# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email tshuva@chem.ch.huji.ac.il _publ_contact_author_name 'Edit Tshuva' loop_ _publ_author_name 'Sigalit Meker' 'Cesar Manna' 'Dani Peri' 'Edit Tshuva' data_L3Ti(OiPr)2 _database_code_depnum_ccdc_archive 'CCDC 829875' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H40 N2 O4 Ti' _chemical_formula_sum 'C26 H40 N2 O4 Ti' _chemical_formula_weight 492.50 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 Trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 19.5096(9) _cell_length_b 19.5096(9) _cell_length_c 12.4020(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4088.1(5) _cell_formula_units_Z 6 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description shapeless _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.200 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 0.345 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42199 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0219 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5370 _reflns_number_gt 5075 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1065P)^2^+6.8097P] 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 5370 _refine_ls_number_parameters 314 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1013 _refine_ls_R_factor_gt 0.0973 _refine_ls_wR_factor_ref 0.2456 _refine_ls_wR_factor_gt 0.2425 _refine_ls_goodness_of_fit_ref 1.246 _refine_ls_restrained_S_all 1.246 _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 C1 C 0.2540(2) 0.0556(2) 0.4453(3) 0.0284(8) Uani 1 1 d . . . C2 C 0.1986(2) 0.0798(2) 0.4245(3) 0.0272(7) Uani 1 1 d . . . H2 H 0.1802 0.0977 0.4831 0.033 Uiso 1 1 calc R . . C3 C 0.1694(2) 0.0786(2) 0.3221(3) 0.0290(8) Uani 1 1 d . . . C4 C 0.1957(2) 0.0522(2) 0.2353(3) 0.0334(8) Uani 1 1 d . . . C5 C 0.2504(2) 0.0276(2) 0.2558(3) 0.0368(9) Uani 1 1 d . . . H5 H 0.2679 0.0089 0.1971 0.044 Uiso 1 1 calc R . . C6 C 0.2806(2) 0.0289(2) 0.3579(3) 0.0327(8) Uani 1 1 d . . . C7 C 0.3424(3) 0.0044(3) 0.3704(3) 0.0434(10) Uani 1 1 d . . . H7A H 0.3362 -0.0324 0.3113 0.052 Uiso 1 1 calc R . . H7B H 0.3956 0.0518 0.3637 0.052 Uiso 1 1 calc R . . C8 C 0.2640(3) -0.1117(3) 0.4866(4) 0.0437(10) Uani 1 1 d . . . H8A H 0.2666 -0.1511 0.4391 0.052 Uiso 1 1 calc R . . H8B H 0.2175 -0.1073 0.4653 0.052 Uiso 1 1 calc R . . C9 C 0.2561(3) -0.1379(3) 0.6019(4) 0.0463(11) Uani 1 1 d . . . H9A H 0.2048 -0.1872 0.6125 0.056 Uiso 1 1 calc R . . H9B H 0.2991 -0.1488 0.6205 0.056 Uiso 1 1 calc R . . C10 C 0.2634(3) -0.0920(3) 0.7874(4) 0.0506(12) Uani 1 1 d . . . H10A H 0.2190 -0.1454 0.8047 0.061 Uiso 1 1 calc R . . H10B H 0.2566 -0.0531 0.8305 0.061 Uiso 1 1 calc R . . C11 C 0.3408(3) -0.0875(4) 0.8191(4) 0.0556(13) Uani 1 1 d . . . C12 C 0.3415(3) -0.1289(4) 0.9106(4) 0.0725(19) Uani 1 1 d . . . H12 H 0.2928 -0.1613 0.9468 0.087 Uiso 1 1 calc R . . C13 C 0.4093(4) -0.1252(5) 0.9514(5) 0.085(2) Uani 1 1 d . . . C14 C 0.4806(4) -0.0781(5) 0.8971(5) 0.081(2) Uani 1 1 d . . . C15 C 0.4812(3) -0.0376(4) 0.8049(4) 0.0643(16) Uani 1 1 d . . . H15 H 0.5299 -0.0062 0.7681 0.077 Uiso 1 1 calc R . . C16 C 0.4120(3) -0.0414(4) 0.7641(4) 0.0530(13) Uani 1 1 d . . . C17 C 0.1110(2) 0.1071(2) 0.3069(4) 0.0404(10) Uani 1 1 d . . . H17A H 0.0778 0.0945 0.3714 0.061 Uiso 1 1 calc R . . H17B H 0.0776 0.0808 0.2441 0.061 Uiso 1 1 calc R . . H17C H 0.1397 0.1644 0.2955 0.061 Uiso 1 1 calc R . . C18 C 0.1663(3) 0.0492(3) 0.1217(3) 0.0479(11) Uani 1 1 d . . . H18A H 0.1912 0.0284 0.0731 0.072 Uiso 1 1 calc R . . H18B H 0.1800 0.1027 0.0988 0.072 Uiso 1 1 calc R . . H18C H 0.1087 0.0147 0.1197 0.072 Uiso 1 1 calc R . . C19 C 0.4062(5) -0.1713(7) 1.0504(6) 0.120(4) Uani 1 1 d . . . H19A H 0.3526 -0.1975 1.0803 0.180 Uiso 1 1 calc R . . H19B H 0.4435 -0.1352 1.1043 0.180 Uiso 1 1 calc R . . H19C H 0.4206 -0.2112 1.0311 0.180 Uiso 1 1 calc R . . C20 C 0.5573(4) -0.0707(6) 0.9380(5) 0.105(3) Uani 1 1 d . . . H20A H 0.5577 -0.1199 0.9232 0.158 Uiso 1 1 calc R . . H20B H 0.5617 -0.0609 1.0158 0.158 Uiso 1 1 calc R . . H20C H 0.6022 -0.0266 0.9013 0.158 Uiso 1 1 calc R . . C21 C 0.5253(4) 0.1427(5) 0.5301(7) 0.095(2) Uani 1 1 d . . . H21 H 0.5252 0.0920 0.5176 0.114 Uiso 1 1 calc R . . C22 C 0.5546(5) 0.1911(6) 0.4314(8) 0.125(3) Uani 1 1 d . . . H22A H 0.5180 0.1636 0.3717 0.187 Uiso 1 1 calc R . . H22B H 0.6071 0.1994 0.4134 0.187 Uiso 1 1 calc R . . H22C H 0.5580 0.2424 0.4434 0.187 Uiso 1 1 calc R . . C23 C 0.5710(4) 0.1796(7) 0.6306(9) 0.151(5) Uani 1 1 d . . . H23A H 0.5621 0.2227 0.6531 0.227 Uiso 1 1 calc R . . H23B H 0.6275 0.2007 0.6169 0.227 Uiso 1 1 calc R . . H23C H 0.5533 0.1397 0.6878 0.227 Uiso 1 1 calc R . . C24 C 0.3400(3) 0.1484(3) 0.7886(4) 0.0565(13) Uani 1 1 d . . . H24 H 0.3096 0.1622 0.7365 0.068 Uiso 1 1 calc R . . C25 C 0.2941(4) 0.1212(4) 0.8923(4) 0.0728(17) Uani 1 1 d . . . H25A H 0.2419 0.0751 0.8782 0.109 Uiso 1 1 calc R . . H25B H 0.2876 0.1641 0.9224 0.109 Uiso 1 1 calc R . . H25C H 0.3228 0.1068 0.9438 0.109 Uiso 1 1 calc R . . C26 C 0.4201(4) 0.2198(4) 0.8045(5) 0.0812(19) Uani 1 1 d . . . H26A H 0.4497 0.2079 0.8579 0.122 Uiso 1 1 calc R . . H26B H 0.4141 0.2640 0.8300 0.122 Uiso 1 1 calc R . . H26C H 0.4489 0.2341 0.7359 0.122 Uiso 1 1 calc R . . N1 N 0.3368(2) -0.0345(2) 0.4752(3) 0.0408(9) Uani 1 1 d . . . H1N H 0.372(3) -0.041(3) 0.480(4) 0.035(12) Uiso 1 1 d . . . N2 N 0.2604(2) -0.0759(2) 0.6711(3) 0.0415(9) Uani 1 1 d . . . H2N H 0.227(3) -0.070(3) 0.665(4) 0.031(12) Uiso 1 1 d . . . O1 O 0.28003(15) 0.06001(17) 0.5459(2) 0.0337(6) Uani 1 1 d . . . O2 O 0.41827(17) -0.0008(2) 0.6741(2) 0.0468(8) Uani 1 1 d . . . O3 O 0.44440(17) 0.1238(2) 0.5507(3) 0.0500(8) Uani 1 