Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Andrew L. Johnson' _publ_contact_author_address ;Department of Chemistry, University of Bath, Claverton Down, Bath. BA2 7AY ; _publ_contact_author_email 'A.L. Johnson@bath.ac.uk' _publ_contact_author_phone '+44 (0) 1225 384467' loop_ _publ_author_name _publ_author_address M.G.Davidson ;Department of Chemistry, University of Bath, Claverton Down, Bath. BA2 7AY ; M.F.Mahon ;Department of Chemistry, University of Bath, Claverton Down, Bath. BA2 7AY ; 'Andrew Johnson' ; ? ; _publ_section_title ; Reactivity of Boranes with the Titanium (IV) Alkoxide Complex [Ti(OiPr)(OC6Me2H2CH2)3N]; Formation of the Titanium (IV) Tetrahydroborate Complex [Ti{BH4}(OC6Me2H2CH2)3N] by Alkoxide/Hydride Exchange, and the Lewis Acid Adduct [Ti(OC6Me2H2CH2)3N][HO.B(C6F5)3] ; data_Compound-3 _database_code_depnum_ccdc_archive 'CCDC 648697' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H42 B N O3 Ti' _chemical_formula_weight 571.40 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' B B 0.0013 0.0007 '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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'R -3' _symmetry_int_tables_number 148 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 14.1580(2) _cell_length_b 14.1580(2) _cell_length_c 26.3930(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4581.66(14) _cell_formula_units_Z 6 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 23103 _cell_measurement_theta_min 3.69 _cell_measurement_theta_max 27.46 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 0.314 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6092 _exptl_absorpt_correction_T_max 0.8586 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23103 _diffrn_reflns_av_R_equivalents 0.0547 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 27.46 _reflns_number_total 2311 _reflns_number_gt 1803 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo and Scalepack (otwinowski&Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (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^)+(0.0646P)^2^+7.1940P] 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 0.0011(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2311 _refine_ls_number_parameters 137 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0670 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1343 _refine_ls_wR_factor_gt 0.1232 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.661 _refine_ls_shift/su_max 0.127 _refine_ls_shift/su_mean 0.027 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 0.0000 0.0000 0.16769(3) 0.0318(3) Uani 1 3 d S . . O1 O 0.04064(19) 0.14266(18) 0.17815(8) 0.0372(6) Uani 1 1 d . . . N1 N 0.0000 0.0000 0.25835(15) 0.0302(9) Uani 1 3 d S . . B1 B 0.0000 0.0000 0.0832(3) 0.0499(18) Uani 1 3 d S . . H1B H 0.0000 0.0000 0.043(3) 0.07(3) Uiso 1 3 d S . . H2B H -0.062(3) 0.018(4) 0.1003(18) 0.063(13) Uiso 1 1 d . . . C1 C 0.0201(3) 0.2026(2) 0.21235(12) 0.0342(7) Uani 1 1 d . . . C2 C -0.0156(3) 0.2728(3) 0.19528(13) 0.0395(8) Uani 1 1 d . . . C3 C -0.0367(3) 0.3309(3) 0.23176(14) 0.0433(8) Uani 1 1 d . . . H3 H -0.0624 0.3795 0.2221 0.052 Uiso 1 1 d R . . C4 C -0.0215(3) 0.3227(3) 0.28328(14) 0.0418(8) Uani 1 1 d . . . C5 C 0.0146(3) 0.2521(3) 0.29874(12) 0.0374(7) Uani 1 1 d . . . H5 H 0.0246 0.2447 0.3342 0.045 Uiso 1 1 d R . . C6 C 0.0353(3) 0.1910(2) 0.26342(11) 0.0333(7) Uani 1 1 d . . . C7 C -0.0319(4) 0.2819(3) 0.13966(14) 0.0514(9) Uani 1 1 d . . . H7A H -0.0551 0.3344 0.1347 0.062 Uiso 1 1 d R . . H7B H -0.0871 0.2121 0.1272 0.062 Uiso 1 1 d R . . H7C H 0.0349 0.3047 0.1216 0.062 Uiso 1 1 d R . . C8 C -0.0444(4) 0.3880(3) 0.32161(16) 0.0553(10) Uani 1 1 d . . . H8A H -0.0310 0.3719 0.3553 0.066 Uiso 1 1 d R . . H8B H -0.1190 0.3707 0.3188 0.066 Uiso 1 1 d R . . H8C H 0.0029 0.4642 0.3147 0.066 Uiso 1 1 d R . . C9 C 0.0739(2) 0.1138(2) 0.27850(9) 0.0328(7) Uani 1 1 d . . . H9A H 0.0752 0.1111 0.3148 0.039 Uiso 1 1 d R . . H9B H 0.1463 0.1414 0.2656 0.039 Uiso 1 1 d R . . C101 C -0.0703(2) -0.0627(2) 0.43279(9) 0.069(3) Uani 0.50 1 d PRD A -1 C102 C -0.1035(2) -0.0029(2) 0.42909(9) 0.068(3) Uani 0.50 1 d PRD A -1 C104 C 0.0514(2) 0.1426(2) 0.42819(9) 0.083(4) Uani 0.50 1 d PRD A -1 C103 C -0.0638(2) 0.0873(2) 0.42486(9) 0.089(3) Uani 0.50 1 d PRD A -1 C105 C 0.0915(2) 0.2029(2) 0.44414(9) 0.138(7) Uani 0.50 1 d PRD . . 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 0.0366(4) 0.0366(4) 0.0222(5) 0.000 0.000 0.0183(2) O1 0.0482(14) 0.0378(12) 0.0266(11) 0.0027(9) 0.0043(9) 0.0222(11) N1 0.0323(14) 0.0323(14) 0.026(2) 0.000 0.000 0.0162(7) B1 0.062(3) 0.062(3) 0.025(3) 0.000 0.000 0.0312(15) C1 0.0354(16) 0.0300(15) 0.0330(16) 0.0004(12) 0.0014(12) 0.0132(13) C2 0.0403(18) 0.0327(17) 0.0416(17) 0.0024(13) -0.0032(14) 0.0153(14) C3 0.0428(19) 0.0325(17) 0.055(2) -0.0001(14) -0.0025(15) 0.0190(15) C4 0.0411(18) 0.0314(17) 0.048(2) -0.0049(14) 0.0016(14) 0.0146(15) C5 0.0389(17) 0.0333(16) 0.0340(16) -0.0033(13) 0.0005(13) 0.0137(14) C6 0.0334(16) 0.0310(16) 0.0316(15) -0.0014(12) -0.0009(12) 0.0132(13) C7 0.063(2) 0.048(2) 0.046(2) 0.0071(16) -0.0061(17) 0.0298(19) C8 0.064(3) 0.044(2) 0.062(2) -0.0121(18) 0.0012(19) 0.030(2) C9 0.0361(16) 0.0336(16) 0.0265(14) -0.0025(12) -0.0030(12) 0.0158(13) C101 0.035(4) 0.086(7) 0.026(4) 0.015(4) -0.014(3) -0.015(4) C102 0.099(8) 0.104(8) 0.047(5) 0.039(5) 0.035(5) 0.084(7) C104 0.087(9) 0.124(12) 0.042(5) 0.022(7) 0.010(5) 0.056(9) C103 0.102(9) 0.101(9) 0.061(6) -0.007(6) -0.014(6) 0.049(8) C105 0.112(12) 0.072(9) 0.21(2) -0.037(10) -0.032(12) 0.029(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 O1 1.823(2) 3 ? Ti1 O1 1.823(2) . ? Ti1 O1 1.823(2) 2 ? Ti1 B1 2.231(7) . ? Ti1 N1 2.393(4) . ? Ti1 H2B 2.06(5) . ? O1 C1 1.367(4) . ? N1 C9 1.512(3) 3 ? N1 C9 1.512(3) . ? N1 C9 1.512(3) 2 ? B1 H1B 1.06(8) . ? B1 H2B 1.13(4) . ? C1 C6 1.388(4) . ? C1 C2 1.395(5) . ? C2 C3 1.392(5) . ? C2 C7 1.502(5) . ? C3 C4 1.391(5) . ? C3 H3 0.9599 . ? C4 C5 1.393(5) . ? C4 C8 1.511(5) . ? C5 C6 1.398(4) . ? C5 H5 0.9600 . ? C6 C9 1.500(4) . ? C7 H7A 0.9600 . ? C7 H7B 0.9602 . ? C7 H7C 0.9602 . ? C8 H8A 0.9599 . ? C8 H8B 0.9602 . ? C8 H8C 0.9599 . ? C9 H9A 0.9602 . ? C9 H9B 0.9598 . ? C101 C102 1.1600 . ? C101 C105 1.672(4) 2 ? C102 C103 1.1153 . ? C102 C105 1.527(4) 2 ? C104 C105 0.8619 . ? C104 C103 1.4152 . ? C105 C102 1.527(4) 3 ? C105 C101 1.672(4) 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 O1 Ti1 O1 117.75(4) 3 . ? O1 Ti1 O1 117.75(3) 3 2 ? O1 Ti1 O1 117.75(3) . 2 ? O1 Ti1 B1 98.71(7) 3 . ? O1 Ti1 B1 98.71(7) . . ? O1 Ti1 B1 98.71(7) 2 . ? O1 Ti1 N1 81.29(7) 3 . ? O1 Ti1 N1 81.29(7) . . ? O1 Ti1 N1 81.29(7) 2 . ? B1 Ti1 N1 180.0 . . ? O1 Ti1 H2B 128.8(12) 3 . ? O1 Ti1 H2B 84.9(12) . . ? O1 Ti1 H2B 81.7(12) 2 . ? B1 Ti1 H2B 30.1(12) . . ? N1 Ti1 H2B 149.9(12) . . ? C1 O1 Ti1 137.8(2) . . ? C9 N1 C9 108.33(18) 3 . ? C9 N1 C9 108.33(18) 3 2 ? C9 N1 C9 108.33(18) . 