# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_publication_text _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author_name 'Thomas Huhn' _publ_contact_author_address ;Universit\"at Konstanz Fachbereich Chemie D-78457 Konstanz ; _publ_contact_author_email thomas.huhn@uni-konstanz.de _publ_contact_author_fax +49-7531-884424 _publ_author_address ;Universit\"at Konstanz Fachbereich Chemie D-78457 Konstanz ; loop_ _publ_author_name 'Thomas Huhn' 'Timo A. Immel' A.-K.Spate 'Ulrich Groth' P.Ohlschlager # Attachment 'aks05_pub.cif' data_aks05 _database_code_depnum_ccdc_archive 'CCDC 804775' #TrackingRef 'aks05_pub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H36 N2 O4 Ti' _chemical_formula_sum 'C24 H36 N2 O4 Ti' _chemical_formula_weight 464.45 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2918(7) _cell_length_b 11.8315(8) _cell_length_c 18.3210(12) _cell_angle_alpha 98.082(5) _cell_angle_beta 102.992(5) _cell_angle_gamma 97.181(5) _cell_volume 2330.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 39932 _cell_measurement_theta_min 1.78 _cell_measurement_theta_max 27.28 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 0.400 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8507 _exptl_absorpt_correction_T_max 0.9471 _exptl_absorpt_process_details ; 'X-SHAPE 2.07 (03-Aug-2005) Stoe & Cie, Darmstadt, Germany' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'plane graphite' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33475 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 26.86 _reflns_number_total 9894 _reflns_number_gt 8287 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0478P)^2^+0.9372P] 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 9894 _refine_ls_number_parameters 570 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0892 _refine_ls_wR_factor_gt 0.0859 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.020 _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 C13 C 0.10761(14) 0.46993(15) 0.94752(9) 0.0175(3) Uani 1 1 d . . . H13A H 0.0907 0.5354 0.9815 0.021 Uiso 1 1 calc R . . H13B H 0.1147 0.4048 0.9759 0.021 Uiso 1 1 calc R . . C14 C 0.42849(15) 0.61234(15) 0.78400(9) 0.0174(3) Uani 1 1 d . . . H14A H 0.3996 0.6711 0.7537 0.021 Uiso 1 1 calc R . . H14B H 0.4632 0.5580 0.7516 0.021 Uiso 1 1 calc R . . C15 C 0.35778(15) 0.45346(14) 0.84297(10) 0.0175(3) Uani 1 1 d . . . H15A H 0.4349 0.4837 0.8827 0.021 Uiso 1 1 calc R . . H15B H 0.3738 0.3894 0.8074 0.021 Uiso 1 1 calc R . . C16 C 0.25750(15) 0.40865(14) 0.87954(10) 0.0178(3) Uani 1 1 d . . . H16A H 0.1824 0.3726 0.8395 0.021 Uiso 1 1 calc R . . H16B H 0.2852 0.3489 0.9093 0.021 Uiso 1 1 calc R . . C17 C 0.23329(15) 0.49541(15) 0.72650(9) 0.0194(3) Uani 1 1 d . . . H17A H 0.2048 0.5574 0.7004 0.029 Uiso 1 1 calc R . . H17B H 0.1625 0.4461 0.7345 0.029 Uiso 1 1 calc R . . H17C H 0.2759 0.4489 0.6954 0.029 Uiso 1 1 calc R . . C18 C 0.32216(15) 0.53121(16) 1.00465(9) 0.0205(3) Uani 1 1 d . . . H18A H 0.3027 0.5954 1.0376 0.031 Uiso 1 1 calc R . . H18B H 0.4041 0.5529 0.9962 0.031 Uiso 1 1 calc R . . H18C H 0.3212 0.4626 1.0290 0.031 Uiso 1 1 calc R . . C19 C -0.30149(18) 0.21739(17) 0.82093(11) 0.0298(4) Uani 1 1 d . . . H19A H -0.3362 0.1757 0.7688 0.045 Uiso 1 1 calc R . . H19B H -0.3665 0.2490 0.8407 0.045 Uiso 1 1 calc R . . H19C H -0.2668 0.1641 0.8531 0.045 Uiso 1 1 calc R . . C20 C -0.14233(15) 0.54178(16) 0.69885(10) 0.0214(4) Uani 1 1 d . . . H20A H -0.0658 0.5550 0.6823 0.032 Uiso 1 1 calc R . . H20B H -0.1635 0.6163 0.7180 0.032 Uiso 1 1 calc R . . H20C H -0.2089 0.5006 0.6557 0.032 Uiso 1 1 calc R . . C21 C 0.57708(16) 0.85206(16) 1.04810(10) 0.0228(4) Uani 1 1 d . . . H21A H 0.5302 0.7958 1.0697 0.034 Uiso 1 1 calc R . . H21B H 0.5289 0.9132 1.0358 0.034 Uiso 1 1 calc R . . H21C H 0.6547 0.8861 1.0852 0.034 Uiso 1 1 calc R . . C22 C 0.87921(16) 0.76426(19) 0.89050(12) 0.0311(4) Uani 1 1 d . . . H22A H 0.9345 0.8134 0.9359 0.047 Uiso 0.50 1 calc PR . . H22B H 0.8822 0.8006 0.8459 0.047 Uiso 0.50 1 calc PR . . H22C H 0.9052 0.6884 0.8833 0.047 Uiso 0.50 1 calc PR . . H22D H 0.8801 0.7215 0.8408 0.047 Uiso 0.50 1 calc PR . . H22E H 0.9324 0.7343 0.9308 0.047 Uiso 0.50 1 calc PR . . H22F H 0.9094 0.8465 0.8935 0.047 Uiso 0.50 1 calc PR . . C23 C 0.12773(16) 0.78594(16) 0.74481(10) 0.0230(4) Uani 1 1 d . . . H23A H 0.1592 0.8472 0.7199 0.034 Uiso 1 1 calc R . . H23B H 0.0591 0.8085 0.7650 0.034 Uiso 1 1 calc R . . H23C H 0.0990 0.7140 0.7077 0.034 Uiso 1 1 calc R . . C24 C 0.20917(17) 0.86250(15) 0.98520(10) 0.0234(4) Uani 1 1 d . . . H24A H 0.1649 0.8812 1.0245 0.035 Uiso 1 1 calc R . . H24B H 0.1918 0.9121 0.9468 0.035 Uiso 1 1 calc R . . H24C H 0.2979 0.8754 1.0085 0.035 Uiso 1 1 calc R . . C113 C 0.79608(14) 0.85296(14) 0.63846(9) 0.0157(3) Uani 1 1 d . . . H11A H 0.8514 0.9161 0.6768 0.019 Uiso 1 1 calc R . . H11B H 0.8254 0.7796 0.6477 0.019 Uiso 1 1 calc R . . C114 C 0.64501(14) 0.84895(14) 0.33267(9) 0.0162(3) Uani 1 1 d . . . H11C H 0.6110 0.9120 0.3089 0.019 Uiso 1 1 calc R . . H11D H 0.5899 0.7755 0.3071 0.019 Uiso 1 1 calc R . . C115 C 0.72875(15) 0.97551(14) 0.45670(9) 0.0161(3) Uani 1 1 d . . . H11E H 0.6920 1.0444 0.4447 0.019 Uiso 1 1 calc R . . H11F H 0.8066 0.9787 0.4402 0.019 Uiso 1 1 calc R . . C116 C 0.75582(15) 0.97718(14) 0.54186(9) 0.0154(3) Uani 1 1 d . . . H11G H 0.8157 1.0471 0.5687 0.018 Uiso 1 1 calc R . . H11H H 0.6791 0.9804 0.5591 0.018 Uiso 1 1 calc R . . C117 C 0.51394(14) 0.88226(15) 0.41622(10) 0.0188(3) Uani 1 1 d . . . H11I H 0.4585 0.8100 0.3911 0.028 Uiso 1 1 calc R . . H11J H 0.4901 0.9451 0.3894 0.028 Uiso 1 1 calc R . . H11K H 0.5083 0.9005 0.4691 0.028 Uiso 1 1 calc R . . C118 C 0.94029(14) 0.88767(15) 0.56359(9) 0.0176(3) Uani 1 1 d . . . H11L H 0.9724 0.8168 0.5739 0.026 Uiso 1 1 calc R . . H11M H 0.9841 0.9524 0.6040 0.026 Uiso 1 1 calc R . . H11N H 0.9524 0.9040 0.5146 0.026 Uiso 1 1 calc R . . C119 C 0.33798(15) 0.71177(16) 0.54683(10) 0.0214(3) Uani 1 1 d . . . H11O H 0.3355 0.7391 0.4985 0.032 Uiso 1 1 calc R . . H11P H 0.2621 0.7225 0.5625 0.032 Uiso 1 1 calc R . . H11Q H 0.3452 0.6295 0.5404 0.032 Uiso 1 1 calc R . . C120 C 0.51496(16) 0.94869(15) 0.80950(9) 0.0200(3) Uani 1 1 d . . . H12A H 0.4408 0.9066 0.8187 0.030 Uiso 1 1 calc R . . H12B H 0.5054 1.0297 0.8085 0.030 Uiso 1 1 calc R . . H12C H 0.5866 0.9449 0.8502 0.030 Uiso 1 1 calc R . . C121 C 1.05704(14) 0.71567(15) 0.39265(10) 0.0183(3) Uani 1 1 d . . . H12D H 1.0716 0.7495 0.4465 0.028 Uiso 1 1 calc R . . H12E H 1.1352 