# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2008 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Sergey Karlov' _publ_contact_author_email SERGEJ@ORG.CHEM.MSU.RU _publ_section_title ; Titanium complexes based on chiral enantiopure dialkanolamines: synthesis, structures and catalytic activity ; loop_ _publ_author_name 'Sergey Karlov' 'Maxim V. Bermeshev' 'Andrei Churakov' 'J Howard' 'Juri F. Oprunenko' ; A.A.Samsonov ; 'Kirill V. Zaitsev' 'Galina S. Zaitseva' # Attachment '27new.CIF' data_i _database_code_depnum_ccdc_archive 'CCDC 679771' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H42 N2 O4 Ti, C H2 Cl2' _chemical_formula_sum 'C29 H44 Cl2 N2 O4 Ti' _chemical_formula_weight 603.46 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.162(3) _cell_length_b 10.972(3) _cell_length_c 27.065(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3017.6(16) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5767 _cell_measurement_theta_min 2.396 _cell_measurement_theta_max 28.284 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 0.497 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8859 _exptl_absorpt_correction_T_max 0.9248 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 21553 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 27.99 _reflns_number_total 7219 _reflns_number_gt 6580 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0770P)^2^+0.4746P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(2) _chemical_absolute_configuration ad _refine_ls_number_reflns 7219 _refine_ls_number_parameters 351 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1234 _refine_ls_wR_factor_gt 0.1201 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti 0.62671(4) 0.56308(4) 0.084628(15) 0.00960(10) Uani 1 1 d . . . N1 N 0.8419(2) 0.65287(19) 0.05979(8) 0.0134(4) Uani 1 1 d . . . N2 N 0.5750(2) 0.33878(18) 0.07114(8) 0.0125(4) Uani 1 1 d . . . O11 O 0.63000(18) 0.56012(16) 0.01600(6) 0.0142(3) Uani 1 1 d . . . O12 O 0.6224(2) 0.72066(15) 0.10644(7) 0.0157(4) Uani 1 1 d . . . O21 O 0.73291(18) 0.47573(16) 0.12901(6) 0.0133(4) Uani 1 1 d . . . O22 O 0.45467(17) 0.53979(16) 0.10355(7) 0.0134(4) Uani 1 1 d . . . C1 C 0.8247(3) 0.7847(2) 0.07147(10) 0.0168(5) Uani 1 1 d . . . H1A H 0.7923 0.8278 0.0417 0.020 Uiso 1 1 calc R . . H1B H 0.9110 0.8201 0.0805 0.020 Uiso 1 1 calc R . . C2 C 0.7277(3) 0.8041(2) 0.11390(10) 0.0165(5) Uani 1 1 d . . . C3 C 0.6744(3) 0.9339(3) 0.11211(11) 0.0235(6) Uani 1 1 d . . . H3A H 0.6056 0.9437 0.1372 0.035 Uiso 1 1 calc R . . H3B H 0.6373 0.9500 0.0793 0.035 Uiso 1 1 calc R . . H3C H 0.7460 0.9916 0.1187 0.035 Uiso 1 1 calc R . . C4 C 0.7880(3) 0.7811(3) 0.16473(10) 0.0231(6) Uani 1 1 d . . . H4A H 0.7279 0.8107 0.1904 0.035 Uiso 1 1 calc R . . H4B H 0.8721 0.8243 0.1673 0.035 Uiso 1 1 calc R . . H4C H 0.8027 0.6935 0.1692 0.035 Uiso 1 1 calc R . . C5 C 0.4407(3) 0.3254(2) 0.09167(10) 0.0151(5) Uani 1 1 d . . . H5A H 0.4467 0.2960 0.1262 0.018 Uiso 1 1 calc R . . H5B H 0.3920 0.2637 0.0723 0.018 Uiso 1 1 calc R . . C6 C 0.3647(3) 0.4468(2) 0.09059(9) 0.0148(5) Uani 1 1 d . . . C7 C 0.3070(3) 0.4771(3) 0.03983(10) 0.0187(5) Uani 1 1 d . . . H7A H 0.2551 0.5522 0.0421 0.028 Uiso 1 1 calc R . . H7B H 0.2503 0.4101 0.0289 0.028 Uiso 1 1 calc R . . H7C H 0.3786 0.4885 0.0160 0.028 Uiso 1 1 calc R . . C8 C 0.2549(3) 0.4437(3) 0.12887(10) 0.0205(6) Uani 1 1 d . . . H8A H 0.2099 0.5227 0.1295 0.031 Uiso 1 1 calc R . . H8B H 0.2924 0.4268 0.1615 0.031 Uiso 1 1 calc R . . H8C H 0.1918 0.3796 0.1202 0.031 Uiso 1 1 calc R . . C10 C 0.9617(3) 0.6075(2) 0.08463(11) 0.0190(5) Uani 1 1 d . . . H10A H 1.0396 0.6415 0.0684 0.028 Uiso 1 1 calc R . . H10B H 0.9643 0.5183 0.0826 0.028 Uiso 1 1 calc R . . H10C H 0.9606 0.6325 0.1194 0.028 Uiso 1 1 calc R . . C11 C 0.8486(3) 0.6360(2) 0.00551(9) 0.0142(5) Uani 1 1 d . . . H11A H 0.8997 0.7047 -0.0094 0.017 Uiso 1 1 calc R . . C12 C 0.7046(3) 0.6416(2) -0.01289(9) 0.0136(5) Uani 1 1 d . . . H12A H 0.6706 0.7259 -0.0069 0.016 Uiso 1 1 calc R . . C13 C 0.9107(3) 0.5151(3) -0.00971(10) 0.0206(6) Uani 1 1 d . . . H13A H 1.0020 0.5121 0.0020 0.031 Uiso 1 1 calc R . . H13B H 0.9092 0.5078 -0.0458 0.031 Uiso 1 1 calc R . . H13C H 0.8609 0.4477 0.0049 0.031 Uiso 1 1 calc R . . C14 C 0.6931(3) 0.6152(2) -0.06747(10) 0.0162(5) Uani 1 1 d . . . C15 C 0.7595(3) 0.6883(3) -0.10126(10) 0.0228(6) Uani 1 1 d . . . H15A H 0.8132 0.7534 -0.0898 0.027 Uiso 1 1 calc R . . C16 C 0.7476(4) 0.6669(3) -0.15120(11) 0.0319(7) Uani 1 1 d . . . H16A H 0.7933 0.7174 -0.1740 0.038 Uiso 1 1 calc R . . C17 C 0.6706(4) 0.5735(3) -0.16844(11) 0.0341(8) Uani 1 1 d . . . H17A H 0.6629 0.5600 -0.2030 0.041 Uiso 1 1 calc R . . C18 C 0.6043(3) 0.4991(3) -0.13573(11) 0.0303(7) Uani 1 1 d . . . H18A H 0.5510 0.4343 -0.1476 0.036 Uiso 1 1 calc R . . C19 C 0.6159(3) 0.5195(3) -0.08527(10) 0.0219(5) Uani 1 1 d . . . H19A H 0.5710 0.4679 -0.0627 0.026 Uiso 1 1 calc R . . C20 C 0.5773(3) 0.2932(2) 0.02009(9) 0.0168(5) Uani 1 1 d . . . H20A H 0.5673 0.2044 0.0202 0.025 Uiso 1 1 calc R . . H20B H 0.6613 0.3148 0.0046 0.025 Uiso 1 1 calc R . . H20C H 0.5049 0.3300 0.0014 0.025 Uiso 1 1 calc R . . C21 C 0.6724(3) 0.2746(2) 0.10349(10) 0.0134(5) Uani 1 1 d . . . H21A H 0.6322 0.1971 0.1158 0.016 Uiso 1 1 calc R . . C22 C 0.6951(3) 0.3613(2) 0.14782(9) 0.0128(5) Uani 1 1 d . . . H22A H 0.6098 0.3713 0.1658 0.015 Uiso 1 1 calc R . . C23 C 0.8018(3) 0.2453(2) 0.07776(10) 0.0174(5) Uani 1 1 d . . . H23A H 0.7858 0.1870 0.0510 0.026 Uiso 1 1 calc R . . H23B H 0.8633 0.2098 0.1016 0.026 Uiso 1 1 calc R . . H23C H 0.8395 0.3203 0.0641 0.026 Uiso 1 1 calc R . . C24 C 0.7945(3) 0.3072(2) 0.18320(9) 0.0143(5) Uani 1 1 d . . . C25 C 0.7606(3) 0.2025(3) 0.20868(10) 0.0218(6) Uani 1 1 d . . . H25A H 0.6740 0.1705 0.2059 0.026 Uiso 1 1 calc R . . C26 C 0.8532(3) 0.1432(3) 0.23865(11) 0.0267(7) Uani 1 1 d . . . H26A H 0.8300 0.0704 0.2556 0.032 Uiso 1 1 calc R . . C27 C 0.9776(3) 0.1907(3) 0.24338(10) 0.0252(6) Uani 1 1 d . . . H27A H 1.0407 0.1504 0.2635 0.030 Uiso 1 1 calc R . . C28 C 1.0113(3) 0.2967(3) 0.21907(11) 0.0230(6) Uani 1 1 d . . . H28A H 1.0971 0.3299 0.2228 0.028 Uiso 1 1 calc R . . C29 C 0.9197(3) 0.3547(3) 0.18921(10) 0.0186(5) Uani 1 1 d . . . H29A H 0.9431 0.4280 0.1727 0.022 Uiso 1 1 calc R . . Cl1 Cl 0.86916(11) 0.33040(9) -0.21849(4) 0.0481(2) Uani 1 1 d . . . Cl2 Cl 1.02230(11) 0.53989(9) -0.24948(4) 0.0474(3) Uani 1 1 d . . . C9 C 0.9277(6) 0.4144(4) -0.26908(15) 0.0591(13) Uani 1 1 d . . . H9A H 0.8523 0.4437 -0.2890 0.071 Uiso 1 1 calc R . . H9B H 0.9822 0.3610 -0.2903 0.071 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti 0.0095(2) 0.00824(18) 0.01110(18) -0.00038(15) -0.00043(17) 0.00017(17) N1 0.0122(11) 0.0125(9) 0.0155(10) 0.0025(8) -0.0031(8) 0.0001(8) N2 0.0137(10) 0.0101(9) 0.0137(10) -0.0001(7) -0.0017(8) 0.0010(8) O11 0.0125(8) 0.0172(8) 0.0129(7) 0.0013(7) 0.0008(7) -0.0026(8) O12 0.0154(9) 0.0099(8) 0.0218(9) -0.0027(7) -0.0007(8) -0.0005(8) O21 0.0141(9) 0.0107(8) 0.0153(8) 0.0011(7) -0.0017(7) -0.0013(7) O22 0.0110(9) 0.0126(8) 0.0166(8) -0.0022(7) 0.0010(7) -0.0005(7) C1 0.0183(13) 0.0111(11) 0.0209(13) 0.0030(9) -0.0040(10) -0.0050(10) C2 0.0218(15) 0.0092(11) 0.0185(12) 0.0004(9) -0.0057(11) -0.0023(10) C3 0.0288(15) 0.0123(12) 0.0294(14) 0.0001(11) -0.0044(12) 0.0002(12) C4 0.0257(16) 0.0237(14) 0.0200(13) 0.0003(11) -0.0049(12) -0.0026(12) C5 0.0131(12) 0.0140(11) 0.0183(12) -0.0001(10) 0.0006(10) -0.0021(10) C6 0.0118(11) 0.0149(10) 0.0178(11) 0.0012(9) 0.0012(10) -0.0012(10) C7 0.0142(13) 0.0206(13) 0.0214(13) -0.0008(10) -0.0022(10) 0.0012(11) C8 0.0126(12) 0.0281(14) 0.0207(12) 0.0000(11) 0.0031(10) -0.0025(12) C10 0.0135(12) 0.0198(12) 0.0237(13) 0.0033(11) -0.0043(11) 0.0014(10) C11 0.0117(12) 0.0147(11) 0.0161(11) 0.0030(9) 0.0021(10) -0.0007(10) C12 0.0138(12) 0.0124(11) 0.0146(11) 0.0014(9) 0.0021(10) 0.0019(10) C13 0.0157(14) 0.0226(13) 0.0233(13) 0.0036(11) 0.0038(10) 0.0054(11) C14 0.0158(13) 0.0183(12) 0.0143(11) 0.0010(10) -0.0008(10) 0.0078(10) C15 0.0275(16) 0.0217(13) 0.0193(13) 0.0052(11) 0.0043(12) 0.0043(12) C16 0.0365(19) 0.0393(18) 0.0200(14) 0.0089(13) 0.0067(14) 0.0067(16) C17 0.0403(19) 0.048(2) 0.0137(13) -0.0010(13) 0.0009(12) 0.0141(17) C18 0.0331(19) 0.0372(17) 0.0204(13) -0.0100(12) -0.0074(13) 0.0043(14) C19 0.0221(14) 0.0259(13) 0.0176(12) 0.0007(11) 0.0000(12) 0.0047(12) C20 0.0187(13) 0.0131(12) 0.0185(12) -0.0054(10) -0.0043(11) 0.0005(10) C21 0.0146(12) 0.0104(11) 0.0151(11) -0.0004(9) 0.0000(10) 0.0009(9) C22 0.0118(12) 0.0117(11) 0.0149(11) 0.0001(9) 0.0004(10) 0.0013(9) C23 0.0181(14) 0.0162(12) 0.0179(13) -0.0016(10) 0.0000(11) 0.0033(10) C24 0.0172(13) 0.0126(11) 0.0131(11) -0.0012(9) 0.0011(10) 0.0037(10) C25 0.0220(15) 0.0222(14) 0.0212(13) 0.0046(11) -0.0020(12) -0.0016(12) C26 0.0387(19) 0.0203(13) 0.0211(13) 0.0094(11) -0.0038(13) 0.0008(13) C27 0.0297(17) 0.0288(15) 0.0172(13) -0.0009(11) -0.0131(12) 0.0110(13) C28 0.0217(15) 0.0266(15) 0.0207(13) -0.0024(11) -0.0045(12) 0.0039(12) C29 0.0214(14) 0.0180(12) 0.0163(12) 0.0016(10) -0.0030(11) 0.0012(11) Cl1 0.0542(6) 0.0457(5) 0.0444(5) 0.0109(4) 0.0005(5) -0.0040(5) Cl2 0.0537(6) 0.0419(5) 0.0465(5) 0.0078(4) -0.0175(4) -0.0075(4) C9 0.085(4) 0.050(2) 0.042(2) 0.0132(18) -0.020(2) -0.029(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti O12 1.8274(18) . ? Ti O22 1.8395(19) . ? Ti O11 1.8581(18) . ? Ti O21 1.8779(18) . ? Ti N1 2.491(2) . ? Ti N2 2.543(2) . ? N1 C10 1.477(3) . ? N1 C11 1.482(3) . ? N1 C1 1.490(3) . ? N2 C20 1.470(3) . ? N2 C5 1.480(3) . ? N2 C21 1.497(3) . ? O11 C12 1.409(3) . ? O12 C2 1.423(3) . ? O21 C22 1.408(3) . ? O22 C6 1.414(3) . ? C1 C2 1.528(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.526(4) . ? C2 C4 1.527(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.541(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C8 1.523(3) . ? C6 C7 1.530(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.526(4) . ? C11 C12 1.547(4) . ? C11 H11A 1.0000 . ? C12 C14 1.510(4) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.392(4) . ? C14 C19 1.396(4) . ? C15 C16 1.377(4) . ? C15 H15A 0.9500 . ? C16 C17 1.371(5) . ? C16 H16A 0.9500 . ? C17 C18 1.381(5) . ? C17 H17A 0.9500 . ? C18 C19 1.389(4) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C23 1.522(4) . ? C21 C22 1.548(3) . ? C21 H21A 1.0000 . ? C22 C24 1.513(4) . ? C22 H22A 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.384(4) . ? C24 C29 1.385(4) . ? C25 C26 1.402(4) . ? C25 H25A 0.9500 . ? C26 C27 1.374(5) . ? C26 H26A 0.9500 . ? C27 C28 1.380(4) . ? C27 H27A 0.9500 . ? C28 C29 1.388(4) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? Cl1 C9 1.754(4) . ? Cl2 C9 1.761(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? 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 O12 Ti O22 91.08(9) . . ? O12 Ti O11 109.87(8) . . ? O22 Ti O11 107.04(8) . . ? O12 Ti O21 106.85(8) . . ? O22 Ti O21 107.29(8) . . ? O11 Ti O21 128.34(8) . . ? O12 Ti N1 74.57(8) . . ? O22 Ti N1 164.67(8) . . ? O11 Ti N1 73.82(7) . . ? O21 Ti N1 82.53(8) . . ? O12 Ti N2 163.15(8) . . ? O22 Ti N2 73.09(8) . . ? O11 Ti N2 80.98(7) . . ? O21 Ti N2 73.54(7) . . ? N1 Ti N2 121.70(7) . . ? C10 N1 C11 111.8(2) . . ? C10 N1 C1 109.1(2) . . ? C11 N1 C1 109.66(19) . . ? C10 N1 Ti 117.86(15) . . ? C11 N1 Ti 105.00(15) . . ? C1 N1 Ti 102.92(15) . . ? C20 N2 C5 109.5(2) . . ? C20 N2 C21 112.3(2) . . ? C5 N2 C21 110.04(19) . . ? C20 N2 Ti 117.45(15) . . ? C5 N2 Ti 103.44(14) . . ? C21 N2 Ti 103.57(14) . . ? C12 O11 Ti 123.59(15) . . ? C2 O12 Ti 129.52(17) . . ? C22 O21 Ti 121.98(15) . . ? C6 O22 Ti 130.23(15) . . ? N1 C1 C2 111.7(2) . . ? N1 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? N1 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 107.9 . . ? O12 C2 C3 109.2(2) . . ? O12 C2 C4 108.9(2) . . ? C3 C2 C4 109.0(2) . . ? O12 C2 C1 106.8(2) . . ? C3 C2 C1 109.6(2) . . ? C4 C2 C1 113.3(2) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C6 111.7(2) . . ? N2 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? N2 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 107.9 . . ? O22 C6 C8 108.7(2) . . ? O22 C6 C7 108.3(2) . . ? C8 C6 C7 109.6(2) . . ? O22 C6 C5 107.1(2) . . ? C8 C6 C5 109.6(2) . . ? C7 C6 C5 113.4(2) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C13 113.3(2) . . ? N1 C11 C12 105.7(2) . . ? C13 C11 C12 109.8(2) . . ? N1 C11 H11A 109.3 . . ? C13 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? O11 C12 C14 112.3(2) . . ? O11 C12 C11 107.8(2) . . ? C14 C12 C11 112.4(2) . . ? O11 C12 H12A 108.1 . . ? C14 C12 H12A 108.1 . . ? C11 C12 H12A 108.1 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C19 118.6(3) . . ? C15 C14 C12 119.6(3) . . ? C19 C14 C12 121.7(2) . . ? C16 C15 C14 120.2(3) . . ? C16 C15 H15A 119.9 . . ? C14 C15 H15A 119.9 . . ? C17 C16 C15 120.8(3) . . ? C17 C16 H16A 119.6 . . ? C15 C16 H16A 119.6 . . ? C16 C17 C18 120.2(3) . . ? C16 C17 H17A 119.9 . . ? C18 C17 H17A 119.9 . . ? C17 C18 C19 119.6(3) . . ? C17 C18 H18A 120.2 . . ? C19 C18 H18A 120.2 . . ? C18 C19 C14 120.6(3) . . ? C18 C19 H19A 119.7 . . ? C14 C19 H19A 119.7 . . ? N2 C20 H20A 109.5 . . ? N2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N2 C21 C23 113.7(2) . . ? N2 C21 C22 105.25(19) . . ? C23 C21 C22 110.8(2) . . ? N2 C21 H21A 109.0 . . ? C23 C21 H21A 109.0 . . ? C22 C21 H21A 109.0 . . ? O21 C22 C24 113.4(2) . . ? O21 C22 C21 108.0(2) . . ? C24 C22 C21 110.4(2) . . ? O21 C22 H22A 108.3 . . ? C24 C22 H22A 108.3 . . ? C21 C22 H22A 108.3 . . ? 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 . . ? C25 C24 C29 118.9(3) . . ? C25 C24 C22 118.4(3) . . ? C29 C24 C22 122.6(2) . . ? C24 C25 C26 120.4(3) . . ? C24 C25 H25A 119.8 . . ? C26 C25 H25A 119.8 . . ? C27 C26 C25 119.7(3) . . ? C27 C26 H26A 120.2 . . ? C25 C26 H26A 120.2 . . ? C26 C27 C28 120.3(3) . . ? C26 C27 H27A 119.9 . . ? C28 C27 H27A 119.9 . . ? C27 C28 C29 119.9(3) . . ? C27 C28 H28A 120.1 . . ? C29 C28 H28A 120.1 . . ? C24 C29 C28 120.8(3) . . ? C24 C29 H29A 119.6 . . ? C28 C29 H29A 119.6 . . ? Cl1 C9 Cl2 111.1(2) . . ? Cl1 C9 H9A 109.4 . . ? Cl2 C9 H9A 109.4 . . ? Cl1 C9 H9B 109.4 . . ? Cl2 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.512 _refine_diff_density_min -0.716 _refine_diff_density_rms 0.084 # Attachment '30new.CIF' data_f _database_code_depnum_ccdc_archive 'CCDC 679772' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H50 N2 O4 Ti' _chemical_formula_sum 'C42 H50 N2 O4 Ti' _chemical_formula_weight 694.74 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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.096(2) _cell_length_b 12.761(2) _cell_length_c 26.595(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3766.