Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Levason, William' ; Department of Chemistry University of Southampton Southampton SO17 1BJ, UK ; 'Popham, Michael C.' ; Department of Chemistry University of Southampton Southampton SO17 1BJ, UK ; 'Reid, Gillian' ; Department of Chemistry University of Southampton Southampton SO17 1BJ, UK ; 'Webster, Michael' ; Department of Chemistry University of Southampton Southampton SO17 1BJ, UK ; _publ_contact_author_name 'Professor W. Levason' _publ_contact_author_address ; Department of Chemistry University of Southampton Southampton SO17 1BJ, UK ; _publ_contact_author_email wxl@soton.ac.uk _publ_contact_author_fax '023 8059 6805' _publ_contact_author_phone '023 8059 3792' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_section_title ; Crown Ether Complexes of Titanium(IV) Chloride and Bromide and the Structures of the Hydrolysis Products [Ti2Cl6(mu-O)(18-crown-6)2] and [Ti4Cl8(mu-O)4(15-crown-5)4] ; _publ_contact_letter ; 12th October 2002 This is the cif to accompany paper ref. B210012F It contains details of two structures. W Levason ; _publ_section_references ; Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., Garcia-Granda, S., Gould, R.O., Smits, J.M.M. and Smykalla, C. (1992). The DIRDIF program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. Blessing, R. H. (1997). J. Appl. Cryst. 30, 421-426. Hooft, R. (1998). COLLECT. Nonius BV, Delft, The Netherlands. Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Molecular Structure Corporation. (1997-1999). teXsan for Windows. Single Crystal Structure Analysis Software. Version 1.06. MSC, 9009 New Trails Drive, The Woodlands, TX 77381, USA. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter & R. M. Sweet, pp. 307-326. London: Academic Press. Sheldrick, G. M. (1997). SHELXL97. University of Gottingen, Germany. ; data_d059 _database_code_CSD 195314 _audit_creation_method 'SHELXL-97 + hand edit' _chemical_name_systematic ; mu-oxo-bis(trichloro(1,4,7,10,13,16-hexaoxacyclooctadecane)titanium(IV)) toluene solvate ; _chemical_name_common ? _chemical_formula_moiety 'C24 H48 Cl6 O13 Ti2, 0.5(C7 H8)' _chemical_formula_sum 'C27.50 H52 Cl6 O13 Ti2' _chemical_formula_weight 899.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 10.2483(5) _cell_length_b 13.8350(10) _cell_length_c 14.7207(10) _cell_angle_alpha 84.669(3) _cell_angle_beta 81.909(3) _cell_angle_gamma 79.892(3) _cell_volume 2029.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 8816 _cell_measurement_theta_min 2.9 _cell_measurement_theta_max 27.5 _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 934 _exptl_absorpt_coefficient_mu 0.844 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SORTAV, R H Blessing, J. Appl. Cryst., 1997, 30, 421-426.' _exptl_absorpt_correction_T_min 0.8048 # shelxl 0.8494 _exptl_absorpt_correction_T_max 0.8515 # shelxl 0.9204 _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38655 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9239 _reflns_number_gt 8071 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+1.5908P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9239 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0916 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.07900(3) 0.09499(2) 0.21149(2) 0.01254(8) Uani 1 d . . . Ti2 Ti -0.22700(3) 0.24497(2) 0.16125(2) 0.01324(8) Uani 1 d . . . Cl1 Cl -0.01868(5) 0.04503(3) 0.35361(3) 0.02063(10) Uani 1 d . . . Cl2 Cl 0.15873(5) 0.21644(3) 0.26749(3) 0.01957(10) Uani 1 d . . . Cl3 Cl 0.20258(4) 0.11213(3) 0.06692(3) 0.01826(10) Uani 1 d . . . Cl4 Cl -0.36741(5) 0.16656(3) 0.26172(3) 0.02188(10) Uani 1 d . . . Cl5 Cl -0.19756(5) 0.35126(3) 0.26573(3) 0.02164(10) Uani 1 d . . . Cl6 Cl -0.25651(5) 0.16819(3) 0.03381(3) 0.02074(10) Uani 1 d . . . O1 O 0.25259(12) -0.01374(9) 0.24136(9) 0.0170(3) Uani 1 d . . . O2 O 0.04727(12) -0.03872(9) 0.16861(9) 0.0156(3) Uani 1 d . . . O3 O -0.15313(13) -0.17338(9) 0.21529(9) 0.0201(3) Uani 1 d . . . O4 O -0.07330(15) -0.22405(12) 0.39482(9) 0.0277(3) Uani 1 d . . . O5 O 0.21196(16) -0.24845(13) 0.44624(10) 0.0341(4) Uani 1 d . . . O6 O 0.42071(16) -0.13307(12) 0.36302(11) 0.0348(4) Uani 1 d . . . O7 O -0.14294(12) 0.34726(9) 0.06250(9) 0.0181(3) Uani 1 d . . . O8 O -0.39584(12) 0.35558(9) 0.12625(9) 0.0163(3) Uani 1 d . . . O9 O -0.58237(13) 0.33573(9) -0.00470(9) 0.0194(3) Uani 1 