# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Daniel Mindiola' _publ_contact_author_address ; Department of Chemistry Indiana University Bloomington IN 47405 ; _publ_contact_author_email MINDIOLA@INDIANA.EDU _publ_section_title ; Latent low-coordinate titanium imides supported by a sterically encumbering beta-diketiminate ligand ; loop_ _publ_author_name 'Daniel Mindiola' 'Brad C. Bailey' 'Falguni Basuli' 'Doug Brown' 'Rodney L. Clark' 'John C. Huffman' data_04277 _database_code_depnum_ccdc_archive 'CCDC 260834' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C51 H78 N3 O Ti, C24 B F20, C4 H8 O' _chemical_formula_sum 'C79 H86 B F20 N3 O2 Ti' _chemical_formula_weight 1548.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' _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 13.5052(10) _cell_length_b 15.0870(12) _cell_length_c 18.9553(14) _cell_angle_alpha 99.273(2) _cell_angle_beta 104.999(2) _cell_angle_gamma 93.197(2) _cell_volume 3662.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 128(2) _cell_measurement_reflns_used 974 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 24.85 _exptl_crystal_description parallelopiped _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 0.217 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; _diffrn_ambient_temperature 128(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details ' 0.30 degree frames measured for 10.17 seconds each' _diffrn_measurement_method '\w scans' _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 59016 _diffrn_reflns_av_R_equivalents 0.0768 _diffrn_reflns_av_sigmaI/netI 0.0937 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 27.55 _reflns_number_total 16905 _reflns_number_gt 9698 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999), XTEL (local program)' _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. Disorder present in thf solvent, one t-Bu group and one i-Pr group. Significant deviations in expected prarmeters for solvent molecule. ; _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^)+(0.0294P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16905 _refine_ls_number_parameters 1276 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0826 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.0934 _refine_ls_wR_factor_gt 0.0817 _refine_ls_goodness_of_fit_ref 0.833 _refine_ls_restrained_S_all 0.833 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.11131(3) 0.19448(2) 0.321692(19) 0.01979(9) Uani 1 1 d . . . N2 N 0.06153(12) 0.17662(11) 0.21366(8) 0.0204(4) Uani 1 1 d . . . C3 C 0.14974(15) 0.17600(13) 0.18953(10) 0.0218(4) Uani 1 1 d . . . C4 C 0.23682(16) 0.23258(14) 0.23100(11) 0.0244(5) Uani 1 1 d . . . C5 C 0.25827(15) 0.30939(14) 0.29130(11) 0.0239(5) Uani 1 1 d . . . N6 N 0.20731(12) 0.31220(10) 0.34229(8) 0.0200(4) Uani 1 1 d . . . C7 C -0.04089(15) 0.15489(13) 0.16362(10) 0.0216(4) Uani 1 1 d . . . C8 C -0.09848(15) 0.07227(14) 0.16038(11) 0.0233(5) Uani 1 1 d . . . C9 C -0.19612(16) 0.05517(15) 0.11049(12) 0.0276(5) Uani 1 1 d . . . C10 C -0.23638(17) 0.11588(16) 0.06687(12) 0.0320(5) Uani 1 1 d . . . C11 C -0.18072(17) 0.19755(16) 0.07335(12) 0.0312(5) Uani 1 1 d . . . C12 C -0.08262(16) 0.21886(14) 0.12163(11) 0.0258(5) Uani 1 1 d . . . C13 C -0.0255(2) 0.31157(16) 0.12797(14) 0.0358(6) Uani 1 1 d . . . C14 C -0.0888(4) 0.3897(4) 0.1294(3) 0.0463(15) Uiso 0.492(4) 1 d P . . H114 H -0.1304 0.3858 0.1644 0.070 Uiso 0.492(4) 1 calc PR . . H113 H -0.1343 0.3883 0.0796 0.070 Uiso 0.492(4) 1 calc PR . . H112 H -0.0432 0.4463 0.1452 0.070 Uiso 0.492(4) 1 calc PR . . C15 C 0.0427(4) 0.3166(3) 0.0778(3) 0.0368(15) Uani 0.492(4) 1 d P . . H117 H 0.0021 0.2969 0.0261 0.055 Uiso 0.492(4) 1 calc PR . . H116 H 0.0977 0.2773 0.0897 0.055 Uiso 0.492(4) 1 calc PR . . H115 H 0.0731 0.3790 0.0847 0.055 Uiso 0.492(4) 1 calc PR . . C16 C -0.06032(17) 0.00229(14) 0.20789(12) 0.0264(5) Uani 1 1 d . . . C17 C -0.0711(2) -0.09286(16) 0.16222(14) 0.0319(5) Uani 1 1 d . . . C18 C -0.11739(19) -0.00031(17) 0.26763(13) 0.0297(5) Uani 1 1 d . . . C19 C 0.16021(16) 0.10944(16) 0.12040(12) 0.0352(6) Uani 1 1 d . . . C20 C 0.2613(2) 0.1267(2) 0.10251(16) 0.0412(7) Uani 1 1 d . . . C21 C 0.0925(3) 0.1463(4) 0.0455(2) 0.0342(14) Uani 0.491(4) 1 d P . . H129 H 0.1077 0.1140 0.0010 0.051 Uiso 0.491(4) 1 calc PR . . H128 H 0.1115 0.2112 0.0507 0.051 Uiso 0.491(4) 1 calc PR . . H130 H 0.0188 0.1355 0.0411 0.051 Uiso 0.491(4) 1 calc PR . . C22 C 0.1292(4) 0.0209(3) 0.1155(3) 0.0329(13) Uiso 0.491(4) 1 d P . . H132 H 0.0548 0.0134 0.1098 0.049 Uiso 0.491(4) 1 calc PR . . H133 H 0.1657 0.0003 0.1608 0.049 Uiso 0.491(4) 1 calc PR . . H131 H 0.1447 -0.0149 0.0725 0.049 Uiso 0.491(4) 1 calc PR . . C23 C 0.34014(17) 0.38183(15) 0.28438(11) 0.0312(5) Uani 1 1 d . . . C24 C 0.2935(3) 0.4095(2) 0.20875(15) 0.0500(8) Uani 1 1 d . . . C25 C 0.4418(2) 0.3402(2) 0.28336(17) 0.0447(7) Uani 1 1 d . . . C26 C 0.3661(2) 0.46847(16) 0.34296(13) 0.0327(6) Uani 1 1 d . . . C27 C 0.23371(15) 0.37740(13) 0.41157(10) 0.0206(4) Uani 1 1 d . . . C28 C 0.32148(15) 0.36835(13) 0.46815(11) 0.0218(4) Uani 1 1 d . . . C29 C 0.34341(17) 0.43114(15) 0.53396(12) 0.0280(5) Uani 1 1 d . . . C30 C 0.28334(17) 0.49985(15) 0.54355(13) 0.0310(5) Uani 1 1 d . . . C31 C 0.19711(17) 0.50629(15) 0.48811(13) 0.0296(5) Uani 1 1 d . . . C32 C 0.16866(16) 0.44468(13) 0.42164(11) 0.0252(5) Uani 1 1 d . . . C33 C 0.07107(17) 0.45443(15) 0.36260(13) 0.0312(5) Uani 1 1 d . . . C34 C 0.0872(2) 0.5329(2) 0.3238(2) 0.0520(8) Uani 1 1 d . . . C35 C -0.01921(19) 0.46763(18) 0.39606(16) 0.0384(6) Uani 1 1 d . . . C36 C 0.39252(16) 0.29457(14) 0.46218(12) 0.0261(5) Uani 1 1 d . . . C37 C 0.3724(2) 0.22300(18) 0.50700(16) 0.0370(6) Uani 1 1 d . . . C38 C 0.50678(17) 0.33055(17) 0.48824(15) 0.0320(5) Uani 1 1 d . . . N39 N 0.01250(12) 0.21085(11) 0.36179(8) 0.0215(4) Uani 1 1 d . . . C40 C -0.06093(15) 0.22411(13) 0.40297(11) 0.0208(4) Uani 1 1 d . . . C41 C -0.02850(15) 0.22896(13) 0.48094(11) 0.0214(4) Uani 1 1 d . . . C42 C -0.09944(16) 0.24536(14) 0.52169(12) 0.0258(5) Uani 1 1 d . . . C43 C -0.19999(17) 0.25704(15) 0.48836(12) 0.0293(5) Uani 1 1 d . . . C44 C -0.23177(17) 0.25044(14) 0.41236(12) 0.0260(5) Uani 1 1 d . . . C45 C -0.16529(15) 0.23360(13) 0.36780(11) 0.0217(4) Uani 1 1 d . . . C46 C -0.20856(16) 0.22463(15) 0.28446(11) 0.0261(5) Uani 1 1 d . . . C47 C -0.30402(18) 0.15636(18) 0.25446(14) 0.0328(5) Uani 1 1 d . . . C48 C -0.2377(3) 0.31468(19) 0.26317(16) 0.0531(8) Uani 1 1 d . . . C49 C 0.08027(16) 0.21527(14) 0.52176(11) 0.0237(5) Uani 1 1 d . . . C50 C 0.0808(2) 0.13793(17) 0.56533(14) 0.0341(6) Uani 1 1 d . . . C51 C 0.13671(19) 0.30106(16) 0.57315(13) 0.0304(5) Uani 1 1 d . . . O52 O 0.17886(10) 0.08790(9) 0.36094(8) 0.0265(3) Uani 1 1 d . . . C53 C 0.2734(2) 0.05563(18) 0.3453(2) 0.0486(8) Uani 1 1 d . . . C54 C 0.2767(2) -0.03839(19) 0.35875(19) 0.0492(7) Uani 1 1 d . . . C55 C 0.1719(2) -0.06493(17) 0.36862(18) 0.0415(6) Uani 1 1 d . . . C56 C 0.13908(18) 0.02258(15) 0.39978(13) 0.0291(5) Uani 1 1 d . . . O57 O 0.3272(4) 0.3391(3) 0.0312(3) 0.0645(17) Uani 0.714(12) 1 d P A 1 C58 C 0.3606(5) 0.4283(4) 0.0315(4) 0.0582(17) Uani 0.714(12) 1 d P A 1 H186 H 0.4142 0.4308 0.0046 0.070 Uiso 0.714(12) 1 calc PR A 1 H185 H 0.3892 0.4617 0.0830 0.070 Uiso 0.714(12) 1 calc PR A 1 C59 C 0.2596(8) 0.4700(7) -0.0099(7) 0.148(6) Uani 0.714(12) 1 d P A 1 H187 H 0.2307 0.5073 0.0264 0.178 Uiso 0.714(12) 1 calc PR A 1 H188 H 0.2755 0.5078 -0.0445 0.178 Uiso 0.714(12) 1 calc PR A 1 C60 C 0.1883(11) 0.3917(10) -0.0500(8) 0.153(6) Uani 0.714(12) 1 d P A 1 H190 H 0.1654 0.3925 -0.1039 0.184 Uiso 0.714(12) 1 calc PR A 1 H189 H 0.1273 0.3868 -0.0305 0.184 Uiso 0.714(12) 1 calc PR A 1 C61 C 0.2653(10) 0.3072(5) -0.0313(5) 0.073(2) Uani 0.714(12) 1 d P A 1 H191 H 0.2241 0.2518 -0.0293 0.088 Uiso 0.714(12) 1 calc PR A 1 H192 H 0.3028 0.2929 -0.0696 0.088 Uiso 0.714(12) 1 calc PR A 1 B62 B 0.49684(18) 0.79348(16) 0.19496(12) 0.0225(5) Uani 1 1 d . . . C63 C 0.53134(15) 0.88970(13) 0.25558(11) 0.0217(4) Uani 1 1 d . . . C64 C 0.47913(15) 0.96472(14) 0.24249(11) 0.0241(5) Uani 1 1 d . . . C65 C 0.49208(16) 1.04369(14) 0.29302(12) 0.0264(5) Uani 1 1 d . . . C66 C 0.55783(16) 1.05027(14) 0.36273(12) 0.0285(5) Uani 1 1 d . . . C67 C 0.61238(16) 0.97924(15) 0.37910(11) 0.0285(5) Uani 1 1 d . . . C68 C 0.59924(15) 0.90178(14) 0.32604(11) 0.0247(5) Uani 1 1 d . . . F69 F 0.40905(9) 0.96186(8) 0.17660(6) 0.0315(3) Uani 1 1 d . . . F70 F 0.44113(9) 1.11498(8) 0.27555(7) 0.0359(3) Uani 1 1 d . . . F71 F 0.56815(10) 1.12566(8) 0.41391(7) 0.0425(3) Uani 1 1 d . . . F72 F 0.67810(10) 0.98451(9) 0.44700(6) 0.0413(3) Uani 1 1 d . . . F73 F 0.65628(9) 0.83544(8) 0.34818(6) 0.0305(3) Uani 1 1 d . . . C74 C 0.57866(15) 0.71789(13) 0.21185(10) 0.0223(4) Uani 1 1 d . . . C75 C 0.55688(16) 0.62769(14) 0.21523(11) 0.0278(5) Uani 1 1 d . . . C76 C 0.63019(18) 0.56742(14) 0.22551(12) 0.0319(5) Uani 1 1 d . . . C77 C 0.73092(17) 0.59482(15) 0.23277(12) 0.0306(5) Uani 1 1 d . . . C78 C 0.75776(16) 0.68315(15) 0.22975(11) 0.0273(5) Uani 1 1 d . . . C79 C 0.68229(16) 0.74003(13) 0.21799(11) 0.0243(5) Uani 1 1 d . . . F80 F 0.45902(9) 0.59369(8) 0.20794(7) 0.0353(3) Uani 1 1 d . . . F81 F 0.60232(11) 0.48105(8) 0.22825(8) 0.0486(4) Uani 1 1 d . . . F82 F 0.80315(10) 0.53690(9) 0.24329(8) 0.0446(3) Uani 1 1 d . . . F83 F 0.85695(9) 0.71131(8) 0.23696(7) 0.0362(3) Uani 1 1 d . . . F84 F 0.71345(9) 0.82573(7) 0.21385(6) 0.0298(3) Uani 1 1 d . . . C85 C 0.38191(15) 0.76576(13) 0.20608(11) 0.0231(5) Uani 1 1 d . . . C86 C 0.28716(16) 0.77456(14) 0.15937(11) 0.0268(5) Uani 1 1 d . . . C87 C 0.19363(16) 0.75834(15) 0.17474(12) 0.0310(5) Uani 1 1 d . . . C88 C 0.19139(17) 0.73279(15) 0.24055(12) 0.0311(5) Uani 1 1 d . . . C89 C 0.28324(17) 0.72418(14) 0.28984(11) 0.0297(5) Uani 1 1 d . . . C90 C 0.37411(16) 0.74055(14) 0.27225(11) 0.0248(5) Uani 1 1 d . . . F91 F 0.28000(9) 0.80110(9) 0.09355(6) 0.0352(3) Uani 1 1 d . . . F92 F 0.10488(9) 0.76913(9) 0.12599(7) 0.0438(3) Uani 1 1 d . . . F93 F 0.10163(9) 0.71902(9) 0.25729(7) 0.0434(3) Uani 1 1 d . . . F94 F 0.28352(10) 0.70128(9) 0.35600(7) 0.0412(3) Uani 1 1 d . . . F95 F 0.46103(9) 0.73274(8) 0.32472(6) 0.0327(3) Uani 1 1 d . . . C96 C 0.49313(15) 0.80264(14) 0.10851(11) 0.0229(4) Uani 1 1 d . . . C97 C 0.44999(16) 0.73050(14) 0.05181(11) 0.0272(5) Uani 1 1 d . . . C98 C 0.44813(16) 0.72713(15) -0.02134(11) 0.0303(5) Uani 1 1 d . . . C99 C 0.49374(16) 0.79919(16) -0.04165(11) 0.0301(5) Uani 1 1 d . . . C100 C 0.53862(15) 0.87200(15) 0.01196(11) 0.0263(5) Uani 1 1 d . . . C101 C 0.53871(15) 0.87285(14) 0.08519(11) 0.0238(5) Uani 1 1 d . . . F102 F 0.40448(9) 0.65608(8) 0.06791(6) 0.0358(3) Uani 1 1 d . . . F103 F 0.40342(10) 0.65364(9) -0.07339(7) 0.0443(4) Uani 1 1 d . . . F104 F 0.49405(10) 0.79729(9) -0.11260(6) 0.0419(3) Uani 1 1 d . . . F105 F 0.58347(9) 0.94423(8) -0.00643(6) 0.0350(3) Uani 1 1 d . . . F106 F 0.58754(9) 0.94774(8) 0.13393(6) 0.0297(3) Uani 1 1 d . . . H107 H 0.2940(15) 0.2251(12) 0.2118(10) 0.021(5) Uiso 1 1 d . . . H108 H -0.2369(15) -0.0022(13) 0.1081(10) 0.023(5) Uiso 1 1 d . . . H109 H -0.3053(16) 0.1004(14) 0.0308(11) 0.031(6) Uiso 1 1 d . . . H110 H -0.2122(15) 0.2386(14) 0.0438(11) 0.030(6) Uiso 1 1 d . . . H111 H 0.034(2) 0.317(2) 0.1616(16) 0.081(11) Uiso 1 1 d . . . H118 H 0.0111(15) 0.0194(13) 0.2320(10) 0.021(5) Uiso 1 1 d . . . H119 H -0.0396(17) -0.0959(15) 0.1206(13) 0.045(7) Uiso 1 1 d . . . H120 H -0.0379(16) -0.1366(15) 0.1960(12) 0.039(6) Uiso 1 1 d . . . H121 H -0.1421(18) -0.1127(14) 0.1419(11) 0.035(6) Uiso 1 1 d . . . H122 H -0.1936(17) -0.0148(14) 0.2453(11) 0.033(6) Uiso 1 1 d . . . H123 H -0.1074(15) 0.0547(15) 0.3027(11) 0.028(6) Uiso 1 1 d . . . H124 H -0.0936(17) -0.0460(16) 0.2971(12) 0.042(7) Uiso 1 1 d . . . H125 H 0.325(2) 0.1178(17) 0.1450(15) 0.063(9) Uiso 1 1 d . . . H126 H 0.271(2) 0.185(2) 0.0919(15) 0.077(10) Uiso 1 1 d . . . H127 H 0.2562(15) 0.0851(15) 0.0572(12) 0.034(6) Uiso 1 1 d . . . H134 H 0.2796(18) 0.3598(17) 0.1661(14) 0.046(7) Uiso 1 1 d . . . H135 H 0.2259(19) 0.4342(16) 0.2071(12) 0.043(8) Uiso 1 1 d . . . H136 H 0.3393(19) 0.4582(17) 0.2034(13) 0.054(7) Uiso 1 1 d . . . H137 H 0.4349(18) 0.2947(17) 0.2386(14) 0.052(8) Uiso 1 1 d . . . H138 H 0.4912(17) 0.3888(15) 0.2825(11) 0.039(6) Uiso 1 1 d . . . H139 H 0.4744(19) 0.3169(17) 0.3307(14) 0.055(8) Uiso 1 1 d . . . H140 H 0.4097(18) 0.5121(16) 0.3249(12) 0.048(7) Uiso 1 1 d . . . H141 H 0.4068(14) 0.4602(13) 0.3930(11) 0.020(5) Uiso 1 1 d . . . H142 H 0.3072(17) 0.4972(14) 0.3500(11) 0.031(6) Uiso 1 1 d . . . H143 H 0.4016(15) 0.4248(12) 0.5708(10) 0.018(5) Uiso 1 1 d . . . H144 H 0.3038(16) 0.5422(15) 0.5900(12) 0.040(7) Uiso 1 1 d . . . H145 H 0.1539(16) 0.5516(14) 0.4961(11) 0.032(6) Uiso 1 1 d . . . H146 H 0.0560(15) 0.3998(15) 0.3284(11) 0.030(6) Uiso 1 1 d . . . H147 H 0.116(2) 0.590(2) 0.3599(17) 0.092(12) Uiso 1 1 d . . . H148 H 0.025(2) 0.5431(17) 0.2903(14) 0.061(8) Uiso 1 1 d . . . H149 H 0.137(2) 0.5238(18) 0.2957(15) 0.068(9) Uiso 1 1 d . . . H150 H -0.0074(17) 0.5237(17) 0.4320(13) 0.044(7) Uiso 1 1 d . . . H151 H -0.0816(16) 0.4737(13) 0.3573(11) 0.027(6) Uiso 1 1 d . . . H152 H -0.0319(17) 0.4151(17) 0.4222(13) 0.051(7) Uiso 1 1 d . . . H153 H 0.3803(14) 0.2676(13) 0.4089(10) 0.019(5) Uiso 1 1 d . . . H154 H 0.3894(18) 0.2500(17) 0.5604(14) 0.056(8) Uiso 1 1 d . . . H155 H 0.2989(18) 0.1969(15) 0.4906(12) 0.041(6) Uiso 1 1 d . . . H156 H 0.4209(17) 0.1726(16) 0.5031(12) 0.044(7) Uiso 1 1 d . . . H157 H 0.5292(15) 0.3462(14) 0.5409(12) 0.031(6) Uiso 1 1 d . . . H158 H 0.5486(18) 0.2786(16) 0.4783(12) 0.047(7) Uiso 1 1 d . . . H159 H 0.5216(16) 0.3781(15) 0.4618(11) 0.034(6) Uiso 1 1 d . . . H160 H -0.0758(15) 0.2519(13) 0.5762(11) 0.030(6) Uiso 1 1 d . . . H161 H -0.2479(16) 0.2706(13) 0.5167(11) 0.028(6) Uiso 1 1 d . . . H162 H -0.3043(16) 0.2594(13) 0.3891(11) 0.030(6) Uiso 1 1 d . . . H163 H -0.1564(15) 0.2045(13) 0.2595(10) 0.024(5) Uiso 1 1 d . . . H164 H -0.3637(18) 0.1791(15) 0.2675(12) 0.040(7) Uiso 1 1 d . . . H165 H -0.3253(15) 0.1409(14) 0.1997(12) 0.032(6) Uiso 1 1 d . . . H166 H -0.2948(19) 0.0983(18) 0.2709(14) 0.062(8) Uiso 1 1 d . . . H167 H -0.293(3) 0.335(2) 0.2908(18) 0.105(13) Uiso 1 1 d . . . H168 H -0.176(2) 0.357(2) 0.2758(15) 0.079(10) Uiso 1 1 d . . . H169 H -0.2653(16) 0.3085(14) 0.2112(13) 0.035(6) Uiso 1 1 d . . . H170 H 0.1171(14) 0.1988(12) 0.4839(10) 0.015(5) Uiso 1 1 d . . . H171 H 0.0466(17) 0.1561(15) 0.6068(12) 0.042(7) Uiso 1 1 d . . . H172 H 0.1521(17) 0.1227(14) 0.5857(11) 0.033(6) Uiso 1 1 d . . . H173 H 0.0398(18) 0.0817(16) 0.5335(12) 0.044(7) Uiso 1 1 d . . . H174 H 0.2062(17) 0.2910(14) 0.5984(11) 0.035(6) Uiso 1 1 d . . . H175 H 0.1392(16) 0.3494(15) 0.5446(12) 0.035(6) Uiso 1 1 d . . . H176 H 0.1027(16) 0.3223(14) 0.6118(12) 0.034(6) Uiso 1 1 d . . . H177 H 0.327(3) 0.089(3) 0.375(2) 0.120(15) Uiso 1 1 d . . . H178 H 0.263(3) 0.058(2) 0.294(2) 0.110(14) Uiso 1 1 d . . . H179 H 0.296(2) -0.0732(18) 0.3206(15) 0.061(9) Uiso 1 1 d . . . H180 H 0.334(2) -0.037(2) 0.4098(17) 0.089(11) Uiso 1 1 d . . . H181 H 0.1780(19) -0.1015(18) 0.4042(14) 0.062(9) Uiso 1 1 d . . . H182 H 0.124(2) -0.0873(17) 0.3218(14) 0.056(8) Uiso 1 1 d . . . H183 H 0.0620(16) 0.0269(13) 0.3889(10) 0.029(6) Uiso 1 1 d . . . H184 H 0.1752(15) 0.0407(13) 0.4544(11) 0.026(5) Uiso 1 1 d . . . C14A C -0.0687(4) 0.3817(3) 0.1733(3) 0.0362(13) Uiso 0.508(4) 1 d P . . H2A H -0.0332 0.4412 0.1762 0.054 Uiso 0.508(4) 1 calc PR . . H3A H -0.0587 0.3684 0.2234 0.054 Uiso 0.508(4) 1 calc PR . . H1A H -0.1425 0.3816 0.1499 0.054 Uiso 0.508(4) 1 calc PR . . C15A C -0.0473(4) 0.3377(3) 0.0450(2) 0.0391(14) Uiso 0.508(4) 1 d P . . H6A H -0.1192 0.3502 0.0282 0.059 Uiso 0.508(4) 1 calc PR . . H4A H -0.0341 0.2871 0.0103 0.059 Uiso 0.508(4) 1 calc PR . . H5A H -0.0016 0.3913 0.0470 0.059 Uiso 0.508(4) 1 calc PR . . C21A C 0.0653(3) 0.0793(3) 0.0576(2) 0.0326(13) Uiso 0.509(4) 1 d P . . H7A H 0.0826 0.0386 0.0177 0.049 Uiso 0.509(4) 1 calc PR . . H9A H 0.0372 0.1321 0.0387 0.049 Uiso 0.509(4) 1 calc PR . . H8A H 0.0138 0.0475 0.0752 0.049 Uiso 0.509(4) 1 calc PR . . C22A C 0.1817(4) 0.0112(3) 0.1534(2) 0.0278(12) Uiso 0.509(4) 1 d P . . H11A H 0.1268 -0.0046 0.1757 0.042 Uiso 0.509(4) 1 calc PR . . H12A H 0.2483 0.0192 0.1910 0.042 Uiso 0.509(4) 1 calc PR . . H10A H 0.1823 -0.0373 0.1123 0.042 Uiso 0.509(4) 1 calc PR . . O57A O 0.265(4) 0.3457(17) 0.0275(13) 0.38(2) Uani 0.286(12) 1 d P A 2 C58A C 0.3455(15) 0.4174(15) -0.0139(16) 0.102(7) Uani 0.286(12) 1 d P A 2 H13A H 0.4129 0.4447 0.0200 0.122 Uiso 0.286(12) 1 calc PR A 2 H14A H 0.3510 0.3905 -0.0637 0.122 Uiso 0.286(12) 1 calc PR A 2 C59A C 0.2705(16) 0.4657(12) -0.0134(14) 0.070(8) Uani 0.286(12) 1 d P A 2 H16A H 0.2715 0.5152 -0.0418 0.084 Uiso 0.286(12) 1 calc PR A 2 H15A H 0.2666 0.4899 0.0374 0.084 Uiso 0.286(12) 1 calc PR A 2 C60A C 0.1886(12) 0.3909(11) -0.0528(9) 0.033(4) Uiso 0.286(12) 1 d P A 2 H21A H 0.1254 0.4038 -0.0373 0.039 Uiso 0.286(12) 1 calc PR A 2 H17A H 0.1728 0.3911 -0.1067 0.039 Uiso 0.286(12) 1 calc PR A 2 C61A C 0.2073(15) 0.3186(14) -0.0431(9) 0.053(5) Uani 0.286(12) 1 d P A 2 H20A H 0.2469 0.2901 -0.0763 0.063 Uiso 0.286(12) 1 calc PR A 2 H19A H 0.1450 0.2782 -0.0469 0.063 Uiso 0.286(12) 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 0.0199(2) 0.01883(19) 0.01988(19) 0.00121(16) 0.00640(15) -0.00236(15) N2 0.0176(9) 0.0205(9) 0.0232(9) 0.0015(7) 0.0080(7) -0.0009(7) C3 0.0216(11) 0.0247(11) 0.0178(10) 0.0024(9) 0.0044(8) 0.0000(9) C4 0.0211(12) 0.0312(12) 0.0206(11) 0.0006(10) 0.0093(9) -0.0045(9) C5 0.0203(11) 0.0264(12) 0.0230(11) 0.0054(9) 0.0031(9) -0.0033(9) N6 0.0200(9) 0.0192(9) 0.0189(9) 0.0030(7) 0.0033(7) -0.0024(7) C7 0.0193(11) 0.0249(11) 0.0200(10) -0.0004(9) 0.0075(8) 0.0004(8) C8 0.0218(11) 0.0258(11) 0.0219(11) 0.0012(9) 0.0077(9) -0.0001(9) C9 0.0228(12) 0.0315(13) 0.0272(12) 0.0012(10) 0.0079(9) -0.0014(10) C10 0.0246(13) 0.0442(15) 0.0237(12) 0.0021(11) 0.0026(10) 0.0033(11) C11 0.0335(14) 0.0390(14) 0.0238(12) 0.0097(11) 0.0082(10) 0.0123(11) C12 0.0282(12) 0.0282(12) 0.0242(11) 0.0041(10) 0.0126(9) 0.0043(9) C13 0.0387(15) 0.0304(13) 0.0430(15) 0.0141(12) 0.0147(12) 0.0041(11) C15 0.036(3) 0.036(3) 0.040(3) 0.010(2) 0.014(2) -0.009(2) C16 0.0210(12) 0.0246(12) 0.0298(12) 0.0029(10) 0.0028(9) -0.0052(9) C17 0.0335(15) 0.0275(13) 0.0331(14) 0.0010(11) 0.0105(11) -0.0032(11) C18 0.0392(15) 0.0227(13) 0.0250(12) 0.0023(11) 0.0071(11) -0.0029(11) C19 0.0226(12) 0.0487(15) 0.0278(12) -0.0128(11) 0.0078(10) 0.0005(11) C20 0.0514(18) 0.0351(15) 0.0420(16) -0.0071(14) 0.0315(14) -0.0023(13) C21 0.031(3) 0.053(4) 0.015(2) -0.004(2) 0.0037(19) 0.010(2) C23 0.0328(13) 0.0339(13) 0.0246(12) 0.0021(10) 0.0096(10) -0.0152(10) C24 0.062(2) 0.0506(18) 0.0305(15) 0.0109(14) 0.0062(14) -0.0304(16) C25 0.0353(15) 0.0508(18) 0.0439(17) -0.0120(15) 0.0212(13) -0.0206(13) C26 0.0325(14) 0.0325(14) 0.0316(14) 0.0062(11) 0.0091(11) -0.0119(11) C27 0.0229(11) 0.0195(10) 0.0183(10) 0.0019(9) 0.0064(8) -0.0062(8) C28 0.0214(11) 0.0222(11) 0.0217(11) 0.0027(9) 0.0076(9) -0.0044(8) C29 0.0225(12) 0.0333(13) 0.0233(12) -0.0001(10) 0.0028(10) -0.0052(10) C30 0.0310(13) 0.0282(13) 0.0287(13) -0.0093(11) 0.0097(10) -0.0070(10) C31 0.0274(13) 0.0208(12) 0.0398(14) -0.0023(11) 0.0135(11) -0.0014(10) C32 0.0265(12) 0.0187(11) 0.0287(12) 0.0034(10) 0.0063(9) -0.0032(9) C33 0.0308(13) 0.0219(12) 0.0361(13) 0.0022(11) 0.0027(10) 0.0030(10) C34 0.0391(18) 0.060(2) 0.061(2) 0.0343(18) 0.0060(16) 0.0082(15) C35 0.0259(14) 0.0315(14) 0.0519(17) 0.0051(14) 0.0016(12) 0.0047(11) C36 0.0239(12) 0.0276(12) 0.0239(12) 0.0026(10) 0.0036(9) -0.0010(9) C37 0.0271(14) 0.0366(15) 0.0472(17) 0.0172(13) 0.0046(12) 0.0018(11) C38 0.0230(12) 0.0323(14) 0.0367(15) 0.0015(12) 0.0047(11) -0.0005(10) N39 0.0238(9) 0.0197(9) 0.0198(9) 0.0025(7) 0.0057(7) -0.0025(7) C40 0.0237(11) 0.0155(10) 0.0252(11) 0.0030(9) 0.0113(9) -0.0011(8) C41 0.0248(11) 0.0175(10) 0.0223(11) 0.0031(9) 0.0077(9) 0.0001(8) C42 0.0300(13) 0.0269(12) 0.0214(11) 0.0046(10) 0.0085(9) 0.0017(9) C43 0.0290(13) 0.0337(13) 0.0296(12) 0.0038(10) 0.0163(10) 0.0050(10) C44 0.0228(12) 0.0272(12) 0.0285(12) 0.0039(10) 0.0084(9) 0.0025(9) C45 0.0251(11) 0.0175(10) 0.0236(11) 0.0035(9) 0.0092(9) 0.0007(8) C46 0.0247(12) 0.0315(13) 0.0227(11) 0.0042(10) 0.0078(9) 0.0025(10) C47 0.0262(13) 0.0404(15) 0.0290(14) 0.0013(12) 0.0067(11) -0.0014(11) C48 0.083(2) 0.0381(16) 0.0282(15) 0.0111(13) -0.0032(16) -0.0039(16) C49 0.0270(12) 0.0225(11) 0.0218(11) 0.0033(9) 0.0079(9) 0.0009(9) C50 0.0306(14) 0.0346(14) 0.0390(15) 0.0148(12) 0.0077(12) 0.0047(11) C51 0.0290(14) 0.0322(14) 0.0282(13) 0.0023(11) 0.0073(11) -0.0008(10) O52 0.0236(8) 0.0241(8) 0.0352(8) 0.0068(7) 0.0134(6) 0.0020(6) C53 0.0343(16) 0.0314(15) 0.088(2) 0.0059(16) 0.0321(16) 0.0088(12) C54 0.0545(19) 0.0387(16) 0.069(2) 0.0170(15) 0.0353(17) 0.0175(13) C55 0.0505(17) 0.0255(14) 0.0536(18) 0.0109(14) 0.0202(15) 0.0055(12) C56 0.0302(13) 0.0269(12) 0.0330(13) 0.0096(11) 0.0111(11) 0.0024(10) O57 0.109(4) 0.036(2) 0.062(3) 0.0001(19) 0.051(2) 0.0109(19) C58 0.073(4) 0.042(3) 0.066(4) 0.012(3) 0.030(4) 0.005(3) C59 0.099(8) 0.054(6) 0.219(12) 0.009(7) -0.077(7) 0.006(5) C60 0.177(11) 0.156(9) 0.123(8) -0.037(7) 0.090(7) -0.066(8) C61 0.128(7) 0.044(3) 0.062(5) 0.010(3) 0.053(6) 0.000(5) B62 0.0225(13) 0.0232(13) 0.0216(12) 0.0045(10) 0.0064(10) -0.0011(10) C63 0.0209(11) 0.0232(11) 0.0214(11) 0.0029(9) 0.0080(9) -0.0013(8) C64 0.0186(11) 0.0306(12) 0.0235(11) 0.0065(10) 0.0063(9) 0.0000(9) C65 0.0237(12) 0.0215(11) 0.0369(13) 0.0055(10) 0.0131(10) 0.0031(9) C66 0.0306(13) 0.0230(12) 0.0315(12) -0.0035(10) 0.0142(10) -0.0042(9) C67 0.0280(12) 0.0313(13) 0.0230(11) 0.0016(10) 0.0047(9) -0.0036(10) C68 0.0235(11) 0.0238(12) 0.0269(12) 0.0048(10) 0.0071(9) 0.0012(9) F69 0.0276(7) 0.0334(7) 0.0315(7) 0.0090(6) 0.0017(5) 0.0057(5) F70 0.0329(7) 0.0281(7) 0.0506(8) 0.0083(6) 0.0166(6) 0.0081(6) F71 0.0507(9) 0.0289(7) 0.0439(8) -0.0087(7) 0.0170(7) -0.0033(6) F72 0.0477(8) 0.0394(8) 0.0255(7) -0.0026(6) -0.0034(6) -0.0019(6) F73 0.0317(7) 0.0299(7) 0.0271(7) 0.0063(6) 0.0021(5) 0.0053(5) C74 0.0255(11) 0.0231(11) 0.0176(10) 0.0026(9) 0.0062(9) -0.0013(9) C75 0.0278(12) 0.0288(12) 0.0291(12) 0.0061(10) 0.0119(10) -0.0011(10) C76 0.0411(14) 0.0205(12) 0.0382(13) 0.0109(10) 0.0148(11) 0.0011(10) C77 0.0347(14) 0.0288(13) 0.0316(12) 0.0090(10) 0.0112(10) 0.0115(10) C78 0.0245(12) 0.0318(13) 0.0263(12) 0.0055(10) 0.0083(9) 0.0017(9) C79 0.0283(12) 0.0195(11) 0.0246(11) 0.0038(9) 0.0071(9) -0.0009(9) F80 0.0331(7) 0.0264(7) 0.0481(8) 0.0072(6) 0.0156(6) -0.0066(6) F81 0.0571(9) 0.0239(7) 0.0732(10) 0.0195(7) 0.0259(8) 0.0036(6) F82 0.0449(9) 0.0354(8) 0.0605(9) 0.0185(7) 0.0181(7) 0.0170(6) F83 0.0258(7) 0.0377(8) 0.0464(8) 0.0089(6) 0.0114(6) 0.0035(6) F84 0.0268(7) 0.0210(6) 0.0429(7) 0.0072(6) 0.0118(6) -0.0019(5) C85 0.0249(11) 0.0202(11) 0.0227(11) 0.0000(9) 0.0071(9) -0.0028(9) C86 0.0274(12) 0.0293(12) 0.0226(11) 0.0034(10) 0.0063(9) -0.0004(9) C87 0.0239(12) 0.0339(13) 0.0315(12) 0.0012(11) 0.0044(10) 0.0012(10) C88 0.0269(13) 0.0305(13) 0.0381(13) 0.0001(11) 0.0178(10) -0.0030(10) C89 0.0371(14) 0.0292(12) 0.0248(12) 0.0021(10) 0.0149(10) -0.0036(10) C90 0.0259(12) 0.0237(11) 0.0218(11) -0.0003(9) 0.0051(9) -0.0025(9) F91 0.0284(7) 0.0511(8) 0.0266(7) 0.0129(6) 0.0049(5) 0.0025(6) F92 0.0233(7) 0.0581(9) 0.0493(8) 0.0150(7) 0.0051(6) 0.0045(6) F93 0.0312(8) 0.0517(9) 0.0536(9) 0.0099(7) 0.0233(7) 0.0001(6) F94 0.0443(8) 0.0530(9) 0.0320(7) 0.0119(7) 0.0196(6) -0.0030(7) F95 0.0290(7) 0.0442(8) 0.0237(6) 0.0099(6) 0.0043(5) -0.0027(6) C96 0.0206(11) 0.0250(11) 0.0225(11) 0.0036(9) 0.0053(9) 0.0020(9) C97 0.0262(12) 0.0298(12) 0.0264(12) 0.0063(10) 0.0085(9) -0.0016(9) C98 0.0280(12) 0.0352(13) 0.0221(11) -0.0029(10) 0.0028(9) -0.0016(10) C99 0.0258(12) 0.0463(15) 0.0198(11) 0.0086(11) 0.0067(9) 0.0060(10) C100 0.0207(11) 0.0336(13) 0.0282(12) 0.0123(10) 0.0087(9) 0.0037(9) C101 0.0197(11) 0.0267(12) 0.0244(11) 0.0028(10) 0.0059(9) 0.0023(9) F102 0.0451(8) 0.0298(7) 0.0292(7) 0.0003(6) 0.0107(6) -0.0110(6) F103 0.0493(9) 0.0492(9) 0.0261(7) -0.0074(7) 0.0081(6) -0.0117(7) F104 0.0409(8) 0.0643(10) 0.0212(7) 0.0087(7) 0.0101(6) -0.0002(7) F105 0.0319(7) 0.0431(8) 0.0366(7) 0.0173(6) 0.0152(6) 0.0015(6) F106 0.0313(7) 0.0283(7) 0.0297(7) 0.0052(6) 0.0104(5) -0.0044(5) O57A 0.84(7) 0.17(2) 0.110(16) 0.009(14) 0.19(3) -0.20(3) C58A 0.079(11) 0.106(14) 0.108(16) 0.040(15) -0.004(13) -0.016(10) C59A 0.055(11) 0.017(8) 0.15(2) -0.009(10) 0.072(15) -0.010(7) C61A 0.056(9) 0.056(10) 0.033(7) -0.014(7) 0.010(7) -0.020(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 N39 1.7090(16) . ? Ti1 N2 1.9512(16) . ? Ti1 O52 2.0417(14) . ? Ti1 N6 2.0605(15) . ? Ti1 C3 2.6622(19) . ? N2 C3 1.382(2) . ? N2 C7 1.446(2) . ? C3 C4 1.387(3) . ? C3 C19 1.560(3) . ? C4 C5 1.448(3) . ? C4 H107 0.941(19) . ? C5 N6 1.321(2) . ? C5 C23 1.556(3) . ? N6 C27 1.457(2) . ? C7 C12 1.399(3) . ? C7 C8 1.416(3) . ? C8 C9 1.392(3) . ? C8 C16 1.523(3) . ? C9 C10 1.373(3) . ? C9 H108 0.988(19) . ? C10 C11 1.378(3) . ? C10 H109 0.99(2) . ? C11 C12 1.388(3) . ? C11 H110 0.95(2) . ? C12 C13 1.531(3) . ? C13 C15 1.492(5) . ? C13 C14A 1.494(5) . ? C13 C14 1.496(6) . ? C13 C15A 1.639(5) . ? C13 H111 0.88(3) . ? C14 H114 0.9800 . ? C14 H113 0.9800 . ? C14 H112 0.9800 . ? C15 H117 0.9800 . ? C15 H116 0.9800 . ? C15 H115 0.9800 . ? C16 C18 1.530(3) . ? C16 C17 1.530(3) . ? C16 H118 0.955(19) . ? C17 H119 0.98(2) . ? C17 H120 1.03(2) . ? C17 H121 0.95(2) . ? C18 H122 1.00(2) . ? C18 H123 0.96(2) . ? C18 H124 0.97(2) . ? C19 C22 1.359(5) . ? C19 C21A 1.496(5) . ? C19 C20 1.508(3) . ? C19 C21 1.673(5) . ? C19 C22A 1.710(5) . ? C20 H125 1.04(3) . ? C20 H126 0.94(3) . ? C20 H127 0.96(2) . ? C21 H129 0.9800 . ? C21 H128 0.9800 . ? C21 H130 0.9800 . ? C22 H132 0.9800 . ? C22 H133 0.9800 . ? C22 H131 0.9800 . ? C23 C26 1.531(3) . ? C23 C24 1.543(3) . ? C23 C25 1.545(3) . ? C24 H134 0.98(2) . ? C24 H135 1.00(2) . ? C24 H136 0.97(3) . ? C25 H137 0.98(3) . ? C25 H138 0.97(2) . ? C25 H139 1.02(3) . ? C26 H140 1.02(2) . ? C26 H141 0.996(19) . ? C26 H142 0.96(2) . ? C27 C32 1.401(3) . ? C27 C28 1.408(3) . ? C28 C29 1.392(3) . ? C28 C36 1.519(3) . ? C29 C30 1.369(3) . ? C29 H143 0.928(19) . ? C30 C31 1.372(3) . ? C30 H144 0.97(2) . ? C31 C32 1.390(3) . ? C31 H145 0.94(2) . ? C32 C33 1.524(3) . ? C33 C35 1.522(3) . ? C33 C34 1.525(3) . ? C33 H146 0.94(2) . ? C34 H147 1.00(3) . ? C34 H148 0.95(3) . ? C34 H149 0.97(3) . ? C35 H150 0.97(2) . ? C35 H151 0.98(2) . ? C35 H152 1.03(2) . ? C36 C37 1.531(3) . ? C36 C38 1.531(3) . ? C36 H153 0.993(18) . ? C37 H154 0.99(2) . ? C37 H155 1.00(2) . ? C37 H156 1.04(2) . ? C38 H157 0.95(2) . ? C38 H158 1.01(2) . ? C38 H159 0.98(2) . ? N39 C40 1.416(2) . ? C40 C41 1.417(3) . ? C40 C45 1.421(3) . ? C41 C42 1.387(3) . ? C41 C49 1.515(3) . ? C42 C43 1.376(3) . ? C42 H160 0.99(2) . ? C43 C44 1.378(3) . ? C43 H161 0.95(2) . ? C44 C45 1.390(3) . ? C44 H162 0.99(2) . ? C45 C46 1.517(3) . ? C46 C48 1.522(3) . ? C46 C47 1.526(3) . ? C46 H163 0.981(19) . ? C47 H164 0.97(2) . ? C47 H165 0.99(2) . ? C47 H166 0.98(3) . ? C48 H167 1.06(3) . ? C48 H168 0.98(3) . ? C48 H169 0.95(2) . ? C49 C51 1.518(3) . ? C49 C50 1.534(3) . ? C49 H170 0.982(18) . ? C50 H171 1.02(2) . ? C50 H172 0.99(2) . ? C50 H173 1.00(2) . ? C51 H174 0.97(2) . ? C51 H175 0.98(2) . ? C51 H176 0.98(2) . ? O52 C53 1.474(3) . ? O52 C56 1.477(2) . ? C53 C54 1.482(4) . ? C53 H177 0.87(4) . ? C53 H178 0.95(3) . ? C54 C55 1.516(4) . ? C54 H179 0.93(3) . ? C54 H180 1.07(3) . ? C55 C56 1.496(3) . ? C55 H181 0.93(3) . ? C55 H182 0.95(3) . ? C56 H183 1.02(2) . ? C56 H184 1.01(2) . ? O57 C61 1.263(11) . ? O57 C58 1.394(7) . ? C58 C59 1.605(13) . ? C58 H186 0.9900 . ? C58 H185 0.9900 . ? C59 C60 1.451(17) . ? C59 H187 0.9900 . ? C59 H188 0.9900 . ? C60 C61 1.714(16) . ? C60 H190 0.9900 . ? C60 H189 0.9900 . ? C61 H191 0.9900 . ? C61 H192 0.9900 . ? B62 C74 1.643(3) . ? B62 C96 1.655(3) . ? B62 C85 1.659(3) . ? B62 C63 1.660(3) . ? C63 C68 1.388(3) . ? C63 C64 1.389(3) . ? C64 F69 1.350(2) . ? C64 C65 1.375(3) . ? C65 F70 1.349(2) . ? C65 C66 1.373(3) . ? C66 F71 1.346(2) . ? C66 C67 1.365(3) . ? C67 F72 1.349(2) . ? C67 C68 1.384(3) . ? C68 F73 1.351(2) . ? C74 C79 1.391(3) . ? C74 C75 1.391(3) . ? C75 F80 1.355(2) . ? C75 C76 1.379(3) . ? C76 F81 1.349(2) . ? C76 C77 1.365(3) . ? C77 F82 1.344(2) . ? C77 C78 1.375(3) . ? C78 F83 1.348(2) . ? C78 C79 1.366(3) . ? C79 F84 1.358(2) . ? C85 C86 1.382(3) . ? C85 C90 1.395(3) . ? C86 F91 1.353(2) . ? C86 C87 1.385(3) . ? C87 F92 1.347(2) . ? C87 C88 1.371(3) . ? C88 F93 1.344(2) . ? C88 C89 1.373(3) . ? C89 F94 1.352(2) . ? C89 C90 1.372(3) . ? C90 F95 1.353(2) . ? C96 C97 1.381(3) . ? C96 C101 1.384(3) . ? C97 F102 1.365(2) . ? C97 C98 1.373(3) . ? C98 F103 1.353(2) . ? C98 C99 1.376(3) . ? C99 F104 1.341(2) . ? C99 C100 1.362(3) . ? C100 F105 1.354(2) . ? C100 C101 1.386(3) . ? C101 F106 1.353(2) . ? C14A H2A 0.9800 . ? C14A H3A 0.9800 . ? C14A H1A 0.9800 . ? C15A H6A 0.9800 . ? C15A H4A 0.9800 . ? C15A H5A 0.9800 . ? C21A H7A 0.9800 . ? C21A H9A 0.9800 . ? C21A H8A 0.9800 . ? C22A H11A 0.9800 . ? C22A H12A 0.9800 . ? C22A H10A 0.9800 . ? O57A C61A 1.35(4) . ? O57A C58A 1.88(4) . ? C58A C59A 1.28(3) . ? C58A H13A 0.9900 . ? C58A H14A 0.9900 . ? C59A C60A 1.49(3) . ? C59A H16A 0.9900 . ? C59A H15A 0.9900 . ? C60A C61A 1.17(3) . ? C60A H21A 0.9900 . ? C60A H17A 0.9900 . ? C61A H20A 0.9900 . ? C61A H19A 0.9900 . ? 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 N39 Ti1 N2 111.04(7) . . ? N39 Ti1 O52 105.57(7) . . ? N2 Ti1 O52 114.24(6) . . ? N39 Ti1 N6 110.51(7) . . ? N2 Ti1 N6 100.10(6) . . ? O52 Ti1 N6 115.48(6) . . ? N39 Ti1 C3 140.82(7) . . ? N2 Ti1 C3 30.14(6) . . ? O52 Ti1 C3 100.66(6) . . ? N6 Ti1 C3 82.76(6) . . ? C3 N2 C7 122.94(15) . . ? C3 N2 Ti1 104.71(12) . . ? C7 N2 Ti1 131.79(12) . . ? N2 C3 C4 119.31(18) . . ? N2 C3 C19 123.46(17) . . ? C4 C3 C19 117.07(17) . . ? N2 C3 Ti1 45.15(9) . . ? C4 C3 Ti1 81.18(12) . . ? C19 C3 Ti1 146.70(14) . . ? C3 C4 C5 135.3(2) . . ? C3 C4 H107 113.2(12) . . ? C5 C4 H107 110.8(12) . . ? N6 C5 C4 119.48(17) . . ? N6 C5 C23 128.22(18) . . ? C4 C5 C23 112.26(17) . . ? C5 N6 C27 124.35(16) . . ? C5 N6 Ti1 109.50(13) . . ? C27 N6 Ti1 124.53(11) . . ? C12 C7 C8 121.41(18) . . ? C12 C7 N2 118.47(17) . . ? C8 C7 N2 120.06(18) . . ? C9 C8 C7 117.11(19) . . ? C9 C8 C16 118.75(18) . . ? C7 C8 C16 124.14(18) . . ? C10 C9 C8 122.0(2) . . ? C10 C9 H108 120.4(11) . . ? C8 C9 H108 117.6(11) . . ? C9 C10 C11 119.8(2) . . ? C9 C10 H109 119.6(12) . . ? C11 C10 H109 120.5(12) . . ? C10 C11 C12 121.2(2) . . ? C10 C11 H110 117.4(12) . . ? C12 C11 H110 121.4(13) . . ? C11 C12 C7 118.29(19) . . ? C11 C12 C13 119.0(2) . . ? C7 C12 C13 122.74(19) . . ? C15 C13 C14A 133.0(3) . . ? C15 C13 C14 111.5(3) . . ? C15 C13 C12 116.0(3) . . ? C14A C13 C12 109.6(2) . . ? C14 C13 C12 115.9(3) . . ? C14A C13 C15A 106.3(3) . . ? C12 C13 C15A 108.8(2) . . ? C15 C13 H111 82(2) . . ? C14A C13 H111 93(2) . . ? C14 C13 H111 117(2) . . ? C12 C13 H111 110(2) . . ? C15A C13 H111 127(2) . . ? C13 C14 H114 109.5 . . ? C13 C14 H113 109.5 . . ? H114 C14 H113 109.5 . . ? C13 C14 H112 109.5 . . ? H114 C14 H112 109.5 . . ? H113 C14 H112 109.5 . . ? C13 C15 H117 109.5 . . ? C13 C15 H116 109.5 . . ? H117 C15 H116 109.5 . . ? C13 C15 H115 109.5 . . ? H117 C15 H115 109.5 . . ? H116 C15 H115 109.5 . . ? C8 C16 C18 111.32(18) . . ? C8 C16 C17 112.82(18) . . ? C18 C16 C17 108.61(18) . . ? C8 C16 H118 107.6(11) . . ? C18 C16 H118 108.3(11) . . ? C17 C16 H118 108.1(12) . . ? C16 C17 H119 113.3(13) . . ? C16 C17 H120 109.9(12) . . ? H119 C17 H120 108.6(18) . . ? C16 C17 H121 108.7(13) . . ? H119 C17 H121 107.5(18) . . ? H120 C17 H121 108.7(17) . . ? C16 C18 H122 111.7(12) . . ? C16 C18 H123 114.2(12) . . ? H122 C18 H123 107.0(17) . . ? C16 C18 H124 110.8(13) . . ? H122 C18 H124 107.6(17) . . ? H123 C18 H124 105.1(17) . . ? C22 C19 C20 114.6(3) . . ? C21A C19 C20 118.5(3) . . ? C22 C19 C3 116.8(3) . . ? C21A C19 C3 117.8(2) . . ? C20 C19 C3 113.17(19) . . ? C22 C19 C21 109.5(3) . . ? C20 C19 C21 93.2(2) . . ? C3 C19 C21 106.6(2) . . ? C21A C19 C22A 100.9(3) . . ? C20 C19 C22A 98.8(2) . . ? C3 C19 C22A 103.1(2) . . ? C21 C19 C22A 140.3(3) . . ? C19 C20 H125 112.7(14) . . ? C19 C20 H126 112.6(17) . . ? H125 C20 H126 108(2) . . ? C19 C20 H127 105.3(12) . . ? H125 C20 H127 111.5(19) . . ? H126 C20 H127 106(2) . . ? C19 C21 H129 109.5 . . ? C19 C21 H128 109.5 . . ? H129 C21 H128 109.5 . . ? C19 C21 H130 109.5 . . ? H129 C21 H130 109.5 . . ? H128 C21 H130 109.5 . . ? C19 C22 H132 109.5 . . ? C19 C22 H133 109.5 . . ? H132 C22 H133 109.5 . . ? C19 C22 H131 109.5 . . ? H132 C22 H131 109.5 . . ? H133 C22 H131 109.5 . . ? C26 C23 C24 107.0(2) . . ? C26 C23 C25 107.86(19) . . ? C24 C23 C25 109.4(2) . . ? C26 C23 C5 117.37(18) . . ? C24 C23 C5 104.74(18) . . ? C25 C23 C5 110.22(19) . . ? C23 C24 H134 114.3(14) . . ? C23 C24 H135 111.1(13) . . ? H134 C24 H135 105.7(19) . . ? C23 C24 H136 108.1(14) . . ? H134 C24 H136 111.1(19) . . ? H135 C24 H136 106(2) . . ? C23 C25 H137 112.5(14) . . ? C23 C25 H138 106.8(14) . . ? H137 C25 H138 107.0(18) . . ? C23 C25 H139 113.4(14) . . ? H137 C25 H139 112(2) . . ? H138 C25 H139 104.3(19) . . ? C23 C26 H140 106.7(13) . . ? C23 C26 H141 114.2(11) . . ? H140 C26 H141 107.4(17) . . ? C23 C26 H142 114.0(13) . . ? H140 C26 H142 107.6(18) . . ? H141 C26 H142 106.5(16) . . ? C32 C27 C28 121.66(18) . . ? C32 C27 N6 119.35(17) . . ? C28 C27 N6 118.92(17) . . ? C29 C28 C27 117.28(19) . . ? C29 C28 C36 118.34(18) . . ? C27 C28 C36 124.38(18) . . ? C30 C29 C28 121.9(2) . . ? C30 C29 H143 121.5(12) . . ? C28 C29 H143 116.7(12) . . ? C29 C30 C31 119.8(2) . . ? C29 C30 H144 117.8(13) . . ? C31 C30 H144 122.4(13) . . ? C30 C31 C32 121.7(2) . . ? C30 C31 H145 119.5(13) . . ? C32 C31 H145 118.8(13) . . ? C31 C32 C27 117.64(19) . . ? C31 C32 C33 119.28(19) . . ? C27 C32 C33 123.05(19) . . ? C35 C33 C32 111.1(2) . . ? C35 C33 C34 109.8(2) . . ? C32 C33 C34 111.2(2) . . ? C35 C33 H146 108.2(12) . . ? C32 C33 H146 106.2(13) . . ? C34 C33 H146 110.3(12) . . ? C33 C34 H147 112.2(18) . . ? C33 C34 H148 111.8(16) . . ? H147 C34 H148 108(2) . . ? C33 C34 H149 113.1(17) . . ? H147 C34 H149 104(2) . . ? H148 C34 H149 107(2) . . ? C33 C35 H150 111.5(13) . . ? C33 C35 H151 110.1(12) . . ? H150 C35 H151 105.1(18) . . ? C33 C35 H152 111.1(13) . . ? H150 C35 H152 108.4(18) . . ? H151 C35 H152 110.5(18) . . ? C28 C36 C37 110.13(18) . . ? C28 C36 C38 112.98(18) . . ? C37 C36 C38 109.35(19) . . ? C28 C36 H153 108.5(11) . . ? C37 C36 H153 111.0(11) . . ? C38 C36 H153 104.8(10) . . ? C36 C37 H154 110.0(15) . . ? C36 C37 H155 111.6(12) . . ? H154 C37 H155 108.4(18) . . ? C36 C37 H156 110.3(12) . . ? H154 C37 H156 105.7(19) . . ? H155 C37 H156 110.7(18) . . ? C36 C38 H157 110.7(12) . . ? C36 C38 H158 108.2(13) . . ? H157 C38 H158 101.6(18) . . ? C36 C38 H159 111.3(12) . . ? H157 C38 H159 115.1(18) . . ? H158 C38 H159 109.3(18) . . ? C40 N39 Ti1 173.32(14) . . ? N39 C40 C41 118.82(17) . . ? N39 C40 C45 121.35(17) . . ? C41 C40 C45 119.83(17) . . ? C42 C41 C40 118.87(19) . . ? C42 C41 C49 118.37(18) . . ? C40 C41 C49 122.75(17) . . ? C43 C42 C41 121.7(2) . . ? C43 C42 H160 119.5(12) . . ? C41 C42 H160 118.7(12) . . ? C42 C43 C44 119.3(2) . . ? C42 C43 H161 121.6(12) . . ? C44 C43 H161 119.2(12) . . ? C43 C44 C45 122.3(2) . . ? C43 C44 H162 118.4(11) . . ? C45 C44 H162 119.3(11) . . ? C44 C45 C40 117.99(18) . . ? C44 C45 C46 118.27(18) . . ? C40 C45 C46 123.73(17) . . ? C45 C46 C48 111.34(19) . . ? C45 C46 C47 111.82(17) . . ? C48 C46 C47 108.1(2) . . ? C45 C46 H163 109.7(11) . . ? C48 C46 H163 107.5(11) . . ? C47 C46 H163 108.2(11) . . ? C46 C47 H164 112.3(13) . . ? C46 C47 H165 112.9(12) . . ? H164 C47 H165 104.6(17) . . ? C46 C47 H166 113.8(15) . . ? H164 C47 H166 107.9(19) . . ? H165 C47 H166 104.7(19) . . ? C46 C48 H167 106.1(18) . . ? C46 C48 H168 109.7(18) . . ? H167 C48 H168 114(3) . . ? C46 C48 H169 110.9(14) . . ? H167 C48 H169 110(2) . . ? H168 C48 H169 106(2) . . ? C41 C49 C51 111.87(18) . . ? C41 C49 C50 111.29(17) . . ? C51 C49 C50 110.24(18) . . ? C41 C49 H170 106.9(10) . . ? C51 C49 H170 108.1(11) . . ? C50 C49 H170 108.3(11) . . ? C49 C50 H171 108.8(13) . . ? C49 C50 H172 111.3(12) . . ? H171 C50 H172 110.9(17) . . ? C49 C50 H173 111.9(13) . . ? H171 C50 H173 106.6(18) . . ? H172 C50 H173 107.4(18) . . ? C49 C51 H174 110.6(13) . . ? C49 C51 H175 109.9(12) . . ? H174 C51 H175 109.7(17) . . ? C49 C51 H176 112.3(12) . . ? H174 C51 H176 106.9(17) . . ? H175 C51 H176 107.4(17) . . ? C53 O52 C56 107.15(17) . . ? C53 O52 Ti1 123.76(14) . . ? C56 O52 Ti1 128.63(12) . . ? O52 C53 C54 107.2(2) . . ? O52 C53 H177 110(3) . . ? C54 C53 H177 110(3) . . ? O52 C53 H178 103(2) . . ? C54 C53 H178 112(2) . . ? H177 C53 H178 114(3) . . ? C53 C54 C55 105.3(2) . . ? C53 C54 H179 108.7(17) . . ? C55 C54 H179 117.0(17) . . ? C53 C54 H180 106.9(17) . . ? C55 C54 H180 109.1(16) . . ? H179 C54 H180 109(2) . . ? C56 C55 C54 103.8(2) . . ? C56 C55 H181 107.3(16) . . ? C54 C55 H181 110.4(16) . . ? C56 C55 H182 107.5(16) . . ? C54 C55 H182 110.3(15) . . ? H181 C55 H182 117(2) . . ? O52 C56 C55 103.33(18) . . ? O52 C56 H183 106.1(11) . . ? C55 C56 H183 116.5(11) . . ? O52 C56 H184 107.5(11) . . ? C55 C56 H184 110.4(11) . . ? H183 C56 H184 112.2(15) . . ? C61 O57 C58 108.4(6) . . ? O57 C58 C59 105.0(6) . . ? O57 C58 H186 110.7 . . ? C59 C58 H186 110.7 . . ? O57 C58 H185 110.7 . . ? C59 C58 H185 110.7 . . ? H186 C58 H185 108.8 . . ? C60 C59 C58 104.3(9) . . ? C60 C59 H187 110.9 . . ? C58 C59 H187 110.9 . . ? C60 C59 H188 110.9 . . ? C58 C59 H188 110.9 . . ? H187 C59 H188 108.9 . . ? C59 C60 C61 100.1(10) . . ? C59 C60 H190 111.7 . . ? C61 C60 H190 111.8 . . ? C59 C60 H189 111.7 . . ? C61 C60 H189 111.8 . . ? H190 C60 H189 109.5 . . ? O57 C61 C60 104.2(7) . . ? O57 C61 H191 110.9 . . ? C60 C61 H191 110.9 . . ? O57 C61 H192 110.9 . . ? C60 C61 H192 110.9 . . ? H191 C61 H192 108.9 . . ? C74 B62 C96 102.42(16) . . ? C74 B62 C85 114.14(16) . . ? C96 B62 C85 113.28(16) . . ? C74 B62 C63 112.96(16) . . ? C96 B62 C63 114.41(16) . . ? C85 B62 C63 100.19(15) . . ? C68 C63 C64 113.10(18) . . ? C68 C63 B62 126.41(18) . . ? C64 C63 B62 119.79(17) . . ? F69 C64 C65 115.95(18) . . ? F69 C64 C63 119.51(18) . . ? C65 C64 C63 124.53(19) . . ? F70 C65 C66 119.20(19) . . ? F70 C65 C64 121.26(19) . . ? C66 C65 C64 119.53(19) . . ? F71 C66 C67 120.73(19) . . ? F71 C66 C65 120.3(2) . . ? C67 C66 C65 118.93(19) . . ? F72 C67 C66 119.96(19) . . ? F72 C67 C68 120.29(19) . . ? C66 C67 C68 119.76(19) . . ? F73 C68 C67 114.93(17) . . ? F73 C68 C63 120.97(18) . . ? C67 C68 C63 124.08(19) . . ? C79 C74 C75 112.46(19) . . ? C79 C74 B62 119.52(17) . . ? C75 C74 B62 127.79(18) . . ? F80 C75 C76 115.67(18) . . ? F80 C75 C74 120.46(19) . . ? C76 C75 C74 123.9(2) . . ? F81 C76 C77 119.8(2) . . ? F81 C76 C75 120.0(2) . . ? C77 C76 C75 120.2(2) . . ? F82 C77 C76 120.8(2) . . ? F82 C77 C78 120.3(2) . . ? C76 C77 C78 118.9(2) . . ? F83 C78 C79 121.47(19) . . ? F83 C78 C77 119.66(19) . . ? C79 C78 C77 118.9(2) . . ? F84 C79 C78 115.97(18) . . ? F84 C79 C74 118.41(18) . . ? C78 C79 C74 125.60(19) . . ? C86 C85 C90 112.64(18) . . ? C86 C85 B62 126.87(18) . . ? C90 C85 B62 120.03(18) . . ? F91 C86 C85 120.88(18) . . ? F91 C86 C87 114.63(18) . . ? C85 C86 C87 124.48(19) . . ? F92 C87 C88 119.71(19) . . ? F92 C87 C86 120.41(19) . . ? C88 C87 C86 119.9(2) . . ? F93 C88 C87 120.7(2) . . ? F93 C88 C89 120.83(19) . . ? C87 C88 C89 118.41(19) . . ? F94 C89 C88 119.69(19) . . ? F94 C89 C90 120.5(2) . . ? C88 C89 C90 119.81(19) . . ? F95 C90 C89 115.92(18) . . ? F95 C90 C85 119.30(18) . . ? C89 C90 C85 124.8(2) . . ? C97 C96 C101 113.23(18) . . ? C97 C96 B62 119.26(18) . . ? C101 C96 B62 127.15(18) . . ? F102 C97 C98 115.98(18) . . ? F102 C97 C96 118.95(17) . . ? C98 C97 C96 125.1(2) . . ? F103 C98 C97 121.02(19) . . ? F103 C98 C99 119.67(18) . . ? C97 C98 C99 119.3(2) . . ? F104 C99 C100 121.06(19) . . ? F104 C99 C98 120.6(2) . . ? C100 C99 C98 118.37(19) . . ? F105 C100 C99 119.73(18) . . ? F105 C100 C101 119.72(19) . . ? C99 C100 C101 120.55(19) . . ? F106 C101 C96 121.12(17) . . ? F106 C101 C100 115.44(17) . . ? C96 C101 C100 123.44(19) . . ? C13 C14A H2A 109.5 . . ? C13 C14A H3A 109.5 . . ? H2A C14A H3A 109.5 . . ? C13 C14A H1A 109.5 . . ? H2A C14A H1A 109.5 . . ? H3A C14A H1A 109.5 . . ? C13 C15A H6A 109.5 . . ? C13 C15A H4A 109.5 . . ? H6A C15A H4A 109.5 . . ? C13 C15A H5A 109.5 . . ? H6A C15A H5A 109.5 . . ? H4A C15A H5A 109.5 . . ? C19 C21A H7A 109.5 . . ? C19 C21A H9A 109.5 . . ? H7A C21A H9A 109.5 . . ? C19 C21A H8A 109.5 . . ? H7A C21A H8A 109.5 . . ? H9A C21A H8A 109.5 . . ? C19 C22A H11A 109.5 . . ? C19 C22A H12A 109.5 . . ? H11A C22A H12A 109.5 . . ? C19 C22A H10A 109.5 . . ? H11A C22A H10A 109.5 . . ? H12A C22A H10A 109.5 . . ? C61A O57A C58A 84.9(15) . . ? C59A C58A O57A 80(2) . . ? C59A C58A H13A 115.3 . . ? O57A C58A H13A 115.3 . . ? C59A C58A H14A 115.2 . . ? O57A C58A H14A 115.2 . . ? H13A C58A H14A 112.3 . . ? C58A C59A C60A 95.2(16) . . ? C58A C59A H16A 112.7 . . ? C60A C59A H16A 112.7 . . ? C58A C59A H15A 112.7 . . ? C60A C59A H15A 112.7 . . ? H16A C59A H15A 110.2 . . ? C61A C60A C59A 116.2(15) . . ? C61A C60A H21A 108.2 . . ? C59A C60A H21A 108.2 . . ? C61A C60A H17A 108.2 . . ? C59A C60A H17A 108.2 . . ? H21A C60A H17A 107.4 . . ? C60A C61A O57A 95(2) . . ? C60A C61A H20A 112.7 . . ? O57A C61A H20A 112.7 . . ? C60A C61A H19A 112.7 . . ? O57A C61A H19A 112.7 . . ? H20A C61A H19A 110.2 . . ? 