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5397 _cell_measurement_theta_min 2.205 _cell_measurement_theta_max 25.771 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.225 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 0.270 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9355 _exptl_absorpt_correction_T_max 0.9530 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 24191 _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_sigmaI/netI 0.0698 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 27.99 _reflns_number_total 9038 _reflns_number_gt 7506 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0498P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(2) _chemical_absolute_configuration ad _refine_ls_number_reflns 9038 _refine_ls_number_parameters 446 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0638 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1058 _refine_ls_wR_factor_gt 0.1018 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 Ti Ti 0.56234(4) 0.51144(3) 0.886988(16) 0.01843(10) Uani 1 1 d . . . N1 N 0.74647(17) 0.47723(15) 0.93054(7) 0.0228(4) Uani 1 1 d . . . N2 N 0.51026(18) 0.61117(15) 0.80975(8) 0.0246(5) Uani 1 1 d . . . O11 O 0.40604(14) 0.47254(11) 0.86828(6) 0.0206(3) Uani 1 1 d . . . O12 O 0.59116(15) 0.65038(11) 0.90091(6) 0.0245(4) Uani 1 1 d . . . O21 O 0.52018(14) 0.45658(12) 0.95002(6) 0.0216(4) Uani 1 1 d . . . O22 O 0.65554(16) 0.43496(13) 0.84282(6) 0.0291(4) Uani 1 1 d . . . C11 C 0.3260(2) 0.51090(18) 0.83232(8) 0.0202(5) Uani 1 1 d . . . C12 C 0.4013(2) 0.55852(19) 0.78855(9) 0.0253(6) Uani 1 1 d . . . H12A H 0.3517 0.6094 0.7688 0.030 Uiso 1 1 calc R . . C13 C 0.4576(2) 0.4761(2) 0.75369(10) 0.0343(6) Uani 1 1 d . . . H13A H 0.4853 0.4144 0.7730 0.041 Uiso 1 1 calc R . . H13B H 0.3991 0.4528 0.7279 0.041 Uiso 1 1 calc R . . C14 C 0.5632(3) 0.5328(3) 0.72965(11) 0.0506(8) Uani 1 1 d . . . H14A H 0.5380 0.5689 0.6984 0.061 Uiso 1 1 calc R . . H14B H 0.6290 0.4832 0.7215 0.061 Uiso 1 1 calc R . . C15 C 0.6038(3) 0.6119(2) 0.76941(10) 0.0346(7) Uani 1 1 d . . . H15A H 0.6832 0.5917 0.7833 0.041 Uiso 1 1 calc R . . H15B H 0.6108 0.6828 0.7545 0.041 Uiso 1 1 calc R . . C16 C 0.4850(2) 0.71650(18) 0.83041(10) 0.0266(6) Uani 1 1 d . . . H16A H 0.4020 0.7185 0.8440 0.032 Uiso 1 1 calc R . . H16B H 0.4909 0.7693 0.8032 0.032 Uiso 1 1 calc R . . C17 C 0.5749(2) 0.74323(17) 0.87221(9) 0.0269(5) Uani 1 1 d . . . C18 C 0.6955(3) 0.7823(2) 0.85367(11) 0.0367(7) Uani 1 1 d . . . H18A H 0.7329 0.7288 0.8324 0.055 Uiso 1 1 calc R . . H18B H 0.7479 0.7969 0.8825 0.055 Uiso 1 1 calc R . . H18C H 0.6839 0.8467 0.8341 0.055 Uiso 1 1 calc R . . C19 C 0.5172(3) 0.8261(2) 0.90697(11) 0.0372(7) Uani 1 1 d . . . H19A H 0.5736 0.8438 0.9341 0.056 Uiso 1 1 calc R . . H19B H 0.4428 0.7979 0.9214 0.056 Uiso 1 1 calc R . . H19C H 0.4988 0.8892 0.8875 0.056 Uiso 1 1 calc R . . C21 C 0.5888(2) 0.42143(17) 0.99091(9) 0.0205(5) Uani 1 1 d . . . C22 C 0.7165(2) 0.47069(18) 0.98530(9) 0.0221(5) Uani 1 1 d . . . H22A H 0.7779 0.4277 1.0035 0.026 Uiso 1 1 calc R . . C23 C 0.7232(2) 0.58540(18) 1.00203(10) 0.0255(6) Uani 1 1 d . . . H23A H 0.6472 0.6227 0.9942 0.031 Uiso 1 1 calc R . . H23B H 0.7390 0.5906 1.0386 0.031 Uiso 1 1 calc R . . C24 C 0.8280(2) 0.6305(2) 0.97180(10) 0.0307(6) Uani 1 1 d . . . H24A H 0.8113 0.7040 0.9622 0.037 Uiso 1 1 calc R . . H24B H 0.9033 0.6284 0.9917 0.037 Uiso 1 1 calc R . . C25 C 0.8392(2) 0.56161(19) 0.92515(10) 0.0288(6) Uani 1 1 d . . . H25A H 0.8242 0.6032 0.8944 0.035 Uiso 1 1 calc R . . H25B H 0.9209 0.5308 0.9230 0.035 Uiso 1 1 calc R . . C26 C 0.7861(2) 0.37650(19) 0.90802(10) 0.0287(6) Uani 1 1 d . . . H26A H 0.7411 0.3178 0.9236 0.034 Uiso 1 1 calc R . . H26B H 0.8730 0.3657 0.9146 0.034 Uiso 1 1 calc R . . C27 C 0.7634(2) 0.3778(2) 0.85115(10) 0.0305(6) Uani 1 1 d . . . C28 C 0.8650(3) 0.4276(3) 0.82104(12) 0.0441(8) Uani 1 1 d . . . H28A H 0.8456 0.4246 0.7851 0.066 Uiso 1 1 calc R . . H28B H 0.9401 0.3894 0.8273 0.066 Uiso 1 1 calc R . . H28C H 0.8748 0.5008 0.8313 0.066 Uiso 1 1 calc R . . C29 C 0.7439(3) 0.2647(2) 0.83271(12) 0.0492(8) Uani 1 1 d . . . H29A H 0.7246 0.2653 0.7968 0.074 Uiso 1 1 calc R . . H29B H 0.6771 0.2328 0.8514 0.074 Uiso 1 1 calc R . . H29C H 0.8175 0.2238 0.8383 0.074 Uiso 1 1 calc R . . C31 C 0.5889(2) 0.30031(18) 0.99185(9) 0.0205(5) Uani 1 1 d . . . C32 C 0.6538(2) 0.24410(19) 1.02753(10) 0.0286(6) Uani 1 1 d . . . H32A H 0.7029 0.2811 1.0508 0.034 Uiso 1 1 calc R . . C33 C 0.6492(3) 0.13614(19) 1.03021(11) 0.0344(7) Uani 1 1 d . . . H33A H 0.6933 0.0997 1.0553 0.041 Uiso 1 1 calc R . . C34 C 0.5793(3) 0.0815(2) 0.99579(11) 0.0360(7) Uani 1 1 d . . . H34A H 0.5760 0.0072 0.9970 0.043 Uiso 1 1 calc R . . C35 C 0.5143(2) 0.1355(2) 0.95955(11) 0.0340(7) Uani 1 1 d . . . H35A H 0.4672 0.0981 0.9357 0.041 Uiso 1 1 calc R . . C36 C 0.5179(2) 0.24423(19) 0.95805(10) 0.0262(6) Uani 1 1 d . . . H36A H 0.4714 0.2808 0.9337 0.031 Uiso 1 1 calc R . . C41 C 0.5269(2) 0.45415(17) 1.04034(9) 0.0218(5) Uani 1 1 d . . . C42 C 0.4021(2) 0.46851(18) 1.04017(9) 0.0258(5) Uani 1 1 d . . . H42A H 0.3587 0.4629 1.0095 0.031 Uiso 1 1 calc R . . C43 C 0.3410(2) 0.4909(2) 1.08422(10) 0.0329(6) Uani 1 1 d . . . H43A H 0.2561 0.5001 1.0834 0.039 Uiso 1 1 calc R . . C44 C 0.4015(2) 0.50004(19) 1.12935(9) 0.0316(6) Uani 1 1 d . . . H44A H 0.3587 0.5156 1.1594 0.038 Uiso 1 1 calc R . . C45 C 0.5245(2) 0.48642(19) 1.13047(9) 0.0295(6) Uani 1 1 d . . . H45A H 0.5670 0.4929 1.1613 0.035 Uiso 1 1 calc R . . C46 C 0.5864(2) 0.46315(18) 1.08638(9) 0.0252(5) Uani 1 1 d . . . H46A H 0.6712 0.4532 1.0876 0.030 Uiso 1 1 calc R . . C51 C 0.2499(2) 0.41872(18) 0.81212(9) 0.0224(5) Uani 1 1 d . . . C52 C 0.1752(2) 0.4292(2) 0.77009(10) 0.0294(6) Uani 1 1 d . . . H52A H 0.1691 0.4950 0.7535 0.035 Uiso 1 1 calc R . . C53 C 0.1101(2) 0.3442(2) 0.75256(10) 0.0316(6) Uani 1 1 d . . . H53A H 0.0600 0.3521 0.7238 0.038 Uiso 1 1 calc R . . C54 C 0.1171(2) 0.2485(2) 0.77623(11) 0.0365(7) Uani 1 1 d . . . H54A H 0.0723 0.1903 0.7640 0.044 Uiso 1 1 calc R . . C55 C 0.1898(3) 0.2381(2) 0.81781(11) 0.0361(7) Uani 1 1 d . . . H55A H 0.1945 0.1726 0.8346 0.043 Uiso 1 1 calc R . . C56 C 0.2562(2) 0.32231(19) 0.83549(10) 0.0277(6) Uani 1 1 d . . . H56A H 0.3067 0.3136 0.8640 0.033 Uiso 1 1 calc R . . C61 C 0.2403(2) 0.59097(17) 0.85773(9) 0.0206(5) Uani 1 1 d . . . C62 C 0.1573(3) 0.6500(2) 0.83120(10) 0.0338(6) Uani 1 1 d . . . H62A H 0.1519 0.6426 0.7957 0.041 Uiso 1 1 calc R . . C63 C 0.0818(3) 0.7200(2) 0.85579(11) 0.0393(7) Uani 1 1 d . . . H63A H 0.0246 0.7591 0.8369 0.047 Uiso 1 1 calc R . . C64 C 0.0884(2) 0.73392(19) 0.90748(11) 0.0327(6) Uani 1 1 d . . . H64A H 0.0374 0.7827 0.9241 0.039 Uiso 1 1 calc R . . C65 C 0.1708(2) 0.67538(18) 0.93420(10) 0.0282(6) Uani 1 1 d . . . H65A H 0.1761 0.6834 0.9696 0.034 Uiso 1 1 calc R . . C66 C 0.2461(2) 0.60463(18) 0.90990(9) 0.0220(5) Uani 1 1 d . . . H66A H 0.3024 0.5650 0.9290 0.026 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti 0.0202(2) 0.01600(18) 0.0191(2) -0.00141(16) 0.00196(18) -0.00130(16) N1 0.0200(10) 0.0224(10) 0.0261(11) -0.0023(9) 0.0036(9) 0.0003(8) N2 0.0285(11) 0.0241(10) 0.0213(11) -0.0010(9) 0.0023(9) -0.0084(9) O11 0.0219(8) 0.0200(8) 0.0200(8) 0.0018(6) -0.0019(7) -0.0020(7) O12 0.0337(10) 0.0175(8) 0.0222(9) 0.0016(6) -0.0004(7) -0.0047(7) O21 0.0192(8) 0.0227(8) 0.0227(9) 0.0024(7) -0.0007(7) -0.0007(6) O22 0.0247(9) 0.0358(10) 0.0269(10) -0.0080(8) 0.0048(8) 0.0055(8) C11 0.0234(11) 0.0210(11) 0.0163(11) 0.0012(10) 0.0008(9) -0.0032(10) C12 0.0289(14) 0.0287(13) 0.0182(13) 0.0024(10) -0.0003(11) -0.0093(11) C13 0.0361(15) 0.0422(15) 0.0245(13) -0.0108(12) 0.0093(12) -0.0121(13) C14 0.0489(18) 0.069(2) 0.0338(16) -0.0158(15) 0.0204(15) -0.0229(18) C15 0.0398(16) 0.0415(16) 0.0224(14) 0.0035(12) 0.0080(12) -0.0126(13) C16 0.0328(14) 0.0193(12) 0.0279(14) 0.0072(10) -0.0013(12) -0.0042(10) C17 0.0329(14) 0.0197(11) 0.0281(14) 0.0036(9) -0.0041(11) -0.0062(11) C18 0.0388(16) 0.0339(15) 0.0374(17) 0.0084(13) -0.0075(14) -0.0130(12) C19 0.0508(18) 0.0217(13) 0.0392(17) -0.0063(11) -0.0100(14) -0.0003(12) C21 0.0210(13) 0.0220(12) 0.0186(12) 0.0031(9) -0.0015(10) 0.0002(10) C22 0.0228(12) 0.0225(12) 0.0210(13) -0.0002(9) -0.0050(10) 0.0023(10) C23 0.0261(14) 0.0272(12) 0.0233(14) -0.0010(10) -0.0043(11) -0.0051(11) C24 0.0269(14) 0.0316(14) 0.0335(16) -0.0036(12) -0.0020(12) -0.0068(11) C25 0.0193(13) 0.0307(14) 0.0366(16) -0.0011(11) 0.0042(12) -0.0024(11) C26 0.0257(14) 0.0235(12) 0.0368(16) -0.0046(11) 0.0084(12) 0.0051(11) C27 0.0246(14) 0.0344(14) 0.0324(16) -0.0045(12) 0.0085(12) 0.0053(12) C28 0.0298(16) 0.062(2) 0.0409(18) -0.0034(15) 0.0169(14) 0.0049(15) C29 0.063(2) 0.0367(16) 0.048(2) -0.0153(14) 0.0068(17) 0.0059(16) C31 0.0190(12) 0.0234(11) 0.0193(12) -0.0009(9) 0.0030(10) 0.0029(9) C32 0.0374(15) 0.0225(12) 0.0258(14) -0.0002(11) -0.0007(12) 0.0044(11) C33 0.0463(17) 0.0254(14) 0.0314(16) 0.0073(12) 0.0103(14) 0.0093(12) C34 0.0408(17) 0.0219(13) 0.0453(18) -0.0013(12) 0.0189(15) 0.0016(12) C35 0.0332(15) 0.0274(14) 0.0415(18) -0.0113(12) 0.0085(13) -0.0062(11) C36 0.0260(13) 0.0265(13) 0.0261(14) -0.0008(11) 0.0048(11) 0.0002(11) C41 0.0271(13) 0.0147(11) 0.0237(13) 0.0000(9) -0.0013(10) -0.0011(9) C42 0.0272(13) 0.0273(13) 0.0228(13) -0.0044(10) -0.0033(11) 0.0040(10) C43 0.0265(12) 0.0369(15) 0.0352(15) -0.0025(13) 0.0028(12) 0.0082(12) C44 0.0404(15) 0.0294(14) 0.0250(13) -0.0033(11) 0.0053(11) 0.0095(12) C45 0.0432(15) 0.0227(12) 0.0227(13) -0.0016(10) -0.0057(11) 0.0070(11) C46 0.0253(13) 0.0240(12) 0.0264(13) 0.0020(10) -0.0054(11) 0.0053(10) C51 0.0253(13) 0.0243(12) 0.0176(12) -0.0013(10) 0.0024(11) -0.0040(10) C52 0.0300(15) 0.0309(14) 0.0271(14) -0.0036(11) 0.0007(12) -0.0038(11) C53 0.0290(14) 0.0429(16) 0.0228(14) -0.0101(12) -0.0020(11) -0.0069(12) C54 0.0316(15) 0.0405(16) 0.0375(17) -0.0171(13) 0.0073(13) -0.0135(13) C55 0.0450(17) 0.0267(14) 0.0364(17) -0.0010(12) 0.0041(14) -0.0105(12) C56 0.0307(14) 0.0268(13) 0.0257(14) -0.0021(11) 0.0015(12) -0.0068(11) C61 0.0241(13) 0.0163(11) 0.0213(13) 0.0004(9) -0.0066(10) -0.0020(9) C62 0.0408(16) 0.0334(15) 0.0271(15) -0.0049(12) -0.0135(13) 0.0043(13) C63 0.0433(18) 0.0343(15) 0.0404(17) -0.0026(12) -0.0160(15) 0.0078(13) C64 0.0316(15) 0.0240(13) 0.0426(16) -0.0046(11) 0.0013(13) 0.0040(11) C65 0.0364(15) 0.0213(12) 0.0270(14) -0.0024(10) 0.0087(12) -0.0041(11) C66 0.0262(13) 0.0191(12) 0.0207(13) 0.0035(10) -0.0028(11) -0.0038(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti O12 1.8393(16) . ? Ti O22 1.8444(17) . ? Ti O11 1.8714(16) . ? Ti O21 1.8758(17) . ? Ti N1 2.389(2) . ? Ti N2 2.485(2) . ? N1 C26 1.485(3) . ? N1 C22 1.496(3) . ? N1 C25 1.496(3) . ? N2 C16 1.479(3) . ? N2 C12 1.494(3) . ? N2 C15 1.493(3) . ? O11 C11 1.394(3) . ? O12 C17 1.421(3) . ? O21 C21 1.402(3) . ? O22 C27 1.419(3) . ? C11 C51 1.544(3) . ? C11 C61 1.551(3) . ? C11 C12 1.556(3) . ? C12 C13 1.535(3) . ? C12 H12A 1.0000 . ? C13 C14 1.519(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.530(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.532(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.510(4) . ? C17 C19 1.544(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C21 C41 1.541(3) . ? C21 C31 1.546(3) . ? C21 C22 1.557(3) . ? C22 C23 1.532(3) . ? C22 H22A 1.0000 . ? C23 C24 1.526(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.526(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.534(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.523(4) . ? C27 C29 1.540(4) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C31 C32 1.391(3) . ? C31 C36 1.393(3) . ? C32 C33 1.380(3) . ? C32 H32A 0.9500 . ? C33 C34 1.388(4) . ? C33 H33A 0.9500 . ? C34 C35 1.387(4) . ? C34 H34A 0.9500 . ? C35 C36 1.388(3) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C41 C46 1.396(3) . ? C41 C42 1.397(3) . ? C42 C43 1.383(3) . ? C42 H42A 0.9500 . ? C43 C44 1.380(4) . ? C43 H43A 0.9500 . ? C44 C45 1.376(4) . ? C44 H44A 0.9500 . ? C45 C46 1.392(3) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C51 C56 1.380(3) . ? C51 C52 1.398(3) . ? C52 C53 1.384(3) . ? C52 H52A 0.9500 . ? C53 C54 1.377(4) . ? C53 H53A 0.9500 . ? C54 C55 1.375(4) . ? C54 H54A 0.9500 . ? C55 C56 1.385(4) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? C61 C62 1.383(3) . ? C61 C66 1.400(3) . ? C62 C63 1.388(4) . ? C62 H62A 0.9500 . ? C63 C64 1.388(4) . ? C63 H63A 0.9500 . ? C64 C65 1.378(4) . ? C64 H64A 0.9500 . ? C65 C66 1.390(3) . ? C65 H65A 0.9500 . ? C66 H66A 0.9500 . ? 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 O12 Ti O22 122.74(8) . . ? O12 Ti O11 118.06(7) . . ? O22 Ti O11 102.12(8) . . ? O12 Ti O21 102.89(7) . . ? O22 Ti O21 120.77(8) . . ? O11 Ti O21 84.69(7) . . ? O12 Ti N1 85.98(7) . . ? O22 Ti N1 74.49(7) . . ? O11 Ti N1 150.83(7) . . ? O21 Ti N1 73.25(7) . . ? O12 Ti N2 73.33(7) . . ? O22 Ti N2 82.81(8) . . ? O11 Ti N2 72.57(6) . . ? O21 Ti N2 150.69(7) . . ? N1 Ti N2 133.90(7) . . ? C26 N1 C22 114.22(19) . . ? C26 N1 C25 112.38(19) . . ? C22 N1 C25 106.63(18) . . ? C26 N1 Ti 102.47(15) . . ? C22 N1 Ti 106.99(13) . . ? C25 N1 Ti 114.22(15) . . ? C16 N2 C12 113.3(2) . . ? C16 N2 C15 113.11(19) . . ? C12 N2 C15 107.15(19) . . ? C16 N2 Ti 101.68(14) . . ? C12 N2 Ti 105.65(14) . . ? C15 N2 Ti 115.83(16) . . ? C11 O11 Ti 132.83(13) . . ? C17 O12 Ti 132.35(14) . . ? C21 O21 Ti 132.64(14) . . ? C27 O22 Ti 130.21(16) . . ? O11 C11 C51 108.63(18) . . ? O11 C11 C61 108.85(18) . . ? C51 C11 C61 108.54(19) . . ? O11 C11 C12 107.97(18) . . ? C51 C11 C12 109.31(18) . . ? C61 C11 C12 113.44(19) . . ? N2 C12 C13 101.9(2) . . ? N2 C12 C11 109.14(19) . . ? C13 C12 C11 113.8(2) . . ? N2 C12 H12A 110.6 . . ? C13 C12 H12A 110.6 . . ? C11 C12 H12A 110.6 . . ? C14 C13 C12 104.0(2) . . ? C14 C13 H13A 110.9 . . ? C12 C13 H13A 110.9 . . ? C14 C13 H13B 110.9 . . ? C12 C13 H13B 110.9 . . ? H13A C13 H13B 109.0 . . ? C13 C14 C15 104.5(2) . . ? C13 C14 H14A 110.8 . . ? C15 C14 H14A 110.9 . . ? C13 C14 H14B 110.9 . . ? C15 C14 H14B 110.9 . . ? H14A C14 H14B 108.9 . . ? N2 C15 C14 106.7(2) . . ? N2 C15 H15A 110.4 . . ? C14 C15 H15A 110.4 . . ? N2 C15 H15B 110.4 . . ? C14 C15 H15B 110.4 . . ? H15A C15 H15B 108.6 . . ? N2 C16 C17 110.4(2) . . ? N2 C16 H16A 109.6 . . ? C17 C16 H16A 109.6 . . ? N2 C16 H16B 109.6 . . ? C17 C16 H16B 109.6 . . ? H16A C16 H16B 108.1 . . ? O12 C17 C18 109.8(2) . . ? O12 C17 C16 106.66(18) . . ? C18 C17 C16 114.4(2) . . ? O12 C17 C19 107.6(2) . . ? C18 C17 C19 109.7(2) . . ? C16 C17 C19 108.5(2) . . ? 