# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Kongprakaiwoot, Natcharee' 'Armstrong, Jack' 'Noll, Bruce' 'Brown, Seth' _publ_contact_author_name 'Brown, Seth' _publ_contact_author_email seth.n.brown.114@nd.edu _publ_section_title ; Optically active bis(\^I^2^-diketonate) complexes of titanium ; # Attachment '- Tol2BobTiBINOL.cif' data_p43 _database_code_depnum_ccdc_archive 'CCDC 784598' #TrackingRef '- Tol2BobTiBINOL.cif' # Collected as bcn224 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (S,R,\D)-(2,2'-Biphenyl-bis(4-p-tolyl-2,4-butanedionato))(1,1'-bi-2- naphtholato)titanium(IV) ; _chemical_name_common (S,\D,R)-(Tol2Bob)Ti(BINOL) _chemical_melting_point ? _chemical_formula_moiety 'C54 H40 O6 Ti' _chemical_formula_sum 'C54 H40 O6 Ti' _chemical_formula_weight 832.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti .2776 .4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(3)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 13.8132(3) _cell_length_b 13.8132(3) _cell_length_c 21.5907(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4119.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9681 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 28.74 _exptl_crystal_description 'trigonal pyramid' _exptl_crystal_colour red _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method . _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 0.262 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8822 _exptl_absorpt_correction_T_max 0.9494 _exptl_absorpt_process_details ; Blessing, R. H. (1995) Acta Cryst. A51, 33-38. Sheldrick, G.M. (2008) SADABS v2008/1. Bruker AXS Inc. Madison, WI USA. ; _exptl_crystal_recrystallization_method ; Slow evaporation of ether solution. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8-ApexII CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 117265 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 31.55 _reflns_number_total 6907 _reflns_number_gt 6167 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)' _computing_structure_solution 'XS (Sheldrick, 2001)' _computing_structure_refinement 'XL (Sheldrick, 2001)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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^)+(0.0649P)^2^+0.6151P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary direct _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.002(18) _chemical_absolute_configuration rmad _refine_ls_number_reflns 6907 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0443 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.1005 _refine_ls_wR_factor_gt 0.0939 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 Ti Ti -0.816765(16) -0.816765(16) 0.0000 0.01686(7) Uani 1 2 d S . . O1 O -0.69660(7) -0.78470(7) -0.04783(4) 0.02040(19) Uani 1 1 d . . . O2 O -0.87864(7) -0.73636(7) -0.06484(4) 0.01963(19) Uani 1 1 d . . . O3 O -0.82722(7) -0.93981(7) -0.03529(4) 0.01903(18) Uani 1 1 d . . . C1 C -0.57192(10) -0.68998(11) -0.09353(6) 0.0229(3) Uani 1 1 d . . . H1B H -0.5451(13) -0.7449(14) -0.1177(8) 0.023(5) Uiso 1 1 d . . . H1A H -0.5697(13) -0.6310(13) -0.1229(8) 0.021(4) Uiso 1 1 d . . . C2 C -0.67777(10) -0.70821(9) -0.07953(6) 0.0191(2) Uani 1 1 d . . . C3 C -0.74748(10) -0.64661(10) -0.10394(6) 0.0210(2) Uani 1 1 d . . . H3 H -0.7291(15) -0.6010(14) -0.1292(9) 0.028(5) Uiso 1 1 d . . . C4 C -0.84616(10) -0.66854(9) -0.10045(6) 0.0189(2) Uani 1 1 d . . . C11 C -0.52353(10) -0.59902(11) 0.00511(7) 0.0241(3) Uani 1 1 d . . . C12 C -0.51031(9) -0.67719(11) -0.03557(6) 0.0225(2) Uani 1 1 d . . . C13 C -0.43797(11) -0.74512(13) -0.02305(7) 0.0292(3) Uani 1 1 d . . . H13 H -0.4250(15) -0.8036(16) -0.0496(9) 0.033(5) Uiso 1 1 d . . . C14 C -0.37824(12) -0.73488(16) 0.02845(8) 0.0368(4) Uani 1 1 d . . . H14 H -0.329(2) -0.778(2) 0.0348(12) 0.060(7) Uiso 1 1 d . . . C15 C -0.39042(12) -0.65813(16) 0.06777(8) 0.0381(4) Uani 1 1 d . . . H15 H -0.3537(15) -0.6491(15) 0.1025(9) 0.033(5) Uiso 1 1 d . . . C16 C -0.46210(12) -0.59029(14) 0.05634(8) 0.0318(3) Uani 1 1 d . . . H16 H -0.4695(14) -0.5375(15) 0.0856(9) 0.029(5) Uiso 1 1 d . . . C20 C -0.91340(15) -1.17205(12) 0.07437(8) 0.0348(4) Uani 1 1 d . . . C21 C -0.95648(10) -1.02799(9) 0.01172(6) 0.0210(2) Uani 1 1 d . . . C22 C -0.85924(10) -1.01730(9) -0.00226(6) 0.0199(2) Uani 1 1 d . . . C23 C -0.78963(12) -1.08581(11) 0.01795(7) 0.0257(3) Uani 1 1 d . . . H23 H -0.7214(15) -1.0744(14) 0.0084(9) 0.029(5) Uiso 1 1 d . . . C24 C -0.81690(15) -1.16108(11) 0.05480(8) 0.0339(3) Uani 1 1 d . . . H24 H -0.771(2) -1.207(2) 0.0627(12) 0.062(8) Uiso 1 1 d . . . C25 C -0.9417(2) -1.24580(15) 0.11661(10) 0.0483(5) Uani 1 1 d . . . H25 H -0.899(2) -1.285(3) 0.1309(16) 0.086(11) Uiso 1 1 d . . . C26 C -1.0340(2) -1.25415(16) 0.13652(11) 0.0586(7) Uani 1 1 d . . . H26 H -1.0564(19) -1.300(2) 0.1734(12) 0.059(7) Uiso 1 1 d . . . C27 C -1.10539(19) -1.18950(15) 0.11345(11) 0.0520(6) Uani 1 1 d . . . H27 H -1.170(2) -1.195(2) 0.1204(15) 0.083(10) Uiso 1 1 d . . . C28 C -1.08119(15) -1.11715(13) 0.07283(9) 0.0373(4) Uani 1 1 d . . . H28 H -1.1308(15) -1.0738(16) 0.0620(9) 0.031(5) Uiso 1 1 d . . . C29 C -0.98440(12) -1.10569(11) 0.05209(7) 0.0281(3) Uani 1 1 d . . . C31 C -0.91705(10) -0.62201(11) -0.14200(6) 0.0218(3) Uani 1 1 d . . . C32 C -0.90058(11) -0.53128(11) -0.16846(7) 0.0268(3) Uani 1 1 d . . . H32 H -0.8437(16) -0.4957(14) -0.1544(9) 0.031(5) Uiso 1 1 d . . . C33 C -0.96522(12) -0.49405(13) -0.21240(7) 0.0311(3) Uani 1 1 d . . . H33 H -0.9548(15) -0.4295(16) -0.2322(8) 0.031(5) Uiso 1 1 d . . . C34 C -1.04634(12) -0.54737(13) -0.23041(7) 0.0329(4) Uani 1 1 d . . . C35 C -1.06304(12) -0.63679(14) -0.20279(8) 0.0332(3) Uani 1 1 d . . . H35 H -1.1201(16) -0.6717(16) -0.2146(10) 0.038(5) Uiso 1 1 d . . . C36 C -0.99987(11) -0.67403(12) -0.15870(7) 0.0269(3) Uani 1 1 d . . . H36 H -1.0113(15) -0.7386(15) -0.1411(9) 0.028(5) Uiso 1 1 d . . . C37 C -1.11564(17) -0.50938(19) -0.27840(9) 0.0455(5) Uani 1 1 d . . . H37A H -1.135(3) -0.562(3) -0.3044(17) 0.095(12) Uiso 1 1 d . . . H37B H -1.085(3) -0.475(3) -0.3069(16) 0.089(11) Uiso 1 1 d . . . H37C H -1.165(3) -0.477(3) -0.2588(17) 0.100(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti 0.01595(9) 0.01595(9) 0.01869(13) 0.00152(8) -0.00152(8) 0.00021(11) O1 0.0184(4) 0.0193(4) 0.0234(4) 0.0026(3) -0.0005(3) 0.0003(3) O2 0.0173(4) 0.0199(4) 0.0217(4) 0.0036(3) -0.0008(3) 0.0003(3) O3 0.0186(4) 0.0172(4) 0.0213(4) 0.0011(3) -0.0005(3) -0.0006(3) C1 0.0192(6) 0.0290(7) 0.0205(6) -0.0004(5) 0.0022(4) -0.0026(5) C2 0.0190(5) 0.0214(5) 0.0170(5) -0.0018(4) 0.0004(4) -0.0020(5) C3 0.0215(6) 0.0214(6) 0.0202(6) 0.0034(5) -0.0005(5) -0.0016(5) C4 0.0212(6) 0.0167(6) 0.0189(5) 0.0003(4) -0.0006(4) 0.0019(4) C11 0.0203(6) 0.0307(7) 0.0212(6) 0.0029(5) -0.0002(5) -0.0064(5) C12 0.0177(5) 0.0285(7) 0.0214(6) 0.0032(5) 0.0013(4) -0.0038(5) C13 0.0194(6) 0.0372(8) 0.0311(7) 0.0062(6) 0.0027(5) 0.0004(6) C14 0.0205(7) 0.0532(11) 0.0366(8) 0.0102(8) -0.0026(6) 0.0025(7) C15 0.0217(7) 0.0651(13) 0.0276(7) 0.0051(7) -0.0055(6) -0.0064(7) C16 0.0262(7) 0.0447(9) 0.0246(7) -0.0022(6) -0.0033(6) -0.0094(6) C20 0.0555(11) 0.0185(7) 0.0303(7) 0.0022(6) 0.0013(7) -0.0040(7) C21 0.0245(6) 0.0165(5) 0.0220(6) -0.0017(4) 0.0012(5) -0.0026(5) C22 0.0232(6) 0.0171(5) 0.0193(5) 0.0008(5) -0.0014(5) 0.0003(4) C23 0.0288(7) 0.0201(6) 0.0281(7) -0.0002(5) -0.0038(5) 0.0041(5) C24 0.0481(9) 0.0214(6) 0.0321(7) 0.0034(5) -0.0075(7) 0.0056(7) C25 0.0795(16) 0.0255(8) 0.0399(10) 0.0089(7) 0.0065(10) -0.0039(9) C26 0.097(2) 0.0306(9) 0.0484(12) 0.0097(9) 0.0226(12) -0.0166(11) C27 0.0686(14) 0.0304(9) 0.0569(12) -0.0034(9) 0.0335(11) -0.0182(10) C28 0.0452(10) 0.0239(7) 0.0428(9) -0.0051(6) 0.0203(8) -0.0106(7) C29 0.0393(8) 0.0185(6) 0.0265(6) -0.0032(5) 0.0074(6) -0.0072(6) C31 0.0219(6) 0.0249(7) 0.0187(6) 0.0044(5) -0.0001(5) 0.0036(5) C32 0.0253(7) 0.0266(7) 0.0285(7) 0.0067(5) 0.0013(5) 0.0047(5) C33 0.0328(8) 0.0323(8) 0.0282(7) 0.0103(6) 0.0036(6) 0.0114(6) C34 0.0299(8) 0.0436(9) 0.0252(7) 0.0071(6) -0.0013(6) 0.0133(7) C35 0.0265(7) 0.0420(9) 0.0311(7) 0.0066(7) -0.0079(6) 0.0025(7) C36 0.0235(6) 0.0320(7) 0.0252(6) 0.0058(6) -0.0030(5) 0.0005(6) C37 0.0478(11) 0.0556(12) 0.0329(9) 0.0108(9) -0.0107(8) 0.0165(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti O3 1.8682(10) . y Ti O3 1.8682(10) 7 ? Ti O2 1.9808(9) 7 ? Ti O2 1.9808(9) . y Ti O1 2.0044(10) . y Ti O1 2.0044(10) 7 ? O1 C2 1.2855(15) . ? O2 C4 1.2923(16) . ? O3 C22 1.3601(16) . ? C1 C2 1.5142(18) . ? C1 C12 1.5237(19) . ? C1 H1B 0.992(19) . ? C1 H1A 1.033(18) . ? C2 C3 1.3888(19) . ? C3 C4 1.3984(19) . ? C3 H3 0.87(2) . ? C4 C31 1.4753(18) . ? C11 C16 1.399(2) . ? C11 C12 1.404(2) . ? C11 C11 1.491(3) 7 ? C12 C13 1.397(2) . ? C13 C14 1.392(2) . ? C13 H13 1.01(2) . ? C14 C15 1.369(3) . ? C14 H14 0.92(3) . ? C15 C16 1.385(3) . ? C15 H15 0.91(2) . ? C16 H16 0.97(2) . ? C20 C24 1.406(3) . ? C20 C25 1.422(2) . ? C20 C29 1.426(3) . ? C21 C22 1.3845(19) . ? C21 C29 1.4354(19) . ? C21 C21 1.486(3) 7 ? C22 C23 1.4179(19) . ? C23 C24 1.362(2) . ? C23 H23 0.98(2) . ? C24 H24 0.92(3) . ? C25 C26 1.350(4) . ? C25 H25 0.86(3) . ? C26 C27 1.421(4) . ? C26 H26 1.06(3) . ? C27 C28 1.371(3) . ? C27 H27 0.91(3) . ? C28 C29 1.419(2) . ? C28 H28 0.94(2) . ? C31 C32 1.396(2) . ? C31 C36 1.398(2) . ? C32 C33 1.401(2) . ? C32 H32 0.98(2) . ? C33 C34 1.396(3) . ? C33 H33 1.00(2) . ? C34 C35 1.391(3) . ? C34 C37 1.505(2) . ? C35 C36 1.390(2) . ? C35 H35 0.96(2) . ? C36 H36 0.98(2) . ? C37 H37A 0.95(4) . ? C37 H37B 0.89(4) . ? C37 H37C 0.92(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ti O3 91.47(6) . 7 y O3 Ti O2 86.50(4) . 7 y O3 Ti O2 100.87(4) 7 7 ? O3 Ti O2 100.87(4) . . y O3 Ti O2 86.50(4) 7 . y O2 Ti O2 169.51(6) 7 . y O3 Ti O1 93.15(4) . . y O3 Ti O1 168.69(4) 7 . y O2 Ti O1 89.72(4) 7 . y O2 Ti O1 82.49(4) . . y O3 Ti O1 168.69(4) . 7 ? O3 Ti O1 93.15(4) 7 7 ? O2 Ti O1 82.49(4) 7 7 ? O2 Ti O1 89.72(4) . 7 ? O1 Ti O1 84.23(6) . 