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 N39 Ti1 N2 C3 172.55(12) . . . . ? O52 Ti1 N2 C3 -68.20(13) . . . . ? N6 Ti1 N2 C3 55.82(13) . . . . ? N39 Ti1 N2 C7 -16.10(19) . . . . ? O52 Ti1 N2 C7 103.15(17) . . . . ? N6 Ti1 N2 C7 -132.83(17) . . . . ? C3 Ti1 N2 C7 171.3(2) . . . . ? C7 N2 C3 C4 151.46(19) . . . . ? Ti1 N2 C3 C4 -36.2(2) . . . . ? C7 N2 C3 C19 -33.2(3) . . . . ? Ti1 N2 C3 C19 139.08(17) . . . . ? C7 N2 C3 Ti1 -172.3(2) . . . . ? N39 Ti1 C3 N2 -11.04(18) . . . . ? O52 Ti1 C3 N2 120.51(12) . . . . ? N6 Ti1 C3 N2 -124.81(13) . . . . ? N39 Ti1 C3 C4 137.54(14) . . . . ? N2 Ti1 C3 C4 148.6(2) . . . . ? O52 Ti1 C3 C4 -90.91(13) . . . . ? N6 Ti1 C3 C4 23.76(13) . . . . ? N39 Ti1 C3 C19 -95.4(3) . . . . ? N2 Ti1 C3 C19 -84.4(3) . . . . ? O52 Ti1 C3 C19 36.1(2) . . . . ? N6 Ti1 C3 C19 150.8(2) . . . . ? N2 C3 C4 C5 -13.6(4) . . . . ? C19 C3 C4 C5 170.8(2) . . . . ? Ti1 C3 C4 C5 -38.7(2) . . . . ? C3 C4 C5 N6 35.2(4) . . . . ? C3 C4 C5 C23 -142.9(2) . . . . ? C4 C5 N6 C27 169.19(18) . . . . ? C23 C5 N6 C27 -13.1(3) . . . . ? C4 C5 N6 Ti1 3.2(2) . . . . ? C23 C5 N6 Ti1 -179.15(17) . . . . ? N39 Ti1 N6 C5 -157.26(13) . . . . ? N2 Ti1 N6 C5 -40.13(14) . . . . ? O52 Ti1 N6 C5 83.02(14) . . . . ? C3 Ti1 N6 C5 -15.37(13) . . . . ? N39 Ti1 N6 C27 36.77(16) . . . . ? N2 Ti1 N6 C27 153.90(15) . . . . ? O52 Ti1 N6 C27 -82.95(15) . . . . ? C3 Ti1 N6 C27 178.65(15) . . . . ? C3 N2 C7 C12 -75.0(2) . . . . ? Ti1 N2 C7 C12 114.98(18) . . . . ? C3 N2 C7 C8 107.9(2) . . . . ? Ti1 N2 C7 C8 -62.1(2) . . . . ? C12 C7 C8 C9 3.6(3) . . . . ? N2 C7 C8 C9 -179.38(17) . . . . ? C12 C7 C8 C16 -176.18(18) . . . . ? N2 C7 C8 C16 0.9(3) . . . . ? C7 C8 C9 C10 -1.0(3) . . . . ? C16 C8 C9 C10 178.75(19) . . . . ? C8 C9 C10 C11 -1.8(3) . . . . ? C9 C10 C11 C12 2.2(3) . . . . ? C10 C11 C12 C7 0.4(3) . . . . ? C10 C11 C12 C13 -178.5(2) . . . . ? C8 C7 C12 C11 -3.3(3) . . . . ? N2 C7 C12 C11 179.64(17) . . . . ? C8 C7 C12 C13 175.49(19) . . . . ? N2 C7 C12 C13 -1.6(3) . . . . ? C11 C12 C13 C15 -92.1(3) . . . . ? C7 C12 C13 C15 89.2(3) . . . . ? C11 C12 C13 C14A 76.2(3) . . . . ? C7 C12 C13 C14A -102.6(3) . . . . ? C11 C12 C13 C14 41.6(4) . . . . ? C7 C12 C13 C14 -137.2(3) . . . . ? C11 C12 C13 C15A -39.7(3) . . . . ? C7 C12 C13 C15A 141.6(3) . . . . ? C9 C8 C16 C18 -71.5(2) . . . . ? C7 C8 C16 C18 108.3(2) . . . . ? C9 C8 C16 C17 50.9(3) . . . . ? C7 C8 C16 C17 -129.3(2) . . . . ? N2 C3 C19 C22 -47.7(4) . . . . ? C4 C3 C19 C22 127.7(3) . . . . ? Ti1 C3 C19 C22 10.1(4) . . . . ? N2 C3 C19 C21A 31.6(4) . . . . ? C4 C3 C19 C21A -153.0(3) . . . . ? Ti1 C3 C19 C21A 89.4(4) . . . . ? N2 C3 C19 C20 176.0(2) . . . . ? C4 C3 C19 C20 -8.6(3) . . . . ? Ti1 C3 C19 C20 -126.3(2) . . . . ? N2 C3 C19 C21 75.0(3) . . . . ? C4 C3 C19 C21 -109.6(3) . . . . ? Ti1 C3 C19 C21 132.7(3) . . . . ? N2 C3 C19 C22A -78.3(3) . . . . ? C4 C3 C19 C22A 97.1(2) . . . . ? Ti1 C3 C19 C22A -20.6(3) . . . . ? N6 C5 C23 C26 -0.5(3) . . . . ? C4 C5 C23 C26 177.3(2) . . . . ? N6 C5 C23 C24 -118.9(3) . . . . ? C4 C5 C23 C24 58.9(3) . . . . ? N6 C5 C23 C25 123.5(2) . . . . ? C4 C5 C23 C25 -58.7(2) . . . . ? C5 N6 C27 C32 110.0(2) . . . . ? Ti1 N6 C27 C32 -86.0(2) . . . . ? C5 N6 C27 C28 -73.0(2) . . . . ? Ti1 N6 C27 C28 90.89(19) . . . . ? C32 C27 C28 C29 -2.2(3) . . . . ? N6 C27 C28 C29 -179.09(16) . . . . ? C32 C27 C28 C36 177.20(18) . . . . ? N6 C27 C28 C36 0.3(3) . . . . ? C27 C28 C29 C30 -0.8(3) . . . . ? C36 C28 C29 C30 179.73(19) . . . . ? C28 C29 C30 C31 2.0(3) . . . . ? C29 C30 C31 C32 -0.2(3) . . . . ? C30 C31 C32 C27 -2.7(3) . . . . ? C30 C31 C32 C33 179.0(2) . . . . ? C28 C27 C32 C31 3.9(3) . . . . ? N6 C27 C32 C31 -179.23(17) . . . . ? C28 C27 C32 C33 -177.85(18) . . . . ? N6 C27 C32 C33 -1.0(3) . . . . ? C31 C32 C33 C35 -48.2(3) . . . . ? C27 C32 C33 C35 133.6(2) . . . . ? C31 C32 C33 C34 74.3(3) . . . . ? C27 C32 C33 C34 -103.9(3) . . . . ? C29 C28 C36 C37 75.3(2) . . . . ? C27 C28 C36 C37 -104.1(2) . . . . ? C29 C28 C36 C38 -47.3(3) . . . . ? C27 C28 C36 C38 133.3(2) . . . . ? N39 C40 C41 C42 177.59(17) . . . . ? C45 C40 C41 C42 -1.7(3) . . . . ? N39 C40 C41 C49 -3.6(3) . . . . ? C45 C40 C41 C49 177.17(18) . . . . ? C40 C41 C42 C43 -0.1(3) . . . . ? C49 C41 C42 C43 -178.96(19) . . . . ? C41 C42 C43 C44 1.4(3) . . . . ? C42 C43 C44 C45 -1.0(3) . . . . ? C43 C44 C45 C40 -0.8(3) . . . . ? C43 C44 C45 C46 178.10(19) . . . . ? N39 C40 C45 C44 -177.18(17) . . . . ? C41 C40 C45 C44 2.1(3) . . . . ? N39 C40 C45 C46 4.0(3) . . . . ? C41 C40 C45 C46 -176.74(18) . . . . ? C44 C45 C46 C48 69.1(3) . . . . ? C40 C45 C46 C48 -112.1(3) . . . . ? C44 C45 C46 C47 -52.0(3) . . . . ? C40 C45 C46 C47 126.8(2) . . . . ? C42 C41 C49 C51 -67.3(2) . . . . ? C40 C41 C49 C51 113.8(2) . . . . ? C42 C41 C49 C50 56.5(3) . . . . ? C40 C41 C49 C50 -122.4(2) . . . . ? N39 Ti1 O52 C53 -174.6(2) . . . . ? N2 Ti1 O52 C53 63.1(2) . . . . ? N6 Ti1 O52 C53 -52.3(2) . . . . ? C3 Ti1 O52 C53 34.7(2) . . . . ? N39 Ti1 O52 C56 14.20(17) . . . . ? N2 Ti1 O52 C56 -108.09(16) . . . . ? N6 Ti1 O52 C56 136.59(15) . . . . ? C3 Ti1 O52 C56 -136.41(16) . . . . ? C56 O52 C53 C54 12.9(3) . . . . ? Ti1 O52 C53 C54 -159.9(2) . . . . ? O52 C53 C54 C55 10.2(4) . . . . ? C53 C54 C55 C56 -29.0(3) . . . . ? C53 O52 C56 C55 -30.9(3) . . . . ? Ti1 O52 C56 C55 141.40(17) . . . . ? C54 C55 C56 O52 36.6(3) . . . . ? C61 O57 C58 C59 41.1(7) . . . . ? O57 C58 C59 C60 -18.2(11) . . . . ? C58 C59 C60 C61 -4.5(11) . . . . ? C58 O57 C61 C60 -43.5(8) . . . . ? C59 C60 C61 O57 29.1(11) . . . . ? C74 B62 C63 C68 -20.2(3) . . . . ? C96 B62 C63 C68 -136.8(2) . . . . ? C85 B62 C63 C68 101.7(2) . . . . ? C74 B62 C63 C64 170.14(17) . . . . ? C96 B62 C63 C64 53.5(2) . . . . ? C85 B62 C63 C64 -68.0(2) . . . . ? C68 C63 C64 F69 -178.76(16) . . . . ? B62 C63 C64 F69 -7.8(3) . . . . ? C68 C63 C64 C65 0.2(3) . . . . ? B62 C63 C64 C65 171.15(18) . . . . ? F69 C64 C65 F70 -3.3(3) . . . . ? C63 C64 C65 F70 177.79(17) . . . . ? F69 C64 C65 C66 176.53(17) . . . . ? C63 C64 C65 C66 -2.4(3) . . . . ? F70 C65 C66 F71 2.6(3) . . . . ? C64 C65 C66 F71 -177.18(17) . . . . ? F70 C65 C66 C67 -177.35(18) . . . . ? C64 C65 C66 C67 2.9(3) . . . . ? F71 C66 C67 F72 -0.6(3) . . . . ? C65 C66 C67 F72 179.40(18) . . . . ? F71 C66 C67 C68 178.89(17) . . . . ? C65 C66 C67 C68 -1.1(3) . . . . ? F72 C67 C68 F73 -0.1(3) . . . . ? C66 C67 C68 F73 -179.52(18) . . . . ? F72 C67 C68 C63 178.23(18) . . . . ? C66 C67 C68 C63 -1.2(3) . . . . ? C64 C63 C68 F73 179.87(17) . . . . ? B62 C63 C68 F73 9.6(3) . . . . ? C64 C63 C68 C67 1.7(3) . . . . ? B62 C63 C68 C67 -168.60(19) . . . . ? C96 B62 C74 C79 69.0(2) . . . . ? C85 B62 C74 C79 -168.15(17) . . . . ? C63 B62 C74 C79 -54.5(2) . . . . ? C96 B62 C74 C75 -105.0(2) . . . . ? C85 B62 C74 C75 17.8(3) . . . . ? C63 B62 C74 C75 131.4(2) . . . . ? C79 C74 C75 F80 -178.03(17) . . . . ? B62 C74 C75 F80 -3.6(3) . . . . ? C79 C74 C75 C76 1.6(3) . . . . ? B62 C74 C75 C76 176.0(2) . . . . ? F80 C75 C76 F81 -0.5(3) . . . . ? C74 C75 C76 F81 179.87(19) . . . . ? F80 C75 C76 C77 179.41(19) . . . . ? C74 C75 C76 C77 -0.3(3) . . . . ? F81 C76 C77 F82 -0.6(3) . . . . ? C75 C76 C77 F82 179.56(19) . . . . ? F81 C76 C77 C78 179.95(19) . . . . ? C75 C76 C77 C78 0.1(3) . . . . ? F82 C77 C78 F83 0.4(3) . . . . ? C76 C77 C78 F83 179.88(19) . . . . ? F82 C77 C78 C79 179.13(18) . . . . ? C76 C77 C78 C79 -1.4(3) . . . . ? F83 C78 C79 F84 0.2(3) . . . . ? C77 C78 C79 F84 -178.50(18) . . . . ? F83 C78 C79 C74 -178.18(18) . . . . ? C77 C78 C79 C74 3.1(3) . . . . ? C75 C74 C79 F84 178.55(17) . . . . ? B62 C74 C79 F84 3.6(3) . . . . ? C75 C74 C79 C78 -3.1(3) . . . . ? B62 C74 C79 C78 -178.03(19) . . . . ? C74 B62 C85 C86 -136.0(2) . . . . ? C96 B62 C85 C86 -19.3(3) . . . . ? C63 B62 C85 C86 103.0(2) . . . . ? C74 B62 C85 C90 52.4(2) . . . . ? C96 B62 C85 C90 169.11(18) . . . . ? C63 B62 C85 C90 -68.6(2) . . . . ? C90 C85 C86 F91 178.11(18) . . . . ? B62 C85 C86 F91 6.0(3) . . . . ? C90 C85 C86 C87 -1.5(3) . . . . ? B62 C85 C86 C87 -173.6(2) . . . . ? F91 C86 C87 F92 0.1(3) . . . . ? C85 C86 C87 F92 179.7(2) . . . . ? F91 C86 C87 C88 -178.72(19) . . . . ? C85 C86 C87 C88 0.9(3) . . . . ? F92 C87 C88 F93 -0.5(3) . . . . ? C86 C87 C88 F93 178.27(19) . . . . ? F92 C87 C88 C89 -178.64(19) . . . . ? C86 C87 C88 C89 0.1(3) . . . . ? F93 C88 C89 F94 0.2(3) . . . . ? C87 C88 C89 F94 178.34(19) . . . . ? F93 C88 C89 C90 -178.53(19) . . . . ? C87 C88 C89 C90 -0.4(3) . . . . ? F94 C89 C90 F95 -0.4(3) . . . . ? C88 C89 C90 F95 178.38(19) . . . . ? F94 C89 C90 C85 -179.04(19) . . . . ? C88 C89 C90 C85 -0.3(3) . . . . ? C86 C85 C90 F95 -177.46(18) . . . . ? B62 C85 C90 F95 -4.7(3) . . . . ? C86 C85 C90 C89 1.2(3) . . . . ? B62 C85 C90 C89 173.9(2) . . . . ? C74 B62 C96 C97 67.6(2) . . . . ? C85 B62 C96 C97 -55.8(3) . . . . ? C63 B62 C96 C97 -169.80(18) . . . . ? C74 B62 C96 C101 -105.1(2) . . . . ? C85 B62 C96 C101 131.5(2) . . . . ? C63 B62 C96 C101 17.5(3) . . . . ? C101 C96 C97 F102 178.63(18) . . . . ? B62 C96 C97 F102 5.0(3) . . . . ? C101 C96 C97 C98 -1.9(3) . . . . ? B62 C96 C97 C98 -175.5(2) . . . . ? F102 C97 C98 F103 0.0(3) . . . . ? C96 C97 C98 F103 -179.56(19) . . . . ? F102 C97 C98 C99 -179.12(19) . . . . ? C96 C97 C98 C99 1.3(3) . . . . ? F103 C98 C99 F104 0.2(3) . . . . ? C97 C98 C99 F104 179.26(19) . . . . ? F103 C98 C99 C100 -179.64(19) . . . . ? C97 C98 C99 C100 -0.5(3) . . . . ? F104 C99 C100 F105 0.7(3) . . . . ? C98 C99 C100 F105 -179.52(19) . . . . ? F104 C99 C100 C101 -179.37(18) . . . . ? C98 C99 C100 C101 0.4(3) . . . . ? C97 C96 C101 F106 -177.91(17) . . . . ? B62 C96 C101 F106 -4.8(3) . . . . ? C97 C96 C101 C100 1.7(3) . . . . ? B62 C96 C101 C100 174.77(19) . . . . ? F105 C100 C101 F106 -1.5(3) . . . . ? C99 C100 C101 F106 178.53(18) . . . . ? F105 C100 C101 C96 178.85(18) . . . . ? C99 C100 C101 C96 -1.1(3) . . . . ? C61A O57A C58A C59A 79(3) . . . . ? O57A C58A C59A C60A -52.2(15) . . . . ? C58A C59A C60A C61A 30(3) . . . . ? C59A C60A C61A O57A 33(2) . . . . ? C58A O57A C61A C60A -58.0(19) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.318 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.052 data_04191 _database_code_depnum_ccdc_archive 'CCDC 260835' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H70 F3 N3 O3 S Ti' _chemical_formula_weight 874.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pbca ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 21.124(10) _cell_length_b 22.856(11) _cell_length_c 38.962(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 18811(16) _cell_formula_units_Z 16 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 1450 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 17.27 _exptl_crystal_description 'irregular fragment' _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7488 _exptl_absorpt_coefficient_mu 0.281 _exptl_absorpt_correction_type none _exptl_special_details ; All crystals examined tended to be severely twinned and/or split and appeared to decompose repidly, even when handled in the nitrogen filled glove bag. After several attempts to locate a suitable crystal one was chosen that had one well-formed lattice present as determined using graphical techniques (RLATT and local programs). The crystal was twinned with a minor component as well as numerous small fragments. The secondary component was rotated from first (primary) domain by 2.3 degrees about reciprocal axis -0.099 0.182 1.000 and real axis -0.331 0.529 1.000. Attempts to utilize the integrated intensities of the secondary component were unsuccessful. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details ' 0.30 degree frames measured for 30.16 seconds each' _diffrn_measurement_method '\w scans' _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 281424 _diffrn_reflns_av_R_equivalents 0.6168 _diffrn_reflns_av_sigmaI/netI 0.3542 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 27.46 _reflns_number_total 21492 _reflns_number_gt 6126 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999), XTEL (local package)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Reciprocal Net (http://recipnet.org)' _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^)+(0.0566P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21492 _refine_ls_number_parameters 1094 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2777 _refine_ls_R_factor_gt 0.0867 _refine_ls_wR_factor_ref 0.2183 _refine_ls_wR_factor_gt 0.1529 _refine_ls_goodness_of_fit_ref 0.833 _refine_ls_restrained_S_all 0.833 _refine_ls_shift/su_max 0.000 _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 0.20807(5) 0.22129(5) 0.00668(3) 0.0201(3) Uani 1 1 d . . . N2 N 0.2292(2) 0.3074(2) -0.00214(12) 0.0180(12) Uani 1 1 d . . . C3 C 0.1734(3) 0.3327(3) -0.00824(15) 0.0201(14) Uani 1 1 d . . . C4 C 0.1210(3) 0.2987(3) -0.01885(15) 0.0228(15) Uani 1 1 d . . . H4 H 0.0815 0.3161 -0.0132 0.027 Uiso 1 1 calc R . . C5 C 0.1142(3) 0.2436(3) -0.03634(15) 0.0220(15) Uani 1 1 d . . . N6 N 0.1629(2) 0.2070(2) -0.03763(12) 0.0221(13) Uani 1 1 d . . . C7 C 0.2857(3) 0.3383(3) 0.00793(17) 0.0246(15) Uani 1 1 d . . . C8 C 0.3322(3) 0.3523(3) -0.01671(16) 0.0230(15) Uani 1 1 d . . . C9 C 0.3836(3) 0.3860(3) -0.00649(18) 0.0289(16) Uani 1 1 d . . . H9 H 0.4144 0.3974 -0.0229 0.035 Uiso 1 1 calc R . . C10 C 0.3902(3) 0.4029(3) 0.02739(18) 0.0332(18) Uani 1 1 d . . . H10 H 0.4253 0.4264 0.0339 0.040 Uiso 1 1 calc R . . C11 C 0.3468(3) 0.3863(3) 0.05167(18) 0.0294(17) Uani 1 1 d . . . H11 H 0.3528 0.3976 0.0749 0.035 Uiso 1 1 calc R . . C12 C 0.2948(3) 0.3535(3) 0.04292(15) 0.0219(15) Uani 1 1 d . . . C13 C 0.2491(3) 0.3343(3) 0.07089(16) 0.0303(17) Uani 1 1 d . . . H13 H 0.2078 0.3243 0.0599 0.036 Uiso 1 1 calc R . . C14 C 0.2372(4) 0.3814(3) 0.09795(18) 0.043(2) Uani 1 1 d . . . H14A H 0.2757 0.3872 0.1116 0.064 Uiso 1 1 calc R . . H14B H 0.2026 0.3690 0.1130 0.064 Uiso 1 1 calc R . . H14C H 0.2258 0.4182 0.0866 0.064 Uiso 1 1 calc R . . C15 C 0.2763(3) 0.2785(3) 0.08740(17) 0.041(2) Uani 1 1 d . . . H15A H 0.3152 0.2881 0.0999 0.062 Uiso 1 1 calc R . . H15B H 0.2857 0.2497 0.0695 0.062 Uiso 1 1 calc R . . H15C H 0.2451 0.2621 0.1034 0.062 Uiso 1 1 calc R . . C16 C 0.3259(3) 0.3324(3) -0.05439(17) 0.0292(16) Uani 1 1 d . . . H16 H 0.3107 0.2909 -0.0541 0.035 Uiso 1 1 calc R . . C17 C 0.3889(3) 0.3332(3) -0.07343(18) 0.041(2) Uani 1 1 d . . . H17A H 0.3843 0.3129 -0.0955 0.062 Uiso 1 1 calc R . . H17B H 0.4211 0.3134 -0.0596 0.062 Uiso 1 1 calc R . . H17C H 0.4018 0.3738 -0.0775 0.062 Uiso 1 1 calc R . . C18 C 0.2775(4) 0.3680(3) -0.07411(17) 0.040(2) Uani 1 1 d . . . H18A H 0.2886 0.4096 -0.0728 0.061 Uiso 1 1 calc R . . H18B H 0.2355 0.3620 -0.0641 0.061 Uiso 1 1 calc R . . H18C H 0.2772 0.3556 -0.0982 0.061 Uiso 1 1 calc R . . C19 C 0.1542(3) 0.3988(3) -0.00282(16) 0.0265(16) Uani 1 1 d . . . C20 C 0.2079(3) 0.4422(3) 0.00268(17) 0.0283(16) Uani 1 1 d . . . H20A H 0.1908 0.4820 0.0031 0.043 Uiso 1 1 calc R . . H20B H 0.2386 0.4385 -0.0161 0.043 Uiso 1 1 calc R . . H20C H 0.2288 0.4338 0.0246 0.043 Uiso 1 1 calc R . . C21 C 0.1189(3) 0.4209(3) -0.03528(17) 0.0340(18) Uani 1 1 d . . . H21A H 0.1070 0.4620 -0.0321 0.051 Uiso 1 1 calc R . . H21B H 0.0807 0.3974 -0.0389 0.051 Uiso 1 1 calc R . . H21C H 0.1467 0.4173 -0.0553 0.051 Uiso 1 1 calc R . . C22 C 0.1087(3) 0.4025(3) 0.02799(17) 0.0342(18) Uani 1 1 d . . . H22A H 0.1307 0.3896 0.0488 0.051 Uiso 1 1 calc R . . H22B H 0.0720 0.3772 0.0239 0.051 Uiso 1 1 calc R . . H22C H 0.0945 0.4430 0.0309 0.051 Uiso 1 1 calc R . . C23 C 0.0451(3) 0.2338(3) -0.04936(18) 0.0308(17) Uani 1 1 d . . . C24 C 0.0180(4) 0.2878(3) -0.0669(2) 0.054(2) Uani 1 1 d . . . H24A H 0.0452 0.2989 -0.0862 0.081 Uiso 1 1 calc R . . H24B H 0.0160 0.3201 -0.0504 0.081 Uiso 1 1 calc R . . H24C H -0.0247 0.2791 -0.0754 0.081 Uiso 1 1 calc R . . C25 C 0.0343(3) 0.1830(3) -0.07409(19) 0.039(2) Uani 1 1 d . . . H25A H -0.0110 0.1791 -0.0788 0.059 Uiso 1 1 calc R . . H25B H 0.0501 0.1467 -0.0637 0.059 Uiso 1 1 calc R . . H25C H 0.0570 0.1905 -0.0956 0.059 Uiso 1 1 calc R . . C26 C 0.0043(3) 0.2201(3) -0.01655(19) 0.043(2) Uani 1 1 d . . . H26A H -0.0397 0.2131 -0.0233 0.064 Uiso 1 1 calc R . . H26B H 0.0062 0.2535 -0.0008 0.064 Uiso 1 1 calc R . . H26C H 0.0211 0.1852 -0.0051 0.064 Uiso 1 1 calc R . . C27 C 0.1675(3) 0.1572(3) -0.06045(17) 0.0276(17) Uani 1 1 d . . . C28 C 0.1520(3) 0.1009(3) -0.04891(17) 0.0285(17) Uani 1 1 d . . . C29 C 0.1595(3) 0.0546(3) -0.07133(18) 0.0353(18) Uani 1 1 d . . . H29 H 0.1509 0.0160 -0.0635 0.042 Uiso 1 1 calc R . . C30 C 0.1794(4) 0.0630(3) -0.10506(19) 0.042(2) Uani 1 1 d . . . H30 H 0.1823 0.0308 -0.1204 0.050 Uiso 1 1 calc R . . C31 C 0.1944(4) 0.1180(4) -0.11577(19) 0.042(2) Uani 1 1 d . . . H31 H 0.2082 0.1234 -0.1388 0.051 Uiso 1 1 calc R . . C32 C 0.1904(3) 0.1659(3) -0.09454(17) 0.0326(18) Uani 1 1 d . . . C33 C 0.2096(4) 0.2262(3) -0.10791(17) 0.0392(19) Uani 1 1 d . . . H33 H 0.2144 0.2523 -0.0875 0.047 Uiso 1 1 calc R . . C34 C 0.2720(4) 0.2255(4) -0.1262(2) 0.067(3) Uani 1 1 d . . . H34A H 0.2700 0.1979 -0.1454 0.100 Uiso 1 1 calc R . . H34B H 0.3053 0.2133 -0.1102 0.100 Uiso 1 1 calc R . . H34C H 0.2814 0.2648 -0.1349 0.100 Uiso 1 1 calc R . . C35 C 0.1600(5) 0.2531(4) -0.1305(3) 0.092(4) Uani 1 1 d . . . H35A H 0.1709 0.2941 -0.1351 0.137 Uiso 1 1 calc R . . H35B H 0.1188 0.2513 -0.1190 0.137 Uiso 1 1 calc R . . H35C H 0.1579 0.2317 -0.1523 0.137 Uiso 1 1 calc R . . C36 C 0.1270(3) 0.0885(3) -0.01256(17) 0.0301(17) Uani 1 1 d . . . H36 H 0.1194 0.1272 -0.0013 0.036 Uiso 1 1 calc R . . C37 C 0.0645(3) 0.0561(3) -0.0128(2) 0.044(2) Uani 1 1 d . . . H37A H 0.0714 0.0156 -0.0203 0.066 Uiso 1 1 calc R . . H37B H 0.0352 0.0754 -0.0287 0.066 Uiso 1 1 calc R . . H37C H 0.0464 0.0561 0.0103 0.066 Uiso 1 1 calc R . . C38 C 0.1753(3) 0.0561(3) 0.00906(18) 0.0389(19) Uani 1 1 d . . . H38A H 0.1596 0.0527 0.0327 0.058 Uiso 1 1 calc R . . H38B H 0.2154 0.0776 0.0090 0.058 Uiso 1 1 calc R . . H38C H 0.1820 0.0169 -0.0005 0.058 Uiso 1 1 calc R . . N39 N 0.2744(2) 0.1789(2) 0.01020(12) 0.0194(12) Uani 1 1 d . . . C40 C 0.3273(3) 0.1410(3) 0.01472(16) 0.0234(15) Uani 1 1 d . . . C41 C 0.3680(3) 0.1278(3) -0.01274(16) 0.0255(16) Uani 1 1 d . . . C42 C 0.4205(3) 0.0925(3) -0.00697(19) 0.0351(18) Uani 1 1 d . . . H42 H 0.4474 0.0831 -0.0257 0.042 Uiso 1 1 calc R . . C43 C 0.4348(3) 0.0706(3) 0.0249(2) 0.0370(19) Uani 1 1 d . . . H43 H 0.4719 0.0480 0.0285 0.044 Uiso 1 1 calc R . . C44 C 0.3940(3) 0.0823(3) 0.05146(19) 0.0366(19) Uani 1 1 d . . . H44 H 0.4035 0.0668 0.0735 0.044 Uiso 1 1 calc R . . C45 C 0.3397(3) 0.1159(3) 0.04766(16) 0.0265(16) Uani 1 1 d . . . C46 C 0.2948(3) 0.1217(3) 0.07790(16) 0.0307(17) Uani 1 1 d . . . H46 H 0.2593 0.1481 0.0711 0.037 Uiso 1 1 calc R . . C47 C 0.2672(3) 0.0620(3) 0.08712(17) 0.041(2) Uani 1 1 d . . . H47A H 0.2504 0.0433 0.0664 0.061 Uiso 1 1 calc R . . H47B H 0.2330 0.0670 0.1039 0.061 Uiso 1 1 calc R . . H47C H 0.3005 0.0373 0.0970 0.061 Uiso 1 1 calc R . . C48 C 0.3276(4) 0.1479(3) 0.10978(18) 0.049(2) Uani 1 1 d . . . H48A H 0.3595 0.1203 0.1183 0.073 Uiso 1 1 calc R . . H48B H 0.2960 0.1550 0.1277 0.073 Uiso 1 1 calc R . . H48C H 0.3481 0.1848 0.1036 0.073 Uiso 1 1 calc R . . C49 C 0.3532(3) 0.1472(3) -0.04925(17) 0.0338(18) Uani 1 1 d . . . H49 H 0.3158 0.1740 -0.0487 0.041 Uiso 1 1 calc R . . C50 C 0.3368(3) 0.0941(3) -0.07108(18) 0.042(2) Uani 1 1 d . . . H50A H 0.3284 0.1067 -0.0947 0.062 Uiso 1 1 calc R . . H50B H 0.2991 0.0750 -0.0617 0.062 Uiso 1 1 calc R . . H50C H 0.3723 0.0666 -0.0709 0.062 Uiso 1 1 calc R . . C51 C 0.4097(4) 0.1801(4) -0.06426(18) 0.049(2) Uani 1 1 d . . . H51A H 0.4471 0.1549 -0.0638 0.073 Uiso 1 1 calc R . . H51B H 0.4177 0.2154 -0.0506 0.073 Uiso 1 1 calc R . . H51C H 0.4003 0.1913 -0.0880 0.073 Uiso 1 1 calc R . . O52 O 0.1534(2) 0.21065(19) 0.04756(10) 0.0304(11) Uani 1 1 d . . . S53 S 0.11384(9) 0.18357(8) 0.07529(4) 0.0309(4) Uani 1 1 d . . . O54 O 0.0645(2) 0.1478(2) 0.06237(12) 0.0430(13) Uani 1 1 d . . . O55 O 0.1506(2) 0.1636(2) 0.10338(12) 0.0489(15) Uani 1 1 d . . . C56 C 0.0744(4) 0.2494(3) 0.09155(19) 0.041(2) Uani 1 1 d . . . F57 F 0.1155(2) 0.2850(2) 0.10540(11) 0.0593(14) Uani 1 1 d . . . F58 F 0.0458(2) 0.2770(2) 0.06590(12) 0.0662(15) Uani 1 1 d . . . F59 F 0.0307(2) 0.23541(19) 0.11440(12) 0.0588(14) Uani 1 1 d . . . Ti60 Ti 0.55995(5) 0.01249(5) 0.24189(3) 0.0207(3) Uani 1 1 d . . . N61 N 0.5241(2) 0.0883(2) 0.26154(12) 0.0197(12) Uani 1 1 d . . . C62 C 0.5784(3) 0.1154(3) 0.26889(14) 0.0220(15) Uani 1 1 d . . . C63 C 0.6342(3) 0.0809(3) 0.27579(14) 0.0214(15) Uani 1 1 d . . . H63 H 0.6721 0.1016 0.2710 0.026 Uiso 1 1 calc R . . C64 C 0.6460(3) 0.0237(3) 0.28799(15) 0.0192(14) Uiso 1 1 d . . . N65 N 0.5988(2) -0.0158(2) 0.28556(12) 0.0230(13) Uani 1 1 d . . . C66 C 0.4628(3) 0.1158(3) 0.25643(16) 0.0259(16) Uani 1 1 d . . . C67 C 0.4472(3) 0.1365(3) 0.22320(16) 0.0257(16) Uani 1 1 d . . . C68 C 0.3877(3) 0.1613(3) 0.21824(18) 0.0288(17) Uani 1 1 d . . . H68 H 0.3767 0.1757 0.1961 0.035 Uiso 1 1 calc R . . C69 C 0.3449(3) 0.1655(3) 0.2442(2) 0.0338(18) Uani 1 1 d . . . H69 H 0.3046 0.1826 0.2400 0.041 Uiso 1 1 calc R . . C70 C 0.3596(3) 0.1451(3) 0.27660(18) 0.0310(17) Uani 1 1 d . . . H70 H 0.3301 0.1496 0.2948 0.037 Uiso 1 1 calc R . . C71 C 0.4185(3) 0.1177(3) 0.28268(16) 0.0246(16) Uani 1 1 d . . . C72 C 0.4318(3) 0.0926(3) 0.31876(16) 0.0300(17) Uani 1 1 d . . . H72 H 0.4519 0.0533 0.3158 0.036 Uiso 1 1 calc R . . C73 C 0.4777(3) 0.1307(3) 0.33952(17) 0.0365(19) Uani 1 1 d . . . H73A H 0.4625 0.1712 0.3397 0.055 Uiso 1 1 calc R . . H73B H 0.5198 0.1292 0.3290 0.055 Uiso 1 1 calc R . . H73C H 0.4801 0.1160 0.3631 0.055 Uiso 1 1 calc R . . C74 C 0.3716(3) 0.0843(3) 0.34035(18) 0.0384(19) Uani 1 1 d . . . H74A H 0.3819 0.0626 0.3613 0.058 Uiso 1 1 calc R . . H74B H 0.3402 0.0624 0.3270 0.058 Uiso 1 1 calc R . . H74C H 0.3542 0.1227 0.3465 0.058 Uiso 1 1 calc R . . C75 C 0.4917(3) 0.1307(3) 0.19243(16) 0.0356(19) Uani 1 1 d . . . H75 H 0.5345 0.1187 0.2009 0.043 Uiso 1 1 calc R . . C76 C 0.4982(4) 0.1888(4) 0.17242(19) 0.051(2) Uani 1 1 d . . . H76A H 0.5296 0.1842 0.1541 0.076 Uiso 1 1 calc R . . H76B H 0.5118 0.2199 0.1881 0.076 Uiso 1 1 calc R . . H76C H 0.4572 0.1993 0.1623 0.076 Uiso 1 1 calc R . . C77 C 0.4660(4) 0.0824(3) 0.16908(18) 0.046(2) Uani 1 1 d . . . H77A H 0.4639 0.0455 0.1819 0.069 Uiso 1 1 calc R . . H77B H 0.4941 0.0777 0.1493 0.069 Uiso 1 1 calc R . . H77C H 0.4235 0.0931 0.1611 0.069 Uiso 1 1 calc R . . C78 C 0.5928(3) 0.1822(3) 0.27032(17) 0.0319(18) Uani 1 1 d . . . C79 C 0.5352(3) 0.2228(3) 0.26949(19) 0.0351(18) Uani 1 1 d . . . H79A H 0.5488 0.2631 0.2739 0.053 Uiso 1 1 calc R . . H79B H 0.5049 0.2108 0.2872 0.053 Uiso 1 1 calc R . . H79C H 0.5150 0.2205 0.2469 0.053 Uiso 1 1 calc R . . C80 C 0.6336(3) 0.1962(3) 0.23864(19) 0.041(2) Uani 1 1 d . . . H80A H 0.6102 0.1861 0.2178 0.062 Uiso 1 1 calc R . . H80B H 0.6729 0.1735 0.2396 0.062 Uiso 1 1 calc R . . H80C H 0.6438 0.2381 0.2384 0.062 Uiso 1 1 calc R . . C81 C 0.6306(3) 0.1962(3) 0.30316(18) 0.0373(19) Uani 1 1 d . . . H81A H 0.6375 0.2385 0.3047 0.056 Uiso 1 1 calc R . . H81B H 0.6716 0.1761 0.3023 0.056 Uiso 1 1 calc R . . H81C H 0.6068 0.1828 0.3233 0.056 Uiso 1 1 calc R . . C82 C 0.7155(3) 0.0130(3) 0.29971(14) 0.0208(14) Uani 1 1 d . . . C83 C 0.7256(3) -0.0402(3) 0.32334(16) 0.0291(17) Uani 1 1 d . . . H83A H 0.7709 -0.0449 0.3281 0.044 Uiso 1 1 calc R . . H83B H 0.7095 -0.0755 0.3120 0.044 Uiso 1 1 calc R . . H83C H 0.7028 -0.0341 0.3449 0.044 Uiso 1 1 calc R . . C84 C 0.7532(3) 0.0025(3) 0.26617(15) 0.0321(18) Uani 1 1 d . . . H84A H 0.7515 0.0377 0.2519 0.048 Uiso 1 1 calc R . . H84B H 0.7347 -0.0305 0.2536 0.048 Uiso 1 1 calc R . . H84C H 0.7974 -0.0064 0.2718 0.048 Uiso 1 1 calc R . . C85 C 0.7438(3) 0.0659(3) 0.31777(17) 0.0299(17) Uani 1 1 d . . . H85A H 0.7145 0.0796 0.3355 0.045 Uiso 1 1 calc R . . H85B H 0.7509 0.0973 0.3010 0.045 Uiso 1 1 calc R . . H85C H 0.7842 0.0550 0.3284 0.045 Uiso 1 1 calc R . . C86 C 0.5953(3) -0.0696(3) 0.30446(15) 0.0220(15) Uani 1 1 d . . . C87 C 0.5751(3) -0.0671(3) 0.33944(15) 0.0253(16) Uani 1 1 d . . . C88 C 0.5748(3) -0.1178(3) 0.35813(17) 0.0355(19) Uani 1 1 d . . . H88 H 0.5617 -0.1163 0.3814 0.043 Uiso 1 1 calc R . . C89 C 0.5927(4) -0.1706(3) 0.34472(18) 0.041(2) Uani 1 1 d . . . H89 H 0.5937 -0.2047 0.3587 0.049 Uiso 1 1 calc R . . C90 C 0.6093(3) -0.1734(3) 0.31011(18) 0.0347(18) Uani 1 1 d . . . H90 H 0.6196 -0.2102 0.3002 0.042 Uiso 1 1 calc R . . C91 C 0.6110(3) -0.1237(3) 0.28979(17) 0.0280(16) Uani 1 1 d . . . C92 C 0.6289(3) -0.1312(3) 0.25163(17) 0.0286(17) Uani 1 1 d . . . H92 H 0.6257 -0.0922 0.2401 0.034 Uiso 1 1 calc R . . C93 C 0.6970(3) -0.1539(3) 0.2474(2) 0.044(2) Uani 1 1 d . . . H93A H 0.6997 -0.1940 0.2561 0.066 Uiso 1 1 calc R . . H93B H 0.7260 -0.1288 0.2604 0.066 Uiso 1 1 calc R . . H93C H 0.7086 -0.1532 0.2231 0.066 Uiso 1 1 calc R . . C94 C 0.5831(3) -0.1733(3) 0.23392(18) 0.040(2) Uani 1 1 d . . . H94A H 0.5958 -0.1783 0.2099 0.060 Uiso 1 1 calc R . . H94B H 0.5401 -0.1572 0.2349 0.060 Uiso 1 1 calc R . . H94C H 0.5841 -0.2112 0.2456 0.060 Uiso 1 1 calc R . . C95 C 0.5512(3) -0.0108(3) 0.35586(15) 0.0287(16) Uani 1 1 d . . . H95 H 0.5406 0.0171 0.3369 0.034 Uiso 1 1 calc R . . C96 C 0.6008(3) 0.0181(3) 0.37821(18) 0.0382(19) Uani 1 1 d . . . H96A H 0.5830 0.0534 0.3887 0.057 Uiso 1 1 calc R . . H96B H 0.6375 0.0288 0.3641 0.057 Uiso 1 1 calc R . . H96C H 0.6141 -0.0092 0.3962 0.057 Uiso 1 1 calc R . . C97 C 0.4910(3) -0.0208(3) 0.37674(17) 0.042(2) Uani 1 1 d . . . H97A H 0.5011 -0.0439 0.3972 0.063 Uiso 1 1 calc R . . H97B H 0.4600 -0.0419 0.3627 0.063 Uiso 1 1 calc R . . H97C H 0.4733 0.0170 0.3837 0.063 Uiso 1 1 calc R . . N98 N 0.4999(2) -0.0332(2) 0.23032(11) 0.0237(13) Uani 1 1 d . . . C99 C 0.4517(3) -0.0723(3) 0.22008(15) 0.0199(15) Uani 1 1 d . . . C100 C 0.4112(3) -0.0967(3) 0.24496(16) 0.0226(15) Uani 1 1 d . . . C101 C 0.3619(3) -0.1322(3) 0.23477(16) 0.0243(16) Uani 1 1 d . . . H101 H 0.3349 -0.1490 0.2516 0.029 Uiso 1 1 calc R . . C102 C 0.3512(3) -0.1436(3) 0.20018(17) 0.0269(16) Uani 1 1 d . . . H102 H 0.3158 -0.1663 0.1932 0.032 Uiso 1 1 calc R . . C103 C 0.3925(3) -0.1218(3) 0.17639(18) 0.0318(18) Uani 1 1 d . . . H103 H 0.3865 -0.1322 0.1530 0.038 Uiso 1 1 calc R . . C104 C 0.4425(3) -0.0855(3) 0.18469(15) 0.0236(15) Uani 1 1 d . . . C105 C 0.4893(3) -0.0662(3) 0.15719(16) 0.0330(18) Uani 1 1 d . . . H105 H 0.5135 -0.0320 0.1664 0.040 Uiso 1 1 calc R . . C106 C 0.4552(4) -0.0461(4) 0.12406(18) 0.061(3) Uani 1 1 d . . . H10A H 0.4362 -0.0800 0.1127 0.092 Uiso 1 1 calc R . . H10B H 0.4859 -0.0276 0.1086 0.092 Uiso 1 1 calc R . . H10C H 0.4220 -0.0179 0.1299 0.092 Uiso 1 1 calc R . . C107 C 0.5363(4) -0.1136(4) 0.1486(2) 0.067(3) Uani 1 1 d . . . H10D H 0.5632 -0.1212 0.1686 0.101 Uiso 1 1 calc R . . H10E H 0.5627 -0.1009 0.1293 0.101 Uiso 1 1 calc R . . H10F H 0.5136 -0.1494 0.1423 0.101 Uiso 1 1 calc R . . C108 C 0.4206(3) -0.0856(3) 0.28332(15) 0.0260(16) Uani 1 1 d . . . H108 H 0.4592 -0.0608 0.2861 0.031 Uiso 1 1 calc R . . C109 C 0.3648(3) -0.0520(3) 0.29789(16) 0.0368(19) Uani 1 1 d . . . H10G H 0.3264 -0.0758 0.2960 0.055 Uiso 1 1 calc R . . H10H H 0.3591 -0.0155 0.2850 0.055 Uiso 1 1 calc R . . H10I H 0.3728 -0.0429 0.3221 0.055 Uiso 1 1 calc R . . C110 C 0.4318(4) -0.1427(3) 0.30262(17) 0.042(2) Uani 1 1 d . . . H11A H 0.4377 -0.1344 0.3271 0.064 Uiso 1 1 calc R . . H11B H 0.4697 -0.1620 0.2935 0.064 Uiso 1 1 calc R . . H11C H 0.3951 -0.1685 0.2996 0.064 Uiso 1 1 calc R . . O111 O 0.6139(2) 0.0237(2) 0.19990(10) 0.0322(12) Uani 1 1 d . . . S112 S 0.67525(10) 0.02723(12) 0.18176(5) 0.0531(7) Uani 1 1 d . . . O113 O 0.7124(3) 0.0765(3) 0.19255(12) 0.0641(18) Uani 1 1 d . . . O114 O 0.7067(3) -0.0291(3) 0.17773(15) 0.077(2) Uani 1 1 d . . . C115 C 0.6500(4) 0.0447(4) 0.13845(18) 0.053(2) Uani 1 1 d . . . F116 F 0.6094(2) 0.0072(2) 0.12660(10) 0.0584(13) Uani 1 1 d . . . F117 F 0.7012(2) 0.0452(2) 0.11813(11) 0.0724(16) Uani 1 1 d . . . F118 F 0.6229(3) 0.0983(2) 0.13886(13) 0.0714(15) 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 Ti1 0.0273(7) 0.0219(6) 0.0111(5) -0.0008(5) 0.0002(5) -0.0026(6) N2 0.016(3) 0.025(3) 0.013(3) -0.001(2) -0.003(2) -0.002(2) C3 0.027(4) 0.020(4) 0.014(3) 0.007(3) 0.007(3) -0.003(3) C4 0.022(4) 0.027(4) 0.019(3) 0.008(3) 0.003(3) 0.009(3) C5 0.027(4) 0.022(4) 0.017(3) 0.006(3) 0.001(3) 0.006(3) N6 0.025(3) 0.027(3) 0.014(3) 0.000(2) -0.006(2) -0.002(3) C7 0.027(4) 0.015(3) 0.032(4) 0.007(3) 0.004(3) 0.006(3) C8 0.028(4) 0.017(4) 0.024(4) 0.004(3) -0.004(3) -0.001(3) C9 0.022(4) 0.026(4) 0.039(4) 0.005(3) 0.003(3) 0.004(3) C10 0.030(4) 0.024(4) 0.046(5) -0.002(4) -0.011(4) -0.002(3) C11 0.025(4) 0.032(4) 0.031(4) 0.000(3) -0.007(3) -0.001(3) C12 0.028(4) 0.017(3) 0.021(4) -0.001(3) 0.000(3) 0.002(3) C13 0.034(4) 0.038(5) 0.019(4) -0.006(3) -0.007(3) -0.001(4) C14 0.046(5) 0.045(5) 0.037(5) -0.010(4) 0.003(4) -0.009(4) C15 0.048(5) 0.051(5) 0.026(4) -0.003(4) -0.004(3) -0.011(4) C16 0.027(4) 0.028(4) 0.033(4) 0.001(3) 0.001(3) -0.002(3) C17 0.039(5) 0.048(5) 0.037(4) -0.001(4) 0.005(4) 0.000(4) C18 0.055(5) 0.046(5) 0.020(4) 0.006(4) 0.001(4) 0.011(4) C19 0.028(4) 0.026(4) 0.025(4) 0.000(3) 0.001(3) -0.003(3) C20 0.030(4) 0.018(3) 0.038(4) -0.001(3) -0.005(3) 0.004(3) C21 0.041(5) 0.019(4) 0.043(4) 0.009(3) -0.004(4) 0.001(4) C22 0.037(5) 0.027(4) 0.039(4) -0.011(3) 0.003(4) 0.006(4) C23 0.029(4) 0.027(4) 0.037(4) -0.007(3) -0.006(3) 0.006(3) C24 0.061(6) 0.034(5) 0.067(6) -0.014(4) -0.040(5) 0.007(4) C25 0.035(5) 0.037(5) 0.046(5) -0.004(4) -0.022(4) 0.002(4) C26 0.030(4) 0.042(5) 0.056(5) -0.012(4) 0.004(4) -0.002(4) C27 0.028(4) 0.029(4) 0.026(4) -0.009(3) -0.011(3) 0.008(3) C28 0.024(4) 0.031(4) 0.030(4) -0.010(3) -0.012(3) 0.005(3) C29 0.038(5) 0.026(4) 0.042(5) -0.011(4) -0.013(4) 0.005(4) C30 0.054(5) 0.039(5) 0.032(5) -0.026(4) -0.015(4) 0.013(4) C31 0.052(6) 0.051(5) 0.025(4) -0.009(4) -0.009(4) 0.006(4) C32 0.047(5) 0.032(4) 0.019(4) -0.008(3) -0.010(3) 0.005(4) C33 0.049(5) 0.049(5) 0.019(4) -0.012(4) -0.001(4) -0.004(4) C34 0.063(7) 0.071(7) 0.066(6) 0.028(5) 0.011(5) 0.004(5) C35 0.062(7) 0.079(8) 0.134(10) 0.047(7) -0.010(7) 0.005(6) C36 0.043(5) 0.014(4) 0.033(4) -0.003(3) -0.008(3) 0.002(3) C37 0.033(5) 0.035(5) 0.065(6) 0.008(4) -0.004(4) 0.000(4) C38 0.038(5) 0.036(5) 0.042(5) 0.008(4) 0.002(4) -0.005(4) N39 0.024(3) 0.025(3) 0.009(2) -0.001(2) 0.002(2) -0.011(2) C40 0.024(4) 0.020(4) 0.025(4) 0.000(3) -0.004(3) -0.003(3) C41 0.022(4) 0.029(4) 0.026(4) -0.006(3) 0.005(3) -0.005(3) C42 0.025(4) 0.035(4) 0.045(5) -0.006(4) 0.004(4) -0.001(3) C43 0.020(4) 0.036(5) 0.055(5) 0.004(4) -0.006(4) 0.000(4) C44 0.040(5) 0.035(5) 0.035(4) 0.005(4) -0.010(4) -0.006(4) C45 0.024(4) 0.030(4) 0.026(4) -0.002(3) -0.001(3) 0.000(3) C46 0.038(4) 0.035(4) 0.019(4) 0.003(3) -0.001(3) 0.002(4) C47 0.049(5) 0.051(5) 0.022(4) 0.003(4) -0.006(3) -0.003(4) C48 0.065(6) 0.050(5) 0.031(4) 0.001(4) -0.016(4) 0.013(5) C49 0.039(5) 0.037(5) 0.025(4) -0.005(3) 0.009(3) 0.002(4) C50 0.032(5) 0.051(5) 0.042(5) -0.008(4) 0.005(4) -0.003(4) C51 0.058(6) 0.056(6) 0.032(4) -0.007(4) 0.009(4) -0.010(5) O52 0.034(3) 0.036(3) 0.020(2) 0.003(2) 0.008(2) 0.000(2) S53 0.0357(11) 0.0315(10) 0.0254(9) 0.0034(8) 0.0110(8) 0.0013(9) O54 0.041(3) 0.045(3) 0.043(3) 0.001(3) 0.015(3) -0.014(3) O55 0.060(4) 0.061(4) 0.026(3) 0.018(3) -0.001(3) 0.003(3) C56 0.052(6) 0.040(5) 0.031(4) 0.011(4) 0.020(4) 0.003(4) F57 0.072(4) 0.046(3) 0.060(3) -0.027(3) 0.020(3) -0.013(3) F58 0.071(4) 0.064(3) 0.064(3) 0.010(3) 0.017(3) 0.027(3) F59 0.061(3) 0.055(3) 0.060(3) 0.001(2) 0.040(3) 0.001(2) Ti60 0.0279(7) 0.0248(6) 0.0094(5) 0.0010(5) -0.0002(5) -0.0007(6) N61 0.028(3) 0.022(3) 0.010(3) 0.000(2) -0.003(2) 0.006(3) C62 0.031(4) 0.029(4) 0.006(3) 0.005(3) 0.004(3) -0.003(3) C63 0.022(4) 0.029(4) 0.014(3) -0.004(3) -0.003(3) -0.009(3) N65 0.019(3) 0.040(4) 0.011(3) -0.005(2) -0.004(2) -0.007(3) C66 0.035(4) 0.018(3) 0.026(4) -0.006(3) 0.001(3) -0.005(3) C67 0.040(5) 0.016(3) 0.022(4) 0.000(3) -0.003(3) -0.006(3) C68 0.037(4) 0.018(4) 0.032(4) 0.002(3) -0.010(3) 0.005(3) C69 0.026(4) 0.020(4) 0.055(5) 0.001(4) -0.013(4) 0.001(3) C70 0.027(4) 0.029(4) 0.038(4) -0.010(3) 0.002(3) -0.003(3) C71 0.027(4) 0.023(4) 0.024(4) -0.007(3) -0.001(3) -0.004(3) C72 0.034(4) 0.034(4) 0.022(4) -0.007(3) -0.002(3) 0.001(4) C73 0.037(5) 0.047(5) 0.025(4) -0.007(4) -0.001(3) 0.007(4) C74 0.029(4) 0.048(5) 0.038(4) 0.000(4) 0.003(4) 0.001(4) C75 0.036(5) 0.049(5) 0.022(4) 0.005(4) -0.005(3) 0.001(4) C76 0.053(6) 0.060(6) 0.039(5) 0.021(4) -0.005(4) 0.009(5) C77 0.053(5) 0.058(6) 0.028(4) -0.006(4) -0.010(4) 0.019(4) C78 0.033(4) 0.026(4) 0.037(4) 0.007(3) -0.009(3) -0.004(3) C79 0.034(4) 0.019(4) 0.053(5) -0.003(4) -0.007(4) -0.009(3) C80 0.043(5) 0.026(4) 0.055(5) 0.017(4) -0.004(4) -0.002(4) C81 0.045(5) 0.017(4) 0.050(5) -0.007(3) -0.017(4) 0.000(3) C82 0.022(4) 0.023(4) 0.017(3) 0.004(3) 0.003(3) -0.007(3) C83 0.028(4) 0.031(4) 0.029(4) -0.001(3) -0.006(3) -0.005(3) C84 0.026(4) 0.048(5) 0.022(4) 0.003(3) -0.001(3) 0.000(3) C85 0.027(4) 0.033(4) 0.029(4) 0.004(3) -0.010(3) -0.013(3) C86 0.025(4) 0.025(4) 0.017(3) 0.006(3) -0.013(3) -0.006(3) C87 0.031(4) 0.031(4) 0.014(3) 0.007(3) -0.008(3) -0.011(3) C88 0.046(5) 0.045(5) 0.015(4) 0.006(3) -0.015(3) -0.019(4) C89 0.063(6) 0.025(4) 0.034(4) 0.022(4) -0.026(4) -0.018(4) C90 0.049(5) 0.020(4) 0.035(4) -0.002(3) -0.015(4) -0.004(4) C91 0.030(4) 0.025(4) 0.029(4) 0.002(3) -0.010(3) -0.003(3) C92 0.037(4) 0.016(4) 0.033(4) -0.004(3) -0.006(3) -0.002(3) C93 0.043(5) 0.035(4) 0.053(5) -0.015(4) -0.005(4) 0.002(4) C94 0.040(5) 0.036(5) 0.044(5) -0.006(4) -0.007(4) 0.004(4) C95 0.032(4) 0.042(4) 0.012(3) 0.011(3) -0.005(3) -0.007(4) C96 0.036(5) 0.037(5) 0.041(4) -0.007(4) -0.005(4) -0.003(4) C97 0.049(5) 0.052(5) 0.026(4) -0.001(4) 0.006(4) -0.009(4) N98 0.029(3) 0.035(4) 0.007(3) 0.007(2) 0.001(2) 0.005(3) C99 0.029(4) 0.017(3) 0.014(3) 0.000(3) -0.002(3) 0.002(3) C100 0.031(4) 0.013(3) 0.024(4) 0.001(3) -0.002(3) 0.003(3) C101 0.023(4) 0.018(4) 0.032(4) 0.004(3) -0.001(3) -0.001(3) C102 0.032(4) 0.021(4) 0.028(4) -0.007(3) -0.010(3) 0.003(3) C103 0.040(5) 0.032(4) 0.024(4) -0.013(3) -0.011(3) 0.009(4) C104 0.033(4) 0.019(4) 0.018(3) -0.003(3) -0.002(3) 0.006(3) C105 0.043(5) 0.041(5) 0.016(4) -0.003(3) -0.003(3) -0.005(4) C106 0.088(7) 0.073(7) 0.023(4) 0.009(4) -0.015(4) -0.031(6) C107 0.092(8) 0.062(6) 0.049(6) -0.006(5) 0.043(5) 0.006(6) C108 0.034(4) 0.026(4) 0.017(3) 0.005(3) 0.002(3) -0.007(3) C109 0.039(5) 0.055(5) 0.016(4) -0.003(3) 0.002(3) 0.003(4) C110 0.052(5) 0.051(5) 0.025(4) 0.002(4) -0.010(4) -0.005(4) O111 0.030(3) 0.050(3) 0.017(2) 0.002(2) 0.002(2) -0.003(2) S112 0.0406(13) 0.098(2) 0.0207(10) 0.0069(12) 0.0039(9) -0.0092(14) O113 0.063(4) 0.105(5) 0.024(3) 0.017(3) -0.006(3) -0.044(4) O114 0.074(4) 0.100(5) 0.057(4) 0.018(4) 0.019(3) 0.058(4) C115 0.066(6) 0.077(7) 0.016(4) 0.004(4) 0.009(4) -0.027(6) F116 0.086(4) 0.065(3) 0.024(2) -0.007(2) 0.003(2) -0.020(3) F117 0.067(3) 0.119(5) 0.032(3) 0.012(3) 0.024(2) -0.004(3) F118 0.094(4) 0.049(3) 0.071(4) 0.015(3) -0.004(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 N39 1.708(5) . ? Ti1 O52 1.982(4) . ? Ti1 N6 1.999(5) . ? Ti1 N2 2.046(5) . ? Ti1 C5 2.647(6) . ? Ti1 C3 2.712(6) . ? N2 C3 1.334(7) . ? N2 C7 1.442(8) . ? C3 C4 1.414(8) . ? C3 C19 1.580(9) . ? C4 C5 1.439(9) . ? C5 N6 1.328(8) . ? C5 C23 1.561(9) . ? N6 C27 1.447(8) . ? C7 C8 1.410(8) . ? C7 C12 1.420(8) . ? C8 C9 1.389(9) . ? C8 C16 1.543(9) . ? C9 C10 1.383(9) . ? C10 C11 1.372(9) . ? C11 C12 1.372(9) . ? C12 C13 1.519(9) . ? C13 C14 1.527(9) . ? C13 C15 1.540(9) . ? C16 C18 1.517(9) . ? C16 C17 1.523(9) . ? C19 C20 1.521(9) . ? C19 C22 1.539(9) . ? C19 C21 1.552(9) . ? C23 C24 1.522(9) . ? C23 C25 1.526(9) . ? C23 C26 1.573(9) . ? C27 C28 1.402(9) . ? C27 C32 1.427(9) . ? C28 C29 1.381(9) . ? C28 C36 1.538(9) . ? C29 C30 1.393(10) . ? C30 C31 1.361(10) . ? C31 C32 1.375(9) . ? C32 C33 1.529(10) . ? C33 C34 1.498(10) . ? C33 C35 1.502(11) . ? C36 C37 1.515(9) . ? C36 C38 1.517(9) . ? N39 C40 1.424(8) . ? C40 C41 1.406(8) . ? C40 C45 1.431(8) . ? C41 C42 1.390(9) . ? C41 C49 1.522(9) . ? C42 C43 1.371(9) . ? C43 C44 1.373(10) . ? C44 C45 1.388(9) . ? C45 C46 1.518(9) . ? C46 C47 1.527(9) . ? C46 C48 1.543(9) . ? C49 C50 1.521(9) . ? C49 C51 1.527(9) . ? O52 S53 1.500(4) . ? S53 O54 1.417(5) . ? S53 O55 1.418(5) . ? S53 C56 1.834(8) . ? C56 F57 1.306(9) . ? C56 F59 1.321(8) . ? C56 F58 1.327(8) . ? Ti60 N98 1.704(6) . ? Ti60 N65 1.997(5) . ? Ti60 O111 2.010(4) . ? Ti60 N61 2.040(5) . ? Ti60 C64 2.568(6) . ? Ti60 C63 2.578(6) . ? Ti60 C62 2.605(7) . ? N61 C62 1.335(8) . ? N61 C66 1.453(8) . ? C62 C63 1.443(9) . ? C62 C78 1.558(9) . ? C63 C64 1.413(8) . ? C64 N65 1.348(7) . ? C64 C82 1.558(8) . ? N65 C86 1.434(8) . ? C66 C71 1.387(9) . ? C66 C67 1.417(9) . ? C67 C68 1.393(9) . ? C67 C75 1.529(9) . ? C68 C69 1.360(9) . ? C69 C70 1.381(9) . ? C70 C71 1.413(9) . ? C71 C72 1.544(9) . ? C72 C73 1.533(9) . ? C72 C74 1.538(9) . ? C75 C77 1.529(10) . ? C75 C76 1.547(10) . ? C78 C79 1.531(9) . ? C78 C80 1.540(9) . ? C78 C81 1.541(9) . ? C82 C85 1.522(8) . ? C82 C83 1.539(8) . ? C82 C84 1.549(8) . ? C86 C91 1.402(9) . ? C86 C87 1.429(8) . ? C87 C88 1.369(9) . ? C87 C95 1.523(9) . ? C88 C89 1.368(10) . ? C89 C90 1.395(9) . ? C90 C91 1.386(9) . ? C91 C92 1.543(9) . ? C92 C94 1.528(9) . ? C92 C93 1.538(9) . ? C95 C96 1.514(9) . ? C95 C97 1.528(9) . ? N98 C99 1.412(8) . ? C99 C100 1.408(8) . ? C99 C104 1.425(8) . ? C100 C101 1.378(8) . ? C100 C108 1.529(8) . ? C101 C102 1.391(8) . ? C102 C103 1.367(9) . ? C103 C104 1.382(9) . ? C104 C105 1.524(9) . ? C105 C107 1.506(10) . ? C105 C106 1.548(9) . ? C108 C109 1.517(9) . ? C108 C110 1.525(9) . ? O111 S112 1.479(5) . ? S112 O113 1.436(6) . ? S112 O114 1.457(6) . ? S112 C115 1.814(8) . ? C115 F116 1.297(9) . ? C115 F117 1.341(9) . ? C115 F118 1.353(10) . ? 