data_CRYSTALS_cif _audit_creation_date 98-05-26 _audit_creation_method CRYSTALS # RP326 # Copyright the Royal Society of Chemistry, 1998 #**************************************************************************** # The contents of this file between this point and the next #***** line # are held in the file CRYSTALS\SCRIPT\CIF.REF. # This is a character file which you may edit to reflect local # conditions # # 1. SUBMISSION DETAILS _publ_contact_author ; Pr. L. G. Hubert-Pfalzgraf, Laboratoire de Chimie Moleculaire, Universite de Nice, Parc Valrose, 06108 NICE Cedex 2, France ; _publ_contact_author_phone ' 33 04 92 07 61 33' _publ_contact_author_fax ' 33 04 92 07 61 44 ' _publ_contact_author_email ' hubert@unice.fr ' _publ_requested_journal 'J. Chem. Soc. Dalton Comm.' _publ_requested_coeditor_name ' ? ' _publ_contact_letter ; Please find herein for deposit the X-Ray data concerning the paper ref. 8/03266A ; #============================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and characterization of new titanium hexanuclear oxocarboxylatoalkoxides. Molecular structure of Ti6(mu3-O)6(mu-O2CC6H4OC6H5)6(OEt)6 ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Papiernik, R.' ; ? ; 'Hubert-Pfalzgraf, L. G.' ; ? ; 'Vaissermann, J.' ; ? ; 'Henriques Baptista Goncalves, M.C.' ; ? ; #============================================================================== # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; Carruthers, J.R. and Watkin, D.J. (1979), (Chebychev Weighting) Acta Cryst, A35, 698-699 Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Watkin, D.J., Prout, C.K. Carruthers, R.J. & Betteridge, P. (1996) CRYSTALS Issue 10. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. (1994), RC93, Chemical Crystallography Laboratory, Oxford, UK. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #========================================================================== # Now, all the strucure specific goodies #========================================================================== _computing_data_collection 'CAD-4 software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 software (Enraf-Nonius, 1989)' _computing_data_reduction ; RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994) ; _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; # _computing_structure_solution 'SHELXS86 (Sheldrick, 1986)' #========================================================================== # NOW THE GOODIES TO BE ENTERED BY HAND #========================================================================== _chemical_melting_point ? _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' Enraf-nonius CAD4 ' _refine_ls_matrix_type full _refine_ls_weighting_scheme ; Chebychev polynomial (Carruthers & Watkin, 1979) ; _atom_sites_solution_primary Direct_Methods _atom_sites_solution_hydrogens Geometric _refine_ls_hydrogen_treatment ; H atoms placed geometrically after each cycle, one overall isotropic thermal parameter refined ; #**************************************************************************** _chemical_name_systematic ; ? ; _cell_length_a 13.162(6) _cell_angle_alpha 102.97(2) _cell_length_b 14.977(6) _cell_angle_beta 103.48(3) _cell_length_c 