d . . . O10 O -0.41540(13) 0.34650(11) -0.17935(9) 0.0227(3) Uani 1 d . . . O11 O -0.21944(14) 0.47693(10) -0.23153(9) 0.0220(3) Uani 1 d . . . O12 O -0.01580(13) 0.42423(9) -0.10861(9) 0.0198(3) Uani 1 d . . . O13 O -0.07188(12) 0.16489(9) 0.17447(9) 0.0165(3) Uani 1 d . . . C1 C 0.26360(19) -0.10719(14) 0.20060(14) 0.0203(4) Uani 1 d . . . H1A H 0.3188 -0.1601 0.2351 0.0275(9) Uiso 1 calc R . . H1B H 0.3056 -0.1027 0.1359 0.0275(9) Uiso 1 calc R . . C2 C 0.12433(18) -0.12824(13) 0.20558(13) 0.0176(4) Uani 1 d . . . H2A H 0.1227 -0.1841 0.1686 0.0275(9) Uiso 1 calc R . . H2B H 0.0879 -0.1445 0.2700 0.0275(9) Uiso 1 calc R . . C3 C -0.05911(18) -0.05056(13) 0.11680(12) 0.0166(4) Uani 1 d . . . H3A H -0.0262 -0.1043 0.0751 0.0275(9) Uiso 1 calc R . . H3B H -0.0838 0.0108 0.0785 0.0275(9) Uiso 1 calc R . . C4 C -0.18047(19) -0.07385(13) 0.17858(13) 0.0191(4) Uani 1 d . . . H4A H -0.2026 -0.0290 0.2292 0.0275(9) Uiso 1 calc R . . H4B H -0.2577 -0.0649 0.1434 0.0275(9) Uiso 1 calc R . . C5 C -0.2412(2) -0.19553(15) 0.29523(14) 0.0244(4) Uani 1 d . . . H5A H -0.2443 -0.2670 0.3008 0.0275(9) Uiso 1 calc R . . H5B H -0.3323 -0.1602 0.2883 0.0275(9) Uiso 1 calc R . . C6 C -0.1994(2) -0.16738(16) 0.38143(14) 0.0269(4) Uani 1 d . . . H6A H -0.1933 -0.0964 0.3760 0.0275(9) Uiso 1 calc R . . H6B H -0.2664 -0.1799 0.4347 0.0275(9) Uiso 1 calc R . . C7 C -0.0339(2) -0.20579(18) 0.47968(14) 0.0319(5) Uani 1 d . . . H7A H -0.1057 -0.2157 0.5304 0.0275(9) Uiso 1 calc R . . H7B H -0.0193 -0.1367 0.4776 0.0275(9) Uiso 1 calc R . . C8 C 0.0921(2) -0.27406(19) 0.49696(14) 0.0326(5) Uani 1 d . . . H8A H 0.1005 -0.2769 0.5634 0.0275(9) Uiso 1 calc R . . H8B H 0.0838 -0.3409 0.4822 0.0275(9) Uiso 1 calc R . . C9 C 0.2670(3) -0.1836(2) 0.49225(16) 0.0476(7) Uani 1 d . . . H9A H 0.2639 -0.2062 0.5582 0.0275(9) Uiso 1 calc R . . H9B H 0.2124 -0.1172 0.4876 0.0275(9) Uiso 1 calc R . . C10 C 0.4056(3) -0.1778(2) 0.45378(17) 0.0460(7) Uani 1 d . . . H10A H 0.4441 -0.1401 0.4944 0.0275(9) Uiso 1 calc R . . H10B H 0.4578 -0.2452 0.4540 0.0275(9) Uiso 1 calc R . . C11 C 0.4026(2) -0.02820(18) 0.35583(16) 0.0338(5) Uani 1 d . . . H11A H 0.4826 -0.0056 0.3715 0.0275(9) Uiso 1 calc R . . H11B H 0.3244 -0.0012 0.3990 0.0275(9) Uiso 1 calc R . . C12 C 0.38059(19) 0.00666(15) 0.25848(14) 0.0228(4) Uani 1 d . . . H12A H 0.3821 0.0782 0.2487 0.0275(9) Uiso 1 calc R . . H12B H 0.4529 -0.0276 0.2152 0.0275(9) Uiso 1 calc R . . C13 C -0.22623(19) 0.44375(14) 0.05369(14) 0.0217(4) Uani 1 d . . . H13A H -0.1937 0.4817 -0.0027 0.0275(9) Uiso 1 calc R . . H13B H -0.2255 0.4815 0.1075 0.0275(9) Uiso 1 calc R . . C14 C -0.36327(19) 0.42405(14) 0.04879(14) 0.0214(4) Uani 1 d . . . H14A H -0.4283 0.4860 0.0521 0.0275(9) Uiso 1 calc R . . H14B H -0.3663 0.3952 -0.0098 0.0275(9) Uiso 1 calc R . . C15 C -0.53941(17) 0.35424(14) 0.14774(13) 0.0189(4) Uani 1 d . . . H15A H -0.5882 0.4224 0.1411 0.0275(9) Uiso 1 calc R . . H15B H -0.5587 0.3294 0.2126 0.0275(9) Uiso 1 calc R . . C16 C -0.58995(19) 0.29147(14) 0.08716(13) 0.0208(4) Uani 1 d . . . H16A H -0.5354 0.2249 0.0880 0.0275(9) Uiso 1 calc R . . H16B H -0.6837 0.2849 0.1103 0.0275(9) Uiso 1 calc R . . C17 C -0.56668(19) 0.26619(14) -0.07235(13) 0.0204(4) Uani 1 d . . . H17A H -0.6478 0.2353 -0.0670 0.0275(9) Uiso 1 calc R . . H17B H -0.4897 0.2137 -0.0627 0.0275(9) Uiso 1 calc R . . C18 C -0.54389(19) 0.31735(15) -0.16590(14) 0.0223(4) Uani 1 d . . . H18A H -0.5495 0.2726 -0.2134 0.0275(9) Uiso 1 calc R . . H18B H -0.6138 0.3760 -0.1719 0.0275(9) Uiso 1 calc R . . C19 C -0.3909(2) 0.39535(16) -0.26799(13) 0.0248(4) Uani 1 d . . . H19A H -0.4484 0.4608 -0.2702 0.0275(9) Uiso 1 calc R . . H19B H -0.4136 0.3566 -0.3151 0.0275(9) Uiso 1 calc R . . C20 C -0.2471(2) 0.40760(15) -0.28877(13) 0.0237(4) Uani 1 d . . . H20A H -0.1892 0.3434 -0.2781 0.0275(9) Uiso 1 calc R . . H20B H -0.2276 0.4307 -0.3542 0.0275(9) Uiso 1 calc R . . C21 C -0.0853(2) 0.49467(14) -0.25072(14) 0.0223(4) Uani 1 d . . . H21A H -0.0807 0.5596 -0.2293 0.0275(9) Uiso 1 calc R . . H21B H -0.0588 0.4974 -0.3181 0.0275(9) Uiso 1 calc R . . C22 C 0.01244(19) 0.41723(14) -0.20570(13) 0.0211(4) Uani 1 d . . . H22A H 0.0032 0.3510 -0.2217 0.0275(9) Uiso 1 calc R . . H22B H 0.1051 0.4280 -0.2273 0.0275(9) Uiso 1 calc R . . C23 C 0.04719(19) 0.34222(14) -0.05656(13) 0.0211(4) Uani 1 d . . . H23A H 0.1453 0.3390 -0.0677 0.0275(9) Uiso 1 calc R . . H23B H 0.0257 0.2807 -0.0756 0.0275(9) Uiso 1 calc R . . C24 C -0.00090(18) 0.35243(13) 0.04368(13) 0.0178(4) Uani 1 d . . . H24A H 0.0497 0.2992 0.0807 0.0275(9) Uiso 1 calc R . . H24B H 0.0151 0.4162 0.0615 0.0275(9) Uiso 1 calc R . . C25 C 0.2668(5) 0.4697(4) 0.5527(3) 0.0391(11) Uani 0.50 d P . . C26 C 0.3832(3) 0.4995(2) 0.54089(18) 0.0411(6) Uiso 1 d . . . C27 C 0.4878(4) 0.4690(3) 0.4709(3) 0.0286(9) Uiso 0.50 d P . . C28 C 0.4664(5) 0.3978(3) 0.4157(3) 0.0291(9) Uani 0.50 d P . . C29 C 0.3452(5) 0.3636(3) 0.4282(3) 0.0345(10) Uani 0.50 d P . . C30 C 0.2445(5) 0.3995(4) 0.4969(3) 0.0390(11) Uani 0.50 d P . . 