# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1420 data_global _publ_contact_author ; Dr P.Hubert Mutin Chimie Mol\'eculaire et Organisation du Solide UMR CNRS 5637 Universit\'e de Montpellier II, cc 007 34095 Montpellier Cedex 5 France ; _publ_contact_author_phone '(33) 0467143972' _publ_contact_author_fax '(33) 04671438532' _publ_contact_author_email mutin@cri.univ-montp2.fr _publ_requested_coeditor_name 'Graham Mc Cann' _publ_requested_journal 'J.C.S. Dalton Trans.' _publ_section_title ; Synthesis and X-ray molecular structure of novel soluble phosphonato- and phosphinato-bridged titanium oxo alkoxides. ; loop_ _publ_author_name _publ_author_address 'Gilles Guerrero' ; Chimie Mol\'eculaire et Organisation du Solide UMR CNRS 5637 Universit\'e de Montpellier II, cc 007 34095 Montpellier Cedex 5 France ; 'Michael Mehring' ; Chimie Mol\'eculaire et Organisation du Solide UMR CNRS 5637 Universit\'e de Montpellier II, cc 007 34095 Montpellier Cedex 5 France ; 'P.Hubert Mutin,' ; Chimie Mol\'eculaire et Organisation du Solide UMR CNRS 5637 Universit\'e de Montpellier II, cc 007 34095 Montpellier Cedex 5 France ; 'Fran\,coise Dahan' ; Laboratoire de Chimie de Coordination du CNRS UPR CNRS 8241 205 Route de Narbonne 31077 Toulouse Cedex 4 France ; 'Andr\'e Vioux' ; Chimie Mol\'eculaire et Organisation du Solide UMR CNRS 5637 Universit\'e de Montpellier II, cc 007 34095 Montpellier Cedex 5 France ; data_(1) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H77 O19 P3 S Ti4' _chemical_formula_weight 1226.63 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 11.6668(13) _cell_length_b 13.9198(12) _cell_length_c 35.885(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.533(15) _cell_angle_gamma 90.00 _cell_volume 5827.5(10) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'Plate' _exptl_crystal_colour 'Colourless' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2568 _exptl_absorpt_coefficient_mu 0.712 _exptl_absorpt_correction_type 'Numerical' _exptl_absorpt_process_details 'X-SHAPE (Stoe & Cie, 1996)' _exptl_absorpt_correction_T_min 0.4166 _exptl_absorpt_correction_T_max 0.6322 _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 'STOE-IPDS' _diffrn_measurement_method 'Imaging Plate Detector System' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27893 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 20.93 _reflns_number_total 5980 _reflns_number_gt 4478 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE-IPDS software (Stoe, 2.87, 1997)' _computing_cell_refinement 'STOE-IPDS software (Stoe, 2.87, 1997)' _computing_data_reduction 'XRED (Stoe, 1.08, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP (Zsolnai, 1996)' _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 w=1/[\s^2^(Fo^2^)+(0.0259P)^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 5980 _refine_ls_number_parameters 640 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0549 _refine_ls_wR_factor_gt 0.0526 _refine_ls_goodness_of_fit_ref 0.892 _refine_ls_restrained_S_all 0.892 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.59578(4) 0.19188(3) 0.106137(13) 0.01753(14) Uani 1 d . . . Ti2 Ti 0.65721(4) 0.40851(3) 0.103172(13) 0.01633(13) Uani 1 d . . . Ti3 Ti 0.82675(4) 0.25686(3) 0.071619(13) 0.01860(14) Uani 1 d . . . Ti4 Ti 0.87719(4) 0.26562(3) 0.206118(13) 0.01593(13) Uani 1 d . . . O1 O 0.55042(15) 0.22721(12) 0.15657(5) 0.0180(4) Uani 1 d . . . P1 P 0.59481(6) 0.31388(5) 0.179147(19) 0.01592(18) Uani 1 d . . . C1 C 0.4892(2) 0.33345(19) 0.21460(7) 0.0196(7) Uani 1 d . . . C2 C 0.3960(2) 0.3942(2) 0.20966(8) 0.0245(7) Uani 1 d . . . H2 H 0.3862 0.4274 0.1867 0.027 Uiso 1 calc R . . C3 C 0.3177(3) 0.4065(2) 0.23760(8) 0.0289(8) Uani 1 d . . . H3 H 0.2537 0.4477 0.2337 0.032 Uiso 1 calc R . . C4 C 0.3312(3) 0.3601(2) 0.27092(9) 0.0369(9) Uani 1 d . . . H4 H 0.2776 0.3702 0.2903 0.041 Uiso 1 calc R . . C5 C 0.4223(3) 0.2986(2) 0.27647(9) 0.0365(9) Uani 1 d . . . H5 H 0.4310 0.2654 0.2995 0.040 Uiso 1 calc R . . C6 C 0.5005(3) 0.2855(2) 0.24855(8) 0.0261(7) Uani 1 d . . . H6 H 0.5634 0.2432 0.2524 0.029 Uiso 1 calc R . . O2 O 0.69333(15) 0.09160(12) 0.12702(5) 0.0189(4) Uani 1 d . . . P2 P 0.82334(6) 0.10036(5) 0.13456(2) 0.01941(19) Uani 1 d . . . C7 C 0.8707(3) -0.0226(2) 0.13552(8) 0.0243(7) Uani 1 d . . . C8 C 0.9747(3) -0.0506(2) 0.12171(9) 0.0404(9) Uani 1 d . . . H8 H 1.0259 -0.0037 0.1122 0.044 Uiso 1 calc R . . C9 C 1.0062(3) -0.1472(3) 0.12146(9) 0.0468(10) Uani 1 d . . . H9 H 1.0779 -0.1659 0.1115 0.051 Uiso 1 calc R . . C10 C 0.9343(3) -0.2147(2) 0.13553(9) 0.0405(9) Uani 1 d . . . H10 H 0.9561 -0.2805 0.1355 0.045 Uiso 1 calc R . . C11 C 0.8305(3) -0.1878(2) 0.14976(9) 0.0379(9) Uani 1 d . . . H11 H 0.7803 -0.2349 0.1596 0.042 Uiso 1 calc R . . C12 C 0.7991(3) -0.0930(2) 0.14973(9) 0.0341(8) Uani 1 d . . . H12 H 0.7269 -0.0751 0.1596 0.038 Uiso 1 calc R . . O3 O 0.90926(15) 0.35335(12) 0.16497(5) 0.0205(5) Uani 1 d . . . P3 P 0.91324(6) 0.40789(5) 0.128756(19) 0.01616(18) Uani 1 d . . . C13 C 1.0280(2) 0.49325(19) 0.13355(7) 0.0192(7) Uani 1 d . . . C14 C 1.0784(3) 0.5090(2) 0.16831(9) 0.0334(8) Uani 1 d . . . H14 H 1.0544 0.4725 0.1892 0.037 Uiso 1 calc R . . C15 C 1.1629(3) 0.5773(2) 0.17247(10) 0.0410(9) Uani 1 d . . . H15 H 1.1959 0.5882 0.1964 0.045 Uiso 1 calc R . . C16 C 1.2003(3) 0.6297(2) 0.14262(9) 0.0332(8) Uani 1 d . . . H16 H 1.2586 0.6766 0.1460 0.036 Uiso 1 calc R . . C17 C 1.1536(3) 0.6146(2) 0.10797(9) 0.0344(8) Uani 1 d . . . H17 H 1.1797 0.6505 0.0872 0.038 Uiso 1 calc R . . C18 C 1.0680(3) 0.5463(2) 0.10348(8) 0.0292(8) Uani 1 d . . . H18 H 1.0360 0.5355 0.0794 0.032 Uiso 1 calc R . . O4 O 0.82130(16) 0.17680(13) 0.24806(5) 0.0255(5) Uani 1 d . . . S1 S 0.75137(6) 0.08479(5) 0.24442(2) 0.02298(19) Uani 1 d . . . C19 C 0.7092(3) 0.0624(2) 0.29111(8) 0.0387(9) Uani 1 d . . . H19A H 0.6510 0.1094 0.2984 0.043 Uiso 1 calc R . . H19B H 0.7761 0.0680 0.3077 0.043 Uiso 1 calc R . . H19C H 0.6773 -0.0025 0.2929 0.043 Uiso 1 calc R . . C20 C 0.8523(3) -0.0090(2) 0.24092(10) 0.0459(9) Uani 1 d . . . H20A H 0.8859 -0.0086 0.2160 0.051 Uiso 1 calc R . . H20B H 0.8141 -0.0707 0.2452 0.051 Uiso 1 calc R . . H20C H 0.9129 0.0001 0.2597 0.051 Uiso 1 calc R . . O5 O 0.72425(15) 0.28284(11) 0.11300(5) 0.0155(4) Uani 1 d . . . O6 O 0.53063(15) 0.31677(12) 0.08710(5) 0.0197(4) Uani 1 d . . . C21 C 0.4145(2) 0.3311(2) 0.07418(8) 