17.110(2) _cell_angle_gamma 112.15(3) _cell_volume 2849(2) _symmetry_cell_setting 'Triclinic ' _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'Ti ' 0.2480 0.4460 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C104 H100 Ti6 O30 ' _chemical_formula_moiety ' C90 H84 Ti6 O30,(C7 H8)2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 2301.6 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 12.4 _cell_measurement_temperature 22C _cell_formula_units_Z 1 _exptl_crystal_description ' prism ' _exptl_crystal_colour ' white ' _exptl_crystal_size_min 0.22 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.34 _exptl_crystal_density_meas ? _exptl_crystal_F_000 ? _exptl_absorpt_coefficient_mu 0.47 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_process_details 'psiscan' _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 1.00 _diffrn_standards_interval_time 3600s _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% 4.65 _diffrn_ambient_temperature 22_C _diffrn_reflns_number 10493 _reflns_number_total 10018 _diffrn_reflns_av_R_equivalents 0.0223 _reflns_number_observed 4138 _diffrn_reflns_theta_min 1 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _reflns_limit_h_min -15 _reflns_limit_h_max 15 _reflns_limit_k_min -17 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -0.35 _refine_diff_density_max 0.74 _refine_ls_number_reflns 4138 _refine_ls_number_parameters 626 _refine_ls_R_factor_obs 0.0617 _refine_ls_wR_factor_obs 0.0735 _refine_ls_goodness_of_fit_obs 1.14 _refine_ls_shift/esd_max 3.187 _refine_ls_structure_factor_coef F _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method 2\q/\w loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type TI1 0.0557(1) 0.91789(9) 0.89675(8) 0.0355 1.0000 Uani TI2 -0.1032(1) 1.0285(1) 0.88536(8) 0.0361 1.0000 Uani TI3 0.1400(1) 1.16790(9) 1.02856(8) 0.0354 1.0000 Uani O1 -0.1163(4) 0.8995(3) 0.8917(3) 0.0359 1.0000 Uani O2 0.0761(4) 1.0545(3) 0.9253(3) 0.0357 1.0000 Uani O3 -0.0455(4) 1.1111(3) 1.0012(3) 0.0359 1.0000 Uani O4 -0.2532(4) 0.9995(4) 0.8559(3) 0.0488 1.0000 Uani O5 0.2915(4) 1.2133(4) 1.0491(3) 0.0465 1.0000 Uani O6 0.2009(4) 0.9416(4) 0.9113(3) 0.0476 1.0000 Uani O11 0.0145(4) 1.2398(4) 1.1629(3) 0.0444 1.0000 Uani O12 0.1612(4) 1.2979(3) 1.1161(3) 0.0416 1.0000 Uani O13 0.0490(6) 1.3853(5) 1.3117(4) 0.0621 1.0000 Uani O21 0.0062(4) 0.9029(4) 0.7710(3) 0.0436 1.0000 Uani O22 -0.1186(4) 0.9698(4) 0.7585(3) 0.0451 1.0000 Uani O23 -0.1656(9) 0.9983(6) 0.6056(4) 0.0868 1.0000 Uani O31 -0.0498(4) 1.1570(4) 0.8540(3) 0.0440 1.0000 Uani O32 0.1277(4) 1.2576(4) 0.9536(3) 0.0441 1.0000 Uani O33 0.1934(6) 1.4563(4) 0.9535(4) 0.0652 1.0000 Uani C1 0.0979(7) 1.3106(6) 1.1583(4) 0.0419 1.0000 Uani C2 -0.0706(6) 0.9201(6) 0.7279(4) 0.0411 1.0000 Uani C3 0.0502(7) 1.2360(5) 0.8850(5) 0.0419 1.0000 Uani C4 -0.370(1) 0.931(1) 0.806(1) 0.1248 1.0000 Uani C5 -0.421(2) 0.964(2) 0.747(1) 0.1564 1.0000 Uani C6 0.405(1) 1.281(1) 1.055(2) 0.1283 1.0000 Uani C7 0.424(2) 1.378(1) 1.061(2) 0.1613 1.0000 Uani C8 0.318(1) 0.977(2) 0.937(1) 0.1287 1.0000 Uani C9 0.375(2) 0.983(3) 0.889(2) 0.1864 1.0000 Uani C11 0.1251(6) 1.4201(5) 1.2009(5) 0.0422 1.0000 Uani C12 0.1792(7) 1.4922(6) 1.1664(5) 0.0548 1.0000 Uani