# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2004 #======================================================================== data_global #======================================================================== _audit_creation_date 24-05-01 # 1. SUBMISSION DETAILS _publ_contact_author_name 'Marc HENRY' _publ_contact_author_address ; Université Louis Pasteur, Institut Le Bel Laboratoire de Chimie Moléculaire de l'État Solide UMR CNRS/ULP 7513 4, Rue Blaise Pascal 67070 Strasbourg Cedex, France ; _publ_contact_author_phone '+33.3.90.24.13.56' _publ_contact_author_fax '+33.3.90.24.13.25' _publ_contact_author_email 'henry@chimie.u-strasbg.fr' _publ_requested_journal 'New J. Chem.' _publ_contact_letter ; Please consider this CIF submission for publication as a 2 new structures and 3 theoretical ones in New J. Chem. ; #========================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_coden_Cambridge 440 _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? #=========================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; General principles driving the chemical reactivity of titanium(IV) alkoxides ; loop_ _publ_author_name _publ_author_address 'Biechel, Frédérique' ; LCMES Université Louis Pasteur Strasbourg France ; 'Dubuc, Julien' ; LCMES Université Louis Pasteur Strasbourg France ; 'Henry, Marc' ; LCMES Université Louis Pasteur Strasbourg France ; # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. Enraf-Nonius, Cad4-Express Operations Manual, Delft, 1994. Fair, C.K. (1990). MolEN, An Interactive Intelligent System for Crystal Structure Analysis, User Manual, Enraf - Nonius, Delft, The Netherlands. North, A.C.T., Phillips, D.C., Mathews, F.S. (1968). Acta Cryst., A24, 351-359. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #========================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. data_ST993 _database_code_depnum_ccdc_archive 'CCDC 168599' #======================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; (µ2-1,3-propanediolato(O,O'))-bis(µ4-oxo)-bis(µ3-oxo)-octakis(µ2-ethoxo)- decakis(ethoxy)-hepta-titanium ; _chemical_name_common 'lid-shaped heptatitanate' _chemical_formula_moiety 'C39H96O24Ti7' _chemical_formula_structural '[Ti7(µ2-O(CH2)3-O)(µ4-O)2(µ3-O)2(µ2-OC2H5)8(OC2H5)10]' _chemical_formula_analytical ? _chemical_formula_sum 'C39H96O24Ti7' _chemical_formula_weight 1284.49 _chemical_melting_point ? _chemical_compound_source 'Synthetic' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 Ti ? 0.248 0.446 International_Tables_Vol_IV_Table_2.3.1 #========================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,-y,-z _cell_length_a 12.0601(8) _cell_length_b 13.733(1) _cell_length_c 20.595(2) _cell_angle_alpha 105.244(6) _cell_angle_beta 91.599(7) _cell_angle_gamma 108.298(6) _cell_volume 3101(1) _cell_formula_units_z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 18.5 _cell_measurement_theta_max 22.5 _cell_special_details ; ? ; _exptl_crystal_description prism _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.38 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 0.912 _exptl_absorpt_correction_type psi_scans_(North,_Phillips,_Mathews,_1968) _exptl_absorpt_correction_T_min 0.9210 _exptl_absorpt_correction_T_max 1.0000 #========================================================================= # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device Enraf_Nonius_CAD4 _diffrn_measurement_method \q/2\q _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 5 -6 2 -1 -5 0 -3 1 -7 _diffrn_reflns_number 12914 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 26.29 _reflns_number_total 12549 _reflns_number_observed 6263 _reflns_observed_criterion >3.0\s(I) _computing_data_collection 'CAD4_(Enraf-Nonius,_1994)' _computing_cell_refinement CAD4_(Enraf-Nonius,_1994) _computing_data_reduction 'process_MolEN_(Fair,_1990)' _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_MolEN_(Fair,_1990) _computing_molecular_graphics ? _computing_publication_material BTABLE_PTABLE_CIF_IN_MolEN_(Fair,_1990) #========================================================================= # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^) + 0.0064 Fo^4^)' _refine_ls_hydrogen_treatment included_not_refined _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 6263 _refine_ls_number_parameters 608 _refine_ls_number_restraints 0 _refine_ls_number_constraints 8 _refine_ls_abs_structure_details ; ? ; _refine_ls_R_factor_all 0.148 _refine_ls_R_factor_obs 0.051 _refine_ls_wR_factor_all 0.171 _refine_ls_wR_factor_obs 0.074 _refine_ls_goodness_of_fit_all 3.450 _refine_ls_goodness_of_fit_obs 1.390 _refine_ls_shift/esd_max 0.055 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.876 _refine_diff_density_min -0.257 #========================================================================= # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol TI1 0.31765(7) 0.30102(7) 0.29354(4) 0.0277(4) Uij ? ? Ti TI2 0.37977(8) 0.30609(8) 0.14958(5) 0.0333(5) Uij ? ? Ti TI3 0.42967(8) 0.52741(8) 0.26642(5) 0.0345(5) Uij ? ? Ti TI4 0.15124(8) 0.41926(7) 0.26313(5) 0.0336(4) Uij ? ? Ti TI5 0.05034(8) 0.19571(8) 0.29464(5) 0.0331(4) Uij ? ? Ti TI6 0.23066(9) 0.08683(8) 0.33814(5) 0.0390(5) Uij ? ? Ti TI7 0.28870(8) 0.08659(8) 0.18702(5) 0.0340(5) Uij ? ? Ti O1 0.2981(3) 0.3840(2) 0.2289(2) 0.028(2) Uij ? ? O O2 0.1821(3) 0.3334(3) 0.3236(2) 0.031(2) Uij ? ? O O3 0.2006(3) 0.1516(3) 0.2634(2) 0.030(2) Uij ? ? O O4 0.3956(3) 0.2407(3) 0.2232(2) 0.031(2) Uij ? ? O O5 0.3570(3) 0.2461(3) 0.3656(2) 0.036(2) Uij ? ? O C1 0.4494(6) 0.2910(5) 0.4208(3) 0.055(3) Uij ? ? C C2 0.5493(5) 0.3782(5) 0.4090(3) 0.055(3) Uij ? ? C C3 0.5185(5) 0.4683(5) 0.3965(3) 0.045(3) Uij ? ? C O6 0.4418(3) 0.4360(3) 0.3350(2) 0.032(2) Uij ? ? O O7 0.2467(3) 0.1658(3) 0.1253(2) 0.035(2) Uij ? ? O C4 0.1623(5) 0.1208(5) 0.0654(3) 0.045(3) Uij ? ? C C5 0.2168(7) 0.0758(7) 0.0044(3) 0.062(5) Uij ? ? C O8 0.4865(3) 0.2664(3) 0.0982(2) 0.043(2) Uij ? ? O C6 0.5324(6) 0.2925(7) 0.0415(3) 0.078(4) Uij ? ? C C7 0.6504(6) 0.2868(7) 0.0329(4) 0.079(4) Uij ? ? C O9 0.3211(3) 0.3576(3) 0.0906(2) 0.043(2) Uij ? ? O C8 0.2475(5) 0.3972(5) 0.0603(3) 0.062(3) Uij ? ? C C9 0.2715(7) 0.3992(7) -0.0099(4) 0.101(5) Uij ? ? C O10 0.5110(3) 0.4422(3) 0.2051(2) 0.037(2) Uij ? ? O C10 0.6288(6) 0.4421(6) 0.2234(4) 0.064(4) Uij ? ? C C11 0.7197(7) 0.5243(8) 0.2046(5) 0.094(6) Uij ? ? C O11 0.5515(3) 0.6324(3) 0.3229(2) 0.044(2) Uij ? ? O C12 0.6223(9) 0.7361(8) 0.3344(5) 0.101(7) Uij ? ? C C13 0.718(1) 0.777(1) 0.3756(8) 0.16(1) Uij ? ? C O12 0.4167(3) 0.5980(3) 0.2068(2) 0.051(2) Uij ? ? O C14 0.483(1) 0.6382(7) 0.1582(5) 0.104(6) Uij ? ? C C15 0.466(1) 0.7289(8) 0.1479(5) 0.135(8) Uij ? ? C O13 0.2922(3) 0.5519(3) 0.3096(2) 0.037(2) Uij ? ? O C16 0.2908(5) 0.6536(5) 0.3482(3) 0.051(3) Uij ? ? C C17 0.3411(7) 0.6788(7) 0.4196(4) 0.080(5) Uij ? ? C O14 0.1153(3) 0.4585(3) 0.1899(2) 0.047(2) Uij ? ? O C18 0.0693(6) 0.5362(5) 0.1805(4) 0.088(4) Uij ? ? C C19 0.0023(7) 0.5063(7) 0.1135(4) 0.123(5) Uij ? ? C O15 0.0567(3) 0.4728(3) 0.3161(2) 0.047(2) Uij ? ? O