0.0252(7) Uani 1 d . . . H21 H 0.3796 0.2667 0.0694 0.028 Uiso 1 calc R . . C22 C 0.4146(3) 0.3859(2) 0.03823(9) 0.0421(9) Uani 1 d . . . H22A H 0.4601 0.3511 0.0198 0.046 Uiso 1 calc R . . H22B H 0.4480 0.4497 0.0424 0.046 Uiso 1 calc R . . H22C H 0.3357 0.3928 0.0290 0.046 Uiso 1 calc R . . C23 C 0.3444(3) 0.3812(2) 0.10372(9) 0.0413(9) Uani 1 d . . . H23A H 0.3459 0.3430 0.1267 0.045 Uiso 1 calc R . . H23B H 0.2650 0.3880 0.0949 0.045 Uiso 1 calc R . . H23C H 0.3768 0.4449 0.1087 0.045 Uiso 1 calc R . . O7 O 0.68661(15) 0.17899(12) 0.05796(5) 0.0209(5) Uani 1 d . . . C24 C 0.6762(3) 0.1139(2) 0.02696(8) 0.0288(8) Uani 1 d . . . H24 H 0.7335 0.1339 0.0079 0.032 Uiso 1 calc R . . C25 C 0.7050(3) 0.0130(2) 0.03861(9) 0.0434(9) Uani 1 d . . . H25A H 0.7819 0.0116 0.0498 0.048 Uiso 1 calc R . . H25B H 0.7030 -0.0292 0.0167 0.048 Uiso 1 calc R . . H25C H 0.6489 -0.0094 0.0568 0.048 Uiso 1 calc R . . C26 C 0.5591(3) 0.1230(2) 0.00943(9) 0.0435(9) Uani 1 d . . . H26A H 0.5457 0.1899 0.0022 0.048 Uiso 1 calc R . . H26B H 0.5009 0.1031 0.0274 0.048 Uiso 1 calc R . . H26C H 0.5543 0.0818 -0.0127 0.048 Uiso 1 calc R . . O8 O 0.47600(15) 0.11589(12) 0.09695(5) 0.0220(5) Uani 1 d . . . C27 C 0.3937(3) 0.0472(2) 0.10920(10) 0.0396(9) Uani 1 d . . . H27 H 0.3678 0.0666 0.1346 0.044 Uiso 1 calc R . . C28 C 0.4463(3) -0.0493(2) 0.11202(10) 0.0516(10) Uani 1 d . . . H28A H 0.5113 -0.0471 0.1295 0.057 Uiso 1 calc R . . H28B H 0.4731 -0.0694 0.0874 0.057 Uiso 1 calc R . . H28C H 0.3893 -0.0953 0.1210 0.057 Uiso 1 calc R . . C29 C 0.2908(3) 0.0507(2) 0.08307(10) 0.0448(9) Uani 1 d . . . H29A H 0.2597 0.1161 0.0825 0.049 Uiso 1 calc R . . H29B H 0.2319 0.0062 0.0919 0.049 Uiso 1 calc R . . H29C H 0.3143 0.0320 0.0579 0.049 Uiso 1 calc R . . O9 O 0.59605(15) 0.40408(12) 0.15435(5) 0.0174(4) Uani 1 d . . . O10 O 0.59715(15) 0.51952(12) 0.08874(5) 0.0218(5) Uani 1 d . . . C30 C 0.5675(3) 0.6161(2) 0.08371(11) 0.0501(10) Uani 1 d . . . H30 H 0.5066 0.6183 0.0639 0.055 Uiso 1 calc R . . C31 C 0.5156(3) 0.6540(3) 0.11867(11) 0.0594(11) Uani 1 d . . . H31A H 0.4508 0.6133 0.1258 0.065 Uiso 1 calc R . . H31B H 0.4885 0.7198 0.1145 0.065 Uiso 1 calc R . . H31C H 0.5732 0.6538 0.1387 0.065 Uiso 1 calc R . . C32 C 0.6636(4) 0.6750(3) 0.07055(10) 0.0564(11) Uani 1 d . . . H32A H 0.6895 0.6506 0.0464 0.062 Uiso 1 calc R . . H32B H 0.7268 0.6718 0.0887 0.062 Uiso 1 calc R . . H32C H 0.6384 0.7418 0.0678 0.062 Uiso 1 calc R . . O11 O 0.80318(15) 0.46577(12) 0.12122(5) 0.0180(4) Uani 1 d . . . O12 O 0.73881(15) 0.37598(12) 0.05521(5) 0.0203(5) Uani 1 d . . . C33 C 0.7425(3) 0.4322(2) 0.02182(8) 0.0271(8) Uani 1 d . . . H33 H 0.6807 0.4818 0.0232 0.030 Uiso 1 calc R . . C34 C 0.7178(3) 0.3693(3) -0.01169(8) 0.0452(10) Uani 1 d . . . H34A H 0.6433 0.3378 -0.0087 0.050 Uiso 1 calc R . . H34B H 0.7778 0.3204 -0.0138 0.050 Uiso 1 calc R . . H34C H 0.7162 0.4089 -0.0343 0.050 Uiso 1 calc R . . C35 C 0.8555(3) 0.4836(3) 0.01885(10) 0.0515(10) Uani 1 d . . . H35A H 0.8677 0.5236 0.0410 0.057 Uiso 1 calc R . . H35B H 0.8550 0.5243 -0.0034 0.057 Uiso 1 calc R . . H35C H 0.9175 0.4363 0.0170 0.057 Uiso 1 calc R . . O13 O 0.94020(15) 0.34427(12) 0.09516(5) 0.0195(4) Uani 1 d . . . O14 O 0.91015(16) 0.23118(13) 0.03188(5) 0.0262(5) Uani 1 d . . . C36 C 1.0065(3) 0.1850(3) 0.01595(10) 0.0511(10) Uani 1 d . . . H36 H 1.0147 0.1208 0.0282 0.056 Uiso 1 calc R . . C37 C 1.1125(3) 0.2420(3) 0.02504(11) 0.0608(11) Uani 1 d . . . H37A H 1.1209 0.2478 0.0521 0.067 Uiso 1 calc R . . H37B H 1.1061 0.3061 0.0140 0.067 Uiso 1 calc R . . H37C H 1.1797 0.2091 0.0149 0.067 Uiso 1 calc R . . C38 C 0.9888(4) 0.1685(3) -0.02435(10) 0.0649(12) Uani 1 d . . . H38A H 0.9200 0.1292 -0.0282 0.071 Uiso 1 calc R . . H38B H 1.0554 0.1349 -0.0345 0.071 Uiso 1 calc R . . H38C H 0.9792 0.2303 -0.0371 0.071 Uiso 1 calc R . . O15 O 0.88399(15) 0.14746(12) 0.10154(5) 0.0207(5) Uani 1 d . . . O16 O 0.84949(15) 0.14672(12) 0.17139(5) 0.0205(5) Uani 1 d . . . O17 O 0.70741(15) 0.29619(12) 0.19894(5) 0.0173(4) Uani 1 d . . . O18 O 0.90192(15) 0.35630(12) 0.24233(5) 0.0188(4) Uani 1 d . . . C39 C 1.0008(2) 0.36816(19) 0.26570(8) 0.0209(7) Uani 1 d . . . H39 H 1.0701 0.3517 0.2508 0.023 Uiso 1 calc R . . C40 C 1.0115(3) 0.4715(2) 0.27812(8) 0.0307(8) Uani 1 d . . . H40A H 1.0158 0.5133 0.2562 0.034 Uiso 1 calc R . . H40B H 1.0812 0.4791 0.2933 0.034 Uiso 1 calc R . . H40C H 0.9445 0.4890 0.2929 0.034 Uiso 1 calc R . . C41 C 0.9954(3) 0.3000(2) 0.29847(8) 0.0332(8) Uani 1 d . . . H41A H 0.9883 0.2339 0.2893 0.037 Uiso 1 calc R . . H41B H 0.9290 0.3159 0.3138 0.037 Uiso 1 calc R . . H41C H 1.0656 0.3061 0.3135 0.037 Uiso 1 calc R . . O19 O 1.02163(16) 0.22349(12) 0.20882(5) 0.0218(5) Uani 1 d . . . C42 C 1.1044(3) 0.1648(2) 0.19148(8) 0.0320(8) Uani 1 d . . . H42 H 1.0674 0.1034 0.1833 0.035 Uiso 1 calc R . . C43 C 1.1505(3) 0.2161(3) 0.15810(9) 0.0479(10) Uani 1 d . . . H43A H 1.0880 0.2284 0.1403 0.053 Uiso 1 calc R . . H43B H 1.2089 0.1761 0.1462 0.053 Uiso 1 calc R . . H43C H 1.1848 0.2772 0.1659 0.053 Uiso 1 calc R . . C44 C 1.1970(3) 0.1426(2) 0.21969(9) 0.0401(9) Uani 1 d . . . H44A H 1.1638 0.1079 0.2407 0.044 Uiso 1 calc R . . H44B H 1.2313 0.2027 0.2286 0.044 Uiso 1 calc R . . H44C H 1.2561 0.1029 0.2081 0.044 Uiso 1 calc R . . 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 0.0173(3) 0.0158(3) 0.0193(3) -0.0020(2) -0.0043(2) 0.0015(2) Ti2 0.0169(3) 0.0154(3) 0.0168(3) 0.0016(2) -0.0005(2) 0.0034(2) Ti3 0.0189(3) 0.0196(3) 0.0173(3) -0.0030(2) 0.0001(2) 0.0033(2) Ti4 0.0160(3) 0.0130(3) 0.0188(3) 0.0012(2) -0.0025(2) 0.0000(2) O1 0.0187(12) 0.0171(10) 0.0181(10) 0.0001(8) -0.0041(8) 0.0008(8) P1 0.0163(5) 0.0159(4) 0.0155(4) 0.0002(3) 0.0005(3) 0.0002(3) C1 0.0209(18) 0.0195(16) 0.0184(17) -0.0020(13) -0.0032(13) -0.0029(14) C2 0.0214(19) 0.0285(18) 0.0235(17) 0.0023(14) -0.0015(14) 0.0028(15) C3 0.0180(19) 0.0327(19) 0.036(2) -0.0053(16) 0.0056(15) 0.0075(15) C4 0.029(2) 0.047(2) 0.035(2) -0.0013(17) 0.0139(16) -0.0003(18) C5 0.038(2) 0.046(2) 0.0261(19) 0.0095(16) 0.0028(17) -0.0057(18) C6 0.0217(19) 0.0307(19) 0.0259(18) 0.0055(15) 0.0029(14) 0.0049(14) O2 0.0195(12) 0.0144(10) 0.0228(11) -0.0004(8) -0.0033(8) 0.0017(8) P2 0.0199(5) 0.0148(4) 0.0235(4) -0.0016(3) -0.0037(3) 0.0031(3) C7 0.025(2) 0.0211(18) 0.0265(17) -0.0009(14) -0.0151(14) 0.0018(16) C8 0.045(3) 0.031(2) 0.045(2) 0.0054(16) 0.0137(18) 0.0117(18) C9 