#Supplementary Material (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2001 data_global _audit_creation_date 08-02-2001 # 1. SUBMISSION DETAILS _journal_coden_Cambridge 186 _publ_contact_author 'Prof Marc Henry' _publ_contact_author_address ; Prof Marc Henry Chimie Moleculaire de l'Etat Solide Universite Louis Pasteur UMR CNRS/ULP 7513 Institute Le Bel 4 Rue Blaise Pascal Strasbourg Cedex 67070 FRANCE ; _publ_contact_author_phone '+33.3.90.24.13.56' _publ_contact_author_fax '+33.3.90.24.13.29' _publ_contact_author_email henry@chimie.u-strasbg.fr _publ_requested_journal Dalton Transactions' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for publication as a new structure paper in Dalton Transactions. The figures, chemical structure diagram (scheme), Transfert of Copyright Agreement form and structure factors will be sent on receipt of your acknowledgement lett= er ; #=========================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) #=========================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Mechanistic aspects of the hydrolysis and condensation of titanium alkoxides complexed by tripodal ligands ; loop_ _publ_author_name _publ_author_address 'Weymann-Schildknecht, Sandrine' ; Laboratoire de Chimie Moleculaire de l'etat Solide Universite Louis Pasteur, Institut Le Bel UMR CNRS/ULP 7513 4, Rue Blaise Pascal 67070 Strasbourg Cedex FRANCE ; 'Henry, Marc' ; Laboratoire de Chimie Moleculaire de l'etat Solide Universite Louis Pasteur, Institut Le Bel UMR CNRS/ULP 7513 4, Rue Blaise Pascal 67070 Strasbourg Cedex FRANCE ; # 4. TEXT #=========================================================================== data_ST821 _database_code_CSD 158128 #=========================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C38H82N2O20Ti4' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C38H82N2O20Ti4' _chemical_formula_weight 1078.7 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 'International_Tables_Vol_IV_Table_2.3.1' H ? 0.000 0.000 'International_Tables_Vol_IV_Table_2.3.1' O ? 0.008 0.006 'International_Tables_Vol_IV_Table_2.3.1' Ti ? 0.248 0.446 'International_Tables_Vol_IV_Table_2.3.1' #=========================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P21/n' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 13.970(4) _cell_length_b 11.088(3) _cell_length_c 17.488(5) _cell_angle_alpha 90.0 _cell_angle_beta 96.19(2) _cell_angle_gamma 90.0 _cell_volume 3101(1) _cell_formula_units_z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 3 _cell_measurement_theta_max 54 _cell_special_details ; ? ; _exptl_crystal_description prism _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method 'none' _exptl_absorpt_coefficient_mu 54.840 #=========================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type Cu-K\a _diffrn_radiation_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device Philips PW1100/16 _diffrn_measurement_method \q/2\q _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3 _diffrn_reflns_theta_max 54 _reflns_number_total 3552 _reflns_number_observed 2622 _reflns_observed_criterion >3.0\s(I) #=========================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^) + 0.0064 Fo^4^)' _refine_ls_hydrogen_treatment included_not_refined _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 6263 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_number_constraints 8 _refine_ls_abs_structure_details ; ? ; _refine_ls_R_factor_obs 0.043 _refine_ls_wR_factor_obs 0.063 _refine_ls_goodness_of_fit_obs 1.406 _refine_ls_shift/esd_max 0.07 _refine_ls_shift/esd_mean 0.08 _refine_diff_density_max 1.37 _refine_diff_density_min 0.81 #=========================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol TI1 0.80928(4) -0.07990(6) 1.02252(4) 2.33(1) Biso ? ? Ti TI2 0.95706(4) 0.04944(6) 0.90746(4) 2.32(1) Biso ? ? Ti O1 0.7227(2) 0.0230(2) 0.9768(2) 3.32(6) Biso ? ? O C1 0.6564(3) 0.0554(5) 0.9138(3) 5.7(1) Biso ? ? C C2 0.5886(4) 0.1490(6) 0.9388(4) 8.6(2) Biso ? ? C C3 0.6026(4) -0.0527(7) 0.8799(4) 8.8(2) Biso ? ? C O2 0.7813(2) -0.0520(2) 1.1202(1) 2.95(5) Biso ? ? O C4 0.6915(3) -0.0144(4) 1.1457(2) 3.56(9) Biso ? ? C C5 0.6743(3) -0.0833(5) 1.2169(3) 5.1(1) Biso ? ? C C6 0.6926(3) 0.1197(5) 1.1581(3) 5.4(1) Biso ? ? C O3 0.7513(2) -0.2240(2) 1.0026(1) 