C20 0.0203(7) 0.4927(6) 0.3823(4) 0.084(5) Uij ? ? C C21 -0.0912(9) 0.5143(9) 0.3798(6) 0.204(7) Uij ? ? C O16 0.0430(3) 0.2678(3) 0.2218(2) 0.034(2) Uij ? ? O C22 -0.0448(5) 0.2300(5) 0.1642(3) 0.052(3) Uij ? ? C C23 -0.1527(6) 0.2552(7) 0.1829(4) 0.078(4) Uij ? ? C O17 -0.0588(3) 0.2359(3) 0.3442(2) 0.047(2) Uij ? ? O C24 -0.1763(6) 0.1836(7) 0.3513(4) 0.074(5) Uij ? ? C C25 -0.2123(7) 0.2342(7) 0.4145(4) 0.109(5) Uij ? ? C O18 -0.0459(3) 0.0679(3) 0.2451(2) 0.041(2) Uij ? ? O C26 -0.0782(6) -0.0302(5) 0.1942(3) 0.052(4) Uij ? ? C C27 -0.2019(7) -0.0936(7) 0.1906(5) 0.085(6) Uij ? ? C O19 0.1124(3) 0.1531(3) 0.3731(2) 0.041(2) Uij ? ? O C28 0.1134(7) 0.2099(8) 0.4441(4) 0.166(5) Uij ? ? C C29 0.048(1) 0.153(1) 0.4775(6) 0.22(1) Uij ? ? C O20 0.1249(3) -0.0433(3) 0.3120(2) 0.050(2) Uij ? ? O C30 0.0296(9) -0.1068(7) 0.3317(5) 0.094(6) Uij ? ? C C31 0.0007(9) -0.2225(6) 0.2983(6) 0.101(7) Uij ? ? C O21 0.3336(3) 0.0456(3) 0.2703(2) 0.042(2) Uij ? ? O C32 0.3834(6) -0.0359(5) 0.2695(4) 0.082(4) Uij ? ? C C33 0.4966(7) 0.0067(8) 0.3131(5) 0.139(6) Uij ? ? C O22 0.2957(3) 0.0765(3) 0.4154(2) 0.058(1) Uiso ? ? O C34 0.2790 -0.0056 0.4523 0.1298 Uiso ? ? C C35 0.3577 0.0198 0.4967 0.1267 Uiso ? ? C O23 0.4030(3) 0.0458(3) 0.1462(2) 0.047(2) Uij ? ? O C36 0.5292(5) 0.0795(6) 0.1509(4) 0.072(4) Uij ? ? C C37 0.5660(8) 0.0117(8) 0.1003(7) 0.138(7) Uij ? ? C O24 0.1708(3) -0.0358(3) 0.1446(2) 0.046(2) Uij ? ? O C38 0.1634(7) -0.1421(6) 0.1082(5) 0.083(5) Uij ? ? C C39 0.069(1) -0.1914(8) 0.0547(6) 0.115(7) Uij ? ? C H1 0.4775 0.2361 0.4265 0.0790 Uiso calc C1 H H2 0.4189 0.3191 0.4608 0.0790 Uiso calc C1 H H3 0.5824 0.3482 0.3706 0.0764 Uiso calc C2 H H4 0.6063 0.4059 0.4478 0.0764 Uiso calc C2 H H5 0.5887 0.5225 0.3937 0.0665 Uiso calc C3 H H6 0.4807 0.4961 0.4332 0.0665 Uiso calc C3 H H7 0.1354 0.1751 0.0574 0.0662 Uiso calc C4 H H8 0.0977 0.0651 0.0723 0.0662 Uiso calc C4 H H9 0.1597 0.0466 -0.0345 0.1102 Uiso calc C5 H H10 0.2813 0.1313 -0.0028 0.1102 Uiso calc C5 H H11 0.2435 0.0213 0.0121 0.1102 Uiso calc C5 H H12 0.5353 0.3635 0.0448 0.1048 Uiso calc C6 H H13 0.4809 0.2446 0.0025 0.1048 Uiso calc C6 H H14 0.6747 0.3058 -0.0069 0.1101 Uiso calc C7 H H15 0.7038 0.3350 0.0711 0.1101 Uiso calc C7 H H16 0.6494 0.2160 0.0288 0.1101 Uiso calc C7 H H17 0.2581 0.4681 0.0870 0.0753 Uiso calc C8 H H18 0.1684 0.3533 0.0588 0.0753 Uiso calc C8 H H19 0.2190 0.4269 -0.0283 0.1216 Uiso calc C9 H H20 0.3502 0.4434 -0.0090 0.1216 Uiso calc C9 H H21 0.2605 0.3286 -0.0372 0.1216 Uiso calc C9 H H22 0.6344 0.3742 0.2008 0.0919 Uiso calc C10 H H23 0.6410 0.4541 0.2710 0.0919 Uiso calc C10 H H24 0.7947 0.5215 0.2174 0.1498 Uiso calc C11 H H25 0.7086 0.5126 0.1570 0.1498 Uiso calc C11 H H26 0.7152 0.5926 0.2272 0.1498 Uiso calc C11 H H27 0.5748 0.7789 0.3505 0.1723 Uiso calc C12 H H28 0.6440 0.7437 0.2915 0.1723 Uiso calc C12 H H29 0.7545 0.8498 0.3765 0.2755 Uiso calc C13 H H30 0.7008 0.7736 0.4198 0.2755 Uiso calc C13 H H31 0.7701 0.7384 0.3608 0.2755 Uiso calc C13 H H32 0.4616 0.5836 0.1162 0.1488 Uiso calc C14 H H33 0.5639 0.6554 0.1728 0.1488 Uiso calc C14 H H34 0.5135 0.7507 0.1147 0.1932 Uiso calc C15 H H35 0.3858 0.7130 0.1326 0.1932 Uiso calc C15 H H36 0.4881 0.7849 0.1892 0.1932 Uiso calc C15 H H37 0.2119 0.6534 0.3472 0.0688 Uiso calc C16 H H38 0.3359 0.7068 0.3289 0.0688 Uiso calc C16 H H39 0.3393 0.7471 0.4444 0.1198 Uiso calc C17 H H40 0.2961 0.6260 0.4392 0.1198 Uiso calc C17 H H41 0.4202 0.6794 0.4209 0.1198 Uiso calc C17 H H42 0.1327 0.6008 0.1857 0.1006 Uiso calc C18 H H43 0.0187 0.5474 0.2141 0.1006 Uiso calc C18 H H44 -0.0265 0.5620 0.1102 0.1443 Uiso calc C19 H H45 0.0520 0.4955 0.0793 0.1443 Uiso calc C19 H H46 -0.0620 0.4421 0.1076 0.1443 Uiso calc C19 H H47 0.0787 0.5529 0.4122 0.1148 Uiso calc C20 H H48 0.0099 0.4318 0.3981 0.1148 Uiso calc C20 H H49 -0.1152 0.5275 0.4239 0.2268 Uiso calc C21 H H50 -0.0809 0.5752 0.3640 0.2268 Uiso calc C21 H H51 -0.1497 0.4541 0.3499 0.2268 Uiso calc C21 H H52 -0.0645 0.1547 0.1467 0.0692 Uiso calc C22 H H53 -0.0140 0.2633 0.1306 0.0692 Uiso calc C22 H H54 -0.2091 0.2293 0.1439 0.1137 Uiso calc C23 H H55 -0.1843 0.2219 0.2164 0.1137 Uiso calc C23 H H56 -0.1338 0.3305 0.2003 0.1137 Uiso calc C23 H H57 -0.1853 0.1117 0.3498 0.1184 Uiso calc C24 H H58 -0.2256 0.1840 0.3146 0.1184 Uiso calc C24 H H59 -0.2921 0.1959 0.4168 0.1364 Uiso calc C25 H H60 -0.1640 0.2337 0.4516 0.1364 Uiso calc C25 H H61 -0.2043 0.3060 0.4164 0.1364 Uiso calc C25 H H62 -0.0311 -0.0702 0.2033 0.0749 Uiso calc C26 H H63 -0.0645 -0.0164 0.1518 0.0749 Uiso calc C26 H H64 -0.2196 -0.1590 0.1555 0.1404 Uiso calc C27 H H65 -0.2165 -0.1084 0.2326 0.1404 Uiso calc C27 H H66 -0.2499 -0.0547 0.1811 0.1404 Uiso calc C27 H H67 0.0875 0.2688 0.4454 0.1977 Uiso calc C28 H H68 0.1919 0.2354 0.4656 0.1977 Uiso calc C28 H H69 0.0529 0.1947 0.5230 0.2663 Uiso calc C29 H H70 -0.0316 0.1270 0.4571 0.2663 Uiso calc C29 H H71 0.0729 0.0936 0.4773 0.2663 Uiso calc C29 H H72 -0.0362 -0.0868 0.3219 0.1316 Uiso calc C30 H H73 0.0437 -0.0949 0.3792 0.1316 Uiso calc C30 H H74 -0.0669 -0.2614 0.3147 0.1688 Uiso calc C31 H H75 -0.0148 -0.2362 0.2507 0.1688 Uiso calc C31 H H76 0.0652 -0.2443 0.3079 0.1688 Uiso calc C31 H H77 0.3956 -0.0661 0.2243 0.0961 Uiso calc C32 H H78 0.3302 -0.0898 0.2851 0.0961 Uiso calc C32 H H79 0.5273 -0.0495 0.3114 0.1742 Uiso calc C33 H H80 0.5504 0.0605 0.2976 0.1742 Uiso calc C33 H H81 0.4850 0.0368 0.3584 0.1742 Uiso calc C33 H H82 0.2759 -0.0715 0.4213 0.1687 Uiso calc C34 H H83 0.2070 -0.0144 0.4715 0.1687 Uiso calc C34 H H84 0.3444 -0.0341 0.5193 0.1646 Uiso calc C35 H H85 0.4300 0.0284 0.4779 0.1646 Uiso calc C35 H H86 0.3611 0.0855 0.5282 0.1646 Uiso calc C35 H H87 0.5597 0.0792 0.1938 0.0954 Uiso calc C36 H H88 0.5580 0.1499 0.1464 0.0954 Uiso calc C36 H H89 0.6495 0.0356 0.1045 0.2149 Uiso calc C37 H H90 0.5377 -0.0589 0.1046 0.2149 Uiso calc C37 H H91 0.5360 0.0118 0.0572 0.2149 Uiso calc C37 H H92 0.1526 -0.1841 0.1389 0.1306 Uiso calc C38 H H93 0.2349 -0.1395 0.0894 0.1306 Uiso calc C38 H H94 0.0678 -0.2616 0.0322 0.1774 Uiso calc C39 H H95 -0.0035 -0.1950 0.0729 0.1774 Uiso calc C39 H H96 0.0788 -0.1504 0.0233 0.1774 Uiso calc C39 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol TI1 0.0270(4) 0.0329(4) 0.0239(4) 0.0092(3) 0.0011(4) 0.0051(4) Ti TI2 0.0318(4) 0.0442(5) 0.0263(4) 0.0118(4) 0.0062(4) 0.0061(4) Ti TI3 0.0333(5) 0.0362(5) 0.0341(5) 0.0058(4) 0.0046(4) 0.0078(4) Ti TI4 0.0315(4) 0.0380(5) 0.0317(4) 0.0147(3) 0.0050(4) 0.0088(4) Ti TI5 0.0279(4) 0.0397(5) 0.0327(5) 0.0089(4) 0.0063(4) 0.0102(4) Ti TI6 0.0430(5) 0.0377(5) 0.0367(5) 0.0133(4) 0.0007(4) 0.0125(4) Ti TI7 0.0316(4) 0.0359(5) 0.0348(5) 0.0121(4) 0.0032(4) 0.0007(4) Ti O1 0.027(2) 0.029(2) 0.028(2) 0.009(1) 0.003(1) 0.005(1) O O2 0.031(2) 0.039(2) 0.024(2) 0.011(1) 0.004(1) 0.008(1) O O3 0.028(2) 0.034(2) 0.027(2) 0.007(1) 0.003(1) 0.005(1) O O4 0.028(2) 0.035(2) 0.029(2) 0.011(1) 0.003(1) 0.006(1) O O5 0.035(2) 0.042(2) 0.031(2) 0.012(1) -0.005(1) 0.009(1) O C1 0.066(4) 0.049(3) 0.053(3) 0.004(3) -0.034(3) 0.013(3) C C2 0.048(3) 0.055(3) 0.063(4) 0.005(3) -0.023(3) 0.018(3) C