# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full ? _journal_coden_cambridge 182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Ba L. Tran' 'Marlena P. Washington' 'Xinfeng Gao.' 'Maren Pink' 'Daniel J. Mindiola' _publ_contact_author_email batran@umail.iu.edu _publ_contact_author_name 'Ba L. Tran' data_08146 _database_code_depnum_ccdc_archive 'CCDC 829540' #TrackingRef '08146.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H55 Cl N3 Ti' _chemical_formula_sum 'C43 H55 Cl N3 Ti' _chemical_formula_weight 697.25 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.6177(10) _cell_length_b 33.391(3) _cell_length_c 11.5326(11) _cell_angle_alpha 90.00 _cell_angle_beta 107.582(2) _cell_angle_gamma 90.00 _cell_volume 3897.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9977 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 27.3 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.188 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1492 _exptl_absorpt_coefficient_mu 0.321 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.9099 _exptl_absorpt_correction_T_max 0.9156 _exptl_absorpt_process_details 'SADABS, R. Blessing; 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details '0.30 degree frames measured for 2 seconds each' _diffrn_measurement_method 'omega and phi scans' _diffrn_measurement_device 'APEX Kappa Duo' _diffrn_measurement_device_type Kappa _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker APEXII' _diffrn_detector_area_resol_mean 83.33 _diffrn_reflns_number 39483 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 27.60 _reflns_number_total 9003 _reflns_number_gt 7423 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II v.2.2 (Bruker, 2007)' _computing_cell_refinement 'APEX II v.2.2 (Bruker, 2007)' _computing_data_reduction 'APEX II v.2.2 (Bruker, 2007)' _computing_structure_solution 'SIR-2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Bruker, 2008)' _computing_publication_material 'SHELXTL (Bruker, 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. ; _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^)+(0.0390P)^2^+2.3800P] 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 9003 _refine_ls_number_parameters 478 _refine_ls_number_restraints 250 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1045 _refine_ls_wR_factor_gt 0.0985 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.002 _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 0.11448(3) 0.608614(8) 0.59304(3) 0.02085(8) Uani 1 1 d . A . Cl1 Cl -0.10170(4) 0.591084(14) 0.57626(4) 0.03197(11) Uani 1 1 d . . . N1 N 0.14858(13) 0.59568(4) 0.43310(12) 0.0205(3) Uani 1 1 d . . . N2 N 0.22460(13) 0.56207(4) 0.67368(12) 0.0216(3) Uani 1 1 d . . . N3 N 0.15073(15) 0.66423(4) 0.64105(14) 0.0285(3) Uani 1 1 d . . . C1 C 0.13988(19) 0.54620(5) 0.27355(16) 0.0310(4) Uani 1 1 d . . . H1A H 0.2072 0.5608 0.2482 0.047 Uiso 1 1 calc R . . H1B H 0.0521 0.5531 0.2194 0.047 Uiso 1 1 calc R . . H1C H 0.1545 0.5173 0.2693 0.047 Uiso 1 1 calc R . . C2 C 0.14885(16) 0.55751(5) 0.40151(14) 0.0218(3) Uani 1 1 d . A . C3 C 0.15768(17) 0.52594(5) 0.48487(15) 0.0239(3) Uani 1 1 d . . . H3 H 0.1321 0.5003 0.4499 0.029 Uiso 1 1 calc R A . C4 C 0.19845(16) 0.52727(5) 0.61031(15) 0.0233(3) Uani 1 1 d . A . C5 C 0.2120(2) 0.48814(5) 0.67779(17) 0.0345(4) Uani 1 1 d . . . H5A H 0.3004 0.4863 0.7367 0.052 Uiso 1 1 calc R A . H5B H 0.1992 0.4659 0.6199 0.052 Uiso 1 1 calc R . . H5C H 0.1454 0.4867 0.7208 0.052 Uiso 1 1 calc R . . C6 C 0.14863(17) 0.62676(5) 0.34577(14) 0.0233(3) Uani 1 1 d . . . C7 C 0.26834(18) 0.64572(5) 0.35211(16) 0.0294(4) Uani 1 1 d . . . C8 C 0.2648(2) 0.67653(6) 0.26992(18) 0.0392(5) Uani 1 1 d . . . H8 H 0.3446 0.6897 0.2716 0.047 Uiso 1 1 calc R . . C9 C 0.1485(2) 0.68840(6) 0.18631(18) 0.0412(5) Uani 1 1 d . . . H9 H 0.1485 0.7095 0.1312 0.049 Uiso 1 1 calc R . . C10 C 0.0325(2) 0.66969(6) 0.18277(17) 0.0352(4) Uani 1 1 d . . . H10 H -0.0474 0.6782 0.1252 0.042 Uiso 1 1 calc R . . C11 C 0.02937(17) 0.63844(5) 0.26157(15) 0.0259(4) Uani 1 1 d . . . C12 C 0.39818(18) 0.63309(6) 0.44190(19) 0.0361(4) Uani 1 1 d . . . H12 H 0.3773 0.6166 0.5061 0.043 Uiso 1 1 calc R . . C13 C 0.4755(3) 0.60675(11) 0.3803(3) 0.0787(9) Uani 1 1 d . . . H13A H 0.4244 0.5825 0.3490 0.118 Uiso 1 1 calc R . . H13B H 0.5599 0.5993 0.4393 0.118 Uiso 1 1 calc R . . H13C H 0.4920 0.6215 0.3128 0.118 Uiso 1 1 calc R . . C14 C 0.4797(3) 0.66841(8) 0.5044(3) 0.0739(9) Uani 1 1 d . . . H14A H 0.4281 0.6845 0.5448 0.111 Uiso 1 1 calc R . . H14B H 0.5037 0.6849 0.4440 0.111 Uiso 1 1 calc R . . H14C H 0.5601 0.6587 0.5649 0.111 Uiso 1 1 calc R . . C15 C -0.10154(18) 0.61891(5) 0.25312(16) 0.0297(4) Uani 1 1 d . . . H15A H -0.0838 0.5954 0.3094 0.036 Uiso 1 1 calc R . . C16 C -0.1710(2) 0.60360(7) 0.12453(19) 0.0443(5) Uani 1 1 d . . . H16A H -0.1110 0.5860 0.0981 0.066 Uiso 1 1 calc R . . H16B H -0.1960 0.6264 0.0687 0.066 Uiso 1 1 calc R . . H16C H -0.2503 0.5886 0.1245 0.066 Uiso 1 1 calc R . . C17 C -0.1923(2) 0.64746(6) 0.2930(2) 0.0415(5) Uani 1 1 d . . . H17A H -0.1513 0.6549 0.3783 0.062 Uiso 1 1 calc R . . H17B H -0.2771 0.6343 0.2842 0.062 Uiso 1 1 calc R . . H17C H -0.2068 0.6716 0.2422 0.062 Uiso 1 1 calc R . . C18 C 0.3147(19) 0.5639(6) 0.799(2) 0.0198(15) Uani 0.437(5) 1 d PDU A 1 C19 C 0.448(2) 0.5551(8) 0.819(3) 0.0276(6) Uani 0.437(5) 1 d PDU A 1 C20 C 0.529(2) 0.5518(12) 0.938(3) 0.0372(5) Uani 0.437(5) 1 d PDU A 1 H20 H 0.6185 0.5443 0.9539 0.045 Uiso 0.437(5) 1 calc PR A 1 C21 C 0.480(2) 0.5591(11) 1.034(3) 0.039(2) Uani 0.437(5) 1 d PDU A 1 H21 H 0.5372 0.5577 1.1150 0.047 Uiso 0.437(5) 1 calc PR A 1 C22 C 0.3498(19) 0.5682(7) 1.0136(19) 0.036(2) Uani 0.437(5) 1 d PDU A 1 H22 H 0.3176 0.5731 1.0807 0.043 Uiso 0.437(5) 1 calc PR A 1 C23 C 0.2637(12) 0.5704(5) 0.8959(18) 0.0299(16) Uani 0.437(5) 1 d PDU A 1 C24 C 0.509(3) 0.5526(12) 0.715(3) 0.0367(5) Uani 0.437(5) 1 d PDU A 1 H24 H 0.4402 0.5625 0.6405 0.044 Uiso 0.437(5) 1 calc PR A 1 C25 C 0.544(5) 0.5104(12) 0.689(5) 0.062(2) Uani 0.437(5) 1 d PDU A 1 H25A H 0.4631 0.4949 0.6554 0.092 Uiso 0.437(5) 1 d PR A 1 H25B H 0.5972 0.4983 0.7656 0.092 Uiso 0.437(5) 1 d PR A 1 H25C H 0.5954 0.5104 0.6309 0.092 Uiso 0.437(5) 1 d PR A 1 C26 C 0.627(5) 0.5805(13) 0.737(6) 0.056(2) Uani 0.437(5) 1 d PDU A 1 H26A H 0.6054 0.6074 0.7589 0.084 Uiso 0.437(5) 1 d PR A 1 H26B H 0.6557 0.5819 0.6641 0.084 Uiso 0.437(5) 1 d PR A 1 H26C H 0.6987 0.5693 0.8045 0.084 Uiso 0.437(5) 1 d PR A 1 C27 C 0.1221(9) 0.5833(2) 0.8770(8) 0.0367(11) Uani 0.437(5) 1 d PDU A 1 H27 H 0.0838 0.5917 0.7902 0.044 Uiso 0.437(5) 1 calc PR A 1 C28 C 0.1130(9) 0.6188(2) 0.9577(8) 0.0539(13) Uani 0.437(5) 1 d PDU