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 . . ? O21 C21 C41 109.44(18) . . ? O21 C21 C31 109.45(18) . . ? C41 C21 C31 104.92(18) . . ? O21 C21 C22 106.91(18) . . ? C41 C21 C22 112.21(19) . . ? C31 C21 C22 113.87(19) . . ? N1 C22 C23 102.64(18) . . ? N1 C22 C21 108.54(18) . . ? C23 C22 C21 113.7(2) . . ? N1 C22 H22A 110.6 . . ? C23 C22 H22A 110.6 . . ? C21 C22 H22A 110.6 . . ? C24 C23 C22 104.1(2) . . ? C24 C23 H23A 110.9 . . ? C22 C23 H23A 110.9 . . ? C24 C23 H23B 110.9 . . ? C22 C23 H23B 110.9 . . ? H23A C23 H23B 109.0 . . ? C25 C24 C23 105.9(2) . . ? C25 C24 H24A 110.6 . . ? C23 C24 H24A 110.6 . . ? C25 C24 H24B 110.6 . . ? C23 C24 H24B 110.6 . . ? H24A C24 H24B 108.7 . . ? N1 C25 C24 106.28(19) . . ? N1 C25 H25A 110.5 . . ? C24 C25 H25A 110.5 . . ? N1 C25 H25B 110.5 . . ? C24 C25 H25B 110.5 . . ? H25A C25 H25B 108.7 . . ? N1 C26 C27 109.9(2) . . ? N1 C26 H26A 109.7 . . ? C27 C26 H26A 109.7 . . ? N1 C26 H26B 109.7 . . ? C27 C26 H26B 109.7 . . ? H26A C26 H26B 108.2 . . ? O22 C27 C28 109.1(2) . . ? O22 C27 C29 108.3(2) . . ? C28 C27 C29 109.2(2) . . ? O22 C27 C26 107.3(2) . . ? C28 C27 C26 113.7(2) . . ? C29 C27 C26 109.1(2) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C32 C31 C36 117.9(2) . . ? C32 C31 C21 121.8(2) . . ? C36 C31 C21 120.2(2) . . ? C33 C32 C31 122.1(3) . . ? C33 C32 H32A 119.0 . . ? C31 C32 H32A 119.0 . . ? C32 C33 C34 119.2(3) . . ? C32 C33 H33A 120.4 . . ? C34 C33 H33A 120.4 . . ? C33 C34 C35 120.0(2) . . ? C33 C34 H34A 120.0 . . ? C35 C34 H34A 120.0 . . ? C34 C35 C36 120.1(3) . . ? C34 C35 H35A 120.0 . . ? C36 C35 H35A 120.0 . . ? C35 C36 C31 120.7(3) . . ? C35 C36 H36A 119.6 . . ? C31 C36 H36A 119.6 . . ? C46 C41 C42 117.5(2) . . ? C46 C41 C21 124.0(2) . . ? C42 C41 C21 118.4(2) . . ? C43 C42 C41 120.7(2) . . ? C43 C42 H42A 119.7 . . ? C41 C42 H42A 119.7 . . ? C44 C43 C42 121.1(2) . . ? C44 C43 H43A 119.5 . . ? C42 C43 H43A 119.5 . . ? C45 C44 C43 119.4(2) . . ? C45 C44 H44A 120.3 . . ? C43 C44 H44A 120.3 . . ? C44 C45 C46 119.9(2) . . ? C44 C45 H45A 120.0 . . ? C46 C45 H45A 120.0 . . ? C45 C46 C41 121.5(2) . . ? C45 C46 H46A 119.2 . . ? C41 C46 H46A 119.2 . . ? C56 C51 C52 118.4(2) . . ? C56 C51 C11 119.7(2) . . ? C52 C51 C11 121.9(2) . . ? C53 C52 C51 120.2(2) . . ? C53 C52 H52A 119.9 . . ? C51 C52 H52A 119.9 . . ? C54 C53 C52 120.8(3) . . ? C54 C53 H53A 119.6 . . ? C52 C53 H53A 119.6 . . ? C55 C54 C53 119.1(2) . . ? C55 C54 H54A 120.5 . . ? C53 C54 H54A 120.5 . . ? C54 C55 C56 120.7(3) . . ? C54 C55 H55A 119.6 . . ? C56 C55 H55A 119.6 . . ? C55 C56 C51 120.8(2) . . ? C55 C56 H56A 119.6 . . ? C51 C56 H56A 119.6 . . ? C62 C61 C66 118.0(2) . . ? C62 C61 C11 123.0(2) . . ? C66 C61 C11 119.0(2) . . ? C63 C62 C61 120.8(3) . . ? C63 C62 H62A 119.6 . . ? C61 C62 H62A 119.6 . . ? C62 C63 C64 121.1(3) . . ? C62 C63 H63A 119.5 . . ? C64 C63 H63A 119.5 . . ? C65 C64 C63 118.5(3) . . ? C65 C64 H64A 120.8 . . ? C63 C64 H64A 120.8 . . ? C64 C65 C66 120.8(3) . . ? C64 C65 H65A 119.6 . . ? C66 C65 H65A 119.6 . . ? C65 C66 C61 120.9(2) . . ? C65 C66 H66A 119.6 . . ? C61 C66 H66A 119.6 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.472 _refine_diff_density_min -0.922 _refine_diff_density_rms 0.059 # Attachment '23.CIF' data_r _database_code_depnum_ccdc_archive 'CCDC 683792' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H39 N O4 Ti' _chemical_formula_sum 'C27 H39 N O4 Ti' _chemical_formula_weight 489.49 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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.8754(8) _cell_length_b 14.0332(11) _cell_length_c 17.5810(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2683.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6611 _cell_measurement_theta_min 2.201 _cell_measurement_theta_max 26.461 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.212 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 0.350 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9334 _exptl_absorpt_correction_T_max 0.9494 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 17527 _diffrn_reflns_av_R_equivalents 0.0594 _diffrn_reflns_av_sigmaI/netI 0.0809 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 28.00 _reflns_number_total 6473 _reflns_number_gt 4886 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0239P)^2^+1.2334P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(3) _refine_ls_number_reflns 6473 _refine_ls_number_parameters 304 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0877 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.0953 _refine_ls_wR_factor_gt 0.0875 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _chemical_absolute_configuration ad loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.92373(4) -0.00157(4) 0.86217(3) 0.01805(10) Uani 1 1 d . . . N1 N 0.7413(2) 0.07369(15) 0.89390(13) 0.0165(5) Uani 1 1 d . . . O1 O 0.8670(2) 0.04266(14) 0.77028(12) 0.0297(5) Uani 1 1 d . . . O2 O 0.96876(17) 0.07972(13) 0.94162(11) 0.0193(4) Uani 1 1 d . . . O3 O 0.8573(2) -0.11445(13) 0.89286(12) 0.0252(5) Uani 1 1 d . . . O4 O 1.0758(2) -0.03809(13) 0.83660(11) 0.0256(4) Uani 1 1 d . . . C1 C 0.7621(3) 0.1015(2) 0.75550(17) 0.0217(7) Uani 1 1 d . . . C2 C 0.7236(3) 0.14330(19) 0.83201(16) 0.0185(6) Uani 1 1 d . . . H2A H 0.7730 0.2011 0.8426 0.022 Uiso 1 1 calc R . . H2B H 0.6360 0.1623 0.8298 0.022 Uiso 1 1 calc R . . C3 C 0.6612(3) 0.0418(2) 0.71856(19) 0.0369(9) Uani 1 1 d . . . H3A H 0.6442 -0.0141 0.7502 0.055 Uiso 1 1 calc R . . H3B H 0.6883 0.0210 0.6680 0.055 Uiso 1 1 calc R . . H3C H 0.5864 0.0802 0.7137 0.055 Uiso 1 1 calc R . . C4 C 0.8020(3) 0.1804(2) 0.70159(18) 0.0298(8) Uani 1 1 d . . . H4A H 0.8699 0.2162 0.7244 0.045 Uiso 1 1 calc R . . H4B H 0.7326 0.2234 0.6923 0.045 Uiso 1 1 calc R . . H4C H 0.8290 0.1524 0.6533 0.045 Uiso 1 1 calc R . . C5 C 1.2048(3) -0.0470(2) 0.8302(2) 0.0289(7) Uani 1 1 d . . . H5A H 1.2231 -0.0984 0.7924 0.035 Uiso 1 1 calc R . . C6 C 1.2581(4) -0.0761(3) 0.9060(2) 0.0522(11) Uani 1 1 d . . . H6A H 1.2180 -0.1347 0.9234 0.078 Uiso 1 1 calc R . . H6B H 1.2442 -0.0252 0.9432 0.078 Uiso 1 1 calc R . . H6C H 1.3466 -0.0872 0.9005 0.078 Uiso 1 1 calc R . . C7 C 1.2586(3) 0.0456(2) 0.8007(2) 0.0397(9) Uani 1 1 d . . . H7A H 1.2214 0.0612 0.7515 0.060 Uiso 1 1 calc R . . H7B H 1.3477 0.0386 0.7946 0.060 Uiso 1 1 calc R . . H7C H 1.2414 0.0969 0.8370 0.060 Uiso 1 1 calc R . . C8 C 0.9128(3) -0.20299(19) 0.9145(2) 0.0339(8) Uani 1 1 d . . . H8A H 0.9930 -0.2099 0.8873 0.041 Uiso 1 1 calc R . . C9 C 0.9360(4) -0.2028(3) 0.9990(2) 0.0523(11) Uani 1 1 d . . . H9A H 0.9893 -0.1489 1.0122 0.079 Uiso 1 1 calc R . . H9B H 0.9763 -0.2625 1.0137 0.079 Uiso 1 1 calc R . . H9C H 0.8577 -0.1968 1.0261 0.079 Uiso 1 1 calc R . . C10 C 0.8282(5) -0.2833(2) 0.8906(3) 0.0669(15) Uani 1 1 d . . . H10A H 0.8182 -0.2824 0.8352 0.100 Uiso 1 1 calc R . . H10B H 0.7479 -0.2752 0.9149 0.100 Uiso 1 1 calc R . . H10C H 0.8639 -0.3444 0.9061 0.100 Uiso 1 1 calc R . . C11 C 0.8975(2) 0.15148(18) 0.97620(16) 0.0166(6) Uani 1 1 d . . . C12 C 0.7611(3) 0.11756(19) 0.97032(16) 0.0163(6) Uani 1 1 d . . . H12A H 0.7034 0.1720 0.9785 0.020 Uiso 1 1 calc R . . C13 C 0.7327(3) 0.03593(19) 1.02512(17) 0.0202(6) Uani 1 1 d . . . H13A H 0.7008 0.0609 1.0740 0.024 Uiso 1 1 calc R . . H13B H 0.8075 -0.0022 1.0353 0.024 Uiso 1 1 calc R . . C14 C 0.6347(3) -0.0249(2) 0.98492(17) 0.0269(7) Uani 1 1 d . . . H14A H 0.6569 -0.0933 0.9870 0.032 Uiso 1 1 calc R . . H14B H 0.5534 -0.0161 1.0092 0.032 Uiso 1 1 calc R . . C15 C 0.6322(3) 0.0099(2) 0.90325(16) 0.0230(6) Uani 1 1 d . . . H15A H 0.6372 -0.0446 0.8676 0.028 Uiso 1 1 calc R . . H15B H 0.5553 0.0454 0.8930 0.028 Uiso 1 1 calc R . . C16 C 0.9352(3) 0.15959(18) 1.06049(16) 0.0174(6) Uani 1 1 d . . . C17 C 1.0416(3) 0.1158(2) 1.08598(17) 0.0220(7) Uani 1 1 d . . . H17A H 1.0913 0.0812 1.0512 0.026 Uiso 1 1 calc R . . C18 C 1.0763(3) 0.1218(2) 1.16175(17) 0.0268(7) Uani 1 1 d . . . H18A H 1.1497 0.0914 1.1782 0.032 Uiso 1 1 calc R . . C19 C 1.0056(3) 0.1713(2) 1.21339(18) 0.0243(7) Uani 1 1 d . . . H19A H 1.0293 0.1746 1.2653 0.029 Uiso 1 1 calc R . . C20 C 0.8998(3) 0.2159(2) 1.18851(16) 0.0243(7) Uani 1 1 d . . . H20A H 0.8507 0.2507 1.2235 0.029 Uiso 1 1 calc R . . C21 C 0.8651(3) 0.2103(2) 1.11315(16) 0.0246(7) Uani 1 1 d . . . H21A H 0.7922 0.2415 1.0969 0.030 Uiso 1 1 calc R . . C22 C 0.9227(3) 0.24763(18) 0.93659(15) 0.0172(5) Uani 1 1 d . . . C23 C 0.8544(3) 0.32893(19) 0.95257(17) 0.0198(6) Uani 1 1 d . . . H23A H 0.7935 0.3267 0.9913 0.024 Uiso 1 1 calc R . . C24 C 0.8733(3) 0.4132(2) 0.91316(17) 0.0231(7) Uani 1 1 d . . . H24A H 0.8254 0.4678 0.9251 0.028 Uiso 1 1 calc R . . C25 C 0.9616(3) 0.4184(2) 0.85650(18) 0.0237(6) Uani 1 1 d . . . H25A H 0.9741 0.4759 0.8290 0.028 Uiso 1 1 calc R . . C26 C 1.0311(3) 0.3387(2) 0.84088(17) 0.0253(7) Uani 1 1 d . . . H26A H 1.0925 0.3415 0.8025 0.030 Uiso 1 1 calc R . . C27 C 1.0125(3) 0.2547(2) 0.88029(17) 0.0223(7) Uani 1 1 d . . . H27A H 1.0618 0.2007 0.8688 0.027 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0186(2) 0.01580(19) 0.0197(2) -0.0003(3) 0.0041(2) 0.0026(3) N1 0.0172(12) 0.0155(11) 0.0169(12) -0.0020(10) -0.0018(10) -0.0015(10) O1 0.0365(13) 0.0303(11) 0.0223(11) 0.0019(10) 0.0073(10) 0.0160(10) O2 0.0139(10) 0.0188(10) 0.0251(11) -0.0027(9) 0.0014(9) 0.0038(8) O3 0.0246(11) 0.0189(10) 0.0320(12) -0.0004(9) 0.0043(10) 0.0047(9) O4 0.0216(11) 0.0244(9) 0.0309(11) -0.0032(9) 0.0060(10) 0.0062(9) C1 0.0223(17) 0.0192(14) 0.0236(16) 0.0006(12) -0.0001(13) 0.0018(12) C2 0.0197(15) 0.0176(14) 0.0183(14) -0.0008(12) -0.0044(12) 0.0018(11) C3 0.047(2) 0.0376(18) 0.0261(18) -0.0104(16) -0.0002(16) -0.0128(17) C4 0.036(2) 0.0313(17) 0.0219(17) 0.0011(14) -0.0026(15) -0.0050(14) C5 0.0247(18) 0.0307(17) 0.0313(18) -0.0023(15) 0.0076(15) 0.0050(14) C6 0.045(3) 0.063(3) 0.049(3) 0.007(2) -0.011(2) 0.004(2) C7 0.032(2) 0.0282(17) 0.059(3) -0.0040(18) 0.0086(19) -0.0039(15) C8 0.038(2) 0.0156(13) 0.048(2) 0.0035(14) 0.0081(19) 0.0057(15) C9 0.056(3) 0.045(2) 0.056(3) 0.0148(19) -0.006(2) 0.013(2) C10 0.096(4) 0.0198(17) 0.084(4) 0.003(2) -0.024(3) -0.008(2) C11 0.0127(15) 0.0185(13) 0.0186(14) -0.0025(12) 0.0005(11) 0.0021(10) C12 0.0146(14) 0.0188(13) 0.0155(14) -0.0031(12) 0.0026(12) 0.0041(11) C13 0.0164(14) 0.0228(14) 0.0213(15) -0.0025(12) 0.0048(12) -0.0018(12) C14 0.0227(15) 0.0274(17) 0.0305(17) -0.0024(13) 0.0064(14) -0.0075(13) C15 0.0150(13) 0.0250(15) 0.0290(15) -0.0046(15) -0.0001(12) -0.0042(14) C16 0.0139(14) 0.0170(12) 0.0213(14) 0.0031(11) -0.0018(13) -0.0028(12) C17 0.0138(15) 0.0285(15) 0.0238(16) 0.0028(13) 0.0004(12) 0.0003(12) C18 0.0178(15) 0.0345(15) 0.0281(16) 0.0092(13) -0.0052(15) -0.0032(14) C19 0.0288(18) 0.0256(16) 0.0185(16) 0.0036(13) -0.0032(13) -0.0117(13) C20 0.032(2) 0.0214(14) 0.0197(15) -0.0034(12) 0.0016(13) -0.0021(13) C21 0.0257(17) 0.0257(15) 0.0225(16) -0.0014(13) -0.0010(13) 0.0042(13) C22 0.0143(13) 0.0188(12) 0.0185(13) -0.0027(11) -0.0028(13) -0.0039(13) C23 0.0183(15) 0.0209(14) 0.0204(15) -0.0013(12) 0.0001(13) -0.0025(12) C24 0.0250(16) 0.0195(14) 0.0250(16) -0.0036(13) -0.0056(13) 0.0008(13) C25 0.0236(16) 0.0246(14) 0.0230(16) 0.0031(14) -0.0036(14) -0.0077(12) C26 0.0176(16) 0.0351(17) 0.0231(17) 0.0022(14) -0.0002(13) -0.0056(13) C27 0.0153(15) 0.0263(15) 0.0254(17) -0.0022(13) -0.0002(12) 0.0000(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O4 1.789(2) . ? Ti1 O3 1.823(2) . ? Ti1 O1 1.837(2) . ? Ti1 O2 1.869(2) . ? Ti1 N1 2.316(2) . ? N1 C2 1.475(3) . ? N1 C12 1.494(3) . ? N1 C15 1.496(3) . ? O1 C1 1.432(4) . ? O2 C11 1.409(3) . ? O3 C8 1.433(3) . ? O4 C5 1.412(4) . ? C1 C4 1.521(4) . ? C1 C3 1.525(4) . ? C1 C2 1.526(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.510(5) . ? C5 C7 1.516(4) . ? C5 H5A 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.508(5) . ? C8 C10 1.515(5) . ? C8 H8A 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C16 1.542(4) . ? C11 C22 1.543(4) . ? C11 C12 1.561(4) . ? C12 C13 1.529(4) . ? C12 H12A 1.0000 . ? C13 C14 1.537(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.517(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.384(4) . ? C16 C21 1.394(4) . ? C17 C18 1.387(4) . ? C17 H17A 0.9500 . ? C18 C19 1.377(4) . ? C18 H18A 0.9500 . ? C19 C20 1.381(4) . ? C19 H19A 0.9500 . ? C20 C21 1.380(4) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C23 1.390(4) . ? C22 C27 1.394(4) . ? C23 C24 1.387(4) . ? C23 H23A 0.9500 . ? C24 C25 1.386(4) . ? C24 H24A 0.9500 . ? C25 C26 1.378(4) . ? C25 H25A 0.9500 . ? C26 C27 1.383(4) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? 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 O4 Ti1 O3 101.06(9) . . ? O4 Ti1 O1 100.72(10) . . ? O3 Ti1 O1 114.89(10) . . ? O4 Ti1 O2 96.91(9) . . ? O3 Ti1 O2 114.40(9) . . ? O1 Ti1 O2 122.62(9) . . ? O4 Ti1 N1 169.50(9) . . ? O3 Ti1 N1 89.17(9) . . ? O1 Ti1 N1 76.72(9) . . ? O2 Ti1 N1 76.47(8) . . ? C2 N1 C12 114.2(2) . . ? C2 N1 C15 112.0(2) . . ? C12 N1 C15 105.2(2) . . ? C2 N1 Ti1 103.64(17) . . ? C12 N1 Ti1 106.32(17) . . ? C15 N1 Ti1 115.67(16) . . ? C1 O1 Ti1 128.44(18) . . ? C11 O2 Ti1 127.94(17) . . ? C8 O3 Ti1 131.7(2) . . ? C5 O4 Ti1 164.4(2) . . ? O1 C1 C4 107.8(2) . . ? O1 C1 C3 109.5(2) . . ? C4 C1 C3 109.8(3) . . ? O1 C1 C2 106.3(2) . . ? C4 C1 C2 110.3(2) . . ? C3 C1 C2 112.9(3) . . ? N1 C2 C1 111.1(2) . . ? N1 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 . . ? N1 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O4 C5 C6 109.5(3) . . ? O4 C5 C7 109.6(3) . . ? C6 C5 C7 112.7(3) . . ? O4 C5 H5A 108.3 . . ? C6 C5 H5A 108.3 . . ? C7 C5 H5A 108.3 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O3 C8 C9 109.3(3) . . ? O3 C8 C10 108.4(3) . . ? C9 C8 C10 112.2(3) . . ? O3 C8 H8A 109.0 . . ? C9 C8 H8A 109.0 . . ? C10 C8 H8A 109.0 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O2 C11 C16 108.7(2) . . ? O2 C11 C22 109.4(2) . . ? C16 C11 C22 108.8(2) . . ? O2 C11 C12 106.0(2) . . ? C16 C11 C12 109.8(2) . . ? C22 C11 C12 113.9(2) . . ? N1 C12 C13 103.2(2) . . ? N1 C12 C11 108.8(2) . . ? C13 C12 C11 112.3(2) . . ? N1 C12 H12A 110.8 . . ? C13 C12 H12A 110.8 . . ? C11 C12 H12A 110.8 . . ? C12 C13 C14 105.5(2) . . ? C12 C13 H13A 110.6 . . ? C14 C13 H13A 110.6 . . ? C12 C13 H13B 110.6 . . ? C14 C13 H13B 110.6 . . ? H13A C13 H13B 108.8 . . ? C15 C14 C13 105.6(2) . . ? C15 C14 H14A 110.6 . . ? C13 C14 H14A 110.6 . . ? C15 C14 H14B 110.6 . . ? C13 C14 H14B 110.6 . . ? H14A C14 H14B 108.7 . . ? N1 C15 C14 106.4(2) . . ? N1 C15 H15A 110.5 . . ? C14 C15 H15A 110.5 . . ? N1 C15 H15B 110.5 . . ? C14 C15 H15B 110.5 . . ? H15A C15 H15B 108.6 . . ? C17 C16 C21 117.9(3) . . ? C17 C16 C11 120.0(3) . . ? C21 C16 C11 122.0(3) . . ? C16 C17 C18 120.8(3) . . ? C16 C17 H17A 119.6 . . ? C18 C17 H17A 119.6 . . ? C19 C18 C17 120.8(3) . . ? C19 C18 H18A 119.6 . . ? C17 C18 H18A 119.6 . . ? C18 C19 C20 119.0(3) . . ? C18 C19 H19A 120.5 . . ? C20 C19 H19A 120.5 . . ? C21 C20 C19 120.4(3) . . ? C21 C20 H20A 119.8 . . ? C19 C20 H20A 119.8 . . ? C20 C21 C16 121.1(3) . . ? C20 C21 H21A 119.4 . . ? C16 C21 H21A 119.4 . . ? C23 C22 C27 117.4(3) . . ? C23 C22 C11 122.1(3) . . ? C27 C22 C11 120.5(2) . . ? C24 C23 C22 121.3(3) . . ? C24 C23 H23A 119.3 . . ? C22 C23 H23A 119.3 . . ? C25 C24 C23 120.5(3) . . ? C25 C24 H24A 119.8 . . ? C23 C24 H24A 119.8 . . ? C26 C25 C24 118.7(3) . . ? C26 C25 H25A 120.6 . . ? C24 C25 H25A 120.6 . . ? C25 C26 C27 120.8(3) . . ? C25 C26 H26A 119.6 . . ? C27 C26 H26A 119.6 . . ? C26 C27 C22 121.3(3) . . ? C26 C27 H27A 119.4 . . ? C22 C27 H27A 119.4 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.329 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.060 # Attachment '25.CIF' data_mI _database_code_depnum_ccdc_archive 'CCDC 683793' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H50 N2 O4 Ti' _chemical_formula_sum 'C32 H50 N2 O4 Ti' _chemical_formula_weight 574.64 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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.6073(4) _cell_length_b 18.8704(9) _cell_length_c 19.0174(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3088.