# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2014 data_t _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H34 N6 O2 Ti' _chemical_formula_sum 'C28 H34 N6 O2 Ti' _chemical_formula_weight 534.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.2191(8) _cell_length_b 11.4180(10) _cell_length_c 24.491(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.554(2) _cell_angle_gamma 90.00 _cell_volume 2809.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6951 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 27.10 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.264 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.340 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9050 _exptl_absorpt_correction_T_max 0.9701 _exptl_absorpt_process_details 'SADABS (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17827 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_unetI/netI 0.0284 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 27.12 _reflns_number_total 6183 _reflns_number_gt 5395 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction 'SAINT (Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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. During the refinement, DFIX restraints were used for reasonable bond distances between C23 C24, C23 C25, C26 C28 and C26 C28'. Thermal motion of C7 N3, C18 N6, C24 C25, C26 C26' C27 C27' and C28 C28' are restrained by commond 'EADP'. ; _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^)+(0.1011P)^2^+5.2998P] 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_number_reflns 6183 _refine_ls_number_parameters 330 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0739 _refine_ls_R_factor_gt 0.0668 _refine_ls_wR_factor_ref 0.1906 _refine_ls_wR_factor_gt 0.1842 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.21840(5) 0.20565(4) 0.136478(18) 0.02152(16) Uani 1 1 d . . . N1 N 0.1462(2) 0.03312(19) 0.12436(9) 0.0243(5) Uani 1 1 d . . . O1 O 0.3728(2) 0.16279(18) 0.17806(8) 0.0309(4) Uani 1 1 d . . . C1 C 0.1865(3) -0.0741(2) 0.14479(12) 0.0281(6) Uani 1 1 d . . . H1 H 0.2644 -0.0886 0.1716 0.034 Uiso 1 1 calc R . . N2 N 0.0310(2) 0.2166(2) 0.06897(9) 0.0245(5) Uani 1 1 d . . . C2 C 0.0971(3) -0.1600(2) 0.12076(13) 0.0312(6) Uani 1 1 d . . . H2 H 0.1027 -0.2416 0.1283 0.037 Uiso 1 1 calc R . . O2 O 0.1298(2) 0.25445(19) 0.18745(9) 0.0337(5) Uani 1 1 d . . . N3 N -0.2270(3) 0.3444(2) 0.08239(12) 0.0382(5) Uani 1 1 d . . . C3 C -0.0022(3) -0.1028(3) 0.08344(13) 0.0314(6) Uani 1 1 d . . . H3 H -0.0770 -0.1378 0.0605 0.038 Uiso 1 1 calc R . . N4 N 0.2636(2) 0.37383(19) 0.11130(9) 0.0241(5) Uani 1 1 d . . . C4 C 0.0304(3) 0.0156(2) 0.08662(11) 0.0263(5) Uani 1 1 d . . . N5 N 0.3032(2) 0.17988(19) 0.05854(9) 0.0231(4) Uani 1 1 d . . . C5 C -0.0260(3) 0.1172(2) 0.05728(11) 0.0275(6) Uani 1 1 d . . . H5 H -0.1041 0.1113 0.0297 0.033 Uiso 1 1 calc R . . N6 N 0.5560(3) 0.0562(2) 0.09067(11) 0.0336(4) Uani 1 1 d . . . C6 C -0.0265(3) 0.3196(3) 0.03698(12) 0.0292(6) Uani 1 1 d . . . H6B H -0.0807 0.2930 0.0014 0.035 Uiso 1 1 calc R . . H6C H 0.0465 0.3690 0.0282 0.035 Uiso 1 1 calc R . . C7 C -0.1123(3) 0.3922(3) 0.06784(14) 0.0382(5) Uani 1 1 d . . . C8 C -0.0811(3) 0.5084(3) 0.08061(14) 0.0367(7) Uani 1 1 d . . . H8 H -0.0035 0.5419 0.0709 0.044 Uiso 1 1 calc R . . C9 C -0.1624(4) 0.5764(3) 0.10751(17) 0.0472(8) Uani 1 1 d . . . H9 H -0.1404 0.6559 0.1160 0.057 Uiso 1 1 calc R . . C10 C -0.2754(4) 0.5284(3) 0.12201(18) 0.0503(9) Uani 1 1 d . . . H10 H -0.3306 0.5749 0.1406 0.060 Uiso 1 1 calc R . . C11 C -0.3082(3) 0.4130(3) 0.10957(16) 0.0443(8) Uani 1 1 d . . . H11 H -0.3861 0.3803 0.1195 0.053 Uiso 1 1 calc R . . C12 C 0.2526(3) 0.4845(2) 0.13021(12) 0.0284(6) Uani 1 1 d . . . H12 H 0.2193 0.5043 0.1628 0.034 Uiso 1 1 calc R . . C13 C 0.2973(3) 0.5649(2) 0.09487(13) 0.0325(6) Uani 1 1 d . . . H13 H 0.3002 0.6476 0.0991 0.039 Uiso 1 1 calc R A . C14 C 0.3371(3) 0.5005(2) 0.05200(13) 0.0317(6) Uani 1 1 d . A . H14 H 0.3719 0.5307 