data_cmpd_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H37 N2 Ti' _chemical_formula_weight 353.42 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' '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.717(3) _cell_length_b 16.961(3) _cell_length_c 17.638(4) _cell_angle_alpha 90.00 _cell_angle_beta 115.06(3) _cell_angle_gamma 90.00 _cell_volume 4259.2(15) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.102 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 0.404 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9057 _exptl_absorpt_correction_T_max 0.9418 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Nonius KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17461 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0925 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 28.27 _reflns_number_total 10511 _reflns_number_gt 6107 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement Denzo _computing_data_reduction Denzo _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material XCIF _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^)+(0.0797P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10511 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1184 _refine_ls_R_factor_gt 0.0579 _refine_ls_wR_factor_ref 0.1596 _refine_ls_wR_factor_gt 0.1385 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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 0.24154(3) 0.08145(2) 0.75963(3) 0.02783(13) Uani 1 1 d . . . N1 N 0.23610(14) 0.15800(11) 0.66571(13) 0.0334(5) Uani 1 1 d . . . N2 N 0.36534(13) 0.14260(11) 0.78361(13) 0.0322(5) Uani 1 1 d . . . C1 C 0.2403(2) -0.04289(14) 0.69678(17) 0.0473(8) Uani 1 1 d . . . C2 C 0.30808(17) -0.04893(13) 0.78045(17) 0.0335(6) Uani 1 1 d . . . C3 C 0.26247(16) -0.04061(13) 0.83306(15) 0.0300(6) Uani 1 1 d . . . C4 C 0.16512(17) -0.03038(14) 0.78237(18) 0.0370(6) Uani 1 1 d . . . C5 C 0.1508(2) -0.03185(15) 0.69812(18) 0.0471(8) Uani 1 1 d . . . C6 C 0.2587(3) -0.04917(19) 0.6198(2) 0.0867(14) Uani 1 1 d . . . H6A H 0.2553 -0.1046 0.6030 0.130 Uiso 1 1 calc R . . H6B H 0.3214 -0.0284 0.6321 0.130 Uiso 1 1 calc R . . H6C H 0.2114 -0.0186 0.5742 0.130 Uiso 1 1 calc R . . C7 C 0.4113(2) -0.06555(16) 0.8075(2) 0.0601(9) Uani 1 1 d . . . H7A H 0.4219 -0.1226 0.8121 0.090 Uiso 1 1 calc R . . H7B H 0.4477 -0.0409 0.8620 0.090 Uiso 1 1 calc R . . H7C H 0.4312 -0.0439 0.7661 0.090 Uiso 1 1 calc R . . C8 C 0.3050(2) -0.04604(17) 0.92659(17) 0.0495(7) Uani 1 1 d . . . H8A H 0.3069 -0.1013 0.9433 0.074 Uiso 1 1 calc R . . H8B H 0.2669 -0.0156 