Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_tropI _database_code_depnum_ccdc_archive 'CCDC 252929' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C18 H10 Cl2 F5 N O Ti' _chemical_formula_sum 'C18 H10 Cl2 F5 N O Ti' _chemical_formula_weight 470.07 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.068(1) _cell_length_b 10.0972(7) _cell_length_c 11.086(2) _cell_angle_alpha 90.605(8) _cell_angle_beta 106.216(9) _cell_angle_gamma 112.989(8) _cell_volume 889.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 73 _cell_measurement_theta_min 6.12 _cell_measurement_theta_max 21.56 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.21 _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 468 _exptl_absorpt_coefficient_mu 0.841 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6548 _exptl_absorpt_correction_T_max 0.8432 _exptl_absorpt_process_details ; SADABS (Bruker, 2000) ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_detector 'CCD plate' _diffrn_detector_type ; Bruker-Nonius 95mm CCD camera on \k-goniostat ; _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 7578 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0820 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3992 _reflns_number_gt 2416 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 3992 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1013 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.0883 _refine_ls_wR_factor_gt 0.0762 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 0.05405(6) 0.24160(5) 0.25069(4) 0.02605(15) Uani 1 1 d . . . Cl1 Cl -0.01418(11) 0.00613(7) 0.29743(8) 0.0470(2) Uani 1 1 d . . . Cl2 Cl -0.23136(10) 0.18572(8) 0.15817(7) 0.0457(2) Uani 1 1 d . . . F1 F 0.0994(2) -0.08316(16) 0.07671(16) 0.0483(5) Uani 1 1 d . . . F2 F 0.2433(3) -0.26596(17) 0.16957(18) 0.0635(6) Uani 1 1 d . . . F3 F 0.5360(3) -0.1641(2) 0.36196(18) 0.0697(6) Uani 1 1 d . . . F4 F 0.6882(2) 0.1224(2) 0.45901(17) 0.0619(5) Uani 1 1 d . . . F5 F 0.5462(2) 0.30382(17) 0.36553(16) 0.0489(4) Uani 1 1 d . . . O1 O 0.0833(2) 0.36186(17) 0.11294(16) 0.0302(4) Uani 1 1 d . . . N1 N 0.2311(3) 0.2058(2) 0.17750(19) 0.0253(5) Uani 1 1 d . . . C1 C 0.2420(4) -0.0327(3) 0.1723(3) 0.0333(7) Uani 1 1 d . . . C2 C 0.3166(4) -0.1251(3) 0.2189(3) 0.0403(8) Uani 1 1 d . . . C3 C 0.4642(4) -0.0736(3) 0.3156(3) 0.0413(8) Uani 1 1 d . . . C4 C 0.5413(4) 0.0703(3) 0.3659(3) 0.0390(7) Uani 1 1 d . . . C5 C 0.4655(4) 0.1620(3) 0.3182(3) 0.0318(7) Uani 1 1 d . . . C6 C 0.3137(4) 0.1128(3) 0.2233(2) 0.0269(6) Uani 1 1 d . . . C7 C 0.2601(3) 0.2667(2) 0.0737(2) 0.0236(6) Uani 1 1 d . . . C8 C 0.3577(4) 0.2389(3) 0.0080(3) 0.0386(7) Uani 1 1 d . . . H8 H 0.4052 0.1755 0.0418 0.039 Uiso 1 1 calc R . . C9 C 0.3950(4) 0.2908(3) -0.0995(3) 0.0461(8) Uani 1 1 d . . . H9 H 0.4623 0.2557 -0.1273 0.046 Uiso 1 1 calc R . . C10 C 0.3487(4) 0.3860(3) -0.1719(3) 0.0482(9) Uani 1 1 d . . . H10 H 0.3858 0.4050 -0.2426 0.048 Uiso 1 1 calc R . . C11 C 0.2534(4) 0.4559(3) -0.1508(3) 0.0452(8) Uani 1 1 d . . . H11 H 0.2383 0.5198 -0.2079 0.045 Uiso 1 1 calc R . . C12 C 0.1764(4) 0.4456(3) -0.0575(3) 0.0350(7) Uani 1 1 d . . . H12 H 0.1188 0.5047 -0.0604 0.035 Uiso 1 1 calc R . . C13 C 0.1727(3) 0.3604(2) 0.0391(2) 0.0262(6) Uani 1 1 d . . . C14 C 0.2753(4) 0.4429(3) 0.3865(3) 0.0496(9) Uani 1 1 d . . . H14 H 0.3709 0.4929 0.3626 0.050 Uiso 1 1 calc R . . C15 C 0.1326(4) 0.4721(3) 0.3608(3) 0.0447(8) Uani 1 1 d . . . H15 H 0.1158 0.5450 0.3160 0.045 Uiso 1 1 calc R . . C16 C 0.0197(4) 0.3740(3) 0.4136(3) 0.0432(8) Uani 1 1 d . . . H16 H -0.0856 0.3700 0.4103 0.043 Uiso 1 1 calc R . . C17 C 0.0908(5) 0.2830(3) 0.4718(3) 0.0494(9) Uani 1 1 d . . . H17 H 0.0421 0.2076 0.5149 0.049 Uiso 1 1 calc R . . C18 C 0.2486(5) 0.3248(3) 0.4544(3) 0.0518(9) Uani 1 1 d . . . H18 H 0.3231 0.2814 0.4831 0.052 Uiso 1 1 calc R . . 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 0.0277(3) 0.0266(3) 0.0263(3) 0.00364(19) 0.0101(2) 0.0125(2) Cl1 0.0568(6) 0.0325(4) 0.0602(6) 0.0160(3) 0.0313(5) 0.0174(4) Cl2 0.0301(5) 0.0595(5) 0.0478(5) 0.0094(4) 0.0131(4) 0.0179(4) F1 0.0428(12) 0.0401(9) 0.0521(12) -0.0114(8) -0.0004(10) 0.0176(9) F2 0.0835(16) 0.0365(10) 0.0870(15) 0.0114(9) 0.0366(13) 0.0343(10) F3 0.0915(17) 0.0918(14) 0.0716(14) 0.0452(12) 0.0359(13) 0.0764(14) F4 0.0390(13) 0.1044(15) 0.0478(12) 0.0253(11) 0.0078(11) 0.0384(12) F5 0.0354(11) 0.0453(10) 0.0468(11) -0.0056(8) -0.0005(9) 0.0064(8) O1 0.0337(13) 0.0374(10) 0.0319(11) 0.0128(8) 0.0162(10) 0.0230(9) N1 0.0246(14) 0.0259(11) 0.0252(13) 0.0032(9) 0.0048(11) 0.0122(10) C1 0.0306(19) 0.0368(16) 0.0372(18) 0.0060(13) 0.0101(16) 0.0189(14) C2 0.049(2) 0.0341(17) 0.052(2) 0.0122(15) 0.0264(19) 0.0239(16) C3 0.053(2) 0.0502(19) 0.047(2) 0.0271(16) 0.0289(19) 0.0387(18) C4 0.0272(19) 0.070(2) 0.0290(18) 0.0225(15) 0.0099(15) 0.0282(17) C5 0.0256(18) 0.0393(16) 0.0302(17) 0.0055(13) 0.0113(15) 0.0114(14) C6 0.0277(17) 0.0311(14) 0.0276(16) 0.0072(12) 0.0096(14) 0.0170(13) C7 0.0190(16) 0.0246(13) 0.0219(15) 0.0002(11) 0.0014(13) 0.0069(11) C8 0.043(2) 0.0464(17) 0.0392(19) 0.0101(14) 0.0185(17) 0.0274(16) C9 0.048(2) 0.062(2) 0.043(2) 0.0071(16) 0.0246(18) 0.0305(18) C10 0.055(2) 0.063(2) 0.0338(19) 0.0136(16) 0.0257(18) 0.0233(19) C11 0.051(2) 0.0507(18) 0.0410(19) 0.0221(15) 0.0214(18) 0.0225(17) C12 0.038(2) 0.0367(15) 0.0391(19) 0.0131(13) 0.0164(16) 0.0207(14) C13 0.0240(17) 0.0248(13) 0.0269(16) 0.0002(11) 0.0065(13) 0.0080(12) C14 0.039(2) 0.0520(19) 0.040(2) -0.0144(15) 0.0125(18) 0.0007(17) C15 0.063(3) 0.0294(16) 0.0360(19) -0.0040(13) 0.0112(18) 0.0163(16) C16 0.045(2) 0.0475(18) 0.041(2) -0.0067(15) 0.0181(17) 0.0206(16) C17 0.074(3) 0.0477(18) 0.0243(18) 0.0034(13) 0.0199(18) 0.0192(18) C18 0.060(3) 0.068(2) 0.0280(19) -0.0069(16) -0.0060(18) 0.041(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 O1 1.9725(16) . no Ti1 N1 2.131(2) . no Ti1 Cl1 2.3152(7) . no Ti1 Cl2 2.3308(10) . no Ti1 C14 2.342(3) . no Ti1 C18 2.344(3) . no Ti1 C15 2.361(2) . no Ti1 C17 2.390(3) . no Ti1 C16 2.395(2) . no F1 C1 1.328(3) . no F2 C2 1.344(3) . no F3 C3 1.346(3) . no F4 C4 1.338(3) . no F5 C5 1.346(3) . no O1 C13 1.307(3) . no N1 C7 1.353(3) . no N1 C6 1.431(3) . no C1 C2 1.379(4) . no C1 C6 1.390(3) . no C2 C3 1.362(4) . no C3 C4 1.372(4) . no C4 C5 1.384(4) . no C5 C6 1.376(4) . no C7 C8 1.394(3) . no C7 C13 1.446(3) . no C8 C9 1.382(4) . no C8 H8 0.9300 . no C9 C10 1.373(4) . no C9 H9 0.9300 . no C10 C11 1.373(4) . no C10 H10 0.9300 . no C11 C12 1.384(3) . no C11 H11 0.9300 . no C12 C13 1.381(3) . no C12 H12 0.9300 . no C14 C15 1.391(4) . no C14 C18 1.393(4) . no C14 H14 0.9300 . no C15 C16 1.388(4) . no C15 H15 0.9300 . no C16 C17 1.385(4) . no C16 H16 0.9300 . no C17 C18 1.396(4) . no C17 H17 0.9300 . no C18 H18 0.9300 . no 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 N1 72.69(7) . . no O1 Ti1 Cl1 143.06(6) . . no N1 Ti1 Cl1 84.67(5) . . no O1 Ti1 Cl2 84.29(6) . . no N1 Ti1 Cl2 131.10(6) . . no Cl1 Ti1 Cl2 89.51(3) . . no O1 Ti1 C14 86.31(10) . . no N1 Ti1 C14 89.12(10) . . no Cl1 Ti1 C14 122.87(9) . . no Cl2 Ti1 C14 132.57(9) . . no O1 Ti1 C18 120.03(11) . . no N1 Ti1 C18 92.05(10) . . no Cl1 Ti1 C18 88.85(8) . . no Cl2 Ti1 C18 136.42(9) . . no C14 Ti1 C18 34.60(11) . . no O1 Ti1 C15 80.03(9) . . no N1 Ti1 C15 118.60(10) . . no Cl1 Ti1 C15 136.91(8) . . no Cl2 Ti1 C15 98.16(9) . . no C14 Ti1 C15 34.41(10) . . no C18 Ti1 C15 56.97(11) . . no O1 Ti1 C17 136.40(9) . . no N1 Ti1 C17 123.79(11) . . no Cl1 Ti1 C17 80.48(8) . . no Cl2 Ti1 C17 102.76(9) . . no C14 Ti1 C17 57.06(11) . . no C18 Ti1 C17 34.28(11) . . no C15 Ti1 C17 56.45(10) . . no O1 Ti1 C16 108.20(8) . . no N1 Ti1 C16 145.26(10) . . no Cl1 Ti1 C16 107.00(7) . . no Cl2 Ti1 C16 82.55(8) . . no C14 Ti1 C16 56.83(11) . . no C18 Ti1 C16 56.58(11) . . no C15 Ti1 C16 33.93(9) . . no C17 Ti1 C16 33.67(10) . . no C13 O1 Ti1 125.04(14) . . no C7 N1 C6 116.34(19) . . no C7 N1 Ti1 118.19(15) . . no C6 N1 Ti1 125.29(15) . . no F1 C1 C2 119.6(2) . . no F1 C1 C6 119.2(2) . . no C2 C1 C6 121.2(3) . . no F2 C2 C3 120.0(3) . . no F2 C2 C1 120.1(3) . . no C3 C2 C1 119.9(3) . . no F3 C3 C2 119.9(3) . . no F3 C3 C4 119.5(3) . . no C2 C3 C4 120.6(3) . . no F4 C4 C3 120.9(3) . . no F4 C4 C5 120.1(3) . . no C3 C4 C5 119.0(3) . . no F5 C5 C6 119.9(2) . . no F5 C5 C4 118.1(3) . . no C6 C5 C4 122.0(3) . . no C5 C6 C1 117.2(2) . . no C5 C6 N1 122.2(2) . . no C1 C6 N1 120.5(3) . . no N1 C7 C8 124.0(2) . . no N1 C7 C13 110.8(2) . . no C8 C7 C13 125.2(2) . . no C9 C8 C7 130.0(3) . . no C9 C8 H8 115.0 . . no C7 C8 H8 115.0 . . no C10 C9 C8 130.4(3) . . no C10 C9 H9 114.8 . . no C8 C9 H9 114.8 . . no C11 C10 C9 126.9(3) . . no C11 C10 H10 116.6 . . no C9 C10 H10 116.6 . . no C10 C11 C12 129.8(3) . . no C10 C11 H11 115.1 . . no C12 C11 H11 115.1 . . no C13 C12 C11 129.4(2) . . no C13 C12 H12 115.3 . . no C11 C12 H12 115.3 . . no O1 C13 C12 119.1(2) . . no O1 C13 C7 112.8(2) . . no C12 C13 C7 128.1(2) . . no C15 C14 C18 107.4(3) . . no C15 C14 Ti1 73.53(18) . . no C18 C14 Ti1 72.77(18) . . no C15 C14 H14 126.3 . . no C18 C14 H14 126.3 . . no Ti1 C14 H14 119.3 . . no C16 C15 C14 108.4(3) . . no C16 C15 Ti1 74.37(15) . . no C14 C15 Ti1 72.05(16) . . no C16 C15 H15 125.8 . . no C14 C15 H15 125.8 . . no Ti1 C15 H15 119.6 . . no C17 C16 C15 108.2(3) . . no C17 C16 Ti1 72.98(15) . . no C15 C16 Ti1 71.71(15) . . no C17 C16 H16 125.9 . . no C15 C16 H16 125.9 . . no Ti1 C16 H16 121.2 . . no C16 C17 C18 107.7(3) . . no C16 C17 Ti1 73.36(16) . . no C18 C17 Ti1 71.06(17) . . no C16 C17 H17 126.1 . . no C18 C17 H17 126.1 . . no Ti1 C17 H17 121.2 . . no C14 C18 C17 108.3(3) . . no C14 C18 Ti1 72.63(18) . . no C17 C18 Ti1 74.65(19) . . no C14 C18 H18 125.9 . . no C17 C18 H18 125.9 . . no Ti1 C18 H18 118.7 . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ti1 O1 C13 5.4(2) . . . . no Cl1 Ti1 O1 C13 -49.4(2) . . . . no Cl2 Ti1 O1 C13 -130.9(2) . . . . no C14 Ti1 O1 C13 95.6(2) . . . . no C18 Ti1 O1 C13 87.5(2) . . . . no C15 Ti1 O1 C13 129.7(2) . . . . no C17 Ti1 O1 C13 126.5(2) . . . . no C16 Ti1 O1 C13 148.9(2) . . . . no O1 Ti1 N1 C7 -6.03(17) . . . . no Cl1 Ti1 N1 C7 144.42(18) . . . . no Cl2 Ti1 N1 C7 59.75(19) . . . . no C14 Ti1 N1 C7 -92.44(19) . . . . no C18 Ti1 N1 C7 -126.92(19) . . . . no C15 Ti1 N1 C7 -73.9(2) . . . . no C17 Ti1 N1 C7 -140.79(18) . . . . no C16 Ti1 N1 C7 -103.2(2) . . . . no O1 Ti1 N1 C6 179.0(2) . . . . no Cl1 Ti1 N1 C6 -30.52(19) . . . . no Cl2 Ti1 N1 C6 -115.19(19) . . . . no C14 Ti1 N1 C6 92.6(2) . . . . no C18 Ti1 N1 C6 58.1(2) . . . . no C15 Ti1 N1 C6 111.1(2) . . . . no C17 Ti1 N1 C6 44.3(2) . . . . no C16 Ti1 N1 C6 81.9(2) . . . . no F1 C1 C2 F2 -1.4(4) . . . . no C6 C1 C2 F2 178.8(2) . . . . no F1 C1 C2 C3 179.0(3) . . . . no C6 C1 C2 C3 -0.8(4) . . . . no F2 C2 C3 F3 -0.3(4) . . . . no C1 C2 C3 F3 179.3(2) . . . . no F2 C2 C3 C4 179.3(2) . . . . no C1 C2 C3 C4 -1.1(4) . . . . no F3 C3 C4 F4 1.1(4) . . . . no C2 C3 C4 F4 -178.5(3) . . . . no F3 C3 C4 C5 -179.4(2) . . . . no C2 C3 C4 C5 1.0(4) . . . . no F4 C4 C5 F5 2.0(4) . . . . no C3 C4 C5 F5 -177.6(2) . . . . no F4 C4 C5 C6 -179.4(2) . . . . no C3 C4 C5 C6 1.1(4) . . . . no F5 C5 C6 C1 175.8(2) . . . . no C4 C5 C6 C1 -2.9(4) . . . . no F5 C5 C6 N1 -4.2(4) . . . . no C4 C5 C6 N1 177.1(2) . . . . no F1 C1 C6 C5 -177.0(2) . . . . no C2 C1 C6 C5 2.7(4) . . . . no F1 C1 C6 N1 2.9(4) . . . . no C2 C1 C6 N1 -177.3(2) . . . . no C7 N1 C6 C5 94.9(3) . . . . no Ti1 N1 C6 C5 -90.1(3) . . . . no C7 N1 C6 C1 -85.1(3) . . . . no Ti1 N1 C6 C1 89.9(3) . . . . no C6 N1 C7 C8 2.9(4) . . . . no Ti1 N1 C7 C8 -172.5(2) . . . . no C6 N1 C7 C13 -178.7(2) . . . . no Ti1 N1 C7 C13 5.9(3) . . . . no N1 C7 C8 C9 178.7(3) . . . . no C13 C7 C8 C9 0.5(5) . . . . no C7 C8 C9 C10 0.9(6) . . . . no C8 C9 C10 C11 1.5(6) . . . . no C9 C10 C11 C12 -2.6(6) . . . . no C10 C11 C12 C13 -1.0(6) . . . . no Ti1 O1 C13 C12 177.1(2) . . . . no Ti1 O1 C13 C7 -3.9(3) . . . . no C11 C12 C13 O1 -176.1(3) . . . . no C11 C12 C13 C7 5.1(5) . . . . no N1 C7 C13 O1 -1.7(3) . . . . no C8 C7 C13 O1 176.7(3) . . . . no N1 C7 C13 C12 177.2(3) . . . . no C8 C7 C13 C12 -4.4(4) . . . . no O1 Ti1 C14 C15 77.70(18) . . . . no N1 Ti1 C14 C15 150.41(18) . . . . no Cl1 Ti1 C14 C15 -126.52(16) . . . . no Cl2 Ti1 C14 C15 -1.1(2) . . . . no C18 Ti1 C14 C15 -114.7(3) . . . . no C17 Ti1 C14 C15 -77.31(19) . . . . no C16 Ti1 C14 C15 -36.89(16) . . . . no O1 Ti1 C14 C18 -167.60(19) . . . . no N1 Ti1 C14 C18 -94.9(2) . . . . no Cl1 Ti1 C14 C18 -11.8(2) . . . . no Cl2 Ti1 C14 C18 113.62(19) . . . . no C15 Ti1 C14 C18 114.7(3) . . . . no C17 Ti1 C14 C18 37.38(18) . . . . no C16 Ti1 C14 C18 77.8(2) . . . . no C18 C14 C15 C16 0.6(3) . . . . no Ti1 C14 C15 C16 66.0(2) . . . . no C18 C14 C15 Ti1 -65.4(2) . . . . no O1 Ti1 C15 C16 146.1(2) . . . . no N1 Ti1 C15 C16 -150.03(18) . . . . no Cl1 Ti1 C15 C16 -34.7(3) . . . . no Cl2 Ti1 C15 C16 63.38(19) . . . . no C14 Ti1 C15 C16 -115.8(3) . . . . no C18 Ti1 C15 C16 -77.8(2) . . . . no C17 Ti1 C15 C16 -36.55(19) . . . . no O1 Ti1 C15 C14 -98.11(19) . . . . no N1 Ti1 C15 C14 -34.2(2) . . . . no Cl1 Ti1 C15 C14 81.1(2) . . . . no Cl2 Ti1 C15 C14 179.20(17) . . . . no C18 Ti1 C15 C14 37.97(19) . . . . no C17 Ti1 C15 C14 79.3(2) . . . . no C16 Ti1 C15 C14 115.8(3) . . . . no C14 C15 C16 C17 -0.2(3) . . . . no Ti1 C15 C16 C17 64.3(2) . . . . no C14 C15 C16 Ti1 -64.5(2) . . . . no O1 Ti1 C16 C17 -151.82(19) . . . . no N1 Ti1 C16 C17 -66.1(3) . . . . no Cl1 Ti1 C16 C17 39.5(2) . . . . no Cl2 Ti1 C16 C17 126.7(2) . . . . no C14 Ti1 C16 C17 -79.0(2) . . . . no C18 Ti1 C16 C17 -37.35(19) . . . . no C15 Ti1 C16 C17 -116.5(3) . . . . no O1 Ti1 C16 C15 -35.4(2) . . . . no N1 Ti1 C16 C15 50.3(3) . . . . no Cl1 Ti1 C16 C15 156.00(18) . . . . no Cl2 Ti1 C16 C15 -116.81(19) . . . . no C14 Ti1 C16 C15 37.43(19) . . . . no C18 Ti1 C16 C15 79.1(2) . . . . no C17 Ti1 C16 C15 116.5(3) . . . . no C15 C16 C17 C18 -0.3(3) . . . . no Ti1 C16 C17 C18 63.2(2) . . . . no C15 C16 C17 Ti1 -63.5(2) . . . . no O1 Ti1 C17 C16 40.6(3) . . . . no N1 Ti1 C17 C16 141.16(18) . . . . no Cl1 Ti1 C17 C16 -141.9(2) . . . . no Cl2 Ti1 C17 C16 -54.6(2) . . . . no C14 Ti1 C17 C16 78.3(2) . . . . no C18 Ti1 C17 C16 116.0(3) . . . . no C15 Ti1 C17 C16 36.84(19) . . . . no O1 Ti1 C17 C18 -75.4(2) . . . . no N1 Ti1 C17 C18 25.2(2) . . . . no Cl1 Ti1 C17 C18 102.12(17) . . . . no Cl2 Ti1 C17 C18 -170.56(16) . . . . no C14 Ti1 C17 C18 -37.73(18) . . . . no C15 Ti1 C17 C18 -79.16(19) . . . . no C16 Ti1 C17 C18 -116.0(3) . . . . no C15 C14 C18 C17 -0.8(3) . . . . no Ti1 C14 C18 C17 -66.7(2) . . . . no C15 C14 C18 Ti1 65.9(2) . . . . no C16 C17 C18 C14 0.7(3) . . . . no Ti1 C17 C18 C14 65.4(2) . . . . no C16 C17 C18 Ti1 -64.7(2) . . . . no O1 Ti1 C18 C14 14.3(2) . . . . no N1 Ti1 C18 C14 85.47(19) . . . . no Cl1 Ti1 C18 C14 170.09(19) . . . . no Cl2 Ti1 C18 C14 -101.8(2) . . . . no C15 Ti1 C18 C14 -37.76(17) . . . . no C17 Ti1 C18 C14 -115.2(3) . . . . no C16 Ti1 C18 C14 -78.6(2) . . . . no O1 Ti1 C18 C17 129.57(17) . . . . no N1 Ti1 C18 C17 -159.29(17) . . . . no Cl1 Ti1 C18 C17 -74.67(17) . . . . no Cl2 Ti1 C18 C17 13.4(2) . . . . no C14 Ti1 C18 C17 115.2(3) . . . . no C15 Ti1 C18 C17 77.48(18) . . . . no C16 Ti1 C18 C17 36.66(16) . . . . no _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.349 _refine_diff_density_min -0.286 _refine_diff_density_rms 0.067 data_tropII _database_code_depnum_ccdc_archive 'CCDC 252930' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C23 H15 Cl3 F5 N1 O2 Ti2, C1 H2 Cl2' _chemical_formula_sum 'C24 H17 Cl5 F5 N1 O2 Ti2' _chemical_formula_weight 719.38 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.990(2) _cell_length_b 11.647(2) _cell_length_c 13.425(5) _cell_angle_alpha 94.23(2) _cell_angle_beta 113.80(2) _cell_angle_gamma 113.96(2) _cell_volume 1377.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.68 _cell_measurement_theta_max 14.87 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.24 _exptl_crystal_density_diffrn 1.734 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 1.124 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 2 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_absorpt_correction_T_min 0.9335 _exptl_absorpt_correction_T_max 0.9567 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_wavelength 0.71069 _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'scintillation LiF' _diffrn_detector_dtime 1.195 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega scans' _diffrn_standards_number 1 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 5 -7 2 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 1 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_UB_11 -0.085379 _diffrn_orient_matrix_UB_12 -0.035663 _diffrn_orient_matrix_UB_13 0.018423 _diffrn_orient_matrix_UB_21 0.032481 _diffrn_orient_matrix_UB_22 -0.064188 _diffrn_orient_matrix_UB_23 0.030747 _diffrn_orient_matrix_UB_31 0.066852 _diffrn_orient_matrix_UB_32 0.064897 _diffrn_orient_matrix_UB_33 0.076976 _diffrn_ambient_temperature 293(2) _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_number 6924 _diffrn_reflns_av_R_equivalents 0.0134 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.96 _reflns_number_total 6643 _reflns_number_gt 4685 _reflns_threshold_expression >2sigma(I) _symmetry_Int_Tables_number 2 _computing_data_collection 'MACH3 Software (Enraf Nonius, 1996)' _computing_cell_refinement 'MACH3 Software(Enraf Nonius, 1996)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+0.6302P] 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_number_reflns 6643 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0725 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.1069 _refine_ls_wR_factor_gt 0.0945 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.003 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 0.63232(5) 0.30725(4) 0.22062(4) 0.03208(11) Uani 1 1 d . . . Ti2 Ti 0.71273(6) 0.08036(5) 0.36566(4) 0.03759(12) Uani 1 1 d . . . Cl2 Cl 0.58646(10) 0.35874(8) 0.36564(7) 0.0583(2) Uani 1 1 d . . . Cl3 Cl 0.46577(9) -0.07137(8) 0.29205(9) 0.0661(2) Uani 1 1 d . . . Cl4 Cl 0.79185(10) -0.03064(8) 0.28230(7) 0.0567(2) Uani 1 1 d . . . Cl5 Cl 0.40367(13) 0.59467(13) 0.36466(10) 0.0894(3) Uani 1 1 d . . . Cl6 Cl 0.34021(17) 0.54515(15) 0.13040(10) 0.1056(4) Uani 1 1 d . . . F1 F 1.0624(2) 0.42049(19) 0.41546(16) 0.0689(5) Uani 1 1 d . . . F2 F 1.2289(2) 0.2962(2) 0.44929(19) 0.0852(7) Uani 1 1 d . . . F3 F 1.1805(2) 0.1263(2) 0.2706(2) 0.0795(7) Uani 1 1 d . . . F4 F 0.9633(3) 0.0795(2) 0.06051(19) 0.0790(6) Uani 1 1 d . . . F5 F 0.7956(2) 0.20297(19) 0.02621(15) 0.0624(5) Uani 1 1 d . . . O1 O 0.6951(2) 0.49214(17) 0.22070(17) 0.0435(4) Uani 1 1 d . . . O2 O 0.70541(19) 0.19671(17) 0.29306(15) 0.0377(4) Uani 1 1 d . . . N1 N 0.8347(2) 0.3792(2) 0.20723(18) 0.0354(5) Uani 1 1 d . . . C1 C 1.0364(3) 0.3367(3) 0.3268(3) 0.0468(7) Uani 1 1 d . . . C2 C 1.1237(3) 0.2743(3) 0.3440(3) 0.0549(8) Uani 1 1 d . . . C3 C 1.0988(3) 0.1891(3) 0.2539(3) 0.0535(8) Uani 1 1 d . . . C4 C 0.9884(4) 0.1648(3) 0.1481(3) 0.0501(7) Uani 1 1 d . . . C5 C 0.9012(3) 0.2270(3) 0.1316(3) 0.0430(6) Uani 1 1 d . . . C6 C 0.9230(3) 0.3141(2) 0.2207(2) 0.0367(6) Uani 1 1 d . . . C7 C 0.8883(3) 0.4983(2) 0.1895(2) 0.0337(5) Uani 1 1 d . . . C8 C 1.0118(3) 0.5527(3) 0.1693(3) 0.0460(7) Uani 1 1 d . . . H8 H 1.0560 0.4999 0.1675 0.046 Uiso 1 1 calc R . . C9 C 1.0785(4) 0.6720(3) 0.1516(3) 0.0563(8) Uani 1 1 d . . . H9 H 1.1612 0.6876 0.1403 0.056 Uiso 1 1 calc R . . C10 C 1.0421(4) 0.7722(3) 0.1479(3) 0.0568(8) Uani 1 1 d . . . H10 H 1.1017 0.8452 0.1334 0.057 Uiso 1 1 calc R . . C11 C 0.9282(3) 0.7764(3) 0.1633(3) 0.0507(7) Uani 1 1 d . . . H11 H 0.9204 0.8525 0.1577 0.051 Uiso 1 1 calc R . . C12 C 0.8236(3) 0.6845(3) 0.1858(2) 0.0421(6) Uani 1 1 d . . . H12 H 0.7569 0.7087 0.1948 0.042 Uiso 1 1 calc R . . C13 C 0.8017(3) 0.5611(2) 0.1973(2) 0.0348(5) Uani 1 1 d . . . C14 C 0.4643(4) 0.1091(3) 0.0758(3) 0.0604(9) Uani 1 1 d . . . H14 H 0.4863 0.0399 0.0775 0.060 Uiso 1 1 calc R . . C15 C 0.3842(3) 0.1328(3) 0.1242(3) 0.0589(8) Uani 1 1 d . . . H15 H 0.3441 0.0829 0.1649 0.059 Uiso 1 1 calc R . . C16 C 0.3742(3) 0.2429(4) 0.1017(3) 0.0640(9) Uani 1 1 d . . . H16 H 0.3259 0.2803 0.1245 0.064 Uiso 1 1 calc R . . C17 C 0.4483(4) 0.2883(3) 0.0392(3) 0.0609(9) Uani 1 1 d . . . H17 H 0.4578 0.3610 0.0121 0.061 Uiso 1 1 calc R . . C18 C 0.5061(4) 0.2060(4) 0.0242(3) 0.0617(9) Uani 1 1 d . . . H18 H 0.5626 0.2145 -0.0136 0.062 Uiso 1 1 calc R . . C19 C 0.8624(6) 0.2464(4) 0.5341(3) 0.0786(12) Uani 1 1 d . . . H19 H 0.8917 0.3328 0.5321 0.079 Uiso 1 1 calc R . . C20 C 0.7343(5) 0.1647(5) 0.5380(3) 0.0787(12) Uani 1 1 d . . . H20 H 0.6600 0.1848 0.5367 0.079 Uiso 1 1 calc R . . C21 C 0.7349(5) 0.0458(4) 0.5443(3) 0.0761(11) Uani 1 1 d . . . H21 H 0.6622 -0.0268 0.5497 0.076 Uiso 1 1 calc R . . C22 C 0.8620(5) 0.0551(4) 0.5411(3) 0.0715(11) Uani 1 1 d . . . H22 H 0.8897 -0.0106 0.5434 0.072 Uiso 1 1 calc R . . C23 C 0.9418(4) 0.1789(5) 0.5337(3) 0.0743(11) Uani 1 1 d . . . H23 H 1.0314 0.2109 0.5294 0.074 Uiso 1 1 calc R . . C24 C 0.4806(4) 0.6136(4) 0.2730(3) 0.0691(10) Uani 1 1 d . . . H24A H 0.5442 0.5719 0.2888 0.069 Uiso 1 1 calc R . . H24B H 0.5438 0.7062 0.2862 0.069 Uiso 1 1 calc R . . 