# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global #TrackingRef '09dalton.cif' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Ying Mu' _publ_contact_author_email YMU@JLU.EDU.CN _publ_section_title ; Propylene polymerization to high molecular weight atactic polypropylene and copolymerization with 1-hexene using monocyclopentadienyl titanium catalysts ; loop_ _publ_author_name 'Ying Mu' 'Qiaolin Wu' 'Qing Su' 'Ling Ye' 'Guanghua Li' # Attachment 'CIFs.txt' data_complex6 #1-(4-iPr-C6H4)-2,3,4,5-Me4-CpTiCl2(OC6H3iPr2-2,6) #TrackingRef '09dalton.cif' _database_code_depnum_ccdc_archive 'CCDC 750232' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H40 Cl2 O Ti' _chemical_formula_weight 535.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' 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 22.757(5) _cell_length_b 8.7719(18) _cell_length_c 15.626(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.38(3) _cell_angle_gamma 90.00 _cell_volume 3034.7(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 14146 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.172 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 0.477 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.883 _exptl_absorpt_correction_T_max 0.905 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22357 _diffrn_reflns_av_R_equivalents 0.0852 _diffrn_reflns_av_sigmaI/netI 0.0690 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5298 _reflns_number_gt 3151 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0468P)^2^+0.7947P] 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 5298 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1075 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1254 _refine_ls_wR_factor_gt 0.1082 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.007 _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 0.20424(3) 0.35346(6) 0.08595(4) 0.04257(19) Uani 1 1 d . . . Cl1 Cl 0.27666(4) 0.43929(11) 0.01931(6) 0.0580(3) Uani 1 1 d . . . Cl2 Cl 0.12132(4) 0.36800(12) -0.02641(7) 0.0699(3) Uani 1 1 d . . . O1 O 0.19408(9) 0.5094(2) 0.15330(14) 0.0463(6) Uani 1 1 d . . . C1 C 0.26658(17) 0.1780(4) 0.1796(2) 0.0510(9) Uani 1 1 d . . . C2 C 0.21210(17) 0.1926(4) 0.2077(2) 0.0482(9) Uani 1 1 d . . . C3 C 0.16477(17) 0.1354(4) 0.1400(3) 0.0548(9) Uani 1 1 d . . . C4 C 0.19022(19) 0.0827(4) 0.0709(3) 0.0599(10) Uani 1 1 d . . . C5 C 0.25245(19) 0.1086(4) 0.0935(2) 0.0562(10) Uani 1 1 d . . . C6 C 0.20406(19) 0.2555(4) 0.2940(2) 0.0649(11) Uani 1 1 d . . . H6A H 0.2039 0.1732 0.3344 0.097 Uiso 1 1 calc R . . H6B H 0.1664 0.3095 0.2846 0.097 Uiso 1 1 calc R . . H6C H 0.2367 0.3238 0.3178 0.097 Uiso 1 1 calc R . . C7 C 0.09985(19) 0.1224(5) 0.1439(3) 0.0821(13) Uani 1 1 d . . . H7A H 0.0923 0.0219 0.1632 0.123 Uiso 1 1 calc R . . H7B H 0.0746 0.1404 0.0865 0.123 Uiso 1 1 calc R . . H7C H 0.0910 0.1964 0.1844 0.123 Uiso 1 1 calc R . . C8 C 0.1565(2) 0.0018(5) -0.0112(3) 0.0931(15) Uani 1 1 d . . . H8A H 0.1774 0.0164 -0.0574 0.140 Uiso 1 1 calc R . . H8B H 0.1164 0.0427 -0.0291 0.140 Uiso 1 1 calc R . . H8C H 0.1543 -0.1051 0.0007 0.140 Uiso 1 1 calc R . . C9 C 0.2963(2) 0.0594(5) 0.0406(3) 0.0828(14) Uani 1 1 d . . . H9A H 0.2809 -0.0294 0.0068 0.124 Uiso 1 1 calc R . . H9B H 0.3344 0.0358 0.0795 0.124 Uiso 1 1 calc R . . H9C H 0.3015 0.1402 0.0017 0.124 Uiso 1 1 calc R . . C10 C 0.32796(18) 0.2050(4) 0.2340(3) 0.0596(10) Uani 1 1 d . . . C11 C 0.37446(19) 0.2679(5) 0.2020(3) 0.0807(13) Uani 1 1 d . . . H11 H 0.3671 0.2998 0.1438 0.097 Uiso 1 1 calc R . . C12 C 0.4318(2) 0.2840(6) 0.2558(4) 0.1092(19) Uani 1 1 d . . . H12 H 0.4623 0.3263 0.2327 0.131 Uiso 1 1 calc R . . C13 C 0.4448(2) 0.2388(6) 0.3426(4) 0.1074(19) Uani 1 1 d . . . C14 C 0.3984(3) 0.1759(6) 0.3744(4) 0.1038(18) Uani 1 1 d . . . H14 H 0.4058 0.1443 0.4327 0.125 Uiso 1 1 calc R . . C15 C 0.3419(2) 0.1592(5) 0.3217(3) 0.0765(12) Uani 1 1 d . . . H15 H 0.3118 0.1158 0.3451 0.092 Uiso 1 1 calc R . . C16 C 0.5080(3) 0.2560(10) 0.4036(6) 0.185(4) Uani 1 1 d . . . H16 H 0.4976 0.2584 0.4610 0.222 Uiso 1 1 calc R . . C17 C 0.5425(3) 0.1199(9) 0.4119(5) 0.172(3) Uani 1 1 d . . . H17A H 0.5500 0.0932 0.3559 0.258 Uiso 1 1 calc R . . H17B H 0.5206 0.0391 0.4319 0.258 Uiso 1 1 calc R . . H17C H 0.5802 0.1352 0.4537 0.258 Uiso 1 1 calc R . . C18 C 0.5332(3) 0.4011(10) 0.4024(6) 0.206(4) Uani 1 1 d . . . H18A H 0.5731 0.4020 0.4398 0.309 Uiso 1 1 calc R . . H18B H 0.5085 0.4745 0.4234 0.309 Uiso 1 1 calc R . . H18C H 0.5352 0.4264 0.3434 0.309 Uiso 1 1 calc R . . C19 C 0.18731(16) 0.6079(3) 0.2183(2) 0.0455(8) Uani 1 1 d . . . C20 C 0.23896(17) 0.6716(4) 0.2726(2) 0.0505(9) Uani 1 1 d . . . C21 C 0.2309(2) 0.7746(4) 0.3357(3) 0.0675(11) Uani 1 1 d . . . H21 H 0.2645 0.8192 0.3725 0.081 Uiso 1 1 calc R . . C22 C 0.1741(2) 0.8126(4) 0.3454(3) 0.0780(13) Uani 1 1 d . . . H22 H 0.1697 0.8823 0.3883 0.094 Uiso 1 1 calc R . . C23 C 0.1239(2) 0.7474(4) 