Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Anjana Devi' _publ_contact_author_address ; Lehrstuhl fur Anorganische Chemie II Ruhr-University Bochum Universitaetsstrasse 150 Bochum 44789 GERMANY ; _publ_contact_author_email ANJANA.DEVI@RUB.DE _publ_section_title ; Precursor chemistry for TiO2: Titanium complexes with mixed nitrogen/oxygen ligand sphere ; loop_ _publ_author_name 'Anjana Devi' 'Arne Baunemann' 'Raghunandan Bhakta' 'Roland A. Fischer' 'Malte Hellwig' ; S.A.Shivashankar ; 'Ashish Varade' 'Manuela Winter' data_cvd73 _database_code_depnum_ccdc_archive 'CCDC 297832' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H100 N4 O16 Ti2' _chemical_formula_weight 1133.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7058(9) _cell_length_b 11.9666(9) _cell_length_c 23.9999(18) _cell_angle_alpha 99.452(6) _cell_angle_beta 98.297(6) _cell_angle_gamma 93.037(6) _cell_volume 3271.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 105(2) _cell_measurement_reflns_used 4691 _cell_measurement_theta_min 2.88 _cell_measurement_theta_max 27.49 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.150 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.304 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.889 _exptl_absorpt_correction_T_max 0.938 _exptl_absorpt_process_details 'Gaussian face-indexed' _exptl_special_details ; ? ; _diffrn_ambient_temperature 105(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '1330 images at 1.0 deg. in \w and 20 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34903 _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_sigmaI/netI 0.0966 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11427 _reflns_number_gt 6835 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0359P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11427 _refine_ls_number_parameters 699 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0817 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.0915 _refine_ls_wR_factor_gt 0.0811 _refine_ls_goodness_of_fit_ref 0.860 _refine_ls_restrained_S_all 0.860 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti2 Ti 0.76613(4) 0.20624(4) 0.392334(18) 0.02461(13) Uani 1 1 d . . . O26 O 0.69987(13) 0.24577(13) 0.31243(7) 0.0243(4) Uani 1 1 d . . . O210 O 0.77863(13) 0.05414(13) 0.34603(7) 0.0240(4) Uani 1 1 d . . . O27 O 0.65447(13) 0.23317(13) 0.21665(7) 0.0262(4) Uani 1 1 d . . . O29 O 0.79925(13) -0.08498(13) 0.27296(6) 0.0246(4) Uani 1 1 d . . . O21 O 0.92469(13) 0.25234(14) 0.36800(6) 0.0261(4) Uani 1 1 d . . . O25 O 0.77193(13) 0.37328(13) 0.42206(6) 0.0259(4) Uani 1 1 d . . . O22 O 1.08065(13) 0.35662(13) 0.35323(7) 0.0296(4) Uani 1 1 d . . . O24 O 0.81481(13) 0.56342(14) 0.43964(7) 0.0303(4) Uani 1 1 d . . . N22 N 0.61254(16) 0.17104(17) 0.40611(8) 0.0281(5) Uani 1 1 d . . . C215 C 0.5181(2) 0.1181(2) 0.36188(12) 0.0432(8) Uani 1 1 d . . . H21A H 0.4772 0.0567 0.3754 0.065 Uiso 1 1 calc R . . H21B H 0.5493 0.0870 0.3273 0.065 Uiso 1 1 calc R . . H21C H 0.4642 0.1750 0.3531 0.065 Uiso 1 1 calc R . . C292 C 0.7070(2) -0.1912(2) 0.33538(12) 0.0435(8) Uani 1 1 d . . . H29A H 0.6992 -0.1257 0.3646 0.065 Uiso 1 1 calc R . . H29B H 0.7116 -0.2597 0.3528 0.065 Uiso 1 1 calc R . . H29C H 0.6395 -0.2010 0.3051 0.065 Uiso 1 1 calc R . . C223 C 1.0356(2) 0.2329(2) 0.26043(10) 0.0354(7) Uani 1 1 d . . . H22A H 0.9640 0.1954 0.2677 0.053 Uiso 1 1 calc R . . H22B H 1.0695 0.1819 0.2321 0.053 Uiso 1 1 calc R . . H22C H 1.0182 0.3029 0.2459 0.053 Uiso 1 1 calc R . . C222 C 1.2352(2) 0.3123(2) 0.30494(12) 0.0414(7) Uani 1 1 d . . . H22D H 1.2219 0.3788 0.2866 0.062 Uiso 1 1 calc R . . H22E H 1.2709 0.2557 0.2800 0.062 Uiso 1 1 calc R . . H22F H 1.2869 0.3354 0.3415 0.062 Uiso 1 1 calc R . . C214 C 0.5716(2) 0.2090(2) 0.45965(11) 0.0445(8) Uani 1 1 d . . . H21D H 0.5210 0.2706 0.4553 0.067 Uiso 1 1 calc R . . H21E H 0.6379 0.2365 0.4896 0.067 Uiso 1 1 calc R . . H21F H 0.5283 0.1455 0.4703 0.067 Uiso 1 1 calc R . . C273 C 0.5769(2) 0.3556(2) 0.15788(11) 0.0399(7) Uani 1 1 d . . . H27A H 0.6440 0.3471 0.1378 0.060 Uiso 1 1 calc R . . H27B H 0.5468 0.4296 0.1550 0.060 Uiso 1 1 calc R . . H27C H 0.5165 0.2950 0.1405 0.060 Uiso 1 1 calc R . . N21 N 0.83967(17) 0.17107(17) 0.46281(8) 0.0289(5) Uani 1 1 d . . . C29 C 0.77009(19) 0.0195(2) 0.29247(10) 0.0210(6) Uani 1 1 d . . . C28 C 0.73155(19) 0.0806(2) 0.25018(10) 0.0225(6) Uani 1 1 d . . . H28 H 0.7291 0.0470 0.2113 0.027 Uiso 1 1 calc R . . C241 C 0.7118(2) 0.5850(2) 0.46770(10) 0.0252(6) Uani 1 1 d . . . C291 C 0.8164(2) -0.1714(2) 0.30993(10) 0.0270(6) Uani 1 1 d . . . C27 C 0.69607(19) 0.1904(2) 0.26312(11) 0.0231(6) Uani 1 1 d . . . C271 C 0.6131(2) 0.3479(2) 0.22040(11) 0.0293(6) Uani 1 1 d . . . C239 C 0.9420(2) 0.4520(2) 0.39573(10) 0.0295(6) Uani 1 1 d . . . H23 H 0.9883 0.5199 0.3962 0.035 Uiso 1 1 calc R . . C24 C 0.8401(2) 0.4582(2) 0.41886(10) 0.0266(6) Uani 1 1 d . . . C244 C 0.7256(2) 0.7130(2) 0.48535(11) 0.0354(7) Uani 1 1 d . . . H24A H 0.7983 0.7351 0.5118 0.053 Uiso 1 1 calc R . . H24B H 0.6605 0.7384 0.5043 0.053 Uiso 1 1 calc R . . H24C H 0.7271 0.7484 0.4514 0.053 Uiso 1 1 calc R . . C221 C 1.1206(2) 0.2612(2) 0.31551(10) 0.0271(6) Uani 1 1 d . . . C243 C 0.7183(2) 0.5287(2) 0.52007(10) 0.0340(7) Uani 1 1 d . . . H24D H 0.7049 0.4461 0.5081 0.051 Uiso 1 1 calc R . . H24E H 0.6592 0.5563 0.5428 0.051 Uiso 1 1 calc R . . H24F H 0.7952 0.5472 0.5432 0.051 Uiso 1 1 calc R . . C293 C 0.8340(2) -0.2753(2) 0.26744(11) 0.0356(7) Uani 1 1 d . . . H29D H 0.7656 -0.2930 0.2378 0.053 Uiso 1 1 calc R . . H29E H 0.8456 -0.3401 0.2873 0.053 Uiso 1 1 calc R . . H29F H 0.9022 -0.2600 0.2497 0.053 Uiso 1 1 calc R . . C274 C 0.5092(2) 0.3555(2) 0.25170(11) 0.0329(6) Uani 1 1 d . . . H27D H 0.4519 0.2919 0.2347 0.049 Uiso 1 1 calc R . . H27E H 0.4745 0.4274 0.2484 0.049 Uiso 1 1 calc R . . H27F H 0.5342 0.3522 0.2921 0.049 Uiso 1 1 calc R . . C242 C 0.6024(2) 0.5479(2) 0.42575(11) 0.0353(7) Uani 1 1 d . . . H24G H 0.6056 0.5817 0.3914 0.053 Uiso 1 1 calc R . . H24H H 0.5355 0.5731 0.4433 0.053 Uiso 1 1 calc R . . H24I H 0.5951 0.4649 0.4153 0.053 Uiso 1 1 calc R . . C272 C 0.7111(2) 0.4366(2) 0.24751(13) 0.0448(8) Uani 1 1 d . . . H27G H 0.7285 0.4352 0.2886 0.067 Uiso 1 1 calc R . . H27H H 0.6882 0.5119 0.2417 0.067 Uiso 1 1 calc R . . H27I H 0.7801 0.4199 0.2298 0.067 Uiso 1 1 calc R . . C216 C 0.8089(2) 0.0694(2) 0.48546(11) 0.0429(7) Uani 1 1 d . . . H21G H 0.8725 0.0193 0.4846 0.064 Uiso 1 1 calc R . . H21H H 0.7386 0.0294 0.4620 0.064 Uiso 1 1 calc R . . H21I H 0.7952 0.0913 0.5250 0.064 Uiso 1 1 calc R . . C294 C 0.9230(2) -0.1380(2) 0.35457(11) 0.0422(7) Uani 1 1 d . . . H29G H 0.9890 -0.1198 0.3359 0.063 Uiso 1 1 calc R . . H29H H 0.9396 -0.2013 0.3750 0.063 Uiso 1 1 calc R . . H29I H 0.9094 -0.0714 0.3818 0.063 Uiso 1 1 calc R . . C217 C 0.9419(2) 0.2346(2) 0.49832(11) 0.0418(7) Uani 1 1 d . . . H21J H 0.9249 0.2600 0.5370 0.063 Uiso 1 1 calc R . . H21K H 0.9632 0.3008 0.4817 0.063 Uiso 1 1 calc R . . H21L H 1.0064 0.1856 0.5001 0.063 Uiso 1 1 calc R . . C224 C 1.1410(2) 0.1597(2) 0.34527(11) 0.0391(7) Uani 1 1 d . . . H22G H 1.1877 0.1852 0.3830 0.059 Uiso 1 1 calc R . . H22H H 1.1821 0.1047 0.3223 0.059 Uiso 1 1 calc R . . H22I H 1.0664 0.1238 0.3497 0.059 Uiso 1 1 calc R . . C229 C 0.9777(2) 0.3487(2) 0.37189(10) 0.0261(6) Uani 1 1 d . . . Ti1 Ti 0.25450(4) 0.81567(4) 0.143482(18) 0.02096(12) Uani 1 1 d . . . O6 O 0.29274(13) 0.77255(13) 0.22094(6) 0.0218(4) Uani 1 1 d . . . O10 O 0.41945(13) 0.76146(13) 0.13454(6) 0.0229(4) Uani 1 1 d . . . O7 O 0.36418(13) 0.68211(14) 0.29251(7) 0.0286(4) Uani 1 1 d . . . O9 O 0.57153(13) 0.65303(13) 0.14341(7) 0.0275(4) Uani 1 1 d . . . O5 O 0.20370(13) 0.64146(13) 0.11506(6) 0.0228(4) Uani 1 1 d . . . O1 O 0.23457(13) 0.81838(13) 0.05982(6) 0.0219(4) Uani 1 1 d . . . O2 O 0.20509(13) 0.77237(13) -0.03642(6) 0.0269(4) Uani 1 1 d . . . O4 O 0.15617(14) 0.47159(13) 0.05681(7) 0.0291(4) Uani 1 1 d . . . N1 N 0.31738(16) 0.96906(16) 0.16667(8) 0.0247(5) Uani 1 1 d . . . N2 N 0.09906(15) 0.84827(16) 0.15058(8) 0.0231(5) Uani 1 1 d . . . C911 C 0.7110(2) 0.6045(2) 0.08621(12) 0.0381(7) Uani 1 1 d . . . H19A H 0.7661 0.6167 0.1219 0.057 Uiso 1 1 calc R . . H19B H 0.7510 0.6209 0.0549 0.057 Uiso 1 1 calc R . . H19C H 0.6785 0.5253 0.0777 0.057 Uiso 1 1 calc R . . C711 C 0.1540(2) 0.6604(2) 0.29185(11) 0.0364(7) Uani 1 1 d . . . H17A H 0.1321 0.6990 0.2594 0.055 Uiso 1 1 calc R . . H17B H 0.0947 0.6682 0.3169 0.055 Uiso 1 1 calc R . . H17C H 0.1604 0.5797 0.2778 0.055 Uiso 1 1 calc R . . C413 C 0.0457(2) 0.4550(2) 0.13451(12) 0.0448(8) Uani 1 1 d . . . H14A H 0.0700 0.5316 0.1559 0.067 Uiso 1 1 calc R . . H14B H 0.0278 0.4048 0.1610 0.067 Uiso 1 1 calc R . . H14C H -0.0234 0.4578 0.1065 0.067 Uiso 1 1 calc R . . C11 C 0.2664(2) 1.0665(2) 0.14663(11) 0.0328(6) Uani 1 1 d . . . H11A H 0.2641 1.1268 0.1794 0.049 Uiso 1 1 calc R . . H11B H 0.1875 1.0436 0.1266 0.049 Uiso 1 1 calc R . . H11C H 0.3133 1.0947 0.1204 0.049 Uiso 1 1 calc R . . C12 C 0.4326(2) 1.0033(2) 0.19951(12) 0.0388(7) Uani 1 1 d . . . H11D H 0.4839 1.0291 0.1745 0.058 Uiso 1 1 calc R . . H11E H 0.4639 0.9384 0.2150 0.058 Uiso 1 1 calc R . . H11F H 0.4273 1.0653 0.2310 0.058 Uiso 1 1 calc R . . C7 C 0.3690(2) 0.7114(2) 0.24125(10) 0.0226(6) Uani 1 1 d . . . C3 C 0.18561(19) 0.6271(2) 0.01514(10) 0.0235(6) Uani 1 1 d . . . H13 H 0.1694 0.5763 -0.0204 0.028 Uiso 1 1 calc R . . C4 C 0.18403(19) 0.5847(2) 0.06526(11) 0.0229(6) Uani 1 1 d . . . C9 C 0.4790(2) 0.6996(2) 0.16282(10) 0.0230(6) Uani 1 1 d . . . C211 C 0.1388(2) 0.9643(2) -0.01748(10) 0.0299(6) Uani 1 1 d . . . H12A H 0.0604 0.9296 -0.0327 0.045 Uiso 1 1 calc R . . H12B H 0.1468 1.0405 -0.0272 0.045 Uiso 1 1 calc R . . H12C H 0.1525 0.9699 0.0242 0.045 Uiso 1 1 calc R . . C71 C 0.2692(2) 0.7135(2) 0.32501(10) 0.0261(6) Uani 1 1 d . . . C21 C 0.2263(2) 0.8917(2) -0.04332(10) 0.0286(6) Uani 1 1 d . . . C8 C 0.46068(19) 0.6723(2) 0.21539(10) 0.0235(6) Uani 1 1 d . . . H8A H 0.5122 0.6259 0.2337 0.028 Uiso 1 1 calc R . . C2 C 0.21036(19) 0.7421(2) 0.01533(10) 0.0229(6) Uani 1 1 d . . . C912 C 0.6617(2) 0.8064(2) 0.10578(12) 