Electronic Supplementary Material for Chemical Communications This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author_name 'Juergen Heck' _publ_contact_author_address ;Universitaet Hamburg Fachbereich Chemie Martin-Luther-King-Platz 6 20146 Hamburg Germany ; _publ_contact_author_email juergen.heck@chemie.uni-hamburg.de _publ_contact_author_phone '+4940 42838 6375' _publ_contact_author_fax '+4940 42838 6945' _publ_section_title ; Sugar Ligands in Organotitanium Complexes ; loop_ _publ_author_name _publ_author_address J.Heck ;Universitaet Hamburg Fachbereich Chemie Martin-Luther-King-Platz 6 20146 Hamburg Germany ; D.Kuentzer ;Universitaet Hamburg Fachbereich Chemie Martin-Luther-King-Platz 6 20146 Hamburg Germany ; L.Jessen ;Universitaet Hamburg Fachbereich Chemie Martin-Luther-King-Platz 6 20146 Hamburg Germany ; _publ_section_abstract ; Using ligands dervied from D-glucose, dinuclear organotitanium compounds with interesting structural features were synthesized. ; data_dk1 _database_code_depnum_ccdc_archive 'CCDC 274863' _vrf_RINTA01_dk1 ; PROBLEM: The value of Rint is greater than 0.20 RESPONSE: The crystal is small and weakly diffracting. ; _vrf_THETM01_dk1 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: The crystal is small and weakly diffracting. ; _vrf_PLAT020_dk1 ; PROBLEM: The value of Rint is greater than 0.10 ......... 0.35 RESPONSE: The crystal is small and weakly diffracting. ; _vrf_PLAT023_dk1 ; PROBLEM: Resolution (too) Low [sin(th)/Lambda < 0.6]..... 20.00 Deg. RESPONSE: The crystal is small and weakly diffracting. ; _vrf_PLAT027_dk1 ; PROBLEM: _diffrn_reflns_theta_full (too) Low ............ 20.00 Deg. RESPONSE: The crystal is small and weakly diffracting. ; _vrf_PLAT201_dk1 ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 60 RESPONSE: The crystal is small and weakly diffracting. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[chloro(pentamethylcyclopentadienyl)-(methyl-4,6-O-beta- naphthyl-2-methyliden-beta-D-glucopyranosidato)titan] ; _chemical_name_common ; Bis(chloro(pentamethylcyclopentadienyl)-(methyl-4,6-O-beta- naphthyl-2-methyliden-beta-D-glucopyranosidato)titan) ; _chemical_melting_point ? _chemical_formula_moiety 'C48 H62 Cl2 O12 Ti2, C7 H8' _chemical_formula_sum 'C55 H70 Cl2 O12 Ti2' _chemical_formula_weight 1089.81 _chemical_absolute_configuration known loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_int_tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.203(7) _cell_length_b 21.613(17) _cell_length_c 30.49(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5406(8) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 100 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2296 _exptl_absorpt_coefficient_mu 0.454 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9146 _exptl_absorpt_correction_T_max 0.9560 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 1998)' _exptl_special_details ; Crystals were grown from a solution in dichloromethane. ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS, 1998' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 32757 _diffrn_reflns_av_R_equivalents 0.3488 _diffrn_reflns_av_sigmaI/netI 0.3230 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 20.00 _reflns_number_total 5036 _reflns_number_gt 1670 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 1998)' _computing_cell_refinement 'SAINT (Bruker AXS, 1998)' _computing_data_reduction 'SAINT (Bruker AXS, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker AXS, 1998)' _computing_publication_material 'SHELXTL (Bruker AXS, 1998)' _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^)+(0.0080P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00026(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.09(7) _refine_ls_number_reflns 5036 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1719 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1159 _refine_ls_wR_factor_gt 0.0930 _refine_ls_goodness_of_fit_ref 0.666 _refine_ls_restrained_S_all 0.666 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 1.0678(3) 0.51569(12) 0.02317(9) 0.0549(9) Uani 1 1 d . . . Ti2 Ti 1.0677(3) 0.51257(12) 0.18746(9) 0.0574(9) Uani 1 1 d . . . Cl1 Cl 0.8200(4) 0.52430(17) -0.01055(12) 0.0651(13) Uani 1 1 d . . . Cl2 Cl 0.8212(4) 0.49860(17) 0.22198(12) 0.0661(13) Uani 1 1 d . . . O21 O 0.9627(12) 0.6880(4) 0.0216(3) 0.063(3) Uiso 1 1 d . . . O22 O 1.0452(12) 0.5733(4) 0.0640(3) 0.062(3) Uiso 1 1 d . . . O23 O 1.0511(12) 0.5885(4) 0.1592(3) 0.054(3) Uiso 1 1 d . . . O25 O 0.8287(12) 0.7197(4) 0.0816(3) 0.060(3) Uiso 1 1 d . . . O26 O 0.6115(10) 0.7426(4) 0.1845(3) 0.066(3) Uiso 1 1 d . . . O24 O 0.7855(10) 0.6570(4) 0.1926(3) 0.052(3) Uiso 1 1 d . . . O42 O 1.0452(11) 0.4554(4) 0.1454(3) 0.059(3) Uiso 1 1 d . . . O43 O 1.0603(11) 0.4410(4) 0.0532(3) 0.055(3) Uiso 1 1 d . . . O41 O 0.9674(11) 0.3429(4) 0.1883(3) 0.059(3) Uiso 1 1 d . . . O45 O 0.8247(11) 0.3099(4) 0.1300(3) 0.051(3) Uiso 1 1 d . . . O44 O 0.8105(10) 0.3642(3) 