# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'David S.McGuinness' _publ_contact_author_email David.McGuinness@utas.edu.au loop_ _publ_author_name 'James Suttil' 'David S.McGuinness' 'Markus Pichler' 'Michael Gardiner' 'David Morgan' 'Stephen Evans' data_d:\as8f1\new\new _database_code_depnum_ccdc_archive 'CCDC 844799' #TrackingRef '- compound 12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H18 Cl2 O4 Ti' _chemical_formula_sum 'C24 H18 Cl2 O4 Ti' _chemical_formula_weight 489.18 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 14.144(3) _cell_length_b 16.3860(17) _cell_length_c 19.049(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4414.9(11) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 37972 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 26.23 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 0.658 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Data completeness is low owing to the single axis rotation goniometer available at the Australian Synchrotron. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77488 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Synchrotron ID' _diffrn_radiation_monochromator Si<111> _diffrn_measurement_device_type '3-ID1 Australian Synchrotron' _diffrn_measurement_method Rotation _diffrn_detector_area_resol_mean 'ADSC Q315' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43808 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0192 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 26.23 _reflns_number_total 3402 _reflns_number_gt 3201 _reflns_threshold_expression >2sigma(I) _computing_data_collection BLU-ICE _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; 'X-SEED (Barbour, 2008) and ORTEPIII (Farrugia, 1998)' ; _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0449P)^2^+4.0709P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3402 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0849 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 0.94579(2) 0.17325(2) 0.359148(18) 0.02074(13) Uani 1 1 d . . . Cl1 Cl 0.80446(4) 0.23506(3) 0.35409(3) 0.03141(15) Uani 1 1 d . . . Cl2 Cl 0.90772(4) 0.06210(3) 0.42280(3) 0.02743(15) Uani 1 1 d . . . O1 O 1.00549(10) 0.23027(8) 0.43128(7) 0.0228(3) Uani 1 1 d . . . O2 O 1.01262(10) 0.28212(8) 0.30763(7) 0.0242(3) Uani 1 1 d . . . O3 O 0.94680(9) 0.12929(8) 0.26912(7) 0.0241(3) Uani 1 1 d . . . O4 O 1.09653(9) 0.12588(8) 0.34030(7) 0.0230(3) Uani 1 1 d . . . C1 C 1.06224(14) 0.29647(12) 0.42259(10) 0.0217(4) Uani 1 1 d . . . C2 C 1.06739(14) 0.32841(12) 0.35505(11) 0.0227(5) Uani 1 1 d . . . C3 C 1.12083(15) 0.39609(13) 0.33842(11) 0.0266(5) Uani 1 1 d . . . H3 H 1.1230 0.4170 0.2919 0.032 Uiso 1 1 calc R . . C4 C 1.17170(15) 0.43254(13) 0.39294(12) 0.0285(5) Uani 1 1 d . . . H4 H 1.2088 0.4796 0.3836 0.034 Uiso 1 1 calc R . . C5 C 1.16881(15) 0.40088(13) 0.46057(12) 0.0295(5) Uani 1 1 d . . . H5 H 1.2048 0.4260 0.4967 0.035 Uiso 1 1 calc R . . C6 C 1.11388(15) 0.33283(13) 0.47601(11) 0.0275(5) Uani 1 1 d . . . H6 H 1.1118 0.3116 0.5224 0.033 Uiso 1 1 calc R . . C7 C 1.00452(15) 0.31198(12) 0.23769(10) 0.0227(4) Uani 1 1 d . . . C8 C 0.92841(16) 0.36044(13) 0.22092(12) 0.0293(5) Uani 1 1 d . . . H8 H 0.8819 0.3740 0.2550 0.035 Uiso 1 1 calc R . . C9 C 0.92190(18) 0.38911(15) 0.15189(12) 0.0347(5) Uani 1 1 d . . . H9 H 0.8700 0.4224 0.1384 0.042 Uiso 1 1 calc R . . C10 C 0.99062(17) 0.36916(13) 0.10318(11) 0.0337(5) Uani 1 1 d . . . H10 H 0.9854 0.3885 0.0563 0.040 Uiso 1 1 calc R . . C11 C 1.06695(17) 0.32123(13) 0.12215(12) 0.0322(5) Uani 1 1 d . . . H11 H 1.1143 0.3084 0.0885 0.039 Uiso 1 1 calc R . . C12 C 1.07442(15) 0.29181(13) 0.19028(11) 0.0281(5) Uani 1 1 d . . . H12 H 1.1264 0.2586 0.2039 0.034 Uiso 1 1 calc R . . C13 C 1.02245(15) 0.09599(12) 0.23549(10) 0.0231(4) Uani 1 1 d . . . C14 C 1.10718(15) 0.09259(12) 0.27271(10) 0.0231(4) Uani 1 1 d . . . C15 C 1.18852(15) 0.05905(12) 0.24476(11) 0.0268(5) Uani 1 1 d . . . H15 H 1.2458 0.0576 0.2707 0.032 Uiso 1 1 calc R . . C16 C 1.18312(16) 0.02730(13) 0.17664(12) 0.0317(5) Uani 1 1 d . . . H16 H 1.2376 0.0034 0.1560 0.038 Uiso 1 1 calc R . . C17 C 1.09926(17) 0.03019(14) 0.13884(11) 0.0322(5) Uani 1 1 d . . . H17 H 1.0970 0.0081 0.0928 0.039 Uiso 1 1 calc R . . C18 C 1.01842(16) 0.06506(12) 0.16771(11) 0.0277(5) Uani 1 1 d . . . H18 H 0.9614 0.0677 0.1415 0.033 Uiso 1 1 calc R . . C19 C 1.17699(14) 0.13455(12) 0.38456(10) 0.0215(4) Uani 1 1 d . . . C20 C 1.17256(14) 0.09707(12) 0.44943(10) 0.0235(4) Uani 1 1 d . . . H20 H 1.1199 0.0643 0.4621 0.028 Uiso 1 1 calc R . . C21 C 1.24785(16) 0.10883(14) 0.49571(11) 0.0311(5) Uani 1 1 d . . . H21 H 1.2462 0.0845 0.5410 0.037 Uiso 1 1 calc R . . C22 C 1.32482(16) 0.15567(14) 0.47600(13) 0.0350(5) Uani 1 1 d . . . H22 H 1.3760 0.1631 0.5077 0.042 Uiso 1 1 calc R . . C23 C 1.32751(16) 0.19199(14) 0.40993(14) 0.0359(5) Uani 1 1 d . . . H23 H 1.3808 0.2237 0.3965 0.043 Uiso 1 1 calc R . . C24 C 1.25243(16) 0.18203(13) 0.36363(12) 0.0293(5) Uani 1 1 d . . . H24 H 1.2531 0.2073 0.3187 0.035 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 0.0199(2) 0.0246(2) 0.0177(2) -0.00143(14) -0.00062(14) -0.00034(14) Cl1 0.0226(3) 0.0375(3) 0.0341(3) -0.0043(2) -0.0025(2) 0.0051(2) Cl2 0.0284(3) 0.0290(3) 0.0248(3) 0.0019(2) -0.0008(2) -0.0051(2) O1 0.0238(7) 0.0262(7) 0.0183(7) -0.0011(6) 0.0009(6) -0.0012(6) O2 0.0272(7) 0.0281(7) 0.0173(7) 0.0010(6) -0.0040(6) -0.0045(6) O3 0.0234(8) 0.0276(7) 0.0213(7) -0.0019(6) -0.0016(6) 0.0000(6) O4 0.0216(7) 0.0319(8) 0.0155(7) -0.0029(6) -0.0009(5) 0.0021(6) C1 0.0213(10) 0.0217(10) 0.0222(10) -0.0028(8) 0.0008(8) 0.0022(8) C2 0.0197(10) 0.0255(11) 0.0228(11) -0.0037(8) -0.0032(8) 0.0018(8) C3 0.0274(11) 0.0274(11) 0.0250(11) 0.0025(9) -0.0002(9) 0.0006(9) C4 0.0272(11) 0.0262(11) 0.0320(12) -0.0015(9) -0.0004(9) -0.0033(9) C5 0.0306(12) 0.0303(11) 0.0277(11) -0.0065(9) -0.0039(9) -0.0031(9) C6 0.0300(11) 0.0313(11) 0.0212(11) -0.0026(9) -0.0018(9) 0.0011(9) C7 0.0293(11) 0.0233(10) 0.0155(10) 0.0012(8) -0.0025(8) -0.0034(9) C8 0.0296(12) 0.0311(11) 0.0273(11) -0.0020(9) -0.0012(9) 0.0031(9) C9 0.0384(13) 0.0329(12) 0.0328(13) 0.0059(10) -0.0119(10) 0.0015(10) C10 0.0476(14) 0.0314(12) 0.0220(11) 0.0042(9) -0.0054(10) -0.0116(10) C11 0.0434(14) 0.0282(12) 0.0249(11) -0.0007(9) 0.0087(10) -0.0075(10) C12 0.0289(11) 0.0270(11) 0.0283(12) 0.0037(9) 0.0032(9) 0.0006(9) C13 0.0281(11) 0.0205(10) 0.0207(10) 0.0023(8) 0.0010(8) -0.0036(8) C14 0.0308(11) 0.0230(10) 0.0157(10) 0.0004(8) 0.0021(8) -0.0021(8) C15 0.0270(11) 0.0270(11) 0.0265(11) 0.0019(9) 0.0045(9) 0.0005(8) C16 0.0363(12) 0.0314(12) 0.0273(12) -0.0019(9) 0.0129(10) -0.0017(10) C17 0.0440(14) 0.0320(12) 0.0207(11) -0.0045(9) 0.0057(9) -0.0073(10) C18 0.0361(12) 0.0274(11) 0.0195(10) -0.0011(8) -0.0008(9) -0.0061(9) C19 0.0206(10) 0.0235(10) 0.0205(10) -0.0040(8) -0.0032(8) 0.0037(8) C20 0.0237(10) 0.0261(10) 0.0208(10) -0.0030(8) 0.0010(8) 0.0047(8) C21 0.0329(12) 0.0378(12) 0.0226(11) -0.0058(9) -0.0047(9) 0.0111(10) C22 0.0269(12) 0.0402(13) 0.0379(13) -0.0153(11) -0.0099(10) 0.0052(10) C23 0.0264(12) 0.0304(12) 0.0509(15) -0.0085(11) 0.0011(10) -0.0032(10) C24 0.0287(12) 0.0257(11) 0.0336(12) 0.0019(9) 0.0018(9) -0.0005(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O3 1.8601(14) . ? Ti1 O1 1.8637(14) . ? Ti1 Cl1 2.2429(7) . ? Ti1 O2 2.2448(14) . ? Ti1 Cl2 2.2532(6) . ? Ti1 O4 2.2972(14) . ? O1 C1 1.360(2) . ? O2 C2 1.411(2) . ? O2 C7 1.424(2) . ? O3 C13 1.361(2) . ? O4 C14 1.406(2) . ? O4 C19 1.423(2) . ? C1 C6 1.387(3) . ? C1 C2 1.391(3) . ? C2 C3 1.379(3) . ? C3 C4 1.398(3) . ? C4 C5 1.389(3) . ? C5 C6 1.390(3) . ? C7 C8 1.375(3) . ? C7 C12 1.379(3) . ? C8 C9 1.399(3) . ? C9 C10 1.383(3) . ? C10 C11 1.383(3) . ? C11 C12 1.388(3) . ? C13 C18 1.388(3) . ? C13 C14 1.394(3) . ? C14 C15 1.382(3) . ? C15 C16 1.400(3) . ? C16 C17 1.388(3) . ? C17 C18 1.391(3) . ? C19 C24 1.379(3) . ? C19 C20 1.381(3) . ? C20 C21 1.396(3) . ? C21 C22 1.384(3) . ? C22 C23 1.393(4) . ? C23 C24 1.390(3) . ? 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 O3 Ti1 O1 150.49(6) . . ? O3 Ti1 Cl1 98.17(5) . . ? O1 Ti1 Cl1 102.07(5) . . ? O3 Ti1 O2 84.34(6) . . ? O1 Ti1 O2 74.52(5) . . ? Cl1 Ti1 O2 89.86(4) . . ? O3 Ti1 Cl2 100.66(5) . . ? O1 Ti1 Cl2 96.70(5) . . ? Cl1 Ti1 Cl2 100.09(2) . . ? O2 Ti1 Cl2 168.02(4) . . ? O3 Ti1 O4 73.62(5) . . ? O1 Ti1 O4 82.19(6) . . ? Cl1 Ti1 O4 166.66(4) . . ? O2 Ti1 O4 79.01(5) . . ? Cl2 Ti1 O4 91.88(4) . . ? C1 O1 Ti1 125.29(12) . . ? C2 O2 C7 117.28(15) . . ? C2 O2 Ti1 112.24(11) . . ? C7 O2 Ti1 130.41(11) . . ? C13 O3 Ti1 126.52(12) . . ? C14 O4 C19 119.69(15) . . ? C14 O4 Ti1 111.93(11) . . ? C19 O4 Ti1 128.01(11) . . ? O1 C1 C6 124.36(18) . . ? O1 C1 C2 116.34(17) . . ? C6 C1 C2 119.29(19) . . ? C3 C2 C1 122.95(19) . . ? C3 C2 O2 125.88(18) . . ? C1 C2 O2 111.16(17) . . ? C2 C3 C4 117.1(2) . . ? C5 C4 C3 121.0(2) . . ? C4 C5 C6 120.8(2) . . ? C1 C6 C5 118.9(2) . . ? C8 C7 C12 123.19(19) . . ? C8 C7 O2 118.60(18) . . ? C12 C7 O2 118.20(18) . . ? C7 C8 C9 117.6(2) . . ? C10 C9 C8 120.3(2) . . ? C9 C10 C11 120.5(2) . . ? C10 C11 C12 120.0(2) . . ? C7 C12 C11 118.3(2) . . ? O3 C13 C18 123.48(19) . . ? O3 C13 C14 116.91(17) . . ? C18 C13 C14 119.60(19) . . ? C15 C14 C13 122.40(19) . . ? C15 C14 O4 126.60(18) . . ? C13 C14 O4 110.99(17) . . ? C14 C15 C16 117.4(2) . . ? C17 C16 C15 121.0(2) . . ? C16 C17 C18 120.7(2) . . ? C13 C18 C17 118.9(2) . . ? C24 C19 C20 122.99(19) . . ? C24 C19 O4 120.23(18) . . ? C20 C19 O4 116.69(18) . . ? C19 C20 C21 118.0(2) . . ? C22 C21 C20 120.3(2) . . ? C21 C22 C23 120.2(2) . . ? C24 C23 C22 120.2(2) . . ? C19 C24 C23 118.3(2) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.23 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.234 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.053 # Attachment '- compound 13.cif' data_d:\as10js5 _database_code_depnum_ccdc_archive 'CCDC 844800' #TrackingRef '- compound 13.