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4381 _cell_measurement_theta_min 2.398 _cell_measurement_theta_max 27.103 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.314 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9692 _exptl_absorpt_correction_T_max 0.9814 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19614 _diffrn_reflns_av_R_equivalents 0.0879 _diffrn_reflns_av_sigmaI/netI 0.1091 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.00 _reflns_number_total 6735 _reflns_number_gt 5068 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0333P)^2^+0.1331P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(3) _refine_ls_number_reflns 6735 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0898 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1029 _refine_ls_wR_factor_gt 0.0957 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 Ti Ti 0.35372(6) 0.09632(3) 0.81516(3) 0.01339(13) Uani 1 1 d . . . N1 N 0.4207(3) 0.06758(14) 0.94995(14) 0.0138(6) Uani 1 1 d . . . N2 N 0.5464(3) 0.17099(14) 0.71902(14) 0.0149(6) Uani 1 1 d . . . O11 O 0.5025(2) 0.02604(10) 0.81815(12) 0.0161(5) Uani 1 1 d . . . O12 O 0.1746(2) 0.06930(11) 0.85827(10) 0.0141(5) Uani 1 1 d . . . O21 O 0.3952(2) 0.18680(11) 0.84555(11) 0.0152(5) Uani 1 1 d . . . O22 O 0.2748(2) 0.09497(12) 0.72690(11) 0.0164(5) Uani 1 1 d . . . C11 C 0.5165(4) -0.02823(17) 0.86907(18) 0.0172(8) Uani 1 1 d . . . C12 C 0.6672(4) -0.06913(17) 0.85470(18) 0.0222(8) Uani 1 1 d . . . H12A H 0.6604 -0.0922 0.8087 0.033 Uiso 1 1 calc R . . H12B H 0.6821 -0.1051 0.8913 0.033 Uiso 1 1 calc R . . H12C H 0.7552 -0.0362 0.8550 0.033 Uiso 1 1 calc R . . C13 C 0.3801(4) -0.07996(16) 0.86263(18) 0.0223(8) Uani 1 1 d . . . H13A H 0.3825 -0.1026 0.8163 0.033 Uiso 1 1 calc R . . H13B H 0.2821 -0.0541 0.8683 0.033 Uiso 1 1 calc R . . H13C H 0.3884 -0.1163 0.8993 0.033 Uiso 1 1 calc R . . C14 C 0.5295(4) 0.00773(17) 0.94145(17) 0.0153(7) Uani 1 1 d . . . H14A H 0.5087 -0.0278 0.9786 0.018 Uiso 1 1 calc R . . H14B H 0.6371 0.0251 0.9479 0.018 Uiso 1 1 calc R . . C15 C 0.1319(4) 0.07450(16) 0.93016(16) 0.0151(7) Uani 1 1 d . . . C16 C 0.0948(4) 0.15209(17) 0.94689(17) 0.0185(8) Uani 1 1 d . . . H16A H 0.0089 0.1682 0.9171 0.028 Uiso 1 1 calc R . . H16B H 0.1867 0.1813 0.9379 0.028 Uiso 1 1 calc R . . H16C H 0.0650 0.1564 0.9964 0.028 Uiso 1 1 calc R . . C17 C -0.0126(4) 0.02937(19) 0.94133(19) 0.0205(8) Uani 1 1 d . . . H17A H -0.0960 0.0462 0.9104 0.031 Uiso 1 1 calc R . . H17B H -0.0461 0.0331 0.9905 0.031 Uiso 1 1 calc R . . H17C H 0.0111 -0.0202 0.9303 0.031 Uiso 1 1 calc R . . C18 C 0.2655(4) 0.04427(17) 0.97393(17) 0.0158(7) Uani 1 1 d . . . H18A H 0.2514 0.0588 1.0236 0.019 Uiso 1 1 calc R . . H18B H 0.2609 -0.0081 0.9721 0.019 Uiso 1 1 calc R . . C19 C 0.4843(4) 0.12665(16) 0.99510(17) 0.0138(7) Uani 1 1 d . . . H19A H 0.4072 0.1662 0.9920 0.017 Uiso 1 1 calc R . . C20 C 0.6368(4) 0.15628(17) 0.96725(17) 0.0181(8) Uani 1 1 d . . . H20A H 0.6313 0.1603 0.9159 0.027 Uiso 1 1 calc R . . H20B H 0.7221 0.1244 0.9802 0.027 Uiso 1 1 calc R . . H20C H 0.6552 0.2032 0.9877 0.027 Uiso 1 1 calc R . . C21 C 0.4048(4) 0.24986(16) 0.80470(17) 0.0154(7) Uani 1 1 d . . . C22 C 0.2452(4) 0.26500(17) 0.77205(19) 0.0192(8) Uani 1 1 d . . . H22A H 0.1700 0.2750 0.8095 0.029 Uiso 1 1 calc R . . H22B H 0.2108 0.2236 0.7451 0.029 Uiso 1 1 calc R . . H22C H 0.2528 0.3061 0.7407 0.029 Uiso 1 1 calc R . . C23 C 0.4462(4) 0.31083(17) 0.85481(19) 0.0235(8) Uani 1 1 d . . . H23A H 0.3609 0.3181 0.8882 0.035 Uiso 1 1 calc R . . H23B H 0.4629 0.3543 0.8276 0.035 Uiso 1 1 calc R . . H23C H 0.5413 0.2990 0.8806 0.035 Uiso 1 1 calc R . . C24 C 0.5405(4) 0.24076(17) 0.75262(17) 0.0169(8) Uani 1 1 d . . . H24A H 0.5318 0.2774 0.7156 0.020 Uiso 1 1 calc R . . H24B H 0.6394 0.2489 0.7780 0.020 Uiso 1 1 calc R . . C25 C 0.3394(4) 0.10022(19) 0.65803(15) 0.0183(7) Uani 1 1 d . . . C26 C 0.4297(4) 0.03166(18) 0.64323(19) 0.0229(8) Uani 1 1 d . . . H26A H 0.3576 -0.0085 0.6424 0.034 Uiso 1 1 calc R . . H26B H 0.5073 0.0243 0.6802 0.034 Uiso 1 1 calc R . . H26C H 0.4820 0.0354 0.5976 0.034 Uiso 1 1 calc R . . C27 C 0.2060(4) 0.1096(2) 0.60609(17) 0.0246(9) Uani 1 1 d . . . H27A H 0.1385 0.0678 0.6076 0.037 Uiso 1 1 calc R . . H27B H 0.2479 0.1153 0.5585 0.037 Uiso 1 1 calc R . . H27C H 0.1458 0.1518 0.6188 0.037 Uiso 1 1 calc R . . C28 C 0.4429(4) 0.16698(17) 0.65730(17) 0.0149(7) Uani 1 1 d . . . H28A H 0.5067 0.1669 0.6140 0.018 Uiso 1 1 calc R . . H28B H 0.3759 0.2096 0.6562 0.018 Uiso 1 1 calc R . . C29 C 0.7093(4) 0.14736(17) 0.70145(17) 0.0161(8) Uani 1 1 d . . . H29A H 0.6976 0.1012 0.6762 0.019 Uiso 1 1 calc R . . C30 C 0.8038(4) 0.13096(19) 0.76738(18) 0.0220(8) Uani 1 1 d . . . H30A H 0.7499 0.0949 0.7953 0.033 Uiso 1 1 calc R . . H30B H 0.8157 0.1742 0.7954 0.033 Uiso 1 1 calc R . . H30C H 0.9065 0.1132 0.7538 0.033 Uiso 1 1 calc R . . C31 C 0.4943(3) 0.10672(17) 1.07298(16) 0.0143(7) Uani 1 1 d . . . C32 C 0.6108(4) 0.06233(17) 1.09967(17) 0.0192(8) Uani 1 1 d . . . H32A H 0.6919 0.0465 1.0697 0.023 Uiso 1 1 calc R . . C33 C 0.6083(4) 0.04140(18) 1.16971(18) 0.0255(9) Uani 1 1 d . . . H33A H 0.6890 0.0121 1.1875 0.031 Uiso 1 1 calc R . . C34 C 0.4896(5) 0.0627(2) 1.21372(18) 0.0279(9) Uani 1 1 d . . . H34A H 0.4857 0.0463 1.2609 0.033 Uiso 1 1 calc R . . C35 C 0.3774(4) 0.10781(18) 1.18885(18) 0.0257(8) Uani 1 1 d . . . H35A H 0.2971 0.1238 1.2192 0.031 Uiso 1 1 calc R . . C36 C 0.3813(4) 0.13007(18) 1.11915(17) 0.0203(8) Uani 1 1 d . . . H36A H 0.3043 0.1622 1.1028 0.024 Uiso 1 1 calc R . . C41 C 0.7967(4) 0.19619(18) 0.65066(18) 0.0174(8) Uani 1 1 d . . . C42 C 0.7997(4) 0.1816(2) 0.57881(19) 0.0278(9) Uani 1 1 d . . . H42A H 0.7486 0.1404 0.5616 0.033 Uiso 1 1 calc R . . C43 C 0.8754(4) 0.2256(2) 0.5322(2) 0.0393(11) Uani 1 1 d . . . H43A H 0.8743 0.2150 0.4834 0.047 Uiso 1 1 calc R . . C44 C 0.9529(4) 0.2849(2) 0.5561(2) 0.0349(11) Uani 1 1 d . . . H44A H 1.0053 0.3152 0.5240 0.042 Uiso 1 1 calc R . . C45 C 0.9535(4) 0.2998(2) 0.6266(2) 0.0295(9) Uani 1 1 d . . . H45A H 1.0069 0.3404 0.6435 0.035 Uiso 1 1 calc R . . C46 C 0.8771(4) 0.25603(17) 0.67331(18) 0.0217(8) Uani 1 1 d . . . H46A H 0.8794 0.2670 0.7221 0.026 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti 0.0132(3) 0.0151(3) 0.0118(3) -0.0014(3) 0.0001(3) -0.0009(3) N1 0.0088(13) 0.0126(14) 0.0198(16) -0.0012(12) -0.0005(11) 0.0021(12) N2 0.0152(15) 0.0160(14) 0.0136(15) 0.0010(12) -0.0012(12) 0.0018(12) O11 0.0171(11) 0.0165(11) 0.0147(12) -0.0023(11) 0.0017(11) 0.0016(10) O12 0.0136(11) 0.0199(12) 0.0087(11) -0.0011(10) 0.0005(9) -0.0009(10) O21 0.0152(12) 0.0140(11) 0.0164(12) 0.0040(10) 0.0016(10) -0.0014(10) O22 0.0170(11) 0.0199(12) 0.0123(11) 0.0000(11) 0.0008(9) -0.0058(11) C11 0.0196(18) 0.0153(17) 0.0166(18) -0.0022(15) -0.0040(15) 0.0018(15) C12 0.0234(19) 0.0192(18) 0.024(2) -0.0047(15) -0.0013(16) 0.0018(16) C13 0.0239(19) 0.0165(19) 0.0266(19) -0.0033(15) -0.0052(16) -0.0015(15) C14 0.0131(17) 0.0151(17) 0.0177(18) 0.0014(15) -0.0025(15) 0.0004(14) C15 0.0156(17) 0.0192(18) 0.0104(16) 0.0018(13) 0.0004(14) -0.0004(15) C16 0.0160(18) 0.025(2) 0.0147(18) -0.0025(16) 0.0022(14) 0.0026(15) C17 0.0117(17) 0.032(2) 0.0179(19) 0.0043(17) 0.0010(15) 0.0004(16) C18 0.0158(17) 0.0171(18) 0.0144(18) 0.0011(15) 0.0039(14) -0.0052(15) C19 0.0136(17) 0.0119(16) 0.0158(18) -0.0023(14) -0.0009(14) 0.0017(14) C20 0.0183(18) 0.0190(18) 0.0171(18) 0.0007(14) -0.0024(16) -0.0031(17) C21 0.0179(17) 0.0136(16) 0.0148(18) 0.0025(15) -0.0002(14) -0.0006(14) C22 0.0189(18) 0.0150(18) 0.0237(19) 0.0004(16) -0.0011(15) 0.0020(15) C23 0.027(2) 0.0164(18) 0.027(2) -0.0028(16) 0.0047(17) -0.0027(16) C24 0.0200(18) 0.0150(17) 0.0158(19) -0.0002(14) -0.0016(15) -0.0059(15) C25 0.0167(16) 0.0269(18) 0.0112(15) -0.0012(15) 0.0007(13) -0.0041(18) C26 0.027(2) 0.0228(19) 0.019(2) -0.0056(16) 0.0038(17) -0.0018(17) C27 0.026(2) 0.031(2) 0.0162(18) -0.0005(17) -0.0016(15) -0.0050(17) C28 0.0140(18) 0.0172(18) 0.0134(17) 0.0020(14) 0.0005(14) 0.0019(14) C29 0.0170(17) 0.0158(17) 0.0156(19) -0.0031(14) -0.0030(14) 0.0006(14) C30 0.0180(19) 0.028(2) 0.0205(19) 0.0042(17) 0.0003(15) 0.0014(16) C31 0.0102(16) 0.0175(18) 0.0152(17) -0.0043(15) -0.0010(13) -0.0057(15) C32 0.0190(19) 0.0172(18) 0.0215(19) -0.0047(15) 0.0013(15) 0.0000(15) C33 0.031(2) 0.0229(19) 0.023(2) 0.0007(16) -0.0072(16) 0.0005(17) C34 0.037(2) 0.034(2) 0.0125(18) -0.0014(17) 0.0017(17) -0.008(2) C35 0.0204(18) 0.036(2) 0.0203(18) -0.0107(19) 0.0069(17) -0.0044(17) C36 0.016(2) 0.028(2) 0.0174(19) -0.0069(15) -0.0010(15) -0.0026(16) C41 0.0077(16) 0.0238(19) 0.0206(19) 0.0041(16) -0.0006(14) 0.0012(14) C42 0.024(2) 0.036(2) 0.024(2) -0.0063(19) 0.0005(17) -0.0024(18) C43 0.024(2) 0.074(3) 0.019(2) 0.002(2) 0.0042(19) -0.002(2) C44 0.020(2) 0.058(3) 0.027(2) 0.019(2) 0.0043(19) -0.003(2) C45 0.018(2) 0.029(2) 0.041(3) 0.0100(19) 0.0052(18) -0.0003(17) C46 0.0157(18) 0.0264(19) 0.023(2) 0.0016(16) 0.0047(16) 0.0031(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti O22 1.811(2) . ? Ti O12 1.819(2) . ? Ti O21 1.838(2) . ? Ti O11 1.844(2) . ? Ti N1 2.683(3) . ? Ti N2 2.842(3) . ? N1 C14 1.476(4) . ? N1 C18 1.479(4) . ? N1 C19 1.510(4) . ? N2 C24 1.464(4) . ? N2 C28 1.476(4) . ? N2 C29 1.508(4) . ? O11 C11 1.415(4) . ? O12 C15 1.419(4) . ? O21 C21 1.424(4) . ? O22 C25 1.426(3) . ? C11 C13 1.532(4) . ? C11 C12 1.534(5) . ? C11 C14 1.539(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C17 1.523(4) . ? C15 C18 1.530(4) . ? C15 C16 1.532(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.522(5) . ? C19 C31 1.531(4) . ? C19 H19A 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.535(4) . ? C21 C23 1.536(5) . ? C21 C24 1.541(4) . ? 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 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C27 1.525(4) . ? C25 C26 1.536(5) . ? C25 C28 1.543(5) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.526(4) . ? C29 C41 1.532(4) . ? C29 H29A 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C36 1.382(4) . ? C31 C32 1.402(4) . ? C32 C33 1.389(4) . ? C32 H32A 0.9500 . ? C33 C34 1.381(5) . ? C33 H33A 0.9500 . ? C34 C35 1.371(5) . ? C34 H34A 0.9500 . ? C35 C36 1.391(5) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C41 C46 1.393(4) . ? C41 C42 1.394(5) . ? C42 C43 1.378(5) . ? C42 H42A 0.9500 . ? C43 C44 1.381(5) . ? C43 H43A 0.9500 . ? C44 C45 1.370(5) . ? C44 H44A 0.9500 . ? C45 C46 1.379(5) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? 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 O22 Ti O12 95.51(9) . . ? O22 Ti O21 112.18(10) . . ? O12 Ti O21 106.45(9) . . ? O22 Ti O11 106.19(10) . . ? O12 Ti O11 111.90(10) . . ? O21 Ti O11 121.57(10) . . ? O22 Ti N1 164.45(9) . . ? O12 Ti N1 72.23(9) . . ? O21 Ti N1 81.11(9) . . ? O11 Ti N1 71.09(9) . . ? O22 Ti N2 68.26(9) . . ? O12 Ti N2 157.43(9) . . ? O21 Ti N2 68.19(8) . . ? O11 Ti N2 88.34(9) . . ? N1 Ti N2 126.11(8) . . ? C14 N1 C18 112.3(2) . . ? C14 N1 C19 113.4(2) . . ? C18 N1 C19 111.8(2) . . ? C14 N1 Ti 100.74(18) . . ? C18 N1 Ti 99.24(18) . . ? C19 N1 Ti 118.17(18) . . ? C24 N2 C28 111.8(3) . . ? C24 N2 C29 113.3(3) . . ? C28 N2 C29 111.7(2) . . ? C24 N2 Ti 98.32(18) . . ? C28 N2 Ti 97.69(17) . . ? C29 N2 Ti 122.57(19) . . ? C11 O11 Ti 126.9(2) . . ? C15 O12 Ti 129.37(19) . . ? C21 O21 Ti 128.05(18) . . ? C25 O22 Ti 134.77(18) . . ? O11 C11 C13 110.0(3) . . ? O11 C11 C12 108.3(3) . . ? C13 C11 C12 108.2(3) . . ? O11 C11 C14 107.4(3) . . ? C13 C11 C14 114.1(3) . . ? C12 C11 C14 108.6(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 C11 112.9(3) . . ? N1 C14 H14A 109.0 . . ? C11 C14 H14A 109.0 . . ? N1 C14 H14B 109.0 . . ? C11 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? O12 C15 C17 107.9(3) . . ? O12 C15 C18 107.7(3) . . ? C17 C15 C18 109.2(3) . . ? O12 C15 C16 108.7(2) . . ? C17 C15 C16 109.6(3) . . ? C18 C15 C16 113.6(3) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N1 C18 C15 113.6(3) . . ? N1 C18 H18A 108.8 . . ? C15 C18 H18A 108.8 . . ? N1 C18 H18B 108.8 . . ? C15 C18 H18B 108.8 . . ? H18A C18 H18B 107.7 . . ? N1 C19 C20 112.7(3) . . ? N1 C19 C31 112.9(3) . . ? C20 C19 C31 112.2(3) . . ? N1 C19 H19A 106.1 . . ? C20 C19 H19A 106.1 . . ? C31 C19 H19A 106.1 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O21 C21 C22 108.9(2) . . ? O21 C21 C23 107.5(3) . . ? C22 C21 C23 108.6(3) . . ? O21 C21 C24 107.6(2) . . ? C22 C21 C24 116.1(3) . . ? C23 C21 C24 107.8(3) . . ? 