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 0.01244(15) 0.01150(15) 0.01371(15) -0.00164(12) -0.00321(12) -0.00043(11) Ti2 0.01240(15) 0.01273(15) 0.01423(15) -0.00156(12) -0.00296(12) 0.00026(12) Cl1 0.0241(2) 0.0210(2) 0.0159(2) -0.00129(17) 0.00124(17) -0.00435(18) Cl2 0.0224(2) 0.0185(2) 0.0199(2) -0.00518(17) -0.00409(17) -0.00617(17) Cl3 0.0204(2) 0.0187(2) 0.0155(2) -0.00200(16) -0.00029(16) -0.00388(17) Cl4 0.0182(2) 0.0222(2) 0.0241(2) 0.00222(18) -0.00008(17) -0.00439(17) Cl5 0.0257(2) 0.0189(2) 0.0216(2) -0.00623(17) -0.00774(18) -0.00090(18) Cl6 0.0213(2) 0.0203(2) 0.0209(2) -0.00749(17) -0.00832(17) 0.00343(17) O1 0.0135(6) 0.0167(6) 0.0212(6) -0.0040(5) -0.0058(5) 0.0006(5) O2 0.0166(6) 0.0109(6) 0.0203(6) -0.0009(5) -0.0075(5) -0.0009(5) O3 0.0203(7) 0.0157(6) 0.0231(7) -0.0004(5) -0.0007(5) -0.0015(5) O4 0.0257(7) 0.0390(9) 0.0179(7) -0.0041(6) -0.0028(6) -0.0026(6) O5 0.0324(8) 0.0498(10) 0.0216(7) -0.0059(7) -0.0022(6) -0.0098(7) O6 0.0312(8) 0.0418(9) 0.0318(8) 0.0117(7) -0.0131(7) -0.0071(7) O7 0.0137(6) 0.0144(6) 0.0239(7) 0.0036(5) -0.0019(5) 0.0012(5) O8 0.0118(6) 0.0154(6) 0.0210(6) -0.0006(5) -0.0032(5) 0.0006(5) O9 0.0229(7) 0.0165(6) 0.0192(6) -0.0026(5) -0.0037(5) -0.0023(5) O10 0.0176(7) 0.0320(8) 0.0200(6) -0.0014(6) -0.0047(5) -0.0064(6) O11 0.0206(7) 0.0218(7) 0.0230(7) -0.0071(6) -0.0017(5) -0.0002(5) O12 0.0240(7) 0.0149(6) 0.0188(6) -0.0012(5) -0.0021(5) 0.0009(5) O13 0.0158(6) 0.0147(6) 0.0190(6) -0.0021(5) -0.0042(5) -0.0006(5) C1 0.0182(9) 0.0174(9) 0.0251(9) -0.0059(7) -0.0065(8) 0.0027(7) C2 0.0196(9) 0.0120(8) 0.0203(9) -0.0006(7) -0.0063(7) 0.0028(7) C3 0.0203(9) 0.0147(8) 0.0163(8) -0.0019(7) -0.0089(7) -0.0014(7) C4 0.0172(9) 0.0152(8) 0.0253(9) -0.0017(7) -0.0066(7) -0.0006(7) C5 0.0189(9) 0.0258(10) 0.0280(10) -0.0008(8) 0.0000(8) -0.0054(8) C6 0.0222(10) 0.0325(11) 0.0251(10) -0.0047(9) 0.0020(8) -0.0048(9) C7 0.0345(12) 0.0432(13) 0.0160(9) -0.0027(9) -0.0027(8) -0.0008(10) C8 0.0305(11) 0.0457(13) 0.0191(10) 0.0041(9) -0.0026(8) -0.0034(10) C9 0.0540(16) 0.0717(19) 0.0230(11) -0.0066(12) -0.0041(11) -0.0250(15) C10 0.0428(15) 0.0649(18) 0.0339(13) 0.0100(12) -0.0211(11) -0.0128(13) C11 0.0241(11) 0.0463(14) 0.0339(12) -0.0075(10) -0.0150(9) -0.0021(10) C12 0.0132(9) 0.0249(10) 0.0312(10) -0.0004(8) -0.0079(8) -0.0028(7) C13 0.0187(9) 0.0135(8) 0.0310(10) 0.0027(8) -0.0043(8) 0.0015(7) C14 0.0181(9) 0.0159(9) 0.0295(10) 0.0060(8) -0.0062(8) -0.0023(7) C15 0.0098(8) 0.0241(9) 0.0205(9) -0.0032(8) 0.0002(7) 0.0025(7) C16 0.0156(9) 0.0223(9) 0.0243(9) 0.0015(8) -0.0025(7) -0.0039(7) C17 0.0148(8) 0.0196(9) 0.0275(10) -0.0080(8) -0.0035(7) -0.0011(7) C18 0.0150(9) 0.0276(10) 0.0254(10) -0.0072(8) -0.0054(7) -0.0017(8) C19 0.0264(10) 0.0298(11) 0.0188(9) -0.0032(8) -0.0055(8) -0.0033(8) C20 0.0274(10) 0.0253(10) 0.0188(9) -0.0055(8) -0.0004(8) -0.0050(8) C21 0.0242(10) 0.0204(9) 0.0218(9) 0.0002(8) -0.0009(8) -0.0049(8) C22 0.0204(9) 0.0212(9) 0.0203(9) -0.0030(7) 0.0005(7) -0.0010(7) C23 0.0191(9) 0.0155(9) 0.0259(10) 0.0007(7) 0.0006(8) 0.0009(7) C24 0.0134(8) 0.0155(8) 0.0247(9) 0.0019(7) -0.0049(7) -0.0028(7) C25 0.048(3) 0.034(2) 0.029(2) 0.006(2) 0.005(2) -0.003(2) C28 0.036(2) 0.025(2) 0.024(2) 0.0010(17) -0.0076(18) 0.0031(18) C29 0.047(3) 0.023(2) 0.032(2) 0.0066(18) -0.005(2) -0.007(2) C30 0.046(3) 0.030(2) 0.038(3) 0.012(2) -0.001(2) -0.011(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O13 1.7993(12) . ? Ti1 O2 2.1004(12) . ? Ti1 O1 2.1860(13) . ? Ti1 Cl2 2.2582(5) . ? Ti1 Cl1 2.2893(5) . ? Ti1 Cl3 2.3329(5) . ? Ti2 O13 1.7948(12) . ? Ti2 O7 2.1334(13) . ? Ti2 O8 2.1856(12) . ? Ti2 Cl4 2.2551(5) . ? Ti2 Cl5 2.3077(5) . ? Ti2 Cl6 2.3199(5) . ? O1 C12 1.449(2) . ? O1 C1 1.455(2) . ? O2 C2 