C13 0.1965(8) 1.5923(7) 1.1976(7) 0.0648 1.0000 Uani C14 0.1614(8) 1.6218(7) 1.2640(6) 0.0639 1.0000 Uani C15 0.1113(8) 1.5517(6) 1.3020(5) 0.0574 1.0000 Uani C16 0.0928(7) 1.4509(6) 1.2697(5) 0.0499 1.0000 Uani C21 -0.1085(7) 0.8729(6) 0.6326(5) 0.0459 1.0000 Uani C22 -0.1006(8) 0.7831(7) 0.6016(5) 0.0577 1.0000 Uani C23 -0.143(1) 0.7291(8) 0.5139(6) 0.0687 1.0000 Uani C24 -0.1948(9) 0.7644(9) 0.4573(6) 0.0726 1.0000 Uani C25 -0.2037(9) 0.8528(8) 0.4859(5) 0.0660 1.0000 Uani C26 -0.1587(8) 0.9076(7) 0.5743(5) 0.0581 1.0000 Uani C31 0.0756(7) 1.3020(5) 0.8304(5) 0.0419 1.0000 Uani C32 0.0304(8) 1.2532(6) 0.7435(5) 0.0540 1.0000 Uani C33 0.0598(9) 1.3066(7) 0.6892(6) 0.0621 1.0000 Uani C34 0.1370(9) 1.4107(7) 0.7246(6) 0.0665 1.0000 Uani C35 0.1820(8) 1.4611(7) 0.8119(6) 0.0639 1.0000 Uani C36 0.1491(7) 1.4070(5) 0.8661(5) 0.0471 1.0000 Uani C41 -0.062(1) 1.3674(7) 1.3148(7) 0.0662 1.0000 Uani C42 -0.156(1) 1.3271(8) 1.2408(8) 0.0787 1.0000 Uani C43 -0.265(1) 1.3095(9) 1.250(1) 0.1048 1.0000 Uani C44 -0.275(2) 1.333(1) 1.329(2) 0.1032 1.0000 Uani C45 -0.178(2) 1.376(2) 1.399(1) 0.1130 1.0000 Uani C46 -0.069(1) 1.3921(9) 1.3954(8) 0.0909 1.0000 Uani C51 -0.202(1) 1.0451(8) 0.5544(6) 0.0690 1.0000 Uani C52 -0.146(1) 1.0846(9) 0.5043(8) 0.0882 1.0000 Uani C53 -0.186(1) 1.138(1) 0.4607(9) 0.0975 1.0000 Uani C54 -0.283(2) 1.147(1) 0.465(1) 0.1135 1.0000 Uani C55 -0.341(1) 1.108(1) 0.513(1) 0.1267 1.0000 Uani C56 -0.300(1) 1.056(1) 0.5575(9) 0.1089 1.0000 Uani C61 0.2151(8) 1.5595(6) 0.9834(5) 0.0517 1.0000 Uani C62 0.3266(9) 1.6305(7) 1.0336(6) 0.0694 1.0000 Uani C63 0.348(1) 1.7337(8) 1.0685(7) 0.0835 1.0000 Uani C64 0.258(2) 1.7566(9) 1.0484(8) 0.0872 1.0000 Uani C65 0.147(1) 1.684(1) 0.9998(8) 0.0884 1.0000 Uani C66 0.1256(9) 1.5849(8) 0.9660(6) 0.0735 1.0000 Uani C101 0.677(2) 0.748(2) 0.216(1) 0.182(8) 1.0000 Uiso C102 0.715(2) 0.854(2) 0.244(2) 0.24(1) 1.0000 Uiso C103 0.641(2) 0.879(1) 0.284(1) 0.163(7) 1.0000 Uiso C104 0.549(2) 0.801(1) 0.291(1) 0.182(8) 1.0000 Uiso C105 0.521(2) 0.696(2) 0.264(2) 0.21(1) 1.0000 Uiso C106 0.586(2) 0.669(1) 0.223(2) 0.22(1) 1.0000 Uiso C107 0.480(4) 0.828(3) 0.330(3) 0.49(3) 1.0000 Uiso C201 0.563(1) 0.455(1) 0.430(1) 0.134(5) 1.0000 Uiso C202 0.456(2) 0.371(1) 0.377(1) 0.22(1) 1.0000 Uiso C203 0.421(1) 0.288(1) 0.401(1) 0.159(6) 1.0000 Uiso C204 0.493(2) 0.285(1) 0.474(1) 0.205(9) 1.0000 Uiso C205 0.594(2) 0.367(2) 0.528(1) 0.170(7) 1.0000 Uiso C206 0.632(1) 0.453(1) 0.504(1) 0.168(7) 1.0000 Uiso C207 0.384(2) 0.373(2) 0.304(1) 0.22(1) 1.0000 Uiso H121 0.2059 1.4714 1.1182 0.118(6) 1.0000 Uiso H131 0.2346 1.6433 1.1716 0.118(6) 1.0000 Uiso H141 0.1718 1.6937 1.2853 0.118(6) 1.0000 Uiso H151 0.0889 1.5739 1.3523 0.118(6) 1.0000 Uiso H221 -0.0636 0.7566 0.6427 0.118(6) 1.0000 Uiso H231 -0.1364 0.6645 0.4923 0.118(6) 1.0000 Uiso H241 -0.2262 0.7250 0.3944 0.118(6) 1.0000 Uiso H251 -0.2417 0.8784 0.4444 0.118(6) 1.0000 Uiso H321 -0.0246 1.1780 0.7188 0.118(6) 1.0000 Uiso H331 0.0259 1.2706 0.6256 0.118(6) 1.0000 Uiso H341 0.1602 1.4497 0.6860 0.118(6) 1.0000 Uiso H351 0.2382 1.5360 0.8366 0.118(6) 1.0000 Uiso H421 -0.1478 1.3110 1.1832 0.118(6) 1.0000 Uiso H431 -0.3365 1.2794 1.1970 0.118(6) 1.0000 Uiso H441 -0.3537 1.3176 1.3341 