Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Simon Lancaster' 'Manfred Bochmann' 'Simon J. Coles' 'David L. Hughes' 'Michael B. Hursthouse' 'Mark E. Light' 'Dale A. Pennington' 'Mark Schormann' _publ_contact_author_name 'Dr Simon Lancaster' _publ_contact_author_address ; School of Chemical Sciences and Pharmacy University of East Anglia Norwich Norfolk NR4 7TJ UNITED KINGDOM ; _publ_contact_author_email S.LANCASTER@UEA.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; The synthesis, structure and catalytic activity of mono(salicylaldiminato) titanium and zirconium complexes ; data_dalep3 _database_code_depnum_ccdc_archive 'CCDC 214921' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 2a' _chemical_melting_point ? _chemical_formula_moiety 'C21 H26 Cl3 N O2 Ti' _chemical_formula_structural '[TiCl3(thf)(OC6H3tBu-6,-CHNPh-2)]' _chemical_formula_sum 'C21 H26 Cl3 N O2 Ti' _chemical_formula_weight 478.68 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' N N 0.0061 0.0033 '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 'P 21/c' #(no. 14) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.3850(15) _cell_length_b 31.797(6) _cell_length_c 9.815(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.50(3) _cell_angle_gamma 90.00 _cell_volume 2250.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plates _exptl_crystal_colour deep-red _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.413 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 0.753 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku R-Axis-IIc' _diffrn_measurement_method 'image-plate oscillation photos' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7928 _diffrn_reflns_av_R_equivalents 0.2680 _diffrn_reflns_av_sigmaI/netI 0.2324 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 25.36 _reflns_number_total 3383 _reflns_number_gt 1907 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'MSC R-Axis-II control software' _computing_cell_refinement 'DENZO/CELL (Otwinowski and Minor, 1985)' _computing_data_reduction 'DENZO, SCALEPACK (Otwinowski and Minor, 1985)' _computing_structure_solution 'SHELXS (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1371P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3383 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1406 _refine_ls_R_factor_gt 0.0882 _refine_ls_wR_factor_ref 0.2371 _refine_ls_wR_factor_gt 0.2088 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.931 _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 Ti Ti 0.19168(15) 0.61446(3) 0.03125(14) 0.0256(4) Uani 1 1 d . . . O1 O 0.1375(6) 0.65290(12) 0.1497(5) 0.0286(11) Uani 1 1 d . . . C11 C 0.0071(8) 0.68036(17) 0.1776(8) 0.0241(15) Uani 1 1 d . . . C12 C -0.1606(8) 0.68258(18) 0.0780(8) 0.0254(16) Uani 1 1 d . . . C13 C -0.2922(9) 0.71241(18) 0.0938(9) 0.0290(17) Uani 1 1 d . . . H13 H -0.4032 0.7150 0.0281 0.035 Uiso 1 1 calc R . . C14 C -0.2521(9) 0.73851(18) 0.2121(9) 0.0333(19) Uani 1 1 d . . . H14 H -0.3362 0.7593 0.2230 0.040 Uiso 1 1 calc R . . C15 C -0.0888(9) 0.73384(18) 0.3135(9) 0.0315(18) Uani 1 1 d . . . H15 H -0.0685 0.7510 0.3920 0.038 Uiso 1 1 calc R . . C16 C 0.0447(9) 0.70401(17) 0.2998(8) 0.0275(16) Uani 1 1 d . . . C161 C 0.2189(9) 0.69686(18) 0.4155(8) 0.0278(17) Uani 1 1 d . . . C162 C 0.2167(10) 0.7250(2) 0.5427(10) 0.040(2) Uani 1 1 d . . . H16A H 0.3266 0.7200 0.6134 0.060 Uiso 1 1 calc R . . H16B H 0.1092 0.7186 0.5791 0.060 Uiso 1 1 calc R . . H16C H 0.2130 0.7540 0.5150 0.060 Uiso 1 1 calc R . . C163 C 0.2240(10) 0.65104(19) 0.4654(9) 0.0345(17) Uani 1 1 d . . . H16D H 0.3333 0.6466 0.5372 0.052 Uiso 1 1 calc R . . H16E H 0.2259 0.6326 0.3884 0.052 Uiso 1 1 calc R . . H16F H 0.1159 0.6453 0.5018 0.052 Uiso 1 1 calc R . . C164 C 0.3949(9) 0.70738(19) 0.3619(9) 0.0358(19) Uani 1 1 d . . . H16G H 0.5025 0.7026 0.4349 0.054 Uiso 1 1 calc R . . H16H H 0.3914 0.7364 0.3340 0.054 Uiso 1 1 calc R . . H16I H 0.4006 0.6898 0.2835 0.054 Uiso 1 1 calc R . . N2 N -0.1008(7) 0.62661(15) -0.0827(7) 0.0323(16) Uani 1 1 d . . . C20 C -0.2041(9) 0.65554(18) -0.0457(8) 0.0290(17) Uani 1 1 d . . . H20 H -0.3196 0.6596 -0.1046 0.035 Uiso 1 1 calc R . . C21 C -0.1778(9) 0.60627(19) -0.2145(9) 0.0283(18) Uani 1 1 d . . . C22 C -0.2066(9) 0.5629(2) -0.2187(10) 0.039(2) Uani 1 1 d . . . H22 H -0.1765 0.5472 -0.1371 0.046 Uiso 1 1 calc R . . C23 C -0.2800(9) 0.5435(2) -0.3445(10) 0.043(2) Uani 1 1 d . . . H23 H -0.3010 0.5146 -0.3468 0.051 Uiso 1 1 calc R . . C24 C -0.3234(10) 0.5669(2) -0.4694(11) 0.047(2) Uani 1 1 d . . . H24 H -0.3728 0.5538 -0.5540 0.057 Uiso 1 1 calc R . . C25 C -0.2907(11) 0.6100(2) -0.4634(10) 0.048(2) Uani 1 1 d . . . H25 H -0.3165 0.6259 -0.5447 0.058 Uiso 1 1 calc R . . C26 C -0.2199(10) 0.6290(2) -0.3371(10) 0.038(2) Uani 1 1 d . . . H26 H -0.2000 0.6579 -0.3344 0.046 Uiso 1 1 calc R . . O3 O 0.2153(6) 0.56887(12) -0.1252(6) 0.0291(12) Uani 1 1 d . . . C31 C 0.2366(10) 0.5760(2) -0.2690(8) 0.0335(17) Uani 1 1 d . . . H31A H 0.3554 0.5890 -0.2687 0.040 Uiso 1 1 calc R . . H31B H 0.1391 0.5943 -0.3182 0.040 Uiso 1 1 calc R . . C32 C 0.2246(10) 0.5331(2) -0.3396(10) 0.044(2) Uani 1 1 d . . . H32A H 0.2931 0.5323 -0.4135 0.052 Uiso 1 1 calc R . . H32B H 0.0973 0.5246 -0.3763 0.052 Uiso 1 1 calc R . . C33 C 0.3193(11) 0.5060(2) -0.2112(9) 0.042(2) Uani 1 1 d . . . H33A H 0.2798 0.4769 -0.2241 0.051 Uiso 1 1 calc R . . H33B H 0.4532 0.5071 -0.1981 0.051 Uiso 1 1 calc R . . C34 C 0.2599(10) 0.52441(19) -0.0910(10) 0.047(2) Uani 1 1 d . . . H34A H 0.3585 0.5223 -0.0080 0.056 Uiso 1 1 calc R . . H34B H 0.1517 0.5098 -0.0740 0.056 Uiso 1 1 calc R . . Cl4 Cl 0.4950(2) 0.60402(5) 0.1371(2) 0.0345(5) Uani 1 1 d . . . Cl5 Cl 0.2576(2) 0.66431(4) -0.1268(2) 0.0316(5) Uani 1 1 d . . . Cl6 Cl 0.0745(3) 0.56024(5) 0.1461(2) 0.0385(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti 0.0263(7) 0.0229(6) 0.0257(9) -0.0012(5) 0.0017(6) 0.0000(4) O1 0.030(2) 0.028(2) 0.027(4) -0.0003(18) 0.004(2) 0.0025(17) C11 0.026(3) 0.022(3) 0.025(5) 0.003(3) 0.007(3) 0.005(2) C12 0.027(3) 0.026(3) 0.021(5) 0.003(2) 0.001(3) -0.001(2) C13 0.020(3) 0.032(3) 0.036(6) 0.002(3) 0.008(3) -0.003(2) C14 0.027(4) 0.023(3) 0.049(6) 0.000(3) 0.006(4) 0.001(2) C15 0.033(4) 0.026(3) 0.035(6) -0.010(3) 0.007(4) -0.004(3) C16 0.033(4) 0.025(3) 0.023(5) -0.001(3) 0.002(3) -0.002(2) C161 0.024(3) 0.031(3) 0.027(5) 0.001(3) 0.002(3) -0.003(3) C162 0.036(4) 0.036(4) 0.047(7) -0.006(3) 0.006(4) -0.001(3) C163 0.040(4) 0.034(4) 0.025(5) 0.005(3) -0.001(4) 0.001(3) C164 0.031(4) 0.031(3) 0.042(6) -0.005(3) 0.003(4) -0.005(3) N2 0.024(3) 0.026(3) 0.043(5) -0.002(2) -0.002(3) 0.000(2) C20 0.028(3) 0.028(3) 0.032(6) -0.002(3) 0.008(3) 0.000(3) C21 0.022(3) 0.032(3) 0.032(6) -0.005(3) 0.007(3) 0.003(2) C22 0.028(4) 0.035(4) 0.051(7) -0.014(3) 0.007(4) -0.005(3) C23 0.027(4) 0.049(4) 0.053(8) -0.022(4) 0.013(4) -0.007(3) C24 0.033(4) 0.060(5) 0.045(8) -0.021(4) 0.000(4) 0.004(3) C25 0.045(5) 0.057(5) 0.037(7) -0.001(4) -0.002(5) 0.014(4) C26 0.037(4) 0.035(4) 0.041(7) -0.007(3) 0.004(4) 0.004(3) O3 0.034(2) 0.019(2) 0.034(4) 0.0040(18) 0.008(2) 0.0026(17) C31 0.039(4) 0.036(4) 0.020(5) 0.000(3) -0.006(3) 0.005(3) C32 0.034(4) 0.035(4) 0.059(8) -0.009(3) 0.005(4) 0.002(3) C33 0.050(5) 0.028(4) 0.050(7) -0.005(3) 0.014(5) 0.002(3) C34 0.043(4) 0.021(3) 0.076(8) -0.003(3) 0.012(5) 0.006(3) Cl4 0.0298(9) 0.0338(9) 0.0358(13) -0.0019(7) -0.0017(8) 0.0039(6) Cl5 0.0364(9) 0.0261(8) 0.0312(12) 0.0027(6) 0.0047(8) -0.0030(6) Cl6 0.0484(11) 0.0320(9) 0.0364(13) 0.0016(7) 0.0121(10) -0.0067(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti O1 1.791(5) . ? Ti O3 2.146(5) . ? Ti N2 2.240(6) . ? Ti Cl4 2.281(2) . ? Ti Cl6 2.327(2) . ? Ti Cl5 2.342(2) . ? O1 C11 1.371(7) . ? C11 C16 1.392(10) . ? C11 C12 1.403(9) . ? C12 C13 1.391(8) . ? C12 C20 1.465(9) . ? C13 C14 1.406(11) . ? C13 H13 0.9300 . ? C14 C15 1.395(10) . ? C14 H14 0.9300 . ? C15 C16 1.396(8) . ? C15 H15 0.9300 . ? C16 C161 1.537(9) . ? C161 C163 1.535(9) . ? C161 C162 1.540(10) . ? C161 C164 1.541(9) . ? C162 H16A 0.9600 . ? C162 H16B 0.9600 . ? C162 H16C 0.9600 . ? C163 H16D 0.9600 . ? C163 H16E 0.9600 . ? C163 H16F 0.9600 . ? C164 H16G 0.9600 . ? C164 H16H 0.9600 . ? C164 H16I 0.9600 . ? N2 C20 1.296(8) . ? N2 C21 1.448(10) . ? C20 H20 0.9300 . ? C21 C26 1.381(11) . ? C21 C22 1.393(9) . ? C22 C23 1.383(11) . ? C22 H22 0.9300 . ? C23 C24 1.411(12) . ? C23 H23 0.9300 . ? C24 C25 1.389(11) . ? C24 H24 0.9300 . ? C25 C26 1.377(12) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? O3 C31 1.472(9) . ? O3 C34 1.474(7) . ? C31 C32 1.523(10) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.562(11) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.468(11) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? 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 Ti O3 171.76(19) . . ? O1 Ti N2 83.1(2) . . ? O3 Ti N2 88.8(2) . . ? O1 Ti Cl4 98.00(16) . . ? O3 Ti Cl4 90.21(14) . . ? N2 Ti Cl4 176.72(18) . . ? O1 Ti Cl6 91.85(15) . . ? O3 Ti Cl6 86.70(13) . . ? N2 Ti Cl6 87.14(16) . . ? Cl4 Ti Cl6 95.91(8) . . ? O1 Ti Cl5 94.36(15) . . ? O3 Ti Cl5 85.55(13) . . ? N2 Ti Cl5 82.48(16) . . ? Cl4 Ti Cl5 94.34(8) . . ? Cl6 Ti Cl5 167.17(9) . . ? C11 O1 Ti 146.1(5) . . ? O1 C11 C16 119.9(6) . . ? O1 C11 C12 116.4(6) . . ? C16 C11 C12 123.7(6) . . ? C13 C12 C11 119.3(6) . . ? C13 C12 C20 117.3(6) . . ? C11 C12 C20 123.4(6) . . ? C12 C13 C14 117.9(7) . . ? C12 C13 H13 121.1 . . ? C14 C13 H13 121.1 . . ? C15 C14 C13 121.4(6) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C14 C15 C16 121.5(7) . . ? C14 C15 H15 119.2 . . ? C16 C15 H15 119.2 . . ? C11 C16 C15 115.9(7) . . ? C11 C16 C161 122.4(6) . . ? C15 C16 C161 121.7(6) . . ? C163 C161 C16 109.6(5) . . ? C163 C161 C162 107.3(6) . . ? C16 C161 C162 111.0(5) . . ? C163 C161 C164 110.5(5) . . ? C16 C161 C164 110.4(6) . . ? C162 C161 C164 107.9(5) . . ? C161 C162 H16A 109.5 . . ? C161 C162 H16B 109.5 . . ? H16A C162 H16B 109.5 . . ? C161 C162 H16C 109.5 . . ? H16A C162 H16C 109.5 . . ? H16B C162 H16C 109.5 . . ? C161 C163 H16D 109.5 . . ? C161 C163 H16E 109.5 . . ? H16D C163 H16E 109.5 . . ? C161 C163 H16F 109.5 . . ? H16D C163 H16F 109.5 . . ? H16E C163 H16F 109.5 . . ? C161 C164 H16G 109.5 . . ? C161 C164 H16H 109.5 . . ? H16G C164 H16H 109.5 . . ? C161 C164 H16I 109.5 . . ? H16G C164 H16I 109.5 . . ? H16H C164 H16I 109.5 . . ? C20 N2 C21 115.2(6) . . ? C20 N2 Ti 123.0(5) . . ? C21 N2 Ti 121.2(4) . . ? N2 C20 C12 127.7(7) . . ? N2 C20 H20 116.2 . . ? C12 C20 H20 116.2 . . ? C26 C21 C22 119.2(8) . . ? C26 C21 N2 121.1(6) . . ? C22 C21 N2 119.7(7) . . ? C23 C22 C21 119.8(9) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 120.8(8) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C25 C24 C23 118.6(8) . . ? C25 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? C26 C25 C24 120.1(9) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C21 121.6(7) . . ? C25 C26 H26 119.2 . . ? C21 C26 H26 119.2 . . ? C31 O3 C34 107.5(5) . . ? C31 O3 Ti 128.7(3) . . ? C34 O3 Ti 122.3(5) . . ? O3 C31 C32 106.9(6) . . ? O3 C31 H31A 110.3 . . ? C32 C31 H31A 110.3 . . ? O3 C31 H31B 110.3 . . ? C32 C31 H31B 110.3 . . ? H31A C31 H31B 108.6 . . ? C31 C32 C33 99.0(6) . . ? C31 C32 H32A 112.0 . . ? C33 C32 H32A 112.0 . . ? C31 C32 H32B 112.0 . . ? C33 C32 H32B 112.0 . . ? H32A C32 H32B 109.7 . . ? C34 C33 C32 105.6(6) . . ? C34 C33 H33A 110.6 . . ? C32 C33 H33A 110.6 . . ? C34 C33 H33B 110.6 . . ? C32 C33 H33B 110.6 . . ? H33A C33 H33B 108.8 . . ? C33 C34 O3 106.9(7) . . ? C33 C34 H34A 110.3 . . ? O3 C34 H34A 110.3 . . ? C33 C34 H34B 110.3 . . ? O3 C34 H34B 110.3 . . ? H34A C34 H34B 108.6 . . ? _diffrn_measured_fraction_theta_max 0.822 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 0.822 _refine_diff_density_max 0.683 _refine_diff_density_min -0.719 _refine_diff_density_rms 0.165 #===END data_dale1 _database_code_depnum_ccdc_archive 'CCDC 214922' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 3b' _chemical_melting_point ? _chemical_formula_moiety 'C23 H30 Cl7 N O Ti2' _chemical_formula_structural '[TiCl3(mu-Cl)3TiCl{O-C6H3(tBu-6)-2-CHN-C6H3(iPr2-2,6)}]' _chemical_formula_sum 'C23 H30 Cl7 N O Ti2' _chemical_formula_weight 680.43 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' N N 0.0061 0.0033 '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 'P 21/n' #(equiv. to no. 14) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.880(1) _cell_length_b 19.315(1) _cell_length_c 15.511(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.80(1) _cell_angle_gamma 90.00 _cell_volume 2886.