1 d . . . O4 O 0.34752(18) 0.0863(2) 0.7451(2) 0.0478(8) Uani 1 1 d . . . Ti1 Ti 0.35823(4) 0.04510(5) 0.62015(6) 0.0364(3) Uani 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 C1 0.0205(16) 0.0269(18) 0.0325(19) 0.0034(14) 0.0005(14) 0.0078(14) C2 0.0210(16) 0.0226(16) 0.0338(19) 0.0008(14) 0.0001(14) 0.0076(14) C3 0.0208(17) 0.0195(16) 0.037(2) 0.0037(14) -0.0029(14) 0.0031(13) C4 0.0278(18) 0.0286(19) 0.033(2) 0.0070(15) -0.0007(15) 0.0061(15) C5 0.033(2) 0.042(2) 0.031(2) 0.0023(16) 0.0079(16) 0.0149(18) C6 0.0251(18) 0.039(2) 0.0324(19) 0.0032(16) 0.0039(14) 0.0151(16) C7 0.035(2) 0.065(3) 0.038(2) -0.001(2) 0.0051(17) 0.031(2) C8 0.038(2) 0.048(2) 0.054(3) -0.008(2) -0.0079(19) 0.028(2) C9 0.036(2) 0.050(3) 0.063(3) 0.005(2) -0.007(2) 0.029(2) C10 0.033(2) 0.077(3) 0.052(3) 0.015(2) 0.0055(19) 0.035(2) C11 0.039(2) 0.097(4) 0.043(3) 0.013(3) 0.0031(19) 0.044(3) C12 0.054(3) 0.132(6) 0.052(3) 0.034(3) 0.014(2) 0.062(4) C13 0.069(4) 0.160(7) 0.052(3) 0.040(4) 0.010(3) 0.078(4) C14 0.061(3) 0.162(7) 0.052(3) 0.023(4) 0.002(3) 0.078(4) C15 0.042(3) 0.126(5) 0.045(3) 0.015(3) 0.005(2) 0.057(3) C16 0.041(2) 0.094(4) 0.041(2) 0.006(2) 0.0011(19) 0.046(3) C17 0.036(2) 0.031(2) 0.051(2) -0.0003(17) -0.0137(18) 0.0138(17) C18 0.051(3) 0.054(3) 0.034(2) 0.0041(19) -0.0040(19) 0.024(2) C19 0.097(6) 0.218(11) 0.082(5) 0.068(6) 0.016(4) 0.107(7) C20 0.066(4) 0.214(9) 0.066(4) 0.038(5) 0.001(3) 0.093(6) C21 0.041(3) 0.092(5) 0.125(6) 0.036(5) 0.001(3) 0.014(3) C22 0.061(4) 0.137(8) 0.141(8) -0.009(6) 0.035(5) 0.024(5) C23 0.041(4) 0.192(11) 0.165(9) 0.058(8) -0.034(5) 0.017(5) C24 0.058(3) 0.078(4) 0.041(3) -0.005(2) -0.013(2) 0.040(3) C25 0.075(4) 0.114(5) 0.044(3) -0.005(3) 0.000(3) 0.058(4) C26 0.090(5) 0.075(4) 0.069(4) -0.010(3) -0.025(3) 0.034(4) N1 0.0300(18) 0.058(2) 0.048(2) -0.0021(17) -0.0019(15) 0.0322(18) N2 0.0256(17) 0.057(2) 0.052(2) 0.0073(17) -0.0029(15) 0.0281(17) O1 0.0275(13) 0.0466(16) 0.0318(14) -0.0042(11) -0.0034(10) 0.0222(12) O2 0.0310(15) 0.074(2) 0.0442(17) 0.0118(15) -0.0003(12) 0.0329(15) O3 0.0287(15) 0.061(2) 0.0552(19) 0.0080(15) -0.0012(13) 0.0190(14) O4 0.0459(17) 0.066(2) 0.0387(16) -0.0103(14) -0.0102(13) 0.0335(16) Ti1 0.0253(4) 0.0533(5) 0.0344(4) 0.0001(3) -0.0043(3) 0.0225(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 C1 O1 1.333(4) . ? C1 C2 1.403(5) . ? C1 C6 1.408(5) . ? C2 C3 1.387(5) . ? C2 H2 0.9500 . ? C3 C4 1.396(6) . ? C3 C17 1.508(5) . ? C4 C5 1.395(6) . ? C4 C18 1.510(6) . ? C5 C6 1.392(6) . ? C5 H5 0.9500 . ? C6 C7 1.511(5) . ? C7 N1 1.482(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N1 1.472(6) . ? C8 C9 1.500(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 N2 1.451(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N2 1.485(6) . ? C10 C11 1.519(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.397(7) . ? C11 C16 1.398(7) . ? C12 C13 1.384(7) . ? C12 H12 0.9500 . ? C13 C14 1.399(9) . ? C13 C19 1.505(8) . ? C14 C15 1.386(8) . ? C14 C20 1.517(7) . ? C15 C16 1.409(6) . ? C15 H15 0.9500 . ? C16 O2 1.338(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 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 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 O3 1.453(7) . ? C21 C22 1.476(12) . ? C21 C23 1.491(12) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 O4 1.398(6) . ? C24 C26 1.498(8) . ? C24 C25 1.505(8) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? N1 Ti1 2.273(4) . ? N1 H1N 0.75(5) . ? N2 Ti1 2.260(4) . ? N2 H2N 0.71(5) . ? O1 Ti1 1.925(3) . ? O2 Ti1 1.917(3) . ? O3 Ti1 1.829(3) . ? O4 Ti1 1.806(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 118.9(3) . . ? O1 C1 C6 123.0(3) . . ? C2 C1 C6 118.1(3) . . ? C3 C2 C1 122.7(3) . . ? C3 C2 H2 118.6 . . ? C1 C2 H2 118.6 . . ? C2 C3 C4 119.3(3) . . ? C2 C3 C17 119.1(4) . . ? C4 C3 C17 121.6(3) . . ? C5 C4 C3 118.1(3) . . ? C5 C4 C18 119.8(4) . . ? C3 C4 C18 122.1(4) . . ? C6 C5 C4 123.3(4) . . ? C6 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? C5 C6 C1 118.5(3) . . ? C5 C6 C7 119.0(3) . . ? C1 C6 C7 122.5(3) . . ? N1 C7 C6 112.7(3) . . ? N1 C7 H7A 109.1 . . ? C6 C7 H7A 109.1 . . ? N1 C7 H7B 109.1 . . ? C6 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? N1 C8 C9 108.8(4) . . ? N1 C8 H8A 109.9 . . ? C9 C8 H8A 109.9 . . ? N1 C8 H8B 109.9 . . ? C9 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? N2 C9 C8 109.1(4) . . ? N2 C9 H9A 109.9 . . ? C8 C9 H9A 109.9 . . ? N2 C9 H9B 109.9 . . ? C8 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? N2 C10 C11 112.6(4) . . ? N2 C10 H10A 109.1 . . ? C11 C10 H10A 109.1 . . ? N2 C10 H10B 109.1 . . ? C11 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? C12 C11 C16 118.4(4) . . ? C12 C11 C10 118.2(4) . . ? C16 C11 C10 123.3(4) . . ? C13 C12 C11 123.5(5) . . ? C13 C12 H12 118.2 . . ? C11 C12 H12 118.2 . . ? C12 C13 C14 117.9(5) . . ? C12 C13 C19 121.1(6) . . ? C14 C13 C19 121.0(5) . . ? C15 C14 C13 119.6(5) . . ? C15 C14 C20 119.7(6) . . ? C13 C14 C20 120.7(5) . . ? C14 C15 C16 122.1(5) . . ? C14 C15 H15 118.9 . . ? C16 C15 H15 118.9 . . ? O2 C16 C11 123.7(4) . . ? O2 C16 C15 117.8(4) . . ? C11 C16 C15 118.4(4) . . ? C3 C17 H17A 109.5 . . ? C3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C4 C18 H18A 109.5 . . ? C4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C13 C19 H19A 109.5 . . ? C13 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C13 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C14 C20 H20A 109.5 . . ? C14 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C14 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O3 C21 C22 109.4(6) . . ? O3 C21 C23 106.7(7) . . ? C22 C21 C23 116.0(7) . . ? O3 