# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email duncan.wass@bristol.ac.uk _publ_contact_author_name 'Duncan Wass' _publ_author_name 'Duncan Wass' data_amc307h2 _database_code_depnum_ccdc_archive 'CCDC 864986' #TrackingRef '- 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H33 B F20 O P Ti' _chemical_formula_weight 1095.42 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pbca ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.5031(8) _cell_length_b 17.8620(8) _cell_length_c 27.4342(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9067.1(7) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9882 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 23.45 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_min 0.09 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_max 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4408 _exptl_absorpt_coefficient_mu 0.345 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6013 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'SADABS V2008/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 153693 _diffrn_reflns_av_R_equivalents 0.1055 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.87 _reflns_number_total 10740 _reflns_number_gt 7590 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker Apex II' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker ShelXTL' _computing_publication_material 'Bruker ShelXTL' _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 'calc w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+8.3455P] 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 10740 _refine_ls_number_parameters 659 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0766 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1092 _refine_ls_wR_factor_gt 0.0933 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.07532(2) 0.09480(2) 0.407688(14) 0.01813(9) Uani 1 1 d . . . P1 P 0.32510(3) 0.15230(3) 0.39665(2) 0.02410(14) Uani 1 1 d . . . O1 O 0.16486(8) 0.13981(8) 0.38532(6) 0.0228(3) Uani 1 1 d . . . C1 C 0.04175(13) 0.09653(13) 0.49087(8) 0.0260(5) Uani 1 1 d . . . H1 H 0.0466 0.0540 0.5143 0.031 Uiso 1 1 calc R . . C2 C -0.02024(13) 0.11427(13) 0.46349(9) 0.0254(5) Uani 1 1 d . . . H2 H -0.0669 0.0861 0.4641 0.031 Uiso 1 1 calc R . . C3 C -0.00792(13) 0.18262(13) 0.43891(9) 0.0262(5) Uani 1 1 d . . . H3 H -0.0444 0.2113 0.4195 0.031 Uiso 1 1 calc R . . C4 C 0.06141(14) 0.20808(13) 0.45230(9) 0.0266(5) Uani 1 1 d . . . H4 H 0.0830 0.2576 0.4436 0.032 Uiso 1 1 calc R . . C5 C 0.09181(13) 0.15465(14) 0.48416(8) 0.0269(5) Uani 1 1 d . . . H5 H 0.1389 0.1600 0.5018 0.032 Uiso 1 1 calc R . . C6 C 0.07793(14) 0.03885(15) 0.32912(9) 0.0332(6) Uani 1 1 d . . . H6 H 0.1025 0.0597 0.2996 0.040 Uiso 1 1 calc R . . C7 C 0.10798(14) -0.01276(14) 0.36221(9) 0.0299(6) Uani 1 1 d . . . H7 H 0.1575 -0.0349 0.3601 0.036 Uiso 1 1 calc R . . C8 C 0.05383(13) -0.03380(13) 0.39549(9) 0.0283(5) Uani 1 1 d . . . H8 H 0.0580 -0.0739 0.4208 0.034 Uiso 1 1 calc R . . C9 C -0.00967(13) 0.00444(14) 0.38274(9) 0.0275(5) Uani 1 1 d . . . H9 H -0.0583 -0.0037 0.3977 0.033 Uiso 1 1 calc R . . C10 C 0.00501(14) 0.05074(15) 0.34243(9) 0.0322(6) Uani 1 1 d . . . H10 H -0.0313 0.0805 0.3236 0.039 Uiso 1 1 calc R . . C11 C 0.19152(12) 0.20349(12) 0.36772(8) 0.0191(4) Uani 1 1 d . . . C12 C 0.14626(12) 0.25646(13) 0.34579(8) 0.0209(5) Uani 1 1 d . . . H12 H 0.0958 0.2470 0.3440 0.025 Uiso 1 1 calc R . . C13 C 0.17348(12) 0.32234(13) 0.32662(8) 0.0223(5) Uani 1 1 d . . . H13 H 0.1416 0.3576 0.3121 0.027 Uiso 1 1 calc R . . C14 C 0.24724(13) 0.33743(13) 0.32839(8) 0.0237(5) Uani 1 1 d . . . H14 H 0.2658 0.3826 0.3151 0.028 Uiso 1 1 calc R . . C15 C 0.29310(12) 0.28601(13) 0.34962(8) 0.0228(5) Uani 1 1 d . . . H15 H 0.3435 0.2961 0.3508 0.027 Uiso 1 1 calc R . . C16 C 0.26650(12) 0.21887(12) 0.36956(8) 0.0198(4) Uani 1 1 d . . . C17 C 0.36957(13) 0.09589(14) 0.34892(11) 0.0348(6) Uani 1 1 d . . . C18 C 0.42080(16) 0.03788(17) 0.37140(15) 