C3 0.057(4) 0.043(3) 0.038(3) 0.000(3) -0.017(3) 0.008(2) C O6 0.034(2) 0.038(2) 0.027(2) 0.006(1) -0.004(1) 0.004(1) O O7 0.033(2) 0.045(2) 0.028(2) 0.009(1) 0.001(2) 0.001(2) O C4 0.038(3) 0.062(4) 0.038(3) 0.003(3) -0.012(3) 0.007(3) C C5 0.080(5) 0.103(6) 0.029(3) 0.002(5) -0.002(4) -0.016(4) C O8 0.043(2) 0.058(2) 0.032(2) 0.019(2) 0.015(2) 0.009(2) O C6 0.059(3) 0.141(6) 0.057(4) 0.045(3) 0.028(3) 0.036(4) C C7 0.049(3) 0.148(6) 0.068(4) 0.038(4) 0.027(3) 0.041(4) C O9 0.046(2) 0.055(2) 0.032(2) 0.019(2) 0.007(2) 0.017(2) O C8 0.061(3) 0.070(3) 0.055(3) 0.029(3) 0.007(3) 0.029(3) C C9 0.109(5) 0.137(5) 0.069(4) 0.062(4) 0.009(4) 0.058(3) C O10 0.027(2) 0.052(2) 0.036(2) 0.009(1) 0.006(2) 0.009(2) O C10 0.047(3) 0.082(5) 0.067(4) 0.018(3) 0.015(3) -0.002(4) C C11 0.051(4) 0.108(7) 0.150(8) 0.009(4) 0.025(5) -0.005(6) C O11 0.047(2) 0.036(2) 0.050(2) -0.001(2) 0.000(2) 0.009(2) O C12 0.107(7) 0.109(7) 0.088(6) -0.043(6) 0.015(6) -0.033(6) C C13 0.090(8) 0.18(1) 0.24(1) -0.025(8) 0.008(9) -0.07(1) C O12 0.053(2) 0.054(2) 0.046(2) 0.008(2) 0.011(2) 0.023(2) O C14 0.157(9) 0.080(5) 0.089(6) 0.012(6) -0.016(6) 0.034(4) C C15 0.24(1) 0.107(7) 0.095(6) 0.039(7) 0.014(8) 0.044(5) C O13 0.043(2) 0.032(2) 0.036(2) 0.015(1) 0.006(2) 0.006(1) O C16 0.057(3) 0.038(3) 0.061(4) 0.018(2) 0.012(3) 0.005(3) C C17 0.087(5) 0.109(6) 0.054(4) 0.040(4) -0.007(4) -0.027(4) C O14 0.042(2) 0.051(2) 0.049(2) 0.024(1) 0.005(2) 0.021(2) O C18 0.082(4) 0.095(4) 0.089(5) 0.057(3) 0.014(4) 0.049(3) C C19 0.101(5) 0.180(6) 0.102(5) 0.083(4) 0.010(4) 0.080(4) C O15 0.044(2) 0.050(2) 0.046(2) 0.024(1) 0.014(2) 0.010(2) O C20 0.101(5) 0.074(5) 0.079(5) 0.026(4) 0.050(4) 0.004(4) C C21 0.196(6) 0.206(8) 0.210(8) 0.137(5) 0.164(5) 0.106(7) C O16 0.031(2) 0.041(2) 0.030(2) 0.013(1) -0.001(1) 0.011(1) O C22 0.048(3) 0.056(3) 0.051(3) 0.010(3) -0.012(3) 0.018(3) C C23 0.035(3) 0.131(5) 0.103(5) 0.018(3) -0.007(3) 0.057(4) C O17 0.032(2) 0.070(2) 0.047(2) 0.014(2) 0.014(2) 0.019(2) O C24 0.046(4) 0.130(7) 0.070(4) 0.006(4) 0.030(3) 0.008(5) C C25 0.083(4) 0.133(6) 0.118(5) 0.052(4) 0.070(4) 0.042(5) C O18 0.034(2) 0.046(2) 0.044(2) 0.003(2) 0.004(2) 0.015(2) O C26 0.061(4) 0.044(3) 0.052(4) -0.000(3) -0.004(3) 0.009(3) C C27 0.058(5) 0.086(6) 0.121(7) -0.026(5) 0.005(5) -0.007(6) C O19 0.045(2) 0.049(2) 0.032(2) 0.012(2) 0.010(2) 0.014(2) O C28 0.155(5) 0.335(7) 0.088(4) 0.188(4) 0.083(4) 0.128(4) C C29 0.186(9) 0.36(1) 0.162(9) 0.160(8) 0.099(7) 0.140(8) C O20 0.045(2) 0.043(2) 0.063(2) 0.003(2) 0.012(2) 0.022(2) O C30 0.131(7) 0.069(5) 0.091(6) 0.021(5) -0.006(6) 0.020(4) C C31 0.136(8) 0.039(4) 0.19(1) 0.011(5) 0.058(7) 0.017(6) C O21 0.040(2) 0.041(2) 0.047(2) 0.018(1) 0.003(2) 0.008(2) O C32 0.087(4) 0.069(3) 0.092(5) 0.051(3) 0.024(4) 0.035(3) C C33 0.103(4) 0.222(7) 0.118(7) 0.112(4) 0.002(5) 0.046(6) C O23 0.039(2) 0.053(2) 0.052(2) 0.021(2) 0.007(2) -0.001(2) O C36 0.042(3) 0.086(4) 0.104(5) 0.035(3) 0.022(3) 0.029(4) C C37 0.098(5) 0.107(7) 0.25(1) 0.033(5) 0.086(6) -0.023(7) C O24 0.048(2) 0.041(2) 0.051(2) 0.008(2) 0.004(2) -0.002(2) O C38 0.079(5) 0.066(5) 0.110(6) 0.014(4) -0.013(5) -0.037(5) C C39 0.128(8) 0.088(6) 0.136(8) 0.022(6) -0.028(7) -0.042(6) C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag TI1 O1 2.019(3) . . ? TI1 O2 1.903(3) . . ? TI1 O3 2.013(3) . . ? TI1 O4 1.897(3) . . ? TI1 O5 1.941(3) . . ? TI1 O6 1.939(3) . . ? TI2 O1 2.148(2) . . ? TI2 O4 1.987(3) . . ? TI2 O7 2.011(3) . . ? TI2 O8 1.812(3) . . ? TI2 O9 1.787(3) . . ? TI2 O10 2.055(3) . . ? TI3 O1 2.041(3) . . ? TI3 O6 2.151(3) . . ? TI3 O10 1.985(3) . . ? TI3 O11 1.812(3) . . ? TI3 O12 1.784(3) . . ? TI3 O13 1.982(3) . . ? TI4 O1 2.073(3) . . ? TI4 O2 2.026(3) . . ? TI4 O13 2.042(3) . . ? TI4 O14 1.815(3) . . ? TI4 O15 1.790(3) . . ? TI4 O16 2.015(3) . . ? TI5 O2 1.980(3) . . ? TI5 O3 2.148(3) . . ? TI5 O16 2.017(3) . . ? TI5 O17 1.820(3) . . ? TI5 O18 1.784(3) . . ? TI5 O19 2.053(3) . . ? TI6 O3 2.046(3) . . ? TI6 O5 2.153(3) . . ? TI6 O19 1.977(3) . . ? TI6 O20 1.771(3) . . ? TI6 O21 1.984(3) . . ? TI6 O22 1.813(3) . . ? TI7 O3 2.086(3) . . ? TI7 O4 2.025(3) . . ? TI7 O7 2.024(3) . . ? TI7 O21 2.048(3) . . ? TI7 O23 1.794(3) . . ? TI7 O24 1.808(3) . . ? O5 C1 1.430(5) . . ? C1 C2 1.486(7) . . ? C2 C3 1.478(7) . . ? C3 O6 1.428(5) . . ? O7 C4 1.439(5) . . ? C4 C5 1.512(7) . . ? O8 C6 1.390(6) . . ? C6 C7 1.462(7) . . ? O9 C8 1.387(5) . . ? C8 C9 1.488(7) . . ? O10 C10 1.461(6) . . ? C10 C11 1.449(9) . . ? O11 C12 1.365(8) . . ? C12 C13 1.29(1) . . ? O12 C14 1.416(8) . . ? C14 C15 1.39(1) . . ? O13 C16 1.420(5) . . ? C16 C17 1.483(7) . . ? O14 C18 1.398(6) . . ? C18 C19 1.469(9) . . ? O15 C20 1.428(6) . . ? C20 C21 1.47(1) . . ? O16 C22 1.434(5) . . ? C22 C23 1.483(7) . . ? O17 C24 1.405(6) . . ? C24 C25 1.453(8) . . ? O18 C26 1.404(5) . . ? C26 C27 1.460(7) . . ? O19 C28 1.464(9) . . ? C28 C29 1.28(1) . . ? O20 C30 1.352(8) . . ? C30 C31 1.478(9) . . ? O21 C32 1.424(6) . . ? C32 C33 1.472(9) . . ? O22 C34 1.486(3) . . ? C34 C35 1.1969 . . ? O23 C36 1.437(6) . . ? C36 C37 1.387(9) . . ? O24 C38 1.428(6) . . ? C38 C39 1.42(1) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 TI1 O2 81.0(1) . . . ? O1 TI1 O3 110.4(1) . . . ? O1 TI1 O4 81.9(1) . . . ? O1 TI1 O5 169.5(1) . . . ? O1 TI1 O6 80.0(1) . . . ? O2 TI1 O3 81.6(1) . . . ? O2 TI1 O4 150.3(1) . . . ? O2 TI1 O5 99.9(1) . . . ? O2 TI1 O6 101.6(1) . . . ? O3 TI1 O4 81.7(1) . . . ? O3 TI1 O5 80.1(1) . . . ? O3 TI1 O6 169.6(1) . . . ? O4 TI1 O5 101.2(1) . . . ? O4 TI1 O6 99.2(1) . . . ? O5 TI1 O6 89.6(1) . . . ? O1 TI2 O4 76.7(1) . . . ? O1 TI2 O7 94.3(1) . . . ? O1 TI2 O8 163.6(1) . . . ? O1 TI2 O9 90.6(1) . . . ? O1 TI2 O10 74.4(1) . . . ? O4 TI2 O7 74.8(1) . . . ? O4 TI2 O8 98.9(1) . . . ? O4 TI2 O9 162.4(1) . . . ? O4 TI2 O10 88.0(1) . . . ? O7 TI2 O8 99.8(1) . . . ? O7 TI2 O9 94.4(1) . . . ? O7 TI2 O10 161.3(1) . . . ? O8 TI2 O9 96.6(1) . . . ? O8 TI2 O10 89.8(1) . . . ? O9 TI2 O10 100.4(1) . . . ? O1 TI3 O6 74.7(1) . . . ? O1 TI3 O10 78.3(1) . . . ? O1 TI3 O11 159.6(1) . . . ? O1 TI3 O12 103.1(1) . . . ? O1 TI3 O13 76.3(1) . . . ? O6 TI3 O10 86.6(1) . . . ? O6 TI3 O11 84.9(1) . . . ? O6 TI3 O12 177.6(1) . . . ? O6 TI3 O13 87.9(1) . . . ? O10 TI3 O11 102.2(1) . . . ? O10 TI3 O12 92.0(1) . . . ? O10 TI3 O13 154.6(1) . . . ? O11 TI3 O12 97.3(1) . . . ? O11 TI3 O13 102.0(1) . . . ? O12 TI3 O13 92.5(1) . . . ? O1 TI4 O2 76.9(1) . . . ? O1 TI4 O13 74.3(1) . . . ? O1 TI4 O14 95.4(1) . . . ? O1 TI4 O15 161.9(1) . . . ? O1 TI4 O16 93.1(1) . . . ? O2 TI4 O13 93.8(1) . . . ? O2 TI4 O14 162.9(1) . . . ? O2 TI4 O15 95.0(1) . . . ? O2 TI4 O16 73.8(1) . . . ? O13 TI4 O14 98.8(1) . . . ? O13 TI4 O15 90.4(1) . . . ? O13 TI4 O16 164.3(1) . . . ? O14 TI4 O15 96.4(1) . . . ? O14 TI4 O16 91.6(1) . . . ? O15 TI4 O16 100.2(1) . . . ? O2 TI5 O3 76.5(1) . . . ? O2 TI5 O16 74.7(1) . . . ? O2 TI5 O17 98.8(1) . . . ? O2 TI5 O18 162.0(1) . . . ? O2 TI5 O19 88.6(1) . . . ? O3 TI5 O16 94.9(1) . . . ? O3 TI5 O17 164.1(1) . . . ? O3 TI5 O18 90.5(1) . . . ? O3 TI5 O19 73.7(1) . . . ? O16 TI5 O17 98.5(1) . . . ? O16 TI5 O18 94.3(1) . . . ? O16 TI5 O19 161.8(1) . . . ? O17 TI5 O18 