C21 H21 108.2 . . ? C22 C21 H21 108.2 . . ? C23 C21 H21 108.2 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O4 C24 C26 110.1(5) . . ? O4 C24 C25 109.0(5) . . ? C26 C24 C25 112.1(5) . . ? O4 C24 H24 108.5 . . ? C26 C24 H24 108.5 . . ? C25 C24 H24 108.5 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C8 N1 C7 113.3(3) . . ? C8 N1 Ti1 112.2(3) . . ? C7 N1 Ti1 113.8(3) . . ? C8 N1 H1N 108(4) . . ? C7 N1 H1N 108(3) . . ? Ti1 N1 H1N 100(3) . . ? C9 N2 C10 112.9(4) . . ? C9 N2 Ti1 111.8(3) . . ? C10 N2 Ti1 113.0(3) . . ? C9 N2 H2N 113(4) . . ? C10 N2 H2N 106(4) . . ? Ti1 N2 H2N 99(4) . . ? C1 O1 Ti1 138.0(2) . . ? C16 O2 Ti1 132.2(3) . . ? C21 O3 Ti1 136.2(4) . . ? C24 O4 Ti1 143.3(3) . . ? O4 Ti1 O3 107.02(16) . . ? O4 Ti1 O2 98.18(14) . . ? O3 Ti1 O2 92.13(14) . . ? O4 Ti1 O1 93.80(12) . . ? O3 Ti1 O1 96.49(13) . . ? O2 Ti1 O1 162.52(14) . . ? O4 Ti1 N2 89.99(15) . . ? O3 Ti1 N2 161.87(16) . . ? O2 Ti1 N2 78.97(13) . . ? O1 Ti1 N2 88.38(13) . . ? O4 Ti1 N1 163.77(15) . . ? O3 Ti1 N1 88.80(15) . . ? O2 Ti1 N1 84.48(14) . . ? O1 Ti1 N1 80.53(12) . . ? N2 Ti1 N1 74.74(14) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.126 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.107 #===END data_L22Ti2(m-O)2 _database_code_depnum_ccdc_archive 'CCDC 829876' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H56 N4 O6 Ti2, C4 H8 O' _chemical_formula_sum 'C46 H64 N4 O7 Ti2' _chemical_formula_weight 880.81 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.9826(10) _cell_length_b 12.7055(18) _cell_length_c 14.613(2) _cell_angle_alpha 66.685(2) _cell_angle_beta 84.776(3) _cell_angle_gamma 83.530(3) _cell_volume 1181.4(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description shapeless _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 468 _exptl_absorpt_coefficient_mu 0.389 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13613 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 28.01 _reflns_number_total 5470 _reflns_number_gt 5301 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0824P)^2^+0.9986P] 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 5470 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1556 _refine_ls_wR_factor_gt 0.1548 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.156 _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 C1 C 0.3420(3) 0.4324(2) 0.79853(16) 0.0250(4) Uani 1 1 d . . . C2 C 0.2991(3) 0.3604(2) 0.89816(17) 0.0298(5) Uani 1 1 d . . . H2 H 0.2948 0.2821 0.9148 0.036 Uiso 1 1 calc R . . C3 C 0.2628(3) 0.4037(2) 0.97285(17) 0.0336(5) Uani 1 1 d . . . C4 C 0.2672(3) 0.5218(2) 0.94849(19) 0.0346(5) Uani 1 1 d . . . C5 C 0.3096(3) 0.5925(2) 0.84946(18) 0.0312(5) Uani 1 1 d . . . H5 H 0.3129 0.6709 0.8329 0.037 Uiso 1 1 calc R . . C6 C 0.3473(3) 0.5504(2) 0.77415(17) 0.0267(4) Uani 1 1 d . . . C7 C 0.4010(3) 0.62881(19) 0.66902(17) 0.0268(4) Uani 1 1 d . . . H7A H 0.2935 0.6412 0.6273 0.032 Uiso 1 1 calc R . . H7B H 0.4267 0.7027 0.6680 0.032 Uiso 1 1 calc R . . C8 C 0.7489(3) 0.5588(2) 0.68538(17) 0.0284(5) Uani 1 1 d . . . H8A H 0.7136 0.5268 0.7562 0.034 Uiso 1 1 calc R . . H8B H 0.8039 0.6311 0.6698 0.034 Uiso 1 1 calc R . . C9 C 0.8965(3) 0.4766(2) 0.66026(19) 0.0311(5) Uani 1 1 d . . . H9A H 0.9438 0.5127 0.5914 0.037 Uiso 1 1 calc R . . H9B H 1.0050 0.4585 0.7024 0.037 Uiso 1 1 calc R . . C10 C 0.6740(3) 0.19182(19) 0.60796(17) 0.0283(5) Uani 1 1 d . . . C11 C 0.6236(4) 0.0916(2) 0.60359(18) 0.0319(5) Uani 1 1 d . . . H11 H 0.4975 0.0880 0.5900 0.038 Uiso 1 1 calc R . . C12 C 0.7548(4) -0.0038(2) 0.61871(19) 0.0359(5) Uani 1 1 d . . . C13 C 0.9449(4) 0.0005(2) 0.6389(2) 0.0416(6) Uani 1 1 d . . . C14 C 0.9973(4) 0.1022(2) 0.6405(2) 0.0378(6) Uani 1 1 d . . . H14 H 1.1245 0.1058 0.6526 0.045 Uiso 1 1 calc R . . C15 C 0.8675(3) 0.1995(2) 0.62480(18) 0.0309(5) Uani 1 1 d . . . C16 C 0.9401(3) 0.3093(2) 0.62040(18) 0.0310(5) Uani 1 1 d . . . H16A H 1.0663 0.2915 0.6483 0.037 Uiso 1 1 calc R . . H16B H 0.9551 0.3616 0.5511 0.037 Uiso 1 1 calc R . . C17 C 0.2227(4) 0.3225(3) 1.07929(19) 0.0450(7) Uani 1 1 d . . . H17A H 0.2131 0.2468 1.0814 0.068 Uiso 1 1 calc R . . H17B H 0.1036 0.3487 1.1049 0.068 Uiso 1 1 calc R . . H17C H 0.3259 0.3205 1.1192 0.068 Uiso 1 1 calc R . . C18 C 0.2354(4) 0.5726(3) 1.0270(2) 0.0435(6) Uani 1 1 d . . . H18A H 0.3428 0.5479 1.0693 0.065 Uiso 1 1 calc R . . H18B H 0.1191 0.5472 1.0663 0.065 Uiso 1 1 calc R . . H18C H 0.2241 0.6550 0.9950 0.065 Uiso 1 1 calc R . . C19 C 0.6918(5) -0.1113(3) 0.6146(3) 0.0540(8) Uani 1 1 d . . . H19A H 0.5574 -0.1000 0.6010 0.081 Uiso 1 1 calc R . . H19B H 0.7117 -0.1744 0.6775 0.081 Uiso 1 1 calc R . . H19C H 0.7661 -0.1282 0.5628 0.081 Uiso 1 1 calc R . . C20 C 1.0925(5) -0.1017(3) 0.6567(3) 0.0565(8) Uani 1 1 d . . . H20A H 1.2148 -0.0824 0.6679 0.085 Uiso 1 1 calc R . . H20B H 1.1050 -0.1215 0.5993 0.085 Uiso 1 1 calc R . . H20C H 1.0510 -0.1660 0.7141 0.085 Uiso 1 1 calc R . . C21 C 0.7987(4) 0.2932(2) 0.78241(17) 0.0343(5) Uani 1 1 d . . . H21A H 0.9259 0.2749 0.8074 0.051 Uiso 1 1 calc R . . H21B H 0.7441 0.2235 0.7913 0.051 Uiso 1 1 calc R . . H21C H 0.7189 0.3322 0.8182 0.051 Uiso 1 1 calc R . . N1 N 0.5744(3) 0.57952(16) 0.62782(14) 0.0235(4) Uani 1 1 d . . . H1N H 0.596(4) 0.630(3) 0.567(2) 0.033(7) Uiso 1 1 d . . . N2 N 0.8098(3) 0.36819(15) 0.67529(13) 0.0238(4) Uani 1 1 d . . . O1 O 0.3239(2) 0.49958(12) 0.51925(10) 0.0215(3) Uani 1 1 d . . . O2 O 0.3813(2) 0.38754(13) 0.72904(11) 0.0242(3) Uani 1 1 d . . . O3 O 0.5382(2) 0.28072(13) 0.59302(12) 0.0267(3) Uani 1 1 d . . . Ti1 Ti 0.51325(5) 0.42634(3) 0.60112(2) 0.01877(13) Uani 1 1 d . . . O4 O 0.3588(17) 0.8895(8) 0.8717(9) 