# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Daniel Mindiola' 'Falguni Basuli' 'John C. Huffman' _publ_contact_author_name 'Prof Daniel Mindiola' _publ_contact_author_address ; Chemistry Indiana University 800 E. Kirkwood Ave, Bloomington IN 47405 UNITED STATES OF AMERICA ; _publ_contact_author_email MINDIOLA@INDIANA.EDU _publ_requested_journal 'Chemical Communications' _publ_section_title ; Snapshots of an oxidatively induced alpha-hydrogen abstraction reaction to prepare a terminal and four-coordinate titanium imide ; data_d:\2002data\02188lb\02188 _database_code_CSD 209461 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _exptl_crystal_id MSC02188 _audit_creation_date 12/26/2002 _chemical_formula_structural Ti(C29H41N2)(NHC6H3iPr2)2 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H77 N4 Ti' _chemical_formula_weight 818.09 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' 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 11.3389(14) _cell_length_b 11.7121(15) _cell_length_c 20.010(2) _cell_angle_alpha 90.265(3) _cell_angle_beta 95.720(3) _cell_angle_gamma 115.017(3) _cell_volume 2392.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 138(2) _cell_measurement_reflns_used 7608 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 30.01 _exptl_crystal_description 'cleaved fragment' _exptl_crystal_colour 'dark green' _exptl_crystal_size_max .3 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.135 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 890 _exptl_absorpt_coefficient_mu 0.217 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 138(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 3.16 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 26431 _diffrn_reflns_av_R_equivalents 0.1253 _diffrn_reflns_av_sigmaI/netI 0.1613 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 30.07 _reflns_number_total 13917 _reflns_number_gt 7605 _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 ? _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^)+(0.0670P)^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 13917 _refine_ls_number_parameters 831 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1173 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.1694 _refine_ls_wR_factor_gt 0.1465 _refine_ls_goodness_of_fit_ref 0.880 _refine_ls_restrained_S_all 0.880 _refine_ls_shift/su_max 0.009 _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 0.75727(4) 0.69215(4) 0.75201(2) 0.01664(11) Uani 1 1 d . . . H132 H 0.463(3) 0.707(3) 0.6263(17) 0.047(9) Uiso 1 1 d . . . H133 H 0.399(3) 0.761(3) 0.6745(15) 0.035(8) Uiso 1 1 d . . . N2 N 0.94748(18) 0.72401(17) 0.73833(10) 0.0178(4) Uani 1 1 d . . . C3 C 1.0525(2) 0.8230(2) 0.76869(12) 0.0201(5) Uani 1 1 d . . . C4 C 1.0477(2) 0.9314(2) 0.79553(13) 0.0223(5) Uani 1 1 d . . . C5 C 0.9437(2) 0.9673(2) 0.78782(12) 0.0205(5) Uani 1 1 d . . . N6 N 0.82149(18) 0.88850(17) 0.76415(10) 0.0185(4) Uani 1 1 d . . . C7 C 0.9738(2) 0.6377(2) 0.69662(12) 0.0191(5) Uani 1 1 d . . . C8 C 0.9490(2) 0.5149(2) 0.71811(12) 0.0199(5) Uani 1 1 d . . . C9 C 0.9732(2) 0.4348(2) 0.67473(13) 0.0226(5) Uani 1 1 d . . . C11 C 1.0174(2) 0.4706(2) 0.61335(13) 0.0245(5) Uani 1 1 d . . . C12 C 1.0392(2) 0.5901(2) 0.59287(13) 0.0256(5) Uani 1 1 d . . . C13 C 1.0184(2) 0.6750(2) 0.63359(12) 0.0230(5) Uani 1 1 d . . . C14 C 1.0449(3) 0.8057(2) 0.60769(14) 0.0293(6) Uani 1 1 d . . . C15 C 1.1873(3) 0.8768(3) 0.5918(2) 0.0437(7) Uani 1 1 d . . . C16 C 0.9504(3) 0.7952(3) 0.54562(16) 0.0374(7) Uani 1 1 d . . . C17 C 0.9002(2) 0.4688(2) 0.78443(12) 0.0211(5) Uani 1 1 d . . . C18 C 0.9978(3) 0.4359(3) 0.82976(14) 0.0286(6) Uani 1 1 d . . . C19 C 0.7665(3) 0.3530(2) 0.77403(15) 0.0275(5) Uani 1 1 d . . . C20 C 1.1853(2) 0.8202(3) 0.77588(16) 0.0281(6) Uani 1 1 d . . . C21 C 0.9780(3) 1.1033(2) 0.80810(17) 0.0301(6) Uani 1 1 d . . . C22 C 0.7243(2) 0.9376(2) 0.74998(12) 0.0198(5) Uani 1 1 d . . . C23 C 0.6988(2) 0.9664(2) 0.68365(13) 0.0231(5) Uani 1 1 d . . . C24 C 0.6020(3) 1.0104(2) 0.66967(14) 0.0281(6) Uani 1 1 d . . . C25 C 0.5335(3) 1.0255(2) 0.71979(14) 0.0290(6) Uani 1 1 d . . . C26 C 0.5591(2) 0.9958(2) 0.78423(14) 0.0269(5) Uani 1 1 d . . . C27 C 0.6549(2) 0.9521(2) 0.80155(13) 0.0232(5) Uani 1 1 d . . . C28 C 0.6828(3) 0.9261(3) 0.87422(13) 0.0285(6) Uani 1 1 d . . . C29 C 0.7184(4) 1.0429(4) 0.92133(18) 0.0445(8) Uani 1 1 d . . . C30 C 0.5680(3) 0.8127(3) 0.89757(16) 0.0376(7) Uani 1 1 d . . . C31 C 0.7766(3) 0.9548(2) 0.62807(13) 0.0268(5) Uani 1 1 d . . . C32 C 0.8978(3) 1.0789(3) 0.62345(18) 0.0369(7) Uani 1 1 d . . . C33 C 0.6959(3) 0.9144(3) 0.55942(15) 0.0402(7) Uani 1 1 d . . . N34 N 0.6765(2) 0.59053(19) 0.82653(10) 0.0231(4) Uani 1 1 d . . . C35 C 0.6908(2) 0.5326(2) 0.88607(12) 0.0210(5) Uani 1 1 d . . . C36 C 0.5912(2) 0.4145(2) 0.90124(12) 0.0237(5) Uani 1 1 d . . . C37 C 0.6135(3) 0.3553(3) 0.95775(14) 0.0317(6) Uani 1 1 d . . . C38 C 0.7286(3) 0.4078(3) 1.00046(15) 0.0370(7) Uani 1 1 d . . . C39 C 0.8227(3) 0.5249(3) 0.98750(14) 0.0340(6) Uani 1 1 d . . . C40 C 0.8068(2) 0.5890(2) 0.93150(12) 0.0235(5) Uani 1 1 d . . . C41 C 0.9095(2) 0.7214(2) 0.92281(13) 0.0247(5) Uani 1 1 d . . . C42 C 1.0494(3) 0.7310(3) 0.92994(16) 0.0333(6) Uani 1 1 d . . . C43 C 0.9014(3) 0.8151(3) 0.97367(16) 0.0347(6) Uani 1 1 d . . . C44 C 0.4573(3) 0.3530(2) 0.85998(15) 0.0283(5) Uani 1 1 d . . . C45 C 0.4203(3) 0.2168(3) 0.8354(2) 0.0504(9) Uani 1 1 d . . . C46 C 0.3527(3) 0.3612(4) 0.8995(2) 0.0489(8) Uani 1 1 d . . . N47 N 0.6631(2) 0.61742(18) 0.66345(11) 0.0210(4) Uani 1 1 d . . . C48 C 0.5478(2) 0.5039(2) 0.65252(11) 0.0198(5) Uani 1 1 d . . . C49 C 0.4347(2) 0.4941(2) 0.68098(12) 0.0230(5) Uani 1 1 d . . . C50 C 0.3235(3) 0.3797(3) 0.67364(15) 0.0310(6) Uani 1 1 d . . . C51 C 0.3202(3) 0.2768(3) 0.63734(16) 0.0350(6) Uani 1 1 d . . . C52 C 0.4297(3) 0.2883(2) 0.60746(14) 0.0288(6) Uani 1 1 d . . . C53 C 0.5436(2) 0.4004(2) 0.61382(12) 0.0223(5) Uani 1 1 d . . . C54 C 0.6604(2) 0.4148(2) 0.57749(12) 0.0234(5) Uani 1 1 d . . . C55 C 0.6590(3) 0.4814(3) 0.51164(14) 0.0318(6) Uani 1 1 d . . . C56 C 0.6698(3) 0.2905(3) 0.56287(17) 0.0337(6) Uani 1 1 d . . . C57 C 0.4295(2) 0.6100(2) 0.71328(13) 0.0263(5) Uani 1 1 d . . . C58 C 0.3991(3) 0.6865(3) 0.65824(16) 0.0322(6) Uani 1 1 d . . . C59 C 0.3323(3) 0.5814(3) 0.76496(16) 0.0340(6) Uani 1 1 d . . . H60 H 1.128(3) 0.992(2) 0.8193(13) 0.019(6) Uiso 1 1 d . . . H61 H 0.953(3) 0.356(3) 0.6858(13) 0.021(7) Uiso 1 1 d . . . H62 H 1.028(2) 0.411(2) 0.5838(13) 0.020(6) Uiso 1 1 d . . . H63 H 1.066(3) 0.614(2) 0.5481(14) 0.020(6) Uiso 1 1 d . . . H64 H 1.036(2) 0.855(2) 0.6433(13) 0.017(6) Uiso 1 1 d . . . H65 H 1.252(3) 0.891(3) 0.6301(17) 0.039(8) Uiso 1 1 d . . . H66 H 1.200(3) 0.959(3) 0.5791(18) 0.053(10) Uiso 1 1 d . . . H67 H 1.204(3) 0.838(3) 0.5482(17) 0.043(9) Uiso 1 1 d . . . H68 H 0.968(3) 0.876(3) 0.5315(17) 0.047(9) Uiso 1 1 d . . . H69 H 0.965(3) 0.751(3) 0.5097(15) 0.029(7) Uiso 1 1 d . . . H70 H 0.853(4) 0.753(3) 0.5548(18) 0.054(10) Uiso 1 1 d . . . H71 H 0.895(2) 0.539(2) 0.8106(13) 0.018(6) Uiso 1 1 d . . . H72 H 0.971(3) 0.412(3) 0.8730(17) 0.037(8) Uiso 1 1 d . . . H73 H 1.010(3) 0.368(2) 0.8091(14) 0.024(7) Uiso 1 1 d . . . H74 H 1.084(3) 0.512(3) 0.8386(14) 0.031(7) Uiso 1 1 d . . . H75 H 0.704(3) 0.373(3) 0.7448(15) 0.031(7) Uiso 1 1 d . . . H76 H 0.738(2) 0.330(2) 0.8176(14) 0.018(6) Uiso 1 1 d . . . H77 H 0.779(2) 0.282(2) 0.7515(13) 0.019(6) Uiso 1 1 d . . . H78 H 1.179(4) 0.743(4) 0.7916(19) 0.062(11) Uiso 1 1 d . . . H79 H 1.212(3) 0.826(3) 0.7338(17) 0.038(9) Uiso 1 1 d . . . H80 H 1.240(3) 0.879(3) 0.8106(18) 0.056(10) Uiso 1 1 d . . . H81 H 1.068(4) 1.166(3) 0.8014(18) 0.057(10) Uiso 1 1 d . . . H82 H 0.978(3) 1.112(3) 0.8527(18) 0.041(9) Uiso 1 1 d . . . H83 H 0.913(3) 1.130(3) 0.7917(15) 0.036(8) Uiso 1 1 d . . . H84 H 0.582(3) 1.027(2) 0.6246(14) 0.021(7) Uiso 1 1 d . . . H85 H 0.469(3) 1.061(3) 0.7078(17) 0.049(9) Uiso 1 1 d . . . H86 H 0.520(3) 1.009(2) 0.8212(14) 0.021(7) Uiso 1 1 d . . . H87 H 0.757(3) 0.906(2) 0.8779(14) 0.028(7) Uiso 1 1 d . . . H88 H 0.740(3) 1.027(3) 0.9667(19) 0.048(9) Uiso 1 1 d . . . H89 H 0.785(4) 1.115(4) 0.911(2) 0.077(14) Uiso 1 1 d . . . H90 H 0.641(4) 1.062(3) 0.9236(18) 0.058(10) Uiso 1 1 d . . . H91 H 0.586(3) 0.801(3) 0.9431(17) 0.043(9) Uiso 1 1 d . . . H92 H 0.489(3) 0.831(3) 0.8966(15) 0.039(8) Uiso 1 1 d . . . H93 H 0.547(3) 0.736(3) 0.8722(15) 0.034(8) Uiso 1 1 d . . . H94 H 0.808(3) 0.888(3) 0.6418(14) 0.028(7) Uiso 1 1 d . . . H95 H 0.941(3) 1.072(3) 0.5867(17) 0.038(8) Uiso 1 1 d . . . H96 H 0.945(4) 1.103(3) 0.663(2) 0.057(11) Uiso 1 1 d . . . H97 H 0.871(3) 1.148(3) 0.6144(16) 0.042(9) Uiso 1 1 d . . . H98 H 0.740(3) 0.895(3) 0.5244(18) 0.046(9) Uiso 1 1 d . . . H99 H 0.615(3) 0.831(3) 0.5608(17) 0.050(9) Uiso 1 1 d . . . H100 H 0.660(3) 0.970(3) 0.5438(18) 0.049(10) Uiso 1 1 d . . . H101 H 0.600(3) 0.549(2) 0.8063(13) 0.017(6) Uiso 1 1 d . . . H102 H 0.546(3) 0.273(3) 0.9642(15) 0.032(8) Uiso 1 1 d . . . H103 H 0.746(3) 0.369(3) 1.0388(17) 0.046(9) Uiso 1 1 d . . . H104 H 0.897(3) 0.560(3) 1.0162(18) 0.050(10) Uiso 1 1 d . . . H105 H 0.896(2) 0.745(2) 0.8779(13) 0.018(6) Uiso 1 1 d . . . H106 H 1.070(3) 0.712(3) 0.9745(17) 0.042(9) Uiso 1 1 d . . . H107 H 1.049(3) 0.662(3) 0.8969(17) 0.047(9) Uiso 1 1 d . . . H108 H 1.111(3) 0.814(3) 0.9263(15) 0.036(8) Uiso 1 1 d . . . H109 H 0.814(3) 0.810(3) 0.9728(15) 0.035(8) Uiso 1 1 d . . . H110 H 0.923(3) 0.805(3) 1.0192(18) 0.049(10) Uiso 1 1 d . . . H111 H 0.957(3) 0.898(3) 0.9649(15) 0.037(8) Uiso 1 1 d . . . H112 H 0.456(3) 0.395(2) 0.8217(14) 0.022(7) Uiso 1 1 d . . . H113 H 0.334(4) 0.186(3) 0.8073(19) 0.060(11) Uiso 1 1 d . . . H114 H 0.490(4) 0.209(4) 0.806(2) 0.076(12) Uiso 1 1 d . . . H115 H 0.413(4) 0.172(4) 0.874(2) 0.055(11) Uiso 1 1 d . . . H116 H 0.262(3) 0.329(3) 0.8722(15) 0.030(7) Uiso 1 1 d . . . H117 H 0.344(4) 0.310(4) 0.937(2) 0.074(13) Uiso 1 1 d . . . H118 H 0.380(3) 0.452(3) 0.9143(17) 0.045(9) Uiso 1 1 d . . . H119 H 0.704(3) 0.627(3) 0.6298(18) 0.047(10) Uiso 1 1 d . . . H120 H 0.250(3) 0.371(3) 0.6906(16) 0.042(9) Uiso 1 1 d . . . H121 H 0.250(3) 0.202(3) 0.6358(15) 0.032(8) Uiso 1 1 d . . . H122 H 0.421(3) 0.216(2) 0.5802(13) 0.022(7) Uiso 1 1 d . . . H123 H 0.734(2) 0.467(2) 0.6058(13) 0.017(6) Uiso 1 1 d . . . H124 H 0.741(4) 0.498(3) 0.4889(18) 0.057(10) Uiso 1 1 d . . . H125 H 0.588(4) 0.430(3) 0.4818(18) 0.054(10) Uiso 1 1 d . . . H126 H 0.656(3) 0.559(3) 0.5205(16) 0.039(8) Uiso 1 1 d . . . H127 H 0.756(3) 0.310(3) 0.5443(17) 0.050(9) Uiso 1 1 d . . . H128 H 0.665(3) 0.245(3) 0.6050(16) 0.035(8) Uiso 1 1 d . . . H129 H 0.591(3) 0.234(3) 0.5315(15) 0.034(8) Uiso 1 1 d . . . H130 H 0.516(3) 0.663(2) 0.7380(13) 0.021(6) Uiso 1 1 d . . . H131 H 0.317(4) 0.640(3) 0.6340(18) 0.049(9) Uiso 1 1 d . . . H134 H 0.338(3) 0.527(3) 0.8007(17) 0.046(9) Uiso 1 1 d . . . H135 H 0.351(3) 0.660(3) 0.7867(15) 0.035(8) Uiso 1 1 d . . . H136 H 0.237(3) 0.538(3) 0.7409(16) 0.040(8) 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 0.01444(19) 0.01780(19) 0.0187(2) 0.00072(15) 0.00001(15) 0.00821(15) N2 0.0140(9) 0.0189(9) 0.0213(10) -0.0012(7) 0.0001(7) 0.0082(7) C3 0.0145(10) 0.0231(11) 0.0227(12) 0.0011(9) 0.0023(9) 0.0081(9) C4 0.0155(11) 0.0212(11) 0.0274(13) -0.0049(10) -0.0022(10) 0.0060(9) C5 0.0199(11) 0.0198(11) 0.0227(12) -0.0001(9) 0.0019(9) 0.0094(9) N6 0.0168(9) 0.0187(9) 0.0213(10) -0.0004(7) -0.0006(8) 0.0094(7) C7 0.0131(10) 0.0216(11) 0.0232(11) -0.0031(9) -0.0031(9) 0.0091(9) C8 0.0143(10) 0.0223(11) 0.0231(12) -0.0021(9) -0.0028(9) 0.0088(9) C9 0.0198(11) 0.0211(11) 0.0286(13) -0.0025(10) -0.0039(10) 0.0119(9) C11 0.0212(12) 0.0285(12) 0.0258(13) -0.0079(10) -0.0018(10) 0.0135(10) C12 0.0235(12) 0.0302(13) 0.0248(13) -0.0010(10) 0.0064(10) 0.0121(10) C13 0.0209(12) 0.0251(11) 0.0250(12) 0.0007(10) 0.0028(10) 0.0116(10) C14 0.0385(15) 0.0261(12) 0.0256(13) 0.0037(10) 0.0115(11) 0.0143(11) C15 0.0406(18) 0.0349(16) 0.051(2) 0.0121(15) 0.0119(16) 0.0101(14) C16 0.053(2) 0.0339(15) 0.0328(16) 0.0086(13) 0.0093(14) 0.0242(14) C17 0.0218(11) 0.0187(11) 0.0246(12) 0.0003(9) 0.0000(10) 0.0107(9) C18 0.0335(15) 0.0289(13) 0.0277(14) 0.0016(11) -0.0009(12) 0.0183(12) C19 0.0227(13) 0.0242(12) 0.0333(15) 0.0006(11) 0.0049(11) 0.0075(10) C20 0.0175(12) 0.0303(14) 0.0374(16) -0.0066(12) 0.0009(11) 0.0117(10) C21 0.0255(14) 0.0225(12) 0.0421(17) -0.0071(12) -0.0037(12) 0.0117(11) C22 0.0177(11) 0.0142(10) 0.0259(12) -0.0018(9) -0.0037(9) 0.0067(8) C23 0.0225(12) 0.0172(10) 0.0276(13) 0.0002(9) 0.0000(10) 0.0073(9) C24 0.0295(13) 0.0219(12) 0.0330(14) 0.0042(10) -0.0035(11) 0.0125(10) C25 0.0243(13) 0.0238(12) 0.0410(15) 0.0004(11) -0.0032(11) 0.0138(10) C26 0.0209(12) 0.0262(12) 0.0364(15) -0.0029(11) 0.0017(11) 0.0130(10) C27 0.0214(12) 0.0209(11) 0.0280(13) -0.0025(9) -0.0009(10) 0.0104(9) C28 0.0268(13) 0.0368(14) 0.0279(13) -0.0015(11) 0.0013(11) 0.0198(11) C29 0.046(2) 0.056(2) 0.0367(18) -0.0137(16) -0.0024(15) 0.0281(18) C30 0.0347(16) 0.0518(19) 0.0309(16) 0.0080(14) 0.0078(13) 0.0219(14) C31 0.0319(14) 0.0243(12) 0.0268(13) 0.0050(10) 0.0036(11) 0.0144(11) C32 0.0353(16) 0.0346(15) 0.0375(17) 0.0001(13) 0.0106(14) 0.0105(13) C33 0.0387(17) 0.0512(19) 0.0270(15) 0.0048(14) 0.0042(13) 0.0153(16) N34 0.0171(10) 0.0267(10) 0.0234(10) 0.0029(8) -0.0027(8) 0.0084(8) C35 0.0215(11) 0.0276(12) 0.0215(12) 0.0045(9) 0.0050(9) 0.0172(10) C36 0.0247(12) 0.0269(12) 0.0264(13) 0.0052(10) 0.0085(10) 0.0165(10) C37 0.0359(15) 0.0330(14) 0.0355(15) 0.0138(12) 0.0145(12) 0.0211(12) C38 0.0446(17) 0.0502(17) 0.0300(15) 0.0186(13) 0.0089(13) 0.0322(15) C39 0.0332(15) 0.0499(17) 0.0258(14) 0.0049(12) -0.0026(12) 0.0257(14) C40 0.0234(12) 0.0309(12) 0.0222(12) 0.0011(10) 0.0017(10) 0.0174(10) C41 0.0203(12) 0.0333(13) 0.0217(12) -0.0026(10) -0.0038(10) 0.0140(10) C42 0.0232(13) 0.0401(16) 0.0372(16) -0.0064(13) -0.0058(12) 0.0161(12) C43 0.0333(16) 0.0387(16) 0.0359(17) -0.0053(13) -0.0010(13) 0.0201(13) C44 0.0247(13) 0.0274(13) 0.0358(15) 0.0061(11) 0.0092(11) 0.0127(11) C45 0.0336(18) 0.0309(16) 0.083(3) -0.0046(18) 0.0027(19) 0.0113(14) C46 0.0278(16) 0.070(2) 0.056(2) 0.0020(19) 0.0107(16) 0.0266(17) N47 0.0193(10) 0.0221(10) 0.0218(10) 0.0007(8) 0.0006(8) 0.0094(8) C48 0.0182(11) 0.0228(11) 0.0193(11) 0.0001(9) -0.0040(9) 0.0110(9) C49 0.0185(11) 0.0286(12) 0.0234(12) -0.0020(10) -0.0041(9) 0.0129(10) C50 0.0183(12) 0.0346(14) 0.0395(16) -0.0014(12) 0.0014(11) 0.0111(11) C51 0.0235(14) 0.0280(14) 0.0464(17) -0.0030(12) 0.0023(12) 0.0047(11) C52 0.0258(13) 0.0252(12) 0.0339(14) -0.0072(11) -0.0043(11) 0.0113(10) C53 0.0216(12) 0.0257(12) 0.0218(12) -0.0009(9) -0.0046(9) 0.0136(10) C54 0.0233(12) 0.0253(12) 0.0230(12) -0.0043(10) -0.0030(10) 0.0129(10) C55 0.0339(15) 0.0407(16) 0.0249(13) -0.0002(12) -0.0008(12) 0.0208(13) C56 0.0311(15) 0.0318(14) 0.0424(17) -0.0068(13) -0.0015(13) 0.0188(12) C57 0.0173(12) 0.0309(13) 0.0316(14) -0.0053(11) -0.0045(10) 0.0129(10) C58 0.0308(15) 0.0256(13) 0.0396(16) -0.0021(12) -0.0013(13) 0.0126(12) C59 0.0327(15) 0.0433(16) 0.0354(16) -0.0003(13) 0.0075(12) 0.0247(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 N34 1.961(2) . ? Ti1 N47 1.966(2) . ? Ti1 N2 2.0746(19) . ? Ti1 N6 2.1027(18) . ? N2 C3 1.346(3) . ? N2 C7 1.450(3) . ? C3 C4 1.401(3) . ? C3 C20 1.512(3) . ? C4 C5 1.405(3) . ? C5 N6 1.334(3) . ? C5 C21 1.514(3) . ? N6 C22 1.449(3) . ? C7 C13 1.408(4) . ? C7 C8 1.422(3) . ? C8 C9 1.402(3) . ? C8 C17 1.503(3) . ? C9 C11 1.373(4) . ? C11 C12 1.386(4) . ? C12 C13 1.393(3) . ? C13 C14 1.533(4) . ? C14 C16 1.526(4) . ? C14 C15 1.539(4) . ? C17 C18 1.537(3) . ? C17 C19 1.542(3) . ? C22 C23 1.403(3) . ? C22 C27 1.410(3) . ? C23 C24 1.402(3) . ? C23 C31 1.527(4) . ? C24 C25 1.382(4) . ? C25 C26 1.372(4) . ? C26 C27 1.399(3) . ? C27 C28 1.517(4) . ? C28 C30 1.530(4) . ? C28 C29 1.540(4) . ? C31 C33 1.525(4) . ? C31 C32 1.532(4) . ? N34 C35 1.403(3) . ? C35 C40 1.419(3) . ? C35 C36 1.425(3) . ? C36 C37 1.387(4) . ? C36 C44 1.525(4) . ? C37 C38 1.381(4) . ? C38 C39 1.381(4) . ? C39 C40 1.390(4) . ? C40 C41 1.519(4) . ? C41 C43 1.530(4) . ? C41 C42 1.534(3) . ? C44 C46 1.524(4) . ? C44 C45 1.533(4) . ? N47 C48 1.413(3) . ? C48 C49 1.415(3) . ? C48 C53 1.417(3) . ? C49 C50 1.393(4) . ? C49 C57 1.527(3) . ? C50 C51 1.388(4) . ? C51 C52 1.387(4) . ? C52 C53 1.392(3) . ? C53 C54 1.521(3) . ? C54 C56 1.533(3) . ? C54 C55 1.536(4) . ? C57 C59 1.521(4) . ? C57 C58 1.525(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 N34 Ti1 N47 112.99(9) . . ? N34 Ti1 N2 118.60(8) . . ? N47 Ti1 N2 101.65(8) . . ? N34 Ti1 N6 117.20(8) . . ? N47 Ti1 N6 114.88(8) . . ? N2 Ti1 N6 88.42(7) . . ? C3 N2 C7 116.52(18) . . ? C3 N2 Ti1 122.29(14) . . ? C7 N2 Ti1 121.16(14) . . ? N2 C3 C4 124.0(2) . . ? N2 C3 C20 119.8(2) . . ? C4 C3 C20 116.2(2) . . ? C3 C4 C5 128.3(2) . . ? N6 C5 C4 123.3(2) . . ? N6 C5 C21 120.9(2) . . ? C4 C5 C21 115.8(2) . . ? C5 N6 C22 119.33(18) . . ? C5 N6 Ti1 123.31(15) . . ? C22 N6 Ti1 117.23(14) . . ? C13 C7 C8 120.6(2) . . ? C13 C7 N2 119.3(2) . . ? C8 C7 N2 120.1(2) . . ? C9 C8 C7 117.3(2) . . ? C9 C8 C17 119.4(2) . . ? C7 C8 C17 123.3(2) . . ? C11 C9 C8 122.5(2) . . ? C9 C11 C12 119.4(2) . . ? C11 C12 C13 121.3(2) . . ? C12 C13 C7 118.9(2) . . ? C12 C13 C14 118.4(2) . . ? C7 C13 C14 122.7(2) . . ? C16 C14 C13 110.9(2) . . ? C16 C14 C15 110.1(3) . . ? C13 C14 C15 111.7(2) . . ? C8 C17 C18 112.1(2) . . ? C8 C17 C19 111.0(2) . . ? C18 C17 C19 109.5(2) . . ? C23 C22 C27 121.3(2) . . ? C23 C22 N6 118.4(2) . . ? C27 C22 N6 120.3(2) . . ? C24 C23 C22 118.3(2) . . ? C24 C23 C31 120.2(2) . . ? C22 C23 C31 121.5(2) . . ? C25 C24 C23 121.1(3) . . ? C26 C25 C24 119.8(2) . . ? C25 C26 C27 122.0(2) . . ? C26 C27 C22 117.6(2) . . ? C26 C27 C28 119.6(2) . . ? C22 C27 C28 122.7(2) . . ? C27 C28 C30 111.9(2) . . ? C27 C28 C29 111.4(2) . . ? C30 C28 C29 110.2(3) . . ? C33 C31 C23 113.4(2) . . ? C33 C31 C32 109.8(3) . . ? C23 C31 C32 110.6(2) . . ? C35 N34 Ti1 148.64(17) . . ? N34 C35 C40 120.5(2) . . ? N34 C35 C36 120.8(2) . . ? C40 C35 C36 118.7(2) . . ? C37 C36 C35 119.1(2) . . ? C37 C36 C44 118.0(2) . . ? C35 C36 C44 122.8(2) . . ? C38 C37 C36 122.1(3) . . ? C39 C38 C37 118.8(3) . . ? C38 C39 C40 121.9(3) . . ? C39 C40 C35 119.3(2) . . ? C39 C40 C41 119.3(2) . . ? C35 C40 C41 121.3(2) . . ? C40 C41 C43 110.4(2) . . ? C40 C41 C42 113.0(2) . . ? C43 C41 C42 109.1(2) . . ? C46 C44 C36 110.3(2) . . ? C46 C44 C45 111.3(3) . . ? C36 C44 C45 113.2(2) . . ? C48 N47 Ti1 125.11(17) . . ? N47 C48 C49 119.0(2) . . ? N47 C48 C53 121.2(2) . . ? C49 C48 C53 119.7(2) . . ? C50 C49 C48 118.9(2) . . ? C50 C49 C57 120.0(2) . . ? C48 C49 C57 120.8(2) . . ? C51 C50 C49 121.4(3) . . ? C52 C51 C50 119.4(3) . . ? C51 C52 C53 121.4(2) . . ? C52 C53 C48 119.0(2) . . ? C52 C53 C54 121.1(2) . . ? C48 C53 C54 119.8(2) . . ? C53 C54 C56 114.2(2) . . ? C53 C54 C55 110.3(2) . . ? C56 C54 C55 109.6(2) . . ? C59 C57 C58 109.7(2) . . ? C59 C57 C49 114.8(2) . . ? C58 C57 C49 109.1(2) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 30.07 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.042 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.089 data_compound2 _database_code_CSD 209462 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _exptl_crystal_id MSC02190 _audit_creation_date 10/27/2002 _chemical_formula_structural Ti(C29H41N2)(NC6H3iPr2)(O3SCF3);C5H12 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H70 F3 N3 O3 S Ti' _chemical_formula_weight 862.02 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2710(14) _cell_length_b 12.9651(17) _cell_length_c 18.451(3) _cell_angle_alpha 93.783(7) _cell_angle_beta 106.097(9) _cell_angle_gamma 96.880(9) _cell_volume 2330.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 138(2) _cell_measurement_reflns_used 7572 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 27.47 _exptl_crystal_description irregular _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 0.282 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9202 _exptl_absorpt_correction_T_max 0.9328 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 138(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 15.14 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 51577 _diffrn_reflns_av_R_equivalents 0.0834 _diffrn_reflns_av_sigmaI/netI 0.0725 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.60 _reflns_number_total 10763 _reflns_number_gt 7221 _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 ? _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^)+(0.0435P)^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 10763 _refine_ls_number_parameters 829 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.0978 _refine_ls_wR_factor_gt 0.0861 _refine_ls_goodness_of_fit_ref 0.933 _refine_ls_restrained_S_all 0.933 _refine_ls_shift/su_max 0.505 _refine_ls_shift/su_mean 0.009 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 0.24096(3) 0.31161(3) 0.297992(18) 0.01512(9) Uani 1 1 d . . . H1S H 0.388(4) -0.206(3) 0.128(2) 0.112(13) Uiso 1 1 d . . . N2 N 0.37879(15) 0.37166(12) 0.25005(8) 0.0167(3) Uani 1 1 d . . . H2S H 0.447(5) -0.140(4) 0.077(3) 0.156(19) Uiso 1 1 d . . . C3 C 0.49658(18) 0.40367(14) 0.30720(10) 0.0194(4) Uani 1 1 d . . . H3S H 0.396(4) -0.255(3) 0.052(2) 0.100(13) Uiso 1 1 d . . . C4 C 0.5363(2) 0.35065(15) 0.37087(11) 0.0210(4) Uani 1 1 d . . . H4S H 