0.2917(3) 0.0726(12) Uani 1 1 d . . . H23 H 0.0858 0.7738 0.2990 0.087 Uiso 1 1 calc R . . C24 C 0.12892(16) 0.6433(4) 0.2270(3) 0.0550(9) Uani 1 1 d . . . C25 C 0.30104(16) 0.6368(4) 0.2581(3) 0.0612(10) Uani 1 1 d . . . H25 H 0.2998 0.5331 0.2343 0.073 Uiso 1 1 calc R . . C26 C 0.3509(2) 0.6407(6) 0.3414(3) 0.1048(17) Uani 1 1 d . . . H26A H 0.3545 0.7421 0.3652 0.157 Uiso 1 1 calc R . . H26B H 0.3884 0.6114 0.3280 0.157 Uiso 1 1 calc R . . H26C H 0.3414 0.5712 0.3837 0.157 Uiso 1 1 calc R . . C27 C 0.3143(2) 0.7438(5) 0.1890(3) 0.0889(15) Uani 1 1 d . . . H27A H 0.3160 0.8466 0.2103 0.133 Uiso 1 1 calc R . . H27B H 0.2829 0.7354 0.1362 0.133 Uiso 1 1 calc R . . H27C H 0.3524 0.7172 0.1764 0.133 Uiso 1 1 calc R . . C28 C 0.07415(17) 0.5740(4) 0.1654(3) 0.0677(12) Uani 1 1 d . . . H28 H 0.0876 0.4802 0.1417 0.081 Uiso 1 1 calc R . . C29 C 0.0238(2) 0.5299(6) 0.2105(4) 0.114(2) Uani 1 1 d . . . H29A H 0.0402 0.4679 0.2610 0.172 Uiso 1 1 calc R . . H29B H -0.0067 0.4736 0.1701 0.172 Uiso 1 1 calc R . . H29C H 0.0063 0.6204 0.2287 0.172 Uiso 1 1 calc R . . C30 C 0.0501(2) 0.6795(5) 0.0875(4) 0.1040(18) Uani 1 1 d . . . H30A H 0.0347 0.7710 0.1079 0.156 Uiso 1 1 calc R . . H30B H 0.0183 0.6290 0.0461 0.156 Uiso 1 1 calc R . . H30C H 0.0822 0.7047 0.0595 0.156 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 0.0523(4) 0.0426(3) 0.0340(4) 0.0019(3) 0.0125(3) -0.0014(3) Cl1 0.0631(6) 0.0687(6) 0.0464(6) 0.0106(5) 0.0211(4) -0.0010(5) Cl2 0.0615(6) 0.0874(7) 0.0546(6) 0.0082(5) 0.0005(5) -0.0106(5) O1 0.0531(14) 0.0414(12) 0.0468(15) -0.0018(11) 0.0167(11) 0.0005(11) C1 0.074(3) 0.0409(19) 0.041(2) 0.0103(16) 0.0194(19) 0.0099(18) C2 0.072(2) 0.0387(18) 0.039(2) 0.0055(15) 0.0240(19) 0.0014(17) C3 0.071(2) 0.0401(19) 0.058(2) 0.0070(18) 0.026(2) -0.0083(19) C4 0.091(3) 0.041(2) 0.051(3) -0.0066(18) 0.021(2) -0.004(2) C5 0.083(3) 0.043(2) 0.048(2) 0.0033(17) 0.027(2) 0.011(2) C6 0.098(3) 0.058(2) 0.046(2) 0.0125(19) 0.031(2) 0.005(2) C7 0.086(3) 0.071(3) 0.098(4) -0.001(3) 0.038(3) -0.025(2) C8 0.139(4) 0.065(3) 0.075(3) -0.027(2) 0.024(3) -0.027(3) C9 0.116(4) 0.071(3) 0.074(3) 0.000(2) 0.048(3) 0.026(3) C10 0.065(3) 0.057(2) 0.056(3) 0.0113(19) 0.013(2) 0.013(2) C11 0.068(3) 0.098(3) 0.075(3) 0.027(3) 0.013(3) 0.020(3) C12 0.067(3) 0.122(4) 0.132(5) 0.039(4) 0.011(3) 0.014(3) C13 0.081(4) 0.100(4) 0.122(5) 0.027(4) -0.016(4) 0.018(3) C14 0.110(4) 0.102(4) 0.078(4) 0.026(3) -0.022(3) 0.003(4) C15 0.086(3) 0.076(3) 0.063(3) 0.019(2) 0.007(2) 0.007(2) C16 0.090(5) 0.161(7) 0.253(10) 0.038(7) -0.062(6) 0.002(5) C17 0.080(4) 0.210(8) 0.217(9) 0.047(7) 0.016(5) 0.049(5) C18 0.106(5) 0.219(9) 0.253(11) 0.029(8) -0.041(6) -0.052(6) C19 0.057(2) 0.0320(17) 0.050(2) -0.0004(15) 0.0193(18) -0.0011(16) C20 0.067(2) 0.0342(18) 0.052(2) 0.0008(16) 0.0174(19) -0.0016(18) C21 0.086(3) 0.051(2) 0.067(3) -0.007(2) 0.018(2) -0.002(2) C22 0.113(4) 0.052(2) 0.079(3) -0.017(2) 0.042(3) 0.006(3) C23 0.084(3) 0.055(2) 0.091(4) 0.002(2) 0.046(3) 0.019(2) C24 0.061(2) 0.0397(19) 0.072(3) 0.0056(19) 0.030(2) 0.0025(19) C25 0.056(2) 0.056(2) 0.069(3) 0.001(2) 0.010(2) -0.008(2) C26 0.073(3) 0.142(5) 0.089(4) -0.004(3) -0.001(3) 0.004(3) C27 0.087(3) 0.090(3) 0.101(4) 0.011(3) 0.045(3) -0.014(3) C28 0.054(2) 0.056(2) 0.100(4) -0.001(2) 0.031(2) -0.005(2) C29 0.084(3) 0.113(4) 0.164(6) -0.005(4) 0.064(4) -0.024(3) C30 0.080(3) 0.091(3) 0.126(5) 0.016(3) -0.006(3) -0.016(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O1 1.773(2) . ? Ti1 Cl2 2.2643(13) . ? Ti1 Cl1 2.2719(12) . ? Ti1 C2 2.342(3) . ? Ti1 C3 2.351(3) . ? Ti1 C1 2.359(3) . ? Ti1 C4 2.401(3) . ? Ti1 C5 2.402(3) . ? O1 C19 1.370(4) . ? C1 C2 1.414(5) . ? C1 C5 1.444(5) . ? C1 C10 1.477(5) . ? C2 C3 1.415(5) . ? C2 C6 1.507(5) . ? C3 C4 1.416(5) . ? C3 C7 1.497(5) . ? C4 C5 1.396(5) . ? C4 C8 1.511(5) . ? C5 C9 1.498(5) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.385(5) . ? C10 C15 1.392(5) . ? C11 C12 1.386(6) . ? C11 H11 0.9300 . ? C12 C13 1.379(7) . ? C12 H12 0.9300 . ? C13 C14 1.381(7) . ? C13 C16 1.539(7) . ? C14 C15 1.365(6) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C18 1.397(9) . ? C16 C17 1.418(8) . ? C16 H16 0.9800 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.397(5) . ? C19 C24 1.401(5) . ? C20 C21 1.381(5) . ? C20 C25 1.513(5) . ? C21 C22 1.376(6) . ? C21 H21 0.9300 . ? C22 C23 1.375(6) . ? C22 H22 0.9300 . ? C23 C24 1.387(5) . ? C23 H23 0.9300 . ? C24 C28 1.515(5) . ? C25 C27 1.513(5) . ? C25 C26 1.516(5) . ? C25 H25 0.9800 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C30 1.526(6) . ? C28 C29 1.527(5) . ? C28 H28 0.9800 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ti1 Cl2 102.54(8) . . ? O1 Ti1 Cl1 102.97(8) . . ? Cl2 Ti1 Cl1 100.88(5) . . ? O1 Ti1 C2 88.77(11) . . ? Cl2 Ti1 C2 123.86(10) . . ? Cl1 Ti1 C2 130.15(10) . . ? O1 Ti1 C3 107.52(12) . . ? Cl2 Ti1 C3 90.30(10) . . ? Cl1 Ti1 C3 144.30(10) . . ? C2 Ti1 C3 