Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_bj9841 _database_code_CSD 159819 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Johnson, Brian F. G.' 'Klunduk, Marek C.' 'McIntosh, Calum' 'O'Connell, Timothy J.' 'Ridland, John' _publ_contact_author_name 'Prof Brian F G Johnson' _publ_contact_author_address ; Prof Brian F G Johnson The University Chemical Laboratory University of Cambridge Lensfield Road Cambridge CB2 1EW UNITED KINGDOM ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H80 N8 O12 Ti4' _chemical_formula_weight 960.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.444(9) _cell_length_b 11.479(9) _cell_length_c 20.085(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.24(5) _cell_angle_gamma 90.00 _cell_volume 2408(3) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 0.698 _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 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'R-Axis IIc' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7716 _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_av_sigmaI/netI 0.1303 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 25.15 _reflns_number_total 4182 _reflns_number_gt 2722 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0720P)^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 SHELXL _refine_ls_extinction_coef 0.037(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4182 _refine_ls_number_parameters 253 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0941 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.1668 _refine_ls_wR_factor_gt 0.1513 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.423 _refine_ls_shift/su_mean 0.019 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 0.04223(7) 0.11616(7) 0.02442(4) 0.0353(3) Uani 1 1 d . . . Ti2 Ti 0.05913(8) 0.04309(7) -0.12778(4) 0.0401(3) Uani 1 1 d . . . O1 O -0.0511(3) 0.1087(3) 0.10351(14) 0.0378(7) Uani 1 1 d . . . O2 O -0.0578(2) 0.0588(2) -0.04566(14) 0.0350(7) Uani 1 1 d . . . O3 O 0.1677(3) 0.1135(3) -0.05282(15) 0.0454(8) Uani 1 1 d . . . O4 O 0.0242(3) 0.2771(3) 0.02346(15) 0.0483(9) Uani 1 1 d . A . O5 O -0.0608(4) 0.0260(3) -0.19687(16) 0.0575(9) Uani 1 1 d . B . O6 O 0.2084(3) 0.0490(3) -0.17649(17) 0.0634(11) Uani 1 1 d D . . N1 N -0.2537(5) 0.3230(5) 0.0171(2) 0.0793(16) Uani 1 1 d D . . N2 N 0.0136(5) 0.2351(4) -0.1610(2) 0.0614(12) Uani 1 1 d D . . N3 N 0.2414(4) 0.1361(4) 0.0728(2) 0.0567(12) Uani 1 1 d . . . N4 N 0.4234(5) -0.0911(5) -0.2955(3) 0.097(2) Uani 1 1 d D . . C1 C -0.0408(6) 0.3546(4) 0.0665(3) 0.0602(15) Uani 1 1 d . . . H1A H 0.0175 0.4195 0.0782 0.072 Uiso 1 1 calc R A . H1B H -0.0622 0.3129 0.1082 0.072 Uiso 1 1 calc R . . C2 C -0.1599(6) 0.4036(5) 0.0378(3) 0.083(2) Uani 1 1 d D A . H2A H -0.1987 0.4559 0.0713 0.099 Uiso 1 1 calc R . . H2B H -0.1365 0.4522 -0.0010 0.099 Uiso 1 1 calc R . . C3 C -0.315(2) 0.260(2) 0.0709(9) 0.0949(19) Uiso 0.50 1 d PD A 1 H3A H -0.2531 0.2493 0.1074 0.142 Uiso 0.50 1 calc PR A 1 H3B H -0.3434 0.1840 0.0547 0.142 Uiso 0.50 1 calc PR A 