1.451(2) . ? O2 C3 1.455(2) . ? O3 C5 1.423(2) . ? O3 C4 1.427(2) . ? O4 C6 1.418(3) . ? O4 C7 1.423(2) . ? O5 C9 1.407(3) . ? O5 C8 1.428(3) . ? O6 C10 1.419(3) . ? O6 C11 1.426(3) . ? O7 C24 1.456(2) . ? O7 C13 1.458(2) . ? O8 C14 1.453(2) . ? O8 C15 1.464(2) . ? O9 C17 1.422(2) . ? O9 C16 1.429(2) . ? O10 C19 1.423(2) . ? O10 C18 1.426(2) . ? O11 C20 1.423(2) . ? O11 C21 1.424(2) . ? O12 C23 1.418(2) . ? O12 C22 1.427(2) . ? C1 C2 1.497(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.498(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.499(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.498(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.467(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.504(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.489(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.500(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.496(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.498(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.506(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.500(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.312(6) . ? C25 C30 1.396(8) . ? C26 C27 1.414(5) . ? C26 C27 1.447(5) 2_666 ? C27 C27 1.344(9) 2_666 ? C27 C28 1.397(6) . ? C27 C26 1.447(5) 2_666 ? C28 C29 1.388(7) . ? C29 C30 1.398(7) . ? 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 O13 Ti1 O2 94.50(5) . . ? O13 Ti1 O1 168.28(5) . . ? O2 Ti1 O1 73.95(5) . . ? O13 Ti1 Cl2 99.32(4) . . ? O2 Ti1 Cl2 166.18(4) . . ? O1 Ti1 Cl2 92.23(4) . . ? O13 Ti1 Cl1 95.55(4) . . ? O2 Ti1 Cl1 86.16(4) . . ? O1 Ti1 Cl1 85.78(4) . . ? Cl2 Ti1 Cl1 92.78(2) . . ? O13 Ti1 Cl3 93.49(4) . . ? O2 Ti1 Cl3 85.26(4) . . ? O1 Ti1 Cl3 83.78(4) . . ? Cl2 Ti1 Cl3 93.541(19) . . ? Cl1 Ti1 Cl3 167.99(2) . . ? O13 Ti2 O7 95.70(5) . . ? O13 Ti2 O8 170.17(5) . . ? O7 Ti2 O8 74.54(5) . . ? O13 Ti2 Cl4 99.98(4) . . ? O7 Ti2 Cl4 164.30(4) . . ? O8 Ti2 Cl4 89.80(4) . . ? O13 Ti2 Cl5 93.85(4) . . ? O7 Ti2 Cl5 83.81(4) . . ? O8 Ti2 Cl5 86.34(4) . . ? Cl4 Ti2 Cl5 94.24(2) . . ? O13 Ti2 Cl6 92.21(4) . . ? O7 Ti2 Cl6 84.68(4) . . ? O8 Ti2 Cl6 85.83(4) . . ? Cl4 Ti2 Cl6 95.50(2) . . ? Cl5 Ti2 Cl6 167.46(2) . . ? C12 O1 C1 112.67(14) . . ? C12 O1 Ti1 126.45(11) . . ? C1 O1 Ti1 114.84(10) . . ? C2 O2 C3 116.66(13) . . ? C2 O2 Ti1 117.11(10) . . ? C3 O2 Ti1 125.50(10) . . ? C5 O3 C4 113.83(14) . . ? C6 O4 C7 111.01(16) . . ? C9 O5 C8 111.98(18) . . ? C10 O6 C11 115.7(2) . . ? C24 O7 C13 112.41(13) . . ? C24 O7 Ti2 124.35(10) . . ? C13 O7 Ti2 114.58(11) . . ? C14 O8 C15 113.09(13) . . ? C14 O8 Ti2 114.31(10) . . ? C15 O8 Ti2 129.63(11) . . ? C17 O9 C16 113.09(14) . . ? C19 O10 C18 110.93(14) . . ? C20 O11 C21 112.57(14) . . ? C23 O12 C22 113.96(14) . . ? Ti2 O13 Ti1 167.75(8) . . ? O1 C1 C2 106.50(14) . . ? O1 C1 H1A 110.4 . . ? C2 C1 H1A 110.4 . . ? O1 C1 H1B 110.4 . . ? C2 C1 H1B 110.4 . . ? H1A C1 H1B 108.6 . . ? O2 C2 C1 105.52(14) . . ? O2 C2 H2A 110.6 . . ? C1 C2 H2A 110.6 . . ? O2 C2 H2B 110.6 . . ? C1 C2 H2B 110.6 . . ? H2A C2 H2B 108.8 . . ? O2 C3 C4 111.96(14) . . ? O2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? O2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? O3 C4 C3 108.56(15) . . ? O3 C4 H4A 110.0 . . ? C3 C4 H4A 110.0 . . ? O3 C4 H4B 110.0 . . ? C3 C4 H4B 110.0 . . ? H4A C4 H4B 108.4 . . ? O3 C5 C6 112.60(16) . . ? O3 C5 H5A 109.1 . . ? C6 C5 H5A 109.1 . . ? O3 C5 H5B 109.1 . . ? C6 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? O4 C6 C5 108.77(17) . . ? O4 C6 H6A 109.9 . . ? C5 C6 H6A 109.9 . . ? O4 C6 H6B 109.9 . . ? C5 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? O4 C7 C8 109.98(18) . . ? O4 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? O4 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? O5 C8 C7 115.50(19) . . ? O5 C8 H8A 108.4 . . ? C7 C8 H8A 108.4 . . ? O5 C8 H8B 108.4 . . ? C7 C8 H8B 108.4 . . ? H8A C8 H8B 107.5 . . ? O5 C9 C10 111.9(2) . . ? O5 C9 H9A 109.2 . . ? C10 C9 H9A 109.2 . . ? O5 C9 H9B 109.2 . . ? C10 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? O6 C10 C9 114.4(2) . . ? O6 C10 H10A 108.7 . . ? C9 C10 H10A 108.7 . . ? O6 C10 H10B 108.7 . . ? C9 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? O6 C11 C12 108.02(18) . . ? O6 C11 H11A 110.1 . . ? C12 C11 H11A 110.1 . . ? O6 C11 H11B 110.1 . . ? C12 C11 H11B 110.1 . . ? H11A C11 H11B 108.4 . . ? O1 C12 C11 109.27(16) . . ? O1 