2 ? C9 N1 Ti1 110.59(17) 3 . ? C9 N1 Ti1 110.59(17) . . ? C9 N1 Ti1 110.59(17) 2 . ? Ti1 B1 H1B 180.000(4) . . ? Ti1 B1 H2B 66(2) . . ? H1B B1 H2B 114(2) . . ? O1 C1 C6 118.3(3) . . ? O1 C1 C2 119.6(3) . . ? C6 C1 C2 122.1(3) . . ? C3 C2 C1 117.3(3) . . ? C3 C2 C7 122.5(3) . . ? C1 C2 C7 120.2(3) . . ? C4 C3 C2 122.7(3) . . ? C4 C3 H3 116.7 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 118.3(3) . . ? C3 C4 C8 121.0(3) . . ? C5 C4 C8 120.8(3) . . ? C4 C5 C6 120.9(3) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.6 . . ? C1 C6 C5 118.8(3) . . ? C1 C6 C9 118.6(3) . . ? C5 C6 C9 122.6(3) . . ? C2 C7 H7A 109.1 . . ? C2 C7 H7B 109.0 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 110.3 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.4 . . ? C4 C8 H8A 110.2 . . ? C4 C8 H8B 109.7 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 108.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 N1 111.9(2) . . ? C6 C9 H9A 108.4 . . ? N1 C9 H9A 109.0 . . ? C6 C9 H9B 108.3 . . ? N1 C9 H9B 109.7 . . ? H9A C9 H9B 109.4 . . ? C102 C101 C105 62.23(16) . 2 ? C103 C102 C101 133.5 . . ? C103 C102 C105 149.43(17) . 2 ? C101 C102 C105 75.55(17) . 2 ? C105 C104 C103 125.8 . . ? C102 C103 C104 114.1 . . ? C104 C105 C102 43.87(15) . 3 ? C104 C105 C101 19.0 . 3 ? C102 C105 C101 42.22(11) 3 3 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.330 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.052 #===End data_Compound-4 _database_code_depnum_ccdc_archive 'CCDC 648698' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75 H83 N2 O6 Ti2' _chemical_formula_weight 1204.23 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' 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 10.1340(2) _cell_length_b 13.3940(2) _cell_length_c 13.7670(3) _cell_angle_alpha 66.7420(10) _cell_angle_beta 70.8950(10) _cell_angle_gamma 80.5040(10) _cell_volume 1620.87(5) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 30318 _cell_measurement_theta_min 3.76 _cell_measurement_theta_max 27.12 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 639 _exptl_absorpt_coefficient_mu 0.300 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9206 _exptl_absorpt_correction_T_max 0.9563 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30318 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 27.12 _reflns_number_total 7110 _reflns_number_gt 5402 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo and Scalepack (otwinowski&Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (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^)+(0.0557P)^2^+0.7596P] 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 0.011(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7110 _refine_ls_number_parameters 439 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1215 _refine_ls_wR_factor_gt 0.1102 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.118 _refine_ls_shift/su_mean 0.004 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 0.38784(3) 0.55587(3) 0.47262(3) 0.02477(12) Uani 1 1 d . . . N1 N 0.33637(15) 0.72803(12) 0.37422(12) 0.0242(3) Uani 1 1 d . . . O1 O 0.36908(14) 0.52092(10) 0.35890(11) 0.0306(3) Uani 1 1 d . . . O2 O 0.28193(14) 0.59460(10) 0.59318(10) 0.0303(3) Uani 1 1 d . . . O3 O 0.57923(13) 0.60284(10) 0.43573(10) 0.0265(3) Uani 1 1 d . . . C1 C 0.3733(2) 0.74803(15) 0.25377(15) 0.0274(4) Uani 1 1 d . . . H1A H 0.4750 0.7335 0.2262 0.033 Uiso 1 1 calc R . . H1B H 0.3528 0.8257 0.2137 0.033 Uiso 1 1 calc R . . C2 C 0.18279(19) 0.74997(15) 0.41614(15) 0.0274(4) Uani 1 1 d . . . H2A H 0.1323 0.6946 0.4130 0.033 Uiso 1 1 calc R . . H2B H 0.1572 0.8218 0.3660 0.033 Uiso 1 1 calc R . . C3 C 0.41255(19) 0.80476(15) 0.38830(16) 0.0275(4) Uani 1 1 d . . . H3A H 0.3866 0.7922 0.4679 0.033 Uiso 1 1 calc R . . H3B H 0.3803 0.8798 0.3502 0.033 Uiso 1 1 calc R . . C11 C 0.30193(19) 0.56641(15) 0.28033(15) 0.0269(4) Uani 1 1 d . . . C12 C 0.2376(2) 0.49962(16) 0.25378(16) 0.0311(4) Uani 1 1 d . . . C13 C 0.1686(2) 0.54988(17) 0.17270(17) 0.0354(5) Uani 1 1 d . . . H13 H 0.1255 0.5055 0.1533 0.042 Uiso 1 1 calc R . . C14 C 0.1604(2) 0.66166(18) 0.11947(17) 0.0353(5) Uani 1 1 d . . . C15 C 0.2250(2) 0.72566(16) 0.14822(16) 0.0306(4) Uani 1 1 d . . . H15 H 0.2203 0.8025 0.1129 0.037 Uiso 1 1 calc R . . C16 C 0.29612(19) 0.67919(15) 0.22754(15) 0.0271(4) Uani 1 1 d . . . C17 C 0.2427(3) 0.37871(17) 0.3121(2) 0.0448(5) Uani 1 1 d . . . H17A H 0.3389 0.3533 0.3130 0.067 Uiso 1 1 calc R . . H17B H 0.2110 0.3441 0.2733 0.067 Uiso 1 1 calc R . . H17C H 0.1817 0.3597 0.3881 0.067 Uiso 1 1 calc R . . C18 C 0.0842(3) 0.7138(2) 0.0325(2) 0.0547(7) Uani 1 1 d . . . H18A H 0.1517 0.7306 -0.0410 0.082 Uiso 1 1 calc R . . H18B H 0.0351 0.7811 0.0398 0.082 Uiso 1 1 calc R . . H18C H 0.0165 0.6636 0.0424 0.082 Uiso 1 1 calc R . . C21 C 0.1824(2) 0.66899(15) 0.61632(16) 0.0286(4) Uani 1 1 d . . . C22 C 0.1299(2) 0.66456(17) 0.72580(16) 0.0341(4) Uani 1 1 d . . . C23 C 0.0295(2) 0.74313(17) 0.74792(17) 0.0370(5) Uani 1 1 d . . . H23 H -0.0064 0.7410 0.8216 0.044 Uiso 1 1 calc R . . C24 C -0.0203(2) 0.82464(16) 0.66628(17) 0.0335(4) Uani 1 1 d . . . C25 C 0.0330(2) 0.82645(16) 0.55909(17) 0.0310(4) Uani 1 1 d . . . H25 H 0.0003 0.8818 0.5022 0.037 Uiso 1 1 calc R . . C26 C 0.13328(19) 0.74934(15) 0.53257(15) 0.0269(4) Uani 1 1 d . . . C27 C 0.1830(3) 0.5752(2) 0.81346(18) 0.0510(6) Uani 1 1 d . . . H27A H 0.1723 0.5047 0.8113 0.076 Uiso 1 1 calc R . . H27B H 0.1294 0.5776 0.8861 0.076 Uiso 1 1 calc R . . H27C H 0.2819 0.5848 0.8002 0.076 Uiso 1 1 calc R . . C28 C -0.1317(3) 0.90754(19) 0.6943(2) 0.0481(6) Uani 1 1 d . . . H28A H -0.1592 0.9548 0.6282 0.072 Uiso 1 1 calc R . . H28B H -0.0945 0.9516 0.7210 0.072 Uiso 1 1 calc R . . H28C H -0.2133 0.8698 0.7520 0.072 Uiso 1 1 calc R . . C31 C 0.64784(19) 0.69897(15) 0.37659(15) 0.0268(4) Uani 1 1 d . . . C32 C 0.7939(2) 0.69844(16) 0.34944(16) 0.0308(4) Uani 1 1 d . . . C33 C 0.8587(2) 0.79713(17) 0.28559(17) 0.0357(5) Uani 1 1 d . . . H33 H 0.9577 0.7975 0.2662 0.043 Uiso 1 1 calc R . . C34 C 0.7855(2) 0.89432(17) 0.24929(18) 0.0374(5) Uani 1 1 d . . . C35 C 0.6405(2) 0.89302(16) 0.28138(17) 0.0334(4) Uani 1 1 d . . . H35 H 0.5882 0.9594 0.2590 0.040 Uiso 1 1 calc R . . C36 C 0.5697(2) 0.79684(15) 0.34559(15) 0.0273(4) Uani 1 1 d . . . C37 C 0.8809(2) 0.59631(17) 0.38758(19) 0.0377(5) Uani 1 1 d . . . H37A H 0.8741 0.5464 0.3532 0.056 Uiso 1 1 calc R . . H37B H 0.8467 0.5613 0.4681 0.056 Uiso 1 1 calc R . . H37C H 0.9787 0.6146 0.3663 0.056 Uiso 1 1 calc R . . C38 C 0.8605(3) 0.9998(2) 0.1775(2) 0.0566(7) Uani 1 1 d . . . H38A H 0.9604 0.9834 0.1493 0.085 Uiso 1 1 calc R . . H38B H 0.8477 1.0449 0.2215 0.085 Uiso 1 1 calc R . . H38C H 0.8216 1.0391 0.1153 0.085 Uiso 1 1 calc R . . C101 C 0.5878(4) 0.7308(2) 0.9744(3) 0.0514(11) Uani 0.60 