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 N39 Ti1 O52 110.1(2) . . ? N39 Ti1 N6 111.6(2) . . ? O52 Ti1 N6 113.3(2) . . ? N39 Ti1 N2 112.3(2) . . ? O52 Ti1 N2 112.32(19) . . ? N6 Ti1 N2 96.7(2) . . ? N39 Ti1 C5 140.8(2) . . ? O52 Ti1 C5 95.50(19) . . ? N6 Ti1 C5 29.21(19) . . ? N2 Ti1 C5 82.64(19) . . ? N39 Ti1 C3 140.4(2) . . ? O52 Ti1 C3 97.47(18) . . ? N6 Ti1 C3 80.8(2) . . ? N2 Ti1 C3 28.41(18) . . ? C5 Ti1 C3 58.74(19) . . ? C3 N2 C7 124.6(5) . . ? C3 N2 Ti1 104.7(4) . . ? C7 N2 Ti1 127.3(4) . . ? N2 C3 C4 120.4(6) . . ? N2 C3 C19 128.2(6) . . ? C4 C3 C19 111.3(5) . . ? N2 C3 Ti1 46.9(3) . . ? C4 C3 Ti1 76.0(4) . . ? C19 C3 Ti1 159.9(4) . . ? C3 C4 C5 134.2(6) . . ? N6 C5 C4 119.4(6) . . ? N6 C5 C23 128.5(6) . . ? C4 C5 C23 111.9(5) . . ? N6 C5 Ti1 47.3(3) . . ? C4 C5 Ti1 78.1(4) . . ? C23 C5 Ti1 151.5(4) . . ? C5 N6 C27 124.8(5) . . ? C5 N6 Ti1 103.5(4) . . ? C27 N6 Ti1 128.8(4) . . ? C8 C7 C12 120.3(6) . . ? C8 C7 N2 120.2(6) . . ? C12 C7 N2 119.5(6) . . ? C9 C8 C7 118.3(6) . . ? C9 C8 C16 120.2(6) . . ? C7 C8 C16 121.4(6) . . ? C10 C9 C8 120.6(6) . . ? C11 C10 C9 120.8(7) . . ? C10 C11 C12 121.0(6) . . ? C11 C12 C7 118.7(6) . . ? C11 C12 C13 119.1(6) . . ? C7 C12 C13 122.2(6) . . ? C12 C13 C14 113.3(6) . . ? C12 C13 C15 107.6(6) . . ? C14 C13 C15 110.9(6) . . ? C18 C16 C17 109.6(6) . . ? C18 C16 C8 112.4(5) . . ? C17 C16 C8 112.6(5) . . ? C20 C19 C22 108.7(5) . . ? C20 C19 C21 105.2(5) . . ? C22 C19 C21 108.6(6) . . ? C20 C19 C3 116.7(5) . . ? C22 C19 C3 108.4(5) . . ? C21 C19 C3 109.0(5) . . ? C24 C23 C25 106.1(6) . . ? C24 C23 C5 112.4(6) . . ? C25 C23 C5 117.0(5) . . ? C24 C23 C26 108.7(6) . . ? C25 C23 C26 106.3(6) . . ? C5 C23 C26 106.0(5) . . ? C28 C27 C32 120.4(6) . . ? C28 C27 N6 120.6(6) . . ? C32 C27 N6 119.0(6) . . ? C29 C28 C27 118.2(7) . . ? C29 C28 C36 118.8(6) . . ? C27 C28 C36 123.0(6) . . ? C28 C29 C30 121.7(7) . . ? C31 C30 C29 119.1(7) . . ? C30 C31 C32 122.4(7) . . ? C31 C32 C27 118.0(7) . . ? C31 C32 C33 119.8(6) . . ? C27 C32 C33 122.2(6) . . ? C34 C33 C35 109.8(7) . . ? C34 C33 C32 112.6(7) . . ? C35 C33 C32 112.7(7) . . ? C37 C36 C38 110.5(6) . . ? C37 C36 C28 112.5(6) . . ? C38 C36 C28 111.7(6) . . ? C40 N39 Ti1 176.0(4) . . ? C41 C40 N39 121.1(6) . . ? C41 C40 C45 118.9(6) . . ? N39 C40 C45 120.0(6) . . ? C42 C41 C40 119.4(6) . . ? C42 C41 C49 119.0(6) . . ? C40 C41 C49 121.5(6) . . ? C43 C42 C41 122.2(7) . . ? C42 C43 C44 118.3(7) . . ? C43 C44 C45 123.1(7) . . ? C44 C45 C40 118.0(6) . . ? C44 C45 C46 118.8(6) . . ? C40 C45 C46 123.1(6) . . ? C45 C46 C47 110.0(6) . . ? C45 C46 C48 112.2(6) . . ? C47 C46 C48 109.2(6) . . ? C50 C49 C41 109.7(6) . . ? C50 C49 C51 110.9(6) . . ? C41 C49 C51 109.9(6) . . ? S53 O52 Ti1 162.6(3) . . ? O54 S53 O55 119.5(3) . . ? O54 S53 O52 113.1(3) . . ? O55 S53 O52 112.5(3) . . ? O54 S53 C56 105.2(4) . . ? O55 S53 C56 104.3(4) . . ? O52 S53 C56 99.4(3) . . ? F57 C56 F59 109.7(6) . . ? F57 C56 F58 108.6(7) . . ? F59 C56 F58 107.7(7) . . ? F57 C56 S53 110.6(6) . . ? F59 C56 S53 110.5(5) . . ? F58 C56 S53 109.6(5) . . ? N98 Ti60 N65 109.4(2) . . ? N98 Ti60 O111 106.5(2) . . ? N65 Ti60 O111 120.15(19) . . ? N98 Ti60 N61 110.1(2) . . ? N65 Ti60 N61 96.2(2) . . ? O111 Ti60 N61 114.1(2) . . ? N98 Ti60 C64 140.6(2) . . ? N65 Ti60 C64 31.30(19) . . ? O111 Ti60 C64 98.97(19) . . ? N61 Ti60 C64 85.2(2) . . ? N98 Ti60 C63 163.7(2) . . ? N65 Ti60 C63 60.7(2) . . ? O111 Ti60 C63 89.72(19) . . ? N61 Ti60 C63 61.2(2) . . ? C64 Ti60 C63 31.87(18) . . ? N98 Ti60 C62 140.5(2) . . ? N65 Ti60 C62 83.5(2) . . ? O111 Ti60 C62 97.40(19) . . ? N61 Ti60 C62 30.42(19) . . ? C64 Ti60 C62 61.4(2) . . ? C63 Ti60 C62 32.32(19) . . ? C62 N61 C66 126.4(5) . . ? C62 N61 Ti60 98.9(4) . . ? C66 N61 Ti60 130.4(4) . . ? N61 C62 C63 119.2(6) . . ? N61 C62 C78 129.0(6) . . ? C63 C62 C78 111.7(6) . . ? N61 C62 Ti60 50.7(3) . . ? C63 C62 Ti60 72.8(4) . . ? C78 C62 Ti60 158.2(4) . . ? C64 C63 C62 135.4(6) . . ? C64 C63 Ti60 73.7(3) . . ? C62 C63 Ti60 74.9(4) . . ? N65 C64 C63 117.8(6) . . ? N65 C64 C82 127.7(5) . . ? C63 C64 C82 114.2(5) . . ? N65 C64 Ti60 50.3(3) . . ? C63 C64 Ti60 74.5(3) . . ? C82 C64 Ti60 148.9(4) . . ? C64 N65 C86 125.2(5) . . ? C64 N65 Ti60 98.4(4) . . ? C86 N65 Ti60 134.0(4) . . ? C71 C66 C67 120.4(6) . . ? C71 C66 N61 120.9(6) . . ? C67 C66 N61 118.5(6) . . ? C68 C67 C66 118.2(6) . . ? C68 C67 C75 118.8(6) . . ? C66 C67 C75 123.0(6) . . ? C69 C68 C67 121.7(6) . . ? C68 C69 C70 120.4(7) . . ? C69 C70 C71 120.1(7) . . ? C66 C71 C70 119.0(6) . . ? C66 C71 C72 122.4(6) . . ? C70 C71 C72 118.6(6) . . ? C73 C72 C74 107.7(5) . . ? C73 C72 C71 112.7(6) . . ? C74 C72 C71 113.1(6) . . ? C77 C75 C67 108.1(6) . . ? C77 C75 C76 110.6(6) . . ? C67 C75 C76 112.0(6) . . ? C79 C78 C80 107.6(6) . . ? C79 C78 C81 107.7(6) . . ? C80 C78 C81 109.4(6) . . ? C79 C78 C62 116.0(6) . . ? C80 C78 C62 106.6(5) . . ? C81 C78 C62 109.5(5) . . ? C85 C82 C83 107.3(5) . . ? C85 C82 C84 108.1(5) . . ? C83 C82 C84 108.1(5) . . ? C85 C82 C64 112.3(5) . . ? C83 C82 C64 115.5(5) . . ? C84 C82 C64 105.2(5) . . ? C91 C86 C87 119.6(6) . . ? C91 C86 N65 122.2(6) . . ? C87 C86 N65 118.1(6) . . ? C88 C87 C86 118.4(6) . . ? C88 C87 C95 119.4(6) . . ? C86 C87 C95 122.2(5) . . ? C89 C88 C87 122.9(7) . . ? C88 C89 C90 118.6(6) . . ? C91 C90 C89 121.5(7) . . ? C90 C91 C86 118.9(6) . . ? C90 C91 C92 117.8(6) . . ? C86 C91 C92 123.3(6) . . ? C94 C92 C93 109.4(5) . . ? C94 C92 C91 110.5(6) . . ? C93 C92 C91 111.6(6) . . ? C96 C95 C87 112.4(6) . . ? C96 C95 C97 109.6(5) . . ? C87 C95 C97 111.9(6) . . ? C99 N98 Ti60 178.0(5) . . ? C100 C99 N98 119.6(5) . . ? C100 C99 C104 120.0(6) . . ? N98 C99 C104 120.4(5) . . ? C101 C100 C99 119.6(6) . . ? C101 C100 C108 118.5(6) . . ? C99 C100 C108 121.9(6) . . ? C100 C101 C102 120.8(6) . . ? C103 C102 C101 119.0(6) . . ? C102 C103 C104 123.2(6) . . ? C103 C104 C99 117.3(6) . . ? C103 C104 C105 120.4(6) . . ? C99 C104 C105 122.0(6) . . ? C107 C105 C104 112.0(6) . . ? C107 C105 C106 109.6(6) . . ? C104 C105 C106 111.7(6) . . ? C109 C108 C110 111.7(6) . . ? C109 C108 C100 110.5(5) . . ? C110 C108 C100 111.1(5) . . ? S112 O111 Ti60 153.2(3) . . ? O113 S112 O114 118.4(4) . . ? O113 S112 O111 112.4(3) . . ? O114 S112 O111 113.8(4) . . ? O113 S112 C115 105.1(4) . . ? O114 S112 C115 103.2(4) . . ? O111 S112 C115 101.5(3) . . ? F116 C115 F117 109.2(7) . . ? F116 C115 F118 108.9(8) . . ? F117 C115 F118 109.9(7) . . ? F116 C115 S112 112.3(6) . . ? F117 C115 S112 108.3(6) . . ? F118 C115 S112 108.2(6) . . ? 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 N39 Ti1 N2 C3 172.9(4) . . . . ? O52 Ti1 N2 C3 -62.4(4) . . . . ? N6 Ti1 N2 C3 56.2(4) . . . . ? C5 Ti1 N2 C3 30.6(4) . . . . ? N39 Ti1 N2 C7 -27.4(5) . . . . ? O52 Ti1 N2 C7 97.3(5) . . . . ? N6 Ti1 N2 C7 -144.0(5) . . . . ? C5 Ti1 N2 C7 -169.7(5) . . . . ? C3 Ti1 N2 C7 159.7(7) . . . . ? C7 N2 C3 C4 178.4(5) . . . . ? Ti1 N2 C3 C4 -21.2(6) . . . . ? C7 N2 C3 C19 -6.2(9) . . . . ? Ti1 N2 C3 C19 154.2(5) . . . . ? C7 N2 C3 Ti1 -160.4(7) . . . . ? N39 Ti1 C3 N2 -10.4(5) . . . . ? O52 Ti1 C3 N2 124.2(4) . . . . ? N6 Ti1 C3 N2 -123.2(4) . . . . ? C5 Ti1 C3 N2 -143.9(4) . . . . ? N39 Ti1 C3 C4 150.9(4) . . . . ? O52 Ti1 C3 C4 -74.5(4) . . . . ? N6 Ti1 C3 C4 38.0(4) . . . . ? N2 Ti1 C3 C4 161.3(6) . . . . ? C5 Ti1 C3 C4 17.4(3) . . . . ? N39 Ti1 C3 C19 -94.9(12) . . . . ? O52 Ti1 C3 C19 39.7(12) . . . . ? N6 Ti1 C3 C19 152.2(12) . . . . ? N2 Ti1 C3 C19 -84.6(13) . . . . ? C5 Ti1 C3 C19 131.6(13) . . . . ? N2 C3 C4 C5 -25.3(10) . . . . ? C19 C3 C4 C5 158.6(6) . . . . ? Ti1 C3 C4 C5 -41.0(7) . . . . ? C3 C4 C5 N6 18.1(10) . . . . ? C3 C4 C5 C23 -166.1(6) . . . . ? C3 C4 C5 Ti1 41.8(7) . . . . ? N39 Ti1 C5 N6 1.6(6) . . . . ? O52 Ti1 C5 N6 -130.0(4) . . . . ? N2 Ti1 C5 N6 118.1(4) . . . . ? C3 Ti1 C5 N6 134.6(5) . . . . ? N39 Ti1 C5 C4 -149.9(4) . . . . ? O52 Ti1 C5 C4 78.5(4) . . . . ? N6 Ti1 C5 C4 -151.5(6) . . . . ? N2 Ti1 C5 C4 -33.4(4) . . . . ? C3 Ti1 C5 C4 -17.0(3) . . . . ? N39 Ti1 C5 C23 95.8(9) . . . . ? O52 Ti1 C5 C23 -35.8(9) . . . . ? N6 Ti1 C5 C23 94.2(10) . . . . ? N2 Ti1 C5 C23 -147.6(9) . . . . ? C3 Ti1 C5 C23 -131.2(10) . . . . ? C4 C5 N6 C27 -165.2(6) . . . . ? C23 C5 N6 C27 19.8(10) . . . . ? Ti1 C5 N6 C27 162.4(7) . . . . ? C4 C5 N6 Ti1 32.4(6) . . . . ? C23 C5 N6 Ti1 -142.6(6) . . . . ? N39 Ti1 N6 C5 -178.9(4) . . . . ? O52 Ti1 N6 C5 56.1(4) . . . . ? N2 Ti1 N6 C5 -61.7(4) . . . . ? C3 Ti1 N6 C5 -38.1(4) . . . . ? N39 Ti1 N6 C27 19.7(6) . . . . ? O52 Ti1 N6 C27 -105.2(5) . . . . ? N2 Ti1 N6 C27 136.9(5) . . . . ? C5 Ti1 N6 C27 -161.4(8) . . . . ? C3 Ti1 N6 C27 160.5(6) . . . . ? C3 N2 C7 C8 -98.9(7) . . . . ? Ti1 N2 C7 C8 105.1(6) . . . . ? C3 N2 C7 C12 82.3(7) . . . . ? Ti1 N2 C7 C12 -73.7(7) . . . . ? C12 C7 C8 C9 -6.1(9) . . . . ? N2 C7 C8 C9 175.1(6) . . . . ? C12 C7 C8 C16 175.5(6) . . . . ? N2 C7 C8 C16 -3.3(9) . . . . ? C7 C8 C9 C10 2.9(9) . . . . ? C16 C8 C9 C10 -178.6(6) . . . . ? C8 C9 C10 C11 0.9(10) . . . . ? C9 C10 C11 C12 -1.6(10) . . . . ? C10 C11 C12 C7 -1.6(10) . . . . ? C10 C11 C12 C13 177.9(6) . . . . ? C8 C7 C12 C11 5.4(9) . . . . ? N2 C7 C12 C11 -175.8(6) . . . . ? C8 C7 C12 C13 -174.0(6) . . . . ? N2 C7 C12 C13 4.8(9) . . . . ? C11 C12 C13 C14 39.7(9) . . . . ? C7 C12 C13 C14 -140.8(6) . . . . ? C11 C12 C13 C15 -83.3(7) . . . . ? C7 C12 C13 C15 96.2(7) . . . . ? C9 C8 C16 C18 -103.2(7) . . . . ? C7 C8 C16 C18 75.2(8) . . . . ? C9 C8 C16 C17 21.2(9) . . . . ? C7 C8 C16 C17 -160.4(6) . . . . ? N2 C3 C19 C20 14.3(9) . . . . ? C4 C3 C19 C20 -169.9(5) . . . . ? Ti1 C3 C19 C20 81.9(13) . . . . ? N2 C3 C19 C22 -108.7(7) . . . . ? C4 C3 C19 C22 67.0(7) . . . . ? Ti1 C3 C19 C22 -41.1(14) . . . . ? N2 C3 C19 C21 133.2(6) . . . . ? C4 C3 C19 C21 -51.0(7) . . . . ? Ti1 C3 C19 C21 -159.2(10) . . . . ? N6 C5 C23 C24 -139.2(7) . . . . ? C4 C5 C23 C24 45.5(8) . . . . ? Ti1 C5 C23 C24 151.4(8) . . . . ? N6 C5 C23 C25 -16.1(10) . . . . ? C4 C5 C23 C25 168.6(6) . . . . ? Ti1 C5 C23 C25 -85.4(11) . . . . ? N6 C5 C23 C26 102.1(7) . . . . ? C4 C5 C23 C26 -73.1(7) . . . . ? Ti1 C5 C23 C26 32.8(11) . . . . ? C5 N6 C27 C28 -97.7(8) . . . . ? Ti1 N6 C27 C28 60.1(8) . . . . ? C5 N6 C27 C32 84.7(8) . . . . ? Ti1 N6 C27 C32 -117.5(6) . . . . ? C32 C27 C28 C29 0.0(10) . . . . ? N6 C27 C28 C29 -177.6(6) . . . . ? C32 C27 C28 C36 -179.9(6) . . . . ? N6 C27 C28 C36 2.5(10) . . . . ? C27 C28 C29 C30 -2.7(10) . . . . ? C36 C28 C29 C30 177.2(6) . . . . ? C28 C29 C30 C31 2.9(11) . . . . ? C29 C30 C31 C32 -0.4(12) . . . . ? C30 C31 C32 C27 -2.2(11) . . . . ? C30 C31 C32 C33 178.5(7) . . . . ? C28 C27 C32 C31 2.4(10) . . . . ? N6 C27 C32 C31 -180.0(6) . . . . ? C28 C27 C32 C33 -178.4(6) . . . . ? N6 C27 C32 C33 -0.7(10) . . . . ? C31 C32 C33 C34 -47.6(9) . . . . ? C27 C32 C33 C34 133.1(7) . . . . ? C31 C32 C33 C35 77.3(9) . . . . ? C27 C32 C33 C35 -101.9(8) . . . . ? C29 C28 C36 C37 -55.0(8) . . . . ? C27 C28 C36 C37 124.9(7) . . . . ? C29 C28 C36 C38 70.0(8) . . . . ? C27 C28 C36 C38 -110.2(7) . . . . ? O52 Ti1 N39 C40 24(7) . . . . ? N6 Ti1 N39 C40 -102(7) . . . . ? N2 Ti1 N39 C40 150(7) . . . . ? C5 Ti1 N39 C40 -103(7) . . . . ? C3 Ti1 N39 C40 156(6) . . . . ? Ti1 N39 C40 C41 142(6) . . . . ? Ti1 N39 C40 C45 -38(7) . . . . ? N39 C40 C41 C42 177.5(6) . . . . ? C45 C40 C41 C42 -2.3(9) . . . . ? N39 C40 C41 C49 -7.5(9) . . . . ? C45 C40 C41 C49 172.7(6) . . . . ? C40 C41 C42 C43 -1.2(10) . . . . ? C49 C41 C42 C43 -176.3(6) . . . . ? C41 C42 C43 C44 2.8(11) . . . . ? C42 C43 C44 C45 -1.0(11) . . . . ? C43 C44 C45 C40 -2.4(10) . . . . ? C43 C44 C45 C46 174.6(6) . . . . ? C41 C40 C45 C44 4.0(9) . . . . ? N39 C40 C45 C44 -175.8(6) . . . . ? C41 C40 C45 C46 -172.9(6) . . . . ? N39 C40 C45 C46 7.3(9) . . . . ? C44 C45 C46 C47 -63.5(8) . . . . ? C40 C45 C46 C47 113.5(7) . . . . ? C44 C45 C46 C48 58.3(8) . . . . ? C40 C45 C46 C48 -124.8(7) . . . . ? C42 C41 C49 C50 64.5(8) . . . . ? C40 C41 C49 C50 -110.5(7) . . . . ? C42 C41 C49 C51 -57.7(8) . . . . ? C40 C41 C49 C51 127.3(7) . . . . ? N39 Ti1 O52 S53 -54.7(10) . . . . ? N6 Ti1 O52 S53 71.1(10) . . . . ? N2 Ti1 O52 S53 179(100) . . . . ? C5 Ti1 O52 S53 95.1(10) . . . . ? C3 Ti1 O52 S53 154.2(10) . . . . ? Ti1 O52 S53 O54 -54.4(11) . . . . ? Ti1 O52 S53 O55 84.7(10) . . . . ? Ti1 O52 S53 C56 -165.4(10) . . . . ? O54 S53 C56 F57 177.6(5) . . . . ? O55 S53 C56 F57 51.1(6) . . . . ? O52 S53 C56 F57 -65.2(5) . . . . ? O54 S53 C56 F59 56.0(6) . . . . ? O55 S53 C56 F59 -70.6(6) . . . . ? O52 S53 C56 F59 173.1(6) . . . . ? O54 S53 C56 F58 -62.6(6) . . . . ? O55 S53 C56 F58 170.8(5) . . . . ? O52 S53 C56 F58 54.5(6) . . . . ? N98 Ti60 N61 C62 179.1(3) . . . . ? N65 Ti60 N61 C62 65.8(4) . . . . ? O111 Ti60 N61 C62 -61.2(4) . . . . ? C64 Ti60 N61 C62 36.5(4) . . . . ? C63 Ti60 N61 C62 14.3(3) . . . . ? N98 Ti60 N61 C66 -23.6(6) . . . . ? N65 Ti60 N61 C66 -136.9(5) . . . . ? O111 Ti60 N61 C66 96.1(5) . . . . ? C64 Ti60 N61 C66 -166.2(5) . . . . ? C63 Ti60 N61 C66 171.5(6) . . . . ? C62 Ti60 N61 C66 157.3(7) . . . . ? C66 N61 C62 C63 175.2(5) . . . . ? Ti60 N61 C62 C63 -26.2(6) . . . . ? C66 N61 C62 C78 -6.8(10) . . . . ? Ti60 N61 C62 C78 151.7(5) . . . . ? C66 N61 C62 Ti60 -158.6(7) . . . . ? N98 Ti60 C62 N61 -1.3(5) . . . . ? N65 Ti60 C62 N61 -114.1(4) . . . . ? O111 Ti60 C62 N61 126.2(4) . . . . ? C64 Ti60 C62 N61 -137.6(4) . . . . ? C63 Ti60 C62 N61 -156.2(5) . . . . ? N98 Ti60 C62 C63 154.9(4) . . . . ? N65 Ti60 C62 C63 42.0(3) . . . . ? O111 Ti60 C62 C63 -77.6(3) . . . . ? N61 Ti60 C62 C63 156.2(5) . . . . ? C64 Ti60 C62 C63 18.6(3) . . . . ? N98 Ti60 C62 C78 -99.6(12) . . . . ? N65 Ti60 C62 C78 147.5(12) . . . . ? O111 Ti60 C62 C78 27.9(12) . . . . ? N61 Ti60 C62 C78 -98.3(13) . . . . ? C64 Ti60 C62 C78 124.1(13) . . . . ? C63 Ti60 C62 C78 105.5(13) . . . . ? N61 C62 C63 C64 -25.5(10) . . . . ? C78 C62 C63 C64 156.2(7) . . . . ? Ti60 C62 C63 C64 -46.5(7) . . . . ? N61 C62 C63 Ti60 21.0(5) . . . . ? C78 C62 C63 Ti60 -157.3(5) . . . . ? N98 Ti60 C63 C64 73.2(9) . . . . ? N65 Ti60 C63 C64 17.7(3) . . . . ? O111 Ti60 C63 C64 -107.6(4) . . . . ? N61 Ti60 C63 C64 134.5(4) . . . . ? C62 Ti60 C63 C64 148.0(5) . . . . ? N98 Ti60 C63 C62 -74.7(9) . . . . ? N65 Ti60 C63 C62 -130.2(4) . . . . ? O111 Ti60 C63 C62 104.4(3) . . . . ? N61 Ti60 C63 C62 -13.5(3) . . . . ? C64 Ti60 C63 C62 -148.0(5) . . . . ? C62 C63 C64 N65 20.5(10) . . . . ? Ti60 C63 C64 N65 -26.4(5) . . . . ? C62 C63 C64 C82 -165.0(6) . . . . ? Ti60 C63 C64 C82 148.2(5) . . . . ? C62 C63 C64 Ti60 46.8(7) . . . . ? N98 Ti60 C64 N65 -5.8(6) . . . . ? O111 Ti60 C64 N65 -136.0(4) . . . . ? N61 Ti60 C64 N65 110.4(4) . . . . ? C63 Ti60 C64 N65 149.3(6) . . . . ? C62 Ti60 C64 N65 130.4(4) . . . . ? N98 Ti60 C64 C63 -155.0(4) . . . . ? N65 Ti60 C64 C63 -149.3(6) . . . . ? O111 Ti60 C64 C63 74.7(4) . . . . ? N61 Ti60 C64 C63 -38.9(4) . . . . ? C62 Ti60 C64 C63 -18.8(3) . . . . ? N98 Ti60 C64 C82 93.6(8) . . . . ? N65 Ti60 C64 C82 99.4(9) . . . . ? O111 Ti60 C64 C82 -36.6(8) . . . . ? N61 Ti60 C64 C82 -150.2(8) . . . . ? C63 Ti60 C64 C82 -111.3(9) . . . . ? C62 Ti60 C64 C82 -130.2(8) . . . . ? C63 C64 N65 C86 -161.9(6) . . . . ? C82 C64 N65 C86 24.3(9) . . . . ? Ti60 C64 N65 C86 164.3(7) . . . . ? C63 C64 N65 Ti60 33.8(6) . . . . ? C82 C64 N65 Ti60 -139.9(5) . . . . ? N98 Ti60 N65 C64 176.1(4) . . . . ? O111 Ti60 N65 C64 52.5(4) . . . . ? N61 Ti60 N65 C64 -70.0(4) . . . . ? C63 Ti60 N65 C64 -18.0(3) . . . . ? C62 Ti60 N65 C64 -42.3(4) . . . . ? N98 Ti60 N65 C86 14.1(6) . . . . ? O111 Ti60 N65 C86 -109.5(6) . . . . ? N61 Ti60 N65 C86 128.0(6) . . . . ? C64 Ti60 N65 C86 -162.0(8) . . . . ? C63 Ti60 N65 C86 179.9(6) . . . . ? C62 Ti60 N65 C86 155.7(6) . . . . ? C62 N61 C66 C71 -98.6(7) . . . . ? Ti60 N61 C66 C71 109.7(6) . . . . ? C62 N61 C66 C67 86.6(7) . . . . ? Ti60 N61 C66 C67 -65.1(7) . . . . ? C71 C66 C67 C68 3.3(9) . . . . ? N61 C66 C67 C68 178.1(5) . . . . ? C71 C66 C67 C75 -174.3(6) . . . . ? N61 C66 C67 C75 0.5(9) . . . . ? C66 C67 C68 C69 -0.6(10) . . . . ? C75 C67 C68 C69 177.2(6) . . . . ? C67 C68 C69 C70 0.1(10) . . . . ? C68 C69 C70 C71 -2.4(10) . . . . ? C67 C66 C71 C70 -5.5(9) . . . . ? N61 C66 C71 C70 179.8(5) . . . . ? C67 C66 C71 C72 176.5(6) . . . . ? N61 C66 C71 C72 1.8(9) . . . . ? C69 C70 C71 C66 5.1(10) . . . . ? C69 C70 C71 C72 -176.9(6) . . . . ? C66 C71 C72 C73 73.1(8) . . . . ? C70 C71 C72 C73 -104.9(7) . . . . ? C66 C71 C72 C74 -164.5(6) . . . . ? C70 C71 C72 C74 17.5(9) . . . . ? C68 C67 C75 C77 -71.9(8) . . . . ? C66 C67 C75 C77 105.8(7) . . . . ? C68 C67 C75 C76 50.2(8) . . . . ? C66 C67 C75 C76 -132.2(7) . . . . ? N61 C62 C78 C79 12.0(9) . . . . ? C63 C62 C78 C79 -170.0(5) . . . . ? Ti60 C62 C78 C79 92.2(13) . . . . ? N61 C62 C78 C80 -107.7(7) . . . . ? C63 C62 C78 C80 70.3(6) . . . . ? Ti60 C62 C78 C80 -27.5(15) . . . . ? N61 C62 C78 C81 134.1(6) . . . . ? C63 C62 C78 C81 -47.9(7) . . . . ? Ti60 C62 C78 C81 -145.7(10) . . . . ? N65 C64 C82 C85 -148.3(6) . . . . ? C63 C64 C82 C85 37.7(7) . . . . ? Ti60 C64 C82 C85 138.0(7) . . . . ? N65 C64 C82 C83 -24.9(8) . . . . ? C63 C64 C82 C83 161.2(5) . . . . ? Ti60 C64 C82 C83 -98.5(8) . . . . ? N65 C64 C82 C84 94.2(7) . . . . ? C63 C64 C82 C84 -79.7(6) . . . . ? Ti60 C64 C82 C84 20.6(10) . . . . ? C64 N65 C86 C91 -101.4(7) . . . . ? Ti60 N65 C86 C91 56.7(9) . . . . ? C64 N65 C86 C87 78.5(8) . . . . ? Ti60 N65 C86 C87 -123.4(6) . . . . ? C91 C86 C87 C88 3.3(9) . . . . ? N65 C86 C87 C88 -176.6(6) . . . . ? C91 C86 C87 C95 -174.0(6) . . . . ? N65 C86 C87 C95 6.2(9) . . . . ? C86 C87 C88 C89 -0.4(10) . . . . ? C95 C87 C88 C89 176.9(6) . . . . ? C87 C88 C89 C90 -2.8(11) . . . . ? C88 C89 C90 C91 3.3(11) . . . . ? C89 C90 C91 C86 -0.5(10) . . . . ? C89 C90 C91 C92 -179.0(6) . . . . ? C87 C86 C91 C90 -2.8(10) . . . . ? N65 C86 C91 C90 177.1(6) . . . . ? C87 C86 C91 C92 175.6(6) . . . . ? N65 C86 C91 C92 -4.5(10) . . . . ? C90 C91 C92 C94 58.0(8) . . . . ? C86 C91 C92 C94 -120.4(7) . . . . ? C90 C91 C92 C93 -63.9(8) . . . . ? C86 C91 C92 C93 117.6(7) . . . . ? C88 C87 C95 C96 81.3(8) . . . . ? C86 C87 C95 C96 -101.5(7) . . . . ? C88 C87 C95 C97 -42.5(8) . . . . ? C86 C87 C95 C97 134.7(6) . . . . ? N65 Ti60 N98 C99 -91(14) . . . . ? O111 Ti60 N98 C99 41(14) . . . . ? N61 Ti60 N98 C99 165(100) . . . . ? C64 Ti60 N98 C99 -88(14) . . . . ? C63 Ti60 N98 C99 -140(14) . . . . ? C62 Ti60 N98 C99 165(100) . . . . ? Ti60 N98 C99 C100 130(14) . . . . ? Ti60 N98 C99 C104 -52(14) . . . . ? N98 C99 C100 C101 176.3(6) . . . . ? C104 C99 C100 C101 -1.6(9) . . . . ? N98 C99 C100 C108 -4.3(9) . . . . ? C104 C99 C100 C108 177.8(6) . . . . ? C99 C100 C101 C102 -0.7(9) . . . . ? C108 C100 C101 C102 179.9(6) . . . . ? C100 C101 C102 C103 3.6(10) . . . . ? C101 C102 C103 C104 -4.3(10) . . . . ? C102 C103 C104 C99 2.1(10) . . . . ? C102 C103 C104 C105 175.8(6) . . . . ? C100 C99 C104 C103 1.0(9) . . . . ? N98 C99 C104 C103 -176.9(6) . . . . ? C100 C99 C104 C105 -172.7(6) . . . . ? N98 C99 C104 C105 9.4(9) . . . . ? C103 C104 C105 C107 -77.7(8) . . . . ? C99 C104 C105 C107 95.8(8) . . . . ? C103 C104 C105 C106 45.7(9) . . . . ? C99 C104 C105 C106 -140.9(7) . . . . ? C101 C100 C108 C109 -65.0(8) . . . . ? C99 C100 C108 C109 115.6(7) . . . . ? C101 C100 C108 C110 59.6(8) . . . . ? C99 C100 C108 C110 -119.9(7) . . . . ? N98 Ti60 O111 S112 -134.9(7) . . . . ? N65 Ti60 O111 S112 -10.0(8) . . . . ? N61 Ti60 O111 S112 103.4(7) . . . . ? C64 Ti60 O111 S112 14.7(7) . . . . ? C63 Ti60 O111 S112 45.3(7) . . . . ? C62 Ti60 O111 S112 76.8(7) . . . . ? Ti60 O111 S112 O113 -66.0(8) . . . . ? Ti60 O111 S112 O114 72.1(8) . . . . ? Ti60 O111 S112 C115 -177.8(7) . . . . ? O113 S112 C115 F116 -172.2(6) . . . . ? O114 S112 C115 F116 63.1(7) . . . . ? O111 S112 C115 F116 -54.9(7) . . . . ? O113 S112 C115 F117 67.1(7) . . . . ? O114 S112 C115 F117 -57.6(7) . . . . ? O111 S112 C115 F117 -175.7(6) . . . . ? O113 S112 C115 F118 -52.0(6) . . . . ? O114 S112 C115 F118 -176.6(6) . . . . ? O111 S112 C115 F118 65.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.213 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.095 data_04217 _database_code_depnum_ccdc_archive 'CCDC 260836' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H75.50 N3 O0.25 Ti' _chemical_formula_weight 758.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ti Ti 0.2776 0.4457 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 12.5278(9) _cell_length_b 18.9350(14) _cell_length_c 19.1865(14) _cell_angle_alpha 86.622(2) _cell_angle_beta 88.397(2) _cell_angle_gamma 89.408(2) _cell_volume 4541.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 126(2) _cell_measurement_reflns_used 1020 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 30.15 _exptl_crystal_description 'cleaved fragment' _exptl_crystal_colour red/pink _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.109 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1658 _exptl_absorpt_coefficient_mu 0.224 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; _diffrn_ambient_temperature 126(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details ' 0.30 degree frames measured for 5.16 seconds each' _diffrn_measurement_method '\w scans' _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 153748 _diffrn_reflns_av_R_equivalents 0.0802 _diffrn_reflns_av_sigmaI/netI 0.1012 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 33.18 _reflns_number_total 34685 _reflns_number_gt 19445 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999), XTEL (local package)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Reciprocal Net (http://recipnet.org)' _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. A disorder occurs with the diethyl ether lying at a center of inversion. All hydrogen atoms With the exception of those associated with the solvent were located and refined isotropically. While a few of the ranges lie outside "ideal" values all are qualatively correct. The correctness of the hydrogen atoms on the methyl groups attached to the metals can be judged by the overall behaviour of the hydrogen atoms. Note that two independent molecules are present. ; _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^)+(0.0340P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 34685 _refine_ls_number_parameters 1569 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0931 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.0980 _refine_ls_wR_factor_gt 0.0851 _refine_ls_goodness_of_fit_ref 0.851 _refine_ls_restrained_S_all 0.851 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 1.183619(17) 0.341375(11) 0.229708(11) 0.01288(5) Uani 1 1 d . . . N2 N 1.29639(8) 0.38915(5) 0.16869(5) 0.0134(2) Uani 1 1 d . . . C3 C 1.36660(9) 0.41282(6) 0.21575(6) 0.0141(2) Uani 1 1 d . . . C4 C 1.32998(10) 0.44018(7) 0.27743(6) 0.0153(2) Uani 1 1 d . . . C5 C 1.22664(10) 0.46042(6) 0.30626(6) 0.0144(2) Uani 1 1 d . . . N6 N 1.14081(8) 0.42492(5) 0.29151(5) 0.01330(19) Uani 1 1 d . . . C7 C 1.31304(9) 0.39344(6) 0.09423(6) 0.0151(2) Uani 1 1 d . . . C8 C 1.31606(9) 0.46073(7) 0.05822(6) 0.0164(2) Uani 1 1 d . . . C9 C 1.31716(11) 0.46375(8) -0.01452(7) 0.0214(3) Uani 1 1 d . . . C10 C 1.31881(11) 0.40315(8) -0.05105(7) 0.0242(3) Uani 1 1 d . . . C11 C 1.32211(11) 0.33794(8) -0.01548(7) 0.0217(3) Uani 1 1 d . . . C12 C 1.31969(10) 0.33125(7) 0.05747(6) 0.0175(2) Uani 1 1 d . . . C13 C 1.33344(12) 0.25767(7) 0.09259(7) 0.0231(3) Uani 1 1 d . . . C14 C 1.44178(14) 0.22599(9) 0.07118(9) 0.0334(4) Uani 1 1 d . . . C15 C 1.24392(13) 0.20661(8) 0.07787(9) 0.0295(3) Uani 1 1 d . . . C16 C 1.31888(10) 0.52901(7) 0.09586(7) 0.0185(3) Uani 1 1 d . . . C17 C 1.37625(13) 0.58884(8) 0.05349(9) 0.0279(3) Uani 1 1 d . . . C18 C 1.20770(12) 0.55260(9) 0.11796(9) 0.0295(3) Uani 1 1 d . . . C19 C 1.48981(9) 0.40202(7) 0.20846(6) 0.0174(2) Uani 1 1 d . . . C20 C 1.53563(11) 0.40782(9) 0.13346(8) 0.0258(3) Uani 1 1 d . . . C21 C 1.55171(13) 0.45387(11) 0.24927(11) 0.0403(4) Uani 1 1 d . . . C22 C 1.51295(13) 0.32647(9) 0.23913(9) 0.0329(4) Uani 1 1 d . . . C23 C 1.23393(10) 0.52486(7) 0.35280(6) 0.0184(3) Uani 1 1 d . . . C24 C 1.30751(12) 0.50695(9) 0.41442(8) 0.0260(3) Uani 1 1 d . . . C25 C 1.28467(13) 0.58590(8) 0.30637(8) 0.0262(3) Uani 1 1 d . . . C26 C 1.12812(11) 0.55351(8) 0.38250(8) 0.0224(3) Uani 1 1 d . . . C27 C 1.03755(9) 0.43047(6) 0.32682(6) 0.0143(2) Uani 1 1 d . . . C28 C 0.95018(10) 0.46087(6) 0.29100(6) 0.0156(2) Uani 1 1 d . . . C29 C 0.85298(10) 0.46625(7) 0.32760(7) 0.0202(3) Uani 1 1 d . . . C30 C 0.84012(11) 0.43942(7) 0.39571(7) 0.0224(3) Uani 1 1 d . . . C31 C 0.92461(10) 0.40482(7) 0.42818(7) 0.0202(3) Uani 1 1 d . . . C32 C 1.02464(10) 0.39963(6) 0.39526(6) 0.0164(2) Uani 1 1 d . . . C33 C 1.11144(11) 0.35834(7) 0.43449(6) 0.0193(3) Uani 1 1 d . . . C34 C 1.12382(13) 0.38091(9) 0.50940(7) 0.0270(3) Uani 1 1 d . . . C35 C 1.08734(13) 0.27910(8) 0.43627(8) 0.0247(3) Uani 1 1 d . . . C36 C 0.95824(10) 0.49008(7) 0.21565(7) 0.0182(3) Uani 1 1 d . . . C37 C 0.86114(11) 0.47160(8) 0.17383(8) 0.0247(3) Uani 1 1 d . . . C38 C 0.97346(13) 0.57028(8) 0.21158(8) 0.0267(3) Uani 1 1 d . . . N39 N 1.07256(8) 0.31686(5) 0.18598(5) 0.0161(2) Uani 1 1 d . . . C40 C 0.97552(10) 0.29727(6) 0.15904(6) 0.0163(2) Uani 1 1 d . . . C41 C 0.95684(10) 0.30629(7) 0.08645(7) 0.0200(3) Uani 1 1 d . . . C42 C 0.85667(12) 0.28994(8) 0.06230(8) 0.0277(3) Uani 1 1 d . . . C43 C 0.77630(12) 0.26419(8) 0.10695(8) 0.0309(3) Uani 1 1 d . . . C44 C 0.79552(11) 0.25319(8) 0.17724(8) 0.0255(3) Uani 1 1 d . . . C45 C 0.89345(10) 0.26922(6) 0.20476(7) 0.0181(3) Uani 1 1 d . . . C46 C 0.91405(10) 0.25383(7) 0.28140(7) 0.0191(3) Uani 1 1 d . . . C47 C 0.96355(12) 0.17992(8) 0.29219(9) 0.0267(3) Uani 1 1 d . . . C48 C 0.81588(12) 0.26193(9) 0.32902(8) 0.0269(3) Uani 1 1 d . . . C49 C 1.04265(11) 0.33535(7) 0.03601(7) 0.0219(3) Uani 1 1 d . . . C50 C 1.03459(13) 0.41550(8) 0.02658(8) 0.0283(3) Uani 1 1 d . . . C51 C 1.04281(14) 0.30182(9) -0.03501(8) 0.0304(3) Uani 1 1 d . . . C52 C 1.24978(11) 0.25168(7) 0.29014(8) 0.0134(2) Uani 1 1 d . . . Ti53 Ti 0.546195(18) 0.124513(12) 0.654278(11) 0.01501(5) Uani 1 1 d . . . N54 N 0.67790(8) 0.10911(5) 0.71413(5) 0.0170(2) Uani 1 1 d . . . C55 C 0.68776(10) 0.03858(7) 0.71635(6) 0.0178(2) Uani 1 1 d . . . C56 C 0.59615(10) -0.00380(7) 0.70767(7) 0.0174(2) Uani 1 1 d . . . C57 C 0.48474(10) 0.00515(6) 0.71599(6) 0.0161(2) Uani 1 1 d . . . N58 N 0.44150(8) 0.07059(5) 0.71890(5) 0.0149(2) Uani 1 1 d . . . C59 C 0.76112(10) 0.15804(7) 0.72951(7) 0.0212(3) Uani 1 1 d . . . C60 C 0.77167(11) 0.17748(7) 0.79869(8) 0.0268(3) Uani 1 1 d . . . C61 C 0.85626(13) 0.22210(8) 0.81190(10) 0.0364(4) Uani 1 1 d . . . C62 C 0.92364(13) 0.24851(8) 0.75973(11) 0.0409(4) Uani 1 1 d . . . C63 C 0.90746(12) 0.23332(8) 0.69179(10) 0.0348(4) Uani 1 1 d . . . C64 C 0.82567(11) 0.18791(7) 0.67476(8) 0.0260(3) Uani 1 1 d . . . C65 C 0.81077(12) 0.17434(8) 0.59864(8) 0.0308(3) Uani 1 1 d . . . C66 C 0.77747(14) 0.24296(10) 0.55857(10) 0.0393(4) Uani 1 1 d . . . C67 C 0.91065(15) 0.14343(11) 0.56285(11) 0.0427(4) Uani 1 1 d . . . C68 C 0.69457(13) 0.15279(8) 0.85739(8) 0.0308(3) Uani 1 1 d . . . C69 C 0.71730(17) 0.07789(10) 0.88683(10) 0.0429(4) Uani 1 1 d . . . C70 C 0.68847(16) 0.20247(11) 0.91736(11) 0.0434(5) Uani 1 1 d . . . C71 C 0.79338(10) -0.00638(7) 0.71984(7) 0.0222(3) Uani 1 1 d . . . C72 C 0.81236(13) -0.03463(9) 0.64666(9) 0.0308(3) Uani 1 1 d . . . C73 C 0.77997(13) -0.06929(8) 0.77362(9) 0.0272(3) Uani 1 1 d . . . C74 C 0.89449(12) 0.03221(8) 0.73908(10) 0.0298(3) Uani 1 1 d . . . C75 C 0.42135(10) -0.06492(7) 0.71169(7) 0.0217(3) Uani 1 1 d . . . C76 C 0.47215(15) -0.12502(10) 0.75706(14) 0.0474(5) Uani 1 1 d . . . C77 C 0.42962(16) -0.08306(11) 0.63461(10) 0.0416(5) Uani 1 1 d . . . C78 C 0.30233(12) -0.06296(8) 0.73238(9) 0.0289(3) Uani 1 1 d . . . C79 C 0.33732(10) 0.08475(6) 0.74878(7) 0.0176(2) Uani 1 1 d . . . C80 C 0.32130(11) 0.07531(7) 0.82152(7) 0.0214(3) Uani 1 1 d . . . C81 C 0.21907(12) 0.08719(8) 0.84964(8) 0.0307(3) Uani 1 1 d . . . C82 C 0.13580(12) 0.10857(9) 0.80812(9) 0.0347(4) Uani 1 1 d . . . C83 C 0.15396(11) 0.12064(8) 0.73732(9) 0.0304(3) Uani 1 1 d . . . C84 C 0.25407(10) 0.11013(7) 0.70603(7) 0.0231(3) Uani 1 1 d . . . C85 C 0.26609(13) 0.12552(9) 0.62772(8) 0.0352(4) Uani 1 1 d . . . C86 C 0.22562(15) 0.19983(10) 0.60662(10) 0.0395(4) Uani 1 1 d . . . C87 C 0.2094(2) 0.07121(13) 0.58634(13) 0.0616(7) Uani 1 1 d . . . C88 C 0.41012(13) 0.05502(8) 0.87103(7) 0.0278(3) Uani 1 1 d . . . C89 C 0.3873(2) -0.01405(11) 0.91438(12) 0.0566(6) Uani 1 1 d . . . C90 C 0.42641(16) 0.11390(10) 0.92040(9) 0.0358(4) Uani 1 1 d . . . N91 N 0.51035(8) 0.21238(5) 0.64092(5) 0.0174(2) Uani 1 1 d . . . C92 C 0.47131(10) 0.28099(7) 0.63045(7) 0.0176(2) Uani 1 1 d . . . C94 C 0.38277(12) 0.38357(8) 0.67624(8) 0.0261(3) Uani 1 1 d . . . C95 C 0.39136(12) 0.41934(8) 0.61161(8) 0.0296(3) Uani 1 1 d . . . C96 C 0.43730(12) 0.38608(8) 0.55614(8) 0.0267(3) Uani 1 1 d . . . C97 C 0.47676(10) 0.31698(7) 0.56330(7) 0.0202(3) Uani 1 1 d . . . C98 C 0.51939(12) 0.28058(8) 0.49995(7) 0.0247(3) Uani 1 1 d . . . C99 C 0.58982(17) 0.32847(10) 0.45164(10) 0.0423(4) Uani 1 1 d . . . C100 C 0.42785(16) 0.25145(12) 0.45962(10) 0.0448(5) Uani 1 1 d . . . C101 C 0.41210(12) 0.27764(8) 0.75923(7) 0.0249(3) Uani 1 1 d . . . C102 C 0.49541(14) 0.30527(10) 0.80692(9) 0.0339(4) Uani 1 1 d . . . C103 C 0.29966(14) 0.28324(10) 0.79232(9) 0.0341(4) Uani 1 1 d . . . C104 C 0.56255(14) 0.08464(8) 0.55196(8) 0.0251(3) Uani 1 1 d . . . H105 H 1.3827(11) 0.4521(7) 0.3070(7) 0.019(4) Uiso 1 1 d . . . H106 H 1.3191(11) 0.5081(7) -0.0393(7) 0.018(4) Uiso 1 1 d . . . H107 H 1.3195(11) 0.4072(8) -0.1009(8) 0.027(4) Uiso 1 1 d . . . H108 H 1.3261(11) 0.2972(8) -0.0404(7) 0.024(4) Uiso 1 1 d . . . H109 H 1.3325(11) 0.2621(7) 0.1419(8) 0.024(4) Uiso 1 1 d . . . H110 H 1.5002(13) 0.2558(9) 0.0825(8) 0.039(5) Uiso 1 1 d . . . H111 H 1.4491(12) 0.2192(8) 0.0196(8) 0.033(4) Uiso 1 1 d . . . H112 H 1.4483(13) 0.1784(9) 0.0943(8) 0.041(5) Uiso 1 1 d . . . H113 H 1.1752(13) 0.2210(8) 0.0977(8) 0.031(4) Uiso 1 1 d . . . H114 H 1.2344(13) 0.2033(8) 0.0273(9) 0.039(5) Uiso 1 1 d . . . H115 H 1.2621(12) 0.1584(9) 0.0972(8) 0.036(4) Uiso 1 1 d . . . H116 H 1.3593(11) 0.5215(7) 0.1382(7) 0.023(4) Uiso 1 1 d . . . H117 H 1.3332(14) 0.6080(9) 0.0110(9) 0.052(5) Uiso 1 1 d . . . H118 H 1.4491(13) 0.5732(8) 0.0348(8) 0.037(4) Uiso 1 1 d . . . H119 H 1.3849(13) 0.6285(9) 0.0833(9) 0.043(5) Uiso 1 1 d . . . H120 H 1.2093(12) 0.5986(8) 0.1413(8) 0.030(4) Uiso 1 1 d . . . H121 H 1.1708(14) 0.5152(9) 0.1505(9) 0.052(5) Uiso 1 1 d . . . H122 H 1.1669(11) 0.5645(7) 0.0761(7) 0.016(4) Uiso 1 1 d . . . H123 H 1.5245(13) 0.4583(9) 0.1125(8) 0.041(5) Uiso 1 1 d . . . H124 H 1.5052(12) 0.3731(8) 0.1032(8) 0.032(4) Uiso 1 1 d . . . H125 H 1.6144(12) 0.3981(8) 0.1361(7) 0.029(4) Uiso 1 1 d . . . H126 H 1.5316(13) 0.5028(9) 0.2333(8) 0.039(5) Uiso 1 1 d . . . H127 H 1.6261(14) 0.4492(9) 0.2382(9) 0.046(5) Uiso 1 1 d . . . H128 H 1.5409(14) 0.4478(10) 0.2996(10) 0.056(6) Uiso 1 1 d . . . H129 H 1.5908(13) 0.3194(8) 0.2373(8) 0.031(4) Uiso 1 1 d . . . H130 H 1.4761(15) 0.2894(10) 0.2119(10) 0.058(6) Uiso 1 1 d . . . H131 H 1.4907(13) 0.3209(8) 0.2865(9) 0.039(5) Uiso 1 1 d . . . H132 H 1.3813(12) 0.5011(8) 0.4002(8) 0.029(4) Uiso 1 1 d . . . H133 H 1.3052(11) 0.5466(8) 0.4431(8) 0.026(4) Uiso 1 1 d . . . H134 H 1.2817(12) 0.4638(8) 0.4420(8) 0.031(4) Uiso 1 1 d . . . H135 H 1.2394(12) 0.6020(8) 0.2654(8) 0.036(4) Uiso 1 1 d . . . H136 H 1.3549(12) 0.5744(8) 0.2873(8) 0.031(4) Uiso 1 1 d . . . H137 H 1.2949(12) 0.6264(9) 0.3335(8) 0.036(4) Uiso 1 1 d . . . H138 H 1.0740(12) 0.5628(8) 0.3470(8) 0.027(4) Uiso 1 1 d . . . H139 H 1.0944(11) 0.5215(8) 0.4184(7) 0.024(4) Uiso 1 1 d . . . H140 H 1.1433(11) 0.5992(8) 0.4036(8) 0.029(4) Uiso 1 1 d . . . H141 H 0.7911(11) 0.4902(7) 0.3053(7) 0.023(4) Uiso 1 1 d . . . H142 H 0.7722(12) 0.4418(7) 0.4209(7) 0.026(4) Uiso 1 1 d . . . H143 H 0.9146(11) 0.3836(7) 0.4746(7) 0.024(4) Uiso 1 1 d . . . H144 H 1.1777(10) 0.3660(7) 0.4109(7) 0.013(3) Uiso 1 1 d . . . H145 H 1.0655(13) 0.3641(8) 0.5394(8) 0.037(5) Uiso 1 1 d . . . H146 H 1.1868(13) 0.3596(8) 0.5298(8) 0.036(5) Uiso 1 1 d . . . H147 H 1.1285(12) 0.4328(9) 0.5113(8) 0.035(4) Uiso 1 1 d . . . H148 H 1.0799(12) 0.2638(8) 0.3895(8) 0.030(4) Uiso 1 1 d . . . H149 H 1.1438(12) 0.2510(7) 0.4587(7) 0.025(4) Uiso 1 1 d . . . H150 H 1.0215(12) 0.2692(8) 0.4631(8) 0.028(4) Uiso 1 1 d . . . H151 H 1.0198(11) 0.4687(7) 0.1952(7) 0.016(3) Uiso 1 1 d . . . H152 H 0.8439(11) 0.4203(8) 0.1770(7) 0.027(4) Uiso 1 1 d . . . H153 H 0.8747(12) 0.4844(8) 0.1244(8) 0.031(4) Uiso 1 1 d . . . H154 H 0.7979(12) 0.4979(8) 0.1892(7) 0.028(4) Uiso 1 1 d . . . H155 H 0.9756(11) 0.5902(8) 0.1630(8) 0.027(4) Uiso 1 1 d . . . H156 H 0.9132(13) 0.5940(8) 0.2342(8) 0.033(4) Uiso 1 1 d . . . H157 H 1.0403(12) 0.5841(7) 0.2333(7) 0.024(4) Uiso 1 1 d . . . H158 H 0.8438(12) 0.2989(8) 0.0151(8) 0.030(4) Uiso 1 1 d . . . H159 H 0.7081(12) 0.2517(8) 0.0900(8) 0.033(4) Uiso 1 1 d . . . H160 H 0.7420(12) 0.2339(8) 0.2081(8) 0.029(4) Uiso 1 1 d . . . H161 H 0.9668(11) 0.2877(7) 0.2947(7) 0.017(3) Uiso 1 1 d . . . H162 H 0.9810(12) 0.1669(8) 0.3430(9) 0.039(5) Uiso 1 1 d . . . H163 H 0.9145(12) 0.1434(8) 0.2784(7) 0.028(4) Uiso 1 1 d . . . H164 H 1.0329(13) 0.1762(8) 0.2630(8) 0.040(5) Uiso 1 1 d . . . H165 H 0.7597(13) 0.2241(8) 0.3222(8) 0.038(5) Uiso 1 1 d . . . H166 H 0.8381(12) 0.2574(8) 0.3774(8) 0.034(4) Uiso 1 1 d . . . H167 H 0.7812(13) 0.3093(9) 0.3210(8) 0.041(5) Uiso 1 1 d . . . H168 H 1.1123(11) 0.3238(7) 0.0574(7) 0.019(4) Uiso 1 1 d . . . H169 H 0.9636(13) 0.4319(8) 0.0089(8) 0.039(5) Uiso 1 1 d . . . H170 H 1.0928(12) 0.4362(8) -0.0077(8) 0.036(4) Uiso 1 1 d . . . H171 H 1.0438(12) 0.4380(8) 0.0718(8) 0.029(4) Uiso 1 1 d . . . H172 H 1.1061(13) 0.3162(8) -0.0629(8) 0.034(4) Uiso 1 1 d . . . H173 H 1.0454(12) 0.2491(9) -0.0307(8) 0.034(4) Uiso 1 1 d . . . H174 H 0.9811(14) 0.3177(9) -0.0630(9) 0.050(5) Uiso 1 1 d . . . H175 H 1.2095(14) 0.2269(9) 0.3011(9) 0.036(5) Uiso 1 1 d . . . H176 H 1.2899(14) 0.2369(9) 0.2665(9) 0.041(5) Uiso 1 1 d . . . H177 H 1.2743(14) 0.2651(9) 0.3175(9) 0.038(6) Uiso 1 1 d . . . H178 H 0.6136(11) -0.0484(7) 0.6973(7) 0.020(4) Uiso 1 1 d . . . H179 H 0.8654(12) 0.2345(8) 0.8585(8) 0.035(5) Uiso 1 1 d . . . H180 H 0.9819(13) 0.2785(9) 0.7701(8) 0.042(5) Uiso 1 1 d . . . H181 H 0.9492(12) 0.2528(8) 0.6542(8) 0.033(4) Uiso 1 1 d . . . H182 H 0.7535(11) 0.1403(7) 0.5951(7) 0.023(4) Uiso 1 1 d . . . H183 H 0.7107(14) 0.2656(9) 0.5793(9) 0.043(5) Uiso 1 1 d . . . H184 H 0.8385(14) 0.2774(9) 0.5563(9) 0.047(5) Uiso 1 1 d . . . H185 H 0.7634(13) 0.2319(9) 0.5116(9) 0.041(5) Uiso 1 1 d . . . H186 H 0.9704(14) 0.1781(9) 0.5614(9) 0.046(5) Uiso 1 1 d . . . H187 H 0.9359(13) 0.0976(9) 0.5855(9) 0.046(5) Uiso 1 1 d . . . H188 H 0.8961(14) 0.1304(9) 0.5143(10) 0.048(5) Uiso 1 1 d . . . H189 H 0.6231(13) 0.1518(8) 0.8383(8) 0.043(5) Uiso 1 1 d . . . H190 H 0.6672(17) 0.0651(11) 0.9292(12) 0.082(7) Uiso 1 1 d . . . H191 H 0.7086(15) 0.0416(10) 0.8510(10) 0.064(6) Uiso 1 1 d . . . H192 H 0.7935(12) 0.0811(7) 0.9043(7) 0.020(4) Uiso 1 1 d . . . H193 H 0.7549(16) 0.1986(10) 0.9437(10) 0.059(6) Uiso 1 1 d . . . H194 H 0.6841(14) 0.2498(10) 0.8979(9) 0.052(6) Uiso 1 1 d . . . H195 H 0.6280(15) 0.1867(10) 0.9500(10) 0.054(6) Uiso 1 1 d . . . H196 H 0.8813(13) -0.0586(8) 0.6446(8) 0.038(5) Uiso 1 1 d . . . H197 H 0.7609(13) -0.0701(9) 0.6347(8) 0.036(5) Uiso 1 1 d . . . H198 H 0.8107(12) 0.0031(9) 0.6116(8) 0.035(5) Uiso 1 1 d . . . H199 H 0.8436(13) -0.0967(8) 0.7732(8) 0.038(5) Uiso 1 1 d . . . H200 H 0.7220(13) -0.1000(8) 0.7653(8) 0.038(5) Uiso 1 1 d . . . H201 H 0.7686(14) -0.0531(9) 0.8195(9) 0.048(5) Uiso 1 1 d . . . H202 H 0.8910(12) 0.0512(8) 0.7832(8) 0.027(4) Uiso 1 1 d . . . H203 H 0.9542(13) -0.0030(8) 0.7390(8) 0.036(4) Uiso 1 1 d . . . H204 H 0.9189(12) 0.0691(8) 0.7057(8) 0.034(4) Uiso 1 1 d . . . H205 H 0.4805(16) -0.1106(10) 0.8049(11) 0.063(7) Uiso 1 1 d . . . H206 H 0.4311(14) -0.1654(10) 0.7575(9) 0.050(5) Uiso 1 1 d . . . H207 H 0.5434(16) -0.1398(10) 0.7392(9) 0.057(6) Uiso 1 1 d . . . H208 H 0.3987(19) -0.0459(13) 0.6038(12) 0.093(9) Uiso 1 1 d . . . H209 H 0.5031(15) -0.0923(9) 0.6203(9) 0.046(5) Uiso 1 1 d . . . H210 H 0.3885(14) -0.1267(10) 0.6277(9) 0.054(5) Uiso 1 1 d . . . H211 H 0.2737(12) -0.1092(8) 0.7251(8) 0.032(4) Uiso 1 1 d . . . H212 H 0.2631(12) -0.0265(8) 0.7047(8) 0.034(4) Uiso 1 1 d . . . H213 H 0.2886(13) -0.0526(8) 0.7818(9) 0.040(5) Uiso 1 1 d . . . H214 H 0.2065(12) 0.0800(8) 0.8981(8) 0.034(4) Uiso 1 1 d . . . H215 H 0.0658(14) 0.1152(9) 0.8270(8) 0.044(5) Uiso 1 1 d . . . H216 H 0.0971(13) 0.1371(8) 0.7084(8) 0.037(5) Uiso 1 1 d . . . H217 H 0.3393(13) 0.1219(8) 0.6154(8) 0.037(5) Uiso 1 1 d . . . H218 H 0.2377(14) 0.2087(9) 0.5565(10) 0.054(6) Uiso 1 1 d . . . H219 H 0.2606(15) 0.2369(10) 0.6323(10) 0.058(6) Uiso 1 1 d . . . H220 H 0.1489(15) 0.2046(9) 0.6134(9) 0.045(5) Uiso 1 1 d . . . H221 H 0.2160(18) 0.0829(12) 0.5365(13) 0.088(8) Uiso 1 1 d . . . H222 H 0.1336(17) 0.0687(11) 0.5995(10) 0.065(7) Uiso 1 1 d . . . C223 C 0.42175(10) 0.31501(7) 0.68716(7) 0.0210(3) Uani 1 1 d . . . H223 H 0.2306(17) 0.0261(12) 0.5944(11) 0.070(7) Uiso 1 1 d . . . H224 H 0.4746(12) 0.0494(7) 0.8457(7) 0.024(4) Uiso 1 1 d . . . H225 H 0.3730(16) -0.0526(11) 0.8874(11) 0.070(7) Uiso 1 1 d . . . H226 H 0.4501(16) -0.0257(10) 0.9391(10) 0.056(6) Uiso 1 1 d . . . H227 H 0.332(2) -0.0046(15) 0.9471(15) 0.130(13) Uiso 1 1 d . . . H228 H 0.4858(14) 0.1046(9) 0.9518(9) 0.041(5) Uiso 1 1 d . . . H229 H 0.3637(15) 0.1198(9) 0.9496(9) 0.054(6) Uiso 1 1 d . . . H230 H 0.4433(13) 0.1599(9) 0.8948(9) 0.045(5) Uiso 1 1 d . . . H231 H 0.3499(12) 0.4065(8) 0.7148(8) 0.034(4) Uiso 1 1 d . . . H232 H 0.3653(12) 0.4657(8) 0.6054(8) 0.036(4) Uiso 1 1 d . . . H233 H 0.4436(11) 0.4098(8) 0.5118(8) 0.027(4) Uiso 1 1 d . . . H234 H 0.5598(11) 0.2408(7) 0.5149(7) 0.020(4) Uiso 1 1 d . . . H235 H 0.5492(14) 0.3660(10) 0.4318(9) 0.046(5) Uiso 1 1 d . . . H236 H 0.6161(14) 0.3007(10) 0.4141(10) 0.054(6) Uiso 1 1 d . . . H237 H 0.6505(17) 0.3488(11) 0.4777(11) 0.071(7) Uiso 1 1 d . . . H238 H 0.3753(15) 0.2896(10) 0.4464(9) 0.055(6) Uiso 1 1 d . . . H239 H 0.3903(14) 0.2131(9) 0.4881(9) 0.048(5) Uiso 1 1 d . . . H240 H 0.4544(14) 0.2297(10) 0.4178(10) 0.055(6) Uiso 1 1 d . . . H241 H 0.4261(11) 0.2281(8) 0.7536(7) 0.022(4) Uiso 1 1 d . . . H242 H 0.5658(13) 0.2954(8) 0.7870(8) 0.035(4) Uiso 1 1 d . . . H243 H 0.4823(13) 0.3572(9) 0.8116(8) 0.042(5) Uiso 1 1 d . . . H244 H 0.4865(13) 0.2808(9) 0.8554(9) 0.044(5) Uiso 1 1 d . . . H245 H 0.2839(13) 0.3318(9) 0.8012(8) 0.040(5) Uiso 1 1 d . . . H246 H 0.2945(13) 0.2570(9) 0.8379(9) 0.047(5) Uiso 1 1 d . . . H247 H 0.2451(14) 0.2661(9) 0.7637(9) 0.042(5) Uiso 1 1 d . . . H248 H 0.5008(16) 0.0760(10) 0.5366(10) 0.060(6) Uiso 1 1 d . . . H249 H 0.5963(15) 0.1159(10) 0.5218(10) 0.055(6) Uiso 1 1 d . . . H250 H 0.5992(14) 0.0418(10) 0.5525(9) 0.048(5) Uiso 1 1 d . . . C1S C 1.0499(6) -0.0932(4) -0.0955(4) 0.093(2) Uani 0.50 1 d P A 1 H1S1 H 1.1269 -0.1029 -0.0962 0.140 Uiso 0.50 1 calc PR A 1 H1S2 H 1.0329 -0.0591 -0.1342 0.140 Uiso 0.50 1 calc PR A 1 H1S3 H 1.0113 -0.1372 -0.1006 0.140 Uiso 0.50 1 calc PR A 1 C2S C 1.0198(12) -0.0652(4) -0.0327(6) 0.138(5) Uani 0.50 1 d P A 1 H2S1 H 1.0646 -0.0901 0.0029 0.165 Uiso 0.50 1 calc PR A 1 H2S2 H 0.9459 -0.0817 -0.0226 0.165 Uiso 0.50 1 calc PR A 1 O3S O 1.0197(5) 0.0004(3) -0.0180(3) 0.0761(18) Uani 0.50 1 d P . 1 C4S C 0.9908(11) 0.0303(4) 0.0395(6) 0.122(5) Uani 0.50 1 d P . 1 H4S1 H 0.9176 0.0131 0.0509 0.146 Uiso 0.50 1 calc PR . 1 H4S2 H 1.0367 0.0082 0.0760 0.146 Uiso 0.50 1 calc PR . 