0.648(4) -0.230(3) 0.089(2) 0.013(9) Uiso 0.50 1 d P . . C5 C 0.48177(18) 0.25312(15) 0.38928(10) 0.0184(4) Uani 1 1 d . . . H5S H 0.628(5) -0.167(5) 0.184(3) 0.063(16) Uiso 0.50 1 d P . . N6 N 0.35339(14) 0.20898(11) 0.35587(8) 0.0162(3) Uani 1 1 d . . . H6S H 0.573(4) -0.269(3) 0.215(2) 0.107(14) Uiso 1 1 d . . . C7 C 0.36210(18) 0.41015(14) 0.17716(10) 0.0172(4) Uani 1 1 d . . . H7S H 0.565(4) -0.369(3) 0.135(2) 0.012(9) Uiso 0.50 1 d P . . C8 C 0.26722(18) 0.47962(14) 0.15339(11) 0.0196(4) Uani 1 1 d . . . H8S H 0.774(4) -0.379(3) 0.222(2) 0.018(10) Uiso 0.50 1 d P . . C9 C 0.2454(2) 0.50919(16) 0.08005(11) 0.0241(4) Uani 1 1 d . . . H9S H 0.797(4) -0.273(3) 0.281(3) 0.021(12) Uiso 0.50 1 d P . . C10 C 0.3149(2) 0.47286(16) 0.03210(11) 0.0249(4) Uani 1 1 d . . . H10S H 0.821(7) -0.291(6) 0.147(4) 0.09(2) Uiso 0.50 1 d P . . C11 C 0.4103(2) 0.40656(16) 0.05706(11) 0.0244(4) Uani 1 1 d . . . H11S H 0.971(5) -0.260(3) 0.233(2) 0.027(11) Uiso 0.50 1 d P . . C12 C 0.43637(18) 0.37377(15) 0.12945(10) 0.0196(4) Uani 1 1 d . . . H12S H 0.891(3) -0.180(3) 0.2126(19) 0.069(11) Uiso 1 1 d . . . C13 C 0.5381(2) 0.29754(16) 0.15243(12) 0.0239(4) Uani 1 1 d . . . C14 C 0.6738(2) 0.3313(2) 0.13591(14) 0.0305(5) Uani 1 1 d . . . C15 C 0.4749(2) 0.18823(18) 0.11298(15) 0.0341(5) Uani 1 1 d . . . C16 C 0.1914(2) 0.52621(16) 0.20448(12) 0.0240(4) Uani 1 1 d . . . C17 C 0.2314(3) 0.64468(18) 0.21983(15) 0.0339(5) Uani 1 1 d . . . C18 C 0.0359(2) 0.49674(19) 0.17237(14) 0.0311(5) Uani 1 1 d . . . C19 C 0.5892(3) 0.49970(19) 0.30159(14) 0.0317(5) Uani 1 1 d . . . C20 C 0.5789(2) 0.20355(18) 0.44871(12) 0.0245(4) Uani 1 1 d . . . C21 C 0.29976(17) 0.10941(14) 0.37590(10) 0.0175(4) Uani 1 1 d . . . C22 C 0.27141(18) 0.02229(15) 0.32231(11) 0.0197(4) Uani 1 1 d . . . C23 C 0.2170(2) -0.07277(16) 0.34091(12) 0.0250(4) Uani 1 1 d . . . C24 C 0.1901(2) -0.08049(17) 0.40989(13) 0.0293(5) Uani 1 1 d . . . C25 C 0.2174(2) 0.00633(17) 0.46134(12) 0.0276(5) Uani 1 1 d . . . C26 C 0.27233(18) 0.10340(15) 0.44641(10) 0.0209(4) Uani 1 1 d . . . C27 C 0.2965(2) 0.19621(17) 0.50584(11) 0.0254(4) Uani 1 1 d . . . C28 C 0.1605(2) 0.2229(2) 0.51577(14) 0.0332(5) Uani 1 1 d . . . C29 C 0.3901(3) 0.1763(2) 0.58292(13) 0.0349(5) Uani 1 1 d . . . C30 C 0.3071(2) 0.02838(16) 0.24795(11) 0.0217(4) Uani 1 1 d . . . C31 C 0.4532(2) 0.0054(2) 0.25925(15) 0.0359(6) Uani 1 1 d . . . C32 C 0.2066(2) -0.04325(18) 0.18197(13) 0.0302(5) Uani 1 1 d . . . N33 N 0.10391(15) 0.24187(12) 0.23110(8) 0.0171(3) Uani 1 1 d . . . C34 C -0.01207(18) 0.17605(14) 0.18631(10) 0.0169(4) Uani 1 1 d . . . C35 C -0.04234(18) 0.16269(14) 0.10643(10) 0.0184(4) Uani 1 1 d . . . C36 C -0.1567(2) 0.09298(16) 0.06537(11) 0.0230(4) Uani 1 1 d . . . C37 C -0.2394(2) 0.03644(16) 0.10050(12) 0.0264(5) Uani 1 1 d . . . C38 C -0.2111(2) 0.05113(15) 0.17879(12) 0.0243(4) Uani 1 1 d . . . C39 C -0.09977(18) 0.12086(15) 0.22302(11) 0.0199(4) Uani 1 1 d . . . C40 C -0.07534(19) 0.14307(16) 0.30769(11) 0.0234(4) Uani 1 1 d . . . C41 C -0.1249(2) 0.0507(2) 0.34513(15) 0.0360(6) Uani 1 1 d . . . C42 C -0.1403(2) 0.2393(2) 0.32393(13) 0.0319(5) Uani 1 1 d . . . C43 C 0.04509(19) 0.22284(15) 0.06436(11) 0.0204(4) Uani 1 1 d . . . C44 C -0.0388(2) 0.29128(19) 0.01067(13) 0.0296(5) Uani 1 1 d . . . C45 C 0.1076(2) 0.14982(18) 0.01964(13) 0.0285(5) Uani 1 1 d . . . O46 O 0.18173(13) 0.40316(10) 0.37075(7) 0.0241(3) Uani 1 1 d . . . S47 S 0.23118(5) 0.49625(4) 0.42808(3) 0.02438(12) Uani 1 1 d . . . O48 O 0.32779(15) 0.57040(12) 0.40945(9) 0.0368(4) Uani 1 1 d . . . O49 O 0.25901(15) 0.46806(11) 0.50352(8) 0.0328(4) Uani 1 1 d . . . C50 C 0.0758(2) 0.55752(18) 0.41290(12) 0.0327(5) Uani 1 1 d . . . F51 F -0.02910(13) 0.49154(11) 0.41790(7) 0.0419(3) Uani 1 1 d . . . F52 F 0.04282(15) 0.59265(13) 0.34542(8) 0.0563(4) Uani 1 1 d . . . F53 F 0.09759(14) 0.63824(10) 0.46525(8) 0.0465(4) Uani 1 1 d . . . C54S C 0.4444(3) -0.2082(3) 0.09359(17) 0.0436(6) Uani 1 1 d . . . C55A C 0.5742(8) -0.2609(9) 0.1256(5) 0.070(2) Uani 0.50 1 d P . . C55S C 0.5881(9) -0.2209(6) 0.1181(5) 0.044(2) Uiso 0.50 1 d P . . C56A C 0.6443(6) -0.2400(4) 0.2068(3) 0.0403(12) Uani 0.50 1 d P . . C56S C 0.6210(5) -0.3092(4) 0.1630(3) 0.0405(12) Uani 0.50 1 d P . . C57A C 0.7673(6) -0.3249(5) 0.1882(4) 0.0502(16) Uiso 0.50 1 d P . . C57S C 0.7763(6) -0.2896(5) 0.2311(4) 0.0428(13) Uani 0.50 1 d P . . C58A C 0.8641(12) -0.2359(9) 0.2391(8) 0.086(4) Uani 0.50 1 d P . . C58S C 0.8899(10) -0.2367(8) 0.2011(6) 0.053(2) Uani 0.50 1 d P . . H59 H 0.620(2) 0.3819(15) 0.4065(11) 0.021(5) Uiso 1 1 d . . . H60 H 0.183(2) 0.5575(15) 0.0644(11) 0.020(5) Uiso 1 1 d . . . H61 H 0.302(2) 0.4917(17) -0.0163(12) 0.033(6) Uiso 1 1 d . . . H62 H 0.4585(19) 0.3819(15) 0.0236(11) 0.019(5) Uiso 1 1 d . . . H63 H 0.5533(19) 0.2929(15) 0.2036(11) 0.018(5) Uiso 1 1 d . . . H64 H 0.714(2) 0.3993(18) 0.1616(12) 0.032(6) Uiso 1 1 d . . . H65 H 0.742(2) 0.2827(16) 0.1562(11) 0.029(6) Uiso 1 1 d . . . H66 H 0.663(2) 0.3309(16) 0.0811(13) 0.029(6) Uiso 1 1 d . . . H67 H 0.539(2) 0.1398(18) 0.1278(12) 0.039(6) Uiso 1 1 d . . . H68 H 0.400(3) 0.1653(19) 0.1308(13) 0.046(7) Uiso 1 1 d . . . H69 H 0.453(2) 0.1872(18) 0.0574(14) 0.041(7) Uiso 1 1 d . . . H70 H 0.218(2) 0.5007(16) 0.2522(12) 0.029(6) Uiso 1 1 d . . . H71 H 0.200(2) 0.6800(17) 0.1729(13) 0.033(6) Uiso 1 1 d . . . H72 H 0.187(2) 0.6768(18) 0.2575(13) 0.039(6) Uiso 1 1 d . . . H73 H 0.330(3) 0.663(2) 0.2400(15) 0.063(9) Uiso 1 1 d . . . H74 H 0.001(2) 0.5232(17) 0.1222(13) 0.035(6) Uiso 1 1 d . . . H75 H -0.009(2) 0.5276(18) 0.2051(13) 0.044(7) Uiso 1 1 d . . . H76 H 0.007(2) 0.4179(18) 0.1662(11) 0.028(6) Uiso 1 1 d . . . H77 H 0.638(3) 0.488(2) 0.2651(16) 0.067(9) Uiso 1 1 d . . . H78 H 0.539(3) 0.551(2) 0.2871(15) 0.055(8) Uiso 1 1 d . . . H79 H 0.650(3) 0.522(2) 0.3476(16) 0.055(8) Uiso 1 1 d . . . H80 H 0.664(2) 0.2046(17) 0.4372(12) 0.035(6) Uiso 1 1 d . . . H81 H 0.597(2) 0.2409(17) 0.4993(13) 0.036(6) Uiso 1 1 d . . . H82 H 0.549(2) 0.1345(18) 0.4526(12) 0.031(6) Uiso 1 1 d . . . H83 H 0.2021(19) -0.1352(16) 0.3050(11) 0.020(5) Uiso 1 1 d . . . H84 H 0.155(2) -0.1447(17) 0.4227(12) 0.032(6) Uiso 1 1 d . . . H85 H 0.199(2) 0.0005(16) 0.5071(12) 0.030(6) Uiso 1 1 d . . . H86 H 0.3366(18) 0.2573(14) 0.4891(10) 0.014(5) Uiso 1 1 d . . . H87 H 0.111(2) 0.1636(18) 0.5326(12) 0.039(7) Uiso 1 1 d . . . H88 H 0.178(2) 0.2842(18) 0.5536(13) 0.035(6) Uiso 1 1 d . . . H89 H 0.103(2) 0.2429(17) 0.4699(14) 0.039(7) Uiso 1 1 d . . . H90 H 0.345(2) 0.1222(19) 0.6078(13) 0.043(7) Uiso 1 1 d . . . H91 H 0.413(2) 0.2373(19) 0.6160(14) 0.041(7) Uiso 1 1 d . . . H92 H 0.474(3) 0.1523(19) 0.5786(14) 0.049(7) Uiso 1 1 d . . . H93 H 0.3053(19) 0.0989(15) 0.2347(10) 0.017(5) Uiso 1 1 d . . . H94 H 0.514(2) 0.0545(19) 0.2975(14) 0.042(7) Uiso 1 1 d . . . H95 H 0.477(2) 0.0097(18) 0.2140(14) 0.044(7) Uiso 1 1 d . . . H96 H 0.462(2) -0.066(2) 0.2744(13) 0.042(7) Uiso 1 1 d . . . H97 H 0.231(2) -0.0324(16) 0.1348(12) 0.027(6) Uiso 1 1 d . . . H98 H 0.211(2) -0.116(2) 0.1883(13) 0.046(7) Uiso 1 1 d . . . H99 H 0.112(3) -0.0278(18) 0.1743(13) 0.042(7) Uiso 1 1 d . . . H100 H -0.1751(19) 0.0836(14) 0.0140(11) 0.016(5) Uiso 1 1 d . . . H101 H -0.315(2) -0.0125(17) 0.0702(12) 0.039(6) Uiso 1 1 d . . . H102 H -0.269(2) 0.0133(15) 0.2043(11) 0.025(5) Uiso 1 1 d . . . H103 H 0.024(2) 0.1614(14) 0.3320(10) 0.017(5) Uiso 1 1 d . . . H104 H -0.089(2) -0.0140(18) 0.3331(12) 0.032(6) Uiso 1 1 d . . . H105 H -0.223(3) 0.0347(19) 0.3299(14) 0.053(8) Uiso 1 1 d . . . H106 H -0.097(2) 0.0690(18) 0.4005(15) 0.047(7) Uiso 1 1 d . . . H107 H -0.241(2) 0.2257(17) 0.3028(12) 0.039(6) Uiso 1 1 d . . . H108 H -0.120(2) 0.2612(18) 0.3776(14) 0.043(7) Uiso 1 1 d . . . H109 H -0.105(2) 0.3019(18) 0.3016(13) 0.041(7) Uiso 1 1 d . . . H110 H 0.115(2) 0.2672(15) 0.1002(11) 0.018(5) Uiso 1 1 d . . . H111 H -0.084(2) 0.3387(18) 0.0367(13) 0.040(7) Uiso 1 1 d . . . H112 H -0.106(3) 0.2453(19) -0.0314(14) 0.046(7) Uiso 1 1 d . . . H113 H 0.018(2) 0.3340(17) -0.0146(12) 0.031(6) Uiso 1 1 d . . . H114 H 0.160(2) 0.1016(17) 0.0524(12) 0.034(6) Uiso 1 1 d . . . H115 H 0.038(2) 0.1030(18) -0.0182(13) 0.038(6) Uiso 1 1 d . . . H116 H 0.168(2) 0.1899(17) -0.0055(12) 0.035(6) 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 0.01491(16) 0.01706(18) 0.01433(17) 0.00446(13) 0.00456(13) 0.00354(13) N2 0.0165(8) 0.0172(8) 0.0170(8) 0.0048(6) 0.0044(6) 0.0034(6) C3 0.0189(9) 0.0195(10) 0.0191(9) 0.0023(8) 0.0049(8) 0.0014(8) C4 0.0185(9) 0.0239(11) 0.0162(9) 0.0025(8) 0.0002(8) -0.0025(8) C5 0.0186(9) 0.0228(10) 0.0140(9) 0.0013(8) 0.0049(7) 0.0032(8) N6 0.0147(7) 0.0182(8) 0.0153(8) 0.0046(6) 0.0032(6) 0.0021(6) C7 0.0185(9) 0.0160(9) 0.0160(9) 0.0047(7) 0.0042(7) -0.0008(7) C8 0.0190(9) 0.0184(10) 0.0225(10) 0.0054(8) 0.0072(8) 0.0023(7) C9 0.0224(10) 0.0232(11) 0.0281(11) 0.0119(9) 0.0061(9) 0.0070(8) C10 0.0258(10) 0.0304(12) 0.0188(10) 0.0115(9) 0.0052(9) 0.0027(9) C11 0.0245(10) 0.0296(11) 0.0228(10) 0.0074(9) 0.0108(9) 0.0068(9) C12 0.0176(9) 0.0215(10) 0.0204(10) 0.0060(8) 0.0058(8) 0.0026(8) C13 0.0233(10) 0.0333(12) 0.0200(10) 0.0108(9) 0.0088(8) 0.0126(9) C14 0.0229(11) 0.0381(14) 0.0332(13) 0.0088(11) 0.0096(10) 0.0090(10) C15 0.0306(12) 0.0296(13) 0.0476(16) 0.0127(11) 0.0154(12) 0.0116(10) C16 0.0287(11) 0.0229(11) 0.0256(11) 0.0093(9) 0.0119(9) 0.0107(9) C17 0.0422(14) 0.0256(12) 0.0379(14) 0.0051(10) 0.0163(12) 0.0083(11) C18 0.0277(11) 0.0331(13) 0.0386(14) 0.0087(11) 0.0155(10) 0.0116(10) C19 0.0325(12) 0.0291(13) 0.0264(12) 0.0092(10) 0.0006(11) -0.0086(10) C20 0.0180(10) 0.0283(12) 0.0251(11) 0.0096(9) 0.0019(9) 0.0023(9) C21 0.0131(8) 0.0198(10) 0.0197(9) 0.0096(8) 0.0026(7) 0.0033(7) C22 0.0150(9) 0.0210(10) 0.0227(10) 0.0079(8) 0.0028(8) 0.0036(7) C23 0.0250(10) 0.0199(11) 0.0286(11) 0.0054(9) 0.0048(9) 0.0029(8) C24 0.0265(11) 0.0244(11) 0.0373(13) 0.0160(10) 0.0082(10) 0.0004(9) C25 0.0279(11) 0.0336(12) 0.0251(11) 0.0160(10) 0.0101(9) 0.0065(9) C26 0.0166(9) 0.0263(11) 0.0200(10) 0.0084(8) 0.0032(8) 0.0060(8) C27 0.0286(11) 0.0315(12) 0.0174(10) 0.0077(9) 0.0079(8) 0.0042(9) C28 0.0365(13) 0.0384(14) 0.0277(12) 0.0065(11) 0.0116(11) 0.0103(11) C29 0.0369(14) 0.0459(16) 0.0203(11) 0.0085(11) 0.0049(10) 0.0057(12) C30 0.0247(10) 0.0182(10) 0.0221(10) 0.0041(8) 0.0057(8) 0.0038(8) C31 0.0278(12) 0.0526(17) 0.0304(13) 0.0064(12) 0.0118(11) 0.0084(11) C32 0.0358(13) 0.0263(12) 0.0246(12) 0.0010(9) 0.0024(10) 0.0054(10) N33 0.0172(8) 0.0191(8) 0.0166(8) 0.0056(6) 0.0059(6) 0.0047(6) C34 0.0155(9) 0.0143(9) 0.0219(10) 0.0043(7) 0.0043(7) 0.0072(7) C35 0.0172(9) 0.0178(9) 0.0208(10) 0.0044(8) 0.0043(8) 0.0067(7) C36 0.0235(10) 0.0262(11) 0.0177(10) 0.0006(8) 