A 1 H28A H 0.1405 0.6104 1.0431 0.081 Uiso 0.437(5) 1 d PR A 1 H28B H 0.0217 0.6285 0.9350 0.081 Uiso 0.437(5) 1 d PR A 1 H28C H 0.1711 0.6403 0.9465 0.081 Uiso 0.437(5) 1 d PR A 1 C29 C 0.0418(9) 0.5480(3) 0.8994(7) 0.0497(12) Uani 0.437(5) 1 d PDU A 1 H29A H 0.0421 0.5265 0.8419 0.075 Uiso 0.437(5) 1 d PR A 1 H29B H -0.0493 0.5565 0.8888 0.075 Uiso 0.437(5) 1 d PR A 1 H29C H 0.0814 0.5383 0.9827 0.075 Uiso 0.437(5) 1 d PR A 1 C18D C 0.3070(14) 0.5574(4) 0.7957(15) 0.0198(15) Uani 0.563(5) 1 d PDU A 2 C19D C 0.4438(16) 0.5539(6) 0.817(2) 0.0276(6) Uani 0.563(5) 1 d PDU A 2 C20D C 0.5243(17) 0.5521(9) 0.936(2) 0.0372(5) Uani 0.563(5) 1 d PDU A 2 H20D H 0.6170 0.5494 0.9519 0.045 Uiso 0.563(5) 1 calc PR A 2 C21D C 0.4734(16) 0.5541(9) 1.032(2) 0.039(2) Uani 0.563(5) 1 d PDU A 2 H21D H 0.5295 0.5509 1.1133 0.047 Uiso 0.563(5) 1 calc PR A 2 C22D C 0.3416(15) 0.5607(5) 1.0102(15) 0.036(2) Uani 0.563(5) 1 d PDU A 2 H22D H 0.3079 0.5644 1.0770 0.043 Uiso 0.563(5) 1 calc PR A 2 C23D C 0.2551(9) 0.5623(4) 0.8928(14) 0.0299(16) Uani 0.563(5) 1 d PDU A 2 C24D C 0.507(2) 0.5535(9) 0.715(3) 0.0367(5) Uani 0.563(5) 1 d PDU A 2 H24D H 0.4378 0.5610 0.6376 0.044 Uiso 0.563(5) 1 calc PR A 2 C25D C 0.557(4) 0.5118(10) 0.698(4) 0.062(2) Uani 0.563(5) 1 d PDU A 2 H25D H 0.4854 0.4922 0.6848 0.092 Uiso 0.563(5) 1 d PR A 2 H25E H 0.6295 0.5043 0.7702 0.092 Uiso 0.563(5) 1 d PR A 2 H25F H 0.5893 0.5124 0.6269 0.092 Uiso 0.563(5) 1 d PR A 2 C26D C 0.619(4) 0.5838(10) 0.737(5) 0.056(2) Uani 0.563(5) 1 d PDU A 2 H26D H 0.5839 0.6103 0.7460 0.084 Uiso 0.563(5) 1 d PR A 2 H26E H 0.6529 0.5839 0.6663 0.084 Uiso 0.563(5) 1 d PR A 2 H26F H 0.6909 0.5771 0.8101 0.084 Uiso 0.563(5) 1 d PR A 2 C27D C 0.1085(6) 0.56647(17) 0.8736(6) 0.0367(11) Uani 0.563(5) 1 d PDU A 2 H27D H 0.0626 0.5637 0.7845 0.044 Uiso 0.563(5) 1 calc PR A 2 C28D C 0.0747(7) 0.60794(19) 0.9126(6) 0.0539(13) Uani 0.563(5) 1 d PDU A 2 H28D H 0.1135 0.6110 1.0008 0.081 Uiso 0.563(5) 1 d PR A 2 H28E H -0.0215 0.6108 0.8909 0.081 Uiso 0.563(5) 1 d PR A 2 H28F H 0.1103 0.6286 0.8709 0.081 Uiso 0.563(5) 1 d PR A 2 C29D C 0.0560(6) 0.53365(19) 0.9386(5) 0.0497(12) Uani 0.563(5) 1 d PDU A 2 H29D H 0.0803 0.5074 0.9141 0.075 Uiso 0.563(5) 1 d PR A 2 H29E H -0.0405 0.5357 0.9167 0.075 Uiso 0.563(5) 1 d PR A 2 H29F H 0.0943 0.5369 1.0267 0.075 Uiso 0.563(5) 1 d PR A 2 C30 C 0.04994(18) 0.69199(5) 0.57878(16) 0.0280(4) Uani 1 1 d . A . C31 C 0.0620(2) 0.71336(5) 0.48003(18) 0.0344(4) Uani 1 1 d . . . H31 H 0.1380 0.7100 0.4539 0.041 Uiso 1 1 calc R A . C32 C -0.0365(2) 0.73969(6) 0.41909(19) 0.0410(5) Uani 1 1 d . A . H32 H -0.0261 0.7543 0.3520 0.049 Uiso 1 1 calc R . . C33 C -0.1492(2) 0.74526(6) 0.45289(18) 0.0395(5) Uani 1 1 d . . . C34 C -0.1608(2) 0.72346(6) 0.55113(18) 0.0381(4) Uani 1 1 d . A . H34 H -0.2375 0.7266 0.5763 0.046 Uiso 1 1 calc R . . C35 C -0.06347(19) 0.69717(6) 0.61343(17) 0.0333(4) Uani 1 1 d . . . H35 H -0.0741 0.6825 0.6805 0.040 Uiso 1 1 calc R A . C36 C -0.2556(3) 0.77372(8) 0.3844(2) 0.0585(7) Uani 1 1 d . A . H36A H -0.3424 0.7619 0.3756 0.088 Uiso 1 1 calc R . . H36B H -0.2463 0.7788 0.3036 0.088 Uiso 1 1 calc R . . H36C H -0.2473 0.7990 0.4292 0.088 Uiso 1 1 calc R . . C37 C 0.24511(17) 0.67827(5) 0.74735(17) 0.0287(4) Uani 1 1 d . A . C38 C 0.2285(2) 0.71238(6) 0.80990(19) 0.0403(5) Uani 1 1 d . . . H38 H 0.1542 0.7292 0.7766 0.048 Uiso 1 1 calc R A . C39 C 0.3190(2) 0.72210(6) 0.9200(2) 0.0463(5) Uani 1 1 d . A . H39 H 0.3049 0.7455 0.9613 0.056 Uiso 1 1 calc R . . C40 C 0.4290(2) 0.69902(6) 0.9720(2) 0.0402(5) Uani 1 1 d . . . C41 C 0.4489(2) 0.66629(6) 0.9055(2) 0.0423(5) Uani 1 1 d . A . H41 H 0.5254 0.6502 0.9372 0.051 Uiso 1 1 calc R . . C42 C 0.36056(19) 0.65660(6) 0.7947(2) 0.0390(5) Uani 1 1 d . . . H42 H 0.3790 0.6347 0.7499 0.047 Uiso 1 1 calc R A . C43 C 0.5231(2) 0.70933(8) 1.0945(2) 0.0576(6) Uani 1 1 d . A . H43A H 0.5280 0.6869 1.1506 0.086 Uiso 1 1 calc R . . H43B H 0.4916 0.7333 1.1262 0.086 Uiso 1 1 calc R . . H43C H 0.6110 0.7145 1.0866 0.086 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 0.02304(15) 0.01995(14) 0.01985(15) -0.00163(11) 0.00691(11) 0.00165(11) Cl1 0.0251(2) 0.0386(2) 0.0329(2) -0.00210(18) 0.00976(18) -0.00137(18) N1 0.0198(7) 0.0222(6) 0.0189(7) 0.0008(5) 0.0052(5) -0.0003(5) N2 0.0229(7) 0.0239(7) 0.0182(7) -0.0001(5) 0.0065(5) 0.0006(5) N3 0.0302(8) 0.0226(7) 0.0332(8) -0.0051(6) 0.0101(7) 0.0002(6) C1 0.0406(11) 0.0312(9) 0.0219(9) -0.0037(7) 0.0104(8) 0.0030(8) C2 0.0208(8) 0.0246(8) 0.0200(8) -0.0029(6) 0.0060(6) -0.0002(6) C3 0.0267(9) 0.0202(8) 0.0239(8) -0.0030(6) 0.0064(7) -0.0017(6) C4 0.0229(8) 0.0225(8) 0.0245(8) 0.0004(6) 0.0072(7) 0.0001(6) C5 0.0461(12) 0.0243(9) 0.0293(10) 0.0044(7) 0.0058(8) -0.0011(8) C6 0.0283(9) 0.0237(8) 0.0193(8) 0.0000(6) 0.0092(7) -0.0010(7) C7 0.0304(10) 0.0313(9) 0.0288(9) 0.0010(7) 0.0123(8) -0.0032(7) C8 0.0428(12) 0.0412(11) 0.0363(11) 0.0060(9) 0.0162(9) -0.0126(9) C9 0.0556(13) 0.0371(11) 0.0303(10) 0.0117(8) 0.0119(10) -0.0071(9) C10 0.0430(11) 0.0320(9) 0.0253(9) 0.0053(7) 0.0025(8) 0.0016(8) C11 0.0295(9) 0.0262(8) 0.0212(8) -0.0011(6) 0.0063(7) -0.0007(7) C12 0.0260(9) 0.0425(11) 0.0388(11) 0.0079(8) 0.0087(8) -0.0048(8) C13 0.0435(15) 0.113(3) 0.076(2) -0.0134(18) 0.0114(14) 0.0270(16) C14 0.0578(17) 0.0609(16) 0.077(2) 0.0097(14) -0.0189(14) -0.0202(13) C15 0.0264(9) 0.0318(9) 0.0262(9) 0.0013(7) 0.0008(7) 0.0006(7) C16 0.0388(12) 0.0522(13) 0.0341(11) -0.0051(9) -0.0007(9) -0.0079(10) C17 0.0303(10) 0.0480(12) 0.0428(12) 0.0017(9) 0.0060(9) 0.0054(9) C18 0.0277(16) 0.011(4) 0.0188(11) -0.002(2) 0.0032(12) -0.004(2) C19 0.0273(12) 0.0268(13) 0.0262(11) -0.0002(9) 0.0042(10) 0.0011(10) C20 0.0286(13) 0.0428(11) 0.0334(12) 0.0002(9) -0.0009(10) 0.0022(11) C21 0.0414(17) 0.045(6) 0.0214(10) 0.002(2) -0.0035(12) -0.006(2) C22 0.0435(19) 0.043(6) 0.0200(12) -0.002(3) 0.0071(12) -0.004(3) C23 0.0339(14) 0.033(5) 0.0218(11) -0.001(3) 0.0072(12) -0.002(2) C24 0.0270(10) 0.0506(15) 0.0319(10) 0.0050(10) 0.0078(8) 0.0090(10) C25 0.068(5) 0.065(2) 0.061(5) -0.004(2) 0.035(4) 0.021(3) C26 0.034(4) 0.078(5) 0.0589(17) 0.007(3) 0.020(3) -0.001(3) C27 0.0375(17) 0.053(3) 0.0220(11) 0.004(3) 0.0130(12) 0.003(3) C28 0.056(4) 0.059(3) 0.057(4) 0.004(2) 0.032(3) 0.010(2) C29 0.049(2) 0.072(4) 0.032(3) -0.009(2) 0.018(2) -0.022(3) C18D 0.0277(16) 0.011(4) 0.0188(11) -0.002(2) 0.0032(12) -0.004(2) C19D 0.0273(12) 0.0268(13) 0.0262(11) -0.0002(9) 0.0042(10) 0.0011(10) C20D 0.0286(13) 0.0428(11) 0.0334(12) 0.0002(9) -0.0009(10) 0.0022(11) C21D 0.0414(17) 0.045(6) 0.0214(10) 0.002(2) -0.0035(12) -0.006(2) C22D 0.0435(19) 0.043(6) 0.0200(12) -0.002(3) 0.0071(12) -0.004(3) C23D 0.0339(14) 0.033(5) 