0.0581(10) Uani 1 1 d . . . H18A H 0.4364 0.0025 0.3462 0.087 Uiso 1 1 calc R . . H18B H 0.3956 0.0107 0.3973 0.087 Uiso 1 1 calc R . . H18C H 0.4631 0.0634 0.3850 0.087 Uiso 1 1 calc R . . C19 C 0.30702(15) 0.05524(17) 0.32340(13) 0.0486(8) Uani 1 1 d . . . H19A H 0.3261 0.0246 0.2967 0.073 Uiso 1 1 calc R . . H19B H 0.2730 0.0922 0.3103 0.073 Uiso 1 1 calc R . . H19C H 0.2820 0.0231 0.3469 0.073 Uiso 1 1 calc R . . C20 C 0.41000(17) 0.14533(17) 0.31240(12) 0.0482(8) Uani 1 1 d . . . H20A H 0.4493 0.1717 0.3291 0.072 Uiso 1 1 calc R . . H20B H 0.3765 0.1819 0.2983 0.072 Uiso 1 1 calc R . . H20C H 0.4301 0.1141 0.2864 0.072 Uiso 1 1 calc R . . C21 C 0.37985(14) 0.19416(16) 0.44607(9) 0.0329(6) Uani 1 1 d . . . C22 C 0.40135(16) 0.1314(2) 0.48123(12) 0.0547(9) Uani 1 1 d . . . H22A H 0.4307 0.0943 0.4639 0.082 Uiso 1 1 calc R . . H22B H 0.3577 0.1073 0.4941 0.082 Uiso 1 1 calc R . . H22C H 0.4294 0.1525 0.5082 0.082 Uiso 1 1 calc R . . C23 C 0.33015(15) 0.2503(2) 0.47281(10) 0.0464(8) Uani 1 1 d . . . H23A H 0.2859 0.2247 0.4833 0.070 Uiso 1 1 calc R . . H23B H 0.3176 0.2914 0.4507 0.070 Uiso 1 1 calc R . . H23C H 0.3554 0.2703 0.5014 0.070 Uiso 1 1 calc R . . C24 C 0.44772(13) 0.23441(15) 0.42731(10) 0.0329(6) Uani 1 1 d . . . H24A H 0.4735 0.2571 0.4548 0.049 Uiso 1 1 calc R . . H24B H 0.4336 0.2736 0.4042 0.049 Uiso 1 1 calc R . . H24C H 0.4794 0.1983 0.4110 0.049 Uiso 1 1 calc R . . H25 H 0.2825(15) 0.1028(15) 0.4206(10) 0.040(8) Uiso 1 1 d . . . F1 F 0.09513(7) 0.08651(7) 0.09761(5) 0.0226(3) Uani 1 1 d . . . F2 F 0.07382(8) 0.14190(9) 0.00891(5) 0.0366(4) Uani 1 1 d . . . F3 F 0.17437(9) 0.12089(10) -0.06294(5) 0.0433(4) Uani 1 1 d . . . F4 F 0.29683(9) 0.04155(9) -0.04263(5) 0.0412(4) Uani 1 1 d . . . F5 F 0.32018(7) -0.01323(8) 0.04517(5) 0.0289(3) Uani 1 1 d . . . F6 F 0.34102(7) 0.00792(8) 0.20792(5) 0.0318(3) Uani 1 1 d . . . F7 F 0.44185(8) -0.09376(11) 0.21883(7) 0.0566(5) Uani 1 1 d . . . F8 F 0.44745(10) -0.21675(11) 0.15921(8) 0.0707(7) Uani 1 1 d . . . F9 F 0.34278(11) -0.23595(9) 0.08990(6) 0.0601(6) Uani 1 1 d . . . F10 F 0.23824(8) -0.13437(8) 0.07909(5) 0.0342(3) Uani 1 1 d . . . F11 F 0.08490(7) -0.06486(7) 0.07950(5) 0.0267(3) Uani 1 1 d . . . F12 F -0.01112(7) -0.15591(8) 0.11771(5) 0.0291(3) Uani 1 1 d . . . F13 F -0.00411(7) -0.19604(7) 0.21388(5) 0.0242(3) Uani 1 1 d . . . F14 F 0.09994(7) -0.13419(7) 0.27186(5) 0.0231(3) Uani 1 1 d . . . F15 F 0.19732(7) -0.04008(7) 0.23435(4) 0.0212(3) Uani 1 1 d . . . F16 F 0.11240(7) 0.08588(7) 0.20319(5) 0.0221(3) Uani 1 1 d . . . F17 F 0.13371(8) 0.22048(7) 0.23894(5) 0.0309(3) Uani 1 1 d . . . F18 F 0.25769(9) 0.29815(7) 0.21911(5) 0.0360(4) Uani 1 1 d . . . F19 F 0.35994(8) 0.23486(8) 0.15982(6) 0.0378(4) Uani 1 1 d . . . F20 F 0.33912(7) 0.09941(7) 0.12221(5) 0.0268(3) Uani 1 1 d . . . C25 C 0.20682(11) 0.03011(11) 0.07654(8) 0.0172(4) Uani 1 1 d . . . C26 C 0.14672(11) 0.07266(12) 0.06353(8) 0.0191(4) Uani 1 1 d . . . C27 C 0.13459(12) 0.10269(13) 0.01829(9) 0.0252(5) Uani 1 1 d . . . C28 C 0.18483(14) 0.09220(14) -0.01799(9) 0.0292(5) Uani 1 1 d . . . C29 C 0.24621(13) 0.05206(14) -0.00743(8) 0.0270(5) Uani 1 1 d . . . C30 C 0.25624(12) 0.02311(12) 0.03863(8) 0.0214(5) Uani 1 1 d . . . C31 C 0.28475(11) -0.05623(12) 0.14175(8) 0.0210(5) Uani 1 1 d . . . C32 C 0.33806(12) -0.05122(14) 0.17702(9) 0.0277(5) Uani 1 1 d . . . C33 C 0.39199(13) -0.10381(17) 0.18365(11) 0.0392(7) Uani 1 1 d . . . C34 C 0.39465(16) -0.16562(17) 0.15397(12) 0.0459(8) Uani 1 1 d . . . C35 C 0.34234(17) -0.17473(15) 0.11879(11) 0.0409(7) Uani 1 1 d . . . C36 C 0.28890(14) -0.12130(13) 0.11387(9) 0.0284(5) Uani 1 1 d . . . C37 C 0.14726(11) -0.04684(11) 0.15480(8) 0.0154(4) Uani 1 1 d . . . C38 C 0.09181(12) -0.07844(11) 0.12796(8) 0.0183(4) Uani 1 1 d . . . C39 C 0.04052(11) -0.12629(12) 0.14715(8) 0.0191(4) Uani 1 1 d . . . C40 C 0.04285(11) -0.14582(11) 0.19544(8) 0.0177(4) Uani 1 1 d . . . C41 C 0.09573(11) -0.11502(11) 0.22434(7) 0.0171(4) Uani 1 1 d . . . C42 C 0.14580(11) -0.06738(11) 0.20377(8) 0.0161(4) Uani 1 1 d . . . C43 C 0.22650(11) 0.08320(11) 0.16205(8) 0.0170(4) Uani 1 1 d . . . C44 C 0.17619(12) 0.11860(12) 0.19165(8) 0.0186(4) Uani 1 1 d . . . C45 C 0.18566(13) 0.18971(12) 0.21112(8) 0.0224(5) Uani 1 1 d . . . C46 C 0.24815(14) 0.22891(12) 0.20090(8) 0.0260(5) Uani 1 1 d . . . C47 C 0.29891(13) 0.19733(13) 0.17112(9) 0.0262(5) Uani 1 1 d . . . C48 C 0.28687(12) 0.12643(12) 0.15234(8) 0.0213(5) Uani 1 1 d . . . B1 B 0.21625(13) 0.00243(13) 0.13368(9) 0.0164(5) Uani 1 1 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 0.01325(18) 0.01763(18) 0.0235(2) -0.00093(15) -0.00008(16) -0.00159(15) P1 0.0129(3) 0.0251(3) 0.0343(3) 0.0064(3) -0.0015(2) -0.0016(2) O1 0.0142(8) 0.0206(8) 0.0337(9) 0.0006(7) 0.0018(7) -0.0018(6) C1 0.0296(13) 0.0259(12) 0.0226(11) 0.0008(10) 0.0048(10) 0.0011(10) C2 0.0203(12) 0.0252(12) 0.0308(13) -0.0034(10) 0.0061(10) 0.0000(9) C3 0.0237(12) 0.0263(12) 0.0285(12) -0.0024(10) 0.0021(10) 0.0069(10) C4 0.0332(14) 0.0183(11) 0.0283(12) -0.0059(9) 0.0052(10) -0.0035(10) C5 0.0245(13) 0.0336(13) 0.0226(12) -0.0065(10) -0.0011(10) -0.0007(10) C6 0.0320(14) 0.0442(15) 0.0233(12) -0.0107(11) 0.0047(11) -0.0150(12) C7 0.0232(12) 0.0279(13) 0.0386(14) -0.0162(11) 0.0036(11) -0.0012(10) C8 0.0261(13) 0.0218(11) 0.0369(14) -0.0053(10) -0.0015(11) -0.0033(10) C9 0.0189(12) 0.0315(13) 0.0322(13) -0.0083(10) 0.0011(10) -0.0088(10) C10 0.0283(14) 0.0394(14) 0.0290(13) -0.0036(11) -0.0092(11) -0.0044(11) C11 0.0153(10) 0.0208(11) 0.0212(11) -0.0052(8) 0.0023(9) -0.0024(8) C12 0.0125(10) 0.0266(11) 0.0238(11) -0.0036(9) -0.0006(9) -0.0005(9) C13 0.0202(12) 0.0250(11) 0.0218(11) 0.0001(9) -0.0010(9) 0.0050(9) C14 0.0254(12) 0.0234(11) 0.0222(11) 0.0021(9) 0.0013(10) -0.0031(9) C15 0.0156(11) 0.0294(12) 0.0233(11) -0.0009(9) 0.0012(9) -0.0059(9) C16 0.0147(11) 0.0235(11) 0.0214(11) -0.0009(9) -0.0001(9) 0.0006(9) C17 0.0190(12) 0.0283(13) 0.0573(17) -0.0073(12) 0.0036(12) 0.0013(10) C18 0.0268(15) 0.0384(17) 0.109(3) -0.0026(18) -0.0034(18) 0.0126(13) C19 0.0306(15) 0.0455(17) 0.070(2) -0.0263(16) 0.0059(15) -0.0007(13) C20 0.0410(17) 0.0466(17) 0.0569(19) -0.0132(15) 0.0199(15) -0.0003(14) C21 0.0226(13) 0.0456(16) 0.0304(13) 0.0116(12) -0.0068(11) -0.0054(11) C22 0.0343(16) 0.075(2) 0.0551(19) 0.0390(17) -0.0171(15) -0.0183(16) C23 0.0325(15) 0.077(2) 0.0298(14) -0.0116(14) -0.0028(12) -0.0029(15) C24 0.0214(12) 0.0390(14) 0.0384(14) 0.0078(12) -0.0064(11) -0.0088(11) F1 0.0155(6) 0.0273(7) 0.0249(7) 0.0027(5) 0.0045(5) 0.0049(5) F2 0.0247(8) 0.0481(9) 0.0372(8) 0.0186(7) 0.0013(6) 0.0134(7) F3 0.0421(9) 0.0599(10) 0.0277(8) 0.0199(7) 0.0043(7) 0.0080(8) F4 0.0389(9) 0.0533(10) 0.0314(8) 0.0087(7) 0.0191(7) 0.0104(8) F5 0.0197(7) 0.0338(8) 0.0332(8) 0.0063(6) 0.0098(6) 0.0101(6) F6 0.0211(7) 0.0382(8) 0.0361(8) 0.0097(7) -0.0097(6) -0.0053(6) F7 0.0188(8) 0.0808(13) 0.0702(12) 0.0444(10) -0.0068(8) 0.0067(8) F8 0.0536(11) 0.0749(13) 0.0837(14) 0.0466(11) 0.0360(10) 0.0528(10) F9 0.0919(15) 0.0303(9) 0.0581(11) 0.0087(8) 0.0393(11) 0.0332(9) F10 0.0458(9) 0.0225(7) 0.0344(8) -0.0051(6) 0.0083(7) 0.0030(6) F11 0.0308(8) 0.0315(7) 0.0178(6) -0.0009(5) -0.0009(6) -0.0127(6) F12 0.0256(7) 0.0335(8) 0.0280(7) -0.0045(6) -0.0031(6) -0.0154(6) F13 0.0191(7) 0.0230(7) 0.0305(7) 0.0020(5) 0.0037(6) -0.0085(5) F14 0.0203(7) 0.0266(7) 0.0225(6) 0.0066(5) -0.0005(5) -0.0028(5) F15 0.0152(6) 0.0246(6) 0.0239(6) 0.0032(5) -0.0055(5) -0.0049(5) F16 0.0171(6) 0.0196(6) 0.0297(7) -0.0034(5) 0.0065(5) -0.0031(5) F17 0.0410(9) 0.0238(7) 0.0280(7) -0.0090(6) 0.0084(6) -0.0012(6) F18 0.0519(10) 0.0219(7) 0.0341(8) -0.0091(6) 0.0009(7) -0.0160(7) F19 0.0326(8) 0.0339(8) 0.0469(9) -0.0032(7) 0.0041(7) -0.0222(7) F20 0.0159(7) 0.0269(7) 0.0376(8) 0.0000(6) 0.0056(6) -0.0045(6) C25 0.0160(10) 0.0137(9) 0.0220(10) -0.0003(8) 0.0035(9) -0.0021(8) C26 0.0136(11) 0.0210(11) 0.0228(11) 0.0000(9) 0.0039(9) 0.0003(8) C27 0.0171(11) 0.0270(12) 0.0314(13) 