1 d PG A 1 C102 C 0.6849(5) 0.7221(3) 1.0293(4) 0.072(3) Uani 0.60 1 d PG A 1 H102 H 0.7247 0.6529 1.0638 0.086 Uiso 0.60 1 calc PR A 1 C103 C 0.7237(5) 0.8147(4) 1.0336(4) 0.078(3) Uani 0.60 1 d PG A 1 H103 H 0.7901 0.8088 1.0711 0.094 Uiso 0.60 1 calc PR A 1 C104 C 0.6654(5) 0.9160(3) 0.9832(4) 0.0661(16) Uani 0.60 1 d PG A 1 H104 H 0.6920 0.9793 0.9862 0.079 Uiso 0.60 1 calc PR A 1 C105 C 0.5683(4) 0.9247(2) 0.9283(3) 0.0587(14) Uani 0.60 1 d PG A 1 H105 H 0.5285 0.9939 0.8938 0.070 Uiso 0.60 1 calc PR A 1 C106 C 0.5295(4) 0.8321(3) 0.9239(3) 0.0478(15) Uani 0.60 1 d PG A 1 H106 H 0.4631 0.8381 0.8864 0.057 Uiso 0.60 1 calc PR A 1 C107 C 0.5402(10) 0.6313(6) 0.9707(9) 0.100(4) Uani 0.60 1 d P A 1 H10A H 0.6208 0.5815 0.9583 0.150 Uiso 0.60 1 calc PR A 1 H10B H 0.4976 0.6534 0.9104 0.150 Uiso 0.60 1 calc PR A 1 H10C H 0.4714 0.5945 1.0410 0.150 Uiso 0.60 1 calc PR A 1 C201 C 0.6535(7) 0.8144(9) 0.9848(6) 0.127(6) Uani 0.40 1 d PG B 2 C202 C 0.5621(7) 0.8623(6) 0.9210(6) 0.061(3) Uani 0.40 1 d PG B 2 H202 H 0.5496 0.9393 0.8918 0.073 Uiso 0.40 1 calc PR B 2 C203 C 0.4889(6) 0.7977(6) 0.9000(5) 0.083(3) Uani 0.40 1 d PG B 2 H203 H 0.4264 0.8305 0.8565 0.100 Uiso 0.40 1 calc PR B 2 C204 C 0.5071(9) 0.6852(6) 0.9428(7) 0.121(6) Uani 0.40 1 d PG B 2 H204 H 0.4570 0.6410 0.9284 0.145 Uiso 0.40 1 calc PR B 2 C205 C 0.5985(11) 0.6372(6) 1.0066(8) 0.143(11) Uani 0.40 1 d PG B 2 H205 H 0.6109 0.5603 1.0358 0.171 Uiso 0.40 1 calc PR B 2 C206 C 0.6717(9) 0.7018(10) 1.0276(6) 0.129(9) Uani 0.40 1 d PG B 2 H206 H 0.7342 0.6690 1.0711 0.154 Uiso 0.40 1 calc PR B 2 C207 C 0.7202(18) 0.8714(13) 1.0015(14) 0.109(5) Uani 0.40 1 d P B 2 H20A H 0.8170 0.8734 0.9547 0.163 Uiso 0.40 1 calc PR B 2 H20B H 0.7187 0.8409 1.0793 0.163 Uiso 0.40 1 calc PR B 2 H20C H 0.6780 0.9453 0.9840 0.163 Uiso 0.40 1 calc PR B 2 C301 C 0.5330(7) 1.0972(5) 0.4215(5) 0.1200(18) Uani 1 1 d . . 2 C302 C 0.6373(7) 1.0234(7) 0.4607(7) 0.149(3) Uani 1 1 d . C 2 H302 H 0.7318 1.0441 0.4323 0.179 Uiso 1 1 calc R C 2 C303 C 0.6052(7) 0.9271(7) 0.5355(7) 0.158(3) Uani 1 1 d . . 2 H303 H 0.6754 0.8756 0.5594 0.189 Uiso 1 1 calc R . 2 C307 C 0.5612(8) 1.1847(6) 0.3510(6) 0.0758(19) Uani 0.50 1 d P D 2 H30A H 0.5122 1.1987 0.2960 0.114 Uiso 0.50 1 calc PR D 2 H30B H 0.6623 1.1866 0.3154 0.114 Uiso 0.50 1 calc PR D 2 H30C H 0.5323 1.2406 0.3840 0.114 Uiso 0.50 1 calc PR D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.02410(19) 0.02366(19) 0.02752(19) -0.00890(14) -0.00940(14) -0.00076(13) N1 0.0232(8) 0.0264(8) 0.0249(8) -0.0109(7) -0.0068(6) -0.0027(6) O1 0.0340(7) 0.0277(7) 0.0346(7) -0.0119(6) -0.0160(6) 0.0005(6) O2 0.0332(7) 0.0290(7) 0.0282(7) -0.0099(6) -0.0110(6) 0.0029(6) O3 0.0245(6) 0.0237(6) 0.0307(7) -0.0074(5) -0.0095(5) -0.0027(5) C1 0.0285(10) 0.0271(10) 0.0250(9) -0.0076(8) -0.0066(8) -0.0040(8) C2 0.0259(9) 0.0275(10) 0.0297(10) -0.0099(8) -0.0107(8) 0.0007(8) C3 0.0293(10) 0.0228(9) 0.0335(10) -0.0113(8) -0.0117(8) -0.0013(7) C11 0.0233(9) 0.0327(10) 0.0256(9) -0.0126(8) -0.0060(7) -0.0013(8) C12 0.0314(10) 0.0331(10) 0.0318(10) -0.0151(9) -0.0072(8) -0.0044(8) C13 0.0348(11) 0.0420(12) 0.0376(11) -0.0202(10) -0.0117(9) -0.0067(9) C14 0.0353(11) 0.0442(12) 0.0319(10) -0.0162(9) -0.0141(9) -0.0016(9) C15 0.0319(10) 0.0321(10) 0.0268(9) -0.0098(8) -0.0079(8) -0.0022(8) C16 0.0249(9) 0.0315(10) 0.0259(9) -0.0129(8) -0.0050(8) -0.0023(8) C17 0.0579(15) 0.0343(12) 0.0493(13) -0.0152(11) -0.0216(12) -0.0077(10) C18 0.0698(17) 0.0540(15) 0.0568(15) -0.0199(13) -0.0407(14) -0.0003(13) C21 0.0290(10) 0.0274(10) 0.0303(10) -0.0107(8) -0.0080(8) -0.0039(8) C22 0.0393(11) 0.0352(11) 0.0290(10) -0.0122(9) -0.0102(9) -0.0026(9) C23 0.0397(12) 0.0422(12) 0.0310(10) -0.0189(10) -0.0045(9) -0.0049(9) C24 0.0304(10) 0.0322(11) 0.0373(11) -0.0164(9) -0.0029(9) -0.0043(8) C25 0.0277(10) 0.0296(10) 0.0349(10) -0.0106(9) -0.0086(8) -0.0030(8) C26 0.0242(9) 0.0283(10) 0.0293(10) -0.0114(8) -0.0066(8) -0.0037(7) C27 0.0664(16) 0.0538(15) 0.0318(11) -0.0162(11) -0.0176(11) 0.0083(12) C28 0.0486(14) 0.0447(13) 0.0455(13) -0.0225(11) -0.0018(11) 0.0041(11) C31 0.0279(9) 0.0262(9) 0.0274(9) -0.0089(8) -0.0083(8) -0.0061(8) C32 0.0284(10) 0.0333(11) 0.0341(10) -0.0145(9) -0.0099(8) -0.0028(8) C33 0.0269(10) 0.0404(12) 0.0406(11) -0.0145(10) -0.0080(9) -0.0079(9) C34 0.0352(11) 0.0349(11) 0.0416(12) -0.0097(10) -0.0108(9) -0.0119(9) C35 0.0362(11) 0.0262(10) 0.0396(11) -0.0098(9) -0.0147(9) -0.0036(8) C36 0.0291(10) 0.0269(10) 0.0289(9) -0.0103(8) -0.0107(8) -0.0039(8) C37 0.0244(10) 0.0382(12) 0.0488(13) -0.0138(10) -0.0112(9) -0.0013(8) C38 0.0457(14) 0.0404(14) 0.0709(18) -0.0041(13) -0.0131(13) -0.0181(11) C101 0.047(3) 0.048(3) 0.042(2) -0.015(2) 0.008(2) -0.003(2) C102 0.073(6) 0.054(4) 0.048(5) 0.000(3) -0.010(4) 0.041(3) C103 0.050(3) 0.131(8) 0.064(4) -0.050(5) -0.024(3) 0.022(4) C104 0.060(4) 0.068(4) 0.067(4) -0.038(3) 0.007(3) -0.011(3) C105 0.069(3) 0.052(3) 0.048(3) -0.016(2) -0.006(2) -0.010(3) C106 0.036(3) 0.068(4) 0.042(3) -0.021(3) -0.007(2) -0.014(3) C107 0.087(6) 0.056(5) 0.113(7) -0.038(5) 0.035(5) -0.001(4) C201 0.061(6) 0.26(2) 0.083(8) -0.112(11) 0.032(6) -0.060(9) C202 0.033(4) 0.091(8) 0.037(4) -0.005(5) -0.012(3) 0.011(5) C203 0.066(6) 0.095(8) 0.061(5) -0.016(5) -0.006(4) 0.014(5) C204 0.109(9) 0.100(10) 0.071(7) -0.014(7) 0.025(6) 0.063(8) C205 0.082(12) 0.127(16) 0.108(12) 0.020(11) 0.014(9) 0.040(11) C206 0.093(15) 0.104(11) 0.105(16) -0.009(11) 0.031(12) 0.017(10) C207 0.100(10) 0.141(14) 0.092(10) -0.074(10) -0.029(9) 0.061(9) C301 0.148(5) 0.150(4) 0.145(4) -0.119(4) -0.087(4) 0.036(4) C302 0.106(4) 0.241(7) 0.225(8) -0.205(7) -0.087(5) 0.051(5) C303 0.111(5) 0.246(8) 0.247(9) -0.206(8) -0.099(6) 0.046(6) C307 0.097(5) 0.076(4) 0.084(5) -0.039(4) -0.059(4) 0.016(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O2 1.8724(13) . ? Ti1 O1 1.8734(13) . ? Ti1 O3 1.9801(12) . ? Ti1 O3 2.0361(13) 2_666 ? Ti1 N1 2.2412(15) . ? Ti1 Ti1 2.6616(6) 2_666 ? N1 C3 1.486(2) . ? N1 C2 1.496(2) . ? N1 C1 1.496(2) . ? O1 C11 1.352(2) . ? O2 C21 1.349(2) . ? O3 C31 1.379(2) . ? O3 Ti1 2.0361(13) 2_666 ? C1 C16 1.509(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C26 1.512(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C36 1.508(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C11 C16 1.395(3) . ? C11 C12 1.402(3) . ? C12 C13 1.397(3) . ? C12 C17 1.498(3) . ? C13 C14 1.385(3) . ? C13 H13 0.9500 . ? C14 C15 1.394(3) . ? C14 C18 1.511(3) . ? C15 C16 1.389(3) . ? C15 H15 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C21 C26 1.398(3) . ? C21 C22 1.405(3) . ? C22 C23 1.390(3) . ? C22 C27 1.500(3) . ? C23 C24 1.389(3) . ? C23 H23 0.9500 . ? C24 C25 1.387(3) . ? C24 C28 1.515(3) . ? C25 C26 1.393(3) . ? C25 H25 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C31 C36 1.401(3) . ? C31 C32 1.402(3) . ? C32 C33 1.394(3) . ? C32 C37 