0.0160(3) 0.049(3) Uiso 1 1 d . . . O46 O 0.6448(10) 0.2780(4) 0.0225(3) 0.058(3) Uiso 1 1 d . . . C1 C 1.3425(17) 0.4917(6) 0.0108(4) 0.055(4) Uiso 1 1 d . . . C2 C 1.2586(16) 0.4573(6) -0.0190(5) 0.056(5) Uiso 1 1 d . . . C3 C 1.1740(16) 0.4930(6) -0.0490(4) 0.042(4) Uiso 1 1 d . . . C4 C 1.2110(18) 0.5528(7) -0.0368(5) 0.057(5) Uiso 1 1 d . . . C5 C 1.3161(19) 0.5559(7) -0.0019(5) 0.060(5) Uiso 1 1 d . . . C6 C 1.2189(16) 0.4679(6) 0.2459(4) 0.047(4) Uiso 1 1 d . . . C7 C 1.1807(18) 0.5288(7) 0.2605(5) 0.055(4) Uiso 1 1 d . . . C8 C 1.2501(17) 0.5715(7) 0.2318(5) 0.056(5) Uiso 1 1 d . . . C9 C 1.3450(17) 0.5375(6) 0.1988(4) 0.049(4) Uiso 1 1 d . . . C10 C 1.3219(17) 0.4738(6) 0.2090(4) 0.055(4) Uiso 1 1 d . . . C21 C 0.8786(18) 0.6666(6) 0.0582(5) 0.067(5) Uiso 1 1 d . . . H21A H 0.7837 0.6400 0.0497 0.081 Uiso 1 1 calc R . . C22 C 1.0048(18) 0.6302(6) 0.0873(4) 0.061(5) Uiso 1 1 d . . . H22A H 1.1051 0.6557 0.0919 0.074 Uiso 1 1 calc R . . C23 C 0.9333(17) 0.6123(6) 0.1298(4) 0.045(4) Uiso 1 1 d . . . H23A H 0.8424 0.5821 0.1255 0.054 Uiso 1 1 calc R . . C24 C 0.8704(16) 0.6721(6) 0.1516(4) 0.047(5) Uiso 1 1 d . . . H24A H 0.9627 0.7013 0.1573 0.057 Uiso 1 1 calc R . . C25 C 0.7420(17) 0.7028(6) 0.1219(4) 0.059(5) Uiso 1 1 d . . . H25A H 0.6510 0.6734 0.1154 0.071 Uiso 1 1 calc R . . C26 C 0.6782(17) 0.7604(6) 0.1433(5) 0.070(5) Uiso 1 1 d . . . H26A H 0.7675 0.7907 0.1476 0.085 Uiso 1 1 calc R . . H26B H 0.5931 0.7797 0.1248 0.085 Uiso 1 1 calc R . . C27 C 0.7295(18) 0.7126(7) 0.2122(5) 0.065(5) Uiso 1 1 d . . . H27A H 0.8237 0.7410 0.2176 0.077 Uiso 1 1 calc R . . C28 C 0.6491(16) 0.6980(6) 0.2538(5) 0.049(4) Uiso 1 1 d . . . C29 C 0.6480(18) 0.6375(6) 0.2717(5) 0.071(5) Uiso 1 1 d . . . H29A H 0.7016 0.6048 0.2567 0.086 Uiso 1 1 calc R . . C30 C 0.5705(17) 0.6261(6) 0.3101(5) 0.057(4) Uiso 1 1 d . . . H30A H 0.5652 0.5847 0.3205 0.068 Uiso 1 1 calc R . . C31 C 0.4984(17) 0.6730(7) 0.3351(5) 0.072(5) Uiso 1 1 d . . . H31A H 0.4515 0.6646 0.3630 0.086 Uiso 1 1 calc R . . C32 C 0.4981(15) 0.7333(6) 0.3172(5) 0.055(5) Uiso 1 1 d . . . H32A H 0.4445 0.7659 0.3323 0.065 Uiso 1 1 calc R . . C33 C 0.5746(16) 0.7448(6) 0.2783(4) 0.051(4) Uiso 1 1 d . . . H33A H 0.5773 0.7861 0.2675 0.062 Uiso 1 1 calc R . . C34 C 0.8514(17) 0.7054(6) -0.0115(5) 0.084(6) Uiso 1 1 d . . . H34A H 0.9116 0.7206 -0.0371 0.127 Uiso 1 1 calc R . . H34B H 0.7797 0.7381 -0.0005 0.127 Uiso 1 1 calc R . . H34C H 0.7857 0.6694 -0.0200 0.127 Uiso 1 1 calc R . . C41 C 0.8803(16) 0.3638(6) 0.1508(4) 0.042(4) Uiso 1 1 d . . . H41A H 0.7874 0.3912 0.1593 0.050 Uiso 1 1 calc R . . C42 C 1.0072(17) 0.3990(6) 0.1241(4) 0.053(5) Uiso 1 1 d . . . H42A H 1.1079 0.3734 0.1206 0.064 Uiso 1 1 calc R . . C43 C 0.9359(19) 0.4144(6) 0.0798(4) 0.053(4) Uiso 1 1 d . . . H43A H 0.8425 0.4438 0.0830 0.063 Uiso 1 1 calc R . . C44 C 0.8787(15) 0.3541(5) 0.0580(4) 0.044(4) Uiso 1 1 d . . . H44A H 0.9742 0.3256 0.0550 0.053 Uiso 1 1 calc R . . C45 C 0.7538(16) 0.3243(6) 0.0883(4) 0.034(4) Uiso 1 1 d . . . H45A H 0.6589 0.3528 0.0924 0.041 Uiso 1 1 calc R . . C46 C 0.6980(17) 0.2654(5) 0.0669(4) 0.053(4) Uiso 1 1 d . . . H46A H 0.7886 0.2352 0.0664 0.063 Uiso 1 1 calc R . . H46B H 0.6070 0.2473 0.0839 0.063 Uiso 1 1 calc R . . C47 C 0.7781(17) 0.3044(6) -0.0029(4) 0.055(5) Uiso 1 1 d . . . H47A H 0.8767 0.2771 -0.0033 0.066 Uiso 1 1 calc R . . C48 C 0.7095(19) 0.3160(7) -0.0484(5) 0.061(5) Uiso 1 1 d . . . C49 C 0.7171(15) 0.2666(6) -0.0765(4) 0.056(5) Uiso 1 1 d . . . H49A H 0.7653 0.2288 -0.0673 0.067 Uiso 1 1 calc R . . C50 C 0.6519(16) 0.2727(7) -0.1196(5) 0.072(5) Uiso 1 1 d . . . H50A H 0.6484 0.2384 -0.1391 0.086 Uiso 1 1 calc R . . C51 C 0.5937(17) 0.3302(7) -0.1321(5) 0.071(5) Uiso 1 1 d . . . H51D H 0.5532 0.3356 -0.1610 0.086 Uiso 1 1 calc R . . C52 C 0.5930(17) 0.3787(6) -0.1042(6) 0.068(5) Uiso 1 1 d . . . H52A H 0.5509 0.4175 -0.1135 0.082 Uiso 1 1 calc R . . C53 C 0.6533(16) 0.3720(7) -0.0623(5) 0.066(5) Uiso 1 1 d . . . H53A H 0.6557 0.4065 -0.0430 0.079 Uiso 1 1 calc R . . C54 C 0.8633(17) 0.3171(6) 0.2218(4) 0.081(6) Uiso 1 1 d . . . H54E H 0.9301 0.3032 0.2465 0.122 Uiso 1 1 calc R . . H54F H 0.8030 0.2819 0.2097 0.122 Uiso 1 1 calc R . . H54G H 0.7863 0.3488 0.2318 0.122 Uiso 1 1 calc R . . C61 C 1.4477(16) 0.4721(5) 0.0475(4) 0.064(5) Uiso 1 1 d . . . H61N H 1.5578 0.4637 0.0365 0.096 Uiso 1 1 calc R . . H61O H 1.4028 0.4345 0.0608 0.096 Uiso 1 1 calc R . . H61P H 1.4523 0.5051 0.0695 0.096 Uiso 1 1 calc R . . C62 C 1.2530(16) 0.3833(5) -0.0200(4) 0.070(5) Uiso 1 1 d . . . H62K H 1.3402 0.3678 -0.0390 0.105 Uiso 1 1 calc R . . H62L H 1.1472 0.3697 -0.0314 0.105 Uiso 1 1 calc R . . H62M H 1.2680 0.3673 0.0097 0.105 Uiso 1 1 calc R . . C63 C 1.0823(17) 0.4743(6) -0.0875(4) 0.089(6) Uiso 1 1 d . . . H63A H 1.1570 0.4690 -0.1123 0.134 Uiso 1 1 calc R . . H63B H 1.0016 0.5062 -0.0946 0.134 Uiso 1 1 calc R . . H63C H 1.0265 0.4351 -0.0815 0.134 Uiso 1 1 calc R . . C64 C 1.1550(17) 0.6102(6) -0.0632(4) 0.079(5) Uiso 1 1 d . . . H64E H 1.2315 0.6178 -0.0873 0.119 Uiso 1 1 calc R . . H64F H 1.1521 0.6464 -0.0439 0.119 Uiso 1 1 calc R . . H64G H 1.0458 0.6028 -0.0752 0.119 Uiso 1 1 calc R . . C65 C 1.3940(16) 0.6132(5) 0.0209(4) 0.071(5) Uiso 1 1 d . . . H65B H 1.4961 0.6240 0.0060 0.107 Uiso 1 1 calc R . . H65C H 1.4166 0.6034 0.0517 0.107 Uiso 1 1 calc R . . H65D H 1.3185 0.6483 0.0193 0.107 Uiso 1 1 calc R . . C66 C 1.1649(17) 0.4104(6) 0.2686(4) 0.073(5) Uiso 1 1 d . . . H66A H 1.2434 0.3998 0.2916 0.109 Uiso 1 1 calc R . . H66B H 1.1585 0.3765 0.2474 0.109 Uiso 1 1 calc R . . H66C H 1.0574 0.4172 0.2817 0.109 Uiso 1 1 calc R . . C67 C 1.0835(17) 0.5468(6) 0.2991(5) 0.091(6) Uiso 1 1 d . . . H67A H 1.1557 0.5518 0.3245 0.136 Uiso 1 1 calc R . . H67B H 1.0027 0.5146 0.3053 0.136 Uiso 1 1 calc R . . H67C H 1.0277 0.5860 0.2931 0.136 Uiso 1 1 calc R . . C68 C 1.2321(16) 0.6436(6) 0.2341(4) 0.071(5) Uiso 1 1 d . . . H68H H 1.3160 0.6606 0.2535 0.106 Uiso 1 1 calc R . . H68I H 1.1240 0.6542 0.2455 0.106 Uiso 1 1 calc R . . H68J H 1.2449 0.6611 0.2047 0.106 Uiso 1 1 calc R . . C69 C 1.4390(18) 0.5637(6) 0.1610(4) 0.081(5) Uiso 1 1 d . . . H69A H 1.5510 0.5725 0.1703 0.121 Uiso 1 1 calc R . . H69B H 1.3870 0.6021 0.1511 0.121 Uiso 1 1 calc R . . H69C H 1.4406 0.5337 0.1369 0.121 Uiso 1 1 calc R . . C70 C 1.4039(10) 0.4203(4) 0.1819(3) 0.077(5) Uiso 1 1 d . . . H70A H 1.5094 0.4098 0.1950 0.116 Uiso 1 1 calc R . . H70B H 1.4203 0.4339 0.1516 0.116 Uiso 1 1 calc R . . H70C H 1.3331 0.3838 0.1823 0.116 Uiso 1 1 calc R . . C81 C 0.7943(10) 0.6032(4) -0.1605(3) 0.077(6) Uiso 1 1 d R . . C82 C 0.7011(10) 0.5660(4) -0.1331(3) 0.078(6) Uiso 1 1 d R . . H82B H 0.7139 0.5223 -0.1348 0.094 Uiso 1 1 calc R . . C83 C 0.590(2) 0.5901(7) -0.1034(6) 0.109(7) Uiso 1 1 d . . . H83C H 0.5207 0.5649 -0.0860 0.131 Uiso 1 1 calc R . . C84 C 0.589(2) 0.6551(8) -0.1013(6) 0.125(7) Uiso 1 1 d . . . H84D H 0.5267 0.6753 -0.0793 0.150 Uiso 1 1 calc R . . C85 C 0.678(2) 0.6903(9) -0.1310(6) 0.128(8) Uiso 1 1 d . . . H85E H 0.6614 0.7339 -0.1307 0.153 Uiso 1 1 calc R . . C86 C 0.787(2) 0.6672(7) -0.1605(5) 0.084(6) Uiso 1 1 d . . . H86F H 0.8508 0.6924 -0.1792 0.100 Uiso 1 1 calc R . . C87 C 0.917(2) 0.5721(7) -0.1914(6) 0.139(8) Uiso 1 1 d . . . H87G H 0.9080 0.5271 -0.1888 0.208 Uiso 1 1 calc R . . H87H H 1.0281 0.5849 -0.1833 0.208 Uiso 1 1 calc R . . H87I H 0.8948 0.5846 -0.2217 0.208 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 0.053(2) 0.0482(19) 0.063(2) 0.0001(17) 0.0023(17) -0.0018(18) Ti2 0.0487(19) 0.057(2) 0.066(2) -0.0053(18) -0.0028(18) -0.0006(18) Cl1 0.054(3) 0.061(3) 0.080(3) 0.007(2) -0.006(3) -0.002(3) Cl2 0.050(3) 0.062(3) 0.086(3) -0.005(3) 0.008(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O22 1.770(9) . ? Ti1 O43 1.857(8) . ? Ti1 Cl1 2.286(5) . ? Ti1 C4 2.317(14) . ? Ti1 C5 2.342(15) . ? Ti1 C1 2.343(14) . ? Ti1 C2 2.387(13) . ? Ti1 C3 2.416(12) . ? Ti1 Ti2 5.010(5) . ? Ti2 O42 1.789(9) . ? Ti2 O23 1.860(8) . ? Ti2 Cl2 2.299(4) . ? Ti2 C10 2.341(14) . ? Ti2 C9 2.363(14) . ? Ti2 C6 2.375(13) . ? Ti2 C8 2.386(14) . ? Ti2 C7 2.437(14) . ? O21 C21 1.391(14) . ? O21 C34 1.412(13) . ? O22 C22 1.459(14) . ? O23 C23 1.415(14) . ? O25 C21 1.412(14) . ? O25 C25 1.466(13) . ? O26 C26 1.424(13) . ? O26 C27 1.439(14) . ? O24 C27 1.418(14) . ? O24 C24 1.470(13) . ? O42 C42 1.415(13) . ? O43 C43 1.425(14) . ? O41 C41 1.420(13) . ? O41 C54 1.443(13) . ? O45 C41 1.401(13) . ? O45 C45 1.432(12) . ? O44 C44 1.414(13) . ? O44 C47 1.440(12) . ? O46 C46 1.448(12) . ? O46 C47 1.455(13) . ? C1 C2 1.361(16) . ? C1 C5 1.456(15) . ? C1 C61 1.476(15) . ? C2 C3 1.382(15) . ? C2 C62 1.600(15) . ? C3 C4 1.378(15) . ? C3 C63 1.453(15) . ? C4 C5 1.371(16) . ? C4 C64 1.549(15) . ? C5 C65 1.558(15) . ? C6 C10 1.412(16) . ? C6 C7 1.424(15) . ? C6 C66 1.490(15) . ? C7 C8 1.392(16) . ? C7 C67 1.474(16) . ? C8 C9 1.470(16) . ? C8 C68 1.566(15) . ? C9 C10 1.424(16) . ? C9 C69 1.497(15) . ? C10 C70 1.573(14) . ? C21 C22 1.574(16) . ? C21 H21A 1.0000 . ? C22 C23 1.474(15) . ? C22 H22A 1.0000 . ? C23 C24 1.543(15) . ? C23 H23A 1.0000 . ? C24 C25 1.539(16) . ? C24 H24A 1.0000 . ? C25 C26 1.500(16) . ? C25 H25A 1.0000 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.463(16) . ? C27 H27A 1.0000 . ? C28 C33 1.400(15) . ? C28 C29 1.416(16) . ? C29 C30 1.357(17) . ? C29 H29A 0.9500 . ? C30 C31 1.398(16) . ? C30 H30A 0.9500 . ? C31 C32 1.413(15) . ? C31 H31A 0.9500 . ? C32 C33 1.365(15) . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C41 C42 1.526(15) . ? C41 H41A 1.0000 . ? C42 C43 1.511(15) . ? C42 H42A 1.0000 . ? C43 C44 1.536(15) . ? C43 H43A 1.0000 . ? C44 C45 1.523(15) . ? C44 H44A 1.0000 . ? C45 C46 1.503(14) . ? C45 H45A 1.0000 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.518(16) . ? C47 H47A 1.0000 . ? C48 C53 1.363(16) . ? C48 C49 1.370(16) . ? C49 C50 1.426(15) . ? C49 H49A 0.9500 . ? C50 C51 1.384(15) . ? C50 H50A 0.9500 . ? C51 C52 1.351(16) . ? C51 H51D 0.9500 . ? C52 C53 1.378(17) . ? C52 H52A 0.9500 . ? C53 H53A 0.9500 . ? C54 H54E 0.9800 . ? C54 H54F 0.9800 . ? C54 H54G 0.9800 . ? C61 H61N 0.9800 . ? C61 H61O 0.9800 . ? C61 H61P 0.9800 . ? C62 H62K 0.9800 . ? C62 H62L 0.9800 . ? C62 H62M 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64E 0.9800 . ? C64 H64F 0.9800 . ? C64 H64G 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C65 H65D 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68H 0.9800 . ? C68 H68I 0.9800 . ? C68 H68J 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C81 C86 1.383(16) . ? C81 C82 1.3900 . ? C81 C87 1.535(16) . ? C82 C83 1.386(18) . ? C82 H82B 0.9500 . ? C83 C84 1.408(17) . ? C83 H83C 0.9500 . ? C84 C85 1.39(2) . ? C84 H84D 0.9500 . ? C85 C86 1.362(19) . ? C85 H85E 0.9500 . ? C86 H86F 0.9500 . ? C87 H87G 0.9800 . ? C87 H87H 0.9800 . ? C87 H87I 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O22 Ti1 O43 105.2(4) . . ? O22 Ti1 Cl1 99.5(3) . . ? O43 Ti1 Cl1 105.2(3) . . ? O22 Ti1 C4 111.4(5) . . ? O43 Ti1 C4 135.0(5) . . ? Cl1 Ti1 C4 93.9(4) . . ? O22 Ti1 C5 93.4(5) . . ? O43 Ti1 C5 120.8(5) . . ? Cl1 Ti1 C5 126.6(4) . . ? C4 Ti1 C5 34.2(4) . . ? O22 Ti1 C1 111.7(5) . . ? O43 Ti1 C1 85.4(5) . . ? Cl1 Ti1 C1 143.2(4) . . ? C4 Ti1 C1 57.4(5) . . ? C5 Ti1 C1 36.2(4) . . ? O22 Ti1 C2 145.1(5) . . ? O43 Ti1 C2 80.1(4) . . ? Cl1 Ti1 C2 112.6(4) . . ? C4 Ti1 C2 54.9(5) . . ? C5 Ti1 C2 56.6(5) . . ? C1 Ti1 C2 33.4(4) . . ? O22 Ti1 C3 145.1(5) . . ? O43 Ti1 C3 106.5(4) . . ? Cl1 Ti1 C3 85.9(3) . . ? C4 Ti1 C3 33.8(4) . . ? C5 Ti1 C3 57.6(5) . . ? C1 Ti1 C3 57.4(5) . . ? C2 Ti1 C3 33.4(4) . . ? O22 Ti1 Ti2 46.1(3) . . ? O43 Ti1 Ti2 59.7(3) . . ? Cl1 Ti1 Ti2 116.79(13) . . ? C4 Ti1 Ti2 142.6(4) . . ? C5 Ti1 Ti2 109.4(4) . . ? C1 Ti1 Ti2 99.1(3) . . ? C2 Ti1 Ti2 122.2(4) . . ? C3 Ti1 Ti2 155.2(3) . . ? O42 Ti2 O23 105.7(4) . . ? O42 Ti2 Cl2 98.4(3) . . ? O23 Ti2 Cl2 105.3(3) . . ? O42 Ti2 C10 92.6(5) . . ? O23 Ti2 C10 120.7(5) . . ? Cl2 Ti2 C10 127.4(4) . . ? O42 Ti2 C9 111.2(5) . . ? O23 Ti2 C9 86.4(4) . . ? Cl2 Ti2 C9 144.0(4) . . ? C10 Ti2 C9 35.2(4) . . ? O42 Ti2 C6 108.1(4) . . ? O23 Ti2 C6 138.1(5) . . ? Cl2 Ti2 C6 93.6(4) . . ? C10 Ti2 C6 34.8(4) . . ? C9 Ti2 C6 58.7(5) . . ? O42 Ti2 C8 147.1(5) . . ? O23 Ti2 C8 80.6(5) . . ? Cl2 Ti2 C8 111.2(4) . . ? C10 Ti2 C8 58.2(5) . . ? C9 Ti2 C8 36.1(4) . . ? C6 Ti2 C8 57.6(5) . . ? O42 Ti2 C7 142.4(5) . . ? O23 Ti2 C7 108.9(4) . . ? Cl2 Ti2 C7 86.3(4) . . ? C10 Ti2 C7 57.1(5) . . ? C9 Ti2 C7 57.8(5) . . ? C6 Ti2 C7 34.4(4) . . ? C8 Ti2 C7 33.5(4) . . ? O42 Ti2 Ti1 45.0(3) . . ? O23 Ti2 Ti1 61.6(3) . . ? Cl2 Ti2 Ti1 117.37(13) . . ? C10 Ti2 Ti1 106.6(3) . . ? C9 Ti2 Ti1 98.2(3) . . ? C6 Ti2 Ti1 139.0(3) . . ? C8 Ti2 Ti1 124.0(4) . . ? C7 Ti2 Ti1 155.7(4) . . ? C21 O21 C34 110.0(11) . . ? C22 O22 Ti1 163.6(9) . . ? C23 O23 Ti2 131.7(8) . . ? C21 O25 C25 111.3(10) . . ? C26 O26 C27 112.4(11) . . ? C27 O24 C24 108.9(9) . . ? C42 O42 Ti2 161.0(9) . . ? C43 O43 Ti1 130.9(8) . . ? C41 O41 C54 113.2(10) . . ? C41 O45 C45 110.7(9) . . ? C44 O44 C47 107.1(9) . . ? C46 O46 C47 110.1(10) . . ? C2 C1 C5 105.5(14) . . ? C2 C1 C61 130.2(14) . . ? C5 C1 C61 124.2(13) . . ? C2 C1 Ti1 75.1(9) . . ? C5 C1 Ti1 71.9(9) . . ? C61 C1 Ti1 120.2(10) . . ? C1 C2 C3 112.9(14) . . ? C1 C2 C62 125.0(14) . . ? C3 C2 C62 122.1(13) . . ? C1 C2 Ti1 71.5(8) . . ? C3 C2 Ti1 74.4(8) . . ? C62 C2 Ti1 121.3(8) . . ? C4 C3 C2 103.7(13) . . ? C4 C3 C63 126.3(13) . . ? C2 C3 C63 129.6(14) . . ? C4 C3 Ti1 69.2(8) . . ? C2 C3 Ti1 72.2(8) . . ? C63 C3 Ti1 127.3(10) . . ? C5 C4 C3 113.1(14) . . ? C5 C4 C64 123.5(14) . . ? C3 C4 C64 123.1(13) . . ? C5 C4 Ti1 73.9(9) . . ? C3 C4 Ti1 77.0(8) . . ? C64 C4 Ti1 122.5(10) . . ? C4 C5 C1 104.7(13) . . ? C4 C5 C65 130.0(14) . . ? C1 C5 C65 125.3(14) . . ? C4 C5 Ti1 71.9(9) . . ? C1 C5 Ti1 71.9(8) . . ? C65 C5 Ti1 120.4(9) . . ? C10 C6 C7 107.2(13) . . ? C10 C6 C66 128.6(13) . . ? C7 C6 C66 124.1(13) . . ? C10 C6 Ti2 71.3(8) . . ? C7 C6 Ti2 75.2(8) . . ? C66 C6 Ti2 122.2(9) . . ? C8 C7 C6 109.1(13) . . ? C8 C7 C67 123.1(14) . . ? C6 C7 C67 127.7(14) . . ? C8 C7 Ti2 71.2(8) . . ? C6 C7 Ti2 70.4(8) . . ? C67 C7 Ti2 124.2(11) . . ? C7 C8 C9 108.3(13) . . ? C7 C8 C68 126.4(14) . . ? C9 C8 C68 125.3(13) . . ? C7 C8 Ti2 75.2(9) . . ? C9 C8 Ti2 71.1(8) . . ? C68 C8 Ti2 119.8(9) . . ? C10 C9 C8 105.2(13) . . ? C10 C9 C69 127.0(13) . . ? C8 C9 C69 127.7(13) . . ? C10 C9 Ti2 71.5(9) . . ? C8 C9 Ti2 72.8(8) . . ? C69 C9 Ti2 118.0(10) . . ? C6 C10 C9 109.9(13) . . ? C6 C10 C70 127.4(12) . . ? C9 C10 C70 122.7(12) . . ? C6 C10 Ti2 73.9(8) . . ? C9 C10 Ti2 73.2(9) . . ? C70 C10 Ti2 119.8(8) . . ? O21 C21 O25 106.1(11) . . ? O21 C21 C22 107.0(12) . . ? O25 C21 C22 108.1(13) . . ? O21 C21 H21A 111.8 . . ? O25 C21 H21A 111.8 . . ? C22 C21 H21A 111.8 . . ? O22 C22 C23 107.3(11) . . ? O22 C22 C21 107.2(12) . . ? C23 C22 C21 111.4(12) . . ? O22 C22 H22A 110.3 . . ? C23 C22 H22A 110.3 . . ? C21 C22 H22A 110.3 . . ? O23 C23 C22 112.4(12) . . ? O23 C23 C24 105.0(10) . . ? C22 C23 C24 107.0(11) . . ? O23 C23 H23A 110.7 . . ? C22 C23 H23A 110.7 . . ? C24 C23 H23A 110.7 . . ? O24 C24 C25 105.8(10) . . ? O24 C24 C23 109.9(10) . . ? C25 C24 C23 109.7(11) . . ? O24 C24 H24A 110.5 . . ? C25 C24 H24A 110.5 . . ? C23 C24 H24A 110.5 . . ? O25 C25 C26 109.1(11) . . ? O25 C25 C24 105.5(11) . . ? C26 C25 C24 109.9(11) . . ? O25 C25 H25A 110.7 . . ? C26 C25 H25A 110.7 . . ? C24 C25 H25A 110.7 . . ? O26 C26 C25 107.1(11) . . ? O26 C26 H26A 110.3 . . ? C25 C26 H26A 110.3 . . ? O26 C26 H26B 110.3 . . ? C25 C26 H26B 110.3 . . ? H26A C26 H26B 108.6 . . ? O24 C27 O26 110.7(11) . . ? O24 C27 C28 109.1(12) . . ? O26 C27 C28 107.6(12) . . ? O24 C27 H27A 109.8 . . ? O26 C27 H27A 109.8 . . ? C28 C27 H27A 109.8 . . ? C33 C28 C29 117.3(14) . . ? C33 C28 C27 120.2(13) . . ? C29 C28 C27 122.4(14) . . ? C30 C29 C28 120.3(14) . . ? C30 C29 H29A 119.9 . . ? C28 C29 H29A 119.9 . . ? C29 C30 C31 122.5(14) . . ? C29 C30 H30A 118.8 . . ? C31 C30 H30A 118.8 . . ? C30 C31 C32 117.3(15) . . ? C30 C31 H31A 121.3 . . ? C32 C31 H31A 121.3 . . ? C33 C32 C31 120.2(14) . . ? C33 C32 H32A 119.9 . . ? C31 C32 H32A 119.9 . . ? C32 C33 C28 122.2(13) . . ? C32 C33 H33A 118.9 . . ? C28 C33 H33A 118.9 . . ? O21 C34 H34A 109.5 . . ? O21 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O21 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O45 C41 O41 105.3(10) . . ? O45 C41 C42 113.3(11) . . ? O41 C41 C42 104.1(10) . . ? O45 C41 H41A 111.2 . . ? O41 C41 H41A 111.2 . . ? C42 C41 H41A 111.2 . . ? O42 C42 C43 107.9(11) . . ? O42 C42 C41 109.6(11) . . ? C43 C42 C41 108.8(12) . . ? O42 C42 H42A 110.1 . . ? C43 C42 H42A 110.1 . . ? C41 C42 H42A 110.1 . . ? O43 C43 C42 108.7(12) . . ? O43 C43 C44 108.3(11) . . ? C42 C43 C44 108.6(11) . . ? O43 C43 H43A 110.4 . . ? C42 C43 H43A 110.4 . . ? C44 C43 H43A 110.4 . . ? O44 C44 C45 110.4(10) . . ? O44 C44 C43 112.4(10) . . ? C45 C44 C43 107.5(11) . . ? O44 C44 H44A 108.8 . . ? C45 C44 H44A 108.8 . . ? C43 C44 H44A 108.8 . . ? O45 C45 C46 109.1(10) . . ? O45 C45 C44 111.0(11) . . ? C46 C45 C44 107.3(10) . . ? O45 C45 H45A 109.8 . . ? C46 C45 H45A 109.8 . . ? C44 C45 H45A 109.8 . . ? O46 C46 C45 109.8(10) . . ? O46 C46 H46A 109.7 . . ? C45 C46 H46A 109.7 . . ? O46 C46 H46B 109.7 . . ? C45 C46 H46B 109.7 . . ? H46A C46 H46B 108.2 . . ? O44 C47 O46 106.1(10) . . ? O44 C47 C48 106.5(11) . . ? O46 C47 C48 105.7(11) . . ? O44 C47 H47A 112.6 . . ? O46 C47 H47A 112.6 . . ? C48 C47 H47A 112.6 . . ? C53 C48 C49 120.8(15) . . ? C53 C48 C47 123.8(14) . . ? C49 C48 C47 115.2(14) . . ? C48 C49 C50 119.3(14) . . ? C48 C49 H49A 120.4 . . ? C50 C49 H49A 120.4 . . ? C51 C50 C49 117.7(14) . . ? C51 C50 H50A 121.2 . . ? C49 C50 H50A 121.2 . . ? C52 C51 C50 121.8(16) . . ? C52 C51 H51D 119.1 . . ? C50 C51 H51D 119.1 . . ? C51 C52 C53 120.0(15) . . ? C51 C52 H52A 120.0 . . ? C53 C52 H52A 120.0 . . ? C48 C53 C52 120.3(15) . . ? C48 C53 H53A 119.9 . . ? C52 C53 H53A 119.9 . . ? O41 C54 H54E 109.5 . . ? O41 C54 H54F 109.5 . . ? H54E C54 H54F 109.5 . . ? O41 C54 H54G 109.5 . . ? H54E C54 H54G 109.5 . . ? H54F C54 H54G 109.5 . . ? C1 C61 H61N 109.5 . . ? C1 C61 H61O 109.5 . . ? H61N C61 H61O 109.5 . . ? C1 C61 H61P 109.5 . . ? H61N C61 H61P 109.5 . . ? H61O C61 H61P 109.5 . . ? C2 C62 H62K 109.5 . . ? C2 C62 H62L 109.5 . . ? H62K C62 H62L 109.5 . . ? C2 C62 H62M 109.5 . . ? H62K C62 H62M 109.5 . . ? H62L C62 H62M 109.5 . . ? C3 C63 H63A 109.5 . . ? C3 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C3 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C4 C64 H64E 109.5 . . ? C4 C64 H64F 109.5 . . ? H64E C64 H64F 109.5 . . ? C4 C64 H64G 109.5 . . ? H64E C64 H64G 109.5 . . ? H64F C64 H64G 109.5 . . ? C5 C65 H65B 109.5 . . ? C5 C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C5 C65 H65D 109.5 . . ? H65B C65 H65D 109.5 . . ? H65C C65 H65D 109.5 . . ? C6 C66 H66A 109.5 . . ? C6 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C6 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C7 C67 H67A 109.5 . . ? C7 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C7 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C8 C68 H68H 109.5 . . ? C8 C68 H68I 109.5 . . ? H68H C68 H68I 109.5 . . ? C8 C68 H68J 109.5 . . ? H68H C68 H68J 109.5 . . ? H68I C68 H68J 109.5 . . ? C9 C69 H69A 109.5 . . ? C9 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C9 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C10 C70 H70A 109.5 . . ? C10 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C10 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C86 C81 C82 123.6(8) . . ? C86 C81 C87 117.9(12) . . ? C82 C81 C87 118.5(7) . . ? C83 C82 C81 122.4(8) . . ? C83 C82 H82B 118.8 . . ? C81 C82 H82B 118.8 . . ? C82 C83 C84 114.1(16) . . ? C82 C83 H83C 123.0 . . ? C84 C83 H83C 123.0 . . ? C85 C84 C83 121(2) . . ? C85 C84 H84D 119.5 . . ? C83 C84 H84D 119.5 . . ? C86 C85 C84 125(2) . . ? C86 C85 H85E 117.6 . . ? C84 C85 H85E 117.6 . . ? C85 C86 C81 113.4(15) . . ? C85 C86 H86F 123.3 . . ? C81 C86 H86F 123.3 . . ? C81 C87 H87G 109.5 . . ? C81 C87 H87H 109.5 . . ? H87G C87 H87H 109.5 . . ? C81 C87 H87I 109.5 . . ? H87G C87 H87I 109.5 . . ? H87H C87 H87I 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.227 _refine_diff_density_min -0.302 _refine_diff_density_rms 0.052 data_dk33a _database_code_depnum_ccdc_archive 'CCDC 275215' _vrf_PLAT220_dk33a ; PROBLEM: Large Non-Solvent C18 Ueq(max)/Ueq(min) ... 