0.054(3) 0.037(2) 0.050(2) 0.0004(18) 0.0142(19) 0.027(2) C10 0.059(3) 0.022(2) 0.040(2) -0.0037(17) -0.0152(19) 0.012(2) C11 0.040(2) 0.023(2) 0.051(2) 0.0055(16) -0.0072(17) 0.0016(17) C12 0.026(2) 0.028(2) 0.049(2) 0.0036(16) -0.0047(16) 0.0049(17) O3 0.0215(12) 0.0183(11) 0.0216(11) 0.0043(9) -0.0009(8) -0.0012(9) P3 0.0165(5) 0.0156(4) 0.0164(4) 0.0008(3) 0.0014(3) 0.0009(3) C13 0.0141(17) 0.0196(16) 0.0240(18) -0.0033(14) 0.0023(14) 0.0071(13) C14 0.030(2) 0.0251(19) 0.045(2) 0.0055(16) -0.0059(16) -0.0110(16) C15 0.038(2) 0.031(2) 0.053(2) 0.0031(18) -0.0188(18) -0.0041(18) C16 0.021(2) 0.0288(19) 0.049(2) -0.0036(18) -0.0004(17) -0.0066(15) C17 0.042(2) 0.0232(19) 0.038(2) 0.0019(15) 0.0202(17) -0.0072(17) C18 0.034(2) 0.0299(19) 0.0234(18) -0.0033(15) 0.0104(15) -0.0050(16) O4 0.0332(13) 0.0191(11) 0.0240(11) 0.0076(9) -0.0084(9) -0.0101(9) S1 0.0246(5) 0.0181(4) 0.0261(4) 0.0025(3) -0.0022(3) -0.0028(3) C19 0.057(2) 0.0226(18) 0.037(2) 0.0020(15) 0.0066(17) -0.0086(17) C20 0.050(2) 0.032(2) 0.056(2) 0.0141(18) 0.0125(18) 0.0107(18) O5 0.0167(11) 0.0118(10) 0.0181(10) 0.0005(8) -0.0016(8) 0.0028(8) O6 0.0169(12) 0.0197(11) 0.0225(10) 0.0025(8) -0.0019(8) 0.0028(9) C21 0.0203(19) 0.0270(18) 0.0283(18) 0.0009(14) -0.0126(14) 0.0035(14) C22 0.038(2) 0.053(2) 0.036(2) 0.0098(17) -0.0129(16) 0.0095(18) C23 0.025(2) 0.054(2) 0.045(2) 0.0015(18) -0.0017(16) 0.0083(17) O7 0.0203(11) 0.0211(11) 0.0211(11) -0.0066(9) -0.0028(8) 0.0006(9) C24 0.033(2) 0.0297(19) 0.0231(17) -0.0119(15) -0.0002(14) -0.0021(15) C25 0.051(2) 0.041(2) 0.038(2) -0.0207(17) -0.0070(17) 0.0068(18) C26 0.046(2) 0.050(2) 0.035(2) -0.0150(17) -0.0125(17) -0.0038(18) O8 0.0197(12) 0.0197(11) 0.0265(11) -0.0027(9) -0.0050(9) -0.0035(9) C27 0.025(2) 0.040(2) 0.053(2) 0.0009(17) 0.0036(17) -0.0051(17) C28 0.062(3) 0.041(2) 0.051(2) 0.0149(18) -0.0113(19) -0.014(2) C29 0.031(2) 0.042(2) 0.061(2) -0.0030(18) -0.0098(17) -0.0095(17) O9 0.0176(11) 0.0165(11) 0.0182(10) -0.0007(8) 0.0009(8) 0.0025(8) O10 0.0247(12) 0.0159(12) 0.0248(11) 0.0052(9) -0.0008(8) 0.0086(9) C30 0.057(3) 0.029(2) 0.064(3) 0.0034(19) -0.010(2) 0.0077(19) C31 0.065(3) 0.045(2) 0.068(3) -0.018(2) 0.022(2) 0.006(2) C32 0.088(3) 0.040(2) 0.042(2) -0.0016(18) 0.009(2) -0.015(2) O11 0.0178(11) 0.0159(10) 0.0203(10) -0.0008(8) -0.0002(8) 0.0003(8) O12 0.0222(12) 0.0223(11) 0.0163(10) 0.0031(9) -0.0020(8) 0.0024(9) C33 0.029(2) 0.0342(19) 0.0184(17) 0.0080(15) -0.0010(13) 0.0078(15) C34 0.063(3) 0.055(2) 0.0174(18) 0.0041(16) 0.0031(17) 0.0195(19) C35 0.035(2) 0.056(2) 0.062(3) 0.028(2) -0.0030(18) -0.0024(19) O13 0.0167(11) 0.0189(11) 0.0229(11) -0.0014(9) 0.0006(8) -0.0011(9) O14 0.0247(13) 0.0324(12) 0.0218(11) -0.0082(9) 0.0104(9) 0.0008(10) C36 0.040(3) 0.057(2) 0.057(2) -0.024(2) 0.0097(19) -0.003(2) C37 0.050(3) 0.070(3) 0.062(3) -0.002(2) 0.002(2) 0.011(2) C38 0.063(3) 0.082(3) 0.049(3) -0.014(2) -0.004(2) 0.012(2) O15 0.0175(11) 0.0193(11) 0.0252(11) -0.0050(9) -0.0011(8) 0.0048(9) O16 0.0231(12) 0.0145(10) 0.0239(11) -0.0011(9) -0.0057(9) 0.0019(9) O17 0.0170(12) 0.0168(11) 0.0181(10) -0.0006(8) 0.0000(8) -0.0005(8) O18 0.0190(12) 0.0175(10) 0.0198(11) 0.0015(8) -0.0020(9) -0.0019(8) C39 0.0140(17) 0.0252(17) 0.0236(16) -0.0039(14) -0.0034(13) 0.0008(13) C40 0.0245(19) 0.032(2) 0.0358(19) -0.0069(15) -0.0044(14) -0.0062(15) C41 0.035(2) 0.036(2) 0.0283(18) -0.0018(16) -0.0156(15) -0.0007(15) O19 0.0213(12) 0.0194(11) 0.0246(11) -0.0025(9) -0.0046(9) 0.0048(9) C42 0.0202(19) 0.0312(19) 0.044(2) -0.0094(16) -0.0039(15) 0.0091(15) C43 0.033(2) 0.062(3) 0.048(2) -0.0020(19) 0.0055(17) 0.0131(19) C44 0.028(2) 0.047(2) 0.045(2) -0.0058(17) -0.0105(16) 0.0175(17) _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 O8 1.7810(18) . ? Ti1 O2 1.9467(17) . ? Ti1 O1 1.9530(17) . ? Ti1 O5 1.9757(18) . ? Ti1 O6 2.0141(18) . ? Ti1 O7 2.0439(18) . ? Ti1 Ti2 3.1014(6) . ? Ti1 Ti3 3.1106(6) . ? Ti2 O10 1.7720(18) . ? Ti2 O5 1.9470(17) . ? Ti2 O9 1.9773(17) . ? Ti2 O11 1.9836(18) . ? Ti2 O12 2.0259(18) . ? Ti2 O6 2.0319(18) . ? Ti2 Ti3 3.1132(6) . ? Ti3 O14 1.7702(18) . ? Ti3 O5 1.9490(18) . ? Ti3 O15 1.9761(18) . ? Ti3 O13 1.9811(18) . ? Ti3 O7 2.0183(18) . ? Ti3 O12 2.0341(18) . ? Ti4 O19 1.7861(19) . ? Ti4 O18 1.8325(17) . ? Ti4 O3 1.9549(17) . ? Ti4 O17 2.0399(18) . ? Ti4 O4 2.0585(18) . ? Ti4 O16 2.0952(17) . ? O1 P1 1.5403(18) . ? P1 O17 1.5078(19) . ? P1 O9 1.5391(18) . ? P1 C1 1.800(3) . ? C1 C2 1.388(4) . ? C1 C6 1.394(4) . ? C2 C3 1.373(4) . ? C3 C4 1.367(4) . ? C4 C5 1.378(4) . ? C5 C6 1.374(4) . ? O2 P2 1.5431(19) . ? P2 O16 1.4996(19) . ? P2 O15 1.533(2) . ? P2 C7 1.798(3) . ? C7 C8 1.372(4) . ? C7 C12 1.389(4) . ? C8 C9 1.394(5) . ? C9 C10 1.359(5) . ? C10 C11 1.371(5) . ? C11 C12 1.370(4) . ? O3 P3 1.5062(19) . ? P3 O13 1.5310(19) . ? P3 O11 1.5377(19) . ? P3 C13 1.797(3) . ? C13 C14 1.391(4) . ? C13 C18 1.391(4) . ? C14 C15 1.377(4) . ? C15 C16 1.370(5) . ? C16 C17 1.369(4) . ? C17 C18 1.388(4) . ? O4 S1 1.5234(19) . ? S1 C20 1.763(3) . ? S1 C19 1.778(3) . ? O6 C21 1.442(3) . ? C21 C22 1.499(4) . ? C21 C23 1.515(4) . ? O7 C24 1.439(3) . ? C24 C25 1.503(4) . ? C24 C26 1.505(4) . ? O8 C27 1.427(4) . ? C27 C28 1.480(5) . ? C27 C29 1.517(4) . ? O10 C30 1.400(4) . ? C30 C32 1.470(5) . ? C30 C31 1.495(5) . ? O12 C33 1.432(3) . ? C33 C35 1.505(4) . ? C33 C34 1.513(4) . ? O14 C36 1.419(4) . ? C36 C38 1.477(5) . ? C36 C37 1.502(5) . ? O18 C39 1.430(3) . ? C39 C40 1.510(4) . ? C39 C41 1.513(4) . ? O19 C42 1.414(3) . ? C42 C43 1.499(4) . ? C42 C44 1.505(4) . ? 