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'thick plate' _exptl_crystal_colour 'deep red,' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 1.220 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku R-Axis-IIc' _diffrn_measurement_method 'image-plate oscillation photos' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 15791 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0424 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.56 _reflns_number_total 5091 _reflns_number_gt 4308 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'MSC R-Axis-II control software' _computing_cell_refinement 'DENZO/CELL (Otwinowski and Minor, 1985)' _computing_data_reduction 'DENZO, SCALEPACK (Otwinowski and Minor, 1985)' _computing_structure_solution 'SHELXS (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0528P)^2^+0.7236P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5091 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0420 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0941 _refine_ls_wR_factor_gt 0.0912 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.005 _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 0.48748(4) 0.23512(2) 0.05157(3) 0.02925(12) Uani 1 1 d . . . Ti2 Ti 0.83005(5) 0.20370(2) 0.10730(3) 0.03549(13) Uani 1 1 d . . . Cl3 Cl 0.37410(7) 0.26493(3) -0.08172(4) 0.04049(16) Uani 1 1 d . . . Cl4 Cl 0.64779(6) 0.20096(3) 0.19276(4) 0.03375(15) Uani 1 1 d . . . Cl5 Cl 0.68539(6) 0.30923(3) 0.04806(4) 0.03352(14) Uani 1 1 d . . . Cl6 Cl 0.62823(6) 0.15181(3) -0.00416(4) 0.03790(15) Uani 1 1 d . . . Cl7 Cl 0.94944(7) 0.21249(4) 0.00294(5) 0.04721(18) Uani 1 1 d . . . Cl8 Cl 0.96043(7) 0.26834(3) 0.20815(5) 0.04563(17) Uani 1 1 d . . . Cl9 Cl 0.89849(7) 0.09999(3) 0.15668(5) 0.04993(19) Uani 1 1 d . . . O1 O 0.36764(16) 0.17877(7) 0.08728(11) 0.0313(4) Uani 1 1 d . . . C1 C 0.3260(2) 0.16791(11) 0.16354(16) 0.0293(5) Uani 1 1 d . . . C2 C 0.3168(2) 0.22714(11) 0.21491(17) 0.0311(5) Uani 1 1 d . . . C20 C 0.3449(2) 0.29539(11) 0.18669(17) 0.0327(5) Uani 1 1 d . . . H20 H 0.3146 0.3319 0.2167 0.039 Uiso 1 1 calc R . . C3 C 0.2736(3) 0.22036(13) 0.29394(17) 0.0357(5) Uani 1 1 d . . . H3 H 0.2649 0.2593 0.3276 0.043 Uiso 1 1 calc R . . C4 C 0.2441(3) 0.15575(13) 0.32190(18) 0.0398(6) Uani 1 1 d . . . H4 H 0.2184 0.1506 0.3757 0.048 Uiso 1 1 calc R . . C5 C 0.2526(3) 0.09850(13) 0.26994(17) 0.0385(6) Uani 1 1 d . . . H5 H 0.2302 0.0555 0.2899 0.046 Uiso 1 1 calc R . . C6 C 0.2924(2) 0.10140(11) 0.19009(17) 0.0327(5) Uani 1 1 d . . . C61 C 0.3024(3) 0.03652(12) 0.13434(18) 0.0370(6) Uani 1 1 d . . . C62 C 0.2626(4) -0.02815(14) 0.1805(2) 0.0659(10) Uani 1 1 d . . . H62A H 0.3246 -0.0332 0.2373 0.099 Uiso 1 1 calc R . . H62B H 0.2693 -0.0683 0.1451 0.099 Uiso 1 1 calc R . . H62C H 0.1692 -0.0235 0.1879 0.099 Uiso 1 1 calc R . . C63 C 0.2038(3) 0.04289(15) 0.0446(2) 0.0538(8) Uani 1 1 d . . . H63A H 0.1105 0.0479 0.0524 0.081 Uiso 1 1 calc R . . H63B H 0.2100 0.0021 0.0104 0.081 Uiso 1 1 calc R . . H63C H 0.2283 0.0827 0.0144 0.081 Uiso 1 1 calc R . . C64 C 0.4502(3) 0.02784(14) 0.1232(2) 0.0544(8) Uani 1 1 d . . . H64A H 0.5118 0.0241 0.1803 0.082 Uiso 1 1 calc R . . H64B H 0.4757 0.0673 0.0927 0.082 Uiso 1 1 calc R . . H64C H 0.4565 -0.0133 0.0897 0.082 Uiso 1 1 calc R . . N2 N 0.4068(2) 0.31242(9) 0.12517(13) 0.0290(4) Uani 1 1 d . . . C21 C 0.4163(2) 0.38714(11) 0.11099(16) 0.0301(5) Uani 1 1 d . . . C22 C 0.3086(2) 0.41944(12) 0.05084(17) 0.0329(5) Uani 1 1 d . . . C221 C 0.1770(3) 0.38236(12) 0.00435(17) 0.0366(6) Uani 1 1 d . . . H221 H 0.1943 0.3324 0.0099 0.044 Uiso 1 1 calc R . . C222 C 0.0596(3) 0.39949(14) 0.0502(2) 0.0471(7) Uani 1 1 d . . . H22A H -0.0235 0.3761 0.0206 0.071 Uiso 1 1 calc R . . H22B H 0.0439 0.4486 0.0482 0.071 Uiso 1 1 calc R . . H22C H 0.0846 0.3846 0.1107 0.071 Uiso 1 1 calc R . . C223 C 0.1349(3) 0.39979(14) -0.09421(19) 0.0459(7) Uani 1 1 d . . . H22D H 0.0516 0.3751 -0.1205 0.069 Uiso 1 1 calc R . . H22E H 0.2080 0.3865 -0.1226 0.069 Uiso 1 1 calc R . . H22F H 0.1186 0.4487 -0.1014 0.069 Uiso 1 1 calc R . . C23 C 0.3218(3) 0.49064(12) 0.03855(18) 0.0362(5) Uani 1 1 d . . . H23 H 0.2528 0.5139 -0.0015 0.043 Uiso 1 1 calc R . . C24 C 0.4341(3) 0.52674(12) 0.08430(18) 0.0388(6) Uani 1 1 d . . . H24 H 0.4417 0.5739 0.0740 0.047 Uiso 1 1 calc R . . C25 C 0.5359(3) 0.49370(12) 0.14553(18) 0.0378(6) Uani 1 1 d . . . H25 H 0.6103 0.5193 0.1771 0.045 Uiso 1 1 calc R . . C26 C 0.5302(2) 0.42308(11) 0.16121(17) 0.0335(5) Uani 1 1 d . . . C261 C 0.6390(3) 0.38847(12) 0.23266(18) 0.0404(6) Uani 1 1 d . . . H261 H 0.6450 0.3398 0.2161 0.048 Uiso 1 1 calc R . . C262 C 0.5988(3) 0.39055(15) 0.32158(19) 0.0534(8) Uani 1 1 d . . . H26A H 0.6696 0.3684 0.3653 0.080 Uiso 1 1 calc R . . H26B H 0.5123 0.3667 0.3173 0.080 Uiso 1 1 calc R . . H26C H 0.5891 0.4378 0.3383 0.080 Uiso 1 1 calc R . . C263 C 0.7821(3) 0.42053(15) 0.2419(2) 0.0604(9) Uani 1 1 d . . . H26D H 0.8471 0.3971 0.2879 0.091 Uiso 1 1 calc R . . H26E H 0.7785 0.4687 0.2567 0.091 Uiso 1 1 calc R . . H26F H 0.8112 0.4160 0.1871 0.091 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 0.0328(2) 0.0256(2) 0.0304(2) 0.00069(16) 0.00912(17) 0.00142(15) Ti2 0.0344(3) 0.0345(2) 0.0389(3) 0.00716(18) 0.01088(19) 0.00537(16) Cl3 0.0455(4) 0.0447(3) 0.0305(3) 0.0026(2) 0.0068(3) 0.0064(3) Cl4 0.0342(3) 0.0347(3) 0.0329(3) 0.0056(2) 0.0087(2) 0.0020(2) Cl5 0.0367(3) 0.0282(3) 0.0366(3) 0.0049(2) 0.0101(2) 0.0012(2) Cl6 0.0432(3) 0.0311(3) 0.0414(4) -0.0034(2) 0.0137(3) 0.0045(2) Cl7 0.0452(4) 0.0538(4) 0.0476(4) 0.0084(3) 0.0210(3) 0.0080(3) Cl8 0.0362(3) 0.0535(4) 0.0456(4) 0.0052(3) 0.0054(3) -0.0008(3) Cl9 0.0493(4) 0.0410(3) 0.0613(5) 0.0164(3) 0.0162(3) 0.0142(3) O1 0.0337(9) 0.0283(8) 0.0327(9) 0.0000(6) 0.0088(7) 0.0002(6) C1 0.0262(11) 0.0330(11) 0.0279(13) 0.0006(9) 0.0047(9) 0.0004(8) C2 0.0304(12) 0.0308(11) 0.0325(14) 0.0014(9) 0.0078(10) 0.0014(9) C20 0.0340(13) 0.0300(11) 0.0341(14) -0.0018(9) 0.0072(10) 0.0039(9) C3 0.0356(13) 0.0385(13) 0.0328(14) -0.0021(10) 0.0073(10) -0.0002(9) C4 0.0424(14) 0.0442(14) 0.0339(15) 0.0033(11) 0.0109(11) -0.0043(10) C5 0.0417(14) 0.0373(13) 0.0363(15) 0.0051(10) 0.0084(11) -0.0056(10) C6 0.0322(12) 0.0309(11) 0.0333(14) 0.0023(9) 0.0037(10) -0.0019(9) C61 0.0427(14) 0.0281(11) 0.0410(16) -0.0001(10) 0.0113(11) -0.0028(9) C62 0.109(3) 0.0321(14) 0.067(2) -0.0049(14) 0.043(2) -0.0169(15) C63 0.0604(19) 0.0466(16) 0.0491(19) -0.0150(13) 0.0010(14) 0.0029(13) C64 0.0496(17) 0.0334(14) 0.083(2) -0.0058(14) 0.0209(16) 0.0068(11) N2 0.0316(10) 0.0256(9) 0.0297(11) -0.0001(7) 0.0065(8) 0.0014(7) C21 0.0368(12) 0.0231(10) 0.0326(13) -0.0008(9) 0.0123(10) 0.0020(8) C22 0.0367(13) 0.0304(11) 0.0344(14) 0.0007(10) 0.0138(10) 0.0053(9) C221 0.0363(13) 0.0320(12) 0.0409(15) 0.0024(10) 0.0075(11) 0.0038(9) C222 0.0417(15) 0.0425(14) 0.059(2) 0.0051(12) 0.0157(13) 0.0026(11) C223 0.0435(16) 0.0483(15) 0.0430(17) 0.0031(12) 0.0034(12) 0.0034(11) C23 0.0430(14) 0.0312(12) 0.0376(15) 0.0035(10) 0.0161(11) 0.0080(10) C24 0.0521(16) 0.0249(11) 0.0448(16) 0.0005(10) 0.0225(12) 0.0024(10) C25 0.0445(14) 0.0300(12) 0.0420(15) -0.0067(10) 0.0162(11) -0.0044(10) C26 0.0392(13) 0.0290(11) 0.0338(14) -0.0039(9) 0.0118(10) 0.0011(9) C261 0.0410(14) 0.0333(12) 0.0426(16) -0.0049(11) 0.0003(11) 0.0004(10) C262 0.069(2) 0.0514(16) 0.0342(16) -0.0043(12) -0.0004(13) 0.0125(13) C263 0.0486(18) 0.0470(16) 0.076(2) -0.0069(15) -0.0056(15) -0.0046(13) _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 1.7843(16) . ? Ti1 N2 2.138(2) . ? Ti1 Cl3 2.1987(10) . ? Ti1 Cl6 2.4091(7) . ? Ti1 Cl5 2.4336(7) . ? Ti1 Cl4 2.4907(10) . ? Ti1 Ti2 3.3578(7) . ? Ti2 Cl8 2.1845(9) . ? Ti2 Cl9 2.1971(7) . ? Ti2 Cl7 2.2106(10) . ? Ti2 Cl4 2.4618(9) . ? Ti2 Cl6 2.5381(9) . ? Ti2 Cl5 2.5417(7) . ? O1 C1 1.352(3) . ? C1 C2 1.409(3) . ? C1 C6 1.411(3) . ? C2 C3 1.390(4) . ? C2 C20 1.436(3) . ? C20 N2 1.285(3) . ? C20 H20 0.9300 . ? C3 C4 1.374(4) . ? C3 H3 0.9300 . ? C4 C5 1.382(4) . ? C4 H4 0.9300 . ? C5 C6 1.381(4) . ? C5 H5 0.9300 . ? C6 C61 1.538(3) . ? C61 C63 1.516(4) . ? C61 C64 1.517(4) . ? C61 C62 1.533(4) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? N2 C21 1.466(3) . ? C21 C22 1.397(3) . ? C21 C26 1.402(3) . ? C22 C23 1.398(3) . ? C22 C221 1.519(4) . ? C221 C222 1.525(4) . ? C221 C223 1.530(4) . ? C221 H221 0.9800 . ? C222 H22A 0.9600 . ? C222 H22B 0.9600 . ? C222 H22C 0.9600 . ? C223 H22D 0.9600 . ? C223 H22E 0.9600 . ? C223 H22F 0.9600 . ? C23 C24 1.368(4) . ? C23 H23 0.9300 . ? C24 C25 1.378(4) . ? C24 H24 0.9300 . ? C25 C26 1.389(3) . ? C25 H25 0.9300 . ? C26 C261 1.518(3) . ? C261 C262 1.518(4) . ? C261 C263 1.521(4) . ? C261 H261 0.9800 . ? C262 H26A 0.9600 . ? C262 H26B 0.9600 . ? C262 H26C 0.9600 . ? C263 H26D 0.9600 . ? C263 H26E 0.9600 . ? C263 H26F 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 N2 84.76(7) . . ? O1 Ti1 Cl3 102.52(6) . . ? N2 Ti1 Cl3 98.44(6) . . ? O1 Ti1 Cl6 100.33(5) . . ? N2 Ti1 Cl6 166.23(6) . . ? Cl3 Ti1 Cl6 92.97(3) . . ? O1 Ti1 Cl5 163.22(6) . . ? N2 Ti1 Cl5 89.87(5) . . ? Cl3 Ti1 Cl5 93.98(3) . . ? Cl6 Ti1 Cl5 81.62(2) . . ? O1 Ti1 Cl4 84.37(6) . . ? N2 Ti1 Cl4 87.43(6) . . ? Cl3 Ti1 Cl4 171.28(3) . . ? Cl6 Ti1 Cl4 80.40(3) . . ? Cl5 Ti1 Cl4 79.51(2) . . ? O1 Ti1 Ti2 120.67(5) . . ? N2 Ti1 Ti2 117.55(5) . . ? Cl3 Ti1 Ti2 124.33(3) . . ? Cl6 Ti1 Ti2 48.89(2) . . ? Cl5 Ti1 Ti2 48.930(17) . . ? Cl4 Ti1 Ti2 46.95(2) . . ? Cl8 Ti2 Cl9 100.63(4) . . ? Cl8 Ti2 Cl7 98.90(4) . . ? Cl9 Ti2 Cl7 98.76(3) . . ? Cl8 Ti2 Cl4 90.71(3) . . ? Cl9 Ti2 Cl4 89.89(3) . . ? Cl7 Ti2 Cl4 165.61(3) . . ? Cl8 Ti2 Cl6 164.38(3) . . ? Cl9 Ti2 Cl6 90.69(3) . . ? Cl7 Ti2 Cl6 89.87(4) . . ? Cl4 Ti2 Cl6 78.48(3) . . ? Cl8 Ti2 Cl5 89.75(3) . . ? Cl9 Ti2 Cl5 164.20(3) . . ? Cl7 Ti2 Cl5 91.27(3) . . ? Cl4 Ti2 Cl5 78.00(3) . . ? Cl6 Ti2 Cl5 77.08(2) . . ? Cl8 Ti2 Ti1 118.81(3) . . ? Cl9 Ti2 Ti1 117.99(3) . . ? Cl7 Ti2 Ti1 117.94(3) . . ? Cl4 Ti2 Ti1 47.67(2) . . ? Cl6 Ti2 Ti1 45.659(18) . . ? Cl5 Ti2 Ti1 46.208(16) . . ? Ti2 Cl4 Ti1 85.38(3) . . ? Ti1 Cl5 Ti2 84.86(2) . . ? Ti1 Cl6 Ti2 85.45(3) . . ? C1 O1 Ti1 135.86(14) . . ? O1 C1 C2 116.1(2) . . ? O1 C1 C6 122.2(2) . . ? C2 C1 C6 121.7(2) . . ? C3 C2 C1 119.6(2) . . ? C3 C2 C20 118.2(2) . . ? C1 C2 C20 122.1(2) . . ? N2 C20 C2 128.1(2) . . ? N2 C20 H20 115.9 . . ? C2 C20 H20 115.9 . . ? C4 C3 C2 119.5(2) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 119.9(3) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C6 C5 C4 123.8(2) . . ? C6 C5 H5 118.1 . . ? C4 C5 H5 118.1 . . ? C5 C6 C1 115.5(2) . . ? C5 C6 C61 122.5(2) . . ? C1 C6 C61 122.0(2) . . ? C63 C61 C64 110.1(3) . . ? C63 C61 C62 108.4(2) . . ? C64 C61 C62 108.4(2) . . ? C63 C61 C6 110.0(2) . . ? C64 C61 C6 109.7(2) . . ? C62 C61 C6 110.3(2) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C20 N2 C21 114.85(19) . . ? C20 N2 Ti1 120.85(15) . . ? C21 N2 Ti1 124.29(15) . . ? C22 C21 C26 123.3(2) . . ? C22 C21 N2 118.4(2) . . ? C26 C21 N2 118.3(2) . . ? C21 C22 C23 116.8(2) . . ? C21 C22 C221 123.5(2) . . ? C23 C22 C221 119.6(2) . . ? C22 C221 C222 109.6(2) . . ? C22 C221 C223 112.7(2) . . ? C222 C221 C223 110.6(2) . . ? C22 C221 H221 107.9 . . ? C222 C221 H221 107.9 . . ? C223 C221 H221 107.9 . . ? C221 C222 H22A 109.5 . . ? C221 C222 H22B 109.5 . . ? H22A C222 H22B 109.5 . . ? C221 C222 H22C 109.5 . . ? H22A C222 H22C 109.5 . . ? H22B C222 H22C 109.5 . . ? C221 C223 H22D 109.5 . . ? C221 C223 H22E 109.5 . . ? H22D C223 H22E 109.5 . . ? C221 C223 H22F 109.5 . . ? H22D C223 H22F 109.5 . . ? H22E C223 H22F 109.5 . . ? C24 C23 C22 121.3(2) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C23 C24 C25 120.4(2) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C26 121.6(2) . . ? C24 C25 H25 119.2 . . ? C26 C25 H25 119.2 . . ? C25 C26 C21 116.6(2) . . ? C25 C26 C261 120.7(2) . . ? C21 C26 C261 122.6(2) . . ? C26 C261 C262 111.5(2) . . ? C26 C261 C263 112.5(2) . . ? C262 C261 C263 109.2(2) . . ? C26 C261 H261 107.8 . . ? C262 C261 H261 107.8 . . ? C263 C261 H261 107.8 . . ? C261 C262 H26A 109.5 . . ? C261 C262 H26B 109.5 . . ? H26A C262 H26B 109.5 . . ? C261 C262 H26C 109.5 . . ? H26A C262 H26C 109.5 . . ? H26B C262 H26C 109.5 . . ? C261 C263 H26D 109.5 . . ? C261 C263 H26E 109.5 . . ? H26D C263 H26E 109.5 . . ? C261 C263 H26F 109.5 . . ? H26D C263 H26F 109.5 . . ? H26E C263 H26F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ti1 Ti2 Cl8 -105.95(7) . . . . ? N2 Ti1 Ti2 Cl8 -5.01(7) . . . . ? Cl3 Ti1 Ti2 Cl8 118.81(4) . . . . ? Cl6 Ti1 Ti2 Cl8 177.98(4) . . . . ? Cl5 Ti1 Ti2 Cl8 57.72(4) . . . . ? Cl4 Ti1 Ti2 Cl8 -61.20(4) . . . . ? O1 Ti1 Ti2 Cl9 16.10(7) . . . . ? N2 Ti1 Ti2 Cl9 117.04(7) . . . . ? Cl3 Ti1 Ti2 Cl9 -119.14(4) . . . . ? Cl6 Ti1 Ti2 Cl9 -59.97(4) . . . . ? Cl5 Ti1 Ti2 Cl9 179.77(4) . . . . ? Cl4 Ti1 Ti2 Cl9 60.85(3) . . . . ? O1 Ti1 Ti2 Cl7 134.60(7) . . . . ? N2 Ti1 Ti2 Cl7 -124.46(7) . . . . ? Cl3 Ti1 Ti2 Cl7 -0.64(4) . . . . ? Cl6 Ti1 Ti2 Cl7 58.53(4) . . . . ? Cl5 Ti1 Ti2 Cl7 -61.72(3) . . . . ? Cl4 Ti1 Ti2 Cl7 179.35(4) . . . . ? O1 Ti1 Ti2 Cl4 -44.75(7) . . . . ? N2 Ti1 Ti2 Cl4 56.19(6) . . . . ? Cl3 Ti1 Ti2 Cl4 -179.99(3) . . . . ? Cl6 Ti1 Ti2 Cl4 -120.82(3) . . . . ? Cl5 Ti1 Ti2 Cl4 118.92(3) . . . . ? O1 Ti1 Ti2 Cl6 76.07(7) . . . . ? N2 Ti1 Ti2 Cl6 177.01(6) . . . . ? Cl3 Ti1 Ti2 Cl6 -59.17(4) . . . . ? Cl5 Ti1 Ti2 Cl6 -120.26(4) . . . . ? Cl4 Ti1 Ti2 Cl6 120.82(3) . . . . ? O1 Ti1 Ti2 Cl5 -163.67(7) . . . . ? N2 Ti1 Ti2 Cl5 -62.74(6) . . . . ? Cl3 Ti1 Ti2 Cl5 61.09(3) . . . . ? Cl6 Ti1 Ti2 Cl5 120.26(4) . . . . ? Cl4 Ti1 Ti2 Cl5 -118.92(3) . . . . ? Cl8 Ti2 Cl4 Ti1 129.83(3) . . . . ? Cl9 Ti2 Cl4 Ti1 -129.54(3) . . . . ? Cl7 Ti2 Cl4 Ti1 -2.30(13) . . . . ? Cl6 Ti2 Cl4 Ti1 -38.82(2) . . . . ? Cl5 Ti2 Cl4 Ti1 40.24(2) . . . . ? O1 Ti1 Cl4 Ti2 142.52(5) . . . . ? N2 Ti1 Cl4 Ti2 -132.49(5) . . . . ? Cl3 Ti1 Cl4 Ti2 0.05(19) . . . . ? Cl6 Ti1 Cl4 Ti2 41.02(2) . . . . ? Cl5 Ti1 Cl4 Ti2 -42.15(2) . . . . ? O1 Ti1 Cl5 Ti2 56.89(19) . . . . ? N2 Ti1 Cl5 Ti2 127.99(6) . . . . ? Cl3 Ti1 Cl5 Ti2 -133.56(3) . . . . ? Cl6 Ti1 Cl5 Ti2 -41.14(3) . . . . ? Cl4 Ti1 Cl5 Ti2 40.58(2) . . . . ? Cl8 Ti2 Cl5 Ti1 -132.20(3) . . . . ? Cl9 Ti2 Cl5 Ti1 -0.74(13) . . . . ? Cl7 Ti2 Cl5 Ti1 128.90(3) . . . . ? Cl4 Ti2 Cl5 Ti1 -41.42(2) . . . . ? Cl6 Ti2 Cl5 Ti1 39.33(3) . . . . ? O1 Ti1 Cl6 Ti2 -121.94(6) . . . . ? N2 Ti1 Cl6 Ti2 -11.2(2) . . . . ? Cl3 Ti1 Cl6 Ti2 134.76(3) . . . . ? Cl5 Ti1 Cl6 Ti2 41.17(2) . . . . ? Cl4 Ti1 Cl6 Ti2 -39.53(2) . . . . ? Cl8 Ti2 Cl6 Ti1 -6.59(12) . . . . ? Cl9 Ti2 Cl6 Ti1 130.13(3) . . . . ? Cl7 Ti2 Cl6 Ti1 -131.10(3) . . . . ? Cl4 Ti2 Cl6 Ti1 40.39(2) . . . . ? Cl5 Ti2 Cl6 Ti1 -39.77(2) . . . . ? N2 Ti1 O1 C1 -42.0(2) . . . . ? Cl3 Ti1 O1 C1 -139.54(19) . . . . ? Cl6 Ti1 O1 C1 125.04(19) . . . . ? Cl5 Ti1 O1 C1 29.8(3) . . . . ? Cl4 Ti1 O1 C1 45.89(19) . . . . ? Ti2 Ti1 O1 C1 77.0(2) . . . . ? Ti1 O1 C1 C2 36.2(3) . . . . ? Ti1 O1 C1 C6 -144.30(18) . . . . ? O1 C1 C2 C3 179.5(2) . . . . ? C6 C1 C2 C3 0.0(3) . . . . ? O1 C1 C2 C20 2.2(3) . . . . ? C6 C1 C2 C20 -177.3(2) . . . . ? C3 C2 C20 N2 167.3(2) . . . . ? C1 C2 C20 N2 -15.4(4) . . . . ? C1 C2 C3 C4 1.7(3) . . . . ? C20 C2 C3 C4 179.1(2) . . . . ? C2 C3 C4 C5 -2.3(4) . . . . ? C3 C4 C5 C6 1.3(4) . . . . ? C4 C5 C6 C1 0.4(4) . . . . ? C4 C5 C6 C61 179.3(2) . . . . ? O1 C1 C6 C5 179.5(2) . . . . ? C2 C1 C6 C5 -1.0(3) . . . . ? O1 C1 C6 C61 0.6(3) . . . . ? C2 C1 C6 C61 -180.0(2) . . . . ? C5 C6 C61 C63 119.4(3) . . . . ? C1 C6 C61 C63 -61.7(3) . . . . ? C5 C6 C61 C64 -119.3(3) . . . . ? C1 C6 C61 C64 59.5(3) . . . . ? C5 C6 C61 C62 0.0(4) . . . . ? C1 C6 C61 C62 178.8(2) . . . . ? C2 C20 N2 C21 178.6(2) . . . . ? C2 C20 N2 Ti1 -1.5(3) . . . . ? O1 Ti1 N2 C20 21.13(19) . . . . ? Cl3 Ti1 N2 C20 123.04(18) . . . . ? Cl6 Ti1 N2 C20 -91.4(3) . . . . ? Cl5 Ti1 N2 C20 -142.96(18) . . . . ? Cl4 Ti1 N2 C20 -63.45(18) . . . . ? Ti2 Ti1 N2 C20 -100.88(18) . . . . ? O1 Ti1 N2 C21 -158.90(18) . . . . ? Cl3 Ti1 N2 C21 -56.99(17) . . . . ? Cl6 Ti1 N2 C21 88.6(3) . . . . ? Cl5 Ti1 N2 C21 37.01(17) . . . . ? Cl4 Ti1 N2 C21 116.52(17) . . . . ? Ti2 Ti1 N2 C21 79.09(17) . . . . ? C20 N2 C21 C22 -89.5(3) . . . . ? Ti1 N2 C21 C22 90.5(2) . . . . ? C20 N2 C21 C26 87.8(3) . . . . ? Ti1 N2 C21 C26 -92.1(2) . . . . ? C26 C21 C22 C23 3.3(4) . . . . ? N2 C21 C22 C23 -179.5(2) . . . . ? C26 C21 C22 C221 -172.5(2) . . . . ? N2 C21 C22 C221 4.7(4) . . . . ? C21 C22 C221 C222 100.7(3) . . . . ? C23 C22 C221 C222 -75.0(3) . . . . ? C21 C22 C221 C223 -135.7(2) . . . . ? C23 C22 C221 C223 48.6(3) . . . . ? C21 C22 C23 C24 -0.8(4) . . . . ? C221 C22 C23 C24 175.1(2) . . . . ? C22 C23 C24 C25 -1.5(4) . . . . ? C23 C24 C25 C26 1.7(4) . . . . ? C24 C25 C26 C21 0.6(4) . . . . ? C24 C25 C26 C261 -176.4(2) . . . . ? C22 C21 C26 C25 -3.2(4) . . . . ? N2 C21 C26 C25 179.6(2) . . . . ? C22 C21 C26 C261 173.9(2) . . . . ? N2 C21 C26 C261 -3.3(4) . . . . ? C25 C26 C261 C262 88.2(3) . . . . ? C21 C26 C261 C262 -88.6(3) . . . . ? C25 C26 C261 C263 -34.8(3) . . . . ? C21 C26 C261 C263 148.