0.118(6) 1.0000 Uiso H451 -0.1850 1.3975 1.4570 0.118(6) 1.0000 Uiso H461 0.0014 1.4202 1.4484 0.118(6) 1.0000 Uiso H521 -0.0767 1.0748 0.4991 0.118(6) 1.0000 Uiso H531 -0.1429 1.1702 0.4256 0.118(6) 1.0000 Uiso H541 -0.3122 1.1835 0.4302 0.118(6) 1.0000 Uiso H551 -0.4116 1.1172 0.5168 0.118(6) 1.0000 Uiso H561 -0.3432 1.0250 0.5935 0.118(6) 1.0000 Uiso H621 0.3915 1.6105 1.0454 0.118(6) 1.0000 Uiso H631 0.4280 1.7883 1.1072 0.118(6) 1.0000 Uiso H641 0.2742 1.8301 1.0700 0.118(6) 1.0000 Uiso H651 0.0812 1.7039 0.9889 0.118(6) 1.0000 Uiso H661 0.0445 1.5306 0.9287 0.118(6) 1.0000 Uiso H1011 0.7200 0.7254 0.1818 0.118(6) 1.0000 Uiso H1021 0.7872 0.9065 0.2385 0.118(6) 1.0000 Uiso H1031 0.6547 0.9518 0.3053 0.118(6) 1.0000 Uiso H1051 0.4544 0.6438 0.2725 0.118(6) 1.0000 Uiso H1061 0.5722 0.5960 0.2002 0.118(6) 1.0000 Uiso H2011 0.5926 0.5175 0.4133 0.118(6) 1.0000 Uiso H2031 0.3433 0.2279 0.3660 0.118(6) 1.0000 Uiso H2041 0.4680 0.2196 0.4874 0.118(6) 1.0000 Uiso H2051 0.6406 0.3657 0.5824 0.118(6) 1.0000 Uiso H2061 0.7078 0.5143 0.5411 0.118(6) 1.0000 Uiso 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 0.0345(7) 0.0388(7) 0.0360(7) 0.0121(6) 0.0139(6) 0.0185(6) TI2 0.0346(7) 0.0397(7) 0.0360(7) 0.0144(6) 0.0107(6) 0.0184(6) TI3 0.0332(7) 0.0352(7) 0.0390(7) 0.0132(6) 0.0134(6) 0.0157(6) O1 0.037(3) 0.035(3) 0.034(2) 0.012(2) 0.011(2) 0.014(2) O2 0.037(3) 0.036(3) 0.034(2) 0.012(2) 0.014(2) 0.017(2) O3 0.038(3) 0.036(3) 0.039(3) 0.013(2) 0.016(2) 0.020(2) O4 0.039(3) 0.053(3) 0.054(3) 0.015(3) 0.009(2) 0.023(3) O5 0.033(3) 0.054(3) 0.055(3) 0.019(3) 0.016(2) 0.017(2) O6 0.038(3) 0.052(3) 0.058(3) 0.018(3) 0.020(3) 0.021(2) O11 0.049(3) 0.035(3) 0.050(3) 0.012(2) 0.021(2) 0.017(2) O12 0.041(3) 0.035(3) 0.048(3) 0.005(2) 0.017(2) 0.016(2) O13 0.095(5) 0.066(4) 0.055(3) 0.028(3) 0.038(3) 0.046(4) O21 0.053(3) 0.050(3) 0.036(3) 0.019(2) 0.017(2) 0.027(3) O22 0.054(3) 0.049(3) 0.037(3) 0.017(2) 0.014(2) 0.026(3) O23 0.23(1) 0.095(5) 0.050(4) 0.024(4) 0.021(5) 0.108(6) O31 0.049(3) 0.039(3) 0.051(3) 0.021(2) 0.019(2) 0.021(3) O32 0.055(3) 0.035(3) 0.043(3) 0.018(2) 0.013(3) 0.016(2) O33 0.109(5) 0.043(3) 0.053(4) 0.016(3) 0.018(3) 0.026(3) C1 0.043(4) 0.043(4) 0.037(4) 0.012(3) 0.007(3) 0.020(4) C2 0.039(4) 0.046(4) 0.038(4) 0.017(3) 0.013(3) 0.016(4) C3 0.054(5) 0.039(4) 0.041(4) 0.014(3) 0.021(4) 0.024(4) C4 0.058(8) 0.18(2) 0.16(1) -0.00(1) -0.014(8) 0.045(9) C5 0.16(2) 0.31(3) 0.11(1) 0.04(2) -0.03(1) 0.14(2) C6 0.10(1) 0.09(1) 0.32(3) 0.07(1) 0.11(1) 0.008(9) C7 0.12(1) 0.12(1) 0.29(3) 0.05(2) 0.10(2) 0.01(1) C8 0.048(8) 0.35(3) 0.20(2) 0.09(2) 0.05(1) 0.08(1) C9 0.11(2) 0.49(5) 0.47(5) 0.35(4) 0.19(2) 0.16(2) C11 0.047(4) 0.033(4) 0.041(4) 0.004(3) 0.010(3) 0.017(3) C12 0.059(5) 0.046(5) 0.059(5) 0.013(4) 0.024(4) 0.022(4) C13 0.066(6) 0.046(5) 0.093(7) 0.021(5) 0.040(5) 0.020(4) C14 0.072(6) 0.046(5) 0.081(7) 0.001(5) 0.028(5) 0.028(5) C15 0.071(6) 0.051(5) 0.058(5) 0.011(4) 0.026(5) 0.033(5) C16 0.057(5) 0.040(4) 0.046(4) 0.007(4) 0.014(4) 0.018(4) C21 0.050(5) 0.057(5) 0.041(4) 0.021(4) 0.022(4) 0.025(4) C22 0.073(6) 0.082(6) 0.043(5) 0.019(4) 0.024(4) 0.049(5) C23 0.107(8) 0.082(7) 0.043(5) 0.011(5) 0.017(5) 0.059(6) C24 0.088(7) 0.104(8) 0.039(5) 0.011(5) 