1 H3C H -0.3883 0.3047 0.0869 0.142 Uiso 0.50 1 calc PR A 1 C4 C -0.3522(12) 0.3942(12) -0.0194(8) 0.0949(19) Uiso 0.50 1 d PD A 1 H4A H -0.3791 0.4596 0.0085 0.142 Uiso 0.50 1 calc PR A 1 H4B H -0.4265 0.3453 -0.0299 0.142 Uiso 0.50 1 calc PR A 1 H4C H -0.3152 0.4241 -0.0608 0.142 Uiso 0.50 1 calc PR A 1 C3' C -0.304(2) 0.257(2) 0.0756(8) 0.0949(19) Uiso 0.50 1 d PD A 2 H3D H -0.2355 0.2096 0.0950 0.142 Uiso 0.50 1 calc PR A 2 H3E H -0.3745 0.2065 0.0611 0.142 Uiso 0.50 1 calc PR A 2 H3F H -0.3356 0.3122 0.1091 0.142 Uiso 0.50 1 calc PR A 2 C4' C -0.3563(12) 0.3549(13) -0.0252(8) 0.0949(19) Uiso 0.50 1 d PD A 2 H4D H -0.4292 0.3803 0.0017 0.142 Uiso 0.50 1 calc PR A 2 H4E H -0.3816 0.2877 -0.0524 0.142 Uiso 0.50 1 calc PR A 2 H4F H -0.3293 0.4187 -0.0544 0.142 Uiso 0.50 1 calc PR A 2 C5 C 0.3007(5) 0.1353(6) -0.0448(3) 0.0723(18) Uani 1 1 d . . . H5A H 0.3329 0.1840 -0.0818 0.087 Uiso 1 1 calc R . . H5B H 0.3491 0.0612 -0.0442 0.087 Uiso 1 1 calc R . . C6 C 0.3154(5) 0.1984(6) 0.0208(3) 0.079(2) Uani 1 1 d . . . H6A H 0.4069 0.2015 0.0336 0.094 Uiso 1 1 calc R . . H6B H 0.2835 0.2792 0.0164 0.094 Uiso 1 1 calc R . . C7 C 0.3040(5) 0.0228(6) 0.0893(3) 0.0762(18) Uani 1 1 d . . . H7A H 0.3929 0.0367 0.1029 0.114 Uiso 1 1 calc R . . H7B H 0.3024 -0.0279 0.0501 0.114 Uiso 1 1 calc R . . H7C H 0.2577 -0.0148 0.1258 0.114 Uiso 1 1 calc R . . C8 C 0.2357(5) 0.2070(6) 0.1343(3) 0.0740(18) Uani 1 1 d . . . H8A H 0.3226 0.2188 0.1517 0.111 Uiso 1 1 calc R . . H8B H 0.1840 0.1665 0.1676 0.111 Uiso 1 1 calc R . . H8C H 0.1969 0.2827 0.1241 0.111 Uiso 1 1 calc R . . C9 C -0.0982(7) 0.1128(5) -0.2417(3) 0.079(2) Uani 1 1 d . . . H9A H -0.1875 0.1367 -0.2327 0.095 Uiso 1 1 calc R B . H9B H -0.0941 0.0825 -0.2878 0.095 Uiso 1 1 calc R . . C10 C -0.0102(7) 0.2156(5) -0.2343(3) 0.0767(19) Uani 1 1 d . B . H10A H -0.0499 0.2857 -0.2543 0.092 Uiso 1 1 calc R . . H10B H 0.0717 0.2002 -0.2573 0.092 Uiso 1 1 calc R . . C11 C -0.1027(6) 0.2806(5) -0.1305(3) 0.0766(19) Uani 1 1 d . B . H11A H -0.0885 0.2911 -0.0826 0.115 Uiso 1 1 calc R . . H11B H -0.1732 0.2255 -0.1376 0.115 Uiso 1 1 calc R . . H11C H -0.1246 0.3557 -0.1507 0.115 Uiso 1 1 calc R . . C12 C 0.1078(13) 0.3226(14) -0.1439(10) 0.090(3) Uiso 0.55 1 d PD B 1 H12A H 0.0860 0.3960 -0.1661 0.135 Uiso 0.55 1 calc PR B 1 H12B H 0.1926 0.2967 -0.1585 0.135 Uiso 0.55 1 calc PR B 1 H12C H 0.1085 0.3343 -0.0956 0.135 Uiso 0.55 1 calc PR B 1 C12' C 0.1297(15) 0.3062(18) -0.1556(13) 0.090(3) Uiso 0.45 1 d PD B 2 H12D H 0.1167 0.3800 -0.1791 0.135 Uiso 0.45 1 calc PR B 2 H12E H 0.2018 0.2643 -0.1755 0.135 Uiso 0.45 1 calc PR B 2 H12F H 0.1482 0.3217 -0.1086 0.135 Uiso 0.45 1 calc PR B 2 C13 C 0.2594(8) 0.0209(8) -0.2393(5) 0.0635(15) Uiso 0.60 1 d PD C 1 H13A H 0.2946 0.0922 -0.2601 0.076 Uiso 0.60 1 calc PR C 1 H13B H 0.1901 -0.0089 -0.2685 0.076 Uiso 0.60 1 calc PR C 1 C14 C 0.3593(8) -0.0658(7) -0.2342(4) 0.0635(15) Uiso 0.60 1 d PD C 1 H14A H 0.4236 -0.0387 -0.2014 0.076 Uiso 0.60 1 calc PR C 1 H14B H 0.3215 -0.1388 -0.2169 0.076 Uiso 