#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/1/1100935.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100935 _publ_section_title ; Titanium(IV) Citrate Speciation and Structure Under Environmentally and Biologically Relevant Conditions ; loop_ _publ_author_name 'Collins, J. M.' 'Uppal, R' 'Incarvito, C. D.' 'Valentine, A. M.' _chemical_formula_sum 'C18 H46 Na8 O38 Ti' _chemical_formula_weight 1102.37 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' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.634(2) _cell_length_b 13.223(3) _cell_length_c 13.291(3) _cell_angle_alpha 99.27(3) _cell_angle_beta 92.21(3) _cell_angle_gamma 99.95(3) _cell_volume 1982.9(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.846 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 0.430 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16679 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 28.66 _reflns_number_total 9836 _reflns_number_gt 7889 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 9836 _refine_ls_number_parameters 701 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1858 _refine_ls_wR_factor_gt 0.1748 _refine_ls_goodness_of_fit_ref 1.342 _refine_ls_restrained_S_all 1.341 _refine_ls_shift/su_max 1.258 _refine_ls_shift/su_mean 0.055 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.64581(4) 0.19287(3) 0.66419(3) 0.01312(13) Uani 1 1 d . . . O1 O 0.61682(15) 0.16471(13) 0.51165(13) 0.0167(4) Uani 1 1 d . . . O2 O 0.69536(15) 0.32515(14) 0.63458(13) 0.0168(4) Uani 1 1 d . . . O3 O 0.63402(17) 0.23328(15) 0.37234(14) 0.0226(4) Uani 1 1 d . . . O4 O 0.9103(2) 0.50630(19) 0.6478(2) 0.0508(8) Uani 1 1 d . . . O5 O 0.8564(2) 0.57073(16) 0.51652(17) 0.0321(5) Uani 1 1 d . . . O6 O 0.46190(17) 0.41610(16) 0.64284(15) 0.0259(4) Uani 1 1 d . . . O7 O 0.42277(16) 0.31810(14) 0.49177(14) 0.0208(4) Uani 1 1 d . . . O8 O 0.46476(15) 0.17245(13) 0.65512(13) 0.0148(4) Uani 1 1 d . . . O9 O 0.61669(15) 0.23188(14) 0.79811(13) 0.0161(4) Uani 1 1 d . . . O10 O 0.31277(15) 0.21222(14) 0.73794(14) 0.0184(4) Uani 1 1 d . . . O11 O 0.39159(16) 0.00328(14) 0.79334(14) 0.0201(4) Uani 1 1 d . . . O12 O 0.55594(18) 0.01049(15) 0.88735(15) 0.0259(4) Uani 1 1 d . . . O13 O 0.4790(2) 0.36268(17) 1.05472(15) 0.0309(5) Uani 1 1 d . . . O14 O 