# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Pascual Royo' _publ_contact_author_email PASCUAL.ROYO@UAH.ES loop_ _publ_author_name P.Royo M.E.G.Mosquera L.Postigo J.Sanchez-Nieves data_1a _database_code_depnum_ccdc_archive 'CCDC 708809' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H41 Cl2 O5 Si2 Ti2' _chemical_formula_weight 644.46 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.207(5) _cell_length_b 11.438(3) _cell_length_c 17.691(3) _cell_angle_alpha 90.00 _cell_angle_beta 116.591(10) _cell_angle_gamma 90.00 _cell_volume 3113.5(14) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 124 _cell_measurement_theta_min 3.025 _cell_measurement_theta_max 19.356 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.484 _exptl_crystal_size_mid 0.431 _exptl_crystal_size_min 0.362 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1348 _exptl_absorpt_coefficient_mu 0.793 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.489 _exptl_absorpt_correction_T_max 0.748 _exptl_special_details ; ? ; _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_ub_11 0.01 _diffrn_orient_matrix_ub_12 0 _diffrn_orient_matrix_ub_13 0 _diffrn_orient_matrix_ub_21 0 _diffrn_orient_matrix_ub_22 0.01 _diffrn_orient_matrix_ub_23 0 _diffrn_orient_matrix_ub_31 0 _diffrn_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_number 67211 _diffrn_reflns_av_R_equivalents 0.0667 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 27.51 _reflns_number_total 7118 _reflns_number_gt 5687 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0737P)^2^+10.2233P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.058(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7118 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_gt 0.0646 _refine_ls_wR_factor_ref 0.1711 _refine_ls_wR_factor_gt 0.1616 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 0.000 0.500 218.0 2.0 2 0.500 0.500 1.000 218.0 2.3 _platon_squeeze_details ;Half a molecule of hexane crystallize with every molecule of this compound but presented severe disorder and it was not possible to get a chemical sensible model for it, so Squeeze procedure was used to remove its contribution to the structure factors. ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.20209(4) 0.14064(6) 0.06115(4) 0.01612(19) Uani 1 1 d . . . Ti2 Ti 0.17148(4) -0.08985(6) -0.15430(4) 0.01612(19) Uani 1 1 d . . . Si1 Si 0.33348(7) -0.07431(9) 0.05569(6) 0.0188(2) Uani 1 1 d . . . Si2 Si 0.32514(7) 0.11198(9) -0.05585(6) 0.0179(2) Uani 1 1 d . . . Cl1 Cl 0.20666(8) 0.15948(10) 0.19318(6) 0.0314(3) Uani 1 1 d . . . Cl2 Cl 0.11359(7) -0.10365(10) -0.29989(6) 0.0311(3) Uani 1 1 d . . . O5 O 0.09132(17) 0.0987(3) -0.00349(17) 0.0223(6) Uani 1 1 d . . . O4 O 0.07995(18) -0.0369(3) -0.14329(18) 0.0235(6) Uani 1 1 d . . . O1 O 0.26278(18) 0.0019(2) 0.07375(17) 0.0212(6) Uani 1 1 d . . . O3 O 0.38390(17) 0.0176(2) 0.02016(17) 0.0212(6) Uani 1 1 d . . . O2 O 0.24423(17) 0.0391(2) -0.12912(16) 0.0199(5) Uani 1 1 d . . . C1 C 0.0116(2) 0.0866(4) -0.0778(2) 0.0215(8) Uani 1 1 d . . . H1A H 0.0045 0.1526 -0.1166 0.026 Uiso 1 1 calc R . . H1B H -0.0374 0.0889 -0.0628 0.026 Uiso 1 1 calc R . . C2 C 0.0095(2) -0.0291(4) -0.1223(2) 0.0221(8) Uani 1 1 d . . . H2A H 0.0126 -0.0950 -0.0849 0.027 Uiso 1 1 calc R . . H2B H -0.0460 -0.0353 -0.1745 0.027 Uiso 1 1 calc R . . C3 C 0.3966(3) 0.1796(4) -0.0970(3) 0.0310(9) Uani 1 1 d . . . H3A H 0.4438 0.2220 -0.0514 0.046 Uiso 1 1 calc R . . H3B H 0.3626 0.2342 -0.1427 0.046 Uiso 1 1 calc R . . H3C H 0.4211 0.1184 -0.1188 0.046 Uiso 1 1 calc R . . C4 C 0.4117(3) -0.1454(4) 0.1554(3) 0.0338(10) Uani 1 1 d . . . H4A H 0.4541 -0.1907 0.1447 0.051 Uiso 1 1 calc R . . H4B H 0.3802 -0.1976 0.1761 0.051 Uiso 1 1 calc R . . H4C H 0.4420 -0.0853 0.1980 0.051 Uiso 1 1 calc R . . C10 C 0.2793(2) 0.2208(3) -0.0059(2) 0.0183(7) Uani 1 1 d . . . C11 C 0.1944(3) 0.2746(3) -0.0451(2) 0.0211(8) Uani 1 1 d . . . C12 C 0.1837(3) 0.3437(3) 0.0170(3) 0.0229(8) Uani 1 1 d . . . C13 C 0.2636(3) 0.3389(3) 0.0936(2) 0.0226(8) Uani 1 1 d . . . C14 C 0.3213(3) 0.2624(3) 0.0800(2) 0.0217(8) Uani 1 1 d . . . C15 C 0.1310(3) 0.2707(4) -0.1383(2) 0.0242(8) Uani 1 1 d . . . H15A H 0.1528 0.2170 -0.1676 0.036 Uiso 1 1 calc R . . H15B H 0.1249 0.3492 -0.1626 0.036 Uiso 1 1 calc R . . H15C H 0.0743 0.2435 -0.1450 0.036 Uiso 1 1 calc R . . C16 C 0.1043(3) 0.4119(4) 0.0059(3) 0.0340(10) Uani 1 1 d . . . H16A H 0.0583 0.4014 -0.0518 0.051 Uiso 1 1 calc R . . H16B H 0.1191 0.4951 0.0162 0.051 Uiso 1 1 calc R . . H16C H 0.0840 0.3837 0.0463 0.051 Uiso 1 1 calc R . . C17 C 0.2837(3) 0.4111(4) 0.1719(3) 0.0327(10) Uani 1 1 d . . . H17A H 0.2320 0.4557 0.1641 0.049 Uiso 1 1 calc R . . H17B H 0.3314 0.4652 0.1814 0.049 Uiso 1 1 calc R . . H17C H 0.3008 0.3592 0.2208 0.049 Uiso 1 1 calc R . . C18 C 0.4128(3) 0.2340(4) 0.1466(3) 0.0305(9) Uani 1 1 d . . . H18A H 0.4403 0.1798 0.1228 0.046 Uiso 1 1 calc R . . H18B H 0.4102 0.1977 0.1956 0.046 Uiso 1 1 calc R . . H18C H 0.4470 0.3061 0.1643 0.046 Uiso 1 1 calc R . . C20 C 0.2734(2) -0.1805(3) -0.0329(2) 0.0202(8) Uani 1 1 d . . . C21 C 0.1916(3) -0.2362(3) -0.0500(2) 0.0218(8) Uani 1 1 d . . . C22 C 0.1608(3) -0.2978(3) -0.1284(3) 0.0248(8) Uani 1 1 d . . . C23 C 0.2259(3) -0.2857(4) -0.1581(3) 0.0256(8) Uani 1 1 d . . . C24 C 