0.0218(11) -0.001(3) 0.0072(12) -0.002(2) C24D 0.0270(10) 0.0506(15) 0.0319(10) 0.0050(10) 0.0078(8) 0.0090(10) C25D 0.068(5) 0.065(2) 0.061(5) -0.004(2) 0.035(4) 0.021(3) C26D 0.034(4) 0.078(5) 0.0589(17) 0.007(3) 0.020(3) -0.001(3) C27D 0.0375(17) 0.053(3) 0.0220(11) 0.004(3) 0.0130(12) 0.003(3) C28D 0.056(4) 0.059(3) 0.057(4) 0.004(2) 0.032(3) 0.010(2) C29D 0.049(2) 0.072(4) 0.032(3) -0.009(2) 0.018(2) -0.022(3) C30 0.0313(9) 0.0221(8) 0.0300(9) -0.0065(7) 0.0083(7) -0.0014(7) C31 0.0400(11) 0.0289(9) 0.0380(11) -0.0034(8) 0.0172(9) -0.0021(8) C32 0.0563(13) 0.0352(10) 0.0331(11) 0.0032(8) 0.0161(10) 0.0056(9) C33 0.0455(12) 0.0374(10) 0.0317(10) -0.0056(8) 0.0057(9) 0.0090(9) C34 0.0359(11) 0.0442(11) 0.0356(11) -0.0054(9) 0.0129(9) 0.0093(9) C35 0.0367(10) 0.0337(10) 0.0312(10) -0.0016(8) 0.0129(8) 0.0034(8) C36 0.0634(16) 0.0637(15) 0.0430(13) 0.0042(11) 0.0077(12) 0.0259(13) C37 0.0272(9) 0.0224(8) 0.0368(10) -0.0003(7) 0.0099(8) -0.0018(7) C38 0.0383(11) 0.0317(10) 0.0418(11) -0.0080(8) -0.0017(9) 0.0100(8) C39 0.0429(12) 0.0412(11) 0.0462(13) -0.0147(10) 0.0005(10) 0.0062(9) C40 0.0298(10) 0.0431(11) 0.0416(12) 0.0048(9) 0.0017(9) -0.0037(9) C41 0.0274(10) 0.0307(10) 0.0610(14) 0.0078(9) 0.0016(9) 0.0013(8) C42 0.0288(10) 0.0246(9) 0.0620(14) -0.0050(9) 0.0112(10) 0.0000(7) C43 0.0421(13) 0.0756(17) 0.0441(14) 0.0031(12) -0.0035(11) -0.0036(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 N3 1.9428(14) . ? Ti1 N2 1.9977(14) . ? Ti1 N1 2.0306(13) . ? Ti1 Cl1 2.3195(6) . ? N1 C2 1.326(2) . ? N1 C6 1.446(2) . ? N2 C4 1.356(2) . ? N2 C18D 1.423(17) . ? N2 C18 1.48(2) . ? N3 C37 1.409(2) . ? N3 C30 1.434(2) . ? C1 C2 1.498(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.411(2) . ? C3 C4 1.380(2) . ? C3 H3 0.9500 . ? C4 C5 1.505(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C11 1.398(2) . ? C6 C7 1.402(2) . ? C7 C8 1.392(3) . ? C7 C12 1.513(3) . ? C8 C9 1.376(3) . ? C8 H8 0.9500 . ? C9 C10 1.370(3) . ? C9 H9 0.9500 . ? C10 C11 1.391(2) . ? C10 H10 0.9500 . ? C11 C15 1.512(2) . ? C12 C14 1.511(3) . ? C12 C13 1.518(3) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.522(3) . ? C15 C16 1.531(3) . ? C15 H15A 1.0000 . ? 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 C19 1.397(11) . ? C18 C23 1.397(10) . ? C19 C20 1.386(11) . ? C19 C24 1.519(10) . ? C20 C21 1.377(11) . ? C20 H20 0.9500 . ? C21 C22 1.362(11) . ? C21 H21 0.9500 . ? C22 C23 1.391(11) . ? C22 H22 0.9500 . ? C23 C27 1.515(10) . ? C24 C25 1.516(11) . ? C24 C26 1.523(12) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C25 H25D 0.8628 . ? C25 H25E 1.1073 . ? C25 H25F 0.9742 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C26 H26D 1.1149 . ? C26 H26E 0.9443 . ? C26 H26F 0.9126 . ? C27 C29 1.520(8) . ? C27 C28 1.530(8) . ? C27 H27 1.0000 . ? C27 H28F 1.5191 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C28 H28D 0.5602 . ? C28 H28E 1.4278 . ? C28 H28F 1.0454 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C29 H29D 1.4131 . ? C29 H29E 1.0385 . ? C29 H29F 1.4524 . ? C18D C23D 1.399(8) . ? C18D C19D 1.402(8) . ? C19D C20D 1.385(8) . ? C19D C24D 1.520(8) . ? C20D C21D 1.374(9) . ? C20D H20D 0.9500 . ? C21D C22D 1.363(9) . ? C21D H21D 0.9500 . ? C22D C23D 1.388(8) . ? C22D H22D 0.9500 . ? C23D C27D 1.512(7) . ? C24D C25D 1.522(10) . ? C24D C26D 1.524(9) . ? C24D H24D 1.0000 . ? C25D H25A 1.1230 . ? C25D H25B 0.8896 . ? C25D H25C 0.9791 . ? C25D H25D 0.9800 . ? C25D H25E 0.9800 . ? C25D H25F 0.9800 . ? C26D H26A 0.8557 . ? C26D H26B 1.0248 . ? C26D H26C 1.0779 . ? C26D H26D 0.9800 . ? C26D H26E 0.9800 . ? C26D H26F 0.9800 . ? C27D C29D 1.525(6) . ? C27D C28D 1.532(6) . ? C27D H29A 1.5028 . ? C27D H27D 1.0000 . ? C28D H28A 1.4577 . ? C28D H28B 0.9719 . ? C28D H28C 1.4580 . ? C28D H28D 0.9800 . ? C28D H28E 0.9800 . ? C28D H28F 0.9800 . ? C29D H29A 1.1064 . ? C29D H29B 1.3325 . ? C29D H29C 0.5230 . ? C29D H29D 0.9800 . ? C29D H29E 0.9800 . ? C29D H29F 0.9800 . ? C30 C31 1.382(3) . ? C30 C35 1.389(3) . ? C31 C32 1.384(3) . ? C31 H31 0.9500 . ? C32 C33 1.378(3) . ? C32 H32 0.9500 . ? C33 C34 1.383(3) . ? C33 C36 1.505(3) . ? C34 C35 1.381(3) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C42 1.386(3) . ? C37 C38 1.388(3) . ? C38 C39 1.380(3) . ? C38 H38 0.9500 . ? C39 C40 1.376(3) . ? C39 H39 0.9500 . ? C40 C41 1.387(3) . ? C40 C43 1.504(3) . ? C41 C42 1.376(3) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 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 N3 Ti1 N2 124.98(6) . . ? N3 Ti1 N1 112.82(6) . . ? N2 Ti1 N1 91.01(5) . . ? N3 Ti1 Cl1 111.77(5) . . ? N2 Ti1 Cl1 105.53(4) . . ? N1 Ti1 Cl1 108.30(4) . . ? C2 N1 C6 119.87(13) . . ? C2 N1 Ti1 118.02(11) . . ? C6 N1 Ti1 121.17(10) . . ? C4 N2 C18D 113.8(6) . . ? C4 N2 C18 122.1(7) . . ? C18D N2 C18 9.0(13) . . ? C4 N2 Ti1 114.84(11) . . ? C18D N2 Ti1 130.1(5) . . ? C18 N2 Ti1 122.6(7) . . ? C37 N3 C30 116.60(14) . . ? C37 N3 Ti1 126.42(12) . . ? C30 N3 Ti1 114.94(11) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 122.44(14) . . ? N1 C2 C1 120.55(15) . . ? C3 C2 C1 117.02(14) . . ? C4 C3 C2 128.74(15) . . ? C4 C3 H3 115.6 . . ? C2 C3 H3 115.6 . . ? N2 C4 C3 122.75(15) . . ? N2 C4 C5 119.54(15) . . ? C3 C4 C5 117.70(15) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 C7 121.79(15) . . ? C11 C6 N1 119.54(15) . . ? C7 C6 N1 118.60(15) . . ? C8 C7 C6 117.42(17) . . ? C8 C7 C12 120.27(17) . . ? C6 C7 C12 122.30(16) . . ? C9 C8 C7 121.62(18) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C10 C9 C8 119.86(17) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 121.43(18) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C10 C11 C6 117.87(16) . . ? C10 C11 C15 119.00(16) . . ? C6 C11 C15 123.13(15) . . ? C14 C12 C7 112.41(18) . . ? C14 C12 C13 111.3(2) . . ? C7 C12 C13 110.55(19) . . ? C14 C12 H12 107.5 . . ? C7 C12 H12 107.5 . . ? C13 C12 H12 107.5 . . ? 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 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C17 111.34(15) . . ? C11 C15 C16 111.77(16) . . ? C17 C15 C16 109.79(16) . . ? C11 C15 H15A 107.9 . . ? C17 C15 H15A 107.9 . . ? C16 C15 H15A 107.9 . . ? 