# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_Braun9 _database_code_depnum_ccdc_archive 'CCDC 871140' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C24 H26 N2 O4 Ti' _chemical_formula_sum 'C24 H26 N2 O4 Ti' _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour red _diffrn_ambient_temperature 173(2) _chemical_formula_weight 454.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? 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 11.1702(2) _cell_length_b 14.4223(5) _cell_length_c 15.9597(5) _cell_angle_alpha 90.00 _cell_angle_beta 114.419(2) _cell_angle_gamma 90.00 _cell_volume 2341.11(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10903 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 0.397 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17236 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0354 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5361 _reflns_number_gt 4570 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material PLATON _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. PLAT220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... PLAT222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... attempts to refine the isopropyl groups as disordered failes. The large Ueq(max)/Ueq(min) is then probably due to rather different thermal properties of the two alcoholates, which is consistent with the nature of these ligands. ; _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^)+(0.0510P)^2^+1.4778P] 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 5361 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0514 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.1114 _refine_ls_wR_factor_gt 0.1064 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 0.15544(3) 0.77768(2) 0.43109(2) 0.02278(10) Uani 1 1 d . . . O1 O 0.18249(12) 0.83072(9) 0.55083(8) 0.0288(3) Uani 1 1 d . . . O2 O 0.16722(13) 0.77483(8) 0.31203(8) 0.0279(3) Uani 1 1 d . . . O3 O -0.01613(12) 0.75430(9) 0.39792(9) 0.0320(3) Uani 1 1 d . . . O4 O 0.22879(13) 0.66537(9) 0.46525(9) 0.0329(3) Uani 1 1 d . . . N1 N 0.35734(14) 0.84125(10) 0.48278(10) 0.0272(3) Uani 1 1 d . . . N2 N 0.10480(13) 0.92258(10) 0.37847(9) 0.0218(3) Uani 1 1 d . . . C1 C 0.29934(18) 0.86446(13) 0.60701(13) 0.0310(4) Uani 1 1 d . . . C2 C 0.3330(2) 0.88946(18) 0.69720(15) 0.0476(5) Uani 1 1 d . . . H2 H 0.2724 0.8835 0.7229 0.057 Uiso 1 1 calc R . . C3 C 0.4602(3) 0.9241(2) 0.75031(17) 0.0605(7) Uani 1 1 d . . . H3 H 0.4822 0.9399 0.8114 0.073 Uiso 1 1 calc R . . C4 C 0.5521(2) 0.93534(18) 0.71553(18) 0.0568(7) Uani 1 1 d . . . H4 H 0.6338 0.9606 0.7519 0.068 Uiso 1 1 calc R . . C5 C 0.52271(19) 0.90846(14) 0.62386(16) 0.0407(5) Uani 1 1 d . . . C6 C 0.6090(2) 0.91256(15) 0.57983(19) 0.0483(6) Uani 1 1 d . . . H6 H 0.6935 0.9360 0.6112 0.058 Uiso 1 1 calc R . . C7 C 0.5696(2) 0.88264(16) 0.49210(18) 0.0466(6) Uani 1 1 d . . . H7 H 0.6267 0.8861 0.4632 0.056 Uiso 1 1 calc R . . C8 C 0.44166(18) 0.84604(13) 0.44434(15) 0.0349(4) Uani 1 1 d . . . H8 H 0.4163 0.8248 0.3844 0.042 Uiso 1 1 calc R . . C9 C 0.39561(17) 0.87281(12) 0.57081(13) 0.0291(4) Uani 1 1 d . . . C10 C 0.13200(16) 0.84876(12) 0.25635(11) 0.0243(3) Uani 1 1 d . . . C11 C 0.12812(19) 0.85142(14) 0.16886(12) 0.0320(4) Uani 1 1 d . . . H11 H 0.1519 0.7995 0.1447 0.038 Uiso 1 1 calc R . . C12 C 0.0878(2) 0.93344(15) 0.11624(13) 0.0366(4) Uani 1 1 d . . . H12 H 0.0856 0.9342 0.0573 0.044 Uiso 1 1 calc R . . C13 C 0.05203(18) 1.01179(14) 0.14831(12) 0.0329(4) Uani 1 1 d . . . H13 H 0.0257 1.0645 0.1116 0.039 Uiso 1 1 calc R . . C14 C 0.05534(16) 1.01201(12) 0.23819(12) 0.0255(3) Uani 1 1 d . . . C15 C 0.01997(18) 1.08745(13) 0.27961(13) 0.0315(4) Uani 1 1 d . . . H15 H -0.0100 1.1424 0.2471 0.038 Uiso 1 1 calc R . . C16 C 0.02991(18) 1.07954(13) 0.36783(13) 0.0317(4) Uani 1 1 d . . . H16 H 0.0076 1.1291 0.3958 0.038 Uiso 1 1 calc R . . C17 C 0.07411(16) 0.99583(12) 0.41544(12) 0.0265(4) Uani 1 1 d . . . H17 H 0.0822 0.9917 0.4757 0.032 Uiso 1 1 calc R . . C18 C 0.09610(15) 0.92992(11) 0.29080(11) 0.0215(3) Uani 1 1 d . . . C19 C -0.1420(2) 0.7863(2) 0.3827(2) 0.0606(7) Uani 1 1 d . . . H19 H -0.1300 0.8456 0.4152 0.073 Uiso 1 1 calc R . . C20 C -0.2179(3) 0.8062(3) 0.2843(3) 0.1206(17) Uani 1 1 d . . . H20A H -0.1728 0.8522 0.2647 0.181 Uiso 1 1 calc R . . H20B H -0.3034 0.8288 0.2746 0.181 Uiso 1 1 calc R . . H20C H -0.2270 0.7504 0.2493 0.181 Uiso 1 1 calc R . . C21 C -0.2045(3) 0.7213(2) 0.4263(2) 0.0703(9) Uani 1 1 d . . . H21A H -0.2099 0.6604 0.4007 0.105 Uiso 1 1 calc R . . H21B H -0.2913 0.7429 0.4147 0.105 Uiso 1 1 calc R . . H21C H -0.1523 0.7190 0.4915 0.105 Uiso 1 1 calc R . . C22 C 0.34363(19) 0.61025(15) 0.49120(15) 0.0391(5) Uani 1 1 d . . . H22 H 0.3924 0.6299 0.4554 0.047 Uiso 1 1 calc R . . C24 C 0.4290(3) 0.62545(19) 0.59211(18) 0.0618(7) Uani 1 1 d . . . H24A H 0.4522 0.6898 0.6027 0.093 Uiso 1 1 calc R . . H24B H 0.5074 0.5888 0.6100 0.093 Uiso 1 1 calc R . . H24C H 0.3816 0.6074 0.6278 0.093 Uiso 1 1 calc R . . C25 C 0.3039(2) 0.51050(17) 0.4692(2) 0.0671(8) Uani 1 1 d . . . H25A H 0.2533 0.4912 0.5023 0.101 Uiso 1 1 calc R . . H25B H 0.3812 0.4726 0.4870 0.101 Uiso 1 1 calc R . . H25C H 0.2519 0.5040 0.4043 0.101 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 0.02340(16) 0.01963(16) 0.02376(16) 0.00191(11) 0.00818(12) -0.00250(11) O1 0.0267(6) 0.0354(7) 0.0238(6) 0.0001(5) 0.0100(5) -0.0042(5) O2 0.0375(7) 0.0192(6) 0.0276(6) -0.0020(5) 0.0139(5) 0.0018(5) O3 0.0245(6) 0.0298(7) 0.0384(7) -0.0001(6) 0.0097(6) -0.0046(5) O4 0.0326(7) 0.0234(6) 0.0408(7) 0.0080(5) 0.0133(6) 0.0029(5) N1 0.0250(7) 0.0224(7) 0.0339(8) 0.0031(6) 0.0120(6) 0.0001(6) N2 0.0217(7) 0.0223(7) 0.0225(7) -0.0008(5) 0.0102(6) -0.0006(5) C1 0.0301(9) 0.0287(9) 0.0287(9) -0.0015(7) 0.0068(7) -0.0008(7) C2 0.0465(12) 0.0563(14) 0.0350(11) -0.0130(10) 0.0118(9) -0.0021(10) C3 0.0559(15) 0.0685(18) 0.0403(13) -0.0248(12) 0.0032(11) -0.0054(13) C4 0.0389(12) 0.0527(15) 0.0548(15) -0.0206(12) -0.0047(11) -0.0090(10) C5 0.0262(9) 0.0285(10) 0.0548(13) -0.0050(9) 0.0041(9) -0.0022(7) C6 0.0234(9) 0.0351(12) 0.0769(17) -0.0040(11) 0.0111(10) -0.0044(8) C7 0.0299(10) 0.0373(11) 0.0804(17) 0.0034(11) 0.0306(11) 0.0003(8) C8 0.0318(10) 0.0293(10) 0.0483(12) 0.0037(8) 0.0212(9) 0.0010(7) C9 0.0252(8) 0.0209(8) 0.0340(9) -0.0015(7) 0.0051(7) -0.0010(7) C10 0.0257(8) 0.0234(8) 0.0234(8) -0.0020(6) 0.0096(7) -0.0015(6) C11 0.0395(10) 0.0329(10) 0.0258(9) -0.0060(7) 0.0157(8) 0.0006(8) C12 0.0432(11) 0.0453(12) 0.0219(9) 0.0023(8) 0.0140(8) -0.0005(9) C13 0.0347(10) 0.0344(10) 0.0256(9) 0.0090(8) 0.0086(8) 0.0020(8) C14 0.0223(8) 0.0256(9) 0.0257(8) 0.0024(7) 0.0070(7) 0.0004(6) C15 0.0298(9) 0.0240(9) 0.0363(10) 0.0055(7) 0.0094(8) 0.0066(7) C16 0.0321(9) 0.0256(9) 0.0390(10) -0.0034(8) 0.0161(8) 0.0068(7) C17 0.0280(9) 0.0276(9) 0.0279(9) -0.0041(7) 0.0154(7) 0.0003(7) C18 0.0209(7) 0.0220(8) 0.0209(8) 0.0000(6) 0.0081(6) -0.0016(6) C19 0.0387(13) 0.0560(16) 0.088(2) 0.0083(14) 0.0272(13) 0.0063(11) C20 0.0443(17) 0.150(4) 0.120(3) 0.052(3) -0.0145(19) 0.007(2) C21 0.0563(16) 0.0633(18) 0.114(3) -0.0154(17) 0.0579(18) -0.0098(13) C22 0.0320(10) 0.0342(11) 0.0523(13) 0.0063(9) 0.0187(9) 0.0053(8) C24 0.0571(15) 0.0456(14) 0.0604(16) 0.0098(12) 0.0020(12) 0.0194(12) C25 0.0414(13) 0.0363(13) 0.114(2) -0.0114(14) 0.0224(14) 0.0087(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 O4 1.7953(13) . ? Ti1 O3 1.7967(12) . ? Ti1 O2 1.9587(13) . ? Ti1 O1 1.9623(12) . ? Ti1 N2 2.2359(14) . ? Ti1 N1 2.2514(15) . ? O1 C1 1.333(2) . ? O2 C10 1.339(2) . ? O3 C19 1.402(3) . ? O4 C22 1.418(2) . ? N1 C8 1.321(2) . ? N1 C9 1.367(2) . ? N2 C17 1.322(2) . ? N2 C18 1.366(2) . ? C1 C2 1.377(3) . ? C1 C9 1.421(3) . ? C2 C3 1.411(3) . ? C3 C4 1.363(4) . ? C4 C5 1.415(3) . ? C5 C6 1.409(3) . ? C5 C9 1.415(3) . ? C6 C7 1.353(3) . ? C7 C8 1.415(3) . ? C10 C11 1.379(2) . ? C10 C18 1.420(2) . ? C11 C12 1.412(3) . ? C12 C13 1.367(3) . ? C13 C14 1.420(2) . ? C14 C15 1.412(3) . ? C14 C18 1.413(2) . ? C15 C16 1.371(3) . ? C16 C17 1.403(3) . ? C19 C20 1.472(5) . ? C19 C21 1.502(4) . ? C22 C25 1.504(3) . ? C22 C24 1.510(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 O4 Ti1 O3 102.56(6) . . ? O4 Ti1 O2 94.03(6) . . ? O3 Ti1 O2 101.62(6) . . ? O4 Ti1 O1 100.88(6) . . ? O3 Ti1 O1 94.37(6) . . ? O2 Ti1 O1 155.21(5) . . ? O4 Ti1 N2 165.97(6) . . ? O3 Ti1 N2 89.51(6) . . ? O2 Ti1 N2 76.31(5) . . ? O1 Ti1 N2 85.11(5) . . ? O4 Ti1 N1 89.65(6) . . ? O3 Ti1 N1 165.77(6) . . ? O2 Ti1 N1 84.56(5) . . ? O1 Ti1 N1 75.93(5) . . ? N2 Ti1 N1 79.43(5) . . ? C1 O1 Ti1 120.74(11) . . ? C10 O2 Ti1 120.53(10) . . ? C19 O3 Ti1 149.31(15) . . ? C22 O4 Ti1 147.02(12) . . ? C8 N1 C9 118.68(16) . . ? C8 N1 Ti1 130.50(14) . . ? C9 N1 Ti1 110.64(11) . . ? C17 N2 C18 118.25(14) . . ? C17 N2 Ti1 130.62(11) . . ? C18 N2 Ti1 110.92(10) . . ? O1 C1 C2 124.57(18) . . ? O1 C1 C9 116.92(16) . . ? C2 C1 C9 118.50(18) . . ? C1 C2 C3 119.5(2) . . ? C4 C3 C2 122.5(2) . . ? C3 C4 C5 119.8(2) . . ? C6 C5 C9 116.1(2) . . ? C6 C5 C4 126.2(2) . . ? C9 C5 C4 117.7(2) . . ? C7 C6 C5 120.38(19) . . ? C6 C7 C8 120.0(2) . . ? N1 C8 C7 121.6(2) . . ? N1 C9 C5 123.10(18) . . ? N1 C9 C1 114.98(15) . . ? C5 C9 C1 121.89(18) . . ? O2 C10 C11 124.87(16) . . ? O2 C10 C18 116.88(14) . . ? C11 C10 C18 118.25(16) . . ? C10 C11 C12 119.61(17) . . ? C13 C12 C11 122.72(17) . . ? C12 C13 C14 119.40(17) . . ? C15 C14 C18 116.82(16) . . ? C15 C14 C13 125.42(17) . . ? C18 C14 C13 117.76(16) . . ? C16 C15 C14 119.83(16) . . ? C15 C16 C17 119.26(16) . . ? N2 C17 C16 122.95(16) . . ? N2 C18 C14 122.85(15) . . ? N2 C18 C10 114.89(14) . . ? C14 C18 C10 122.26(15) . . ? O3 C19 C20 110.1(3) . . ? O3 C19 C21 109.8(2) . . ? C20 C19 C21 116.3(3) . . ? O4 C22 C25 108.92(17) . . ? O4 C22 C24 109.04(18) . . ? C25 C22 C24 112.5(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.754 _refine_diff_density_min -0.440 _refine_diff_density_rms 0.053 data_Braun10 _database_code_depnum_ccdc_archive 'CCDC 871141' #TrackingRef 'allcifs_Ti.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C46 H84 O8 Ti2' _chemical_formula_sum 'C46 H84 O8 Ti2' _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour red _diffrn_ambient_temperature 173(2) _chemical_formula_weight 860.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? 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 26.3870(6) _cell_length_b 10.8511(3) _cell_length_c 18.6970(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.0800(10) _cell_angle_gamma 90.00 _cell_volume 5214.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10903 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.097 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 0.350 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30806 _diffrn_reflns_av_R_equivalents 0.0531 _diffrn_reflns_av_sigmaI/netI 0.0563 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 27.47 _reflns_number_total 11827 _reflns_number_gt 8364 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material PLATON _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^)+(0.0725P)^2^+2.7530P] 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 11827 _refine_ls_number_parameters 529 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0880 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1594 _refine_ls_wR_factor_gt 0.1431 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.791026(15) 0.05027(4) -0.02542(2) 0.03133(12) Uani 1 1 d . . . Ti2 Ti 0.705905(15) -0.07966(4) 0.05401(2) 0.03364(12) Uani 1 1 d . . . O1 O 0.81226(6) -0.07137(15) -0.08351(9) 0.0401(4) Uani 1 1 d . . . O2 O 0.75534(6) 0.17200(16) -0.07820(9) 0.0441(4) Uani 1 1 d . . . O3 O 0.85238(6) 0.12237(16) 0.00409(9) 0.0393(4) Uani 1 1 d . . . O4 O 0.77720(6) 0.01731(15) 0.07049(8) 0.0343(4) Uani 1 1 d . . . O5 O 0.72120(6) -0.05267(16) -0.04122(8) 0.0378(4) Uani 1 1 d . . . O6 O 0.68769(7) 0.04527(16) 0.11180(10) 0.0442(4) Uani 1 1 d . . . O7 O 0.64285(6) -0.14274(18) 0.02355(10) 0.0493(5) Uani 1 1 d . . . O8 O 0.73882(7) -0.20533(16) 0.10624(10) 0.0467(4) Uani 1 1 d . . . C1 C 0.84606(9) -0.0665(2) -0.12868(12) 0.0346(5) Uani 1 1 d . . . C2 C 0.84676(10) 0.0383(2) -0.17110(14) 0.0406(6) Uani 1 1 d . . . H2 H 0.8239 0.1024 -0.1684 0.049 Uiso 1 1 calc R . . C3 C 0.88069(10) 0.0493(3) -0.21722(14) 0.0446(6) Uani 1 1 d . . . H3 H 0.8806 0.1209 -0.2446 0.053 Uiso 1 1 calc R . . C4 C 0.91476(9) -0.0448(2) -0.22320(13) 0.0392(6) Uani 1 1 d . . . C5 C 0.91312(9) -0.1496(2) -0.18114(12) 0.0358(5) Uani 1 1 d . . . H5 H 0.9360 -0.2134 -0.1846 0.043 Uiso 1 1 calc R . . C6 C 0.87937(9) -0.1654(2) -0.13398(12) 0.0330(5) Uani 1 1 d . . . C7 C 0.87844(11) -0.2864(2) -0.09197(15) 0.0456(6) Uani 1 1 d . . . C8 C 0.89071(15) -0.2632(3) -0.00910(16) 0.0698(9) Uani 1 1 d . . . H8A H 0.8651 -0.2087 0.0026 0.105 Uiso 1 1 calc R . . H8B H 0.9245 -0.2264 0.0059 0.105 Uiso 1 1 calc R . . H8C H 0.8902 -0.3400 0.0162 0.105 Uiso 1 1 calc R . . C9 C 0.82470(13) -0.3456(3) -0.1172(2) 0.0714(10) Uani 1 1 d . . . H9A H 0.7986 -0.2902 -0.1078 0.107 Uiso 1 1 calc R . . H9B H 0.8236 -0.4211 -0.0907 0.107 Uiso 1 1 calc R . . H9C H 0.8182 -0.3628 -0.1688 0.107 Uiso 1 1 calc R . . C10 C 0.91958(13) -0.3780(3) -0.10544(19) 