C12 H12A 109.8 . . ? C11 C12 H12A 109.8 . . ? O1 C12 H12B 109.8 . . ? C11 C12 H12B 109.8 . . ? H12A C12 H12B 108.3 . . ? O7 C13 C14 105.62(15) . . ? O7 C13 H13A 110.6 . . ? C14 C13 H13A 110.6 . . ? O7 C13 H13B 110.6 . . ? C14 C13 H13B 110.6 . . ? H13A C13 H13B 108.7 . . ? O8 C14 C13 107.47(15) . . ? O8 C14 H14A 110.2 . . ? C13 C14 H14A 110.2 . . ? O8 C14 H14B 110.2 . . ? C13 C14 H14B 110.2 . . ? H14A C14 H14B 108.5 . . ? O8 C15 C16 113.06(15) . . ? O8 C15 H15A 109.0 . . ? C16 C15 H15A 109.0 . . ? O8 C15 H15B 109.0 . . ? C16 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? O9 C16 C15 109.44(15) . . ? O9 C16 H16A 109.8 . . ? C15 C16 H16A 109.8 . . ? O9 C16 H16B 109.8 . . ? C15 C16 H16B 109.8 . . ? H16A C16 H16B 108.2 . . ? O9 C17 C18 109.27(15) . . ? O9 C17 H17A 109.8 . . ? C18 C17 H17A 109.8 . . ? O9 C17 H17B 109.8 . . ? C18 C17 H17B 109.8 . . ? H17A C17 H17B 108.3 . . ? O10 C18 C17 109.70(15) . . ? O10 C18 H18A 109.7 . . ? C17 C18 H18A 109.7 . . ? O10 C18 H18B 109.7 . . ? C17 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? O10 C19 C20 110.44(16) . . ? O10 C19 H19A 109.6 . . ? C20 C19 H19A 109.6 . . ? O10 C19 H19B 109.6 . . ? C20 C19 H19B 109.6 . . ? H19A C19 H19B 108.1 . . ? O11 C20 C19 109.97(16) . . ? O11 C20 H20A 109.7 . . ? C19 C20 H20A 109.7 . . ? O11 C20 H20B 109.7 . . ? C19 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? O11 C21 C22 113.15(16) . . ? O11 C21 H21A 108.9 . . ? C22 C21 H21A 108.9 . . ? O11 C21 H21B 108.9 . . ? C22 C21 H21B 108.9 . . ? H21A C21 H21B 107.8 . . ? O12 C22 C21 107.98(15) . . ? O12 C22 H22A 110.1 . . ? C21 C22 H22A 110.1 . . ? O12 C22 H22B 110.1 . . ? C21 C22 H22B 110.1 . . ? H22A C22 H22B 108.4 . . ? O12 C23 C24 109.26(15) . . ? O12 C23 H23A 109.8 . . ? C24 C23 H23A 109.8 . . ? O12 C23 H23B 109.8 . . ? C24 C23 H23B 109.8 . . ? H23A C23 H23B 108.3 . . ? O7 C24 C23 110.32(15) . . ? O7 C24 H24A 109.6 . . ? C23 C24 H24A 109.6 . . ? O7 C24 H24B 109.6 . . ? C23 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? C26 C25 C30 119.3(4) . . ? C25 C26 C27 124.1(3) . . ? C25 C26 C27 179.0(3) . 2_666 ? C27 C26 C27 56.0(3) . 2_666 ? C27 C27 C28 175.0(6) 2_666 . ? C27 C27 C26 63.2(3) 2_666 . ? C28 C27 C26 116.6(4) . . ? C27 C27 C26 60.8(3) 2_666 2_666 ? C28 C27 C26 119.2(4) . 2_666 ? C26 C27 C26 124.0(3) . 2_666 ? C29 C28 C27 120.2(4) . . ? C28 C29 C30 120.1(4) . . ? C25 C30 C29 119.6(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O13 Ti1 O1 C12 152.2(3) . . . . ? O2 Ti1 O1 C12 161.98(15) . . . . ? Cl2 Ti1 O1 C12 -18.18(14) . . . . ? Cl1 Ti1 O1 C12 -110.81(14) . . . . ? Cl3 Ti1 O1 C12 75.14(13) . . . . ? O13 Ti1 O1 C1 1.8(3) . . . . ? O2 Ti1 O1 C1 11.55(11) . . . . ? Cl2 Ti1 O1 C1 -168.62(11) . . . . ? Cl1 Ti1 O1 C1 98.76(11) . . . . ? Cl3 Ti1 O1 C1 -75.29(11) . . . . ? O13 Ti1 O2 C2 -163.30(12) . . . . ? O1 Ti1 O2 C2 18.69(11) . . . . ? Cl2 Ti1 O2 C2 18.0(2) . . . . ? Cl1 Ti1 O2 C2 -68.02(11) . . . . ? Cl3 Ti1 O2 C2 103.56(11) . . . . ? O13 Ti1 O2 C3 6.58(13) . . . . ? O1 Ti1 O2 C3 -171.44(14) . . . . ? Cl2 Ti1 O2 C3 -172.11(13) . . . . ? Cl1 Ti1 O2 C3 101.86(13) . . . . ? Cl3 Ti1 O2 C3 -86.56(12) . . . . ? O13 Ti2 O7 C24 -15.17(14) . . . . ? O8 Ti2 O7 C24 166.00(14) . . . . ? Cl4 Ti2 O7 C24 161.74(12) . . . . ? Cl5 Ti2 O7 C24 78.10(13) . . . . ? Cl6 Ti2 O7 C24 -106.87(13) . . . . ? O13 Ti2 O7 C13 -160.28(12) . . . . ? O8 Ti2 O7 C13 20.88(12) . . . . ? Cl4 Ti2 O7 C13 16.6(2) . . . . ? Cl5 Ti2 O7 C13 -67.01(12) . . . . ? Cl6 Ti2 O7 C13 108.01(12) . . . . ? O13 Ti2 O8 C14 2.5(4) . . . . ? O7 Ti2 O8 C14 9.34(11) . . . . ? Cl4 Ti2 O8 C14 -171.81(11) . . . . ? Cl5 Ti2 O8 C14 93.92(11) . . . . ? Cl6 Ti2 O8 C14 -76.29(11) . . . . ? O13 Ti2 O8 C15 161.4(3) . . . . ? O7 Ti2 O8 C15 168.22(15) . . . . ? Cl4 Ti2 O8 C15 -12.93(13) . . . . ? Cl5 Ti2 O8 C15 -107.20(13) . . . . ? Cl6 Ti2 O8 C15 82.59(13) . . . . ? O7 Ti2 O13 Ti1 109.2(4) . . . . ? O8 Ti2 O13 Ti1 115.8(4) . . . . ? Cl4 Ti2 O13 Ti1 -70.0(4) . . . . ? Cl5 Ti2 O13 Ti1 25.0(4) . . . . ? Cl6 Ti2 O13 Ti1 -165.9(4) . . . . ? O2 Ti1 O13 Ti2 133.5(4) . . . . ? O1 Ti1 O13 Ti2 143.0(3) . . . . ? Cl2 Ti1 O13 Ti2 -46.8(4) . . . . ? Cl1 Ti1 O13 Ti2 47.0(4) . . . . ? Cl3 Ti1 O13 Ti2 -141.0(4) . . . . ? C12 O1 C1 C2 168.20(15) . . . . ? Ti1 O1 C1 C2 -37.27(17) . . . . ? C3 O2 C2 C1 145.47(15) . . . . ? Ti1 O2 C2 C1 -43.74(17) . . . . ? O1 C1 C2 O2 49.53(18) . . . . ? C2 O2 C3 C4 77.59(18) . . . . ? Ti1 O2 