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 0.0301(2) 0.0292(2) 0.0360(2) 0.00852(18) 0.01372(19) 0.01542(18) Ti2 0.0437(3) 0.0368(2) 0.0388(3) 0.0149(2) 0.0204(2) 0.0234(2) Cl2 0.0784(6) 0.0651(5) 0.0554(5) 0.0186(4) 0.0416(4) 0.0451(4) Cl3 0.0507(4) 0.0552(5) 0.0879(6) 0.0301(4) 0.0356(4) 0.0172(4) Cl4 0.0689(5) 0.0515(4) 0.0674(5) 0.0164(4) 0.0382(4) 0.0384(4) Cl5 0.0861(7) 0.1205(9) 0.0860(7) 0.0415(7) 0.0521(6) 0.0573(7) Cl6 0.1428(11) 0.1328(11) 0.0773(7) 0.0305(7) 0.0497(8) 0.0995(10) F1 0.0579(11) 0.0646(12) 0.0560(11) -0.0070(9) 0.0035(9) 0.0321(10) F2 0.0587(12) 0.1019(17) 0.0808(15) 0.0242(13) 0.0073(11) 0.0520(13) F3 0.0768(14) 0.0838(14) 0.130(2) 0.0551(14) 0.0623(14) 0.0657(13) F4 0.1056(17) 0.0803(14) 0.0906(16) 0.0203(12) 0.0603(14) 0.0659(14) F5 0.0725(12) 0.0736(13) 0.0503(11) 0.0122(9) 0.0265(10) 0.0463(11) O1 0.0447(10) 0.0346(9) 0.0623(13) 0.0168(9) 0.0295(10) 0.0239(8) O2 0.0383(10) 0.0365(9) 0.0420(10) 0.0153(8) 0.0185(8) 0.0211(8) N1 0.0326(11) 0.0306(10) 0.0452(12) 0.0114(9) 0.0181(10) 0.0174(9) C1 0.0373(14) 0.0382(14) 0.0581(18) 0.0102(13) 0.0178(13) 0.0176(12) C2 0.0343(15) 0.0563(18) 0.069(2) 0.0253(16) 0.0157(14) 0.0246(14) C3 0.0481(17) 0.0490(17) 0.088(2) 0.0332(17) 0.0418(18) 0.0332(15) C4 0.0568(18) 0.0434(15) 0.073(2) 0.0225(15) 0.0434(17) 0.0301(14) C5 0.0449(15) 0.0412(14) 0.0524(17) 0.0170(13) 0.0275(14) 0.0238(13) C6 0.0317(12) 0.0302(12) 0.0517(16) 0.0153(11) 0.0218(12) 0.0152(10) C7 0.0319(12) 0.0291(12) 0.0334(13) 0.0074(10) 0.0101(10) 0.0142(10) C8 0.0402(15) 0.0400(14) 0.0614(18) 0.0180(13) 0.0245(14) 0.0214(12) C9 0.0465(17) 0.0511(18) 0.079(2) 0.0306(17) 0.0361(17) 0.0217(14) C10 0.0555(19) 0.0391(16) 0.073(2) 0.0260(15) 0.0328(17) 0.0158(14) C11 0.0555(18) 0.0334(14) 0.0570(18) 0.0171(13) 0.0202(15) 0.0216(13) C12 0.0439(15) 0.0343(13) 0.0456(15) 0.0105(12) 0.0157(13) 0.0222(12) C13 0.0323(12) 0.0317(12) 0.0327(13) 0.0068(10) 0.0095(10) 0.0149(10) C14 0.0564(19) 0.0439(17) 0.0478(18) -0.0074(14) 0.0004(15) 0.0227(15) C15 0.0359(15) 0.0503(18) 0.060(2) 0.0087(15) 0.0134(14) 0.0047(14) C16 0.0357(16) 0.076(2) 0.067(2) 0.0091(18) 0.0103(15) 0.0312(16) C17 0.0492(18) 0.060(2) 0.0474(18) 0.0165(15) 0.0008(15) 0.0253(16) C18 0.0503(18) 0.081(2) 0.0366(16) 0.0041(16) 0.0114(14) 0.0272(18) C19 0.113(3) 0.063(2) 0.0343(17) 0.0031(16) 0.015(2) 0.042(2) C20 0.107(3) 0.115(4) 0.051(2) 0.026(2) 0.045(2) 0.078(3) C21 0.096(3) 0.095(3) 0.054(2) 0.040(2) 0.044(2) 0.050(3) C22 0.095(3) 0.096(3) 0.0466(19) 0.034(2) 0.029(2) 0.068(3) C23 0.062(2) 0.103(3) 0.0355(17) 0.0099(19) 0.0097(16) 0.035(2) C24 0.067(2) 0.063(2) 0.093(3) 0.024(2) 0.046(2) 0.0372(19) _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 O2 1.9085(17) . no Ti1 O1 1.9762(18) . no Ti1 N1 2.124(2) . no Ti1 Cl2 2.2956(11) . no Ti1 C14 2.345(3) . no Ti1 C15 2.346(3) . no Ti1 C18 2.351(3) . no Ti1 C16 2.366(3) . no Ti1 C17 2.377(3) . no Ti2 O2 1.7358(17) . no Ti2 Cl3 2.2689(13) . no Ti2 Cl4 2.2725(10) . no Ti2 C19 2.309(4) . no Ti2 C20 2.326(4) . no Ti2 C23 2.331(4) . no Ti2 C22 2.387(3) . no Ti2 C21 2.393(4) . no Cl5 C24 1.734(4) . no Cl6 C24 1.753(4) . no F1 C1 1.333(3) . no F2 C2 1.337(4) . no F3 C3 1.336(3) . no F4 C4 1.337(4) . no F5 C5 1.334(3) . no O1 C13 1.299(3) . no N1 C7 1.351(3) . no N1 C6 1.424(3) . no C1 C6 1.377(4) . no C1 C2 1.384(4) . no C2 C3 1.364(5) . no C3 C4 1.358(5) . no C4 C5 1.381(4) . no C5 C6 1.381(4) . no C7 C8 1.393(4) . no C7 C13 1.444(3) . no C8 C9 1.374(4) . no C8 H8 0.9300 . no C9 C10 1.376(4) . no C9 H9 0.9300 . no C10 C11 1.367(4) . no C10 H10 0.9300 . no C11 C12 1.374(4) . no C11 H11 0.9300 . no C12 C13 1.388(3) . no C12 H12 0.9300 . no C14 C15 1.380(5) . no C14 C18 1.384(5) . no C14 H14 0.9300 . no C15 C16 1.376(5) . no C15 H15 0.9300 . no C16 C17 1.383(5) . no C16 H16 0.9300 . no C17 C18 1.390(5) . no C17 H17 0.9300 . no C18 H18 0.9300 . no C19 C20 1.367(6) . no C19 C23 1.393(6) . no C19 H19 0.9300 . no C20 C21 1.396(6) . no C20 H20 0.9300 . no C21 C22 1.376(5) . no C21 H21 0.9300 . no C22 C23 1.386(6) . no C22 H22 0.9300 . no C23 H23 0.9300 . no C24 H24A 0.9700 . no C24 H24B 0.9700 . no 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 O2 Ti1 O1 142.29(8) . . no O2 Ti1 N1 82.49(8) . . no O1 Ti1 N1 72.85(8) . . no O2 Ti1 Cl2 90.44(6) . . no O1 Ti1 Cl2 85.36(6) . . no N1 Ti1 Cl2 131.56(7) . . no O2 Ti1 C14 80.73(10) . . no O1 Ti1 C14 132.56(11) . . no N1 Ti1 C14 104.87(12) . . no Cl2 Ti1 C14 121.21(11) . . no O2 Ti1 C15 91.06(11) . . no O1 Ti1 C15 126.21(11) . . no N1 Ti1 C15 138.88(11) . . no Cl2 Ti1 C15 88.82(10) . . no C14 Ti1 C15 34.22(12) . . no O2 Ti1 C18 106.41(11) . . no O1 Ti1 C18 99.95(12) . . no N1 Ti1 C18 85.98(11) . . no Cl2 Ti1 C18 141.18(9) . . no C14 Ti1 C18 34.27(12) . . no C15 Ti1 C18 56.93(13) . . no O2 Ti1 C16 124.71(11) . . no O1 Ti1 C16 92.25(11) . . no N1 Ti1 C16 137.27(12) . . no Cl2 Ti1 C16 84.81(10) . . no C14 Ti1 C16 56.56(13) . . no C15 Ti1 C16 33.96(12) . . no C18 Ti1 C16 56.73(13) . . no O2 Ti1 C17 137.15(11) . . no O1 Ti1 C17 77.43(11) . . no N1 Ti1 C17 103.40(11) . . no Cl2 Ti1 C17 113.48(10) . . no C14 Ti1 C17 56.58(12) . . no C15 Ti1 C17 56.48(13) . . no C18 Ti1 C17 34.18(12) . . no C16 Ti1 C17 33.91(12) . . no O2 Ti2 Cl3 103.29(7) . . no O2 Ti2 Cl4 103.60(7) . . no Cl3 Ti2 Cl4 99.93(5) . . no O2 Ti2 C19 88.93(12) . . no Cl3 Ti2 C19 128.14(14) . . no Cl4 Ti2 C19 126.17(13) . . no O2 Ti2 C20 104.83(13) . . no Cl3 Ti2 C20 94.46(13) . . no Cl4 Ti2 C20 144.07(11) . . no C19 Ti2 C20 34.30(15) . . no O2 Ti2 C23 108.36(13) . . no Cl3 Ti2 C23 141.97(11) . . no Cl4 Ti2 C23 92.70(11) . . no C19 Ti2 C23 34.93(15) . . no C20 Ti2 C23 57.59(15) . . no O2 Ti2 C22 142.18(13) . . no Cl3 Ti2 C22 110.39(12) . . no Cl4 Ti2 C22 87.34(10) . . no C19 Ti2 C22 56.82(14) . . no C20 Ti2 C22 56.74(14) . . no C23 Ti2 C22 34.15(14) . . no O2 Ti2 C21 139.22(13) . . no Cl3 Ti2 C21 85.57(12) . . no Cl4 Ti2 C21 114.08(11) . . no C19 Ti2 C21 56.66(15) . . no C20 Ti2 C21 34.39(14) . . no C23 Ti2 C21 56.64(15) . . no C22 Ti2 C21 33.45(13) . . no C13 O1 Ti1 123.74(16) . . no Ti2 O2 Ti1 158.56(11) . . no C7 N1 C6 116.9(2) . . no C7 N1 Ti1 118.11(16) . . no C6 N1 Ti1 124.96(16) . . no F1 C1 C6 119.2(2) . . no F1 C1 C2 119.0(3) . . no C6 C1 C2 121.7(3) . . no F2 C2 C3 120.9(3) . . no F2 C2 C1 119.4(3) . . no C3 C2 C1 119.6(3) . . no F3 C3 C4 120.0(3) . . no F3 C3 C2 119.8(3) . . no C4 C3 C2 120.2(3) . . no F4 C4 C3 119.8(3) . . no F4 C4 C5 120.4(3) . . no C3 C4 C5 119.8(3) . . no F5 C5 C6 120.0(2) . . no F5 C5 C4 118.3(3) . . no C6 C5 C4 121.7(3) . . no C1 C6 C5 116.9(2) . . no C1 C6 N1 119.8(2) . . no C5 C6 N1 123.3(2) . . no N1 C7 C8 124.3(2) . . no N1 C7 C13 110.3(2) . . no C8 C7 C13 125.4(2) . . no C9 C8 C7 130.1(3) . . no C9 C8 H8 114.9 . . no C7 C8 H8 114.9 . . no C8 C9 C10 130.2(3) . . no C8 C9 H9 114.9 . . no C10 C9 H9 114.9 . . no C11 C10 C9 127.3(3) . . no C11 C10 H10 116.4 . . no C9 C10 H10 116.4 . . no C10 C11 C12 129.3(3) . . no C10 C11 H11 115.3 . . no C12 C11 H11 115.3 . . no C11 C12 C13 130.2(3) . . no C11 C12 H12 114.9 . . no C13 C12 H12 114.9 . . no O1 C13 C12 118.8(2) . . no O1 C13 C7 113.8(2) . . no C12 C13 C7 127.4(2) . . no C15 C14 C18 108.2(3) . . no C15 C14 Ti1 72.94(18) . . no C18 C14 Ti1 73.11(19) . . no C15 C14 H14 125.9 . . no C18 C14 H14 125.9 . . no Ti1 C14 H14 119.9 . . no C16 C15 C14 108.2(3) . . no C16 C15 Ti1 73.84(18) . . no C14 C15 Ti1 72.85(18) . . no C16 C15 H15 125.9 . . no C14 C15 H15 125.9 . . no Ti1 C15 H15 119.2 . . no C15 C16 C17 108.2(3) . . no C15 C16 Ti1 72.20(18) . . no C17 C16 Ti1 73.49(18) . . no C15 C16 H16 125.9 . . no C17 C16 H16 125.9 . . no Ti1 C16 H16 120.2 . . no C16 C17 C18 107.8(3) . . no C16 C17 Ti1 72.61(18) . . no C18 C17 Ti1 71.86(18) . . no C16 C17 H17 126.1 . . no C18 C17 H17 126.1 . . no Ti1 C17 H17 121.2 . . no C14 C18 C17 107.6(3) . . no C14 C18 Ti1 72.62(18) . . no C17 C18 Ti1 73.96(19) . . no C14 C18 H18 126.2 . . no C17 C18 H18 126.2 . . no Ti1 C18 H18 119.1 . . no C20 C19 C23 108.8(4) . . no C20 C19 Ti2 73.5(2) . . no C23 C19 Ti2 73.4(2) . . no C20 C19 H19 125.6 . . no C23 C19 H19 125.6 . . no Ti2 C19 H19 119.2 . . no C19 C20 C21 107.8(4) . . no C19 C20 Ti2 72.2(2) . . no C21 C20 Ti2 75.4(2) . . no C19 C20 H20 126.1 . . no C21 C20 H20 126.1 . . no Ti2 C20 H20 118.3 . . no C22 C21 C20 107.8(4) . . no C22 C21 Ti2 73.1(2) . . no C20 C21 Ti2 70.2(2) . . no C22 C21 H21 126.1 . . no C20 C21 H21 126.1 . . no Ti2 C21 H21 122.4 . . no C21 C22 C23 108.5(4) . . no C21 C22 Ti2 73.5(2) . . no C23 C22 Ti2 70.70(19) . . no C21 C22 H22 125.8 . . no C23 C22 H22 125.8 . . no Ti2 C22 H22 121.7 . . no C22 C23 C19 107.1(4) . . no C22 C23 Ti2 75.2(2) . . no C19 