7 ? C2 O1 Ti 128.57(9) . . y C4 O2 Ti 132.62(9) . . y C22 O3 Ti 121.82(8) . . y C2 C1 C12 113.24(10) . . ? C2 C1 H1B 109.8(11) . . ? C12 C1 H1B 108.2(11) . . ? C2 C1 H1A 106.4(10) . . ? C12 C1 H1A 113.3(10) . . ? H1B C1 H1A 105.6(14) . . ? O1 C2 C3 124.42(12) . . ? O1 C2 C1 116.00(12) . . ? C3 C2 C1 119.46(12) . . ? C2 C3 C4 121.51(12) . . ? C2 C3 H3 118.6(14) . . ? C4 C3 H3 118.3(14) . . ? O2 C4 C3 121.84(12) . . ? O2 C4 C31 116.56(12) . . ? C3 C4 C31 121.32(12) . . ? C16 C11 C12 118.81(14) . . ? C16 C11 C11 118.73(15) . 7 ? C12 C11 C11 122.44(14) . 7 ? C13 C12 C11 119.25(13) . . ? C13 C12 C1 118.72(14) . . ? C11 C12 C1 122.03(13) . . ? C14 C13 C12 120.68(16) . . ? C14 C13 H13 115.5(12) . . ? C12 C13 H13 123.8(12) . . ? C15 C14 C13 120.10(17) . . ? C15 C14 H14 120.3(16) . . ? C13 C14 H14 119.5(16) . . ? C14 C15 C16 120.08(16) . . ? C14 C15 H15 123.2(13) . . ? C16 C15 H15 116.7(13) . . ? C15 C16 C11 121.07(17) . . ? C15 C16 H16 117.9(11) . . ? C11 C16 H16 121.1(11) . . ? C24 C20 C25 122.05(19) . . ? C24 C20 C29 118.77(14) . . ? C25 C20 C29 119.16(19) . . ? C22 C21 C29 118.22(13) . . ? C22 C21 C21 119.98(10) . 7 ? C29 C21 C21 121.69(11) . 7 ? O3 C22 C21 120.92(12) . . ? O3 C22 C23 117.78(12) . . ? C21 C22 C23 121.30(13) . . ? C24 C23 C22 120.11(15) . . ? C24 C23 H23 120.9(12) . . ? C22 C23 H23 118.8(12) . . ? C23 C24 C20 121.31(15) . . ? C23 C24 H24 116.7(17) . . ? C20 C24 H24 121.7(17) . . ? C26 C25 C20 121.7(2) . . ? C26 C25 H25 119(2) . . ? C20 C25 H25 119(2) . . ? C25 C26 C27 119.33(18) . . ? C25 C26 H26 124.4(15) . . ? C27 C26 H26 115.7(15) . . ? C28 C27 C26 120.9(2) . . ? C28 C27 H27 114(2) . . ? C26 C27 H27 125(2) . . ? C27 C28 C29 120.9(2) . . ? C27 C28 H28 116.5(13) . . ? C29 C28 H28 122.5(13) . . ? C28 C29 C20 118.03(15) . . ? C28 C29 C21 121.89(16) . . ? C20 C29 C21 120.04(15) . . ? C32 C31 C36 119.28(13) . . ? C32 C31 C4 122.13(13) . . ? C36 C31 C4 118.43(13) . . ? C31 C32 C33 120.20(15) . . ? C31 C32 H32 117.2(12) . . ? C33 C32 H32 122.6(12) . . ? C32 C33 C34 120.44(15) . . ? C32 C33 H33 121.8(12) . . ? C34 C33 H33 117.8(12) . . ? C35 C34 C33 118.83(14) . . ? C35 C34 C37 119.95(18) . . ? C33 C34 C37 121.22(17) . . ? C36 C35 C34 121.21(16) . . ? C36 C35 H35 120.8(13) . . ? C34 C35 H35 117.9(13) . . ? C35 C36 C31 120.00(15) . . ? C35 C36 H36 120.0(12) . . ? C31 C36 H36 119.9(12) . . ? C34 C37 H37A 108(2) . . ? C34 C37 H37B 111(2) . . ? H37A C37 H37B 98(3) . . ? C34 C37 H37C 109(2) . . ? H37A C37 H37C 116(3) . . ? H37B C37 H37C 114(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 31.55 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max .379 _refine_diff_density_min -.166 _refine_diff_density_rms .052 # Attachment '- bistrif.cif' data_bistrif _database_code_depnum_ccdc_archive 'CCDC 784599' #TrackingRef '- bistrif.cif' # collected as bcn284 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (2,2'-Biphenyl-bis(4-p-tolyl-2,4-butanedionato))- bis(trifluoromethanesulfonato)titanium(IV) dideuterochloroform solvate ; _chemical_name_common '(Tol2Bob)Ti(OTf)2 . 2 CDCl3' _chemical_melting_point ? _chemical_formula_moiety 'C36 H28 F6 O10 S2 Ti, 2 (C D Cl3)' _chemical_formula_sum 'C38 H28 D2 Cl6 F6 O10 S2 Ti' _chemical_formula_weight 1087.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti .2776 .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 11.1948(5) _cell_length_b 14.8069(7) _cell_length_c 16.0008(8) _cell_angle_alpha 62.997(2) _cell_angle_beta 71.233(3) _cell_angle_gamma 78.832(3) _cell_volume 2233.95(18) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7920 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 31.44 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.617 _exptl_crystal_density_method . _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 0.724 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8236 _exptl_absorpt_correction_T_max 0.9661 _exptl_absorpt_process_details ; Blessing, R. H. (1995) Acta Cryst. A51, 33-38. Sheldrick, G.M. (2008) SADABS v2008/1. Bruker AXS Inc. Madison, WI USA. ; _exptl_crystal_recrystallization_method ; Spontaneous crystallization from reaction of (Tol2Bob)Ti(BINOL) with HOTf in CDCl3 solution ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8-ApexII CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 93398 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 31.65 _reflns_number_total 14774 _reflns_number_gt 11437 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)' _computing_structure_solution 'XS (Sheldrick, 2001)' _computing_structure_refinement 'XL (Sheldrick, 2001)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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. One of the CDCl3 molecules of solvation was disordered over two orientations, with the major orientation refining to 81.87(10)% occupancy. Corresponding chlorines in the two orientations were constrained to have identical thermal parameters during refinement. ; _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^)+(0.0494P)^2^+1.8598P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14774 _refine_ls_number_parameters 698 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0617 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1107 _refine_ls_wR_factor_gt 0.1008 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 Ti Ti -0.87655(3) -0.80321(2) -0.31103(2) 0.01505(6) Uani 1 1 d . . . S1 S -0.65048(4) -0.66522(3) -0.48318(3) 0.01729(8) Uani 1 1 d . . . S2 S -0.80021(4) -1.04215(3) -0.26621(3) 0.02033(9) Uani 1 1 d . . . O1 O -1.03708(11) -0.85463(9) -0.22326(8) 0.0182(2) Uani 1 1 d . . . O2 O -0.82329(10) -0.84577(9) -0.19571(8) 0.0168(2) Uani 1 1 d . . . O3 O -0.93536(11) -0.67697(9) -0.30095(8) 0.0171(2) Uani 1 1 d . . . O4 O -0.95069(11) -0.74989(9) -0.41728(8) 0.0164(2) Uani 1 1 d . . . O5 O -0.70504(11) -0.75616(9) -0.39426(8) 0.0195(2) Uani 1 1 d . . . O6 O -0.82542(11) -0.93242(9) -0.32645(9) 0.0197(2) Uani 1 1 d . . . O11 O -0.54119(15) -0.63634(13) -0.47666(11) 0.0371(4) Uani 1 1 d . . . O12 O -0.74509(13) -0.58896(10) -0.51660(10) 0.0280(3) Uani 1 1 d . . . O21 O -0.85055(16) -1.10549(12) -0.29068(15) 0.0448(4) Uani 1 1 d . . . O22 O -0.82159(14) -1.06559(11) -0.16596(10) 0.0342(3) Uani 1 1 d . . . F11 F -0.52175(17) -0.80015(11) -0.54522(11) 0.0609(5) Uani 1 1 d . . . F12 F -0.69049(15) -0.73708(13) -0.59230(11) 0.0500(4) Uani 1 1 d . . . F13 F -0.52725(12) -0.64860(10) -0.65653(8) 0.0348(3) Uani 1 1 d . . . F21 F -0.58705(12) -1.14850(10) -0.26556(10) 0.0389(3) Uani 1 1 d . . . F22 F -0.57521(11) -0.99122(10) -0.29948(11) 0.0405(3) Uani 1 1 d . . . F23 F -0.59651(14) -1.03138(12) -0.40672(9) 0.0477(4) Uani 1 1 d . . . C1 C -1.22891(14) -0.86369(12) -0.10175(12) 0.0161(3) Uani 1 1 d . . . C2 C -1.08739(14) -0.85908(12) -0.13639(11) 0.0156(3) Uani 1 1 d . . . C3 C -1.01820(15) -0.86047(12) -0.07791(12) 0.0169(3) Uani 1 1 d . . . C4 C -0.88573(15) -0.85774(12) -0.10807(11) 0.0154(3) Uani 1 1 d . . . C5 C -1.07657(15) -0.54189(12) -0.28144(11) 0.0159(3) Uani 1 1 d . . . C6 C -1.02941(14) -0.61526(11) -0.32782(11) 0.0142(3) Uani 1 1 d . . . C7 C -1.08338(15) -0.61471(12) -0.39446(11) 0.0157(3) Uani 1 1 d . . . C8 C -1.03872(14) -0.67972(11) -0.44147(11) 0.0143(3) Uani 1 1 d . . . C10 C -0.59380(19) -0.71695(14) -0.57383(14) 0.0267(4) Uani 1 1 d . . . C11 C -1.29823(14) -0.67423(12) -0.17467(11) 0.0158(3) Uani 1 1 d . . . C12 C -1.29498(14) -0.77275(12) -0.16843(11) 0.0156(3) Uani 1 1 d . . . C13 C -1.35341(16) -0.78757(13) -0.22563(12) 0.0199(3) Uani 1 1 d . . . C14 C -1.41836(16) -0.70800(15) -0.28617(13) 0.0234(3) Uani 1 1 d . . . C15 C -1.42625(16) -0.61219(14) -0.28874(13) 0.0233(3) Uani 1 1 d . . . C16 C -1.36632(15) -0.59548(13) -0.23385(12) 0.0200(3) Uani 1 1 d . . . C20 C -0.62931(17) -1.05354(14) -0.31318(14) 0.0257(4) Uani 1 1 d . . . C21 C -1.22708(15) -0.65319(12) -0.12130(11) 0.0157(3) Uani 1 1 d . . . C22 C -1.11996(15) -0.59463(12) -0.17100(11) 0.0159(3) Uani 1 1 d . . . C23 C -1.05030(17) -0.58530(13) -0.11722(13) 0.0212(3) Uani 1 1 d . . . C24 C -1.0867(2) -0.63012(15) -0.01612(14) 0.0260(4) Uani 1 1 d . . . C25 C -1.19545(19) -0.68406(14) 0.03296(13) 0.0253(4) Uani 1 1 d . . . C26 C -1.26442(17) -0.69544(13) -0.01965(12) 0.0209(3) Uani 1 1 d . . . C31 C -0.81116(14) -0.86885(12) -0.04316(11) 0.0162(3) Uani 1 1 d . . . C32 C -0.67909(16) -0.87289(14) -0.07613(12) 0.0210(3) Uani 1 1 d . . . C33 C -0.60670(17) -0.88474(15) -0.01573(13) 0.0242(3) Uani 1 1 d . . . C34 C -0.66273(16) -0.89168(13) 0.07819(12) 0.0205(3) Uani 1 1 d . . . C35 C -0.79457(17) -0.88629(13) 0.11047(13) 0.0211(3) Uani 1 1 d . . . C36 C -0.86827(16) -0.87519(13) 0.05112(12) 0.0190(3) Uani 1 1 d . . . C37 C -0.5830(2) -0.90373(17) 0.14265(15) 0.0291(4) Uani 1 1 d . . . C41 C -1.08590(14) -0.67101(12) -0.52022(11) 0.0149(3) Uani 1 1 d . . . C42 C -1.02306(15) -0.72661(13) -0.57467(12) 0.0181(3) Uani 1 1 d . . . C43 C -1.06506(17) -0.71768(14) -0.65061(13) 0.0215(3) Uani 1 1 d . . . C44 C -1.17005(16) -0.65350(13) -0.67464(12) 0.0210(3) Uani 1 1 d . . . C45 C -1.23342(16) -0.59999(14) -0.61908(13) 0.0211(3) Uani 1 1 d . . . C46 C -1.19294(15) -0.60826(13) -0.54253(12) 0.0175(3) Uani 1 1 d . . . C47 C -1.2130(2) -0.64337(18) -0.75841(15) 0.0295(4) Uani 1 1 d . . . H1A H -1.2568(19) -0.8709(15) -0.0343(15) 0.016(5) Uiso 1 1 d . . . H1B H -1.248(2) -0.9246(16) -0.1035(15) 0.020(5) Uiso 1 1 d . . . H3 H -1.062(2) -0.8651(17) -0.0154(17) 0.023(5) Uiso 1 1 d . . . H5A H -1.1427(19) -0.4992(15) -0.3090(15) 0.015(5) Uiso 1 1 d . . . H5B H -1.007(2) -0.5004(16) -0.2998(15) 0.020(5) Uiso 1 1 d . . . H7 H -1.149(2) -0.5674(17) -0.4095(16) 0.021(5) Uiso 1 1 d . . . H13 H -1.349(2) -0.8547(17) -0.2221(16) 0.023(5) Uiso 1 1 d . . . H14 H -1.458(2) -0.7205(18) -0.3249(17) 0.028(6) Uiso 1 1 d . . . H15 H -1.470(2) -0.557(2) -0.3303(19) 0.037(7) Uiso 1 1 d . . . H16 H -1.371(2) -0.5262(17) -0.2379(16) 0.023(5) Uiso 1 1 d . . . H23 H -0.977(2) -0.5450(17) -0.1533(16) 0.022(5) Uiso 1 1 d . . . H24 H -1.038(2) -0.6241(19) 0.0191(19) 0.038(7) Uiso 1 1 d . . . H25 H -1.223(2) -0.7136(17) 0.0993(17) 0.023(5) Uiso 1 1 d . . . H26 H -1.335(2) -0.7328(15) 0.0120(15) 0.015(5) Uiso 1 1 d . . . H32 H -0.640(2) -0.8679(17) -0.1405(17) 0.027(6) Uiso 1 1 d . . . H33 H -0.520(2) -0.8864(19) -0.0382(18) 0.035(6) Uiso 1 1 d . . . H35 H -0.837(2) -0.8917(17) 