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 . . ? C19 C18 C23 121.4(12) . . ? C19 C18 N2 118.5(13) . . ? C23 C18 N2 119.8(13) . . ? C20 C19 C18 118.0(12) . . ? C20 C19 C24 119.7(14) . . ? C18 C19 C24 122.1(14) . . ? C21 C20 C19 120.9(14) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C22 C21 C20 120.6(14) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C23 120.9(13) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C22 C23 C18 118.2(11) . . ? C22 C23 C27 119.1(12) . . ? C18 C23 C27 122.5(13) . . ? C25 C24 C19 113.6(16) . . ? C25 C24 C26 110.8(16) . . ? C19 C24 C26 111.1(16) . . ? C25 C24 H24 107.0 . . ? C19 C24 H24 107.0 . . ? C26 C24 H24 107.0 . . ? C24 C25 H25A 109.1 . . ? C24 C25 H25B 108.2 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 111.1 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C25 H25D 116.3 . . ? H25A C25 H25D 21.4 . . ? H25B C25 H25D 88.1 . . ? H25C C25 H25D 120.4 . . ? C24 C25 H25E 101.1 . . ? H25A C25 H25E 129.2 . . ? H25B C25 H25E 20.2 . . ? H25C C25 H25E 95.8 . . ? H25D C25 H25E 108.0 . . ? C24 C25 H25F 107.0 . . ? H25A C25 H25F 108.3 . . ? H25B C25 H25F 114.6 . . ? H25C C25 H25F 5.5 . . ? H25D C25 H25F 121.1 . . ? H25E C25 H25F 100.3 . . ? C24 C26 H26A 110.7 . . ? C24 C26 H26B 110.0 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 107.7 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C26 H26D 102.5 . . ? H26A C26 H26D 11.6 . . ? H26B C26 H26D 106.1 . . ? H26C C26 H26D 120.7 . . ? C24 C26 H26E 111.8 . . ? H26A C26 H26E 105.1 . . ? H26B C26 H26E 4.4 . . ? H26C C26 H26E 112.0 . . ? H26D C26 H26E 101.7 . . ? C24 C26 H26F 115.1 . . ? H26A C26 H26F 92.6 . . ? H26B C26 H26F 117.6 . . ? H26C C26 H26F 16.9 . . ? H26D C26 H26F 103.8 . . ? H26E C26 H26F 119.0 . . ? C23 C27 C29 109.8(8) . . ? C23 C27 C28 112.0(8) . . ? C29 C27 C28 110.8(6) . . ? C23 C27 H27 108.0 . . ? C29 C27 H27 108.0 . . ? C28 C27 H27 108.0 . . ? C23 C27 H28F 110.7 . . ? C29 C27 H28F 137.5 . . ? C28 C27 H28F 40.1 . . ? H27 C27 H28F 70.8 . . ? C27 C28 H28A 109.6 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.3 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C28 H28D 101.0 . . ? H28A C28 H28D 19.1 . . ? H28B C28 H28D 97.8 . . ? H28C C28 H28D 128.4 . . ? C27 C28 H28E 76.3 . . ? H28A C28 H28E 115.8 . . ? H28B C28 H28E 34.0 . . ? H28C C28 H28E 129.3 . . ? H28D C28 H28E 97.5 . . ? C27 C28 H28F 69.4 . . ? H28A C28 H28F 164.9 . . ? H28B C28 H28F 84.4 . . ? H28C C28 H28F 58.7 . . ? H28D C28 H28F 170.3 . . ? H28E C28 H28F 79.0 . . ? C27 C29 H29A 109.6 . . ? C27 C29 H29B 109.7 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.1 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C29 H29D 127.4 . . ? H29A C29 H29D 46.8 . . ? H29B C29 H29D 122.2 . . ? H29C C29 H29D 62.8 . . ? C27 C29 H29E 152.6 . . ? H29A C29 H29E 90.8 . . ? H29B C29 H29E 44.2 . . ? H29C C29 H29E 79.4 . . ? H29D C29 H29E 79.9 . . ? C27 C29 H29F 107.9 . . ? H29A C29 H29F 114.7 . . ? H29B C29 H29F 105.3 . . ? H29C C29 H29F 5.5 . . ? H29D C29 H29F 67.9 . . ? H29E C29 H29F 78.0 . . ? C23D C18D C19D 120.6(9) . . ? C23D C18D N2 120.3(10) . . ? C19D C18D N2 118.4(10) . . ? C20D C19D C18D 118.2(9) . . ? C20D C19D C24D 118.9(11) . . ? C18D C19D C24D 122.9(11) . . ? C21D C20D C19D 121.6(11) . . ? C21D C20D H20D 119.2 . . ? C19D C20D H20D 119.2 . . ? C22D C21D C20D 119.3(11) . . ? C22D C21D H21D 120.4 . . ? C20D C21D H21D 120.4 . . ? C21D C22D C23D 121.9(10) . . ? C21D C22D H22D 119.1 . . ? C23D C22D H22D 119.1 . . ? C22D C23D C18D 118.1(9) . . ? C22D C23D C27D 119.7(9) . . ? C18D C23D C27D 122.1(9) . . ? C19D C24D C25D 111.1(13) . . ? C19D C24D C26D 111.8(13) . . ? C25D C24D C26D 110.0(12) . . ? C19D C24D H24D 107.9 . . ? C25D C24D H24D 107.9 . . ? C26D C24D H24D 107.9 . . ? C24D C25D H25A 102.6 . . ? C24D C25D H25B 116.5 . . ? H25A C25D H25B 104.8 . . ? C24D C25D H25C 112.8 . . ? H25A C25D H25C 98.9 . . ? H25B C25D H25C 117.7 . . ? C24D C25D H25D 110.2 . . ? H25A C25D H25D 18.2 . . ? H25B C25D H25D 86.6 . . ? H25C C25D H25D 109.5 . . ? C24D C25D H25E 110.0 . . ? H25A C25D H25E 127.4 . . ? H25B C25D H25E 23.2 . . ? H25C C25D H25E 104.7 . . ? H25D C25D H25E 109.5 . . ? C24D C25D H25F 108.2 . . ? H25A C25D H25F 97.5 . . ? H25B C25D H25F 123.2 . . ? H25C C25D H25F 5.5 . . ? H25D C25D H25F 109.5 . . ? H25E C25D H25F 109.5 . . ? C24D C26D H26A 117.7 . . ? C24D C26D H26B 107.1 . . ? H26A C26D H26B 116.4 . . ? C24D C26D H26C 103.0 . . ? H26A C26D H26C 111.2 . . ? H26B C26D H26C 99.1 . . ? C24D C26D H26D 108.3 . . ? H26A C26D H26D 13.7 . . ? H26B C26D H26D 113.4 . . ? H26C C26D H26D 124.5 . . ? C24D C26D H26E 109.3 . . ? H26A C26D H26E 112.5 . . ? H26B C26D H26E 3.9 . . ? H26C C26D H26E 101.6 . . ? H26D C26D H26E 109.5 . . ? C24D C26D H26F 110.9 . . ? H26A C26D H26F 96.2 . . ? H26B C26D H26F 107.7 . . ? H26C C26D H26F 15.0 . . ? H26D C26D H26F 109.5 . . ? H26E C26D H26F 109.5 . . ? C23D C27D C29D 112.0(6) . . ? C23D C27D C28D 111.2(6) . . ? C29D C27D C28D 110.7(5) . . ? C23D C27D H29A 109.9 . . ? C29D C27D H29A 42.9 . . ? C28D C27D H29A 137.8 . . ? C23D C27D H27D 107.6 . . ? C29D C27D H27D 107.6 . . ? C28D C27D H27D 107.6 . . ? H29A C27D H27D 67.7 . . ? C27D C28D H28A 105.9 . . ? C27D C28D H28B 157.4 . . ? H28A C28D H28B 79.7 . . ? C27D C28D H28C 122.8 . . ? H28A C28D H28C 66.6 . . ? H28B C28D H28C 79.6 . . ? C27D C28D H28D 109.6 . . ? H28A C28D H28D 4.4 . . ? H28B C28D H28D 75.3 . . ? H28C C28D H28D 66.7 . . ? C27D C28D H28E 109.3 . . ? H28A C28D H28E 113.3 . . ? H28B C28D H28E 49.9 . . ? H28C C28D H28E 126.1 . . ? H28D C28D H28E 109.5 . . ? C27D C28D H28F 109.4 . . ? H28A C28D H28F 109.3 . . ? H28B C28D H28F 88.5 . . ? H28C C28D H28F 42.8 . . ? H28D C28D H28F 109.5 . . ? H28E C28D H28F 109.5 . . ? C27D C29D H29A 67.5 . . ? C27D C29D H29B 76.1 . . ? H29A C29D H29B 81.4 . . ? C27D C29D H29C 96.1 . . ? H29A C29D H29C 156.8 . . ? H29B C29D H29C 111.5 . . ? C27D C29D H29D 109.6 . . ? H29A C29D H29D 58.8 . . ? H29B C29D H29D 130.5 . . ? H29C C29D H29D 116.4 . . ? C27D C29D H29E 109.5 . . ? H29A C29D H29E 86.9 . . ? H29B C29D H29E 34.4 . . ? H29C C29D H29E 114.9 . . ? H29D C29D H29E 109.5 . . ? C27D C29D H29F 109.4 . . ? H29A C29D H29F 163.0 . . ? H29B C29D H29F 114.6 . . ? H29C C29D H29F 13.3 . . ? H29D C29D H29F 109.5 . . ? H29E C29D H29F 109.5 . . ? C31 C30 C35 118.47(17) . . ? C31 C30 N3 120.37(16) . . ? C35 C30 N3 121.13(16) . . ? C30 C31 C32 120.16(18) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C33 C32 C31 121.96(19) . . ? C33 C32 H32 119.0 . . ? C31 C32 H32 119.0 . . ? C32 C33 C34 117.42(19) . . ? C32 C33 C36 121.0(2) . . ? C34 C33 C36 121.6(2) . . ? C35 C34 C33 121.52(19) . . ? C35 C34 H34 119.2 . . ? C33 C34 H34 119.2 . . ? C34 C35 C30 120.47(18) . . ? C34 C35 H35 119.8 . . ? C30 C35 H35 119.8 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C42 C37 C38 117.38(18) . . ? C42 C37 N3 118.77(16) . . ? C38 C37 N3 123.84(17) . . ? C39 C38 C37 120.61(19) . . ? C39 C38 H38 119.7 . . ? C37 C38 H38 119.7 . . ? C40 C39 C38 122.2(2) . . ? C40 C39 H39 118.9 . . ? C38 C39 H39 118.9 . . ? C39 C40 C41 116.84(19) . . ? C39 C40 C43 121.1(2) . . ? C41 C40 C43 122.1(2) . . ? C42 C41 C40 121.57(19) . . ? C42 C41 H41 119.2 . . ? C40 C41 H41 119.2 . . ? C41 C42 C37 121.13(19) . . ? C41 C42 H42 119.4 . . ? C37 C42 H42 119.4 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 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 N3 Ti1 N1 C2 168.84(12) . . . . ? N2 Ti1 N1 C2 39.83(12) . . . . ? Cl1 Ti1 N1 C2 -66.90(12) . . . . ? N3 Ti1 N1 C6 -22.26(14) . . . . ? N2 Ti1 N1 C6 -151.27(12) . . . . ? Cl1 Ti1 N1 C6 102.00(12) . . . . ? N3 Ti1 N2 C4 -166.34(11) . . . . ? N1 Ti1 N2 C4 -47.29(12) . . . . ? Cl1 Ti1 N2 C4 62.04(11) . . . . ? N3 Ti1 N2 C18D 27.5(7) . . . . ? N1 Ti1 N2 C18D 146.6(7) . . . . ? Cl1 Ti1 N2 C18D -104.1(7) . . . . ? N3 Ti1 N2 C18 21.4(8) . . . . ? N1 Ti1 N2 C18 140.4(8) . . . . ? Cl1 Ti1 N2 C18 -110.2(8) . . . . ? N2 Ti1 N3 C37 -10.15(17) . . . . ? N1 Ti1 N3 C37 -118.67(14) . . . . ? Cl1 Ti1 N3 C37 119.00(14) . . . . ? N2 Ti1 N3 C30 -173.23(11) . . . . ? N1 Ti1 N3 C30 78.26(13) . . . . ? Cl1 Ti1 N3 C30 -44.08(13) . . . . ? C6 N1 C2 C3 175.68(15) . . . . ? Ti1 N1 C2 C3 -15.3(2) . . . . ? C6 N1 C2 C1 -4.2(2) . . . . ? Ti1 N1 C2 C1 164.85(12) . . . . ? N1 C2 C3 C4 -17.3(3) . . . . ? C1 C2 C3 C4 162.59(17) . . . . ? C18D N2 C4 C3 -159.1(6) . . . . ? C18 N2 C4 C3 -155.3(8) . . . . ? Ti1 N2 C4 C3 32.4(2) . . . . ? C18D N2 C4 C5 21.7(6) . . . . ? C18 N2 C4 C5 25.6(8) . . . . ? Ti1 N2 C4 C5 -146.74(13) . . . . ? C2 C3 C4 N2 7.2(3) . . . . ? C2 C3 C4 C5 -173.66(17) . . . . ? C2 N1 C6 C11 83.0(2) . . . . ? Ti1 N1 C6 C11 -85.67(17) . . . . ? C2 N1 C6 C7 -100.04(18) . . . . ? Ti1 N1 C6 C7 91.26(16) . . . . ? C11 C6 C7 C8 -0.8(3) . . . . ? N1 C6 C7 C8 -177.67(16) . . . . ? C11 C6 C7 C12 -179.36(17) . . . . ? N1 C6 C7 C12 3.8(2) . . . . ? C6 C7 C8 C9 0.7(3) . . . . ? C12 C7 C8 C9 179.28(19) . . . . ? C7 C8 C9 C10 0.0(3) . . . . ? C8 C9 C10 C11 -0.6(3) . . . . ? C9 C10 C11 C6 0.5(3) . . . . ? C9 C10 C11 C15 -179.87(18) . . . . ? C7 C6 C11 C10 0.2(3) . . . . ? N1 C6 C11 C10 177.07(15) . . . . ? C7 C6 C11 C15 -179.41(16) . . . . ? N1 C6 C11 C15 -2.6(2) . . . . ? C8 C7 C12 C14 46.4(3) . . . . ? C6 C7 C12 C14 -135.1(2) . . . . ? C8 C7 C12 C13 -78.6(3) . . . . ? C6 C7 C12 C13 99.9(2) . . . . ? C10 C11 C15 C17 -67.9(2) . . . . ? C6 C11 C15 C17 111.74(19) . . . . ? C10 C11 C15 C16 55.3(2) . . . . ? C6 C11 C15 C16 -125.08(19) . . . . ? C4 N2 C18 C19 65.2(13) . . . . ? C18D N2 C18 C19 88(7) . . . . ? Ti1 N2 C18 C19 -123.1(11) . . . . ? C4 N2 C18 C23 -108.6(14) . . . . ? C18D N2 C18 C23 -85(7) . . . . ? Ti1 N2 C18 C23 63.2(17) . . . . ? C23 C18 C19 C20 2.0(12) . . . . ? N2 C18 C19 C20 -171.7(17) . . . . ? C23 C18 C19 C24 -172.9(18) . . . . ? N2 C18 C19 C24 13(2) . . . . ? C18 C19 C20 C21 -3.5(19) . . . . ? C24 C19 C20 C21 172(2) . . . . ? C19 C20 C21 C22 3(3) . . . . ? C20 C21 C22 C23 0(4) . . . . ? C21 C22 C23 C18 -1(3) . . . . ? C21 C22 C23 C27 -176(2) . . . . ? C19 C18 C23 C22 0(2) . . . . ? N2 C18 C23 C22 174.0(16) . . . . ? C19 C18 C23 C27 174.9(13) . . . . ? N2 C18 C23 C27 -12(2) . . . . ? C20 C19 C24 C25 76(3) . . . . ? C18 C19 C24 C25 -109(3) . . . . ? C20 C19 C24 C26 -50(3) . . . . ? C18 C19 C24 C26 125(3) . . . . ? C22 C23 C27 C29 -80.5(16) . . . . ? C18 C23 C27 C29 105.1(15) . . . . ? C22 C23 C27 C28 43.1(18) . . . . ? C18 C23 C27 C28 -131.3(14) . . . . ? C4 N2 C18D C23D -109.4(10) . . . . ? C18 N2 C18D C23D 92(7) . . . . ? Ti1 N2 C18D C23D 56.8(13) . . . . ? C4 N2 C18D C19D 80.3(9) . . . . ? C18 N2 C18D C19D -78(7) . . . . ? Ti1 N2 C18D C19D -113.4(9) . . . . ? C23D C18D C19D C20D 5.5(9) . . . . ? N2 C18D C19D C20D 175.7(13) . . . . ? C23D C18D C19D C24D -172.5(14) . . . . ? N2 C18D C19D C24D -2.3(16) . . . . ? C18D C19D C20D C21D -0.9(15) . . . . ? C24D C19D C20D C21D 177.2(19) . . . . ? C19D C20D C21D C22D -4(3) . . . . ? C20D C21D C22D C23D 5(3) . . . . ? C21D C22D C23D C18D -1(2) . . . . ? C21D C22D C23D C27D 175.2(16) . . . . ? C19D C18D C23D C22D -4.7(15) . . . . ? N2 C18D C23D C22D -174.7(12) . . . . ? C19D C18D C23D C27D 179.5(10) . . . . ? N2 C18D C23D C27D 9.4(16) . . . . ? C20D C19D C24D C25D 74(2) . . . . ? C18D C19D C24D C25D -108(2) . . . . ? C20D C19D C24D C26D -49(2) . . . . ? C18D C19D C24D C26D 129(2) . . . . ? C22D C23D C27D C29D -55.2(12) . . . . ? C18D C23D C27D C29D 120.6(10) . . . . ? C22D C23D C27D C28D 69.3(12) . . . . ? C18D C23D C27D C28D -114.9(11) . . . . ? C37 N3 C30 C31 97.5(2) . . . . ? Ti1 N3 C30 C31 -97.72(17) . . . . ? C37 N3 C30 C35 -84.6(2) . . . . ? Ti1 N3 C30 C35 80.26(18) . . . . ? C35 C30 C31 C32 1.0(3) . . . . ? N3 C30 C31 C32 179.03(17) . . . . ? C30 C31 C32 C33 -0.7(3) . . . . ? C31 C32 C33 C34 0.1(3) . . . . ? C31 C32 C33 C36 -179.3(2) . . . . ? C32 C33 C34 C35 0.2(3) . . . . ? C36 C33 C34 C35 179.6(2) . . . . ? C33 C34 C35 C30 0.2(3) . . . . ? C31 C30 C35 C34 -0.7(3) . . . . ? N3 C30 C35 C34 -178.76(17) . . . . ? C30 N3 C37 C42 -164.99(17) . . . . ? Ti1 N3 C37 C42 32.2(2) . . . . ? C30 N3 C37 C38 16.4(3) . . . . ? Ti1 N3 C37 C38 -146.41(17) . . . . ? C42 C37 C38 C39 -5.2(3) . . . . ? N3 C37 C38 C39 173.4(2) . . . . ? C37 C38 C39 C40 0.6(4) . . . . ? C38 C39 C40 C41 3.1(4) . . . . ? C38 C39 C40 C43 -177.4(2) . . . . ? C39 C40 C41 C42 -2.1(3) . . . . ? C43 C40 C41 C42 178.5(2) . . . . ? C40 C41 C42 C37 -2.7(3) . . . . ? C38 C37 C42 C41 6.3(3) . . . . ? N3 C37 C42 C41 -172.41(18) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.60 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.362 _refine_diff_density_min -0.329 _refine_diff_density_rms 0.046 # Attachment '09531.cif' data_p21c _database_code_depnum_ccdc_archive 'CCDC 829541' #TrackingRef '09531.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C43 H56 N4 Ti' _chemical_formula_sum 'C43 H56 N4 Ti' _chemical_melting_point ? _exptl_crystal_description needle _exptl_crystal_colour yellow _diffrn_ambient_temperature 120(2) _chemical_formula_weight 676.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2060 0.2830 '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' _symmetry_int_tables_number 14 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 11.7466(9) _cell_length_b 28.974(2) _cell_length_c 12.3682(9) _cell_angle_alpha 90.00 _cell_angle_beta 115.276(2) _cell_angle_gamma 90.00 _cell_volume 3806.