0.6571(2) 0.40940(18) 1.00478(16) 0.0338(5) Uani 1 1 d . . . O15 O 0.60765(15) 0.03122(13) 0.64114(14) 0.0172(4) Uani 1 1 d . . . O16 O 0.79369(15) 0.15954(13) 0.68038(13) 0.0150(4) Uani 1 1 d . . . O17 O 0.68628(17) -0.11198(14) 0.63425(15) 0.0220(4) Uani 1 1 d . . . O18 O 0.9240(2) 0.1936(2) 0.9073(2) 0.0335(6) Uani 0.80 1 d P A 1 O18' O 0.9774(10) 0.0708(13) 0.9150(9) 0.052(4) Uani 0.20 1 d P B 2 O19 O 1.04682(17) 0.14690(18) 0.79047(17) 0.0298(5) Uani 1 1 d . . . O20 O 0.90643(17) 0.13674(15) 0.46379(15) 0.0228(4) Uani 1 1 d . . . O21 O 0.77351(16) -0.00872(15) 0.43987(15) 0.0211(4) Uani 1 1 d . . . C1 C 0.6452(2) 0.2420(2) 0.46503(19) 0.0174(5) Uani 1 1 d . . . C2 C 0.6933(2) 0.3461(2) 0.53483(19) 0.0173(5) Uani 1 1 d . . . C3 C 0.8173(2) 0.3859(2) 0.5043(2) 0.0214(5) Uani 1 1 d . . . H3A H 0.8687 0.3394 0.5203 0.026 Uiso 1 1 calc R . . H3B H 0.8150 0.3848 0.4311 0.026 Uiso 1 1 calc R . . C4 C 0.8667(2) 0.4962(2) 0.5593(2) 0.0235(6) Uani 1 1 d . . . C5 C 0.6117(2) 0.42426(19) 0.5259(2) 0.0167(5) Uani 1 1 d . . . H5A H 0.6432 0.4896 0.5704 0.020 Uiso 1 1 calc R . . H5B H 0.6078 0.4375 0.4563 0.020 Uiso 1 1 calc R . . C6 C 0.4890(2) 0.3836(2) 0.5549(2) 0.0186(5) Uani 1 1 d . . . C7 C 0.4175(2) 0.20788(18) 0.73524(18) 0.0140(5) Uani 1 1 d . . . C8 C 0.5036(2) 0.23979(19) 0.82960(18) 0.0151(5) Uani 1 1 d . . . C9 C 0.4709(2) 0.1627(2) 0.90293(19) 0.0183(5) Uani 1 1 d . . . H9A H 0.5248 0.1828 0.9632 0.022 Uiso 1 1 calc R . . H9B H 0.3931 0.1677 0.9245 0.022 Uiso 1 1 calc R . . C10 C 0.4731(2) 0.0499(2) 0.85718(19) 0.0182(5) Uani 1 1 d . . . C11 C 0.4973(2) 0.3522(2) 0.87878(19) 0.0189(5) Uani 1 1 d . . . H11A H 0.5398 0.4002 0.8393 0.023 Uiso 1 1 calc R . . H11B H 0.4164 0.3613 0.8769 0.023 Uiso 1 1 calc R . . C12 C 0.5477(3) 0.3780(2) 0.9872(2) 0.0219(6) Uani 1 1 d . . . C13 C 0.6933(2) -0.0165(2) 0.64711(19) 0.0163(5) Uani 1 1 d . . . C14 C 0.8126(2) 0.05617(19) 0.67509(19) 0.0157(5) Uani 1 1 d . . . C15 C 0.8567(2) 0.0405(2) 0.7795(2) 0.0235(6) Uani 1 1 d . . . H15A H 0.8900 -0.0224 0.7724 0.028 Uiso 1 1 calc R C 1 H15B H 0.7918 0.0321 0.8229 0.028 Uiso 1 1 calc R C 1 C16 C 0.9518(3) 0.1360(4) 0.8309(3) 0.0222(7) Uani 0.80 1 d P A 1 C16' C 0.9646(13) 0.0797(14) 0.8225(10) 0.020(3) Uani 0.20 1 d P B 2 C17 C 0.8975(2) 0.0333(2) 0.59300(19) 