0.1746(17) 0.027(6) Uiso 1 1 d . . . H36 H -0.958(2) -0.8720(17) 0.0751(16) 0.025(6) Uiso 1 1 d . . . H37A H -0.613(3) -0.953(2) 0.208(2) 0.058(9) Uiso 1 1 d . . . H37B H -0.497(4) -0.925(3) 0.120(3) 0.080(11) Uiso 1 1 d . . . H37C H -0.577(3) -0.843(3) 0.144(3) 0.071(10) Uiso 1 1 d . . . H42 H -0.950(2) -0.7696(16) -0.5596(15) 0.018(5) Uiso 1 1 d . . . H43 H -1.021(2) -0.7561(17) -0.6862(17) 0.026(6) Uiso 1 1 d . . . H45 H -1.311(2) -0.5563(17) -0.6325(16) 0.025(6) Uiso 1 1 d . . . H46 H -1.237(2) -0.5713(17) -0.5077(16) 0.022(5) Uiso 1 1 d . . . H47A H -1.262(3) -0.701(3) -0.739(2) 0.069(10) Uiso 1 1 d . . . H47B H -1.146(3) -0.643(2) -0.810(2) 0.058(9) Uiso 1 1 d . . . H47C H -1.268(3) -0.585(3) -0.781(2) 0.067(10) Uiso 1 1 d . . . C01 C -0.6840(2) -0.58778(17) 0.07272(17) 0.0378(5) Uani 1 1 d . . . D01 H -0.709(2) -0.5167(19) 0.0544(18) 0.032(6) Uiso 1 1 d . . . Cl1 Cl -0.80909(9) -0.65990(6) 0.16025(9) 0.0796(4) Uani 0.8187(10) 1 d P A 1 Cl2 Cl -0.55373(9) -0.61573(7) 0.12539(6) 0.0531(2) Uani 0.8187(10) 1 d P A 1 Cl3 Cl -0.63151(11) -0.61455(6) -0.02871(6) 0.0527(2) Uani 0.8187(10) 1 d P A 1 Cl11 Cl -0.5795(5) -0.5848(3) -0.0342(4) 0.0796(4) Uani 0.1813(10) 1 d P A 2 Cl21 Cl -0.8301(4) -0.6416(3) 0.0870(3) 0.0531(2) Uani 0.1813(10) 1 d P A 2 Cl31 Cl -0.6388(5) -0.6413(3) 0.1713(3) 0.0527(2) Uani 0.1813(10) 1 d P A 2 C02 C -0.19111(17) 0.04659(15) -0.44983(14) 0.0256(4) Uani 1 1 d . . . D02 H -0.1549(19) 0.0753(16) -0.5173(15) 0.016(5) Uiso 1 1 d . . . Cl4 Cl -0.31029(5) 0.13491(4) -0.42650(4) 0.03820(12) Uani 1 1 d . . . Cl5 Cl -0.07437(5) 0.02609(5) -0.39009(4) 0.03874(12) Uani 1 1 d . . . Cl6 Cl -0.25542(5) -0.06908(4) -0.41381(4) 0.03526(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti 0.01351(12) 0.01648(13) 0.01306(12) -0.00554(10) -0.00448(9) 0.00352(10) S1 0.01759(17) 0.01709(18) 0.01601(18) -0.00585(15) -0.00498(14) -0.00049(14) S2 0.01507(17) 0.01549(18) 0.0261(2) -0.00551(16) -0.00570(15) 0.00060(13) O1 0.0152(5) 0.0227(6) 0.0167(5) -0.0092(5) -0.0042(4) 0.0007(4) O2 0.0146(5) 0.0193(5) 0.0134(5) -0.0047(4) -0.0045(4) 0.0015(4) O3 0.0160(5) 0.0194(5) 0.0173(5) -0.0090(5) -0.0066(4) 0.0029(4) O4 0.0163(5) 0.0168(5) 0.0157(5) -0.0070(4) -0.0061(4) 0.0033(4) O5 0.0156(5) 0.0197(6) 0.0159(5) -0.0030(5) -0.0034(4) 0.0020(4) O6 0.0190(5) 0.0174(5) 0.0203(6) -0.0074(5) -0.0062(4) 0.0041(4) O11 0.0347(8) 0.0504(9) 0.0269(7) -0.0085(7) -0.0096(6) -0.0217(7) O12 0.0295(7) 0.0179(6) 0.0267(7) -0.0050(5) -0.0065(5) 0.0074(5) O21 0.0430(9) 0.0241(7) 0.0782(13) -0.0176(8) -0.0364(9) -0.0008(6) O22 0.0348(7) 0.0260(7) 0.0204(6) 0.0001(5) 0.0022(6) 0.0027(6) F11 0.0794(11) 0.0384(8) 0.0364(8) -0.0145(6) -0.0030(7) 0.0338(8) F12 0.0563(9) 0.0671(10) 0.0446(8) -0.0383(8) -0.0011(7) -0.0262(8) F13 0.0362(6) 0.0395(7) 0.0180(5) -0.0085(5) 0.0024(5) -0.0049(5) F21 0.0307(6) 0.0297(6) 0.0431(7) -0.0086(6) -0.0140(5) 0.0171(5) F22 0.0227(6) 0.0392(7) 0.0547(8) -0.0092(6) -0.0170(6) -0.0069(5) F23 0.0458(8) 0.0543(9) 0.0247(6) -0.0162(6) -0.0019(5) 0.0229(7) C1 0.0143(6) 0.0148(7) 0.0168(7) -0.0049(6) -0.0036(5) -0.0010(5) C2 0.0155(6) 0.0122(6) 0.0158(7) -0.0039(6) -0.0041(5) 0.0009(5) C3 0.0153(7) 0.0182(7) 0.0153(7) -0.0059(6) -0.0042(5) 0.0006(5) C4 0.0159(6) 0.0129(6) 0.0145(7) -0.0034(6) -0.0048(5) 0.0007(5) C5 0.0178(7) 0.0146(7) 0.0139(7) -0.0055(6) -0.0035(5) -0.0002(5) C6 0.0142(6) 0.0128(6) 0.0119(6) -0.0034(5) -0.0014(5) -0.0007(5) C7 0.0149(6) 0.0155(7) 0.0154(7) -0.0064(6) -0.0053(5) 0.0035(5) C8 0.0129(6) 0.0139(6) 0.0136(7) -0.0039(5) -0.0037(5) 0.0000(5) C10 0.0306(9) 0.0228(8) 0.0213(8) -0.0092(7) -0.0017(7) 0.0012(7) C11 0.0128(6) 0.0172(7) 0.0145(7) -0.0060(6) -0.0011(5) -0.0004(5) C12 0.0121(6) 0.0170(7) 0.0146(7) -0.0052(6) -0.0021(5) -0.0003(5) C13 0.0180(7) 0.0214(8) 0.0201(8) -0.0080(6) -0.0049(6) -0.0031(6) C14 0.0192(7) 0.0305(9) 0.0207(8) -0.0081(7) -0.0084(6) -0.0031(7) C15 0.0177(7) 0.0251(8) 0.0205(8) -0.0037(7) -0.0072(6) 0.0018(6) C16 0.0171(7) 0.0186(8) 0.0197(8) -0.0064(6) -0.0032(6) 0.0018(6) C20 0.0198(8) 0.0255(9) 0.0238(9) -0.0067(7) -0.0059(7) 0.0070(7) C21 0.0175(7) 0.0138(7) 0.0141(7) -0.0060(6) -0.0028(5) 0.0010(5) C22 0.0180(7) 0.0144(7) 0.0150(7) -0.0071(6) -0.0041(5) 0.0016(5) C23 0.0238(8) 0.0211(8) 0.0200(8) -0.0094(7) -0.0058(6) -0.0024(6) C24 0.0368(10) 0.0260(9) 0.0201(8) -0.0108(7) -0.0113(7) -0.0032(7) C25 0.0388(10) 0.0222(8) 0.0138(7) -0.0066(7) -0.0055(7) -0.0043(7) C26 0.0254(8) 0.0179(7) 0.0162(7) -0.0069(6) -0.0014(6) -0.0024(6) C31 0.0155(7) 0.0151(7) 0.0152(7) -0.0034(6) -0.0053(5) -0.0005(5) C32 0.0169(7) 0.0279(9) 0.0159(7) -0.0068(7) -0.0039(6) -0.0032(6) C33 0.0169(7) 0.0317(9) 0.0221(8) -0.0076(7) -0.0060(6) -0.0053(7) C34 0.0230(8) 0.0203(8) 0.0194(8) -0.0053(6) -0.0098(6) -0.0043(6) C35 0.0236(8) 0.0224(8) 0.0177(8) -0.0082(7) -0.0066(6) -0.0012(6) C36 0.0174(7) 0.0209(8) 0.0171(7) -0.0069(6) -0.0049(6) 0.0001(6) C37 0.0303(10) 0.0341(10) 0.0265(10) -0.0093(8) -0.0151(8) -0.0059(8) C41 0.0157(6) 0.0148(7) 0.0127(7) -0.0044(6) -0.0040(5) -0.0013(5) C42 0.0184(7) 0.0181(7) 0.0171(7) -0.0076(6) -0.0045(6) 0.0002(6) C43 0.0254(8) 0.0230(8) 0.0176(8) -0.0105(7) -0.0036(6) -0.0034(6) C44 0.0242(8) 0.0233(8) 0.0159(7) -0.0057(6) -0.0065(6) -0.0069(6) C45 0.0194(7) 0.0236(8) 0.0201(8) -0.0068(7) -0.0089(6) -0.0008(6) C46 0.0169(7) 0.0186(7) 0.0162(7) -0.0069(6) -0.0050(6) 0.0006(6) C47 0.0355(10) 0.0384(11) 0.0213(9) -0.0135(8) -0.0126(8) -0.0054(9) C01 0.0391(11) 0.0248(10) 0.0383(12) -0.0141(9) 0.0065(9) -0.0044(8) Cl1 0.0522(5) 0.0324(4) 0.1029(9) -0.0207(5) 0.0389(5) -0.0138(3) Cl2 0.0675(5) 0.0467(4) 0.0493(4) -0.0253(4) -0.0193(4) 0.0073(4) Cl3 0.0809(6) 0.0376(4) 0.0370(4) -0.0157(3) -0.0124(4) -0.0037(4) Cl11 0.0522(5) 0.0324(4) 0.1029(9) -0.0207(5) 0.0389(5) -0.0138(3) Cl21 0.0675(5) 0.0467(4) 0.0493(4) -0.0253(4) -0.0193(4) 0.0073(4) Cl31 0.0809(6) 0.0376(4) 0.0370(4) -0.0157(3) -0.0124(4) -0.0037(4) C02 0.0230(8) 0.0269(9) 0.0256(9) -0.0089(7) -0.0057(7) -0.0052(7) Cl4 0.0316(2) 0.0286(2) 0.0490(3) -0.0185(2) 0.0014(2) -0.00530(19) Cl5 0.0344(3) 0.0503(3) 0.0289(2) -0.0070(2) -0.0126(2) -0.0144(2) Cl6 0.0309(2) 0.0283(2) 0.0488(3) -0.0190(2) -0.0073(2) -0.00523(18) _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 Ti O4 1.9073(11) . ? Ti O2 1.9140(11) . ? Ti O3 1.9190(12) . ? Ti O1 1.9279(12) . ? Ti O6 1.9906(12) . ? Ti O5 1.9940(12) . ? S1 O11 1.4198(14) . ? S1 O12 1.4267(13) . ? S1 O5 1.4934(12) . ? S1 C10 1.8226(19) . ? S2 O22 1.4249(15) . ? S2 O21 1.4249(16) . ? S2 O6 1.4913(12) . ? S2 C20 1.8217(18) . ? O1 C2 1.2966(19) . ? O2 C4 1.2955(19) . ? O3 C6 1.3001(19) . ? O4 C8 1.2977(18) . ? F11 C10 1.311(2) . ? F12 C10 1.326(2) . ? F13 C10 1.331(2) . ? F21 C20 1.335(2) . ? F22 C20 1.324(2) . ? F23 C20 1.315(2) . ? C1 C2 1.505(2) . ? C1 C12 1.522(2) . ? C1 H1A 0.98(2) . ? C1 H1B 0.98(2) . ? C2 C3 1.385(2) . ? C3 C4 1.407(2) . ? C3 H3 0.94(2) . ? C4 C31 1.467(2) . ? C5 C6 1.506(2) . ? C5 C22 1.520(2) . ? C5 H5A 0.96(2) . ? C5 H5B 0.97(2) . ? C6 C7 1.381(2) . ? C7 C8 1.404(2) . ? C7 H7 0.92(2) . ? C8 C41 1.462(2) . ? C11 C16 1.398(2) . ? C11 C12 1.410(2) . ? C11 C21 1.495(2) . ? C12 C13 1.392(2) . ? C13 C14 1.393(2) . ? C13 H13 0.96(2) . ? C14 C15 1.387(3) . ? C14 H14 0.96(2) . ? C15 C16 1.387(3) . ? C15 H15 0.96(3) . ? C16 H16 0.99(2) . ? C21 C26 1.397(2) . ? C21 C22 1.409(2) . ? C22 C23 1.396(2) . ? C23 C24 1.389(3) . ? C23 H23 0.97(2) . ? C24 C25 1.389(3) . ? C24 H24 0.94(3) . ? C25 C26 1.389(3) . ? C25 H25 0.91(2) . ? C26 H26 0.92(2) . ? C31 C32 1.400(2) . ? C31 C36 1.403(2) . ? C32 C33 1.384(2) . ? C32 H32 0.95(2) . ? C33 C34 1.393(3) . ? C33 H33 0.92(3) . ? C34 C35 1.397(2) . ? C34 C37 1.502(2) . ? C35 C36 1.385(2) . ? C35 H35 0.96(2) . ? C36 H36 0.95(2) . ? C37 H37A 0.95(3) . ? C37 H37B 0.96(4) . ? C37 H37C 0.92(4) . ? C41 C42 1.401(2) . ? C41 C46 1.403(2) . ? C42 C43 1.383(2) . ? C42 H42 0.96(2) . ? C43 C44 1.400(3) . ? C43 H43 0.95(2) . ? C44 C45 1.392(3) . ? C44 C47 1.501(2) . ? C45 C46 1.386(2) . ? C45 H45 1.00(2) . ? C46 H46 0.92(2) . ? C47 H47A 0.98(4) . ? C47 H47B 0.92(3) . ? C47 H47C 0.95(4) . ? C01 Cl31 1.611(5) . ? C01 Cl11 1.720(5) . ? C01 Cl3 1.737(2) . ? C01 Cl1 1.739(2) . ? C01 Cl2 1.802(3) . ? C01 Cl21 1.861(5) . ? C01 D01 0.97(3) . ? C02 Cl4 1.754(2) . ? C02 Cl5 1.7608(19) . ? C02 Cl6 1.7602(19) . ? C02 D02 0.94(2) . ? 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 Ti O2 171.21(5) . . ? O4 Ti O3 85.63(5) . . ? O2 Ti O3 87.14(5) . . ? O4 Ti O1 89.23(5) . . ? O2 Ti O1 85.43(5) . . ? O3 Ti O1 87.24(5) . . ? O4 Ti O6 90.45(5) . . ? O2 Ti O6 96.62(5) . . ? O3 Ti O6 175.74(5) . . ? O1 Ti O6 91.05(5) . . ? O4 Ti O5 94.64(5) . . ? O2 Ti O5 90.85(5) . . ? O3 Ti O5 94.01(5) . . ? O1 Ti O5 176.02(5) . . ? O6 Ti O5 87.95(5) . . ? O11 S1 O12 119.11(10) . . ? O11 S1 O5 111.94(8) . . ? O12 S1 O5 112.49(8) . . ? O11 S1 C10 105.67(10) . . ? O12 S1 C10 104.20(9) . . ? O5 S1 C10 101.17(8) . . ? O22 S2 O21 118.48(11) . . ? O22 S2 O6 113.14(8) . . ? O21 S2 O6 111.57(9) . . ? O22 S2 C20 105.30(9) . . ? O21 S2 C20 105.87(10) . . ? O6 S2 C20 100.26(8) . . ? C2 O1 Ti 128.02(10) . . ? C4 O2 Ti 131.77(10) . . ? C6 O3 Ti 129.07(10) . . ? C8 O4 Ti 132.75(10) . . ? S1 O5 Ti 137.17(7) . . ? S2 O6 Ti 139.20(8) . . ? C2 C1 C12 112.30(13) . . ? C2 C1 H1A 108.6(12) . . ? C12 C1 H1A 112.4(12) . . ? C2 C1 H1B 106.2(13) . . ? C12 C1 H1B 107.7(13) . . ? H1A C1 H1B 109.4(17) . . ? O1 C2 C3 123.60(14) . . ? O1 C2 C1 115.06(14) . . ? C3 C2 C1 121.34(14) . . ? C2 C3 C4 122.41(15) . . ? C2 C3 H3 118.0(14) . . ? C4 C3 H3 119.6(13) . . ? O2 C4 C3 120.86(14) . . ? O2 C4 C31 116.58(13) . . ? C3 C4 C31 122.55(14) . . ? C6 C5 C22 112.87(13) . . ? C6 C5 H5A 107.1(12) . . ? C22 C5 H5A 112.2(12) . . ? C6 C5 H5B 107.4(13) . . ? C22 C5 H5B 108.5(13) . . ? H5A C5 H5B 108.6(17) . . ? O3 C6 C7 123.63(14) . . ? O3 C6 C5 115.15(13) . . ? C7 C6 C5 121.22(14) . . ? C6 C7 C8 122.57(14) . . ? C6 C7 H7 117.2(13) . . ? C8 C7 H7 120.2(13) . . ? O4 C8 C7 120.57(14) . . ? O4 C8 C41 116.94(13) . . ? C7 C8 C41 122.48(14) . . ? F11 C10 F12 108.87(18) . . ? F11 C10 F13 108.53(16) . . ? F12 C10 F13 107.78(16) . . ? F11 C10 S1 111.86(14) . . ? F12 C10 S1 