.070 Uiso 1 1 calc R . . H5C H 0.6734 0.8865 0.8875 0.070 Uiso 1 1 calc R . . C8 C 0.9748(3) 1.11029(14) 0.67616(19) 0.0533(6) Uani 1 1 d . . . H8 H 0.9620 1.1596 0.7090 0.064 Uiso 1 1 calc R . . C10 C 1.1280(3) 1.10760(16) 0.6858(2) 0.0628(7) Uani 1 1 d . . . H10A H 1.1944 1.1108 0.7683 0.094 Uiso 1 1 calc R . . H10B H 1.1454 1.1498 0.6428 0.094 Uiso 1 1 calc R . . H10C H 1.1443 1.0604 0.6525 0.094 Uiso 1 1 calc R . . C3 C 0.7116(3) 0.92989(17) 0.63586(18) 0.0582(7) Uani 1 1 d . . . H3 H 0.7241 0.9793 0.6032 0.070 Uiso 1 1 calc R . . C12 C 1.1397(3) 0.82338(14) 0.7777(3) 0.0633(7) Uani 1 1 d . . . H12A H 1.1952 0.7988 0.8526 0.095 Uiso 1 1 calc R . . H12B H 1.1721 0.8048 0.7181 0.095 Uiso 1 1 calc R . . H12C H 1.0365 0.8123 0.7538 0.095 Uiso 1 1 calc R . . C13 C 1.3207(3) 0.92791(17) 0.8274(2) 0.0623(7) Uani 1 1 d . . . H13A H 1.3314 0.9825 0.8356 0.093 Uiso 1 1 calc R . . H13B H 1.3544 0.9107 0.7678 0.093 Uiso 1 1 calc R . . H13C H 1.3784 0.9041 0.9025 0.093 Uiso 1 1 calc R . . C9 C 0.8663(3) 1.10736(19) 0.5529(2) 0.0772(9) Uani 1 1 d . . . H9A H 0.8674 1.0574 0.5205 0.116 Uiso 1 1 calc R . . H9B H 0.8905 1.1451 0.5063 0.116 Uiso 1 1 calc R . . H9C H 0.7698 1.1177 0.5509 0.116 Uiso 1 1 calc R . . C2 C 0.5591(3) 0.9236(2) 0.6228(2) 0.0759(8) Uani 1 1 d . . . H2A H 0.5439 0.8746 0.6517 0.114 Uiso 1 1 calc R . . H2B H 0.4945 0.9287 0.5400 0.114 Uiso 1 1 calc R . . H2C H 0.5381 0.9634 0.6680 0.114 Uiso 1 1 calc R . . C4 C 0.7506(4) 0.8695(4) 0.5711(3) 0.155(3) Uani 1 1 d . . . H4A H 0.8519 0.8754 0.5817 0.233 Uiso 1 1 calc R . . H4B H 0.6879 0.8728 0.4877 0.233 Uiso 1 1 calc R . . H4C H 0.7378 0.8206 0.6014 0.233 Uiso 1 1 calc R . . C14 C 0.5590(3) 1.15169(17) 0.8094(3) 0.0733(8) Uani 1 1 d . . . H14A H 0.4827 1.1128 0.7823 0.088 Uiso 1 1 calc R . . H14B H 0.5811 1.1618 0.8930 0.088 Uiso 1 1 calc R . . C15 C 0.5027(3) 1.22128(19) 0.7413(4) 0.0945(11) Uani 1 1 d . . . H15A H 0.5769 1.2604 0.7685 0.142 Uiso 1 1 calc R . . H15B H 0.4162 1.2380 0.7522 0.142 Uiso 1 1 calc R . . H15C H 0.4777 1.2114 0.6581 0.142 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 0.0251(2) 0.0272(2) 0.0252(2) 0.00011(11) 0.01138(15) 0.00196(11) O1 0.0291(6) 0.0241(6) 0.0288(6) -0.0003(5) 0.0131(5) -0.0009(5) O3 0.0424(7) 0.0372(7) 0.0307(6) 0.0057(5) 0.0171(6) 0.0010(6) O2 0.0335(6) 0.0410(7) 0.0340(7) -0.0007(5) 0.0183(5) 0.0090(5) N1 0.0302(8) 0.0431(9) 0.0338(8) 0.0024(7) 0.0113(6) 0.0087(7) O4 0.0380(7) 0.0407(7) 0.0294(6) -0.0045(5) 0.0111(5) -0.0063(6) C6 0.0405(10) 0.0296(9) 0.0370(9) 0.0002(7) 0.0185(8) -0.0073(7) C7 0.0635(13) 0.0291(10) 0.0538(12) -0.0031(9) 0.0273(11) -0.0056(9) C11 0.0445(11) 0.0423(11) 0.0419(10) -0.0008(8) 0.0271(9) 0.0096(8) C1 0.0462(11) 0.0451(12) 0.0527(12) 0.0069(10) 0.0156(10) 0.0154(10) C5 0.0418(11) 0.0514(12) 0.0516(12) -0.0034(10) 0.0228(9) -0.0145(9) C8 0.0590(13) 0.0557(13) 0.0461(12) 0.0177(10) 0.0217(10) -0.0005(11) C10 0.0676(15) 0.0667(16) 0.0674(16) 0.0207(13) 0.0408(13) -0.0011(13) C3 0.0530(13) 0.0867(18) 0.0293(10) -0.0039(11) 0.0103(9) -0.0259(12) C12 0.0830(17) 0.0456(13) 0.0798(17) -0.0104(12) 0.0520(15) 0.0073(12) C13 0.0493(13) 0.0744(17) 0.0791(17) -0.0003(13) 0.0425(13) 0.0075(12) C9 0.0829(19) 0.095(2) 0.0430(13) 0.0255(14) 0.0131(13) -0.0155(16) C2 0.0486(14) 0.107(3) 0.0545(15) -0.0003(15) 0.0019(12) -0.0076(14) C4 0.079(2) 0.292(7) 0.083(2) -0.116(4) 0.0196(19) -0.004(3) C14 0.0606(16) 0.0628(16) 0.093(2) 0.0104(15) 0.0274(15) 0.0241(13) C15 0.0678(18) 0.0595(18) 0.140(3) 0.0117(19) 0.0243(19) 0.0205(15) _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 O3 1.8050(13) . ? Ti1 O4 1.8404(13) . ? Ti1 O2 1.8693(12) . ? Ti1 O1 2.0489(12) . ? Ti1 O1 2.0814(12) 3_777 ? Ti1 N1 2.3110(15) . ? Ti1 Ti1 3.3279(6) 3_777 ? O1 C6 1.434(2) . ? O1 Ti1 2.0814(12) 3_777 ? O3 C8 1.411(2) . ? O2 C11 1.416(2) . ? N1 C1 1.456(3) . ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? O4 C3 1.413(2) . ? C6 C7 1.513(3) . ? C6 C5 1.521(3) . ? C6 H6 1.0000 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C11 C12 1.511(3) . ? C11 C13 1.514(3) . ? C11 H11 1.0000 . ? C1 C14 1.531(3) . ? C1 H1C 0.9900 . ? C1 H1D 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C8 C9 1.489(3) . ? C8 C10 1.500(3) . ? C8 H8 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C3 C2 1.483(3) . ? C3 C4 1.489(5) . ? C3 H3 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C14 C15 1.484(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? 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 O3 Ti1 O4 95.92(6) . . ? O3 Ti1 O2 98.15(6) . . ? O4 Ti1 O2 99.68(6) . . ? O3 Ti1 O1 165.37(5) . . ? O4 Ti1 O1 94.10(5) . . ? O2 Ti1 O1 90.61(5) . . ? O3 Ti1 O1 95.15(5) . 3_777 ? O4 Ti1 O1 161.97(5) . 3_777 ? O2 Ti1 O1 92.78(5) . 3_777 ? O1 Ti1 O1 72.64(5) . 