1 C5S C 0.9881(12) 0.0961(6) 0.0508(7) 0.164(6) Uani 0.50 1 d P B 1 H5S1 H 1.0520 0.1084 0.0757 0.246 Uiso 0.50 1 calc PR B 1 H5S2 H 0.9243 0.1066 0.0791 0.246 Uiso 0.50 1 calc PR B 1 H5S3 H 0.9861 0.1240 0.0061 0.246 Uiso 0.50 1 calc PR B 1 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 0.01230(10) 0.01417(10) 0.01211(10) -0.00066(8) 0.00055(8) -0.00042(8) N2 0.0135(5) 0.0148(5) 0.0120(5) -0.0016(4) 0.0002(4) -0.0001(4) C3 0.0131(5) 0.0137(5) 0.0155(6) 0.0008(4) -0.0002(4) -0.0006(4) C4 0.0131(6) 0.0187(6) 0.0143(6) -0.0021(5) -0.0008(5) -0.0016(5) C5 0.0161(6) 0.0161(6) 0.0108(5) 0.0010(4) -0.0009(4) 0.0002(4) N6 0.0133(5) 0.0148(5) 0.0115(5) 0.0005(4) 0.0013(4) 0.0005(4) C7 0.0123(5) 0.0198(6) 0.0128(5) 0.0004(5) 0.0007(4) -0.0004(5) C8 0.0127(5) 0.0196(6) 0.0168(6) 0.0004(5) 0.0000(5) -0.0016(5) C9 0.0214(7) 0.0259(7) 0.0163(6) 0.0041(5) 0.0006(5) -0.0024(5) C10 0.0258(7) 0.0339(8) 0.0127(6) -0.0011(6) 0.0024(5) -0.0031(6) C11 0.0240(7) 0.0254(7) 0.0161(6) -0.0060(5) 0.0016(5) 0.0014(6) C12 0.0166(6) 0.0207(6) 0.0153(6) -0.0024(5) 0.0008(5) 0.0015(5) C13 0.0332(8) 0.0201(7) 0.0165(6) -0.0046(5) -0.0024(6) 0.0067(6) C14 0.0344(9) 0.0290(8) 0.0384(9) -0.0124(7) -0.0075(7) 0.0109(7) C15 0.0377(9) 0.0187(7) 0.0316(8) 0.0007(6) 0.0013(7) 0.0029(6) C16 0.0209(6) 0.0188(6) 0.0157(6) 0.0009(5) -0.0018(5) -0.0012(5) C17 0.0317(8) 0.0218(7) 0.0297(8) -0.0004(6) 0.0046(7) -0.0057(6) C18 0.0234(7) 0.0297(8) 0.0359(9) -0.0095(7) 0.0049(7) -0.0011(6) C19 0.0123(6) 0.0228(6) 0.0172(6) -0.0030(5) 0.0019(5) -0.0002(5) C20 0.0157(7) 0.0381(9) 0.0229(7) 0.0015(6) 0.0048(5) 0.0017(6) C21 0.0151(7) 0.0587(12) 0.0500(11) -0.0290(10) 0.0037(7) -0.0082(7) C22 0.0186(7) 0.0407(9) 0.0373(9) 0.0121(8) 0.0043(7) 0.0091(7) C23 0.0185(6) 0.0201(6) 0.0169(6) -0.0049(5) 0.0026(5) -0.0028(5) C24 0.0251(8) 0.0348(8) 0.0192(7) -0.0099(6) -0.0020(6) -0.0042(6) C25 0.0304(8) 0.0208(7) 0.0276(8) -0.0058(6) 0.0076(6) -0.0058(6) C26 0.0238(7) 0.0208(7) 0.0233(7) -0.0085(6) 0.0051(6) -0.0018(5) C27 0.0132(5) 0.0142(5) 0.0154(6) -0.0023(5) 0.0028(4) -0.0002(4) C28 0.0151(6) 0.0141(6) 0.0174(6) -0.0010(5) 0.0015(5) 0.0005(4) C29 0.0154(6) 0.0214(6) 0.0234(7) 0.0008(5) 0.0024(5) 0.0033(5) C30 0.0169(6) 0.0262(7) 0.0237(7) -0.0012(6) 0.0082(5) 0.0018(5) C31 0.0214(7) 0.0216(7) 0.0172(6) -0.0001(5) 0.0056(5) -0.0008(5) C32 0.0175(6) 0.0167(6) 0.0151(6) -0.0017(5) 0.0015(5) 0.0003(5) C33 0.0189(6) 0.0244(7) 0.0141(6) 0.0018(5) 0.0016(5) 0.0006(5) C34 0.0306(8) 0.0339(9) 0.0165(7) -0.0010(6) -0.0022(6) 0.0005(7) C35 0.0280(8) 0.0235(7) 0.0221(7) 0.0044(6) -0.0026(6) 0.0032(6) C36 0.0155(6) 0.0200(6) 0.0185(6) 0.0031(5) 0.0016(5) 0.0036(5) C37 0.0201(7) 0.0310(8) 0.0225(7) 0.0016(6) -0.0030(6) 0.0030(6) C38 0.0269(8) 0.0234(7) 0.0286(8) 0.0059(6) 0.0024(6) 0.0010(6) N39 0.0148(5) 0.0175(5) 0.0161(5) -0.0007(4) 0.0006(4) -0.0010(4) C40 0.0139(6) 0.0155(6) 0.0199(6) -0.0030(5) -0.0020(5) 0.0002(5) C41 0.0190(6) 0.0207(6) 0.0206(6) -0.0018(5) -0.0027(5) 0.0000(5) C42 0.0241(7) 0.0348(8) 0.0248(7) -0.0022(6) -0.0078(6) -0.0032(6) C43 0.0186(7) 0.0394(9) 0.0353(8) -0.0028(7) -0.0086(6) -0.0063(6) C44 0.0162(6) 0.0276(7) 0.0328(8) -0.0011(6) 0.0009(6) -0.0053(5) C45 0.0159(6) 0.0160(6) 0.0223(6) -0.0014(5) 0.0000(5) 0.0003(5) C46 0.0166(6) 0.0184(6) 0.0221(6) 0.0001(5) 0.0009(5) -0.0031(5) C47 0.0258(8) 0.0214(7) 0.0328(8) 0.0010(6) -0.0020(6) 0.0011(6) C48 0.0232(7) 0.0291(8) 0.0285(8) -0.0050(6) 0.0059(6) -0.0032(6) C49 0.0196(7) 0.0273(7) 0.0188(6) 0.0003(5) -0.0037(5) -0.0016(5) C50 0.0280(8) 0.0275(8) 0.0293(8) 0.0003(6) -0.0017(7) -0.0037(6) C51 0.0332(9) 0.0371(9) 0.0213(7) -0.0043(7) -0.0027(7) -0.0032(7) C52 0.0126(6) 0.0137(6) 0.0143(6) -0.0028(5) 0.0000(5) -0.0027(5) Ti53 0.01621(11) 0.01494(11) 0.01391(10) -0.00108(8) -0.00040(8) 0.00025(8) N54 0.0157(5) 0.0144(5) 0.0207(5) -0.0006(4) -0.0013(4) -0.0003(4) C55 0.0172(6) 0.0178(6) 0.0183(6) -0.0010(5) 0.0001(5) 0.0019(5) C56 0.0182(6) 0.0129(6) 0.0212(6) -0.0028(5) -0.0003(5) 0.0015(5) C57 0.0189(6) 0.0163(6) 0.0133(5) -0.0007(5) -0.0016(5) -0.0011(5) N58 0.0145(5) 0.0165(5) 0.0140(5) -0.0016(4) -0.0027(4) 0.0002(4) C59 0.0149(6) 0.0133(6) 0.0357(8) -0.0016(5) -0.0063(5) 0.0005(5) C60 0.0240(7) 0.0185(7) 0.0391(8) -0.0055(6) -0.0112(6) 0.0025(5) C61 0.0331(9) 0.0245(8) 0.0538(11) -0.0116(8) -0.0188(8) 0.0007(7) C62 0.0253(8) 0.0224(8) 0.0765(14) -0.0053(8) -0.0189(9) -0.0044(6) C63 0.0193(7) 0.0214(7) 0.0629(12) 0.0071(8) -0.0034(7) -0.0028(6) C64 0.0165(6) 0.0185(7) 0.0425(9) 0.0030(6) -0.0035(6) 0.0005(5) C65 0.0201(7) 0.0312(8) 0.0400(9) 0.0046(7) 0.0047(6) -0.0057(6) C66 0.0273(9) 0.0458(11) 0.0429(10) 0.0118(9) 0.0016(8) 0.0023(8) C67 0.0328(9) 0.0402(10) 0.0529(12) 0.0073(9) 0.0147(9) 0.0018(8) C68 0.0339(9) 0.0308(8) 0.0290(8) -0.0100(7) -0.0098(7) 0.0022(7) C69 0.0558(12) 0.0388(10) 0.0343(10) -0.0045(8) -0.0009(9) 0.0084(9) C70 0.0408(11) 0.0459(11) 0.0465(11) -0.0230(9) -0.0137(9) 0.0068(9) C71 0.0160(6) 0.0184(6) 0.0320(7) -0.0003(6) 0.0000(5) 0.0035(5) C72 0.0247(8) 0.0301(8) 0.0373(9) -0.0054(7) 0.0061(7) 0.0070(7) C73 0.0242(8) 0.0189(7) 0.0380(9) 0.0023(6) -0.0021(7) 0.0043(6) C74 0.0169(7) 0.0216(7) 0.0506(10) 0.0011(7) -0.0043(7) 0.0036(6) C75 0.0202(6) 0.0154(6) 0.0296(7) -0.0019(5) -0.0002(6) -0.0041(5) C76 0.0291(9) 0.0237(8) 0.0871(17) 0.0203(10) -0.0069(10) -0.0072(7) C77 0.0422(10) 0.0414(10) 0.0438(10) -0.0252(9) 0.0087(9) -0.0202(9) C78 0.0219(7) 0.0225(7) 0.0426(9) -0.0050(7) -0.0004(7) -0.0071(6) C79 0.0154(6) 0.0166(6) 0.0208(6) -0.0012(5) -0.0003(5) -0.0010(5) C80 0.0224(7) 0.0205(6) 0.0212(6) -0.0006(5) 0.0016(5) 0.0008(5) C81 0.0284(8) 0.0342(8) 0.0288(8) -0.0011(7) 0.0107(7) -0.0005(6) C82 0.0191(7) 0.0375(9) 0.0471(10) -0.0049(8) 0.0106(7) 0.0008(6) C83 0.0158(7) 0.0343(8) 0.0415(9) -0.0027(7) -0.0045(6) 0.0014(6) C84 0.0170(6) 0.0258(7) 0.0267(7) -0.0033(6) -0.0046(5) 0.0007(5) C85 0.0224(8) 0.0565(11) 0.0266(8) -0.0012(7) -0.0081(6) 0.0103(7) C86 0.0286(9) 0.0529(11) 0.0360(10) 0.0110(9) -0.0125(8) -0.0024(8) C87 0.0840(19) 0.0581(14) 0.0458(13) -0.0170(11) -0.0366(13) 0.0278(13) C88 0.0332(8) 0.0332(8) 0.0168(7) -0.0005(6) -0.0008(6) 0.0066(6) C89 0.0943(19) 0.0381(11) 0.0378(11) 0.0082(9) -0.0295(13) -0.0015(12) C90 0.0396(10) 0.0400(10) 0.0285(8) -0.0062(7) -0.0042(8) 0.0026(8) N91 0.0187(5) 0.0181(5) 0.0155(5) -0.0011(4) -0.0003(4) 0.0007(4) C92 0.0153(6) 0.0168(6) 0.0208(6) -0.0004(5) -0.0032(5) -0.0008(5) C94 0.0260(7) 0.0221(7) 0.0309(8) -0.0073(6) -0.0027(6) 0.0044(6) C95 0.0300(8) 0.0185(7) 0.0402(9) 0.0001(6) -0.0084(7) 0.0066(6) C96 0.0264(7) 0.0236(7) 0.0295(8) 0.0069(6) -0.0078(6) 0.0014(6) C97 0.0172(6) 0.0210(6) 0.0223(6) 0.0016(5) -0.0044(5) -0.0002(5) C98 0.0275(7) 0.0259(7) 0.0200(7) 0.0041(6) 0.0003(6) 0.0021(6) C99 0.0492(11) 0.0385(10) 0.0363(10) 0.0126(8) 0.0149(9) 0.0065(9) C100 0.0402(10) 0.0626(13) 0.0342(10) -0.0213(10) -0.0073(8) 0.0019(10) C101 0.0324(8) 0.0203(7) 0.0223(7) -0.0042(6) 0.0030(6) 0.0016(6) C102 0.0341(9) 0.0411(10) 0.0263(8) 0.0014(7) -0.0044(7) 0.0003(7) C103 0.0315(9) 0.0419(10) 0.0295(9) -0.0091(8) 0.0044(7) -0.0060(7) C104 0.0318(8) 0.0240(8) 0.0195(7) -0.0034(6) 0.0022(6) -0.0016(6) C223 0.0203(6) 0.0195(6) 0.0236(7) -0.0033(5) -0.0027(5) 0.0000(5) C1S 0.115(6) 0.060(4) 0.105(5) -0.019(4) 0.014(4) -0.010(4) C2S 0.250(13) 0.045(5) 0.109(7) 0.032(6) 0.057(7) 0.037(8) O3S 0.084(4) 0.042(2) 0.101(5) 0.002(3) 0.018(3) -0.028(3) C4S 0.191(11) 0.057(7) 0.109(9) 0.031(6) 0.078(8) 0.029(8) C5S 0.187(12) 0.090(8) 0.222(14) -0.075(10) 0.042(9) -0.043(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 N39 1.7262(10) . ? Ti1 N2 1.9984(10) . ? Ti1 N6 2.0890(10) . ? Ti1 C52 2.1699(13) . ? Ti1 C3 2.6727(12) . ? N2 C3 1.3748(15) . ? N2 C7 1.4356(15) . ? C3 C4 1.3844(16) . ? C3 C19 1.5584(16) . ? C4 C5 1.4503(17) . ? C4 H105 0.921(14) . ? C5 N6 1.3201(15) . ? C5 C23 1.5587(17) . ? N6 C27 1.4491(15) . ? C7 C12 1.4084(17) . ? C7 C8 1.4137(17) . ? C8 C9 1.3931(17) . ? C8 C16 1.5187(18) . ? C9 C10 1.379(2) . ? C9 H106 0.942(14) . ? C10 C11 1.3761(19) . ? C10 H107 0.955(14) . ? C11 C12 1.3974(17) . ? C11 H108 0.932(14) . ? C12 C13 1.5218(18) . ? C13 C15 1.531(2) . ? C13 C14 1.534(2) . ? C13 H109 0.954(14) . ? C14 H110 0.965(17) . ? C14 H111 1.007(16) . ? C14 H112 0.984(17) . ? C15 H113 0.975(16) . ? C15 H114 0.986(16) . ? C15 H115 0.992(16) . ? C16 C18 1.5152(19) . ? C16 C17 1.5286(19) . ? C16 H116 0.972(14) . ? C17 H117 1.036(18) . ? C17 H118 1.019(16) . ? C17 H119 0.980(17) . ? C18 H120 1.003(15) . ? C18 H121 1.022(18) . ? C18 H122 0.978(13) . ? C19 C21 1.523(2) . ? C19 C20 1.5326(18) . ? C19 C22 1.542(2) . ? C20 H123 1.026(17) . ? C20 H124 0.988(16) . ? C20 H125 1.004(15) . ? C21 H126 0.991(17) . ? C21 H127 0.954(18) . ? C21 H128 0.971(19) . ? C22 H129 0.983(16) . ? C22 H130 1.020(19) . ? C22 H131 0.944(17) . ? C23 C26 1.5348(18) . ? C23 C24 1.5395(19) . ? C23 C25 1.5478(19) . ? C24 H132 0.963(15) . ? C24 H133 0.956(15) . ? C24 H134 0.999(15) . ? C25 H135 1.012(16) . ? C25 H136 0.971(16) . ? C25 H137 0.963(16) . ? C26 H138 0.981(15) . ? C26 H139 0.980(15) . ? C26 H140 0.999(15) . ? C27 C28 1.4086(17) . ? C27 C32 1.4112(16) . ? C28 C29 1.3944(17) . ? C28 C36 1.5181(17) . ? C29 C30 1.3797(18) . ? C29 H141 0.989(14) . ? C30 C31 1.3829(19) . ? C30 H142 0.969(14) . ? C31 C32 1.3926(17) . ? C31 H143 0.961(14) . ? C32 C33 1.5229(18) . ? C33 C35 1.5317(19) . ? C33 C34 1.5360(19) . ? C33 H144 0.943(13) . ? C34 H145 0.962(16) . ? C34 H146 0.965(16) . ? C34 H147 0.988(16) . ? C35 H148 0.966(15) . ? C35 H149 0.975(15) . ? C35 H150 0.973(15) . ? C36 C38 1.5295(19) . ? C36 C37 1.5306(19) . ? C36 H151 0.953(13) . ? C37 H152 0.995(15) . ? C37 H153 0.975(15) . ? C37 H154 0.979(15) . ? C38 H155 0.985(15) . ? C38 H156 0.978(16) . ? C38 H157 0.990(14) . ? N39 C40 1.3963(15) . ? C40 C41 1.4190(17) . ? C40 C45 1.4193(17) . ? C41 C42 1.3939(19) . ? C41 C49 1.5119(18) . ? C42 C43 1.378(2) . ? C42 H158 0.930(15) . ? C43 C44 1.380(2) . ? C43 H159 0.959(15) . ? C44 C45 1.3924(18) . ? C44 H160 0.944(15) . ? C45 C46 1.5109(18) . ? C46 C48 1.5233(19) . ? C46 C47 1.5301(19) . ? C46 H161 0.975(13) . ? C47 H162 1.020(16) . ? C47 H163 0.983(15) . ? C47 H164 1.025(17) . ? C48 H165 1.026(16) . ? C48 H166 0.974(16) . ? C48 H167 0.998(17) . ? C49 C50 1.520(2) . ? C49 C51 1.537(2) . ? C49 H168 0.991(13) . ? C50 H169 1.001(16) . ? C50 H170 1.033(16) . ? C50 H171 0.999(15) . ? C51 H172 0.977(16) . ? C51 H173 0.998(16) . ? C51 H174 0.987(18) . ? C52 H175 0.712(18) . ? C52 H176 0.732(18) . ? C52 H177 0.679(18) . ? Ti53 N91 1.7251(11) . ? Ti53 N58 2.0217(10) . ? Ti53 N54 2.0452(10) . ? Ti53 C104 2.1483(15) . ? Ti53 C57 2.6024(12) . ? Ti53 C55 2.6535(13) . ? Ti53 C56 2.6563(13) . ? N54 C55 1.3382(15) . ? N54 C59 1.4497(16) . ? C55 C56 1.4263(17) . ? C55 C71 1.5669(17) . ? C56 C57 1.4101(17) . ? C56 H178 0.902(14) . ? C57 N58 1.3507(15) . ? C57 C75 1.5608(17) . ? N58 C79 1.4398(16) . ? C59 C64 1.4034(19) . ? C59 C60 1.408(2) . ? C60 C61 1.400(2) . ? C60 C68 1.519(2) . ? C61 C62 1.366(3) . ? C61 H179 0.948(16) . ? C62 C63 1.372(3) . ? C62 H180 0.962(17) . ? C63 C64 1.402(2) . ? C63 H181 0.939(16) . ? C64 C65 1.515(2) . ? C65 C66 1.530(2) . ? C65 C67 1.538(2) . ? C65 H182 0.976(14) . ? C66 H183 1.018(17) . ? C66 H184 1.008(18) . ? C66 H185 0.959(17) . ? C67 H186 0.999(18) . ? C67 H187 1.000(18) . ? C67 H188 1.000(18) . ? C68 C69 1.522(2) . ? C68 C70 1.528(2) . ? C68 H189 0.978(16) . ? C69 H190 1.03(2) . ? C69 H191 1.01(2) . ? C69 H192 1.025(14) . ? C70 H193 0.99(2) . ? C70 H194 0.952(19) . ? C70 H195 1.006(19) . ? C71 C74 1.534(2) . ? C71 C73 1.537(2) . ? C71 C72 1.543(2) . ? C72 H196 0.973(16) . ? C72 H197 0.977(16) . ? C72 H198 0.952(16) . ? C73 H199 0.946(17) . ? C73 H200 0.957(17) . ? C73 H201 0.956(18) . ? C74 H202 0.939(15) . ? C74 H203 0.997(16) . ? C74 H204 0.965(16) . ? C75 C78 1.5328(19) . ? C75 C76 1.535(2) . ? C75 C77 1.538(2) . ? C76 H205 0.98(2) . ? C76 H206 0.925(18) . ? C76 H207 0.990(19) . ? C77 H208 0.98(2) . ? C77 H209 0.970(18) . ? C77 H210 0.995(19) . ? C78 H211 0.969(16) . ? C78 H212 0.983(16) . ? C78 H213 0.989(17) . ? C79 C80 1.4057(18) . ? C79 C84 1.4080(18) . ? C80 C81 1.3970(19) . ? C80 C88 1.5151(19) . ? C81 C82 1.373(2) . ? C81 H214 0.940(15) . ? C82 C83 1.377(2) . ? C82 H215 0.949(17) . ? C83 C84 1.3927(19) . ? C83 H216 0.954(16) . ? C84 C85 1.517(2) . ? C85 C86 1.527(2) . ? C85 C87 1.528(3) . ? C85 H217 0.943(16) . ? C86 H218 0.974(19) . ? C86 H219 0.993(19) . ? C86 H220 0.970(18) . ? C87 H221 0.97(2) . ? C87 H222 0.98(2) . ? C87 H223 0.90(2) . ? C88 C90 1.524(2) . ? C88 C89 1.533(2) . ? C88 H224 0.939(14) . ? C89 H225 0.94(2) . ? C89 H226 0.95(2) . ? C89 H227 0.94(3) . ? C90 H228 0.979(17) . ? C90 H229 0.961(19) . ? C90 H230 0.997(18) . ? N91 C92 1.3890(16) . ? C92 C223 1.4214(18) . ? C92 C97 1.4219(17) . ? C94 C95 1.380(2) . ? C94 C223 1.3887(19) . ? C94 H231 0.960(15) . ? C95 C96 1.378(2) . ? C95 H232 0.935(16) . ? C96 C97 1.3945(18) . ? C96 H233 0.941(15) . ? C97 C98 1.5140(19) . ? C98 C99 1.527(2) . ? C98 C100 1.527(2) . ? C98 H234 0.938(14) . ? C99 H235 0.938(18) . ? C99 H236 0.966(19) . ? C99 H237 1.01(2) . ? C100 H238 0.999(19) . ? C100 H239 0.996(18) . ? C100 H240 0.973(19) . ? C101 C223 1.5182(19) . ? C101 C102 1.523(2) . ? C101 C103 1.534(2) . ? C101 H241 0.964(14) . ? C102 H242 0.972(16) . ? C102 H243 1.004(17) . ? C102 H244 1.018(17) . ? C103 H245 0.963(17) . ? C103 H246 0.980(18) . ? C103 H247 0.959(17) . ? C104 H248 0.86(2) . ? C104 H249 0.904(19) . ? C104 H250 0.927(18) . ? C1S C2S 1.386(12) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C2S O3S 1.291(10) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? O3S C4S 0.747(11) 2_755 ? O3S O3S 0.838(10) 2_755 ? O3S C4S 1.310(11) . ? O3S C2S 1.673(11) 2_755 ? O3S C5S 1.972(11) 2_755 ? C4S C5S 1.278(11) . ? C4S C4S 1.961(19) 2_755 ? C4S H4S1 0.9900 . ? C4S H4S2 0.9900 . ? C5S H5S1 0.9800 . ? C5S H5S2 0.9800 . ? C5S H5S3 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 N39 Ti1 N2 114.37(4) . . ? N39 Ti1 N6 108.55(4) . . ? N2 Ti1 N6 99.35(4) . . ? N39 Ti1 C52 110.79(5) . . ? N2 Ti1 C52 110.83(5) . . ? N6 Ti1 C52 112.49(5) . . ? N39 Ti1 C3 143.87(4) . . ? N2 Ti1 C3 30.05(4) . . ? N6 Ti1 C3 82.05(4) . . ? C52 Ti1 C3 95.43(5) . . ? C3 N2 C7 124.98(10) . . ? C3 N2 Ti1 103.25(7) . . ? C7 N2 Ti1 131.44(8) . . ? N2 C3 C4 120.86(11) . . ? N2 C3 C19 122.97(10) . . ? C4 C3 C19 115.72(10) . . ? N2 C3 Ti1 46.70(5) . . ? C4 C3 Ti1 82.29(7) . . ? C19 C3 Ti1 142.12(8) . . ? C3 C4 C5 135.50(12) . . ? C3 C4 H105 114.8(8) . . ? C5 C4 H105 109.5(8) . . ? N6 C5 C4 119.68(11) . . ? N6 C5 C23 128.07(11) . . ? C4 C5 C23 112.25(10) . . ? C5 N6 C27 125.02(10) . . ? C5 N6 Ti1 109.95(8) . . ? C27 N6 Ti1 123.23(7) . . ? C12 C7 C8 120.70(11) . . ? C12 C7 N2 120.15(11) . . ? C8 C7 N2 119.04(11) . . ? C9 C8 C7 118.15(12) . . ? C9 C8 C16 119.39(11) . . ? C7 C8 C16 122.46(11) . . ? C10 C9 C8 121.50(13) . . ? C10 C9 H106 119.2(8) . . ? C8 C9 H106 119.3(8) . . ? C11 C10 C9 119.80(13) . . ? C11 C10 H107 121.0(9) . . ? C9 C10 H107 119.2(9) . . ? C10 C11 C12 121.50(13) . . ? C10 C11 H108 119.5(9) . . ? C12 C11 H108 119.0(9) . . ? C11 C12 C7 118.15(12) . . ? C11 C12 C13 118.07(11) . . ? C7 C12 C13 123.58(11) . . ? C12 C13 C15 113.80(11) . . ? C12 C13 C14 110.20(12) . . ? C15 C13 C14 109.84(12) . . ? C12 C13 H109 108.0(9) . . ? C15 C13 H109 106.7(9) . . ? C14 C13 H109 108.0(9) . . ? C13 C14 H110 111.7(10) . . ? C13 C14 H111 113.1(9) . . ? H110 C14 H111 106.4(13) . . ? C13 C14 H112 108.5(10) . . ? H110 C14 H112 111.4(13) . . ? H111 C14 H112 105.7(13) . . ? C13 C15 H113 112.4(9) . . ? C13 C15 H114 111.7(9) . . ? H113 C15 H114 106.8(13) . . ? C13 C15 H115 109.7(9) . . ? H113 C15 H115 109.1(13) . . ? H114 C15 H115 107.0(13) . . ? C18 C16 C8 111.40(11) . . ? C18 C16 C17 110.35(12) . . ? C8 C16 C17 113.16(11) . . ? C18 C16 H116 106.9(8) . . ? C8 C16 H116 109.6(8) . . ? C17 C16 H116 105.0(8) . . ? C16 C17 H117 112.5(10) . . ? C16 C17 H118 112.0(9) . . ? H117 C17 H118 107.1(13) . . ? C16 C17 H119 108.8(10) . . ? H117 C17 H119 106.7(13) . . ? H118 C17 H119 109.6(13) . . ? C16 C18 H120 111.4(9) . . ? C16 C18 H121 111.6(10) . . ? H120 C18 H121 109.5(13) . . ? C16 C18 H122 108.7(8) . . ? H120 C18 H122 103.1(11) . . ? H121 C18 H122 112.3(12) . . ? C21 C19 C20 106.53(12) . . ? C21 C19 C22 108.37(14) . . ? C20 C19 C22 107.80(12) . . ? C21 C19 C3 112.66(11) . . ? C20 C19 C3 115.22(10) . . ? C22 C19 C3 106.01(10) . . ? C19 C20 H123 109.5(9) . . ? C19 C20 H124 113.2(9) . . ? H123 C20 H124 110.6(12) . . ? C19 C20 H125 107.0(8) . . ? H123 C20 H125 108.6(12) . . ? H124 C20 H125 107.7(12) . . ? C19 C21 H126 109.1(10) . . ? C19 C21 H127 109.2(10) . . ? H126 C21 H127 105.8(14) . . ? C19 C21 H128 114.1(11) . . ? H126 C21 H128 109.4(15) . . ? H127 C21 H128 108.9(15) . . ? C19 C22 H129 107.3(9) . . ? C19 C22 H130 111.4(10) . . ? H129 C22 H130 110.6(13) . . ? C19 C22 H131 111.4(10) . . ? H129 C22 H131 107.0(13) . . ? H130 C22 H131 108.9(14) . . ? C26 C23 C24 107.87(11) . . ? C26 C23 C25 106.68(11) . . ? C24 C23 C25 108.45(12) . . ? C26 C23 C5 116.60(11) . . ? C24 C23 C5 110.25(11) . . ? C25 C23 C5 106.68(10) . . ? C23 C24 H132 113.2(9) . . ? C23 C24 H133 107.1(9) . . ? H132 C24 H133 106.0(12) . . ? C23 C24 H134 110.3(9) . . ? H132 C24 H134 110.3(12) . . ? H133 C24 H134 109.8(12) . . ? C23 C25 H135 113.2(9) . . ? C23 C25 H136 113.5(9) . . ? H135 C25 H136 106.8(12) . . ? C23 C25 H137 110.1(9) . . ? H135 C25 H137 107.2(12) . . ? H136 C25 H137 105.5(13) . . ? C23 C26 H138 113.4(9) . . ? C23 C26 H139 113.5(8) . . ? H138 C26 H139 105.6(12) . . ? C23 C26 H140 107.7(8) . . ? H138 C26 H140 107.8(12) . . ? H139 C26 H140 108.6(11) . . ? C28 C27 C32 121.04(11) . . ? C28 C27 N6 120.13(10) . . ? C32 C27 N6 118.62(10) . . ? C29 C28 C27 118.00(11) . . ? C29 C28 C36 118.91(11) . . ? C27 C28 C36 123.06(11) . . ? C30 C29 C28 121.58(12) . . ? C30 C29 H141 117.9(8) . . ? C28 C29 H141 120.5(8) . . ? C29 C30 C31 119.48(12) . . ? C29 C30 H142 121.8(8) . . ? C31 C30 H142 118.6(8) . . ? C30 C31 C32 121.69(12) . . ? C30 C31 H143 119.6(8) . . ? C32 C31 H143 118.7(8) . . ? C31 C32 C27 117.89(11) . . ? C31 C32 C33 117.67(11) . . ? C27 C32 C33 124.39(11) . . ? C32 C33 C35 109.60(11) . . ? C32 C33 C34 113.15(11) . . ? C35 C33 C34 109.38(11) . . ? C32 C33 H144 109.3(8) . . ? C35 C33 H144 108.3(8) . . ? C34 C33 H144 107.0(8) . . ? C33 C34 H145 111.2(9) . . ? C33 C34 H146 110.8(9) . . ? H145 C34 H146 104.8(13) . . ? C33 C34 H147 112.0(9) . . ? H145 C34 H147 109.1(13) . . ? H146 C34 H147 108.7(13) . . ? C33 C35 H148 110.6(9) . . ? C33 C35 H149 111.5(8) . . ? H148 C35 H149 108.5(12) . . ? C33 C35 H150 110.0(9) . . ? H148 C35 H150 109.1(12) . . ? H149 C35 H150 107.1(12) . . ? C28 C36 C38 111.08(11) . . ? C28 C36 C37 112.43(11) . . ? C38 C36 C37 109.78(11) . . ? C28 C36 H151 106.6(8) . . ? C38 C36 H151 108.6(8) . . ? C37 C36 H151 108.2(8) . . ? C36 C37 H152 113.8(8) . . ? C36 C37 H153 109.7(9) . . ? H152 C37 H153 106.2(12) . . ? C36 C37 H154 110.6(9) . . ? H152 C37 H154 108.3(12) . . ? H153 C37 H154 108.0(12) . . ? C36 C38 H155 111.9(9) . . ? C36 C38 H156 110.9(9) . . ? H155 C38 H156 105.3(12) . . ? C36 C38 H157 112.4(8) . . ? H155 C38 H157 107.3(12) . . ? H156 C38 H157 108.8(12) . . ? C40 N39 Ti1 172.47(9) . . ? N39 C40 C41 120.84(11) . . ? N39 C40 C45 119.84(11) . . ? C41 C40 C45 119.31(11) . . ? C42 C41 C40 118.94(12) . . ? C42 C41 C49 120.17(12) . . ? C40 C41 C49 120.86(11) . . ? C43 C42 C41 121.66(14) . . ? C43 C42 H158 120.0(9) . . ? C41 C42 H158 118.3(9) . . ? C42 C43 C44 119.42(13) . . ? C42 C43 H159 121.4(9) . . ? C44 C43 H159 119.1(9) . . ? C43 C44 C45 121.71(13) . . ? C43 C44 H160 120.3(9) . . ? C45 C44 H160 118.0(9) . . ? C44 C45 C40 118.90(12) . . ? C44 C45 C46 120.67(12) . . ? C40 C45 C46 120.36(11) . . ? C45 C46 C48 114.08(11) . . ? C45 C46 C47 109.43(11) . . ? C48 C46 C47 110.97(12) . . ? C45 C46 H161 107.3(8) . . ? C48 C46 H161 107.4(8) . . ? C47 C46 H161 107.4(8) . . ? C46 C47 H162 113.1(9) . . ? C46 C47 H163 111.1(9) . . ? H162 C47 H163 106.0(12) . . ? C46 C47 H164 110.5(9) . . ? H162 C47 H164 107.6(12) . . ? H163 C47 H164 108.2(12) . . ? C46 C48 H165 112.2(9) . . ? C46 C48 H166 108.6(9) . . ? H165 C48 H166 108.4(13) . . ? C46 C48 H167 111.6(9) . . ? H165 C48 H167 108.0(13) . . ? H166 C48 H167 108.0(13) . . ? C41 C49 C50 110.97(12) . . ? C41 C49 C51 113.21(12) . . ? C50 C49 C51 110.75(12) . . ? C41 C49 H168 107.0(8) . . ? C50 C49 H168 107.2(8) . . ? C51 C49 H168 107.4(8) . . ? C49 C50 H169 112.4(9) . . ? C49 C50 H170 111.9(9) . . ? H169 C50 H170 107.8(12) . . ? C49 C50 H171 111.2(8) . . ? H169 C50 H171 106.4(12) . . ? H170 C50 H171 106.8(12) . . ? C49 C51 H172 110.3(9) . . ? C49 C51 H173 112.9(9) . . ? H172 C51 H173 105.8(12) . . ? C49 C51 H174 112.0(10) . . ? H172 C51 H174 105.8(13) . . ? H173 C51 H174 109.6(13) . . ? Ti1 C52 H175 111.4(14) . . ? Ti1 C52 H176 104.1(13) . . ? H175 C52 H176 112.6(18) . . ? Ti1 C52 H177 106.3(15) . . ? H175 C52 H177 112.4(18) . . ? H176 C52 H177 109.6(18) . . ? N91 Ti53 N58 112.14(5) . . ? N91 Ti53 N54 113.38(5) . . ? N58 Ti53 N54 97.38(4) . . ? N91 Ti53 C104 105.59(6) . . ? N58 Ti53 C104 114.22(5) . . ? N54 Ti53 C104 114.34(6) . . ? N91 Ti53 C57 142.88(5) . . ? N58 Ti53 C57 30.83(4) . . ? N54 Ti53 C57 83.87(4) . . ? C104 Ti53 C57 95.30(5) . . ? N91 Ti53 C55 143.02(5) . . ? N58 Ti53 C55 83.12(4) . . ? N54 Ti53 C55 29.64(4) . . ? C104 Ti53 C55 97.24(5) . . ? C57 Ti53 C55 59.98(4) . . ? N91 Ti53 C56 165.89(5) . . ? N58 Ti53 C56 59.80(4) . . ? N54 Ti53 C56 59.47(4) . . ? C104 Ti53 C56 88.51(5) . . ? C57 Ti53 C56 31.09(4) . . ? C55 Ti53 C56 31.16(4) . . ? C55 N54 C59 125.54(10) . . ? C55 N54 Ti53 101.25(8) . . ? C59 N54 Ti53 130.01(8) . . ? N54 C55 C56 119.75(11) . . ? N54 C55 C71 127.56(11) . . ? C56 C55 C71 112.37(11) . . ? N54 C55 Ti53 49.11(6) . . ? C56 C55 Ti53 74.52(7) . . ? C71 C55 Ti53 154.57(9) . . ? C57 C56 C55 135.77(12) . . ? C57 C56 Ti53 72.35(7) . . ? C55 C56 Ti53 74.31(7) . . ? C57 C56 H178 111.6(9) . . ? C55 C56 H178 112.4(9) . . ? Ti53 C56 H178 144.6(9) . . ? N58 C57 C56 120.40(11) . . ? N58 C57 C75 125.75(11) . . ? C56 C57 C75 113.41(11) . . ? N58 C57 Ti53 50.10(6) . . ? C56 C57 Ti53 76.57(7) . . ? C75 C57 Ti53 147.76(8) . . ? C57 N58 C79 123.91(10) . . ? C57 N58 Ti53 99.07(8) . . ? C79 N58 Ti53 135.54(8) . . ? C64 C59 C60 121.34(12) . . ? C64 C59 N54 119.42(12) . . ? C60 C59 N54 119.15(12) . . ? C61 C60 C59 117.31(15) . . ? C61 C60 C68 120.25(14) . . ? C59 C60 C68 122.43(12) . . ? C62 C61 C60 121.87(16) . . ? C62 C61 H179 120.0(10) . . ? C60 C61 H179 118.1(10) . . ? C61 C62 C63 120.08(15) . . ? C61 C62 H180 120.4(10) . . ? C63 C62 H180 119.5(10) . . ? C62 C63 C64 121.20(16) . . ? C62 C63 H181 122.6(10) . . ? C64 C63 H181 116.2(10) . . ? C63 C64 C59 117.86(15) . . ? C63 C64 C65 118.59(14) . . ? C59 C64 C65 123.54(12) . . ? C64 C65 C66 109.83(14) . . ? C64 C65 C67 113.55(14) . . ? C66 C65 C67 109.37(14) . . ? C64 C65 H182 109.2(8) . . ? C66 C65 H182 107.6(8) . . ? C67 C65 H182 107.0(8) . . ? C65 C66 H183 113.2(9) . . ? C65 C66 H184 109.6(10) . . ? H183 C66 H184 110.3(14) . . ? C65 C66 H185 107.7(10) . . ? H183 C66 H185 108.4(14) . . ? H184 C66 H185 107.4(14) . . ? C65 C67 H186 110.4(10) . . ? C65 C67 H187 113.8(10) . . ? H186 C67 H187 108.7(14) . . ? C65 C67 H188 111.6(10) . . ? H186 C67 H188 109.3(14) . . ? H187 C67 H188 102.6(14) . . ? C60 C68 C69 113.48(14) . . ? C60 C68 C70 113.30(14) . . ? C69 C68 C70 109.05(15) . . ? C60 C68 H189 107.9(10) . . ? C69 C68 H189 106.0(10) . . ? C70 C68 H189 106.7(10) . . ? C68 C69 H190 110.6(12) . . ? C68 C69 H191 112.3(11) . . ? H190 C69 H191 108.6(16) . . ? C68 C69 H192 103.0(8) . . ? H190 C69 H192 108.3(14) . . ? H191 C69 H192 113.9(13) . . ? C68 C70 H193 109.6(11) . . ? C68 C70 H194 108.3(11) . . ? H193 C70 H194 106.9(15) . . ? C68 C70 H195 108.2(11) . . ? H193 C70 H195 107.7(15) . . ? H194 C70 H195 116.0(15) . . ? C74 C71 C73 106.41(12) . . ? C74 C71 C72 108.03(12) . . ? C73 C71 C72 109.05(12) . . ? C74 C71 C55 116.66(11) . . ? C73 C71 C55 110.10(11) . . ? C72 C71 C55 106.42(11) . . ? C71 C72 H196 109.5(9) . . ? C71 C72 H197 114.1(9) . . ? H196 C72 H197 104.8(13) . . ? C71 C72 H198 110.7(9) . . ? H196 C72 H198 109.5(13) . . ? H197 C72 H198 108.0(13) . . ? C71 C73 H199 108.4(10) . . ? C71 C73 H200 114.8(10) . . ? H199 C73 H200 107.7(13) . . ? C71 C73 H201 110.6(10) . . ? H199 C73 H201 108.3(14) . . ? H200 C73 H201 106.9(14) . . ? C71 C74 H202 114.5(9) . . ? C71 C74 H203 107.1(9) . . ? H202 C74 H203 107.8(13) . . ? C71 C74 H204 115.6(9) . . ? H202 C74 H204 107.6(13) . . ? H203 C74 H204 103.3(13) . . ? C78 C75 C76 106.84(13) . . ? C78 C75 C77 107.20(13) . . ? C76 C75 C77 109.19(16) . . ? C78 C75 C57 116.99(11) . . ? C76 C75 C57 110.77(12) . . ? C77 C75 C57 105.62(11) . . ? C75 C76 H205 110.5(12) . . ? C75 C76 H206 110.6(11) . . ? H205 C76 H206 110.0(16) . . ? C75 C76 H207 113.2(11) . . ? H205 C76 H207 107.7(16) . . ? H206 C76 H207 104.7(15) . . ? C75 C77 H208 111.9(14) . . ? C75 C77 H209 111.2(10) . . ? H208 C77 H209 110.3(17) . . ? C75 C77 H210 109.9(10) . . ? H208 C77 H210 106.2(17) . . ? H209 C77 H210 107.2(14) . . ? C75 C78 H211 107.3(9) . . ? C75 C78 H212 112.2(9) . . ? H211 C78 H212 109.9(12) . . ? C75 C78 H213 113.4(9) . . ? H211 C78 H213 108.3(13) . . ? H212 C78 H213 105.8(13) . . ? C80 C79 C84 120.63(12) . . ? C80 C79 N58 118.89(11) . . ? C84 C79 N58 120.44(11) . . ? C81 C80 C79 118.31(13) . . ? C81 C80 C88 118.45(13) . . ? C79 C80 C88 123.21(12) . . ? C82 C81 C80 121.58(14) . . ? C82 C81 H214 118.9(10) . . ? C80 C81 H214 119.5(10) . . ? C81 C82 C83 119.35(14) . . ? C81 C82 H215 121.6(10) . . ? C83 C82 H215 119.0(10) . . ? C82 C83 C84 121.93(14) . . ? C82 C83 H216 119.8(10) . . ? C84 C83 H216 118.3(10) . . ? C83 C84 C79 118.03(13) . . ? C83 C84 C85 117.90(13) . . ? C79 C84 C85 124.07(12) . . ? C84 C85 C86 111.01(14) . . ? C84 C85 C87 112.49(17) . . ? C86 C85 C87 109.87(14) . . ? C84 C85 H217 107.9(10) . . ? C86 C85 H217 109.4(10) . . ? C87 C85 H217 106.0(10) . . ? C85 C86 H218 108.7(11) . . ? C85 C86 H219 112.6(11) . . ? H218 C86 H219 110.0(15) . . ? C85 C86 H220 112.4(10) . . ? H218 C86 H220 104.4(14) . . ? H219 C86 H220 108.4(15) . . ? C85 C87 H221 111.1(14) . . ? C85 C87 H222 111.0(12) . . ? H221 C87 H222 108.5(18) . . ? C85 C87 H223 115.6(13) . . ? H221 C87 H223 108.2(19) . . ? H222 C87 H223 101.9(19) . . ? C80 C88 C90 109.92(13) . . ? C80 C88 C89 112.46(15) . . ? C90 C88 C89 108.88(14) . . ? C80 C88 H224 109.9(9) . . ? C90 C88 H224 107.2(9) . . ? C89 C88 H224 108.3(9) . . ? C88 C89 H225 113.9(12) . . ? C88 C89 H226 106.7(12) . . ? H225 C89 H226 106.9(17) . . ? C88 C89 H227 107.5(18) . . ? H225 C89 H227 113(2) . . ? H226 C89 H227 108(2) . . ? C88 C90 H228 113.2(10) . . ? C88 C90 H229 110.4(11) . . ? H228 C90 H229 106.6(14) . . ? C88 C90 H230 112.1(10) . . ? H228 C90 H230 105.2(13) . . ? H229 C90 H230 109.0(14) . . ? C92 N91 Ti53 174.47(9) . . ? N91 C92 C223 119.58(11) . . ? N91 C92 C97 121.05(11) . . ? C223 C92 C97 119.33(12) . . ? C95 C94 C223 121.38(14) . . ? C95 C94 H231 119.7(9) . . ? C223 C94 H231 119.0(9) . . ? C96 C95 C94 119.60(13) . . ? C96 C95 H232 120.2(10) . . ? C94 C95 H232 120.2(10) . . ? C95 C96 C97 121.93(14) . . ? C95 C96 H233 120.5(9) . . ? C97 C96 H233 117.6(9) . . ? C96 C97 C92 118.46(13) . . ? C96 C97 C98 120.19(12) . . ? C92 C97 C98 121.29(12) . . ? C97 C98 C99 112.92(13) . . ? C97 C98 C100 110.55(13) . . ? C99 C98 C100 110.36(15) . . ? C97 C98 H234 109.0(8) . . ? C99 C98 H234 108.5(8) . . ? C100 C98 H234 105.3(9) . . ? C98 C99 H235 110.1(11) . . ? C98 C99 H236 107.5(11) . . ? H235 C99 H236 107.5(15) . . ? C98 C99 H237 111.4(11) . . ? H235 C99 H237 108.7(16) . . ? H236 C99 H237 111.5(16) . . ? C98 C100 H238 110.9(11) . . ? C98 C100 H239 110.7(10) . . ? H238 C100 H239 109.1(15) . . ? C98 C100 H240 111.0(11) . . ? H238 C100 H240 109.4(15) . . ? H239 C100 H240 105.5(15) . . ? C223 C101 C102 110.30(12) . . ? C223 C101 C103 112.97(13) . . ? C102 C101 C103 110.87(13) . . ? C223 C101 H241 107.0(8) . . ? C102 C101 H241 108.6(8) . . ? C103 C101 H241 106.9(8) . . ? C101 C102 H242 108.3(9) . . ? C101 C102 H243 108.7(9) . . ? H242 C102 H243 112.5(13) . . ? C101 C102 H244 109.4(9) . . ? H242 C102 H244 110.5(13) . . ? H243 C102 H244 107.5(13) . . ? C101 C103 H245 109.6(10) . . ? C101 C103 H246 111.5(10) . . ? H245 C103 H246 105.8(14) . . ? C101 C103 H247 113.2(10) . . ? H245 C103 H247 108.7(14) . . ? H246 C103 H247 107.8(14) . . ? Ti53 C104 H248 109.8(13) . . ? Ti53 C104 H249 111.3(12) . . ? H248 C104 H249 109.2(17) . . ? Ti53 C104 H250 112.1(11) . . ? H248 C104 H250 105.3(16) . . ? H249 C104 H250 108.9(15) . . ? C94 C223 C92 119.23(13) . . ? C94 C223 C101 119.90(12) . . ? C92 C223 C101 120.86(12) . . ? C1S C2S O3S 127.4(8) . . ? C1S C2S H2S1 105.4 . . ? O3S C2S H2S1 105.5 . . ? C1S C2S H2S2 105.5 . . ? O3S C2S H2S2 105.4 . . ? H2S1 C2S H2S2 106.0 . . ? C4S O3S O3S 111.4(15) 2_755 2_755 ? C4S O3S C4S 143.5(9) 2_755 . ? O3S O3S C4S 32.1(8) 2_755 . ? C4S O3S C2S 23.9(14) 2_755 . ? O3S O3S C2S 101.5(11) 2_755 . ? C4S O3S C2S 130.4(6) . . ? C4S O3S C2S 152.6(15) 2_755 2_755 ? O3S O3S C2S 49.1(8) 2_755 2_755 ? C4S O3S C2S 22.4(5) . 2_755 ? C2S O3S C2S 150.6(5) . 2_755 ? C4S O3S C5S 17.2(12) 2_755 2_755 ? O3S O3S C5S 104.5(10) 2_755 2_755 ? C4S O3S C5S 134.8(6) . 2_755 ? C2S O3S C5S 6.7(8) . 2_755 ? C2S O3S C5S 153.1(7) 2_755 2_755 ? C5S C4S O3S 128.2(10) . . ? C5S C4S C4S 138.7(12) . 2_755 ? O3S C4S C4S 13.1(4) . 2_755 ? C5S C4S H4S1 105.3 . . ? O3S C4S H4S1 105.2 . . ? C4S C4S H4S1 93.1 2_755 . ? C5S C4S H4S2 105.2 . . ? O3S C4S H4S2 105.3 . . ? C4S C4S H4S2 104.6 2_755 . ? H4S1 C4S H4S2 106.0 . . ? 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 N39 Ti1 N2 C3 170.99(7) . . . . ? N6 Ti1 N2 C3 55.61(8) . . . . ? C52 Ti1 N2 C3 -62.90(9) . . . . ? N39 Ti1 N2 C7 -15.48(12) . . . . ? N6 Ti1 N2 C7 -130.85(10) . . . . ? C52 Ti1 N2 C7 110.63(11) . . . . ? C3 Ti1 N2 C7 173.53(15) . . . . ? C7 N2 C3 C4 146.96(12) . . . . ? Ti1 N2 C3 C4 -38.95(13) . . . . ? C7 N2 C3 C19 -41.12(17) . . . . ? Ti1 N2 C3 C19 132.96(10) . . . . ? C7 N2 C3 Ti1 -174.08(14) . . . . ? N39 Ti1 C3 N2 -14.00(11) . . . . ? N6 Ti1 C3 N2 -124.69(8) . . . . ? C52 Ti1 C3 N2 123.30(8) . . . . ? N39 Ti1 C3 C4 133.00(9) . . . . ? N2 Ti1 C3 C4 147.00(11) . . . . ? N6 Ti1 C3 C4 22.31(7) . . . . ? C52 Ti1 C3 C4 -89.70(8) . . . . ? N39 Ti1 C3 C19 -104.37(14) . . . . ? N2 Ti1 C3 C19 -90.37(15) . . . . ? N6 Ti1 C3 C19 144.93(13) . . . . ? C52 Ti1 C3 C19 32.93(14) . . . . ? N2 C3 C4 C5 -9.4(2) . . . . ? C19 C3 C4 C5 178.10(13) . . . . ? Ti1 C3 C4 C5 -36.93(15) . . . . ? C3 C4 C5 N6 33.8(2) . . . . ? C3 C4 C5 C23 -146.16(14) . . . . ? C4 C5 N6 C27 167.53(11) . . . . ? C23 C5 N6 C27 -12.56(19) . . . . ? C4 C5 N6 Ti1 2.47(13) . . . . ? C23 C5 N6 Ti1 -177.63(10) . . . . ? N39 Ti1 N6 C5 -158.57(8) . . . . ? N2 Ti1 N6 C5 -38.81(8) . . . . ? C52 Ti1 N6 C5 78.47(9) . . . . ? C3 Ti1 N6 C5 -14.15(8) . . . . ? N39 Ti1 N6 C27 36.05(10) . . . . ? N2 Ti1 N6 C27 155.81(9) . . . . ? C52 Ti1 N6 C27 -86.92(10) . . . . ? C3 Ti1 N6 C27 -179.53(9) . . . . ? C3 N2 C7 C12 117.85(13) . . . . ? Ti1 N2 C7 C12 -54.46(15) . . . . ? C3 N2 C7 C8 -65.99(15) . . . . ? Ti1 N2 C7 C8 121.70(11) . . . . ? C12 C7 C8 C9 5.03(18) . . . . ? N2 C7 C8 C9 -171.12(11) . . . . ? C12 C7 C8 C16 -174.54(11) . . . . ? N2 C7 C8 C16 9.31(17) . . . . ? C7 C8 C9 C10 -2.09(19) . . . . ? C16 C8 C9 C10 177.50(12) . . . . ? C8 C9 C10 C11 -1.6(2) . . . . ? C9 C10 C11 C12 2.5(2) . . . . ? C10 C11 C12 C7 0.39(19) . . . . ? C10 C11 C12 C13 -174.74(13) . . . . ? C8 C7 C12 C11 -4.20(18) . . . . ? N2 C7 C12 C11 171.90(11) . . . . ? C8 C7 C12 C13 170.65(12) . . . . ? N2 C7 C12 C13 -13.25(18) . . . . ? C11 C12 C13 C15 -63.72(16) . . . . ? C7 C12 C13 C15 121.43(14) . . . . ? C11 C12 C13 C14 60.16(16) . . . . ? C7 C12 C13 C14 -114.69(14) . . . . ? C9 C8 C16 C18 96.34(15) . . . . ? C7 C8 C16 C18 -84.10(15) . . . . ? C9 C8 C16 C17 -28.69(17) . . . . ? C7 C8 C16 C17 150.87(12) . . . . ? N2 C3 C19 C21 159.14(14) . . . . ? C4 C3 C19 C21 -28.56(17) . . . . ? Ti1 C3 C19 C21 -140.69(14) . . . . ? N2 C3 C19 C20 36.64(17) . . . . ? C4 C3 C19 C20 -151.07(12) . . . . ? Ti1 C3 C19 C20 96.80(15) . . . . ? N2 C3 C19 C22 -82.49(15) . . . . ? C4 C3 C19 C22 89.81(14) . . . . ? Ti1 C3 C19 C22 -22.32(18) . . . . ? N6 C5 C23 C26 -3.41(18) . . . . ? C4 C5 C23 C26 176.50(11) . . . . ? N6 C5 C23 C24 120.01(13) . . . . ? C4 C5 C23 C24 -60.08(13) . . . . ? N6 C5 C23 C25 -122.43(13) . . . . ? C4 C5 C23 C25 57.48(14) . . . . ? C5 N6 C27 C28 112.16(13) . . . . ? Ti1 N6 C27 C28 -84.67(12) . . . . ? C5 N6 C27 C32 -73.07(15) . . . . ? Ti1 N6 C27 C32 90.10(12) . . . . ? C32 C27 C28 C29 6.56(18) . . . . ? N6 C27 C28 C29 -178.80(11) . . . . ? C32 C27 C28 C36 -175.61(11) . . . . ? N6 C27 C28 C36 -0.98(18) . . . . ? C27 C28 C29 C30 -3.41(19) . . . . ? C36 C28 C29 C30 178.67(12) . . . . ? C28 C29 C30 C31 -1.6(2) . . . . ? C29 C30 C31 C32 3.6(2) . . . . ? C30 C31 C32 C27 -0.51(19) . . . . ? C30 C31 C32 C33 -178.01(12) . . . . ? C28 C27 C32 C31 -4.65(18) . . . . ? N6 C27 C32 C31 -179.36(11) . . . . ? C28 C27 C32 C33 172.67(12) . . . . ? N6 C27 C32 C33 -2.05(18) . . . . ? C31 C32 C33 C35 72.27(15) . . . . ? C27 C32 C33 C35 -105.04(14) . . . . ? C31 C32 C33 C34 -50.10(16) . . . . ? C27 C32 C33 C34 132.58(13) . . . . ? C29 C28 C36 C38 80.48(15) . . . . ? C27 C28 C36 C38 -97.33(14) . . . . ? C29 C28 C36 C37 -42.99(16) . . . . ? C27 C28 C36 C37 139.20(13) . . . . ? N2 Ti1 N39 C40 -156.7(7) . . . . ? N6 Ti1 N39 C40 -46.8(7) . . . . ? C52 Ti1 N39 C40 77.2(7) . . . . ? C3 Ti1 N39 C40 -149.1(7) . . . . ? Ti1 N39 C40 C41 159.5(6) . . . . ? Ti1 N39 C40 C45 -19.3(8) . . . . ? N39 C40 C41 C42 -176.25(12) . . . . ? C45 C40 C41 C42 2.52(19) . . . . ? N39 C40 C41 C49 1.82(19) . . . . ? C45 C40 C41 C49 -179.41(12) . . . . ? C40 C41 C42 C43 -1.1(2) . . . . ? C49 C41 C42 C43 -179.21(14) . . . . ? C41 C42 C43 C44 -1.0(2) . . . . ? C42 C43 C44 C45 1.7(2) . . . . ? C43 C44 C45 C40 -0.3(2) . . . . ? C43 C44 C45 C46 -177.41(13) . . . . ? N39 C40 C45 C44 176.96(12) . . . . ? C41 C40 C45 C44 -1.83(18) . . . . ? N39 C40 C45 C46 -5.93(18) . . . . ? C41 C40 C45 C46 175.29(11) . . . . ? C44 C45 C46 C48 -33.50(18) . . . . ? C40 C45 C46 C48 149.43(12) . . . . ? C44 C45 C46 C47 91.47(15) . . . . ? C40 C45 C46 C47 -85.59(14) . . . . ? C42 C41 C49 C50 87.59(16) . . . . ? C40 C41 C49 C50 -90.45(15) . . . . ? C42 C41 C49 C51 -37.65(18) . . . . ? C40 C41 C49 C51 144.30(13) . . . . ? N91 Ti53 N54 C55 179.88(8) . . . . ? N58 Ti53 N54 C55 61.84(8) . . . . ? C104 Ti53 N54 C55 -58.99(9) . . . . ? C57 Ti53 N54 C55 34.06(8) . . . . ? C56 Ti53 N54 C55 13.55(7) . . . . ? N91 Ti53 N54 C59 -19.92(12) . . . . ? N58 Ti53 N54 C59 -137.96(11) . . . . ? C104 Ti53 N54 C59 101.20(12) . . . . ? C57 Ti53 N54 C59 -165.74(11) . . . . ? C55 Ti53 N54 C59 160.19(16) . . . . ? C56 Ti53 N54 C59 173.74(12) . . . . ? C59 N54 C55 C56 172.95(12) . . . . ? Ti53 N54 C55 C56 -25.65(13) . . . . ? C59 N54 C55 C71 -14.1(2) . . . . ? Ti53 N54 C55 C71 147.26(11) . . . . ? C59 N54 C55 Ti53 -161.40(15) . . . . ? N91 Ti53 C55 N54 -0.18(12) . . . . ? N58 Ti53 C55 N54 -118.27(8) . . . . ? C104 Ti53 C55 N54 128.08(9) . . . . ? C57 Ti53 C55 N54 -139.97(9) . . . . ? C56 Ti53 C55 N54 -157.05(12) . . . . ? N91 Ti53 C55 C56 156.87(8) . . . . ? N58 Ti53 C55 C56 38.77(7) . . . . ? N54 Ti53 C55 C56 157.05(12) . . . . ? C104 Ti53 C55 C56 -74.88(8) . . . . ? C57 Ti53 C55 C56 17.08(7) . . . . ? N91 Ti53 C55 C71 -93.4(2) . . . . ? N58 Ti53 C55 C71 148.5(2) . . . . ? N54 Ti53 C55 C71 -93.2(2) . . . . ? C104 Ti53 C55 C71 34.8(2) . . . . ? C57 Ti53 C55 C71 126.8(2) . . . . ? C56 Ti53 C55 C71 109.7(2) . . . . ? N54 C55 C56 C57 -22.4(2) . . . . ? C71 C55 C56 C57 163.65(14) . . . . ? Ti53 C55 C56 C57 -42.27(15) . . . . ? N54 C55 C56 Ti53 19.85(10) . . . . ? C71 C55 C56 Ti53 -154.08(10) . . . . ? N91 Ti53 C56 C57 74.7(2) . . . . ? N58 Ti53 C56 C57 16.50(7) . . . . ? N54 Ti53 C56 C57 137.56(9) . . . . ? C104 Ti53 C56 C57 -102.83(8) . . . . ? C55 Ti53 C56 C57 150.50(12) . . . . ? N91 Ti53 C56 C55 -75.8(2) . . . . ? N58 Ti53 C56 C55 -134.00(8) . . . . ? N54 Ti53 C56 C55 -12.94(7) . . . . ? C104 Ti53 C56 C55 106.67(8) . . . . ? C57 Ti53 C56 C55 -150.50(12) . . . . ? C55 C56 C57 N58 17.6(2) . . . . ? Ti53 C56 C57 N58 -25.21(10) . . . . ? C55 C56 C57 C75 -169.60(14) . . . . ? Ti53 C56 C57 C75 147.59(10) . . . . ? C55 C56 C57 Ti53 42.81(15) . . . . ? N91 Ti53 C57 N58 -5.68(11) . . . . ? N54 Ti53 C57 N58 115.61(8) . . . . ? C104 Ti53 C57 N58 -130.41(8) . . . . ? C55 Ti53 C57 N58 134.27(8) . . . . ? C56 Ti53 C57 N58 151.38(12) . . . . ? N91 Ti53 C57 C56 -157.07(8) . . . . ? N58 Ti53 C57 C56 -151.38(12) . . . . ? N54 Ti53 C57 C56 -35.78(7) . . . . ? C104 Ti53 C57 C56 78.20(8) . . . . ? C55 Ti53 C57 C56 -17.12(7) . . . . ? N91 Ti53 C57 C75 90.16(17) . . . . ? N58 Ti53 C57 C75 95.84(18) . . . . ? N54 Ti53 C57 C75 -148.55(16) . . . . ? C104 Ti53 C57 C75 -34.57(17) . . . . ? C55 Ti53 C57 C75 -129.89(17) . . . . ? C56 Ti53 C57 C75 -112.77(18) . . . . ? C56 C57 N58 C79 -159.29(11) . . . . ? C75 C57 N58 C79 28.85(18) . . . . ? Ti53 C57 N58 C79 168.02(13) . . . . ? C56 C57 N58 Ti53 32.69(12) . . . . ? C75 C57 N58 Ti53 -139.16(11) . . . . ? N91 Ti53 N58 C57 176.30(7) . . . . ? N54 Ti53 N58 C57 -64.70(8) . . . . ? C104 Ti53 N58 C57 56.23(9) . . . . ? C55 Ti53 N58 C57 -38.65(7) . . . . ? C56 Ti53 N58 C57 -16.63(7) . . . . ? N91 Ti53 N58 C79 10.54(13) . . . . ? N54 Ti53 N58 C79 129.54(11) . . . . ? C104 Ti53 N58 C79 -109.53(12) . . . . ? C57 Ti53 N58 C79 -165.76(16) . . . . ? C55 Ti53 N58 C79 155.59(12) . . . . ? C56 Ti53 N58 C79 177.61(13) . . . . ? C55 N54 C59 C64 94.01(16) . . . . ? Ti53 N54 C59 C64 -61.88(16) . . . . ? C55 N54 C59 C60 -89.37(16) . . . . ? Ti53 N54 C59 C60 114.74(12) . . . . ? C64 C59 C60 C61 -6.50(19) . . . . ? N54 C59 C60 C61 176.96(12) . . . . ? C64 C59 C60 C68 172.56(13) . . . . ? N54 C59 C60 C68 -3.99(19) . . . . ? C59 C60 C61 C62 2.7(2) . . . . ? C68 C60 C61 C62 -176.33(14) . . . . ? C60 C61 C62 C63 2.1(2) . . . . ? C61 C62 C63 C64 -3.3(2) . . . . ? C62 C63 C64 C59 -0.4(2) . . . . ? C62 C63 C64 C65 178.92(14) . . . . ? C60 C59 C64 C63 5.37(19) . . . . ? N54 C59 C64 C63 -178.09(12) . . . . ? C60 C59 C64 C65 -173.90(13) . . . . ? N54 C59 C64 C65 2.64(19) . . . . ? C63 C64 C65 C66 -64.72(17) . . . . ? C59 C64 C65 C66 114.55(15) . . . . ? C63 C64 C65 C67 58.09(18) . . . . ? C59 C64 C65 C67 -122.64(15) . . . . ? C61 C60 C68 C69 -100.68(17) . . . . ? C59 C60 C68 C69 80.29(18) . . . . ? C61 C60 C68 C70 24.4(2) . . . . ? C59 C60 C68 C70 -154.65(14) . . . . ? N54 C55 C71 C74 14.8(2) . . . . ? C56 C55 C71 C74 -171.89(13) . . . . ? Ti53 C55 C71 C74 87.0(2) . . . . ? N54 C55 C71 C73 136.12(14) . . . . ? C56 C55 C71 C73 -50.54(15) . . . . ? Ti53 C55 C71 C73 -151.69(17) . . . . ? N54 C55 C71 C72 -105.84(15) . . . . ? C56 C55 C71 C72 67.51(14) . . . . ? Ti53 C55 C71 C72 -33.6(2) . . . . ? N58 C57 C75 C78 -17.75(19) . . . . ? C56 C57 C75 C78 169.90(12) . . . . ? Ti53 C57 C75 C78 -87.86(19) . . . . ? N58 C57 C75 C76 -140.50(15) . . . . ? C56 C57 C75 C76 47.15(17) . . . . ? Ti53 C57 C75 C76 149.39(16) . . . . ? N58 C57 C75 C77 101.39(15) . . . . ? C56 C57 C75 C77 -70.96(15) . . . . ? Ti53 C57 C75 C77 31.3(2) . . . . ? C57 N58 C79 C80 70.15(16) . . . . ? Ti53 N58 C79 C80 -126.87(12) . . . . ? C57 N58 C79 C84 -112.17(14) . . . . ? Ti53 N58 C79 C84 50.81(17) . . . . ? C84 C79 C80 C81 4.2(2) . . . . ? N58 C79 C80 C81 -178.11(12) . . . . ? C84 C79 C80 C88 -173.91(13) . . . . ? N58 C79 C80 C88 3.77(19) . . . . ? C79 C80 C81 C82 -0.9(2) . . . . ? C88 C80 C81 C82 177.27(14) . . . . ? C80 C81 C82 C83 -1.9(2) . . . . ? C81 C82 C83 C84 1.6(2) . . . . ? C82 C83 C84 C79 1.6(2) . . . . ? C82 C83 C84 C85 -179.50(15) . . . . ? C80 C79 C84 C83 -4.51(19) . . . . ? N58 C79 C84 C83 177.85(12) . . . . ? C80 C79 C84 C85 176.64(14) . . . . ? N58 C79 C84 C85 -1.0(2) . . . . ? C83 C84 C85 C86 52.78(19) . . . . ? C79 C84 C85 C86 -128.36(15) . . . . ? C83 C84 C85 C87 -70.8(2) . . . . ? C79 C84 C85 C87 108.06(18) . . . . ? C81 C80 C88 C90 -61.16(18) . . . . ? C79 C80 C88 C90 116.95(15) . . . . ? C81 C80 C88 C89 60.3(2) . . . . ? C79 C80 C88 C89 -121.57(17) . . . . ? N58 Ti53 N91 C92 -35.4(10) . . . . ? N54 Ti53 N91 C92 -144.5(10) . . . . ? C104 Ti53 N91 C92 89.6(10) . . . . ? C57 Ti53 N91 C92 -32.2(10) . . . . ? C55 Ti53 N91 C92 -144.4(9) . . . . ? C56 Ti53 N91 C92 -87.9(10) . . . . ? Ti53 N91 C92 C223 73.2(10) . . . . ? Ti53 N91 C92 C97 -104.6(9) . . . . ? C223 C94 C95 C96 1.5(2) . . . . ? C94 C95 C96 C97 -0.6(2) . . . . ? C95 C96 C97 C92 -1.6(2) . . . . ? C95 C96 C97 C98 175.61(13) . . . . ? N91 C92 C97 C96 -179.32(12) . . . . ? C223 C92 C97 C96 2.87(18) . . . . ? N91 C92 C97 C98 3.54(19) . . . . ? C223 C92 C97 C98 -174.26(12) . . . . ? C96 C97 C98 C99 43.36(19) . . . . ? C92 C97 C98 C99 -139.55(14) . . . . ? C96 C97 C98 C100 -80.83(18) . . . . ? C92 C97 C98 C100 96.25(16) . . . . ? C95 C94 C223 C92 -0.1(2) . . . . ? C95 C94 C223 C101 179.24(13) . . . . ? N91 C92 C223 C94 -179.90(12) . . . . ? C97 C92 C223 C94 -2.06(19) . . . . ? N91 C92 C223 C101 0.73(18) . . . . ? C97 C92 C223 C101 178.57(12) . . . . ? C102 C101 C223 C94 -76.55(17) . . . . ? C103 C101 C223 C94 48.15(18) . . . . ? C102 C101 C223 C92 102.82(15) . . . . ? C103 C101 C223 C92 -132.48(14) . . . . ? C1S C2S O3S C4S 46(3) . . . 2_755 ? C1S C2S O3S O3S 163.1(16) . . . 2_755 ? C1S C2S O3S C4S 178.8(10) . . . . ? C1S C2S O3S C2S 163.1(17) . . . 2_755 ? C1S C2S O3S C5S 46(7) . . . 2_755 ? C4S O3S C4S C5S -147(3) 2_755 . . . ? O3S O3S C4S C5S -147(3) 2_755 . . . ? C2S O3S C4S C5S -177.0(17) . . . . ? C2S O3S C4S C5S -17.3(19) 2_755 . . . ? C5S O3S C4S C5S -170.1(10) 2_755 . . . ? O3S O3S C4S C4S 0.000(8) 2_755 . . 2_755 ? C2S O3S C4S C4S -30(2) . . . 2_755 ? C2S O3S C4S C4S 130(4) 2_755 . . 2_755 ? C5S O3S C4S C4S -23(2) 2_755 . . 2_755 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 33.18 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.457 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.055 data_04337 _database_code_depnum_ccdc_archive 'CCDC 260837' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H73 B F15 N3 Ti, C6 H5 F' _chemical_formula_sum 'C72 H78 B F16 N3 Ti' _chemical_formula_weight 1348.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' _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 13.3722(14) _cell_length_b 14.0266(14) _cell_length_c 17.6246(18) _cell_angle_alpha 79.495(3) _cell_angle_beta 88.114(3) _cell_angle_gamma 86.204(3) _cell_volume 3242.