0.0636(8) Uani 1 1 d . . . H10A H 0.9174 -0.4526 -0.0787 0.095 Uiso 1 1 calc R . . H10B H 0.9536 -0.3426 -0.0891 0.095 Uiso 1 1 calc R . . H10C H 0.9135 -0.3962 -0.1569 0.095 Uiso 1 1 calc R . . C11 C 0.95392(10) -0.0359(3) -0.27233(15) 0.0542(8) Uani 1 1 d . . . C12 C 0.94245(17) 0.0690(5) -0.3252(3) 0.122(2) Uani 1 1 d . . . H12A H 0.9459 0.1454 -0.2986 0.183 Uiso 1 1 calc R . . H12B H 0.9076 0.0614 -0.3542 0.183 Uiso 1 1 calc R . . H12C H 0.9665 0.0677 -0.3568 0.183 Uiso 1 1 calc R . . C13 C 1.00831(12) -0.0331(4) -0.22582(19) 0.0852(13) Uani 1 1 d . . . H13A H 1.0327 -0.0387 -0.2568 0.128 Uiso 1 1 calc R . . H13B H 1.0133 -0.1014 -0.1924 0.128 Uiso 1 1 calc R . . H13C H 1.0138 0.0426 -0.1986 0.128 Uiso 1 1 calc R . . C14 C 0.94973(16) -0.1552(5) -0.3208(2) 0.0995(15) Uani 1 1 d . . . H14A H 0.9148 -0.1635 -0.3496 0.149 Uiso 1 1 calc R . . H14B H 0.9584 -0.2260 -0.2896 0.149 Uiso 1 1 calc R . . H14C H 0.9734 -0.1493 -0.3528 0.149 Uiso 1 1 calc R . . C15 C 0.75863(11) 0.2951(3) -0.10263(17) 0.0560(7) Uani 1 1 d . . . H15 H 0.7954 0.3178 -0.0955 0.067 Uiso 1 1 calc R . . C16 C 0.7338(2) 0.3788(4) -0.0596(3) 0.125(2) Uani 1 1 d . . . H16A H 0.6989 0.3517 -0.0617 0.187 Uiso 1 1 calc R . . H16B H 0.7330 0.4606 -0.0795 0.187 Uiso 1 1 calc R . . H16C H 0.7531 0.3792 -0.0095 0.187 Uiso 1 1 calc R . . C17 C 0.7334(2) 0.3022(5) -0.1833(2) 0.1245(19) Uani 1 1 d . . . H17A H 0.7447 0.2340 -0.2083 0.187 Uiso 1 1 calc R . . H17B H 0.7430 0.3781 -0.2030 0.187 Uiso 1 1 calc R . . H17C H 0.6962 0.2991 -0.1898 0.187 Uiso 1 1 calc R . . C18 C 0.90332(9) 0.1730(2) 0.02401(14) 0.0431(6) Uani 1 1 d . . . H18 H 0.9112 0.1907 0.0768 0.052 Uiso 1 1 calc R . . C19 C 0.90479(13) 0.2922(3) -0.0165(2) 0.0694(9) Uani 1 1 d . . . H19A H 0.8971 0.2766 -0.0684 0.104 Uiso 1 1 calc R . . H19B H 0.9388 0.3282 -0.0017 0.104 Uiso 1 1 calc R . . H19C H 0.8794 0.3479 -0.0053 0.104 Uiso 1 1 calc R . . C20 C 0.94268(10) 0.0810(3) 0.00939(18) 0.0584(8) Uani 1 1 d . . . H20A H 0.9395 0.0056 0.0348 0.088 Uiso 1 1 calc R . . H20B H 0.9771 0.1138 0.0265 0.088 Uiso 1 1 calc R . . H20C H 0.9365 0.0653 -0.0424 0.088 Uiso 1 1 calc R . . C21 C 0.80752(10) 0.0295(3) 0.14507(13) 0.0498(7) Uani 1 1 d . . . H21 H 0.7861 -0.0001 0.1780 0.060 Uiso 1 1 calc R . . C22 C 0.85470(11) -0.0530(3) 0.15537(16) 0.0642(9) Uani 1 1 d . . . H22A H 0.8438 -0.1359 0.1422 0.096 Uiso 1 1 calc R . . H22B H 0.8733 -0.0507 0.2058 0.096 Uiso 1 1 calc R . . H22C H 0.8770 -0.0247 0.1247 0.096 Uiso 1 1 calc R . . C23 C 0.82010(13) 0.1626(3) 0.16314(17) 0.0699(10) Uani 1 1 d . . . H23A H 0.8423 0.1932 0.1330 0.105 Uiso 1 1 calc R . . H23B H 0.8375 0.1698 0.2139 0.105 Uiso 1 1 calc R . . H23C H 0.7885 0.2097 0.1541 0.105 Uiso 1 1 calc R . . C24 C 0.69348(11) -0.0778(3) -0.11626(15) 0.0652(10) Uani 1 1 d . . . H24 H 0.7170 -0.0582 -0.1484 0.078 Uiso 1 1 calc R . . C25 C 0.64714(12) 0.0058(5) -0.13723(18) 0.0880(13) Uani 1 1 d . . . H25A H 0.6226 -0.0135 -0.1080 0.132 Uiso 1 1 calc R . . H25B H 0.6310 -0.0055 -0.1882 0.132 Uiso 1 1 calc R . . H25C H 0.6582 0.0899 -0.1288 0.132 Uiso 1 1 calc R . . C26 C 0.68090(15) -0.2123(4) -0.1251(2) 0.1032(17) Uani 1 1 d . . . H26A H 0.7119 -0.2596 -0.1072 0.155 Uiso 1 1 calc R . . H26B H 0.6673 -0.2304 -0.1761 0.155 Uiso 1 1 calc R . . H26C H 0.6554 -0.2329 -0.0977 0.155 Uiso 1 1 calc R . . C27 C 0.65122(9) 0.0558(2) 0.15302(13) 0.0357(5) Uani 1 1 d . . . C28 C 0.64721(11) -0.0365(2) 0.20193(16) 0.0484(6) Uani 1 1 d . . . H28 H 0.6689 -0.1049 0.2054 0.058 Uiso 1 1 calc R . . C29 C 0.61143(10) -0.0298(3) 0.24646(15) 0.0478(6) Uani 1 1 d . . . H29 H 0.6093 -0.0938 0.2787 0.057 Uiso 1 1 calc R . . C30 C 0.57928(9) 0.0707(2) 0.24297(13) 0.0373(5) Uani 1 1 d . . . C31 C 0.58391(9) 0.1619(2) 0.19304(13) 0.0375(5) Uani 1 1 d . . . H31 H 0.5619 0.2296 0.1896 0.045 Uiso 1 1 calc R . . C32 C 0.61914(9) 0.1600(2) 0.14758(13) 0.0356(5) Uani 1 1 d . . . C33 C 0.53944(10) 0.0848(3) 0.29104(15) 0.0466(6) Uani 1 1 d . . . C34 C 0.54666(15) -0.0118(4) 0.3512(2) 0.0807(11) Uani 1 1 d . . . H34A H 0.5211 0.0003 0.3799 0.121 Uiso 1 1 calc R . . H34B H 0.5809 -0.0044 0.3823 0.121 Uiso 1 1 calc R . . H34C H 0.5425 -0.0924 0.3296 0.121 Uiso 1 1 calc R . . C35 C 0.48453(11) 0.0762(4) 0.24258(19) 0.0735(10) Uani 1 1 d . . . H35A H 0.4795 -0.0039 0.2202 0.110 Uiso 1 1 calc R . . H35B H 0.4801 0.1382 0.2050 0.110 Uiso 1 1 calc R . . H35C H 0.4595 0.0887 0.2720 0.110 Uiso 1 1 calc R . . C36 C 0.54562(14) 0.2124(3) 0.32763(19) 0.0723(10) Uani 1 1 d . . . H36A H 0.5222 0.2195 0.3599 0.108 Uiso 1 1 calc R . . H36B H 0.5378 0.2751 0.2906 0.108 Uiso 1 1 calc R . . H36C H 0.5808 0.2224 0.3553 0.108 Uiso 1 1 calc R . . C37 C 0.62312(12) 0.2679(3) 0.09625(16) 0.0529(7) Uani 1 1 d . . . C38 C 0.61313(15) 0.2246(4) 0.01653(17) 0.0759(10) Uani 1 1 d . . . H38A H 0.6396 0.1670 0.0112 0.114 Uiso 1 1 calc R . . H38B H 0.6138 0.2942 -0.0149 0.114 Uiso 1 1 calc R . . H38C H 0.5797 0.1855 0.0033 0.114 Uiso 1 1 calc R . . C39 C 0.67695(14) 0.3253(3) 0.1181(2) 0.0749(10) Uani 1 1 d . . . H39A H 0.6835 0.3509 0.1685 0.112 Uiso 1 1 calc R . . H39B H 0.6787 0.3954 0.0875 0.112 Uiso 1 1 calc R . . H39C H 0.7026 0.2657 0.1122 0.112 Uiso 1 1 calc R . . C40 C 0.58197(18) 0.3667(3) 0.0988(3) 0.1059(17) Uani 1 1 d . . . H40A H 0.5480 0.3297 0.0877 0.159 Uiso 1 1 calc R . . H40B H 0.5836 0.4297 0.0634 0.159 Uiso 1 1 calc R . . H40C H 0.5885 0.4024 0.1470 0.159 Uiso 1 1 calc R . . C41 C 0.59152(12) -0.1911(4) 0.0061(3) 0.0820(11) Uani 1 1 d . . . H41 H 0.5862 -0.2234 -0.0440 0.098 Uiso 1 1 calc R . . C42 C 0.55287(14) -0.0979(4) 0.0037(4) 0.124(2) Uani 1 1 d . . . H42A H 0.5572 -0.0610 0.0513 0.185 Uiso 1 1 calc R . . H42B H 0.5189 -0.1343 -0.0104 0.185 Uiso 1 1 calc R . . H42C H 0.5566 -0.0360 -0.0314 0.185 Uiso 1 1 calc R . . C43 C 0.58790(15) -0.2968(4) 0.0527(4) 0.135(2) Uani 1 1 d . . . H43A H 0.6104 -0.3611 0.0431 0.203 Uiso 1 1 calc R . . H43B H 0.5527 -0.3262 0.0424 0.203 Uiso 1 1 calc R . . H43C H 0.5982 -0.2727 0.1033 0.203 Uiso 1 1 calc R . . C44 C 0.73760(11) -0.3330(3) 0.12244(16) 0.0492(6) Uani 1 1 d . . . H44 H 0.7062 -0.3683 0.0908 0.059 Uiso 1 1 calc R . . C45 C 0.7346(2) -0.3521(4) 0.2003(2) 0.1045(16) Uani 1 1 d . . . H45A H 0.7621 -0.3072 0.2320 0.157 Uiso 1 1 calc R . . H45B H 0.7381 -0.4383 0.2119 0.157 Uiso 1 1 calc R . . H45C H 0.7016 -0.3231 0.2070 0.157 Uiso 1 1 calc R . . C46 C 0.78366(17) -0.3966(4) 0.1057(3) 0.1029(15) Uani 1 1 d . . . H46A H 0.7849 -0.3812 0.0556 0.154 Uiso 1 1 calc R . . H46B H 0.7809 -0.4837 0.1132 0.154 Uiso 1 1 calc R . . H46C H 0.8148 -0.3660 0.1377 0.154 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 0.0247(2) 0.0358(2) 0.0336(2) -0.00440(17) 0.00682(16) -0.00141(16) Ti2 0.0252(2) 0.0362(2) 0.0409(2) -0.00674(18) 0.01042(17) -0.00302(17) O1 0.0382(9) 0.0421(10) 0.0456(10) -0.0056(8) 0.0212(8) -0.0029(7) O2 0.0390(9) 0.0456(10) 0.0456(10) 0.0029(8) 0.0049(7) 0.0033(8) O3 0.0282(8) 0.0475(10) 0.0418(9) -0.0021(8) 0.0075(7) -0.0067(7) O4 0.0274(8) 0.0439(9) 0.0310(8) -0.0065(7) 0.0050(6) -0.0065(7) O5 0.0270(8) 0.0511(10) 0.0342(8) -0.0128(7) 0.0047(6) -0.0076(7) O6 0.0396(10) 0.0436(10) 0.0556(11) -0.0080(8) 0.0240(8) -0.0022(8) O7 0.0297(9) 0.0553(12) 0.0638(12) -0.0091(9) 0.0122(8) -0.0121(8) O8 0.0434(10) 0.0393(10) 0.0574(11) 0.0027(8) 0.0113(8) -0.0014(8) C1 0.0302(12) 0.0405(13) 0.0343(12) -0.0058(10) 0.0103(9) -0.0043(10) C2 0.0384(13) 0.0386(13) 0.0451(14) 0.0023(11) 0.0104(11) 0.0036(11) C3 0.0442(14) 0.0467(15) 0.0414(14) 0.0128(11) 0.0069(11) -0.0025(12) C4 0.0314(12) 0.0531(15) 0.0326(12) 0.0071(11) 0.0063(9) -0.0056(11) C5 0.0320(12) 0.0418(14) 0.0354(12) 0.0016(10) 0.0111(9) 0.0009(10) C6 0.0346(12) 0.0339(12) 0.0321(11) 0.0008(9) 0.0111(9) -0.0033(10) C7 0.0529(16) 0.0386(14) 0.0532(15) 0.0075(12) 0.0285(12) 0.0025(12) C8 0.100(3) 0.065(2) 0.0508(17) 0.0224(16) 0.0310(17) 0.0204(19) C9 0.069(2) 0.0429(17) 0.110(3) 0.0093(18) 0.0372(19) -0.0132(15) C10 0.081(2) 0.0420(16) 0.078(2) 0.0183(15) 0.0407(18) 0.0152(15) C11 0.0366(14) 0.085(2) 0.0427(15) 0.0192(15) 0.0121(11) -0.0038(14) C12 0.087(3) 0.173(5) 0.128(4) 0.106(4) 0.070(3) 0.044(3) C13 0.0417(17) 0.147(4) 0.067(2) 0.015(2) 0.0122(15) -0.021(2) C14 0.093(3) 0.155(4) 0.066(2) -0.031(3) 0.051(2) -0.030(3) C15 0.0469(16) 0.0555(18) 0.0679(18) 0.0190(15) 0.0176(14) 0.0033(13) C16 0.198(5) 0.045(2) 0.167(5) 0.005(3) 0.119(4) 0.007(3) C17 0.140(4) 0.147(5) 0.080(3) 0.055(3) 0.010(3) 0.061(4) C18 0.0281(12) 0.0523(16) 0.0462(14) -0.0034(12) 0.0027(10) -0.0099(11) C19 0.0540(18) 0.063(2) 0.086(2) 0.0180(18) 0.0042(16) -0.0197(16) C20 0.0318(14) 0.073(2) 0.0699(19) -0.0098(16) 0.0098(13) -0.0052(13) C21 0.0373(14) 0.078(2) 0.0322(13) -0.0069(13) 0.0047(10) -0.0158(13) C22 0.0399(15) 0.098(3) 0.0477(16) 0.0135(16) -0.0044(12) -0.0089(16) C23 0.0597(19) 0.092(3) 0.0589(18) -0.0365(18) 0.0154(15) -0.0280(18) C24 0.0409(15) 0.116(3) 0.0392(15) -0.0328(16) 0.0098(12) -0.0288(17) C25 0.0406(17) 0.161(4) 0.0526(19) 0.006(2) -0.0100(14) -0.016(2) C26 0.078(3) 0.134(4) 0.109(3) -0.087(3) 0.046(2) -0.059(3) C27 0.0321(12) 0.0379(13) 0.0396(13) -0.0062(10) 0.0134(10) -0.0032(10) C28 0.0473(15) 0.0387(14) 0.0629(17) 0.0087(13) 0.0202(13) 0.0105(12) C29 0.0480(15) 0.0441(15) 0.0540(16) 0.0145(12) 0.0174(12) 0.0015(12) C30 0.0330(12) 0.0417(14) 0.0382(13) 0.0021(10) 0.0098(10) -0.0069(10) C31 0.0379(13) 0.0333(13) 0.0436(13) -0.0002(10) 0.0141(10) 0.0035(10) C32 0.0386(13) 0.0309(12) 0.0397(12) 0.0009(10) 0.0142(10) -0.0015(10) C33 0.0367(14) 0.0606(18) 0.0459(14) 0.0014(13) 0.0163(11) -0.0080(12) C34 0.082(2) 0.098(3) 0.076(2) 0.026(2) 0.0466(19) 0.004(2) C35 0.0402(16) 0.108(3) 0.075(2) -0.009(2) 0.0194(15) -0.0156(17) C36 0.077(2) 0.085(2) 0.066(2) -0.0212(18) 0.0397(17) -0.0118(19) C37 0.0620(18) 0.0415(15) 0.0652(18) 0.0134(13) 0.0353(14) 0.0040(13) C38 0.086(2) 0.089(3) 0.0547(18) 0.0247(18) 0.0209(17) -0.002(2) C39 0.094(3) 0.0502(19) 0.089(2) 0.0069(17) 0.039(2) -0.0255(18) C40 0.128(4) 0.059(2) 0.158(4) 0.062(3) 0.089(3) 0.042(2) C41 0.0366(17) 0.079(3) 0.130(3) -0.007(2) 0.0176(18) -0.0198(17) C42 0.0357(19) 0.094(3) 0.238(6) 0.012(4) 0.026(3) -0.001(2) C43 0.051(2) 0.090(3) 0.259(7) 0.062(4) 0.023(3) -0.021(2) C44 0.0451(15) 0.0425(15) 0.0587(17) 0.0022(13) 0.0090(12) -0.0010(12) C45 0.192(5) 0.059(2) 0.067(2) 0.0147(19) 0.037(3) 0.023(3) C46 0.106(3) 0.059(2) 0.161(4) 0.003(3) 0.068(3) 0.015(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O3 1.7700(15) . ? Ti1 O2 1.7846(17) . ? Ti1 O1 1.8739(16) . ? Ti1 O4 1.9423(15) . ? Ti1 O5 2.1174(16) . ? Ti1 Ti2 3.2785(6) . ? Ti2 O7 1.7699(17) . ? Ti2 O8 1.7843(18) . ? Ti2 O6 1.8630(17) . ? Ti2 O5 1.9351(16) . ? Ti2 O4 2.1164(15) . ? O1 C1 1.361(3) . ? O2 C15 1.421(3) . ? O3 C18 1.421(3) . ? O4 C21 1.448(3) . ? O5 C24 1.454(3) . ? O6 C27 1.367(3) . ? O7 C41 1.420(3) . ? O8 C44 1.420(3) . ? C1 C2 1.389(3) . ? C1 C6 1.404(3) . ? C2 C3 1.381(4) . ? C2 H2 0.9300 . ? C3 C4 1.381(4) . ? C3 H3 0.9300 . ? C4 C5 1.389(3) . ? C4 C11 1.533(3) . ? C5 C6 1.398(3) . ? C5 H5 0.9300 . ? C6 C7 1.533(3) . ? C7 C8 1.530(4) . ? C7 C9 1.531(4) . ? C7 C10 1.535(4) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.493(5) . ? C11 C13 1.501(4) . ? C11 C14 1.570(5) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.463(5) . ? C15 C17 1.506(5) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.504(4) . ? C18 C20 1.509(4) . ? C18 H18 0.9800 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C23 1.503(4) . ? C21 C22 1.510(4) . ? C21 H21 0.9800 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C26 1.497(5) . ? C24 C25 1.502(5) . ? C24 H24 0.9800 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.376(4) . ? C27 C32 1.403(3) . ? C28 C29 1.395(4) . ? C28 H28 0.9300 . ? C29 C30 1.374(4) . ? C29 H29 0.9300 . ? C30 C31 1.385(3) . ? C30 C33 1.537(3) . ? C31 C32 1.394(3) . ? C31 H31 0.9300 . ? C32 C37 1.532(3) . ? C33 C34 1.518(4) . ? C33 C35 1.528(4) . ? C33 C36 1.537(4) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C39 1.520(4) . ? C37 C38 1.528(4) . ? C37 C40 1.535(4) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C42 1.429(5) . ? C41 C43 1.456(6) . ? C41 H41 0.9800 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 C45 1.490(5) . ? C44 C46 1.491(5) . ? C44 H44 0.9800 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ti1 O2 100.14(8) . . ? O3 Ti1 O1 96.87(8) . . ? O2 Ti1 O1 112.98(8) . . ? O3 Ti1 O4 98.24(7) . . ? O2 Ti1 O4 117.45(8) . . ? O1 Ti1 O4 123.28(7) . . ? O3 Ti1 O5 169.19(7) . . ? O2 Ti1 O5 88.84(7) . . ? O1 Ti1 O5 84.98(7) . . ? O4 Ti1 O5 72.08(6) . . ? O3 Ti1 Ti2 136.13(6) . . ? O2 Ti1 Ti2 103.83(6) . . ? O1 Ti1 Ti2 106.56(5) . . ? O4 Ti1 Ti2 37.96(4) . . ? O5 Ti1 Ti2 34.17(4) . . ? O7 Ti2 O8 100.73(9) . . ? O7 Ti2 O6 96.95(8) . . ? O8 Ti2 O6 113.34(9) . . ? O7 Ti2 O5 97.99(8) . . ? O8 Ti2 O5 116.25(8) . . ? O6 Ti2 O5 123.95(8) . . ? O7 Ti2 O4 168.27(8) . . ? O8 Ti2 O4 89.64(7) . . ? O6 Ti2 O4 83.76(7) . . ? O5 Ti2 O4 72.24(6) . . ? O7 Ti2 Ti1 135.32(6) . . ? O8 Ti2 Ti1 106.15(6) . . ? O6 Ti2 Ti1 104.06(5) . . ? O5 Ti2 Ti1 37.92(4) . . ? O4 Ti2 Ti1 34.36(4) . . ? C1 O1 Ti1 131.02(15) . . ? C15 O2 Ti1 144.17(17) . . ? C18 O3 Ti1 175.12(17) . . ? C21 O4 Ti1 133.94(14) . . ? C21 O4 Ti2 117.69(14) . . ? Ti1 O4 Ti2 107.68(7) . . ? C24 O5 Ti2 134.06(15) . . ? C24 O5 Ti1 117.75(15) . . ? Ti2 O5 Ti1 107.91(7) . . ? C27 O6 Ti2 133.99(15) . . ? C41 O7 Ti2 174.4(2) . . ? C44 O8 Ti2 146.16(17) . . ? O1 C1 C2 118.8(2) . . ? O1 C1 C6 121.5(2) . . ? C2 C1 C6 119.7(2) . . ? C3 C2 C1 121.4(2) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C4 C3 C2 120.8(2) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 117.1(2) . . ? C3 C4 C11 122.8(2) . . ? C5 C4 C11 120.2(2) . . ? C4 C5 C6 124.3(2) . . ? C4 C5 H5 117.9 . . ? C6 C5 H5 117.9 . . ? C5 C6 C1 116.7(2) . . ? C5 C6 C7 121.0(2) . . ? C1 C6 C7 122.4(2) . . ? C8 C7 C9 110.5(3) . . ? C8 C7 C6 110.7(2) . . ? C9 C7 C6 108.9(2) . . ? C8 C7 C10 106.1(2) . . ? C9 C7 C10 108.5(3) . . ? C6 C7 C10 112.1(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C13 113.1(3) . . ? C12 C11 C4 112.4(3) . . ? C13 C11 C4 109.9(2) . . ? C12 C11 C14 105.6(3) . . ? C13 C11 C14 106.5(3) . . ? C4 C11 C14 108.9(2) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O2 C15 C16 109.9(3) . . ? O2 C15 C17 108.9(3) . . ? C16 C15 C17 111.5(4) . . ? O2 C15 H15 108.8 . . ? C16 C15 H15 108.8 . . ? C17 C15 H15 108.