0.147(4) Uani 0.50 1 d P . . C22 C 0.1902(19) 0.9187(9) 0.9160(10) 0.105(4) Uani 0.50 1 d P . . H22A H 0.1801 0.8693 0.9863 0.126 Uiso 0.50 1 calc PR . . H22B H 0.0791 0.9117 0.8841 0.126 Uiso 0.50 1 calc PR . . C23 C 0.2014(13) 1.0360(7) 0.9028(7) 0.074(2) Uani 0.50 1 d P . . H23A H 0.0987 1.0856 0.8624 0.089 Uiso 0.50 1 calc PR . . H23B H 0.1915 1.0432 0.9668 0.089 Uiso 0.50 1 calc PR . . C24 C 0.3838(12) 1.0650(6) 0.8541(6) 0.0629(18) Uani 0.50 1 d P . . H24A H 0.3698 1.1131 0.7841 0.075 Uiso 0.50 1 calc PR . . H24B H 0.4475 1.1065 0.8843 0.075 Uiso 0.50 1 calc PR . . C25 C 0.4882(17) 0.9635(9) 0.8649(6) 0.089(3) Uani 0.50 1 d P . . H25A H 0.5775 0.9736 0.8078 0.107 Uiso 0.50 1 calc PR . . H25B H 0.5610 0.9352 0.9246 0.107 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0196(9) 0.0339(11) 0.0223(10) -0.0122(8) -0.0016(7) -0.0006(8) C2 0.0255(11) 0.0371(12) 0.0248(11) -0.0100(9) -0.0011(8) -0.0030(9) C3 0.0233(10) 0.0523(15) 0.0238(11) -0.0140(10) -0.0010(8) -0.0002(10) C4 0.0229(11) 0.0550(15) 0.0320(12) -0.0248(11) -0.0039(9) 0.0033(10) C5 0.0263(11) 0.0392(12) 0.0333(12) -0.0207(10) -0.0047(9) 0.0035(9) C6 0.0234(10) 0.0327(11) 0.0256(10) -0.0134(9) -0.0033(8) 0.0013(8) C7 0.0286(11) 0.0251(10) 0.0282(11) -0.0129(8) -0.0039(8) 0.0026(8) C8 0.0261(10) 0.0311(11) 0.0306(11) -0.0134(9) -0.0041(8) -0.0056(8) C9 0.0250(11) 0.0348(12) 0.0354(12) -0.0145(10) -0.0035(9) -0.0049(9) C10 0.0328(11) 0.0252(10) 0.0262(10) -0.0100(8) -0.0038(8) 0.0026(8) C11 0.0334(12) 0.0280(11) 0.0356(12) -0.0141(9) 0.0002(9) -0.0023(9) C12 0.0441(14) 0.0253(11) 0.0375(13) -0.0130(10) 0.0020(11) 0.0002(10) C13 0.0471(15) 0.0311(12) 0.0449(15) -0.0160(11) -0.0059(12) 0.0104(11) C14 0.0335(12) 0.0370(13) 0.0407(14) -0.0145(11) -0.0038(10) 0.0056(10) C15 0.0307(11) 0.0304(11) 0.0291(11) -0.0100(9) -0.0011(9) 0.0009(9) C16 0.0236(10) 0.0338(12) 0.0326(12) -0.0111(9) -0.0005(9) 0.0020(9) C17 0.0403(14) 0.0655(19) 0.0250(12) -0.0145(12) 0.0018(10) -0.0018(13) C18 0.0337(13) 0.0707(19) 0.0368(14) -0.0342(14) -0.0030(10) 0.0044(12) C19 0.0618(19) 0.0326(14) 0.074(2) -0.0285(14) -0.0054(16) 0.0001(13) C20 0.0561(19) 0.0388(15) 0.074(2) -0.0257(15) -0.0103(16) 0.0181(13) C21 0.0353(12) 0.0371(13) 0.0252(11) -0.0062(9) -0.0064(9) -0.0006(10) N1 0.0248(9) 0.0237(9) 0.0210(8) -0.0077(7) -0.0021(7) -0.0014(7) N2 0.0231(8) 0.0251(9) 0.0223(8) -0.0080(7) -0.0036(7) -0.0006(7) O1 0.0185(7) 0.0252(7) 0.0203(7) -0.0084(6) -0.0019(5) -0.0001(5) O2 0.0253(7) 0.0274(7) 0.0198(7) -0.0087(6) 0.0000(5) -0.0040(6) O3 0.0270(8) 0.0233(7) 0.0309(8) -0.0118(6) -0.0050(6) 0.0009(6) Ti1 0.0182(2) 0.0204(2) 0.01755(19) -0.00727(14) -0.00227(13) -0.00043(13) O4 0.134(8) 0.089(6) 0.206(11) -0.057(7) 0.010(8) 0.019(6) C22 0.108(9) 0.068(6) 0.115(9) -0.011(6) 0.005(7) -0.021(6) C23 0.069(5) 0.067(5) 0.083(6) -0.029(4) -0.014(4) 0.014(4) C24 0.073(5) 0.058(4) 0.061(4) -0.029(3) 0.016(4) -0.010(3) C25 0.107(8) 0.087(7) 0.045(4) -0.002(4) 0.012(4) 0.007(6) _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 C1 O2 1.343(3) . ? C1 C6 1.401(3) . ? C1 C2 1.405(3) . ? C2 C3 1.397(3) . ? C2 H2 0.9300 . ? C3 C4 1.401(4) . ? C3 C17 1.509(3) . ? C4 C5 1.394(4) . ? C4 C18 1.513(3) . ? C5 C6 1.396(3) . ? C5 H5 0.9300 . ? C6 C7 1.504(3) . ? C7 N1 1.488(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N1 1.483(3) . ? C8 C9 1.510(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N2 1.495(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O3 1.350(3) . ? C10 C11 1.386(3) . ? C10 C15 1.416(3) . ? C11 C12 1.390(3) . ? C11 H11 0.9300 . ? C12 C13 1.398(4) . ? C12 C19 1.505(4) . ? C13 C14 1.392(4) . ? C13 C20 1.515(4) . ? C14 C15 1.401(3) . ? C14 H14 0.9300 . ? C15 C16 1.514(3) . ? C16 N2 1.490(3) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 N2 1.476(3) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? N1 Ti1 2.2227(18) . ? N1 H1N 0.87(3) . ? N2 Ti1 2.3322(18) . ? O1 Ti1 1.7817(14) . ? O1 Ti1 1.9594(15) 2_666 ? O2 Ti1 1.9093(15) . ? O3 Ti1 1.8880(16) . ? Ti1 O1 1.9594(15) 2_666 ? Ti1 Ti1 2.8133(7) 2_666 ? O4 C25 1.345(15) . ? O4 C22 1.376(15) . ? C22 C23 1.436(13) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.413(11) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.368(12) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? 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 C1 C6 121.15(19) . . ? O2 C1 C2 120.0(2) . . ? C6 C1 C2 118.8(2) . . ? C3 C2 C1 121.6(2) . . ? C3 C2 H2 119.2 . . ? C1 C2 H2 119.2 . . ? C2 C3 C4 119.7(2) . . ? C2 C3 C17 119.6(3) . . ? C4 C3 C17 120.7(2) . . ? C5 C4 C3 118.3(2) . . ? C5 C4 C18 119.8(3) . . ? C3 C4 C18 121.9(2) . . ? C4 C5 C6 122.6(2) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C5 C6 C1 119.0(2) . . ? C5 C6 C7 121.0(2) . . ? C1 C6 C7 119.99(19) . . ? N1 C7 C6 111.42(18) . . ? N1 C7 H7A 109.3 . . ? C6 C7 H7A 109.3 . . ? N1 C7 H7B 109.3 . . ? C6 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? N1 C8 C9 110.31(18) . . ? N1 C8 H8A 109.6 . . ? C9 C8 H8A 109.6 . . ? N1 C8 H8B 109.6 . . ? C9 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? N2 C9 C8 110.62(18) . . ? N2 C9 H9A 109.5 . . ? C8 C9 H9A 109.5 . . ? N2 C9 H9B 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? O3 C10 C11 119.0(2) . . ? O3 C10 C15 121.9(2) . . ? C11 C10 C15 119.1(2) . . ? C10 C11 C12 122.4(2) . . ? C10 C11 H11 118.8 . . ? C12 C11 H11 118.8 . . ? C11 C12 C13 119.4(2) . . ? C11 C12 C19 120.3(3) . . ? C13 C12 C19 120.4(2) . . ? C14 C13 C12 118.4(2) . . ? C14 C13 C20 120.4(3) . . ? C12 C13 C20 121.2(3) . . ? C13 C14 C15 123.0(3) . . ? C13 C14 H14 118.5 . . ? C15 C14 H14 118.5 . . ? C14 C15 C10 117.6(2) . . ? C14 C15 C16 119.5(2) . . ? C10 C15 C16 