96.9(1) . . . ? O17 TI5 O19 91.1(1) . . . ? O18 TI5 O19 99.9(1) . . . ? O3 TI6 O5 74.6(1) . . . ? O3 TI6 O19 77.6(1) . . . ? O3 TI6 O20 102.8(1) . . . ? O3 TI6 O21 76.8(1) . . . ? O3 TI6 O22 159.6(1) . . . ? O5 TI6 O19 87.1(1) . . . ? O5 TI6 O20 177.4(1) . . . ? O5 TI6 O21 87.2(1) . . . ? O5 TI6 O22 85.0(1) . . . ? O19 TI6 O20 92.6(1) . . . ? O19 TI6 O21 154.4(1) . . . ? O19 TI6 O22 101.2(1) . . . ? O20 TI6 O21 91.9(1) . . . ? O20 TI6 O22 97.6(2) . . . ? O21 TI6 O22 103.1(1) . . . ? O3 TI7 O4 77.0(1) . . . ? O3 TI7 O7 92.1(1) . . . ? O3 TI7 O21 74.6(1) . . . ? O3 TI7 O23 159.9(1) . . . ? O3 TI7 O24 99.0(1) . . . ? O4 TI7 O7 73.7(1) . . . ? O4 TI7 O21 93.7(1) . . . ? O4 TI7 O23 92.3(1) . . . ? O4 TI7 O24 165.2(1) . . . ? O7 TI7 O21 163.6(1) . . . ? O7 TI7 O23 101.3(1) . . . ? O7 TI7 O24 92.4(1) . . . ? O21 TI7 O23 89.5(1) . . . ? O21 TI7 O24 99.0(1) . . . ? O23 TI7 O24 95.4(1) . . . ? TI1 O1 TI2 95.7(1) . . . ? TI1 O1 TI3 103.2(1) . . . ? TI1 O1 TI4 98.2(1) . . . ? TI2 O1 TI3 100.1(1) . . . ? TI2 O1 TI4 149.9(1) . . . ? TI3 O1 TI4 102.5(1) . . . ? TI1 O2 TI4 103.8(1) . . . ? TI1 O2 TI5 105.7(1) . . . ? TI4 O2 TI5 104.8(1) . . . ? TI1 O3 TI5 96.1(1) . . . ? TI1 O3 TI6 103.3(1) . . . ? TI1 O3 TI7 97.7(1) . . . ? TI5 O3 TI6 100.5(1) . . . ? TI5 O3 TI7 150.2(1) . . . ? TI6 O3 TI7 101.9(1) . . . ? TI1 O4 TI2 105.4(1) . . . ? TI1 O4 TI7 103.7(1) . . . ? TI2 O4 TI7 104.6(1) . . . ? TI1 O5 TI6 101.9(1) . . . ? TI1 O5 C1 131.7(3) . . . ? TI6 O5 C1 126.2(3) . . . ? O5 C1 C2 112.2(4) . . . ? C1 C2 C3 115.2(4) . . . ? C2 C3 O6 112.0(4) . . . ? TI1 O6 TI3 102.0(1) . . . ? TI1 O6 C3 129.2(3) . . . ? TI3 O6 C3 128.7(3) . . . ? TI2 O7 TI7 103.8(1) . . . ? TI2 O7 C4 127.0(3) . . . ? TI7 O7 C4 127.0(3) . . . ? O7 C4 C5 110.9(4) . . . ? TI2 O8 C6 132.3(3) . . . ? O8 C6 C7 115.2(5) . . . ? TI2 O9 C8 160.4(3) . . . ? O9 C8 C9 112.7(5) . . . ? TI2 O10 TI3 105.3(1) . . . ? TI2 O10 C10 122.1(3) . . . ? TI3 O10 C10 123.4(3) . . . ? O10 C10 C11 112.1(6) . . . ? TI3 O11 C12 143.0(5) . . . ? O11 C12 C13 122(1) . . . ? TI3 O12 C14 138.1(4) . . . ? O12 C14 C15 114.6(8) . . . ? TI3 O13 TI4 105.7(1) . . . ? TI3 O13 C16 124.0(3) . . . ? TI4 O13 C16 127.7(3) . . . ? O13 C16 C17 110.9(4) . . . ? TI4 O14 C18 134.2(3) . . . ? O14 C18 C19 113.4(6) . . . ? TI4 O15 C20 145.4(4) . . . ? O15 C20 C21 109.7(6) . . . ? TI4 O16 TI5 103.8(1) . . . ? TI4 O16 C22 126.9(3) . . . ? TI5 O16 C22 126.7(3) . . . ? O16 C22 C23 111.4(4) . . . ? TI5 O17 C24 134.2(4) . . . ? O17 C24 C25 112.8(5) . . . ? TI5 O18 C26 156.2(3) . . . ? O18 C26 C27 112.5(5) . . . ? TI5 O19 TI6 106.3(1) . . . ? TI5 O19 C28 122.2(4) . . . ? TI6 O19 C28 124.8(3) . . . ? O19 C28 C29 114(1) . . . ? TI6 O20 C30 141.6(4) . . . ? O20 C30 C31 114.6(7) . . . ? TI6 O21 TI7 105.4(1) . . . ? TI6 O21 C32 123.4(3) . . . ? TI7 O21 C32 125.6(3) . . . ? O21 C32 C33 111.6(6) . . . ? TI6 O22 C34 137.1(2) . . . ? O22 C34 C35 111.6(1) . . . ? TI7 O23 C36 140.0(3) . . . ? O23 C36 C37 111.2(6) . . . ? TI7 O24 C38 135.4(3) . . . ? O24 C38 C39 112.9(6) . . . ? data_st181 #========================================================================= _database_code_depnum_ccdc_archive 'CCDC 168598' # 5. CHEMICAL DATA _chemical_name_systematic ; (µ4-2,2-bis(hydroxymethyl)-1,3-propanediolato(O,O',O'',O'''))- tetrakis(µ2-ethoxo)-octakis(ethoxy)-tetra-titanium ; _chemical_name_common 'tentacular tetratitanate' _chemical_formula_moiety 'C29 H68 O16 Ti4' _chemical_formula_structural '[Ti4(µ4-(OCH2)4C)(µ2-OC2H5)4(OC2H5)8]' _chemical_formula_analytical ? _chemical_formula_sum 'C29 H68 O16 Ti4' _chemical_formula_weight 864.46 _chemical_melting_point ? _chemical_compound_source 'Synthetic' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 Ti ? 0.248 0.446 International_Tables_Vol_IV_Table_2.3.1 #======================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,-y,-z _cell_length_a 9.5168(3) _cell_length_b 13.4861(7) _cell_length_c 17.8842(9) _cell_angle_alpha 99.008(9) _cell_angle_beta 90.923(9) _cell_angle_gamma 105.676(9) _cell_volume 2178.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 18477 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 28.3 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.32 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 916 _exptl_absorpt_coefficient_mu 0.756 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #======================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 180 frames, 30 sec/frame, delta phi = 1.0 deg. Each frame measured 2 times. Detector to crystal distance 25 mm. ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18477 _diffrn_reflns_av_R_equivalents 0.091 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 28.26 _reflns_number_total 9422 _reflns_number_gt 5655 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #========================================================================= # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^) + 0.0064 Fo^4^)' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5655 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_abs_structure_details ; ? ; _refine_ls_R_factor_all 0.103 _refine_ls_R_factor_gt 0.053 _refine_ls_wR_factor_all 0.119 _refine_ls_wR_factor_ref 0.080 _refine_ls_goodness_of_fit_all 2.265 _refine_ls_goodness_of_fit_ref 1.518 _refine_ls_shift/su_max 0.006 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.641 _refine_diff_density_min -0.129 #======================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol TI1 0.39264(7) 0.66559(5) 0.33277(4) 0.0425(4) Uani ? ? Ti TI2 0.26018(7) 0.17030(5) 0.28303(4) 0.0466(4) Uani ? ? Ti TI3 0.13402(7) 0.29097(5) 0.16300(4) 0.0380(3) Uani ? ? Ti TI4 0.08163(6) 0.50378(5) 0.25685(4) 0.0351(3) Uani ? ? Ti O1 0.3561(3) 0.7395(3) 0.4183(2) 0.068(2) Uani ? ? O C1 0.4294(5) 0.8242(4) 0.4737(3) 0.068(3) Uani ? ? C C2 0.3329(7) 0.8412(5) 0.5360(3) 0.096(4) Uani ? ? C O2 0.5075(3) 0.7591(2) 0.2816(2) 0.066(2) Uani ? ? O C3 0.6591(5) 0.7912(4) 0.2685(3) 0.075(3) Uani ? ? C C4 0.7396(6) 0.8787(5) 0.3266(4) 0.094(4) Uani ? ? C O3 0.5419(3) 0.6144(2) 0.3570(2) 0.058(2) Uani ? ? O C5 0.5682(4) 0.5237(3) 0.3736(2) 0.045(2) Uani ? ? C C6 0.4394(4) 0.4256(3) 0.3511(2) 0.038(2) Uani ? ? C C7 0.2967(4) 0.4505(3) 0.3747(2) 0.038(2) Uani ? ? C O4 0.2606(2) 0.5218(2) 0.3317(1) 0.037(1) Uani ? ? O C8 0.4309(4) 0.3883(3) 0.2658(2) 0.040(2) Uani ? ? C O5 0.3053(2) 0.3028(2) 0.2413(1) 0.037(1) Uani ? ? O C9 0.4683(4) 0.3421(3) 0.3937(2) 0.047(2) Uani ? ? C O6 0.3964(3) 0.2399(2) 0.3589(2) 0.051(1) Uani ? ? O O7 0.1214(4) 0.1186(3) 0.3457(2) 0.087(2) Uani ? ? O C10 0.1231(6) 0.1175(4) 0.4275(3) 0.087(3) Uani ? ? C C11 0.1648(7) 0.0259(5) 0.4389(4) 0.094(4) Uani ? ? C O8 0.3378(3) 0.0724(2) 0.2389(2) 0.091(2) Uani ? ? O C12 0.4506(5) 0.0233(4) 0.2443(4) 0.071(3) Uani ? ? C C13 0.5031(7) -0.0024(5) 0.1691(5) 0.122(4) Uani ? ? C O9 0.0993(3) 0.1574(2) 0.2045(2) 0.043(1) Uani ? ? O C14 -0.0202(5) 0.0635(3) 0.1828(3) 0.057(2) Uani ? ? C C15 0.0200(6) -0.0075(4) 0.1199(4) 0.080(3) Uani ? ? C O10 -0.0334(3) 0.2530(2) 0.1053(2) 0.049(1) Uani ? ? O C16 -0.0924(6) 0.2192(5) 0.0313(3) 0.084(3) Uani ? ? C C17 -0.1796(8) 