5.82 Ratio RESPONSE: This is because of disorder of C18. ; _vrf_PLAT222_dk33a ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 7.20 Ratio RESPONSE: This is because of disorder of the methyl group. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[chloro(pentamethylcyclopentadienyl)-(methyl-4,6-O- beta-naphthyl-2-methyliden-beta-D-glucopyranosidato)titan] ; _chemical_name_common ; Bis(chloro(pentamethylcyclopentadienyl)-(methyl-4,6-O-beta- naphthyl-2-methyliden-beta-D-glucopyranosidato)titan) ; _chemical_melting_point ? _chemical_formula_moiety 'C56 H66 Cl2 O12 Ti2, 2(C H2 Cl2)' _chemical_formula_sum 'C58 H70 Cl6 O12 Ti2' _chemical_formula_weight 1267.64 _chemical_absolute_configuration 'known, Flack' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 14.8415(9) _cell_length_b 25.3203(16) _cell_length_c 8.0438(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3022.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 100 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 27.5 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.588 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6505 _exptl_absorpt_correction_T_max 0.9328 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 1998)' _exptl_special_details ; Crystals were grown from a solution in toluene which was overlayered with hexane. ; _diffrn_ambient_temperature 153(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 AXS, 1998' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 36490 _diffrn_reflns_av_R_equivalents 0.0846 _diffrn_reflns_av_sigmaI/netI 0.0501 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6875 _reflns_number_gt 6275 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 1998)' _computing_cell_refinement 'SAINT (Bruker AXS, 1998)' _computing_data_reduction 'SAINT (Bruker AXS, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker AXS, 1998)' _computing_publication_material 'SHELXTL (Bruker AXS, 1998)' _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^)+(0.0940P)^2^+2.2680P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(4) _refine_ls_number_reflns 6875 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.1651 _refine_ls_wR_factor_gt 0.1598 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 0.62136(4) 0.56849(2) 0.24539(7) 0.02027(14) Uani 1 1 d . . . Cl1 Cl 0.68718(7) 0.58664(4) 0.49832(11) 0.0334(2) Uani 1 1 d . . . O1 O 0.1927(2) 0.54101(15) 0.2902(5) 0.0627(12) Uani 1 1 d . . . O2 O 0.37029(16) 0.50156(9) 0.2515(3) 0.0287(5) Uani 1 1 d . . . O3 O 0.50278(16) 0.58369(10) 0.2735(3) 0.0275(5) Uani 1 1 d . . . O4 O 0.46943(15) 0.66012(9) 0.5187(3) 0.0230(5) Uani 1 1 d . . . O5 O 0.24390(17) 0.60831(11) 0.4490(4) 0.0332(6) Uani 1 1 d . . . O6 O 0.36766(17) 0.70821(10) 0.6800(3) 0.0299(6) Uani 1 1 d . . . C1 C 0.2632(3) 0.55610(15) 0.3936(6) 0.0362(9) Uani 1 1 d . . . H1 H 0.2679 0.5315 0.4905 0.043 Uiso 1 1 calc R . . C2 C 0.3495(2) 0.55414(13) 0.2892(4) 0.0239(7) Uani 1 1 d . . . H2 H 0.3387 0.5736 0.1829 0.029 Uiso 1 1 calc R . . C3 C 0.4289(2) 0.57956(12) 0.3787(4) 0.0206(6) Uani 1 1 d . . . H3 H 0.4453 0.5580 0.4784 0.025 Uiso 1 1 calc R . . C4 C 0.3986(2) 0.63366(13) 0.4328(4) 0.0209(6) Uani 1 1 d . . . H4 H 0.3821 0.6547 0.3320 0.025 Uiso 1 1 calc R . . C5 C 0.3162(2) 0.62920(14) 0.5450(4) 0.0255(7) Uani 1 1 d . . . H5 H 0.3294 0.6058 0.6422 0.031 Uiso 1 1 calc R . . C6 C 0.2903(2) 0.68477(15) 0.6040(5) 0.0320(8) Uani 1 1 d . . . H6A H 0.2703 0.7064 0.5084 0.038 Uiso 1 1 calc R . . H6B H 0.2403 0.6827 0.6851 0.038 Uiso 1 1 calc R . . C7 C 0.4411(2) 0.71105(13) 0.5649(4) 0.0240(7) Uani 1 1 d . . . H7 H 0.4225 0.7314 0.4641 0.029 Uiso 1 1 calc R . . C8 C 0.5169(2) 0.73914(14) 0.6518(4) 0.0275(7) Uani 1 1 d . . . C9 C 0.5025(3) 0.79064(16) 0.7136(6) 0.0407(10) Uani 1 1 d . . . H9 H 0.4456 0.8070 0.6975 0.049 Uiso 1 1 calc R . . C10 C 0.5671(3) 0.81694(18) 0.7943(6) 0.0438(11) Uani 1 1 d . . . H10 H 0.5553 0.8515 0.8346 0.053 Uiso 1 1 calc R . . C11 C 0.6535(3) 0.79382(18) 0.8209(5) 0.0385(9) Uani 1 1 d . . . C12 C 0.7229(3) 0.8196(2) 0.9119(6) 0.0504(13) Uani 1 1 d . . . H12 H 0.7133 0.8543 0.9532 0.061 Uiso 1 1 calc R . . C13 C 0.8019(3) 0.7954(2) 0.9398(6) 0.0542(14) Uani 1 1 d . . . H13 H 0.8470 0.8130 1.0027 0.065 Uiso 1 1 calc R . . C14 C 0.8190(3) 0.7442(2) 0.8773(6) 0.0517(13) Uani 1 1 d . . . H14 H 0.8754 0.7277 0.8976 0.062 Uiso 1 1 calc R . . C15 C 0.7536(3) 0.7183(2) 0.7868(5) 0.0417(10) Uani 1 1 d . . . H15 H 0.7654 0.6842 0.7427 0.050 Uiso 1 1 calc R . . C16 C 0.6692(2) 0.74236(15) 0.7594(5) 0.0317(8) Uani 1 1 d . . . C17 C 0.5989(2) 0.71592(15) 0.6716(4) 0.0284(8) Uani 1 1 d . . . H17 H 0.6094 0.6818 0.6267 0.034 Uiso 1 1 