122.8(2) . . ? N2 C16 C15 113.43(19) . . ? N2 C16 H16A 108.9 . . ? C15 C16 H16A 108.9 . . ? N2 C16 H16B 108.9 . . ? C15 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? C3 C17 H17A 109.5 . . ? C3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C4 C18 H18A 109.5 . . ? C4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C12 C19 H19A 109.5 . . ? C12 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C12 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C13 C20 H20A 109.5 . . ? C13 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C13 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N2 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C8 N1 C7 113.83(17) . . ? C8 N1 Ti1 112.71(13) . . ? C7 N1 Ti1 112.06(13) . . ? C8 N1 H1N 109(2) . . ? C7 N1 H1N 105.7(19) . . ? Ti1 N1 H1N 102.5(19) . . ? C21 N2 C16 109.38(18) . . ? C21 N2 C9 110.06(18) . . ? C16 N2 C9 106.90(17) . . ? C21 N2 Ti1 114.81(14) . . ? C16 N2 Ti1 109.67(13) . . ? C9 N2 Ti1 105.68(13) . . ? Ti1 O1 Ti1 97.41(7) . 2_666 ? C1 O2 Ti1 138.40(14) . . ? C10 O3 Ti1 138.05(15) . . ? O1 Ti1 O3 101.82(7) . . ? O1 Ti1 O2 101.93(7) . . ? O3 Ti1 O2 99.48(7) . . ? O1 Ti1 O1 82.59(7) . 2_666 ? O3 Ti1 O1 95.42(7) . 2_666 ? O2 Ti1 O1 163.12(7) . 2_666 ? O1 Ti1 N1 94.87(7) . . ? O3 Ti1 N1 162.33(7) . . ? O2 Ti1 N1 82.50(7) . . ? O1 Ti1 N1 80.91(7) 2_666 . ? O1 Ti1 N2 164.37(7) . . ? O3 Ti1 N2 84.92(7) . . ? O2 Ti1 N2 90.68(7) . . ? O1 Ti1 N2 82.75(6) 2_666 . ? N1 Ti1 N2 77.48(7) . . ? O1 Ti1 Ti1 43.68(5) . 2_666 ? O3 Ti1 Ti1 101.27(5) . 2_666 ? O2 Ti1 Ti1 142.88(5) . 2_666 ? O1 Ti1 Ti1 38.90(4) 2_666 2_666 ? N1 Ti1 Ti1 86.78(5) . 2_666 ? N2 Ti1 Ti1 121.47(5) . 2_666 ? C25 O4 C22 108.2(10) . . ? O4 C22 C23 105.2(9) . . ? O4 C22 H22A 110.7 . . ? C23 C22 H22A 110.7 . . ? O4 C22 H22B 110.7 . . ? C23 C22 H22B 110.7 . . ? H22A C22 H22B 108.8 . . ? C24 C23 C22 105.1(8) . . ? C24 C23 H23A 110.7 . . ? C22 C23 H23A 110.7 . . ? C24 C23 H23B 110.7 . . ? C22 C23 H23B 110.7 . . ? H23A C23 H23B 108.8 . . ? C25 C24 C23 106.3(8) . . ? C25 C24 H24A 110.5 . . ? C23 C24 H24A 110.5 . . ? C25 C24 H24B 110.5 . . ? C23 C24 H24B 110.5 . . ? H24A C24 H24B 108.7 . . ? O4 C25 C24 106.0(10) . . ? O4 C25 H25A 110.5 . . ? C24 C25 H25A 110.5 . . ? O4 C25 H25B 110.5 . . ? C24 C25 H25B 110.5 . . ? H25A C25 H25B 108.7 . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 28.01 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.638 _refine_diff_density_min -0.303 _refine_diff_density_rms 0.086 #===END data_L42Ti2(OiPr)2(m-O) _database_code_depnum_ccdc_archive 'CCDC 829877' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H45 Cl4 N4 O7 Ti2,0.5(C4 H10 O)' _chemical_formula_sum 'C40 H50 Cl4 N4 O7.50 Ti2' _chemical_formula_weight 944.44 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' Cl Cl 0.1484 0.1585 '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 _symmetry_space_group_name_Hall '-P 2ybc' 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 13.0593(13) _cell_length_b 23.948(2) _cell_length_c 15.3506(16) _cell_angle_alpha 90.00 _cell_angle_beta 95.966(2) _cell_angle_gamma 90.00 _cell_volume 4774.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description shapeless _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 0.607 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51349 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 27.00 _reflns_number_total 10419 _reflns_number_gt 8611 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1233P)^2^+0.7828P] 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 10419 _refine_ls_number_parameters 556 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1760 _refine_ls_wR_factor_gt 0.1667 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3824(2) 0.58864(11) 0.83719(16) 0.0411(6) Uani 1 1 d . . . C2 C 0.3947(3) 0.64415(12) 0.8666(2) 0.0522(8) Uani 1 1 d . . . C3 C 0.4755(3) 0.65912(16) 0.9273(2) 0.0682(11) Uani 1 1 d . . . H3 H 0.4829 0.6968 0.9463 0.082 Uiso 1 1 calc R . . C4 C 0.5454(3) 0.61955(18) 0.9603(2) 0.0708(11) Uani 1 1 d . . . H4 H 0.6013 0.6300 1.0018 0.085 Uiso 1 1 calc R . . C5 C 0.5345(3) 0.56473(16) 0.93327(19) 0.0593(9) Uani 1 1 d . . . H5 H 0.5828 0.5375 0.9564 0.071 Uiso 1 1 calc R . . C6 C 0.4529(2) 0.54888(12) 0.87211(16) 0.0459(7) Uani 1 1 d . . . C7 C 0.4393(2) 0.48913(11) 0.84256(17) 0.0427(6) Uani 1 1 d . . . H7A H 0.5022 0.4677 0.8625 0.051 Uiso 1 1 calc R . . H7B H 0.3811 0.4724 0.8698 0.051 Uiso 1 1 calc R . . C8 C 0.5073(2) 0.50485(11) 0.70083(17) 0.0374(6) Uani 1 1 d . . . H8A H 0.5599 0.4751 0.7012 0.045 Uiso 1 1 calc R . . H8B H 0.5392 0.5376 0.7322 0.045 Uiso 1 1 calc R . . C9 C 0.47090(19) 0.52067(10) 0.60788(16) 0.0320(5) Uani 1 1 d . . . H9A H 0.5272 0.5389 0.5801 0.038 Uiso 1 1 calc R . . H9B H 0.4491 0.4869 0.5735 0.038 Uiso 1 1 calc R . . C10 C 0.3375(2) 0.57492(10) 0.52082(15) 0.0339(5) Uani 1 1 d . . . H10A H 0.3037 0.5419 0.4916 0.041 Uiso 1 1 calc R . . H10B H 0.3925 0.5876 0.4856 0.041 Uiso 1 1 calc R . . C11 C 0.2598(2) 0.62094(10) 0.52603(16) 0.0341(5) Uani 1 1 d . . . C12 C 0.2634(2) 0.66951(13) 0.4763(2) 0.0483(7) Uani 1 1 d . . . H12 H 0.3148 0.6733 0.4373 0.058 Uiso 1 1 calc R . . C13 C 0.1937(3) 0.71200(14) 0.4829(2) 0.0574(9) Uani 1 1 d . . . H13 H 0.1962 0.7444 0.4474 0.069 Uiso 1 1 calc R . . C14 C 0.1205(2) 0.70774(12) 0.5409(2) 0.0484(7) Uani 1 1 d . . . H14 H 0.0725 0.7371 0.5460 0.058 Uiso 1 1 calc R . . C15 C 0.11748(19) 0.66007(10) 0.59170(17) 0.0340(5) Uani 1 1 d . . . C16 C 0.18364(18) 0.61510(9) 0.58346(15) 0.0293(5) Uani 1 1 d . . . C17 C 0.1489(2) 0.49364(11) 0.84345(17) 0.0414(6) Uani 1 1 d . . . H17 H 0.2026 0.5152 0.8806 0.050 Uiso 1 1 calc R . . C18 C 