# 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 dstephan@chem.utoronto.ca _publ_contact_author_name 'Douglas W. Stephan' loop_ _publ_author_name 'Rebecca C. Neu' 'Gabriel Menard' 'Douglas W. Stephan' data_compound2_C26H27BF13O5PS _database_code_depnum_ccdc_archive 'CCDC 864916' #TrackingRef 'combined-cifs-revised.txt' _audit_creation_method shelxl-97 _chemical_formula_sum 'C26 H27 B F13 O5 P S' _chemical_formula_weight 740.32 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' s s 0.1246 0.1234 'international tables vol c tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_h-m P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7343(4) _cell_length_b 10.7665(4) _cell_length_c 14.9487(6) _cell_angle_alpha 98.1230(10) _cell_angle_beta 97.127(2) _cell_angle_gamma 106.6580(10) _cell_volume 1463.34(10) _cell_formula_units_z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9907 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_method 'not measured' _exptl_crystal_f_000 752 _exptl_absorpt_coefficient_mu 0.287 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_t_min 0.6979 _exptl_absorpt_correction_t_max 0.7456 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type mok\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24536 _diffrn_reflns_av_r_equivalents 0.0226 _diffrn_reflns_av_sigmai/neti 0.0203 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.51 _reflns_number_total 6690 _reflns_number_gt 5865 _reflns_threshold_expression >2sigma(i) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0427P)^2^+0.6114P] 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 6690 _refine_ls_number_parameters 444 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0835 _refine_ls_wR_factor_gt 0.0803 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.000 _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 S1 S 0.19149(4) 0.65154(3) 0.13474(2) 0.02047(8) Uani 1 1 d . . . P1 P 0.37198(3) 0.27250(3) 0.16440(2) 0.01431(8) Uani 1 1 d . . . F1 F 0.23039(10) 0.47379(8) 0.41267(6) 0.0289(2) Uani 1 1 d . . . F2 F 0.12951(10) 0.56128(10) 0.55775(6) 0.0345(2) Uani 1 1 d . . . F3 F 0.16566(11) 0.82339(11) 0.60849(6) 0.0393(2) Uani 1 1 d . . . F4 F 0.30698(11) 0.99732(9) 0.50846(7) 0.0357(2) Uani 1 1 d . . . F5 F 0.40904(9) 0.91200(8) 0.36277(6) 0.02623(19) Uani 1 1 d . . . F6 F 0.58513(9) 0.60589(9) 0.42928(6) 0.02593(19) Uani 1 1 d . . . F7 F 0.87068(9) 0.73687(10) 0.48349(6) 0.0327(2) Uani 1 1 d . . . F8 F 1.00734(9) 0.92478(9) 0.39287(6) 0.0322(2) Uani 1 1 d . . . F9 F 0.85676(9) 0.97331(9) 0.24268(6) 0.0295(2) Uani 1 1 d . . . F10 F 0.57456(9) 0.84981(8) 0.18986(6) 0.02383(18) Uani 1 1 d . . . F11 F 0.03066(10) 0.53665(11) 0.24544(7) 0.0405(2) Uani 1 1 d . . . F12 F 0.04376(12) 0.73976(11) 0.24889(9) 0.0483(3) Uani 1 1 d . . . F13 F -0.08621(10) 0.59153(12) 0.13393(8) 0.0480(3) Uani 1 1 d . . . O1 O 0.35462(10) 0.50266(9) 0.25933(6) 0.01584(18) Uani 1 1 d . . . O2 O 0.48186(11) 0.52050(9) 0.14302(7) 0.0217(2) Uani 1 1 d . . . O3 O 0.31887(10) 0.70533(9) 0.21213(6) 0.01856(19) Uani 1 1 d . . . O4 O 0.18567(12) 0.75270(11) 0.08417(8) 0.0315(3) Uani 1 1 d . . . O5 O 0.17712(13) 0.52291(11) 0.08778(8) 0.0349(3) Uani 1 1 d . . . C1 C 0.32384(14) 0.68771(13) 0.37926(9) 0.0175(3) Uani 1 1 d . . . C2 C 0.25200(14) 0.60422(14) 0.43302(9) 0.0204(3) Uani 1 1 d . . . C3 C 0.19844(15) 0.64739(16) 0.50899(10) 0.0247(3) Uani 1 1 d . . . C4 C 0.21696(16) 0.78023(17) 0.53476(10) 0.0272(3) Uani 1 1 d . . . C5 C 0.28858(16) 0.86757(15) 0.48467(10) 0.0253(3) Uani 1 1 d . . . C6 C 0.34003(15) 0.82069(14) 0.40925(9) 0.0204(3) Uani 1 1 d . . . C7 C 0.56516(14) 0.72265(12) 0.30807(9) 0.0162(2) Uani 1 1 d . . . C8 C 0.64901(15) 0.69777(13) 0.38158(9) 0.0186(3) Uani 1 1 d . . . C9 C 0.79600(15) 0.76269(14) 0.41066(9) 0.0216(3) Uani 1 1 d . . . C10 C 0.86559(14) 0.85762(14) 0.36463(10) 0.0220(3) Uani 1 1 d . . . C11 C 0.78859(15) 0.88379(13) 0.28942(10) 0.0198(3) Uani 1 1 d . . . C12 C 0.64159(14) 0.81695(13) 0.26298(9) 0.0175(3) Uani 1 1 d . . . C13 C 0.40762(14) 0.45724(12) 0.18924(9) 0.0156(2) Uani 1 1 d . . . C14 C 0.56552(15) 0.26674(14) 0.17822(10) 0.0212(3) Uani 1 1 d . . . C15 C 0.65784(16) 0.37085(15) 0.26184(11) 0.0276(3) Uani 1 1 d . . . H15A H 0.7549 0.3607 0.2741 0.041 Uiso 1 1 calc R . . H15B H 0.6106 0.3587 0.3156 0.041 Uiso 1 1 calc R . . H15C H 0.6667 0.4594 0.2491 0.041 Uiso 1 1 calc R . . C16 C 0.63725(17) 0.30054(16) 0.09482(11) 0.0286(3) Uani 1 1 d . . . H16A H 0.6290 0.3854 0.0826 0.043 Uiso 1 1 calc R . . H16B H 0.5881 0.2315 0.0410 0.043 Uiso 1 1 calc R . . H16C H 0.7403 0.3062 0.1078 0.043 Uiso 1 1 calc R . . C17 C 0.57188(17) 0.12924(15) 0.19205(11) 0.0276(3) Uani 1 1 d . . . H17A H 0.5084 0.0623 0.1407 0.041 Uiso 1 1 calc R . . H17B H 0.5391 0.1111 0.2496 0.041 Uiso 1 1 calc R . . H17C H 0.6722 0.1269 0.1946 0.041 Uiso 1 1 calc R . . C18 C 0.27267(15) 0.20973(13) 0.04243(9) 0.0203(3) Uani 1 1 d . . . C19 C 0.32969(18) 0.30913(15) -0.01973(10) 0.0258(3) Uani 1 1 d . . . H19A H 0.2810 0.2721 -0.0833 0.039 Uiso 1 1 calc R . . H19B H 0.4350 0.3268 -0.0159 0.039 Uiso 1 1 calc R . . H19C H 0.3093 0.3916 0.0006 0.039 Uiso 1 1 calc R . . C20 C 0.29179(18) 0.07577(14) 0.00509(10) 0.0265(3) Uani 1 1 d . . . H20A H 0.2588 0.0136 0.0457 0.040 Uiso 1 1 calc R . . H20B H 0.3948 0.0877 0.0024 0.040 Uiso 1 1 calc R . . H20C H 0.2340 0.0409 -0.0566 0.040 Uiso 1 1 calc R . . C21 C 0.10947(16) 0.19190(15) 0.03703(11) 0.0282(3) Uani 1 1 d . . . H21A H 0.0617 0.1687 -0.0274 0.042 Uiso 1 1 calc R . . H21B H 0.0963 0.2744 0.0657 0.042 Uiso 1 1 calc R . . H21C H 0.0662 0.1212 0.0693 0.042 Uiso 1 1 calc R . . C22 C 0.26641(15) 0.19308(13) 0.24956(9) 0.0196(3) Uani 1 1 d . . . C23 C 0.21903(17) 0.04157(14) 0.22348(11) 0.0264(3) Uani 1 1 d . . . H23A H 0.1700 0.0029 0.2710 0.040 Uiso 1 1 calc R . . H23B H 0.3049 0.0127 0.2182 0.040 Uiso 1 1 calc R . . H23C H 0.1520 0.0127 0.1646 0.040 Uiso 1 1 calc R . . C25 C 0.36064(17) 0.23635(15) 0.34616(10) 0.0259(3) Uani 1 1 d . . . H25A H 0.3946 0.3329 0.3623 0.039 Uiso 1 1 calc R . . H25B H 0.4447 0.2034 0.3466 0.039 Uiso 1 1 calc R . . H25C H 0.3025 0.2002 0.3909 0.039 Uiso 1 1 calc R . . C26 C 0.03578(16) 0.62854(15) 0.19420(11) 0.0283(3) Uani 1 1 d . . . B1 B 0.39022(15) 0.64889(14) 0.28825(10) 0.0155(3) Uani 1 1 d . . . C24 C 0.12816(16) 0.23567(15) 0.25405(11) 0.0254(3) Uani 1 1 d . . . H24C H 0.148(2) 0.3284(19) 0.2598(12) 0.030(5) Uiso 1 1 d . . . H24A H 0.051(2) 0.1897(18) 0.2023(13) 0.032(5) Uiso 1 1 d . . . H24B H 0.091(2) 0.213(2) 0.3095(15) 0.043(5) Uiso 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 S1 0.02328(17) 0.01902(17) 0.01925(17) 0.00077(13) -0.00060(12) 0.00990(13) P1 0.01789(16) 0.00996(15) 0.01519(16) 0.00211(12) 0.00346(12) 0.00435(12) F1 0.0413(5) 0.0179(4) 0.0260(4) 0.0039(3) 0.0134(4) 0.0039(4) F2 0.0317(5) 0.0442(6) 0.0214(4) 0.0043(4) 0.0098(4) 0.0008(4) F3 0.0396(5) 0.0537(6) 0.0250(5) -0.0084(4) 0.0109(4) 0.0205(5) F4 0.0459(6) 0.0274(5) 0.0343(5) -0.0091(4) 0.0034(4) 0.0206(4) F5 0.0340(5) 0.0156(4) 0.0292(5) 0.0024(3) 0.0054(4) 0.0087(3) F6 0.0251(4) 0.0271(5) 0.0261(4) 0.0135(4) 0.0037(3) 0.0051(3) F7 0.0240(4) 0.0441(6) 0.0286(5) 0.0116(4) -0.0031(4) 0.0088(4) F8 0.0166(4) 0.0367(5) 0.0354(5) 0.0014(4) 0.0022(3) -0.0007(4) F9 0.0259(4) 0.0249(5) 0.0357(5) 0.0107(4) 0.0109(4) -0.0003(3) F10 0.0260(4) 0.0216(4) 0.0258(4) 0.0115(3) 0.0047(3) 0.0071(3) F11 