0.0214 0.038 Uiso 1 1 calc R . . C15 C 0.3154(3) 0.3836(2) 0.06331(11) 0.0249(5) Uani 1 1 d . A . C16 C 0.3346(3) 0.2759(2) 0.03616(12) 0.0258(5) Uani 1 1 d . A . H16 H 0.3693 0.2749 0.0027 0.031 Uiso 1 1 calc R . . C17 C 0.3251(3) 0.0684(2) 0.03227(12) 0.0265(5) Uani 1 1 d . . . H17A H 0.3432 0.0837 -0.0054 0.032 Uiso 1 1 calc R . . H17B H 0.2430 0.0206 0.0284 0.032 Uiso 1 1 calc R . . C18 C 0.4398(3) 0.0000(3) 0.06509(13) 0.0336(4) Uani 1 1 d . . . C19 C 0.4322(3) -0.1214(3) 0.06838(14) 0.0358(7) Uani 1 1 d . . . H19 H 0.3533 -0.1604 0.0511 0.043 Uiso 1 1 calc R . . C20 C 0.5382(4) -0.1865(3) 0.09662(17) 0.0443(8) Uani 1 1 d . . . H20 H 0.5318 -0.2693 0.0983 0.053 Uiso 1 1 calc R A . C21 C 0.6533(3) -0.1304(3) 0.12231(15) 0.0435(8) Uani 1 1 d . . . H21 H 0.7255 -0.1747 0.1420 0.052 Uiso 1 1 calc R . . C22 C 0.6630(3) -0.0091(3) 0.11920(14) 0.0369(7) Uani 1 1 d . . . H22 H 0.7423 0.0294 0.1364 0.044 Uiso 1 1 calc R A . C24 C 0.5796(5) 0.2103(5) 0.2359(2) 0.0798(12) Uani 1 1 d D . . H24A H 0.5785 0.2617 0.2038 0.120 Uiso 1 1 calc R . . H24B H 0.6436 0.1468 0.2350 0.120 Uiso 1 1 calc R . . H24C H 0.6055 0.2557 0.2702 0.120 Uiso 1 1 calc R . . C23 C 0.4423(4) 0.1592(4) 0.23406(17) 0.0602(11) Uani 1 1 d D . . H23 H 0.3937 0.2100 0.2570 0.072 Uiso 1 1 calc R . . C25 C 0.4488(5) 0.0416(5) 0.2570(2) 0.0798(12) Uani 1 1 d D . . H25A H 0.3727 -0.0041 0.2381 0.120 Uiso 1 1 calc R . . H25B H 0.4465 0.0456 0.2968 0.120 Uiso 1 1 calc R . . H25C H 0.5317 0.0039 0.2516 0.120 Uiso 1 1 calc R . . C27 C -0.0680(5) 0.2204(5) 0.2225(2) 0.0590(14) Uani 0.822(8) 1 d P A 1 H27A H -0.0965 0.1716 0.1896 0.088 Uiso 0.822(8) 1 calc PR A 1 H27B H -0.1457 0.2590 0.2327 0.088 Uiso 0.822(8) 1 calc PR A 1 H27C H -0.0248 0.1710 0.2534 0.088 Uiso 0.822(8) 1 calc PR A 1 C27' C 0.021(2) 0.170(2) 0.2557(10) 0.0590(14) Uani 0.178(8) 1 d P A 2 H27D H 0.0705 0.1024 0.2458 0.088 Uiso 0.178(8) 1 calc PR A 2 H27E H -0.0733 0.1620 0.2387 0.088 Uiso 0.178(8) 1 calc PR A 2 H27F H 0.0294 0.1742 0.2962 0.088 Uiso 0.178(8) 1 calc PR A 2 C26 C 0.0221(8) 0.3052(8) 0.2110(3) 0.0442(12) Uani 0.437(7) 1 d PD A 1 H26 H -0.0250 0.3672 0.1859 0.053 Uiso 0.437(7) 1 calc PR A 1 C26' C 0.0715(6) 0.2718(5) 0.2365(2) 0.0442(12) Uani 0.563(7) 1 d PD A 2 H26' H 0.1588 0.2648 0.2625 0.053 Uiso 0.563(7) 1 calc PR A 2 C28 C 0.0974(17) 0.3583(17) 0.2635(5) 0.066(2) Uani 0.282(13) 1 d PD A 1 H28A H 0.0397 0.4135 0.2785 0.098 Uiso 0.282(13) 1 calc PR A 1 H28B H 0.1756 0.3999 0.2555 0.098 Uiso 0.282(13) 1 calc PR A 1 H28C H 0.1260 0.2963 0.2907 0.098 Uiso 0.282(13) 1 calc PR A 1 C28' C 0.0594(9) 0.4004(5) 0.2469(3) 0.066(2) Uani 0.718(13) 1 d PD A 2 H28D H 0.1260 0.4432 0.2306 0.098 Uiso 0.718(13) 1 calc PR A 2 H28E H 0.0741 0.4149 0.2870 0.098 Uiso 0.718(13) 1 calc PR A 2 H28F H -0.0299 0.4273 0.2299 0.098 Uiso 0.718(13) 1 calc PR A 2 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 0.0255(3) 0.0170(2) 0.0216(3) -0.00030(16) 0.00319(18) 0.00231(16) N1 0.0285(11) 0.0203(10) 0.0247(11) 0.0016(8) 0.0065(9) 0.0014(9) O1 0.0346(11) 0.0264(10) 0.0282(10) 0.0016(8) -0.0037(8) 0.0024(8) C1 0.0345(14) 0.0223(13) 0.0296(13) 0.0044(10) 0.0112(11) 0.0035(11) N2 0.0234(11) 0.0249(11) 0.0250(11) 0.0042(8) 0.0043(9) 0.0025(8) C2 0.0374(15) 0.0191(12) 0.0416(16) 0.0007(11) 0.0190(13) -0.0003(11) O2 0.0437(12) 0.0281(10) 0.0327(11) -0.0045(8) 0.0157(9) 0.0004(9) N3 0.0305(10) 0.0372(11) 0.0452(11) 0.0137(9) 0.0026(8) 0.0039(8) C3 0.0316(14) 0.0254(14) 0.0397(15) -0.0052(11) 0.0133(12) -0.0045(11) N4 0.0248(11) 0.0181(10) 0.0277(11) -0.0002(8) 0.0006(9) 0.0017(8) C4 0.0258(13) 0.0251(13) 0.0291(13) -0.0015(10) 0.0081(10) -0.0010(10) N5 0.0207(10) 0.0217(10) 0.0265(11) -0.0028(8) 0.0030(8) 0.0033(8) C5 0.0241(13) 0.0290(14) 0.0289(13) 0.0001(11) 0.0039(10) -0.0001(10) N6 0.0320(10) 0.0292(10) 0.0416(11) -0.0026(8) 0.0119(8) 0.0030(8) C6 0.0263(13) 0.0285(14) 0.0314(14) 0.0105(11) 0.0015(11) 0.0019(11) C7 0.0305(10) 0.0372(11) 0.0452(11) 0.0137(9) 0.0026(8) 0.0039(8) C8 0.0319(15) 