0.9481 0.074 Uiso 1 1 calc R . . H8C H 0.3689 -0.0247 0.9496 0.074 Uiso 1 1 calc R . . C9 C 0.0905(2) -0.02640(17) 0.8136(2) 0.0671(10) Uani 1 1 d . . . H9A H 0.0694 -0.0798 0.8180 0.101 Uiso 1 1 calc R . . H9B H 0.0373 0.0044 0.7744 0.101 Uiso 1 1 calc R . . H9C H 0.1159 -0.0012 0.8687 0.101 Uiso 1 1 calc R . . C10 C 0.0576(3) -0.03379(19) 0.6231(2) 0.0964(16) Uani 1 1 d . . . H10A H 0.0356 -0.0884 0.6112 0.145 Uiso 1 1 calc R . . H10B H 0.0645 -0.0118 0.5746 0.145 Uiso 1 1 calc R . . H10C H 0.0119 -0.0025 0.6344 0.145 Uiso 1 1 calc R . . C11 C 0.31765(17) 0.18972(13) 0.71884(16) 0.0330(6) Uani 1 1 d . . . C12 C 0.34803(19) 0.27201(15) 0.70895(19) 0.0495(8) Uani 1 1 d . . . H12A H 0.3878 0.2698 0.6787 0.074 Uiso 1 1 calc R . . H12B H 0.3835 0.2954 0.7643 0.074 Uiso 1 1 calc R . . H12C H 0.2925 0.3043 0.6774 0.074 Uiso 1 1 calc R . . C13 C 0.16838(18) 0.19979(16) 0.59291(17) 0.0426(7) Uani 1 1 d . . . H13A H 0.1766 0.2577 0.6045 0.051 Uiso 1 1 calc R . . C14 C 0.1848(3) 0.1828(2) 0.5167(2) 0.0786(12) Uani 1 1 d . . . H14A H 0.2490 0.1981 0.5273 0.118 Uiso 1 1 calc R . . H14C H 0.1400 0.2130 0.4692 0.118 Uiso 1 1 calc R . . H14D H 0.1761 0.1264 0.5040 0.118 Uiso 1 1 calc R . . C15 C 0.0696(2) 0.17716(19) 0.5798(2) 0.0675(10) Uani 1 1 d . . . H15A H 0.0613 0.1889 0.6307 0.101 Uiso 1 1 calc R . . H15B H 0.0600 0.1207 0.5675 0.101 Uiso 1 1 calc R . . H15C H 0.0239 0.2073 0.5328 0.101 Uiso 1 1 calc R . . C16 C 0.45077(17) 0.16857(14) 0.85424(17) 0.0394(7) Uani 1 1 d . . . H16A H 0.4500 0.2274 0.8571 0.047 Uiso 1 1 calc R . . C17 C 0.53787(18) 0.14329(18) 0.8426(2) 0.0524(8) Uani 1 1 d . . . H17A H 0.5351 0.1655 0.7903 0.079 Uiso 1 1 calc R . . H17B H 0.5400 0.0856 0.8403 0.079 Uiso 1 1 calc R . . H17C H 0.5943 0.1626 0.8897 0.079 Uiso 1 1 calc R . . C18 C 0.4523(2) 0.13546(18) 0.93457(17) 0.0501(8) Uani 1 1 d . . . H18A H 0.3959 0.1525 0.9405 0.075 Uiso 1 1 calc R . . H18B H 0.5082 0.1547 0.9823 0.075 Uiso 1 1 calc R . . H18C H 0.4539 0.0777 0.9329 0.075 Uiso 1 1 calc R . . C19 C 0.17917(19) 0.14878(14) 0.82619(19) 0.0429(7) Uani 1 1 d . . . H19A H 0.1102 0.1423 0.7971 0.051 Uiso 1 1 calc R . . H19B H 0.1998 0.1257 0.8828 0.051 Uiso 1 1 calc R . . C20 C 0.2010(2) 0.23729(15) 0.8360(2) 0.0506(8) Uani 1 1 d . . . H20A H 0.1689 0.2617 0.8670 0.076 Uiso 1 1 calc R . . H20B H 0.1792 0.2617 0.7806 0.076 Uiso 1 1 calc R . . H20C H 0.2689 0.2451 0.8666 0.076 Uiso 1 1 calc R . . Ti1' Ti 0.25420(3) -0.17678(2) 0.31504(3) 0.02922(13) Uani 1 1 d . . . N1' N 0.25116(14) -0.09761(12) 0.22367(12) 0.0334(5) Uani 1 1 d . . . N2' N 