0.0031(8) 0.0045(8) C37 0.0203(10) 0.0231(11) 0.0326(12) -0.0022(9) 0.0050(9) 0.0000(8) C38 0.0190(10) 0.0213(10) 0.0341(12) 0.0074(9) 0.0096(9) 0.0016(8) C39 0.0161(9) 0.0214(10) 0.0244(10) 0.0072(8) 0.0064(8) 0.0076(8) C40 0.0151(9) 0.0328(12) 0.0235(10) 0.0101(9) 0.0058(8) 0.0040(8) C41 0.0266(12) 0.0495(16) 0.0338(14) 0.0218(12) 0.0092(11) 0.0024(11) C42 0.0292(12) 0.0456(15) 0.0233(12) 0.0027(10) 0.0095(10) 0.0108(10) C43 0.0201(10) 0.0215(10) 0.0170(10) 0.0030(8) 0.0019(8) 0.0005(8) C44 0.0307(12) 0.0318(13) 0.0267(12) 0.0114(10) 0.0060(10) 0.0076(10) C45 0.0284(12) 0.0321(13) 0.0275(12) 0.0047(10) 0.0109(10) 0.0069(10) O46 0.0253(7) 0.0262(8) 0.0221(7) 0.0003(6) 0.0082(6) 0.0063(6) S47 0.0265(3) 0.0251(3) 0.0222(3) -0.0007(2) 0.0084(2) 0.0045(2) O48 0.0364(9) 0.0322(9) 0.0430(9) -0.0008(7) 0.0176(7) -0.0026(7) O49 0.0403(9) 0.0357(9) 0.0194(7) -0.0011(6) 0.0045(7) 0.0058(7) C50 0.0385(13) 0.0362(13) 0.0290(12) 0.0044(10) 0.0157(10) 0.0125(10) F51 0.0299(7) 0.0508(9) 0.0464(8) -0.0061(7) 0.0159(6) 0.0057(6) F52 0.0639(10) 0.0783(11) 0.0434(9) 0.0280(8) 0.0233(8) 0.0449(9) F53 0.0546(9) 0.0336(8) 0.0587(9) -0.0064(7) 0.0281(7) 0.0137(7) C54S 0.0379(14) 0.0522(18) 0.0418(16) 0.0039(14) 0.0134(13) 0.0072(13) C55A 0.038(4) 0.093(8) 0.073(5) 0.029(6) 0.003(3) 0.005(5) C56A 0.043(3) 0.039(3) 0.044(3) 0.009(3) 0.022(3) 0.002(2) C56S 0.039(3) 0.026(3) 0.046(3) 0.008(3) -0.005(2) 0.000(2) C57S 0.033(3) 0.054(4) 0.046(4) 0.026(3) 0.013(3) 0.011(3) C58A 0.049(7) 0.041(5) 0.141(12) 0.030(7) -0.023(6) 0.004(5) C58S 0.031(4) 0.024(4) 0.100(8) 0.015(5) 0.013(4) 0.003(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 N33 1.7049(15) . ? Ti1 N2 1.9783(15) . ? Ti1 O46 1.9991(13) . ? Ti1 N6 2.0289(15) . ? N2 C3 1.365(2) . ? N2 C7 1.438(2) . ? C3 C4 1.388(3) . ? C3 C19 1.501(3) . ? C4 C5 1.421(3) . ? C5 N6 1.330(2) . ? C5 C20 1.500(3) . ? N6 C21 1.453(2) . ? C7 C8 1.407(3) . ? C7 C12 1.408(3) . ? C8 C9 1.396(3) . ? C8 C16 1.518(3) . ? C9 C10 1.374(3) . ? C10 C11 1.384(3) . ? C11 C12 1.393(3) . ? C12 C13 1.518(3) . ? C13 C14 1.528(3) . ? C13 C15 1.530(3) . ? C16 C17 1.528(3) . ? C16 C18 1.532(3) . ? C21 C22 1.397(3) . ? C21 C26 1.410(3) . ? C22 C23 1.395(3) . ? C22 C30 1.520(3) . ? C23 C24 1.383(3) . ? C24 C25 1.372(3) . ? C25 C26 1.393(3) . ? C26 C27 1.521(3) . ? C27 C28 1.535(3) . ? C27 C29 1.537(3) . ? C30 C31 1.525(3) . ? C30 C32 1.528(3) . ? N33 C34 1.396(2) . ? C34 C35 1.414(3) . ? C34 C39 1.425(2) . ? C35 C36 1.390(3) . ? C35 C43 1.522(3) . ? C36 C37 1.378(3) . ? C37 C38 1.388(3) . ? C38 C39 1.388(3) . ? C39 C40 1.514(3) . ? C40 C41 1.525(3) . ? C40 C42 1.534(3) . ? C43 C45 1.525(3) . ? C43 C44 1.529(3) . ? O46 S47 1.4901(14) . ? S47 O49 1.4227(15) . ? S47 O48 1.4252(15) . ? S47 C50 1.828(2) . ? C50 F51 1.322(2) . ? C50 F52 1.323(2) . ? C50 F53 1.330(2) . ? C54S C55S 1.453(9) . ? C54S C55A 1.558(9) . ? C55A C55S 0.558(11) . ? C55A C56S 1.022(9) . ? C55A C56A 1.463(10) . ? C55S C56S 1.473(8) . ? C55S C56A 1.624(10) . ? C56A C56S 1.123(7) . ? C56A C57S 1.537(7) . ? C56A C57A 1.859(9) . ? C56S C57A 1.488(8) . ? C56S C57S 1.714(8) . ? C57A C57S 0.865(7) . ? C57A C58A 1.506(14) . ? C57A C58S 1.550(12) . ? C57S C58A 1.040(11) . ? C57S C58S 1.533(10) . ? C58A C58S 0.814(15) . ? 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 N33 Ti1 N2 110.31(7) . . ? N33 Ti1 O46 111.46(6) . . ? N2 Ti1 O46 119.46(6) . . ? N33 Ti1 N6 108.06(7) . . ? N2 Ti1 N6 97.10(6) . . ? O46 Ti1 N6 109.07(6) . . ? C3 N2 C7 119.92(15) . . ? C3 N2 Ti1 106.63(11) . . ? C7 N2 Ti1 130.58(12) . . ? N2 C3 C4 122.88(17) . . ? N2 C3 C19 119.33(17) . . ? C4 C3 C19 117.78(17) . . ? C3 C4 C5 131.72(18) . . ? N6 C5 C4 122.10(17) . . ? N6 C5 C20 122.45(17) . . ? C4 C5 C20 115.45(16) . . ? C5 N6 C21 121.10(15) . . ? C5 N6 Ti1 111.22(12) . . ? C21 N6 Ti1 126.05(11) . . ? C8 C7 C12 121.19(16) . . ? C8 C7 N2 119.40(16) . . ? C12 C7 N2 119.34(16) . . ? C9 C8 C7 118.08(18) . . ? C9 C8 C16 118.81(17) . . ? C7 C8 C16 123.08(17) . . ? C10 C9 C8 121.58(19) . . ? C9 C10 C11 119.57(19) . . ? C10 C11 C12 121.65(19) . . ? C11 C12 C7 117.90(17) . . ? C11 C12 C13 119.19(17) . . ? C7 C12 C13 122.87(16) . . ? C12 C13 C14 112.74(17) . . ? C12 C13 C15 109.99(17) . . ? C14 C13 C15 110.37(18) . . ? C8 C16 C17 111.12(17) . . ? C8 C16 C18 112.00(18) . . ? C17 C16 C18 110.97(18) . . ? C22 C21 C26 121.77(17) . . ? C22 C21 N6 118.07(16) . . ? C26 C21 N6 120.11(17) . . ? C23 C22 C21 118.04(18) . . ? C23 C22 C30 120.45(18) . . ? C21 C22 C30 121.38(16) . . ? C24 C23 C22 121.1(2) . . ? C25 C24 C23 119.84(19) . . ? C24 C25 C26 121.9(2) . . ? C25 C26 C21 117.33(19) . . ? C25 C26 C27 118.53(18) . . ? C21 C26 C27 124.13(17) . . ? C26 C27 C28 110.92(18) . . ? C26 C27 C29 111.91(18) . . ? C28 C27 C29 109.34(18) . . ? C22 C30 C31 109.18(17) . . ? C22 C30 C32 113.39(17) . . ? C31 C30 C32 111.18(19) . . ? C34 N33 Ti1 170.47(13) . . ? N33 C34 C35 121.45(16) . . ? N33 C34 C39 118.42(16) . . ? C35 C34 C39 120.13(16) . . ? C36 C35 C34 118.54(17) . . ? C36 C35 C43 119.31(17) . . ? C34 C35 C43 122.14(16) . . ? C37 C36 C35 121.78(19) . . ? C36 C37 C38 119.60(19) . . ? C37 C38 C39 121.47(18) . . ? C38 C39 C34 118.41(17) . . ? C38 C39 C40 121.38(17) . . ? C34 C39 C40 120.12(16) . . ? C39 C40 C41 114.09(18) . . ? C39 C40 C42 109.61(16) . . ? C41 C40 C42 110.79(19) . . ? C35 C43 C45 111.70(16) . . ? C35 C43 C44 110.91(16) . . ? C45 C43 C44 109.44(17) . . ? S47 O46 Ti1 142.36(9) . . ? O49 S47 O48 119.16(9) . . ? O49 S47 O46 111.94(8) . . ? O48 S47 O46 112.61(8) . . ? O49 S47 C50 105.05(10) . . ? O48 S47 C50 104.98(10) . . ? O46 S47 C50 100.76(9) . . ? F51 C50 F52 108.38(19) . . ? F51 C50 F53 108.50(17) . . ? F52 C50 F53 108.09(18) . . ? F51 C50 S47 111.62(15) . . ? F52 C50 S47 111.03(15) . . ? F53 C50 S47 109.13(15) . . ? C55S C54S C55A 21.0(4) . . ? C55S C55A C56S 135.7(19) . . ? C55S C55A C56A 96.5(18) . . ? C56S C55A C56A 50.0(5) . . ? C55S C55A C54S 68.8(15) . . ? C56S C55A C54S 147.1(8) . . ? C56A C55A C54S 117.7(7) . . ? C55A C55S C54S 90.2(16) . . ? C55A C55S C56S 29.0(13) . . ? C54S C55S C56S 115.8(6) . . ? C55A C55S C56A 63.6(15) . . ? C54S C55S C56A 114.3(6) . . ? C56S C55S C56A 42.2(3) . . ? C56S C56A C55A 44.2(5) . . ? C56S C56A C57S 78.5(5) . . ? C55A C56A C57S 113.2(6) . . ? C56S C56A C55S 61.7(5) . . ? C55A C56A C55S 20.0(5) . . ? C57S C56A C55S 117.4(5) . . ? C56S C56A C57A 53.2(4) . . ? C55A C56A C57A 85.9(5) . . ? C57S C56A C57A 27.5(3) . . ? C55S C56A C57A 92.8(5) . . ? C55A C56S C56A 85.9(7) . . ? C55A C56S C55S 15.3(7) . . ? C56A C56S C55S 76.1(5) . . ? C55A C56S C57A 129.9(7) . . ? C56A C56S C57A 89.6(5) . . ? C55S C56S C57A 117.1(6) . . ? C55A C56S C57S 131.0(7) . . ? C56A C56S C57S 61.5(5) . . ? C55S C56S C57S 115.7(5) . . ? C57A C56S C57S 30.3(3) . . ? C57S C57A C56S 89.4(7) . . ? C57S C57A C58A 42.1(7) . . ? C56S C57A C58A 115.6(7) . . ? C57S C57A C58S 72.7(7) . . ? C56S C57A C58S 124.3(6) . . ? C58A C57A C58S 30.8(6) . . ? C57S C57A C56A 55.1(6) . . ? C56S C57A C56A 37.2(3) . . ? C58A C57A C56A 79.2(6) . . ? C58S C57A C56A 96.4(5) . . ? C57A C57S C58A 104.1(11) . . ? C57A C57S C58S 74.8(7) . . ? C58A C57S C58S 29.7(10) . . ? C57A C57S C56A 97.4(7) . . ? C58A C57S C56A 112.7(8) . . ? C58S C57S C56A 112.2(6) . . ? C57A C57S C56S 60.3(6) . . ? C58A C57S C56S 132.3(8) . . ? C58S C57S C56S 111.5(6) . . ? C56A C57S C56S 40.0(3) . . ? C58S C58A C57S 111(2) . . ? C58S C58A C57A 77.6(16) . . ? C57S C58A C57A 33.8(6) . . ? C58A C58S C57S 39.3(12) . . ? C58A C58S C57A 71.6(13) . . ? C57S C58S C57A 32.6(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.60 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.562 _refine_diff_density_min -0.303 _refine_diff_density_rms 0.054 data_03054 _database_code_CSD 209463 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _exptl_crystal_id MSC03054 _audit_creation_date 10/27/2002 _chemical_formula_structural '[Ti(C29H41N2)(NHC6H3iPr2)2]+ [B(C6F5)4]- Et2O' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C81 H87 B F20 N4 O Ti' _chemical_formula_weight 1571.26 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 Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.8639(6) _cell_length_b 39.2661(16) _cell_length_c 13.9675(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.2700(10) _cell_angle_gamma 90.00 _cell_volume 7591.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 136(2) _cell_measurement_reflns_used 7190 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.44 _exptl_crystal_description plate _exptl_crystal_colour orange/red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3264 _exptl_absorpt_coefficient_mu 0.210 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9396 _exptl_absorpt_correction_T_max 0.9691 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 136(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_details ' 0.30 degree frames measured for 15.14 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 111677 _diffrn_reflns_av_R_equivalents 0.1095 _diffrn_reflns_av_sigmaI/netI 0.0941 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -51 _diffrn_reflns_limit_k_max 50 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.55 _reflns_number_total 17467 _reflns_number_gt 9392 _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 ? _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^)+(0.0422P)^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 17467 _refine_ls_number_parameters 1321 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1144 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1116 _refine_ls_wR_factor_gt 0.0883 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.962 _refine_ls_shift/su_max 0.020 _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 0.05060(3) 0.116645(11) 0.25898(3) 0.01632(10) Uani 1 1 d . . . N2 N 0.05595(14) 0.07043(5) 0.19682(13) 0.0166(4) Uani 1 1 d . . . C3 C -0.02560(17) 0.05597(6) 0.15952(16) 0.0174(5) Uani 1 1 d . . . C4 C -0.11165(18) 0.07482(6) 0.14407(17) 0.0194(5) Uani 1 1 d . . . C5 C -0.12606(17) 0.10972(6) 0.14160(16) 0.0191(5) Uani 1 1 d . . . N6 N -0.05541(14) 0.13248(5) 0.16794(13) 0.0163(4) Uani 1 1 d . . . C7 C 0.14690(17) 0.05190(6) 0.19739(17) 0.0173(5) Uani 1 1 d . . . C8 C 0.21106(18) 0.05998(6) 0.12689(17) 0.0203(5) Uani 1 1 d . . . C9 C 0.29928(19) 0.04333(6) 0.1293(2) 0.0252(6) Uani 1 1 d . . . C10 C 0.3243(2) 0.02001(7) 0.20015(19) 0.0258(6) Uani 1 1 d . . . C11 C 0.26033(19) 0.01222(7) 0.26828(19) 0.0242(6) Uani 1 1 d . . . C12 C 0.17005(18) 0.02763(6) 0.26872(17) 0.0215(6) Uani 1 1 d . . . C13 C 0.1005(2) 0.01691(7) 0.34334(19) 0.0307(7) Uani 1 1 d . . . C14 C 0.1338(3) 0.02998(10) 0.4425(2) 0.0431(8) Uani 1 1 d . . . C15 C 0.0859(3) -0.02158(8) 0.3440(3) 