data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year 2011 _journal_volume 47 _journal_page_first 1833 _publ_contact_author_email dstephan@chem.utoronto.ca _publ_contact_author_name 'Douglas W. Stephan' loop_ _publ_author_name 'Xiaoxi Zhao.' 'Douglas W. Stephan' data_((C6F5)2B)2O _database_code_depnum_ccdc_archive 'CCDC 803523' #TrackingRef '- all-cifs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 B2 F20 O' _chemical_formula_weight 705.86 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' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1407(6) _cell_length_b 11.3624(6) _cell_length_c 11.4867(6) _cell_angle_alpha 107.322(3) _cell_angle_beta 94.603(2) _cell_angle_gamma 117.977(2) _cell_volume 1183.43(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9896 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 35.20 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.981 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 0.228 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6825 _exptl_absorpt_correction_T_max 0.7470 _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 21638 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0194 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5153 _reflns_number_gt 4362 _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^)+(0.0390P)^2^+0.6204P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5153 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0402 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0880 _refine_ls_wR_factor_gt 0.0824 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 O1 O 0.60357(11) 0.56183(11) 0.73785(10) 0.0250(2) Uani 1 1 d . . . B1 B 0.59908(18) 0.65282(18) 0.84037(16) 0.0219(3) Uani 1 1 d . . . B2 B 0.67027(17) 0.51420(17) 0.66075(15) 0.0202(3) Uani 1 1 d . . . C1 C 0.73329(16) 0.76224(15) 0.95464(14) 0.0232(3) Uani 1 1 d . . . C2 C 0.72905(17) 0.84613(16) 1.06985(15) 0.0262(3) Uani 1 1 d . . . C3 C 0.84572(19) 0.94122(16) 1.17139(14) 0.0289(3) Uani 1 1 d . . . C4 C 0.97327(18) 0.95440(16) 1.16143(15) 0.0293(3) Uani 1 1 d . . . C5 C 0.98390(17) 0.87273(17) 1.05116(15) 0.0277(3) Uani 1 1 d . . . C6 C 0.86566(17) 0.78050(16) 0.95135(14) 0.0247(3) Uani 1 1 d . . . C7 C 0.45099(16) 0.63922(16) 0.84007(13) 0.0229(3) Uani 1 1 d . . . C8 C 0.33705(17) 0.51612(17) 0.84061(14) 0.0257(3) Uani 1 1 d . . . C9 C 0.20695(18) 0.50076(19) 0.84202(16) 0.0317(4) Uani 1 1 d . . . C10 C 0.18697(19) 0.6107(2) 0.83989(16) 0.0346(4) Uani 1 1 d . . . C11 C 0.2967(2) 