0.0268(14) 0.0505(18) 0.0137(13) 0.0052(13) 0.0031(12) C9 0.051(2) 0.0268(16) 0.064(2) 0.0097(15) 0.0124(17) 0.0102(14) C10 0.049(2) 0.0405(19) 0.065(2) 0.0157(17) 0.0213(18) 0.0239(16) C11 0.0290(15) 0.0487(19) 0.058(2) 0.0225(16) 0.0153(15) 0.0122(14) C12 0.0284(13) 0.0199(12) 0.0346(14) -0.0041(11) -0.0004(11) 0.0017(10) C13 0.0284(14) 0.0173(12) 0.0495(17) 0.0027(11) 0.0015(12) 0.0006(10) C14 0.0256(13) 0.0249(14) 0.0440(16) 0.0089(12) 0.0049(12) 0.0005(11) C15 0.0208(12) 0.0225(13) 0.0307(13) 0.0034(10) 0.0025(10) 0.0015(10) C16 0.0213(12) 0.0273(13) 0.0290(13) 0.0011(10) 0.0053(10) 0.0032(10) C17 0.0251(13) 0.0239(13) 0.0314(13) -0.0080(10) 0.0077(10) 0.0007(10) C18 0.0320(10) 0.0292(10) 0.0416(11) -0.0026(8) 0.0119(8) 0.0030(8) C19 0.0340(15) 0.0246(14) 0.0534(19) -0.0006(13) 0.0204(14) -0.0005(12) C20 0.0472(19) 0.0237(14) 0.068(2) 0.0101(14) 0.0280(17) 0.0086(13) C21 0.0408(18) 0.0400(18) 0.053(2) 0.0118(15) 0.0159(15) 0.0198(14) C22 0.0279(15) 0.0392(17) 0.0436(17) -0.0027(13) 0.0065(13) 0.0081(12) C24 0.077(2) 0.094(3) 0.0554(18) 0.0246(18) -0.0213(16) -0.029(2) C23 0.056(2) 0.072(3) 0.044(2) 0.0162(19) -0.0134(18) -0.013(2) C25 0.077(2) 0.094(3) 0.0554(18) 0.0246(18) -0.0213(16) -0.029(2) C27 0.054(3) 0.073(4) 0.053(3) -0.008(2) 0.020(2) -0.021(2) C27' 0.054(3) 0.073(4) 0.053(3) -0.008(2) 0.020(2) -0.021(2) C26 0.037(3) 0.068(4) 0.028(3) 0.006(2) 0.007(2) 0.010(2) C26' 0.037(3) 0.068(4) 0.028(3) 0.006(2) 0.007(2) 0.010(2) C28 0.113(6) 0.032(3) 0.069(4) -0.002(3) 0.061(4) 0.013(3) C28' 0.113(6) 0.032(3) 0.069(4) -0.002(3) 0.061(4) 0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O2 1.761(2) . ? Ti1 O1 1.783(2) . ? Ti1 N4 2.094(2) . ? Ti1 N1 2.106(2) . ? Ti1 N5 2.255(2) . ? Ti1 N2 2.293(2) . ? N1 C1 1.358(3) . ? N1 C4 1.376(4) . ? O1 C23 1.425(4) . ? C1 C2 1.395(4) . ? C1 H1 0.9500 . ? N2 C5 1.283(4) . ? N2 C6 1.474(3) . ? C2 C3 1.397(4) . ? C2 H2 0.9500 . ? O2 C26' 1.450(6) . ? O2 C26 1.453(8) . ? N3 C11 1.396(5) . ? N3 C7 1.396(4) . ? C3 C4 1.392(4) . ? C3 H3 0.9500 . ? N4 C12 1.358(3) . ? N4 C15 1.379(4) . ? C4 C5 1.429(4) . ? N5 C16 1.292(4) . ? N5 C17 1.462(3) . ? C5 H5 0.9500 . ? N6 C18 1.394(4) . ? N6 C22 1.400(4) . ? C6 C7 1.506(4) . ? C6 H6B 0.9900 . ? C6 H6C 0.9900 . ? C7 C8 1.388(5) . ? C8 C9 1.388(5) . ? C8 H8 0.9500 . ? C9 C10 1.381(5) . ? C9 H9 0.9500 . ? C10 C11 1.379(6) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.395(4) . ? C12 H12 0.9500 . ? C13 C14 1.402(4) . ? C13 H13 0.9500 . ? C14 C15 1.390(4) . ? C14 H14 0.9500 . ? C15 C16 1.428(4) . ? C16 H16 0.9500 . ? C17 C18 1.512(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.392(4) . ? C19 C20 1.389(5) . ? C19 H19 0.9500 . ? C20 C21 1.385(5) . ? C20 H20 0.9500 . ? C21 C22 1.392(5) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C24 C23 1.512(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C23 C25 1.452(6) . ? C23 H23 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C27 C26 1.401(10) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C27' C26' 1.39(2) . ? C27' H27D 0.9800 . ? C27' H27E 0.9800 . ? C27' H27F 0.9800 . ? C26 C28 1.5000(10) . ? C26 H26 1.0000 . ? C26' C28' 1.5001(10) . ? C26' H26' 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C28' H28D 0.9800 . ? C28' H28E 0.9800 . ? C28' H28F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ti1 O1 101.42(10) . . ? O2 Ti1 N4 95.06(10) . . ? O1 Ti1 N4 101.54(9) . . ? O2 Ti1 N1 100.58(9) . . ? O1 Ti1 N1 94.27(9) . . ? N4 Ti1 N1 155.09(9) . . ? O2 Ti1 N5 165.49(9) . . ? O1 Ti1 N5 90.61(9) . . ? N4 Ti1 N5 74.38(9) . . ? N1 Ti1 N5 86.43(8) . . ? O2 Ti1 N2 91.38(9) . . ? O1 Ti1 N2 164.15(9) . . ? N4 Ti1 N2 86.44(8) . . ? N1 Ti1 N2 74.00(8) . . ? N5 Ti1 N2 78.25(8) . . ? C1 N1 C4 106.4(2) . . ? C1 N1 Ti1 135.8(2) . . ? C4 N1 Ti1 117.80(18) . . ? C23 O1 Ti1 142.3(3) . . ? N1 C1 C2 110.3(3) . . ? N1 C1 H1 124.8 . . ? C2 C1 H1 124.8 . . ? C5 N2 C6 117.8(2) . . ? C5 N2 Ti1 113.41(18) . . ? C6 N2 Ti1 128.74(18) . . ? C1 C2 C3 106.8(2) . . ? C1 C2 H2 126.6 . . ? C3 