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 25.56 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 0.300 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.063 # #===END # data_ssc0766 _database_code_depnum_ccdc_archive 'CCDC 250156' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Complex 4c' _chemical_melting_point ? _chemical_formula_moiety 'C20 H24 Cl3 N O Ti' _chemical_formula_structural '[TiCl3(OC6H3tBu-6,CHNMes-2)]' _chemical_formula_sum 'C20 H24 Cl3 N O Ti' _chemical_formula_weight 448.65 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' N N 0.0061 0.0033 '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' 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 9.6328(5) _cell_length_b 14.9548(8) _cell_length_c 14.9811(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2158.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6761 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 29.35 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 0.777 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 0.97 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.69840 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 15 _diffrn_reflns_number 12774 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0397 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 30.00 _reflns_number_total 5935 _reflns_number_gt 5352 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0463P)^2^+0.1632P] 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_abs_structure_Flack 0.06(2) _refine_ls_number_reflns 5935 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0807 _refine_ls_wR_factor_gt 0.0772 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 0.63031(4) 0.51263(2) 0.40348(2) 0.01891(8) Uani 1 1 d . . . Cl1 Cl 0.45181(6) 0.53873(4) 0.31205(3) 0.03405(12) Uani 1 1 d . . . Cl2 Cl 0.63196(6) 0.36319(3) 0.37440(3) 0.02698(10) Uani 1 1 d . . . Cl3 Cl 0.83761(5) 0.53860(4) 0.34206(3) 0.03043(12) Uani 1 1 d . . . O1 O 0.62071(15) 0.62397(8) 0.45132(8) 0.0194(3) Uani 1 1 d . . . N1 N 0.62714(17) 0.47687(10) 0.54232(9) 0.0184(3) Uani 1 1 d . . . C1 C 0.6307(2) 0.38384(11) 0.57164(11) 0.0187(3) Uani 1 1 d . . . C2 C 0.7588(2) 0.34448(13) 0.58917(13) 0.0211(4) Uani 1 1 d . . . C3 C 0.7599(2) 0.25473(14) 0.61423(12) 0.0225(4) Uani 1 1 d . . . H3 H 0.8460 0.2267 0.6274 0.027 Uiso 1 1 calc R . . C4 C 0.6384(2) 0.20521(11) 0.62050(11) 0.0218(3) Uani 1 1 d . . . C5 C 0.5128(2) 0.24740(13) 0.60403(12) 0.0201(4) Uani 1 1 d . . . H5 H 0.4292 0.2141 0.6093 0.024 Uiso 1 1 calc R . . C6 C 0.5059(2) 0.33731(13) 0.57998(11) 0.0193(4) Uani 1 1 d . . . C7 C 0.8928(2) 0.39604(15) 0.58039(14) 0.0277(4) Uani 1 1 d . . . H7A H 0.9713 0.3563 0.5929 0.042 Uiso 1 1 calc R . . H7B H 0.8931 0.4458 0.6230 0.042 Uiso 1 1 calc R . . H7C H 0.9010 0.4196 0.5196 0.042 Uiso 1 1 calc R . . C8 C 0.6431(3) 0.10790(13) 0.64465(14) 0.0276(4) Uani 1 1 d . . . H8A H 0.7386 0.0910 0.6595 0.041 Uiso 1 1 calc R . . H8B H 0.6108 0.0721 0.5939 0.041 Uiso 1 1 calc R . . H8C H 0.5828 0.0970 0.6962 0.041 Uiso 1 1 calc R . . C9 C 0.3691(2) 0.38228(13) 0.56446(14) 0.0257(4) Uani 1 1 d . . . H9A H 0.3547 0.4285 0.6099 0.039 Uiso 1 1 calc R . . H9B H 0.2944 0.3379 0.5682 0.039 Uiso 1 1 calc R . . H9C H 0.3687 0.4099 0.5051 0.039 Uiso 1 1 calc R . . C10 C 0.62965(19) 0.53316(11) 0.60890(10) 0.0181(3) Uani 1 1 d . . . H10 H 0.6299 0.5073 0.6668 0.022 Uiso 1 1 calc R . . C11 C 0.6320(2) 0.62861(11) 0.60575(11) 0.0174(3) Uani 1 1 d . . . C12 C 0.6395(2) 0.67658(12) 0.68613(11) 0.0212(3) Uani 1 1 d . . . H12 H 0.6409 0.6461 0.7418 0.025 Uiso 1 1 calc R . . C13 C 0.6448(2) 0.76838(13) 0.68308(12) 0.0253(4) Uani 1 1 d . . . H13 H 0.6506 0.8018 0.7369 0.030 Uiso 1 1 calc R . . C14 C 0.6417(2) 0.81268(12) 0.60102(12) 0.0223(3) Uani 1 1 d . . . H14 H 0.6451 0.8762 0.6009 0.027 Uiso 1 1 calc R . . C15 C 0.6340(2) 0.76850(11) 0.51922(11) 0.0182(3) Uani 1 1 d . . . C16 C 0.6287(2) 0.67484(12) 0.52408(11) 0.0171(3) Uani 1 1 d . . . C17 C 0.6337(2) 0.81771(12) 0.42990(12) 0.0207(3) Uani 1 1 d . . . C18 C 0.7600(2) 0.78905(17) 0.37452(15) 0.0309(5) Uani 1 1 d . . . H18A H 0.8452 0.8018 0.4080 0.046 Uiso 1 1 calc R . . H18B H 0.7611 0.8223 0.3181 0.046 Uiso 1 1 calc R . . H18C H 0.7545 0.7248 0.3621 0.046 Uiso 1 1 calc R . . C19 C 0.6426(3) 0.91883(13) 0.44342(15) 0.0353(5) Uani 1 1 d . . . H19A H 0.6398 0.9488 0.3853 0.053 Uiso 1 1 calc R . . H19B H 0.7297 0.9336 0.4739 0.053 Uiso 1 1 calc R . . H19C H 0.5640 0.9389 0.4798 0.053 Uiso 1 1 calc R . . C20 C 0.4999(2) 0.79695(16) 0.37838(15) 0.0319(5) Uani 1 1 d . . . H20A H 0.5005 0.8292 0.3215 0.048 Uiso 1 1 calc R . . H20B H 0.4195 0.8158 0.4138 0.048 Uiso 1 1 calc R . . H20C H 0.4943 0.7325 0.3670 0.048 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 0.02217(16) 0.02135(15) 0.01321(13) -0.00179(11) 0.00107(12) -0.00250(13) Cl1 0.0339(3) 0.0362(3) 0.0321(2) 0.0015(2) -0.0129(2) -0.0055(2) Cl2 0.0357(3) 0.0240(2) 0.02129(19) -0.00627(16) 0.00375(19) -0.0031(2) Cl3 0.0277(2) 0.0337(3) 0.0299(2) -0.0090(2) 0.00977(18) -0.0062(2) O1 0.0245(7) 0.0201(6) 0.0138(5) 0.0008(4) 0.0004(5) -0.0005(6) N1 0.0193(7) 0.0179(7) 0.0180(6) 0.0008(5) 0.0007(6) 0.0001(7) C1 0.0235(9) 0.0170(8) 0.0158(7) 0.0000(6) 0.0005(7) 0.0011(8) C2 0.0209(9) 0.0209(9) 0.0216(9) -0.0016(7) 0.0002(7) -0.0013(7) C3 0.0231(9) 0.0218(9) 0.0224(9) 0.0002(7) -0.0018(7) 0.0043(7) C4 0.0287(9) 0.0183(8) 0.0184(8) -0.0012(6) 0.0022(7) 0.0031(8) C5 0.0228(9) 0.0196(9) 0.0180(8) -0.0008(7) 0.0030(7) -0.0006(7) C6 0.0202(9) 0.0221(9) 0.0156(8) -0.0005(6) 0.0019(6) 0.0008(7) C7 0.0209(10) 0.0277(10) 0.0345(11) 0.0012(8) -0.0021(8) -0.0035(8) C8 0.0320(11) 0.0189(8) 0.0318(10) -0.0003(7) 0.0023(9) 0.0036(9) C9 0.0226(9) 0.0248(9) 0.0297(9) 0.0019(7) 0.0016(8) 0.0027(9) C10 0.0198(8) 0.0207(8) 0.0138(7) 0.0017(6) 0.0007(6) 0.0005(8) C11 0.0176(8) 0.0188(7) 0.0158(7) 0.0011(6) 0.0002(7) -0.0003(7) C12 0.0253(9) 0.0225(8) 0.0158(7) -0.0013(6) 0.0008(7) 0.0000(9) C13 0.0325(11) 0.0218(9) 0.0215(8) -0.0051(7) 0.0000(8) -0.0018(9) C14 0.0224(8) 0.0181(8) 0.0264(8) -0.0017(7) 0.0022(8) 0.0004(8) C15 0.0142(8) 0.0182(8) 0.0222(8) 0.0023(6) 0.0005(7) -0.0002(8) C16 0.0146(7) 0.0202(8) 0.0164(7) 0.0005(6) 0.0012(6) 0.0000(7) C17 0.0179(8) 0.0205(8) 0.0238(8) 0.0066(6) 0.0000(7) -0.0008(8) C18 0.0270(11) 0.0352(12) 0.0305(10) 0.0109(9) 0.0090(8) -0.0006(9) C19 0.0486(14) 0.0221(9) 0.0353(11) 0.0089(8) -0.0018(11) -0.0029(11) C20 0.0248(10) 0.0367(12) 0.0342(11) 0.0131(9) -0.0079(8) -0.0018(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 Cl1 2.2327(6) . ? Ti1 Cl2 2.2769(6) . ? Ti1 Cl3 2.2327(6) . ? Ti1 O1 1.8152(13) . ? Ti1 N1 2.1478(14) . ? O1 C16 1.331(2) . ? N1 C1 1.459(2) . ? N1 C10 1.305(2) . ? C1 C2 1.392(3) . ? C1 C6 1.395(3) . ? C2 C3 1.394(3) . ? C2 C7 1.509(3) . ? C3 C4 1.388(3) . ? C4 C5 1.387(3) . ? C4 C8 1.500(2) . ? C5 C6 1.394(3) . ? C6 C9 1.497(3) . ? C10 C11 1.428(2) . ? C11 C12 1.404(2) . ? C11 C16 1.406(2) . ? C12 C13 1.375(3) . ? C13 C14 1.397(3) . ? C14 C15 1.394(2) . ? C15 C16 1.403(2) . ? C15 C17 1.527(2) . ? C17 C18 1.534(3) . ? C17 C19 1.528(3) . ? C17 C20 1.534(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Ti1 Cl2 93.42(2) . . ? Cl1 Ti1 Cl3 113.93(3) . . ? Cl1 Ti1 O1 92.45(5) . . ? Cl1 Ti1 N1 128.80(5) . . ? Cl2 Ti1 Cl3 94.91(2) . . ? Cl2 Ti1 O1 167.49(4) . . ? Cl2 Ti1 N1 86.62(4) . . ? Cl3 Ti1 O1 92.79(5) . . ? Cl3 Ti1 N1 117.07(5) . . ? O1 Ti1 N1 81.10(5) . . ? Ti1 O1 C16 147.61(11) . . ? Ti1 N1 C1 121.90(10) . . ? Ti1 N1 C10 125.39(12) . . ? C1 N1 C10 112.60(14) . . ? N1 C1 C2 118.71(17) . . ? N1 C1 C6 118.85(17) . . ? C2 C1 C6 122.43(16) . . ? C1 C2 C3 117.67(17) . . ? C1 C2 C7 121.71(17) . . ? C3 C2 C7 120.61(18) . . ? C2 C3 C4 121.73(18) . . ? C3 C4 C5 118.73(16) . . ? C3 C4 C8 120.60(19) . . ? C5 C4 C8 120.67(19) . . ? C4 C5 C6 121.79(17) . . ? C1 C6 C5 117.59(17) . . ? C1 C6 C9 121.35(17) . . ? C5 C6 C9 121.05(18) . . ? N1 C10 C11 128.27(15) . . ? C10 C11 C12 118.90(15) . . ? C10 C11 C16 121.33(15) . . ? C12 C11 C16 119.77(15) . . ? C11 C12 C13 118.94(16) . . ? C12 C13 C14 120.14(17) . . ? C13 C14 C15 123.36(16) . . ? C14 C15 C16 115.43(16) . . ? C14 C15 C17 122.80(15) . . ? C16 C15 C17 121.76(15) . . ? O1 C16 C11 115.65(15) . . ? O1 C16 C15 122.00(15) . . ? C11 C16 C15 122.35(15) . . ? C15 C17 C18 109.75(16) . . ? C15 C17 C19 111.14(15) . . ? C15 C17 C20 110.17(16) . . ? C18 C17 C19 107.68(18) . . ? C18 C17 C20 109.74(17) . . ? C19 C17 C20 108.31(18) . . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.475 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.093 # #===END # data_dalep4 _database_code_depnum_ccdc_archive 'CCDC 250157' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Complex 5c' _chemical_formula_moiety 'C24 H32 Cl3 N O2 Ti' _chemical_formula_structural '[TiCl3(thf)(OC6H3tBu-6,-CHNMes-2)]' _chemical_formula_sum 'C24 H32 Cl3 N O2 Ti' _chemical_formula_weight 520.76 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' N N 0.0061 0.0033 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.9120(16) _cell_length_b 10.469(2) _cell_length_c 15.803(3) _cell_angle_alpha 91.76(3) _cell_angle_beta 102.27(3) _cell_angle_gamma 94.09(3) _cell_volume 1274.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour dark_red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 0.671 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-Axis-IIc' _diffrn_measurement_method 'image-plate oscillation photos' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7307 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.0617 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.35 _reflns_number_total 4351 _reflns_number_gt 3830 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC R-Axis-II control software' _computing_cell_refinement 'DENZO (Otwinowski and Minor, 1985)' _computing_data_reduction 'DENZO, Scalepack (Otwinowski and Minor, 1985)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (SHELXTL, v.5, 1994)' _computing_publication_material 'XL (SHELXTL, v.5, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0545P)^2^+0.1585P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4351 _refine_ls_number_parameters 283 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.1067 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti 0.06051(4) 0.73852(3) 0.25009(2) 0.02454(12) Uani 1 d . . . Cl1 Cl -0.09258(6) 0.76631(5) 0.11036(3) 0.03170(14) Uani 1 d . . . Cl2 Cl -0.17057(6) 0.63882(5) 0.29508(3) 0.03349(15) Uani 1 d . . . Cl3 Cl 0.02999(7) 0.94329(5) 0.29680(3) 0.03396(15) Uani 1 d . . . O1 O 0.21858(16) 0.71572(13) 0.35045(8) 0.0263(3) Uani 1 d . . . O2 O 0.10542(18) 0.54943(13) 0.20407(9) 0.0290(3) Uani 1 d . . . N N 0.3052(2) 0.80176(15) 0.20602(10) 0.0247(3) Uani 1 d . . . C1 C 0.3698(2) 0.77051(18) 0.39927(12) 0.0255(4) Uani 1 d . . . C2 C 0.4871(2) 0.83093(19) 0.35460(13) 0.0278(4) Uani 1 d . . . C3 C 0.6476(3) 0.8883(2) 0.40183(14) 0.0327(5) Uani 1 d . . . H3 H 0.7274 0.9262 0.3728 0.039 Uiso 1 calc R . . C4 C 0.6859(3) 0.8881(2) 0.49124(14) 0.0351(5) Uani 1 d . . . H4 H 0.7901 0.9279 0.5228 0.042 Uiso 1 calc R . . C5 C 0.5672(3) 0.8277(2) 0.53394(13) 0.0338(5) Uani 1 d . . . H5 H 0.5951 0.8290 0.5942 0.041 Uiso 1 calc R . . C6 C 0.4076(3) 0.7650(2) 0.49084(13) 0.0295(4) Uani 1 d . . . C61 C 0.2815(3) 0.6960(2) 0.53991(13) 0.0331(5) Uani 1 d . . . C62 C 0.3585(3) 0.7005(3) 0.63765(15) 0.0499(6) Uani 1 d . . . H62A H 0.3825 0.7881 0.6591 0.075 Uiso 1 calc R . . H62B H 0.4641 0.6581 0.6484 0.075 Uiso 1 calc R . . H62C H 0.2771 0.6580 0.6667 0.075 Uiso 1 calc R . . C63 C 0.2443(3) 0.5538(2) 0.50804(15) 0.0420(5) Uani 1 d . . . H63A H 0.1954 0.5484 0.4469 0.063 Uiso 1 calc R . . H63B H 0.1638 0.5123 0.5381 0.063 Uiso 1 calc R . . H63C H 0.3506 0.5121 0.5193 0.063 Uiso 1 calc R . . C64 C 