3.02(5) Biso ? ? O C7 0.6860(3) -0.3007(4) 1.0361(2) 3.87(9) Biso ? ? C C8 0.7387(4) -0.3682(5) 1.1029(3) 5.6(1) Biso ? ? C C9 0.6366(5) -0.3794(6) 0.9771(4) 9.1(2) Biso ? ? C O4 0.9286(2) 0.0582(2) 1.0267(1) 2.09(5) Biso ? ? O C10 0.9151(2) 0.1763(3) 1.0562(2) 2.70(8) Biso ? ? C C11 1.0068(2) 0.2537(3) 1.0561(2) 2.83(8) Biso ? ? C C12 1.0930(3) 0.2077(3) 1.1082(2) 3.11(8) Biso ? ? C O5 1.1230(2) 0.0929(2) 1.0822(1) 2.40(5) Biso ? ? O N1 0.9795(2) 0.3765(3) 1.0857(2) 4.42(8) Biso ? ? N O6 0.9141(3) 0.4318(3) 1.0482(2) 7.1(1) Biso ? ? O O7 1.0210(3) 0.4141(3) 1.1441(2) 8.0(1) Biso ? ? O C13 1.0351(3) 0.2773(3) 0.9741(2) 2.91(8) Biso ? ? C O8 1.0600(2) 0.1680(2) 0.9397(1) 2.32(5) Biso ? ? O O9 0.9968(2) 0.0085(2) 0.8191(1) 3.13(5) Biso ? ? O C14 1.0440(3) -0.0023(4) 0.7505(2) 3.54(9) Biso ? ? C C15 1.0588(3) 0.1213(5) 0.7196(2) 4.8(1) Biso ? ? C C16 0.9853(4) -0.0848(5) 0.6944(3) 5.4(1) Biso ? ? C O10 0.8691(2) 0.1626(2) 0.8796(1) 3.26(6) Biso ? ? O C17 0.8490(3) 0.2491(4) 0.8194(3) 4.9(1) Biso ? ? C C18 0.7937(4) 0.1880(6) 0.7498(3) 7.5(2) Biso ? ? C C19 0.7969(4) 0.3546(5) 0.8478(4) 7.8(1) Biso ? ? C H1 0.6905 0.0883 0.8745 7 Biso ? ? H H2 0.5437 0.1709 0.8963 11 Biso ? ? H H3 0.5550 0.1170 0.9786 11 Biso ? ? H H4 0.6241 0.2181 0.9571 11 Biso ? ? H H5 0.5584 -0.0281 0.8375 11 Biso ? ? H H6 0.6469 -0.1089 0.8627 11 Biso ? ? H H7 0.5683 -0.0893 0.9178 11 Biso ? ? H H8 0.6394 -0.0317 1.1077 4 Biso ? ? H H9 0.6149 -0.0585 1.2338 6 Biso ? ? H H10 0.6718 -0.1671 1.2057 6 Biso ? ? H H11 0.7252 -0.0677 1.2562 6 Biso ? ? H H12 0.6332 0.1443 1.1749 7 Biso ? ? H H13 0.7439 0.1402 1.1959 7 Biso ? ? H H14 0.7013 0.1592 1.1111 7 Biso ? ? H H15 0.6371 -0.2547 1.0563 5 Biso ? ? H H16 0.6948 -0.4194 1.1252 7 Biso ? ? H H17 0.7885 -0.4153 1.0851 7 Biso ? ? H H18 0.7657 -0.3121 1.1403 7 Biso ? ? H H19 0.5930 -0.4304 0.9999 11 Biso ? ? H H20 0.6020 -0.3316 0.9383 11 Biso ? ? H H21 0.6827 -0.4272 0.9548 11 Biso ? ? H H22 0.8990 0.1697 1.1074 3 Biso ? ? H H23 0.8639 0.2146 1.0251 3 Biso ? ? H H24 1.0759 0.1999 1.1590 4 Biso ? ? H H25 1.1445 0.2635 1.1077 4 Biso ? ? H H26 1.0886 0.3305 0.9772 3 Biso ? ? H H27 0.9822 0.3129 0.9435 3 Biso ? ? H H28 1.1058 -0.0380 0.7603 4 Biso ? ? H H29 1.0899 0.1154 0.6740 6 Biso ? ? H H30 0.9981 0.1598 0.7081 6 Biso ? ? H H31 1.0975 0.1672 0.7569 6 Biso ? ? H H32 1.0161 -0.0923 0.6488 6 Biso ? ? H H33 0.9801 -0.1620 0.7171 6 Biso ? ? H H34 0.9227 -0.0517 0.6821 6 Biso ? ? H H35 0.9072 0.2793 0.8033 6 Biso ? ? H H36 0.7802 0.2453 0.7096 9 Biso ? ? H H37 0.8314 0.1243 0.7323 9 Biso ? ? H H38 0.7349 0.1562 0.7639 9 Biso ? ? H H39 0.7839 0.4114 0.8074 10 Biso ? ? H H40 0.7380 0.3282 0.8647 10 Biso ? ? H H41 0.8356 0.3912 0.8894 10 Biso ? ? H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol TI1 0.0250(3) 0.0297(3) 0.0339(3) 0.0002(3) 0.0025(3) 0.0003(3) Ti TI2 0.0269(3) 0.0303(3) 0.0302(3) 0.0009(3) 0.0006(3) 0.0046(3) Ti O1 0.030(1) 0.046(1) 0.050(1) 0.007(1) 0.002(1) 0.008(1) O C1 0.037(2) 0.110(4) 0.069(3) 0.013(3) 0.004(2) 0.040(3) C C2 0.066(3) 0.099(4) 0.158(6) 0.036(3) 0.006(4) 0.040(4) C C3 0.074(4) 0.162(6) 0.089(4) 0.015(4) 0.036(3) 0.028(4) C O2 0.033(1) 0.044(1) 0.035(1) 0.004(1) 0.006(1) 0.004(1) O C4 0.032(2) 0.058(3) 0.046(2) 0.002(2) 0.008(2) 0.011(2) C C5 0.051(2) 0.091(4) 0.057(3) 0.002(3) 0.025(2) 0.009(3) C C6 0.057(3) 0.060(3) 0.093(3) 0.010(2) 0.023(2) 0.028(3) C O3 0.035(1) 0.038(1) 0.042(1) 0.011(1) 0.008(1) 0.001(1) O C7 0.044(2) 0.051(2) 0.054(2) 0.014(2) 0.013(2) 0.003(2) C C8 0.067(3) 0.065(3) 0.086(3) 0.007(3) 0.025(2) 0.025(3) C C9 0.135(4) 0.125(4) 0.090(4) 0.094(3) 0.025(3) 0.034(3) C O4 0.027(1) 0.019(1) 0.034(1) 0.003(1) 0.005(1) 0.000(1) O C10 0.032(2) 0.028(2) 0.043(2) 0.001(2) 0.009(2) 0.003(2) C C11 0.029(2) 0.024(2) 0.056(2) 0.001(2) 0.011(2) 0.009(2) C C12 0.045(2) 0.037(2) 0.038(2) 0.013(2) 0.011(2) 0.012(2) C O5 0.027(1) 0.033(1) 0.031(1) 0.006(1) 0.003(1) 0.000(1) O N1 0.052(2) 0.035(2) 0.086(2) 0.012(2) 0.029(2) 0.020(2) N O6 0.085(2) 0.042(2) 0.146(3) 0.019(2) 0.032(2) 0.012(2) O O7 0.107(3) 0.069(2) 0.129(3) 0.004(2) 0.017(2) 0.060(2) O C13 0.033(2) 0.021(2) 0.056(2) 0.001(2) 0.004(2) 0.004(2) C O8 0.028(1) 0.025(1) 0.036(1) 0.002(1) 0.005(1) 0.003(1) O O9 0.041(1) 0.048(2) 0.029(1) 0.010(1) 0.004(1) 0.001(1) O C14 0.042(2) 0.059(3) 0.035(2) 0.011(2) 0.011(2) 0.003(2) C C15 0.069(3) 0.073(3) 0.041(2) 