C2 H2 126.6 . . ? C26' O2 Ti1 166.8(3) . . ? C26 O2 Ti1 158.8(4) . . ? C11 N3 C7 120.1(3) . . ? C4 C3 C2 106.3(3) . . ? C4 C3 H3 126.9 . . ? C2 C3 H3 126.9 . . ? C12 N4 C15 106.5(2) . . ? C12 N4 Ti1 135.8(2) . . ? C15 N4 Ti1 117.70(17) . . ? N1 C4 C3 110.2(3) . . ? N1 C4 C5 116.0(2) . . ? C3 C4 C5 133.7(3) . . ? C16 N5 C17 118.8(2) . . ? C16 N5 Ti1 114.33(18) . . ? C17 N5 Ti1 126.84(18) . . ? N2 C5 C4 118.7(2) . . ? N2 C5 H5 120.6 . . ? C4 C5 H5 120.6 . . ? C18 N6 C22 120.1(3) . . ? N2 C6 C7 112.6(2) . . ? N2 C6 H6B 109.1 . . ? C7 C6 H6B 109.1 . . ? N2 C6 H6C 109.1 . . ? C7 C6 H6C 109.1 . . ? H6B C6 H6C 107.8 . . ? C8 C7 N3 119.0(3) . . ? C8 C7 C6 120.6(3) . . ? N3 C7 C6 120.4(3) . . ? C7 C8 C9 120.6(3) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C10 C9 C8 120.1(3) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C11 C10 C9 120.2(3) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 N3 120.0(3) . . ? C10 C11 H11 120.0 . . ? N3 C11 H11 120.0 . . ? N4 C12 C13 110.1(3) . . ? N4 C12 H12 124.9 . . ? C13 C12 H12 124.9 . . ? C12 C13 C14 107.0(2) . . ? C12 C13 H13 126.5 . . ? C14 C13 H13 126.5 . . ? C15 C14 C13 106.0(3) . . ? C15 C14 H14 127.0 . . ? C13 C14 H14 127.0 . . ? N4 C15 C14 110.4(2) . . ? N4 C15 C16 115.7(2) . . ? C14 C15 C16 133.9(3) . . ? N5 C16 C15 117.8(2) . . ? N5 C16 H16 121.1 . . ? C15 C16 H16 121.1 . . ? N5 C17 C18 112.5(2) . . ? N5 C17 H17A 109.1 . . ? C18 C17 H17A 109.1 . . ? N5 C17 H17B 109.1 . . ? C18 C17 H17B 109.1 . . ? H17A C17 H17B 107.8 . . ? C19 C18 N6 119.0(3) . . ? C19 C18 C17 120.0(3) . . ? N6 C18 C17 121.0(3) . . ? C20 C19 C18 121.0(3) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C21 C20 C19 120.0(3) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 119.9(3) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C21 C22 N6 120.0(3) . . ? C21 C22 H22 120.0 . . ? N6 C22 H22 120.0 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O1 C23 C25 112.2(4) . . ? O1 C23 C24 108.3(3) . . ? C25 C23 C24 111.7(4) . . ? O1 C23 H23 108.2 . . ? C25 C23 H23 108.2 . . ? C24 C23 H23 108.2 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26' C27' H27D 109.5 . . ? C26' C27' H27E 109.5 . . ? H27D C27' H27E 109.5 . . ? C26' C27' H27F 109.5 . . ? H27D C27' H27F 109.5 . . ? H27E C27' H27F 109.5 . . ? C27 C26 O2 112.2(7) . . ? C27 C26 C28 111.1(9) . . ? O2 C26 C28 101.2(8) . . ? C27 C26 H26 110.7 . . ? O2 C26 H26 110.7 . . ? C28 C26 H26 110.7 . . ? C27' C26' O2 113.7(11) . . ? C27' C26' C28' 135.6(12) . . ? O2 C26' C28' 109.5(4) . . ? C27' C26' H26' 93.6 . . ? O2 C26' H26' 93.6 . . ? C28' C26' H26' 93.6 . . ? C26' C28' H28D 109.5 . . ? C26' C28' H28E 109.5 . . ? H28D C28' H28E 109.5 . . ? C26' C28' H28F 109.5 . . ? H28D C28' H28F 109.5 . . ? H28E C28' H28F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Ti1 N1 C1 -94.4(3) . . . . ? O1 Ti1 N1 C1 8.0(3) . . . . ? N4 Ti1 N1 C1 137.6(3) . . . . ? N5 Ti1 N1 C1 98.4(3) . . . . ? N2 Ti1 N1 C1 177.2(3) . . . . ? O2 Ti1 N1 C4 86.5(2) . . . . ? O1 Ti1 N1 C4 -171.08(19) . . . . ? N4 Ti1 N1 C4 -41.5(3) . . . . ? N5 Ti1 N1 C4 -80.73(19) . . . . ? N2 Ti1 N1 C4 -1.94(18) . . . . ? O2 Ti1 O1 C23 -2.5(4) . . . . ? N4 Ti1 O1 C23 95.2(4) . . . . ? N1 Ti1 O1 C23 -104.2(4) . . . . ? N5 Ti1 O1 C23 169.4(4) . . . . ? N2 Ti1 O1 C23 -145.7(4) . . . . ? C4 N1 C1 C2 -0.4(3) . . . . ? Ti1 N1 C1 C2 -179.6(2) . . . . ? O2 Ti1 N2 C5 -99.9(2) . . . . ? O1 Ti1 N2 C5 44.2(4) . . . . ? N4 Ti1 N2 C5 165.1(2) . . . . ? N1 Ti1 N2 C5 0.74(19) . . . . ? N5 Ti1 N2 C5 90.4(2) . . . . ? O2 Ti1 N2 C6 82.8(2) . . . . ? O1 Ti1 N2 C6 -133.1(3) . . . . ? N4 Ti1 N2 C6 -12.2(2) . . . . ? N1 Ti1 N2 C6 -176.6(2) . . . . ? N5 Ti1 N2 C6 -86.9(2) . . . . ? N1 C1 C2 C3 0.5(3) . . . . ? O1 Ti1 O2 C26' -39.2(13) . . . . ? N4 Ti1 O2 C26' -142.1(13) . . . . ? N1 Ti1 O2 C26' 57.4(13) . . . . ? N5 Ti1 O2 C26' 175.3(12) . . . . ? N2 Ti1 O2 C26' 131.4(13) . . . . ? O1 Ti1 O2 C26 175.6(11) . . . . ? N4 Ti1 O2 C26 72.7(11) . . . . ? N1 Ti1 O2 C26 -87.8(11) . . . . ? N5 Ti1 O2 C26 