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O3 C18 C19 109.3(2) . . ? O3 C18 C20 110.3(2) . . ? C19 C18 C20 112.3(3) . . ? O3 C18 H18 108.3 . . ? C19 C18 H18 108.3 . . ? C20 C18 H18 108.3 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O4 C21 C23 110.5(2) . . ? O4 C21 C22 109.2(2) . . ? C23 C21 C22 114.0(2) . . ? O4 C21 H21 107.6 . . ? C23 C21 H21 107.6 . . ? C22 C21 H21 107.6 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O5 C24 C26 109.9(3) . . ? O5 C24 C25 109.9(2) . . ? C26 C24 C25 114.4(3) . . ? O5 C24 H24 107.5 . . ? C26 C24 H24 107.5 . . ? C25 C24 H24 107.5 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O6 C27 C28 118.9(2) . . ? O6 C27 C32 121.1(2) . . ? C28 C27 C32 119.9(2) . . ? C27 C28 C29 121.5(2) . . ? C27 C28 H28 119.2 . . ? C29 C28 H28 119.2 . . ? C30 C29 C28 120.5(2) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C30 C31 116.8(2) . . ? C29 C30 C33 123.2(2) . . ? C31 C30 C33 119.9(2) . . ? C30 C31 C32 125.0(2) . . ? C30 C31 H31 117.5 . . ? C32 C31 H31 117.5 . . ? C31 C32 C27 116.2(2) . . ? C31 C32 C37 121.3(2) . . ? C27 C32 C37 122.4(2) . . ? C34 C33 C35 109.9(3) . . ? C34 C33 C36 108.0(3) . . ? C35 C33 C36 108.1(3) . . ? C34 C33 C30 112.1(2) . . ? C35 C33 C30 109.2(2) . . ? C36 C33 C30 109.4(2) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C39 C37 C38 109.4(3) . . ? C39 C37 C32 109.7(2) . . ? C38 C37 C32 110.8(2) . . ? C39 C37 C40 109.3(3) . . ? C38 C37 C40 106.2(3) . . ? C32 C37 C40 111.4(2) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O7 C41 C42 112.5(3) . . ? O7 C41 C43 110.0(3) . . ? C42 C41 C43 115.6(4) . . ? O7 C41 H41 106.0 . . ? C42 C41 H41 106.0 . . ? C43 C41 H41 106.0 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O8 C44 C45 110.7(3) . . ? O8 C44 C46 110.4(3) . . ? C45 C44 C46 111.5(3) . . ? O8 C44 H44 108.0 . . ? C45 C44 H44 108.0 . . ? C46 C44 H44 108.0 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.610 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.061 data_Braun11 _database_code_depnum_ccdc_archive 'CCDC 871142' #TrackingRef 'allcifs_Ti.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C58 H74 O4 P2 Ti' _chemical_formula_sum 'C58 H74 O4 P2 Ti' _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour yellow _diffrn_ambient_temperature 173(2) _chemical_formula_weight 944.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ti Ti 0.2780 0.4460 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1020 0.0940 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? 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 23.0760(8) _cell_length_b 13.0154(6) _cell_length_c 19.6086(9) _cell_angle_alpha 90.00 _cell_angle_beta 111.386(2) _cell_angle_gamma 90.00 _cell_volume 5483.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 24450 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.144 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 0.257 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38952 _diffrn_reflns_av_R_equivalents 0.1881 _diffrn_reflns_av_sigmaI/netI 0.2463 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.47 _reflns_number_total 12524 _reflns_number_gt 6404 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material PLATON _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. Answers to Checkcif ALERTS level B: RINTA01_ALERT_3_B The value of Rint is greater than 0.18 the crystals were of bad quality. Attempts to obtain crystals of higher quality failed. PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) 5.00 Ratio PLAT222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) 4.36 Ratio As expected, the isopropyl groups show much higher thermal motion then the rigid aromatic moieties. ; _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^)+(0.0715P)^2^+5.9272P] 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 12524 _refine_ls_number_parameters 602 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2354 _refine_ls_R_factor_gt 0.1222 _refine_ls_wR_factor_ref 0.2297 _refine_ls_wR_factor_gt 0.1933 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.33605(4) -0.01540(7) 0.26820(5) 0.0229(2) Uani 1 1 d . . . O1 O 0.26239(14) -0.0915(3) 0.20250(17) 0.0269(8) Uani 1 1 d . . . O2 O 0.30868(14) -0.0311(3) 0.34660(17) 0.0259(8) Uani 1 1 d . . . O3 O 0.38835(15) 0.0916(3) 0.30041(19) 0.0342(9) Uani 1 1 d . . . O4 O 0.39016(15) -0.1174(3) 0.28089(19) 0.0349(9) Uani 1 1 d . . . P1 P 0.32441(6) 0.03337(11) 0.13544(7) 0.0245(3) Uani 1 1 d . . . P2 P 0.24337(6) 0.13826(11) 0.25672(7) 0.0242(3) Uani 1 1 d . . . C1 C 0.2522(2) -0.0298(4) 0.0848(2) 0.0223(11) Uani 1 1 d . . . C2 C 0.2295(2) -0.0880(4) 0.1304(3) 0.0230(11) Uani 1 1 d . . . C3 C 0.1723(2) -0.1411(4) 0.0983(3) 0.0274(12) Uani 1 1 d . . . C4 C 0.1394(2) -0.1250(4) 0.0246(3) 0.0284(12) Uani 1 1 d . . . H11 H 0.1007 -0.1564 0.0038 0.034 Uiso 1 1 calc R . . C5 C 0.1602(2) -0.0647(4) -0.0210(3) 0.0266(12) Uani 1 1 d . . . C6 C 0.2172(2) -0.0188(4) 0.0096(3) 0.0288(12) Uani 1 1 d . . . H1 H 0.2330 0.0200 -0.0196 0.035 Uiso 1 1 calc R . . C7 C 0.1177(2) -0.0500(5) -0.1025(3) 0.0387(15) Uani 1 1 d . . . C8 C 0.0959(3) -0.1549(5) -0.1386(3) 0.0457(16) Uani 1 1 d . . . H2 H 0.0732 -0.1455 -0.1901 0.059 Uiso 1 1 calc R . . H3 H 0.0694 -0.1867 -0.1167 0.059 Uiso 1 1 calc R . . H4 H 0.1314 -0.1979 -0.1316 0.059 Uiso 1 1 calc R . . C9 C 0.0606(3) 0.0134(5) -0.1058(3) 0.0524(17) Uani 1 1 d . . . H5 H 0.0739 0.0794 -0.0837 0.068 Uiso 1 1 calc R . . H6 H 0.0386 -0.0219 -0.0797 0.068 Uiso 1 1 calc R . . H7 H 0.0337 0.0224 -0.1559 0.068 Uiso 1 1 calc R . . C10 C 0.1514(3) 0.0056(6) -0.1460(3) 0.059(2) Uani 1 1 d . . . H8 H 0.1241 0.0111 -0.1963 0.077 Uiso 1 1 calc R . . H9 H 0.1878 -0.0326 -0.1429 0.077 Uiso 1 1 calc R . . H10 H 0.1633 0.0730 -0.1260 0.077 Uiso 1 1 calc R . . C11 C 0.1477(2) -0.2096(4) 0.1461(3) 0.0299(13) Uani 1 1 d . . . C12 C 0.0860(2) -0.2621(5) 0.0995(3) 0.0473(17) Uani 1 1 d . . . H12 H 0.0916 -0.2991 0.0600 0.062 Uiso 1 1 calc R . . H13 H 0.0543 -0.2109 0.0800 0.062 Uiso 1 1 calc R . . H14 H 0.0738 -0.3090 0.1296 0.062 Uiso 1 1 calc R . . C13 C 0.1945(3) -0.2949(5) 0.1822(3) 0.0459(16) Uani 1 1 d . . . H15 H 0.2011 -0.3360 0.1450 0.060 Uiso 1 1 calc R . . H16 H 0.1785 -0.3373 0.2114 0.060 Uiso 1 1 calc R . . H17 H 0.2332 -0.2648 0.2128 0.060 Uiso 1 1 calc R . . C14 C 0.1348(3) -0.1460(5) 0.2052(3) 0.0453(16) Uani 1 1 d . . . H18 H 0.1175 -0.1896 0.2323 0.059 Uiso 1 1 calc R . . H19 H 0.1059 -0.0920 0.1823 0.059 Uiso 1 1 calc R . . H20 H 0.1730 -0.1166 0.2378 0.059 Uiso 1 1 calc R . . C15 C 0.3872(2) -0.0193(4) 0.1100(3) 0.0267(12) Uani 1 1 d . . . C16 C 0.4474(2) -0.0172(5) 0.1627(3) 0.0416(15) Uani 1 1 d . . . H25 H 0.4539 0.0077 0.2094 0.050 Uiso 1 1 calc R . . C17 C 0.4973(3) -0.0519(5) 0.1460(3) 0.0471(17) Uani 1 1 d . . . H24 H 0.5373 -0.0498 0.1813 0.056 Uiso 1 1 calc R . . C18 C 0.4880(3) -0.0894(5) 0.0772(3) 0.0440(16) Uani 1 1 d . . . H23 H 0.5216 -0.1111 0.0654 0.053 Uiso 1 1 calc R . . C19 C 0.4286(3) -0.0944(4) 0.0262(3) 0.0411(15) Uani 1 1 d . . . H22 H 0.4222 -0.1218 -0.0198 0.049 Uiso 1 1 calc R . . C20 C 0.3784(2) -0.0598(4) 0.0416(3) 0.0307(13) Uani 1 1 d . . . H21 H 0.3386 -0.0637 0.0061 0.037 Uiso 1 1 calc R . . C21 C 0.3185(2) 0.1665(4) 0.1039(3) 0.0264(12) Uani 1 1 d . . . C22 C 0.2618(2) 0.2154(5) 0.0715(3) 0.0339(13) Uani 1 1 d . . . H30 H 0.2253 0.1785 0.0628 0.041 Uiso 1 1 calc R . . C23 C 0.2584(3) 0.3171(5) 0.0520(3) 0.0455(16) Uani 1 1 d . . . H29 H 0.2198 0.3481 0.0290 0.055 Uiso 1 1 calc R . . C24 C 0.3116(3) 0.3725(5) 0.0663(4) 0.0597(19) Uani 1 1 d . . . H28 H 0.3094 0.4415 0.0533 0.072 Uiso 1 1 calc R . . C25 C 0.3687(3) 0.3265(6) 0.1000(4) 0.073(2) Uani 1 1 d . . . H27 H 0.4049 0.3648 0.1106 0.088 Uiso 1 1 calc R . . C26 C 0.3723(3) 0.2230(5) 0.1181(4) 0.0523(18) Uani 1 1 d . . . H26 H 0.4109 0.1917 0.1399 0.063 Uiso 1 1 calc R . . C27 C 0.2202(2) 0.0731(4) 0.3255(3) 0.0240(12) Uani 1 1 d . . . C28 C 0.2584(2) -0.0075(4) 0.3624(3) 0.0241(12) Uani 1 1 d . . . C29 C 0.2437(2) -0.0655(4) 0.4153(2) 0.0247(12) Uani 1 1 d . . . C30 C 0.1891(2) -0.0380(4) 0.4257(3) 0.0271(12) Uani 1 1 d . . . H41 H 0.1786 -0.0749 0.4602 0.033 Uiso 1 1 calc R . . C31 C 0.1493(2) 0.0400(4) 0.3885(3) 0.0287(12) Uani 1 1 d . . . C32 C 0.1661(2) 0.0966(4) 0.3380(3) 0.0289(12) Uani 1 1 d . . . H31 H 0.1409 0.1504 0.3126 0.035 Uiso 1 1 calc R . . C33 C 0.0876(2) 0.0632(5) 0.3979(3) 0.0390(15) Uani 1 1 d . . . C34 C 0.0822(3) 0.1780(5) 0.4112(4) 0.059(2) Uani 1 1 d . . . H32 H 0.1155 0.1983 0.4552 0.077 Uiso 1 1 calc R . . H33 H 0.0430 0.1915 0.4161 0.077 Uiso 1 1 calc R . . H34 H 0.0847 0.2163 0.3705 0.077 Uiso 1 1 calc R . . C35 C 0.0795(3) 0.0042(6) 0.4605(4) 0.072(2) Uani 1 1 d . . . H35 H 0.0794 -0.0682 0.4511 0.094 Uiso 1 1 calc R . . H36 H 0.0407 0.0231 0.4648 0.094 Uiso 1 1 calc R . . H37 H 0.1132 0.0202 0.5053 0.094 Uiso 1 1 calc R . . C36 C 0.0349(2) 0.0324(6) 0.3274(3) 0.0587(19) Uani 1 1 d . . . H38 H 0.0391 0.0687 0.2869 0.076 Uiso 1 1 calc R . . H39 H -0.0044 0.0492 0.3311 0.076 Uiso 1 1 calc R . . H40 H 0.0368 -0.0402 0.3199 0.076 Uiso 1 1 calc R . . C37 C 0.2841(2) -0.1569(4) 0.4535(3) 0.0297(12) Uani 1 1 d . . . C38 C 0.2631(3) -0.2021(4) 0.5137(3) 0.0413(15) Uani 1 1 d . . . H42 H 0.2674 -0.1509 0.5505 0.054 Uiso 1 1 calc R . . H43 H 0.2885 -0.2605 0.5357 0.054 Uiso 1 1 calc R . . H44 H 0.2204 -0.2231 0.4924 0.054 Uiso 1 1 calc R . . C39 C 0.3533(2) -0.1284(4) 0.4916(3) 0.0374(14) Uani 1 1 d . . . H45 H 0.3689 -0.1014 0.4561 0.049 Uiso 1 1 calc R . . H46 H 0.3766 -0.1885 0.5139 0.049 Uiso 1 1 calc R . . H47 H 0.3575 -0.0774 0.5285 0.049 Uiso 1 1 calc R . . C40 C 0.2776(3) -0.2402(4) 0.3963(3) 0.0398(14) Uani 1 1 d . . . H48 H 0.2348 -0.2612 0.3749 0.052 Uiso 1 1 calc R . . H49 H 0.3029 -0.2982 0.4193 0.052 Uiso 1 1 calc R . . H50 H 0.2909 -0.2135 0.3588 0.052 Uiso 1 1 calc R . . C41 C 0.2813(2) 0.2558(4) 0.3022(3) 0.0252(12) Uani 1 1 d . . . C42 C 0.2958(2) 0.2765(4) 0.3757(3) 0.0357(14) Uani 1 1 d . . . H55 H 0.2858 0.2289 0.4051 0.043 Uiso 1 1 calc R . . C43 C 0.3248(3) 0.3667(5) 0.4059(3) 0.0468(16) Uani 1 1 d . . . H54 H 0.3346 0.3791 0.4555 0.056 Uiso 1 1 calc R . . C44 C 0.3395(3) 0.4383(5) 0.3638(3) 0.0451(16) Uani 1 1 d . . . H53 H 0.3585 0.4996 0.3847 0.054 Uiso 1 1 calc R . . C45 C 0.3263(3) 0.4201(5) 0.2902(3) 0.0457(16) Uani 1 1 d . . . H52 H 0.3364 0.4685 0.2615 0.055 Uiso 1 1 calc R . . C46 C 0.2975(2) 0.3284(5) 0.2596(3) 0.0365(14) Uani 1 1 d . . . H51 H 0.2890 0.3151 0.2103 0.044 Uiso 1 1 calc R . . C47 C 0.1694(2) 0.1882(4) 0.1918(3) 0.0267(12) Uani 1 1 d . . . C48 C 0.1351(2) 0.1289(4) 0.1325(3) 0.0329(13) Uani 1 1 d . . . H60 H 0.1503 0.0653 0.1255 0.040 Uiso 1 1 calc R . . C49 C 0.0783(2) 0.1625(5) 0.0832(3) 0.0418(15) Uani 1 1 d . . . H59 H 0.0553 0.1209 0.0442 0.050 Uiso 1 1 calc R . . C50 C 0.0558(3) 0.2586(5) 0.0922(3) 0.0482(17) Uani 1 1 d . . . H58 H 0.0180 0.2822 0.0588 0.058 Uiso 1 1 calc R . . C51 C 0.0895(3) 0.3174(5) 0.1502(3) 0.0546(18) Uani 1 1 d . . . H57 H 0.0746 0.3816 0.1566 0.066 Uiso 1 1 calc R . . C52 C 0.1458(2) 0.2831(5) 0.2000(3) 0.0418(15) Uani 1 1 d . . . H56 H 0.1681 0.3244 0.2395 0.050 Uiso 1 1 calc R . . C53 C 0.4360(3) 0.1465(6) 0.3533(3) 0.063(2) Uani 1 1 d . . . H67 H 0.4210 0.2175 0.3479 0.076 Uiso 1 1 calc R . . C54 C 0.4438(3) 0.1187(6) 0.4282(3) 0.073(2) Uani 1 1 d . . . H61 H 0.4039 0.1187 0.4333 0.095 Uiso 1 1 calc R . . H62 H 0.4706 0.1676 0.4616 0.095 Uiso 1 1 calc R . . H63 H 0.4618 0.0514 0.4391 0.095 Uiso 1 1 calc R . . C55 C 0.4920(3) 0.1506(7) 0.3361(4) 0.087(3) Uani 1 1 d . . . H64 H 0.5093 0.0829 0.3394 0.113 Uiso 1 1 calc R . . H65 H 0.5218 0.1952 0.3702 0.113 Uiso 1 1 calc R . . H66 H 0.4820 0.1766 0.2873 0.113 Uiso 1 1 calc R . . C56 C 0.4153(5) -0.2149(6) 0.2845(4) 0.102(3) Uani 1 1 d . . . H74 H 0.4501 -0.1995 0.2688 0.122 Uiso 1 1 calc R . . C57 C 0.3801(4) -0.2829(7) 0.2270(6) 0.111(4) Uani 1 1 d . . . H68 H 0.3692 -0.2484 0.1807 0.144 Uiso 1 1 calc R . . H69 H 0.3429 -0.3034 0.2345 0.144 Uiso 1 1 calc R . . H70 H 0.4046 -0.3426 0.2272 0.144 Uiso 1 1 calc R . . C58 C 0.4489(4) -0.2498(7) 0.3576(5) 0.105(3) Uani 