35.11(12) . . ? O1 Ti1 C1 106.10(11) . . ? Cl2 Ti1 C1 142.34(9) . . ? Cl1 Ti1 C1 96.01(10) . . ? C2 Ti1 C1 35.00(12) . . ? C3 Ti1 C1 58.07(13) . . ? O1 Ti1 C4 142.07(12) . . ? Cl2 Ti1 C4 84.93(10) . . ? Cl1 Ti1 C4 112.14(11) . . ? C2 Ti1 C4 57.80(13) . . ? C3 Ti1 C4 34.66(12) . . ? C1 Ti1 C4 57.48(13) . . ? O1 Ti1 C5 141.38(12) . . ? Cl2 Ti1 C5 112.18(10) . . ? Cl1 Ti1 C5 86.97(10) . . ? C2 Ti1 C5 58.22(12) . . ? C3 Ti1 C5 57.54(13) . . ? C1 Ti1 C5 35.29(12) . . ? C4 Ti1 C5 33.81(12) . . ? C19 O1 Ti1 168.4(2) . . ? C2 C1 C5 107.8(3) . . ? C2 C1 C10 126.0(3) . . ? C5 C1 C10 125.5(3) . . ? C2 C1 Ti1 71.84(19) . . ? C5 C1 Ti1 74.00(19) . . ? C10 C1 Ti1 127.3(2) . . ? C1 C2 C3 107.8(3) . . ? C1 C2 C6 127.4(3) . . ? C3 C2 C6 124.7(4) . . ? C1 C2 Ti1 73.16(19) . . ? C3 C2 Ti1 72.81(19) . . ? C6 C2 Ti1 120.3(2) . . ? C2 C3 C4 108.1(3) . . ? C2 C3 C7 125.8(4) . . ? C4 C3 C7 126.0(4) . . ? C2 C3 Ti1 72.08(19) . . ? C4 C3 Ti1 74.6(2) . . ? C7 C3 Ti1 122.6(3) . . ? C5 C4 C3 108.9(3) . . ? C5 C4 C8 125.3(4) . . ? C3 C4 C8 125.7(4) . . ? C5 C4 Ti1 73.2(2) . . ? C3 C4 Ti1 70.76(19) . . ? C8 C4 Ti1 125.3(3) . . ? C4 C5 C1 107.4(3) . . ? C4 C5 C9 125.4(4) . . ? C1 C5 C9 127.0(4) . . ? C4 C5 Ti1 73.0(2) . . ? C1 C5 Ti1 70.71(18) . . ? C9 C5 Ti1 125.8(3) . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 116.8(4) . . ? C11 C10 C1 123.8(4) . . ? C15 C10 C1 119.4(4) . . ? C10 C11 C12 120.9(5) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C13 C12 C11 121.6(5) . . ? C13 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? C12 C13 C14 117.5(5) . . ? C12 C13 C16 122.5(6) . . ? C14 C13 C16 120.0(6) . . ? C15 C14 C13 121.1(5) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C10 122.1(5) . . ? C14 C15 H15 118.9 . . ? C10 C15 H15 118.9 . . ? C18 C16 C17 123.3(7) . . ? C18 C16 C13 114.1(6) . . ? C17 C16 C13 113.1(7) . . ? C18 C16 H16 100.3 . . ? C17 C16 H16 100.3 . . ? C13 C16 H16 100.3 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O1 C19 C20 118.7(3) . . ? O1 C19 C24 118.9(3) . . ? C20 C19 C24 122.4(3) . . ? C21 C20 C19 117.6(4) . . ? C21 C20 C25 121.5(4) . . ? C19 C20 C25 120.8(3) . . ? C22 C21 C20 121.4(4) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C23 C22 C21 120.0(4) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 121.5(4) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.3 . . ? C23 C24 C19 117.1(4) . . ? C23 C24 C28 122.3(4) . . ? C19 C24 C28 120.6(3) . . ? C27 C25 C20 109.2(3) . . ? C27 C25 C26 111.4(4) . . ? C20 C25 C26 113.9(4) . . ? C27 C25 H25 107.3 . . ? C20 C25 H25 107.3 . . ? C26 C25 H25 107.3 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 C30 110.8(3) . . ? C24 C28 C29 113.8(4) . . ? C30 C28 C29 110.7(4) . . ? C24 C28 H28 107.1 . . ? C30 C28 H28 107.1 . . ? C29 C28 H28 107.1 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.204 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.051 #===END data_complex7 #1-(4-Me-C6H4)-2,3,4,5-Me4-CpTiCl2(OC6H3iPr2-2,6) #TrackingRef '09dalton.cif' _database_code_depnum_ccdc_archive 'CCDC 750233' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H36 Cl2 O Ti' _chemical_formula_weight 507.37 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 Pbca 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' '-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 8.3715(17) _cell_length_b 17.975(4) _cell_length_c 36.081(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5429.6(19) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30174 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 27.59 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2144 _exptl_absorpt_coefficient_mu 0.529 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.862 _exptl_absorpt_correction_T_max 0.904 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47290 _diffrn_reflns_av_R_equivalents 0.0659 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6203 _reflns_number_gt 4061 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0540P)^2^+1.0543P] 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 6203 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0756 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1172 _refine_ls_wR_factor_gt 0.1063 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.59414(5) 0.337160(19) 0.124794(11) 0.03960(12) Uani 1 1 d . . . Cl1 Cl 0.60933(10) 0.22453(3) 0.09611(2) 0.0704(2) Uani 1 1 d . . . Cl2 Cl 0.47509(9) 0.30387(4) 0.178510(18) 0.0663(2) Uani 1 1 d . . . O1 O 0.43972(18) 0.38318(8) 0.09960(4) 0.0427(4) Uani 1 1 d . . . C1 C 0.7536(3) 0.43338(11) 0.15115(6) 0.0382(5) Uani 1 1 d . . . C2 C 0.8289(3) 0.36477(12) 0.16137(6) 0.0461(5) Uani 1 1 d . . . C3 C 0.8788(3) 0.32933(12) 0.12881(7) 0.0503(6) Uani 1 1 d . . . C4 C 0.8354(3) 0.37480(12) 0.09815(6) 0.0444(5) Uani 1 1 d . . . C5 C 0.7608(3) 0.43943(11) 0.11186(6) 0.0382(5) Uani 1 1 d . . . C6 C 0.8656(4) 0.34018(14) 0.20006(7) 0.0644(7) Uani 1 1 d . . . H6A H 0.9529 