calc R . . C18 C 0.1118(4) 0.5307(3) 0.3784(13) 0.120(4) Uani 1 1 d . . . H18A H 0.0689 0.5128 0.3049 0.180 Uiso 1 1 calc R . . H18B H 0.0857 0.5641 0.4169 0.180 Uiso 1 1 calc R . . H18C H 0.1249 0.5081 0.4742 0.180 Uiso 1 1 calc R . . C19 C 0.6173(3) 0.64378(14) 0.0687(5) 0.0283(7) Uani 1 1 d . . . C20 C 0.7025(2) 0.64434(14) 0.1475(5) 0.0268(7) Uani 1 1 d . . . C21 C 0.7501(2) 0.59910(14) 0.0964(5) 0.0271(7) Uani 1 1 d . . . C22 C 0.6943(2) 0.56968(15) -0.0130(4) 0.0271(7) Uani 1 1 d . . . C23 C 0.6103(3) 0.59788(14) -0.0285(4) 0.0279(7) Uani 1 1 d . . . C24 C 0.5458(3) 0.68553(17) 0.0904(6) 0.0428(10) Uani 1 1 d . . . H24A H 0.5431 0.6962 0.2074 0.064 Uiso 1 1 calc R . . H24B H 0.4873 0.6713 0.0563 0.064 Uiso 1 1 calc R . . H24C H 0.5606 0.7163 0.0216 0.064 Uiso 1 1 calc R . . C25 C 0.7366(3) 0.68700(16) 0.2593(6) 0.0427(10) Uani 1 1 d . . . H25A H 0.6855 0.7069 0.3046 0.064 Uiso 1 1 calc R . . H25B H 0.7756 0.7109 0.1959 0.064 Uiso 1 1 calc R . . H25C H 0.7710 0.6712 0.3506 0.064 Uiso 1 1 calc R . . C26 C 0.8455(3) 0.5857(2) 0.1429(6) 0.0425(10) Uani 1 1 d . . . H26A H 0.8549 0.5475 0.1320 0.064 Uiso 1 1 calc R . . H26B H 0.8568 0.5964 0.2582 0.064 Uiso 1 1 calc R . . H26C H 0.8872 0.6044 0.0690 0.064 Uiso 1 1 calc R . . C27 C 0.7191(3) 0.51906(16) -0.0981(5) 0.0400(10) Uani 1 1 d . . . H27A H 0.6649 0.4976 -0.1140 0.060 Uiso 1 1 calc R . . H27B H 0.7624 0.4996 -0.0294 0.060 Uiso 1 1 calc R . . H27C H 0.7462 0.5269 -0.2063 0.060 Uiso 1 1 calc R . . C28 C 0.5308(3) 0.58097(18) -0.1298(5) 0.0381(9) Uani 1 1 d . . . H28A H 0.5301 0.5424 -0.1386 0.057 Uiso 1 1 calc R . . H28B H 0.5351 0.5964 -0.2412 0.057 Uiso 1 1 calc R . . H28C H 0.4753 0.5930 -0.0760 0.057 Uiso 1 1 calc R . . C29 C 0.0453(5) 0.6359(3) 0.7087(15) 0.110(3) Uani 1 1 d . . . H29A H 0.0825 0.6438 0.6097 0.132 Uiso 1 1 calc R . . H29B H 0.0445 0.6675 0.7810 0.132 Uiso 1 1 calc R . . Cl3 Cl 0.09214(19) 0.58112(11) 0.8190(4) 0.1254(10) Uani 1 1 d . . . Cl4 Cl -0.06738(13) 0.61944(10) 0.6462(3) 0.1037(7) 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 0.0212(3) 0.0232(3) 0.0165(3) 0.0022(2) 0.0019(2) -0.0020(2) Cl1 0.0401(5) 0.0416(5) 0.0184(4) 0.0016(4) -0.0046(4) -0.0048(4) O1 0.0227(14) 0.076(2) 0.089(3) -0.054(2) 0.0074(16) -0.0133(14) O2 0.0313(12) 0.0246(10) 0.0301(12) -0.0045(11) 0.0047(13) -0.0010(9) O3 0.0239(11) 0.0326(12) 0.0261(13) -0.0068(10) 0.0037(10) -0.0040(9) O4 0.0228(11) 0.0249(11) 0.0212(12) -0.0028(9) -0.0004(9) -0.0001(9) O5 0.0203(12) 0.0357(14) 0.0434(17) -0.0155(12) 0.0023(11) -0.0015(10) O6 0.0273(13) 0.0329(13) 0.0296(13) -0.0085(10) 0.0028(11) -0.0015(11) C1 0.0261(18) 0.034(2) 0.048(2) -0.0174(17) 0.0110(17) -0.0075(15) C2 0.0228(15) 0.0256(15) 0.0234(17) -0.0042(12) 0.0015(12) 0.0002(12) C3 0.0206(14) 0.0242(16) 0.0170(15) 0.0013(12) 0.0004(12) 0.0012(12) C4 0.0226(15) 0.0228(15) 0.0174(15) 0.0006(12) -0.0010(12) -0.0021(12) C5 0.0235(16) 0.0277(17) 0.0254(18) -0.0060(13) 0.0045(13) -0.0018(14) C6 0.0262(17) 0.0326(18) 0.037(2) -0.0129(16) 0.0039(16) 0.0003(15) C7 0.0256(16) 0.0248(15) 0.0215(16) -0.0002(13) 0.0005(13) -0.0027(13) C8 0.0316(18) 0.0290(17) 0.0218(17) -0.0011(13) 0.0009(14) -0.0050(14) C9 0.037(2) 0.0334(19) 0.051(3) -0.0101(18) -0.0014(19) -0.0004(17) C10 0.043(2) 0.039(2) 0.049(3) -0.0172(18) 0.0010(19) -0.0036(18) C11 0.040(2) 0.049(2) 0.0261(19) -0.0072(17) 0.0050(16) -0.0162(18) C12 0.054(3) 0.067(3) 0.030(2) -0.009(2) 0.007(2) -0.036(2) C13 0.046(3) 0.092(4) 0.024(2) -0.001(2) 0.0023(19) -0.030(3) C14 0.036(2) 0.088(4) 0.031(2) 0.018(2) -0.0027(19) -0.022(2) C15 0.038(2) 0.063(3) 0.023(2) 0.0066(17) -0.0020(16) -0.012(2) C16 0.0328(18) 0.0431(19) 0.0192(16) 0.0008(16) 0.0048(16) -0.0097(14) C17 0.0338(19) 0.0320(18) 0.0193(17) 0.0004(13) 0.0039(14) -0.0045(15) C18 0.038(3) 0.134(6) 0.188(9) -0.118(7) 0.043(4) -0.038(4) C19 0.0328(18) 0.0258(16) 0.0264(17) 0.0081(13) 0.0043(15) -0.0025(15) C20 0.0299(18) 0.0267(16) 0.0237(17) 0.0023(13) 0.0030(14) -0.0074(14) C21 0.0255(17) 0.0318(18) 0.0239(18) 0.0072(13) 0.0059(14) -0.0057(14) C22 0.0304(17) 0.0305(16) 0.0204(16) 0.0026(15) 0.0075(14) -0.0014(15) C23 0.0301(18) 0.0353(18) 0.0182(17) 0.0079(13) -0.0009(14) -0.0043(15) C24 0.044(2) 0.039(2) 0.045(3) 0.0128(19) 0.013(2) 0.0122(19) C25 0.059(3) 0.0349(19) 0.034(2) -0.0010(19) 0.003(2) -0.0211(18) C26 0.0264(18) 0.060(3) 0.041(2) 0.006(2) 0.0026(17) -0.0074(18) C27 0.059(3) 0.039(2) 0.022(2) -0.0030(15) 0.0084(18) -0.0002(19) C28 0.037(2) 0.052(2) 0.0245(19) 0.0031(17) -0.0056(16) -0.0108(18) C29 0.071(4) 0.097(5) 0.162(10) -0.046(6) 0.003(5) 0.006(4) Cl3 0.135(2) 0.1297(19) 0.1121(18) -0.0313(15) -0.0515(16) 0.0423(16) Cl4 0.0637(10) 0.1399(19) 0.1076(17) 0.0106(14) 0.0074(11) 0.0207(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O2 1.779(2) 2_665 ? Ti1 O3 1.816(2) . ? Ti1 Cl1 2.3032(11) . ? Ti1 C23 2.331(3) . ? Ti1 C22 2.343(3) . ? Ti1 C19 2.379(3) . ? Ti1 C21 2.385(3) . ? Ti1 C20 2.400(3) . ? O1 C1 1.390(5) . ? O1 C18 1.419(7) . ? O2 C2 1.400(4) . ? O2 Ti1 1.779(2) 