0.0290(5) 0.0440(6) 0.0475(6) 0.0221(5) 0.0050(4) 0.0040(4) F12 0.0404(6) 0.0394(6) 0.0679(8) -0.0038(5) 0.0264(5) 0.0160(5) F13 0.0212(5) 0.0569(7) 0.0604(7) 0.0196(6) -0.0082(4) 0.0057(4) O1 0.0186(4) 0.0118(4) 0.0167(4) 0.0011(3) 0.0045(3) 0.0042(3) O2 0.0291(5) 0.0143(5) 0.0226(5) 0.0043(4) 0.0108(4) 0.0053(4) O3 0.0194(4) 0.0144(4) 0.0213(5) 0.0029(4) 0.0012(4) 0.0054(4) O4 0.0371(6) 0.0346(6) 0.0268(6) 0.0118(5) 0.0011(5) 0.0164(5) O5 0.0410(6) 0.0282(6) 0.0315(6) -0.0103(5) -0.0098(5) 0.0187(5) C1 0.0162(6) 0.0173(6) 0.0177(6) -0.0003(5) 0.0005(5) 0.0060(5) C2 0.0206(6) 0.0184(7) 0.0196(7) -0.0010(5) 0.0019(5) 0.0049(5) C3 0.0196(6) 0.0332(8) 0.0184(7) 0.0028(6) 0.0031(5) 0.0048(6) C4 0.0235(7) 0.0408(9) 0.0171(7) -0.0058(6) 0.0021(5) 0.0158(6) C5 0.0255(7) 0.0235(7) 0.0256(7) -0.0064(6) -0.0016(6) 0.0134(6) C6 0.0200(6) 0.0196(7) 0.0207(7) 0.0005(5) 0.0009(5) 0.0074(5) C7 0.0182(6) 0.0117(6) 0.0182(6) -0.0005(5) 0.0038(5) 0.0052(5) C8 0.0217(6) 0.0148(6) 0.0198(6) 0.0033(5) 0.0059(5) 0.0055(5) C9 0.0211(6) 0.0255(7) 0.0190(6) 0.0020(5) 0.0013(5) 0.0105(5) C10 0.0158(6) 0.0210(7) 0.0254(7) -0.0029(5) 0.0046(5) 0.0030(5) C11 0.0224(6) 0.0138(6) 0.0235(7) 0.0023(5) 0.0096(5) 0.0045(5) C12 0.0212(6) 0.0141(6) 0.0189(6) 0.0018(5) 0.0047(5) 0.0080(5) C13 0.0176(6) 0.0126(6) 0.0164(6) 0.0017(5) 0.0020(5) 0.0052(5) C14 0.0207(6) 0.0190(7) 0.0258(7) 0.0032(5) 0.0053(5) 0.0091(5) C15 0.0207(7) 0.0279(8) 0.0315(8) 0.0011(6) -0.0008(6) 0.0074(6) C16 0.0268(7) 0.0266(8) 0.0362(8) 0.0063(6) 0.0144(6) 0.0101(6) C17 0.0326(8) 0.0237(8) 0.0324(8) 0.0063(6) 0.0062(6) 0.0172(6) C18 0.0283(7) 0.0152(6) 0.0157(6) 0.0006(5) 0.0005(5) 0.0068(5) C19 0.0412(8) 0.0208(7) 0.0172(7) 0.0047(5) 0.0042(6) 0.0122(6) C20 0.0400(8) 0.0167(7) 0.0205(7) -0.0013(5) 0.0021(6) 0.0087(6) C21 0.0272(7) 0.0233(7) 0.0293(8) 0.0013(6) -0.0048(6) 0.0059(6) C22 0.0258(7) 0.0130(6) 0.0205(7) 0.0048(5) 0.0088(5) 0.0039(5) C23 0.0351(8) 0.0137(7) 0.0307(8) 0.0077(6) 0.0114(6) 0.0037(6) C25 0.0373(8) 0.0236(7) 0.0191(7) 0.0071(6) 0.0081(6) 0.0099(6) C26 0.0199(7) 0.0255(8) 0.0382(9) 0.0066(6) 0.0014(6) 0.0060(6) B1 0.0176(6) 0.0115(6) 0.0172(7) 0.0025(5) 0.0025(5) 0.0048(5) C24 0.0236(7) 0.0183(7) 0.0326(8) 0.0023(6) 0.0115(6) 0.0023(6) _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 S1 O4 1.4206(11) . ? S1 O5 1.4214(11) . ? S1 O3 1.5014(10) . ? S1 C26 1.8248(16) . ? P1 C22 1.8804(13) . ? P1 C18 1.8857(14) . ? P1 C14 1.8894(14) . ? P1 C13 1.8916(13) . ? F1 C2 1.3427(16) . ? F2 C3 1.3404(17) . ? F3 C4 1.3434(16) . ? F4 C5 1.3455(17) . ? F5 C6 1.3530(16) . ? F6 C8 1.3529(15) . ? F7 C9 1.3401(16) . ? F8 C10 1.3424(16) . ? F9 C11 1.3403(16) . ? F10 C12 1.3455(15) . ? F11 C26 1.3279(19) . ? F12 C26 1.3276(19) . ? F13 C26 1.3200(17) . ? O1 C13 1.3180(15) . ? O1 B1 1.4978(16) . ? O2 C13 1.1993(16) . ? O3 B1 1.5453(17) . ? C1 C2 1.3879(19) . ? C1 C6 1.3955(19) . ? C1 B1 1.629(2) . ? C2 C3 1.383(2) . ? C3 C4 1.381(2) . ? C4 C5 1.373(2) . ? C5 C6 1.379(2) . ? C7 C12 1.3869(18) . ? C7 C8 1.3898(19) . ? C7 B1 1.6283(19) . ? C8 C9 1.3825(19) . ? C9 C10 1.376(2) . ? C10 C11 1.381(2) . ? C11 C12 1.3822(19) . ? C14 C16 1.540(2) . ? C14 C17 1.541(2) . ? C14 C15 1.541(2) . ? C18 C21 1.535(2) . ? C18 C20 1.5422(19) . ? C18 C19 1.5444(19) . ? C22 C23 1.5395(19) . ? C22 C25 1.543(2) . ? C22 C24 1.547(2) . ? 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 O4 S1 O5 119.90(7) . . ? O4 S1 O3 108.69(6) . . ? O5 S1 O3 113.77(6) . . ? O4 S1 C26 105.34(7) . . ? O5 S1 C26 104.46(8) . . ? O3 S1 C26 102.79(6) . . ? C22 P1 C18 112.63(6) . . ? C22 P1 C14 113.41(6) . . ? C18 P1 C14 112.33(6) . . ? C22 P1 C13 110.30(6) . . ? C18 P1 C13 107.41(6) . . ? C14 P1 C13 99.85(6) . . ? C13 O1 B1 118.70(10) . . ? S1 O3 B1 135.61(8) . . ? C2 C1 C6 114.12(12) . . ? C2 C1 B1 128.07(12) . . ? C6 C1 B1 117.80(12) . . ? F1 C2 C3 116.03(13) . . ? F1 C2 C1 120.46(12) . . ? C3 C2 C1 123.52(13) . . ? F2 C3 C4 119.96(13) . . ? F2 C3 C2 120.46(14) . . ? C4 C3 C2 119.58(14) . . ? F3 C4 C5 120.43(14) . . ? F3 C4 C3 120.13(15) . . ? C5 C4 C3 119.43(13) . . ? F4 C5 C4 120.27(13) . . ? F4 C5 C6 120.45(14) . . ? C4 C5 C6 119.27(13) . . ? F5 C6 C5 116.21(12) . . ? F5 C6 C1 119.72(12) . . ? C5 C6 C1 124.07(14) . . ? C12 C7 C8 114.59(12) . . ? C12 C7 B1 126.93(12) . . ? C8 C7 B1 118.32(11) . . ? F6 C8 C9 116.81(12) . . ? F6 C8 C7 119.22(12) . . ? C9 C8 C7 123.97(13) . . ? F7 C9 C10 119.68(12) . . ? F7 C9 C8 121.38(13) . . ? C10 C9 C8 118.93(13) . . ? F8 C10 C9 120.23(13) . . ? F8 C10 C11 120.16(13) . . ? C9 C10 C11 119.61(12) . . ? F9 C11 C10 119.87(12) . . ? F9 C11 C12 120.61(12) . . ? C10 C11 C12 119.51(12) . . ? F10 C12 C11 115.62(12) . . ? F10 C12 C7 121.02(12) . . ? C11 C12 C7 123.35(12) . . ? O2 C13 O1 127.19(12) . . ? O2 C13 P1 116.84(10) . . ? O1 C13 P1 115.84(9) . . ? C16 C14 C17 108.24(12) . . ? C16 C14 C15 106.58(12) . . ? C17 C14 C15 109.38(12) . . ? C16 C14 P1 112.28(10) . . ? C17 C14 P1 111.07(10) . . ? C15 C14 P1 109.16(9) . . ? C21 C18 C20 108.73(12) . . ? C21 C18 C19 106.79(12) . . ? C20 C18 C19 109.48(12) . . ? C21 C18 P1 110.75(10) . . ? C20 C18 P1 110.09(9) . . ? C19 C18 P1 110.91(9) . . ? C23 C22 C25 108.92(11) . . ? C23 C22 C24 108.17(12) . . ? C25 C22 C24 107.79(12) . . ? C23 C22 P1 111.23(9) . . ? C25 C22 P1 109.94(9) . . ? C24 C22 P1 110.70(10) . . ? F13 C26 F12 108.70(13) . . ? F13 C26 F11 108.45(12) . . ? F12 C26 F11 107.86(14) . . ? F13 C26 S1 109.91(12) . . ? F12 C26 S1 110.84(10) . . ? F11 C26 S1 111.01(10) . . ? O1 B1 O3 109.68(10) . . ? O1 B1 C7 111.72(10) . . ? O3 B1 C7 108.72(10) . . ? O1 B1 C1 112.15(10) . . ? O3 B1 C1 105.51(10) . . ? C7 B1 C1 108.82(10) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.550 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.048 #===end data_compound3_C31H27AlF15O2P _database_code_depnum_ccdc_archive 'CCDC 864917' #TrackingRef 'combined-cifs-revised.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H27 Al F15 O2 P' _chemical_formula_weight 774.48 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 18.2162(8) _cell_length_b 15.2634(7) _cell_length_c 24.7764(11) _cell_angle_alpha 90.00 _cell_angle_beta 108.346(2) _cell_angle_gamma 90.00 _cell_volume 6538.7(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16087 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 27.59 _exptl_crystal_description blocks _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3136 _exptl_absorpt_coefficient_mu 0.226 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9331 _exptl_absorpt_correction_T_max 0.9604 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59519 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0537 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 27.85 _reflns_number_total 15499 _reflns_number_gt 10350 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0549P)^2^+2.1180P] 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_number_reflns 15499 _refine_ls_number_parameters 919 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0843 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1219 _refine_ls_wR_factor_gt 0.1059 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 Al3 Al 0.95871(4) 0.72839(4) 0.61765(3) 0.02012(14) Uani 1 1 d . . . Al4 Al 0.54877(4) 0.25295(4) 0.38952(3) 0.02066(14) Uani 1 1 d . . . O1 O 0.95342(8) 0.72162(9) 0.54273(6) 0.0236(3) Uani 1 1 d . . . O2 O 1.00938(10) 0.85174(10) 0.54562(7) 0.0349(4) Uani 