0.0063(10) 0.0000(10) 0.0040(9) C28 0.0298(13) 0.0350(13) 0.0227(12) 0.0098(10) 0.0033(10) 0.0003(11) C29 0.0227(12) 0.0329(13) 0.0253(12) 0.0029(10) 0.0105(10) 0.0014(10) C30 0.0160(11) 0.0199(11) 0.0283(12) 0.0011(9) 0.0032(9) 0.0025(9) C31 0.0132(10) 0.0206(11) 0.0291(12) 0.0067(9) 0.0063(9) 0.0030(9) C32 0.0145(11) 0.0316(13) 0.0369(14) 0.0135(11) 0.0037(10) 0.0008(10) C33 0.0149(12) 0.0530(18) 0.0497(17) 0.0295(14) 0.0055(12) 0.0074(12) C34 0.0314(15) 0.0451(17) 0.0611(19) 0.0301(15) 0.0249(15) 0.0268(13) C35 0.0497(18) 0.0274(13) 0.0457(16) 0.0131(12) 0.0275(15) 0.0188(12) C36 0.0304(14) 0.0236(12) 0.0311(13) 0.0074(10) 0.0102(11) 0.0057(10) C37 0.0134(10) 0.0111(9) 0.0217(10) -0.0013(8) 0.0010(8) 0.0022(8) C38 0.0184(11) 0.0167(10) 0.0199(10) -0.0010(8) 0.0021(9) -0.0007(8) C39 0.0150(11) 0.0180(10) 0.0242(11) -0.0058(9) -0.0009(9) -0.0019(8) C40 0.0121(10) 0.0143(10) 0.0267(11) -0.0013(8) 0.0040(9) -0.0021(8) C41 0.0161(10) 0.0172(10) 0.0179(10) 0.0020(8) 0.0012(8) 0.0036(8) C42 0.0101(10) 0.0127(9) 0.0254(11) -0.0020(8) -0.0024(8) 0.0009(8) C43 0.0136(10) 0.0176(10) 0.0198(10) 0.0024(8) -0.0030(8) -0.0010(8) C44 0.0167(11) 0.0183(10) 0.0208(10) 0.0024(8) -0.0014(9) -0.0036(8) C45 0.0282(12) 0.0191(11) 0.0200(11) -0.0024(9) 0.0011(10) 0.0010(9) C46 0.0370(14) 0.0173(11) 0.0238(11) -0.0031(9) -0.0046(10) -0.0076(10) C47 0.0230(12) 0.0255(12) 0.0301(13) 0.0019(10) -0.0023(10) -0.0129(10) C48 0.0168(11) 0.0235(11) 0.0236(11) 0.0013(9) -0.0006(9) -0.0020(9) B1 0.0112(11) 0.0168(11) 0.0210(12) 0.0000(9) 0.0008(9) 0.0004(9) _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 O1 1.9410(15) . ? Ti1 C10 2.349(2) . ? Ti1 C8 2.355(2) . ? Ti1 C9 2.355(2) . ? Ti1 C3 2.359(2) . ? Ti1 C2 2.364(2) . ? Ti1 C1 2.365(2) . ? Ti1 C7 2.369(2) . ? Ti1 C5 2.374(2) . ? Ti1 C6 2.376(2) . ? Ti1 C4 2.379(2) . ? P1 C16 1.772(2) . ? P1 C17 1.846(3) . ? P1 C21 1.850(3) . ? O1 C11 1.331(3) . ? C1 C5 1.403(3) . ? C1 C2 1.407(3) . ? C2 C3 1.413(3) . ? C3 C4 1.410(3) . ? C4 C5 1.411(3) . ? C6 C7 1.408(4) . ? C6 C10 1.414(4) . ? C7 C8 1.407(4) . ? C8 C9 1.403(3) . ? C9 C10 1.407(4) . ? C11 C12 1.399(3) . ? C11 C16 1.415(3) . ? C12 C13 1.384(3) . ? C13 C14 1.392(3) . ? C14 C15 1.379(3) . ? C15 C16 1.407(3) . ? C17 C20 1.531(4) . ? C17 C19 1.535(4) . ? C17 C18 1.534(4) . ? C21 C22 1.531(4) . ? C21 C24 1.536(3) . ? C21 C23 1.545(4) . ? F1 C26 1.359(2) . ? F2 C27 1.349(3) . ? F3 C28 1.349(3) . ? F4 C29 1.358(3) . ? F5 C30 1.361(2) . ? F6 C32 1.356(3) . ? F7 C33 1.347(3) . ? F8 C34 1.345(3) . ? F9 C35 1.351(3) . ? F10 C36 1.358(3) . ? F11 C38 1.357(2) . ? F12 C39 1.358(2) . ? F13 C40 1.347(2) . ? F14 C41 1.350(2) . ? F15 C42 1.360(2) . ? F16 C44 1.355(2) . ? F17 C45 1.345(3) . ? F18 C46 1.345(2) . ? F19 C47 1.349(3) . ? F20 C48 1.361(3) . ? C25 C30 1.391(3) . ? C25 C26 1.393(3) . ? C25 B1 1.653(3) . ? C26 C27 1.371(3) . ? C27 C28 1.375(3) . ? C28 C29 1.374(3) . ? C29 C30 1.378(3) . ? C31 C32 1.385(3) . ? C31 C36 1.393(3) . ? C31 B1 1.659(3) . ? C32 C33 1.382(3) . ? C33 C34 1.373(5) . ? C34 C35 1.376(5) . ? C35 C36 1.381(3) . ? C37 C38 1.383(3) . ? C37 C42 1.393(3) . ? C37 B1 1.655(3) . ? C38 C39 1.381(3) . ? C39 C40 1.371(3) . ? C40 C41 1.374(3) . ? C41 C42 1.379(3) . ? C43 C48 1.384(3) . ? C43 C44 1.388(3) . ? C43 B1 1.650(3) . ? C44 C45 1.389(3) . ? C45 C46 1.380(3) . ? C46 C47 1.367(3) . ? C47 C48 1.385(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 O1 Ti1 C10 111.75(8) . . ? O1 Ti1 C8 120.21(8) . . ? C10 Ti1 C8 58.09(9) . . ? O1 Ti1 C9 139.64(8) . . ? C10 Ti1 C9 34.82(9) . . ? C8 Ti1 C9 34.67(9) . . ? O1 Ti1 C3 113.36(8) . . ? C10 Ti1 C3 97.93(9) . . ? C8 Ti1 C3 126.15(9) . . ? C9 Ti1 C3 97.19(9) . . ? O1 Ti1 C2 141.45(8) . . ? C10 Ti1 C2 97.39(9) . . ? C8 Ti1 C2 96.27(9) . . ? C9 Ti1 C2 77.85(8) . . ? C3 Ti1 C2 34.82(8) . . ? O1 Ti1 C1 121.58(8) . . ? C10 Ti1 C1 126.47(9) . . ? C8 Ti1 C1 96.06(9) . . ? C9 Ti1 C1 96.54(8) . . ? C3 Ti1 C1 57.97(8) . . ? C2 Ti1 C1 34.62(8) . . ? O1 Ti1 C7 87.23(8) . . ? C10 Ti1 