0.3056 0.1996 0.097 Uiso 1 1 calc R . . H6B H 0.7732 0.3166 0.2106 0.097 Uiso 1 1 calc R . . H6C H 0.8942 0.3826 0.2148 0.097 Uiso 1 1 calc R . . C7 C 0.9768(4) 0.25902(14) 0.12670(8) 0.0713(8) Uani 1 1 d . . . H7A H 1.0881 0.2712 0.1287 0.107 Uiso 1 1 calc R . . H7B H 0.9574 0.2347 0.1034 0.107 Uiso 1 1 calc R . . H7C H 0.9472 0.2264 0.1466 0.107 Uiso 1 1 calc R . . C8 C 0.8731(3) 0.35891(15) 0.05818(7) 0.0627(7) Uani 1 1 d . . . H8A H 0.7966 0.3835 0.0426 0.094 Uiso 1 1 calc R . . H8B H 0.8684 0.3062 0.0539 0.094 Uiso 1 1 calc R . . H8C H 0.9783 0.3768 0.0525 0.094 Uiso 1 1 calc R . . C9 C 0.7055(3) 0.50365(12) 0.08850(6) 0.0449(5) Uani 1 1 d . . . H9A H 0.7952 0.5345 0.0823 0.067 Uiso 1 1 calc R . . H9B H 0.6286 0.5324 0.1021 0.067 Uiso 1 1 calc R . . H9C H 0.6572 0.4851 0.0662 0.067 Uiso 1 1 calc R . . C10 C 0.7071(3) 0.49294(11) 0.17751(6) 0.0400(5) Uani 1 1 d . . . C11 C 0.7653(3) 0.56450(12) 0.17218(6) 0.0432(5) Uani 1 1 d . . . H11 H 0.8245 0.5752 0.1510 0.052 Uiso 1 1 calc R . . C12 C 0.7366(3) 0.62012(12) 0.19784(6) 0.0491(6) Uani 1 1 d . . . H12 H 0.7776 0.6675 0.1937 0.059 Uiso 1 1 calc R . . C13 C 0.6484(3) 0.60685(13) 0.22958(6) 0.0510(6) Uani 1 1 d . . . C14 C 0.5869(3) 0.53625(13) 0.23449(6) 0.0561(7) Uani 1 1 d . . . H14 H 0.5247 0.5263 0.2553 0.067 Uiso 1 1 calc R . . C15 C 0.6155(3) 0.48022(13) 0.20924(6) 0.0508(6) Uani 1 1 d . . . H15 H 0.5732 0.4331 0.2134 0.061 Uiso 1 1 calc R . . C16 C 0.6204(4) 0.66727(15) 0.25803(7) 0.0747(9) Uani 1 1 d . . . H16A H 0.5325 0.6979 0.2503 0.112 Uiso 1 1 calc R . . H16B H 0.7148 0.6973 0.2603 0.112 Uiso 1 1 calc R . . H16C H 0.5960 0.6450 0.2815 0.112 Uiso 1 1 calc R . . C17 C 0.3467(3) 0.43134(11) 0.07934(6) 0.0405(5) Uani 1 1 d . . . C18 C 0.3279(3) 0.41740(12) 0.04127(6) 0.0447(5) Uani 1 1 d . . . C19 C 0.2304(3) 0.46622(14) 0.02175(7) 0.0555(6) Uani 1 1 d . . . H19 H 0.2147 0.4588 -0.0035 0.067 Uiso 1 1 calc R . . C20 C 0.1564(3) 0.52522(15) 0.03893(7) 0.0605(7) Uani 1 1 d . . . H20 H 0.0907 0.5567 0.0253 0.073 Uiso 1 1 calc R . . C21 C 0.1791(3) 0.53804(13) 0.07630(8) 0.0567(6) Uani 1 1 d . . . H21 H 0.1290 0.5784 0.0875 0.068 Uiso 1 1 calc R . . C22 C 0.2756(3) 0.49174(12) 0.09757(6) 0.0456(5) Uani 1 1 d . . . C23 C 0.4074(3) 0.35106(13) 0.02316(6) 0.0496(6) Uani 1 1 d . . . H23 H 0.5074 0.3418 0.0365 0.060 Uiso 1 1 calc R . . C24 C 0.4503(4) 0.36346(17) -0.01757(7) 0.0730(8) Uani 1 1 d . . . H24A H 0.5185 0.3239 -0.0259 0.110 Uiso 1 1 calc R . . H24B H 0.5048 0.4102 -0.0202 0.110 Uiso 1 1 calc R . . H24C H 0.3544 0.3641 -0.0322 0.110 Uiso 1 1 calc R . . C25 C 0.3037(4) 0.28179(15) 0.02757(9) 0.0773(9) Uani 1 1 d . . . H25A H 0.2068 0.2879 0.0136 0.116 Uiso 1 1 calc R . . H25B H 0.2782 0.2748 0.0533 0.116 Uiso 1 1 calc R . . H25C H 0.3607 0.2391 0.0186 0.116 Uiso 1 1 calc R . . C26 C 0.3037(3) 0.50471(13) 0.13851(7) 0.0504(6) Uani 1 1 d . . . H26 H 0.4109 0.4860 0.1442 0.061 Uiso 1 1 calc R . . C27 C 0.3009(5) 0.58700(15) 0.14932(9) 0.0880(10) Uani 1 1 d . . . H27A H 0.3721 0.6143 0.1335 0.132 Uiso 1 1 calc R . . H27B H 0.3344 0.5923 0.1746 0.132 Uiso 1 1 calc R . . H27C H 0.1944 0.6061 0.1466 0.132 Uiso 1 1 calc R . . C28 C 0.1873(4) 0.46056(17) 0.16180(8) 0.0729(8) Uani 1 1 d . . . H28A H 0.0810 0.4788 0.1577 0.109 Uiso 1 1 calc R . . H28B H 0.2144 0.4658 0.1875 0.109 Uiso 1 1 calc R . . H28C H 0.1926 0.4090 0.1549 0.109 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 0.0425(2) 0.03049(19) 0.0458(2) 0.00381(16) 0.00281(18) -0.00232(17) Cl1 0.0775(5) 0.0372(3) 0.0965(5) -0.0133(3) 0.0008(4) -0.0011(3) Cl2 0.0743(5) 0.0630(4) 0.0617(4) 0.0205(3) 0.0136(3) -0.0152(4) O1 0.0412(9) 0.0394(8) 0.0476(8) -0.0003(6) -0.0021(7) -0.0035(7) C1 0.0393(12) 0.0321(10) 0.0431(11) 0.0049(8) -0.0006(10) -0.0034(9) C2 0.0451(14) 0.0382(11) 0.0551(13) 0.0056(10) -0.0044(11) 0.0003(10) C3 0.0432(14) 0.0398(12) 0.0679(16) 0.0017(11) 0.0022(12) 0.0027(10) C4 0.0388(13) 0.0428(12) 0.0516(13) -0.0006(10) 0.0097(10) -0.0010(10) C5 0.0359(12) 0.0364(10) 0.0424(11) 0.0038(9) 0.0031(9) -0.0048(9) C6 0.078(2) 0.0532(14) 0.0623(16) 0.0158(12) -0.0168(14) 0.0069(14) C7 0.0633(19) 0.0509(15) 0.100(2) -0.0032(14) -0.0002(16) 0.0213(14) C8 0.0651(19) 0.0622(15) 0.0609(16) -0.0077(13) 0.0233(13) -0.0022(13) C9 0.0469(14) 0.0433(12) 0.0445(12) 0.0087(10) 0.0020(10) -0.0072(10) C10 0.0409(13) 0.0380(10) 0.0412(11) 0.0025(9) -0.0036(10) -0.0017(9) C11 0.0447(14) 0.0407(11) 0.0441(12) 0.0016(9) 0.0033(10) -0.0015(10) C12 0.0544(16) 0.0382(11) 0.0546(14) -0.0009(10) -0.0017(12) -0.0021(11) C13 0.0604(16) 0.0498(13) 0.0427(12) -0.0028(10) -0.0063(11) 0.0058(12) C14 0.0718(19) 0.0569(14) 0.0397(12) -0.0001(11) 0.0093(12) -0.0014(13) C15 0.0629(17) 0.0451(12) 0.0444(12) 0.0038(10) 0.0057(11) -0.0081(12) C16 0.109(3) 0.0577(16) 0.0577(16) -0.0138(13) 0.0092(16) 0.0053(16) C17 0.0303(12) 0.0392(11) 0.0520(13) 0.0032(9) -0.0023(10) -0.0057(9) C18 0.0357(13) 0.0484(12) 0.0501(13) 