0.0163(5) Uani 1 1 d . . . H17A H 0.9738 0.0760 0.6140 0.020 Uiso 1 1 calc R A . H17B H 0.9058 -0.0392 0.5860 0.020 Uiso 1 1 calc R . . C18 C 0.8556(2) 0.05501(19) 0.49130(19) 0.0162(5) Uani 1 1 d . A . Na1 Na 0.59341(9) 0.02602(8) 0.37963(8) 0.0187(2) Uani 1 1 d . . . Na2 Na 0.68444(11) 0.18367(9) 0.20307(8) 0.0257(3) Uani 1 1 d . . . O201 O 0.8648(2) 0.13845(18) 0.26630(16) 0.0321(5) Uani 1 1 d D . . H201 H 0.885(3) 0.142(3) 0.3369(7) 0.048 Uiso 1 1 d D . . H202 H 0.924(2) 0.190(2) 0.247(3) 0.048 Uiso 1 1 d D . . O202 O 0.7263(2) 0.12346(19) 0.02529(17) 0.0358(5) Uani 1 1 d D . . H203 H 0.791(2) 0.162(3) -0.002(3) 0.054 Uiso 1 1 d D . . H204 H 0.670(3) 0.109(3) -0.031(2) 0.054 Uiso 1 1 d D . . O203 O 0.7424(2) 0.36145(17) 0.18465(17) 0.0332(5) Uani 1 1 d D . . H205 H 0.709(3) 0.375(3) 0.1227(17) 0.050 Uiso 1 1 d D . . H206 H 0.727(3) 0.417(2) 0.234(2) 0.050 Uiso 1 1 d D . . O204 O 0.4820(2) 0.19418(16) 0.17002(15) 0.0279(5) Uani 1 1 d D . . H207 H 0.449(3) 0.1225(8) 0.150(3) 0.042 Uiso 1 1 d D . . H208 H 0.433(3) 0.235(2) 0.143(3) 0.042 Uiso 1 1 d D . . Na3 Na 0.42911(11) 0.26374(9) 0.32372(8) 0.0271(3) Uani 1 1 d . . . O301 O 0.4190(2) 0.41153(18) 0.24796(17) 0.0389(6) Uani 1 1 d D . . H301 H 0.471(3) 0.467(2) 0.289(3) 0.058 Uiso 1 1 d D . . H302 H 0.443(4) 0.387(3) 0.1822(14) 0.058 Uiso 1 1 d D . . O302 O 0.1827(4) 0.2678(3) 0.3180(2) 0.0669(10) Uani 1 1 d D . . H303 H 0.179(5) 0.320(3) 0.375(3) 0.100 Uiso 1 1 d D . . H304 H 0.1029(15) 0.269(5) 0.301(5) 0.100 Uiso 1 1 d D . . Na4 Na 0.29758(9) 0.18417(8) 0.54334(8) 0.0186(2) Uani 1 1 d . . . O401 O 0.11750(17) 0.23970(15) 0.55092(16) 0.0232(4) Uani 1 1 d D . . H401 H 0.0417(14) 0.204(2) 0.525(3) 0.035 Uiso 1 1 d D . . H402 H 0.121(3) 0.3043(13) 0.527(3) 0.035 Uiso 1 1 d D . . Na5 Na 0.14807(9) 0.30208(8) 0.74140(8) 0.0219(2) Uani 1 1 d . . . O501 O 0.1839(2) 0.40121(19) 0.90673(18) 0.0366(5) Uani 1 1 d D . . H501 H 0.241(3) 0.459(2) 0.940(3) 0.055 Uiso 1 1 d D . . H502 H 0.214(3) 0.362(3) 0.952(3) 0.055 Uiso 1 1 d D . . O502 O -0.03771(18) 0.34410(17) 0.72872(17) 0.0300(5) Uani 1 1 d D . . H503 H -0.090(3) 0.2812(16) 0.701(3) 0.045 Uiso 1 1 d D . . H504 H -0.061(3) 0.394(2) 0.692(3) 0.045 Uiso 1 1 d D . . O503 O 0.24577(17) 0.45325(16) 0.67910(15) 0.0245(4) Uani 1 1 d D . . H505 H 0.3273(7) 0.454(3) 