0.37814(14) -0.11523(11) 0.34211(13) 0.0342(5) Uani 1 1 d . . . C1' C 0.22213(18) -0.29262(14) 0.22950(16) 0.0344(6) Uani 1 1 d . . . C2' C 0.30768(17) -0.30541(14) 0.30005(18) 0.0373(6) Uani 1 1 d . . . C3' C 0.29071(19) -0.30678(14) 0.37224(17) 0.0404(7) Uani 1 1 d . . . C4' C 0.19341(19) -0.29449(15) 0.34571(17) 0.0394(6) Uani 1 1 d . . . C5' C 0.15088(16) -0.28513(14) 0.25865(16) 0.0329(6) Uani 1 1 d . . . C6' C 0.2096(2) -0.28885(18) 0.14040(19) 0.0579(8) Uani 1 1 d . . . H6'A H 0.1971 -0.3419 0.1160 0.087 Uiso 1 1 calc R . . H6'B H 0.2670 -0.2681 0.1387 0.087 Uiso 1 1 calc R . . H6'C H 0.1567 -0.2542 0.1083 0.087 Uiso 1 1 calc R . . C7' C 0.4009(2) -0.31875(17) 0.2959(3) 0.0680(11) Uani 1 1 d . . . H7'A H 0.4096 -0.3752 0.2899 0.102 Uiso 1 1 calc R . . H7'B H 0.4519 -0.2993 0.3475 0.102 Uiso 1 1 calc R . . H7'C H 0.4015 -0.2904 0.2478 0.102 Uiso 1 1 calc R . . C8' C 0.3604(2) -0.32722(18) 0.4595(2) 0.0728(11) Uani 1 1 d . . . H8'A H 0.3620 -0.3845 0.4670 0.109 Uiso 1 1 calc R . . H8'B H 0.3418 -0.3019 0.5001 0.109 Uiso 1 1 calc R . . H8'C H 0.4229 -0.3086 0.4682 0.109 Uiso 1 1 calc R . . C9' C 0.1435(2) -0.3001(2) 0.4027(2) 0.0682(10) Uani 1 1 d . . . H9'A H 0.1252 -0.3549 0.4052 0.102 Uiso 1 1 calc R . . H9'B H 0.0873 -0.2667 0.3807 0.102 Uiso 1 1 calc R . . H9'C H 0.1857 -0.2822 0.4590 0.102 Uiso 1 1 calc R . . C10' C 0.04714(17) -0.27662(17) 0.2054(2) 0.0536(8) Uani 1 1 d . . . H10D H 0.0188 -0.3290 0.1893 0.080 Uiso 1 1 calc R . . H10E H 0.0370 -0.2463 0.1550 0.080 Uiso 1 1 calc R . . H10F H 0.0181 -0.2491 0.2373 0.080 Uiso 1 1 calc R . . C11' C 0.33232(18) -0.06706(14) 0.27841(17) 0.0357(6) Uani 1 1 d . . . C12' C 0.3647(2) 0.01545(15) 0.2707(2) 0.0528(8) Uani 1 1 d . . . H12D H 0.4044 0.0135 0.2403 0.079 Uiso 1 1 calc R . . H12E H 0.4007 0.0374 0.3266 0.079 Uiso 1 1 calc R . . H12F H 0.3099 0.0489 0.2400 0.079 Uiso 1 1 calc R . . C13' C 0.18494(19) -0.05197(16) 0.15251(17) 0.0440(7) Uani 1 1 d . . . H13B H 0.1912 0.0049 0.1689 0.053 Uiso 1 1 calc R . . C14' C 0.2074(2) -0.0606(2) 0.0782(2) 0.0732(10) Uani 1 1 d . . . H14B H 0.2722 -0.0434 0.0934 0.110 Uiso 1 1 calc R . . H14E H 0.1642 -0.0280 0.0321 0.110 Uiso 1 1 calc R . . H14F H 0.2006 -0.1159 0.0607 0.110 Uiso 1 1 calc R . . C15' C 0.0871(2) -0.0776(2) 0.1327(2) 0.0647(10) Uani 1 1 d . . . H15D H 0.0749 -0.0714 0.1825 0.097 Uiso 1 1 calc R . . H15E H 0.0793 -0.1330 0.1156 0.097 Uiso 1 1 calc R . . H15F H 0.0427 -0.0451 0.0871 0.097 Uiso 1 1 calc R . . C16' C 0.46375(18) -0.09086(16) 0.41457(17) 0.0450(7) Uani 1 1 d . . . H16B H 0.4634 -0.0321 0.4188 0.054 Uiso 1 1 calc R . . C17' C 0.5508(2) -0.1151(2) 0.4034(2) 0.0854(13) Uani 1 1 d . . . H17D H 0.5487 -0.0918 0.3518 0.128 Uiso 1 1 calc R . . H17E H 0.5529 -0.1727 0.4000 0.128 Uiso 1 1 calc R . . H17F H 0.6070 -0.0964 0.4512 0.128 Uiso 1 1 calc R . . C18' C 0.4631(2) -0.12524(19) 0.49334(18) 0.0659(10) Uani 1 1 d . . . H18D H 0.4060 -0.1085 0.4983 0.099 Uiso 1 1 calc R . . H18E H 0.5184 -0.1066 0.5421 0.099 Uiso 1 1 calc R . . H18G H 0.4645 -0.1829 0.4908 0.099 Uiso 1 1 calc R . . C19' C 0.1871(2) -0.11213(17) 0.37901(18) 0.0501(7) Uani 1 1 d . . . H19C H 0.1186 -0.1220 0.3503 0.060 Uiso 1 1 calc R . . H19E H 0.2094 -0.1333 0.4365 0.060 Uiso 1 1 calc R . . C20' C 0.2033(2) -0.02252(17) 0.3847(2) 0.0637(9) Uani 1 1 d . . . H20G H 0.1698 0.0014 0.4149 0.096 Uiso 1 1 calc R . . H20D H 0.1798 -0.0003 0.3282 0.096 Uiso 1 1 calc R . . H20E H 0.2707 -0.0116 0.4148 0.096 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 0.0318(2) 0.0192(2) 0.0303(3) 0.00063(18) 0.0110(2) 0.00119(17) N1 0.0386(12) 0.0266(11) 0.0322(12) 0.0051(9) 0.0123(10) 0.0040(9) N2 0.0296(11) 0.0258(10) 0.0369(12) -0.0032(9) 0.0099(10) 0.0007(9) C1 0.090(2) 0.0168(13) 0.0401(17) -0.0003(11) 0.0330(17) -0.0003(13) C2 0.0409(14) 0.0202(12) 0.0458(16) 0.0026(11) 0.0245(13) 0.0025(11) C3 0.0368(14) 0.0193(12) 0.0338(14) 0.0039(10) 0.0150(12) 0.0007(10) C4 0.0326(14) 0.0216(12) 0.0552(18) 0.0020(12) 0.0172(13) -0.0025(10) C5 0.0492(17) 0.0225(13) 0.0468(18) 0.0010(12) -0.0016(14) -0.0026(12) C6 0.187(4) 0.0414(19) 0.055(2) -0.0055(16) 0.074(3) 0.004(2) C7 0.0507(18) 0.0357(15) 0.108(3) -0.0016(17) 0.047(2) 0.0065(13) C8 0.0632(19) 0.0436(16) 0.0387(17) 0.0080(13) 0.0187(15) -0.0012(14) C9 0.0492(18) 0.0389(17) 0.129(3) 0.0002(19) 0.053(2) -0.0038(14) C10 0.091(3) 0.0468(19) 0.073(3) 0.0050(18) -0.041(2) -0.0185(19) C11 0.0388(14) 0.0223(12) 0.0405(16) 0.0002(11) 0.0193(13) 0.0004(11) C12 0.0514(17) 0.0294(14) 0.065(2) 0.0058(14) 0.0215(16) -0.0063(12) C13 0.0427(16) 0.0336(14) 0.0457(17) 0.0133(13) 0.0132(14) 0.0096(12) C14 0.084(3) 0.107(3) 0.044(2) 0.032(2) 0.0267(19) 0.041(2) C15 0.0464(19) 0.071(2) 0.067(2) 0.0313(18) 0.0072(17) 0.0160(16) C16 0.0361(15) 0.0285(13) 0.0457(17) -0.0071(12) 0.0096(13) -0.0031(11) C17 0.0356(16) 0.0550(18) 0.064(2) -0.0070(16) 0.0180(15) -0.0064(13) C18 0.0460(17) 0.0582(19) 0.0373(17) -0.0073(14) 0.0091(14) -0.0008(14) C19 0.0500(17) 0.0292(13) 0.0546(18) 0.0004(13) 0.0270(15) 0.0032(12) C20 0.0535(18) 0.0376(16) 0.068(2) -0.0068(15) 0.0328(16) 0.0040(13) Ti1' 0.0333(3) 0.0256(2) 0.0282(3) -0.00296(19) 