0.0013(10) -0.0015(10) -0.0068(10) C19 0.0450(15) 0.0681(16) 0.0535(14) 0.0049(12) -0.0053(12) 0.0002(13) C20 0.0450(15) 0.0647(16) 0.0717(18) 0.0119(14) -0.0075(13) 0.0084(13) C21 0.0416(15) 0.0509(14) 0.0777(18) -0.0008(13) 0.0028(13) 0.0070(11) C22 0.0335(13) 0.0448(12) 0.0585(14) -0.0021(10) 0.0015(10) -0.0048(10) C23 0.0486(15) 0.0526(13) 0.0477(13) -0.0044(10) -0.0014(11) -0.0021(11) C24 0.076(2) 0.083(2) 0.0604(16) -0.0032(15) 0.0130(15) 0.0105(16) C25 0.090(3) 0.0585(16) 0.084(2) -0.0152(15) 0.0123(18) -0.0152(16) C26 0.0367(13) 0.0529(13) 0.0617(14) -0.0148(11) 0.0003(11) -0.0003(11) C27 0.103(3) 0.0624(18) 0.098(2) -0.0309(17) -0.016(2) -0.0023(18) C28 0.0550(19) 0.097(2) 0.0664(17) -0.0139(16) 0.0096(14) -0.0065(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O1 1.7839(16) . ? Ti1 Cl2 2.2600(8) . ? Ti1 Cl1 2.2774(8) . ? Ti1 C4 2.337(2) . ? Ti1 C5 2.355(2) . ? Ti1 C1 2.383(2) . ? Ti1 C3 2.392(3) . ? Ti1 C2 2.419(2) . ? O1 C17 1.375(3) . ? C1 C5 1.423(3) . ? C1 C2 1.433(3) . ? C1 C10 1.484(3) . ? C2 C3 1.400(3) . ? C2 C6 1.496(3) . ? C3 C4 1.423(3) . ? C3 C7 1.508(3) . ? C4 C5 1.408(3) . ? C4 C8 1.504(3) . ? C5 C9 1.503(3) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.389(3) . ? C10 C15 1.396(3) . ? C11 C12 1.384(3) . ? C11 H11 0.9300 . ? C12 C13 1.383(3) . ? C12 H12 0.9300 . ? C13 C14 1.381(3) . ? C13 C16 1.513(3) . ? C14 C15 1.379(3) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C22 1.402(3) . ? C17 C18 1.405(3) . ? C18 C19 1.390(3) . ? C18 C23 1.514(3) . ? C19 C20 1.375(3) . ? C19 H19 0.9300 . ? C20 C21 1.381(4) . ? C20 H20 0.9300 . ? C21 C22 1.391(3) . ? C21 H21 0.9300 . ? C22 C26 1.514(3) . ? C23 C25 1.527(3) . ? C23 C24 1.529(3) . ? C23 H23 0.9800 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C28 1.512(4) . ? C26 C27 1.530(3) . ? C26 H26 0.9800 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ti1 Cl2 103.91(6) . . ? O1 Ti1 Cl1 102.77(5) . . ? Cl2 Ti1 Cl1 100.31(3) . . ? O1 Ti1 C4 106.40(8) . . ? Cl2 Ti1 C4 144.15(6) . . ? Cl1 Ti1 C4 91.27(6) . . ? O1 Ti1 C5 88.08(7) . . ? Cl2 Ti1 C5 129.64(6) . . ? Cl1 Ti1 C5 124.81(6) . . ? C4 Ti1 C5 34.94(7) . . ? O1 Ti1 C1 105.83(7) . . ? Cl2 Ti1 C1 95.57(6) . . ? Cl1 Ti1 C1 142.69(6) . . ? C4 Ti1 C1 57.98(7) . . ? C5 Ti1 C1 34.95(7) . . ? O1 Ti1 C3 141.28(8) . . ? Cl2 Ti1 C3 111.83(6) . . ? Cl1 Ti1 C3 85.39(6) . . ? C4 Ti1 C3 35.00(8) . . ? C5 Ti1 C3 57.82(8) . . ? C1 Ti1 C3 57.33(8) . . ? O1 Ti1 C2 140.51(7) . . ? Cl2 Ti1 C2 86.83(6) . . ? Cl1 Ti1 C2 112.64(6) . . ? C4 Ti1 C2 57.51(8) . . ? C5 Ti1 C2 57.75(7) . . ? C1 Ti1 C2 34.72(7) . . ? C3 Ti1 C2 33.84(8) . . ? C17 O1 Ti1 166.77(14) . . ? C5 C1 C2 107.67(18) . . ? C5 C1 C10 126.47(18) . . ? C2 C1 C10 124.84(19) . . ? C5 C1 Ti1 71.44(11) . . ? C2 C1 Ti1 74.01(12) . . ? C10 C1 Ti1 129.20(15) . . ? C3 C2 C1 107.86(19) . . ? C3 C2 C6 126.0(2) . . ? C1 C2 C6 125.8(2) . . ? C3 C2 Ti1 72.02(14) . . ? C1 C2 Ti1 71.27(13) . . ? C6 C2 Ti1 127.97(17) . . ? C2 C3 C4 108.3(2) . . ? C2 C3 C7 125.8(2) . . ? C4 C3 C7 125.5(2) . . ? C2 C3 Ti1 74.14(14) . . ? C4 C3 Ti1 70.38(13) . . ? C7 C3 Ti1 126.01(18) . . ? C5 C4 C3 108.30(19) . . ? C5 C4 C8 125.9(2) . . ? C3 C4 C8 125.6(2) . . ? C5 C4 Ti1 73.23(13) . . ? C3 C4 Ti1 74.62(13) . . ? C8 C4 Ti1 121.41(17) . . ? C4 C5 C1 107.80(18) . . ? C4 C5 C9 124.98(19) . . ? C1 C5 C9 127.18(19) . . ? C4 C5 Ti1 71.83(12) . . ? C1 C5 Ti1 73.61(11) . . ? C9 C5 Ti1 121.87(15) . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 117.2(2) . . ? C11 C10 C1 119.14(19) . . ? C15 C10 C1 123.47(19) . . ? C12 C11 C10 121.0(2) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C13 C12 C11 121.5(2) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C14 C13 C12 117.6(2) . . ? C14 C13 C16 121.0(2) . . ? C12 C13 C16 121.4(2) . . ? C15 C14 C13 121.4(2) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C14 C15 C10 121.2(2) . . ? C14 C15 H15 119.4 . . ? C10 C15 H15 119.4 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O1 C17 C22 118.61(19) . . ? O1 C17 C18 118.08(19) . . ? C22 C17 C18 123.3(2) . . ? C19 C18 C17 116.6(2) . . ? C19 C18 C23 122.5(2) . . ? C17 C18 C23 120.9(2) . . ? C20 C19 C18 121.5(2) . . ? C20 C19 H19 119.2 . . ? C18 C19 H19 119.2 . . ? C19 C20 C21 120.5(2) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C20 C21 C22 121.2(2) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C21 C22 C17 116.8(2) . . ? C21 C22 C26 122.4(2) . . ? C17 C22 C26 120.7(2) . . ? C18 C23 C25 110.3(2) . . ? C18 C23 C24 113.8(2) . . ? C25 C23 C24 110.6(2) . . ? C18 C23 H23 107.3 . . ? C25 C23 H23 107.3 . . ? C24 C23 H23 107.3 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C28 C26 C22 111.2(2) . . ? C28 C26 C27 110.8(2) . . ? C22 C26 C27 113.3(2) . . ? C28 C26 H26 107.1 . . ? C22 C26 H26 107.1 . . ? C27 C26 H26 107.1 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.226 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.044 #===END data_complex8 #1-(3,5-CF3-C6H3)-2,3,4,5-Me4-CpTiCl2(OC6H3iPr2-2,6) #TrackingRef '09dalton.cif' _database_code_depnum_ccdc_archive 'CCDC 750234' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H32 Cl2 F6 O Ti' _chemical_formula_weight 629.35 _chemical_absolute_configuration unk loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'Pc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 12.1002(17) _cell_length_b 8.7661(12) _cell_length_c 15.896(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.918(3) _cell_angle_gamma 90.00 _cell_volume 1564.