0.0383(7) Uani 1 1 d . . . H19D H 0.5980 0.8551 0.1111 0.057 Uiso 1 1 calc R . . H19E H 0.6988 0.8246 0.0740 0.057 Uiso 1 1 calc R . . H19F H 0.7186 0.8193 0.1408 0.057 Uiso 1 1 calc R . . C23 C -0.0028(2) 0.7896(2) 0.11319(11) 0.0349(7) Uani 1 1 d . . . H11G H -0.0443 0.7413 0.1342 0.052 Uiso 1 1 calc R . . H11H H 0.0211 0.7425 0.0801 0.052 Uiso 1 1 calc R . . H11I H -0.0538 0.8455 0.1001 0.052 Uiso 1 1 calc R . . C91 C 0.6145(2) 0.6825(2) 0.09257(11) 0.0283(6) Uani 1 1 d . . . C722 C 0.2721(2) 0.8414(2) 0.34193(11) 0.0385(7) Uani 1 1 d . . . H17D H 0.3504 0.8714 0.3604 0.058 Uiso 1 1 calc R . . H17E H 0.2172 0.8603 0.3686 0.058 Uiso 1 1 calc R . . H17F H 0.2506 0.8752 0.3077 0.058 Uiso 1 1 calc R . . C41 C 0.1420(2) 0.4101(2) 0.10395(11) 0.0332(7) Uani 1 1 d . . . C22 C 0.0664(2) 0.9246(2) 0.19838(11) 0.0360(7) Uani 1 1 d . . . H11J H 0.0137 0.9778 0.1838 0.054 Uiso 1 1 calc R . . H11K H 0.1359 0.9671 0.2214 0.054 Uiso 1 1 calc R . . H11L H 0.0276 0.8802 0.2221 0.054 Uiso 1 1 calc R . . C723 C 0.3005(2) 0.6592(2) 0.37766(11) 0.0409(7) Uani 1 1 d . . . H17G H 0.3009 0.5768 0.3660 0.061 Uiso 1 1 calc R . . H17H H 0.2432 0.6754 0.4034 0.061 Uiso 1 1 calc R . . H17I H 0.3774 0.6904 0.3975 0.061 Uiso 1 1 calc R . . C412 C 0.1090(3) 0.2896(2) 0.07186(12) 0.0481(8) Uani 1 1 d . . . H14D H 0.0376 0.2883 0.0447 0.072 Uiso 1 1 calc R . . H14E H 0.0967 0.2392 0.0991 0.072 Uiso 1 1 calc R . . H14F H 0.1715 0.2636 0.0510 0.072 Uiso 1 1 calc R . . C913 C 0.5217(2) 0.6570(3) 0.03992(11) 0.0459(8) Uani 1 1 d . . . H19G H 0.4798 0.5834 0.0389 0.069 Uiso 1 1 calc R . . H19H H 0.5581 0.6544 0.0055 0.069 Uiso 1 1 calc R . . H19I H 0.4675 0.7166 0.0414 0.069 Uiso 1 1 calc R . . C411 C 0.2560(2) 0.4150(2) 0.14382(13) 0.0508(9) Uani 1 1 d . . . H14G H 0.3170 0.3912 0.1215 0.076 Uiso 1 1 calc R . . H14H H 0.2484 0.3640 0.1714 0.076 Uiso 1 1 calc R . . H14I H 0.2761 0.4929 0.1644 0.076 Uiso 1 1 calc R . . C213 C 0.2045(3) 0.8825(2) -0.10768(11) 0.0444(8) Uani 1 1 d . . . H12D H 0.2617 0.8363 -0.1244 0.067 Uiso 1 1 calc R . . H12E H 0.2112 0.9586 -0.1176 0.067 Uiso 1 1 calc R . . H12F H 0.1265 0.8467 -0.1227 0.067 Uiso 1 1 calc R . . C212 C 0.3507(2) 0.9334(2) -0.01933(13) 0.0446(8) Uani 1 1 d . . . H12G H 0.3625 0.9394 0.0223 0.067 Uiso 1 1 calc R . . H12H H 0.3677 1.0082 -0.0292 0.067 Uiso 1 1 calc R . . H12I H 0.4024 0.8797 -0.0356 0.067 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 Ti2 0.0244(3) 0.0253(3) 0.0227(3) -0.0001(2) 0.0042(2) 0.0017(2) O26 0.0286(10) 0.0195(10) 0.0227(10) -0.0005(8) 0.0011(8) 0.0025(7) O210 0.0297(10) 0.0218(10) 0.0197(10) 0.0029(8) 0.0007(7) 0.0048(7) O27 0.0337(10) 0.0213(10) 0.0258(10) 0.0088(8) 0.0051(8) 0.0072(8) O29 0.0350(10) 0.0177(10) 0.0227(9) 0.0064(7) 0.0058(8) 0.0050(8) O21 0.0259(9) 0.0239(10) 0.0275(10) -0.0008(8) 0.0072(8) 0.0006(8) O25 0.0229(9) 0.0249(10) 0.0275(10) -0.0048(8) 0.0071(7) 0.0000(8) O22 0.0250(9) 0.0278(10) 0.0343(10) -0.0072(8) 0.0147(8) 0.0002(8) O24 0.0267(10) 0.0254(11) 0.0385(11) -0.0041(8) 0.0152(8) 0.0030(8) N22 0.0260(12) 0.0301(13) 0.0268(12) -0.0006(10) 0.0070(10) -0.0012(10) C215 0.0279(16) 0.053(2) 0.0450(18) 0.0088(15) -0.0017(14) -0.0083(14) C292 0.0576(19) 0.0329(18) 0.0423(18) 0.0124(14) 0.0129(15) -0.0072(14) C223 0.0385(16) 0.0412(18) 0.0262(15) -0.0006(13) 0.0107(13) 0.0054(13) C222 0.0344(16) 0.0387(18) 0.0509(19) -0.0061(14) 0.0221(14) 0.0028(13) C214 0.0418(17) 0.049(2) 0.0437(19) 0.0021(15) 0.0186(14) 0.0014(14) C273 0.0427(17) 0.0365(18) 0.0472(18) 0.0208(14) 0.0104(14) 0.0130(14) N21 0.0317(12) 0.0315(13) 0.0221(12) 0.0010(10) 0.0031(10) 0.0029(10) C29 0.0200(13) 0.0177(14) 0.0250(15) 0.0022(11) 0.0049(11) -0.0001(11) C28 0.0267(14) 0.0212(15) 0.0197(13) 0.0043(11) 0.0033(11) 0.0022(11) C241 0.0252(14) 0.0264(15) 0.0253(14) 0.0005(12) 0.0112(11) 0.0063(11) C291 0.0357(15) 0.0202(15) 0.0251(14) 0.0090(12) -0.0009(12) 0.0016(12) C27 0.0172(13) 0.0241(15) 0.0285(16) 0.0069(13) 0.0038(11) -0.0016(11) C271 0.0316(15) 0.0177(15) 0.0417(17) 0.0117(12) 0.0071(13) 0.0049(12) C239 0.0280(15) 0.0236(15) 0.0349(16) -0.0057(12) 0.0113(12) -0.0006(12) C24 0.0249(14) 0.0275(16) 0.0237(15) -0.0043(12) 0.0005(11) 0.0040(12) C244 0.0358(16) 0.0289(17) 0.0444(17) 0.0030(13) 0.0174(13) 0.0088(13) C221 0.0275(14) 0.0237(15) 0.0296(15) -0.0044(12) 0.0119(12) 0.0047(11) C243 0.0394(16) 0.0365(17) 0.0261(15) 0.0022(13) 0.0074(12) 0.0060(13) C293 0.0460(17) 0.0210(15) 0.0375(17) 0.0048(13) -0.0016(13) 0.0054(13) C274 0.0321(15) 0.0302(16) 0.0381(16) 0.0089(13) 0.0063(13) 0.0079(12) C242 0.0288(15) 0.0376(17) 0.0407(17) 0.0097(14) 0.0047(13) 0.0067(13) C272 0.0349(17) 0.0246(17) 0.075(2) 0.0149(15) 0.0017(15) 0.0014(13) C216 0.0508(19) 0.049(2) 0.0299(16) 0.0089(14) 0.0047(14) 0.0066(15) C294 0.0533(19) 0.0307(17) 0.0364(17) 0.0005(13) -0.0113(14) 0.0124(14) C217 0.0362(17) 0.056(2) 0.0320(16) 0.0065(15) 0.0000(13) 0.0056(15) C224 0.0403(17) 0.0411(18) 0.0397(17) 0.0070(14) 0.0142(14) 0.0155(14) C229 0.0226(14) 0.0310(17) 0.0242(14) 0.0015(12) 0.0051(11) 0.0031(12) Ti1 0.0229(2) 0.0189(3) 0.0206(3) 0.00331(19) 0.00168(19) 0.00267(19) O6 0.0234(9) 0.0219(10) 0.0206(9) 0.0037(7) 0.0037(7) 0.0061(7) O10 0.0240(9) 0.0214(10) 0.0245(9) 0.0065(8) 0.0040(7) 0.0054(7) O7 0.0312(10) 0.0360(11) 0.0220(10) 0.0099(8) 0.0063(8) 0.0124(8) O9 0.0251(9) 0.0264(10) 0.0353(10) 0.0086(8) 0.0126(8) 0.0090(8) O5 0.0280(9) 0.0180(9) 0.0209(10) 0.0029(8) -0.0001(7) -0.0001(7) O1 0.0268(9) 0.0215(10) 0.0159(9) 0.0017(8) 0.0009(7) 0.0008(7) O2 0.0402(10) 0.0245(10) 0.0179(9) 0.0051(8) 0.0078(8) 0.0071(8) O4 0.0390(10) 0.0146(10) 0.0317(10) 0.0041(8) 0.0002(8) -0.0007(8) N1 0.0253(12) 0.0236(12) 0.0234(11) 0.0035(9) -0.0024(9) 0.0022(9) N2 0.0218(11) 0.0241(12) 0.0230(11) 0.0052(9) 0.0002(9) 0.0029(9) C911 0.0386(16) 0.0302(17) 0.0513(19) 0.0071(14) 0.0241(14) 0.0092(13) C711 0.0353(16) 0.0389(18) 0.0375(17) 0.0104(14) 0.0090(13) 0.0055(13) C413 0.0509(19) 0.0421(19) 0.0410(18) 0.0132(15) 0.0040(15) -0.0100(15) C11 0.0423(16) 0.0230(15) 0.0329(16) 0.0049(12) 0.0046(13) 0.0030(13) C12 0.0392(17) 0.0242(16) 0.0474(18) 0.0012(13) -0.0047(14) -0.0020(13) C7 0.0246(14) 0.0202(14) 0.0216(14) 0.0039(11) -0.0012(11) 0.0008(11) C3 0.0270(14) 0.0175(14) 0.0244(14) -0.0015(11) 0.0039(11) 0.0025(11) C4 0.0189(13) 0.0196(15) 0.0288(16) 0.0026(12) -0.0006(11) 0.0031(11) C9 0.0209(14) 0.0164(14) 0.0293(15) -0.0015(12) 0.0037(11) -0.0014(11) C211 0.0400(16) 0.0247(15) 0.0272(15) 0.0054(12) 0.0093(12) 0.0088(12) C71 0.0306(15) 0.0319(16) 0.0193(14) 0.0075(12) 0.0081(12) 0.0118(12) C21 0.0378(16) 0.0251(15) 0.0272(15) 0.0096(12) 0.0114(12) 0.0068(12) C8 0.0211(13) 0.0245(15) 0.0251(14) 0.0064(11) 0.0007(11) 0.0052(11) C2 0.0192(13) 0.0330(16) 0.0178(14) 0.0057(12) 0.0043(11) 0.0070(11) C912 0.0344(16) 0.0317(17) 0.0557(19) 0.0167(14) 0.0179(14) 0.0071(13) C23 0.0275(15) 0.0364(17) 0.0412(17) 0.0089(14) 0.0026(13) 0.0079(13) C91 0.0274(14) 0.0291(16) 0.0317(15) 0.0071(12) 0.0127(12) 0.0058(12) C722 0.0509(18) 0.0350(18) 0.0288(16) 0.0022(13) 0.0047(13) 0.0108(14) C41 0.0376(16) 0.0190(15) 0.0399(17) 0.0119(13) -0.0105(13) -0.0014(12) C22 0.0390(16) 0.0338(17) 0.0366(17) 0.0030(13) 0.0117(13) 0.0086(13) C723 0.0502(18) 0.051(2) 0.0278(16) 0.0158(14) 0.0132(13) 0.0172(15) C412 0.056(2) 0.0222(17) 0.058(2) 0.0098(14) -0.0182(16) -0.0089(14) C913 0.0411(17) 0.064(2) 0.0317(17) -0.0013(15) 0.0127(14) 0.0083(15) C411 0.0500(19) 0.0294(18) 0.065(2) 0.0187(15) -0.0268(16) -0.0036(14) C213 0.071(2) 0.0410(19) 0.0293(16) 0.0134(14) 0.0213(15) 0.0166(15) C212 0.0361(17) 0.0454(19) 0.061(2) 0.0268(16) 0.0152(15) 0.0043(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti2 N21 1.906(2) . ? Ti2 N22 1.9122(19) . ? Ti2 O210 1.9949(16) . ? Ti2 O25 2.0031(17) . ? Ti2 O21 2.0977(16) . ? Ti2 O26 2.1001(16) . ? O26 C27 1.251(3) . ? O210 C29 1.272(3) . ? O27 C27 1.342(3) . ? O27 C271 1.473(3) . ? O29 C29 1.341(3) . ? O29 C291 1.473(3) . ? O21 C229 1.263(3) . ? O25 C24 1.277(3) . ? O22 C229 1.349(3) . ? O22 C221 1.477(3) . ? O24 C24 1.341(3) . ? O24 C241 1.478(3) . ? N22 C214 1.448(3) . ? N22 C215 1.455(3) . ? C215 H21A 0.9800 . ? C215 H21B 0.9800 . ? C215 H21C 0.9800 . ? C292 C291 1.520(3) . ? C292 H29A 0.9800 . ? C292 H29B 0.9800 . ? C292 H29C 0.9800 . ? C223 C221 1.513(3) . ? C223 H22A 0.9800 . ? C223 H22B 0.9800 . ? C223 H22C 0.9800 . ? C222 C221 1.517(3) . ? C222 H22D 0.9800 . ? C222 H22E 0.9800 . ? C222 H22F 0.9800 . ? C214 H21D 0.9800 . ? C214 H21E 0.9800 . ? C214 H21F 0.9800 . ? C273 C271 1.518(3) . ? C273 H27A 0.9800 . ? C273 H27B 0.9800 . ? C273 H27C 0.9800 . ? N21 C216 1.460(3) . ? N21 C217 1.461(3) . ? C29 C28 1.383(3) . ? C28 C27 1.399(3) . ? C28 H28 0.9500 . ? C241 C242 1.507(3) . ? C241 C244 1.514(3) . ? C241 C243 1.515(3) . ? C291 C294 1.511(3) . ? C291 C293 1.517(3) . ? C271 C272 1.515(3) . ? C271 C274 1.518(3) . ? C239 C229 1.386(3) . ? C239 C24 1.387(3) . ? C239 H23 0.9500 . ? C244 H24A 0.9800 . ? C244 H24B 0.9800 . ? C244 H24C 0.9800 . ? C221 C224 1.519(3) . ? C243 H24D 0.9800 . ? C243 H24E 0.9800 . ? C243 H24F 0.9800 . ? C293 H29D 0.9800 . ? C293 H29E 0.9800 . ? C293 H29F 0.9800 . ? C274 H27D 0.9800 . ? C274 H27E 0.9800 . ? C274 H27F 0.9800 . ? C242 H24G 0.9800 . ? C242 H24H 0.9800 . ? C242 H24I 0.9800 . ? C272 H27G 0.9800 . ? C272 H27H 0.9800 . ? C272 H27I 0.9800 . ? C216 H21G 0.9800 . ? C216 H21H 0.9800 . ? C216 H21I 0.9800 . ? C294 H29G 0.9800 . ? C294 H29H 0.9800 . ? C294 H29I 0.9800 . ? C217 H21J 0.9800 . ? C217 H21K 0.9800 . ? C217 H21L 0.9800 . ? C224 H22G 0.9800 . ? C224 H22H 0.9800 . ? C224 H22I 0.9800 . ? Ti1 N1 1.9037(19) . ? Ti1 N2 1.9066(19) . ? Ti1 O1 1.9936(15) . ? Ti1 O6 2.0054(15) . ? Ti1 O10 2.0981(16) . ? Ti1 O5 2.1093(16) . ? O6 C7 1.277(3) . ? O10 C9 1.256(3) . ? O7 C7 1.341(3) . ? O7 C71 1.477(3) . ? O9 C9 1.351(3) . ? O9 C91 1.471(3) . ? O5 C4 1.257(3) . ? O1 C2 1.272(3) . ? O2 C2 1.344(3) . ? O2 C21 1.476(3) . ? O4 C4 1.351(3) . ? O4 C41 1.471(3) . ? N1 C11 1.457(3) . ? N1 C12 1.462(3) . ? N2 C23 1.454(3) . ? N2 C22 1.455(3) . ? C911 C91 1.512(3) . ? C911 H19A 0.9800 . ? C911 H19B 0.9800 . ? C911 H19C 0.9800 . ? C711 C71 1.514(3) . ? C711 H17A 0.9800 . ? C711 H17B 0.9800 . ? C711 H17C 0.9800 . ? C413 C41 1.507(4) . ? C413 H14A 0.9800 . ? C413 H14B 0.9800 . ? C413 H14C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H11D 0.9800 . ? C12 H11E 0.9800 . ? C12 H11F 0.9800 . ? C7 C8 1.381(3) . ? C3 C4 1.382(3) . ? C3 C2 1.390(3) . ? C3 H13 0.9500 . ? C9 C8 1.396(3) . ? C211 C21 1.513(3) . ? C211 H12A 0.9800 . ? C211 H12B 0.9800 . ? C211 H12C 0.9800 . ? C71 C722 1.515(3) . ? C71 C723 1.521(3) . ? C21 C212 1.512(3) . ? C21 C213 1.513(3) . ? C8 H8A 0.9500 . ? C912 C91 1.521(3) . ? C912 H19D 0.9800 . ? C912 H19E 0.9800 . ? C912 H19F 0.9800 . ? C23 H11G 0.9800 . ? C23 H11H 0.9800 . ? C23 H11I 0.9800 . ? C91 C913 1.520(3) . ? C722 H17D 0.9800 . ? C722 H17E 0.9800 . ? C722 H17F 0.9800 . ? C41 C411 1.518(3) . ? C41 C412 1.520(3) . ? C22 H11J 0.9800 . ? C22 H11K 0.9800 . ? C22 H11L 0.9800 . ? C723 H17G 0.9800 . ? C723 H17H 0.9800 . ? C723 H17I 0.9800 . ? C412 H14D 0.9800 . ? C412 H14E 0.9800 . ? C412 H14F 0.9800 . ? C913 H19G 0.9800 . ? C913 H19H 0.9800 . ? C913 H19I 0.9800 . ? C411 H14G 0.9800 . ? C411 H14H 0.9800 . ? C411 H14I 0.9800 . ? C213 H12D 0.9800 . ? C213 H12E 0.9800 . ? C213 H12F 0.9800 . ? C212 H12G 0.9800 . ? C212 H12H 0.9800 . ? C212 H12I 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 N21 Ti2 N22 94.63(9) . . ? N21 Ti2 O210 95.60(8) . . ? N22 Ti2 O210 94.62(8) . . ? N21 Ti2 O25 94.16(8) . . ? N22 Ti2 O25 96.19(8) . . ? O210 Ti2 O25 164.78(6) . . ? N21 Ti2 O21 92.58(7) . . ? N22 Ti2 O21 172.73(8) . . ? O210 Ti2 O21 85.52(6) . . ? O25 Ti2 O21 82.41(6) . . ? N21 Ti2 O26 174.85(8) . . ? N22 Ti2 O26 90.43(7) . . ? O210 Ti2 O26 83.04(6) . . ? O25 Ti2 O26 86.21(6) . . ? O21 Ti2 O26 82.37(6) . . ? C27 O26 Ti2 130.40(16) . . ? C29 O210 Ti2 132.47(15) . . ? C27 O27 C271 122.39(19) . . ? C29 O29 C291 122.14(18) . . ? C229 O21 Ti2 130.79(15) . . ? C24 O25 Ti2 133.67(15) . . ? C229 O22 C221 121.75(18) . . ? C24 O24 C241 122.25(18) . . ? C214 N22 C215 111.4(2) . . ? C214 N22 Ti2 123.99(16) . . ? C215 N22 Ti2 124.02(16) . . ? N22 C215 H21A 109.5 . . ? N22 C215 H21B 109.5 . . ? H21A C215 H21B 109.5 . . ? N22 C215 H21C 109.5 . . ? H21A C215 H21C 109.5 . . ? H21B C215 H21C 109.5 . . ? C291 C292 H29A 109.5 . . ? C291 C292 H29B 109.5 . . ? H29A C292 H29B 109.5 . . ? C291 C292 H29C 109.5 . . ? H29A C292 H29C 109.5 . . ? H29B C292 H29C 109.5 . . ? C221 C223 H22A 109.5 . . ? C221 C223 H22B 109.5 . . ? H22A C223 H22B 109.5 . . ? C221 C223 H22C 109.5 . . ? H22A C223 H22C 109.5 . . ? H22B C223 H22C 109.5 . . ? C221 C222 H22D 109.5 . . ? C221 C222 H22E 109.5 . . ? H22D C222 H22E 109.5 . . ? C221 C222 H22F 109.5 . . ? H22D C222 H22F 109.5 . . ? H22E C222 H22F 109.5 . . ? N22 C214 H21D 109.5 . . ? N22 C214 H21E 109.5 . . ? H21D C214 H21E 109.5 . . ? N22 C214 H21F 109.5 . . ? H21D C214 H21F 109.5 . . ? H21E C214 H21F 109.5 . . ? C271 C273 H27A 109.5 . . ? C271 C273 H27B 109.5 . . ? H27A C273 H27B 109.5 . . ? C271 C273 H27C 109.5 . . ? H27A C273 H27C 109.5 . . ? H27B C273 H27C 109.5 . . ? C216 N21 C217 110.5(2) . . ? C216 N21 Ti2 124.23(16) . . ? C217 N21 Ti2 124.93(17) . . ? O210 C29 O29 119.8(2) . . ? O210 C29 C28 125.7(2) . . ? O29 C29 C28 114.5(2) . . ? C29 C28 C27 121.8(2) . . ? C29 C28 H28 119.1 . . ? C27 C28 H28 119.1 . . ? O24 C241 C242 110.53(19) . . ? O24 C241 C244 101.66(18) . . ? C242 C241 C244 111.1(2) . . ? O24 C241 C243 110.07(19) . . ? C242 C241 C243 112.8(2) . . ? C244 C241 C243 110.2(2) . . ? O29 C291 C294 110.65(19) . . ? O29 C291 C293 101.83(18) . . ? C294 C291 C293 110.9(2) . . ? O29 C291 C292 109.5(2) . . ? C294 C291 C292 113.2(2) . . ? C293 C291 C292 110.2(2) . . ? O26 C27 O27 121.4(2) . . ? O26 C27 C28 125.3(2) . . ? O27 C27 C28 113.3(2) . . ? O27 C271 C272 110.23(19) . . ? O27 C271 C274 110.13(18) . . ? C272 C271 C274 113.0(2) . . ? O27 C271 C273 102.07(19) . . ? C272 C271 C273 110.6(2) . . ? C274 C271 C273 110.3(2) . . ? C229 C239 C24 121.3(2) . . ? C229 C239 H23 119.4 . . ? C24 C239 H23 119.4 . . ? O25 C24 O24 119.4(2) . . ? O25 C24 C239 125.4(2) . . ? O24 C24 C239 115.2(2) . . ? C241 C244 H24A 109.5 . . ? C241 C244 H24B 109.5 . . ? H24A C244 H24B 109.5 . . ? C241 C244 H24C 109.5 . . ? H24A C244 H24C 109.5 . . ? H24B C244 H24C 109.5 . . ? O22 C221 C223 109.03(19) . . ? O22 C221 C222 101.85(18) . . ? C223 C221 C222 110.7(2) . . ? O22 C221 C224 111.79(19) . . ? C223 C221 C224 113.2(2) . . ? C222 C221 C224 109.7(2) . . ? C241 C243 H24D 109.5 . . ? C241 C243 H24E 109.5 . . ? H24D C243 H24E 109.5 . . ? C241 C243 H24F 109.5 . . ? H24D C243 H24F 109.5 . . ? H24E C243 H24F 109.5 . . ? C291 C293 H29D 109.5 . . ? C291 C293 H29E 109.5 . . ? H29D C293 H29E 109.5 . . ? C291 C293 H29F 109.5 . . ? H29D C293 H29F 109.5 . . ? H29E C293 H29F 109.5 . . ? C271 C274 H27D 109.5 . . ? C271 C274 H27E 109.5 . . ? H27D C274 H27E 109.5 . . ? C271 C274 H27F 109.5 . . ? H27D C274 H27F 109.5 . . ? H27E C274 H27F 109.5 . . ? C241 C242 H24G 109.5 . . ? C241 C242 H24H 109.5 . . ? H24G C242 H24H 109.5 . . ? C241 C242 H24I 109.5 . . ? H24G C242 H24I 109.5 . . ? H24H C242 H24I 109.5 . . ? C271 C272 H27G 109.5 . . ? C271 C272 H27H 109.5 . . ? H27G C272 H27H 109.5 . . ? C271 C272 H27I 109.5 . . ? H27G C272 H27I 109.5 . . ? H27H C272 H27I 109.5 . . ? N21 C216 H21G 109.5 . . ? N21 C216 H21H 109.5 . . ? H21G C216 H21H 109.5 . . ? N21 C216 H21I 109.5 . . ? H21G C216 H21I 109.5 . . ? H21H C216 H21I 109.5 . . ? C291 C294 H29G 109.5 . . ? C291 C294 H29H 109.5 . . ? H29G C294 H29H 109.5 . . ? C291 C294 H29I 109.5 . . ? H29G C294 H29I 109.5 . . ? H29H C294 H29I 109.5 . . ? N21 C217 H21J 109.5 . . ? N21 C217 H21K 109.5 . . ? H21J C217 H21K 109.5 . . ? N21 C217 H21L 109.5 . . ? H21J C217 H21L 109.5 . . ? H21K C217 H21L 109.5 . . ? C221 C224 H22G 109.5 . . ? C221 C224 H22H 109.5 . . ? H22G C224 H22H 109.5 . . ? C221 C224 H22I 109.5 . . ? H22G C224 H22I 109.5 . . ? H22H C224 H22I 109.5 . . ? O21 C229 O22 119.8(2) . . ? O21 C229 C239 126.1(2) . . ? O22 C229 C239 114.1(2) . . ? N1 Ti1 N2 95.15(8) . . ? N1 Ti1 O1 95.65(7) . . ? N2 Ti1 O1 94.39(7) . . ? N1 Ti1 O6 95.30(7) . . ? N2 Ti1 O6 95.79(7) . . ? O1 Ti1 O6 164.30(7) . . ? N1 Ti1 O10 90.85(7) . . ? N2 Ti1 O10 173.91(7) . . ? O1 Ti1 O10 86.06(6) . . ? O6 Ti1 O10 82.57(6) . . ? N1 Ti1 O5 173.34(8) . . ? N2 Ti1 O5 91.41(7) . . ? O1 Ti1 O5 82.67(6) . . ? O6 Ti1 O5 85.16(6) . . ? O10 Ti1 O5 82.62(6) . . ? C7 O6 Ti1 132.16(15) . . ? C9 O10 Ti1 128.99(15) . . ? C7 O7 C71 121.77(18) . . ? C9 O9 C91 121.95(18) . . ? C4 O5 Ti1 130.15(15) . . ? C2 O1 Ti1 133.80(15) . . ? C2 O2 C21 122.02(18) . . ? C4 O4 C41 122.66(18) . . ? C11 N1 C12 110.16(19) . . ? C11 N1 Ti1 124.81(15) . . ? C12 N1 Ti1 124.33(16) . . ? C23 N2 C22 110.95(19) . . ? C23 N2 Ti1 124.50(16) . . ? C22 N2 Ti1 124.10(15) . . ? C91 C911 H19A 109.5 . . ? C91 C911 H19B 109.5 . . ? H19A C911 H19B 109.5 . . ? C91 C911 H19C 109.5 . . ? H19A C911 H19C 109.5 . . ? H19B C911 H19C 109.5 . . ? C71 C711 H17A 109.5 . . ? C71 C711 H17B 109.5 . . ? H17A C711 H17B 109.5 . . ? C71 C711 H17C 109.5 . . ? H17A C711 H17C 109.5 . . ? H17B C711 H17C 109.5 . . ? C41 C413 H14A 109.5 . . ? C41 C413 H14B 109.5 . . ? H14A C413 H14B 109.5 . . ? C41 C413 H14C 109.5 . . ? H14A C413 H14C 109.5 . . ? H14B C413 H14C 109.5 . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H11D 109.5 . . ? N1 C12 H11E 109.5 . . ? H11D C12 H11E 109.5 . . ? N1 C12 H11F 109.5 . . ? H11D C12 H11F 109.5 . . ? H11E C12 H11F 109.5 . . ? O6 C7 O7 119.5(2) . . ? O6 C7 C8 125.7(2) . . ? O7 C7 C8 114.8(2) . . ? C4 C3 C2 121.7(2) . . ? C4 C3 H13 119.1 . . ? C2 C3 H13 119.1 . . ? O5 C4 O4 120.3(2) . . ? O5 C4 C3 126.2(2) . . ? O4 C4 C3 113.5(2) . . ? O10 C9 O9 120.5(2) . . ? O10 C9 C8 126.2(2) . . ? O9 C9 C8 113.3(2) . . ? C21 C211 H12A 109.5 . . ? C21 C211 H12B 109.5 . . ? H12A C211 H12B 109.5 . . ? C21 C211 H12C 109.5 . . ? H12A C211 H12C 109.5 . . ? H12B C211 H12C 109.5 . . ? O7 C71 C711 110.55(19) . . ? O7 C71 C722 110.50(19) . . ? C711 C71 C722 113.2(2) . . ? O7 C71 C723 101.72(18) . . ? C711 C71 C723 110.0(2) . . ? C722 C71 C723 110.3(2) . . ? O2 C21 C212 109.8(2) . . ? O2 C21 C211 110.47(19) . . ? C212 C21 C211 113.7(2) . . ? O2 C21 C213 102.00(19) . . ? C212 C21 C213 110.9(2) . . ? C211 C21 C213 109.4(2) . . ? C7 C8 C9 121.1(2) . . ? C7 C8 H8A 119.4 . . ? C9 C8 H8A 119.4 . . ? O1 C2 O2 119.1(2) . . ? O1 C2 C3 125.3(2) . . ? O2 C2 C3 115.6(2) . . ? C91 C912 H19D 109.5 . . ? C91 C912 H19E 109.5 . . ? H19D C912 H19E 109.5 . . ? C91 C912 H19F 109.5 . . ? H19D C912 H19F 109.5 . . ? H19E C912 H19F 109.5 . . ? N2 C23 H11G 109.5 . . ? N2 C23 H11H 109.5 . . ? H11G C23 H11H 109.5 . . ? N2 C23 H11I 109.5 . . ? H11G C23 H11I 109.5 . . ? H11H C23 H11I 109.5 . . ? O9 C91 C911 101.98(19) . . ? O9 C91 C913 111.76(19) . . ? C911 C91 C913 110.5(2) . . ? O9 C91 C912 108.7(2) . . ? C911 C91 C912 111.0(2) . . ? C913 C91 C912 112.5(2) . . ? C71 C722 H17D 109.5 . . ? C71 C722 H17E 109.5 . . ? H17D C722 H17E 109.5 . . ? C71 C722 H17F 109.5 . . ? H17D C722 H17F 109.5 . . ? H17E C722 H17F 109.5 . . ? O4 C41 C413 110.4(2) . . ? O4 C41 C411 110.4(2) . . ? C413 C41 C411 112.7(2) . . ? O4 C41 C412 101.5(2) . . ? C413 C41 C412 111.0(2) . . ? C411 C41 C412 110.2(2) . . ? N2 C22 H11J 109.5 . . ? N2 C22 H11K 109.5 . . ? H11J C22 H11K 109.5 . . ? N2 C22 H11L 109.5 . . ? H11J C22 H11L 109.5 . . ? H11K C22 H11L 109.5 . . ? C71 C723 H17G 109.5 . . ? C71 C723 H17H 109.5 . . ? H17G C723 H17H 109.5 . . ? C71 C723 H17I 109.5 . . ? H17G C723 H17I 109.5 . . ? H17H C723 H17I 109.5 . . ? C41 C412 H14D 109.5 . . ? C41 C412 H14E 109.5 . . ? H14D C412 H14E 109.5 . . ? C41 C412 H14F 109.5 . . ? H14D C412 H14F 109.5 . . ? H14E C412 H14F 109.5 . . ? C91 C913 H19G 109.5 . . ? C91 C913 H19H 109.5 . . ? H19G C913 H19H 109.5 . . ? C91 C913 H19I 109.5 . . ? H19G C913 H19I 109.5 . . ? H19H C913 H19I 109.5 . . ? C41 C411 H14G 109.5 . . ? C41 C411 H14H 109.5 . . ? H14G C411 H14H 109.5 . . ? C41 C411 H14I 109.5 . . ? H14G C411 H14I 109.5 . . ? H14H C411 H14I 109.5 . . ? C21 C213 H12D 109.5 . . ? C21 C213 H12E 109.5 . . ? H12D C213 H12E 109.5 . . ? C21 C213 H12F 109.5 . . ? H12D C213 H12F 109.5 . . ? H12E C213 H12F 109.5 . . ? C21 C212 H12G 109.5 . . ? C21 C212 H12H 109.5 . . ? H12G C212 H12H 109.5 . . ? C21 C212 