1.504(3) . ? C33 C34 1.380(3) . ? C33 H33 0.9500 . ? C34 C35 1.390(3) . ? C34 C38 1.519(3) . ? C35 C36 1.395(3) . ? C35 H35 0.9500 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C101 C102 1.3900 . ? C101 C106 1.3900 . ? C101 C107 1.515(9) . ? C102 C103 1.3900 . ? C102 H102 0.9500 . ? C103 C104 1.3900 . ? C103 H103 0.9500 . ? C104 C105 1.3900 . ? C104 H104 0.9500 . ? C105 C106 1.3900 . ? C105 H105 0.9500 . ? C106 H106 0.9500 . ? C107 H10A 0.9800 . ? C107 H10B 0.9800 . ? C107 H10C 0.9800 . ? C201 C207 1.226(17) . ? C201 C202 1.3900 . ? C201 C206 1.3900 . ? C202 C203 1.3900 . ? C202 H202 0.9500 . ? C203 C204 1.3900 . ? C203 H203 0.9500 . ? C204 C205 1.3900 . ? C204 H204 0.9500 . ? C205 C206 1.3900 . ? C205 H205 0.9500 . ? C206 H206 0.9500 . ? C207 H20A 0.9800 . ? C207 H20B 0.9800 . ? C207 H20C 0.9800 . ? C301 C307 1.195(8) . ? C301 C303 1.368(9) 2_676 ? C301 C302 1.412(8) . ? C302 C303 1.304(9) . ? C302 H302 0.9500 . ? C303 C301 1.368(9) 2_676 ? C303 H303 0.9500 . ? C307 H30A 0.9800 . ? C307 H30B 0.9800 . ? C307 H30C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ti1 O1 141.67(6) . . ? O2 Ti1 O3 105.71(6) . . ? O1 Ti1 O3 110.43(6) . . ? O2 Ti1 O3 95.39(5) . 2_666 ? O1 Ti1 O3 92.57(5) . 2_666 ? O3 Ti1 O3 97.00(5) . 2_666 ? O2 Ti1 N1 83.42(5) . . ? O1 Ti1 N1 86.11(5) . . ? O3 Ti1 N1 86.92(5) . . ? O3 Ti1 N1 176.08(5) 2_666 . ? O2 Ti1 Ti1 105.86(4) . 2_666 ? O1 Ti1 Ti1 107.10(4) . 2_666 ? O3 Ti1 Ti1 49.40(4) . 2_666 ? O3 Ti1 Ti1 47.60(4) 2_666 2_666 ? N1 Ti1 Ti1 136.32(4) . 2_666 ? C3 N1 C2 108.65(14) . . ? C3 N1 C1 108.57(14) . . ? C2 N1 C1 108.97(14) . . ? C3 N1 Ti1 110.41(11) . . ? C2 N1 Ti1 108.25(11) . . ? C1 N1 Ti1 111.93(11) . . ? C11 O1 Ti1 135.61(12) . . ? C21 O2 Ti1 139.60(12) . . ? C31 O3 Ti1 135.98(11) . . ? C31 O3 Ti1 141.02(11) . 2_666 ? Ti1 O3 Ti1 83.00(5) . 2_666 ? N1 C1 C16 113.87(15) . . ? N1 C1 H1A 108.8 . . ? C16 C1 H1A 108.8 . . ? N1 C1 H1B 108.8 . . ? C16 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? N1 C2 C26 114.96(15) . . ? N1 C2 H2A 108.5 . . ? C26 C2 H2A 108.5 . . ? N1 C2 H2B 108.5 . . ? C26 C2 H2B 108.5 . . ? H2A C2 H2B 107.5 . . ? N1 C3 C36 115.63(15) . . ? N1 C3 H3A 108.4 . . ? C36 C3 H3A 108.4 . . ? N1 C3 H3B 108.4 . . ? C36 C3 H3B 108.4 . . ? H3A C3 H3B 107.4 . . ? O1 C11 C16 119.68(16) . . ? O1 C11 C12 119.54(17) . . ? C16 C11 C12 120.78(17) . . ? C13 C12 C11 117.74(18) . . ? C13 C12 C17 121.90(18) . . ? C11 C12 C17 120.36(18) . . ? C14 C13 C12 122.73(18) . . ? C14 C13 H13 118.6 . . ? C12 C13 H13 118.6 . . ? C13 C14 C15 118.02(18) . . ? C13 C14 C18 121.57(19) . . ? C15 C14 C18 120.4(2) . . ? C16 C15 C14 121.26(19) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C11 119.47(17) . . ? C15 C16 C1 121.23(17) . . ? C11 C16 C1 119.24(16) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O2 C21 C26 120.48(17) . . ? O2 C21 C22 118.81(17) . . ? C26 C21 C22 120.72(18) . . ? C23 C22 C21 118.11(19) . . ? C23 C22 C27 123.02(18) . . ? C21 C22 C27 118.86(19) . . ? C24 C23 C22 122.50(19) . . ? C24 C23 H23 118.8 . . ? C22 C23 H23 118.8 . . ? C25 C24 C23 118.03(18) . . ? C25 C24 C28 121.2(2) . . ? C23 C24 C28 120.77(19) . . ? C24 C25 C26 121.77(19) . . ? C24 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C25 C26 C21 118.86(17) . . ? C25 C26 C2 120.27(17) . . ? C21 C26 C2 120.81(16) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O3 C31 C36 119.20(16) . . ? O3 C31 C32 120.13(17) . . ? C36 C31 C32 120.67(17) . . ? C33 C32 C31 117.91(18) . . ? C33 C32 C37 119.67(18) . . ? C31 C32 C37 122.41(18) . . ? C34 C33 C32 122.90(19) . . ? C34 C33 H33 118.6 . . ? C32 C33 H33 118.6 . . ? C33 C34 C35 117.87(19) . . ? C33 C34 C38 121.3(2) . . ? C35 C34 C38 120.9(2) . . ? C34 C35 C36 121.81(19) . . ? C34 C35 H35 119.1 . . ? C36 C35 H35 119.1 . . ? C35 C36 C31 118.70(18) . . ? C35 C36 C3 118.11(17) . . ? C31 C36 C3 122.87(17) . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C38 H38A 109.5 . . ? C34 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C34 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C102 C101 C106 120.0 . . ? C102 C101 C107 121.4(5) . . ? C106 C101 C107 118.6(5) . . ? C103 C102 C101 120.0 . . ? C103 C102 H102 120.0 . . ? C101 C102 H102 120.0 . . ? C102 C103 C104 120.0 . . ? C102 C103 H103 120.0 . . ? C104 C103 H103 120.0 . . ? C103 C104 C105 120.0 . . ? C103 C104 H104 120.0 . . ? C105 C104 H104 120.0 . . ? C106 C105 C104 120.0 . . ? C106 C105 H105 120.0 . . ? C104 C105 H105 120.0 . . ? C105 C106 C101 120.0 . . ? C105 C106 H106 120.0 . . ? C101 C106 H106 120.0 . . ? C207 C201 C202 120.0(11) . . ? C207 C201 C206 120.0(11) . . ? C202 C201 C206 120.0 . . ? C201 C202 C203 120.0 . . ? C201 C202 H202 120.0 . . ? C203 C202 H202 120.0 . . ? C204 C203 C202 120.0 . . ? C204 C203 H203 120.0 . . ? C202 C203 H203 120.0 . . ? C203 C204 C205 120.0 . . ? C203 C204 H204 120.0 . . ? C205 C204 H204 120.0 . . ? C204 C205 C206 120.0 . . ? C204 C205 H205 120.0 . . ? C206 C205 H205 120.0 . . ? C205 C206 C201 120.0 . . ? C205 C206 H206 120.0 . . ? C201 C206 H206 120.0 . . ? C201 C207 H20A 109.5 . . ? C201 C207 H20B 109.5 . . ? H20A C207 H20B 109.5 . . ? C201 C207 H20C 109.5 . . ? H20A C207 H20C 109.5 . . ? H20B C207 H20C 109.5 . . ? C307 C301 C303 117.1(8) . 2_676 ? C307 C301 C302 121.4(8) . . ? C303 C301 C302 121.5(6) 2_676 . ? C303 C302 C301 120.6(8) . . ? C303 C302 H302 119.7 . . ? C301 C302 H302 119.7 . . ? C302 C303 C301 117.8(8) . 2_676 ? C302 C303 H303 121.1 . . ? C301 C303 H303 121.1 2_676 . ? C301 C307 H30A 109.5 . . ? C301 C307 H30B 109.5 . . ? H30A C307 H30B 109.5 . . ? C301 C307 H30C 109.5 . . ? H30A C307 H30C 109.5 . . ? H30B C307 H30C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.12 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.496 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.064 #===End data_Compound-5 _database_code_depnum_ccdc_archive 'CCDC 648699' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55.50 H43 B F15 N O4 Ti' _chemical_formula_weight 1131.62 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' B B 0.0013 0.0007 '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' 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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8900(5) _cell_length_b 14.5430(4) _cell_length_c 16.4190(7) _cell_angle_alpha 108.3880(10) _cell_angle_beta 100.7370(10) _cell_angle_gamma 99.759(3) _cell_volume 2566.42(17) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 48049 _cell_measurement_theta_min 3.55 _cell_measurement_theta_max 27.26 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1154 _exptl_absorpt_coefficient_mu 0.269 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9236 _exptl_absorpt_correction_T_max 0.9557 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48049 _diffrn_reflns_av_R_equivalents 0.0932 _diffrn_reflns_av_sigmaI/netI 0.1021 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 