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 O8 Ti1 O2 95.76(8) . . ? O8 Ti1 O1 95.87(8) . . ? O2 Ti1 O1 89.21(7) . . ? O8 Ti1 O5 175.37(8) . . ? O2 Ti1 O5 88.36(7) . . ? O1 Ti1 O5 86.27(7) . . ? O8 Ti1 O6 99.02(8) . . ? O2 Ti1 O6 165.22(8) . . ? O1 Ti1 O6 89.56(7) . . ? O5 Ti1 O6 76.86(7) . . ? O8 Ti1 O7 101.73(8) . . ? O2 Ti1 O7 87.53(7) . . ? O1 Ti1 O7 162.33(8) . . ? O5 Ti1 O7 76.29(7) . . ? O6 Ti1 O7 89.19(7) . . ? O8 Ti1 Ti2 138.79(6) . . ? O2 Ti1 Ti2 125.16(6) . . ? O1 Ti1 Ti2 81.47(5) . . ? O5 Ti1 Ti2 37.43(5) . . ? O6 Ti1 Ti2 40.17(5) . . ? O7 Ti1 Ti2 86.25(5) . . ? O8 Ti1 Ti3 141.27(6) . . ? O2 Ti1 Ti3 81.74(6) . . ? O1 Ti1 Ti3 122.61(6) . . ? O5 Ti1 Ti3 37.27(5) . . ? O6 Ti1 Ti3 86.54(5) . . ? O7 Ti1 Ti3 39.72(5) . . ? Ti2 Ti1 Ti3 60.152(16) . . ? O10 Ti2 O5 173.44(8) . . ? O10 Ti2 O9 98.82(8) . . ? O5 Ti2 O9 87.23(7) . . ? O10 Ti2 O11 94.64(8) . . ? O5 Ti2 O11 87.69(7) . . ? O9 Ti2 O11 91.46(7) . . ? O10 Ti2 O12 97.72(8) . . ? O5 Ti2 O12 76.23(7) . . ? O9 Ti2 O12 163.45(7) . . ? O11 Ti2 O12 87.62(7) . . ? O10 Ti2 O6 100.41(8) . . ? O5 Ti2 O6 77.08(7) . . ? O9 Ti2 O6 88.64(7) . . ? O11 Ti2 O6 164.75(7) . . ? O12 Ti2 O6 87.97(7) . . ? O10 Ti2 Ti1 140.08(7) . . ? O5 Ti2 Ti1 38.08(5) . . ? O9 Ti2 Ti1 81.51(5) . . ? O11 Ti2 Ti1 125.27(5) . . ? O12 Ti2 Ti1 85.55(5) . . ? O6 Ti2 Ti1 39.74(5) . . ? O10 Ti2 Ti3 137.38(6) . . ? O5 Ti2 Ti3 36.98(5) . . ? O9 Ti2 Ti3 123.55(5) . . ? O11 Ti2 Ti3 81.07(5) . . ? O12 Ti2 Ti3 40.03(5) . . ? O6 Ti2 Ti3 86.17(5) . . ? Ti1 Ti2 Ti3 60.071(17) . . ? O14 Ti3 O5 175.49(8) . . ? O14 Ti3 O15 95.54(8) . . ? O5 Ti3 O15 86.31(7) . . ? O14 Ti3 O13 95.59(8) . . ? O5 Ti3 O13 88.48(7) . . ? O15 Ti3 O13 91.17(7) . . ? O14 Ti3 O7 98.40(8) . . ? O5 Ti3 O7 77.48(7) . . ? O15 Ti3 O7 89.25(7) . . ? O13 Ti3 O7 165.90(7) . . ? O14 Ti3 O12 102.18(8) . . ? O5 Ti3 O12 75.99(7) . . ? O15 Ti3 O12 162.27(8) . . ? O13 Ti3 O12 87.48(7) . . ? O7 Ti3 O12 87.84(7) . . ? O14 Ti3 Ti1 138.31(7) . . ? O5 Ti3 Ti1 37.87(5) . . ? O15 Ti3 Ti1 81.32(6) . . ? O13 Ti3 Ti1 125.91(5) . . ? O7 Ti3 Ti1 40.33(5) . . ? O12 Ti3 Ti1 85.17(5) . . ? O14 Ti3 Ti2 141.79(7) . . ? O5 Ti3 Ti2 36.94(5) . . ? O15 Ti3 Ti2 122.52(5) . . ? O13 Ti3 Ti2 81.53(5) . . ? O7 Ti3 Ti2 86.36(5) . . ? O12 Ti3 Ti2 39.84(5) . . ? Ti1 Ti3 Ti2 59.778(17) . . ? O19 Ti4 O18 92.61(8) . . ? O19 Ti4 O3 93.38(8) . . ? O18 Ti4 O3 94.32(8) . . ? O19 Ti4 O17 171.83(8) . . ? O18 Ti4 O17 95.29(7) . . ? O3 Ti4 O17 88.10(7) . . ? O19 Ti4 O4 93.91(8) . . ? O18 Ti4 O4 86.80(8) . . ? O3 Ti4 O4 172.56(8) . . ? O17 Ti4 O4 84.48(7) . . ? O19 Ti4 O16 85.01(8) . . ? O18 Ti4 O16 171.24(8) . . ? O3 Ti4 O16 94.23(7) . . ? O17 Ti4 O16 86.87(7) . . ? O4 Ti4 O16 84.97(7) . . ? P1 O1 Ti1 126.30(11) . . ? O17 P1 O9 113.13(10) . . ? O17 P1 O1 114.02(10) . . ? O9 P1 O1 109.85(10) . . ? O17 P1 C1 106.90(11) . . ? O9 P1 C1 107.18(11) . . ? O1 P1 C1 105.16(11) . . ? C2 C1 C6 118.1(3) . . ? C2 C1 P1 122.9(2) . . ? C6 C1 P1 119.1(2) . . ? C3 C2 C1 120.6(3) . . ? C4 C3 C2 120.5(3) . . ? C3 C4 C5 120.2(3) . . ? C6 C5 C4 119.6(3) . . ? C5 C6 C1 121.1(3) . . ? P2 O2 Ti1 125.52(10) . . ? O16 P2 O15 113.93(10) . . ? O16 P2 O2 112.34(11) . . ? O15 P2 O2 111.00(10) . . ? O16 P2 C7 109.42(11) . . ? O15 P2 C7 106.14(13) . . ? O2 P2 C7 103.27(12) . . ? C8 C7 C12 118.0(3) . . ? C8 C7 P2 122.5(2) . . ? C12 C7 P2 119.6(2) . . ? C7 C8 C9 120.7(3) . . ? C10 C9 C8 120.0(3) . . ? C9 C10 C11 120.0(3) . . ? C12 C11 C10 120.0(3) . . ? C11 C12 C7 121.2(3) . . ? P3 O3 Ti4 166.96(12) . . ? O3 P3 O13 113.34(10) . . ? O3 P3 O11 112.54(10) . . ? O13 P3 O11 109.99(10) . . ? O3 P3 C13 106.23(11) . . ? O13 P3 C13 107.43(11) . . ? O11 P3 C13 106.90(11) . . ? C14 C13 C18 118.0(3) . . ? C14 C13 P3 119.9(2) . . ? C18 C13 P3 122.1(2) . . ? C15 C14 C13 120.1(3) . . ? C16 C15 C14 121.0(3) . . ? C17 C16 C15 120.1(3) . . ? C16 C17 C18 119.4(3) . . ? C17 C18 C13 121.3(3) . . ? S1 O4 Ti4 127.97(11) . . ? O4 S1 C20 105.74(14) . . ? O4 S1 C19 102.65(13) . . ? C20 S1 C19 97.36(16) . . ? Ti2 O5 Ti3 106.08(8) . . ? Ti2 O5 Ti1 104.49(8) . . ? Ti3 O5 Ti1 104.85(8) . . ? C21 O6 Ti1 125.40(16) . . ? C21 O6 Ti2 133.03(16) . . ? Ti1 O6 Ti2 100.09(8) . . ? O6 C21 C22 109.8(2) . . ? O6 C21 C23 110.5(2) . . ? C22 C21 C23 111.9(3) . . ? C24 O7 Ti3 126.02(16) . . ? C24 O7 Ti1 131.96(17) . . ? Ti3 O7 Ti1 99.95(7) . . ? O7 C24 C25 110.9(2) . . ? O7 C24 C26 109.9(2) . . ? C25 C24 C26 113.2(3) . . ? C27 O8 Ti1 150.43(18) . . ? O8 C27 C28 110.4(3) . . ? O8 C27 C29 108.6(3) . . ? C28 C27 C29 113.3(3) . . ? P1 O9 Ti2 124.60(10) . . ? C30 O10 Ti2 166.4(2) . . ? O10 C30 C32 112.9(3) . . ? O10 C30 C31 109.4(3) . . ? C32 C30 C31 112.9(3) . . ? P3 O11 Ti2 124.05(10) . . ? C33 O12 Ti2 127.34(16) . . ? C33 O12 Ti3 131.98(17) . . ? Ti2 O12 Ti3 100.13(8) . . ? O12 C33 C35 110.6(2) . . ? O12 C33 C34 110.0(2) . . ? C35 C33 C34 112.3(3) . . ? P3 O13 Ti3 123.35(11) . . ? C36 O14 Ti3 149.2(2) . . ? O14 C36 C38 111.2(3) . . ? O14 C36 C37 109.1(3) . . ? C38 C36 C37 113.7(3) . . ? P2 O15 Ti3 126.41(11) . . ? P2 O16 Ti4 153.28(11) . . ? P1 O17 Ti4 159.10(11) . . ? C39 O18 Ti4 128.05(16) . . ? O18 C39 C40 110.3(2) . . ? O18 C39 C41 110.1(2) . . ? C40 C39 C41 111.8(2) . . ? C42 O19 Ti4 144.48(17) . . ? O19 C42 C43 109.1(2) . . ? O19 C42 C44 108.1(2) . . ? C43 C42 C44 112.0(3) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 20.93 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.259 _refine_diff_density_min -0.253 _refine_diff_density_rms 0.040 #=END data_(2) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C61 H71 O16.50 P4 S0.50 Ti4' _chemical_formula_weight 1399.69 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, z+1/2' '-x, -y, -z' '-x, y-1/2, -z-1/2' _cell_length_a 12.4983(10) _cell_length_b 16.1317(14) _cell_length_c 33.706(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.141(10) _cell_angle_gamma 90.00 _cell_volume 6743.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'Plate' _exptl_crystal_colour 'Colourless' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2900 _exptl_absorpt_coefficient_mu 0.630 _exptl_absorpt_correction_type 'Numerical' _exptl_absorpt_process_details 'X-SHAPE (Stoe & Cie, 1996)' _exptl_absorpt_correction_T_min 0.7034 _exptl_absorpt_correction_T_max 0.8686 _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'STOE-IPDS' _diffrn_measurement_method 'Imaging Plate Detector System' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52425 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0357 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 24.20 _reflns_number_total 10165 _reflns_number_gt 6923 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE-IPDS software (Stoe, 2.87, 1997)' _computing_cell_refinement 'STOE-IPDS software (Stoe, 2.87, 1997)' _computing_data_reduction 'XRED (Stoe, 1.08, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP (Zsolnai, 1996)' _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 w=1/[\s^2^(Fo^2^)+(0.0334P)^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 10165 _refine_ls_number_parameters 793 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0240 _refine_ls_wR_factor_ref 0.0607 _refine_ls_wR_factor_gt 0.0568 _refine_ls_goodness_of_fit_ref 0.836 _refine_ls_restrained_S_all 0.836 _refine_ls_shift/su_max 0.002 _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 0.17916(3) 0.68172(2) 0.079208(11) 0.01758(9) Uani 1 d . . . Ti2 Ti 0.37174(3) 0.78568(2) 0.056390(11) 0.01728(9) Uani 1 d . . . Ti3 Ti 0.21989(3) 0.84108(2) 0.117481(11) 0.01677(9) Uani 1 d . . . Ti4 Ti 0.39404(3) 0.70491(2) 0.133582(11) 0.01745(9) Uani 1 d . . . P1 P 0.24262(5) 0.67012(4) -0.009797(17) 0.02091(13) Uani 1 d . . . P2 P 0.26533(5) 0.53292(4) 0.137379(18) 0.02215(13) Uani 1 d . . . P3 P 0.30538(5) 0.97576(3) 0.059520(17) 0.02083(13) Uani 1 d . . . P4 P 0.35958(5) 0.83370(4) 0.203734(17) 0.02163(13) Uani 1 d . . . O1 O 0.20351(12) 0.79376(8) 0.06509(4) 0.0179(3) Uani 1 d . . . O2 O 0.35193(12) 0.67757(8) 0.07944(4) 0.0180(3) Uani 1 d . . . O3 O 0.22707(12) 0.72540(9) 0.13198(4) 0.0178(3) Uani 1 d . . . O4 O 0.38528(12) 0.81549(9) 0.11216(4) 0.0184(3) Uani 1 d . . . O5 O 0.17860(13) 0.64116(9) 0.02300(4) 0.0238(4) Uani 1 d . . . O6 O 0.31777(13) 0.74285(9) 0.00180(4) 0.0227(4) Uani 1 d . . . O7 O 0.19605(12) 0.56514(9) 0.10041(5) 0.0222(3) Uani 1 d . . . O8 O 0.35890(12) 0.58931(9) 0.15278(5) 0.0236(4) Uani 1 d . . . O9 O 0.34377(13) 0.90254(9) 0.03660(4) 0.0225(3) Uani 1 d . . . O10 O 0.25267(13) 0.95356(9) 0.09611(4) 0.0224(3) Uani 1 d . . . O11 O 0.27731(13) 0.87694(9) 0.17373(4) 0.0232(4) Uani 1 d . . . O12 O 0.39918(13) 0.75065(9) 0.19005(4) 0.0238(4) Uani 1 d . . . O13 O 0.03760(12) 0.68036(10) 0.07802(5) 0.0275(4) Uani 1 d . . . O14 O 0.50998(13) 0.78396(9) 0.05107(5) 0.0247(4) Uani 1 d . . . O15 O 0.08404(13) 0.86227(9) 0.12443(5) 0.0252(4) Uani 1 d . . . O16 O 0.53611(13) 0.68542(9) 0.14042(5) 0.0251(4) Uani 1 d . . . C1 C 0.1499(2) 0.70207(14) -0.05209(7) 0.0267(5) Uani 1 d . . . C2 C 0.1446(2) 0.78282(17) -0.06470(8) 0.0403(7) Uani 1 d . . . H2 H 0.1907 0.8234 -0.0512 0.044 Uiso 1 calc R . . C3 C 0.0716(2) 0.80463(19) -0.09725(9) 0.0448(7) Uani 1 d . . . H3 H 0.0687 0.8602 -0.1066 0.049 Uiso 1 calc R . . C4 C 0.0031(3) 0.74630(19) -0.11613(9) 0.0480(8) Uani 1 d . . . H4 H -0.0481 0.7621 -0.1380 0.053 Uiso 1 calc R . . C5 C 0.0081(3) 0.66700(19) -0.10378(9) 0.0460(7) Uani 1 d . . . H5 H -0.0391 0.6269 -0.1171 0.051 Uiso 1 calc R . . C6 C 0.0820(2) 0.64352(18) -0.07165(9) 0.0434(7) Uani 1 d . . . H6 H 0.0859 0.5874 -0.0631 0.048 Uiso 1 calc R . . C7 C 0.3169(2) 0.58374(15) -0.02553(7) 0.0269(5) Uani 1 d . . . C8 C 0.3269(2) 0.51185(16) -0.00295(8) 0.0356(6) Uani 1 d . . . H8 H 0.2934 0.5079 0.0208 0.039 Uiso 1 calc R . . C9 C 0.3858(2) 0.44563(18) -0.01499(9) 0.0433(7) Uani 1 d . . . H9 H 0.3926 0.3964 0.0006 0.048 Uiso 1 calc R . . C10 C 0.4336(3) 0.45084(19) -0.04889(9) 0.0467(7) Uani 1 d . . . H10 H 0.4728 0.4048 -0.0572 0.051 Uiso 1 calc R . . C11 C 0.4258(2) 0.52221(18) -0.07137(9) 0.0443(7) Uani 1 d . . . H11 H 0.4602 0.5256 -0.0949 0.049 Uiso 1 calc R . . C12 C 0.3676(2) 0.58933(18) -0.05957(8) 0.0418(7) Uani 1 d . . . H12 H 0.3628 0.6389 -0.0749 0.046 Uiso 1 calc R . . C13 C 0.1805(2) 0.51929(15) 0.17612(7) 0.0309(6) Uani 1 d . . . C14 C 0.1515(2) 0.44123(18) 0.18879(8) 0.0399(7) Uani 1 d . . . H14 H 0.1801 0.3927 0.1781 0.044 Uiso 1 calc R . . C15 C 0.0796(2) 0.43487(19) 0.21743(9) 0.0460(7) Uani 1 d . . . H15 H 0.0602 0.3817 0.2263 0.051 Uiso 1 calc R . . C16 C 0.0377(3) 0.50350(18) 0.23250(9) 0.0460(7) Uani 1 d . . . H16 H -0.0126 0.4984 0.2513 0.051 Uiso 1 calc R . . C17 C 0.0680(2) 0.58141(18) 0.22054(9) 0.0436(7) Uani 1 d . . . H17 H 0.0394 0.6295 0.2317 0.048 Uiso 1 calc R . . C18 C 0.1388(2) 0.58963(18) 0.19287(8) 0.0418(7) Uani 1 d . . . H18 H 0.1595 0.6433 0.1850 0.046 Uiso 1 calc R . . C19 C 0.3145(2) 0.43256(16) 0.12495(8) 0.0325(6) Uani 1 d . . . C20 C 0.4003(2) 0.39514(18) 0.14753(9) 0.0436(7) Uani 1 d . . . H20 H 0.4353 0.4219 0.1707 0.048 Uiso 1 calc R . . C21 C 0.4355(3) 0.31829(18) 0.13629(9) 0.0453(7) Uani 1 d . . . H21 H 0.4937 0.2919 0.1522 0.050 Uiso 1 calc R . . C22 C 0.3881(3) 0.2806(2) 0.10306(9) 0.0491(8) Uani 1 d . . . H22 H 0.4143 0.2283 0.0957 0.054 Uiso 1 calc R . . C23 C 0.3036(2) 0.31568(17) 0.07991(9) 0.0427(7) Uani 1 d . . . H23 H 0.2700 0.2885 0.0566 0.047 Uiso 1 calc R . . C24 C 0.2675(2) 0.39256(17) 0.09123(8) 0.0411(7) Uani 1 d . . . H24 H 0.2088 0.4182 0.0752 0.045 Uiso 1 calc R . . C25 C 0.2095(2) 1.03381(14) 0.02633(7) 0.0251(5) Uani 1 d . . . C26 C 0.1635(2) 1.10526(16) 0.04064(8) 0.0384(6) Uani 1 d . . . H26 H 0.1871 1.1251 0.0668 0.042 Uiso 1 calc R . . C27 C 0.0833(2) 1.14684(18) 0.01632(9) 0.0442(7) Uani 1 d . . . H27 H 0.0528 1.1958 0.0258 0.049 Uiso 1 calc R . . C28 C 0.0480(3) 1.11851(18) -0.02066(9) 0.0462(7) Uani 1 d . . . H28 H -0.0081 1.1471 -0.0367 0.051 Uiso 1 calc R . . C29 C 0.0917(2) 1.04989(18) -0.03511(9) 0.0435(7) Uani 1 d . . . H29 H 0.0669 1.0306 -0.0613 0.048 Uiso 1 calc R . . C30 C 0.1742(2) 1.00721(18) -0.01125(8) 0.0420(7) Uani 1 d . . . H30 H 0.2054 0.9593 -0.0215 0.046 Uiso 1 calc R . . C31 C 0.42057(19) 1.03973(13) 0.07542(7) 0.0216(5) Uani 1 d . . . C32 C 0.4773(2) 1.07820(15) 0.04746(7) 0.0297(6) Uani 1 d . . . H32 H 0.4519 1.0738 0.0198 0.033 Uiso 1 calc R . . C33 C 0.5694(2) 1.12238(16) 0.05960(8) 0.0365(6) Uani 1 d . . . H33 H 0.6068 1.1493 0.0404 0.040 Uiso 1 calc R . . C34 C 0.6075(2) 1.12770(17) 0.09943(8) 0.0409(7) Uani 1 d . . . H34 H 0.6712 1.1583 0.1079 0.045 Uiso 1 calc R . . C35 C 0.5527(2) 1.08831(17) 0.12720(9) 0.0430(7) Uani 1 d . . . H35 H 0.5795 1.0917 0.1548 0.047 Uiso 1 calc R . . C36 C 0.4595(2) 1.04411(15) 0.11543(8) 0.0334(6) Uani 1 d . . . H36 H 0.4225 1.0170 0.1347 0.037 Uiso 1 calc R . . C37 C 0.3008(2) 0.81759(14) 0.24920(7) 0.0268(5) Uani 1 d . . . C38 C 0.2423(2) 0.88113(16) 0.26528(8) 0.0347(6) Uani 1 d . . . H38 H 0.2307 0.9324 0.2515 0.038 Uiso 1 calc R . . C39 C 0.2024(2) 0.86898(17) 0.30059(8) 0.0391(7) Uani 1 d . . . H39 H 0.1647 0.9124 0.3119 0.043 Uiso 1 calc R . . C40 C 0.2164(2) 0.79404(17) 0.32004(9) 0.0400(7) Uani 1 d . . . H40 H 0.1900 0.7866 0.3450 0.044 Uiso 1 calc R . . C41 C 0.2681(2) 0.72992(17) 0.30363(8) 0.0398(7) Uani 1 d . . . H41 H 0.2733 0.6773 0.3163 0.044 Uiso 1 calc R . . C42 C 0.3126(2) 0.74222(17) 0.26840(8) 0.0386(7) Uani 1 d . . . H42 H 0.3512 0.6987 0.2575 0.042 Uiso 1 calc R . . C43 C 0.4747(2) 0.90071(14) 0.21511(7) 0.0250(5) Uani 1 d . . . C44 C 0.4771(2) 0.96586(17) 0.24118(8) 0.0418(7) Uani 1 d . . . H44 H 0.4155 0.9771 0.2542 0.046 Uiso 1 calc R . . C45 C 0.5679(2) 1.01600(18) 0.24900(9) 0.0437(7) Uani 1 d . . . H45 H 0.5683 1.0608 0.2673 0.048 