0.7348(2) 0.83768(17) 0.0367(4) Uani 1 1 d . . . C12 C 0.42649(19) 0.74761(18) 0.83884(15) 0.0298(3) Uani 1 1 d . . . C13 C 0.74054(15) 0.59991(15) 0.57568(13) 0.0200(3) Uani 1 1 d . . . C14 C 0.68709(15) 0.67098(15) 0.53048(14) 0.0219(3) Uani 1 1 d . . . C15 C 0.75159(17) 0.75469(16) 0.46320(14) 0.0261(3) Uani 1 1 d . . . C16 C 0.87749(17) 0.77137(17) 0.44078(15) 0.0278(3) Uani 1 1 d . . . C17 C 0.93364(16) 0.70122(17) 0.48202(15) 0.0268(3) Uani 1 1 d . . . C18 C 0.86572(15) 0.61771(16) 0.54809(14) 0.0229(3) Uani 1 1 d . . . C19 C 0.66967(15) 0.37500(15) 0.65811(13) 0.0210(3) Uani 1 1 d . . . C20 C 0.66520(15) 0.27550(16) 0.54953(13) 0.0207(3) Uani 1 1 d . . . C21 C 0.66183(15) 0.15194(16) 0.54634(14) 0.0238(3) Uani 1 1 d . . . C22 C 0.66637(17) 0.12529(17) 0.65579(16) 0.0292(3) Uani 1 1 d . . . C23 C 0.67147(18) 0.22093(18) 0.76621(15) 0.0308(3) Uani 1 1 d . . . C24 C 0.67208(17) 0.34214(17) 0.76558(14) 0.0255(3) Uani 1 1 d . . . F1 F 0.60722(11) 0.83495(11) 1.08731(9) 0.0364(2) Uani 1 1 d . . . F2 F 0.83607(12) 1.01947(11) 1.27875(9) 0.0405(3) Uani 1 1 d . . . F3 F 1.08790(11) 1.04695(11) 1.25817(9) 0.0401(2) Uani 1 1 d . . . F4 F 1.10813(10) 0.88647(12) 1.04208(10) 0.0394(2) Uani 1 1 d . . . F5 F 0.88461(10) 0.70734(11) 0.84550(9) 0.0327(2) Uani 1 1 d . . . F6 F 0.35322(11) 0.40640(10) 0.84352(11) 0.0385(2) Uani 1 1 d . . . F7 F 0.10040(11) 0.38096(13) 0.84680(13) 0.0512(3) Uani 1 1 d . . . F8 F 0.06153(12) 0.59681(15) 0.84215(12) 0.0545(3) Uani 1 1 d . . . F9 F 0.27734(16) 0.84168(15) 0.83599(14) 0.0619(4) Uani 1 1 d . . . F10 F 0.53347(13) 0.87125(12) 0.83974(12) 0.0472(3) Uani 1 1 d . . . F11 F 0.56574(9) 0.66027(10) 0.55204(9) 0.0291(2) Uani 1 1 d . . . F12 F 0.69477(12) 0.81983(11) 0.42101(10) 0.0395(2) Uani 1 1 d . . . F13 F 0.94445(12) 0.85540(12) 0.37935(11) 0.0429(3) Uani 1 1 d . . . F14 F 1.05405(10) 0.71522(12) 0.45768(11) 0.0416(3) Uani 1 1 d . . . F15 F 0.92754(10) 0.55554(11) 0.58930(9) 0.0321(2) Uani 1 1 d . . . F16 F 0.66254(10) 0.29720(10) 0.44088(8) 0.0271(2) Uani 1 1 d . . . F17 F 0.65583(10) 0.05901(10) 0.43891(9) 0.0321(2) Uani 1 1 d . . . F18 F 0.66458(13) 0.00658(11) 0.65432(11) 0.0449(3) Uani 1 1 d . . . F19 F 0.67596(14) 0.19525(13) 0.87242(10) 0.0481(3) Uani 1 1 d . . . F20 F 0.67818(12) 0.43266(11) 0.87608(9) 0.0374(2) 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 O1 0.0268(5) 0.0253(5) 0.0219(5) 0.0048(4) 0.0092(4) 0.0147(5) B1 0.0302(9) 0.0213(8) 0.0212(8) 0.0102(7) 0.0111(7) 0.0166(7) B2 0.0178(7) 0.0219(8) 