30.2(12) . . . . ? N2 Ti1 O2 C26 -13.8(11) . . . . ? C1 C2 C3 C4 -0.4(3) . . . . ? O2 Ti1 N4 C12 9.6(3) . . . . ? O1 Ti1 N4 C12 -93.1(3) . . . . ? N1 Ti1 N4 C12 138.5(3) . . . . ? N5 Ti1 N4 C12 179.5(3) . . . . ? N2 Ti1 N4 C12 100.7(3) . . . . ? O2 Ti1 N4 C15 -168.68(19) . . . . ? O1 Ti1 N4 C15 88.56(19) . . . . ? N1 Ti1 N4 C15 -39.8(3) . . . . ? N5 Ti1 N4 C15 1.18(18) . . . . ? N2 Ti1 N4 C15 -77.61(19) . . . . ? C1 N1 C4 C3 0.1(3) . . . . ? Ti1 N1 C4 C3 179.48(18) . . . . ? C1 N1 C4 C5 -176.5(2) . . . . ? Ti1 N1 C4 C5 2.9(3) . . . . ? C2 C3 C4 N1 0.2(3) . . . . ? C2 C3 C4 C5 175.9(3) . . . . ? O2 Ti1 N5 C16 43.0(5) . . . . ? O1 Ti1 N5 C16 -103.21(19) . . . . ? N4 Ti1 N5 C16 -1.40(18) . . . . ? N1 Ti1 N5 C16 162.55(19) . . . . ? N2 Ti1 N5 C16 88.16(19) . . . . ? O2 Ti1 N5 C17 -137.1(4) . . . . ? O1 Ti1 N5 C17 76.7(2) . . . . ? N4 Ti1 N5 C17 178.5(2) . . . . ? N1 Ti1 N5 C17 -17.6(2) . . . . ? N2 Ti1 N5 C17 -92.0(2) . . . . ? C6 N2 C5 C4 178.1(2) . . . . ? Ti1 N2 C5 C4 0.5(3) . . . . ? N1 C4 C5 N2 -2.2(4) . . . . ? C3 C4 C5 N2 -177.8(3) . . . . ? C5 N2 C6 C7 99.7(3) . . . . ? Ti1 N2 C6 C7 -83.1(3) . . . . ? C11 N3 C7 C8 -0.3(4) . . . . ? C11 N3 C7 C6 -178.2(3) . . . . ? N2 C6 C7 C8 119.8(3) . . . . ? N2 C6 C7 N3 -62.3(4) . . . . ? N3 C7 C8 C9 0.1(5) . . . . ? C6 C7 C8 C9 178.0(3) . . . . ? C7 C8 C9 C10 0.2(5) . . . . ? C8 C9 C10 C11 -0.3(6) . . . . ? C9 C10 C11 N3 0.2(6) . . . . ? C7 N3 C11 C10 0.1(5) . . . . ? C15 N4 C12 C13 -0.2(3) . . . . ? Ti1 N4 C12 C13 -178.6(2) . . . . ? N4 C12 C13 C14 0.3(3) . . . . ? C12 C13 C14 C15 -0.3(3) . . . . ? C12 N4 C15 C14 0.0(3) . . . . ? Ti1 N4 C15 C14 178.80(18) . . . . ? C12 N4 C15 C16 -179.7(2) . . . . ? Ti1 N4 C15 C16 -0.9(3) . . . . ? C13 C14 C15 N4 0.2(3) . . . . ? C13 C14 C15 C16 179.8(3) . . . . ? C17 N5 C16 C15 -178.5(2) . . . . ? Ti1 N5 C16 C15 1.4(3) . . . . ? N4 C15 C16 N5 -0.4(4) . . . . ? C14 C15 C16 N5 180.0(3) . . . . ? C16 N5 C17 C18 108.1(3) . . . . ? Ti1 N5 C17 C18 -71.8(3) . . . . ? C22 N6 C18 C19 0.0(4) . . . . ? C22 N6 C18 C17 -177.7(3) . . . . ? N5 C17 C18 C19 142.6(3) . . . . ? N5 C17 C18 N6 -39.7(4) . . . . ? N6 C18 C19 C20 0.0(5) . . . . ? C17 C18 C19 C20 177.7(3) . . . . ? C18 C19 C20 C21 0.4(5) . . . . ? C19 C20 C21 C22 -0.7(5) . . . . ? C20 C21 C22 N6 0.7(5) . . . . ? C18 N6 C22 C21 -0.3(5) . . . . ? Ti1 O1 C23 C25 105.2(5) . . . . ? Ti1 O1 C23 C24 -131.1(4) . . . . ? C26' O2 C26 C27 -73.7(9) . . . . ? Ti1 O2 C26 C27 92.4(12) . . . . ? C26' O2 C26 C28 44.8(9) . . . . ? Ti1 O2 C26 C28 -149.1(10) . . . . ? C26 O2 C26' C27' 111.2(16) . . . . ? Ti1 O2 C26' C27' -46(2) . . . . ? C26 O2 C26' C28' -58.2(8) . . . . ? Ti1 O2 C26' C28' 144.2(10) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.12 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.268 _refine_diff_density_min -1.170 _refine_diff_density_rms 0.086 _database_code_depnum_ccdc_archive 'CCDC 862428' data_t _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H36 N4 O2 Ti' _chemical_formula_sum 'C30 H36 N4 O2 Ti' _chemical_formula_weight 532.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.268(2) _cell_length_b 11.468(3) _cell_length_c 24.648(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.635(4) _cell_angle_gamma 90.00 _cell_volume 2852.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5656 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 26.95 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.332 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8954 _exptl_absorpt_correction_T_max 0.9127 _exptl_absorpt_process_details 'SADABS (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14823 _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_unetI/netI 0.0559 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5014 _reflns_number_gt 4353 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction 'SAINT (Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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. During the refinement, the command 'omit -2 50' was used to