0.676(3) 0.037 Uiso 1 1 d D . . H506 H 0.202(3) 0.456(3) 0.6183(15) 0.037 Uiso 1 1 d D . . Na6 Na 0.19551(10) 0.04728(9) 0.76925(10) 0.0292(3) Uani 1 1 d . . . O601 O 0.1887(3) 0.0550(3) 0.9487(2) 0.0627(9) Uani 1 1 d D . . H601 H 0.227(4) 0.001(3) 0.965(4) 0.094 Uiso 1 1 d D . . H602 H 0.117(3) 0.050(4) 0.982(4) 0.094 Uiso 1 1 d D . . Na7 Na 0.82373(15) 0.36216(15) 0.88873(14) 0.0288(4) Uani 0.65 1 d P D 1 Na7' Na 0.7881(4) 0.4489(4) 0.8500(4) 0.0518(11) Uani 0.35 1 d P E 2 O70A O 0.9652(3) 0.3858(3) 0.8987(2) 0.0277(7) Uani 0.65 1 d P F 1 O70B O 1.0138(5) 0.5151(5) 0.9428(5) 0.0307(13) Uani 0.35 1 d P . 2 O702 O 0.7739(4) 0.5225(5) 0.8013(4) 0.1088(15) Uani 1 1 d . . . O703 O 0.945(3) 0.297(3) 1.011(3) 0.77(2) Uiso 1 1 d . . . Na8 Na 0.8650(2) 0.7031(2) 0.8353(2) 0.0411(6) Uani 0.50 1 d P G 1 Na8' Na 0.8072(3) 0.6172(3) 0.7965(2) 0.0526(8) Uani 0.50 1 d P H 2 O801 O 1.0324(3) 0.6531(3) 0.7881(3) 0.0858(12) Uani 1 1 d . . . O802 O 0.9720(5) 0.8570(4) 0.9273(4) 0.1235(18) Uani 1 1 d . . . O803 O 0.7523(3) 0.7185(3) 0.9581(2) 0.0548(7) Uani 1 1 d D . . H805 H 0.770(5) 0.7907(9) 0.954(4) 0.082 Uiso 1 1 d D . . H806 H 0.6729(14) 0.702(4) 0.974(4) 0.082 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0124(2) 0.0126(2) 0.0143(2) 0.00173(16) 0.00027(15) 0.00268(16) O1 0.0203(9) 0.0140(8) 0.0152(8) 0.0014(7) 0.0010(7) 0.0025(7) O2 0.0181(9) 0.0159(9) 0.0158(8) 0.0032(7) 0.0007(6) 0.0013(7) O3 0.0284(10) 0.0240(10) 0.0157(9) 0.0031(8) 0.0032(7) 0.0054(8) O4 0.0637(17) 0.0295(13) 0.0499(16) 0.0162(11) -0.0356(13) -0.0177(12) O5 0.0422(13) 0.0207(10) 0.0331(12) 0.0099(9) -0.0031(9) 0.0014(9) O6 0.0264(10) 0.0309(11) 0.0206(10) 0.0010(8) 0.0062(8) 0.0080(8) O7 0.0216(9) 0.0184(9) 0.0209(9) 0.0027(7) 0.0000(7) 0.0001(7) O8 0.0147(8) 0.0177(9) 0.0122(8) 0.0007(7) 0.0013(6) 0.0047(7) O9 0.0160(9) 0.0198(9) 0.0127(8) 0.0015(7) 0.0011(6) 0.0049(7) O10 0.0152(9) 0.0204(9) 0.0207(9) 0.0022(7) 0.0034(7) 0.0070(7) O11 0.0243(10) 0.0187(9) 0.0163(9) 0.0014(7) -0.0002(7) 0.0029(7) O12 0.0292(11) 0.0194(10) 0.0287(11) 0.0010(8) -0.0082(8) 0.0080(8) O13 0.0441(13) 0.0319(11) 0.0163(10) 0.0011(8) 0.0062(9) 0.0079(10) O14 0.0369(12) 0.0330(12) 0.0250(11) -0.0002(9) -0.0073(9) -0.0053(10) O15 0.0135(8) 0.0129(8) 0.0245(9) 0.0029(7) 0.0006(7) 0.0012(7) O16 0.0139(8) 