0.2800(8) 0.0069(4) 0.147(5) Uani ? ? C O11 0.2445(3) 0.2642(2) 0.0858(2) 0.051(1) Uani ? ? O C18 0.3818(6) 0.2465(5) 0.0695(3) 0.083(3) Uani ? ? C C19 0.3787(7) 0.1753(7) 0.0022(4) 0.148(5) Uani ? ? C O12 0.0329(2) 0.3522(2) 0.2562(1) 0.035(1) Uani ? ? O C20 -0.0797(4) 0.2941(3) 0.2976(2) 0.049(2) Uani ? ? C C21 -0.2271(5) 0.2823(4) 0.2639(3) 0.063(3) Uani ? ? C O13 0.1953(2) 0.4441(2) 0.1693(1) 0.038(1) Uani ? ? O C22 0.2271(4) 0.4906(3) 0.1027(2) 0.049(2) Uani ? ? C C23 0.3875(5) 0.5454(4) 0.1023(3) 0.069(3) Uani ? ? C O14 -0.0278(3) 0.5310(2) 0.3349(1) 0.043(1) Uani ? ? O C24 -0.0276(4) 0.5504(4) 0.4146(2) 0.056(2) Uani ? ? C C25 -0.0459(5) 0.6548(4) 0.4431(3) 0.063(3) Uani ? ? C O15 -0.0454(3) 0.5185(2) 0.1864(1) 0.045(1) Uani ? ? O C26 -0.1830(4) 0.5376(4) 0.1787(3) 0.062(2) Uani ? ? C C27 -0.1884(6) 0.6043(5) 0.1225(3) 0.096(3) Uani ? ? C O16 0.2222(3) 0.6462(2) 0.2588(2) 0.044(1) Uani ? ? O C28 0.1966(4) 0.7280(3) 0.2220(3) 0.055(2) Uani ? ? C C29 0.1232(6) 0.7958(4) 0.2722(3) 0.082(3) Uani ? ? C H1 0.4581 0.8853 0.4512 0.0932 Uiso calc C1 H H2 0.5137 0.8102 0.4939 0.0932 Uiso calc C1 H H3 0.3843 0.8988 0.5730 0.1291 Uiso calc C2 H H4 0.2486 0.8554 0.5161 0.1291 Uiso calc C2 H H5 0.3042 0.7803 0.5588 0.1291 Uiso calc C2 H H6 0.6697 0.8124 0.2202 0.0988 Uiso calc C3 H H7 0.6989 0.7339 0.2692 0.0988 Uiso calc C3 H H8 0.8400 0.8980 0.3162 0.1313 Uiso calc C4 H H9 0.7008 0.9365 0.3261 0.1313 Uiso calc C4 H H10 0.7300 0.8580 0.3751 0.1313 Uiso calc C4 H H11 0.5900 0.5328 0.4266 0.0602 Uiso calc C5 H H12 0.6503 0.5131 0.3473 0.0602 Uiso calc C5 H H13 0.3077 0.4806 0.4269 0.0502 Uiso calc C7 H H14 0.2197 0.3875 0.3670 0.0502 Uiso calc C7 H H15 0.5160 0.3670 0.2529 0.0526 Uiso calc C8 H H16 0.4269 0.4445 0.2405 0.0526 Uiso calc C8 H H17 0.4361 0.3531 0.4436 0.0614 Uiso calc C9 H H18 0.5705 0.3496 0.3964 0.0614 Uiso calc C9 H H19 0.0288 0.1143 0.4453 0.1101 Uiso calc C10 H H20 0.1919 0.1784 0.4537 0.1101 Uiso calc C10 H H21 0.1673 0.0222 0.4915 0.1223 Uiso calc C11 H H22 0.0958 -0.0345 0.4122 0.1223 Uiso calc C11 H H23 0.2589 0.0296 0.4206 0.1223 Uiso calc C11 H H24 0.4140 -0.0391 0.2647 0.1018 Uiso calc C12 H H25 0.5292 0.0691 0.2767 0.1018 Uiso calc C12 H H26 0.5787 -0.0353 0.1733 0.1552 Uiso calc C13 H H27 0.4246 -0.0483 0.1365 0.1552 Uiso calc C13 H H28 0.5398 0.0599 0.1486 0.1552 Uiso calc C13 H H29 -0.1039 0.0819 0.1667 0.0787 Uiso calc C14 H H30 -0.0417 0.0287 0.2252 0.0787 Uiso calc C14 H H31 -0.0593 -0.0687 0.1064 0.1137 Uiso calc C15 H H32 0.0413 0.0269 0.0773 0.1137 Uiso calc C15 H H33 0.1036 -0.0263 0.1358 0.1137 Uiso calc C15 H H34 -0.1516 0.1492 0.0273 0.1209 Uiso calc C16 H H35 -0.0143 0.2213 -0.0014 0.1209 Uiso calc C16 H H36 -0.2161 0.2524 -0.0440 0.2073 Uiso calc C17 H H37 -0.2591 0.2781 0.0386 0.2073 Uiso calc C17 H H38 -0.1219 0.3501 0.0098 0.2073 Uiso calc C17 H H39 0.4145 0.2198 0.1106 0.1096 Uiso calc C18 H H40 0.4489 0.3114 0.0649 0.1096 Uiso calc C18 H H41 0.4739 0.1672 -0.0051 0.2169 Uiso calc C19 H H42 0.3129 0.1096 0.0061 0.2169 Uiso calc C19 H H43 0.3473 0.2012 -0.0396 0.2169 Uiso calc C19 H H44 -0.0719 0.3298 0.3484 0.0624 Uiso calc C20 H H45 -0.0665 0.2267 0.2975 0.0624 Uiso calc C20 H H46 -0.2985 0.2437 0.2927 0.0855 Uiso calc C21 H H47 -0.2416 0.3493 0.2641 0.0855 Uiso calc C21 H H48 -0.2362 0.2463 0.2132 0.0855 Uiso calc C21 H H49 0.1726 0.5399 0.1011 0.0649 Uiso calc C22 H H50 0.1997 0.4375 0.0592 0.0649 Uiso calc C22 H H51 0.4055 0.5754 0.0576 0.0907 Uiso calc C23 H H52 0.4156 0.5988 0.1455 0.0907 Uiso calc C23 H H53 0.4426 0.4965 0.1036 0.0907 Uiso calc C23 H H54 0.0627 0.5461 0.4354 0.0754 Uiso calc C24 H H55 -0.1056 0.4989 0.4304 0.0754 Uiso calc C24 H H56 -0.0452 0.6651 0.4969 0.0896 Uiso calc C25 H H57 0.0320 0.7068 0.4278 0.0896 Uiso calc C25 H H58 -0.1363 0.6596 0.4229 0.0896 Uiso calc C25 H H59 -0.2043 0.5707 0.2263 0.0781 Uiso calc C26 H H60 -0.2548 0.4727 0.1638 0.0781 Uiso calc C26 H H61 -0.2830 0.6147 0.1195 0.1195 Uiso calc C27 H H62 -0.1176 0.6698 0.1369 0.1195 Uiso calc C27 H H63 -0.1680 0.5717 0.0744 0.1195 Uiso calc C27 H H64 0.1361 0.6973 0.1770 0.0712 Uiso calc C28 H H65 0.2877 0.7698 0.2093 0.0712 Uiso calc C28 H H66 0.1079 0.8488 0.2463 0.1032 Uiso calc C29 H H67 0.0318 0.7545 0.2848 0.1032 Uiso calc C29 H H68 0.1833 0.8271 0.3172 0.1032 Uiso calc C29 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol TI1 0.0407(3) 0.0391(3) 0.0483(4) 0.0088(3) -0.0038(3) -0.0008(3) Ti TI2 0.0494(3) 0.0415(3) 0.0493(4) 0.0186(2) -0.0025(3) 0.0054(3) Ti TI3 0.0385(3) 0.0464(3) 0.0307(3) 0.0149(2) -0.0004(3) -0.0012(3) Ti TI4 0.0349(3) 0.0400(3) 0.0310(3) 0.0120(2) 0.0003(2) 0.0027(3) Ti O1 0.062(2) 0.077(2) 0.065(2) 0.013(1) -0.007(2) -0.031(2) O C1 0.076(3) 0.070(3) 0.060(3) 0.018(2) -0.012(2) -0.011(3) C C2 0.133(4) 0.114(4) 0.059(3) 0.066(3) -0.014(3) -0.016(3) C O2 0.039(1) 0.068(2) 0.107(2) 0.009(1) 0.004(1) 0.037(2) O C3 0.065(3) 0.073(3) 0.087(4) 0.010(2) 0.012(3) 0.024(3) C C4 0.064(3) 0.107(5) 0.122(5) 0.005(3) 0.005(3) 0.020(4) C O3 0.045(1) 0.046(2) 0.093(2) 0.002(1) -0.023(1) 0.014(1) O C5 0.036(2) 0.056(2) 0.046(2) 0.013(1) -0.006(2) 0.005(2) C C6 0.035(2) 0.046(2) 0.034(2) 0.012(1) -0.003(1) 0.001(2) C C7 0.039(2) 0.046(2) 0.031(2) 0.013(1) -0.000(1) 0.004(2) C O4 0.036(1) 0.040(1) 0.035(1) 0.0128(9) -0.003(1) 0.004(1) O C8 0.033(2) 0.051(2) 0.040(2) 0.015(1) 0.002(1) 0.007(2) C O5 0.036(1) 0.042(1) 0.034(1) 0.0124(9) 0.001(1) 0.002(1) O C9 0.049(2) 0.052(2) 0.041(2) 0.016(2) -0.004(2) 0.006(2) C O6 0.063(1) 0.046(1) 0.047(2) 0.017(1) -0.011(1) 0.008(1) O O7 0.065(2) 0.125(3) 0.080(2) -0.003(2) -0.006(2) 0.062(2) O C10 0.087(3) 0.081(3) 0.093(4) 0.020(3) 0.015(3) 0.037(3) C C11 0.096(4) 0.089(4) 0.096(4) 0.032(3) 0.007(3) 0.004(3) C O8 0.095(2) 0.084(2) 0.095(3) 0.063(1) -0.026(2) -0.024(2) O C12 0.054(2) 0.051(2) 0.130(5) 0.022(2) 0.000(3) 0.001(3) C C13 0.106(4) 0.129(4) 0.133(6) 0.065(3) 0.016(4) -0.006(4) C O9 0.045(1) 0.040(1) 0.044(1) 0.010(1) -0.002(1) -0.002(1) O C14 0.064(2) 0.043(2) 0.066(3) 0.003(2) -0.010(2) 0.005(2) C C15 0.094(3) 0.055(3) 0.098(4) 0.014(3) -0.027(3) -0.019(3) C O10 0.049(1) 0.058(2) 0.041(1) 0.016(1) -0.010(1) -0.005(1) O C16 0.101(3) 0.115(4) 0.051(3) 0.031(3) -0.031(3) -0.020(3) C C17 0.122(4) 0.282(8) 0.092(4) 0.078(4) -0.033(3) 0.050(5) C O11 0.055(1) 0.064(2) 0.037(1) 0.025(1) 0.007(1) -0.003(1) O C18 0.083(3) 0.107(4) 0.065(3) 0.043(2) 0.017(2) -0.010(3) C C19 0.101(4) 0.221(6) 0.146(5) 0.062(3) 0.018(3) -0.100(4) C O12 0.032(1) 0.041(1) 0.033(1) 0.0092(9) 0.0025(9) 0.003(1) O C20 0.050(2) 0.052(2) 0.044(2) 0.017(2) 0.014(2) 0.008(2) C C21 0.042(2) 0.073(3) 0.080(3) 0.010(2) 0.014(2) 0.016(3) C O13 0.039(1) 0.047(1) 0.029(1) 0.0134(9) 0.003(1) 0.007(1) O C22 0.057(2) 0.060(2) 0.035(2) 0.017(2) 0.009(2) 0.011(2) C C23 0.071(3) 0.076(3) 0.060(3) 0.008(2) 0.024(2) 0.023(2) C O14 0.045(1) 0.049(1) 0.035(1) 0.0185(9) 0.003(1) 0.002(1) O C24 0.055(2) 0.086(3) 0.037(2) 0.032(2) 0.003(2) -0.000(2) C C25 0.059(2) 0.077(3) 0.055(3) 0.010(2) 0.006(2) -0.020(2) C O15 0.042(1) 0.055(1) 0.040(1) 0.0205(9) 0.000(1) 0.008(1) O C26 0.052(2) 0.079(3) 0.059(3) 0.028(2) 0.001(2) 0.022(2) C