0.2948(3) -0.2148(4) -0.1003(2) 0.0233(8) Uani 1 1 d . . . C25 C 0.1503(3) -0.2372(4) 0.0090(3) 0.0271(9) Uani 1 1 d . . . H25A H 0.1844 -0.1883 0.0583 0.041 Uiso 1 1 calc R . . H25B H 0.1486 -0.3175 0.0275 0.041 Uiso 1 1 calc R . . H25C H 0.0910 -0.2064 -0.0203 0.041 Uiso 1 1 calc R . . C26 C 0.0766(3) -0.3648(4) -0.1720(3) 0.0367(11) Uani 1 1 d . . . H26A H 0.0720 -0.3981 -0.2249 0.055 Uiso 1 1 calc R . . H26B H 0.0276 -0.3118 -0.1844 0.055 Uiso 1 1 calc R . . H26C H 0.0755 -0.4280 -0.1351 0.055 Uiso 1 1 calc R . . C27 C 0.2236(4) -0.3468(5) -0.2352(3) 0.0410(12) Uani 1 1 d . . . H27A H 0.1690 -0.3901 -0.2640 0.062 Uiso 1 1 calc R . . H27B H 0.2726 -0.4012 -0.2175 0.062 Uiso 1 1 calc R . . H27C H 0.2278 -0.2886 -0.2738 0.062 Uiso 1 1 calc R . . C28 C 0.3763(3) -0.1854(4) -0.1100(3) 0.0336(10) Uani 1 1 d . . . H28A H 0.4144 -0.1353 -0.0630 0.050 Uiso 1 1 calc R . . H28B H 0.3598 -0.1443 -0.1636 0.050 Uiso 1 1 calc R . . H28C H 0.4070 -0.2577 -0.1096 0.050 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0170(3) 0.0165(3) 0.0152(3) -0.0010(2) 0.0075(3) -0.0011(2) Ti2 0.0143(3) 0.0182(3) 0.0149(3) -0.0014(2) 0.0057(3) -0.0010(2) Si1 0.0158(5) 0.0205(5) 0.0162(5) 0.0000(4) 0.0037(4) 0.0033(4) Si2 0.0151(5) 0.0216(5) 0.0175(5) -0.0024(4) 0.0077(4) -0.0034(4) Cl1 0.0454(6) 0.0334(6) 0.0223(5) -0.0051(4) 0.0212(5) -0.0081(4) Cl2 0.0351(6) 0.0376(6) 0.0167(4) -0.0033(4) 0.0080(4) -0.0075(4) O5 0.0177(13) 0.0263(14) 0.0219(14) 0.0025(11) 0.0079(11) -0.0020(11) O4 0.0204(13) 0.0273(15) 0.0264(14) 0.0014(11) 0.0135(11) 0.0007(11) O1 0.0215(13) 0.0207(13) 0.0212(13) 0.0003(10) 0.0093(11) -0.0008(10) O3 0.0156(12) 0.0251(14) 0.0209(13) -0.0015(11) 0.0063(10) -0.0010(10) O2 0.0197(13) 0.0203(13) 0.0184(13) -0.0016(10) 0.0073(11) -0.0013(10) C1 0.0131(16) 0.029(2) 0.0204(18) 0.0023(15) 0.0058(14) 0.0029(14) C2 0.0167(17) 0.029(2) 0.0223(18) 0.0022(15) 0.0100(15) -0.0011(15) C3 0.025(2) 0.038(2) 0.035(2) -0.0006(19) 0.0176(18) -0.0073(18) C4 0.027(2) 0.039(3) 0.027(2) 0.0087(18) 0.0043(18) 0.0076(19) C10 0.0178(17) 0.0189(18) 0.0180(17) -0.0013(13) 0.0079(14) -0.0040(14) C11 0.0228(19) 0.0206(18) 0.0191(18) 0.0030(14) 0.0087(15) -0.0007(14) C12 0.031(2) 0.0164(18) 0.0231(19) 0.0029(14) 0.0136(17) 0.0007(15) C13 0.030(2) 0.0180(18) 0.0212(18) -0.0027(14) 0.0127(16) -0.0045(15) C14 0.025(2) 0.0196(18) 0.0203(18) -0.0035(14) 0.0100(16) -0.0057(15) C15 0.026(2) 0.029(2) 0.0168(18) 0.0031(15) 0.0093(16) 0.0022(16) C16 0.037(2) 0.030(2) 0.034(2) 0.0027(18) 0.015(2) 0.0135(19) C17 0.042(3) 0.027(2) 0.029(2) -0.0107(17) 0.017(2) -0.0077(19) C18 0.022(2) 0.031(2) 0.029(2) -0.0052(17) 0.0034(17) -0.0042(17) C20 0.0214(18) 0.0181(18) 0.0187(17) 0.0017(14) 0.0068(15) 0.0046(14) C21 0.0247(19) 0.0165(17) 0.0210(18) 0.0011(14) 0.0074(16) 0.0005(14) C22 0.028(2) 0.0184(19) 0.025(2) -0.0033(15) 0.0094(17) -0.0021(15) C23 0.028(2) 0.0222(19) 0.0238(19) -0.0062(15) 0.0088(16) 0.0022(16) C24 0.0192(18) 0.025(2) 0.0217(18) -0.0022(15) 0.0051(15) 0.0063(15) C25 0.030(2) 0.029(2) 0.025(2) 0.0031(16) 0.0151(18) -0.0020(17) C26 0.042(3) 0.030(2) 0.031(2) -0.0050(18) 0.010(2) -0.013(2) C27 0.046(3) 0.039(3) 0.035(3) -0.021(2) 0.014(2) 0.001(2) C28 0.026(2) 0.042(3) 0.032(2) -0.0069(19) 0.0126(19) 0.0063(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O5 1.794(3) . ? Ti1 O1 1.857(3) . ? Ti1 Cl1 2.3116(12) . ? Ti1 C10 2.329(4) . ? Ti1 C14 2.377(4) . ? Ti1 C11 2.383(4) . ? Ti1 C12 2.426(4) . ? Ti1 C13 2.459(4) . ? Ti2 O4 1.778(3) . ? Ti2 O2 1.856(3) . ? Ti2 Cl2 2.3140(12) . ? Ti2 C20 2.322(4) . ? Ti2 C24 2.375(4) . ? Ti2 C21 2.398(4) . ? Ti2 C23 2.441(4) . ? Ti2 C22 2.444(4) . ? Si1 O1 1.640(3) . ? Si1 O3 1.655(3) . ? Si1 C4 1.860(4) . ? Si1 C20 1.884(4) . ? Si2 O2 1.642(3) . ? Si2 O3 1.667(3) . ? Si2 C3 1.856(4) . ? Si2 C10 1.891(4) . ? O5 C1 1.420(4) . ? O4 C2 1.420(5) . ? C1 C2 1.532(6) . ? C10 C11 1.444(5) . ? C10 C14 1.441(5) . ? C11 C12 1.431(6) . ? C11 C15 1.516(5) . ? C12 C13 1.436(6) . ? C12 C16 1.508(6) . ? C13 C14 1.423(6) . ? C13 C17 1.513(5) . ? C14 C18 1.520(6) . ? C20 C21 1.448(5) . ? C20 C24 1.450(5) . ? C21 C22 1.428(5) . ? C21 C25 1.504(6) . ? C22 C23 1.442(6) . ? C22 C26 1.511(6) . ? C23 C24 1.423(6) . ? C23 C27 1.516(6) . ? C24 C28 1.524(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Ti1 O1 103.18(13) . . ? O5 Ti1 Cl1 102.41(10) . . ? O1 Ti1 Cl1 101.27(9) . . ? O5 Ti1 C10 117.77(13) . . ? O1 Ti1 C10 88.81(13) . . ? Cl1 Ti1 C10 135.14(10) . . ? O5 Ti1 C14 148.24(13) . . ? O1 Ti1 C14 94.58(13) . . ? Cl1 Ti1 C14 99.59(10) . . ? C10 Ti1 C14 35.65(12) . . ? O5 Ti1 C11 90.06(13) . . ? O1 Ti1 C11 118.27(13) . . ? Cl1 Ti1 C11 134.59(10) . . ? C10 Ti1 C11 35.67(13) . . ? C14 Ti1 C11 58.23(13) . . ? O5 Ti1 C12 95.88(14) . . ? O1 Ti1 C12 147.35(13) . . ? Cl1 Ti1 C12 100.18(10) . . ? C10 Ti1 C12 58.72(14) . . ? C14 Ti1 C12 57.61(14) . . ? C11 Ti1 C12 34.61(13) . . ? O5 Ti1 C13 128.21(14) . . ? O1 Ti1 C13 126.85(13) . . ? Cl1 Ti1 C13 82.05(10) . . ? C10 Ti1 C13 58.12(13) . . ? C14 Ti1 C13 34.18(13) . . ? C11 Ti1 C13 57.13(13) . . ? C12 Ti1 C13 34.17(14) . . ? O4 Ti2 O2 103.77(13) . . ? O4 Ti2 Cl2 100.61(10) . . ? O2 Ti2 Cl2 103.27(9) . . ? O4 Ti2 C20 112.96(14) . . ? O2 Ti2 C20 89.09(13) . . ? Cl2 Ti2 C20 140.34(10) . . ? O4 Ti2 C24 146.79(14) . . ? O2 Ti2 C24 89.80(14) . . ? Cl2 Ti2 C24 105.60(10) . . ? C20 