1 1 d . . . H71 H 0.4787 -0.1986 0.3837 0.136 Uiso 1 1 calc R . . H72 H 0.4701 -0.3126 0.3559 0.136 Uiso 1 1 calc R . . H73 H 0.4203 -0.2616 0.3822 0.136 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 0.0186(4) 0.0291(6) 0.0209(5) 0.0008(4) 0.0072(4) 0.0002(4) O1 0.0238(17) 0.034(2) 0.0214(19) 0.0027(16) 0.0066(15) -0.0070(16) O2 0.0263(17) 0.031(2) 0.0234(19) 0.0056(16) 0.0125(15) 0.0068(16) O3 0.0253(18) 0.039(2) 0.035(2) -0.0072(19) 0.0070(16) -0.0128(17) O4 0.035(2) 0.036(2) 0.039(2) 0.0058(18) 0.0192(18) 0.0140(18) P1 0.0208(6) 0.0305(9) 0.0228(7) -0.0009(6) 0.0089(5) -0.0034(6) P2 0.0226(7) 0.0264(8) 0.0244(7) 0.0019(6) 0.0096(6) 0.0016(6) C1 0.019(2) 0.026(3) 0.022(3) -0.002(2) 0.008(2) -0.004(2) C2 0.022(3) 0.021(3) 0.026(3) -0.003(2) 0.010(2) -0.001(2) C3 0.026(3) 0.028(3) 0.029(3) -0.001(2) 0.011(2) -0.005(2) C4 0.019(2) 0.030(3) 0.033(3) -0.005(3) 0.006(2) -0.006(2) C5 0.024(3) 0.032(3) 0.021(3) -0.005(2) 0.004(2) -0.003(2) C6 0.030(3) 0.033(3) 0.024(3) 0.000(2) 0.011(2) -0.003(3) C7 0.033(3) 0.048(4) 0.030(3) -0.001(3) 0.006(2) -0.005(3) C8 0.049(3) 0.052(4) 0.029(3) -0.009(3) 0.006(3) -0.002(3) C9 0.044(3) 0.063(5) 0.035(4) -0.002(3) -0.004(3) 0.005(3) C10 0.052(4) 0.094(6) 0.023(3) 0.009(3) 0.005(3) -0.013(4) C11 0.027(3) 0.034(3) 0.032(3) -0.004(3) 0.014(2) -0.013(3) C12 0.036(3) 0.058(5) 0.045(4) 0.002(3) 0.011(3) -0.022(3) C13 0.051(4) 0.037(4) 0.052(4) 0.002(3) 0.022(3) -0.010(3) C14 0.048(3) 0.054(4) 0.045(4) -0.004(3) 0.030(3) -0.016(3) C15 0.029(3) 0.024(3) 0.030(3) -0.001(2) 0.014(2) -0.003(2) C16 0.028(3) 0.061(4) 0.031(3) -0.011(3) 0.006(2) -0.005(3) C17 0.028(3) 0.063(5) 0.053(4) -0.002(4) 0.018(3) 0.001(3) C18 0.032(3) 0.044(4) 0.066(4) 0.011(3) 0.029(3) 0.014(3) C19 0.050(4) 0.036(4) 0.044(4) 0.002(3) 0.025(3) 0.013(3) C20 0.033(3) 0.025(3) 0.035(3) 0.005(3) 0.012(3) 0.002(2) C21 0.031(3) 0.027(3) 0.027(3) 0.003(2) 0.016(2) -0.001(2) C22 0.031(3) 0.042(4) 0.025(3) 0.007(3) 0.006(2) 0.004(3) C23 0.046(4) 0.043(4) 0.037(4) 0.014(3) 0.003(3) 0.003(3) C24 0.064(5) 0.037(4) 0.072(5) 0.024(4) 0.018(4) -0.001(4) C25 0.049(4) 0.059(6) 0.109(7) 0.022(5) 0.027(4) -0.018(4) C26 0.031(3) 0.041(4) 0.080(5) 0.011(4) 0.014(3) -0.010(3) C27 0.022(3) 0.027(3) 0.023(3) -0.003(2) 0.008(2) -0.002(2) C28 0.019(2) 0.028(3) 0.024(3) -0.001(2) 0.007(2) -0.001(2) C29 0.022(2) 0.029(3) 0.019(3) -0.007(2) 0.003(2) -0.005(2) C30 0.027(3) 0.032(3) 0.024(3) 0.004(2) 0.012(2) -0.006(2) C31 0.023(3) 0.036(4) 0.027(3) -0.003(3) 0.010(2) 0.001(2) C32 0.027(3) 0.029(3) 0.030(3) 0.000(2) 0.010(2) 0.000(2) C33 0.026(3) 0.051(4) 0.048(4) 0.005(3) 0.022(3) 0.001(3) C34 0.043(4) 0.065(5) 0.085(5) -0.009(4) 0.043(4) 0.004(3) C35 0.050(4) 0.106(7) 0.082(5) 0.031(5) 0.052(4) 0.016(4) C36 0.026(3) 0.086(6) 0.064(4) -0.008(4) 0.016(3) -0.011(3) C37 0.036(3) 0.030(3) 0.024(3) 0.007(2) 0.011(2) 0.006(3) C38 0.056(4) 0.036(4) 0.036(3) 0.008(3) 0.023(3) 0.008(3) C39 0.039(3) 0.035(4) 0.034(3) 0.007(3) 0.009(3) 0.011(3) C40 0.052(4) 0.032(4) 0.034(3) 0.000(3) 0.015(3) -0.002(3) C41 0.020(2) 0.024(3) 0.033(3) 0.003(2) 0.011(2) 0.002(2) C42 0.043(3) 0.034(4) 0.030(3) -0.004(3) 0.013(3) -0.002(3) C43 0.059(4) 0.045(4) 0.042(4) -0.012(3) 0.026(3) -0.007(3) C44 0.048(4) 0.035(4) 0.051(4) -0.019(3) 0.017(3) -0.011(3) C45 0.047(4) 0.038(4) 0.056(4) 0.000(3) 0.023(3) -0.016(3) C46 0.034(3) 0.044(4) 0.031(3) 0.001(3) 0.012(3) -0.004(3) C47 0.021(2) 0.036(4) 0.022(3) 0.004(2) 0.007(2) 0.001(2) C48 0.028(3) 0.031(3) 0.040(3) -0.003(3) 0.013(3) 0.003(3) C49 0.025(3) 0.061(5) 0.035(3) -0.001(3) 0.005(3) -0.007(3) C50 0.029(3) 0.065(5) 0.045(4) 0.009(4) 0.007(3) 0.014(3) C51 0.049(4) 0.050(5) 0.049(4) -0.001(4) -0.001(3) 0.029(3) C52 0.041(3) 0.041(4) 0.036(3) -0.009(3) 0.006(3) 0.012(3) C53 0.042(4) 0.103(6) 0.035(4) -0.007(4) 0.003(3) -0.031(4) C54 0.063(5) 0.108(7) 0.036(4) -0.006(4) 0.002(3) -0.009(4) C55 0.046(4) 0.145(8) 0.069(5) -0.049(5) 0.022(4) -0.042(5) C56 0.186(10) 0.048(6) 0.052(5) 0.006(4) 0.020(6) 0.060(6) C57 0.076(6) 0.077(7) 0.180(10) -0.057(7) 0.047(6) -0.006(5) C58 0.087(6) 0.105(8) 0.124(8) 0.062(6) 0.039(6) 0.062(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O4 1.777(3) . ? Ti1 O3 1.800(3) . ? Ti1 O2 1.874(3) . ? Ti1 O1 1.983(3) . ? Ti1 P1 2.5967(15) . ? Ti1 P2 2.8764(15) . ? O1 C2 1.339(5) . ? O2 C28 1.342(5) . ? O3 C53 1.401(6) . ? O4 C56 1.386(8) . ? P1 C1 1.798(5) . ? P1 C21 1.828(5) . ? P1 C15 1.829(5) . ? P2 C41 1.826(5) . ? P2 C27 1.830(5) . ? P2 C47 1.837(5) . ? C1 C6 1.408(6) . ? C1 C2 1.410(6) . ? C2 C3 1.418(6) . ? C3 C4 1.382(7) . ? C3 C11 1.543(7) . ? C4 C5 1.400(7) . ? C4 H11 0.9300 . ? C5 C6 1.368(6) . ? C5 C7 1.552(7) . ? C6 H1 0.9300 . ? C7 C10 1.528(7) . ? C7 C8 1.536(8) . ? C7 C9 1.535(8) . ? C8 H2 0.9600 . ? C8 H3 0.9600 . ? C8 H4 0.9600 . ? C9 H5 0.9600 . ? C9 H6 0.9600 . ? C9 H7 0.9600 . ? C10 H8 0.9600 . ? C10 H9 0.9600 . ? C10 H10 0.9600 . ? C11 C13 1.530(8) . ? C11 C14 1.540(7) . ? C11 C12 1.542(7) . ? C12 H12 0.9600 . ? C12 H13 0.9600 . ? C12 H14 0.9600 . ? C13 H15 0.9600 . ? C13 H16 0.9600 . ? C13 H17 0.9600 . ? C14 H18 0.9600 . ? C14 H19 0.9600 . ? C14 H20 0.9600 . ? C15 C20 1.386(7) . ? C15 C16 1.396(7) . ? C16 C17 1.384(7) . ? C16 H25 0.9300 . ? C17 C18 1.375(8) . ? C17 H24 0.9300 . ? C18 C19 1.373(8) . ? C18 H23 0.9300 . ? C19 C20 1.375(7) . ? C19 H22 0.9300 . ? C20 H21 0.9300 . ? C21 C26 1.381(7) . ? C21 C22 1.383(7) . ? C22 C23 1.372(8) . ? C22 H30 0.9300 . ? C23 C24 1.363(8) . ? C23 H29 0.9300 . ? C24 C25 1.376(9) . ? C24 H28 0.9300 . ? C25 C26 1.388(9) . ? C25 H27 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.391(7) . ? C27 C32 1.392(6) . ? C28 C29 1.420(7) . ? C29 C30 1.395(6) . ? C29 C37 1.528(7) . ? C30 C31 1.384(7) . ? C30 H41 0.9300 . ? C31 C32 1.398(7) . ? C31 C33 1.532(7) . ? C32 H31 0.9300 . ? C33 C35 1.516(8) . ? C33 C36 1.525(8) . ? C33 C34 1.529(8) . ? C34 H32 0.9600 . ? C34 H33 0.9600 . ? C34 H34 0.9600 . ? C35 H35 0.9600 . ? C35 H36 0.9600 . ? C35 H37 0.9600 . ? C36 H38 0.9600 . ? C36 H39 0.9600 . ? C36 H40 0.9600 . ? C37 C40 1.528(7) . ? C37 C39 1.541(7) . ? C37 C38 1.546(7) . ? C38 H42 0.9600 . ? C38 H43 0.9600 . ? C38 H44 0.9600 . ? C39 H45 0.9600 . ? C39 H46 0.9600 . ? C39 H47 0.9600 . ? C40 H48 0.9600 . ? C40 H49 0.9600 . ? C40 H50 0.9600 . ? C41 C42 1.382(7) . ? C41 C46 1.399(7) . ? C42 C43 1.374(8) . ? C42 H55 0.9300 . ? C43 C44 1.368(8) . ? C43 H54 0.9300 . ? C44 C45 1.382(8) . ? C44 H53 0.9300 . ? C45 C46 1.391(8) . ? C45 H52 0.9300 . ? C46 H51 0.9300 . ? C47 C48 1.379(7) . ? C47 C52 1.381(7) . ? C48 C49 1.384(7) . ? C48 H60 0.9300 . ? C49 C50 1.389(8) . ? C49 H59 0.9300 . ? C50 C51 1.357(8) . ? C50 H58 0.9300 . ? C51 C52 1.384(7) . ? C51 H57 0.9300 . ? C52 H56 0.9300 . ? C53 C55 1.451(8) . ? C53 C54 1.460(8) . ? C53 H67 0.9800 . ? C54 H61 0.9600 . ? C54 H62 0.9600 . ? C54 H63 0.9600 . ? C55 H64 0.9600 . ? C55 H65 0.9600 . ? C55 H66 0.9600 . ? C56 C58 1.432(10) . ? C56 C57 1.432(10) . ? C56 H74 0.9800 . ? C57 H68 0.9600 . ? C57 H69 0.9600 . ? C57 H70 0.9600 . ? C58 H71 0.9600 . ? C58 H72 0.9600 . ? C58 H73 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Ti1 O3 100.50(17) . . ? O4 Ti1 O2 103.50(15) . . ? O3 Ti1 O2 100.37(15) . . ? O4 Ti1 O1 96.30(16) . . ? O3 Ti1 O1 157.02(16) . . ? O2 Ti1 O1 90.75(14) . . ? O4 Ti1 P1 97.68(12) . . ? O3 Ti1 P1 88.49(12) . . ? O2 Ti1 P1 155.02(11) . . ? O1 Ti1 P1 73.74(10) . . ? O4 Ti1 P2 174.26(12) . . ? O3 Ti1 P2 82.74(12) . . ? O2 Ti1 P2 71.13(10) . . ? O1 Ti1 P2 81.94(11) . . ? P1 Ti1 P2 87.10(5) . . ? C2 O1 Ti1 133.7(3) . . ? C28 O2 Ti1 138.0(3) . . ? C53 O3 Ti1 154.0(4) . . ? C56 O4 Ti1 162.0(5) . . ? C1 P1 C21 107.9(2) . . ? C1 P1 C15 110.2(2) . . ? C21 P1 C15 103.4(2) . . ? C1 P1 Ti1 100.23(15) . . ? C21 P1 Ti1 122.59(16) . . ? C15 P1 Ti1 112.30(17) . . ? C41 P2 C27 104.2(2) . . ? C41 P2 C47 101.6(2) . . ? C27 P2 C47 103.1(2) . . ? C41 P2 Ti1 109.53(15) . . ? C27 P2 Ti1 91.64(16) . . ? C47 P2 Ti1 141.00(18) . . ? C6 C1 C2 121.1(4) . . ? C6 C1 P1 126.4(4) . . ? C2 C1 P1 112.3(3) . . ? O1 C2 C1 119.2(4) . . ? O1 C2 C3 122.0(4) . . ? C1 C2 C3 118.7(4) . . ? C4 C3 C2 117.3(4) . . ? C4 C3 C11 122.6(4) . . ? C2 C3 C11 120.0(4) . . ? C3 C4 C5 124.5(4) . . ? C3 C4 H11 117.7 . . ? C5 C4 H11 117.7 . . ? C6 C5 C4 117.7(4) . . ? C6 C5 C7 122.9(5) . . ? C4 C5 C7 119.4(4) . . ? C5 C6 C1 120.4(5) . . ? C5 C6 H1 119.8 . . ? C1 C6 H1 119.8 . . ? C10 C7 C8 108.1(5) . . ? C10 C7 C9 109.0(5) . . ? C8 C7 C9 109.0(5) . . ? C10 C7 C5 111.9(4) . . ? C8 C7 C5 110.1(5) . . ? C9 C7 C5 108.7(4) . . ? C7 C8 H2 109.5 . . ? C7 C8 H3 109.5 . . ? H2 C8 H3 109.5 . . ? C7 C8 H4 109.5 . . ? H2 C8 H4 109.5 . . ? H3 C8 H4 109.5 . . ? C7 C9 H5 109.5 . . ? C7 C9 H6 109.5 . . ? H5 C9 H6 109.5 . . ? C7 C9 H7 109.5 . . ? H5 C9 H7 109.5 . . ? H6 C9 H7 109.5 . . ? C7 C10 H8 109.5 . . ? C7 C10 H9 109.5 . . ? H8 C10 H9 109.5 . . ? C7 C10 H10 109.5 . . ? H8 C10 H10 109.5 . . ? H9 C10 H10 109.5 . . ? C13 C11 C14 109.8(5) . . ? C13 C11 C12 107.2(5) . . ? C14 C11 C12 107.1(4) . . ? C13 C11 C3 110.3(4) . . ? C14 C11 C3 111.2(4) . . ? C12 C11 C3 111.1(4) . . ? C11 C12 H12 109.5 . . ? C11 C12 H13 109.5 . . ? H12 C12 H13 109.5 . . ? C11 C12 H14 109.5 . . ? H12 C12 H14 109.5 . . ? H13 C12 H14 109.5 . . ? C11 C13 H15 109.5 . . ? C11 C13 H16 109.5 . . ? H15 C13 H16 109.5 . . ? C11 C13 H17 109.5 . . ? H15 C13 H17 109.5 . . ? H16 C13 H17 109.5 . . ? C11 C14 H18 109.5 . . ? C11 C14 H19 109.5 . . ? H18 C14 H19 109.5 . . ? C11 C14 H20 109.5 . . ? H18 C14 H20 109.5 . . ? H19 C14 H20 109.5 . . ? C20 C15 C16 118.6(5) . . ? C20 C15 P1 123.8(4) . . ? C16 C15 P1 117.6(4) . . ? C17 C16 C15 120.5(5) . . ? C17 C16 H25 119.7 . . ? C15 C16 H25 119.7 . . ? C18 C17 C16 120.2(5) . . ? C18 C17 H24 119.9 . . ? C16 C17 H24 119.9 . . ? C19 C18 C17 119.2(5) . . ? C19 C18 H23 120.4 . . ? C17 C18 H23 120.4 . . ? C18 C19 C20 121.5(5) . . ? C18 C19 H22 119.3 . . ? C20 C19 H22 119.3 . . ? C19 C20 C15 119.9(5) . . ? C19 C20 H21 120.0 . . ? C15 C20 H21 120.0 . . ? C26 C21 C22 118.5(5) . . ? C26 C21 P1 119.1(4) . . ? C22 C21 P1 122.2(4) . . ? C23 C22 C21 121.4(5) . . ? C23 C22 H30 119.3 . . ? C21 C22 H30 119.3 . . ? C24 C23 C22 119.8(6) . . ? C24 C23 H29 120.1 . . ? C22 C23 H29 120.1 . . ? C23 C24 C25 120.1(6) . . ? C23 C24 H28 119.9 . . ? C25 C24 H28 119.9 . . ? C24 C25 C26 120.2(6) . . ? C24 C25 H27 119.9 . . ? C26 C25 H27 119.9 . . ? C21 C26 C25 120.0(6) . . ? C21 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C28 C27 C32 120.8(4) . . ? C28 C27 P2 115.7(3) . . ? C32 C27 P2 123.4(4) . . ? O2 C28 C27 119.3(4) . . ? O2 C28 C29 120.2(4) . . ? C27 C28 C29 120.4(4) . . ? C30 C29 C28 116.0(4) . . ? C30 C29 C37 123.3(4) . . ? C28 C29 C37 120.5(4) . . ? C31 C30 C29 124.9(5) . . ? C31 C30 H41 117.5 . . ? C29 C30 H41 117.5 . . ? C30 C31 C32 117.3(4) . . ? C30 C31 C33 123.3(5) . . ? C32 C31 C33 119.4(5) . . ? C27 C32 C31 120.5(5) . . ? C27 C32 H31 119.8 . . ? C31 C32 H31 119.8 . . ? C35 C33 C36 107.9(5) . . ? C35 C33 C34 108.5(5) . . ? C36 C33 C34 108.9(5) . . ? C35 C33 C31 113.0(5) . . ? C36 C33 C31 107.9(4) . . ? C34 C33 C31 110.5(4) . . ? C33 C34 H32 109.5 . . ? C33 C34 H33 109.5 . . ? H32 C34 H33 109.5 . . ? C33 C34 H34 109.5 . . ? H32 C34 H34 109.5 . . ? H33 C34 H34 109.5 . . ? C33 C35 H35 109.5 . . ? C33 C35 H36 109.5 . . ? H35 C35 H36 109.5 . . ? C33 C35 H37 109.5 . . ? H35 C35 H37 109.5 . . ? H36 C35 H37 109.5 . . ? C33 C36 H38 109.5 . . ? C33 C36 H39 109.5 . . ? H38 C36 H39 109.5 . . ? C33 C36 H40 109.5 . . ? H38 C36 H40 109.5 . . ? H39 C36 H40 109.5 . . ? C29 C37 C40 108.2(4) . . ? C29 C37 C39 112.9(4) . . ? C40 C37 C39 109.5(4) . . ? C29 C37 C38 111.5(4) . . ? C40 C37 C38 108.4(4) . . ? C39 C37 C38 106.2(4) . . ? C37 C38 H42 109.5 . . ? C37 C38 H43 109.5 . . ? H42 C38 H43 109.5 . . ? C37 C38 H44 109.5 . . ? H42 C38 H44 109.5 . . ? H43 C38 H44 109.5 . . ? C37 C39 H45 109.5 . . ? C37 C39 H46 109.5 . . ? H45 C39 H46 109.5 . . ? C37 C39 H47 109.5 . . ? H45 C39 H47 109.5 . . ? H46 C39 H47 109.5 . . ? C37 C40 H48 109.5 . . ? C37 C40 H49 109.5 . . ? H48 C40 H49 109.5 . . ? C37 C40 H50 109.5 . . ? H48 C40 H50 109.5 . . ? H49 C40 H50 109.5 . . ? C42 C41 C46 118.4(5) . . ? C42 C41 P2 124.3(4) . . ? C46 C41 P2 117.3(4) . . ? C43 C42 C41 120.6(5) . . ? C43 C42 H55 119.7 . . ? C41 C42 H55 119.7 . . ? C44 C43 C42 120.8(6) . . ? C44 C43 H54 119.6 . . ? C42 C43 H54 119.6 . . ? C43 C44 C45 120.3(6) . . ? C43 C44 H53 119.9 . . ? C45 C44 H53 119.9 . . ? C44 C45 C46 119.1(6) . . ? C44 C45 H52 120.5 . . ? C46 C45 H52 120.5 . . ? C45 C46 C41 120.8(5) . . ? C45 C46 H51 119.6 . . ? C41 C46 H51 119.6 . . ? C48 C47 C52 117.9(5) . . ? C48 C47 P2 119.3(4) . . ? C52 C47 P2 122.8(4) . . ? C47 C48 C49 121.2(5) . . ? C47 C48 H60 119.4 . . ? C49 C48 H60 119.4 . . ? C48 C49 C50 119.9(6) . . ? C48 C49 H59 120.0 . . ? C50 C49 H59 120.0 . . ? C51 C50 C49 119.1(5) . . ? C51 C50 H58 120.4 . . ? C49 C50 H58 120.5 . . ? C50 C51 C52 120.9(6) . . ? C50 C51 H57 119.5 . . ? C52 C51 H57 119.5 . . ? C47 C52 C51 120.9(6) . . ? C47 C52 H56 119.5 . . ? C51 C52 H56 119.5 . . ? O3 C53 C55 111.9(5) . . ? O3 C53 C54 113.2(5) . . ? C55 C53 C54 116.8(6) . . ? O3 C53 H67 104.5 . . ? C55 C53 H67 104.5 . . ? C54 C53 H67 104.5 . . ? C53 C54 H61 109.5 . . ? C53 C54 H62 109.5 . . ? H61 C54 H62 109.5 . . ? C53 C54 H63 109.5 . . ? H61 C54 H63 109.5 . . ? H62 C54 H63 109.5 . . ? C53 C55 H64 109.5 . . ? C53 C55 H65 109.5 . . ? H64 C55 H65 109.5 . . ? C53 C55 H66 109.5 . . ? H64 C55 H66 109.5 . . ? H65 C55 H66 109.5 . . ? O4 C56 C58 114.0(7) . . ? O4 C56 C57 114.8(7) . . ? C58 C56 C57 122.4(9) . . ? O4 C56 H74 100.0 . . ? C58 C56 H74 100.0 . . ? C57 C56 H74 100.0 . . ? C56 C57 H68 109.5 . . ? C56 C57 H69 109.5 . . ? H68 C57 H69 109.5 . . ? C56 C57 H70 109.5 . . ? H68 C57 H70 109.5 . . ? H69 C57 H70 109.5 . . ? C56 C58 H71 109.5 . . ? C56 C58 H72 109.5 . . ? H71 C58 H72 109.5 . . ? C56 C58 H73 109.5 . . ? H71 C58 H73 109.5 . . ? H72 C58 H73 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.435 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.083 data_jbc _database_code_depnum_ccdc_archive 'CCDC 871143' #TrackingRef 'allcifs_Ti.cif' _audit_creation_date 10-03-06 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H52 O6 Ti' _chemical_formula_sum 'C32 H52 O6 Ti' _chemical_formula_weight 580.64 _chemical_absolute_configuration ? 