3_777 ? O3 Ti1 N1 89.59(6) . . ? O4 Ti1 N1 85.44(6) . . ? O2 Ti1 N1 170.18(5) . . ? O1 Ti1 N1 80.61(5) . . ? O1 Ti1 N1 80.45(5) 3_777 . ? O3 Ti1 Ti1 130.68(5) . 3_777 ? O4 Ti1 Ti1 129.70(4) . 3_777 ? O2 Ti1 Ti1 92.11(4) . 3_777 ? O1 Ti1 Ti1 36.65(3) . 3_777 ? O1 Ti1 Ti1 35.99(3) 3_777 3_777 ? N1 Ti1 Ti1 78.22(4) . 3_777 ? C6 O1 Ti1 129.91(10) . . ? C6 O1 Ti1 122.72(10) . 3_777 ? Ti1 O1 Ti1 107.36(5) . 3_777 ? C8 O3 Ti1 169.36(14) . . ? C11 O2 Ti1 130.78(12) . . ? C1 N1 Ti1 122.15(13) . . ? C1 N1 H1A 106.8 . . ? Ti1 N1 H1A 106.8 . . ? C1 N1 H1B 106.8 . . ? Ti1 N1 H1B 106.8 . . ? H1A N1 H1B 106.6 . . ? C3 O4 Ti1 135.51(14) . . ? O1 C6 C7 112.28(15) . . ? O1 C6 C5 110.48(16) . . ? C7 C6 C5 112.11(17) . . ? O1 C6 H6 107.2 . . ? C7 C6 H6 107.2 . . ? C5 C6 H6 107.2 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O2 C11 C12 110.02(17) . . ? O2 C11 C13 109.20(17) . . ? C12 C11 C13 112.0(2) . . ? O2 C11 H11 108.5 . . ? C12 C11 H11 108.5 . . ? C13 C11 H11 108.5 . . ? N1 C1 C14 113.9(2) . . ? N1 C1 H1C 108.8 . . ? C14 C1 H1C 108.8 . . ? N1 C1 H1D 108.8 . . ? C14 C1 H1D 108.8 . . ? H1C C1 H1D 107.7 . . ? C6 C5 H5A 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C6 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C8 C9 111.7(2) . . ? O3 C8 C10 110.94(19) . . ? C9 C8 C10 113.0(2) . . ? O3 C8 H8 106.9 . . ? C9 C8 H8 106.9 . . ? C10 C8 H8 106.9 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O4 C3 C2 111.32(19) . . ? O4 C3 C4 108.6(3) . . ? C2 C3 C4 111.8(3) . . ? O4 C3 H3 108.3 . . ? C2 C3 H3 108.3 . . ? C4 C3 H3 108.3 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C3 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C3 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C15 C14 C1 113.3(3) . . ? C15 C14 H14A 108.9 . . ? C1 C14 H14A 108.9 . . ? C15 C14 H14B 108.9 . . ? C1 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Ti1 O1 C6 147.0(2) . . . . ? O4 Ti1 O1 C6 13.86(14) . . . . ? O2 Ti1 O1 C6 -85.89(14) . . . . ? O1 Ti1 O1 C6 -178.61(16) 3_777 . . . ? N1 Ti1 O1 C6 98.55(14) . . . . ? Ti1 Ti1 O1 C6 -178.61(16) 3_777 . . . ? O3 Ti1 O1 Ti1 -34.4(2) . . . 3_777 ? O4 Ti1 O1 Ti1 -167.53(6) . . . 3_777 ? O2 Ti1 O1 Ti1 92.72(6) . . . 3_777 ? O1 Ti1 O1 Ti1 0.0 3_777 . . 3_777 ? N1 Ti1 O1 Ti1 -82.85(6) . . . 3_777 ? O4 Ti1 O3 C8 -170.0(8) . . . . ? O2 Ti1 O3 C8 -69.3(8) . . . . ? O1 Ti1 O3 C8 57.0(8) . . . . ? O1 Ti1 O3 C8 24.2(8) 3_777 . . . ? N1 Ti1 O3 C8 104.6(8) . . . . ? Ti1 Ti1 O3 C8 30.6(8) 3_777 . . . ? O3 Ti1 O2 C11 -43.07(17) . . . . ? O4 Ti1 O2 C11 54.41(17) . . . . ? O1 Ti1 O2 C11 148.67(16) . . . . ? O1 Ti1 O2 C11 -138.68(16) 3_777 . . . ? N1 Ti1 O2 C11 175.2(3) . . . . ? Ti1 Ti1 O2 C11 -174.70(16) 3_777 . . . ? O3 Ti1 N1 C1 -1.90(16) . . . . ? O4 Ti1 N1 C1 -97.87(16) . . . . ? O2 Ti1 N1 C1 140.2(3) . . . . ? O1 Ti1 N1 C1 167.20(16) . . . . ? O1 Ti1 N1 C1 93.39(16) 3_777 . . . ? Ti1 Ti1 N1 C1 129.97(16) 3_777 . . . ? O3 Ti1 O4 C3 -11.0(2) . . . . ? O2 Ti1 O4 C3 -110.3(2) . . . . ? O1 Ti1 O4 C3 158.4(2) . . . . ? O1 Ti1 O4 C3 116.6(2) 3_777 . . . ? N1 Ti1 O4 C3 78.1(2) . . . . ? Ti1 Ti1 O4 C3 148.70(18) 3_777 . . . ? Ti1 O1 C6 C7 49.8(2) . . . . ? Ti1 O1 C6 C7 -128.64(14) 3_777 . . . ? Ti1 O1 C6 C5 -76.19(18) . . . . ? Ti1 O1 C6 C5 105.39(15) 3_777 . . . ? Ti1 O2 C11 C12 -104.9(2) . . . . ? Ti1 O2 C11 C13 131.81(17) . . . . ? Ti1 N1 C1 C14 174.28(17) . . . . ? Ti1 O3 C8 C9 180(100) . . . . ? Ti1 O3 C8 C10 52.4(9) . . . . ? Ti1 O4 C3 C2 -120.6(2) . . . . ? Ti1 O4 C3 C4 116.0(3) . . . . ? N1 C1 C14 C15 178.3(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1B O2 0.92 2.07 2.952(2) 160.0 3_777 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.643 _refine_diff_density_min -0.273 _refine_diff_density_rms 0.056 # -----end-of-data-block----- data_hf_sil2 _database_code_depnum_ccdc_archive 'CCDC 245950' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H110 N2 O14 Si2 Ti2' _chemical_formula_weight 1067.34 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 9.394(6) _cell_length_b 12.441(9) _cell_length_c 14.435(9) _cell_angle_alpha 100.633(14) _cell_angle_beta 95.931(16) _cell_angle_gamma 111.947(12) _cell_volume 1510.1(17) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1696 _cell_measurement_theta_min 5.174 _cell_measurement_theta_max 49.130 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.98 _exptl_crystal_size_mid 0.86 _exptl_crystal_size_min 0.74 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.174 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 0.360 _exptl_absorpt_correction_type ¥SADABS¥ _exptl_absorpt_correction_T_min 0.7194 _exptl_absorpt_correction_T_max 0.7767 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker-AXS APEX CCD Detector' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time 20 _diffrn_standards_decay_% ? _diffrn_reflns_number 7279 _diffrn_reflns_av_R_equivalents 