1 1 d . . . O3 O 0.51636(9) 0.12363(9) 0.46847(6) 0.0278(4) Uani 1 1 d . . . O4 O 0.55127(9) 0.26263(9) 0.46355(6) 0.0237(3) Uani 1 1 d . . . P1 P 0.50714(3) 0.22124(3) 0.55539(2) 0.01749(12) Uani 1 1 d . . . P2 P 0.99729(3) 0.75971(3) 0.45091(2) 0.02038(12) Uani 1 1 d . . . F1 F 1.06837(8) 0.56798(8) 0.63274(6) 0.0374(3) Uani 1 1 d . . . F2 F 1.21954(9) 0.54500(11) 0.68569(7) 0.0571(5) Uani 1 1 d . . . F3 F 1.30879(9) 0.68354(14) 0.73770(7) 0.0688(6) Uani 1 1 d . . . F4 F 1.24368(9) 0.84443(12) 0.73563(7) 0.0603(5) Uani 1 1 d . . . F5 F 1.09168(8) 0.86750(9) 0.68194(6) 0.0411(4) Uani 1 1 d . . . F6 F 0.79570(8) 0.66035(9) 0.54591(6) 0.0399(4) Uani 1 1 d . . . F7 F 0.71044(8) 0.52241(11) 0.55816(6) 0.0514(4) Uani 1 1 d . . . F8 F 0.76712(9) 0.40889(9) 0.64600(7) 0.0481(4) Uani 1 1 d . . . F9 F 0.90791(9) 0.43726(12) 0.72262(7) 0.0661(6) Uani 1 1 d . . . F10 F 0.99015(8) 0.58012(11) 0.71516(6) 0.0507(4) Uani 1 1 d . . . F11 F 0.97107(8) 0.81674(9) 0.73328(5) 0.0329(3) Uani 1 1 d . . . F12 F 0.90680(9) 0.96293(9) 0.76026(5) 0.0402(4) Uani 1 1 d . . . F13 F 0.80614(8) 1.05895(9) 0.67746(6) 0.0403(4) Uani 1 1 d . . . F14 F 0.76751(8) 1.00653(9) 0.56719(6) 0.0378(3) Uani 1 1 d . . . F15 F 0.83458(7) 0.86441(9) 0.53911(5) 0.0318(3) Uani 1 1 d . . . F16 F 0.69110(7) 0.13935(9) 0.47184(5) 0.0325(3) Uani 1 1 d . . . F17 F 0.77259(8) 0.00705(10) 0.44715(6) 0.0420(4) Uani 1 1 d . . . F18 F 0.73859(9) -0.05149(10) 0.33849(6) 0.0451(4) Uani 1 1 d . . . F19 F 0.62598(9) 0.02707(9) 0.25395(5) 0.0404(4) Uani 1 1 d . . . F20 F 0.54685(8) 0.16362(9) 0.27742(5) 0.0348(3) Uani 1 1 d . . . F21 F 0.68124(8) 0.38033(9) 0.46566(6) 0.0380(3) Uani 1 1 d . . . F22 F 0.73403(9) 0.53479(10) 0.44129(7) 0.0497(4) Uani 1 1 d . . . F23 F 0.67719(9) 0.60367(9) 0.33500(7) 0.0487(4) Uani 1 1 d . . . F24 F 0.56736(9) 0.51538(10) 0.25309(6) 0.0480(4) Uani 1 1 d . . . F25 F 0.51150(9) 0.36365(9) 0.27734(5) 0.0398(4) Uani 1 1 d . . . F26 F 0.41418(9) 0.39226(9) 0.35573(6) 0.0460(4) Uani 1 1 d . . . F27 F 0.26223(10) 0.37786(12) 0.29745(7) 0.0619(5) Uani 1 1 d . . . F28 F 0.19955(8) 0.21851(13) 0.26177(7) 0.0609(5) Uani 1 1 d . . . F29 F 0.29039(9) 0.07308(11) 0.28317(7) 0.0539(4) Uani 1 1 d . . . F30 F 0.44251(8) 0.08687(8) 0.33860(6) 0.0361(3) Uani 1 1 d . . . C1 C 0.89818(12) 0.62445(14) 0.62868(9) 0.0228(5) Uani 1 1 d . . . C2 C 0.92235(13) 0.56659(16) 0.67374(9) 0.0296(5) Uani 1 1 d . . . C3 C 0.88036(14) 0.49372(17) 0.67959(11) 0.0361(6) Uani 1 1 d . . . C4 C 0.80914(14) 0.47868(15) 0.64040(10) 0.0318(5) Uani 1 1 d . . . C5 C 0.78099(13) 0.53558(15) 0.59559(10) 0.0307(5) Uani 1 1 d . . . C6 C 0.82604(13) 0.60595(14) 0.59103(9) 0.0246(5) Uani 1 1 d . . . C7 C 1.07232(12) 0.71819(14) 0.65749(9) 0.0228(5) Uani 1 1 d . . . C8 C 1.10986(13) 0.63838(15) 0.65951(9) 0.0271(5) Uani 1 1 d . . . C9 C 1.18758(14) 0.62451(17) 0.68554(10) 0.0363(6) Uani 1 1 d . . . C10 C 1.23240(14) 0.6942(2) 0.71164(10) 0.0422(7) Uani 1 1 d . . . C11 C 1.19931(14) 0.77573(19) 0.71057(10) 0.0394(6) Uani 1 1 d . . . C12 C 1.12102(13) 0.78586(15) 0.68339(9) 0.0283(5) Uani 1 1 d . . . C13 C 0.90717(12) 0.83531(14) 0.63523(9) 0.0212(4) Uani 1 1 d . . . C14 C 0.85422(12) 0.88548(14) 0.59518(9) 0.0230(5) Uani 1 1 d . . . C15 C 0.81861(12) 0.95888(15) 0.60815(9) 0.0262(5) Uani 1 1 d . . . C16 C 0.83792(13) 0.98570(15) 0.66398(10) 0.0276(5) Uani 1 1 d . . . C17 C 0.88975(13) 0.93780(15) 0.70573(9) 0.0269(5) Uani 1 1 d . . . C18 C 0.92194(13) 0.86390(14) 0.69046(9) 0.0238(5) Uani 1 1 d . . . C19 C 0.69905(13) 0.01600(15) 0.35051(10) 0.0294(5) Uani 1 1 d . . . C20 C 0.64160(14) 0.05562(15) 0.30765(9) 0.0282(5) Uani 1 1 d . . . C21 C 0.60186(13) 0.12473(14) 0.32106(9) 0.0245(5) Uani 1 1 d . . . C22 C 0.61420(12) 0.15591(13) 0.37566(9) 0.0215(4) Uani 1 1 d . . . C23 C 0.67336(12) 0.11434(14) 0.41676(9) 0.0234(5) Uani 1 1 d . . . C24 C 0.71614(13) 0.04619(15) 0.40549(9) 0.0283(5) Uani 1 1 d . . . C25 C 0.43558(13) 0.24037(15) 0.34827(9) 0.0255(5) Uani 1 1 d . . . C26 C 0.40010(13) 0.16101(15) 0.32909(9) 0.0286(5) Uani 1 1 d . . . C27 C 0.32182(14) 0.15221(18) 0.30057(10) 0.0372(6) Uani 1 1 d . . . C28 C 0.27582(14) 0.2254(2) 0.28987(11) 0.0415(7) Uani 1 1 d . . . C29 C 0.30776(15) 0.30577(19) 0.30811(11) 0.0413(7) Uani 1 1 d . . . C30 C 0.38569(15) 0.31130(16) 0.33694(10) 0.0335(6) Uani 1 1 d . . . C31 C 0.64956(13) 0.41273(15) 0.41221(10) 0.0270(5) Uani 1 1 d . . . C32 C 0.59207(13) 0.36664(14) 0.37321(9) 0.0240(5) Uani 1 1 d . . . C33 C 0.56658(13) 0.40455(15) 0.31978(9) 0.0276(5) Uani 1 1 d . . . C34 C 0.59403(14) 0.48254(15) 0.30580(10) 0.0295(5) Uani 1 1 d . . . C35 C 0.64993(14) 0.52648(15) 0.34706(11) 0.0322(5) Uani 1 1 d . . . C36 C 0.67876(13) 0.49171(16) 0.40079(11) 0.0316(5) Uani 1 1 d . . . C37 C 1.06884(16) 0.92326(17) 0.45017(11) 0.0418(7) Uani 1 1 d . . . H37A H 1.1147 0.8953 0.4452 0.063 Uiso 1 1 calc R . . H37B H 1.0736 0.9245 0.4907 0.063 Uiso 1 1 calc R . . H37C H 1.0644 0.9833 0.4354 0.063 Uiso 1 1 calc R . . C38 C 0.99617(14) 0.87084(15) 0.41744(10) 0.0305(5) Uani 1 1 d . . . C39 C 0.99296(19) 0.86482(18) 0.35520(10) 0.0483(7) Uani 1 1 d . . . H39A H 0.9977 0.9236 0.3408 0.072 Uiso 1 1 calc R . . H39B H 0.9436 0.8389 0.3328 0.072 Uiso 1 1 calc R . . H39C H 1.0356 0.8281 0.3521 0.072 Uiso 1 1 calc R . . C40 C 0.92653(16) 0.92419(17) 0.42274(12) 0.0462(7) Uani 1 1 d . . . H40A H 0.9266 0.9231 0.4623 0.069 Uiso 1 1 calc R . . H40B H 0.8783 0.8984 0.3981 0.069 Uiso 1 1 calc R . . H40C H 0.9306 0.9849 0.4111 0.069 Uiso 1 1 calc R . . C41 C 0.91773(15) 0.68615(16) 0.40731(10) 0.0357(6) Uani 1 1 d . . . C42 C 0.90326(18) 0.60730(17) 0.44146(11) 0.0477(8) Uani 1 1 d . . . H42A H 0.8651 0.5682 0.4161 0.072 Uiso 1 1 calc R . . H42B H 0.8837 0.6281 0.4717 0.072 Uiso 1 1 calc R . . H42C H 0.9518 0.5754 0.4583 0.072 Uiso 1 1 calc R . . C43 C 0.9387(2) 0.65082(19) 0.35570(11) 0.0573(9) Uani 1 1 d . . . H43A H 0.9838 0.6122 0.3689 0.086 Uiso 1 1 calc R . . H43B H 0.9507 0.7000 0.3345 0.086 Uiso 1 1 calc R . . H43C H 0.8948 0.6178 0.3309 0.086 Uiso 1 1 calc R . . C44 C 0.84276(16) 0.7383(2) 0.38607(13) 0.0580(9) Uani 1 1 d . . . H44A H 0.8486 0.7847 0.3604 0.087 Uiso 1 1 calc R . . H44B H 0.8310 0.7644 0.4185 0.087 Uiso 1 1 calc R . . H44C H 0.8005 0.6991 0.3656 0.087 Uiso 1 1 calc R . . C45 C 1.09614(14) 0.70652(16) 0.47240(11) 0.0339(6) Uani 1 1 d . . . C46 C 0.58491(13) 0.16114(14) 0.61220(9) 0.0252(5) Uani 1 1 d . . . C47 C 0.56071(16) 0.14634(16) 0.66573(9) 0.0365(6) Uani 1 1 d . . . H47A H 0.6035 0.1190 0.6954 0.055 Uiso 1 1 calc R . . H47B H 0.5154 0.1078 0.6564 0.055 Uiso 1 1 calc R . . H47C H 0.5479 0.2027 0.6794 0.055 Uiso 1 1 calc R . . C48 C 0.66031(13) 0.21460(16) 0.62775(10) 0.0335(6) Uani 1 1 d . . . H48A H 0.6529 0.2702 0.6451 0.050 Uiso 1 1 calc R . . H48B H 0.6742 0.2263 0.5933 0.050 Uiso 1 1 calc R . . H48C H 0.7019 0.1813 0.6548 0.050 Uiso 1 1 calc R . . C49 C 0.60299(14) 0.07228(15) 0.58960(10) 0.0303(5) Uani 1 1 d . . . H49A H 0.6228 0.0822 0.5576 0.046 Uiso 1 1 calc R . . H49B H 0.5557 0.0371 0.5768 0.046 Uiso 1 1 calc R . . H49C H 0.6420 0.0411 0.6200 0.046 Uiso 1 1 calc R . . C50 C 0.40743(13) 0.17201(15) 0.54026(10) 0.0279(5) Uani 1 1 d . . . C51 C 0.35779(13) 0.19552(17) 0.47914(10) 0.0377(6) Uani 1 1 d . . . H51A H 0.3045 0.1758 0.4727 0.057 Uiso 1 1 calc R . . H51B H 0.3790 0.1665 0.4520 0.057 Uiso 1 1 calc R . . H51C H 0.3584 0.2591 0.4739 0.057 Uiso 1 1 calc R . . C52 C 0.50659(15) 0.36216(15) 0.62852(10) 0.0334(6) Uani 1 1 d . . . H52A H 0.5548 0.3414 0.6560 0.050 Uiso 1 1 calc R . . H52B H 0.4627 0.3318 0.6350 0.050 Uiso 1 1 calc R . . H52C H 0.5015 0.4254 0.6332 0.050 Uiso 1 1 calc R . . C53 C 0.50774(13) 0.34308(13) 0.56781(9) 0.0237(5) Uani 1 1 d . . . C54 C 0.57913(14) 0.38902(15) 0.56025(10) 0.0316(5) Uani 1 1 d . . . H54A H 0.5777 0.4515 0.5690 0.047 Uiso 1 1 calc R . . H54B H 0.5789 0.3821 0.5209 0.047 Uiso 1 1 calc R . . H54C H 0.6262 0.3627 0.5860 0.047 Uiso 1 1 calc R . . C55 C 0.98472(12) 0.78357(14) 0.52215(8) 0.0210(4) Uani 1 1 d . . . C56 C 0.52797(12) 0.19754(13) 0.48702(8) 0.0194(4) Uani 1 1 d . . . C57 C 0.43640(14) 0.38601(15) 0.52467(10) 0.0327(6) Uani 1 1 d . . . H57A H 0.3892 0.3626 0.5302 0.049 Uiso 1 1 calc R . . H57B H 0.4364 0.3731 0.4859 0.049 Uiso 1 1 calc R . . H57C H 0.4384 0.4496 0.5306 0.049 Uiso 1 1 calc R . . C58 C 0.41214(14) 0.07094(15) 0.54321(11) 0.0345(6) Uani 1 1 d . . . H58A H 0.4379 0.0526 0.5826 0.052 Uiso 1 1 calc R . . H58B H 0.4417 0.0498 0.5189 0.052 Uiso 1 1 calc R . . H58C H 0.3598 0.0463 0.5300 0.052 Uiso 1 1 calc R . . C59 C 0.36725(15) 0.20379(18) 0.58283(12) 0.0415(6) Uani 1 1 d . . . H59A H 0.3186 0.1719 0.5764 0.062 Uiso 1 1 calc R . . H59B H 0.3565 0.2667 0.5775 0.062 Uiso 1 1 calc R . . H59C H 0.4011 0.1931 0.6217 0.062 Uiso 1 1 calc R . . C60 C 1.14958(15) 0.7506(2) 0.52689(12) 0.0485(7) Uani 1 1 d . . . H60A H 1.2014 0.7247 0.5367 0.073 Uiso 1 1 calc R . . H60B H 1.1285 0.7413 0.5583 0.073 Uiso 1 1 calc R . . H60C H 1.1528 0.8135 0.5202 0.073 Uiso 1 1 calc R . . C61 C 1.09144(19) 0.60950(18) 0.48815(14) 0.0574(8) Uani 1 1 d . . . H61A H 1.0638 0.5762 0.4540 0.086 Uiso 1 1 calc R . . H61B H 1.0637 0.6047 0.5161 0.086 Uiso 1 1 calc R . . H61C H 1.1438 0.5859 0.5044 0.086 Uiso 1 1 calc R . . C62 C 1.13364(18) 0.7128(2) 0.42547(13) 0.0549(8) Uani 1 1 d . . . H62A H 1.1843 0.6840 0.4380 0.082 Uiso 1 1 calc R . . H62B H 1.1403 0.7746 0.4172 0.082 Uiso 1 1 calc R . . H62C H 1.1005 0.6840 0.3911 0.082 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 Al3 0.0223(3) 0.0177(3) 0.0213(3) -0.0013(2) 0.0081(3) -0.0016(3) Al4 0.0270(3) 0.0165(3) 0.0196(3) 0.0004(2) 0.0090(3) -0.0029(3) O1 0.0279(8) 0.0221(8) 0.0241(7) -0.0009(6) 0.0129(6) -0.0061(6) O2 0.0516(11) 0.0249(9) 0.0326(9) -0.0107(7) 0.0194(8) -0.0119(8) O3 0.0433(10) 0.0170(8) 0.0270(8) -0.0041(6) 0.0165(7) -0.0037(7) O4 0.0325(8) 0.0205(8) 0.0217(7) -0.0010(6) 0.0137(6) -0.0060(6) P1 0.0200(3) 0.0143(3) 0.0201(3) -0.0001(2) 0.0089(2) -0.0006(2) P2 0.0255(3) 0.0151(3) 0.0240(3) -0.0024(2) 0.0128(2) -0.0034(2) F1 0.0428(8) 0.0206(7) 0.0529(9) -0.0032(6) 0.0208(7) 0.0016(6) F2 0.0471(10) 0.0571(11) 0.0744(11) 0.0175(9) 0.0295(9) 0.0296(8) F3 0.0215(8) 0.1209(17) 0.0601(11) -0.0025(11) 0.0072(7) 0.0093(9) F4 0.0393(9) 0.0848(13) 0.0576(10) -0.0316(9) 0.0163(8) -0.0324(9) F5 0.0437(9) 0.0282(8) 0.0564(9) -0.0188(7) 0.0229(7) -0.0105(6) F6 0.0322(8) 0.0407(9) 0.0393(8) 0.0194(6) 0.0007(6) -0.0059(6) F7 0.0375(9) 0.0602(11) 0.0458(9) 0.0085(8) -0.0022(7) -0.0260(8) F8 0.0487(9) 0.0320(8) 0.0672(10) 0.0134(7) 0.0236(8) -0.0139(7) F9 0.0449(10) 0.0741(12) 0.0746(12) 0.0567(10) 0.0123(9) -0.0015(9) F10 0.0299(8) 0.0789(12) 0.0344(8) 0.0233(8) -0.0024(6) -0.0134(8) F11 0.0414(8) 0.0326(8) 0.0243(7) 0.0073(5) 0.0099(6) 0.0154(6) F12 0.0549(9) 0.0393(8) 0.0270(7) -0.0047(6) 0.0137(7) 0.0150(7) F13 0.0453(9) 0.0291(8) 0.0495(9) -0.0003(6) 0.0192(7) 0.0170(6) F14 0.0307(7) 0.0420(9) 0.0385(8) 0.0135(6) 0.0079(6) 0.0150(6) F15 0.0289(7) 0.0410(8) 0.0237(6) 0.0013(6) 0.0058(5) 0.0027(6) F16 0.0311(7) 0.0425(8) 0.0225(6) -0.0039(6) 0.0067(5) 0.0001(6) F17 0.0339(8) 0.0515(9) 0.0378(8) 0.0078(7) 0.0073(6) 0.0158(7) F18 0.0508(9) 0.0391(9) 0.0494(9) -0.0034(7) 0.0217(7) 0.0185(7) F19 0.0591(10) 0.0362(8) 0.0274(7) -0.0078(6) 0.0157(7) 0.0057(7) F20 0.0453(8) 0.0340(8) 0.0222(6) 0.0036(6) 0.0063(6) 0.0098(6) F21 0.0328(8) 0.0454(9) 0.0334(7) 0.0049(6) 0.0072(6) -0.0076(7) F22 0.0425(9) 0.0497(10) 0.0572(10) -0.0100(8) 0.0161(8) -0.0262(8) F23 0.0557(10) 0.0235(8) 0.0766(11) 0.0075(7) 0.0346(9) -0.0124(7) F24 0.0631(10) 0.0383(9) 0.0450(9) 0.0203(7) 0.0202(8) -0.0020(8) F25 0.0592(10) 0.0326(8) 0.0260(7) 0.0004(6) 0.0112(7) -0.0152(7) F26 0.0522(10) 0.0312(8) 0.0583(10) -0.0046(7) 0.0228(8) 0.0087(7) F27 0.0475(10) 0.0701(12) 0.0712(12) 0.0160(9) 0.0229(9) 0.0311(9) F28 0.0251(8) 0.0994(15) 0.0526(10) 0.0217(10) 0.0044(7) -0.0050(8) F29 0.0428(9) 0.0572(11) 0.0529(10) 0.0034(8) 0.0027(7) -0.0287(8) F30 0.0379(8) 0.0243(7) 0.0413(8) 0.0041(6) 0.0055(6) -0.0070(6) C1 0.0251(11) 0.0220(11) 0.0243(10) -0.0002(9) 0.0120(9) 0.0004(9) C2 0.0247(12) 0.0353(14) 0.0280(12) 0.0074(10) 0.0072(10) -0.0024(10) C3 0.0336(13) 0.0351(14) 0.0413(14) 0.0209(11) 0.0141(11) 0.0039(11) C4 0.0351(13) 0.0219(12) 0.0434(14) 0.0052(10) 0.0194(11) -0.0062(10) C5 0.0287(12) 0.0290(13) 0.0339(13) 0.0001(10) 0.0089(10) -0.0079(10) C6 0.0275(12) 0.0217(11) 0.0250(11) 0.0057(9) 0.0087(9) 0.0004(9) C7 0.0256(11) 0.0234(11) 0.0223(10) -0.0025(9) 0.0115(9) -0.0017(9) C8 0.0272(12) 0.0284(13) 0.0290(12) 0.0009(9) 0.0135(10) -0.0005(10) C9 0.0329(14) 0.0419(15) 0.0399(14) 0.0090(12) 0.0197(11) 0.0127(12) C10 0.0189(12) 0.074(2) 0.0346(14) 0.0003(13) 0.0089(10) 0.0040(13) C11 0.0286(13) 0.0594(18) 0.0320(13) -0.0144(12) 0.0123(11) -0.0184(13) C12 0.0317(12) 0.0288(13) 0.0285(12) -0.0091(10) 0.0154(10) -0.0044(10) C13 0.0210(11) 0.0204(11) 0.0254(11) 0.0021(8) 0.0117(9) -0.0011(8) C14 0.0218(11) 0.0269(12) 0.0231(11) 0.0014(9) 0.0109(9) -0.0049(9) C15 0.0195(11) 0.0278(12) 0.0319(12) 0.0104(10) 0.0088(9) 0.0032(9) C16 0.0281(12) 0.0216(12) 0.0376(13) 0.0010(9) 0.0170(10) 0.0049(9) C17 0.0322(12) 0.0274(12) 0.0240(11) 0.0011(9) 0.0132(10) 0.0032(10) C18 0.0265(11) 0.0222(11) 0.0231(11) 0.0062(9) 0.0081(9) 0.0032(9) C19 0.0312(13) 0.0268(13) 0.0357(13) 0.0005(10) 0.0183(10) 0.0038(10) C20 0.0381(13) 0.0267(12) 0.0231(11) -0.0019(9) 0.0142(10) -0.0021(10) C21 0.0292(12) 0.0224(12) 0.0220(11) 0.0035(9) 0.0081(9) -0.0004(9) C22 0.0260(11) 0.0182(11) 0.0224(10) 0.0009(8) 0.0108(9) -0.0056(9) C23 0.0252(11) 0.0252(12) 0.0214(10) -0.0003(9) 0.0094(9) -0.0046(9) C24 0.0242(12) 0.0321(13) 0.0298(12) 0.0062(10) 0.0102(10) 0.0013(10) C25 0.0294(12) 0.0289(12) 0.0209(10) 0.0031(9) 0.0116(9) -0.0005(10) C26 0.0294(12) 0.0306(13) 0.0249(11) 0.0074(9) 0.0073(10) -0.0033(10) C27 0.0337(14) 0.0459(16) 0.0298(13) 0.0061(11) 0.0067(11) -0.0137(12) C28 0.0254(13) 0.066(2) 0.0336(13) 0.0151(13) 0.0095(11) -0.0003(13) C29 0.0350(14) 0.0529(18) 0.0410(15) 0.0139(13) 0.0190(12) 0.0172(13) C30 0.0394(14) 0.0305(14) 0.0345(13) 0.0013(11) 0.0172(11) 0.0033(11) C31 0.0259(12) 0.0277(12) 0.0325(12) 0.0019(10) 0.0165(10) 0.0014(10) C32 0.0311(12) 0.0177(11) 0.0276(11) -0.0005(9) 0.0155(10) 0.0011(9) C33 0.0349(13) 0.0219(12) 0.0296(12) -0.0011(9) 0.0152(10) -0.0028(10) C34 0.0387(13) 0.0220(12) 0.0344(13) 0.0076(10) 0.0212(11) 0.0049(10) C35 0.0342(13) 0.0183(12) 0.0529(15) 0.0044(11) 0.0263(12) -0.0023(10) C36 0.0255(12) 0.0282(13) 0.0460(14) -0.0092(11) 0.0181(11) -0.0102(10) C37 0.0569(17) 0.0254(13) 0.0498(16) 0.0003(11) 0.0263(14) -0.0157(12) C38 0.0407(14) 0.0182(11) 0.0356(13) 0.0047(9) 0.0165(11) -0.0018(10) C39 0.076(2) 0.0378(16) 0.0343(14) 0.0097(12) 0.0210(14) -0.0111(14) C40 0.0489(17) 0.0279(14) 0.0597(18) 0.0058(12) 0.0141(14) 0.0070(12) C41 