0.0413(8) Uani 1 1 d . . . C16 C 0.18431(19) 0.08545(7) 0.04816(19) 0.0253(6) Uani 1 1 d . . . C17 C 0.2671(2) 0.10941(8) 0.0277(3) 0.0357(7) Uani 1 1 d . . . C18 C 0.1434(3) 0.06801(8) -0.0427(2) 0.0353(7) Uani 1 1 d . . . C19 C -0.0283(2) 0.01911(7) 0.1311(2) 0.0255(6) Uani 1 1 d . . . C20 C -0.2246(2) 0.12275(8) 0.1081(2) 0.0252(6) Uani 1 1 d . . . C21 C -0.06831(17) 0.16812(6) 0.14193(17) 0.0182(5) Uani 1 1 d . . . C22 C -0.03429(17) 0.17902(6) 0.05361(17) 0.0215(6) Uani 1 1 d . . . C23 C -0.04553(19) 0.21318(7) 0.0302(2) 0.0267(6) Uani 1 1 d . . . C24 C -0.0867(2) 0.23594(7) 0.0911(2) 0.0281(6) Uani 1 1 d . . . C25 C -0.12006(19) 0.22480(7) 0.17658(19) 0.0238(6) Uani 1 1 d . . . C26 C -0.11283(17) 0.19083(6) 0.20367(17) 0.0202(5) Uani 1 1 d . . . C27 C -0.15608(19) 0.17998(7) 0.29680(18) 0.0248(6) Uani 1 1 d . . . C28 C -0.2634(2) 0.18963(8) 0.2964(2) 0.0337(7) Uani 1 1 d . . . C29 C -0.1008(2) 0.19524(8) 0.3844(2) 0.0321(7) Uani 1 1 d . . . C30 C 0.01083(19) 0.15462(7) -0.01554(18) 0.0250(6) Uani 1 1 d . . . C31 C -0.0645(2) 0.13626(9) -0.0811(2) 0.0377(8) Uani 1 1 d . . . C32 C 0.0842(2) 0.17134(9) -0.0773(2) 0.0379(8) Uani 1 1 d . . . N33 N 0.16881(17) 0.13871(6) 0.25084(17) 0.0238(5) Uani 1 1 d . . . C34 C 0.23148(19) 0.15657(6) 0.32068(18) 0.0261(6) Uani 1 1 d . . . C35 C 0.21430(19) 0.19147(7) 0.33636(19) 0.0283(6) Uani 1 1 d . . . C36 C 0.2695(2) 0.20756(8) 0.4090(2) 0.0391(8) Uani 1 1 d . . . C37 C 0.3391(3) 0.19013(8) 0.4635(3) 0.0518(10) Uani 1 1 d . . . C38 C 0.3575(3) 0.15681(8) 0.4449(3) 0.0531(10) Uani 1 1 d . . . C39 C 0.3048(2) 0.13898(7) 0.3726(2) 0.0385(8) Uani 1 1 d . . . C40 C 0.3359(3) 0.10313(8) 0.3486(2) 0.0463(9) Uani 1 1 d . . . C41 C 0.4235(3) 0.10473(11) 0.2875(4) 0.0703(13) Uani 1 1 d . . . C42 C 0.3559(5) 0.08093(10) 0.4373(4) 0.0824(18) Uani 1 1 d . . . C43 C 0.1451(2) 0.21138(7) 0.2703(2) 0.0295(7) Uani 1 1 d . . . C44 C 0.1927(3) 0.21928(9) 0.1769(2) 0.0397(8) Uani 1 1 d . . . C45 C 0.1084(2) 0.24423(8) 0.3139(3) 0.0388(8) Uani 1 1 d . . . N46 N 0.02677(17) 0.11675(6) 0.38977(15) 0.0234(5) Uani 1 1 d . . . C47 C -0.02835(19) 0.11695(6) 0.47185(17) 0.0226(6) Uani 1 1 d . . . C48 C 0.0103(2) 0.13228(7) 0.55753(18) 0.0304(7) Uani 1 1 d . . . C49 C -0.0461(3) 0.13174(8) 0.6365(2) 0.0378(8) Uani 1 1 d . . . C50 C -0.1361(3) 0.11724(8) 0.6338(2) 0.0413(8) Uani 1 1 d . . . C51 C -0.1737(2) 0.10292(8) 0.5492(2) 0.0345(7) Uani 1 1 d . . . C52 C -0.1215(2) 0.10228(6) 0.46730(18) 0.0254(6) Uani 1 1 d . . . C53 C -0.1623(2) 0.08417(7) 0.3787(2) 0.0272(6) Uani 1 1 d . . . C54 C -0.2691(2) 0.09199(9) 0.3541(3) 0.0410(8) Uani 1 1 d . . . C55 C -0.1484(2) 0.04593(7) 0.3911(2) 0.0326(7) Uani 1 1 d . . . C56 C 0.1106(2) 0.14741(8) 0.5684(2) 0.0379(8) Uani 1 1 d . . . C57 C 0.1120(4) 0.18283(10) 0.6139(3) 0.0578(10) Uani 1 1 d . . . C58 C 0.1779(4) 0.12307(13) 0.6258(4) 0.0743(14) Uani 1 1 d . . . B59 B 0.5439(2) 0.10509(7) 0.8125(2) 0.0193(6) Uani 1 1 d . . . C60 C 0.48079(17) 0.07698(6) 0.74729(17) 0.0209(6) Uani 1 1 d . . . C61 C 0.38337(18) 0.06912(7) 0.75136(18) 0.0247(6) Uani 1 1 d . . . C62 C 0.33899(19) 0.04212(7) 0.7022(2) 0.0305(7) Uani 1 1 d . . . C63 C 0.3920(2) 0.02128(7) 0.6476(2) 0.0334(7) Uani 1 1 d . . . C64 C 0.48925(19) 0.02752(7) 0.64100(19) 0.0272(6) Uani 1 1 d . . . C65 C 0.52962(18) 0.05491(6) 0.68986(18) 0.0229(6) Uani 1 1 d . . . F66 F 0.32543(10) 0.08761(4) 0.80593(10) 0.0297(4) Uani 1 1 d . . . F67 F 0.24410(11) 0.03608(4) 0.71053(13) 0.0456(5) Uani 1 1 d . . . F68 F 0.35066(12) -0.00537(4) 0.60049(13) 0.0513(5) Uani 1 1 d . . . F69 F 0.54326(11) 0.00706(4) 0.58889(11) 0.0392(4) Uani 1 1 d . . . F70 F 0.62574(10) 0.05964(4) 0.68002(10) 0.0258(3) Uani 1 1 d . . . C71 C 0.47911(17) 0.13303(6) 0.86878(18) 0.0200(5) Uani 1 1 d . . . C72 C 0.41229(17) 0.15308(6) 0.81588(18) 0.0220(6) Uani 1 1 d . . . C73 C 0.36011(19) 0.17922(7) 0.8526(2) 0.0278(6) Uani 1 1 d . . . C74 C 0.37374(19) 0.18736(6) 0.9475(2) 0.0279(6) Uani 1 1 d . . . C75 C 0.43942(19) 0.16913(6) 1.00387(19) 0.0256(6) Uani 1 1 d . . . C76 C 0.49019(18) 0.14290(6) 0.96424(18) 0.0214(6) Uani 1 1 d . . . F77 F 0.39764(10) 0.14707(4) 0.72055(10) 0.0289(4) Uani 1 1 d . . . F78 F 0.29635(11) 0.19706(4) 0.79597(12) 0.0387(4) Uani 1 1 d . . . F79 F 0.32393(12) 0.21299(4) 0.98572(12) 0.0398(4) Uani 1 1 d . . . F80 F 0.45402(12) 0.17685(4) 1.09769(11) 0.0365(4) Uani 1 1 d . . . F81 F 0.55406(10) 0.12680(3) 1.02609(10) 0.0272(3) Uani 1 1 d . . . C82 C 0.60686(17) 0.07935(6) 0.88626(17) 0.0178(5) Uani 1 1 d . . . C83 C 0.55861(17) 0.06061(6) 0.95290(17) 0.0186(5) Uani 1 1 d . . . C84 C 0.60068(18) 0.03648(6) 1.01353(18) 0.0220(6) Uani 1 1 d . . . C85 C 0.69705(19) 0.02903(6) 1.00643(18) 0.0223(6) Uani 1 1 d . . . C86 C 0.74823(17) 0.04577(6) 0.93999(18) 0.0202(5) Uani 1 1 d . . . C87 C 0.70349(17) 0.07036(6) 0.88235(17) 0.0184(5) Uani 1 1 d . . . F88 F 0.46274(10) 0.06576(3) 0.96127(10) 0.0257(3) Uani 1 1 d . . . F89 F 0.54911(11) 0.02015(4) 1.07856(10) 0.0298(4) Uani 1 1 d . . . F90 F 0.73973(11) 0.00534(4) 1.06431(10) 0.0311(4) Uani 1 1 d . . . F91 F 0.84169(10) 0.03804(4) 0.92984(10) 0.0285(4) Uani 1 1 d . . . F92 F 0.76021(9) 0.08559(3) 0.81977(10) 0.0234(3) Uani 1 1 d . . . C93 C 0.61012(17) 0.13058(6) 0.74848(17) 0.0194(5) Uani 1 1 d . . . C94 C 0.59718(18) 0.13626(6) 0.65077(18) 0.0227(6) Uani 1 1 d . . . C95 C 0.6450(2) 0.16140(7) 0.60265(18) 0.0275(6) Uani 1 1 d . . . C96 C 0.70833(19) 0.18246(6) 0.6521(2) 0.0288(6) Uani 1 1 d . . . C97 C 0.72360(18) 0.17819(6) 0.74919(19) 0.0258(6) Uani 1 1 d . . . C98 C 0.67513(18) 0.15288(6) 0.79396(17) 0.0209(5) Uani 1 1 d . . . F99 F 0.53521(10) 0.11708(4) 0.59482(10) 0.0297(4) Uani 1 1 d . . . F100 F 0.62904(12) 0.16496(4) 0.50708(11) 0.0407(4) Uani 1 1 d . . . F101 F 0.75619(12) 0.20651(4) 0.60583(12) 0.0426(4) Uani 1 1 d . . . F102 F 0.78649(11) 0.19884(4) 0.79836(11) 0.0358(4) Uani 1 1 d . . . F103 F 0.69246(10) 0.15011(3) 0.89017(10) 0.0255(3) Uani 1 1 d . . . C104 C 0.6588(3) 0.22307(11) 0.9995(3) 0.0606(11) Uani 1 1 d . . . C105 C 0.5836(3) 0.24477(9) 0.9468(3) 0.0515(9) Uani 1 1 d . . . O106 O 0.57178(16) 0.23287(6) 0.84984(16) 0.0525(6) Uani 1 1 d . . . C107 C 0.5000(3) 0.25207(9) 0.7940(3) 0.0502(9) Uani 1 1 d . . . C108 C 0.4915(3) 0.23756(11) 0.6948(3) 0.0575(10) Uani 1 1 d . . . H109 H -0.1643(17) 0.0620(6) 0.1272(16) 0.018(6) Uiso 1 1 d . . . H110 H 0.3444(18) 0.0487(6) 0.0814(18) 0.023(7) Uiso 1 1 d . . . H111 H 0.3829(18) 0.0087(6) 0.2002(16) 0.017(6) Uiso 1 1 d . . . H112 H 0.2760(18) -0.0040(6) 0.3175(18) 0.027(7) Uiso 1 1 d . . . H113 H 0.0402(19) 0.0279(7) 0.3292(18) 0.030(7) Uiso 1 1 d . . . H114 H 0.198(2) 0.0217(7) 0.4630(18) 0.029(7) Uiso 1 1 d . . . H115 H 0.1469(19) 0.0545(7) 0.4469(18) 0.030(8) Uiso 1 1 d . . . H116 H 0.084(3) 0.0250(9) 0.490(3) 0.072(12) Uiso 1 1 d . . . H117 H 0.143(2) -0.0336(7) 0.368(2) 0.046(9) Uiso 1 1 d . . . H118 H 0.070(2) -0.0313(8) 0.274(2) 0.053(9) Uiso 1 1 d . . . H119 H 0.033(2) -0.0283(8) 0.386(2) 0.060(10) Uiso 1 1 d . . . H120 H 0.1351(17) 0.0996(6) 0.0722(16) 0.017(6) Uiso 1 1 d . . . H121 H 0.291(2) 0.1204(8) 0.089(2) 0.053(10) Uiso 1 1 d . . . H122 H 0.320(2) 0.0960(7) -0.001(2) 0.043(8) Uiso 1 1 d . . . H123 H 0.245(2) 0.1266(8) -0.017(2) 0.051(9) Uiso 1 1 d . . . H124 H 0.192(2) 0.0530(7) -0.066(2) 0.041(9) Uiso 1 1 d . . . H125 H 0.125(2) 0.0838(8) -0.096(2) 0.050(9) Uiso 1 1 d . . . H126 H 0.093(2) 0.0535(7) -0.0313(19) 0.032(8) Uiso 1 1 d . . . H127 H 0.037(2) 0.0092(7) 0.1252(19) 0.043(8) Uiso 1 1 d . . . H128 H -0.059(2) 0.0170(7) 0.072(2) 0.051(9) Uiso 1 1 d . . . H129 H -0.059(2) 0.0053(8) 0.179(2) 0.050(9) Uiso 1 1 d . . . H130 H -0.224(2) 0.1406(8) 0.064(2) 0.048(9) Uiso 1 1 d . . . H131 H -0.259(2) 0.1303(7) 0.165(2) 0.042(9) Uiso 1 1 d . . . H132 H -0.260(2) 0.1040(8) 0.078(2) 0.050(9) Uiso 1 1 d . . . H133 H -0.0235(16) 0.2206(6) -0.0267(17) 0.012(6) Uiso 1 1 d . . . H134 H -0.0899(17) 0.2592(6) 0.0767(17) 0.022(7) Uiso 1 1 d . . . H135 H -0.1471(17) 0.2404(6) 0.2193(17) 0.017(6) Uiso 1 1 d . . . H136 H -0.1522(16) 0.1571(6) 0.3018(15) 0.012(6) Uiso 1 1 d . . . H137 H -0.2694(19) 0.2133(7) 0.2974(18) 0.031(8) Uiso 1 1 d . . . H138 H -0.294(2) 0.1811(7) 0.353(2) 0.045(9) Uiso 1 1 d . . . H139 H -0.3003(19) 0.1804(7) 0.237(2) 0.033(8) Uiso 1 1 d . . . H140 H -0.106(2) 0.2197(7) 0.3838(19) 0.038(8) Uiso 1 1 d . . . H141 H -0.1305(19) 0.1875(7) 0.443(2) 0.031(8) Uiso 1 1 d . . . H142 H -0.031(2) 0.1885(7) 0.3860(18) 0.032(8) Uiso 1 1 d . . . H143 H 0.0388(17) 0.1368(6) 0.0198(17) 0.018(6) Uiso 1 1 d . . . H144 H -0.111(2) 0.1222(8) -0.049(2) 0.054(10) Uiso 1 1 d . . . H145 H -0.099(2) 0.1554(8) -0.115(2) 0.048(9) Uiso 1 1 d . . . H146 H -0.030(2) 0.1206(7) -0.126(2) 0.047(9) Uiso 1 1 d . . . H147 H 0.128(2) 0.1842(8) -0.036(2) 0.046(9) Uiso 1 1 d . . . H148 H 0.051(2) 0.1885(8) -0.123(2) 0.056(10) Uiso 1 1 d . . . H149 H 0.122(2) 0.1547(7) -0.113(2) 0.040(8) Uiso 1 1 d . . . H150 H 0.177(3) 0.1419(10) 0.199(3) 0.084(16) Uiso 1 1 d . . . H151 H 0.261(2) 0.2303(7) 0.4240(19) 0.036(8) Uiso 1 1 d . . . H152 H 0.377(2) 0.2016(8) 0.515(2) 0.063(10) Uiso 1 1 d . . . H153 H 0.408(2) 0.1465(8) 0.476(2) 0.059(11) Uiso 1 1 d . . . H154 H 0.285(2) 0.0922(7) 0.3132(18) 0.032(8) Uiso 1 1 d . . . H155 H 0.413(2) 0.1192(8) 0.229(2) 0.052(11) Uiso 1 1 d . . . H156 H 0.445(2) 0.0812(9) 0.273(2) 0.054(10) Uiso 1 1 d . . . H157 H 0.478(3) 0.1145(9) 0.327(3) 0.080(12) Uiso 1 1 d . . . H158 H 0.368(2) 0.0566(9) 0.420(2) 0.064(10) Uiso 1 1 d . . . H159 H 0.419(3) 0.0884(8) 0.464(2) 0.060(11) Uiso 1 1 d . . . H160 H 0.288(4) 0.0794(14) 0.489(4) 0.18(3) Uiso 1 1 d . . . H161 H 0.0920(19) 0.1970(6) 0.2594(17) 0.025(7) Uiso 1 1 d . . . H162 H 0.150(2) 0.2327(8) 0.132(2) 0.059(10) Uiso 1 1 d . . . H163 H 0.251(2) 0.2341(8) 0.190(2) 0.054(10) Uiso 1 1 d . . . H164 H 0.214(2) 0.1985(7) 0.144(2) 0.039(8) Uiso 1 1 d . . . H165 H 0.166(2) 0.2626(8) 0.322(2) 0.054(9) Uiso 1 1 d . . . H166 H 0.085(2) 0.2399(7) 0.379(2) 0.033(8) Uiso 1 1 d . . . H167 H 0.060(2) 0.2539(8) 0.271(2) 0.054(10) Uiso 1 1 d . . . H168 H 0.082(2) 0.1227(7) 0.4001(19) 0.032(9) Uiso 1 1 d . . . H169 H -0.0201(19) 0.1417(7) 0.694(2) 0.034(8) Uiso 1 1 d . . . H170 H -0.168(2) 0.1179(7) 0.692(2) 0.047(9) Uiso 1 1 d . . . H171 H -0.234(2) 0.0925(7) 0.5449(18) 0.028(8) Uiso 1 1 d . . . H172 H -0.1264(15) 0.0913(5) 0.3267(15) 0.007(6) Uiso 1 1 d . . . H173 H -0.279(2) 0.1171(8) 0.3505(19) 0.040(8) Uiso 1 1 d . . . H174 H -0.289(2) 0.0817(7) 0.292(2) 0.042(9) Uiso 1 1 d . . . H175 H -0.310(2) 0.0816(8) 0.405(2) 0.052(9) Uiso 1 1 d . . . H176 H -0.1911(19) 0.0377(6) 0.4433(19) 0.030(7) Uiso 1 1 d . . . H177 H -0.078(2) 0.0399(7) 0.409(2) 0.049(9) Uiso 1 1 d . . . H178 H -0.167(2) 