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 128(2) _cell_measurement_reflns_used 1002 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 25.32 _exptl_crystal_description prism _exptl_crystal_colour orange/red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1404 _exptl_absorpt_coefficient_mu 0.224 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; _diffrn_ambient_temperature 128(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details ' 0.30 degree frames measured for 10.17 seconds each' _diffrn_measurement_method '\w scans' _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 109449 _diffrn_reflns_av_R_equivalents 0.0624 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 33.16 _reflns_number_total 24759 _reflns_number_gt 16524 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999), XTEL (local program)' _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. Large residuals near C91 and C92 in the fluorobenzene indicated that the F is disordered over three sites. Partial occupancy F atoms were placed and allowed to vary without constraints at the three sites, with the total F occupancy converging to 1.11. The excess is due to the fact that no partial occupancy hydrogen atoms were included at the three sites. ; _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^)+(0.0431P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 24759 _refine_ls_number_parameters 1163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0654 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0941 _refine_ls_wR_factor_gt 0.0859 _refine_ls_goodness_of_fit_ref 0.905 _refine_ls_restrained_S_all 0.905 _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 0.782228(13) 0.160527(13) 0.239771(10) 0.01199(4) Uani 1 1 d . . . H107 H 0.4355(13) -0.0698(12) 0.2078(11) 0.052(5) Uiso 1 1 d . . . H143 H 0.8500(12) -0.1207(12) 0.0999(10) 0.043(4) Uiso 1 1 d . . . H157 H 1.0082(13) 0.1641(12) 0.0601(10) 0.049(5) Uiso 1 1 d . . . H159 H 0.8425(11) -0.2308(11) 0.2999(9) 0.036(4) Uiso 1 1 d . . . H160 H 0.9525(15) -0.2314(14) 0.2574(11) 0.067(6) Uiso 1 1 d . . . H161 H 0.8626(14) -0.1515(13) 0.2256(11) 0.058(5) Uiso 1 1 d . . . H170 H 0.4416(16) 0.4993(15) 0.2043(12) 0.075(6) Uiso 1 1 d . . . H122 H 0.4629(11) 0.3692(11) 0.0290(9) 0.035(4) Uiso 1 1 d . . . H147 H 0.6329(13) 0.0099(12) 0.0091(9) 0.046(5) Uiso 1 1 d . . . N2 N 0.67575(6) 0.08430(6) 0.29556(5) 0.01323(16) Uani 1 1 d . . . C3 C 0.59246(7) 0.14804(7) 0.28323(6) 0.01392(18) Uani 1 1 d . . . C4 C 0.58099(7) 0.20984(8) 0.21271(6) 0.01532(19) Uani 1 1 d . . . C5 C 0.62609(8) 0.21203(7) 0.13631(6) 0.01506(19) Uani 1 1 d . . . N6 N 0.72265(6) 0.18764(6) 0.12973(5) 0.01402(16) Uani 1 1 d . . . C7 C 0.67736(7) -0.00863(7) 0.34724(6) 0.01488(19) Uani 1 1 d . . . C8 C 0.63402(8) -0.08629(8) 0.32295(7) 0.0184(2) Uani 1 1 d . . . C9 C 0.63808(9) -0.17654(8) 0.37237(7) 0.0234(2) Uani 1 1 d . . . C10 C 0.68596(9) -0.19026(8) 0.44217(7) 0.0247(2) Uani 1 1 d . . . C11 C 0.72914(8) -0.11347(8) 0.46458(7) 0.0211(2) Uani 1 1 d . . . C12 C 0.72539(7) -0.02118(8) 0.41873(6) 0.01632(19) Uani 1 1 d . . . C13 C 0.76997(8) 0.06076(8) 0.44988(6) 0.0176(2) Uani 1 1 d . . . C14 C 0.73824(11) 0.06290(10) 0.53411(7) 0.0287(3) Uani 1 1 d . . . C15 C 0.88470(9) 0.05536(10) 0.44395(8) 0.0245(2) Uani 1 1 d . . . C16 C 0.58207(9) -0.07661(9) 0.24610(7) 0.0231(2) Uani 1 1 d . . . C17 C 0.46836(10) -0.07559(15) 0.25669(11) 0.0420(4) Uani 1 1 d . . . C18 C 0.61737(11) -0.15743(11) 0.20216(9) 0.0318(3) Uani 1 1 d . . . C19 C 0.51216(8) 0.16568(8) 0.34654(6) 0.0179(2) Uani 1 1 d . . . C20 C 0.50405(10) 0.08209(10) 0.41504(8) 0.0268(3) Uani 1 1 d . . . C21 C 0.40650(9) 0.18662(13) 0.31308(9) 0.0359(3) Uani 1 1 d . . . C22 C 0.54163(12) 0.25489(10) 0.37768(9) 0.0330(3) Uani 1 1 d . . . C23 C 0.54804(8) 0.24350(9) 0.07136(6) 0.0216(2) Uani 1 1 d . . . C24 C 0.50492(12) 0.34805(11) 0.07420(8) 0.0328(3) Uani 1 1 d . . . C25 C 0.46324(10) 0.17268(12) 0.09022(9) 0.0338(3) Uani 1 1 d . . . C26 C 0.58301(10) 0.23949(10) -0.01185(7) 0.0267(3) Uani 1 1 d . . . C27 C 0.77714(8) 0.19541(8) 0.05597(6) 0.01577(19) Uani 1 1 d . . . C28 C 0.80040(8) 0.11118(8) 0.02492(6) 0.0184(2) Uani 1 1 d . . . C29 C 0.85077(9) 0.12026(9) -0.04641(7) 0.0222(2) Uani 1 1 d . . . C30 C 0.87918(9) 0.20898(10) -0.08529(7) 0.0257(2) Uani 1 1 d . . . C31 C 0.85863(10) 0.29049(9) -0.05280(7) 0.0254(2) Uani 1 1 d . . . C32 C 0.80764(8) 0.28625(8) 0.01812(6) 0.0197(2) Uani 1 1 d . . . C33 C 0.78899(10) 0.38134(8) 0.04791(7) 0.0240(2) Uani 1 1 d . . . C34 C 0.73697(13) 0.46130(10) -0.01194(8) 0.0340(3) Uani 1 1 d . . . C35 C 0.88808(11) 0.41694(10) 0.06951(8) 0.0301(3) Uani 1 1 d . . . C36 C 0.77270(10) 0.01065(8) 0.06347(7) 0.0240(2) Uani 1 1 d . . . C37 C 0.86775(12) -0.05605(10) 0.07728(9) 0.0338(3) Uani 1 1 d . . . C38 C 0.69922(11) -0.03045(10) 0.01462(9) 0.0321(3) Uani 1 1 d . . . N39 N 0.89225(6) 0.08989(7) 0.23975(5) 0.01596(17) Uani 1 1 d . . . C40 C 0.98908(7) 0.04409(8) 0.24058(6) 0.0180(2) Uani 1 1 d . . . C41 C 1.00890(8) -0.05418(8) 0.27751(7) 0.0211(2) Uani 1 1 d . . . C42 C 1.10700(9) -0.09494(10) 0.27509(9) 0.0304(3) Uani 1 1 d . . . C43 C 1.18439(9) -0.04238(11) 0.23922(9) 0.0366(3) Uani 1 1 d . . . C44 C 1.16549(9) 0.05282(11) 0.20468(9) 0.0316(3) Uani 1 1 d . . . C45 C 1.06929(8) 0.09797(9) 0.20394(7) 0.0221(2) Uani 1 1 d . . . C46 C 1.05395(9) 0.20118(9) 0.16080(7) 0.0238(2) Uani 1 1 d . . . C47 C 1.13074(11) 0.26861(12) 0.18042(9) 0.0344(3) Uani 1 1 d . . . C48 C 1.05701(11) 0.20215(13) 0.07390(8) 0.0341(3) Uani 1 1 d . . . C49 C 0.92976(8) -0.11809(9) 0.31998(7) 0.0215(2) Uani 1 1 d . . . C50 C 0.89482(13) -0.18862(13) 0.27160(9) 0.0391(3) Uani 1 1 d . . . C51 C 0.96668(11) -0.17695(11) 0.39711(8) 0.0328(3) Uani 1 1 d . . . C52 C 0.79878(8) 0.31009(8) 0.28613(6) 0.01524(19) Uani 1 1 d . . . B53 B 0.82058(8) 0.41232(8) 0.31822(7) 0.0148(2) Uani 1 1 d . . . C54 C 0.93486(8) 0.40892(8) 0.35120(6) 0.01614(19) Uani 1 1 d . . . C55 C 1.00593(8) 0.33132(8) 0.35742(6) 0.0183(2) Uani 1 1 d . . . C56 C 1.09954(8) 0.33119(9) 0.38940(7) 0.0232(2) Uani 1 1 d . . . C57 C 1.12566(9) 0.41054(10) 0.41700(7) 0.0264(3) Uani 1 1 d . . . C58 C 1.05841(9) 0.48991(9) 0.41310(7) 0.0233(2) Uani 1 1 d . . . C59 C 0.96563(8) 0.48698(8) 0.38153(6) 0.0192(2) Uani 1 1 d . . . F60 F 0.98767(5) 0.24873(5) 0.33219(4) 0.02408(14) Uani 1 1 d . . . F61 F 1.16505(5) 0.25354(6) 0.39150(5) 0.03487(18) Uani 1 1 d . . . F62 F 1.21687(6) 0.41194(6) 0.44624(5) 0.0406(2) Uani 1 1 d . . . F63 F 1.08364(6) 0.56953(6) 0.43871(5) 0.03283(17) Uani 1 1 d . . . F64 F 0.90302(5) 0.56688(5) 0.37959(4) 0.02424(14) Uani 1 1 d . . . C65 C 0.74660(8) 0.42539(8) 0.39314(6) 0.01640(19) Uani 1 1 d . . . C66 C 0.75121(8) 0.35381(8) 0.45924(6) 0.0192(2) Uani 1 1 d . . . C67 C 0.69929(9) 0.35878(9) 0.52770(7) 0.0245(2) Uani 1 1 d . . . C68 C 0.63928(9) 0.44061(10) 0.53323(7) 0.0255(2) Uani 1 1 d . . . C69 C 0.63230(8) 0.51471(9) 0.47062(7) 0.0223(2) Uani 1 1 d . . . C70 C 0.68493(8) 0.50626(8) 0.40290(6) 0.0188(2) Uani 1 1 d . . . F71 F 0.81290(5) 0.27304(5) 0.45883(4) 0.02495(15) Uani 1 1 d . . . F72 F 0.70939(7) 0.28582(6) 0.58841(4) 0.0386(2) Uani 1 1 d . . . F73 F 0.59043(6) 0.44939(6) 0.59954(4) 0.03679(19) Uani 1 1 d . . . F74 F 0.57754(5) 0.59713(5) 0.47668(4) 0.03072(17) Uani 1 1 d . . . F75 F 0.67513(5) 0.58533(5) 0.34618(4) 0.02612(15) Uani 1 1 d . . . C76 C 0.79863(7) 0.50122(7) 0.24419(6) 0.01531(19) Uani 1 1 d . . . C77 C 0.70398(8) 0.51560(8) 0.21166(6) 0.0184(2) Uani 1 1 d . . . C78 C 0.67720(8) 0.58705(8) 0.14977(7) 0.0217(2) Uani 1 1 d . . . C79 C 0.74695(9) 0.65032(8) 0.11599(6) 0.0218(2) Uani 1 1 d . . . C80 C 0.84182(9) 0.63990(8) 0.14481(6) 0.0199(2) Uani 1 1 d . . . C81 C 0.86558(8) 0.56628(8) 0.20648(6) 0.01676(19) Uani 1 1 d . . . F82 F 0.62983(5) 0.45771(5) 0.24254(4) 0.02438(15) Uani 1 1 d . . . F83 F 0.58410(5) 0.59478(6) 0.12136(4) 0.03252(17) Uani 1 1 d . . . F84 F 0.72281(6) 0.71862(5) 0.05428(4) 0.03173(17) Uani 1 1 d . . . F85 F 0.91246(5) 0.69795(5) 0.11078(4) 0.02779(16) Uani 1 1 d . . . F86 F 0.96283(5) 0.55992(5) 0.22639(4) 0.02260(14) Uani 1 1 d . . . F87 F 0.30641(12) 0.39547(11) 0.21072(11) 0.0526(7) Uani 0.576(3) 1 d P . . C88 C 0.29387(11) 0.47951(13) 0.22333(9) 0.0416(4) Uani 1 1 d . . . C89 C 0.20157(10) 0.52047(11) 0.24016(8) 0.0331(3) Uani 1 1 d . . . C90 C 0.19439(11) 0.61619(11) 0.24914(8) 0.0368(3) Uani 1 1 d . . . C91 C 0.27824(12) 0.66991(13) 0.24098(9) 0.0424(4) Uani 1 1 d . . . C92 C 0.36982(12) 0.62741(15) 0.22360(10) 0.0489(4) Uani 1 1 d . . . C93 C 0.37886(11) 0.53182(15) 0.21513(10) 0.0495(4) Uani 1 1 d . . . F94 F 0.2868(4) 0.7473(3) 0.2407(3) 0.066(2) Uani 0.216(4) 1 d P . . H94 H 0.5240(9) 0.2558(9) 0.2117(7) 0.015(3) Uiso 1 1 d . . . F95 F 0.4460(2) 0.6674(3) 0.2264(2) 0.0654(14) Uani 0.322(4) 1 d P . . H96 H 0.6088(10) -0.2292(10) 0.3574(8) 0.029(4) Uiso 1 1 d . . . H97 H 0.6894(12) -0.2499(12) 0.4743(9) 0.041(4) Uiso 1 1 d . . . H98 H 0.7610(10) -0.1239(10) 0.5144(8) 0.025(3) Uiso 1 1 d . . . H99 H 0.7464(9) 0.1227(9) 0.4168(7) 0.014(3) Uiso 1 1 d . . . H100 H 0.6643(13) 0.0663(11) 0.5415(9) 0.042(4) Uiso 1 1 d . . . H101 H 0.7652(11) 0.1180(11) 0.5512(9) 0.034(4) Uiso 1 1 d . . . H102 H 0.7679(12) 0.0022(12) 0.5687(10) 0.047(5) Uiso 1 1 d . . . H103 H 0.9082(11) -0.0046(11) 0.4736(9) 0.035(4) Uiso 1 1 d . . . H104 H 0.9105(11) 0.1100(11) 0.4620(9) 0.037(4) Uiso 1 1 d . . . H105 H 0.9110(11) 0.0569(10) 0.3883(9) 0.030(4) Uiso 1 1 d . . . H106 H 0.5987(10) -0.0164(10) 0.2139(8) 0.025(3) Uiso 1 1 d . . . H108 H 0.4497(13) -0.1344(13) 0.2893(10) 0.048(5) Uiso 1 1 d . . . H109 H 0.4448(13) -0.0253(13) 0.2808(10) 0.052(5) Uiso 1 1 d . . . H110 H 0.5845(11) -0.1499(10) 0.1517(9) 0.032(4) Uiso 1 1 d . . . H111 H 0.6883(13) -0.1556(12) 0.1926(9) 0.044(5) Uiso 1 1 d . . . H112 H 0.6033(11) -0.2223(12) 0.2322(9) 0.039(4) Uiso 1 1 d . . . H113 H 0.4914(11) 0.0205(11) 0.3983(9) 0.034(4) Uiso 1 1 d . . . H114 H 0.4507(11) 0.1006(10) 0.4478(9) 0.033(4) Uiso 1 1 d . . . H115 H 0.5638(12) 0.0717(11) 0.4433(9) 0.034(4) Uiso 1 1 d . . . H116 H 0.3881(14) 0.1327(14) 0.2866(11) 0.060(6) Uiso 1 1 d . . . H117 H 0.3645(12) 0.1920(12) 0.3543(10) 0.042(4) Uiso 1 1 d . . . H118 H 0.4015(12) 0.2459(13) 0.2795(10) 0.043(5) Uiso 1 1 d . . . H119 H 0.5426(12) 0.3122(12) 0.3368(9) 0.039(4) Uiso 1 1 d . . . H120 H 0.4970(12) 0.2690(11) 0.4179(9) 0.036(4) Uiso 1 1 d . . . H121 H 0.6068(14) 0.2434(13) 0.4020(10) 0.053(5) Uiso 1 1 d . . . H123 H 0.4638(12) 0.3521(11) 0.1213(10) 0.041(4) Uiso 1 1 d . . . H124 H 0.5588(13) 0.3949(12) 0.0705(10) 0.048(5) Uiso 1 1 d . . . H125 H 0.4288(12) 0.1763(11) 0.1413(10) 0.043(4) Uiso 1 1 d . . . H126 H 0.4881(13) 0.1037(13) 0.0888(10) 0.046(5) Uiso 1 1 d . . . H127 H 0.4127(12) 0.1903(12) 0.0512(10) 0.043(4) Uiso 1 1 d . . . H128 H 0.5226(11) 0.2539(10) -0.0429(8) 0.029(4) Uiso 1 1 d . . . H129 H 0.6290(11) 0.2878(11) -0.0331(9) 0.034(4) Uiso 1 1 d . . . H130 H 0.6109(11) 0.1774(11) -0.0178(8) 0.030(4) Uiso 1 1 d . . . H131 H 0.8649(10) 0.0638(10) -0.0680(8) 0.023(3) Uiso 1 1 d . . . H132 H 0.9148(10) 0.2146(10) -0.1329(8) 0.025(3) Uiso 1 1 d . . . H133 H 0.8804(11) 0.3529(11) -0.0809(9) 0.035(4) Uiso 1 1 d . . . H134 H 0.7454(10) 0.3696(9) 0.0953(8) 0.023(3) Uiso 1 1 d . . . H135 H 0.7834(12) 0.4829(11) -0.0563(10) 0.042(4) Uiso 1 1 d . . . H136 H 0.6783(14) 0.4425(13) -0.0306(10) 0.053(5) Uiso 1 1 d . . . H137 H 0.7194(11) 0.5202(11) 0.0106(9) 0.037(4) Uiso 1 1 d . . . H138 H 0.8763(11) 0.4807(11) 0.0837(9) 0.037(4) Uiso 1 1 d . . . H139 H 0.9343(11) 0.4239(11) 0.0257(9) 0.036(4) Uiso 1 1 d . . . H140 H 0.9213(10) 0.3715(10) 0.1130(8) 0.025(4) Uiso 1 1 d . . . H141 H 0.7386(10) 0.0151(10) 0.1118(8) 0.027(4) Uiso 1 1 d . . . H142 H 0.9116(12) -0.0350(12) 0.1145(10) 0.045(5) Uiso 1 1 d . . . H144 H 0.9047(12) -0.0617(11) 0.0284(10) 0.040(4) Uiso 1 1 d . . . H145 H 0.6836(12) -0.0951(12) 0.0384(10) 0.044(5) Uiso 1 1 d . . . H146 H 0.7280(12) -0.0335(11) -0.0375(9) 0.038(4) Uiso 1 1 d . . . H148 H 1.1194(10) -0.1602(10) 0.3002(8) 0.027(4) Uiso 1 1 d . . . H149 H 1.2500(13) -0.0714(12) 0.2398(10) 0.048(5) Uiso 1 1 d . . . H150 H 1.2173(12) 0.0889(11) 0.1805(9) 0.036(4) Uiso 1 1 d . . . H151 H 0.9846(10) 0.2244(9) 0.1759(8) 0.021(3) Uiso 1 1 d . . . H152 H 1.1384(11) 0.2596(11) 0.2363(10) 0.037(4) Uiso 1 1 d . . . H153 H 1.1975(13) 0.2532(12) 0.1583(9) 0.043(4) Uiso 1 1 d . . . H154 H 1.1138(12) 0.3343(13) 0.1567(10) 0.045(5) Uiso 1 1 d . . . H155 H 1.1203(12) 0.1759(11) 0.0597(9) 0.039(4) Uiso 1 1 d . . . H156 H 1.0488(13) 0.2704(13) 0.0459(10) 0.051(5) Uiso 1 1 d . . . H158 H 0.8745(10) -0.0775(10) 0.3309(8) 0.027(4) Uiso 1 1 d . . . H162 H 0.9993(14) -0.1311(14) 0.4262(11) 0.060(5) Uiso 1 1 d . . . H163 H 1.0144(12) -0.2283(12) 0.3905(9) 0.041(4) Uiso 1 1 d . . . H164 H 0.9106(12) -0.2086(11) 0.4274(9) 0.036(4) Uiso 1 1 d . . . H165 H 0.8092(9) 0.2525(10) 0.3247(8) 0.020(3) Uiso 1 1 d . . . H166 H 0.7294(10) 0.3128(9) 0.2700(7) 0.021(3) Uiso 1 1 d . . . H167 H 0.8428(10) 0.3036(10) 0.2422(8) 0.027(4) Uiso 1 1 d . . . H168 H 0.1398(12) 0.4815(11) 0.2459(9) 0.041(4) Uiso 1 1 d . . . H169 H 0.1261(11) 0.6491(11) 0.2641(9) 0.037(4) Uiso 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 Ti1 0.01148(8) 0.01262(8) 0.01204(8) -0.00221(6) -0.00056(6) -0.00182(6) N2 0.0117(4) 0.0128(4) 0.0149(4) -0.0016(3) -0.0010(3) -0.0008(3) C3 0.0108(4) 0.0140(4) 0.0174(5) -0.0032(4) -0.0005(3) -0.0022(3) C4 0.0134(4) 0.0155(5) 0.0167(5) -0.0027(4) -0.0016(3) 0.0017(4) C5 0.0168(4) 0.0131(4) 0.0153(5) -0.0026(4) -0.0031(4) 0.0006(4) N6 0.0160(4) 0.0131(4) 0.0132(4) -0.0031(3) -0.0004(3) -0.0012(3) C7 0.0122(4) 0.0132(4) 0.0181(5) -0.0003(4) 0.0021(3) -0.0007(3) C8 0.0149(4) 0.0164(5) 0.0242(5) -0.0040(4) 0.0013(4) -0.0022(4) C9 0.0239(5) 0.0149(5) 0.0318(6) -0.0043(5) 0.0035(5) -0.0049(4) C10 0.0271(6) 0.0146(5) 0.0296(6) 0.0028(5) 0.0043(5) -0.0009(4) C11 0.0206(5) 0.0201(5) 0.0200(5) 0.0023(4) 0.0011(4) 0.0001(4) C12 0.0147(4) 0.0155(5) 0.0174(5) 0.0000(4) 0.0015(4) -0.0001(4) C13 0.0188(5) 0.0177(5) 0.0155(5) -0.0003(4) -0.0015(4) -0.0026(4) C14 0.0369(7) 0.0310(7) 0.0192(6) -0.0054(5) 0.0054(5) -0.0085(6) C15 0.0191(5) 0.0290(6) 0.0268(6) -0.0082(5) -0.0050(4) -0.0025(5) C16 0.0214(5) 0.0207(5) 0.0290(6) -0.0076(5) -0.0040(4) -0.0049(4) C17 0.0202(6) 0.0615(11) 0.0512(10) -0.0280(9) -0.0062(6) -0.0009(7) C18 0.0319(7) 0.0332(7) 0.0339(7) -0.0149(6) -0.0003(6) -0.0044(6) C19 0.0142(4) 0.0196(5) 0.0189(5) -0.0022(4) 0.0039(4) 0.0007(4) C20 0.0228(6) 0.0270(6) 0.0262(6) 0.0033(5) 0.0106(5) 0.0029(5) C21 0.0154(5) 0.0557(10) 0.0306(7) 0.0036(7) 0.0044(5) 0.0077(6) C22 0.0394(8) 0.0289(7) 0.0338(7) -0.0143(6) 0.0194(6) -0.0101(6) C23 0.0206(5) 0.0262(6) 0.0169(5) -0.0024(4) -0.0072(4) 0.0055(4) C24 0.0387(7) 0.0342(7) 0.0225(6) -0.0029(5) -0.0080(5) 0.0192(6) C25 0.0225(6) 0.0507(9) 0.0298(7) -0.0081(6) -0.0103(5) -0.0060(6) C26 0.0296(6) 0.0320(7) 0.0180(5) -0.0053(5) -0.0090(5) 0.0069(5) C27 0.0171(5) 0.0179(5) 0.0123(4) -0.0031(4) -0.0009(4) -0.0006(4) C28 0.0202(5) 0.0201(5) 0.0156(5) -0.0054(4) -0.0020(4) 0.0007(4) C29 0.0243(5) 0.0251(6) 0.0190(5) -0.0099(5) 0.0006(4) 0.0000(4) C30 0.0299(6) 0.0336(7) 0.0154(5) -0.0084(5) 0.0049(4) -0.0061(5) C31 0.0348(6) 0.0251(6) 0.0164(5) -0.0029(4) 0.0047(5) -0.0072(5) C32 0.0259(5) 0.0194(5) 0.0139(5) -0.0033(4) 0.0012(4) -0.0023(4) C33 0.0381(7) 0.0170(5) 0.0165(5) -0.0021(4) 0.0043(5) -0.0031(5) C34 0.0572(9) 0.0200(6) 0.0230(6) -0.0001(5) -0.0019(6) 0.0007(6) C35 0.0461(8) 0.0220(6) 0.0242(6) -0.0076(5) 0.0059(6) -0.0103(6) C36 0.0350(6) 0.0173(5) 0.0207(6) -0.0065(4) 0.0024(5) -0.0015(5) C37 0.0496(8) 0.0224(6) 0.0299(7) -0.0081(5) -0.0108(6) 0.0082(6) C38 0.0383(7) 0.0228(6) 0.0372(8) -0.0083(6) -0.0010(6) -0.0070(6) N39 0.0134(4) 0.0193(4) 0.0162(4) -0.0056(3) -0.0009(3) -0.0014(3) C40 0.0124(4) 0.0242(5) 0.0198(5) -0.0108(4) -0.0017(4) -0.0001(4) C41 0.0155(5) 0.0245(6) 0.0251(6) -0.0104(5) -0.0030(4) 0.0027(4) C42 0.0189(5) 0.0291(7) 0.0443(8) -0.0116(6) -0.0032(5) 0.0065(5) C43 0.0146(5) 0.0412(8) 0.0567(9) -0.0182(7) 0.0002(5) 0.0045(5) C44 0.0147(5) 0.0381(7) 0.0457(8) -0.0172(6) 0.0043(5) -0.0047(5) C45 0.0152(5) 0.0284(6) 0.0260(6) -0.0135(5) 0.0015(4) -0.0034(4) C46 0.0193(5) 0.0301(6) 0.0240(6) -0.0097(5) 0.0061(4) -0.0059(5) C47 0.0329(7) 0.0365(8) 0.0372(8) -0.0122(6) 0.0062(6) -0.0158(6) C48 0.0296(7) 0.0482(9) 0.0269(7) -0.0146(6) 0.0039(5) -0.0012(6) C49 0.0184(5) 0.0235(6) 0.0226(5) -0.0057(4) -0.0015(4) 0.0044(4) C50 0.0389(8) 0.0512(9) 0.0317(8) -0.0138(7) 0.0031(6) -0.0212(7) C51 0.0348(7) 0.0310(7) 0.0303(7) -0.0018(6) -0.0077(6) 0.0074(6) C52 0.0151(4) 0.0152(5) 0.0153(5) -0.0018(4) -0.0007(4) -0.0023(4) B53 0.0144(5) 0.0148(5) 0.0155(5) -0.0023(4) -0.0006(4) -0.0028(4) C54 0.0161(4) 0.0174(5) 0.0147(5) -0.0012(4) -0.0008(4) -0.0036(4) C55 0.0180(5) 0.0177(5) 0.0189(5) -0.0006(4) -0.0035(4) -0.0036(4) C56 0.0186(5) 0.0241(6) 0.0244(6) 0.0027(5) -0.0071(4) 0.0005(4) C57 0.0183(5) 0.0368(7) 0.0234(6) 0.0008(5) -0.0097(4) -0.0084(5) C58 0.0250(5) 0.0273(6) 0.0193(5) -0.0050(4) -0.0030(4) -0.0115(5) C59 0.0193(5) 0.0199(5) 0.0187(5) -0.0034(4) -0.0004(4) -0.0040(4) F60 0.0207(3) 0.0174(3) 0.0347(4) -0.0061(3) -0.0067(3) 0.0012(3) F61 0.0229(4) 0.0324(4) 0.0461(5) 0.0008(4) -0.0135(3) 0.0064(3) F62 0.0257(4) 0.0485(5) 0.0480(5) -0.0036(4) -0.0224(4) -0.0084(4) F63 0.0329(4) 0.0374(4) 0.0337(4) -0.0152(3) -0.0061(3) -0.0153(3) F64 0.0237(3) 0.0205(3) 0.0312(4) -0.0108(3) -0.0004(3) -0.0037(3) C65 0.0152(4) 0.0177(5) 0.0175(5) -0.0048(4) -0.0003(4) -0.0055(4) C66 0.0227(5) 0.0185(5) 0.0178(5) -0.0058(4) -0.0004(4) -0.0049(4) C67 0.0329(6) 0.0260(6) 0.0159(5) -0.0044(4) 0.0021(4) -0.0111(5) C68 0.0251(6) 0.0360(7) 0.0199(5) -0.0144(5) 0.0072(4) -0.0124(5) C69 0.0176(5) 0.0259(6) 0.0272(6) -0.0135(5) 0.0030(4) -0.0051(4) C70 0.0172(5) 0.0200(5) 0.0202(5) -0.0054(4) 0.0008(4) -0.0041(4) F71 0.0361(4) 0.0193(3) 0.0183(3) -0.0013(3) -0.0003(3) 0.0005(3) F72 0.0645(6) 0.0339(4) 0.0159(3) -0.0003(3) 0.0073(3) -0.0068(4) F73 0.0398(4) 0.0513(5) 0.0230(4) -0.0167(4) 0.0120(3) -0.0091(4) F74 0.0245(4) 0.0337(4) 0.0377(4) -0.0185(3) 0.0066(3) 0.0009(3) F75 0.0286(4) 0.0204(3) 0.0278(4) -0.0028(3) 0.0040(3) 0.0044(3) C76 0.0151(4) 0.0143(5) 0.0166(5) -0.0031(4) 0.0001(4) -0.0008(4) C77 0.0167(5) 0.0177(5) 0.0202(5) -0.0013(4) 0.0001(4) -0.0017(4) C78 0.0191(5) 0.0222(5) 0.0223(5) -0.0015(4) -0.0039(4) 0.0036(4) C79 0.0295(6) 0.0158(5) 0.0179(5) 0.0009(4) -0.0010(4) 0.0043(4) C80 0.0261(5) 0.0140(5) 0.0192(5) -0.0022(4) 0.0042(4) -0.0036(4) C81 0.0161(5) 0.0161(5) 0.0183(5) -0.0039(4) 0.0004(4) -0.0016(4) F82 0.0147(3) 0.0273(4) 0.0289(4) 0.0027(3) -0.0027(3) -0.0051(3) F83 0.0211(3) 0.0409(4) 0.0311(4) 0.0043(3) -0.0095(3) 0.0046(3) F84 0.0418(4) 0.0239(4) 0.0244(4) 0.0076(3) -0.0040(3) 0.0043(3) F85 0.0343(4) 0.0213(3) 0.0257(4) 0.0028(3) 0.0063(3) -0.0102(3) F86 0.0159(3) 0.0255(3) 0.0250(3) 0.0009(3) -0.0004(2) -0.0062(3) F87 0.0384(9) 0.0309(9) 0.0907(15) -0.0174(8) 0.0043(8) -0.0030(7) C88 0.0306(7) 0.0553(10) 0.0392(8) -0.0135(7) -0.0042(6) 0.0090(7) C89 0.0254(6) 0.0409(8) 0.0289(7) 0.0028(6) 0.0023(5) 0.0010(6) C90 0.0314(7) 0.0409(8) 0.0343(7) -0.0004(6) 0.0039(6) 0.0057(6) C91 0.0442(9) 0.0480(10) 0.0350(8) -0.0051(7) -0.0026(6) -0.0068(7) C92 0.0357(8) 0.0775(13) 0.0388(9) -0.0211(9) -0.0024(6) -0.0128(8) C93 0.0224(7) 0.0832(13) 0.0483(10) -0.0296(9) -0.0024(6) 0.0057(8) F94 0.084(4) 0.036(3) 0.080(4) -0.017(3) -0.009(3) -0.003(2) F95 0.0427(19) 0.075(3) 0.090(3) -0.040(2) 0.0193(16) -0.0322(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 N39 1.7186(9) . ? Ti1 N2 1.9656(9) . ? Ti1 N6 2.0817(9) . ? Ti1 C52 2.4116(11) . ? Ti1 C3 2.6342(10) . ? Ti1 H165 2.200(13) . ? Ti1 H167 2.221(13) . ? N2 C3 1.3784(12) . ? N2 C7 1.4470(13) . ? C3 C4 1.3863(14) . ? C3 C19 1.5639(14) . ? C4 C5 1.4533(15) . ? C4 H94 0.964(12) . ? C5 N6 1.3206(13) . ? C5 C23 1.5581(14) . ? N6 C27 1.4591(13) . ? C7 C8 1.4056(15) . ? C7 C12 1.4102(15) . ? C8 C9 1.3986(16) . ? C8 C16 1.5225(16) . ? C9 C10 1.3820(18) . ? C9 H96 0.941(15) . ? C10 C11 1.3790(18) . ? C10 H97 0.920(16) . ? C11 C12 1.3943(15) . ? C11 H98 0.971(14) . ? C12 C13 1.5231(16) . ? C13 C15 1.5321(16) . ? C13 C14 1.5355(16) . ? C13 H99 0.992(12) . ? C14 H100 0.993(16) . ? C14 H101 0.974(16) . ? C14 H102 1.018(17) . ? C15 H103 0.946(15) . ? C15 H104 0.968(16) . ? C15 H105 1.028(15) . ? C16 C17 1.5253(18) . ? C16 C18 1.5274(18) . ? C16 H106 0.962(14) . ? C17 H107 0.968(18) . ? C17 H108 0.958(18) . ? C17 H109 0.922(18) . ? C18 H110 0.990(15) . ? C18 H111 0.959(17) . ? C18 H112 0.991(16) . ? C19 C20 1.5285(16) . ? C19 C22 1.5337(18) . ? C19 C21 1.5386(17) . ? C20 H113 0.989(15) . ? C20 H114 0.956(15) . ? C20 H115 0.945(15) . ? C21 H116 1.006(19) . ? C21 H117 0.915(17) . ? C21 H118 0.929(17) . ? C22 H119 0.977(16) . ? C22 H120 0.951(16) . ? C22 H121 0.975(18) . ? C23 C26 1.5342(17) . ? C23 C25 1.5450(19) . ? C23 C24 1.5487(18) . ? C24 H122 0.979(16) . ? C24 H123 0.988(16) . ? C24 H124 0.999(17) . ? C25 H125 1.006(17) . ? C25 H126 1.006(17) . ? C25 H127 0.968(17) . ? C26 H128 0.980(14) . ? C26 H129 0.961(16) . ? C26 H130 0.946(15) . ? C27 C28 1.4029(15) . ? C27 C32 1.4056(15) . ? C28 C29 1.3957(15) . ? C28 C36 1.5134(16) . ? C29 C30 1.3772(17) . ? C29 H131 0.945(14) . ? C30 C31 1.3775(17) . ? C30 H132 0.945(14) . ? C31 C32 1.3975(16) . ? C31 H133 0.980(15) . ? C32 C33 1.5230(16) . ? C33 C35 1.5298(19) . ? C33 C34 1.5388(18) . ? C33 H134 0.997(14) . ? C34 H135 0.998(17) . ? C34 H136 0.933(18) . ? C34 H137 0.992(16) . ? C35 H138 0.974(16) . ? C35 H139 0.968(16) . ? C35 H140 0.999(14) . ? C36 C37 1.5264(19) . ? C36 C38 1.5332(19) . ? C36 H141 0.963(14) . ? C37 H143 0.963(17) . ? C37 H142 0.990(17) . ? C37 H144 0.992(16) . ? C38 H147 1.017(17) . ? C38 H145 0.960(17) . ? C38 H146 0.992(16) . ? N39 C40 1.4061(13) . ? C40 C45 1.4222(16) . ? C40 C41 1.4246(16) . ? C41 C42 1.3984(15) . ? C41 C49 1.5208(17) . ? C42 C43 1.379(2) . ? C42 H148 0.948(14) . ? C43 C44 1.374(2) . ? C43 H149 0.942(17) . ? C44 C45 1.3951(16) . ? C44 H150 0.930(15) . ? C45 C46 1.5117(18) . ? C46 C48 1.5284(18) . ? C46 C47 1.5296(18) . ? C46 H151 1.006(13) . ? C47 H152 0.978(16) . ? C47 H153 0.989(17) . ? C47 H154 0.956(17) . ? C48 H157 0.935(18) . ? C48 H155 0.945(16) . ? C48 H156 0.995(18) . ? C49 C50 1.5228(19) . ? C49 C51 1.5344(18) . ? C49 H158 0.939(14) . ? C50 H159 1.006(16) . ? C50 H160 1.00(2) . ? C50 H161 0.976(19) . ? C51 H162 1.019(19) . ? C51 H163 0.951(16) . ? C51 H164 0.988(16) . ? C52 B53 1.6803(16) . ? C52 H165 0.962(13) . ? C52 H166 0.975(13) . ? C52 H167 0.970(14) . ? B53 C54 1.6474(15) . ? B53 C76 1.6514(15) . ? B53 C65 1.6535(16) . ? C54 C55 1.3879(15) . ? C54 C59 1.3934(15) . ? C55 F60 1.3535(13) . ? C55 C56 1.3893(15) . ? C56 F61 1.3477(13) . ? C56 C57 1.3629(18) . ? C57 F62 1.3423(13) . ? C57 C58 1.3770(18) . ? C58 F63 1.3449(14) . ? C58 C59 1.3825(16) . ? C59 F64 1.3498(13) . ? C65 C70 1.3908(15) . ? C65 C66 1.3925(15) . ? C66 F71 1.3575(13) . ? C66 C67 1.3827(16) . ? C67 F72 1.3426(14) . ? C67 C68 1.3728(18) . ? C68 F73 1.3413(13) . ? C68 C69 1.3720(18) . ? C69 F74 1.3460(13) . ? C69 C70 1.3853(16) . ? C70 F75 1.3533(13) . ? C76 C81 1.3870(14) . ? C76 C77 1.3940(15) . ? C77 F82 1.3597(12) . ? C77 C78 1.3792(15) . ? C78 F83 1.3474(13) . ? C78 C79 1.3756(17) . ? C79 F84 1.3443(13) . ? C79 C80 1.3709(16) . ? C80 F85 1.3422(13) . ? C80 C81 1.3851(15) . ? C81 F86 1.3511(12) . ? F87 C88 1.238(2) . ? C88 C89 1.3732(19) . ? C88 C93 1.383(2) . ? C89 C90 1.377(2) . ? C89 H168 1.012(16) . ? C90 C91 1.381(2) . ? C90 H169 1.044(15) . ? C91 F94 1.098(5) . ? C91 C92 1.376(2) . ? C92 F95 1.201(3) . ? C92 C93 1.373(3) . ? C93 H170 0.96(2) . ? 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 N39 Ti1 N2 110.39(4) . . ? N39 Ti1 N6 109.64(4) . . ? N2 Ti1 N6 99.10(4) . . ? N39 Ti1 C52 113.79(4) . . ? N2 Ti1 C52 112.09(4) . . ? N6 Ti1 C52 110.88(4) . . ? N39 Ti1 C3 140.88(4) . . ? N2 Ti1 C3 30.72(3) . . ? N6 Ti1 C3 82.96(3) . . ? C52 Ti1 C3 94.10(3) . . ? N39 Ti1 H165 102.9(3) . . ? N2 Ti1 H165 99.1(3) . . ? N6 Ti1 H165 133.9(4) . . ? C52 Ti1 H165 23.5(3) . . ? C3 Ti1 H165 92.0(3) . . ? N39 Ti1 H167 100.0(4) . . ? N2 Ti1 H167 135.7(4) . . ? N6 Ti1 H167 100.1(4) . . ? C52 Ti1 H167 23.7(4) . . ? C3 Ti1 H167 114.5(4) . . ? H165 Ti1 H167 41.5(5) . . ? C3 N2 C7 124.27(8) . . ? C3 N2 Ti1 102.53(6) . . ? C7 N2 Ti1 132.64(6) . . ? N2 C3 C4 119.90(9) . . ? N2 C3 C19 124.85(9) . . ? C4 C3 C19 114.90(9) . . ? N2 C3 Ti1 46.75(5) . . ? C4 C3 Ti1 80.58(6) . . ? C19 C3 Ti1 145.27(7) . . ? C3 C4 C5 134.19(9) . . ? C3 C4 H94 113.4(7) . . ? C5 C4 H94 111.6(7) . . ? N6 C5 C4 119.23(9) . . ? N6 C5 C23 128.72(9) . . ? C4 C5 C23 112.04(9) . . ? C5 N6 C27 123.65(9) . . ? C5 N6 Ti1 108.01(7) . . ? C27 N6 Ti1 127.61(7) . . ? C8 C7 C12 121.27(9) . . ? C8 C7 N2 118.46(9) . . ? C12 C7 N2 120.22(9) . . ? C9 C8 C7 118.16(10) . . ? C9 C8 C16 118.58(10) . . ? C7 C8 C16 123.25(10) . . ? C10 C9 C8 121.21(11) . . ? C10 C9 H96 119.3(9) . . ? C8 C9 H96 119.4(9) . . ? C11 C10 C9 119.76(11) . . ? C11 C10 H97 119.2(10) . . ? C9 C10 H97 121.1(10) . . ? C10 C11 C12 121.71(11) . . ? C10 C11 H98 118.8(8) . . ? C12 C11 H98 119.5(8) . . ? C11 C12 C7 117.85(10) . . ? C11 C12 C13 118.25(10) . . ? C7 C12 C13 123.86(9) . . ? C12 C13 C15 112.15(9) . . ? C12 C13 C14 112.66(9) . . ? C15 C13 C14 108.54(10) . . ? C12 C13 H99 107.3(7) . . ? C15 C13 H99 106.7(7) . . ? C14 C13 H99 109.3(7) . . ? C13 C14 H100 112.2(9) . . ? C13 C14 H101 110.4(9) . . ? H100 C14 H101 109.1(12) . . ? C13 C14 H102 109.4(9) . . ? H100 C14 H102 109.0(13) . . ? H101 C14 H102 106.5(13) . . ? C13 C15 H103 107.6(9) . . ? C13 C15 H104 110.1(9) . . ? H103 C15 H104 111.8(13) . . ? C13 C15 H105 112.5(8) . . ? H103 C15 H105 107.4(12) . . ? H104 C15 H105 107.5(12) . . ? C8 C16 C17 111.62(11) . . ? C8 C16 C18 112.26(10) . . ? C17 C16 C18 109.12(11) . . ? C8 C16 H106 108.8(8) . . ? C17 C16 H106 108.2(8) . . ? C18 C16 H106 106.6(8) . . ? C16 C17 H107 111.5(10) . . ? C16 C17 H108 110.1(10) . . ? H107 C17 H108 108.5(15) . . ? C16 C17 H109 110.8(11) . . ? H107 C17 H109 109.3(15) . . ? H108 C17 H109 106.6(15) . . ? C16 C18 H110 111.9(8) . . ? C16 C18 H111 109.3(10) . . ? H110 C18 H111 107.9(13) . . ? C16 C18 H112 111.3(9) . . ? H110 C18 H112 108.0(12) . . ? H111 C18 H112 108.4(13) . . ? C20 C19 C22 107.76(11) . . ? C20 C19 C21 106.27(10) . . ? C22 C19 C21 108.81(12) . . ? C20 C19 C3 115.37(9) . . ? C22 C19 C3 106.74(9) . . ? C21 C19 C3 111.71(10) . . ? C19 C20 H113 111.9(9) . . ? C19 C20 H114 107.0(9) . . ? H113 C20 H114 111.0(12) . . ? C19 C20 H115 110.9(9) . . ? H113 C20 H115 107.5(12) . . ? H114 C20 H115 108.6(13) . . ? C19 C21 H116 110.8(11) . . ? C19 C21 H117 105.5(10) . . ? H116 C21 H117 111.4(15) . . ? C19 C21 H118 111.2(10) . . ? H116 C21 H118 110.6(15) . . ? H117 C21 H118 107.1(14) . . ? C19 C22 H119 111.3(9) . . ? C19 C22 H120 111.6(9) . . ? H119 C22 H120 108.8(13) . . ? C19 C22 H121 111.5(10) . . ? H119 C22 H121 109.5(14) . . ? H120 C22 H121 104.0(14) . . ? C26 C23 C25 106.33(10) . . ? C26 C23 C24 108.20(10) . . ? C25 C23 C24 109.19(11) . . ? C26 C23 C5 117.66(9) . . ? C25 C23 C5 106.04(9) . . ? C24 C23 C5 109.15(10) . . ? C23 C24 H122 107.5(9) . . ? C23 C24 H123 112.8(9) . . ? H122 C24 H123 108.8(13) . . ? C23 C24 H124 112.0(10) . . ? H122 C24 H124 106.9(13) . . ? H123 C24 H124 108.6(13) . . ? C23 C25 H125 112.7(9) . . ? C23 C25 H126 111.8(10) . . ? H125 C25 H126 109.8(13) . . ? C23 C25 H127 108.5(10) . . ? H125 C25 H127 106.7(13) . . ? H126 C25 H127 107.0(13) . . ? C23 C26 H128 105.6(8) . . ? C23 C26 H129 114.1(9) . . ? H128 C26 H129 106.3(12) . . ? C23 C26 H130 112.8(9) . . ? H128 C26 H130 108.2(12) . . ? H129 C26 H130 109.3(12) . . ? C28 C27 C32 121.04(10) . . ? C28 C27 N6 119.15(9) . . ? C32 C27 N6 119.79(9) . . ? C29 C28 C27 118.36(10) . . ? C29 C28 C36 117.64(10) . . ? C27 C28 C36 123.99(10) . . ? C30 C29 C28 121.44(11) . . ? C30 C29 H131 120.1(8) . . ? C28 C29 H131 118.4(8) . . ? C29 C30 C31 119.44(11) . . ? C29 C30 H132 121.2(8) . . ? C31 C30 H132 119.3(8) . . ? C30 C31 C32 121.81(11) . . ? C30 C31 H133 118.3(9) . . ? C32 C31 H133 119.8(9) . . ? C31 C32 C27 117.85(10) . . ? C31 C32 C33 116.93(10) . . ? C27 C32 C33 125.22(10) . . ? C32 C33 C35 110.20(10) . . ? C32 C33 C34 112.14(10) . . ? C35 C33 C34 108.85(11) . . ? C32 C33 H134 108.6(8) . . ? C35 C33 H134 108.2(8) . . ? C34 C33 H134 108.7(8) . . ? C33 C34 H135 110.7(9) . . ? C33 C34 H136 113.4(11) . . ? H135 C34 H136 109.1(14) . . ? C33 C34 H137 110.6(9) . . ? H135 C34 H137 105.1(12) . . ? H136 C34 H137 107.6(14) . . ? C33 C35 H138 109.6(9) . . ? C33 C35 H139 110.3(9) . . ? H138 C35 H139 107.3(12) . . ? C33 C35 H140 112.6(8) . . ? H138 C35 H140 109.2(12) . . ? H139 C35 H140 107.8(12) . . ? C28 C36 C37 109.34(11) . . ? C28 C36 C38 111.12(10) . . ? C37 C36 C38 110.76(11) . . ? C28 C36 H141 108.8(8) . . ? C37 C36 H141 110.2(8) . . ? C38 C36 H141 106.6(8) . . ? C36 C37 H143 109.4(10) . . ? C36 C37 H142 111.3(9) . . ? H143 C37 H142 106.5(13) . . ? C36 C37 H144 112.0(9) . . ? H143 C37 H144 106.3(13) . . ? H142 C37 H144 111.1(13) . . ? C36 C38 H147 111.6(9) . . ? C36 C38 H145 110.9(10) . . ? H147 C38 H145 106.3(13) . . ? C36 C38 H146 111.1(9) . . ? H147 C38 H146 109.0(13) . . ? H145 C38 H146 107.7(13) . . ? C40 N39 Ti1 171.86(8) . . ? N39 C40 C45 118.81(10) . . ? N39 C40 C41 121.84(10) . . ? C45 C40 C41 119.35(10) . . ? C42 C41 C40 118.44(11) . . ? C42 C41 C49 117.52(11) . . ? C40 C41 C49 124.04(9) . . ? C43 C42 C41 121.90(13) . . ? C43 C42 H148 120.4(9) . . ? C41 C42 H148 117.7(9) . . ? C44 C43 C42 119.60(12) . . ? C44 C43 H149 120.5(10) . . ? C42 C43 H149 119.8(10) . . ? C43 C44 C45 121.70(12) . . ? C43 C44 H150 120.2(9) . . ? C45 C44 H150 118.1(9) . . ? C44 C45 C40 118.99(12) . . ? C44 C45 C46 118.30(11) . . ? C40 C45 C46 122.65(10) . . ? C45 C46 C48 109.80(11) . . ? C45 C46 C47 113.27(11) . . ? C48 C46 C47 109.63(11) . . ? C45 C46 H151 105.7(7) . . ? C48 C46 H151 108.3(8) . . ? C47 C46 H151 109.9(7) . . ? C46 C47 H152 110.3(9) . . ? C46 C47 H153 110.7(9) . . ? H152 C47 H153 106.5(13) . . ? C46 C47 H154 110.6(10) . . ? H152 C47 H154 113.8(13) . . ? H153 C47 H154 104.7(13) . . ? C46 C48 H157 111.3(11) . . ? C46 C48 H155 109.1(10) . . ? H157 C48 H155 107.8(14) . . ? C46 C48 H156 109.3(10) . . ? H157 C48 H156 111.4(14) . . ? H155 C48 H156 107.9(14) . . ? C41 C49 C50 111.88(10) . . ? C41 C49 C51 112.52(10) . . ? C50 C49 C51 108.25(12) . . ? C41 C49 H158 108.0(8) . . ? C50 C49 H158 108.6(8) . . ? C51 C49 H158 107.4(8) . . ? C49 C50 H159 111.6(9) . . ? C49 C50 H160 110.6(11) . . ? H159 C50 H160 108.7(14) . . ? C49 C50 H161 108.8(11) . . ? H159 C50 H161 106.1(14) . . ? H160 C50 H161 111.0(15) . . ? C49 C51 H162 108.2(11) . . ? C49 C51 H163 112.5(10) . . ? H162 C51 H163 108.7(14) . . ? C49 C51 H164 110.6(9) . . ? H162 C51 H164 111.4(14) . . ? H163 C51 H164 105.4(13) . . ? B53 C52 Ti1 175.28(7) . . ? B53 C52 H165 113.0(8) . . ? Ti1 C52 H165 65.8(8) . . ? B53 C52 H166 109.8(8) . . ? Ti1 C52 H166 74.8(8) . . ? H165 C52 H166 107.3(11) . . ? B53 C52 H167 109.8(8) . . ? Ti1 C52 H167 67.0(8) . . ? H165 C52 H167 108.1(11) . . ? H166 C52 H167 108.8(11) . . ? C54 B53 C76 113.09(8) . . ? C54 B53 C65 104.37(8) . . ? C76 B53 C65 111.55(8) . . ? C54 B53 C52 111.87(8) . . ? C76 B53 C52 105.26(8) . . ? C65 B53 C52 110.86(8) . . ? C55 C54 C59 113.42(10) . . ? C55 C54 B53 126.57(9) . . ? C59 C54 B53 119.86(9) . . ? F60 C55 C54 121.26(9) . . ? F60 C55 C56 114.91(10) . . ? C54 C55 C56 123.82(11) . . ? F61 C56 C57 120.19(10) . . ? F61 C56 C55 119.95(11) . . ? C57 C56 C55 119.85(11) . . ? F62 C57 C56 120.22(12) . . ? F62 C57 C58 120.40(12) . . ? C56 C57 C58 119.37(10) . . ? F63 C58 C57 120.17(10) . . ? F63 C58 C59 120.71(11) . . ? C57 C58 C59 119.11(11) . . ? F64 C59 C58 116.25(10) . . ? F64 C59 C54 119.33(9) . . ? C58 C59 C54 124.40(11) . . ? C70 C65 C66 112.84(10) . . ? C70 C65 B53 127.63(9) . . ? C66 C65 B53 119.15(9) . . ? F71 C66 C67 115.93(10) . . ? F71 C66 C65 118.88(9) . . ? C67 C66 C65 125.17(11) . . ? F72 C67 C68 120.52(10) . . ? F72 C67 C66 120.53(11) . . ? C68 C67 C66 118.93(11) . . ? F73 C68 C69 120.34(11) . . ? F73 C68 C67 120.59(11) . . ? C69 C68 C67 119.04(10) . . ? F74 C69 C68 119.47(10) . . ? F74 C69 C70 120.37(11) . . ? C68 C69 C70 120.10(11) . . ? F75 C70 C69 114.73(10) . . ? F75 C70 C65 121.31(10) . . ? C69 C70 C65 123.91(11) . . ? C81 C76 C77 112.55(9) . . ? C81 C76 B53 127.63(9) . . ? C77 C76 B53 119.81(9) . . ? F82 C77 C78 115.55(9) . . ? F82 C77 C76 119.56(9) . . ? C78 C77 C76 124.88(10) . . ? F83 C78 C79 119.66(10) . . ? F83 C78 C77 120.85(10) . . ? C79 C78 C77 119.49(10) . . ? F84 C79 C80 121.08(10) . . ? F84 C79 C78 120.18(10) . . ? C80 C79 C78 118.69(10) . . ? F85 C80 C79 119.86(10) . . ? F85 C80 C81 120.31(10) . . ? C79 C80 C81 119.75(10) . . ? F86 C81 C80 114.04(9) . . ? F86 C81 C76 121.31(9) . . ? C80 C81 C76 124.61(10) . . ? F87 C88 C89 122.90(16) . . ? F87 C88 C93 115.26(15) . . ? C89 C88 C93 121.76(16) . . ? C88 C89 C90 118.60(14) . . ? C88 C89 H168 121.1(9) . . ? C90 C89 H168 120.3(9) . . ? C89 C90 C91 120.63(14) . . ? C89 C90 H169 120.9(8) . . ? C91 C90 H169 118.5(8) . . ? F94 C91 C92 108.7(3) . . ? F94 C91 C90 131.4(3) . . ? C92 C91 C90 119.68(17) . . ? F95 C92 C93 117.2(2) . . ? F95 C92 C91 121.2(2) . . ? C93 C92 C91 120.66(16) . . ? C92 C93 C88 118.66(15) . . ? C92 C93 H170 123.1(13) . . ? C88 C93 H170 118.3(13) . . ? 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 N39 Ti1 N2 C3 -174.17(6) . . . . ? N6 Ti1 N2 C3 -59.17(7) . . . . ? C52 Ti1 N2 C3 57.86(7) . . . . ? N39 Ti1 N2 C7 14.40(10) . . . . ? N6 Ti1 N2 C7 129.40(9) . . . . ? C52 Ti1 N2 C7 -113.57(9) . . . . ? C3 Ti1 N2 C7 -171.43(13) . . . . ? C7 N2 C3 C4 -150.76(10) . . . . ? Ti1 N2 C3 C4 36.86(11) . . . . ? C7 N2 C3 C19 36.33(15) . . . . ? Ti1 N2 C3 C19 -136.05(9) . . . . ? C7 N2 C3 Ti1 172.38(12) . . . . ? N39 Ti1 C3 N2 8.67(9) . . . . ? N6 Ti1 C3 N2 121.31(7) . . . . ? C52 Ti1 C3 N2 -128.13(7) . . . . ? N39 Ti1 C3 C4 -139.52(7) . . . . ? N2 Ti1 C3 C4 -148.19(10) . . . . ? N6 Ti1 C3 C4 -26.88(6) . . . . ? C52 Ti1 C3 C4 83.68(6) . . . . ? N39 Ti1 C3 C19 99.83(13) . . . . ? N2 Ti1 C3 C19 91.16(13) . . . . ? N6 Ti1 C3 C19 -147.53(12) . . . . ? C52 Ti1 C3 C19 -36.98(12) . . . . ? N2 C3 C4 C5 17.10(18) . . . . ? C19 C3 C4 C5 -169.31(11) . . . . ? Ti1 C3 C4 C5 43.39(12) . . . . ? C3 C4 C5 N6 -39.08(18) . . . . ? C3 C4 C5 C23 140.24(12) . . . . ? C4 C5 N6 C27 -174.45(9) . . . . ? C23 C5 N6 C27 6.35(17) . . . . ? C4 C5 N6 Ti1 -3.59(11) . . . . ? C23 C5 N6 Ti1 177.21(9) . . . . ? N39 Ti1 N6 C5 159.20(7) . . . . ? N2 Ti1 N6 C5 43.62(7) . . . . ? C52 Ti1 N6 C5 -74.33(7) . . . . ? C3 Ti1 N6 C5 17.39(7) . . . . ? N39 Ti1 N6 C27 -30.41(9) . . . . ? N2 Ti1 N6 C27 -145.99(8) . . . . ? C52 Ti1 N6 C27 96.06(8) . . . . ? C3 Ti1 N6 C27 -172.22(8) . . . . ? C3 N2 C7 C8 76.71(13) . . . . ? Ti1 N2 C7 C8 -113.43(10) . . . . ? C3 N2 C7 C12 -106.02(11) . . . . ? Ti1 N2 C7 C12 63.84(13) . . . . ? C12 C7 C8 C9 1.17(15) . . . . ? N2 C7 C8 C9 178.41(9) . . . . ? C12 C7 C8 C16 -179.53(10) . . . . ? N2 C7 C8 C16 -2.29(15) . . . . ? C7 C8 C9 C10 -1.97(17) . . . . ? C16 C8 C9 C10 178.69(11) . . . . ? C8 C9 C10 C11 1.20(18) . . . . ? C9 C10 C11 C12 0.44(18) . . . . ? C10 C11 C12 C7 -1.20(16) . . . . ? C10 C11 C12 C13 176.68(10) . . . . ? C8 C7 C12 C11 0.37(15) . . . . ? N2 C7 C12 C11 -176.82(9) . . . . ? C8 C7 C12 C13 -177.37(10) . . . . ? N2 C7 C12 C13 5.43(15) . . . . ? C11 C12 C13 C15 76.93(12) . . . . ? C7 C12 C13 C15 -105.33(12) . . . . ? C11 C12 C13 C14 -45.88(14) . . . . ? C7 C12 C13 C14 131.85(11) . . . . ? C9 C8 C16 C17 73.95(15) . . . . ? C7 C8 C16 C17 -105.35(14) . . . . ? C9 C8 C16 C18 -48.93(14) . . . . ? C7 C8 C16 C18 131.77(12) . . . . ? N2 C3 C19 C20 -24.13(15) . . . . ? C4 C3 C19 C20 162.65(10) . . . . ? Ti1 C3 C19 C20 -86.68(15) . . . . ? N2 C3 C19 C22 95.54(13) . . . . ? C4 C3 C19 C22 -77.68(12) . . . . ? Ti1 C3 C19 C22 32.99(16) . . . . ? N2 C3 C19 C21 -145.63(11) . . . . ? C4 C3 C19 C21 41.15(14) . . . . ? Ti1 C3 C19 C21 151.82(11) . . . . ? N6 C5 C23 C26 5.04(17) . . . . ? C4 C5 C23 C26 -174.20(10) . . . . ? N6 C5 C23 C25 123.79(12) . . . . ? C4 C5 C23 C25 -55.45(12) . . . . ? N6 C5 C23 C24 -118.70(13) . . . . ? C4 C5 C23 C24 62.06(13) . . . . ? C5 N6 C27 C28 -102.69(12) . . . . ? Ti1 N6 C27 C28 88.31(11) . . . . ? C5 N6 C27 C32 78.89(13) . . . . ? Ti1 N6 C27 C32 -90.11(11) . . . . ? C32 C27 C28 C29 -2.86(16) . . . . ? N6 C27 C28 C29 178.74(10) . . . . ? C32 C27 C28 C36 178.18(11) . . . . ? N6 C27 C28 C36 -0.22(16) . . . . ? C27 C28 C29 C30 1.28(17) . . . . ? C36 C28 C29 C30 -179.69(11) . . . . ? C28 C29 C30 C31 0.80(19) . . . . ? C29 C30 C31 C32 -1.37(19) . . . . ? C30 C31 C32 C27 -0.17(18) . . . . ? C30 C31 C32 C33 -179.76(12) . . . . ? C28 C27 C32 C31 2.32(16) . . . . ? N6 C27 C32 C31 -179.29(10) . . . . ? C28 C27 C32 C33 -178.13(11) . . . . ? N6 C27 C32 C33 0.26(16) . . . . ? C31 C32 C33 C35 -68.22(14) . . . . ? C27 C32 C33 C35 112.23(13) . . . . ? C31 C32 C33 C34 53.21(15) . . . . ? C27 C32 C33 C34 -126.35(13) . . . . ? C29 C28 C36 C37 59.64(14) . . . . ? C27 C28 C36 C37 -121.40(12) . . . . ? C29 C28 C36 C38 -62.93(14) . . . . ? C27 C28 C36 C38 116.03(12) . . . . ? N2 Ti1 N39 C40 -144.1(6) . . . . ? N6 Ti1 N39 C40 107.7(6) . . . . ? C52 Ti1 N39 C40 -17.1(6) . . . . ? C3 Ti1 N39 C40 -148.8(5) . . . . ? Ti1 N39 C40 C45 -35.2(6) . . . . ? Ti1 N39 C40 C41 144.3(5) . . . . ? N39 C40 C41 C42 179.28(11) . . . . ? C45 C40 C41 C42 -1.20(16) . . . . ? N39 C40 C41 C49 -0.92(17) . . . . ? C45 C40 C41 C49 178.60(10) . . . . ? C40 C41 C42 C43 1.01(19) . . . . ? C49 C41 C42 C43 -178.80(13) . . . . ? C41 C42 C43 C44 0.0(2) . . . . ? C42 C43 C44 C45 -0.8(2) . . . . ? C43 C44 C45 C40 0.6(2) . . . . ? C43 C44 C45 C46 -176.61(13) . . . . ? N39 C40 C45 C44 179.95(11) . . . . ? C41 C40 C45 C44 0.42(17) . . . . ? N39 C40 C45 C46 -2.96(16) . . . . ? C41 C40 C45 C46 177.51(10) . . . . ? C44 C45 C46 C48 74.30(14) . . . . ? C40 C45 C46 C48 -102.80(13) . . . . ? C44 C45 C46 C47 -48.62(15) . . . . ? C40 C45 C46 C47 134.27(12) . . . . ? C42 C41 C49 C50 -78.55(15) . . . . ? C40 C41 C49 C50 101.65(14) . . . . ? C42 C41 C49 C51 43.57(15) . . . . ? C40 C41 C49 C51 -136.23(12) . . . . ? N39 Ti1 C52 B53 9.7(9) . . . . ? N2 Ti1 C52 B53 135.8(9) . . . . ? N6 Ti1 C52 B53 -114.5(9) . . . . ? C3 Ti1 C52 B53 161.5(9) . . . . ? Ti1 C52 B53 C54 -17.2(9) . . . . ? Ti1 C52 B53 C76 106.0(9) . . . . ? Ti1 C52 B53 C65 -133.2(9) . . . . ? C76 B53 C54 C55 -122.19(11) . . . . ? C65 B53 C54 C55 116.39(11) . . . . ? C52 B53 C54 C55 -3.54(15) . . . . ? C76 B53 C54 C59 62.50(13) . . . . ? C65 B53 C54 C59 -58.92(12) . . . . ? C52 B53 C54 C59 -178.85(9) . . . . ? C59 C54 C55 F60 178.75(9) . . . . ? B53 C54 C55 F60 3.18(17) . . . . ? C59 C54 C55 C56 -1.06(16) . . . . ? B53 C54 C55 C56 -176.63(10) . . . . ? F60 C55 C56 F61 1.76(16) . . . . ? C54 C55 C56 F61 -178.41(10) . . . . ? F60 C55 C56 C57 -179.70(10) . . . . ? C54 C55 C56 C57 0.13(18) . . . . ? F61 C56 C57 F62 0.18(18) . . . . ? C55 C56 C57 F62 -178.36(11) . . . . ? F61 C56 C57 C58 178.83(11) . . . . ? C55 C56 C57 C58 0.30(18) . . . . ? F62 C57 C58 F63 -0.08(18) . . . . ? C56 C57 C58 F63 -178.73(11) . . . . ? F62 C57 C58 C59 178.94(11) . . . . ? C56 C57 C58 C59 0.29(18) . . . . ? F63 C58 C59 F64 -1.19(16) . . . . ? C57 C58 C59 F64 179.79(10) . . . . ? F63 C58 C59 C54 177.63(10) . . . . ? C57 C58 C59 C54 -1.38(18) . . . . ? C55 C54 C59 F64 -179.51(9) . . . . ? B53 C54 C59 F64 -3.61(15) . . . . ? C55 C54 C59 C58 1.70(16) . . . . ? B53 C54 C59 C58 177.60(10) . . . . ? C54 B53 C65 C70 111.29(12) . . . . ? C76 B53 C65 C70 -11.15(15) . . . . ? C52 B53 C65 C70 -128.11(11) . . . . ? C54 B53 C65 C66 -61.10(12) . . . . ? C76 B53 C65 C66 176.46(9) . . . . ? C52 B53 C65 C66 59.51(12) . . . . ? C70 C65 C66 F71 -176.64(9) . . . . ? B53 C65 C66 F71 -3.18(15) . . . . ? C70 C65 C66 C67 1.53(16) . . . . ? B53 C65 C66 C67 174.99(10) . . . . ? F71 C66 C67 F72 -1.41(16) . . . . ? C65 C66 C67 F72 -179.63(10) . . . . ? F71 C66 C67 C68 176.92(10) . . . . ? C65 C66 C67 C68 -1.30(18) . . . . ? F72 C67 C68 F73 0.58(18) . . . . ? C66 C67 C68 F73 -177.75(10) . . . . ? F72 C67 C68 C69 178.60(11) . . . . ? C66 C67 C68 C69 0.27(18) . . . . ? F73 C68 C69 F74 1.25(17) . . . . ? C67 C68 C69 F74 -176.79(10) . . . . ? F73 C68 C69 C70 178.36(10) . . . . ? C67 C68 C69 C70 0.33(17) . . . . ? F74 C69 C70 F75 -0.56(15) . . . . ? C68 C69 C70 F75 -177.64(10) . . . . ? F74 C69 C70 C65 177.09(10) . . . . ? C68 C69 C70 C65 0.00(17) . . . . ? C66 C65 C70 F75 176.63(9) . . . . ? B53 C65 C70 F75 3.84(17) . . . . ? C66 C65 C70 C69 -0.86(16) . . . . ? B53 C65 C70 C69 -173.65(10) . . . . ? C54 B53 C76 C81 3.81(15) . . . . ? C65 B53 C76 C81 121.10(11) . . . . ? C52 B53 C76 C81 -118.60(11) . . . . ? C54 B53 C76 C77 -177.74(9) . . . . ? C65 B53 C76 C77 -60.45(13) . . . . ? C52 B53 C76 C77 59.85(12) . . . . ? C81 C76 C77 F82 -179.66(9) . . . . ? B53 C76 C77 F82 1.67(15) . . . . ? C81 C76 C77 C78 -1.11(16) . . . . ? B53 C76 C77 C78 -179.78(10) . . . . ? F82 C77 C78 F83 -2.33(16) . . . . ? C76 C77 C78 F83 179.07(11) . . . . ? F82 C77 C78 C79 178.59(10) . . . . ? C76 C77 C78 C79 -0.01(18) . . . . ? F83 C78 C79 F84 -0.95(17) . . . . ? C77 C78 C79 F84 178.14(10) . . . . ? F83 C78 C79 C80 -178.67(10) . . . . ? C77 C78 C79 C80 0.42(17) . . . . ? F84 C79 C80 F85 -0.62(17) . . . . ? C78 C79 C80 F85 177.08(10) . . . . ? F84 C79 C80 C81 -177.33(10) . . . . ? C78 C79 C80 C81 0.36(17) . . . . ? F85 C80 C81 F86 -0.59(15) . . . . ? C79 C80 C81 F86 176.11(10) . . . . ? F85 C80 C81 C76 -178.38(10) . . . . ? C79 C80 C81 C76 -1.68(17) . . . . ? C77 C76 C81 F86 -175.68(9) . . . . ? B53 C76 C81 F86 2.86(17) . . . . ? C77 C76 C81 C80 1.96(16) . . . . ? B53 C76 C81 C80 -179.50(10) . . . . ? F87 C88 C89 C90 -176.49(17) . . . . ? C93 C88 C89 C90 -0.1(2) . . . . ? C88 C89 C90 C91 0.3(2) . . . . ? C89 C90 C91 F94 173.7(4) . . . . ? C89 C90 C91 C92 0.1(2) . . . . ? F94 C91 C92 F95 15.2(4) . . . . ? C90 C91 C92 F95 -169.8(3) . . . . ? F94 C91 C92 C93 -175.7(3) . . . . ? C90 C91 C92 C93 -0.7(2) . . . . ? F95 C92 C93 C88 170.4(3) . . . . ? C91 C92 C93 C88 0.9(3) . . . . ? F87 C88 C93 C92 176.14(17) . . . . ? C89 C88 C93 C92 -0.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 33.16 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.445 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.053 data_04270 _database_code_depnum_ccdc_archive 'CCDC 260838' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _exptl_crystal_id MSC04270 _audit_creation_date 10/11/2004 _chemical_formula_structural ; TiCl(C35H53N2)(C12H17N); 1.5CH2Cl2 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48.50 H73 Cl4 N3 Ti' _chemical_formula_weight 887.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.8762(7) _cell_length_b 20.6426(10) _cell_length_c 18.4262(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.511(2) _cell_angle_gamma 90.00 _cell_volume 4830.