# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Li, Yuesheng' _publ_contact_author_email ysli@ciac.jl.cn _publ_section_title ; Novel heteroligated titanium complexes with fluorinated salicylaldiminato and b-enaminoketonato ligands: synthesis, characterization and catalytic behavior of vinyl addition polymerization of norbornene ; loop_ _publ_author_name 'Yingyun Long' 'Weping Ye' 'Ping Tao' 'Yuesheng Li' # Attachment '- 3d,3f_and_3g.cif' data_3d _database_code_depnum_ccdc_archive 'CCDC 791299' #TrackingRef '- 3d,3f_and_3g.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H28 Cl4 F8 N2 O2 Ti' _chemical_formula_weight 886.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.6015(7) _cell_length_b 15.5255(7) _cell_length_c 17.1760(8) _cell_angle_alpha 90.00 _cell_angle_beta 97.2350(10) _cell_angle_gamma 90.00 _cell_volume 3862.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used 9914 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 26.17 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.574 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8793 _exptl_absorpt_correction_T_max 0.9502 _exptl_absorpt_process_details (SADABS) _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21431 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 26.24 _reflns_number_total 7736 _reflns_number_gt 6074 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0874P)^2^+3.8371P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7736 _refine_ls_number_parameters 499 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0660 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1624 _refine_ls_wR_factor_gt 0.1496 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.18919(3) 0.80351(3) 0.23841(3) 0.02477(15) Uani 1 1 d . . . C1 C 0.22851(19) 0.69747(18) 0.09900(16) 0.0264(6) Uani 1 1 d . . . C2 C 0.2553(2) 0.70883(19) 0.02413(17) 0.0295(6) Uani 1 1 d . . . C3 C 0.2598(2) 0.6339(2) -0.01976(18) 0.0359(7) Uani 1 1 d . . . H3 H 0.2759 0.6387 -0.0715 0.043 Uiso 1 1 calc R . . C4 C 0.2419(2) 0.5521(2) 0.00852(19) 0.0397(8) Uani 1 1 d . . . H4 H 0.2432 0.5032 -0.0246 0.048 Uiso 1 1 calc R . . C5 C 0.2225(2) 0.5424(2) 0.08395(18) 0.0357(7) Uani 1 1 d . . . H5 H 0.2138 0.4866 0.1044 0.043 Uiso 1 1 calc R . . C6 C 0.2157(2) 0.61561(18) 0.13069(17) 0.0283(6) Uani 1 1 d . . . C7 C 0.2794(2) 0.7973(2) -0.00629(17) 0.0341(7) Uani 1 1 d . . . C8 C 0.3586(2) 0.8375(2) 0.0506(2) 0.0423(8) Uani 1 1 d . . . H8A H 0.3382 0.8452 0.1023 0.063 Uiso 1 1 calc R . . H8B H 0.3754 0.8935 0.0302 0.063 Uiso 1 1 calc R . . H8C H 0.4124 0.7992 0.0551 0.063 Uiso 1 1 calc R . . C9 C 0.1955(3) 0.8566(2) -0.0146(2) 0.0423(8) Uani 1 1 d . . . H9A H 0.1442 0.8286 -0.0473 0.063 Uiso 1 1 calc R . . H9B H 0.2108 0.9108 -0.0392 0.063 Uiso 1 1 calc R . . H9C H 0.1775 0.8685 0.0375 0.063 Uiso 1 1 calc R . . C10 C 0.3141(3) 0.7909(2) -0.08675(19) 0.0460(9) Uani 1 1 d . . . H10A H 0.3695 0.7546 -0.0825 0.069 Uiso 1 1 calc R . . H10B H 0.3292 0.8485 -0.1045 0.069 Uiso 1 1 calc R . . H10C H 0.2659 0.7653 -0.1246 0.069 Uiso 1 1 calc R . . C11 C 0.20414(19) 0.60374(19) 0.21188(17) 0.0283(6) Uani 1 1 d . . . H11 H 0.1988 0.5461 0.2294 0.034 Uiso 1 1 calc R . . C12 C 0.2042(2) 0.63515(18) 0.34349(17) 0.0287(6) Uani 1 1 d . . . C13 C 0.1255(2) 0.6259(2) 0.38012(19) 0.0337(7) Uani 1 1 d . . . C14 C 0.1302(2) 0.6003(2) 0.45710(19) 0.0370(7) Uani 1 1 d . . . C15 C 0.2142(2) 0.5831(2) 0.49942(18) 0.0371(7) Uani 1 1 d . . . C16 C 0.2936(2) 0.5924(2) 0.46466(18) 0.0336(7) Uani 1 1 d . . . C17 C 0.2882(2) 0.61933(18) 0.38785(17) 0.0283(6) Uani 1 1 d . . . C18 C 0.0105(2) 0.7319(2) 0.14349(18) 0.0316(6) Uani 1 1 d . . . C19 C -0.0123(2) 0.6462(2) 0.1512(2) 0.0379(7) Uani 1 1 d . . . H19 H -0.0107 0.6213 0.2019 0.046 Uiso 1 1 calc R . . C20 C -0.0377(2) 0.5965(2) 0.0845(2) 0.0490(9) Uani 1 1 d . . . H20 H -0.0534 0.5376 0.0897 0.059 Uiso 1 1 calc R . . C21 C -0.0399(3) 0.6329(3) 0.0110(2) 0.0534(10) Uani 1 1 d . . . H21 H -0.0571 0.5989 -0.0345 0.064 Uiso 1 1 calc R . . C22 C -0.0172(3) 0.7182(3) 0.0035(2) 0.0513(10) Uani 1 1 d . . . H22 H -0.0190 0.7431 -0.0472 0.062 Uiso 1 1 calc R . . C23 C 0.0084(2) 0.7683(2) 0.06979(19) 0.0397(8) Uani 1 1 d . . . H23 H 0.0245 0.8271 0.0645 0.048 Uiso 1 1 calc R . . C24 C -0.0178(2) 0.81831(19) 0.25444(18) 0.0306(6) Uani 1 1 d . . . C25 C -0.1209(2) 0.8181(3) 0.22347(19) 0.0442(9) Uani 1 1 d . . . C26 C 0.0031(2) 0.8532(2) 0.32983(18) 0.0315(6) Uani 1 1 d . . . H26 H -0.0418 0.8875 0.3507 0.038 Uiso 1 1 calc R . . C27 C 0.0874(2) 0.83929(18) 0.37478(17) 0.0274(6) Uani 1 1 d . . . C28 C 0.1031(2) 0.85153(18) 0.46073(17) 0.0276(6) Uani 1 1 d . . . C29 C 0.0344(2) 0.8760(2) 0.50353(18) 0.0333(7) Uani 1 1 d . . . H29 H -0.0255 0.8877 0.4772 0.040 Uiso 1 1 calc R . . C30 C 0.0506(2) 0.8842(2) 0.58575(18) 0.0358(7) Uani 1 1 d . . . C31 C -0.0201(3) 0.9073(3) 0.6309(2) 0.0496(9) Uani 1 1 d . . . H31 H -0.0807 0.9184 0.6056 0.060 Uiso 1 1 calc R . . C32 C -0.0020(3) 0.9138(3) 0.7103(2) 0.0625(12) Uani 1 1 d . . . H32 H -0.0504 0.9278 0.7402 0.075 Uiso 1 1 calc R . . C33 C 0.0866(3) 0.9001(3) 0.7483(2) 0.0662(13) Uani 1 1 d . . . H33 H 0.0982 0.9060 0.8037 0.079 Uiso 1 1 calc R . . C34 C 0.1563(3) 0.8786(3) 0.7074(2) 0.0577(11) Uani 1 1 d . . . H34 H 0.2167 0.8702 0.7342 0.069 Uiso 1 1 calc R . . C35 C 0.1400(3) 0.8685(2) 0.62423(18) 0.0387(7) Uani 1 1 d . . . C36 C 0.2107(2) 0.8435(2) 0.57923(19) 0.0407(8) Uani 1 1 d . . . H36 H 0.2713 0.8328 0.6047 0.049 Uiso 1 1 calc R . . C37 C 0.1926(2) 0.8348(2) 0.49998(18) 0.0328(7) Uani 1 1 d . . . H37 H 0.2404 0.8172 0.4707 0.039 Uiso 1 1 calc R . . C38 C 0.0578(4) 0.6465(4) 0.7197(3) 0.0735(13) Uani 1 1 d . . . H38A H 0.0014 0.6819 0.7078 0.088 Uiso 1 1 calc R . . H38B H 0.1056 0.6700 0.6895 0.088 Uiso 1 1 calc R . . Cl1 Cl 0.33921(5) 0.82841(6) 0.29117(5) 0.0384(2) Uani 1 1 d . . . Cl2 Cl 0.15714(6) 0.94187(5) 0.20184(5) 0.0368(2) Uani 1 1 d . . . Cl3 Cl 0.09722(10) 0.65284(11) 0.82078(8) 0.0925(5) Uani 1 1 d . . . Cl4 Cl 0.03357(13) 0.54065(10) 0.69109(9) 0.0987(5) Uani 1 1 d . . . F1 F 0.04253(13) 0.64324(13) 0.34097(12) 0.0442(5) Uani 1 1 d . . . F2 F 0.05302(15) 0.59271(15) 0.49058(12) 0.0544(6) Uani 1 1 d . . . F3 F 0.21879(16) 0.55711(14) 0.57411(11) 0.0495(5) Uani 1 1 d . . . F4 F 0.37552(14) 0.57324(13) 0.50456(11) 0.0445(5) Uani 1 1 d . . . F5 F 0.36637(12) 0.62886(11) 0.35619(10) 0.0347(4) Uani 1 1 d . . . F6 F -0.15702(14) 0.74023(17) 0.23055(13) 0.0608(6) Uani 1 1 d . . . F7 F -0.13760(16) 0.8390(2) 0.14871(13) 0.0830(10) Uani 1 1 d . . . F8 F -0.16849(14) 0.87224(16) 0.26364(13) 0.0584(6) Uani 1 1 d . . . N1 N 0.20038(16) 0.66430(15) 0.26359(14) 0.0268(5) Uani 1 1 d . . . N2 N 0.04201(16) 0.78225(15) 0.21247(14) 0.0272(5) Uani 1 1 d . . . O1 O 0.21500(13) 0.76561(12) 0.14370(11) 0.0265(4) Uani 1 1 d . . . O2 O 0.15686(14) 0.80929(13) 0.34390(12) 0.0291(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0244(3) 0.0256(3) 0.0250(3) -0.00271(19) 0.0057(2) -0.0024(2) C1 0.0232(13) 0.0299(14) 0.0248(14) -0.0058(11) -0.0014(11) 0.0024(11) C2 0.0271(14) 0.0342(16) 0.0263(14) -0.0013(12) -0.0004(12) 0.0023(12) C3 0.0419(18) 0.0399(17) 0.0249(15) -0.0038(13) 0.0003(13) 0.0041(14) C4 0.051(2) 0.0335(17) 0.0329(16) -0.0096(13) -0.0013(15) 0.0020(15) C5 0.0405(18) 0.0308(16) 0.0345(16) -0.0037(13) -0.0010(14) 0.0009(13) C6 