0.7235 0.3775 0.028 Uiso 1 1 calc R . . H12F H 1.0219 0.6336 0.3848 0.028 Uiso 1 1 calc R . . C122 C 0.94756(17) 0.93059(17) 0.17407(10) 0.0243(4) Uani 1 1 d . . . H12G H 1.0296 0.9779 0.1909 0.036 Uiso 1 1 calc R . . H12H H 0.8869 0.9784 0.1546 0.036 Uiso 1 1 calc R . . H12I H 0.9473 0.8667 0.1337 0.036 Uiso 1 1 calc R . . C123 C 0.47954(15) 0.53789(16) 0.39267(11) 0.0234(4) Uani 1 1 d . . . H12J H 0.4395 0.4981 0.3407 0.035 Uiso 1 1 calc R . . H12K H 0.4223 0.5816 0.4129 0.035 Uiso 1 1 calc R . . H12L H 0.5032 0.4808 0.4248 0.035 Uiso 1 1 calc R . . C124 C 0.87901(16) 0.55852(15) 0.51401(10) 0.0217(4) Uani 1 1 d . . . H12M H 0.9023 0.5150 0.5553 0.033 Uiso 1 1 calc R . . H12N H 0.9501 0.6145 0.5131 0.033 Uiso 1 1 calc R . . H12O H 0.8519 0.5049 0.4653 0.033 Uiso 1 1 calc R . . N1 N 0.31932(12) 0.54665(12) 0.80124(7) 0.0149(3) Uani 1 1 d . . . N2 N 0.22885(12) 0.50507(12) 0.93038(8) 0.0155(3) Uani 1 1 d . . . N101 N 0.80688(12) 0.87225(12) 0.56103(7) 0.0141(3) Uani 1 1 d . . . N102 N 0.64247(12) 0.86890(12) 0.41482(8) 0.0149(3) Uani 1 1 d . . . O3 O 0.17027(10) 0.74572(10) 0.95041(7) 0.0193(2) Uani 1 1 d . . . O4 O 0.22232(10) 0.76882(10) 0.80477(7) 0.0196(2) Uani 1 1 d . . . O103 O 0.78222(11) 0.61758(10) 0.52596(7) 0.0193(2) Uani 1 1 d . . . O104 O 0.58549(10) 0.61435(10) 0.39214(7) 0.0188(2) Uani 1 1 d . . . C1 C 0.50667(14) 0.72796(14) 0.91781(9) 0.0148(3) Uani 1 1 d . . . C2 C 0.53059(14) 0.67266(14) 0.85112(9) 0.0155(3) Uani 1 1 d . . . C3 C 0.65186(15) 0.68353(15) 0.84392(10) 0.0186(3) Uani 1 1 d . . . H3 H 0.6683 0.6446 0.7992 0.022 Uiso 1 1 calc R . . C4 C 0.74930(15) 0.74959(15) 0.90027(10) 0.0208(3) Uani 1 1 d . . . C5 C 0.72291(15) 0.80251(15) 0.96635(10) 0.0193(3) Uani 1 1 d . . . H5 H 0.7885 0.8473 1.0057 0.023 Uiso 1 1 calc R . . C6 C 0.60392(14) 0.79221(14) 0.97688(9) 0.0163(3) Uani 1 1 d . . . C7 C -0.01677(14) 0.49727(14) 0.81994(9) 0.0145(3) Uani 1 1 d . . . C8 C -0.12521(14) 0.47050(15) 0.76086(9) 0.0169(3) Uani 1 1 d . . . C9 C -0.21517(15) 0.38015(15) 0.76301(10) 0.0198(3) Uani 1 1 d . . . H9 H -0.2887 0.3622 0.7234 0.024 Uiso 1 1 calc R . . C10 C -0.20128(15) 0.31496(15) 0.82131(10) 0.0204(3) Uani 1 1 d . . . C11 C -0.09342(15) 0.34277(14) 0.87884(9) 0.0178(3) Uani 1 1 d . . . H11 H -0.0819 0.2987 0.9187 0.021 Uiso 1 1 calc R . . C12 C -0.00122(14) 0.43400(14) 0.87959(9) 0.0158(3) Uani 1 1 d . . . C101 C 0.85307(14) 0.78482(13) 0.36129(9) 0.0139(3) Uani 1 1 d . . . C102 C 0.77025(14) 0.84318(14) 0.31797(9) 0.0146(3) Uani 1 1 d . . . C103 C 0.80271(15) 0.89152(14) 0.25849(9) 0.0165(3) Uani 1 1 d . . . H103 H 0.7467 0.9317 0.2296 0.020 Uiso 1 1 calc R . . C104 C 0.91488(15) 0.88248(14) 0.24033(9) 0.0173(3) Uani 1 1 d . . . C105 C 0.99645(15) 0.82548(14) 0.28498(9) 0.0171(3) Uani 1 1 d . . . H105 H 1.0737 0.8191 0.2737 0.021 Uiso 1 1 calc R . . C106 C 0.96871(14) 0.77777(14) 0.34527(9) 0.0149(3) Uani 1 1 d . . . C107 C 0.56614(14) 0.78511(13) 0.59443(9) 0.0144(3) Uani 1 1 d . . . C108 C 0.44716(14) 0.77958(14) 0.60677(9) 0.0156(3) Uani 1 1 d . . . C109 C 0.43393(15) 0.83466(14) 0.67619(9) 0.0167(3) Uani 1 1 d . . . H109 H 0.3536 0.8313 0.6845 0.020 Uiso 1 1 calc R . . C110 C 0.53351(15) 0.89441(14) 0.73391(9) 0.0169(3) Uani 1 1 d . . . C111 C 0.65025(15) 0.90085(14) 0.71952(9) 0.0164(3) Uani 1 1 d . . . H111 H 0.7195 0.9425 0.7576 0.020 Uiso 1 1 calc R . . C112 C 0.66782(14) 0.84770(14) 0.65064(9) 0.0151(3) Uani 1 1 d . . . O1 O 0.39147(10) 0.72347(10) 0.92640(6) 0.0160(2) Uani 1 1 d . . . O2 O 0.06971(10) 0.58475(10) 0.81840(6) 0.0157(2) Uani 1 1 d . . . O101 O 0.82398(10) 0.73402(10) 0.41712(6) 0.0147(2) Uani 1 1 d . . . O102 O 0.58075(10) 0.73019(10) 0.52846(6) 0.0154(2) Uani 1 1 d . . . Ti1 Ti 0.69840(2) 0.71230(2) 0.470353(16) 0.01263(7) Uani 1 1 d . . . Ti2 Ti 0.22549(2) 0.66897(2) 0.873359(16) 0.01310(7) Uani 1 1 d . . . 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 C13 0.0152(7) 0.0231(8) 0.0152(7) 0.0060(6) 0.0053(6) 0.0012(6) C14 0.0173(8) 0.0210(8) 0.0133(7) 0.0010(6) 0.0055(6) 0.0001(6) C15 0.0164(7) 0.0161(8) 0.0208(8) 0.0023(6) 0.0058(6) 0.0044(6) C16 0.0172(7) 0.0155(8) 0.0217(8) 0.0043(7) 0.0055(6) 0.0036(6) C17 0.0183(8) 0.0208(8) 0.0150(8) -0.0031(6) 0.0014(6) 0.0000(6) C18 0.0172(8) 0.0258(9) 0.0165(8) 0.0051(7) -0.0004(6) 0.0022(7) C19 0.0260(9) 0.0307(10) 0.0274(10) 0.0039(8) 0.0049(8) -0.0108(8) C20 0.0158(8) 0.0285(9) 0.0186(8) 0.0067(7) 0.0013(6) 0.0005(7) C21 0.0178(8) 0.0291(9) 0.0172(8) -0.0030(7) 0.0020(6) 0.0002(7) C22 0.0164(8) 0.0364(11) 0.0384(11) -0.0029(9) 0.0094(8) 0.0017(8) C23 0.0207(8) 0.0224(9) 0.0262(9) 0.0104(7) 0.0029(7) 0.0034(7) C24 0.0280(9) 0.0190(9) 0.0228(9) -0.0009(7) 0.0077(7) 0.0046(7) C113 0.0129(7) 0.0200(8) 0.0128(7) 0.0019(6) 0.0019(6) 0.0013(6) C114 0.0147(7) 0.0191(8) 0.0147(7) 0.0039(6) 0.0020(6) 0.0046(6) C115 0.0177(7) 0.0133(7) 0.0175(8) 0.0027(6) 0.0046(6) 0.0025(6) C116 0.0172(7) 0.0120(7) 0.0169(8) 0.0011(6) 0.0046(6) 0.0031(6) C117 0.0147(7) 0.0210(8) 0.0220(8) 0.0049(7) 0.0046(6) 0.0066(6) C118 0.0126(7) 0.0198(8) 0.0192(8) 0.0004(6) 0.0041(6) 0.0010(6) C119 0.0138(7) 0.0242(9) 0.0246(9) 0.0005(7) 0.0048(7) 0.0015(6) C120 0.0237(8) 0.0203(8) 0.0171(8) 0.0025(7) 0.0084(7) 0.0024(7) C121 0.0148(7) 0.0215(8) 0.0199(8) 0.0045(7) 0.0048(6) 0.0056(6) C122 0.0244(9) 0.0314(10) 0.0178(8) 0.0081(7) 0.0057(7) 0.0026(7) C123 0.0173(8) 0.0215(9) 0.0273(9) -0.0011(7) 0.0035(7) -0.0032(7) C124 0.0231(8) 0.0216(9) 0.0258(9) 0.0089(7) 0.0100(7) 0.0108(7) N1 0.0142(6) 0.0150(7) 0.0138(6) 0.0006(5) 0.0022(5) -0.0001(5) N2 0.0123(6) 0.0186(7) 0.0148(6) 0.0025(5) 0.0025(5) 0.0019(5) N101 0.0116(6) 0.0158(7) 0.0150(6) 0.0030(5) 0.0033(5) 0.0024(5) N102 0.0133(6) 0.0158(7) 0.0158(6) 0.0017(5) 0.0039(5) 0.0040(5) O3 0.0156(5) 0.0196(6) 0.0225(6) -0.0005(5) 0.0068(5) 0.0027(5) O4 0.0179(6) 0.0184(6) 0.0219(6) 0.0067(5) 0.0025(5) 0.0007(5) O103 0.0211(6) 0.0197(6) 0.0215(6) 0.0077(5) 0.0087(5) 0.0086(5) O104 0.0169(5) 0.0178(6) 0.0189(6) -0.0023(5) 0.0045(5) -0.0022(5) C1 0.0124(7) 0.0156(8) 0.0171(8) 0.0048(6) 0.0041(6) 0.0023(6) C2 0.0153(7) 0.0155(8) 0.0166(8) 0.0040(6) 0.0053(6) 0.0024(6) C3 0.0178(8) 0.0194(8) 0.0203(8) 0.0023(7) 0.0086(6) 0.0040(6) C4 0.0155(8) 0.0208(9) 0.0273(9) 0.0047(7) 0.0075(7) 0.0029(6) C5 0.0138(7) 0.0197(8) 0.0207(8) 0.0012(7) -0.0006(6) -0.0002(6) C6 0.0156(7) 0.0169(8) 0.0158(8) 0.0027(6) 0.0023(6) 0.0031(6) C7 0.0128(7) 0.0143(7) 0.0164(7) 0.0008(6) 0.0057(6) 0.0009(6) C8 0.0149(7) 0.0201(8) 0.0159(8) 0.0017(6) 0.0052(6) 0.0021(6) C9 0.0149(7) 0.0242(9) 