27.26 _reflns_number_total 11290 _reflns_number_gt 6259 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo and Scalepack (Otwinowski&Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (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^)+(0.0891P)^2^+3.3855P] 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 0.0032(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11290 _refine_ls_number_parameters 695 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1480 _refine_ls_R_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.2095 _refine_ls_wR_factor_gt 0.1727 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.80894(6) 0.15847(5) 0.30378(5) 0.0303(2) Uani 1 1 d . . . O1 O 0.8112(2) 0.04434(19) 0.32394(19) 0.0353(6) Uani 1 1 d . . . O2 O 0.8489(2) 0.1741(2) 0.20640(18) 0.0362(7) Uani 1 1 d . . . O3 O 0.8131(2) 0.26748(19) 0.39643(18) 0.0347(6) Uani 1 1 d . . . O4 O 0.6377(2) 0.1276(2) 0.2348(2) 0.0334(6) Uani 1 1 d . . . N1 N 1.0034(3) 0.1971(2) 0.3610(2) 0.0311(7) Uani 1 1 d . . . F42 F 0.3791(2) -0.12011(18) 0.13924(17) 0.0499(7) Uani 1 1 d . . . F43 F 0.3662(2) -0.26117(19) 0.2094(2) 0.0707(9) Uani 1 1 d . . . F44 F 0.4795(3) -0.2188(2) 0.3829(2) 0.0739(9) Uani 1 1 d . . . F45 F 0.6125(2) -0.0293(2) 0.48283(18) 0.0588(7) Uani 1 1 d . . . F46 F 0.6259(2) 0.11333(17) 0.41294(16) 0.0428(6) Uani 1 1 d . . . F52 F 0.5674(2) 0.29889(19) 0.23472(19) 0.0535(7) Uani 1 1 d . . . F53 F 0.5099(3) 0.4622(2) 0.3294(2) 0.0764(10) Uani 1 1 d . . . F54 F 0.3854(3) 0.4550(2) 0.4533(2) 0.0772(10) Uani 1 1 d . . . F55 F 0.3314(2) 0.2836(2) 0.48464(19) 0.0598(8) Uani 1 1 d . . . F56 F 0.3822(2) 0.11987(18) 0.38987(17) 0.0451(6) Uani 1 1 d . . . F62 F 0.5580(2) 0.1211(2) 0.06802(17) 0.0495(7) Uani 1 1 d . . . F63 F 0.3924(2) 0.0947(2) -0.07589(18) 0.0612(8) Uani 1 1 d . . . F64 F 0.1587(2) 0.0410(2) -0.08290(18) 0.0590(7) Uani 1 1 d . . . F65 F 0.0956(2) 0.0099(2) 0.06049(19) 0.0603(8) Uani 1 1 d . . . F66 F 0.25904(19) 0.03765(19) 0.20569(17) 0.0463(6) Uani 1 1 d . . . C1 C 1.0316(3) 0.1540(3) 0.4323(3) 0.0337(9) Uani 1 1 d . . . H1A H 1.1168 0.1798 0.4629 0.040 Uiso 1 1 calc R . . H1B H 0.9867 0.1766 0.4768 0.040 Uiso 1 1 calc R . . C2 C 1.0635(3) 0.1548(3) 0.2904(3) 0.0346(9) Uani 1 1 d . . . H2A H 1.1475 0.1627 0.3185 0.042 Uiso 1 1 calc R . . H2B H 1.0267 0.0823 0.2601 0.042 Uiso 1 1 calc R . . C3 C 1.0502(3) 0.3085(3) 0.3996(3) 0.0344(9) Uani 1 1 d . . . H3A H 1.1375 0.3244 0.4165 0.041 Uiso 1 1 calc R . . H3B H 1.0257 0.3366 0.3534 0.041 Uiso 1 1 calc R . . C11 C 0.8890(3) -0.0107(3) 0.3450(3) 0.0344(9) Uani 1 1 d . . . C12 C 0.8543(3) -0.1144(3) 0.3136(3) 0.0382(10) Uani 1 1 d . . . C13 C 0.9404(4) -0.1644(3) 0.3337(3) 0.0397(10) Uani 1 1 d . . . H13 H 0.9191 -0.2353 0.3136 0.048 Uiso 1 1 calc R . . C14 C 1.0551(4) -0.1144(3) 0.3817(3) 0.0371(10) Uani 1 1 d . . . C15 C 1.0848(3) -0.0098(3) 0.4139(3) 0.0363(9) Uani 1 1 d . . . H15 H 1.1628 0.0256 0.4483 0.044 Uiso 1 1 calc R . . C16 C 1.0026(3) 0.0424(3) 0.3966(3) 0.0329(9) Uani 1 1 d . . . C17 C 0.7313(4) -0.1709(3) 0.2571(4) 0.0502(12) Uani 1 1 d . . . H17A H 0.6732 -0.1461 0.2878 0.075 Uiso 1 1 calc R . . H17B H 0.7214 -0.2423 0.2469 0.075 Uiso 1 1 calc R . . H17C H 0.7194 -0.1612 0.2000 0.075 Uiso 1 1 calc R . . C18 C 1.1481(4) -0.1715(3) 0.3962(3) 0.0500(12) Uani 1 1 d . . . H18A H 1.1105 -0.2431 0.3745 0.075 Uiso 1 1 calc R . . H18B H 1.1869 -0.1486 0.4597 0.075 Uiso 1 1 calc R . . H18C H 1.2070 -0.1596 0.3637 0.075 Uiso 1 1 calc R . . C21 C 0.9456(3) 0.2086(3) 0.1796(3) 0.0347(9) Uani 1 1 d . . . C22 C 0.9326(3) 0.2492(3) 0.1131(3) 0.0364(9) Uani 1 1 d . . . C23 C 1.0351(4) 0.2893(3) 0.0941(3) 0.0425(10) Uani 1 1 d . . . H23 H 1.0283 0.3175 0.0490 0.051 Uiso 1 1 calc R . . C24 C 1.1474(4) 0.2899(4) 0.1388(3) 0.0460(11) Uani 1 1 d . . . C25 C 1.1552(4) 0.2458(3) 0.2019(3) 0.0392(10) Uani 1 1 d . . . H25 H 1.2308 0.2440 0.2320 0.047 Uiso 1 1 calc R . . C26 C 1.0563(3) 0.2041(3) 0.2228(3) 0.0347(9) Uani 1 1 d . . . C27 C 0.8121(4) 0.2491(3) 0.0649(3) 0.0402(10) Uani 1 1 d . . . H27A H 0.7652 0.1800 0.0339 0.060 Uiso 1 1 calc R . . H27B H 0.8196 0.2818 0.0217 0.060 Uiso 1 1 calc R . . H27C H 0.7729 0.2853 0.1076 0.060 Uiso 1 1 calc R . . C28 C 1.2577(4) 0.3367(5) 0.1190(4) 0.0658(15) Uani 1 1 d . . . H28A H 1.2584 0.4061 0.1255 0.099 Uiso 1 1 calc R . . H28B H 1.2587 0.2992 0.0581 0.099 Uiso 1 1 calc R . . H28C H 1.3274 0.3350 0.1605 0.099 Uiso 1 1 calc R . . C31 C 0.8887(3) 0.3371(3) 0.4745(3) 0.0328(9) Uani 1 1 d . . . C32 C 0.8431(3) 0.3818(3) 0.5448(3) 0.0355(9) Uani 1 1 d . . . C33 C 0.9255(4) 0.4501(3) 0.6221(3) 0.0383(10) Uani 1 1 d . . . H33 H 0.8975 0.4830 0.6713 0.046 Uiso 1 1 calc R . . C34 C 1.0459(4) 0.4716(3) 0.6298(3) 0.0409(10) Uani 1 1 d . . . C35 C 1.0866(4) 0.4251(3) 0.5577(3) 0.0380(10) Uani 1 1 d . . . H35 H 1.1689 0.4396 0.5619 0.046 Uiso 1 1 calc R . . C36 C 1.0084(3) 0.3571(3) 0.4785(3) 0.0332(9) Uani 1 1 d . . . C37 C 0.7134(4) 0.3559(3) 0.5386(3) 0.0436(10) Uani 1 1 d . . . H37A H 0.6692 0.3617 0.4845 0.065 Uiso 1 1 calc R . . H37B H 0.6969 0.4019 0.5906 0.065 Uiso 1 1 calc R . . H37C H 0.6893 0.2872 0.5366 0.065 Uiso 1 1 calc R . . C38 C 1.1331(4) 0.5455(4) 0.7148(3) 0.0538(12) Uani 1 1 d . . . H38A H 1.1836 0.5960 0.7008 0.081 Uiso 1 1 calc R . . H38B H 1.1821 0.5099 0.7422 0.081 Uiso 1 1 calc R . . H38C H 1.0898 0.5782 0.7561 0.081 Uiso 1 1 calc R . . C41 C 0.4988(3) 0.0058(3) 0.2737(3) 0.0327(9) Uani 1 1 d . . . C42 C 0.4368(3) -0.0918(3) 0.2256(3) 0.0389(10) Uani 1 1 d . . . C43 C 0.4283(4) -0.1663(3) 0.2613(4) 0.0489(12) Uani 1 1 d . . . C44 C 0.4857(4) -0.1458(4) 0.3474(4) 0.0493(12) Uani 1 1 d . . . C45 C 0.5528(4) -0.0515(4) 0.3978(3) 0.0445(11) Uani 1 1 d . . . C46 C 0.5581(3) 0.0204(3) 0.3602(3) 0.0376(10) Uani 1 1 d . . . C51 C 0.4822(3) 0.2009(3) 0.3087(3) 0.0348(9) Uani 1 1 d . . . C52 C 0.5109(4) 0.2918(3) 0.2974(3) 0.0430(11) Uani 1 1 d . . . C53 C 0.4807(4) 0.3779(3) 0.3458(4) 0.0562(14) Uani 1 1 d . . . C54 C 0.4197(4) 0.3736(4) 0.4075(4) 0.0525(13) Uani 1 1 d . . . C55 C 0.3903(4) 0.2866(4) 0.4223(3) 0.0474(12) Uani 1 1 d . . . C56 C 0.4205(3) 0.2023(3) 0.3729(3) 0.0383(10) Uani 1 1 d . . . C61 C 0.4168(3) 0.0791(3) 0.1443(3) 0.0344(9) Uani 1 1 d . . . C62 C 0.4422(4) 0.0921(3) 0.0701(3) 0.0409(10) Uani 1 1 d . . . C63 C 0.3590(4) 0.0800(3) -0.0069(3) 0.0446(11) Uani 1 1 d . . . C64 C 0.2417(4) 0.0518(3) -0.0097(3) 0.0443(11) Uani 1 1 d . . . C65 C 0.2094(3) 0.0375(3) 0.0618(3) 0.0422(11) Uani 1 1 d . . . C66 C 0.2967(4) 0.0512(3) 0.1361(3) 0.0388(10) Uani 1 1 d . . . B1 B 0.5101(4) 0.1014(3) 0.2405(3) 0.0313(10) Uani 1 1 d . . . C1T C 1.0126(6) 0.7322(5) 0.1368(4) 0.0686(15) Uani 1 1 d . . . C2T C 0.8891(5) 0.7084(5) 0.1095(4) 0.0761(17) Uani 1 1 d . . . H2T H 0.8497 0.7591 0.1057 0.091 Uiso 1 1 calc R . . C3T C 0.8257(7) 0.6146(7) 0.0888(4) 0.093(2) Uani 1 1 d . . . H3T H 0.7420 0.6004 0.0707 