0.0450(15) 0.0267(13) 0.0351(13) -0.0119(10) 0.0124(11) -0.0150(11) C42 0.070(2) 0.0354(15) 0.0455(15) -0.0169(12) 0.0300(14) -0.0353(14) C43 0.095(3) 0.0440(18) 0.0398(15) -0.0202(13) 0.0312(16) -0.0313(17) C44 0.0365(16) 0.064(2) 0.063(2) -0.0153(16) 0.0008(14) -0.0194(15) C45 0.0333(13) 0.0276(13) 0.0467(15) 0.0025(11) 0.0211(11) 0.0075(10) C46 0.0308(12) 0.0202(11) 0.0224(11) 0.0024(8) 0.0051(9) 0.0046(9) C47 0.0543(17) 0.0317(14) 0.0246(12) 0.0060(10) 0.0139(11) 0.0071(12) C48 0.0250(12) 0.0341(14) 0.0349(13) -0.0030(10) 0.0001(10) 0.0015(10) C49 0.0360(13) 0.0218(12) 0.0320(12) 0.0046(9) 0.0089(10) 0.0079(10) C50 0.0246(12) 0.0237(12) 0.0393(13) -0.0043(10) 0.0154(10) -0.0057(9) C51 0.0230(12) 0.0382(15) 0.0463(15) -0.0055(12) 0.0030(11) -0.0034(11) C52 0.0442(15) 0.0251(13) 0.0331(13) -0.0076(10) 0.0155(11) 0.0016(11) C53 0.0299(12) 0.0155(11) 0.0267(11) -0.0030(8) 0.0105(9) 0.0002(9) C54 0.0388(14) 0.0166(11) 0.0420(13) -0.0052(10) 0.0163(11) -0.0083(10) C55 0.0219(11) 0.0203(11) 0.0213(10) -0.0009(9) 0.0075(8) 0.0004(9) C56 0.0204(10) 0.0190(11) 0.0188(10) 0.0017(8) 0.0062(8) 0.0008(8) C57 0.0383(14) 0.0201(12) 0.0394(13) 0.0032(10) 0.0117(11) 0.0064(10) C58 0.0364(14) 0.0226(12) 0.0498(15) -0.0053(11) 0.0210(12) -0.0131(10) C59 0.0362(14) 0.0376(15) 0.0628(17) -0.0074(13) 0.0328(13) -0.0073(12) C60 0.0309(14) 0.0565(19) 0.0559(18) 0.0041(14) 0.0105(13) 0.0054(13) C61 0.063(2) 0.0353(17) 0.081(2) 0.0146(15) 0.0332(17) 0.0200(15) C62 0.0551(19) 0.0527(19) 0.071(2) 0.0031(16) 0.0399(16) 0.0129(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al3 O1 1.8311(15) . ? Al3 C13 1.998(2) . ? Al3 C7 1.999(2) . ? Al3 C1 1.999(2) . ? Al4 O4 1.8264(15) . ? Al4 C22 1.997(2) . ? Al4 C32 1.999(2) . ? Al4 C25 2.002(2) . ? O1 C55 1.289(3) . ? O2 C55 1.208(2) . ? O3 C56 1.211(2) . ? O4 C56 1.289(2) . ? P1 C56 1.884(2) . ? P1 C53 1.884(2) . ? P1 C46 1.891(2) . ? P1 C50 1.891(2) . ? P2 C41 1.882(2) . ? P2 C38 1.885(2) . ? P2 C55 1.885(2) . ? P2 C45 1.893(2) . ? F1 C8 1.360(3) . ? F2 C9 1.345(3) . ? F3 C10 1.347(3) . ? F4 C11 1.350(3) . ? F5 C12 1.352(3) . ? F6 C6 1.362(2) . ? F7 C5 1.342(3) . ? F8 C4 1.344(3) . ? F9 C3 1.340(3) . ? F10 C2 1.350(3) . ? F11 C18 1.359(2) . ? F12 C17 1.343(2) . ? F13 C16 1.349(2) . ? F14 C15 1.353(2) . ? F15 C14 1.360(2) . ? F16 C23 1.355(2) . ? F17 C24 1.346(2) . ? F18 C19 1.343(3) . ? F19 C20 1.343(2) . ? F20 C21 1.358(2) . ? F21 C31 1.360(3) . ? F22 C36 1.348(3) . ? F23 C35 1.348(3) . ? F24 C34 1.339(3) . ? F25 C33 1.356(3) . ? F26 C30 1.364(3) . ? F27 C29 1.353(3) . ? F28 C28 1.348(3) . ? F29 C27 1.348(3) . ? F30 C26 1.348(3) . ? C1 C6 1.380(3) . ? C1 C2 1.382(3) . ? C2 C3 1.383(3) . ? C3 C4 1.373(3) . ? C4 C5 1.375(3) . ? C5 C6 1.378(3) . ? C7 C12 1.381(3) . ? C7 C8 1.390(3) . ? C8 C9 1.375(3) . ? C9 C10 1.373(4) . ? C10 C11 1.379(4) . ? C11 C12 1.381(3) . ? C13 C14 1.378(3) . ? C13 C18 1.380(3) . ? C14 C15 1.382(3) . ? C15 C16 1.378(3) . ? C16 C17 1.372(3) . ? C17 C18 1.378(3) . ? C19 C20 1.374(3) . ? C19 C24 1.378(3) . ? C20 C21 1.378(3) . ? C21 C22 1.384(3) . ? C22 C23 1.382(3) . ? C23 C24 1.380(3) . ? C25 C30 1.384(3) . ? C25 C26 1.385(3) . ? C26 C27 1.384(3) . ? C27 C28 1.371(4) . ? C28 C29 1.372(4) . ? C29 C30 1.376(4) . ? C31 C32 1.374(3) . ? C31 C36 1.383(3) . ? C32 C33 1.384(3) . ? C33 C34 1.377(3) . ? C34 C35 1.370(3) . ? C35 C36 1.374(3) . ? C37 C38 1.541(3) . ? C38 C39 1.527(3) . ? C38 C40 1.547(4) . ? C41 C44 1.524(4) . ? C41 C42 1.541(3) . ? C41 C43 1.542(4) . ? C45 C62 1.526(4) . ? C45 C61 1.541(4) . ? C45 C60 1.548(4) . ? C46 C48 1.539(3) . ? C46 C47 1.540(3) . ? C46 C49 1.542(3) . ? C50 C59 1.539(3) . ? C50 C51 1.542(3) . ? C50 C58 1.546(3) . ? C52 C53 1.539(3) . ? C53 C54 1.540(3) . ? C53 C57 1.545(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 Al3 C13 112.87(8) . . ? O1 Al3 C7 102.25(8) . . ? C13 Al3 C7 116.14(9) . . ? O1 Al3 C1 103.80(8) . . ? C13 Al3 C1 107.52(9) . . ? C7 Al3 C1 113.61(9) . . ? O4 Al4 C22 113.89(8) . . ? O4 Al4 C32 104.24(8) . . ? C22 Al4 C32 108.31(9) . . ? O4 Al4 C25 102.50(8) . . ? C22 Al4 C25 114.56(9) . . ? C32 Al4 C25 112.87(9) . . ? C55 O1 Al3 118.08(13) . . ? C56 O4 Al4 118.89(13) . . ? C56 P1 C53 110.11(10) . . ? C56 P1 C46 105.10(10) . . ? C53 P1 C46 113.13(10) . . ? C56 P1 C50 101.43(10) . . ? C53 P1 C50 112.36(10) . . ? C46 P1 C50 113.74(10) . . ? C41 P2 C38 112.61(11) . . ? C41 P2 C55 110.74(10) . . ? C38 P2 C55 104.50(10) . . ? C41 P2 C45 113.46(12) . . ? C38 P2 C45 112.78(11) . . ? C55 P2 C45 101.81(10) . . ? C6 C1 C2 114.1(2) . . ? C6 C1 Al3 121.24(16) . . ? C2 C1 Al3 124.63(16) . . ? F10 C2 C1 119.9(2) . . ? F10 C2 C3 116.6(2) . . ? C1 C2 C3 123.5(2) . . ? F9 C3 C4 119.3(2) . . ? F9 C3 C2 121.3(2) . . ? C4 C3 C2 119.4(2) . . ? F8 C4 C3 120.1(2) . . ? F8 C4 C5 120.3(2) . . ? C3 C4 C5 119.6(2) . . ? F7 C5 C4 119.7(2) . . ? F7 C5 C6 121.7(2) . . ? C4 C5 C6 118.6(2) . . ? F6 C6 C5 116.37(19) . . ? F6 C6 C1 118.95(19) . . ? C5 C6 C1 124.7(2) . . ? C12 C7 C8 113.7(2) . . ? C12 C7 Al3 125.80(17) . . ? C8 C7 Al3 120.47(16) . . ? F1 C8 C9 116.0(2) . . ? F1 C8 C7 118.90(19) . . ? C9 C8 C7 125.0(2) . . ? F2 C9 C10 120.3(2) . . ? F2 C9 C8 121.4(2) . . ? C10 C9 C8 118.3(2) . . ? F3 C10 C9 120.2(3) . . ? F3 C10 C11 119.8(3) . . ? C9 C10 C11 119.9(2) . . ? F4 C11 C10 119.8(2) . . ? F4 C11 C12 120.9(3) . . ? C10 C11 C12 119.2(2) . . ? F5 C12 C11 117.1(2) . . ? F5 C12 C7 119.1(2) . . ? C11 C12 C7 123.8(2) . . ? C14 C13 C18 114.34(19) . . ? C14 C13 Al3 124.58(16) . . ? C18 C13 Al3 121.08(15) . . ? F15 C14 C13 120.24(19) . . ? F15 C14 C15 115.94(18) . . ? C13 C14 C15 123.8(2) . . ? F14 C15 C16 119.4(2) . . ? F14 C15 C14 121.6(2) . . ? C16 C15 C14 118.95(19) . . ? F13 C16 C17 120.2(2) . . ? F13 C16 C15 120.1(2) . . ? C17 C16 C15 119.8(2) . . ? F12 C17 C16 119.5(2) . . ? F12 C17 C18 121.75(19) . . ? C16 C17 C18 118.7(2) . . ? F11 C18 C17 116.85(18) . . ? F11 C18 C13 118.80(19) . . ? C17 C18 C13 124.35(19) . . ? F18 C19 C20 119.8(2) . . ? F18 C19 C24 120.4(2) . . ? C20 C19 C24 119.8(2) . . ? F19 C20 C19 119.7(2) . . ? F19 C20 C21 121.6(2) . . ? C19 C20 C21 118.7(2) . . ? F20 C21 C20 117.04(18) . . ? F20 C21 C22 118.71(19) . . ? C20 C21 C22 124.3(2) . . ? C23 C22 C21 114.3(2) . . ? C23 C22 Al4 125.65(16) . . ? C21 C22 Al4 120.05(16) . . ? F16 C23 C24 116.45(19) . . ? F16 C23 C22 119.76(19) . . ? C24 C23 C22 123.8(2) . . ? F17 C24 C19 119.4(2) . . ? F17 C24 C23 121.5(2) . . ? C19 C24 C23 119.1(2) . . ? C30 C25 C26 114.1(2) . . ? C30 C25 Al4 122.25(18) . . ? C26 C25 Al4 123.62(17) . . ? F30 C26 C27 116.7(2) . . ? F30 C26 C25 119.6(2) . . ? C27 C26 C25 123.7(2) . . ? F29 C27 C28 119.7(2) . . ? F29 C27 C26 121.0(2) . . ? C28 C27 C26 119.2(2) . . ? F28 C28 C27 120.3(3) . . ? F28 C28 C29 120.1(3) . . ? C27 C28 C29 119.7(2) . . ? F27 C29 C28 119.5(2) . . ? F27 C29 C30 121.3(3) . . ? C28 C29 C30 119.1(2) . . ? F26 C30 C29 116.9(2) . . ? F26 C30 C25 119.0(2) . . ? C29 C30 C25 124.2(2) . . ? F21 C31 C32 119.6(2) . . ? F21 C31 C36 116.3(2) . . ? C32 C31 C36 124.0(2) . . ? C31 C32 C33 114.2(2) . . ? C31 C32 Al4 124.33(16) . . ? C33 C32 Al4 121.42(16) . . ? F25 C33 C34 116.2(2) . . ? F25 C33 C32 119.53(19) . . ? C34 C33 C32 124.3(2) . . ? F24 C34 C35 120.1(2) . . ? F24 C34 C33 121.3(2) . . ? C35 C34 C33 118.6(2) . . ? F23 C35 C34 120.1(2) . . ? F23 C35 C36 119.8(2) . . ? C34 C35 C36 120.1(2) . . ? F22 C36 C35 120.1(2) . . ? F22 C36 C31 121.2(2) . . ? C35 C36 C31 118.7(2) . . ? C39 