0.016(5) 0.047(7) C25 0.081(7) 0.103(8) 0.040(5) 0.024(5) 0.018(5) 0.051(6) C26 0.075(6) 0.073(6) 0.039(4) 0.021(4) 0.014(4) 0.040(5) C31 0.058(5) 0.043(4) 0.049(4) 0.019(4) 0.030(4) 0.032(4) C32 0.079(6) 0.046(5) 0.051(5) 0.019(4) 0.027(4) 0.031(4) C33 0.095(7) 0.065(6) 0.054(5) 0.029(5) 0.040(5) 0.039(5) C34 0.090(7) 0.063(6) 0.073(7) 0.037(5) 0.043(6) 0.035(5) C35 0.081(7) 0.054(5) 0.063(6) 0.029(5) 0.027(5) 0.023(5) C36 0.064(5) 0.034(4) 0.055(5) 0.020(4) 0.026(4) 0.018(4) C41 0.114(9) 0.058(6) 0.093(8) 0.041(6) 0.069(7) 0.052(6) C42 0.079(8) 0.060(6) 0.110(9) 0.028(6) 0.047(7) 0.025(6) C43 0.11(1) 0.070(8) 0.19(2) 0.059(9) 0.08(1) 0.033(7) C44 0.16(2) 0.09(1) 0.27(3) 0.09(1) 0.17(2) 0.07(1) C45 0.23(2) 0.14(2) 0.21(2) 0.12(2) 0.18(2) 0.12(2) C46 0.15(1) 0.101(9) 0.106(9) 0.053(7) 0.088(9) 0.074(9) C51 0.097(8) 0.068(6) 0.059(6) 0.028(5) -0.002(6) 0.040(6) C52 0.090(8) 0.083(8) 0.078(7) 0.030(6) -0.001(6) 0.024(6) C53 0.10(1) 0.083(8) 0.11(1) 0.054(8) 0.019(8) 0.012(7) C54 0.12(1) 0.09(1) 0.16(1) 0.07(1) 0.00(1) 0.033(9) C55 0.13(1) 0.13(1) 0.19(2) 0.10(1) 0.05(1) 0.08(1) C56 0.13(1) 0.11(1) 0.11(1) 0.055(8) 0.029(9) 0.055(9) C61 0.077(6) 0.038(4) 0.052(5) 0.020(4) 0.022(4) 0.025(4) C62 0.066(6) 0.060(6) 0.067(6) 0.016(5) 0.019(5) 0.016(5) C63 0.11(1) 0.053(6) 0.072(7) 0.006(5) 0.023(7) 0.000(6) C64 0.17(1) 0.054(7) 0.081(8) 0.022(6) 0.021(9) 0.054(9) C65 0.14(1) 0.101(9) 0.086(8) 0.033(7) 0.026(8) 0.090(9) C66 0.086(7) 0.073(6) 0.064(6) 0.025(5) 0.014(5) 0.039(6) _refine_ls_extinction_coef 54.0(259) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag TI1 . TI2 . 3.119(2) yes TI1 . TI3 2_577 3.114(2) yes TI1 . O1 . 2.154(4) yes TI1 . O2 . 1.891(4) yes TI1 . O3 2_577 1.912(4) yes TI1 . O6 . 1.751(5) yes TI1 . O11 2_577 2.075(5) yes TI1 . O21 . 2.030(5) yes TI2 . TI3 . 3.101(2) yes TI2 . O1 . 1.904(4) yes TI2 . O2 . 2.150(5) yes TI2 . O3 . 1.878(4) yes TI2 . O4 . 1.770(5) yes TI2 . O22 . 2.081(5) yes TI2 . O31 . 2.026(5) yes TI3 . O1 2_577 1.886(4) yes TI3 . O2 . 1.896(4) yes TI3 . O3 . 2.151(4) yes TI3 . O5 . 1.762(5) yes TI3 . O12 . 2.049(5) yes TI3 . O32 . 2.077(5) yes O4 . C4 . 1.39(1) yes O5 . C6 . 1.42(1) yes O6 . C8 . 1.35(1) yes O11 . C1 . 1.238(8) yes O12 . C1 . 1.260(8) yes O13 . C16 . 1.378(9) yes O13 . C41 . 1.39(1) yes O21 . C2 . 1.251(8) yes O22 . C2 . 1.249(8) yes O23 . C26 . 1.39(1) yes O23 . C51 . 1.35(1) yes O31 . C3 . 1.277(8) yes O32 . C3 . 1.244(9) yes O33 . C36 . 1.377(9) yes O33 . C61 . 1.406(9) yes C1 . C11 . 1.50(1) yes C2 . C21 . 1.50(1) yes C3 . C31 . 1.51(1) yes C4 . C5 . 1.37(2) yes C6 . C7 . 1.36(2) yes C8 . C9 . 1.23(3) yes C11 . C12 . 1.39(1) yes C11 . C16 . 1.39(1) yes C12 . C13 . 1.38(1) yes C12 . H121 . 1.001(8) no C13 . C14 . 1.37(1) yes C13 . H131 . 1.000(9) no C14 . C15 . 1.39(1) yes C14 . H141 . 1.001(8) no C15 . C16 . 1.39(1) yes C15 . H151 . 1.000(8) no C21 . C22 . 1.38(1) yes C21 . C26 . 1.37(1) yes C22 . C23 . 1.39(1) yes C22 . H221 . 1.001(9) no C23 . C24 . 1.37(1) yes C23 . H231 . 1.000(9) no C24 . C25 . 1.36(1) yes C24 . H241 . 1.001(9) no C25 . C26 . 1.40(1) yes C25 . H251 . 1.000(9) no C31 . C32 . 1.37(1) yes C31 . C36 . 1.39(1) yes C32 . C33 . 1.39(1) yes C32 . H321 . 1.000(8) no C33 . C34 . 1.39(1) yes C33 . H331 . 