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H25 Cl3 O4 Ti' _chemical_formula_sum 'C20 H25 Cl3 O4 Ti' _chemical_formula_weight 483.65 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.713(5) _cell_length_b 12.471(5) _cell_length_c 18.199(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.988(15) _cell_angle_gamma 90.00 _cell_volume 2192.4(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 20318 _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 30.60 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 0.779 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Data completeness is low owing to the single axis rotation goniometer available at the Australian Synchrotron. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.70000 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Synchrotron ID' _diffrn_radiation_monochromator Si<111> _diffrn_measurement_device_type '3-ID1 Australian Synchrotron' _diffrn_measurement_method Rotation _diffrn_detector_area_resol_mean 'ADSC Q315' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44892 _diffrn_reflns_av_R_equivalents 0.1065 _diffrn_reflns_av_sigmaI/netI 0.0650 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 30.60 _reflns_number_total 6801 _reflns_number_gt 5004 _reflns_threshold_expression >2sigma(I) _computing_data_collection BLU-ICE _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; 'X-SEED (Barbour, 2008) and ORTEPIII (Farrugia, 1998)' ; _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.1804P)^2^+0.6882P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6801 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1102 _refine_ls_R_factor_gt 0.0860 _refine_ls_wR_factor_ref 0.2552 _refine_ls_wR_factor_gt 0.2353 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 0.91258(5) 0.26886(4) 0.12307(3) 0.02436(18) Uani 1 1 d . . . Cl1 Cl 0.90161(9) 0.27724(6) -0.00462(5) 0.0321(2) Uani 1 1 d . . . Cl2 Cl 0.78826(10) 0.42340(6) 0.13180(6) 0.0421(3) Uani 1 1 d . . . Cl3 Cl 0.96380(9) 0.25185(7) 0.25081(5) 0.0356(2) Uani 1 1 d . . . O1 O 0.7664(2) 0.17997(17) 0.12467(13) 0.0263(5) Uani 1 1 d . . . O2 O 0.6669(2) -0.01295(17) 0.09123(13) 0.0284(5) Uani 1 1 d . . . O3 O 1.0980(2) 0.36022(19) 0.12641(14) 0.0324(5) Uani 1 1 d . . . O4 O 1.0474(2) 0.13748(17) 0.11594(13) 0.0275(5) Uani 1 1 d . . . C1 C 0.6633(3) 0.1438(2) 0.16245(18) 0.0251(6) Uani 1 1 d . . . C2 C 0.6095(3) 0.0412(2) 0.14650(17) 0.0238(6) Uani 1 1 d . . . C3 C 0.5051(3) 0.0022(3) 0.18542(19) 0.0302(7) Uani 1 1 d . . . H3 H 0.4687 -0.0675 0.1754 0.036 Uiso 1 1 calc R . . C4 C 0.4536(3) 0.0655(3) 0.23933(19) 0.0321(7) Uani 1 1 d . . . H4 H 0.3824 0.0383 0.2662 0.038 Uiso 1 1 calc R . . C5 C 0.5051(3) 0.1675(3) 0.2542(2) 0.0331(7) Uani 1 1 d . . . H5 H 0.4680 0.2103 0.2906 0.040 Uiso 1 1 calc R . . C6 C 0.6105(3) 0.2076(3) 0.2163(2) 0.0306(7) Uani 1 1 d . . . H6 H 0.6464 0.2775 0.2267 0.037 Uiso 1 1 calc R . . C7 C 0.6406(3) -0.1228(2) 0.08234(17) 0.0231(6) Uani 1 1 d . . . C8 C 0.5243(3) -0.1574(3) 0.0384(2) 0.0302(7) Uani 1 1 d . . . H8 H 0.4586 -0.1073 0.0165 0.036 Uiso 1 1 calc R . . C9 C 0.5054(4) -0.2677(3) 0.0267(2) 0.0335(7) Uani 1 1 d . . . H9 H 0.4252 -0.2930 -0.0025 0.040 Uiso 1 1 calc R . . C10 C 0.6025(4) -0.3394(3) 0.0573(2) 0.0324(7) Uani 1 1 d . . . H10 H 0.5892 -0.4141 0.0491 0.039 Uiso 1 1 calc R . . C11 C 0.7204(3) -0.3028(3) 0.1003(2) 0.0296(6) Uani 1 1 d . . . H11 H 0.7881 -0.3525 0.1206 0.036 Uiso 1 1 calc R . . C12 C 0.7391(3) -0.1940(2) 0.11350(17) 0.0247(6) Uani 1 1 d . . . H12 H 0.8184 -0.1688 0.1435 0.030 Uiso 1 1 calc R . . C13 C 1.1181(4) 0.4529(3) 0.0781(3) 0.0471(10) Uani 1 1 d . . . H13A H 1.0486 0.5093 0.0845 0.057 Uiso 1 1 calc R . . H13B H 1.1093 0.4307 0.0256 0.057 Uiso 1 1 calc R . . C14 C 1.2633(4) 0.4940(3) 0.1017(3) 0.0419(9) Uani 1 1 d . . . H14A H 1.2615 0.5543 0.1370 0.050 Uiso 1 1 calc R . . H14B H 1.3095 0.5178 0.0586 0.050 Uiso 1 1 calc R . . C15 C 1.3356(4) 0.3960(3) 0.1385(2) 0.0403(8) Uani 1 1 d . . . H15A H 1.3656 0.3455 0.1014 0.048 Uiso 1 1 calc R . . H15B H 1.4167 0.4170 0.1730 0.048 Uiso 1 1 calc R . . C16 C 1.2229(4) 0.3480(3) 0.1793(2) 0.0398(8) Uani 1 1 d . . . H16A H 1.2417 0.2715 0.1910 0.048 Uiso 1 1 calc R . . H16B H 1.2132 0.3874 0.2257 0.048 Uiso 1 1 calc R . . C17 C 1.1633(5) 0.1267(3) 0.0716(3) 0.0490(11) Uani 1 1 d . . . H17A H 1.2471 0.1613 0.0968 0.059 Uiso 1 1 calc R . . H17B H 1.1411 0.1608 0.0227 0.059 Uiso 1 1 calc R . . C18 C 1.1863(4) 0.0100(3) 0.0632(2) 0.0365(8) Uani 1 1 d . . . H18A H 1.2864 -0.0056 0.0639 0.044 Uiso 1 1 calc R . . H18B H 1.1382 -0.0161 0.0159 0.044 Uiso 1 1 calc R . . C19 C 1.1281(4) -0.0428(3) 0.1276(2) 0.0408(8) Uani 1 1 d . . . H19A H 1.0815 -0.1110 0.1122 0.049 Uiso 1 1 calc R . . H19B H 1.2025 -0.0580 0.1677 0.049 Uiso 1 1 calc R . . C20 C 1.0276(5) 0.0349(3) 0.1526(2) 0.0450(10) Uani 1 1 d . . . H20A H 0.9320 0.0088 0.1396 0.054 Uiso 1 1 calc R . . H20B H 1.0431 0.0438 0.2069 0.054 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 0.0207(3) 0.0189(3) 0.0358(4) -0.00380(19) 0.0140(2) 0.00121(17) Cl1 0.0330(4) 0.0289(4) 0.0358(4) 0.0015(3) 0.0107(3) -0.0050(3) Cl2 0.0386(5) 0.0209(4) 0.0707(7) -0.0018(3) 0.0238(4) 0.0087(3) Cl3 0.0333(4) 0.0406(4) 0.0350(5) -0.0073(3) 0.0141(3) -0.0025(3) O1 0.0208(9) 0.0215(9) 0.0396(12) -0.0005(8) 0.0172(9) -0.0003(8) O2 0.0303(11) 0.0194(9) 0.0402(12) 0.0005(8) 0.0258(9) 0.0000(8) O3 0.0278(11) 0.0282(11) 0.0424(14) 0.0029(9) 0.0100(10) -0.0043(9) O4 0.0254(10) 0.0218(10) 0.0392(12) 0.0031(8) 0.0218(9) 0.0036(8) C1 0.0203(12) 0.0233(12) 0.0341(15) 0.0030(11) 0.0152(11) 0.0061(10) C2 0.0198(12) 0.0229(12) 0.0313(14) 0.0023(11) 0.0147(11) 0.0055(10) C3 0.0268(14) 0.0272(14) 0.0402(18) 0.0044(12) 0.0206(13) 0.0015(11) C4 0.0273(15) 0.0360(16) 0.0368(17) 0.0063(13) 0.0218(13) 0.0050(12) C5 0.0285(15) 0.0353(16) 0.0396(17) -0.0005(13) 0.0235(13) 0.0071(13) C6 0.0280(15) 0.0263(14) 0.0408(18) -0.0030(12) 0.0192(13) 0.0028(12) C7 0.0221(12) 0.0186(12) 0.0319(15) 0.0010(10) 0.0179(11) 0.0015(9) C8 0.0205(13) 0.0309(15) 0.0405(18) 0.0053(13) 0.0094(12) 0.0069(11) C9 0.0240(14) 0.0372(17) 0.0403(19) -0.0002(14) 0.0088(13) -0.0047(12) C10 0.0351(16) 0.0208(13) 0.0449(19) -0.0026(12) 0.0205(14) -0.0021(12) C11 0.0249(14) 0.0244(14) 0.0418(17) 0.0065(12) 0.0142(12) 0.0060(11) C12 0.0230(13) 0.0237(13) 0.0295(15) 0.0042(11) 0.0124(11) 0.0013(10) C13 0.0342(18) 0.0383(19) 0.068(3) 0.0203(19) 0.0027(18) -0.0113(15) C14 0.0360(18) 0.0324(17) 0.058(2) 0.0028(16) 0.0096(16) -0.0123(14) C15 0.0269(16) 0.044(2) 0.051(2) 0.0034(16) 0.0065(15) -0.0066(14) C16 0.0309(17) 0.045(2) 0.044(2) 0.0065(16) 0.0064(15) -0.0033(15) C17 0.051(2) 0.0263(16) 0.079(3) 0.0075(17) 0.054(2) 0.0072(15) C18 0.0357(17) 0.0355(17) 0.0421(19) 0.0051(14) 0.0225(15) 0.0124(14) C19 0.0425(19) 0.0252(15) 0.060(2) 0.0030(15) 0.0296(17) 0.0039(14) C20 0.051(2) 0.0315(17) 0.060(2) 0.0178(16) 0.0399(19) 0.0174(16) _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 1.804(2) . ? Ti1 O4 2.110(2) . ? Ti1 O3 2.127(2) . ? Ti1 Cl2 2.2886(11) . ? Ti1 Cl1 2.3174(13) . ? Ti1 Cl3 2.3357(13) . ? O1 C1 1.350(3) . ? O2 C2 1.376(3) . ? O2 C7 1.400(4) . ? O3 C16 1.475(5) . ? O3 C13 1.477(4) . ? O4 C17 1.457(4) . ? O4 C20 1.464(4) . ? C1 C6 1.400(4) . ? C1 C2 1.402(4) . ? C2 C3 1.383(4) . ? C3 C4 1.392(5) . ? C4 C5 1.384(5) . ? C5 C6 1.386(4) . ? C7 C8 1.383(5) . ? C7 C12 1.383(4) . ? C8 C9 1.401(5) . ? C9 C10 1.374(5) . ? C10 C11 1.396(5) . ? C11 C12 1.386(4) . ? C13 C14 1.520(5) . ? C14 C15 1.529(6) . ? C15 C16 1.508(5) . ? C17 C18 1.482(5) . ? C18 C19 1.506(5) . ? C19 C20 1.480(5) . ? 