0.1087(3) 0.7607(2) 0.52563(15) 0.0375(5) Uani 1 d . . . H64A H 0.1311 0.8490 0.5458 0.056 Uiso 1 calc R . . H64B H 0.0324 0.7176 0.5573 0.056 Uiso 1 calc R . . H64C H 0.0553 0.7557 0.4650 0.056 Uiso 1 calc R . . C10 C 0.4519(3) 0.83308(18) 0.26069(13) 0.0273(4) Uani 1 d . . . H10 H 0.5451 0.8600 0.2366 0.033 Uiso 1 calc R . . C11 C 0.3157(2) 0.81274(18) 0.11518(12) 0.0246(4) Uani 1 d . . . C12 C 0.2659(3) 0.92530(19) 0.07303(14) 0.0301(4) Uani 1 d . . . C13 C 0.2781(3) 0.9346(2) -0.01340(14) 0.0340(5) Uani 1 d . . . H13 H 0.2469 1.0088 -0.0416 0.041 Uiso 1 calc R . . C14 C 0.3352(3) 0.8370(2) -0.05861(13) 0.0340(5) Uani 1 d . . . C15 C 0.3874(3) 0.7289(2) -0.01487(13) 0.0315(4) Uani 1 d . . . H15 H 0.4285 0.6636 -0.0443 0.038 Uiso 1 calc R . . C16 C 0.3804(2) 0.71454(19) 0.07255(13) 0.0268(4) Uani 1 d . . . C121 C 0.2049(3) 1.0359(2) 0.11859(16) 0.0382(5) Uani 1 d . . . H12A H 0.2210 1.1129 0.0888 0.057 Uiso 1 calc R . . H12B H 0.2708 1.0463 0.1772 0.057 Uiso 1 calc R . . H12C H 0.0842 1.0190 0.1188 0.057 Uiso 1 calc R . . C141 C 0.3401(3) 0.8489(3) -0.15335(15) 0.0488(6) Uani 1 d . . . H14A H 0.2290 0.8707 -0.1849 0.073 Uiso 1 calc R . . H14B H 0.3668 0.7688 -0.1765 0.073 Uiso 1 calc R . . H14C H 0.4275 0.9148 -0.1587 0.073 Uiso 1 calc R . . C161 C 0.4493(3) 0.5973(2) 0.11649(14) 0.0340(5) Uani 1 d . . . H16A H 0.5739 0.6054 0.1282 0.051 Uiso 1 calc R . . H16B H 0.4068 0.5225 0.0793 0.051 Uiso 1 calc R . . H16C H 0.4113 0.5893 0.1700 0.051 Uiso 1 calc R . . C21 C 0.1729(4) 0.4558(2) 0.26667(15) 0.0462(6) Uani 1 d . . . H21A H 0.1023 0.4467 0.3097 0.055 Uiso 1 calc R . . H21B H 0.2912 0.4825 0.2961 0.055 Uiso 1 calc R . . C22 C 0.1661(6) 0.3311(3) 0.2157(2) 0.0919(14) Uani 1 d . . . H22A H 0.2824 0.3050 0.2189 0.110 Uiso 1 calc R . . H22B H 0.0999 0.2644 0.2388 0.110 Uiso 1 calc R . . C23 C 0.0813(3) 0.3523(2) 0.12394(16) 0.0448(6) Uani 1 d . . . H23A H -0.0057 0.2830 0.1007 0.054 Uiso 1 calc R . . H23B H 0.1663 0.3584 0.0878 0.054 Uiso 1 calc R . . C24 C -0.0003(4) 0.4763(2) 0.12839(17) 0.0541(7) Uani 1 d . . . H24A H -0.0004 0.5225 0.0761 0.065 Uiso 1 calc R . . H24B H -0.1191 0.4610 0.1350 0.065 Uiso 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 Ti 0.0241(2) 0.0271(2) 0.0217(2) -0.00223(14) 0.00309(14) 0.00429(15) Cl1 0.0325(3) 0.0340(3) 0.0258(3) 0.00186(19) -0.0008(2) 0.0045(2) Cl2 0.0275(3) 0.0414(3) 0.0311(3) 0.0022(2) 0.0062(2) 0.0006(2) Cl3 0.0382(3) 0.0312(3) 0.0343(3) -0.0055(2) 0.0113(2) 0.0077(2) O1 0.0243(7) 0.0311(7) 0.0226(7) -0.0020(5) 0.0033(5) 0.0021(6) O2 0.0327(7) 0.0272(7) 0.0239(7) -0.0048(5) -0.0008(6) 0.0047(6) N 0.0280(8) 0.0238(8) 0.0225(8) -0.0029(6) 0.0054(7) 0.0055(7) C1 0.0240(9) 0.0275(9) 0.0247(10) -0.0045(8) 0.0038(8) 0.0060(8) C2 0.0264(9) 0.0307(10) 0.0257(10) -0.0058(8) 0.0046(8) 0.0053(8) C3 0.0263(10) 0.0398(11) 0.0316(11) -0.0066(9) 0.0074(8) 0.0013(9) C4 0.0245(10) 0.0445(12) 0.0331(11) -0.0102(9) 0.0005(9) 0.0027(9) C5 0.0314(10) 0.0458(12) 0.0223(10) -0.0047(9) 0.0010(8) 0.0074(9) C6 0.0285(10) 0.0355(11) 0.0238(10) -0.0030(8) 0.0030(8) 0.0076(9) C61 0.0324(11) 0.0434(12) 0.0230(10) -0.0007(9) 0.0055(8) 0.0030(9) C62 0.0486(14) 0.0726(18) 0.0260(12) 0.0062(11) 0.0049(10) -0.0033(13) C63 0.0482(13) 0.0406(13) 0.0395(13) 0.0048(10) 0.0147(11) 0.0031(11) C64 0.0346(11) 0.0483(13) 0.0318(11) -0.0010(9) 0.0120(9) 0.0038(10) C10 0.0285(10) 0.0261(9) 0.0287(10) -0.0037(8) 0.0092(8) 0.0054(8) C11 0.0245(9) 0.0275(9) 0.0212(9) -0.0015(7) 0.0044(7) 0.0009(8) C12 0.0303(10) 0.0277(10) 0.0320(11) 0.0001(8) 0.0061(8) 0.0033(8) C13 0.0334(10) 0.0356(11) 0.0324(11) 0.0080(9) 0.0050(9) 0.0031(9) C14 0.0301(10) 0.0456(12) 0.0250(10) 0.0003(9) 0.0045(8) -0.0006(9) C15 0.0287(10) 0.0387(11) 0.0261(10) -0.0084(8) 0.0050(8) 0.0034(9) C16 0.0239(9) 0.0286(10) 0.0268(10) -0.0038(8) 0.0036(8) 0.0026(8) C121 0.0446(12) 0.0262(10) 0.0467(13) 0.0010(9) 0.0142(10) 0.0087(9) C141 0.0472(14) 0.0709(17) 0.0286(12) 0.0061(11) 0.0089(10) 0.0023(13) C161 0.0345(11) 0.0330(11) 0.0359(12) -0.0019(9) 0.0085(9) 0.0114(9) C21 0.0698(16) 0.0325(11) 0.0330(12) -0.0002(9) -0.0007(11) 0.0188(12) C22 0.167(4) 0.0352(14) 0.0546(19) -0.0131(13) -0.024(2) 0.0303(19) C23 0.0475(13) 0.0368(12) 0.0450(14) -0.0135(10) 0.0000(11) 0.0063(10) C24 0.0619(16) 0.0419(13) 0.0434(14) -0.0218(11) -0.0227(13) 0.0155(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti O1 1.8328(15) . ? Ti O2 2.1669(14) . ? Ti N 2.2558(17) . ? Ti Cl3 2.2914(8) . ? Ti Cl2 2.2943(9) . ? Ti Cl1 2.3196(9) . ? O1 C1 1.356(2) . ? O2 C21 1.461(3) . ? O2 C24 1.464(3) . ? N C10 1.305(3) . ? N C11 1.463(2) . ? C1 C2 1.408(3) . ? C1 C6 1.418(3) . ? C2 C3 1.410(3) . ? C2 C10 1.452(3) . ? C3 C4 1.381(3) . ? C3 H3 0.9300 . ? C4 C5 1.396(3) . ? C4 H4 0.9300 . ? C5 C6 1.406(3) . ? C5 H5 0.9300 . ? C6 C61 1.542(3) . ? C61 C62 1.533(3) . ? C61 C63 1.544(3) . ? C61 C64 1.546(3) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C10 H10 0.9300 . ? C11 C16 1.397(3) . ? C11 C12 1.411(3) . ? C12 C13 1.396(3) . ? C12 C121 1.506(3) . ? C13 C14 1.385(3) . ? C13 H13 0.9300 . ? C14 C15 1.387(3) . ? C14 C141 1.515(3) . ? C15 C16 1.406(3) . ? C15 H15 0.9300 . ? C16 C161 1.508(3) . ? C121 H12A 0.9600 . ? C121 H12B 0.9600 . ? C121 H12C 0.9600 . ? C141 H14A 0.9600 . ? C141 H14B 0.9600 . ? C141 H14C 0.9600 . ? C161 H16A 0.9600 . ? C161 H16B 0.9600 . ? C161 H16C 0.9600 . ? C21 C22 1.504(3) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.493(4) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.497(3) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? 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 Ti O2 88.40(6) . . ? O1 Ti N 81.27(6) . . ? O2 Ti N 84.55(6) . . ? O1 Ti Cl3 90.72(5) . . ? O2 Ti Cl3 176.26(4) . . ? N Ti Cl3 91.73(5) . . ? O1 Ti Cl2 94.97(5) . . ? O2 Ti Cl2 85.95(5) . . ? N Ti Cl2 169.86(4) . . ? Cl3 Ti Cl2 97.75(3) . . ? O1 Ti Cl1 168.64(5) . . ? O2 Ti Cl1 86.89(5) . . ? N Ti Cl1 87.99(5) . . ? Cl3 Ti Cl1 93.32(4) . . ? Cl2 Ti Cl1 95.00(3) . . ? C1 O1 Ti 140.64(13) . . ? C21 O2 C24 106.57(17) . . ? C21 O2 Ti 119.47(12) . . ? C24 O2 Ti 125.90(13) . . ? C10 N C11 113.68(16) . . ? C10 N Ti 122.19(13) . . ? C11 N Ti 124.13(12) . . ? O1 C1 C2 116.83(17) . . ? O1 C1 C6 121.07(18) . . ? C2 C1 C6 122.09(18) . . ? C1 C2 C3 119.42(19) . . ? C1 C2 C10 122.38(18) . . ? C3 C2 C10 118.17(19) . . ? C4 C3 C2 119.9(2) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 119.5(2) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C4 C5 C6 123.59(19) . . ? C4 C5 H5 118.2 . . ? C6 C5 H5 118.2 . . ? C5 C6 C1 115.44(19) . . ? C5 C6 C61 122.27(18) . . ? C1 C6 C61 122.29(18) . . ? C62 C61 C6 111.11(18) . . ? C62 C61 C63 107.90(19) . . ? C6 C61 C63 110.25(17) . . ? C62 C61 C64 107.89(18) . . ? C6 C61 C64 110.44(17) . . ? C63 C61 C64 109.17(18) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? N C10 C2 127.82(19) . . ? N C10 H10 116.1 . . ? C2 C10 H10 116.1 . . ? C16 C11 C12 121.05(18) . . ? C16 C11 N 119.89(17) . . ? C12 C11 N 119.02(17) . . ? C13 C12 C11 118.25(19) . . ? C13 C12 C121 119.35(19) . . ? C11 C12 C121 122.38(19) . . ? C14 C13 C12 122.2(2) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? C13 C14 C15 118.28(19) . . ? C13 C14 C141 120.5(2) . . ? C15 C14 C141 121.3(2) . . ? C14 C15 C16 122.22(19) . . ? C14 C15 H15 118.9 . . ? C16 C15 H15 118.9 . . ? C11 C16 C15 117.96(19) . . ? C11 C16 C161 123.31(18) . . ? C15 C16 C161 118.68(18) . . ? C12 C121 H12A 109.5 . . ? C12 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? C12 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? C14 C141 H14A 109.5 . . ? C14 C141 H14B 109.5 . . ? H14A C141 H14B 109.5 . . ? C14 C141 H14C 109.5 . . ? H14A C141 H14C 109.5 . . ? H14B C141 H14C 109.5 . . ? C16 C161 H16A 109.5 . . ? C16 C161 H16B 109.5 . . ? H16A C161 H16B 109.5 . . ? C16 C161 H16C 109.5 . . ? H16A C161 H16C 109.5 . . ? H16B C161 H16C 109.5 . . ? O2 C21 C22 106.32(19) . . ? O2 C21 H21A 110.5 . . ? C22 C21 H21A 110.5 . . ? O2 C21 H21B 110.5 . . ? C22 C21 H21B 110.5 . . ? H21A C21 H21B 108.7 . . ? C23 C22 C21 107.3(2) . . ? C23 C22 H22A 110.2 . . ? C21 C22 H22A 110.2 . . ? C23 C22 H22B 110.2 . . ? C21 C22 H22B 110.2 . . ? H22A C22 H22B 108.5 . . ? C22 C23 C24 104.5(2) . . ? C22 C23 H23A 110.8 . . ? C24 C23 H23A 110.8 . . ? C22 C23 H23B 110.8 . . ? C24 C23 H23B 110.8 . . ? H23A C23 H23B 108.9 . . ? O2 C24 C23 105.82(18) . . ? O2 C24 H24A 110.6 . . ? C23 C24 H24A 110.6 . . ? O2 C24 H24B 110.6 . . ? C23 C24 H24B 110.6 . . ? H24A C24 H24B 108.7 . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 0.336 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.057 # #===END # data_03src0743 _database_code_depnum_ccdc_archive 'CCDC 250158' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Complex 5e' _chemical_melting_point ? _chemical_formula_moiety 'C21 H21 Cl3 F5 N O2 Ti' _chemical_formula_structural '[TiCl3(thf)(OC6H3tBu-6,-CHNC6F5-2)]' _chemical_formula_sum 'C21 H21 Cl3 F5 N O2 Ti' _chemical_formula_weight 568.64 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' N N 0.0061 0.0033 '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' 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 7.2176(2) _cell_length_b 34.4138(9) _cell_length_c 9.3904(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.5740(10) _cell_angle_gamma 90.00 _cell_volume 2317.10(10) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 18362 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.630 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 0.775 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8358 _exptl_absorpt_correction_T_max 0.9847 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 Nonius Kappa CCD Area detector' _diffrn_measurement_method '\f and \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean '9.091 pixels mm^1^' _diffrn_standards_decay_% ? _diffrn_reflns_number 25995 _diffrn_reflns_av_R_equivalents 0.0864 _diffrn_reflns_av_sigmaI/netI 0.0820 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5294 _reflns_number_gt 3410 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO (Otwinowski and MInor, 1997)' _computing_data_reduction 'DENZO, COLLECT, MAXUS (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 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^)+(0.0317P)^2^+0.6385P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0015(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5294 _refine_ls_number_parameters 302 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0915 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.0915 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _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 C1 C 0.2381(3) 0.11079(8) 0.3496(3) 0.0209(6) Uani 1 1 d . . . C2 C 0.2159(4) 0.12887(8) 0.2183(3) 0.0243(7) Uani 1 1 d . . . C3 C 0.1355(4) 0.11074(9) 0.0958(3) 0.0321(8) Uani 1 1 d . . . C4 C 0.0672(4) 0.07372(10) 0.1063(3) 0.0341(8) Uani 1 1 d . . . C5 C 0.0856(4) 0.05508(9) 0.2356(4) 0.0295(7) Uani 1 1 d . . . C6 C 0.1716(4) 0.07306(8) 0.3559(3) 0.0238(7) Uani 1 1 d . . . C7 C 0.2337(4) 0.15923(8) 0.5159(3) 0.0187(6) Uani 1 1 d . . . H7 H 0.1148 0.1636 0.4637 0.022 Uiso 1 1 calc R . . C8 C 0.2871(3) 0.18514(7) 0.6324(3) 0.0178(6) Uani 1 1 d . . . C9 C 0.1686(4) 0.21643(7) 0.6533(3) 0.0206(6) Uani 1 1 d . . . H9 H 0.0580 0.2204 0.5898 0.025 Uiso 1 1 calc R . . C10 C 0.2141(4) 0.24124(8) 0.7666(3) 0.0233(6) Uani 1 1 d . . . H10 H 0.1381 0.2632 0.7794 0.028 Uiso 1 1 calc R . . C11 C 0.3723(4) 0.23407(8) 0.8629(3) 0.0221(6) Uani 1 1 d . . . H11 H 0.3994 0.2514 0.9413 0.026 Uiso 1 1 calc R . . C12 C 0.4923(4) 0.20303(7) 0.8506(3) 0.0187(6) Uani 1 1 d . . . C13 C 0.4495(3) 0.17948(7) 0.7291(3) 0.0166(6) Uani 1 1 d . . . C14 C 0.6640(4) 0.19598(8) 0.9585(3) 0.0214(6) Uani 1 1 d . . . C15 C 0.8393(4) 0.20492(8) 0.8864(3) 0.0252(7) Uani 1 1 d . . . H15A H 0.8440 0.1877 0.8037 0.038 Uiso 1 1 calc R . . H15B H 0.9503 0.2007 0.9552 0.038 Uiso 1 1 calc R . . H15C H 0.8359 0.2320 0.8544 0.038 Uiso 1 1 calc R . . C16 C 0.6712(4) 0.15391(8) 1.0145(3) 0.0247(7) Uani 1 1 d . . . H16A H 0.5512 0.1472 1.0474 0.037 Uiso 1 1 calc R . . H16B H 0.7704 0.1515 1.0945 0.037 Uiso 1 1 calc R . . H16C H 0.6966 0.1362 0.9373 0.037 Uiso 1 1 calc R . . C17 C 0.6653(4) 0.22292(8) 1.0884(3) 0.0284(7) Uani 1 1 d . . . H17A H 0.6635 0.2500 1.0564 0.043 Uiso 1 1 calc R . . H17B H 0.7782 0.2182 1.1546 0.043 Uiso 1 1 calc R . . H17C H 0.5550 0.2178 1.1375 0.043 Uiso 1 1 calc R . . C18 C 0.6109(4) 0.03349(8) 0.6714(4) 0.0351(8) Uani 1 1 d . . . H18A H 0.7482 0.0341 0.6726 0.042 Uiso 1 1 calc R . . H18B H 0.5566 0.0187 0.5864 0.042 Uiso 1 1 calc R . . C19 C 0.5573(4) 0.01582(9) 0.8058(4) 0.0377(8) Uani 1 1 d . . . H19A H 0.6506 0.0218 0.8887 0.045 Uiso 1 1 calc R . . H19B H 0.5436 -0.0127 0.7964 0.045 Uiso 1 1 calc R . . C20 C 0.3730(4) 0.03494(9) 0.8215(4) 0.0446(9) Uani 1 1 d . . . H20A H 0.2706 0.0226 0.7580 0.054 Uiso 1 1 calc R . . H20B H 0.3436 0.0336 0.9218 0.054 Uiso 1 1 calc R . . C21 C 0.4036(4) 0.07620(8) 0.7773(3) 0.0271(7) Uani 1 1 d . . . H21A H 0.2851 0.0883 0.7357 0.033 Uiso 1 1 calc R . . H21B H 0.4575 0.0920 0.8601 0.033 Uiso 1 1 calc R . . N1 N 0.3295(3) 0.13042(6) 0.4733(2) 0.0187(5) Uani 1 1 d . . . O1 O 0.5617(2) 0.15016(5) 0.70045(19) 0.0183(4) Uani 1 1 d . . . O2 O 0.5348(2) 0.07286(5) 0.6697(2) 0.0225(4) Uani 1 1 d . . . F1 F 0.2770(2) 0.16563(5) 0.20592(17) 0.0311(4) Uani 1 1 d . . . F2 F 0.1229(3) 0.12878(6) -0.03054(19) 0.0442(5) Uani 1 1 d . . . F3 F -0.0164(3) 0.05567(6) -0.0108(2) 0.0504(6) Uani 1 1 d . . . F4 F 0.0195(2) 0.01892(5) 0.2458(2) 0.0433(5) Uani 1 1 d . . . F5 F 0.1932(2) 0.05363(4) 0.47989(18) 0.0317(4) Uani 1 1 d . . . Cl1 Cl 0.63686(9) 0.07814(2) 0.36360(8) 0.02882(19) Uani 1 1 d . . . Cl2 Cl 0.92246(9) 0.10675(2) 0.65712(8) 0.02579(18) Uani 1 1 d . . . Cl3 Cl 0.70850(9) 