####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_jp031032 _database_code_depnum_ccdc_archive 'CCDC 605305' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H26 F15 Li O4 Ti' _chemical_formula_weight 742.31 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4160(13) _cell_length_b 11.6326(13) _cell_length_c 12.4470(15) _cell_angle_alpha 86.285(3) _cell_angle_beta 73.048(3) _cell_angle_gamma 70.442(2) _cell_volume 1488.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 198(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Irregular _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.325 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.175 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.656 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 0.414 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997b)' _exptl_special_details ; Crystal decay was monitored by repeating the initial 50 frames at the end of the data collection and analyzing duplicate reflections. ; _diffrn_ambient_temperature 198(1) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Bruker AXS SMART1000/P4' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10701 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6503 _reflns_number_gt 5365 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0637P)^2^+0.3793P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6503 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0514 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1200 _refine_ls_wR_factor_gt 0.1131 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _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 Ti Ti 0.09416(3) 0.85829(3) 0.00177(3) 0.02105(10) Uani 1 1 d . . . Li Li 0.1814(3) 1.0882(3) 0.0734(3) 0.0313(7) Uani 1 1 d . . . F1 F -0.02987(10) 0.82055(10) -0.04395(9) 0.0286(2) Uani 1 1 d . . . F2 F -0.05833(10) 0.99575(9) 0.09538(8) 0.0247(2) Uani 1 1 d . . . F3 F 0.19685(10) 0.92922(10) 0.04914(10) 0.0290(2) Uani 1 1 d . . . O1 O 0.22778(13) 0.76865(12) -0.11054(11) 0.0285(3) Uani 1 1 d . . . O2 O 0.09157(12) 0.75557(11) 0.11783(10) 0.0242(3) Uani 1 1 d . . . C1 C 0.32668(18) 0.68225(17) -0.18450(16) 0.0278(4) Uani 1 1 d . . . C2 C 0.4295(2) 0.6218(2) -0.1226(2) 0.0424(5) Uani 1 1 d . . . C3 C 0.2675(2) 0.5890(2) -0.21118(18) 0.0373(5) Uani 1 1 d . . . C4 C 0.38452(18) 0.73724(18) -0.29411(16) 0.0280(4) Uani 1 1 d . . . C5 C 0.3209(2) 0.8566(2) -0.31517(18) 0.0338(4) Uani 1 1 d . . . H5 H 0.2440 0.9038 -0.2613 0.041 Uiso 1 1 calc R . . C6 C 0.3696(2) 0.9073(2) -0.4153(2) 0.0452(6) Uani 1 1 d . . . H6 H 0.3253 0.9891 -0.4298 0.054 Uiso 1 1 calc R . . C7 C 0.4811(2) 0.8405(2) -0.4936(2) 0.0458(6) Uani 1 1 d . . . H7 H 0.5143 0.8761 -0.5614 0.055 Uiso 1 1 calc R . . C8 C 0.5444(2) 0.7216(2) -0.4732(2) 0.0478(6) Uani 1 1 d . . . H8 H 0.6213 0.6750 -0.5273 0.057 Uiso 1 1 calc R . . C9 C 0.4964(2) 0.6693(2) -0.3740(2) 0.0425(5) Uani 1 1 d . . . H9 H 0.5402 0.5869 -0.3607 0.051 Uiso 1 1 calc R . . C10 C 0.04671(18) 0.69150(17) 0.20908(15) 0.0251(4) Uani 1 1 d . . . C11 C 0.0551(2) 0.5686(2) 0.16147(18) 0.0369(5) Uani 1 1 d . . . C12 C -0.09624(19) 0.7685(2) 0.26725(17) 0.0343(5) Uani 1 1 d . . . C13 C 0.12485(18) 0.67247(17) 0.29390(16) 0.0261(4) Uani 1 1 d . . . C14 C 0.2118(2) 0.7345(2) 0.28134(17) 0.0334(4) Uani 1 1 d . . . H14 H 0.2261 0.7843 0.2186 0.040 Uiso 1 1 calc R . . C15 C 0.2787(2) 0.7240(3) 0.36083(19) 0.0438(6) Uani 1 1 d . . . H15 H 0.3378 0.7676 0.3522 0.053 Uiso 1 1 calc R . . C16 C 0.2603(2) 0.6517(3) 0.4515(2) 0.0469(6) Uani 1 1 d . . . H16 H 0.3060 0.6456 0.5055 0.056 Uiso 1 1 calc R . . C17 C 0.1756(2) 0.5884(3) 0.4638(2) 0.0480(6) Uani 1 1 d . . . H17 H 0.1635 0.5374 0.5259 0.058 Uiso 1 1 calc R . . C18 C 0.1076(2) 0.5983(2) 0.38591(19) 0.0403(5) Uani 1 1 d . . . H18 H 0.0488 0.5544 0.3952 0.048 Uiso 1 1 calc R . . O19 O 0.33210(14) 1.11914(13) -0.02213(13) 0.0362(3) Uani 1 1 d . . . C20 C 0.3368(2) 1.2411(2) -0.0424(2) 0.0415(5) Uani 1 1 d . . . H20A H 0.3550 1.2723 0.0209 0.050 Uiso 1 1 calc R . . H20B H 0.2529 1.2966 -0.0507 0.050 Uiso 1 1 calc R . . C21 C 0.4433(4) 1.2333(3) -0.1488(3) 0.0880(13) Uani 1 1 d . . . H21A H 0.4068 1.2704 -0.2108 0.106 Uiso 1 1 calc R . . H21B H 0.5007 1.2768 -0.1386 0.106 Uiso 1 1 