0.0268(14) 0.0276(14) 0.0292(14) -0.0033(11) -0.0016(12) 0.0001(11) C7 0.0396(17) 0.0368(17) 0.0266(15) -0.0001(12) 0.0069(13) -0.0009(14) C8 0.0438(19) 0.0456(19) 0.0381(18) -0.0025(15) 0.0079(15) -0.0130(16) C9 0.050(2) 0.0382(18) 0.0403(18) 0.0081(14) 0.0111(16) 0.0037(15) C10 0.059(2) 0.050(2) 0.0312(17) 0.0002(15) 0.0139(16) -0.0014(17) C11 0.0259(14) 0.0250(14) 0.0330(15) 0.0001(12) -0.0004(12) -0.0006(11) C12 0.0335(16) 0.0260(14) 0.0271(14) -0.0002(11) 0.0058(12) 0.0002(12) C13 0.0312(16) 0.0339(16) 0.0362(16) 0.0043(13) 0.0044(13) -0.0017(13) C14 0.0421(18) 0.0343(16) 0.0372(17) 0.0034(13) 0.0152(14) -0.0009(14) C15 0.052(2) 0.0334(16) 0.0265(15) 0.0020(12) 0.0076(14) -0.0034(14) C16 0.0396(17) 0.0307(15) 0.0289(15) -0.0042(12) -0.0021(13) 0.0001(13) C17 0.0319(15) 0.0272(14) 0.0267(14) -0.0046(11) 0.0071(12) -0.0017(12) C18 0.0233(14) 0.0379(16) 0.0328(15) -0.0014(13) 0.0005(12) -0.0022(12) C19 0.0297(16) 0.0371(17) 0.0447(18) -0.0007(14) -0.0047(14) -0.0029(13) C20 0.0370(19) 0.043(2) 0.064(2) -0.0115(17) -0.0055(17) -0.0060(15) C21 0.041(2) 0.065(3) 0.051(2) -0.0233(19) -0.0058(17) -0.0044(18) C22 0.042(2) 0.077(3) 0.0325(18) -0.0040(17) -0.0031(15) -0.0039(19) C23 0.0323(17) 0.049(2) 0.0353(17) 0.0021(14) -0.0035(13) -0.0036(14) C24 0.0254(15) 0.0340(16) 0.0324(15) 0.0097(12) 0.0034(12) -0.0020(12) C25 0.0301(17) 0.075(3) 0.0280(16) 0.0098(16) 0.0070(13) 0.0080(17) C26 0.0290(15) 0.0350(16) 0.0321(15) 0.0013(12) 0.0103(12) 0.0016(12) C27 0.0293(15) 0.0240(14) 0.0298(15) 0.0012(11) 0.0080(12) -0.0031(11) C28 0.0303(15) 0.0244(14) 0.0290(14) 0.0003(11) 0.0078(12) -0.0011(11) C29 0.0303(16) 0.0384(17) 0.0316(15) -0.0028(13) 0.0050(13) 0.0012(13) C30 0.0408(18) 0.0367(16) 0.0318(16) -0.0012(13) 0.0120(14) 0.0054(14) C31 0.048(2) 0.065(2) 0.0389(19) -0.0041(17) 0.0153(16) 0.0145(18) C32 0.074(3) 0.075(3) 0.042(2) -0.0044(19) 0.025(2) 0.028(2) C33 0.090(3) 0.081(3) 0.0285(18) 0.0000(18) 0.012(2) 0.040(3) C34 0.066(3) 0.076(3) 0.0299(18) 0.0052(17) 0.0030(18) 0.031(2) C35 0.049(2) 0.0386(18) 0.0292(16) 0.0019(13) 0.0080(14) 0.0119(15) C36 0.0404(18) 0.0491(19) 0.0321(16) 0.0066(14) 0.0027(14) 0.0134(15) C37 0.0327(16) 0.0368(16) 0.0304(15) 0.0037(12) 0.0094(13) 0.0052(13) C38 0.065(3) 0.095(4) 0.059(3) 0.010(3) 0.003(2) -0.001(3) Cl1 0.0265(4) 0.0512(5) 0.0374(4) -0.0079(3) 0.0033(3) -0.0066(3) Cl2 0.0408(4) 0.0248(4) 0.0465(4) 0.0005(3) 0.0119(3) -0.0017(3) Cl3 0.0780(9) 0.1208(12) 0.0720(8) -0.0031(8) -0.0172(7) -0.0132(8) Cl4 0.1371(14) 0.0820(9) 0.0759(9) -0.0013(7) 0.0086(9) -0.0109(9) F1 0.0301(10) 0.0530(12) 0.0495(11) 0.0152(9) 0.0050(8) -0.0003(8) F2 0.0480(12) 0.0685(14) 0.0508(12) 0.0149(10) 0.0225(10) -0.0016(11) F3 0.0650(14) 0.0568(13) 0.0272(10) 0.0064(8) 0.0081(9) -0.0044(10) F4 0.0444(11) 0.0527(12) 0.0331(10) 0.0020(8) -0.0077(8) 0.0007(9) F5 0.0308(9) 0.0396(10) 0.0335(9) -0.0018(7) 0.0041(7) 0.0010(7) F6 0.0370(11) 0.0893(18) 0.0562(13) -0.0170(12) 0.0061(10) -0.0251(12) F7 0.0418(13) 0.170(3) 0.0381(12) 0.0394(15) 0.0074(10) 0.0375(16) F8 0.0309(11) 0.0857(17) 0.0586(13) -0.0045(12) 0.0055(10) 0.0170(11) N1 0.0255(12) 0.0290(12) 0.0256(12) -0.0001(10) 0.0023(10) 0.0000(10) N2 0.0258(12) 0.0288(12) 0.0271(12) 0.0011(10) 0.0035(10) -0.0030(10) O1 0.0288(10) 0.0252(10) 0.0259(10) -0.0012(8) 0.0050(8) -0.0007(8) O2 0.0254(10) 0.0349(11) 0.0278(10) -0.0039(8) 0.0057(8) 0.0001(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O1 1.814(2) . ? Ti1 O2 1.931(2) . ? Ti1 N2 2.164(2) . ? Ti1 N1 2.206(2) . ? Ti1 Cl2 2.2702(9) . ? Ti1 Cl1 2.2955(9) . ? C1 O1 1.336(3) . ? C1 C2 1.402(4) . ? C1 C6 1.405(4) . ? C2 C3 1.392(4) . ? C2 C7 1.527(4) . ? C3 C4 1.396(5) . ? C3 H3 0.9500 . ? C4 C5 1.369(5) . ? C4 H4 0.9500 . ? C5 C6 1.402(4) . ? C5 H5 0.9500 . ? C6 C11 1.437(4) . ? C7 C9 1.525(5) . ? C7 C10 1.534(4) . ? C7 C8 1.547(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N1 1.299(4) . ? C11 H11 0.9500 . ? C12 C17 1.381(4) . ? C12 C13 1.386(4) . ? C12 N1 1.439(4) . ? C13 F1 1.337(4) . ? C13 C14 1.374(4) . ? C14 F2 1.333(4) . ? C14 C15 1.371(5) . ? C15 F3 1.338(4) . ? C15 C16 1.377(5) . ? C16 F4 1.335(4) . ? C16 C17 1.377(4) . ? C17 F5 1.334(3) . ? C18 C19 1.382(5) . ? C18 C23 1.383(4) . ? C18 N2 1.445(4) . ? C19 C20 1.392(5) . ? C19 H19 0.9500 . ? C20 C21 1.381(6) . ? C20 H20 0.9500 . ? C21 C22 1.376(6) . ? C21 H21 0.9500 . ? C22 C23 1.390(5) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 N2 1.325(4) . ? C24 C26 1.402(4) . ? C24 C25 1.532(4) . ? C25 F7 1.317(4) . ? C25 F6 1.331(5) . ? C25 F8 1.336(4) . ? C26 C27 1.385(4) . ? C26 H26 0.9500 . ? C27 O2 1.289(4) . ? C27 C28 1.477(4) . ? C28 C29 1.370(4) . ? C28 C37 1.417(4) . ? C29 C30 1.408(4) . ? C29 H29 0.9500 . ? C30 C35 1.408(5) . ? C30 C31 1.414(5) . ? C31 C32 1.360(5) . ? C31 H31 0.9500 . ? C32 C33 1.389(6) . ? C32 H32 0.9500 . ? C33 C34 1.350(6) . ? C33 H33 0.9500 . ? C34 C35 1.427(5) . ? C34 H34 0.9500 . ? C35 C36 1.419(5) . ? C36 C37 1.360(4) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 Cl4 1.739(6) . ? C38 Cl3 1.761(5) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ti1 O2 163.67(9) . . ? O1 Ti1 N2 94.53(9) . . ? O2 Ti1 N2 81.17(9) . . ? O1 Ti1 N1 80.76(9) . . ? O2 Ti1 N1 83.25(9) . . ? N2 Ti1 N1 86.45(9) . . ? O1 Ti1 Cl2 96.75(7) . . ? O2 Ti1 Cl2 98.59(7) . . ? N2 Ti1 Cl2 85.56(7) . . ? N1 Ti1 Cl2 171.42(7) . . ? O1 Ti1 Cl1 96.48(7) . . ? O2 Ti1 Cl1 87.46(6) . . ? N2 Ti1 Cl1 168.63(7) . . ? N1 Ti1 Cl1 92.53(7) . . ? Cl2 Ti1 Cl1 95.92(4) . . ? O1 C1 C2 120.4(3) . . ? O1 C1 C6 117.2(3) . . ? C2 C1 C6 122.4(3) . . ? C3 C2 C1 115.4(3) . . ? C3 C2 C7 122.5(3) . . ? C1 C2 C7 122.0(3) . . ? C2 C3 C4 123.2(3) . . ? C2 C3 H3 118.4 . . ? C4 C3 H3 118.4 . . ? C5 C4 C3 120.0(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 119.4(3) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C5 C6 C1 119.3(3) . . ? C5 C6 C11 118.5(3) . . ? C1 C6 C11 122.0(3) . . ? C9 C7 C2 110.9(3) . . ? C9 C7 C10 108.0(3) . . ? C2 C7 C10 111.5(3) . . ? C9 C7 C8 110.1(3) . . ? C2 C7 C8 109.5(3) . . ? C10 C7 C8 106.8(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C6 126.2(3) . . ? N1 C11 H11 116.9 . . ? C6 C11 H11 116.9 . . ? C17 C12 C13 117.4(3) . . ? C17 C12 N1 120.5(3) . . ? C13 C12 N1 122.0(3) . . ? F1 C13 C14 118.3(3) . . ? F1 C13 C12 120.1(3) . . ? C14 C13 C12 121.5(3) . . ? F2 C14 C15 120.2(3) . . ? F2 C14 C13 119.9(3) . . ? C15 C14 C13 120.0(3) . . ? F3 C15 C14 120.0(3) . . ? F3 C15 C16 120.3(3) . . ? C14 C15 C16 119.7(3) . . ? F4 C16 C17 120.0(3) . . ? F4 C16 C15 120.2(3) . . ? C17 C16 C15 119.8(3) . . ? F5 C17 C16 118.4(3) . . ? F5 C17 C12 120.1(3) . . ? C16 C17 C12 121.5(3) . . ? C19 C18 C23 120.2(3) . . ? C19 C18 N2 119.9(3) . . ? C23 C18 N2 119.8(3) . . ? C18 C19 C20 119.8(3) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C21 C20 C19 119.9(3) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C22 C21 C20 120.1(3) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 120.4(4) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C18 C23 C22 119.6(3) . . ? C18 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? N2 C24 C26 125.7(3) . . ? N2 C24 C25 119.8(3) . . ? C26 C24 C25 114.3(3) . . ? F7 C25 F6 106.6(3) . . ? F7 C25 F8 107.7(3) . . ? F6 C25 F8 106.7(3) . . ? F7 C25 C24 113.0(3) . . ? F6 C25 C24 110.7(3) . . ? F8 C25 C24 111.8(3) . . ? C27 C26 C24 122.0(3) . . ? C27 