0.112 Uiso 1 1 calc R . . C4T C 0.8779(10) 0.5399(7) 0.0930(6) 0.117(3) Uani 1 1 d . . . H4T H 0.8318 0.4740 0.0780 0.141 Uiso 1 1 calc R . . C5T C 1.0000(12) 0.5615(7) 0.1195(7) 0.136(3) Uani 1 1 d . . . H5T H 1.0380 0.5096 0.1218 0.163 Uiso 1 1 calc R . . C6T C 1.0635(7) 0.6526(7) 0.1414(5) 0.099(2) Uani 1 1 d . . . H6T H 1.1469 0.6655 0.1611 0.119 Uiso 1 1 calc R . . C7T C 1.0811(7) 0.8332(5) 0.1578(5) 0.095(2) Uani 1 1 d . . . H7T1 H 1.1654 0.8360 0.1753 0.142 Uiso 1 1 calc R . . H7T2 H 1.0594 0.8794 0.2068 0.142 Uiso 1 1 calc R . . H7T3 H 1.0648 0.8523 0.1054 0.142 Uiso 1 1 calc R . . C11T C 0.5370(11) 0.3888(8) -0.0322(7) 0.112(5) Uiso 0.50 1 d PGU A -1 H11T H 0.5496 0.3301 -0.0717 0.134 Uiso 0.50 1 calc PR A -1 C12T C 0.5485(12) 0.4014(9) 0.0567(8) 0.119(7) Uiso 0.50 1 d PGU A -1 H12T H 0.5690 0.3512 0.0780 0.143 Uiso 0.50 1 calc PR A -1 C13T C 0.5301(11) 0.4873(10) 0.1145(6) 0.111(5) Uiso 0.50 1 d PGU A -1 H13T H 0.5380 0.4959 0.1752 0.133 Uiso 0.50 1 calc PR A -1 C14T C 0.5002(11) 0.5607(8) 0.0833(7) 0.116(7) Uiso 0.50 1 d PGDU A -1 H14T H 0.4876 0.6194 0.1228 0.140 Uiso 0.50 1 calc PR A -1 C15T C 0.4886(12) 0.5481(8) -0.0056(7) 0.100(4) Uiso 0.50 1 d PGU A -1 C16T C 0.5070(11) 0.4622(9) -0.0634(6) 0.101(6) Uiso 0.50 1 d PGDU A -1 H16T H 0.4991 0.4536 -0.1242 0.121 Uiso 0.50 1 calc PR A -1 C17T C 0.460(4) 0.621(3) -0.0297(17) 0.242(18) Uiso 0.50 1 d PD A -1 H17D H 0.4545 0.6047 -0.0932 0.363 Uiso 0.50 1 calc PR A -1 H17E H 0.5212 0.6832 0.0043 0.363 Uiso 0.50 1 calc PR A -1 H17F H 0.3842 0.6298 -0.0180 0.363 Uiso 0.50 1 calc PR A -1 H4 H 0.643(3) 0.132(2) 0.187(2) 0.002(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0214(3) 0.0296(4) 0.0371(4) 0.0117(3) 0.0018(3) 0.0058(3) O1 0.0235(13) 0.0329(15) 0.0479(17) 0.0150(13) 0.0037(12) 0.0080(11) O2 0.0226(13) 0.0399(16) 0.0404(16) 0.0120(13) -0.0003(12) 0.0070(12) O3 0.0236(13) 0.0320(15) 0.0424(17) 0.0091(13) 0.0012(12) 0.0071(11) O4 0.0235(14) 0.0411(17) 0.0374(18) 0.0193(14) 0.0032(12) 0.0078(12) N1 0.0258(16) 0.0287(17) 0.0389(19) 0.0134(15) 0.0058(14) 0.0066(13) F42 0.0428(14) 0.0363(14) 0.0534(17) 0.0051(12) -0.0057(12) 0.0062(11) F43 0.0487(16) 0.0349(15) 0.116(3) 0.0265(16) 0.0022(16) -0.0017(12) F44 0.0673(19) 0.0629(19) 0.111(3) 0.0595(19) 0.0202(18) 0.0131(15) F45 0.0567(17) 0.076(2) 0.0569(18) 0.0412(16) 0.0091(13) 0.0236(14) F46 0.0356(13) 0.0394(14) 0.0443(15) 0.0119(12) -0.0045(10) 0.0081(11) F52 0.0478(15) 0.0425(15) 0.0687(19) 0.0275(14) 0.0034(14) 0.0055(12) F53 0.075(2) 0.0353(16) 0.107(3) 0.0253(17) -0.0004(18) 0.0098(14) F54 0.0574(18) 0.0454(17) 0.100(2) -0.0061(16) -0.0038(17) 0.0258(14) F55 0.0427(15) 0.0692(19) 0.0577(18) 0.0059(15) 0.0109(13) 0.0233(13) F56 0.0384(13) 0.0480(15) 0.0541(16) 0.0217(13) 0.0138(11) 0.0152(11) F62 0.0318(13) 0.0711(18) 0.0466(15) 0.0259(14) 0.0065(11) 0.0096(12) F63 0.0571(17) 0.086(2) 0.0425(16) 0.0285(15) 0.0039(13) 0.0211(15) F64 0.0442(15) 0.0670(18) 0.0498(16) 0.0153(14) -0.0162(12) 0.0144(13) F65 0.0227(12) 0.077(2) 0.0671(19) 0.0219(16) -0.0085(12) 0.0059(12) F66 0.0252(12) 0.0607(16) 0.0507(16) 0.0206(13) 0.0045(11) 0.0095(11) C1 0.0267(19) 0.033(2) 0.040(2) 0.0159(19) 0.0001(17) 0.0074(16) C2 0.0240(19) 0.038(2) 0.043(2) 0.016(2) 0.0059(17) 0.0104(17) C3 0.0194(18) 0.034(2) 0.046(3) 0.0140(19) 0.0020(17) 0.0032(16) C11 0.028(2) 0.037(2) 0.044(2) 0.020(2) 0.0071(17) 0.0135(17) C12 0.031(2) 0.038(2) 0.050(3) 0.020(2) 0.0089(19) 0.0108(18) C13 0.041(2) 0.032(2) 0.050(3) 0.018(2) 0.012(2) 0.0108(18) C14 0.034(2) 0.037(2) 0.044(3) 0.020(2) 0.0082(19) 0.0128(18) C15 0.031(2) 0.041(2) 0.040(2) 0.020(2) 0.0061(18) 0.0104(18) C16 0.028(2) 0.035(2) 0.036(2) 0.0158(19) 0.0041(17) 0.0083(17) C17 0.036(2) 0.034(2) 0.074(3) 0.017(2) 0.006(2) 0.0059(19) C18 0.048(3) 0.044(3) 0.062(3) 0.025(2) 0.007(2) 0.018(2) C21 0.028(2) 0.035(2) 0.041(2) 0.0116(19) 0.0108(18) 0.0099(17) C22 0.033(2) 0.038(2) 0.036(2) 0.0107(19) 0.0065(18) 0.0093(18) C23 0.041(2) 0.045(3) 0.046(3) 0.022(2) 0.012(2) 0.010(2) C24 0.035(2) 0.055(3) 0.048(3) 0.019(2) 0.013(2) 0.006(2) C25 0.029(2) 0.041(2) 0.049(3) 0.018(2) 0.0074(19) 0.0102(18) C26 0.028(2) 0.035(2) 0.037(2) 0.0081(19) 0.0073(17) 0.0080(17) C27 0.036(2) 0.042(2) 0.039(2) 0.015(2) 0.0024(18) 0.0079(19) C28 0.042(3) 0.088(4) 0.079(4) 0.048(3) 0.016(3) 0.008(3) C31 0.033(2) 0.025(2) 0.036(2) 0.0103(18) 0.0000(17) 0.0055(16) C32 0.035(2) 0.029(2) 0.043(3) 0.016(2) 0.0052(19) 0.0085(17) C33 0.047(2) 0.027(2) 0.041(3) 0.0115(19) 0.010(2) 0.0105(18) C34 0.043(2) 0.030(2) 0.045(3) 0.015(2) 0.001(2) 0.0064(19) C35 0.036(2) 0.029(2) 0.046(3) 0.015(2) 0.0040(19) 0.0057(18) C36 0.028(2) 0.027(2) 0.043(2) 0.0146(19) 0.0032(17) 0.0033(16) C37 0.038(2) 0.044(3) 0.048(3) 0.013(2) 0.012(2) 0.014(2) C38 0.049(3) 0.044(3) 0.049(3) 0.003(2) -0.002(2) 0.004(2) C41 0.0197(18) 0.037(2) 0.040(2) 0.0123(19) 0.0055(17) 0.0082(16) C42 0.027(2) 0.038(2) 0.050(3) 0.016(2) 0.0038(19) 0.0086(18) C43 0.028(2) 0.035(3) 0.078(4) 0.018(2) 0.009(2) 0.0040(18) C44 0.037(2) 0.050(3) 0.078(4) 0.043(3) 0.018(2) 0.013(2) C45 0.037(2) 0.057(3) 0.050(3) 0.029(2) 0.011(2) 0.016(2) C46 0.027(2) 0.036(2) 0.051(3) 0.016(2) 0.0098(19) 0.0094(18) C51 0.0236(19) 0.032(2) 0.040(2) 0.0096(19) -0.0044(17) 0.0041(16) C52 0.033(2) 0.039(3) 0.050(3) 0.016(2) -0.001(2) 0.0048(19) C53 0.044(3) 0.028(2) 0.079(4) 0.017(2) -0.016(3) 0.003(2) C54 0.038(2) 0.042(3) 0.062(3) 0.002(2) -0.001(2) 0.017(2) C55 0.030(2) 0.054(3) 0.050(3) 0.010(2) 0.000(2) 0.016(2) C56 0.026(2) 0.036(2) 0.042(3) 0.004(2) -0.0045(18) 0.0105(17) C61 0.026(2) 0.029(2) 0.040(2) 0.0073(18) -0.0008(17) 0.0080(16) C62 0.034(2) 0.044(3) 0.041(3) 0.012(2) 0.0019(19) 0.0144(19) C63 0.047(3) 0.050(3) 0.034(2) 0.013(2) 0.003(2) 0.019(2) C64 0.036(2) 0.045(3) 0.038(3) 0.006(2) -0.0112(19) 0.016(2) C65 0.021(2) 0.044(3) 0.051(3) 0.011(2) -0.0059(18) 0.0081(18) C66 0.033(2) 0.041(2) 0.037(2) 0.009(2) 0.0042(18) 0.0112(18) B1 0.023(2) 0.032(2) 0.036(3) 0.012(2) 0.0018(18) 0.0061(18) C1T 0.078(4) 0.069(4) 0.053(3) 0.017(3) 0.025(3) 0.003(3) C2T 0.061(4) 0.103(5) 0.060(4) 0.027(4) 0.023(3) 0.006(3) C3T 0.088(5) 0.113(6) 0.063(4) 0.029(4) 0.022(4) -0.012(5) C4T 0.128(8) 0.081(6) 0.126(7) 0.046(5) 0.010(6) -0.012(5) C5T 0.175(11) 0.080(6) 0.146(9) 0.041(6) 0.023(8) 0.031(7) C6T 0.074(5) 0.117(7) 0.103(6) 0.037(5) 0.015(4) 0.027(5) C7T 0.107(5) 0.094(5) 0.075(5) 0.024(4) 0.038(4) -0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O1 1.795(3) . ? Ti1 O3 1.804(3) . ? Ti1 O2 1.819(3) . ? Ti1 O4 2.034(3) . ? Ti1 N1 2.227(3) . ? O1 C11 1.387(4) . ? O2 C21 1.378(5) . ? O3 C31 1.386(5) . ? O4 B1 1.528(5) . ? N1 C2 1.498(5) . ? N1 C3 1.500(5) . ? N1 C1 1.505(5) . ? F42 C42 1.350(5) . ? F43 C43 1.361(5) . ? F44 C44 1.362(5) . ? F45 C45 1.352(5) . ? F46 C46 1.363(5) . ? F52 C52 1.350(5) . ? F53 C53 1.339(5) . ? F54 C54 1.359(5) . ? F55 C55 1.351(6) . ? F56 C56 1.340(5) . ? F62 C62 