calc R . . C22 C 0.5141(3) 1.1061(3) -0.1732(3) 0.0766(10) Uani 1 1 d . . . H22A H 0.5916 1.0813 -0.1453 0.092 Uiso 1 1 calc R . . H22B H 0.5429 1.0883 -0.2553 0.092 Uiso 1 1 calc R . . C23 C 0.4228(2) 1.0386(2) -0.1142(2) 0.0433(5) Uani 1 1 d . . . H23A H 0.3777 1.0220 -0.1654 0.052 Uiso 1 1 calc R . . H23B H 0.4702 0.9602 -0.0867 0.052 Uiso 1 1 calc R . . O24 O 0.16975(17) 1.11387(17) 0.22821(13) 0.0473(4) Uani 1 1 d . . . C25 C 0.0676(3) 1.0929(3) 0.3176(2) 0.0590(7) Uani 1 1 d . . . H25A H 0.0629 1.0108 0.3085 0.071 Uiso 1 1 calc R . . H25B H -0.0171 1.1548 0.3191 0.071 Uiso 1 1 calc R . . C26 C 0.1020(4) 1.1028(3) 0.4230(3) 0.0722(9) Uani 1 1 d . . . H26A H 0.0232 1.1414 0.4853 0.087 Uiso 1 1 calc R . . H26B H 0.1491 1.0213 0.4457 0.087 Uiso 1 1 calc R . . C27 C 0.1869(5) 1.1809(5) 0.3933(3) 0.1000(15) Uani 1 1 d . . . H27A H 0.1417 1.2613 0.4336 0.120 Uiso 1 1 calc R . . H27B H 0.2682 1.1412 0.4142 0.120 Uiso 1 1 calc R . . C28 C 0.2156(3) 1.1958(3) 0.2709(2) 0.0579(7) Uani 1 1 d . . . H28A H 0.1711 1.2810 0.2542 0.070 Uiso 1 1 calc R . . H28B H 0.3101 1.1763 0.2362 0.070 Uiso 1 1 calc R . . F21 F 0.48897(17) 0.70031(18) -0.11301(16) 0.0713(5) Uani 1 1 d . . . F22 F 0.52013(15) 0.52105(16) -0.17490(14) 0.0679(5) Uani 1 1 d . . . F23 F 0.37749(15) 0.59285(16) -0.01931(12) 0.0623(5) Uani 1 1 d . . . F31 F 0.35399(17) 0.50075(13) -0.28488(13) 0.0605(4) Uani 1 1 d . . . F32 F 0.21998(16) 0.53545(14) -0.11993(12) 0.0562(4) Uani 1 1 d . . . F33 F 0.17273(15) 0.64536(15) -0.25603(13) 0.0539(4) Uani 1 1 d . . . F111 F 0.17802(15) 0.49914(12) 0.12184(12) 0.0513(4) Uani 1 1 d . . . F112 F -0.00384(17) 0.50492(13) 0.23945(13) 0.0568(4) Uani 1 1 d . . . F113 F 0.00028(16) 0.58497(14) 0.07858(12) 0.0524(4) Uani 1 1 d . . . F121 F -0.15326(13) 0.71174(14) 0.35301(12) 0.0512(4) Uani 1 1 d . . . F122 F -0.16841(12) 0.79716(15) 0.19691(12) 0.0499(4) Uani 1 1 d . . . F123 F -0.10040(12) 0.87281(12) 0.30868(11) 0.0434(3) 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 0.02425(17) 0.02052(17) 0.01832(17) 0.00195(12) -0.00633(12) -0.00738(13) Li 0.0331(17) 0.0348(18) 0.0311(18) 0.0013(14) -0.0136(14) -0.0140(14) F1 0.0319(6) 0.0280(6) 0.0298(6) 0.0017(5) -0.0131(5) -0.0112(5) F2 0.0284(5) 0.0242(5) 0.0180(5) 0.0036(4) -0.0042(4) -0.0067(4) F3 0.0314(6) 0.0281(6) 0.0325(6) 0.0040(5) -0.0135(5) -0.0131(5) O1 0.0303(7) 0.0271(7) 0.0216(7) -0.0004(5) -0.0032(5) -0.0048(6) O2 0.0281(6) 0.0240(6) 0.0205(6) 0.0055(5) -0.0064(5) -0.0097(5) C1 0.0284(9) 0.0249(9) 0.0255(10) -0.0007(8) -0.0061(8) -0.0040(8) C2 0.0352(11) 0.0492(14) 0.0364(12) 0.0059(10) -0.0123(9) -0.0048(10) C3 0.0505(13) 0.0345(11) 0.0277(11) 0.0026(9) -0.0059(9) -0.0200(10) C4 0.0284(9) 0.0307(10) 0.0245(10) 0.0002(8) -0.0044(8) -0.0120(8) C5 0.0351(10) 0.0339(11) 0.0278(10) 0.0011(8) -0.0036(8) -0.0102(9) C6 0.0524(14) 0.0399(13) 0.0384(13) 0.0110(10) -0.0070(11) -0.0161(11) C7 0.0492(13) 0.0539(15) 0.0338(12) 0.0073(10) -0.0011(10) -0.0270(12) C8 0.0401(12) 0.0559(15) 0.0366(13) -0.0016(11) 0.0071(10) -0.0170(11) C9 0.0352(11) 0.0408(13) 0.0402(13) 0.0009(10) -0.0001(9) -0.0072(10) C10 0.0305(9) 0.0255(9) 0.0209(9) 0.0054(7) -0.0078(7) -0.0118(8) C11 0.0531(13) 0.0330(11) 0.0306(11) 0.0048(9) -0.0116(10) -0.0230(10) C12 0.0304(10) 0.0459(12) 0.0266(10) 0.0077(9) -0.0082(8) -0.0137(9) C13 0.0274(9) 0.0263(9) 0.0226(9) 0.0032(7) -0.0075(7) -0.0067(7) C14 0.0357(10) 0.0418(12) 0.0259(10) 0.0064(9) -0.0099(8) -0.0168(9) C15 0.0384(11) 0.0684(16) 0.0327(12) 0.0046(11) -0.0140(10) -0.0251(11) C16 0.0416(12) 0.0687(17) 0.0317(12) 0.0069(11) -0.0189(10) -0.0138(12) C17 0.0525(14) 0.0612(16) 0.0349(13) 0.0232(11) -0.0216(11) -0.0209(12) C18 0.0461(12) 0.0457(13) 0.0359(12) 0.0187(10) -0.0179(10) -0.0218(11) O19 0.0327(7) 0.0312(8) 0.0434(9) 0.0003(6) -0.0059(6) -0.0130(6) C20 0.0449(12) 0.0343(12) 0.0489(14) -0.0008(10) -0.0107(11) -0.0196(10) C21 0.087(2) 0.058(2) 0.094(3) -0.0065(18) 0.032(2) -0.0401(18) C22 0.069(2) 0.0555(18) 0.069(2) 0.0098(15) 0.0204(16) -0.0108(15) C23 0.0458(13) 0.0342(12) 0.0434(13) -0.0003(10) -0.0117(10) -0.0058(10) O24 0.0543(10) 0.0638(11) 0.0304(8) -0.0018(8) -0.0153(7) -0.0246(9) C25 0.0569(16) 0.080(2) 0.0436(15) 0.0025(14) -0.0127(13) -0.0282(15) C26 0.084(2) 0.095(3) 