0.60 1 calc PR C 1 C15 C 0.4623(13) -0.2159(7) -0.2949(6) 0.094(2) Uiso 0.60 1 d PD C 1 H15A H 0.5461 -0.2236 -0.2733 0.141 Uiso 0.60 1 calc PR C 1 H15B H 0.4674 -0.2447 -0.3408 0.141 Uiso 0.60 1 calc PR C 1 H15C H 0.3988 -0.2616 -0.2703 0.141 Uiso 0.60 1 calc PR C 1 C16 C 0.5403(10) -0.0239(10) -0.3062(6) 0.094(2) Uiso 0.60 1 d PD C 1 H16A H 0.5181 0.0578 -0.3147 0.141 Uiso 0.60 1 calc PR C 1 H16B H 0.5862 -0.0554 -0.3447 0.141 Uiso 0.60 1 calc PR C 1 H16C H 0.5950 -0.0289 -0.2666 0.141 Uiso 0.60 1 calc PR C 1 C13' C 0.2605(11) -0.0414(13) -0.2169(7) 0.0635(15) Uiso 0.40 1 d PD C 2 H13C H 0.2696 -0.1128 -0.1896 0.076 Uiso 0.40 1 calc PR C 2 H13D H 0.1999 -0.0587 -0.2536 0.076 Uiso 0.40 1 calc PR C 2 C14' C 0.3817(10) -0.0124(10) -0.2443(6) 0.0635(15) Uiso 0.40 1 d PD C 2 H14C H 0.4463 -0.0116 -0.2081 0.076 Uiso 0.40 1 calc PR C 2 H14D H 0.3771 0.0672 -0.2631 0.076 Uiso 0.40 1 calc PR C 2 C15' C 0.471(2) -0.2013(10) -0.2746(9) 0.094(2) Uiso 0.40 1 d PD C 2 H15D H 0.5370 -0.1900 -0.2404 0.141 Uiso 0.40 1 calc PR C 2 H15E H 0.5083 -0.2421 -0.3128 0.141 Uiso 0.40 1 calc PR C 2 H15F H 0.4009 -0.2478 -0.2563 0.141 Uiso 0.40 1 calc PR C 2 C16' C 0.5172(15) -0.0284(13) -0.3366(8) 0.094(2) Uiso 0.40 1 d PD C 2 H16D H 0.4862 0.0507 -0.3453 0.141 Uiso 0.40 1 calc PR C 2 H16E H 0.5285 -0.0696 -0.3789 0.141 Uiso 0.40 1 calc PR C 2 H16F H 0.5993 -0.0246 -0.3130 0.141 Uiso 0.40 1 calc PR C 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 0.0329(4) 0.0463(5) 0.0265(4) -0.0046(4) 0.0029(3) -0.0061(3) Ti2 0.0468(5) 0.0476(5) 0.0258(5) 0.0001(4) 0.0071(3) 0.0027(4) O1 0.0402(15) 0.0454(17) 0.0279(16) -0.0024(14) 0.0037(13) 0.0016(13) O2 0.0328(14) 0.0451(16) 0.0272(15) -0.0034(13) 0.0009(12) 0.0007(12) O3 0.0362(16) 0.062(2) 0.0385(17) -0.0071(16) 0.0088(14) -0.0128(14) O4 0.059(2) 0.0471(17) 0.0388(18) -0.0103(16) 0.0125(16) -0.0096(16) O5 0.086(3) 0.059(2) 0.0283(17) -0.0019(17) -0.0126(17) 0.0127(19) O6 0.070(2) 0.081(3) 0.039(2) -0.0004(19) 0.0229(18) 0.005(2) N1 0.062(3) 0.105(4) 0.071(3) -0.006(3) 0.006(3) 0.023(3) N2 0.092(3) 0.047(2) 0.045(3) 0.005(2) 0.008(2) -0.003(2) N3 0.035(2) 0.085(3) 0.050(3) -0.019(2) -0.0009(18) -0.012(2) N4 0.102(4) 0.103(4) 0.085(4) -0.014(3) 0.037(4) 0.020(4) C1 0.085(4) 0.048(3) 0.048(3) -0.019(3) 0.018(3) -0.017(3) C2 0.104(5) 0.074(4) 0.070(5) -0.001(4) 0.021(4) 0.027(4) C5 0.042(3) 0.120(5) 0.055(3) -0.020(4) 0.014(3) -0.033(3) C6 0.051(3) 0.120(5) 0.065(4) -0.033(4) 0.009(3) -0.040(3) C7 0.035(3) 0.122(5) 0.071(4) -0.022(4) -0.017(3) 0.011(3) C8 0.056(3) 0.109(5) 0.057(3) -0.037(4) -0.010(3) -0.015(3) C9 0.128(6) 0.076(4) 0.033(3) 0.002(3) -0.018(3) 0.032(4) C10 0.128(5) 0.070(4) 0.033(3) 0.012(3) 0.016(3) 0.025(4) C11 0.124(5) 0.067(4) 0.039(3) 0.002(3) 0.005(3) 0.035(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O4 1.857(3) . ? Ti1 O2 1.869(3) . ? Ti1 O1 1.869(3) . ? Ti1 O3 2.035(3) . ? Ti1 O2 2.060(3) 3 ? Ti1 N3 2.304(4) . ? Ti1 Ti2 2.9648(16) 3 ? Ti1 Ti1 2.974(2) 3 ? Ti1 Ti2 3.1757(13) . ? Ti2 O1 1.811(3) 3 ? Ti2 O6 