0.0163(7) 0.0024(6) 0.0025(6) 0.0101(6) C1 0.0312(8) 0.0206(7) 0.0203(7) 0.0079(6) 0.0078(6) 0.0150(6) C2 0.0357(8) 0.0249(7) 0.0235(8) 0.0098(6) 0.0108(7) 0.0188(7) C3 0.0461(10) 0.0214(7) 0.0185(7) 0.0053(6) 0.0084(7) 0.0183(7) C4 0.0370(9) 0.0201(7) 0.0216(8) 0.0073(6) 0.0011(7) 0.0094(7) C5 0.0290(8) 0.0259(8) 0.0275(8) 0.0118(7) 0.0068(7) 0.0127(7) C6 0.0332(8) 0.0232(7) 0.0196(7) 0.0076(6) 0.0080(6) 0.0162(7) C7 0.0320(8) 0.0270(7) 0.0161(7) 0.0078(6) 0.0092(6) 0.0198(7) C8 0.0320(8) 0.0254(7) 0.0225(7) 0.0074(6) 0.0066(6) 0.0180(7) C9 0.0288(8) 0.0348(9) 0.0260(8) 0.0075(7) 0.0066(7) 0.0149(7) C10 0.0344(9) 0.0540(11) 0.0245(8) 0.0111(8) 0.0075(7) 0.0318(9) C11 0.0567(11) 0.0478(10) 0.0307(9) 0.0176(8) 0.0149(8) 0.0437(10) C12 0.0437(9) 0.0314(8) 0.0270(8) 0.0154(7) 0.0157(7) 0.0253(8) C13 0.0199(7) 0.0191(7) 0.0165(7) 0.0025(5) 0.0032(5) 0.0096(6) C14 0.0197(7) 0.0210(7) 0.0203(7) 0.0014(6) 0.0025(6) 0.0112(6) C15 0.0327(8) 0.0237(7) 0.0229(8) 0.0071(6) 0.0037(6) 0.0171(7) C16 0.0327(8) 0.0241(7) 0.0230(8) 0.0099(6) 0.0101(7) 0.0112(7) C17 0.0213(7) 0.0292(8) 0.0263(8) 0.0073(7) 0.0090(6) 0.0119(7) C18 0.0224(7) 0.0251(7) 0.0213(7) 0.0063(6) 0.0039(6) 0.0141(6) C19 0.0204(7) 0.0227(7) 0.0195(7) 0.0066(6) 0.0056(6) 0.0115(6) C20 0.0186(7) 0.0246(7) 0.0189(7) 0.0079(6) 0.0055(6) 0.0115(6) C21 0.0221(7) 0.0213(7) 0.0243(7) 0.0040(6) 0.0072(6) 0.0112(6) C22 0.0312(8) 0.0247(8) 0.0360(9) 0.0142(7) 0.0104(7) 0.0160(7) C23 0.0378(9) 0.0345(9) 0.0262(8) 0.0170(7) 0.0103(7) 0.0198(8) C24 0.0298(8) 0.0265(7) 0.0187(7) 0.0057(6) 0.0076(6) 0.0150(7) F1 0.0424(6) 0.0426(6) 0.0269(5) 0.0049(4) 0.0135(4) 0.0282(5) F2 0.0597(7) 0.0366(5) 0.0211(5) 0.0003(4) 0.0081(5) 0.0285(5) F3 0.0417(6) 0.0307(5) 0.0259(5) 0.0026(4) -0.0041(4) 0.0091(5) F4 0.0288(5) 0.0452(6) 0.0351(6) 0.0096(5) 0.0044(4) 0.0165(5) F5 0.0299(5) 0.0412(5) 0.0233(5) 0.0020(4) 0.0067(4) 0.0218(4) F6 0.0398(6) 0.0266(5) 0.0572(7) 0.0200(5) 0.0164(5) 0.0202(4) F7 0.0306(6) 0.0443(6) 0.0680(8) 0.0197(6) 0.0160(6) 0.0119(5) F8 0.0424(6) 0.0830(9) 0.0537(7) 0.0211(7) 0.0139(6) 0.0470(7) F9 0.0865(9) 0.0704(8) 0.0812(9) 0.0438(8) 0.0356(8) 0.0686(8) F10 0.0587(7) 0.0375(6) 0.0658(8) 0.0325(6) 0.0312(6) 0.0303(6) F11 0.0251(5) 0.0324(5) 0.0361(5) 0.0119(4) 0.0095(4) 0.0199(4) F12 0.0527(6) 0.0419(6) 0.0440(6) 0.0248(5) 0.0151(5) 0.0342(5) F13 0.0522(7) 0.0437(6) 0.0459(6) 0.0303(5) 0.0262(5) 0.0246(5) F14 0.0302(5) 0.0535(6) 0.0549(7) 0.0296(6) 0.0261(5) 0.0244(5) F15 0.0280(5) 0.0442(6) 0.0410(6) 