C7 57.87(9) . . ? C8 Ti1 C7 34.64(9) . . ? C9 Ti1 C7 57.42(8) . . ? C3 Ti1 C7 153.75(9) . . ? C2 Ti1 C7 130.62(9) . . ? C1 Ti1 C7 125.86(9) . . ? O1 Ti1 C5 89.03(8) . . ? C10 Ti1 C5 153.58(9) . . ? C8 Ti1 C5 125.91(9) . . ? C9 Ti1 C5 130.63(9) . . ? C3 Ti1 C5 57.57(8) . . ? C2 Ti1 C5 57.17(8) . . ? C1 Ti1 C5 34.45(8) . . ? C7 Ti1 C5 142.91(9) . . ? O1 Ti1 C6 82.53(8) . . ? C10 Ti1 C6 34.82(9) . . ? C8 Ti1 C6 57.61(9) . . ? C9 Ti1 C6 57.44(8) . . ? C3 Ti1 C6 128.48(9) . . ? C2 Ti1 C6 131.63(9) . . ? C1 Ti1 C6 152.37(9) . . ? C7 Ti1 C6 34.52(9) . . ? C5 Ti1 C6 171.19(9) . . ? O1 Ti1 C4 84.41(8) . . ? C10 Ti1 C4 128.11(9) . . ? C8 Ti1 C4 152.19(9) . . ? C9 Ti1 C4 131.31(9) . . ? C3 Ti1 C4 34.62(8) . . ? C2 Ti1 C4 57.38(8) . . ? C1 Ti1 C4 57.59(8) . . ? C7 Ti1 C4 171.25(9) . . ? C5 Ti1 C4 34.54(8) . . ? C6 Ti1 C4 145.75(9) . . ? C16 P1 C17 109.97(12) . . ? C16 P1 C21 111.78(11) . . ? C17 P1 C21 119.76(12) . . ? C11 O1 Ti1 141.75(14) . . ? C5 C1 C2 107.5(2) . . ? C5 C1 Ti1 73.13(13) . . ? C2 C1 Ti1 72.66(13) . . ? C1 C2 C3 108.5(2) . . ? C1 C2 Ti1 72.72(13) . . ? C3 C2 Ti1 72.40(13) . . ? C4 C3 C2 107.5(2) . . ? C4 C3 Ti1 73.44(13) . . ? C2 C3 Ti1 72.78(13) . . ? C3 C4 C5 107.8(2) . . ? C3 C4 Ti1 71.94(13) . . ? C5 C4 Ti1 72.56(13) . . ? C1 C5 C4 108.6(2) . . ? C1 C5 Ti1 72.42(13) . . ? C4 C5 Ti1 72.90(13) . . ? C7 C6 C10 108.0(2) . . ? C7 C6 Ti1 72.46(14) . . ? C10 C6 Ti1 71.53(14) . . ? C8 C7 C6 108.2(2) . . ? C8 C7 Ti1 72.13(13) . . ? C6 C7 Ti1 73.02(14) . . ? C9 C8 C7 107.7(2) . . ? C9 C8 Ti1 72.67(13) . . ? C7 C8 Ti1 73.23(14) . . ? C8 C9 C10 108.7(2) . . ? C8 C9 Ti1 72.66(13) . . ? C10 C9 Ti1 72.34(14) . . ? C9 C10 C6 107.4(2) . . ? C9 C10 Ti1 72.84(14) . . ? C6 C10 Ti1 73.66(14) . . ? O1 C11 C12 120.80(19) . . ? O1 C11 C16 121.1(2) . . ? C12 C11 C16 118.1(2) . . ? C13 C12 C11 121.4(2) . . ? C12 C13 C14 120.5(2) . . ? C15 C14 C13 119.3(2) . . ? C14 C15 C16 121.1(2) . . ? C15 C16 C11 119.6(2) . . ? C15 C16 P1 121.39(17) . . ? C11 C16 P1 118.98(17) . . ? C20 C17 C19 110.1(3) . . ? C20 C17 C18 110.5(2) . . ? C19 C17 C18 109.2(2) . . ? C20 C17 P1 111.55(18) . . ? C19 C17 P1 104.22(17) . . ? C18 C17 P1 111.0(2) . . ? C22 C21 C24 110.0(2) . . ? C22 C21 C23 109.3(2) . . ? C24 C21 C23 110.0(2) . . ? C22 C21 P1 107.9(2) . . ? C24 C21 P1 113.03(18) . . ? C23 C21 P1 106.51(17) . . ? C30 C25 C26 112.48(19) . . ? C30 C25 B1 127.81(19) . . ? C26 C25 B1 119.36(18) . . ? F1 C26 C27 115.89(19) . . ? F1 C26 C25 118.93(19) . . ? C27 C26 C25 125.2(2) . . ? F2 C27 C26 120.8(2) . . ? F2 C27 C28 119.8(2) . . ? C26 C27 C28 119.4(2) . . ? F3 C28 C27 120.9(2) . . ? F3 C28 C29 120.6(2) . . ? C27 C28 C29 118.5(2) . . ? F4 C29 C28 119.5(2) . . ? F4 C29 C30 120.5(2) . . ? C28 C29 C30 120.0(2) . . ? F5 C30 C29 114.65(19) . . ? F5 C30 C25 121.04(19) . . ? C29 C30 C25 124.3(2) . . ? C32 C31 C36 113.5(2) . . ? C32 C31 B1 126.6(2) . . ? C36 C31 B1 119.7(2) . . ? F6 C32 C33 114.7(2) . . ? F6 C32 C31 121.1(2) . . ? C33 C32 C31 124.2(3) . . ? F7 C33 C34 120.5(2) . . ? F7 C33 C32 119.9(3) . . ? C34 C33 C32 119.6(3) . . ? F8 C34 C35 120.4(3) . . ? F8 C34 C33 120.6(3) . . ? C35 C34 C33 119.1(2) . . ? F9 C35 C34 120.2(2) . . ? F9 C35 C36 120.4(3) . . ? C34 C35 C36 119.4(3) . . ? F10 C36 C35 116.4(2) . . ? F10 C36 C31 119.4(2) . . ? C35 C36 C31 124.2(3) . . ? C38 C37 C42 113.05(19) . . ? C38 C37 B1 127.06(19) . . ? C42 C37 B1 119.52(18) . . ? F11 C38 C39 114.78(18) . . ? F11 C38 C37 121.22(18) . . ? C39 C38 C37 124.0(2) . . ? F12 C39 C40 119.85(19) . . ? F12 C39 C38 119.84(19) . . ? C40 C39 C38 120.3(2) . . ? F13 C40 C39 120.80(19) . . ? F13 C40 C41 120.59(19) . . ? C39 C40 C41 118.57(19) . . ? F14 C41 C40 119.78(19) . . ? F14 C41 C42 120.86(19) . . ? C40 C41 C42 119.29(19) . . ? F15 C42 C41 116.09(18) . . ? F15 C42 C37 119.13(18) . . ? C41 C42 C37 124.78(19) . . ? C48 C43 C44 113.57(19) . . ? C48 C43 B1 119.33(19) . . ? C44 C43 B1 126.67(19) . . ? F16 C44 C45 114.49(19) . . ? F16 C44 C43 121.64(18) . . ? C45 C44 C43 123.9(2) . . ? F17 