0.0396(16) -0.0010(16) -0.0122(15) -0.037(2) C27 0.126(3) 0.163(4) 0.0412(18) -0.020(2) -0.0110(19) -0.093(3) C28 0.086(2) 0.0477(15) 0.0479(15) -0.0024(12) -0.0257(15) -0.0263(15) F21 0.0649(10) 0.0959(13) 0.0781(12) 0.0099(10) -0.0484(9) -0.0354(10) F22 0.0501(9) 0.0642(10) 0.0549(10) 0.0060(8) -0.0112(7) 0.0208(8) F23 0.0535(9) 0.0802(11) 0.0365(8) 0.0190(8) -0.0164(7) -0.0009(8) F31 0.0828(11) 0.0408(8) 0.0505(9) -0.0163(7) 0.0009(8) -0.0252(8) F32 0.0829(11) 0.0500(9) 0.0406(8) 0.0088(7) -0.0056(7) -0.0400(8) F33 0.0600(9) 0.0675(10) 0.0556(9) 0.0101(8) -0.0299(7) -0.0382(8) F111 0.0654(9) 0.0282(7) 0.0498(9) -0.0072(6) -0.0099(7) -0.0063(6) F112 0.0901(11) 0.0501(9) 0.0464(8) 0.0110(7) -0.0145(8) -0.0499(9) F113 0.0812(10) 0.0543(9) 0.0411(8) 0.0021(7) -0.0281(7) -0.0381(8) F121 0.0376(7) 0.0691(10) 0.0399(8) 0.0162(7) 0.0003(6) -0.0212(7) F122 0.0321(6) 0.0749(10) 0.0430(8) 0.0073(7) -0.0188(6) -0.0123(7) F123 0.0416(7) 0.0392(7) 0.0359(7) -0.0061(6) -0.0055(6) 0.0001(6) _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 1.8024(13) . ? Ti O2 1.8141(13) . ? Ti F1 1.8548(11) . ? Ti F3 1.8752(11) . ? Ti F2 2.0173(11) 2_575 ? Ti F2 2.0347(11) . ? Ti Ti 3.2839(7) 2_575 ? Ti Li 3.389(3) 2_575 ? Ti Li 3.398(3) . ? Li F1 1.828(4) 2_575 ? Li F3 1.834(4) . ? Li O19 1.916(4) . ? Li O24 1.928(4) . ? Li Ti 3.389(3) 2_575 ? F1 Li 1.828(4) 2_575 ? F2 Ti 2.0173(11) 2_575 ? O1 C1 1.373(2) . ? O2 C10 1.384(2) . ? C1 C4 1.533(3) . ? C1 C2 1.539(3) . ? C1 C3 1.553(3) . ? C2 F23 1.323(3) . ? C2 F22 1.328(3) . ? C2 F21 1.337(3) . ? C3 F33 1.320(3) . ? C3 F32 1.322(2) . ? C3 F31 1.336(3) . ? C4 C5 1.383(3) . ? C4 C9 1.389(3) . ? C5 C6 1.390(3) . ? C5 H5 0.9500 . ? C6 C7 1.374(3) . ? C6 H6 0.9500 . ? C7 C8 1.375(4) . ? C7 H7 0.9500 . ? C8 C9 1.387(3) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C13 1.532(3) . ? C10 C11 1.546(3) . ? C10 C12 1.551(3) . ? C11 F111 1.324(3) . ? C11 F113 1.328(3) . ? C11 F112 1.343(2) . ? C12 F122 1.325(2) . ? C12 F123 1.330(3) . ? C12 F121 1.338(2) . ? C13 C14 1.381(3) . ? C13 C18 1.396(3) . ? C14 C15 1.392(3) . ? C14 H14 0.9500 . ? C15 C16 1.372(3) . ? C15 H15 0.9500 . ? C16 C17 1.370(4) . ? C16 H16 0.9500 . ? C17 C18 1.386(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? O19 C23 1.436(3) . ? O19 C20 1.440(3) . ? C20 C21 1.498(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.432(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.507(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? O24 C28 1.424(3) . ? O24 C25 1.434(3) . ? C25 C26 1.496(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.496(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.474(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ti O2 103.32(6) . . ? O1 Ti F1 94.02(6) . . ? O2 Ti F1 94.66(5) . . ? O1 Ti F3 93.64(6) . . ? O2 Ti F3 92.11(5) . . ? F1 Ti F3 168.34(5) . . ? O1 Ti F2 92.17(5) . 2_575 ? O2 Ti F2 164.48(5) . 2_575 ? F1 Ti F2 85.16(5) . 2_575 ? F3 Ti F2 85.78(5) . 2_575 ? O1 Ti F2 163.88(5) . . ? O2 Ti F2 92.78(5) . . ? F1 Ti F2 85.24(5) . . ? F3 Ti F2 84.97(5) . . ? F2 Ti F2 71.72(5) 2_575 . ? O1 Ti Ti 128.21(5) . 2_575 ? O2 Ti Ti 128.46(4) . 2_575 ? F1 Ti Ti 84.07(4) . 2_575 ? F3 Ti Ti 84.29(4) . 2_575 ? F2 Ti Ti 36.04(3) 2_575 2_575 ? F2 Ti Ti 35.68(3) . 2_575 ? O1 Ti Li 107.63(7) . 2_575 ? O2 Ti Li 108.37(7) . 2_575 ? F1 Ti Li 22.87(7) . 2_575 ? F3 Ti Li 145.48(7) . 2_575 ? F2 Ti Li 67.00(7) 2_575 2_575 ? F2 Ti Li 67.04(7) . 2_575 ? Ti Ti Li 61.20(6) 2_575 2_575 ? O1 Ti Li 107.19(7) . . ? O2 Ti Li 106.67(7) . . ? F1 Ti Li 145.00(7) . . ? F3 Ti Li 23.36(7) . . ? F2 Ti Li 66.94(7) 2_575 . ? F2 Ti Li 66.68(7) . . ? Ti Ti Li 60.93(6) 2_575 . ? Li Ti Li 122.13(5) 2_575 . ? F1 Li F3 105.00(16) 2_575 . ? F1 Li O19 114.06(19) 2_575 . ? F3 Li O19 108.65(18) . . ? F1 Li O24 110.11(19) 2_575 . ? F3 Li O24 109.57(19) . . ? O19 Li O24 109.31(17) . . ? F1 Li Ti 23.22(6) 2_575 2_575 ? F3 Li Ti 81.78(11) . 2_575 ? O19 Li Ti 123.07(15) . 2_575 ? O24 Li Ti 119.45(15) . 