0.1631 _diffrn_reflns_av_sigmaI/netI 0.3015 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5188 _reflns_number_gt 1770 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-AXS SMART Software' _computing_cell_refinement 'Bruker-AXS SAINT Software' _computing_data_reduction 'Bruker-AXS SAINT Software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker-AXS SHELXTL Software' _computing_publication_material 'Bruker-AXS SHELXTL Software' _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^)+(0.1233P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5188 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2755 _refine_ls_R_factor_gt 0.1158 _refine_ls_wR_factor_ref 0.2910 _refine_ls_wR_factor_gt 0.2523 _refine_ls_goodness_of_fit_ref 0.829 _refine_ls_restrained_S_all 0.829 _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 0.50405(14) 0.87145(10) 0.50871(10) 0.0582(5) Uani 1 1 d . . . O2 O 0.6586(6) 0.8224(4) 0.5014(4) 0.0745(16) Uani 1 1 d . . . O3 O 0.6198(5) 1.0238(3) 0.4701(3) 0.0531(13) Uani 1 1 d . . . O1 O 0.3902(6) 0.7673(4) 0.5697(4) 0.0796(18) Uani 1 1 d . . . O4 O 0.3899(6) 0.7929(4) 0.3881(4) 0.0807(18) Uani 1 1 d . . . N1 N 0.6303(7) 0.9905(5) 0.6591(5) 0.0686(19) Uani 1 1 d . . . H1A H 0.6386 1.0664 0.6584 0.082 Uiso 1 1 calc R . . H1B H 0.5647 0.9646 0.7009 0.082 Uiso 1 1 calc R . . Si1 Si 1.1100(3) 1.21264(19) 0.95560(19) 0.0758(9) Uani 1 1 d . . . O7 O 1.2867(7) 1.2287(5) 0.9896(5) 0.091(2) Uani 1 1 d . . . O5 O 1.0069(8) 1.1774(5) 1.0356(5) 0.0864(19) Uani 1 1 d . . . O6 O 1.1225(7) 1.3406(4) 0.9444(5) 0.101(2) Uani 1 1 d . . . C1 C 0.7860(9) 1.0017(7) 0.7022(6) 0.071(2) Uani 1 1 d . . . H1C H 0.8592 1.0288 0.6584 0.085 Uiso 1 1 calc R . . H1D H 0.7793 0.9219 0.7078 0.085 Uiso 1 1 calc R . . C2 C 0.7736(10) 1.0378(9) 0.3478(7) 0.089(3) Uani 1 1 d . . . H2A H 0.7146 0.9520 0.3200 0.134 Uiso 1 1 calc R . . H2B H 0.8815 1.0609 0.3376 0.134 Uiso 1 1 calc R . . H2C H 0.7250 1.0825 0.3167 0.134 Uiso 1 1 calc R . . C3 C 1.0122(9) 1.0972(7) 0.8449(6) 0.072(2) Uani 1 1 d . . . H3A H 1.0808 1.1122 0.7969 0.087 Uiso 1 1 calc R . . H3B H 0.9999 1.0191 0.8578 0.087 Uiso 1 1 calc R . . C4 C 0.7731(8) 1.0650(6) 0.4528(7) 0.070(2) Uani 1 1 d . . . H4A H 0.8318 1.0265 0.4852 0.084 Uiso 1 1 calc R . . H4B H 0.8261 1.1523 0.4799 0.084 Uiso 1 1 calc R . . C5 C 0.3270(11) 0.6734(7) 0.3378(7) 0.083(3) Uani 1 1 d . . . H5 H 0.3699 0.6255 0.3714 0.100 Uiso 1 1 calc R . . C6 C 0.8532(9) 1.0885(6) 0.8013(6) 0.068(2) Uani 1 1 d . . . H6A H 0.8619 1.1688 0.7958 0.082 Uiso 1 1 calc R . . H6B H 0.7796 1.0622 0.8451 0.082 Uiso 1 1 calc R . . C7 C 1.3327(13) 1.1318(9) 1.0013(9) 0.100(4) Uani 1 1 d . . . H7 H 1.2377 1.0558 0.9902 0.121 Uiso 1 1 calc R . . C8 C 0.7695(19) 0.7782(14) 0.4892(13) 0.150(6) Uani 1 1 d . . . H8 H 0.8687 0.8491 0.5201 0.179 Uiso 1 1 calc R . . C9 C 0.3625(16) 0.6832(11) 0.6173(12) 0.145(6) Uani 1 1 d . . . H9 H 0.3790 0.6264 0.5652 0.174 Uiso 1 1 calc R . . C10 C 0.7899(16) 0.7503(11) 0.3941(11) 0.145(5) Uani 1 1 d . . . H10A H 0.6880 0.7011 0.3524 0.217 Uiso 1 1 calc R . . H10B H 0.8571 0.7060 0.3902 0.217 Uiso 1 1 calc R . . H10C H 0.8387 0.8242 0.3733 0.217 Uiso 1 1 calc R . . C11 C 1.4186(17) 1.1663(11) 1.1039(11) 0.180(7) Uani 1 1 d . . . H11A H 1.4922 1.2503 1.1199 0.270 Uiso 1 1 calc R . . H11B H 1.4760 1.1159 1.1112 0.270 Uiso 1 1 calc R . . H11C H 1.3432 1.1552 1.1472 0.270 Uiso 1 1 calc R . . C12 C 1.2470(15) 1.4444(9) 0.9446(12) 0.145(6) Uani 1 1 d . . . H12 H 1.3321 1.4604 0.9995 0.174 Uiso 1 1 calc R . . C13 C 0.1543(12) 0.6253(9) 0.3254(10) 0.145(5) Uani 1 1 d . . . H13A H 0.1246 0.6463 0.3872 0.218 Uiso 1 1 calc R . . H13B H 0.1109 0.5382 0.3020 0.218 Uiso 1 1 calc R . . H13C H 0.1131 0.6597 0.2788 0.218 Uiso 1 1 calc R . . C14 C 1.0136(19) 1.2611(12) 1.1170(11) 0.119(4) Uani 1 1 d . . . H14 H 1.0347 1.3385 1.0986 0.143 Uiso 1 1 calc R . . C15 C 1.4306(17) 1.1193(11) 0.9297(8) 0.135(5) Uani 1 1 d . . . H15A H 1.3644 1.0826 0.8658 0.202 Uiso 1 1 calc R . . H15B H 1.4835 1.0687 0.9455 0.202 Uiso 1 1 calc R . . H15C H 1.5086 1.1983 0.9303 0.202 Uiso 1 1 calc R . . C16 C 0.3635(16) 0.6685(11) 0.2404(10) 0.158(6) Uani 1 1 d . . . H16A H 0.2918 0.6902 0.2012 0.237 Uiso 1 1 calc R . . H16B H 0.3518 0.5874 0.2108 0.237 Uiso 1 1 calc R . . H16C H 0.4713 0.7246 0.2444 0.237 Uiso 1 1 calc R . . C17 C 0.1987(17) 0.6073(10) 0.6089(12) 0.193(8) Uani 1 1 d . . . H17A H 0.1899 0.5372 0.6335 0.289 Uiso 1 1 calc R . . H17B H 0.1471 0.5814 0.5413 0.289 Uiso 1 1 calc R . . H17C H 0.1485 0.6521 0.6462 0.289 Uiso 1 1 calc R . . C21 C 0.771(3) 0.6967(16) 0.5431(14) 0.222(9) Uani 1 1 d . . . H21A H 0.6752 0.6240 0.5206 0.333 Uiso 1 1 calc R . . H21B H 0.7786 0.7318 0.6109 0.333 Uiso 1 1 calc R . . H21C H 0.8619 0.6768 0.5357 0.333 Uiso 1 1 calc R . . C20 C 