H12I 109.5 . . ? H12G C212 H12I 109.5 . . ? H12H C212 H12I 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 N21 Ti2 O26 C27 65.7(9) . . . . ? N22 Ti2 O26 C27 -103.84(19) . . . . ? O210 Ti2 O26 C27 -9.23(18) . . . . ? O25 Ti2 O26 C27 159.98(19) . . . . ? O21 Ti2 O26 C27 77.15(19) . . . . ? N21 Ti2 O210 C29 -162.77(19) . . . . ? N22 Ti2 O210 C29 102.1(2) . . . . ? O25 Ti2 O210 C29 -33.1(4) . . . . ? O21 Ti2 O210 C29 -70.60(19) . . . . ? O26 Ti2 O210 C29 12.24(19) . . . . ? N21 Ti2 O21 C229 -97.5(2) . . . . ? N22 Ti2 O21 C229 75.7(7) . . . . ? O210 Ti2 O21 C229 167.1(2) . . . . ? O25 Ti2 O21 C229 -3.7(2) . . . . ? O26 Ti2 O21 C229 83.5(2) . . . . ? N21 Ti2 O25 C24 98.2(2) . . . . ? N22 Ti2 O25 C24 -166.7(2) . . . . ? O210 Ti2 O25 C24 -31.6(4) . . . . ? O21 Ti2 O25 C24 6.1(2) . . . . ? O26 Ti2 O25 C24 -76.7(2) . . . . ? N21 Ti2 N22 C214 46.0(2) . . . . ? O210 Ti2 N22 C214 142.0(2) . . . . ? O25 Ti2 N22 C214 -48.7(2) . . . . ? O21 Ti2 N22 C214 -127.2(6) . . . . ? O26 Ti2 N22 C214 -134.9(2) . . . . ? N21 Ti2 N22 C215 -143.8(2) . . . . ? O210 Ti2 N22 C215 -47.7(2) . . . . ? O25 Ti2 N22 C215 121.5(2) . . . . ? O21 Ti2 N22 C215 43.1(7) . . . . ? O26 Ti2 N22 C215 35.3(2) . . . . ? N22 Ti2 N21 C216 45.8(2) . . . . ? O210 Ti2 N21 C216 -49.3(2) . . . . ? O25 Ti2 N21 C216 142.4(2) . . . . ? O21 Ti2 N21 C216 -135.0(2) . . . . ? O26 Ti2 N21 C216 -123.7(8) . . . . ? N22 Ti2 N21 C217 -141.3(2) . . . . ? O210 Ti2 N21 C217 123.6(2) . . . . ? O25 Ti2 N21 C217 -44.7(2) . . . . ? O21 Ti2 N21 C217 37.8(2) . . . . ? O26 Ti2 N21 C217 49.2(10) . . . . ? Ti2 O210 C29 O29 170.20(13) . . . . ? Ti2 O210 C29 C28 -10.2(3) . . . . ? C291 O29 C29 O210 13.9(3) . . . . ? C291 O29 C29 C28 -165.75(19) . . . . ? O210 C29 C28 C27 -0.5(4) . . . . ? O29 C29 C28 C27 179.07(19) . . . . ? C24 O24 C241 C242 -64.5(3) . . . . ? C24 O24 C241 C244 177.5(2) . . . . ? C24 O24 C241 C243 60.7(3) . . . . ? C29 O29 C291 C294 -68.2(3) . . . . ? C29 O29 C291 C293 173.94(19) . . . . ? C29 O29 C291 C292 57.3(3) . . . . ? Ti2 O26 C27 O27 -176.80(13) . . . . ? Ti2 O26 C27 C28 4.1(3) . . . . ? C271 O27 C27 O26 1.3(3) . . . . ? C271 O27 C27 C28 -179.53(18) . . . . ? C29 C28 C27 O26 3.3(3) . . . . ? C29 C28 C27 O27 -175.9(2) . . . . ? C27 O27 C271 C272 62.2(3) . . . . ? C27 O27 C271 C274 -63.2(3) . . . . ? C27 O27 C271 C273 179.64(19) . . . . ? Ti2 O25 C24 O24 174.27(14) . . . . ? Ti2 O25 C24 C239 -6.5(4) . . . . ? C241 O24 C24 O25 1.6(3) . . . . ? C241 O24 C24 C239 -177.7(2) . . . . ? C229 C239 C24 O25 1.8(4) . . . . ? C229 C239 C24 O24 -178.9(2) . . . . ? C229 O22 C221 C223 60.8(3) . . . . ? C229 O22 C221 C222 177.8(2) . . . . ? C229 O22 C221 C224 -65.2(3) . . . . ? Ti2 O21 C229 O22 179.58(14) . . . . ? Ti2 O21 C229 C239 1.6(4) . . . . ? C221 O22 C229 O21 15.6(3) . . . . ? C221 O22 C229 C239 -166.2(2) . . . . ? C24 C239 C229 O21 0.5(4) . . . . ? C24 C239 C229 O22 -177.6(2) . . . . ? N1 Ti1 O6 C7 -107.0(2) . . . . ? N2 Ti1 O6 C7 157.2(2) . . . . ? O1 Ti1 O6 C7 27.1(4) . . . . ? O10 Ti1 O6 C7 -16.88(19) . . . . ? O5 Ti1 O6 C7 66.3(2) . . . . ? N1 Ti1 O10 C9 113.81(19) . . . . ? N2 Ti1 O10 C9 -56.2(8) . . . . ? O1 Ti1 O10 C9 -150.58(19) . . . . ? O6 Ti1 O10 C9 18.57(19) . . . . ? O5 Ti1 O10 C9 -67.48(19) . . . . ? N1 Ti1 O5 C4 -71.0(7) . . . . ? N2 Ti1 O5 C4 98.95(19) . . . . ? O1 Ti1 O5 C4 4.71(19) . . . . ? O6 Ti1 O5 C4 -165.36(19) . . . . ? O10 Ti1 O5 C4 -82.24(19) . . . . ? N1 Ti1 O1 C2 169.3(2) . . . . ? N2 Ti1 O1 C2 -95.1(2) . . . . ? O6 Ti1 O1 C2 35.2(3) . . . . ? O10 Ti1 O1 C2 78.8(2) . . . . ? O5 Ti1 O1 C2 -4.26(19) . . . . ? N2 Ti1 N1 C11 -44.75(19) . . . . ? O1 Ti1 N1 C11 50.18(19) . . . . ? O6 Ti1 N1 C11 -141.07(18) . . . . ? O10 Ti1 N1 C11 136.30(19) . . . . ? O5 Ti1 N1 C11 125.2(6) . . . . ? N2 Ti1 N1 C12 145.79(19) . . . . ? O1 Ti1 N1 C12 -119.27(19) . . . . ? O6 Ti1 N1 C12 49.47(19) . . . . ? O10 Ti1 N1 C12 -33.15(19) . . . . ? O5 Ti1 N1 C12 -44.2(7) . . . . ? N1 Ti1 N2 C23 144.75(18) . . . . ? O1 Ti1 N2 C23 48.66(18) . . . . ? O6 Ti1 N2 C23 -119.37(18) . . . . ? O10 Ti1 N2 C23 -45.3(8) . . . . ? O5 Ti1 N2 C23 -34.09(18) . . . . ? N1 Ti1 N2 C22 -43.61(19) . . . . ? O1 Ti1 N2 C22 -139.70(18) . . . . ? O6 Ti1 N2 C22 52.27(19) . . . . ? O10 Ti1 N2 C22 126.4(7) . . . . ? O5 Ti1 N2 C22 137.55(18) . . . . ? Ti1 O6 C7 O7 -169.79(13) . . . . ? Ti1 O6 C7 C8 11.4(4) . . . . ? C71 O7 C7 O6 3.3(3) . . . . ? C71 O7 C7 C8 -177.7(2) . . . . ? Ti1 O5 C4 O4 177.56(13) . . . . ? Ti1 O5 C4 C3 -3.7(3) . . . . ? C41 O4 C4 O5 2.9(3) . . . . ? C41 O4 C4 C3 -175.9(2) . . . . ? C2 C3 C4 O5 0.0(4) . . . . ? C2 C3 C4 O4 178.8(2) . . . . ? Ti1 O10 C9 O9 165.36(14) . . . . ? Ti1 O10 C9 C8 -15.4(3) . . . . ? C91 O9 C9 O10 7.1(3) . . . . ? C91 O9 C9 C8 -172.29(19) . . . . ? C7 O7 C71 C711 61.6(3) . . . . ? C7 O7 C71 C722 -64.5(3) . . . . ? C7 O7 C71 C723 178.4(2) . . . . ? C2 O2 C21 C212 65.2(3) . . . . ? C2 O2 C21 C211 -60.9(3) . . . . ? C2 O2 C21 C213 -177.1(2) . . . . ? O6 C7 C8 C9 1.1(4) . . . . ? O7 C7 C8 C9 -177.7(2) . . . . ? O10 C9 C8 C7 1.5(4) . . . . ? O9 C9 C8 C7 -179.2(2) . . . . ? Ti1 O1 C2 O2 -178.84(13) . . . . ? Ti1 O1 C2 C3 2.7(3) . . . . ? C21 O2 C2 O1 -0.1(3) . . . . ? C21 O2 C2 C3 178.5(2) . . . . ? C4 C3 C2 O1 0.7(4) . . . . ? C4 C3 C2 O2 -177.8(2) . . . . ? C9 O9 C91 C911 -176.4(2) . . . . ? C9 O9 C91 C913 -58.3(3) . . . . ? C9 O9 C91 C912 66.4(3) . . . . ? C4 O4 C41 C413 60.9(3) . . . . ? C4 O4 C41 C411 -64.4(3) . . . . ? C4 O4 C41 C412 178.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.328 _refine_diff_density_min -0.237 _refine_diff_density_rms 0.049 # Attachment 'Compound 4.cif' data_cvd7 _database_code_depnum_ccdc_archive 'CCDC 297833' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H58 N2 O8 Ti' _chemical_formula_weight 622.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.217(2) _cell_length_b 16.078(2) _cell_length_c 17.156(4) _cell_angle_alpha 83.955(15) _cell_angle_beta 86.138(15) _cell_angle_gamma 85.097(12) _cell_volume 3605.9(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1500 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 27.50 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.147 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 0.282 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '1109 images at 1.0 deg. in \w and 15 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28009 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0840 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 25.05 _reflns_number_total 12725 _reflns_number_gt 8006 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0361P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12725 _refine_ls_number_parameters 849 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0851 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.0920 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 0.893 _refine_ls_restrained_S_all 0.904 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.21776(3) 0.26705(3) 0.50547(3) 0.01870(11) Uani 1 1 d . . . O6 O 0.27999(11) 0.20986(9) 0.60333(9) 0.0192(4) Uani 1 1 d . . . C7 C 0.37247(18) 0.18598(13) 0.61758(14) 0.0194(5) Uani 1 1 d . . . O7 O 0.39468(12) 0.14520(9) 0.68772(9) 0.0248(4) Uani 1 1 d . . . C21 C 0.31913(19) 0.11325(15) 0.74714(14) 0.0278(6) Uani 1 1 d . . . C113 C 0.2527(2) 0.18541(17) 0.77838(15) 0.0411(8) Uani 1 1 d . . . H11A H 0.2958 0.2264 0.7946 0.062 Uiso 1 1 calc R . . H11B H 0.2097 0.1641 0.8236 0.062 Uiso 1 1 calc R . . H11C H 0.2096 0.2124 0.7372 0.062 Uiso 1 1 calc R . . C212 C 0.2599(2) 0.05062(16) 0.71298(17) 0.0440(8) Uani 1 1 d . . . H11D H 0.2202 0.0794 0.6704 0.066 Uiso 1 1 calc R . . H11E H 0.2138 0.0251 0.7541 0.066 Uiso 1 1 calc R . . H11F H 0.3073 0.0069 0.6923 0.066 Uiso 1 1 calc R . . C213 C 0.3864(2) 0.06976(16) 0.81063(15) 0.0366(7) Uani 1 1 d . . . H11G H 0.4322 0.0258 0.7886 0.055 Uiso 1 1 calc R . . H11H H 0.3437 0.0446 0.8542 0.055 Uiso 1 1 calc R . . H11I H 0.4267 0.1110 0.8299 0.055 Uiso 1 1 calc R . . C8 C 0.45667(18) 0.19829(14) 0.56781(14) 0.0220(6) Uani 1 1 d . . . H12 H 0.5216 0.1768 0.5849 0.026 Uiso 1 1 calc R . . C9 C 0.45037(18) 0.24141(14) 0.49269(14) 0.0204(6) Uani 1 1 d . . . O9 O 0.54096(12) 0.24639(10) 0.45312(9) 0.0259(4) Uani 1 1 d . . . C41 C 0.5510(2) 0.28747(17) 0.37227(15) 0.0318(7) Uani 1 1 d . . . C412 C 0.66455(19) 0.27181(19) 0.35343(16) 0.0454(8) Uani 1 1 d . . . H13A H 0.7019 0.2992 0.3897 0.068 Uiso 1 1 calc R . . H13B H 0.6814 0.2948 0.2994 0.068 Uiso 1 1 calc R . . H13C H 0.6836 0.2113 0.3591 0.068 Uiso 1 1 calc R . . C411 C 0.5199(2) 0.38011(17) 0.37225(18) 0.0494(9) Uani 1 1 d . . . H13D H 0.4468 0.3882 0.3860 0.074 Uiso 1 1 calc R . . H13E H 0.5350 0.4086 0.3199 0.074 Uiso 1 1 calc R . . H13F H 0.5577 0.4036 0.4108 0.074 Uiso 1 1 calc R . . C413 C 0.4914(2) 0.24553(19) 0.31787(16) 0.0475(8) Uani 1 1 d . . . H13G H 0.5064 0.1846 0.3261 0.071 Uiso 1 1 calc R . . H13H H 0.5104 0.2654 0.2633 0.071 Uiso 1 1 calc R . . H13I H 0.4185 0.2593 0.3288 0.071 Uiso 1 1 calc R . . O10 O 0.36997(11) 0.27421(9) 0.46314(9) 0.0193(4) Uani 1 1 d . . . O1 O 0.18746(11) 0.30401(9) 0.39304(9) 0.0203(4) Uani 1 1 d . . . C2 C 0.19267(17) 0.26500(14) 0.33173(14) 0.0201(5) Uani 1 1 d . . . O2 O 0.17307(12) 0.30733(9) 0.26175(9) 0.0239(4) Uani 1 1 d . . . C91 C 0.1580(2) 0.39958(14) 0.24945(15) 0.0260(6) Uani 1 1 d . . . C912 C 0.0637(2) 0.43090(15) 0.29646(16) 0.0349(7) Uani 1 1 d . . . H16A H 0.0053 0.4023 0.2836 0.052 Uiso 1 1 calc R . . H16B H 0.0506 0.4915 0.2835 0.052 Uiso 1 1 calc R . . H16C H 0.0742 0.4191 0.3527 0.052 Uiso 1 1 calc R . . C913 C 0.1427(2) 0.41466(15) 0.16185(15) 0.0340(7) Uani 1 1 d . . . H16D H 0.2029 0.3914 0.1326 0.051 Uiso 1 1 calc R . . H16E H 0.1323 0.4751 0.1465 0.051 Uiso 1 1 calc R . . H16F H 0.0829 0.3872 0.1500 0.051 Uiso 1 1 calc R . . C911 C 0.2542(2) 0.43665(16) 0.26886(16) 0.0376(7) Uani 1 1 d . . . H16G H 0.2641 0.4246 0.3251 0.056 Uiso 1 1 calc R . . H16H H 0.2478 0.4975 0.2551 0.056 Uiso 1 1 calc R . . H16I H 0.3128 0.4118 0.2389 0.056 Uiso 1 1 calc R . . C3 C 0.21421(17) 0.17958(14) 0.32888(14) 0.0203(6) Uani 1 1 d . . . H17 H 0.2151 0.1567 0.2800 0.024 Uiso 1 1 calc R . . C4 C 0.23474(17) 0.12626(14) 