2_575 ? F1 Li Ti 81.09(11) 2_575 . ? F3 Li Ti 23.92(6) . . ? O19 Li Ti 119.36(15) . . ? O24 Li Ti 119.66(15) . . ? Ti Li Ti 57.87(5) 2_575 . ? Li F1 Ti 133.91(12) 2_575 . ? Ti F2 Ti 108.28(5) 2_575 . ? Li F3 Ti 132.72(12) . . ? C1 O1 Ti 169.41(12) . . ? C10 O2 Ti 161.17(12) . . ? O1 C1 C4 112.40(16) . . ? O1 C1 C2 106.26(16) . . ? C4 C1 C2 111.23(16) . . ? O1 C1 C3 106.58(16) . . ? C4 C1 C3 109.24(16) . . ? C2 C1 C3 111.01(18) . . ? F23 C2 F22 107.3(2) . . ? F23 C2 F21 106.7(2) . . ? F22 C2 F21 107.6(2) . . ? F23 C2 C1 112.20(18) . . ? F22 C2 C1 113.5(2) . . ? F21 C2 C1 109.28(19) . . ? F33 C3 F32 108.33(19) . . ? F33 C3 F31 106.94(19) . . ? F32 C3 F31 107.26(18) . . ? F33 C3 C1 109.65(17) . . ? F32 C3 C1 111.89(18) . . ? F31 C3 C1 112.56(18) . . ? C5 C4 C9 119.34(19) . . ? C5 C4 C1 118.82(17) . . ? C9 C4 C1 121.81(19) . . ? C4 C5 C6 119.8(2) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C7 C6 C5 120.7(2) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C7 C8 119.6(2) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C7 C8 C9 120.4(2) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C8 C9 C4 120.1(2) . . ? C8 C9 H9 119.9 . . ? C4 C9 H9 119.9 . . ? O2 C10 C13 111.98(15) . . ? O2 C10 C11 106.53(15) . . ? C13 C10 C11 111.60(16) . . ? O2 C10 C12 106.98(15) . . ? C13 C10 C12 108.76(16) . . ? C11 C10 C12 110.90(16) . . ? F111 C11 F113 108.18(19) . . ? F111 C11 F112 107.14(18) . . ? F113 C11 F112 107.04(18) . . ? F111 C11 C10 110.13(17) . . ? F113 C11 C10 111.49(17) . . ? F112 C11 C10 112.66(17) . . ? F122 C12 F123 107.06(18) . . ? F122 C12 F121 107.69(17) . . ? F123 C12 F121 107.14(17) . . ? F122 C12 C10 112.53(17) . . ? F123 C12 C10 109.60(16) . . ? F121 C12 C10 112.53(17) . . ? C14 C13 C18 118.80(19) . . ? C14 C13 C10 118.82(17) . . ? C18 C13 C10 122.33(17) . . ? C13 C14 C15 119.9(2) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 120.9(2) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C17 C16 C15 119.6(2) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 120.3(2) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C17 C18 C13 120.5(2) . . ? C17 C18 H18 119.7 . . ? C13 C18 H18 119.7 . . ? C23 O19 C20 109.59(16) . . ? C23 O19 Li 123.13(17) . . ? C20 O19 Li 122.09(17) . . ? O19 C20 C21 106.6(2) . . ? O19 C20 H20A 110.4 . . ? C21 C20 H20A 110.4 . . ? O19 C20 H20B 110.4 . . ? C21 C20 H20B 110.4 . . ? H20A C20 H20B 108.6 . . ? C22 C21 C20 106.3(2) . . ? C22 C21 H21A 110.5 . . ? C20 C21 H21A 110.5 . . ? C22 C21 H21B 110.5 . . ? C20 C21 H21B 110.5 . . ? H21A C21 H21B 108.7 . . ? C21 C22 C23 106.4(2) . . ? C21 C22 H22A 110.4 . . ? C23 C22 H22A 110.4 . . ? C21 C22 H22B 110.4 . . ? C23 C22 H22B 110.4 . . ? H22A C22 H22B 108.6 . . ? O19 C23 C22 104.6(2) . . ? O19 C23 H23A 110.8 . . ? C22 C23 H23A 110.8 . . ? O19 C23 H23B 110.8 . . ? C22 C23 H23B 110.8 . . ? H23A C23 H23B 108.9 . . ? C28 O24 C25 107.6(2) . . ? C28 O24 Li 127.00(19) . . ? C25 O24 Li 120.76(18) . . ? O24 C25 C26 105.3(2) . . ? O24 C25 H25A 110.7 . . ? C26 C25 H25A 110.7 . . ? O24 C25 H25B 110.7 . . ? C26 C25 H25B 110.7 . . ? H25A C25 H25B 108.8 . . ? C27 C26 C25 104.4(3) . . ? C27 C26 H26A 110.9 . . ? C25 C26 H26A 110.9 . . ? C27 C26 H26B 110.9 . . ? C25 C26 H26B 110.9 . . ? H26A C26 H26B 108.9 . . ? C28 C27 C26 106.8(3) . . ? C28 C27 H27A 110.4 . . ? C26 C27 H27A 110.4 . . ? C28 C27 H27B 110.4 . . ? C26 C27 H27B 110.4 . . ? H27A C27 H27B 108.6 . . ? O24 C28 C27 106.8(2) . . ? O24 C28 H28A 110.4 . . ? C27 C28 H28A 110.4 . . ? O24 C28 H28B 110.4 . . ? C27 C28 H28B 110.4 . . ? H28A C28 H28B 108.6 . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.684 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.062 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_jp031149 _database_code_depnum_ccdc_archive 'CCDC 605306' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H20 F24 O4 Ti' _chemical_formula_weight 1020.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.6982(8) _cell_length_b 16.9668(11) _cell_length_c 21.8494(15) _cell_angle_alpha 90.00 _cell_angle_beta 101.998(1) _cell_angle_gamma 90.00 _cell_volume 3879.