0.17256(2) 0.42886(8) 0.02631(18) Uani 1 1 d . . . Ti1 Ti 0.63001(6) 0.119965(14) 0.55626(5) 0.01816(13) 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 C1 0.0141(13) 0.0239(15) 0.0240(16) -0.0067(13) -0.0003(11) 0.0041(12) C2 0.0194(14) 0.0272(17) 0.0258(17) -0.0051(13) 0.0002(12) 0.0011(13) C3 0.0292(17) 0.040(2) 0.0249(18) -0.0048(15) -0.0054(13) 0.0105(15) C4 0.0244(16) 0.044(2) 0.0318(19) -0.0177(16) -0.0075(14) 0.0058(15) C5 0.0195(15) 0.0256(17) 0.043(2) -0.0130(15) 0.0002(14) -0.0006(13) C6 0.0187(14) 0.0251(16) 0.0267(17) -0.0032(14) -0.0017(12) 0.0021(12) C7 0.0145(13) 0.0222(15) 0.0189(15) 0.0049(12) -0.0001(11) 0.0002(11) C8 0.0190(13) 0.0164(14) 0.0191(15) 0.0001(12) 0.0063(11) -0.0021(11) C9 0.0173(13) 0.0199(15) 0.0252(16) 0.0031(12) 0.0046(11) -0.0005(12) C10 0.0197(14) 0.0182(14) 0.0339(18) -0.0023(13) 0.0108(13) 0.0010(12) C11 0.0258(15) 0.0203(15) 0.0209(16) -0.0053(12) 0.0064(12) -0.0057(12) C12 0.0217(14) 0.0174(14) 0.0182(15) -0.0007(12) 0.0075(11) -0.0045(12) C13 0.0191(13) 0.0134(13) 0.0188(15) 0.0040(11) 0.0082(11) -0.0015(11) C14 0.0231(14) 0.0234(15) 0.0173(15) -0.0031(12) 0.0014(11) -0.0033(12) C15 0.0198(14) 0.0286(16) 0.0265(17) 0.0009(13) -0.0006(12) -0.0025(12) C16 0.0289(16) 0.0257(16) 0.0194(16) -0.0013(13) 0.0017(12) -0.0002(13) C17 0.0355(17) 0.0263(16) 0.0226(17) -0.0024(13) -0.0001(13) -0.0010(14) C18 0.0445(19) 0.0192(16) 0.042(2) 0.0021(15) 0.0063(16) 0.0096(14) C19 0.0411(19) 0.0215(16) 0.050(2) 0.0076(15) 0.0013(16) -0.0036(15) C20 0.0386(19) 0.038(2) 0.059(2) 0.0151(18) 0.0105(17) -0.0071(16) C21 0.0253(15) 0.0286(16) 0.0287(17) 0.0031(14) 0.0080(13) -0.0001(13) N1 0.0171(11) 0.0199(12) 0.0186(13) -0.0004(10) -0.0001(9) 0.0007(10) O1 0.0175(9) 0.0197(10) 0.0177(10) -0.0009(8) 0.0022(7) 0.0026(8) O2 0.0230(10) 0.0183(10) 0.0270(11) 0.0008(9) 0.0063(8) 0.0029(8) F1 0.0355(9) 0.0314(10) 0.0256(10) 0.0017(8) 0.0000(7) 0.0006(8) F2 0.0487(11) 0.0598(13) 0.0213(10) -0.0052(9) -0.0082(8) 0.0086(10) F3 0.0449(11) 0.0572(13) 0.0444(13) -0.0287(10) -0.0161(9) 0.0015(10) F4 0.0343(10) 0.0279(10) 0.0653(14) -0.0172(10) -0.0050(9) -0.0054(8) F5 0.0338(9) 0.0240(9) 0.0365(11) -0.0004(8) 0.0004(8) -0.0030(7) Cl1 0.0249(4) 0.0349(4) 0.0264(4) -0.0125(3) 0.0016(3) 0.0050(3) Cl2 0.0179(3) 0.0333(4) 0.0255(4) -0.0010(3) -0.0008(3) 0.0041(3) Cl3 0.0253(4) 0.0294(4) 0.0240(4) 0.0054(3) 0.0021(3) -0.0023(3) Ti1 0.0162(2) 0.0201(3) 0.0180(3) -0.0020(2) 0.00122(19) 0.0014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.373(4) . ? C1 C6 1.388(4) . ? C1 N1 1.437(3) . ? C2 F1 1.349(3) . ? C2 C3 1.377(4) . ? C3 F2 1.333(4) . ? C3 C4 1.374(4) . ? C4 F3 1.344(3) . ? C4 C5 1.366(4) . ? C5 F4 1.340(3) . ? C5 C6 1.372(4) . ? C6 F5 1.337(3) . ? C7 N1 1.297(3) . ? C7 C8 1.430(4) . ? C7 H7 0.9500 . ? C8 C9 1.403(4) . ? C8 C13 1.411(4) . ? C9 C10 1.375(4) . ? C9 H9 0.9500 . ? C10 C11 1.394(4) . ? C10 H10 0.9500 . ? C11 C12 1.388(4) . ? C11 H11 0.9500 . ? C12 C13 1.405(4) . ? C12 C14 1.528(4) . ? C13 O1 1.340(3) . ? C14 C17 1.532(4) . ? C14 C15 1.533(4) . ? C14 C16 1.540(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 O2 1.462(3) . ? C18 C19 1.492(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.506(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.503(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 O2 1.466(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? N1 Ti1 2.248(2) . ? O1 Ti1 1.8191(18) . ? O2 Ti1 2.0981(19) . ? Cl1 Ti1 2.3169(8) . ? Cl2 Ti1 2.2587(8) . ? Cl3 Ti1 2.2768(8) . ? 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 C2 C1 C6 117.2(3) . . ? C2 C1 N1 120.5(2) . . ? C6 C1 N1 122.3(3) . . ? F1 C2 C1 119.8(2) . . ? F1 C2 C3 117.6(3) . . ? C1 C2 C3 122.6(3) . . ? F2 C3 C4 120.5(3) . . ? F2 C3 C2 120.8(3) . . ? C4 C3 C2 118.7(3) . . ? F3 C4 C5 119.9(3) . . ? F3 C4 C3 120.1(3) . . ? C5 C4 C3 120.0(3) . . ? F4 C5 C4 120.0(3) . . ? F4 C5 C6 119.4(3) . . ? C4 C5 C6 120.6(3) . . ? F5 C6 C5 119.2(3) . . ? F5 C6 C1 119.9(2) . . ? C5 C6 C1 120.9(3) . . ? N1 C7 C8 127.2(2) . . ? N1 C7 H7 116.4 . . ? C8 C7 H7 116.4 . . ? C9 C8 C13 119.4(2) . . ? C9 C8 C7 118.0(2) . . ? C13 C8 C7 122.5(2) . . ? C10 C9 C8 119.3(3) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C9 C10 C11 119.8(3) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C12 C11 C10 123.7(3) . . ? C12 C11 H11 118.2 . . ? C10 C11 H11 118.2 . . ? C11 C12 C13 115.5(2) . . ? C11 C12 C14 122.3(2) . . ? C13 C12 C14 122.2(2) . . ? O1 C13 C12 121.0(2) . . ? O1 C13 C8 116.8(2) . . ? C12 C13 C8 122.1(2) . . ? C12 C14 C17 111.3(2) . . ? C12 C14 C15 108.9(2) . . ? C17 C14 C15 107.5(2) . . ? C12 C14 C16 111.7(2) . . ? C17 C14 C16 107.5(2) . . ? C15 C14 C16 110.0(2) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O2 C18 C19 104.7(2) . . ? O2 C18 H18A 110.8 . . ? C19 C18 H18A 110.8 . . ? O2 C18 H18B 110.8 . . ? C19 C18 H18B 110.8 . . ? H18A C18 H18B 108.9 . . ? C18 C19 C20 102.8(3) . . ? C18 C19 H19A 111.2 . . ? C20 C19 H19A 111.2 . . ? C18 C19 H19B 111.2 . . ? C20 C19 H19B 111.2 . . ? H19A C19 H19B 109.1 . . ? C21 C20 C19 103.1(2) . . ? C21 C20 H20A 111.1 . . ? C19 C20 H20A 111.1 . . ? C21 C20 H20B 111.1 . . ? C19 C20 H20B 111.1 . . ? H20A C20 H20B 109.1 . . ? O2 C21 C20 104.1(2) . . ? O2 C21 H21A 110.9 . . ? C20 C21 H21A 110.9 . . ? O2 C21 H21B 110.9 . . ? C20 C21 H21B 110.9 . . ? H21A C21 H21B 109.0 . . ? C7 N1 C1 113.4(2) . . ? C7 N1 Ti1 122.87(17) . . ? C1 N1 Ti1 122.68(16) . . ? C13 O1 Ti1 143.21(17) . . ? C18 O2 C21 109.7(2) . . ? C18 O2 Ti1 125.26(17) . . ? C21 O2 Ti1 124.35(16) . . ? O1 Ti1 O2 86.04(8) . . ? O1 Ti1 N1 80.41(8) . . ? O2 Ti1 N1 86.59(8) . . ? O1 Ti1 Cl2 97.06(6) . . ? O2 Ti1 Cl2 88.63(5) . . ? N1 Ti1 Cl2 174.73(6) . . ? O1 Ti1 Cl3 92.40(6) . . ? O2 Ti1 Cl3 175.31(6) . . ? N1 Ti1 Cl3 88.80(6) . . ? Cl2 Ti1 Cl3 95.95(3) . . ? O1 Ti1 Cl1 165.45(6) . . ? O2 Ti1 Cl1 87.36(6) . . ? N1 Ti1 Cl1 86.28(6) . . ? Cl2 Ti1 Cl1 95.73(3) . . ? Cl3 Ti1 Cl1 93.14(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.375 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.077 # #===END # data_dale2 _database_code_depnum_ccdc_archive 'CCDC 250159' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Complex 6b' _chemical_formula_moiety 'C34 H46 Cl3 N O2 Zr' _chemical_formula_structural dalep2 _chemical_formula_sum 'C34 H46 Cl3 N O2 Zr' _chemical_formula_weight 698.29 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' N N 0.0061 0.0033 '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' Zr Zr -2.9673 0.5597 '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 15.200(3) _cell_length_b 16.336(3) _cell_length_c 27.710(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6881(2) _cell_formula_units_Z 8 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2912 _exptl_absorpt_coefficient_mu 0.582 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-Axis-IIc' _diffrn_measurement_method 'image-plate oscillation photos' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10569 _diffrn_reflns_av_R_equivalents 0.0185 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.35 _reflns_number_total 5788 _reflns_number_gt 4580 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'MSC R-Axis-II control software' _computing_cell_refinement 'DENZO (Otwinowski and Minor, 1985)' _computing_data_reduction 'DENZO, Scalepack (Otwinowski and Minor, 1985)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (SHELXTL, v.5, 1994)' _computing_publication_material 'XL (SHELXTL, v.5, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0504P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5788 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0820 _refine_ls_wR_factor_gt 0.0787 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.003 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr Zr 0.363009(16) 0.019428(12) 0.667193(7) 0.02197(8) Uani 1 d . . . Cl1 Cl 0.31963(4) 0.15475(3) 0.69385(2) 0.03025(15) Uani 1 d . . . Cl2 Cl 0.50672(4) 0.01454(3) 0.70554(2) 0.03269(15) Uani 1 d . . . Cl3 Cl 0.41311(5) 0.06636(3) 0.58996(2) 0.03745(17) Uani 1 d . . . O1 O 0.24804(11) -0.01318(8) 0.64246(5) 0.0247(4) Uani 1 d . . . C1 C 0.19602(16) -0.07121(12) 0.62271(7) 0.0216(5) Uani 1 d . . . C2 C 0.23094(16) -0.15100(12) 0.62080(7) 0.0217(5) Uani 1 d . . . C3 C 0.17879(17) -0.21433(12) 0.60163(8) 0.0258(5) Uani 1 d . . . H3 H 0.2006 -0.2675 0.6004 0.031 Uiso 1 calc R . . C4 C 0.09620(17) -0.19795(13) 0.58477(8) 0.0287(6) Uani 1 d . . . H4 H 0.0614 -0.2400 0.5727 0.034 Uiso 1 calc R . . C5 C 0.06425(17) -0.11792(13) 0.58575(8) 0.0285(5) Uani 1 d . . . H5 H 0.0084 -0.1077 0.5735 0.034 Uiso 1 calc R . . C6 C 0.11273(16) -0.05223(13) 0.60442(8) 0.0239(5) Uani 1 d . . . C61 C 0.07754(17) 0.03612(13) 0.60341(8) 0.0295(6) Uani 1 d . . . C62 C 0.13687(19) 0.08776(14) 0.57054(10) 0.0406(7) Uani 1 d . . . H62A H 0.1962 0.0860 0.5823 0.061 Uiso 1 calc R . . H62B H 0.1165 0.1434 0.5704 0.061 Uiso 1 calc R . . H62C H 0.1350 0.0662 0.5383 0.061 Uiso 1 calc R . . C63 C 0.07559(18) 0.07338(15) 0.65452(9) 0.0375(6) Uani 1 d . . . H63A H 0.0384 0.0408 0.6749 0.056 Uiso 1 calc R . . H63B H 0.0530 0.1282 0.6529 0.056 Uiso 1 calc R . . H63C H 0.1341 0.0743 0.6675 0.056 Uiso 1 calc R . . C64 C -0.01649(19) 0.04053(15) 0.58339(10) 0.0429(7) Uani 1 d . . . H64A H -0.0550 0.0086 0.6034 0.064 Uiso 1 calc R . . H64B H -0.0174 0.0193 0.5511 0.064 Uiso 1 calc R . . H64C H -0.0359 0.0964 0.5832 0.064 Uiso 1 calc R . . C10 C 0.31932(16) -0.17087(12) 0.63517(7) 0.0231(5) Uani 1 d . . . H10 H 0.3344 -0.2258 0.6321 0.028 Uiso 1 calc R . . N N 0.38184(13) -0.12369(10) 0.65189(6) 0.0208(4) Uani 1 d . . . C11 C 0.46583(16) -0.16755(12) 0.65669(8) 0.0220(5) Uani 1 d . . . C12 C 0.51821(16) -0.17790(13) 0.61528(8) 0.0252(5) Uani 1 d . . . C121 C 0.49836(17) -0.13752(13) 0.56706(8) 0.0278(5) Uani 1 d . . . H121 H 0.4432 -0.1070 0.5702 0.033 Uiso 1 calc R . . C122 C 0.4869(2) -0.20099(15) 0.52657(9) 0.0417(7) Uani 1 d . . . H12A H 0.4745 -0.1734 0.4968 0.063 Uiso 1 calc R . . H12B H 0.4391 -0.2370 0.5344 0.063 Uiso 1 calc R . . H12C H 0.5401 -0.2322 0.5233 0.063 Uiso 1 calc R . . C123 C 0.57122(19) -0.07690(15) 0.55409(10) 0.0433(7) Uani 1 d . . . H12D H 0.5581 -0.0517 0.5236 0.065 Uiso 1 calc R . . H12E H 0.6263 -0.1054 0.5519 0.065 Uiso 1 calc R . . H12F H 0.5750 -0.0355 0.5786 0.065 Uiso 1 calc R . . C13 C 0.59450(17) -0.22542(13) 0.61968(8) 0.0285(5) Uani 1 d . . . H13 H 0.6299 -0.2336 0.5927 0.034 Uiso 1 calc R . . C14 C 0.61822(18) -0.26034(14) 0.66307(8) 0.0303(6) Uani 1 d . . . H14 H 0.6687 -0.2923 0.6651 0.036 Uiso 1 calc R . . C15 C 0.56666(17) -0.24772(13) 0.70350(8) 0.0291(6) Uani 1 d . . . H15 H 0.5835 -0.2710 0.7327 0.035 Uiso 1 calc R . . C16 C 0.49015(16) -0.20106(12) 0.70156(8) 0.0239(5) Uani 1 d . . . C161 C 0.43416(16) -0.19120(13) 0.74650(8) 0.0258(5) Uani 1 d . . . H161 H 0.3933 -0.1459 0.7407 0.031 Uiso 1 calc R . . C162 C 0.48969(18) -0.16912(15) 0.79097(8) 0.0346(6) Uani 1 d . . . H16A H 0.4520 -0.1634 0.8186 0.052 Uiso 1 calc R . . H16B H 0.5199 -0.1184 0.7853 0.052 Uiso 1 calc R . . H16C H 0.5319 -0.2117 0.7969 0.052 Uiso 1 calc R . . C163 C 0.37942(18) -0.26779(15) 0.75586(9) 0.0378(7) Uani 1 d . . . H16D H 0.3446 -0.2601 0.7844 0.057 Uiso 1 calc R . . H16E H 0.4178 -0.3139 0.7602 0.057 Uiso 1 calc R . . H16F H 0.3414 -0.2776 0.7288 0.057 Uiso 1 calc R . . O2 O 0.30836(11) -0.01848(8) 0.73966(5) 0.0250(4) Uani 1 d . . . C21 C 0.33843(18) 0.01643(14) 0.78581(8) 0.0319(6) Uani 1 d . . . H21A H 0.3523 0.0741 0.7823 0.038 Uiso 1 calc R . . H21B H 0.3901 -0.0121 0.7976 0.038 Uiso 1 calc R . . C22 C 0.2613(2) 0.00435(16) 0.81958(9) 0.0380(6) Uani 1 d . . . H22A H 0.2195 0.0489 0.8168 0.046 Uiso 1 calc R . . H22B H 0.2807 0.0001 0.8528 0.046 Uiso 1 calc R . . C23 C 0.22186(19) -0.07554(14) 0.80212(8) 0.0357(6) Uani 1 d . . . H23A H 0.2561 -0.1222 0.8129 0.043 Uiso 1 calc R . . H23B H 0.1615 -0.0817 0.8130 0.043 Uiso 1 calc R . . C24 C 0.22676(17) -0.06556(14) 0.74783(8) 0.0302(5) Uani 1 d . . . H24A H 0.2297 -0.1184 0.7320 0.036 Uiso 1 calc R . . H24B H 0.1760 -0.0360 0.7358 0.036 Uiso 1 calc R . . C31 C 0.7192(2) 0.15147(18) 0.54018(10) 0.0485(7) Uani 1 d . . . C311 C 0.7525(3) 0.0770(2) 0.51531(14) 0.0777(11) Uani 1 d . . . H31A H 0.8043 0.0904 0.4972 0.117 Uiso 1 calc R . . H31B H 0.7080 0.0565 0.4939 0.117 Uiso 1 calc R . . H31C H 0.7665 0.0359 0.5388 0.117 Uiso 1 calc R . . C32 C 0.7369(2) 0.23113(19) 0.52278(10) 0.0496(8) Uani 1 d . . . H32 H 0.7713 0.2382 0.4953 0.060 Uiso 1 calc R . . C33 C 0.7031(2) 0.2986(2) 0.54655(13) 0.0597(9) Uani 1 d . . . H33 H 0.7145 0.3508 0.5347 0.072 Uiso 1 calc R . . C34 C 0.6534(2) 0.2899(2) 0.58696(13) 0.0632(10) Uani 1 d . . . H34 H 0.6324 0.3356 0.6033 0.076 Uiso 1 calc R . . C35 C 0.6348(2) 0.2135(2) 0.60320(11) 0.0558(8) Uani 1 d . . . H35 H 0.5994 0.2078 0.6304 0.067 Uiso 1 calc R . . C36 C 0.6657(2) 0.14498(19) 0.58131(10) 0.0469(7) Uani 1 d . . . H36 H 0.6514 0.0937 0.5936 0.056 Uiso 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 Zr 0.01952(15) 0.02163(13) 0.02477(12) -0.00098(8) -0.00092(9) -0.00085(9) Cl1 0.0329(4) 0.0240(3) 0.0338(3) -0.0046(2) -0.0036(3) 0.0023(2) Cl2 0.0213(4) 0.0331(3) 0.0437(3) -0.0013(2) -0.0057(3) -0.0014(3) Cl3 0.0471(5) 0.0332(3) 0.0321(3) 0.0049(2) 0.0110(3) 0.0013(3) O1 0.0237(10) 0.0207(7) 0.0298(9) -0.0016(6) -0.0028(7) 0.0006(7) C1 0.0208(15) 0.0242(10) 0.0199(11) -0.0004(8) -0.0017(9) -0.0037(10) C2 0.0213(15) 0.0233(10) 0.0205(11) 0.0006(8) -0.0005(9) -0.0014(10) C3 0.0291(16) 0.0237(10) 0.0247(12) -0.0015(8) 0.0017(10) -0.0024(10) C4 0.0266(16) 0.0322(12) 0.0271(12) -0.0037(9) -0.0028(10) -0.0047(11) C5 0.0197(16) 0.0373(13) 0.0285(12) -0.0013(9) -0.0025(10) 0.0003(11) C6 0.0202(15) 0.0274(11) 0.0240(12) -0.0006(8) 0.0012(9) 0.0023(10) C61 0.0245(17) 0.0291(12) 0.0350(13) -0.0007(9) -0.0052(11) 