Ti2 C24 35.95(13) . . ? O4 Ti2 C21 89.07(14) . . ? O2 Ti2 C21 121.38(13) . . ? Cl2 Ti2 C21 130.57(10) . . ? C20 Ti2 C21 35.67(13) . . ? C24 Ti2 C21 58.35(15) . . ? O4 Ti2 C23 133.31(15) . . ? O2 Ti2 C23 120.68(14) . . ? Cl2 Ti2 C23 83.45(10) . . ? C20 Ti2 C23 58.36(13) . . ? C24 Ti2 C23 34.33(13) . . ? C21 Ti2 C23 57.02(14) . . ? O4 Ti2 C22 99.60(14) . . ? O2 Ti2 C22 145.86(13) . . ? Cl2 Ti2 C22 96.40(10) . . ? C20 Ti2 C22 58.73(14) . . ? C24 Ti2 C22 57.84(15) . . ? C21 Ti2 C22 34.28(13) . . ? C23 Ti2 C22 34.33(15) . . ? O1 Si1 O3 107.27(15) . . ? O1 Si1 C4 109.42(19) . . ? O3 Si1 C4 110.97(19) . . ? O1 Si1 C20 109.02(16) . . ? O3 Si1 C20 106.22(16) . . ? C4 Si1 C20 113.7(2) . . ? O2 Si2 O3 107.57(15) . . ? O2 Si2 C3 112.22(18) . . ? O3 Si2 C3 108.51(19) . . ? O2 Si2 C10 108.61(16) . . ? O3 Si2 C10 106.19(16) . . ? C3 Si2 C10 113.4(2) . . ? C1 O5 Ti1 158.0(3) . . ? C2 O4 Ti2 162.1(3) . . ? Si1 O1 Ti1 148.98(18) . . ? Si1 O3 Si2 119.06(16) . . ? Si2 O2 Ti2 146.65(17) . . ? O5 C1 C2 110.5(3) . . ? O4 C2 C1 111.3(3) . . ? C11 C10 C14 106.8(3) . . ? C11 C10 Si2 126.9(3) . . ? C14 C10 Si2 126.3(3) . . ? C11 C10 Ti1 74.2(2) . . ? C14 C10 Ti1 74.0(2) . . ? Si2 C10 Ti1 115.54(18) . . ? C12 C11 C10 108.5(3) . . ? C12 C11 C15 125.0(4) . . ? C10 C11 C15 126.2(4) . . ? C12 C11 Ti1 74.3(2) . . ? C10 C11 Ti1 70.1(2) . . ? C15 C11 Ti1 126.7(3) . . ? C13 C12 C11 107.8(4) . . ? C13 C12 C16 124.8(4) . . ? C11 C12 C16 127.4(4) . . ? C13 C12 Ti1 74.2(2) . . ? C11 C12 Ti1 71.0(2) . . ? C16 C12 Ti1 121.1(3) . . ? C14 C13 C12 108.1(3) . . ? C14 C13 C17 126.8(4) . . ? C12 C13 C17 125.0(4) . . ? C14 C13 Ti1 69.7(2) . . ? C12 C13 Ti1 71.6(2) . . ? C17 C13 Ti1 128.0(3) . . ? C13 C14 C10 108.8(3) . . ? C13 C14 C18 124.1(4) . . ? C10 C14 C18 127.2(4) . . ? C13 C14 Ti1 76.1(2) . . ? C10 C14 Ti1 70.4(2) . . ? C18 C14 Ti1 120.9(3) . . ? C21 C20 C24 106.8(3) . . ? C21 C20 Si1 125.3(3) . . ? C24 C20 Si1 127.7(3) . . ? C21 C20 Ti2 75.0(2) . . ? C24 C20 Ti2 74.0(2) . . ? Si1 C20 Ti2 112.80(18) . . ? C22 C21 C20 108.9(4) . . ? C22 C21 C25 125.8(4) . . ? C20 C21 C25 125.1(4) . . ? C22 C21 Ti2 74.6(2) . . ? C20 C21 Ti2 69.3(2) . . ? C25 C21 Ti2 126.1(3) . . ? C21 C22 C23 107.2(4) . . ? C21 C22 C26 126.9(4) . . ? C23 C22 C26 125.9(4) . . ? C21 C22 Ti2 71.1(2) . . ? C23 C22 Ti2 72.7(2) . . ? C26 C22 Ti2 122.2(3) . . ? C24 C23 C22 108.9(4) . . ? C24 C23 C27 126.0(4) . . ? C22 C23 C27 124.9(4) . . ? C24 C23 Ti2 70.3(2) . . ? C22 C23 Ti2 73.0(2) . . ? C27 C23 Ti2 126.3(3) . . ? C23 C24 C20 108.0(4) . . ? C23 C24 C28 123.8(4) . . ? C20 C24 C28 128.2(4) . . ? C23 C24 Ti2 75.4(2) . . ? C20 C24 Ti2 70.0(2) . . ? C28 C24 Ti2 121.5(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.664 _refine_diff_density_min -0.617 _refine_diff_density_rms 0.128 #====== END data_1b _database_code_depnum_ccdc_archive 'CCDC 708810' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H34 Cl2 O5 Si2 Ti2' _chemical_formula_weight 649.41 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.112(3) _cell_length_b 10.4098(7) _cell_length_c 21.228(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.083(14) _cell_angle_gamma 90.00 _cell_volume 3024.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 123 _cell_measurement_theta_max 21.373 _cell_measurement_theta_min 5.364 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.496 _exptl_crystal_size_mid 0.347 _exptl_crystal_size_min 0.313 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 0.817 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.654 _exptl_absorpt_correction_T_max 0.775 _exptl_special_details ; ? ; _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_ub_11 0.01 _diffrn_orient_matrix_ub_12 0 _diffrn_orient_matrix_ub_13 0 _diffrn_orient_matrix_ub_21 0 _diffrn_orient_matrix_ub_22 0.01 _diffrn_orient_matrix_ub_23 0 _diffrn_orient_matrix_ub_31 0 _diffrn_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_number 21976 _diffrn_reflns_av_R_equivalents 0.0674 _diffrn_reflns_av_sigmaI/netI 0.0684 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6948 _reflns_number_gt 4787 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0541P)^2^+1.3284P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6948 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0808 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.1184 _refine_ls_wR_factor_gt 0.1067 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.14607(3) 0.88090(5) 0.67354(2) 0.02391(14) Uani 1 1 d . . . Ti2 Ti 0.36572(3) 1.07220(5) 0.83419(2) 0.02240(13) Uani 1 1 d . . . Si1 Si 0.16923(5) 1.19373(7) 0.71234(4) 0.02414(18) Uani 1 1 d . . . Si2 Si 0.34212(5) 1.10411(7) 0.67559(4) 0.02265(18) Uani 1 1 d . . . Cl1 Cl -0.01196(5) 0.82509(8) 0.62537(4) 0.0398(2) Uani 1 1 d . . . Cl2 Cl 0.51760(5) 1.06099(8) 0.90394(4) 0.0402(2) Uani 1 1 d . . . O1 O 0.12831(13) 1.04581(17) 0.69929(9) 0.0271(4) Uani 1 1 d . . . O2 O 0.39200(13) 1.08031(18) 0.75300(9) 0.0244(4) Uani 1 1 d . . . O3 O 0.25357(13) 1.21143(17) 0.67048(9) 0.0248(4) Uani 1 1 d . . . O4 O 0.32336(14) 0.90845(18) 0.83627(10) 0.0309(5) Uani 1 1 d . . . O5 O 0.16991(14) 0.79018(19) 0.74897(10) 0.0325(5) Uani 1 1 d . . . C1 C 0.28250(19) 0.9504(3) 0.63910(13) 0.0234(6) Uani 1 1 d . . . C2 C 0.30179(19) 0.8187(3) 0.66095(13) 0.0259(6) Uani 1 1 d . . . C3 C 0.2342(2) 