0.0359(7) 0.330(2) 0.045(9) Uiso 1 1 d . . . H179 H 0.136(2) 0.1503(8) 0.511(2) 0.049(10) Uiso 1 1 d . . . H180 H 0.072(3) 0.1989(10) 0.575(3) 0.086(14) Uiso 1 1 d . . . H181 H 0.182(3) 0.1941(9) 0.612(3) 0.083(13) Uiso 1 1 d . . . H182 H 0.087(3) 0.1821(10) 0.677(3) 0.089(14) Uiso 1 1 d . . . H183 H 0.237(3) 0.1316(10) 0.621(3) 0.083(15) Uiso 1 1 d . . . H184 H 0.181(3) 0.0981(10) 0.599(3) 0.080(12) Uiso 1 1 d . . . H185 H 0.158(3) 0.1215(12) 0.695(4) 0.12(2) Uiso 1 1 d . . . H186 H 0.730(4) 0.2243(11) 0.971(3) 0.126(17) Uiso 1 1 d . . . H187 H 0.670(3) 0.2308(9) 1.072(3) 0.084(13) Uiso 1 1 d . . . H188 H 0.633(3) 0.1928(12) 1.003(3) 0.131(17) Uiso 1 1 d . . . H189 H 0.515(2) 0.2452(8) 0.984(2) 0.056(10) Uiso 1 1 d . . . H190 H 0.605(3) 0.2742(9) 0.947(2) 0.081(12) Uiso 1 1 d . . . H191 H 0.426(3) 0.2489(8) 0.832(2) 0.069(11) Uiso 1 1 d . . . H192 H 0.522(2) 0.2801(9) 0.795(2) 0.078(12) Uiso 1 1 d . . . H193 H 0.438(3) 0.2537(10) 0.651(3) 0.088(13) Uiso 1 1 d . . . H194 H 0.558(3) 0.2400(8) 0.659(2) 0.069(11) Uiso 1 1 d . . . H195 H 0.471(3) 0.2114(10) 0.698(3) 0.082(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 0.0180(2) 0.0176(2) 0.0130(2) -0.00089(18) -0.00195(17) 0.00124(19) N2 0.0158(10) 0.0204(11) 0.0134(10) -0.0002(8) -0.0002(8) 0.0012(9) C3 0.0190(13) 0.0189(12) 0.0142(12) 0.0010(10) 0.0011(10) -0.0020(10) C4 0.0143(13) 0.0244(14) 0.0190(13) -0.0022(11) -0.0026(10) -0.0026(11) C5 0.0177(13) 0.0290(14) 0.0105(12) -0.0015(10) 0.0001(10) 0.0034(11) N6 0.0184(11) 0.0180(10) 0.0124(10) 0.0003(8) -0.0002(8) 0.0008(9) C7 0.0159(12) 0.0154(12) 0.0201(13) -0.0043(10) -0.0038(10) 0.0016(10) C8 0.0228(14) 0.0155(12) 0.0223(14) -0.0002(10) 0.0006(11) -0.0011(10) C9 0.0217(14) 0.0229(14) 0.0318(16) 0.0018(12) 0.0074(12) 0.0005(11) C10 0.0201(14) 0.0244(14) 0.0326(16) -0.0027(12) -0.0015(12) 0.0067(12) C11 0.0243(15) 0.0259(14) 0.0215(14) 0.0011(12) -0.0064(11) 0.0035(12) C12 0.0225(14) 0.0226(13) 0.0190(13) 0.0001(11) -0.0019(11) 0.0024(11) C13 0.0277(16) 0.0402(17) 0.0245(15) 0.0101(13) 0.0027(12) 0.0106(14) C14 0.054(2) 0.049(2) 0.0256(18) 0.0043(15) 0.0027(16) 0.0199(19) C15 0.041(2) 0.044(2) 0.039(2) 0.0181(16) 0.0067(17) -0.0003(16) C16 0.0266(15) 0.0223(14) 0.0278(15) 0.0062(12) 0.0107(12) 0.0083(12) C17 0.0363(18) 0.0303(17) 0.042(2) 0.0112(15) 0.0145(16) 0.0029(14) C18 0.041(2) 0.0331(18) 0.0315(18) 0.0103(14) 0.0015(15) 0.0040(16) C19 0.0257(16) 0.0201(14) 0.0299(17) 0.0002(12) -0.0055(13) 0.0012(12) C20 0.0212(14) 0.0271(16) 0.0267(16) -0.0008(13) -0.0044(12) 0.0057(12) C21 0.0164(13) 0.0199(13) 0.0179(13) 0.0009(10) -0.0031(10) 0.0009(10) C22 0.0177(13) 0.0252(14) 0.0216(14) 0.0042(11) 0.0013(11) 0.0041(11) C23 0.0264(15) 0.0299(15) 0.0243(15) 0.0107(12) 0.0064(12) 0.0039(12) C24 0.0279(15) 0.0211(14) 0.0355(17) 0.0080(13) 0.0029(12) 0.0045(12) C25 0.0238(14) 0.0215(14) 0.0262(15) -0.0022(12) 0.0021(12) 0.0055(11) C26 0.0197(13) 0.0206(13) 0.0199(13) 0.0016(11) -0.0010(10) -0.0006(10) C27 0.0307(16) 0.0204(14) 0.0239(15) 0.0009(11) 0.0079(12) 0.0035(12) C28 0.0350(18) 0.0315(18) 0.0359(19) 0.0019(15) 0.0133(15) 0.0069(14) C29 0.048(2) 0.0269(16) 0.0220(16) -0.0022(13) 0.0039(14) 0.0015(15) C30 0.0260(15) 0.0298(15) 0.0193(14) 0.0084(12) 0.0023(11) 0.0105(12) C31 0.0384(19) 0.045(2) 0.0301(18) -0.0075(16) 0.0100(15) 0.0021(16) C32 0.0360(19) 0.0429(19) 0.0365(19) -0.0010(16) 0.0155(15) 0.0035(16) N33 0.0274(13) 0.0244(12) 0.0191(13) -0.0015(10) -0.0028(10) -0.0055(10) C34 0.0303(15) 0.0246(14) 0.0231(14) -0.0016(11) -0.0027(12) -0.0096(12) C35 0.0266(15) 0.0287(15) 0.0295(16) -0.0032(12) 0.0010(12) -0.0076(12) C36 0.047(2) 0.0250(16) 0.0444(19) -0.0089(14) -0.0060(15) -0.0112(15) C37 0.062(2) 0.0350(18) 0.055(2) -0.0075(16) -0.0305(19) -0.0124(17) C38 0.059(2) 0.0344(19) 0.061(2) -0.0004(16) -0.0398(19) -0.0044(17) C39 0.0446(19) 0.0255(15) 0.0431(18) 0.0008(13) -0.0188(15) -0.0072(14) C40 0.050(2) 0.0263(16) 0.059(2) -0.0029(15) -0.0333(18) -0.0027(15) C41 0.047(3) 0.045(2) 0.116(4) -0.019(3) -0.021(3) 0.006(2) C42 0.124(4) 0.026(2) 0.089(3) 0.002(2) -0.068(3) 0.001(2) C43 0.0222(15) 0.0230(14) 0.0431(18) -0.0063(13) 0.0004(13) -0.0050(12) C44 0.038(2) 0.0378(19) 0.043(2) 0.0045(16) 0.0008(16) 0.0026(16) C45 0.0332(18) 0.0278(17) 0.055(2) -0.0091(16) 0.0021(17) -0.0016(14) N46 0.0217(12) 0.0295(12) 0.0187(12) -0.0014(10) -0.0005(9) 0.0016(11) C47 0.0300(14) 0.0235(13) 0.0146(13) 0.0038(11) 0.0033(11) 0.0112(12) C48 0.0396(17) 0.0318(15) 0.0194(15) -0.0013(12) -0.0004(12) 0.0121(13) C49 0.056(2) 0.0415(18) 0.0159(15) -0.0035(13) 0.0034(14) 0.0136(16) C50 0.062(2) 0.0418(18) 0.0219(16) 0.0060(14) 0.0198(16) 0.0152(17) C51 0.0374(18) 0.0331(17) 0.0344(18) 0.0081(14) 0.0130(14) 0.0061(14) C52 0.0334(16) 0.0220(13) 0.0215(14) 0.0069(11) 0.0074(12) 0.0054(12) C53 0.0280(15) 0.0302(15) 0.0241(15) 0.0083(12) 0.0081(12) -0.0033(12) C54 0.0371(19) 0.040(2) 0.045(2) 0.0130(17) -0.0014(16) -0.0002(16) C55 0.0313(18) 0.0323(17) 0.0347(18) 0.0009(14) 0.0061(15) -0.0017(14) C56 0.0436(19) 0.0482(19) 0.0208(16) -0.0096(14) -0.0090(14) 0.0038(15) C57 0.081(3) 0.050(2) 0.043(2) -0.0129(19) 0.006(2) -0.005(2) C58 0.058(3) 0.066(3) 0.094(4) -0.008(3) -0.043(3) 0.008(2) B59 0.0163(14) 0.0204(14) 0.0214(15) 0.0021(12) 0.0008(11) 0.0013(12) C60 0.0197(13) 0.0227(13) 0.0197(13) 0.0076(11) -0.0036(11) 0.0004(11) C61 0.0213(14) 0.0269(14) 0.0256(15) 0.0056(12) -0.0002(11) 0.0008(12) C62 0.0190(14) 0.0354(16) 0.0364(17) 0.0034(13) -0.0049(12) -0.0061(12) C63 0.0315(16) 0.0296(15) 0.0374(17) -0.0053(13) -0.0123(13) -0.0065(13) C64 0.0267(15) 0.0290(15) 0.0251(15) -0.0017(12) -0.0051(12) 0.0042(12) C65 0.0180(13) 0.0269(14) 0.0231(14) 0.0060(11) -0.0050(11) 0.0015(11) F66 0.0180(8) 0.0345(9) 0.0366(9) -0.0007(7) 0.0025(7) -0.0021(7) F67 0.0217(9) 0.0507(11) 0.0638(12) -0.0053(9) -0.0031(8) -0.0138(8) F68 0.0399(11) 0.0483(11) 0.0640(12) -0.0225(9) -0.0121(9) -0.0115(9) F69 0.0353(10) 0.0434(10) 0.0375(10) -0.0173(8) -0.0101(8) 0.0057(8) F70 0.0194(8) 0.0320(8) 0.0258(8) -0.0026(7) -0.0012(6) 0.0038(6) C71 0.0131(12) 0.0203(13) 0.0269(14) 0.0031(11) 0.0024(10) -0.0028(10) C72 0.0166(13) 0.0229(14) 0.0261(15) 0.0028(11) -0.0003(11) -0.0010(11) C73 0.0214(14) 0.0240(14) 0.0379(17) 0.0118(12) 0.0008(12) 0.0048(11) C74 0.0249(15) 0.0170(13) 0.0430(18) 0.0035(12) 0.0131(13) 0.0047(11) C75 0.0298(15) 0.0220(14) 0.0258(15) 0.0009(12) 0.0081(12) -0.0023(12) C76 0.0186(13) 0.0205(13) 0.0252(14) 0.0073(11) 0.0007(11) 0.0015(11) F77 0.0242(8) 0.0322(8) 0.0294(9) 0.0055(7) -0.0063(7) 0.0061(7) F78 0.0298(9) 0.0350(9) 0.0508(11) 0.0123(8) -0.0009(8) 0.0142(7) F79 0.0416(10) 0.0273(9) 0.0520(11) 0.0047(8) 0.0163(8) 0.0143(8) F80 0.0489(11) 0.0319(9) 0.0296(9) -0.0035(7) 0.0091(8) 0.0080(8) F81 0.0298(9) 0.0278(8) 0.0235(8) 0.0011(6) -0.0026(7) 0.0064(7) C82 0.0179(13) 0.0173(12) 0.0180(13) -0.0031(10) -0.0012(10) -0.0008(10) C83 0.0131(12) 0.0191(13) 0.0235(14) -0.0006(11) 0.0013(10) 0.0011(10) C84 0.0226(14) 0.0211(13) 0.0222(14) 0.0004(11) 0.0019(11) -0.0035(11) C85 0.0278(15) 0.0151(12) 0.0227(14) 0.0016(11) -0.0092(11) 0.0044(11) C86 0.0134(12) 0.0222(13) 0.0245(14) -0.0045(11) -0.0036(10) 0.0033(10) C87 0.0178(13) 0.0180(12) 0.0194(13) -0.0024(10) -0.0001(10) -0.0026(10) F88 0.0164(7) 0.0300(8) 0.0312(8) 0.0084(7) 0.0049(6) 0.0031(6) F89 0.0305(9) 0.0305(8) 0.0284(9) 0.0120(7) 0.0012(7) -0.0033(7) F90 0.0301(9) 0.0258(8) 0.0361(9) 0.0084(7) -0.0091(7) 0.0050(7) F91 0.0171(8) 0.0356(9) 0.0324(9) -0.0014(7) -0.0030(6) 0.0081(7) F92 0.0156(7) 0.0285(8) 0.0263(8) 0.0026(6) 0.0033(6) -0.0010(6) C93 0.0173(13) 0.0192(13) 0.0219(14) 0.0026(11) 0.0036(10) 0.0039(10) C94 0.0179(13) 0.0229(14) 0.0268(15) 0.0009(11) -0.0027(11) -0.0003(11) C95 0.0315(16) 0.0292(15) 0.0220(15) 0.0086(12) 0.0037(12) 0.0011(13) C96 0.0282(15) 0.0227(14) 0.0362(17) 0.0110(12) 0.0092(13) -0.0036(12) C97 0.0198(14) 0.0221(14) 0.0355(16) -0.0014(12) 0.0013(12) -0.0039(11) C98 0.0210(13) 0.0226(13) 0.0191(14) 0.0009(11) 0.0020(11) 0.0036(11) F99 0.0304(9) 0.0347(9) 0.0231(8) 0.0055(7) -0.0054(6) -0.0041(7) F100 0.0506(11) 0.0474(10) 0.0243(9) 0.0140(8) 0.0032(8) -0.0054(9) F101 0.0442(11) 0.0399(10) 0.0447(10) 0.0145(8) 0.0103(8) -0.0126(8) F102 0.0320(9) 0.0302(9) 0.0449(10) 0.0010(7) -0.0017(7) -0.0123(7) F103 0.0252(8) 0.0277(8) 0.0231(8) 0.0005(6) -0.0031(6) -0.0044(6) C104 0.046(2) 0.071(3) 0.064(3) -0.022(2) -0.003(2) 0.000(2) C105 0.051(2) 0.050(2) 0.053(2) -0.0188(18) 0.0031(18) -0.0053(18) O106 0.0458(14) 0.0546(14) 0.0569(15) -0.0122(12) 0.0014(12) -0.0011(12) C107 0.047(2) 0.043(2) 0.061(2) 0.0008(18) 0.0088(18) 0.0032(17) C108 0.064(3) 0.058(3) 0.051(2) 0.007(2) 0.011(2) 0.001(2) _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 N33 1.863(2) . ? Ti1 N46 1.875(2) . ? Ti1 N6 1.9876(19) . ? Ti1 N2 2.0150(19) . ? Ti1 H150 2.22(4) . ? Ti1 H168 2.01(3) . ? N2 C3 1.343(3) . ? N2 C7 1.455(3) . ? C3 C4 1.410(3) . ? C3 C19 1.501(3) . ? C4 C5 1.385(3) . ? C4 H109 0.91(2) . ? C5 N6 1.361(3) . ? C5 C20 1.508(3) . ? N6 C21 1.454(3) . ? C7 C8 1.401(3) . ? C7 C12 1.402(3) . ? C8 C9 1.386(3) . ? C8 C16 1.517(3) . ? C9 C10 1.379(4) . ? C9 H110 0.96(2) . ? C10 C11 1.372(4) . ? C10 H111 0.93(2) . ? C11 C12 1.391(3) . ? C11 H112 0.95(3) . ? C12 C13 1.519(4) . ? C13 C14 1.524(4) . ? C13 C15 1.525(4) . ? C13 H113 0.95(3) . ? C14 H114 0.98(3) . ? C14 H115 0.98(3) . ? C14 H116 1.00(4) . ? C15 H117 0.96(3) . ? C15 H118 1.07(3) . ? C15 H119 1.00(3) . ? C16 C18 1.523(4) . ? C16 C17 1.524(4) . ? C16 H120 0.96(2) . ? C17 H121 0.99(3) . ? C17 H122 1.00(3) . ? C17 H123 0.96(3) . ? C18 H124 0.96(3) . ? C18 H125 0.99(3) . ? C18 H126 0.92(3) . ? C19 H127 0.99(3) . ? C19 H128 0.91(3) . ? C19 H129 0.98(3) . ? C20 H130 0.93(3) . ? C20 H131 0.99(3) . ? C20 H132 0.97(3) . ? C21 C26 1.407(3) . ? C21 C22 1.412(3) . ? C22 C23 1.388(3) . ? C22 C30 1.520(3) . ? C23 C24 1.379(4) . ? C23 H133 0.92(2) . ? C24 C25 1.376(4) . ? C24 H134 0.94(2) . ? C25 C26 1.389(3) . ? C25 H135 0.95(2) . ? C26 C27 1.524(3) . ? C27 C29 1.529(4) . ? C27 C28 1.535(4) . ? C27 H136 0.90(2) . ? C28 H137 0.93(3) . ? C28 H138 0.98(3) . ? C28 H139 1.02(3) . ? C29 H140 0.96(3) . ? C29 H141 0.99(3) . ? C29 H142 1.01(3) . ? C30 C32 1.520(4) . ? C30 C31 1.530(4) . ? C30 H143 0.93(2) . ? C31 H144 0.98(3) . ? C31 H145 1.00(3) . ? C31 H146 1.02(3) . ? C32 H147 0.95(3) . ? C32 H148 1.02(3) . ? C32 H149 1.00(3) . ? N33 C34 1.450(3) . ? N33 H150 0.74(4) . ? C34 C39 1.397(4) . ? C34 C35 1.410(4) . ? C35 C36 1.388(4) . ? C35 C43 1.511(4) . ? C36 C37 1.377(4) . ? C36 H151 0.93(3) . ? C37 C38 1.361(4) . ? C37 H152 0.97(3) . ? C38 C39 1.400(4) . ? C38 H153 0.90(3) . ? C39 C40 1.516(4) . ? C40 C41 1.525(6) . ? C40 C42 1.526(5) . ? C40 H154 0.94(3) . ? C41 