0.0057(11) C62 0.043(2) 0.0322(13) 0.0465(16) 0.0096(11) -0.0023(13) 0.0040(13) C63 0.0301(19) 0.0380(14) 0.0443(15) -0.0103(11) -0.0035(12) 0.0079(12) C64 0.0327(19) 0.0404(14) 0.0556(18) -0.0062(12) -0.0141(13) 0.0105(13) C10 0.0287(15) 0.0201(10) 0.0205(11) -0.0006(8) 0.0006(9) 0.0004(10) N 0.0188(12) 0.0235(9) 0.0201(9) 0.0013(7) 0.0001(7) 0.0012(8) C11 0.0187(15) 0.0204(10) 0.0269(12) -0.0013(8) -0.0024(9) 0.0004(9) C12 0.0219(16) 0.0256(11) 0.0282(12) -0.0013(9) 0.0009(10) 0.0005(10) C121 0.0247(16) 0.0320(12) 0.0266(12) 0.0023(9) 0.0028(10) 0.0040(11) C122 0.051(2) 0.0457(15) 0.0282(14) -0.0006(11) -0.0045(13) 0.0049(13) C123 0.036(2) 0.0423(14) 0.0512(17) 0.0166(12) 0.0054(13) -0.0010(13) C13 0.0247(16) 0.0311(12) 0.0298(13) -0.0028(9) 0.0026(10) 0.0012(11) C14 0.0232(17) 0.0292(12) 0.0384(14) -0.0004(9) -0.0040(11) 0.0041(10) C15 0.0305(18) 0.0287(11) 0.0281(13) 0.0020(9) -0.0068(10) 0.0020(11) C16 0.0229(15) 0.0239(11) 0.0250(12) 0.0003(8) -0.0030(10) 0.0012(10) C161 0.0254(16) 0.0277(11) 0.0244(12) 0.0018(9) -0.0004(10) 0.0019(10) C162 0.0369(18) 0.0427(14) 0.0241(12) 0.0000(10) -0.0024(11) 0.0010(12) C163 0.0359(19) 0.0434(15) 0.0341(14) -0.0008(11) 0.0043(12) -0.0064(12) O2 0.0229(11) 0.0281(8) 0.0242(8) -0.0019(6) 0.0000(7) -0.0047(7) C21 0.0347(18) 0.0351(13) 0.0259(13) -0.0046(9) -0.0035(11) -0.0041(11) C22 0.0356(19) 0.0493(14) 0.0292(13) -0.0039(11) 0.0013(11) 0.0038(13) C23 0.0265(17) 0.0456(14) 0.0350(14) 0.0078(10) 0.0051(11) 0.0021(12) C24 0.0196(15) 0.0357(12) 0.0353(13) 0.0014(10) 0.0034(11) -0.0068(11) C31 0.035(2) 0.0671(18) 0.0432(16) -0.0113(13) -0.0095(14) 0.0008(15) C311 0.065(3) 0.089(2) 0.080(3) -0.027(2) 0.004(2) 0.009(2) C32 0.034(2) 0.082(2) 0.0337(15) 0.0055(14) -0.0044(13) -0.0128(16) C33 0.043(2) 0.065(2) 0.071(2) 0.0017(16) -0.0279(18) -0.0046(17) C34 0.044(3) 0.085(2) 0.060(2) -0.0170(18) -0.0166(17) 0.0151(19) C35 0.045(2) 0.080(2) 0.0420(18) -0.0043(15) -0.0042(15) -0.0002(17) C36 0.042(2) 0.0664(18) 0.0323(14) 0.0021(13) -0.0023(13) 0.0000(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr O1 1.9512(17) . ? Zr O2 2.2596(15) . ? Zr N 2.3934(17) . ? Zr Cl3 2.3974(7) . ? Zr Cl1 2.4223(7) . ? Zr Cl2 2.4303(8) . ? O1 C1 1.350(2) . ? C1 C6 1.399(3) . ? C1 C2 1.408(3) . ? C2 C3 1.407(3) . ? C2 C10 1.438(3) . ? C3 C4 1.366(3) . ? C3 H3 0.9300 . ? C4 C5 1.395(3) . ? C4 H4 0.9300 . ? C5 C6 1.401(3) . ? C5 H5 0.9300 . ? C6 C61 1.539(3) . ? C61 C62 1.534(3) . ? C61 C64 1.535(4) . ? C61 C63 1.542(3) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C10 N 1.308(3) . ? C10 H10 0.9300 . ? N C11 1.470(3) . ? C11 C12 1.407(3) . ? C11 C16 1.408(3) . ? C12 C13 1.401(3) . ? C12 C121 1.520(3) . ? C121 C123 1.528(3) . ? C121 C122 1.538(3) . ? C121 H121 0.9800 . ? C122 H12A 0.9600 . ? C122 H12B 0.9600 . ? C122 H12C 0.9600 . ? C123 H12D 0.9600 . ? C123 H12E 0.9600 . ? C123 H12F 0.9600 . ? C13 C14 1.379(3) . ? C13 H13 0.9300 . ? C14 C15 1.383(3) . ? C14 H14 0.9300 . ? C15 C16 1.391(3) . ? C15 H15 0.9300 . ? C16 C161 1.517(3) . ? C161 C163 1.525(3) . ? C161 C162 1.537(3) . ? C161 H161 0.9800 . ? C162 H16A 0.9600 . ? C162 H16B 0.9600 . ? C162 H16C 0.9600 . ? C163 H16D 0.9600 . ? C163 H16E 0.9600 . ? C163 H16F 0.9600 . ? O2 C21 1.473(3) . ? O2 C24 1.477(3) . ? C21 C22 1.513(4) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.516(4) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.515(3) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C31 C36 1.405(4) . ? C31 C32 1.413(4) . ? C31 C311 1.487(4) . ? C311 H31A 0.9600 . ? C311 H31B 0.9600 . ? C311 H31C 0.9600 . ? C32 C33 1.384(4) . ? C32 H32 0.9300 . ? C33 C34 1.358(5) . ? C33 H33 0.9300 . ? C34 C35 1.356(5) . ? C34 H34 0.9300 . ? C35 C36 1.357(4) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? 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 Zr O2 84.73(6) . . ? O1 Zr N 77.19(6) . . ? O2 Zr N 86.20(5) . . ? O1 Zr Cl3 93.34(5) . . ? O2 Zr Cl3 176.11(4) . . ? N Zr Cl3 96.68(4) . . ? O1 Zr Cl1 96.46(4) . . ? O2 Zr Cl1 83.05(4) . . ? N Zr Cl1 167.99(5) . . ? Cl3 Zr Cl1 93.83(2) . . ? O1 Zr Cl2 161.72(4) . . ? O2 Zr Cl2 86.15(5) . . ? N Zr Cl2 86.44(5) . . ? Cl3 Zr Cl2 96.62(3) . . ? Cl1 Zr Cl2 98.13(2) . . ? C1 O1 Zr 149.14(14) . . ? O1 C1 C6 121.42(18) . . ? O1 C1 C2 116.4(2) . . ? C6 C1 C2 122.19(19) . . ? C3 C2 C1 118.8(2) . . ? C3 C2 C10 117.69(19) . . ? C1 C2 C10 123.40(19) . . ? C4 C3 C2 120.2(2) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 119.8(2) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C4 C5 C6 122.8(2) . . ? C4 C5 H5 118.6 . . ? C6 C5 H5 118.6 . . ? C1 C6 C5 116.1(2) . . ? C1 C6 C61 121.94(19) . . ? C5 C6 C61 121.9(2) . . ? C62 C61 C64 107.9(2) . . ? C62 C61 C6 108.8(2) . . ? C64 C61 C6 111.97(19) . . ? C62 C61 C63 109.8(2) . . ? C64 C61 C63 107.2(2) . . ? C6 C61 C63 111.10(19) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? N C10 C2 130.05(19) . . ? N C10 H10 115.0 . . ? C2 C10 H10 115.0 . . ? C10 N C11 112.07(17) . . ? C10 N Zr 123.46(15) . . ? C11 N Zr 124.33(13) . . ? C12 C11 C16 121.7(2) . . ? C12 C11 N 118.44(19) . . ? C16 C11 N 119.8(2) . . ? C13 C12 C11 117.6(2) . . ? C13 C12 C121 118.8(2) . . ? C11 C12 C121 123.5(2) . . ? C12 C121 C123 110.1(2) . . ? C12 C121 C122 111.79(18) . . ? C123 C121 C122 110.3(2) . . ? C12 C121 H121 108.2 . . ? C123 C121 H121 108.2 . . ? C122 C121 H121 108.2 . . ? C121 C122 H12A 109.5 . . ? C121 C122 H12B 109.5 . . ? H12A C122 H12B 109.5 . . ? C121 C122 H12C 109.5 . . ? H12A C122 H12C 109.5 . . ? H12B C122 H12C 109.5 . . ? C121 C123 H12D 109.5 . . ? C121 C123 H12E 109.5 . . ? H12D C123 H12E 109.5 . . ? C121 C123 H12F 109.5 . . ? H12D C123 H12F 109.5 . . ? H12E C123 H12F 109.5 . . ? C14 C13 C12 121.4(2) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C13 C14 C15 119.8(2) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C15 C16 121.6(2) . . ? C14 C15 H15 119.2 . . ? C16 C15 H15 119.2 . . ? C15 C16 C11 117.8(2) . . ? C15 C16 C161 119.7(2) . . ? C11 C16 C161 122.4(2) . . ? C16 C161 C163 111.02(18) . . ? C16 C161 C162 112.0(2) . . ? C163 C161 C162 110.85(19) . . ? C16 C161 H161 107.6 . . ? C163 C161 H161 107.6 . . ? C162 C161 H161 107.6 . . ? C161 C162 H16A 109.5 . . ? C161 C162 H16B 109.5 . . ? H16A C162 H16B 109.5 . . ? C161 C162 H16C 109.5 . . ? H16A C162 H16C 109.5 . . ? H16B C162 H16C 109.5 . . ? C161 C163 H16D 109.5 . . ? C161 C163 H16E 109.5 . . ? H16D C163 H16E 109.5 . . ? C161 C163 H16F 109.5 . . ? H16D C163 H16F 109.5 . . ? H16E C163 H16F 109.5 . . ? C21 O2 C24 109.22(17) . . ? C21 O2 Zr 123.46(13) . . ? C24 O2 Zr 125.99(13) . . ? O2 C21 C22 104.3(2) . . ? O2 C21 H21A 110.9 . . ? C22 C21 H21A 110.9 . . ? O2 C21 H21B 110.9 . . ? C22 C21 H21B 110.9 . . ? H21A C21 H21B 108.9 . . ? C21 C22 C23 102.8(2) . . ? C21 C22 H22A 111.2 . . ? C23 C22 H22A 111.2 . . ? C21 C22 H22B 111.2 . . ? C23 C22 H22B 111.2 . . ? H22A C22 H22B 109.1 . . ? C24 C23 C22 101.81(19) . . ? C24 C23 H23A 111.4 . . ? C22 C23 H23A 111.4 . . ? C24 C23 H23B 111.4 . . ? C22 C23 H23B 111.4 . . ? H23A C23 H23B 109.3 . . ? O2 C24 C23 104.45(19) . . ? O2 C24 H24A 110.9 . . ? C23 C24 H24A 110.9 . . ? O2 C24 H24B 110.9 . . ? C23 C24 H24B 110.9 . . ? H24A C24 H24B 108.9 . . ? C36 C31 C32 117.2(3) . . ? C36 C31 C311 120.7(3) . . ? C32 C31 C311 122.1(3) . . ? C31 C311 H31A 109.5 . . ? C31 C311 H31B 109.5 . . ? H31A C311 H31B 109.5 . . ? C31 C311 H31C 109.5 . . ? H31A C311 H31C 109.5 . . ? H31B C311 H31C 109.5 . . ? C33 C32 C31 120.0(3) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C34 C33 C32 121.0(3) . . ? C34 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? C35 C34 C33 119.1(3) . . ? C35 C34 H34 120.4 . . ? C33 C34 H34 120.4 . . ? C34 C35 C36 122.5(3) . . ? C34 C35 H35 118.7 . . ? C36 C35 H35 118.7 . . ? C35 C36 C31 120.1(3) . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? _diffrn_measured_fraction_theta_max 0.836 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.836 _refine_diff_density_max 0.411 _refine_diff_density_min -0.627 _refine_diff_density_rms 0.057 # #===END # data_03src0744 _database_code_depnum_ccdc_archive 'CCDC 250160' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Complex 6d' _chemical_melting_point ? _chemical_formula_moiety 'C27 H30 Cl3 N O2 Zr, C H2 Cl2' _chemical_formula_structural '[ZrCl3(thf)(OC6H3tBu-6,-CHNC6H4Ph-2)].CH2Cl2' _chemical_formula_sum 'C28 H32 Cl5 N O2 Zr' _chemical_formula_weight 683.1 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' N N 0.0061 0.0033 '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' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.5401(8) _cell_length_b 16.4653(6) _cell_length_c 18.4558(6) _cell_angle_alpha 90.00 _cell_angle_beta 129.333(2) _cell_angle_gamma 90.00 _cell_volume 6003.0(3) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 39717 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2784 _exptl_absorpt_coefficient_mu 0.839 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8916 _exptl_absorpt_correction_T_max 0.9753 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator '10cm Confocal mirrors' _diffrn_measurement_device_type 'Bruker Nonius Kappa CCD Area detector' _diffrn_measurement_method '\f and \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean '9.091 pixels mm^1^' _diffrn_standards_decay_% ? _diffrn_reflns_number 34137 _diffrn_reflns_av_R_equivalents 0.0907 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6847 _reflns_number_gt 5756 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO (Otwinowski and MInor, 1997)' _computing_data_reduction 'DENZO, COLLECT, MAXUS (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 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^)+(0.0758P)^2^+36.4731P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0016(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6847 _refine_ls_number_parameters 343 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.1689 _refine_ls_wR_factor_gt 0.1599 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 4.184 _refine_ls_shift/su_max 1.574 _refine_ls_shift/su_mean 0.025 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 Cl4 Cl -0.0261(4) 0.3123(5) 1.1534(5) 0.076(2) Uani 1 1 d U . . Cl5 Cl 0.4584(5) -0.0537(10) 1.6499(8) 0.123(3) Uani 1 1 d U . . C29 C 0.470(3) -0.002(3) 1.730(5) 0.16(2) Uani 1 1 d U . . H29A H 0.4488 0.0522 1.7092 0.194 Uiso 1 1 calc R . . H29B H 0.4571 -0.0311 1.7637 0.194 Uiso 1 1 calc R . . C28 C 0.0000 0.259(4) 1.2500 0.22(2) Uani 1 2 d SU . . H28A H -0.0377 0.2235 1.2323 0.262 Uiso 0.50 1 calc PR . . H28B H 0.0377 0.2235 1.2677 0.262 Uiso 0.50 1 calc PR . . C1 C 0.0902(7) 0.0775(9) 1.0381(10) 0.021(3) Uani 1 1 d . . . C2 C 0.0522(7) 0.1473(10) 1.0222(10) 0.023(3) Uani 1 1 d . . . C3 C 0.0433(8) 0.2169(10) 0.9612(11) 0.027(3) Uani 1 1 d . . . C4 C 0.0058(9) 0.1879(11) 0.8595(12) 0.032(4) Uani 1 1 d . . . H4A H 0.0316 0.1441 0.8591 0.049 Uiso 1 1 calc R . . H4B H 0.0013 0.2334 0.8216 0.049 Uiso 1 1 calc R . . H4C H -0.0392 0.1680 0.8332 0.049 Uiso 1 1 calc R . . C5 C 0.0019(10) 0.2872(12) 0.9578(14) 0.037(4) Uani 1 1 d . . . H5A H -0.0427 0.2671 0.9335 0.055 Uiso 1 1 calc R . . H5B H -0.0037 0.3302 0.9167 0.055 Uiso 1 1 calc R . . H5C H 0.0258 0.3090 1.0210 0.055 Uiso 1 1 calc R . . C6 C 0.1127(9) 0.2531(11) 1.0004(13) 0.033(4) Uani 1 1 d . . . H6A H 0.1373 0.2695 1.0657 0.050 Uiso 1 1 calc R . . H6B H 0.1056 0.3006 0.9631 0.050 Uiso 1 1 calc R . . H6C H 0.1390 0.2122 0.9972 0.050 Uiso 1 1 calc R . . C7 C 0.0241(8) 0.1485(11) 1.0674(11) 0.029(3) Uani 1 1 d . . . H7 H -0.0030 0.1938 1.0570 0.034 Uiso 1 1 calc R . . C8 C 0.0335(9) 0.0875(12) 1.1262(12) 0.031(4) Uani 1 1 d . . . H8 H 0.0134 0.0915 1.1552 0.037 Uiso 1 1 calc R . . C9 C 0.0723(8) 0.0207(11) 1.1424(12) 0.027(3) Uani 1 1 d . . . H9 H 0.0791 -0.0214 1.1829 0.032 Uiso 1 1 calc R . . C10 C 0.1016(8) 0.0152(9) 1.0989(11) 0.022(3) Uani 1 1 d . . . C11 C 0.1426(8) -0.0551(10) 1.1189(11) 0.023(3) Uani 1 1 d . . . H11 H 0.1419 -0.0973 1.1533 0.027 Uiso 1 1 calc R . . C12 C 0.2145(8) -0.1464(9) 1.1247(11) 0.024(3) Uani 1 1 d . . . C13 C 0.1817(10) -0.2104(11) 1.0611(13) 0.033(4) Uani 1 1 d . . . H13 H 0.1373 -0.2030 1.0037 0.040 Uiso 1 1 calc R . . C14 C 0.2135(12) -0.2843(11) 1.0812(15) 0.041(5) Uani 1 1 d . . . H14 H 0.1907 -0.3279 1.0378 0.049 Uiso 1 1 calc R . . C15 C 0.2784(12) -0.2952(11) 1.1643(16) 0.042(5) Uani 1 1 d . . . H15 H 0.3007 -0.3458 1.1777 0.050 Uiso 1 1 calc R . . C16 C 0.3108(10) -0.2318(10) 1.2282(14) 0.033(4) Uani 1 1 d . . . H16 H 0.3554 -0.2398 1.2853 0.039 Uiso 1 1 calc R . . C17 C 0.2794(9) -0.1561(10) 1.2106(12) 0.026(3) Uani 1 1 d . . . C18 C 0.3163(8) -0.0912(10) 1.2827(11) 0.025(3) Uani 1 1 d . . . C19 C 0.2930(9) -0.0619(11) 1.3286(12) 0.029(3) Uani 1 1 d . . . H19 H 0.2517 -0.0821 1.3117 0.035 Uiso 1 1 calc R . . C20 C 0.3289(10) -0.0037(11) 1.3982(13) 0.035(4) Uani 1 1 d . . . H20 H 0.3123 0.0161 1.4285 0.042 Uiso 1 1 calc R . . C21 C 0.3895(10) 0.0256(12) 1.4233(13) 0.039(4) Uani 1 1 d . . . H21 H 0.4145 0.0654 1.4712 0.047 Uiso 1 1 calc R . . C22 C 0.4133(10) -0.0030(13) 1.3792(14) 0.041(5) Uani 1 1 d . . . H22 H 0.4548 0.0172 1.3967 0.049 Uiso 1 1 calc R . . C23 C 0.3773(9) -0.0609(12) 1.3093(13) 0.034(4) Uani 1 1 d . . . H23 H 0.3943 -0.0802 1.2792 0.041 Uiso 1 1 calc R . . C24 C 0.2583(9) 0.1272(10) 1.1844(11) 0.027(3) Uani 1 1 d . . . H24A H 0.2776 0.0823 1.2305 0.033 Uiso 1 1 calc R . . H24B H 0.2131 0.1414 1.1643 0.033 Uiso 1 1 calc R . . C25 C 0.3047(9) 0.2002(11) 1.2257(13) 0.035(4) Uani 1 1 d . . . H25A H 0.3290 0.2049 1.2937 0.042 Uiso 1 1 calc R . . H25B H 0.2793 0.2509 1.1942 0.042 Uiso 1 1 calc R . . C26 C 0.3533(9) 0.1818(12) 1.2065(13) 0.034(4) Uani 1 1 d . . . H26A H 0.3763 0.2316 1.2096 0.041 Uiso 1 1 calc R . . H26B H 0.3877 0.1414 1.2515 0.041 Uiso 1 1 calc R . . C27 C 0.3070(9) 0.1480(12) 