1.309(3) 1.4477(17) 0.8624(13) 0.240(11) Uani 1 1 d . . . H20A H 1.2282 1.4349 0.8081 0.360 Uiso 1 1 calc R . . H20B H 1.3488 1.3848 0.8500 0.360 Uiso 1 1 calc R . . H20C H 1.3953 1.5257 0.8706 0.360 Uiso 1 1 calc R . . C18 C 1.122(3) 1.2824(16) 1.1951(13) 0.264(14) Uani 1 1 d . . . H18A H 1.1150 1.3413 1.2476 0.395 Uiso 1 1 calc R . . H18B H 1.2269 1.3134 1.1793 0.395 Uiso 1 1 calc R . . H18C H 1.1041 1.2079 1.2151 0.395 Uiso 1 1 calc R . . C19 C 0.870(3) 1.2248(14) 1.1428(14) 0.212(9) Uani 1 1 d . . . H19A H 0.8453 1.1480 1.1598 0.318 Uiso 1 1 calc R . . H19B H 0.7908 1.2160 1.0889 0.318 Uiso 1 1 calc R . . H19C H 0.8716 1.2845 1.1981 0.318 Uiso 1 1 calc R . . C22 C 1.188(3) 1.5440(12) 0.9630(16) 0.270(12) Uani 1 1 d . . . H22A H 1.2747 1.6213 0.9699 0.405 Uiso 1 1 calc R . . H22B H 1.1450 1.5438 1.0221 0.405 Uiso 1 1 calc R . . H22C H 1.1061 1.5308 0.9090 0.405 Uiso 1 1 calc R . . C23 C 0.440(5) 0.670(3) 0.676(2) 0.53(4) Uani 1 1 d . . . H23A H 0.5159 0.6442 0.6478 0.791 Uiso 1 1 calc R . . H23B H 0.3757 0.6095 0.7059 0.791 Uiso 1 1 calc R . . H23C H 0.4955 0.7459 0.7241 0.791 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 0.0557(8) 0.0466(7) 0.0696(11) 0.0175(7) 0.0118(7) 0.0160(5) O2 0.081(4) 0.070(3) 0.092(4) 0.025(3) 0.022(3) 0.047(3) O3 0.042(3) 0.054(2) 0.067(4) 0.019(2) 0.020(2) 0.0183(19) O1 0.092(4) 0.062(3) 0.096(5) 0.040(3) 0.033(3) 0.030(3) O4 0.083(4) 0.049(2) 0.094(4) 0.001(3) -0.005(3) 0.022(2) N1 0.072(4) 0.068(4) 0.072(5) 0.022(3) 0.012(4) 0.033(3) Si1 0.0846(17) 0.0589(12) 0.083(2) 0.0276(13) 0.0019(14) 0.0271(11) O7 0.086(4) 0.073(3) 0.113(5) 0.037(4) 0.005(4) 0.029(3) O5 0.131(5) 0.072(3) 0.058(4) 0.014(3) 0.020(4) 0.044(3) O6 0.093(4) 0.064(3) 0.142(6) 0.047(4) -0.010(4) 0.027(3) C1 0.066(5) 0.067(4) 0.077(6) 0.023(4) 0.005(5) 0.023(4) C2 0.080(6) 0.123(7) 0.088(8) 0.044(6) 0.039(6) 0.051(5) C3 0.078(6) 0.073(5) 0.073(6) 0.024(5) 0.018(5) 0.034(4) C4 0.052(5) 0.059(4) 0.093(7) 0.015(4) 0.019(5) 0.016(3) C5 0.106(7) 0.065(5) 0.077(7) 0.012(5) 0.016(6) 0.036(5) C6 0.072(5) 0.060(4) 0.072(6) 0.016(4) 0.009(5) 0.027(4) C7 0.105(8) 0.088(6) 0.109(9) 0.039(6) -0.014(7) 0.041(5) C8 0.182(14) 0.161(12) 0.178(16) 0.062(13) 0.080(13) 0.128(11) C9 0.163(12) 0.124(9) 0.198(15) 0.120(11) 0.074(11) 0.063(8) C10 0.143(11) 0.126(9) 0.176(15) 0.003(10) 0.041(11) 0.079(8) C11 0.171(13) 0.138(10) 0.235(18) 0.111(12) 0.011(13) 0.043(10) C12 0.129(10) 0.093(7) 0.219(16) 0.083(10) -0.010(10) 0.042(7) C13 0.098(9) 0.103(7) 0.185(13) 0.037(8) -0.018(8) -0.005(6) C14 0.147(11) 0.120(9) 0.103(11) 0.040(9) 0.030(10) 0.059(8) C15 0.207(14) 0.154(11) 0.096(10) 0.042(8) 0.055(10) 0.118(10) C16 0.172(13) 0.143(11) 0.133(12) -0.032(10) 0.031(11) 0.066(9) C17 0.196(14) 0.106(8) 0.274(19) 0.081(11) 0.137(15) 0.019(9) C21 0.29(2) 0.176(15) 0.26(2) 0.047(17) 0.056(19) 0.156(16) C20 0.34(3) 0.202(17) 0.21(2) 0.121(17) 0.12(2) 0.092(17) C18 0.45(4) 0.167(15) 0.161(17) 0.001(14) -0.07(2) 0.16(2) C19 0.31(3) 0.149(13) 0.21(2) 0.056(13) 0.11(2) 0.101(16) C22 0.37(3) 0.106(10) 0.36(3) 0.105(16) 0.09(3) 0.098(14) C23 0.52(6) 0.48(5) 0.40(4) 0.37(4) -0.06(4) -0.09(4) _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 O2 1.778(6) . ? Ti1 O1 1.783(5) . ? Ti1 O4 1.828(6) . ? Ti1 O3 2.015(4) . ? Ti1 O3 2.050(5) 2_676 ? Ti1 N1 2.298(6) . ? Ti1 Ti1 3.282(3) 2_676 ? O2 C8 1.360(14) . ? O3 C4 1.403(8) . ? O3 Ti1 2.050(5) 2_676 ? O1 C9 1.317(11) . ? O4 C5 1.394(9) . ? N1 C1 1.474(10) . ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? Si1 O6 1.591(6) . ? Si1 O5 1.601(7) . ? Si1 O7 1.608(7) . ? Si1 C3 1.823(8) . ? O7 C7 1.456(11) . ? O5 C14 1.397(14) . ? O6 C12 1.381(12) . ? C1 C6 1.532(11) . ? C1 H1C 0.9900 . ? C1 H1D 0.9900 . ? C2 C4 1.492(11) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C6 1.516(11) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C16 1.477(14) . ? C5 C13 1.482(13) . ? C5 H5 1.0000 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C15 1.476(15) . ? C7 C11 1.513(15) . ? C7 H7 1.0000 . ? C8 C21 1.391(19) . ? C8 C10 1.403(16) . ? C8 H8 1.0000 . ? C9 C23 1.13(3) . ? C9 C17 1.451(18) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C20 1.38(2) . ? C12 C22 1.53(2) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C18 1.36(2) . ? C14 C19 1.37(2) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? 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 O2 Ti1 O1 98.4(3) . . ? O2 Ti1 O4 98.1(3) . . ? O1 Ti1 O4 96.8(2) . . ? O2 Ti1 O3 93.7(2) . . ? O1 Ti1 O3 162.6(2) . . ? O4 Ti1 O3 93.9(2) . . ? O2 Ti1 O3 163.05(19) . 2_676 ? O1 Ti1 O3 93.4(2) . 2_676 ? O4 Ti1 O3 92.5(2) . 2_676 ? O3 Ti1 O3 72.3(2) . 2_676 ? O2 Ti1 N1 89.7(3) . . ? O1 Ti1 N1 85.8(2) . . ? O4 Ti1 N1 171.3(3) . . ? O3 Ti1 N1 81.8(2) . . ? O3 Ti1 N1 79.0(2) 2_676 . ? O2 Ti1 Ti1 129.56(17) . 2_676 ? O1 Ti1 Ti1 128.5(2) . 