omit the reflections above 50 degree. DFIX restraints were used for reasonable bond distances between c25 C26, C25 C27, C28 C30, c28 C29, C28 O2 and C25 O1. Thermal motion of o2 c28 and C25 C26 O1 are restrained by commond 'SIMU'. ; _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^)+(0.0926P)^2^+10.2012P] 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_number_reflns 5014 _refine_ls_number_parameters 338 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0987 _refine_ls_R_factor_gt 0.0894 _refine_ls_wR_factor_ref 0.2362 _refine_ls_wR_factor_gt 0.2296 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.136 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.28170(8) 0.20565(7) 0.36354(3) 0.0297(3) Uani 1 1 d . A . O1 O 0.1275(3) 0.1631(3) 0.32203(13) 0.0391(8) Uani 1 1 d DU . . N1 N 0.3534(4) 0.0335(3) 0.37575(16) 0.0318(9) Uani 1 1 d . . . C1 C 0.4693(5) 0.0156(4) 0.4133(2) 0.0338(10) Uani 1 1 d . . . N2 N 0.4689(4) 0.2169(3) 0.43118(16) 0.0316(9) Uani 1 1 d . . . O2 O 0.3703(4) 0.2541(3) 0.31294(15) 0.0436(9) Uani 1 1 d DU . . C2 C 0.5029(5) -0.1032(4) 0.4165(2) 0.0394(12) Uani 1 1 d . . . H2A H 0.5775 -0.1381 0.4392 0.047 Uiso 1 1 calc R . . N3 N 0.2365(4) 0.3735(3) 0.38896(16) 0.0313(9) Uani 1 1 d . . . C3 C 0.4026(5) -0.1597(4) 0.3790(2) 0.0387(11) Uani 1 1 d . . . H3A H 0.3967 -0.2408 0.3712 0.046 Uiso 1 1 calc R . . N4 N 0.1966(4) 0.1795(3) 0.44112(16) 0.0312(9) Uani 1 1 d . . . C4 C 0.3142(5) -0.0743(4) 0.3556(2) 0.0338(11) Uani 1 1 d . . . H4A H 0.2365 -0.0889 0.3289 0.041 Uiso 1 1 calc R . . C5 C 0.5259(5) 0.1173(4) 0.4426(2) 0.0362(11) Uani 1 1 d . . . H5A H 0.6040 0.1113 0.4699 0.043 Uiso 1 1 calc R . . C6 C 0.5268(5) 0.3193(4) 0.4632(2) 0.0361(11) Uani 1 1 d . . . H6A H 0.5808 0.2926 0.4985 0.043 Uiso 1 1 calc R . . H6B H 0.4543 0.3687 0.4720 0.043 Uiso 1 1 calc R . . C7 C 0.6132(5) 0.3923(4) 0.4322(2) 0.0347(11) Uani 1 1 d . . . C8 C 0.7274(5) 0.3455(5) 0.4177(2) 0.0446(13) Uani 1 1 d . . . H8A H 0.7508 0.2668 0.4266 0.053 Uiso 1 1 calc R . . C9 C 0.8071(6) 0.4128(5) 0.3903(3) 0.0524(15) Uani 1 1 d . . . H9A H 0.8837 0.3794 0.3801 0.063 Uiso 1 1 calc R . . C10 C 0.7756(6) 0.5292(5) 0.3777(3) 0.0558(16) Uani 1 1 d . . . H10A H 0.8308 0.5754 0.3593 0.067 Uiso 1 1 calc R . . C11 C 0.6621(6) 0.5769(5) 0.3925(3) 0.0568(16) Uani 1 1 d . . . H11A H 0.6398 0.6561 0.3843 0.068 Uiso 1 1 calc R . . C12 C 0.5818(5) 0.5085(5) 0.4192(2) 0.0433(13) Uani 1 1 d . . . H12A H 0.5042 0.5414 0.4288 0.052 Uiso 1 1 calc R . . C13 C 0.1841(5) 0.3834(4) 0.4366(2) 0.0332(10) Uani 1 1 d . A . C14 C 0.1627(5) 0.5005(4) 0.4478(2) 0.0384(11) Uani 1 1 d . . . H14A H 0.1282 0.5308 0.4781 0.046 Uiso 1 1 calc R A . C15 C 0.2026(5) 0.5643(4) 0.4050(2) 0.0402(12) Uani 1 1 d . A . H15A H 0.2001 0.6467 0.4009 0.048 Uiso 1 1 calc R . . C16 C 0.2466(5) 0.4847(4) 0.3696(2) 0.0354(11) Uani 1 1 d . A . H16A H 0.2787 0.5044 0.3370 0.042 Uiso 1 1 calc R . . C17 C 0.1660(4) 0.2757(4) 0.4636(2) 0.0336(10) Uani 1 1 d . A . H17A H 0.1325 0.2747 0.4971 0.040 Uiso 1 1 calc R . . C18 C 0.1747(5) 0.0682(4) 0.4678(2) 0.0356(11) Uani 1 1 d . A . H18A H 0.1561 0.0839 0.5051 0.043 Uiso 1 1 calc R . . H18B H 0.2564 0.0206 0.4721 0.043 Uiso 1 1 calc R . . C19 C 0.0604(5) -0.0001(4) 0.4348(2) 0.0334(10) Uani 1 1 d . . . C20 C 0.0669(5) -0.1211(5) 0.4313(2) 0.0451(13) Uani 1 1 d . A . H20A H 0.1452 -0.1602 0.4486 0.054 Uiso 1 1 calc R . . C21 C -0.0387(6) -0.1859(5) 0.4031(3) 0.0529(15) Uani 1 1 d . . . H21A H -0.0321 -0.2684 0.4010 0.063 Uiso 1 1 calc R A . C22 C -0.1526(6) -0.1302(5) 0.3783(3) 0.0528(15) Uani 1 1 d . A . H22A H -0.2249 -0.1744 0.3591 0.063 Uiso 1 1 calc R . . C23 C -0.1627(5) -0.0097(5) 0.3811(2) 0.0453(13) Uani 1 1 d . . . H23A H -0.2417 0.0286 0.3639 0.054 Uiso 1 1 calc R A . C24 C -0.0554(5) 0.0549(4) 0.4094(2) 0.0384(11) Uani 1 1 d . A . H24A H -0.0620 0.1374 0.4113 0.046 Uiso 1 1 calc R . . C25 C 0.0559(6) 0.1594(6) 0.2658(3) 0.0819(17) Uani 1 1 d DU . . H25 H 0.1044 0.2089 0.2427 0.098 Uiso 1 1 calc R . . C26 C 