C26 H26 119.0 . . ? C24 C26 H26 119.0 . . ? O2 C27 C26 121.1(3) . . ? O2 C27 C28 115.2(3) . . ? C26 C27 C28 123.5(3) . . ? C29 C28 C37 119.3(3) . . ? C29 C28 C27 122.7(3) . . ? C37 C28 C27 118.0(3) . . ? C28 C29 C30 121.4(3) . . ? C28 C29 H29 119.3 . . ? C30 C29 H29 119.3 . . ? C29 C30 C35 119.0(3) . . ? C29 C30 C31 122.0(3) . . ? C35 C30 C31 119.0(3) . . ? C32 C31 C30 120.3(4) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C31 C32 C33 120.8(4) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C34 C33 C32 120.8(4) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C33 C34 C35 120.4(4) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C30 C35 C36 119.1(3) . . ? C30 C35 C34 118.6(3) . . ? C36 C35 C34 122.3(3) . . ? C37 C36 C35 120.6(3) . . ? C37 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C36 C37 C28 120.6(3) . . ? C36 C37 H37 119.7 . . ? C28 C37 H37 119.7 . . ? Cl4 C38 Cl3 111.2(3) . . ? Cl4 C38 H38A 109.4 . . ? Cl3 C38 H38A 109.4 . . ? Cl4 C38 H38B 109.4 . . ? Cl3 C38 H38B 109.4 . . ? H38A C38 H38B 108.0 . . ? C11 N1 C12 115.1(2) . . ? C11 N1 Ti1 125.7(2) . . ? C12 N1 Ti1 119.20(18) . . ? C24 N2 C18 120.7(2) . . ? C24 N2 Ti1 122.0(2) . . ? C18 N2 Ti1 117.18(19) . . ? C1 O1 Ti1 146.57(19) . . ? C27 O2 Ti1 134.48(19) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.24 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.099 _refine_diff_density_min -0.914 _refine_diff_density_rms 0.077 # Attachment '3f.cif' data_lyy5 _database_code_depnum_ccdc_archive 'CCDC 791300' #TrackingRef '3f.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H22 Cl4 F8 N2 O2 Ti' _chemical_formula_weight 820.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.5344(5) _cell_length_b 12.2293(4) _cell_length_c 20.8540(8) _cell_angle_alpha 90.00 _cell_angle_beta 99.9460(10) _cell_angle_gamma 90.00 _cell_volume 3399.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7615 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 26.06 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 0.645 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8105 _exptl_absorpt_correction_T_max 0.9324 _exptl_absorpt_process_details (SADABS) _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18614 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 26.07 _reflns_number_total 6720 _reflns_number_gt 5093 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0331P)^2^+1.2333P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6720 _refine_ls_number_parameters 454 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0855 _refine_ls_wR_factor_gt 0.0774 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.22155(3) 0.15160(3) 0.115619(18) 0.02291(10) Uani 1 1 d . . . C1 C 0.38516(15) 0.31356(16) 0.09946(10) 0.0225(5) Uani 1 1 d . . . C2 C 0.47431(16) 0.31883(17) 0.07337(10) 0.0248(5) Uani 1 1 d . . . C3 C 0.52181(17) 0.42012(18) 0.07793(11) 0.0324(5) Uani 1 1 d . . . H3 H 0.5798 0.4275 0.0600 0.039 Uiso 1 1 calc R . . C4 C 0.48769(18) 0.51089(19) 0.10775(12) 0.0380(6) Uani 1 1 d . . . H4 H 0.5208 0.5776 0.1079 0.046 Uiso 1 1 calc R . . C5 C 0.40491(18) 0.50131(18) 0.13695(12) 0.0347(6) Uani 1 1 d . . . H5 H 0.3836 0.5603 0.1592 0.042 Uiso 1 1 calc R . . C6 C 0.35256(16) 0.40193(17) 0.13312(10) 0.0253(5) Uani 1 1 d . . . C7 C 0.51887(16) 0.21822(18) 0.04460(11) 0.0279(5) Uani 1 1 d . . . C8 C 0.53844(18) 0.12819(19) 0.09685(12) 0.0352(6) Uani 1 1 d . . . H8A H 0.4758 0.1048 0.1080 0.053 Uiso 1 1 calc R . . H8B H 0.5808 0.1565 0.1349 0.053 Uiso 1 1 calc R . . H8C H 0.5709 0.0672 0.0802 0.053 Uiso 1 1 calc R . . C9 C 0.44705(18) 0.1760(2) -0.01519(12) 0.0398(6) Uani 1 1 d . . . H9A H 0.4321 0.2339 -0.0464 0.060 Uiso 1 1 calc R . . H9B H 0.3861 0.1512 -0.0023 0.060 Uiso 1 1 calc R . . H9C H 0.4779 0.1165 -0.0343 0.060 Uiso 1 1 calc R . . C10 C 0.61904(17) 0.2456(2) 0.02370(12) 0.0353(6) Uani 1 1 d . . . H10A H 0.6455 0.1813 0.0065 0.053 Uiso 1 1 calc R . . H10B H 0.6656 0.2714 0.0607 0.053 Uiso 1 1 calc R . . H10C H 0.6088 0.3015 -0.0091 0.053 Uiso 1 1 calc R . . C11 C 0.26889(16) 0.39384(17) 0.16658(10) 0.0256(5) Uani 1 1 d . . . H11 H 0.2538 0.4559 0.1888 0.031 Uiso 1 1 calc R . . C12 C 0.13513(16) 0.32652(17) 0.20778(10) 0.0242(5) Uani 1 1 d . . . C13 C 0.04872(17) 0.38391(18) 0.18375(10) 0.0292(5) Uani 1 1 d . . . C14 C -0.02479(17) 0.4015(2) 0.22097(12) 0.0346(6) Uani 1 1 d . . . C15 C -0.01281(18) 0.36105(19) 0.28298(12) 0.0349(6) Uani 1 1 d . . . C16 C 0.07264(19) 0.30504(19) 0.30813(11) 0.0340(6) Uani 1 1 d . . . C17 C 0.14550(18) 0.28796(18) 0.27075(11) 0.0308(5) Uani 1 1 d . . . C18 C 0.15517(16) 0.29334(18) -0.00760(10) 0.0270(5) Uani 1 1 d . . . C19 C 0.17569(17) 0.40339(19) 0.00218(11) 0.0328(5) Uani 1 1 d . . . H19 H 0.1585 0.4390 0.0381 0.039 Uiso 1 1 calc R . . C20 C 0.22200(19) 0.4604(2) -0.04178(12) 0.0401(6) Uani 1 1 d . . . H20 H 0.2355 0.5346 -0.0356 0.048 Uiso 1 1 calc R . . C21 C 0.24797(18) 0.4074(2) -0.09446(12) 0.0421(6) Uani 1 1 d . . . H21 H 0.2794 0.4456 -0.1238 0.051 Uiso 1 1 calc R . . C22 C 0.22761(19) 0.2977(2) -0.10390(12) 0.0421(6) Uani 1 1 d . . . H22 H 0.2451 0.2624 -0.1398 0.051 Uiso 1 1 calc R . . C23 C 0.18158(18) 0.2396(2) -0.06058(11) 0.0351(6) Uani 1 1 d . . . H23 H 0.1685 0.1653 -0.0669 0.042 Uiso 1 1 calc R . . C24 C 0.01255(17) 0.22232(17) 0.03229(10) 0.0266(5) Uani 1 1 d . . . C25 C -0.05558(18) 0.2754(2) -0.02592(12) 0.0345(6) Uani 1 1 d . . . C26 C -0.03956(17) 0.16243(18) 0.07442(11) 0.0306(5) Uani 1 1 d . . . H26 H -0.1090 0.1570 0.0635 0.037 Uiso 1 1 calc R . . C27 C 0.00668(16) 0.11256(17) 0.12986(11) 0.0264(5) Uani 1 1 d . . . C28 C -0.04834(16) 0.04299(19) 0.17057(10) 0.0284(5) Uani 1 1 d . . . C29 C -0.13709(18) 0.0709(2) 0.19168(12) 0.0364(6) Uani 1 1 d . . . C30 C -0.1845(2) -0.0017(2) 0.22738(12) 0.0472(7) Uani 1 1 d . . . H30 H -0.2437 0.0184 0.2412 0.057 Uiso 1 1 calc R . . C31 C -0.1439(2) -0.1034(2) 0.24226(13) 0.0498(7) Uani 1 1 d . . . H31 H -0.1760 -0.1528 0.2657 0.060 Uiso 1 1 calc R . . C32 C -0.0555(2) -0.1319(2) 0.22234(11) 0.0397(6) Uani 1 1 d . . . C33 C -0.00726(18) -0.05929(19) 0.18771(11) 0.0318(5) Uani 1 1 d . . . H33 H 0.0534 -0.0789 0.1757 0.038 Uiso 1 1 calc R . . Cl1 Cl 0.31306(4) 0.06681(5) 0.20370(3) 0.03594(15) Uani 1 1 d . . . Cl2 Cl 0.21501(5) 0.00922(5) 0.04583(3) 0.04215(16) Uani 1 1 d . . . Cl3 Cl -0.18945(5) 0.20069(6) 0.17745(3) 0.04976(18) Uani 1 1 d . . . Cl4 Cl -0.00293(7) -0.25925(6) 0.24106(3) 0.0591(2) Uani 1 1 d . . . F1 F 0.03573(10) 0.42530(12) 0.12345(6) 0.0434(4) Uani 1 1 d . . . F2 F -0.10816(11) 0.45667(14) 0.19633(7) 0.0554(4) Uani 1 1 d . . . F3 F -0.08474(11) 0.37719(13) 0.31891(7) 0.0530(4) Uani 1 1 d . . . F4 F 0.08586(13) 0.26834(12) 0.36947(7) 0.0557(4) Uani 1 1 d . . . F5 F 0.22979(11) 0.23672(12) 0.29759(7) 0.0491(4) Uani 1 1 d . . . F6 F -0.15228(10) 0.26626(13) -0.02232(7) 0.0512(4) Uani 1 1 d . . . F7 F -0.03870(12) 0.38131(12) -0.03039(8) 0.0589(5) Uani 1 1 d . . . F8 F -0.04370(12) 0.22932(15) -0.08141(7) 0.0634(5) Uani 1 1 d . . . N1 N 0.21200(13) 0.30937(14) 0.16913(8) 0.0230(4) Uani 1 1 d . . . N2 N 0.10996(13) 0.23248(14) 0.03976(8) 0.0252(4) Uani 1 1 d . . . O1 O 0.32824(10) 0.22304(11) 0.09323(7) 0.0233(3) Uani 1 1 d . . . O2 O 0.10271(11) 0.11603(12) 0.15011(7) 0.0282(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0218(2) 0.0208(2) 0.0277(2) 