0.0123(8) 0.0187(9) 0.0012(7) 0.0001(6) 0.0037(7) O17 0.0238(10) 0.0142(9) 0.0285(10) 0.0050(8) 0.0049(8) 0.0028(7) O18 0.0314(15) 0.0386(16) 0.0270(14) -0.0035(12) 0.0017(11) 0.0050(12) O18' 0.025(6) 0.103(12) 0.021(6) 0.017(6) -0.001(4) -0.010(7) O19 0.0178(10) 0.0396(12) 0.0351(11) 0.0167(10) 0.0003(8) 0.0044(9) O20 0.0226(10) 0.0217(10) 0.0216(9) 0.0058(8) -0.0038(7) -0.0038(8) O21 0.0186(9) 0.0173(9) 0.0266(10) 0.0042(8) -0.0041(7) 0.0019(7) C1 0.0173(12) 0.0181(12) 0.0174(12) 0.0031(10) 0.0015(9) 0.0051(10) C2 0.0195(12) 0.0152(12) 0.0175(12) 0.0059(10) 0.0009(9) 0.0017(10) C3 0.0190(13) 0.0212(13) 0.0260(14) 0.0066(11) 0.0060(10) 0.0053(10) C4 0.0189(13) 0.0225(14) 0.0293(14) 0.0089(11) 0.0026(11) -0.0002(11) C5 0.0174(12) 0.0148(12) 0.0185(12) 0.0044(10) 0.0019(9) 0.0027(9) C6 0.0212(13) 0.0168(12) 0.0212(13) 0.0064(10) 0.0023(10) 0.0094(10) C7 0.0158(11) 0.0114(11) 0.0152(11) 0.0024(9) 0.0008(9) 0.0034(9) C8 0.0152(11) 0.0163(12) 0.0137(11) 0.0008(9) 0.0020(9) 0.0041(9) C9 0.0232(13) 0.0181(12) 0.0135(11) 0.0032(9) 0.0024(9) 0.0027(10) C10 0.0220(13) 0.0176(12) 0.0152(11) 0.0035(9) 0.0037(9) 0.0031(10) C11 0.0252(13) 0.0156(12) 0.0162(12) 0.0020(10) 0.0006(10) 0.0057(10) C12 0.0358(16) 0.0125(12) 0.0165(12) -0.0019(10) -0.0002(11) 0.0065(11) C13 0.0166(12) 0.0184(12) 0.0158(12) 0.0047(10) 0.0053(9) 0.0053(10) C14 0.0148(11) 0.0145(11) 0.0198(12) 0.0059(9) 0.0014(9) 0.0054(9) C15 0.0211(13) 0.0302(15) 0.0220(13) 0.0108(11) 0.0045(10) 0.0058(11) C16 0.0196(17) 0.027(2) 0.0205(18) 0.0048(17) -0.0039(13) 0.0057(16) C16' 0.023(7) 0.025(8) 0.011(6) 0.001(6) -0.002(5) 0.003(6) C17 0.0131(11) 0.0171(12) 0.0206(12) 0.0065(10) 0.0028(9) 0.0047(9) C18 0.0140(11) 0.0160(12) 0.0194(12) 0.0032(10) 0.0029(9) 0.0041(9) Na1 0.0165(5) 0.0194(5) 0.0180(5) -0.0025(4) -0.0009(4) 0.0029(4) Na2 0.0340(6) 0.0215(6) 0.0214(6) 0.0047(4) 0.0003(5) 0.0044(5) O201 0.0323(12) 0.0383(13) 0.0247(11) 0.0092(10) -0.0004(9) 0.0006(10) O202 0.0359(13) 0.0412(13) 0.0254(11) 0.0029(10) -0.0050(9) -0.0024(10) O203 0.0503(14) 0.0241(11) 0.0234(11) 0.0044(9) -0.0080(9) 0.0037(10) O204 0.0449(13) 0.0201(10) 0.0198(10) 0.0031(8) -0.0009(9) 0.0101(9) Na3 0.0396(7) 0.0227(6) 0.0174(5) 0.0048(4) 0.0027(5) 0.0001(5) O301 0.0698(17) 0.0258(12) 0.0214(11) 0.0000(9) 0.0055(11) 0.0135(11) O302 