110.29(13) . . ? F13 C10 S1 109.42(13) . . ? C16 C11 C12 118.98(15) . . ? C16 C11 C21 120.23(15) . . ? C12 C11 C21 120.77(14) . . ? C13 C12 C11 119.04(15) . . ? C13 C12 C1 118.62(14) . . ? C11 C12 C1 122.33(14) . . ? C14 C13 C12 121.40(16) . . ? C14 C13 H13 119.9(13) . . ? C12 C13 H13 118.7(13) . . ? C15 C14 C13 119.35(16) . . ? C15 C14 H14 121.2(14) . . ? C13 C14 H14 119.5(14) . . ? C16 C15 C14 120.05(16) . . ? C16 C15 H15 119.4(15) . . ? C14 C15 H15 120.5(16) . . ? C15 C16 C11 121.07(16) . . ? C15 C16 H16 118.9(13) . . ? C11 C16 H16 120.1(13) . . ? F23 C20 F22 108.73(17) . . ? F23 C20 F21 108.83(16) . . ? F22 C20 F21 108.58(16) . . ? F23 C20 S2 111.40(13) . . ? F22 C20 S2 109.82(13) . . ? F21 C20 S2 109.43(13) . . ? C26 C21 C22 118.93(15) . . ? C26 C21 C11 119.50(14) . . ? C22 C21 C11 121.52(14) . . ? C23 C22 C21 119.05(15) . . ? C23 C22 C5 118.66(14) . . ? C21 C22 C5 122.29(14) . . ? C24 C23 C22 121.26(16) . . ? C24 C23 H23 121.6(13) . . ? C22 C23 H23 117.2(13) . . ? C25 C24 C23 119.74(17) . . ? C25 C24 H24 120.1(16) . . ? C23 C24 H24 120.2(16) . . ? C24 C25 C26 119.57(16) . . ? C24 C25 H25 122.2(14) . . ? C26 C25 H25 118.2(14) . . ? C25 C26 C21 121.35(16) . . ? C25 C26 H26 120.4(13) . . ? C21 C26 H26 118.2(13) . . ? C32 C31 C36 118.85(15) . . ? C32 C31 C4 119.22(14) . . ? C36 C31 C4 121.93(14) . . ? C33 C32 C31 120.26(16) . . ? C33 C32 H32 120.6(14) . . ? C31 C32 H32 119.2(14) . . ? C32 C33 C34 121.21(16) . . ? C32 C33 H33 119.9(16) . . ? C34 C33 H33 118.8(16) . . ? C33 C34 C35 118.40(15) . . ? C33 C34 C37 120.62(16) . . ? C35 C34 C37 120.97(17) . . ? C36 C35 C34 121.05(16) . . ? C36 C35 H35 117.5(14) . . ? C34 C35 H35 121.5(14) . . ? C35 C36 C31 120.22(15) . . ? C35 C36 H36 119.3(14) . . ? C31 C36 H36 120.5(14) . . ? C34 C37 H37A 113.1(19) . . ? C34 C37 H37B 113(2) . . ? H37A C37 H37B 106(3) . . ? C34 C37 H37C 112(2) . . ? H37A C37 H37C 109(3) . . ? H37B C37 H37C 104(3) . . ? C42 C41 C46 119.16(14) . . ? C42 C41 C8 119.36(14) . . ? C46 C41 C8 121.48(14) . . ? C43 C42 C41 120.05(15) . . ? C43 C42 H42 120.6(13) . . ? C41 C42 H42 119.4(13) . . ? C42 C43 C44 121.08(16) . . ? C42 C43 H43 118.4(14) . . ? C44 C43 H43 120.5(14) . . ? C45 C44 C43 118.54(15) . . ? C45 C44 C47 121.09(17) . . ? C43 C44 C47 120.37(17) . . ? C46 C45 C44 121.16(16) . . ? C46 C45 H45 118.5(13) . . ? C44 C45 H45 120.3(13) . . ? C45 C46 C41 119.98(15) . . ? C45 C46 H46 118.8(14) . . ? C41 C46 H46 121.2(14) . . ? C44 C47 H47A 110(2) . . ? C44 C47 H47B 112(2) . . ? H47A C47 H47B 106(3) . . ? C44 C47 H47C 114(2) . . ? H47A C47 H47C 105(3) . . ? H47B C47 H47C 108(3) . . ? Cl31 C01 Cl11 119.3(3) . . ? Cl31 C01 Cl3 128.6(2) . . ? Cl11 C01 Cl3 25.3(2) . . ? Cl31 C01 Cl1 75.4(2) . . ? Cl11 C01 Cl1 136.8(2) . . ? Cl3 C01 Cl1 112.49(14) . . ? Cl31 C01 Cl2 33.96(18) . . ? Cl11 C01 Cl2 89.7(3) . . ? Cl3 C01 Cl2 107.78(13) . . ? Cl1 C01 Cl2 108.69(14) . . ? Cl31 C01 Cl21 111.7(2) . . ? Cl11 C01 Cl21 106.8(3) . . ? Cl3 C01 Cl21 81.77(17) . . ? Cl1 C01 Cl21 37.71(14) . . ? Cl2 C01 Cl21 141.96(19) . . ? Cl31 C01 D01 113.6(15) . . ? Cl11 C01 D01 101.2(15) . . ? Cl3 C01 D01 110.9(15) . . ? Cl1 C01 D01 109.2(15) . . ? Cl2 C01 D01 107.7(15) . . ? Cl21 C01 D01 102.5(15) . . ? Cl4 C02 Cl5 111.09(11) . . ? Cl4 C02 Cl6 110.59(10) . . ? Cl5 C02 Cl6 110.06(11) . . ? Cl4 C02 D02 105.9(13) . . ? Cl5 C02 D02 109.2(13) . . ? Cl6 C02 D02 109.9(13) . . ? _diffrn_measured_fraction_theta_max .981 _diffrn_reflns_theta_full 31.65 _diffrn_measured_fraction_theta_full .981 _refine_diff_density_max 1.305 _refine_diff_density_min -.969 _refine_diff_density_rms .073 # Attachment '- bobbinaptioipr2.cif' data_bobbi0 _database_code_depnum_ccdc_archive 'CCDC 784600' #TrackingRef '- bobbinaptioipr2.cif' # Collected as bcn343 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (R,\L)-(1,1'-Binaphthyl-2,2'-bis(4-p-tolyl-2,4-butanedionato))- diisopropoxytitanium(IV) ; _chemical_name_common (R,\L)-(Tol2Bobbinap)Ti(OiPr)2 _chemical_melting_point ? _chemical_formula_moiety 'C48 H46 O6 Ti' _chemical_formula_sum 'C48 H46 O6 Ti' _chemical_formula_weight 766.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti .2776 .4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) _symmetry_space_group_name_Hall '2 yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.6568(3) _cell_length_b 7.8240(2) _cell_length_c 21.7522(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.5330(16) _cell_angle_gamma 90.00 _cell_volume 1981.92(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9728 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 28.21 _exptl_crystal_description wedge _exptl_crystal_colour yellow _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method . _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.266 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9276 _exptl_absorpt_correction_T_max 0.9657 _exptl_absorpt_process_details ; Blessing, R. H. (1995) Acta Cryst. A51, 33-38. Sheldrick, G.M. (2008) SADABS v2008/1. Bruker AXS Inc. Madison, WI USA. ; _exptl_crystal_recrystallization_method ; Crystals were grown from hexanes. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8-ApexII CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37130 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 28.34 _reflns_number_total 9848 _reflns_number_gt 9182 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)' _computing_structure_solution 'XS (Sheldrick, 2001)' _computing_structure_refinement 'XL (Sheldrick, 2001)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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^)+(0.0441P)^2^+0.1692P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.004(11) _chemical_absolute_configuration rmad _refine_ls_number_reflns 9848 _refine_ls_number_parameters 680 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0311 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0711 _refine_ls_wR_factor_gt 0.0685 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 Ti Ti 0.728489(19) 0.55326(3) 0.141757(9) 0.01510(5) Uani 1 1 d . . . O1 O 0.69752(8) 0.75624(12) 0.19864(4) 0.01629(18) Uani 1 1 d . . . O2 O 0.88545(8) 0.66018(13) 0.13923(4) 0.01788(19) Uani 1 1 d . . . O3 O 0.79956(8) 0.46025(12) 0.22746(4) 0.01749(19) Uani 1 1 d . . . O4 O 0.58302(8) 0.45926(13) 0.17340(4) 0.01801(19) Uani 1 1 d . . . O5 O 0.77419(8) 0.36171(12) 0.10598(4) 0.01830(19) Uani 1 1 d . . . O6 O 0.66593(8) 0.65621(12) 0.07469(4) 0.01775(19) Uani 1 1 d . . . C1 C 0.71779(11) 0.94959(17) 0.28177(6) 0.0154(2) Uani 1 1 d . . . H1A H 0.7765(13) 1.013(2) 0.3041(7) 0.019(4) Uiso 1 1 d . . . H1B H 0.6668(14) 1.031(3) 0.2629(8) 0.026(4) Uiso 1 1 d . . . C2 C 0.76902(11) 0.84068(17) 0.23228(6) 0.0153(2) Uani 1 1 d . . . C3 C 0.88714(11) 0.84143(18) 0.22603(6) 0.0169(2) Uani 1 1 d . . . H3 H 0.9304(13) 0.913(2) 0.2531(7) 0.013(4) Uiso 1 1 d . . . C4 C 0.94027(11) 0.75535(18) 0.17852(6) 0.0160(2) Uani 1 1 d . . . C5 C 0.81959(12) 0.41585(18) 0.33570(6) 0.0169(3) Uani 1 1 d . . . H5A H 0.7720(14) 0.382(2) 0.3688(7) 0.018(4) Uiso 1 1 d . . . H5B H 0.8755(15) 0.330(2) 0.3325(8) 0.024(4) Uiso 1 1 d . . . C6 C 0.74672(11) 0.43020(16) 0.27600(6) 0.0153(2) Uani 1 1 d . . . C7 C 0.62824(12) 0.40370(17) 0.27827(6) 0.0172(3) Uani 1 1 d . . . H7 H 0.6008(14) 0.375(2) 0.3165(8) 0.024(4) Uiso 1 1 d . . . C8 C 0.55255(11) 0.41345(17) 0.22695(6) 0.0159(2) Uani 1 1 d . . . C11 C 0.69795(11) 0.73703(17) 0.36945(5) 0.0153(2) Uani 1 1 d . . . C12 C 0.64734(11) 0.84151(17) 0.32428(6) 0.0157(2) Uani 1 1 d . . . C13 C 0.52635(12) 0.84155(19) 0.31466(6) 0.0197(3) Uani 1 1 d . . . H13 H 0.4914(13) 0.907(2) 0.2818(7) 0.015(4) Uiso 1 1 d . . . C14 C 0.45795(12) 0.7403(2) 0.34884(6) 0.0214(3) Uani 1 1 d . . . H14 H 0.3768(16) 0.738(2) 0.3413(8) 0.031(5) Uiso 1 1 d . . . C15 C 0.43696(12) 0.5357(2) 0.43445(7) 0.0261(3) Uani 1 1 d . . . H15 H 0.3591(14) 0.533(2) 0.4237(7) 0.023(4) Uiso 1 1 d . . . C16 C 0.48456(14) 0.4423(2) 0.48190(8) 0.0318(4) Uani 1 1 d . . . H16 H 0.4354(16) 0.365(3) 0.5075(9) 0.033(5) Uiso 1 1 d . . . C17 C 0.60476(14) 0.4468(2) 0.49457(7) 0.0290(3) Uani 1 1 d . . . H17 H 0.6376(15) 0.380(3) 0.5260(8) 0.028(5) Uiso 1 1 d . . . C18 C 0.67394(11) 0.5423(2) 0.45856(6) 0.0216(3) Uani 1 1 d . . . H18 H 0.7551(13) 0.551(2) 0.4669(6) 0.016(3) Uiso 1 1 d . . . C19 C 0.62713(11) 0.63945(18) 0.40837(6) 0.0172(2) Uani 1 1 d . . . C10 C 0.50573(11) 0.63810(19) 0.39700(6) 0.0196(3) Uani 1 1 d . . . C21 C 0.82603(11) 0.72271(17) 0.37642(5) 0.0151(2) Uani 1 1 d . . . C22 C 0.88233(11) 0.57706(18) 0.35661(5) 0.0160(2) Uani 1 1 d . . . C23 C 1.00456(11) 0.57584(19) 0.35848(6) 0.0194(3) Uani 1 1 d . . . H23 H 1.0433(14) 0.478(2) 0.3444(7) 0.021(4) Uiso 1 1 d . . . C24 C 1.06749(12) 0.7126(2) 0.37896(6) 0.0215(3) Uani 1 1 d . . . H24 H 1.1509(16) 0.702(3) 0.3804(8) 0.032(5) Uiso 1 1 d . . . C25 C 1.07614(13) 1.0018(2) 0.42616(7) 0.0249(3) Uani 1 1 d . . . H25 H 1.1527(16) 0.993(2) 0.4247(8) 0.027(5) Uiso 1 1 d . . . C26 C 1.02253(14) 1.1375(2) 0.45154(7) 0.0279(3) Uani 1 1 d . . . H26 H 1.0597(16) 1.234(3) 0.4669(9) 0.035(5) Uiso 1 1 d . . . C27 C 0.90145(14) 1.1385(2) 0.45406(6) 0.0256(3) Uani 1 1 d . . . H27 H 0.8622(16) 1.231(3) 0.4718(8) 0.032(5) Uiso 1 1 d . . . C28 C 0.83760(13) 1.00666(18) 0.42926(6) 0.0204(3) Uani 1 1 d . . . H28 H 0.7563(13) 1.009(2) 0.4307(7) 0.011(4) Uiso 1 1 d . . . C29 C 0.89123(11) 0.86361(18) 0.40208(6) 0.0170(3) Uani 1 1 d . . . C20 C 1.01322(12) 0.85984(19) 0.40195(6) 0.0195(3) Uani 1 1 d . . . C31 C 1.06496(11) 0.77750(18) 0.16949(6) 0.0171(2) Uani 1 1 d . . . C32 C 1.10843(12) 0.74507(19) 0.11182(6) 0.0206(3) Uani 1 1 d . . . H32 H 1.0585(15) 0.706(2) 0.0809(8) 0.024(4) Uiso 1 1 d . . . C33 C 1.22415(12) 0.7728(2) 0.10190(7) 0.0225(3) Uani 1 1 d . . . H33 H 1.2482(14) 0.755(2) 0.0629(8) 0.020(4) Uiso 1 1 d . . . C34 C 1.29910(12) 0.83080(19) 0.14875(6) 0.0208(3) Uani 1 1 d . . . C35 C 1.25511(12) 0.8594(2) 0.20636(7) 0.0242(3) Uani 1 1 d . . . H35 H 1.3041(15) 0.902(3) 0.2398(8) 0.029(5) Uiso 1 1 d . . . C36 C 1.14031(12) 0.8338(2) 0.21692(6) 0.0225(3) Uani 1 1 d . . . H36 H 1.1117(15) 0.849(3) 0.2575(8) 0.030(5) Uiso 1 1 d . . . C37 C 1.42449(13) 0.8625(3) 0.13856(8) 