0.017(3) 0.012(2) 0.009(2) C C16 0.068(3) 0.093(4) 0.044(2) 0.027(3) 0.013(2) 0.016(2) C O10 0.031(1) 0.045(1) 0.048(1) 0.001(1) 0.000(1) 0.015(1) O C17 0.039(2) 0.067(3) 0.080(3) 0.005(2) 0.000(2) 0.049(2) C C18 0.064(3) 0.153(5) 0.062(3) 0.009(4) 0.021(3) 0.047(3) C C19 0.061(3) 0.076(3) 0.157(5) 0.020(3) 0.002(3) 0.063(3) C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag TI1 O1 1.788(2) . . ? C7 C8 1.511(5) . . ? TI1 O2 1.819(2) . . ? C7 C9 1.466(5) . . ? TI1 O3 1.808(2) . . ? O4 C10 1.428(3) . . ? TI1 O4 2.258(2) . . ? C10 C11 1.542(4) . . ? TI1 O5 2.155(2) . . ? C11 C12 1.518(4) . . ? TI1 O8 2.113(2) . . ? C11 N1 1.520(4) . . ? TI2 O4 2.167(2) . . ? C11 C13 1.550(4) . . ? TI2 O4 2.215(2) . . ? C12 O5 1.430(3) . . ? TI2 O5 1.953(2) . . ? N1 O6 1.231(4) . . ? TI2 O8 1.984(2) . . ? N1 O7 1.192(4) . . ? TI2 O9 1.757(2) . . ? O6 O7 2.131(5) . . ? TI2 O10 1.786(2) . . ? C13 O8 1.413(3) . . ? O1 C1 1.407(4) . . ? O9 C14 1.435(3) . . ? C1 C2 1.501(6) . . ? C14 C15 1.496(5) . . ? C1 C3 1.502(6) . . ? C14 C16 1.515(5) . . ? O2 C4 1.439(3) . . ? O10 C17 1.430(3) . . ? C4 C5 1.502(5) . . ? C17 C18 1.528(6) . . ? C4 C6 1.502(5) . . ? C17 C19 1.491(6) . . ? O3 C7 1.419(3) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 TI1 O2 96.21(9) . . . ? O4 TI2 O8 75.46(6) . . . ? O1 TI1 O3 102.10(9) . . . ? O4 TI2 O9 92.27(8) . . . ? O1 TI1 O4 92.49(8) . . . ? O4 TI2 O10 163.02(8) . . . ? O1 TI1 O5 90.02(8) . . . ? O5 TI2 O8 155.91(7) . . . ? O1 TI1 O8 162.76(8) . . . ? O5 TI2 O9 96.36(8) . . . ? O2 TI1 O3 101.22(8) . . . ? O5 TI2 O10 102.05(8) . . . ? O2 TI1 O4 94.97(8) . . . ? O8 TI2 O9 97.68(8) . . . ? O2 TI1 O5 165.37(8) . . . ? O8 TI2 O10 93.92(8) . . . ? O2 TI1 O8 92.94(7) . . . ? O9 TI2 O10 102.40(9) . . . ? O3 TI1 O4 156.77(7) . . . ? TI1 O1 C1 150.4(2) . . . ? O3 TI1 O5 90.33(7) . . . ? O1 C1 C2 109.4(4) . . . ? O3 TI1 O8 90.36(8) . . . ? O1 C1 C3 111.4(3) . . . ? O4 TI1 O5 71.48(6) . . . ? C2 C1 C3 111.2(4) . . . ? O4 TI1 O8 72.13(6) . . . ? TI1 O2 C4 128.6(2) . . . ? O5 TI1 O8 77.90(6) . . . ? O2 C4 C5 109.5(3) . . . ? O4 TI2 O4 73.79(7) . . . ? O2 C4 C6 109.5(3) . . . ? O4 TI2 O5 77.32(7) . . . ? C5 C4 C6 112.6(3) . . . ? O4 TI2 O8 84.22(6) . . . ? TI1 O3 C7 138.1(2) . . . ? O4 TI2 O9 165.06(8) . . . ? O3 C7 C8 109.6(3) . . . ? O4 TI2 O10 92.22(7) . . . ? O3 C7 C9 110.0(3) . . . ? O4 TI2 O5 84.52(7) . . . ? C8 C7 C9 113.7(4) . . . ? TI1 O4 TI2 98.64(7) . . . ? C11 N1 O6 117.6(3) . . . ? TI1 O4 TI2 98.05(6) . . . ? C11 N1 O7 119.3(3) . . . ? TI1 O4 C10 120.5(1) . . . ? O6 N1 O7 123.1(3) . . . ? TI2 O4 TI2 106.21(7) . . . ? N1 O6 O7 28.0(2) . . . ? TI2 O4 C10 115.7(1) . . . ? N1 O7 O6 28.9(2) . . . ? TI2 O4 C10 115.0(1) . . . ? C11 C13 O8 110.3(2) . . . ? O4 C10 C11 111.6(2) . . . ? TI1 O8 TI2 110.99(8) . . . ? C10 C11 C12 114.7(2) . . . ? TI1 O8 C13 120.5(2) . . . ? C10 C11 N1 105.0(2) . . . ? TI2 O8 C13 119.1(1) . . . ? C10 C11 C13 113.0(2) . . . ? TI2 O9 C14 166.9(2) . . . ? C12 C11 N1 107.9(2) . . . ? O9 C14 C15 108.6(3) . . . ? C12 C11 C13 110.3(2) . . . ? O9 C14 C16 109.0(2) . . . ? N1 C11 C13 105.2(2) . . . ? C15 C14 C16 113.9(3) . . . ? C11 C12 O5 110.4(2) . . . ? TI2 O10 C17 138.3(2) . . . ? TI1 O5 TI2 109.45(8) . . . ? O10 C17 C18 109.4(3) . . . ? TI1 O5 C12 120.0(1) . . . ? O10 C17 C19 110.1(3) . . . ? TI2 O5 C12 120.0(1) . . . ? C18 C17 C19 113.0(3) . . . ? #======END data_ST854 _database_code_CSD 158129 #=========================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C28H62N2O20Ti4' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28H62N2O20Ti4' _chemical_formula_weight 938.4 _chemical_melting_point ? _chemical_compound_source ? #=========================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C2/c' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z -x,y,1/2-z 1/2+x,1/2+y,z x,-y,1/2+z 1/2-x,1/2-y,-z _cell_length_a 13.351(5) _cell_length_b 13.158(4) _cell_length_c 13.182(5) _cell_angle_alpha 90.0 _cell_angle_beta 102.44(2) _cell_angle_gamma 90.0 _cell_volume 4287(1) _cell_formula_units_z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; ? ; _exptl_crystal_description prism _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_method 'none' _exptl_absorpt_coefficient_mu 68.101 #=========================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type Cu-K\a _diffrn_radiation_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device Philips PW1100/16 _diffrn_measurement_method \q/2\q _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3 _diffrn_reflns_theta_max 52 _reflns_number_total 2634 _reflns_number_observed 1763 _reflns_observed_criterion >3.0\s(I) #=========================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^) + 0.0064 Fo^4^)' _refine_ls_hydrogen_treatment included_not_refined _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 6263 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_number_constraints 8 _refine_ls_abs_structure_details ; ? ; _refine_ls_R_factor_obs 0.048 _refine_ls_wR_factor_obs 0.070 _refine_ls_goodness_of_fit_obs 1.439 _refine_ls_shift/esd_max 0.08 _refine_ls_shift/esd_mean 0.03 _refine_diff_density_max 1.17 _refine_diff_density_min 0.82 #=========================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol TI1 0.60998(6) 0.27999(9) 0.53987(6) 4.95(3) Biso ? ? Ti TI2 0.73303(5) 0.11918(8) 0.49251(5) 4.23(2) Biso ? ? Ti O1 0.5180(2) 0.3036(4) 0.4851(2) 7.2(1) Biso ? ? O C1 0.4547(4) 0.3605(7) 0.4693(5) 9.8(3) Biso ? ? C C2 0.4101(4) 0.3603(7) 0.5263(5) 11.5(3) Biso ? ? C O2 0.5911(2) 0.1729(3) 0.5945(2) 5.9(1) Biso ? ? O C3 0.5385(4) 0.0951(6) 0.5764(5) 9.3(2) Biso ? ? C C4 0.5097(5) 0.0602(9) 0.6394(6) 16.2(3) Biso ? ? C O3 0.6217(2) 0.3732(3) 0.6135(2) 6.7(1) Biso ? ? O C5 0.6043(6) 0.3962(9) 0.6808(5) 14.5(3) Biso ? ? C C6 0.6000(9) 0.359(1) 0.7317(6) 24.2(6) Biso ? ? C O4 0.6325(2) 0.1750(3) 0.4577(2) 4.12(8) Biso ? ? O C7 0.6052(3) 0.1915(5) 0.3804(3) 5.2(2) Biso ? ? C C8 0.6443(3) 0.2809(5) 0.3522(3) 5.1(1) Biso ? ? C C9 0.7278(3) 0.2626(4) 0.3579(3) 4.4(1) Biso ? ? C O5 0.7669(2) 0.2508(2) 0.4341(2) 3.80(8) Biso ? ? O N1 0.6125(3) 0.2975(5) 0.2694(3) 7.4(2) Biso ? ? N O6 0.5592(6) 0.3640(8) 0.2512(6) 10.1(3) Biso ? ? O O7 0.5926(5) 0.2255(5) 0.2337(3) 15.0(3) Biso ? ? O O6' 0.3609(5) 0.3467(8) 0.2701(4) 9.0(3) Biso ? ? O C10 0.6275(3) 0.3783(5) 0.3897(3) 5.5(2) Biso ? ? C O8 0.6579(2) 0.3752(3) 0.4688(2) 4.61(9) Biso ? ? O O9 0.7175(2) 0.0325(3) 0.5619(2) 5.8(1) Biso ? ? O C11 0.7085(6) -0.0522(8) 0.5979(8) 23.2(4) Biso ? ? C C12 0.7032(9) -0.1283(8) 0.600(1) 21.2(6) Biso ? ? C O10 0.7299(2) 0.0396(3) 0.4140(2) 5.7(1) Biso ? ? O C13 0.7363(6) -0.0404(8) 0.3684(6) 16.1(3) Biso ? ? C C14 0.6950(7) -0.0951(9) 0.3292(7) 19.3(4) Biso ? ? C H1 0.4244 0.3354 0.4237 12 Biso ? ? H H2 0.4686 0.4287 0.4622 12 Biso ? ? H H3 0.3673 0.4019 0.5101 14 Biso ? ? H H4 0.3947 0.2928 0.5338 14 Biso ? ? H H5 0.4389 0.3860 0.5722 14 Biso ? ? H H6 0.5613 0.0392 0.5570 12 Biso ? ? H H7 0.4980 0.1194 0.5387 12 Biso ? ? H H8 0.4743 0.0075 0.6235 21 Biso ? ? H H9 0.5494 0.0349 0.6773 21 Biso ? ? H H10 0.4861 0.1150 0.6591 21 Biso ? ? H H11 0.5559 0.4247 0.6650 18 Biso ? ? H H12 0.6391 0.4486 0.6989 18 Biso ? ? H H13 0.5855 0.4067 0.7649 31 Biso ? ? H H14 0.5636 0.3065 0.7207 31 Biso ? ? H H15 0.6469 0.3304 0.7546 31 Biso ? ? H H16 0.5532 0.2053 0.3717 6 Biso ? ? H H17 0.6132 0.1320 0.3536 6 Biso ? ? H H18 0.7480 0.3189 0.3365 5 Biso ? ? H H19 0.7339 0.2027 0.3307 5 Biso ? ? H H20 0.5750 0.3869 0.3812 7 Biso ? ? H H21 0.6487 0.4338 0.3683 7 Biso ? ? H H22 0.6636 -0.0341 0.6127 30 Biso ? ? H H23 0.7494 -0.0443 0.6394 30 Biso ? ? H H24 0.6972 -0.1470 0.6492 27 Biso ? ? H H25 0.6608 -0.1496 0.5639 27 Biso ? ? H H26 0.7467 -0.1598 0.5906 27 Biso ? ? H H27 0.7670 -0.0861 0.4017 20 Biso ? ? H H28 0.7640 -0.0120 0.3348 20 Biso ? ? H H29 0.7224 -0.1422 0.3063 25 Biso ? ? H H30 0.6660 -0.1307 0.3582 25 Biso ? ? H H31 0.6629 -0.0566 0.2912 25 Biso ? ? H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol TI1 0.0514(5) 0.0830(7) 0.0563(6) 0.0004(6) 0.0178(4) 0.0030(6) Ti TI2 0.0601(6) 0.0482(5) 0.0526(5) 0.0040(5) 0.0124(5) 0.0024(5) Ti O1 0.056(2) 0.132(4) 0.087(3) 0.022(3) 0.018(2) 0.006(3) O C1 0.075(5) 0.169(8) 0.128(6) 0.032(5) 0.019(4) 0.008(6) C C2 0.099(5) 0.176(8) 0.178(7) 0.047(5) 0.066(4) 0.001(7) C O2 0.066(2) 0.091(3) 0.070(2) 0.023(2) 0.023(2) 0.002(2) O C3 0.103(5) 0.100(6) 0.154(7) 0.012(5) 0.037(5) 0.004(5) C C4 0.229(7) 0.189(9) 0.245(8) 0.096(6) 0.155(5) 0.006(7) C O3 0.097(3) 0.091(3) 0.079(2) 0.001(2) 0.048(2) 0.020(2) O C5 0.218(8) 0.24(1) 0.121(5) 0.082(8) 0.101(5) 0.080(6) C C6 0.46(2) 0.37(2) 0.137(7) 0.18(1) 0.158(8) 0.09(1) C O4 0.049(2) 0.065(2) 0.041(2) 0.008(2) 0.005(2) 0.001(2) O