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 . . ? N2 C24 C21 114.0(3) . . ? N2 C24 H24A 108.7 . . ? C21 C24 H24A 108.7 . . ? N2 C24 H24B 108.7 . . ? C21 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? O22 C25 C27 108.0(3) . . ? O22 C25 C26 107.9(3) . . ? C27 C25 C26 111.2(3) . . ? O22 C25 C28 106.9(3) . . ? C27 C25 C28 109.5(3) . . ? C26 C25 C28 113.2(3) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N2 C28 C25 112.5(3) . . ? N2 C28 H28A 109.1 . . ? C25 C28 H28A 109.1 . . ? N2 C28 H28B 109.1 . . ? C25 C28 H28B 109.1 . . ? H28A C28 H28B 107.8 . . ? N2 C29 C30 111.9(3) . . ? N2 C29 C41 114.7(3) . . ? C30 C29 C41 112.2(3) . . ? N2 C29 H29A 105.7 . . ? C30 C29 H29A 105.7 . . ? C41 C29 H29A 105.7 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C36 C31 C32 117.6(3) . . ? C36 C31 C19 119.8(3) . . ? C32 C31 C19 122.5(3) . . ? C33 C32 C31 120.4(3) . . ? C33 C32 H32A 119.8 . . ? C31 C32 H32A 119.8 . . ? C34 C33 C32 120.6(3) . . ? C34 C33 H33A 119.7 . . ? C32 C33 H33A 119.7 . . ? C35 C34 C33 119.5(3) . . ? C35 C34 H34A 120.2 . . ? C33 C34 H34A 120.2 . . ? C34 C35 C36 119.9(3) . . ? C34 C35 H35A 120.0 . . ? C36 C35 H35A 120.0 . . ? C31 C36 C35 121.7(3) . . ? C31 C36 H36A 119.1 . . ? C35 C36 H36A 119.1 . . ? C46 C41 C42 117.0(3) . . ? C46 C41 C29 122.5(3) . . ? C42 C41 C29 120.5(3) . . ? C43 C42 C41 121.3(4) . . ? C43 C42 H42A 119.4 . . ? C41 C42 H42A 119.4 . . ? C42 C43 C44 120.4(4) . . ? C42 C43 H43A 119.8 . . ? C44 C43 H43A 119.8 . . ? C45 C44 C43 119.3(4) . . ? C45 C44 H44A 120.3 . . ? C43 C44 H44A 120.3 . . ? C44 C45 C46 120.4(4) . . ? C44 C45 H45A 119.8 . . ? C46 C45 H45A 119.8 . . ? C45 C46 C41 121.6(3) . . ? C45 C46 H46A 119.2 . . ? C41 C46 H46A 119.2 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.376 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.064 # Attachment '26.CIF' data_z _database_code_depnum_ccdc_archive 'CCDC 683794' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H50 N2 O4 Ti' _chemical_formula_sum 'C40 H50 N2 O4 Ti' _chemical_formula_weight 670.72 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 orthorhombic _symmetry_space_group_name_H-M 'C 2 2 21' _symmetry_space_group_name_Hall 'C 2c 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.8805(14) _cell_length_b 17.269(2) _cell_length_c 18.868(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3545.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3798 _cell_measurement_theta_min 3.092 _cell_measurement_theta_max 23.513 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.284 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9070 _exptl_absorpt_correction_T_max 0.9453 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13938 _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_sigmaI/netI 0.0537 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 28.00 _reflns_number_total 4121 _reflns_number_gt 3577 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0383P)^2^+2.1966P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(3) _refine_ls_number_reflns 4121 _refine_ls_number_parameters 313 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.0937 _refine_ls_wR_factor_gt 0.0898 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _chemical_absolute_configuration ad loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.5000 0.79967(3) 0.2500 0.01860(13) Uani 1 2 d S . . O1 O 0.55396(14) 0.75596(9) 0.33430(8) 0.0206(3) Uani 1 1 d . . . O2 O 0.61333(14) 0.86989(9) 0.21858(8) 0.0210(4) Uani 1 1 d . . . N1 N 0.69748(18) 0.72047(10) 0.22293(10) 0.0189(4) Uani 1 1 d . . . C1 C 0.6896(2) 0.66649(13) 0.16064(12) 0.0202(5) Uani 1 1 d . . . C2 C 0.5945(2) 0.60252(14) 0.17086(14) 0.0234(5) Uani 1 1 d . . . C3 C 0.8103(2) 0.63066(12) 0.13640(12) 0.0191(5) Uani 1 1 d . . . C4 C 0.8514(2) 0.64524(14) 0.06782(13) 0.0226(5) Uani 1 1 d . . . C5 C 0.9542(2) 0.60806(14) 0.04101(13) 0.0272(5) Uani 1 1 d . . . C6 C 1.0188(3) 0.55585(14) 0.08211(13) 0.0274(6) Uani 1 1 d . . . C7 C 0.9796(2) 0.54003(13) 0.15071(13) 0.0252(6) Uani 1 1 d . . . C8 C 0.8750(2) 0.57637(13) 0.17719(13) 0.0237(5) Uani 1 1 d . . . C11 C 0.7258(2) 0.68233(13) 0.29080(12) 0.0211(5) Uani 1 1 d . . . C12 C 0.6692(2) 0.72694(13) 0.35420(13) 0.0212(5) Uani 1 1 d . . . C13 C 0.7517(2) 0.78878(13) 0.38629(12) 0.0213(5) Uani 1 1 d . . . C14 C 0.8613(2) 0.76614(16) 0.41843(14) 0.0295(6) Uani 1 1 d . . . C15 C 0.9385(3) 0.81926(16) 0.45009(15) 0.0345(6) Uani 1 1 d . . . C16 C 0.9071(3) 0.89730(16) 0.45020(15) 0.0340(6) Uani 1 1 d . . . C17 C 0.7977(3) 0.92085(15) 0.41921(13) 0.0300(6) Uani 1 1 d . . . C18 C 0.7208(3) 0.86679(14) 0.38738(13) 0.0240(5) Uani 1 1 d . . . C21 C 0.7856(2) 0.78470(12) 0.20947(12) 0.0199(5) Uani 1 1 d . . . C22 C 0.7245(2) 0.85780(13) 0.18016(12) 0.0218(5) Uani 1 1 d . . . C23 C 0.6943(3) 0.85310(16) 0.10129(13) 0.0262(6) Uani 1 1 d . . . C24 C 0.8095(3) 0.92676(14) 0.19400(15) 0.0262(5) Uani 1 1 d . . . H1 H 0.663(2) 0.6996(14) 0.1223(12) 0.012(6) Uiso 1 1 d . . . H2 H 0.885(3) 0.9183(14) 0.1702(13) 0.025(7) Uiso 1 1 d . . . H3 H 0.823(2) 0.6777(13) 0.2999(12) 0.015(6) Uiso 1 1 d . . . H4 H 0.823(2) 0.7986(14) 0.2554(16) 0.034(7) Uiso 1 1 d . . . H5 H 0.687(2) 0.6294(16) 0.2921(14) 0.031(7) Uiso 1 1 d . . . H6 H 0.660(2) 0.6867(14) 0.3952(13) 0.019(6) Uiso 1 1 d . . . H7 H 0.619(2) 0.5622(14) 0.2048(13) 0.018(6) Uiso 1 1 d . . . H8 H 0.771(3) 0.9733(18) 0.1741(15) 0.039(8) Uiso 1 1 d . . . H9 H 0.664(2) 0.9041(16) 0.0822(14) 0.027(7) Uiso 1 1 d . . . H10 H 0.825(2) 0.9321(13) 0.2440(17) 0.029(7) Uiso 1 1 d . . . H11 H 1.020(2) 0.5051(13) 0.1807(12) 0.020(6) Uiso 1 1 d . . . H12 H 1.091(3) 0.5327(15) 0.0622(13) 0.025(7) Uiso 1 1 d . . . H13 H 0.977(3) 0.6171(17) -0.0058(16) 0.041(8) Uiso 1 1 d . . . H14 H 0.846(2) 0.5623(14) 0.2256(13) 0.025(7) Uiso 1 1 d . . . H15 H 0.577(2) 0.5789(14) 0.1249(14) 0.024(7) Uiso 1 1 d . . . H17 H 0.650(3) 0.8831(16) 0.3681(14) 0.028(8) Uiso 1 1 d . . . H18 H 0.626(3) 0.8142(18) 0.0936(15) 0.043(9) Uiso 1 1 d . . . H19 H 0.771(3) 0.8372(16) 0.0723(15) 0.035(8) Uiso 1 1 d . . . H20 H 0.854(2) 0.7679(13) 0.1767(12) 0.012(6) Uiso 1 1 d . . . H21 H 0.808(2) 0.6797(14) 0.0360(13) 0.022(6) Uiso 1 1 d . . . H22 H 0.518(3) 0.6183(15) 0.1891(13) 0.030(7) Uiso 1 1 d . . . H23 H 0.775(3) 0.9781(17) 0.4207(14) 0.036(8) Uiso 1 1 d . . . H24 H 0.877(3) 0.7126(18) 0.4185(15) 0.038(8) Uiso 1 1 d . . . H26 H 1.019(3) 0.8007(18) 0.4765(16) 0.054(9) Uiso 1 1 d . . . H27 H 0.964(3) 0.9366(16) 0.4744(14) 0.038(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0161(3) 0.0152(3) 0.0245(3) 0.000 -0.0001(3) 0.000 O1 0.0129(8) 0.0218(8) 0.0269(8) 0.0003(7) -0.0006(7) 0.0032(6) O2 0.0161(9) 0.0164(8) 0.0305(8) 0.0013(7) 0.0036(7) 0.0006(6) N1 0.0188(11) 0.0136(9) 0.0245(8) -0.0007(7) 0.0016(8) -0.0002(7) C1 0.0178(13) 0.0168(11) 0.0259(11) -0.0013(9) -0.0001(10) 0.0016(9) C2 0.0191(13) 0.0194(12) 0.0315(12) -0.0016(11) 0.0003(11) -0.0016(9) C3 0.0155(12) 0.0152(10) 0.0266(11) -0.0025(9) -0.0014(10) 0.0005(8) C4 0.0227(14) 0.0190(11) 0.0259(11) 0.0010(10) -0.0006(10) 0.0000(9) C5 0.0239(14) 0.0290(13) 0.0286(12) -0.0022(10) 0.0042(11) -0.0026(10) C6 0.0196(16) 0.0243(12) 0.0382(12) -0.0081(10) 0.0020(12) 0.0026(10) C7 0.0215(16) 0.0190(11) 0.0352(12) -0.0037(9) -0.0068(11) 0.0042(9) C8 0.0220(14) 0.0219(12) 0.0273(11) -0.0012(10) -0.0006(10) 0.0035(9) C11 0.0218(14) 0.0156(12) 0.0260(11) -0.0008(9) -0.0006(10) 0.0009(8) C12 0.0189(13) 0.0183(11) 0.0265(11) 0.0019(9) -0.0012(10) 0.0029(9) C13 0.0196(12) 0.0211(12) 0.0234(10) -0.0023(9) 0.0025(9) 0.0000(9) C14 0.0232(14) 0.0283(14) 0.0369(13) -0.0068(11) -0.0042(11) 0.0034(10) C15 0.0227(15) 0.0387(16) 0.0422(15) -0.0096(12) -0.0052(12) 0.0012(11) C16 0.0308(16) 0.0342(14) 0.0370(14) -0.0077(12) 0.0030(13) -0.0134(12) C17 0.0378(17) 0.0220(13) 0.0303(12) -0.0001(10) 0.0032(12) -0.0048(11) C18 0.0257(15) 0.0203(12) 0.0261(11) 0.0010(10) -0.0015(11) 0.0022(10) C21 0.0144(12) 0.0192(12) 0.0262(11) -0.0014(9) 0.0008(10) -0.0008(8) C22 0.0184(13) 0.0178(11) 0.0291(11) -0.0005(9) 0.0034(10) 0.0002(9) C23 0.0281(16) 0.0232(13) 0.0273(12) 0.0042(11) -0.0011(12) 0.0006(11) C24 0.0234(14) 0.0192(12) 0.0359(13) -0.0009(11) 0.0048(12) -0.0022(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O2 1.8283(16) 3_655 ? Ti1 O2 1.8283(16) . ? Ti1 O1 1.8558(15) 3_655 ? Ti1 O1 1.8559(15) . ? Ti1 N1 2.5978(19) . ? Ti1 N1 2.5978(19) 3_655 ? O1 C12 1.401(3) . ? O2 C22 1.425(3) . ? N1 C11 1.472(3) . ? N1 C21 1.488(3) . ? N1 C1 1.503(3) . ? C1 C3 1.522(3) . ? C1 C2 1.526(3) . ? C1 H1 0.97(2) . ? C2 H7 0.98(2) . ? C2 H15 0.98(3) . ? C2 H22 0.94(3) . ? C3 C4 1.392(3) . ? C3 C8 1.402(3) . ? C4 C5 1.385(3) . ? C4 H21 0.97(3) . ? C5 C6 1.382(4) . ? C5 H13 0.93(3) . ? C6 C7 1.390(3) . ? C6 H12 0.95(3) . ? C7 C8 1.392(3) . ? C7 H11 0.94(2) . ? C8 H14 1.00(2) . ? C11 C12 1.551(3) . ? C11 H3 1.07(2) . ? C11 H5 1.00(3) . ? C12 C13 1.521(3) . ? C12 H6 1.04(2) . ? C13 C18 1.389(3) . ? C13 C14 1.394(3) . ? C14 C15 1.380(4) . ? C14 H24 0.94(3) . ? C15 C16 1.390(4) . ? C15 H26 1.05(3) . ? C16 C17 1.388(4) . ? C16 H27 1.03(3) . ? C17 C18 1.390(4) . ? C17 H23 1.02(3) . ? C18 H17 0.90(3) . ? C21 C22 1.530(3) . ? C21 H4 0.99(3) . ? C21 H20 1.01(2) . ? C22 C23 1.526(3) . ? C22 C24 1.530(3) . ? C23 H9 1.01(3) . ? C23 H18 1.02(3) . ? C23 H19 1.03(3) . ? C24 H2 0.95(3) . ? C24 H8 0.98(3) . ? C24 H10 0.96(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 O2 Ti1 O2 96.90(10) 3_655 . ? O2 Ti1 O1 109.53(7) 3_655 3_655 ? O2 Ti1 O1 101.85(7) . 3_655 ? O2 Ti1 O1 101.84(7) 3_655 . ? O2 Ti1 O1 109.53(7) . . ? O1 Ti1 O1 132.00(10) 3_655 . ? O2 Ti1 N1 166.13(6) 3_655 . ? O2 Ti1 N1 74.20(6) . . ? O1 Ti1 N1 83.05(7) 3_655 . ? O1 Ti1 N1 72.10(6) . . ? O2 Ti1 N1 74.20(6) 3_655 3_655 ? O2 Ti1 N1 166.13(6) . 3_655 ? O1 Ti1 N1 72.10(6) 3_655 3_655 ? O1 Ti1 N1 83.05(7) . 3_655 ? N1 Ti1 N1 116.46(8) . 3_655 ? C12 O1 Ti1 131.16(14) . . ? C22 O2 Ti1 129.79(14) . . ? C11 N1 C21 110.31(18) . . ? C11 N1 C1 114.50(17) . . ? C21 N1 C1 111.44(18) . . ? C11 N1 Ti1 103.74(13) . . ? C21 N1 Ti1 100.03(12) . . ? C1 N1 Ti1 115.68(14) . . ? N1 C1 C3 115.99(19) . . ? N1 C1 C2 112.87(19) . . ? C3 C1 C2 109.20(19) . . ? N1 C1 H1 103.6(14) . . ? C3 C1 H1 105.7(14) . . ? C2 C1 H1 108.8(14) . . ? C1 C2 H7 114.3(14) . . ? C1 C2 H15 108.8(15) . . ? H7 C2 H15 110(2) . . ? C1 C2 H22 115.9(16) . . ? H7 C2 H22 102(2) . . ? H15 C2 H22 106(2) . . ? C4 C3 C8 118.0(2) . . ? C4 C3 C1 118.9(2) . . ? C8 C3 C1 122.7(2) . . ? C5 C4 C3 121.0(2) . . ? C5 C4 H21 116.9(15) . . ? C3 C4 H21 122.0(15) . . ? C6 C5 C4 120.6(2) . . ? C6 C5 H13 120.5(19) . . ? C4 C5 H13 118.8(19) . . ? C5 C6 C7 119.6(2) . . ? C5 C6 H12 117.9(15) . . ? C7 C6 H12 122.4(15) . . ? C6 C7 C8 119.8(2) . . ? C6 C7 H11 122.8(15) . . ? C8 C7 H11 117.4(15) . . ? C7 C8 C3 121.0(2) . . ? C7 C8 H14 118.4(15) . . ? C3 C8 H14 120.6(15) . . ? N1 C11 C12 111.44(18) . . ? N1 C11 H3 112.3(13) . . ? C12 C11 H3 107.7(12) . . ? N1 C11 H5 110.0(15) . . ? C12 C11 H5 105.5(15) . . ? H3 C11 H5 110(2) . . ? O1 C12 C13 112.56(18) . . ? O1 C12 C11 109.05(19) . . ? C13 C12 C11 114.9(2) . . ? O1 C12 H6 110.7(14) . . ? C13 C12 H6 103.1(13) . . ? C11 C12 H6 106.2(14) . . ? C18 C13 C14 118.2(2) . . ? C18 C13 C12 123.0(2) . . ? C14 C13 C12 118.8(2) . . ? C15 C14 C13 121.5(3) . . ? C15 C14 H24 122.8(19) . . ? C13 C14 H24 115.6(19) . . ? C14 C15 C16 119.7(3) . . ? C14 C15 H26 120.4(17) . . ? C16 C15 H26 119.8(17) . . ? C17 C16 C15 119.6(3) . . ? C17 C16 H27 120.8(15) . . ? C15 C16 H27 119.6(16) . . ? C16 C17 C18 120.1(3) . . ? C16 C17 H23 118.8(16) . . ? C18 C17 H23 121.1(16) . . ? C13 C18 C17 120.8(3) . . ? C13 C18 H17 120.4(18) . . ? C17 C18 H17 118.8(18) . . ? N1 C21 C22 113.34(19) . . ? N1 C21 H4 107.5(15) . . ? C22 C21 H4 107.2(14) . . ? N1 C21 H20 111.5(13) . . ? C22 C21 H20 109.6(13) . . ? H4 C21 H20 107(2) . . ? O2 C22 C23 108.8(2) . . ? O2 C22 C24 108.18(19) . . ? C23 C22 C24 109.7(2) . . ? O2 C22 C21 107.82(18) . . ? C23 C22 C21 113.7(2) . . ? C24 C22 C21 108.5(2) . . ? C22 C23 H9 111.9(15) . . ? C22 C23 H18 109.5(17) . . ? H9 C23 H18 106(2) . . ? C22 C23 H19 111.0(16) . . ? H9 C23 H19 108(2) . . ? H18 C23 H19 110(2) . . ? C22 C24 H2 108.8(16) . . ? C22 C24 H8 108.4(18) . . ? H2 C24 H8 108(2) . . ? C22 C24 H10 110.2(15) . . ? H2 C24 H10 109(2) . . ? H8 C24 H10 112(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Ti1 O1 C12 -147.09(18) 3_655 . . . ? O2 Ti1 O1 C12 -45.3(2) . . . . ? O1 Ti1 O1 C12 82.48(18) 3_655 . . . ? N1 Ti1 O1 C12 19.99(18) . . . . ? N1 Ti1 O1 C12 140.72(18) 3_655 . . . ? O2 Ti1 O2 C22 -173.2(2) 3_655 . . . ? O1 Ti1 O2 C22 -61.54(19) 3_655 . . . ? O1 Ti1 O2 C22 81.57(19) . . . . ? N1 Ti1 O2 C22 17.63(17) . . . . ? N1 Ti1 O2 C22 -124.1(3) 3_655 . . . ? O2 Ti1 N1 C11 71.2(3) 3_655 . . . ? O2 Ti1 N1 C11 122.51(14) . . . . ? O1 Ti1 N1 C11 -133.04(13) 3_655 . . . ? O1 Ti1 N1 C11 5.35(13) . . . . ? N1 Ti1 N1 C11 -67.03(12) 3_655 . . . ? O2 Ti1 N1 C21 -42.7(3) 3_655 . . . ? O2 Ti1 N1 C21 8.55(12) . . . . ? O1 Ti1 N1 C21 113.00(13) 3_655 . . . ? O1 Ti1 N1 C21 -108.61(13) . . . . ? N1 Ti1 N1 C21 179.01(14) 3_655 . . . ? O2 Ti1 N1 C1 -162.5(2) 3_655 . . . ? O2 Ti1 N1 C1 -111.24(15) . . . . ? O1 Ti1 N1 C1 -6.80(15) 3_655 . . . ? O1 Ti1 N1 C1 131.59(15) . . . . ? N1 Ti1 N1 C1 59.21(13) 3_655 . . . ? C11 N1 C1 C3 -69.8(3) . . . . ? C21 N1 C1 C3 56.3(2) . . . . ? Ti1 N1 C1 C3 169.64(14) . . . . ? C11 N1 C1 C2 57.3(3) . . . . ? C21 N1 C1 C2 -176.65(19) . . . . ? Ti1 N1 C1 C2 -63.3(2) . . . . ? N1 C1 C3 C4 -119.3(2) . . . . ? C2 C1 C3 C4 111.8(2) . . . . ? N1 C1 C3 C8 68.3(3) . . . . ? C2 C1 C3 C8 -60.6(3) . . . . ? C8 C3 C4 C5 -0.9(3) . . . . ? C1 C3 C4 C5 -173.7(2) . . . . ? C3 C4 C5 C6 -0.4(4) . . . . ? C4 C5 C6 C7 0.6(4) . . . . ? C5 C6 C7 C8 0.6(4) . . . . ? C6 C7 C8 C3 -1.9(4) . . . . ? C4 C3 C8 C7 2.1(3) . . . . ? C1 C3 C8 C7 174.6(2) . . . . ? C21 N1 C11 C12 82.8(2) . . . . ? C1 N1 C11 C12 -150.6(2) . . . . ? Ti1 N1 C11 C12 -23.6(2) . . . . ? Ti1 O1 C12 C13 89.2(2) . . . . ? Ti1 O1 C12 C11 -39.6(3) . . . . ? N1 C11 C12 O1 37.3(2) . . . . ? N1 C11 C12 C13 -90.1(2) . . . . ? O1 C12 C13 C18 -7.4(3) . . . . ? C11 C12 C13 C18 118.3(2) . . . . ? O1 C12 C13 C14 170.2(2) . . . . ? C11 C12 C13 C14 -64.2(3) . . . . ? C18 C13 C14 C15 -0.6(4) . . . . ? C12 C13 C14 C15 -178.3(2) . . . . ? C13 C14 C15 C16 0.0(4) . . . . ? C14 C15 C16 C17 0.8(4) . . . . ? C15 C16 C17 C18 -0.9(4) . . . . ? C14 C13 C18 C17 0.5(4) . . . . ? C12 C13 C18 C17 178.1(2) . . . . ? C16 C17 C18 C13 0.3(4) . . . . ? C11 N1 C21 C22 -137.67(19) . . . . ? C1 N1 C21 C22 94.0(2) . . . . ? Ti1 N1 C21 C22 -28.84(19) . . . . ? Ti1 O2 C22 C23 84.5(2) . . . . ? Ti1 O2 C22 C24 -156.36(16) . . . . ? Ti1 O2 C22 C21 -39.2(2) . . . . ? N1 C21 C22 O2 42.4(2) . . . . ? N1 C21 C22 C23 -78.3(3) . . . . ? N1 C21 C22 C24 159.33(19) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.324 _refine_diff_density_min -0.627 _refine_diff_density_rms 0.048 # Attachment '28.CIF' data_mII _database_code_depnum_ccdc_archive 'CCDC 683795' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H50 N2 O4 Ti' _chemical_formula_sum 'C48 H50 N2 O4 Ti' _chemical_formula_weight 766.80 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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.3503(12) _cell_length_b 17.9768(19) _cell_length_c 20.083(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4097.