0.0172(8) -0.0005(7) 0.0021(6) -0.0010(6) C10 0.0188(8) 0.0198(8) 0.0209(8) 0.0004(7) 0.0072(7) -0.0032(7) C11 0.0205(8) 0.0169(8) 0.0174(8) 0.0031(6) 0.0081(6) 0.0013(6) C12 0.0145(7) 0.0169(8) 0.0159(7) 0.0005(6) 0.0054(6) 0.0015(6) C101 0.0159(7) 0.0115(7) 0.0127(7) 0.0005(6) 0.0026(6) 0.0002(6) C102 0.0145(7) 0.0139(7) 0.0137(7) -0.0003(6) 0.0023(6) 0.0011(6) C103 0.0181(8) 0.0162(8) 0.0134(7) 0.0019(6) 0.0004(6) 0.0030(6) C104 0.0200(8) 0.0174(8) 0.0127(7) 0.0007(6) 0.0032(6) -0.0005(6) C105 0.0150(7) 0.0180(8) 0.0169(8) -0.0006(6) 0.0049(6) 0.0001(6) C106 0.0152(7) 0.0132(7) 0.0140(7) -0.0008(6) 0.0014(6) 0.0009(6) C107 0.0163(7) 0.0129(7) 0.0150(7) 0.0035(6) 0.0052(6) 0.0032(6) C108 0.0153(7) 0.0140(8) 0.0184(8) 0.0046(6) 0.0044(6) 0.0031(6) C109 0.0162(7) 0.0167(8) 0.0204(8) 0.0070(6) 0.0084(6) 0.0033(6) C110 0.0214(8) 0.0155(8) 0.0163(8) 0.0057(6) 0.0072(6) 0.0046(6) C111 0.0177(8) 0.0163(8) 0.0143(7) 0.0032(6) 0.0027(6) 0.0016(6) C112 0.0151(7) 0.0150(8) 0.0160(7) 0.0042(6) 0.0039(6) 0.0032(6) O1 0.0118(5) 0.0188(6) 0.0159(5) -0.0010(4) 0.0037(4) 0.0012(4) O2 0.0124(5) 0.0171(6) 0.0165(5) 0.0043(4) 0.0017(4) -0.0003(4) O101 0.0150(5) 0.0153(5) 0.0155(5) 0.0042(4) 0.0054(4) 0.0039(4) O102 0.0144(5) 0.0157(6) 0.0154(5) 0.0003(4) 0.0046(4) 0.0012(4) Ti1 0.01230(13) 0.01225(14) 0.01341(14) 0.00151(10) 0.00363(10) 0.00219(10) Ti2 0.01060(13) 0.01370(14) 0.01445(14) 0.00184(11) 0.00291(10) 0.00097(10) _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 C13 N2 1.494(2) . ? C13 C12 1.508(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N1 1.493(2) . ? C14 C2 1.504(2) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 N1 1.482(2) . ? C15 C16 1.518(2) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 N2 1.484(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 N1 1.486(2) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 N2 1.487(2) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C10 1.510(2) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C8 1.500(2) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C6 1.506(2) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C4 1.509(2) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C22 H22D 0.9800 . ? C22 H22E 0.9800 . ? C22 H22F 0.9800 . ? C23 O4 1.406(2) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 O3 1.408(2) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C113 N101 1.4971(19) . ? C113 C112 1.509(2) . ? C113 H11A 0.9900 . ? C113 H11B 0.9900 . ? C114 N102 1.498(2) . ? C114 C102 1.506(2) . ? C114 H11C 0.9900 . ? C114 H11D 0.9900 . ? C115 N102 1.488(2) . ? C115 C116 1.518(2) . ? C115 H11E 0.9900 . ? C115 H11F 0.9900 . ? C116 N101 1.486(2) . ? C116 H11G 0.9900 . ? C116 H11H 0.9900 . ? C117 N102 1.4849(19) . ? C117 H11I 0.9800 . ? C117 H11J 0.9800 . ? C117 H11K 0.9800 . ? C118 N101 1.4839(19) . ? C118 H11L 0.9800 . ? C118 H11M 0.9800 . ? C118 H11N 0.9800 . ? C119 C108 1.505(2) . ? C119 H11O 0.9800 . ? C119 H11P 0.9800 . ? C119 H11Q 0.9800 . ? C120 C110 1.513(2) . ? C120 H12A 0.9800 . ? C120 H12B 0.9800 . ? C120 H12C 0.9800 . ? C121 C106 1.504(2) . ? C121 H12D 0.9800 . ? C121 H12E 0.9800 . ? C121 H12F 0.9800 . ? C122 C104 1.509(2) . ? C122 H12G 0.9800 . ? C122 H12H 0.9800 . ? C122 H12I 0.9800 . ? C123 O104 1.410(2) . ? C123 H12J 0.9800 . ? C123 H12K 0.9800 . ? C123 H12L 0.9800 . ? C124 O103 1.409(2) . ? C124 H12M 0.9800 . ? C124 H12N 0.9800 . ? C124 H12O 0.9800 . ? N1 Ti2 2.3320(14) . ? N2 Ti2 2.3289(14) . ? N101 Ti1 2.3373(14) . ? N102 Ti1 2.3239(13) . ? O3 Ti2 1.8393(12) . ? O4 Ti2 1.8395(12) . ? O103 Ti1 1.8282(11) . ? O104 Ti1 1.8341(12) . ? C1 O1 1.3404(18) . ? C1 C2 1.401(2) . ? C1 C6 1.407(2) . ? C2 C3 1.397(2) . ? C3 C4 1.391(2) . ? C3 H3 0.9500 . ? C4 C5 1.394(2) . ? C5 C6 1.393(2) . ? C5 H5 0.9500 . ? C7 O2 1.3392(19) . ? C7 C12 1.401(2) . ? C7 C8 1.408(2) . ? C8 C9 1.391(2) . ? C9 C10 1.395(2) . ? C9 H9 0.9500 . ? C10 C11 1.388(2) . ? C11 C12 1.399(2) . ? C11 H11 0.9500 . ? C101 O101 1.3379(18) . ? C101 C102 1.401(2) . ? C101 C106 1.411(2) . ? C102 C103 1.397(2) . ? C103 C104 1.393(2) . ? C103 H103 0.9500 . ? C104 C105 1.394(2) . ? C105 C106 1.387(2) . ? C105 H105 0.9500 . ? C107 O102 1.3439(19) . ? C107 C112 1.403(2) . ? C107 C108 1.407(2) . ? C108 C109 1.393(2) . ? C109 C110 1.392(2) . ? C109 H109 0.9500 . ? C110 C111 1.396(2) . ? C111 C112 1.396(2) . ? C111 H111 0.9500 . ? O1 Ti2 1.8910(11) . ? O2 Ti2 1.8932(11) . ? O101 Ti1 1.9051(11) . ? O102 Ti1 1.8936(11) . ? 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 N2 C13 C12 115.83(13) . . ? N2 C13 H13A 108.3 . . ? C12 C13 H13A 108.3 . . ? N2 C13 H13B 108.3 . . ? C12 C13 H13B 108.3 . . ? H13A C13 H13B 107.4 . . ? N1 C14 C2 116.57(13) . . ? N1 C14 H14A 108.2 . . ? C2 C14 H14A 108.2 . . ? N1 C14 H14B 108.2 . . ? C2 C14 H14B 108.2 . . ? H14A C14 H14B 107.3 . . ? N1 C15 C16 109.97(13) . . ? N1 C15 H15A 109.7 . . ? C16 C15 H15A 109.7 . . ? N1 C15 H15B 109.7 . . ? C16 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? N2 C16 C15 110.08(13) . . ? N2 C16 H16A 109.6 . . ? C15 C16 H16A 109.6 . . ? N2 C16 H16B 109.6 . . ? C15 C16 H16B 109.6 . . ? H16A C16 H16B 108.2 . . ? N1 C17 H17A 109.5 . . ? N1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C10 C19 H19A 109.5 . . ? C10 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C10 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C8 C20 H20A 109.5 . . ? C8 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C8 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C6 C21 H21A 109.5 . . ? C6 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C6 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C4 C22 H22A 109.5 . . ? C4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C4 C22 H22D 109.5 . . ? H22A C22 H22D 141.1 . . ? H22B C22 H22D 56.3 . . ? H22C C22 H22D 56.3 . . ? C4 C22 H22E 109.5 . . ? H22A C22 H22E 56.3 . . ? H22B C22 H22E 141.1 . . ? H22C C22 H22E 56.3 . . ? H22D C22 H22E 109.5 . . ? C4 C22 H22F 109.5 . . ? H22A C22 H22F 56.3 . . ? H22B C22 H22F 56.3 . . ? H22C C22 H22F 141.1 . . ? H22D C22 H22F 109.5 . . ? H22E C22 H22F 109.5 . . ? O4 C23 H23A 109.5 . . ? O4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O3 C24 H24A 109.5 . . ? O3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N101 C113 C112 114.94(12) . . ? N101 C113 H11A 108.5 . . ? C112 C113 H11A 108.5 . . ? N101 C113 H11B 108.5 . . ? C112 C113 H11B 108.5 . . ? H11A C113 H11B 107.5 . . ? N102 C114 C102 115.21(13) . . ? N102 C114 H11C 108.5 . . ? C102 C114 H11C 108.5 . . ? N102 C114 H11D 