H155 1.00(3) . ? C41 H156 0.99(3) . ? C41 H157 0.99(4) . ? C42 H158 1.00(3) . ? C42 H159 0.97(3) . ? C42 H160 1.22(6) . ? C43 C45 1.526(4) . ? C43 C44 1.527(4) . ? C43 H161 0.93(3) . ? C44 H162 0.99(3) . ? C44 H163 1.00(3) . ? C44 H164 0.99(3) . ? C45 H165 1.07(3) . ? C45 H166 1.00(3) . ? C45 H167 0.95(3) . ? N46 C47 1.414(3) . ? N46 H168 0.81(3) . ? C47 C52 1.412(4) . ? C47 C48 1.417(3) . ? C48 C49 1.389(4) . ? C48 C56 1.512(4) . ? C49 C50 1.370(5) . ? C49 H169 0.94(3) . ? C50 C51 1.383(4) . ? C50 H170 0.95(3) . ? C51 C52 1.388(4) . ? C51 H171 0.93(3) . ? C52 C53 1.509(4) . ? C53 C55 1.522(4) . ? C53 C54 1.533(4) . ? C53 H172 0.95(2) . ? C54 H173 1.00(3) . ? C54 H174 0.98(3) . ? C54 H175 1.02(3) . ? C55 H176 1.02(3) . ? C55 H177 1.03(3) . ? C55 H178 0.96(3) . ? C56 C57 1.529(5) . ? C56 C58 1.530(5) . ? C56 H179 0.89(3) . ? C57 H180 0.98(4) . ? C57 H181 1.07(4) . ? C57 H182 0.97(4) . ? C58 H183 0.90(4) . ? C58 H184 1.05(4) . ? C58 H185 1.02(5) . ? B59 C71 1.645(4) . ? B59 C60 1.650(4) . ? B59 C93 1.655(4) . ? B59 C82 1.656(4) . ? C60 C65 1.384(3) . ? C60 C61 1.390(3) . ? C61 F66 1.350(3) . ? C61 C62 1.387(4) . ? C62 F67 1.348(3) . ? C62 C63 1.363(4) . ? C63 F68 1.347(3) . ? C63 C64 1.378(4) . ? C64 F69 1.341(3) . ? C64 C65 1.375(3) . ? C65 F70 1.360(3) . ? C71 C76 1.389(3) . ? C71 C72 1.395(3) . ? C72 F77 1.356(3) . ? C72 C73 1.372(3) . ? C73 F78 1.349(3) . ? C73 C74 1.366(4) . ? C74 F79 1.348(3) . ? C74 C75 1.371(4) . ? C75 F80 1.349(3) . ? C75 C76 1.381(3) . ? C76 F81 1.357(3) . ? C82 C83 1.388(3) . ? C82 C87 1.390(3) . ? C83 F88 1.356(3) . ? C83 C84 1.378(3) . ? C84 F89 1.350(3) . ? C84 C85 1.377(3) . ? C85 F90 1.347(3) . ? C85 C86 1.368(3) . ? C86 F91 1.346(3) . ? C86 C87 1.381(3) . ? C87 F92 1.348(3) . ? C93 C98 1.385(3) . ? C93 C94 1.384(3) . ? C94 F99 1.356(3) . ? C94 C95 1.384(3) . ? C95 F100 1.348(3) . ? C95 C96 1.364(4) . ? C96 F101 1.341(3) . ? C96 C97 1.371(4) . ? C97 F102 1.349(3) . ? C97 C98 1.371(3) . ? C98 F103 1.356(3) . ? C104 C105 1.506(5) . ? C104 H186 1.09(5) . ? C104 H187 1.06(4) . ? C104 H188 1.24(5) . ? C105 O106 1.433(4) . ? C105 H189 1.11(3) . ? C105 H190 1.19(4) . ? O106 C107 1.442(4) . ? C107 C108 1.497(5) . ? C107 H191 1.18(3) . ? C107 H192 1.14(4) . ? C108 H193 1.12(4) . ? C108 H194 1.08(4) . ? C108 H195 1.07(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 N33 Ti1 N46 105.25(11) . . ? N33 Ti1 N6 115.88(9) . . ? N46 Ti1 N6 117.24(9) . . ? N33 Ti1 N2 109.78(9) . . ? N46 Ti1 N2 115.77(9) . . ? N6 Ti1 N2 92.87(8) . . ? N33 Ti1 H150 18.6(10) . . ? N46 Ti1 H150 123.5(10) . . ? N6 Ti1 H150 101.0(10) . . ? N2 Ti1 H150 101.1(10) . . ? N33 Ti1 H168 82.0(8) . . ? N46 Ti1 H168 23.7(8) . . ? N6 Ti1 H168 134.6(8) . . ? N2 Ti1 H168 121.2(8) . . ? H150 Ti1 H168 100.5(13) . . ? C3 N2 C7 120.03(19) . . ? C3 N2 Ti1 119.79(16) . . ? C7 N2 Ti1 120.07(14) . . ? N2 C3 C4 121.6(2) . . ? N2 C3 C19 121.2(2) . . ? C4 C3 C19 117.2(2) . . ? C5 C4 C3 130.0(2) . . ? C5 C4 H109 115.5(15) . . ? C3 C4 H109 114.2(15) . . ? N6 C5 C4 122.8(2) . . ? N6 C5 C20 119.1(2) . . ? C4 C5 C20 118.0(2) . . ? C5 N6 C21 119.21(19) . . ? C5 N6 Ti1 117.52(15) . . ? C21 N6 Ti1 122.46(15) . . ? C8 C7 C12 121.6(2) . . ? C8 C7 N2 117.9(2) . . ? C12 C7 N2 120.4(2) . . ? C9 C8 C7 118.1(2) . . ? C9 C8 C16 120.5(2) . . ? C7 C8 C16 121.4(2) . . ? C10 C9 C8 121.1(3) . . ? C10 C9 H110 119.7(15) . . ? C8 C9 H110 119.2(15) . . ? C11 C10 C9 120.0(3) . . ? C11 C10 H111 119.6(14) . . ? C9 C10 H111 120.3(14) . . ? C10 C11 C12 121.6(2) . . ? C10 C11 H112 121.3(15) . . ? C12 C11 H112 117.1(15) . . ? C11 C12 C7 117.5(2) . . ? C11 C12 C13 119.3(2) . . ? C7 C12 C13 123.2(2) . . ? C12 C13 C14 111.1(3) . . ? C12 C13 C15 111.6(2) . . ? C14 C13 C15 111.2(3) . . ? C12 C13 H113 108.4(15) . . ? C14 C13 H113 104.7(15) . . ? C15 C13 H113 109.6(16) . . ? C13 C14 H114 112.2(15) . . ? C13 C14 H115 115.6(16) . . ? H114 C14 H115 98(2) . . ? C13 C14 H116 111(2) . . ? H114 C14 H116 113(2) . . ? H115 C14 H116 106(3) . . ? C13 C15 H117 112.5(18) . . ? C13 C15 H118 111.6(16) . . ? H117 C15 H118 105(2) . . ? C13 C15 H119 111.5(18) . . ? H117 C15 H119 107(2) . . ? H118 C15 H119 109(3) . . ? C8 C16 C18 111.8(2) . . ? C8 C16 C17 112.8(2) . . ? C18 C16 C17 111.7(3) . . ? C8 C16 H120 106.2(14) . . ? C18 C16 H120 108.3(14) . . ? C17 C16 H120 105.5(14) . . ? C16 C17 H121 109.3(18) . . ? C16 C17 H122 108.8(16) . . ? H121 C17 H122 111(2) . . ? C16 C17 H123 110.0(18) . . ? H121 C17 H123 109(2) . . ? H122 C17 H123 109(2) . . ? C16 C18 H124 109.1(17) . . ? C16 C18 H125 114.4(17) . . ? H124 C18 H125 106(2) . . ? C16 C18 H126 112.6(17) . . ? H124 C18 H126 103(2) . . ? H125 C18 H126 110(2) . . ? C3 C19 H127 112.9(16) . . ? C3 C19 H128 109.2(19) . . ? H127 C19 H128 106(2) . . ? C3 C19 H129 111.0(18) . . ? H127 C19 H129 106(2) . . ? H128 C19 H129 112(3) . . ? C5 C20 H130 114.8(19) . . ? C5 C20 H131 108.5(16) . . ? H130 C20 H131 109(2) . . ? C5 C20 H132 107.8(18) . . ? H130 C20 H132 108(2) . . ? H131 C20 H132 109(2) . . ? C26 C21 C22 121.6(2) . . ? C26 C21 N6 120.6(2) . . ? C22 C21 N6 117.9(2) . . ? C23 C22 C21 117.4(2) . . ? C23 C22 C30 120.3(2) . . ? C21 C22 C30 122.3(2) . . ? C24 C23 C22 121.7(3) . . ? C24 C23 H133 119.9(14) . . ? C22 C23 H133 118.4(14) . . ? C25 C24 C23 120.0(3) . . ? C25 C24 H134 118.9(15) . . ? C23 C24 H134 121.0(15) . . ? C24 C25 C26 121.3(2) . . ? C24 C25 H135 120.4(14) . . ? C26 C25 H135 118.3(14) . . ? C25 C26 C21 118.0(2) . . ? C25 C26 C27 118.4(2) . . ? C21 C26 C27 123.6(2) . . ? C26 C27 C29 111.7(2) . . ? C26 C27 C28 110.9(2) . . ? C29 C27 C28 110.4(2) . . ? C26 C27 H136 108.6(14) . . ? C29 C27 H136 107.7(15) . . ? C28 C27 H136 107.5(15) . . ? C27 C28 H137 109.4(17) . . ? C27 C28 H138 111.9(17) . . ? H137 C28 H138 107(2) . . ? C27 C28 H139 110.9(15) . . ? H137 C28 H139 109(2) . . ? H138 C28 H139 109(2) . . ? C27 C29 H140 110.6(17) . . ? C27 C29 H141 109.2(15) . . ? H140 C29 H141 106(2) . . ? C27 C29 H142 110.8(15) . . ? H140 C29 H142 109(2) . . ? H141 C29 H142 110(2) . . ? C32 C30 C22 113.7(2) . . ? C32 C30 C31 108.7(2) . . ? C22 C30 C31 112.7(2) . . ? C32 C30 H143 110.8(15) . . ? C22 C30 H143 108.2(14) . . ? C31 C30 H143 102.3(15) . . ? C30 C31 H144 116.1(18) . . ? C30 C31 H145 102.9(17) . . ? H144 C31 H145 110(3) . . ? C30 C31 H146 109.0(16) . . ? H144 C31 H146 107(2) . . ? H145 C31 H146 113(2) . . ? C30 C32 H147 107.8(18) . . ? C30 C32 H148 110.7(18) . . ? H147 C32 H148 106(2) . . ? C30 C32 H149 113.3(16) . . ? H147 C32 H149 108(2) . . ? H148 C32 H149 110(2) . . ? C34 N33 Ti1 132.80(19) . . ? C34 N33 H150 117(3) . . ? Ti1 N33 H150 109(3) . . ? C39 C34 C35 121.6(2) . . ? C39 C34 N33 120.0(2) . . ? C35 C34 N33 118.3(2) . . ? C36 C35 C34 117.7(3) . . ? C36 C35 C43 121.1(3) . . ? C34 C35 C43 121.0(2) . . ? C37 C36 C35 121.2(3) . . ? C37 C36 H151 116.4(17) . . ? C35 C36 H151 122.4(18) . . ? C38 C37 C36 120.4(3) . . ? C38 C37 H152 119.1(19) . . ? C36 C37 H152 120.5(19) . . ? C37 C38 C39 121.5(3) . . ? C37 C38 H153 119(2) . . ? C39 C38 H153 119(2) . . ? C34 C39 C38 117.5(3) . . ? C34 C39 C40 123.6(2) . . ? C38 C39 C40 118.7(3) . . ? C39 C40 C41 109.4(3) . . ? C39 C40 C42 113.1(3) . . ? C41 C40 C42 111.3(4) . . ? C39 C40 H154 109.2(16) . . ? C41 C40 H154 108.5(16) . . ? C42 C40 H154 105.2(16) . . ? C40 C41 H155 113.5(19) . . ? C40 C41 H156 109.3(18) . . ? H155 C41 H156 113(3) . . ? C40 C41 H157 108(2) . . ? H155 C41 H157 108(3) . . ? H156 C41 H157 104(3) . . ? C40 C42 H158 111.7(19) . . ? C40 C42 H159 105(2) . . ? H158 C42 H159 103(3) . . ? C40 C42 H160 113(3) . . ? H158 C42 H160 104(3) . . ? H159 C42 H160 120(3) . . ? C35 C43 C45 114.1(3) . . ? C35 C43 C44 109.7(2) . . ? C45 C43 C44 109.8(3) . . ? C35 C43 H161 104.6(15) . . ? C45 C43 H161 107.4(15) . . ? C44 C43 H161 111.1(15) . . ? C43 C44 H162 112.6(19) . . ? C43 C44 H163 110.3(18) . . ? H162 C44 H163 104(2) . . ? C43 C44 H164 112.7(16) . . ? H162 C44 H164 109(2) . . ? H163 C44 H164 108(2) . . ? C43 C45 H165 110.3(16) . . ? C43 C45 H166 110.7(16) . . ? H165 C45 H166 107(2) . . ? C43 C45 H167 109.0(19) . . ? H165 C45 H167 107(2) . . ? H166 C45 H167 113(3) . . ? C47 N46 Ti1 157.47(19) . . ? C47 N46 H168 114(2) . . ? Ti1 N46 H168 88(2) . . ? C52 C47 N46 119.8(2) . . ? C52 C47 C48 120.8(2) . . ? N46 C47 C48 119.4(2) . . ? C49 C48 C47 117.5(3) . . ? C49 C48 C56 118.9(3) . . ? C47 C48 C56 123.6(2) . . ? C50 C49 C48 122.5(3) . . ? C50 C49 H169 120.0(17) . . ? C48 C49 H169 117.4(17) . . ? C49 C50 C51 119.4(3) . . ? C49 C50 H170 115.6(18) . . ? C51 C50 H170 125.0(18) . . ? C50 C51 C52 121.5(3) . . ? C50 C51 H171 121.8(16) . . ? C52 C51 H171 116.7(16) . . ? C51 C52 C47 118.3(3) . . ? C51 C52 C53 119.7(3) . . ? C47 C52 C53 121.9(2) . . ? C52 C53 C55 109.5(2) . . ? C52 C53 C54 113.7(2) . . ? C55 C53 C54 109.7(2) . . ? C52 C53 H172 107.5(13) . . ? C55 C53 H172 108.2(13) . . ? C54 C53 H172 108.1(13) . . ? C53 C54 H173 110.0(16) . . ? C53 C54 H174 109.7(17) . . ? H173 C54 H174 109(2) . . ? C53 C54 H175 109.1(17) . . ? H173 C54 H175 110(2) . . ? H174 C54 H175 108(2) . . ? C53 C55 H176 108.5(15) . . ? C53 C55 H177 111.7(17) . . ? H176 C55 H177 110(2) . . ? C53 C55 H178 106.2(17) . . ? H176 C55 H178 111(2) . . ? H177 C55 H178 109(2) . . ? C48 C56 C57 112.9(3) . . ? C48 C56 C58 109.7(3) . . ? C57 C56 C58 110.9(3) . . ? C48 C56 H179 111(2) . . ? C57 C56 H179 105(2) . . ? C58 C56 H179 107(2) . . ? C56 C57 H180 111(2) . . ? C56 C57 H181 111(2) . . ? H180 C57 H181 102(3) . . ? C56 C57 H182 111(2) . . ? H180 C57 H182 108(3) . . ? H181 C57 H182 114(3) . . ? C56 C58 H183 105(3) . . ? C56 C58 H184 116(2) . . ? H183 C58 H184 105(3) . . ? C56 C58 H185 110(3) . . ? H183 C58 H185 113(4) . . ? H184 C58 H185 108(3) . . ? C71 B59 C60 115.0(2) . . ? C71 B59 C93 100.94(19) . . ? C60 B59 C93 113.5(2) . . ? C71 B59 C82 113.1(2) . . ? C60 B59 C82 100.33(18) . . ? C93 B59 C82 114.6(2) . . ? C65 C60 C61 113.2(2) . . ? C65 C60 B59 118.5(2) . . ? C61 C60 B59 127.7(2) . . ? F66 C61 C62 115.4(2) . . ? F66 C61 C60 120.9(2) . . ? C62 C61 C60 123.7(2) . . ? F67 C62 C63 120.2(2) . . ? F67 C62 C61 120.0(3) . . ? C63 C62 C61 119.8(2) . . ? F68 C63 C62 120.8(3) . . ? F68 C63 C64 119.8(3) . . ? C62 C63 C64 119.4(2) . . ? F69 C64 C65 120.9(2) . . ? F69 C64 C63 120.5(2) . . ? C65 C64 C63 118.5(2) . . ? F70 C65 C64 115.5(2) . . ? F70 C65 C60 119.2(2) . . ? C64 C65 C60 125.4(2) . . ? C76 C71 C72 112.6(2) . . ? C76 C71 B59 127.7(2) . . ? C72 C71 B59 119.2(2) . . ? F77 C72 C73 116.4(2) . . ? F77 C72 C71 118.7(2) . . ? C73 C72 C71 124.9(2) . . ? F78 C73 C74 119.9(2) . . ? F78 C73 C72 120.7(2) . . ? C74 C73 C72 119.4(2) . . ? F79 C74 C73 120.9(2) . . ? F79 C74 C75 120.1(2) . . ? C73 C74 C75 119.0(2) . . ? F80 C75 C74 119.9(2) . . ? F80 C75 C76 120.4(2) . . ? C74 C75 C76 