C27 0.075(3) 0.139(4) 0.085(3) 0.052(2) -0.001(2) 0.049(3) C O16 0.049(1) 0.039(1) 0.045(1) 0.010(1) -0.003(1) 0.008(1) O C28 0.055(2) 0.048(2) 0.062(3) 0.012(2) -0.000(2) 0.016(2) C C29 0.097(3) 0.062(2) 0.091(4) 0.041(2) 0.006(3) 0.017(3) C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag TI1 O1 1.783(3) . . ? TI1 O2 1.809(3) . . ? TI1 O3 1.813(3) . . ? TI2 O5 1.986(3) . . ? TI2 O6 1.813(3) . . ? TI2 O7 1.811(4) . . ? TI2 O8 1.770(3) . . ? TI3 O10 1.790(3) . . ? TI3 O11 1.799(3) . . ? TI3 O13 1.973(3) . . ? TI4 O12 1.969(3) . . ? TI4 O14 1.806(3) . . ? TI4 O15 1.802(3) . . ? O1 C1 1.403(6) . . ? C1 C2 1.484(8) . . ? O2 C3 1.424(6) . . ? C3 C4 1.470(9) . . ? O3 C5 1.387(5) . . ? C5 C6 1.535(6) . . ? C6 C7 1.535(5) . . ? C6 C8 1.524(5) . . ? C6 C9 1.534(6) . . ? C7 O4 1.427(5) . . ? C8 O5 1.425(5) . . ? C9 O6 1.401(5) . . ? O7 C10 1.466(7) . . ? C10 C11 1.436(9) . . ? O8 C12 1.415(6) . . ? C12 C13 1.47(1) . . ? O9 C14 1.450(5) . . ? C14 C15 1.484(8) . . ? O10 C16 1.388(6) . . ? C16 C17 1.42(1) . . ? O11 C18 1.417(6) . . ? C18 C19 1.412(9) . . ? O12 C20 1.437(5) . . ? C20 C21 1.476(6) . . ? O13 C22 1.431(5) . . ? C22 C23 1.506(7) . . ? O14 C24 1.409(5) . . ? C24 C25 1.478(7) . . ? O15 C26 1.410(5) . . ? C26 C27 1.458(8) . . ? O16 C28 1.441(5) . . ? C28 C29 1.496(7) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 TI1 O2 106.0(2) . . . ? O1 TI1 O3 106.2(2) . . . ? O2 TI1 O3 92.9(1) . . . ? O5 TI2 O6 86.4(1) . . . ? O5 TI2 O7 130.7(2) . . . ? O5 TI2 O8 116.7(2) . . . ? O6 TI2 O7 94.9(2) . . . ? O6 TI2 O8 102.3(2) . . . ? O7 TI2 O8 111.1(2) . . . ? O10 TI3 O11 94.7(1) . . . ? O10 TI3 O13 102.8(1) . . . ? O11 TI3 O13 95.7(1) . . . ? O12 TI4 O14 95.7(1) . . . ? O12 TI4 O15 104.5(1) . . . ? O14 TI4 O15 93.8(1) . . . ? TI1 O1 C1 139.2(3) . . . ? O1 C1 C2 110.6(5) . . . ? TI1 O2 C3 135.9(3) . . . ? O2 C3 C4 111.8(5) . . . ? TI1 O3 C5 140.9(3) . . . ? O3 C5 C6 114.1(3) . . . ? C5 C6 C7 109.4(3) . . . ? C5 C6 C8 110.1(3) . . . ? C5 C6 C9 106.7(3) . . . ? C7 C6 C8 110.0(3) . . . ? C7 C6 C9 110.4(3) . . . ? C8 C6 C9 110.2(3) . . . ? C6 C7 O4 111.8(3) . . . ? C6 C8 O5 112.0(3) . . . ? TI2 O5 C8 123.5(2) . . . ? C6 C9 O6 113.2(3) . . . ? TI2 O6 C9 140.4(3) . . . ? TI2 O7 C10 133.3(3) . . . ? O7 C10 C11 106.7(6) . . . ? TI2 O8 C12 145.3(4) . . . ? O8 C12 C13 110.1(6) . . . ? O9 C14 C15 110.5(4) . . . ? TI3 O10 C16 143.5(4) . . . ? O10 C16 C17 114.3(6) . . . ? TI3 O11 C18 142.5(3) . . . ? O11 C18 C19 114.1(6) . . . ? TI4 O12 C20 125.4(2) . . . ? O12 C20 C21 111.9(4) . . . ? TI3 O13 C22 121.0(3) . . . ? O13 C22 C23 111.2(4) . . . ? TI4 O14 C24 143.4(3) . . . ? O14 C24 C25 111.8(4) . . . ? TI4 O15 C26 141.5(3) . . . ? O15 C26 C27 112.8(4) . . . ? O16 C28 C29 111.5(4) . . . ? data_SOFTOW _audit_creation_date 2001-07-02 #_audit_creation_date 2001-06-29 _audit_creation_method 'Created by WinPacha v3.5' _audit_update_record ; This file contains both experimental data and outputs from a crystal structure optimization package designed to remove disorder and/or add missing hydrogen atoms to an existing experimental structural data file. Atoms whose coordinates must be added or changed are introduced using a Z-matrix. Important torsional angles are further optimized following a downhill simplex prodecure in order to minimize the quantity (EB + RB) where EB stands for the attractive long range Madelung energy of the crystal [1], and RB the sum of all short range repulsive interactions. Attractive term EB is evaluated from a point charge approximation of DFT equations [1] using configuration energies [2,3] and ab initio atomic orbital radii of the elements [4]. Repulsive RB term is evaluated from ab initio atom-atom potentials derived from the Gordon-Kim electron gas model [5] given the full content of 8 unit-cells. Computed structures are identified by a _database_code field followed by the compound identification and the full reference of publication. The atom_site_calc_flag should be either 'd', 'c' or 'o'. 'd' means that original position was not modified 'c' means that position have been computed (or recomputed) using fixed bond length, bond angle and torsion angle. 'o' means that position have been computed (or recomputed) using fixed bond length and bond angle with a variable torsion angle. References: [1] Henry, M., Coordin. Chem. Revs., 1998, 178, 1109-1163. [2] Mann, J.B.; Meek, T.L.; Allen, L.C., J. Am. Chem. Soc., 2000, 122, 2780-2783. [3] Mann, J.B.; Meek, T.L.; Knight, E.T.; Capitani, J.F.; Allen, L.C., J. Am. Chem. Soc., 2000, 122, 5132-5137. [4] Waber, J.T.; Cromer, D.T., J. Chem. Phys., 1965, 42, 4116-4123. [5] Spackman, M.A., J. Chem. Phys., 1986, 85, 6579-6586. ; _database_code_csd 'SOFTOW' _chemical_name_systematic ; bis(mu!4$-Oxo)-bis(mu!3$-oxo)-octakis(mu!2$-ethoxo)-dodecakis(ethoxy)- hepta-titanium ; _chemical_compound_source 'Synthetic' _chemical_formula_structural '[Ti7(µ4-O)2(µ3-O)2(µ2-OEt)8(OEt)12]' _chemical_formula_sum 'H200 C80 O48 Ti14 ' _publ_section_title ; New compounds in the chemistry of group 4 transition-metal alkoxides. Part 4. Synthesis and molecular structures of two polymorphs of [Ti16O16(OEt)32] and refinement of the structure of [Ti7O4(OEt)20]. ; loop_ _publ_author_name 'R. Schmid' 'A. Mosset' 'J. Galy' _journal_name_full ; J.Chem.Soc.,Dalton Trans. ; _journal_volume ? _journal_year '1991' _journal_page_first '1999' _journal_page_last '2005' _cell_length_a 13.91000 _cell_length_b 20.21200 _cell_length_c 12.16200 _cell_angle_alpha 90.49000 _cell_angle_beta 108.20000 _cell_angle_gamma 74.65000 _symmetry_space_group_name_H-M 'P -1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_calc_flag Ti1 0.70189 0.29430 0.20470 d Ti2 0.81330 0.29430 0.46880 d Ti3 0.91080 0.18680 0.22300 d Ti4 0.59470 0.25901 0.37440 d Ti5 0.69490 0.14845 0.13380 d Ti6 0.48020 0.26433 0.10270 d Ti7 0.91560 0.33798 0.28750 d O1 0.76050 0.36340 0.16270 d O2 0.83460 0.12390 0.26170 d O3 0.95500 0.26940 0.18070 d O4 0.92780 0.41570 0.23180 d O5 1.03220 0.14480 0.33480 d O6 1.04660 0.31120 0.39010 d O7 0.85400 0.37330 0.40840 d O8 0.94010 0.24570 0.55930 d O9 0.77590 0.34530 0.57850 d O10 0.74510 0.21970 0.47560 d O11 0.85260 0.26240 0.31600 d O12 0.75800 0.22390 0.12200 d O13 0.62400 0.22570 0.22430 d O14 0.73140 0.09900 0.02110 d O15 0.56270 0.33890 0.10120 d O16 0.64640 0.08760 0.18720 d O17 0.55960 0.20550 0.01260 d O18 0.37290 0.31440 -0.01490 d O19 0.41780 0.19890 0.12250 d O20 0.45750 0.30600 0.24420 d O21 0.94740 0.14450 0.10620 d O22 0.67590 0.32240 0.34390 d O23 0.54800 0.31240 0.47580 d O24 0.55600 0.18520 0.40860 d C1 0.73530 0.40150 0.05560 o C2 0.70600 0.36630 -0.04400 c C3 0.87820 0.06530 0.34060 o C4 0.91900 0.00320 0.28400 o C5 1.04630 0.26230 0.14620 d C6 1.02440 0.30730 0.04240 d C7 0.98000 0.46060 0.23800 d C8 0.97800 0.49790 0.14600 d C9 1.13200 0.10450 0.34000 d C10 1.19401 0.07889 0.45998 o C11 1.11240 0.33160 0.48500 d C12 1.22230 0.29550 0.50700 d C13 0.79620 0.44195 0.40958 c C14 0.85805 0.47582 0.50026 o C15 1.03420 0.19430 0.58850 d C16 1.09740 0.19330 0.71200 d C17 0.82270 0.35470 0.69670 d C18 0.78600 0.42440 0.72400 d C19 0.78150 0.16290 