0.0283(3) Uani 1 1 d . . . H37A H 1.4399(19) 0.867(3) 0.0954(11) 0.054(6) Uiso 1 1 d . . . H37B H 1.445(2) 0.975(4) 0.1480(12) 0.067(8) Uiso 1 1 d . . . H37C H 1.4721(19) 0.792(3) 0.1645(10) 0.050(6) Uiso 1 1 d . . . C41 C 0.42826(11) 0.37139(17) 0.23184(6) 0.0170(3) Uani 1 1 d . . . C42 C 0.35316(12) 0.39990(19) 0.18107(6) 0.0207(3) Uani 1 1 d . . . H42 H 0.3810(15) 0.446(2) 0.1456(8) 0.024(4) Uiso 1 1 d . . . C43 C 0.23732(12) 0.3646(2) 0.18389(7) 0.0229(3) Uani 1 1 d . . . H43 H 0.1872(17) 0.386(3) 0.1484(9) 0.038(5) Uiso 1 1 d . . . C44 C 0.19203(12) 0.29822(18) 0.23699(7) 0.0213(3) Uani 1 1 d . . . C45 C 0.26690(13) 0.2696(2) 0.28768(7) 0.0258(3) Uani 1 1 d . . . H45 H 0.2367(16) 0.221(3) 0.3271(9) 0.038(5) Uiso 1 1 d . . . C46 C 0.38332(13) 0.3052(2) 0.28537(7) 0.0242(3) Uani 1 1 d . . . H46 H 0.4323(15) 0.289(3) 0.3222(8) 0.027(4) Uiso 1 1 d . . . C47 C 0.06605(13) 0.2569(2) 0.23885(7) 0.0274(3) Uani 1 1 d . . . H47C H 0.0231(16) 0.356(3) 0.2332(8) 0.030(5) Uiso 1 1 d . . . H47B H 0.0443(15) 0.172(3) 0.2029(8) 0.028(5) Uiso 1 1 d . . . H47A H 0.0482(17) 0.211(3) 0.2811(9) 0.038(5) Uiso 1 1 d . . . C51 C 0.7474(2) 0.0663(3) 0.08791(10) 0.0506(6) Uani 1 1 d . . . H51A H 0.724(3) 0.086(5) 0.0455(14) 0.096(10) Uiso 1 1 d . . . H51B H 0.6749(19) 0.078(3) 0.1053(10) 0.044(6) Uiso 1 1 d . . . H51C H 0.7790(19) -0.050(3) 0.0914(10) 0.049(6) Uiso 1 1 d . . . C52 C 0.82866(13) 0.20144(19) 0.11169(6) 0.0224(3) Uani 1 1 d . . . H52 H 0.8434(14) 0.182(2) 0.1571(8) 0.024(4) Uiso 1 1 d . . . C53 C 0.9389(2) 0.2091(4) 0.07777(9) 0.0538(7) Uani 1 1 d . . . H53A H 0.975(2) 0.106(4) 0.0855(12) 0.073(8) Uiso 1 1 d . . . H53B H 0.990(3) 0.299(5) 0.0927(16) 0.107(13) Uiso 1 1 d . . . H53C H 0.917(2) 0.223(3) 0.0332(11) 0.061(7) Uiso 1 1 d . . . C61 C 0.55663(16) 0.7254(2) -0.01760(7) 0.0322(4) Uani 1 1 d . . . H61A H 0.5488(17) 0.702(3) -0.0621(10) 0.041(5) Uiso 1 1 d . . . H61B H 0.5687(16) 0.839(3) -0.0107(9) 0.034(5) Uiso 1 1 d . . . H61C H 0.4854(17) 0.688(3) 0.0001(9) 0.026(4) Uiso 1 1 d . . . C62 C 0.65774(13) 0.62517(19) 0.01022(6) 0.0209(3) Uani 1 1 d . . . H62 H 0.6423(13) 0.503(2) 0.0046(7) 0.013(4) Uiso 1 1 d . . . C63 C 0.76992(16) 0.6719(2) -0.01802(8) 0.0324(4) Uani 1 1 d . . . H63C H 0.7872(17) 0.791(3) -0.0114(9) 0.040(5) Uiso 1 1 d . . . H63B H 0.7665(17) 0.648(3) -0.0620(10) 0.045(6) Uiso 1 1 d . . . H63A H 0.8315(18) 0.617(3) -0.0004(9) 0.040(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti 0.01581(10) 0.01586(11) 0.01361(10) -0.00137(9) 0.00045(7) -0.00019(9) O1 0.0157(4) 0.0180(5) 0.0151(4) -0.0023(4) -0.0005(3) 0.0004(4) O2 0.0167(4) 0.0206(5) 0.0164(4) -0.0024(4) 0.0013(3) -0.0007(4) O3 0.0166(4) 0.0193(5) 0.0166(4) -0.0003(4) 0.0009(3) 0.0007(4) O4 0.0169(4) 0.0204(5) 0.0168(4) 0.0005(4) -0.0001(3) -0.0025(4) O5 0.0208(5) 0.0155(5) 0.0186(4) -0.0021(4) 0.0017(4) 0.0005(4) O6 0.0206(5) 0.0186(5) 0.0140(4) -0.0006(4) 0.0000(3) -0.0001(4) C1 0.0162(6) 0.0149(6) 0.0148(6) -0.0001(5) -0.0009(5) 0.0017(5) C2 0.0186(6) 0.0138(6) 0.0134(5) 0.0028(5) 0.0001(4) 0.0019(5) C3 0.0175(6) 0.0175(6) 0.0155(6) -0.0003(5) -0.0008(5) -0.0016(5) C4 0.0167(6) 0.0163(6) 0.0149(5) 0.0038(5) 0.0001(4) 0.0004(5) C5 0.0165(6) 0.0163(6) 0.0177(6) 0.0015(5) -0.0002(5) 0.0028(5) C6 0.0188(6) 0.0104(6) 0.0164(6) -0.0015(4) -0.0016(5) 0.0004(5) C7 0.0191(6) 0.0172(6) 0.0154(6) -0.0011(5) 0.0015(5) -0.0019(5) C8 0.0167(6) 0.0121(6) 0.0187(6) -0.0020(5) 0.0005(5) -0.0006(5) C11 0.0167(6) 0.0162(6) 0.0129(5) -0.0033(5) 0.0007(4) 0.0007(5) C12 0.0175(6) 0.0162(6) 0.0135(5) -0.0029(5) 0.0013(4) 0.0015(5) C13 0.0195(7) 0.0218(7) 0.0174(6) -0.0001(5) -0.0016(5) 0.0046(5) C14 0.0138(6) 0.0280(8) 0.0222(6) -0.0016(6) -0.0005(5) 0.0024(6) C15 0.0188(6) 0.0316(8) 0.0281(7) 0.0020(7) 0.0030(5) -0.0020(6) C16 0.0260(8) 0.0380(9) 0.0318(8) 0.0098(7) 0.0072(6) -0.0042(7) C17 0.0285(8) 0.0355(9) 0.0230(7) 0.0118(7) 0.0024(6) 0.0004(7) C18 0.0199(6) 0.0264(7) 0.0184(6) 0.0033(6) 0.0003(5) 0.0022(6) C19 0.0178(6) 0.0191(6) 0.0149(5) -0.0016(5) 0.0016(5) 0.0012(5) C10 0.0188(6) 0.0220(7) 0.0180(6) -0.0006(5) 0.0025(5) -0.0001(5) C21 0.0161(6) 0.0182(6) 0.0108(5) 0.0013(5) -0.0004(4) -0.0007(5) C22 0.0165(6) 0.0182(7) 0.0131(5) 0.0014(5) -0.0019(4) -0.0002(5) C23 0.0171(6) 0.0238(7) 0.0172(6) -0.0011(5) -0.0007(4) 0.0041(5) C24 0.0144(6) 0.0308(8) 0.0189(6) 0.0008(5) -0.0023(5) -0.0006(5) C25 0.0223(7) 0.0300(8) 0.0218(7) 0.0016(6) -0.0055(6) -0.0067(6) C26 0.0350(8) 0.0254(8) 0.0222(7) 0.0004(6) -0.0111(6) -0.0070(7) C27 0.0354(8) 0.0223(7) 0.0183(6) -0.0020(6) -0.0069(6) 0.0029(6) C28 0.0242(7) 0.0216(7) 0.0151(6) 0.0005(5) -0.0039(5) 0.0017(5) C29 0.0198(6) 0.0194(6) 0.0115(5) 0.0025(5) -0.0036(5) -0.0011(5) C20 0.0208(7) 0.0230(7) 0.0142(6) 0.0013(5) -0.0041(5) -0.0022(6) C31 0.0151(6) 0.0183(6) 0.0180(6) 0.0023(5) 0.0013(5) 0.0011(5) C32 0.0183(7) 0.0259(7) 0.0175(6) -0.0010(5) 0.0001(5) -0.0015(6) C33 0.0196(7) 0.0287(7) 0.0196(6) 0.0005(6) 0.0044(5) 0.0002(6) C34 0.0171(6) 0.0226(7) 0.0226(6) 0.0039(5) 0.0007(5) 0.0016(5) C35 0.0176(7) 0.0328(8) 0.0219(7) -0.0020(6) -0.0042(5) 0.0005(6) C36 0.0173(7) 0.0315(8) 0.0186(6) -0.0020(6) 0.0000(5) 0.0034(6) C37 0.0168(7) 0.0391(9) 0.0289(8) 0.0055(7) 0.0010(6) -0.0006(7) C41 0.0158(6) 0.0161(6) 0.0193(6) -0.0034(5) 0.0005(5) -0.0011(5) C42 0.0217(7) 0.0224(7) 0.0179(6) 0.0001(5) 0.0009(5) -0.0018(5) C43 0.0197(7) 0.0252(7) 0.0233(7) -0.0027(6) -0.0045(5) -0.0005(6) C44 0.0176(6) 0.0195(7) 0.0269(7) -0.0064(5) 0.0027(5) -0.0019(5) C45 0.0220(7) 0.0347(8) 0.0209(6) 0.0008(6) 0.0029(5) -0.0072(6) C46 0.0208(7) 0.0314(8) 0.0200(6) 0.0017(6) -0.0024(5) -0.0040(6) C47 0.0184(7) 0.0323(8) 0.0316(8) -0.0052(7) 0.0026(6) -0.0035(6) C51 0.0837(17) 0.0203(8) 0.0447(10) 0.0063(8) -0.0338(11) -0.0108(10) C52 0.0288(8) 0.0194(7) 0.0186(6) -0.0006(5) -0.0037(5) 0.0053(6) C53 0.0441(12) 0.0875(19) 0.0307(9) 0.0081(10) 0.0107(8) 0.0394(13) C61 0.0394(10) 0.0345(10) 0.0217(7) -0.0021(6) -0.0101(7) 0.0056(8) C62 0.0276(7) 0.0186(7) 0.0162(6) -0.0025(5) -0.0007(5) -0.0018(6) C63 0.0384(9) 0.0340(9) 0.0257(8) -0.0023(7) 0.0114(7) -0.0049(7) _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 Ti O5 1.7811(10) . ? Ti O6 1.7930(9) . ? Ti O4 1.9983(10) . ? Ti O2 2.0148(10) . ? Ti O1 2.0549(9) . ? Ti O3 2.1342(9) . ? O1 C2 1.2700(16) . ? O2 C4 1.2825(16) . ? O3 C6 1.2677(16) . ? O4 C8 1.2837(16) . ? O5 C52 1.4086(17) . ? O6 C62 1.4221(16) . ? C1 C2 1.5161(17) . ? C1 C12 1.5203(18) . ? C1 H1A 0.959(16) . ? C1 H1B 0.952(19) . ? C2 C3 1.3895(18) . ? C3 C4 1.4007(18) . ? C3 H3 0.942(16) . ? C4 C31 1.4854(18) . ? C5 C22 1.5176(19) . ? C5 C6 1.5241(18) . ? C5 H5A 0.966(16) . ? C5 H5B 0.941(19) . ? C6 C7 1.3996(19) . ? C7 C8 1.3940(18) . ? C7 H7 0.931(18) . ? C8 C41 1.4941(18) . ? C11 C12 1.3894(18) . ? C11 C19 1.4293(18) . ? C11 C21 1.4982(18) . ? C12 C13 1.4166(18) . ? C13 C14 1.367(2) . ? C13 H13 0.956(16) . ? C14 C10 1.413(2) . ? C14 H14 0.953(19) . ? C15 C16 1.363(2) . ? C15 C10 1.416(2) . ? C15 H15 0.927(16) . ? C16 C17 1.416(2) . ? C16 H16 1.02(2) . ? C17 C18 1.371(2) . ? C17 H17 0.928(19) . ? C18 C19 1.4192(18) . ? C18 H18 0.957(15) . ? C19 C10 1.4258(18) . ? C21 C22 1.3928(18) . ? C21 C29 1.4377(18) . ? C22 C23 1.4237(18) . ? C23 C24 1.361(2) . ? C23 H23 0.948(18) . ? C24 C20 1.416(2) . ? C24 H24 0.975(19) . ? C25 C26 1.361(2) . ? C25 C20 1.420(2) . ? C25 H25 0.897(18) . ? C26 C27 1.415(2) . ? C26 H26 0.92(2) . ? C27 C28 1.369(2) . ? C27 H27 0.95(2) . ? C28 C29 1.423(2) . ? C28 H28 0.950(15) . ? C29 C20 1.4225(19) . ? C31 C32 1.3966(18) . ? C31 C36 1.3964(19) . ? C32 C33 1.393(2) . ? C32 H32 0.923(18) . ? C33 C34 1.389(2) . ? C33 H33 0.915(17) . ? C34 C35 1.393(2) . ? C34 C37 1.508(2) . ? C35 C36 1.382(2) . ? C35 H35 0.964(18) . ? C36 H36 0.965(18) . ? C37 H37A 0.96(2) . ? C37 H37B 0.93(3) . ? C37 H37C 0.95(2) . ? C41 C42 1.3965(19) . ? C41 C46 1.3973(19) . ? C42 C43 1.382(2) . ? C42 H42 0.923(18) . ? C43 C44 1.392(2) . ? C43 H43 0.961(19) . ? C44 C45 1.394(2) . ? C44 C47 1.506(2) . ? C45 C46 1.388(2) . ? C45 H45 1.02(2) . ? C46 H46 0.971(18) . ? C47 H47C 0.93(2) . ? C47 H47B 1.050(19) . ? C47 H47A 1.02(2) . ? C51 C52 1.496(2) . ? C51 H51A 0.96(3) . ? C51 H51B 0.94(2) . ? C51 H51C 0.99(3) . ? C52 C53 1.511(3) . ? C52 H52 1.007(17) . ? C53 H53A 0.92(3) . ? C53 H53B 0.97(4) . ? C53 H53C 1.00(2) . ? C61 C62 1.519(2) . ? C61 H61A 0.98(2) . ? C61 H61B 0.91(2) . ? C61 H61C 0.97(2) . ? C62 C63 1.514(2) . ? C62 H62 0.983(17) . ? C63 H63C 0.97(2) . ? C63 H63B 0.97(2) . ? C63 H63A 0.91(2) . ? 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 O5 Ti O6 98.12(4) . . ? O5 Ti O4 96.63(4) . . ? O6 Ti O4 97.17(4) . . ? O5 Ti O2 92.75(4) . . ? O6 Ti O2 97.38(4) . . ? O4 Ti O2 161.38(4) . . ? O5 Ti O1 167.77(4) . . ? O6 Ti O1 93.83(4) . . ? O4 Ti O1 84.42(4) . . ? O2 Ti O1 83.08(4) . . ? O5 Ti O3 89.01(4) . . ? O6 Ti O3 172.81(4) . . ? O4 Ti O3 82.89(4) . . ? O2 Ti O3 81.23(4) . . ? O1 Ti O3 79.01(4) . . ? C2 O1 Ti 128.37(8) . . ? C4 O2 Ti 130.48(8) . . ? C6 O3 Ti 127.35(8) . . ? C8 O4 Ti 133.50(8) . . ? C52 O5 Ti 148.53(9) . . ? C62 O6 Ti 137.12(9) . . ? C2 C1 C12 111.07(11) . . ? C2 C1 H1A 110.8(9) . . ? C12 C1 H1A 111.7(9) . . ? C2 C1 H1B 109.2(10) . . ? C12 C1 H1B 106.9(10) . . ? H1A C1 H1B 106.9(15) . . ? O1 C2 C3 125.01(12) . . ? O1 C2 C1 115.63(11) . . ? C3 C2 C1 119.36(12) . . ? C2 C3 C4 122.86(12) . . ? C2 C3 H3 116.5(9) . . ? C4 C3 H3 120.3(9) . . ? O2 C4 C3 123.18(12) . . ? O2 C4 C31 116.19(11) . . ? C3 C4 C31 120.57(12) . . ? C22 C5 C6 115.93(11) . . ? C22 C5 H5A 107.0(10) . . ? C6 C5 H5A 109.8(9) . . ? C22 C5 H5B 106.8(11) . . ? C6 C5 H5B 110.6(11) . . ? H5A C5 H5B 106.3(15) . . ? O3 C6 C7 124.98(12) . . ? O3 C6 C5 116.77(11) . . ? C7 C6 C5 118.22(11) . . ? C8 C7 C6 123.67(12) . . ? C8 C7 H7 119.8(10) . . ? C6 C7 H7 116.5(10) . . ? O4 C8 C7 123.44(12) . . ? O4 C8 C41 115.73(11) . . ? C7 C8 C41 120.82(12) . . ? C12 C11 C19 119.66(12) . . ? C12 C11 C21 120.37(11) . . ? C19 C11 C21 119.95(11) . . ? C11 C12 C13 119.57(12) . . ? C11 C12 C1 122.24(12) . . ? C13 C12 C1 118.10(12) . . ? C14 C13 C12 121.36(13) . . ? C14 C13 H13 118.6(9) . . ? C12 C13 H13 119.9(9) . . ? C13 C14 C10 120.74(12) . . ? C13 C14 H14 