0.0126(2) -0.00014(18) N1' 0.0340(12) 0.0336(11) 0.0286(12) 0.0046(9) 0.0094(10) 0.0023(9) N2' 0.0343(11) 0.0271(10) 0.0325(12) -0.0022(9) 0.0059(10) -0.0020(9) C1' 0.0464(16) 0.0263(13) 0.0376(15) -0.0073(11) 0.0246(13) -0.0057(11) C2' 0.0336(14) 0.0237(12) 0.0577(19) -0.0007(12) 0.0224(14) -0.0015(10) C3' 0.0426(16) 0.0276(13) 0.0420(17) 0.0057(12) 0.0093(13) -0.0039(11) C4' 0.0474(16) 0.0357(14) 0.0435(17) -0.0060(12) 0.0275(14) -0.0109(12) C5' 0.0302(13) 0.0277(13) 0.0399(15) -0.0061(11) 0.0138(12) -0.0013(10) C6' 0.089(2) 0.0482(18) 0.0502(19) -0.0166(15) 0.0430(18) -0.0136(17) C7' 0.0481(18) 0.0442(18) 0.126(3) -0.0076(19) 0.050(2) 0.0012(14) C8' 0.077(2) 0.052(2) 0.058(2) 0.0212(17) -0.0019(19) -0.0123(17) C9' 0.088(2) 0.068(2) 0.077(2) -0.0153(18) 0.063(2) -0.0273(19) C10' 0.0361(16) 0.0453(17) 0.069(2) -0.0146(15) 0.0126(15) -0.0014(13) C11' 0.0409(15) 0.0265(13) 0.0418(16) -0.0015(12) 0.0196(13) 0.0009(11) C12' 0.0546(18) 0.0328(15) 0.064(2) 0.0025(14) 0.0190(16) -0.0082(13) C13' 0.0468(16) 0.0427(16) 0.0372(16) 0.0094(13) 0.0126(13) 0.0078(13) C14' 0.071(2) 0.103(3) 0.046(2) 0.0268(19) 0.0256(18) 0.029(2) C15' 0.0439(18) 0.092(3) 0.049(2) 0.0140(18) 0.0114(16) 0.0205(17) C16' 0.0411(16) 0.0363(15) 0.0428(17) -0.0074(13) 0.0034(14) -0.0074(12) C17' 0.0353(18) 0.117(3) 0.083(3) -0.027(2) 0.0052(19) -0.0081(19) C18' 0.068(2) 0.060(2) 0.0404(18) 0.0029(16) -0.0048(17) -0.0107(17) C19' 0.0599(19) 0.0509(17) 0.0444(18) -0.0080(14) 0.0269(15) 0.0057(15) C20' 0.090(2) 0.0479(18) 0.061(2) -0.0123(16) 0.0390(19) 0.0132(17) _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 N1 2.078(2) . ? Ti1 N2 2.084(2) . ? Ti1 C19 2.149(3) . ? Ti1 C5 2.365(3) . ? Ti1 C4 2.368(2) . ? Ti1 C1 2.379(3) . ? Ti1 C3 2.390(2) . ? Ti1 C2 2.407(2) . ? Ti1 C11 2.460(2) . ? N1 C11 1.339(3) . ? N1 C13 1.458(3) . ? N2 C11 1.334(3) . ? N2 C16 1.460(3) . ? C1 C2 1.411(4) . ? C1 C5 1.429(4) . ? C1 C6 1.508(4) . ? C2 C3 1.399(3) . ? C2 C7 1.511(4) . ? C3 C4 1.418(3) . ? C3 C8 1.498(4) . ? C4 C5 1.406(4) . ? C4 C9 1.493(4) . ? C5 C10 1.502(4) . ? C11 C12 1.509(3) . ? C13 C14 1.499(4) . ? C13 C15 1.518(4) . ? C16 C18 1.515(4) . ? C16 C17 1.529(4) . ? C19 C20 1.533(3) . ? Ti1' N2' 2.080(2) . ? Ti1' N1' 2.082(2) . ? Ti1' C19' 2.144(3) . ? Ti1' C4' 2.373(3) . ? Ti1' C5' 2.374(2) . ? Ti1' C3' 2.391(2) . ? Ti1' C2' 2.393(2) . ? Ti1' C1' 2.397(2) . ? Ti1' C11' 2.462(3) . ? N1' C11' 1.336(3) . ? N1' C13' 1.467(3) . ? N2' C11' 1.328(3) . ? N2' C16' 1.469(3) . ? C1' C2' 1.409(4) . ? C1' C5' 1.422(3) . ? C1' C6' 1.500(4) . ? C2' C3' 1.407(4) . ? C2' C7' 1.514(4) . ? C3' C4' 1.412(4) . ? C3' C8' 1.503(4) . ? C4' C5' 1.400(4) . ? C4' C9' 1.518(4) . ? C5' C10' 1.504(3) . ? C11' C12' 1.515(3) . ? C13' C15' 1.490(4) . ? C13' C14' 1.502(4) . ? C16' C18' 1.511(4) . ? C16' C17' 1.519(4) . ? C19' C20' 1.537(4) . ? 