108.5 . . ? C102 C114 H11D 108.5 . . ? H11C C114 H11D 107.5 . . ? N102 C115 C116 110.65(13) . . ? N102 C115 H11E 109.5 . . ? C116 C115 H11E 109.5 . . ? N102 C115 H11F 109.5 . . ? C116 C115 H11F 109.5 . . ? H11E C115 H11F 108.1 . . ? N101 C116 C115 110.53(13) . . ? N101 C116 H11G 109.5 . . ? C115 C116 H11G 109.5 . . ? N101 C116 H11H 109.5 . . ? C115 C116 H11H 109.5 . . ? H11G C116 H11H 108.1 . . ? N102 C117 H11I 109.5 . . ? N102 C117 H11J 109.5 . . ? H11I C117 H11J 109.5 . . ? N102 C117 H11K 109.5 . . ? H11I C117 H11K 109.5 . . ? H11J C117 H11K 109.5 . . ? N101 C118 H11L 109.5 . . ? N101 C118 H11M 109.5 . . ? H11L C118 H11M 109.5 . . ? N101 C118 H11N 109.5 . . ? H11L C118 H11N 109.5 . . ? H11M C118 H11N 109.5 . . ? C108 C119 H11O 109.5 . . ? C108 C119 H11P 109.5 . . ? H11O C119 H11P 109.5 . . ? C108 C119 H11Q 109.5 . . ? H11O C119 H11Q 109.5 . . ? H11P C119 H11Q 109.5 . . ? C110 C120 H12A 109.5 . . ? C110 C120 H12B 109.5 . . ? H12A C120 H12B 109.5 . . ? C110 C120 H12C 109.5 . . ? H12A C120 H12C 109.5 . . ? H12B C120 H12C 109.5 . . ? C106 C121 H12D 109.5 . . ? C106 C121 H12E 109.5 . . ? H12D C121 H12E 109.5 . . ? C106 C121 H12F 109.5 . . ? H12D C121 H12F 109.5 . . ? H12E C121 H12F 109.5 . . ? C104 C122 H12G 109.5 . . ? C104 C122 H12H 109.5 . . ? H12G C122 H12H 109.5 . . ? C104 C122 H12I 109.5 . . ? H12G C122 H12I 109.5 . . ? H12H C122 H12I 109.5 . . ? O104 C123 H12J 109.5 . . ? O104 C123 H12K 109.5 . . ? H12J C123 H12K 109.5 . . ? O104 C123 H12L 109.5 . . ? H12J C123 H12L 109.5 . . ? H12K C123 H12L 109.5 . . ? O103 C124 H12M 109.5 . . ? O103 C124 H12N 109.5 . . ? H12M C124 H12N 109.5 . . ? O103 C124 H12O 109.5 . . ? H12M C124 H12O 109.5 . . ? H12N C124 H12O 109.5 . . ? C15 N1 C17 109.86(13) . . ? C15 N1 C14 109.80(12) . . ? C17 N1 C14 106.11(12) . . ? C15 N1 Ti2 109.75(9) . . ? C17 N1 Ti2 110.40(10) . . ? C14 N1 Ti2 110.87(10) . . ? C16 N2 C18 110.17(13) . . ? C16 N2 C13 109.85(13) . . ? C18 N2 C13 106.35(12) . . ? C16 N2 Ti2 109.98(9) . . ? C18 N2 Ti2 109.95(10) . . ? C13 N2 Ti2 110.48(9) . . ? C118 N101 C116 109.98(12) . . ? C118 N101 C113 106.39(12) . . ? C116 N101 C113 110.90(12) . . ? C118 N101 Ti1 111.19(10) . . ? C116 N101 Ti1 108.84(9) . . ? C113 N101 Ti1 109.53(9) . . ? C117 N102 C115 110.18(13) . . ? C117 N102 C114 106.13(12) . . ? C115 N102 C114 110.59(12) . . ? C117 N102 Ti1 110.70(9) . . ? C115 N102 Ti1 109.03(9) . . ? C114 N102 Ti1 110.20(9) . . ? C24 O3 Ti2 126.28(10) . . ? C23 O4 Ti2 131.80(10) . . ? C124 O103 Ti1 131.05(10) . . ? C123 O104 Ti1 130.50(11) . . ? O1 C1 C2 121.29(14) . . ? O1 C1 C6 118.45(14) . . ? C2 C1 C6 120.24(14) . . ? C3 C2 C1 119.01(15) . . ? C3 C2 C14 118.87(15) . . ? C1 C2 C14 121.81(14) . . ? C4 C3 C2 122.02(16) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C3 C4 C5 117.67(15) . . ? C3 C4 C22 121.48(16) . . ? C5 C4 C22 120.85(16) . . ? C6 C5 C4 122.42(15) . . ? C6 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? C5 C6 C1 118.59(15) . . ? C5 C6 C21 121.55(15) . . ? C1 C6 C21 119.81(14) . . ? O2 C7 C12 121.00(14) . . ? O2 C7 C8 118.86(14) . . ? C12 C7 C8 120.14(14) . . ? C9 C8 C7 118.65(15) . . ? C9 C8 C20 121.87(15) . . ? C7 C8 C20 119.46(14) . . ? C8 C9 C10 122.32(15) . . ? C8 C9 H9 118.8 . . ? C10 C9 H9 118.8 . . ? C11 C10 C9 117.99(15) . . ? C11 C10 C19 121.70(16) . . ? C9 C10 C19 120.31(16) . . ? C10 C11 C12 121.66(15) . . ? C10 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? C11 C12 C7 119.23(15) . . ? C11 C12 C13 119.84(14) . . ? C7 C12 C13 120.69(14) . . ? O101 C101 C102 121.22(14) . . ? O101 C101 C106 119.13(14) . . ? C102 C101 C106 119.64(14) . . ? C103 C102 C101 119.31(14) . . ? C103 C102 C114 120.09(14) . . ? C101 C102 C114 120.53(14) . . ? C104 C103 C102 121.90(15) . . ? C104 C103 H103 119.1 . . ? C102 C103 H103 119.1 . . ? C103 C104 C105 117.69(14) . . ? C103 C104 C122 121.78(15) . . ? C105 C104 C122 120.53(15) . . ? C106 C105 C104 122.29(15) . . ? C106 C105 H105 118.9 . . ? C104 C105 H105 118.9 . . ? C105 C106 C101 119.13(14) . . ? C105 C106 C121 121.81(14) . . ? C101 C106 C121 119.04(14) . . ? O102 C107 C112 120.78(14) . . ? O102 C107 C108 119.26(14) . . ? C112 C107 C108 119.96(15) . . ? C109 C108 C107 118.54(15) . . ? C109 C108 C119 121.33(14) . . ? C107 C108 C119 120.10(15) . . ? C110 C109 C108 122.76(15) . . ? C110 C109 H109 118.6 . . ? C108 C109 H109 118.6 . . ? C109 C110 C111 117.52(15) . . ? C109 C110 C120 120.77(14) . . ? C111 C110 C120 121.70(15) . . ? C112 C111 C110 121.70(15) . . ? C112 C111 H111 119.2 . . ? C110 C111 H111 119.2 . . ? C111 C112 C107 119.47(14) . . ? C111 C112 C113 120.03(14) . . ? C107 C112 C113 120.43(14) . . ? C1 O1 Ti2 141.77(10) . . ? C7 O2 Ti2 142.78(10) . . ? C101 O101 Ti1 142.35(10) . . ? C107 O102 Ti1 142.65(10) . . ? O103 Ti1 O104 105.07(6) . . ? O103 Ti1 O102 96.73(5) . . ? O104 Ti1 O102 92.35(5) . . ? O103 Ti1 O101 91.30(5) . . ? O104 Ti1 O101 96.44(5) . . ? O102 Ti1 O101 166.16(5) . . ? O103 Ti1 N102 163.95(5) . . ? O104 Ti1 N102 89.57(5) . . ? O102 Ti1 N102 89.05(5) . . ? O101 Ti1 N102 80.36(5) . . ? O103 Ti1 N101 89.53(5) . . ? O104 Ti1 N101 164.63(5) . . ? O102 Ti1 N101 80.98(5) . . ? O101 Ti1 N101 87.85(5) . . ? N102 Ti1 N101 76.56(5) . . ? O3 Ti2 O4 104.05(6) . . ? O3 Ti2 O1 91.39(5) . . ? O4 Ti2 O1 95.12(5) . . ? O3 Ti2 O2 96.00(5) . . ? O4 Ti2 O2 91.77(5) . . ? O1 Ti2 O2 168.38(5) . . ? O3 Ti2 N2 91.06(5) . . ? O4 Ti2 N2 163.92(5) . . ? O1 Ti2 N2 89.88(5) . . ? O2 Ti2 N2 81.05(5) . . ? O3 Ti2 N1 164.77(5) . . ? O4 Ti2 N1 89.97(5) . . ? O1 Ti2 N1 81.33(5) . . ? O2 Ti2 N1 89.35(5) . . ? N2 Ti2 N1 75.66(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 C15 C16 N2 -56.77(17) . . . . ? N102 C115 C116 N101 57.09(17) . . . . ? C16 C15 N1 C17 -79.36(16) . . . . ? C16 C15 N1 C14 164.32(13) . . . . ? C16 C15 N1 Ti2 42.21(15) . . . . ? C2 C14 N1 C15 -61.06(18) . . . . ? C2 C14 N1 C17 -179.72(14) . . . . ? C2 C14 N1 Ti2 60.38(15) . . . . ? C15 C16 N2 C18 -80.19(16) . . . . ? C15 C16 N2 C13 162.97(12) . . . . ? C15 C16 N2 Ti2 41.16(14) . . . . ? C12 C13 N2 C16 -58.22(18) . . . . ? C12 C13 N2 C18 -177.43(14) . . . . ? C12 C13 N2 Ti2 63.28(16) . . . . ? C115 C116 N101 C118 80.86(16) . . . . ? C115 C116 N101 C113 -161.74(13) . . . . ? C115 C116 N101 Ti1 -41.17(14) . . . . ? C112 C113 N101 C118 173.84(13) . . . . ? C112 C113 N101 C116 54.27(18) . . . . ? C112 C113 N101 Ti1 -65.88(15) . . . . ? C116 C115 N102 C117 80.00(15) . . . . ? C116 C115 N102 C114 -162.98(12) . . . . ? C116 C115 N102 Ti1 -41.67(14) . . . . ? C102 C114 N102 C117 174.94(13) . . . . ? C102 