0.39704(14) 0.0203(6) Uani 1 1 d . . . O4 O 0.24857(12) 0.04492(9) 0.38385(9) 0.0233(4) Uani 1 1 d . . . C71 C 0.26961(19) -0.02132(14) 0.44818(14) 0.0251(6) Uani 1 1 d . . . C722 C 0.1819(2) -0.02318(15) 0.50913(16) 0.0418(8) Uani 1 1 d . . . H18A H 0.1799 0.0264 0.5381 0.063 Uiso 1 1 calc R . . H18B H 0.1907 -0.0740 0.5457 0.063 Uiso 1 1 calc R . . H18C H 0.1180 -0.0231 0.4832 0.063 Uiso 1 1 calc R . . C711 C 0.2758(2) -0.09996(14) 0.40481(16) 0.0311(7) Uani 1 1 d . . . H18D H 0.2112 -0.1035 0.3809 0.047 Uiso 1 1 calc R . . H18E H 0.2891 -0.1497 0.4420 0.047 Uiso 1 1 calc R . . H18F H 0.3310 -0.0972 0.3637 0.047 Uiso 1 1 calc R . . C723 C 0.3705(2) -0.01116(15) 0.48191(16) 0.0333(7) Uani 1 1 d . . . H18G H 0.4231 -0.0046 0.4391 0.050 Uiso 1 1 calc R . . H18H H 0.3895 -0.0610 0.5175 0.050 Uiso 1 1 calc R . . H18I H 0.3642 0.0386 0.5109 0.050 Uiso 1 1 calc R . . O5 O 0.23891(11) 0.14789(9) 0.46462(9) 0.0192(4) Uani 1 1 d . . . N1 N 0.21377(14) 0.37685(11) 0.53915(11) 0.0201(5) Uani 1 1 d . . . C12 C 0.13069(18) 0.44106(14) 0.52263(15) 0.0272(6) Uani 1 1 d . . . H1A H 0.0987 0.4579 0.5730 0.033 Uiso 1 1 calc R . . H1B H 0.0785 0.4164 0.4954 0.033 Uiso 1 1 calc R . . C14 C 0.1640(2) 0.51940(15) 0.47233(17) 0.0396(7) Uani 1 1 d . . . H2A H 0.2060 0.5500 0.5027 0.059 Uiso 1 1 calc R . . H2B H 0.1038 0.5556 0.4567 0.059 Uiso 1 1 calc R . . H2C H 0.2037 0.5028 0.4253 0.059 Uiso 1 1 calc R . . C11 C 0.29788(19) 0.40734(15) 0.57737(15) 0.0270(6) Uani 1 1 d . . . H3A H 0.3270 0.4534 0.5424 0.032 Uiso 1 1 calc R . . H3B H 0.3520 0.3613 0.5851 0.032 Uiso 1 1 calc R . . C13 C 0.2644(2) 0.43875(18) 0.65610(17) 0.0478(8) Uani 1 1 d . . . H4A H 0.2155 0.4878 0.6483 0.072 Uiso 1 1 calc R . . H4B H 0.3237 0.4544 0.6809 0.072 Uiso 1 1 calc R . . H4C H 0.2323 0.3943 0.6900 0.072 Uiso 1 1 calc R . . N2 N 0.07962(14) 0.24772(11) 0.53742(11) 0.0214(5) Uani 1 1 d . . . C24 C 0.03462(19) 0.26302(15) 0.61506(15) 0.0291(6) Uani 1 1 d . . . H5A H -0.0251 0.3042 0.6089 0.035 Uiso 1 1 calc R . . H5B H 0.0848 0.2883 0.6438 0.035 Uiso 1 1 calc R . . C15 C 0.0012(2) 0.18404(16) 0.66400(16) 0.0397(7) Uani 1 1 d . . . H6A H -0.0582 0.1652 0.6418 0.060 Uiso 1 1 calc R . . H6B H -0.0164 0.1965 0.7182 0.060 Uiso 1 1 calc R . . H6C H 0.0570 0.1397 0.6635 0.060 Uiso 1 1 calc R . . C22 C 0.01226(18) 0.20885(15) 0.48956(15) 0.0266(6) Uani 1 1 d . . . H7A H -0.0061 0.1548 0.5178 0.032 Uiso 1 1 calc R . . H7B H 0.0500 0.1965 0.4397 0.032 Uiso 1 1 calc R . . C16 C -0.08461(19) 0.26266(16) 0.47065(16) 0.0366(7) Uani 1 1 d . . . H8A H -0.1244 0.2727 0.5195 0.055 Uiso 1 1 calc R . . H8B H -0.1247 0.2336 0.4375 0.055 Uiso 1 1 calc R . . H8C H -0.0673 0.3164 0.4427 0.055 Uiso 1 1 calc R . . Ti2 Ti 0.21910(3) 0.76080(3) 0.02230(3) 0.02377(12) Uani 1 1 d . A . O20 O 0.29009(12) 0.70570(9) 0.11715(9) 0.0207(4) Uani 1 1 d . . . C219 C 0.33538(17) 0.63298(15) 0.13208(14) 0.0200(6) Uani 1 1 d . . . O211 O 0.37652(12) 0.61255(9) 0.20200(9) 0.0244(4) Uani 1 1 d . . . C217 C 0.37882(19) 0.67152(14) 0.26206(14) 0.0247(6) Uani 1 1 d . . . C218 C 0.4313(2) 0.61629(16) 0.32762(15) 0.0392(7) Uani 1 1 d . . . H21A H 0.3886 0.5709 0.3476 0.059 Uiso 1 1 calc R . . H21B H 0.4417 0.6501 0.3703 0.059 Uiso 1 1 calc R . . H21C H 0.4972 0.5924 0.3071 0.059 Uiso 1 1 calc R . . C214 C 0.4426(2) 0.74273(16) 0.22987(16) 0.0381(7) Uani 1 1 d . . . H21D H 0.5087 0.7197 0.2090 0.057 Uiso 1 1 calc R . . H21E H 0.4528 0.7773 0.2720 0.057 Uiso 1 1 calc R . . H21F H 0.4075 0.7773 0.1878 0.057 Uiso 1 1 calc R . . C215 C 0.27227(19) 0.70074(15) 0.29013(15) 0.0311(6) Uani 1 1 d . . . H21G H 0.2395 0.7367 0.2478 0.047 Uiso 1 1 calc R . . H21H H 0.2752 0.7325 0.3355 0.047 Uiso 1 1 calc R . . H21I H 0.2330 0.6520 0.3053 0.047 Uiso 1 1 calc R . . C220 C 0.34535(19) 0.56920(15) 0.08337(14) 0.0249(6) Uani 1 1 d . . . H22 H 0.3840 0.5184 0.0991 0.030 Uiso 1 1 calc R . . C23 C 0.29967(19) 0.57799(16) 0.01132(15) 0.0248(6) Uani 1 1 d . . . O231 O 0.31480(14) 0.50835(10) -0.02681(10) 0.0326(4) Uani 1 1 d . . . C232 C 0.2785(2) 0.50563(17) -0.10507(15) 0.0419(8) Uani 1 1 d . . . C233 C 0.1649(3) 0.51560(19) -0.1031(2) 0.0640(10) Uani 1 1 d . . . H23A H 0.1370 0.4778 -0.0600 0.096 Uiso 1 1 calc R . . H23B H 0.1418 0.5018 -0.1530 0.096 Uiso 1 1 calc R . . H23C H 0.1413 0.5737 -0.0952 0.096 Uiso 1 1 calc R . . C234 C 0.3276(3) 0.57072(18) -0.16315(17) 0.0688(11) Uani 1 1 d . . . H23D H 0.3022 0.6271 -0.1506 0.103 Uiso 1 1 calc R . . H23E H 0.3105 0.5631 -0.2165 0.103 Uiso 1 1 calc R . . H23F H 0.4016 0.5639 -0.1598 0.103 Uiso 1 1 calc R . . C235 C 0.3181(3) 0.41752(17) -0.12353(17) 0.0628(11) Uani 1 1 d . . . H23G H 0.3922 0.4111 -0.1207 0.094 Uiso 1 1 calc R . . H23H H 0.3003 0.4088 -0.1765 0.094 Uiso 1 1 calc R . . H23I H 0.2872 0.3761 -0.0852 0.094 Uiso 1 1 calc R . . O24 O 0.24817(12) 0.64136(10) -0.01764(9) 0.0258(4) Uani 1 1 d . . . O25 O 0.36640(12) 0.77461(10) -0.02953(9) 0.0282(4) Uani 1 1 d . . . C26 C 0.39267(18) 0.80834(14) -0.09627(14) 0.0214(6) Uani 1 1 d . . . O261 O 0.49094(12) 0.81835(10) -0.11645(9) 0.0254(4) Uani 1 1 d . . . C262 C 0.57373(19) 0.77535(16) -0.07047(15) 0.0301(6) Uani 1 1 d . . . C263 C 0.6670(2) 0.80147(18) -0.12042(16) 0.0417(8) Uani 1 1 d . . . H26A H 0.6654 0.7825 -0.1727 0.062 Uiso 1 1 calc R . . H26B H 0.7285 0.7761 -0.0956 0.062 Uiso 1 1 calc R . . H26C H 0.6675 0.8627 -0.1251 0.062 Uiso 1 1 calc R . . C264 C 0.5725(2) 0.80640(19) 0.00950(16) 0.0466(8) Uani 1 1 d . . . H26D H 0.5627 0.8678 0.0043 0.070 Uiso 1 1 calc R . . H26E H 0.6372 0.7884 0.0331 0.070 Uiso 1 1 calc R . . H26F H 0.5166 0.7832 0.0431 0.070 Uiso 1 1 calc R . . C265 C 0.5674(2) 0.68147(16) -0.06669(18) 0.0439(8) Uani 1 1 d . . . H26G H 0.5063 0.6658 -0.0348 0.066 Uiso 1 1 calc R . . H26H H 0.6278 0.6526 -0.0429 0.066 Uiso 1 1 calc R . . H26I H 0.5639 0.6652 -0.1199 0.066 Uiso 1 1 calc R . . C27 C 0.32783(18) 0.83905(14) -0.15540(14) 0.0224(6) Uani 1 1 d . . . H27 H 0.3559 0.8661 -0.2028 0.027 Uiso 1 1 calc R . . C28 C 0.22428(19) 0.83151(14) -0.14742(14) 0.0207(6) Uani 1 1 d . . . O281 O 0.17391(12) 0.86391(9) -0.21064(9) 0.0242(4) Uani 1 1 d . . . C282 C 0.06724(18) 0.85089(15) -0.22049(14) 0.0241(6) Uani 1 1 d . . . C283 C 0.0493(2) 0.89646(16) -0.30096(15) 0.0376(7) Uani 1 1 d . . . H28A H 0.0578 0.9563 -0.3001 0.056 Uiso 1 1 calc R . . H28B H -0.0198 0.8893 -0.3149 0.056 Uiso 1 1 calc R . . H28C H 0.0985 0.8732 -0.3399 0.056 Uiso 1 1 calc R . . C284 C 0.0567(2) 0.75847(16) -0.22081(19) 0.0495(9) Uani 1 1 d . . . H28D H 0.1044 0.7360 -0.2610 0.074 Uiso 1 1 calc R . . H28E H -0.0130 0.7497 -0.2324 0.074 Uiso 1 1 calc R . . H28F H 0.0717 0.7296 -0.1692 0.074 Uiso 1 1 calc R . . C285 C -0.0019(2) 0.8908(2) -0.15957(18) 0.0576(9) Uani 1 1 d . . . H28G H 0.0078 0.8596 -0.1080 0.086 Uiso 1 1 calc R . . H28H H -0.0727 0.8899 -0.1728 0.086 Uiso 1 1 calc R . . H28I H 0.0142 0.9490 -0.1581 0.086 Uiso 1 1 calc R . . O29 O 0.17627(12) 0.79877(11) -0.08739(10) 0.0330(5) Uani 1 1 d . . . N21 N 0.08477(15) 0.73386(11) 0.05887(11) 0.0228(5) Uani 1 1 d D . . C31 C 0.0503(3) 0.7399(3) 0.1371(2) 0.0215(12) Uani 0.524(3) 1 d PD A 1 H31A H -0.0179 0.7705 0.1379 0.026 Uiso 0.524(3) 1 calc PR A 1 H31B H 0.0965 0.7740 0.1612 0.026 Uiso 0.524(3) 1 calc PR A 1 C32 C 0.0436(6) 0.6573(6) 0.1875(5) 0.028(2) Uani 0.524(3) 1 d PD A 1 H32A H -0.0082 0.6257 0.1683 0.042 Uiso 0.524(3) 1 calc PR A 1 H32B H 0.0250 0.6680 0.2420 0.042 Uiso 0.524(3) 1 calc PR A 1 H32C H 0.1097 0.6247 0.1848 0.042 Uiso 0.524(3) 1 calc PR A 1 C33 C 0.0194(3) 0.6852(3) 0.0129(3) 0.0233(13) Uani 0.524(3) 1 d PD A 1 H33A H 0.0463 0.6884 -0.0425 0.028 Uiso 0.524(3) 1 calc PR A 1 H33B H 0.0251 0.6255 0.0343 0.028 Uiso 0.524(3) 1 calc PR A 1 C34 C -0.0920(5) 0.7170(4) 0.0154(4) 0.0324(18) Uani 0.524(3) 1 d PD A 1 H34A H -0.1213 0.7084 0.0693 0.049 Uiso 0.524(3) 1 calc PR A 1 H34B H -0.1284 0.6863 -0.0188 0.049 Uiso 0.524(3) 1 calc PR A 1 H34C H -0.0983 0.7770 -0.0028 0.049 Uiso 0.524(3) 1 calc PR A 1 C31' C 0.0616(4) 0.6533(3) 0.0992(3) 0.0251(14) Uani 0.476(3) 1 d PD A 2 H31C H 0.1265 0.6184 0.1049 0.030 Uiso 0.476(3) 1 calc PR A 2 H31D H 0.0207 0.6258 0.0645 0.030 Uiso 0.476(3) 1 calc PR A 2 C32' C 0.0059(7) 0.6510(7) 0.1790(5) 0.032(3) Uani 0.476(3) 1 d PD A 2 H32D H 0.0465 0.6752 0.2154 0.048 Uiso 0.476(3) 1 calc PR A 2 H32E H -0.0049 0.5928 0.1985 0.048 Uiso 0.476(3) 1 calc PR A 2 H32F H -0.0600 0.6836 0.1748 0.048 Uiso 0.476(3) 1 calc PR A 2 C33' C -0.0080(3) 0.7946(3) 0.0530(3) 0.0239(14) Uani 0.476(3) 1 d PD A 2 H33C H 0.0114 0.8485 0.0250 0.029 Uiso 0.476(3) 1 calc PR A 2 H33D H -0.0351 0.8055 0.1065 0.029 Uiso 0.476(3) 1 calc PR A 2 C34' C -0.0909(6) 0.7618(4) 0.0098(5) 0.0335(19) Uani 0.476(3) 1 d PD A 2 H34D H -0.0626 0.7459 -0.0413 0.050 Uiso 0.476(3) 1 calc PR A 2 H34E H -0.1464 0.8057 0.0020 0.050 Uiso 0.476(3) 1 calc PR A 2 H34F H -0.1169 0.7127 0.0409 0.050 Uiso 0.476(3) 1 calc PR A 2 N22 N 0.21177(16) 0.87059(12) 0.05618(12) 0.0281(5) Uani 1 1 d D . . C35 C 0.2443(4) 0.9505(3) 0.0139(3) 0.0237(14) Uani 0.465(3) 1 d PD A 1 H35A H 0.2854 0.9364 -0.0340 0.028 Uiso 0.465(3) 1 calc PR A 1 H35B H 0.2901 0.9741 0.0477 0.028 Uiso 0.465(3) 1 calc PR A 1 C36 C 0.1640(9) 1.0192(6) -0.0106(8) 0.039(3) Uani 0.465(3) 1 d PDU A 1 H36A H 0.1114 0.9956 -0.0372 0.058 Uiso 0.465(3) 1 calc PR A 1 H36B H 0.1954 1.0625 -0.0466 0.058 Uiso 0.465(3) 1 calc PR A 1 H36C H 0.1332 1.0442 0.0359 0.058 Uiso 0.465(3) 1 calc PR A 1 C37 C 0.1547(4) 0.8950(3) 0.1346(3) 0.0266(15) Uani 0.465(3) 1 d PD A 1 H37A H 0.0935 0.9323 0.1214 0.032 Uiso 0.465(3) 1 calc PR A 1 H37B H 0.1312 0.8433 0.1644 0.032 Uiso 0.465(3) 1 calc PR A 1 C38 C 0.2159(5) 0.9383(4) 0.1880(4) 0.0372(17) Uani 0.465(3) 1 d PD A 1 H38A H 0.2801 0.9047 0.1977 0.056 Uiso 0.465(3) 1 calc PR A 1 H38B H 0.1768 0.9441 0.2380 0.056 Uiso 0.465(3) 1 calc PR A 1 H38C H 0.2303 0.9939 0.1628 0.056 Uiso 0.465(3) 1 calc PR A 1 C35' C 0.1296(3) 0.9256(3) 0.0403(3) 0.0281(13) Uani 0.535(3) 1 d PD A 2 H35C H 0.1039 0.9494 0.0895 0.034 Uiso 0.535(3) 1 calc PR A 2 H35D H 0.0752 0.8942 0.0232 0.034 Uiso 0.535(3) 1 calc PR A 2 C36' C 0.1501(8) 0.9978(5) -0.0223(7) 0.037(3) Uani 0.535(3) 1 d PDU A 2 H36D H 0.2014 1.0312 -0.0049 0.055 Uiso 0.535(3) 1 calc PR A 2 H36E H 0.0870 1.0333 -0.0306 0.055 Uiso 0.535(3) 1 calc PR A 2 H36F H 0.1750 0.9752 -0.0715 0.055 Uiso 0.535(3) 1 calc PR A 2 C37' C 0.3064(3) 0.9016(3) 0.0807(3) 0.0284(13) Uani 0.535(3) 1 d PD A 2 H37C H 0.3307 0.9453 0.0405 0.034 Uiso 0.535(3) 1 calc PR A 2 H37D H 0.3601 0.8548 0.0857 0.034 Uiso 0.535(3) 1 calc PR A 2 C38' C 0.2856(5) 0.9380(4) 0.1590(3) 0.0447(17) Uani 0.535(3) 1 d PD A 2 H38D H 0.2392 0.9888 0.1523 0.067 Uiso 0.535(3) 1 calc PR A 2 H38E H 0.3497 0.9520 0.1780 0.067 Uiso 0.535(3) 1 calc PR A 2 H38F H 0.2544 0.8966 0.1972 0.067 Uiso 0.535(3) 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 0.0166(2) 0.0193(2) 0.0209(3) -0.00475(18) -0.0005(2) -0.00260(19) O6 0.0168(9) 0.0208(9) 0.0205(9) -0.0029(7) -0.0021(7) -0.0030(7) C7 0.0226(15) 0.0154(13) 0.0213(14) -0.0037(10) -0.0042(12) -0.0023(11) O7 0.0242(10) 0.0312(10) 0.0184(10) 0.0036(7) -0.0024(8) -0.0047(8) C21 0.0306(16) 0.0306(15) 0.0224(15) 0.0052(11) -0.0008(12) -0.0137(12) C113 0.0373(18) 0.060(2) 0.0232(16) -0.0007(14) 0.0058(13) 0.0001(15) C212 0.0469(19) 0.0415(17) 0.0457(19) 0.0107(14) -0.0167(16) -0.0226(15) C213 0.0441(18) 0.0398(16) 0.0261(16) 0.0092(13) -0.0062(14) -0.0161(14) C8 0.0192(14) 0.0257(14) 0.0214(14) -0.0047(11) -0.0037(11) 0.0013(11) C9 0.0195(14) 0.0187(13) 0.0233(14) -0.0048(11) 0.0019(12) -0.0028(11) O9 0.0164(9) 0.0368(10) 0.0217(10) 0.0037(8) 0.0038(8) 0.0017(8) C41 0.0229(15) 0.0460(18) 0.0233(15) 0.0071(13) 0.0047(12) -0.0025(13) C412 0.0216(16) 0.074(2) 0.0343(18) 0.0144(15) 0.0067(13) 0.0035(15) C411 0.0365(19) 0.0455(19) 0.060(2) 0.0175(16) 0.0110(16) -0.0048(15) C413 0.0330(18) 0.084(2) 0.0256(17) -0.0123(15) 0.0030(14) -0.0019(17) O10 0.0161(9) 0.0219(9) 0.0198(9) -0.0013(7) -0.0015(7) -0.0022(7) O1 0.0223(10) 0.0168(9) 0.0223(10) -0.0023(7) -0.0051(8) -0.0018(7) C2 0.0135(13) 0.0258(14) 0.0207(14) -0.0002(11) -0.0011(11) -0.0029(11) O2 0.0270(10) 0.0221(9) 0.0222(10) 0.0007(7) -0.0048(8) -0.0009(8) C91 0.0333(16) 0.0187(14) 0.0266(15) 0.0001(11) -0.0019(12) -0.0076(12) C912 0.0406(18) 0.0240(15) 0.0377(17) 0.0019(12) -0.0036(14) 0.0061(13) C913 0.0474(19) 0.0230(14) 0.0313(16) 0.0050(12) -0.0062(14) -0.0068(13) C911 0.0479(19) 0.0344(16) 0.0325(17) 0.0003(12) -0.0044(14) -0.0177(14) C3 0.0219(14) 0.0211(13) 0.0187(14) -0.0049(10) -0.0015(11) -0.0022(11) C4 0.0138(13) 0.0215(14) 0.0258(15) -0.0024(11) -0.0006(11) -0.0039(11) O4 0.0308(10) 0.0171(9) 0.0223(10) -0.0045(7) -0.0038(8) 0.0013(8) C71 0.0313(16) 0.0173(13) 0.0259(15) 0.0011(11) -0.0020(12) -0.0012(11) C722 0.055(2) 0.0238(15) 0.0459(19) -0.0037(13) 0.0151(16) -0.0107(14) C711 0.0325(16) 0.0195(14) 0.0430(18) -0.0062(12) -0.0102(14) -0.0016(12) C723 0.0393(17) 0.0240(14) 0.0382(17) -0.0067(12) -0.0131(14) 0.0019(13) O5 0.0216(10) 0.0175(9) 0.0188(10) -0.0033(7) -0.0017(7) -0.0019(7) N1 0.0167(11) 0.0200(11) 0.0244(12) -0.0049(9) -0.0025(9) -0.0012(9) C12 0.0239(15) 0.0239(14) 0.0344(16) -0.0082(12) -0.0026(12) 0.0016(12) C14 0.0397(18) 0.0296(16) 0.0491(19) -0.0035(13) -0.0059(15) 0.0011(14) C11 0.0244(15) 0.0250(14) 0.0333(16) -0.0085(12) -0.0031(12) -0.0032(12) C13 0.047(2) 0.061(2) 0.0411(19) -0.0238(15) -0.0070(16) -0.0102(16) N2 0.0192(11) 0.0213(11) 0.0251(12) -0.0085(9) -0.0011(9) -0.0017(9) C24 0.0233(15) 0.0355(16) 0.0296(16) -0.0088(12) 0.0027(12) -0.0051(12) C15 0.0390(18) 0.0461(18) 0.0343(17) -0.0015(13) 0.0093(14) -0.0169(14) C22 0.0201(14) 0.0275(14) 0.0333(16) -0.0084(12) 0.0015(12) -0.0036(12) C16 0.0281(16) 0.0397(17) 0.0447(18) -0.0149(14) -0.0074(14) -0.0011(13) Ti2 0.0210(3) 0.0318(3) 0.0185(3) 0.0020(2) -0.0011(2) -0.0075(2) O20 0.0237(10) 0.0180(9) 0.0210(9) -0.0013(7) -0.0014(8) -0.0053(8) C219 0.0146(13) 0.0257(14) 0.0204(14) -0.0028(11) 0.0019(11) -0.0073(11) O211 0.0301(10) 0.0232(9) 0.0208(10) -0.0048(7) -0.0078(8) 0.0006(8) C217 0.0284(15) 0.0271(14) 0.0211(14) -0.0081(11) -0.0059(12) -0.0059(12) C218 0.0483(19) 0.0410(17) 0.0302(17) -0.0081(13) -0.0171(15) 0.0020(15) C214 0.0410(18) 0.0394(16) 0.0374(18) -0.0071(13) -0.0065(14) -0.0161(14) C215 0.0369(17) 0.0339(15) 0.0226(15) -0.0067(12) 0.0027(13) -0.0022(13) C220 0.0294(15) 0.0244(14) 0.0212(14) -0.0039(11) -0.0012(12) -0.0020(12) C23 0.0196(14) 0.0317(16) 0.0240(15) -0.0053(12) 0.0057(12) -0.0100(12) O231 0.0467(12) 0.0325(10) 0.0215(10) -0.0109(8) -0.0012(9) -0.0094(9) C232 0.071(2) 0.0393(17) 0.0208(16) -0.0062(13) -0.0071(15) -0.0270(16) C233 0.079(3) 0.057(2) 0.064(2) -0.0041(17) -0.038(2) -0.0255(19) C234 0.137(4) 0.0464(19) 0.0267(18) -0.0101(14) 0.021(2) -0.041(2) C235 0.125(3) 0.0371(18) 0.0315(19) -0.0123(14) -0.012(2) -0.0206(19) O24 0.0246(10) 0.0335(10) 0.0199(10) -0.0042(8) -0.0010(8) -0.0042(8) O25 0.0213(10) 0.0454(11) 0.0173(10) 0.0055(8) -0.0009(8) -0.0096(8) C26 0.0225(15) 0.0199(13) 0.0227(15) -0.0060(11) 0.0003(12) -0.0033(11) O261 0.0188(10) 0.0328(10) 0.0232(10) 0.0009(8) 0.0020(8) -0.0024(8) C262 0.0198(15) 0.0410(17) 0.0287(16) -0.0012(12) -0.0029(12) 0.0004(13) C263 0.0250(16) 0.063(2) 0.0355(18) -0.0021(15) 0.0012(14) -0.0011(15) C264 0.0304(17) 0.078(2) 0.0341(18) -0.0137(15) -0.0030(14) -0.0086(16) C265 0.0345(18) 0.0428(18) 0.053(2) 0.0012(15) -0.0102(15) 0.0044(14) C27 0.0215(14) 0.0229(14) 0.0213(14) 0.0051(11) 0.0005(11) -0.0033(11) C28 0.0260(15) 0.0163(13) 0.0202(14) -0.0042(10) -0.0031(12) -0.0006(11) O281 0.0192(9) 0.0314(10) 0.0220(10) 0.0044(7) -0.0052(8) -0.0070(8) C282 0.0204(14) 0.0310(15) 0.0217(14) -0.0005(11) -0.0034(11) -0.0069(12) C283 0.0332(17) 0.0487(18) 0.0309(17) 0.0070(13) -0.0113(14) -0.0094(14) C284 0.048(2) 0.0392(17) 0.065(2) 0.0078(15) -0.0264(17) -0.0219(15) C285 0.0296(18) 0.105(3) 0.039(2) -0.0189(18) -0.0059(15) 0.0087(18) O29 0.0206(10) 0.0566(12) 0.0206(10) 0.0111(9) -0.0027(8) -0.0129(9) N21 0.0218(12) 0.0212(11) 0.0247(12) 0.0033(9) -0.0027(10) -0.0044(9) C31 0.016(3) 0.031(3) 0.017(3) -0.002(2) 0.004(2) -0.003(2) C32 0.029(5) 0.029(4) 0.027(4) 0.001(3) 0.002(4) -0.012(4) C33 0.020(3) 0.029(3) 0.021(3) -0.004(2) 0.000(2) -0.005(2) C34 0.032(4) 0.037(4) 0.031(4) -0.008(4) -0.009(3) -0.005(4) C31' 0.020(3) 0.021(3) 0.034(3) -0.005(2) 0.002(3) -0.005(2) C32' 0.032(6) 0.035(5) 0.029(4) 0.004(3) 0.001(4) -0.011(4) C33' 0.021(3) 0.022(3) 0.027(3) 0.004(2) 0.003(2) -0.005(2) C34' 0.022(4) 0.035(5) 0.044(4) 0.001(4) -0.003(3) -0.007(4) N22 0.0289(13) 0.0310(12) 0.0243(13) 0.0070(10) -0.0046(10) -0.0111(11) C35 0.028(3) 0.018(3) 0.026(3) -0.003(2) 0.006(3) -0.007(2) C36 0.046(6) 0.029(5) 0.038(5) 0.003(4) 0.007(4) 0.000(5) C37 0.027(3) 0.022(3) 0.031(3) -0.001(2) 0.001(3) -0.004(2) C38 0.052(5) 0.034(4) 0.027(4) -0.010(3) -0.003(3) -0.002(4) C35' 0.027(3) 0.024(3) 0.033(3) -0.003(2) -0.003(2) 0.000(2) C36' 0.033(4) 0.023(4) 0.052(5) 0.007(4) -0.005(3) 0.000(4) C37' 0.025(3) 0.026(3) 0.036(3) -0.004(2) -0.005(2) -0.002(2) C38' 0.054(4) 0.037(3) 0.047(4) -0.023(3) -0.017(3) 0.005(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 N1 1.9101(19) . ? Ti1 N2 1.912(2) . ? Ti1 O1 2.0140(16) . ? Ti1 O6 2.0180(15) . ? Ti1 O5 2.0987(15) . ? Ti1 O10 2.1007(16) . ? O6 C7 1.281(3) . ? C7 O7 1.346(3) . ? C7 C8 1.371(3) . ? O7 C21 1.463(3) . ? C21 C212 1.514(3) . ? C21 C113 1.516(3) . ? C21 C213 1.527(3) . ? C113 H11A 0.9800 . ? C113 H11B 0.9800 . ? C113 H11C 0.9800 . ? C212 H11D 0.9800 . ? C212 H11E 0.9800 . ? C212 H11F 0.9800 . ? C213 H11G 0.9800 . ? C213 H11H 0.9800 . ? C213 H11I 0.9800 . ? C8 C9 1.402(3) . ? C8 H12 0.9500 . ? C9 O10 1.259(3) . ? C9 O9 1.340(3) . ? O9 C41 1.475(3) . ? C41 C413 1.506(4) . ? C41 C411 1.511(4) . ? C41 C412 1.519(3) . ? C412 H13A 0.9800 . ? C412 H13B 0.9800 . ? C412 H13C 0.9800 . ? C411 H13D 0.9800 . ? C411 H13E 0.9800 . ? C411 H13F 0.9800 . ? C413 H13G 0.9800 . ? C413 H13H 0.9800 . ? C413 H13I 0.9800 . ? O1 C2 1.275(3) . ? C2 O2 1.346(3) . ? C2 C3 1.384(3) . ? O2 C91 1.474(3) . ? C91 C912 1.517(3) . ? C91 C911 1.520(3) . ? C91 C913 1.521(3) . ? C912 H16A 0.9800 . ? C912 H16B 0.9800 . ? C912 H16C 0.9800 . ? C913 H16D 0.9800 . ? C913 H16E 0.9800 . ? C913 H16F 0.9800 . ? C911 H16G 0.9800 . ? C911 H16H 0.9800 . ? C911 H16I 0.9800 . ? C3 C4 1.403(3) . ? C3 H17 0.9500 . ? C4 O5 1.251(3) . ? C4 O4 1.346(3) . ? O4 C71 1.474(3) . ? C71 C722 1.508(3) . ? C71 C723 1.517(3) . ? C71 C711 1.527(3) . ? C722 H18A 0.9800 . ? C722 H18B 0.9800 . ? C722 H18C 0.9800 . ? C711 H18D 0.9800 . ? C711 H18E 0.9800 . ? C711 H18F 0.9800 . ? C723 H18G 0.9800 . ? C723 H18H 0.9800 . ? C723 H18I 0.9800 . ? N1 C12 1.462(3) . ? N1 C11 1.471(3) . ? C12 C14 1.530(3) . ? C12 H1A 0.9900 . ? C12 H1B 0.9900 . ? C14 H2A 0.9800 . ? C14 H2B 0.9800 . ? C14 H2C 0.9800 . ? C11 C13 1.517(3) . ? C11 H3A 0.9900 . ? C11 H3B 0.9900 . ? C13 H4A 0.9800 . ? C13 H4B 0.9800 . ? C13 H4C 0.9800 . ? N2 C24 1.458(3) . ? N2 C22 1.469(3) . ? C24 C15 1.527(3) . ? C24 H5A 0.9900 . ? C24 H5B 0.9900 . ? C15 H6A 0.9800 . ? C15 H6B 0.9800 . ? C15 H6C 0.9800 . ? C22 C16 1.517(3) . ? C22 H7A 0.9900 . ? C22 H7B 0.9900 . ? C16 H8A 0.9800 . ? C16 H8B 0.9800 . ? C16 H8C 0.9800 . ? Ti2 N22 1.909(2) . ? Ti2 N21 1.913(2) . ? Ti2 O20 2.0183(16) . ? Ti2 O29 2.0191(17) . ? Ti2 O24 2.1025(17) . ? Ti2 O25 2.1047(17) . ? O20 C219 1.276(2) . ? C219 O211 1.348(3) . ? C219 C220 1.382(3) . ? O211 C217 1.475(3) . ? C217 C215 1.510(3) . ? C217 C214 1.515(3) . ? C217 C218 1.524(3) . ? C218 H21A 0.9800 . ? C218 H21B 0.9800 . ? C218 H21C 0.9800 . ? C214 H21D 0.9800 . ? C214 H21E 0.9800 . ? C214 H21F 0.9800 . ? C215 H21G 0.9800 . ? C215 H21H 0.9800 . ? C215 H21I 0.9800 . ? C220 C23 1.401(3) . ? C220 H22 0.9500 . ? C23 O24 1.252(3) . ? C23 O231 1.349(3) . ? O231 C232 1.462(3) . ? C232 C233 1.495(4) . ? C232 C234 1.522(4) . ? C232 C235 1.525(4) . ? C233 H23A 0.9800 . ? C233 H23B 0.9800 . ? C233 H23C 0.9800 . ? C234 H23D 0.9800 . ? C234 H23E 0.9800 . ? C234 H23F 0.9800 . ? C235 H23G 0.9800 . ? C235 H23H 0.9800 . ? C235 H23I 0.9800 . ? O25 C26 1.255(3) . ? C26 O261 1.340(3) . ? C26 C27 1.395(3) . ? O261 C262 1.473(3) . ? C262 C264 1.507(4) . ? C262 C265 1.513(4) . ? C262 C263 1.517(4) . ? C263 H26A 0.9800 . ? C263 H26B 0.9800 . ? C263 H26C 0.9800 . ? C264 H26D 0.9800 . ? C264 H26E 0.9800 . ? C264 H26F 0.9800 . ? C265 