0.0236(5) 0.0139(4) 0.0261(5) F16 0.0376(5) 0.0315(5) 0.0176(4) 0.0086(4) 0.0099(4) 0.0218(4) F17 0.0395(5) 0.0254(5) 0.0304(5) 0.0039(4) 0.0125(4) 0.0196(4) F18 0.0685(8) 0.0351(6) 0.0487(7) 0.0229(5) 0.0216(6) 0.0348(6) F19 0.0803(8) 0.0519(7) 0.0322(6) 0.0271(5) 0.0204(6) 0.0417(7) F20 0.0609(7) 0.0392(6) 0.0179(5) 0.0092(4) 0.0138(5) 0.0307(5) _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 O1 B1 1.3383(19) . ? O1 B2 1.3517(18) . ? B1 C1 1.573(2) . ? B1 C7 1.583(2) . ? B2 C19 1.570(2) . ? B2 C13 1.578(2) . ? C1 C6 1.395(2) . ? C1 C2 1.401(2) . ? C2 F1 1.3399(18) . ? C2 C3 1.381(2) . ? C3 F2 1.3345(17) . ? C3 C4 1.375(2) . ? C4 F3 1.3371(19) . ? C4 C5 1.381(2) . ? C5 F4 1.3346(19) . ? C5 C6 1.376(2) . ? C6 F5 1.3483(17) . ? C7 C8 1.381(2) . ? C7 C12 1.384(2) . ? C8 F6 1.3499(17) . ? C8 C9 1.378(2) . ? C9 F7 1.343(2) . ? C9 C10 1.374(2) . ? C10 F8 1.3342(19) . ? C10 C11 1.376(3) . ? C11 F9 1.3347(19) . ? C11 C12 1.382(2) . ? C12 F10 1.346(2) . ? C13 C14 1.388(2) . ? C13 C18 1.3896(19) . ? C14 F11 1.3496(16) . ? C14 C15 1.380(2) . ? C15 F12 1.3369(17) . ? C15 C16 1.381(2) . ? C16 F13 1.3354(17) . ? C16 C17 1.377(2) . ? C17 F14 1.3376(17) . ? C17 C18 1.377(2) . ? C18 F15 1.3418(17) . ? C19 C20 1.391(2) . ? C19 C24 1.394(2) . ? C20 F16 1.3429(16) . ? C20 C21 1.376(2) . ? C21 F17 1.3366(17) . ? C21 C22 1.380(2) . ? C22 F18 1.3346(18) . ? C22 C23 1.379(2) . ? C23 F19 1.3387(18) . ? C23 C24 1.376(2) . ? C24 F20 1.3478(17) . ? 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 B1 O1 B2 153.88(14) . . ? O1 B1 C1 121.01(13) . . ? O1 B1 C7 115.93(14) . . ? C1 B1 C7 123.03(13) . . ? O1 B2 C19 118.33(13) . . ? O1 B2 C13 117.73(13) . . ? C19 B2 C13 123.91(12) . . ? C6 C1 C2 114.31(14) . . ? C6 C1 B1 122.84(13) . . ? C2 C1 B1 122.82(14) . . ? F1 C2 C3 116.19(13) . . ? F1 C2 C1 120.42(14) . . ? C3 C2 C1 123.38(15) . . ? F2 C3 C4 119.80(15) . . ? F2 C3 C2 120.95(15) . . ? C4 C3 C2 119.25(14) . . ? F3 C4 C3 120.22(14) . . ? F3 C4 C5 119.59(15) . . ? C3 C4 C5 120.19(15) . . ? F4 C5 C6 121.26(14) . . ? F4 C5 C4 119.83(15) . . ? C6 C5 C4 118.90(15) . . ? F5 C6 C5 115.71(14) . . ? F5 C6 C1 120.32(13) . . ? C5 C6 C1 123.96(14) . . ? C8 C7 C12 115.77(14) . . ? C8 C7 B1 121.27(13) . . ? C12 C7 B1 122.96(14) . . ? F6 C8 C9 117.69(14) . . ? F6 C8 C7 119.23(14) . . ? C9 C8 C7 123.05(14) . . ? F7 C9 C10 119.74(15) . . ? F7 C9 C8 121.01(15) . . ? C10 C9 C8 119.25(16) . . ? F8 C10 C9 119.51(17) . . ? F8 C10 C11 120.58(16) . . ? C9 C10 C11 119.90(15) . . ? F9 C11 C10 