119.8(2) . . ? F81 C76 C75 114.9(2) . . ? F81 C76 C71 120.9(2) . . ? C75 C76 C71 124.2(2) . . ? C83 C82 C87 113.2(2) . . ? C83 C82 B59 118.9(2) . . ? C87 C82 B59 127.3(2) . . ? F88 C83 C84 115.6(2) . . ? F88 C83 C82 119.4(2) . . ? C84 C83 C82 125.0(2) . . ? F89 C84 C85 120.1(2) . . ? F89 C84 C83 121.2(2) . . ? C85 C84 C83 118.7(2) . . ? F90 C85 C86 120.8(2) . . ? F90 C85 C84 119.9(2) . . ? C86 C85 C84 119.3(2) . . ? F91 C86 C85 120.2(2) . . ? F91 C86 C87 120.0(2) . . ? C85 C86 C87 119.9(2) . . ? F92 C87 C86 115.4(2) . . ? F92 C87 C82 120.8(2) . . ? C86 C87 C82 123.8(2) . . ? C98 C93 C94 113.2(2) . . ? C98 C93 B59 120.1(2) . . ? C94 C93 B59 125.9(2) . . ? F99 C94 C95 114.9(2) . . ? F99 C94 C93 121.4(2) . . ? C95 C94 C93 123.7(2) . . ? F100 C95 C96 120.2(2) . . ? F100 C95 C94 119.9(2) . . ? C96 C95 C94 119.9(2) . . ? F101 C96 C95 120.3(2) . . ? F101 C96 C97 120.6(2) . . ? C95 C96 C97 119.0(2) . . ? F102 C97 C98 121.5(2) . . ? F102 C97 C96 119.3(2) . . ? C98 C97 C96 119.2(2) . . ? F103 C98 C97 116.5(2) . . ? F103 C98 C93 118.6(2) . . ? C97 C98 C93 124.9(2) . . ? C105 C104 H186 115(2) . . ? C105 C104 H187 111(2) . . ? H186 C104 H187 104(3) . . ? C105 C104 H188 111(2) . . ? H186 C104 H188 109(3) . . ? H187 C104 H188 106(3) . . ? O106 C105 C104 108.4(3) . . ? O106 C105 H189 112.9(16) . . ? C104 C105 H189 111.9(16) . . ? O106 C105 H190 109.6(17) . . ? C104 C105 H190 112.4(17) . . ? H189 C105 H190 102(2) . . ? C105 O106 C107 112.3(3) . . ? O106 C107 C108 108.5(3) . . ? O106 C107 H191 106.8(16) . . ? C108 C107 H191 110.6(16) . . ? O106 C107 H192 108.7(18) . . ? C108 C107 H192 113.0(17) . . ? H191 C107 H192 109(2) . . ? C107 C108 H193 107.7(19) . . ? C107 C108 H194 111.7(19) . . ? H193 C108 H194 105(3) . . ? C107 C108 H195 109.6(19) . . ? H193 C108 H195 113(3) . . ? H194 C108 H195 110(3) . . ? 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 N33 Ti1 N2 C3 -153.14(17) . . . . ? N46 Ti1 N2 C3 87.92(19) . . . . ? N6 Ti1 N2 C3 -34.29(18) . . . . ? N33 Ti1 N2 C7 30.51(19) . . . . ? N46 Ti1 N2 C7 -88.43(18) . . . . ? N6 Ti1 N2 C7 149.35(17) . . . . ? C7 N2 C3 C4 -170.0(2) . . . . ? Ti1 N2 C3 C4 13.6(3) . . . . ? C7 N2 C3 C19 9.0(3) . . . . ? Ti1 N2 C3 C19 -167.31(19) . . . . ? N2 C3 C4 C5 15.8(4) . . . . ? C19 C3 C4 C5 -163.2(3) . . . . ? C3 C4 C5 N6 -9.4(4) . . . . ? C3 C4 C5 C20 170.5(3) . . . . ? C4 C5 N6 C21 165.3(2) . . . . ? C20 C5 N6 C21 -14.7(3) . . . . ? C4 C5 N6 Ti1 -24.8(3) . . . . ? C20 C5 N6 Ti1 155.25(19) . . . . ? N33 Ti1 N6 C5 152.73(17) . . . . ? N46 Ti1 N6 C5 -81.93(19) . . . . ? N2 Ti1 N6 C5 39.10(17) . . . . ? N33 Ti1 N6 C21 -37.7(2) . . . . ? N46 Ti1 N6 C21 87.68(19) . . . . ? N2 Ti1 N6 C21 -151.30(17) . . . . ? C3 N2 C7 C8 100.8(3) . . . . ? Ti1 N2 C7 C8 -82.9(2) . . . . ? C3 N2 C7 C12 -81.4(3) . . . . ? Ti1 N2 C7 C12 95.0(2) . . . . ? C12 C7 C8 C9 -0.2(4) . . . . ? N2 C7 C8 C9 177.6(2) . . . . ? C12 C7 C8 C16 178.1(2) . . . . ? N2 C7 C8 C16 -4.1(3) . . . . ? C7 C8 C9 C10 -1.4(4) . . . . ? C16 C8 C9 C10 -179.7(2) . . . . ? C8 C9 C10 C11 1.9(4) . . . . ? C9 C10 C11 C12 -0.8(4) . . . . ? C10 C11 C12 C7 -0.8(4) . . . . ? C10 C11 C12 C13 177.4(2) . . . . ? C8 C7 C12 C11 1.2(4) . . . . ? N2 C7 C12 C11 -176.5(2) . . . . ? C8 C7 C12 C13 -176.9(2) . . . . ? N2 C7 C12 C13 5.4(4) . . . . ? C11 C12 C13 C14 72.0(3) . . . . ? C7 C12 C13 C14 -109.9(3) . . . . ? C11 C12 C13 C15 -52.7(3) . . . . ? C7 C12 C13 C15 125.4(3) . . . . ? C9 C8 C16 C18 83.2(3) . . . . ? C7 C8 C16 C18 -95.0(3) . . . . ? C9 C8 C16 C17 -43.7(3) . . . . ? C7 C8 C16 C17 138.1(3) . . . . ? C5 N6 C21 C26 90.0(3) . . . . ? Ti1 N6 C21 C26 -79.5(3) . . . . ? C5 N6 C21 C22 -90.4(3) . . . . ? Ti1 N6 C21 C22 100.1(2) . . . . ? C26 C21 C22 C23 0.6(4) . . . . ? N6 C21 C22 C23 -179.0(2) . . . . ? C26 C21 C22 C30 -177.8(2) . . . . ? N6 C21 C22 C30 2.6(3) . . . . ? C21 C22 C23 C24 1.1(4) . . . . ? C30 C22 C23 C24 179.6(2) . . . . ? C22 C23 C24 C25 -1.6(4) . . . . ? C23 C24 C25 C26 0.3(4) . . . . ? C24 C25 C26 C21 1.4(4) . . . . ? C24 C25 C26 C27 -176.8(2) . . . . ? C22 C21 C26 C25 -1.8(4) . . . . ? N6 C21 C26 C25 177.8(2) . . . . ? C22 C21 C26 C27 176.2(2) . . . . ? N6 C21 C26 C27 -4.2(4) . . . . ? C25 C26 C27 C29 -67.8(3) . . . . ? C21 C26 C27 C29 114.2(3) . . . . ? C25 C26 C27 C28 55.8(3) . . . . ? C21 C26 C27 C28 -122.3(3) . . . . ? C23 C22 C30 C32 30.2(4) . . . . ? C21 C22 C30 C32 -151.4(3) . . . . ? C23 C22 C30 C31 -94.0(3) . . . . ? C21 C22 C30 C31 84.4(3) . . . . ? N46 Ti1 N33 C34 -6.6(3) . . . . ? N6 Ti1 N33 C34 124.7(2) . . . . ? N2 Ti1 N33 C34 -131.8(2) . . . . ? Ti1 N33 C34 C39 91.3(3) . . . . ? Ti1 N33 C34 C35 -86.7(3) . . . . ? C39 C34 C35 C36 -3.3(4) . . . . ? N33 C34 C35 C36 174.7(3) . . . . ? C39 C34 C35 C43 170.9(3) . . . . ? N33 C34 C35 C43 -11.1(4) . . . . ? C34 C35 C36 C37 0.4(5) . . . . ? C43 C35 C36 C37 -173.8(3) . . . . ? C35 C36 C37 C38 2.3(6) . . . . ? C36 C37 C38 C39 -2.1(6) . . . . ? C35 C34 C39 C38 3.5(5) . . . . ? N33 C34 C39 C38 -174.5(3) . . . . ? C35 C34 C39 C40 -170.5(3) . . . . ? N33 C34 C39 C40 11.5(5) . . . . ? C37 C38 C39 C34 -0.7(6) . . . . ? C37 C38 C39 C40 173.6(4) . . . . ? C34 C39 C40 C41 96.1(4) . . . . ? C38 C39 C40 C41 -77.8(4) . . . . ? C34 C39 C40 C42 -139.2(4) . . . . ? C38 C39 C40 C42 46.9(5) . . . . ? C36 C35 C43 C45 -25.7(4) . . . . ? C34 C35 C43 C45 160.2(3) . . . . ? C36 C35 C43 C44 97.9(3) . . . . ? C34 C35 C43 C44 -76.1(3) . . . . ? N33 Ti1 N46 C47 150.6(5) . . . . ? N6 Ti1 N46 C47 20.2(5) . . . . ? N2 Ti1 N46 C47 -88.0(5) . . . . ? Ti1 N46 C47 C52 28.6(6) . . . . ? Ti1 N46 C47 C48 -150.6(4) . . . . ? C52 C47 C48 C49 1.0(4) . . . . ? N46 C47 C48 C49 -179.7(2) . . . . ? C52 C47 C48 C56 177.9(2) . . . . ? N46 C47 C48 C56 -2.8(4) . . . . ? C47 C48 C49 C50 -0.2(4) . . . . ? C56 C48 C49 C50 -177.2(3) . . . . ? C48 C49 C50 C51 -1.0(5) . . . . ? C49 C50 C51 C52 1.3(5) . . . . ? C50 C51 C52 C47 -0.5(4) . . . . ? C50 C51 C52 C53 175.6(3) . . . . ? N46 C47 C52 C51 -180.0(2) . . . . ? C48 C47 C52 C51 -0.7(4) . . . . ? N46 C47 C52 C53 4.1(4) . . . . ? C48 C47 C52 C53 -176.7(2) . . . . ? C51 C52 C53 C55 -77.9(3) . . . . ? C47 C52 C53 C55 98.0(3) . . . . ? C51 C52 C53 C54 45.2(3) . . . . ? C47 C52 C53 C54 -138.9(3) . . . . ? C49 C48 C56 C57 -50.8(4) . . . . ? C47 C48 C56 C57 132.4(3) . . . . ? C49 C48 C56 C58 73.5(4) . . . . ? C47 C48 C56 C58 -103.4(4) . . . . ? C71 B59 C60 C65 173.3(2) . . . . ? C93 B59 C60 C65 57.7(3) . . . . ? C82 B59 C60 C65 -65.0(3) . . . . ? C71 B59 C60 C61 -16.2(3) . . . . ? C93 B59 C60 C61 -131.8(3) . . . . ? C82 B59 C60 C61 105.5(3) . . . . ? C65 C60 C61 F66 178.5(2) . . . . ? B59 C60 C61 F66 7.6(4) . . . . ? C65 C60 C61 C62 -0.6(4) . . . . ? B59 C60 C61 C62 -171.5(2) . . . . ? F66 C61 C62 F67 0.4(4) . . . . ? C60 C61 C62 F67 179.6(2) . . . . ? F66 C61 C62 C63 -178.0(2) . . . . ? C60 C61 C62 C63 1.2(4) . . . . ? F67 C62 C63 F68 0.6(4) . . . . ? C61 C62 C63 F68 179.0(2) . . . . ? F67 C62 C63 C64 -179.1(2) . . . . ? C61 C62 C63 C64 -0.7(4) . . . . ? F68 C63 C64 F69 -0.7(4) . . . . ? C62 C63 C64 F69 178.9(2) . . . . ? F68 C63 C64 C65 -180.0(2) . . . . ? C62 C63 C64 C65 -0.3(4) . . . . ? F69 C64 C65 F70 0.9(3) . . . . ? C63 C64 C65 F70 -179.8(2) . . . . ? F69 C64 C65 C60 -178.3(2) . . . . ? C63 C64 C65 C60 0.9(4) . . . . ? C61 C60 C65 F70 -179.7(2) . . . . ? B59 C60 C65 F70 -7.8(3) . . . . ? C61 C60 C65 C64 -0.5(4) . . . . ? B59 C60 C65 C64 171.4(2) . . . . ? C60 B59 C71 C76 132.5(3) . . . . ? C93 B59 C71 C76 -104.9(3) . . . . ? C82 B59 C71 C76 18.0(3) . . . . ? C60 B59 C71 C72 -56.5(3) . . . . ? C93 B59 C71 C72 66.1(3) . . . . ? C82 B59 C71 C72 -171.0(2) . . . . ? C76 C71 C72 F77 177.2(2) . . . . ? B59 C71 C72 F77 5.0(3) . . . . ? C76 C71 C72 C73 -1.8(4) . . . . ? B59 C71 C72 C73 -174.0(2) . . . . ? F77 C72 C73 F78 1.6(4) . . . . ? C71 C72 C73 F78 -179.4(2) . . . . ? F77 C72 C73 C74 -177.9(2) . . . . ? C71 C72 C73 C74 1.2(4) . . . . ? F78 C73 C74 F79 0.3(4) . . . . ? C72 C73 C74 F79 179.7(2) . . . . ? F78 C73 C74 C75 -179.5(2) . . . . ? C72 C73 C74 C75 -0.1(4) . . . . ? F79 C74 C75 F80 0.1(4) . . . . ? C73 C74 C75 F80 179.9(2) . . . . ? F79 C74 C75 C76 180.0(2) . . . . ? C73 C74 C75 C76 -0.2(4) . . . . ? F80 C75 C76 F81 -0.8(3) . . . . ? C74 C75 C76 F81 179.3(2) . . . . ? F80 C75 C76 C71 179.4(2) . . . . ? C74 C75 C76 C71 -0.5(4) . . . . ? C72 C71 C76 F81 -178.4(2) . . . . ? B59 C71 C76 F81 -6.9(4) . . . . ? C72 C71 C76 C75 1.4(4) . . . . ? B59 C71 C76 C75 172.9(2) . . . . ? C71 B59 C82 C83 55.7(3) . . . . ? C60 B59 C82 C83 -67.4(3) . . . . ? C93 B59 C82 C83 170.7(2) . . . . ? C71 B59 C82 C87 -133.5(2) . . . . ? C60 B59 C82 C87 103.4(3) . . . . ? C93 B59 C82 C87 -18.5(3) . . . . ? C87 C82 C83 F88 -177.2(2) . . . . ? B59 C82 C83 F88 -5.2(3) . . . . ? C87 C82 C83 C84 2.9(4) . . . . ? B59 C82 C83 C84 175.0(2) . . . . ? F88 C83 C84 F89 -2.1(3) . . . . ? C82 C83 C84 F89 177.8(2) . . . . ? F88 C83 C84 C85 177.6(2) . . . . ? C82 C83 C84 C85 -2.5(4) . . . . ? F89 C84 C85 F90 0.2(4) . . . . ? C83 C84 C85 F90 -179.5(2) . . . . ? F89 C84 C85 C86 179.9(2) . . . . ? C83 C84 C85 C86 0.2(4) . . . . ? F90 C85 C86 F91 1.9(3) . . . . ? C84 C85 C86 F91 -177.8(2) . . . . ? F90 C85 C86 C87 -179.0(2) . . . . ? C84 C85 C86 C87 1.3(4) . . . . ? F91 C86 C87 F92 -1.4(3) . . . . ? C85 C86 C87 F92 179.5(2) . . . . ? F91 C86 C87 C82 178.3(2) . . . . ? C85 C86 C87 C82 -0.8(4) . . . . ? C83 C82 C87 F92 178.5(2) . . . . ? B59 C82 C87 F92 7.3(4) . . . . ? C83 C82 C87 C86 -1.2(3) . . . . ? B59 C82 C87 C86 -172.5(2) . . . . ? C71 B59 C93 C98 63.7(3) . . . . ? C60 B59 C93 C98 -172.7(2) . . . . ? C82 B59 C93 C98 -58.3(3) . . . . ? C71 B59 C93 C94 -105.2(3) . . . . ? C60 B59 C93 C94 18.5(3) . . . . ? C82 B59 C93 C94 132.9(2) . . . . ? C98 C93 C94 F99 -179.2(2) . . . . ? B59 C93 C94 F99 -9.7(4) . . . . ? C98 C93 C94 C95 0.7(4) . . . . ? B59 C93 C94 C95 170.2(2) . . . . ? F99 C94 C95 F100 -0.8(4) . . . . ? C93 C94 C95 F100 179.2(2) . . . . ? F99 C94 C95 C96 179.3(2) . . . . ? C93 C94 C95 C96 -0.7(4) . . . . ? F100 C95 C96 F101 -1.0(4) . . . . ? C94 C95 C96 F101 178.9(2) . . . . ? F100 C95 C96 C97 -179.7(2) . . . . ? C94 C95 C96 C97 0.2(4) . . . . ? F101 C96 C97 F102 1.0(4) . . . . ? C95 C96 C97 F102 179.7(2) . . . . ? F101 C96 C97 C98 -178.6(2) . . . . ? C95 C96 C97 C98 0.1(4) . . . . ? F102 C97 C98 F103 1.1(4) . . . . ? C96 C97 C98 F103 -179.4(2) . . . . ? F102 C97 C98 C93 -179.6(2) . . . . ? C96 C97 C98 C93 0.0(4) . . . . ? C94 C93 C98 F103 178.9(2) . . . . ? B59 C93 C98 F103 8.8(3) . . . . ? C94 C93 C98 C97 -0.4(4) . . . . ? B59 C93 C98 C97 -170.6(2) . . . . ? C104 C105 O106 C107 179.4(3) . . . . ? C105 O106 C107 C108 -179.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.366 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.059