C23 Ti2 71.7(2) . . no C22 C23 H23 126.5 . . no C19 C23 H23 126.4 . . no Ti2 C23 H23 118.7 . . no Cl5 C24 Cl6 111.9(2) . . no Cl5 C24 H24A 109.2 . . no Cl6 C24 H24A 109.2 . . no Cl5 C24 H24B 109.2 . . no Cl6 C24 H24B 109.2 . . no H24A C24 H24B 107.9 . . no 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 O2 Ti1 O1 C13 61.8(3) . . . . no N1 Ti1 O1 C13 10.36(19) . . . . no Cl2 Ti1 O1 C13 146.5(2) . . . . no C14 Ti1 O1 C13 -84.3(2) . . . . no C15 Ti1 O1 C13 -128.3(2) . . . . no C18 Ti1 O1 C13 -72.2(2) . . . . no C16 Ti1 O1 C13 -128.8(2) . . . . no C17 Ti1 O1 C13 -98.1(2) . . . . no Cl3 Ti2 O2 Ti1 37.8(3) . . . . no Cl4 Ti2 O2 Ti1 141.7(3) . . . . no C19 Ti2 O2 Ti1 -91.2(3) . . . . no C20 Ti2 O2 Ti1 -60.5(3) . . . . no C23 Ti2 O2 Ti1 -120.8(3) . . . . no C22 Ti2 O2 Ti1 -114.8(3) . . . . no C21 Ti2 O2 Ti1 -60.9(4) . . . . no O1 Ti1 O2 Ti2 126.1(3) . . . . no N1 Ti1 O2 Ti2 175.1(3) . . . . no Cl2 Ti1 O2 Ti2 43.2(3) . . . . no C14 Ti1 O2 Ti2 -78.4(3) . . . . no C15 Ti1 O2 Ti2 -45.7(3) . . . . no C18 Ti1 O2 Ti2 -101.4(3) . . . . no C16 Ti1 O2 Ti2 -40.8(4) . . . . no C17 Ti1 O2 Ti2 -83.3(3) . . . . no O2 Ti1 N1 C7 -160.28(19) . . . . no O1 Ti1 N1 C7 -9.14(18) . . . . no Cl2 Ti1 N1 C7 -76.4(2) . . . . no C14 Ti1 N1 C7 121.4(2) . . . . no C15 Ti1 N1 C7 116.8(2) . . . . no C18 Ti1 N1 C7 92.6(2) . . . . no C16 Ti1 N1 C7 65.0(3) . . . . no C17 Ti1 N1 C7 62.9(2) . . . . no O2 Ti1 N1 C6 16.7(2) . . . . no O1 Ti1 N1 C6 167.8(2) . . . . no Cl2 Ti1 N1 C6 100.6(2) . . . . no C14 Ti1 N1 C6 -61.6(2) . . . . no C15 Ti1 N1 C6 -66.3(3) . . . . no C18 Ti1 N1 C6 -90.5(2) . . . . no C16 Ti1 N1 C6 -118.0(2) . . . . no C17 Ti1 N1 C6 -120.1(2) . . . . no F1 C1 C2 F2 1.9(4) . . . . no C6 C1 C2 F2 -177.7(3) . . . . no F1 C1 C2 C3 -179.6(3) . . . . no C6 C1 C2 C3 0.8(5) . . . . no F2 C2 C3 F3 0.0(5) . . . . no C1 C2 C3 F3 -178.5(3) . . . . no F2 C2 C3 C4 178.0(3) . . . . no C1 C2 C3 C4 -0.5(5) . . . . no F3 C3 C4 F4 -1.0(4) . . . . no C2 C3 C4 F4 -179.0(3) . . . . no F3 C3 C4 C5 178.2(3) . . . . no C2 C3 C4 C5 0.2(5) . . . . no F4 C4 C5 F5 -2.2(4) . . . . no C3 C4 C5 F5 178.7(3) . . . . no F4 C4 C5 C6 179.0(3) . . . . no C3 C4 C5 C6 -0.1(4) . . . . no F1 C1 C6 C5 179.7(2) . . . . no C2 C1 C6 C5 -0.7(4) . . . . no F1 C1 C6 N1 -0.5(4) . . . . no C2 C1 C6 N1 179.1(3) . . . . no F5 C5 C6 C1 -178.4(2) . . . . no C4 C5 C6 C1 0.3(4) . . . . no F5 C5 C6 N1 1.7(4) . . . . no C4 C5 C6 N1 -179.5(2) . . . . no C7 N1 C6 C1 87.9(3) . . . . no Ti1 N1 C6 C1 -89.1(3) . . . . no C7 N1 C6 C5 -92.3(3) . . . . no Ti1 N1 C6 C5 90.7(3) . . . . no C6 N1 C7 C8 8.6(4) . . . . no Ti1 N1 C7 C8 -174.2(2) . . . . no C6 N1 C7 C13 -170.1(2) . . . . no Ti1 N1 C7 C13 7.1(3) . . . . no N1 C7 C8 C9 -179.1(3) . . . . no C13 C7 C8 C9 -0.6(5) . . . . no C7 C8 C9 C10 -0.5(6) . . . . no C8 C9 C10 C11 1.1(6) . . . . no C9 C10 C11 C12 0.1(6) . . . . no C10 C11 C12 C13 -1.3(6) . . . . no Ti1 O1 C13 C12 171.95(19) . . . . no Ti1 O1 C13 C7 -9.8(3) . . . . no C11 C12 C13 O1 178.9(3) . . . . no C11 C12 C13 C7 1.0(5) . . . . no N1 C7 C13 O1 1.0(3) . . . . no C8 C7 C13 O1 -177.7(3) . . . . no N1 C7 C13 C12 179.0(3) . . . . no C8 C7 C13 C12 0.3(4) . . . . no O2 Ti1 C14 C15 105.8(2) . . . . no O1 Ti1 C14 C15 -94.4(2) . . . . no N1 Ti1 C14 C15 -174.5(2) . . . . no Cl2 Ti1 C14 C15 21.0(2) . . . . no C18 Ti1 C14 C15 -115.8(3) . . . . no C16 Ti1 C14 C15 -37.2(2) . . . . no C17 Ti1 C14 C15 -78.1(2) . . . . no O2 Ti1 C14 C18 -138.4(2) . . . . no O1 Ti1 C14 C18 21.4(3) . . . . no N1 Ti1 C14 C18 -58.8(2) . . . . no Cl2 Ti1 C14 C18 136.77(19) . . . . no C15 Ti1 C14 C18 115.8(3) . . . . no C16 Ti1 C14 C18 78.6(2) . . . . no C17 Ti1 C14 C18 37.7(2) . . . . no C18 C14 C15 C16 0.8(4) . . . . no Ti1 C14 C15 C16 65.9(2) . . . . no C18 C14 C15 Ti1 -65.1(2) . . . . no O2 Ti1 C15 C16 172.9(2) . . . . no O1 Ti1 C15 C16 -0.9(3) . . . . no N1 Ti1 C15 C16 -107.4(2) . . . . no Cl2 Ti1 C15 C16 82.4(2) . . . . no C14 Ti1 C15 C16 -115.4(3) . . . . no C18 Ti1 C15 C16 -78.2(2) . . . . no C17 Ti1 C15 C16 -37.0(2) . . . . no O2 Ti1 C15 C14 -71.7(2) . . . . no O1 Ti1 C15 C14 114.5(2) . . . . no N1 Ti1 C15 C14 8.0(3) . . . . no Cl2 Ti1 C15 C14 -162.2(2) . . . . no C18 Ti1 C15 C14 37.2(2) . . . . no C16 Ti1 C15 C14 115.4(3) . . . . no C17 Ti1 C15 C14 78.4(2) . . . . no C14 C15 C16 C17 -0.1(4) . . . . no Ti1 C15 C16 C17 65.2(2) . . . . no C14 C15 C16 Ti1 -65.3(2) . . . . no O2 Ti1 C16 C15 -8.7(3) . . . . no O1 Ti1 C16 C15 179.2(2) . . . . no N1 Ti1 C16 C15 112.3(2) . . . . no Cl2 Ti1 C16 C15 -95.6(2) . . . . no C14 Ti1 C16 C15 37.5(2) . . . . no C18 Ti1 C16 C15 78.8(2) . . . . no C17 Ti1 C16 C15 115.9(3) . . . . no O2 Ti1 C16 C17 -124.6(2) . . . . no O1 Ti1 C16 C17 63.3(2) . . . . no N1 Ti1 C16 C17 -3.6(3) . . . . no Cl2 Ti1 C16 C17 148.5(2) . . . . no C14 Ti1 C16 C17 -78.4(2) . . . . no C15 Ti1 C16 C17 -115.9(3) . . . . no C18 Ti1 C16 C17 -37.1(2) . . . . no C15 C16 C17 C18 -0.7(4) . . . . no Ti1 C16 C17 C18 63.7(2) . . . . no C15 C16 C17 Ti1 -64.3(2) . . . . no O2 Ti1 C17 C16 84.1(3) . . . . no O1 Ti1 C17 C16 -113.8(2) . . . . no N1 Ti1 C17 C16 177.5(2) . . . . no Cl2 Ti1 C17 C16 -34.6(2) . . . . no C14 Ti1 C17 C16 78.4(2) . . . . no C15 Ti1 C17 C16 37.1(2) . . . . no C18 Ti1 C17 C16 116.1(3) . . . . no O2 Ti1 C17 C18 -32.0(3) . . . . no O1 Ti1 C17 C18 130.0(2) . . . . no N1 Ti1 C17 C18 61.4(2) . . . . no Cl2 Ti1 C17 C18 -150.7(2) . . . . no C14 Ti1 C17 C18 -37.8(2) . . . . no C15 Ti1 C17 C18 -79.1(2) . . . . no C16 Ti1 C17 C18 -116.1(3) . . . . no C15 C14 C18 C17 -1.2(4) . . . . no Ti1 C14 C18 C17 -66.2(2) . . . . no C15 C14 C18 Ti1 65.0(2) . . . . no C16 C17 C18 C14 1.2(4) . . . . no Ti1 C17 C18 C14 65.3(2) . . . . no C16 C17 C18 Ti1 -64.2(2) . . . . no O2 Ti1 C18 C14 43.1(2) . . . . no O1 Ti1 C18 C14 -164.2(2) . . . . no N1 Ti1 C18 C14 124.1(2) . . . . no Cl2 Ti1 C18 C14 -69.2(3) . . . . no C15 Ti1 C18 C14 -37.2(2) . . . . no C16 Ti1 C18 C14 -78.0(2) . . . . no C17 Ti1 C18 C14 -114.8(3) . . . . no O2 Ti1 C18 C17 157.9(2) . . . . no O1 Ti1 C18 C17 -49.3(2) . . . . no N1 Ti1 C18 C17 -121.1(2) . . . . no Cl2 Ti1 C18 C17 45.7(3) . . . . no C14 Ti1 C18 C17 114.8(3) . . . . no C15 Ti1 C18 C17 77.6(2) . . . . no C16 Ti1 C18 C17 36.8(2) . . . . no O2 Ti2 C19 C20 118.8(2) . . . . no Cl3 Ti2 C19 C20 12.7(3) . . . . no Cl4 Ti2 C19 C20 -135.1(2) . . . . no C23 Ti2 C19 C20 -116.0(4) . . . . no C22 Ti2 C19 C20 -78.2(3) . . . . no C21 Ti2 C19 C20 -38.0(2) . . . . no O2 Ti2 C19 C23 -125.2(3) . . . . no Cl3 Ti2 C19 C23 128.7(2) . . . . no Cl4 Ti2 C19 C23 -19.1(3) . . . . no C20 Ti2 C19 C23 116.0(4) . . . . no C22 Ti2 C19 C23 37.7(2) . . . . no C21 Ti2 C19 C23 78.0(3) . . . . no C23 C19 C20 C21 2.1(4) . . . . no Ti2 C19 C20 C21 67.6(3) . . . . no C23 C19 C20 Ti2 -65.5(3) . . . . no O2 Ti2 C20 C19 -65.0(3) . . . . no Cl3 Ti2 C20 C19 -170.0(2) . . . . no Cl4 Ti2 C20 C19 76.2(3) . . . . no C23 Ti2 C20 C19 37.6(2) . . . . no C22 Ti2 C20 C19 78.5(3) . . . . no C21 Ti2 C20 C19 114.5(4) . . . . no O2 Ti2 C20 C21 -179.5(3) . . . . no Cl3 Ti2 C20 C21 75.4(3) . . . . no Cl4 Ti2 C20 C21 -38.3(4) . . . . no C19 Ti2 C20 C21 -114.5(4) . . . . no C23 Ti2 C20 C21 -77.0(3) . . . . no C22 Ti2 C20 C21 -36.1(3) . . . . no C19 C20 C21 C22 -1.6(4) . . . . no Ti2 C20 C21 C22 63.8(3) . . . . no C19 C20 C21 Ti2 -65.4(3) . . . . no O2 Ti2 C21 C22 -116.1(3) . . . . no Cl3 Ti2 C21 C22 138.7(3) . . . . no Cl4 Ti2 C21 C22 39.8(3) . . . . no C19 Ti2 C21 C22 -78.9(3) . . . . no C20 Ti2 C21 C22 -116.7(4) . . . . no C23 Ti2 C21 C22 -36.8(3) . . . . no O2 Ti2 C21 C20 0.7(4) . . . . no Cl3 Ti2 C21 C20 -104.6(3) . . . . no Cl4 Ti2 C21 C20 156.5(3) . . . . no C19 Ti2 C21 C20 37.9(3) . . . . no C23 Ti2 C21 C20 80.0(3) . . . . no C22 Ti2 C21 C20 116.7(4) . . . . no C20 C21 C22 C23 0.5(4) . . . . no Ti2 C21 C22 C23 62.4(2) . . . . no C20 C21 C22 Ti2 -62.0(3) . . . . no O2 Ti2 C22 C21 106.9(3) . . . . no Cl3 Ti2 C22 C21 -44.6(3) . . . . no Cl4 Ti2 C22 C21 -144.2(3) . . . . no C19 Ti2 C22 C21 78.4(3) . . . . no C20 Ti2 C22 C21 37.1(3) . . . . no C23 Ti2 C22 C21 117.0(4) . . . . no O2 Ti2 C22 C23 -10.1(3) . . . . no Cl3 Ti2 C22 C23 -161.6(2) . . . . no Cl4 Ti2 C22 C23 98.8(2) . . . . no C19 Ti2 C22 C23 -38.6(3) . . . . no C20 Ti2 C22 C23 -79.9(3) . . . . no C21 Ti2 C22 C23 -117.0(4) . . . . no C21 C22 C23 C19 0.8(4) . . . . no Ti2 C22 C23 C19 65.0(2) . . . . no C21 C22 C23 Ti2 -64.2(3) . . . . no C20 C19 C23 C22 -1.8(4) . . . . no Ti2 C19 C23 C22 -67.4(3) . . . . no C20 C19 C23 Ti2 65.6(3) . . . . no O2 Ti2 C23 C22 173.5(2) . . . . no Cl3 Ti2 C23 C22 28.7(3) . . . . no Cl4 Ti2 C23 C22 -81.2(2) . . . . no C19 Ti2 C23 C22 114.1(4) . . . . no C20 Ti2 C23 C22 77.2(3) . . . . no C21 Ti2 C23 C22 36.0(2) . . . . no O2 Ti2 C23 C19 59.4(3) . . . . no Cl3 Ti2 C23 C19 -85.4(3) . . . . no Cl4 Ti2 C23 C19 164.7(3) . . . . no C20 Ti2 C23 C19 -36.9(2) . . . . no C22 Ti2 C23 C19 -114.1(4) . . . . no C21 Ti2 C23 C19 -78.1(3) . . . . no _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.96 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.511 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.063 data_tropIII _database_code_depnum_ccdc_archive 'CCDC 252931' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C38 H44 Cl2 N2 O2 Ti1' _chemical_formula_sum 'C38 H44 Cl2 N2 O2 Ti1' _chemical_formula_weight 679.55 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 12.310(10) _cell_length_b 16.80(5) _cell_length_c 17.040(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.39(5) _cell_angle_gamma 90.00 _cell_volume 3524(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 11.35 _cell_measurement_theta_max 12.38 _exptl_crystal_density_diffrn 1.281 _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.430 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 2 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_absorpt_correction_T_min 0.7457 _exptl_absorpt_correction_T_max 0.8755 _diffrn_ambient_temperature 293 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.3 _exptl_crystal_density_method 'not