0.7367(3) 0.61887(14) 0.0287(6) Uani 1 1 d . . . C4 C 0.1741(2) 0.8133(3) 0.56865(14) 0.0318(7) Uani 1 1 d . . . C5 C 0.2021(2) 0.9445(3) 0.58102(14) 0.0276(6) Uani 1 1 d . . . C6 C 0.1572(2) 1.0572(3) 0.53976(14) 0.0370(7) Uani 1 1 d . . . H6A H 0.1888 1.1350 0.5580 0.055 Uiso 1 1 calc R . . H6B H 0.0888 1.0619 0.5386 0.055 Uiso 1 1 calc R . . H6C H 0.1652 1.0463 0.4965 0.055 Uiso 1 1 calc R . . C7 C 0.0994(2) 0.7611(3) 0.51079(16) 0.0430(8) Uani 1 1 d . . . H7A H 0.0947 0.6696 0.5149 0.065 Uiso 1 1 calc R . . H7B H 0.1192 0.7810 0.4717 0.065 Uiso 1 1 calc R . . H7C H 0.0370 0.7995 0.5090 0.065 Uiso 1 1 calc R . . C8 C 0.2274(2) 0.5924(3) 0.62545(17) 0.0391(8) Uani 1 1 d . . . H8A H 0.1758 0.5598 0.5910 0.059 Uiso 1 1 calc R . . H8B H 0.2140 0.5720 0.6665 0.059 Uiso 1 1 calc R . . H8C H 0.2882 0.5538 0.6230 0.059 Uiso 1 1 calc R . . C9 C 0.3828(2) 0.7707(3) 0.71584(14) 0.0290(7) Uani 1 1 d . . . H9A H 0.4193 0.8424 0.7377 0.043 Uiso 1 1 calc R . . H9B H 0.4253 0.7158 0.6989 0.043 Uiso 1 1 calc R . . H9C H 0.3554 0.7234 0.7460 0.043 Uiso 1 1 calc R . . C13 C 0.2087(2) 0.7352(3) 0.80781(14) 0.0266(6) Uani 1 1 d . . . C14 C 0.1723(2) 0.6195(3) 0.82509(15) 0.0325(7) Uani 1 1 d . . . H14 H 0.1227 0.5772 0.7955 0.039 Uiso 1 1 calc R . . C15 C 0.2096(3) 0.5669(3) 0.88632(17) 0.0411(8) Uani 1 1 d . . . H15 H 0.1850 0.4894 0.8974 0.049 Uiso 1 1 calc R . . C16 C 0.2833(2) 0.6294(3) 0.93089(16) 0.0377(8) Uani 1 1 d . . . H16 H 0.3078 0.5938 0.9718 0.045 Uiso 1 1 calc R . . C17 C 0.3208(2) 0.7447(3) 0.91487(14) 0.0307(7) Uani 1 1 d . . . H17 H 0.3698 0.7866 0.9451 0.037 Uiso 1 1 calc R . . C18 C 0.2848(2) 0.7983(3) 0.85313(14) 0.0253(6) Uani 1 1 d . . . C21 C 0.4311(2) 1.1670(3) 0.63194(15) 0.0330(7) Uani 1 1 d . . . H21A H 0.3991 1.1795 0.5870 0.049 Uiso 1 1 calc R . . H21B H 0.4836 1.1065 0.6355 0.049 Uiso 1 1 calc R . . H21C H 0.4568 1.2474 0.6507 0.049 Uiso 1 1 calc R . . C22 C 0.0701(2) 1.3123(3) 0.68562(16) 0.0353(7) Uani 1 1 d . . . H22A H 0.0962 1.3975 0.6939 0.053 Uiso 1 1 calc R . . H22B H 0.0209 1.2989 0.7091 0.053 Uiso 1 1 calc R . . H22C H 0.0419 1.3020 0.6400 0.053 Uiso 1 1 calc R . . C23 C 0.1320(2) 1.0421(3) 0.85204(16) 0.0354(7) Uani 1 1 d . . . H23A H 0.0932 1.0356 0.8082 0.053 Uiso 1 1 calc R . . H23B H 0.0920 1.0725 0.8796 0.053 Uiso 1 1 calc R . . H23C H 0.1580 0.9592 0.8667 0.053 Uiso 1 1 calc R . . C24 C 0.2336(2) 1.2086(3) 0.80073(14) 0.0253(6) Uani 1 1 d . . . C25 C 0.2150(2) 1.1352(3) 0.85454(14) 0.0276(6) Uani 1 1 d . . . C26 C 0.2871(2) 1.1684(3) 0.91175(14) 0.0316(7) Uani 1 1 d . . . C27 C 0.3493(2) 1.2651(3) 0.89499(14) 0.0299(7) Uani 1 1 d . . . C28 C 0.3163(2) 1.2913(3) 0.82708(14) 0.0263(6) Uani 1 1 d . . . C29 C 0.3599(2) 1.3918(3) 0.79163(15) 0.0331(7) Uani 1 1 d . . . H29A H 0.3257 1.3922 0.7466 0.050 Uiso 1 1 calc R . . H29B H 0.4276 1.3728 0.7955 0.050 Uiso 1 1 calc R . . H29C H 0.3541 1.4747 0.8102 0.050 Uiso 1 1 calc R . . C30 C 0.4324(3) 1.3335(3) 0.94127(16) 0.0461(9) Uani 1 1 d . . . H30A H 0.4406 1.2986 0.9841 0.069 Uiso 1 1 calc R . . H30B H 0.4178 1.4235 0.9419 0.069 Uiso 1 1 calc R . . H30C H 0.4915 1.3218 0.9272 0.069 Uiso 1 1 calc R . . C31 C 0.2954(3) 1.1122(3) 0.97851(15) 0.0464(9) Uani 1 1 d . . . H31A H 0.3499 1.1505 1.0087 0.070 Uiso 1 1 calc R . . H31B H 0.3051 1.0211 0.9771 0.070 Uiso 1 1 calc R . . H31C H 0.2366 1.1294 0.9921 0.070 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0209(3) 0.0234(3) 0.0268(3) 0.0029(2) 0.0046(2) 0.0002(2) Ti2 0.0227(3) 0.0222(3) 0.0218(3) 0.0041(2) 0.0045(2) 0.0016(2) Si1 0.0201(4) 0.0229(4) 0.0278(4) 0.0037(3) 0.0029(3) 0.0034(3) Si2 0.0213(4) 0.0249(4) 0.0218(4) 0.0040(3) 0.0052(3) 0.0000(3) Cl1 0.0251(4) 0.0436(5) 0.0473(5) 0.0024(4) 0.0023(3) -0.0079(3) Cl2 0.0298(4) 0.0534(5) 0.0320(4) 0.0051(4) -0.0028(3) 0.0069(4) O1 0.0240(10) 0.0263(10) 0.0312(11) 0.0008(8) 0.0069(8) 0.0004(8) O2 0.0224(10) 0.0263(10) 0.0240(10) 0.0037(8) 0.0046(8) 0.0005(8) O3 0.0253(10) 0.0235(10) 0.0247(10) 0.0063(8) 0.0039(8) 0.0001(8) O4 0.0320(11) 0.0246(11) 0.0386(12) 0.0045(9) 0.0134(9) 0.0007(9) O5 0.0324(11) 0.0346(12) 0.0313(12) 0.0077(9) 0.0091(9) 0.0044(9) C1 0.0218(14) 0.0275(15) 0.0217(14) 0.0022(11) 0.0068(11) 0.0020(12) C2 0.0232(14) 0.0305(16) 0.0257(15) 0.0016(12) 0.0091(12) 0.0035(12) C3 0.0292(15) 0.0272(15) 0.0308(16) -0.0020(13) 0.0093(13) -0.0002(12) C4 0.0296(16) 0.0380(18) 0.0271(16) -0.0039(13) 0.0056(13) -0.0029(13) C5 0.0246(15) 0.0346(16) 0.0230(15) 0.0001(12) 0.0047(12) 0.0010(12) C6 0.0428(19) 0.0398(19) 0.0234(16) 0.0046(14) -0.0016(13) 0.0019(15) C7 0.0413(19) 0.048(2) 0.0343(19) -0.0075(16) -0.0008(15) -0.0044(16) C8 0.0412(19) 0.0276(16) 0.049(2) -0.0042(15) 0.0114(15) 0.0010(14) C9 0.0253(15) 0.0292(16) 0.0323(17) 0.0017(13) 0.0068(12) 0.0053(12) C13 0.0281(15) 0.0259(15) 0.0296(16) 0.0060(12) 0.0142(12) 0.0082(12) C14 0.0335(17) 0.0280(16) 0.0387(18) 0.0003(14) 0.0142(14) -0.0001(13) C15 0.053(2) 0.0263(16) 0.051(2) 0.0134(15) 0.0260(17) 0.0032(15) C16 0.0459(19) 0.0356(18) 0.0341(18) 0.0158(14) 0.0145(15) 0.0062(15) C17 0.0292(16) 0.0346(17) 0.0284(16) 0.0031(13) 0.0072(12) 0.0056(13) C18 0.0271(15) 0.0190(14) 0.0336(17) 0.0053(12) 0.0143(13) 0.0051(12) C21 0.0307(16) 0.0364(17) 0.0322(17) 0.0089(14) 0.0084(13) -0.0026(14) C22 0.0294(16) 0.0331(17) 0.0408(19) 0.0054(14) 0.0037(14) 