1.380(5) . ? F63 C63 1.334(5) . ? F64 C64 1.352(5) . ? F65 C65 1.338(5) . ? F66 C66 1.359(5) . ? C1 C16 1.494(5) . ? C2 C26 1.497(6) . ? C3 C36 1.486(6) . ? C11 C12 1.388(6) . ? C11 C16 1.395(5) . ? C12 C13 1.401(6) . ? C12 C17 1.511(6) . ? C13 C14 1.383(6) . ? C14 C15 1.400(6) . ? C14 C18 1.518(6) . ? C15 C16 1.378(5) . ? C21 C22 1.392(6) . ? C21 C26 1.397(5) . ? C22 C23 1.392(6) . ? C22 C27 1.502(5) . ? C23 C24 1.396(6) . ? C24 C25 1.378(6) . ? C24 C28 1.512(6) . ? C25 C26 1.381(6) . ? C31 C32 1.387(6) . ? C31 C36 1.389(5) . ? C32 C33 1.403(6) . ? C32 C37 1.501(6) . ? C33 C34 1.386(6) . ? C34 C35 1.383(6) . ? C34 C38 1.521(6) . ? C35 C36 1.399(6) . ? C41 C42 1.380(6) . ? C41 C46 1.395(6) . ? C41 B1 1.640(6) . ? C42 C43 1.384(6) . ? C43 C44 1.363(7) . ? C44 C45 1.367(7) . ? C45 C46 1.370(6) . ? C51 C52 1.387(6) . ? C51 C56 1.390(6) . ? C51 B1 1.655(6) . ? C52 C53 1.399(7) . ? C53 C54 1.362(7) . ? C54 C55 1.364(7) . ? C55 C56 1.385(6) . ? C61 C62 1.370(6) . ? C61 C66 1.385(6) . ? C61 B1 1.653(6) . ? C62 C63 1.393(6) . ? C63 C64 1.373(6) . ? C64 C65 1.366(6) . ? C65 C66 1.382(6) . ? C1T C2T 1.401(8) . ? C1T C6T 1.411(10) . ? C1T C7T 1.452(8) . ? C2T C3T 1.344(9) . ? C3T C4T 1.354(11) . ? C4T C5T 1.385(13) . ? C5T C6T 1.309(11) . ? C11T C12T 1.3900 . ? C11T C16T 1.3900 . ? C12T C13T 1.3900 . ? C13T C14T 1.3900 . ? C14T C15T 1.3900 . ? C15T C17T 1.32(3) . ? C15T C16T 1.3900 . ? 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 O3 117.58(13) . . ? O1 Ti1 O2 120.20(13) . . ? O3 Ti1 O2 119.33(13) . . ? O1 Ti1 O4 100.56(11) . . ? O3 Ti1 O4 99.68(12) . . ? O2 Ti1 O4 86.82(12) . . ? O1 Ti1 N1 84.64(11) . . ? O3 Ti1 N1 84.19(12) . . ? O2 Ti1 N1 84.18(11) . . ? O4 Ti1 N1 170.98(13) . . ? C11 O1 Ti1 141.1(2) . . ? C21 O2 Ti1 140.9(2) . . ? C31 O3 Ti1 141.6(2) . . ? B1 O4 Ti1 143.5(3) . . ? C2 N1 C3 108.7(3) . . ? C2 N1 C1 108.3(3) . . ? C3 N1 C1 109.5(3) . . ? C2 N1 Ti1 110.2(2) . . ? C3 N1 Ti1 110.0(2) . . ? C1 N1 Ti1 110.1(2) . . ? C16 C1 N1 112.6(3) . . ? C26 C2 N1 112.7(3) . . ? C36 C3 N1 113.2(3) . . ? O1 C11 C12 120.5(3) . . ? O1 C11 C16 117.2(3) . . ? C12 C11 C16 122.3(3) . . ? C11 C12 C13 116.8(4) . . ? C11 C12 C17 121.7(3) . . ? C13 C12 C17 121.4(4) . . ? C14 C13 C12 122.5(4) . . ? C13 C14 C15 118.5(4) . . ? C13 C14 C18 120.9(4) . . ? C15 C14 C18 120.6(4) . . ? C16 C15 C14 120.9(4) . . ? C15 C16 C11 118.9(4) . . ? C15 C16 C1 121.8(3) . . ? C11 C16 C1 119.3(3) . . ? O2 C21 C22 120.5(3) . . ? O2 C21 C26 118.0(4) . . ? C22 C21 C26 121.5(4) . . ? C21 C22 C23 117.3(4) . . ? C21 C22 C27 120.5(4) . . ? C23 C22 C27 122.3(4) . . ? C22 C23 C24 122.6(4) . . ? C25 C24 C23 117.9(4) . . ? C25 C24 C28 120.5(4) . . ? C23 C24 C28 121.6(4) . . ? C24 C25 C26 121.9(4) . . ? C25 C26 C21 118.8(4) . . ? C25 C26 C2 122.4(4) . . ? C21 C26 C2 118.8(3) . . ? O3 C31 C32 119.6(3) . . ? O3 C31 C36 117.2(4) . . ? C32 C31 C36 123.2(4) . . ? C31 C32 C33 116.2(4) . . ? C31 C32 C37 121.5(4) . . ? C33 C32 C37 122.3(4) . . ? C34 C33 C32 122.8(4) . . ? C35 C34 C33 118.6(4) . . ? C35 C34 C38 119.8(4) . . ? C33 C34 C38 121.6(4) . . ? C34 C35 C36 121.1(4) . . ? C31 C36 C35 118.1(4) . . ? C31 C36 C3 120.0(3) . . ? C35 C36 C3 121.8(4) . . ? C42 C41 C46 113.3(4) . . ? C42 C41 B1 127.9(4) . . ? C46 C41 B1 118.9(3) . . ? F42 C42 C41 121.0(4) . . ? F42 C42 C43 115.7(4) . . ? C41 C42 C43 123.3(4) . . ? F43 C43 C44 119.9(4) . . ? F43 C43 C42 119.9(4) . . ? C44 C43 C42 120.1(4) . . ? F44 C44 C43 120.7(4) . . ? F44 C44 C45 119.7(4) . . ? C43 C44 C45 119.6(4) . . ? F45 C45 C44 120.9(4) . . ? F45 C45 C46 120.6(4) . . ? C44 C45 C46 118.5(4) . . ? F46 C46 C45 116.5(4) . . ? F46 C46 C41 118.4(3) . . ? C45 C46 C41 125.1(4) . . ? C52 C51 C56 114.0(4) . . ? C52 C51 B1 119.2(4) . . ? C56 C51 B1 126.4(3) . . ? F52 C52 C51 119.5(4) . . ? F52 C52 C53 116.9(4) . . ? C51 C52 C53 123.6(5) . . ? F53 C53 C54 121.2(5) . . ? F53 C53 C52 119.7(5) . . ? C54 C53 C52 119.1(4) . . ? F54 C54 C53 120.5(5) . . ? F54 C54 C55 119.5(5) . . ? C53 C54 C55 119.9(4) . . ? F55 C55 C54 119.5(4) . . ? F55 C55 C56 120.9(4) . . ? C54 C55 C56 119.6(5) . . ? F56 C56 C55 114.6(4) . . ? F56 C56 C51 121.7(4) . . ? C55 C56 C51 123.7(4) . . ? C62 C61 C66 113.0(4) . . ? C62 C61 B1 127.8(3) . . ? C66 C61 B1 119.0(4) . . ? C61 C62 F62 120.1(3) . . ? C61 C62 C63 125.3(4) . . ? F62 C62 C63 114.6(4) . . ? F63 C63 C64 121.0(4) . . ? F63 C63 C62 120.9(4) . . ? C64 C63 C62 118.0(4) . . ? F64 C64 C65 120.4(4) . . ? F64 C64 C63 119.5(4) . . ? C65 C64 C63 120.1(4) . . ? F65 C65 C64 121.2(4) . . ? F65 C65 C66 120.1(4) . . ? C64 C65 C66 118.7(4) . . ? F66 C66 C65 116.0(4) . . ? F66 C66 C61 119.2(3) . . ? C65 C66 C61 124.8(4) . . ? O4 B1 C41 105.8(3) . . ? O4 B1 C61 110.8(3) . . ? C41 B1 C61 113.8(3) . . ? O4 B1 C51 108.9(3) . . ? C41 B1 C51 113.9(3) . . ? C61 B1 C51 103.6(3) . . ? C2T C1T C6T 115.8(6) . . ? C2T C1T C7T 120.7(7) . . ? C6T C1T C7T 123.5(7) . . ? C3T C2T C1T 120.7(7) . . ? C2T C3T C4T 121.8(8) . . ? C3T C4T C5T 118.6(8) . . ? C6T C5T C4T 120.7(9) . . ? C5T C6T C1T 122.4(8) . . ? C12T C11T C16T 120.0 . . ? C11T C12T C13T 120.0 . . ? C12T C13T C14T 120.0 . . ? C15T C14T C13T 120.0 . . ? C17T C15T C16T 123.8(8) . . ? C17T C15T C14T 116.2(8) . . ? C16T C15T C14T 120.0 . . ? C15T C16T C11T 120.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 F62 0.82(3) 1.97(3) 2.691(4) 147(3) . _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.26 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.755 _refine_diff_density_min -0.532 _refine_diff_density_rms 0.095 #===End data_Compound-6 _database_code_depnum_ccdc_archive 'CCDC 648700' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H42 F10 O6 Ti2' _chemical_formula_weight 784.44 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 8.8980(3) _cell_length_b 16.8170(5) _cell_length_c 12.0480(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.5380(10) _cell_angle_gamma 90.00 _cell_volume 1791.11(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 31754 _cell_measurement_theta_min 3.87 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.536 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8346 _exptl_absorpt_correction_T_max 0.8912 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31754 _diffrn_reflns_av_R_equivalents 0.0942 _diffrn_reflns_av_sigmaI/netI 0.0612 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.87 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4084 _reflns_number_gt 2765 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (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^)+(0.0395P)^2^+0.7085P] 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 0.0033(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4084 _refine_ls_number_parameters 224 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0866 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1035 _refine_ls_wR_factor_gt 0.0877 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.51999(5) 