2_676 ? O4 Ti1 Ti1 93.93(18) . 2_676 ? O3 Ti1 Ti1 36.52(14) . 2_676 ? O3 Ti1 Ti1 35.80(11) 2_676 2_676 ? N1 Ti1 Ti1 78.07(17) . 2_676 ? C8 O2 Ti1 175.3(9) . . ? C4 O3 Ti1 126.9(5) . . ? C4 O3 Ti1 124.0(4) . 2_676 ? Ti1 O3 Ti1 107.68(19) . 2_676 ? C9 O1 Ti1 155.1(8) . . ? C5 O4 Ti1 133.2(6) . . ? C1 N1 Ti1 121.9(5) . . ? C1 N1 H1A 106.9 . . ? Ti1 N1 H1A 106.9 . . ? C1 N1 H1B 106.9 . . ? Ti1 N1 H1B 106.9 . . ? H1A N1 H1B 106.7 . . ? O6 Si1 O5 108.0(4) . . ? O6 Si1 O7 105.4(3) . . ? O5 Si1 O7 111.3(4) . . ? O6 Si1 C3 112.2(4) . . ? O5 Si1 C3 107.3(4) . . ? O7 Si1 C3 112.6(4) . . ? C7 O7 Si1 124.6(5) . . ? C14 O5 Si1 122.7(7) . . ? C12 O6 Si1 133.0(7) . . ? N1 C1 C6 114.1(7) . . ? N1 C1 H1C 108.7 . . ? C6 C1 H1C 108.7 . . ? N1 C1 H1D 108.7 . . ? C6 C1 H1D 108.7 . . ? H1C C1 H1D 107.6 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C6 C3 Si1 115.5(6) . . ? C6 C3 H3A 108.4 . . ? Si1 C3 H3A 108.4 . . ? C6 C3 H3B 108.4 . . ? Si1 C3 H3B 108.4 . . ? H3A C3 H3B 107.5 . . ? O3 C4 C2 110.9(7) . . ? O3 C4 H4A 109.5 . . ? C2 C4 H4A 109.5 . . ? O3 C4 H4B 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 108.0 . . ? O4 C5 C16 107.9(8) . . ? O4 C5 C13 109.3(9) . . ? C16 C5 C13 106.4(9) . . ? O4 C5 H5 111.1 . . ? C16 C5 H5 111.1 . . ? C13 C5 H5 111.1 . . ? C3 C6 C1 113.2(7) . . ? C3 C6 H6A 108.9 . . ? C1 C6 H6A 108.9 . . ? C3 C6 H6B 108.9 . . ? C1 C6 H6B 108.9 . . ? H6A C6 H6B 107.8 . . ? O7 C7 C15 107.7(9) . . ? O7 C7 C11 106.1(10) . . ? C15 C7 C11 113.4(11) . . ? O7 C7 H7 109.8 . . ? C15 C7 H7 109.8 . . ? C11 C7 H7 109.8 . . ? O2 C8 C21 115.0(15) . . ? O2 C8 C10 115.0(14) . . ? C21 C8 C10 116.0(14) . . ? O2 C8 H8 102.6 . . ? C21 C8 H8 102.6 . . ? C10 C8 H8 102.6 . . ? C23 C9 O1 131(2) . . ? C23 C9 C17 112.2(18) . . ? O1 C9 C17 115.2(14) . . ? C23 C9 H9 93.8 . . ? O1 C9 H9 93.8 . . ? C17 C9 H9 93.8 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C11 H11A 109.5 . . ? C7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C20 C12 O6 116.9(15) . . ? C20 C12 C22 108.5(14) . . ? O6 C12 C22 106.0(13) . . ? C20 C12 H12 108.4 . . ? O6 C12 H12 108.4 . . ? C22 C12 H12 108.4 . . ? C5 C13 H13A 109.5 . . ? C5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C18 C14 C19 108.1(17) . . ? C18 C14 O5 116.9(16) . . ? C19 C14 O5 108.5(14) . . ? C18 C14 H14 107.7 . . ? C19 C14 H14 107.7 . . ? O5 C14 H14 107.7 . . ? C7 C15 H15A 109.5 . . ? C7 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C7 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C5 C16 H16A 109.5 . . ? C5 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C5 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C9 C17 H17A 109.5 . . ? C9 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C9 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C8 C21 H21A 109.5 . . ? C8 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C8 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C12 C20 H20A 109.5 . . ? C12 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C12 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C12 C22 H22A 109.5 . . ? C12 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C12 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C9 C23 H23A 109.5 . . ? C9 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C9 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ti1 O2 C8 85(10) . . . . ? O4 Ti1 O2 C8 -13(10) . . . . ? O3 Ti1 O2 C8 -107(10) . . . . ? O3 Ti1 O2 C8 -141(10) 2_676 . . . ? N1 Ti1 O2 C8 171(10) . . . . ? Ti1 Ti1 O2 C8 -115(10) 2_676 . . . ? O2 Ti1 O3 C4 -3.6(6) . . . . ? O1 Ti1 O3 C4 130.6(9) . . . . ? O4 Ti1 O3 C4 -102.0(6) . . . . ? O3 Ti1 O3 C4 166.7(7) 2_676 . . . ? N1 Ti1 O3 C4 85.6(6) . . . . ? Ti1 Ti1 O3 C4 166.7(7) 2_676 . . . ? O2 Ti1 O3 Ti1 -170.2(3) . . . 2_676 ? O1 Ti1 O3 Ti1 -36.1(9) . . . 2_676 ? O4 Ti1 O3 Ti1 91.4(3) . . . 2_676 ? O3 Ti1 O3 Ti1 0.0 2_676 . . 2_676 ? N1 Ti1 O3 Ti1 -81.0(3) . . . 2_676 ? O2 Ti1 O1 C9 10(2) . . . . ? O4 Ti1 O1 C9 109(2) . . . . ? O3 Ti1 O1 C9 -123(2) . . . . ? O3 Ti1 O1 C9 -158(2) 2_676 . . . ? N1 Ti1 O1 C9 -79(2) . . . . ? Ti1 Ti1 O1 C9 -150(2) 2_676 . . . ? O2 Ti1 O4 C5 54.9(8) . . . . ? O1 Ti1 O4 C5 -44.7(8) . . . . ? O3 Ti1 O4 C5 149.2(8) . . . . ? O3 Ti1 O4 C5 -138.4(8) 2_676 . . . ? N1 Ti1 O4 C5 -151.0(13) . . . . ? Ti1 Ti1 O4 C5 -174.2(7) 2_676 . . . ? O2 Ti1 N1 C1 3.8(5) . . . . ? O1 Ti1 N1 C1 102.3(5) . . . . ? O4 Ti1 N1 C1 -150.5(14) . . . . ? O3 Ti1 N1 C1 -89.9(5) . . . . ? O3 Ti1 N1 C1 -163.4(5) 2_676 . . . ? Ti1 Ti1 N1 C1 -126.9(5) 2_676 . . . ? O6 Si1 O7 C7 -174.7(8) . . . . ? O5 Si1 O7 C7 68.5(9) . . . . ? C3 Si1 O7 C7 -52.1(9) . . . . ? O6 Si1 O5 C14 -36.3(10) . . . . ? O7 Si1 O5 C14 78.9(9) . . . . ? C3 Si1 O5 C14 -157.4(9) . . . . ? O5 Si1 O6 C12 129.9(12) . . . . ? O7 Si1 O6 C12 10.9(13) . . . . ? C3 Si1 O6 C12 -112.0(12) . . . . ? Ti1 