2_665 ? O3 C3 1.389(4) . ? O4 C7 1.406(4) . ? O4 C4 1.426(4) . ? O5 C1 1.424(4) . ? O5 C5 1.425(4) . ? O6 C6 1.429(4) . ? O6 C7 1.432(4) . ? C1 C2 1.533(5) . ? C1 H1 1.0000 . ? C2 C3 1.523(4) . ? C2 H2 1.0000 . ? C3 C4 1.506(4) . ? C3 H3 1.0000 . ? C4 C5 1.523(4) . ? C4 H4 1.0000 . ? C5 C6 1.534(5) . ? C5 H5 1.0000 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.503(5) . ? C7 H7 1.0000 . ? C8 C17 1.361(5) . ? C8 C9 1.412(5) . ? C9 C10 1.335(6) . ? C9 H9 0.9500 . ? C10 C11 1.425(7) . ? C10 H10 0.9500 . ? C11 C16 1.413(6) . ? C11 C12 1.423(6) . ? C12 C13 1.341(8) . ? C12 H12 0.9500 . ? C13 C14 1.414(8) . ? C13 H13 0.9500 . ? C14 C15 1.379(6) . ? C14 H14 0.9500 . ? C15 C16 1.410(6) . ? C15 H15 0.9500 . ? C16 C17 1.426(5) . ? C17 H17 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C23 1.405(5) . ? C19 C20 1.415(5) . ? C19 C24 1.508(5) . ? C20 C21 1.407(5) . ? C20 C25 1.493(5) . ? C21 C22 1.419(5) . ? C21 C26 1.504(5) . ? C22 C23 1.442(5) . ? C22 C27 1.499(5) . ? C23 C28 1.495(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 Cl3 1.786(10) . ? C29 Cl4 1.795(8) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ti1 O3 106.00(11) 2_665 . ? O2 Ti1 Cl1 98.34(9) 2_665 . ? O3 Ti1 Cl1 105.01(9) . . ? O2 Ti1 C23 110.44(13) 2_665 . ? O3 Ti1 C23 88.93(13) . . ? Cl1 Ti1 C23 143.23(10) . . ? O2 Ti1 C22 90.29(12) 2_665 . ? O3 Ti1 C22 123.73(13) . . ? Cl1 Ti1 C22 125.79(10) . . ? C23 Ti1 C22 35.94(13) . . ? O2 Ti1 C19 144.83(13) 2_665 . ? O3 Ti1 C19 83.10(13) . . ? Cl1 Ti1 C19 112.25(10) . . ? C23 Ti1 C19 34.69(13) . . ? C22 Ti1 C19 58.09(13) . . ? O2 Ti1 C21 106.38(12) 2_665 . ? O3 Ti1 C21 140.37(12) . . ? Cl1 Ti1 C21 92.25(10) . . ? C23 Ti1 C21 58.53(13) . . ? C22 Ti1 C21 34.92(13) . . ? C19 Ti1 C21 57.29(13) . . ? O2 Ti1 C20 140.54(12) 2_665 . ? O3 Ti1 C20 110.96(12) . . ? Cl1 Ti1 C20 85.24(9) . . ? C23 Ti1 C20 58.00(12) . . ? C22 Ti1 C20 57.79(13) . . ? C19 Ti1 C20 34.45(13) . . ? C21 Ti1 C20 34.21(12) . . ? C1 O1 C18 112.8(5) . . ? C2 O2 Ti1 165.9(2) . 2_665 ? C3 O3 Ti1 145.6(2) . . ? C7 O4 C4 109.8(2) . . ? C1 O5 C5 111.3(3) . . ? C6 O6 C7 110.8(3) . . ? O1 C1 O5 106.9(3) . . ? O1 C1 C2 107.0(3) . . ? O5 C1 C2 111.7(3) . . ? O1 C1 H1 110.4 . . ? O5 C1 H1 110.4 . . ? C2 C1 H1 110.4 . . ? O2 C2 C3 109.5(3) . . ? O2 C2 C1 109.5(3) . . ? C3 C2 C1 111.9(3) . . ? O2 C2 H2 108.6 . . ? C3 C2 H2 108.6 . . ? C1 C2 H2 108.6 . . ? O3 C3 C4 110.1(3) . . ? O3 C3 C2 110.7(3) . . ? C4 C3 C2 106.8(3) . . ? O3 C3 H3 109.7 . . ? C4 C3 H3 109.7 . . ? C2 C3 H3 109.7 . . ? O4 C4 C3 110.3(3) . . ? O4 C4 C5 109.8(3) . . ? C3 C4 C5 110.1(3) . . ? O4 C4 H4 108.9 . . ? C3 C4 H4 108.9 . . ? C5 C4 H4 108.9 . . ? O5 C5 C4 108.1(3) . . ? O5 C5 C6 108.6(3) . . ? C4 C5 C6 108.4(3) . . ? O5 C5 H5 110.5 . . ? C4 C5 H5 110.5 . . ? C6 C5 H5 110.5 . . ? O6 C6 C5 108.2(3) . . ? O6 C6 H6A 110.1 . . ? C5 C6 H6A 110.1 . . ? O6 C6 H6B 110.1 . . ? C5 C6 H6B 110.1 . . ? H6A C6 H6B 108.4 . . ? O4 C7 O6 110.6(3) . . ? O4 C7 C8 109.5(3) . . ? O6 C7 C8 107.1(3) . . ? O4 C7 H7 109.9 . . ? O6 C7 H7 109.9 . . ? C8 C7 H7 109.9 . . ? C17 C8 C9 119.5(4) . . ? C17 C8 C7 121.3(3) . . ? C9 C8 C7 119.2(3) . . ? C10 C9 C8 121.6(4) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C9 C10 C11 120.9(4) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C16 C11 C12 118.9(4) . . ? C16 C11 C10 118.4(4) . . ? C12 C11 C10 122.7(4) . . ? C13 C12 C11 120.6(5) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 121.1(4) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C15 C14 C13 119.8(5) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 120.2(5) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C11 119.3(4) . . ? C15 C16 C17 121.6(4) . . ? C11 C16 C17 119.0(4) . . ? C8 C17 C16 120.6(4) . . ? C8 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? O1 C18 H18A 109.5 . . ? O1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C23 C19 C20 108.9(3) . . ? C23 C19 C24 126.3(4) . . ? C20 C19 C24 124.8(4) . . ? C23 C19 Ti1 70.81(19) . . ? C20 C19 Ti1 73.60(19) . . ? C24 C19 Ti1 120.7(3) . . ? C21 C20 C19 108.0(3) . . ? C21 C20 C25 126.5(4) . . ? C19 C20 C25 125.4(4) . . ? C21 C20 Ti1 72.33(19) . . ? C19 C20 Ti1 71.96(19) . . ? C25 C20 Ti1 123.5(3) . . ? C20 C21 C22 108.4(3) . . ? C20 C21 C26 125.7(4) . . ? C22 C21 C26 125.8(4) . . ? C20 C21 Ti1 73.5(2) . . ? C22 C21 Ti1 70.92(19) . . ? C26 C21 Ti1 123.8(3) . . ? C21 C22 C23 107.4(3) . . ? C21 C22 C27 126.0(4) . . ? C23 C22 C27 126.6(4) . . ? C21 C22 Ti1 74.2(2) . . ? C23 C22 Ti1 71.58(19) . . ? C27 C22 Ti1 120.5(2) . . ? C19 C23 C22 107.3(3) . . ? C19 C23 C28 126.8(4) . . ? C22 C23 C28 125.9(3) . . ? C19 C23 Ti1 74.5(2) . . ? C22 C23 Ti1 72.48(19) . . ? C28 C23 Ti1 118.6(2) . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Cl3 C29 Cl4 108.8(5) . . ? Cl3 C29 H29A 109.9 . . ? Cl4 C29 H29A 109.9 . . ? Cl3 C29 H29B 109.9 . . ? Cl4 C29 H29B 109.9 . . ? H29A C29 H29B 108.3 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.089 _refine_diff_density_min -0.775 _refine_diff_density_rms 0.105