C7 0.053(3) 0.083(4) 0.059(3) 0.008(3) 0.007(3) 0.006(3) C C8 0.063(3) 0.080(4) 0.045(3) 0.002(3) 0.002(3) 0.009(3) C C9 0.050(3) 0.071(4) 0.046(3) 0.008(3) 0.005(2) 0.001(3) C O5 0.052(2) 0.054(2) 0.037(2) 0.004(2) 0.006(2) 0.001(2) O N1 0.071(3) 0.136(5) 0.057(3) 0.012(4) 0.021(3) 0.013(3) N O6 0.135(9) 0.150(9) 0.080(6) 0.034(7) 0.021(7) 0.036(6) O O7 0.273(8) 0.201(6) 0.069(4) 0.041(6) 0.022(5) 0.009(4) O O6' 0.120(7) 0.173(8) 0.042(4) 0.066(6) 0.001(4) 0.044(5) O C10 0.054(3) 0.087(4) 0.063(4) 0.008(3) 0.001(3) 0.021(3) C O8 0.058(2) 0.060(2) 0.058(2) 0.010(2) 0.014(2) 0.006(2) O O9 0.088(3) 0.057(2) 0.075(2) 0.008(2) 0.018(2) 0.016(2) O C11 0.172(9) 0.167(7) 0.57(1) 0.046(7) 0.144(9) 0.239(7) C C12 0.33(2) 0.126(9) 0.35(2) 0.050(9) 0.07(1) 0.07(1) C O10 0.086(3) 0.061(2) 0.070(2) 0.002(2) 0.016(2) 0.019(2) O C13 0.157(8) 0.190(8) 0.277(9) 0.043(7) 0.070(7) 0.162(6) C C14 0.20(1) 0.26(1) 0.27(1) 0.054(9) 0.044(9) 0.194(7) C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag TI1 O1 1.792(3) . . ? O4 C7 1.402(5) . . ? TI1 O2 1.800(3) . . ? C7 C8 1.525(6) . . ? TI1 O3 1.794(3) . . ? C8 C9 1.531(6) . . ? TI1 O4 2.140(3) . . ? C8 N1 1.508(6) . . ? TI1 O5 2.243(3) . . ? C8 C10 1.513(6) . . ? TI1 O8 2.122(3) . . ? C9 O5 1.424(5) . . ? TI2 O4 1.960(3) . . ? N1 O6 1.302(9) . . ? TI2 O5 2.191(2) . . ? N1 O7 1.161(7) . . ? TI2 O5 2.170(3) . . ? N1 O6' 1.151(7) . . ? TI2 O8 1.974(3) . . ? O6 O7 1.97(1) . . ? TI2 O9 1.768(3) . . ? O6 O6' 1.61(1) . . ? TI2 O10 1.761(3) . . ? O7 O6' 1.82(1) . . ? O1 C1 1.359(6) . . ? C10 O8 1.428(5) . . ? C1 C2 1.454(9) . . ? O9 C11 1.321(9) . . ? O2 C3 1.397(7) . . ? C11 C12 1.01(1) . . ? C3 C4 1.438(9) . . ? O10 C13 1.361(8) . . ? O3 C5 1.362(8) . . ? C13 C14 1.17(1) . . ? C5 C6 1.07(1) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 TI1 O2 99.9(2) . . . ? O5 TI2 O8 76.8(1) . . . ? O1 TI1 O3 104.1(2) . . . ? O5 TI2 O9 164.1(1) . . . ? O1 TI1 O4 91.4(1) . . . ? O5 TI2 O10 92.3(1) . . . ? O1 TI1 O5 159.0(1) . . . ? O5 TI2 O8 83.4(1) . . . ? O1 TI1 O8 91.3(1) . . . ? O5 TI2 O9 92.8(1) . . . ? O2 TI1 O3 97.4(2) . . . ? O5 TI2 O10 164.4(1) . . . ? O2 TI1 O4 88.2(1) . . . ? O8 TI2 O9 94.4(1) . . . ? O2 TI1 O5 92.7(1) . . . ? O8 TI2 O10 99.4(1) . . . ? O2 TI1 O8 162.3(1) . . . ? O9 TI2 O10 102.3(1) . . . ? O3 TI1 O4 162.2(1) . . . ? O1 C1 C2 115.8(6) . . . ? O3 TI1 O5 90.7(1) . . . ? O2 C3 C4 113.6(6) . . . ? O3 TI1 O8 93.0(1) . . . ? O3 C5 C6 139.(2) . . . ? O4 TI1 O5 72.17(9) . . . ? O4 C7 C8 111.4(3) . . . ? O4 TI1 O8 77.8(1) . . . ? C7 C8 C9 113.1(4) . . . ? O5 TI1 O8 72.8(1) . . . ? C7 C8 N1 109.8(4) . . . ? O4 TI2 O5 83.8(1) . . . ? C7 C8 C10 110.2(4) . . . ? O4 TI2 O5 77.2(1) . . . ? C9 C8 N1 104.9(4) . . . ? O4 TI2 O8 155.9(1) . . . ? C9 C8 C10 113.6(4) . . . ? O4 TI2 O9 100.8(1) . . . ? N1 C8 C10 104.8(4) . . . ? O4 TI2 O10 95.6(1) . . . ? C8 C9 O5 111.8(3) . . . ? O5 TI2 O5 73.3(1) . . . ? C8 N1 O6 117.3(6) . . . ? C8 N1 O7 116.6(6) . . . ? N1 O7 O6' 38.0(4) . . . ? C8 N1 O6' 125.4(6) . . . ? O6 O7 O6' 50.2(5) . . . ? O6 N1 O7 106.1(6) . . . ? N1 O6' O6 53.1(5) . . . ? O6 N1 O6' 81.9(8) . . . ? N1 O6' O7 38.4(4) . . . ? O7 N1 O6' 103.6(7) . . . ? O6 O6' O7 69.8(5) . . . ? N1 O6 O7 34.5(4) . . . ? C8 C10 O8 110.9(3) . . . ? N1 O6 O6' 45.0(5) . . . ? O9 C11 C12 152.(2) . . . ? O7 O6 O6' 60.0(5) . . . ? O10 C13 C14 136.(1) . . . ? N1 O7 O6 39.4(4) . . . ? #======END data_ST874 _database_code_CSD 158130 #=========================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C80H168N4O38Ti8' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C80H168N4O38Ti8' _chemical_formula_weight 2177.4 _chemical_melting_point ? _chemical_compound_source ? #=========================================================================== # 6. CRYSTAL DATA _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 11.057(3) _cell_length_b 14.115(4) _cell_length_c 18.362(5) _cell_angle_alpha 70.45(2) _cell_angle_beta 81.54(2) _cell_angle_gamma 86.30(2) _cell_volume 2671(1) _cell_formula_units_z 1 _cell_measurement_temperature 173 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; ? ; _exptl_crystal_description prism _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'none' _exptl_absorpt_coefficient_mu 6.358 _exptl_absorpt_correction_type 'psi_scans_(North,_Phillips,_Mathews,_1968)' _exptl_absorpt_correction_T_min 0.9210 _exptl_absorpt_correction_T_max 1.0000 #=========================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device Enraf_Nonius_CAD4 _diffrn_measurement_method \q/2\q _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2 _diffrn_reflns_theta_max 26 _reflns_number_total 11266 _reflns_number_observed 5089 _reflns_observed_criterion >3.0\s(I) #_computing_data_collection 'CAD4_(Enraf-Nonius,_1994)' _computing_cell_refinement CAD4_(Enraf-Nonius,_1994) _computing_data_reduction 'process_MolEN_(Fair,_1990)' _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_MolEN_(Fair,_1990) _computing_molecular_graphics ? _computing_publication_material BTABLE_PTABLE_CIF_IN_MolEN_(Fair,_1990) #========================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^) + 0.0064 Fo^4^)' _refine_ls_hydrogen_treatment 'included_not_refined' _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5089 _refine_ls_number_parameters 525 _refine_ls_number_restraints 0 _refine_ls_number_constraints 8 _refine_ls_abs_structure_details ; ? ; _refine_ls_R_factor_obs 0.078 _refine_ls_wR_factor_obs 0.093 _refine_ls_goodness_of_fit_obs 1.181 _refine_ls_shift/esd_max 0.11 _refine_ls_shift/esd_mean 0.08 _refine_diff_density_max 1.00 _refine_diff_density_min 0.90 #=========================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol TI1 0.4793(1) 0.0337(1) 1.23996(9) 3.22(4) Biso ? ? Ti TI2 0.5943(1) -0.0856(1) 1.10518(8) 2.43(3) Biso ? ? Ti TI3 0.5724(1) -0.2047(1) 1.29730(9) 3.38(4) Biso ? ? Ti TI4 0.4937(1) -0.1541(1) 0.95078(8) 2.78(3) Biso ? ? Ti O1 0.4486(5) -0.1519(4) 0.8457(3) 3.6(1) Biso ? ? O C1 0.455(1) -0.2487(7) 0.8299(6) 4.8(2) Biso ? ? C C2 0.325(1) -0.2832(9) 0.8383(7) 6.9(3) Biso ? ? C C3 0.337(1) -0.3935(9) 0.8265(9) 10.1(4) Biso ? ? C C4 0.216(2) -0.427(2) 0.835(2) 16.7(9)* Biso ? ? C O2 0.5467(6) 0.0527(5) 1.3145(4) 4.8(2) Biso ? ? O C5 0.610(1) 0.051(1) 1.3768(7) 8.9(4) Biso ? ? C C6 0.591(1) 0.142(1) 1.3982(7) 8.3(4) Biso ? ? C C7 0.656(2) 0.134(1) 1.4701(8) 11.5(4) Biso ? ? C C8 0.654(2) 0.223(2) 1.485(1) 14.9(6) Biso ? ? C O3 0.3324(6) 0.0878(4) 1.2529(3) 4.6(2) Biso ? ? O C9 0.254 0.146 1.290 16* Biso ? ? C C10 0.133 0.104 1.339 15* Biso ? ? C C11 0.081 0.218 1.303 15* Biso ? ? C C12 -0.049 0.229 1.327 15* Biso ? ? C O4 0.4215(5) -0.1059(4) 1.2926(3) 3.3(1) Biso ? ? O C13 0.3019(8) -0.1316(7) 1.2850(5) 3.7(2) Biso ? ? C C14 0.3040(7) -0.1350(7) 1.2013(5) 3.1(2) Biso ? ? C C15 0.3881(7) -0.2190(6) 1.1873(5) 2.9(2) Biso ? ? C O5 0.5126(5) -0.1976(4) 1.1896(3) 2.8(1) Biso ? ? O N1 0.1762(6) -0.1639(6) 1.1951(4) 3.9(2) Biso ? ? N O6 0.0961(7) -0.162(1) 1.2453(5) 11.4(4) Biso ? ? O O7 0.1576(6) -0.1778(6) 1.1379(4) 6.5(2) Biso ? ? O C16 0.3235(7) -0.0320(6) 1.1378(5) 3.1(2) Biso ? ? C O8 0.4457(5) 0.0047(4) 1.1359(3) 2.6(1) Biso ? ? O O9 0.6322(5) -0.0586(4) 1.2125(3) 2.7(1) Biso ? ? O C17 0.7510(8) -0.0205(7) 1.2115(5) 3.7(2) Biso ? ? C C18 0.8274(7) -0.0025(7) 1.1314(5) 3.4(2) Biso ? ? C C19 0.7770(7) 0.0786(6) 1.0628(5) 3.3(2) Biso ? ? C O10 0.6553(5) 0.0539(4) 1.0568(3) 2.5(1) Biso ? ? O N2 0.9499(7) 0.0400(6) 1.1356(4) 4.2(2) Biso ? ? N O11 1.0322(6) 0.0391(6) 1.0866(4) 6.2(2) Biso ? ? O O12 0.9570(7) 0.0735(7) 1.1865(5) 9.9(2) Biso ? ? O C20 0.8583(8) -0.1011(7) 1.1128(6) 3.8(2) Biso ? ? C O13 0.7486(5) -0.1346(4) 1.0977(3) 3.1(1) Biso ? ? O O14 0.4745(6) -0.3107(5) 1.3485(4) 4.7(2) Biso ? ? O C21 0.460(1) -0.400(1) 1.4119(7) 7.6(4) Biso ? ? C C22 0.369(2) -0.468(1) 1.401(1) 11.5(6) Biso ? ? C C23 0.428(2) -0.516(2) 1.344(1) 12.3(7) Biso ? ? C C24 0.346(2) -0.598(1) 1.335(1) 11.0(5) Biso ? ? C O15 0.6253(6) -0.1734(5) 1.3753(3) 4.4(2) Biso ? ? O C25 0.6942(9) -0.227(1) 1.4370(6) 5.7(3) Biso ? ? C C26 0.828(1) -0.197(1) 1.4115(7) 7.5(4) Biso ? ? C C27 0.901(1) -0.259(2) 1.4775(9) 12.0(7) Biso ? ? C C28 1.037(2) -0.226(2) 1.453(1) 17(1) Biso ? ? C O16 0.7095(6) -0.2701(5) 1.2734(4) 4.4(2) Biso ? ? O C29 0.745(1) -0.3484(8) 1.2427(6) 5.2(3) Biso ? ? C C30 0.866(2) -0.398(1) 1.2741(9) 10.7(5) Biso ? ? C C31 0.842(2) -0.454(2) 1.353(1) 13.7(7)* Biso ? ? C C32 0.977(3) -0.493(2) 1.382(2) 18(1)* Biso ? ? C O17 0.5336(5) -0.1071(4) 1.0295(3) 2.6(1) Biso ? ? O O18 0.4070(5) -0.2647(4) 1.0078(3) 3.6(1) Biso ? ? O C33 0.449(1) -0.3663(8) 1.0464(8) 5.9(3) Biso ? ? C C34 0.351(1) -0.4402(9) 1.0694(8) 6.9(4) Biso ? ? C C35 0.255(1) -0.427(1) 1.1330(8) 