1.1088(13) 0.035(4) Uani 1 1 d . . . H27A H 0.2870 0.1922 1.0618 0.042 Uiso 1 1 calc R . . H27B H 0.3316 0.1103 1.0980 0.042 Uiso 1 1 calc R . . N1 N 0.1804(7) -0.0677(8) 1.0956(9) 0.022(3) Uani 1 1 d . . . O1 O 0.1177(5) 0.0688(6) 0.9963(7) 0.022(2) Uani 1 1 d . . . O2 O 0.2540(6) 0.1045(7) 1.1039(8) 0.026(2) Uani 1 1 d . . . Cl1 Cl 0.1789(2) 0.1065(3) 0.8859(3) 0.0310(10) Uani 1 1 d . . . Cl2 Cl 0.1087(2) -0.0815(3) 0.8685(3) 0.0313(10) Uani 1 1 d . . . Cl3 Cl 0.2882(2) -0.0571(2) 1.0561(3) 0.0286(10) Uani 1 1 d . . . Zr1 Zr 0.18339(7) 0.01339(9) 0.99220(10) 0.0205(6) 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 Cl4 0.091(4) 0.070(3) 0.067(3) -0.008(2) 0.051(3) -0.001(3) Cl5 0.092(4) 0.196(6) 0.110(5) -0.026(3) 0.078(4) -0.005(3) C29 0.16(2) 0.16(2) 0.16(2) -0.001(4) 0.103(15) 0.001(4) C28 0.43(2) 0.07(2) 0.09(2) 0.000 0.142(13) 0.000 C1 0.019(7) 0.026(8) 0.019(7) -0.006(6) 0.012(6) -0.005(6) C2 0.017(7) 0.030(8) 0.018(7) -0.005(6) 0.009(6) 0.000(6) C3 0.022(8) 0.029(8) 0.024(8) 0.002(6) 0.012(7) 0.007(6) C4 0.032(9) 0.036(9) 0.023(8) 0.002(7) 0.014(7) 0.010(7) C5 0.037(10) 0.033(9) 0.036(10) 0.001(8) 0.021(9) 0.013(8) C6 0.031(9) 0.027(8) 0.038(10) 0.001(7) 0.020(8) 0.002(7) C7 0.021(8) 0.036(9) 0.025(8) -0.005(7) 0.013(7) 0.002(6) C8 0.026(8) 0.046(10) 0.027(8) -0.004(7) 0.020(7) -0.001(7) C9 0.025(8) 0.033(9) 0.025(8) -0.002(7) 0.018(7) -0.003(7) C10 0.019(7) 0.025(8) 0.023(7) -0.005(6) 0.013(6) -0.004(6) C11 0.025(8) 0.024(8) 0.021(7) 0.000(6) 0.016(7) -0.002(6) C12 0.029(8) 0.020(7) 0.028(8) -0.001(6) 0.020(7) -0.001(6) C13 0.045(10) 0.025(8) 0.034(9) -0.002(7) 0.027(9) -0.003(7) C14 0.068(14) 0.021(8) 0.050(12) -0.005(8) 0.045(12) 0.000(8) C15 0.064(13) 0.024(9) 0.061(13) 0.005(9) 0.051(12) 0.011(9) C16 0.041(10) 0.028(9) 0.041(10) 0.009(7) 0.032(9) 0.010(7) C17 0.036(9) 0.023(8) 0.034(9) 0.002(6) 0.029(8) 0.002(7) C18 0.025(8) 0.025(8) 0.024(8) 0.006(6) 0.016(7) 0.006(6) C19 0.030(8) 0.032(9) 0.028(8) 0.002(7) 0.020(7) 0.004(7) C20 0.042(10) 0.033(9) 0.030(9) -0.001(7) 0.022(9) 0.002(8) C21 0.039(10) 0.035(10) 0.027(9) -0.002(7) 0.014(8) -0.005(8) C22 0.028(9) 0.048(11) 0.036(10) 0.002(9) 0.015(9) -0.006(8) C23 0.029(9) 0.038(10) 0.037(10) 0.004(8) 0.022(8) 0.003(7) C24 0.030(8) 0.028(8) 0.023(8) -0.004(6) 0.017(7) -0.002(7) C25 0.035(10) 0.033(9) 0.035(9) -0.011(8) 0.021(8) -0.009(8) C26 0.025(8) 0.035(9) 0.034(9) -0.004(8) 0.014(8) -0.008(7) C27 0.034(9) 0.036(10) 0.040(10) -0.006(8) 0.026(9) -0.012(8) N1 0.025(7) 0.020(6) 0.023(6) -0.003(5) 0.016(6) -0.002(5) O1 0.024(5) 0.023(5) 0.022(5) 0.000(4) 0.016(5) 0.000(4) O2 0.025(6) 0.028(6) 0.027(6) -0.006(5) 0.018(5) -0.005(5) Cl1 0.037(2) 0.033(2) 0.030(2) 0.0056(16) 0.0246(19) 0.0021(17) Cl2 0.033(2) 0.037(2) 0.027(2) -0.0095(16) 0.0202(18) -0.0082(17) Cl3 0.030(2) 0.028(2) 0.036(2) 0.0042(16) 0.0256(19) 0.0054(15) Zr1 0.0224(9) 0.0219(9) 0.0217(9) -0.0010(6) 0.0162(7) -0.0002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl4 C28 1.70(3) . ? Cl5 C29 1.55(7) . ? Cl5 C29 1.96(7) 2_658 ? C29 C29 1.22(11) 2_658 ? C29 Cl5 1.96(7) 2_658 ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C28 Cl4 1.70(3) 2_557 ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C1 O1 1.340(18) . ? C1 C10 1.41(2) . ? C1 C2 1.41(2) . ? C2 C7 1.40(2) . ? C2 C3 1.52(2) . ? C3 C5 1.54(2) . ? C3 C4 1.55(2) . ? C3 C6 1.55(2) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.38(3) . ? C7 H7 0.9500 . ? C8 C9 1.38(2) . ? C8 H8 0.9500 . ? C9 C10 1.41(2) . ? C9 H9 0.9500 . ? C10 C11 1.44(2) . ? C11 N1 1.30(2) . ? C11 H11 0.9500 . ? C12 C13 1.39(2) . ? C12 C17 1.40(2) . ? C12 N1 1.46(2) . ? C13 C14 1.38(3) . ? C13 H13 0.9500 . ? C14 C15 1.38(3) . ? C14 H14 0.9500 . ? C15 C16 1.39(3) . ? C15 H15 0.9500 . ? C16 C17 1.40(2) . ? C16 H16 0.9500 . ? C17 C18 1.49(2) . ? C18 C19 1.39(2) . ? C18 C23 1.40(2) . ? C19 C20 1.38(3) . ? C19 H19 0.9500 . ? C20 C21 1.39(3) . ? C20 H20 0.9500 . ? C21 C22 1.37(3) . ? C21 H21 0.9500 . ? C22 C23 1.38(3) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 O2 1.467(19) . ? C24 C25 1.51(2) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.52(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.50(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 O2 1.48(2) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? N1 Zr1 2.369(13) . ? O1 Zr1 1.952(11) . ? O2 Zr1 2.245(11) . ? Cl1 Zr1 2.435(4) . ? Cl2 Zr1 2.403(4) . ? Cl3 Zr1 2.430(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C29 Cl5 C29 38(4) . 2_658 ? C29 C29 Cl5 89(6) 2_658 . ? C29 C29 Cl5 52(5) 2_658 2_658 ? Cl5 C29 Cl5 109(3) . 2_658 ? C29 C29 H29A 113.9 2_658 . ? Cl5 C29 H29A 114.0 . . ? Cl5 C29 H29A 135.2 2_658 . ? C29 C29 H29B 113.5 2_658 . ? Cl5 C29 H29B 113.6 . . ? Cl5 C29 H29B 61.2 2_658 . ? H29A C29 H29B 111.0 . . ? Cl4 C28 Cl4 118(4) 2_557 . ? Cl4 C28 H28A 107.8 2_557 . ? Cl4 C28 H28A 107.8 . . ? Cl4 C28 H28B 107.8 2_557 . ? Cl4 C28 H28B 107.8 . . ? H28A C28 H28B 107.1 . . ? O1 C1 C10 117.5(14) . . ? O1 C1 C2 120.7(14) . . ? C10 C1 C2 121.8(14) . . ? C7 C2 C1 115.6(15) . . ? C7 C2 C3 122.5(14) . . ? C1 C2 C3 121.9(14) . . ? C2 C3 C5 111.9(14) . . ? C2 C3 C4 110.7(14) . . ? C5 C3 C4 107.5(13) . . ? C2 C3 C6 110.8(13) . . ? C5 C3 C6 106.4(15) . . ? C4 C3 C6 109.3(15) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C2 123.7(16) . . ? C8 C7 H7 118.1 . . ? C2 C7 H7 118.1 . . ? C9 C8 C7 119.5(15) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 119.8(16) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C9 C10 C1 119.5(15) . . ? C9 C10 C11 117.9(15) . . ? C1 C10 C11 122.6(14) . . ? N1 C11 C10 127.9(14) . . ? N1 C11 H11 116.1 . . ? C10 C11 H11 116.1 . . ? C13 C12 C17 121.1(15) . . ? C13 C12 N1 117.5(15) . . ? C17 C12 N1 121.3(14) . . ? C14 C13 C12 120.4(18) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 120.0(18) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C16 119.7(17) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 C17 121.6(18) . . ? C15 C16 H16 119.2 . . ? C17 C16 H16 119.2 . . ? C12 C17 C16 117.1(16) . . ? C12 C17 C18 123.8(14) . . ? C16 C17 C18 119.0(16) . . ? C19 C18 C23 118.3(16) . . ? C19 C18 C17 121.3(15) . . ? C23 C18 C17 120.3(15) . . ? C20 C19 C18 121.1(17) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C19 C20 C21 119.6(18) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C22 C21 C20 120.1(18) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 120.5(19) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C22 C23 C18 120.5(18) . . ? C22 C23 H23 119.8 . . ? C18 C23 H23 119.8 . . ? O2 C24 C25 104.1(13) . . ? O2 C24 H24A 110.9 . . ? C25 C24 H24A 110.9 . . ? O2 C24 H24B 110.9 . . ? C25 C24 H24B 110.9 . . ? H24A C24 H24B 108.9 . . ? C24 C25 C26 102.7(14) . . ? C24 C25 H25A 111.2 . . ? C26 C25 H25A 111.2 . . ? C24 C25 H25B 111.2 . . ? C26 C25 H25B 111.2 . . ? H25A C25 H25B 109.1 . . ? C27 C26 C25 102.5(14) . . ? C27 C26 H26A 111.3 . . ? C25 C26 H26A 111.3 . . ? C27 C26 H26B 111.3 . . ? C25 C26 H26B 111.3 . . ? H26A C26 H26B 109.2 . . ? O2 C27 C26 104.2(14) . . ? O2 C27 H27A 110.9 . . ? C26 C27 H27A 110.9 . . ? O2 C27 H27B 110.9 . . ? C26 C27 H27B 110.9 . . ? H27A C27 H27B 108.9 . . ? C11 N1 C12 114.4(13) . . ? C11 N1 Zr1 126.0(11) . . ? C12 N1 Zr1 118.7(9) . . ? C1 O1 Zr1 148.1(10) . . ? C24 O2 C27 109.6(12) . . ? C24 O2 Zr1 127.0(9) . . ? C27 O2 Zr1 123.3(10) . . ? O1 Zr1 O2 82.0(4) . . ? O1 Zr1 N1 76.4(4) . . ? O2 Zr1 N1 93.1(4) . . ? O1 Zr1 Cl2 99.0(3) . . ? O2 Zr1 Cl2 177.6(3) . . ? N1 Zr1 Cl2 89.3(3) . . ? O1 Zr1 Cl3 156.0(3) . . ? O2 Zr1 Cl3 82.9(3) . . ? N1 Zr1 Cl3 85.9(3) . . ? Cl2 Zr1 Cl3 96.74(15) . . ? O1 Zr1 Cl1 97.8(3) . . ? O2 Zr1 Cl1 85.4(3) . . ? N1 Zr1 Cl1 174.1(3) . . ? Cl2 Zr1 Cl1 92.30(15) . . ? Cl3 Zr1 Cl1 99.56(15) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.156 _refine_diff_density_min -2.889 _refine_diff_density_rms 0.135 # #===END # data_03src0487 _database_code_depnum_ccdc_archive 'CCDC 250161' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Complex 6e' _chemical_melting_point ? _chemical_formula_moiety 'C21 H21 Cl3 F5 N O2 Zr' _chemical_formula_structural '[ZrCl3(OC6H3tBu-6,-CHNC6F5-2)]' _chemical_formula_sum 'C21 H21 Cl3 F5 N O2 Zr' _chemical_formula_weight 611.96 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' N N 0.0061 0.0033 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.49490(10) _cell_length_b 9.4703(2) _cell_length_c 17.3848(5) _cell_angle_alpha 82.6990(10) _cell_angle_beta 80.7480(10) _cell_angle_gamma 87.446(2) _cell_volume 1207.66(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 21583 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.683 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 0.845 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8103 _exptl_absorpt_correction_T_max 0.9511 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker Nonius Kappa CCD Area detector' _diffrn_measurement_method '\f and \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean '9.091 pixels mm^1^' _diffrn_standards_number ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22105 _diffrn_reflns_av_R_equivalents 0.0965 _diffrn_reflns_av_sigmaI/netI 0.0576 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5485 _reflns_number_gt 5002 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0400P)^2^+0.8095P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0076(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5485 _refine_ls_number_parameters 302 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0952 _refine_ls_wR_factor_gt 0.0920 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6900(3) 0.2847(2) 0.22178(13) 0.0213(4) Uani 1 1 d . . . C2 C 0.7139(3) 0.1506(3) 0.26240(15) 0.0270(5) Uani 1 1 d . . . C3 C 0.8118(4) 0.0432(3) 0.22690(17) 0.0345(6) Uani 1 1 d . . . C4 C 0.8933(4) 0.0692(3) 0.14999(18) 0.0395(7) Uani 1 1 d . . . C5 C 0.8728(3) 0.2014(3) 0.10845(15) 0.0341(6) Uani 1 1 d . . . C6 C 0.7701(3) 0.3079(3) 0.14392(14) 0.0260(5) Uani 1 1 d . . . C7 C 0.6637(3) 0.4324(2) 0.31689(12) 0.0187(4) Uani 1 1 d . . . H7 H 0.7728 0.3824 0.3256 0.022 Uiso 1 1 calc R . . C8 C 0.6042(3) 0.5390(2) 0.36785(12) 0.0189(4) Uani 1 1 d . . . C9 C 0.7079(3) 0.5519(3) 0.42712(13) 0.0229(5) Uani 1 1 d . . . H9 H 0.8099 0.4907 0.4330 0.027 Uiso 1 1 calc R . . C10 C 0.6594(3) 0.6545(3) 0.47643(13) 0.0261(5) Uani 1 1 d . . . H10 H 0.7246 0.6618 0.5183 0.031 Uiso 1 1 calc R . . C11 C 0.5149(3) 0.7473(3) 0.46481(13) 0.0237(5) Uani 1 1 d . . . H11 H 0.4871 0.8195 0.4984 0.028 Uiso 1 1 calc R . . C12 C 0.4077(3) 0.7409(2) 0.40655(12) 0.0190(4) Uani 1 1 d . . . C13 C 0.4528(3) 0.6300(2) 0.35976(12) 0.0171(4) Uani 1 1 d . . . C14 C 0.2500(3) 0.8461(2) 0.39563(13) 0.0229(5) Uani 1 1 d . . . C15 C 0.2405(4) 0.9634(3) 0.44935(15) 0.0302(5) Uani 1 1 d . . . H15A H 0.2218 0.9205 0.5043 0.045 Uiso 1 1 calc R . . H15B H 0.1397 1.0295 0.4401 0.045 Uiso 1 1 calc R . . H15C H 0.3539 1.0151 0.4380 0.045 Uiso 1 1 calc R . . C16 C 0.0714(3) 0.7667(3) 0.41616(15) 0.0271(5) Uani 1 1 d . . . H16A H 0.0557 0.7251 0.4713 0.041 Uiso 1 1 calc R . . H16B H 0.0737 0.6909 0.3826 0.041 Uiso 1 1 calc R . . H16C H -0.0293 0.8335 0.4077 0.041 Uiso 1 1 calc R . . C17 C 0.2688(3) 0.9191(3) 0.31034(14) 0.0270(5) Uani 1 1 d . . . H17A H 0.1757 0.9946 0.3064 0.041 Uiso 1 1 calc R . . H17B H 0.2538 0.8487 0.2753 0.041 Uiso 1 1 calc R . . H17C H 0.3887 0.9605 0.2951 0.041 Uiso 1 1 calc R . . C18 C 0.5799(3) 0.7289(3) 0.15081(14) 0.0262(5) Uani 1 1 d . . . H18A H 0.6954 0.6771 0.1569 0.031 Uiso 1 1 calc R . . H18B H 0.5400 0.7788 0.1976 0.031 Uiso 1 1 calc R . . C19 C 0.6013(5) 0.8314(4) 0.0783(2) 0.0627(11) Uani 1 1 d . . . H19A H 0.7121 0.8080 0.0424 0.075 Uiso 1 1 calc R . . H19B H 0.6099 0.9296 0.0910 0.075 Uiso 1 1 calc R . . C20 C 0.4342(4) 0.8180(3) 0.04062(15) 0.0308(5) Uani 1 1 d . . . H20A H 0.3317 0.8771 0.0634 0.037 Uiso 1 1 calc R . . H20B H 0.4590 0.8447 -0.0169 0.037 Uiso 1 1 calc R . . C21 C 0.3989(4) 0.6625(3) 0.06130(13) 0.0302(5) Uani 1 1 d . . . H21A H 0.2710 0.6426 0.0598 0.036 Uiso 1 1 calc R . . H21B H 0.4776 0.6058 0.0246 0.036 Uiso 1 1 calc R . . N1 N 0.5876(2) 0.39498(19) 0.26009(10) 0.0177(4) Uani 1 1 d . . . O1 O 0.35269(19) 0.60631(15) 0.30543(8) 0.0177(3) Uani 1 1 d . . . O2 O 0.4411(2) 0.62980(17) 0.14099(9) 0.0213(3) Uani 1 1 d . . . F1 F 0.75193(19) 0.43444(17) 0.10155(8) 0.0318(3) Uani 1 1 d . . . F2 F 0.9514(2) 0.2273(2) 0.03330(9) 0.0482(5) Uani 1 1 d . . . F3 F 0.9917(2) -0.0333(2) 0.11507(12) 0.0562(5) Uani 1 1 d . . . F4 F 0.8287(2) -0.08620(17) 0.26758(12) 0.0491(5) Uani 1 1 d . . . F5 F 0.6399(2) 0.12297(15) 0.33805(9) 0.0321(3) Uani 1 1 d . . . Cl2 Cl 0.14353(7) 0.31169(6) 0.33982(3) 0.02213(13) Uani 1 1 d . . . Cl3 Cl 0.32768(7) 0.30362(6) 0.13995(3) 0.02518(14) Uani 1 1 d . . . Cl1 Cl 0.02024(7) 0.59421(6) 0.20262(3) 0.02663(14) Uani 1 1 d . . . Zr1 Zr 0.29462(2) 0.47652(2) 0.234500(11) 0.01515(9) 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 C1 0.0147(10) 0.0244(11) 0.0274(11) -0.0100(9) -0.0063(8) 0.0014(8) C2 0.0207(11) 0.0264(12) 0.0370(13) -0.0110(10) -0.0087(9) 0.0005(9) C3 0.0286(13) 0.0278(13) 0.0524(17) -0.0151(12) -0.0169(11) 0.0078(10) C4 0.0264(13) 0.0415(16) 0.0585(18) -0.0300(14) -0.0158(12) 0.0130(11) C5 0.0209(12) 0.0539(17) 0.0319(13) -0.0218(12) -0.0062(9) 0.0054(11) C6 0.0183(11) 0.0322(13) 0.0302(12) -0.0098(10) -0.0080(9) 0.0019(9) C7 0.0148(10) 0.0197(10) 0.0213(10) 0.0000(8) -0.0031(7) -0.0013(8) C8 0.0168(10) 0.0233(11) 0.0172(10) -0.0031(8) -0.0024(7) -0.0052(8) C9 0.0189(11) 0.0305(12) 0.0201(10) -0.0020(9) -0.0050(8) -0.0045(9) C10 0.0213(11) 0.0396(14) 0.0202(11) -0.0082(10) -0.0061(8) -0.0096(10) C11 0.0227(11) 0.0292(12) 0.0205(11) -0.0100(9) 0.0006(8) -0.0083(9) C12 0.0186(10) 0.0198(10) 0.0185(10) -0.0037(8) 0.0000(8) -0.0069(8) C13 0.0188(10) 0.0176(10) 