0.00073(16) 0.00872(16) -0.00239(16) C1 0.0243(11) 0.0211(11) 0.0222(11) 0.0030(9) 0.0042(9) -0.0030(9) C2 0.0242(11) 0.0274(12) 0.0235(11) 0.0025(9) 0.0058(9) -0.0016(9) C3 0.0271(12) 0.0337(13) 0.0392(14) 0.0013(11) 0.0138(10) -0.0065(10) C4 0.0338(14) 0.0268(13) 0.0564(16) -0.0004(12) 0.0158(12) -0.0103(10) C5 0.0382(14) 0.0230(12) 0.0455(15) -0.0040(11) 0.0144(12) -0.0016(10) C6 0.0260(12) 0.0225(11) 0.0291(12) 0.0013(9) 0.0100(9) -0.0011(9) C7 0.0254(12) 0.0305(12) 0.0300(12) -0.0029(10) 0.0113(10) -0.0017(10) C8 0.0349(14) 0.0293(13) 0.0444(15) -0.0009(11) 0.0150(11) 0.0059(10) C9 0.0336(14) 0.0517(16) 0.0360(14) -0.0117(12) 0.0114(11) -0.0073(12) C10 0.0275(13) 0.0437(14) 0.0379(14) -0.0035(11) 0.0146(11) -0.0017(11) C11 0.0294(12) 0.0220(11) 0.0264(12) -0.0018(9) 0.0075(9) 0.0020(9) C12 0.0254(11) 0.0227(11) 0.0266(12) -0.0033(9) 0.0105(9) -0.0018(9) C13 0.0307(13) 0.0329(13) 0.0247(12) 0.0006(10) 0.0065(10) -0.0003(10) C14 0.0254(12) 0.0415(14) 0.0380(14) -0.0043(11) 0.0083(11) 0.0051(11) C15 0.0340(14) 0.0376(14) 0.0387(14) -0.0036(11) 0.0219(11) -0.0007(11) C16 0.0492(15) 0.0307(13) 0.0267(13) 0.0032(10) 0.0194(11) 0.0012(11) C17 0.0354(13) 0.0272(12) 0.0314(13) 0.0026(10) 0.0098(10) 0.0063(10) C18 0.0222(11) 0.0345(13) 0.0243(12) 0.0065(10) 0.0043(9) -0.0022(9) C19 0.0353(13) 0.0317(13) 0.0325(13) 0.0040(10) 0.0085(11) -0.0015(10) C20 0.0401(15) 0.0371(14) 0.0429(15) 0.0130(12) 0.0064(12) -0.0060(11) C21 0.0316(14) 0.0610(18) 0.0351(14) 0.0190(13) 0.0092(11) -0.0026(12) C22 0.0370(14) 0.0639(18) 0.0273(13) -0.0005(12) 0.0106(11) -0.0015(13) C23 0.0351(14) 0.0416(14) 0.0287(13) -0.0014(11) 0.0056(11) -0.0028(11) C24 0.0297(12) 0.0239(11) 0.0264(12) -0.0030(9) 0.0052(10) 0.0002(9) C25 0.0293(13) 0.0396(14) 0.0357(14) 0.0033(11) 0.0084(11) 0.0011(11) C26 0.0243(12) 0.0336(13) 0.0350(13) -0.0003(11) 0.0079(10) -0.0062(10) C27 0.0245(12) 0.0248(11) 0.0318(12) -0.0045(10) 0.0101(10) -0.0039(9) C28 0.0248(12) 0.0359(13) 0.0255(12) -0.0028(10) 0.0068(9) -0.0095(10) C29 0.0290(13) 0.0447(15) 0.0367(14) -0.0061(11) 0.0089(11) -0.0096(11) C30 0.0327(15) 0.071(2) 0.0419(15) -0.0050(14) 0.0174(12) -0.0188(14) C31 0.0518(18) 0.0607(19) 0.0397(16) 0.0037(14) 0.0156(13) -0.0279(15) C32 0.0515(17) 0.0389(14) 0.0277(13) 0.0023(11) 0.0046(12) -0.0175(12) C33 0.0327(13) 0.0346(13) 0.0291(13) -0.0004(10) 0.0078(10) -0.0081(10) Cl1 0.0332(3) 0.0354(3) 0.0400(3) 0.0133(3) 0.0085(3) 0.0052(2) Cl2 0.0493(4) 0.0300(3) 0.0486(4) -0.0130(3) 0.0124(3) -0.0057(3) Cl3 0.0316(3) 0.0581(4) 0.0625(5) -0.0049(4) 0.0161(3) 0.0064(3) Cl4 0.0907(6) 0.0401(4) 0.0455(4) 0.0136(3) 0.0085(4) -0.0130(4) F1 0.0452(9) 0.0574(9) 0.0294(8) 0.0091(7) 0.0118(6) 0.0196(7) F2 0.0359(9) 0.0803(11) 0.0518(10) 0.0040(8) 0.0128(7) 0.0256(8) F3 0.0493(9) 0.0663(10) 0.0534(9) -0.0017(8) 0.0370(8) 0.0062(8) F4 0.0850(12) 0.0557(10) 0.0351(8) 0.0156(7) 0.0344(8) 0.0210(9) F5 0.0519(9) 0.0630(10) 0.0344(8) 0.0130(7) 0.0131(7) 0.0272(8) F6 0.0251(8) 0.0704(11) 0.0563(10) 0.0193(8) 0.0014(7) 0.0007(7) F7 0.0460(10) 0.0418(9) 0.0823(12) 0.0252(8) -0.0076(8) -0.0008(7) F8 0.0592(11) 0.0985(14) 0.0297(8) -0.0071(8) 0.0001(7) 0.0220(10) N1 0.0232(9) 0.0247(9) 0.0228(9) 0.0017(8) 0.0082(8) -0.0001(8) N2 0.0272(10) 0.0236(9) 0.0258(10) 0.0005(8) 0.0073(8) -0.0018(8) O1 0.0226(8) 0.0227(7) 0.0266(8) -0.0003(6) 0.0096(6) -0.0026(6) O2 0.0222(8) 0.0312(8) 0.0323(9) 0.0042(7) 0.0080(7) -0.0046(6) _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 O1 1.8164(14) . ? Ti1 O2 1.9218(14) . ? Ti1 N2 2.2219(18) . ? Ti1 N1 2.2439(17) . ? Ti1 Cl2 2.2612(7) . ? Ti1 Cl1 2.2797(7) . ? C1 O1 1.342(2) . ? C1 C6 1.401(3) . ? C1 C2 1.408(3) . ? C2 C3 1.391(3) . ? C2 C7 1.537(3) . ? C3 C4 1.390(3) . ? C3 H3 0.9300 . ? C4 C5 1.370(3) . ? C4 H4 0.9300 . ? C5 C6 1.402(3) . ? C5 H5 0.9300 . ? C6 C11 1.432(3) . ? C7 C9 1.532(3) . ? C7 C10 1.531(3) . ? C7 C8 1.539(3) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 N1 1.295(3) . ? C11 H11 0.9300 . ? C12 C17 1.379(3) . ? C12 C13 1.382(3) . ? C12 N1 1.437(2) . ? C13 F1 1.339(2) . ? C13 C14 1.380(3) . ? C14 F2 1.339(3) . ? C14 C15 1.368(3) . ? C15 F3 1.342(2) . ? C15 C16 1.368(3) . ? C16 F4 1.338(2) . ? C16 C17 1.375(3) . ? C17 F5 1.337(3) . ? C18 C19 1.382(3) . ? C18 C23 1.385(3) . ? C18 N2 1.454(3) . ? C19 C20 1.385(3) . ? C19 H19 0.9300 . ? C20 C21 1.373(4) . ? C20 H20 0.9300 . ? C21 C22 1.377(4) . ? C21 H21 0.9300 . ? C22 C23 1.380(3) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 N2 1.306(3) . ? C24 C26 1.421(3) . ? C24 C25 1.536(3) . ? C25 F8 1.321(3) . ? C25 F7 1.322(3) . ? C25 F6 1.329(3) . ? C26 C27 1.360(3) . ? C26 H26 0.9300 . ? C27 O2 1.296(2) . ? C27 C28 1.489(3) . ? C28 C33 1.390(3) . ? C28 C29 1.391(3) . ? C29 C30 1.386(3) . ? C29 Cl3 1.743(3) . ? C30 C31 1.373(4) . ? C30 H30 0.9300 . ? C31 C32 1.378(4) . ? C31 H31 0.9300 . ? C32 C33 1.378(3) . ? C32 Cl4 1.729(3) . ? C33 H33 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ti1 O2 163.53(6) . . ? O1 Ti1 N2 94.34(6) . . ? O2 Ti1 N2 81.79(6) . . ? O1 Ti1 N1 80.26(6) . . ? O2 Ti1 N1 83.38(6) . . ? N2 Ti1 N1 83.16(6) . . ? O1 Ti1 Cl2 98.59(5) . . ? O2 Ti1 Cl2 97.14(5) . . ? N2 Ti1 Cl2 86.46(5) . . ? N1 Ti1 Cl2 169.43(5) . . ? O1 Ti1 Cl1 94.62(5) . . ? O2 Ti1 Cl1 88.22(5) . . ? N2 Ti1 Cl1 169.75(5) . . ? N1 Ti1 Cl1 93.46(5) . . ? Cl2 Ti1 Cl1 97.11(3) . . ? O1 C1 C6 117.36(18) . . ? O1 C1 C2 121.08(18) . . ? C6 C1 C2 121.57(19) . . ? C3 C2 C1 115.5(2) . . ? C3 C2 C7 122.11(19) . . ? C1 C2 C7 122.30(19) . . ? C4 C3 C2 123.8(2) . . ? C4 C3 H3 118.1 . . ? C2 C3 H3 118.1 . . ? C5 C4 C3 119.4(2) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 119.5(2) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C5 C6 C1 119.82(19) . . ? C5 C6 C11 117.80(19) . . ? C1 C6 C11 122.33(19) . . ? C9 C7 C10 108.10(18) . . ? C9 C7 C2 110.54(19) . . ? C10 C7 C2 111.23(18) . . ? C9 C7 C8 110.03(19) . . ? C10 C7 C8 107.79(19) . . ? C2 C7 C8 109.11(17) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C6 126.93(19) . . ? N1 C11 H11 116.5 . . ? C6 C11 H11 116.5 . . ? C17 C12 C13 117.36(19) . . ? C17 C12 N1 121.30(19) . . ? C13 C12 N1 121.34(19) . . ? F1 C13 C14 118.6(2) . . ? F1 C13 C12 119.89(19) . . ? C14 C13 C12 121.5(2) . . ? F2 C14 C15 120.0(2) . . ? F2 C14 C13 120.3(2) . . ? C15 C14 C13 119.7(2) . . ? F3 C15 C14 119.7(2) . . ? F3 C15 C16 120.4(2) . . ? C14 C15 C16 119.9(2) . . ? F4 C16 C15 119.9(2) . . ? F4 C16 C17 120.0(2) . . ? C15 C16 C17 120.0(2) . . ? F5 C17 C16 118.5(2) . . ? F5 C17 C12 119.86(19) . . ? C16 C17 C12 121.5(2) . . ? C19 C18 C23 120.5(2) . . ? C19 C18 N2 119.72(19) . . ? C23 C18 N2 119.7(2) . . ? C18 C19 C20 119.7(2) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? C21 C20 C19 120.0(2) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 120.2(2) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C21 C22 C23 120.7(2) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C22 C23 C18 119.1(2) . . ? C22 C23 H23 120.5 . . ? C18 C23 H23 120.5 . . ? N2 C24 C26 125.0(2) . . ? N2 C24 C25 120.65(19) . . ? C26 C24 C25 114.3(2) . . ? F8 C25 F7 107.9(2) . . ? F8 C25 F6 106.5(2) . . ? F7 C25 F6 105.68(19) . . ? F8 C25 C24 111.40(19) . . ? F7 C25 C24 112.5(2) . . ? F6 C25 C24 112.51(19) . . ? C27 C26 C24 123.5(2) . . ? C27 C26 H26 118.3 . . ? C24 C26 H26 118.3 . . ? O2 C27 C26 123.4(2) . . ? O2 C27 C28 113.90(19) . . ? C26 C27 C28 122.6(2) . . ? C33 C28 C29 117.9(2) . . ? C33 C28 C27 116.3(2) . . ? C29 C28 C27 125.8(2) . . ? C30 C29 C28 121.2(2) . . ? C30 C29 Cl3 117.5(2) . . ? C28 C29 Cl3 121.15(18) . . ? C31 C30 C29 119.8(3) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C30 C31 C32 119.7(2) . . ? C30 C31 H31 120.1 . . ? C32 C31 H31 120.1 . . ? C31 C32 C33 120.7(2) . . ? C31 C32 Cl4 120.3(2) . . ? C33 C32 Cl4 119.0(2) . . ? C32 C33 C28 120.7(2) . . ? C32 C33 H33 119.7 . . ? C28 C33 H33 119.7 . . ? C11 N1 C12 113.57(17) . . ? C11 N1 Ti1 125.43(14) . . ? C12 N1 Ti1 120.92(13) . . ? C24 N2 C18 120.16(18) . . ? C24 N2 Ti1 126.18(14) . . ? C18 N2 Ti1 113.42(13) . . ? C1 O1 Ti1 147.18(13) . . ? C27 O2 Ti1 137.95(14) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.07 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.296 _refine_diff_density_min -0.355 _refine_diff_density_rms 0.053 # Attachment '3g.cif' data_lyy1 _database_code_depnum_ccdc_archive 'CCDC 791301' #TrackingRef '3g.