7.4(4) Biso ? ? C C36 0.159(1) -0.513(1) 1.158(1) 9.4(5) Biso ? ? C O19 0.6389(6) -0.2114(5) 0.9357(4) 4.0(2) Biso ? ? O C37 0.7659(9) -0.2211(9) 0.9428(8) 5.9(3) Biso ? ? C C38 0.790(1) -0.3266(9) 0.9958(8) 11.6(6) Biso ? ? C C39 0.9046 -0.3407 1.0193 22(1)* Biso ? ? C C40 1.0208 -0.2961 1.0054 19(1)* Biso ? ? C loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol TI1 0.0370(8) 0.0510(8) 0.0393(7) 0.0066(7) 0.0056(6) 0.0200(6) Ti TI2 0.0262(6) 0.0344(7) 0.0315(6) 0.0020(6) 0.0099(5) 0.0078(5) Ti TI3 0.0378(8) 0.0525(9) 0.0343(7) 0.0045(7) 0.0125(6) 0.0054(7) Ti TI4 0.0354(7) 0.0326(7) 0.0407(7) 0.0045(6) 0.0116(6) 0.0129(5) Ti O1 0.050(3) 0.041(3) 0.053(3) 0.003(3) 0.015(3) 0.022(2) O C1 0.066(6) 0.061(5) 0.073(5) 0.010(5) 0.015(5) 0.038(4) C C2 0.083(8) 0.080(6) 0.122(8) 0.026(5) 0.007(6) 0.060(5) C C3 0.097(9) 0.135(7) 0.208(9) 0.049(6) 0.000(7) 0.128(5) C O2 0.063(4) 0.076(4) 0.050(3) 0.013(3) 0.009(3) 0.029(3) O C5 0.15(1) 0.13(1) 0.084(6) 0.001(8) 0.059(6) 0.058(5) C C6 0.12(1) 0.140(8) 0.095(6) 0.001(7) 0.033(6) 0.087(4) C C7 0.15(1) 0.200(9) 0.155(7) 0.036(8) 0.025(7) 0.142(5) C C8 0.10(1) 0.34(2) 0.21(1) 0.01(1) 0.036(9) 0.188(9) C O3 0.052(4) 0.063(4) 0.067(4) 0.002(3) 0.000(3) 0.033(3) O O4 0.033(3) 0.056(3) 0.038(3) 0.007(3) 0.006(2) 0.013(2) O C13 0.029(4) 0.074(6) 0.041(4) 0.014(4) 0.004(3) 0.018(4) C C14 0.024(4) 0.048(5) 0.044(4) 0.011(3) 0.011(3) 0.008(3) C C15 0.026(4) 0.042(4) 0.045(4) 0.007(3) 0.009(3) 0.013(3) C O5 0.030(3) 0.037(3) 0.036(3) 0.002(2) 0.012(2) 0.006(2) O N1 0.025(3) 0.071(5) 0.046(4) 0.018(3) 0.004(3) 0.008(3) N O6 0.056(4) 0.30(1) 0.074(5) 0.073(5) 0.003(4) 0.058(6) O O7 0.048(4) 0.126(5) 0.089(4) 0.022(4) 0.017(3) 0.052(3) O C16 0.023(4) 0.043(4) 0.051(4) 0.007(3) 0.014(3) 0.008(4) C O8 0.026(3) 0.038(3) 0.035(3) 0.005(2) 0.006(2) 0.011(2) O O9 0.025(3) 0.048(3) 0.030(2) 0.005(2) 0.007(2) 0.011(2) O C17 0.033(4) 0.065(5) 0.046(4) 0.019(4) 0.012(3) 0.016(4) C C18 0.027(4) 0.060(5) 0.045(4) 0.010(4) 0.015(3) 0.013(4) C C19 0.035(4) 0.040(4) 0.047(4) 0.012(3) 0.023(3) 0.000(3) C O10 0.025(3) 0.033(3) 0.037(3) 0.004(2) 0.008(2) 0.009(2) O N2 0.036(4) 0.075(5) 0.048(4) 0.017(3) 0.016(3) 0.013(3) N O11 0.042(4) 0.117(5) 0.080(4) 0.033(4) 0.009(3) 0.040(4) O O12 0.057(4) 0.253(7) 0.114(4) 0.069(4) 0.010(3) 0.119(4) O C20 0.029(4) 0.054(5) 0.069(5) 0.001(4) 0.019(4) 0.023(4) C O13 0.027(3) 0.049(3) 0.041(3) 0.000(2) 0.011(2) 0.013(2) O O14 0.059(4) 0.055(4) 0.053(4) 0.011(3) 0.020(3) 0.006(3) O C21 0.13(1) 0.089(8) 0.060(7) 0.049(7) 0.020(7) 0.004(6) C C22 0.22(2) 0.09(1) 0.10(1) 0.07(1) 0.02(1) 0.017(9) C C23 0.17(2) 0.16(1) 0.15(1) 0.02(1) 0.05(1) 0.05(1) C C24 0.17(1) 0.11(1) 0.14(1) 0.074(8) 0.043(9) 0.012(9) C O15 0.046(3) 0.084(4) 0.036(3) 0.000(3) 0.013(3) 0.014(3) O C25 0.054(5) 0.104(9) 0.052(5) 0.007(6) 0.029(4) 0.006(5) C C26 0.058(6) 0.15(1) 0.065(7) 0.004(7) 0.031(5) 0.003(7) C C27 0.069(8) 0.28(2) 0.087(9) 0.01(1) 0.036(7) 0.02(1) C C28 0.071(9) 0.40(3) 0.12(1) 0.06(1) 0.024(9) 0.02(2) C O16 0.051(3) 0.061(4) 0.055(3) 0.009(3) 0.026(3) 0.012(3) O C29 0.067(6) 0.068(6) 0.068(6) 0.031(5) 0.029(5) 0.029(4) C C30 0.17(1) 0.13(1) 0.10(1) 0.096(9) 0.04(1) 0.040(8) C O17 0.032(3) 0.032(3) 0.036(2) 0.003(2) 0.013(2) 0.008(2) O O18 0.045(3) 0.043(3) 0.053(3) 0.008(3) 0.008(3) 0.018(2) O C33 0.077(7) 0.034(5) 0.098(8) 0.011(5) 0.001(7) 0.007(5) C C34 0.085(9) 0.064(7) 0.105(9) 0.013(7) 0.007(8) 0.024(6) C C35 0.077(8) 0.095(9) 0.104(9) 0.019(7) 0.011(8) 0.032(7) C C36 0.10(1) 0.10(1) 0.14(1) 0.040(8) 0.00(1) 0.026(9) C O19 0.044(3) 0.048(3) 0.068(3) 0.005(3) 0.015(3) 0.027(2) O C37 0.039(5) 0.059(7) 0.111(9) 0.014(5) 0.009(6) 0.008(6) C C38 0.062(7) 0.09(1) 0.26(2) 0.008(8) 0.071(9) 0.00(1) C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag TI1 O1 1.984(6) . . ? TI4 O17 1.896(5) . . ? TI1 O2 1.753(6) . . ? TI4 O18 1.804(6) . . ? TI1 O3 1.768(6) . . ? TI4 O19 1.778(6) . . ? TI1 O4 1.983(6) . . ? O1 C1 1.48(1) . . ? TI1 O8 2.170(5) . . ? C1 C2 1.52(1) . . ? TI1 O9 2.171(5) . . ? C2 C3 1.64(2) . . ? TI2 O5 1.962(5) . . ? C3 C4 1.41(3) . . ? TI2 O8 2.140(5) . . ? O2 C5 1.42(1) . . ? TI2 O9 2.231(5) . . ? C5 C6 1.45(2) . . ? TI2 O10 1.987(5) . . ? C6 C7 1.56(2) . . ? TI2 O13 1.803(5) . . ? C7 C8 1.37(2) . . ? TI2 O17 1.748(5) . . ? O3 C9 1.419(6) . . ? TI3 O4 2.098(6) . . ? C9 C10 1.529(0) . . ? TI3 O5 2.145(5) . . ? C9 