C114 N102 C115 55.45(17) . . . . ? C102 C114 N102 Ti1 -65.17(15) . . . . ? O1 C1 C2 C3 177.69(14) . . . . ? C6 C1 C2 C3 -0.8(2) . . . . ? O1 C1 C2 C14 4.1(2) . . . . ? C6 C1 C2 C14 -174.36(15) . . . . ? N1 C14 C2 C3 147.70(15) . . . . ? N1 C14 C2 C1 -38.7(2) . . . . ? C1 C2 C3 C4 -1.4(2) . . . . ? C14 C2 C3 C4 172.39(15) . . . . ? C2 C3 C4 C5 2.1(3) . . . . ? C2 C3 C4 C22 -177.66(17) . . . . ? C3 C4 C5 C6 -0.7(3) . . . . ? C22 C4 C5 C6 179.08(17) . . . . ? C4 C5 C6 C1 -1.4(2) . . . . ? C4 C5 C6 C21 -178.77(16) . . . . ? O1 C1 C6 C5 -176.39(14) . . . . ? C2 C1 C6 C5 2.1(2) . . . . ? O1 C1 C6 C21 1.0(2) . . . . ? C2 C1 C6 C21 179.55(15) . . . . ? O2 C7 C8 C9 -179.52(15) . . . . ? C12 C7 C8 C9 -0.4(2) . . . . ? O2 C7 C8 C20 -1.3(2) . . . . ? C12 C7 C8 C20 177.86(15) . . . . ? C7 C8 C9 C10 -0.4(3) . . . . ? C20 C8 C9 C10 -178.59(16) . . . . ? C8 C9 C10 C11 0.2(3) . . . . ? C8 C9 C10 C19 -179.79(17) . . . . ? C9 C10 C11 C12 0.7(3) . . . . ? C19 C10 C11 C12 -179.27(17) . . . . ? C10 C11 C12 C7 -1.5(2) . . . . ? C10 C11 C12 C13 173.01(15) . . . . ? O2 C7 C12 C11 -179.60(14) . . . . ? C8 C7 C12 C11 1.3(2) . . . . ? O2 C7 C12 C13 6.0(2) . . . . ? C8 C7 C12 C13 -173.15(15) . . . . ? N2 C13 C12 C11 142.41(15) . . . . ? N2 C13 C12 C7 -43.2(2) . . . . ? O101 C101 C102 C103 -177.78(14) . . . . ? C106 C101 C102 C103 1.3(2) . . . . ? O101 C101 C102 C114 -0.8(2) . . . . ? C106 C101 C102 C114 178.31(14) . . . . ? N102 C114 C102 C103 -142.17(15) . . . . ? N102 C114 C102 C101 40.8(2) . . . . ? C101 C102 C103 C104 0.7(2) . . . . ? C114 C102 C103 C104 -176.38(15) . . . . ? C102 C103 C104 C105 -1.6(2) . . . . ? C102 C103 C104 C122 177.49(16) . . . . ? C103 C104 C105 C106 0.6(2) . . . . ? C122 C104 C105 C106 -178.51(16) . . . . ? C104 C105 C106 C101 1.3(2) . . . . ? C104 C105 C106 C121 179.51(15) . . . . ? O101 C101 C106 C105 176.84(14) . . . . ? C102 C101 C106 C105 -2.2(2) . . . . ? O101 C101 C106 C121 -1.4(2) . . . . ? C102 C101 C106 C121 179.52(15) . . . . ? O102 C107 C108 C109 178.48(14) . . . . ? C112 C107 C108 C109 -1.7(2) . . . . ? O102 C107 C108 C119 0.6(2) . . . . ? C112 C107 C108 C119 -179.54(15) . . . . ? C107 C108 C109 C110 -0.3(2) . . . . ? C119 C108 C109 C110 177.54(15) . . . . ? C108 C109 C110 C111 1.8(2) . . . . ? C108 C109 C110 C120 -177.50(15) . . . . ? C109 C110 C111 C112 -1.3(2) . . . . ? C120 C110 C111 C112 177.97(15) . . . . ? C110 C111 C112 C107 -0.6(2) . . . . ? C110 C111 C112 C113 -177.72(14) . . . . ? O102 C107 C112 C111 -178.03(14) . . . . ? C108 C107 C112 C111 2.1(2) . . . . ? O102 C107 C112 C113 -0.9(2) . . . . ? C108 C107 C112 C113 179.21(14) . . . . ? N101 C113 C112 C111 -139.48(15) . . . . ? N101 C113 C112 C107 43.5(2) . . . . ? C2 C1 O1 Ti2 -4.6(3) . . . . ? C6 C1 O1 Ti2 173.89(12) . . . . ? C12 C7 O2 Ti2 -1.0(3) . . . . ? C8 C7 O2 Ti2 178.09(12) . . . . ? C102 C101 O101 Ti1 -3.8(3) . . . . ? C106 C101 O101 Ti1 177.08(12) . . . . ? C112 C107 O102 Ti1 -8.7(3) . . . . ? C108 C107 O102 Ti1 171.19(12) . . . . ? C124 O103 Ti1 O104 79.86(15) . . . . ? C124 O103 Ti1 O102 174.14(14) . . . . ? C124 O103 Ti1 O101 -17.16(15) . . . . ? C124 O103 Ti1 N102 -75.4(2) . . . . ? C124 O103 Ti1 N101 -105.00(15) . . . . ? C123 O104 Ti1 O103 69.29(15) . . . . ? C123 O104 Ti1 O102 -28.33(14) . . . . ? C123 O104 Ti1 O101 162.38(14) . . . . ? C123 O104 Ti1 N102 -117.37(14) . . . . ? C123 O104 Ti1 N101 -92.1(2) . . . . ? C107 O102 Ti1 O103 76.16(17) . . . . ? C107 O102 Ti1 O104 -178.36(16) . . . . ? C107 O102 Ti1 O101 -48.9(3) . . . . ? C107 O102 Ti1 N102 -88.83(16) . . . . ? C107 O102 Ti1 N101 -12.28(16) . . . . ? C101 O101 Ti1 O103 176.58(17) . . . . ? C101 O101 Ti1 O104 71.25(17) . . . . ? C101 O101 Ti1 O102 -57.8(3) . . . . ? C101 O101 Ti1 N102 -17.21(16) . . . . ? C101 O101 Ti1 N101 -93.94(17) . . . . ? C117 N102 Ti1 O103 -137.33(18) . . . . ? C115 N102 Ti1 O103 -16.0(2) . . . . ? C114 N102 Ti1 O103 105.58(19) . . . . ? C117 N102 Ti1 O104 66.55(11) . . . . ? C115 N102 Ti1 O104 -172.09(10) . . . . ? C114 N102 Ti1 O104 -50.55(10) . . . . ? C117 N102 Ti1 O102 -25.81(11) . . . . ? C115 N102 Ti1 O102 95.55(10) . . . . ? C114 N102 Ti1 O102 -142.90(10) . . . . ? C117 N102 Ti1 O101 163.15(11) . . . . ? C115 N102 Ti1 O101 -75.49(10) . . . . ? C114 N102 Ti1 O101 46.06(10) . . . . ? C117 N102 Ti1 N101 -106.76(11) . . . . ? C115 N102 Ti1 N101 14.60(9) . . . . ? C114 N102 Ti1 N101 136.14(10) . . . . ? C118 N101 Ti1 O103 64.80(10) . . . . ? C116 N101 Ti1 O103 -173.90(10) . . . . ? C113 N101 Ti1 O103 -52.50(10) . . . . ? C118 N101 Ti1 O104 -133.19(18) . . . . ? C116 N101 Ti1 O104 -11.9(2) . . . . ? C113 N101 Ti1 O104 109.51(19) . . . . ? C118 N101 Ti1 O102 161.70(10) . . . . ? C116 N101 Ti1 O102 -77.00(10) . . . . ? C113 N101 Ti1 O102 44.39(9) . . . . ? C118 N101 Ti1 O101 -26.51(10) . . . . ? C116 N101 Ti1 O101 94.78(10) . . . . ? C113 N101 Ti1 O101 -143.82(10) . . . . ? C118 N101 Ti1 N102 -107.11(10) . . . . ? C116 N101 Ti1 N102 14.19(9) . . . . ? C113 N101 Ti1 N102 135.58(10) . . . . ? C24 O3 Ti2 O4 -46.41(14) . . . . ? C24 O3 Ti2 O1 49.23(13) . . . . ? C24 O3 Ti2 O2 -139.75(13) . . . . ? C24 O3 Ti2 N2 139.13(13) . . . . ? C24 O3 Ti2 N1 110.2(2) . . . . ? C23 O4 Ti2 O3 -85.71(15) . . . . ? C23 O4 Ti2 O1 -178.43(15) . . . . ? C23 O4 Ti2 O2 10.93(15) . . . . ? C23 O4 Ti2 N2 73.9(2) . . . . ? C23 O4 Ti2 N1 100.28(15) . . . . ? C1 O1 Ti2 O3 -171.12(17) . . . . ? C1 O1 Ti2 O4 -66.87(17) . . . . ? C1 O1 Ti2 O2 59.3(3) . . . . ? C1 O1 Ti2 N2 97.82(17) . . . . ? C1 O1 Ti2 N1 22.31(16) . . . . ? C7 O2 Ti2 O3 -71.93(17) . . . . ? C7 O2 Ti2 O4 -176.26(17) . . . . ? C7 O2 Ti2 O1 57.3(3) . . . . ? C7 O2 Ti2 N2 18.21(17) . . . . ? C7 O2 Ti2 N1 93.79(17) . . . . ? C16 N2 Ti2 O3 173.54(10) . . . . ? C18 N2 Ti2 O3 -64.97(10) . . . . ? C13 N2 Ti2 O3 52.11(11) . . . . ? C16 N2 Ti2 O4 13.3(2) . . . . ? C18 N2 Ti2 O4 134.80(18) . . . . ? C13 N2 Ti2 O4 -108.12(19) . . . . ? C16 N2 Ti2 O1 -95.07(10) . . . . ? C18 N2 Ti2 O1 26.42(10) . . . . ? C13 N2 Ti2 O1 143.50(10) . . . . ? C16 N2 Ti2 O2 77.63(10) . . . . ? C18 N2 Ti2 O2 -160.88(11) . . . . ? C13 N2 Ti2 O2 -43.80(10) . . . . ? C16 N2 Ti2 N1 -14.00(9) . . . . ? C18 N2 Ti2 N1 107.49(10) . . . . ? C13 N2 Ti2 N1 -135.43(11) . . . . ? C15 N1 Ti2 O3 14.8(2) . . . . ? C17 N1 Ti2 O3 135.99(18) . . . . ? C14 N1 Ti2 O3 -106.7(2) . . . . ? C15 N1 Ti2 O4 172.09(10) . . . . ? C17 N1 Ti2 O4 -66.67(10) . . . . ? C14 N1 Ti2 O4 50.63(10) . . . . ? C15 N1 Ti2 O1 76.90(10) . . . . ? C17 N1 Ti2 O1 -161.86(11) . . . . ? C14 N1 Ti2 O1 -44.56(10) . . . . ? C15 N1 Ti2 O2 -96.14(10) . . . . ? C17 N1 Ti2 O2 25.10(10) . . . . ? C14 N1 Ti2 O2 142.40(10) . . . . ? C15 N1 Ti2 N2 -15.21(10) . . . . ? C17 N1 Ti2 N2 106.03(10) . . . . ? C14 N1 Ti2 N2 -136.67(10) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.86 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.576 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.052 # Attachment 'mgh_14_pub.cif' data_mgh_14_pub _database_code_depnum_ccdc_archive 'CCDC 804777' #TrackingRef 'mgh_14_pub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point >350 _chemical_formula_moiety 'C29 H33 N3 O6 Ti' _chemical_formula_sum 'C29 H33 N3 O6 Ti' _chemical_formula_weight 567.