H26G 0.9800 . ? C265 H26H 0.9800 . ? C265 H26I 0.9800 . ? C27 C28 1.381(3) . ? C27 H27 0.9500 . ? C28 O29 1.263(3) . ? C28 O281 1.345(3) . ? O281 C282 1.466(3) . ? C282 C285 1.500(4) . ? C282 C284 1.505(3) . ? C282 C283 1.517(3) . ? C283 H28A 0.9800 . ? C283 H28B 0.9800 . ? C283 H28C 0.9800 . ? C284 H28D 0.9800 . ? C284 H28E 0.9800 . ? C284 H28F 0.9800 . ? C285 H28G 0.9800 . ? C285 H28H 0.9800 . ? C285 H28I 0.9800 . ? N21 C31 1.399(4) . ? N21 C31' 1.449(4) . ? N21 C33' 1.503(4) . ? N21 C33 1.523(4) . ? C31 C32 1.512(8) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.516(7) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C31' C32' 1.508(9) . ? C31' H31C 0.9900 . ? C31' H31D 0.9900 . ? C32' H32D 0.9800 . ? C32' H32E 0.9800 . ? C32' H32F 0.9800 . ? C33' C34' 1.522(7) . ? C33' H33C 0.9900 . ? C33' H33D 0.9900 . ? C34' H34D 0.9800 . ? C34' H34E 0.9800 . ? C34' H34F 0.9800 . ? N22 C35' 1.364(4) . ? N22 C37' 1.487(4) . ? N22 C35 1.489(4) . ? N22 C37 1.568(5) . ? C35 C36 1.512(9) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.519(6) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C35' C36' 1.524(8) . ? C35' H35C 0.9900 . ? C35' H35D 0.9900 . ? C36' H36D 0.9800 . ? C36' H36E 0.9800 . ? C36' H36F 0.9800 . ? C37' C38' 1.520(6) . ? C37' H37C 0.9900 . ? C37' H37D 0.9900 . ? C38' H38D 0.9800 . ? C38' H38E 0.9800 . ? C38' H38F 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 N1 Ti1 N2 96.28(8) . . ? N1 Ti1 O1 96.55(7) . . ? N2 Ti1 O1 94.07(8) . . ? N1 Ti1 O6 94.25(7) . . ? N2 Ti1 O6 96.82(7) . . ? O1 Ti1 O6 163.73(6) . . ? N1 Ti1 O5 173.74(8) . . ? N2 Ti1 O5 89.98(7) . . ? O1 Ti1 O5 83.09(6) . . ? O6 Ti1 O5 84.85(6) . . ? N1 Ti1 O10 90.95(7) . . ? N2 Ti1 O10 172.67(7) . . ? O1 Ti1 O10 83.88(6) . . ? O6 Ti1 O10 83.80(6) . . ? O5 Ti1 O10 82.79(6) . . ? C7 O6 Ti1 131.29(15) . . ? O6 C7 O7 120.1(2) . . ? O6 C7 C8 126.6(2) . . ? O7 C7 C8 113.3(2) . . ? C7 O7 C21 124.56(18) . . ? O7 C21 C212 109.3(2) . . ? O7 C21 C113 110.21(19) . . ? C212 C21 C113 113.6(2) . . ? O7 C21 C213 101.77(19) . . ? C212 C21 C213 110.9(2) . . ? C113 C21 C213 110.4(2) . . ? C21 C113 H11A 109.5 . . ? C21 C113 H11B 109.5 . . ? H11A C113 H11B 109.5 . . ? C21 C113 H11C 109.5 . . ? H11A C113 H11C 109.5 . . ? H11B C113 H11C 109.5 . . ? C21 C212 H11D 109.5 . . ? C21 C212 H11E 109.5 . . ? H11D C212 H11E 109.5 . . ? C21 C212 H11F 109.5 . . ? H11D C212 H11F 109.5 . . ? H11E C212 H11F 109.5 . . ? C21 C213 H11G 109.5 . . ? C21 C213 H11H 109.5 . . ? H11G C213 H11H 109.5 . . ? C21 C213 H11I 109.5 . . ? H11G C213 H11I 109.5 . . ? H11H C213 H11I 109.5 . . ? C7 C8 C9 122.3(2) . . ? C7 C8 H12 118.8 . . ? C9 C8 H12 118.8 . . ? O10 C9 O9 121.2(2) . . ? O10 C9 C8 125.6(2) . . ? O9 C9 C8 113.2(2) . . ? C9 O9 C41 121.92(18) . . ? O9 C41 C413 110.9(2) . . ? O9 C41 C411 109.5(2) . . ? C413 C41 C411 112.7(2) . . ? O9 C41 C412 101.18(19) . . ? C413 C41 C412 110.7(2) . . ? C411 C41 C412 111.3(2) . . ? C41 C412 H13A 109.5 . . ? C41 C412 H13B 109.5 . . ? H13A C412 H13B 109.5 . . ? C41 C412 H13C 109.5 . . ? H13A C412 H13C 109.5 . . ? H13B C412 H13C 109.5 . . ? C41 C411 H13D 109.5 . . ? C41 C411 H13E 109.5 . . ? H13D C411 H13E 109.5 . . ? C41 C411 H13F 109.5 . . ? H13D C411 H13F 109.5 . . ? H13E C411 H13F 109.5 . . ? C41 C413 H13G 109.5 . . ? C41 C413 H13H 109.5 . . ? H13G C413 H13H 109.5 . . ? C41 C413 H13I 109.5 . . ? H13G C413 H13I 109.5 . . ? H13H C413 H13I 109.5 . . ? C9 O10 Ti1 129.77(15) . . ? C2 O1 Ti1 132.48(14) . . ? O1 C2 O2 119.8(2) . . ? O1 C2 C3 126.3(2) . . ? O2 C2 C3 113.9(2) . . ? C2 O2 C91 123.22(18) . . ? O2 C91 C912 110.4(2) . . ? O2 C91 C911 108.98(19) . . ? C912 C91 C911 113.4(2) . . ? O2 C91 C913 102.10(18) . . ? C912 C91 C913 110.7(2) . . ? C911 C91 C913 110.7(2) . . ? C91 C912 H16A 109.5 . . ? C91 C912 H16B 109.5 . . ? H16A C912 H16B 109.5 . . ? C91 C912 H16C 109.5 . . ? H16A C912 H16C 109.5 . . ? H16B C912 H16C 109.5 . . ? C91 C913 H16D 109.5 . . ? C91 C913 H16E 109.5 . . ? H16D C913 H16E 109.5 . . ? C91 C913 H16F 109.5 . . ? H16D C913 H16F 109.5 . . ? H16E C913 H16F 109.5 . . ? C91 C911 H16G 109.5 . . ? C91 C911 H16H 109.5 . . ? H16G C911 H16H 109.5 . . ? C91 C911 H16I 109.5 . . ? H16G C911 H16I 109.5 . . ? H16H C911 H16I 109.5 . . ? C2 C3 C4 121.1(2) . . ? C2 C3 H17 119.5 . . ? C4 C3 H17 119.5 . . ? O5 C4 O4 120.8(2) . . ? O5 C4 C3 126.4(2) . . ? O4 C4 C3 112.8(2) . . ? C4 O4 C71 121.25(18) . . ? O4 C71 C722 110.57(19) . . ? O4 C71 C723 110.5(2) . . ? C722 C71 C723 113.2(2) . . ? O4 C71 C711 101.25(19) . . ? C722 C71 C711 109.9(2) . . ? C723 C71 C711 110.9(2) . . ? C71 C722 H18A 109.5 . . ? C71 C722 H18B 109.5 . . ? H18A C722 H18B 109.5 . . ? C71 C722 H18C 109.5 . . ? H18A C722 H18C 109.5 . . ? H18B C722 H18C 109.5 . . ? C71 C711 H18D 109.5 . . ? C71 C711 H18E 109.5 . . ? H18D C711 H18E 109.5 . . ? C71 C711 H18F 109.5 . . ? H18D C711 H18F 109.5 . . ? H18E C711 H18F 109.5 . . ? C71 C723 H18G 109.5 . . ? C71 C723 H18H 109.5 . . ? H18G C723 H18H 109.5 . . ? C71 C723 H18I 109.5 . . ? H18G C723 H18I 109.5 . . ? H18H C723 H18I 109.5 . . ? C4 O5 Ti1 130.47(14) . . ? C12 N1 C11 113.60(18) . . ? C12 N1 Ti1 122.84(15) . . ? C11 N1 Ti1 123.32(14) . . ? N1 C12 C14 113.9(2) . . ? N1 C12 H1A 108.8 . . ? C14 C12 H1A 108.8 . . ? N1 C12 H1B 108.8 . . ? C14 C12 H1B 108.8 . . ? H1A C12 H1B 107.7 . . ? C12 C14 H2A 109.5 . . ? C12 C14 H2B 109.5 . . ? H2A C14 H2B 109.5 . . ? C12 C14 H2C 109.5 . . ? H2A C14 H2C 109.5 . . ? H2B C14 H2C 109.5 . . ? N1 C11 C13 112.6(2) . . ? N1 C11 H3A 109.1 . . ? C13 C11 H3A 109.1 . . ? N1 C11 H3B 109.1 . . ? C13 C11 H3B 109.1 . . ? H3A C11 H3B 107.8 . . ? C11 C13 H4A 109.5 . . ? C11 C13 H4B 109.5 . . ? H4A C13 H4B 109.5 . . ? C11 C13 H4C 109.5 . . ? H4A C13 H4C 109.5 . . ? H4B C13 H4C 109.5 . . ? C24 N2 C22 113.7(2) . . ? C24 N2 Ti1 122.59(15) . . ? C22 N2 Ti1 123.47(16) . . ? N2 C24 C15 113.7(2) . . ? N2 C24 H5A 108.8 . . ? C15 C24 H5A 108.8 . . ? N2 C24 H5B 108.8 . . ? C15 C24 H5B 108.8 . . ? H5A C24 H5B 107.7 . . ? C24 C15 H6A 109.5 . . ? C24 C15 H6B 109.5 . . ? H6A C15 H6B 109.5 . . ? C24 C15 H6C 109.5 . . ? H6A C15 H6C 109.5 . . ? H6B C15 H6C 109.5 . . ? N2 C22 C16 113.96(19) . . ? N2 C22 H7A 108.8 . . ? C16 C22 H7A 108.8 . . ? N2 C22 H7B 108.8 . . ? C16 C22 H7B 108.8 . . ? H7A C22 H7B 107.7 . . ? C22 C16 H8A 109.5 . . ? C22 C16 H8B 109.5 . . ? H8A C16 H8B 109.5 . . ? C22 C16 H8C 109.5 . . ? H8A C16 H8C 109.5 . . ? H8B C16 H8C 109.5 . . ? N22 Ti2 N21 97.48(9) . . ? N22 Ti2 O20 94.25(8) . . ? N21 Ti2 O20 96.68(7) . . ? N22 Ti2 O29 95.57(8) . . ? N21 Ti2 O29 92.74(8) . . ? O20 Ti2 O29 165.39(7) . . ? N22 Ti2 O24 172.34(8) . . ? N21 Ti2 O24 90.01(8) . . ? O20 Ti2 O24 83.27(6) . . ? O29 Ti2 O24 85.59(7) . . ? N22 Ti2 O25 91.30(8) . . ? N21 Ti2 O25 170.74(8) . . ? O20 Ti2 O25 85.52(6) . . ? O29 Ti2 O25 83.47(7) . . ? O24 Ti2 O25 81.30(7) . . ? C219 O20 Ti2 132.28(14) . . ? O20 C219 O211 119.5(2) . . ? O20 C219 C220 126.2(2) . . ? O211 C219 C220 114.3(2) . . ? C219 O211 C217 123.89(17) . . ? O211 C217 C215 110.73(19) . . ? O211 C217 C214 109.3(2) . . ? C215 C217 C214 113.4(2) . . ? O211 C217 C218 101.76(18) . . ? C215 C217 C218 110.1(2) . . ? C214 C217 C218 110.9(2) . . ? C217 C218 H21A 109.5 . . ? C217 C218 H21B 109.5 . . ? H21A C218 H21B 109.5 . . ? C217 C218 H21C 109.5 . . ? H21A C218 H21C 109.5 . . ? H21B C218 H21C 109.5 . . ? C217 C214 H21D 109.5 . . ? C217 C214 H21E 109.5 . . ? H21D C214 H21E 109.5 . . ? C217 C214 H21F 109.5 . . ? H21D C214 H21F 109.5 . . ? H21E C214 H21F 109.5 . . ? C217 C215 H21G 109.5 . . ? C217 C215 H21H 109.5 . . ? H21G C215 H21H 109.5 . . ? C217 C215 H21I 109.5 . . ? H21G C215 H21I 109.5 . . ? H21H C215 H21I 109.5 . . ? C219 C220 C23 121.4(2) . . ? C219 C220 H22 119.3 . . ? C23 C220 H22 119.3 . . ? O24 C23 O231 120.5(2) . . ? O24 C23 C220 126.6(2) . . ? O231 C23 C220 112.9(2) . . ? C23 O231 C232 121.9(2) . . ? O231 C232 C233 110.9(2) . . ? O231 C232 C234 110.1(2) . . ? C233 C232 C234 112.6(3) . . ? O231 C232 C235 101.8(2) . . ? C233 C232 C235 110.8(3) . . ? C234 C232 C235 110.0(3) . . ? C232 C233 H23A 109.5 . . ? C232 C233 H23B 109.5 . . ? H23A C233 H23B 109.5 . . ? C232 C233 H23C 109.5 . . ? H23A C233 H23C 109.5 . . ? H23B C233 H23C 109.5 . . ? C232 C234 H23D 109.5 . . ? C232 C234 H23E 109.5 . . ? H23D C234 H23E 109.5 . . ? C232 C234 H23F 109.5 . . ? H23D C234 H23F 109.5 . . ? H23E C234 H23F 109.5 . . ? C232 C235 H23G 109.5 . . ? C232 C235 H23H 109.5 . . ? H23G C235 H23H 109.5 . . ? C232 C235 H23I 109.5 . . ? H23G C235 H23I 109.5 . . ? H23H C235 H23I 109.5 . . ? C23 O24 Ti2 129.83(15) . . ? C26 O25 Ti2 129.03(15) . . ? O25 C26 O261 120.5(2) . . ? O25 C26 C27 126.1(2) . . ? O261 C26 C27 113.4(2) . . ? C26 O261 C262 122.38(18) . . ? O261 C262 C264 111.4(2) . . ? O261 C262 C265 109.3(2) . . ? C264 C262 C265 112.9(2) . . ? O261 C262 C263 101.59(19) . . ? C264 C262 C263 110.6(2) . . ? C265 C262 C263 110.6(2) . . ? C262 C263 H26A 109.5 . . ? C262 C263 H26B 109.5 . . ? H26A C263 H26B 109.5 . . ? C262 C263 H26C 109.5 . . ? H26A C263 H26C 109.5 . . ? H26B C263 H26C 109.5 . . ? C262 C264 H26D 109.5 . . ? C262 C264 H26E 109.5 . . ? H26D C264 H26E 109.5 . . ? C262 C264 H26F 109.5 . . ? H26D C264 H26F 109.5 . . ? H26E C264 H26F 109.5 . . ? C262 C265 H26G 109.5 . . ? C262 C265 H26H 109.5 . . ? H26G C265 H26H 109.5 . . ? C262 C265 H26I 109.5 . . ? H26G C265 H26I 109.5 . . ? H26H C265 H26I 109.5 . . ? C28 C27 C26 122.4(2) . . ? C28 C27 H27 118.8 . . ? C26 C27 H27 118.8 . . ? O29 C28 O281 120.0(2) . . ? O29 C28 C27 125.8(2) . . ? O281 C28 C27 114.2(2) . . ? C28 O281 C282 123.45(18) . . ? O281 C282 C285 111.1(2) . . ? O281 C282 C284 109.02(19) . . ? C285 C282 C284 113.4(2) . . ? O281 C282 C283 102.48(19) . . ? C285 C282 C283 109.8(2) . . ? C284 C282 C283 110.5(2) . . ? C282 C283 H28A 109.5 . . ? C282 C283 H28B 109.5 . . ? H28A C283 H28B 109.5 . . ? C282 C283 H28C 109.5 . . ? H28A C283 H28C 109.5 . . ? H28B C283 H28C 109.5 . . ? C282 C284 H28D 109.5 . . ? C282 C284 H28E 109.5 . . ? H28D C284 H28E 109.5 . . ? C282 C284 H28F 109.5 . . ? H28D C284 H28F 109.5 . . ? H28E C284 H28F 109.5 . . ? C282 C285 H28G 109.5 . . ? C282 C285 H28H 109.5 . . ? H28G C285 H28H 109.5 . . ? C282 C285 H28I 109.5 . . ? H28G C285 