0.0102(14) C23 0.0336(17) 0.0322(17) 0.045(2) 0.0031(14) 0.0182(15) 0.0037(13) C24 0.0254(14) 0.0225(14) 0.0294(16) 0.0031(12) 0.0097(12) 0.0061(12) C25 0.0304(16) 0.0248(15) 0.0312(16) 0.0003(12) 0.0142(13) 0.0059(12) C26 0.0408(18) 0.0285(16) 0.0273(16) 0.0015(13) 0.0114(13) 0.0103(14) C27 0.0353(16) 0.0241(15) 0.0282(16) -0.0034(12) 0.0038(13) 0.0029(13) C28 0.0277(15) 0.0224(14) 0.0281(16) 0.0009(12) 0.0056(12) 0.0039(12) C29 0.0358(17) 0.0223(15) 0.0413(19) 0.0019(13) 0.0095(14) -0.0020(13) C30 0.058(2) 0.0378(19) 0.0343(19) -0.0054(15) -0.0052(16) 0.0010(17) C31 0.070(2) 0.043(2) 0.0295(18) 0.0065(15) 0.0181(17) 0.0110(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 Ti1 O5 1.818(2) . ? Ti1 O1 1.8373(19) . ? Ti1 Cl1 2.2906(10) . ? Ti1 C1 2.334(3) . ? Ti1 C2 2.368(3) . ? Ti1 C5 2.383(3) . ? Ti1 C3 2.418(3) . ? Ti1 C4 2.457(3) . ? Ti2 O4 1.810(2) . ? Ti2 O2 1.8510(19) . ? Ti2 Cl2 2.2925(10) . ? Ti2 C24 2.313(3) . ? Ti2 C25 2.364(3) . ? Ti2 C28 2.379(3) . ? Ti2 C26 2.416(3) . ? Ti2 C27 2.428(3) . ? Si1 O1 1.644(2) . ? Si1 O3 1.660(2) . ? Si1 C22 1.847(3) . ? Si1 C24 1.881(3) . ? Si2 O2 1.642(2) . ? Si2 O3 1.660(2) . ? Si2 C21 1.852(3) . ? Si2 C1 1.884(3) . ? O4 C18 1.355(3) . ? O5 C13 1.362(3) . ? C1 C2 1.451(4) . ? C1 C5 1.459(4) . ? C2 C3 1.422(4) . ? C2 C9 1.505(4) . ? C3 C4 1.432(4) . ? C3 C8 1.514(4) . ? C4 C5 1.428(4) . ? C4 C7 1.511(4) . ? C5 C6 1.509(4) . ? C13 C14 1.393(4) . ? C13 C18 1.417(4) . ? C14 C15 1.391(4) . ? C15 C16 1.386(5) . ? C16 C17 1.387(4) . ? C17 C18 1.401(4) . ? C23 C25 1.511(4) . ? C24 C28 1.449(4) . ? C24 C25 1.450(4) . ? C25 C26 1.424(4) . ? C26 C27 1.436(4) . ? C26 C31 1.511(4) . ? C27 C28 1.429(4) . ? C27 C30 1.512(4) . ? C28 C29 1.505(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 O5 Ti1 O1 103.46(9) . . ? O5 Ti1 Cl1 102.28(7) . . ? O1 Ti1 Cl1 100.44(6) . . ? O5 Ti1 C1 116.54(9) . . ? O1 Ti1 C1 89.21(9) . . ? Cl1 Ti1 C1 136.58(7) . . ? O5 Ti1 C2 88.83(9) . . ? O1 Ti1 C2 119.12(9) . . ? Cl1 Ti1 C2 135.22(8) . . ? C1 Ti1 C2 35.95(9) . . ? O5 Ti1 C5 147.42(10) . . ? O1 Ti1 C5 94.73(9) . . ? Cl1 Ti1 C5 100.65(7) . . ? C1 Ti1 C5 36.03(9) . . ? C2 Ti1 C5 58.63(10) . . ? O5 Ti1 C3 95.37(10) . . ? O1 Ti1 C3 147.79(9) . . ? Cl1 Ti1 C3 100.76(7) . . ? C1 Ti1 C3 58.84(9) . . ? C2 Ti1 C3 34.56(10) . . ? C5 Ti1 C3 57.60(10) . . ? O5 Ti1 C4 127.80(10) . . ? O1 Ti1 C4 126.95(10) . . ? Cl1 Ti1 C4 82.92(7) . . ? C1 Ti1 C4 58.54(10) . . ? C2 Ti1 C4 57.37(10) . . ? C5 Ti1 C4 34.28(10) . . ? C3 Ti1 C4 34.14(10) . . ? O4 Ti2 O2 101.99(9) . . ? O4 Ti2 Cl2 101.46(7) . . ? O2 Ti2 Cl2 103.65(6) . . ? O4 Ti2 C24 109.82(10) . . ? O2 Ti2 C24 90.87(9) . . ? Cl2 Ti2 C24 141.87(8) . . ? O4 Ti2 C25 86.55(9) . . ? O2 Ti2 C25 123.41(9) . . ? Cl2 Ti2 C25 129.61(8) . . ? C24 Ti2 C25 36.11(10) . . ? O4 Ti2 C28 144.17(10) . . ? O2 Ti2 C28 91.11(9) . . ? Cl2 Ti2 C28 107.66(7) . . ? C24 Ti2 C28 35.93(10) . . ? C25 Ti2 C28 58.85(10) . . ? O4 Ti2 C26 99.48(10) . . ? O2 Ti2 C26 147.68(9) . . ? Cl2 Ti2 C26 95.36(8) . . ? C24 Ti2 C26 59.01(10) . . ? C25 Ti2 C26 34.64(10) . . ? C28 Ti2 C26 57.96(10) . . ? O4 Ti2 C27 133.70(10) . . ? O2 Ti2 C27 121.59(9) . . ? Cl2 Ti2 C27 83.91(7) . . ? C24 Ti2 C27 58.79(10) . . ? C25 Ti2 C27 57.79(10) . . ? C28 Ti2 C27 34.58(10) . . ? C26 Ti2 C27 34.49(10) . . ? O1 Si1 O3 106.38(10) . . ? O1 Si1 C22 111.41(13) . . ? O3 Si1 C22 110.44(12) . . ? O1 Si1 C24 108.04(11) . . ? O3 Si1 C24 106.84(11) . . ? C22 Si1 C24 113.39(13) . . ? O2 Si2 O3 107.43(10) . . ? O2 Si2 C21 112.11(12) . . ? O3 Si2 C21 108.72(12) . . ? O2 Si2 C1 108.85(11) . . ? O3 Si2 C1 106.91(11) . . ? C21 Si2 C1 112.56(14) . . ? Si1 O1 Ti1 149.03(12) . . ? Si2 O2 Ti2 143.59(12) . . ? Si2 O3 Si1 121.12(11) . . ? C18 O4 Ti2 163.73(19) . . ? C13 O5 Ti1 166.61(19) . . ? C2 C1 C5 106.1(2) . . ? C2 C1 Si2 129.8(2) . . ? C5 C1 Si2 124.1(2) . . ? C2 C1 Ti1 73.27(15) . . ? C5 C1 Ti1 73.79(16) . . ? Si2 C1 Ti1 117.02(13) . . ? C3 C2 C1 108.7(2) . . ? C3 C2 C9 123.7(3) . . ? C1 C2 C9 127.5(3) . . ? C3 C2 Ti1 74.66(16) . . ? C1 C2 Ti1 70.77(15) . . ? C9 C2 Ti1 123.66(19) . . ? C2 C3 C4 108.6(3) . . ? C2 C3 C8 125.8(3) . . ? C4 C3 C8 125.6(3) . . ? C2 C3 Ti1 70.79(16) . . ? C4 C3 Ti1 74.44(17) . . ? C8 C3 Ti1 121.4(2) . . ? C5 C4 C3 108.0(2) . . ? C5 C4 C7 126.9(3) . . ? C3 C4 C7 125.1(3) . . ? C5 C4 Ti1 69.99(16) . . ? C3 C4 Ti1 71.42(16) . . ? C7 C4 Ti1 127.2(2) . . ? C4 C5 C1 108.6(2) . . ? C4 C5 C6 125.4(3) . . ? C1 C5 C6 126.0(3) . . ? C4 C5 Ti1 75.72(17) . . ? C1 C5 Ti1 70.18(15) . . ? C6 C5 Ti1 121.2(2) . . ? O5 C13 C14 120.9(3) . . ? O5 C13 C18 119.8(2) . . ? C14 C13 C18 119.3(3) . . ? C15 C14 C13 120.4(3) . . ? C16 C15 C14 120.2(3) . . ? C15 C16 C17 120.4(3) . . ? C16 C17 C18 120.1(3) . . ? O4 C18 C17 120.4(3) . . ? O4 C18 C13 120.0(2) . . ? C17 C18 C13 119.6(3) . . ? C28 C24 C25 107.0(2) . . ? C28 C24 Si1 125.6(2) . . ? C25 C24 Si1 127.3(2) . . ? C28 C24 Ti2 74.52(15) . . ? C25 C24 Ti2 73.84(15) . . ? Si1 C24 Ti2 114.41(13) . . ? C26 C25 C24 108.4(3) . . ? C26 C25 C23 124.9(3) . . ? C24 C25 C23 126.7(3) . . ? C26 C25 Ti2 74.67(17) . . ? C24 C25 Ti2 70.05(15) . . ? C23 C25 Ti2 122.68(19) . . ? C25 C26 C27 108.2(3) . . ? C25 C26 C31 125.6(3) . . ? C27 C26 C31 126.2(3) . . ? C25 C26 Ti2 70.69(16) . . ? C27 C26 Ti2 73.23(16) . . ? C31 C26 Ti2 122.3(2) . . ? C28 C27 C26 108.4(3) . . ? C28 C27 C30 125.2(3) . . ? C26 C27 C30 126.4(3) . . ? C28 C27 Ti2 70.85(16) . . ? C26 C27 Ti2 72.28(16) . . ? C30 C27 Ti2 125.1(2) . . ? C27 C28 C24 108.1(2) . . ? C27 C28 C29 124.4(3) . . ? C24 C28 C29 127.5(3) . . ? C27 C28 Ti2 74.58(16) . . ? C24 C28 Ti2 69.55(15) . . ? C29 C28 Ti2 123.31(19) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.549 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.078 #====== END data_7 _database_code_depnum_ccdc_archive 'CCDC 708811' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H34 Cl F5 O5 Si2 Ti2' _chemical_formula_weight 781.