1.845(3) . ? Ti2 O5 1.876(4) . ? Ti2 O3 2.047(3) . ? Ti2 O2 2.064(3) . ? Ti2 N2 2.351(5) . ? Ti2 Ti1 2.9648(16) 3 ? O1 Ti2 1.811(3) 3 ? O2 Ti1 2.060(3) 3 ? O3 C5 1.420(6) . ? O4 C1 1.417(5) . ? O5 C9 1.398(6) . ? O6 C13 1.410(9) . ? O6 C13' 1.427(11) . ? N1 C2 1.408(7) . ? N1 C4' 1.414(8) . ? N1 C3 1.447(9) . ? N1 C3' 1.495(9) . ? N1 C4 1.503(9) . ? N2 C12 1.446(9) . ? N2 C11 1.460(7) . ? N2 C12' 1.465(10) . ? N2 C10 1.508(7) . ? N3 C8 1.480(6) . ? N3 C6 1.485(7) . ? N3 C7 1.491(8) . ? N4 C15' 1.422(9) . ? N4 C14 1.433(8) . ? N4 C14' 1.438(9) . ? N4 C16 1.462(8) . ? N4 C16' 1.472(9) . ? N4 C15 1.489(8) . ? C1 C2 1.479(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C3' H3D 0.9800 . ? C3' H3E 0.9800 . ? C3' H3F 0.9800 . ? C4' H4D 0.9800 . ? C4' H4E 0.9800 . ? C4' H4F 0.9800 . ? C5 C6 1.511(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.503(9) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C12' H12D 0.9800 . ? C12' H12E 0.9800 . ? C12' H12F 0.9800 . ? C13 C14 1.445(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C13' C14' 1.422(10) . ? C13' H13C 0.9900 . ? C13' H13D 0.9900 . ? C14' H14C 0.9900 . ? C14' H14D 0.9900 . ? C15' H15D 0.9800 . ? C15' H15E 0.9800 . ? C15' H15F 0.9800 . ? C16' H16D 0.9800 . ? C16' H16E 0.9800 . ? C16' H16F 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 O4 Ti1 O2 106.63(15) . . ? O4 Ti1 O1 90.09(13) . . ? O2 Ti1 O1 109.39(13) . . ? O4 Ti1 O3 94.15(13) . . ? O2 Ti1 O3 77.29(13) . . ? O1 Ti1 O3 170.72(14) . . ? O4 Ti1 O2 168.58(13) . 3 ? O2 Ti1 O2 81.71(14) . 3 ? O1 Ti1 O2 79.63(11) . 3 ? O3 Ti1 O2 95.33(12) . 3 ? O4 Ti1 N3 89.83(16) . . ? O2 Ti1 N3 148.59(13) . . ? O1 Ti1 N3 96.85(15) . . ? O3 Ti1 N3 74.94(14) . . ? O2 Ti1 N3 86.51(15) 3 . ? O4 Ti1 Ti2 125.75(10) . 3 ? O2 Ti1 Ti2 96.33(10) . 3 ? O1 Ti1 Ti2 35.66(9) . 3 ? O3 Ti1 Ti2 139.24(10) . 3 ? O2 Ti1 Ti2 44.09(7) 3 3 ? N3 Ti1 Ti2 95.17(12) . 3 ? O4 Ti1 Ti1 149.17(12) . 3 ? O2 Ti1 Ti1 43.26(9) . 3 ? O1 Ti1 Ti1 94.82(10) . 3 ? O3 Ti1 Ti1 85.76(9) . 3 ? O2 Ti1 Ti1 38.45(9) 3 3 ? N3 Ti1 Ti1 119.61(12) . 3 ? Ti2 Ti1 Ti1 64.65(4) 3 3 ? O4 Ti1 Ti2 105.00(10) . . ? O2 Ti1 Ti2 38.28(8) . . ? O1 Ti1 Ti2 146.84(10) . . ? O3 Ti1 Ti2 39.07(9) . . ? O2 Ti1 Ti2 86.39(8) 3 . ? N3 Ti1 Ti2 112.25(11) . . ? Ti2 Ti1 Ti2 122.18(4) 3 . ? Ti1 Ti1 Ti2 57.53(3) 3 . ? O1 Ti2 O6 102.61(14) 3 . ? O1 Ti2 O5 93.85(15) 3 . ? O6 Ti2 O5 100.05(17) . . ? O1 Ti2 O3 101.99(14) 3 . ? O6 Ti2 O3 84.78(15) . . ? O5 Ti2 O3 162.05(14) . . ? O1 Ti2 O2 80.85(11) 3 . ? O6 Ti2 O2 157.56(16) . . ? O5 Ti2 O2 101.83(15) . . ? O3 Ti2 O2 72.85(12) . . ? O1 Ti2 N2 165.65(15) 3 . ? O6 Ti2 N2 89.14(16) . . ? O5 Ti2 N2 75.78(16) . . ? O3 Ti2 N2 87.09(16) . . ? O2 Ti2 N2 91.45(13) . . ? O1 Ti2 Ti1 37.00(8) 3 3 ? O6 Ti2 Ti1 134.35(12) . 3 ? O5 Ti2 Ti1 102.37(12) . 3 ? O3 Ti2 Ti1 85.80(9) . 3 ? O2 Ti2 Ti1 43.98(9) . 3 ? N2 Ti2 Ti1 134.79(11) . 3 ? O1 Ti2 Ti1 89.54(10) 3 . ? O6 Ti2 Ti1 123.45(13) . . ? O5 Ti2 Ti1 134.44(11) . . ? O3 Ti2 Ti1 38.79(8) . . ? O2 Ti2 Ti1 34.12(9) . . ? N2 Ti2 Ti1 90.79(11) . . ? Ti1 Ti2 Ti1 57.82(4) 3 . ? Ti2 O1 Ti1 107.33(14) 3 . ? Ti1 O2 Ti1 98.29(14) . 