C45 C46 120.44(19) . . ? F17 C45 C44 120.1(2) . . ? C46 C45 C44 119.4(2) . . ? F18 C46 C47 120.7(2) . . ? F18 C46 C45 120.0(2) . . ? C47 C46 C45 119.2(2) . . ? F19 C47 C46 120.5(2) . . ? F19 C47 C48 120.2(2) . . ? C46 C47 C48 119.3(2) . . ? F20 C48 C43 119.52(19) . . ? F20 C48 C47 115.85(19) . . ? C43 C48 C47 124.6(2) . . ? C43 B1 C25 101.42(16) . . ? C43 B1 C37 112.85(17) . . ? C25 B1 C37 114.18(17) . . ? C43 B1 C31 113.66(18) . . ? C25 B1 C31 113.33(17) . . ? C37 B1 C31 101.93(16) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.361 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.062 # Attachment '- 6.cif' data_amc309 _database_code_depnum_ccdc_archive 'CCDC 864987' #TrackingRef '- 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H32 O P Ti' _chemical_formula_sum 'C24 H32 O P Ti' _chemical_formula_weight 415.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2191 1.8069 '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 _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.599(2) _cell_length_b 10.528(3) _cell_length_c 10.456(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.260(6) _cell_angle_gamma 90.00 _cell_volume 1050.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9870 _cell_measurement_theta_min 4.25 _cell_measurement_theta_max 66.19 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 442 _exptl_absorpt_coefficient_mu 4.239 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4950 _exptl_absorpt_correction_T_max 0.7528 _exptl_absorpt_process_details 'SADABS V2008/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Microstar CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12230 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.25 _diffrn_reflns_theta_max 66.36 _reflns_number_total 3587 _reflns_number_gt 3560 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker ShelXTL' _computing_publication_material 'Bruker ShelXTL' _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 'calc w=1/[\s^2^(Fo^2^)+(0.0810P)^2^+0.2542P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.005(5) _refine_ls_number_reflns 3587 _refine_ls_number_parameters 251 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.1004 _refine_ls_wR_factor_gt 0.1000 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.71898(4) 0.77487(3) 0.13432(3) 0.01242(14) Uani 1 1 d . . . P1 P 0.71193(6) 0.56617(5) 0.31550(5) 0.01259(16) Uani 1 1 d . . . O1 O 0.53412(17) 0.68096(17) 0.10427(15) 0.0152(3) Uani 1 1 d . . . C1 C 0.8822(3) 0.6431(3) 0.0347(2) 0.0211(5) Uani 1 1 d . . . H1 H 0.9253 0.5625 0.0709 0.025 Uiso 1 1 calc R . . C2 C 0.9415(2) 0.7657(3) 0.0502(2) 0.0218(5) Uani 1 1 d . . . H2 H 1.0343 0.7867 0.0986 0.026 Uiso 1 1 calc R . . C3 C 0.8562(3) 0.8500(3) -0.0286(2) 0.0216(5) Uani 1 1 d . . . H3 H 0.8784 0.9409 -0.0450 0.026 Uiso 1 1 calc R . . C4 C 0.7420(2) 0.7819(3) -0.0895(2) 0.0205(5) Uani 1 1 d . . . H4 H 0.6705 0.8155 -0.1579 0.025 Uiso 1 1 calc R . . C5 C 0.7588(3) 0.6526(3) -0.0519(2) 0.0214(5) Uani 1 1 d . . . H5 H 0.7002 0.5799 -0.0882 0.026 Uiso 1 1 calc R . . C6 C 0.7911(3) 0.9852(3) 0.2002(3) 0.0232(6) Uani 1 1 d . . . H6 H 0.8788 1.0284 0.1799 0.028 Uiso 1 1 calc R . . C7 C 0.6576(3) 0.9975(2) 0.1290(3) 0.0228(6) Uani 1 1 d . . . H7 H 0.6349 1.0502 0.0499 0.027 Uiso 1 1 calc R . . C8 C 0.5611(3) 0.9358(2) 0.1979(2) 0.0193(5) Uani 1 1 d . . . H8 H 0.4571 0.9363 0.1755 0.023 Uiso 1 1 calc R . . C9 C 0.6323(3) 0.8821(2) 0.3089(2) 0.0184(5) Uani 1 1 d . . . H9 H 0.5879 0.8412 0.3806 0.022 Uiso 1 1 calc R . . C10 C 0.7766(3) 0.9133(2) 0.3102(2) 0.0204(5) Uani 1 1 d . . . H10 H 0.8511 0.8987 0.3833 0.024 Uiso 1 1 calc R . . C11 C 0.4603(3) 0.6440(2) 0.1972(2) 0.0147(5) Uani 1 1 d . . . C12 C 0.3140(3) 0.6614(2) 0.1833(2) 0.0170(5) Uani 1 1 d . . . H12 H 0.2694 0.6996 0.1073 0.020 Uiso 1 1 calc R . . C13 C 0.2343(3) 0.6235(3) 0.2794(3) 0.0202(5) Uani 1 1 d . . . H13 H 0.1357 0.6359 0.2685 0.024 Uiso 1 1 calc R . . C14 C 0.2967(3) 0.5679(3) 0.3910(2) 0.0210(5) Uani 1 1 d . . . H14 H 0.2415 0.5435 0.4569 0.025 Uiso 1 1 calc R . . C15 C 0.4398(3) 0.5480(2) 0.4061(2) 0.0183(5) Uani 1 1 d . . . H15 H 0.4822 0.5084 0.4822 0.022 Uiso 1 1 calc R . . C16 C 0.5230(2) 0.5854(2) 0.3112(2) 0.0159(5) Uani 1 1 d . . . C17 C 0.7946(2) 0.5767(3) 0.4900(2) 0.0169(5) Uani 1 1 d . . . C18 C 0.7351(3) 0.6894(3) 0.5595(2) 0.0197(5) Uani 1 1 d . . . H18A H 0.7794 0.6928 0.6485 0.030 Uiso 1 1 calc R . . H18B H 0.6336 0.6788 0.5595 0.030 Uiso 1 1 calc R . . H18C H 0.7542 0.7684 0.5152 0.030 Uiso 1 1 calc R . . C19 C 0.9503(3) 0.6033(3) 0.4806(3) 0.0206(5) Uani 1 1 d . . . H19A H 0.9992 0.6140 0.5673 0.031 Uiso 1 1 calc R . . H19B H 0.9598 0.6810 0.4307 0.031 Uiso 1 1 calc R . . H19C H 0.9915 0.5318 0.4379 0.031 Uiso 1 1 calc R . . C20 C 0.7844(3) 0.4587(3) 0.5762(2) 0.0216(5) Uani 1 1 d . . . H20A H 0.6858 0.4420 0.5867 0.032 Uiso 1 1 calc R . . H20B H 0.8365 0.4742 0.6606 0.032 Uiso 1 1 calc R . . H20C H 0.8243 0.3850 0.5360 0.032 Uiso 1 1 calc R . . C21 C 0.7237(3) 0.3932(2) 0.2613(2) 0.0181(5) Uani 1 1 d . . . C22 C 0.8770(3) 0.3486(3) 0.2737(3) 0.0240(6) Uani 1 1 d . . . H22A H 0.9341 0.4112 0.2337 0.036 Uiso 1 1 calc R . . H22B H 0.8829 0.2665 0.2305 0.036 Uiso 1 1 calc R . . H22C H 0.9118 0.3396 0.3649 0.036 Uiso 1 1 calc R . . C23 C 0.6664(3) 0.3884(3) 0.1179(3) 0.0220(6) Uani 1 1 d . . . H23A H 0.5786 0.4365 0.1044 0.033 Uiso 1 1 calc R . . H23B H 0.6489 0.2998 0.0919 0.033 Uiso 1 1 calc R . . H23C H 0.7351 0.4257 0.0661 0.033 Uiso 1 1 calc R . . C24 C 0.6348(3) 0.3004(3) 0.3308(2) 0.0229(6) Uani 1 1 d . . . H24A H 0.6439 0.2148 0.2960 0.034 Uiso 1 1 calc R . . H24B H 0.5364 0.3268 0.3180 0.034 Uiso 1 1 calc R . . H24C H 0.6673 0.3004 0.4230 0.034 Uiso 1 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 0.0100(2) 0.0144(2) 0.0130(2) -0.00082(16) 0.00230(15) -0.00032(16) P1 0.0087(3) 0.0159(3) 0.0133(3) 0.0000(2) 0.0018(2) 0.0002(2) O1 0.0120(8) 0.0208(8) 0.0130(7) 0.0001(7) 0.0028(6) -0.0017(7) C1 0.0187(13) 0.0220(13) 0.0248(12) -0.0012(11) 0.0122(10) 0.0060(10) C2 0.0106(11) 0.0301(13) 0.0259(12) 0.0013(12) 0.0073(9) -0.0001(11) C3 0.0195(13) 0.0249(13) 0.0227(12) 0.0056(11) 0.0127(10) -0.0016(11) C4 0.0163(11) 0.0343(14) 0.0115(10) 0.0015(11) 0.0045(9) 0.0024(12) C5 0.0221(13) 0.0285(14) 0.0149(11) -0.0069(10) 0.0084(10) -0.0018(11) C6 0.0275(14) 0.0135(12) 0.0279(13) -0.0045(10) 0.0002(11) -0.0058(11) C7 0.0311(15) 0.0139(12) 0.0228(12) 0.0015(10) 0.0008(11) 0.0039(11) C8 0.0215(13) 0.0156(11) 0.0210(12) -0.0021(9) 0.0026(10) 0.0064(10) C9 0.0216(13) 0.0174(12) 0.0164(11) -0.0054(9) 0.0030(9) 0.0063(10) C10 0.0254(14) 0.0160(12) 0.0187(12) -0.0071(10) -0.0027(10) 0.0012(10) C11 0.0134(12) 0.0157(11) 0.0156(11) -0.0021(9) 0.0040(9) -0.0022(9) C12 0.0114(11) 0.0229(13) 0.0163(11) 0.0020(9) 0.0006(9) 0.0020(10) C13 0.0097(11) 0.0284(13) 0.0229(12) 0.0010(11) 0.0033(9) 0.0009(10) C14 0.0136(12) 0.0286(14) 0.0218(11) 0.0052(12) 0.0067(9) -0.0024(11) C15 0.0135(12) 0.0231(13) 0.0184(11) 0.0035(10) 0.0022(9) 0.0009(10) C16 0.0135(11) 0.0171(12) 0.0170(11) -0.0007(9) 0.0015(9) 0.0008(9) C17 0.0128(11) 0.0215(12) 0.0160(11) 0.0022(10) 0.0002(9) 0.0020(10) C18 0.0179(12) 0.0252(13) 0.0160(10) -0.0038(10) 0.0016(9) 0.0038(10) C19 0.0143(12) 0.0262(14) 0.0206(12) -0.0005(10) -0.0016(10) 0.0021(10) C20 0.0188(13) 0.0259(14) 0.0198(12) 0.0054(11) -0.0002(10) 0.0001(11) C21 0.0195(13) 0.0149(11) 0.0199(12) -0.0018(9) 0.0025(9) -0.0013(10) C22 0.0236(14) 0.0205(13) 0.0286(13) -0.0020(11) 0.0062(11) 0.0055(11) C23 0.0266(15) 0.0192(13) 0.0203(12) -0.0024(10) 0.0034(10) -0.0037(11) C24 0.0246(13) 0.0219(14) 0.0222(12) 0.0015(10) 0.0021(10) -0.0018(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 O1 2.0256(17) . ? Ti1 C10 2.365(2) . ? Ti1 C9 2.373(2) . ? Ti1 C4 2.376(2) . ? Ti1 C3 2.398(2) . ? Ti1 C6 2.398(3) . ? Ti1 C2 2.399(2) . ? Ti1 C5 2.400(2) . ? Ti1 C1 2.412(2) . ? Ti1 C8 2.414(3) . ? Ti1 C7 2.416(3) . ? Ti1 P1 2.9067(8) . ? P1 C16 1.820(2) . ? P1 C17 1.912(2) . ? P1 C21 