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.597(4) _cell_length_b 17.888(3) _cell_length_c 16.826(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.61(2) _cell_angle_gamma 90.00 _cell_volume 3473.8(15) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 84 _cell_measurement_theta_max 19.513 _cell_measurement_theta_min 3.178 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.454 _exptl_crystal_size_mid 0.203 _exptl_crystal_size_min 0.102 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 0.671 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.702 _exptl_absorpt_correction_T_max 0.936 _exptl_special_details ; ? ; _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_ub_11 0.01 _diffrn_orient_matrix_ub_12 0 _diffrn_orient_matrix_ub_13 0 _diffrn_orient_matrix_ub_21 0 _diffrn_orient_matrix_ub_22 0.01 _diffrn_orient_matrix_ub_23 0 _diffrn_orient_matrix_ub_31 0 _diffrn_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_number 70795 _diffrn_reflns_av_R_equivalents 0.1090 _diffrn_reflns_av_sigmaI/netI 0.0887 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7957 _reflns_number_gt 4936 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0754P)^2^+2.3454P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0080(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7957 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1132 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1613 _refine_ls_wR_factor_gt 0.1427 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.50145(6) 0.27217(4) 0.54552(4) 0.02500(19) Uani 1 1 d . . . Ti2 Ti 0.21311(6) 0.37765(4) 0.65931(4) 0.02247(18) Uani 1 1 d . . . Cl1 Cl 0.65508(10) 0.28954(7) 0.47227(8) 0.0488(3) Uani 1 1 d . . . Si1 Si 0.23528(9) 0.30980(6) 0.46231(6) 0.0259(3) Uani 1 1 d . . . Si2 Si 0.23035(9) 0.20337(6) 0.59104(6) 0.0257(2) Uani 1 1 d . . . O1 O 0.3774(2) 0.30685(15) 0.47893(16) 0.0284(6) Uani 1 1 d . . . O4 O 0.3534(2) 0.40678(16) 0.70613(16) 0.0313(6) Uani 1 1 d . . . O2 O 0.2232(2) 0.27618(15) 0.65026(15) 0.0260(6) Uani 1 1 d . . . O3 O 0.1849(2) 0.23167(15) 0.49910(16) 0.0291(6) Uani 1 1 d . . . O5 O 0.5214(3) 0.34599(16) 0.61956(17) 0.0348(7) Uani 1 1 d . . . C1 C 0.5527(3) 0.3933(2) 0.6802(2) 0.0287(8) Uani 1 1 d . . . C2 C 0.4656(3) 0.4278(2) 0.7224(2) 0.0269(8) Uani 1 1 d . . . C3 C 0.6690(4) 0.4108(3) 0.7010(3) 0.0391(10) Uani 1 1 d . . . H3 H 0.7264 0.3871 0.6754 0.047 Uiso 1 1 calc R . . C4 C 0.6993(4) 0.4644(3) 0.7606(3) 0.0467(12) Uani 1 1 d . . . H4 H 0.7769 0.4758 0.7746 0.056 Uiso 1 1 calc R . . C5 C 0.6141(4) 0.5003(3) 0.7985(3) 0.0397(11) Uani 1 1 d . . . H5 H 0.6346 0.5368 0.8366 0.048 Uiso 1 1 calc R . . C6 C 0.4970(4) 0.4819(2) 0.7795(2) 0.0315(9) Uani 1 1 d . . . H6 H 0.4402 0.5060 0.8053 0.038 Uiso 1 1 calc R . . C10 C 0.1892(4) 0.3178(3) 0.3542(2) 0.0371(10) Uani 1 1 d . . . H10A H 0.1061 0.3193 0.3459 0.056 Uiso 1 1 calc R . . H10B H 0.2171 0.2754 0.3267 0.056 Uiso 1 1 calc R . . H10C H 0.2205 0.3628 0.3338 0.056 Uiso 1 1 calc R . . C11 C 0.1054(3) 0.3851(2) 0.7604(2) 0.0271(8) Uani 1 1 d . . . C12 C 0.1234(4) 0.4333(3) 0.8185(3) 0.0366(10) Uani 1 1 d . . . C13 C 0.0659(4) 0.4341(3) 0.8876(3) 0.0415(11) Uani 1 1 d . . . C14 C -0.0183(4) 0.3801(3) 0.8959(3) 0.0464(12) Uani 1 1 d . . . C15 C -0.0421(4) 0.3275(3) 0.8359(3) 0.0452(12) Uani 1 1 d . . . C16 C 0.0183(4) 0.3307(3) 0.7685(3) 0.0371(10) Uani 1 1 d . . . C20 C 0.3820(4) 0.1199(3) 0.4469(3) 0.0441(11) Uani 1 1 d . . . H20A H 0.3002 0.1286 0.4461 0.066 Uiso 1 1 calc R . . H20B H 0.3959 0.0674 0.4408 0.066 Uiso 1 1 calc R . . H20C H 0.4116 0.1468 0.4039 0.066 Uiso 1 1 calc R . . C21 C 0.3885(3) 0.1781(2) 0.5913(2) 0.0271(8) Uani 1 1 d . . . C22 C 0.4413(4) 0.1461(2) 0.5242(3) 0.0311(9) Uani 1 1 d . . . C23 C 0.5638(4) 0.1414(2) 0.5452(3) 0.0356(10) Uani 1 1 d . . . C24 C 0.5887(4) 0.1707(2) 0.6244(3) 0.0366(10) Uani 1 1 d . . . C25 C 0.4820(3) 0.1907(2) 0.6540(2) 0.0309(9) Uani 1 1 d . . . C26 C 0.4696(4) 0.2178(3) 0.7376(2) 0.0373(10) Uani 1 1 d . . . H26A H 0.3894 0.2276 0.7433 0.056 Uiso 1 1 calc R . . H26B H 0.5135 0.2629 0.7474 0.056 Uiso 1 1 calc R . . H26C H 0.4979 0.1802 0.7753 0.056 Uiso 1 1 calc R . . C28 C 0.7083(4) 0.1785(3) 0.6691(3) 0.0509(13) Uani 1 1 d . . . H28A H 0.7656 0.1611 0.6359 0.076 Uiso 1 1 calc R . . H28B H 0.7124 0.1493 0.7171 0.076 Uiso 1 1 calc R . . H28C H 0.7227 0.2301 0.6824 0.076 Uiso 1 1 calc R . . C29 C 0.6497(4) 0.1079(3) 0.4957(3) 0.0511(13) Uani 1 1 d . . . H29A H 0.7258 0.1118 0.5234 0.077 Uiso 1 1 calc R . . H29B H 0.6476 0.1341 0.4458 0.077 Uiso 1 1 calc R . . H29C H 0.6311 0.0562 0.4859 0.077 Uiso 1 1 calc R . . C31 C 0.1793(3) 0.3886(2) 0.5210(2) 0.0271(8) Uani 1 1 d . . . C32 C 0.2387(3) 0.4570(2) 0.5491(2) 0.0265(8) Uani 1 