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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.1940(4) _cell_length_b 13.2380(3) _cell_length_c 19.8430(8) _cell_angle_alpha 78.2420(10) _cell_angle_beta 76.0210(12) _cell_angle_gamma 85.2070(9) _cell_volume 3290.46(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11480 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.172 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 0.298 _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 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean . _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 28319 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0901 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 30.03 _reflns_number_total 19200 _reflns_number_gt 11856 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; # start Validation Reply Form _vrf_PLAT220_shelxl ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.66 Ratio RESPONSE: due to a small disorder on this isopropoxo group. ; _vrf_PLAT222_shelxl ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.59 Ratio RESPONSE: due to a small disorder on this isopropoxo group. ; # end Validation Reply Form _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^)+(0.0750P)^2^+0.4529P] 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 19200 _refine_ls_number_parameters 703 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1134 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1630 _refine_ls_wR_factor_gt 0.1374 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.22508(3) 0.24310(3) 0.575992(18) 0.02443(10) Uani 1 1 d . . . Ti2 Ti 0.74050(3) 0.73440(3) 0.021757(18) 0.02370(9) Uani 1 1 d . . . O1 O 0.86825(12) 0.76652(11) 0.06963(7) 0.0317(3) Uani 1 1 d . . . O2 O 0.82089(12) 0.82608(10) -0.05862(7) 0.0263(3) Uani 1 1 d . . . O3 O 0.80037(13) 0.61642(10) 0.00219(8) 0.0335(4) Uani 1 1 d . . . O4 O 0.62451(12) 0.74655(11) -0.01005(8) 0.0322(3) Uani 1 1 d . . . O5 O 0.69046(13) 0.88493(10) 0.06026(7) 0.0304(3) Uani 1 1 d . . . O6 O 0.67809(12) 0.67858(10) 0.12002(7) 0.0265(3) Uani 1 1 d . . . O7 O 0.21224(15) 0.09572(11) 0.65748(7) 0.0424(4) Uani 1 1 d . . . O8 O 0.15091(12) 0.29682(10) 0.65837(7) 0.0284(3) Uani 1 1 d . . . O9 O 0.11505(13) 0.20730(12) 0.55070(8) 0.0390(4) Uani 1 1 d . . . O10 O 0.26059(13) 0.36293(11) 0.52037(8) 0.0374(4) Uani 1 1 d . . . O11 O 0.36017(12) 0.25275(11) 0.62550(8) 0.0344(4) Uani 1 1 d . . . O12 O 0.32553(11) 0.15651(10) 0.52415(7) 0.0267(3) Uani 1 1 d . . . C1 C 0.93432(19) 0.85347(16) 0.03356(11) 0.0331(5) Uani 1 1 d . . . H1A H 0.9868 0.8588 0.0608 0.040 Uiso 1 1 calc . . . H1B H 0.8908 0.9182 0.0312 0.040 Uiso 1 1 calc . . . C2 C 0.98908(18) 0.84055(15) -0.03980(11) 0.0296(5) Uani 1 1 d . . . C3 C 1.09614(19) 0.84235(16) -0.06353(12) 0.0337(5) Uani 1 1 d . . . H3 H 1.1375 0.8517 -0.0323 0.040 Uiso 1 1 calc . . . C4 C 1.14505(18) 0.83087(15) -0.13187(12) 0.0323(5) Uani 1 1 d . . . C5 C 1.2624(2) 0.82540(19) -0.15662(14) 0.0454(6) Uani 1 1 d . . . H5A H 1.2866 0.7532 -0.1555 0.068 Uiso 1 1 calc . . . H5B H 1.2939 0.8551 -0.1254 0.068 Uiso 1 1 calc . . . H5C H 1.2830 0.8644 -0.2051 0.068 Uiso 1 1 calc . . . C6 C 1.08089(18) 0.82036(15) -0.17614(11) 0.0304(5) Uani 1 1 d . . . H6 H 1.1134 0.8126 -0.2231 0.037 Uiso 1 1 calc . . . C7 C 0.97151(17) 0.82038(14) -0.15607(10) 0.0260(4) Uani 1 1 d . . . C8 C 0.92509(17) 0.82834(14) -0.08492(10) 0.0256(4) Uani 1 1 d . . . C9 C 0.90517(18) 0.81136(16) -0.20807(11) 0.0309(5) Uani 1 1 d . . . C10 C 0.9721(2) 0.8076(2) -0.28254(12) 0.0479(7) Uani 1 1 d . . . H10A H 0.9266 0.8025 -0.3140 0.072 Uiso 1 1 calc . . . H10B H 1.0205 0.7474 -0.2805 0.072 Uiso 1 1 calc . . . H10C H 1.0119 0.8706 -0.3007 0.072 Uiso 1 1 calc . . . C11 C 0.8278(2) 0.90483(18) -0.21382(12) 0.0394(6) Uani 1 1 d . . . H11A H 0.7840 0.8973 -0.2458 0.059 Uiso 1 1 calc . . . H11B H 0.8668 0.9683 -0.2324 0.059 Uiso 1 1 calc . . . H11C H 0.7835 0.9083 -0.1669 0.059 Uiso 1 1 calc . . . C12 C 0.8448(2) 0.71162(17) -0.18294(12) 0.0389(6) Uani 1 1 d . . . H12A H 0.8069 0.7075 -0.1335 0.058 Uiso 1 1 calc . . . H12B H 0.8939 0.6521 -0.1868 0.058 Uiso 1 1 calc . . . H12C H 0.7950 0.7113 -0.2124 0.058 Uiso 1 1 calc . . . C13 C 0.8361(2) 0.52120(16) -0.01868(14) 0.0448(6) Uani 1 1 d . . . H13 H 0.9037 0.5321 -0.0548 0.054 Uiso 1 1 calc . . . C14 C 0.7582(3) 0.4838(2) -0.05167(15) 0.0608(9) Uani 1 1 d . . . H14A H 0.6911 0.4740 -0.0171 0.091 Uiso 1 1 calc . . . H14B H 0.7840 0.4181 -0.0662 0.091 Uiso 1 1 calc . . . H14C H 0.7489 0.5351 -0.0931 0.091 Uiso 1 1 calc . . . C15 C 0.8564(3) 0.4454(2) 0.04614(17) 0.0680(9) Uani 1 1 d . . . H15A H 0.9096 0.4722 0.0641 0.102 Uiso 1 1 calc . . . H15B H 0.8810 0.3786 0.0330 0.102 Uiso 1 1 calc . . . H15C H 0.7915 0.4366 0.0830 0.102 Uiso 1 1 calc . . . C16 C 0.54013(18) 0.72168(16) -0.03511(12) 0.0329(5) Uani 1 1 d . . . H16 H 0.5463 0.6465 -0.0370 0.039 Uiso 1 1 calc . . . C17 C 0.4385(2) 0.74265(19) 0.01534(14) 0.0447(6) Uani 1 1 d . . . H17A H 0.4379 0.7016 0.0625 0.067 Uiso 1 1 calc . . . H17B H 0.3800 0.7238 -0.0015 0.067 Uiso 1 1 calc . . . H17C H 0.4316 0.8162 0.0178 0.067 Uiso 1 1 calc . . . C18 C 0.5465(2) 0.7829(2) -0.10916(13) 0.0519(7) Uani 1 1 d . . . H18A H 0.5467 0.8568 -0.1087 0.078 Uiso 1 1 calc . . . H18B H 0.4860 0.7690 -0.1260 0.078 Uiso 1 1 calc . . . H18C H 0.6109 0.7627 -0.1408 0.078 Uiso 1 1 calc . . . C19 C 0.9212(2) 0.68311(18) 0.10758(13) 0.0413(6) Uani 1 1 d . . . H19A H 0.9721 0.6488 0.0739 0.062 Uiso 1 1 calc . . . H19B H 0.8701 0.6334 0.1374 0.062 Uiso 1 1 calc . . . H19C H 0.9575 0.7103 0.1374 0.062 Uiso 1 1 calc . . . C20 C 0.6621(2) 0.87800(15) 0.13649(11) 0.0335(5) Uani 1 1 d . . . H20A H 0.6426 0.9479 0.1472 0.040 Uiso 1 1 calc . . . H20B H 0.7234 0.8517 0.1563 0.040 Uiso 1 1 calc . . . C21 C 0.57300(19) 0.80849(15) 0.17123(10) 0.0295(5) Uani 1 1 d . . . C22 C 0.48084(19) 0.84130(15) 0.21328(11) 0.0324(5) Uani 1 1 d . . . H22 H 0.4715 0.9115 0.2184 0.039 Uiso 1 1 calc . . . C23 C 0.40269(19) 0.77314(17) 0.24775(11) 0.0338(5) Uani 1 1 d . . . C24 C 0.3029(2) 0.80685(19) 0.29513(13) 0.0434(6) Uani 1 1 d . . . H24A H 0.3152 0.8073 0.3419 0.065 Uiso 1 1 calc . . . H24B H 0.2480 0.7587 0.3000 0.065 Uiso 1 1 calc . . . H24C H 0.2811 0.8764 0.2743 0.065 Uiso 1 1 calc . . . C25 C 0.41974(18) 0.67076(16) 0.23891(11) 0.0314(5) Uani 1 1 d . . . H25 H 0.3665 0.6235 0.2630 0.038 Uiso 1 1 calc . . . C26 C 0.50975(18) 0.63351(15) 0.19710(10) 0.0279(4) Uani 1 1 d . . . C27 C 0.58845(17) 0.70542(15) 0.16146(10) 0.0261(4) Uani 1 1 d . . . C28 C 0.52675(19) 0.51889(15) 0.19235(11) 0.0330(5) Uani 1 1 d . . . C29 C 0.4297(2) 0.45604(18) 0.23186(14) 0.0517(7) Uani 1 1 d . . . H29A H 0.4133 0.4610 0.2820 0.078 Uiso 1 1 calc . . . H29B H 0.4438 0.3836 0.2273 0.078 Uiso 1 1 calc . . . H29C H 0.3702 0.4836 0.2114 0.078 Uiso 1 1 calc . . . C30 C 0.6196(2) 0.47444(17) 0.22517(13) 0.0473(7) Uani 1 1 d . . . H30A H 0.6817 0.5141 0.2006 0.071 Uiso 1 1 calc . . . H30B H 0.6334 0.4020 0.2204 0.071 Uiso 1 1 calc . . . H30C H 0.6025 0.4789 0.2754 0.071 Uiso 1 1 calc . . . C31 C 0.5493(2) 0.50398(16) 0.11527(12) 0.0385(6) Uani 1 1 d . . . H31A H 0.4858 0.5205 0.0973 0.058 Uiso 1 1 calc . . . H31B H 0.5720 0.4321 0.1130 0.058 Uiso 1 1 calc . . . H31C H 0.6046 0.5499 0.0863 0.058 Uiso 1 1 calc . . . C32 C 0.6273(2) 0.95894(17) 0.02440(13) 0.0435(6) Uani 1 1 d . . . H32A H 0.5540 0.9398 0.0410 0.065 Uiso 1 1 calc . . . H32B H 0.6498 0.9607 -0.0266 0.065 Uiso 1 1 calc . . . H32C H 0.6346 1.0273 0.0342 0.065 Uiso 1 1 calc . . . C33 C 0.1825(2) 0.10423(17) 0.73181(11) 0.0374(6) Uani 1 1 d . . . H33A H 0.2366 0.1414 0.7429 0.045 Uiso 1 1 calc . . . H33B H 0.1788 0.0342 0.7615 0.045 Uiso 1 1 calc . . . C34 C 0.08007(18) 0.15980(15) 0.74908(10) 0.0290(5) Uani 1 1 d . . . C35 C -0.00283(19) 0.11697(16) 0.80296(11) 0.0327(5) Uani 1 1 d . . . H35 H 0.0042 0.0482 0.8276 0.039 Uiso 1 1 calc . . . C36 C -0.09490(19) 0.17354(17) 0.82076(11) 0.0341(5) Uani 1 1 d . . . C37 C -0.1857(2) 0.1278(2) 0.87887(12) 0.0459(6) Uani 1 1 d . . . H37A H -0.1673 0.0563 0.8983 0.069 Uiso 1 1 calc . . . H37B H -0.2474 0.1291 0.8594 0.069 Uiso 1 1 calc . . . H37C H -0.2010 0.1684 0.9165 0.069 Uiso 1 1 calc . . . C38 C -0.10210(18) 0.27470(17) 0.78380(11) 0.0329(5) Uani 1 1 d . . . H38 H -0.1650 0.3140 0.7965 0.040 Uiso 1 1 calc . . . C39 C -0.02231(18) 0.32137(15) 0.72932(10) 0.0279(4) Uani 1 1 d . . . C40 C 0.07019(18) 0.26053(15) 0.71100(10) 0.0265(4) Uani 1 1 d . . . C41 C -0.03282(19) 0.43319(16) 0.69127(12) 0.0355(5) Uani 1 1 d . . . C42 C -0.1365(2) 0.48532(19) 0.72135(14) 0.0472(6) Uani 1 1 d . . . H42A H -0.1413 0.4877 0.7711 0.071 Uiso 1 1 calc . . . H42B H -0.1942 0.4460 0.7179 0.071 Uiso 1 1 calc . . . H42C H -0.1407 0.5557 0.6944 0.071 Uiso 1 1 calc . . . C43 C -0.0284(2) 0.43538(19) 0.61275(13) 0.0453(6) Uani 1 1 d . . . H43A H -0.0865 0.3970 0.6089 0.068 Uiso 1 1 calc . . . H43B H 0.0380 0.4035 0.5911 0.068 Uiso 1 1 calc . . . H43C H -0.0339 0.5071 0.5882 0.068 Uiso 1 1 calc . . . C44 C 0.0548(2) 0.49664(18) 0.69775(15) 0.0480(6) Uani 1 1 d . . . H44A H 0.0439 0.5691 0.6765 0.072 Uiso 1 1 calc . . . H44B H 0.1223 0.4703 0.6731 0.072 Uiso 1 1 calc . . . H44C H 0.0545 0.4912 0.7478 0.072 Uiso 1 1 calc . . . C45 C 0.0338(3) 0.1731(3) 0.5327(2) 0.1048(16) Uani 1 1 d . . . H45 H 0.0714 0.1161 0.5094 0.126 Uiso 1 1 calc . . . C46 C -0.0371(4) 0.1132(5) 0.5883(3) 0.146(2) Uani 1 1 d . . . H46A H 0.0017 0.0613 0.6160 0.218 Uiso 1 1 calc . . . H46B H -0.0830 0.0787 0.5686 0.218 Uiso 1 1 calc . . . H46C H -0.0794 0.1581 0.6189 0.218 Uiso 1 1 calc . . . C47 C 0.0021(4) 0.2354(5) 0.4728(2) 0.1222(18) Uani 1 1 d . . . H47A H -0.0387 0.2961 0.4870 0.183 Uiso 1 1 calc . . . H47B H -0.0409 0.1950 0.4549 0.183 Uiso 1 1 calc . . . H47C H 0.0640 0.2577 0.4357 0.183 Uiso 1 1 calc . . . C48 C 0.28076(19) 0.44976(16) 0.46452(11) 0.0334(5) Uani 1 1 d . . . H48 H 0.2466 0.4409 0.4264 0.040 Uiso 1 1 calc . . . C49 C 0.2334(3) 0.54543(19) 0.49292(15) 0.0555(8) Uani 1 1 d . . . H49A H 0.1578 0.5385 0.5107 0.083 Uiso 1 1 calc . . . H49B H 0.2472 0.6063 0.4549 0.083 Uiso 1 1 calc . . . H49C H 0.2647 0.5534 0.5315 0.083 Uiso 1 1 calc . . . C50 C 0.3970(2) 0.4572(2) 0.43456(14) 0.0515(7) Uani 1 1 d . . . H50A H 0.4307 0.4693 0.4709 0.077 Uiso 1 1 calc . . . H50B H 0.4104 0.5145 0.3940 0.077 Uiso 1 1 calc . . . H50C H 0.4252 0.3926 0.4193 0.077 Uiso 1 1 calc . . . C51 C 0.2234(3) -0.0017(2) 0.64391(15) 0.0786(12) Uani 1 1 d . . . H51A H 0.2861 -0.0358 0.6577 0.118 Uiso 1 1 calc . . . H51B H 0.2302 0.0013 0.5933 0.118 Uiso 1 1 calc . . . H51C H 0.1619 -0.0408 0.6710 0.118 Uiso 1 1 calc . . . C52 C 0.45420(19) 0.19152(18) 0.60458(11) 0.0358(5) Uani 1 1 d . . . H52A H 0.4404 0.1178 0.6247 0.043 Uiso 1 1 calc . . . H52B H 0.5097 0.2114 0.6247 0.043 Uiso 1 1 calc . . . C53 C 0.49285(18) 0.20423(16) 0.52575(11) 0.0298(5) Uani 1 1 d . . . C54 C 0.59348(19) 0.23409(17) 0.49081(12) 0.0356(5) Uani 1 1 d . . . H54 H 0.6389 0.2527 0.5165 0.043 Uiso 1 1 calc . . . C55 C 0.62787(19) 0.23694(17) 0.41869(12) 0.0367(5) Uani 1 1 d . . . C56 C 0.7364(2) 0.2724(2) 0.37954(14) 0.0503(7) Uani 1 1 d . . . H56A H 0.7345 0.3477 0.3646 0.075 Uiso 1 1 calc . . . H56B H 0.7602 0.2402 0.3379 0.075 Uiso 1 1 calc . . . H56C H 0.7848 0.2524 0.4109 0.075 Uiso 1 1 calc . . . C57 C 0.56085(19) 0.20562(16) 0.38338(11) 0.0323(5) Uani 1 1 d . . . H57 H 0.5855 0.2053 0.3343 0.039 Uiso 1 1 calc . . . C58 C 0.45953(17) 0.17459(14) 0.41574(10) 0.0265(4) Uani 1 1 d . . . C59 C 0.42436(17) 0.17822(15) 0.48843(10) 0.0257(4) Uani 1 1 d . . . C60 C 0.38836(19) 0.13938(16) 0.37482(11) 0.0307(5) Uani 1 1 d . . . C61 C 0.4474(2) 0.12665(19) 0.30014(12) 0.0438(6) Uani 1 1 d . . . H61A H 0.5029 0.0731 0.3033 0.066 Uiso 1 1 calc . . . H61B H 0.4783 0.1922 0.2741 0.066 Uiso 1 1 calc . . . H61C H 0.3987 0.1066 0.2753 0.066 Uiso 1 1 calc . . . C62 C 0.2986(2) 0.21922(17) 0.36811(11) 0.0371(5) Uani 1 1 d . . . H62A H 0.3269 0.2847 0.3398 0.056 Uiso 1 1 calc . . . H62B H 0.2609 0.2298 0.4153 0.056 Uiso 1 1 calc . . . H62C H 0.2506 0.1942 0.3449 0.056 Uiso 1 1 calc . . . C63 C 0.3427(2) 0.03411(17) 0.41345(13) 0.0412(6) Uani 1 1 d . . . H63A H 0.2999 0.0113 0.3856 0.062 Uiso 1 1 calc . . . H63B H 0.2993 0.0408 0.4601 0.062 Uiso 1 1 calc . . . H63C H 0.3998 -0.0168 0.4192 0.062 Uiso 1 1 calc . . . C64 C 0.3793(2) 0.34887(19) 0.64202(14) 0.0460(6) Uani 1 1 d . . . H64A H 0.4181 0.3357 0.6795 0.069 Uiso 1 1 calc . . . H64B H 0.3126 0.3848 0.6582 0.069 Uiso 1 1 calc . . . H64C H 0.4204 0.3919 0.5997 0.069 Uiso 1 1 calc . . . 