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 28.00 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 0.500 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.869 _exptl_absorpt_correction_T_max 0.919 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10396 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0535 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 28.32 _reflns_number_total 5719 _reflns_number_gt 4029 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0602P)^2^+0.1712P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_number_reflns 5719 _refine_ls_number_parameters 415 _refine_ls_number_restraints 158 _refine_ls_R_factor_all 0.0758 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1233 _refine_ls_wR_factor_gt 0.1044 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.119 _refine_ls_shift/su_max 0.004 _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 C1 C 0.7873(4) 0.4529(4) 0.3833(3) 0.0390(8) Uani 1 1 d . . . C2 C 0.8078(4) 0.3827(5) 0.3091(3) 0.0467(10) Uani 1 1 d . . . C3 C 0.9285(5) 0.3313(5) 0.3439(3) 0.0512(11) Uani 1 1 d . . . C4 C 0.9798(4) 0.3697(5) 0.4372(3) 0.0461(10) Uani 1 1 d . . . C5 C 0.8928(4) 0.4432(4) 0.4623(3) 0.0388(8) Uani 1 1 d . . . C6 C 0.6668(4) 0.4961(5) 0.3815(3) 0.0433(9) Uani 1 1 d . . . C7 C 0.5934(5) 0.6020(5) 0.3211(3) 0.0511(10) Uani 1 1 d . . . H7 H 0.6202 0.6528 0.2810 0.061 Uiso 1 1 calc R . . C8 C 0.4794(4) 0.6327(6) 0.3205(4) 0.0606(12) Uani 1 1 d . A . C9 C 0.4377(5) 0.5538(7) 0.3774(4) 0.0648(15) Uani 1 1 d . . . H9 H 0.3610 0.5715 0.3754 0.078 Uiso 1 1 calc R . . C10 C 0.5093(4) 0.4490(6) 0.4370(4) 0.0594(12) Uani 1 1 d . A . C11 C 0.6227(4) 0.4202(5) 0.4392(3) 0.0521(11) Uani 1 1 d . . . H11 H 0.6704 0.3489 0.4800 0.063 Uiso 1 1 calc R . . C12 C 0.4025(5) 0.7514(7) 0.2576(4) 0.0768(16) Uani 1 1 d D . . C13 C 0.4635(5) 0.3612(7) 0.4983(4) 0.0832(18) Uani 1 1 d D . . C14 C 0.7180(6) 0.3533(7) 0.2169(4) 0.0706(15) Uani 1 1 d . . . H14A H 0.6474 0.4116 0.2082 0.106 Uiso 1 1 calc R . . H14B H 0.6986 0.2467 0.2105 0.106 Uiso 1 1 calc R . . H14C H 0.7500 0.3828 0.1724 0.106 Uiso 1 1 calc R . . C15 C 0.9853(7) 0.2392(7) 0.2913(5) 0.0832(19) Uani 1 1 d . . . H15A H 1.0697 0.2570 0.3152 0.125 Uiso 1 1 calc R . . H15B H 0.9525 0.2689 0.2287 0.125 Uiso 1 1 calc R . . H15C H 0.9701 0.1328 0.2965 0.125 Uiso 1 1 calc R . . C16 C 1.1041(5) 0.3292(7) 0.4997(4) 0.0716(15) Uani 1 1 d . . . H16A H 1.1042 0.2291 0.5243 0.107 Uiso 1 1 calc R . . H16B H 1.1314 0.4020 0.5483 0.107 Uiso 1 1 calc R . . H16C H 1.1561 0.3306 0.4666 0.107 Uiso 1 1 calc R . . C17 C 0.9092(4) 0.4944(5) 0.5565(3) 0.0529(10) Uani 1 1 d . . . H17A H 0.8959 0.4099 0.5899 0.079 Uiso 1 1 calc R . . H17B H 0.8534 0.5742 0.5531 0.079 Uiso 1 1 calc R . . H17C H 0.9889 0.5319 0.5866 0.079 Uiso 1 1 calc R . . C18 C 0.9922(5) 0.8459(5) 0.5148(3) 0.0522(11) Uani 1 1 d . . . C19 C 0.8975(6) 0.9267(5) 0.5230(4) 0.0619(14) Uani 1 1 d . . . C20 C 0.9239(7) 1.0266(6) 0.5954(5) 0.0787(18) Uani 1 1 d . . . H20 H 0.8624 1.0819 0.6025 0.094 Uiso 1 1 calc R . . C21 C 1.0375(8) 1.0464(7) 0.6567(5) 0.091(2) Uani 1 1 d . . . H21 H 1.0530 1.1163 0.7038 0.110 Uiso 1 1 calc R . . C22 C 1.1276(7) 0.9629(7) 0.6481(4) 0.0840(19) Uani 1 1 d . . . H22 H 1.2042 0.9739 0.6913 0.101 Uiso 1 1 calc R . . C23 C 1.1082(6) 0.8608(6) 0.5763(4) 0.0692(15) Uani 1 1 d . . . C24 C 0.7723(5) 0.9079(5) 0.4553(4) 0.0645(14) Uani 1 1 d . . . H24 H 0.7676 0.8060 0.4288 0.077 Uiso 1 1 calc R . . C25 C 0.6765(7) 0.9141(9) 0.4983(6) 0.101(2) Uani 1 1 d . . . H25A H 0.6910 0.8342 0.5424 0.152 Uiso 1 1 calc R . . H25B H 0.5990 0.9009 0.4519 0.152 Uiso 1 1 calc R . . H25C H 0.6803 1.0111 0.5273 0.152 Uiso 1 1 calc R . . C26 C 0.7471(7) 1.0223(7) 0.3778(5) 0.093(2) Uani 1 1 d . . . H26A H 0.7571 1.1241 0.4017 0.139 Uiso 1 1 calc R . . H26B H 0.6669 1.0093 0.3354 0.139 Uiso 1 1 calc R . . H26C H 0.8016 1.0052 0.3476 0.139 Uiso 1 1 calc R . . C27 C 1.2119(6) 0.7744(7) 0.5664(5) 0.093(2) Uani 1 1 d . . . H27 H 1.1777 0.6857 0.5279 0.112 Uiso 1 1 calc R . . C28 C 1.2689(10) 0.8739(12) 0.5146(9) 0.154(4) Uani 1 1 d . . . H28A H 1.2100 0.9003 0.4565 0.231 Uiso 1 1 calc R . . H28B H 1.3325 0.8186 0.5061 0.231 Uiso 1 1 calc R . . H28C H 1.2999 0.9652 0.5485 0.231 Uiso 1 1 calc R . . C29 C 1.2988(11) 0.7125(13) 0.6563(8) 0.176(6) Uani 1 1 d . . . H29A H 1.3417 0.7956 0.6936 0.265 Uiso 1 1 calc R . . H29B