1 d . . . C33 C 0.1665(3) 0.4966(2) 0.5976(2) 0.0276(8) Uani 1 1 d . . . C34 C 0.0583(3) 0.4567(2) 0.5979(2) 0.0300(9) Uani 1 1 d . . . C35 C 0.0668(3) 0.3910(2) 0.5507(2) 0.0280(8) Uani 1 1 d . . . C36 C 0.3551(4) 0.4836(2) 0.5284(3) 0.0334(9) Uani 1 1 d . . . H36A H 0.3874 0.4473 0.4949 0.050 Uiso 1 1 calc R . . H36B H 0.4058 0.4899 0.5765 0.050 Uiso 1 1 calc R . . H36C H 0.3463 0.5304 0.5007 0.050 Uiso 1 1 calc R . . C37 C 0.1970(4) 0.5687(2) 0.6411(3) 0.0398(10) Uani 1 1 d . . . H37A H 0.1334 0.5840 0.6698 0.060 Uiso 1 1 calc R . . H37B H 0.2125 0.6067 0.6033 0.060 Uiso 1 1 calc R . . H37C H 0.2645 0.5613 0.6780 0.060 Uiso 1 1 calc R . . C38 C -0.0469(4) 0.4829(3) 0.6347(3) 0.0402(11) Uani 1 1 d . . . H38A H -0.0295 0.5286 0.6633 0.060 Uiso 1 1 calc R . . H38B H -0.0699 0.4455 0.6709 0.060 Uiso 1 1 calc R . . H38C H -0.1089 0.4913 0.5935 0.060 Uiso 1 1 calc R . . C39 C -0.0311(4) 0.3347(3) 0.5332(3) 0.0408(11) Uani 1 1 d . . . H39A H -0.0057 0.2952 0.5004 0.061 Uiso 1 1 calc R . . H39B H -0.0969 0.3592 0.5056 0.061 Uiso 1 1 calc R . . H39C H -0.0523 0.3142 0.5824 0.061 Uiso 1 1 calc R . . C40 C 0.1376(4) 0.1258(2) 0.6213(3) 0.0340(9) Uani 1 1 d . . . H40A H 0.1434 0.0841 0.5860 0.051 Uiso 1 1 calc R . . H40B H 0.0585 0.1422 0.6185 0.051 Uiso 1 1 calc R . . H40C H 0.1629 0.1109 0.6750 0.051 Uiso 1 1 calc R . . F2 F 0.2058(3) 0.48929(15) 0.81501(16) 0.0484(7) Uani 1 1 d . . . F3 F 0.0911(3) 0.48554(19) 0.94626(18) 0.0641(9) Uani 1 1 d . . . F4 F -0.0732(3) 0.3777(2) 0.9630(2) 0.0750(11) Uani 1 1 d . . . F5 F -0.1231(3) 0.2751(2) 0.84421(19) 0.0686(10) Uani 1 1 d . . . F6 F -0.0100(3) 0.27777(19) 0.71311(17) 0.0573(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0217(3) 0.0230(4) 0.0305(4) -0.0001(3) 0.0037(3) -0.0015(3) Ti2 0.0190(3) 0.0246(4) 0.0239(3) 0.0040(3) 0.0025(2) 0.0000(3) Cl1 0.0349(6) 0.0468(7) 0.0688(8) 0.0080(6) 0.0259(5) -0.0007(5) Si1 0.0246(5) 0.0290(6) 0.0239(5) 0.0019(4) 0.0010(4) -0.0007(4) Si2 0.0229(5) 0.0242(5) 0.0301(6) 0.0031(4) 0.0030(4) -0.0028(4) O1 0.0268(14) 0.0281(15) 0.0300(14) 0.0030(11) 0.0007(11) -0.0010(11) O4 0.0211(13) 0.0374(16) 0.0349(15) 0.0023(13) 0.0010(11) -0.0026(12) O2 0.0253(13) 0.0256(14) 0.0270(13) 0.0039(11) 0.0019(10) -0.0002(11) O3 0.0300(14) 0.0273(14) 0.0294(14) 0.0004(11) -0.0004(11) -0.0033(12) O5 0.0382(17) 0.0306(16) 0.0350(16) -0.0045(13) 0.0008(12) -0.0054(13) C1 0.029(2) 0.025(2) 0.031(2) -0.0002(16) 0.0005(16) -0.0055(16) C2 0.0237(19) 0.026(2) 0.031(2) 0.0041(16) 0.0016(15) -0.0053(16) C3 0.028(2) 0.035(2) 0.055(3) -0.011(2) 0.0083(19) -0.0033(19) C4 0.026(2) 0.057(3) 0.056(3) -0.015(2) 0.000(2) -0.012(2) C5 0.038(2) 0.039(3) 0.041(2) -0.014(2) 0.0020(19) -0.016(2) C6 0.028(2) 0.030(2) 0.036(2) -0.0010(18) 0.0053(16) -0.0003(17) C10 0.042(2) 0.040(2) 0.029(2) 0.0000(18) -0.0018(18) 0.002(2) C11 0.0217(18) 0.028(2) 0.033(2) 0.0136(17) 0.0098(15) 0.0118(16) C12 0.026(2) 0.042(3) 0.042(2) 0.016(2) 0.0044(18) -0.0013(19) C13 0.038(2) 0.050(3) 0.037(2) -0.005(2) 0.0076(19) 0.005(2) C14 0.038(3) 0.069(3) 0.034(2) 0.003(2) 0.0139(19) 0.009(2) C15 0.030(2) 0.059(3) 0.047(3) 0.011(2) 0.009(2) -0.001(2) C16 0.033(2) 0.045(3) 0.033(2) 0.0001(19) 0.0025(18) -0.003(2) C20 0.048(3) 0.036(3) 0.049(3) -0.015(2) 0.007(2) -0.002(2) C21 0.030(2) 0.0174(18) 0.034(2) 0.0038(16) 0.0062(16) -0.0028(16) C22 0.033(2) 0.0188(19) 0.043(2) 0.0019(17) 0.0100(18) -0.0014(16) C23 0.029(2) 0.025(2) 0.053(3) 0.0022(19) 0.0065(19) 0.0031(17) C24 0.028(2) 0.030(2) 0.051(3) 0.010(2) -0.0009(18) 0.0029(18) C25 0.028(2) 0.028(2) 0.036(2) 0.0080(17) 0.0008(16) -0.0006(17) C26 0.035(2) 0.042(3) 0.034(2) 0.0076(19) 0.0001(18) -0.0019(19) C28 0.032(2) 0.051(3) 0.069(3) 0.011(3) -0.001(2) 0.007(2) C29 0.039(3) 0.039(3) 0.078(4) -0.007(3) 0.021(2) 0.005(2) C31 0.0270(19) 0.030(2) 0.0236(18) 0.0098(16) -0.0006(15) 0.0005(16) C32 0.0265(19) 0.028(2) 0.0255(19) 0.0075(16) 0.0028(15) -0.0022(16) C33 0.031(2) 0.0231(19) 0.0285(19) 0.0079(16) 0.0034(16) 0.0047(16) C34 0.029(2) 0.032(2) 0.030(2) 0.0141(17) 0.0051(16) 0.0087(17) C35 0.0234(19) 0.033(2) 0.0272(19) 0.0068(16) -0.0007(15) 0.0022(16) C36 0.027(2) 0.036(2) 0.038(2) 0.0072(19) 0.0071(17) -0.0028(18) C37 0.050(3) 0.030(2) 0.041(2) 0.0029(19) 0.010(2) 0.001(2) C38 0.032(2) 0.049(3) 0.041(2) 0.013(2) 0.0109(18) 0.013(2) C39 0.027(2) 0.052(3) 0.042(2) 0.002(2) -0.0043(18) -0.007(2) C40 0.027(2) 0.031(2) 0.044(2) 0.0034(19) 0.0031(17) -0.0057(18) F2 0.0574(17) 0.0398(15) 0.0498(16) -0.0059(12) 0.0145(13) -0.0113(13) F3 0.071(2) 0.073(2) 0.0512(17) -0.0243(16) 0.0226(15) -0.0072(17) F4 0.062(2) 0.113(3) 0.0562(19) -0.0075(19) 0.0351(16) -0.013(2) F5 0.0514(18) 0.095(3) 0.0618(19) 0.0022(18) 0.0192(15) -0.0320(18) F6 0.0512(17) 0.070(2) 0.0518(17) -0.0088(15) 0.0102(13) -0.0222(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O5 1.815(3) . ? Ti1 O1 1.843(3) . ? Ti1 Cl1 2.2846(14) . ? Ti1 C21 2.311(4) . ? Ti1 C25 2.364(4) . ? Ti1 C22 2.378(4) . ? Ti1 C24 2.412(4) . ? Ti1 C23 2.449(4) . ? Ti2 O4 1.813(3) . ? Ti2 O2 1.826(3) . ? Ti2 C11 2.210(4) . ? Ti2 C31 2.329(4) . ? Ti2 C32 2.378(4) . ? Ti2 C35 2.381(4) . ? Ti2 C33 2.406(4) . ? Ti2 C34 2.435(4) . ? Si1 O1 1.645(3) . ? Si1 O3 1.658(3) . ? Si1 C10 1.851(4) . ? Si1 C31 1.874(4) . ? Si2 O2 1.647(3) . ? Si2 O3 1.664(3) . ? Si2 C40 1.858(4) . ? Si2 C21 