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H22 Cl2 F12 N2 O3 Ti' _chemical_formula_weight 853.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.5519(8) _cell_length_b 11.7525(5) _cell_length_c 27.6927(11) _cell_angle_alpha 90.00 _cell_angle_beta 96.1620(10) _cell_angle_gamma 90.00 _cell_volume 6973.7(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9111 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 26.05 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.626 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3424 _exptl_absorpt_coefficient_mu 0.502 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8559 _exptl_absorpt_correction_T_max 0.9469 _exptl_absorpt_process_details (SADABS) _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38066 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 0.95 _diffrn_reflns_theta_max 26.08 _reflns_number_total 13799 _reflns_number_gt 10462 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0570P)^2^+7.3087P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13799 _refine_ls_number_parameters 969 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1278 _refine_ls_wR_factor_gt 0.1159 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.002 _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 0.11422(2) 0.39579(4) 0.118876(16) 0.02469(11) Uani 1 1 d . . . Ti2 Ti 0.36776(2) 0.59123(4) 0.630477(18) 0.02779(12) Uani 1 1 d . . . C1 C 0.10872(12) 0.2204(2) 0.19860(9) 0.0253(6) Uani 1 1 d . . . C2 C 0.07243(13) 0.1923(2) 0.23644(10) 0.0302(6) Uani 1 1 d . . . C3 C 0.09213(15) 0.0956(2) 0.26350(10) 0.0362(7) Uani 1 1 d . . . H3 H 0.0695 0.0736 0.2887 0.043 Uiso 1 1 calc R . . C4 C 0.14376(15) 0.0309(3) 0.25465(11) 0.0384(7) Uani 1 1 d . . . H4 H 0.1541 -0.0339 0.2731 0.046 Uiso 1 1 calc R . . C5 C 0.17930(13) 0.0624(2) 0.21886(11) 0.0335(6) Uani 1 1 d . . . H5 H 0.2143 0.0201 0.2132 0.040 Uiso 1 1 calc R . . C6 C 0.16271(12) 0.1589(2) 0.19071(9) 0.0266(6) Uani 1 1 d . . . C7 C 0.01785(14) 0.2665(3) 0.24919(11) 0.0370(7) Uani 1 1 d . . . C8 C -0.01468(17) 0.2138(3) 0.29073(13) 0.0499(9) Uani 1 1 d . . . H8A H -0.0295 0.1391 0.2815 0.060 Uiso 1 1 calc R . . H8B H -0.0492 0.2608 0.2972 0.060 Uiso 1 1 calc R . . H8C H 0.0145 0.2087 0.3194 0.060 Uiso 1 1 calc R . . C9 C -0.03189(15) 0.2816(3) 0.20564(12) 0.0476(8) Uani 1 1 d . . . H9A H -0.0136 0.3184 0.1796 0.057 Uiso 1 1 calc R . . H9B H -0.0654 0.3274 0.2151 0.057 Uiso 1 1 calc R . . H9C H -0.0477 0.2084 0.1950 0.057 Uiso 1 1 calc R . . C10 C 0.0440(2) 0.3844(3) 0.26555(17) 0.0693(8) Uani 1 1 d . . . H10A H 0.0733 0.3759 0.2939 0.083 Uiso 1 1 calc R . . H10B H 0.0103 0.4327 0.2730 0.083 Uiso 1 1 calc R . . H10C H 0.0645 0.4180 0.2399 0.083 Uiso 1 1 calc R . . C11 C 0.20385(12) 0.1947(2) 0.15590(9) 0.0269(6) Uani 1 1 d . . . H11 H 0.2396 0.1511 0.1544 0.032 Uiso 1 1 calc R . . C12 C 0.25036(13) 0.3001(2) 0.10037(10) 0.0298(6) Uani 1 1 d . . . C13 C 0.25238(14) 0.2650(3) 0.05284(11) 0.0384(7) Uani 1 1 d . . . C14 C 0.30522(17) 0.2781(3) 0.02933(12) 0.0492(9) Uani 1 1 d . . . C15 C 0.35725(15) 0.3282(3) 0.05298(13) 0.0497(9) Uani 1 1 d . . . C16 C 0.35648(14) 0.3659(3) 0.09999(12) 0.0418(7) Uani 1 1 d . . . C17 C 0.30358(13) 0.3521(2) 0.12332(10) 0.0329(6) Uani 1 1 d . . . C18 C 0.06022(14) 0.1590(2) 0.08319(10) 0.0316(6) Uani 1 1 d . . . C19 C 0.00338(16) 0.1486(3) 0.10197(12) 0.0475(8) Uani 1 1 d . . . H19 H -0.0240 0.2099 0.1010 0.057 Uiso 1 1 calc R . . C20 C -0.0120(2) 0.0464(4) 0.12204(14) 0.0654(12) Uani 1 1 d . . . H20 H -0.0503 0.0383 0.1343 0.078 Uiso 1 1 calc R . . C21 C 0.0290(2) -0.0434(3) 0.12402(12) 0.0658(13) Uani 1 1 d . . . H21 H 0.0186 -0.1117 0.1381 0.079 Uiso 1 1 calc R . . C22 C 0.0849(2) -0.0327(3) 0.10541(12) 0.0554(10) Uani 1 1 d . . . H22 H 0.1123 -0.0940 0.1068 0.066 Uiso 1 1 calc R . . C23 C 0.10105(16) 0.0693(2) 0.08444(11) 0.0400(7) Uani 1 1 d . . . H23 H 0.1389 0.0765 0.0715 0.048 Uiso 1 1 calc R . . C24 C 0.06406(13) 0.2919(2) 0.01830(10) 0.0332(6) Uani 1 1 d . . . C25 C 0.03332(17) 0.2032(3) -0.01735(11) 0.0432(8) Uani 1 1 d . . . C26 C 0.07858(15) 0.3957(3) -0.00350(10) 0.0366(7) Uani 1 1 d . . . H26 H 0.0589 0.4125 -0.0342 0.044 Uiso 1 1 calc R . . C27 C 0.11982(13) 0.4724(2) 0.01807(10) 0.0321(6) Uani 1 1 d . . . C28 C 0.13597(14) 0.5773(3) -0.00802(10) 0.0340(6) Uani 1 1 d . . . C29 C 0.14359(15) 0.6812(3) 0.01536(11) 0.0387(7) Uani 1 1 d . . . C30 C 0.15758(17) 0.7801(3) -0.00822(13) 0.0494(8) Uani 1 1 d . . . C31 C 0.16661(18) 0.7792(3) -0.05700(14) 0.0550(9) Uani 1 1 d . . . C32 C 0.15957(17) 0.6754(3) -0.08073(12) 0.0525(9) Uani 1 1 d . . . C33 C 0.14424(15) 0.5781(3) -0.05745(11) 0.0417(7) Uani 1 1 d . . . C34 C 0.2035(2) 0.9715(3) -0.06186(17) 0.0693(8) Uani 1 1 d . . . H34A H 0.1692 1.0155 -0.0526 0.083 Uiso 1 1 calc R . . H34B H 0.2252 1.0144 -0.0844 0.083 Uiso 1 1 calc R . . H34C H 0.2317 0.9542 -0.0336 0.083 Uiso 1 1 calc R . . C35 C 0.35502(12) 0.7508(2) 0.54572(10) 0.0279(6) Uani 1 1 d . . . C36 C 0.36710(13) 0.7559(3) 0.49639(10) 0.0353(7) Uani 1 1 d . . . C37 C 0.33829(15) 0.8446(3) 0.46930(11) 0.0418(7) Uani 1 1 d . . . H37 H 0.3453 0.8508 0.4369 0.050 Uiso 1 1 calc R . . C38 C 0.29965(15) 0.9243(3) 0.48790(11) 0.0429(8) Uani 1 1 d . . . H38 H 0.2821 0.9824 0.4682 0.051 Uiso 1 1 calc R . . C39 C 0.28747(14) 0.9172(3) 0.53531(10) 0.0345(6) Uani 1 1 d . . . H39 H 0.2612 0.9697 0.5479 0.041 Uiso 1 1 calc R . . C40 C 0.31513(12) 0.8297(2) 0.56484(10) 0.0285(6) Uani 1 1 d . . . C41 C 0.40907(15) 0.6689(3) 0.47463(11) 0.0449(8) Uani 1 1 d . . . C42 C 0.4748(2) 0.6700(5) 0.5021(2) 0.0962(12) Uani 1 1 d . . . H42A H 0.4910 0.7461 0.5029 0.115 Uiso 1 1 calc R . . H42B H 0.5016 0.6210 0.4859 0.115 Uiso 1 1 calc R . . H42C H 0.4729 0.6434 0.5347 0.115 Uiso 1 1 calc R . . C43 C 0.3815(2) 0.5494(3) 0.47686(15) 0.0675(11) Uani 1 1 d . . . H43A H 0.3773 0.5300 0.5100 0.081 Uiso 1 1 calc R . . H43B H 0.4086 0.4957 0.4636 0.081 Uiso 1 1 calc R . . H43C H 0.3412 0.5474 0.4584 0.081 Uiso 1 1 calc R . . C44 C 0.4156(2) 0.6960(4) 0.42095(13) 0.0746(14) Uani 1 1 d . . . H44A H 0.3750 0.6980 0.4029 0.090 Uiso 1 1 calc R . . H44B H 0.4404 0.6383 0.4078 0.090 Uiso 1 1 calc R . . H44C H 0.4355 0.7687 0.4187 0.090 Uiso 1 1 calc R . . C45 C 0.30305(12) 0.8300(2) 0.61505(10) 0.0274(6) Uani 1 1 d . . . H45 H 0.2791 0.8898 