C11 2.124(0) . . ? TI3 O9 2.200(5) . . ? C10 C11 1.617(0) . . ? TI3 O14 1.806(6) . . ? C11 C12 1.454(0) . . ? TI3 O15 1.814(6) . . ? O4 C13 1.431(8) . . ? TI3 O16 1.799(6) . . ? C13 C14 1.55(1) . . ? TI4 O1 2.052(5) . . ? C14 C15 1.53(1) . . ? TI4 O8 2.249(5) . . ? C14 N1 1.526(9) . . ? TI4 O10 2.090(5) . . ? C14 C16 1.53(1) . . ? C15 O5 1.438(8) . . ? C23 C24 1.58(2) . . ? N1 O6 1.19(1) . . ? O15 C25 1.43(1) . . ? N1 O7 1.179(9) . . ? C25 C26 1.53(1) . . ? O6 O7 2.07(1) . . ? C26 C27 1.54(2) . . ? C16 O8 1.470(8) . . ? C27 C28 1.55(2) . . ? O9 C17 1.446(8) . . ? O16 C29 1.41(1) . . ? C17 C18 1.53(1) . . ? C29 C30 1.57(2) . . ? C18 C19 1.54(1) . . ? C30 C31 1.40(2) . . ? C18 N2 1.538(9) . . ? C31 C32 1.66(3) . . ? C18 C20 1.55(1) . . ? O18 C33 1.45(1) . . ? C19 O10 1.440(8) . . ? C33 C34 1.47(1) . . ? N2 O11 1.185(9) . . ? C34 C35 1.51(2) . . ? N2 O12 1.19(1) . . ? C35 C36 1.58(2) . . ? O11 O12 2.09(1) . . ? O19 C37 1.42(1) . . ? C20 O13 1.426(8) . . ? C37 C38 1.51(1) . . ? O14 C21 1.40(1) . . ? C38 C39 1.38(1) . . ? C21 C22 1.52(2) . . ? C39 C40 1.418(0) . . ? C22 C23 1.48(2) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 TI1 O2 96.7(3) . . . ? O8 TI2 O10 76.2(2) . . . ? O1 TI1 O3 96.5(3) . . . ? O8 TI2 O13 157.4(2) . . . ? O1 TI1 O4 158.0(2) . . . ? O8 TI2 O17 97.1(2) . . . ? O1 TI1 O8 76.9(2) . . . ? O9 TI2 O10 81.2(2) . . . ? O1 TI1 O9 89.5(2) . . . ? O9 TI2 O13 86.9(2) . . . ? O2 TI1 O3 101.2(3) . . . ? O9 TI2 O17 168.4(2) . . . ? O2 TI1 O4 100.4(3) . . . ? O10 TI2 O13 90.4(2) . . . ? O2 TI1 O8 164.8(3) . . . ? O10 TI2 O17 103.2(2) . . . ? O2 TI1 O9 92.5(3) . . . ? O13 TI2 O17 103.7(2) . . . ? O3 TI1 O4 93.7(2) . . . ? O4 TI3 O5 78.3(2) . . . ? O3 TI1 O8 93.2(2) . . . ? O4 TI3 O9 73.2(2) . . . ? O3 TI1 O9 164.2(2) . . . ? O4 TI3 O14 90.5(3) . . . ? O4 TI1 O8 83.1(2) . . . ? O4 TI3 O15 92.7(2) . . . ? O4 TI1 O9 76.0(2) . . . ? O4 TI3 O16 164.3(2) . . . ? O8 TI1 O9 73.8(2) . . . ? O5 TI3 O9 73.9(2) . . . ? O5 TI2 O8 85.2(2) . . . ? O5 TI3 O14 89.9(2) . . . ? O5 TI2 O9 76.8(2) . . . ? O5 TI3 O15 164.1(3) . . . ? O5 TI2 O10 154.5(2) . . . ? O5 TI3 O16 89.7(2) . . . ? O5 TI2 O13 101.0(2) . . . ? O9 TI3 O14 158.8(2) . . . ? O5 TI2 O17 96.3(2) . . . ? O9 TI3 O15 91.0(2) . . . ? O8 TI2 O9 73.2(2) . . . ? O9 TI3 O16 93.9(2) . . . ? O14 TI3 O15 103.4(3) . . . ? O2 C5 C6 114.(1) . . . ? O14 TI3 O16 99.7(3) . . . ? C5 C6 C7 112.(1) . . . ? O15 TI3 O16 96.5(3) . . . ? C6 C7 C8 113.(2) . . . ? O1 TI4 O8 73.8(2) . . . ? O3 C9 C10 120.5(2) . . . ? O1 TI4 O10 81.3(2) . . . ? O3 C9 C11 148.7(2) . . . ? O1 TI4 O17 159.9(2) . . . ? C10 C9 C11 49.(0) . . . ? O1 TI4 O18 95.1(2) . . . ? C9 C10 C11 84.(0) . . . ? O1 TI4 O19 92.8(3) . . . ? C9 C11 C10 45.(0) . . . ? O8 TI4 O10 71.9(2) . . . ? C9 C11 C12 159.(0) . . . ? O8 TI4 O17 87.5(2) . . . ? C10 C11 C12 113.(0) . . . ? O8 TI4 O18 164.1(2) . . . ? O4 C13 C14 108.1(6) . . . ? O8 TI4 O19 92.5(2) . . . ? C13 C14 C15 111.6(6) . . . ? O10 TI4 O17 86.0(2) . . . ? C13 C14 N1 107.1(6) . . . ? O10 TI4 O18 95.5(2) . . . ? C13 C14 C16 113.5(7) . . . ? O10 TI4 O19 164.3(2) . . . ? C15 C14 N1 105.0(6) . . . ? O17 TI4 O18 101.6(2) . . . ? C15 C14 C16 114.8(6) . . . ? O17 TI4 O19 95.3(2) . . . ? N1 C14 C16 103.9(6) . . . ? O18 TI4 O19 99.6(3) . . . ? C14 C15 O5 109.6(6) . . . ? O1 C1 C2 107.5(8) . . . ? C14 N1 O6 117.9(8) . . . ? C1 C2 C3 105.9(9) . . . ? C14 N1 O7 119.5(7) . . . ? C2 C3 C4 106.(2) . . . ? O6 N1 O7 122.1(8) . . . ? N1 O6 O7 28.8(4) . . . ? C18 C20 O13 107.6(6) . . . ? N1 O7 O6 29.1(4) . . . ? O14 C21 C22 111(1) . . . ? C14 C16 O8 109.9(6) . . . ? C21 C22 C23 109.(2) . . . ? O9 C17 C18 110.4(6) . . . ? C22 C23 C24 113.(2) . . . ? C17 C18 C19 115.5(7) . . . ? O15 C25 C26 108.7(8) . . . ? C17 C18 N2 106.4(6) . . . ? C25 C26 C27 108(1) . . . ? C17 C18 C20 112.4(7) . . . ? C26 C27 C28 108.(1) . . . ? C19 C18 N2 103.9(6) . . . ? O16 C29 C30 108.3(9) . . . ? C19 C18 C20 111.1(7) . . . ? C29 C30 C31 110.(2) . . . ? N2 C18 C20 106.5(6) . . . ? C30 C31 C32 106.(2) . . . ? C18 C19 O10 110.2(6) . . . ? O18 C33 C34 112.6(9) . . . ? C18 N2 O11 117.4(7) . . . ? C33 C34 C35 113.(1) . . . ? C18 N2 O12 119.1(8) . . . ? C34 C35 C36 110.(1) . . . ? O11 N2 O12 123.5(8) . . . ? O19 C37 C38 108.0(8) . . . ? N2 O11 O12 28.4(4) . . . ? C37 C38 C39 114.0(9) . . . ? N2 O12 O11 28.2(4) . . . ? C38 C39 C40 143.3(5) . . . ? #======END