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 O4 91.05(10) . . ? O1 Ti1 O3 173.92(10) . . ? O4 Ti1 O3 83.61(10) . . ? O1 Ti1 Cl2 95.42(8) . . ? O4 Ti1 Cl2 173.51(7) . . ? O3 Ti1 Cl2 89.91(8) . . ? O1 Ti1 Cl1 95.16(8) . . ? O4 Ti1 Cl1 86.40(7) . . ? O3 Ti1 Cl1 87.41(8) . . ? Cl2 Ti1 Cl1 93.57(4) . . ? O1 Ti1 Cl3 90.82(8) . . ? O4 Ti1 Cl3 85.50(7) . . ? O3 Ti1 Cl3 85.89(8) . . ? Cl2 Ti1 Cl3 93.81(4) . . ? Cl1 Ti1 Cl3 170.01(4) . . ? C1 O1 Ti1 147.2(2) . . ? C2 O2 C7 118.8(2) . . ? C16 O3 C13 108.6(3) . . ? C16 O3 Ti1 126.8(2) . . ? C13 O3 Ti1 124.5(2) . . ? C17 O4 C20 108.5(2) . . ? C17 O4 Ti1 128.7(2) . . ? C20 O4 Ti1 122.61(18) . . ? O1 C1 C6 120.8(3) . . ? O1 C1 C2 118.7(3) . . ? C6 C1 C2 120.5(3) . . ? O2 C2 C3 125.2(3) . . ? O2 C2 C1 115.4(2) . . ? C3 C2 C1 119.4(3) . . ? C2 C3 C4 119.9(3) . . ? C5 C4 C3 120.6(3) . . ? C4 C5 C6 120.4(3) . . ? C5 C6 C1 119.1(3) . . ? C8 C7 C12 121.7(3) . . ? C8 C7 O2 120.0(3) . . ? C12 C7 O2 118.1(3) . . ? C7 C8 C9 118.7(3) . . ? C10 C9 C8 120.3(3) . . ? C9 C10 C11 120.2(3) . . ? C12 C11 C10 120.2(3) . . ? C7 C12 C11 119.0(3) . . ? O3 C13 C14 105.8(3) . . ? C13 C14 C15 102.9(3) . . ? C16 C15 C14 102.1(3) . . ? O3 C16 C15 103.2(3) . . ? O4 C17 C18 106.4(3) . . ? C17 C18 C19 106.0(3) . . ? C20 C19 C18 105.4(3) . . ? O4 C20 C19 108.1(3) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 30.60 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 2.248 _refine_diff_density_min -0.780 _refine_diff_density_rms 0.162 data_d:\as4d4\d4orig\new _database_code_depnum_ccdc_archive 'CCDC 844801' #TrackingRef '- revised compound 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C24 H16 Cl4 F4 O4 T2), 0.5(C6 H6)' _chemical_formula_sum 'C27 H19 Cl4 F4 O4 Ti2' _chemical_formula_weight 721.02 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' 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' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6850(12) _cell_length_b 11.9650(19) _cell_length_c 12.1750(10) _cell_angle_alpha 83.761(4) _cell_angle_beta 77.674(11) _cell_angle_gamma 61.545(16) _cell_volume 1462.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13230 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 26.44 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 722 _exptl_absorpt_coefficient_mu 0.970 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Data completeness is limited by the single axis goniometer on the MX beamlines at the Australian Synchrotron. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.710894 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Synchrotron ID' _diffrn_radiation_monochromator Si<111> _diffrn_measurement_device_type '3-ID1 Australian Synchrotron' _diffrn_measurement_method Rotation _diffrn_detector_area_resol_mean 'ADSC Q315' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16033 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 26.44 _reflns_number_total 4172 _reflns_number_gt 3753 _reflns_threshold_expression >2sigma(I) _computing_data_collection BLU-ICE _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; 'X-SEED (Barbour, 2008) and ORTEPIII (Farrugia, 1998)' ; _computing_publication_material 'WinGX (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Disorder was apparent in the lattice benzene. The molecule lies on an inversion centre and the refinement was handled with the use of partial occupancies, EXYZ/EADP cards. ; _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^)+(0.0647P)^2^+7.6204P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4172 _refine_ls_number_parameters 363 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0638 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1486 _refine_ls_wR_factor_gt 0.1445 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.84593(8) 0.57765(8) 0.48315(7) 0.0181(2) Uani 1 1 d . . . Ti2 Ti 0.66444(8) 0.38289(8) 0.53721(7) 0.0206(2) Uani 1 1 d . . . Cl1 Cl 0.79666(12) 0.76508(11) 0.55409(11) 0.0273(3) Uani 1 1 d . . . Cl2 Cl 0.87352(11) 0.36514(11) 0.43731(10) 0.0225(3) Uani 1 1 d . . . Cl3 Cl 0.65899(11) 0.57383(11) 0.61168(10) 0.0220(3) Uani 1 1 d . . . Cl4 Cl 0.43794(11) 0.46116(11) 0.62076(10) 0.0227(3) Uani 1 1 d . . . F1 F 0.4606(4) 1.0444(3) 0.1212(3) 0.0524(10) Uani 1 1 d . . . F2 F 1.1399(4) 0.5863(4) -0.0540(3) 0.0519(10) Uani 1 1 d . . . F3 F 0.9012(4) -0.0534(4) 0.0931(3) 0.0621(11) Uani 1 1 d . . . F4 F 0.8757(4) -0.1646(3) 0.8748(4) 0.0578(11) Uani 1 1 d . . . O1 O 0.7660(3) 0.6503(3) 0.3690(3) 0.0211(7) Uani 1 1 d . . . O2 O 1.0260(3) 0.5212(3) 0.4018(3) 0.0191(7) Uani 1 1 d . . . O3 O 0.6862(3) 0.2554(4) 0.4512(3) 0.0325(9) Uani 1 1 d . . . O4 O 0.7208(3) 0.2904(3) 0.6591(3) 0.0280(8) Uani 1 1 d . . . C1 C 0.6878(5) 0.7473(5) 0.3058(4) 0.0224(11) Uani 1 1 d . . . C2 C 0.7268(5) 0.7460(5) 0.1906(4) 0.0274(12) Uani 1 1 d . . . H2 H 0.8057 0.6769 0.1550 0.033 Uiso 1 1 calc R . . C3 C 0.6497(6) 0.8464(6) 0.1280(5) 0.0356(14) Uani 1 1 d . . . H3 H 0.6748 0.8482 0.0485 0.043 Uiso 1 1 calc R . . C4 C 0.5365(6) 0.9432(6) 0.1824(5) 0.0362(14) Uani 1 1 d . . . C5 C 0.4944(6) 0.9449(6) 0.2973(5) 0.0392(14) Uani 1 1 d . . . H5 H 0.4143 1.0133 0.3323 0.047 Uiso 1 1 calc R . . C6 C 0.5715(5) 0.8448(5) 0.3601(5) 0.0317(13) Uani 1 1 d . . . H6 H 0.5453 0.8427 0.4394 0.038 Uiso 1 1 calc R . . C7 C 1.0590(4) 0.5349(5) 0.2855(4) 0.0213(11) Uani 1 1 d . . . C8 C 1.0773(5) 0.4434(5) 0.2147(4) 0.0283(12) Uani 1 1 d . . . H8 H 1.0708 0.3695 0.2444 0.034 Uiso 1 1 calc R . . C9 C 1.1055(6) 0.4605(6) 0.0991(5) 0.0368(14) Uani 1 1 d . . . H9 H 1.1183 0.3989 0.0484 0.044 Uiso 1 1 calc R . . C10 C 1.1144(5) 0.5682(6) 0.0605(5) 0.0363(14) Uani 1 1 d . . . C11 C 1.0994(6) 0.6585(6) 0.1289(5) 0.0395(15) Uani 1 1 d . . . H11 H 1.1084 0.7310 0.0984 0.047 Uiso 1 1 calc R . . C12 C 1.0706(5) 0.6423(6) 0.2445(5) 0.0309(12) Uani 1 1 d . . . H12 H 1.0591 0.7040 0.2946 0.037 Uiso 1 1 calc R . . C13 C 0.7346(6) 0.1862(6) 0.3667(6) 0.0383(16) Uani 1 1 d . . . C14 C 0.7777(6) 0.2275(6) 0.2592(5) 0.0371(14) Uani 1 1 d . . . H14 H 0.7687 0.3111 0.2500 0.045 Uiso 1 1 calc R . . C15 C 0.8333(6) 0.1460(6) 0.1673(5) 0.0445(15) Uani 1 1 d . . . H15 H 0.8615 0.1731 0.0951 0.053 Uiso 1 1 calc R . . C16 C 0.8460(6) 0.0267(6) 0.1839(6) 0.0428(15) Uani 1 1 d . . . C17 C 0.8070(6) -0.0189(6) 0.2849(6) 0.0445(15) Uani 1 1 d . . . H17 H 0.8177 -0.1031 0.2922 0.053 Uiso 1 1 calc R . . C18 C 0.7516(6) 0.0613(6) 0.3758(6) 0.0405(15) Uani 1 1 d . . . H18 H 0.7240 0.0313 0.4467 0.049 Uiso 1 1 calc R . . C19 C 0.7627(5) 0.1767(5) 0.7105(5) 0.0283(12) Uani 1 1 d . . . C20 C 0.8467(5) 0.0642(5) 0.6509(5) 0.0344(13) Uani 1 1 d . . . H20 H 0.8778 0.0666 0.5724 0.041 Uiso 1 1 calc R . . C21 C 0.8836(6) -0.0498(6) 0.7074(5) 0.0386(14) Uani 1 1 d . . . H21 H 0.9399 -0.1274 0.6683 0.046 Uiso 1 1 calc R . . C22 C 0.8388(6) -0.0506(5) 0.8198(6) 0.0397(15) Uani 1 1 d . . . C23 C 0.7570(6) 0.0576(6) 0.8811(5) 0.0431(15) Uani 1 1 d . . . H23 H 0.7272 0.0534 0.9596 0.052 Uiso 1 1 calc R . . C24 C 0.7189(6) 0.1737(5) 0.8252(5) 0.0356(13) Uani 1 1 d . . . H24 H 0.6631 0.2506 0.8655 0.043 Uiso 1 1 calc R . . C25 C 1.5120(19) 0.3972(14) 0.1012(18) 0.082(5) Uiso 0.50 1 d PD . . H25 H 1.5381 0.3556 0.1694 0.099 Uiso 0.50 1 calc PR . . C26 C 1.4591(14) 0.3484(13) 0.0571(10) 0.050(3) Uiso 0.50 1 d PD . . H26 H 1.4375 0.2830 0.0883 0.060 Uiso 0.50 1 calc PR . . C27 C 1.4388(18) 0.4069(13) -0.0434(12) 0.081(5) Uiso 0.50 1 d PD . . H27 H 1.4085 0.3754 -0.0931 0.098 Uiso 0.50 1 calc PR . . C28 C 1.4595(9) 0.5067(9) -0.0761(7) 0.081(3) Uiso 0.50 1 d P . . H28 H 1.4254 0.4808 -0.1269 0.098 Uiso 0.50 1 calc PR . . C28A C 1.4595(9) 0.5067(9) -0.0761(7) 0.081(3) Uiso 0.50 1 d PD . . H28A H 1.4287 0.5497 -0.1423 0.098 Uiso 0.50 1 calc PR . . C29 C 1.5194(15) 0.5534(14) -0.0251(9) 0.062(4) Uiso 0.25 1 d PD . . H29 H 1.5432 0.6179 -0.0549 0.074 Uiso 0.50 1 calc PR . . C29A C 1.5194(15) 0.5534(14) -0.0251(9) 0.062(4) Uiso 0.25 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0145(4) 0.0200(5) 0.0195(5) 0.0025(4) -0.0052(3) -0.0075(3) Ti2 0.0163(4) 0.0233(5) 0.0232(5) 0.0047(4) -0.0059(3) -0.0102(4) Cl1 0.0225(6) 0.0225(6) 0.0352(7) -0.0012(6) -0.0074(5) -0.0081(5) Cl2 0.0161(6) 0.0233(6) 0.0275(6) -0.0027(5) -0.0016(4) -0.0093(5) Cl3 0.0173(6) 0.0269(6) 0.0212(6) -0.0011(5) -0.0019(4) -0.0102(5) Cl4 0.0180(6) 0.0300(6) 0.0214(6) 0.0055(5) -0.0051(4) -0.0128(5) F1 0.054(2) 0.041(2) 0.051(2) 0.0217(18) -0.0269(18) -0.0107(17) F2 0.052(2) 0.085(3) 0.0199(17) 0.0179(18) -0.0069(15) -0.037(2) F3 0.076(3) 0.054(2) 0.048(2) -0.017(2) -0.002(2) -0.024(2) F4 0.069(3) 0.0307(19) 0.070(3) 0.0184(19) -0.020(2) -0.0215(18) O1 0.0176(16) 0.0233(17) 0.0230(18) 0.0039(15) -0.0065(13) -0.0096(14) O2 0.0151(16) 0.0231(17) 0.0204(17) 0.0006(15) -0.0049(13) -0.0094(14) O3 0.0179(18) 0.040(2) 0.025(2) 0.013(2) -0.0002(15) -0.0063(16) O4 0.0202(18) 0.032(2) 0.034(2) 0.0062(17) -0.0071(15) -0.0139(15) C1 0.017(2) 0.026(3) 0.027(3) 0.006(2) -0.010(2) -0.012(2) C2 0.028(3) 0.031(3) 0.023(3) 0.000(2) -0.007(2) -0.013(2) C3 0.037(3) 0.043(3) 0.026(3) 0.011(3) -0.010(2) -0.018(3) C4 0.036(3) 0.032(3) 0.041(3) 0.013(3) -0.020(3) -0.013(3) C5 0.027(3) 0.032(3) 0.042(4) 0.002(3) -0.008(2) 0.000(2) C6 0.025(3) 0.035(3) 0.026(3) 0.001(3) -0.001(2) -0.009(2) C7 0.015(2) 0.027(3) 0.020(3) 0.002(2) -0.0041(18) -0.008(2) C8 0.028(3) 0.027(3) 0.027(3) 0.001(2) -0.005(2) -0.011(2) C9 0.033(3) 0.042(3) 0.026(3) 0.002(3) -0.004(2) -0.011(3) C10 0.030(3) 0.056(4) 0.020(3) 0.011(3) -0.006(2) -0.020(3) C11 0.045(3) 0.053(4) 0.031(3) 0.018(3) -0.013(3) -0.033(3) C12 0.032(3) 0.039(3) 0.029(3) 0.005(3) -0.007(2) -0.024(3) C13 0.042(3) 0.031(3) 0.061(4) 0.013(3) -0.035(3) -0.024(3) C14 0.043(3) 0.035(3) 0.032(3) 0.004(3) -0.007(3) -0.018(3) C15 0.051(4) 0.045(4) 0.035(4) 