0.0558(4) 0.52920(19) 0.8265(3) 0.0829(13) Uani 1 1 d . . . H18A H 0.0735 0.5633 0.7962 0.124 Uiso 1 1 calc R . . H18B H 0.0301 0.5390 0.8822 0.124 Uiso 1 1 calc R . . H18C H 0.0025 0.5087 0.7899 0.124 Uiso 1 1 calc R . . C19 C 0.1276(4) 0.44031(15) 0.8907(2) 0.0795(13) Uani 1 1 d . . . H19A H 0.0728 0.4195 0.8564 0.119 Uiso 1 1 calc R . . H19B H 0.1059 0.4493 0.9483 0.119 Uiso 1 1 calc R . . H19C H 0.1903 0.4175 0.8981 0.119 Uiso 1 1 calc R . . C20 C 0.17064(19) 0.27277(9) 0.57787(15) 0.0300(5) Uani 1 1 d . . . C21 C 0.1515(2) 0.22658(10) 0.52202(17) 0.0345(5) Uani 1 1 d . . . C22 C 0.0774(2) 0.18711(10) 0.5367(2) 0.0430(6) Uani 1 1 d . . . H22 H 0.0659 0.1561 0.4984 0.052 Uiso 1 1 calc R . . C23 C 0.0204(2) 0.19305(11) 0.6071(2) 0.0463(7) Uani 1 1 d . . . H23 H -0.0297 0.1659 0.6179 0.056 Uiso 1 1 calc R . . C24 C 0.0369(2) 0.23913(11) 0.66218(19) 0.0410(6) Uani 1 1 d . . . H24 H -0.0034 0.2436 0.7098 0.049 Uiso 1 1 calc R . . C25 C 0.1116(2) 0.27866(9) 0.64838(16) 0.0337(5) Uani 1 1 d . . . C26 C 0.1316(2) 0.32782(10) 0.70886(16) 0.0357(5) Uani 1 1 d . . . H26A H 0.0757 0.3305 0.7476 0.043 Uiso 1 1 calc R . . H26B H 0.1971 0.3219 0.7463 0.043 Uiso 1 1 calc R . . C27 C 0.03820(19) 0.39553(10) 0.60863(18) 0.0359(5) Uani 1 1 d . . . H27A H -0.0065 0.4156 0.6465 0.043 Uiso 1 1 calc R . . H27B H 0.0023 0.3610 0.5872 0.043 Uiso 1 1 calc R . . C28 C 0.05795(19) 0.43187(10) 0.53210(17) 0.0345(5) Uani 1 1 d . . . H28A H -0.0060 0.4363 0.4921 0.041 Uiso 1 1 calc R . . H28B H 0.0814 0.4693 0.5529 0.041 Uiso 1 1 calc R . . C29 C 0.1658(2) 0.43712(10) 0.40988(16) 0.0359(5) Uani 1 1 d . . . H29A H 0.2012 0.4720 0.4304 0.043 Uiso 1 1 calc R . . H29B H 0.1027 0.4473 0.3718 0.043 Uiso 1 1 calc R . . C30 C 0.2354(2) 0.40306(11) 0.35869(16) 0.0382(6) Uani 1 1 d . . . C31 C 0.2120(3) 0.39249(15) 0.26926(18) 0.0512(7) Uani 1 1 d . . . H31 H 0.1510 0.4077 0.2393 0.061 Uiso 1 1 calc R . . C32 C 0.2761(3) 0.36023(16) 0.2237(2) 0.0593(9) Uani 1 1 d . . . H32 H 0.2593 0.3538 0.1628 0.071 Uiso 1 1 calc R . . C33 C 0.3641(3) 0.33744(14) 0.2662(2) 0.0520(8) Uani 1 1 d . . . H33 H 0.4088 0.3156 0.2348 0.062 Uiso 1 1 calc R . . C34 C 0.3871(2) 0.34671(11) 0.35556(17) 0.0384(6) Uani 1 1 d . . . C35 C 0.3253(2) 0.38022(10) 0.40297(15) 0.0324(5) Uani 1 1 d . . . C36 C 0.4211(2) 0.32492(11) 0.71471(18) 0.0415(6) Uani 1 1 d . . . H36 H 0.3745 0.2920 0.7033 0.050 Uiso 1 1 calc R . . C37 C 0.5148(4) 0.3159(2) 0.6697(3) 0.0949(17) Uani 1 1 d . . . H37A H 0.4951 0.3102 0.6069 0.142 Uiso 1 1 calc R . . H37B H 0.5516 0.2829 0.6942 0.142 Uiso 1 1 calc R . . H37C H 0.5596 0.3487 0.6780 0.142 Uiso 1 1 calc R . . C38 C 0.4450(3) 0.33181(14) 0.8119(2) 0.0605(9) Uani 1 1 d . . . H38A H 0.4969 0.3611 0.8239 0.091 Uiso 1 1 calc R . . H38B H 0.4715 0.2965 0.8376 0.091 Uiso 1 1 calc R . . H38C H 0.3821 0.3422 0.8377 0.091 Uiso 1 1 calc R . . C39 C 0.7490(13) 0.4247(6) 0.9302(7) 0.134(6) Uani 0.50 1 d P . . H39A H 0.7996 0.4120 0.9786 0.161 Uiso 0.50 1 calc PR . . H39B H 0.6780 0.4193 0.9459 0.161 Uiso 0.50 1 calc PR . . C40 C 0.7682(10) 0.4819(8) 0.9017(10) 0.155(7) Uani 0.50 1 d P . . H40A H 0.7935 0.5046 0.9526 0.233 Uiso 0.50 1 calc PR . . H40B H 0.7041 0.4980 0.8737 0.233 Uiso 0.50 1 calc PR . . H40C H 0.8200 0.4813 0.8598 0.233 Uiso 0.50 1 calc PR . . C41 C 0.7791(11) 0.3418(6) 0.8682(12) 0.153(7) Uani 0.50 1 d P . . H41A H 0.7133 0.3253 0.8825 0.183 Uiso 0.50 1 calc PR . . H41B H 0.8308 0.3372 0.9196 0.183 Uiso 0.50 1 calc PR . . C42 C 0.8147(12) 0.3124(6) 0.7904(9) 0.133(5) Uani 0.50 1 d P . . H42A H 0.8187 0.3393 0.7426 0.200 Uiso 0.50 1 calc PR . . H42B H 0.7659 0.2827 0.7712 0.200 Uiso 0.50 1 calc PR . . H42C H 0.8829 0.2962 0.8066 0.200 Uiso 0.50 1 calc PR . . Cl1 Cl 0.30561(8) 0.69318(3) 0.82313(7) 0.0705(3) Uani 1 1 d . . . Cl2 Cl 0.02734(5) 0.65592(3) 0.66671(4) 0.04040(17) Uani 1 1 d . . . Cl3 Cl 0.22315(6) 0.21993(3) 0.43390(5) 0.0519(2) Uani 1 1 d . . . Cl4 Cl 0.49668(5) 0.31604(3) 0.40948(5) 0.04601(19) Uani 1 1 d . . . N1 N 0.41903(17) 0.48488(8) 0.74576(13) 0.0330(5) Uani 1 1 d . . . H1N H 0.407(2) 0.4528(13) 0.734(2) 0.040 Uiso 1 1 d . . . N2 N 0.38313(15) 0.55948(8) 0.61004(12) 0.0290(4) Uani 1 1 d . . . N3 N 0.13750(17) 0.38108(8) 0.65988(14) 0.0307(4) Uani 1 1 d . . . H3N H 0.156(2) 0.4062(13) 0.6914(19) 0.037 Uiso 1 1 d . . . N4 N 0.13799(16) 0.40473(8) 0.48590(13) 0.0311(4) Uani 1 1 d . . . H4N H 0.113(2) 0.3718(13) 0.4708(19) 0.037 Uiso 1 1 d . . . O1 O 0.26792(12) 0.46226(6) 0.61120(10) 0.0271(3) Uani 1 1 d . . . O2 O 0.30462(15) 0.57609(7) 0.77777(11) 0.0376(4) Uani 1 1 d . . . O3 O 0.17334(13) 0.56804(6) 0.62799(11) 0.0307(4) Uani 1 1 d . . . O4 O 0.18842(14) 0.48010(7) 0.76338(11) 0.0334(4) Uani 1 1 d . . . O5 O 0.24357(13) 0.30956(6) 0.56297(11) 0.0311(4) Uani 1 1 d . . . O6 O 0.35149(13) 0.39108(7) 0.48791(10) 0.0300(4) Uani 1 1 d . . . O7 O 0.36911(13) 0.37358(6) 0.68016(11) 0.0305(4) Uani 1 1 d . . . O8 O 0.7650(10) 0.4003(3) 0.8481(5) 0.162(5) Uani 0.50 1 d P . . Ti1 Ti 0.26817(3) 0.519423(15) 0.69077(3) 0.02638(13) Uani 1 1 d . . . Ti2 Ti 0.27364(3) 0.387348(15) 0.58530(3) 0.02469(13) Uani 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 C1 0.0620(17) 0.0328(13) 0.0300(12) -0.0111(10) 0.0116(12) -0.0125(12) C2 0.078(2) 0.0353(15) 0.0463(16) -0.0185(12) 0.0183(15) -0.0150(14) C3 0.103(3) 0.053(2) 0.0495(18) -0.0283(16) 0.0091(19) -0.026(2) C4 0.093(3) 0.078(3) 0.0394(17) -0.0219(17) -0.0015(17) -0.034(2) C5 0.079(2) 0.066(2) 0.0315(14) -0.0113(14) -0.0050(14) -0.0187(18) C6 0.0666(19) 0.0439(16) 0.0265(12) -0.0072(11) 0.0016(12) -0.0136(13) C7 0.0595(17) 0.0343(14) 0.0320(13) 0.0011(10) -0.0058(12) -0.0057(12) C8 0.0393(13) 0.0304(12) 