0.55920 d C20 0.76200 0.18210 0.66920 d C21 0.71660 0.03770 -0.02440 d C22 0.71990 0.03280 -0.14340 d C23 0.50580 0.41100 0.07910 d C24 0.52790 0.45340 0.18230 d C25 0.60890 0.05560 0.25870 d C26 0.60300 -0.01320 0.22500 d C27 0.55300 0.22180 -0.10570 d C28 0.48700 0.19770 -0.18900 d C29 0.28832 0.34873 -0.11269 c C30 0.32562 0.38668 -0.18474 o C31 0.36300 0.15920 0.05000 d C32 0.26564 0.16263 0.07461 o C33 0.35780 0.32190 0.26360 d C34 0.29050 0.38800 0.20500 d C35 0.91760 0.15080 -0.01620 d C36 0.99310 0.10490 -0.05960 d C37 0.52200 0.38080 0.50200 d C38 0.49400 0.38780 0.60200 d C39 0.49620 0.16920 0.47100 d C40 0.51118 0.09492 0.47949 o H72 0.79924 0.42161 0.05505 c H73 0.66848 0.44279 0.05586 c H74 0.82033 0.05702 0.37606 c H75 0.94260 0.07406 0.40971 c H76 0.07723 0.20969 0.13136 c H77 0.10382 0.27812 0.21473 c H78 0.05970 0.43972 0.29337 c H79 0.93895 0.50060 0.27878 c H80 0.12538 0.06243 0.28638 c H81 0.17087 0.13559 0.30821 c H82 0.09013 0.32516 0.56027 c H83 0.10205 0.38550 0.46830 c H84 0.77610 0.46931 0.32672 c H85 0.72549 0.44217 0.42789 c H86 0.07867 0.20092 0.53352 c H87 0.01578 0.14600 0.57382 c H88 0.90682 0.34017 0.71851 c H89 0.80522 0.32056 0.75005 c H90 0.86393 0.13955 0.57512 c H91 0.73769 0.12693 0.52366 c H92 0.77409 0.99470 0.03072 c H93 0.63903 0.03632 0.97171 c H94 0.51972 0.43327 0.00773 c H95 0.42431 0.41228 0.05660 c H96 0.53285 0.08661 0.25748 c H97 0.66396 0.05131 0.34456 c H98 0.63005 0.20673 0.88549 c H99 0.52155 0.27669 0.87996 c H100 0.24944 0.31272 0.84091 c H101 0.23285 0.38700 0.91516 c H102 0.41088 0.10697 0.06050 c H103 0.34288 0.17884 0.96164 c H104 0.36904 0.32206 0.35498 c H105 0.32080 0.28256 0.22877 c H106 0.84166 0.14199 0.94678 c H107 0.91422 0.20224 0.95809 c H108 0.45924 0.41140 0.43040 c H109 0.58923 0.40009 0.51491 c H110 0.52009 0.18539 0.55723 c H111 0.41527 0.19630 0.42802 c H112 0.77631 0.33325 -0.05915 o H113 0.66080 0.40398 -0.11864 c H114 0.65617 0.33504 -0.03159 c H115 0.86291 -0.02789 0.26288 o H116 0.99493 -0.02709 0.34344 c H117 0.93061 0.01975 0.20463 c H118 1.00285 0.27979 -0.03563 o H119 1.09481 0.32357 0.04791 c H120 0.95972 0.35292 0.03931 c H121 1.04614 0.47388 0.11826 o H122 0.97951 0.55005 0.17030 c H123 0.90494 0.50083 0.07511 c H124 1.22222 0.11997 0.50763 o H125 1.26098 0.03556 0.46024 c H126 1.14466 0.06085 0.50092 c H127 1.25645 0.27025 0.59528 o H128 1.26446 0.33253 0.49649 c H129 1.22826 0.25706 0.44357 c H130 0.81091 0.50132 0.55377 o H131 0.88258 0.51376 0.45947 c H132 0.92834 0.43713 0.55423 c H133 1.09939 0.24568 0.73429 o H134 1.17752 0.16062 0.72593 c H135 1.06198 0.17149 0.76655 c H136 0.82720 0.45706 0.69639 o H137 0.80072 0.42494 0.81790 c H138 0.70107 0.44341 0.67921 c H139 0.82196 0.20581 0.72111 o H140 0.76439 0.13575 0.71727 c H141 0.68360 0.21839 0.64960 c H142 0.66971 0.08021 -0.19685 o H143 0.69236 -0.01132 -0.17914 c H144 0.80142 0.02461 -0.14191 c H145 0.48762 0.44325 0.24202 o H146 0.50009 0.50806 0.15144 c H147 0.61306 0.43990 0.22671 c H148 0.55858 -0.01074 0.13246 o H149 0.56410 -0.03363 0.27708 c H150 0.68305 -0.04686 0.24261 c H151 0.50107 0.14240 -0.16999 o H152 0.49885 0.20703 -0.27184 c H153 0.40609 0.22516 -0.19461 c H154 0.32880 0.43690 -0.15151 o H155 0.27181 0.39364 -0.27416 c H156 0.40419 0.35668 -0.18350 c H157 0.28004 0.16114 0.16857 o H158 0.23688 0.11886 0.03922 c H159 0.20655 0.21050 0.03208 c H160 0.24366 0.41459 0.25806 o H161 0.23843 0.37957 0.12081 c H162 0.33981 0.41906 0.19050 c H163 1.06191 0.12443 -0.04655 o H164 0.95617 0.10085 -0.15233 c H165 1.01702 0.05389 -0.01337 c H166 0.42074 0.37343 0.58853 o H167 0.48347 0.44141 0.62381 c H168 0.55752 0.35448 0.67321 c H169 0.47135 0.07861 0.39527 o H170 0.47879 0.08197 0.54520 c H171 0.59569 0.06885 0.50657 c data_ZELDEZ _audit_creation_date 2001-06-29 _audit_creation_method 'Created by WinPacha v3.5' _audit_update_record ; This file contains both experimental data and outputs from a crystal structure optimization package designed to remove disorder and/or add missing hydrogen atoms to an existing experimental structural data file. Atoms whose coordinates must be added or changed are introduced using a Z-matrix. Important torsional angles are further optimized following a downhill simplex prodecure in order to minimize the quantity (EB + RB) where EB stands for the attractive long range Madelung energy of the crystal [1], and RB the sum of all short range repulsive interactions. Attractive term EB is evaluated from a point charge approximation of DFT equations [1] using configuration energies [2,3] and ab initio atomic orbital radii of the elements [4]. Repulsive RB term is evaluated from ab initio atom-atom potentials derived from the Gordon-Kim electron gas model [5] given the full content of 8 unit-cells. Computed structures are identified by a _database_code field followed by the compound identification and the full reference of publication. The atom_site_calc_flag should be either 'd', 'c' or 'o'. 'd' means that original position was not modified 'c' means that position have been computed (or recomputed) using fixed bond length, bond angle and torsion angle. 'o' means that position have been computed (or recomputed) using fixed bond length and bond angle with a variable torsion angle. References: [1] Henry, M., Coordin. Chem. Revs., 1998, 178, 1109-1163. [2] Mann, J.B.; Meek, T.L.; Allen, L.C., J. Am. Chem. Soc., 2000, 122, 2780-2783. [3] Mann, J.B.; Meek, T.L.; Knight, E.T.; Capitani, J.F.; Allen, L.C., J. Am. Chem. Soc., 2000, 122, 5132-5137. [4] Waber, J.T.; Cromer, D.T., J. Chem. Phys., 1965, 42, 4116-4123. [5] Spackman, M.A., J. Chem. Phys., 1986, 85, 6579-6586. ; _database_code_csd 'ZELDEZ' _chemical_name_systematic ; (µ2-Ethanediolato)-(µ4-ethanediolato)-tris(µ3-ethanediolato)-(µ2-iso propoxo)-nonakis(isopropoxy)-penta-titanium ; _chemical_compound_source 'Synthetic' _chemical_formula_structural '[Ti5(OPri)9(µ-O2C2H4)3(µ3-O2C2H4)]' _chemical_formula_sum 'H180 C80 O40 Ti10 ' _publ_section_title ; Metal-assisted activation of the C-O bond of 2-hydroxyethylmethacryslate. Synthesis and molecular structure of [Ti5(OPri)9(µ-O2C2H4)3(µ3-O2C2H4)]. ; loop_ _publ_author_name 'N.Pajot' 'R.Papiernik' 'L.G.Hubert-Pfalzgraf' 'J.Vaissermann' 'S.Parraud' _journal_name_full ; Journal of Chemical Society, Chemical Communications ; _journal_volume ? _journal_year '1995' _journal_page_first '1817' _journal_page_last '1819' _cell_length_a 11.51300 _cell_length_b 16.09600 _cell_length_c 16.16400 _cell_angle_alpha 78.70000 _cell_angle_beta 76.49000 _cell_angle_gamma 87.67000 _symmetry_space_group_name_H-M 'P -1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_calc_flag Ti1 0.00360 0.32200 0.75800 d Ti2 -0.18240 0.47580 0.79940 d Ti3 -0.30450 0.24880 0.91870 d Ti4 -0.17840 0.14950 0.78230 d Ti5 -0.32980 0.08680 0.65260 d O1 -0.29500 0.37190 0.89080 d O2 -0.21900 0.51770 0.90280 d O3 -0.14300 0.38400 0.72800 d O4 -0.29500 0.24630 0.78940 d O5 -0.04200 0.22570 0.70770 d O6 -0.17900 0.14230 0.65760 d O7 -0.31700 0.07590 0.77770 d O8 -0.27500 0.12550 0.90680 d O9 0.10900 0.25630 0.81180 d O10 -0.11800 0.22800 