Uiso 1 calc R . . C46 C 0.6562(2) 1.00031(17) 0.23021(8) 0.0398(7) Uani 1 d . . . H46 H 0.7188 1.0338 0.2357 0.044 Uiso 1 calc R . . C47 C 0.6548(3) 0.93674(18) 0.20353(9) 0.0435(7) Uani 1 d . . . H47 H 0.7162 0.9263 0.1903 0.048 Uiso 1 calc R . . C48 C 0.5635(2) 0.88703(17) 0.19564(8) 0.0404(7) Uani 1 d . . . H48 H 0.5626 0.8434 0.1767 0.044 Uiso 1 calc R . . C49 C -0.0670(2) 0.6463(2) 0.06982(9) 0.0505(8) Uani 1 d . . . H49 H -0.1190 0.6930 0.0713 0.056 Uiso 1 calc R . . C50 C -0.0819(3) 0.6159(2) 0.02729(9) 0.0544(8) Uani 1 d . . . H50A H -0.0672 0.6612 0.0094 0.060 Uiso 1 calc R . . H50B H -0.1561 0.5966 0.0203 0.060 Uiso 1 calc R . . H50C H -0.0319 0.5700 0.0245 0.060 Uiso 1 calc R . . C51 C -0.0887(3) 0.58608(19) 0.10036(9) 0.0489(8) Uani 1 d . . . H51A H -0.0777 0.6124 0.1268 0.054 Uiso 1 calc R . . H51B H -0.0395 0.5389 0.0999 0.054 Uiso 1 calc R . . H51C H -0.1634 0.5667 0.0948 0.054 Uiso 1 calc R . . C52 C 0.6211(2) 0.79327(18) 0.06377(9) 0.0395(7) Uani 1 d . . . H52 H 0.6437 0.7489 0.0838 0.043 Uiso 1 calc R . . C53 C 0.6401(3) 0.8753(2) 0.08373(10) 0.0529(8) Uani 1 d . . . H53A H 0.5978 0.8791 0.1063 0.058 Uiso 1 calc R . . H53B H 0.6182 0.9196 0.0645 0.058 Uiso 1 calc R . . H53C H 0.7169 0.8813 0.0935 0.058 Uiso 1 calc R . . C54 C 0.6835(2) 0.78280(17) 0.02927(9) 0.0418(7) Uani 1 d . . . H54A H 0.6693 0.7278 0.0175 0.046 Uiso 1 calc R . . H54B H 0.7607 0.7883 0.0385 0.046 Uiso 1 calc R . . H54C H 0.6618 0.8254 0.0092 0.046 Uiso 1 calc R . . C55 C -0.0098(2) 0.86430(19) 0.14252(9) 0.0452(7) Uani 1 d . . . H55 H -0.0707 0.8468 0.1222 0.050 Uiso 1 calc R . . C56 C -0.0011(3) 0.80196(19) 0.17626(9) 0.0473(7) Uani 1 d . . . H56A H 0.0133 0.7469 0.1659 0.052 Uiso 1 calc R . . H56B H -0.0689 0.8008 0.1881 0.052 Uiso 1 calc R . . H56C H 0.0580 0.8178 0.1967 0.052 Uiso 1 calc R . . C57 C -0.0319(3) 0.9497(2) 0.15510(10) 0.0580(9) Uani 1 d . . . H57A H -0.0373 0.9866 0.1318 0.064 Uiso 1 calc R . . H57B H 0.0269 0.9685 0.1750 0.064 Uiso 1 calc R . . H57C H -0.0999 0.9508 0.1668 0.064 Uiso 1 calc R . . C58 C 0.6202(2) 0.65977(18) 0.17051(9) 0.0459(7) Uani 1 d . . . H58 H 0.5960 0.6756 0.1967 0.051 Uiso 1 calc R . . C59 C 0.6317(2) 0.56894(18) 0.17149(10) 0.0487(8) Uani 1 d . . . H59A H 0.5616 0.5434 0.1737 0.054 Uiso 1 calc R . . H59B H 0.6832 0.5529 0.1946 0.054 Uiso 1 calc R . . H59C H 0.6582 0.5500 0.1468 0.054 Uiso 1 calc R . . C60 C 0.7225(2) 0.70587(18) 0.16817(9) 0.0468(7) Uani 1 d . . . H60A H 0.7082 0.7656 0.1681 0.052 Uiso 1 calc R . . H60B H 0.7519 0.6905 0.1436 0.052 Uiso 1 calc R . . H60C H 0.7748 0.6918 0.1913 0.052 Uiso 1 calc R . . S1 S 0.19945(12) 0.14600(8) 0.20900(4) 0.0382(3) Uani 0.50 d P . . O17 O 0.1919(3) 0.0860(2) 0.24063(11) 0.0459(10) Uani 0.50 d P . . C61 C 0.2384(6) 0.0986(4) 0.16669(18) 0.0511(16) Uani 0.50 d P . . H61A H 0.1869 0.0547 0.1576 0.056 Uiso 0.50 calc PR . . H61B H 0.3105 0.0745 0.1732 0.056 Uiso 0.50 calc PR . . H61C H 0.2399 0.1399 0.1454 0.056 Uiso 0.50 calc PR . . C62 C 0.3042(7) 0.2205(5) 0.2188(2) 0.071(2) Uani 0.50 d P . . H62A H 0.2925 0.2533 0.2423 0.078 Uiso 0.50 calc PR . . H62B H 0.3041 0.2573 0.1956 0.078 Uiso 0.50 calc PR . . H62C H 0.3739 0.1921 0.2237 0.078 Uiso 0.50 calc PR . . 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 0.0146(2) 0.0182(2) 0.0197(2) 0.00035(16) 0.00109(15) -0.00366(15) Ti2 0.0151(2) 0.0183(2) 0.0186(2) -0.00053(16) 0.00289(15) -0.00276(15) Ti3 0.0153(2) 0.0173(2) 0.01770(19) -0.00012(16) 0.00205(15) -0.00017(15) Ti4 0.0148(2) 0.0181(2) 0.0191(2) 0.00099(16) 0.00053(16) -0.00044(15) P1 0.0213(3) 0.0228(3) 0.0183(3) -0.0021(2) 0.0014(2) -0.0043(2) P2 0.0216(3) 0.0199(3) 0.0251(3) 0.0048(2) 0.0032(2) -0.0026(2) P3 0.0233(3) 0.0174(3) 0.0219(3) 0.0024(2) 0.0029(2) -0.0024(2) P4 0.0235(3) 0.0236(3) 0.0175(3) -0.0015(2) 0.0013(2) -0.0013(2) O1 0.0175(9) 0.0171(7) 0.0186(8) 0.0012(6) 0.0003(6) -0.0027(6) O2 0.0173(8) 0.0167(7) 0.0201(8) 0.0002(6) 0.0027(6) -0.0007(6) O3 0.0146(8) 0.0185(8) 0.0203(8) 0.0017(6) 0.0021(6) -0.0007(6) O4 0.0151(8) 0.0193(8) 0.0202(8) -0.0016(6) 0.0004(6) -0.0031(6) O5 0.0255(10) 0.0244(8) 0.0217(8) -0.0005(7) 0.0043(7) -0.0099(7) O6 0.0245(9) 0.0250(8) 0.0183(8) -0.0028(6) 0.0017(7) -0.0079(7) O7 0.0194(9) 0.0195(8) 0.0273(8) 0.0031(6) 0.0015(7) -0.0053(6) O8 0.0201(9) 0.0220(8) 0.0284(9) 0.0056(7) 0.0018(7) -0.0015(6) O9 0.0278(10) 0.0172(8) 0.0238(8) 0.0009(6) 0.0073(7) -0.0021(6) O10 0.0267(10) 0.0178(8) 0.0242(8) 0.0024(6) 0.0083(7) 0.0008(6) O11 0.0266(10) 0.0239(8) 0.0189(8) -0.0016(6) 0.0019(7) 0.0022(7) O12 0.0255(10) 0.0258(8) 0.0195(8) -0.0012(7) -0.0001(7) 0.0028(7) O13 0.0129(9) 0.0317(9) 0.0377(9) 0.0033(8) 0.0022(7) -0.0060(7) O14 0.0170(9) 0.0289(9) 0.0288(9) 0.0011(7) 0.0053(7) -0.0037(7) O15 0.0169(9) 0.0288(9) 0.0305(9) 0.0019(7) 0.0054(7) 0.0038(7) O16 0.0186(9) 0.0266(9) 0.0298(9) 0.0042(7) 0.0015(7) 0.0024(7) C1 0.0241(15) 0.0304(13) 0.0259(13) -0.0001(10) 0.0043(10) -0.0004(10) C2 0.0414(18) 0.0400(16) 0.0396(16) -0.0001(13) 0.0049(13) 0.0039(13) C3 0.0431(19) 0.0452(17) 0.0461(17) 0.0017(13) 0.0055(14) 0.0044(13) C4 0.043(2) 0.0560(18) 0.0441(18) 0.0014(14) 0.0019(15) 0.0034(14) C5 0.0451(19) 0.0507(18) 0.0413(17) -0.0008(14) 0.0018(14) -0.0035(14) C6 0.0440(19) 0.0435(17) 0.0416(17) 0.0010(13) 0.0006(14) -0.0025(13) C7 0.0254(15) 0.0279(13) 0.0275(13) -0.0005(10) 0.0037(10) -0.0005(10) C8 0.0350(17) 0.0352(15) 0.0362(15) 0.0001(12) 0.0030(12) -0.0014(12) C9 0.0404(19) 0.0398(17) 0.0492(17) -0.0011(13) 0.0029(13) -0.0030(13) C10 0.042(2) 0.0470(18) 0.0502(18) -0.0059(14) 0.0026(14) 0.0009(14) C11 0.0413(19) 0.0472(17) 0.0446(17) -0.0025(14) 0.0060(14) 0.0021(14) C12 0.0408(19) 0.0429(16) 0.0420(16) -0.0016(13) 0.0063(13) 0.0015(13) C13 0.0290(16) 0.0336(14) 0.0301(13) 0.0026(11) 0.0041(11) -0.0010(11) C14 0.0417(18) 0.0415(16) 0.0365(16) 0.0022(12) 0.0044(13) -0.0046(12) C15 0.045(2) 0.0489(17) 0.0442(17) 0.0021(14) 0.0051(14) -0.0059(14) C16 0.041(2) 0.0532(18) 0.0443(17) 0.0030(14) 0.0074(14) -0.0014(14) C17 0.0405(19) 0.0476(17) 0.0437(17) -0.0002(13) 0.0089(14) 0.0033(13) C18 0.0410(19) 0.0437(16) 0.0412(16) 0.0017(13) 0.0076(13) 0.0010(13) C19 0.0340(16) 0.0294(14) 0.0343(14) 0.0023(11) 0.0053(11) -0.0010(11) C20 0.0410(19) 0.0419(17) 0.0473(17) 0.0029(13) 0.0029(14) -0.0003(13) C21 0.0439(19) 0.0405(17) 0.0506(17) 0.0037(14) 0.0024(14) 0.0028(13) C22 0.052(2) 0.0428(18) 0.0532(18) -0.0005(15) 0.0103(15) 