0.0417(14) -0.0066(10) -0.0001(11) 0.0008(10) C9 0.0359(12) 0.0242(11) 0.0365(12) -0.0048(9) 0.0070(10) -0.0029(9) C10 0.0416(13) 0.0313(12) 0.0294(11) 0.0017(9) 0.0067(10) -0.0032(10) C11 0.0390(13) 0.0278(12) 0.0353(12) 0.0046(10) 0.0032(10) -0.0017(10) C12 0.0444(15) 0.0478(17) 0.0530(17) 0.0245(13) 0.0060(13) 0.0017(13) C13 0.0561(18) 0.0425(17) 0.074(2) 0.0321(16) 0.0073(16) 0.0028(14) C14 0.0445(15) 0.0301(14) 0.0690(19) 0.0139(13) -0.0011(14) 0.0044(11) C15 0.0367(13) 0.0246(11) 0.0404(13) 0.0006(10) 0.0018(10) -0.0014(9) C16 0.0362(12) 0.0187(10) 0.0321(11) 0.0005(8) -0.0009(9) -0.0027(9) C17 0.0643(18) 0.0294(13) 0.0334(13) -0.0002(10) 0.0190(12) -0.0008(12) C18 0.103(3) 0.081(3) 0.072(2) 0.017(2) 0.046(2) 0.043(2) C19 0.145(4) 0.0415(18) 0.062(2) 0.0107(16) 0.059(2) -0.001(2) C20 0.0403(12) 0.0148(10) 0.0335(12) 0.0012(8) -0.0031(10) -0.0006(9) C21 0.0449(14) 0.0205(11) 0.0368(12) -0.0040(9) -0.0023(10) 0.0010(10) C22 0.0547(16) 0.0157(11) 0.0559(16) -0.0025(10) -0.0073(13) -0.0022(10) C23 0.0536(17) 0.0212(12) 0.0630(18) 0.0079(12) 0.0011(14) -0.0091(11) C24 0.0506(15) 0.0246(12) 0.0483(15) 0.0079(10) 0.0073(12) -0.0054(11) C25 0.0448(14) 0.0194(11) 0.0363(12) 0.0050(9) 0.0008(10) -0.0031(9) C26 0.0491(15) 0.0255(12) 0.0335(12) 0.0019(9) 0.0088(11) -0.0049(10) C27 0.0358(13) 0.0251(11) 0.0474(14) -0.0035(10) 0.0071(11) 0.0001(10) C28 0.0361(13) 0.0223(11) 0.0442(14) -0.0024(10) 0.0003(10) 0.0018(9) C29 0.0423(14) 0.0288(12) 0.0350(12) 0.0041(10) -0.0035(10) -0.0018(10) C30 0.0506(15) 0.0332(13) 0.0303(12) -0.0001(10) 0.0019(11) -0.0102(11) C31 0.0570(18) 0.063(2) 0.0321(14) -0.0016(13) -0.0004(12) -0.0127(15) C32 0.070(2) 0.077(2) 0.0311(14) -0.0155(15) 0.0044(14) -0.0167(18) C33 0.0628(19) 0.0520(18) 0.0434(15) -0.0191(13) 0.0155(14) -0.0155(15) C34 0.0459(14) 0.0302(13) 0.0405(13) -0.0102(10) 0.0109(11) -0.0123(11) C35 0.0435(13) 0.0245(11) 0.0300(11) -0.0044(9) 0.0068(10) -0.0125(10) C36 0.0559(16) 0.0217(12) 0.0445(14) 0.0020(10) -0.0067(12) 0.0091(11) C37 0.094(3) 0.116(4) 0.077(3) 0.012(3) 0.019(2) 0.069(3) C38 0.087(2) 0.0477(18) 0.0430(16) 0.0108(14) -0.0101(16) 0.0097(17) C39 0.205(15) 0.106(10) 0.082(7) -0.023(7) -0.027(8) 0.062(10) C40 0.101(9) 0.23(2) 0.132(11) -0.063(12) -0.024(8) 0.047(11) C41 0.111(9) 0.095(9) 0.24(2) 0.052(11) -0.022(11) 0.025(8) C42 0.151(12) 0.103(9) 0.135(11) -0.046(8) -0.036(9) 0.028(8) Cl1 0.0949(7) 0.0294(4) 0.0888(6) -0.0248(4) 0.0172(5) -0.0066(4) Cl2 0.0440(4) 0.0316(3) 0.0463(4) -0.0076(2) 0.0079(3) 0.0040(2) Cl3 0.0699(5) 0.0362(4) 0.0505(4) -0.0197(3) 0.0116(3) -0.0057(3) Cl4 0.0488(4) 0.0319(3) 0.0591(4) -0.0128(3) 0.0137(3) -0.0027(3) N1 0.0465(12) 0.0191(9) 0.0320(10) -0.0039(8) -0.0027(9) -0.0036(8) N2 0.0353(10) 0.0210(9) 0.0313(10) -0.0017(7) 0.0054(8) -0.0014(8) N3 0.0425(11) 0.0182(9) 0.0317(10) -0.0038(8) 0.0060(9) -0.0042(8) N4 0.0401(11) 0.0192(9) 0.0332(10) -0.0029(8) -0.0008(8) -0.0010(8) O1 0.0361(8) 0.0161(7) 0.0286(8) -0.0005(6) 0.0015(6) -0.0009(6) O2 0.0545(11) 0.0226(8) 0.0361(9) -0.0086(7) 0.0061(8) -0.0053(7) O3 0.0385(9) 0.0170(7) 0.0379(9) 0.0011(6) 0.0099(7) -0.0005(6) O4 0.0496(10) 0.0214(8) 0.0309(8) -0.0015(6) 0.0121(7) -0.0029(7) O5 0.0411(9) 0.0176(7) 0.0349(9) -0.0044(6) 0.0060(7) -0.0025(6) O6 0.0377(9) 0.0241(8) 0.0283(8) -0.0044(6) 0.0043(7) -0.0049(7) O7 0.0407(9) 0.0188(7) 0.0310(8) -0.0001(6) -0.0010(7) 0.0029(6) O8 0.341(15) 0.083(5) 0.069(4) -0.008(4) 0.053(7) -0.067(7) Ti1 0.0379(2) 0.0147(2) 0.0270(2) -0.00218(14) 0.00565(17) -0.00205(15) Ti2 0.0337(2) 0.0149(2) 0.0254(2) -0.00196(14) 0.00224(16) -0.00064(14) _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 C1 O2 1.328(3) . ? C1 C6 1.392(4) . ? C1 C2 1.408(4) . ? C2 C3 1.380(5) . ? C2 Cl1 1.737(4) . ? C3 C4 1.376(6) . ? C3 H3 0.9500 . ? C4 C5 1.380(5) . ? C4 H4 0.9500 . ? C5 C6 1.397(4) . ? C5 H5 0.9500 . ? C6 C7 1.506(4) . ? C7 N1 1.485(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N1 1.483(4) . ? C8 C9 1.505(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 N2 1.479(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N2 1.482(3) . ? C10 C11 1.506(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.395(4) . ? C11 C16 1.403(4) . ? C12 C13 1.376(5) . ? C12 H12 0.9500 . ? C13 C14 1.376(5) . ? C13 H13 0.9500 . ? C14 C15 1.385(4) . ? C14 H14 0.9500 . ? C15 C16 1.395(3) . ? C15 Cl2 1.733(3) . ? C16 O3 1.332(3) . ? C17 O4 1.419(3) . ? C17 C18 1.485(5) . ? C17 C19 1.509(4) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 O5 1.334(3) . ? C20 C25 1.399(4) . ? C20 C21 1.406(3) . ? C21 C22 1.388(4) . ? C21 Cl3 1.730(3) . ? C22 C23 1.381(4) . ? C22 H22 0.9500 . ? C23 C24 1.393(4) . ? C23 H23 0.9500 . ? C24 C25 1.391(3) . ? C24 H24 0.9500 . ? C25 C26 1.505(3) . ? C26 N3 1.487(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 N3 1.486(3) . ? C27 C28 1.506(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 N4 1.474(3) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 N4 1.478(3) . ? C29 C30 1.502(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.398(4) . ? C30 C35 1.405(4) . ? C31 C32 1.382(5) . ? C31 H31 0.9500 . ? C32 C33 1.374(5) . ? C32 H32 0.9500 . ? C33 C34 1.392(4) . ? C33 H33 0.9500 . ? C34 C35 1.396(4) . ? C34 Cl4 1.739(3) . ? C35 O6 1.339(3) . ? C36 O7 1.423(3) . ? C36 C37 1.482(5) . ? C36 C38 1.502(4) . ? C36 H36 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 O8 1.426(13) . ? C39 C40 1.47(2) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 O8 1.442(14) . ? C41 C42 1.50(2) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? N1 Ti1 2.221(2) . ? N1 H1N 0.80(3) . ? N2 Ti1 2.258(2) . ? N3 Ti2 2.217(2) . ? N3 H3N 0.79(3) . ? N4 Ti2 2.253(2) . ? N4 H4N 0.88(3) . ? O1 Ti1 1.8345(15) . ? O1 Ti2 1.8406(15) . ? O2 Ti1 1.9285(17) . ? O3 Ti1 1.8895(17) . ? O4 Ti1 1.8588(17) . ? O5 Ti2 1.9272(16) . ? O6 Ti2 1.8953(17) . ? O7 Ti2 1.8456(17) . ? 