1.914(3) . ? O1 C11 1.322(3) . ? C1 C2 1.413(4) . ? C1 C5 1.414(4) . ? C2 C3 1.411(4) . ? C3 C4 1.403(4) . ? C4 C5 1.421(4) . ? C6 C10 1.397(4) . ? C6 C7 1.416(4) . ? C7 C8 1.394(4) . ? C8 C9 1.401(4) . ? C9 C10 1.423(4) . ? C11 C12 1.408(4) . ? C11 C16 1.416(3) . ? C12 C13 1.386(4) . ? C13 C14 1.382(4) . ? C14 C15 1.381(4) . ? C15 C16 1.397(4) . ? C17 C18 1.534(4) . ? C17 C19 1.534(3) . ? C17 C20 1.544(4) . ? C21 C24 1.532(4) . ? C21 C22 1.536(4) . ? C21 C23 1.541(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 O1 Ti1 C10 123.25(9) . . ? O1 Ti1 C9 88.67(8) . . ? C10 Ti1 C9 34.95(10) . . ? O1 Ti1 C4 92.08(8) . . ? C10 Ti1 C4 135.07(10) . . ? C9 Ti1 C4 145.20(10) . . ? O1 Ti1 C3 126.19(8) . . ? C10 Ti1 C3 104.43(10) . . ? C9 Ti1 C3 130.95(10) . . ? C4 Ti1 C3 34.18(9) . . ? O1 Ti1 C6 135.69(9) . . ? C10 Ti1 C6 34.09(10) . . ? C9 Ti1 C6 56.93(9) . . ? C4 Ti1 C6 101.49(10) . . ? C3 Ti1 C6 74.69(10) . . ? O1 Ti1 C2 136.34(8) . . ? C10 Ti1 C2 99.66(10) . . ? C9 Ti1 C2 134.60(9) . . ? C4 Ti1 C2 57.18(8) . . ? C3 Ti1 C2 34.20(9) . . ? C6 Ti1 C2 84.37(10) . . ? O1 Ti1 C5 80.02(8) . . ? C10 Ti1 C5 156.55(9) . . ? C9 Ti1 C5 168.48(9) . . ? C4 Ti1 C5 34.62(10) . . ? C3 Ti1 C5 56.77(9) . . ? C6 Ti1 C5 131.44(10) . . ? C2 Ti1 C5 56.90(9) . . ? O1 Ti1 C1 104.57(8) . . ? C10 Ti1 C1 125.62(10) . . ? C9 Ti1 C1 154.75(9) . . ? C4 Ti1 C1 57.18(9) . . ? C3 Ti1 C1 56.64(9) . . ? C6 Ti1 C1 118.31(10) . . ? C2 Ti1 C1 34.15(10) . . ? C5 Ti1 C1 34.17(9) . . ? O1 Ti1 C8 79.61(8) . . ? C10 Ti1 C8 56.91(9) . . ? C9 Ti1 C8 34.01(9) . . ? C4 Ti1 C8 112.20(9) . . ? C3 Ti1 C8 111.96(9) . . ? C6 Ti1 C8 56.16(9) . . ? C2 Ti1 C8 137.72(10) . . ? C5 Ti1 C8 139.48(9) . . ? C1 Ti1 C8 168.27(9) . . ? O1 Ti1 C7 105.22(9) . . ? C10 Ti1 C7 57.03(10) . . ? C9 Ti1 C7 56.71(9) . . ? C4 Ti1 C7 89.75(10) . . ? C3 Ti1 C7 79.35(10) . . ? C6 Ti1 C7 34.21(10) . . ? C2 Ti1 C7 104.79(10) . . ? C5 Ti1 C7 124.18(10) . . ? C1 Ti1 C7 135.74(10) . . ? C8 Ti1 C7 33.55(10) . . ? O1 Ti1 P1 69.51(5) . . ? C10 Ti1 P1 88.80(7) . . ? C9 Ti1 P1 79.81(7) . . ? C4 Ti1 P1 132.60(8) . . ? C3 Ti1 P1 139.98(7) . . ? C6 Ti1 P1 122.49(7) . . ? C2 Ti1 P1 107.06(7) . . ? C5 Ti1 P1 98.08(7) . . ? C1 Ti1 P1 84.78(7) . . ? C8 Ti1 P1 106.93(7) . . ? C7 Ti1 P1 136.50(7) . . ? C16 P1 C17 109.04(10) . . ? C16 P1 C21 100.93(11) . . ? C17 P1 C21 107.83(11) . . ? C16 P1 Ti1 89.63(8) . . ? C17 P1 Ti1 122.78(9) . . ? C21 P1 Ti1 121.30(8) . . ? C11 O1 Ti1 124.06(15) . . ? C2 C1 C5 107.9(2) . . ? C2 C1 Ti1 72.41(14) . . ? C5 C1 Ti1 72.43(14) . . ? C3 C2 C1 107.8(2) . . ? C3 C2 Ti1 72.85(14) . . ? C1 C2 Ti1 73.43(13) . . ? C4 C3 C2 108.6(2) . . ? C4 C3 Ti1 72.06(14) . . ? C2 C3 Ti1 72.95(14) . . ? C3 C4 C5 107.7(2) . . ? C3 C4 Ti1 73.76(13) . . ? C5 C4 Ti1 73.60(13) . . ? C1 C5 C4 107.9(2) . . ? C1 C5 Ti1 73.40(14) . . ? C4 C5 Ti1 71.78(13) . . ? C10 C6 C7 108.5(2) . . ? C10 C6 Ti1 71.65(14) . . ? C7 C6 Ti1 73.56(14) . . ? C8 C7 C6 107.5(2) . . ? C8 C7 Ti1 73.17(14) . . ? C6 C7 Ti1 72.23(15) . . ? C7 C8 C9 108.9(2) . . ? C7 C8 Ti1 73.28(15) . . ? C9 C8 Ti1 71.36(14) . . ? C8 C9 C10 107.6(2) . . ? C8 C9 Ti1 74.62(14) . . ? C10 C9 Ti1 72.23(14) . . ? C6 C10 C9 107.5(2) . . ? C6 C10 Ti1 74.26(15) . . ? C9 C10 Ti1 72.82(14) . . ? O1 C11 C12 119.6(2) . . ? O1 C11 C16 122.3(2) . . ? C12 C11 C16 118.1(2) . . ? C13 C12 C11 120.7(2) . . ? C14 C13 C12 120.7(2) . . ? C15 C14 C13 119.7(2) . . ? C14 C15 C16 121.0(2) . . ? C15 C16 C11 119.8(2) . . ? C15 C16 P1 126.60(19) . . ? C11 C16 P1 113.61(17) . . ? C18 C17 C19 107.8(2) . . ? C18 C17 C20 107.1(2) . . ? C19 C17 C20 108.0(2) . . ? C18 C17 P1 111.11(17) . . ? C19 C17 P1 104.83(16) . . ? C20 C17 P1 117.67(19) . . ? C24 C21 C22 110.0(2) . . ? C24 C21 C23 106.4(2) . . ? C22 C21 C23 108.0(2) . . ? C24 C21 P1 114.32(17) . . ? C22 C21 P1 110.66(18) . . ? C23 C21 P1 107.08(17) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 66.36 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.440 _refine_diff_density_min -0.307 _refine_diff_density_rms 0.061