0.0019(15) C23 0.0476(19) 0.0386(16) 0.0422(16) -0.0016(13) 0.0064(13) -0.0007(13) C24 0.0444(18) 0.0377(16) 0.0417(16) -0.0011(13) 0.0079(13) -0.0005(13) C25 0.0252(14) 0.0253(12) 0.0250(12) 0.0015(10) 0.0033(10) -0.0006(10) C26 0.0361(17) 0.0406(15) 0.0387(15) 0.0020(12) 0.0051(12) 0.0043(12) C27 0.0420(19) 0.0458(17) 0.0449(17) 0.0047(13) 0.0064(14) 0.0049(13) C28 0.043(2) 0.0462(18) 0.0489(18) 0.0057(14) 0.0055(14) -0.0011(14) C29 0.0455(19) 0.0433(17) 0.0400(17) 0.0021(13) -0.0014(13) -0.0038(13) C30 0.0445(19) 0.0391(16) 0.0418(16) 0.0003(13) 0.0027(13) -0.0001(13) C31 0.0212(13) 0.0217(12) 0.0218(12) 0.0006(9) 0.0024(9) -0.0006(9) C32 0.0287(15) 0.0306(13) 0.0295(13) 0.0004(11) 0.0027(11) -0.0003(11) C33 0.0369(17) 0.0365(15) 0.0362(15) 0.0011(12) 0.0048(12) -0.0028(12) C34 0.0411(18) 0.0409(16) 0.0402(16) 0.0007(13) 0.0036(13) -0.0051(13) C35 0.0424(19) 0.0465(16) 0.0396(17) 0.0009(13) 0.0024(13) -0.0022(13) C36 0.0334(16) 0.0349(14) 0.0319(14) 0.0021(11) 0.0035(11) -0.0015(11) C37 0.0261(14) 0.0278(13) 0.0261(12) 0.0011(10) 0.0021(10) 0.0003(10) C38 0.0330(17) 0.0364(14) 0.0349(14) -0.0003(11) 0.0049(12) 0.0007(11) C39 0.0393(18) 0.0403(16) 0.0386(16) -0.0010(12) 0.0085(13) -0.0008(12) C40 0.0420(18) 0.0431(16) 0.0356(16) 0.0035(13) 0.0074(13) 0.0014(13) C41 0.0413(18) 0.0407(16) 0.0375(15) 0.0043(13) 0.0052(13) 0.0013(12) C42 0.0406(18) 0.0382(15) 0.0373(15) 0.0023(12) 0.0058(12) 0.0016(12) C43 0.0236(14) 0.0259(12) 0.0252(12) 0.0004(10) 0.0020(10) -0.0017(10) C44 0.0412(19) 0.0444(16) 0.0406(16) -0.0041(13) 0.0085(13) -0.0036(13) C45 0.046(2) 0.0447(17) 0.0406(17) -0.0034(13) 0.0054(14) -0.0054(14) C46 0.0390(18) 0.0403(16) 0.0393(16) 0.0022(13) 0.0018(13) -0.0042(12) C47 0.0378(19) 0.0424(17) 0.0506(17) -0.0045(13) 0.0061(13) -0.0024(13) C48 0.0381(18) 0.0394(16) 0.0439(16) -0.0054(13) 0.0049(13) -0.0006(13) C49 0.0324(18) 0.063(2) 0.0536(19) 0.0023(15) -0.0043(14) -0.0221(14) C50 0.041(2) 0.066(2) 0.0539(19) -0.0104(16) -0.0039(15) -0.0211(15) C51 0.043(2) 0.0494(18) 0.0577(19) -0.0051(15) 0.0191(15) -0.0188(14) C52 0.0214(15) 0.0473(17) 0.0493(17) 0.0144(13) 0.0030(12) -0.0043(12) C53 0.0389(19) 0.062(2) 0.057(2) -0.0176(16) 0.0059(15) -0.0176(15) C54 0.0300(17) 0.0383(16) 0.0597(19) 0.0007(13) 0.0156(13) 0.0004(12) C55 0.0340(19) 0.0570(19) 0.0477(17) 0.0049(14) 0.0174(14) 0.0060(13) C56 0.0416(19) 0.0546(18) 0.0494(18) 0.0125(14) 0.0201(14) -0.0043(14) C57 0.066(2) 0.056(2) 0.055(2) -0.0003(16) 0.0210(17) 0.0195(17) C58 0.0345(17) 0.0465(17) 0.0532(18) 0.0113(14) -0.0082(14) 0.0012(13) C59 0.0394(19) 0.0467(18) 0.0568(19) 0.0193(15) -0.0066(14) 0.0013(13) C60 0.0400(19) 0.0465(17) 0.0535(18) 0.0018(14) 0.0039(14) -0.0023(13) S1 0.0467(9) 0.0344(7) 0.0369(7) -0.0010(6) 0.0189(6) 0.0067(6) O17 0.045(3) 0.051(2) 0.040(2) -0.0001(18) 0.0015(18) -0.0011(18) C61 0.074(5) 0.039(3) 0.043(3) -0.004(3) 0.019(3) 0.010(3) C62 0.087(6) 0.071(5) 0.053(4) 0.008(4) -0.003(4) -0.019(4) _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 1.7648(16) . ? Ti1 O1 1.9032(14) . ? Ti1 O3 1.9376(15) . ? Ti1 O5 2.0037(15) . ? Ti1 O7 2.0135(15) . ? Ti1 O2 2.1595(15) . ? Ti1 Ti3 2.8929(6) . ? Ti1 Ti4 3.0802(6) . ? Ti1 Ti2 3.1077(6) . ? Ti2 O14 1.7594(16) . ? Ti2 O4 1.9273(14) . ? Ti2 O2 1.9375(14) . ? Ti2 O6 2.0024(15) . ? Ti2 O9 2.0155(15) . ? Ti2 O1 2.1626(15) . ? Ti2 Ti4 2.8922(6) . ? Ti2 Ti3 3.1003(6) . ? Ti3 O15 1.7758(16) . ? Ti3 O1 1.9114(14) . ? Ti3 O3 1.9282(14) . ? Ti3 O10 2.0130(15) . ? Ti3 O11 2.0262(15) . ? Ti3 O4 2.1372(15) . ? Ti3 Ti4 3.0924(6) . ? Ti4 O16 1.7897(16) . ? Ti4 O2 1.8876(14) . ? Ti4 O4 1.9224(15) . ? Ti4 O12 2.0348(15) . ? Ti4 O8 2.0395(15) . ? Ti4 O3 2.1069(15) . ? P1 O5 1.5166(16) . ? P1 O6 1.5233(16) . ? P1 C7 1.791(2) . ? P1 C1 1.797(2) . ? P2 O7 1.5180(16) . ? P2 O8 1.5211(16) . ? P2 C13 1.795(3) . ? P2 C19 1.800(3) . ? P3 O10 1.5119(16) . ? P3 O9 1.5213(16) . ? P3 C25 1.797(2) . ? P3 C31 1.798(2) . ? P4 O11 1.5193(16) . ? P4 O12 1.5197(16) . ? P4 C37 1.799(2) . ? P4 C43 1.803(2) . ? O13 C49 1.414(3) . ? O14 C52 1.409(3) . ? O15 C55 1.387(3) . ? O16 C58 1.428(3) . ? C1 C2 1.369(4) . ? C1 C6 1.381(4) . ? C2 C3 1.383(4) . ? C3 C4 1.373(4) . ? C4 C5 1.344(4) . ? C5 C6 1.386(4) . ? C7 C12 1.381(4) . ? C7 C8 1.384(4) . ? C8 C9 1.386(4) . ? C9 C10 1.356(4) . ? C10 C11 1.375(4) . ? C11 C12 1.390(4) . ? C13 C14 1.392(4) . ? C13 C18 1.397(4) . ? C14 C15 1.402(4) . ? C15 C16 1.351(4) . ? C16 C17 1.387(4) . ? C17 C18 1.369(4) . ? C19 C24 1.374(4) . ? C19 C20 1.375(4) . ? C20 C21 1.384(4) . ? C21 C22 1.345(4) . ? C22 C23 1.356(4) . ? C23 C24 1.389(4) . ? C25 C30 1.358(4) . ? C25 C26 1.400(4) . ? C26 C27 1.387(4) . ? C27 C28 1.349(4) . ? C28 C29 1.352(4) . ? C29 C30 1.406(4) . ? C31 C36 1.377(3) . ? C31 C32 1.393(3) . ? C32 C33 1.373(4) . ? C33 C34 1.370(4) . ? C34 C35 1.381(4) . ? C35 C36 1.381(4) . ? C37 C42 1.377(4) . ? C37 C38 1.406(4) . ? C38 C39 1.361(4) . ? C39 C40 1.376(4) . ? C40 C41 1.372(4) . ? C41 C42 1.387(4) . ? C43 C44 1.368(4) . ? C43 C48 1.376(4) . ? C44 C45 1.392(4) . ? C45 C46 1.362(4) . ? C46 C47 1.363(4) . ? C47 C48 1.392(4) . ? C49 C51 1.465(4) . ? C49 C50 1.505(4) . ? C52 C54 1.489(4) . ? C52 C53 1.491(4) . ? C55 C57 1.478(4) . ? C55 C56 1.512(4) . ? C58 C59 1.472(4) . ? C58 C60 1.490(4) . ? S1 O17 1.451(4) . ? S1 C61 1.740(6) . ? S1 C62 1.778(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 O1 101.37(7) . . ? O13 Ti1 O3 102.71(7) . . ? O1 Ti1 O3 80.99(6) . . ? O13 Ti1 O5 95.09(7) . . ? O1 Ti1 O5 93.18(6) . . ? O3 Ti1 O5 162.03(7) . . ? O13 Ti1 O7 93.27(7) . . ? O1 Ti1 O7 164.32(7) . . ? O3 Ti1 O7 90.40(6) . . ? O5 Ti1 O7 91.06(6) . . ? O13 Ti1 O2 177.29(7) . . ? O1 Ti1 O2 80.76(6) . . ? O3 Ti1 O2 79.23(6) . . ? O5 Ti1 O2 83.07(6) . . ? O7 Ti1 O2 84.79(6) . . ? O13 Ti1 Ti3 98.14(6) . . ? O1 Ti1 Ti3 40.79(4) . . ? O3 Ti1 Ti3 41.43(4) . . ? O5 Ti1 Ti3 133.76(4) . . ? O7 Ti1 Ti3 131.82(5) . . ? O2 Ti1 Ti3 84.57(4) . . ? O13 Ti1 Ti4 144.34(6) . . ? O1 Ti1 Ti4 83.04(5) . . ? O3 Ti1 Ti4 42.48(4) . . ? O5 Ti1 Ti4 120.17(5) . . ? O7 Ti1 Ti4 81.78(4) . . ? O2 Ti1 Ti4 37.26(4) . . ? Ti3 Ti1 Ti4 62.266(13) . . ? O13 Ti1 Ti2 143.72(5) . . ? O1 Ti1 Ti2 43.34(5) . . ? O3 Ti1 Ti2 82.56(4) . . ? O5 Ti1 Ti2 81.60(5) . . ? O7 Ti1 Ti2 122.79(5) . . ? O2 Ti1 Ti2 38.07(4) . . ? Ti3 Ti1 Ti2 62.096(14) . . ? Ti4 Ti1 Ti2 55.728(13) . . ? O14 Ti2 O4 97.77(7) . . ? O14 Ti2 O2 101.69(7) . . ? O4 Ti2 O2 80.42(6) . . ? O14 Ti2 O6 