0.0503(8) 0.0374(6) 0.2436(3) 0.0828(17) Uani 1 1 d DU . . H26A H 0.1406 0.0090 0.2441 0.124 Uiso 1 1 calc R . . H26B H 0.0007 0.0368 0.2056 0.124 Uiso 1 1 calc R . . H26C H 0.0061 -0.0133 0.2666 0.124 Uiso 1 1 calc R . . C27 C -0.0791(7) 0.2112(8) 0.2638(3) 0.085(3) Uani 1 1 d D . . H27A H -0.1251 0.1686 0.2891 0.128 Uiso 1 1 calc R . . H27B H -0.1301 0.2054 0.2262 0.128 Uiso 1 1 calc R . . H27C H -0.0702 0.2933 0.2748 0.128 Uiso 1 1 calc R . . C28 C 0.4378(8) 0.2753(6) 0.2688(4) 0.100(3) Uani 1 1 d DU A 1 H28 H 0.3846 0.2323 0.2369 0.119 Uiso 1 1 calc R A 1 C29 C 0.5701(8) 0.2159(8) 0.2781(4) 0.099(3) Uani 1 1 d D . . H29A H 0.6049 0.2108 0.3178 0.149 Uiso 1 1 calc R A 1 H29B H 0.6316 0.2608 0.2602 0.149 Uiso 1 1 calc R A 1 H29C H 0.5602 0.1373 0.2623 0.149 Uiso 1 1 calc R A 1 C30 C 0.4337(11) 0.3997(6) 0.2499(4) 0.108(4) Uani 1 1 d D . . H30A H 0.3444 0.4311 0.2486 0.162 Uiso 1 1 calc R A 1 H30B H 0.4565 0.4036 0.2131 0.162 Uiso 1 1 calc R A 1 H30C H 0.4976 0.4457 0.2758 0.162 Uiso 1 1 calc R A 1 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 0.0340(5) 0.0224(4) 0.0322(5) 0.0001(3) 0.0045(3) -0.0023(3) O1 0.0435(19) 0.0323(18) 0.0369(18) -0.0010(14) -0.0048(15) 0.0008(15) N1 0.035(2) 0.024(2) 0.036(2) -0.0028(16) 0.0067(17) -0.0001(16) C1 0.029(2) 0.029(2) 0.045(3) 0.002(2) 0.011(2) 0.0027(19) N2 0.031(2) 0.027(2) 0.036(2) -0.0046(16) 0.0045(16) -0.0030(16) O2 0.057(2) 0.0340(18) 0.044(2) 0.0051(15) 0.0200(17) 0.0006(17) C2 0.036(3) 0.032(3) 0.052(3) 0.007(2) 0.014(2) 0.006(2) N3 0.032(2) 0.0241(19) 0.037(2) 0.0024(16) 0.0046(16) -0.0013(16) C3 0.044(3) 0.023(2) 0.053(3) -0.002(2) 0.021(2) 0.000(2) N4 0.028(2) 0.025(2) 0.040(2) 0.0030(16) 0.0051(16) -0.0038(15) C4 0.037(3) 0.026(2) 0.041(3) -0.0047(19) 0.014(2) -0.004(2) C5 0.034(3) 0.034(3) 0.040(3) 0.000(2) 0.006(2) 0.001(2) C6 0.033(2) 0.031(3) 0.043(3) -0.009(2) 0.002(2) -0.002(2) C7 0.028(2) 0.032(3) 0.042(3) -0.011(2) 0.000(2) -0.0012(19) C8 0.040(3) 0.035(3) 0.057(3) -0.011(2) 0.006(2) -0.002(2) C9 0.038(3) 0.051(3) 0.070(4) -0.018(3) 0.014(3) -0.008(3) C10 0.056(4) 0.047(3) 0.067(4) -0.017(3) 0.018(3) -0.025(3) C11 0.060(4) 0.034(3) 0.077(4) -0.005(3) 0.015(3) -0.010(3) C12 0.035(3) 0.033(3) 0.060(3) -0.012(2) 0.006(2) -0.004(2) C13 0.030(2) 0.027(2) 0.043(3) -0.002(2) 0.005(2) -0.0022(19) C14 0.030(2) 0.032(3) 0.052(3) -0.008(2) 0.007(2) 0.000(2) C15 0.034(3) 0.025(2) 0.061(3) -0.003(2) 0.005(2) -0.001(2) C16 0.033(2) 0.024(2) 0.047(3) 0.004(2) 0.002(2) -0.0016(19) C17 0.027(2) 0.032(3) 0.041(3) 0.001(2) 0.005(2) -0.0009(19) C18 0.034(3) 0.031(3) 0.044(3) 0.010(2) 0.010(2) -0.002(2) C19 0.033(2) 0.027(2) 0.044(3) 0.002(2) 0.015(2) -0.0039(19) C20 0.042(3) 0.032(3) 0.068(4) 0.001(2) 0.026(3) 0.002(2) C21 0.052(3) 0.030(3) 0.083(4) -0.013(3) 0.030(3) -0.012(3) C22 0.049(3) 0.047(3) 0.065(4) -0.014(3) 0.018(3) -0.018(3) C23 0.034(3) 0.046(3) 0.056(3) 0.004(3) 0.008(2) -0.006(2) C24 0.039(3) 0.030(3) 0.047(3) 0.000(2) 0.010(2) -0.007(2) C25 0.080(3) 0.086(4) 0.066(3) -0.026(3) -0.021(3) 0.016(3) C26 0.081(3) 0.087(4) 0.067(3) -0.026(3) -0.021(3) 0.016(3) C27 0.084(5) 0.096(6) 0.063(5) -0.011(4) -0.023(4) 0.041(5) C28 0.104(6) 0.094(5) 0.118(6) 0.031(5) 0.067(5) 0.018(5) C29 0.104(7) 0.100(7) 0.107(7) 0.034(5) 0.055(6) 0.043(6) C30 0.162(10) 0.072(5) 0.116(7) 0.030(5) 0.093(7) 0.015(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O2 1.764(3) . ? Ti1 O1 1.787(3) . ? Ti1 N3 2.103(4) . ? Ti1 N1 2.109(4) . ? Ti1 N4 2.264(4) . ? Ti1 N2 2.304(4) . ? O1 C25 1.444(6) . ? N1 C4 1.366(6) . ? N1 C1 1.381(6) . ? C1 C2 1.404(7) . ? C1 C5 1.437(7) . ? N2 C5 1.291(6) . ? N2 C6 1.478(6) . ? O2 C28 1.414(7) . ? C2 C3 1.408(8) . ? C2 H2A 0.9500 . ? N3 C16 1.372(6) . ? N3 C13 1.383(6) . ? C3 C4 1.386(7) . ? C3 H3A 0.9500 . ? N4 C17 1.300(6) . ? N4 C18 1.472(6) . ? C4 H4A 0.9500 . ? C5 H5A 0.9500 . ? C6 C7 1.524(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C12 1.394(7) . ? C7 C8 1.395(7) . ? C8 C9 1.388(8) . ? C8 H8A 0.9500 . ? C9 C10 1.394(9) . ? C9 