0.86020 d O11 0.10900 0.37170 0.66520 d O12 -0.03200 0.40730 0.83000 d O13 -0.08600 0.56050 0.73860 d O14 -0.30800 0.51010 0.75390 d O15 -0.26900 0.23820 1.02350 d O16 -0.46200 0.23670 0.95320 d O17 -0.08100 0.06080 0.79750 d O18 -0.32200 -0.02300 0.65200 d O19 -0.47500 0.12000 0.68000 d O20 -0.30600 0.13200 0.54200 d C1 -0.36700 0.41400 0.95700 d C2 -0.28500 0.47000 0.97900 d C3 -0.21500 0.36400 0.67300 d C4 -0.32500 0.31600 0.72700 d C5 0.01300 0.19800 0.62700 d C6 -0.08600 0.17800 0.58700 d C7 -0.41200 0.06200 0.85100 d C8 -0.36300 0.05800 0.92800 d C9 0.07700 0.18100 0.87100 d C10 -0.04800 0.18900 0.92000 d C11 0.13000 0.43900 0.60000 d C12 0.04300 0.44200 0.87800 d C13 -0.08900 0.65000 0.71500 d C14 -0.41500 0.54300 0.75300 d C15 -0.31600 0.21600 1.11100 d C16 -0.58500 0.22400 0.96100 d C17 -0.07500 -0.02900 0.80600 d C18 -0.32300 -0.08700 0.60300 d C19 -0.59600 0.13400 0.68300 d C20 -0.28800 0.16100 0.44400 d C21 0.10100 0.41700 0.52000 d C22 0.25500 0.47400 0.58100 d C23 0.16200 0.47200 0.82000 d C24 0.04600 0.38300 0.96300 d C25 0.01400 0.68200 0.64200 d C26 -0.10100 0.69200 0.78600 d C27 -0.46000 0.61000 0.80000 d C28 -0.46100 0.54100 0.67200 d C29 -0.23900 0.25700 1.15700 d C30 -0.32700 0.12300 1.14000 d C31 -0.61700 0.28800 0.88700 d C32 -0.65600 0.23000 1.04800 d C33 -0.05500 -0.06900 0.89200 d C34 0.01100 -0.05300 0.73000 d C35 -0.19800 -0.10200 0.55300 d C36 -0.36700 -0.16500 0.66000 d C37 -0.65939 0.05379 0.70445 c C38 -0.61162 0.17923 0.59948 c C39 -0.36000 0.24000 0.45100 d C40 -0.33000 0.10500 0.40300 d H66 0.07390 0.48940 0.62023 c H67 0.00379 0.49855 0.89755 c H68 0.82970 0.66568 0.69436 c H69 0.54091 0.49522 0.80555 c H70 0.59411 0.23820 0.12631 c H71 0.39961 0.16099 0.95372 c H72 0.84095 0.94658 0.80378 c H73 0.62070 0.93277 0.55870 c H74 0.36854 0.17114 0.73120 c H75 0.80383 0.17696 0.41534 c H76 0.59390 0.36795 0.01329 c H77 0.56448 0.45079 0.93214 c H78 0.66496 0.51100 0.01917 c H79 0.77434 0.43214 0.01305 c H80 0.76014 0.42109 0.63450 c H81 0.83628 0.32582 0.63019 c H82 0.61409 0.35783 0.75963 c H83 0.63403 0.29063 0.68404 c H84 0.06585 0.14257 0.63980 c H85 0.06918 0.24735 0.58371 c H86 0.88386 0.23511 0.55174 c H87 0.94445 0.13317 0.54556 c H88 0.52495 0.11275 0.84707 c H89 0.54443 0.00320 0.85497 c H90 0.56709 0.06739 0.98223 c H91 0.67870 0.99782 0.94283 c H92 0.13564 0.16939 0.91473 c H93 0.08352 0.12941 0.83702 c H94 0.94964 0.22690 0.96807 c H95 0.91602 0.12730 0.95114 c H96 0.16049 0.36684 0.49799 o H97 0.11220 0.47385 0.46883 c H98 0.00780 0.39572 0.53594 c H99 0.26782 0.50012 0.63599 o H100 0.26868 0.52369 0.52257 c H101 0.31901 0.42295 0.56920 c H102 0.21154 0.41857 0.79613 o H103 0.21275 0.50058 0.85691 c H104 0.14707 0.52009 0.76535 c H105 -0.04456 0.36094 0.99702 o H106 0.08388 0.41712 1.00304 c H107 0.10321 0.32887 0.94950 c H108 0.09726 0.67400 0.66445 o H109 0.00008 0.74919 0.61729 c H110 0.01823 0.64655 0.58999 c H111 -0.18253 0.67049 0.83508 o H112 -0.10487 0.76048 0.76246 c H113 -0.02274 0.67802 0.81399 c H114 -0.55601 0.60118 0.82812 o H115 -0.44335 0.67117 0.75522 c H116 -0.41217 0.60855 0.85147 c H117 -0.39521 0.57020 0.61385 o H118 -0.54550 0.57561 0.67619 c H119 -0.47698 0.47500 0.66941 c H120 -0.14799 0.23191 1.14395 o H121 -0.27854 0.24352 1.22686 c H122 -0.23746 0.32572 1.13362 c H123 -0.37965 0.09677 1.10267 o H124 -0.37070 0.10873 1.20915 c H125 -0.23743 0.09530 1.13063 c H126 -0.62498 0.18322 1.09712 o H127 -0.75020 0.21843 1.05103 c H128 -0.64652 0.29405 1.05937 c H129 -0.59303 0.35211 0.89086 o H130 -0.71318 0.28406 0.89156 c H131 -0.56845 0.27222 0.82522 c H132 0.02542 -0.04237 0.90232 o H133 -0.04475 -0.13745 0.89503 c H134 -0.13294 -0.05752 0.94212 c H135 -0.02136 -0.03078 0.67089 o H136 0.02021 -0.12209 0.74123 c H137 0.09818 -0.02434 0.72358 c H138 -0.17210 -0.05107 0.49619 o H139 -0.19590 -0.16314 0.53250 c H140 -0.13608 -0.10399 0.59556 c H141 -0.31187 -0.18366 0.70738 o H142 -0.36440 -0.21425 0.62142 c H143 -0.45975 -0.15614 0.69347 c H144 -0.72787 0.05657 0.66694 o H145 -0.70106 0.04062 0.77398 c H146 -0.59537 0.00349 0.68963 c H147 -0.56503 0.24042 0.58245 o H148 -0.70726 0.18906 0.60291 c H149 -0.57561 0.14081 0.55041 c H150 -0.45552 0.22502 0.46557 o H151 -0.33492 0.28523 0.38949 c H152 -0.33976 0.26795 0.50268 c H153 -0.25843 0.06209 0.38041 o H154 -0.36222 0.14095 0.34788 c H155 -0.40456 0.06861 0.44874 c data_DOFWOK _audit_creation_date 2001-07-26 _audit_creation_method 'Created by WinPacha v3.5' _database_code_csd 'DOFWOK' _chemical_name_systematic 'tetrakis(2,6-Di-isopropylphenolato)-titanium(iv)' _chemical_compound_source 'Synthetic' _chemical_formula_structural '[Ti{OC6H4(Pri)2}4]' _chemical_formula_sum 'H272 C192 O16 Ti4' _publ_section_title ; Chemical and electrochemical reduction of titanium(IV) aryloxides ; loop_ _publ_author_name 'L.D. Durfee' 'S.L. Latesky' 'I.P. Rothwell' 'J.C. Huffman' 'K. Folting' _journal_name_full ; Inorganic Chemistry ; _journal_volume '24' _journal_year '1985' _journal_page_first '4569' _journal_page_last '4573' _cell_length_a 20.81100 _cell_length_b 11.06800 _cell_length_c 19.79700 _cell_angle_alpha 90.00000 _cell_angle_beta 75.48000 _cell_angle_gamma 90.00000 _symmetry_space_group_name_H-M 'I 12/a 1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_calc_flag Ti1 0.75000 0.20510 0.50000 d O1 0.78470 0.11290 0.42610 d C1 0.81560 0.02460 0.38120 d C2 0.88490 0.02560 0.35840 d C3 0.91380 -0.06590 0.31360 d C4 0.87680 -0.15310 0.29160 d C5 0.80870 -0.15050 0.31440 d C6 0.77660 -0.06340 0.35950 d C7 0.92570 0.12190 0.38310 d C8 0.94740 0.07990 0.44660 d C9 0.98490 0.16380 0.32720 d C10 0.70130 -0.06260 0.38680 d C11 0.66660 -0.08020 0.33190 d C12 0.68020 -0.14470 0.44870 d O2 0.68550 0.29720 0.48340 d C13 0.64490 0.39160 0.47780 d C14 0.62370 0.39980 0.41600 d C15 0.58670 0.50000 0.40850 d C16 0.56990 0.58600 0.45920 d C17 0.58980 0.57480 0.52030 d C18 0.62770 0.47670 0.53090 d C19 0.64070 0.30310 0.36010 d C20 0.57920 0.23670 0.35470 d C21 0.67650 0.35120 0.28940 d C22 0.65010 0.46670 0.59750 d C23 0.70320 0.55590 0.60080 d C24 0.59120 0.48170 0.66160 d H28 0.96748 -0.06750 0.29580 c H29 0.90095 -0.22312 0.25588 c H30 0.77922 -0.21917 0.29719 c H31 0.57091 0.50929 0.36057 c H32 0.54032 0.66298 0.45150 c H33 0.57630 0.64345 0.56042 c H34 0.89412 0.19857 0.39851 c H35 0.68861 0.02675 0.40628 c H36 0.67284 0.23940 0.37576 c H37 0.67007 0.37805 0.59939 c H38 1.00096 0.09341 0.43854 o H39 0.92128 0.13135 0.49261 c H40 0.93610 -0.01631 0.45589 c H41 0.96937 0.18947 0.28021 o H42 1.00783 0.24212 0.34571 c H43 1.02165 0.09105 0.31399 c H44 0.70253 -0.09596 0.28181 o H45 0.63338 -0.15836 0.34419 c H46 0.63718 0.00018 0.32744 c H47 0.70386 -0.23328 0.43676 o H48 0.69474 -0.10596 0.49362 c H49 0.62619 -0.15640 0.46212 c H50 0.54686 0.29697 0.33413 o H51 0.59263 0.15907 0.31962 c H52 0.55208 0.20437 0.40631 c H53 0.64782 0.42475 0.27411 o H54 0.72546 0.38564 0.29103 c H55 0.68291 0.27907 0.25034 c H56 0.73874 0.56300 0.54970 o H57 0.68118 0.64496 0.61575 c H58 0.72961 0.52682 0.63942 c H59 0.54851 0.42984 0.65450 o H60 0.60475 0.44904 0.70844 c H61 0.57723 0.57720 0.66877 c