3 ? Ti1 O2 Ti2 107.59(13) . . ? Ti1 O2 Ti2 91.93(11) 3 . ? C5 O3 Ti1 122.9(3) . . ? C5 O3 Ti2 133.7(3) . . ? Ti1 O3 Ti2 102.14(13) . . ? C1 O4 Ti1 131.9(3) . . ? C9 O5 Ti2 125.9(4) . . ? C13 O6 C13' 34.7(6) . . ? C13 O6 Ti2 142.2(5) . . ? C13' O6 Ti2 126.9(5) . . ? C2 N1 C4' 122.1(7) . . ? C2 N1 C3 114.5(8) . . ? C4' N1 C3 104.1(13) . . ? C2 N1 C3' 110.4(7) . . ? C4' N1 C3' 109.6(7) . . ? C3 N1 C3' 5.5(14) . . ? C2 N1 C4 105.1(6) . . ? C4' N1 C4 18.1(9) . . ? C3 N1 C4 109.5(8) . . ? C3' N1 C4 114.6(15) . . ? C12 N2 C11 102.6(8) . . ? C12 N2 C12' 14.9(14) . . ? C11 N2 C12' 117.3(10) . . ? C12 N2 C10 116.4(9) . . ? C11 N2 C10 109.2(5) . . ? C12' N2 C10 106.7(11) . . ? C12 N2 Ti2 116.6(9) . . ? C11 N2 Ti2 112.6(3) . . ? C12' N2 Ti2 109.6(10) . . ? C10 N2 Ti2 99.8(3) . . ? C8 N3 C6 110.1(4) . . ? C8 N3 C7 108.3(5) . . ? C6 N3 C7 110.3(4) . . ? C8 N3 Ti1 111.5(3) . . ? C6 N3 Ti1 102.8(3) . . ? C7 N3 Ti1 113.6(3) . . ? C15' N4 C14 95.3(8) . . ? C15' N4 C14' 117.1(8) . . ? C14 N4 C14' 27.7(5) . . ? C15' N4 C16 102.8(12) . . ? C14 N4 C16 114.4(7) . . ? C14' N4 C16 91.7(7) . . ? C15' N4 C16' 111.5(8) . . ? C14 N4 C16' 134.2(8) . . ? C14' N4 C16' 107.3(7) . . ? C16 N4 C16' 25.9(9) . . ? C15' N4 C15 17.6(11) . . ? C14 N4 C15 108.5(6) . . ? C14' N4 C15 133.1(8) . . ? C16 N4 C15 106.4(6) . . ? C16' N4 C15 107.0(9) . . ? O4 C1 C2 113.9(5) . . ? O4 C1 H1A 108.8 . . ? C2 C1 H1A 108.8 . . ? O4 C1 H1B 108.8 . . ? C2 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? N1 C2 C1 116.6(5) . . ? N1 C2 H2A 108.1 . . ? C1 C2 H2A 108.1 . . ? N1 C2 H2B 108.1 . . ? C1 C2 H2B 108.1 . . ? H2A C2 H2B 107.3 . . ? N1 C3 H3A 109.7 . . ? N1 C3 H3B 109.8 . . ? N1 C3 H3C 108.9 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.6 . . ? N1 C4 H4C 109.3 . . ? N1 C3' H3D 109.0 . . ? N1 C3' H3E 109.4 . . ? H3D C3' H3E 109.5 . . ? N1 C3' H3F 110.0 . . ? H3D C3' H3F 109.5 . . ? H3E C3' H3F 109.5 . . ? N1 C4' H4D 109.4 . . ? N1 C4' H4E 109.5 . . ? H4D C4' H4E 109.5 . . ? N1 C4' H4F 109.6 . . ? H4D C4' H4F 109.5 . . ? H4E C4' H4F 109.5 . . ? O3 C5 C6 106.2(4) . . ? O3 C5 H5A 110.5 . . ? C6 C5 H5A 110.5 . . ? O3 C5 H5B 110.5 . . ? C6 C5 H5B 110.5 . . ? H5A C5 H5B 108.7 . . ? N3 C6 C5 109.4(4) . . ? N3 C6 H6A 109.8 . . ? C5 C6 H6A 109.8 . . ? N3 C6 H6B 109.8 . . ? C5 C6 H6B 109.8 . . ? H6A C6 H6B 108.2 . . ? N3 C7 H7A 109.5 . . ? N3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O5 C9 C10 109.0(5) . . ? O5 C9 H9A 109.9 . . ? C10 C9 H9A 109.9 . . ? O5 C9 H9B 109.9 . . ? C10 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? C9 C10 N2 108.2(4) . . ? C9 C10 H10A 110.1 . . ? N2 C10 H10A 110.1 . . ? C9 C10 H10B 110.1 . . ? N2 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? N2 C11 H11A 109.5 . . ? N2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 H12A 109.5 . . ? N2 C12 H12B 109.5 . . ? N2 C12 H12C 109.5 . . ? N2 C12' H12D 109.5 . . ? N2 C12' H12E 109.5 . . ? H12D C12' H12E 109.5 . . ? N2 C12' H12F 109.5 . . ? H12D C12' H12F 109.5 . . ? H12E C12' H12F 109.5 . . ? O6 C13 C14 111.7(7) . . ? O6 C13 H13A 109.3 . . ? C14 C13 H13A 109.3 . . ? O6 C13 H13B 109.3 . . ? C14 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? N4 C14 C13 114.7(7) . . ? N4 C14 H14A 108.6 . . ? C13 C14 H14A 108.6 . . ? N4 C14 H14B 108.6 . . ? C13 C14 H14B 108.6 . . ? H14A C14 H14B 107.6 . . ? N4 C15 H15A 109.5 . . ? N4 C15 H15B 109.5 . . ? N4 C15 H15C 109.5 . . ? N4 C16 H16A 109.5 . . ? N4 C16 H16B 109.5 . . ? N4 C16 H16C 109.5 . . ? C14' C13' O6 113.1(9) . . ? C14' C13' H13C 109.0 . . ? O6 C13' H13C 109.0 . . ? C14' C13' H13D 108.9 . . ? O6 C13' H13D 108.9 . . ? H13C C13' H13D 107.8 . . ? C13' C14' N4 113.8(9) . . ? C13' C14' H14C 108.8 . . ? N4 C14' H14C 108.8 . . ? C13' C14' H14D 108.8 . . ? N4 C14' H14D 108.8 . . ? H14C C14' H14D 107.7 . . ? N4 C15' H15D 109.5 . . ? N4 C15' H15E 109.5 . . ? H15D C15' H15E 109.5 . . ? N4 C15' H15F 109.5 . . ? H15D C15' H15F 109.5 . . ? H15E C15' H15F 109.5 . . ? N4 C16' H16D 109.5 . . ? N4 C16' H16E 109.5 . . ? H16D C16' H16E 109.5 . . ? N4 C16' H16F 109.5 . . ? H16D C16' H16F 109.5 . . ? H16E C16' H16F 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 O4 Ti1 Ti2 O1 -172.21(14) . . . 3 ? O2 Ti1 Ti2 O1 -74.23(17) . . . 3 ? O1 Ti1 Ti2 O1 -57.8(2) . . . 3 ? O3 Ti1 Ti2 O1 109.97(18) . . . 3 ? O2 Ti1 Ti2 O1 6.95(12) 3 . . 3 ? N3 Ti1 Ti2 O1 91.69(16) . . . 3 ? Ti2 Ti1 Ti2 O1 -20.18(10) 3 . . 3 ? Ti1 Ti1 Ti2 O1 -20.18(10) 3 . . 3 ? O4 Ti1 Ti2 O6 82.93(18) . . . . ? O2 Ti1 Ti2 O6 -179.1(2) . . . . ? O1 Ti1 Ti2 O6 -162.7(2) . . . . ? O3 Ti1 Ti2 O6 5.1(2) . . . . ? O2 Ti1 Ti2 O6 -97.91(16) 3 . . . ? N3 Ti1 Ti2 O6 -13.2(2) . . . . ? Ti2 Ti1 Ti2 O6 -125.04(14) 3 . . . ? Ti1 Ti1 Ti2 O6 -125.04(14) 3 . . . ? O4 Ti1 Ti2 O5 -77.26(19) . . . . ? O2 Ti1 Ti2 O5 20.7(2) . . . . ? O1 Ti1 Ti2 O5 37.1(2) . . . . ? O3 Ti1 Ti2 O5 -155.1(2) . . . . ? O2 Ti1 Ti2 O5 101.90(17) 3 . . . ? N3 Ti1 Ti2 O5 -173.4(2) . . . . ? Ti2 Ti1 Ti2 O5 74.77(16) 3 . . . ? Ti1 Ti1 Ti2 O5 74.77(16) 3 . . . ? O4 Ti1 Ti2 O3 77.81(18) . . . . ? O2 Ti1 Ti2 O3 175.8(2) . . . . ? O1 Ti1 Ti2 O3 -167.8(2) . . . . ? O2 Ti1 Ti2 O3 -103.02(17) 3 . . . ? N3 Ti1 Ti2 O3 -18.3(2) . . . . ? Ti2 Ti1 Ti2 O3 -130.15(16) 3 . . . ? Ti1 Ti1 Ti2 O3 -130.15(16) 3 . . . ? O4 Ti1 Ti2 O2 -97.98(18) . . . . ? O1 Ti1 Ti2 O2 16.4(2) . . . . ? O3 Ti1 Ti2 O2 -175.8(2) . . . . ? O2 Ti1 Ti2 O2 81.19(17) 3 . . . ? N3 Ti1 Ti2 O2 165.9(2) . . . . ? Ti2 Ti1 Ti2 O2 54.06(14) 3 . . . ? Ti1 Ti1 Ti2 O2 54.06(14) 3 . . . ? O4 Ti1 Ti2 N2 -6.56(15) . . . . ? O2 Ti1 Ti2 N2 91.42(19) . . . . ? O1 Ti1 Ti2 N2 107.8(2) . . . . ? O3 Ti1 Ti2 N2 -84.38(19) . . . . ? O2 Ti1 Ti2 N2 172.60(14) 3 . . . ? N3 Ti1 Ti2 N2 -102.66(17) . . . . ? Ti2 Ti1 Ti2 N2 145.47(12) 3 . . . ? Ti1 Ti1 Ti2 N2 145.47(12) 3 . . . ? O4 Ti1 Ti2 Ti1 -152.03(12) . . . 3 ? O2 Ti1 Ti2 Ti1 -54.06(14) . . . 3 ? O1 Ti1 Ti2 Ti1 -37.65(17) . . . 3 ? O3 Ti1 Ti2 Ti1 130.15(16) . . . 3 ? O2 Ti1 Ti2 Ti1 27.13(8) 3 . . 3 ? N3 Ti1 Ti2 Ti1 111.87(14) . . . 3 ? Ti2 Ti1 Ti2 Ti1 0.0 3 . . 3 ? O4 Ti1 O1 Ti2 -179.16(17) . . . 