C38 C37 108.4(2) . . ? C39 C38 C40 110.2(2) . . ? C37 C38 C40 105.9(2) . . ? C39 C38 P2 112.44(17) . . ? C37 C38 P2 110.31(16) . . ? C40 C38 P2 109.37(17) . . ? C44 C41 C42 107.9(2) . . ? C44 C41 C43 108.9(2) . . ? C42 C41 C43 108.2(2) . . ? C44 C41 P2 109.35(17) . . ? C42 C41 P2 112.62(17) . . ? C43 C41 P2 109.75(18) . . ? C62 C45 C61 109.1(2) . . ? C62 C45 C60 109.1(2) . . ? C61 C45 C60 105.4(2) . . ? C62 C45 P2 111.91(18) . . ? C61 C45 P2 111.08(19) . . ? C60 C45 P2 109.91(17) . . ? C48 C46 C47 109.69(19) . . ? C48 C46 C49 106.35(19) . . ? C47 C46 C49 109.60(18) . . ? C48 C46 P1 109.25(15) . . ? C47 C46 P1 111.21(16) . . ? C49 C46 P1 110.61(14) . . ? C59 C50 C51 110.0(2) . . ? C59 C50 C58 108.3(2) . . ? C51 C50 C58 106.58(19) . . ? C59 C50 P1 111.91(16) . . ? C51 C50 P1 109.39(16) . . ? C58 C50 P1 110.59(16) . . ? C52 C53 C54 107.73(18) . . ? C52 C53 C57 109.19(19) . . ? C54 C53 C57 106.35(18) . . ? C52 C53 P1 110.19(15) . . ? C54 C53 P1 113.04(15) . . ? C57 C53 P1 110.20(15) . . ? O2 C55 O1 125.8(2) . . ? O2 C55 P2 118.73(17) . . ? O1 C55 P2 115.32(15) . . ? O3 C56 O4 126.15(19) . . ? O3 C56 P1 117.35(16) . . ? O4 C56 P1 116.47(15) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.85 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.527 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.059 #===end data_compound4_C47H37BClF20O2PTi _database_code_depnum_ccdc_archive 'CCDC 864918' #TrackingRef 'combined-cifs-revised.txt' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C47 H37 B Cl F20 O2 P Ti' _chemical_formula_weight 1138.90 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7349(9) _cell_length_b 14.4145(12) _cell_length_c 15.0880(11) _cell_angle_alpha 85.942(4) _cell_angle_beta 88.205(4) _cell_angle_gamma 81.850(5) _cell_volume 2304.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5033 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 23.01 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method ? _exptl_crystal_F_000 1148 _exptl_absorpt_coefficient_mu 0.400 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7056 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35285 _diffrn_reflns_av_R_equivalents 0.0578 _diffrn_reflns_av_sigmaI/netI 0.0833 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 27.57 _reflns_number_total 10393 _reflns_number_gt 6346 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0399P)^2^+0.4528P] 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 10393 _refine_ls_number_parameters 707 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1021 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1080 _refine_ls_wR_factor_gt 0.0911 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.000 _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 0.46903(5) 0.43578(3) 0.24380(3) 0.02196(13) Uani 1 1 d . . . P1 P 0.26754(7) 0.16576(5) 0.28294(5) 0.02028(17) Uani 1 1 d . . . F1 F 0.23687(14) 0.35232(10) 0.89193(10) 0.0284(4) Uani 1 1 d . . . F2 F 0.10718(15) 0.42721(11) 1.02686(10) 0.0316(4) Uani 1 1 d . . . F3 F -0.13095(15) 0.39130(11) 1.06605(10) 0.0342(4) Uani 1 1 d . . . F4 F -0.23720(14) 0.27603(11) 0.96420(10) 0.0298(4) Uani 1 1 d . . . F5 F -0.10096(13) 0.18672(10) 0.83650(10) 0.0263(4) Uani 1 1 d . . . F6 F 0.09886(15) 0.08054(11) 0.93850(10) 0.0305(4) Uani 1 1 d . . . F7 F 0.14059(16) -0.10336(11) 0.94987(11) 0.0399(4) Uani 1 1 d . . . F8 F 0.22394(15) -0.20103(11) 0.80655(12) 0.0371(4) Uani 1 1 d . . . F9 F 0.26828(15) -0.10447(11) 0.64809(11) 0.0348(4) Uani 1 1 d . . . F10 F 0.23111(14) 0.08217(10) 0.63537(10) 0.0273(4) Uani 1 1 d . . . F11 F -0.03136(14) 0.11848(10) 0.65577(10) 0.0288(4) Uani 1 1 d . . . F12 F -0.18291(15) 0.20964(12) 0.53482(10) 0.0356(4) Uani 1 1 d . . . F13 F -0.19073(16) 0.39826(12) 0.49840(11) 0.0413(5) Uani 1 1 d . . . F14 F -0.03794(16) 0.49328(11) 0.58893(11) 0.0358(4) Uani 1 1 d . . . F15 F 0.11869(14) 0.40315(10) 0.70986(10) 0.0271(4) Uani 1 1 d . . . F16 F 0.29013(14) 0.27830(11) 0.60403(10) 0.0267(4) Uani 1 1 d . . . F17 F 0.53539(14) 0.27623(11) 0.58953(11) 0.0340(4) Uani 1 1 d . . . F18 F 0.68612(14) 0.22255(12) 0.73126(12) 0.0392(4) Uani 1 1 d . . . F19 F 0.58145(15) 0.16962(12) 0.89101(11) 0.0385(4) Uani 1 1 d . . . F20 F 0.33484(14) 0.16534(11) 0.90648(10) 0.0291(4) Uani 1 1 d . . . O1 O 0.37776(17) 0.32321(12) 0.26674(12) 0.0244(4) Uani 1 1 d . . . O2 O 0.49740(18) 0.19317(14) 0.22383(14) 0.0345(5) Uani 1 1 d . . . C1 C 0.6132(3) 0.3427(3) 0.3428(2) 0.0397(9) Uani 1 1 d . . . C2 C 0.6807(3) 0.4014(2) 0.2901(3) 0.0410(8) Uani 1 1 d . . . C3 C 0.6339(3) 0.4950(2) 0.3096(2) 0.0417(9) Uani 1 1 d . . . C4 C 0.5423(4) 0.4915(2) 0.3757(2) 0.0448(9) Uani 1 1 d . . . C5 C 0.5259(4) 0.3971(2) 0.3949(2) 0.0421(9) Uani 1 1 d . . . C6 C 0.5638(3) 0.3897(2) 0.1082(2) 0.0337(8) Uani 1 1 d . . . C7 C 0.5848(3) 0.4827(2) 0.1168(2) 0.0358(8) Uani 1 1 d . . . C11 C 0.4004(3) 0.23659(19) 0.25251(17) 0.0229(6) Uani 1 1 d . . . C12 C 0.3422(3) 0.07865(19) 0.37069(18) 0.0285(7) Uani 1 1 d . . . C13 C 0.4178(3) 0.1277(2) 0.43365(19) 0.0331(7) Uani 1 1 d . . . H13A H 0.3618 0.1777 0.4613 0.050 Uiso 1 1 calc R . . H13B H 0.4850 0.1547 0.3998 0.050 Uiso 1 1 calc R . . H13C H 0.4549 0.0818 0.4799 0.050 Uiso 1 1 calc R . . C14 C 0.4367(3) 0.0034(2) 0.3276(2) 0.0387(8) Uani 1 1 d . . . H14A H 0.4824 -0.0374 0.3742 0.058 Uiso 1 1 calc R . . H14B H 0.4966 0.0340 0.2895 0.058 Uiso 1 1 calc R . . H14C H 0.3913 -0.0344 0.2917 0.058 Uiso 1 1 calc R . . C15 C 0.2451(3) 0.0286(2) 0.4254(2) 0.0390(8) Uani 1 1 d . . . H15A H 0.1941 -0.0003 0.3853 0.059 Uiso 1 1 calc R . . H15B H 0.1903 0.0744 0.4593 0.059 Uiso 1 1 calc R . . H15C H 0.2888 -0.0201 0.4665 0.059 Uiso 1 1 calc R . . C16 C 0.1278(3) 0.2461(2) 0.32721(18) 0.0268(7) Uani 1 1 d . . . C17 C 0.0125(3) 0.1955(2) 0.3399(2) 0.0393(8) Uani 1 1 d . . . H17A H 0.0326 0.1391 0.3799 0.059 Uiso 1 1 calc R . . H17B H -0.0122 0.1776 0.2823 0.059 Uiso 1 1 calc R . . H17C H -0.0569 0.2374 0.3658 0.059 Uiso 1 1 calc R . . C18 C 0.0929(3) 0.3356(2) 0.2650(2) 0.0348(8) Uani 1 1 d . . . H18A H 0.0656 0.3179 0.2079 0.052 Uiso 1 1 calc R . . H18B H 0.1666 0.3684 0.2552 0.052 Uiso 1 1 calc R . . H18C H 0.0245 0.3771 0.2925 0.052 Uiso 1 1 calc R . . C19 C 0.1616(3) 0.2789(2) 0.41728(19) 0.0327(7) Uani 1 1 d . . . H19A H 0.0925 0.3246 0.4383 0.049 Uiso 1 1 calc R . . H19B H 0.2386 0.3083 0.4102 0.049 Uiso 1 1 calc R . . H19C H 0.1753 0.2247 0.4606 0.049 Uiso 1 1 calc R . . C20 C 0.2326(3) 0.1104(2) 0.17826(18) 0.0280(7) Uani 1 1 d . . . C21 C 0.1611(3) 0.0263(2) 0.2001(2) 0.0368(8) Uani 1 1 d . . . H21A H 0.0877 0.0454 0.2382 0.055 Uiso 1 1 calc R . . H21B H 0.2168 -0.0246 0.2312 0.055 Uiso 1 1 calc R . . H21C H 0.1333 0.0045 0.1449 0.055 Uiso 1 1 calc R . . C22 C 0.1503(3) 0.1839(2) 0.1192(2) 0.0377(8) Uani 1 1 d . . . H22A H 0.1900 0.2412 0.1109 0.057 Uiso 1 1 calc R . . H22B H 0.0671 0.1984 0.1475 0.057 Uiso 1 1 calc R . . H22C H 0.1413 0.1591 0.0612 0.057 Uiso 1 1 calc R . . C23 C 0.3515(3) 0.0783(2) 0.12344(19) 0.0363(8) Uani 1 1 d . . . H23A H 0.3288 0.0463 0.0723 0.054 Uiso 1 1 calc R . . H23B H 0.4102 0.0349 0.1605 0.054 Uiso 1 1 calc R . . H23C H 0.3916 0.1330 0.1025 0.054 Uiso 1 1 calc R . . C24 C 0.0765(2) 0.26217(17) 0.85736(16) 0.0176(6) Uani 1 1 d . . . C25 C 0.1204(2) 0.32667(18) 0.90784(18) 0.0206(6) Uani 1 1 d . . . C26 C 0.0537(3) 0.36927(18) 0.97688(17) 0.0217(6) Uani 1 1 d . . . C27 C -0.0658(3) 