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'p 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.2989(6) _cell_length_b 22.7397(17) _cell_length_c 14.9120(10) _cell_angle_alpha 90.00 _cell_angle_beta 122.978(4) _cell_angle_gamma 90.00 _cell_volume 2645.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 21801 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.23 _exptl_crystal_description fragment _exptl_crystal_colour orange _exptl_crystal_size_max 0.380 _exptl_crystal_size_mid 0.270 _exptl_crystal_size_min 0.150 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 0.373 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.9112 _exptl_absorpt_correction_T_max 0.9521 _exptl_absorpt_process_details ; 'X-SHAPE 2.07 (03-Aug-2005) Stoe & Cie, Darmstadt, Germany' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25319 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 26.88 _reflns_number_total 5643 _reflns_number_gt 4378 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0437P)^2^+0.4546P] 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 5643 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0839 _refine_ls_wR_factor_gt 0.0794 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 C1 C -0.0386(2) 0.45045(8) 0.19866(13) 0.0155(3) Uani 1 1 d . . . C2 C -0.1787(2) 0.41581(8) 0.12494(14) 0.0175(4) Uani 1 1 d . . . C3 C -0.1488(2) 0.35772(8) 0.10938(14) 0.0188(4) Uani 1 1 d . . . H3 H -0.2430 0.3340 0.0595 0.023 Uiso 1 1 calc R . . C4 C 0.0153(2) 0.33348(8) 0.16485(14) 0.0184(4) Uani 1 1 d . . . C5 C 0.1515(2) 0.36963(8) 0.23449(14) 0.0176(4) Uani 1 1 d . . . H5 H 0.2644 0.3540 0.2714 0.021 Uiso 1 1 calc R . . C6 C 0.1284(2) 0.42775(8) 0.25209(13) 0.0163(3) Uani 1 1 d . . . C7 C 0.2812(2) 0.46423(8) 0.32997(14) 0.0181(4) Uani 1 1 d . . . H7A H 0.2936 0.4631 0.4002 0.022 Uiso 1 1 calc R . . H7B H 0.3852 0.4462 0.3390 0.022 Uiso 1 1 calc R . . C8 C 0.2388(2) 0.68950(8) 0.32078(14) 0.0165(4) Uani 1 1 d . . . C9 C 0.3723(2) 0.72048(8) 0.40745(14) 0.0177(4) Uani 1 1 d . . . C10 C 0.4386(2) 0.76973(8) 0.38697(15) 0.0194(4) Uani 1 1 d . . . H10 H 0.5293 0.7909 0.4454 0.023 Uiso 1 1 calc R . . C11 C 0.3760(2) 0.78887(8) 0.28350(15) 0.0214(4) Uani 1 1 d . . . C12 C 0.2471(2) 0.75595(8) 0.19880(14) 0.0202(4) Uani 1 1 d . . . H12 H 0.2060 0.7677 0.1276 0.024 Uiso 1 1 calc R . . C13 C 0.1769(2) 0.70644(8) 0.21559(14) 0.0183(4) Uani 1 1 d . . . C14 C 0.0331(2) 0.67262(8) 0.12236(14) 0.0196(4) Uani 1 1 d . . . H14A H -0.0769 0.6845 0.1128 0.024 Uiso 1 1 calc R . . H14B H 0.0284 0.6837 0.0566 0.024 Uiso 1 1 calc R . . C15 C 0.2628(2) 0.52857(8) 0.19518(14) 0.0199(4) Uani 1 1 d . . . H15A H 0.1760 0.5000 0.1444 0.024 Uiso 1 1 calc R . . H15B H 0.3751 0.5174 0.2075 0.024 Uiso 1 1 calc R . . C16 C 0.2152(2) 0.58936(8) 0.14846(15) 0.0206(4) Uani 1 1 d . . . H16A H 0.3067 0.6174 0.1964 0.025 Uiso 1 1 calc R . . H16B H 0.2031 0.5900 0.0783 0.025 Uiso 1 1 calc R . . C17 C -0.3554(2) 0.44206(9) 0.06470(16) 0.0244(4) Uani 1 1 d . . . H17A H -0.4387 0.4121 0.0180 0.037 Uiso 1 1 calc R . . H17B H -0.3591 0.4751 0.0213 0.037 Uiso 1 1 calc R . . H17C H -0.3837 0.4561 0.1155 0.037 Uiso 1 1 calc R . . C18 C 0.0473(3) 0.27011(8) 0.15021(16) 0.0246(4) Uani 1 1 d . . . H18A H 0.1451 0.2680 0.1423 0.037 Uiso 1 1 calc R . . H18B H -0.0548 0.2541 0.0861 0.037 Uiso 1 1 calc R . . H18C H 0.0723 0.2472 0.2128 0.037 Uiso 1 1 calc R . . C19 C 0.4346(2) 0.70122(9) 0.51957(14) 0.0219(4) Uani 1 1 d . . . H19A H 0.5283 0.7269 0.5708 0.033 Uiso 1 1 calc R . . H19B H 0.4758 0.6606 0.5301 0.033 Uiso 1 1 calc R . . H19C H 0.3402 0.7036 0.5307 0.033 Uiso 1 1 calc R . . C20 C 0.4412(3) 0.84480(9) 0.26374(17) 0.0293(5) Uani 1 1 d . . . H20A H 0.3661 0.8775 0.2552 0.044 Uiso 1 1 calc R . . H20B H 0.4420 0.8406 0.1986 0.044 Uiso 1 1 calc R . . H20C H 0.5578 0.8526 0.3246 0.044 Uiso 1 1 calc R . . C21 C 0.4348(2) 0.55500(9) 0.38255(14) 0.0205(4) Uani 1 1 d . . . H21A H 0.5323 0.5333 0.3908 0.031 Uiso 1 1 calc R . . H21B H 0.4411 0.5545 0.4503 0.031 Uiso 1 1 calc R . . H21C H 0.4380 0.5957 0.3623 0.031 Uiso 1 1 calc R . . C22 C -0.0935(2) 0.58085(9) 0.03477(13) 0.0223(4) Uani 1 1 d . . . H22A H -0.0898 0.5950 -0.0260 0.033 Uiso 1 1 calc R . . H22B H -0.2026 0.5924 0.0252 0.033 Uiso 1 1 calc R . . H22C H -0.0832 0.5379 0.0389 0.033 Uiso 1 1 calc R . . C30 C -0.0028(2) 0.58725(8) 0.47307(14) 0.0171(4) Uani 1 1 d . . . C31 C -0.0591(2) 0.61000(8) 0.53546(15) 0.0222(4) Uani 1 1 d . . . H31 H -0.0006 0.6013 0.6096 0.027 Uiso 1 1 calc R . . C32 C -0.2034(3) 0.64575(9) 0.48593(16) 0.0246(4) Uani 1 1 d . . . H32 H -0.2436 0.6625 0.5267 0.030 Uiso 1 1 calc R . . C33 C -0.2890(2) 0.65716(8) 0.37722(16) 0.0216(4) Uani 1 1 d . . . H33 H -0.3889 0.6810 0.3423 0.026 Uiso 1 1 calc R . . C34 C -0.2241(2) 0.63263(8) 0.32111(14) 0.0171(4) Uani 1 1 d . . . C35 C -0.2909(2) 0.64096(8) 0.20474(15) 0.0191(4) Uani 1 1 d . . . C36 C 0.1504(2) 0.54895(8) 0.50907(14) 0.0183(4) Uani 1 1 d . . . N1 N 0.27218(19) 0.52686(7) 0.29790(11) 0.0168(3) Uani 1 1 d . . . N2 N 0.05063(19) 0.60713(7) 0.13516(12) 0.0178(3) Uani 1 1 d . . . N3 N -0.08367(19) 0.59923(6) 0.36920(12) 0.0156(3) Uani 1 1 d . . . O1 O -0.06682(15) 0.50614(5) 0.21629(9) 0.0165(3) Uani 1 1 d . . . O2 O 0.16836(16) 0.64332(5) 0.33972(9) 0.0169(3) Uani 1 1 d . . . O3 O 0.17157(16) 0.53796(5) 0.43155(9) 0.0180(3) Uani 1 1 d . . . O4 O -0.18786(16) 0.61812(6) 0.18048(10) 0.0193(3) Uani 1 1 d . . . O5 O 0.23971(18) 0.53094(6) 0.60060(10) 0.0266(3) Uani 1 1 d . . . O6 O -0.42449(17) 0.66643(6) 0.14384(11) 0.0274(3) Uani 1 1 d . . . Ti1 Ti 0.03777(4) 0.575888(14) 0.28327(2) 0.01413(8) Uani 1 1 d . . . 