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1845 _cell_measurement_theta_min 0.82 _cell_measurement_theta_max 18.54 _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.181 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 0.142 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9860 _exptl_absorpt_correction_T_max 0.9958 _exptl_absorpt_process_details 'SADABS, R. Blessing; 1995' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.41328 _diffrn_source synchrotron _diffrn_source_type 'APS beamline 15-ID' _diffrn_radiation_monochromator 'diamond 111' _diffrn_measurement_device_type ? _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean 83.33 _diffrn_reflns_number 85507 _diffrn_reflns_av_R_equivalents 0.0790 _diffrn_reflns_av_sigmaI/netI 0.0737 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 0.82 _diffrn_reflns_theta_max 18.54 _reflns_number_total 14417 _reflns_number_gt 9323 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II v.2.2 (Bruker, 2009)' _computing_cell_refinement 'APEX II v.2.2 (Bruker, 2009)' _computing_data_reduction 'APEX II v.2.2 (Bruker, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Bruker, 2008)' _computing_publication_material 'SHELXTL (Bruker, 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. ; _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^)+(0.0774P)^2^+0.7444P] 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 14417 _refine_ls_number_parameters 445 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1017 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1568 _refine_ls_wR_factor_gt 0.1320 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 0.27280(3) 0.651832(9) 0.22578(2) 0.01323(7) Uani 1 1 d . . . N1 N 0.19561(12) 0.69933(4) 0.09361(11) 0.0143(2) Uani 1 1 d . . . N2 N 0.13034(12) 0.60636(4) 0.14973(11) 0.0147(2) Uani 1 1 d . . . N3 N 0.44371(13) 0.62707(5) 0.25444(12) 0.0163(3) Uani 1 1 d . . . N4 N 0.26926(14) 0.67239(5) 0.35206(12) 0.0197(3) Uani 1 1 d . . . H4 H 0.2674 0.6831 0.4179 0.024 Uiso 1 1 calc R . . C1 C 0.18413(17) 0.70540(6) -0.11023(15) 0.0207(3) Uani 1 1 d . . . H1A H 0.1257 0.7315 -0.1309 0.031 Uiso 1 1 calc R . . H1B H 0.1617 0.6854 -0.1802 0.031 Uiso 1 1 calc R . . H1C H 0.2702 0.7169 -0.0850 0.031 Uiso 1 1 calc R . . C2 C 0.17621(14) 0.67838(5) -0.00972(13) 0.0136(3) Uani 1 1 d . . . C3 C 0.15279(14) 0.63048(5) -0.02731(13) 0.0139(3) Uani 1 1 d . . . H3 H 0.1601 0.6183 -0.0953 0.017 Uiso 1 1 calc R . . C4 C 0.12039(14) 0.59781(5) 0.03912(13) 0.0142(3) Uani 1 1 d . . . C5 C 0.07621(17) 0.55145(5) -0.01726(15) 0.0202(3) Uani 1 1 d . . . H5A H 0.1189 0.5272 0.0412 0.030 Uiso 1 1 calc R . . H5B H 0.0958 0.5480 -0.0863 0.030 Uiso 1 1 calc R . . H5C H -0.0149 0.5489 -0.0435 0.030 Uiso 1 1 calc R . . C6 C 0.06615(16) 0.57699(5) 0.19939(15) 0.0178(3) Uani 1 1 d . . . C7 C 0.13523(17) 0.54787(6) 0.29629(15) 0.0205(3) Uani 1 1 d . . . C8 C 0.0693(2) 0.52000(6) 0.34206(18) 0.0289(4) Uani 1 1 d . . . H8 H 0.1149 0.4998 0.4067 0.035 Uiso 1 1 calc R . . C9 C -0.0598(2) 0.52101(7) 0.2960(2) 0.0315(4) Uani 1 1 d . . . H9 H -0.1028 0.5016 0.3284 0.038 Uiso 1 1 calc R . . C10 C -0.12690(19) 0.55045(6) 0.20226(19) 0.0279(4) Uani 1 1 d . . . H10 H -0.2161 0.5511 0.1709 0.033 Uiso 1 1 calc R . . C11 C -0.06621(17) 0.57924(6) 0.15269(16) 0.0219(3) Uani 1 1 d . . . C12 C 0.27746(17) 0.54490(6) 0.35205(15) 0.0223(3) Uani 1 1 d . . . H12 H 0.3086 0.5677 0.3102 0.027 Uiso 1 1 calc R . . C13 C 0.3234(2) 0.49705(6) 0.33586(19) 0.0314(4) Uani 1 1 d . . . H13A H 0.3010 0.4743 0.3822 0.047 Uiso 1 1 calc R . . H13B H 0.4151 0.4976 0.3640 0.047 Uiso 1 1 calc R . . H13C H 0.2836 0.4886 0.2511 0.047 Uiso 1 1 calc R . . C14 C 0.3338(2) 0.55804(7) 0.48439(17) 0.0333(4) Uani 1 1 d . . . H14A H 0.3025 0.5885 0.4933 0.050 Uiso 1 1 calc R . . H14B H 0.4258 0.5590 0.5160 0.050 Uiso 1 1 calc R . . H14C H 0.3092 0.5351 0.5287 0.050 Uiso 1 1 calc R . . C15 C -0.14437(17) 0.61345(7) 0.05709(18) 0.0280(4) Uani 1 1 d . . . H15 H -0.0871 0.6298 0.0289 0.034 Uiso 1 1 calc R . . C16 C -0.2000(2) 0.64915(7) 0.1112(2) 0.0398(5) Uani 1 1 d . . . H16A H -0.2536 0.6337 0.1427 0.060 Uiso 1 1 calc R . . H16B H -0.2503 0.6713 0.0495 0.060 Uiso 1 1 calc R . . H16C H -0.1317 0.6654 0.1761 0.060 Uiso 1 1 calc R . . C17 C -0.2490(2) 0.59031(9) -0.0515(2) 0.0433(6) Uani 1 1 d . . . H17A H -0.2123 0.5666 -0.0836 0.065 Uiso 1 1 calc R . . H17B H -0.2917 0.6136 -0.1132 0.065 Uiso 1 1 calc R . . H17C H -0.3100 0.5760 -0.0272 0.065 Uiso 1 1 calc R . . C18 C 0.19183(15) 0.74888(5) 0.09712(13) 0.0158(3) Uani 1 1 d . . . C19 C 0.30421(16) 0.77424(5) 0.14373(14) 0.0180(3) Uani 1 1 d . . . C20 C 0.29589(18) 0.82240(6) 0.14226(16) 0.0234(3) Uani 1 1 d . . . H20 H 0.3709 0.8402 0.1744 0.028 Uiso 1 1 calc R . . C21 C 0.1809(2) 0.84459(6) 0.09508(17) 0.0259(4) Uani 1 1 d . . . H21 H 0.1773 0.8773 0.0917 0.031 Uiso 1 1 calc R . . C22 C 0.07143(19) 0.81910(6) 0.05286(16) 0.0248(4) Uani 1 1 d . . . H22 H -0.0073 0.8347 0.0216 0.030 Uiso 1 1 calc R . . C23 C 0.07345(17) 0.77095(6) 0.05491(15) 0.0203(3) Uani 1 1 d . . . C24 C 0.43237(16) 0.75128(6) 0.19738(15) 0.0205(3) Uani 1 1 d . . . H24 H 0.4188 0.7176 0.1780 0.025 Uiso 1 1 calc R . . C25 C 0.4941(2) 0.75557(8) 0.33261(18) 0.0354(5) Uani 1 1 d . . . H25A H 0.5150 0.7880 0.3549 0.053 Uiso 1 1 calc R . . H25B H 0.5711 0.7370 0.3654 0.053 Uiso 1 1 calc R . . H25C H 0.4359 0.7445 0.3648 0.053 Uiso 1 1 calc R . . C26 C 0.5201(2) 0.76913(9) 0.1451(2) 0.0378(5) Uani 1 1 d . . . H26A H 0.4776 0.7674 0.0576 0.057 Uiso 1 1 calc R . . H26B H 0.5965 0.7502 0.1743 0.057 Uiso 1 1 calc R . . H26C H 0.5426 0.8013 0.1696 0.057 Uiso 1 1 calc R . . C27 C -0.04850(17) 0.74392(6) 0.01916(18) 0.0289(4) Uani 1 1 d . . . H27 H -0.0250 0.7137 0.0624 0.035 Uiso 1 1 calc R . . C28 C -0.1383(2) 0.76736(8) 0.0607(2) 0.0422(5) Uani 1 1 d . . . H28A H -0.1709 0.7957 0.0144 0.063 Uiso 1 1 calc R . . H28B H -0.0935 0.7750 0.1457 0.063 Uiso 1 1 calc R . . H28C H -0.2084 0.7465 0.0486 0.063 Uiso 1 1 calc R . . C29 C -0.1149(2) 0.73266(12) -0.1115(2) 0.0561(8) Uani 1 1 d . . . H29A H -0.1369 0.7613 -0.1580 0.084 Uiso 1 1 calc R . . H29B H -0.1917 0.7152 -0.1269 0.084 Uiso 1 1 calc R . . H29C H -0.0594 0.7141 -0.1350 0.084 Uiso 1 1 calc R . . C30 C 0.55778(15) 0.62124(5) 0.35708(14) 0.0168(3) Uani 1 1 d . . . C31 C 0.56793(17) 0.63618(6) 0.46840(15) 0.0221(3) Uani 1 1 d . . . H31 H 0.4974 0.6501 0.4739 0.026 Uiso 1 1 calc R . . C32 C 0.67904(17) 0.63096(6) 0.57068(15) 0.0246(4) Uani 1 1 d . . . H32 H 0.6828 0.6413 0.6450 0.030 Uiso 1 1 calc R . . C33 C 0.78549(16) 0.61098(6) 0.56762(15) 0.0220(3) Uani 1 1 d . . . C34 C 0.77590(17) 0.59625(6) 0.45806(16) 0.0234(3) Uani 1 1 d . . . H34 H 0.8470 0.5825 0.4532 0.028 Uiso 1 1 calc R . . C35 C 0.66442(16) 0.60103(6) 0.35400(15) 0.0209(3) Uani 1 1 d . . . H35 H 0.6610 0.5904 0.2800 0.025 Uiso 1 1 calc R . . C36 C 0.90483(18) 0.60603(7) 0.68123(17) 0.0307(4) Uani 1 1 d . . . H36A H 0.9728 0.5949 0.6619 0.046 Uiso 1 1 calc R . . H36B H 0.8911 0.5839 0.7344 0.046 Uiso 1 1 calc R . . H36C H 0.9281 0.6361 0.7211 0.046 Uiso 1 1 calc R . . C37 C 0.40979(16) 0.56131(6) 0.11850(15) 0.0196(3) Uani 1 1 d . . . H37 H 0.3983 0.5418 0.1748 0.023 Uiso 1 1 calc R . . C38 C 0.39543(17) 0.54324(6) 0.00952(15) 0.0215(3) Uani 1 1 d . . . H38 H 0.3733 0.5117 -0.0078 0.026 