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 126(2) _cell_measurement_reflns_used 1726 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.02 _exptl_crystal_description 'irregular fragment' _exptl_crystal_colour red/orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1900 _exptl_absorpt_coefficient_mu 0.433 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; _diffrn_ambient_temperature 126(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details ' 0.30 degree frames measured for 2.17 seconds each' _diffrn_measurement_method '\w scans' _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 22542 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.1080 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 27.51 _reflns_number_total 11082 _reflns_number_gt 6340 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999), XTEL (local program)' _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^)+(0.0119P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11082 _refine_ls_number_parameters 807 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0842 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.0824 _refine_ls_wR_factor_gt 0.0712 _refine_ls_goodness_of_fit_ref 0.824 _refine_ls_restrained_S_all 0.824 _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 0.40741(3) 0.210430(16) 0.76064(2) 0.01613(9) Uani 1 1 d . . . N2 N 0.28667(14) 0.16952(7) 0.79598(9) 0.0165(4) Uani 1 1 d . . . C3 C 0.27567(18) 0.10773(9) 0.76739(11) 0.0172(5) Uani 1 1 d . . . C4 C 0.36397(18) 0.07271(10) 0.75849(11) 0.0182(5) Uani 1 1 d . . . C5 C 0.47565(17) 0.07977(9) 0.78257(11) 0.0164(5) Uani 1 1 d . . . N6 N 0.51712(14) 0.13863(7) 0.79218(8) 0.0154(4) Uani 1 1 d . . . C7 C 0.21495(17) 0.19832(9) 0.83842(11) 0.0176(5) Uani 1 1 d . . . C8 C 0.14688(18) 0.24840(9) 0.80868(11) 0.0189(5) Uani 1 1 d . . . C9 C 0.08097(18) 0.27600(10) 0.85295(12) 0.0220(5) Uani 1 1 d . . . C10 C 0.08091(19) 0.25482(11) 0.92410(13) 0.0253(5) Uani 1 1 d . . . C11 C 0.14978(19) 0.20648(11) 0.95278(12) 0.0252(5) Uani 1 1 d . . . C12 C 0.21860(18) 0.17780(10) 0.91169(11) 0.0210(5) Uani 1 1 d . . . C13 C 0.2969(2) 0.12740(12) 0.94694(13) 0.0307(6) Uani 1 1 d . . . C14 C 0.2434(3) 0.06663(15) 0.9685(2) 0.0544(10) Uani 1 1 d . . . C15 C 0.3694(3) 0.15540(17) 1.01332(17) 0.0450(8) Uani 1 1 d . . . C16 C 0.14057(18) 0.27129(10) 0.72913(11) 0.0205(5) Uani 1 1 d . . . C17 C 0.1978(2) 0.33590(12) 0.72560(15) 0.0274(6) Uani 1 1 d . . . C18 C 0.0277(2) 0.27744(13) 0.68840(14) 0.0289(6) Uani 1 1 d . . . C19 C 0.16845(18) 0.07476(9) 0.73672(12) 0.0215(5) Uani 1 1 d . . . C20 C 0.0712(2) 0.10194(12) 0.76403(16) 0.0295(6) Uani 1 1 d . . . H20 H 0.823(2) 0.1982(10) 0.9284(12) 0.039(7) Uiso 1 1 d . . . C21 C 0.1530(2) 0.08414(14) 0.65289(14) 0.0334(6) Uani 1 1 d . . . C22 C 0.1700(2) 0.00202(11) 0.75395(17) 0.0328(6) Uani 1 1 d . . . C23 C 0.53329(18) 0.01337(9) 0.79758(11) 0.0191(5) Uani 1 1 d . . . C24 C 0.4797(2) -0.02010(12) 0.85668(14) 0.0259(6) Uani 1 1 d . . . C25 C 0.5172(2) -0.02811(11) 0.72748(13) 0.0237(5) Uani 1 1 d . . . H25 H 0.6710(18) 0.4417(9) 0.8087(11) 0.027(6) Uiso 1 1 d . . . C26 C 0.6514(2) 0.01489(12) 0.82757(14) 0.0244(5) Uani 1 1 d . . . C27 C 0.62886(17) 0.15197(9) 0.80479(12) 0.0190(5) Uani 1 1 d . . . C28 C 0.67961(19) 0.17249(10) 0.87443(12) 0.0237(5) Uani 1 1 d . . . C29 C 0.7871(2) 0.18466(12) 0.88379(15) 0.0330(6) Uani 1 1 d . . . C30 C 0.8429(2) 0.17886(13) 0.82643(15) 0.0367(7) Uani 1 1 d . . . C31 C 0.7912(2) 0.16159(11) 0.75787(14) 0.0302(6) Uani 1 1 d . . . C32 C 0.68434(18) 0.14774(9) 0.74458(12) 0.0209(5) Uani 1 1 d . . . C33 C 0.6344(2) 0.12942(11) 0.66631(12) 0.0238(5) Uani 1 1 d . . . C34 C 0.6317(2) 0.18708(13) 0.61430(15) 0.0334(6) Uani 1 1 d . . . C35 C 0.6934(2) 0.07356(12) 0.63596(15) 0.0294(6) Uani 1 1 d . . . C36 C 0.6227(2) 0.17943(12) 0.93967(13) 0.0301(6) Uani 1 1 d . . . C37 C 0.6496(3) 0.12364(14) 0.99462(16) 0.0443(8) Uani 1 1 d . . . C38 C 0.6491(2) 0.24387(13) 0.97942(15) 0.0358(7) Uani 1 1 d . . . N39 N 0.44724(14) 0.27912(7) 0.81052(9) 0.0176(4) Uani 1 1 d . . . C40 C 0.49006(17) 0.33838(9) 0.83724(11) 0.0187(5) Uani 1 1 d . . . C41 C 0.57135(18) 0.36637(9) 0.80453(12) 0.0222(5) Uani 1 1 d . . . C42 C 0.6167(2) 0.42431(11) 0.83194(14) 0.0295(6) Uani 1 1 d . . . C43 C 0.5838(2) 0.45484(11) 0.89130(14) 0.0309(6) Uani 1 1 d . . . C44 C 0.5045(2) 0.42818(10) 0.92240(14) 0.0271(6) Uani 1 1 d . . . C45 C 0.45486(18) 0.37013(9) 0.89668(12) 0.0213(5) Uani 1 1 d . . . C46 C 0.3655(2) 0.34483(10) 0.93331(12) 0.0246(5) Uani 1 1 d . . . C47 C 0.4015(3) 0.33353(15) 1.01602(15) 0.0391(7) Uani 1 1 d . . . C48 C 0.2731(2) 0.39169(13) 0.92377(16) 0.0328(6) Uani 1 1 d . . . C49 C 0.6066(2) 0.33543(11) 0.73763(13) 0.0282(6) Uani 1 1 d . . . C50 C 0.7251(3) 0.33761(16) 0.7391(2) 0.0505(9) Uani 1 1 d . . . C51 C 0.5468(3) 0.36710(15) 0.66808(16) 0.0511(9) Uani 1 1 d . . . Cl52 Cl 0.37234(5) 0.22680(3) 0.63584(3) 0.02801(14) Uani 1 1 d . . . Cl53 Cl 0.89310(8) 0.38449(4) 0.92374(4) 0.0693(3) Uani 1 1 d . . . C54 C 0.8305(3) 0.39992(14) 0.99961(15) 0.0409(7) Uani 1 1 d . . . Cl55 Cl 0.89114(6) 0.46443(3) 1.05185(4) 0.04682(19) Uani 1 1 d . . . Cl56 Cl 0.0471(7) -0.0442(7) 1.0362(13) 0.164(4) Uani 0.372(16) 1 d P . . C57 C 0.0224(6) -0.0344(4) 0.9767(4) 0.065(2) Uiso 0.50 1 d P . . H58 H 0.3481(15) 0.0325(8) 0.7357(9) 0.009(5) Uiso 1 1 d . . . H59 H 0.0359(17) 0.3092(9) 0.8327(11) 0.024(6) Uiso 1 1 d . . . H60 H 0.0341(18) 0.2750(9) 0.9545(11) 0.028(6) Uiso 1 1 d . . . H61 H 0.1513(18) 0.1931(9) 1.0010(12) 0.033(7) Uiso 1 1 d . . . H62 H 0.3355(18) 0.1155(10) 0.9144(11) 0.026(7) Uiso 1 1 d . . . H63 H 0.297(2) 0.0313(12) 0.9888(13) 0.053(8) Uiso 1 1 d . . . H64 H 0.202(3) 0.0475(13) 0.9283(16) 0.076(11) Uiso 1 1 d . . . H65 H 0.199(3) 0.0739(13) 1.0064(16) 0.068(11) Uiso 1 1 d . . . H66 H 0.321(2) 0.1625(12) 1.0518(14) 0.053(9) Uiso 1 1 d . . . H67 H 0.404(3) 0.1957(14) 1.0058(15) 0.077(11) Uiso 1 1 d . . . H68 H 0.420(2) 0.1224(10) 1.0303(12) 0.035(7) Uiso 1 1 d . . . H69 H 0.1754(15) 0.2390(8) 0.7030(9) 0.001(5) Uiso 1 1 d . . . H70 H 0.270(2) 0.3357(11) 0.7507(12) 0.038(7) Uiso 1 1 d . . . H71 H 0.1613(19) 0.3712(10) 0.7488(12) 0.036(7) Uiso 1 1 d . . . H72 H 0.1994(17) 0.3466(9) 0.6759(12) 0.021(6) Uiso 1 1 d . . . H73 H -0.0097(19) 0.3088(10) 0.7098(12) 0.032(7) Uiso 1 1 d . . . H74 H 0.021(2) 0.2875(10) 0.6346(13) 0.043(7) Uiso 1 1 d . . . H75 H -0.0086(19) 0.2380(10) 0.6879(11) 0.030(7) Uiso 1 1 d . . . H76 H 0.0768(19) 0.0969(10) 0.8169(13) 0.037(7) Uiso 1 1 d . . . H77 H 0.0575(19) 0.1482(11) 0.7506(12) 0.038(7) Uiso 1 1 d . . . H78 H 0.0105(18) 0.0761(9) 0.7396(11) 0.023(6) Uiso 1 1 d . . . H79 H 0.1483(19) 0.1327(11) 0.6395(12) 0.043(7) Uiso 1 1 d . . . H80 H 0.084(2) 0.0669(10) 0.6307(12) 0.033(7) Uiso 1 1 d . . . H81 H 0.210(2) 0.0642(11) 0.6312(13) 0.046(8) Uiso 1 1 d . . . H82 H 0.101(2) -0.0158(11) 0.7380(13) 0.052(8) Uiso 1 1 d . . . H83 H 0.219(2) -0.0236(10) 0.7309(12) 0.032(7) Uiso 1 1 d . . . H84 H 0.192(2) -0.0087(10) 0.8084(13) 0.043(8) Uiso 1 1 d . . . H85 H 0.406(2) -0.0258(10) 0.8414(12) 0.038(7) Uiso 1 1 d . . . H86 H 0.5117(17) -0.0641(9) 0.8673(10) 0.022(6) Uiso 1 1 d . . . H87 H 0.4916(18) 0.0022(9) 0.9038(11) 0.025(6) Uiso 1 1 d . . . H88 H 0.447(2) -0.0402(10) 0.7118(12) 0.031(7) Uiso 1 1 d . . . H89 H 0.5445(17) -0.0047(9) 0.6858(11) 0.023(6) Uiso 1 1 d . . . H90 H 0.5550(17) -0.0678(9) 0.7369(10) 0.016(5) Uiso 1 1 d . . . H91 H 0.6717(19) -0.0268(11) 0.8401(12) 0.035(7) Uiso 1 1 d . . . H92 H 0.6934(18) 0.0290(9) 0.7912(12) 0.027(6) Uiso 1 1 d . . . H93 H 0.6662(18) 0.0412(9) 0.8720(12) 0.027(6) Uiso 1 1 d . . . H95 H 0.913(2) 0.1911(11) 0.8338(13) 0.046(8) Uiso 1 1 d . . . H96 H 0.8277(18) 0.1612(10) 0.7177(12) 0.032(7) Uiso 1 1 d . . . H97 H 0.5656(18) 0.1152(9) 0.6668(11) 0.021(6) Uiso 1 1 d . . . H98 H 0.706(2) 0.2010(10) 0.6114(12) 0.035(7) Uiso 1 1 d . . . H99 H 0.5867(19) 0.2232(10) 0.6295(11) 0.032(7) Uiso 1 1 d . . . H100 H 0.5952(18) 0.1729(9) 0.5641(12) 0.031(7) Uiso 1 1 d . . . H101 H 0.761(2) 0.0880(10) 0.6266(12) 0.033(7) Uiso 1 1 d . . . H102 H 0.7029(18) 0.0370(10) 0.6689(12) 0.029(6) Uiso 1 1 d . . . H103 H 0.657(2) 0.0586(10) 0.5879(13) 0.040(7) Uiso 1 1 d . . . H104 H 0.548(2) 0.1771(10) 0.9216(12) 0.040(7) Uiso 1 1 d . . . H105 H 0.613(2) 0.1303(10) 1.0362(13) 0.041(7) Uiso 1 1 d . . . H106 H 0.622(2) 0.0811(12) 0.9732(13) 0.056(8) Uiso 1 1 d . . . H107 H 0.726(2) 0.1226(11) 1.0159(13) 0.046(8) Uiso 1 1 d . . . H108 H 0.605(2) 0.2475(11) 1.0215(13) 0.050(8) Uiso 1 1 d . . . H109 H 0.633(2) 0.2804(11) 0.9464(13) 0.046(8) Uiso 1 1 d . . . H110 H 0.725(2) 0.2465(11) 1.0030(13) 0.046(8) Uiso 1 1 d . . . H111 H 0.6129(19) 0.4956(10) 0.9084(12) 0.042(7) Uiso 1 1 d . . . H112 H 0.4790(17) 0.4479(9) 0.9634(11) 0.023(6) Uiso 1 1 d . . . H113 H 0.3436(16) 0.3023(9) 0.9136(10) 0.016(5) Uiso 1 1 d . . . H114 H 0.421(2) 0.3774(13) 1.0442(14) 0.072(10) Uiso 1 1 d . . . H115 H 0.347(2) 0.3113(11) 1.0371(13) 0.040(8) Uiso 1 1 d . . . H116 H 0.459(2) 0.3037(11) 1.0250(13) 0.047(8) Uiso 1 1 d . . . H117 H 0.288(2) 0.4345(11) 0.9470(12) 0.043(7) Uiso 1 1 d . . . H118 H 0.246(2) 0.3996(12) 0.8726(15) 0.062(9) Uiso 1 1 d . . . H119 H 0.214(2) 0.3759(10) 0.9470(12) 0.039(7) Uiso 1 1 d . . . H120 H 0.5895(16) 0.2900(9) 0.7392(10) 0.012(5) Uiso 1 1 d . . . H121 H 0.750(2) 0.3827(13) 0.7345(13) 0.059(9) Uiso 1 1 d . . . H122 H 0.740(2) 0.3172(12) 0.6892(15) 0.062(9) Uiso 1 1 d . . . H123 H 0.764(3) 0.3219(17) 0.7799(19) 0.110(17) Uiso 1 1 d . . . H124 H 0.5685(19) 0.4145(11) 0.6678(11) 0.035(7) Uiso 1 1 d . . . H125 H 0.558(2) 0.3461(10) 0.6216(13) 0.041(7) Uiso 1 1 d . . . H126 H 0.464(2) 0.3626(12) 0.6645(14) 0.063(10) Uiso 1 1 d . . . H127 H 0.847(2) 0.3636(12) 1.0302(14) 0.064(9) Uiso 1 1 d . . . H128 H 0.758(2) 0.4139(12) 0.9838(13) 0.050(8) Uiso 1 1 d . . . Cl1 Cl 0.0655(3) -0.03211(13) 1.0689(2) 0.0705(12) Uani 0.628(16) 1 d P . . 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 0.0165(2) 0.01618(18) 0.0160(2) 0.00048(16) 0.00352(16) 0.00045(17) N2 0.0166(10) 0.0160(8) 0.0166(9) 0.0003(7) 0.0015(8) 0.0013(8) C3 0.0189(12) 0.0191(10) 0.0137(11) 0.0026(9) 0.0026(9) -0.0016(9) C4 0.0210(13) 0.0137(10) 0.0201(12) -0.0042(9) 0.0038(10) -0.0030(9) C5 0.0184(12) 0.0175(10) 0.0140(11) 0.0005(9) 0.0048(9) 0.0017(9) N6 0.0148(10) 0.0190(8) 0.0129(9) -0.0016(7) 0.0033(8) -0.0012(8) C7 0.0167(12) 0.0186(10) 0.0174(11) -0.0039(9) 0.0026(9) -0.0029(9) C8 0.0173(12) 0.0181(10) 0.0209(12) -0.0021(9) 0.0017(10) -0.0020(9) C9 0.0192(13) 0.0219(11) 0.0240(12) -0.0056(10) 0.0004(10) 0.0035(10) C10 0.0197(13) 0.0306(12) 0.0270(13) -0.0096(11) 0.0083(11) -0.0003(11) C11 0.0275(14) 0.0343(13) 0.0140(12) -0.0021(11) 0.0042(10) -0.0013(11) C12 0.0223(13) 0.0219(11) 0.0191(12) -0.0002(9) 0.0039(10) -0.0007(10) C13 0.0365(17) 0.0355(14) 0.0218(13) 0.0066(11) 0.0098(12) 0.0102(12) C14 0.062(3) 0.0344(16) 0.059(2) 0.0158(16) -0.011(2) -0.0028(17) C15 0.0307(18) 0.056(2) 0.0435(19) 0.0113(16) -0.0070(15) 0.0056(16) C16 0.0206(13) 0.0213(11) 0.0193(12) -0.0003(9) 0.0021(10) 0.0057(10) C17 0.0280(16) 0.0287(13) 0.0248(14) 0.0050(11) 0.0019(12) 0.0037(12) C18 0.0262(15) 0.0327(15) 0.0257(14) 0.0029(12) -0.0024(11) 0.0049(12) C19 0.0191(13) 0.0176(10) 0.0265(13) -0.0033(9) 0.0001(10) 0.0001(10) C20 0.0171(14) 0.0286(14) 0.0424(17) -0.0101(13) 0.0041(12) -0.0038(11) C21 0.0264(16) 0.0413(16) 0.0307(15) -0.0041(13) -0.0008(13) -0.0088(13) C22 0.0219(15) 0.0205(12) 0.0549(19) -0.0007(13) 0.0031(14) -0.0047(11) C23 0.0200(13) 0.0169(10) 0.0201(11) 0.0026(9) 0.0026(10) 0.0020(9) C24 0.0279(16) 0.0248(13) 0.0246(14) 0.0058(11) 0.0029(12) 0.0018(12) C25 0.0237(15) 0.0170(11) 0.0304(14) -0.0007(10) 0.0046(12) 0.0035(11) C26 0.0217(14) 0.0211(12) 0.0290(14) 0.0023(11) 0.0002(11) 0.0062(11) C27 0.0158(12) 0.0163(10) 0.0251(12) 0.0029(9) 0.0038(10) 0.0015(9) C28 0.0204(13) 0.0247(11) 0.0254(13) -0.0037(10) 0.0020(10) -0.0021(10) C29 0.0206(14) 0.0441(15) 0.0325(15) -0.0091(12) -0.0008(12) -0.0032(12) C30 0.0178(15) 0.0446(15) 0.0483(18) -0.0094(13) 0.0073(13) -0.0095(13) C31 0.0210(14) 0.0352(13) 0.0371(16) -0.0013(12) 0.0134(12) -0.0021(11) C32 0.0201(13) 0.0181(10) 0.0252(12) 0.0000(9) 0.0058(10) 0.0013(10) C33 0.0216(14) 0.0272(12) 0.0244(13) 0.0026(10) 0.0090(11) 0.0008(11) C34 0.0374(18) 0.0367(15) 0.0289(15) 0.0067(12) 0.0139(14) 0.0105(14) C35 0.0322(17) 0.0294(14) 0.0290(15) -0.0019(12) 0.0124(13) 0.0053(12) C36 0.0205(14) 0.0456(15) 0.0228(13) -0.0082(11) -0.0010(11) -0.0038(12) C37 0.062(2) 0.0429(17) 0.0303(16) -0.0051(14) 0.0158(17) -0.0067(17) C38 0.0367(18) 0.0397(15) 0.0284(15) -0.0061(13) -0.0021(13) 0.0101(14) N39 0.0182(10) 0.0175(9) 0.0181(9) 0.0017(7) 0.0055(8) -0.0008(8) C40 0.0179(12) 0.0159(10) 0.0220(12) 0.0019(9) 0.0024(10) 0.0012(9) C41 0.0229(13) 0.0182(10) 0.0265(12) 0.0016(10) 0.0067(10) 0.0009(10) C42 0.0234(14) 0.0242(12) 0.0427(16) 0.0014(11) 0.0102(12) -0.0072(11) C43 0.0286(15) 0.0192(12) 0.0440(16) -0.0092(11) 0.0031(12) -0.0045(11) C44 0.0280(15) 0.0215(12) 0.0321(14) -0.0061(11) 0.0052(12) 0.0013(11) C45 0.0221(13) 0.0177(10) 0.0240(12) 0.0017(9) 0.0031(10) 0.0014(10) C46 0.0281(15) 0.0205(11) 0.0270(13) -0.0052(10) 0.0097(11) -0.0025(11) C47 0.0376(19) 0.0475(18) 0.0357(16) 0.0101(14) 0.0166(14) 0.0110(15) C48 0.0257(16) 0.0359(15) 0.0370(16) -0.0051(13) 0.0058(13) -0.0017(12) C49 0.0311(16) 0.0219(12) 0.0350(14) 0.0005(11) 0.0154(12) -0.0069(11) C50 0.041(2) 0.0465(18) 0.073(3) -0.0198(19) 0.034(2) -0.0159(16) C51 0.086(3) 0.0378(17) 0.0326(17) 0.0029(14) 0.0196(18) 0.0005(18) Cl52 0.0319(4) 0.0341(3) 0.0178(3) 0.0026(2) 0.0035(2) 0.0040(3) Cl53 0.0944(8) 0.0739(5) 0.0419(4) -0.0073(4) 0.0177(5) 0.0407(5) C54 0.047(2) 0.0415(16) 0.0336(16) 0.0052(13) 0.0055(15) -0.0030(15) Cl55 0.0528(5) 0.0473(4) 0.0410(4) -0.0051(3) 0.0097(4) -0.0023(4) Cl56 0.063(3) 0.182(7) 0.238(12) 0.124(6) -0.001(6) -0.014(4) Cl1 0.073(2) 0.0496(15) 0.096(2) 0.0061(13) 0.0334(15) -0.0015(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 Ti1 N39 1.7212(16) . ? Ti1 N2 1.9720(18) . ? Ti1 N6 2.0637(17) . ? Ti1 Cl52 2.2941(6) . ? N2 C3 1.378(2) . ? N2 C7 1.434(3) . ? C3 C4 1.380(3) . ? C3 C19 1.559(3) . ? C4 C5 1.441(3) . ? C4 H58 0.937(17) . ? C5 N6 1.327(2) . ? C5 C23 1.561(3) . ? N6 C27 1.445(3) . ? C7 C8 1.407(3) . ? C7 C12 1.408(3) . ? C8 C9 1.392(3) . ? C8 C16 1.529(3) . ? C9 C10 1.382(3) . ? C9 H59 0.93(2) . ? C10 C11 1.381(3) . ? C10 H60 0.98(2) . ? C11 C12 1.389(3) . ? C11 H61 0.93(2) . ? C12 C13 1.518(3) . ? C13 C14 1.515(4) . ? C13 C15 1.524(4) . ? C13 H62 0.87(2) . ? C14 H63 1.03(3) . ? C14 H64 0.93(3) . ? C14 H65 0.99(3) . ? C15 H66 1.03(3) . ? C15 H67 0.96(3) . ? C15 H68 0.96(2) . ? C16 C18 1.527(3) . ? C16 C17 1.530(3) . ? C16 H69 0.973(17) . ? C17 H70 0.96(2) . ? C17 H71 1.00(2) . ? C17 H72 0.95(2) . ? C18 H73 0.93(2) . ? C18 H74 1.00(2) . ? C18 H75 0.94(2) . ? C19 C20 1.531(3) . ? C19 C22 1.534(3) . ? C19 C21 1.537(3) . ? C20 H76 0.97(2) . ? C20 H77 1.00(2) . ? C20 H78 0.99(2) . ? C21 H79 1.03(2) . ? C21 H80 0.98(2) . ? C21 H81 0.99(3) . ? C22 H82 0.97(3) . ? C22 H83 0.98(2) . ? C22 H84 1.02(2) . ? C23 C26 1.530(3) . ? C23 C25 1.535(3) . ? C23 C24 1.545(3) . ? C24 H85 0.96(3) . ? C24 H86 1.003(19) . ? C24 H87 0.97(2) . ? C25 H88 0.94(2) . ? C25 H89 1.02(2) . ? C25 H90 0.954(19) . ? C26 H91 0.92(2) . ? C26 H92 0.97(2) . ? C26 H93 0.98(2) . ? C27 C28 1.406(3) . ? C27 C32 1.418(3) . ? C28 C29 1.389(3) . ? C28 C36 1.514(3) . ? C29 C30 1.378(3) . ? C29 H20 0.92(2) . ? C30 C31 1.374(3) . ? C30 H95 0.92(3) . ? C31 C32 1.387(3) . ? C31 H96 0.94(2) . ? C32 C33 1.526(3) . ? C33 C34 1.525(3) . ? C33 C35 1.536(3) . ? C33 H97 0.94(2) . ? C34 H98 1.00(2) . ? C34 H99 1.01(2) . ? C34 H100 1.01(2) . ? C35 H101 0.96(2) . ? C35 H102 0.96(2) . ? C35 H103 0.98(2) . ? C36 C38 1.529(3) . ? C36 C37 1.535(4) . ? C36 H104 0.97(2) . ? C37 H105 0.97(2) . ? C37 H106 1.00(3) . ? C37 H107 1.00(3) . ? C38 H108 1.04(3) . ? C38 H109 0.97(2) . ? C38 H110 1.00(3) . ? N39 C40 1.398(2) . ? C40 C45 1.414(3) . ? C40 C41 1.415(3) . ? C41 C42 1.389(3) . ? C41 C49 1.523(3) . ? C42 C43 1.387(3) . ? C42 H25 0.95(2) . ? C43 C44 1.366(3) . ? C43 H111 0.95(2) . ? C44 C45 1.404(3) . ? C44 H112 0.96(2) . ? C45 C46 1.519(3) . ? C46 C48 1.521(3) . ? C46 C47 1.536(3) . ? C46 H113 0.974(18) . ? C47 H114 1.05(3) . ? C47 H115 0.97(3) . ? C47 H116 0.96(3) . ? C48 H117 0.99(2) . ? C48 H118 0.96(3) . ? C48 H119 0.99(3) . ? C49 C50 1.522(4) . ? C49 C51 1.529(4) . ? C49 H120 0.965(17) . ? C50 H121 0.99(3) . ? C50 H122 1.06(3) . ? C50 H123 0.89(3) . ? C51 H124 1.02(2) . ? C51 H125 0.99(2) . ? C51 H126 1.07(3) . ? Cl53 C54 1.754(3) . ? C54 Cl55 1.750(3) . ? C54 H127 0.94(3) . ? C54 H128 0.97(3) . ? Cl56 Cl1 0.66(2) . ? Cl56 C57 1.11(2) . ? Cl56 C57 1.849(12) 3_557 ? Cl56 Cl56 2.459(16) 3_557 ? C57 Cl1 1.697(8) . ? C57 C57 1.804(14) 3_557 ? C57 Cl56 1.849(12) 3_557 ? C57 Cl1 1.887(10) 3_557 ? Cl1 C57 1.887(10) 3_557 ? 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 N39 Ti1 N2 110.98(8) . . ? N39 Ti1 N6 108.15(7) . . ? N2 Ti1 N6 98.03(7) . . ? N39 Ti1 Cl52 113.94(6) . . ? N2 Ti1 Cl52 111.02(5) . . ? N6 Ti1 Cl52 113.60(5) . . ? C3 N2 C7 123.86(17) . . ? C3 N2 Ti1 107.88(14) . . ? C7 N2 Ti1 128.06(12) . . ? N2 C3 C4 119.7(2) . . ? N2 C3 C19 124.85(19) . . ? C4 C3 C19 115.20(17) . . ? C3 C4 C5 135.3(2) . . ? C3 C4 H58 113.2(12) . . ? C5 C4 H58 111.1(12) . . ? N6 C5 C4 119.53(19) . . ? N6 C5 C23 127.65(19) . . ? C4 C5 C23 112.76(17) . . ? C5 N6 C27 124.31(17) . . ? C5 N6 Ti1 112.23(14) . . ? C27 N6 Ti1 121.69(12) . . ? C8 C7 C12 121.0(2) . . ? C8 C7 N2 120.54(18) . . ? C12 C7 N2 118.40(18) . . ? C9 C8 C7 118.2(2) . . ? C9 C8 C16 119.61(19) . . ? C7 C8 C16 122.10(19) . . ? C10 C9 C8 121.5(2) . . ? C10 C9 H59 120.9(13) . . ? C8 C9 H59 117.7(13) . . ? C11 C10 C9 119.4(2) . . ? C11 C10 H60 120.3(12) . . ? C9 C10 H60 120.3(12) . . ? C10 C11 C12 121.8(2) . . ? C10 C11 H61 119.5(14) . . ? C12 C11 H61 118.7(14) . . ? C11 C12 C7 118.1(2) . . ? C11 C12 C13 119.8(2) . . ? C7 C12 C13 122.1(2) . . ? C14 C13 C12 112.4(2) . . ? C14 C13 C15 110.4(2) . . ? C12 C13 C15 111.0(2) . . ? C14 C13 H62 106.4(14) . . ? C12 C13 H62 108.1(14) . . ? C15 C13 H62 108.3(15) . . ? C13 C14 H63 111.8(15) . . ? C13 C14 H64 111.8(19) . . ? H63 C14 H64 105(2) . . ? C13 C14 H65 113.8(17) . . ? H63 C14 H65 107(2) . . ? H64 C14 H65 108(3) . . ? C13 C15 H66 104.1(15) . . ? C13 C15 H67 116.5(18) . . ? H66 C15 H67 109(2) . . ? C13 C15 H68 106.7(13) . . ? H66 C15 H68 109.7(19) . . ? H67 C15 H68 111(2) . . ? C18 C16 C8 113.1(2) . . ? C18 C16 C17 109.45(19) . . ? C8 C16 C17 111.12(18) . . ? C18 C16 H69 107.0(11) . . ? C8 C16 H69 107.9(10) . . ? C17 C16 H69 108.1(10) . . ? C16 C17 H70 114.0(14) . . ? C16 C17 H71 110.6(13) . . ? H70 C17 H71 106.3(18) . . ? C16 C17 H72 109.4(12) . . ? H70 C17 H72 107.1(19) . . ? H71 C17 H72 109.3(17) . . ? C16 C18 H73 111.4(14) . . ? C16 C18 H74 114.7(15) . . ? H73 C18 H74 108.2(18) . . ? C16 C18 H75 111.4(14) . . ? H73 C18 H75 108(2) . . ? H74 C18 H75 102.2(18) . . ? C20 C19 C22 105.9(2) . . ? C20 C19 C21 107.9(2) . . ? C22 C19 C21 109.0(2) . . ? C20 C19 C3 116.37(18) . . ? C22 C19 C3 111.83(19) . . ? C21 C19 C3 105.60(19) . . ? C19 C20 H76 111.2(14) . . ? C19 C20 H77 113.0(14) . . ? H76 C20 H77 109.4(18) . . ? C19 C20 H78 106.2(12) . . ? H76 C20 H78 108.7(18) . . ? H77 C20 H78 108.0(18) . . ? C19 C21 H79 110.8(12) . . ? C19 C21 H80 109.5(13) . . ? H79 C21 H80 103.9(18) . . ? C19 C21 H81 112.0(14) . . ? H79 C21 H81 109(2) . . ? H80 C21 H81 111.4(19) . . ? C19 C22 H82 109.3(15) . . ? C19 C22 H83 115.3(13) . . ? H82 C22 H83 107.3(19) . . ? C19 C22 H84 114.1(13) . . ? H82 C22 H84 108(2) . . ? H83 C22 H84 102.7(19) . . ? C26 C23 C25 107.64(19) . . ? C26 C23 C24 106.71(19) . . ? C25 C23 C24 109.26(19) . . ? C26 C23 C5 117.45(18) . . ? C25 C23 C5 110.28(17) . . ? C24 C23 C5 105.23(18) . . ? C23 C24 H85 112.8(14) . . ? C23 C24 H86 109.0(12) . . ? H85 C24 H86 107.7(18) . . ? C23 C24 H87 113.3(12) . . ? H85 C24 H87 108.8(19) . . ? H86 C24 H87 104.8(16) . . ? C23 C25 H88 113.4(14) . . ? C23 C25 H89 110.8(11) . . ? H88 C25 H89 109.3(18) . . ? C23 C25 H90 109.4(11) . . ? H88 C25 H90 105.3(17) . . ? H89 C25 H90 108.4(16) . . ? C23 C26 H91 107.2(15) . . ? C23 C26 H92 112.9(13) . . ? H91 C26 H92 106.7(19) . . ? C23 C26 H93 111.1(14) . . ? H91 C26 H93 107.5(18) . . ? H92 C26 H93 111.1(18) . . ? C28 C27 C32 121.0(2) . . ? C28 C27 N6 120.29(19) . . ? C32 C27 N6 118.64(18) . . ? C29 C28 C27 118.1(2) . . ? C29 C28 C36 119.2(2) . . ? C27 C28 C36 122.7(2) . . ? C30 C29 C28 121.6(2) . . ? C30 C29 H20 117.5(16) . . ? C28 C29 H20 120.8(16) . . ? C31 C30 C29 119.5(3) . . ? C31 C30 H95 121.3(16) . . ? C29 C30 H95 118.9(15) . . ? C30 C31 C32 122.1(2) . . ? C30 C31 H96 119.8(14) . . ? C32 C31 H96 118.0(14) . . ? C31 C32 C27 117.6(2) . . ? C31 C32 C33 117.9(2) . . ? C27 C32 C33 124.5(2) . . ? C34 C33 C32 111.3(2) . . ? C34 C33 C35 108.6(2) . . ? C32 C33 C35 111.9(2) . . ? C34 C33 H97 109.2(13) . . ? C32 C33 H97 108.7(13) . . ? C35 C33 H97 107.1(12) . . ? C33 C34 H98 109.5(13) . . ? C33 C34 H99 110.8(12) . . ? H98 C34 H99 113.3(17) . . ? C33 C34 H100 107.9(12) . . ? H98 C34 H100 109.7(18) . . ? H99 C34 H100 105.5(18) . . ? C33 C35 H101 110.4(13) . . ? C33 C35 H102 112.1(13) . . ? H101 C35 H102 109(2) . . ? C33 C35 H103 111.8(14) . . ? H101 C35 H103 104.4(19) . . ? H102 C35 H103 108.4(17) . . ? C28 C36 C38 111.3(2) . . ? C28 C36 C37 111.5(2) . . ? C38 C36 C37 109.2(2) . . ? C28 C36 H104 108.0(14) . . ? C38 C36 H104 109.8(14) . . ? C37 C36 H104 107.0(14) . . ? C36 C37 H105 109.2(14) . . ? C36 C37 H106 111.7(14) . . ? H105 C37 H106 104(2) . . ? C36 C37 H107 112.1(15) . . ? H105 C37 H107 105(2) . . ? H106 C37 H107 114(2) . . ? C36 C38 H108 108.3(14) . . ? C36 C38 H109 111.5(14) . . ? H108 C38 H109 109(2) . . ? C36 C38 H110 112.2(14) . . ? H108 C38 H110 106.7(19) . . ? H109 C38 H110 109(2) . . ? C40 N39 Ti1 167.06(15) . . ? N39 C40 C45 121.36(19) . . ? N39 C40 C41 118.95(19) . . ? C45 C40 C41 119.68(19) . . ? C42 C41 C40 119.5(2) . . ? C42 C41 C49 119.5(2) . . ? C40 C41 C49 120.95(19) . . ? C43 C42 C41 120.9(2) . . ? C43 C42 H25 121.8(13) . . ? C41 C42 H25 117.3(13) . . ? C44 C43 C42 119.6(2) . . ? C44 C43 H111 119.8(15) . . ? C42 C43 H111 120.5(15) . . ? C43 C44 C45 122.2(2) . . ? C43 C44 H112 122.3(13) . . ? C45 C44 H112 115.5(13) . . ? C44 C45 C40 118.1(2) . . ? C44 C45 C46 118.7(2) . . ? C40 C45 C46 123.23(19) . . ? C45 C46 C48 111.42(19) . . ? C45 C46 C47 111.5(2) . . ? C48 C46 C47 108.3(2) . . ? C45 C46 H113 109.7(12) . . ? C48 C46 H113 110.9(12) . . ? C47 C46 H113 104.8(11) . . ? C46 C47 H114 111.5(14) . . ? C46 C47 H115 110.3(15) . . ? H114 C47 H115 110(2) . . ? C46 C47 H116 111.6(15) . . ? H114 C47 H116 111(2) . . ? H115 C47 H116 102.7(19) . . ? C46 C48 H117 115.4(15) . . ? C46 C48 H118 111.6(17) . . ? H117 C48 H118 106(2) . . ? C46 C48 H119 112.6(14) . . ? H117 C48 H119 102.4(19) . . ? H118 C48 H119 108(2) . . ? C50 C49 C41 113.9(2) . . ? C50 C49 C51 111.5(3) . . ? C41 C49 C51 108.8(2) . . ? C50 C49 H120 105.2(12) . . ? C41 C49 H120 106.5(11) . . ? C51 C49 H120 110.8(11) . . ? C49 C50 H121 111.6(17) . . ? C49 C50 H122 107.3(16) . . ? H121 C50 H122 101(2) . . ? C49 C50 H123 115(3) . . ? H121 C50 H123 105(3) . . ? H122 C50 H123 116(3) . . ? C49 C51 H124 108.3(13) . . ? C49 C51 H125 114.4(14) . . ? H124 C51 H125 109.8(18) . . ? C49 C51 H126 112.2(15) . . ? H124 C51 H126 111(2) . . ? H125 C51 H126 101(2) . . ? Cl55 C54 Cl53 110.75(17) . . ? Cl55 C54 H127 103.9(16) . . ? Cl53 C54 H127 104.0(17) . . ? Cl55 C54 H128 104.9(15) . . ? Cl53 C54 H128 111.0(15) . . ? H127 C54 H128 122(2) . . ? Cl1 Cl56 C57 146.8(18) . . ? Cl1 Cl56 C57 83.1(17) . 3_557 ? C57 Cl56 C57 70.1(7) . 3_557 ? Cl1 Cl56 Cl56 107(2) . 3_557 ? C57 Cl56 Cl56 45.0(6) . 3_557 ? C57 Cl56 Cl56 25.1(5) 3_557 3_557 ? Cl56 C57 Cl1 12.3(9) . . ? Cl56 C57 C57 74.6(10) . 3_557 ? Cl1 C57 C57 65.2(4) . 3_557 ? Cl56 C57 Cl56 109.9(7) . 3_557 ? Cl1 C57 Cl56 100.1(9) . 3_557 ? C57 C57 Cl56 35.3(8) 3_557 3_557 ? Cl56 C57 Cl1 128.7(10) . 3_557 ? Cl1 C57 Cl1 119.9(4) . 3_557 ? C57 C57 Cl1 54.7(4) 3_557 3_557 ? Cl56 C57 Cl1 20.2(7) 3_557 3_557 ? Cl56 Cl1 C57 21.0(10) . . ? Cl56 Cl1 C57 76.7(11) . 3_557 ? C57 Cl1 C57 60.1(4) . 3_557 ? 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 N39 Ti1 N2 C3 -165.23(13) . . . . ? N6 Ti1 N2 C3 -52.21(13) . . . . ? Cl52 Ti1 N2 C3 66.97(13) . . . . ? N39 Ti1 N2 C7 19.85(18) . . . . ? N6 Ti1 N2 C7 132.88(16) . . . . ? Cl52 Ti1 N2 C7 -107.95(16) . . . . ? C7 N2 C3 C4 -149.8(2) . . . . ? Ti1 N2 C3 C4 35.0(2) . . . . ? C7 N2 C3 C19 36.0(3) . . . . ? Ti1 N2 C3 C19 -139.18(17) . . . . ? N2 C3 C4 C5 12.0(4) . . . . ? C19 C3 C4 C5 -173.3(2) . . . . ? C3 C4 C5 N6 -31.0(4) . . . . ? C3 C4 C5 C23 146.5(2) . . . . ? C4 C5 N6 C27 -169.83(18) . . . . ? C23 C5 N6 C27 13.1(3) . . . . ? C4 C5 N6 Ti1 -4.8(2) . . . . ? C23 C5 N6 Ti1 178.05(15) . . . . ? N39 Ti1 N6 C5 153.23(13) . . . . ? N2 Ti1 N6 C5 37.97(14) . . . . ? Cl52 Ti1 N6 C5 -79.23(14) . . . . ? N39 Ti1 N6 C27 -41.33(16) . . . . ? N2 Ti1 N6 C27 -156.59(15) . . . . ? Cl52 Ti1 N6 C27 86.22(15) . . . . ? C3 N2 C7 C8 -108.8(2) . . . . ? Ti1 N2 C7 C8 65.4(2) . . . . ? C3 N2 C7 C12 74.8(3) . . . . ? Ti1 N2 C7 C12 -111.06(19) . . . . ? C12 C7 C8 C9 -1.8(3) . . . . ? N2 C7 C8 C9 -178.14(18) . . . . ? C12 C7 C8 C16 -179.48(19) . . . . ? N2 C7 C8 C16 4.1(3) . . . . ? C7 C8 C9 C10 -0.6(3) . . . . ? C16 C8 C9 C10 177.2(2) . . . . ? C8 C9 C10 C11 1.9(3) . . . . ? C9 C10 C11 C12 -0.8(4) . . . . ? C10 C11 C12 C7 -1.5(3) . . . . ? C10 C11 C12 C13 176.7(2) . . . . ? C8 C7 C12 C11 2.8(3) . . . . ? N2 C7 C12 C11 179.22(19) . . . . ? C8 C7 C12 C13 -175.4(2) . . . . ? N2 C7 C12 C13 1.1(3) . . . . ? C11 C12 C13 C14 65.1(3) . . . . ? C7 C12 C13 C14 -116.8(3) . . . . ? C11 C12 C13 C15 -59.1(3) . . . . ? C7 C12 C13 C15 119.0(3) . . . . ? C9 C8 C16 C18 -45.3(3) . . . . ? C7 C8 C16 C18 132.4(2) . . . . ? C9 C8 C16 C17 78.3(3) . . . . ? C7 C8 C16 C17 -104.1(2) . . . . ? N2 C3 C19 C20 -22.2(3) . . . . ? C4 C3 C19 C20 163.3(2) . . . . ? N2 C3 C19 C22 -144.1(2) . . . . ? C4 C3 C19 C22 41.5(3) . . . . ? N2 C3 C19 C21 97.4(2) . . . . ? C4 C3 C19 C21 -77.0(2) . . . . ? N6 C5 C23 C26 0.6(3) . . . . ? C4 C5 C23 C26 -176.7(2) . . . . ? N6 C5 C23 C25 -123.2(2) . . . . ? C4 C5 C23 C25 59.5(2) . . . . ? N6 C5 C23 C24 119.1(2) . . . . ? C4 C5 C23 C24 -58.2(2) . . . . ? C5 N6 C27 C28 -108.8(2) . . . . ? Ti1 N6 C27 C28 87.6(2) . . . . ? C5 N6 C27 C32 75.0(3) . . . . ? Ti1 N6 C27 C32 -88.6(2) . . . . ? C32 C27 C28 C29 -3.9(3) . . . . ? N6 C27 C28 C29 180.0(2) . . . . ? C32 C27 C28 C36 178.3(2) . . . . ? N6 C27 C28 C36 2.2(3) . . . . ? C27 C28 C29 C30 1.9(4) . . . . ? C36 C28 C29 C30 179.7(2) . . . . ? C28 C29 C30 C31 1.0(4) . . . . ? C29 C30 C31 C32 -2.0(4) . . . . ? C30 C31 C32 C27 0.0(3) . . . . ? C30 C31 C32 C33 179.6(2) . . . . ? C28 C27 C32 C31 3.0(3) . . . . ? N6 C27 C32 C31 179.18(19) . . . . ? C28 C27 C32 C33 -176.64(19) . . . . ? N6 C27 C32 C33 -0.5(3) . . . . ? C31 C32 C33 C34 -68.6(3) . . . . ? C27 C32 C33 C34 111.1(2) . . . . ? C31 C32 C33 C35 53.1(3) . . . . ? C27 C32 C33 C35 -127.2(2) . . . . ? C29 C28 C36 C38 49.1(3) . . . . ? C27 C28 C36 C38 -133.1(2) . . . . ? C29 C28 C36 C37 -73.1(3) . . . . ? C27 C28 C36 C37 104.7(3) . . . . ? N2 Ti1 N39 C40 -159.8(7) . . . . ? N6 Ti1 N39 C40 93.7(7) . . . . ? Cl52 Ti1 N39 C40 -33.6(7) . . . . ? Ti1 N39 C40 C45 163.2(6) . . . . ? Ti1 N39 C40 C41 -17.7(8) . . . . ? N39 C40 C41 C42 -178.2(2) . . . . ? C45 C40 C41 C42 0.9(3) . . . . ? N39 C40 C41 C49 4.5(3) . . . . ? C45 C40 C41 C49 -176.4(2) . . . . ? C40 C41 C42 C43 0.5(4) . . . . ? C49 C41 C42 C43 177.9(2) . . . . ? C41 C42 C43 C44 -1.2(4) . . . . ? C42 C43 C44 C45 0.5(4) . . . . ? C43 C44 C45 C40 0.9(3) . . . . ? C43 C44 C45 C46 -178.5(2) . . . . ? N39 C40 C45 C44 177.47(19) . . . . ? C41 C40 C45 C44 -1.6(3) . . . . ? N39 C40 C45 C46 -3.1(3) . . . . ? C41 C40 C45 C46 177.8(2) . . . . ? C44 C45 C46 C48 62.7(3) . . . . ? C40 C45 C46 C48 -116.7(2) . . . . ? C44 C45 C46 C47 -58.4(3) . . . . ? C40 C45 C46 C47 122.2(2) . . . . ? C42 C41 C49 C50 42.0(3) . . . . ? C40 C41 C49 C50 -140.6(3) . . . . ? C42 C41 C49 C51 -83.1(3) . . . . ? C40 C41 C49 C51 94.2(3) . . . . ? C57 Cl56 C57 Cl1 38(3) 3_557 . . . ? Cl56 Cl56 C57 Cl1 38(3) 3_557 . . . ? Cl1 Cl56 C57 C57 -38(3) . . . 3_557 ? Cl56 Cl56 C57 C57 0.000(3) 3_557 . . 3_557 ? Cl1 Cl56 C57 Cl56 -38(3) . . . 3_557 ? C57 Cl56 C57 Cl56 0.0 3_557 . . 3_557 ? Cl1 Cl56 C57 Cl1 -47(3) . . . 3_557 ? C57 Cl56 C57 Cl1 -8.7(7) 3_557 . . 3_557 ? Cl56 Cl56 C57 Cl1 -8.7(7) 3_557 . . 3_557 ? C57 Cl56 Cl1 C57 -36(3) 3_557 . . . ? Cl56 Cl56 Cl1 C57 -27(2) 3_557 . . . ? C57 Cl56 Cl1 C57 36(3) . . . 3_557 ? Cl56 Cl56 Cl1 C57 8.7(7) 3_557 . . 3_557 ? C57 C57 Cl1 Cl56 139(3) 3_557 . . . ? Cl56 C57 Cl1 Cl56 144(3) 3_557 . . . ? Cl1 C57 Cl1 Cl56 139(3) 3_557 . . . ? Cl56 C57 Cl1 C57 -139(3) . . . 3_557 ? Cl56 C57 Cl1 C57 4.9(3) 3_557 . . 3_557 ? Cl1 C57 Cl1 C57 0.000(1) 3_557 . . 3_557 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.411 _refine_diff_density_min -0.412 _refine_diff_density_rms 0.057 data_04279 _database_code_depnum_ccdc_archive 'CCDC 260839' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _exptl_crystal_id MSC04279 _audit_creation_date 10/18//2004 _chemical_formula_structural ; 0.55[Ti(C35H53N2)(C12H17N)(Et2O)]+ 0.45[Ti(C35H53N2)(C12H17N)(thf)]+[B(C6F5)4]-;C6H5F ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C81 H84.11 B F21 N3 O Ti' _chemical_formula_weight 1573.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' _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 13.5063(9) _cell_length_b 15.1201(10) _cell_length_c 18.9733(12) _cell_angle_alpha 98.775(2) _cell_angle_beta 104.464(2) _cell_angle_gamma 93.096(2) _cell_volume 3690.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 131(2) _cell_measurement_reflns_used 1924 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 24.75 _exptl_crystal_description 'cleaved fragment' _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1630 _exptl_absorpt_coefficient_mu 0.218 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; _diffrn_ambient_temperature 131(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details ' 0.30 degree frames measured for 2.17 seconds each' _diffrn_measurement_method '\w scans' _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 84065 _diffrn_reflns_av_R_equivalents 0.0587 _diffrn_reflns_av_sigmaI/netI 0.0581 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.55 _reflns_number_total 17007 _reflns_number_gt 11430 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999), XTEL (local program)' _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^)+(0.0441P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17007 _refine_ls_number_parameters 1391 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0604 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.0918 _refine_ls_wR_factor_gt 0.0853 _refine_ls_goodness_of_fit_ref 0.891 _refine_ls_restrained_S_all 0.891 _refine_ls_shift/su_max 0.016 _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 0.89002(2) 0.805491(18) 0.673309(15) 0.01722(7) Uani 1 1 d . . . N2 N 0.94318(10) 0.81483(8) 0.78046(7) 0.0189(3) Uani 1 1 d . A . C3 C 0.85983(12) 0.81486(10) 0.80962(8) 0.0186(3) Uani 1 1 d . A . C4 C 0.76837(12) 0.76463(11) 0.76942(9) 0.0199(3) Uani 1 1 d . . . C5 C 0.74139(11) 0.69229(10) 0.70646(8) 0.0192(3) Uani 1 1 d . A . N6 N 0.79040(9) 0.69068(8) 0.65409(7) 0.0180(3) Uani 1 1 d . A . C7 C 1.04722(12) 0.83349(10) 0.82657(8) 0.0192(3) Uani 1 1 d . . . C8 C 1.09198(13) 0.76439(11) 0.86197(9) 0.0231(4) Uani 1 1 d . A . C9 C 1.18902(14) 0.78511(12) 0.91064(9) 0.0278(4) Uani 1 1 d . . . C10 C 1.24112(14) 0.86942(13) 0.92276(10) 0.0300(4) Uani 1 1 d . A . C11 C 1.19916(13) 0.93387(12) 0.88327(10) 0.0268(4) Uani 1 1 d . . . C12 C 1.10191(12) 0.91767(11) 0.83369(9) 0.0213(3) Uani 1 1 d . A . C13 C 1.06166(14) 0.99097(11) 0.79083(9) 0.0244(4) Uani 1 1 d . . . C14 C 1.07035(16) 1.08285(12) 0.84028(11) 0.0309(4) Uani 1 1 d . A . C15 C 1.11831(17) 1.00037(13) 0.73123(11) 0.0317(4) Uani 1 1 d . A . C16 C 1.03831(15) 0.66959(11) 0.84821(10) 0.0288(4) Uani 1 1 d . . . C17 C 1.1137(2) 0.59762(14) 0.85260(15) 0.0482(6) Uani 1 1 d . A . C18 C 0.97282(16) 0.65619(14) 0.90088(12) 0.0345(4) Uani 1 1 d . A . C19 C 0.85661(13) 0.87574(11) 0.88380(9) 0.0246(4) Uani 1 1 d . . . C20 C 0.77039(16) 0.84092(15) 0.91543(11) 0.0360(5) Uani 1 1 d . A . C21 C 0.95502(15) 0.88698(14) 0.94709(10) 0.0307(4) Uani 1 1 d . A . C22 C 0.83389(16) 0.96916(13) 0.86539(12) 0.0330(4) Uani 1 1 d . A . C23 C 0.65528(12) 0.62270(11) 0.71201(9) 0.0243(4) Uani 1 1 d . . . C24 C 0.69431(16) 0.59080(13) 0.78666(10) 0.0311(4) Uani 1 1 d . A . C25 C 0.62706(15) 0.53711(12) 0.65300(10) 0.0280(4) Uani 1 1 d . A . C26 C 0.55565(14) 0.66816(14) 0.71214(12) 0.0314(4) Uani 1 1 d . A . C27 C 0.76373(12) 0.62582(10) 0.58569(8) 0.0193(3) Uani 1 1 d . . . C28 C 0.82779(12) 0.55738(10) 0.57661(9) 0.0213(3) Uani 1 1 d . A . C29 C 0.79865(13) 0.49454(11) 0.51150(9) 0.0249(4) Uani 1 1 d . . . C30 C 0.71253(13) 0.50144(11) 0.45603(10) 0.0264(4) Uani 1 1 d . A . C31 C 0.65342(13) 0.57213(11) 0.46451(9) 0.0248(4) Uani 1 1 d . . . C32 C 0.67682(12) 0.63580(11) 0.52930(9) 0.0211(3) Uani 1 1 d . A . C33 C 0.60742(12) 0.71114(11) 0.53502(9) 0.0234(4) Uani 1 1 d . . . C34 C 0.63182(16) 0.78371(14) 0.49253(12) 0.0333(4) Uani 1 1 d . A . C35 C 0.49252(14) 0.67799(14) 0.50681(12) 0.0317(4) Uani 1 1 d . A . C36 C 0.92447(13) 0.54754(11) 0.63534(9) 0.0250(4) Uani 1 1 d . . . C37 C 0.90694(18) 0.47335(16) 0.67840(13) 0.0391(5) Uani 1 1 d . A . C38 C 1.01413(14) 0.52920(14) 0.60166(11) 0.0306(4) Uani 1 1 d . A . N39 N 0.98650(10) 0.78820(8) 0.63011(7) 0.0188(3) Uani 1 1 d . A . C40 C 1.05771(12) 0.77565(10) 0.58748(9) 0.0190(3) Uani 1 1 d . . . C41 C 1.16271(12) 0.76765(10) 0.62011(9) 0.0221(3) Uani 1 1 d . A . C42 C 1.22839(14) 0.75232(11) 0.57434(10) 0.0268(4) Uani 1 1 d . . . C43 C 1.19455(14) 0.74495(12) 0.49841(10) 0.0283(4) Uani 1 1 d . A . C44 C 1.09272(14) 0.75478(11) 0.46708(10) 0.0258(4) Uani 1 1 d . . . C45 C 1.02338(12) 0.77088(10) 0.50970(9) 0.0209(3) Uani 1 1 d . A . C46 C 0.91331(13) 0.78174(11) 0.47077(9) 0.0235(4) Uani 1 1 d . . . C47 C 0.90753(17) 0.85493(14) 0.42261(12) 0.0357(5) Uani 1 1 d . A . C48 C 0.85843(15) 0.69333(13) 0.42459(11) 0.0301(4) Uani 1 1 d . A . C49 C 1.20770(13) 0.77493(12) 0.70277(9) 0.0253(4) Uani 1 1 d . . . C50 C 1.30342(15) 0.84274(14) 0.73181(11) 0.0328(4) Uani 1 1 d . A . C51 C 1.2371(2) 0.68471(14) 0.72324(12) 0.0419(5) Uani 1 1 d . A . O52 O 0.8387(9) 0.9266(7) 0.6408(8) 0.0183(12) Uani 0.553(5) 1 d P A 1 C53 C 0.8932(5) 0.9837(4) 0.6037(4) 0.0217(12) Uani 0.553(5) 1 d P A 1 C54 C 0.8239(3) 1.0065(2) 0.5352(2) 0.0296(10) Uani 0.553(5) 1 d P A 1 C55 C 0.7325(13) 0.9455(10) 0.6614(12) 0.031(3) Uani 0.553(5) 1 d P A 1 C56 C 0.7687(4) 1.0554(3) 0.6987(3) 0.0354(12) Uani 0.553(5) 1 d P A 1 B57 B 0.49158(14) 0.79332(12) 0.18009(10) 0.0219(4) Uani 1 1 d . . . C58 C 0.37569(12) 0.76273(11) 0.18833(9) 0.0240(4) Uani 1 1 d . . . C59 C 0.28238(13) 0.76783(12) 0.13883(9) 0.0273(4) Uani 1 1 d . . . C60 C 0.18765(13) 0.74995(13) 0.15189(10) 0.0327(4) Uani 1 1 d . . . C61 C 0.18228(14) 0.72567(13) 0.21775(11) 0.0362(5) Uani 1 1 d . . . C62 C 0.27224(14) 0.72049(13) 0.26955(10) 0.0343(4) Uani 1 1 d . . . C63 C 0.36475(13) 0.73893(12) 0.25431(9) 0.0280(4) Uani 1 1 d . . . F64 F 0.27873(7) 0.79316(7) 0.07309(5) 0.0343(2) Uani 1 1 d . . . F65 F 0.10035(8) 0.75704(8) 0.10070(6) 0.0442(3) Uani 1 1 d . . . F66 F 0.09081(8) 0.70989(9) 0.23195(7) 0.0522(3) Uani 1 1 d . . . F67 F 0.26917(9) 0.69952(9) 0.33566(6) 0.0484(3) Uani 1 1 d . . . F68 F 0.44958(7) 0.73459(7) 0.30923(5) 0.0344(2) Uani 1 1 d . . . C69 C 0.49485(12) 0.80359(11) 0.09523(9) 0.0218(3) Uani 1 1 d . . . C70 C 0.54091(12) 0.87527(11) 0.07318(9) 0.0223(3) Uani 1 1 d . . . C71 C 0.54488(12) 0.87732(11) 0.00157(10) 0.0255(4) Uani 1 1 d . . . C72 C 0.50259(13) 0.80509(13) -0.05317(9) 0.0277(4) Uani 1 1 d . . . C73 C 0.45734(13) 0.73113(12) -0.03471(9) 0.0275(4) Uani 1 1 d . . . C74 C 0.45579(12) 0.73206(11) 0.03754(9) 0.0251(4) Uani 1 1 d . . . F75 F 0.58620(7) 0.94941(6) 0.12296(5) 0.0269(2) Uani 1 1 d . . . F76 F 0.58955(7) 0.95019(7) -0.01552(5) 0.0330(2) Uani 1 1 d . . . F77 F 0.50499(8) 0.80632(8) -0.12335(5) 0.0390(3) Uani 1 1 d . . . F78 F 0.41607(8) 0.65934(7) -0.08733(5) 0.0380(3) Uani 1 1 d . . . F79 F 0.41120(8) 0.65664(6) 0.05198(5) 0.0336(2) Uani 1 1 d . . . C80 C 0.57518(12) 0.72004(11) 0.20172(9) 0.0224(3) Uani 1 1 d . . . C81 C 0.67935(13) 0.74484(11) 0.21180(9) 0.0231(4) Uani 1 1 d . . . C82 C 0.75618(13) 0.68986(12) 0.22931(9) 0.0262(4) Uani 1 1 d . . . C83 C 0.73148(14) 0.60304(12) 0.23639(9) 0.0302(4) Uani 1 1 d . . . C84 C 0.63014(15) 0.57330(11) 0.22507(10) 0.0315(4) Uani 1 1 d . . . C85 C 0.55541(13) 0.63078(11) 0.20765(9) 0.0268(4) Uani 1 1 d . . . F86 F 0.70891(7) 0.82960(6) 0.20515(5) 0.0289(2) Uani 1 1 d . . . F87 F 0.85560(7) 0.72054(7) 0.24043(5) 0.0344(2) Uani 1 1 d . . . F88 F 0.80531(9) 0.54835(7) 0.25475(6) 0.0433(3) Uani 1 1 d . . . F89 F 0.60411(9) 0.48828(7) 0.23164(7) 0.0469(3) Uani 1 1 d . . . F90 F 0.45758(8) 0.59469(6) 0.19677(6) 0.0355(3) Uani 1 1 d . . . C91 C 0.51811(12) 0.88977(11) 0.23884(9) 0.0242(4) Uani 1 1 d . . . C92 C 0.57870(14) 0.90429(12) 0.31084(10) 0.0292(4) Uani 1 1 d . . . C93 C 0.58357(16) 0.98187(13) 0.36138(10) 0.0392(5) Uani 1 1 d . . . C94 C 0.52794(17) 1.05077(13) 0.34038(12) 0.0419(5) Uani 1 1 d . . . C95 C 0.46880(14) 1.04150(12) 0.26907(12) 0.0368(5) Uani 1 1 d . . . C96 C 0.46333(13) 0.96248(12) 0.22108(10) 0.0287(4) Uani 1 1 d . . . F97 F 0.63755(8) 0.84074(7) 0.33710(5) 0.0348(2) Uani 1 1 d . . . F98 F 0.64212(11) 0.98962(8) 0.43117(6) 0.0609(4) Uani 1 1 d . . . F99 F 0.53126(10) 1.12680(8) 0.38875(7) 0.0604(4) Uani 1 1 d . . . F100 F 0.41543(9) 1.11013(7) 0.24734(7) 0.0518(3) Uani 1 1 d . . . F101 F 0.39882(8) 0.95671(7) 0.15336(6) 0.0354(2) Uani 1 1 d . . . F102 F 0.87032(11) 0.45488(9) 0.96108(8) 0.0662(4) Uani 1 1 d . . . C103 C 0.82276(15) 0.52481(12) 0.98733(11) 0.0356(4) Uani 1 1 d . . . C104 C 0.88129(15) 0.59323(14) 1.03960(11) 0.0377(5) Uani 1 1 d . . . C105 C 0.83119(18) 0.66478(15) 1.06326(11) 0.0430(5) Uani 1 1 d . . . C106 C 0.7270(2) 0.66582(17) 1.03599(13) 0.0502(6) Uani 1 1 d . . . C107 C 0.67137(18) 0.59539(17) 0.98458(13) 0.0501(6) Uani 1 1 d . . . C108 C 0.71937(17) 0.52323(15) 0.95897(12) 0.0416(5) Uani 1 1 d . . . H109 H 0.7150(12) 0.7699(10) 0.7904(9) 0.017(4) Uiso 1 1 d . . . H110 H 1.2212(13) 0.7408(11) 0.9378(9) 0.024(5) Uiso 1 1 d . . . H111 H 1.3065(14) 0.8834(12) 0.9568(10) 0.033(5) Uiso 1 1 d . . . H112 H 1.2351(12) 0.9897(11) 0.8898(9) 0.019(4) Uiso 1 1 d . . . H113 H 0.9882(13) 0.9750(10) 0.7668(9) 0.018(4) Uiso 1 1 d . . . H114 H 1.0407(12) 1.0815(11) 0.8831(9) 0.022(4) Uiso 1 1 d . . . H115 H 1.0339(15) 1.1262(13) 0.8104(10) 0.040(5) Uiso 1 1 d . . . H116 H 1.1425(15) 1.1065(13) 0.8615(10) 0.039(5) Uiso 1 1 d . . . H117 H 1.1937(16) 1.0146(13) 0.7550(10) 0.041(6) Uiso 1 1 d . . . H118 H 1.0919(14) 1.0496(13) 0.7069(10) 0.036(5) Uiso 1 1 d . . . H119 H 1.1082(12) 0.9461(12) 0.6938(9) 0.023(4) Uiso 1 1 d . . . H120 H 0.9926(13) 0.6599(12) 0.7982(10) 0.030(5) Uiso 1 1 d . . . H21 H 1.158(2) 0.6022(17) 0.8192(14) 0.079(8) Uiso 1 1 d . . . H122 H 1.0741(15) 0.5362(14) 0.8380(11) 0.045(6) Uiso 1 1 d . . . H123 H 1.1583(18) 0.6010(16) 0.9042(14) 0.070(8) Uiso 1 1 d . . . H124 H 1.0177(14) 0.6711(12) 0.9518(11) 0.034(5) Uiso 1 1 d . . . H125 H 0.9454(14) 0.5929(14) 0.8915(10) 0.041(5) Uiso 1 1 d . . . H126 H 0.9146(14) 0.6936(12) 0.8955(9) 0.029(5) Uiso 1 1 d . . . H127 H 0.7765(14) 0.8775(13) 0.9622(11) 0.038(5) Uiso 1 1 d . . . H128 H 0.7788(14) 0.7775(14) 0.9244(10) 0.037(5) Uiso 1 1 d . . . H129 H 0.7024(15) 0.8470(12) 0.8852(10) 0.035(5) Uiso 1 1 d . . . H130 H 1.0119(14) 0.9182(12) 0.9361(10) 0.035(5) Uiso 1 1 d . . . H131 H 0.9414(14) 0.9238(12) 0.9896(11) 0.036(5) Uiso 1 1 d . . . H132 H 0.9735(14) 0.8295(14) 0.9611(10) 0.039(6) Uiso 1 1 d . . . H133 H 0.8300(14) 1.0099(13) 0.9071(11) 0.040(5) Uiso 1 1 d . . . H134 H 0.8848(15) 0.9955(12) 0.8443(10) 0.036(5) Uiso 1 1 d . . . H135 H 0.7661(15) 0.9660(12) 0.8286(10) 0.033(5) Uiso 1 1 d . . . H136 H 0.7577(16) 0.5609(13) 0.7893(11) 0.044(6) Uiso 1 1 d . . . H137 H 0.7078(14) 0.6403(13) 0.8298(10) 0.036(5) Uiso 1 1 d . . . H138 H 0.6440(14) 0.5438(13) 0.7922(10) 0.035(5) Uiso 1 1 d . . . H139 H 0.5805(14) 0.4994(13) 0.6704(10) 0.038(5) Uiso 1 1 d . . . H140 H 0.6855(14) 0.5057(12) 0.6468(9) 0.028(5) Uiso 1 1 d . . . H142 H 0.5046(14) 0.6209(13) 0.7132(10) 0.037(5) Uiso 1 1 d . . . H143 H 0.5303(14) 0.6952(13) 0.6673(11) 0.035(5) Uiso 1 1 d . . . H144 H 0.5657(14) 0.7166(13) 0.7570(10) 0.035(5) Uiso 1 1 d . . . H145 H 0.8385(12) 0.4475(11) 0.5056(9) 0.020(4) Uiso 1 1 d . . . H146 H 0.6961(13) 0.4590(12) 0.4112(10) 0.028(5) Uiso 1 1 d . . . H147 H 0.5934(14) 0.5791(11) 0.4264(10) 0.028(5) Uiso 1 1 d . . . H148 H 0.6198(11) 0.7398(10) 0.5856(9) 0.013(4) Uiso 1 1 d . . . H149 H 0.7085(15) 0.8084(12) 0.5126(10) 0.035(5) Uiso 1 1 d . . . H150 H 0.5876(16) 0.8349(14) 0.4970(11) 0.048(6) Uiso 1 1 d . . . H151 H 0.6203(15) 0.7619(13) 0.4427(12) 0.042(6) Uiso 1 1 d . . . H152 H 0.4522(16) 0.7308(15) 0.5193(11) 0.054(6) Uiso 1 1 d . . . H153 H 0.4740(15) 0.6285(14) 0.5299(11) 0.041(6) Uiso 1 1 d . . . H154 H 0.4689(15) 0.6592(13) 0.4526(12) 0.043(6) Uiso 1 1 d . . . H155 H 0.9438(13) 0.6021(12) 0.6698(9) 0.028(5) Uiso 1 1 d . . . H156 H 0.8603(18) 0.4876(15) 0.7037(12) 0.058(7) Uiso 1 1 d . . . H157 H 0.8803(16) 0.4168(16) 0.6450(12) 0.055(7) Uiso 1 1 d . . . H158 H 0.9693(17) 0.4638(14) 0.7145(12) 0.049(6) Uiso 1 1 d . . . H159 H 1.0266(14) 0.5774(13) 0.5764(10) 0.038(5) Uiso 1 1 d . . . H160 H 1.0003(16) 0.4716(15) 0.5675(12) 0.052(6) Uiso 1 1 d . . . H161 H 1.0764(15) 0.5224(12) 0.6392(11) 0.038(5) Uiso 1 1 d . . . H162 H 1.3020(14) 0.7455(12) 0.5973(10) 0.032(5) Uiso 1 1 d . . . H163 H 1.2399(14) 0.7340(12) 0.4678(10) 0.037(5) Uiso 1 1 d . . . H164 H 1.0687(13) 0.7507(11) 0.4172(10) 0.023(4) Uiso 1 1 d . . . H165 H 0.8811(12) 0.8012(11) 0.5099(9) 0.021(4) Uiso 1 1 d . . . H166 H 0.8360(17) 0.8633(13) 0.4017(11) 0.047(6) Uiso 1 1 d . . . H167 H 0.9414(15) 0.8375(13) 0.3826(11) 0.043(6) Uiso 1 1 d . . . H168 H 0.9434(16) 0.9114(15) 0.4517(11) 0.047(6) Uiso 1 1 d . . . H169 H 0.8907(13) 0.6726(12) 0.3875(10) 0.028(5) Uiso 1 1 d . . . H170 H 0.7872(15) 0.7026(12) 0.3982(10) 0.033(5) Uiso 1 1 d . . . H171 H 0.8584(13) 0.6453(12) 0.4556(10) 0.031(5) Uiso 1 1 d . . . H172 H 1.1585(14) 0.7962(12) 0.7281(10) 0.029(5) Uiso 1 1 d . . . H173 H 1.3243(13) 0.8546(12) 0.7864(10) 0.031(5) Uiso 1 1 d . . . H174 H 1.2901(15) 0.9012(14) 0.7132(11) 0.047(6) Uiso 1 1 d . . . H175 H 1.3661(16) 0.8172(13) 0.7163(11) 0.047(6) Uiso 1 1 d . . . H176 H 1.2819(16) 0.6587(14) 0.6940(12) 0.049(6) Uiso 1 1 d . . . H177 H 1.1779(19) 0.6407(17) 0.7112(13) 0.069(8) Uiso 1 1 d . . . H178 H 1.2675(15) 0.6891(13) 0.7755(11) 0.040(5) Uiso 1 1 d . . . H179 H 0.924(3) 1.034(2) 0.6423(19) 0.028(9) Uiso 0.553(5) 1 d P A 1 H180 H 0.951(3) 0.947(3) 0.590(2) 0.041(15) Uiso 0.553(5) 1 d P A 1 H181 H 0.863(3) 1.042(2) 0.5118(19) 0.039(10) Uiso 0.553(5) 1 d P A 1 H182 H 0.789(3) 0.950(3) 0.498(2) 0.050(12) Uiso 0.553(5) 1 d P A 1 H183 H 0.773(3) 1.048(3) 0.549(2) 0.035(10) Uiso 0.553(5) 1 d P A 1 H184 H 0.692(3) 0.948(2) 0.6134(19) 0.022(9) Uiso 0.553(5) 1 d P A 1 H185 H 0.726(3) 0.911(2) 0.695(2) 0.014(9) Uiso 0.553(5) 1 d P A 1 H186 H 0.781(3) 1.089(3) 0.671(3) 0.042(12) Uiso 0.553(5) 1 d P A 1 H187 H 0.824(3) 1.063(3) 0.738(2) 