0.35186(19) 0.99735(17) 0.0235(6) Uani 1 1 d . . . C28 C -0.1177(2) 0.29173(19) 0.94699(18) 0.0222(6) Uani 1 1 d . . . C29 C -0.0463(2) 0.24832(18) 0.88065(17) 0.0204(6) Uani 1 1 d . . . C30 C 0.1590(2) 0.09325(18) 0.78519(17) 0.0188(6) Uani 1 1 d . . . C31 C 0.1408(2) 0.03993(19) 0.86301(18) 0.0217(6) Uani 1 1 d . . . C32 C 0.1632(3) -0.05709(19) 0.87144(19) 0.0257(7) Uani 1 1 d . . . C33 C 0.2063(3) -0.10604(19) 0.7997(2) 0.0273(7) Uani 1 1 d . . . C34 C 0.2273(3) -0.05732(19) 0.72044(19) 0.0257(7) Uani 1 1 d . . . C35 C 0.2053(2) 0.03889(19) 0.71524(17) 0.0208(6) Uani 1 1 d . . . C36 C 0.0567(2) 0.25483(18) 0.68815(17) 0.0187(6) Uani 1 1 d . . . C37 C -0.0252(2) 0.21209(19) 0.64108(18) 0.0222(6) Uani 1 1 d . . . C38 C -0.1065(2) 0.2579(2) 0.57801(18) 0.0242(6) Uani 1 1 d . . . C39 C -0.1110(3) 0.3527(2) 0.55925(18) 0.0255(7) Uani 1 1 d . . . C40 C -0.0335(3) 0.39986(19) 0.60488(18) 0.0250(6) Uani 1 1 d . . . C41 C 0.0463(2) 0.35121(19) 0.66612(17) 0.0214(6) Uani 1 1 d . . . C42 C 0.2963(2) 0.22436(17) 0.75741(17) 0.0182(6) Uani 1 1 d . . . C43 C 0.3558(2) 0.25139(18) 0.67886(17) 0.0205(6) Uani 1 1 d . . . C44 C 0.4846(3) 0.25164(18) 0.66963(18) 0.0231(6) Uani 1 1 d . . . C45 C 0.5614(2) 0.22510(19) 0.7401(2) 0.0269(7) Uani 1 1 d . . . C46 C 0.5080(3) 0.19704(19) 0.82008(19) 0.0257(7) Uani 1 1 d . . . C47 C 0.3799(3) 0.19657(18) 0.82623(18) 0.0226(6) Uani 1 1 d . . . Cl Cl 0.29589(8) 0.53987(6) 0.28538(6) 0.0452(2) Uani 1 1 d . . . B1 B 0.1467(3) 0.2090(2) 0.7714(2) 0.0192(7) Uani 1 1 d . . . C8 C 0.4685(3) 0.5393(2) 0.1148(2) 0.0382(8) Uani 1 1 d . . . C10 C 0.4346(3) 0.3916(2) 0.09675(19) 0.0370(8) Uani 1 1 d . . . C9 C 0.3752(3) 0.4828(3) 0.1021(2) 0.0403(8) Uani 1 1 d . . . H8A H 0.455(3) 0.604(2) 0.125(2) 0.059(11) Uiso 1 1 d . . . H1A H 0.619(3) 0.277(2) 0.343(2) 0.047(10) Uiso 1 1 d . . . H4A H 0.489(3) 0.539(2) 0.3966(18) 0.029(9) Uiso 1 1 d . . . H3A H 0.662(3) 0.551(2) 0.281(2) 0.047(10) Uiso 1 1 d . . . H9A H 0.286(3) 0.502(2) 0.102(2) 0.044(10) Uiso 1 1 d . . . H10A H 0.393(3) 0.339(2) 0.0886(18) 0.033(8) Uiso 1 1 d . . . H6A H 0.620(3) 0.336(2) 0.1103(18) 0.028(8) Uiso 1 1 d . . . H5A H 0.458(3) 0.380(2) 0.432(2) 0.060(11) Uiso 1 1 d . . . H7A H 0.668(3) 0.500(2) 0.124(2) 0.059(11) Uiso 1 1 d . . . H2A H 0.747(3) 0.386(3) 0.245(2) 0.073(13) Uiso 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 0.0230(3) 0.0196(3) 0.0238(3) -0.0029(2) 0.0028(2) -0.0050(2) P1 0.0232(4) 0.0206(4) 0.0181(4) -0.0018(3) -0.0026(3) -0.0058(3) F1 0.0239(9) 0.0284(9) 0.0367(10) -0.0111(8) 0.0035(7) -0.0131(7) F2 0.0351(10) 0.0289(9) 0.0334(9) -0.0149(8) -0.0059(8) -0.0055(8) F3 0.0343(10) 0.0364(10) 0.0312(10) -0.0119(8) 0.0089(8) 0.0001(8) F4 0.0193(8) 0.0323(10) 0.0373(10) -0.0021(8) 0.0064(7) -0.0038(7) F5 0.0228(9) 0.0288(9) 0.0306(9) -0.0084(7) -0.0004(7) -0.0123(7) F6 0.0418(10) 0.0270(9) 0.0227(9) -0.0023(7) 0.0044(7) -0.0052(8) F7 0.0492(11) 0.0295(10) 0.0385(11) 0.0135(8) 0.0050(9) -0.0065(8) F8 0.0357(10) 0.0169(9) 0.0577(12) 0.0007(8) -0.0050(9) -0.0013(7) F9 0.0394(10) 0.0269(9) 0.0373(10) -0.0138(8) 0.0015(8) 0.0033(8) F10 0.0338(9) 0.0255(9) 0.0226(9) -0.0026(7) 0.0053(7) -0.0045(7) F11 0.0310(9) 0.0243(9) 0.0339(9) -0.0031(7) -0.0075(7) -0.0117(7) F12 0.0313(10) 0.0445(11) 0.0337(10) -0.0059(8) -0.0103(8) -0.0107(8) F13 0.0419(11) 0.0455(11) 0.0333(10) 0.0065(9) -0.0151(8) 0.0032(9) F14 0.0465(11) 0.0238(9) 0.0350(10) 0.0042(8) 0.0012(8) -0.0009(8) F15 0.0286(9) 0.0231(9) 0.0314(9) -0.0011(7) -0.0018(7) -0.0098(7) F16 0.0246(9) 0.0332(10) 0.0217(9) 0.0018(7) 0.0000(7) -0.0043(7) F17 0.0270(9) 0.0381(10) 0.0358(10) 0.0020(8) 0.0114(8) -0.0058(8) F18 0.0162(9) 0.0430(11) 0.0583(12) 0.0017(9) -0.0013(8) -0.0066(8) F19 0.0269(9) 0.0446(11) 0.0448(11) 0.0037(9) -0.0148(8) -0.0079(8) F20 0.0304(9) 0.0343(10) 0.0235(9) 0.0030(7) -0.0018(7) -0.0090(8) O1 0.0291(11) 0.0210(11) 0.0247(10) -0.0021(8) 0.0031(9) -0.0098(9) O2 0.0281(12) 0.0292(12) 0.0464(13) -0.0075(10) 0.0048(10) -0.0029(10) C1 0.044(2) 0.0304(19) 0.046(2) 0.0001(17) -0.0241(17) -0.0072(17) C2 0.0300(19) 0.039(2) 0.056(2) -0.0031(18) -0.0128(18) -0.0095(16) C3 0.047(2) 0.032(2) 0.051(2) 0.0001(17) -0.0153(18) -0.0205(17) C4 0.070(3) 0.031(2) 0.037(2) -0.0114(17) -0.0123(19) -0.0112(19) C5 0.059(2) 0.045(2) 0.0273(18) -0.0023(16) -0.0119(17) -0.0199(19) C6 0.045(2) 0.0280(18) 0.0261(17) 0.0003(14) 0.0117(15) -0.0014(16) C7 0.035(2) 0.040(2) 0.0334(18) 0.0042(15) 0.0108(15) -0.0167(17) C11 0.0334(17) 0.0189(15) 0.0167(14) 0.0003(12) -0.0047(12) -0.0043(13) C12 0.0404(18) 0.0216(16) 0.0244(16) 0.0016(13) -0.0064(14) -0.0075(14) C13 0.0396(19) 0.0344(18) 0.0253(16) 0.0025(14) -0.0135(14) -0.0047(15) C14 0.052(2) 0.0224(17) 0.0394(19) -0.0016(14) -0.0176(16) 0.0059(15) C15 0.059(2) 0.0329(19) 0.0268(17) 0.0097(14) -0.0100(16) -0.0174(17) C16 0.0230(16) 0.0304(17) 0.0288(16) -0.0089(14) -0.0002(13) -0.0065(13) C17 0.0340(19) 0.047(2) 0.0389(19) -0.0035(16) 0.0035(15) -0.0121(16) C18 0.0309(18) 0.0320(18) 0.0392(19) 0.0002(15) -0.0062(14) 0.0033(14) C19 0.0318(17) 0.0369(18) 0.0302(17) -0.0126(14) 0.0044(14) -0.0038(14) C20 0.0394(18) 0.0243(16) 0.0223(15) -0.0043(13) -0.0073(13) -0.0085(14) C21 0.050(2) 0.0297(17) 0.0355(18) -0.0053(15) -0.0104(15) -0.0167(15) C22 0.056(2) 0.0319(18) 0.0269(17) -0.0022(14) -0.0180(15) -0.0078(16) C23 0.051(2) 0.0347(18) 0.0251(17) -0.0103(14) 0.0008(15) -0.0103(16) C24 0.0190(14) 0.0161(14) 0.0176(13) 0.0007(11) -0.0013(11) -0.0027(11) C25 0.0159(14) 0.0211(15) 0.0254(15) -0.0008(12) 0.0009(12) -0.0052(12) C26 0.0274(16) 0.0170(14) 0.0218(15) -0.0027(12) -0.0056(12) -0.0053(12) C27 0.0259(16) 0.0229(15) 0.0194(14) -0.0023(12) 0.0044(12) 0.0042(12) C28 0.0164(14) 0.0219(15) 0.0275(15) 0.0030(12) 0.0026(12) -0.0035(12) C29 0.0234(15) 0.0171(14) 0.0210(14) -0.0008(12) -0.0013(12) -0.0037(12) C30 0.0151(14) 0.0203(14) 0.0219(14) -0.0023(12) -0.0012(11) -0.0054(11) C31 0.0203(15) 0.0219(15) 0.0241(15) -0.0056(13) -0.0010(12) -0.0052(12) C32 0.0232(15) 0.0240(16) 0.0304(17) 0.0062(13) -0.0029(13) -0.0085(13) C33 0.0237(16) 0.0161(15) 0.0420(19) -0.0006(14) -0.0065(14) -0.0016(12) C34 0.0213(15) 0.0242(16) 0.0318(17) -0.0078(14) -0.0006(13) -0.0011(12) C35 0.0191(14) 0.0222(15) 0.0218(15) 0.0000(12) -0.0014(12) -0.0059(12) C36 0.0173(14) 0.0213(15) 0.0174(14) -0.0016(11) 0.0035(11) -0.0035(11) C37 0.0205(15) 0.0215(15) 0.0256(15) -0.0028(12) 0.0037(12) -0.0064(12) C38 0.0189(15) 0.0343(17) 0.0216(15) -0.0071(13) -0.0008(12) -0.0080(13) C39 0.0227(15) 0.0349(18) 0.0167(14) 0.0019(13) 0.0000(12) 0.0015(13) C40 0.0274(16) 0.0218(16) 0.0244(16) 0.0012(13) 0.0070(13) -0.0019(13) C41 0.0174(14) 0.0267(16) 0.0219(15) -0.0058(13) 0.0009(12) -0.0075(12) C42 0.0182(14) 0.0153(14) 0.0219(14) -0.0032(11) -0.0011(11) -0.0040(11) C43 0.0228(15) 0.0150(14) 0.0237(15) -0.0016(12) -0.0035(12) -0.0012(11) C44 0.0217(15) 0.0184(15) 0.0297(16) -0.0035(13) 0.0073(13) -0.0049(12) C45 0.0151(15) 0.0216(15) 0.0448(19) -0.0059(14) 0.0021(14) -0.0039(12) C46 0.0215(15) 0.0225(15) 0.0341(17) -0.0047(13) -0.0088(13) -0.0030(12) C47 0.0267(16) 0.0192(15) 0.0230(15) -0.0035(12) 0.0035(13) -0.0064(12) Cl 0.0382(5) 0.0318(4) 0.0641(6) -0.0122(4) 0.0205(4) -0.0002(4) B1 0.0194(16) 0.0198(16) 0.0198(16) -0.0047(13) 0.0017(13) -0.0063(13) C8 0.056(2) 0.0253(18) 0.0325(19) 0.0053(15) 0.0067(16) -0.0080(17) C10 0.053(2) 0.040(2) 0.0223(17) 0.0021(15) 0.0003(15) -0.0241(18) C9 