Uiso 1 1 calc R . . C39 C 0.41277(16) 0.57040(6) -0.07458(14) 0.0198(3) Uani 1 1 d . . . C40 C 0.44775(16) 0.61620(6) -0.04476(15) 0.0211(3) Uani 1 1 d . . . H40 H 0.4618 0.6354 -0.1002 0.025 Uiso 1 1 calc R . . C41 C 0.46256(16) 0.63449(6) 0.06441(15) 0.0187(3) Uani 1 1 d . . . H41 H 0.4878 0.6657 0.0830 0.022 Uiso 1 1 calc R . . C42 C 0.44086(14) 0.60759(5) 0.14657(14) 0.0159(3) Uani 1 1 d . . . C43 C 0.3940(2) 0.55135(7) -0.19455(16) 0.0291(4) Uani 1 1 d . . . H43A H 0.3904 0.5176 -0.1928 0.044 Uiso 1 1 calc R . . H43B H 0.4643 0.5609 -0.2123 0.044 Uiso 1 1 calc R . . H43C H 0.3149 0.5632 -0.2566 0.044 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 0.01339(13) 0.01367(12) 0.01077(12) -0.00033(10) 0.00338(9) 0.00105(10) N1 0.0152(6) 0.0129(5) 0.0123(5) -0.0002(4) 0.0033(5) 0.0000(5) N2 0.0147(6) 0.0144(6) 0.0146(6) 0.0009(5) 0.0060(5) 0.0003(5) N3 0.0144(6) 0.0191(6) 0.0124(6) -0.0008(5) 0.0030(5) 0.0022(5) N4 0.0235(7) 0.0205(7) 0.0132(6) -0.0010(5) 0.0059(5) 0.0036(5) C1 0.0270(9) 0.0205(7) 0.0165(7) 0.0024(6) 0.0110(7) -0.0011(6) C2 0.0116(6) 0.0152(6) 0.0123(6) 0.0009(5) 0.0034(5) 0.0009(5) C3 0.0127(7) 0.0155(6) 0.0120(6) -0.0018(5) 0.0038(5) 0.0011(5) C4 0.0115(6) 0.0139(6) 0.0155(7) -0.0009(5) 0.0042(5) 0.0010(5) C5 0.0236(8) 0.0147(7) 0.0205(8) -0.0029(6) 0.0076(6) -0.0023(6) C6 0.0212(8) 0.0154(7) 0.0203(7) -0.0010(6) 0.0124(6) -0.0023(6) C7 0.0278(9) 0.0151(7) 0.0223(8) -0.0001(6) 0.0143(7) 0.0003(6) C8 0.0408(11) 0.0218(8) 0.0307(10) 0.0058(7) 0.0216(9) -0.0009(8) C9 0.0418(12) 0.0232(8) 0.0423(11) 0.0011(8) 0.0301(10) -0.0062(8) C10 0.0269(9) 0.0251(9) 0.0399(11) -0.0037(8) 0.0223(9) -0.0050(7) C11 0.0205(8) 0.0202(7) 0.0287(9) -0.0019(7) 0.0141(7) -0.0020(6) C12 0.0285(9) 0.0178(7) 0.0207(8) 0.0058(6) 0.0107(7) 0.0036(6) C13 0.0379(11) 0.0206(8) 0.0392(11) 0.0056(8) 0.0199(9) 0.0067(8) C14 0.0385(11) 0.0339(10) 0.0220(9) 0.0028(8) 0.0077(8) 0.0023(9) C15 0.0190(8) 0.0304(9) 0.0372(10) 0.0066(8) 0.0143(8) 0.0012(7) C16 0.0338(11) 0.0263(10) 0.0629(15) 0.0040(10) 0.0241(11) 0.0050(8) C17 0.0234(10) 0.0563(15) 0.0426(13) -0.0028(11) 0.0067(9) 0.0044(10) C18 0.0210(8) 0.0137(6) 0.0118(6) 0.0000(5) 0.0061(6) -0.0004(6) C19 0.0244(8) 0.0158(7) 0.0153(7) -0.0021(5) 0.0097(6) -0.0026(6) C20 0.0329(10) 0.0165(7) 0.0244(8) -0.0041(6) 0.0156(8) -0.0072(7) C21 0.0402(11) 0.0134(7) 0.0278(9) 0.0009(6) 0.0179(8) -0.0003(7) C22 0.0321(10) 0.0169(7) 0.0230(8) 0.0023(6) 0.0095(7) 0.0066(7) C23 0.0226(8) 0.0164(7) 0.0169(7) -0.0005(6) 0.0038(6) 0.0029(6) C24 0.0195(8) 0.0191(7) 0.0225(8) -0.0043(6) 0.0087(6) -0.0054(6) C25 0.0345(11) 0.0463(12) 0.0223(9) 0.0075(8) 0.0090(8) 0.0108(9) C26 0.0237(10) 0.0610(15) 0.0311(10) 0.0076(10) 0.0141(8) -0.0038(9) C27 0.0195(9) 0.0212(8) 0.0355(10) -0.0048(7) 0.0015(8) 0.0039(7) C28 0.0419(13) 0.0399(12) 0.0518(14) -0.0128(10) 0.0267(11) -0.0127(10) C29 0.0301(12) 0.087(2) 0.0439(14) -0.0239(14) 0.0091(11) -0.0098(13) C30 0.0146(7) 0.0160(6) 0.0156(7) 0.0014(5) 0.0026(6) 0.0001(5) C31 0.0202(8) 0.0249(8) 0.0160(7) 0.0002(6) 0.0029(6) 0.0044(6) C32 0.0242(9) 0.0266(9) 0.0160(7) -0.0011(6) 0.0017(6) 0.0025(7) C33 0.0191(8) 0.0182(7) 0.0200(8) 0.0045(6) 0.0000(6) 0.0003(6) C34 0.0164(8) 0.0239(8) 0.0253(8) 0.0033(7) 0.0045(7) 0.0027(6) C35 0.0173(8) 0.0245(8) 0.0182(7) 0.0008(6) 0.0051(6) 0.0018(6) C36 0.0220(9) 0.0315(10) 0.0248(9) 0.0038(7) -0.0032(7) 0.0010(7) C37 0.0226(8) 0.0181(7) 0.0190(7) 0.0017(6) 0.0099(6) 0.0029(6) C38 0.0223(8) 0.0194(7) 0.0226(8) -0.0038(6) 0.0096(7) 0.0009(6) C39 0.0179(8) 0.0238(8) 0.0160(7) -0.0014(6) 0.0057(6) 0.0048(6) C40 0.0228(8) 0.0231(8) 0.0196(8) 0.0027(6) 0.0112(7) 0.0031(6) C41 0.0177(7) 0.0188(7) 0.0197(7) -0.0007(6) 0.0081(6) 0.0001(6) C42 0.0118(7) 0.0199(7) 0.0139(7) 0.0006(6) 0.0034(5) 0.0032(5) C43 0.0352(10) 0.0326(10) 0.0193(8) -0.0035(7) 0.0115(8) 0.0046(8) _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 N4 1.6885(14) . ? Ti1 N3 2.0157(14) . ? Ti1 N2 2.0191(13) . ? Ti1 N1 2.0305(13) . ? N1 C2 1.3436(19) . ? N1 C18 1.4376(19) . ? N2 C4 1.345(2) . ? N2 C6 1.437(2) . ? N3 C30 1.408(2) . ? N3 C42 1.436(2) . ? N4 H4 0.8800 . ? C1 C2 1.505(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.414(2) . ? C3 C4 1.408(2) . ? C3 H3 0.9500 . ? C4 C5 1.500(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.406(2) . ? C6 C11 1.410(2) . ? C7 C8 1.395(2) . ? C7 C12 1.513(3) . ? C8 C9 1.375(3) . ? C8 H8 0.9500 . ? C9 C10 1.383(3) . ? C9 H9 0.9500 . ? C10 C11 1.397(2) . ? C10 H10 0.9500 . ? C11 C15 1.515(3) . ? C12 C14 1.529(3) . ? C12 C13 1.532(2) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.522(3) . ? C15 C17 1.535(3) . ? C15 H15 1.0000 . ? 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 C19 1.402(2) . ? C18 C23 1.413(2) . ? C19 C20 1.398(2) . ? C19 C24 1.515(2) . ? C20 C21 1.380(3) . ? C20 H20 0.9500 . ? C21 C22 1.378(3) . ? C21 H21 0.9500 . ? C22 C23 1.395(2) . ? C22 H22 0.9500 . ? C23 C27 1.523(3) . ? C24 C25 1.518(3) . ? C24 C26 1.522(3) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.500(3) . ? C27 C28 1.516(3) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C35 1.398(2) . ? C30 C31 1.399(2) . ? C31 C32 1.384(2) . ? C31 H31 0.9500 . ? C32 C33 1.393(3) . ? C32 H32 0.9500 . ? C33 C34 1.379(3) . ? C33 C36 1.509(2) . ? C34 C35 1.397(2) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.387(2) . ? C37 C42 1.394(2) . ? C37 H37 0.9500 . ? C38 C39 1.387(2) . ? C38 H38 0.9500 . ? C39 C40 1.392(2) . ? C39 C43 1.508(2) . ? C40 C41 1.391(2) . ? C40 H40 0.9500 . ? C41 C42 1.388(2) . ? C41 H41 0.9500 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 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 N4 Ti1 N3 112.27(6) . . ? N4 Ti1 N2 108.56(6) . . ? N3 Ti1 N2 114.51(5) . . ? N4 Ti1 N1 109.06(6) . . ? N3 Ti1 N1 116.85(6) . . ? N2 Ti1 N1 94.06(5) . . ? C2 N1 C18 119.03(12) . . ? C2 N1 Ti1 107.19(10) . . ? C18 N1 Ti1 131.42(10) . . ? C4 N2 C6 119.46(13) . . ? C4 N2 Ti1 106.79(10) . . ? C6 N2 Ti1 131.99(10) . . ? C30 N3 C42 115.23(13) . . ? C30 N3 Ti1 133.96(11) . . ? C42 N3 Ti1 110.50(10) . . ? Ti1 N4 H4 180.0 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 122.20(14) . . ? N1 C2 C1 120.34(13) . . ? C3 C2 C1 117.41(13) . . ? C4 C3 C2 130.81(14) . . ? C4 C3 H3 114.6 . . ? C2 C3 H3 114.6 . . ? N2 C4 C3 122.80(14) . . ? N2 C4 C5 120.01(14) . . ? C3 C4 C5 117.17(14) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 120.74(15) . . ? C7 C6 N2 120.17(15) . . ? C11 C6 N2 119.04(15) . . ? C8 C7 C6 118.36(17) . . ? C8 C7 C12 118.55(16) . . ? C6 C7 C12 123.08(15) . . ? C9 C8 C7 121.69(18) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C8 C9 C10 119.54(17) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C9 C10 C11 121.43(18) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C10 C11 C6 118.20(17) . . ? C10 C11 C15 118.69(16) . . ? C6 C11 C15 122.99(15) . . ? C7 C12 C14 111.27(16) . . ? C7 C12 C13 111.98(15) . . ? C14 C12 C13 110.47(16) . . ? C7 C12 H12 107.6 . . ? C14 C12 H12 107.6 . . ? C13 C12 H12 107.6 . . ? 