C3 C4 -92.33(16) . . . . ? C5 O3 C4 C3 161.41(15) . . . . ? O2 C3 C4 O3 -73.86(18) . . . . ? C4 O3 C5 C6 -83.4(2) . . . . ? C7 O4 C6 C5 -175.37(17) . . . . ? O3 C5 C6 O4 -63.3(2) . . . . ? C6 O4 C7 C8 174.01(18) . . . . ? C9 O5 C8 C7 87.7(3) . . . . ? O4 C7 C8 O5 77.6(3) . . . . ? C8 O5 C9 C10 164.9(2) . . . . ? C11 O6 C10 C9 83.8(3) . . . . ? O5 C9 C10 O6 67.3(3) . . . . ? C10 O6 C11 C12 -163.10(18) . . . . ? C1 O1 C12 C11 -94.05(19) . . . . ? Ti1 O1 C12 C11 114.98(16) . . . . ? O6 C11 C12 O1 68.5(2) . . . . ? C24 O7 C13 C14 164.65(15) . . . . ? Ti2 O7 C13 C14 -46.07(18) . . . . ? C15 O8 C14 C13 161.25(15) . . . . ? Ti2 O8 C14 C13 -36.31(18) . . . . ? O7 C13 C14 O8 51.5(2) . . . . ? C14 O8 C15 C16 81.46(19) . . . . ? Ti2 O8 C15 C16 -77.62(18) . . . . ? C17 O9 C16 C15 152.26(15) . . . . ? O8 C15 C16 O9 -67.98(19) . . . . ? C16 O9 C17 C18 -173.51(15) . . . . ? C19 O10 C18 C17 179.93(16) . . . . ? O9 C17 C18 O10 69.73(19) . . . . ? C18 O10 C19 C20 -168.69(16) . . . . ? C21 O11 C20 C19 -177.63(16) . . . . ? O10 C19 C20 O11 -69.3(2) . . . . ? C20 O11 C21 C22 -81.4(2) . . . . ? C23 O12 C22 C21 166.23(15) . . . . ? O11 C21 C22 O12 -67.0(2) . . . . ? C22 O12 C23 C24 -173.99(15) . . . . ? C13 O7 C24 C23 -90.14(18) . . . . ? Ti2 O7 C24 C23 124.10(13) . . . . ? O12 C23 C24 O7 65.19(19) . . . . ? C30 C25 C26 C27 3.6(6) . . . . ? C30 C25 C26 C27 -95(21) . . . 2_666 ? C25 C26 C27 C27 -178.8(4) . . . 2_666 ? C25 C26 C27 C28 -4.4(6) . . . . ? C27 C26 C27 C28 174.4(6) 2_666 . . . ? C25 C26 C27 C26 -178.8(4) . . . 2_666 ? C27 C26 C27 C26 0.000(1) 2_666 . . 2_666 ? C27 C27 C28 C29 89(7) 2_666 . . . ? C26 C27 C28 C29 2.8(6) . . . . ? C26 C27 C28 C29 177.5(4) 2_666 . . . ? C27 C28 C29 C30 -0.8(7) . . . . ? C26 C25 C30 C29 -1.3(7) . . . . ? C28 C29 C30 C25 0.0(7) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.160 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.071 #===END OF CIF====================================================== data_ticl15 _database_code_CSD 195315 _audit_creation_method 'SHELXL-97 + hand edit ' _chemical_name_systematic ; cyclo-tetrakis((mu-oxo)-dichloro-(1,4,7,10,13-pentaoxacyclopentadecane)- titanium(IV)) toluene solvate hydrate ; _chemical_name_common ? _chemical_formula_moiety 'C40 H80 Cl8 O24 Ti, 4(C7 H8), 2(H2 O)' _chemical_formula_sum 'C68 H116 Cl8 O26 Ti4' _chemical_formula_weight 1824.81 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 4/n' _symmetry_Int_Tables_number 85 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' _cell_length_a 20.353(3) _cell_length_b 20.353(3) _cell_length_c 10.739(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4448.6(12) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 26637 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 0.655 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SORTAV, R H Blessing, J. Appl. Cryst., 1997, 30, 421-426.' _exptl_absorpt_correction_T_min 0.8134 # shelxl 0.8802 _exptl_absorpt_correction_T_max 0.8295 # shelxl 0.9374 _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16577 _diffrn_reflns_av_R_equivalents 0.1785 _diffrn_reflns_av_sigmaI/netI 0.1917 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3883 _reflns_number_gt 1722 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1040P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3883 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1935 _refine_ls_R_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.2180 _refine_ls_wR_factor_gt 0.1671 _refine_ls_goodness_of_fit_ref 0.910 _refine_ls_restrained_S_all 0.910 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.65825(7) 0.33827(7) 0.01282(12) 0.0297(4) Uani 1 d . . . Cl1 Cl 0.63989(10) 0.44852(9) 0.06801(18) 0.0379(5) Uani 1 d . . . Cl2 Cl 0.63420(10) 0.35778(10) -0.19428(17) 0.0388(5) Uani 1 d . . . O1 O 0.5504(2) 0.3223(2) 0.0437(5) 0.0347(13) Uani 1 d . . . O2 O 0.4522(3) 0.3986(3) 0.1755(5) 0.0425(14) Uani 1 d . . . O3 O 0.5342(3) 0.4548(3) 0.3754(5) 0.0443(15) Uani 1 d . . . O4 O 0.6470(3) 0.3796(3) 0.4513(5) 0.0470(15) Uani 1 d . . . O5 O 0.6462(2) 0.3117(2) 0.2020(5) 0.0344(13) Uani 1 d . . . O6 O 0.7411(2) 0.3432(2) 0.0159(4) 0.0325(12) Uani 1 d . . . C1 C 0.4922(4) 0.3496(4) -0.0131(8) 0.041(2) Uani 1 d . . . H1A H 0.4562 0.3171 -0.0079 0.037(5) Uiso 1 calc R . . H1B H 0.5012 0.3580 -0.1024 0.037(5) Uiso 1 calc R . . C2 C 0.4704(4) 0.4121(4) 0.0468(8) 0.043(2) Uani 