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 198(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Irregular _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.325 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.747 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 0.377 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997b)' _exptl_special_details ; Crystal decay was monitored by repeating the initial 50 frames at the end of the data collection and analyzing duplicate reflections. ; _diffrn_ambient_temperature 198(1) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Bruker AXS SMART1000/P4' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 26803 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8727 _reflns_number_gt 6931 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+1.1740P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens diffmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8727 _refine_ls_number_parameters 666 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0946 _refine_ls_wR_factor_gt 0.0880 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 Ti Ti 0.47133(2) 0.243727(14) 0.386695(12) 0.02247(7) Uani 1 1 d . . . O1 O 0.44538(11) 0.28239(6) 0.45882(5) 0.0311(2) Uani 1 1 d . . . O2 O 0.53670(11) 0.31903(6) 0.34645(5) 0.0347(3) Uani 1 1 d . . . O3 O 0.32548(10) 0.20556(7) 0.34225(5) 0.0346(3) Uani 1 1 d . . . O4 O 0.58627(11) 0.16686(6) 0.40597(6) 0.0347(3) Uani 1 1 d . . . C1 C 0.44233(15) 0.28655(9) 0.52214(7) 0.0277(3) Uani 1 1 d . . . C2 C 0.41732(18) 0.20156(10) 0.54304(8) 0.0384(4) Uani 1 1 d . . . C3 C 0.32836(17) 0.34027(10) 0.52706(8) 0.0379(4) Uani 1 1 d . . . C4 C 0.56590(15) 0.32195(9) 0.55989(7) 0.0300(3) Uani 1 1 d . . . C5 C 0.6093(2) 0.30659(13) 0.62304(9) 0.0477(5) Uani 1 1 d . . . C6 C 0.7209(2) 0.34169(17) 0.65491(10) 0.0627(6) Uani 1 1 d . . . C7 C 0.7889(2) 0.39199(15) 0.62448(10) 0.0572(6) Uani 1 1 d . . . C8 C 0.7462(2) 0.40735(12) 0.56198(10) 0.0495(5) Uani 1 1 d . . . C9 C 0.63507(18) 0.37213(10) 0.52977(9) 0.0376(4) Uani 1 1 d . . . C10 C 0.58332(16) 0.39044(9) 0.32816(7) 0.0323(3) Uani 1 1 d . . . C11 C 0.5884(2) 0.38131(13) 0.25819(9) 0.0499(5) Uani 1 1 d . . . C12 C 0.48418(18) 0.45358(11) 0.33675(9) 0.0427(4) Uani 1 1 d . . . C13 C 0.71728(15) 0.40861(9) 0.36544(7) 0.0306(3) Uani 1 1 d . . . C14 C 0.79039(17) 0.34879(10) 0.39810(9) 0.0377(4) Uani 1 1 d . . . C15 C 0.91374(18) 0.36247(12) 0.43020(10) 0.0453(4) Uani 1 1 d . . . C16 C 0.9658(2) 0.43674(12) 0.43052(10) 0.0496(5) Uani 1 1 d . . . C17 C 0.8940(2) 0.49668(12) 0.39886(12) 0.0554(5) Uani 1 1 d . . . C18 C 0.77103(19) 0.48325(11) 0.36610(10) 0.0462(5) Uani 1 1 d . . . C19 C 0.20894(15) 0.18956(10) 0.30227(8) 0.0341(4) Uani 1 1 d . . . C20 C 0.11207(19) 0.24889(12) 0.31940(12) 0.0530(5) Uani 1 1 d . . . C21 C 0.2327(2) 0.20391(13) 0.23543(9) 0.0524(5) Uani 1 1 d . . . C22 C 0.16467(16) 0.10502(10) 0.31034(8) 0.0346(4) Uani 1 1 d . . . C23 C 0.0594(2) 0.07348(14) 0.27043(11) 0.0635(7) Uani 1 1 d . . . C24 C 0.0208(3) -0.00300(15) 0.27878(12) 0.0707(7) Uani 1 1 d . . . C25 C 0.0850(2) -0.04806(13) 0.32682(12) 0.0586(6) Uani 1 1 d . . . C26 C 0.1873(2) -0.01619(13) 0.36780(12) 0.0565(5) Uani 1 1 d . . . C27 C 0.22703(19) 0.05972(12) 0.35950(9) 0.0435(4) Uani 1 1 d . . . C28 C 0.68017(15) 0.11147(9) 0.40137(8) 0.0317(3) Uani 1 1 d . . . C29 C 0.69701(19) 0.11443(12) 0.33286(9) 0.0442(4) Uani 1 1 d . . . C30 C 0.62641(17) 0.03066(10) 0.41628(10) 0.0428(4) Uani 1 1 d . . . C31 C 0.80443(15) 0.12818(9) 0.44842(8) 0.0306(3) Uani 1 1 d . . . C32 C 0.91899(17) 0.09257(11) 0.44329(10) 0.0425(4) Uani 1 1 d . . . C33 C 1.02884(19) 0.10744(13) 0.48764(11) 0.0525(5) Uani 1 1 d . . . C34 C 1.0263(2) 0.15708(13) 0.53699(11) 0.0521(5) Uani 1 1 d . . . C35 C 0.9134(2) 0.19258(12) 0.54242(10) 0.0481(5) Uani 1 1 d . . . C36 C 0.80212(18) 0.17809(10) 0.49831(9) 0.0375(4) Uani 1 1 d . . . F1 F 0.33013(12) 0.16545(7) 0.49975(6) 0.0556(3) Uani 1 1 d . . . F2 F 0.52315(11) 0.15868(6) 0.55068(6) 0.0528(3) Uani 1 1 d . . . F3 F 0.37567(12) 0.19978(7) 0.59619(5) 0.0521(3) Uani 1 1 d . . . F4 F 0.21733(10) 0.30977(8) 0.49814(6) 0.0605(3) Uani 1 1 d . . . F5 F 0.32087(12) 0.35290(7) 0.58608(5) 0.0568(3) Uani 1 1 d . . . F6 F 0.34059(11) 0.40973(6) 0.50116(6) 0.0522(3) Uani 1 1 d . . . F7 F 0.66103(17) 0.32030(9) 0.25088(6) 0.0779(4) Uani 1 1 d . . . F8 F 0.63740(13) 0.44441(8) 0.23667(5) 0.0648(4) Uani 1 1 d . . . F9 F 0.47386(15) 0.37022(10) 0.22234(6) 0.0831(5) Uani 1 1 d . . . F10 F 0.36551(11) 0.43023(8) 0.31356(7) 0.0681(4) Uani 1 1 d . . . F11 F 0.49273(12) 0.46799(7) 0.39732(6) 0.0574(3) Uani 1 1 d . . . F12 F 0.50106(12) 0.52161(7) 0.30975(6) 0.0616(3) Uani 1 1 d . . . F13 