1.889(4) . ? O4 C2 1.357(5) . ? O5 C1 1.347(5) . ? C1 C3 1.395(6) . ? C1 C2 1.430(6) . ? C2 C6 1.386(6) . ? C3 C4 1.407(6) . ? C4 C5 1.385(7) . ? C5 C6 1.404(6) . ? C11 C12 1.305(6) . ? C11 C16 1.419(6) . ? C12 F2 1.389(5) . ? C12 C13 1.397(6) . ? C13 F3 1.360(5) . ? C13 C14 1.390(7) . ? C14 F4 1.350(5) . ? C14 C15 1.387(7) . ? C15 F5 1.344(6) . ? C15 C16 1.390(6) . ? C16 F6 1.346(5) . ? C20 C22 1.486(6) . ? C21 C22 1.453(6) . ? C21 C25 1.455(6) . ? C22 C23 1.433(6) . ? C23 C24 1.435(7) . ? C23 C29 1.485(6) . ? C24 C25 1.425(6) . ? C24 C28 1.518(6) . ? C25 C26 1.508(6) . ? C31 C35 1.442(6) . ? C31 C32 1.460(6) . ? C32 C33 1.415(6) . ? C32 C36 1.503(6) . ? C33 C34 1.445(6) . ? C33 C37 1.507(6) . ? C34 C35 1.428(6) . ? C34 C38 1.496(6) . ? C35 C39 1.524(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Ti1 O1 102.25(13) . . ? O5 Ti1 Cl1 102.57(11) . . ? O1 Ti1 Cl1 103.30(10) . . ? O5 Ti1 C21 109.85(14) . . ? O1 Ti1 C21 90.77(13) . . ? Cl1 Ti1 C21 140.92(11) . . ? O5 Ti1 C25 86.20(14) . . ? O1 Ti1 C25 123.31(13) . . ? Cl1 Ti1 C25 129.71(11) . . ? C21 Ti1 C25 36.24(14) . . ? O5 Ti1 C22 144.06(14) . . ? O1 Ti1 C22 91.57(14) . . ? Cl1 Ti1 C22 106.28(11) . . ? C21 Ti1 C22 36.08(14) . . ? C25 Ti1 C22 58.86(15) . . ? O5 Ti1 C24 98.69(15) . . ? O1 Ti1 C24 148.07(14) . . ? Cl1 Ti1 C24 95.26(12) . . ? C21 Ti1 C24 59.30(14) . . ? C25 Ti1 C24 34.69(15) . . ? C22 Ti1 C24 58.02(15) . . ? O5 Ti1 C23 132.75(15) . . ? O1 Ti1 C23 122.24(14) . . ? Cl1 Ti1 C23 83.25(11) . . ? C21 Ti1 C23 58.81(14) . . ? C25 Ti1 C23 57.55(15) . . ? C22 Ti1 C23 34.50(14) . . ? C24 Ti1 C23 34.34(16) . . ? O4 Ti2 O2 105.04(12) . . ? O4 Ti2 C11 101.47(14) . . ? O2 Ti2 C11 99.77(13) . . ? O4 Ti2 C31 117.78(14) . . ? O2 Ti2 C31 90.35(13) . . ? C11 Ti2 C31 135.31(14) . . ? O4 Ti2 C32 89.55(13) . . ? O2 Ti2 C32 120.97(13) . . ? C11 Ti2 C32 133.44(14) . . ? C31 Ti2 C32 36.13(14) . . ? O4 Ti2 C35 147.83(14) . . ? O2 Ti2 C35 94.71(13) . . ? C11 Ti2 C35 99.84(14) . . ? C31 Ti2 C35 35.64(14) . . ? C32 Ti2 C35 58.36(13) . . ? O4 Ti2 C33 95.01(13) . . ? O2 Ti2 C33 148.95(13) . . ? C11 Ti2 C33 99.16(14) . . ? C31 Ti2 C33 59.07(14) . . ? C32 Ti2 C33 34.41(14) . . ? C35 Ti2 C33 57.81(14) . . ? O4 Ti2 C34 127.62(14) . . ? O2 Ti2 C34 126.34(13) . . ? C11 Ti2 C34 80.98(13) . . ? C31 Ti2 C34 58.81(14) . . ? C32 Ti2 C34 57.66(13) . . ? C35 Ti2 C34 34.47(14) . . ? C33 Ti2 C34 34.72(14) . . ? O1 Si1 O3 107.05(14) . . ? O1 Si1 C10 110.96(19) . . ? O3 Si1 C10 110.72(18) . . ? O1 Si1 C31 109.11(16) . . ? O3 Si1 C31 106.51(16) . . ? C10 Si1 C31 112.26(19) . . ? O2 Si2 O3 106.97(14) . . ? O2 Si2 C40 111.16(18) . . ? O3 Si2 C40 110.03(17) . . ? O2 Si2 C21 107.11(16) . . ? O3 Si2 C21 107.13(17) . . ? C40 Si2 C21 114.11(18) . . ? Si1 O1 Ti1 145.47(17) . . ? C2 O4 Ti2 165.8(3) . . ? Si2 O2 Ti2 147.56(16) . . ? Si1 O3 Si2 120.83(16) . . ? C1 O5 Ti1 169.6(3) . . ? O5 C1 C3 120.9(4) . . ? O5 C1 C2 119.7(3) . . ? C3 C1 C2 119.4(4) . . ? O4 C2 C6 121.0(4) . . ? O4 C2 C1 119.4(3) . . ? C6 C2 C1 119.7(4) . . ? C1 C3 C4 120.0(4) . . ? C5 C4 C3 120.3(4) . . ? C4 C5 C6 120.3(4) . . ? C2 C6 C5 120.3(4) . . ? C12 C11 C16 116.4(4) . . ? C12 C11 Ti2 123.7(3) . . ? C16 C11 Ti2 119.6(3) . . ? C11 C12 F2 120.4(4) . . ? C11 C12 C13 125.2(4) . . ? F2 C12 C13 114.5(4) . . ? F3 C13 C14 120.1(4) . . ? F3 C13 C12 121.7(4) . . ? C14 C13 C12 118.3(4) . . ? F4 C14 C15 120.7(5) . . ? F4 C14 C13 119.9(5) . . ? C15 C14 C13 119.3(4) . . ? F5 C15 C14 119.2(4) . . ? F5 C15 C16 121.7(5) . . ? C14 C15 C16 119.0(4) . . ? F6 C16 C15 115.4(4) . . ? F6 C16 C11 122.8(4) . . ? C15 C16 C11 121.8(4) . . ? C22 C21 C25 106.5(4) . . ? C22 C21 Si2 125.1(3) . . ? C25 C21 Si2 128.3(3) . . ? C22 C21 Ti1 74.5(2) . . ? C25 C21 Ti1 73.9(2) . . ? Si2 C21 Ti1 114.00(18) . . ? C23 C22 C21 108.3(4) . . ? C23 C22 C20 124.1(4) . . ? C21 C22 C20 127.6(4) . . ? C23 C22 Ti1 75.4(2) . . ? C21 C22 Ti1 69.4(2) . . ? C20 C22 Ti1 122.3(3) . . ? C22 C23 C24 108.2(4) . . ? C22 C23 C29 126.1(4) . . ? C24 C23 C29 125.6(4) . . ? C22 C23 Ti1 70.1(2) . . ? C24 C23 Ti1 71.4(2) . . ? C29 C23 Ti1 126.9(3) . . ? C25 C24 C23 108.3(4) . . ? C25 C24 C28 126.0(4) . . ? C23 C24 C28 125.8(4) . . ? C25 C24 Ti1 70.8(2) . . ? C23 C24 Ti1 74.2(2) . . ? C28 C24 Ti1 121.1(3) . . ? C24 C25 C21 108.6(4) . . ? C24 C25 C26 124.9(4) . . ? C21 C25 C26 126.5(4) . . ? C24 C25 Ti1 74.5(2) . . ? C21 C25 Ti1 69.9(2) . . ? C26 C25 Ti1 123.2(3) . . ? C35 C31 C32 106.1(3) . . ? C35 C31 Si1 125.2(3) . . ? C32 C31 Si1 128.6(3) . . ? C35 C31 Ti2 74.1(2) . . ? C32 C31 Ti2 73.7(2) . . ? Si1 C31 Ti2 115.50(18) . . ? C33 C32 C31 108.6(3) . . ? C33 C32 C36 124.8(4) . . ? C31 C32 C36 126.6(4) . . ? C33 C32 Ti2 73.9(2) . . ? C31 C32 Ti2 70.1(2) . . ? C36 C32 Ti2 123.5(3) . . ? C32 C33 C34 108.5(4) . . ? C32 C33 C37 125.8(4) . . ? C34 C33 C37 125.7(4) . . ? C32 C33 Ti2 71.7(2) . . ? C34 C33 Ti2 73.7(2) . . ? C37 C33 Ti2 121.0(3) . . ? C35 C34 C33 107.3(3) . . ? C35 C34 C38 126.2(4) . . ? C33 C34 C38 126.2(4) . . ? C35 C34 Ti2 70.7(2) . . ? C33 C34 Ti2 71.5(2) . . ? C38 C34 Ti2 127.1(3) . . ? C34 C35 C31 109.3(3) . . ? C34 C35 C39 124.1(4) . . ? C31 C35 C39 126.5(4) . . ? C34 C35 Ti2 74.9(2) . . ? C31 C35 Ti2 70.2(2) . . ? C39 C35 Ti2 123.0(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.495 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.100 #====== END