0.040(2) 0.048(2) 0.0322(19) 0.0104(16) -0.0033(16) -0.0076(18) _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 2.0156(18) . ? Ti1 Cl 2.3171(9) . ? Ti1 C3 2.347(3) . ? Ti1 C6 2.352(3) . ? Ti1 C7 2.362(3) . ? Ti1 C8 2.367(3) . ? Ti1 C2 2.372(3) . ? Ti1 C5 2.386(3) . ? Ti1 C1 2.387(3) . ? Ti1 C4 2.393(3) . ? Ti1 C9 2.404(3) . ? Ti1 C10 2.405(3) . ? P1 C12 1.876(3) . ? P1 C20 1.890(3) . ? P1 C16 1.895(3) . ? P1 C11 1.896(3) . ? F1 C25 1.363(3) . ? F2 C26 1.359(3) . ? F3 C27 1.346(3) . ? F4 C28 1.349(3) . ? F5 C29 1.354(3) . ? F6 C31 1.353(3) . ? F7 C32 1.349(3) . ? F8 C33 1.352(3) . ? F9 C34 1.355(3) . ? F10 C35 1.356(3) . ? F11 C37 1.363(3) . ? F12 C38 1.356(3) . ? F13 C39 1.346(3) . ? F14 C40 1.345(3) . ? F15 C41 1.367(3) . ? F16 C43 1.354(3) . ? F17 C44 1.355(3) . ? F18 C45 1.337(3) . ? F19 C46 1.352(3) . ? F20 C47 1.360(3) . ? O1 C11 1.270(3) . ? O2 C11 1.220(3) . ? C1 C2 1.384(5) . ? C1 C5 1.395(5) . ? C2 C3 1.419(5) . ? C3 C4 1.382(5) . ? C4 C5 1.405(5) . ? C6 C10 1.400(5) . ? C6 C7 1.405(4) . ? C7 C8 1.391(5) . ? C12 C15 1.538(4) . ? C12 C13 1.538(4) . ? C12 C14 1.542(4) . ? C16 C17 1.524(4) . ? C16 C19 1.540(4) . ? C16 C18 1.549(4) . ? C20 C22 1.532(4) . ? C20 C23 1.533(4) . ? C20 C21 1.535(4) . ? C24 C25 1.383(3) . ? C24 C29 1.392(3) . ? C24 B1 1.659(4) . ? C25 C26 1.376(4) . ? C26 C27 1.364(4) . ? C27 C28 1.377(4) . ? C28 C29 1.373(4) . ? C30 C31 1.381(4) . ? C30 C35 1.396(4) . ? C30 B1 1.653(4) . ? C31 C32 1.382(4) . ? C32 C33 1.366(4) . ? C33 C34 1.373(4) . ? C34 C35 1.370(4) . ? C36 C37 1.382(4) . ? C36 C41 1.395(4) . ? C36 B1 1.651(4) . ? C37 C38 1.380(4) . ? C38 C39 1.370(4) . ? C39 C40 1.375(4) . ? C40 C41 1.366(4) . ? C42 C43 1.386(4) . ? C42 C47 1.394(4) . ? C42 B1 1.658(4) . ? C43 C44 1.386(4) . ? C44 C45 1.365(4) . ? C45 C46 1.379(4) . ? C46 C47 1.376(4) . ? C8 C9 1.403(5) . ? C10 C9 1.384(5) . ? 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 Cl 93.09(6) . . ? O1 Ti1 C3 136.07(11) . . ? Cl Ti1 C3 101.82(9) . . ? O1 Ti1 C6 95.78(9) . . ? Cl Ti1 C6 135.49(9) . . ? C3 Ti1 C6 101.42(13) . . ? O1 Ti1 C7 129.83(10) . . ? Cl Ti1 C7 116.57(9) . . ? C3 Ti1 C7 78.98(13) . . ? C6 Ti1 C7 34.69(11) . . ? O1 Ti1 C8 128.59(10) . . ? Cl Ti1 C8 83.65(9) . . ? C3 Ti1 C8 94.28(13) . . ? C6 Ti1 C8 57.20(12) . . ? C7 Ti1 C8 34.22(11) . . ? O1 Ti1 C2 111.15(10) . . ? Cl Ti1 C2 134.58(9) . . ? C3 Ti1 C2 34.99(11) . . ? C6 Ti1 C2 81.33(13) . . ? C7 Ti1 C2 76.87(13) . . ? C8 Ti1 C2 106.83(13) . . ? O1 Ti1 C5 81.72(10) . . ? Cl Ti1 C5 91.72(10) . . ? C3 Ti1 C5 57.03(13) . . ? C6 Ti1 C5 132.70(13) . . ? C7 Ti1 C5 132.26(13) . . ? C8 Ti1 C5 149.44(12) . . ? C2 Ti1 C5 56.78(13) . . ? O1 Ti1 C1 80.75(10) . . ? Cl Ti1 C1 125.70(9) . . ? C3 Ti1 C1 56.95(12) . . ? C6 Ti1 C1 98.79(13) . . ? C7 Ti1 C1 107.70(13) . . ? C8 Ti1 C1 140.20(13) . . ? C2 Ti1 C1 33.81(11) . . ? C5 Ti1 C1 33.99(12) . . ? O1 Ti1 C4 113.70(10) . . ? Cl Ti1 C4 78.62(10) . . ? C3 Ti1 C4 33.89(12) . . ? C6 Ti1 C4 134.71(13) . . ? C7 Ti1 C4 111.36(13) . . ? C8 Ti1 C4 115.76(12) . . ? C2 Ti1 C4 56.76(14) . . ? C5 Ti1 C4 34.19(11) . . ? C1 Ti1 C4 56.31(12) . . ? O1 Ti1 C9 94.71(10) . . ? Cl Ti1 C9 79.01(9) . . ? C3 Ti1 C9 128.47(13) . . ? C6 Ti1 C9 56.86(12) . . ? C7 Ti1 C9 56.81(12) . . ? C8 Ti1 C9 34.20(11) . . ? C2 Ti1 C9 133.05(13) . . ? C5 Ti1 C9 169.91(13) . . ? C1 Ti1 C9 154.89(13) . . ? C4 Ti1 C9 144.48(12) . . ? O1 Ti1 C10 76.81(9) . . ? Cl Ti1 C10 107.90(9) . . ? C3 Ti1 C10 134.00(13) . . ? C6 Ti1 C10 34.20(11) . . ? C7 Ti1 C10 56.59(11) . . ? C8 Ti1 C10 56.19(12) . . ? C2 Ti1 C10 114.59(13) . . ? C5 Ti1 C10 151.44(12) . . ? C1 Ti1 C10 122.48(12) . . ? C4 Ti1 C10 167.77(13) . . ? C9 Ti1 C10 33.45(11) . . ? C12 P1 C20 113.32(13) . . ? C12 P1 C16 112.67(13) . . ? C20 P1 C16 113.16(13) . . ? C12 P1 C11 101.36(12) . . ? C20 P1 C11 106.11(12) . . ? C16 P1 C11 109.24(12) . . ? C11 O1 Ti1 135.77(18) . . ? C2 C1 C5 109.0(3) . . ? C2 C1 Ti1 72.51(19) . . ? C5 C1 Ti1 72.97(19) . . ? C1 C2 C3 107.3(3) . . ? C1 C2 Ti1 73.67(19) . . ? C3 C2 Ti1 71.51(19) . . ? C4 C3 C2 107.9(3) . . ? C4 C3 Ti1 74.88(19) . . ? C2 C3 Ti1 73.50(18) . . ? C3 C4 C5 108.4(3) . . ? C3 C4 Ti1 71.23(19) . . ? C5 C4 Ti1 72.65(18) . . ? C1 C5 C4 107.3(3) . . ? C1 C5 Ti1 73.04(19) . . ? C4 C5 Ti1 73.16(19) . . ? C10 C6 C7 107.3(3) . . ? C10 C6 Ti1 74.97(18) . . ? C7 C6 Ti1 73.02(17) . . ? C8 C7 C6 107.8(3) . . ? C8 C7 Ti1 73.10(18) . . ? C6 C7 Ti1 72.28(17) . . ? O2 C11 O1 128.2(3) . . ? O2 C11 P1 116.3(2) . . ? O1 C11 P1 115.5(2) . . ? C15 C12 C13 109.2(2) . . ? C15 C12 C14 108.1(2) . . ? C13 C12 C14 106.6(2) . . ? C15 C12 P1 112.5(2) . . ? C13 C12 P1 110.20(19) . . ? C14 C12 P1 110.09(19) . . ? C17 C16 C19 109.1(2) . . ? C17 C16 C18 108.4(2) . . ? C19 C16 C18 106.9(2) . . ? C17 C16 P1 111.1(2) . . ? C19 C16 P1 108.95(19) . . ? C18 C16 P1 112.29(19) . . ? C22 C20 C23 106.7(2) . . ? C22 C20 C21 108.6(2) . . ? C23 C20 C21 109.0(2) . . ? C22 C20 P1 108.59(19) . . ? C23 C20 P1 112.8(2) . . ? C21 C20 P1 110.92(19) . . ? C25 C24 C29 112.6(2) . . ? C25 C24 B1 128.4(2) . . ? C29 C24 B1 118.8(2) . . ? F1 C25 C26 114.7(2) . . ? F1 C25 C24 121.0(2) . . ? C26 C25 C24 124.3(2) . . ? F2 C26 C27 119.2(2) . . ? F2 C26 C25 120.5(2) . . ? C27 C26 C25 120.3(2) . . ? F3 C27 C26 120.9(2) . . ? F3 C27 C28 120.7(2) . . ? C26 C27 C28 118.4(2) . . ? F4 C28 C29 121.3(2) . . ? F4 C28 C27 119.4(2) . . ? C29 C28 C27 119.3(2) . . ? F5 C29 C28 116.3(2) . . ? F5 C29 C24 118.8(2) . . ? C28 C29 C24 124.9(2) . . ? C31 C30 C35 112.9(2) . . ? C31 C30 B1 127.4(2) . . ? C35 C30 B1 119.4(2) . . ? F6 C31 C30 121.3(2) . . ? F6 C31 C32 114.4(2) . . ? C30 C31 C32 124.3(2) . . ? F7 C32 C33 120.1(2) . . ? F7 C32 C31 120.1(2) . . ? C33 C32 C31 119.8(3) . . ? F8 C33 C32 120.1(3) . . ? F8 C33 C34 120.9(3) . . ? C32 C33 C34 119.0(3) . . ? F9 C34 C35 120.7(2) . . ? F9 C34 C33 120.0(2) . . ? C35 C34 C33 119.4(2) . . ? F10 C35 C34 116.0(2) . . ? F10 C35 C30 119.3(2) . . ? C34 C35 C30 124.7(3) . . ? C37 C36 C41 112.2(2) . . ? C37 C36 B1 128.3(2) . . ? C41 C36 B1 119.1(2) . . ? F11 C37 C38 114.7(2) . . ? F11 C37 C36 120.6(2) . . ? C38 C37 C36 124.7(3) . . ? F12 C38 C39 119.7(3) . . ? F12 C38 C37 120.4(3) . . ? C39 C38 C37 119.9(2) . . ? F13 C39 C38 120.5(3) . . ? F13 C39 C40 121.1(3) . . ? C38 C39 C40 118.4(3) . . ? F14 C40 C41 121.0(2) . . ? F14 C40 C39 119.5(3) . . ? C41 C40 C39 119.5(3) . . ? C40 C41 F15 116.1(2) . . ? C40 C41 C36 125.3(2) . . ? F15 C41 C36 118.6(2) . . ? C43 C42 C47 112.9(2) . . ? C43 C42 B1 127.0(2) . . ? C47 C42 B1 119.6(2) . . ? F16 C43 C44 114.9(2) . . ? F16 C43 C42 121.3(2) . . ? C44 C43 C42 123.8(2) . . ? F17 C44 C45 119.6(2) . . ? F17 C44 C43 119.8(2) . . ? C45 C44 C43 120.6(2) . . ? F18 C45 C44 121.1(3) . . ? F18 C45 C46 120.4(3) . . ? C44 C45 C46 118.5(2) . . ? F19 C46 C47 120.8(3) . . ? F19 C46 C45 120.0(2) . . ? C47 C46 C45 119.2(3) . . ? F20 C47 C46 115.7(2) . . ? F20 C47 C42 119.2(2) . . ? C46 C47 C42 125.1(2) . . ? C36 B1 C30 113.9(2) . . ? C36 B1 C42 113.8(2) . . ? C30 B1 C42 101.3(2) . . ? C36 B1 C24 102.4(2) . . ? C30 B1 C24 112.7(2) . . ? C42 B1 C24 113.2(2) . . ? C7 C8 C9 108.5(3) . . ? C7 C8 Ti1 72.68(18) . . ? C9 C8 Ti1 74.33(18) . . ? C9 C10 C6 108.9(3) . . ? C9 C10 Ti1 73.22(19) . . ? C6 C10 Ti1 70.83(18) . . ? C10 C9 C8 107.5(3) . . ? C10 C9 Ti1 73.33(19) . . ? C8 C9 Ti1 71.48(19) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.612 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.071 #===end