0.127(3) 0.0534(18) 0.0379(16) 0.0209(14) 0.0224(18) 0.048(2) Na4 0.0188(5) 0.0192(5) 0.0173(5) 0.0037(4) -0.0011(4) 0.0019(4) O401 0.0204(10) 0.0187(9) 0.0298(11) 0.0053(8) -0.0033(8) 0.0017(8) Na5 0.0197(5) 0.0206(5) 0.0255(6) 0.0029(4) -0.0001(4) 0.0054(4) O501 0.0448(14) 0.0330(13) 0.0303(12) 0.0022(10) 0.0040(10) 0.0052(10) O502 0.0241(10) 0.0255(11) 0.0390(12) 0.0030(9) -0.0099(9) 0.0054(8) O503 0.0233(10) 0.0266(10) 0.0218(10) 0.0027(8) 0.0017(8) 0.0012(8) Na6 0.0284(6) 0.0248(6) 0.0368(7) 0.0063(5) 0.0032(5) 0.0099(5) O601 0.0619(19) 0.096(2) 0.0492(17) 0.0270(17) 0.0162(14) 0.0504(18) Na7 0.0213(8) 0.0359(10) 0.0262(9) -0.0004(8) 0.0070(7) 0.0015(7) Na7' 0.049(3) 0.056(3) 0.048(3) 0.006(2) 0.003(2) 0.007(2) O70A 0.0221(15) 0.046(2) 0.0139(14) -0.0055(13) 0.0005(11) 0.0136(14) O70B 0.030(3) 0.037(3) 0.027(3) -0.002(3) -0.003(2) 0.016(3) O702 0.101(3) 0.139(5) 0.095(3) 0.022(3) 0.025(3) 0.041(3) Na8 0.0367(15) 0.0514(18) 0.0377(15) 0.0126(13) 0.0048(11) 0.0102(13) Na8' 0.086(3) 0.0424(18) 0.0370(16) 0.0139(14) 0.0183(16) 0.0221(18) O801 0.055(2) 0.107(3) 0.086(3) 0.002(2) -0.0044(18) 0.007(2) O802 0.142(5) 0.133(4) 0.099(4) 0.018(3) -0.012(3) 0.040(4) O803 0.0436(16) 0.0642(19) 0.0577(17) 0.0193(15) -0.0061(13) 0.0071(15) _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 O9 1.8330(18) . ? Ti1 O2 1.8542(18) . ? Ti1 O16 1.8613(18) . ? Ti1 O1 2.0058(18) . ? Ti1 O8 2.0730(18) . ? Ti1 O15 2.0762(18) . ? O1 C1 1.281(3) . ? O2 C2 1.397(3) . ? O3 C1 1.218(3) . ? O4 C4 1.240(4) . ? O5 C4 1.235(3) . ? O6 C6 1.250(3) . ? O7 C6 1.238(3) . ? O8 C7 1.276(3) . ? O9 C8 1.412(3) . ? O10 C7 1.231(3) . ? O11 C10 1.252(3) . ? O12 C10 1.254(3) . ? O13 C12 1.241(4) . ? O14 C12 1.269(4) . ? O15 C13 1.275(3) . ? O16 C14 1.413(3) . ? O17 C13 1.234(3) . ? O18 C16 1.256(5) . ? O18 O703 1.75(3) . ? O18' C16' 1.260(18) . ? O19 C16 1.244(4) . ? O19 C16' 1.321(15) . ? O20 C18 1.255(3) . ? O21 C18 1.256(3) . ? C1 C2 1.533(4) . ? C2 C5 1.535(4) . ? C2 C3 1.540(4) . ? C3 C4 1.526(4) . ? C5 C6 1.523(4) . ? C7 C8 1.530(3) . ? C8 C9 1.532(3) . ? C8 C11 1.539(3) . ? C9 C10 1.522(4) . ? C11 C12 1.498(4) . ? C13 C14 1.540(4) . ? C14 C15 1.519(4) . ? C14 C17 1.529(3) . ? C15 C16' 1.339(14) . ? C15 C16 1.570(5) . ? C17 C18 1.507(3) . ? O70B O70B 1.664(13) 2_767 ? 