N1 C1 C6 178.0(4) . . . . ? O6 Si1 C3 C6 -53.4(7) . . . . ? O5 Si1 C3 C6 65.0(6) . . . . ? O7 Si1 C3 C6 -172.1(5) . . . . ? Ti1 O3 C4 C2 99.3(8) . . . . ? Ti1 O3 C4 C2 -96.0(7) 2_676 . . . ? Ti1 O4 C5 C16 -134.2(8) . . . . ? Ti1 O4 C5 C13 110.6(9) . . . . ? Si1 C3 C6 C1 172.5(5) . . . . ? N1 C1 C6 C3 179.1(6) . . . . ? Si1 O7 C7 C15 115.0(9) . . . . ? Si1 O7 C7 C11 -123.2(9) . . . . ? Ti1 O2 C8 C21 -98(10) . . . . ? Ti1 O2 C8 C10 41(11) . . . . ? Ti1 O1 C9 C23 40(6) . . . . ? Ti1 O1 C9 C17 -154.6(12) . . . . ? Si1 O6 C12 C20 76.8(17) . . . . ? Si1 O6 C12 C22 -162.2(11) . . . . ? Si1 O5 C14 C18 -88.4(16) . . . . ? Si1 O5 C14 C19 149.0(12) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O4 0.92 2.08 2.966(8) 160.8 2_676 _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.770 _refine_diff_density_min -0.746 _refine_diff_density_rms 0.096 # -----end-of-data-block----- data_diahex _database_code_depnum_ccdc_archive 'CCDC 245951' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H79 N2 O8 Ti2' _chemical_formula_weight 775.82 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6481(11) _cell_length_b 9.8787(11) _cell_length_c 12.2188(14) _cell_angle_alpha 78.936(2) _cell_angle_beta 82.489(2) _cell_angle_gamma 78.503(2) _cell_volume 1114.8(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4666 _cell_measurement_theta_min 5.257 _cell_measurement_theta_max 56.570 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.82 _exptl_crystal_size_mid 0.73 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.156 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 423 _exptl_absorpt_coefficient_mu 0.403 _exptl_absorpt_correction_type ¥SADABS¥ _exptl_absorpt_correction_T_min 0.7334 _exptl_absorpt_correction_T_max 0.8818 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker-AXS APEX CCD Detector' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time 20 _diffrn_standards_decay_% ? _diffrn_reflns_number 6084 _diffrn_reflns_av_R_equivalents 0.0168 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3871 _reflns_number_gt 3549 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-AXS SMART Software' _computing_cell_refinement 'Bruker-AXS SAINT Software' _computing_data_reduction 'Bruker-AXS SAINT Software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker-AXS SHELXTL Software' _computing_publication_material 'Bruker-AXS SHELXTL Software' _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^)+(0.0566P)^2^+0.5135P] 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 3871 _refine_ls_number_parameters 234 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.1006 _refine_ls_wR_factor_gt 0.0986 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 0.46195(3) 0.03002(3) 0.36678(2) 0.01939(12) Uani 1 1 d . . . O3 O 0.32497(13) -0.02387(12) 0.30636(10) 0.0257(3) Uani 1 1 d . . . O4 O 0.58251(11) 0.08199(11) 0.47321(9) 0.0202(2) Uani 1 1 d . . . O2 O 0.61342(13) -0.10831(12) 0.32933(10) 0.0256(3) Uani 1 1 d . . . O1 O 0.49308(13) 0.17522(13) 0.25263(10) 0.0279(3) Uani 1 1 d . . . N1 N 0.29364(15) 0.19459(15) 0.44296(12) 0.0243(3) Uani 1 1 d . . . H1A H 0.3059 0.1827 0.5178 0.029 Uiso 1 1 calc R . . H1B H 0.3141 0.2813 0.4106 0.029 Uiso 1 1 calc R . . C13 C 0.14165(18) 0.19949(19) 0.43463(16) 0.0284(4) Uani 1 1 d . . . H13A H 0.1202 0.1038 0.4592 0.034 Uiso 1 1 calc R . . H13B H 0.1226 0.2293 0.3551 0.034 Uiso 1 1 calc R . . C2 C 0.68671(19) 0.17198(19) 0.44787(15) 0.0270(4) Uani 1 1 d . . . H2 H 0.7436 0.1527 0.5137 0.032 Uiso 1 1 calc R . . C12 C 0.2137(2) -0.0755(2) 0.27274(16) 0.0321(4) Uani 1 1 d . . . H12 H 0.1319 -0.0683 0.3320 0.039 Uiso 1 1 calc R . . C8 C 0.6476(2) -0.17004(19) 0.23138(15) 0.0287(4) Uani 1 1 d . . . H8 H 0.5658 -0.1397 0.1844 0.034 Uiso 1 1 calc R . . C3 C 0.7895(2) 0.1414(2) 0.34671(17) 0.0397(5) Uani 1 1 d . . . H3A H 0.7383 0.1657 0.2794 0.060 Uiso 1 1 calc R . . H3B H 0.8316 0.0415 0.3575 0.060 Uiso 1 1 calc R . . H3C H 0.8648 0.1973 0.3379 0.060 Uiso 1 1 calc R . . C1 C 0.6139(2) 0.3243(2) 0.43569(19) 0.0405(5) Uani 1 1 d . . . H1C H 0.5457 0.3379 0.5012 0.061 Uiso 1 1 calc R . . H1D H 0.5637 0.3494 0.3679 0.061 Uiso 1 1 calc R . . H1E H 0.6852 0.3841 0.4301 0.061 Uiso 1 1 calc R . . C7 C 0.7774(2) -0.1207(2) 0.16473(18) 0.0427(5) Uani 1 1 d . . . H7A H 0.8584 -0.1505 0.2098 0.064 Uiso 1 1 calc R . . H7B H 0.7585 -0.0182 0.1452 0.064 Uiso 1 1 calc R . . H7C H 0.7992 -0.1616 0.0961 0.064 Uiso 1 1 calc R . . C5 C 0.4183(2) 0.2596(2) 0.16460(16) 0.0350(4) Uani 1 1 d . . . H5 H 0.3165 0.2478 0.1789 0.042 Uiso 1 1 calc R . . C11 C 0.2616(2) -0.2290(2) 0.26197(19) 0.0401(5) Uani 1 1 d . . . H11A H 0.2924 -0.2829 0.3334 0.060 Uiso 1 1 calc R . . H11B H 0.3408 -0.2380 0.2033 0.060 Uiso 1 1 calc R . . H11C H 0.1823 -0.2652 0.2423 0.060 Uiso 1 1 calc R . . C9 C 