measured' _chemical_compound_source 'synthesis as described' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _diffrn_radiation_type Mok\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_wavelength 0.71069 _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega scans' _diffrn_standards_number 1 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 6 2 -4 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_UB_11 -0.028729 _diffrn_orient_matrix_UB_12 -0.001848 _diffrn_orient_matrix_UB_13 -0.055076 _diffrn_orient_matrix_UB_21 0.075817 _diffrn_orient_matrix_UB_22 0.003654 _diffrn_orient_matrix_UB_23 -0.020432 _diffrn_orient_matrix_UB_31 0.005651 _diffrn_orient_matrix_UB_32 -0.058546 _diffrn_orient_matrix_UB_33 0.000492 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_number 8885 _diffrn_reflns_av_R_equivalents 0.0170 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 28.37 _reflns_number_total 8601 _reflns_number_gt 5722 _reflns_threshold_expression >2sigma(I) _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^)+(0.0628P)^2^+0.5961P] 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_number_reflns 8601 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0901 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1306 _refine_ls_wR_factor_gt 0.1144 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.002 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 0.34119(3) 0.23626(2) 0.22381(2) 0.03588(11) Uani 1 1 d . . . Cl1 Cl 0.30141(5) 0.16499(4) 0.11402(4) 0.05682(18) Uani 1 1 d . . . Cl2 Cl 0.33434(5) 0.13128(4) 0.30627(4) 0.05644(18) Uani 1 1 d . . . O1A O 0.39339(12) 0.32406(10) 0.16225(10) 0.0468(4) Uani 1 1 d . . . O1B O 0.32853(12) 0.30634(10) 0.31322(9) 0.0458(4) Uani 1 1 d . . . N1A N 0.51237(13) 0.22847(10) 0.22826(10) 0.0342(4) Uani 1 1 d . . . N1B N 0.17654(13) 0.27359(10) 0.22447(10) 0.0332(4) Uani 1 1 d . . . C1A C 0.60698(18) 0.19218(16) 0.34942(14) 0.0479(6) Uani 1 1 d . . . C2A C 0.6605(2) 0.1350(2) 0.39314(17) 0.0650(8) Uani 1 1 d . . . H2A H 0.6828 0.1467 0.4441 0.065 Uiso 1 1 calc R . . C3A C 0.6809(2) 0.0625(2) 0.3627(2) 0.0746(10) Uani 1 1 d . . . H3A H 0.7170 0.0246 0.3930 0.075 Uiso 1 1 calc R . . C4A C 0.6493(2) 0.04403(17) 0.2886(2) 0.0674(8) Uani 1 1 d . . . H4A H 0.6646 -0.0064 0.2691 0.067 Uiso 1 1 calc R . . C5A C 0.59482(18) 0.09818(14) 0.24072(16) 0.0488(6) Uani 1 1 d . . . C6A C 0.57399(16) 0.17168(13) 0.27337(13) 0.0398(5) Uani 1 1 d . . . C7A C 0.56756(16) 0.28419(12) 0.18986(12) 0.0342(4) Uani 1 1 d . . . C8A C 0.68165(18) 0.28562(15) 0.18452(14) 0.0458(5) Uani 1 1 d . . . H8A H 0.7166 0.2424 0.2077 0.046 Uiso 1 1 calc R . . C9A C 0.7492(2) 0.33994(17) 0.15098(17) 0.0583(7) Uani 1 1 d . . . H9A H 0.8227 0.3274 0.1535 0.058 Uiso 1 1 calc R . . C10A C 0.7248(2) 0.41037(18) 0.11404(18) 0.0652(8) Uani 1 1 d . . . H10A H 0.7835 0.4411 0.0982 0.065 Uiso 1 1 calc R . . C11A C 0.6249(3) 0.44013(16) 0.09798(17) 0.0627(7) Uani 1 1 d . . . H11A H 0.6243 0.4891 0.0726 0.063 Uiso 1 1 calc R . . C12A C 0.5235(2) 0.40862(14) 0.11365(15) 0.0519(6) Uani 1 1 d . . . H12A H 0.4653 0.4381 0.0942 0.052 Uiso 1 1 calc R . . C13A C 0.49557(18) 0.34066(13) 0.15341(13) 0.0382(5) Uani 1 1 d . . . C14A C 0.5607(2) 0.07632(15) 0.15879(18) 0.0582(7) Uani 1 1 d . . . H14A H 0.5136 0.1190 0.1391 0.058 Uiso 1 1 calc R . . C15A C 0.4961(3) -0.0002(2) 0.1553(2) 0.0897(11) Uani 1 1 d . . . H15A H 0.4763 -0.0115 0.1019 0.090 Uiso 1 1 calc R . . H15B H 0.4316 0.0053 0.1862 0.090 Uiso 1 1 calc R . . H15C H 0.5394 -0.0431 0.1758 0.090 Uiso 1 1 calc R . . C16A C 0.6588(3) 0.0719(2) 0.1050(2) 0.0771(9) Uani 1 1 d . . . H16A H 0.6354 0.0579 0.0530 0.077 Uiso 1 1 calc R . . H16B H 0.7085 0.0323 0.1244 0.077 Uiso 1 1 calc R . . H16C H 0.6944 0.1227 0.1039 0.077 Uiso 1 1 calc R . . C17A C 0.5864(2) 0.27212(18) 0.38508(15) 0.0555(7) Uani 1 1 d . . . H17A H 0.5429 0.3028 0.3474 0.056 Uiso 1 1 calc R . . C18A C 0.5222(3) 0.2671(3) 0.46045(18) 0.0865(11) Uani 1 1 d . . . H18A H 0.5112 0.3197 0.4810 0.086 Uiso 1 1 calc R . . H18B H 0.5617 0.2357 0.4981 0.086 Uiso 1 1 calc R . . H18C H 0.4531 0.2427 0.4500 0.086 Uiso 1 1 calc R . . C19A C 0.6921(3) 0.3164(2) 0.3975(2) 0.0838(10) Uani 1 1 d . . . H19A H 0.6775 0.3675 0.4204 0.084 Uiso 1 1 calc R . . H19B H 0.7275 0.3235 0.3480 0.084 Uiso 1 1 calc R . . H19C H 0.7384 0.2863 0.4320 0.084 Uiso 1 1 calc R . . C1B C 0.07748(17) 0.28676(14) 0.09911(13) 0.0424(5) Uani 1 1 d . . . C2B C -0.0027(2) 0.25826(18) 0.04859(15) 0.0572(7) Uani 1 1 d . . . H2B H -0.0129 0.2825 0.0000 0.057 Uiso 1 1 calc R . . C3B C -0.0662(2) 0.1958(2) 0.06882(18) 0.0647(8) Uani 1 1 d . . . H3B H -0.1199 0.1779 0.0345 0.065 Uiso 1 1 calc R . . C4B C -0.0513(2) 0.15920(17) 0.13960(17) 0.0577(7) Uani 1 1 d . . . H4B H -0.0954 0.1163 0.1527 0.058 Uiso 1 1 calc R . . C5B C 0.02760(17) 0.18408(14) 0.19255(14) 0.0439(5) Uani 1 1 d . . . C6B C 0.09224(16) 0.24823(13) 0.17083(12) 0.0369(5) Uani 1 1 d . . . C7B C 0.14724(17) 0.31882(12) 0.28459(12) 0.0349(4) Uani 1 1 d . . . C8B C 0.04085(19) 0.34830(14) 0.29440(15) 0.0480(6) Uani 1 1 d . . . H8B H -0.0066 0.3373 0.2531 0.048 Uiso 1 1 calc R . . C9B C -0.0035(2) 0.39026(16) 0.35455(16) 0.0566(7) Uani 1 1 d . . . H9B H -0.0762 0.4040 0.3478 0.057 Uiso 1 1 calc R . . C10B C 0.0433(2) 0.41550(16) 0.42426(17) 0.0614(7) Uani 1 1 d . . . H10B H -0.0024 0.4418 0.4589 0.061 Uiso 1 1 calc R . . C11B C 0.1481(3) 0.40643(16) 0.44822(16) 0.0604(7) Uani 1 1 d . . . H11B H 0.1644 0.4271 0.4975 0.060 Uiso 1 1 calc R . . C12B C 0.2335(2) 0.37109(14) 0.41003(14) 0.0488(6) Uani 1 1 d . . . H12B H 0.2992 0.3722 0.4372 0.049 Uiso 1 1 calc R . . C13B C 0.23689(17) 0.33426(13) 0.33787(12) 0.0374(5) Uani 1 1 d . . . C14B C 0.0406(2) 0.14217(16) 0.27027(16) 0.0547(6) Uani 1 1 d . . . H14B H 0.1004 0.1680 0.2987 0.055 Uiso 1 1 calc R . . C15B C -0.0606(3) 0.1495(2) 0.32024(19) 0.0801(10) Uani 1 1 d . . . H15D H -0.0782 0.2047 0.3271 0.080 Uiso 1 1 calc R . . H15E H -0.0475 0.1256 0.3706 0.080 Uiso 1 1 calc R . . H15F H -0.1200 0.1229 0.2947 0.080 Uiso 1 1 calc R . . C16B C 0.0717(3) 0.05696(18) 0.2579(2) 0.0871(11) Uani 1 1 d . . . H16D H 0.0797 0.0310 0.3078 0.087 Uiso 1 1 calc R . . H16E H 0.1392 0.0545 0.2301 0.087 Uiso 1 1 calc R . . H16F H 0.0161 0.0307 0.2278 0.087 Uiso 1 1 calc R . . C17B C 0.1431(2) 0.35777(16) 0.07660(15) 0.0500(6) Uani 1 1 d . . . H17B H 0.1959 0.3680 0.1187 0.050 Uiso 1 1 calc R . . C18B C 0.0705(3) 0.42954(19) 0.0695(2) 0.0811(10) Uani 1 1 d . . . H18D H 0.1131 0.4750 0.0550 0.081 Uiso 1 1 calc R . . H18E H 0.0361 0.4394 0.1190 0.081 Uiso 1 1 calc R . . H18F H 0.0160 0.4200 0.0301 0.081 Uiso 1 1 calc R . . C19B C 0.2054(3) 0.3460(2) 0.0008(2) 0.0842(10) Uani 1 1 d . . . H19D H 0.2460 0.3933 -0.0108 0.084 Uiso 1 1 calc R . . H19E H 0.1552 0.3354 -0.0413 0.084 Uiso 1 1 calc R . . H19F H 0.2543 0.3019 0.0065 0.084 Uiso 1 1 calc R . . 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 0.02996(18) 0.0419(2) 0.0358(2) 0.00178(17) 0.00013(14) 0.00108(16) Cl1 0.0487(3) 0.0719(4) 0.0499(4) -0.0182(3) -0.0053(3) 0.0111(3) Cl2 0.0472(3) 0.0600(4) 0.0622(4) 0.0217(3) 0.0049(3) -0.0019(3) O1A 0.0396(8) 0.0468(9) 0.0540(10) 0.0157(8) 0.0023(7) 0.0069(7) O1B 0.0374(8) 0.0553(10) 0.0447(9) -0.0096(8) -0.0060(7) -0.0022(7) N1A 0.0334(8) 0.0340(9) 0.0351(9) 0.0020(7) -0.0007(7) 0.0018(7) N1B 0.0307(8) 0.0372(9) 0.0318(8) -0.0003(7) 0.0005(7) -0.0010(7) C1A 0.0339(11) 0.0627(16) 0.0472(13) 0.0138(12) -0.0035(9) -0.0024(10) C2A 0.0518(15) 0.087(2) 0.0556(16) 0.0283(16) -0.0098(12) -0.0028(15) C3A 0.0515(16) 0.074(2) 0.098(3) 0.049(2) -0.0124(16) 0.0043(14) C4A 0.0506(15) 0.0428(14) 0.109(3) 0.0240(16) -0.0018(16) 0.0066(12) C5A 0.0358(11) 0.0406(13) 0.0698(17) 0.0086(12) 0.0013(11) 0.0033(10) C6A 0.0286(10) 0.0423(12) 0.0486(13) 0.0136(10) 0.0010(9) 0.0010(9) C7A 0.0356(10) 0.0348(11) 0.0321(10) -0.0042(8) 0.0016(8) -0.0005(8) C8A 0.0397(12) 0.0491(13) 0.0486(13) 0.0025(11) 0.0023(10) -0.0012(10) C9A 0.0429(13) 0.0679(18) 0.0641(17) -0.0009(14) 0.0057(12) -0.0139(12) C10A 0.0643(18) 0.0594(17) 0.0719(19) 0.0047(15) 0.0112(14) -0.0262(14) C11A 0.084(2) 0.0388(14) 0.0652(18) 0.0047(13) 0.0173(15) -0.0128(14) C12A 0.0631(15) 0.0403(13) 0.0525(15) 0.0056(11) 0.0097(12) 0.0069(11) C13A 0.0419(11) 0.0357(11) 0.0371(11) -0.0013(9) 0.0050(9) 0.0032(9) C14A 0.0569(15) 0.0355(13) 0.082(2) -0.0067(13) -0.0031(14) 0.0102(11) C15A 0.081(2) 0.064(2) 0.125(3) -0.024(2) 0.002(2) -0.0120(17) C16A 0.083(2) 0.065(2) 0.083(2) -0.0027(17) 0.0084(18) 0.0077(16) C17A 0.0476(14) 0.0776(19) 0.0413(13) 0.0002(13) -0.0070(10) 0.0004(13) C18A 0.076(2) 0.129(3) 0.0540(18) -0.003(2) 0.0073(16) 0.001(2) C19A 0.072(2) 0.097(3) 0.082(2) -0.024(2) -0.0064(17) -0.0141(19) C1B 0.0362(11) 0.0521(13) 0.0388(12) -0.0039(10) -0.0015(9) 0.0086(10) C2B 0.0511(14) 0.0787(19) 0.0417(13) -0.0039(13) -0.0097(11) 0.0103(14) C3B 0.0452(14) 0.082(2) 0.0668(18) -0.0227(16) -0.0190(13) -0.0004(14) C4B 0.0432(13) 0.0588(16) 0.0709(18) -0.0094(14) -0.0084(12) -0.0078(12) C5B 0.0343(11) 0.0451(13) 0.0524(14) -0.0057(11) -0.0026(9) -0.0020(9) C6B 0.0299(10) 0.0437(12) 0.0370(11) -0.0071(9) -0.0007(8) 0.0044(8) C7B 0.0393(11) 0.0300(10) 0.0353(11) 0.0033(9) 0.0026(8) -0.0033(8) C8B 0.0426(12) 0.0492(14) 0.0522(14) -0.0063(11) 0.0017(10) 0.0047(10) C9B 0.0538(15) 0.0509(15) 0.0651(17) -0.0084(13) 0.0122(12) 0.0086(12) C10B 0.0779(19) 0.0509(15) 0.0558(16) -0.0128(13) 0.0180(14) 0.0083(14) C11B 0.087(2) 0.0529(16) 0.0413(14) -0.0118(12) 0.0046(13) 0.0021(14) C12B 0.0622(15) 0.0450(13) 0.0392(12) -0.0049(10) -0.0066(11) -0.0025(11) C13B 0.0431(11) 0.0331(11) 0.0359(11) 0.0023(9) 0.0011(9) -0.0046(9) C14B 0.0489(14) 0.0506(15) 0.0644(17) 0.0077(13) -0.0060(12) -0.0157(11) C15B 0.075(2) 0.096(3) 0.069(2) 0.0092(19) 0.0117(16) -0.0237(19) C16B 0.089(2) 0.0500(18) 0.122(3) 0.0151(19) -0.012(2) -0.0115(17) C17B 0.0461(13) 0.0593(15) 0.0446(13) 0.0090(12) -0.0049(10) 0.0074(11) C18B 0.080(2) 0.0566(18) 0.107(3) 0.0045(18) -0.0060(19) 0.0102(16) C19B 