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5368 _cell_measurement_theta_min 2.266 _cell_measurement_theta_max 29.118 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 0.255 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9508 _exptl_absorpt_correction_T_max 0.9603 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 25710 _diffrn_reflns_av_R_equivalents 0.0925 _diffrn_reflns_av_sigmaI/netI 0.1161 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.00 _reflns_number_total 8944 _reflns_number_gt 6408 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0372P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 8944 _refine_ls_number_parameters 500 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1006 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.1098 _refine_ls_wR_factor_gt 0.1006 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _chemical_absolute_configuration ad loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.27727(5) 0.92439(3) 0.16991(3) 0.01278(13) Uani 1 1 d . . . N1 N 0.3815(2) 0.92762(17) 0.07580(12) 0.0154(6) Uani 1 1 d . . . N2 N 0.2229(2) 0.94936(15) 0.27464(12) 0.0151(6) Uani 1 1 d . . . O11 O 0.24831(18) 1.02000(12) 0.13176(10) 0.0156(5) Uani 1 1 d . . . O12 O 0.31822(19) 0.82430(13) 0.15279(10) 0.0150(5) Uani 1 1 d . . . O21 O 0.4177(2) 0.95207(13) 0.21413(11) 0.0154(5) Uani 1 1 d . . . O22 O 0.11625(17) 0.90129(12) 0.17086(11) 0.0155(5) Uani 1 1 d . . . C1 C 0.3014(3) 0.9077(2) 0.02064(15) 0.0205(8) Uani 1 1 d . . . H1A H 0.3476 0.8971 -0.0194 0.031 Uiso 1 1 calc R . . H1B H 0.2478 0.9493 0.0118 0.031 Uiso 1 1 calc R . . H1C H 0.2555 0.8636 0.0330 0.031 Uiso 1 1 calc R . . C2 C 0.2431(3) 0.88311(18) 0.31823(15) 0.0189(8) Uani 1 1 d . . . H2A H 0.2039 0.8908 0.3612 0.028 Uiso 1 1 calc R . . H2B H 0.3278 0.8764 0.3254 0.028 Uiso 1 1 calc R . . H2C H 0.2107 0.8387 0.2967 0.028 Uiso 1 1 calc R . . C11 C 0.4261(3) 0.9969(2) 0.27201(16) 0.0180(8) Uani 1 1 d . . . H11A H 0.4610 1.0454 0.2575 0.022 Uiso 1 1 calc R . . C12 C 0.2978(3) 1.01399(19) 0.29419(15) 0.0161(8) Uani 1 1 d . . . H12A H 0.2711 1.0564 0.2657 0.019 Uiso 1 1 calc R . . C13 C 0.2826(3) 1.0402(2) 0.36566(16) 0.0259(9) Uani 1 1 d . . . H13A H 0.1995 1.0520 0.3738 0.039 Uiso 1 1 calc R . . H13B H 0.3305 1.0848 0.3730 0.039 Uiso 1 1 calc R . . H13C H 0.3079 1.0009 0.3962 0.039 Uiso 1 1 calc R . . C14 C 0.5120(3) 0.96334(19) 0.32258(17) 0.0156(7) Uani 1 1 d . . . C15 C 0.5575(3) 1.0080(2) 0.37314(18) 0.0273(9) Uani 1 1 d . . . H15A H 0.5335 1.0585 0.3767 0.033 Uiso 1 1 calc R . . C16 C 0.6382(3) 0.9788(2) 0.41858(18) 0.0295(10) Uani 1 1 d . . . H16A H 0.6665 1.0090 0.4539 0.035 Uiso 1 1 calc R . . C17 C 0.6773(3) 0.9063(2) 0.41271(17) 0.0255(9) Uani 1 1 d . . . H17A H 0.7330 0.8869 0.4435 0.031 Uiso 1 1 calc R . . C18 C 0.6348(3) 0.8623(2) 0.36171(17) 0.0198(8) Uani 1 1 d . . . H18A H 0.6614 0.8125 0.3573 0.024 Uiso 1 1 calc R . . C19 C 0.5533(3) 0.8907(2) 0.31673(16) 0.0171(8) Uani 1 1 d . . . H19A H 0.5254 0.8601 0.2815 0.020 Uiso 1 1 calc R . . C21 C 0.3350(3) 1.06033(18) 0.09816(15) 0.0134(7) Uani 1 1 d . . . H21A H 0.3762 1.0912 0.1324 0.016 Uiso 1 1 calc R . . C22 C 0.4299(3) 1.0043(2) 0.06962(16) 0.0169(8) Uani 1 1 d . . . H22A H 0.4982 1.0067 0.1010 0.020 Uiso 1 1 calc R . . C23 C 0.4800(3) 1.0232(2) 0.00057(17) 0.0258(9) Uani 1 1 d . . . H23A H 0.5352 0.9842 -0.0132 0.039 Uiso 1 1 calc R . . H23B H 0.5213 1.0710 0.0026 0.039 Uiso 1 1 calc R . . H23C H 0.4155 1.0265 -0.0317 0.039 Uiso 1 1 calc R . . C24 C 0.2820(3) 1.11473(19) 0.04758(15) 0.0171(7) Uani 1 1 d . . . C25 C 0.1702(3) 1.1036(2) 0.02054(16) 0.0210(8) Uani 1 1 d . . . H25A H 0.1260 1.0607 0.0325 0.025 Uiso 1 1 calc R . . C26 C 0.1236(4) 1.1549(2) -0.02375(18) 0.0294(10) Uani 1 1 d . . . H26A H 0.0474 1.1469 -0.0420 0.035 Uiso 1 1 calc R . . C27 C 0.1866(4) 1.2176(2) -0.04170(18) 0.0311(10) Uani 1 1 d . . . H27A H 0.1541 1.2523 -0.0724 0.037 Uiso 1 1 calc R . . C28 C 0.2967(4) 1.2296(2) -0.01485(18) 0.0325(10) Uani 1 1 d . . . H28A H 0.3409 1.2723 -0.0273 0.039 Uiso 1 1 calc R . . C29 C 0.3429(3) 1.1792(2) 0.03038(18) 0.0244(9) Uani 1 1 d . . . H29A H 0.4175 1.1887 0.0500 0.029 Uiso 1 1 calc R . . C31 C 0.4184(3) 0.8006(2) 0.11738(16) 0.0163(8) Uani 1 1 d . . . C32 C 0.4745(3) 0.8715(2) 0.08614(16) 0.0163(8) Uani 1 1 d . . . H32A H 0.5359 0.8915 0.1162 0.020 Uiso 1 1 calc R . . H32B H 0.5119 0.8589 0.0431 0.020 Uiso 1 1 calc R . . C33 C 0.5033(3) 0.76399(18) 0.16741(16) 0.0150(7) Uani 1 1 d . . . C34 C 0.6255(3) 0.76761(19) 0.16041(17) 0.0194(8) Uani 1 1 d . . . H34A H 0.6589 0.7921 0.1230 0.023 Uiso 1 1 calc R . . C35 C 0.6984(3) 0.7355(2) 0.20800(17) 0.0224(8) Uani 1 1 d . . . H35A H 0.7815 0.7387 0.2031 0.027 Uiso 1 1 calc R . . C36 C 0.6512(3) 0.6989(2) 0.26231(18) 0.0233(9) Uani 1 1 d . . . H36A H 0.7015 0.6774 0.2948 0.028 Uiso 1 1 calc R . . C37 C 0.5299(3) 0.6939(2) 0.26901(18) 0.0221(9) Uani 1 1 d . . . H37A H 0.4970 0.6689 0.3063 0.027 Uiso 1 1 calc R . . C38 C 0.4562(3) 0.7254(2) 0.22158(17) 0.0191(8) Uani 1 1 d . . . H38A H 0.3732 0.7207 0.2260 0.023 Uiso 1 1 calc R . . C41 C 0.0339(3) 0.9144(2) 0.22176(16) 0.0154(8) Uani 1 1 d . . . C42 C 0.0965(3) 0.9692(2) 0.27074(17) 0.0167(8) Uani 1 1 d . . . H42A H 0.0878 1.0210 0.2546 0.020 Uiso 1 1 calc R . . H42B H 0.0601 0.9658 0.3154 0.020 Uiso 1 1 calc R . . C43 C -0.0733(3) 0.95625(19) 0.19201(16) 0.0159(8) Uani 1 1 d . . . C44 C -0.0498(3) 1.0103(2) 0.14407(17) 0.0196(8) Uani 1 1 d . . . H44A H 0.0293 1.0184 0.1304 0.023 Uiso 1 1 calc R . . C45 C -0.1392(3) 1.0526(2) 0.11569(18) 0.0230(9) Uani 1 1 d . . . H45A H -0.1215 1.0885 0.0824 0.028 Uiso 1 1 calc R . . C46 C -0.2544(3) 1.0420(2) 0.13649(17) 0.0213(8) Uani 1 1 d . . . H46A H -0.3162 1.0714 0.1184 0.026 Uiso 1 1 calc R . . C47 C -0.2788(3) 0.9881(2) 0.18387(16) 0.0229(8) Uani 1 1 d . . . H47A H -0.3578 0.9805 0.1979 0.027 Uiso 1 1 calc R . . C48 C -0.1895(3) 0.9451(2) 0.21102(16) 0.0207(8) Uani 1 1 d . . . H48A H -0.2079 0.9077 0.2428 0.025 Uiso 1 1 calc R . . C51 C 0.0001(3) 0.8405(2) 0.25587(18) 0.0194(8) Uani 1 1 d . . . C52 C -0.0568(3) 0.8380(2) 0.31760(18) 0.0258(9) Uani 1 1 d . . . H52A H -0.0801 0.8831 0.3384 0.031 Uiso 1 1 calc R . . C53 C -0.0798(3) 0.7710(2) 0.3490(2) 0.0331(10) Uani 1 1 d . . . H53A H -0.1190 0.7705 0.3908 0.040 Uiso 1 1 calc R . . C54 C -0.0455(3) 0.7042(2) 0.3194(2) 0.0365(11) Uani 1 1 d . . . H54A H -0.0599 0.6581 0.3411 0.044 Uiso 1 1 calc R . . C55 C 0.0096(3) 0.7060(2) 0.2581(2) 0.0319(10) Uani 1 1 d . . . H55A H 0.0324 0.6608 0.2373 0.038 Uiso 1 1 calc R . . C56 C 0.0324(3) 0.7736(2) 0.22629(19) 0.0245(9) Uani 1 1 d . . . H56A H 0.0702 0.7739 0.1841 0.029 Uiso 1 1 calc R . . C61 C 0.3856(3) 0.7417(2) 0.06520(17) 0.0180(8) Uani 1 1 d . . . C62 C 0.2762(3) 0.7078(2) 0.06707(17) 0.0229(8) Uani 1 1 d . . . H62A H 0.2211 0.7213 0.1006 0.027 Uiso 1 1 calc R . . C63 C 0.2466(3) 0.6541(2) 0.02010(18) 0.0288(9) Uani 1 1 d . . . H63A H 0.1719 0.6305 0.0225 0.035 Uiso 1 1 calc R . . C64 C 0.3239(4) 0.6347(2) -0.02992(19) 0.0331(11) Uani 1 1 d . . . H64A H 0.3015 0.5994 -0.0627 0.040 Uiso 1 1 calc R . . C65 C 0.4335(4) 0.6669(2) -0.03197(19) 0.0337(11) Uani 1 1 d . . . H65A H 0.4874 0.6535 -0.0661 0.040 Uiso 1 1 calc R . . C66 C 0.4658(4) 0.7193(2) 0.01617(18) 0.0262(9) Uani 1 1 d . . . H66A H 0.5428 0.7399 0.0156 0.031 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0134(3) 0.0144(3) 0.0106(3) 0.0001(3) 0.0002(3) 0.0004(3) N1 0.0143(15) 0.0168(16) 0.0152(14) 0.0012(13) 0.0004(11) 0.0018(14) N2 0.0153(14) 0.0158(15) 0.0141(13) 0.0025(11) -0.0005(12) 0.0029(14) O11 0.0173(13) 0.0150(13) 0.0146(11) 0.0019(9) 0.0026(9) 0.0024(10) O12 0.0145(12) 0.0157(13) 0.0147(12) -0.0008(9) 0.0016(9) 0.0022(10) O21 0.0160(12) 0.0191(14) 0.0110(12) -0.0027(10) -0.0005(10) -0.0014(11) O22 0.0146(11) 0.0176(13) 0.0144(12) -0.0013(10) 0.0031(10) -0.0021(10) C1 0.027(2) 0.023(2) 0.0118(16) -0.0027(14) -0.0010(15) 0.0002(17) C2 0.0191(19) 0.0191(19) 0.0185(18) 0.0046(14) 0.0001(14) 0.0016(15) C11 0.020(2) 0.017(2) 0.0163(18) 0.0017(16) 0.0002(15) -0.0039(17) C12 0.0190(19) 0.0122(18) 0.0172(17) 0.0002(14) -0.0050(15) 0.0019(16) C13 0.027(2) 0.027(2) 0.0234(19) -0.0081(16) 0.0017(18) 0.008(2) C14 0.0123(16) 0.0196(19) 0.0149(17) -0.0021(15) 0.0004(14) -0.0025(15) C15 0.035(2) 0.021(2) 0.026(2) -0.0057(17) -0.0069(18) 0.0002(18) C16 0.035(2) 0.033(3) 0.021(2) -0.0084(18) -0.0122(17) -0.002(2) C17 0.020(2) 0.033(3) 0.024(2) 0.0057(17) -0.0055(16) 0.0027(18) C18 0.0160(19) 0.024(2) 0.0198(19) 0.0012(15) 0.0024(15) 0.0002(16) C19 0.0152(18) 0.023(2) 0.0131(19) 0.0001(15) 0.0018(14) -0.0017(16) C21 0.0148(17) 0.013(2) 0.0120(16) -0.0028(14) -0.0003(13) 0.0004(15) C22 0.0152(19) 0.019(2) 0.0169(18) 0.0036(15) -0.0013(15) -0.0011(16) C23 0.030(2) 0.021(2) 0.026(2) 0.0109(17) 0.0143(17) 0.0055(18) C24 0.0235(19) 0.0159(19) 0.0120(16) -0.0040(13) 0.0037(16) 0.0001(17) C25 0.022(2) 0.022(2) 0.0186(19) -0.0035(16) 0.0032(16) 0.0052(17) C26 0.029(2) 0.039(3) 0.020(2) 0.0001(19) -0.0022(17) 0.013(2) C27 0.046(3) 0.029(3) 0.018(2) 0.0070(17) 0.0074(18) 0.022(2) C28 0.051(3) 0.020(2) 0.026(2) 0.0056(17) 0.015(2) 0.005(2) C29 0.029(2) 0.021(2) 0.023(2) 0.0018(17) 0.0038(17) 0.0015(17) C31 0.0163(18) 0.019(2) 0.0131(18) 0.0003(15) -0.0002(14) 0.0022(16) C32 0.0128(18) 0.021(2) 0.0148(18) 0.0002(15) 0.0033(14) 0.0033(16) C33 0.0163(16) 0.0155(18) 0.0133(17) -0.0026(15) -0.0005(15) 0.0009(14) C34 0.0244(19) 0.0158(19) 0.0179(19) 0.0046(15) 0.0014(15) -0.0014(16) C35 0.0164(19) 0.018(2) 0.033(2) 0.0051(16) -0.0003(16) 0.0044(16) C36 0.027(2) 0.019(2) 0.024(2) 0.0004(16) -0.0106(16) 0.0022(18) C37 0.029(2) 0.017(2) 0.021(2) 0.0046(16) -0.0026(16) -0.0007(18) C38 0.024(2) 0.012(2) 0.0219(19) 0.0000(15) -0.0005(16) -0.0004(16) C41 0.0137(17) 0.016(2) 0.0166(17) -0.0021(15) 0.0037(14) 0.0047(16) C42 0.0164(18) 0.016(2) 0.0182(19) -0.0001(15) 0.0037(15) 0.0075(16) C43 0.0166(18) 0.018(2) 0.0127(17) -0.0046(14) 0.0020(14) -0.0002(16) C44 0.0136(17) 0.019(2) 0.0263(19) 0.0015(16) 0.0005(15) -0.0025(15) C45 0.024(2) 0.019(2) 0.026(2) 0.0054(16) -0.0024(16) -0.0017(17) C46 0.0144(19) 0.022(2) 0.0276(19) -0.0022(16) -0.0051(15) 0.0042(16) C47 0.0151(17) 0.031(2) 0.0222(19) -0.0009(16) 0.0022(16) 0.0029(18) C48 0.021(2) 0.024(2) 0.0166(17) 0.0016(15) 0.0026(14) -0.0018(16) C51 0.0097(17) 0.022(2) 0.026(2) 0.0087(16) 0.0009(15) -0.0005(17) C52 0.0205(19) 0.030(2) 0.027(2) 0.0079(18) 0.0011(16) 0.0021(18) C53 0.0145(19) 0.043(3) 0.041(3) 0.015(2) 0.0011(17) 0.001(2) C54 0.020(2) 0.034(3) 0.056(3) 0.025(2) -0.004(2) -0.0005(18) C55 0.025(2) 0.018(2) 0.053(3) 0.0053(19) 0.000(2) 0.0018(19) C56 0.019(2) 0.027(2) 0.028(2) 0.0014(18) 0.0015(16) -0.0006(18) C61 0.021(2) 0.015(2) 0.0176(18) -0.0006(15) -0.0046(15) 0.0047(16) C62 0.0218(19) 0.021(2) 0.0259(19) -0.0037(15) -0.0065(17) 0.0065(18) C63 0.029(2) 0.022(2) 0.035(2) -0.0035(17) -0.0130(18) 0.0004(18) C64 0.054(3) 0.022(2) 0.023(2) -0.0075(17) -0.021(2) 0.007(2) C65 0.057(3) 0.028(3) 0.017(2) -0.0065(18) 0.0012(19) 0.008(2) C66 0.036(2) 0.022(2) 0.021(2) -0.0029(16) 0.0030(17) 0.0017(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O22 1.874(2) . ? Ti1 O12 1.890(2) . ? Ti1 O21 1.891(2) . ? Ti1 O11 1.910(2) . ? Ti1 N1 2.231(3) . ? Ti1 N2 2.237(3) . ? N1 C32 1.475(4) . ? N1 C1 1.477(4) . ? N1 C22 1.489(4) . ? N2 C42 1.480(4) . ? N2 C12 1.492(4) . ? N2 C2 1.496(4) . ? O11 C21 1.396(4) . ? O12 C31 1.407(4) . ? O21 C11 1.418(4) . ? O22 C41 1.405(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C11 C14 1.532(5) . ? C11 C12 1.553(5) . ? C11 H11A 1.0000 . ? C12 C13 1.521(4) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C19 1.393(5) . ? C14 C15 1.394(5) . ? C15 C16 1.396(5) . ? C15 H15A 0.9500 . ? C16 C17 1.382(5) . ? C16 H16A 0.9500 . ? C17 C18 1.381(5) . ? C17 H17A 0.9500 . ? C18 C19 1.390(5) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C21 C24 1.533(5) . ? C21 C22 1.582(5) . ? C21 H21A 1.0000 . ? C22 C23 1.537(4) . ? C22 H22A 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C29 1.392(5) . ? C24 C25 1.394(5) . ? C25 C26 1.387(5) . ? C25 H25A 0.9500 . ? C26 C27 1.383(6) . ? C26 H26A 0.9500 . ? C27 C28 1.379(6) . ? C27 H27A 0.9500 . ? C28 C29 1.387(5) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C31 C61 1.536(5) . ? C31 C33 1.539(5) . ? C31 C32 1.557(5) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.396(4) . ? C33 C38 1.396(5) . ? C34 C35 1.390(5) . ? C34 H34A 0.9500 . ? C35 C36 1.382(5) . ? C35 H35A 0.9500 . ? C36 C37 1.386(5) . ? C36 H36A 0.9500 . ? C37 C38 1.388(5) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C41 C51 1.543(5) . ? C41 C43 1.551(5) . ? C41 C42 1.564(5) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C48 1.387(5) . ? C43 C44 1.393(5) . ? C44 C45 1.390(5) . ? C44 H44A 0.9500 . ? C45 C46 1.386(5) . ? C45 H45A 0.9500 . ? C46 C47 1.386(5) . ? C46 H46A 0.9500 . ? C47 C48 1.387(5) . ? C47 H47A 0.9500 . ? C48 H48A 0.9500 . ? C51 C56 1.390(6) . ? C51 C52 1.398(5) . ? C52 C53 1.383(5) . ? C52 H52A 0.9500 . ? C53 C54 1.396(6) . ? C53 H53A 0.9500 . ? C54 C55 1.382(6) . ? C54 H54A 0.9500 . ? C55 C56 1.397(5) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? C61 C62 1.383(5) . ? C61 C66 1.400(5) . ? C62 C63 1.391(5) . ? C62 H62A 0.9500 . ? C63 C64 1.378(6) . ? C63 H63A 0.9500 . ? C64 C65 1.372(6) . ? C64 H64A 0.9500 . ? C65 C66 1.399(5) . ? C65 H65A 0.9500 . ? C66 H66A 0.9500 . ? 