0.003(3) -0.008(3) -0.020(3) C16 0.046(4) 0.041(3) 0.039(4) -0.009(3) -0.005(3) -0.018(3) C17 0.051(4) 0.036(3) 0.051(4) -0.006(3) -0.006(3) -0.024(3) C18 0.042(3) 0.043(3) 0.042(4) 0.002(3) -0.007(3) -0.025(3) C19 0.023(3) 0.033(3) 0.031(3) 0.003(3) -0.009(2) -0.014(2) C20 0.027(3) 0.037(3) 0.033(3) -0.002(3) -0.005(2) -0.010(2) C21 0.032(3) 0.030(3) 0.049(4) -0.006(3) -0.012(3) -0.007(2) C22 0.045(4) 0.026(3) 0.050(4) 0.009(3) -0.018(3) -0.016(3) C23 0.049(4) 0.039(3) 0.034(3) 0.006(3) -0.003(3) -0.018(3) C24 0.041(3) 0.028(3) 0.033(3) -0.001(3) -0.005(2) -0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O1 1.754(3) . ? Ti1 O2 1.941(3) . ? Ti1 O2 2.109(3) 2_766 ? Ti1 Cl1 2.2550(16) . ? Ti1 Cl3 2.4172(14) . ? Ti1 Cl2 2.5162(15) . ? Ti1 Ti1 3.2674(17) 2_766 ? Ti2 O4 1.796(4) . ? Ti2 O3 1.831(5) . ? Ti2 Cl4 2.3690(14) . ? Ti2 Cl2 2.4054(14) . ? Ti2 Cl3 2.5165(15) . ? Ti2 Cl4 2.5859(14) 2_666 ? Cl4 Ti2 2.5859(14) 2_666 ? F1 C4 1.367(6) . ? F2 C10 1.377(6) . ? F3 C16 1.376(8) . ? F4 C22 1.364(7) . ? O1 C1 1.368(6) . ? O2 C7 1.399(6) . ? O2 Ti1 2.109(3) 2_766 ? O3 C13 1.246(8) . ? O4 C19 1.339(6) . ? C1 C2 1.378(7) . ? C1 C6 1.385(7) . ? C2 C3 1.378(7) . ? C2 H2 0.9500 . ? C3 C4 1.365(9) . ? C3 H3 0.9500 . ? C4 C5 1.380(9) . ? C5 C6 1.377(8) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.374(8) . ? C7 C12 1.385(7) . ? C8 C9 1.391(8) . ? C8 H8 0.9500 . ? C9 C10 1.367(9) . ? C9 H9 0.9500 . ? C10 C11 1.358(9) . ? C11 C12 1.391(8) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.406(8) . ? C13 C14 1.423(9) . ? C14 C15 1.396(9) . ? C14 H14 0.9500 . ? C15 C16 1.360(9) . ? C15 H15 0.9500 . ? C16 C17 1.367(9) . ? C17 C18 1.377(9) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.385(8) . ? C19 C20 1.396(8) . ? C20 C21 1.372(8) . ? C20 H20 0.9500 . ? C21 C22 1.357(9) . ? C21 H21 0.9500 . ? C22 C23 1.368(9) . ? C23 C24 1.387(8) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.25(2) . ? C25 C28 1.331(5) 2_865 ? C25 H25 0.9500 . ? C26 C27 1.351(5) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C25 1.331(5) 2_865 ? C28 C29A 1.365(5) 2_865 ? C28 H28 0.9500 . ? C29 C28 1.365(5) 2_865 ? C29 H29 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ti1 O2 97.14(14) . . ? O1 Ti1 O2 169.57(14) . 2_766 ? O2 Ti1 O2 72.51(15) . 2_766 ? O1 Ti1 Cl1 93.01(12) . . ? O2 Ti1 Cl1 102.46(11) . . ? O2 Ti1 Cl1 90.55(10) 2_766 . ? O1 Ti1 Cl3 97.69(11) . . ? O2 Ti1 Cl3 159.83(10) . . ? O2 Ti1 Cl3 92.08(9) 2_766 . ? Cl1 Ti1 Cl3 90.35(5) . . ? O1 Ti1 Cl2 91.61(12) . . ? O2 Ti1 Cl2 86.57(10) . . ? O2 Ti1 Cl2 86.59(10) 2_766 . ? Cl1 Ti1 Cl2 169.26(6) . . ? Cl3 Ti1 Cl2 79.42(5) . . ? O1 Ti1 Ti1 135.12(12) . 2_766 ? O2 Ti1 Ti1 38.00(9) . 2_766 ? O2 Ti1 Ti1 34.51(9) 2_766 2_766 ? Cl1 Ti1 Ti1 97.72(5) . 2_766 ? Cl3 Ti1 Ti1 125.53(5) . 2_766 ? Cl2 Ti1 Ti1 85.76(4) . 2_766 ? O4 Ti2 O3 98.71(17) . . ? O4 Ti2 Cl4 93.34(12) . . ? O3 Ti2 Cl4 100.07(12) . . ? O4 Ti2 Cl2 97.99(11) . . ? O3 Ti2 Cl2 89.60(11) . . ? Cl4 Ti2 Cl2 163.85(6) . . ? O4 Ti2 Cl3 91.37(13) . . ? O3 Ti2 Cl3 166.20(12) . . ? Cl4 Ti2 Cl3 88.65(5) . . ? Cl2 Ti2 Cl3 79.64(5) . . ? O4 Ti2 Cl4 172.76(13) . 2_666 ? O3 Ti2 Cl4 87.22(11) . 2_666 ? Cl4 Ti2 Cl4 81.48(5) . 2_666 ? Cl2 Ti2 Cl4 86.14(5) . 2_666 ? Cl3 Ti2 Cl4 83.50(5) . 2_666 ? Ti2 Cl2 Ti1 99.62(5) . . ? Ti1 Cl3 Ti2 99.30(5) . . ? Ti2 Cl4 Ti2 98.52(5) . 2_666 ? C1 O1 Ti1 157.4(3) . . ? C7 O2 Ti1 123.8(3) . . ? C7 O2 Ti1 128.4(3) . 2_766 ? Ti1 O2 Ti1 107.49(15) . 2_766 ? C13 O3 Ti2 154.2(4) . . ? C19 O4 Ti2 147.1(4) . . ? O1 C1 C2 119.5(4) . . ? O1 C1 C6 118.6(5) . . ? C2 C1 C6 121.9(5) . . ? C1 C2 C3 119.0(5) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C4 C3 C2 118.7(5) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C3 C4 F1 119.1(5) . . ? C3 C4 C5 123.1(5) . . ? F1 C4 C5 117.7(5) . . ? C6 C5 C4 118.3(5) . . ? C6 C5 H5 120.9 . . ? C4 C5 H5 120.9 . . ? C5 C6 C1 119.0(5) . . ? C5 C6 H6 120.5 . . ? C1 C6 H6 120.5 . . ? C8 C7 C12 121.6(5) . . ? C8 C7 O2 119.8(4) . . ? C12 C7 O2 118.6(5) . . ? C7 C8 C9 119.2(5) . . ? C7 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? C10 C9 C8 118.3(6) . . ? C10 C9 H9 120.9 . . ? C8 C9 H9 120.9 . . ? C11 C10 C9 123.5(5) . . ? C11 C10 F2 118.1(5) . . ? C9 C10 F2 118.4(6) . . ? C10 C11 C12 118.5(6) . . ? C10 C11 H11 120.7 . . ? C12 C11 H11 120.7 . . ? C7 C12 C11 118.9(6) . . ? C7 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? O3 C13 C18 120.2(6) . . ? O3 C13 C14 122.4(5) . . ? C18 C13 C14 117.4(7) . . ? C15 C14 C13 120.4(6) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C16 C15 C14 118.2(6) . . ? C16 C15 H15 120.9 . . ? C14 C15 H15 120.9 . . ? C15 C16 C17 124.3(7) . . ? C15 C16 F3 117.9(6) . . ? C17 C16 F3 117.8(6) . . ? C16 C17 C18 117.8(6) . . ? C16 C17 H17 121.1 . . ? C18 C17 H17 121.1 . . ? C17 C18 C13 122.0(6) . . ? C17 C18 H18 119.0 . . ? C13 C18 H18 119.0 . . ? O4 C19 C24 117.8(5) . . ? O4 C19 C20 121.6(5) . . ? C24 C19 C20 120.6(5) . . ? C21 C20 C19 119.1(5) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? C22 C21 C20 119.4(6) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C21 C22 F4 118.7(6) . . ? C21 C22 C23 123.2(5) . . ? F4 C22 C23 118.0(6) . . ? C22 C23 C24 118.1(6) . . ? C22 C23 H23 120.9 . . ? C24 C23 H23 120.9 . . ? C19 C24 C23 119.6(6) . . ? C19 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C26 C25 C28 135.6(18) . 2_865 ? C26 C25 H25 112.2 . . ? C28 C25 H25 112.2 2_865 . ? C25 C26 C27 106.5(14) . . ? C25 C26 H26 126.8 . . ? C27 C26 H26 126.8 . . ? C26 C27 H27 118.5 . . ? C25 C28 C29A 118.0(15) 2_865 2_865 ? C25 C28 H28 121.0 2_865 . ? C29A C28 H28 121.0 2_865 . ? C28 C29 H29 125.4 2_865 . ? 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 O4 Ti2 Cl2 Ti1 -100.53(13) . . . . ? O3 Ti2 Cl2 Ti1 160.73(11) . . . . ? Cl4 Ti2 Cl2 Ti1 33.6(2) . . . . ? Cl3 Ti2 Cl2 Ti1 -10.60(5) . . . . ? Cl4 Ti2 Cl2 Ti1 73.49(5) 2_666 . . . ? O1 Ti1 Cl2 Ti2 -86.48(11) . . . . ? O2 Ti1 Cl2 Ti2 176.46(10) . . . . ? O2 Ti1 Cl2 Ti2 103.81(10) 2_766 . . . ? Cl1 Ti1 Cl2 Ti2 29.0(3) . . . . ? Cl3 Ti1 Cl2 Ti2 11.04(5) . . . . ? Ti1 Ti1 Cl2 Ti2 138.39(5) 2_766 . . . ? O1 Ti1 Cl3 Ti2 79.67(12) . . . . ? O2 Ti1 Cl3 Ti2 -57.3(3) . . . . ? O2 Ti1 Cl3 Ti2 -96.68(10) 2_766 . . . ? Cl1 Ti1 Cl3 Ti2 172.76(5) . . . . ? Cl2 Ti1 Cl3 Ti2 -10.54(5) . . . . ? Ti1 Ti1 Cl3 Ti2 -87.50(7) 2_766 . . . ? O4 Ti2 Cl3 Ti1 108.89(12) . . . . ? O3 Ti2 Cl3 Ti1 -28.2(5) . . . . ? Cl4 Ti2 Cl3 Ti1 -157.80(5) . . . . ? Cl2 Ti2 Cl3 Ti1 11.03(5) . . . . ? Cl4 Ti2 Cl3 Ti1 -76.22(5) 2_666 . . . ? O4 Ti2 Cl4 Ti2 174.91(13) . . . 2_666 ? O3 Ti2 Cl4 Ti2 -85.62(12) . . . 2_666 ? Cl2 Ti2 Cl4 Ti2 40.3(2) . . . 2_666 ? Cl3 Ti2 Cl4 Ti2 83.62(5) . . . 2_666 ? Cl4 Ti2 Cl4 Ti2 0.0 2_666 . . 2_666 ? O2 Ti1 O1 C1 -113.4(8) . . . . ? O2 Ti1 O1 C1 -120.3(10) 2_766 . . . ? Cl1 Ti1 O1 C1 -10.5(8) . . . . ? Cl3 Ti1 O1 C1 80.3(8) . . . . ? Cl2 Ti1 O1 C1 159.8(8) . . . . ? Ti1 Ti1 O1 C1 -114.6(7) 2_766 . . . ? O1 Ti1 O2 C7 -4.6(4) . . . . ? O2 Ti1 O2 C7 174.1(4) 2_766 . . . ? Cl1 Ti1 O2 C7 -99.3(3) . . . . ? Cl3 Ti1 O2 C7 132.4(3) . . . . ? Cl2 Ti1 O2 C7 86.6(3) . . . . ? Ti1 Ti1 O2 C7 174.1(4) 2_766 . . . ? O1 Ti1 O2 Ti1 -178.70(16) . . . 2_766 ? O2 Ti1 O2 Ti1 0.0 2_766 . . 2_766 ? Cl1 Ti1 O2 Ti1 86.60(13) . . . 2_766 ? Cl3 Ti1 O2 Ti1 -41.7(4) . . . 2_766 ? Cl2 Ti1 O2 Ti1 -87.51(13) . . . 2_766 ? O4 Ti2 O3 C13 -118.9(8) . . . . ? Cl4 Ti2 O3 C13 146.1(8) . . . . ? Cl2 Ti2 O3 C13 -20.9(8) . . . . ? Cl3 Ti2 O3 C13 17.6(12) . . . . ? Cl4 Ti2 O3 C13 65.3(8) 2_666 . . . ? O3 Ti2 O4 C19 -4.7(6) . . . . ? Cl4 Ti2 O4 C19 96.0(6) . . . . ? Cl2 Ti2 O4 C19 -95.6(6) . . . . ? Cl3 Ti2 O4 C19 -175.3(6) . . . . ? Cl4 Ti2 O4 C19 140.0(8) 2_666 . . . ? Ti1 O1 C1 C2 140.1(7) . . . . ? Ti1 O1 C1 C6 -39.5(10) . . . . ? O1 C1 C2 C3 -177.7(5) . . . . ? C6 C1 C2 C3 1.8(8) . . . . ? C1 C2 C3 C4 -0.6(8) . . . . ? C2 C3 C4 F1 178.8(5) . . . . ? C2 C3 C4 C5 -0.8(9) . . . . ? C3 C4 C5 C6 1.0(10) . . . . ? F1 C4 C5 C6 -178.6(5) . . . . ? C4 C5 C6 C1 0.3(9) . . . . ? O1 C1 C6 C5 177.9(5) . . . . ? C2 C1 C6 C5 -1.7(8) . . . . ? Ti1 O2 C7 C8 -86.6(5) . . . . ? Ti1 O2 C7 C8 86.1(5) 2_766 . . . ? Ti1 O2 C7 C12 92.5(5) . . . . ? Ti1 O2 C7 C12 -94.8(5) 2_766 . . . ? C12 C7 C8 C9 -1.3(8) . . . . ? O2 C7 C8 C9 177.8(4) . . . . ? C7 C8 C9 C10 0.2(8) . . . . ? C8 C9 C10 C11 1.2(9) . . . . ? C8 C9 C10 F2 -178.9(5) . . . . ? C9 C10 C11 C12 -1.5(9) . . . . ? F2 C10 C11 C12 178.6(5) . . . . ? C8 C7 C12 C11 1.0(8) . . . . ? O2 C7 C12 C11 -178.0(5) . . . . ? C10 C11 C12 C7 0.3(8) . . . . ? Ti2 O3 C13 C18 149.8(6) . . . . ? Ti2 O3 C13 C14 -28.5(11) . . . . ? O3 C13 C14 C15 179.0(5) . . . . ? C18 C13 C14 C15 0.6(8) . . . . ? C13 C14 C15 C16 -0.7(9) . . . . ? C14 C15 C16 C17 0.5(10) . . . . ? C14 C15 C16 F3 -179.8(5) . . . . ? C15 C16 C17 C18 -0.2(10) . . . . ? F3 C16 C17 C18 -180.0(6) . . . . ? C16 C17 C18 C13 0.1(9) . . . . ? O3 C13 C18 C17 -178.8(5) . . . . ? C14 C13 C18 C17 -0.4(9) . . . . ? Ti2 O4 C19 C24 -140.5(5) . . . . ? Ti2 O4 C19 C20 38.8(9) . . . . ? O4 C19 C20 C21 -178.2(5) . . . . ? C24 C19 C20 C21 1.1(8) . . . . ? C19 C20 C21 C22 -0.6(9) . . . . ? C20 C21 C22 F4 179.7(5) . . . . ? C20 C21 C22 C23 0.3(10) . . . . ? C21 