1.001(9) no C34 . C35 . 1.38(1) yes C34 . H341 . 1.001(9) no C35 . C36 . 1.40(1) yes C35 . H351 . 1.000(9) no C41 . C42 . 1.37(1) yes C41 . C46 . 1.38(1) yes C42 . C43 . 1.41(2) yes C42 . H421 . 1.00(1) no C43 . C44 . 1.37(2) yes C43 . H431 . 1.00(2) no C44 . C45 . 1.35(3) yes C44 . H441 . 1.00(2) no C45 . C46 . 1.39(2) yes C45 . H451 . 1.00(2) no C46 . H461 . 1.00(1) no C51 . C52 . 1.35(2) yes C51 . C56 . 1.38(2) yes C52 . C53 . 1.37(2) yes C52 . H521 . 1.00(1) no C53 . C54 . 1.34(2) yes C53 . H531 . 1.00(1) no C54 . C55 . 1.34(2) yes C54 . H541 . 1.00(1) no C55 . C56 . 1.36(2) yes C55 . H551 . 1.00(2) no C56 . H561 . 1.00(1) no C61 . C62 . 1.36(1) yes C61 . C66 . 1.36(1) yes C62 . C63 . 1.42(1) yes C62 . H621 . 1.00(1) no C63 . C64 . 1.34(2) yes C63 . H631 . 1.00(1) no C64 . C65 . 1.36(2) yes C64 . H641 . 1.00(1) no C65 . C66 . 1.36(1) yes C65 . H651 . 1.00(1) no C66 . H661 . 1.00(1) no C101 . C102 . 1.39(2) yes C101 . C106 . 1.38(2) yes C101 . H1011 . 0.99(2) no C102 . C103 . 1.42(2) yes C102 . H1021 . 1.02(2) no C103 . C104 . 1.39(1) yes C103 . H1031 . 1.00(2) no C104 . C105 . 1.40(2) yes C104 . C107 . 1.37(2) yes C105 . C106 . 1.35(2) yes C105 . H1051 . 1.00(2) no C106 . H1061 . 1.00(2) no C201 . C202 . 1.39(1) yes C201 . C206 . 1.39(1) yes C201 . H2011 . 1.00(1) no C202 . C203 . 1.35(1) yes C202 . C207 . 1.39(2) yes C203 . C204 . 1.41(2) yes C203 . H2031 . 1.00(1) no C204 . C205 . 1.35(2) yes C204 . H2041 . 1.00(2) no C205 . C206 . 1.38(2) yes C205 . H2051 . 1.00(2) no C206 . H2061 . 1.00(2) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag TI2 . TI1 . TI3 2_577 68.36(4) no TI2 . TI1 . O1 . 36.9(1) no TI3 2_577 TI1 . O1 . 36.5(1) no TI2 . TI1 . O2 . 42.6(1) no TI3 2_577 TI1 . O2 . 97.9(1) no O1 . TI1 . O2 . 77.3(2) no TI2 . TI1 . O3 2_577 98.3(1) no TI3 2_577 TI1 . O3 2_577 42.9(1) no O1 . TI1 . O3 2_577 77.3(2) no O2 . TI1 . O3 2_577 102.3(2) no TI2 . TI1 . O6 . 140.9(2) no TI3 2_577 TI1 . O6 . 141.1(2) no O1 . TI1 . O6 . 174.3(2) no O2 . TI1 . O6 . 99.3(2) no O3 2_577 TI1 . O6 . 99.1(2) no TI2 . TI1 . O11 2_577 121.0(1) no TI3 2_577 TI1 . O11 2_577 77.3(1) no O1 . TI1 . O11 2_577 89.3(2) no O2 . TI1 . O11 2_577 162.0(2) no O3 2_577 TI1 . O11 2_577 86.1(2) no TI2 . TI1 . O21 . 77.7(1) no TI3 2_577 TI1 . O21 . 118.0(1) no O1 . TI1 . O21 . 87.7(2) no O2 . TI1 . O21 . 89.1(2) no O3 2_577 TI1 . O21 . 158.4(2) no O6 . TI1 . O11 2_577 94.9(2) no O6 . TI1 . O21 . 97.0(2) no O11 2_577 TI1 . O21 . 78.3(2) no TI1 . TI2 . TI3 . 68.47(4) no TI1 . TI2 . O1 . 42.8(1) no TI3 . TI2 . O1 . 98.0(1) no TI1 . TI2 . O2 . 36.5(1) no TI3 . TI2 . O2 . 37.0(1) no O1 . TI2 . O2 . 77.1(2) no TI1 . TI2 . O3 . 98.8(1) no TI3 . TI2 . O3 . 43.0(1) no O1 . TI2 . O3 . 102.6(2) no O2 . TI2 . O3 . 78.0(2) no TI1 . TI2 . O4 . 140.1(2) no TI3 . TI2 . O4 . 143.4(2) no O1 . TI2 . O4 . 98.9(2) no O2 . TI2 . O4 . 175.6(2) no O3 . TI2 . O4 . 101.4(2) no TI1 . TI2 . O22 . 76.9(1) no TI3 . TI2 . O22 . 121.2(1) no O1 . TI2 . O22 . 85.8(2) no O2 . TI2 . O22 . 89.2(2) no O3 . TI2 . O22 . 162.5(2) no TI1 . TI2 . O31 . 117.9(1) no TI3 . TI2 . O31 . 78.4(1) no O1 . TI2 . O31 . 158.1(2) no O2 . TI2 . O31 . 87.9(2) no O3 . TI2 . O31 . 89.5(2) no O4 . TI2 . O22 . 92.3(2) no O4 . TI2 . O31 . 