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 O22 Ti1 O12 91.76(10) . . ? O22 Ti1 O21 151.08(10) . . ? O12 Ti1 O21 97.39(10) . . ? O22 Ti1 O11 92.05(9) . . ? O12 Ti1 O11 145.68(9) . . ? O21 Ti1 O11 95.55(10) . . ? O22 Ti1 N1 122.10(10) . . ? O12 Ti1 N1 74.93(10) . . ? O21 Ti1 N1 86.80(10) . . ? O11 Ti1 N1 74.21(10) . . ? O22 Ti1 N2 76.47(10) . . ? O12 Ti1 N2 115.46(10) . . ? O21 Ti1 N2 74.82(10) . . ? O11 Ti1 N2 98.58(9) . . ? N1 Ti1 N2 159.66(10) . . ? C32 N1 C1 112.4(3) . . ? C32 N1 C22 112.4(3) . . ? C1 N1 C22 112.9(3) . . ? C32 N1 Ti1 104.03(18) . . ? C1 N1 Ti1 107.61(19) . . ? C22 N1 Ti1 106.88(19) . . ? C42 N2 C12 112.2(3) . . ? C42 N2 C2 111.8(3) . . ? C12 N2 C2 112.3(2) . . ? C42 N2 Ti1 105.43(19) . . ? C12 N2 Ti1 104.27(18) . . ? C2 N2 Ti1 110.38(19) . . ? C21 O11 Ti1 122.66(19) . . ? C31 O12 Ti1 125.4(2) . . ? C11 O21 Ti1 126.3(2) . . ? C41 O22 Ti1 128.2(2) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N2 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O21 C11 C14 111.2(3) . . ? O21 C11 C12 106.5(3) . . ? C14 C11 C12 119.0(3) . . ? O21 C11 H11A 106.5 . . ? C14 C11 H11A 106.5 . . ? C12 C11 H11A 106.5 . . ? N2 C12 C13 115.2(3) . . ? N2 C12 C11 107.8(3) . . ? C13 C12 C11 116.0(3) . . ? N2 C12 H12A 105.7 . . ? C13 C12 H12A 105.7 . . ? C11 C12 H12A 105.7 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C14 C15 118.5(3) . . ? C19 C14 C11 121.9(3) . . ? C15 C14 C11 119.4(3) . . ? C14 C15 C16 120.1(4) . . ? C14 C15 H15A 119.9 . . ? C16 C15 H15A 119.9 . . ? C17 C16 C15 120.7(4) . . ? C17 C16 H16A 119.6 . . ? C15 C16 H16A 119.6 . . ? C18 C17 C16 119.4(3) . . ? C18 C17 H17A 120.3 . . ? C16 C17 H17A 120.3 . . ? C17 C18 C19 120.3(4) . . ? C17 C18 H18A 119.8 . . ? C19 C18 H18A 119.8 . . ? C18 C19 C14 120.9(3) . . ? C18 C19 H19A 119.6 . . ? C14 C19 H19A 119.6 . . ? O11 C21 C24 112.0(3) . . ? O11 C21 C22 108.9(3) . . ? C24 C21 C22 115.7(3) . . ? O11 C21 H21A 106.6 . . ? C24 C21 H21A 106.6 . . ? C22 C21 H21A 106.6 . . ? N1 C22 C23 114.6(3) . . ? N1 C22 C21 107.9(3) . . ? C23 C22 C21 116.0(3) . . ? N1 C22 H22A 105.8 . . ? C23 C22 H22A 105.8 . . ? C21 C22 H22A 105.8 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C29 C24 C25 118.3(3) . . ? C29 C24 C21 120.0(3) . . ? C25 C24 C21 121.6(3) . . ? C26 C25 C24 120.1(4) . . ? C26 C25 H25A 120.0 . . ? C24 C25 H25A 120.0 . . ? C27 C26 C25 120.8(4) . . ? C27 C26 H26A 119.6 . . ? C25 C26 H26A 119.6 . . ? C28 C27 C26 119.6(4) . . ? C28 C27 H27A 120.2 . . ? C26 C27 H27A 120.2 . . ? C27 C28 C29 119.8(4) . . ? C27 C28 H28A 120.1 . . ? C29 C28 H28A 120.1 . . ? C28 C29 C24 121.3(4) . . ? C28 C29 H29A 119.4 . . ? C24 C29 H29A 119.4 . . ? O12 C31 C61 110.9(3) . . ? O12 C31 C33 107.8(3) . . ? C61 C31 C33 107.6(3) . . ? O12 C31 C32 106.6(3) . . ? C61 C31 C32 112.9(3) . . ? C33 C31 C32 110.9(3) . . ? N1 C32 C31 108.9(3) . . ? N1 C32 H32A 109.9 . . ? C31 C32 H32A 109.9 . . ? N1 C32 H32B 109.9 . . ? C31 C32 H32B 109.9 . . ? H32A C32 H32B 108.3 . . ? C34 C33 C38 118.8(3) . . ? C34 C33 C31 122.4(3) . . ? C38 C33 C31 118.8(3) . . ? C35 C34 C33 120.2(3) . . ? C35 C34 H34A 119.9 . . ? C33 C34 H34A 119.9 . . ? C36 C35 C34 120.6(3) . . ? C36 C35 H35A 119.7 . . ? C34 C35 H35A 119.7 . . ? C35 C36 C37 119.5(3) . . ? C35 C36 H36A 120.2 . . ? C37 C36 H36A 120.2 . . ? C36 C37 C38 120.3(3) . . ? C36 C37 H37A 119.8 . . ? C38 C37 H37A 119.8 . . ? C37 C38 C33 120.4(3) . . ? C37 C38 H38A 119.8 . . ? C33 C38 H38A 119.8 . . ? O22 C41 C51 110.2(3) . . ? O22 C41 C43 108.8(3) . . ? C51 C41 C43 113.2(3) . . ? O22 C41 C42 105.1(3) . . ? C51 C41 C42 112.1(3) . . ? C43 C41 C42 107.0(3) . . ? N2 C42 C41 108.7(3) . . ? N2 C42 H42A 109.9 . . ? C41 C42 H42A 109.9 . . ? N2 C42 H42B 109.9 . . ? C41 C42 H42B 109.9 . . ? H42A C42 H42B 108.3 . . ? C48 C43 C44 118.2(3) . . ? C48 C43 C41 124.7(3) . . ? C44 C43 C41 117.0(3) . . ? C45 C44 C43 121.7(3) . . ? C45 C44 H44A 119.2 . . ? C43 C44 H44A 119.2 . . ? C46 C45 C44 119.3(3) . . ? C46 C45 H45A 120.4 . . ? C44 C45 H45A 120.4 . . ? C47 C46 C45 119.5(3) . . ? C47 C46 H46A 120.3 . . ? C45 C46 H46A 120.3 . . ? C46 C47 C48 120.9(3) . . ? C46 C47 H47A 119.6 . . ? C48 C47 H47A 119.6 . . ? C43 C48 C47 120.4(3) . . ? C43 C48 H48A 119.8 . . ? C47 C48 H48A 119.8 . . ? C56 C51 C52 118.2(4) . . ? C56 C51 C41 119.3(3) . . ? C52 C51 C41 122.4(3) . . ? C53 C52 C51 121.3(4) . . ? C53 C52 H52A 119.4 . . ? C51 C52 H52A 119.4 . . ? C52 C53 C54 120.2(4) . . ? C52 C53 H53A 119.9 . . ? C54 C53 H53A 119.9 . . ? C55 C54 C53 119.0(4) . . ? C55 C54 H54A 120.5 . . ? C53 C54 H54A 120.5 . . ? C54 C55 C56 120.8(4) . . ? C54 C55 H55A 119.6 . . ? C56 C55 H55A 119.6 . . ? C51 C56 C55 120.5(4) . . ? C51 C56 H56A 119.7 . . ? C55 C56 H56A 119.7 . . ? C62 C61 C66 118.4(3) . . ? C62 C61 C31 120.2(3) . . ? C66 C61 C31 121.4(3) . . ? C61 C62 C63 120.3(4) . . ? C61 C62 H62A 119.9 . . ? C63 C62 H62A 119.9 . . ? C64 C63 C62 121.1(4) . . ? C64 C63 H63A 119.5 . . ? C62 C63 H63A 119.5 . . ? C65 C64 C63 119.5(4) . . ? C65 C64 H64A 120.3 . . ? C63 C64 H64A 120.3 . . ? C64 C65 C66 120.0(4) . . ? C64 C65 H65A 120.0 . . ? C66 C65 H65A 120.0 . . ? C65 C66 C61 120.6(4) . . ? C65 C66 H66A 119.7 . . ? C61 C66 H66A 119.7 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.332 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.063 # Attachment '31.CIF' data_t _database_code_depnum_ccdc_archive 'CCDC 683796' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H58 N2 O4 Ti, C H2 Cl2' _chemical_formula_sum 'C63 H60 Cl2 N2 O4 Ti' _chemical_formula_weight 1027.93 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.9885(5) _cell_length_b 19.3301(9) _cell_length_c 22.2363(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5153.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5909 _cell_measurement_theta_min 2.199 _cell_measurement_theta_max 29.997 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 0.322 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9384 _exptl_absorpt_correction_T_max 0.9563 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38038 _diffrn_reflns_av_R_equivalents 0.0682 _diffrn_reflns_av_sigmaI/netI 0.0958 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 29.50 _reflns_number_total 14137 _reflns_number_gt 10347 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0368P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 14137 _refine_ls_number_parameters 649 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0896 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1008 _refine_ls_wR_factor_gt 0.0924 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 Ti Ti 0.69698(3) 0.25429(2) 0.189743(18) 0.01202(9) Uani 1 1 d . . . N1 N 0.57958(16) 0.17645(10) 0.24106(9) 0.0137(4) Uani 1 1 d . . . N2 N 0.81733(16) 0.27212(9) 0.10594(9) 0.0138(4) Uani 1 1 d . . . O11 O 0.69785(14) 0.28104(8) 0.27230(7) 0.0161(4) Uani 1 1 d . . . O12 O 0.58023(12) 0.23358(9) 0.13754(7) 0.0152(4) Uani 1 1 d . . . O21 O 0.70669(14) 0.35011(8) 0.17694(7) 0.0160(4) Uani 1 1 d . . . O22 O 0.80549(13) 0.18537(8) 0.19300(7) 0.0151(3) Uani 1 1 d . . . C11 C 0.63199(19) 0.25895(13) 0.32051(10) 0.0153(5) Uani 1 1 d . . . C12 C 0.60088(19) 0.18283(12) 0.30689(11) 0.0148(5) Uani 1 1 d . . . H12A H 0.5338 0.1685 0.3305 0.018 Uiso 1 1 calc R . . C13 C 0.6979(2) 0.13261(12) 0.31738(11) 0.0169(5) Uani 1 1 d . . . H13A H 0.6940 0.1126 0.3583 0.020 Uiso 1 1 calc R . . H13B H 0.7703 0.1566 0.3127 0.020 Uiso 1 1 calc R . . C14 C 0.6848(2) 0.07573(12) 0.26953(11) 0.0159(5) Uani 1 1 d . . . H14A H 0.7548 0.0698 0.2465 0.019 Uiso 1 1 calc R . . H14B H 0.6649 0.0310 0.2884 0.019 Uiso 1 1 calc R . . C15 C 0.59063(19) 0.10108(12) 0.22858(12) 0.0161(5) Uani 1 1 d . . . H15A H 0.6096 0.0931 0.1858 0.019 Uiso 1 1 calc R . . H15B H 0.5201 0.0766 0.2379 0.019 Uiso 1 1 calc R . . C16 C 0.47065(19) 0.20368(13) 0.22198(11) 0.0136(5) Uani 1 1 d . . . H16A H 0.4568 0.2490 0.2413 0.016 Uiso 1 1 calc R . . H16B H 0.4107 0.1715 0.2344 0.016 Uiso 1 1 calc R . . C17 C 0.47032(19) 0.21200(12) 0.15276(11) 0.0133(5) Uani 1 1 d . . . C21 C 0.77733(19) 0.39129(12) 0.14179(11) 0.0147(5) Uani 1 1 d . . . C22 C 0.8112(2) 0.34607(12) 0.08628(11) 0.0143(5) Uani 1 1 d . . . H22A H 0.8854 0.3614 0.0706 0.017 Uiso 1 1 calc R . . C23 C 0.7251(2) 0.34698(13) 0.03577(12) 0.0193(6) Uani 1 1 d . . . H23A H 0.7490 0.3787 0.0033 0.023 Uiso 1 1 calc R . . H23B H 0.6519 0.3628 0.0512 0.023 Uiso 1 1 calc R . . C24 C 0.7163(2) 0.27298(13) 0.01201(12) 0.0217(6) Uani 1 1 d . . . H24A H 0.6389 0.2557 0.0158 0.026 Uiso 1 1 calc R . . H24B H 0.7387 0.2709 -0.0308 0.026 Uiso 1 1 calc R . . C25 C 0.7948(2) 0.23048(12) 0.05042(11) 0.0178(5) Uani 1 1 d . . . H25A H 0.7601 0.1857 0.0611 0.021 Uiso 1 1 calc R . . H25B H 0.8651 0.2213 0.0285 0.021 Uiso 1 1 calc R . . C26 C 0.92534(18) 0.25330(13) 0.13319(11) 0.0152(5) Uani 1 1 d . . . H26A H 0.9492 0.2900 0.1615 0.018 Uiso 1 1 calc R . . H26B H 0.9828 0.2489 0.1014 0.018 Uiso 1 1 calc R . . C27 C 0.91336(19) 0.18354(13) 0.16730(11) 0.0142(5) Uani 1 1 d . . . C31 C 0.6976(2) 0.26408(12) 0.37974(10) 0.0166(5) Uani 1 1 d . . . C32 C 0.7963(2) 0.30156(13) 0.38220(12) 0.0236(6) Uani 1 1 d . . . H32A H 0.8232 0.3240 0.3471 0.028 Uiso 1 1 calc R . . C33 C 0.8559(2) 0.30649(15) 0.43551(14) 0.0308(7) Uani 1 1 d . . . H33A H 0.9230 0.3325 0.4367 0.037 Uiso 1 1 calc R . . C34 C 0.8184(3) 0.27388(14) 0.48692(13) 0.0290(7) Uani 1 1 d . . . H34A H 0.8601 0.2769 0.5232 0.035 Uiso 1 1 calc R . . C35 C 0.7202(2) 0.23698(15) 0.48535(12) 0.0292(7) Uani 1 1 d . . . H35A H 0.6938 0.2146 0.5206 0.035 Uiso 1 1 calc R . . C36 C 0.6597(2) 0.23249(14) 0.43218(12) 0.0237(6) Uani 1 1 d . . . H36A H 0.5915 0.2075 0.4316 0.028 Uiso 1 1 calc R . . C41 C 0.5298(2) 0.30740(13) 0.32668(11) 0.0182(5) Uani 1 1 d . . . C42 C 0.5335(2) 0.37225(14) 0.29980(14) 0.0308(7) Uani 1 1 d . . . H42A H 0.5992 0.3865 0.2795 0.037 Uiso 1 1 calc R . . C43 C 0.4431(3) 0.41606(16) 0.30225(18) 0.0466(9) Uani 1 1 d . . . H43A H 0.4471 0.4600 0.2833 0.056 Uiso 1 1 calc R . . C44 C 0.3469(3) 0.39683(18) 0.33190(15) 0.0403(8) Uani 1 1 d . . . H44A H 0.2847 0.4272 0.3334 0.048 Uiso 1 1 calc R . . C45 C 0.3422(3) 0.33292(17) 0.35939(14) 0.0391(8) Uani 1 1 d . . . H45A H 0.2767 0.3194 0.3804 0.047 Uiso 1 1 calc R . . C46 C 0.4326(2) 0.28830(15) 0.35649(13) 0.0292(7) Uani 1 1 d . . . H46A H 0.4280 0.2441 0.3751 0.035 Uiso 1 1 calc R . . C51 C 0.4411(2) 0.14451(13) 0.11969(11) 0.0162(5) Uani 1 1 d . . . C52 C 0.3473(2) 0.10601(14) 0.13693(13) 0.0227(6) Uani 1 1 d . . . H52A H 0.2988 0.1233 0.1671 0.027 Uiso 1 1 calc R . . C53 C 0.3250(2) 0.04241(14) 0.10995(14) 0.0295(7) Uani 1 1 d . . . H53A H 0.2623 0.0161 0.1226 0.035 Uiso 1 1 calc R . . C54 C 0.3929(3) 0.01744(15) 0.06531(14) 0.0323(7) Uani 1 1 d . . . H54A H 0.3777 -0.0262 0.0474 0.039 Uiso 1 1 calc R . . C55 C 0.4834(3) 0.05613(16) 0.04658(13) 0.0323(7) Uani 1 1 d . . . H55A H 0.5298 0.0392 0.0152 0.039 Uiso 1 1 calc R . . C56 C 0.5074(2) 0.11991(14) 0.07339(12) 0.0224(6) Uani 1 1 d . . . H56A H 0.5693 0.1464 0.0598 0.027 Uiso 1 1 calc R . . C61 C 0.38722(19) 0.26852(12) 0.13518(11) 0.0147(5) Uani 1 1 d . . . C62 C 0.4148(2) 0.31622(14) 0.09061(12) 0.0200(6) Uani 1 1 d . . . H62A H 0.4854 0.3136 0.0714 0.024 Uiso 1 1 calc R . . C63 C 0.3401(2) 0.36753(13) 0.07405(12) 0.0219(6) Uani 1 1 d . . . H63A H 0.3597 0.3997 0.0435 0.026 Uiso 1 1 calc R . . C64 C 0.2373(2) 0.37200(14) 0.10171(12) 0.0232(6) Uani 1 1 d . . . H64A H 0.1859 0.4068 0.0897 0.028 Uiso 1 1 calc R . . C65 C 0.2088(2) 0.32570(13) 0.14717(13) 0.0235(6) Uani 1 1 d . . . H65A H 0.1389 0.3295 0.1670 0.028 Uiso 1 1 calc R . . C66 C 0.2830(2) 0.27418(13) 0.16327(12) 0.0193(6) Uani 1 1 d . . . H66A H 0.2630 0.2421 0.1938 0.023 Uiso 1 1 calc R . . C71 C 0.7132(2) 0.45635(12) 0.12125(11) 0.0150(5) Uani 1 1 d . . . C72 C 0.7617(2) 0.50626(13) 0.08442(13) 0.0223(6) Uani 1 1 d . . . H72A H 0.8374 0.5014 0.0726 0.027 Uiso 1 1 calc R . . C73 C 0.7011(2) 0.56293(13) 0.06481(12) 0.0241(6) Uani 1 1 d . . . H73A H 0.7356 0.5964 0.0396 0.029 Uiso 1 1 calc R . . C74 C 0.5910(2) 0.57121(14) 0.08152(13) 0.0235(6) Uani 1 1 d . . . H74A H 0.5499 0.6104 0.0684 0.028 Uiso 1 1 calc R . . C75 C 0.5415(2) 0.52179(15) 0.11759(14) 0.0288(7) Uani 1 1 d . . . H75A H 0.4654 0.5268 0.1287 0.035 Uiso 1 1 calc R . . C76 C 0.6017(2) 0.46473(14) 0.13797(13) 0.0218(6) Uani 1 1 d . . . H76A H 0.5669 0.4315 0.1633 0.026 Uiso 1 1 calc R . . C81 C 0.8765(2) 0.41590(13) 0.18089(12) 0.0170(5) Uani 1 1 d . . . C82 C 0.9746(2) 0.44300(13) 0.15711(12) 0.0210(6) Uani 1 1 d . . . H82A H 0.9839 0.4451 0.1147 0.025 Uiso 1 1 calc R . . C83 C 1.0595(2) 0.46712(13) 0.19439(13) 0.0224(6) Uani 1 1 d . . . H83A H 1.1259 0.4855 0.1775 0.027 Uiso 1 1 calc R . . C84 C 1.0466(2) 0.46422(14) 0.25615(13) 0.0236(6) Uani 1 1 d . . . H84A H 1.1044 0.4805 0.2817 0.028 Uiso 1 1 calc R . . C85 C 0.9500(2) 0.43776(13) 0.28064(13) 0.0255(6) Uani 1 1 d . . . H85A H 0.9417 0.4355 0.3231 0.031 Uiso 1 1 calc R . . C86 C 0.8645(2) 0.41432(13) 0.24339(12) 0.0210(6) Uani 1 1 d . . . H86A H 0.7975 0.3971 0.2606 0.025 Uiso 1 1 calc R . . C91 C 0.9239(2) 0.12076(12) 0.12474(11) 0.0157(5) Uani 1 1 d . . . C92 C 1.0200(2) 0.11016(13) 0.09053(12) 0.0196(6) Uani 1 1 d . . . H92A H 1.0799 0.1423 0.0930 0.024 Uiso 1 1 calc R . . C93 C 1.0290(2) 0.05294(14) 0.05277(12) 0.0239(6) Uani 1 1 d . . . H93A H 1.0951 0.0459 0.0300 0.029 Uiso 1 1 calc R . . C94 C 0.9415(2) 0.00607(14) 0.04825(13) 0.0259(6) Uani 1 1 d . . . H94A H 0.9480 -0.0332 0.0227 0.031 Uiso 1 1 calc R . . C95 C 0.8456(2) 0.01668(13) 0.08081(12) 0.0223(6) Uani 1 1 d . . . H95A H 0.7851 -0.0148 0.0771 0.027 Uiso 1 1 calc R . . C96 C 0.8366(2) 0.07342(13) 0.11936(11) 0.0191(6) Uani 1 1 d . . . H96A H 0.7703 0.0799 0.1421 0.023 Uiso 1 1 calc R . . C101 C 0.9981(2) 0.18003(13) 0.21949(12) 0.0163(5) Uani 1 1 d . . . C102 C 0.9964(2) 0.23187(15) 0.26291(12) 0.0270(7) Uani 1 1 d . . . H10A H 0.9450 0.2690 0.2590 0.032 Uiso 1 1 calc R . . C103 C 1.0679(2) 0.23039(16) 0.31149(14) 0.0356(7) Uani 1 1 d . . . H10B H 1.0660 0.2668 0.3401 0.043 Uiso 1 1 calc R . . C104 C 1.1428(2) 0.17599(16) 0.31900(13) 0.0290(7) Uani 1 1 d . . . H10C H 1.1923 0.1751 0.3524 0.035 Uiso 1 1 calc R . . C105 C 1.1437(2) 0.12353(15) 0.27698(13) 0.0265(6) Uani 1 1 d . . . H10D H 1.1933 0.0856 0.2818 0.032 Uiso 1 1 calc R . . C106 C 1.0729(2) 0.12556(13) 0.22775(12) 0.0201(6) Uani 1 1 d . . . H10E H 1.0755 0.0892 0.1991 0.024 Uiso 1 1 calc R . . C1 C 0.4219(2) 0.38125(15) 0.57858(14) 0.0296(7) Uani 1 1 d . . . H1A H 0.4590 0.4009 0.6145 0.036 Uiso 1 1 calc R . . H1B H 0.3796 0.3398 0.5914 0.036 Uiso 1 1 calc R . . Cl1 Cl 0.52343(7) 0.35699(4) 0.52558(4) 0.0419(2) Uani 1 1 d . . . Cl2 Cl 0.32776(6) 0.44350(4) 0.54816(4) 0.03715(19) 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 Ti 0.01138(18) 0.0129(2) 0.01176(19) 0.00080(17) 0.00003(17) -0.00016(18) N1 0.0152(10) 0.0126(10) 0.0133(11) 0.0005(8) -0.0006(8) 0.0008(9) N2 0.0148(10) 0.0112(10) 0.0153(10) -0.0014(8) -0.0018(8) 0.0006(8) O11 0.0223(9) 0.0137(8) 0.0125(8) 0.0010(6) 0.0003(8) -0.0041(8) O12 0.0118(8) 0.0223(10) 0.0115(8) 0.0012(7) 0.0009(7) -0.0003(7) O21 0.0178(8) 0.0140(8) 0.0162(9) 0.0024(7) 0.0043(7) -0.0010(8) O22 0.0120(7) 0.0172(8) 0.0161(9) 0.0021(7) 0.0023(7) 0.0013(7) C11 0.0181(11) 0.0152(13) 0.0126(12) -0.0011(10) 0.0013(9) 0.0022(10) C12 0.0155(11) 0.0155(12) 0.0133(12) 0.0031(10) 0.0017(10) 0.0007(10) C13 0.0184(12) 0.0160(12) 0.0164(13) 0.0019(9) -0.0025(11) 0.0022(11) C14 0.0169(13) 0.0136(12) 0.0171(13) 0.0004(9) 0.0004(11) 