C22 C23 C24 -0.4(10) . . . . ? F4 C22 C23 C24 -179.7(6) . . . . ? O4 C19 C24 C23 178.2(5) . . . . ? C20 C19 C24 C23 -1.1(9) . . . . ? C22 C23 C24 C19 0.8(9) . . . . ? C28 C25 C26 C27 6(3) 2_865 . . . ? _diffrn_measured_fraction_theta_max 0.898 _diffrn_reflns_theta_full 26.44 _diffrn_measured_fraction_theta_full 0.898 _refine_diff_density_max 1.580 _refine_diff_density_min -0.847 _refine_diff_density_rms 0.105 # Attachment '- compound 3.cif' data_d:\as5m9b\new\new _database_code_depnum_ccdc_archive 'CCDC 844802' #TrackingRef '- compound 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H34 Cl2 O2 Ti' _chemical_formula_sum 'C24 H34 Cl2 O2 Ti' _chemical_formula_weight 473.31 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.603(2) _cell_length_b 31.616(2) _cell_length_c 15.1970(13) _cell_angle_alpha 90.00 _cell_angle_beta 95.004(11) _cell_angle_gamma 90.00 _cell_volume 5075.0(13) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 47685 _cell_measurement_theta_min 1.40 _cell_measurement_theta_max 26.42 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.239 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 0.564 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Data completeness is low owing to the single axis rotation goniometer available at the Australian Synchrotron. Crystal selection was difficult owing to the rapid dissolving of the crystals in the mounting oil. This resulted in a high Rint for a number of crystals. The best refinement is presented. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77500 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Synchrotron ID' _diffrn_radiation_monochromator Si<111> _diffrn_measurement_device_type '3-ID1 Australian Synchrotron' _diffrn_measurement_method Rotation _diffrn_detector_area_resol_mean 'ADSC Q315' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55883 _diffrn_reflns_av_R_equivalents 0.1100 _diffrn_reflns_av_sigmaI/netI 0.0616 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 26.42 _reflns_number_total 7576 _reflns_number_gt 6920 _reflns_threshold_expression >2sigma(I) _computing_data_collection BLU-ICE _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; 'X-SEED (Barbour, 2008) and ORTEPIII (Farrugia, 1998)' ; _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0639P)^2^+2.7619P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7576 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1205 _refine_ls_wR_factor_gt 0.1183 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 0.06562(3) 0.241256(12) 0.89050(2) 0.01921(13) Uani 1 1 d . . . Ti2 Ti 0.05778(4) 0.010140(12) 0.70666(3) 0.02200(13) Uani 1 1 d . . . Cl1 Cl -0.04192(5) 0.296501(19) 0.93540(4) 0.03044(16) Uani 1 1 d . . . Cl2 Cl -0.06560(6) 0.18811(2) 0.85276(4) 0.03643(17) Uani 1 1 d . . . Cl3 Cl 0.08111(7) 0.07725(2) 0.74780(5) 0.04451(19) Uani 1 1 d . . . Cl4 Cl 0.18195(6) -0.00453(2) 0.60036(4) 0.03704(17) Uani 1 1 d . . . O1 O 0.14302(14) 0.25716(5) 0.79963(10) 0.0204(3) Uani 1 1 d . . . O2 O 0.17469(14) 0.22467(5) 0.97616(10) 0.0220(3) Uani 1 1 d . . . O3 O 0.10461(14) -0.02211(5) 0.79749(10) 0.0226(3) Uani 1 1 d . . . O4 O -0.10019(14) 0.00191(5) 0.66742(11) 0.0243(4) Uani 1 1 d . . . C1 C 0.20709(19) 0.27276(7) 0.73129(14) 0.0193(4) Uani 1 1 d . . . C2 C 0.2160(2) 0.24706(7) 0.65788(15) 0.0220(5) Uani 1 1 d . . . C3 C 0.2721(2) 0.26497(8) 0.58716(16) 0.0263(5) Uani 1 1 d . . . H3 H 0.2799 0.2486 0.5355 0.032 Uiso 1 1 calc R . . C4 C 0.3166(2) 0.30610(8) 0.59050(16) 0.0264(5) Uani 1 1 d . . . H4 H 0.3524 0.3178 0.5408 0.032 Uiso 1 1 calc R . . C5 C 0.3094(2) 0.33039(7) 0.66599(16) 0.0247(5) Uani 1 1 d . . . H5 H 0.3423 0.3584 0.6679 0.030 Uiso 1 1 calc R . . C6 C 0.2544(2) 0.31419(7) 0.73918(15) 0.0197(5) Uani 1 1 d . . . C7 C 0.1658(2) 0.20208(8) 0.65504(16) 0.0272(5) Uani 1 1 d . . . H7 H 0.1463 0.1946 0.7163 0.033 Uiso 1 1 calc R . . C8 C 0.2639(3) 0.17053(8) 0.6281(2) 0.0398(6) Uani 1 1 d . . . H8A H 0.3418 0.1735 0.6674 0.060 Uiso 1 1 calc R . . H8B H 0.2821 0.1760 0.5671 0.060 Uiso 1 1 calc R . . H8C H 0.2309 0.1417 0.6327 0.060 Uiso 1 1 calc R . . C9 C 0.0431(3) 0.19895(10) 0.5965(3) 0.0607(10) Uani 1 1 d . . . H9A H 0.0128 0.1697 0.5957 0.091 Uiso 1 1 calc R . . H9B H 0.0576 0.2077 0.5363 0.091 Uiso 1 1 calc R . . H9C H -0.0205 0.2174 0.6195 0.091 Uiso 1 1 calc R . . C10 C 0.2447(2) 0.33868(7) 0.82404(15) 0.0228(5) Uani 1 1 d . . . H10 H 0.1570 0.3347 0.8420 0.027 Uiso 1 1 calc R . . C11 C 0.3373(2) 0.32070(8) 0.89856(16) 0.0283(5) Uani 1 1 d . . . H11A H 0.3298 0.3369 0.9529 0.043 Uiso 1 1 calc R . . H11B H 0.4241 0.3228 0.8815 0.043 Uiso 1 1 calc R . . H11C H 0.3168 0.2910 0.9087 0.043 Uiso 1 1 calc R . . C12 C 0.2667(3) 0.38616(8) 0.81503(17) 0.0329(6) Uani 1 1 d . . . H12A H 0.2591 0.4000 0.8721 0.049 Uiso 1 1 calc R . . H12B H 0.2035 0.3979 0.7708 0.049 Uiso 1 1 calc R . . H12C H 0.3517 0.3911 0.7964 0.049 Uiso 1 1 calc R . . C13 C 0.2630(2) 0.21058(6) 1.04180(14) 0.0189(5) Uani 1 1 d . . . C14 C 0.2393(2) 0.21880(7) 1.12942(14) 0.0196(5) Uani 1 1 d . . . C15 C 0.3259(2) 0.20233(7) 1.19488(15) 0.0233(5) Uani 1 1 d . . . H15 H 0.3131 0.2067 1.2553 0.028 Uiso 1 1 calc R . . C16 C 0.4304(2) 0.17965(7) 1.17296(16) 0.0253(5) Uani 1 1 d . . . H16 H 0.4873 0.1681 1.2185 0.030 Uiso 1 1 calc R . . C17 C 0.4530(2) 0.17356(7) 1.08569(16) 0.0243(5) Uani 1 1 d . . . H17 H 0.5268 0.1587 1.0722 0.029 Uiso 1 1 calc R . . C18 C 0.3693(2) 0.18888(7) 1.01671(15) 0.0214(5) Uani 1 1 d . . . C19 C 0.1276(2) 0.24585(7) 1.15026(15) 0.0230(5) Uani 1 1 d . . . H19 H 0.0568 0.2399 1.1040 0.028 Uiso 1 1 calc R . . C20 C 0.1615(2) 0.29264(7) 1.14317(17) 0.0293(5) Uani 1 1 d . . . H20A H 0.0890 0.3100 1.1565 0.044 Uiso 1 1 calc R . . H20B H 0.1831 0.2988 1.0831 0.044 Uiso 1 1 calc R . . H20C H 0.2342 0.2991 1.1853 0.044 Uiso 1 1 calc R . . C21 C 0.0793(2) 0.23615(8) 1.23976(17) 0.0316(6) Uani 1 1 d . . . H21A H 0.0074 0.2546 1.2490 0.047 Uiso 1 1 calc R . . H21B H 0.1473 0.2411 1.2866 0.047 Uiso 1 1 calc R . . H21C H 0.0523 0.2065 1.2412 0.047 Uiso 1 1 calc R . . C22 C 0.3891(2) 0.18158(7) 0.92052(16) 0.0263(5) Uani 1 1 d . . . H22 H 0.3532 0.2065 0.8866 0.032 Uiso 1 1 calc R . . C23 C 0.5284(3) 0.17810(9) 0.90340(19) 0.0392(6) Uani 1 1 d . . . H23A H 0.5352 0.1734 0.8402 0.059 Uiso 1 1 calc R . . H23B H 0.5671 0.1543 0.9372 0.059 Uiso 1 1 calc R . . H23C H 0.5723 0.2043 0.9218 0.059 Uiso 1 1 calc R . . C24 C 0.3158(3) 0.14249(9) 0.88566(19) 0.0432(7) Uani 1 1 d . . . H24A H 0.3295 0.1382 0.8233 0.065 Uiso 1 1 calc R . . H24B H 0.2253 0.1466 0.8914 0.065 Uiso 1 1 calc R . . H24C H 0.3457 0.1176 0.9199 0.065 Uiso 1 1 calc R . . C25 C -0.2254(2) -0.00948(7) 0.64971(15) 0.0223(5) Uani 1 1 d . . . C26 C -0.3175(2) 0.02204(7) 0.65295(15) 0.0256(5) Uani 1 1 d . . . C27 C -0.4426(2) 0.00985(8) 0.63155(18) 0.0333(6) Uani 1 1 d . . . H27 H -0.5081 0.0303 0.6327 0.040 Uiso 1 1 calc R . . C28 C -0.4734(2) -0.03149(9) 0.60859(18) 0.0365(6) Uani 1 1 d . . . H28 H -0.5592 -0.0390 0.5933 0.044 Uiso 1 1 calc R . . C29 C -0.3801(2) -0.06192(8) 0.60779(17) 0.0323(6) Uani 1 1 d . . . H29 H -0.4029 -0.0902 0.5927 0.039 Uiso 1 1 calc R . . C30 C -0.2527(2) -0.05184(7) 0.62872(15) 0.0238(5) Uani 1 1 d . . . C31 C -0.2794(2) 0.06723(8) 0.67612(18) 0.0321(6) Uani 1 1 d . . . H31 H -0.2012 0.0657 0.7177 0.039 Uiso 1 1 calc R . . C32 C -0.3771(3) 0.09180(9) 0.7232(2) 0.0436(7) Uani 1 1 d . . . H32A H -0.3458 0.1205 0.7360 0.065 Uiso 1 1 calc R . . H32B H -0.3918 0.0775 0.7785 0.065 Uiso 1 1 calc R . . H32C H -0.4566 0.0932 0.6852 0.065 Uiso 1 1 calc R . . C33 C -0.2438(3) 0.09075(9) 0.5941(2) 0.0509(8) Uani 1 1 d . . . H33A H -0.2193 0.1198 0.6101 0.076 Uiso 1 1 calc R . . H33B H -0.3165 0.0912 0.5496 0.076 Uiso 1 1 calc R . . H33C H -0.1726 0.0763 0.5699 0.076 Uiso 1 1 calc R . . C34 C -0.1483(2) -0.08449(7) 0.62649(16) 0.0254(5) Uani 1 1 d . . . H34 H -0.0793 -0.0761 0.6722 0.030 Uiso 1 1 calc R . . C35 C -0.0919(3) -0.08404(8) 0.53691(17) 0.0337(6) Uani 1 1 d . . . H35A H -0.0248 -0.1054 0.5369 0.050 Uiso 1 1 calc R . . H35B H -0.0564 -0.0560 0.5267 0.050 Uiso 1 1 calc R . . H35C H -0.1583 -0.0904 0.4899 0.050 Uiso 1 1 calc R . . C36 C -0.1908(3) -0.12865(8) 0.6500(2) 0.0434(7) Uani 1 1 d . . . H36A H -0.1200 -0.1484 0.6474 0.065 Uiso 1 1 calc R . . H36B H -0.2611 -0.1375 0.6079 0.065 Uiso 1 1 calc R . . H36C H -0.2186 -0.1285 0.7098 0.065 Uiso 1 1 calc R . . C37 C 0.1393(2) -0.04571(7) 0.87149(14) 0.0200(5) Uani 1 1 d . . . C38 C 0.0445(2) -0.06495(7) 0.91574(15) 0.0215(5) Uani 1 1 d . . . C39 C 0.0827(2) -0.08744(7) 0.99218(16) 0.0265(5) Uani 1 1 d . . . H39 H 0.0209 -0.1008 1.0244 0.032 Uiso 1 1 calc R . . C40 C 0.2098(2) -0.09065(8) 1.02206(17) 0.0300(5) Uani 1 1 d . . . H40 H 0.2340 -0.1057 1.0749 0.036 Uiso 1 1 calc R . . C41 C 0.3014(2) -0.07200(7) 0.97536(16) 0.0269(5) Uani 1 1 d . . . H41 H 0.3881 -0.0749 0.9962 0.032 Uiso 1 1 calc R . . C42 C 0.2691(2) -0.04904(7) 0.89838(15) 0.0219(5) Uani 1 1 d . . . C43 C -0.0940(2) -0.06005(7) 0.88140(17) 0.0264(5) Uani 1 1 d . . . H43 H -0.0968 -0.0599 0.8155 0.032 Uiso 1 1 calc R . . C44 C -0.1767(3) -0.09637(10) 