121.2(11) . . ? C10 C14 H14 118.1(11) . . ? C16 C15 C10 121.14(13) . . ? C16 C15 H15 122.5(11) . . ? C10 C15 H15 116.3(11) . . ? C15 C16 C17 120.01(14) . . ? C15 C16 H16 120.9(11) . . ? C17 C16 H16 119.0(11) . . ? C18 C17 C16 120.29(14) . . ? C18 C17 H17 119.5(11) . . ? C16 C17 H17 120.1(11) . . ? C17 C18 C19 121.04(13) . . ? C17 C18 H18 122.0(10) . . ? C19 C18 H18 116.9(10) . . ? C18 C19 C10 118.32(12) . . ? C18 C19 C11 121.94(12) . . ? C10 C19 C11 119.74(12) . . ? C14 C10 C15 122.14(13) . . ? C14 C10 C19 118.70(12) . . ? C15 C10 C19 119.15(12) . . ? C22 C21 C29 119.95(12) . . ? C22 C21 C11 120.73(11) . . ? C29 C21 C11 119.29(11) . . ? C21 C22 C23 118.77(12) . . ? C21 C22 C5 123.05(11) . . ? C23 C22 C5 118.13(12) . . ? C24 C23 C22 121.89(13) . . ? C24 C23 H23 119.0(10) . . ? C22 C23 H23 119.1(10) . . ? C23 C24 C20 120.82(13) . . ? C23 C24 H24 117.9(12) . . ? C20 C24 H24 121.1(12) . . ? C26 C25 C20 121.46(14) . . ? C26 C25 H25 123.3(12) . . ? C20 C25 H25 115.2(12) . . ? C25 C26 C27 119.79(14) . . ? C25 C26 H26 124.5(12) . . ? C27 C26 H26 115.7(12) . . ? C28 C27 C26 120.43(14) . . ? C28 C27 H27 118.2(12) . . ? C26 C27 H27 121.3(12) . . ? C27 C28 C29 121.01(14) . . ? C27 C28 H28 119.7(9) . . ? C29 C28 H28 119.3(9) . . ? C20 C29 C28 118.33(13) . . ? C20 C29 C21 119.65(12) . . ? C28 C29 C21 122.00(12) . . ? C24 C20 C25 122.42(13) . . ? C24 C20 C29 118.68(12) . . ? C25 C20 C29 118.89(13) . . ? C32 C31 C36 118.66(12) . . ? C32 C31 C4 119.57(12) . . ? C36 C31 C4 121.75(12) . . ? C33 C32 C31 120.22(13) . . ? C33 C32 H32 121.6(10) . . ? C31 C32 H32 118.2(10) . . ? C34 C33 C32 121.28(13) . . ? C34 C33 H33 121.4(10) . . ? C32 C33 H33 117.3(10) . . ? C33 C34 C35 117.90(13) . . ? C33 C34 C37 121.87(13) . . ? C35 C34 C37 120.22(13) . . ? C36 C35 C34 121.59(13) . . ? C36 C35 H35 118.1(10) . . ? C34 C35 H35 120.3(10) . . ? C35 C36 C31 120.32(13) . . ? C35 C36 H36 120.7(11) . . ? C31 C36 H36 118.9(11) . . ? C34 C37 H37A 111.8(13) . . ? C34 C37 H37B 111.5(15) . . ? H37A C37 H37B 97(2) . . ? C34 C37 H37C 111.3(14) . . ? H37A C37 H37C 118(2) . . ? H37B C37 H37C 106(2) . . ? C42 C41 C46 118.24(12) . . ? C42 C41 C8 118.98(12) . . ? C46 C41 C8 122.78(12) . . ? C43 C42 C41 120.84(13) . . ? C43 C42 H42 119.7(11) . . ? C41 C42 H42 119.4(11) . . ? C42 C43 C44 121.23(13) . . ? C42 C43 H43 119.3(12) . . ? C44 C43 H43 119.4(12) . . ? C43 C44 C45 117.99(13) . . ? C43 C44 C47 120.58(14) . . ? C45 C44 C47 121.43(14) . . ? C46 C45 C44 121.21(14) . . ? C46 C45 H45 118.8(11) . . ? C44 C45 H45 120.0(11) . . ? C45 C46 C41 120.50(13) . . ? C45 C46 H46 118.9(11) . . ? C41 C46 H46 120.5(11) . . ? C44 C47 H47C 109.9(12) . . ? C44 C47 H47B 108.6(10) . . ? H47C C47 H47B 108.5(15) . . ? C44 C47 H47A 109.8(11) . . ? H47C C47 H47A 106.4(16) . . ? H47B C47 H47A 113.5(15) . . ? C52 C51 H51A 111(2) . . ? C52 C51 H51B 110.9(14) . . ? H51A C51 H51B 98(2) . . ? C52 C51 H51C 113.5(13) . . ? H51A C51 H51C 108(2) . . ? H51B C51 H51C 113(2) . . ? O5 C52 C51 108.80(13) . . ? O5 C52 C53 108.16(15) . . ? C51 C52 C53 113.47(19) . . ? O5 C52 H52 106.1(10) . . ? C51 C52 H52 108.1(10) . . ? C53 C52 H52 111.9(10) . . ? C52 C53 H53A 105.6(17) . . ? C52 C53 H53B 113(2) . . ? H53A C53 H53B 108(3) . . ? C52 C53 H53C 107.1(13) . . ? H53A C53 H53C 111(2) . . ? H53B C53 H53C 112(3) . . ? C62 C61 H61A 109.4(12) . . ? C62 C61 H61B 109.1(12) . . ? H61A C61 H61B 110.5(18) . . ? C62 C61 H61C 110.4(11) . . ? H61A C61 H61C 106.7(16) . . ? H61B C61 H61C 110.8(16) . . ? O6 C62 C63 109.71(12) . . ? O6 C62 C61 108.77(12) . . ? C63 C62 C61 112.49(14) . . ? O6 C62 H62 107.1(9) . . ? C63 C62 H62 110.0(9) . . ? C61 C62 H62 108.6(9) . . ? C62 C63 H63C 110.6(12) . . ? C62 C63 H63B 110.7(12) . . ? H63C C63 H63B 109.3(18) . . ? C62 C63 H63A 113.3(13) . . ? H63C C63 H63A 103.8(18) . . ? H63B C63 H63A 108.8(18) . . ? _diffrn_measured_fraction_theta_max .999 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full .999 _refine_diff_density_max .266 _refine_diff_density_min -.187 _refine_diff_density_rms .038 # Attachment '- taddol1.cif' data_taddol1 _database_code_depnum_ccdc_archive 'CCDC 784601' #TrackingRef '- taddol1.cif' # Collected as bcn380 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (S,\D)-(2,2'-Biphenyl-bis(4-p-tolyl-2,4-butanedionato))titanium(IV)- (R,R-Taddol) ; _chemical_name_common (S,\D,R,R)-(Tol2Bob)Ti(Taddol) _chemical_melting_point ? _chemical_formula_moiety 'C65 H56 O8 Ti' _chemical_formula_sum 'C65 H56 O8 Ti' _chemical_formula_weight 1013.00 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 P1 _symmetry_space_group_name_Hall 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.1257(3) _cell_length_b 11.5661(4) _cell_length_c 13.5882(5) _cell_angle_alpha 65.765(2) _cell_angle_beta 74.173(2) _cell_angle_gamma 87.031(2) _cell_volume 1255.28(8) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9917 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 28.37 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.340 _exptl_crystal_density_method . _exptl_crystal_F_000 532 _exptl_absorpt_coefficient_mu 0.231 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9445 _exptl_absorpt_correction_T_max 0.9750 _exptl_absorpt_process_details ; Blessing, R. H. (1995) Acta Cryst. A51, 33-38. Sheldrick, G.M. (2008) SADABS v2008/1. Bruker AXS Inc. Madison, WI USA. ; _exptl_crystal_recrystallization_method ; Crystals were grown from dichloromethane/hexanes. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8-ApexII CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 21338 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 28.41 _reflns_number_total 11051 _reflns_number_gt 10542 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)' _computing_structure_solution 'XS (Sheldrick, 2001)' _computing_structure_refinement 'XL (Sheldrick, 2001)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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^)+(0.0479P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary none _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method . _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.004(10) _chemical_absolute_configuration rmad _refine_ls_number_reflns 11051 _refine_ls_number_parameters 891 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_gt 0.0283 _refine_ls_wR_factor_ref 0.0744 _refine_ls_wR_factor_gt 0.0731 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 Ti Ti -0.24144(2) -0.00977(2) -0.866203(19) 0.01218(6) Uani 1 1 d . . . O1 O -0.27262(12) -0.13498(10) -0.92964(9) 0.0161(2) Uani 1 1 d . . . O2 O -0.40138(12) 0.07786(10) -0.94101(9) 0.0154(2) Uani 1 1 d . . . O3 O -0.08406(12) 0.07237(10) -1.02107(9) 0.0153(2) Uani 1 1 d . . . O4 O -0.06881(12) -0.10477(10) -0.82192(9) 0.0161(2) Uani 1 1 d . . . O5 O -0.20687(11) 0.12727(9) -0.84239(9) 0.0126(2) Uani 1 1 d . . . O6 O -0.37044(12) -0.09236(9) -0.73010(9) 0.0136(2) Uani 1 1 d . . . O7 O -0.45819(12) 0.21687(10) -0.63450(9) 0.0155(2) Uani 1 1 d . . . O8 O -0.45338(12) 0.01721(10) -0.50579(9) 0.0147(2) Uani 1 1 d . . . C1 C -0.25963(18) -0.20806(15) -1.07029(14) 0.0190(3) Uani 1 1 d . . . C2 C -0.30072(17) -0.10983(14) -1.02263(13) 0.0164(3) Uani 1 1 d . . . C3 C -0.36869(17) -0.00113(14) -1.07912(13) 0.0170(3) Uani 1 1 d . . . C4 C -0.42485(16) 0.08427(13) -1.03142(12) 0.0144(3) Uani 1 1 d . . . C5 C 0.11916(18) 0.10468(15) -1.18218(13) 0.0180(3) Uani 1 1 d . . . C6 C 0.04521(16) 0.03653(14) -1.05750(12) 0.0142(3) Uani 1 1 d . . . C7 C 0.12172(17) -0.05705(15) -0.99100(13) 0.0176(3) Uani 1 1 d . . . C8 C 0.06314(16) -0.12321(14) -0.87687(13) 0.0148(3) Uani 1 1 d . . . C11 C 0.02129(18) -0.14317(15) -1.17455(13) 0.0174(3) Uani 1 1 d . . . C12 C -0.09165(19) -0.23206(15) -1.08871(13) 0.0184(3) Uani 1 1 d . . . C13 C -0.0493(2) -0.34466(15) -1.01504(15) 0.0245(4) Uani 1 1 d . . . C14 C 0.1030(2) -0.37012(17) -1.02659(16) 0.0292(4) Uani 1 1 d . . . C15 C 0.2139(2) -0.28482(17) -1.11361(16) 0.0267(4) Uani 1 1 d . . . C16 C 0.17390(19) -0.17279(17) -1.18707(15) 0.0225(3) Uani 1 1 d . . . C21 C -0.01704(17) -0.01906(15) -1.25380(13) 0.0172(3) Uani 1 1 d . . . C22 C 0.02578(17) 0.09646(15) -1.25552(12) 0.0172(3) Uani 1 1 d . . . C23 C -0.01385(19) 0.20880(16) -1.33196(14) 0.0218(3) Uani 1 1 d . . . C24 C -0.0887(2) 0.20851(18) -1.40727(15) 0.0274(4) Uani 1 1 d . . . C25 C -0.1269(2) 0.09453(19) -1.40764(15) 0.0270(4) Uani 1 1 d . . . C26 C -0.09289(18) -0.01791(16) -1.32987(14) 0.0217(3) Uani 1 1 d . . . C31 C -0.52117(17) 0.18524(14) -1.08293(13) 0.0162(3) Uani 1 1 d . . . C32 C -0.64125(19) 0.22110(15) -1.01483(14) 0.0204(3) Uani 1 1 d . . . C33 C -0.7346(2) 0.31320(16) -1.06166(15) 0.0231(3) Uani 1 1 d . . . C34 C -0.70745(19) 0.37507(15) -1.17705(15) 0.0211(3) Uani 1 1 d . . . C35 C -0.58445(19) 0.34227(16) -1.24481(14) 0.0219(3) Uani 1 1 d . . . C36 C -0.49371(18) 0.24706(16) -1.19880(14) 0.0201(3) Uani 1 1 d . . . C37 C -0.8105(3) 0.47448(19) -1.22835(19) 0.0323(4) Uani 1 1 d . . . C41 C 0.14720(17) -0.22183(14) -0.80783(13) 0.0150(3) Uani 1 1 d . . . C42 C 0.06893(18) -0.30017(14) -0.69779(14) 0.0178(3) Uani 1 1 d . . . C43 C 0.14214(19) -0.39215(15) -0.62967(15) 0.0214(3) Uani 1 1 d . . . C44 C 0.2963(2) -0.40827(15) -0.66844(15) 0.0221(3) Uani 1 1 d . . . C45 C 0.37430(19) -0.32924(17) -0.77706(16) 0.0244(4) Uani 1 1 d . . . C46 C 0.30168(19) -0.23678(16) -0.84687(15) 0.0219(3) Uani 1 1 d . . . C47 C 0.3719(2) -0.51113(18) -0.5925(2) 0.0313(4) Uani 1 1 d . . . C51 C -0.27393(16) 0.21530(13) -0.79999(12) 0.0121(3) Uani 1 1 d . . . C52 C -0.41054(16) 0.14279(13) -0.69796(12) 0.0126(3) Uani 1 1 d . . . C53 C -0.37631(16) 0.01571(13) -0.61184(12) 0.0124(3) Uani 1 1 d . . . C54 C -0.42780(16) -0.10662(13) -0.61864(12) 0.0127(3) Uani 1 1 d . . . C55 C -0.53099(16) 0.13245(13) -0.52278(12) 0.0141(3) Uani 1 1 d . . . C56 C -0.50213(19) 0.18312(16) -0.44325(14) 0.0193(3) Uani 1 1 d . . . C57 C -0.69867(18) 0.11078(15) -0.50785(14) 0.0175(3) Uani 1 1 d . . . C61 C -0.32631(17) 0.32170(13) -0.89329(12) 0.0145(3) Uani 1 1 d . . . C62 C -0.45707(18) 0.38463(14) -0.87251(13) 0.0176(3) Uani 1 1 d . . . C63 C -0.50183(19) 0.47799(15) -0.96100(15) 0.0214(3) Uani 1 1 d . . . C64 C -0.4169(2) 0.50906(15) -1.07042(14) 0.0221(3) Uani 1 1 d . . . C65 C -0.2848(2) 0.44760(16) -1.09118(14) 0.0231(3) Uani 1 1 d . . . C66 C -0.24040(18) 0.35514(15) -1.00347(13) 0.0190(3) Uani 1 1 d . . . C71 C -0.15184(17) 0.26866(14) -0.76907(12) 0.0137(3) Uani 1 1 d . . . C72 C -0.01280(18) 0.21360(15) -0.76908(13) 0.0182(3) Uani 1 1 d . . . C73 C 0.10180(19) 0.26378(17) -0.74544(15) 0.0244(3) Uani 1 1 d . . . C74 C 0.0784(2) 0.36939(17) -0.72236(15) 0.0234(3) Uani 1 1 d . . . C75 C -0.0586(2) 0.42547(16) -0.72223(14) 0.0228(3) Uani 1 1 d . . . C76 C -0.17393(18) 0.37501(15) -0.74462(13) 0.0185(3) Uani 1 1 d . . . C81 C -0.60161(16) -0.12517(13) -0.58691(13) 0.0134(3) Uani 1 1 d . . . C82 C -0.68664(17) -0.18935(14) -0.47575(13) 0.0158(3) Uani 1 1 d . . . C83 C -0.84482(17) -0.19807(15) -0.44823(14) 0.0193(3) Uani 1 1 d . . . C84 C -0.91832(18) -0.14306(16) -0.53036(16) 0.0221(3) Uani 1 1 d . . . C85 C -0.83501(18) -0.08222(15) -0.64085(15) 0.0192(3) Uani 1 1 d . . . C86 C -0.67702(17) -0.07434(14) -0.66985(13) 0.0154(3) Uani 1 1 d . . . C91 C -0.36296(16) -0.22507(13) -0.54427(12) 0.0146(3) Uani 1 1 d . . . C92 C -0.34785(18) -0.32909(15) -0.57098(14) 0.0203(3) Uani 1 1 d . . . C93 C -0.2951(2) -0.43997(15) -0.50467(15) 0.0241(4) Uani 1 1 d . . . C94 C -0.25444(19) -0.44794(15) -0.41181(14) 0.0242(4) Uani 1 1 d . . . C95 C -0.26887(19) -0.34472(16) -0.38450(15) 0.0229(3) Uani 1 1 d . . . C96 C -0.32371(18) -0.23378(15) -0.45036(14) 0.0188(3) Uani 1 1 d . . . H1A H -0.316(2) -0.2849(18) -1.0196(16) 0.016(4) Uiso 1 1 d . . . H1B H -0.286(2) -0.1741(17) -1.1452(17) 0.014(4) Uiso 1 1 d . . . H3 H -0.391(2) 0.010(2) -1.1481(19) 0.027(5) Uiso 1 1 d . . . H5A H 0.138(2) 0.1905(18) -1.1960(16) 0.014(4) Uiso 1 1 d . . . H5B H 0.217(3) 0.070(2) -1.2002(18) 0.030(6) Uiso 1 1 d . . . H7 H 0.220(2) -0.0756(19) -1.0325(18) 0.025(5) Uiso 1 1 d . . . H13 H -0.126(2) -0.4092(19) -0.9501(18) 0.025(5) Uiso 1 1 d . . . H14 H 0.127(3) -0.448(2) -0.971(2) 0.046(7) Uiso 1 1 d . . . H15 H 0.324(3) -0.308(2) -1.126(2) 0.043(7) Uiso 1 1 d . . . H16 H 0.254(2) -0.113(2) -1.2537(19) 0.029(6) Uiso 1 1 d . . . H23 H 0.009(2) 0.284(2) -1.3351(19) 0.031(6) Uiso 1 1 d . . . H24 H -0.116(2) 0.282(2) -1.4532(18) 0.026(5) Uiso 1 1 d . . . H25 H -0.175(3) 0.091(2) -1.459(2) 0.034(6) Uiso 1 1 d . . . H26 H -0.116(2) -0.100(2) -1.3288(18) 0.029(6) Uiso 1 1 d . . . H32 H -0.653(2) 0.1799(19) -0.9370(19) 0.021(5) Uiso 1 1 d . . . H33 H -0.830(2) 0.3259(18) -1.0133(17) 0.021(5) Uiso 1 1 d . . . H35 H -0.568(3) 0.385(2) -1.329(2) 0.030(5) Uiso 1 1 d . . . H36 H -0.408(2) 0.2202(17) -1.2507(16) 0.016(4) Uiso 1 1 d . . . H37A H -0.794(3) 0.504(3) -1.303(3) 0.057(8) Uiso 1 1 d . . . H37B H -0.785(4) 0.547(4) -1.225(4) 0.101(13) Uiso 1 1 d . . . H37C H -0.918(5) 0.453(4) -1.205(3) 0.104(14) Uiso 1 1 d . . . H42 H -0.035(2) -0.2891(17) -0.6695(16) 0.015(4) Uiso 1 1 d . . . H43 H 0.091(3) -0.453(2) -0.555(2) 0.034(6) Uiso 1 1 d . . . H45 H 0.483(3) -0.336(2) -0.8064(19) 0.034(6) Uiso 1 1 d . . . H46 H 0.359(2) -0.179(2) -0.9247(19) 0.029(5) Uiso 1 1 d . . . H47A H 0.390(3) -0.487(2) -0.540(2) 0.044(7) Uiso 1 1 d . . . H47B H 0.477(4) -0.520(3) -0.637(3) 0.088(11) Uiso 1 1 d . . . H47C H 0.309(3) -0.587(3) -0.556(2) 0.056(8) Uiso 1 1 d . . . H52 H -0.4888(19) 0.1277(15) -0.7294(14) 0.005(4) Uiso 1 1 d . . . H53 H -0.269(2) 0.0123(16) -0.6160(15) 0.011(4) Uiso 1 1 d . . . H56A H -0.527(2) 0.118(2) -0.370(2) 0.030(5) Uiso 1 1 d . . . H56B H -0.399(2) 0.2081(17) -0.4632(16) 0.015(4) Uiso 1 1 d . . . H56C H -0.553(3) 0.250(2) -0.444(2) 0.033(6) Uiso 1 1 d . . . H57A H -0.710(2) 0.0790(18) -0.5614(17) 0.015(4) Uiso 1 1 d . . . H57B H -0.743(3) 0.060(2) -0.441(2) 0.033(6) Uiso 1 1 d . . . H57C H -0.749(2) 0.1923(18) -0.5209(16) 0.017(5) Uiso 1 1 d . . . H62 H -0.524(2) 0.3620(19) -0.8048(19) 0.023(5) Uiso 1 1 d . . . H63 H -0.593(3) 0.515(2) -0.9447(18) 0.027(5) Uiso 1 1 d . . . H64 H -0.446(2) 0.570(2) -1.1342(18) 0.025(5) Uiso 1 1 d . . . H65 H -0.228(3) 0.465(2) -1.165(2) 0.033(6) Uiso 1 1 d . . . H66 H -0.150(2) 0.3120(19) -1.0243(17) 0.022(5) Uiso 1 1 d . . . H72 H 0.001(2) 0.1436(18) -0.7856(15) 0.012(4) Uiso 1 1 d . . . H73 H 0.200(3) 0.227(2) -0.7429(18) 0.027(5) Uiso 1 1 d . . . H74 H 0.154(3) 0.405(2) -0.7119(19) 0.029(6) Uiso 1 1 d . . . H75 H -0.068(2) 0.496(2) -0.7101(18) 0.025(5) Uiso 1 1 d . . . H76 H -0.268(2) 0.4139(17) -0.7428(15) 0.011(4) Uiso 1 1 d . . . H82 H -0.636(2) -0.2213(19) -0.4163(18) 0.024(5) Uiso 1 1 d . . . H83 H -0.898(2) -0.238(2) -0.3808(19) 0.025(5) Uiso 1 1 d . . . H84 H -1.024(3) -0.1501(19) -0.5130(18) 0.026(5) Uiso 1 1 d . . . H85 H -0.879(2) -0.0491(18) -0.7017(17) 0.016(4) Uiso 1 1 d . . . H86 H -0.622(2) -0.0376(18) -0.7426(17) 0.015(4) Uiso 1 1 d . . . H92 H -0.369(2) -0.3269(19) -0.6365(18) 0.023(5) Uiso 1 1 d . . . H93 H -0.280(3) -0.504(2) -0.528(2) 0.039(6) Uiso 1 1 d . . . H94 H -0.218(3) -0.522(2) -0.373(2) 0.031(6) Uiso 1 1 d . . . H95 H -0.245(2) -0.3472(19) -0.3195(18) 0.023(5) Uiso 1 1 d . . . H96 H -0.337(2) -0.171(2) -0.4250(18) 0.027(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti 0.01447(11) 0.01165(11) 0.00905(12) -0.00414(9) -0.00163(9) 0.00260(8) O1 0.0216(5) 0.0140(5) 0.0120(5) -0.0057(4) -0.0030(4) 0.0021(4) O2 0.0180(5) 0.0169(5) 0.0123(5) -0.0070(4) -0.0044(4) 0.0031(4) O3 0.0168(5) 0.0157(5) 0.0125(5) -0.0065(4) -0.0021(4) 0.0030(4) O4 0.0165(5) 0.0173(5) 0.0124(5) -0.0055(4) -0.0027(4) 0.0060(4) O5 0.0137(5) 0.0143(5) 0.0102(5) -0.0059(4) -0.0027(4) 0.0026(4) O6 0.0155(5) 0.0125(5) 0.0109(5) -0.0045(4) -0.0013(4) 0.0019(4) O7 0.0177(5) 0.0138(5) 0.0117(5) -0.0057(4) 0.0014(4) 0.0014(4) O8 0.0201(5) 0.0139(5) 0.0098(5) -0.0056(4) -0.0030(4) 0.0040(4) C1 0.0209(7) 0.0186(7) 0.0200(8) -0.0119(6) -0.0031(6) -0.0004(6) C2 0.0155(6) 0.0158(7) 0.0161(7) -0.0081(6) 0.0020(5) -0.0039(5) C3 0.0189(7) 0.0204(7) 0.0140(7) -0.0091(6) -0.0048(6) 0.0015(6) C4 0.0129(6) 0.0153(7) 0.0122(7) -0.0045(5) -0.0005(5) -0.0023(5) C5 0.0171(7) 0.0185(7) 0.0140(7) -0.0046(6) -0.0002(6) -0.0014(6) C6 0.0146(6) 0.0157(7) 0.0132(7) -0.0080(5) -0.0013(5) -0.0020(5) C7 0.0143(7) 0.0222(7) 0.0162(7) -0.0095(6) -0.0017(6) 0.0030(5) C8 0.0165(7) 0.0149(6) 0.0173(7) -0.0099(6) -0.0063(6) 0.0026(5) C11 0.0212(7) 0.0202(7) 0.0141(7) -0.0103(6) -0.0056(6) 0.0054(6) C12 0.0248(8) 0.0191(7) 0.0152(7) -0.0115(6) -0.0045(6) 0.0030(6) C13 0.0347(9) 0.0172(8) 0.0197(8) -0.0079(6) -0.0046(7) 0.0030(6) C14 0.0428(11) 0.0216(8) 0.0249(9) -0.0098(7) -0.0137(8) 0.0130(7) C15 0.0289(9) 0.0294(9) 0.0255(9) -0.0142(7) -0.0108(7) 0.0135(7) C16 0.0222(8) 0.0267(8) 0.0192(8) -0.0113(7) -0.0044(7) 0.0046(6) C21 0.0147(7) 0.0226(8) 0.0123(7) -0.0077(6) -0.0009(5) 0.0062(5) C22 0.0159(7) 0.0215(7) 0.0101(7) -0.0059(6) 0.0013(5) 0.0044(5) C23 0.0232(8) 0.0220(8) 0.0156(8) -0.0066(6) -0.0007(6) 0.0053(6) C24 0.0316(9) 0.0292(9) 0.0180(8) -0.0073(7) -0.0079(7) 0.0160(7) C25 0.0277(9) 0.0396(10) 0.0194(9) -0.0156(7) -0.0122(7) 0.0148(7) C26 0.0213(8) 0.0278(9) 0.0200(8) -0.0146(7) -0.0058(6) 0.0097(6) C31 0.0164(7) 0.0177(7) 0.0157(7) -0.0074(6) -0.0051(6) -0.0009(5) C32 0.0259(8) 0.0211(7) 0.0137(8) -0.0070(6) -0.0052(6) 0.0034(6) C33 0.0249(8) 0.0234(8) 0.0234(9) -0.0122(7) -0.0070(7) 0.0061(6) C34 0.0249(8) 0.0176(7) 0.0240(8) -0.0080(6) -0.0125(7) 0.0026(6) C35 0.0245(8) 0.0217(8) 0.0174(8) -0.0045(6) -0.0076(6) -0.0019(6) C36 0.0190(7) 0.0242(8) 0.0162(8) -0.0073(6) -0.0046(6) -0.0014(6) C37 0.0409(11) 0.0265(10) 0.0320(11) -0.0099(8) -0.0195(9) 0.0141(8) C41 0.0179(7) 0.0143(7) 0.0175(7) -0.0095(6) -0.0082(6) 0.0043(5) C42 0.0175(7) 0.0163(7) 0.0193(8) -0.0070(6) -0.0053(6) 0.0012(5) C43 0.0259(8) 0.0165(7) 0.0204(8) -0.0049(6) -0.0086(7) 0.0002(6) C44 0.0271(8) 0.0162(7) 0.0294(9) -0.0099(6) -0.0175(7) 0.0057(6) C45 0.0201(8) 0.0266(8) 0.0299(9) -0.0138(7) -0.0096(7) 0.0073(6) C46 0.0199(7) 0.0262(8) 0.0191(8) -0.0090(6) -0.0058(6) 0.0036(6) C47 0.0313(10) 0.0215(9) 0.0408(11) -0.0066(8) -0.0200(9) 0.0044(7) C51 0.0136(6) 0.0108(6) 0.0107(6) -0.0038(5) -0.0027(5) 0.0025(5) C52 0.0136(6) 0.0106(6) 0.0134(7) -0.0054(5) -0.0032(5) 0.0035(5) C53 0.0131(6) 0.0136(6) 0.0094(7) -0.0050(5) -0.0010(5) 0.0011(5) C54 0.0145(6) 0.0124(6) 0.0096(6) -0.0037(5) -0.0025(5) 0.0018(5) C55 0.0168(7) 0.0132(6) 0.0112(7) -0.0050(5) -0.0026(5) 0.0033(5) C56 0.0249(8) 0.0209(8) 0.0179(8) -0.0125(6) -0.0087(6) 0.0080(6) C57 0.0157(7) 0.0185(7) 0.0159(8) -0.0070(6) -0.0009(6) 0.0017(6) C61 0.0172(7) 0.0110(6) 0.0139(7) -0.0028(5) -0.0057(6) -0.0002(5) C62 0.0180(7) 0.0174(7) 0.0146(7) -0.0048(6) -0.0034(6) 0.0030(5) C63 0.0208(8) 0.0192(7) 0.0239(8) -0.0070(6) -0.0097(7) 0.0061(6) C64 0.0289(8) 0.0176(7) 0.0175(8) -0.0023(6) -0.0111(7) 0.0034(6) C65 0.0300(8) 0.0212(8) 0.0134(8) -0.0031(6) -0.0058(7) 0.0051(6) C66 0.0196(7) 0.0182(7) 0.0149(7) -0.0044(6) -0.0027(6) 0.0042(6) C71 0.0161(7) 0.0140(6) 0.0083(6) -0.0021(5) -0.0027(5) -0.0007(5) C72 0.0196(7) 0.0180(7) 0.0177(8) -0.0075(6) -0.0061(6) 0.0022(6) C73 0.0197(8) 0.0314(9) 0.0259(9) -0.0126(7) -0.0112(7) 0.0043(6) C74 0.0255(8) 0.0265(8) 0.0210(8) -0.0101(7) -0.0092(7) -0.0054(6) C75 0.0289(8) 0.0206(8) 0.0202(8) -0.0109(7) -0.0042(7) -0.0023(6) C76 0.0199(7) 0.0174(7) 0.0177(8) -0.0079(6) -0.0033(6) 0.0009(6) C81 0.0138(7) 0.0123(6) 0.0163(7) -0.0085(5) -0.0036(6) 0.0027(5) C82 0.0171(7) 0.0144(7) 0.0156(7) -0.0061(6) -0.0046(6) 0.0024(5) C83 0.0162(7) 0.0177(7) 0.0200(8) -0.0076(6) 0.0012(6) -0.0005(6) C84 0.0137(7) 0.0232(8) 0.0336(9) -0.0167(7) -0.0050(6) 0.0021(6) C85 0.0201(7) 0.0188(7) 0.0250(8) -0.0128(6) -0.0107(6) 0.0043(6) C86 0.0202(7) 0.0131(6) 0.0147(7) -0.0075(6) -0.0046(6) 0.0016(5) C91 0.0122(6) 0.0120(6) 0.0129(7) -0.0004(5) -0.0008(5) 0.0009(5) C92 0.0223(7) 0.0179(7) 0.0173(8) -0.0052(6) -0.0036(6) 0.0017(6) C93 0.0265(8) 0.0144(7) 0.0244(9) -0.0053(6) -0.0008(7) 0.0033(6) C94 0.0221(8) 0.0153(7) 0.0223(9) 0.0031(6) -0.0038(7) 0.0032(6) C95 0.0227(8) 0.0229(8) 0.0176(8) -0.0014(6) -0.0079(6) -0.0003(6) C96 0.0195(7) 0.0169(7) 0.0170(8) -0.0045(6) -0.0044(6) 0.0009(5) _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 Ti O6 1.7880(10) . ? Ti O5 1.8014(10) . ? Ti O4 1.9611(11) . ? Ti