0.0013(10) C15 0.0159(12) 0.0140(13) 0.0183(14) -0.0008(10) 0.0011(10) 0.0006(10) C16 0.0101(11) 0.0134(12) 0.0174(13) -0.0001(10) -0.0001(10) 0.0012(10) C17 0.0112(12) 0.0156(13) 0.0132(13) -0.0022(9) 0.0017(10) 0.0005(10) C21 0.0153(12) 0.0149(12) 0.0138(12) 0.0030(10) 0.0004(10) -0.0019(10) C22 0.0148(12) 0.0132(11) 0.0150(12) 0.0037(9) 0.0003(10) -0.0012(10) C23 0.0230(14) 0.0158(13) 0.0190(14) 0.0028(10) -0.0039(11) 0.0033(11) C24 0.0262(14) 0.0217(14) 0.0172(14) -0.0021(10) -0.0051(11) 0.0042(11) C25 0.0217(12) 0.0152(12) 0.0166(12) -0.0027(9) 0.0000(11) 0.0014(11) C26 0.0123(11) 0.0173(12) 0.0160(12) -0.0003(11) 0.0007(9) 0.0009(11) C27 0.0111(11) 0.0152(12) 0.0163(13) 0.0007(10) 0.0005(10) 0.0009(10) C31 0.0225(12) 0.0131(12) 0.0140(12) -0.0044(9) -0.0004(10) 0.0069(11) C32 0.0315(15) 0.0187(13) 0.0205(14) -0.0011(10) -0.0033(13) -0.0007(13) C33 0.0314(16) 0.0284(16) 0.0326(18) -0.0079(13) -0.0107(14) -0.0059(14) C34 0.0430(18) 0.0235(14) 0.0205(15) -0.0056(11) -0.0152(13) 0.0114(14) C35 0.0456(18) 0.0277(16) 0.0144(14) 0.0009(11) -0.0036(12) 0.0077(14) C36 0.0289(14) 0.0245(15) 0.0176(14) -0.0013(11) -0.0005(11) -0.0010(12) C41 0.0228(13) 0.0172(13) 0.0145(13) -0.0032(10) -0.0022(11) 0.0045(11) C42 0.0314(15) 0.0182(14) 0.0427(19) 0.0024(13) -0.0020(14) 0.0033(12) C43 0.049(2) 0.0233(17) 0.067(3) 0.0055(17) -0.0020(19) 0.0156(16) C44 0.0409(19) 0.042(2) 0.0376(19) -0.0053(15) 0.0007(16) 0.0247(17) C45 0.0348(17) 0.058(2) 0.0248(17) 0.0022(15) 0.0099(14) 0.0207(17) C46 0.0359(16) 0.0292(16) 0.0225(16) 0.0047(12) 0.0071(13) 0.0154(14) C51 0.0146(12) 0.0162(13) 0.0178(14) 0.0007(10) -0.0052(10) 0.0027(10) C52 0.0179(13) 0.0257(15) 0.0245(15) -0.0034(12) -0.0029(11) -0.0006(12) C53 0.0299(16) 0.0236(15) 0.0350(18) -0.0023(12) -0.0108(14) -0.0049(13) C54 0.0432(18) 0.0204(15) 0.0332(18) -0.0105(13) -0.0120(15) 0.0027(14) C55 0.0397(17) 0.0336(17) 0.0237(16) -0.0127(13) -0.0024(14) 0.0088(15) C56 0.0199(13) 0.0258(15) 0.0215(15) -0.0053(11) -0.0005(11) 0.0021(12) C61 0.0156(12) 0.0158(13) 0.0127(12) -0.0031(10) -0.0029(9) -0.0013(10) C62 0.0165(13) 0.0257(15) 0.0179(14) 0.0007(11) 0.0019(11) 0.0017(11) C63 0.0255(14) 0.0208(14) 0.0193(14) 0.0057(11) 0.0011(11) 0.0037(12) C64 0.0249(14) 0.0204(15) 0.0244(15) 0.0016(11) -0.0025(12) 0.0074(12) C65 0.0175(13) 0.0222(14) 0.0307(16) -0.0013(11) 0.0030(12) 0.0019(12) C66 0.0195(13) 0.0178(13) 0.0206(14) 0.0029(10) 0.0005(10) 0.0014(11) C71 0.0174(12) 0.0128(12) 0.0147(13) -0.0014(9) -0.0016(10) 0.0023(10) C72 0.0190(13) 0.0193(14) 0.0286(16) 0.0059(12) 0.0008(11) 0.0012(11) C73 0.0265(14) 0.0175(13) 0.0284(15) 0.0069(11) -0.0020(13) -0.0027(12) C74 0.0292(15) 0.0166(14) 0.0248(15) -0.0018(11) -0.0019(12) 0.0087(12) C75 0.0218(14) 0.0266(16) 0.0379(19) -0.0020(13) 0.0086(13) 0.0101(13) C76 0.0219(14) 0.0186(14) 0.0249(15) 0.0036(11) 0.0073(12) 0.0049(11) C81 0.0178(12) 0.0138(12) 0.0195(15) 0.0004(10) -0.0016(11) 0.0039(10) C82 0.0207(14) 0.0192(14) 0.0232(15) -0.0001(11) -0.0012(11) 0.0017(12) C83 0.0173(12) 0.0185(13) 0.0313(16) -0.0029(12) -0.0002(12) -0.0014(11) C84 0.0219(14) 0.0187(14) 0.0301(17) -0.0048(11) -0.0097(12) 0.0006(12) C85 0.0356(16) 0.0197(14) 0.0210(15) 0.0003(11) -0.0034(13) -0.0021(13) C86 0.0236(14) 0.0179(14) 0.0213(15) 0.0011(11) -0.0015(11) -0.0035(11) C91 0.0197(13) 0.0139(12) 0.0136(13) 0.0018(10) 0.0019(10) 0.0045(11) C92 0.0195(13) 0.0164(13) 0.0230(15) 0.0029(11) 0.0025(11) 0.0020(11) C93 0.0275(14) 0.0232(14) 0.0209(15) 0.0022(12) 0.0093(12) 0.0061(12) C94 0.0425(17) 0.0166(14) 0.0184(15) -0.0020(11) 0.0064(13) 0.0014(13) C95 0.0295(15) 0.0184(13) 0.0190(14) -0.0010(11) -0.0009(12) -0.0068(12) C96 0.0177(13) 0.0238(14) 0.0158(13) 0.0031(11) 0.0029(10) 0.0005(11) C101 0.0141(12) 0.0174(13) 0.0176(14) 0.0042(10) 0.0022(10) -0.0013(10) C102 0.0259(14) 0.0322(17) 0.0229(15) -0.0079(12) -0.0075(12) 0.0137(13) C103 0.0355(16) 0.0391(18) 0.0324(17) -0.0150(15) -0.0137(14) 0.0083(14) C104 0.0249(14) 0.0390(17) 0.0230(16) 0.0036(13) -0.0096(12) 0.0008(13) C105 0.0206(14) 0.0265(16) 0.0323(17) 0.0103(13) -0.0024(12) 0.0030(12) C106 0.0184(13) 0.0180(14) 0.0240(15) 0.0027(11) -0.0017(11) -0.0004(11) C1 0.0305(16) 0.0286(16) 0.0298(17) -0.0016(13) 0.0067(13) -0.0044(14) Cl1 0.0334(4) 0.0463(5) 0.0459(5) -0.0101(4) 0.0177(4) -0.0088(4) Cl2 0.0416(4) 0.0307(4) 0.0391(5) 0.0103(3) 0.0092(4) -0.0026(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti O12 1.8619(16) . ? Ti O22 1.8635(16) . ? Ti O21 1.8776(16) . ? Ti O11 1.9072(16) . ? Ti N1 2.355(2) . ? Ti N2 2.382(2) . ? N1 C16 1.471(3) . ? N1 C15 1.489(3) . ? N1 C12 1.491(3) . ? N2 C26 1.475(3) . ? N2 C22 1.497(3) . ? N2 C25 1.498(3) . ? O11 C11 1.398(3) . ? O12 C17 1.423(3) . ? O21 C21 1.401(3) . ? O22 C27 1.414(3) . ? C11 C31 1.538(3) . ? C11 C12 1.548(3) . ? C11 C41 1.548(3) . ? C12 C13 1.533(3) . ? C12 H12A 1.0000 . ? C13 C14 1.538(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.531(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.548(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C61 1.529(3) . ? C17 C51 1.538(3) . ? C21 C71 1.543(3) . ? C21 C81 1.548(3) . ? C21 C22 1.566(3) . ? C22 C23 1.526(3) . ? C22 H22A 1.0000 . ? C23 C24 1.528(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.513(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.554(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C101 1.544(3) . ? C27 C91 1.544(3) . ? C31 C32 1.388(4) . ? C31 C36 1.393(4) . ? C32 C33 1.387(4) . ? C32 H32A 0.9500 . ? C33 C34 1.381(4) . ? C33 H33A 0.9500 . ? C34 C35 1.377(4) . ? C34 H34A 0.9500 . ? C35 C36 1.390(4) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C41 C42 1.389(4) . ? C41 C46 1.391(4) . ? C42 C43 1.376(4) . ? C42 H42A 0.9500 . ? C43 C44 1.380(5) . ? C43 H43A 0.9500 . ? C44 C45 1.380(5) . ? C44 H44A 0.9500 . ? C45 C46 1.386(4) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C51 C56 1.385(4) . ? C51 C52 1.401(4) . ? C52 C53 1.394(4) . ? C52 H52A 0.9500 . ? C53 C54 1.371(4) . ? C53 H53A 0.9500 . ? C54 C55 1.383(4) . ? C54 H54A 0.9500 . ? C55 C56 1.399(4) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? C61 C62 1.393(3) . ? C61 C66 1.401(3) . ? C62 C63 1.386(3) . ? C62 H62A 0.9500 . ? C63 C64 1.379(4) . ? C63 H63A 0.9500 . ? C64 C65 1.393(4) . ? C64 H64A 0.9500 . ? C65 C66 1.382(3) . ? C65 H65A 0.9500 . ? C66 H66A 0.9500 . ? C71 C72 1.393(3) . ? C71 C76 1.396(3) . ? C72 C73 1.385(4) . ? C72 H72A 0.9500 . ? C73 C74 1.381(4) . ? C73 H73A 0.9500 . ? C74 C75 1.381(4) . ? C74 H74A 0.9500 . ? C75 C76 1.394(4) . ? C75 H75A 0.9500 . ? C76 H76A 0.9500 . ? C81 C82 1.392(4) . ? C81 C86 1.398(4) . ? C82 C83 1.393(4) . ? C82 H82A 0.9500 . ? C83 C84 1.383(4) . ? C83 H83A 0.9500 . ? C84 C85 1.378(4) . ? C84 H84A 0.9500 . ? C85 C86 1.394(4) . ? C85 H85A 0.9500 . ? C86 H86A 0.9500 . ? C91 C96 1.396(3) . ? C91 C92 1.396(3) . ? C92 C93 1.393(4) . ? C92 H92A 0.9500 . ? C93 C94 1.389(4) . ? C93 H93A 0.9500 . ? C94 C95 1.374(4) . ? C94 H94A 0.9500 . ? C95 C96 1.396(4) . ? C95 H95A 0.9500 . ? C96 H96A 0.9500 . ? C101 C102 1.392(4) . ? C101 C106 1.396(3) . ? C102 C103 1.379(4) . ? C102 H10A 0.9500 . ? C103 C104 1.393(4) . ? C103 H10B 0.9500 . ? C104 C105 1.379(4) . ? C104 H10C 0.9500 . ? C105 C106 1.385(4) . ? C105 H10D 0.9500 . ? C106 H10E 0.9500 . ? C1 Cl1 1.758(3) . ? C1 Cl2 1.783(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? 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 O12 Ti O22 113.28(7) . . ? O12 Ti O21 99.45(7) . . ? O22 Ti O21 131.91(7) . . ? O12 Ti O11 131.49(7) . . ? O22 Ti O11 98.78(7) . . ? O21 Ti O11 83.00(7) . . ? O12 Ti N1 73.47(7) . . ? O22 Ti N1 86.65(7) . . ? O21 Ti N1 137.80(7) . . ? O11 Ti N1 73.15(7) . . ? O12 Ti N2 89.92(7) . . ? O22 Ti N2 73.20(7) . . ? O21 Ti N2 72.61(7) . . ? O11 Ti N2 135.28(7) . . ? N1 Ti N2 146.46(7) . . ? C16 N1 C15 112.05(19) . . ? C16 N1 C12 113.94(19) . . ? C15 N1 C12 104.40(18) . . ? C16 N1 Ti 99.33(14) . . ? C15 N1 Ti 118.80(15) . . ? C12 N1 Ti 108.69(14) . . ? C26 N2 C22 113.48(18) . . ? C26 N2 C25 111.36(18) . . ? C22 N2 C25 105.28(18) . . ? C26 N2 Ti 100.06(13) . . ? C22 N2 Ti 109.70(14) . . ? C25 N2 Ti 117.25(14) . . ? C11 O11 Ti 130.69(14) . . ? C17 O12 Ti 127.65(14) . . ? C21 O21 Ti 133.06(14) . . ? C27 O22 Ti 129.83(14) . . ? O11 C11 C31 110.37(18) . . ? O11 C11 C12 106.05(18) . . ? C31 C11 C12 110.63(19) . . ? O11 C11 C41 109.27(19) . . ? C31 C11 C41 106.86(18) . . ? C12 C11 C41 113.69(19) . . ? N1 C12 C13 103.12(19) . . ? N1 C12 C11 108.18(19) . . ? C13 C12 C11 112.93(19) . . ? N1 C12 H12A 110.8 . . ? C13 C12 H12A 110.8 . . ? C11 C12 H12A 110.8 . . ? C12 C13 C14 105.68(19) . . ? C12 C13 H13A 110.6 . . ? C14 C13 H13A 110.6 . . ? C12 C13 H13B 110.6 . . ? C14 C13 H13B 110.6 . . ? H13A C13 H13B 108.7 . . ? C15 C14 C13 104.93(19) . . ? C15 C14 H14A 110.8 . . ? C13 C14 H14A 110.8 . . ? C15 C14 H14B 110.8 . . ? C13 C14 H14B 110.8 . . ? H14A C14 H14B 108.8 . . ? N1 C15 C14 105.54(19) . . ? N1 C15 H15A 110.6 . . ? C14 C15 H15A 110.6 . . ? N1 C15 H15B 110.6 . . ? C14 C15 H15B 110.6 . . ? H15A C15 H15B 108.8 . . ? N1 C16 C17 109.05(19) . . ? N1 C16 H16A 109.9 . . ? C17 C16 H16A 109.9 . . ? N1 C16 H16B 109.9 . . ? C17 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? O12 C17 C61 109.45(19) . . ? O12 C17 C51 110.25(19) . . ? C61 C17 C51 109.59(19) . . ? O12 C17 C16 105.35(19) . . ? C61 C17 C16 109.27(19) . . ? C51 C17 C16 112.8(2) . . ? O21 C21 C71 109.09(18) . . ? O21 C21 C81 109.01(19) . . ? C71 C21 C81 107.37(19) . . ? O21 C21 C22 106.23(19) . . ? C71 C21 C22 110.54(19) . . ? C81 C21 C22 114.53(19) . . ? N2 C22 C23 105.02(19) . . ? N2 C22 C21 108.39(18) . . ? C23 C22 C21 113.5(2) . . ? N2 C22 H22A 109.9 . . ? C23 C22 H22A 109.9 . . ? C21 C22 H22A 109.9 . . ? C22 C23 C24 106.9(2) . . ? C22 C23 H23A 110.4 . . ? C24 C23 H23A 110.4 . . ? C22 C23 H23B 110.4 . . ? C24 C23 H23B 110.4 . . ? H23A C23 H23B 108.6 . . ? C25 C24 C23 105.7(2) . . ? C25 C24 H24A 110.6 . . ? C23 C24 H24A 110.6 . . ? C25 C24 H24B 110.6 . . ? C23 C24 H24B 110.6 . . ? H24A C24 H24B 108.7 . . ? N2 C25 C24 106.58(19) . . ? N2 C25 H25A 110.4 . . ? C24 C25 H25A 110.4 . . ? N2 C25 H25B 110.4 . . ? C24 C25 H25B 110.4 . . ? H25A C25 H25B 108.6 . . ? N2 C26 C27 109.47(18) . . ? N2 C26 H26A 109.8 . . ? C27 C26 H26A 109.8 . . ? N2 C26 H26B 109.8 . . ? C27 C26 H26B 109.8 . . ? H26A C26 H26B 108.2 . . ? O22 C27 C101 107.40(19) . . ? O22 C27 C91 110.01(19) . . ? C101 C27 C91 111.87(19) . . ? O22 C27 C26 105.07(18) . . ? C101 C27 C26 110.13(19) . . ? C91 C27 C26 112.0(2) . . ? C32 C31 C36 118.3(2) . . ? C32 C31 C11 120.2(2) . . ? C36 C31 C11 121.5(2) . . ? C33 C32 C31 120.5(3) . . ? C33 C32 H32A 119.7 . . ? C31 C32 H32A 119.7 . . ? C34 C33 C32 120.6(3) . . ? C34 C33 H33A 119.7 . . ? C32 C33 H33A 119.7 . . ? C35 C34 C33 119.6(3) . . ? C35 C34 H34A 120.2 . . ? C33 C34 H34A 120.2 . . ? C34 C35 C36 120.0(3) . . ? C34 C35 H35A 120.0 . . ? C36 C35 H35A 120.0 . . ? C35 C36 C31 121.0(3) . . ? C35 C36 H36A 119.5 . . ? C31 C36 H36A 119.5 . . ? C42 C41 C46 118.1(2) . . ? C42 C41 C11 118.9(2) . . ? C46 C41 C11 123.0(2) . . ? C43 C42 C41 120.9(3) . . ? C43 C42 H42A 119.6 . . ? C41 C42 H42A 119.6 . . ? C42 C43 C44 120.7(3) . . ? C42 C43 H43A 119.6 . . ? C44 C43 H43A 119.6 . . ? C45 C44 C43 119.2(3) . . ? C45 C44 H44A 120.4 . . ? C43 C44 H44A 120.4 . . ? C44 C45 C46 120.3(3) . . ? C44 C45 H45A 119.9 . . ? C46 C45 H45A 119.9 . . ? C45 C46 C41 120.8(3) . . ? C45 C46 H46A 119.6 . . ? C41 C46 H46A 119.6 . . ? C56 C51 C52 118.8(2) . . ? C56 C51 C17 121.0(2) . . ? C52 C51 C17 120.2(2) . . ? C53 C52 C51 120.3(3) . . ? C53 C52 H52A 119.8 . . ? C51 C52 H52A 119.8 . . ? C54 C53 C52 120.5(3) . . ? C54 C53 H53A 119.7 . . ? C52 C53 H53A 119.7 . . ? C53 C54 C55 119.6(3) . . ? C53 C54 H54A 120.2 . . ? C55 C54 H54A 120.2 . . ? C54 C55 C56 120.6(3) . . ? C54 C55 H55A 119.7 . . ? C56 C55 H55A 119.7 . . ? C51 C56 C55 120.1(3) . . ? C51 C56 H56A 120.0 . . ? C55 C56 H56A 120.0 . . ? C62 C61 C66 118.5(2) . . ? C62 C61 C17 120.0(2) . . ? C66 C61 C17 121.5(2) . . ? C63 C62 C61 120.6(2) . . ? C63 C62 H62A 119.7 . . ? C61 C62 H62A 119.7 . . ? C64 C63 C62 120.2(2) . . ? C64 C63 H63A 119.9 . . ? C62 C63 H63A 119.9 . . ? C63 C64 C65 120.2(3) . . ? C63 C64 H64A 119.9 . . ? C65 C64 H64A 119.9 . . ? C66 C65 C64 119.6(2) . . ? C66 C65 H65A 120.2 . . ? C64 C65 H65A 120.2 . . ? C65 C66 C61 121.0(2) . . ? C65 C66 H66A 119.5 . . ? C61 C66 H66A 119.5 . . ? C72 C71 C76 118.4(2) . . ? C72 C71 C21 122.0(2) . . ? C76 C71 C21 119.5(2) . . ? C73 C72 C71 121.0(2) . . ? C73 C72 H72A 119.5 . . ? C71 C72 H72A 119.5 . . ? C74 C73 C72 120.5(3) . . ? C74 C73 H73A 119.7 . . ? C72 C73 H73A 119.7 . . ? C73 C74 C75 119.2(3) . . ? C73 C74 H74A 120.4 . . ? C75 C74 H74A 120.4 . . ? C74 C75 C76 120.9(2) . . ? C74 C75 H75A 119.6 . . ? C76 C75 H75A 119.6 . . ? C75 C76 C71 120.1(2) . . ? C75 C76 H76A 120.0 . . ? C71 C76 H76A 120.0 . . ? C82 C81 C86 118.2(2) . . ? C82 C81 C21 123.5(2) . . ? C86 C81 C21 118.2(2) . . ? C81 C82 C83 121.1(3) . . ? C81 C82 H82A 119.4 . . ? C83 C82 H82A 119.4 . . ? C84 C83 C82 119.7(3) . . ? C84 C83 H83A 120.1 . . ? C82 C83 H83A 120.1 . . ? C85 C84 C83 120.1(3) . . ? C85 C84 H84A 120.0 . . ? C83 C84 H84A 120.0 . . ? C84 C85 C86 120.3(3) . . ? C84 C85 H85A 119.9 . . ? C86 C85 H85A 119.9 . . ? C85 C86 C81 120.5(3) . . ? C85 C86 H86A 119.7 . . ? C81 C86 H86A 119.7 . . ? C96 C91 C92 118.4(2) . . ? C96 C91 C27 120.4(2) . . ? C92 C91 C27 121.1(2) . . ? C93 C92 C91 120.6(3) . . ? C93 C92 H92A 119.7 . . ? C91 C92 H92A 119.7 . . ? C94 C93 C92 120.2(2) . . ? C94 C93 H93A 119.9 . . ? C92 C93 H93A 119.9 . . ? C95 C94 C93 119.7(2) . . ? C95 C94 H94A 120.1 . . ? C93 C94 H94A 120.1 . . ? C94 C95 C96 120.4(3) . . ? C94 C95 H95A 119.8 . . ? C96 C95 H95A 119.8 . . ? C91 C96 C95 120.6(2) . . ? C91 C96 H96A 119.7 . . ? C95 C96 H96A 119.7 . . ? C102 C101 C106 117.5(2) . . ? C102 C101 C27 118.7(2) . . ? C106 C101 C27 123.7(2) . . ? C103 C102 C101 121.3(3) . . ? C103 C102 H10A 119.4 . . ? C101 C102 H10A 119.4 . . ? C102 C103 C104 120.7(3) . . ? C102 C103 H10B 119.7 . . ? C104 C103 H10B 119.7 . . ? C105 C104 C103 118.6(3) . . ? C105 C104 H10C 120.7 . . ? C103 C104 H10C 120.7 . . ? C104 C105 C106 120.7(3) . . ? C104 C105 H10D 119.7 . . ? C106 C105 H10D 119.7 . . ? C105 C106 C101 121.3(3) . . ? C105 C106 H10E 119.4 . . ? C101 C106 H10E 119.4 . . ? Cl1 C1 Cl2 111.34(17) . . ? Cl1 C1 H1A 109.4 . . ? Cl2 C1 H1A 109.4 . . ? Cl1 C1 H1B 109.4 . . ? Cl2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 29.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.273 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.063