119.86(16) . . ? F9 C11 C12 120.87(18) . . ? C10 C11 C12 119.27(15) . . ? F10 C12 C11 118.40(14) . . ? F10 C12 C7 118.86(15) . . ? C11 C12 C7 122.73(16) . . ? C14 C13 C18 115.28(13) . . ? C14 C13 B2 122.42(13) . . ? C18 C13 B2 122.16(13) . . ? F11 C14 C15 116.49(13) . . ? F11 C14 C13 119.88(13) . . ? C15 C14 C13 123.63(13) . . ? F12 C15 C14 121.10(14) . . ? F12 C15 C16 120.17(14) . . ? C14 C15 C16 118.73(14) . . ? F13 C16 C17 120.20(14) . . ? F13 C16 C15 120.00(14) . . ? C17 C16 C15 119.79(14) . . ? F14 C17 C18 120.62(14) . . ? F14 C17 C16 119.57(14) . . ? C18 C17 C16 119.81(14) . . ? F15 C18 C17 117.19(13) . . ? F15 C18 C13 120.05(13) . . ? C17 C18 C13 122.73(14) . . ? C20 C19 C24 115.32(13) . . ? C20 C19 B2 122.96(13) . . ? C24 C19 B2 121.72(13) . . ? F16 C20 C21 116.95(13) . . ? F16 C20 C19 119.97(13) . . ? C21 C20 C19 123.09(13) . . ? F17 C21 C20 120.59(13) . . ? F17 C21 C22 120.05(14) . . ? C20 C21 C22 119.35(14) . . ? F18 C22 C23 120.17(14) . . ? F18 C22 C21 119.98(14) . . ? C23 C22 C21 119.84(14) . . ? F19 C23 C24 120.80(15) . . ? F19 C23 C22 119.89(15) . . ? C24 C23 C22 119.31(14) . . ? F20 C24 C23 116.98(13) . . ? F20 C24 C19 119.93(13) . . ? C23 C24 C19 123.07(14) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.330 _refine_diff_density_min -0.303 _refine_diff_density_rms 0.044 #===end data_((C6F5)2B)2O(O2CPBu3) _database_code_depnum_ccdc_archive 'CCDC 803524' #TrackingRef '- all-cifs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H27 B2 F20 O3 P' _chemical_formula_weight 952.18 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 14.5904(11) _cell_length_b 17.0600(15) _cell_length_c 16.9806(13) _cell_angle_alpha 90.00 _cell_angle_beta 111.554(4) _cell_angle_gamma 90.00 _cell_volume 3931.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5922 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 22.09 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 0.203 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6819 _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 34694 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 27.54 _reflns_number_total 9004 _reflns_number_gt 5150 _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^)+(0.0668P)^2^+0.8943P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9004 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1043 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1506 _refine_ls_wR_factor_gt 0.1260 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 P1 P -0.06366(5) 