H28I 109.5 . . ? H28H C285 H28I 109.5 . . ? C28 O29 Ti2 131.69(16) . . ? C31 N21 C31' 67.8(3) . . ? C31 N21 C33' 76.3(3) . . ? C31' N21 C33' 112.1(3) . . ? C31 N21 C33 114.8(3) . . ? C31' N21 C33 66.6(3) . . ? C33' N21 C33 80.3(3) . . ? C31 N21 Ti2 120.9(2) . . ? C31' N21 Ti2 123.6(2) . . ? C33' N21 Ti2 124.3(2) . . ? C33 N21 Ti2 122.6(2) . . ? N21 C31 C32 115.4(5) . . ? N21 C31 H31A 108.4 . . ? C32 C31 H31A 108.4 . . ? N21 C31 H31B 108.4 . . ? C32 C31 H31B 108.4 . . ? H31A C31 H31B 107.5 . . ? C34 C33 N21 113.7(4) . . ? C34 C33 H33A 108.8 . . ? N21 C33 H33A 108.8 . . ? C34 C33 H33B 108.8 . . ? N21 C33 H33B 108.8 . . ? H33A C33 H33B 107.7 . . ? N21 C31' C32' 118.7(5) . . ? N21 C31' H31C 107.6 . . ? C32' C31' H31C 107.6 . . ? N21 C31' H31D 107.6 . . ? C32' C31' H31D 107.6 . . ? H31C C31' H31D 107.1 . . ? C31' C32' H32D 109.5 . . ? C31' C32' H32E 109.5 . . ? H32D C32' H32E 109.5 . . ? C31' C32' H32F 109.5 . . ? H32D C32' H32F 109.5 . . ? H32E C32' H32F 109.5 . . ? N21 C33' C34' 112.2(4) . . ? N21 C33' H33C 109.2 . . ? C34' C33' H33C 109.2 . . ? N21 C33' H33D 109.2 . . ? C34' C33' H33D 109.2 . . ? H33C C33' H33D 107.9 . . ? C33' C34' H34D 109.5 . . ? C33' C34' H34E 109.5 . . ? H34D C34' H34E 109.5 . . ? C33' C34' H34F 109.5 . . ? H34D C34' H34F 109.5 . . ? H34E C34' H34F 109.5 . . ? C35' N22 C37' 119.9(3) . . ? C35' N22 C35 69.2(3) . . ? C37' N22 C35 63.2(3) . . ? C35' N22 C37 69.9(3) . . ? C37' N22 C37 89.8(3) . . ? C35 N22 C37 105.8(3) . . ? C35' N22 Ti2 120.0(2) . . ? C37' N22 Ti2 118.3(2) . . ? C35 N22 Ti2 129.9(2) . . ? C37 N22 Ti2 123.8(2) . . ? N22 C35 C36 119.0(6) . . ? N22 C35 H35A 107.6 . . ? C36 C35 H35A 107.6 . . ? N22 C35 H35B 107.6 . . ? C36 C35 H35B 107.6 . . ? H35A C35 H35B 107.0 . . ? C38 C37 N22 115.9(4) . . ? C38 C37 H37A 108.3 . . ? N22 C37 H37A 108.3 . . ? C38 C37 H37B 108.3 . . ? N22 C37 H37B 108.3 . . ? H37A C37 H37B 107.4 . . ? N22 C35' C36' 115.0(5) . . ? N22 C35' H35C 108.5 . . ? C36' C35' H35C 108.5 . . ? N22 C35' H35D 108.5 . . ? C36' C35' H35D 108.5 . . ? H35C C35' H35D 107.5 . . ? C35' C36' H36D 109.5 . . ? C35' C36' H36E 109.5 . . ? H36D C36' H36E 109.5 . . ? C35' C36' H36F 109.5 . . ? H36D C36' H36F 109.5 . . ? H36E C36' H36F 109.5 . . ? N22 C37' C38' 109.8(4) . . ? N22 C37' H37C 109.7 . . ? C38' C37' H37C 109.7 . . ? N22 C37' H37D 109.7 . . ? C38' C37' H37D 109.7 . . ? H37C C37' H37D 108.2 . . ? C37' C38' H38D 109.5 . . ? C37' C38' H38E 109.5 . . ? H38D C38' H38E 109.5 . . ? C37' C38' H38F 109.5 . . ? H38D C38' H38F 109.5 . . ? H38E C38' H38F 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 N1 Ti1 O6 C7 -97.09(19) . . . . ? N2 Ti1 O6 C7 166.05(19) . . . . ? O1 Ti1 O6 C7 34.4(3) . . . . ? O5 Ti1 O6 C7 76.69(19) . . . . ? O10 Ti1 O6 C7 -6.60(18) . . . . ? Ti1 O6 C7 O7 -177.05(13) . . . . ? Ti1 O6 C7 C8 3.8(3) . . . . ? O6 C7 O7 C21 10.1(3) . . . . ? C8 C7 O7 C21 -170.7(2) . . . . ? C7 O7 C21 C212 59.7(3) . . . . ? C7 O7 C21 C113 -65.8(3) . . . . ? C7 O7 C21 C213 177.0(2) . . . . ? O6 C7 C8 C9 0.9(4) . . . . ? O7 C7 C8 C9 -178.3(2) . . . . ? C7 C8 C9 O10 1.2(4) . . . . ? C7 C8 C9 O9 -179.7(2) . . . . ? O10 C9 O9 C41 -2.3(3) . . . . ? C8 C9 O9 C41 178.5(2) . . . . ? C9 O9 C41 C413 -59.3(3) . . . . ? C9 O9 C41 C411 65.6(3) . . . . ? C9 O9 C41 C412 -176.8(2) . . . . ? O9 C9 O10 Ti1 173.38(14) . . . . ? C8 C9 O10 Ti1 -7.6(3) . . . . ? N1 Ti1 O10 C9 102.63(19) . . . . ? N2 Ti1 O10 C9 -86.8(6) . . . . ? O1 Ti1 O10 C9 -160.89(19) . . . . ? O6 Ti1 O10 C9 8.46(18) . . . . ? O5 Ti1 O10 C9 -77.11(19) . . . . ? N1 Ti1 O1 C2 167.9(2) . . . . ? N2 Ti1 O1 C2 -95.3(2) . . . . ? O6 Ti1 O1 C2 36.7(4) . . . . ? O5 Ti1 O1 C2 -5.8(2) . . . . ? O10 Ti1 O1 C2 77.7(2) . . . . ? Ti1 O1 C2 O2 -176.05(14) . . . . ? Ti1 O1 C2 C3 6.1(4) . . . . ? O1 C2 O2 C91 8.0(3) . . . . ? C3 C2 O2 C91 -173.9(2) . . . . ? C2 O2 C91 C912 -64.3(3) . . . . ? C2 O2 C91 C911 60.9(3) . . . . ? C2 O2 C91 C913 178.0(2) . . . . ? O1 C2 C3 C4 -1.1(4) . . . . ? O2 C2 C3 C4 -179.0(2) . . . . ? C2 C3 C4 O5 -2.1(4) . . . . ? C2 C3 C4 O4 176.6(2) . . . . ? O5 C4 O4 C71 -0.3(3) . . . . ? C3 C4 O4 C71 -179.2(2) . . . . ? C4 O4 C71 C722 62.0(3) . . . . ? C4 O4 C71 C723 -64.1(3) . . . . ? C4 O4 C71 C711 178.4(2) . . . . ? O4 C4 O5 Ti1 -178.36(14) . . . . ? C3 C4 O5 Ti1 0.3(4) . . . . ? N1 Ti1 O5 C4 -84.4(7) . . . . ? N2 Ti1 O5 C4 96.7(2) . . . . ? O1 Ti1 O5 C4 2.6(2) . . . . ? O6 Ti1 O5 C4 -166.4(2) . . . . ? O10 Ti1 O5 C4 -82.0(2) . . . . ? N2 Ti1 N1 C12 -45.88(19) . . . . ? O1 Ti1 N1 C12 48.96(18) . . . . ? O6 Ti1 N1 C12 -143.23(18) . . . . ? O5 Ti1 N1 C12 135.3(6) . . . . ? O10 Ti1 N1 C12 132.91(18) . . . . ? N2 Ti1 N1 C11 140.07(19) . . . . ? O1 Ti1 N1 C11 -125.08(19) . . . . ? O6 Ti1 N1 C11 42.72(19) . . . . ? O5 Ti1 N1 C11 -38.8(8) . . . . ? O10 Ti1 N1 C11 -41.13(19) . . . . ? C11 N1 C12 C14 56.5(3) . . . . ? Ti1 N1 C12 C14 -118.1(2) . . . . ? C12 N1 C11 C13 60.7(3) . . . . ? Ti1 N1 C11 C13 -124.8(2) . . . . ? N1 Ti1 N2 C24 -48.56(18) . . . . ? O1 Ti1 N2 C24 -145.61(17) . . . . ? O6 Ti1 N2 C24 46.51(17) . . . . ? O5 Ti1 N2 C24 131.32(17) . . . . ? O10 Ti1 N2 C24 140.9(5) . . . . ? N1 Ti1 N2 C22 137.49(17) . . . . ? O1 Ti1 N2 C22 40.43(17) . . . . ? O6 Ti1 N2 C22 -127.45(17) . . . . ? O5 Ti1 N2 C22 -42.64(17) . . . . ? O10 Ti1 N2 C22 -33.0(7) . . . . ? C22 N2 C24 C15 57.6(3) . . . . ? Ti1 N2 C24 C15 -116.9(2) . . . . ? C24 N2 C22 C16 62.9(3) . . . . ? Ti1 N2 C22 C16 -122.7(2) . . . . ? N22 Ti2 O20 C219 -167.34(19) . . . . ? N21 Ti2 O20 C219 94.60(19) . . . . ? O29 Ti2 O20 C219 -35.2(4) . . . . ? O24 Ti2 O20 C219 5.38(19) . . . . ? O25 Ti2 O20 C219 -76.37(19) . . . . ? Ti2 O20 C219 O211 -179.76(14) . . . . ? Ti2 O20 C219 C220 -1.5(3) . . . . ? O20 C219 O211 C217 -4.2(3) . . . . ? C220 C219 O211 C217 177.4(2) . . . . ? C219 O211 C217 C215 62.2(3) . . . . ? C219 O211 C217 C214 -63.4(3) . . . . ? C219 O211 C217 C218 179.2(2) . . . . ? O20 C219 C220 C23 -3.5(4) . . . . ? O211 C219 C220 C23 174.8(2) . . . . ? C219 C220 C23 O24 1.2(4) . . . . ? C219 C220 C23 O231 -177.9(2) . . . . ? O24 C23 O231 C232 4.4(3) . . . . ? C220 C23 O231 C232 -176.5(2) . . . . ? C23 O231 C232 C233 -64.7(3) . . . . ? C23 O231 C232 C234 60.6(3) . . . . ? C23 O231 C232 C235 177.3(2) . . . . ? O231 C23 O24 Ti2 -175.33(15) . . . . ? C220 C23 O24 Ti2 5.7(4) . . . . ? N22 Ti2 O24 C23 64.1(6) . . . . ? N21 Ti2 O24 C23 -104.0(2) . . . . ? O20 Ti2 O24 C23 -7.32(19) . . . . ? O29 Ti2 O24 C23 163.2(2) . . . . ? O25 Ti2 O24 C23 79.15(19) . . . . ? N22 Ti2 O25 C26 -84.4(2) . . . . ? N21 Ti2 O25 C26 77.3(5) . . . . ? O20 Ti2 O25 C26 -178.6(2) . . . . ? O29 Ti2 O25 C26 11.1(2) . . . . ? O24 Ti2 O25 C26 97.6(2) . . . . ? Ti2 O25 C26 O261 173.62(14) . . . . ? Ti2 O25 C26 C27 -5.9(4) . . . . ? O25 C26 O261 C262 13.6(3) . . . . ? C27 C26 O261 C262 -166.8(2) . . . . ? C26 O261 C262 C264 -66.6(3) . . . . ? C26 O261 C262 C265 58.8(3) . . . . ? C26 O261 C262 C263 175.6(2) . . . . ? O25 C26 C27 C28 -3.3(4) . . . . ? O261 C26 C27 C28 177.2(2) . . . . ? C26 C27 C28 O29 1.6(4) . . . . ? C26 C27 C28 O281 -179.3(2) . . . . ? O29 C28 O281 C282 -11.2(3) . . . . ? C27 C28 O281 C282 169.6(2) . . . . ? C28 O281 C282 C285 65.0(3) . . . . ? C28 O281 C282 C284 -60.8(3) . . . . ? C28 O281 C282 C283 -177.8(2) . . . . ? O281 C28 O29 Ti2 -169.13(15) . . . . ? C27 C28 O29 Ti2 10.0(4) . . . . ? N22 Ti2 O29 C28 77.5(2) . . . . ? N21 Ti2 O29 C28 175.3(2) . . . . ? O20 Ti2 O29 C28 -54.5(4) . . . . ? O24 Ti2 O29 C28 -94.9(2) . . . . ? O25 Ti2 O29 C28 -13.2(2) . . . . ? N22 Ti2 N21 C31 -54.0(2) . . . . ? O20 Ti2 N21 C31 41.2(2) . . . . ? O29 Ti2 N21 C31 -150.0(2) . . . . ? O24 Ti2 N21 C31 124.4(2) . . . . ? O25 Ti2 N21 C31 144.5(4) . . . . ? N22 Ti2 N21 C31' -136.5(3) . . . . ? O20 Ti2 N21 C31' -41.3(3) . . . . ? O29 Ti2 N21 C31' 127.5(3) . . . . ? O24 Ti2 N21 C31' 41.9(3) . . . . ? O25 Ti2 N21 C31' 61.9(6) . . . . ? N22 Ti2 N21 C33' 40.2(3) . . . . ? O20 Ti2 N21 C33' 135.4(3) . . . . ? O29 Ti2 N21 C33' -55.7(3) . . . . ? O24 Ti2 N21 C33' -141.3(3) . . . . ? O25 Ti2 N21 C33' -121.3(5) . . . . ? N22 Ti2 N21 C33 141.5(2) . . . . ? O20 Ti2 N21 C33 -123.3(2) . . . . ? O29 Ti2 N21 C33 45.5(2) . . . . ? O24 Ti2 N21 C33 -40.1(2) . . . . ? O25 Ti2 N21 C33 -20.0(6) . . . . ? C31' N21 C31 C32 11.2(5) . . . . ? C33' N21 C31 C32 132.3(5) . . . . ? C33 N21 C31 C32 59.9(5) . . . . ? Ti2 N21 C31 C32 -105.7(4) . . . . ? C31 N21 C33 C34 53.9(5) . . . . ? C31' N21 C33 C34 103.2(5) . . . . ? C33' N21 C33 C34 -16.1(4) . . . . ? Ti2 N21 C33 C34 -140.8(4) . . . . ? C31 N21 C31' C32' 11.0(5) . . . . ? C33' N21 C31' C32' -52.9(6) . . . . ? C33 N21 C31' C32' -121.0(6) . . . . ? Ti2 N21 C31' C32' 124.3(5) . . . . ? C31 N21 C33' C34' -117.6(5) . . . . ? C31' N21 C33' C34' -58.7(6) . . . . ? C33 N21 C33' C34' 1.0(5) . . . . ? Ti2 N21 C33' C34' 124.1(4) . . . . ? N21 Ti2 N22 C35' -47.8(3) . . . . ? O20 Ti2 N22 C35' -145.1(3) . . . . ? O29 Ti2 N22 C35' 45.8(3) . . . . ? O24 Ti2 N22 C35' 144.2(6) . . . . ? O25 Ti2 N22 C35' 129.3(3) . . . . ? N21 Ti2 N22 C37' 147.8(2) . . . . ? O20 Ti2 N22 C37' 50.5(3) . . . . ? O29 Ti2 N22 C37' -118.7(2) . . . . ? O24 Ti2 N22 C37' -20.3(7) . . . . ? O25 Ti2 N22 C37' -35.1(2) . . . . ? N21 Ti2 N22 C35 -134.8(3) . . . . ? O20 Ti2 N22 C35 127.9(3) . . . . ? O29 Ti2 N22 C35 -41.2(3) . . . . ? O24 Ti2 N22 C35 57.2(7) . . . . ? O25 Ti2 N22 C35 42.3(3) . . . . ? N21 Ti2 N22 C37 37.0(3) . . . . ? O20 Ti2 N22 C37 -60.3(3) . . . . ? O29 Ti2 N22 C37 130.5(3) . . . . ? O24 Ti2 N22 C37 -131.1(6) . . . . ? O25 Ti2 N22 C37 -145.9(3) . . . . ? C35' N22 C35 C36 -1.3(7) . . . . ? C37' N22 C35 C36 -143.4(8) . . . . ? C37 N22 C35 C36 -61.9(7) . . . . ? Ti2 N22 C35 C36 111.0(7) . . . . ? C35' N22 C37 C38 -118.8(5) . . . . ? C37' N22 C37 C38 3.4(5) . . . . ? C35 N22 C37 C38 -58.6(5) . . . . ? Ti2 N22 C37 C38 128.0(4) . . . . ? C37' N22 C35' C36' 56.2(7) . . . . ? C35 N22 C35' C36' 17.0(6) . . . . ? C37 N22 C35' C36' 133.8(6) . . . . ? Ti2 N22 C35' C36' -108.0(6) . . . . ? C35' N22 C37' C38' 64.0(5) . . . . ? C35 N22 C37' C38' 105.4(4) . . . . ? C37 N22 C37' C38' -2.5(4) . . . . ? Ti2 N22 C37' C38' -131.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.337 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.048