O2 2.0002(11) . ? Ti O1 2.0304(11) . ? Ti O3 2.0604(11) . ? O1 C2 1.271(2) . ? O2 C4 1.2759(19) . ? O3 C6 1.2680(17) . ? O4 C8 1.2910(18) . ? O5 C51 1.4028(16) . ? O6 C54 1.4023(17) . ? O7 C55 1.4140(17) . ? O7 C52 1.4248(17) . ? O8 C53 1.4277(17) . ? O8 C55 1.4387(17) . ? C1 C2 1.509(2) . ? C1 C12 1.514(2) . ? C1 H1A 0.939(19) . ? C1 H1B 1.02(2) . ? C2 C3 1.393(2) . ? C3 C4 1.397(2) . ? C3 H3 0.97(2) . ? C4 C31 1.478(2) . ? C5 C22 1.509(2) . ? C5 C6 1.511(2) . ? C5 H5A 0.947(19) . ? C5 H5B 0.97(2) . ? C6 C7 1.392(2) . ? C7 C8 1.376(2) . ? C7 H7 0.98(2) . ? C8 C41 1.481(2) . ? C11 C16 1.398(2) . ? C11 C12 1.396(2) . ? C11 C21 1.492(2) . ? C12 C13 1.391(2) . ? C13 C14 1.386(3) . ? C13 H13 1.00(2) . ? C14 C15 1.375(3) . ? C14 H14 0.97(3) . ? C15 C16 1.377(2) . ? C15 H15 1.01(3) . ? C16 H16 1.01(2) . ? C21 C26 1.388(2) . ? C21 C22 1.401(2) . ? C22 C23 1.395(2) . ? C23 C24 1.378(3) . ? C23 H23 0.89(2) . ? C24 C25 1.383(3) . ? C24 H24 0.89(2) . ? C25 C26 1.383(2) . ? C25 H25 0.93(2) . ? C26 H26 0.97(2) . ? C31 C36 1.390(2) . ? C31 C32 1.394(2) . ? C32 C33 1.382(2) . ? C32 H32 0.94(2) . ? C33 C34 1.385(2) . ? C33 H33 0.98(2) . ? C34 C35 1.389(2) . ? C34 C37 1.510(2) . ? C35 C36 1.383(2) . ? C35 H35 1.01(2) . ? C36 H36 1.031(19) . ? C37 H37A 0.90(3) . ? C37 H37B 0.90(4) . ? C37 H37C 0.95(4) . ? C41 C42 1.393(2) . ? C41 C46 1.393(2) . ? C42 C43 1.375(2) . ? C42 H42 0.945(19) . ? C43 C44 1.393(2) . ? C43 H43 0.97(2) . ? C44 C45 1.381(3) . ? C44 C47 1.501(2) . ? C45 C46 1.385(2) . ? C45 H45 0.97(2) . ? C46 H46 1.00(2) . ? C47 H47A 0.92(3) . ? C47 H47B 1.01(4) . ? C47 H47C 0.94(3) . ? C51 C61 1.5293(19) . ? C51 C71 1.529(2) . ? C51 C52 1.5462(19) . ? C52 C53 1.5386(19) . ? C52 H52 0.981(17) . ? C53 C54 1.559(2) . ? C53 H53 0.965(18) . ? C54 C81 1.5278(19) . ? C54 C91 1.5342(19) . ? C55 C56 1.507(2) . ? C55 C57 1.508(2) . ? C56 H56A 0.95(2) . ? C56 H56B 0.93(2) . ? C56 H56C 0.88(2) . ? C57 H57A 0.97(2) . ? C57 H57B 0.85(2) . ? C57 H57C 0.996(19) . ? C61 C62 1.389(2) . ? C61 C66 1.386(2) . ? C62 C63 1.391(2) . ? C62 H62 0.90(2) . ? C63 C64 1.379(2) . ? C63 H63 0.93(2) . ? C64 C65 1.389(2) . ? C64 H64 0.96(2) . ? C65 C66 1.378(2) . ? C65 H65 0.94(2) . ? C66 H66 0.98(2) . ? C71 C72 1.390(2) . ? C71 C76 1.392(2) . ? C72 C73 1.390(2) . ? C72 H72 0.920(19) . ? C73 C74 1.374(3) . ? C73 H73 0.97(2) . ? C74 C75 1.378(3) . ? C74 H74 0.90(2) . ? C75 C76 1.387(2) . ? C75 H75 0.89(2) . ? C76 H76 0.945(18) . ? C81 C86 1.388(2) . ? C81 C82 1.391(2) . ? C82 C83 1.387(2) . ? C82 H82 0.97(2) . ? C83 C84 1.372(3) . ? C83 H83 0.85(2) . ? C84 C85 1.376(2) . ? C84 H84 0.93(2) . ? C85 C86 1.384(2) . ? C85 H85 0.95(2) . ? C86 H86 0.90(2) . ? C91 C96 1.381(2) . ? C91 C92 1.383(2) . ? C92 C93 1.383(2) . ? C92 H92 0.95(2) . ? C93 C94 1.376(3) . ? C93 H93 0.91(3) . ? C94 C95 1.379(3) . ? C94 H94 0.91(2) . ? C95 C96 1.390(2) . ? C95 H95 0.96(2) . ? C96 H96 0.91(2) . ? 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 O6 Ti O5 94.77(5) . . ? O6 Ti O4 92.81(5) . . ? O5 Ti O4 98.17(5) . . ? O6 Ti O2 95.80(5) . . ? O5 Ti O2 90.46(5) . . ? O4 Ti O2 167.27(4) . . ? O6 Ti O1 96.35(5) . . ? O5 Ti O1 166.98(4) . . ? O4 Ti O1 88.04(5) . . ? O2 Ti O1 81.71(4) . . ? O6 Ti O3 175.48(5) . . ? O5 Ti O3 88.24(4) . . ? O4 Ti O3 83.41(4) . . ? O2 Ti O3 87.54(4) . . ? O1 Ti O3 81.09(4) . . ? C2 O1 Ti 127.28(9) . . ? C4 O2 Ti 129.58(9) . . ? C6 O3 Ti 129.55(10) . . ? C8 O4 Ti 133.95(10) . . ? C51 O5 Ti 145.37(9) . . ? C54 O6 Ti 148.65(10) . . ? C55 O7 C52 107.50(10) . . ? C53 O8 C55 109.69(11) . . ? C2 C1 C12 111.86(13) . . ? C2 C1 H1A 109.0(12) . . ? C12 C1 H1A 108.1(12) . . ? C2 C1 H1B 107.1(10) . . ? C12 C1 H1B 109.6(10) . . ? H1A C1 H1B 111.2(16) . . ? O1 C2 C3 124.10(14) . . ? O1 C2 C1 115.99(14) . . ? C3 C2 C1 119.90(15) . . ? C2 C3 C4 121.55(15) . . ? C2 C3 H3 119.4(12) . . ? C4 C3 H3 118.4(13) . . ? O2 C4 C3 123.01(14) . . ? O2 C4 C31 116.58(13) . . ? C3 C4 C31 120.38(14) . . ? C22 C5 C6 114.74(13) . . ? C22 C5 H5A 110.4(12) . . ? C6 C5 H5A 105.9(12) . . ? C22 C5 H5B 109.2(13) . . ? C6 C5 H5B 108.6(13) . . ? H5A C5 H5B 107.8(17) . . ? O3 C6 C7 124.76(13) . . ? O3 C6 C5 115.80(13) . . ? C7 C6 C5 119.43(13) . . ? C8 C7 C6 123.23(13) . . ? C8 C7 H7 122.0(12) . . ? C6 C7 H7 114.7(12) . . ? O4 C8 C7 122.85(14) . . ? O4 C8 C41 114.95(13) . . ? C7 C8 C41 122.21(13) . . ? C16 C11 C12 118.75(15) . . ? C16 C11 C21 119.50(14) . . ? C12 C11 C21 121.74(14) . . ? C13 C12 C11 119.38(15) . . ? C13 C12 C1 118.51(15) . . ? C11 C12 C1 122.07(14) . . ? C14 C13 C12 120.88(16) . . ? C14 C13 H13 117.1(12) . . ? C12 C13 H13 122.0(12) . . ? C15 C14 C13 119.77(16) . . ? C15 C14 H14 122.6(15) . . ? C13 C14 H14 117.7(15) . . ? C14 C15 C16 120.02(17) . . ? C14 C15 H15 119.5(14) . . ? C16 C15 H15 120.4(14) . . ? C15 C16 C11 121.11(16) . . ? C15 C16 H16 120.0(12) . . ? C11 C16 H16 118.8(12) . . ? C26 C21 C22 119.22(15) . . ? C26 C21 C11 119.18(15) . . ? C22 C21 C11 121.57(15) . . ? C23 C22 C21 118.41(15) . . ? C23 C22 C5 118.76(15) . . ? C21 C22 C5 122.77(14) . . ? C24 C23 C22 121.69(17) . . ? C24 C23 H23 116.8(14) . . ? C22 C23 H23 121.5(14) . . ? C23 C24 C25 119.77(16) . . ? C23 C24 H24 119.7(14) . . ? C25 C24 H24 120.5(14) . . ? C26 C25 C24 119.21(17) . . ? C26 C25 H25 118.7(14) . . ? C24 C25 H25 122.1(14) . . ? C25 C26 C21 121.64(17) . . ? C25 C26 H26 121.5(13) . . ? C21 C26 H26 116.8(13) . . ? C36 C31 C32 118.77(15) . . ? C36 C31 C4 121.35(14) . . ? C32 C31 C4 119.88(14) . . ? C33 C32 C31 120.54(15) . . ? C33 C32 H32 123.3(12) . . ? C31 C32 H32 116.2(12) . . ? C32 C33 C34 120.80(15) . . ? C32 C33 H33 119.7(12) . . ? C34 C33 H33 118.9(12) . . ? C33 C34 C35 118.51(15) . . ? C33 C34 C37 120.89(17) . . ? C35 C34 C37 120.59(16) . . ? C36 C35 C34 121.14(15) . . ? C36 C35 H35 120.7(12) . . ? C34 C35 H35 118.0(12) . . ? C35 C36 C31 120.16(15) . . ? C35 C36 H36 119.7(10) . . ? C31 C36 H36 120.1(10) . . ? C34 C37 H37A 116.6(18) . . ? C34 C37 H37B 107(2) . . ? H37A C37 H37B 98(3) . . ? C34 C37 H37C 119(2) . . ? H37A C37 H37C 100(3) . . ? H37B C37 H37C 114(3) . . ? C42 C41 C46 118.77(14) . . ? C42 C41 C8 118.23(13) . . ? C46 C41 C8 122.96(14) . . ? C43 C42 C41 120.57(15) . . ? C43 C42 H42 119.8(11) . . ? C41 C42 H42 119.6(11) . . ? C42 C43 C44 120.95(16) . . ? C42 C43 H43 123.5(13) . . ? C44 C43 H43 115.4(13) . . ? C45 C44 C43 118.38(15) . . ? C45 C44 C47 122.08(16) . . ? C43 C44 C47 119.53(16) . . ? C44 C45 C46 121.27(15) . . ? C44 C45 H45 120.8(13) . . ? C46 C45 H45 117.9(13) . . ? C45 C46 C41 120.05(16) . . ? C45 C46 H46 120.6(13) . . ? C41 C46 H46 119.3(12) . . ? C44 C47 H47A 109.8(16) . . ? C44 C47 H47B 109(2) . . ? H47A C47 H47B 105(3) . . ? C44 C47 H47C 109.7(17) . . ? H47A C47 H47C 110(2) . . ? H47B C47 H47C 113(3) . . ? O5 C51 C61 107.60(12) . . ? O5 C51 C71 107.76(11) . . ? C61 C51 C71 109.98(11) . . ? O5 C51 C52 106.68(11) . . ? C61 C51 C52 111.47(11) . . ? C71 C51 C52 113.09(12) . . ? O7 C52 C53 103.54(11) . . ? O7 C52 C51 108.96(11) . . ? C53 C52 C51 115.60(11) . . ? O7 C52 H52 113.8(9) . . ? C53 C52 H52 109.6(9) . . ? C51 C52 H52 105.7(10) . . ? O8 C53 C52 104.02(11) . . ? O8 C53 C54 110.54(11) . . ? C52 C53 C54 116.11(12) . . ? O8 C53 H53 106.7(11) . . ? C52 C53 H53 111.5(10) . . ? C54 C53 H53 107.5(10) . . ? O6 C54 C81 107.91(12) . . ? O6 C54 C91 107.83(11) . . ? C81 C54 C91 110.01(11) . . ? O6 C54 C53 107.91(11) . . ? C81 C54 C53 111.50(11) . . ? C91 C54 C53 111.52(12) . . ? O7 C55 O8 104.81(11) . . ? O7 C55 C56 109.32(12) . . ? O8 C55 C56 107.50(12) . . ? O7 C55 C57 110.52(13) . . ? O8 C55 C57 111.59(12) . . ? C56 C55 C57 112.75(13) . . ? C55 C56 H56A 109.1(13) . . ? C55 C56 H56B 109.8(12) . . ? H56A C56 H56B 108.0(17) . . ? C55 C56 H56C 113.1(16) . . ? H56A C56 H56C 110(2) . . ? H56B C56 H56C 106.7(19) . . ? C55 C57 H57A 109.1(11) . . ? C55 C57 H57B 111.1(15) . . ? H57A C57 H57B 111.0(19) . . ? C55 C57 H57C 109.7(11) . . ? H57A C57 H57C 109.5(15) . . ? H57B C57 H57C 106.3(18) . . ? C62 C61 C66 118.75(14) . . ? C62 C61 C51 122.91(13) . . ? C66 C61 C51 118.33(13) . . ? C61 C62 C63 120.40(15) . . ? C61 C62 H62 123.7(13) . . ? C63 C62 H62 115.3(13) . . ? C64 C63 C62 120.38(15) . . ? C64 C63 H63 121.1(13) . . ? C62 C63 H63 118.4(13) . . ? C63 C64 C65 119.25(15) . . ? C63 C64 H64 123.5(13) . . ? C65 C64 H64 117.2(13) . . ? C66 C65 C64 120.35(16) . . ? C66 C65 H65 119.1(14) . . ? C64 C65 H65 120.5(14) . . ? C65 C66 C61 120.85(14) . . ? C65 C66 H66 116.0(12) . . ? C61 C66 H66 123.0(12) . . ? C72 C71 C76 118.52(14) . . ? C72 C71 C51 119.91(13) . . ? C76 C71 C51 121.52(13) . . ? C73 C72 C71 120.75(15) . . ? C73 C72 H72 121.1(11) . . ? C71 C72 H72 118.2(11) . . ? C74 C73 C72 119.92(16) . . ? C74 C73 H73 116.7(13) . . ? C72 C73 H73 123.4(13) . . ? C73 C74 C75 120.15(16) . . ? C73 C74 H74 120.2(14) . . ? C75 C74 H74 119.5(14) . . ? C74 C75 C76 120.17(16) . . ? C74 C75 H75 117.7(14) . . ? C76 C75 H75 122.0(14) . . ? C75 C76 C71 120.48(15) . . ? C75 C76 H76 118.9(11) . . ? C71 C76 H76 120.6(11) . . ? C86 C81 C82 119.11(13) . . ? C86 C81 C54 119.64(13) . . ? C82 C81 C54 121.23(13) . . ? C83 C82 C81 120.16(15) . . ? C83 C82 H82 119.6(12) . . ? C81 C82 H82 119.9(12) . . ? C84 C83 C82 120.22(15) . . ? C84 C83 H83 118.5(14) . . ? C82 C83 H83 121.3(14) . . ? C83 C84 C85 119.97(15) . . ? C83 C84 H84 120.9(13) . . ? C85 C84 H84 119.1(13) . . ? C84 C85 C86 120.47(15) . . ? C84 C85 H85 123.9(12) . . ? C86 C85 H85 115.5(12) . . ? C85 C86 C81 119.98(14) . . ? C85 C86 H86 120.9(12) . . ? C81 C86 H86 119.1(12) . . ? C96 C91 C92 118.74(14) . . ? C96 C91 C54 123.08(13) . . ? C92 C91 C54 118.15(14) . . ? C91 C92 C93 120.67(16) . . ? C91 C92 H92 122.1(12) . . ? C93 C92 H92 117.2(12) . . ? C94 C93 C92 120.47(16) . . ? C94 C93 H93 121.5(15) . . ? C92 C93 H93 117.8(16) . . ? C93 C94 C95 119.33(15) . . ? C93 C94 H94 116.3(15) . . ? C95 C94 H94 124.3(15) . . ? C94 C95 C96 120.21(17) . . ? C94 C95 H95 122.0(12) . . ? C96 C95 H95 117.8(12) . . ? C91 C96 C95 120.57(16) . . ? C91 C96 H96 123.3(13) . . ? C95 C96 H96 116.0(14) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.41 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.263 _refine_diff_density_min -0.210 _refine_diff_density_rms 0.041