97.11(7) . . ? O4 Ti2 O6 163.97(7) . . ? O2 Ti2 O6 90.73(6) . . ? O14 Ti2 O9 96.50(7) . . ? O4 Ti2 O9 94.59(6) . . ? O2 Ti2 O9 161.61(7) . . ? O6 Ti2 O9 89.65(6) . . ? O14 Ti2 O1 176.80(7) . . ? O4 Ti2 O1 79.73(6) . . ? O2 Ti2 O1 79.93(6) . . ? O6 Ti2 O1 85.60(6) . . ? O9 Ti2 O1 81.78(6) . . ? O14 Ti2 Ti4 95.66(5) . . ? O4 Ti2 Ti4 41.24(4) . . ? O2 Ti2 Ti4 40.23(4) . . ? O6 Ti2 Ti4 130.92(5) . . ? O9 Ti2 Ti4 135.43(5) . . ? O1 Ti2 Ti4 83.79(4) . . ? O14 Ti2 Ti3 139.67(5) . . ? O4 Ti2 Ti3 42.87(4) . . ? O2 Ti2 Ti3 82.75(5) . . ? O6 Ti2 Ti3 123.07(5) . . ? O9 Ti2 Ti3 81.66(5) . . ? O1 Ti2 Ti3 37.52(4) . . ? Ti4 Ti2 Ti3 62.021(14) . . ? O14 Ti2 Ti1 144.82(5) . . ? O4 Ti2 Ti1 82.54(5) . . ? O2 Ti2 Ti1 43.41(4) . . ? O6 Ti2 Ti1 81.86(5) . . ? O9 Ti2 Ti1 118.61(5) . . ? O1 Ti2 Ti1 37.16(4) . . ? Ti4 Ti2 Ti1 61.655(15) . . ? Ti3 Ti2 Ti1 55.549(13) . . ? O15 Ti3 O1 101.80(7) . . ? O15 Ti3 O3 99.67(7) . . ? O1 Ti3 O3 81.02(6) . . ? O15 Ti3 O10 96.55(7) . . ? O1 Ti3 O10 91.87(6) . . ? O3 Ti3 O10 163.31(7) . . ? O15 Ti3 O11 93.14(7) . . ? O1 Ti3 O11 164.43(7) . . ? O3 Ti3 O11 92.25(6) . . ? O10 Ti3 O11 90.76(6) . . ? O15 Ti3 O4 177.25(7) . . ? O1 Ti3 O4 80.73(6) . . ? O3 Ti3 O4 79.59(6) . . ? O10 Ti3 O4 84.38(6) . . ? O11 Ti3 O4 84.26(6) . . ? O15 Ti3 Ti1 96.42(5) . . ? O1 Ti3 Ti1 40.57(4) . . ? O3 Ti3 Ti1 41.68(4) . . ? O10 Ti3 Ti1 132.36(5) . . ? O11 Ti3 Ti1 133.88(5) . . ? O4 Ti3 Ti1 84.80(4) . . ? O15 Ti3 Ti4 141.01(5) . . ? O1 Ti3 Ti4 82.57(5) . . ? O3 Ti3 Ti4 42.15(4) . . ? O10 Ti3 Ti4 122.20(5) . . ? O11 Ti3 Ti4 83.05(5) . . ? O4 Ti3 Ti4 37.87(4) . . ? Ti1 Ti3 Ti4 61.839(14) . . ? O15 Ti3 Ti2 144.82(5) . . ? O1 Ti3 Ti2 43.56(5) . . ? O3 Ti3 Ti2 82.90(4) . . ? O10 Ti3 Ti2 81.58(5) . . ? O11 Ti3 Ti2 121.93(5) . . ? O4 Ti3 Ti2 37.84(4) . . ? Ti1 Ti3 Ti2 62.355(13) . . ? Ti4 Ti3 Ti2 55.683(13) . . ? O16 Ti4 O2 103.67(7) . . ? O16 Ti4 O4 102.75(7) . . ? O2 Ti4 O4 81.82(6) . . ? O16 Ti4 O12 91.59(7) . . ? O2 Ti4 O12 164.07(7) . . ? O4 Ti4 O12 90.49(6) . . ? O16 Ti4 O8 92.74(7) . . ? O2 Ti4 O8 92.75(6) . . ? O4 Ti4 O8 164.39(6) . . ? O12 Ti4 O8 91.02(6) . . ? O16 Ti4 O3 174.00(7) . . ? O2 Ti4 O3 81.70(6) . . ? O4 Ti4 O3 80.49(6) . . ? O12 Ti4 O3 83.29(6) . . ? O8 Ti4 O3 84.26(6) . . ? O16 Ti4 Ti2 100.27(5) . . ? O2 Ti4 Ti2 41.53(4) . . ? O4 Ti4 Ti2 41.36(4) . . ? O12 Ti4 Ti2 131.79(5) . . ? O8 Ti4 Ti2 134.18(5) . . ? O3 Ti4 Ti2 85.52(4) . . ? O16 Ti4 Ti1 146.41(5) . . ? O2 Ti4 Ti1 43.84(5) . . ? O4 Ti4 Ti1 83.37(4) . . ? O12 Ti4 Ti1 121.63(5) . . ? O8 Ti4 Ti1 82.62(4) . . ? O3 Ti4 Ti1 38.39(4) . . ? Ti2 Ti4 Ti1 62.617(15) . . ? O16 Ti4 Ti3 144.37(5) . . ? O2 Ti4 Ti3 83.73(5) . . ? O4 Ti4 Ti3 43.03(4) . . ? O12 Ti4 Ti3 81.16(5) . . ? O8 Ti4 Ti3 122.04(5) . . ? O3 Ti4 Ti3 37.89(4) . . ? Ti2 Ti4 Ti3 62.297(14) . . ? Ti1 Ti4 Ti3 55.894(13) . . ? O5 P1 O6 114.50(8) . . ? O5 P1 C7 108.41(10) . . ? O6 P1 C7 110.47(11) . . ? O5 P1 C1 108.64(11) . . ? O6 P1 C1 107.39(10) . . ? C7 P1 C1 107.18(11) . . ? O7 P2 O8 114.28(8) . . ? O7 P2 C13 108.10(11) . . ? O8 P2 C13 108.88(10) . . ? O7 P2 C19 107.07(10) . . ? O8 P2 C19 110.31(11) . . ? C13 P2 C19 108.00(12) . . ? O10 P3 O9 115.28(9) . . ? O10 P3 C25 107.88(10) . . ? O9 P3 C25 108.44(10) . . ? O10 P3 C31 107.86(10) . . ? O9 P3 C31 107.80(10) . . ? C25 P3 C31 109.49(11) . . ? O11 P4 O12 114.94(9) . . ? O11 P4 C37 108.61(10) . . ? O12 P4 C37 108.31(10) . . ? O11 P4 C43 108.82(10) . . ? O12 P4 C43 108.16(10) . . ? C37 P4 C43 107.77(11) . . ? Ti1 O1 Ti3 98.64(7) . . ? Ti1 O1 Ti2 99.50(6) . . ? Ti3 O1 Ti2 98.92(6) . . ? Ti4 O2 Ti2 98.24(6) . . ? Ti4 O2 Ti1 98.90(6) . . ? Ti2 O2 Ti1 98.52(6) . . ? Ti3 O3 Ti1 96.89(6) . . ? Ti3 O3 Ti4 99.97(6) . . ? Ti1 O3 Ti4 99.12(6) . . ? Ti4 O4 Ti2 97.40(6) . . ? Ti4 O4 Ti3 99.10(6) . . ? Ti2 O4 Ti3 99.29(6) . . ? P1 O5 Ti1 130.43(9) . . ? P1 O6 Ti2 128.90(9) . . ? P2 O7 Ti1 129.43(9) . . ? P2 O8 Ti4 128.71(9) . . ? P3 O9 Ti2 127.66(9) . . ? P3 O10 Ti3 129.36(9) . . ? P4 O11 Ti3 128.57(9) . . ? P4 O12 Ti4 129.05(9) . . ? C49 O13 Ti1 155.47(19) . . ? C52 O14 Ti2 155.55(16) . . ? C55 O15 Ti3 159.48(17) . . ? C58 O16 Ti4 140.65(18) . . ? C2 C1 C6 120.0(2) . . ? C2 C1 P1 121.35(19) . . ? C6 C1 P1 118.67(19) . . ? C1 C2 C3 119.3(3) . . ? C4 C3 C2 120.3(3) . . ? C5 C4 C3 120.4(3) . . ? C4 C5 C6 120.2(3) . . ? C1 C6 C5 119.7(3) . . ? C12 C7 C8 119.5(2) . . ? C12 C7 P1 120.23(19) . . ? C8 C7 P1 120.27(19) . . ? C7 C8 C9 120.0(3) . . ? C10 C9 C8 120.3(3) . . ? C9 C10 C11 120.5(3) . . ? C10 C11 C12 119.9(3) . . ? C7 C12 C11 119.8(3) . . ? C14 C13 C18 119.1(3) . . ? C14 C13 P2 122.3(2) . . ? C18 C13 P2 118.6(2) . . ? C13 C14 C15 119.4(3) . . ? C16 C15 C14 120.7(3) . . ? C15 C16 C17 120.0(3) . . ? C18 C17 C16 120.6(3) . . ? C17 C18 C13 120.1(3) . . ? C24 C19 C20 118.4(3) . . ? C24 C19 P2 119.5(2) . . ? C20 C19 P2 122.1(2) . . ? C19 C20 C21 119.6(3) . . ? C22 C21 C20 120.7(3) . . ? C21 C22 C23 121.4(3) . . ? C22 C23 C24 118.1(3) . . ? C19 C24 C23 121.8(3) . . ? C30 C25 C26 118.8(2) . . ? C30 C25 P3 122.04(19) . . ? C26 C25 P3 118.99(19) . . ? C27 C26 C25 119.5(3) . . ? C28 C27 C26 120.8(3) . . ? C27 C28 C29 120.7(3) . . ? C28 C29 C30 119.7(3) . . ? C25 C30 C29 120.6(3) . . ? C36 C31 C32 119.5(2) . . ? C36 C31 P3 119.56(18) . . ? C32 C31 P3 120.63(17) . . ? C33 C32 C31 120.5(2) . . ? C34 C33 C32 120.1(3) . . ? C33 C34 C35 119.6(3) . . ? C36 C35 C34 121.0(3) . . ? C31 C36 C35 119.3(2) . . ? C42 C37 C38 119.5(2) . . ? C42 C37 P4 119.79(19) . . ? C38 C37 P4 120.66(19) . . ? C39 C38 C37 119.8(2) . . ? C38 C39 C40 120.3(3) . . ? C41 C40 C39 120.6(3) . . ? C40 C41 C42 119.8(3) . . ? C37 C42 C41 119.8(3) . . ? C44 C43 C48 118.4(2) . . ? C44 C43 P4 123.4(2) . . ? C48 C43 P4 118.19(19) . . ? C43 C44 C45 121.3(3) . . ? C46 C45 C44 119.5(3) . . ? C45 C46 C47 120.1(3) . . ? C46 C47 C48 120.2(3) . . ? C43 C48 C47 120.4(3) . . ? O13 C49 C51 111.6(2) . . ? O13 C49 C50 108.3(2) . . ? C51 C49 C50 116.2(3) . . ? O14 C52 C54 110.1(2) . . ? O14 C52 C53 109.1(2) . . ? C54 C52 C53 112.5(2) . . ? O15 C55 C57 110.3(3) . . ? O15 C55 C56 109.2(2) . . ? C57 C55 C56 113.8(3) . . ? O16 C58 C59 111.4(2) . . ? O16 C58 C60 112.2(2) . . ? C59 C58 C60 114.6(3) . . ? O17 S1 C61 111.1(3) . . ? O17 S1 C62 115.4(3) . . ? C61 S1 C62 100.0(4) . . ? _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 24.20 _diffrn_measured_fraction_theta_full 0.936 _refine_diff_density_max 0.419 _refine_diff_density_min -0.206 _refine_diff_density_rms 0.045