F 0.09190(14) 0.23298(8) 0.37547(7) 0.0736(4) Uani 1 1 d . . . F14 F 0.15401(14) 0.32228(7) 0.32035(9) 0.0818(5) Uani 1 1 d . . . F15 F 0.00056(13) 0.24593(9) 0.27915(9) 0.0870(5) Uani 1 1 d . . . F16 F 0.12848(15) 0.19558(10) 0.19106(6) 0.0849(5) Uani 1 1 d . . . F17 F 0.31856(15) 0.15361(10) 0.22349(6) 0.0761(4) Uani 1 1 d . . . F18 F 0.27552(16) 0.27621(9) 0.22991(6) 0.0788(5) Uani 1 1 d . . . F19 F 0.76868(12) 0.17558(7) 0.32402(5) 0.0559(3) Uani 1 1 d . . . F20 F 0.58541(12) 0.12323(9) 0.29339(6) 0.0669(4) Uani 1 1 d . . . F21 F 0.75124(13) 0.05004(8) 0.31579(6) 0.0665(4) Uani 1 1 d . . . F22 F 0.52079(11) 0.01186(7) 0.37539(7) 0.0649(4) Uani 1 1 d . . . F23 F 0.70982(11) -0.02737(6) 0.41569(7) 0.0599(3) Uani 1 1 d . . . F24 F 0.59873(13) 0.03211(7) 0.47243(6) 0.0609(3) Uani 1 1 d . . . H5 H 0.559(2) 0.2766(14) 0.6450(11) 0.061(7) Uiso 1 1 d . . . H6 H 0.749(2) 0.3304(15) 0.6968(13) 0.075(8) Uiso 1 1 d . . . H7 H 0.861(2) 0.4152(13) 0.6472(10) 0.056(6) Uiso 1 1 d . . . H8 H 0.792(2) 0.4391(13) 0.5392(10) 0.054(6) Uiso 1 1 d . . . H9 H 0.6072(18) 0.3842(11) 0.4907(10) 0.038(5) Uiso 1 1 d . . . H14 H 0.7604(19) 0.3022(12) 0.3978(9) 0.041(5) Uiso 1 1 d . . . H15 H 0.964(2) 0.3196(13) 0.4527(10) 0.053(6) Uiso 1 1 d . . . H16 H 1.049(2) 0.4469(14) 0.4528(11) 0.067(7) Uiso 1 1 d . . . H17 H 0.929(2) 0.5467(15) 0.3975(11) 0.068(7) Uiso 1 1 d . . . H18 H 0.724(2) 0.5227(15) 0.3430(11) 0.065(7) Uiso 1 1 d . . . H23 H 0.014(3) 0.1026(16) 0.2355(13) 0.080(8) Uiso 1 1 d . . . H24 H -0.053(3) -0.0221(17) 0.2511(14) 0.090(9) Uiso 1 1 d . . . H25 H 0.056(2) -0.1015(16) 0.3331(12) 0.075(8) Uiso 1 1 d . . . H26 H 0.228(2) -0.0457(15) 0.4019(12) 0.072(8) Uiso 1 1 d . . . H27 H 0.292(2) 0.0776(12) 0.3862(10) 0.049(6) Uiso 1 1 d . . . H32 H 0.917(2) 0.0574(13) 0.4107(10) 0.050(6) Uiso 1 1 d . . . H33 H 1.108(2) 0.0832(14) 0.4831(11) 0.068(7) Uiso 1 1 d . . . H34 H 1.099(2) 0.1655(14) 0.5673(12) 0.065(7) Uiso 1 1 d . . . H35 H 0.909(2) 0.2251(13) 0.5753(11) 0.054(6) Uiso 1 1 d . . . H36 H 0.7278(19) 0.2019(11) 0.5028(9) 0.040(5) 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 Ti 0.02233(13) 0.02396(13) 0.01992(13) -0.00045(10) 0.00166(9) -0.00163(10) O1 0.0375(6) 0.0335(5) 0.0215(5) -0.0029(4) 0.0042(5) -0.0017(5) O2 0.0399(7) 0.0318(6) 0.0322(6) 0.0045(5) 0.0074(5) -0.0079(5) O3 0.0275(6) 0.0427(6) 0.0304(6) -0.0077(5) -0.0014(5) -0.0066(5) O4 0.0299(6) 0.0331(6) 0.0395(6) 0.0011(5) 0.0035(5) 0.0068(5) C1 0.0322(8) 0.0299(7) 0.0208(7) -0.0007(6) 0.0053(6) -0.0003(6) C2 0.0443(10) 0.0358(8) 0.0359(9) 0.0020(7) 0.0104(8) -0.0050(7) C3 0.0350(9) 0.0421(9) 0.0358(9) -0.0031(7) 0.0055(7) 0.0038(7) C4 0.0307(8) 0.0335(8) 0.0249(8) -0.0029(6) 0.0037(6) 0.0013(6) C5 0.0457(11) 0.0694(13) 0.0263(9) 0.0046(9) 0.0037(8) -0.0094(9) C6 0.0516(13) 0.1012(19) 0.0284(10) -0.0026(11) -0.0074(9) -0.0107(12) C7 0.0400(11) 0.0782(15) 0.0466(12) -0.0129(11) -0.0064(9) -0.0130(10) C8 0.0436(11) 0.0531(11) 0.0499(12) -0.0023(9) 0.0053(9) -0.0154(9) C9 0.0410(10) 0.0406(9) 0.0294(9) 0.0019(7) 0.0029(7) -0.0066(7) C10 0.0387(9) 0.0301(7) 0.0276(8) 0.0048(6) 0.0059(7) -0.0060(6) C11 0.0629(13) 0.0576(12) 0.0287(9) 0.0028(8) 0.0087(9) -0.0186(10) C12 0.0396(10) 0.0392(9) 0.0461(11) 0.0105(8) 0.0020(8) 0.0006(7) C13 0.0352(9) 0.0305(7) 0.0274(8) -0.0012(6) 0.0093(6) -0.0037(6) C14 0.0391(10) 0.0289(8) 0.0452(10) 0.0034(7) 0.0087(8) -0.0024(7) C15 0.0351(10) 0.0435(10) 0.0555(12) 0.0050(9) 0.0055(8) 0.0035(8) C16 0.0360(10) 0.0509(11) 0.0590(13) -0.0044(9) 0.0035(9) -0.0066(8) C17 0.0482(12) 0.0385(10) 0.0762(15) 0.0004(10) 0.0049(10) -0.0145(9) C18 0.0459(11) 0.0310(8) 0.0581(12) 0.0077(8) 0.0031(9) -0.0044(8) C19 0.0270(8) 0.0426(9) 0.0293(8) -0.0034(7) -0.0021(6) -0.0059(7) C20 0.0348(10) 0.0477(11) 0.0737(15) 0.0014(10) 0.0050(10) 0.0007(8) C21 0.0550(12) 0.0644(13) 0.0330(10) 0.0008(9) -0.0022(9) -0.0243(10) C22 0.0297(8) 0.0411(9) 0.0322(9) -0.0057(7) 0.0047(7) -0.0063(7) C23 0.0609(14) 0.0648(14) 0.0528(13) 0.0061(11) -0.0160(11) -0.0273(11) C24 0.0710(16) 0.0676(15) 0.0651(15) -0.0056(12) -0.0053(12) -0.0372(13) C25 0.0671(15) 0.0459(11) 0.0674(15) -0.0064(10) 0.0243(12) -0.0163(10) C26 0.0625(14) 0.0471(11) 0.0591(14) 0.0078(10) 0.0107(11) -0.0030(10) C27 0.0396(10) 0.0471(10) 