H 1.3540 0.6443 0.6452 0.265 Uiso 1 1 calc R . . H29C H 1.2556 0.6585 0.6867 0.265 Uiso 1 1 calc R . . O1 O 0.9697(3) 0.7501(3) 0.4419(2) 0.0526(7) Uani 1 1 d . . . Cl1 Cl 0.80654(11) 0.71951(15) 0.23227(8) 0.0617(3) Uani 1 1 d . . . Cl2 Cl 1.09921(11) 0.58862(15) 0.32509(10) 0.0686(4) Uani 1 1 d . . . Ti1 Ti 0.93354(5) 0.60335(7) 0.35902(4) 0.03951(18) Uani 1 1 d . . . F1 F 0.4587(6) 0.8354(9) 0.2178(6) 0.110(2) Uani 0.662(9) 1 d PDU A 1 F2 F 0.3578(9) 0.8414(11) 0.3011(5) 0.118(3) Uani 0.662(9) 1 d PDU A 1 F3 F 0.3106(8) 0.6917(10) 0.1946(7) 0.135(3) Uani 0.662(9) 1 d PDU A 1 F4 F 0.5347(6) 0.2564(9) 0.5481(5) 0.099(2) Uani 0.662(9) 1 d PDU A 1 F5 F 0.3661(7) 0.2884(12) 0.4542(6) 0.125(3) Uani 0.662(9) 1 d PDU A 1 F6 F 0.4340(10) 0.4535(10) 0.5525(7) 0.136(3) Uani 0.662(9) 1 d PDU A 1 F1' F 0.4042(17) 0.743(2) 0.1777(8) 0.113(5) Uani 0.338(9) 1 d PDU A 2 F2' F 0.4244(15) 0.8888(11) 0.2895(10) 0.103(4) Uani 0.338(9) 1 d PDU A 2 F3' F 0.2917(9) 0.7363(18) 0.2427(12) 0.102(5) Uani 0.338(9) 1 d PDU A 2 F4' F 0.5424(12) 0.356(2) 0.5787(8) 0.109(5) Uani 0.338(9) 1 d PDU A 2 F5' F 0.436(3) 0.2239(17) 0.4650(15) 0.160(8) Uani 0.338(9) 1 d PDU A 2 F6' F 0.3656(10) 0.4070(17) 0.4980(10) 0.092(4) Uani 0.338(9) 1 d PDU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.038(2) 0.0368(18) 0.047(2) 0.0022(16) 0.0222(18) -0.0004(16) C2 0.050(2) 0.043(2) 0.054(3) -0.0036(18) 0.028(2) -0.0042(18) C3 0.054(2) 0.0403(19) 0.073(4) -0.006(2) 0.039(2) 0.000(2) C4 0.040(2) 0.044(2) 0.060(3) 0.0089(19) 0.024(2) 0.0056(17) C5 0.038(2) 0.0395(19) 0.045(2) 0.0063(16) 0.0225(18) 0.0005(16) C6 0.033(2) 0.048(2) 0.051(2) -0.0015(18) 0.0177(18) 0.0000(17) C7 0.044(2) 0.059(3) 0.052(3) 0.001(2) 0.020(2) 0.004(2) C8 0.043(3) 0.073(3) 0.065(3) 0.006(2) 0.018(2) 0.012(2) C9 0.031(2) 0.091(3) 0.076(4) 0.008(3) 0.024(3) 0.012(3) C10 0.039(2) 0.073(3) 0.073(3) 0.009(3) 0.029(2) 0.006(2) C11 0.042(2) 0.055(3) 0.064(3) 0.010(2) 0.026(2) 0.0054(19) C12 0.057(3) 0.100(5) 0.072(4) 0.012(3) 0.023(3) 0.022(3) C13 0.052(3) 0.106(5) 0.107(5) 0.023(4) 0.047(4) 0.008(3) C14 0.078(4) 0.081(4) 0.053(3) -0.017(3) 0.024(3) -0.014(3) C15 0.099(5) 0.068(3) 0.111(5) -0.021(3) 0.073(4) 0.007(3) C16 0.048(3) 0.084(4) 0.082(4) 0.025(3) 0.024(3) 0.015(3) C17 0.056(3) 0.063(3) 0.042(2) 0.006(2) 0.022(2) -0.004(2) C18 0.075(3) 0.036(2) 0.049(3) -0.0054(18) 0.027(2) -0.015(2) C19 0.092(4) 0.036(2) 0.071(3) -0.001(2) 0.044(3) -0.012(2) C20 0.123(5) 0.051(3) 0.085(4) -0.019(3) 0.064(4) -0.014(3) C21 0.153(7) 0.058(3) 0.078(4) -0.027(3) 0.061(5) -0.037(4) C22 0.113(5) 0.065(3) 0.068(4) -0.017(3) 0.028(4) -0.036(4) C23 0.090(4) 0.046(2) 0.066(3) -0.005(2) 0.024(3) -0.018(3) C24 0.087(4) 0.037(2) 0.084(4) -0.001(2) 0.048(3) 0.001(2) C25 0.091(5) 0.119(6) 0.114(6) 0.004(4) 0.063(5) 0.009(4) C26 0.115(6) 0.067(4) 0.099(5) 0.020(3) 0.043(4) 0.003(4) C27 0.074(4) 0.076(4) 0.107(5) -0.036(4) 0.009(4) -0.010(3) C28 0.118(8) 0.135(7) 0.244(13) -0.050(8) 0.108(9) -0.039(6) C29 0.143(9) 0.169(10) 0.137(9) -0.036(8) -0.041(7) 0.057(8) O1 0.062(2) 0.0436(15) 0.0561(19) -0.0038(13) 0.0262(16) -0.0085(14) Cl1 0.0637(7) 0.0726(7) 0.0536(7) 0.0195(6) 0.0271(6) 0.0080(6) Cl2 0.0535(7) 0.0811(8) 0.0895(10) 0.0104(7) 0.0479(7) 0.0019(6) Ti1 0.0412(4) 0.0416(3) 0.0430(4) 0.0012(3) 0.0241(3) -0.0003(4) F1 0.094(4) 0.104(4) 0.124(4) 0.054(3) 0.032(3) 0.030(3) F2 0.123(5) 0.119(4) 0.113(4) 0.017(3) 0.043(4) 0.063(4) F3 0.110(5) 0.136(5) 0.112(4) 0.000(4) -0.013(4) 0.017(4) F4 0.083(3) 0.115(4) 0.120(4) 0.051(3) 0.062(3) 0.011(3) F5 0.093(4) 0.141(5) 0.147(5) 0.030(4) 0.051(4) -0.036(4) F6 0.166(5) 0.158(5) 0.132(5) -0.001(4) 0.112(4) 0.000(4) F1' 0.122(7) 0.121(7) 0.099(6) 0.014(4) 0.047(5) 0.017(5) F2' 0.101(6) 0.075(5) 0.108(6) 0.007(4) 0.011(4) 0.006(4) F3' 0.084(6) 0.107(6) 0.110(6) 0.019(5) 0.029(5) 0.019(4) F4' 0.104(6) 0.123(7) 0.101(6) 0.015(5) 0.037(5) -0.016(5) F5' 0.167(9) 0.162(9) 0.162(9) 0.007(5) 0.074(6) -0.011(5) F6' 0.075(5) 0.120(6) 0.098(6) 0.017(4) 0.054(4) 0.002(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.420(6) . ? C1 C2 1.432(6) . ? C1 C6 1.496(5) . ? C1 Ti1 2.351(4) . ? C2 C3 1.427(7) . ? C2 C14 1.485(7) . ? C2 Ti1 2.405(4) . ? C3 C4 1.418(7) . ? C3 C15 1.500(6) . ? C3 Ti1 2.396(4) . ? C4 C5 1.413(6) . ? C4 C16 1.504(7) . ? C4 Ti1 2.352(4) . ? C5 C17 1.503(6) . ? C5 Ti1 2.349(4) . ? C6 C7 1.391(6) . ? C6 C11 1.391(6) . ? C7 C8 1.402(7) . ? C7 H7 0.9300 . ? C8 C9 1.375(8) . ? C8 C12 1.501(8) . ? C9 C10 1.371(7) . ? C9 H9 0.9300 . ? C10 C11 1.383(6) . ? C10 C13 1.501(7) . ? C11 H11 0.9300 . ? C12 F3' 1.279(9) . ? C12 F1' 1.279(9) . ? C12 F2 1.293(7) . ? C12 F2' 1.295(9) . ? C12 F3 1.297(8) . ? C12 F1 1.313(7) . ? C13 F6' 1.248(9) . ? C13 F4' 1.279(9) . ? C13 F5 1.293(8) . ? C13 F4 1.305(7) . ? C13 F5' 1.307(10) . ? C13 F6 1.324(8) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 O1 1.373(5) . ? C18 C23 1.384(8) . ? C18 C19 1.395(8) . ? C19 C20 1.384(8) . ? C19 C24 1.504(8) . ? C20 C21 1.367(11) . ? C20 H20 0.9300 . ? C21 C22 1.362(11) . ? C21 H21 0.9300 . ? C22 C23 1.400(8) . ? C22 H22 0.9300 . ? C23 C27 1.524(10) . ? C24 C26 1.528(8) . ? C24 C25 1.551(9) . ? C24 H24 0.9800 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C29 1.523(12) . ? C27 C28 1.529(13) . ? C27 H27 0.9800 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? O1 Ti1 1.776(3) . ? Cl1 Ti1 2.2685(14) . ? Cl2 Ti1 2.2657(12) . ? 