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 C1 C6 122.5(2) . . ? O2 C1 C2 119.2(3) . . ? C6 C1 C2 118.3(3) . . ? C3 C2 C1 121.0(3) . . ? C3 C2 Cl1 121.2(3) . . ? C1 C2 Cl1 117.8(3) . . ? C4 C3 C2 120.1(3) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.0(3) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 120.6(4) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C1 C6 C5 120.0(3) . . ? C1 C6 C7 118.7(2) . . ? C5 C6 C7 121.2(3) . . ? N1 C7 C6 111.7(2) . . ? N1 C7 H7A 109.3 . . ? C6 C7 H7A 109.3 . . ? N1 C7 H7B 109.3 . . ? C6 C7 H7B 109.3 . . ? H7A C7 H7B 107.9 . . ? N1 C8 C9 109.7(2) . . ? N1 C8 H8A 109.7 . . ? C9 C8 H8A 109.7 . . ? N1 C8 H8B 109.7 . . ? C9 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? N2 C9 C8 107.83(19) . . ? N2 C9 H9A 110.1 . . ? C8 C9 H9A 110.1 . . ? N2 C9 H9B 110.1 . . ? C8 C9 H9B 110.1 . . ? H9A C9 H9B 108.5 . . ? N2 C10 C11 110.0(2) . . ? N2 C10 H10A 109.7 . . ? C11 C10 H10A 109.7 . . ? N2 C10 H10B 109.7 . . ? C11 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? C12 C11 C16 119.6(2) . . ? C12 C11 C10 121.3(2) . . ? C16 C11 C10 119.1(2) . . ? C13 C12 C11 121.1(3) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C14 C13 C12 120.2(3) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 119.2(3) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C14 C15 C16 122.1(3) . . ? C14 C15 Cl2 118.8(2) . . ? C16 C15 Cl2 119.08(19) . . ? O3 C16 C15 120.7(2) . . ? O3 C16 C11 121.5(2) . . ? C15 C16 C11 117.8(2) . . ? O4 C17 C18 110.1(2) . . ? O4 C17 C19 108.9(2) . . ? C18 C17 C19 112.4(3) . . ? O4 C17 H17 108.4 . . ? C18 C17 H17 108.4 . . ? C19 C17 H17 108.4 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O5 C20 C25 121.7(2) . . ? O5 C20 C21 120.0(2) . . ? C25 C20 C21 118.3(2) . . ? C22 C21 C20 121.3(2) . . ? C22 C21 Cl3 120.5(2) . . ? C20 C21 Cl3 118.2(2) . . ? C23 C22 C21 119.9(2) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 119.6(2) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C25 C24 C23 120.9(3) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C20 120.0(2) . . ? C24 C25 C26 121.1(2) . . ? C20 C25 C26 118.8(2) . . ? N3 C26 C25 111.9(2) . . ? N3 C26 H26A 109.2 . . ? C25 C26 H26A 109.2 . . ? N3 C26 H26B 109.2 . . ? C25 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? N3 C27 C28 109.7(2) . . ? N3 C27 H27A 109.7 . . ? C28 C27 H27A 109.7 . . ? N3 C27 H27B 109.7 . . ? C28 C27 H27B 109.7 . . ? H27A C27 H27B 108.2 . . ? N4 C28 C27 107.95(19) . . ? N4 C28 H28A 110.1 . . ? C27 C28 H28A 110.1 . . ? N4 C28 H28B 110.1 . . ? C27 C28 H28B 110.1 . . ? H28A C28 H28B 108.4 . . ? N4 C29 C30 109.9(2) . . ? N4 C29 H29A 109.7 . . ? C30 C29 H29A 109.7 . . ? N4 C29 H29B 109.7 . . ? C30 C29 H29B 109.7 . . ? H29A C29 H29B 108.2 . . ? C31 C30 C35 119.4(3) . . ? C31 C30 C29 122.0(3) . . ? C35 C30 C29 118.6(2) . . ? C32 C31 C30 121.1(3) . . ? C32 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C33 C32 C31 120.2(3) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C32 C33 C34 119.2(3) . . ? C32 C33 H33 120.4 . . ? C34 C33 H33 120.4 . . ? C33 C34 C35 121.9(3) . . ? C33 C34 Cl4 119.0(2) . . ? C35 C34 Cl4 119.1(2) . . ? O6 C35 C34 121.1(2) . . ? O6 C35 C30 120.8(2) . . ? C34 C35 C30 118.1(2) . . ? O7 C36 C37 109.3(3) . . ? O7 C36 C38 108.8(2) . . ? C37 C36 C38 112.6(3) . . ? O7 C36 H36 108.7 . . ? C37 C36 H36 108.7 . . ? C38 C36 H36 108.7 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O8 C39 C40 94.3(11) . . ? O8 C39 H39A 112.9 . . ? C40 C39 H39A 112.9 . . ? O8 C39 H39B 112.9 . . ? C40 C39 H39B 112.9 . . ? H39A C39 H39B 110.3 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O8 C41 C42 109.1(13) . . ? O8 C41 H41A 109.9 . . ? C42 C41 H41A 109.9 . . ? O8 C41 H41B 109.9 . . ? C42 C41 H41B 109.9 . . ? H41A C41 H41B 108.3 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C8 N1 C7 112.1(2) . . ? C8 N1 Ti1 113.89(15) . . ? C7 N1 Ti1 114.41(17) . . ? C8 N1 H1N 110(2) . . ? C7 N1 H1N 108(2) . . ? Ti1 N1 H1N 97(2) . . ? C9 N2 C10 111.95(18) . . ? C9 N2 Ti1 107.85(14) . . ? C10 N2 Ti1 112.77(15) . . ? C27 N3 C26 112.3(2) . . ? C27 N3 Ti2 114.41(15) . . ? C26 N3 Ti2 113.95(16) . . ? C27 N3 H3N 110(2) . . ? C26 N3 H3N 112(2) . . ? Ti2 N3 H3N 93(2) . . ? C28 N4 C29 113.18(19) . . ? C28 N4 Ti2 107.62(15) . . ? C29 N4 Ti2 113.02(15) . . ? C28 N4 H4N 104.9(19) . . ? C29 N4 H4N 112.4(19) . . ? Ti2 N4 H4N 105.1(19) . . ? Ti1 O1 Ti2 150.91(9) . . ? C1 O2 Ti1 138.70(17) . . ? C16 O3 Ti1 133.42(15) . . ? C17 O4 Ti1 132.88(15) . . ? C20 O5 Ti2 138.04(15) . . ? C35 O6 Ti2 130.94(15) . . ? C36 O7 Ti2 134.22(16) . . ? C39 O8 C41 103.8(11) . . ? O1 Ti1 O4 93.37(7) . . ? O1 Ti1 O3 99.47(7) . . ? O4 Ti1 O3 103.87(8) . . ? O1 Ti1 O2 165.79(8) . . ? O4 Ti1 O2 93.13(7) . . ? O3 Ti1 O2 91.21(8) . . ? O1 Ti1 N1 85.14(7) . . ? O4 Ti1 N1 96.52(8) . . ? O3 Ti1 N1 158.73(8) . . ? O2 Ti1 N1 81.58(8) . . ? O1 Ti1 N2 84.66(7) . . ? O4 Ti1 N2 172.08(8) . . ? O3 Ti1 N2 84.04(7) . . ? O2 Ti1 N2 87.18(7) . . ? N1 Ti1 N2 75.68(8) . . ? O1 Ti2 O7 92.46(7) . . ? O1 Ti2 O6 99.30(7) . . ? O7 Ti2 O6 104.89(8) . . ? O1 Ti2 O5 165.56(8) . . ? O7 Ti2 O5 94.37(7) . . ? O6 Ti2 O5 91.23(7) . . ? O1 Ti2 N3 84.36(7) . . ? O7 Ti2 N3 95.32(8) . . ? O6 Ti2 N3 159.22(8) . . ? O5 Ti2 N3 82.35(7) . . ? O1 Ti2 N4 85.38(7) . . ? O7 Ti2 N4 170.51(8) . . ? O6 Ti2 N4 84.59(8) . . ? O5 Ti2 N4 85.80(7) . . ? N3 Ti2 N4 75.29(8) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.314 _refine_diff_density_min -0.332 _refine_diff_density_rms 0.127