0.096(3) 0.087(2) 0.070(2) 0.0174(18) 0.0289(18) 0.003(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 O1A 1.923(4) . no Ti1 O1B 1.933(3) . no Ti1 N1A 2.112(5) . no Ti1 N1B 2.122(5) . no Ti1 Cl2 2.257(4) . no Ti1 Cl1 2.272(6) . no O1A C13A 1.298(3) . no O1B C13B 1.294(3) . no N1A C7A 1.331(3) . no N1A C6A 1.438(3) . no N1B C7B 1.327(3) . no N1B C6B 1.443(3) . no C1A C2A 1.380(4) . no C1A C6A 1.399(3) . no C1A C17A 1.496(5) . no C2A C3A 1.349(6) . no C2A H2A 0.9300 . no C3A C4A 1.355(5) . no C3A H3A 0.9300 . no C4A C5A 1.391(4) . no C4A H4A 0.9300 . no C5A C6A 1.379(5) . no C5A C14A 1.501(4) . no C7A C8A 1.408(3) . no C7A C13A 1.437(4) . no C8A C9A 1.363(4) . no C8A H8A 0.9300 . no C9A C10A 1.372(5) . no C9A H9A 0.9300 . no C10A C11A 1.354(4) . no C10A H10A 0.9300 . no C11A C12A 1.383(4) . no C11A H11A 0.9300 . no C12A C13A 1.373(4) . no C12A H12A 0.9300 . no C14A C15A 1.513(5) . no C14A C16A 1.523(4) . no C14A H14A 0.9800 . no C15A H15A 0.9600 . no C15A H15B 0.9600 . no C15A H15C 0.9600 . no C16A H16A 0.9600 . no C16A H16B 0.9600 . no C16A H16C 0.9600 . no C17A C19A 1.512(4) . no C17A C18A 1.515(4) . no C17A H17A 0.9800 . no C18A H18A 0.9600 . no C18A H18B 0.9600 . no C18A H18C 0.9600 . no C19A H19A 0.9600 . no C19A H19B 0.9600 . no C19A H19C 0.9600 . no C1B C2B 1.390(3) . no C1B C6B 1.394(3) . no C1B C17B 1.493(5) . no C2B C3B 1.354(5) . no C2B H2B 0.9300 . no C3B C4B 1.365(4) . no C3B H3B 0.9300 . no C4B C5B 1.386(3) . no C4B H4B 0.9300 . no C5B C6B 1.391(4) . no C5B C14B 1.508(4) . no C7B C8B 1.411(3) . no C7B C13B 1.448(3) . no C8B C9B 1.361(4) . no C8B H8B 0.9300 . no C9B C10B 1.383(4) . no C9B H9B 0.9300 . no C10B C11B 1.359(4) . no C10B H10B 0.9300 . no C11B C12B 1.375(4) . no C11B H11B 0.9300 . no C12B C13B 1.377(3) . no C12B H12B 0.9300 . no C14B C16B 1.497(6) . no C14B C15B 1.519(4) . no C14B H14B 0.9800 . no C15B H15D 0.9600 . no C15B H15E 0.9600 . no C15B H15F 0.9600 . no C16B H16D 0.9600 . no C16B H16E 0.9600 . no C16B H16F 0.9600 . no C17B C18B 1.505(5) . no C17B C19B 1.520(4) . no C17B H17B 0.9800 . no C18B H18D 0.9600 . no C18B H18E 0.9600 . no C18B H18F 0.9600 . no C19B H19D 0.9600 . no C19B H19E 0.9600 . no C19B H19F 0.9600 . no 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 O1A Ti1 O1B 89.53(18) . . no O1A Ti1 N1A 74.34(8) . . no O1B Ti1 N1A 95.47(8) . . no O1A Ti1 N1B 95.67(12) . . no O1B Ti1 N1B 74.55(9) . . no N1A Ti1 N1B 166.16(8) . . no O1A Ti1 Cl2 162.37(6) . . no O1B Ti1 Cl2 88.95(7) . . no N1A Ti1 Cl2 88.33(6) . . no N1B Ti1 Cl2 100.83(8) . . no O1A Ti1 Cl1 91.49(7) . . no O1B Ti1 Cl1 162.21(5) . . no N1A Ti1 Cl1 101.91(7) . . no N1B Ti1 Cl1 87.68(9) . . no Cl2 Ti1 Cl1 95.28(6) . . no C13A O1A Ti1 123.76(14) . . no C13B O1B Ti1 123.49(15) . . no C7A N1A C6A 117.4(2) . . no C7A N1A Ti1 116.82(15) . . no C6A N1A Ti1 125.64(14) . . no C7B N1B C6B 117.39(17) . . no C7B N1B Ti1 115.97(14) . . no C6B N1B Ti1 126.33(15) . . no C2A C1A C6A 117.6(3) . . no C2A C1A C17A 119.1(3) . . no C6A C1A C17A 123.3(2) . . no C3A C2A C1A 120.7(3) . . no C3A C2A H2A 119.6 . . no C1A C2A H2A 119.6 . . no C2A C3A C4A 120.8(3) . . no C2A C3A H3A 119.6 . . no C4A C3A H3A 119.6 . . no C3A C4A C5A 122.1(3) . . no C3A C4A H4A 119.0 . . no C5A C4A H4A 119.0 . . no C6A C5A C4A 116.0(3) . . no C6A C5A C14A 122.9(2) . . no C4A C5A C14A 121.1(3) . . no C5A C6A C1A 122.7(2) . . no C5A C6A N1A 118.5(2) . . no C1A C6A N1A 118.7(2) . . no N1A C7A C8A 123.8(2) . . no N1A C7A C13A 111.2(2) . . no C8A C7A C13A 125.0(2) . . no C9A C8A C7A 130.6(3) . . no C9A C8A H8A 114.7 . . no C7A C8A H8A 114.7 . . no C8A C9A C10A 129.6(3) . . no C8A C9A H9A 115.2 . . no C10A C9A H9A 115.2 . . no C11A C10A C9A 127.3(3) . . no C11A C10A H10A 116.3 . . no C9A C10A H10A 116.3 . . no C10A C11A C12A 129.7(3) . . no C10A C11A H11A 115.1 . . no C12A C11A H11A 115.1 . . no C13A C12A C11A 130.0(3) . . no C13A C12A H12A 115.0 . . no C11A C12A H12A 115.0 . . no O1A C13A C12A 118.9(2) . . no O1A C13A C7A 113.8(2) . . no C12A C13A C7A 127.3(2) . . no C5A C14A C15A 112.8(3) . . no C5A C14A C16A 110.7(2) . . no C15A C14A C16A 110.7(3) . . no C5A C14A H14A 107.5 . . no C15A C14A H14A 107.5 . . no C16A C14A H14A 107.5 . . no C14A C15A H15A 109.5 . . no C14A C15A H15B 109.5 . . no H15A C15A H15B 109.5 . . no C14A C15A H15C 109.5 . . no H15A C15A H15C 109.5 . . no H15B C15A H15C 109.5 . . no C14A C16A H16A 109.5 . . no C14A C16A H16B 109.5 . . no H16A C16A H16B 109.5 . . no C14A C16A H16C 109.5 . . no H16A C16A H16C 109.5 . . no H16B C16A H16C 109.5 . . no C1A C17A C19A 110.5(3) . . no C1A C17A C18A 112.6(3) . . no C19A C17A C18A 111.2(3) . . no C1A C17A H17A 107.4 . . no C19A C17A H17A 107.4 . . no C18A C17A H17A 107.4 . . no C17A C18A H18A 109.5 . . no C17A C18A H18B 109.5 . . no H18A C18A H18B 109.5 . . no C17A C18A H18C 109.5 . . no H18A C18A H18C 109.5 . . no H18B C18A H18C 109.5 . . no C17A C19A H19A 109.5 . . no C17A C19A H19B 109.5 . . no H19A C19A H19B 109.5 . . no C17A C19A H19C 109.5 . . no H19A C19A H19C 109.5 . . no H19B C19A H19C 109.5 . . no C2B C1B C6B 118.1(3) . . no C2B C1B C17B 120.0(2) . . no C6B C1B C17B 121.9(2) . . no C3B C2B C1B 121.2(3) . . no C3B C2B H2B 119.4 . . no C1B C2B H2B 119.4 . . no C2B C3B C4B 120.0(3) . . no C2B C3B H3B 120.0 . . no C4B C3B H3B 120.0 . . no C3B C4B C5B 121.9(3) . . no C3B C4B H4B 119.0 . . no C5B C4B H4B 119.0 . . no C4B C5B C6B 117.4(2) . . no C4B C5B C14B 120.1(2) . . no C6B C5B C14B 122.5(2) . . no C5B C6B C1B 121.4(2) . . no C5B C6B N1B 118.1(2) . . no C1B C6B N1B 120.5(2) . . no N1B C7B C8B 123.3(2) . . no N1B C7B C13B 112.13(19) . . no C8B C7B C13B 124.5(2) . . no C9B C8B C7B 130.4(2) . . no C9B C8B H8B 114.8 . . no C7B C8B H8B 114.8 . . no C8B C9B C10B 129.7(3) . . no C8B C9B H9B 115.2 . . no C10B C9B H9B 115.2 . . no C11B C10B C9B 127.8(3) . . no C11B C10B H10B 116.1 . . no C9B C10B H10B 116.1 . . no C10B C11B C12B 129.3(3) . . no C10B C11B H11B 115.4 . . no C12B C11B H11B 115.4 . . no C11B C12B C13B 130.2(3) . . no C11B C12B H12B 114.9 . . no C13B C12B H12B 114.9 . . no O1B C13B C12B 119.0(2) . . no O1B C13B C7B 113.2(2) . . no C12B C13B C7B 127.8(2) . . no C16B C14B C5B 110.4(3) . . no C16B C14B C15B 111.6(3) . . no C5B C14B C15B 111.8(2) . . no C16B C14B H14B 107.6 . . no C5B C14B H14B 107.6 . . no C15B C14B H14B 107.6 . . no C14B C15B H15D 109.5 . . no C14B C15B H15E 109.5 . . no H15D C15B H15E 109.5 . . no C14B C15B H15F 109.5 . . no H15D C15B H15F 109.5 . . no H15E C15B H15F 109.5 . . no C14B C16B H16D 109.5 . . no C14B C16B H16E 109.5 . . no H16D C16B H16E 109.5 . . no C14B C16B H16F 109.5 . . no H16D C16B H16F 109.5 . . no H16E C16B H16F 109.5 . . no C1B C17B C18B 109.8(3) . . no C1B C17B C19B 113.1(3) . . no C18B C17B C19B 109.8(3) . . no C1B C17B H17B 108.0 . . no C18B C17B H17B 108.0 . . no C19B C17B H17B 108.0 . . no C17B C18B H18D 109.5 . . no C17B C18B H18E 109.5 . . no H18D C18B H18E 109.5 . . no C17B C18B H18F 109.5 . . no H18D C18B H18F 109.5 . . no H18E C18B H18F 109.5 . . no C17B C19B H19D 109.5 . . no C17B C19B H19E 109.5 . . no H19D C19B H19E 109.5 . . no C17B C19B H19F 109.5 . . no H19D C19B H19F 109.5 . . no H19E C19B H19F 109.5 . . no 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 O1B Ti1 O1A C13A 93.35(19) . . . . no N1A Ti1 O1A C13A -2.46(17) . . . . no N1B Ti1 O1A C13A 167.77(17) . . . . no Cl2 Ti1 O1A C13A 8.3(3) . . . . no Cl1 Ti1 O1A C13A -104.41(19) . . . . no O1A Ti1 O1B C13B 103.79(18) . . . . no N1A Ti1 O1B C13B 178.01(17) . . . . no N1B Ti1 O1B C13B 7.77(17) . . . . no Cl2 Ti1 O1B C13B -93.78(17) . . . . no Cl1 Ti1 O1B C13B 10.4(3) . . . . no O1A Ti1 N1A C7A 0.54(15) . . . . no O1B Ti1 N1A C7A -87.4(2) . . . . no N1B Ti1 N1A C7A -44.4(4) . . . . no Cl2 Ti1 N1A C7A -176.22(14) . . . . no Cl1 Ti1 N1A C7A 88.7(2) . . . . no O1A Ti1 N1A C6A 176.02(18) . . . . no O1B Ti1 N1A C6A 88.0(2) . . . . no N1B Ti1 N1A C6A 131.1(3) . . . . no Cl2 Ti1 N1A C6A -0.74(17) . . . . no Cl1 Ti1 N1A C6A -95.8(2) . . . . no O1A Ti1 N1B C7B -92.1(2) . . . . no O1B Ti1 N1B C7B -4.13(14) . . . . no N1A Ti1 N1B C7B -49.0(3) . . . . no Cl2 Ti1 N1B C7B 81.7(2) . . . . no Cl1 Ti1 N1B C7B 176.68(14) . . . . no O1A Ti1 N1B C6B 94.6(2) . . . . no O1B Ti1 N1B C6B -177.50(18) . . . . no N1A Ti1 N1B C6B 137.6(3) . . . . no Cl2 Ti1 N1B C6B -91.6(2) . . . . no Cl1 Ti1 N1B C6B 3.31(16) . . . . no C6A C1A C2A C3A 0.7(4) . . . . no C17A C1A C2A C3A -179.7(3) . . . . no C1A C2A C3A C4A 0.1(4) . . . . no C2A C3A C4A C5A -0.2(5) . . . . no C3A C4A C5A C6A -0.4(4) . . . . no C3A C4A C5A C14A -180.0(3) . . . . no C4A C5A C6A C1A 1.2(3) . . . . no C14A C5A C6A C1A -179.3(2) . . . . no C4A C5A C6A N1A -176.5(2) . . . . no C14A C5A C6A N1A 3.0(3) . . . . no C2A C1A C6A C5A -1.3(3) . . . . no C17A C1A C6A C5A 179.0(2) . . . . no C2A C1A C6A N1A 176.3(2) . . . . no C17A C1A C6A N1A -3.3(3) . . . . no C7A N1A C6A C5A -98.5(3) . . . . no Ti1 N1A C6A C5A 86.1(2) . . . . no C7A N1A C6A C1A 83.7(3) . . . . no Ti1 N1A C6A C1A -91.7(2) . . . . no C6A N1A C7A C8A 6.7(3) . . . . no Ti1 N1A C7A C8A -177.41(17) . . . . no C6A N1A C7A C13A -174.79(18) . . . . no Ti1 N1A C7A C13A 1.1(2) . . . . no N1A C7A C8A C9A -176.5(3) . . . . no C13A C7A C8A C9A 5.2(4) . . . . no C7A C8A C9A C10A 1.7(5) . . . . no C8A C9A C10A C11A -4.5(6) . . . . no C9A C10A C11A C12A -0.2(6) . . . . no C10A C11A C12A C13A 3.9(5) . . . . no Ti1 O1A C13A C12A -174.57(17) . . . . no Ti1 O1A C13A C7A 3.8(3) . . . . no C11A C12A C13A O1A 178.5(3) . . . . no C11A C12A C13A C7A 0.3(4) . . . . no N1A C7A C13A O1A -2.9(3) . . . . no C8A C7A C13A O1A 175.6(2) . . . . no N1A C7A C13A C12A 175.3(2) . . . . no C8A C7A C13A C12A -6.2(4) . . . . no C6A C5A C14A C15A -127.1(3) . . . . no C4A C5A C14A C15A 52.3(4) . . . . no C6A C5A C14A C16A 108.2(3) . . . . no C4A C5A C14A C16A -72.4(3) . . . . no C2A C1A C17A C19A 67.6(3) . . . . no C6A C1A C17A C19A -112.7(3) . . . . no C2A C1A C17A C18A -57.5(3) . . . . no C6A C1A C17A C18A 122.2(3) . . . . no C6B C1B C2B C3B 1.2(4) . . . . no