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 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 109.41(17) . . ? C11 C15 C17 112.90(17) . . ? C16 C15 C17 110.37(18) . . ? C11 C15 H15 108.0 . . ? C16 C15 H15 108.0 . . ? C17 C15 H15 108.0 . . ? 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 . . ? C19 C18 C23 121.36(14) . . ? C19 C18 N1 120.00(14) . . ? C23 C18 N1 118.63(14) . . ? C20 C19 C18 117.99(16) . . ? C20 C19 C24 119.65(15) . . ? C18 C19 C24 122.35(14) . . ? C21 C20 C19 121.38(17) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C22 C21 C20 119.79(16) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C23 121.55(17) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C22 C23 C18 117.76(16) . . ? C22 C23 C27 120.16(16) . . ? C18 C23 C27 121.99(14) . . ? C19 C24 C25 111.37(15) . . ? C19 C24 C26 113.01(15) . . ? C25 C24 C26 110.43(17) . . ? C19 C24 H24 107.2 . . ? C25 C24 H24 107.2 . . ? C26 C24 H24 107.2 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C28 110.21(19) . . ? C29 C27 C23 114.60(19) . . ? C28 C27 C23 112.03(16) . . ? C29 C27 H27 106.5 . . ? C28 C27 H27 106.5 . . ? C23 C27 H27 106.5 . . ? 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 . . ? C35 C30 C31 117.10(15) . . ? C35 C30 N3 122.99(15) . . ? C31 C30 N3 119.91(15) . . ? C32 C31 C30 121.09(17) . . ? C32 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C31 C32 C33 121.83(17) . . ? C31 C32 H32 119.1 . . ? C33 C32 H32 119.1 . . ? C34 C33 C32 117.25(15) . . ? C34 C33 C36 122.64(17) . . ? C32 C33 C36 120.12(17) . . ? C33 C34 C35 121.73(17) . . ? C33 C34 H34 119.1 . . ? C35 C34 H34 119.1 . . ? C34 C35 C30 120.99(16) . . ? C34 C35 H35 119.5 . . ? C30 C35 H35 119.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C42 121.01(16) . . ? C38 C37 H37 119.5 . . ? C42 C37 H37 119.5 . . ? C39 C38 C37 121.24(16) . . ? C39 C38 H38 119.4 . . ? C37 C38 H38 119.4 . . ? C38 C39 C40 117.62(15) . . ? C38 C39 C43 121.57(16) . . ? C40 C39 C43 120.81(16) . . ? C41 C40 C39 121.41(16) . . ? C41 C40 H40 119.3 . . ? C39 C40 H40 119.3 . . ? C42 C41 C40 120.73(16) . . ? C42 C41 H41 119.6 . . ? C40 C41 H41 119.6 . . ? C41 C42 C37 117.91(15) . . ? C41 C42 N3 121.40(14) . . ? C37 C42 N3 120.62(14) . . ? C39 C43 H43A 109.5 . . ? C39 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C39 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 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 N4 Ti1 N1 C2 -167.50(10) . . . . ? N3 Ti1 N1 C2 63.88(11) . . . . ? N2 Ti1 N1 C2 -56.26(11) . . . . ? N4 Ti1 N1 C18 30.67(16) . . . . ? N3 Ti1 N1 C18 -97.96(14) . . . . ? N2 Ti1 N1 C18 141.91(14) . . . . ? N4 Ti1 N2 C4 168.01(10) . . . . ? N3 Ti1 N2 C4 -65.66(11) . . . . ? N1 Ti1 N2 C4 56.34(10) . . . . ? N4 Ti1 N2 C6 -27.69(15) . . . . ? N3 Ti1 N2 C6 98.63(14) . . . . ? N1 Ti1 N2 C6 -139.36(14) . . . . ? N4 Ti1 N3 C30 3.71(17) . . . . ? N2 Ti1 N3 C30 -120.67(14) . . . . ? N1 Ti1 N3 C30 130.79(14) . . . . ? N4 Ti1 N3 C42 176.74(10) . . . . ? N2 Ti1 N3 C42 52.36(12) . . . . ? N1 Ti1 N3 C42 -56.19(12) . . . . ? C18 N1 C2 C3 -166.73(14) . . . . ? Ti1 N1 C2 C3 28.78(17) . . . . ? C18 N1 C2 C1 15.8(2) . . . . ? Ti1 N1 C2 C1 -148.68(12) . . . . ? N1 C2 C3 C4 14.1(3) . . . . ? C1 C2 C3 C4 -168.35(16) . . . . ? C6 N2 C4 C3 163.79(14) . . . . ? Ti1 N2 C4 C3 -29.57(17) . . . . ? C6 N2 C4 C5 -17.8(2) . . . . ? Ti1 N2 C4 C5 148.88(12) . . . . ? C2 C3 C4 N2 -13.7(3) . . . . ? C2 C3 C4 C5 167.78(15) . . . . ? C4 N2 C6 C7 111.60(17) . . . . ? Ti1 N2 C6 C7 -51.1(2) . . . . ? C4 N2 C6 C11 -70.93(19) . . . . ? Ti1 N2 C6 C11 126.39(15) . . . . ? C11 C6 C7 C8 2.4(2) . . . . ? N2 C6 C7 C8 179.83(15) . . . . ? C11 C6 C7 C12 -178.46(16) . . . . ? N2 C6 C7 C12 -1.0(2) . . . . ? C6 C7 C8 C9 -1.0(3) . . . . ? C12 C7 C8 C9 179.80(18) . . . . ? C7 C8 C9 C10 -0.3(3) . . . . ? C8 C9 C10 C11 0.2(3) . . . . ? C9 C10 C11 C6 1.1(3) . . . . ? C9 C10 C11 C15 -175.01(18) . . . . ? C7 C6 C11 C10 -2.5(2) . . . . ? N2 C6 C11 C10 -179.91(15) . . . . ? C7 C6 C11 C15 173.53(17) . . . . ? N2 C6 C11 C15 -3.9(2) . . . . ? C8 C7 C12 C14 -60.6(2) . . . . ? C6 C7 C12 C14 120.29(18) . . . . ? C8 C7 C12 C13 63.6(2) . . . . ? C6 C7 C12 C13 -115.53(18) . . . . ? C10 C11 C15 C16 65.6(2) . . . . ? C6 C11 C15 C16 -110.4(2) . . . . ? C10 C11 C15 C17 -57.7(2) . . . . ? C6 C11 C15 C17 126.31(19) . . . . ? C2 N1 C18 C19 -100.11(17) . . . . ? Ti1 N1 C18 C19 60.0(2) . . . . ? C2 N1 C18 C23 81.01(19) . . . . ? Ti1 N1 C18 C23 -118.90(15) . . . . ? C23 C18 C19 C20 -2.9(2) . . . . ? N1 C18 C19 C20 178.25(14) . . . . ? C23 C18 C19 C24 175.68(15) . . . . ? N1 C18 C19 C24 -3.2(2) . . . . ? C18 C19 C20 C21 -0.8(2) . . . . ? C24 C19 C20 C21 -179.47(16) . . . . ? C19 C20 C21 C22 2.8(3) . . . . ? C20 C21 C22 C23 -0.9(3) . . . . ? C21 C22 C23 C18 -2.7(3) . . . . ? C21 C22 C23 C27 173.91(17) . . . . ? C19 C18 C23 C22 4.6(2) . . . . ? N1 C18 C23 C22 -176.52(14) . . . . ? C19 C18 C23 C27 -171.90(16) . . . . ? N1 C18 C23 C27 7.0(2) . . . . ? C20 C19 C24 C25 72.0(2) . . . . ? C18 C19 C24 C25 -106.54(19) . . . . ? C20 C19 C24 C26 -53.0(2) . . . . ? C18 C19 C24 C26 128.46(18) . . . . ? C22 C23 C27 C29 89.4(2) . . . . ? C18 C23 C27 C29 -94.2(2) . . . . ? C22 C23 C27 C28 -37.1(3) . . . . ? C18 C23 C27 C28 139.31(19) . . . . ? C42 N3 C30 C35 4.5(2) . . . . ? Ti1 N3 C30 C35 177.31(13) . . . . ? C42 N3 C30 C31 -175.76(15) . . . . ? Ti1 N3 C30 C31 -3.0(2) . . . . ? C35 C30 C31 C32 -0.1(3) . . . . ? N3 C30 C31 C32 -179.86(16) . . . . ? C30 C31 C32 C33 0.4(3) . . . . ? C31 C32 C33 C34 -0.3(3) . . . . ? C31 C32 C33 C36 179.88(18) . . . . ? C32 C33 C34 C35 0.0(3) . . . . ? C36 C33 C34 C35 179.81(17) . . . . ? C33 C34 C35 C30 0.2(3) . . . . ? C31 C30 C35 C34 -0.2(2) . . . . ? N3 C30 C35 C34 179.55(16) . . . . ? C42 C37 C38 C39 0.7(3) . . . . ? C37 C38 C39 C40 1.3(3) . . . . ? C37 C38 C39 C43 -178.34(17) . . . . ? C38 C39 C40 C41 -1.2(3) . . . . ? C43 C39 C40 C41 178.48(16) . . . . ? C39 C40 C41 C42 -1.0(3) . . . . ? C40 C41 C42 C37 3.0(2) . . . . ? C40 C41 C42 N3 -173.83(15) . . . . ? C38 C37 C42 C41 -2.9(2) . . . . ? C38 C37 C42 N3 173.99(15) . . . . ? C30 N3 C42 C41 -97.73(18) . . . . ? Ti1 N3 C42 C41 87.81(16) . . . . ? C30 N3 C42 C37 85.52(19) . . . . ? Ti1 N3 C42 C37 -88.94(16) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 18.54 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.953 _refine_diff_density_min -1.002 _refine_diff_density_rms 0.152