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 C1 0.0190(9) 0.0157(8) 0.0143(8) 0.0020(7) 0.0108(7) 0.0018(7) C2 0.0181(9) 0.0189(9) 0.0168(8) 0.0028(7) 0.0103(7) -0.0005(7) C3 0.0199(9) 0.0184(9) 0.0193(9) 0.0009(7) 0.0113(7) -0.0031(7) C4 0.0255(9) 0.0154(9) 0.0201(8) 0.0031(7) 0.0162(8) 0.0012(7) C5 0.0197(9) 0.0186(9) 0.0181(9) 0.0039(7) 0.0125(8) 0.0043(7) C6 0.0175(8) 0.0189(9) 0.0134(8) 0.0011(7) 0.0090(7) 0.0014(7) C7 0.0154(8) 0.0214(9) 0.0153(8) 0.0007(7) 0.0068(7) 0.0053(7) C8 0.0188(9) 0.0147(8) 0.0198(9) 0.0004(7) 0.0130(8) 0.0024(7) C9 0.0191(9) 0.0182(9) 0.0180(9) -0.0014(7) 0.0115(7) 0.0039(7) C10 0.0187(9) 0.0195(9) 0.0224(9) -0.0051(7) 0.0126(8) -0.0008(7) C11 0.0258(10) 0.0200(9) 0.0268(9) -0.0031(8) 0.0199(8) -0.0020(8) C12 0.0260(10) 0.0212(9) 0.0191(9) -0.0002(7) 0.0159(8) -0.0013(8) C13 0.0209(9) 0.0189(9) 0.0179(8) -0.0007(7) 0.0124(8) 0.0006(7) C14 0.0238(10) 0.0205(9) 0.0146(8) 0.0025(7) 0.0104(7) -0.0019(8) C15 0.0218(9) 0.0235(10) 0.0196(9) -0.0043(7) 0.0147(8) -0.0025(8) C16 0.0239(9) 0.0241(10) 0.0189(9) -0.0030(7) 0.0149(8) -0.0035(8) C17 0.0179(9) 0.0224(10) 0.0271(10) 0.0015(8) 0.0084(8) 0.0006(8) C18 0.0284(10) 0.0174(9) 0.0325(10) -0.0003(8) 0.0195(9) -0.0007(8) C19 0.0238(10) 0.0221(10) 0.0169(9) -0.0012(7) 0.0093(8) 0.0015(8) C20 0.0389(12) 0.0278(11) 0.0299(10) -0.0056(9) 0.0244(10) -0.0125(9) C21 0.0150(9) 0.0237(9) 0.0217(9) -0.0043(7) 0.0092(7) -0.0011(7) C22 0.0256(10) 0.0247(10) 0.0131(8) -0.0022(7) 0.0082(8) -0.0049(8) C30 0.0197(9) 0.0154(9) 0.0198(9) -0.0006(7) 0.0131(8) -0.0031(7) C31 0.0261(10) 0.0234(10) 0.0238(10) -0.0022(8) 0.0178(8) -0.0045(8) C32 0.0287(10) 0.0230(10) 0.0340(11) -0.0060(8) 0.0248(9) -0.0034(8) C33 0.0195(9) 0.0184(9) 0.0328(10) -0.0021(8) 0.0180(8) -0.0014(7) C34 0.0165(8) 0.0123(8) 0.0237(9) -0.0009(7) 0.0117(8) -0.0027(7) C35 0.0196(9) 0.0128(8) 0.0235(9) -0.0009(7) 0.0108(8) -0.0006(7) C36 0.0239(9) 0.0152(9) 0.0186(9) -0.0003(7) 0.0133(8) -0.0014(7) N1 0.0165(7) 0.0191(8) 0.0148(7) -0.0028(6) 0.0085(6) -0.0012(6) N2 0.0200(8) 0.0188(8) 0.0141(7) -0.0012(6) 0.0090(6) -0.0022(6) N3 0.0164(7) 0.0128(7) 0.0202(7) 0.0004(6) 0.0117(6) -0.0011(6) O1 0.0150(6) 0.0161(6) 0.0180(6) -0.0006(5) 0.0088(5) 0.0011(5) O2 0.0208(6) 0.0163(6) 0.0164(6) 0.0002(5) 0.0119(5) -0.0005(5) O3 0.0207(6) 0.0193(6) 0.0162(6) 0.0020(5) 0.0114(5) 0.0034(5) O4 0.0196(6) 0.0201(7) 0.0179(6) 0.0019(5) 0.0100(5) 0.0041(5) O5 0.0328(8) 0.0292(8) 0.0198(7) 0.0053(6) 0.0156(6) 0.0086(6) O6 0.0219(7) 0.0258(7) 0.0286(7) 0.0031(6) 0.0100(6) 0.0085(6) Ti1 0.01511(15) 0.01465(15) 0.01348(14) 0.00070(12) 0.00834(12) 0.00130(13) _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 C1 O1 1.348(2) . ? C1 C6 1.402(2) . ? C1 C2 1.402(3) . ? C2 C3 1.395(3) . ? C2 C17 1.502(3) . ? C3 C4 1.394(3) . ? C3 H3 0.9500 . ? C4 C5 1.388(3) . ? C4 C18 1.511(3) . ? C5 C6 1.387(3) . ? C5 H5 0.9500 . ? C6 C7 1.503(2) . ? C7 N1 1.490(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O2 1.346(2) . ? C8 C13 1.399(2) . ? C8 C9 1.401(3) . ? C9 C10 1.390(3) . ? C9 C19 1.506(2) . ? C10 C11 1.390(3) . ? C10 H10 0.9500 . ? C11 C12 1.394(3) . ? C11 C20 1.505(3) . ? C12 C13 1.390(3) . ? C12 H12 0.9500 . ? C13 C14 1.513(3) . ? C14 N2 1.499(2) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 N1 1.486(2) . ? C15 C16 1.502(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 N2 1.488(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 N1 1.487(2) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 N2 1.487(2) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C30 N3 1.331(2) . ? C30 C31 1.392(2) . ? C30 C36 1.498(3) . ? C31 C32 1.388(3) . ? C31 H31 0.9500 . ? C32 C33 1.387(3) . ? C32 H32 0.9500 . ? C33 C34 1.388(2) . ? C33 H33 0.9500 . ? C34 N3 1.333(2) . ? C34 C35 1.503(3) . ? C35 O6 1.215(2) . ? C35 O4 1.302(2) . ? C36 O5 1.219(2) . ? C36 O3 1.298(2) . ? N1 Ti1 2.3504(15) . ? N2 Ti1 2.3842(15) . ? N3 Ti1 2.1850(14) . ? O1 Ti1 1.8443(12) . ? O2 Ti1 1.8497(13) . ? O3 Ti1 2.0459(12) . ? O4 Ti1 2.0428(13) . ? 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 O1 C1 C6 120.52(16) . . ? O1 C1 C2 118.98(16) . . ? C6 C1 C2 120.50(16) . . ? C3 C2 C1 118.57(17) . . ? C3 C2 C17 121.93(17) . . ? C1 C2 C17 119.50(16) . . ? C4 C3 C2 121.91(17) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C5 C4 C3 117.92(16) . . ? C5 C4 C18 120.10(17) . . ? C3 C4 C18 121.98(17) . . ? C6 C5 C4 122.26(17) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C5 C6 C1 118.76(16) . . ? C5 C6 C7 119.57(16) . . ? C1 C6 C7 121.65(16) . . ? N1 C7 C6 114.53(14) . . ? N1 C7 H7A 108.6 . . ? C6 C7 H7A 108.6 . . ? N1 C7 H7B 108.6 . . ? C6 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? O2 C8 C13 120.01(16) . . ? O2 C8 C9 119.14(16) . . ? C13 C8 C9 120.85(17) . . ? C10 C9 C8 118.63(16) . . ? C10 C9 C19 121.97(16) . . ? C8 C9 C19 119.35(16) . . ? C11 C10 C9 121.89(17) . . ? C11 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? C10 C11 C12 118.14(17) . . ? C10 C11 C20 120.79(17) . . ? C12 C11 C20 121.03(17) . . ? C13 C12 C11 121.86(17) . . ? C13 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? C12 C13 C8 118.56(17) . . ? C12 C13 C14 120.86(16) . . ? C8 C13 C14 120.56(16) . . ? N2 C14 C13 114.05(15) . . ? N2 C14 H14A 108.7 . . ? C13 C14 H14A 108.7 . . ? N2 C14 H14B 108.7 . . ? C13 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? N1 C15 C16 109.84(14) . . ? N1 C15 H15A 109.7 . . ? C16 C15 H15A 109.7 . . ? N1 C15 H15B 109.7 . . ? C16 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? N2 C16 C15 109.48(14) . . ? N2 C16 H16A 109.8 . . ? C15 C16 H16A 109.8 . . ? N2 C16 H16B 109.8 . . ? C15 C16 H16B 109.8 . . ? H16A C16 H16B 108.2 . . ? C2 C17 H17A 109.5 . . ? C2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C4 C18 H18A 109.5 . . ? C4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C9 C19 H19A 109.5 . . ? C9 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C9 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C11 C20 H20A 109.5 . . ? C11 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C11 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N1 C21 H21A 109.5 . . ? N1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N2 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N3 C30 C31 121.47(17) . . ? N3 C30 C36 111.15(15) . . ? C31 C30 C36 127.36(16) . . ? C32 C31 C30 117.90(17) . . ? C32 C31 H31 121.0 . . ? C30 C31 H31 121.0 . . ? C33 C32 C31 120.34(17) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C32 C33 C34 117.91(17) . . ? C32 C33 H33 121.0 . . ? C34 C33 H33 121.0 . . ? N3 C34 C33 121.65(17) . . ? N3 C34 C35 111.18(15) . . ? C33 C34 C35 127.12(17) . . ? O6 C35 O4 126.18(17) . . ? O6 C35 C34 122.34(16) . . ? O4 C35 C34 111.48(15) . . ? O5 C36 O3 