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 C5 C1 C2 109.2(3) . . ? C5 C1 C6 125.4(4) . . ? C2 C1 C6 124.0(4) . . ? C5 C1 Ti1 72.3(2) . . ? C2 C1 Ti1 74.5(2) . . ? C6 C1 Ti1 130.0(3) . . ? C3 C2 C1 106.4(4) . . ? C3 C2 C14 126.4(4) . . ? C1 C2 C14 126.8(4) . . ? C3 C2 Ti1 72.3(2) . . ? C1 C2 Ti1 70.4(2) . . ? C14 C2 Ti1 127.2(3) . . ? C4 C3 C2 108.4(4) . . ? C4 C3 C15 126.7(5) . . ? C2 C3 C15 124.7(5) . . ? C4 C3 Ti1 71.0(2) . . ? C2 C3 Ti1 73.1(2) . . ? C15 C3 Ti1 126.3(3) . . ? C5 C4 C3 108.8(4) . . ? C5 C4 C16 126.0(5) . . ? C3 C4 C16 125.1(4) . . ? C5 C4 Ti1 72.4(2) . . ? C3 C4 Ti1 74.3(2) . . ? C16 C4 Ti1 122.5(3) . . ? C4 C5 C1 107.2(3) . . ? C4 C5 C17 125.6(4) . . ? C1 C5 C17 127.2(4) . . ? C4 C5 Ti1 72.6(2) . . ? C1 C5 Ti1 72.5(2) . . ? C17 C5 Ti1 122.2(3) . . ? C7 C6 C11 118.1(4) . . ? C7 C6 C1 123.3(4) . . ? C11 C6 C1 118.5(4) . . ? C6 C7 C8 120.4(5) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C9 C8 C7 120.0(4) . . ? C9 C8 C12 119.9(5) . . ? C7 C8 C12 120.1(5) . . ? C10 C9 C8 119.9(5) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 120.3(5) . . ? C9 C10 C13 120.1(4) . . ? C11 C10 C13 119.6(4) . . ? C10 C11 C6 121.2(4) . . ? C10 C11 H11 119.4 . . ? C6 C11 H11 119.4 . . ? F3' C12 F1' 102.4(12) . . ? F3' C12 F2 62.8(9) . . ? F1' C12 F2 137.0(9) . . ? F3' C12 F2' 102.5(11) . . ? F1' C12 F2' 111.6(12) . . ? F2 C12 F2' 44.7(8) . . ? F3' C12 F3 43.8(7) . . ? F1' C12 F3 62.4(9) . . ? F2 C12 F3 104.5(8) . . ? F2' C12 F3 132.0(9) . . ? F3' C12 F1 131.6(8) . . ? F1' C12 F1 49.6(8) . . ? F2 C12 F1 108.1(7) . . ? F2' C12 F1 66.5(9) . . ? F3 C12 F1 107.6(8) . . ? F3' C12 C8 113.4(7) . . ? F1' C12 C8 112.6(8) . . ? F2 C12 C8 110.2(5) . . ? F2' C12 C8 113.5(7) . . ? F3 C12 C8 111.9(6) . . ? F1 C12 C8 113.9(5) . . ? F6' C13 F4' 111.7(11) . . ? F6' C13 F5 59.0(8) . . ? F4' C13 F5 135.6(9) . . ? F6' C13 F4 129.7(8) . . ? F4' C13 F4 44.9(7) . . ? F5 C13 F4 104.1(7) . . ? F6' C13 F5' 101.5(14) . . ? F4' C13 F5' 110.7(14) . . ? F5 C13 F5' 44.3(11) . . ? F4 C13 F5' 66.8(12) . . ? F6' C13 F6 47.2(7) . . ? F4' C13 F6 69.8(10) . . ? F5 C13 F6 104.0(8) . . ? F4 C13 F6 108.3(7) . . ? F5' C13 F6 137.6(12) . . ? F6' C13 C10 114.3(7) . . ? F4' C13 C10 110.4(8) . . ? F5 C13 C10 112.5(6) . . ? F4 C13 C10 115.8(4) . . ? F5' C13 C10 107.8(11) . . ? F6 C13 C10 111.3(6) . . ? C2 C14 H14A 109.5 . . ? C2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C3 C15 H15A 109.5 . . ? C3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C4 C16 H16A 109.5 . . ? C4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C5 C17 H17A 109.5 . . ? C5 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C5 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O1 C18 C23 118.9(5) . . ? O1 C18 C19 118.6(5) . . ? C23 C18 C19 122.5(5) . . ? C20 C19 C18 117.1(6) . . ? C20 C19 C24 121.5(6) . . ? C18 C19 C24 121.4(4) . . ? C21 C20 C19 122.1(7) . . ? C21 C20 H20 118.9 . . ? C19 C20 H20 118.9 . . ? C22 C21 C20 119.3(6) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C21 C22 C23 121.9(7) . . ? C21 C22 H22 119.0 . . ? C23 C22 H22 119.0 . . ? C18 C23 C22 117.0(6) . . ? C18 C23 C27 122.5(5) . . ? C22 C23 C27 120.6(6) . . ? C19 C24 C26 110.5(5) . . ? C19 C24 C25 113.5(5) . . ? C26 C24 C25 112.1(5) . . ? C19 C24 H24 106.8 . . ? C26 C24 H24 106.8 . . ? C25 C24 H24 106.8 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C23 112.8(7) . . ? C29 C27 C28 114.6(9) . . ? C23 C27 C28 109.0(6) . . ? C29 C27 H27 106.6 . . ? C23 C27 H27 106.6 . . ? C28 C27 H27 106.6 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C18 O1 Ti1 170.2(3) . . ? O1 Ti1 Cl2 102.90(12) . . ? O1 Ti1 Cl1 103.39(12) . . ? Cl2 Ti1 Cl1 100.39(5) . . ? O1 Ti1 C5 88.40(14) . . ? Cl2 Ti1 C5 124.60(10) . . ? Cl1 Ti1 C5 129.78(11) . . ? O1 Ti1 C1 106.05(14) . . ? Cl2 Ti1 C1 142.56(10) . . ? Cl1 Ti1 C1 95.50(11) . . ? C5 Ti1 C1 35.17(14) . . ? O1 Ti1 C4 107.13(16) . . ? Cl2 Ti1 C4 91.10(11) . . ? Cl1 Ti1 C4 143.97(13) . . ? C5 Ti1 C4 34.99(14) . . ? C1 Ti1 C4 57.99(14) . . ? O1 Ti1 C3 141.79(16) . . ? Cl2 Ti1 C3 84.89(12) . . ? Cl1 Ti1 C3 111.98(14) . . ? C5 Ti1 C3 58.06(14) . . ? C1 Ti1 C3 57.69(14) . . ? C4 Ti1 C3 34.74(17) . . ? O1 Ti1 C2 141.07(14) . . ? Cl2 Ti1 C2 112.48(11) . . ? Cl1 Ti1 C2 86.14(12) . . ? C5 Ti1 C2 58.52(14) . . ? C1 Ti1 C2 35.03(14) . . ? C4 Ti1 C2 58.02(16) . . ? C3 Ti1 C2 34.59(17) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.352 _refine_diff_density_min -0.258 _refine_diff_density_rms 0.048 #===END