0.08499(2) 0.06210(3) 0.02499(14) Uani 1 1 d . . . F2 F 0.22819(16) 0.00191(8) 0.14237(12) 0.0415(4) Uani 1 1 d . . . F3 F 0.11277(17) -0.01388(9) 0.33913(13) 0.0512(4) Uani 1 1 d . . . F4 F 0.26776(19) 0.04368(9) 0.53026(13) 0.0528(4) Uani 1 1 d . . . F5 F 0.53528(18) 0.12092(9) 0.52202(12) 0.0503(4) Uani 1 1 d . . . F6 F 0.64520(16) 0.14197(9) 0.32569(13) 0.0475(4) Uani 1 1 d . . . O1 O 0.43376(17) 0.03634(8) -0.07710(12) 0.0259(3) Uani 1 1 d . . . O2 O 0.44047(18) 0.18065(8) 0.04571(13) 0.0314(4) Uani 1 1 d . . . O3 O 0.71546(18) 0.10648(9) 0.08083(14) 0.0319(4) Uani 1 1 d . . . C1 C 0.4409(3) 0.07215(12) 0.22568(19) 0.0294(5) Uani 1 1 d . . . C2 C 0.3072(3) 0.03340(13) 0.2361(2) 0.0319(5) Uani 1 1 d . . . C3 C 0.2457(3) 0.02381(13) 0.3350(2) 0.0361(6) Uani 1 1 d . . . C4 C 0.3235(3) 0.05377(14) 0.4315(2) 0.0371(6) Uani 1 1 d . . . C5 C 0.4581(3) 0.09237(14) 0.4268(2) 0.0364(6) Uani 1 1 d . . . C6 C 0.5125(3) 0.10128(13) 0.3251(2) 0.0336(6) Uani 1 1 d . . . C21 C 0.3722(3) 0.25752(13) 0.0523(2) 0.0372(6) Uani 1 1 d . . . H21 H 0.2712 0.2570 0.0065 0.045 Uiso 1 1 calc R . . C23 C 0.4704(4) 0.31918(15) 0.0053(3) 0.0502(7) Uani 1 1 d . . . H23A H 0.5670 0.3231 0.0531 0.075 Uiso 1 1 calc R . . H23B H 0.4191 0.3708 0.0027 0.075 Uiso 1 1 calc R . . H23C H 0.4892 0.3037 -0.0703 0.075 Uiso 1 1 calc R . . C22 C 0.3498(3) 0.27418(15) 0.1723(2) 0.0472(7) Uani 1 1 d . . . H22A H 0.2878 0.2320 0.2000 0.071 Uiso 1 1 calc R . . H22B H 0.2988 0.3255 0.1771 0.071 Uiso 1 1 calc R . . H22C H 0.4484 0.2758 0.2177 0.071 Uiso 1 1 calc R . . C11 C 0.3307(3) 0.06670(13) -0.17007(19) 0.0329(6) Uani 1 1 d . . . H11 H 0.3128 0.0232 -0.2266 0.040 Uiso 1 1 calc R . . C12 C 0.1804(3) 0.08734(15) -0.1305(2) 0.0430(7) Uani 1 1 d . . . H12A H 0.1423 0.0413 -0.0923 0.064 Uiso 1 1 calc R . . H12B H 0.1080 0.1017 -0.1947 0.064 Uiso 1 1 calc R . . H12C H 0.1936 0.1323 -0.0786 0.064 Uiso 1 1 calc R . . C13 C 0.4034(3) 0.13521(14) -0.2245(2) 0.0431(7) Uani 1 1 d . . . H13A H 0.4196 0.1794 -0.1714 0.065 Uiso 1 1 calc R . . H13B H 0.3371 0.1526 -0.2906 0.065 Uiso 1 1 calc R . . H13C H 0.5009 0.1181 -0.2469 0.065 Uiso 1 1 calc R . . C31 C 0.8143(3) 0.17408(14) 0.0843(2) 0.0410(6) Uani 1 1 d . . . H31 H 0.7652 0.2198 0.1192 0.049 Uiso 1 1 calc R . . C32 C 0.9584(3) 0.15284(19) 0.1561(3) 0.0632(9) Uani 1 1 d . . . H32A H 0.9346 0.1353 0.2297 0.095 Uiso 1 1 calc R . . H32B H 1.0246 0.1995 0.1648 0.095 Uiso 1 1 calc R . . H32C H 1.0098 0.1098 0.1205 0.095 Uiso 1 1 calc R . . C33 C 0.8381(4) 0.19593(17) -0.0340(3) 0.0594(9) Uani 1 1 d . . . H33A H 0.8798 0.1502 -0.0705 0.089 Uiso 1 1 calc R . . H33B H 0.9090 0.2406 -0.0329 0.089 Uiso 1 1 calc R . . H33C H 0.7412 0.2112 -0.0753 0.089 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 0.0314(2) 0.0202(2) 0.0232(2) -0.00171(16) 0.00219(16) 0.00013(17) F2 0.0452(9) 0.0425(8) 0.0359(9) -0.0080(6) 0.0015(7) -0.0071(6) F3 0.0534(10) 0.0500(9) 0.0529(11) 0.0046(8) 0.0185(8) -0.0108(7) F4 0.0714(11) 0.0576(10) 0.0332(9) 0.0060(7) 0.0224(8) 0.0068(8) F5 0.0674(11) 0.0560(9) 0.0261(8) -0.0088(7) -0.0015(7) 0.0018(8) F6 0.0479(9) 0.0576(9) 0.0366(9) -0.0102(7) 0.0034(7) -0.0140(7) O1 0.0320(8) 0.0221(8) 0.0229(8) -0.0007(6) 0.0002(7) 0.0026(6) O2 0.0438(10) 0.0220(8) 0.0280(9) -0.0023(6) 0.0025(7) 0.0053(7) O3 0.0351(9) 0.0271(8) 0.0335(10) -0.0021(7) 0.0031(7) -0.0040(7) C1 0.0371(13) 0.0237(11) 0.0272(13) -0.0001(9) 0.0030(10) 0.0033(10) C2 0.0420(14) 0.0251(12) 0.0282(13) -0.0020(10) 0.0026(11) 0.0049(10) C3 0.0400(14) 0.0277(12) 0.0424(16) 0.0039(11) 0.0124(12) 0.0001(11) C4 0.0535(16) 0.0318(12) 0.0284(14) 0.0034(11) 0.0142(12) 0.0100(12) C5 0.0497(16) 0.0333(13) 0.0261(14) -0.0039(10) 0.0035(12) 0.0080(11) C6 0.0404(14) 0.0289(12) 0.0317(14) -0.0007(10) 0.0048(11) 0.0017(10) C21 0.0437(15) 0.0229(12) 0.0432(16) -0.0055(11) -0.0035(12) 0.0071(10) C23 0.077(2) 0.0272(13) 0.0472(18) 0.0025(12) 0.0125(15) 0.0065(13) C22 0.0591(18) 0.0329(13) 0.0517(18) -0.0092(12) 0.0147(15) 0.0032(12) C11 0.0439(15) 0.0289(12) 0.0235(13) -0.0026(10) -0.0073(11) 0.0085(10) C12 0.0407(15) 0.0385(14) 0.0467(17) -0.0068(12) -0.0085(12) 0.0102(12) C13 0.0687(19) 0.0314(13) 0.0277(14) 0.0058(11) -0.0008(13) 0.0052(12) C31 0.0374(15) 0.0278(12) 0.0579(18) -0.0082(12) 0.0051(13) -0.0061(11) C32 0.0373(16) 0.0652(19) 0.084(3) -0.0197(18) -0.0046(16) -0.0081(14) C33 0.062(2) 0.0433(16) 0.077(2) 0.0102(15) 0.0248(17) -0.0105(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O2 1.7595(14) . ? Ti1 O3 1.7656(16) . ? Ti1 O1 1.9436(15) . ? Ti1 O1 2.0852(14) 3_655 ? Ti1 C1 2.177(2) . ? Ti1 Ti1 3.2272(7) 3_655 ? F2 C2 1.368(3) . ? F3 C3 1.348(3) . ? F4 C4 1.351(3) . ? F5 C5 1.356(3) . ? F6 C6 1.364(3) . ? O1 C11 1.457(3) . ? O1 Ti1 2.0852(14) 3_655 ? O2 C21 1.434(3) . ? O3 C31 1.435(3) . ? C1 C2 1.375(3) . ? C1 C6 1.381(3) . ? C2 C3 1.376(3) . ? C3 C4 1.379(4) . ? C4 C5 1.369(4) . ? C5 C6 1.376(3) . ? C21 C22 1.507(4) . ? C21 C23 1.508(4) . ? C21 H21 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C11 C13 1.508(3) . ? C11 C12 1.510(3) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C31 C32 1.505(4) . ? C31 C33 1.510(4) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ti1 O3 101.82(7) . . ? O2 Ti1 O1 100.01(7) . . ? O3 Ti1 O1 118.87(7) . . ? O2 Ti1 O1 167.75(7) . 3_655 ? O3 Ti1 O1 90.42(6) . 3_655 ? O1 Ti1 O1 73.59(7) . 3_655 ? O2 Ti1 C1 91.43(8) . . ? O3 Ti1 C1 108.65(8) . . ? O1 Ti1 C1 127.07(8) . . ? O1 Ti1 C1 84.58(7) 3_655 . ? O2 Ti1 Ti1 137.40(6) . 3_655 ? O3 Ti1 Ti1 107.19(5) . 3_655 ? O1 Ti1 Ti1 38.30(4) . 3_655 ? O1 Ti1 Ti1 35.29(4) 3_655 3_655 ? C1 Ti1 Ti1 107.58(6) . 3_655 ? C11 O1 Ti1 131.91(12) . . ? C11 O1 Ti1 120.68(12) . 3_655 ? Ti1 O1 Ti1 106.41(7) . 3_655 ? C21 O2 Ti1 170.12(15) . . ? C31 O3 Ti1 139.25(14) . . ? C2 C1 C6 114.0(2) . . ? C2 C1 Ti1 120.13(17) . . ? C6 C1 Ti1 125.85(17) . . ? F2 C2 C1 118.5(2) . . ? F2 C2 C3 116.9(2) . . ? C1 C2 C3 124.6(2) . . ? F3 C3 C2 121.6(2) . . ? F3 C3 C4 119.9(2) . . ? C2 C3 C4 118.4(2) . . ? F4 C4 C5 120.4(2) . . ? F4 C4 C3 119.8(2) . . ? C5 C4 C3 119.7(2) . . ? F5 C5 C4 119.6(2) . . ? F5 C5 C6 121.3(2) . . ? C4 C5 C6 119.1(2) . . ? F6 C6 C5 116.3(2) . . ? F6 C6 C1 119.7(2) . . ? C5 C6 C1 124.1(2) . . ? O2 C21 C22 108.9(2) . . ? O2 C21 C23 109.4(2) . . ? C22 C21 C23 112.2(2) . . ? O2 C21 H21 108.8 . . ? C22 C21 H21 108.8 . . ? C23 C21 H21 108.8 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O1 C11 C13 109.78(19) . . ? O1 C11 C12 109.9(2) . . ? C13 C11 C12 113.7(2) . . ? O1 C11 H11 107.8 . . ? C13 C11 H11 107.8 . . ? C12 C11 H11 107.8 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O3 C31 C32 107.9(2) . . ? O3 C31 C33 108.5(2) . . ? C32 C31 C33 113.5(2) . . ? O3 C31 H31 109.0 . . ? C32 C31 H31 109.0 . . ? C33 C31 H31 109.0 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.259 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.062