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 N1 Ti1 N2 64.55(8) . . ? N1 Ti1 C19 103.25(9) . . ? N2 Ti1 C19 103.14(9) . . ? N1 Ti1 C5 109.20(10) . . ? N2 Ti1 C5 145.83(10) . . ? C19 Ti1 C5 110.87(11) . . ? N1 Ti1 C4 141.53(9) . . ? N2 Ti1 C4 149.43(8) . . ? C19 Ti1 C4 87.23(10) . . ? C5 Ti1 C4 34.55(10) . . ? N1 Ti1 C1 101.13(9) . . ? N2 Ti1 C1 111.02(10) . . ? C19 Ti1 C1 144.10(10) . . ? C5 Ti1 C1 35.06(10) . . ? C4 Ti1 C1 57.59(10) . . ? N1 Ti1 C3 157.39(8) . . ? N2 Ti1 C3 114.76(8) . . ? C19 Ti1 C3 98.88(10) . . ? C5 Ti1 C3 57.49(9) . . ? C4 Ti1 C3 34.68(8) . . ? C1 Ti1 C3 57.08(9) . . ? N1 Ti1 C2 124.34(9) . . ? N2 Ti1 C2 96.80(8) . . ? C19 Ti1 C2 132.39(10) . . ? C5 Ti1 C2 57.46(9) . . ? C4 Ti1 C2 57.12(8) . . ? C1 Ti1 C2 34.30(9) . . ? C3 Ti1 C2 33.92(8) . . ? N1 Ti1 C11 32.98(8) . . ? N2 Ti1 C11 32.85(8) . . ? C19 Ti1 C11 98.86(9) . . ? C5 Ti1 C11 138.24(10) . . ? C4 Ti1 C11 172.66(9) . . ? C1 Ti1 C11 115.77(9) . . ? C3 Ti1 C11 146.40(8) . . ? C2 Ti1 C11 119.79(8) . . ? C11 N1 C13 123.1(2) . . ? C11 N1 Ti1 89.38(15) . . ? C13 N1 Ti1 140.71(17) . . ? C11 N2 C16 122.0(2) . . ? C11 N2 Ti1 89.24(15) . . ? C16 N2 Ti1 139.94(18) . . ? C2 C1 C5 107.8(2) . . ? C2 C1 C6 126.1(3) . . ? C5 C1 C6 126.2(3) . . ? C2 C1 Ti1 73.95(14) . . ? C5 C1 Ti1 71.95(15) . . ? C6 C1 Ti1 121.03(19) . . ? C3 C2 C1 108.3(2) . . ? C3 C2 C7 126.3(3) . . ? C1 C2 C7 125.3(3) . . ? C3 C2 Ti1 72.36(13) . . ? C1 C2 Ti1 71.76(14) . . ? C7 C2 Ti1 123.96(17) . . ? C2 C3 C4 108.2(2) . . ? C2 C3 C8 127.6(2) . . ? C4 C3 C8 124.1(2) . . ? C2 C3 Ti1 73.72(13) . . ? C4 C3 Ti1 71.83(13) . . ? C8 C3 Ti1 123.03(17) . . ? C5 C4 C3 108.1(2) . . ? C5 C4 C9 126.2(3) . . ? C3 C4 C9 125.4(3) . . ? C5 C4 Ti1 72.60(15) . . ? C3 C4 Ti1 73.49(13) . . ? C9 C4 Ti1 124.05(18) . . ? C4 C5 C1 107.5(2) . . ? C4 C5 C10 126.3(3) . . ? C1 C5 C10 125.6(3) . . ? C4 C5 Ti1 72.85(14) . . ? C1 C5 Ti1 72.99(15) . . ? C10 C5 Ti1 126.55(19) . . ? N2 C11 N1 112.5(2) . . ? N2 C11 C12 124.2(2) . . ? N1 C11 C12 123.1(2) . . ? N2 C11 Ti1 57.92(12) . . ? N1 C11 Ti1 57.65(12) . . ? C12 C11 Ti1 160.27(19) . . ? N1 C13 C14 111.0(2) . . ? N1 C13 C15 109.2(2) . . ? C14 C13 C15 111.6(3) . . ? N2 C16 C18 109.3(2) . . ? N2 C16 C17 110.7(2) . . ? C18 C16 C17 111.2(2) . . ? C20 C19 Ti1 116.73(19) . . ? N2' Ti1' N1' 