126.24(17) . . ? O5 C36 C30 122.14(16) . . ? O3 C36 C30 111.62(15) . . ? C15 N1 C21 109.03(14) . . ? C15 N1 C7 108.50(13) . . ? C21 N1 C7 106.58(14) . . ? C15 N1 Ti1 111.13(11) . . ? C21 N1 Ti1 109.73(11) . . ? C7 N1 Ti1 111.74(11) . . ? C22 N2 C16 108.85(14) . . ? C22 N2 C14 107.17(14) . . ? C16 N2 C14 108.63(14) . . ? C22 N2 Ti1 109.92(11) . . ? C16 N2 Ti1 111.23(11) . . ? C14 N2 Ti1 110.93(10) . . ? C30 N3 C34 120.70(15) . . ? C30 N3 Ti1 119.20(12) . . ? C34 N3 Ti1 119.37(12) . . ? C1 O1 Ti1 144.34(11) . . ? C8 O2 Ti1 145.58(11) . . ? C36 O3 Ti1 125.69(11) . . ? C35 O4 Ti1 126.12(11) . . ? O1 Ti1 O2 168.92(5) . . ? O1 Ti1 O4 88.53(5) . . ? O2 Ti1 O4 95.94(5) . . ? O1 Ti1 O3 93.10(5) . . ? O2 Ti1 O3 89.73(5) . . ? O4 Ti1 O3 141.37(5) . . ? O1 Ti1 N3 103.77(5) . . ? O2 Ti1 N3 87.28(5) . . ? O4 Ti1 N3 71.23(5) . . ? O3 Ti1 N3 70.92(5) . . ? O1 Ti1 N1 80.29(5) . . ? O2 Ti1 N1 90.29(5) . . ? O4 Ti1 N1 144.54(5) . . ? O3 Ti1 N1 73.26(5) . . ? N3 Ti1 N1 144.10(5) . . ? O1 Ti1 N2 91.84(5) . . ? O2 Ti1 N2 79.81(5) . . ? O4 Ti1 N2 73.36(5) . . ? O3 Ti1 N2 145.00(5) . . ? N3 Ti1 N2 140.66(6) . . ? N1 Ti1 N2 73.48(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 O1 C1 C2 C3 -178.27(15) . . . . ? C6 C1 C2 C3 2.6(2) . . . . ? O1 C1 C2 C17 2.1(2) . . . . ? C6 C1 C2 C17 -176.99(16) . . . . ? C1 C2 C3 C4 0.0(3) . . . . ? C17 C2 C3 C4 179.63(16) . . . . ? C2 C3 C4 C5 -2.2(3) . . . . ? C2 C3 C4 C18 178.38(16) . . . . ? C3 C4 C5 C6 1.7(3) . . . . ? C18 C4 C5 C6 -178.82(16) . . . . ? C4 C5 C6 C1 0.8(3) . . . . ? C4 C5 C6 C7 178.99(15) . . . . ? O1 C1 C6 C5 177.84(15) . . . . ? C2 C1 C6 C5 -3.1(2) . . . . ? O1 C1 C6 C7 -0.3(2) . . . . ? C2 C1 C6 C7 178.84(15) . . . . ? C5 C6 C7 N1 143.08(16) . . . . ? C1 C6 C7 N1 -38.8(2) . . . . ? O2 C8 C9 C10 -177.05(15) . . . . ? C13 C8 C9 C10 2.1(3) . . . . ? O2 C8 C9 C19 0.4(2) . . . . ? C13 C8 C9 C19 179.55(16) . . . . ? C8 C9 C10 C11 0.1(3) . . . . ? C19 C9 C10 C11 -177.23(17) . . . . ? C9 C10 C11 C12 -2.3(3) . . . . ? C9 C10 C11 C20 175.51(18) . . . . ? C10 C11 C12 C13 2.3(3) . . . . ? C20 C11 C12 C13 -175.47(18) . . . . ? C11 C12 C13 C8 -0.2(3) . . . . ? C11 C12 C13 C14 177.95(17) . . . . ? O2 C8 C13 C12 177.08(16) . . . . ? C9 C8 C13 C12 -2.1(3) . . . . ? O2 C8 C13 C14 -1.1(3) . . . . ? C9 C8 C13 C14 179.77(16) . . . . ? C12 C13 C14 N2 138.72(17) . . . . ? C8 C13 C14 N2 -43.2(2) . . . . ? N1 C15 C16 N2 -56.51(19) . . . . ? N3 C30 C31 C32 0.1(3) . . . . ? C36 C30 C31 C32 178.72(17) . . . . ? C30 C31 C32 C33 1.1(3) . . . . ? C31 C32 C33 C34 -1.1(3) . . . . ? C32 C33 C34 N3 -0.2(3) . . . . ? C32 C33 C34 C35 -177.31(17) . . . . ? N3 C34 C35 O6 174.70(17) . . . . ? C33 C34 C35 O6 -8.0(3) . . . . ? N3 C34 C35 O4 -5.7(2) . . . . ? C33 C34 C35 O4 171.65(17) . . . . ? N3 C30 C36 O5 -177.39(17) . . . . ? C31 C30 C36 O5 3.9(3) . . . . ? N3 C30 C36 O3 2.0(2) . . . . ? C31 C30 C36 O3 -176.70(17) . . . . ? C16 C15 N1 C21 -76.58(18) . . . . ? C16 C15 N1 C7 167.72(14) . . . . ? C16 C15 N1 Ti1 44.49(16) . . . . ? C6 C7 N1 C15 -61.31(19) . . . . ? C6 C7 N1 C21 -178.59(14) . . . . ? C6 C7 N1 Ti1 61.55(16) . . . . ? C15 C16 N2 C22 -81.35(17) . . . . ? C15 C16 N2 C14 162.27(14) . . . . ? C15 C16 N2 Ti1 39.91(16) . . . . ? C13 C14 N2 C22 -176.48(14) . . . . ? C13 C14 N2 C16 -59.03(19) . . . . ? C13 C14 N2 Ti1 63.53(17) . . . . ? C31 C30 N3 C34 -1.4(3) . . . . ? C36 C30 N3 C34 179.79(15) . . . . ? C31 C30 N3 Ti1 168.68(13) . . . . ? C36 C30 N3 Ti1 -10.12(19) . . . . ? C33 C34 N3 C30 1.5(3) . . . . ? C35 C34 N3 C30 178.98(15) . . . . ? C33 C34 N3 Ti1 -168.62(13) . . . . ? C35 C34 N3 Ti1 8.90(19) . . . . ? C6 C1 O1 Ti1 7.2(3) . . . . ? C2 C1 O1 Ti1 -171.89(13) . . . . ? C13 C8 O2 Ti1 19.4(3) . . . . ? C9 C8 O2 Ti1 -161.40(15) . . . . ? O5 C36 O3 Ti1 -172.58(15) . . . . ? C30 C36 O3 Ti1 8.0(2) . . . . ? O6 C35 O4 Ti1 179.48(14) . . . . ? C34 C35 O4 Ti1 -0.1(2) . . . . ? C1 O1 Ti1 O2 45.3(4) . . . . ? C1 O1 Ti1 O4 159.38(18) . . . . ? C1 O1 Ti1 O3 -59.26(18) . . . . ? C1 O1 Ti1 N3 -130.36(18) . . . . ? C1 O1 Ti1 N1 13.18(18) . . . . ? C1 O1 Ti1 N2 86.07(18) . . . . ? C8 O2 Ti1 O1 43.3(4) . . . . ? C8 O2 Ti1 O4 -70.1(2) . . . . ? C8 O2 Ti1 O3 148.2(2) . . . . ? C8 O2 Ti1 N3 -140.9(2) . . . . ? C8 O2 Ti1 N1 74.9(2) . . . . ? C8 O2 Ti1 N2 1.8(2) . . . . ? C35 O4 Ti1 O1 108.62(14) . . . . ? C35 O4 Ti1 O2 -81.54(14) . . . . ? C35 O4 Ti1 O3 15.50(18) . . . . ? C35 O4 Ti1 N3 3.54(13) . . . . ? C35 O4 Ti1 N1 179.55(12) . . . . ? C35 O4 Ti1 N2 -159.02(15) . . . . ? C36 O3 Ti1 O1 -113.67(14) . . . . ? C36 O3 Ti1 O2 77.06(14) . . . . ? C36 O3 Ti1 O4 -22.14(18) . . . . ? C36 O3 Ti1 N3 -10.16(13) . . . . ? C36 O3 Ti1 N1 167.44(15) . . . . ? C36 O3 Ti1 N2 148.68(13) . . . . ? C30 N3 Ti1 O1 99.20(13) . . . . ? C34 N3 Ti1 O1 -90.58(13) . . . . ? C30 N3 Ti1 O2 -79.97(13) . . . . ? C34 N3 Ti1 O2 90.26(13) . . . . ? C30 N3 Ti1 O4 -177.18(14) . . . . ? C34 N3 Ti1 O4 -6.96(12) . . . . ? C30 N3 Ti1 O3 10.68(12) . . . . ? C34 N3 Ti1 O3 -179.09(14) . . . . ? C30 N3 Ti1 N1 6.77(18) . . . . ? C34 N3 Ti1 N1 176.99(12) . . . . ? C30 N3 Ti1 N2 -150.25(12) . . . . ? C34 N3 Ti1 N2 19.97(18) . . . . ? C15 N1 Ti1 O1 77.90(12) . . . . ? C21 N1 Ti1 O1 -161.44(12) . . . . ? C7 N1 Ti1 O1 -43.45(11) . . . . ? C15 N1 Ti1 O2 -96.23(12) . . . . ? C21 N1 Ti1 O2 24.43(12) . . . . ? C7 N1 Ti1 O2 142.42(11) . . . . ? C15 N1 Ti1 O4 4.46(16) . . . . ? C21 N1 Ti1 O4 125.12(12) . . . . ? C7 N1 Ti1 O4 -116.89(12) . . . . ? C15 N1 Ti1 O3 174.14(12) . . . . ? C21 N1 Ti1 O3 -65.20(11) . . . . ? C7 N1 Ti1 O3 52.79(10) . . . . ? C15 N1 Ti1 N3 178.01(11) . . . . ? C21 N1 Ti1 N3 -61.34(15) . . . . ? C7 N1 Ti1 N3 56.65(15) . . . . ? C15 N1 Ti1 N2 -16.95(11) . . . . ? C21 N1 Ti1 N2 103.70(12) . . . . ? C7 N1 Ti1 N2 -138.31(11) . . . . ? C22 N2 Ti1 O1 28.91(12) . . . . ? C16 N2 Ti1 O1 -91.72(12) . . . . ? C14 N2 Ti1 O1 147.25(12) . . . . ? C22 N2 Ti1 O2 -158.41(12) . . . . ? C16 N2 Ti1 O2 80.95(12) . . . . ? C14 N2 Ti1 O2 -40.08(12) . . . . ? C22 N2 Ti1 O4 -59.01(12) . . . . ? C16 N2 Ti1 O4 -179.64(12) . . . . ? C14 N2 Ti1 O4 59.33(11) . . . . ? C22 N2 Ti1 O3 126.96(12) . . . . ? C16 N2 Ti1 O3 6.33(16) . . . . ? C14 N2 Ti1 O3 -114.70(13) . . . . ? C22 N2 Ti1 N3 -85.59(14) . . . . ? C16 N2 Ti1 N3 153.77(11) . . . . ? C14 N2 Ti1 N3 32.75(16) . . . . ? C22 N2 Ti1 N1 108.22(12) . . . . ? C16 N2 Ti1 N1 -12.41(11) . . . . ? C14 N2 Ti1 N1 -133.44(12) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.88 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.308 _refine_diff_density_min -0.379 _refine_diff_density_rms 0.050