3 ? O2 Ti1 O1 Ti2 73.15(18) . . . 3 ? O3 Ti1 O1 Ti2 -61.9(9) . . . 3 ? O2 Ti1 O1 Ti2 -4.16(14) 3 . . 3 ? N3 Ti1 O1 Ti2 -89.32(18) . . . 3 ? Ti1 Ti1 O1 Ti2 31.32(15) 3 . . 3 ? Ti2 Ti1 O1 Ti2 62.5(2) . . . 3 ? O4 Ti1 O2 Ti1 -172.00(11) . . . 3 ? O1 Ti1 O2 Ti1 -75.87(14) . . . 3 ? O3 Ti1 O2 Ti1 97.42(13) . . . 3 ? O2 Ti1 O2 Ti1 0.0 3 . . 3 ? N3 Ti1 O2 Ti1 69.1(3) . . . 3 ? Ti2 Ti1 O2 Ti1 -41.72(9) 3 . . 3 ? Ti2 Ti1 O2 Ti1 94.70(14) . . . 3 ? O4 Ti1 O2 Ti2 93.30(15) . . . . ? O1 Ti1 O2 Ti2 -170.57(13) . . . . ? O3 Ti1 O2 Ti2 2.72(14) . . . . ? O2 Ti1 O2 Ti2 -94.70(14) 3 . . . ? N3 Ti1 O2 Ti2 -25.6(3) . . . . ? Ti2 Ti1 O2 Ti2 -136.42(11) 3 . . . ? Ti1 Ti1 O2 Ti2 -94.70(14) 3 . . . ? O1 Ti2 O2 Ti1 102.90(17) 3 . . . ? O6 Ti2 O2 Ti1 2.0(5) . . . . ? O5 Ti2 O2 Ti1 -165.04(15) . . . . ? O3 Ti2 O2 Ti1 -2.76(14) . . . . ? N2 Ti2 O2 Ti1 -89.27(17) . . . . ? Ti1 Ti2 O2 Ti1 99.32(16) 3 . . . ? O1 Ti2 O2 Ti1 3.58(12) 3 . . 3 ? O6 Ti2 O2 Ti1 -97.3(4) . . . 3 ? O5 Ti2 O2 Ti1 95.64(14) . . . 3 ? O3 Ti2 O2 Ti1 -102.08(14) . . . 3 ? N2 Ti2 O2 Ti1 171.41(15) . . . 3 ? Ti1 Ti2 O2 Ti1 -99.32(16) . . . 3 ? O4 Ti1 O3 C5 82.2(4) . . . . ? O2 Ti1 O3 C5 -171.7(4) . . . . ? O1 Ti1 O3 C5 -34.8(10) . . . . ? O2 Ti1 O3 C5 -91.5(4) 3 . . . ? N3 Ti1 O3 C5 -6.5(4) . . . . ? Ti2 Ti1 O3 C5 -86.8(4) 3 . . . ? Ti1 Ti1 O3 C5 -128.8(4) 3 . . . ? Ti2 Ti1 O3 C5 -169.0(5) . . . . ? O4 Ti1 O3 Ti2 -108.80(16) . . . . ? O2 Ti1 O3 Ti2 -2.67(14) . . . . ? O1 Ti1 O3 Ti2 134.2(8) . . . . ? O2 Ti1 O3 Ti2 77.57(15) 3 . . . ? N3 Ti1 O3 Ti2 162.50(19) . . . . ? Ti2 Ti1 O3 Ti2 82.25(19) 3 . . . ? Ti1 Ti1 O3 Ti2 40.29(12) 3 . . . ? O1 Ti2 O3 C5 93.4(5) 3 . . . ? O6 Ti2 O3 C5 -8.5(5) . . . . ? O5 Ti2 O3 C5 -115.1(6) . . . . ? O2 Ti2 O3 C5 169.7(5) . . . . ? N2 Ti2 O3 C5 -97.9(5) . . . . ? Ti1 Ti2 O3 C5 126.8(5) 3 . . . ? Ti1 Ti2 O3 C5 167.3(6) . . . . ? O1 Ti2 O3 Ti1 -73.90(15) 3 . . . ? O6 Ti2 O3 Ti1 -175.72(17) . . . . ? O5 Ti2 O3 Ti1 77.6(5) . . . . ? O2 Ti2 O3 Ti1 2.47(13) . . . . ? N2 Ti2 O3 Ti1 94.88(16) . . . . ? Ti1 Ti2 O3 Ti1 -40.44(12) 3 . . . ? O2 Ti1 O4 C1 108.1(4) . . . . ? O1 Ti1 O4 C1 -2.2(5) . . . . ? O3 Ti1 O4 C1 -173.9(4) . . . . ? O2 Ti1 O4 C1 -27.8(9) 3 . . . ? N3 Ti1 O4 C1 -99.0(5) . . . . ? Ti2 Ti1 O4 C1 -2.8(5) 3 . . . ? Ti1 Ti1 O4 C1 97.4(5) 3 . . . ? Ti2 Ti1 O4 C1 147.9(4) . . . . ? O1 Ti2 O5 C9 -176.3(4) 3 . . . ? O6 Ti2 O5 C9 -72.8(4) . . . . ? O3 Ti2 O5 C9 31.6(7) . . . . ? O2 Ti2 O5 C9 102.2(4) . . . . ? N2 Ti2 O5 C9 13.8(4) . . . . ? Ti1 Ti2 O5 C9 147.3(4) 3 . . . ? Ti1 Ti2 O5 C9 90.5(4) . . . . ? O1 Ti2 O6 C13 77.1(7) 3 . . . ? O5 Ti2 O6 C13 -19.2(7) . . . . ? O3 Ti2 O6 C13 178.2(7) . . . . ? O2 Ti2 O6 C13 173.7(7) . . . . ? N2 Ti2 O6 C13 -94.6(7) . . . . ? Ti1 Ti2 O6 C13 99.3(7) 3 . . . ? Ti1 Ti2 O6 C13 175.0(7) . . . . ? O1 Ti2 O6 C13' 32.3(9) 3 . . . ? O5 Ti2 O6 C13' -64.0(9) . . . . ? O3 Ti2 O6 C13' 133.5(9) . . . . ? O2 Ti2 O6 C13' 128.9(9) . . . . ? N2 Ti2 O6 C13' -139.4(9) . . . . ? Ti1 Ti2 O6 C13' 54.6(9) 3 . . . ? Ti1 Ti2 O6 C13' 130.3(9) . . . . ? O1 Ti2 N2 C12 156.3(9) 3 . . . ? O6 Ti2 N2 C12 -58.4(9) . . . . ? O5 Ti2 N2 C12 -159.0(9) . . . . ? O3 Ti2 N2 C12 26.4(9) . . . . ? O2 Ti2 N2 C12 99.1(9) . . . . ? Ti1 Ti2 N2 C12 107.5(9) 3 . . . ? Ti1 Ti2 N2 C12 65.0(9) . . . . ? O1 Ti2 N2 C11 38.1(8) 3 . . . ? O6 Ti2 N2 C11 -176.6(4) . . . . ? O5 Ti2 N2 C11 82.8(4) . . . . ? O3 Ti2 N2 C11 -91.7(4) . . . . ? O2 Ti2 N2 C11 -19.0(4) . . . . ? Ti1 Ti2 N2 C11 -10.6(5) 3 . . . ? Ti1 Ti2 N2 C11 -53.1(4) . . . . ? O1 Ti2 N2 C12' 170.6(11) 3 . . . ? O6 Ti2 N2 C12' -44.1(10) . . . . ? O5 Ti2 N2 C12' -144.7(10) . . . . ? O3 Ti2 N2 C12' 40.7(10) . . . . ? O2 Ti2 N2 C12' 113.5(10) . . . . ? Ti1 Ti2 N2 C12' 121.9(10) 3 . . . ? Ti1 Ti2 N2 C12' 79.4(10) . . . . ? O1 Ti2 N2 C10 -77.6(7) 3 . . . ? O6 Ti2 N2 C10 67.7(4) . . . . ? O5 Ti2 N2 C10 -32.9(3) . . . . ? O3 Ti2 N2 C10 152.6(3) . . . . ? O2 Ti2 N2 C10 -134.7(3) . . . . ? Ti1 Ti2 N2 C10 -126.3(3) 3 . . . ? Ti1 Ti2 N2 C10 -168.8(3) . . . . ? O4 Ti1 N3 C8 54.3(4) . . . . ? O2 Ti1 N3 C8 177.3(4) . . . . ? O1 Ti1 N3 C8 -35.7(4) . . . . ? O3 Ti1 N3 C8 148.7(4) . . . . ? O2 Ti1 N3 C8 -114.8(4) 3 . . . ? Ti2 Ti1 N3 C8 -71.5(4) 3 . . . ? Ti1 Ti1 N3 C8 -135.2(4) 3 . . . ? Ti2 Ti1 N3 C8 160.5(4) . . . . ? O4 Ti1 N3 C6 -63.6(3) . . . . ? O2 Ti1 N3 C6 59.3(5) . . . . ? O1 Ti1 N3 C6 -153.7(3) . . . . ? O3 Ti1 N3 C6 30.7(3) . . . . ? O2 Ti1 N3 C6 127.2(3) 3 . . . ? Ti2 Ti1 N3 C6 170.5(3) 3 . . . ? Ti1 Ti1 N3 C6 106.8(3) 3 . . . ? Ti2 Ti1 N3 C6 42.5(4) . . . . ? O4 Ti1 N3 C7 177.1(3) . . . . ? O2 Ti1 N3 C7 -59.9(5) . . . . ? O1 Ti1 N3 C7 87.0(3) . . . . ? O3 Ti1 N3 C7 -88.5(4) . . . . ? O2 Ti1 N3 C7 7.9(3) 3 . . . ? Ti2 Ti1 N3 C7 51.2(3) 3 . . . ? Ti1 Ti1 N3 C7 -12.5(4) 3 . . . ? Ti2 Ti1 N3 C7 -76.7(3) . . . . ? Ti1 O4 C1 C2 -106.8(5) . . . . ? C4' N1 C2 C1 -164.2(10) . . . . ? C3 N1 C2 C1 68.7(15) . . . . ? C3' N1 C2 C1 64.9(15) . . . . ? C4 N1 C2 C1 -171.0(8) . . . . ? O4 C1 C2 N1 57.5(6) . . . . ? Ti1 O3 C5 C6 -19.4(7) . . . . ? Ti2 O3 C5 C6 175.5(4) . . . . ? C8 N3 C6 C5 -170.1(5) . . . . ? C7 N3 C6 C5 70.4(6) . . . . ? Ti1 N3 C6 C5 -51.1(6) . . . . ? O3 C5 C6 N3 47.8(7) . . . . ? Ti2 O5 C9 C10 10.4(6) . . . . ? O5 C9 C10 N2 -41.8(6) . . . . ? C12 N2 C10 C9 173.3(9) . . . . ? C11 N2 C10 C9 -71.2(6) . . . . ? C12' N2 C10 C9 161.0(11) . . . . ? Ti2 N2 C10 C9 47.0(5) . . . . ? C13' O6 C13 C14 -34.9(10) . . . . ? Ti2 O6 C13 C14 -116.7(8) . . . . ? C15' N4 C14 C13 -159.5(12) . . . . ? C14' N4 C14 C13 56.6(14) . . . . ? C16 N4 C14 C13 93.9(11) . . . . ? C16' N4 C14 C13 73.4(15) . . . . ? C15 N4 C14 C13 -147.6(9) . . . . ? O6 C13 C14 N4 -174.7(7) . . . . ? C13 O6 C13' C14' 53.5(12) . . . . ? Ti2 O6 C13' C14' -175.9(9) . . . . ? O6 C13' C14' N4 -167.9(10) . . . . ? C15' N4 C14' C13' -76.1(17) . . . . ? C14 N4 C14' C13' -35.0(12) . . . . ? C16 N4 C14' C13' 178.5(12) . . . . ? C16' N4 C14' C13' 157.6(13) . . . . ? C15 N4 C14' C13' -67.1(17) . . . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 25.15 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.605 _refine_diff_density_min -0.579 _refine_diff_density_rms 0.084