96.5(2) no O22 . TI2 . O31 . 78.1(2) no TI1 2_577 TI3 . TI2 . 68.15(4) no TI1 2_577 TI3 . O1 2_577 42.8(1) no TI2 . TI3 . O1 2_577 97.6(1) no TI1 2_577 TI3 . O2 . 97.8(1) no TI2 . TI3 . O2 . 43.1(1) no O1 2_577 TI3 . O2 . 101.2(2) no TI1 2_577 TI3 . O3 . 37.2(1) no TI2 . TI3 . O3 . 36.6(1) no O1 2_577 TI3 . O3 . 77.9(2) no O2 . TI3 . O3 . 77.6(2) no TI1 2_577 TI3 . O5 . 143.5(2) no TI2 . TI3 . O5 . 142.5(2) no O1 2_577 TI3 . O5 . 102.6(2) no O2 . TI3 . O5 . 101.5(2) no O3 . TI3 . O5 . 179.0(2) no TI1 2_577 TI3 . O12 . 77.2(1) no TI2 . TI3 . O12 . 118.3(1) no O1 2_577 TI3 . O12 . 88.7(2) no O2 . TI3 . O12 . 159.5(2) no O3 . TI3 . O12 . 87.2(2) no TI1 2_577 TI3 . O32 . 119.6(1) no TI2 . TI3 . O32 . 77.1(1) no O1 2_577 TI3 . O32 . 160.9(2) no O2 . TI3 . O32 . 87.5(2) no O3 . TI3 . O32 . 87.6(2) no O5 . TI3 . O12 . 93.6(2) no O5 . TI3 . O32 . 92.0(2) no O12 . TI3 . O32 . 78.1(2) no TI1 . O1 . TI2 . 100.3(2) no TI1 . O1 . TI3 2_577 100.6(2) no TI2 . O1 . TI3 2_577 135.0(2) no TI1 . O2 . TI2 . 100.9(2) no TI1 . O2 . TI3 . 135.1(3) no TI2 . O2 . TI3 . 99.9(2) no TI1 2_577 O3 . TI2 . 133.5(2) no TI1 2_577 O3 . TI3 . 99.9(2) no TI2 . O3 . TI3 . 100.4(2) no TI2 . O4 . C4 . 149.0(8) no TI3 . O5 . C6 . 156.9(9) no TI1 . O6 . C8 . 167.9(11) no TI1 2_577 O11 . C1 . 129.8(5) no TI3 . O12 . C1 . 130.4(5) no C16 . O13 . C41 . 116.2(7) no TI1 . O21 . C2 . 130.0(5) no TI2 . O22 . C2 . 129.2(4) no C26 . O23 . C51 . 122.9(7) no TI2 . O31 . C3 . 129.3(5) no TI3 . O32 . C3 . 129.5(5) no C36 . O33 . C61 . 117.0(6) no O11 . C1 . O12 . 124.5(7) no O11 . C1 . C11 . 119.9(7) no O12 . C1 . C11 . 115.5(7) no O21 . C2 . O22 . 125.1(6) no O21 . C2 . C21 . 115.6(6) no O22 . C2 . C21 . 119.3(6) no O31 . C3 . O32 . 124.3(7) no O31 . C3 . C31 . 116.2(7) no O32 . C3 . C31 . 119.3(7) no O4 . C4 . C5 . 113.8(18) no O5 . C6 . C7 . 115.3(15) no O6 . C8 . C9 . 124.8(21) no C1 . C11 . C12 . 118.1(7) no C1 . C11 . C16 . 122.9(7) no C12 . C11 . C16 . 118.9(7) no C11 . C12 . C13 . 120.8(8) no C11 . C12 . H121 . 119.6(7) no C13 . C12 . H121 . 119.6(8) no C12 . C13 . C14 . 120.1(9) no C12 . C13 . H131 . 120.0(9) no C14 . C13 . H131 . 120.0(9) no C13 . C14 . C15 . 120.1(8) no C13 . C14 . H141 . 120.0(10) no C15 . C14 . H141 . 119.9(9) no C14 . C15 . C16 . 119.5(7) no C14 . C15 . H151 . 120.2(8) no C16 . C15 . H151 . 120.2(9) no O13 . C16 . C11 . 121.4(7) no O13 . C16 . C15 . 118.0(7) no C11 . C16 . C15 . 120.5(8) no C2 . C21 . C22 . 117.0(7) no C2 . C21 . C26 . 124.9(7) no C22 . C21 . C26 . 117.9(7) no C21 . C22 . C23 . 120.9(8) no C21 . C22 . H221 . 119.5(8) no C23 . C22 . H221 . 119.6(8) no C22 . C23 . C24 . 119.9(8) no C22 . C23 . H231 . 120.1(9) no C24 . C23 . H231 . 120.0(9) no C23 . C24 . C25 . 120.6(8) no C23 . C24 . H241 . 119.7(10) no C25 . C24 . H241 . 119.7(10) no C24 . C25 . C26 . 119.1(8) no C24 . C25 . H251 . 120.5(9) no C26 . C25 . H251 . 120.4(10) no O23 . C26 . C21 . 117.8(7) no O23 . C26 . C25 . 120.7(8) no C21 . C26 . C25 . 121.5(8) no C3 . C31 . C32 . 117.3(7) no C3 . C31 . C36 . 121.9(7) no C32 . C31 . C36 . 120.7(7) no C31 . C32 . C33 . 120.9(8) no C31 . C32 . H321 . 119.6(8) no C33 . C32 . H321 . 119.5(8) no C32 . C33 . C34 . 118.7(8) no C32 . C33 . H331 . 120.6(9) no C34 . C33 . H331 . 