0.6712(2) -0.3281(2) 0.26490(19) 0.0415(5) Uani 1 1 d . . . H9A H 0.5858 -0.3559 0.3088 0.062 Uiso 1 1 calc R . . H9B H 0.7521 -0.3591 0.3101 0.062 Uiso 1 1 calc R . . H9C H 0.6911 -0.3714 0.1975 0.062 Uiso 1 1 calc R . . C10 C 0.1648(3) 0.0119(3) 0.1647(2) 0.0492(6) Uani 1 1 d . . . H10A H 0.2433 0.0053 0.1052 0.074 Uiso 1 1 calc R . . H10B H 0.1342 0.1099 0.1744 0.074 Uiso 1 1 calc R . . H10C H 0.0851 -0.0228 0.1441 0.074 Uiso 1 1 calc R . . C4 C 0.4248(3) 0.4123(2) 0.1611(2) 0.0575(7) Uani 1 1 d . . . H4A H 0.5243 0.4244 0.1515 0.086 Uiso 1 1 calc R . . H4B H 0.3789 0.4414 0.2313 0.086 Uiso 1 1 calc R . . H4C H 0.3756 0.4699 0.0982 0.086 Uiso 1 1 calc R . . C6 C 0.4796(3) 0.2119(3) 0.05527(18) 0.0581(7) Uani 1 1 d . . . H6A H 0.4766 0.1122 0.0612 0.087 Uiso 1 1 calc R . . H6B H 0.5784 0.2262 0.0388 0.087 Uiso 1 1 calc R . . H6C H 0.4239 0.2664 -0.0051 0.087 Uiso 1 1 calc R . . C14 C 0.04174(19) 0.29818(19) 0.50408(16) 0.0293(4) Uani 1 1 d . . . H14A H -0.0571 0.2862 0.5013 0.035 Uiso 1 1 calc R . . H14B H 0.0636 0.2710 0.5831 0.035 Uiso 1 1 calc R . . C15 C 0.05134(19) 0.45179(19) 0.46522(16) 0.0301(4) Uani 1 1 d . . . H15A H 0.0308 0.4791 0.3859 0.036 Uiso 1 1 calc R . . H15B H 0.1496 0.4646 0.4694 0.036 Uiso 1 1 calc R . . C18 C 0.0657(4) 0.6083(4) -0.0083(4) 0.0980(13) Uani 1 1 d . . . C17 C 0.0261(6) 0.5384(6) 0.0955(4) 0.1124(17) Uani 1 1 d . . . C16 C -0.0354(6) 0.4321(7) 0.1055(4) 0.120(2) Uani 1 1 d . . . C19 C 0.1266(6) 0.7134(6) -0.0203(5) 0.0580(13) Uani 0.50 1 d P . . H19A H 0.0553 0.7996 -0.0281 0.087 Uiso 0.50 1 calc PR . . H19B H 0.1943 0.7147 -0.0875 0.087 Uiso 0.50 1 calc PR . . H19C H 0.1774 0.7071 0.0454 0.087 Uiso 0.50 1 calc PR . . H16A H -0.058(3) 0.401(3) 0.172(3) 0.059(9) Uiso 1 1 d . . . H17A H 0.050(5) 0.557(5) 0.171(5) 0.147(19) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.02082(18) 0.01703(18) 0.02000(18) -0.00356(12) -0.00187(11) -0.00232(12) O3 0.0271(6) 0.0263(6) 0.0262(6) -0.0070(5) -0.0057(5) -0.0060(5) O4 0.0215(6) 0.0176(6) 0.0220(6) -0.0028(4) -0.0011(4) -0.0060(5) O2 0.0272(6) 0.0252(6) 0.0233(6) -0.0083(5) -0.0007(5) 0.0011(5) O1 0.0320(7) 0.0251(6) 0.0253(6) 0.0013(5) -0.0048(5) -0.0059(5) N1 0.0238(7) 0.0201(7) 0.0280(8) -0.0046(6) -0.0040(6) 0.0002(6) C13 0.0234(9) 0.0256(9) 0.0368(10) -0.0104(8) -0.0039(7) -0.0003(7) C2 0.0292(9) 0.0268(9) 0.0277(9) -0.0014(7) -0.0042(7) -0.0139(7) C12 0.0306(10) 0.0356(10) 0.0341(10) -0.0088(8) -0.0060(8) -0.0107(8) C8 0.0324(9) 0.0291(10) 0.0246(9) -0.0111(7) -0.0019(7) 0.0004(7) C3 0.0339(10) 0.0560(13) 0.0324(10) -0.0043(9) 0.0024(8) -0.0220(10) C1 0.0526(13) 0.0224(10) 0.0500(12) -0.0002(9) -0.0148(10) -0.0146(9) C7 0.0445(12) 0.0468(13) 0.0341(11) -0.0113(9) 0.0095(9) -0.0061(10) C5 0.0405(11) 0.0322(10) 0.0298(10) 0.0057(8) -0.0093(8) -0.0069(8) C11 0.0469(12) 0.0355(11) 0.0449(12) -0.0155(9) -0.0062(9) -0.0140(9) C9 0.0489(12) 0.0306(11) 0.0451(12) -0.0164(9) -0.0005(10) -0.0008(9) C10 0.0556(14) 0.0501(14) 0.0487(13) -0.0014(10) -0.0279(11) -0.0175(11) C4 0.0868(19) 0.0297(12) 0.0517(14) 0.0072(10) -0.0225(13) -0.0033(12) C6 0.0880(19) 0.0583(16) 0.0280(11) -0.0025(10) -0.0113(12) -0.0143(14) C14 0.0234(9) 0.0276(9) 0.0363(10) -0.0095(8) 0.0001(7) -0.0015(7) C15 0.0276(9) 0.0268(10) 0.0328(10) -0.0069(8) 0.0008(8) 0.0020(7) C18 0.083(2) 0.081(3) 0.104(3) -0.011(2) 0.001(2) 0.037(2) C17 0.133(4) 0.098(3) 0.069(3) 0.006(2) 0.013(3) 0.031(3) C16 0.143(4) 0.114(4) 0.065(3) -0.005(3) 0.008(3) 0.050(3) C19 0.055(3) 0.062(3) 0.055(3) -0.002(3) -0.009(2) -0.013(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 Ti1 O3 1.8059(12) . ? Ti1 O1 1.8405(12) . ? Ti1 O2 1.8659(12) . ? Ti1 O4 2.0487(11) . ? Ti1 O4 2.0906(11) 2_656 ? Ti1 N1 2.2977(14) . ? Ti1 Ti1 3.3466(7) 2_656 ? O3 C12 1.412(2) . ? O4 C2 1.4374(19) . ? O4 Ti1 2.0906(11) 2_656 ? O2 C8 1.418(2) . ? O1 C5 1.411(2) . ? N1 C13 1.474(2) . ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? C13 C14 1.526(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C2 C1 1.516(3) . ? C2 C3 1.518(3) . ? C2 H2 1.0000 . ? C12 C10 1.508(3) . ? C12 C11 1.521(3) . ? C12 H12 1.0000 . ? C8 C7 1.514(3) . ? C8 C9 1.515(3) . ? C8 H8 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C1 H1E 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C5 C6 1.510(3) . ? C5 C4 1.515(3) . ? C5 H5 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C14 C15 1.518(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C15 1.525(3) 2_566 ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C18 C19 1.268(6) . ? C18 C17 1.370(6) . ? C18 C16 1.405(7) 2_565 ? C17 C16 1.284(8) . ? C17 H17A 1.03(5) . ? C16 C18 1.405(7) 2_565 ? C16 H16A 0.83(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? 