0.9062(2) 0.0495(8) Uani 1 1 d . . . H44A H -0.2642 -0.0913 0.8822 0.074 Uiso 1 1 calc R . . H44B H -0.1735 -0.0986 0.9707 0.074 Uiso 1 1 calc R . . H44C H -0.1460 -0.1228 0.8819 0.074 Uiso 1 1 calc R . . C45 C -0.1452(3) -0.01710(10) 0.9086(2) 0.0502(8) Uani 1 1 d . . . H45A H -0.0888 0.0054 0.8914 0.075 Uiso 1 1 calc R . . H45B H -0.1494 -0.0165 0.9727 0.075 Uiso 1 1 calc R . . H45C H -0.2301 -0.0128 0.8791 0.075 Uiso 1 1 calc R . . C46 C 0.3658(2) -0.02732(8) 0.84576(16) 0.0260(5) Uani 1 1 d . . . H46 H 0.3316 -0.0276 0.7823 0.031 Uiso 1 1 calc R . . C47 C 0.4940(2) -0.04989(9) 0.85198(18) 0.0357(6) Uani 1 1 d . . . H47A H 0.5523 -0.0345 0.8169 0.054 Uiso 1 1 calc R . . H47B H 0.4829 -0.0788 0.8292 0.054 Uiso 1 1 calc R . . H47C H 0.5290 -0.0509 0.9138 0.054 Uiso 1 1 calc R . . C48 C 0.3806(3) 0.01890(9) 0.87425(19) 0.0383(6) Uani 1 1 d . . . H48A H 0.4431 0.0327 0.8400 0.057 Uiso 1 1 calc R . . H48B H 0.4092 0.0202 0.9373 0.057 Uiso 1 1 calc R . . H48C H 0.2990 0.0334 0.8637 0.057 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 0.0177(2) 0.0244(2) 0.0155(2) 0.00305(14) 0.00137(15) 0.00015(15) Ti2 0.0183(2) 0.0190(2) 0.0283(3) 0.00418(15) -0.00052(16) -0.00128(15) Cl1 0.0291(3) 0.0382(3) 0.0251(3) 0.0064(2) 0.0084(2) 0.0132(2) Cl2 0.0351(3) 0.0437(4) 0.0300(4) 0.0043(3) -0.0005(3) -0.0187(3) Cl3 0.0418(4) 0.0220(3) 0.0675(5) -0.0029(3) -0.0083(3) -0.0067(3) Cl4 0.0314(3) 0.0452(4) 0.0358(4) 0.0160(3) 0.0102(3) 0.0097(3) O1 0.0215(8) 0.0227(8) 0.0174(8) 0.0003(6) 0.0036(6) -0.0026(6) O2 0.0229(8) 0.0240(8) 0.0187(8) 0.0007(6) -0.0005(6) 0.0015(6) O3 0.0197(8) 0.0252(8) 0.0226(9) 0.0034(6) -0.0005(6) -0.0020(6) O4 0.0197(8) 0.0223(8) 0.0300(9) 0.0016(6) -0.0019(6) -0.0001(6) C1 0.0160(10) 0.0237(11) 0.0184(12) 0.0036(9) 0.0032(8) 0.0001(9) C2 0.0175(11) 0.0266(12) 0.0216(13) -0.0024(9) 0.0005(9) -0.0003(9) C3 0.0263(12) 0.0310(13) 0.0221(13) -0.0033(9) 0.0051(9) 0.0034(10) C4 0.0244(12) 0.0321(13) 0.0240(13) 0.0071(9) 0.0086(9) 0.0041(10) C5 0.0224(12) 0.0239(12) 0.0282(13) 0.0041(9) 0.0040(9) -0.0001(9) C6 0.0172(10) 0.0218(11) 0.0200(12) 0.0008(8) 0.0010(8) 0.0011(8) C7 0.0278(12) 0.0298(13) 0.0246(13) -0.0050(9) 0.0061(9) -0.0059(10) C8 0.0456(16) 0.0271(14) 0.0492(18) -0.0019(11) 0.0184(13) -0.0023(12) C9 0.0424(18) 0.0406(18) 0.094(3) -0.0028(17) -0.0235(17) -0.0145(14) C10 0.0235(11) 0.0236(12) 0.0213(12) -0.0009(9) 0.0023(9) -0.0019(9) C11 0.0318(13) 0.0288(13) 0.0235(13) -0.0020(9) -0.0027(10) -0.0062(10) C12 0.0435(15) 0.0237(13) 0.0314(15) -0.0028(10) 0.0018(11) -0.0025(11) C13 0.0198(11) 0.0176(11) 0.0184(12) 0.0027(8) -0.0026(8) -0.0015(8) C14 0.0210(11) 0.0181(11) 0.0194(12) 0.0003(8) 0.0001(8) -0.0060(8) C15 0.0224(11) 0.0268(12) 0.0200(12) -0.0002(9) -0.0018(9) -0.0050(9) C16 0.0198(11) 0.0280(12) 0.0268(14) 0.0051(9) -0.0052(9) -0.0024(9) C17 0.0195(11) 0.0233(12) 0.0295(14) 0.0023(9) -0.0002(9) 0.0012(9) C18 0.0222(11) 0.0181(11) 0.0239(13) 0.0016(8) 0.0016(9) -0.0023(9) C19 0.0217(12) 0.0249(12) 0.0223(13) -0.0011(9) 0.0002(9) 0.0009(9) C20 0.0306(13) 0.0246(13) 0.0325(14) -0.0042(10) 0.0013(10) 0.0021(10) C21 0.0293(13) 0.0406(15) 0.0255(14) 0.0012(10) 0.0058(10) 0.0048(11) C22 0.0297(12) 0.0258(12) 0.0239(13) 0.0014(9) 0.0057(9) 0.0033(10) C23 0.0368(15) 0.0498(17) 0.0328(16) 0.0055(12) 0.0133(11) 0.0110(12) C24 0.0642(19) 0.0371(15) 0.0295(16) -0.0103(11) 0.0119(13) -0.0100(13) C25 0.0184(11) 0.0261(12) 0.0220(13) 0.0036(9) -0.0004(9) 0.0003(9) C26 0.0248(12) 0.0271(12) 0.0250(13) 0.0038(9) 0.0024(9) 0.0047(10) C27 0.0206(12) 0.0392(15) 0.0399(16) 0.0029(11) 0.0006(10) 0.0086(10) C28 0.0195(12) 0.0481(16) 0.0411(16) -0.0040(12) -0.0025(10) -0.0023(11) C29 0.0291(13) 0.0322(14) 0.0350(15) -0.0032(10) -0.0002(10) -0.0056(10) C30 0.0251(12) 0.0244(12) 0.0214(12) 0.0003(9) -0.0001(9) -0.0002(9) C31 0.0301(13) 0.0257(13) 0.0412(16) 0.0049(11) 0.0064(11) 0.0045(10) C32 0.0521(17) 0.0318(15) 0.0500(19) -0.0006(12) 0.0220(14) 0.0041(13) C33 0.071(2) 0.0311(15) 0.055(2) 0.0059(13) 0.0312(16) 0.0044(14) C34 0.0296(12) 0.0204(12) 0.0257(13) -0.0002(9) 0.0008(9) 0.0005(9) C35 0.0383(14) 0.0320(14) 0.0313(15) 0.0009(10) 0.0067(11) 0.0077(11) C36 0.0455(17) 0.0277(14) 0.059(2) 0.0088(12) 0.0128(13) 0.0017(12) C37 0.0242(11) 0.0175(11) 0.0182(12) -0.0011(8) 0.0015(8) 0.0015(9) C38 0.0228(11) 0.0201(11) 0.0220(12) -0.0049(8) 0.0045(9) -0.0008(9) C39 0.0311(13) 0.0228(12) 0.0269(13) -0.0024(9) 0.0099(10) -0.0018(9) C40 0.0387(14) 0.0253(12) 0.0257(14) 0.0039(9) 0.0017(10) 0.0043(10) C41 0.0257(12) 0.0290(13) 0.0254(13) -0.0026(9) -0.0015(9) 0.0056(10) C42 0.0210(11) 0.0213(11) 0.0233(12) -0.0043(9) 0.0006(9) -0.0003(9) C43 0.0187(12) 0.0270(13) 0.0339(14) -0.0088(10) 0.0040(9) -0.0046(9) C44 0.0335(15) 0.0538(19) 0.060(2) 0.0108(15) -0.0003(13) -0.0202(13) C45 0.0262(14) 0.0497(18) 0.074(2) -0.0228(16) -0.0020(13) 0.0069(13) C46 0.0198(12) 0.0321(13) 0.0259(13) -0.0022(9) 0.0001(9) -0.0036(9) C47 0.0202(12) 0.0549(17) 0.0318(15) 0.0003(11) 0.0012(10) 0.0019(11) C48 0.0356(15) 0.0395(15) 0.0401(16) -0.0031(12) 0.0051(11) -0.0148(12) _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 1.7411(15) . ? Ti1 O2 1.7448(15) . ? Ti1 Cl2 2.2247(7) . ? Ti1 Cl1 2.2254(7) . ? Ti2 O4 1.7477(16) . ? Ti2 O3 1.7528(15) . ? Ti2 Cl3 2.2196(8) . ? Ti2 Cl4 2.2202(8) . ? O1 C1 1.381(3) . ? O2 C13 1.381(3) . ? O3 C37 1.373(3) . ? O4 C25 1.379(3) . ? C1 C2 1.390(3) . ? C1 C6 1.404(3) . ? C2 C3 1.393(3) . ? C2 C7 1.518(3) . ? C3 C4 1.383(4) . ? C4 C5 1.388(3) . ? C5 C6 1.398(3) . ? C6 C10 1.515(3) . ? C7 C9 1.513(4) . ? C7 C8 1.523(4) . ? C10 C12 1.527(3) . ? C10 C11 1.541(3) . ? C13 C18 1.401(3) . ? C13 C14 1.401(3) . ? C14 C15 1.394(3) . ? C14 C19 1.517(3) . ? C15 C16 1.385(3) . ? C16 C17 1.382(4) . ? C17 C18 1.400(3) . ? C18 C22 1.513(3) . ? C19 C21 1.525(3) . ? C19 C20 1.528(3) . ? C22 C23 1.526(3) . ? C22 C24 1.530(4) . ? C25 C26 1.399(3) . ? C25 C30 1.401(3) . ? C26 C27 1.392(4) . ? C26 C31 1.518(4) . ? C27 C28 1.385(4) . ? C28 C29 1.381(4) . ? C29 C30 1.397(3) . ? C30 C34 1.516(3) . ? C31 C32 1.522(4) . ? C31 C33 1.527(4) . ? C34 C36 1.519(3) . ? C34 C35 1.534(4) . ? C37 C38 1.397(3) . ? C37 C42 1.405(3) . ? C38 C39 1.392(3) . ? C38 C43 1.523(3) . ? C39 C40 1.387(4) . ? C40 C41 1.384(4) . ? C41 C42 1.394(3) . ? C42 C46 1.518(3) . ? C43 C44 1.512(4) . ? C43 C45 1.532(4) . ? C46 C48 1.528(4) . ? C46 C47 1.532(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ti1 O2 110.55(7) . . ? O1 Ti1 Cl2 109.94(5) . . ? O2 Ti1 Cl2 108.92(6) . . ? O1 Ti1 Cl1 107.82(5) . . ? O2 Ti1 Cl1 109.33(6) . . ? Cl2 Ti1 Cl1 110.26(3) . . ? O4 Ti2 O3 112.29(7) . . ? O4 Ti2 Cl3 108.56(6) . . ? O3 Ti2 Cl3 108.50(6) . . ? O4 Ti2 Cl4 109.40(6) . . ? O3 Ti2 Cl4 107.84(6) . . ? Cl3 Ti2 Cl4 110.24(3) . . ? C1 O1 Ti1 175.34(14) . . ? C13 O2 Ti1 177.89(15) . . ? C37 O3 Ti2 176.97(15) . . ? C25 O4 Ti2 169.42(15) . . ? O1 C1 C2 117.86(19) . . ? O1 C1 C6 117.67(19) . . ? C2 C1 C6 124.4(2) . . ? C1 C2 C3 116.4(2) . . ? C1 C2 C7 121.5(2) . . ? C3 C2 C7 122.1(2) . . ? C4 C3 C2 121.4(2) . . ? C3 C4 C5 120.5(2) . . ? C4 C5 C6 120.8(2) . . ? C5 C6 C1 116.4(2) . . ? C5 C6 C10 123.6(2) . . ? C1 C6 C10 119.97(19) . . ? C9 C7 C2 111.1(2) . . ? C9 C7 C8 111.8(2) . . ? C2 C7 C8 112.0(2) . . ? C6 C10 C12 113.82(19) . . ? C6 C10 C11 110.55(19) . . ? C12 C10 C11 109.64(19) . . ? O2 C13 C18 118.2(2) . . ? O2 C13 C14 117.41(19) . . ? C18 C13 C14 124.4(2) . . ? C15 C14 C13 116.6(2) . . ? C15 C14 C19 122.6(2) . . ? C13 C14 C19 120.73(19) . . ? C16 C15 C14 120.8(2) . . ? C17 C16 C15 120.8(2) . . ? C16 C17 C18 121.3(2) . . ? C17 C18 C13 116.0(2) . . ? C17 C18 C22 122.6(2) . . ? C13 C18 C22 121.4(2) . . ? C14 C19 C21 113.67(19) . . ? C14 C19 C20 109.76(19) . . ? C21 C19 C20 110.9(2) . . ? C18 C22 C23 113.2(2) . . ? C18 C22 C24 110.4(2) . . ? C23 C22 C24 110.7(2) . . ? O4 C25 C26 118.0(2) . . ? O4 C25 C30 118.0(2) . . ? C26 C25 C30 123.9(2) . . ? C27 C26 C25 116.6(2) . . ? C27 C26 C31 122.9(2) . . ? C25 C26 C31 120.4(2) . . ? C28 C27 C26 121.3(2) . . ? C29 C28 C27 120.4(2) . . ? C28 C29 C30 121.2(2) . . ? C29 C30 C25 116.5(2) . . ? C29 C30 C34 122.2(2) . . ? C25 C30 C34 121.3(2) . . ? C26 C31 C32 114.3(2) . . ? C26 C31 C33 110.4(2) . . ? C32 C31 C33 111.2(2) . . ? C30 C34 C36 112.9(2) . . ? C30 C34 C35 110.83(19) . . ? C36 C34 C35 111.3(2) . . ? O3 C37 C38 118.57(19) . . ? O3 C37 C42 117.69(19) . . ? C38 C37 C42 123.7(2) . . ? C39 C38 C37 117.0(2) . . ? C39 C38 C43 122.7(2) . . ? C37 C38 C43 120.3(2) . . ? C40 C39 C38 121.0(2) . . ? C41 C40 C39 120.4(2) . . ? C40 C41 C42 121.3(2) . . ? C41 C42 C37 116.5(2) . . ? C41 C42 C46 123.3(2) . . ? C37 C42 C46 120.1(2) . . ? C44 C43 C38 113.6(2) . . ? C44 C43 C45 112.3(2) . . ? C38 C43 C45 110.56(19) . . ? C42 C46 C48 109.9(2) . . ? C42 C46 C47 113.2(2) . . ? C48 C46 C47 111.0(2) . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 0.633 _refine_diff_density_min -0.593 _refine_diff_density_rms 0.075 # Attachment '- compound 5.cif' data_d:\as8e3\new\new _database_code_depnum_ccdc_archive 'CCDC 844803' #TrackingRef '- compound 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H15 Cl3 O3 Ti' _chemical_formula_sum 'C7 H15 Cl3 O3 Ti' _chemical_formula_weight 301.44 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 13.6280(7) _cell_length_b 13.1540(8) _cell_length_c 13.825(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2478.3(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 22216 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 26.23 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 1.317 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Data completeness is low owing to the single axis rotation goniometer available at the Australian Synchrotron. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77488 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Synchrotron ID' _diffrn_radiation_monochromator Si<111> _diffrn_measurement_device_type '3-ID1 Australian Synchrotron' _diffrn_measurement_method Rotation _diffrn_detector_area_resol_mean 'ADSC Q315' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24737 _diffrn_reflns_av_R_equivalents 0.0616 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 26.23 _reflns_number_total 1832 _reflns_number_gt 1751 _reflns_threshold_expression >2sigma(I) _computing_data_collection BLU-ICE _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; 'X-SEED (Barbour, 2008) and ORTEPIII (Farrugia, 1998)' ; _computing_publication_material 'WinGX (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A two-site population disorder in the conformation of the THF ring was apparent in difference maps that was modelled by a complimentary model using EXYZ/EAPD cards. ; _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^)+(0.0302P)^2^+2.4654P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1832 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0275 _refine_ls_R_factor_gt 0.0265 _refine_ls_wR_factor_ref 0.0677 _refine_ls_wR_factor_gt 0.0671 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 0.06004(3) 0.20852(3) 0.71594(3) 0.01569(14) Uani 1 1 d . A . Cl1 Cl 0.14567(4) 0.12207(4) 0.60119(4) 0.02189(16) Uani 1 1 d . . . Cl2 Cl -0.04010(4) 0.29730(4) 0.61141(4) 0.02991(17) Uani 1 1 d . . . Cl3 Cl 0.16453(4) 0.34839(4) 0.73370(4) 0.02604(16) Uani 1 1 d . . . O1 O -0.02849(11) 0.10923(11) 0.74433(11) 0.0227(3) Uani 1 1 d . . . O2 O -0.02070(11) 0.27015(11) 0.83927(11) 0.0200(3) Uani 1 1 d . . . O3 O 0.14873(10) 0.14242(11) 0.82497(11) 0.0197(3) Uani 1 1 d . . . C1 C -0.08283(17) 0.10455(18) 0.83253(18) 0.0292(5) Uani 1 1 d . . . H1A H -0.0425 0.0737 0.8844 0.035 Uiso 1 1 calc R . . H1B H -0.1427 0.0630 0.8239 0.035 Uiso 1 1 calc R . . C2 C -0.10955(16) 0.21194(17) 0.85829(17) 0.0241(5) Uani 1 1 d . . . H2A H -0.1646 0.2365 0.8178 0.029 Uiso 1 1 calc R . . H2B H -0.1286 0.2171 0.9272 0.029 Uiso 1 1 calc R . . C3 C -0.03138(18) 0.37450(17) 0.87232(18) 0.0276(5) Uani 1 1 d . . . H3A H 0.0292 0.4121 0.8589 0.041 Uiso 1 1 calc R . . H3B H -0.0443 0.3750 0.9421 0.041 Uiso 1 1 calc R . . H3C H -0.0863 0.4067 0.8383 0.041 Uiso 1 1 calc R . . C4A C 0.16585(18) 0.03193(16) 0.82879(17) 0.0263(5) Uani 0.717(15) 1 d P A 1 H4A H 0.2201 0.0121 0.7851 0.032 Uiso 0.717(15) 1 calc PR A 1 H4B H 0.1060 -0.0059 0.8100 0.032 Uiso 0.717(15) 1 calc PR A 1 C4B C 0.16585(18) 0.03193(16) 0.82879(17) 0.0263(5) Uani 0.283(15) 1 d P A 2 H4B1 H 0.1930 0.0067 0.7668 0.032 Uiso 0.283(15) 1 calc PR A 2 H4B2 H 0.1043 -0.0051 0.8432 0.032 Uiso 0.283(15) 1 calc PR A 2 C5A C 0.1925(6) 0.0111(3) 0.9336(4) 0.0334(14) Uani 0.717(15) 1 d P A 1 H5A H 0.2347 -0.0498 0.9393 0.040 Uiso 0.717(15) 1 calc PR A 1 H5B H 0.1330 0.0015 0.9737 0.040 Uiso 0.717(15) 1 calc PR A 1 C5B C 0.2413(13) 0.0193(10) 0.9122(10) 0.031(3) Uani 0.283(15) 1 d P A 2 H8A H 0.2376 -0.0488 0.9424 0.037 Uiso 0.283(15) 1 calc PR A 2 H8B H 0.3094 0.0327 0.8905 0.037 Uiso 0.283(15) 1 calc PR A 2 C6A C 0.2476(6) 0.1068(4) 0.9628(5) 0.0315(14) Uani 0.717(15) 1 d P A 1 H6A H 0.2480 0.1156 1.0339 0.038 Uiso 0.717(15) 1 calc PR A 1 H6B H 0.3161 0.1054 0.9390 0.038 Uiso 0.717(15) 1 calc PR A 1 C6B C 0.2038(13) 0.1013(12) 0.9782(10) 0.028(3) Uani 0.283(15) 1 d P A 2 H9A H 0.1413 0.0806 1.0090 0.034 Uiso 0.283(15) 1 calc PR A 2 H9B H 0.2523 0.1171 1.0294 0.034 Uiso 0.283(15) 1 calc PR A 2 C7A C 0.18877(18) 0.19019(18) 0.91362(17) 0.0269(5) Uani 0.717(15) 1 d P A 1 H7A H 0.1351 0.2142 0.9561 0.032 Uiso 0.717(15) 1 calc PR A 1 H7B H 0.2314 0.2486 0.8971 0.032 Uiso 0.717(15) 1 calc PR A 1 C7B C 0.18877(18) 0.19019(18) 0.91362(17) 0.0269(5) Uani 0.283(15) 1 d P A 2 H7B1 H 0.1416 0.2391 0.9419 0.032 Uiso 0.283(15) 1 calc PR A 2 H7B2 H 0.2514 0.2256 0.9003 0.032 Uiso 0.283(15) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0157(2) 0.0155(2) 0.0159(2) -0.00029(13) -0.00046(14) 0.00116(14) Cl1 0.0247(3) 0.0225(3) 0.0184(3) -0.0018(2) 0.0033(2) 0.0039(2) Cl2 0.0333(3) 0.0291(3) 0.0273(4) 0.0018(2) -0.0084(2) 0.0110(2) Cl3 0.0264(3) 0.0181(3) 0.0336(4) -0.0005(2) 0.0011(2) -0.0048(2) O1 0.0228(8) 0.0239(8) 0.0213(9) -0.0046(6) -0.0003(6) 0.0000(6) O2 0.0196(7) 0.0168(7) 0.0237(9) -0.0024(6) 0.0022(6) 0.0007(6) O3 0.0252(8) 0.0154(7) 0.0184(8) -0.0024(6) -0.0052(6) 0.0022(6) C1 0.0262(12) 0.0289(13) 0.0325(14) -0.0010(10) 0.0062(10) -0.0083(10) C2 0.0187(11) 0.0315(12) 0.0222(13) -0.0016(9) 0.0021(9) -0.0021(9) C3 0.0330(13) 0.0205(12) 0.0293(14) -0.0059(9) 0.0050(10) 0.0052(10) C4A 0.0364(13) 0.0151(11) 0.0274(14) -0.0020(9) -0.0072(10) 0.0069(9) C4B 0.0364(13) 0.0151(11) 0.0274(14) -0.0020(9) -0.0072(10) 0.0069(9) C5A 0.042(4) 0.027(2) 0.032(3) 0.0092(17) -0.017(2) -0.006(2) C5B 0.032(7) 0.028(5) 0.033(7) 0.002(4) -0.010(6) 0.007(6) C6A 0.028(3) 0.035(2) 0.032(3) 0.0019(17) -0.016(3) -0.004(3) C6B 0.017(7) 0.045(7) 0.024(6) -0.003(4) -0.013(5) 0.009(6) C7A 0.0323(13) 0.0270(12) 0.0213(13) -0.0078(9) -0.0111(10) -0.0020(10) C7B 0.0323(13) 0.0270(12) 0.0213(13) -0.0078(9) -0.0111(10) -0.0020(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O1 1.8209(15) . ? Ti1 O3 2.1186(15) . ? Ti1 O2 2.1852(15) . ? Ti1 Cl1 2.2741(7) . ? Ti1 Cl2 2.3053(7) . ? Ti1 Cl3 2.3394(6) . ? O1 C1 1.428(3) . ? O2 C3 1.454(3) . ? O2 C2 1.457(3) . ? O3 C4A 1.473(3) . ? O3 C7A 1.482(3) . ? C1 C2 1.502(3) . ? C4A C5A 1.519(5) . ? C5A C6A 1.521(9) . ? C5B C6B 1.50(2) . ? C6A C7A 1.520(6) . ? 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 O3 86.00(6) . . ? O1 Ti1 O2 76.37(6) . . ? O3 Ti1 O2 83.36(6) . . ? O1 Ti1 Cl1 97.57(5) . . ? O3 Ti1 Cl1 89.91(4) . . ? O2 Ti1 Cl1 171.20(4) . . ? O1 Ti1 Cl2 96.10(5) . . ? O3 Ti1 Cl2 172.56(4) . . ? O2 Ti1 Cl2 90.18(4) . . ? Cl1 Ti1 Cl2 96.88(3) . . ? O1 Ti1 Cl3 160.87(6) . . ? O3 Ti1 Cl3 84.31(4) . . ? O2 Ti1 Cl3 86.15(4) . . ? Cl1 Ti1 Cl3 98.87(2) . . ? Cl2 Ti1 Cl3 91.59(2) . . ? C1 O1 Ti1 123.96(13) . . ? C3 O2 C2 110.88(16) . . ? C3 O2 Ti1 130.23(13) . . ? C2 O2 Ti1 111.37(12) . . ? C4A O3 C7A 109.30(16) . . ? C4A O3 Ti1 121.39(12) . . ? C7A O3 Ti1 128.65(12) . . ? O1 C1 C2 106.73(18) . . ? O2 C2 C1 104.49(17) . . ? O3 C4A C5A 104.5(2) . . ? C4A C5A C6A 102.8(4) . . ? C7A C6A C5A 102.6(5) . . ? O3 C7A C6A 105.0(3) . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 26.23 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 0.243 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.059 # Attachment '- revised compoundTiCl3(OAriPr).cif' data_d:\as4e1\e1orig\new _database_code_depnum_ccdc_archive 'CCDC 844804' #TrackingRef '- revised compoundTiCl3(OAriPr).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H17 Cl3 O Ti' _chemical_formula_sum 'C12 H17 Cl3 O Ti' _chemical_formula_weight 331.51 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41 c d' _symmetry_space_group_name_Hall 'I 4bw -2c' _symmetry_Int_Tables_number 110 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x+1/2, z+1/4' '-x, -y, z' 'y, -x+1/2, z+1/4' '-x, y, z+1/2' 'x, -y, z+1/2' '-y+1/2, -x, z+1/4' 'y+1/2, x, z+1/4' 'x+1/2, y+1/2, z+1/2' '-y+1/2, x+1, z+3/4' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1, z+3/4' '-x+1/2, y+1/2, z+1' 'x+1/2, -y+1/2, z+1' '-y+1, -x+1/2, z+3/4' 'y+1, x+1/2, z+3/4' _cell_length_a 25.2188(13) _cell_length_b 25.219(2) _cell_length_c 9.3900(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5971.9(12) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 30132 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 26.44 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2720 _exptl_absorpt_coefficient_mu 1.092 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77506 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Synchrotron ID' _diffrn_radiation_monochromator Si<111> _diffrn_measurement_device_type '3-ID1 Australian Synchrotron' _diffrn_measurement_method Rotation _diffrn_detector_area_resol_mean 'ADSC Q315' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30340 _diffrn_reflns_av_R_equivalents 0.0914 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 26.44 _reflns_number_total 2348 _reflns_number_gt 2324 _reflns_threshold_expression >2sigma(I) _computing_data_collection BLU-ICE _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; 'X-SEED (Barbour, 2008) and ORTEPIII (Farrugia, 1998)' ; _computing_publication_material 'WinGX (Farrugia, 