0.0413(10) -0.0012(8) 0.0025(8) -0.0052(8) C28 0.0286(8) 0.0279(7) 0.0384(9) -0.0012(6) 0.0062(7) 0.0033(6) C29 0.0427(10) 0.0496(10) 0.0394(10) -0.0073(8) 0.0060(8) 0.0030(8) C30 0.0335(9) 0.0311(8) 0.0619(12) -0.0018(8) 0.0058(8) -0.0026(7) C31 0.0273(8) 0.0287(7) 0.0351(9) 0.0057(6) 0.0047(6) -0.0016(6) C32 0.0336(9) 0.0440(10) 0.0502(11) 0.0022(9) 0.0091(8) 0.0042(7) C33 0.0305(10) 0.0616(12) 0.0634(14) 0.0119(11) 0.0055(9) 0.0017(9) C34 0.0360(10) 0.0626(12) 0.0510(12) 0.0132(10) -0.0063(9) -0.0126(9) C35 0.0521(12) 0.0481(10) 0.0403(11) -0.0006(9) 0.0005(9) -0.0099(9) C36 0.0364(9) 0.0351(8) 0.0403(10) 0.0004(7) 0.0062(7) -0.0003(7) F1 0.0660(8) 0.0453(6) 0.0523(7) -0.0037(5) 0.0053(6) -0.0240(5) F2 0.0597(7) 0.0359(5) 0.0647(8) 0.0128(5) 0.0172(6) 0.0091(5) F3 0.0626(7) 0.0571(7) 0.0412(6) 0.0102(5) 0.0217(5) -0.0112(5) F4 0.0302(6) 0.0713(8) 0.0750(9) -0.0110(7) -0.0008(5) 0.0026(5) F5 0.0598(7) 0.0722(8) 0.0442(6) -0.0088(6) 0.0244(6) 0.0148(6) F6 0.0575(7) 0.0404(6) 0.0589(7) 0.0061(5) 0.0124(6) 0.0159(5) F7 0.1270(13) 0.0699(9) 0.0452(7) -0.0130(6) 0.0377(8) 0.0025(9) F8 0.0818(9) 0.0772(8) 0.0373(6) 0.0166(6) 0.0164(6) -0.0257(7) F9 0.0878(10) 0.1239(12) 0.0300(6) 0.0034(7) -0.0052(6) -0.0511(9) F10 0.0364(6) 0.0633(8) 0.0962(11) 0.0081(7) -0.0060(6) -0.0008(6) F11 0.0617(8) 0.0602(7) 0.0531(7) 0.0009(6) 0.0188(6) 0.0220(6) F12 0.0622(8) 0.0400(6) 0.0792(9) 0.0253(6) 0.0072(6) 0.0067(5) F13 0.0745(10) 0.0738(9) 0.0833(10) -0.0130(8) 0.0414(8) 0.0118(7) F14 0.0651(9) 0.0412(7) 0.1411(15) -0.0034(8) 0.0264(9) 0.0022(6) F15 0.0354(7) 0.0880(10) 0.1248(14) 0.0072(9) -0.0127(8) 0.0124(7) F16 0.0841(10) 0.1195(12) 0.0362(7) 0.0162(7) -0.0219(7) -0.0430(9) F17 0.0869(10) 0.1004(11) 0.0502(8) -0.0162(7) 0.0353(7) -0.0126(9) F18 0.1062(12) 0.0766(9) 0.0501(8) 0.0097(7) 0.0079(8) -0.0462(8) F19 0.0652(8) 0.0651(7) 0.0402(6) 0.0056(5) 0.0178(6) -0.0086(6) F20 0.0550(8) 0.1020(10) 0.0372(6) -0.0091(6) -0.0055(5) 0.0046(7) F21 0.0773(9) 0.0666(8) 0.0589(8) -0.0228(6) 0.0218(7) 0.0132(7) F22 0.0422(7) 0.0474(6) 0.0962(10) -0.0108(6) -0.0062(6) -0.0116(5) F23 0.0494(7) 0.0282(5) 0.1010(10) 0.0027(6) 0.0128(6) 0.0045(5) F24 0.0678(8) 0.0497(6) 0.0724(9) 0.0102(6) 0.0310(7) -0.0137(6) _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 O2 1.7750(11) . ? Ti O3 1.7796(11) . ? Ti O1 1.7813(11) . ? Ti O4 1.7819(11) . ? O1 C1 1.3923(18) . ? O2 C10 1.3997(18) . ? O3 C19 1.3923(18) . ? O4 C28 1.3944(18) . ? C1 C4 1.528(2) . ? C1 C3 1.544(2) . ? C1 C2 1.552(2) . ? C2 F2 1.327(2) . ? C2 F3 1.328(2) . ? C2 F1 1.332(2) . ? C3 F6 1.326(2) . ? C3 F5 1.326(2) . ? C3 F4 1.329(2) . ? C4 C9 1.381(2) . ? C4 C5 1.386(2) . ? C5 C6 1.386(3) . ? C5 H5 0.94(2) . ? C6 C7 1.379(3) . ? C6 H6 0.92(3) . ? C7 C8 1.372(3) . ? C7 H7 0.91(2) . ? C8 C9 1.385(3) . ? C8 H8 0.94(2) . ? C9 H9 0.87(2) . ? C10 C13 1.525(2) . ? C10 C12 1.546(3) . ? C10 C11 1.549(2) . ? C11 F8 1.321(2) . ? C11 F7 1.323(3) . ? C11 F9 1.324(2) . ? C12 F12 1.326(2) . ? C12 F10 1.326(2) . ? C12 F11 1.330(2) . ? C13 C14 1.385(2) . ? C13 C18 1.390(2) . ? C14 C15 1.379(3) . ? C14 H14 0.85(2) . ? C15 C16 1.377(3) . ? C15 H15 0.98(2) . ? C16 C17 1.372(3) . ? C16 H16 0.94(2) . ? C17 C18 1.380(3) . ? C17 H17 0.93(3) . ? C18 H18 0.92(2) . ? C19 C22 1.532(2) . ? C19 C20 1.545(3) . ? C19 C21 1.553(3) . ? C20 F13 1.315(3) . ? C20 F14 1.322(2) . ? C20 F15 1.328(2) . ? C21 F17 1.319(3) . ? C21 F18 1.324(2) . ? C21 F16 1.324(2) . ? C22 C27 1.375(3) . ? C22 C23 1.381(3) . ? C23 C24 1.385(3) . ? C23 H23 0.95(3) . ? C24 C25 1.363(4) . ? C24 H24 0.95(3) . ? C25 C26 1.373(3) . ? C25 H25 0.98(3) . ? C26 C27 1.380(3) . ? C26 H26 0.93(3) . ? C27 H27 0.86(2) . ? C28 C31 1.528(2) . ? C28 C29 1.545(3) . ? C28 C30 1.547(2) . ? C29 F21 1.326(2) . ? C29 F19 1.328(2) . ? C29 F20 1.328(2) . ? C30 F24 1.321(2) . ? C30 F22 1.326(2) . ? C30 F23 1.331(2) . ? C31 C36 1.385(2) . ? C31 C32 1.392(2) . ? C32 C33 1.382(3) . ? C32 H32 0.93(2) . ? C33 C34 1.373(3) . ? C33 H33 0.97(2) . ? C34 C35 1.376(3) . ? C34 H34 0.92(2) . ? C35 C36 1.389(3) . ? C35 H35 0.91(2) . ? C36 H36 0.92(2) . ? 