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 O3 Ti1 O1 96.73(6) . . ? O3 Ti1 O2 98.24(5) . . ? O1 Ti1 O2 99.92(6) . . ? O3 Ti1 O4 164.88(5) . . ? O1 Ti1 O4 94.65(5) . . ? O2 Ti1 O4 89.57(5) . . ? O3 Ti1 O4 94.40(5) . 2_656 ? O1 Ti1 O4 161.21(5) . 2_656 ? O2 Ti1 O4 93.40(5) . 2_656 ? O4 Ti1 O4 72.11(5) . 2_656 ? O3 Ti1 N1 89.89(5) . . ? O1 Ti1 N1 85.49(5) . . ? O2 Ti1 N1 169.59(5) . . ? O4 Ti1 N1 81.08(5) . . ? O4 Ti1 N1 79.42(5) 2_656 . ? O3 Ti1 Ti1 129.71(4) . 2_656 ? O1 Ti1 Ti1 129.86(4) . 2_656 ? O2 Ti1 Ti1 91.86(4) . 2_656 ? O4 Ti1 Ti1 36.48(3) . 2_656 ? O4 Ti1 Ti1 35.63(3) 2_656 2_656 ? N1 Ti1 Ti1 77.90(4) . 2_656 ? C12 O3 Ti1 172.76(12) . . ? C2 O4 Ti1 128.85(10) . . ? C2 O4 Ti1 123.18(10) . 2_656 ? Ti1 O4 Ti1 107.89(5) . 2_656 ? C8 O2 Ti1 130.40(11) . . ? C5 O1 Ti1 136.77(12) . . ? C13 N1 Ti1 120.03(11) . . ? C13 N1 H1A 107.3 . . ? Ti1 N1 H1A 107.3 . . ? C13 N1 H1B 107.3 . . ? Ti1 N1 H1B 107.3 . . ? H1A N1 H1B 106.9 . . ? N1 C13 C14 114.12(15) . . ? N1 C13 H13A 108.7 . . ? C14 C13 H13A 108.7 . . ? N1 C13 H13B 108.7 . . ? C14 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? O4 C2 C1 110.08(15) . . ? O4 C2 C3 112.37(14) . . ? C1 C2 C3 112.51(17) . . ? O4 C2 H2 107.2 . . ? C1 C2 H2 107.2 . . ? C3 C2 H2 107.2 . . ? O3 C12 C10 110.46(16) . . ? O3 C12 C11 110.02(15) . . ? C10 C12 C11 111.47(18) . . ? O3 C12 H12 108.3 . . ? C10 C12 H12 108.3 . . ? C11 C12 H12 108.3 . . ? O2 C8 C7 109.67(15) . . ? O2 C8 C9 109.01(15) . . ? C7 C8 C9 111.77(16) . . ? O2 C8 H8 108.8 . . ? C7 C8 H8 108.8 . . ? C9 C8 H8 108.8 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C1 H1C 109.5 . . ? C2 C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? C2 C1 H1E 109.5 . . ? H1C C1 H1E 109.5 . . ? H1D C1 H1E 109.5 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O1 C5 C6 109.44(18) . . ? O1 C5 C4 109.91(17) . . ? C6 C5 C4 111.55(19) . . ? O1 C5 H5 108.6 . . ? C6 C5 H5 108.6 . . ? C4 C5 H5 108.6 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 H10A 109.5 . . ? C12 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C12 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C5 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C5 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C15 C14 C13 114.00(15) . . ? C15 C14 H14A 108.8 . . ? C13 C14 H14A 108.8 . . ? C15 C14 H14B 108.8 . . ? C13 C14 H14B 108.8 . . ? H14A C14 H14B 107.6 . . ? C14 C15 C15 112.89(19) . 2_566 ? C14 C15 H15A 109.0 . . ? C15 C15 H15A 109.0 2_566 . ? C14 C15 H15B 109.0 . . ? C15 C15 H15B 109.0 2_566 . ? H15A C15 H15B 107.8 . . ? C19 C18 C17 121.6(6) . . ? C19 C18 C16 117.8(5) . 2_565 ? C17 C18 C16 120.5(5) . 2_565 ? C16 C17 C18 120.5(6) . . ? C16 C17 H17A 114(3) . . ? C18 C17 H17A 125(3) . . ? C17 C16 C18 118.9(6) . 2_565 ? C17 C16 H16A 112(2) . . ? C18 C16 H16A 129(2) 2_565 . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ti1 O3 C12 -164.1(9) . . . . ? O2 Ti1 O3 C12 94.8(9) . . . . ? O4 Ti1 O3 C12 -25.6(10) . . . . ? O4 Ti1 O3 C12 0.8(9) 2_656 . . . ? N1 Ti1 O3 C12 -78.6(9) . . . . ? Ti1 Ti1 O3 C12 -4.5(9) 2_656 . . . ? O3 Ti1 O4 C2 -155.53(19) . . . . ? O1 Ti1 O4 C2 -16.85(13) . . . . ? O2 Ti1 O4 C2 83.06(13) . . . . ? O4 Ti1 O4 C2 176.78(15) 2_656 . . . ? N1 Ti1 O4 C2 -101.54(13) . . . . ? Ti1 Ti1 O4 C2 176.78(15) 2_656 . . . ? O3 Ti1 O4 Ti1 27.7(2) . . . 2_656 ? O1 Ti1 O4 Ti1 166.37(6) . . . 2_656 ? O2 Ti1 O4 Ti1 -93.71(6) . . . 2_656 ? O4 Ti1 O4 Ti1 0.0 2_656 . . 2_656 ? N1 Ti1 O4 Ti1 81.69(6) . . . 2_656 ? O3 Ti1 O2 C8 38.05(15) . . . . ? O1 Ti1 O2 C8 -60.31(15) . . . . ? O4 Ti1 O2 C8 -154.95(14) . . . . ? O4 Ti1 O2 C8 133.00(14) 2_656 . . . ? N1 Ti1 O2 C8 179.0(3) . . . . ? Ti1 Ti1 O2 C8 168.64(14) 2_656 . . . ? O3 Ti1 O1 C5 20.26(18) . . . . ? O2 Ti1 O1 C5 119.88(17) . . . . ? O4 Ti1 O1 C5 -149.75(17) . . . . ? O4 Ti1 O1 C5 -105.6(2) 2_656 . . . ? N1 Ti1 O1 C5 -69.09(17) . . . . ? Ti1 Ti1 O1 C5 -139.23(16) 2_656 . . . ? O3 Ti1 N1 C13 6.33(13) . . . . ? O1 Ti1 N1 C13 103.08(13) . . . . ? O2 Ti1 N1 C13 -135.1(3) . . . . ? O4 Ti1 N1 C13 -161.49(13) . . . . ? O4 Ti1 N1 C13 -88.17(13) 2_656 . . . ? Ti1 Ti1 N1 C13 -124.51(13) 2_656 . . . ? Ti1 N1 C13 C14 171.00(12) . . . . ? Ti1 O4 C2 C1 79.56(17) . . . . ? Ti1 O4 C2 C1 -104.11(15) 2_656 . . . ? Ti1 O4 C2 C3 -46.7(2) . . . . ? Ti1 O4 C2 C3 129.65(14) 2_656 . . . ? Ti1 O3 C12 C10 160.9(8) . . . . ? Ti1 O3 C12 C11 -75.6(10) . . . . ? Ti1 O2 C8 C7 109.06(17) . . . . ? Ti1 O2 C8 C9 -128.27(15) . . . . ? Ti1 O1 C5 C6 -103.9(2) . . . . ? Ti1 O1 C5 C4 133.29(18) . . . . ? N1 C13 C14 C15 65.5(2) . . . . ? C13 C14 C15 C15 179.02(19) . . . 2_566 ? C19 C18 C17 C16 -180.0(5) . . . . ? C16 C18 C17 C16 2.1(8) 2_565 . . . ? C18 C17 C16 C18 -2.1(7) . . . 2_565 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O2 0.92 2.06 2.9512(19) 161.7 2_656 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.470 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.054 #===END