0.6249 0.033 Uiso 1 1 calc R . . C46 C 0.30595(13) 0.7837(2) 0.69536(9) 0.0269(6) Uani 1 1 d . . . C47 C 0.34429(13) 0.8511(3) 0.72706(10) 0.0330(6) Uani 1 1 d . . . C48 C 0.32851(16) 0.8803(3) 0.77230(11) 0.0419(7) Uani 1 1 d . . . C49 C 0.27279(17) 0.8441(3) 0.78657(11) 0.0457(8) Uani 1 1 d . . . C50 C 0.23348(15) 0.7781(3) 0.75564(12) 0.0408(7) Uani 1 1 d . . . C51 C 0.25016(14) 0.7488(2) 0.71080(11) 0.0336(6) Uani 1 1 d . . . C52 C 0.49293(13) 0.7209(3) 0.64733(11) 0.0353(7) Uani 1 1 d . . . C53 C 0.54558(15) 0.6627(3) 0.63654(13) 0.0494(9) Uani 1 1 d . . . H53 H 0.5528 0.5885 0.6474 0.059 Uiso 1 1 calc R . . C54 C 0.58735(16) 0.7163(4) 0.60937(14) 0.0595(11) Uani 1 1 d . . . H54 H 0.6229 0.6777 0.6022 0.071 Uiso 1 1 calc R . . C55 C 0.57725(17) 0.8250(4) 0.59294(13) 0.0605(11) Uani 1 1 d . . . H55 H 0.6061 0.8605 0.5753 0.073 Uiso 1 1 calc R . . C56 C 0.52390(17) 0.8821(3) 0.60263(13) 0.0536(9) Uani 1 1 d . . . H56 H 0.5165 0.9556 0.5910 0.064 Uiso 1 1 calc R . . C57 C 0.48132(14) 0.8302(3) 0.62970(12) 0.0418(7) Uani 1 1 d . . . H57 H 0.4452 0.8683 0.6360 0.050 Uiso 1 1 calc R . . C58 C 0.46117(14) 0.6535(3) 0.72267(11) 0.0369(7) Uani 1 1 d . . . C59 C 0.52055(16) 0.7072(3) 0.74977(13) 0.0476(8) Uani 1 1 d . . . C60 C 0.42547(15) 0.5895(3) 0.75281(11) 0.0388(7) Uani 1 1 d . . . H60 H 0.4400 0.5839 0.7856 0.047 Uiso 1 1 calc R . . C61 C 0.37104(13) 0.5355(2) 0.73705(10) 0.0320(6) Uani 1 1 d . . . C62 C 0.33897(13) 0.4612(3) 0.77015(10) 0.0329(6) Uani 1 1 d . . . C63 C 0.32144(16) 0.4958(3) 0.81432(11) 0.0416(7) Uani 1 1 d . . . C64 C 0.28959(16) 0.4246(3) 0.84286(11) 0.0487(9) Uani 1 1 d . . . C65 C 0.27526(16) 0.3138(3) 0.82928(12) 0.0492(9) Uani 1 1 d . . . C66 C 0.29321(15) 0.2775(3) 0.78513(12) 0.0429(8) Uani 1 1 d . . . C67 C 0.32369(13) 0.3498(3) 0.75671(10) 0.0343(6) Uani 1 1 d . . . C68 C 0.1878(2) 0.2385(5) 0.8578(2) 0.0962(12) Uani 1 1 d . . . H68A H 0.1702 0.3079 0.8441 0.115 Uiso 1 1 calc R . . H68B H 0.1770 0.2300 0.8903 0.115 Uiso 1 1 calc R . . H68C H 0.1716 0.1752 0.8384 0.115 Uiso 1 1 calc R . . Cl1 Cl 0.02175(3) 0.48838(6) 0.10664(3) 0.03931(18) Uani 1 1 d . . . Cl2 Cl 0.17026(4) 0.52498(6) 0.16729(3) 0.03754(17) Uani 1 1 d . . . Cl3 Cl 0.42794(4) 0.43891(7) 0.61879(3) 0.0475(2) Uani 1 1 d . . . Cl4 Cl 0.27397(3) 0.52529(7) 0.59513(3) 0.03979(18) Uani 1 1 d . . . F1 F 0.20263(9) 0.21409(17) 0.02870(6) 0.0495(5) Uani 1 1 d . . . F2 F 0.30527(11) 0.2427(2) -0.01660(8) 0.0749(7) Uani 1 1 d . . . F3 F 0.40818(10) 0.3446(2) 0.02998(9) 0.0780(7) Uani 1 1 d . . . F4 F 0.40677(9) 0.41792(19) 0.12271(8) 0.0608(6) Uani 1 1 d . . . F5 F 0.30407(8) 0.39078(15) 0.16855(6) 0.0398(4) Uani 1 1 d . . . F6 F 0.07034(12) 0.1163(2) -0.02179(9) 0.0785(8) Uani 1 1 d . . . F7 F -0.01847(11) 0.1606(2) -0.00414(9) 0.0818(8) Uani 1 1 d . . . F8 F 0.01895(16) 0.2455(2) -0.06082(8) 0.0995(11) Uani 1 1 d . . . F9 F 0.13573(10) 0.69075(15) 0.06253(6) 0.0515(5) Uani 1 1 d . . . F10 F 0.16063(13) 0.87790(17) 0.01700(9) 0.0723(7) Uani 1 1 d . . . F11 F 0.16879(12) 0.6690(2) -0.12809(7) 0.0764(7) Uani 1 1 d . . . F12 F 0.14030(10) 0.48085(18) -0.08306(7) 0.0576(5) Uani 1 1 d . . . F13 F 0.39823(8) 0.89072(17) 0.71359(7) 0.0487(5) Uani 1 1 d . . . F14 F 0.36708(10) 0.9441(2) 0.80206(7) 0.0651(6) Uani 1 1 d . . . F15 F 0.25701(12) 0.8730(2) 0.83036(7) 0.0728(7) Uani 1 1 d . . . F16 F 0.17829(10) 0.7459(2) 0.76907(8) 0.0651(6) Uani 1 1 d . . . F17 F 0.21025(8) 0.68754(16) 0.68076(7) 0.0452(4) Uani 1 1 d . . . F18 F 0.51510(12) 0.7164(2) 0.79691(8) 0.0806(8) Uani 1 1 d . . . F19 F 0.57011(10) 0.6428(2) 0.74556(10) 0.0773(7) Uani 1 1 d . . . F20 F 0.53241(9) 0.81034(16) 0.73452(7) 0.0533(5) Uani 1 1 d . . . F21 F 0.33438(11) 0.60244(18) 0.83035(7) 0.0621(6) Uani 1 1 d . . . F22 F 0.27408(12) 0.4639(2) 0.88546(7) 0.0736(7) Uani 1 1 d . . . F23 F 0.28125(11) 0.17032(17) 0.77062(8) 0.0615(6) Uani 1 1 d . . . F24 F 0.33985(8) 0.30994(14) 0.71438(6) 0.0397(4) Uani 1 1 d . . . N1 N 0.19685(10) 0.28103(19) 0.12626(8) 0.0261(5) Uani 1 1 d . . . N2 N 0.07604(10) 0.26912(19) 0.06447(8) 0.0283(5) Uani 1 1 d . . . N3 N 0.32209(10) 0.75578(19) 0.64774(8) 0.0265(5) Uani 1 1 d . . . N4 N 0.44840(11) 0.6660(2) 0.67547(9) 0.0326(5) Uani 1 1 d . . . O1 O 0.09350(8) 0.30850(15) 0.16905(6) 0.0267(4) Uani 1 1 d . . . O2 O 0.14798(9) 0.45965(16) 0.06219(6) 0.0303(4) Uani 1 1 d . . . O3 O 0.18099(17) 0.8699(3) -0.08391(11) 0.0833(10) Uani 1 1 d . . . O4 O 0.38068(9) 0.67032(16) 0.57559(7) 0.0297(4) Uani 1 1 d . . . O5 O 0.34386(9) 0.54225(16) 0.69300(7) 0.0319(4) Uani 1 1 d . . . O6 O 0.24778(13) 0.2417(3) 0.85840(10) 0.0778(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0270(2) 0.0234(2) 0.0236(2) 0.00054(19) 0.00276(18) -0.00019(19) Ti2 0.0294(3) 0.0257(3) 0.0278(3) -0.0008(2) 0.00103(19) 0.0017(2) C1 0.0298(14) 0.0212(13) 0.0244(13) -0.0012(10) -0.0001(10) -0.0036(11) C2 0.0366(15) 0.0266(14) 0.0278(14) -0.0021(11) 0.0057(12) -0.0054(12) C3 0.0460(18) 0.0331(15) 0.0304(15) 0.0036(12) 0.0078(13) -0.0091(14) C4 0.0452(18) 0.0270(15) 0.0418(17) 0.0102(13) -0.0009(14) -0.0052(13) C5 0.0311(15) 0.0269(14) 0.0416(16) 0.0021(12) -0.0007(12) -0.0006(12) C6 0.0277(14) 0.0252(13) 0.0261(13) -0.0009(11) -0.0002(10) -0.0033(11) C7 0.0431(17) 0.0351(16) 0.0356(16) -0.0011(13) 0.0167(13) -0.0012(13) C8 0.061(2) 0.0433(19) 0.051(2) -0.0009(16) 0.0296(17) -0.0038(16) C9 0.0344(17) 0.058(2) 0.053(2) -0.0029(17) 0.0162(15) 0.0048(15) C10 0.084(2) 0.0469(16) 0.082(2) 0.0125(15) 0.0315(17) -0.0028(15) C11 0.0264(13) 0.0256(13) 0.0282(14) -0.0040(11) 0.0004(11) 0.0012(11) C12 0.0275(14) 0.0296(14) 0.0335(15) 0.0028(12) 0.0086(11) 0.0023(11) C13 0.0369(17) 0.0407(17) 0.0388(17) -0.0023(14) 0.0089(13) 0.0021(14) C14 0.053(2) 0.061(2) 0.0378(18) -0.0017(16) 0.0224(15) 0.0060(18) C15 0.0351(17) 0.058(2) 0.060(2) 0.0091(18) 0.0239(16) 0.0037(16) C16 0.0276(15) 0.0441(18) 0.054(2) 0.0096(15) 0.0069(14) -0.0023(14) C17 0.0311(15) 0.0326(15) 0.0353(16) 0.0043(13) 0.0048(12) 0.0027(12) C18 0.0394(16) 0.0273(14) 0.0268(14) -0.0035(11) -0.0021(12) -0.0078(12) C19 0.049(2) 0.0459(19) 0.0482(19) -0.0106(16) 0.0100(15) -0.0145(16) C20 0.086(3) 0.058(3) 0.057(2) -0.012(2) 0.028(2) -0.039(2) C21 0.126(4) 0.041(2) 0.0316(18) -0.0033(16) 0.012(2) -0.037(2) C22 0.097(3) 0.0279(17) 0.0360(18) -0.0027(14) -0.0163(19) -0.0055(18) C23 0.0501(19) 0.0291(15) 0.0379(17) -0.0038(13) -0.0077(14) -0.0038(14) C24 0.0344(15) 0.0333(15) 0.0303(15) -0.0020(12) -0.0031(12) 0.0008(12) C25 0.057(2) 0.0363(17) 0.0332(16) -0.0001(14) -0.0085(14) -0.0080(16) C26 0.0461(18) 0.0345(16) 0.0271(14) 0.0040(12) -0.0061(12) -0.0008(14) C27 0.0357(15) 0.0343(15) 0.0265(14) 0.0039(12) 0.0046(12) 0.0041(13) C28 0.0362(16) 0.0379(16) 0.0279(14) 0.0071(12) 0.0031(12) -0.0011(13) C29 0.0445(18) 0.0402(17) 0.0317(15) 0.0075(13) 0.0054(13) -0.0016(14) C30 0.053(2) 0.0386(18) 0.057(2) 0.0095(16) 0.0050(16) -0.0073(16) C31 0.059(2) 0.053(2) 0.054(2) 0.0263(19) 0.0138(17) -0.0037(18) C32 0.053(2) 0.071(3) 0.0353(18) 0.0186(17) 0.0132(15) 0.0015(19) C33 0.0460(18) 0.0476(19) 0.0318(16) 0.0047(14) 0.0064(13) 0.0019(15) C34 0.084(2) 0.0469(16) 0.082(2) 0.0125(15) 0.0315(17) -0.0028(15) C35 0.0268(14) 0.0287(14) 0.0275(14) -0.0009(11) -0.0003(11) 0.0000(11) C36 0.0321(15) 0.0450(17) 0.0290(15) -0.0033(13) 0.0045(12) 0.0021(13) C37 0.0449(18) 0.056(2) 