64.29(8) . . ? N2' Ti1' C19' 104.14(10) . . ? N1' Ti1' C19' 102.85(10) . . ? N2' Ti1' C4' 143.00(9) . . ? N1' Ti1' C4' 147.09(9) . . ? C19' Ti1' C4' 88.56(10) . . ? N2' Ti1' C5' 153.24(8) . . ? N1' Ti1' C5' 112.80(9) . . ? C19' Ti1' C5' 102.39(10) . . ? C4' Ti1' C5' 34.31(9) . . ? N2' Ti1' C3' 109.39(9) . . ? N1' Ti1' C3' 147.54(9) . . ? C19' Ti1' C3' 109.46(11) . . ? C4' Ti1' C3' 34.49(9) . . ? C5' Ti1' C3' 57.47(9) . . ? N2' Ti1' C2' 98.31(8) . . ? N1' Ti1' C2' 113.36(9) . . ? C19' Ti1' C2' 143.00(11) . . ? C4' Ti1' C2' 56.78(9) . . ? C5' Ti1' C2' 57.16(8) . . ? C3' Ti1' C2' 34.22(9) . . ? N2' Ti1' C1' 118.87(9) . . ? N1' Ti1' C1' 96.41(8) . . ? C19' Ti1' C1' 136.99(10) . . ? C4' Ti1' C1' 57.06(9) . . ? C5' Ti1' C1' 34.68(8) . . ? C3' Ti1' C1' 57.23(9) . . ? C2' Ti1' C1' 34.22(9) . . ? N2' Ti1' C11' 32.64(8) . . ? N1' Ti1' C11' 32.86(8) . . ? C19' Ti1' C11' 99.37(10) . . ? C4' Ti1' C11' 171.79(9) . . ? C5' Ti1' C11' 143.52(9) . . ? C3' Ti1' C11' 138.64(9) . . ? C2' Ti1' C11' 115.01(8) . . ? C1' Ti1' C11' 116.73(9) . . ? C11' N1' C13' 121.9(2) . . ? C11' N1' Ti1' 89.36(15) . . ? C13' N1' Ti1' 141.08(17) . . ? C11' N2' C16' 122.1(2) . . ? C11' N2' Ti1' 89.71(15) . . ? C16' N2' Ti1' 139.88(18) . . ? C2' C1' C5' 107.3(2) . . ? C2' C1' C6' 125.7(2) . . ? C5' C1' C6' 127.0(3) . . ? C2' C1' Ti1' 72.71(14) . . ? C5' C1' Ti1' 71.77(14) . . ? C6' C1' Ti1' 121.58(17) . . ? C3' C2' C1' 109.0(2) . . ? C3' C2' C7' 126.8(3) . . ? C1' C2' C7' 124.1(3) . . ? C3' C2' Ti1' 72.85(15) . . ? C1' C2' Ti1' 73.07(14) . . ? C7' C2' Ti1' 122.26(17) . . ? C2' C3' C4' 106.9(2) . . ? C2' C3' C8' 126.5(3) . . ? C4' C3' C8' 126.2(3) . . ? C2' C3' Ti1' 72.94(14) . . ? C4' C3' Ti1' 72.03(14) . . ? C8' C3' Ti1' 125.81(18) . . ? C5' C4' C3' 109.1(2) . . ? C5' C4' C9' 126.4(3) . . ? C3' C4' C9' 124.2(3) . . ? C5' C4' Ti1' 72.89(14) . . ? C3' C4' Ti1' 73.48(14) . . ? C9' C4' Ti1' 125.09(19) . . ? C4' C5' C1' 107.6(2) . . ? C4' C5' C10' 125.6(2) . . ? C1' C5' C10' 126.5(2) . . ? C4' C5' Ti1' 72.79(14) . . ? C1' C5' Ti1' 73.55(14) . . ? C10' C5' Ti1' 123.73(17) . . ? N2' C11' N1' 112.5(2) . . ? N2' C11' C12' 124.2(2) . . ? N1' C11' C12' 123.2(2) . . ? N2' C11' Ti1' 57.65(13) . . ? N1' C11' Ti1' 57.77(12) . . ? C12' C11' Ti1' 161.1(2) . . ? N1' C13' C15' 109.5(2) . . ? N1' C13' C14' 110.6(2) . . ? C15' C13' C14' 111.6(3) . . ? N2' C16' C18' 109.3(2) . . ? N2' C16' C17' 110.8(2) . . ? C18' C16' C17' 111.8(3) . . ? C20' C19' Ti1' 115.8(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.409 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.060