1999)' _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. Inversion of the structure gives the same high flack parameter. THE DISORDER NOTED IN C8 AND C9 HAS BEEN MODELLED AS A TWO PART REFINED COMPLEMENTARY DISORDER (OCCUPANCIES OF 0.493(6) AND 0.507(6)) INVOLVING C8A/C9A AND C8B/C9B THAT INCLUDES THE USE OF PART, DFIX/DANG AND EXYZ/EADP CARDS TO HANDLE THE CALCULATION OF ALL HYDROGEN ATOMS OF THE ISOPROPYL GROUP. DAMP Was NOT NECESSARY IN THE REFINEMENT PROCESS. ; _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^)+(0.0438P)^2^+14.3206P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.90(4) _refine_ls_number_reflns 2348 _refine_ls_number_parameters 173 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0346 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0859 _refine_ls_wR_factor_gt 0.0857 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.085 _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 0.32881(2) 0.22699(2) 0.82229(8) 0.01569(16) Uani 1 1 d . . . Cl1 Cl 0.23743(3) 0.18461(3) 0.82301(9) 0.01810(19) Uani 1 1 d . . . Cl2 Cl 0.27338(3) 0.31303(3) 0.82139(9) 0.01803(19) Uani 1 1 d . . . Cl3 Cl 0.40191(3) 0.27661(3) 0.83359(10) 0.0245(2) Uani 1 1 d . . . O1 O 0.35899(8) 0.16535(8) 0.8121(3) 0.0197(5) Uani 1 1 d . . . C1 C 0.38338(13) 0.11630(12) 0.8109(4) 0.0206(7) Uani 1 1 d . A . C2 C 0.36561(14) 0.07900(14) 0.7108(4) 0.0236(8) Uani 1 1 d . . . C3 C 0.39073(16) 0.02993(16) 0.7127(4) 0.0339(9) Uani 1 1 d . A . H3 H 0.3799 0.0033 0.6472 0.041 Uiso 1 1 calc R . . C4 C 0.43107(16) 0.01901(15) 0.8074(5) 0.0415(11) Uani 1 1 d . . . H4 H 0.4477 -0.0148 0.8061 0.050 Uiso 1 1 calc R A . C5 C 0.44742(17) 0.05681(16) 0.9041(4) 0.0339(9) Uani 1 1 d . A . H5 H 0.4749 0.0484 0.9694 0.041 Uiso 1 1 calc R . . C6 C 0.42448(15) 0.10712(14) 0.9082(4) 0.0238(8) Uani 1 1 d . . . C7A C 0.32272(14) 0.09163(15) 0.6055(4) 0.0282(12) Uani 0.503(6) 1 d PD A 1 H7A H 0.3124 0.1296 0.6184 0.034 Uiso 0.503(6) 1 calc PR A 1 C7B C 0.32272(14) 0.09163(15) 0.6055(4) 0.0282(12) Uani 0.503(6) 1 d PD A 2 H7B H 0.2994 0.1202 0.6450 0.034 Uiso 0.503(6) 1 calc PR A 2 C8A C 0.2744(3) 0.0564(4) 0.6486(15) 0.065(4) Uani 0.503(6) 1 d PD A 1 H8A1 H 0.2659 0.0623 0.7492 0.098 Uiso 0.503(6) 1 calc PR A 1 H8A2 H 0.2832 0.0190 0.6337 0.098 Uiso 0.503(6) 1 calc PR A 1 H8A3 H 0.2437 0.0658 0.5898 0.098 Uiso 0.503(6) 1 calc PR A 1 C9A C 0.3366(6) 0.0834(7) 0.4531(9) 0.109(9) Uani 0.503(6) 1 d PD A 1 H9A1 H 0.3060 0.0924 0.3934 0.163 Uiso 0.503(6) 1 calc PR A 1 H9A2 H 0.3462 0.0461 0.4378 0.163 Uiso 0.503(6) 1 calc PR A 1 H9A3 H 0.3667 0.1061 0.4278 0.163 Uiso 0.503(6) 1 calc PR A 1 C10 C 0.44120(15) 0.14747(14) 1.0192(4) 0.0248(8) Uani 1 1 d . A . H10 H 0.4260 0.1826 0.9912 0.030 Uiso 1 1 calc R . . C11 C 0.41891(18) 0.13292(18) 1.1638(4) 0.0385(10) Uani 1 1 d . . . H11A H 0.4301 0.1593 1.2342 0.058 Uiso 1 1 calc R A . H11B H 0.4321 0.0979 1.1919 0.058 Uiso 1 1 calc R . . H11C H 0.3801 0.1321 1.1589 0.058 Uiso 1 1 calc R . . C12 C 0.50133(19) 0.1536(2) 1.0297(5) 0.0480(12) Uani 1 1 d . . . H12A H 0.5099 0.1800 1.1027 0.072 Uiso 1 1 calc R A . H12B H 0.5154 0.1652 0.9376 0.072 Uiso 1 1 calc R . . H12C H 0.5172 0.1195 1.0556 0.072 Uiso 1 1 calc R . . C9B C 0.3522(3) 0.1130(3) 0.4690(8) 0.026(2) Uani 0.497(6) 1 d PD A 2 H9B1 H 0.3261 0.1220 0.3956 0.038 Uiso 0.497(6) 1 calc PR A 2 H9B2 H 0.3762 0.0856 0.4326 0.038 Uiso 0.497(6) 1 calc PR A 2 H9B3 H 0.3727 0.1447 0.4939 0.038 Uiso 0.497(6) 1 calc PR A 2 C8B C 0.2884(3) 0.0454(3) 0.5542(12) 0.041(2) Uani 0.497(6) 1 d PD A 2 H8B1 H 0.2620 0.0584 0.4859 0.061 Uiso 0.497(6) 1 calc PR A 2 H8B2 H 0.2702 0.0293 0.6357 0.061 Uiso 0.497(6) 1 calc PR A 2 H8B3 H 0.3109 0.0188 0.5080 0.061 Uiso 0.497(6) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0150(3) 0.0150(3) 0.0170(3) 0.0011(3) 0.0009(3) 0.0011(2) Cl1 0.0160(3) 0.0207(4) 0.0177(4) -0.0012(4) 0.0012(4) -0.0019(3) Cl2 0.0196(4) 0.0175(4) 0.0170(4) -0.0003(4) 0.0001(4) 0.0019(3) Cl3 0.0184(4) 0.0252(4) 0.0301(4) 0.0047(4) -0.0014(4) -0.0039(3) O1 0.0208(11) 0.0173(11) 0.0208(12) 0.0017(10) 0.0022(11) 0.0044(8) C1 0.0225(16) 0.0178(15) 0.0215(17) 0.0047(15) 0.0039(16) 0.0028(12) C2 0.0244(19) 0.0223(19) 0.0240(19) 0.0017(15) 0.0016(15) 0.0008(15) C3 0.043(2) 0.022(2) 0.037(2) -0.0075(17) -0.0041(19) 0.0041(17) C4 0.047(2) 0.0233(18) 0.054(3) -0.009(2) -0.009(2) 0.0156(16) C5 0.036(2) 0.028(2) 0.037(2) 0.0041(18) -0.0097(18) 0.0122(17) C6 0.027(2) 0.0220(18) 0.0224(19) 0.0027(14) 0.0010(15) 0.0065(15) C7A 0.026(2) 0.028(2) 0.031(2) -0.0061(16) -0.0043(16) 0.0013(14) C7B 0.026(2) 0.028(2) 0.031(2) -0.0061(16) -0.0043(16) 0.0013(14) C8A 0.037(6) 0.039(6) 0.119(13) 0.006(7) -0.037(7) -0.009(5) C9A 0.115(15) 0.18(2) 0.035(7) -0.059(11) -0.032(8) 0.092(15) C10 0.0264(19) 0.0245(18) 0.0236(18) 0.0033(15) -0.0040(15) 0.0051(15) C11 0.045(3) 0.043(3) 0.028(2) -0.0015(19) 0.0032(19) -0.006(2) C12 0.035(2) 0.059(3) 0.051(3) -0.010(2) 0.011(2) -0.011(2) C9B 0.034(5) 0.036(5) 0.007(4) -0.008(3) -0.002(3) 0.016(4) C8B 0.038(5) 0.031(5) 0.053(7) -0.012(5) -0.002(5) -0.004(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 O1 1.733(2) . ? Ti1 Cl3 2.2306(9) . ? Ti1 Cl2 2.3727(12) 4 ? Ti1 Cl1 2.3797(13) 10_544 ? Ti1 Cl1 2.5402(8) . ? Ti1 Cl2 2.5811(9) . ? Cl1 Ti1 2.3797(13) 4 ? Cl2 Ti1 2.3727(12) 10_544 ? O1 C1 1.382(4) . ? C1 C6 1.401(5) . ? C1 C2 1.403(5) . ? C2 C3 1.390(6) . ? C2 C7A 1.500(5) . ? C3 C4 1.379(6) . ? C3 H3 0.9500 . ? C4 C5 1.379(6) . ? C4 H4 0.9500 . ? C5 C6 1.395(5) . ? C5 H5 0.9500 . ? C6 C10 1.516(5) . ? C7A C9A 1.488(8) . ? C7A C8A 1.561(7) . ? C7A H7A 1.0000 . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? C9A H9A1 0.9800 . ? C9A H9A2 0.9800 . ? C9A H9A3 0.9800 . ? C10 C11 1.515(5) . ? C10 C12 1.527(6) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C9B H9B1 0.9800 . ? C9B H9B2 0.9800 . ? C9B H9B3 0.9800 . ? C8B H8B1 0.9800 . ? C8B H8B2 0.9800 . ? C8B H8B3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ti1 Cl3 98.22(8) . . ? O1 Ti1 Cl2 97.15(9) . 4 ? Cl3 Ti1 Cl2 95.39(4) . 4 ? O1 Ti1 Cl1 96.17(9) . 10_544 ? Cl3 Ti1 Cl1 95.87(4) . 10_544 ? Cl2 Ti1 Cl1 161.13(3) 4 10_544 ? O1 Ti1 Cl1 91.20(7) . . ? Cl3 Ti1 Cl1 170.28(4) . . ? Cl2 Ti1 Cl1 81.00(3) 4 . ? Cl1 Ti1 Cl1 85.42(3) 10_544 . ? O1 Ti1 Cl2 172.51(8) . . ? Cl3 Ti1 Cl2 88.64(3) . . ? Cl2 Ti1 Cl2 85.16(3) 4 . ? Cl1 Ti1 Cl2 80.02(3) 10_544 . ? Cl1 Ti1 Cl2 82.09(3) . . ? Ti1 Cl1 Ti1 99.37(4) 4 . ? Ti1 Cl2 Ti1 98.41(4) 10_544 . ? C1 O1 Ti1 177.3(3) . . ? O1 C1 C6 118.2(3) . . ? O1 C1 C2 117.6(3) . . ? C6 C1 C2 124.2(3) . . ? C3 C2 C1 116.3(3) . . ? C3 C2 C7A 121.7(3) . . ? C1 C2 C7A 122.0(3) . . ? C4 C3 C2 121.5(4) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 120.5(4) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C4 C5 C6 121.5(4) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 116.0(3) . . ? C5 C6 C10 120.9(3) . . ? C1 C6 C10 122.9(3) . . ? C9A C7A C2 115.8(6) . . ? C9A C7A C8A 110.7(7) . . ? C2 C7A C8A 105.8(5) . . ? C9A C7A H7A 108.1 . . ? C2 C7A H7A 108.1 . . ? C8A C7A H7A 108.1 . . ? C7A C8A H8A1 109.5 . . ? C7A C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? C7A C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? C7A C9A H9A1 109.5 . . ? C7A C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? C7A C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? C11 C10 C6 110.5(3) . . ? C11 C10 C12 109.6(3) . . ? C6 C10 C12 112.9(3) . . ? C11 C10 H10 107.9 . . ? C6 C10 H10 107.9 . . ? C12 C10 H10 107.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? H8B1 C8B H8B2 109.5 . . ? H8B1 C8B H8B3 109.5 . . ? H8B2 C8B H8B3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ti1 Cl1 Ti1 88.36(9) . . . 4 ? Cl3 Ti1 Cl1 Ti1 -77.5(3) . . . 4 ? Cl2 Ti1 Cl1 Ti1 -8.69(3) 4 . . 4 ? Cl1 Ti1 Cl1 Ti1 -175.55(3) 10_544 . . 4 ? Cl2 Ti1 Cl1 Ti1 -95.01(3) . . . 4 ? O1 Ti1 Cl2 Ti1 -68.5(7) . . . 10_544 ? Cl3 Ti1 Cl2 Ti1 87.66(4) . . . 10_544 ? Cl2 Ti1 Cl2 Ti1 -176.82(3) 4 . . 10_544 ? Cl1 Ti1 Cl2 Ti1 -8.55(3) 10_544 . . 10_544 ? Cl1 Ti1 Cl2 Ti1 -95.26(3) . . . 10_544 ? Cl3 Ti1 O1 C1 80(4) . . . . ? Cl2 Ti1 O1 C1 -16(4) 4 . . . ? Cl1 Ti1 O1 C1 177(100) 10_544 . . . ? Cl1 Ti1 O1 C1 -98(4) . . . . ? Cl2 Ti1 O1 C1 -124(4) . . . . ? Ti1 O1 C1 C6 -34(5) . . . . ? Ti1 O1 C1 C2 146(4) . . . . ? O1 C1 C2 C3 -179.7(3) . . . . ? C6 C1 C2 C3 1.0(5) . . . . ? O1 C1 C2 C7A 1.6(5) . . . . ? C6 C1 C2 C7A -177.8(3) . . . . ? C1 C2 C3 C4 -0.4(6) . . . . ? C7A C2 C3 C4 178.3(4) . . . . ? C2 C3 C4 C5 0.3(7) . . . . ? C3 C4 C5 C6 -0.9(7) . . . . ? C4 C5 C6 C1 1.3(6) . . . . ? C4 C5 C6 C10 177.3(4) . . . . ? O1 C1 C6 C5 179.2(3) . . . . ? C2 C1 C6 C5 -1.4(5) . . . . ? O1 C1 C6 C10 3.3(5) . . . . ? C2 C1 C6 C10 -177.3(3) . . . . ? C3 C2 C7A C9A -54.2(9) . . . . ? C1 C2 C7A C9A 124.5(9) . . . . ? C3 C2 C7A C8A 68.8(7) . . . . ? C1 C2 C7A C8A -112.6(6) . . . . ? C5 C6 C10 C11 -74.0(5) . . . . ? C1 C6 C10 C11 101.7(4) . . . . ? C5 C6 C10 C12 49.1(5) . . . . ? C1 C6 C10 C12 -135.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.44 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.333 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.068