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 Ti O3 112.50(5) . . ? O2 Ti O1 108.86(5) . . ? O3 Ti O1 109.66(5) . . ? O2 Ti O4 108.68(6) . . ? O3 Ti O4 110.27(5) . . ? O1 Ti O4 106.69(5) . . ? C1 O1 Ti 159.70(10) . . ? C10 O2 Ti 164.79(11) . . ? C19 O3 Ti 169.28(11) . . ? C28 O4 Ti 161.50(11) . . ? O1 C1 C4 111.10(12) . . ? O1 C1 C3 106.33(12) . . ? C4 C1 C3 109.72(13) . . ? O1 C1 C2 106.63(12) . . ? C4 C1 C2 112.88(13) . . ? C3 C1 C2 109.93(13) . . ? F2 C2 F3 108.07(14) . . ? F2 C2 F1 106.88(15) . . ? F3 C2 F1 107.33(15) . . ? F2 C2 C1 110.58(14) . . ? F3 C2 C1 112.84(14) . . ? F1 C2 C1 110.88(14) . . ? F6 C3 F5 107.63(14) . . ? F6 C3 F4 107.51(15) . . ? F5 C3 F4 107.26(15) . . ? F6 C3 C1 110.22(14) . . ? F5 C3 C1 111.81(14) . . ? F4 C3 C1 112.19(14) . . ? C9 C4 C5 119.24(16) . . ? C9 C4 C1 118.30(14) . . ? C5 C4 C1 122.45(15) . . ? C6 C5 C4 119.66(19) . . ? C6 C5 H5 120.1(15) . . ? C4 C5 H5 120.0(15) . . ? C7 C6 C5 120.6(2) . . ? C7 C6 H6 120.6(17) . . ? C5 C6 H6 118.7(17) . . ? C8 C7 C6 119.85(19) . . ? C8 C7 H7 121.9(14) . . ? C6 C7 H7 118.2(14) . . ? C7 C8 C9 119.8(2) . . ? C7 C8 H8 122.1(13) . . ? C9 C8 H8 118.0(13) . . ? C4 C9 C8 120.81(18) . . ? C4 C9 H9 120.4(13) . . ? C8 C9 H9 118.7(13) . . ? O2 C10 C13 111.93(13) . . ? O2 C10 C12 105.73(13) . . ? C13 C10 C12 112.78(13) . . ? O2 C10 C11 106.44(13) . . ? C13 C10 C11 108.97(14) . . ? C12 C10 C11 110.80(15) . . ? F8 C11 F7 107.76(18) . . ? F8 C11 F9 106.94(17) . . ? F7 C11 F9 108.17(18) . . ? F8 C11 C10 111.62(16) . . ? F7 C11 C10 109.84(16) . . ? F9 C11 C10 112.33(17) . . ? F12 C12 F10 107.36(15) . . ? F12 C12 F11 107.17(16) . . ? F10 C12 F11 107.30(16) . . ? F12 C12 C10 112.89(16) . . ? F10 C12 C10 111.91(15) . . ? F11 C12 C10 109.94(14) . . ? C14 C13 C18 118.30(16) . . ? C14 C13 C10 119.62(14) . . ? C18 C13 C10 122.04(15) . . ? C15 C14 C13 121.11(16) . . ? C15 C14 H14 118.6(13) . . ? C13 C14 H14 120.3(13) . . ? C16 C15 C14 119.97(18) . . ? C16 C15 H15 119.8(13) . . ? C14 C15 H15 120.2(13) . . ? C17 C16 C15 119.53(19) . . ? C17 C16 H16 119.8(15) . . ? C15 C16 H16 120.7(15) . . ? C16 C17 C18 120.83(18) . . ? C16 C17 H17 120.3(15) . . ? C18 C17 H17 118.8(15) . . ? C17 C18 C13 120.26(18) . . ? C17 C18 H18 121.4(15) . . ? C13 C18 H18 118.4(15) . . ? O3 C19 C22 111.61(13) . . ? O3 C19 C20 106.21(14) . . ? C22 C19 C20 110.07(14) . . ? O3 C19 C21 105.04(14) . . ? C22 C19 C21 111.70(14) . . ? C20 C19 C21 112.01(17) . . ? F13 C20 F14 107.4(2) . . ? F13 C20 F15 108.08(18) . . ? F14 C20 F15 107.53(18) . . ? F13 C20 C19 109.87(16) . . ? F14 C20 C19 112.01(17) . . ? F15 C20 C19 111.73(18) . . ? F17 C21 F18 108.23(19) . . ? F17 C21 F16 107.53(19) . . ? F18 C21 F16 106.67(18) . . ? F17 C21 C19 109.96(17) . . ? F18 C21 C19 111.00(16) . . ? F16 C21 C19 113.24(17) . . ? C27 C22 C23 118.43(18) . . ? C27 C22 C19 120.11(15) . . ? C23 C22 C19 121.42(17) . . ? C22 C23 C24 120.4(2) . . ? C22 C23 H23 121.0(16) . . ? C24 C23 H23 118.5(16) . . ? C25 C24 C23 120.7(2) . . ? C25 C24 H24 121.3(17) . . ? C23 C24 H24 118.0(17) . . ? C24 C25 C26 119.2(2) . . ? C24 C25 H25 120.4(15) . . ? C26 C25 H25 120.4(15) . . ? C25 C26 C27 120.5(2) . . ? C25 C26 H26 119.2(16) . . ? C27 C26 H26 120.3(16) . . ? C22 C27 C26 120.77(19) . . ? C22 C27 H27 121.5(14) . . ? C26 C27 H27 117.8(14) . . ? O4 C28 C31 111.43(13) . . ? O4 C28 C29 106.19(13) . . ? C31 C28 C29 112.65(14) . . ? O4 C28 C30 106.09(13) . . ? C31 C28 C30 109.40(13) . . ? C29 C28 C30 110.85(14) . . ? F21 C29 F19 107.64(16) . . ? F21 C29 F20 107.26(16) . . ? F19 C29 F20 106.62(16) . . ? F21 C29 C28 113.06(16) . . ? F19 C29 C28 110.70(14) . . ? F20 C29 C28 111.26(15) . . ? F24 C30 F22 107.83(16) . . ? F24 C30 F23 107.63(16) . . ? F22 C30 F23 107.15(15) . . ? F24 C30 C28 110.12(15) . . ? F22 C30 C28 111.92(15) . . ? F23 C30 C28 111.98(14) . . ? C36 C31 C32 119.28(16) . . ? C36 C31 C28 119.18(15) . . ? C32 C31 C28 121.51(16) . . ? C33 C32 C31 119.9(2) . . ? C33 C32 H32 122.3(13) . . ? C31 C32 H32 117.7(13) . . ? C34 C33 C32 120.6(2) . . ? C34 C33 H33 120.2(15) . . ? C32 C33 H33 119.2(15) . . ? C33 C34 C35 119.83(19) . . ? C33 C34 H34 120.4(15) . . ? C35 C34 H34 119.8(15) . . ? C34 C35 C36 120.2(2) . . ? C34 C35 H35 121.3(14) . . ? C36 C35 H35 118.4(14) . . ? C31 C36 C35 120.09(18) . . ? C31 C36 H36 120.8(12) . . ? C35 C36 H36 119.1(12) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.354 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.047