0.0262(15) 0.0031(14) 0.0088(13) 0.0082(16) C38 0.0463(18) 0.0479(19) 0.0340(16) 0.0095(14) 0.0021(13) 0.0105(15) C39 0.0339(15) 0.0357(16) 0.0339(15) -0.0004(13) 0.0034(12) 0.0076(13) C40 0.0252(13) 0.0302(14) 0.0299(14) -0.0003(12) 0.0024(11) 0.0007(11) C41 0.0450(18) 0.058(2) 0.0330(16) -0.0067(15) 0.0083(14) 0.0136(16) C42 0.056(2) 0.117(3) 0.116(3) 0.042(3) 0.0109(19) 0.003(2) C43 0.080(3) 0.059(2) 0.064(3) -0.031(2) 0.011(2) 0.007(2) C44 0.083(3) 0.107(4) 0.0361(19) -0.002(2) 0.0195(19) 0.045(3) C45 0.0235(13) 0.0267(14) 0.0325(14) -0.0018(11) 0.0049(11) 0.0000(11) C46 0.0303(14) 0.0240(13) 0.0270(13) 0.0023(11) 0.0060(11) 0.0044(11) C47 0.0288(15) 0.0359(16) 0.0351(15) -0.0003(13) 0.0064(12) -0.0013(12) C48 0.0505(19) 0.0433(18) 0.0316(16) -0.0074(14) 0.0036(14) -0.0034(15) C49 0.062(2) 0.0453(19) 0.0330(16) -0.0050(14) 0.0201(15) 0.0006(17) C50 0.0456(18) 0.0372(17) 0.0433(18) 0.0052(14) 0.0219(14) -0.0012(14) C51 0.0343(15) 0.0275(14) 0.0388(16) 0.0026(12) 0.0038(12) -0.0015(12) C52 0.0240(14) 0.0433(17) 0.0382(16) -0.0082(14) 0.0015(12) -0.0033(13) C53 0.0318(17) 0.058(2) 0.058(2) -0.0148(18) -0.0002(15) 0.0058(16) C54 0.0298(17) 0.092(3) 0.058(2) -0.029(2) 0.0098(16) -0.0024(19) C55 0.043(2) 0.093(3) 0.048(2) -0.017(2) 0.0152(16) -0.023(2) C56 0.048(2) 0.065(2) 0.048(2) 0.0023(18) 0.0073(16) -0.0162(18) C57 0.0326(16) 0.0462(19) 0.0474(18) -0.0031(15) 0.0086(13) -0.0042(14) C58 0.0341(16) 0.0330(15) 0.0417(17) -0.0043(13) -0.0053(13) 0.0001(13) C59 0.0433(19) 0.047(2) 0.049(2) -0.0041(16) -0.0112(15) -0.0072(16) C60 0.0424(17) 0.0408(17) 0.0306(15) -0.0008(13) -0.0073(13) -0.0038(14) C61 0.0369(16) 0.0282(14) 0.0300(15) -0.0013(12) -0.0005(12) 0.0058(12) C62 0.0344(15) 0.0372(16) 0.0258(14) 0.0031(12) -0.0029(11) 0.0044(13) C63 0.0507(19) 0.0419(18) 0.0306(16) -0.0036(14) -0.0039(14) 0.0057(15) C64 0.050(2) 0.073(3) 0.0243(15) 0.0035(16) 0.0063(14) 0.0121(18) C65 0.0443(19) 0.061(2) 0.0413(19) 0.0208(17) 0.0014(15) 0.0022(17) C66 0.0414(18) 0.0443(19) 0.0419(18) 0.0081(15) -0.0006(14) -0.0007(15) C67 0.0317(15) 0.0409(17) 0.0290(15) 0.0016(13) -0.0028(12) 0.0042(13) C68 0.056(2) 0.117(3) 0.116(3) 0.042(3) 0.0109(19) 0.003(2) Cl1 0.0359(4) 0.0395(4) 0.0423(4) 0.0050(3) 0.0030(3) 0.0110(3) Cl2 0.0442(4) 0.0331(4) 0.0349(4) -0.0067(3) 0.0023(3) -0.0089(3) Cl3 0.0518(5) 0.0360(4) 0.0544(5) -0.0031(4) 0.0042(4) 0.0153(4) Cl4 0.0390(4) 0.0426(4) 0.0361(4) 0.0008(3) -0.0036(3) -0.0108(3) F1 0.0467(11) 0.0658(13) 0.0366(10) -0.0158(9) 0.0071(8) -0.0051(10) F2 0.0760(15) 0.1064(19) 0.0483(12) -0.0162(13) 0.0343(11) 0.0009(14) F3 0.0470(12) 0.110(2) 0.0841(16) 0.0059(15) 0.0407(12) -0.0014(13) F4 0.0322(10) 0.0698(14) 0.0805(15) 0.0088(12) 0.0062(10) -0.0154(10) F5 0.0376(9) 0.0441(10) 0.0365(9) -0.0007(8) -0.0017(7) -0.0059(8) F6 0.0946(18) 0.0639(15) 0.0708(15) -0.0383(12) -0.0196(13) 0.0188(13) F7 0.0651(15) 0.107(2) 0.0709(15) -0.0299(14) -0.0053(12) -0.0394(15) F8 0.188(3) 0.0557(14) 0.0416(12) 0.0078(11) -0.0506(16) -0.0393(17) F9 0.0844(14) 0.0363(10) 0.0350(10) 0.0013(8) 0.0119(9) -0.0086(10) F10 0.1071(19) 0.0382(11) 0.0730(15) 0.0037(11) 0.0158(14) -0.0192(12) F11 0.1021(18) 0.0933(18) 0.0382(11) 0.0219(12) 0.0286(12) 0.0013(15) F12 0.0761(14) 0.0645(13) 0.0346(10) -0.0033(9) 0.0162(10) -0.0023(11) F13 0.0376(10) 0.0590(12) 0.0515(11) -0.0185(9) 0.0148(8) -0.0173(9) F14 0.0719(14) 0.0784(15) 0.0450(12) -0.0280(11) 0.0066(10) -0.0184(12) F15 0.0984(18) 0.0832(16) 0.0433(12) -0.0163(11) 0.0380(12) -0.0135(14) F16 0.0602(13) 0.0720(14) 0.0710(14) -0.0071(11) 0.0430(11) -0.0199(11) F17 0.0368(9) 0.0472(11) 0.0527(11) -0.0080(9) 0.0092(8) -0.0112(8) F18 0.0897(17) 0.1054(19) 0.0427(12) -0.0090(12) -0.0113(11) -0.0501(15) F19 0.0433(12) 0.0641(14) 0.115(2) -0.0160(14) -0.0337(12) 0.0075(11) F20 0.0501(11) 0.0459(11) 0.0606(12) -0.0027(9) -0.0091(9) -0.0147(9) F21 0.0869(16) 0.0567(13) 0.0428(11) -0.0181(10) 0.0075(10) 0.0026(11) F22 0.0859(16) 0.1048(19) 0.0324(11) -0.0052(11) 0.0175(10) 0.0069(15) F23 0.0735(14) 0.0437(12) 0.0683(14) 0.0089(10) 0.0119(11) -0.0132(10) F24 0.0477(10) 0.0362(9) 0.0349(9) -0.0042(7) 0.0027(8) -0.0002(8) N1 0.0261(11) 0.0281(12) 0.0242(11) -0.0028(9) 0.0036(9) -0.0024(9) N2 0.0305(12) 0.0262(12) 0.0275(12) 0.0009(10) 0.0000(9) -0.0019(10) N3 0.0251(11) 0.0267(12) 0.0278(12) -0.0018(9) 0.0037(9) -0.0015(9) N4 0.0302(12) 0.0298(13) 0.0370(13) -0.0023(10) 0.0000(10) 0.0004(10) O1 0.0286(10) 0.0249(9) 0.0269(9) 0.0023(8) 0.0047(7) 0.0001(8) O2 0.0344(10) 0.0316(10) 0.0247(10) 0.0034(8) 0.0022(8) -0.0024(8) O3 0.116(3) 0.0686(19) 0.0692(19) 0.0332(16) 0.0267(18) -0.0182(18) O4 0.0304(10) 0.0298(10) 0.0296(10) -0.0014(8) 0.0058(8) 0.0038(8) O5 0.0339(11) 0.0335(11) 0.0271(10) 0.0017(8) -0.0026(8) -0.0001(9) O6 0.0596(17) 0.112(2) 0.0647(17) 0.0471(18) 0.0187(14) 0.0043(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O1 1.8209(18) . ? Ti1 O2 1.9500(19) . ? Ti1 N2 2.213(2) . ? Ti1 N1 2.226(2) . ? Ti1 Cl1 2.2639(8) . ? Ti1 Cl2 2.2834(8) . ? Ti2 O4 1.8282(19) . ? Ti2 O5 1.9459(19) . ? Ti2 N4 2.209(2) . ? Ti2 N3 2.245(2) . ? Ti2 Cl3 2.2544(9) . ? Ti2 Cl4 2.2846(9) . ? C1 O1 1.338(3) . ? C1 C6 1.407(4) . ? C1 C2 1.412(4) . ? C2 C3 1.401(4) . ? C2 C7 1.536(4) . ? C3 C4 1.391(4) . ? C3 H3 0.9300 . ? C4 C5 1.367(4) . ? C4 H4 0.9300 . ? C5 C6 1.400(4) . ? C5 H5 0.9300 . ? C6 C11 1.441(4) . ? C7 C9 1.535(5) . ? C7 C8 1.540(4) . ? C7 C10 1.545(5) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 N1 1.304(3) . ? C11 H11 0.9300 . ? C12 C13 1.384(4) . ? C12 C17 1.392(4) . ? C12 N1 1.439(3) . ? C13 F1 1.342(4) . ? C13 C14 1.380(4) . ? C14 F2 1.339(4) . ? C14 C15 1.369(5) . ? C15 F3 1.341(4) . ? C15 C16 1.377(5) . ? C16 F4 1.341(4) . ? C16 C17 1.379(4) . ? C17 F5 1.331(3) . ? C18 C23 1.371(4) . ? C18 C19 1.387(4) . ? C18 N2 1.449(3) . ? C19 C20 1.379(5) . ? C19 H19 0.9300 . ? C20 C21 1.374(6) . ? C20 H20 0.9300 . ? C21 C22 1.367(6) . ? C21 H21 0.9300 . ? C22 C23 1.393(5) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 N2 1.305(3) . ? C24 C26 1.412(4) . ? C24 C25 1.536(4) . ? C25 F8 1.309(4) . ? C25 F7 1.311(4) . ? C25 F6 1.310(4) . ? C26 C27 1.358(4) . ? C26 H26 0.9300 . ? C27 O2 1.313(3) . ? C27 C28 1.489(4) . ? C28 C29 1.384(4) . ? C28 C33 1.399(4) . ? C29 F9 1.340(3) . ? C29 C30 1.381(4) . ? C30 F10 1.343(4) . ? C30 C31 1.385(5) . ? C31 O3 1.356(4) . ? C31 C32 1.386(5) . ? C32 F11 1.349(4) . ? C32 C33 1.370(5) . ? C33 F12 1.343(4) . ? C34 O3 1.404(5) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 O4 1.337(3) . ? C35 C40 1.406(4) . ? C35 C36 1.419(4) . ? C36 C37 1.391(4) . ? C36 C41 1.531(4) . ? C37 C38 1.389(4) . ? C37 H37 0.9300 . ? C38 C39 1.369(4) . ? C38 H38 0.9300 . ? C39 C40 1.406(4) . ? C39 H39 0.9300 . ? C40 C45 1.442(4) . ? C41 C42 1.534(6) . ? C41 C43 1.529(5) . ? C41 C44 1.542(5) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 N3 1.292(3) . ? C45 H45 0.9300 . ? C46 C51 1.381(4) . ? C46 C47 1.387(4) . ? C46 N3 1.438(3) . ? C47 F13 1.342(3) . ? C47 C48 1.377(4) . ? C48 F14 1.336(4) . ? C48 C49 1.372(5) . ? C49 F15 1.338(3) . ? C49 C50 1.377(5) . ? C50 F16 1.338(3) . ? C50 C51 1.373(4) . ? C51 F17 1.340(3) . ? C52 C57 1.387(5) . ? C52 C53 1.385(4) . ? C52 N4 1.451(4) . ? C53 C54 1.385(5) . ? C53 H53 0.9300 . ? C54 C55 1.366(6) . ? C54 H54 0.9300 . ? C55 C56 1.382(5) . ? C55 H55 0.9300 . ? C56 C57 1.387(5) . ? C56 H56 0.9300 . ? C57 H57 0.9300 . ? C58 N4 1.315(4) . ? C58 C60 1.411(4) . ? C58 C59 1.547(4) . ? C59 F20 1.317(4) . ? C59 F18 1.328(4) . ? C59 F19 1.324(4) . ? C60 C61 1.364(4) . ? C60 H60 0.9300 . ? C61 O5 1.298(3) . ? C61 C62 1.489(4) . ? C62 C63 1.380(4) . ? C62 C67 1.391(4) . ? C63 F21 1.348(4) . ? C63 C64 1.383(5) . ? C64 F22 1.342(4) . ? C64 C65 1.381(5) . ? C65 O6 1.350(4) . ? C65 C66 1.389(5) . ? C66 F23 1.339(4) . ? C66 C67 1.373(4) . ? C67 F24 1.342(3) . ? C68 O6 1.291(5) . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ti1 O2 167.01(8) . . ? O1 Ti1 N2 92.11(8) . . ? O2 Ti1 N2 81.63(8) . . ? O1 Ti1 N1 81.25(8) . . ? O2 Ti1 N1 86.74(8) . . ? N2 Ti1 N1 83.70(8) . . ? O1 Ti1 Cl1 95.79(6) . . ? O2 Ti1 Cl1 95.34(6) . . ? N2 Ti1 Cl1 87.96(6) . . ? N1 Ti1 Cl1 171.03(6) . . ? O1 Ti1 Cl2 94.83(6) . . ? O2 Ti1 Cl2 89.84(6) . . ? N2 Ti1 Cl2 169.01(7) . . ? N1 Ti1 Cl2 88.94(6) . . ? Cl1 Ti1 Cl2 99.78(3) . . ? O4 Ti2 O5 165.62(9) . . ? O4 Ti2 N4 94.93(9) . . ? O5 Ti2 N4 83.29(9) . . ? O4 Ti2 N3 81.28(8) . . ? O5 Ti2 N3 84.34(8) . . ? N4 Ti2 N3 82.75(8) . . ? O4 Ti2 Cl3 98.22(6) . . ? O5 Ti2 Cl3 95.98(6) . . ? N4 Ti2 Cl3 88.10(7) . . ? N3 Ti2 Cl3 170.75(6) . . ? O4 Ti2 Cl4 91.32(6) . . ? O5 Ti2 Cl4 88.53(6) . . ? N4 Ti2 Cl4 169.38(7) . . ? N3 Ti2 Cl4 89.74(6) . . ? Cl3 Ti2 Cl4 99.51(4) . . ? O1 C1 C6 117.1(2) . . ? O1 C1 C2 121.0(2) . . ? C6 C1 C2 121.9(2) . . ? C3 C2 C1 115.2(3) . . ? C3 C2 C7 122.2(3) . . ? C1 C2 C7 122.5(2) . . ? C4 C3 C2 123.5(3) . . ? C4 C3 H3 118.3 . . ? C2 C3 H3 118.3 . . ? C5 C4 C3 120.0(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 119.6(3) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C5 C6 C1 119.7(2) . . ? C5 C6 C11 118.1(2) . . ? C1 C6 C11 122.2(2) . . ? C9 C7 C2 111.9(2) . . ? C9 C7 C8 107.3(3) . . ? C2 C7 C8 111.4(3) . . ? C9 C7 C10 109.2(3) . . ? C2 C7 C10 108.2(3) . . ? C8 C7 C10 108.8(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C6 127.6(2) . . ? N1 C11 H11 116.2 . . ? C6 C11 H11 116.2 . . ? C13 C12 C17 117.2(3) . . ? C13 C12 N1 122.4(3) . . ? C17 C12 N1 120.4(2) . . ? F1 C13 C14 118.1(3) . . ? F1 C13 C12 120.1(3) . . ? C14 C13 C12 121.8(3) . . ? F2 C14 C15 120.3(3) . . ? F2 C14 C13 119.9(3) . . ? C15 C14 C13 119.8(3) . . ? F3 C15 C16 119.8(3) . . ? F3 C15 C14 120.3(3) . . ? C16 C15 C14 119.9(3) . . ? F4 C16 C15 119.9(3) . . ? F4 C16 C17 120.1(3) . . ? C15 C16 C17 120.0(3) . . ? F5 C17 C16 118.5(3) . . ? F5 C17 C12 120.2(3) . . ? C16 C17 C12 121.3(3) . . ? C23 C18 C19 120.9(3) . . ? C23 C18 N2 121.4(3) . . ? C19 C18 N2 117.6(3) . . ? C20 C19 C18 119.2(4) . . ? C20 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? C21 C20 C19 120.3(4) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C22 C21 C20 120.2(3) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 120.4(4) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C18 C23 C22 118.9(3) . . ? C18 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? N2 C24 C26 124.5(3) . . ? N2 C24 C25 121.1(3) . . ? C26 C24 C25 114.3(2) . . ? F8 C25 F7 106.1(3) . . ? F8 C25 F6 107.2(3) . . ? F7 C25 F6 105.9(3) . . ? F8 C25 C24 112.1(3) . . ? F7 C25 C24 113.6(3) . . ? F6 C25 C24 111.4(3) . . ? C27 C26 C24 123.4(3) . . ? C27 C26 H26 118.3 . . ? C24 C26 H26 118.3 . . ? O2 C27 C26 123.3(3) . . ? O2 C27 C28 115.9(2) . . ? C26 C27 C28 120.8(3) . . ? C29 C28 C33 115.5(3) . . ? C29 C28 C27 121.7(3) . . ? C33 C28 C27 122.8(3) . . ? F9 C29 C30 116.6(3) . . ? F9 C29 C28 120.6(3) . . ? C30 C29 C28 122.8(3) . . ? F10 C30 C29 118.3(3) . . ? F10 C30 C31 120.6(3) . . ? C29 C30 C31 121.0(3) . . ? O3 C31 C32 116.8(3) . . ? O3 C31 C30 126.4(4) . . ? C32 C31 C30 116.7(3) . . ? F11 C32 C33 118.6(4) . . ? F11 C32 C31 119.4(3) . . ? C33 C32 C31 122.0(3) . . ? F12 C33 C32 117.8(3) . . ? F12 C33 C28 120.2(3) . . ? C32 C33 C28 121.9(3) . . ? O3 C34 H34A 109.5 . . ? O3 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O3 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O4 C35 C40 117.6(2) . . ? O4 C35 C36 121.3(2) . . ? C40 C35 C36 121.2(2) . . ? C37 C36 C35 115.7(3) . . ? C37 C36 C41 122.4(3) . . ? C35 C36 C41 121.9(3) . . ? C38 C37 C36 123.8(3) . . ? C38 C37 H37 118.1 . . ? C36 C37 H37 118.1 . . ? C39 C38 C37 120.0(3) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C40 119.3(3) . . ? C38 C39 H39 120.4 . . ? C40 C39 H39 120.4 . . ? C35 C40 C39 120.1(3) . . ? C35 C40 C45 123.1(2) . . ? C39 C40 C45 116.7(2) . . ? C36 C41 C42 110.6(3) . . ? C36 C41 C43 110.4(3) . . ? C42 C41 C43 109.2(3) . . ? C36 C41 C44 111.2(3) . . ? C42 C41 C44 107.5(3) . . ? C43 C41 C44 107.8(3) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N3 C45 C40 126.7(3) . . ? N3 C45 H45 116.7 . . ? C40 C45 H45 116.7 . . ? C51 C46 C47 116.9(2) . . ? C51 C46 N3 121.4(2) . . ? C47 C46 N3 121.6(2) . . ? F13 C47 C48 118.2(3) . . ? F13 C47 C46 119.8(2) . . ? C48 C47 C46 122.0(3) . . ? F14 C48 C49 120.2(3) . . ? F14 C48 C47 120.2(3) . . ? C49 C48 C47 119.6(3) . . ? F15 C49 C48 119.8(3) . . ? F15 C49 C50 120.5(3) . . ? C48 C49 C50 119.7(3) . . ? F16 C50 C49 119.5(3) . . ? F16 C50 C51 120.5(3) . . ? C49 C50 C51 120.0(3) . . ? F17 C51 C46 119.3(3) . . ? F17 C51 C50 118.9(3) . . ? C46 C51 C50 121.8(3) . . ? C57 C52 C53 120.2(3) . . ? C57 C52 N4 119.8(3) . . ? C53 C52 N4 120.0(3) . . ? C54 C53 C52 119.2(4) . . ? C54 C53 H53 120.4 . . ? C52 C53 H53 120.4 . . ? C55 C54 C53 121.1(3) . . ? C55 C54 H54 119.4 . . ? C53 C54 H54 119.4 . . ? C54 C55 C56 119.7(4) . . ? C54 C55 H55 120.2 . . ? C56 C55 H55 120.2 . . ? C55 C56 C57 120.3(4) . . ? C55 C56 H56 119.9 . . ? C57 C56 H56 119.9 . . ? C52 C57 C56 119.5(3) . . ? C52 C57 H57 120.2 . . ? C56 C57 H57 120.2 . . ? N4 C58 C60 125.3(3) . . ? N4 C58 C59 120.7(3) . . ? C60 C58 C59 113.9(3) . . ? F20 C59 F18 106.4(3) . . ? F20 C59 F19 108.1(3) . . ? F18 C59 F19 106.9(3) . . ? F20 C59 C58 113.5(3) . . ? F18 C59 C58 110.7(3) . . ? F19 C59 C58 110.9(3) . . ? C61 C60 C58 124.3(3) . . ? C61 C60 H60 117.8 . . ? C58 C60 H60 117.8 . . ? O5 C61 C60 123.9(3) . . ? O5 C61 C62 115.0(2) . . ? C60 C61 C62 121.1(3) . . ? C63 C62 C67 115.8(3) . . ? C63 C62 C61 124.2(3) . . ? C67 C62 C61 120.0(3) . . ? F21 C63 C64 118.2(3) . . ? F21 C63 C62 120.0(3) . . ? C64 C63 C62 121.8(3) . . ? F22 C64 C63 118.6(3) . . ? F22 C64 C65 119.6(3) . . ? C63 C64 C65 121.7(3) . . ? O6 C65 C64 121.9(3) . . ? O6 C65 C66 121.0(4) . . ? C64 C65 C66 117.0(3) . . ? F23 C66 C67 119.9(3) . . ? F23 C66 C65 119.4(3) . . ? C67 C66 C65 120.7(3) . . ? F24 C67 C66 118.0(3) . . ? F24 C67 C62 119.1(3) . . ? C66 C67 C62 122.9(3) . . ? O6 C68 H68A 109.5 . . ? O6 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? O6 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C11 N1 C12 112.9(2) . . ? C11 N1 Ti1 124.53(18) . . ? C12 N1 Ti1 122.42(17) . . ? C24 N2 C18 120.3(2) . . ? C24 N2 Ti1 123.33(19) . . ? C18 N2 Ti1 116.24(16) . . ? C45 N3 C46 113.5(2) . . ? C45 N3 Ti2 123.10(18) . . ? C46 N3 Ti2 123.17(16) . . ? C58 N4 C52 120.2(2) . . ? C58 N4 Ti2 125.8(2) . . ? C52 N4 Ti2 113.56(17) . . ? C1 O1 Ti1 146.95(17) . . ? C27 O2 Ti1 128.15(18) . . ? C31 O3 C34 121.3(3) . . ? C35 O4 Ti2 141.67(17) . . ? C61 O5 Ti2 135.94(19) . . ? C68 O6 C65 120.9(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.08 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.703 _refine_diff_density_min -1.531 _refine_diff_density_rms 0.063