0.0154(9) -0.0019(8) -0.0030(7) -0.0068(8) C14 0.0243(11) 0.0201(11) 0.0243(11) -0.0069(9) -0.0008(8) -0.0021(8) C15 0.0389(14) 0.0236(12) 0.0294(12) -0.0104(10) -0.0033(10) -0.0018(10) C16 0.0206(11) 0.0246(12) 0.0354(13) -0.0046(10) -0.0016(9) -0.0006(9) C17 0.0333(13) 0.0195(11) 0.0287(12) -0.0043(9) -0.0044(9) -0.0039(9) C18 0.0233(11) 0.0254(12) 0.0313(12) -0.0024(9) -0.0076(9) -0.0073(9) C19 0.073(2) 0.060(2) 0.057(2) 0.0297(17) -0.0339(18) -0.0436(19) C20 0.0413(14) 0.0241(12) 0.0273(12) -0.0005(10) -0.0092(10) 0.0031(10) C21 0.0450(15) 0.0288(13) 0.0178(11) 0.0015(9) -0.0091(10) -0.0087(11) N1 0.0143(8) 0.0195(9) 0.0198(9) -0.0047(7) -0.0030(6) 0.0010(7) O1 0.0187(7) 0.0178(7) 0.0188(7) -0.0057(6) -0.0065(5) -0.0004(6) O2 0.0254(8) 0.0213(8) 0.0185(7) -0.0005(6) -0.0068(6) -0.0068(6) F1 0.0285(8) 0.0425(9) 0.0239(7) -0.0065(6) -0.0017(5) 0.0007(6) F2 0.0327(9) 0.0809(14) 0.0337(9) -0.0272(9) -0.0015(6) 0.0126(8) F3 0.0437(10) 0.0595(12) 0.0748(13) -0.0454(10) -0.0166(9) 0.0283(9) F4 0.0513(11) 0.0247(8) 0.0760(13) -0.0134(8) -0.0218(9) 0.0135(7) F5 0.0329(8) 0.0259(7) 0.0365(8) 0.0005(6) -0.0057(6) 0.0012(6) Cl2 0.0230(3) 0.0206(3) 0.0222(3) 0.0004(2) -0.00344(19) -0.0023(2) Cl3 0.0247(3) 0.0287(3) 0.0251(3) -0.0132(2) -0.0045(2) -0.0022(2) Cl1 0.0209(3) 0.0256(3) 0.0350(3) -0.0007(2) -0.0125(2) 0.0032(2) Zr1 0.01490(13) 0.01529(14) 0.01654(13) -0.00359(8) -0.00487(8) -0.00075(8) _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 C6 1.384(3) . ? C1 C2 1.391(3) . ? C1 N1 1.437(3) . ? C2 F5 1.340(3) . ? C2 C3 1.379(3) . ? C3 F4 1.346(3) . ? C3 C4 1.374(4) . ? C4 F3 1.340(3) . ? C4 C5 1.379(4) . ? C5 F2 1.341(3) . ? C5 C6 1.388(3) . ? C6 F1 1.338(3) . ? C7 N1 1.309(3) . ? C7 C8 1.436(3) . ? C7 H7 0.9500 . ? C8 C9 1.407(3) . ? C8 C13 1.408(3) . ? C9 C10 1.375(3) . ? C9 H9 0.9500 . ? C10 C11 1.388(4) . ? C10 H10 0.9500 . ? C11 C12 1.399(3) . ? C11 H11 0.9500 . ? C12 C13 1.405(3) . ? C12 C14 1.531(3) . ? C13 O1 1.343(2) . ? C14 C15 1.532(3) . ? C14 C16 1.534(3) . ? C14 C17 1.542(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 O2 1.476(3) . ? C18 C19 1.481(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.521(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.496(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 O2 1.462(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? N1 Zr1 2.3857(17) . ? O1 Zr1 1.9561(14) . ? O2 Zr1 2.2187(15) . ? Cl2 Zr1 2.4157(5) . ? Cl3 Zr1 2.4415(5) . ? Cl1 Zr1 2.4049(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 117.6(2) . . ? C6 C1 N1 121.6(2) . . ? C2 C1 N1 120.8(2) . . ? F5 C2 C3 118.2(2) . . ? F5 C2 C1 119.9(2) . . ? C3 C2 C1 121.8(2) . . ? F4 C3 C4 120.2(2) . . ? F4 C3 C2 120.2(3) . . ? C4 C3 C2 119.7(3) . . ? F3 C4 C3 120.4(3) . . ? F3 C4 C5 119.9(3) . . ? C3 C4 C5 119.7(2) . . ? F2 C5 C4 120.0(2) . . ? F2 C5 C6 119.7(3) . . ? C4 C5 C6 120.3(2) . . ? F1 C6 C1 120.5(2) . . ? F1 C6 C5 118.6(2) . . ? C1 C6 C5 120.8(2) . . ? N1 C7 C8 128.6(2) . . ? N1 C7 H7 115.7 . . ? C8 C7 H7 115.7 . . ? C9 C8 C13 120.0(2) . . ? C9 C8 C7 116.6(2) . . ? C13 C8 C7 123.34(19) . . ? C10 C9 C8 119.1(2) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C9 C10 C11 119.7(2) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C10 C11 C12 123.9(2) . . ? C10 C11 H11 118.0 . . ? C12 C11 H11 118.0 . . ? C11 C12 C13 115.4(2) . . ? C11 C12 C14 122.1(2) . . ? C13 C12 C14 122.44(19) . . ? O1 C13 C12 121.22(19) . . ? O1 C13 C8 117.16(18) . . ? C12 C13 C8 121.62(19) . . ? C12 C14 C15 111.7(2) . . ? C12 C14 C16 109.45(18) . . ? C15 C14 C16 107.68(19) . . ? C12 C14 C17 111.03(18) . . ? C15 C14 C17 107.52(18) . . ? C16 C14 C17 109.3(2) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O2 C18 C19 105.4(2) . . ? O2 C18 H18A 110.7 . . ? C19 C18 H18A 110.7 . . ? O2 C18 H18B 110.7 . . ? C19 C18 H18B 110.7 . . ? H18A C18 H18B 108.8 . . ? C18 C19 C20 106.0(2) . . ? C18 C19 H19A 110.5 . . ? C20 C19 H19A 110.5 . . ? C18 C19 H19B 110.5 . . ? C20 C19 H19B 110.5 . . ? H19A C19 H19B 108.7 . . ? C21 C20 C19 101.1(2) . . ? C21 C20 H20A 111.5 . . ? C19 C20 H20A 111.5 . . ? C21 C20 H20B 111.5 . . ? C19 C20 H20B 111.5 . . ? H20A C20 H20B 109.4 . . ? O2 C21 C20 104.26(19) . . ? O2 C21 H21A 110.9 . . ? C20 C21 H21A 110.9 . . ? O2 C21 H21B 110.9 . . ? C20 C21 H21B 110.9 . . ? H21A C21 H21B 108.9 . . ? C7 N1 C1 111.98(18) . . ? C7 N1 Zr1 123.99(14) . . ? C1 N1 Zr1 123.52(13) . . ? C13 O1 Zr1 147.31(14) . . ? C21 O2 C18 108.16(17) . . ? C21 O2 Zr1 125.15(13) . . ? C18 O2 Zr1 126.25(13) . . ? O1 Zr1 O2 84.41(6) . . ? O1 Zr1 N1 76.68(6) . . ? O2 Zr1 N1 85.49(6) . . ? O1 Zr1 Cl1 98.04(5) . . ? O2 Zr1 Cl1 86.88(4) . . ? N1 Zr1 Cl1 171.10(5) . . ? O1 Zr1 Cl2 93.65(4) . . ? O2 Zr1 Cl2 177.67(4) . . ? N1 Zr1 Cl2 92.81(4) . . ? Cl1 Zr1 Cl2 94.68(2) . . ? O1 Zr1 Cl3 161.50(5) . . ? O2 Zr1 Cl3 88.06(4) . . ? N1 Zr1 Cl3 85.92(4) . . ? Cl1 Zr1 Cl3 98.40(2) . . ? Cl2 Zr1 Cl3 93.42(2) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.620 _refine_diff_density_min -0.838 _refine_diff_density_rms 0.100 # #===END # data_03src0767 _database_code_depnum_ccdc_archive 'CCDC 250162' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Complex 7' _chemical_melting_point ? _chemical_formula_moiety 'C15 H21 Cl3 O3 Ti' _chemical_formula_structural '[TiCl3(thf)(OC6H3tBu-6,-CHO-2)]' _chemical_formula_sum 'C15 H21 Cl3 O3 Ti' _chemical_formula_weight 403.57 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.5359(4) _cell_length_b 8.3775(4) _cell_length_c 20.2839(10) _cell_angle_alpha 90.00 _cell_angle_beta 101.350(3) _cell_angle_gamma 90.00 _cell_volume 1755.33(14) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 55955 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.1 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 0.952 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7633 _exptl_absorpt_correction_T_max 0.9953 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 Nonius Kappa CCD Area detector' _diffrn_measurement_method '\f and \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean '9.091 pixels mm^1^' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19393 _diffrn_reflns_av_R_equivalents 0.1232 _diffrn_reflns_av_sigmaI/netI 0.0867 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.08 _reflns_number_total 3826 _reflns_number_gt 3016 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO (Otwinowski and MInor, 1997)' _computing_data_reduction 'DENZO, COLLECT, MAXUS (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 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^)+(0.0000P)^2^+100.6789P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.024(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3826 _refine_ls_number_parameters 203 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1749 _refine_ls_R_factor_gt 0.1491 _refine_ls_wR_factor_ref 0.3641 _refine_ls_wR_factor_gt 0.3535 _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_restrained_S_all 1.147 _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 C1 C 0.3650(12) -0.0154(16) 0.2532(6) 0.018(3) Uani 1 1 d . . . H1 H 0.3483 -0.0937 0.2843 0.021 Uiso 1 1 calc R . . C2 C 0.4541(13) 0.1090(15) 0.2790(6) 0.019(3) Uani 1 1 d . . . C3 C 0.5253(13) 0.0965(15) 0.3456(6) 0.020(3) Uani 1 1 d . . . H3 H 0.5170 0.0049 0.3720 0.024 Uiso 1 1 calc R . . C4 C 0.6057(12) 0.2179(16) 0.3711(6) 0.020(3) Uani 1 1 d . . . H4 H 0.6565 0.2090 0.4151 0.023 Uiso 1 1 calc R . . C5 C 0.6149(13) 0.3561(18) 0.3332(6) 0.024(3) Uani 1 1 d . . . H5 H 0.6715 0.4388 0.3529 0.029 Uiso 1 1 calc R . . C6 C 0.5441(11) 0.3778(15) 0.2674(6) 0.015(2) Uani 1 1 d . . . C7 C 0.4655(14) 0.2512(17) 0.2415(7) 0.025(3) Uani 1 1 d . . . C8 C 0.5547(13) 0.5276(16) 0.2265(7) 0.023(3) Uani 1 1 d . . . C9 C 0.4171(13) 0.5974(16) 0.2018(7) 0.024(3) Uani 1 1 d . . . H9A H 0.3638 0.5197 0.1725 0.037 Uiso 1 1 calc R . . H9B H 0.4232 0.6960 0.1766 0.037 Uiso 1 1 calc R . . H9C H 0.3775 0.6205 0.2406 0.037 Uiso 1 1 calc R . . C10 C 0.6378(15) 0.6551(17) 0.2688(8) 0.031(3) Uani 1 1 d . . . H10A H 0.5981 0.6847 0.3069 0.047 Uiso 1 1 calc R . . H10B H 0.6435 0.7494 0.2410 0.047 Uiso 1 1 calc R . . H10C H 0.7248 0.6126 0.2856 0.047 Uiso 1 1 calc R . . C11 C 0.6160(13) 0.4850(16) 0.1654(6) 0.022(3) Uani 1 1 d . . . H11A H 0.7049 0.4476 0.1812 0.033 Uiso 1 1 calc R . . H11B H 0.6168 0.5798 0.1372 0.033 Uiso 1 1 calc R . . H11C H 0.5651 0.4006 0.1390 0.033 Uiso 1 1 calc R . . C12 C 0.1510(13) -0.1824(18) 0.0634(7) 0.026(3) Uani 1 1 d . . . H12A H 0.0706 -0.1245 0.0435 0.031 Uiso 1 1 calc R . . H12B H 0.1506 -0.2040 0.1113 0.031 Uiso 1 1 calc R . . C13 C 0.1605(14) -0.3346(17) 0.0264(7) 0.028(3) Uani 1 1 d . . . H13A H 0.0738 -0.3763 0.0060 0.034 Uiso 1 1 calc R . . H13B H 0.2086 -0.4169 0.0564 0.034 Uiso 1 1 calc R . . C14 C 0.2350(15) -0.2827(19) -0.0274(7) 0.031(3) Uani 1 1 d . . . H14A H 0.2751 -0.3751 -0.0458 0.038 Uiso 1 1 calc R . . H14B H 0.1782 -0.2255 -0.0646 0.038 Uiso 1 1 calc R . . C15 C 0.3344(15) -0.1749(19) 0.0111(7) 0.030(3) Uani 1 1 d . . . H15A H 0.4081 -0.2364 0.0368 0.036 Uiso 1 1 calc R . . H15B H 0.3671 -0.0993 -0.0192 0.036 Uiso 1 1 calc R . . O1 O 0.3068(9) -0.0305(11) 0.1932(5) 0.023(2) Uani 1 1 d . . . O2 O 0.3977(8) 0.2562(10) 0.1789(4) 0.0169(18) Uani 1 1 d . . . O3 O 0.2637(9) -0.0899(11) 0.0568(5) 0.023(2) Uani 1 1 d . . . Cl1 Cl 0.5337(3) -0.0062(4) 0.12706(16) 0.0223(8) Uani 1 1 d . . . Cl2 Cl 0.1174(3) 0.1860(4) 0.10483(17) 0.0252(8) Uani 1 1 d . . . Cl3 Cl 0.3602(3) 0.2608(4) 0.02330(16) 0.0264(8) Uani 1 1 d . . . Ti1 Ti 0.3325(2) 0.1140(3) 0.11268(11) 0.0173(6) 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 C1 0.021(6) 0.023(6) 0.012(5) 0.006(5) 0.008(5) 0.005(5) C2 0.026(7) 0.016(6) 0.013(5) 0.000(5) 0.003(5) 0.004(5) C3 0.025(7) 0.017(6) 0.017(6) 0.003(5) 0.002(5) 0.002(5) C4 0.022(6) 0.024(7) 0.012(5) 0.002(5) 0.000(5) 0.006(5) C5 0.022(6) 0.029(7) 0.019(6) -0.006(6) 0.000(5) 0.002(6) C6 0.007(5) 0.022(6) 0.017(6) -0.001(5) 0.001(4) 0.005(5) C7 0.035(8) 0.021(7) 0.020(6) 0.007(5) 0.008(6) 0.005(6) C8 0.022(7) 0.021(7) 0.025(7) -0.004(5) 0.004(5) -0.009(5) C9 0.027(7) 0.015(6) 0.029(7) -0.003(5) -0.001(6) -0.002(5) C10 0.037(8) 0.019(7) 0.034(8) -0.006(6) -0.004(6) -0.013(6) C11 0.026(7) 0.019(7) 0.021(6) -0.004(5) 0.001(5) -0.002(5) C12 0.025(7) 0.030(7) 0.023(7) 0.002(6) 0.006(5) -0.004(6) C13 0.026(7) 0.020(7) 0.035(8) -0.001(6) 0.000(6) -0.008(6) C14 0.038(8) 0.030(8) 0.029(7) -0.008(6) 0.012(6) 0.001(7) C15 0.032(8) 0.032(8) 0.030(7) -0.013(6) 0.019(6) -0.009(6) O1 0.032(5) 0.016(5) 0.024(5) 0.003(4) 0.013(4) 0.005(4) O2 0.023(4) 0.012(4) 0.015(4) 0.001(3) 0.003(3) 0.001(4) O3 0.021(5) 0.026(5) 0.023(5) -0.006(4) 0.012(4) -0.006(4) Cl1 0.0187(15) 0.0247(16) 0.0239(15) 0.0013(13) 0.0048(12) -0.0003(13) Cl2 0.0198(15) 0.0291(18) 0.0262(16) -0.0035(14) 0.0031(12) 0.0082(13) Cl3 0.0309(18) 0.0265(18) 0.0207(15) 0.0065(13) 0.0023(13) 0.0006(14) Ti1 0.0173(12) 0.0168(12) 0.0172(11) -0.0005(9) 0.0018(8) 0.0015(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.257(15) . ? C1 C2 1.431(18) . ? C1 H1 0.9500 . ? C2 C3 1.413(17) . ? C2 C7 1.431(18) . ? C3 C4 1.359(18) . ? C3 H3 0.9500 . ? C4 C5 1.403(19) . ? C4 H4 0.9500 . ? C5 C6 1.407(17) . ? C5 H5 0.9500 . ? C6 C7 1.383(19) . ? C6 C8 1.520(18) . ? C7 O2 1.330(16) . ? C8 C10 1.532(18) . ? C8 C11 1.549(18) . ? C8 C9 1.552(19) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 O3 1.446(16) . ? C12 C13 1.49(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.53(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.48(2) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O3 1.481(16) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? O1 Ti1 2.094(9) . ? O2 Ti1 1.825(9) . ? O3 Ti1 2.100(9) . ? Cl1 Ti1 2.312(4) . ? Cl2 Ti1 2.321(4) . ? Cl3 Ti1 2.256(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 126.0(11) . . ? O1 C1 H1 117.0 . . ? C2 C1 H1 117.0 . . ? C3 C2 C1 118.8(11) . . ? C3 C2 C7 119.1(12) . . ? C1 C2 C7 122.0(11) . . ? C4 C3 C2 118.8(12) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 120.9(11) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C4 C5 C6 123.0(13) . . ? C4 C5 H5 118.5 . . ? C6 C5 H5 118.5 . . ? C7 C6 C5 115.3(12) . . ? C7 C6 C8 121.9(11) . . ? C5 C6 C8 122.8(12) . . ? O2 C7 C6 120.5(12) . . ? O2 C7 C2 116.6(12) . . ? C6 C7 C2 122.9(12) . . ? C6 C8 C10 111.5(11) . . ? C6 C8 C11 109.5(11) . . ? C10 C8 C11 109.1(11) . . ? C6 C8 C9 108.8(10) . . ? C10 C8 C9 108.2(11) . . ? C11 C8 C9 109.7(11) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O3 C12 C13 105.9(11) . . ? O3 C12 H12A 110.6 . . ? C13 C12 H12A 110.6 . . ? O3 C12 H12B 110.6 . . ? C13 C12 H12B 110.6 . . ? H12A C12 H12B 108.7 . . ? C12 C13 C14 102.2(11) . . ? C12 C13 H13A 111.3 . . ? C14 C13 H13A 111.3 . . ? C12 C13 H13B 111.3 . . ? C14 C13 H13B 111.3 . . ? H13A C13 H13B 109.2 . . ? C15 C14 C13 102.0(11) . . ? C15 C14 H14A 111.4 . . ? C13 C14 H14A 111.4 . . ? C15 C14 H14B 111.4 . . ? C13 C14 H14B 111.4 . . ? H14A C14 H14B 109.2 . . ? O3 C15 C14 103.3(11) . . ? O3 C15 H15A 111.1 . . ? C14 C15 H15A 111.1 . . ? O3 C15 H15B 111.1 . . ? C14 C15 H15B 111.1 . . ? H15A C15 H15B 109.1 . . ? C1 O1 Ti1 125.7(9) . . ? C7 O2 Ti1 137.4(8) . . ? C12 O3 C15 108.9(10) . . ? C12 O3 Ti1 126.1(8) . . ? C15 O3 Ti1 124.5(8) . . ? O2 Ti1 O1 83.7(4) . . ? O2 Ti1 O3 165.6(4) . . ? O1 Ti1 O3 82.4(4) . . ? O2 Ti1 Cl3 98.4(3) . . ? O1 Ti1 Cl3 177.7(3) . . ? O3 Ti1 Cl3 95.4(3) . . ? O2 Ti1 Cl1 89.3(3) . . ? O1 Ti1 Cl1 84.6(3) . . ? O3 Ti1 Cl1 85.7(3) . . ? Cl3 Ti1 Cl1 94.52(15) . . ? O2 Ti1 Cl2 95.9(3) . . ? O1 Ti1 Cl2 85.9(3) . . ? O3 Ti1 Cl2 86.9(3) . . ? Cl3 Ti1 Cl2 94.70(15) . . ? Cl1 Ti1 Cl2 168.64(17) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.08 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.032 _refine_diff_density_min -0.994 _refine_diff_density_rms 0.257