H9A 0.9500 . ? C10 C11 1.395(9) . ? C10 H10A 0.9500 . ? C11 C12 1.389(8) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.396(7) . ? C13 C17 1.431(7) . ? C14 C15 1.406(8) . ? C14 H14A 0.9500 . ? C15 C16 1.394(7) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C19 1.517(7) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C24 1.389(7) . ? C19 C20 1.393(7) . ? C20 C21 1.391(8) . ? C20 H20A 0.9500 . ? C21 C22 1.373(9) . ? C21 H21A 0.9500 . ? C22 C23 1.389(8) . ? C22 H22A 0.9500 . ? C23 C24 1.403(7) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C26 1.4994(11) . ? C25 C27 1.4999(11) . ? C25 H25 1.0000 . ? 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 C29 1.4988(11) . ? C28 C30 1.4988(11) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ti1 O1 101.50(18) . . ? O2 Ti1 N3 95.35(16) . . ? O1 Ti1 N3 101.51(16) . . ? O2 Ti1 N1 100.58(16) . . ? O1 Ti1 N1 94.32(16) . . ? N3 Ti1 N1 154.82(16) . . ? O2 Ti1 N4 165.64(16) . . ? O1 Ti1 N4 90.47(15) . . ? N3 Ti1 N4 74.27(14) . . ? N1 Ti1 N4 86.24(15) . . ? O2 Ti1 N2 91.37(16) . . ? O1 Ti1 N2 164.19(15) . . ? N3 Ti1 N2 86.21(14) . . ? N1 Ti1 N2 74.11(14) . . ? N4 Ti1 N2 78.26(14) . . ? C25 O1 Ti1 142.9(4) . . ? C4 N1 C1 105.6(4) . . ? C4 N1 Ti1 136.4(3) . . ? C1 N1 Ti1 118.0(3) . . ? N1 C1 C2 110.8(4) . . ? N1 C1 C5 115.7(4) . . ? C2 C1 C5 133.4(5) . . ? C5 N2 C6 117.8(4) . . ? C5 N2 Ti1 113.1(3) . . ? C6 N2 Ti1 129.1(3) . . ? C28 O2 Ti1 171.0(4) . . ? C1 C2 C3 105.4(4) . . ? C1 C2 H2A 127.3 . . ? C3 C2 H2A 127.3 . . ? C16 N3 C13 106.6(4) . . ? C16 N3 Ti1 135.4(3) . . ? C13 N3 Ti1 118.0(3) . . ? C4 C3 C2 107.0(4) . . ? C4 C3 H3A 126.5 . . ? C2 C3 H3A 126.5 . . ? C17 N4 C18 118.5(4) . . ? C17 N4 Ti1 114.1(3) . . ? C18 N4 Ti1 127.4(3) . . ? N1 C4 C3 111.2(4) . . ? N1 C4 H4A 124.4 . . ? C3 C4 H4A 124.4 . . ? N2 C5 C1 118.9(4) . . ? N2 C5 H5A 120.5 . . ? C1 C5 H5A 120.5 . . ? N2 C6 C7 112.5(4) . . ? N2 C6 H6A 109.1 . . ? C7 C6 H6A 109.1 . . ? N2 C6 H6B 109.1 . . ? C7 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? C12 C7 C8 118.6(5) . . ? C12 C7 C6 120.6(4) . . ? C8 C7 C6 120.8(5) . . ? C9 C8 C7 120.7(5) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C8 C9 C10 120.5(5) . . ? C8 C9 H9A 119.8 . . ? C10 C9 H9A 119.8 . . ? C9 C10 C11 119.2(6) . . ? C9 C10 H10A 120.4 . . ? C11 C10 H10A 120.4 . . ? C12 C11 C10 120.0(6) . . ? C12 C11 H11A 120.0 . . ? C10 C11 H11A 120.0 . . ? C11 C12 C7 121.1(5) . . ? C11 C12 H12A 119.5 . . ? C7 C12 H12A 119.5 . . ? N3 C13 C14 110.3(4) . . ? N3 C13 C17 115.4(4) . . ? C14 C13 C17 134.3(5) . . ? C13 C14 C15 105.9(5) . . ? C13 C14 H14A 127.1 . . ? C15 C14 H14A 127.1 . . ? C16 C15 C14 107.6(4) . . ? C16 C15 H15A 126.2 . . ? C14 C15 H15A 126.2 . . ? N3 C16 C15 109.6(5) . . ? N3 C16 H16A 125.2 . . ? C15 C16 H16A 125.2 . . ? N4 C17 C13 118.1(4) . . ? N4 C17 H17A 120.9 . . ? C13 C17 H17A 120.9 . . ? N4 C18 C19 112.0(4) . . ? N4 C18 H18A 109.2 . . ? C19 C18 H18A 109.2 . . ? N4 C18 H18B 109.2 . . ? C19 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? C24 C19 C20 118.2(5) . . ? C24 C19 C18 121.4(4) . . ? C20 C19 C18 120.4(5) . . ? C21 C20 C19 121.4(5) . . ? C21 C20 H20A 119.3 . . ? C19 C20 H20A 119.3 . . ? C22 C21 C20 119.7(5) . . ? C22 C21 H21A 120.2 . . ? C20 C21 H21A 120.2 . . ? C21 C22 C23 120.4(5) . . ? C21 C22 H22A 119.8 . . ? C23 C22 H22A 119.8 . . ? C22 C23 C24 119.4(5) . . ? C22 C23 H23A 120.3 . . ? C24 C23 H23A 120.3 . . ? C19 C24 C23 120.8(5) . . ? C19 C24 H24A 119.6 . . ? C23 C24 H24A 119.6 . . ? O1 C25 C26 110.8(5) . . ? O1 C25 C27 108.9(5) . . ? C26 C25 C27 112.6(6) . . ? O1 C25 H25 108.1 . . ? C26 C25 H25 108.1 . . ? C27 C25 H25 108.1 . . ? 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 . . ? O2 C28 C29 111.3(6) . . ? O2 C28 C30 114.4(6) . . ? C29 C28 C30 116.9(7) . . ? O2 C28 H28 104.2 . . ? C29 C28 H28 104.2 . . ? C30 C28 H28 104.2 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.290 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.096 _database_code_depnum_ccdc_archive 'CCDC 870370'