1 d . . . H2A H 0.5064 0.4448 0.0444 0.037(5) Uiso 1 calc R . . H2B H 0.4323 0.4304 0.0013 0.037(5) Uiso 1 calc R . . C3 C 0.4388(4) 0.4566(4) 0.2446(8) 0.046(2) Uani 1 d . . . H3A H 0.4132 0.4448 0.3196 0.037(5) Uiso 1 calc R . . H3B H 0.4114 0.4863 0.1932 0.037(5) Uiso 1 calc R . . C4 C 0.4992(4) 0.4926(4) 0.2838(8) 0.044(2) Uani 1 d . . . H4A H 0.5278 0.5003 0.2106 0.037(5) Uiso 1 calc R . . H4B H 0.4870 0.5358 0.3192 0.037(5) Uiso 1 calc R . . C5 C 0.5954(4) 0.4855(4) 0.4062(8) 0.046(2) Uani 1 d . . . H5A H 0.5870 0.5293 0.4431 0.037(5) Uiso 1 calc R . . H5B H 0.6219 0.4916 0.3298 0.037(5) Uiso 1 calc R . . C6 C 0.6325(4) 0.4436(4) 0.4974(8) 0.045(2) Uani 1 d . . . H6A H 0.6742 0.4659 0.5191 0.037(5) Uiso 1 calc R . . H6B H 0.6063 0.4394 0.5746 0.037(5) Uiso 1 calc R . . C7 C 0.7011(4) 0.3796(4) 0.3643(7) 0.042(2) Uani 1 d . . . H7A H 0.7433 0.3841 0.4093 0.037(5) Uiso 1 calc R . . H7B H 0.6968 0.4169 0.3055 0.037(5) Uiso 1 calc R . . C8 C 0.6989(4) 0.3141(4) 0.2935(7) 0.040(2) Uani 1 d . . . H8A H 0.7415 0.3073 0.2507 0.037(5) Uiso 1 calc R . . H8B H 0.6930 0.2779 0.3539 0.037(5) Uiso 1 calc R . . C9 C 0.5806(4) 0.3055(4) 0.2533(7) 0.037(2) Uani 1 d . . . H9A H 0.5646 0.3487 0.2828 0.037(5) Uiso 1 calc R . . H9B H 0.5807 0.2746 0.3245 0.037(5) Uiso 1 calc R . . C10 C 0.5377(4) 0.2803(4) 0.1519(8) 0.039(2) Uani 1 d . . . H10A H 0.5485 0.2339 0.1327 0.037(5) Uiso 1 calc R . . H10B H 0.4909 0.2829 0.1766 0.037(5) Uiso 1 calc R . . C11 C 0.7307(5) 0.5897(4) 0.3409(9) 0.052(2) Uani 1 d . . . C12 C 0.7184(5) 0.6221(5) 0.4452(11) 0.063(3) Uani 1 d . . . C13 C 0.7474(9) 0.6104(8) 0.5514(14) 0.102(5) Uani 1 d . . . C14 C 0.7927(9) 0.5665(12) 0.5583(18) 0.121(8) Uani 1 d . . . C15 C 0.8131(6) 0.5267(8) 0.457(2) 0.127(8) Uani 1 d . . . C16 C 0.7766(6) 0.5396(6) 0.3410(13) 0.083(4) Uani 1 d . . . C17 C 0.6962(9) 0.6076(7) 0.2172(14) 0.131(7) Uani 1 d . . . O7 O 0.1912(8) 0.2695(9) 0.1160(16) 0.093(5) Uiso 0.50 d P . . 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 0.0297(8) 0.0302(8) 0.0293(7) 0.0010(6) -0.0001(6) 0.0017(6) Cl1 0.0407(12) 0.0317(11) 0.0414(11) -0.0003(9) -0.0003(9) 0.0031(9) Cl2 0.0413(12) 0.0418(12) 0.0333(10) 0.0036(10) -0.0025(9) -0.0002(9) O1 0.032(3) 0.033(3) 0.040(3) 0.002(3) 0.003(2) 0.003(2) O2 0.041(3) 0.044(3) 0.042(3) -0.002(3) 0.009(3) 0.007(3) O3 0.041(3) 0.045(3) 0.048(3) -0.002(3) -0.002(3) 0.007(3) O4 0.047(4) 0.054(4) 0.040(3) -0.007(3) 0.006(3) 0.008(3) O5 0.030(3) 0.040(3) 0.033(3) 0.001(2) 0.002(3) 0.004(2) O6 0.037(3) 0.031(3) 0.030(3) 0.001(2) 0.002(2) 0.002(2) C1 0.035(5) 0.052(5) 0.037(5) 0.001(4) -0.001(4) 0.007(4) C2 0.037(5) 0.048(5) 0.045(5) 0.005(4) 0.006(4) 0.012(4) C3 0.044(5) 0.042(5) 0.050(5) 0.001(4) 0.005(4) 0.010(4) C4 0.045(5) 0.034(5) 0.052(5) -0.008(4) 0.010(4) 0.014(4) C5 0.040(5) 0.051(6) 0.048(5) 0.002(4) 0.008(4) 0.006(4) C6 0.044(5) 0.058(6) 0.034(4) -0.014(4) 0.002(4) 0.003(4) C7 0.040(5) 0.061(6) 0.025(4) -0.005(4) 0.002(4) -0.003(4) C8 0.040(5) 0.044(5) 0.035(4) 0.001(4) 0.006(4) 0.011(4) C9 0.034(4) 0.037(5) 0.039(5) 0.000(4) 0.014(4) 0.000(4) C10 0.046(5) 0.029(4) 0.044(5) 0.007(4) 0.011(4) 0.001(4) C11 0.064(6) 0.038(5) 0.054(6) 0.003(5) -0.007(5) -0.008(5) C12 0.053(6) 0.060(7) 0.075(8) -0.010(6) 0.018(6) -0.019(5) C13 0.122(13) 0.107(12) 0.076(10) 0.009(9) -0.017(10) -0.070(10) C14 0.056(10) 0.175(19) 0.132(14) 0.095(14) -0.045(10) -0.060(11) C15 0.039(7) 0.100(11) 0.24(2) 0.121(14) 0.056(11) 0.023(7) C16 0.087(9) 0.057(7) 0.104(10) 0.012(7) 0.061(8) 0.010(6) C17 0.214(18) 0.081(9) 0.097(10) 0.034(8) -0.085(12) -0.065(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O6 1.690(5) . ? Ti1 O6 2.001(5) 8_655 ? Ti1 O5 2.117(5) . ? Ti1 O1 2.244(5) . ? Ti1 Cl2 2.312(2) . ? Ti1 Cl1 2.351(2) . ? O1 C1 1.443(9) . ? O1 C10 1.466(9) . ? O2 C3 1.422(10) . ? O2 C2 1.456(10) . ? O3 C5 1.433(10) . ? O3 C4 1.438(10) . ? O4 C6 1.425(10) . ? O4 C7 1.444(10) . ? O5 C9 1.451(9) . ? O5 C8 1.455(9) . ? O6 Ti1 2.001(5) 7_665 ? C1 C2 1.494(12) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.491(12) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.503(12) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.536(12) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.488(11) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.324(14) . ? C11 C16 1.382(15) . ? C11 C17 1.546(15) . ? C12 C13 1.306(18) . ? C13 C14 1.29(2) . ? C14 C15 1.42(3) . ? C15 C16 1.47(2) . ? O7 O7 1.78(2) 4 ? O7 O7 1.78(2) 3 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Ti1 O6 94.3(3) . 