C17B C1B C2B C3B -177.5(2) . . . . no C1B C2B C3B C4B -0.6(4) . . . . no C2B C3B C4B C5B 0.1(4) . . . . no C3B C4B C5B C6B -0.2(4) . . . . no C3B C4B C5B C14B 179.6(3) . . . . no C4B C5B C6B C1B 0.8(3) . . . . no C14B C5B C6B C1B -179.0(2) . . . . no C4B C5B C6B N1B -178.5(2) . . . . no C14B C5B C6B N1B 1.7(3) . . . . no C2B C1B C6B C5B -1.3(3) . . . . no C17B C1B C6B C5B 177.3(2) . . . . no C2B C1B C6B N1B 178.0(2) . . . . no C17B C1B C6B N1B -3.4(3) . . . . no C7B N1B C6B C5B -79.9(3) . . . . no Ti1 N1B C6B C5B 93.4(3) . . . . no C7B N1B C6B C1B 100.8(3) . . . . no Ti1 N1B C6B C1B -85.9(3) . . . . no C6B N1B C7B C8B -5.6(3) . . . . no Ti1 N1B C7B C8B -179.55(17) . . . . no C6B N1B C7B C13B 174.74(17) . . . . no Ti1 N1B C7B C13B 0.7(2) . . . . no N1B C7B C8B C9B 175.0(2) . . . . no C13B C7B C8B C9B -5.3(4) . . . . no C7B C8B C9B C10B -0.7(5) . . . . no C8B C9B C10B C11B 2.6(5) . . . . no C9B C10B C11B C12B 0.5(5) . . . . no C10B C11B C12B C13B -1.0(5) . . . . no Ti1 O1B C13B C12B 167.83(16) . . . . no Ti1 O1B C13B C7B -9.7(3) . . . . no C11B C12B C13B O1B 178.6(3) . . . . no C11B C12B C13B C7B -4.2(4) . . . . no N1B C7B C13B O1B 5.0(3) . . . . no C8B C7B C13B O1B -174.7(2) . . . . no N1B C7B C13B C12B -172.2(2) . . . . no C8B C7B C13B C12B 8.1(4) . . . . no C4B C5B C14B C16B 62.3(3) . . . . no C6B C5B C14B C16B -117.8(3) . . . . no C4B C5B C14B C15B -62.5(4) . . . . no C6B C5B C14B C15B 117.3(3) . . . . no C2B C1B C17B C18B 63.7(3) . . . . no C6B C1B C17B C18B -115.0(3) . . . . no C2B C1B C17B C19B -59.3(3) . . . . no C6B C1B C17B C19B 122.1(3) . . . . no _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.328 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.066 data_tropIV _database_code_depnum_ccdc_archive 'CCDC 252932' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C26 H10 Cl2 F10 N2 O2 Ti1, C1 H2 Cl2' _chemical_formula_sum 'C27 H12 Cl4 F10 N2 O2 Ti1' _chemical_formula_weight 776.09 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2581(14) _cell_length_b 11.123(2) _cell_length_c 14.331(3) _cell_angle_alpha 100.44(3) _cell_angle_beta 90.921(19) _cell_angle_gamma 112.63(3) _cell_volume 1477.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 46 _cell_measurement_theta_min 7.17 _cell_measurement_theta_max 18.36 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.744 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 0.746 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8073 _exptl_absorpt_correction_T_max 0.9292 _exptl_absorpt_process_details ; SADABS (Bruker 2000) ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle difractometer' _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method ; CCD rotation thick slices ; _diffrn_detector_area_resol_mean 9 _diffrn_detector 'CCD plate' _diffrn_detector_type ; Bruker-Nonius 95mm CCD camera on |k-goniostat ; _diffrn_reflns_number 15418 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.1014 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 27.51 _reflns_number_total 6678 _reflns_number_gt 3248 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement ; Dirax/lsq (Duisenberg & Schreurs, 1999-2000) ; _computing_data_reduction ; EvalCCD (Duisenberg & Schreurs, 1990-2000) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The CH2CL2 solvent molecule is disordered on three positions obtained by rotation around C1S-CL2S bond. It was refined anisotropically without constrains with an occupancy factor 0.3333 for CL2S, CL3S and CL4S. ; _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^)+(0.0509P)^2^+0.7301P] 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_number_reflns 6678 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1441 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1394 _refine_ls_wR_factor_gt 0.1025 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _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 0.32423(7) 0.10917(6) 0.77683(5) 0.0417(2) Uani 1 1 d . . . Cl1 Cl 0.26213(12) 0.28967(10) 0.81050(8) 0.0630(3) Uani 1 1 d . . . Cl2 Cl 0.19514(13) 0.02528(12) 0.89722(8) 0.0718(4) Uani 1 1 d . . . F1A F 0.3158(2) 0.3803(2) 0.61534(18) 0.0642(7) Uani 1 1 d . . . F2A F 0.5237(3) 0.6151(2) 0.6157(2) 0.0897(9) Uani 1 1 d . . . F3A F 0.7973(3) 0.6395(3) 0.6200(2) 0.1124(11) Uani 1 1 d . . . F4A F 0.8587(2) 0.4255(3) 0.6246(2) 0.1062(11) Uani 1 1 d . . . F5A F 0.6489(2) 0.1886(3) 0.63036(17) 0.0696(7) Uani 1 1 d . . . F1B F 0.3610(2) -0.1515(2) 0.93933(15) 0.0603(6) Uani 1 1 d . . . F2B F 0.1851(3) -0.4102(2) 0.91348(16) 0.0678(7) Uani 1 1 d . . . F3B F 0.0875(2) -0.5551(2) 0.73666(18) 0.0662(7) Uani 1 1 d . . . F4B F 0.1718(2) -0.4435(2) 0.58260(16) 0.0645(7) Uani 1 1 d . . . F5B F 0.3493(2) -0.1863(2) 0.60692(14) 0.0553(6) Uani 1 1 d . . . O1A O 0.1822(2) -0.0307(2) 0.68573(19) 0.0450(6) Uani 1 1 d . . . O1B O 0.5195(3) 0.2230(2) 0.82168(17) 0.0463(6) Uani 1 1 d . . . N1A N 0.3700(3) 0.1579(3) 0.6411(2) 0.0363(7) Uani 1 1 d . . . N1B N 0.4292(3) -0.0195(3) 0.7864(2) 0.0383(7) Uani 1 1 d . . . C1A C 0.4499(4) 0.3891(4) 0.6224(3) 0.0439(9) Uani 1 1 d . . . C2A C 0.5557(5) 0.5100(4) 0.6205(3) 0.0568(11) Uani 1 1 d . . . C3A C 0.6926(5) 0.5222(5) 0.6221(3) 0.0651(13) Uani 1 1 d . . . C4A C 0.7242(4) 0.4154(5) 0.6248(3) 0.0626(13) Uani 1 1 d . . . C5A C 0.6174(4) 0.2949(4) 0.6285(3) 0.0479(10) Uani 1 1 d . . . C6A C 0.4776(3) 0.2795(3) 0.6290(2) 0.0367(9) Uani 1 1 d . . . C7A C 0.2807(3) 0.0773(3) 0.5654(3) 0.0339(8) Uani 1 1 d . . . C8A C 0.2900(4) 0.1010(4) 0.4720(3) 0.0481(10) Uani 1 1 d . . . H8A H 0.3659 0.1776 0.4650 0.048 Uiso 1 1 calc R . . C9A C 0.2053(5) 0.0296(5) 0.3900(3) 0.0609(12) Uani 1 1 d . . . H9A H 0.2293 0.0674 0.3367 0.061 Uiso 1 1 calc R . . C10A C 0.0886(5) -0.0912(5) 0.3742(3) 0.0702(14) Uani 1 1 d . . . H10A H 0.0459 -0.1237 0.3121 0.070 Uiso 1 1 calc R . . C11A C 0.0291(4) -0.1680(5) 0.4391(4) 0.0675(14) Uani 1 1 d . . . H11A H -0.0469 -0.2479 0.4147 0.067 Uiso 1 1 calc R . . C12A C 0.0661(4) -0.1434(4) 0.5354(3) 0.0561(11) Uani 1 1 d . . . H12A H 0.0106 -0.2091 0.5667 0.056 Uiso 1 1 calc R . . C13A C 0.1726(4) -0.0365(4) 0.5930(3) 0.0420(9) Uani 1 1 d . . . C1B C 0.3120(4) -0.2214(4) 0.8505(3) 0.0428(9) Uani 1 1 d . . . C2B C 0.2243(4) -0.3530(4) 0.8382(3) 0.0459(10) Uani 1 1 d . . . C3B C 0.1751(4) -0.4273(4) 0.7477(3) 0.0460(10) Uani 1 1 d . . . C4B C 0.2170(4) -0.3707(4) 0.6710(3) 0.0441(10) Uani 1 1 d . . . C5B C 0.3067(4) -0.2394(4) 0.6840(2) 0.0401(9) Uani 1 1 d . . . C6B C 0.3533(4) -0.1590(3) 0.7741(3) 0.0376(9) Uani 1 1 d . . . C7B C 0.5671(4) 0.0363(4) 0.8208(2) 0.0376(9) Uani 1 1 d . . . C8B C 0.6481(4) -0.0352(4) 0.8384(3) 0.0477(10) Uani 1 1 d . . . H8B H 0.5986 -0.1270 0.8270 0.048 Uiso 1 1 calc R . . C9B C 0.7890(5) 0.0087(5) 0.8698(3) 0.0578(11) Uani 1 1 d . . . H9B H 0.8197 -0.0575 0.8780 0.058 Uiso 1 1 calc R . . C10B C 0.8924(5) 0.1372(5) 0.8911(3) 0.0631(12) Uani 1 1 d . . . H10B H 0.9828 0.1454 0.9108 0.063 Uiso 1 1 calc R . . C11B C 0.8779(4) 0.2521(5) 0.8869(3) 0.0643(12) Uani 1 1 d . . . H11B H 0.9607 0.3287 0.9022 0.064 Uiso 1 1 calc R . . C12B C 0.7575(4) 0.2717(4) 0.8629(3) 0.0557(11) Uani 1 1 d . . . H12B H 0.7712 0.3598 0.8648 0.056 Uiso 1 1 calc R . . C13B C 0.6189(4) 0.1794(4) 0.8365(2) 0.0429(9) Uani 1 1 d . . . Cl1A Cl 0.561(3) 0.6301(18) 0.873(2) 0.128(7) Uani 0.3333 1 d P A 1 Cl2A Cl 0.8363(2) 0.6517(2) 0.87914(16) 0.1559(8) Uani 1 1 d . A 1 C1S C 0.6792(11) 0.6039(10) 0.9342(6) 0.186(4) Uani 1 1 d . A 1 H1S1 H 0.6458 0.5104 0.9369 0.186 Uiso 1 1 calc R A 1 H1S2 H 0.6954 0.6550 0.9989 0.186 Uiso 1 1 calc R A 1 Cl3A Cl 0.555(2) 0.5861(14) 0.8710(14) 0.120(5) Uani 0.3333 1 d P B 2 Cl4A Cl 0.5380(13) 0.6534(13) 0.9280(9) 0.114(3) Uani 0.3333 1 d P C 3 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 0.0476(4) 0.0361(4) 0.0450(4) 0.0138(3) 0.0102(3) 0.0178(3) Cl1 0.0864(8) 0.0551(7) 0.0650(7) 0.0173(5) 0.0212(6) 0.0441(6) Cl2 0.0901(8) 0.0828(9) 0.0712(8) 0.0441(6) 0.0438(7) 0.0511(7) F1A 0.0490(13) 0.0607(15) 0.1016(19) 0.0419(14) 0.0204(13) 0.0301(12) F2A 0.115(2) 0.0420(15) 0.116(2) 0.0399(15) 0.0357(18) 0.0244(15) F3A 0.0787(19) 0.083(2) 0.125(3) 0.0435(18) 0.0110(18) -0.0329(16) F4A 0.0321(14) 0.164(3) 0.123(2) 0.071(2) 0.0148(15) 0.0198(16) F5A 0.0624(15) 0.096(2) 0.0786(17) 0.0397(15) 0.0251(13) 0.0512(15) F1B 0.0877(17) 0.0459(14) 0.0384(13) 0.0093(11) 0.0020(12) 0.0167(12) F2B 0.0885(17) 0.0501(15) 0.0618(16) 0.0280(12) 0.0153(13) 0.0164(13) F3B 0.0614(14) 0.0383(14) 0.0873(18) 0.0103(12) -0.0116(13) 0.0092(12) F4B 0.0829(16) 0.0555(15) 0.0505(15) -0.0069(12) -0.0121(12) 0.0309(13) F5B 0.0763(15) 0.0596(15) 0.0414(12) 0.0173(11) 0.0153(11) 0.0357(13) O1A 0.0404(14) 0.0368(15) 0.0550(18) 0.0186(12) 0.0091(13) 0.0081(12) O1B 0.0531(16) 0.0336(15) 0.0501(16) 0.0099(12) -0.0019(13) 0.0144(13) N1A 0.0347(16) 0.0277(17) 0.0434(18) 0.0084(14) 0.0042(14) 0.0085(14) N1B 0.0408(18) 0.0336(18) 0.0406(18) 0.0109(14) 0.0050(14) 0.0132(15) C1A 0.037(2) 0.043(2) 0.053(2) 0.0180(19) 0.0106(18) 0.0142(19) C2A 0.065(3) 0.037(3) 0.065(3) 0.021(2) 0.016(2) 0.011(2) C3A 0.053(3) 0.052(3) 0.067(3) 0.026(2) 0.008(2) -0.012(2) C4A 0.027(2) 0.093(4) 0.061(3) 0.034(3) 0.007(2) 0.007(2) C5A 0.046(2) 0.060(3) 0.046(2) 0.021(2) 0.0085(19) 0.025(2) C6A 0.033(2) 0.037(2) 0.036(2) 0.0086(17) 0.0026(16) 0.0092(17) C7A 0.0289(18) 0.029(2) 0.047(2) 0.0074(17) 0.0069(17) 0.0151(16) C8A 0.053(2) 0.046(2) 0.044(2) 0.009(2) 0.011(2) 0.017(2) C9A 0.067(3) 0.075(3) 0.040(3) 0.001(2) 0.004(2) 0.031(3) C10A 0.060(3) 0.083(4) 0.058(3) -0.025(3) -0.011(3) 0.036(3) C11A 0.040(3) 0.060(3) 0.081(4) -0.024(3) -0.009(3) 0.014(2) C12A 0.037(2) 0.043(3) 0.076(3) 0.001(2) 0.002(2) 0.0073(19) C13A 0.035(2) 0.036(2) 0.056(3) 0.0088(19) 0.0059(19) 0.0159(18) C1B 0.054(2) 0.040(2) 0.036(2) 0.0106(18) 0.0051(19) 0.019(2) C2B 0.055(2) 0.035(2) 0.050(3) 0.019(2) 0.010(2) 0.016(2) C3B 0.043(2) 0.031(2) 0.063(3) 0.011(2) 0.000(2) 0.0142(19) C4B 0.050(2) 0.040(2) 0.042(2) -0.004(2) -0.0045(19) 0.023(2) C5B 0.053(2) 