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 O9 Ti1 O2 97.71(9) . . ? O9 Ti1 O16 100.35(8) . . ? O2 Ti1 O16 96.78(8) . . ? O9 Ti1 O1 157.88(8) . . ? O2 Ti1 O1 79.49(8) . . ? O16 Ti1 O1 101.77(8) . . ? O9 Ti1 O8 78.43(8) . . ? O2 Ti1 O8 104.89(8) . . ? O16 Ti1 O8 158.28(8) . . ? O1 Ti1 O8 81.11(8) . . ? O9 Ti1 O15 103.96(8) . . ? O2 Ti1 O15 158.29(8) . . ? O16 Ti1 O15 78.20(8) . . ? O1 Ti1 O15 80.90(8) . . ? O8 Ti1 O15 81.06(8) . . ? C1 O1 Ti1 116.83(16) . . ? C2 O2 Ti1 122.49(16) . . ? C7 O8 Ti1 116.66(15) . . ? C8 O9 Ti1 122.71(15) . . ? C13 O15 Ti1 117.21(16) . . ? C14 O16 Ti1 123.07(15) . . ? C16 O18 O703 156.2(12) . . ? C16 O19 C16' 35.0(7) . . ? O3 C1 O1 122.4(2) . . ? O3 C1 C2 122.7(2) . . ? O1 C1 C2 114.9(2) . . ? O2 C2 C1 106.3(2) . . ? O2 C2 C5 108.8(2) . . ? C1 C2 C5 110.3(2) . . ? O2 C2 C3 111.4(2) . . ? C1 C2 C3 108.0(2) . . ? C5 C2 C3 111.8(2) . . ? C4 C3 C2 112.2(2) . . ? O5 C4 O4 123.3(3) . . ? O5 C4 C3 119.2(3) . . ? O4 C4 C3 117.4(3) . . ? C6 C5 C2 111.5(2) . . ? O7 C6 O6 123.5(3) . . ? O7 C6 C5 118.6(2) . . ? O6 C6 C5 117.8(2) . . ? O10 C7 O8 123.9(2) . . ? O10 C7 C8 123.1(2) . . ? O8 C7 C8 112.9(2) . . ? O9 C8 C7 108.16(19) . . ? O9 C8 C9 108.4(2) . . ? C7 C8 C9 108.3(2) . . ? O9 C8 C11 111.2(2) . . ? C7 C8 C11 108.7(2) . . ? C9 C8 C11 111.9(2) . . ? C10 C9 C8 114.0(2) . . ? O11 C10 O12 125.0(2) . . ? O11 C10 C9 117.7(2) . . ? O12 C10 C9 117.3(2) . . ? C12 C11 C8 112.1(2) . . ? O13 C12 O14 123.9(3) . . ? O13 C12 C11 117.0(3) . . ? O14 C12 C11 119.0(3) . . ? O17 C13 O15 125.5(2) . . ? O17 C13 C14 120.4(2) . . ? O15 C13 C14 114.0(2) . . ? O16 C14 C15 109.6(2) . . ? O16 C14 C17 109.5(2) . . ? C15 C14 C17 112.3(2) . . ? O16 C14 C13 107.35(19) . . ? C15 C14 C13 107.7(2) . . ? C17 C14 C13 110.2(2) . . ? C16' C15 C14 124.5(7) . . ? C16' C15 C16 29.5(7) . . ? C14 C15 C16 110.9(2) . . ? O19 C16 O18 126.9(4) . . ? O19 C16 C15 116.0(3) . . ? O18 C16 C15 117.0(3) . . ? O18' C16' O19 115.5(12) . . ? O18' C16' C15 114.0(12) . . ? O19 C16' C15 128.2(11) . . ? C18 C17 C14 111.6(2) . . ? O20 C18 O21 124.4(2) . . ? O20 C18 C17 116.9(2) . . ? O21 C18 C17 118.7(2) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 28.66 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 1.376 _refine_diff_density_min -0.810 _refine_diff_density_rms 0.102