8_655 ? O6 Ti1 O5 96.4(2) . . ? O6 Ti1 O5 83.9(2) 8_655 . ? O6 Ti1 O1 169.1(2) . . ? O6 Ti1 O1 82.27(19) 8_655 . ? O5 Ti1 O1 73.02(19) . . ? O6 Ti1 Cl2 102.72(18) . . ? O6 Ti1 Cl2 91.05(15) 8_655 . ? O5 Ti1 Cl2 160.55(16) . . ? O1 Ti1 Cl2 87.71(15) . . ? O6 Ti1 Cl1 95.60(18) . . ? O6 Ti1 Cl1 168.41(16) 8_655 . ? O5 Ti1 Cl1 89.06(15) . . ? O1 Ti1 Cl1 86.88(15) . . ? Cl2 Ti1 Cl1 92.58(8) . . ? C1 O1 C10 114.5(6) . . ? C1 O1 Ti1 133.1(5) . . ? C10 O1 Ti1 112.0(4) . . ? C3 O2 C2 112.7(6) . . ? C5 O3 C4 110.7(6) . . ? C6 O4 C7 112.5(6) . . ? C9 O5 C8 115.2(6) . . ? C9 O5 Ti1 119.5(4) . . ? C8 O5 Ti1 123.6(4) . . ? Ti1 O6 Ti1 169.2(3) . 7_665 ? O1 C1 C2 113.0(7) . . ? O1 C1 H1A 109.0 . . ? C2 C1 H1A 109.0 . . ? O1 C1 H1B 109.0 . . ? C2 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? O2 C2 C1 108.8(7) . . ? O2 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? O2 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? O2 C3 C4 113.4(7) . . ? O2 C3 H3A 108.9 . . ? C4 C3 H3A 108.9 . . ? O2 C3 H3B 108.9 . . ? C4 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? O3 C4 C3 109.7(7) . . ? O3 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? O3 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? O3 C5 C6 109.8(7) . . ? O3 C5 H5A 109.7 . . ? C6 C5 H5A 109.7 . . ? O3 C5 H5B 109.7 . . ? C6 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? O4 C6 C5 113.4(7) . . ? O4 C6 H6A 108.9 . . ? C5 C6 H6A 108.9 . . ? O4 C6 H6B 108.9 . . ? C5 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? O4 C7 C8 107.3(7) . . ? O4 C7 H7A 110.3 . . ? C8 C7 H7A 110.3 . . ? O4 C7 H7B 110.3 . . ? C8 C7 H7B 110.3 . . ? H7A C7 H7B 108.5 . . ? O5 C8 C7 112.6(6) . . ? O5 C8 H8A 109.1 . . ? C7 C8 H8A 109.1 . . ? O5 C8 H8B 109.1 . . ? C7 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? O5 C9 C10 107.0(6) . . ? O5 C9 H9A 110.3 . . ? C10 C9 H9A 110.3 . . ? O5 C9 H9B 110.3 . . ? C10 C9 H9B 110.3 . . ? H9A C9 H9B 108.6 . . ? O1 C10 C9 106.0(6) . . ? O1 C10 H10A 110.5 . . ? C9 C10 H10A 110.5 . . ? O1 C10 H10B 110.5 . . ? C9 C10 H10B 110.5 . . ? H10A C10 H10B 108.7 . . ? C12 C11 C16 119.7(11) . . ? C12 C11 C17 121.6(11) . . ? C16 C11 C17 118.8(12) . . ? C13 C12 C11 124.2(13) . . ? C14 C13 C12 120.1(16) . . ? C13 C14 C15 124.1(15) . . ? C14 C15 C16 113.5(11) . . ? C11 C16 C15 118.3(12) . . ? O7 O7 O7 90.000(3) 4 3 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Ti1 O1 C1 164.4(11) . . . . ? O6 Ti1 O1 C1 -123.2(6) 8_655 . . . ? O5 Ti1 O1 C1 150.9(6) . . . . ? Cl2 Ti1 O1 C1 -31.8(6) . . . . ? Cl1 Ti1 O1 C1 60.9(6) . . . . ? O6 Ti1 O1 C10 -8.6(14) . . . . ? O6 Ti1 O1 C10 63.8(4) 8_655 . . . ? O5 Ti1 O1 C10 -22.2(4) . . . . ? Cl2 Ti1 O1 C10 155.1(4) . . . . ? Cl1 Ti1 O1 C10 -112.2(4) . . . . ? O6 Ti1 O5 C9 175.5(5) . . . . ? O6 Ti1 O5 C9 -90.8(5) 8_655 . . . ? O1 Ti1 O5 C9 -7.0(5) . . . . ? Cl2 Ti1 O5 C9 -15.1(8) . . . . ? Cl1 Ti1 O5 C9 80.0(5) . . . . ? O6 Ti1 O5 C8 10.8(5) . . . . ? O6 Ti1 O5 C8 104.5(5) 8_655 . . . ? O1 Ti1 O5 C8 -171.8(5) . . . . ? Cl2 Ti1 O5 C8 -179.8(4) . . . . ? Cl1 Ti1 O5 C8 -84.7(5) . . . . ? O6 Ti1 O6 Ti1 58.5(15) 8_655 . . 7_665 ? O5 Ti1 O6 Ti1 142.9(16) . . . 7_665 ? O1 Ti1 O6 Ti1 129.8(14) . . . 7_665 ? Cl2 Ti1 O6 Ti1 -33.5(16) . . . 7_665 ? Cl1 Ti1 O6 Ti1 -127.5(16) . . . 7_665 ? C10 O1 C1 C2 85.9(8) . . . . ? Ti1 O1 C1 C2 -87.0(8) . . . . ? C3 O2 C2 C1 172.4(7) . . . . ? O1 C1 C2 O2 -63.3(9) . . . . ? C2 O2 C3 C4 -77.2(9) . . . . ? C5 O3 C4 C3 174.8(6) . . . . ? O2 C3 C4 O3 -68.4(9) . . . . ? C4 O3 C5 C6 -177.3(6) . . . . ? C7 O4 C6 C5 77.0(9) . . . . ? O3 C5 C6 O4 59.8(9) . . . . ? C6 O4 C7 C8 -163.6(6) . . . . ? C9 O5 C8 C7 -72.6(8) . . . . ? Ti1 O5 C8 C7 92.7(7) . . . . ? O4 C7 C8 O5 74.2(8) . . . . ? C8 O5 C9 C10 -160.2(6) . . . . ? Ti1 O5 C9 C10 33.8(8) . . . . ? C1 O1 C10 C9 -128.5(7) . . . . ? Ti1 O1 C10 C9 45.9(7) . . . . ? O5 C9 C10 O1 -49.6(8) . . . . ? C16 C11 C12 C13 0.4(16) . . . . ? C17 C11 C12 C13 -178.0(12) . . . . ? C11 C12 C13 C14 2.5(19) . . . . ? C12 C13 C14 C15 -2(2) . . . . ? C13 C14 C15 C16 -1(2) . . . . ? C12 C11 C16 C15 -3.5(15) . . . . ? C17 C11 C16 C15 175.0(11) . . . . ? C14 C15 C16 C11 3.7(16) . . . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 1.402 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.105