0.043(2) 0.033(2) 0.0120(18) 0.0078(18) 0.026(2) C6B 0.041(2) 0.033(2) 0.045(2) 0.0096(18) 0.0046(17) 0.0197(17) C7B 0.046(2) 0.040(2) 0.029(2) 0.0133(17) 0.0112(17) 0.0167(19) C8B 0.053(2) 0.045(2) 0.048(2) 0.0126(19) 0.006(2) 0.021(2) C9B 0.062(3) 0.078(3) 0.048(3) 0.021(2) 0.007(2) 0.039(3) C10B 0.047(3) 0.084(4) 0.057(3) 0.018(3) 0.001(2) 0.024(3) C11B 0.045(3) 0.071(3) 0.062(3) 0.017(2) 0.000(2) 0.006(2) C12B 0.057(3) 0.043(3) 0.053(3) 0.011(2) 0.003(2) 0.006(2) C13B 0.051(2) 0.044(2) 0.033(2) 0.0092(18) 0.0030(18) 0.017(2) Cl1A 0.132(12) 0.054(8) 0.189(15) 0.006(10) -0.032(10) 0.037(8) Cl2A 0.1730(19) 0.1255(16) 0.1571(18) -0.0014(14) -0.0113(16) 0.0601(14) C1S 0.280(12) 0.270(12) 0.106(6) 0.050(7) 0.051(8) 0.208(10) Cl3A 0.112(7) 0.097(11) 0.098(6) 0.001(8) -0.013(5) -0.005(8) Cl4A 0.114(5) 0.069(6) 0.167(11) 0.017(6) -0.022(6) 0.048(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O1A 1.925(3) . no Ti1 O1B 1.934(3) . no Ti1 N1B 2.116(3) . no Ti1 N1A 2.125(3) . no Ti1 Cl2 2.3037(14) . no Ti1 Cl1 2.3049(12) . no F1A C1A 1.342(4) . no F2A C2A 1.343(5) . no F3A C3A 1.340(4) . no F4A C4A 1.341(4) . no F5A C5A 1.344(4) . no F1B C1B 1.341(4) . no F2B C2B 1.340(4) . no F3B C3B 1.336(4) . no F4B C4B 1.340(4) . no F5B C5B 1.347(4) . no O1A C13A 1.319(4) . no O1B C13B 1.316(4) . no N1A C7A 1.343(4) . no N1A C6A 1.421(4) . no N1B C7B 1.350(4) . no N1B C6B 1.419(4) . no C1A C2A 1.370(5) . no C1A C6A 1.373(5) . no C2A C3A 1.357(6) . no C3A C4A 1.354(6) . no C4A C5A 1.378(6) . no C5A C6A 1.378(5) . no C7A C8A 1.409(5) . no C7A C13A 1.450(5) . no C8A C9A 1.365(5) . no C8A H8A 0.9300 . no C9A C10A 1.390(6) . no C9A H9A 0.9300 . no C10A C11A 1.368(7) . no C10A H10A 0.9300 . no C11A C12A 1.375(6) . no C11A H11A 0.9300 . no C12A C13A 1.380(5) . no C12A H12A 0.9300 . no C1B C2B 1.367(5) . no C1B C6B 1.387(5) . no C2B C3B 1.375(5) . no C3B C4B 1.359(5) . no C4B C5B 1.370(5) . no C5B C6B 1.388(5) . no C7B C8B 1.400(5) . no C7B C13B 1.443(5) . no C8B C9B 1.373(5) . no C8B H8B 0.9300 . no C9B C10B 1.387(6) . no C9B H9B 0.9300 . no C10B C11B 1.354(6) . no C10B H10B 0.9300 . no C11B C12B 1.382(6) . no C11B H11B 0.9300 . no C12B C13B 1.392(5) . no C12B H12B 0.9300 . no Cl1A C1S 1.63(3) . no Cl2A C1S 1.743(9) . no C1S H1S1 0.9700 . no C1S H1S2 0.9700 . no 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 O1A Ti1 O1B 151.79(11) . . no O1A Ti1 N1B 89.35(11) . . no O1B Ti1 N1B 73.96(11) . . no O1A Ti1 N1A 73.80(11) . . no O1B Ti1 N1A 87.61(11) . . no N1B Ti1 N1A 102.69(11) . . no O1A Ti1 Cl2 88.82(9) . . no O1B Ti1 Cl2 112.29(9) . . no N1B Ti1 Cl2 87.09(8) . . no N1A Ti1 Cl2 159.75(9) . . no O1A Ti1 Cl1 109.36(8) . . no O1B Ti1 Cl1 90.19(9) . . no N1B Ti1 Cl1 160.84(9) . . no N1A Ti1 Cl1 86.99(8) . . no Cl2 Ti1 Cl1 89.15(5) . . no C13A O1A Ti1 125.1(2) . . no C13B O1B Ti1 124.3(2) . . no C7A N1A C6A 118.9(3) . . no C7A N1A Ti1 117.5(2) . . no C6A N1A Ti1 123.0(2) . . no C7B N1B C6B 119.8(3) . . no C7B N1B Ti1 117.7(2) . . no C6B N1B Ti1 121.6(2) . . no F1A C1A C2A 117.4(4) . . no F1A C1A C6A 120.4(3) . . no C2A C1A C6A 122.2(4) . . no F2A C2A C3A 120.3(4) . . no F2A C2A C1A 120.1(4) . . no C3A C2A C1A 119.6(4) . . no F3A C3A C4A 119.4(4) . . no F3A C3A C2A 120.4(5) . . no C4A C3A C2A 120.2(4) . . no F4A C4A C3A 120.8(4) . . no F4A C4A C5A 119.4(5) . . no C3A C4A C5A 119.8(4) . . no F5A C5A C4A 119.8(4) . . no F5A C5A C6A 118.7(3) . . no C4A C5A C6A 121.5(4) . . no C1A C6A C5A 116.6(3) . . no C1A C6A N1A 122.4(3) . . no C5A C6A N1A 120.9(3) . . no N1A C7A C8A 124.5(3) . . no N1A C7A C13A 110.9(3) . . no C8A C7A C13A 124.6(3) . . no C9A C8A C7A 130.3(4) . . no C9A C8A H8A 114.8 . . no C7A C8A H8A 114.8 . . no C8A C9A C10A 129.8(5) . . no C8A C9A H9A 115.1 . . no C10A C9A H9A 115.1 . . no C11A C10A C9A 127.8(4) . . no C11A C10A H10A 116.1 . . no C9A C10A H10A 116.1 . . no C10A C11A C12A 128.9(4) . . no C10A C11A H11A 115.5 . . no C12A C11A H11A 115.5 . . no C11A C12A C13A 130.1(4) . . no C11A C12A H12A 114.9 . . no C13A C12A H12A 114.9 . . no O1A C13A C12A 119.2(4) . . no O1A C13A C7A 112.5(3) . . no C12A C13A C7A 128.3(4) . . no F1B C1B C2B 118.7(3) . . no F1B C1B C6B 119.2(3) . . no C2B C1B C6B 122.1(3) . . no F2B C2B C1B 120.8(3) . . no F2B C2B C3B 119.6(3) . . no C1B C2B C3B 119.7(4) . . no F3B C3B C4B 121.0(4) . . no F3B C3B C2B 119.1(4) . . no C4B C3B C2B 119.9(3) . . no F4B C4B C3B 120.1(4) . . no F4B C4B C5B 119.9(4) . . no C3B C4B C5B 120.0(3) . . no F5B C5B C4B 118.9(3) . . no F5B C5B C6B 119.1(3) . . no C4B C5B C6B 122.0(4) . . no C1B C6B C5B 116.2(3) . . no C1B C6B N1B 122.3(3) . . no C5B C6B N1B 121.3(3) . . no N1B C7B C8B 124.6(3) . . no N1B C7B C13B 110.4(3) . . no C8B C7B C13B 125.0(3) . . no C9B C8B C7B 130.3(4) . . no C9B C8B H8B 114.9 . . no C7B C8B H8B 114.9 . . no C8B C9B C10B 129.7(4) . . no C8B C9B H9B 115.2 . . no C10B C9B H9B 115.2 . . no C11B C10B C9B 128.0(4) . . no C11B C10B H10B 116.0 . . no C9B C10B H10B 116.0 . . no C10B C11B C12B 129.2(4) . . no C10B C11B H11B 115.4 . . no C12B C11B H11B 115.4 . . no C11B C12B C13B 129.7(4) . . no C11B C12B H12B 115.2 . . no C13B C12B H12B 115.2 . . no O1B C13B C12B 118.7(4) . . no O1B C13B C7B 113.4(3) . . no C12B C13B C7B 127.9(4) . . no Cl1A C1S Cl2A 108.6(13) . . no Cl1A C1S H1S1 110.0 . . no Cl2A C1S H1S1 110.0 . . no Cl1A C1S H1S2 110.0 . . no Cl2A C1S H1S2 110.0 . . no H1S1 C1S H1S2 108.4 . . no 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 O1B Ti1 O1A C13A -51.5(4) . . . . no N1B Ti1 O1A C13A -104.2(3) . . . . no N1A Ti1 O1A C13A -0.8(3) . . . . no Cl2 Ti1 O1A C13A 168.7(3) . . . . no Cl1 Ti1 O1A C13A 80.0(3) . . . . no O1A Ti1 O1B C13B -55.7(4) . . . . no N1B Ti1 O1B C13B 0.2(3) . . . . no N1A Ti1 O1B C13B -103.8(3) . . . . no Cl2 Ti1 O1B C13B 80.1(3) . . . . no Cl1 Ti1 O1B C13B 169.3(3) . . . . no O1A Ti1 N1A C7A 3.0(2) . . . . no O1B Ti1 N1A C7A 161.5(2) . . . . no N1B Ti1 N1A C7A 88.5(2) . . . . no Cl2 Ti1 N1A C7A -28.9(4) . . . . no Cl1 Ti1 N1A C7A -108.2(2) . . . . no O1A Ti1 N1A C6A 174.1(3) . . . . no O1B Ti1 N1A C6A -27.4(3) . . . . no N1B Ti1 N1A C6A -100.4(3) . . . . no Cl2 Ti1 N1A C6A 142.2(2) . . . . no Cl1 Ti1 N1A C6A 62.9(2) . . . . no O1A Ti1 N1B C7B 160.0(2) . . . . no O1B Ti1 N1B C7B 3.1(2) . . . . no N1A Ti1 N1B C7B 86.8(2) . . . . no Cl2 Ti1 N1B C7B -111.1(2) . . . . no Cl1 Ti1 N1B C7B -32.2(4) . . . . no O1A Ti1 N1B C6B -31.3(3) . . . . no O1B Ti1 N1B C6B 171.8(3) . . . . no N1A Ti1 N1B C6B -104.5(3) . . . . no Cl2 Ti1 N1B C6B 57.6(2) . . . . no Cl1 Ti1 N1B C6B 136.6(3) . . . . no F1A C1A C2A F2A 2.6(6) . . . . no C6A C1A C2A F2A -178.8(4) . . . . no F1A C1A C2A C3A -176.4(4) . . . . no C6A C1A C2A C3A 2.2(6) . . . . no F2A C2A C3A F3A 0.8(7) . . . . no C1A C2A C3A F3A 179.8(4) . . . . no F2A C2A C3A C4A -178.5(4) . . . . no C1A C2A C3A C4A 0.4(7) . . . . no F3A C3A C4A F4A -0.5(7) . . . . no C2A C3A C4A F4A 178.8(4) . . . . no F3A C3A C4A C5A 178.9(4) . . . . no C2A C3A C4A C5A -1.8(7) . . . . no F4A C4A C5A F5A -1.1(6) . . . . no C3A C4A C5A F5A 179.4(4) . . . . no F4A C4A C5A C6A 179.9(4) . . . . no C3A C4A C5A C6A 0.5(7) . . . . no F1A C1A C6A C5A 175.2(3) . . . . no C2A C1A C6A C5A -3.4(6) . . . . no F1A C1A C6A N1A -8.3(6) . . . . no C2A C1A C6A N1A 173.1(4) . . . . no F5A C5A C6A C1A -176.9(3) . . . . no C4A C5A C6A C1A 2.1(6) . . . . no F5A C5A C6A N1A 6.5(5) . . . . no C4A C5A C6A N1A -174.6(4) . . . . no C7A N1A C6A C1A 77.3(4) . . . . no Ti1 N1A C6A C1A -93.6(4) . . . . no C7A N1A C6A C5A -106.2(4) . . . . no Ti1 N1A C6A C5A 82.8(4) . . . . no C6A N1A C7A C8A 3.6(5) . . . . no Ti1 N1A C7A C8A 175.1(3) . . . . no C6A N1A C7A C13A -175.9(3) . . . . no Ti1 N1A C7A C13A -4.4(3) . . . . no N1A C7A C8A C9A -178.5(4) . . . . no C13A C7A C8A C9A 0.9(6) . . . . no C7A C8A C9A C10A -3.4(7) . . . . no C8A C9A C10A C11A 0.7(8) . . . . no C9A C10A C11A C12A 2.4(8) . . . . no C10A C11A C12A C13A -0.5(8) . . . . no Ti1 O1A C13A C12A 179.3(2) . . . . no Ti1 O1A C13A C7A -1.3(4) . . . . no C11A C12A C13A O1A 175.6(4) . . . . no C11A C12A C13A C7A -3.6(7) . . . . no N1A C7A C13A O1A 3.6(4) . . . . no C8A C7A C13A O1A -175.8(3) . . . . no N1A C7A C13A C12A -177.1(3) . . . . no C8A C7A C13A C12A 3.5(6) . . . . no F1B C1B C2B F2B 1.8(5) . . . . no C6B C1B C2B F2B -179.3(3) . . . . no F1B C1B C2B C3B -178.7(3) . . . . no C6B C1B C2B C3B 0.2(6) . . . . no F2B C2B C3B F3B 0.7(5) . . . . no C1B C2B C3B F3B -178.8(3) . . . . no F2B C2B C3B C4B -178.5(3) . . . . no C1B C2B C3B C4B 1.9(6) . . . . no F3B C3B C4B F4B -0.7(5) . . . . no C2B C3B C4B F4B 178.5(3) . . . . no F3B C3B C4B C5B 179.9(3) . . . . no C2B C3B C4B C5B -0.9(6) . . . . no F4B C4B C5B F5B -0.8(5) . . . . no C3B C4B C5B F5B 178.5(3) . . . . no F4B C4B C5B C6B 178.2(3) . . . . no C3B C4B C5B C6B -2.4(6) . . . . no F1B C1B C6B C5B 175.6(3) . . . . no C2B C1B C6B C5B -3.3(5) . . . . no F1B C1B C6B N1B -9.2(5) . . . . no C2B C1B C6B N1B 171.9(3) . . . . no F5B C5B C6B C1B -176.6(3) . . . . no C4B C5B C6B C1B 4.4(5) . . . . no F5B C5B C6B N1B 8.2(5) . . . . no C4B C5B C6B N1B -170.8(3) . . . . no C7B N1B C6B C1B 73.0(4) . . . . no Ti1 N1B C6B C1B -95.5(4) . . . . no C7B N1B C6B C5B -112.2(4) . . . . no Ti1 N1B C6B C5B 79.4(4) . . . . no C6B N1B C7B C8B 5.9(5) . . . . no Ti1 N1B C7B C8B 174.8(3) . . . . no C6B N1B C7B C13B -174.2(3) . . . . no Ti1 N1B C7B C13B -5.3(3) . . . . no N1B C7B C8B C9B 177.5(3) . . . . no C13B C7B C8B C9B -2.4(6) . . . . no C7B C8B C9B C10B -1.6(7) . . . . no C8B C9B C10B C11B 0.8(8) . . . . no C9B C10B C11B C12B 1.9(8) . . . . no C10B C11B C12B C13B -0.2(8) . . . . no Ti1 O1B C13B C12B 175.9(2) . . . . no Ti1 O1B C13B C7B -3.1(4) . . . . no C11B C12B C13B O1B 176.4(4) . . . . no C11B C12B C13B C7B -4.8(7) . . . . no N1B C7B C13B O1B 5.2(4) . . . . no C8B C7B C13B O1B -174.9(3) . . . . no N1B C7B C13B C12B -173.6(3) . . . . no C8B C7B C13B C12B 6.3(6) . . . . no _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.358 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.066