0.061(15) Uiso 0.553(5) 1 d P A 1 H188 H 0.720(3) 1.071(2) 0.711(2) 0.035(11) Uiso 0.553(5) 1 d P A 1 H189 H 0.5902(13) 0.5481(11) 0.6021(10) 0.028(5) Uiso 1 1 d . . . H190 H 0.9746(10) 0.5890(9) 1.0697(7) 0.004(3) Uiso 1 1 d . . . H191 H 0.8705(15) 0.7106(14) 1.0992(11) 0.040(6) Uiso 1 1 d . . . H192 H 0.6930(17) 0.7171(16) 1.0530(12) 0.060(7) Uiso 1 1 d . . . H193 H 0.5993(18) 0.5925(15) 0.9666(12) 0.061(7) Uiso 1 1 d . . . H194 H 0.6836(16) 0.4710(15) 0.9231(12) 0.055(6) Uiso 1 1 d . . . H1A H 0.816(3) 0.952(3) 0.543(3) 0.007(9) Uiso 0.447(5) 1 d P A 2 H2A H 0.931(4) 0.974(4) 0.608(3) 0.004(18) Uiso 0.447(5) 1 d P A 2 H3A H 0.815(4) 1.098(4) 0.592(3) 0.053(16) Uiso 0.447(5) 1 d P A 2 H4A H 0.866(4) 1.097(4) 0.668(3) 0.059(17) Uiso 0.447(5) 1 d P A 2 H5A H 0.682(4) 1.075(3) 0.662(3) 0.041(13) Uiso 0.447(5) 1 d P A 2 H6A H 0.638(6) 1.024(5) 0.572(4) 0.12(3) Uiso 0.447(5) 1 d P A 2 H7A H 0.746(4) 0.953(4) 0.702(3) 0.032(18) Uiso 0.447(5) 1 d P A 2 H8A H 0.675(5) 0.893(5) 0.635(4) 0.09(2) Uiso 0.447(5) 1 d P A 2 O52A O 0.8202(12) 0.9080(9) 0.6367(11) 0.0239(19) Uani 0.447(5) 1 d P A 2 C53A C 0.8521(6) 0.9750(7) 0.5939(5) 0.0270(17) Uani 0.447(5) 1 d P A 2 C54A C 0.8193(4) 1.0630(3) 0.6246(4) 0.0456(17) Uani 0.447(5) 1 d P A 2 C55A C 0.7145(6) 1.0321(4) 0.6341(5) 0.067(3) Uani 0.447(5) 1 d P A 2 C56A C 0.7485(17) 0.9622(14) 0.6565(15) 0.031(3) Uani 0.447(5) 1 d P 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 0.01668(14) 0.01735(14) 0.01738(14) 0.00238(11) 0.00454(11) 0.00060(11) N2 0.0185(7) 0.0185(7) 0.0197(7) 0.0013(5) 0.0066(6) -0.0016(5) C3 0.0214(8) 0.0165(8) 0.0183(8) 0.0032(6) 0.0062(7) 0.0008(6) C4 0.0183(8) 0.0220(8) 0.0206(8) 0.0019(6) 0.0086(7) 0.0000(6) C5 0.0166(8) 0.0196(8) 0.0207(8) 0.0041(6) 0.0034(7) 0.0018(6) N6 0.0165(6) 0.0187(7) 0.0177(7) 0.0027(5) 0.0032(5) 0.0005(5) C7 0.0172(8) 0.0233(8) 0.0163(8) -0.0006(6) 0.0055(6) -0.0001(6) C8 0.0277(9) 0.0253(9) 0.0175(8) 0.0019(7) 0.0092(7) 0.0026(7) C9 0.0292(10) 0.0327(10) 0.0221(9) 0.0061(8) 0.0059(8) 0.0079(8) C10 0.0197(9) 0.0399(11) 0.0269(9) 0.0006(8) 0.0026(8) 0.0022(8) C11 0.0218(9) 0.0287(9) 0.0281(9) 0.0012(8) 0.0073(7) -0.0062(7) C12 0.0213(8) 0.0240(8) 0.0194(8) 0.0021(7) 0.0085(7) -0.0003(7) C13 0.0266(9) 0.0200(8) 0.0259(9) 0.0019(7) 0.0078(8) -0.0035(7) C14 0.0373(11) 0.0231(9) 0.0311(10) -0.0004(8) 0.0110(9) -0.0021(8) C15 0.0449(12) 0.0223(9) 0.0297(10) 0.0040(8) 0.0151(9) -0.0032(9) C16 0.0400(11) 0.0232(9) 0.0208(9) 0.0055(7) 0.0034(8) -0.0008(8) C17 0.0672(16) 0.0264(11) 0.0641(17) 0.0098(11) 0.0394(15) 0.0090(11) C18 0.0354(11) 0.0279(10) 0.0418(12) 0.0104(9) 0.0112(10) 0.0002(9) C19 0.0263(9) 0.0255(9) 0.0213(8) -0.0041(7) 0.0110(7) -0.0035(7) C20 0.0336(11) 0.0462(13) 0.0263(10) -0.0085(9) 0.0158(9) -0.0103(9) C21 0.0311(10) 0.0368(11) 0.0220(9) -0.0058(8) 0.0107(8) -0.0043(9) C22 0.0357(11) 0.0274(10) 0.0354(11) -0.0054(8) 0.0146(10) 0.0050(8) C23 0.0239(9) 0.0246(9) 0.0238(9) 0.0023(7) 0.0084(7) -0.0060(7) C24 0.0354(11) 0.0306(10) 0.0257(10) 0.0056(8) 0.0073(8) -0.0102(9) C25 0.0279(10) 0.0273(9) 0.0275(10) 0.0015(8) 0.0091(8) -0.0082(8) C26 0.0222(9) 0.0343(11) 0.0372(11) 0.0006(9) 0.0119(9) -0.0058(8) C27 0.0205(8) 0.0194(8) 0.0176(8) 0.0011(6) 0.0068(7) -0.0034(6) C28 0.0222(8) 0.0197(8) 0.0218(8) 0.0027(6) 0.0065(7) -0.0019(6) C29 0.0262(9) 0.0201(8) 0.0277(9) -0.0005(7) 0.0088(8) 0.0014(7) C30 0.0279(9) 0.0242(9) 0.0232(9) -0.0055(7) 0.0069(8) -0.0044(7) C31 0.0211(9) 0.0292(9) 0.0214(9) 0.0011(7) 0.0035(7) -0.0037(7) C32 0.0191(8) 0.0220(8) 0.0219(8) 0.0036(7) 0.0060(7) -0.0027(6) C33 0.0210(8) 0.0265(9) 0.0198(9) 0.0004(7) 0.0023(7) 0.0008(7) C34 0.0313(11) 0.0334(11) 0.0362(12) 0.0095(9) 0.0077(9) 0.0068(9) C35 0.0194(9) 0.0374(11) 0.0337(11) 0.0003(9) 0.0021(8) 0.0009(8) C36 0.0262(9) 0.0202(8) 0.0251(9) -0.0021(7) 0.0035(7) 0.0031(7) C37 0.0381(12) 0.0460(13) 0.0365(12) 0.0172(10) 0.0085(11) 0.0093(10) C38 0.0242(10) 0.0313(10) 0.0338(11) 0.0044(9) 0.0030(9) 0.0054(8) N39 0.0198(7) 0.0176(7) 0.0182(7) 0.0030(5) 0.0041(6) -0.0004(5) C40 0.0221(8) 0.0146(7) 0.0220(8) 0.0015(6) 0.0100(7) -0.0004(6) C41 0.0236(8) 0.0196(8) 0.0239(8) 0.0031(7) 0.0086(7) 0.0006(7) C42 0.0230(9) 0.0285(9) 0.0291(9) 0.0022(7) 0.0093(8) 0.0017(7) C43 0.0299(10) 0.0305(10) 0.0289(10) 0.0027(8) 0.0175(8) 0.0034(8) C44 0.0324(10) 0.0259(9) 0.0202(9) 0.0031(7) 0.0096(8) 0.0026(7) C45 0.0250(9) 0.0160(8) 0.0228(8) 0.0037(6) 0.0083(7) 0.0002(6) C46 0.0265(9) 0.0264(9) 0.0187(8) 0.0039(7) 0.0081(7) 0.0025(7) C47 0.0342(11) 0.0375(11) 0.0364(11) 0.0148(9) 0.0059(10) 0.0030(9) C48 0.0289(10) 0.0329(10) 0.0267(10) 0.0024(8) 0.0067(9) -0.0027(8) C49 0.0220(9) 0.0317(10) 0.0224(9) 0.0015(7) 0.0079(7) 0.0025(7) C50 0.0260(10) 0.0386(11) 0.0300(11) -0.0014(9) 0.0060(8) -0.0019(8) C51 0.0573(15) 0.0352(11) 0.0285(11) 0.0077(9) 0.0016(11) 0.0043(11) O52 0.023(4) 0.009(3) 0.024(2) 0.005(3) 0.009(3) 0.002(2) C53 0.018(4) 0.022(3) 0.025(3) 0.0102(19) 0.002(3) -0.001(3) C54 0.032(2) 0.024(2) 0.031(2) 0.0080(15) 0.0034(16) 0.0021(15) C55 0.042(7) 0.027(5) 0.039(4) 0.015(4) 0.026(4) 0.021(5) C56 0.039(3) 0.026(2) 0.053(3) 0.0099(19) 0.028(3) 0.0126(17) B57 0.0205(9) 0.0227(9) 0.0229(10) 0.0068(8) 0.0053(8) 0.0001(7) C58 0.0227(9) 0.0249(9) 0.0239(9) 0.0038(7) 0.0063(7) -0.0028(7) C59 0.0267(9) 0.0318(10) 0.0242(9) 0.0067(7) 0.0075(8) -0.0001(7) C60 0.0208(9) 0.0405(11) 0.0341(10) 0.0051(8) 0.0040(8) -0.0012(8) C61 0.0241(9) 0.0450(12) 0.0419(11) 0.0061(9) 0.0164(9) -0.0073(8) C62 0.0344(10) 0.0424(11) 0.0298(10) 0.0103(8) 0.0147(9) -0.0050(9) C63 0.0231(9) 0.0324(10) 0.0270(9) 0.0071(8) 0.0041(8) -0.0033(7) F64 0.0250(5) 0.0523(7) 0.0270(5) 0.0148(5) 0.0048(4) 0.0034(5) F65 0.0202(5) 0.0655(8) 0.0443(7) 0.0113(6) 0.0030(5) 0.0005(5) F66 0.0287(6) 0.0764(9) 0.0574(8) 0.0178(7) 0.0208(6) -0.0066(6) F67 0.0438(7) 0.0725(9) 0.0357(6) 0.0203(6) 0.0192(5) -0.0074(6) F68 0.0303(6) 0.0458(6) 0.0268(5) 0.0140(5) 0.0041(5) -0.0036(5) C69 0.0170(8) 0.0250(8) 0.0249(9) 0.0076(7) 0.0057(7) 0.0046(7) C70 0.0172(8) 0.0239(8) 0.0265(9) 0.0052(7) 0.0062(7) 0.0033(7) C71 0.0191(8) 0.0307(9) 0.0321(10) 0.0139(8) 0.0109(7) 0.0055(7) C72 0.0202(8) 0.0439(11) 0.0220(9) 0.0104(8) 0.0070(7) 0.0083(8) C73 0.0225(9) 0.0319(10) 0.0247(9) -0.0009(7) 0.0033(7) 0.0039(7) C74 0.0214(8) 0.0269(9) 0.0286(9) 0.0085(7) 0.0076(7) 0.0022(7) F75 0.0264(5) 0.0243(5) 0.0310(5) 0.0050(4) 0.0105(4) -0.0022(4) F76 0.0315(6) 0.0370(6) 0.0376(6) 0.0177(5) 0.0158(5) 0.0012(5) F77 0.0350(6) 0.0617(7) 0.0232(5) 0.0114(5) 0.0105(5) 0.0054(5) F78 0.0374(6) 0.0423(6) 0.0286(6) -0.0040(5) 0.0052(5) -0.0020(5) F79 0.0402(6) 0.0264(5) 0.0327(6) 0.0039(4) 0.0094(5) -0.0073(5) C80 0.0232(8) 0.0224(8) 0.0204(8) 0.0042(7) 0.0034(7) 0.0008(7) C81 0.0262(9) 0.0205(8) 0.0216(8) 0.0029(7) 0.0052(7) -0.0004(7) C82 0.0226(9) 0.0326(10) 0.0219(9) 0.0023(7) 0.0037(7) 0.0051(7) C83 0.0353(10) 0.0279(9) 0.0248(9) 0.0022(7) 0.0023(8) 0.0137(8) C84 0.0423(11) 0.0192(9) 0.0314(10) 0.0053(7) 0.0066(9) 0.0018(8) C85 0.0260(9) 0.0255(9) 0.0264(9) 0.0041(7) 0.0039(7) -0.0035(7) F86 0.0242(5) 0.0250(5) 0.0375(6) 0.0083(4) 0.0076(4) -0.0031(4) F87 0.0221(5) 0.0449(6) 0.0347(6) 0.0049(5) 0.0052(5) 0.0057(5) F88 0.0466(7) 0.0365(6) 0.0451(7) 0.0069(5) 0.0050(6) 0.0224(5) F89 0.0576(8) 0.0205(5) 0.0604(8) 0.0130(5) 0.0078(6) 0.0029(5) F90 0.0304(6) 0.0263(5) 0.0469(6) 0.0109(5) 0.0043(5) -0.0074(4) C91 0.0230(8) 0.0237(9) 0.0297(9) 0.0058(7) 0.0143(7) -0.0018(7) C92 0.0357(10) 0.0258(9) 0.0285(9) 0.0054(7) 0.0133(8) -0.0016(8) C93 0.0522(13) 0.0364(11) 0.0288(10) -0.0035(8) 0.0191(10) -0.0103(9) C94 0.0548(13) 0.0249(10) 0.0522(13) -0.0088(9) 0.0370(11) -0.0078(9) C95 0.0339(10) 0.0258(10) 0.0596(14) 0.0038(9) 0.0305(10) 0.0043(8) C96 0.0247(9) 0.0281(9) 0.0379(11) 0.0066(8) 0.0165(8) 0.0005(7) F97 0.0417(6) 0.0341(6) 0.0244(5) 0.0046(4) 0.0021(5) -0.0017(5) F98 0.0967(11) 0.0492(8) 0.0283(6) -0.0083(5) 0.0144(7) -0.0149(7) F99 0.0805(9) 0.0336(7) 0.0725(9) -0.0186(6) 0.0496(8) -0.0080(6) F100 0.0474(7) 0.0279(6) 0.0913(10) 0.0074(6) 0.0386(7) 0.0132(5) F101 0.0281(6) 0.0341(6) 0.0484(7) 0.0120(5) 0.0134(5) 0.0105(5) F102 0.0761(10) 0.0483(8) 0.0754(10) 0.0044(7) 0.0229(8) 0.0198(7) C103 0.0438(12) 0.0288(10) 0.0392(11) 0.0087(8) 0.0176(10) 0.0073(9) C104 0.0364(11) 0.0428(12) 0.0350(11) 0.0107(9) 0.0105(9) -0.0024(9) C105 0.0602(15) 0.0388(12) 0.0305(11) 0.0032(9) 0.0163(11) -0.0035(11) C106 0.0642(16) 0.0524(14) 0.0431(13) 0.0132(11) 0.0241(12) 0.0231(13) C107 0.0374(13) 0.0644(16) 0.0533(15) 0.0233(12) 0.0111(11) 0.0121(12) C108 0.0451(13) 0.0409(12) 0.0373(12) 0.0141(10) 0.0059(10) -0.0065(10) O52A 0.029(4) 0.015(5) 0.030(3) 0.006(4) 0.011(3) -0.004(3) C53A 0.019(4) 0.026(3) 0.034(4) 0.003(3) 0.005(4) -0.002(3) C54A 0.053(3) 0.023(2) 0.074(4) 0.013(3) 0.037(3) 0.004(2) C55A 0.066(4) 0.038(3) 0.127(8) 0.032(4) 0.064(5) 0.021(3) C56A 0.034(5) 0.032(6) 0.035(5) 0.018(4) 0.017(4) 0.002(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 N39 1.7156(13) . ? Ti1 N2 1.9598(13) . ? Ti1 O52A 1.983(18) . ? Ti1 N6 2.0656(13) . ? Ti1 O52 2.117(12) . ? Ti1 C3 2.7012(15) . ? N2 C3 1.3728(19) . ? N2 C7 1.4448(19) . ? C3 C4 1.391(2) . ? C3 C19 1.572(2) . ? C4 C5 1.448(2) . ? C4 H109 0.909(16) . ? C5 N6 1.3225(19) . ? C5 C23 1.560(2) . ? N6 C27 1.4545(19) . ? C7 C12 1.407(2) . ? C7 C8 1.410(2) . ? C8 C9 1.390(2) . ? C8 C16 1.526(2) . ? C9 C10 1.381(3) . ? C9 H110 0.964(17) . ? C10 C11 1.379(3) . ? C10 H111 0.945(19) . ? C11 C12 1.396(2) . ? C11 H112 0.926(17) . ? C12 C13 1.518(2) . ? C13 C14 1.534(2) . ? C13 C15 1.534(2) . ? C13 H113 0.982(16) . ? C14 H114 0.993(17) . ? C14 H115 1.00(2) . ? C14 H116 0.98(2) . ? C15 H117 1.00(2) . ? C15 H118 0.974(19) . ? C15 H119 0.978(18) . ? C16 C18 1.518(3) . ? C16 C17 1.527(3) . ? C16 H120 0.979(18) . ? C17 H21 0.98(3) . ? C17 H122 1.01(2) . ? C17 H123 1.01(2) . ? C18 H124 0.989(19) . ? C18 H125 0.98(2) . ? C18 H126 0.987(18) . ? C19 C21 1.534(2) . ? C19 C22 1.535(3) . ? C19 C20 1.540(2) . ? C20 H127 0.95(2) . ? C20 H128 1.01(2) . ? C20 H129 0.971(19) . ? C21 H130 0.963(19) . ? C21 H131 0.970(19) . ? C21 H132 0.97(2) . ? C22 H133 0.94(2) . ? C22 H134 0.97(2) . ? C22 H135 0.997(19) . ? C23 C25 1.538(2) . ? C23 C24 1.543(2) . ? C23 C26 1.544(2) . ? C24 H136 0.98(2) . ? C24 H137 0.994(19) . ? C24 H138 0.992(19) . ? C25 H139 0.98(2) . ? C25 H140 0.966(18) . ? C25 H189 1.012(18) . ? C26 H142 0.972(19) . ? C26 H143 0.991(19) . ? C26 H144 1.010(19) . ? C27 C28 1.402(2) . ? C27 C32 1.409(2) . ? C28 C29 1.394(2) . ? C28 C36 1.521(2) . ? C29 C30 1.381(2) . ? C29 H145 0.924(17) . ? C30 C31 1.382(2) . ? C30 H146 0.952(17) . ? C31 C32 1.396(2) . ? C31 H147 0.964(18) . ? C32 C33 1.522(2) . ? C33 C34 1.525(3) . ? C33 C35 1.538(2) . ? C33 H148 0.960(15) . ? C34 H149 1.037(19) . ? C34 H150 1.01(2) . ? C34 H151 0.92(2) . ? C35 H152 1.02(2) . ? C35 H153 0.97(2) . ? C35 H154 0.99(2) . ? C36 C38 1.523(3) . ? C36 C37 1.526(3) . ? C36 H155 0.950(18) . ? C37 H156 0.90(2) . ? C37 H157 0.97(2) . ? C37 H158 0.98(2) . ? C38 H159 0.96(2) . ? C38 H160 0.98(2) . ? C38 H161 0.98(2) . ? N39 C40 1.4058(19) . ? C40 C41 1.418(2) . ? C40 C45 1.421(2) . ? C41 C42 1.393(2) . ? C41 C49 1.518(2) . ? C42 C43 1.383(2) . ? C42 H162 0.999(18) . ? C43 C44 1.381(2) . ? C43 H163 0.948(19) . ? C44 C45 1.390(2) . ? C44 H164 0.911(17) . ? C45 C46 1.516(2) . ? C46 C48 1.522(2) . ? C46 C47 1.532(2) . ? C46 H165 0.968(16) . ? C47 H166 0.97(2) . ? C47 H167 0.99(2) . ? C47 H168 0.97(2) . ? C48 H169 0.940(18) . ? C48 H170 0.995(19) . ? C48 H171 1.002(19) . ? C49 C51 1.521(3) . ? C49 C50 1.535(2) . ? C49 H172 0.954(18) . ? C50 H173 0.989(18) . ? C50 H174 1.01(2) . ? C50 H175 1.04(2) . ? C51 H176 0.98(2) . ? C51 H177 0.97(3) . ? C51 H178 0.96(2) . ? O52 C53 1.471(12) . ? O52 C55 1.607(18) . ? C53 C54 1.498(8) . ? C53 H179 0.97(4) . ? C53 H180 1.05(4) . ? C53 H1A 1.34(5) . ? C53 H2A 0.53(5) . ? C54 H181 0.96(4) . ? C54 H182 1.03(4) . ? C54 H183 1.02(4) . ? C54 H1A 0.87(4) . ? C55 C56 1.697(16) . ? C55 H184 0.95(4) . ? C55 H185 0.89(4) . ? C55 H7A 0.73(6) . ? C55 H8A 1.05(8) . ? C56 H186 0.83(5) . ? C56 H187 0.90(4) . ? C56 H188 0.79(4) . ? C56 H5A 1.28(5) . ? C56 H7A 1.58(6) . ? B57 C80 1.647(2) . ? B57 C69 1.652(2) . ? B57 C91 1.657(2) . ? B57 C58 1.660(2) . ? C58 C59 1.385(2) . ? C58 C63 1.394(2) . ? C59 F64 1.3499(19) . ? C59 C60 1.383(2) . ? C60 F65 1.348(2) . ? C60 C61 1.373(3) . ? C61 F66 1.3452(19) . ? C61 C62 1.373(3) . ? C62 F67 1.350(2) . ? C62 C63 1.375(2) . ? C63 F68 1.3547(19) . ? C69 C70 1.390(2) . ? C69 C74 1.391(2) . ? C70 F75 1.3554(18) . ? C70 C71 1.378(2) . ? C71 F76 1.3482(18) . ? C71 C72 1.374(2) . ? C72 F77 1.3430(19) . ? C72 C73 1.378(2) . ? C73 F78 1.3459(19) . ? C73 C74 1.374(2) . ? C74 F79 1.3571(18) . ? C80 C85 1.388(2) . ? C80 C81 1.394(2) . ? C81 F86 1.3553(18) . ? C81 C82 1.373(2) . ? C82 F87 1.3506(19) . ? C82 C83 1.372(2) . ? C83 F88 1.3426(19) . ? C83 C84 1.371(3) . ? C84 F89 1.3468(19) . ? C84 C85 1.378(2) . ? C85 F90 1.3556(19) . ? C91 C92 1.384(2) . ? C91 C96 1.395(2) . ? C92 F97 1.354(2) . ? C92 C93 1.385(2) . ? C93 F98 1.346(2) . ? C93 C94 1.368(3) . ? C94 F99 1.348(2) . ? C94 C95 1.371(3) . ? C95 F100 1.352(2) . ? C95 C96 1.374(2) . ? C96 F101 1.347(2) . ? F102 C103 1.361(2) . ? C103 C108 1.363(3) . ? C103 C104 1.373(3) . ? C104 C105 1.383(3) . ? C104 H190 1.257(13) . ? C105 C106 1.374(3) . ? C105 H191 0.93(2) . ? C106 C107 1.371(3) . ? C106 H192 0.98(2) . ? C107 C108 1.385(3) . ? C107 H193 0.94(2) . ? C108 H194 0.97(2) . ? O52A C56A 1.39(3) . ? O52A C53A 1.500(17) . ? C53A C54A 1.503(11) . ? C53A H179 1.34(4) . ? C53A H180 1.44(4) . ? C53A H1A 0.96(5) . ? C53A H2A 1.03(5) . ? C54A C55A 1.530(8) . ? C54A C56A 2.006(17) . ? C54A H179 1.48(3) . ? C54A H183 1.39(4) . ? C54A H186 1.16(5) . ? C54A H3A 0.87(6) . ? C54A H4A 0.96(6) . ? C55A C56A 1.27(2) . ? C55A H184 1.27(4) . ? C55A H186 1.21(4) . ? C55A H188 1.47(4) . ? C55A H5A 0.97(5) . ? C55A H6A 1.34(7) . ? C56A H184 0.96(5) . ? C56A H185 1.21(4) . ? C56A H7A 0.90(7) . ? C56A H8A 1.34(7) . ? 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 N39 Ti1 N2 110.61(6) . . ? N39 Ti1 O52A 106.9(5) . . ? N2 Ti1 O52A 117.3(6) . . ? N39 Ti1 N6 111.27(6) . . ? N2 Ti1 N6 98.24(5) . . ? O52A Ti1 N6 112.4(3) . . ? N39 Ti1 O52 102.0(4) . . ? N2 Ti1 O52 113.4(4) . . ? O52A Ti1 O52 9.1(5) . . ? N6 Ti1 O52 121.5(3) . . ? N39 Ti1 C3 139.21(5) . . ? N2 Ti1 C3 29.08(5) . . ? O52A Ti1 C3 103.0(6) . . ? N6 Ti1 C3 81.17(5) . . ? O52 Ti1 C3 103.5(4) . . ? C3 N2 C7 122.06(12) . . ? C3 N2 Ti1 106.98(10) . . ? C7 N2 Ti1 130.23(10) . . ? N2 C3 C4 119.57(14) . . ? N2 C3 C19 124.05(13) . . ? C4 C3 C19 116.14(14) . . ? N2 C3 Ti1 43.94(7) . . ? C4 C3 Ti1 81.63(9) . . ? C19 C3 Ti1 147.66(10) . . ? C3 C4 C5 134.03(15) . . ? C3 C4 H109 115.4(10) . . ? C5 C4 H109 109.5(10) . . ? N6 C5 C4 119.67(14) . . ? N6 C5 C23 128.27(14) . . ? C4 C5 C23 112.04(13) . . ? C5 N6 C27 124.20(13) . . ? C5 N6 Ti1 110.66(10) . . ? C27 N6 Ti1 124.19(10) . . ? C12 C7 C8 121.81(14) . . ? C12 C7 N2 120.21(14) . . ? C8 C7 N2 117.96(14) . . ? C9 C8 C7 117.49(15) . . ? C9 C8 C16 119.98(15) . . ? C7 C8 C16 122.52(15) . . ? C10 C9 C8 121.55(17) . . ? C10 C9 H110 118.1(10) . . ? C8 C9 H110 120.4(10) . . ? C11 C10 C9 119.89(17) . . ? C11 C10 H111 119.0(11) . . ? C9 C10 H111 121.0(11) . . ? C10 C11 C12 121.47(16) . . ? C10 C11 H112 120.1(10) . . ? C12 C11 H112 118.4(10) . . ? C11 C12 C7 117.39(15) . . ? C11 C12 C13 118.57(15) . . ? C7 C12 C13 124.04(14) . . ? C12 C13 C14 113.04(14) . . ? C12 C13 C15 110.88(15) . . ? C14 C13 C15 108.81(14) . . ? C12 C13 H113 108.7(9) . . ? C14 C13 H113 106.5(9) . . ? C15 C13 H113 108.8(9) . . ? C13 C14 H114 113.9(10) . . ? C13 C14 H115 109.5(11) . . ? H114 C14 H115 107.8(14) . . ? C13 C14 H116 110.9(11) . . ? H114 C14 H116 105.6(14) . . ? H115 C14 H116 109.0(16) . . ? C13 C15 H117 109.4(11) . . ? C13 C15 H118 107.7(11) . . ? H117 C15 H118 109.6(16) . . ? C13 C15 H119 113.0(10) . . ? H117 C15 H119 108.7(15) . . ? H118 C15 H119 108.4(14) . . ? C18 C16 C8 113.61(15) . . ? C18 C16 C17 107.70(16) . . ? C8 C16 C17 112.53(16) . . ? C18 C16 H120 107.6(10) . . ? C8 C16 H120 106.5(10) . . ? C17 C16 H120 108.7(10) . . ? C16 C17 H21 111.7(15) . . ? C16 C17 H122 109.3(11) . . ? H21 C17 H122 108.0(18) . . ? C16 C17 H123 111.9(14) . . ? H21 C17 H123 109(2) . . ? H122 C17 H123 106.9(18) . . ? C16 C18 H124 107.8(11) . . ? C16 C18 H125 109.1(11) . . ? H124 C18 H125 108.8(15) . . ? C16 C18 H126 112.8(10) . . ? H124 C18 H126 109.9(15) . . ? H125 C18 H126 108.4(15) . . ? C21 C19 C22 108.00(15) . . ? C21 C19 C20 105.64(15) . . ? C22 C19 C20 107.95(16) . . ? C21 C19 C3 116.19(14) . . ? C22 C19 C3 106.64(14) . . ? C20 C19 C3 112.12(13) . . ? C19 C20 H127 107.9(12) . . ? C19 C20 H128 110.8(11) . . ? H127 C20 H128 107.0(15) . . ? C19 C20 H129 112.5(11) . . ? H127 C20 H129 106.0(16) . . ? H128 C20 H129 112.2(16) . . ? C19 C21 H130 112.6(11) . . ? C19 C21 H131 107.4(11) . . ? H130 C21 H131 106.7(15) . . ? C19 C21 H132 111.6(12) . . ? H130 C21 H132 110.6(16) . . ? H131 C21 H132 107.7(15) . . ? C19 C22 H133 112.1(12) . . ? C19 C22 H134 112.9(11) . . ? H133 C22 H134 107.9(16) . . ? C19 C22 H135 110.7(11) . . ? H133 C22 H135 106.2(16) . . ? H134 C22 H135 106.7(15) . . ? C25 C23 C24 106.06(15) . . ? C25 C23 C26 107.59(14) . . ? C24 C23 C26 108.72(15) . . ? C25 C23 C5 117.56(14) . . ? C24 C23 C5 106.31(13) . . ? C26 C23 C5 110.26(14) . . ? C23 C24 H136 112.0(12) . . ? C23 C24 H137 113.2(11) . . ? H136 C24 H137 107.8(16) . . ? C23 C24 H138 110.0(11) . . ? H136 C24 H138 104.2(16) . . ? H137 C24 H138 109.2(15) . . ? C23 C25 H139 104.5(11) . . ? C23 C25 H140 113.6(10) . . ? H139 C25 H140 110.2(15) . . ? C23 C25 H189 113.9(10) . . ? H139 C25 H189 108.4(14) . . ? H140 C25 H189 106.1(14) . . ? C23 C26 H142 106.0(11) . . ? C23 C26 H143 112.5(11) . . ? H142 C26 H143 108.8(15) . . ? C23 C26 H144 111.3(10) . . ? H142 C26 H144 109.7(15) . . ? H143 C26 H144 108.5(15) . . ? C28 C27 C32 121.91(14) . . ? C28 C27 N6 118.94(13) . . ? C32 C27 N6 119.10(14) . . ? C29 C28 C27 117.68(15) . . ? C29 C28 C36 119.36(15) . . ? C27 C28 C36 122.92(14) . . ? C30 C29 C28 121.52(16) . . ? C30 C29 H145 119.8(10) . . ? C28 C29 H145 118.7(10) . . ? C29 C30 C31 119.80(16) . . ? C29 C30 H146 119.7(10) . . ? C31 C30 H146 120.4(10) . . ? C30 C31 C32 121.42(16) . . ? C30 C31 H147 121.6(10) . . ? C32 C31 H147 116.9(10) . . ? C31 C32 C27 117.50(15) . . ? C31 C32 C33 118.45(14) . . ? C27 C32 C33 124.05(14) . . ? C32 C33 C34 110.51(14) . . ? C32 C33 C35 112.98(14) . . ? C34 C33 C35 109.15(15) . . ? C32 C33 H148 110.0(9) . . ? C34 C33 H148 106.4(9) . . ? C35 C33 H148 107.6(9) . . ? C33 C34 H149 109.8(10) . . ? C33 C34 H150 111.4(12) . . ? H149 C34 H150 109.2(15) . . ? C33 C34 H151 112.0(12) . . ? H149 C34 H151 107.6(16) . . ? H150 C34 H151 106.7(16) . . ? C33 C35 H152 107.5(12) . . ? C33 C35 H153 112.3(11) . . ? H152 C35 H153 108.7(16) . . ? C33 C35 H154 113.8(11) . . ? H152 C35 H154 105.9(16) . . ? H153 C35 H154 108.3(16) . . ? C28 C36 C38 111.35(14) . . ? C28 C36 C37 111.58(15) . . ? C38 C36 C37 109.80(16) . . ? C28 C36 H155 109.4(10) . . ? C38 C36 H155 107.2(10) . . ? C37 C36 H155 107.3(10) . . ? C36 C37 H156 110.4(15) . . ? C36 C37 H157 110.8(13) . . ? H156 C37 H157 107.3(19) . . ? C36 C37 H158 112.7(12) . . ? H156 C37 H158 106.7(18) . . ? H157 C37 H158 108.9(17) . . ? C36 C38 H159 109.4(11) . . ? C36 C38 H160 111.1(12) . . ? H159 C38 H160 110.3(17) . . ? C36 C38 H161 111.6(11) . . ? H159 C38 H161 110.1(16) . . ? H160 C38 H161 104.3(16) . . ? C40 N39 Ti1 173.59(11) . . ? N39 C40 C41 121.70(14) . . ? N39 C40 C45 119.03(14) . . ? C41 C40 C45 119.27(14) . . ? C42 C41 C40 118.68(15) . . ? C42 C41 C49 117.97(15) . . ? C40 C41 C49 123.35(14) . . ? C43 C42 C41 122.16(16) . . ? C43 C42 H162 119.3(10) . . ? C41 C42 H162 118.6(10) . . ? C44 C43 C42 118.91(16) . . ? C44 C43 H163 119.7(11) . . ? C42 C43 H163 121.3(11) . . ? C43 C44 C45 121.79(16) . . ? C43 C44 H164 120.6(11) . . ? C45 C44 H164 117.6(11) . . ? C44 C45 C40 119.13(15) . . ? C44 C45 C46 118.25(14) . . ? C40 C45 C46 122.62(14) . . ? C45 C46 C48 111.31(14) . . ? C45 C46 C47 111.64(15) . . ? C48 C46 C47 110.25(15) . . ? C45 C46 H165 105.2(9) . . ? C48 C46 H165 110.2(10) . . ? C47 C46 H165 108.1(9) . . ? C46 C47 H166 109.4(12) . . ? C46 C47 H167 110.0(11) . . ? H166 C47 H167 110.1(16) . . ? C46 C47 H168 110.6(12) . . ? H166 C47 H168 109.5(17) . . ? H167 C47 H168 107.3(17) . . ? C46 C48 H169 110.9(11) . . ? C46 C48 H170 109.8(11) . . ? H169 C48 H170 105.7(15) . . ? C46 C48 H171 111.5(10) . . ? H169 C48 H171 107.5(15) . . ? H170 C48 H171 111.2(15) . . ? C41 C49 C51 111.55(15) . . ? C41 C49 C50 112.10(15) . . ? C51 C49 C50 108.09(17) . . ? C41 C49 H172 109.4(10) . . ? C51 C49 H172 109.0(11) . . ? C50 C49 H172 106.5(11) . . ? C49 C50 H173 110.9(10) . . ? C49 C50 H174 110.7(12) . . ? H173 C50 H174 109.3(15) . . ? C49 C50 H175 111.1(11) . . ? H173 C50 H175 105.1(15) . . ? H174 C50 H175 109.7(16) . . ? C49 C51 H176 110.5(12) . . ? C49 C51 H177 111.9(14) . . ? H176 C51 H177 104.4(19) . . ? C49 C51 H178 112.0(12) . . ? H176 C51 H178 111.7(17) . . ? H177 C51 H178 106.0(18) . . ? C53 O52 C55 125.6(10) . . ? C53 O52 Ti1 123.9(8) . . ? C55 O52 Ti1 110.6(8) . . ? O52 C53 C54 112.3(7) . . ? O52 C53 H179 103(2) . . ? C54 C53 H179 116(2) . . ? O52 C53 H180 106(2) . . ? C54 C53 H180 110(2) . . ? H179 C53 H180 109(3) . . ? O52 C53 H1A 84.6(19) . . ? C54 C53 H1A 35.3(17) . . ? H179 C53 H1A 147(3) . . ? H180 C53 H1A 99(3) . . ? O52 C53 H2A 108(6) . . ? C54 C53 H2A 128(7) . . ? H179 C53 H2A 85(7) . . ? H180 C53 H2A 25(8) . . ? H1A C53 H2A 124(7) . . ? C53 C54 H181 109(2) . . ? C53 C54 H182 112(2) . . ? H181 C54 H182 108(3) . . ? C53 C54 H183 110(2) . . ? H181 C54 H183 104(3) . . ? H182 C54 H183 113(3) . . ? C53 C54 H1A 63(3) . . ? H181 C54 H1A 140(3) . . ? H182 C54 H1A 52(3) . . ? H183 C54 H1A 116(3) . . ? O52 C55 C56 95.2(9) . . ? O52 C55 H184 98(2) . . ? C56 C55 H184 103(3) . . ? O52 C55 H185 107(2) . . ? C56 C55 H185 113(3) . . ? H184 C55 H185 133(4) . . ? O52 C55 H7A 104(5) . . ? C56 C55 H7A 68(5) . . ? H184 C55 H7A 156(5) . . ? H185 C55 H7A 45(4) . . ? O52 C55 H8A 112(3) . . ? C56 C55 H8A 150(3) . . ? H184 C55 H8A 61(4) . . ? H185 C55 H8A 73(4) . . ? H7A C55 H8A 115(6) . . ? C55 C56 H186 117(3) . . ? C55 C56 H187 113(3) . . ? H186 C56 H187 106(4) . . ? C55 C56 H188 102(3) . . ? H186 C56 H188 107(4) . . ? H187 C56 H188 111(4) . . ? C55 C56 H5A 89(2) . . ? H186 C56 H5A 73(3) . . ? H187 C56 H5A 154(4) . . ? H188 C56 H5A 48(3) . . ? C55 C56 H7A 25(2) . . ? H186 C56 H7A 142(4) . . ? H187 C56 H7A 94(3) . . ? H188 C56 H7A 95(3) . . ? H5A C56 H7A 103(3) . . ? C80 B57 C69 103.21(13) . . ? C80 B57 C91 113.20(13) . . ? C69 B57 C91 113.59(13) . . ? C80 B57 C58 113.37(13) . . ? C69 B57 C58 114.27(13) . . ? C91 B57 C58 99.70(13) . . ? C59 C58 C63 112.80(15) . . ? C59 C58 B57 126.88(15) . . ? C63 C58 B57 119.85(14) . . ? F64 C59 C60 114.88(15) . . ? F64 C59 C58 120.71(15) . . ? C60 C59 C58 124.40(16) . . ? F65 C60 C61 119.62(16) . . ? F65 C60 C59 120.54(16) . . ? C61 C60 C59 119.84(17) . . ? F66 C61 C60 120.58(17) . . ? F66 C61 C62 120.83(17) . . ? C60 C61 C62 118.56(16) . . ? F67 C62 C61 119.76(16) . . ? F67 C62 C63 120.54(17) . . ? C61 C62 C63 119.68(16) . . ? F68 C63 C62 115.76(15) . . ? F68 C63 C58 119.52(15) . . ? C62 C63 C58 124.71(16) . . ? C70 C69 C74 112.78(15) . . ? C70 C69 B57 127.32(14) . . ? C74 C69 B57 119.68(14) . . ? F75 C70 C71 115.26(14) . . ? F75 C70 C69 120.62(14) . . ? C71 C70 C69 124.12(15) . . ? F76 C71 C72 119.45(15) . . ? F76 C71 C70 120.46(15) . . ? C72 C71 C70 120.09(15) . . ? F77 C72 C71 120.84(16) . . ? F77 C72 C73 120.48(16) . . ? C71 C72 C73 118.68(15) . . ? F78 C73 C74 121.20(16) . . ? F78 C73 C72 119.71(15) . . ? C74 C73 C72 119.08(16) . . ? F79 C74 C73 115.97(15) . . ? F79 C74 C69 118.82(14) . . ? C73 C74 C69 125.20(16) . . ? C85 C80 C81 112.67(15) . . ? C85 C80 B57 127.92(15) . . ? C81 C80 B57 119.29(14) . . ? F86 C81 C82 116.44(14) . . ? F86 C81 C80 118.72(14) . . ? C82 C81 C80 124.83(15) . . ? F87 C82 C83 119.77(15) . . ? F87 C82 C81 120.81(15) . . ? C83 C82 C81 119.42(16) . . ? F88 C83 C84 120.55(17) . . ? F88 C83 C82 120.60(17) . . ? C84 C83 C82 118.85(16) . . ? F89 C84 C83 119.86(16) . . ? F89 C84 C85 120.29(16) . . ? C83 C84 C85 119.85(16) . . ? F90 C85 C84 115.31(15) . . ? F90 C85 C80 120.38(15) . . ? C84 C85 C80 124.30(16) . . ? C92 C91 C96 113.22(16) . . ? C92 C91 B57 126.88(15) . . ? C96 C91 B57 119.08(15) . . ? F97 C92 C91 120.95(15) . . ? F97 C92 C93 114.95(16) . . ? C91 C92 C93 124.09(18) . . ? F98 C93 C94 119.82(17) . . ? F98 C93 C92 120.42(19) . . ? C94 C93 C92 119.76(18) . . ? F99 C94 C93 120.8(2) . . ? F99 C94 C95 120.35(19) . . ? C93 C94 C95 118.89(17) . . ? F100 C95 C94 119.29(17) . . ? F100 C95 C96 120.97(19) . . ? C94 C95 C96 119.74(18) . . ? F101 C96 C95 116.08(16) . . ? F101 C96 C91 119.66(15) . . ? C95 C96 C91 124.25(18) . . ? F102 C103 C108 117.58(19) . . ? F102 C103 C104 118.56(18) . . ? C108 C103 C104 123.85(19) . . ? C103 C104 C105 117.12(19) . . ? C103 C104 H190 122.3(6) . . ? C105 C104 H190 120.3(6) . . ? C106 C105 C104 120.8(2) . . ? C106 C105 H191 122.0(12) . . ? C104 C105 H191 117.1(12) . . ? C107 C106 C105 120.0(2) . . ? C107 C106 H192 120.2(14) . . ? C105 C106 H192 119.7(14) . . ? C106 C107 C108 120.6(2) . . ? C106 C107 H193 122.3(14) . . ? C108 C107 H193 117.1(15) . . ? C103 C108 C107 117.5(2) . . ? C103 C108 H194 118.3(13) . . ? C107 C108 H194 124.1(13) . . ? C56A O52A C53A 91.4(13) . . ? C56A O52A Ti1 135.5(16) . . ? C53A O52A Ti1 130.4(11) . . ? O52A C53A C54A 105.4(10) . . ? O52A C53A H179 106.7(16) . . ? C54A C53A H179 62.2(15) . . ? O52A C53A H180 99.9(18) . . ? C54A C53A H180 132.3(19) . . ? H179 C53A H180 72(2) . . ? O52A C53A H1A 104(3) . . ? C54A C53A H1A 114(2) . . ? H179 C53A H1A 149(3) . . ? H180 C53A H1A 97(3) . . ? O52A C53A H2A 102(3) . . ? C54A C53A H2A 112(4) . . ? H179 C53A H2A 51(4) . . ? H180 C53A H2A 21(4) . . ? H1A C53A H2A 116(5) . . ? C53A C54A C55A 100.8(5) . . ? C53A C54A C56A 70.6(8) . . ? C55A C54A C56A 39.1(7) . . ? C53A C54A H179 53.6(15) . . ? C55A C54A H179 137.0(13) . . ? C56A C54A H179 98.1(14) . . ? C53A C54A H183 74.3(17) . . ? C55A C54A H183 86.4(15) . . ? C56A C54A H183 101.3(17) . . ? H179 C54A H183 113(2) . . ? C53A C54A H186 137(2) . . ? C55A C54A H186 51(2) . . ? C56A C54A H186 68(2) . . ? H179 C54A H186 121(2) . . ? H183 C54A H186 126(3) . . ? C53A C54A H3A 109(4) . . ? C55A C54A H3A 112(4) . . ? C56A C54A H3A 146(4) . . ? H179 C54A H3A 109(4) . . ? H183 C54A H3A 49(4) . . ? H186 C54A H3A 112(4) . . ? C53A C54A H4A 116(3) . . ? C55A C54A H4A 115(3) . . ? C56A C54A H4A 107(3) . . ? H179 C54A H4A 64(3) . . ? H183 C54A H4A 152(4) . . ? H186 C54A H4A 66(3) . . ? H3A C54A H4A 104(5) . . ? C56A C55A C54A 91.2(9) . . ? C56A C55A H184 44(2) . . ? C54A C55A H184 112.3(16) . . ? C56A C55A H186 101(2) . . ? C54A C55A H186 48(2) . . ? H184 C55A H186 144(3) . . ? C56A C55A H188 88(2) . . ? C54A C55A H188 104.0(17) . . ? H184 C55A H188 118(2) . . ? H186 C55A H188 57(3) . . ? C56A C55A H5A 123(3) . . ? C54A C55A H5A 117(3) . . ? H184 C55A H5A 130(3) . . ? H186 C55A H5A 72(3) . . ? H188 C55A H5A 40(3) . . ? C56A C55A H6A 120(3) . . ? C54A C55A H6A 114(3) . . ? H184 C55A H6A 75(3) . . ? H186 C55A H6A 137(4) . . ? H188 C55A H6A 131(4) . . ? H5A C55A H6A 94(4) . . ? C55A C56A O52A 131.3(17) . . ? C55A C56A C54A 49.7(6) . . ? O52A C56A C54A 87.6(10) . . ? C55A C56A H184 68(3) . . ? O52A C56A H184 102(3) . . ? C54A C56A H184 97(3) . . ? C55A C56A H185 136(3) . . ? O52A C56A H185 92(2) . . ? C54A C56A H185 161(3) . . ? H184 C56A H185 101(3) . . ? C55A C56A H7A 119(4) . . ? O52A C56A H7A 106(4) . . ? C54A C56A H7A 131(4) . . ? H184 C56A H7A 124(4) . . ? H185 C56A H7A 31(4) . . ? C55A C56A H8A 110(4) . . ? O52A C56A H8A 92(3) . . ? C54A C56A H8A 145(4) . . ? H184 C56A H8A 49(3) . . ? H185 C56A H8A 54(3) . . ? H7A C56A H8A 82(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 N39 Ti1 N2 C3 -171.08(9) . . . . ? O52A Ti1 N2 C3 66.0(4) . . . . ? N6 Ti1 N2 C3 -54.58(10) . . . . ? O52 Ti1 N2 C3 75.1(3) . . . . ? N39 Ti1 N2 C7 18.77(14) . . . . ? O52A Ti1 N2 C7 -104.2(4) . . . . ? N6 Ti1 N2 C7 135.27(13) . . . . ? O52 Ti1 N2 C7 -95.1(3) . . . . ? C3 Ti1 N2 C7 -170.15(19) . . . . ? C7 N2 C3 C4 -154.97(14) . . . . ? Ti1 N2 C3 C4 33.90(17) . . . . ? C7 N2 C3 C19 30.9(2) . . . . ? Ti1 N2 C3 C19 -140.20(13) . . . . ? C7 N2 C3 Ti1 171.13(17) . . . . ? N39 Ti1 C3 N2 12.83(13) . . . . ? O52A Ti1 C3 N2 -123.6(3) . . . . ? N6 Ti1 C3 N2 125.29(10) . . . . ? O52 Ti1 C3 N2 -114.3(3) . . . . ? N39 Ti1 C3 C4 -137.81(10) . . . . ? N2 Ti1 C3 C4 -150.64(15) . . . . ? O52A Ti1 C3 C4 85.7(3) . . . . ? N6 Ti1 C3 C4 -25.35(9) . . . . ? O52 Ti1 C3 C4 95.1(3) . . . . ? N39 Ti1 C3 C19 95.3(2) . . . . ? N2 Ti1 C3 C19 82.5(2) . . . . ? O52A Ti1 C3 C19 -41.1(4) . . . . ? N6 Ti1 C3 C19 -152.2(2) . . . . ? O52 Ti1 C3 C19 -31.8(3) . . . . ? N2 C3 C4 C5 16.4(3) . . . . ? C19 C3 C4 C5 -169.09(17) . . . . ? Ti1 C3 C4 C5 39.39(19) . . . . ? C3 C4 C5 N6 -34.5(3) . . . . ? C3 C4 C5 C23 144.13(18) . . . . ? C4 C5 N6 C27 -174.50(14) . . . . ? C23 C5 N6 C27 7.1(2) . . . . ? C4 C5 N6 Ti1 -5.29(17) . . . . ? C23 C5 N6 Ti1 176.33(13) . . . . ? N39 Ti1 N6 C5 156.94(10) . . . . ? N2 Ti1 N6 C5 40.96(11) . . . . ? O52A Ti1 N6 C5 -83.2(6) . . . . ? O52 Ti1 N6 C5 -83.1(5) . . . . ? C3 Ti1 N6 C5 17.33(10) . . . . ? N39 Ti1 N6 C27 -33.84(13) . . . . ? N2 Ti1 N6 C27 -149.82(12) . . . . ? O52A Ti1 N6 C27 86.0(6) . . . . ? O52 Ti1 N6 C27 86.1(5) . . . . ? C3 Ti1 N6 C27 -173.45(12) . . . . ? C3 N2 C7 C12 -103.68(17) . . . . ? Ti1 N2 C7 C12 65.19(19) . . . . ? C3 N2 C7 C8 77.96(18) . . . . ? Ti1 N2 C7 C8 -113.17(14) . . . . ? C12 C7 C8 C9 6.5(2) . . . . ? N2 C7 C8 C9 -175.15(14) . . . . ? C12 C7 C8 C16 -173.08(15) . . . . ? N2 C7 C8 C16 5.3(2) . . . . ? C7 C8 C9 C10 -1.5(2) . . . . ? C16 C8 C9 C10 178.05(16) . . . . ? C8 C9 C10 C11 -3.4(3) . . . . ? C9 C10 C11 C12 3.5(3) . . . . ? C10 C11 C12 C7 1.3(2) . . . . ? C10 C11 C12 C13 -178.60(15) . . . . ? C8 C7 C12 C11 -6.4(2) . . . . ? N2 C7 C12 C11 175.34(14) . . . . ? C8 C7 C12 C13 173.48(15) . . . . ? N2 C7 C12 C13 -4.8(2) . . . . ? C11 C12 C13 C14 -50.2(2) . . . . ? C7 C12 C13 C14 129.97(17) . . . . ? C11 C12 C13 C15 72.30(19) . . . . ? C7 C12 C13 C15 -107.54(18) . . . . ? C9 C8 C16 C18 89.7(2) . . . . ? C7 C8 C16 C18 -90.7(2) . . . . ? C9 C8 C16 C17 -33.0(2) . . . . ? C7 C8 C16 C17 146.55(17) . . . . ? N2 C3 C19 C21 -39.9(2) . . . . ? C4 C3 C19 C21 145.87(16) . . . . ? Ti1 C3 C19 C21 -96.0(2) . . . . ? N2 C3 C19 C22 80.58(19) . . . . ? C4 C3 C19 C22 -93.70(17) . . . . ? Ti1 C3 C19 C22 24.4(3) . . . . ? N2 C3 C19 C20 -161.47(16) . . . . ? C4 C3 C19 C20 24.3(2) . . . . ? Ti1 C3 C19 C20 142.40(18) . . . . ? N6 C5 C23 C25 4.8(2) . . . . ? C4 C5 C23 C25 -173.68(15) . . . . ? N6 C5 C23 C24 123.35(17) . . . . ? C4 C5 C23 C24 -55.14(18) . . . . ? N6 C5 C23 C26 -118.97(18) . . . . ? C4 C5 C23 C26 62.54(18) . . . . ? C5 N6 C27 C28 -106.83(17) . . . . ? Ti1 N6 C27 C28 85.38(16) . . . . ? C5 N6 C27 C32 75.83(19) . . . . ? Ti1 N6 C27 C32 -91.95(15) . . . . ? C32 C27 C28 C29 -4.7(2) . . . . ? N6 C27 C28 C29 178.05(14) . . . . ? C32 C27 C28 C36 177.35(15) . . . . ? N6 C27 C28 C36 0.1(2) . . . . ? C27 C28 C29 C30 3.1(2) . . . . ? C36 C28 C29 C30 -178.89(16) . . . . ? C28 C29 C30 C31 0.2(3) . . . . ? C29 C30 C31 C32 -2.1(3) . . . . ? C30 C31 C32 C27 0.6(2) . . . . ? C30 C31 C32 C33 -179.25(15) . . . . ? C28 C27 C32 C31 2.9(2) . . . . ? N6 C27 C32 C31 -179.83(14) . . . . ? C28 C27 C32 C33 -177.29(15) . . . . ? N6 C27 C32 C33 0.0(2) . . . . ? C31 C32 C33 C34 -78.60(19) . . . . ? C27 C32 C33 C34 101.61(18) . . . . ? C31 C32 C33 C35 44.0(2) . . . . ? C27 C32 C33 C35 -135.76(17) . . . . ? C29 C28 C36 C38 46.9(2) . . . . ? C27 C28 C36 C38 -135.20(16) . . . . ? C29 C28 C36 C37 -76.2(2) . . . . ? C27 C28 C36 C37 101.72(19) . . . . ? N2 Ti1 N39 C40 -170.4(10) . . . . ? O52A Ti1 N39 C40 -41.6(11) . . . . ? N6 Ti1 N39 C40 81.5(10) . . . . ? O52 Ti1 N39 C40 -49.5(10) . . . . ? C3 Ti1 N39 C40 -177.0(9) . . . . ? Ti1 N39 C40 C41 171.6(9) . . . . ? Ti1 N39 C40 C45 -8.4(11) . . . . ? N39 C40 C41 C42 177.89(14) . . . . ? C45 C40 C41 C42 -2.1(2) . . . . ? N39 C40 C41 C49 -2.1(2) . . . . ? C45 C40 C41 C49 177.89(14) . . . . ? C40 C41 C42 C43 0.2(2) . . . . ? C49 C41 C42 C43 -179.82(16) . . . . ? C41 C42 C43 C44 1.2(3) . . . . ? C42 C43 C44 C45 -0.7(3) . . . . ? C43 C44 C45 C40 -1.2(2) . . . . ? C43 C44 C45 C46 179.38(15) . . . . ? N39 C40 C45 C44 -177.37(14) . . . . ? C41 C40 C45 C44 2.6(2) . . . . ? N39 C40 C45 C46 2.0(2) . . . . ? C41 C40 C45 C46 -178.01(14) . . . . ? C44 C45 C46 C48 69.11(19) . . . . ? C40 C45 C46 C48 -110.26(17) . . . . ? C44 C45 C46 C47 -54.6(2) . . . . ? C40 C45 C46 C47 126.07(17) . . . . ? C42 C41 C49 C51 -69.9(2) . . . . ? C40 C41 C49 C51 110.1(2) . . . . ? C42 C41 C49 C50 51.5(2) . . . . ? C40 C41 C49 C50 -128.49(17) . . . . ? N39 Ti1 O52 C53 -10.8(9) . . . . ? N2 Ti1 O52 C53 108.1(9) . . . . ? O52A Ti1 O52 C53 -135(7) . . . . ? N6 Ti1 O52 C53 -135.2(7) . . . . ? C3 Ti1 O52 C53 137.0(8) . . . . ? N39 Ti1 O52 C55 168.4(10) . . . . ? N2 Ti1 O52 C55 -72.7(10) . . . . ? O52A Ti1 O52 C55 45(6) . . . . ? N6 Ti1 O52 C55 44.0(12) . . . . ? C3 Ti1 O52 C55 -43.8(11) . . . . ? C55 O52 C53 C54 -49.8(16) . . . . ? Ti1 O52 C53 C54 129.2(7) . . . . ? C53 O52 C55 C56 -46.9(17) . . . . ? Ti1 O52 C55 C56 133.9(7) . . . . ? C80 B57 C58 C59 -135.78(17) . . . . ? C69 B57 C58 C59 -17.9(2) . . . . ? C91 B57 C58 C59 103.60(18) . . . . ? C80 B57 C58 C63 52.7(2) . . . . ? C69 B57 C58 C63 170.58(15) . . . . ? C91 B57 C58 C63 -67.94(18) . . . . ? C63 C58 C59 F64 177.64(15) . . . . ? B57 C58 C59 F64 5.6(3) . . . . ? C63 C58 C59 C60 -1.1(3) . . . . ? B57 C58 C59 C60 -173.12(17) . . . . ? F64 C59 C60 F65 0.8(3) . . . . ? C58 C59 C60 F65 179.63(16) . . . . ? F64 C59 C60 C61 -178.48(16) . . . . ? C58 C59 C60 C61 0.3(3) . . . . ? F65 C60 C61 F66 -0.7(3) . . . . ? C59 C60 C61 F66 178.59(17) . . . . ? F65 C60 C61 C62 -178.83(17) . . . . ? C59 C60 C61 C62 0.5(3) . . . . ? F66 C61 C62 F67 -0.2(3) . . . . ? C60 C61 C62 F67 177.93(17) . . . . ? F66 C61 C62 C63 -178.52(18) . . . . ? C60 C61 C62 C63 -0.4(3) . . . . ? F67 C62 C63 F68 -0.1(3) . . . . ? C61 C62 C63 F68 178.27(17) . . . . ? F67 C62 C63 C58 -178.80(17) . . . . ? C61 C62 C63 C58 -0.5(3) . . . . ? C59 C58 C63 F68 -177.52(15) . . . . ? B57 C58 C63 F68 -4.9(2) . . . . ? C59 C58 C63 C62 1.2(3) . . . . ? B57 C58 C63 C62 173.82(17) . . . . ? C80 B57 C69 C70 -105.25(18) . . . . ? C91 B57 C69 C70 17.7(2) . . . . ? C58 B57 C69 C70 131.19(17) . . . . ? C80 B57 C69 C74 69.06(18) . . . . ? C91 B57 C69 C74 -167.98(14) . . . . ? C58 B57 C69 C74 -54.5(2) . . . . ? C74 C69 C70 F75 -177.72(13) . . . . ? B57 C69 C70 F75 -3.1(2) . . . . ? C74 C69 C70 C71 2.1(2) . . . . ? B57 C69 C70 C71 176.70(15) . . . . ? F75 C70 C71 F76 -1.3(2) . . . . ? C69 C70 C71 F76 178.86(14) . . . . ? F75 C70 C71 C72 179.09(14) . . . . ? C69 C70 C71 C72 -0.7(3) . . . . ? F76 C71 C72 F77 -0.2(2) . . . . ? C70 C71 C72 F77 179.40(14) . . . . ? F76 C71 C72 C73 179.94(14) . . . . ? C70 C71 C72 C73 -0.5(2) . . . . ? F77 C72 C73 F78 0.6(2) . . . . ? C71 C72 C73 F78 -179.53(15) . . . . ? F77 C72 C73 C74 -179.76(15) . . . . ? C71 C72 C73 C74 0.1(2) . . . . ? F78 C73 C74 F79 0.5(2) . . . . ? C72 C73 C74 F79 -179.20(14) . . . . ? F78 C73 C74 C69 -178.85(15) . . . . ? C72 C73 C74 C69 1.5(3) . . . . ? C70 C69 C74 F79 178.22(14) . . . . ? B57 C69 C74 F79 3.1(2) . . . . ? C70 C69 C74 C73 -2.5(2) . . . . ? B57 C69 C74 C73 -177.58(15) . . . . ? C69 B57 C80 C85 -107.09(18) . . . . ? C91 B57 C80 C85 129.70(17) . . . . ? C58 B57 C80 C85 17.1(2) . . . . ? C69 B57 C80 C81 68.75(18) . . . . ? C91 B57 C80 C81 -54.5(2) . . . . ? C58 B57 C80 C81 -167.10(14) . . . . ? C85 C80 C81 F86 177.99(14) . . . . ? B57 C80 C81 F86 1.5(2) . . . . ? C85 C80 C81 C82 -3.0(2) . . . . ? B57 C80 C81 C82 -179.48(15) . . . . ? F86 C81 C82 F87 1.2(2) . . . . ? C80 C81 C82 F87 -177.81(15) . . . . ? F86 C81 C82 C83 -179.58(14) . . . . ? C80 C81 C82 C83 1.4(3) . . . . ? F87 C82 C83 F88 0.4(2) . . . . ? C81 C82 C83 F88 -178.84(15) . . . . ? F87 C82 C83 C84 179.82(15) . . . . ? C81 C82 C83 C84 0.6(3) . . . . ? F88 C83 C84 F89 -0.7(3) . . . . ? C82 C83 C84 F89 179.92(15) . . . . ? F88 C83 C84 C85 178.75(15) . . . . ? C82 C83 C84 C85 -0.7(3) . . . . ? F89 C84 C85 F90 -1.3(2) . . . . ? C83 C84 C85 F90 179.33(15) . . . . ? F89 C84 C85 C80 178.16(16) . . . . ? C83 C84 C85 C80 -1.3(3) . . . . ? C81 C80 C85 F90 -177.67(14) . . . . ? B57 C80 C85 F90 -1.6(3) . . . . ? C81 C80 C85 C84 2.9(2) . . . . ? B57 C80 C85 C84 179.00(16) . . . . ? C80 B57 C91 C92 -21.1(2) . . . . ? C69 B57 C91 C92 -138.34(17) . . . . ? C58 B57 C91 C92 99.68(18) . . . . ? C80 B57 C91 C96 170.06(14) . . . . ? C69 B57 C91 C96 52.8(2) . . . . ? C58 B57 C91 C96 -69.20(17) . . . . ? C96 C91 C92 F97 -179.55(14) . . . . ? B57 C91 C92 F97 11.0(3) . . . . ? C96 C91 C92 C93 1.4(2) . . . . ? B57 C91 C92 C93 -168.02(17) . . . . ? F97 C92 C93 F98 -1.2(3) . . . . ? C91 C92 C93 F98 177.93(16) . . . . ? F97 C92 C93 C94 179.32(16) . . . . ? C91 C92 C93 C94 -1.6(3) . . . . ? F98 C93 C94 F99 0.3(3) . . . . ? C92 C93 C94 F99 179.78(16) . . . . ? F98 C93 C94 C95 -179.98(17) . . . . ? C92 C93 C94 C95 -0.5(3) . . . . ? F99 C94 C95 F100 1.3(3) . . . . ? C93 C94 C95 F100 -178.45(16) . . . . ? F99 C94 C95 C96 -177.75(16) . . . . ? C93 C94 C95 C96 2.5(3) . . . . ? F100 C95 C96 F101 -2.9(2) . . . . ? C94 C95 C96 F101 176.16(15) . . . . ? F100 C95 C96 C91 178.24(15) . . . . ? C94 C95 C96 C91 -2.7(3) . . . . ? C92 C91 C96 F101 -178.10(14) . . . . ? B57 C91 C96 F101 -7.8(2) . . . . ? C92 C91 C96 C95 0.7(2) . . . . ? B57 C91 C96 C95 171.09(16) . . . . ? F102 C103 C104 C105 177.82(17) . . . . ? C108 C103 C104 C105 -1.1(3) . . . . ? C103 C104 C105 C106 1.0(3) . . . . ? C104 C105 C106 C107 -0.1(3) . . . . ? C105 C106 C107 C108 -0.8(3) . . . . ? F102 C103 C108 C107 -178.65(18) . . . . ? C104 C103 C108 C107 0.2(3) . . . . ? C106 C107 C108 C103 0.7(3) . . . . ? N39 Ti1 O52A C56A -169.0(18) . . . . ? N2 Ti1 O52A C56A -44.2(19) . . . . ? N6 Ti1 O52A C56A 68.6(19) . . . . ? O52 Ti1 O52A C56A -111(7) . . . . ? C3 Ti1 O52A C56A -17.1(19) . . . . ? N39 Ti1 O52A C53A -13.1(14) . . . . ? N2 Ti1 O52A C53A 111.7(13) . . . . ? N6 Ti1 O52A C53A -135.5(11) . . . . ? O52 Ti1 O52A C53A 45(5) . . . . ? C3 Ti1 O52A C53A 138.8(13) . . . . ? C56A O52A C53A C54A 21.2(15) . . . . ? Ti1 O52A C53A C54A -142.2(11) . . . . ? O52A C53A C54A C55A -40.6(9) . . . . ? O52A C53A C54A C56A -15.4(11) . . . . ? C53A C54A C55A C56A 39.6(14) . . . . ? C54A C55A C56A O52A -35(3) . . . . ? C53A O52A C56A C55A 11(3) . . . . ? Ti1 O52A C56A C55A 172.6(16) . . . . ? C53A O52A C56A C54A -15.2(11) . . . . ? Ti1 O52A C56A C54A 146.7(12) . . . . ? C53A C54A C56A C55A -138.4(14) . . . . ? C53A C54A C56A O52A 16.0(12) . . . . ? C55A C54A C56A O52A 154(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.369 _refine_diff_density_min -0.323 _refine_diff_density_rms 0.047 data_04302 _database_code_depnum_ccdc_archive 'CCDC 260840' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C55 H81 N4 Ti, C24 B F20' _chemical_formula_sum 'C79 H81 B F20 N4 Ti' _chemical_formula_weight 1525.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' 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' B B 0.0013 0.0007 '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 12.6445(17) _cell_length_b 17.067(2) _cell_length_c 17.378(2) _cell_angle_alpha 94.190(4) _cell_angle_beta 106.094(4) _cell_angle_gamma 93.621(4) _cell_volume 3580.0(8) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 970 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 26.99 _exptl_crystal_description irregular _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1580 _exptl_absorpt_coefficient_mu 0.220 _exptl_absorpt_correction_type none _exptl_special_details ; Crystals diffracted weakly and reflections were broad. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details ' 0.30 degree frames measured for 30.17 seconds each' _diffrn_measurement_method '\w scans' _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 22136 _diffrn_reflns_av_R_equivalents 0.0653 _diffrn_reflns_av_sigmaI/netI 0.1982 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.54 _reflns_number_total 16157 _reflns_number_gt 6812 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999), XTEL (local program)' _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. All hydrogens except those on C59 and C60 were refined. Some hydrogen parameters are outside of normally expected range but all are qualatively correct. ; _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^)+(0.0368P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16157 _refine_ls_number_parameters 1248 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1420 _refine_ls_R_factor_gt 0.0577 _refine_ls_wR_factor_ref 0.1293 _refine_ls_wR_factor_gt 0.1100 _refine_ls_goodness_of_fit_ref 0.874 _refine_ls_restrained_S_all 0.874 _refine_ls_shift/su_max 0.007 _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 0.95472(5) 0.82246(4) 0.76274(4) 0.01782(16) Uani 1 1 d . . . N2 N 1.1091(2) 0.84111(18) 0.74609(17) 0.0199(7) Uani 1 1 d . . . C3 C 1.1667(3) 0.7829(2) 0.7775(2) 0.0215(9) Uani 1 1 d . . . C4 C 1.1126(3) 0.7186(2) 0.8058(2) 0.0223(9) Uani 1 1 d . . . C5 C 1.0088(3) 0.6763(2) 0.7791(2) 0.0178(8) Uani 1 1 d . . . N6 N 0.9238(2) 0.70816(17) 0.72686(16) 0.0174(7) Uani 1 1 d . . . C7 C 1.1543(3) 0.9104(2) 0.7190(2) 0.0217(9) Uani 1 1 d . . . C8 C 1.1332(3) 0.9144(2) 0.6363(2) 0.0267(9) Uani 1 1 d . . . C9 C 1.1797(3) 0.9809(3) 0.6104(3) 0.0323(10) Uani 1 1 d . . . C10 C 1.2405(3) 1.0413(3) 0.6647(3) 0.0346(11) Uani 1 1 d . . . C11 C 1.2558(3) 1.0367(3) 0.7447(3) 0.0314(10) Uani 1 1 d . . . C12 C 1.2153(3) 0.9721(2) 0.7746(2) 0.0270(10) Uani 1 1 d . . . C13 C 1.2438(3) 0.9730(3) 0.8659(3) 0.0297(10) Uani 1 1 d . . . C14 C 1.3678(3) 0.9914(3) 0.9074(3) 0.0401(12) Uani 1 1 d . . . C15 C 1.1822(4) 1.0337(3) 0.9018(3) 0.0391(12) Uani 1 1 d . . . C16 C 1.0675(3) 0.8504(3) 0.5726(2) 0.0316(10) Uani 1 1 d . . . C17 C 0.9825(4) 0.8844(3) 0.5062(3) 0.0420(12) Uani 1 1 d . . . C18 C 1.1432(5) 0.8016(4) 0.5375(4) 0.0539(14) Uani 1 1 d . . . C19 C 1.2920(3) 0.7730(2) 0.7879(3) 0.0322(10) Uani 1 1 d . . . C20 C 1.3532(4) 0.7773(3) 0.8773(3) 0.0432(13) Uani 1 1 d . . . C21 C 1.3522(3) 0.8316(3) 0.7479(3) 0.0387(12) Uani 1 1 d . . . C22 C 1.2977(4) 0.6898(3) 0.7479(4) 0.0420(13) Uani 1 1 d . . . C23 C 0.9973(3) 0.5975(2) 0.8185(2) 0.0231(9) Uani 1 1 d . . . C24 C 1.1067(3) 0.5583(3) 0.8414(3) 0.0304(10) Uani 1 1 d . . . C25 C 0.9102(3) 0.5339(3) 0.7675(3) 0.0266(10) Uani 1 1 d . . . C26 C 0.9668(4) 0.6196(3) 0.8966(3) 0.0335(11) Uani 1 1 d . . . C27 C 0.8296(3) 0.6619(2) 0.6735(2) 0.0196(8) Uani 1 1 d . . . C28 C 0.8399(3) 0.6232(2) 0.6018(2) 0.0224(9) Uani 1 1 d . . . C29 C 0.7505(3) 0.5759(3) 0.5531(3) 0.0330(10) Uani 1 1 d . . . C30 C 0.6511(3) 0.5703(3) 0.5719(3) 0.0369(11) Uani 1 1 d . . . C31 C 0.6396(3) 0.6110(3) 0.6388(3) 0.0336(11) Uani 1 1 d . . . C32 C 0.7273(3) 0.6577(2) 0.6920(2) 0.0216(8) Uani 1 1 d . . . C33 C 0.7101(3) 0.6988(2) 0.7674(2) 0.0251(9) Uani 1 1 d . . . C34 C 0.6613(4) 0.6413(3) 0.8135(3) 0.0392(12) Uani 1 1 d . . . C35 C 0.6363(3) 0.7669(3) 0.7485(3) 0.0309(10) Uani 1 1 d . . . C36 C 0.9458(3) 0.6340(2) 0.5768(2) 0.0259(9) Uani 1 1 d . . . C37 C 1.0252(3) 0.5707(3) 0.6051(3) 0.0314(10) Uani 1 1 d . . . C38 C 0.9239(4) 0.6347(3) 0.4859(3) 0.0417(12) Uani 1 1 d . . . N39 N 0.8673(2) 0.87773(17) 0.69864(16) 0.0183(7) Uani 1 1 d . . . C40 C 0.8028(3) 0.9297(2) 0.6499(2) 0.0207(8) Uani 1 1 d . . . C41 C 0.7108(3) 0.8994(2) 0.5842(2) 0.0237(9) Uani 1 1 d . . . C42 C 0.6514(3) 0.9532(3) 0.5368(3) 0.0311(10) Uani 1 1 d . . . C43 C 0.6782(3) 1.0335(3) 0.5523(3) 0.0325(10) Uani 1 1 d . . . C44 C 0.7667(3) 1.0619(3) 0.6169(3) 0.0305(10) Uani 1 1 d . . . C45 C 0.8310(3) 1.0117(2) 0.6657(2) 0.0232(9) Uani 1 1 d . . . C46 C 0.9244(3) 1.0470(2) 0.7362(2) 0.0244(9) Uani 1 1 d . . . C47 C 0.8807(4) 1.0748(3) 0.8070(3) 0.0428(13) Uani 1 1 d . . . C48 C 0.9965(4) 1.1134(3) 0.7182(3) 0.0389(12) Uani 1 1 d . . . C49 C 0.6762(3) 0.8126(2) 0.5637(2) 0.0261(9) Uani 1 1 d . . . C50 C 0.5506(3) 0.7946(3) 0.5423(3) 0.0324(11) Uani 1 1 d . . . C51 C 0.7197(4) 0.7789(3) 0.4972(3) 0.0350(11) Uani 1 1 d . . . C52 C 0.9625(3) 0.8814(3) 0.8901(3) 0.0319(11) Uani 1 1 d . . . C53 C 0.8522(4) 0.8751(3) 0.8899(3) 0.0412(12) Uani 1 1 d . . . C54 C 0.8157(3) 0.8254(3) 0.9396(3) 0.0384(11) Uani 1 1 d . . . C55 C 0.8912(3) 0.7872(3) 0.9970(2) 0.0346(10) Uani 1 1 d . . . C56 C 1.0036(3) 0.7998(3) 1.0014(2) 0.0317(10) Uani 1 1 d . . . C57 C 1.0385(3) 0.8463(3) 0.9505(2) 0.0277(10) Uani 1 1 d . . . N58 N 0.8567(3) 0.7402(2) 1.0467(2) 0.0413(10) Uani 1 1 d . . . C59 C 0.7421(3) 0.7304(3) 1.0483(3) 0.0508(13) Uani 1 1 d . . . H183 H 0.7187 0.7815 1.0634 0.076 Uiso 1 1 calc R . . H182 H 0.7352 0.6934 1.0876 0.076 Uiso 1 1 calc R . . H181 H 0.6951 0.7095 0.9948 0.076 Uiso 1 1 calc R . . C60 C 0.9371(4) 0.6988(3) 1.1054(3) 0.0517(13) Uani 1 1 d . . . H186 H 0.9781 0.6662 1.0770 0.078 Uiso 1 1 calc R . . H184 H 0.8977 0.6651 1.1337 0.078 Uiso 1 1 calc R . . H185 H 0.9888 0.7376 1.1444 0.078 Uiso 1 1 calc R . . B61 B 0.4301(3) 0.6879(3) 0.2061(3) 0.0241(10) Uani 1 1 d . . . C62 C 0.3586(3) 0.6676(2) 0.2709(2) 0.0289(10) Uani 1 1 d . . . C63 C 0.2469(3) 0.6749(3) 0.2492(2) 0.0330(10) Uani 1 1 d . . . C64 C 0.1783(3) 0.6628(2) 0.2994(3) 0.0335(10) Uani 1 1 d . . . C65 C 0.2259(3) 0.6431(3) 0.3743(2) 0.0334(10) Uani 1 1 d . . . C66 C 0.3349(3) 0.6364(2) 0.4015(2) 0.0338(10) Uani 1 1 d . . . C67 C 0.4017(3) 0.6498(2) 0.3501(2) 0.0270(9) Uani 1 1 d . . . F68 F 0.19676(15) 0.69538(14) 0.17383(14) 0.0372(6) Uani 1 1 d . . . F69 F 0.07012(18) 0.67015(16) 0.27129(16) 0.0523(7) Uani 1 1 d . . . F70 F 0.1597(2) 0.62861(16) 0.42298(15) 0.0526(7) Uani 1 1 d . . . F71 F 0.38063(19) 0.61817(15) 0.47615(13) 0.0450(7) Uani 1 1 d . . . F72 F 0.50825(17) 0.64290(14) 0.38245(12) 0.0373(6) Uani 1 1 d . . . C73 C 0.4187(3) 0.7824(2) 0.1977(2) 0.0212(9) Uani 1 1 d . . . C74 C 0.4644(3) 0.8370(2) 0.2644(2) 0.0268(9) Uani 1 1 d . . . C75 C 0.4574(3) 0.9181(2) 0.2657(2) 0.0283(10) Uani 1 1 d . . . C76 C 0.4009(3) 0.9478(2) 0.1969(3) 0.0329(10) Uani 1 1 d . . . C77 C 0.3530(3) 0.8978(3) 0.1294(2) 0.0312(10) Uani 1 1 d . . . C78 C 0.3608(3) 0.8176(2) 0.1310(2) 0.0276(10) Uani 1 1 d . . . F79 F 0.52096(16) 0.81114(13) 0.33460(12) 0.0320(6) Uani 1 1 d . . . F80 F 0.50333(17) 0.96575(14) 0.33300(14) 0.0384(6) Uani 1 1 d . . . F81 F 0.39128(17) 1.02644(14) 0.19496(15) 0.0453(7) Uani 1 1 d . . . F82 F 0.29276(17) 0.92665(14) 0.06195(14) 0.0435(7) Uani 1 1 d . . . F83 F 0.30587(16) 0.77313(13) 0.06144(13) 0.0342(6) Uani 1 1 d . . . C84 C 0.5594(3) 0.6643(2) 0.2386(2) 0.0200(8) Uani 1 1 d . . . C85 C 0.5793(3) 0.5883(2) 0.2567(2) 0.0226(9) Uani 1 1 d . . . C86 C 0.6825(3) 0.5602(2) 0.2780(2) 0.0266(9) Uani 1 1 d . . . C87 C 0.7740(3) 0.6111(2) 0.2832(2) 0.0272(9) Uani 1 1 d . . . C88 C 0.7600(3) 0.6862(2) 0.2664(2) 0.0226(9) Uani 1 1 d . . . C89 C 0.6547(3) 0.7120(2) 0.2446(2) 0.0217(8) Uani 1 1 d . . . F90 F 0.49282(16) 0.53498(13) 0.25182(12) 0.0312(5) Uani 1 1 d . . . F91 F 0.69444(18) 0.48538(14) 0.29575(13) 0.0406(6) Uani 1 1 d . . . F92 F 0.87515(16) 0.58415(14) 0.30249(13) 0.0352(6) Uani 1 1 d . . . F93 F 0.84819(15) 0.73649(13) 0.27014(13) 0.0350(6) Uani 1 1 d . . . F94 F 0.64996(15) 0.78758(13) 0.22614(13) 0.0303(5) Uani 1 1 d . . . C95 C 0.3898(3) 0.6328(2) 0.1184(2) 0.0213(9) Uani 1 1 d . . . C96 C 0.3168(3) 0.5652(2) 0.0977(2) 0.0237(9) Uani 1 1 d . . . C97 C 0.3006(3) 0.5159(2) 0.0290(2) 0.0238(9) Uani 1 1 d . . . C98 C 0.3584(3) 0.5312(2) -0.0251(2) 0.0253(9) Uani 1 1 d . . . C99 C 0.4315(3) 0.5981(2) -0.0092(2) 0.0254(9) Uani 1 1 d . . . C100 C 0.4439(3) 0.6469(2) 0.0603(2) 0.0230(9) Uani 1 1 d . . . F101 F 0.25692(16) 0.54365(13) 0.14741(12) 0.0303(5) Uani 1 1 d . . . F102 F 0.22766(16) 0.45124(13) 0.01320(12) 0.0337(6) Uani 1 1 d . . . F103 F 0.34502(17) 0.48307(14) -0.09217(12) 0.0351(6) Uani 1 1 d . . . F104 F 0.48953(16) 0.61490(14) -0.06108(12) 0.0331(6) Uani 1 1 d . . . F105 F 0.51678(15) 0.71118(13) 0.07189(12) 0.0285(5) Uani 1 1 d . . . H106 H 1.169(3) 0.692(2) 0.847(2) 0.041(11) Uiso 1 1 d . . . H107 H 1.169(2) 0.9820(19) 0.5562(18) 0.009(9) Uiso 1 1 d . . . H108 H 1.266(2) 1.081(2) 0.6407(18) 0.011(9) Uiso 1 1 d . . . H109 H 1.297(3) 1.076(2) 0.781(2) 0.021(10) Uiso 1 1 d . . . H110 H 1.221(2) 0.927(2) 0.8795(18) 0.010(9) Uiso 1 1 d . . . H111 H 1.415(3) 0.959(3) 0.884(2) 0.053(14) Uiso 1 1 d . . . H112 H 1.384(3) 0.985(2) 0.962(2) 0.043(14) Uiso 1 1 d . . . H113 H 1.396(3) 1.046(2) 0.8939(19) 0.022(10) Uiso 1 1 d . . . H114 H 1.194(4) 1.031(3) 0.958(3) 0.062(16) Uiso 1 1 d . . . H115 H 1.207(3) 1.085(2) 0.888(2) 0.028(11) Uiso 1 1 d . . . H116 H 1.103(4) 1.026(3) 0.878(3) 0.065(15) Uiso 1 1 d . . . H117 H 1.027(2) 0.813(2) 0.5973(17) 0.012(9) Uiso 1 1 d . . . H118 H 0.943(4) 0.837(3) 0.464(3) 0.092(19) Uiso 1 1 d . . . H119 H 1.018(3) 0.910(2) 0.473(2) 0.031(11) Uiso 1 1 d . . . H120 H 0.939(4) 0.907(3) 0.535(3) 0.065(17) Uiso 1 1 d . . . H121 H 1.197(4) 0.837(3) 0.522(3) 0.077(18) Uiso 1 1 d . . . H122 H 1.094(4) 0.773(3) 0.488(3) 0.077(18) Uiso 1 1 d . . . H123 H 1.189(3) 0.768(3) 0.579(2) 0.044(13) Uiso 1 1 d . . . H124 H 1.430(4) 0.774(3) 0.886(2) 0.056(14) Uiso 1 1 d . . . H125 H 1.333(3) 0.736(3) 0.907(2) 0.032(12) Uiso 1 1 d . . . H126 H 1.348(3) 0.821(3) 0.909(2) 0.050(16) Uiso 1 1 d . . . H127 H 1.364(3) 0.890(3) 0.776(2) 0.041(12) Uiso 1 1 d . . . H128 H 1.320(3) 0.836(2) 0.688(2) 0.044(13) Uiso 1 1 d . . . H129 H 1.421(4) 0.815(3) 0.753(3) 0.097(19) Uiso 1 1 d . . . H130 H 1.255(3) 0.684(2) 0.688(2) 0.041(13) Uiso 1 1 d . . . H131 H 1.376(4) 0.677(3) 0.759(2) 0.060(14) Uiso 1 1 d . . . H132 H 1.270(4) 0.647(3) 0.777(3) 0.069(16) Uiso 1 1 d . . . H133 H 1.165(3) 0.588(2) 0.883(2) 0.037(12) Uiso 1 1 d . . . H134 H 1.130(3) 0.548(2) 0.7975(19) 0.012(10) Uiso 1 1 d . . . H135 H 1.087(3) 0.509(2) 0.8654(19) 0.021(10) Uiso 1 1 d . . . H136 H 0.914(3) 0.522(2) 0.715(2) 0.015(9) Uiso 1 1 d . . . H137 H 0.914(3) 0.496(2) 0.800(2) 0.037(12) Uiso 1 1 d . . . H138 H 0.826(3) 0.551(2) 0.7620(19) 0.029(10) Uiso 1 1 d . . . H139 H 0.958(3) 0.569(3) 0.925(2) 0.054(13) Uiso 1 1 d . . . H140 H 0.895(3) 0.647(2) 0.887(2) 0.039(11) Uiso 1 1 d . . . H141 H 1.027(3) 0.654(2) 0.9310(19) 0.015(9) Uiso 1 1 d . . . H142 H 0.758(3) 0.544(2) 0.504(2) 0.035(11) Uiso 1 1 d . . . H143 H 0.594(3) 0.543(2) 0.536(2) 0.038(12) Uiso 1 1 d . . . H144 H 0.579(3) 0.606(2) 0.650(2) 0.037(12) Uiso 1 1 d . . . H145 H 0.779(2) 0.720(2) 0.8027(18) 0.014(9) Uiso 1 1 d . . . H146 H 0.708(3) 0.591(3) 0.828(2) 0.062(14) Uiso 1 1 d . . . H147 H 0.594(4) 0.629(3) 0.793(3) 0.067(18) Uiso 1 1 d . . . H148 H 0.663(3) 0.669(2) 0.866(2) 0.035(12) Uiso 1 1 d . . . H149 H 0.563(3) 0.746(2) 0.7091(19) 0.019(9) Uiso 1 1 d . . . H150 H 0.625(3) 0.792(2) 0.798(2) 0.032(11) Uiso 1 1 d . . . H151 H 0.675(3) 0.811(2) 0.725(2) 0.039(12) Uiso 1 1 d . . . H152 H 0.983(2) 0.679(2) 0.5994(18) 0.013(9) Uiso 1 1 d . . . H153 H 1.047(2) 0.5711(19) 0.6624(19) 0.010(9) Uiso 1 1 d . . . H154 H 1.089(3) 0.579(3) 0.583(2) 0.054(13) Uiso 1 1 d . . . H155 H 0.985(3) 0.512(3) 0.585(2) 0.039(12) Uiso 1 1 d . . . H156 H 0.993(3) 0.648(2) 0.473(2) 0.033(11) Uiso 1 1 d . . . H157 H 0.890(3) 0.584(3) 0.461(2) 0.043(14) Uiso 1 1 d . . . H158 H 0.864(3) 0.672(3) 0.465(2) 0.047(13) Uiso 1 1 d . . . H159 H 0.595(3) 0.931(2) 0.493(2) 0.029(11) Uiso 1 1 d . . . H160 H 0.642(3) 1.071(2) 0.5149(19) 0.023(10) Uiso 1 1 d . . . H161 H 0.786(3) 1.115(2) 0.6273(19) 0.016(10) Uiso 1 1 d . . . H162 H 0.971(2) 1.008(2) 0.7519(17) 0.011(9) Uiso 1 1 d . . . H163 H 0.838(3) 1.115(2) 0.7847(18) 0.012(9) Uiso 1 1 d . . . H164 H 0.939(4) 1.097(3) 0.853(3) 0.081(18) Uiso 1 1 d . . . H165 H 0.828(3) 1.033(3) 0.821(2) 0.058(14) Uiso 1 1 d . . . H166 H 0.959(4) 1.162(3) 0.702(3) 0.066(15) Uiso 1 1 d . . . H167 H 1.020(3) 1.095(2) 0.670(2) 0.022(10) Uiso 1 1 d . . . H168 H 1.069(4) 1.132(3) 0.767(3) 0.065(15) Uiso 1 1 d . . . H169 H 0.703(2) 0.788(2) 0.6072(18) 0.011(9) Uiso 1 1 d . . . H170 H 0.519(3) 0.821(2) 0.583(2) 0.034(12) Uiso 1 1 d . . . H171 H 0.524(3) 0.741(3) 0.538(2) 0.043(13) Uiso 1 1 d . . . H172 H 0.516(3) 0.814(2) 0.491(2) 0.027(10) Uiso 1 1 d . . . H173 H 0.695(3) 0.805(2) 0.448(2) 0.028(11) Uiso 1 1 d . . . H174 H 0.689(3) 0.717(3) 0.483(2) 0.058(14) Uiso 1 1 d . . . H175 H 0.798(3) 0.783(2) 0.511(2) 0.036(11) Uiso 1 1 d . . . H176 H 0.982(3) 0.918(2) 0.870(2) 0.034(13) Uiso 1 1 d . . . H177 H 0.800(4) 0.897(3) 0.843(3) 0.074(16) Uiso 1 1 d . . . H178 H 0.724(3) 0.816(3) 0.936(2) 0.056(13) Uiso 1 1 d . . . H179 H 1.057(3) 0.773(2) 1.046(2) 0.039(11) Uiso 1 1 d . . . H180 H 1.112(3) 0.857(2) 0.954(2) 0.045(12) Uiso 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 Ti1 0.0145(3) 0.0148(4) 0.0238(4) -0.0002(3) 0.0052(3) 0.0026(3) N2 0.0134(13) 0.0182(19) 0.0278(17) 0.0016(14) 0.0053(13) 0.0026(12) C3 0.0134(16) 0.018(2) 0.032(2) -0.0014(17) 0.0061(16) 0.0037(15) C4 0.0217(18) 0.017(2) 0.025(2) 0.0007(17) 0.0022(17) 0.0025(16) C5 0.0231(17) 0.013(2) 0.019(2) -0.0017(15) 0.0102(16) 0.0055(15) N6 0.0168(14) 0.0138(18) 0.0209(17) 0.0004(13) 0.0043(13) 0.0023(12) C7 0.0133(16) 0.017(2) 0.038(2) 0.0057(18) 0.0100(17) 0.0073(15) C8 0.0217(18) 0.017(2) 0.048(3) 0.0055(19) 0.0179(19) 0.0066(16) C9 0.027(2) 0.032(3) 0.040(3) 0.008(2) 0.012(2) 0.0067(19) C10 0.023(2) 0.026(3) 0.059(3) 0.017(2) 0.016(2) 0.0005(18) C11 0.023(2) 0.020(3) 0.050(3) 0.002(2) 0.010(2) 0.0008(18) C12 0.0111(16) 0.018(2) 0.053(3) 0.007(2) 0.0101(18) 0.0033(15) C13 0.0222(19) 0.018(3) 0.048(3) 0.001(2) 0.009(2) -0.0018(17) C14 0.022(2) 0.043(3) 0.048(3) 0.001(3) 0.001(2) -0.006(2) C15 0.033(2) 0.030(3) 0.054(4) 0.000(3) 0.012(3) 0.003(2) C16 0.035(2) 0.026(3) 0.038(3) 0.003(2) 0.017(2) -0.0016(19) C17 0.054(3) 0.040(4) 0.033(3) 0.008(2) 0.016(3) -0.010(3) C18 0.061(3) 0.048(4) 0.055(4) -0.007(3) 0.022(3) 0.007(3) C19 0.0153(17) 0.021(3) 0.060(3) 0.003(2) 0.009(2) 0.0068(16) C20 0.021(2) 0.032(3) 0.069(4) 0.012(3) -0.002(2) 0.004(2) C21 0.017(2) 0.026(3) 0.076(4) 0.006(3) 0.018(2) 0.0062(18) C22 0.025(2) 0.027(3) 0.078(4) 0.001(3) 0.020(3) 0.0086(19) C23 0.0243(18) 0.019(2) 0.027(2) 0.0056(17) 0.0073(17) 0.0048(16) C24 0.027(2) 0.024(3) 0.039(3) 0.010(2) 0.005(2) 0.0036(19) C25 0.028(2) 0.020(3) 0.034(3) 0.010(2) 0.012(2) -0.0015(18) C26 0.042(3) 0.033(3) 0.028(3) 0.006(2) 0.012(2) 0.007(2) C27 0.0165(16) 0.016(2) 0.025(2) 0.0045(16) 0.0018(16) 0.0026(15) C28 0.0230(18) 0.016(2) 0.027(2) 0.0011(17) 0.0042(17) 0.0053(16) C29 0.031(2) 0.026(3) 0.035(3) -0.006(2) 0.000(2) 0.0059(18) C30 0.025(2) 0.027(3) 0.046(3) -0.011(2) -0.006(2) -0.0040(19) C31 0.0158(19) 0.027(3) 0.057(3) 0.000(2) 0.010(2) -0.0006(17) C32 0.0181(17) 0.014(2) 0.034(2) 0.0062(17) 0.0088(17) 0.0027(15) C33 0.0218(19) 0.024(3) 0.033(2) 0.0046(19) 0.0124(19) 0.0033(17) C34 0.039(3) 0.039(3) 0.047(3) 0.009(3) 0.023(3) 0.008(2) C35 0.027(2) 0.033(3) 0.036(3) 0.001(2) 0.014(2) 0.0104(19) C36 0.034(2) 0.015(2) 0.029(2) -0.0004(19) 0.0118(19) 0.0016(18) C37 0.031(2) 0.038(3) 0.029(3) 0.002(2) 0.012(2) 0.014(2) C38 0.047(3) 0.045(4) 0.040(3) 0.003(3) 0.021(3) 0.018(3) N39 0.0164(14) 0.0143(18) 0.0256(17) -0.0005(13) 0.0088(13) 0.0013(12) C40 0.0195(17) 0.021(2) 0.025(2) 0.0073(17) 0.0094(16) 0.0058(15) C41 0.0188(17) 0.027(3) 0.027(2) 0.0056(18) 0.0087(17) 0.0038(16) C42 0.027(2) 0.032(3) 0.033(3) 0.008(2) 0.004(2) 0.0076(19) C43 0.034(2) 0.024(3) 0.042(3) 0.015(2) 0.010(2) 0.0126(19) C44 0.032(2) 0.018(3) 0.044(3) 0.008(2) 0.012(2) 0.0064(19) C45 0.0217(18) 0.022(2) 0.030(2) 0.0076(18) 0.0134(17) 0.0055(16) C46 0.0262(19) 0.017(2) 0.037(2) 0.0046(19) 0.0186(19) 0.0049(17) C47 0.035(3) 0.046(4) 0.046(3) -0.012(3) 0.013(3) 0.002(2) C48 0.031(2) 0.030(3) 0.057(3) 0.014(3) 0.014(2) 0.000(2) C49 0.0246(19) 0.023(3) 0.028(2) 0.0054(19) 0.0002(19) 0.0054(17) C50 0.027(2) 0.034(3) 0.032(3) 0.004(2) 0.001(2) -0.001(2) C51 0.028(2) 0.036(3) 0.040(3) 0.002(2) 0.008(2) 0.008(2) C52 0.032(2) 0.032(3) 0.035(3) 0.014(2) 0.014(2) -0.002(2) C53 0.042(2) 0.054(4) 0.025(2) -0.008(2) 0.005(2) 0.019(2) C54 0.032(2) 0.046(3) 0.035(3) -0.007(2) 0.009(2) 0.006(2) C55 0.036(2) 0.036(3) 0.030(2) -0.006(2) 0.010(2) -0.001(2) C56 0.032(2) 0.032(3) 0.029(2) -0.005(2) 0.007(2) 0.0034(19) C57 0.024(2) 0.026(3) 0.033(2) -0.0045(19) 0.0128(19) -0.0051(18) N58 0.0316(18) 0.053(3) 0.042(2) 0.008(2) 0.0147(18) -0.0010(18) C59 0.034(2) 0.056(4) 0.065(3) 0.000(3) 0.022(2) -0.006(2) C60 0.049(3) 0.054(4) 0.054(3) 0.013(3) 0.015(2) 0.008(3) B61 0.0177(19) 0.026(3) 0.029(3) -0.002(2) 0.0089(19) -0.0013(18) C62 0.0230(19) 0.017(2) 0.048(3) -0.0034(19) 0.0147(19) -0.0065(16) C63 0.033(2) 0.033(3) 0.032(2) 0.004(2) 0.007(2) 0.0027(19) C64 0.0199(19) 0.024(3) 0.060(3) 0.000(2) 0.018(2) -0.0008(17) C65 0.045(2) 0.026(3) 0.039(3) -0.002(2) 0.030(2) -0.001(2) C66 0.041(2) 0.020(3) 0.034(3) 0.0023(19) 0.002(2) -0.0071(19) C67 0.036(2) 0.024(3) 0.026(2) 0.0011(18) 0.0184(19) -0.0007(18) F68 0.0189(10) 0.0343(16) 0.0621(16) 0.0045(12) 0.0173(11) 0.0044(10) F69 0.0339(13) 0.0450(19) 0.087(2) 0.0077(15) 0.0311(14) 0.0073(12) F70 0.0568(16) 0.050(2) 0.0645(17) 0.0005(14) 0.0409(14) 0.0024(14) F71 0.0599(15) 0.0426(18) 0.0354(14) -0.0020(12) 0.0224(13) -0.0078(13) F72 0.0339(12) 0.0440(18) 0.0347(14) 0.0024(12) 0.0124(11) -0.0028(11) C73 0.0144(16) 0.021(2) 0.031(2) 0.0028(18) 0.0109(17) 0.0008(15) C74 0.0182(17) 0.026(3) 0.038(2) 0.000(2) 0.0112(18) 0.0011(17) C75 0.0168(17) 0.026(3) 0.042(3) -0.002(2) 0.0093(18) 0.0022(17) C76 0.0244(19) 0.013(2) 0.061(3) 0.001(2) 0.013(2) 0.0014(17) C77 0.0206(18) 0.034(3) 0.040(3) 0.011(2) 0.0060(19) 0.0103(18) C78 0.0149(17) 0.028(3) 0.038(2) -0.003(2) 0.0054(18) 0.0020(16) F79 0.0346(12) 0.0252(15) 0.0343(13) 0.0006(11) 0.0071(11) 0.0025(10) F80 0.0329(12) 0.0254(15) 0.0529(16) -0.0099(12) 0.0092(12) 0.0022(11) F81 0.0361(13) 0.0217(16) 0.0759(18) 0.0063(13) 0.0106(13) 0.0076(11) F82 0.0370(13) 0.0355(17) 0.0541(16) 0.0135(13) 0.0027(12) 0.0107(11) F83 0.0294(11) 0.0307(15) 0.0388(14) 0.0020(11) 0.0033(11) 0.0070(10) C84 0.0240(18) 0.019(2) 0.019(2) 0.0002(16) 0.0087(16) 0.0005(16) C85 0.0241(18) 0.020(2) 0.022(2) -0.0016(17) 0.0066(17) -0.0051(16) C86 0.036(2) 0.017(2) 0.027(2) 0.0036(18) 0.0071(18) 0.0088(18) C87 0.0252(19) 0.031(3) 0.025(2) -0.0007(19) 0.0050(18) 0.0089(18) C88 0.0217(18) 0.022(2) 0.025(2) 0.0017(17) 0.0089(17) -0.0002(16) C89 0.0271(19) 0.016(2) 0.025(2) 0.0051(17) 0.0125(17) 0.0028(16) F90 0.0316(11) 0.0213(14) 0.0397(13) 0.0036(11) 0.0099(10) -0.0047(10) F91 0.0471(14) 0.0222(15) 0.0512(15) 0.0049(12) 0.0096(12) 0.0102(11) F92 0.0272(11) 0.0356(16) 0.0420(14) 0.0022(11) 0.0063(11) 0.0136(10) F93 0.0193(10) 0.0302(16) 0.0565(15) 0.0051(12) 0.0127(11) -0.0010(10) F94 0.0236(10) 0.0171(14) 0.0522(14) 0.0098(11) 0.0126(10) 0.0007(9) C95 0.0167(17) 0.021(2) 0.026(2) 0.0008(17) 0.0057(16) 0.0044(15) C96 0.0196(18) 0.024(3) 0.028(2) 0.0067(18) 0.0076(17) 0.0026(16) C97 0.0190(17) 0.019(2) 0.030(2) 0.0036(18) 0.0015(17) 0.0009(16) C98 0.0260(19) 0.027(3) 0.022(2) 0.0012(18) 0.0022(18) 0.0127(17) C99 0.0170(17) 0.035(3) 0.030(2) 0.013(2) 0.0111(18) 0.0093(17) C100 0.0185(17) 0.022(2) 0.030(2) 0.0049(18) 0.0081(17) 0.0062(16) F101 0.0281(11) 0.0246(14) 0.0408(13) -0.0002(11) 0.0167(11) -0.0072(10) F102 0.0332(12) 0.0260(15) 0.0374(13) -0.0035(11) 0.0058(11) -0.0045(10) F103 0.0370(12) 0.0394(17) 0.0264(13) -0.0025(11) 0.0045(11) 0.0109(11) F104 0.0313(11) 0.0415(17) 0.0340(13) 0.0088(11) 0.0187(11) 0.0097(11) F105 0.0235(10) 0.0274(15) 0.0372(13) 0.0038(11) 0.0137(10) -0.0028(9) _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 N39 1.719(3) . ? Ti1 N6 1.984(3) . ? Ti1 N2 2.060(3) . ? Ti1 C52 2.337(5) . ? Ti1 C5 2.642(4) . ? N2 C3 1.329(4) . ? N2 C7 1.446(4) . ? C3 C4 1.443(5) . ? C3 C19 1.566(4) . ? C4 C5 1.397(5) . ? C4 H106 1.01(4) . ? C5 N6 1.371(4) . ? C5 C23 1.570(5) . ? N6 C27 1.437(4) . ? C7 C8 1.395(5) . ? C7 C12 1.404(5) . ? C8 C9 1.405(5) . ? C8 C16 1.520(5) . ? C9 C10 1.378(6) . ? C9 H107 0.92(3) . ? C10 C11 1.359(6) . ? C10 H108 0.91(3) . ? C11 C12 1.380(5) . ? C11 H109 0.91(3) . ? C12 C13 1.526(6) . ? C13 C15 1.532(6) . ? C13 C14 1.534(5) . ? C13 H110 0.90(3) . ? C14 H111 0.98(4) . ? C14 H112 0.93(4) . ? C14 H113 1.05(4) . ? C15 H114 0.94(4) . ? C15 H115 0.97(4) . ? C15 H116 0.96(4) . ? C16 C17 1.521(6) . ? C16 C18 1.527(6) . ? C16 H117 0.98(3) . ? C17 H118 1.04(6) . ? C17 H119 0.95(4) . ? C17 H120 0.93(5) . ? C18 H121 0.99(5) . ? C18 H122 0.99(5) . ? C18 H123 1.02(4) . ? C19 C20 1.525(6) . ? C19 C21 1.536(6) . ? C19 C22 1.550(6) . ? C20 H124 0.95(4) . ? C20 H125 0.97(4) . ? C20 H126 0.92(5) . ? C21 H127 1.06(4) . ? C21 H128 1.01(4) . ? C21 H129 0.92(5) . ? C22 H130 1.02(4) . ? C22 H131 0.99(4) . ? C22 H132 1.02(5) . ? C23 C25 1.531(5) . ? C23 C26 1.538(5) . ? C23 C24 1.540(5) . ? C24 H133 0.97(4) . ? C24 H134 0.90(3) . ? C24 H135 1.01(4) . ? C25 H136 0.93(3) . ? C25 H137 0.88(4) . ? C25 H138 1.10(3) . ? C26 H139 1.04(4) . ? C26 H140 1.03(4) . ? C26 H141 0.96(3) . ? C27 C28 1.408(5) . ? C27 C32 1.415(4) . ? C28 C29 1.378(5) . ? C28 C36 1.523(5) . ? C29 C30 1.383(6) . ? C29 H142 1.01(4) . ? C30 C31 1.358(6) . ? C30 H143 0.89(4) . ? C31 C32 1.390(5) . ? C31 H144 0.84(4) . ? C32 C33 1.517(5) . ? C33 C34 1.515(6) . ? C33 C35 1.534(5) . ? C33 H145 0.95(3) . ? C34 H146 1.08(5) . ? C34 H147 0.83(4) . ? C34 H148 1.00(4) . ? C35 H149 1.02(3) . ? C35 H150 0.98(4) . ? C35 H151 1.05(4) . ? C36 C38 1.527(6) . ? C36 C37 1.535(5) . ? C36 H152 0.88(3) . ? C37 H153 0.96(3) . ? C37 H154 1.00(4) . ? C37 H155 1.09(4) . ? C38 H156 0.98(4) . ? C38 H157 0.95(4) . ? C38 H158 1.03(4) . ? N39 C40 1.410(4) . ? C40 C45 1.411(5) . ? C40 C41 1.422(5) . ? C41 C42 1.393(5) . ? C41 C49 1.507(5) . ? C42 C43 1.380(6) . ? C42 H159 0.93(3) . ? C43 C44 1.380(6) . ? C43 H160 0.99(3) . ? C44 C45 1.388(5) . ? C44 H161 0.91(3) . ? C45 C46 1.503(5) . ? C46 C48 1.514(6) . ? C46 C47 1.539(6) . ? C46 H162 0.93(3) . ? C47 H163 0.93(3) . ? C47 H164 0.96(5) . ? C47 H165 1.03(5) . ? C48 H166 1.00(5) . ? C48 H167 1.00(3) . ? C48 H168 1.07(4) . ? C49 C51 1.505(6) . ? C49 C50 1.532(5) . ? C49 H169 0.89(3) . ? C50 H170 1.00(4) . ? C50 H171 0.94(4) . ? C50 H172 0.97(3) . ? C51 H173 0.98(3) . ? C51 H174 1.09(5) . ? C51 H175 0.94(4) . ? C52 C53 1.392(6) . ? C52 C57 1.411(5) . ? C52 H176 0.80(4) . ? C53 C54 1.398(6) . ? C53 H177 1.02(4) . ? C54 C55 1.406(6) . ? C54 H178 1.14(4) . ? C55 N58 1.358(5) . ? C55 C56 1.404(5) . ? C56 C57 1.373(6) . ? C56 H179 1.03(3) . ? C57 H180 0.92(4) . ? N58 C59 1.456(5) . ? N58 C60 1.483(5) . ? C59 H183 0.9800 . ? C59 H182 0.9800 . ? C59 H181 0.9800 . ? C60 H186 0.9800 . ? C60 H184 0.9800 . ? C60 H185 0.9800 . ? B61 C73 1.643(6) . ? B61 C84 1.660(5) . ? B61 C95 1.664(6) . ? B61 C62 1.670(6) . ? C62 C63 1.373(5) . ? C62 C67 1.396(5) . ? C63 F68 1.369(4) . ? C63 C64 1.407(5) . ? C64 F69 1.336(4) . ? C64 C65 1.351(5) . ? C65 C66 1.342(5) . ? C65 F70 1.369(4) . ? C66 F71 1.334(4) . ? C66 C67 1.410(5) . ? C67 F72 1.325(4) . ? C73 C78 1.388(5) . ? C73 C74 1.396(5) . ? C74 F79 1.352(4) . ? C74 C75 1.392(5) . ? C75 F80 1.338(4) . ? C75 C76 1.362(5) . ? C76 F81 1.358(4) . ? C76 C77 1.366(6) . ? C77 F82 1.355(4) . ? C77 C78 1.380(5) . ? C78 F83 1.362(4) . ? C84 C85 1.380(5) . ? C84 C89 1.386(5) . ? C85 F90 1.357(4) . ? C85 C86 1.381(5) . ? C86 F91 1.344(4) . ? C86 C87 1.380(5) . ? C87 C88 1.348(5) . ? C87 F92 1.349(4) . ? C88 F93 1.347(4) . ? C88 C89 1.388(5) . ? C89 F94 1.352(4) . ? C95 C96 1.390(5) . ? C95 C100 1.394(5) . ? C96 F101 1.352(4) . ? C96 C97 1.368(5) . ? C97 F102 1.353(4) . ? C97 C98 1.370(5) . ? C98 F103 1.340(4) . ? C98 C99 1.384(5) . ? C99 F104 1.346(4) . ? C99 C100 1.382(5) . ? C100 F105 1.353(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N39 Ti1 N6 111.57(13) . . ? N39 Ti1 N2 107.56(12) . . ? N6 Ti1 N2 99.52(12) . . ? N39 Ti1 C52 103.28(15) . . ? N6 Ti1 C52 126.02(14) . . ? N2 Ti1 C52 107.82(13) . . ? N39 Ti1 C5 141.70(13) . . ? N6 Ti1 C5 30.45(10) . . ? N2 Ti1 C5 83.73(11) . . ? C52 Ti1 C5 107.80(13) . . ? C3 N2 C7 125.1(3) . . ? C3 N2 Ti1 106.7(2) . . ? C7 N2 Ti1 127.4(2) . . ? N2 C3 C4 119.7(3) . . ? N2 C3 C19 127.6(3) . . ? C4 C3 C19 112.6(3) . . ? C5 C4 C3 134.7(3) . . ? C5 C4 H106 114(2) . . ? C3 C4 H106 110(2) . . ? N6 C5 C4 119.3(3) . . ? N6 C5 C23 124.9(3) . . ? C4 C5 C23 115.5(3) . . ? N6 C5 Ti1 47.20(17) . . ? C4 C5 Ti1 78.8(2) . . ? C23 C5 Ti1 148.0(2) . . ? C5 N6 C27 123.6(3) . . ? C5 N6 Ti1 102.3(2) . . ? C27 N6 Ti1 132.9(2) . . ? C8 C7 C12 121.4(4) . . ? C8 C7 N2 117.8(3) . . ? C12 C7 N2 120.7(3) . . ? C7 C8 C9 117.6(4) . . ? C7 C8 C16 124.5(4) . . ? C9 C8 C16 117.8(4) . . ? C10 C9 C8 121.1(4) . . ? C10 C9 H107 122(2) . . ? C8 C9 H107 117(2) . . ? C11 C10 C9 119.6(4) . . ? C11 C10 H108 128(2) . . ? C9 C10 H108 113(2) . . ? C10 C11 C12 122.4(4) . . ? C10 C11 H109 120(2) . . ? C12 C11 H109 117(2) . . ? C11 C12 C7 117.8(4) . . ? C11 C12 C13 116.7(4) . . ? C7 C12 C13 125.5(4) . . ? C12 C13 C15 111.7(4) . . ? C12 C13 C14 112.8(4) . . ? C15 C13 C14 107.8(4) . . ? C12 C13 H110 110(2) . . ? C15 C13 H110 105(2) . . ? C14 C13 H110 109.1(19) . . ? C13 C14 H111 114(3) . . ? C13 C14 H112 111(3) . . ? H111 C14 H112 108(3) . . ? C13 C14 H113 110.8(18) . . ? H111 C14 H113 97(3) . . ? H112 C14 H113 115(3) . . ? C13 C15 H114 112(3) . . ? C13 C15 H115 106(2) . . ? H114 C15 H115 113(4) . . ? C13 C15 H116 112(3) . . ? H114 C15 H116 106(4) . . ? H115 C15 H116 107(3) . . ? C8 C16 C17 111.7(4) . . ? C8 C16 C18 111.5(4) . . ? C17 C16 C18 110.6(4) . . ? C8 C16 H117 109.5(18) . . ? C17 C16 H117 107.4(17) . . ? C18 C16 H117 106(2) . . ? C16 C17 H118 107(3) . . ? C16 C17 H119 110(2) . . ? H118 C17 H119 97(3) . . ? C16 C17 H120 101(3) . . ? H118 C17 H120 115(4) . . ? H119 C17 H120 127(4) . . ? C16 C18 H121 110(3) . . ? C16 C18 H122 105(3) . . ? H121 C18 H122 107(4) . . ? C16 C18 H123 112(2) . . ? H121 C18 H123 107(4) . . ? H122 C18 H123 116(4) . . ? C20 C19 C21 108.9(4) . . ? C20 C19 C22 109.2(4) . . ? C21 C19 C22 106.6(4) . . ? C20 C19 C3 109.3(4) . . ? C21 C19 C3 116.3(3) . . ? C22 C19 C3 106.3(3) . . ? C19 C20 H124 112(3) . . ? C19 C20 H125 117(2) . . ? H124 C20 H125 103(3) . . ? C19 C20 H126 118(3) . . ? H124 C20 H126 105(4) . . ? H125 C20 H126 100(4) . . ? C19 C21 H127 114(2) . . ? C19 C21 H128 117(2) . . ? H127 C21 H128 106(3) . . ? C19 C21 H129 107(3) . . ? H127 C21 H129 107(4) . . ? H128 C21 H129 105(4) . . ? C19 C22 H130 111(2) . . ? C19 C22 H131 110(3) . . ? H130 C22 H131 114(3) . . ? C19 C22 H132 112(3) . . ? H130 C22 H132 111(3) . . ? H131 C22 H132 98(3) . . ? C25 C23 C26 108.2(3) . . ? C25 C23 C24 106.0(3) . . ? C26 C23 C24 107.7(3) . . ? C25 C23 C5 115.9(3) . . ? C26 C23 C5 106.7(3) . . ? C24 C23 C5 112.0(3) . . ? C23 C24 H133 114(2) . . ? C23 C24 H134 110(2) . . ? H133 C24 H134 110(3) . . ? C23 C24 H135 103.6(18) . . ? H133 C24 H135 106(3) . . ? H134 C24 H135 113(3) . . ? C23 C25 H136 116(2) . . ? C23 C25 H137 102(3) . . ? H136 C25 H137 120(3) . . ? C23 C25 H138 111.0(19) . . ? H136 C25 H138 106(3) . . ? H137 C25 H138 101(3) . . ? C23 C26 H139 109(2) . . ? C23 C26 H140 113(2) . . ? H139 C26 H140 109(3) . . ? C23 C26 H141 107(2) . . ? H139 C26 H141 109(3) . . ? H140 C26 H141 109(3) . . ? C28 C27 C32 120.9(3) . . ? C28 C27 N6 119.1(3) . . ? C32 C27 N6 120.0(3) . . ? C29 C28 C27 118.5(3) . . ? C29 C28 C36 119.9(4) . . ? C27 C28 C36 121.6(3) . . ? C28 C29 C30 120.6(4) . . ? C28 C29 H142 120(2) . . ? C30 C29 H142 120(2) . . ? C31 C30 C29 120.7(4) . . ? C31 C30 H143 122(3) . . ? C29 C30 H143 117(3) . . ? C30 C31 C32 121.6(4) . . ? C30 C31 H144 120(3) . . ? C32 C31 H144 119(3) . . ? C31 C32 C27 117.4(4) . . ? C31 C32 C33 118.9(3) . . ? C27 C32 C33 123.6(3) . . ? C34 C33 C32 111.3(4) . . ? C34 C33 C35 109.6(3) . . ? C32 C33 C35 112.0(3) . . ? C34 C33 H145 106.3(19) . . ? C32 C33 H145 110.0(19) . . ? C35 C33 H145 107(2) . . ? C33 C34 H146 114(2) . . ? C33 C34 H147 113(3) . . ? H146 C34 H147 114(4) . . ? C33 C34 H148 108(2) . . ? H146 C34 H148 105(3) . . ? H147 C34 H148 102(4) . . ? C33 C35 H149 109(2) . . ? C33 C35 H150 111(2) . . ? H149 C35 H150 111(3) . . ? C33 C35 H151 110(2) . . ? H149 C35 H151 111(3) . . ? H150 C35 H151 105(3) . . ? C28 C36 C38 112.6(3) . . ? C28 C36 C37 112.9(3) . . ? C38 C36 C37 108.3(4) . . ? C28 C36 H152 110(2) . . ? C38 C36 H152 107(2) . . ? C37 C36 H152 105(2) . . ? C36 C37 H153 111.8(19) . . ? C36 C37 H154 109(2) . . ? H153 C37 H154 113(3) . . ? C36 C37 H155 111.8(19) . . ? H153 C37 H155 103(3) . . ? H154 C37 H155 109(3) . . ? C36 C38 H156 110(2) . . ? C36 C38 H157 108(3) . . ? H156 C38 H157 112(3) . . ? C36 C38 H158 110(2) . . ? H156 C38 H158 113(3) . . ? H157 C38 H158 103(3) . . ? C40 N39 Ti1 174.3(3) . . ? N39 C40 C45 119.7(3) . . ? N39 C40 C41 120.1(3) . . ? C45 C40 C41 120.2(3) . . ? C42 C41 C40 117.8(4) . . ? C42 C41 C49 119.1(3) . . ? C40 C41 C49 123.0(3) . . ? C43 C42 C41 122.2(4) . . ? C43 C42 H159 123(2) . . ? C41 C42 H159 115(2) . . ? C44 C43 C42 119.2(4) . . ? C44 C43 H160 118(2) . . ? C42 C43 H160 122(2) . . ? C43 C44 C45 121.7(4) . . ? C43 C44 H161 120(2) . . ? C45 C44 H161 118(2) . . ? C44 C45 C40 118.8(4) . . ? C44 C45 C46 118.7(4) . . ? C40 C45 C46 122.4(3) . . ? C45 C46 C48 115.0(3) . . ? C45 C46 C47 110.6(3) . . ? C48 C46 C47 109.8(4) . . ? C45 C46 H162 107(2) . . ? C48 C46 H162 105(2) . . ? C47 C46 H162 108.8(19) . . ? C46 C47 H163 100(2) . . ? C46 C47 H164 112(3) . . ? H163 C47 H164 110(4) . . ? C46 C47 H165 114(3) . . ? H163 C47 H165 107(3) . . ? H164 C47 H165 112(4) . . ? C46 C48 H166 116(3) . . ? C46 C48 H167 108(2) . . ? H166 C48 H167 104(3) . . ? C46 C48 H168 113(2) . . ? H166 C48 H168 107(4) . . ? H167 C48 H168 109(3) . . ? C51 C49 C41 111.6(4) . . ? C51 C49 C50 110.5(4) . . ? C41 C49 C50 112.3(3) . . ? C51 C49 H169 109(2) . . ? C41 C49 H169 108(2) . . ? C50 C49 H169 105(2) . . ? C49 C50 H170 112(2) . . ? C49 C50 H171 116(2) . . ? H170 C50 H171 105(3) . . ? C49 C50 H172 110(2) . . ? H170 C50 H172 108(3) . . ? H171 C50 H172 106(3) . . ? C49 C51 H173 113(2) . . ? C49 C51 H174 108(2) . . ? H173 C51 H174 108(3) . . ? C49 C51 H175 113(2) . . ? H173 C51 H175 106(3) . . ? H174 C51 H175 109(3) . . ? C53 C52 C57 117.6(4) . . ? C53 C52 Ti1 102.6(3) . . ? C57 C52 Ti1 110.6(3) . . ? C53 C52 H176 117(3) . . ? C57 C52 H176 121(3) . . ? Ti1 C52 H176 78(3) . . ? C52 C53 C54 120.7(4) . . ? C52 C53 H177 115(3) . . ? C54 C53 H177 123(3) . . ? C53 C54 C55 120.9(4) . . ? C53 C54 H178 122(2) . . ? C55 C54 H178 117(2) . . ? N58 C55 C56 121.2(4) . . ? N58 C55 C54 121.3(4) . . ? C56 C55 C54 117.5(4) . . ? C57 C56 C55 121.3(4) . . ? C57 C56 H179 123(2) . . ? C55 C56 H179 116(2) . . ? C56 C57 C52 121.3(4) . . ? C56 C57 H180 122(3) . . ? C52 C57 H180 117(3) . . ? C55 N58 C59 122.9(4) . . ? C55 N58 C60 120.5(3) . . ? C59 N58 C60 116.6(4) . . ? N58 C59 H183 109.5 . . ? N58 C59 H182 109.5 . . ? H183 C59 H182 109.5 . . ? N58 C59 H181 109.5 . . ? H183 C59 H181 109.5 . . ? H182 C59 H181 109.5 . . ? N58 C60 H186 109.5 . . ? N58 C60 H184 109.5 . . ? H186 C60 H184 109.5 . . ? N58 C60 H185 109.5 . . ? H186 C60 H185 109.5 . . ? H184 C60 H185 109.5 . . ? C73 B61 C84 114.2(3) . . ? C73 B61 C95 113.5(3) . . ? C84 B61 C95 99.8(3) . . ? C73 B61 C62 103.3(3) . . ? C84 B61 C62 111.4(3) . . ? C95 B61 C62 115.1(3) . . ? C63 C62 C67 114.2(4) . . ? C63 C62 B61 119.0(4) . . ? C67 C62 B61 126.6(3) . . ? F68 C63 C62 119.0(4) . . ? F68 C63 C64 116.5(3) . . ? C62 C63 C64 124.5(4) . . ? F69 C64 C65 123.0(4) . . ? F69 C64 C63 119.4(4) . . ? C65 C64 C63 117.6(3) . . ? C66 C65 C64 122.1(4) . . ? C66 C65 F70 119.5(4) . . ? C64 C65 F70 118.3(4) . . ? F71 C66 C65 121.2(4) . . ? F71 C66 C67 119.8(4) . . ? C65 C66 C67 118.9(4) . . ? F72 C67 C62 122.7(3) . . ? F72 C67 C66 114.7(3) . . ? C62 C67 C66 122.6(4) . . ? C78 C73 C74 112.4(4) . . ? C78 C73 B61 127.6(3) . . ? C74 C73 B61 119.9(3) . . ? F79 C74 C75 115.5(3) . . ? F79 C74 C73 119.1(4) . . ? C75 C74 C73 125.3(4) . . ? F80 C75 C76 120.7(4) . . ? F80 C75 C74 121.0(3) . . ? C76 C75 C74 118.3(4) . . ? F81 C76 C75 120.7(4) . . ? F81 C76 C77 119.7(4) . . ? C75 C76 C77 119.7(4) . . ? F82 C77 C76 119.8(4) . . ? F82 C77 C78 119.9(4) . . ? C76 C77 C78 120.2(4) . . ? F83 C78 C77 115.2(3) . . ? F83 C78 C73 120.7(4) . . ? C77 C78 C73 124.1(4) . . ? C85 C84 C89 113.3(3) . . ? C85 C84 B61 119.6(3) . . ? C89 C84 B61 126.9(3) . . ? F90 C85 C84 119.3(3) . . ? F90 C85 C86 115.9(3) . . ? C84 C85 C86 124.8(3) . . ? F91 C86 C87 120.3(3) . . ? F91 C86 C85 120.8(3) . . ? C87 C86 C85 118.9(4) . . ? C88 C87 F92 121.3(3) . . ? C88 C87 C86 119.2(3) . . ? F92 C87 C86 119.5(4) . . ? F93 C88 C87 120.0(3) . . ? F93 C88 C89 119.7(3) . . ? C87 C88 C89 120.2(3) . . ? F94 C89 C84 121.1(3) . . ? F94 C89 C88 115.3(3) . . ? C84 C89 C88 123.6(3) . . ? C96 C95 C100 112.8(3) . . ? C96 C95 B61 127.8(3) . . ? C100 C95 B61 118.7(3) . . ? F101 C96 C97 115.4(3) . . ? F101 C96 C95 120.1(3) . . ? C97 C96 C95 124.5(3) . . ? F102 C97 C96 120.7(3) . . ? F102 C97 C98 118.8(4) . . ? C96 C97 C98 120.4(4) . . ? F103 C98 C97 121.4(4) . . ? F103 C98 C99 120.1(3) . . ? C97 C98 C99 118.5(4) . . ? F104 C99 C100 120.9(4) . . ? F104 C99 C98 120.0(4) . . ? C100 C99 C98 119.1(3) . . ? F105 C100 C99 115.8(3) . . ? F105 C100 C95 119.5(3) . . ? C99 C100 C95 124.7(4) . . ? 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 N39 Ti1 N2 C3 -162.7(2) . . . . ? N6 Ti1 N2 C3 -46.3(3) . . . . ? C52 Ti1 N2 C3 86.5(3) . . . . ? C5 Ti1 N2 C3 -20.2(2) . . . . ? N39 Ti1 N2 C7 27.4(3) . . . . ? N6 Ti1 N2 C7 143.8(3) . . . . ? C52 Ti1 N2 C7 -83.4(3) . . . . ? C5 Ti1 N2 C7 169.9(3) . . . . ? C7 N2 C3 C4 177.0(3) . . . . ? Ti1 N2 C3 C4 6.8(4) . . . . ? C7 N2 C3 C19 -3.8(6) . . . . ? Ti1 N2 C3 C19 -174.0(3) . . . . ? N2 C3 C4 C5 38.1(6) . . . . ? C19 C3 C4 C5 -141.1(4) . . . . ? C3 C4 C5 N6 -19.4(6) . . . . ? C3 C4 C5 C23 165.8(4) . . . . ? C3 C4 C5 Ti1 -44.4(4) . . . . ? N39 Ti1 C5 N6 -10.5(3) . . . . ? N2 Ti1 C5 N6 -121.0(2) . . . . ? C52 Ti1 C5 N6 132.3(2) . . . . ? N39 Ti1 C5 C4 139.3(2) . . . . ? N6 Ti1 C5 C4 149.7(3) . . . . ? N2 Ti1 C5 C4 28.7(2) . . . . ? C52 Ti1 C5 C4 -78.0(2) . . . . ? N39 Ti1 C5 C23 -99.9(4) . . . . ? N6 Ti1 C5 C23 -89.4(5) . . . . ? N2 Ti1 C5 C23 149.6(4) . . . . ? C52 Ti1 C5 C23 42.9(5) . . . . ? C4 C5 N6 C27 156.2(3) . . . . ? C23 C5 N6 C27 -29.5(5) . . . . ? Ti1 C5 N6 C27 -169.3(4) . . . . ? C4 C5 N6 Ti1 -34.5(4) . . . . ? C23 C5 N6 Ti1 139.8(3) . . . . ? N39 Ti1 N6 C5 173.0(2) . . . . ? N2 Ti1 N6 C5 59.8(2) . . . . ? C52 Ti1 N6 C5 -60.6(2) . . . . ? N39 Ti1 N6 C27 -19.2(3) . . . . ? N2 Ti1 N6 C27 -132.5(3) . . . . ? C52 Ti1 N6 C27 107.2(3) . . . . ? C5 Ti1 N6 C27 167.8(4) . . . . ? C3 N2 C7 C8 105.0(4) . . . . ? Ti1 N2 C7 C8 -86.9(4) . . . . ? C3 N2 C7 C12 -76.5(5) . . . . ? Ti1 N2 C7 C12 91.7(3) . . . . ? C12 C7 C8 C9 3.0(5) . . . . ? N2 C7 C8 C9 -178.5(3) . . . . ? C12 C7 C8 C16 -179.6(3) . . . . ? N2 C7 C8 C16 -1.1(5) . . . . ? C7 C8 C9 C10 -2.4(5) . . . . ? C16 C8 C9 C10 -179.9(4) . . . . ? C8 C9 C10 C11 -0.1(6) . . . . ? C9 C10 C11 C12 2.0(6) . . . . ? C10 C11 C12 C7 -1.4(6) . . . . ? C10 C11 C12 C13 176.9(4) . . . . ? C8 C7 C12 C11 -1.2(5) . . . . ? N2 C7 C12 C11 -179.7(3) . . . . ? C8 C7 C12 C13 -179.3(3) . . . . ? N2 C7 C12 C13 2.2(5) . . . . ? C11 C12 C13 C15 70.7(4) . . . . ? C7 C12 C13 C15 -111.1(4) . . . . ? C11 C12 C13 C14 -50.9(5) . . . . ? C7 C12 C13 C14 127.2(4) . . . . ? C7 C8 C16 C17 133.1(4) . . . . ? C9 C8 C16 C17 -49.5(5) . . . . ? C7 C8 C16 C18 -102.6(5) . . . . ? C9 C8 C16 C18 74.8(5) . . . . ? N2 C3 C19 C20 115.5(4) . . . . ? C4 C3 C19 C20 -65.2(4) . . . . ? N2 C3 C19 C21 -8.2(6) . . . . ? C4 C3 C19 C21 171.0(4) . . . . ? N2 C3 C19 C22 -126.7(4) . . . . ? C4 C3 C19 C22 52.5(5) . . . . ? N6 C5 C23 C25 32.3(5) . . . . ? C4 C5 C23 C25 -153.2(3) . . . . ? Ti1 C5 C23 C25 95.8(5) . . . . ? N6 C5 C23 C26 -88.2(4) . . . . ? C4 C5 C23 C26 86.3(4) . . . . ? Ti1 C5 C23 C26 -24.8(6) . . . . ? N6 C5 C23 C24 154.2(4) . . . . ? C4 C5 C23 C24 -31.3(5) . . . . ? Ti1 C5 C23 C24 -142.4(4) . . . . ? C5 N6 C27 C28 -78.9(4) . . . . ? Ti1 N6 C27 C28 115.5(3) . . . . ? C5 N6 C27 C32 103.0(4) . . . . ? Ti1 N6 C27 C32 -62.7(4) . . . . ? C32 C27 C28 C29 -5.1(5) . . . . ? N6 C27 C28 C29 176.8(3) . . . . ? C32 C27 C28 C36 173.6(3) . . . . ? N6 C27 C28 C36 -4.5(5) . . . . ? C27 C28 C29 C30 3.8(6) . . . . ? C36 C28 C29 C30 -175.0(4) . . . . ? C28 C29 C30 C31 -0.3(7) . . . . ? C29 C30 C31 C32 -1.9(7) . . . . ? C30 C31 C32 C27 0.5(6) . . . . ? C30 C31 C32 C33 -177.4(4) . . . . ? C28 C27 C32 C31 3.0(5) . . . . ? N6 C27 C32 C31 -178.9(3) . . . . ? C28 C27 C32 C33 -179.1(3) . . . . ? N6 C27 C32 C33 -1.1(5) . . . . ? C31 C32 C33 C34 51.7(5) . . . . ? C27 C32 C33 C34 -126.1(4) . . . . ? C31 C32 C33 C35 -71.4(5) . . . . ? C27 C32 C33 C35 110.8(4) . . . . ? C29 C28 C36 C38 35.0(5) . . . . ? C27 C28 C36 C38 -143.7(4) . . . . ? C29 C28 C36 C37 -88.0(5) . . . . ? C27 C28 C36 C37 93.2(5) . . . . ? N39 C40 C41 C42 -178.5(3) . . . . ? C45 C40 C41 C42 0.4(5) . . . . ? N39 C40 C41 C49 0.9(5) . . . . ? C45 C40 C41 C49 179.8(3) . . . . ? C40 C41 C42 C43 -0.9(6) . . . . ? C49 C41 C42 C43 179.7(4) . . . . ? C41 C42 C43 C44 -0.1(6) . . . . ? C42 C43 C44 C45 1.5(6) . . . . ? C43 C44 C45 C40 -1.9(6) . . . . ? C43 C44 C45 C46 -178.6(3) . . . . ? N39 C40 C45 C44 179.8(3) . . . . ? C41 C40 C45 C44 0.9(5) . . . . ? N39 C40 C45 C46 -3.6(5) . . . . ? C41 C40 C45 C46 177.5(3) . . . . ? C44 C45 C46 C48 -45.9(5) . . . . ? C40 C45 C46 C48 137.6(4) . . . . ? C44 C45 C46 C47 79.2(5) . . . . ? C40 C45 C46 C47 -97.3(4) . . . . ? C42 C41 C49 C51 81.4(4) . . . . ? C40 C41 C49 C51 -98.0(4) . . . . ? C42 C41 C49 C50 -43.4(5) . . . . ? C40 C41 C49 C50 137.2(4) . . . . ? N39 Ti1 C52 C53 58.1(3) . . . . ? N6 Ti1 C52 C53 -71.5(4) . . . . ? N2 Ti1 C52 C53 171.8(3) . . . . ? C5 Ti1 C52 C53 -99.2(3) . . . . ? N39 Ti1 C52 C57 -175.6(3) . . . . ? N6 Ti1 C52 C57 54.7(3) . . . . ? N2 Ti1 C52 C57 -61.9(3) . . . . ? C5 Ti1 C52 C57 27.1(3) . . . . ? C57 C52 C53 C54 -9.8(7) . . . . ? Ti1 C52 C53 C54 111.8(4) . . . . ? C52 C53 C54 C55 6.8(7) . . . . ? C53 C54 C55 N58 178.6(4) . . . . ? C53 C54 C55 C56 -1.1(6) . . . . ? N58 C55 C56 C57 179.0(4) . . . . ? C54 C55 C56 C57 -1.3(6) . . . . ? C55 C56 C57 C52 -2.0(7) . . . . ? C53 C52 C57 C56 7.5(7) . . . . ? Ti1 C52 C57 C56 -109.9(4) . . . . ? C56 C55 N58 C59 175.2(4) . . . . ? C54 C55 N58 C59 -4.5(7) . . . . ? C56 C55 N58 C60 -1.9(7) . . . . ? C54 C55 N58 C60 178.4(4) . . . . ? C73 B61 C62 C63 64.4(4) . . . . ? C84 B61 C62 C63 -172.5(4) . . . . ? C95 B61 C62 C63 -59.8(5) . . . . ? C73 B61 C62 C67 -109.7(4) . . . . ? C84 B61 C62 C67 13.4(6) . . . . ? C95 B61 C62 C67 126.0(4) . . . . ? C67 C62 C63 F68 177.5(4) . . . . ? B61 C62 C63 F68 2.6(6) . . . . ? C67 C62 C63 C64 -2.4(6) . . . . ? B61 C62 C63 C64 -177.2(4) . . . . ? F68 C63 C64 F69 1.3(6) . . . . ? C62 C63 C64 F69 -178.8(4) . . . . ? F68 C63 C64 C65 -179.5(4) . . . . ? C62 C63 C64 C65 0.3(7) . . . . ? F69 C64 C65 C66 -179.8(4) . . . . ? C63 C64 C65 C66 1.2(7) . . . . ? F69 C64 C65 F70 1.2(6) . . . . ? C63 C64 C65 F70 -177.8(4) . . . . ? C64 C65 C66 F71 178.8(4) . . . . ? F70 C65 C66 F71 -2.2(6) . . . . ? C64 C65 C66 C67 -0.4(7) . . . . ? F70 C65 C66 C67 178.6(4) . . . . ? C63 C62 C67 F72 -177.9(4) . . . . ? B61 C62 C67 F72 -3.5(6) . . . . ? C63 C62 C67 C66 3.1(6) . . . . ? B61 C62 C67 C66 177.5(4) . . . . ? F71 C66 C67 F72 -0.2(6) . . . . ? C65 C66 C67 F72 179.1(4) . . . . ? F71 C66 C67 C62 178.8(4) . . . . ? C65 C66 C67 C62 -1.9(7) . . . . ? C84 B61 C73 C78 127.6(4) . . . . ? C95 B61 C73 C78 14.1(5) . . . . ? C62 B61 C73 C78 -111.2(4) . . . . ? C84 B61 C73 C74 -57.1(4) . . . . ? C95 B61 C73 C74 -170.5(3) . . . . ? C62 B61 C73 C74 64.2(4) . . . . ? C78 C73 C74 F79 178.3(3) . . . . ? B61 C73 C74 F79 2.3(5) . . . . ? C78 C73 C74 C75 -1.8(5) . . . . ? B61 C73 C74 C75 -177.9(3) . . . . ? F79 C74 C75 F80 -0.7(5) . . . . ? C73 C74 C75 F80 179.5(3) . . . . ? F79 C74 C75 C76 -179.6(3) . . . . ? C73 C74 C75 C76 0.5(6) . . . . ? F80 C75 C76 F81 0.9(5) . . . . ? C74 C75 C76 F81 179.8(3) . . . . ? F80 C75 C76 C77 -178.8(3) . . . . ? C74 C75 C76 C77 0.1(5) . . . . ? F81 C76 C77 F82 -2.6(5) . . . . ? C75 C76 C77 F82 177.1(3) . . . . ? F81 C76 C77 C78 -179.0(3) . . . . ? C75 C76 C77 C78 0.7(6) . . . . ? F82 C77 C78 F83 0.7(5) . . . . ? C76 C77 C78 F83 177.2(3) . . . . ? F82 C77 C78 C73 -178.7(3) . . . . ? C76 C77 C78 C73 -2.3(6) . . . . ? C74 C73 C78 F83 -176.7(3) . . . . ? B61 C73 C78 F83 -1.1(5) . . . . ? C74 C73 C78 C77 2.7(5) . . . . ? B61 C73 C78 C77 178.3(3) . . . . ? C73 B61 C84 C85 172.8(3) . . . . ? C95 B61 C84 C85 -65.9(4) . . . . ? C62 B61 C84 C85 56.2(5) . . . . ? C73 B61 C84 C89 -12.5(5) . . . . ? C95 B61 C84 C89 108.8(4) . . . . ? C62 B61 C84 C89 -129.1(4) . . . . ? C89 C84 C85 F90 -178.9(3) . . . . ? B61 C84 C85 F90 -3.5(5) . . . . ? C89 C84 C85 C86 -0.8(5) . . . . ? B61 C84 C85 C86 174.6(4) . . . . ? F90 C85 C86 F91 -2.7(5) . . . . ? C84 C85 C86 F91 179.1(3) . . . . ? F90 C85 C86 C87 179.3(3) . . . . ? C84 C85 C86 C87 1.1(6) . . . . ? F91 C86 C87 C88 -178.8(3) . . . . ? C85 C86 C87 C88 -0.9(6) . . . . ? F91 C86 C87 F92 3.2(5) . . . . ? C85 C86 C87 F92 -178.8(3) . . . . ? F92 C87 C88 F93 -1.2(6) . . . . ? C86 C87 C88 F93 -179.1(3) . . . . ? F92 C87 C88 C89 178.3(3) . . . . ? C86 C87 C88 C89 0.3(6) . . . . ? C85 C84 C89 F94 177.6(3) . . . . ? B61 C84 C89 F94 2.6(6) . . . . ? C85 C84 C89 C88 0.2(5) . . . . ? B61 C84 C89 C88 -174.7(4) . . . . ? F93 C88 C89 F94 1.9(5) . . . . ? C87 C88 C89 F94 -177.5(3) . . . . ? F93 C88 C89 C84 179.4(3) . . . . ? C87 C88 C89 C84 0.0(6) . . . . ? C73 B61 C95 C96 -129.7(4) . . . . ? C84 B61 C95 C96 108.4(4) . . . . ? C62 B61 C95 C96 -10.9(5) . . . . ? C73 B61 C95 C100 60.1(4) . . . . ? C84 B61 C95 C100 -61.8(4) . . . . ? C62 B61 C95 C100 178.8(3) . . . . ? C100 C95 C96 F101 -179.4(3) . . . . ? B61 C95 C96 F101 9.9(5) . . . . ? C100 C95 C96 C97 1.6(5) . . . . ? B61 C95 C96 C97 -169.1(3) . . . . ? F101 C96 C97 F102 1.1(5) . . . . ? C95 C96 C97 F102 -179.8(3) . . . . ? F101 C96 C97 C98 -178.9(3) . . . . ? C95 C96 C97 C98 0.2(6) . . . . ? F102 C97 C98 F103 -0.9(5) . . . . ? C96 C97 C98 F103 179.0(3) . . . . ? F102 C97 C98 C99 179.0(3) . . . . ? C96 C97 C98 C99 -1.1(5) . . . . ? F103 C98 C99 F104 -0.1(5) . . . . ? C97 C98 C99 F104 -180.0(3) . . . . ? F103 C98 C99 C100 180.0(3) . . . . ? C97 C98 C99 C100 0.1(5) . . . . ? F104 C99 C100 F105 0.0(5) . . . . ? C98 C99 C100 F105 -180.0(3) . . . . ? F104 C99 C100 C95 -178.0(3) . . . . ? C98 C99 C100 C95 2.0(5) . . . . ? C96 C95 C100 F105 179.4(3) . . . . ? B61 C95 C100 F105 -9.0(5) . . . . ? C96 C95 C100 C99 -2.7(5) . . . . ? B61 C95 C100 C99 169.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.741 _refine_diff_density_min -0.418 _refine_diff_density_rms 0.068