120.7(8) no C33 . C34 . C35 . 121.0(8) no C33 . C34 . H341 . 119.4(9) no C35 . C34 . H341 . 119.6(9) no C34 . C35 . C36 . 119.8(8) no C34 . C35 . H351 . 120.1(8) no C36 . C35 . H351 . 120.1(8) no O33 . C36 . C31 . 120.6(7) no O33 . C36 . C35 . 120.5(7) no C31 . C36 . C35 . 118.8(7) no O13 . C41 . C42 . 120.2(9) no O13 . C41 . C46 . 116.5(11) no C42 . C41 . C46 . 123.3(11) no C41 . C42 . C43 . 116.7(12) no C41 . C42 . H421 . 121.7(11) no C43 . C42 . H421 . 121.6(13) no C42 . C43 . C44 . 121.4(16) no C42 . C43 . H431 . 119.3(16) no C44 . C43 . H431 . 119.3(17) no C43 . C44 . C45 . 118.9(16) no C43 . C44 . H441 . 120.6(26) no C45 . C44 . H441 . 120.5(25) no C44 . C45 . C46 . 122.5(17) no C44 . C45 . H451 . 118.9(23) no C46 . C45 . H451 . 118.6(24) no C41 . C46 . C45 . 117.0(15) no C41 . C46 . H461 . 121.4(12) no C45 . C46 . H461 . 121.5(14) no O23 . C51 . C52 . 124.6(12) no O23 . C51 . C56 . 116.4(12) no C52 . C51 . C56 . 118.9(10) no C51 . C52 . C53 . 119.3(13) no C51 . C52 . H521 . 120.3(12) no C53 . C52 . H521 . 120.4(14) no C52 . C53 . C54 . 120.3(13) no C52 . C53 . H531 . 119.7(16) no C54 . C53 . H531 . 120.0(16) no C53 . C54 . C55 . 122.2(14) no C53 . C54 . H541 . 118.9(20) no C55 . C54 . H541 . 119.0(20) no C54 . C55 . C56 . 117.4(16) no C54 . C55 . H551 . 121.2(16) no C56 . C55 . H551 . 121.4(18) no C51 . C56 . C55 . 121.8(14) no C51 . C56 . H561 . 119.1(13) no C55 . C56 . H561 . 119.1(16) no O33 . C61 . C62 . 117.4(8) no O33 . C61 . C66 . 120.3(8) no C62 . C61 . C66 . 122.2(8) no C61 . C62 . C63 . 117.8(10) no C61 . C62 . H621 . 121.1(9) no C63 . C62 . H621 . 121.1(10) no C62 . C63 . C64 . 118.5(10) no C62 . C63 . H631 . 120.8(14) no C64 . C63 . H631 . 120.7(13) no C63 . C64 . C65 . 123.0(10) no C63 . C64 . H641 . 118.6(15) no C65 . C64 . H641 . 118.5(15) no C64 . C65 . C66 . 118.7(11) no C64 . C65 . H651 . 120.7(13) no C66 . C65 . H651 . 120.6(14) no C61 . C66 . C65 . 119.8(10) no C61 . C66 . H661 . 120.1(10) no C65 . C66 . H661 . 120.2(11) no C102 . C101 . C106 . 131.7(16) no C102 . C101 . H1011 . 114.0(21) no C106 . C101 . H1011 . 114.2(21) no C101 . C102 . C103 . 110.0(13) no C101 . C102 . H1021 . 124.8(22) no C103 . C102 . H1021 . 125.1(21) no C102 . C103 . C104 . 119.6(12) no C102 . C103 . H1031 . 119.9(18) no C104 . C103 . H1031 . 120.5(17) no C103 . C104 . C105 . 125.7(12) no C103 . C104 . C107 . 117.2(14) no C105 . C104 . C107 . 117.1(14) no C104 . C105 . C106 . 116.8(12) no C104 . C105 . H1051 . 121.8(20) no C106 . C105 . H1051 . 121.4(21) no C101 . C106 . C105 . 116.1(14) no C101 . C106 . H1061 . 121.6(23) no C105 . C106 . H1061 . 122.2(22) no C202 . C201 . C206 . 121.5(13) no C202 . C201 . H2011 . 119.5(14) no C206 . C201 . H2011 . 119.1(15) no C201 . C202 . C203 . 117.5(12) no C201 . C202 . C207 . 122.5(13) no C203 . C202 . C207 . 120.0(13) no C202 . C203 . C204 . 120.9(12) no C202 . C203 . H2031 . 119.4(16) no C204 . C203 . H2031 . 119.7(17) no C203 . C204 . C205 . 121.8(12) no C203 . C204 . H2041 . 119.1(19) no C205 . C204 . H2041 . 119.1(19) no C204 . C205 . C206 . 117.9(12) no C204 . C205 . H2051 . 121.0(18) no C206 . C205 . H2051 . 121.1(18) no C201 . C206 . C205 . 120.2(12) no C201 . C206 . H2061 . 120.0(17) no C205 . C206 . H2061 . 119.7(17) no