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 0.0226(2) 0.02674(18) 0.02254(18) -0.00340(13) -0.00297(15) -0.00294(14) Ti2 0.0239(2) 0.02389(17) 0.02382(18) -0.00485(13) -0.00579(15) -0.00214(14) O1 0.0317(9) 0.0365(8) 0.0278(7) -0.0007(6) -0.0112(7) -0.0059(7) O2 0.0251(8) 0.0292(7) 0.0250(7) -0.0053(5) -0.0058(6) -0.0032(6) O3 0.0361(10) 0.0270(7) 0.0357(8) -0.0092(6) -0.0029(7) 0.0006(6) O4 0.0248(9) 0.0405(8) 0.0325(8) -0.0037(6) -0.0097(7) -0.0061(6) O5 0.0375(10) 0.0273(7) 0.0253(7) -0.0045(6) -0.0058(7) -0.0009(6) O6 0.0275(9) 0.0250(7) 0.0250(7) -0.0041(5) -0.0030(6) -0.0008(6) O7 0.0650(13) 0.0281(8) 0.0240(8) -0.0031(6) 0.0040(8) 0.0095(7) O8 0.0274(9) 0.0284(7) 0.0273(7) -0.0061(6) -0.0015(6) -0.0015(6) O9 0.0256(9) 0.0523(10) 0.0432(9) -0.0175(7) -0.0072(7) -0.0050(7) O10 0.0428(11) 0.0303(8) 0.0321(8) 0.0005(6) 0.0003(7) -0.0046(7) O11 0.0280(9) 0.0462(9) 0.0336(8) -0.0176(7) -0.0078(7) -0.0004(7) O12 0.0229(8) 0.0315(7) 0.0249(7) -0.0064(6) -0.0021(6) -0.0031(6) C1 0.0326(13) 0.0384(12) 0.0327(11) -0.0072(9) -0.0119(10) -0.0128(10) C2 0.0308(13) 0.0271(10) 0.0310(11) -0.0026(8) -0.0078(9) -0.0066(9) C3 0.0316(14) 0.0302(11) 0.0418(13) -0.0030(9) -0.0146(11) -0.0065(9) C4 0.0248(12) 0.0273(10) 0.0407(12) 0.0007(9) -0.0046(10) -0.0039(8) C5 0.0277(14) 0.0505(14) 0.0539(15) -0.0009(11) -0.0086(12) -0.0030(11) C6 0.0259(12) 0.0300(10) 0.0322(11) -0.0026(8) -0.0023(9) -0.0034(9) C7 0.0286(12) 0.0228(9) 0.0259(10) -0.0032(7) -0.0049(9) -0.0046(8) C8 0.0250(12) 0.0204(9) 0.0293(10) -0.0007(7) -0.0050(9) -0.0032(8) C9 0.0298(13) 0.0370(11) 0.0259(10) -0.0075(8) -0.0042(9) -0.0044(9) C10 0.0410(17) 0.0745(18) 0.0285(12) -0.0129(11) -0.0025(11) -0.0120(13) C11 0.0445(16) 0.0420(13) 0.0363(12) -0.0055(10) -0.0192(11) -0.0041(11) C12 0.0409(15) 0.0402(12) 0.0387(12) -0.0145(10) -0.0067(11) -0.0091(10) C13 0.0435(16) 0.0274(11) 0.0520(15) -0.0119(10) 0.0136(12) 0.0017(10) C14 0.077(2) 0.0464(15) 0.0558(17) -0.0248(13) 0.0122(16) -0.0253(14) C15 0.069(2) 0.0373(14) 0.080(2) 0.0027(14) -0.0017(18) 0.0167(14) C16 0.0283(13) 0.0339(11) 0.0397(12) -0.0080(9) -0.0127(10) -0.0024(9) C17 0.0278(14) 0.0507(14) 0.0511(15) 0.0011(11) -0.0090(12) -0.0027(11) C18 0.0384(17) 0.0816(19) 0.0372(13) -0.0030(13) -0.0178(12) -0.0035(14) C19 0.0420(16) 0.0415(13) 0.0447(14) -0.0038(10) -0.0231(12) 0.0021(11) C20 0.0464(15) 0.0289(10) 0.0273(11) -0.0111(8) -0.0064(10) -0.0057(10) C21 0.0377(14) 0.0290(10) 0.0233(10) -0.0069(8) -0.0076(9) -0.0023(9) C22 0.0412(15) 0.0288(10) 0.0294(11) -0.0107(8) -0.0090(10) 0.0022(9) C23 0.0360(14) 0.0414(12) 0.0266(11) -0.0129(9) -0.0081(10) 0.0027(10) C24 0.0363(15) 0.0541(15) 0.0420(14) -0.0224(11) -0.0037(11) 0.0033(11) C25 0.0321(13) 0.0356(11) 0.0268(10) -0.0073(8) -0.0058(9) -0.0029(9) C26 0.0314(13) 0.0290(10) 0.0225(10) -0.0042(8) -0.0046(9) -0.0030(9) C27 0.0291(12) 0.0287(10) 0.0216(10) -0.0050(8) -0.0079(9) 0.0004(8) C28 0.0387(14) 0.0275(10) 0.0291(11) -0.0050(8) 0.0000(10) -0.0040(9) C29 0.060(2) 0.0355(13) 0.0512(15) -0.0119(11) 0.0115(14) -0.0168(12) C30 0.062(2) 0.0301(12) 0.0492(15) -0.0027(10) -0.0185(14) 0.0067(11) C31 0.0495(17) 0.0278(11) 0.0366(12) -0.0100(9) -0.0019(11) -0.0065(10) C32 0.0577(18) 0.0281(11) 0.0409(13) -0.0007(9) -0.0124(12) 0.0096(11) C33 0.0487(16) 0.0363(12) 0.0197(10) -0.0004(8) -0.0013(10) 0.0083(10) C34 0.0348(13) 0.0318(10) 0.0204(10) -0.0068(8) -0.0046(9) -0.0026(9) C35 0.0406(15) 0.0336(11) 0.0235(10) -0.0060(8) -0.0035(10) -0.0084(10) C36 0.0343(14) 0.0434(12) 0.0254(10) -0.0107(9) -0.0016(10) -0.0121(10) C37 0.0407(16) 0.0599(15) 0.0340(13) -0.0117(11) 0.0034(11) -0.0140(12) C38 0.0263(13) 0.0440(12) 0.0313(11) -0.0172(9) -0.0022(9) -0.0056(9) C39 0.0278(12) 0.0322(10) 0.0268(10) -0.0126(8) -0.0060(9) -0.0022(9) C40 0.0302(12) 0.0300(10) 0.0205(9) -0.0091(8) -0.0035(8) -0.0048(8) C41 0.0317(14) 0.0327(11) 0.0417(13) -0.0120(9) -0.0047(10) 0.0019(9) C42 0.0388(16) 0.0424(13) 0.0573(16) -0.0165(11) -0.0018(13) 0.0057(11) C43 0.0474(17) 0.0453(14) 0.0407(14) -0.0050(10) -0.0113(12) 0.0085(12) C44 0.0406(16) 0.0345(12) 0.0706(18) -0.0149(12) -0.0112(14) -0.0040(11) C45 0.098(3) 0.102(3) 0.131(3) 0.031(2) -0.083(3) -0.059(3) C46 0.097(4) 0.187(5) 0.143(4) 0.019(4) -0.019(3) -0.100(4) C47 0.086(3) 0.213(5) 0.078(3) -0.030(3) -0.051(3) 0.034(3) C48 0.0394(15) 0.0313(11) 0.0291(11) 0.0011(8) -0.0102(10) -0.0077(9) C49 0.068(2) 0.0330(13) 0.0583(17) -0.0054(11) -0.0050(15) -0.0004(12) C50 0.0487(18) 0.0516(15) 0.0464(15) 0.0034(12) -0.0017(13) -0.0159(13) C51 0.158(4) 0.0337(14) 0.0395(15) -0.0033(11) -0.0102(19) -0.0220(18) C52 0.0270(13) 0.0521(13) 0.0298(11) -0.0095(10) -0.0094(10) 0.0033(10) C53 0.0241(12) 0.0375(11) 0.0286(11) -0.0083(8) -0.0068(9) 0.0010(9) C54 0.0258(13) 0.0413(12) 0.0419(13) -0.0120(10) -0.0085(10) -0.0005(10) C55 0.0277(13) 0.0379(12) 0.0419(13) -0.0116(10) 0.0009(10) -0.0031(10) C56 0.0332(16) 0.0640(17) 0.0522(16) -0.0213(13) 0.0061(12) -0.0152(12) C57 0.0324(13) 0.0325(11) 0.0280(11) -0.0080(8) 0.0026(9) -0.0023(9) C58 0.0266(12) 0.0250(9) 0.0267(10) -0.0055(8) -0.0038(9) 0.0001(8) C59 0.0220(11) 0.0278(10) 0.0256(10) -0.0042(8) -0.0032(8) 0.0006(8) C60 0.0349(14) 0.0326(11) 0.0246(10) -0.0076(8) -0.0049(9) -0.0023(9) C61 0.0466(17) 0.0536(15) 0.0324(12) -0.0158(11) -0.0048(11) -0.0031(12) C62 0.0390(15) 0.0449(13) 0.0305(11) -0.0098(9) -0.0111(10) -0.0028(11) C63 0.0521(17) 0.0323(11) 0.0406(13) -0.0106(10) -0.0079(12) -0.0086(11) C64 0.0455(17) 0.0473(14) 0.0561(15) -0.0169(12) -0.0247(13) -0.0081(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 O10 1.7649(14) . ? Ti1 O9 1.7742(16) . ? Ti1 O12 1.9226(14) . ? Ti1 O8 1.9287(14) . ? Ti1 O7 2.2553(14) . ? Ti1 O11 2.2568(16) . ? Ti2 O3 1.7627(14) . ? Ti2 O4 1.7748(15) . ? Ti2 O2 1.9366(14) . ? Ti2 O6 1.9403(13) . ? Ti2 O1 2.2321(15) . ? Ti2 O5 2.2689(14) . ? O1 C19 1.436(3) . ? O1 C1 1.459(2) . ? O2 C8 1.348(2) . ? O3 C13 1.415(2) . ? O4 C16 1.411(3) . ? O5 C32 1.424(3) . ? O5 C20 1.453(2) . ? O6 C27 1.334(2) . ? O7 C51 1.359(3) . ? O7 C33 1.457(3) . ? O8 C40 1.342(2) . ? O9 C45 1.347(4) . ? O10 C48 1.418(2) . ? O11 C64 1.433(3) . ? O11 C52 1.445(3) . ? O12 C59 1.348(2) . ? C1 C2 1.498(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.377(3) . ? C2 C8 1.410(3) . ? C3 C4 1.387(3) . ? C3 H3 0.9500 . ? C4 C6 1.391(3) . ? C4 C5 1.507(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.401(3) . ? C6 H6 0.9500 . ? C7 C8 1.418(3) . ? C7 C9 1.533(3) . ? C9 C12 1.530(3) . ? C9 C10 1.536(3) . ? C9 C11 1.540(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.508(4) . ? C13 C15 1.526(4) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.510(3) . ? C16 C18 1.513(3) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.495(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.390(3) . ? C21 C27 1.408(3) . ? C22 C23 1.382(3) . ? C22 H22 0.9500 . ? C23 C25 1.395(3) . ? C23 C24 1.513(3) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.391(3) . ? C25 H25 0.9500 . ? C26 C27 1.421(3) . ? C26 C28 1.534(3) . ? C28 C31 1.536(3) . ? C28 C30 1.542(4) . ? C28 C29 1.541(3) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.482(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.397(3) . ? C34 C40 1.405(3) . ? C35 C36 1.382(3) . ? C35 H35 0.9500 . ? C36 C38 1.397(3) . ? C36 C37 1.517(3) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.395(3) . ? C38 H38 0.9500 . ? C39 C40 1.418(3) . ? C39 C41 1.530(3) . ? C41 C42 1.523(3) . ? C41 C44 1.529(3) . ? C41 C43 1.539(3) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.411(6) . ? C45 C47 1.431(5) . ? C45 H45 1.0000 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C50 1.508(4) . ? C48 C49 1.516(3) . ? C48 H48 1.0000 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.502(3) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.390(3) . ? C53 C59 1.401(3) . ? C54 C55 1.386(3) . ? C54 H54 0.9500 . ? C55 C57 1.387(3) . ? C55 C56 1.517(3) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.392(3) . ? C57 H57 0.9500 . ? C58 C59 1.414(3) . ? C58 C60 1.534(3) . ? C60 C62 1.532(3) . ? C60 C61 1.534(3) . ? C60 C63 1.541(3) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 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 O10 Ti1 O9 105.07(8) . . ? O10 Ti1 O12 98.06(7) . . ? O9 Ti1 O12 96.08(7) . . ? O10 Ti1 O8 97.12(7) . . ? O9 Ti1 O8 97.88(7) . . ? O12 Ti1 O8 155.92(6) . . ? O10 Ti1 O7 166.35(8) . . ? O9 Ti1 O7 88.58(7) . . ? O12 Ti1 O7 80.18(6) . . ? O8 Ti1 O7 80.66(5) . . ? O10 Ti1 O11 88.28(7) . . ? O9 Ti1 O11 166.64(7) . . ? O12 Ti1 O11 81.20(6) . . ? O8 Ti1 O11 80.69(6) . . ? O7 Ti1 O11 78.07(6) . . ? O3 Ti2 O4 104.69(7) . . ? O3 Ti2 O2 98.23(6) . . ? O4 Ti2 O2 95.72(6) . . ? O3 Ti2 O6 95.16(6) . . ? O4 Ti2 O6 97.38(7) . . ? O2 Ti2 O6 158.23(6) . . ? O3 Ti2 O1 93.00(7) . . ? O4 Ti2 O1 162.29(6) . . ? O2 Ti2 O1 80.84(6) . . ? O6 Ti2 O1 81.40(6) . . ? O3 Ti2 O5 167.61(7) . . ? O4 Ti2 O5 87.55(6) . . ? O2 Ti2 O5 82.14(5) . . ? O6 Ti2 O5 81.14(5) . . ? O1 Ti2 O5 74.79(6) . . ? C19 O1 C1 113.61(17) . . ? C19 O1 Ti2 120.19(13) . . ? C1 O1 Ti2 118.26(11) . . ? C8 O2 Ti2 129.67(12) . . ? C13 O3 Ti2 171.37(17) . . ? C16 O4 Ti2 161.25(14) . . ? C32 O5 C20 112.84(17) . . ? C32 O5 Ti2 119.47(13) . . ? C20 O5 Ti2 116.13(11) . . ? C27 O6 Ti2 129.88(12) . . ? C51 O7 C33 116.12(17) . . ? C51 O7 Ti1 125.97(14) . . ? C33 O7 Ti1 117.77(12) . . ? C40 O8 Ti1 131.30(12) . . ? C45 O9 Ti1 176.0(2) . . ? C48 O10 Ti1 167.06(15) . . ? C64 O11 C52 113.55(18) . . ? C64 O11 Ti1 119.49(14) . . ? C52 O11 Ti1 118.08(12) . . ? C59 O12 Ti1 127.81(12) . . ? O1 C1 C2 111.03(16) . . ? O1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? O1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? C3 C2 C8 120.8(2) . . ? C3 C2 C1 122.7(2) . . ? C8 C2 C1 116.5(2) . . ? C2 C3 C4 121.6(2) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C3 C4 C6 117.0(2) . . ? C3 C4 C5 121.9(2) . . ? C6 C4 C5 121.1(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 C7 124.4(2) . . ? C4 C6 H6 117.8 . . ? C7 C6 H6 117.8 . . ? C6 C7 C8 116.63(19) . . ? C6 C7 C9 121.82(18) . . ? C8 C7 C9 121.55(19) . . ? O2 C8 C2 118.21(18) . . ? O2 C8 C7 122.30(19) . . ? C2 C8 C7 119.5(2) . . ? C12 C9 C7 110.03(17) . . ? C12 C9 C10 106.96(18) . . ? C7 C9 C10 112.26(19) . . ? C12 C9 C11 109.6(2) . . ? C7 C9 C11 109.90(17) . . ? C10 C9 C11 107.96(19) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O3 C13 C14 110.2(2) . . ? O3 C13 C15 107.9(2) . . ? C14 C13 C15 113.1(2) . . ? O3 C13 H13 108.5 . . ? C14 C13 H13 108.5 . . ? C15 C13 H13 108.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O4 C16 C17 109.50(19) . . ? O4 C16 C18 108.97(19) . . ? C17 C16 C18 112.3(2) . . ? O4 C16 H16 108.7 . . ? C17 C16 H16 108.7 . . ? C18 C16 H16 108.7 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O1 C19 H19A 109.5 . . ? O1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O5 C20 C21 112.09(17) . . ? O5 C20 H20A 109.2 . . ? C21 C20 H20A 109.2 . . ? O5 C20 H20B 109.2 . . ? C21 C20 H20B 109.2 . . ? H20A C20 H20B 107.9 . . ? C22 C21 C27 120.97(19) . . ? C22 C21 C20 122.64(18) . . ? C27 C21 C20 116.4(2) . . ? C23 C22 C21 120.86(19) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C22 C23 C25 117.7(2) . . ? C22 C23 C24 121.6(2) . . ? C25 C23 C24 120.7(2) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C23 124.1(2) . . ? C26 C25 H25 117.9 . . ? C23 C25 H25 117.9 . . ? C25 C26 C27 117.12(18) . . ? C25 C26 C28 121.88(19) . . ? C27 C26 C28 120.92(19) . . ? O6 C27 C21 118.31(18) . . ? O6 C27 C26 122.46(17) . . ? C21 C27 C26 119.2(2) . . ? C26 C28 C31 111.30(16) . . ? C26 C28 C30 108.67(19) . . ? C31 C28 C30 109.7(2) . . ? C26 C28 C29 112.21(19) . . ? C31 C28 C29 106.15(19) . . ? C30 C28 C29 108.8(2) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O5 C32 H32A 109.5 . . ? O5 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O5 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O7 C33 C34 111.66(18) . . ? O7 C33 H33A 109.3 . . ? C34 C33 H33A 109.3 . . ? O7 C33 H33B 109.3 . . ? C34 C33 H33B 109.3 . . ? H33A C33 H33B 107.9 . . ? C35 C34 C40 120.4(2) . . ? C35 C34 C33 122.25(19) . . ? C40 C34 C33 117.30(19) . . ? C36 C35 C34 120.7(2) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C35 C36 C38 118.1(2) . . ? C35 C36 C37 121.2(2) . . ? C38 C36 C37 120.7(2) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C36 123.8(2) . . ? C39 C38 H38 118.1 . . ? C36 C38 H38 118.1 . . ? C38 C39 C40 116.83(19) . . ? C38 C39 C41 122.0(2) . . ? C40 C39 C41 121.16(19) . . ? O8 C40 C34 118.01(19) . . ? O8 C40 C39 121.86(18) . . ? C34 C40 C39 120.12(19) . . ? C42 C41 C44 107.77(19) . . ? C42 C41 C39 112.36(19) . . ? C44 C41 C39 110.3(2) . . ? C42 C41 C43 106.9(2) . . ? C44 C41 C43 109.9(2) . . ? C39 C41 C43 109.48(18) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O9 C45 C46 115.7(4) . . ? O9 C45 C47 115.7(3) . . ? C46 C45 C47 122.2(4) . . ? O9 C45 H45 98.5 . . ? C46 C45 H45 98.5 . . ? C47 C45 H45 98.5 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? O10 C48 C50 109.66(19) . . ? O10 C48 C49 108.52(18) . . ? C50 C48 C49 111.9(2) . . ? O10 C48 H48 108.9 . . ? C50 C48 H48 108.9 . . ? C49 C48 H48 108.9 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O7 C51 H51A 109.5 . . ? O7 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O7 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O11 C52 C53 113.12(18) . . ? O11 C52 H52A 109.0 . . ? C53 C52 H52A 109.0 . . ? O11 C52 H52B 109.0 . . ? C53 C52 H52B 109.0 . . ? H52A C52 H52B 107.8 . . ? C54 C53 C59 120.49(19) . . ? C54 C53 C52 122.7(2) . . ? C59 C53 C52 116.7(2) . . ? C55 C54 C53 120.3(2) . . ? C55 C54 H54 119.8 . . ? C53 C54 H54 119.8 . . ? C57 C55 C54 118.3(2) . . ? C57 C55 C56 120.9(2) . . ? C54 C55 C56 120.8(2) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 C58 123.8(2) . . ? C55 C57 H57 118.1 . . ? C58 C57 H57 118.1 . . ? C57 C58 C59 116.72(19) . . ? C57 C58 C60 122.05(18) . . ? C59 C58 C60 121.22(19) . . ? O12 C59 C53 117.89(18) . . ? O12 C59 C58 121.93(19) . . ? C53 C59 C58 120.18(19) . . ? C62 C60 C58 109.66(17) . . ? C62 C60 C61 108.18(18) . . ? C58 C60 C61 112.09(19) . . ? C62 C60 C63 109.1(2) . . ? C58 C60 C63 110.50(17) . . ? C61 C60 C63 107.18(18) . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C60 C63 H63A 109.5 . . ? C60 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C60 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? O11 C64 H64A 109.5 . . ? O11 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? O11 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 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 O3 Ti2 O1 C19 -33.92(16) . . . . ? O4 Ti2 O1 C19 148.2(2) . . . . ? O2 Ti2 O1 C19 -131.79(16) . . . . ? O6 Ti2 O1 C19 60.85(16) . . . . ? O5 Ti2 O1 C19 143.93(16) . . . . ? O3 Ti2 O1 C1 113.09(15) . . . . ? O4 Ti2 O1 C1 -64.8(3) . . . . ? O2 Ti2 O1 C1 15.23(14) . . . . ? O6 Ti2 O1 C1 -152.14(15) . . . . ? O5 Ti2 O1 C1 -69.05(14) . . . . ? O3 Ti2 O2 C8 -47.75(17) . . . . ? O4 Ti2 O2 C8 -153.54(16) . . . . ? O6 Ti2 O2 C8 79.7(2) . . . . ? O1 Ti2 O2 C8 43.98(16) . . . . ? O5 Ti2 O2 C8 119.74(16) . . . . ? O4 Ti2 O3 C13 4.6(10) . . . . ? O2 Ti2 O3 C13 -93.6(10) . . . . ? O6 Ti2 O3 C13 103.6(9) . . . . ? O1 Ti2 O3 C13 -174.7(9) . . . . ? O5 Ti2 O3 C13 175.6(8) . . . . ? O3 Ti2 O4 C16 16.1(5) . . . . ? O2 Ti2 O4 C16 116.2(4) . . . . ? O6 Ti2 O4 C16 -81.2(4) . . . . ? O1 Ti2 O4 C16 -166.0(4) . . . . ? O5 Ti2 O4 C16 -161.9(4) . . . . ? O3 Ti2 O5 C32 160.3(3) . . . . ? O4 Ti2 O5 C32 -28.39(16) . . . . ? O2 Ti2 O5 C32 67.73(16) . . . . ? O6 Ti2 O5 C32 -126.25(16) . . . . ? O1 Ti2 O5 C32 150.32(16) . . . . ? O3 Ti2 O5 C20 -58.9(3) . . . . ? O4 Ti2 O5 C20 112.32(15) . . . . ? O2 Ti2 O5 C20 -151.56(15) . . . . ? O6 Ti2 O5 C20 14.46(15) . . . . ? O1 Ti2 O5 C20 -68.97(15) . . . . ? O3 Ti2 O6 C27 -147.57(16) . . . . ? O4 Ti2 O6 C27 -41.99(17) . . . . ? O2 Ti2 O6 C27 84.6(2) . . . . ? O1 Ti2 O6 C27 120.17(16) . . . . ? O5 Ti2 O6 C27 44.35(16) . . . . ? O10 Ti1 O7 C51 -117.0(4) . . . . ? O9 Ti1 O7 C51 63.1(3) . . . . ? O12 Ti1 O7 C51 -33.3(3) . . . . ? O8 Ti1 O7 C51 161.3(3) . . . . ? O11 Ti1 O7 C51 -116.3(3) . . . . ? O10 Ti1 O7 C33 67.4(3) . . . . ? O9 Ti1 O7 C33 -112.50(18) . . . . ? O12 Ti1 O7 C33 151.08(18) . . . . ? O8 Ti1 O7 C33 -14.27(17) . . . . ? O11 Ti1 O7 C33 68.10(17) . . . . ? O10 Ti1 O8 C40 150.25(18) . . . . ? O9 Ti1 O8 C40 43.88(18) . . . . ? O12 Ti1 O8 C40 -81.0(2) . . . . ? O7 Ti1 O8 C40 -43.36(18) . . . . ? O11 Ti1 O8 C40 -122.68(18) . . . . ? O10 Ti1 O9 C45 148(4) . . . . ? O12 Ti1 O9 C45 48(4) . . . . ? O8 Ti1 O9 C45 -112(4) . . . . ? O7 Ti1 O9 C45 -32(4) . . . . ? O11 Ti1 O9 C45 -30(4) . . . . ? O9 Ti1 O10 C48 -32.6(7) . . . . ? O12 Ti1 O10 C48 66.0(7) . . . . ? O8 Ti1 O10 C48 -132.8(7) . . . . ? O7 Ti1 O10 C48 147.5(6) . . . . ? O11 Ti1 O10 C48 146.8(7) . . . . ? O10 Ti1 O11 C64 42.97(16) . . . . ? O9 Ti1 O11 C64 -139.4(3) . . . . ? O12 Ti1 O11 C64 141.40(17) . . . . ? O8 Ti1 O11 C64 -54.53(16) . . . . ? O7 Ti1 O11 C64 -136.86(17) . . . . ? O10 Ti1 O11 C52 -102.31(15) . . . . ? O9 Ti1 O11 C52 75.3(3) . . . . ? O12 Ti1 O11 C52 -3.88(14) . . . . ? O8 Ti1 O11 C52 160.19(15) . . . . ? O7 Ti1 O11 C52 77.86(14) . . . . ? O10 Ti1 O12 C59 35.48(17) . . . . ? O9 Ti1 O12 C59 141.69(16) . . . . ? O8 Ti1 O12 C59 -93.1(2) . . . . ? O7 Ti1 O12 C59 -130.81(16) . . . . ? O11 Ti1 O12 C59 -51.50(15) . . . . ? C19 O1 C1 C2 89.5(2) . . . . ? Ti2 O1 C1 C2 -59.6(2) . . . . ? O1 C1 C2 C3 -124.2(2) . . . . ? O1 C1 C2 C8 57.1(2) . . . . ? C8 C2 C3 C4 -0.9(3) . . . . ? C1 C2 C3 C4 -179.58(19) . . . . ? C2 C3 C4 C6 1.8(3) . . . . ? C2 C3 C4 C5 -175.7(2) . . . . ? C3 C4 C6 C7 -0.2(3) . . . . ? C5 C4 C6 C7 177.3(2) . . . . ? C4 C6 C7 C8 -2.2(3) . . . . ? C4 C6 C7 C9 178.33(18) . . . . ? Ti2 O2 C8 C2 -57.8(2) . . . . ? Ti2 O2 C8 C7 123.13(17) . . . . ? C3 C2 C8 O2 179.33(17) . . . . ? C1 C2 C8 O2 -1.9(3) . . . . ? C3 C2 C8 C7 -1.6(3) . . . . ? C1 C2 C8 C7 177.18(17) . . . . ? C6 C7 C8 O2 -177.96(17) . . . . ? C9 C7 C8 O2 1.5(3) . . . . ? C6 C7 C8 C2 3.0(3) . . . . ? C9 C7 C8 C2 -177.53(17) . . . . ? C6 C7 C9 C12 116.4(2) . . . . ? C8 C7 C9 C12 -63.1(2) . . . . ? C6 C7 C9 C10 -2.6(3) . . . . ? C8 C7 C9 C10 177.94(19) . . . . ? C6 C7 C9 C11 -122.7(2) . . . . ? C8 C7 C9 C11 57.8(2) . . . . ? Ti2 O3 C13 C14 -6.5(11) . . . . ? Ti2 O3 C13 C15 -130.5(9) . . . . ? Ti2 O4 C16 C17 119.2(4) . . . . ? Ti2 O4 C16 C18 -117.6(4) . . . . ? C32 O5 C20 C21 83.7(2) . . . . ? Ti2 O5 C20 C21 -59.6(2) . . . . ? O5 C20 C21 C22 -123.1(2) . . . . ? O5 C20 C21 C27 59.2(3) . . . . ? C27 C21 C22 C23 1.3(3) . . . . ? C20 C21 C22 C23 -176.3(2) . . . . ? C21 C22 C23 C25 0.1(3) . . . . ? C21 C22 C23 C24 178.5(2) . . . . ? C22 C23 C25 C26 -0.7(3) . . . . ? C24 C23 C25 C26 -179.1(2) . . . . ? C23 C25 C26 C27 -0.1(3) . . . . ? C23 C25 C26 C28 176.8(2) . . . . ? Ti2 O6 C27 C21 -57.3(2) . . . . ? Ti2 O6 C27 C26 124.18(18) . . . . ? C22 C21 C27 O6 179.41(18) . . . . ? C20 C21 C27 O6 -2.9(3) . . . . ? C22 C21 C27 C26 -2.1(3) . . . . ? C20 C21 C27 C26 175.63(19) . . . . ? C25 C26 C27 O6 179.90(18) . . . . ? C28 C26 C27 O6 3.0(3) . . . . ? C25 C26 C27 C21 1.4(3) . . . . ? C28 C26 C27 C21 -175.43(19) . . . . ? C25 C26 C28 C31 124.9(2) . . . . ? C27 C26 C28 C31 -58.4(3) . . . . ? C25 C26 C28 C30 -114.2(2) . . . . ? C27 C26 C28 C30 62.5(2) . . . . ? C25 C26 C28 C29 6.1(3) . . . . ? C27 C26 C28 C29 -177.2(2) . . . . ? C51 O7 C33 C34 -117.9(3) . . . . ? Ti1 O7 C33 C34 58.1(2) . . . . ? O7 C33 C34 C35 124.8(2) . . . . ? O7 C33 C34 C40 -58.0(3) . . . . ? C40 C34 C35 C36 -1.4(3) . . . . ? C33 C34 C35 C36 175.7(2) . . . . ? C34 C35 C36 C38 -0.6(3) . . . . ? C34 C35 C36 C37 179.7(2) . . . . ? C35 C36 C38 C39 1.0(3) . . . . ? C37 C36 C38 C39 -179.3(2) . . . . ? C36 C38 C39 C40 0.6(3) . . . . ? C36 C38 C39 C41 -178.8(2) . . . . ? Ti1 O8 C40 C34 55.2(3) . . . . ? Ti1 O8 C40 C39 -125.89(17) . . . . ? C35 C34 C40 O8 -177.98(18) . . . . ? C33 C34 C40 O8 4.7(3) . . . . ? C35 C34 C40 C39 3.1(3) . . . . ? C33 C34 C40 C39 -174.19(19) . . . . ? C38 C39 C40 O8 178.47(18) . . . . ? C41 C39 C40 O8 -2.1(3) . . . . ? C38 C39 C40 C34 -2.6(3) . . . . ? C41 C39 C40 C34 176.76(19) . . . . ? C38 C39 C41 C42 1.8(3) . . . . ? C40 C39 C41 C42 -177.6(2) . . . . ? C38 C39 C41 C44 122.0(2) . . . . ? C40 C39 C41 C44 -57.3(3) . . . . ? C38 C39 C41 C43 -116.9(2) . . . . ? C40 C39 C41 C43 63.8(3) . . . . ? Ti1 O9 C45 C46 64(4) . . . . ? Ti1 O9 C45 C47 -143(3) . . . . ? Ti1 O10 C48 C50 -108.1(7) . . . . ? Ti1 O10 C48 C49 129.3(7) . . . . ? C64 O11 C52 C53 -97.1(2) . . . . ? Ti1 O11 C52 C53 50.2(2) . . . . ? O11 C52 C53 C54 124.5(2) . . . . ? O11 C52 C53 C59 -59.4(3) . . . . ? C59 C53 C54 C55 -1.0(3) . . . . ? C52 C53 C54 C55 175.0(2) . . . . ? C53 C54 C55 C57 -2.4(3) . . . . ? C53 C54 C55 C56 178.2(2) . . . . ? C54 C55 C57 C58 2.2(3) . . . . ? C56 C55 C57 C58 -178.4(2) . . . . ? C55 C57 C58 C59 1.5(3) . . . . ? C55 C57 C58 C60 -179.3(2) . . . . ? Ti1 O12 C59 C53 57.5(2) . . . . ? Ti1 O12 C59 C58 -123.00(17) . . . . ? C54 C53 C59 O12 -175.65(19) . . . . ? C52 C53 C59 O12 8.1(3) . . . . ? C54 C53 C59 C58 4.8(3) . . . . ? C52 C53 C59 C58 -171.45(19) . . . . ? C57 C58 C59 O12 175.57(18) . . . . ? C60 C58 C59 O12 -3.7(3) . . . . ? C57 C58 C59 C53 -4.9(3) . . . . ? C60 C58 C59 C53 175.88(18) . . . . ? C57 C58 C60 C62 -111.1(2) . . . . ? C59 C58 C60 C62 68.0(2) . . . . ? C57 C58 C60 C61 9.0(3) . . . . ? C59 C58 C60 C61 -171.78(19) . . . . ? C57 C58 C60 C63 128.5(2) . . . . ? C59 C58 C60 C63 -52.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.554 _refine_diff_density_min -0.579 _refine_diff_density_rms 0.063 data_jbme2ph _database_code_depnum_ccdc_archive 'CCDC 871144' #TrackingRef 'allcifs_Ti.cif' _audit_creation_date 11-06-24 _audit_creation_method CRYSTALS_ver_14.11 _cell_length_a 14.6692(9) _cell_length_b 16.9750(10) _cell_length_c 11.3986(7) _cell_angle_alpha 90 _cell_angle_beta 97.659(6) _cell_angle_gamma 90 _cell_volume 2813.0(3) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall ' -P 2ybc ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ti 0.2776 0.4457 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C21 H21 Cl3.50 N7 O7 Ti1.75 # Dc = 1.63 Fooo = 1064.00 Mu = 8.88 M = 691.35 # Found Formula = C28 H44 O4 Ti1 # Dc = 1.16 FOOO = 1064.00 Mu = 3.33 M = 492.55 _chemical_formula_sum 'C56 H88 O8 Ti2 ' _chemical_formula_moiety 'C56 H88 O8 Ti2 ' _chemical_compound_source ? _chemical_formula_weight 985.00 _cell_measurement_reflns_used 14461 _cell_measurement_theta_min 3.3407 _cell_measurement_theta_max 29.4496 _cell_measurement_temperature 100 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_min 0.131 _exptl_crystal_size_mid 0.320 _exptl_crystal_size_max 0.454 _exptl_crystal_density_diffrn 1.163 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 0.333 # Sheldrick geometric approximatio 0.90 0.96 _exptl_absorpt_correction_T_min 0.903 _exptl_absorpt_correction_T_max 0.962 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_detector_area_resol_mean 10.4685 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 100 _diffrn_reflns_number 38264 _reflns_number_total 7120 _diffrn_reflns_av_R_equivalents 0.049 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 7120 # Theoretical number of reflections is about 15684 _diffrn_reflns_theta_min 3.346 _diffrn_reflns_theta_max 29.504 _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 26.554 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -20 _reflns_limit_h_max 20 _reflns_limit_k_min 0 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.04 _refine_diff_density_max 1.17 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 7120 _refine_ls_number_restraints 0 _refine_ls_number_parameters 299 _refine_ls_R_factor_ref 0.0706 _refine_ls_wR_factor_ref 0.1545 _refine_ls_goodness_of_fit_ref 0.9362 _refine_ls_shift/su_max 0.0010253 _refine_ls_shift/su_mean 0.0000330 # The values computed from all data _oxford_reflns_number_all 7120 _refine_ls_R_factor_all 0.0706 _refine_ls_wR_factor_all 0.1545 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6079 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_gt 0.1370 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; ; # Insert your own references if required - in alphabetical order 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ti1 Ti 0.90010(2) 0.45628(2) 0.47554(3) 0.0164 1.0000 Uani . . . . . . O2 O 0.87189(11) 0.45633(9) 0.31211(13) 0.0202 1.0000 Uani . . . . . . C3 C 0.79880(14) 0.43119(12) 0.23652(17) 0.0176 1.0000 Uani . . . . . . C4 C 0.76502(14) 0.47499(12) 0.13511(18) 0.0174 1.0000 Uani . . . . . . C5 C 0.68940(14) 0.44350(13) 0.06164(18) 0.0184 1.0000 Uani . . . . . . C6 C 0.64769(14) 0.37225(12) 0.08377(17) 0.0180 1.0000 Uani . . . . . . C7 C 0.56537(15) 0.33765(13) 0.00348(19) 0.0209 1.0000 Uani . . . . . . C8 C 0.49164(14) 0.31474(13) 0.08046(18) 0.0199 1.0000 Uani . . . . . . C9 C 0.47010(15) 0.36738(13) 0.16685(19) 0.0224 1.0000 Uani . . . . . . C10 C 0.40296(17) 0.34987(15) 0.2373(2) 0.0281 1.0000 Uani . . . . . . C11 C 0.35574(17) 0.27864(16) 0.2236(2) 0.0314 1.0000 Uani . . . . . . C12 C 0.37546(18) 0.22639(16) 0.1379(2) 0.0333 1.0000 Uani . . . . . . C13 C 0.44329(17) 0.24387(15) 0.0673(2) 0.0279 1.0000 Uani . . . . . . C14 C 0.59995(17) 0.26667(15) -0.0617(2) 0.0294 1.0000 Uani . . . . . . C15 C 0.52151(16) 0.39622(15) -0.0910(2) 0.0262 1.0000 Uani . . . . . . C16 C 0.68411(14) 0.32994(12) 0.18374(18) 0.0197 1.0000 Uani . . . . . . C17 C 0.75796(14) 0.35918(12) 0.25904(18) 0.0189 1.0000 Uani . . . . . . C18 C 0.80927(14) 0.55324(12) 0.10538(19) 0.0192 1.0000 Uani . . . . . . C19 C 0.76084(16) 0.59030(14) -0.0085(2) 0.0273 1.0000 Uani . . . . . . C20 C 0.8034(2) 0.61295(14) 0.2048(2) 0.0306 1.0000 Uani . . . . . . C21 C 0.90967(16) 0.53941(15) 0.0886(2) 0.0276 1.0000 Uani . . . . . . O22 O 0.96165(10) 0.54555(8) 0.55738(13) 0.0180 1.0000 Uani . . . . . . C23 C 0.93105(15) 0.61370(13) 0.61769(19) 0.0222 1.0000 Uani . . . . . . C24 C 0.86720(18) 0.66334(15) 0.5319(2) 0.0295 1.0000 Uani . . . . . . C25 C 0.88826(17) 0.58933(16) 0.7258(2) 0.0288 1.0000 Uani . . . . . . O26 O 0.78763(11) 0.47501(11) 0.51047(15) 0.0259 1.0000 Uani . . . . . . C27 C 0.69746(18) 0.49569(17) 0.5322(3) 0.0346 1.0000 Uani . . . . . . C28 C 0.6720(2) 0.44442(19) 0.6330(3) 0.0379 1.0000 Uani . . . . . . C29 C 0.63075(18) 0.4873(2) 0.4211(3) 0.0404 1.0000 Uani . . . . . . O30 O 0.91817(12) 0.35923(10) 0.53489(15) 0.0269 1.0000 Uani . . . . . . C31 C 0.88216(17) 0.29928(14) 0.6019(2) 0.0262 1.0000 Uani . . . . . . H51 H 0.6645 0.4720 -0.0067 0.0224 1.0000 Uiso R . . . . . H91 H 0.5023 0.4147 0.1777 0.0268 1.0000 Uiso R . . . . . H101 H 0.3899 0.3861 0.2955 0.0344 1.0000 Uiso R . . . . . H111 H 0.3105 0.2669 0.2716 0.0381 1.0000 Uiso R . . . . . H121 H 0.3435 0.1778 0.1273 0.0403 1.0000 Uiso R . . . . . H131 H 0.4565 0.2068 0.0111 0.0333 1.0000 Uiso R . . . . . H141 H 0.5519 0.2444 -0.1189 0.0434 1.0000 Uiso R . . . . . H142 H 0.6502 0.2833 -0.1020 0.0437 1.0000 Uiso R . . . . . H143 H 0.6222 0.2261 -0.0057 0.0437 1.0000 Uiso R . . . . . H151 H 0.4704 0.3710 -0.1385 0.0387 1.0000 Uiso R . . . . . H152 H 0.5668 0.4107 -0.1416 0.0388 1.0000 Uiso R . . . . . H153 H 0.4996 0.4429 -0.0543 0.0384 1.0000 Uiso R . . . . . H161 H 0.6589 0.2809 0.2010 0.0239 1.0000 Uiso R . . . . . H171 H 0.7815 0.3309 0.3279 0.0235 1.0000 Uiso R . . . . . H191 H 0.7912 0.6399 -0.0229 0.0409 1.0000 Uiso R . . . . . H192 H 0.7643 0.5550 -0.0743 0.0408 1.0000 Uiso R . . . . . H193 H 0.6961 0.6012 -0.0023 0.0407 1.0000 Uiso R . . . . . H201 H 0.8305 0.6626 0.1852 0.0458 1.0000 Uiso R . . . . . H202 H 0.8356 0.5939 0.2786 0.0456 1.0000 Uiso R . . . . . H203 H 0.7389 0.6217 0.2129 0.0462 1.0000 Uiso R . . . . . H211 H 0.9365 0.5880 0.0646 0.0407 1.0000 Uiso R . . . . . H212 H 0.9449 0.5214 0.1609 0.0409 1.0000 Uiso R . . . . . H213 H 0.9137 0.5005 0.0271 0.0411 1.0000 Uiso R . . . . . H231 H 0.9853 0.6457 0.6440 0.0269 1.0000 Uiso R . . . . . H241 H 0.8513 0.7107 0.5703 0.0440 1.0000 Uiso R . . . . . H242 H 0.8984 0.6769 0.4655 0.0439 1.0000 Uiso R . . . . . H243 H 0.8124 0.6339 0.5049 0.0438 1.0000 Uiso R . . . . . H251 H 0.8725 0.6358 0.7670 0.0428 1.0000 Uiso R . . . . . H252 H 0.9318 0.5586 0.7771 0.0426 1.0000 Uiso R . . . . . H253 H 0.8331 0.5588 0.7030 0.0428 1.0000 Uiso R . . . . . H271 H 0.6970 0.5535 0.5558 0.0417 1.0000 Uiso R . . . . . H281 H 0.6096 0.4568 0.6463 0.0568 1.0000 Uiso R . . . . . H282 H 0.7135 0.4538 0.7043 0.0571 1.0000 Uiso R . . . . . H283 H 0.6753 0.3905 0.6128 0.0569 1.0000 Uiso R . . . . . H291 H 0.5714 0.5072 0.4356 0.0607 1.0000 Uiso R . . . . . H292 H 0.6520 0.5165 0.3574 0.0606 1.0000 Uiso R . . . . . H293 H 0.6259 0.4315 0.4017 0.0613 1.0000 Uiso R . . . . . H311 H 0.8151 0.3012 0.5882 0.0314 1.0000 Uiso R . . . . . C1 C 0.9126(3) 0.22013(18) 0.5624(3) 0.0551 1.0000 Uani . . . . . . C2 C 0.9143(4) 0.3137(2) 0.7306(3) 0.0715 1.0000 Uani . . . . . . H11 H 0.8875 0.1782 0.6045 0.0816 1.0000 Uiso R . . . . . H12 H 0.9786 0.2167 0.5740 0.0823 1.0000 Uiso R . . . . . H13 H 0.8918 0.2135 0.4798 0.0821 1.0000 Uiso R . . . . . H21 H 0.8938 0.2719 0.7769 0.1056 1.0000 Uiso R . . . . . H22 H 0.9799 0.3164 0.7431 0.1059 1.0000 Uiso R . . . . . H23 H 0.8904 0.3626 0.7543 0.1059 1.0000 Uiso 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 0.01575(19) 0.0182(2) 0.01494(19) -0.00005(12) 0.00101(13) -0.00147(12) O2 0.0186(7) 0.0244(8) 0.0166(7) -0.0001(5) -0.0015(5) -0.0025(6) C3 0.0166(8) 0.0199(9) 0.0160(9) -0.0027(7) 0.0007(7) 0.0005(7) C4 0.0179(9) 0.0172(9) 0.0177(9) -0.0009(7) 0.0041(7) 0.0009(7) C5 0.0177(9) 0.0216(9) 0.0154(9) -0.0003(7) 0.0008(7) 0.0009(7) C6 0.0186(9) 0.0189(9) 0.0163(9) -0.0026(7) 0.0017(7) 0.0003(7) C7 0.0208(9) 0.0224(10) 0.0190(9) -0.0021(8) 0.0012(7) -0.0033(8) C8 0.0198(9) 0.0202(10) 0.0183(9) 0.0017(7) -0.0025(7) -0.0011(8) C9 0.0220(10) 0.0228(10) 0.0219(10) 0.0023(8) 0.0014(8) 0.0010(8) C10 0.0265(11) 0.0341(13) 0.0240(11) 0.0034(9) 0.0044(9) 0.0063(9) C11 0.0233(11) 0.0403(14) 0.0307(12) 0.0106(10) 0.0036(9) -0.0033(10) C12 0.0310(12) 0.0347(13) 0.0333(13) 0.0065(10) 0.0010(10) -0.0112(10) C13 0.0310(12) 0.0266(11) 0.0251(11) -0.0006(9) 0.0004(9) -0.0075(9) C14 0.0287(11) 0.0324(12) 0.0271(11) -0.0108(9) 0.0034(9) -0.0040(9) C15 0.0252(10) 0.0320(12) 0.0197(10) 0.0031(8) -0.0040(8) -0.0054(9) C16 0.0209(9) 0.0179(9) 0.0203(9) -0.0002(7) 0.0026(7) -0.0019(7) C17 0.0200(9) 0.0191(9) 0.0173(9) 0.0012(7) 0.0010(7) 0.0016(7) C18 0.0180(9) 0.0197(9) 0.0192(9) 0.0019(7) 0.0001(7) -0.0006(7) C19 0.0271(11) 0.0266(11) 0.0268(11) 0.0091(9) -0.0013(9) -0.0028(9) C20 0.0469(14) 0.0173(10) 0.0282(11) -0.0024(8) 0.0074(10) -0.0028(10) C21 0.0191(10) 0.0307(12) 0.0334(12) 0.0064(9) 0.0051(9) -0.0015(8) O22 0.0167(7) 0.0186(7) 0.0185(7) -0.0032(5) 0.0015(5) -0.0004(5) C23 0.0219(9) 0.0239(10) 0.0207(9) -0.0074(8) 0.0020(8) 0.0007(8) C24 0.0332(12) 0.0243(11) 0.0309(12) -0.0029(9) 0.0040(9) 0.0062(9) C25 0.0286(11) 0.0372(13) 0.0209(10) -0.0061(9) 0.0049(8) 0.0052(10) O26 0.0200(7) 0.0332(9) 0.0251(8) -0.0045(7) 0.0051(6) -0.0018(7) C27 0.0279(12) 0.0367(14) 0.0405(14) -0.0063(11) 0.0095(10) -0.0017(10) C28 0.0313(13) 0.0473(16) 0.0380(14) -0.0018(12) 0.0156(11) -0.0039(11) C29 0.0249(12) 0.0538(18) 0.0429(15) 0.0005(13) 0.0062(11) 0.0049(12) O30 0.0289(8) 0.0255(8) 0.0263(8) 0.0065(6) 0.0039(6) -0.0007(7) C31 0.0295(11) 0.0253(11) 0.0246(11) 0.0043(8) 0.0060(9) -0.0070(9) C1 0.085(3) 0.0278(14) 0.061(2) 0.0098(14) 0.0419(19) 0.0001(15) C2 0.121(4) 0.063(2) 0.0268(14) 0.0081(14) -0.0006(18) -0.055(3) _refine_ls_extinction_coef 210(20) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 2.72(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ti1 . Ti1 2_766 3.2664(7) yes Ti1 . O22 2_766 2.1112(15) yes Ti1 . O2 . 1.8537(15) yes Ti1 . O22 . 1.9385(15) yes Ti1 . O26 . 1.7767(17) yes Ti1 . O30 . 1.7872(17) yes O2 . C3 . 1.352(2) yes C3 . C4 . 1.408(3) yes C3 . C17 . 1.400(3) yes C4 . C5 . 1.404(3) yes C4 . C18 . 1.536(3) yes C5 . C6 . 1.394(3) yes C5 . H51 . 0.948 no C6 . C7 . 1.532(3) yes C6 . C16 . 1.392(3) yes C7 . C8 . 1.531(3) yes C7 . C14 . 1.537(3) yes C7 . C15 . 1.542(3) yes C8 . C9 . 1.397(3) yes C8 . C13 . 1.394(3) yes C9 . C10 . 1.384(3) yes C9 . H91 . 0.932 no C10 . C11 . 1.392(4) yes C10 . H101 . 0.943 no C11 . C12 . 1.379(4) yes C11 . H111 . 0.936 no C12 . C13 . 1.393(3) yes C12 . H121 . 0.949 no C13 . H131 . 0.936 no C14 . H141 . 0.970 no C14 . H142 . 0.961 no C14 . H143 . 0.965 no C15 . H151 . 0.964 no C15 . H152 . 0.968 no C15 . H153 . 0.971 no C16 . C17 . 1.382(3) yes C16 . H161 . 0.943 no C17 . H171 . 0.944 no C18 . C19 . 1.529(3) yes C18 . C20 . 1.531(3) yes C18 . C21 . 1.528(3) yes C19 . H191 . 0.976 no C19 . H192 . 0.966 no C19 . H193 . 0.979 no C20 . H201 . 0.971 no C20 . H202 . 0.964 no C20 . H203 . 0.974 no C21 . H211 . 0.969 no C21 . H212 . 0.963 no C21 . H213 . 0.970 no O22 . C23 . 1.447(2) yes C23 . C24 . 1.516(3) yes C23 . C25 . 1.514(3) yes C23 . H231 . 0.977 no C24 . H241 . 0.959 no C24 . H242 . 0.964 no C24 . H243 . 0.962 no C25 . H251 . 0.962 no C25 . H252 . 0.960 no C25 . H253 . 0.966 no O26 . C27 . 1.422(3) yes C27 . C28 . 1.526(4) yes C27 . C29 . 1.501(4) yes C27 . H271 . 1.019 no C28 . H281 . 0.971 no C28 . H282 . 0.962 no C28 . H283 . 0.947 no C29 . H291 . 0.968 no C29 . H292 . 0.965 no C29 . H293 . 0.974 no O30 . C31 . 1.416(3) yes C31 . H311 . 0.976 no C31 . C1 . 1.504(4) yes C31 . C2 . 1.500(4) yes C1 . H11 . 0.959 no C1 . H12 . 0.960 no C1 . H13 . 0.957 no C2 . H21 . 0.956 no C2 . H22 . 0.954 no C2 . H23 . 0.955 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Ti1 2_766 Ti1 . O22 2_766 34.48(4) yes Ti1 2_766 Ti1 . O2 . 104.26(5) yes O22 2_766 Ti1 . O2 . 84.98(6) yes Ti1 2_766 Ti1 . O22 . 38.07(4) yes O22 2_766 Ti1 . O22 . 72.55(7) yes O2 . Ti1 . O22 . 120.70(7) yes Ti1 2_766 Ti1 . O26 . 136.00(6) yes O22 2_766 Ti1 . O26 . 170.10(7) yes O2 . Ti1 . O26 . 97.79(7) yes O22 . Ti1 . O26 . 98.00(7) yes Ti1 2_766 Ti1 . O30 . 105.65(6) yes O22 2_766 Ti1 . O30 . 87.49(7) yes O2 . Ti1 . O30 . 112.51(7) yes O22 . Ti1 . O30 . 120.15(7) yes O26 . Ti1 . O30 . 100.11(8) yes Ti1 . O2 . C3 . 133.80(14) yes O2 . C3 . C4 . 121.26(19) yes O2 . C3 . C17 . 118.76(18) yes C4 . C3 . C17 . 119.96(18) yes C3 . C4 . C5 . 116.90(19) yes C3 . C4 . C18 . 121.68(18) yes C5 . C4 . C18 . 121.42(18) yes C4 . C5 . C6 . 123.62(19) yes C4 . C5 . H51 . 118.9 no C6 . C5 . H51 . 117.5 no C5 . C6 . C7 . 123.70(18) yes C5 . C6 . C16 . 117.79(19) yes C7 . C6 . C16 . 118.50(19) yes C6 . C7 . C8 . 108.41(17) yes C6 . C7 . C14 . 107.75(18) yes C8 . C7 . C14 . 112.45(19) yes C6 . C7 . C15 . 113.10(18) yes C8 . C7 . C15 . 107.65(18) yes C14 . C7 . C15 . 107.57(19) yes C7 . C8 . C9 . 119.02(19) yes C7 . C8 . C13 . 123.0(2) yes C9 . C8 . C13 . 117.9(2) yes C8 . C9 . C10 . 121.2(2) yes C8 . C9 . H91 . 119.2 no C10 . C9 . H91 . 119.7 no C9 . C10 . C11 . 120.2(2) yes C9 . C10 . H101 . 119.7 no C11 . C10 . H101 . 120.1 no C10 . C11 . C12 . 119.3(2) yes C10 . C11 . H111 . 120.0 no C12 . C11 . H111 . 120.6 no C11 . C12 . C13 . 120.4(2) yes C11 . C12 . H121 . 120.1 no C13 . C12 . H121 . 119.4 no C8 . C13 . C12 . 120.9(2) yes C8 . C13 . H131 . 120.3 no C12 . C13 . H131 . 118.7 no C7 . C14 . H141 . 111.9 no C7 . C14 . H142 . 108.9 no H141 . C14 . H142 . 109.1 no C7 . C14 . H143 . 110.1 no H141 . C14 . H143 . 108.6 no H142 . C14 . H143 . 108.2 no C7 . C15 . H151 . 109.1 no C7 . C15 . H152 . 109.0 no H151 . C15 . H152 . 108.8 no C7 . C15 . H153 . 110.9 no H151 . C15 . H153 . 109.1 no H152 . C15 . H153 . 109.9 no C6 . C16 . C17 . 120.45(19) yes C6 . C16 . H161 . 120.5 no C17 . C16 . H161 . 119.0 no C3 . C17 . C16 . 121.26(19) yes C3 . C17 . H171 . 118.5 no C16 . C17 . H171 . 120.2 no C4 . C18 . C19 . 112.39(17) yes C4 . C18 . C20 . 109.99(18) yes C19 . C18 . C20 . 106.86(19) yes C4 . C18 . C21 . 109.72(17) yes C19 . C18 . C21 . 107.66(19) yes C20 . C18 . C21 . 110.16(19) yes C18 . C19 . H191 . 109.1 no C18 . C19 . H192 . 109.7 no H191 . C19 . H192 . 109.3 no C18 . C19 . H193 . 111.3 no H191 . C19 . H193 . 108.5 no H192 . C19 . H193 . 109.0 no C18 . C20 . H201 . 109.8 no C18 . C20 . H202 . 110.7 no H201 . C20 . H202 . 108.9 no C18 . C20 . H203 . 108.8 no H201 . C20 . H203 . 108.8 no H202 . C20 . H203 . 109.8 no C18 . C21 . H211 . 109.8 no C18 . C21 . H212 . 111.0 no H211 . C21 . H212 . 108.7 no C18 . C21 . H213 . 110.3 no H211 . C21 . H213 . 108.0 no H212 . C21 . H213 . 109.0 no Ti1 2_766 O22 . Ti1 . 107.45(7) yes Ti1 2_766 O22 . C23 . 117.54(12) yes Ti1 . O22 . C23 . 134.38(13) yes O22 . C23 . C24 . 110.00(17) yes O22 . C23 . C25 . 110.91(19) yes C24 . C23 . C25 . 112.91(19) yes O22 . C23 . H231 . 107.4 no C24 . C23 . H231 . 107.3 no C25 . C23 . H231 . 108.2 no C23 . C24 . H241 . 109.8 no C23 . C24 . H242 . 108.8 no H241 . C24 . H242 . 109.2 no C23 . C24 . H243 . 109.6 no H241 . C24 . H243 . 109.7 no H242 . C24 . H243 . 109.7 no C23 . C25 . H251 . 109.0 no C23 . C25 . H252 . 109.2 no H251 . C25 . H252 . 109.4 no C23 . C25 . H253 . 110.5 no H251 . C25 . H253 . 108.9 no H252 . C25 . H253 . 109.8 no Ti1 . O26 . C27 . 175.18(18) yes O26 . C27 . C28 . 108.5(2) yes O26 . C27 . C29 . 110.3(2) yes C28 . C27 . C29 . 112.6(2) yes O26 . C27 . H271 . 108.9 no C28 . C27 . H271 . 109.9 no C29 . C27 . H271 . 106.7 no C27 . C28 . H281 . 108.9 no C27 . C28 . H282 . 110.6 no H281 . C28 . H282 . 109.5 no C27 . C28 . H283 . 110.1 no H281 . C28 . H283 . 109.1 no H282 . C28 . H283 . 108.6 no C27 . C29 . H291 . 108.8 no C27 . C29 . H292 . 110.3 no H291 . C29 . H292 . 109.8 no C27 . C29 . H293 . 107.6 no H291 . C29 . H293 . 109.7 no H292 . C29 . H293 . 110.6 no Ti1 . O30 . C31 . 145.02(16) yes O30 . C31 . H311 . 109.3 no O30 . C31 . C1 . 109.5(2) yes H311 . C31 . C1 . 108.4 no O30 . C31 . C2 . 108.6(2) yes H311 . C31 . C2 . 109.3 no C1 . C31 . C2 . 111.8(3) yes C31 . C1 . H11 . 111.3 no C31 . C1 . H12 . 110.3 no H11 . C1 . H12 . 109.5 no C31 . C1 . H13 . 109.4 no H11 . C1 . H13 . 108.2 no H12 . C1 . H13 . 108.2 no C31 . C2 . H21 . 109.8 no C31 . C2 . H22 . 109.5 no H21 . C2 . H22 . 109.8 no C31 . C2 . H23 . 109.8 no H21 . C2 . H23 . 109.5 no H22 . C2 . H23 . 108.4 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C20 . H202 . O2 . 122.00 0.96 2.41 3.041(4) yes C21 . H212 . O2 . 121.00 0.96 2.41 3.027(4) yes _iucr_refine_instruction_details_constraints ; # Punched on 24/06/11 at 16:09:21 # #LIST 12 BLOCK SCALE X'S, U'S CONT EXTPARAM RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 10,X'S) H ( 101,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 141,X'S) H ( 142,X'S) H ( 143,X'S) RIDE C ( 15,X'S) H ( 151,X'S) H ( 152,X'S) H ( 153,X'S) RIDE C ( 16,X'S) H ( 161,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 19,X'S) H ( 191,X'S) H ( 192,X'S) H ( 193,X'S) RIDE C ( 20,X'S) H ( 201,X'S) H ( 202,X'S) H ( 203,X'S) RIDE C ( 21,X'S) H ( 211,X'S) H ( 212,X'S) H ( 213,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 241,X'S) H ( 242,X'S) H ( 243,X'S) RIDE C ( 25,X'S) H ( 251,X'S) H ( 252,X'S) H ( 253,X'S) RIDE C ( 27,X'S) H ( 271,X'S) RIDE C ( 28,X'S) H ( 281,X'S) H ( 282,X'S) H ( 283,X'S) RIDE C ( 29,X'S) H ( 291,X'S) H ( 292,X'S) H ( 293,X'S) RIDE C ( 31,X'S) H ( 311,X'S) RIDE C ( 1,X'S) H ( 11,X'S) H ( 12,X'S) H ( 13,X'S) RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S) H ( 23,X'S) ;