0.26749(4) 0.52276(4) 0.03706(17) Uani 1 1 d . . . F1 F -0.10907(13) 0.20950(9) 0.12103(10) 0.0637(5) Uani 1 1 d . . . F2 F -0.22206(13) 0.29615(11) -0.00429(10) 0.0715(5) Uani 1 1 d . . . F3 F -0.25833(13) 0.44851(11) 0.02030(11) 0.0755(5) Uani 1 1 d . . . F4 F -0.16586(15) 0.51445(10) 0.17549(12) 0.0784(6) Uani 1 1 d . . . F5 F -0.04507(14) 0.42984(9) 0.30279(10) 0.0634(5) Uani 1 1 d . . . F6 F 0.16669(12) 0.15701(10) 0.29807(12) 0.0688(5) Uani 1 1 d . . . F7 F 0.14684(14) 0.00499(12) 0.26299(16) 0.0924(7) Uani 1 1 d . . . F8 F -0.02660(15) -0.06868(10) 0.23228(13) 0.0828(6) Uani 1 1 d . . . F9 F -0.18263(14) 0.01296(11) 0.24016(13) 0.0810(6) Uani 1 1 d . . . F10 F -0.16671(11) 0.16654(10) 0.27244(11) 0.0620(4) Uani 1 1 d . . . F11 F 0.09937(16) 0.25004(12) 0.14595(11) 0.0790(6) Uani 1 1 d . . . F12 F 0.06494(16) 0.31358(16) -0.00621(12) 0.1011(8) Uani 1 1 d . . . F13 F 0.08489(15) 0.46905(17) -0.02085(13) 0.1084(9) Uani 1 1 d . . . F14 F 0.13238(17) 0.56238(14) 0.11708(17) 0.1120(8) Uani 1 1 d . . . F15 F 0.16197(15) 0.49882(11) 0.27090(14) 0.0831(6) Uani 1 1 d . . . F16 F 0.33919(15) 0.28434(14) 0.28931(13) 0.0885(6) Uani 1 1 d . . . F17 F 0.52290(15) 0.31856(18) 0.39362(18) 0.1319(11) Uani 1 1 d . . . F18 F 0.55137(17) 0.40725(19) 0.53549(18) 0.1485(13) Uani 1 1 d . . . F19 F 0.3942(2) 0.46222(15) 0.56623(14) 0.1276(10) Uani 1 1 d . . . F20 F 0.21166(16) 0.42724(12) 0.46140(12) 0.0846(6) Uani 1 1 d . . . O1 O 0.10207(12) 0.29551(10) 0.33400(10) 0.0421(4) Uani 1 1 d . . . O2 O -0.03787(12) 0.28044(10) 0.37377(10) 0.0383(4) Uani 1 1 d . . . O3 O 0.06428(15) 0.19795(14) 0.46840(12) 0.0648(6) Uani 1 1 d . . . C1 C -0.07291(17) 0.31414(15) 0.22096(15) 0.0379(6) Uani 1 1 d . . . C2 C -0.12012(19) 0.28515(15) 0.13996(16) 0.0429(6) Uani 1 1 d . . . C3 C -0.18094(19) 0.32894(17) 0.07242(16) 0.0476(7) Uani 1 1 d . . . C4 C -0.19792(19) 0.40571(17) 0.08478(18) 0.0504(7) Uani 1 1 d . . . C5 C -0.1519(2) 0.43791(16) 0.16325(18) 0.0506(7) Uani 1 1 d . . . C6 C -0.09127(19) 0.39272(15) 0.22815(16) 0.0427(6) Uani 1 1 d . . . C7 C 0.00076(17) 0.17031(14) 0.28700(14) 0.0370(5) Uani 1 1 d . . . C8 C 0.07781(19) 0.12491(16) 0.28408(16) 0.0460(6) Uani 1 1 d . . . C9 C 0.0701(2) 0.04576(18) 0.26679(19) 0.0556(7) Uani 1 1 d . . . C10 C -0.0173(2) 0.00806(16) 0.25221(18) 0.0552(7) Uani 1 1 d . . . C11 C -0.0960(2) 0.04922(17) 0.25583(17) 0.0509(7) Uani 1 1 d . . . C12 C -0.08500(18) 0.12778(16) 0.27241(16) 0.0424(6) Uani 1 1 d . . . C13 C 0.13308(18) 0.37274(17) 0.21462(17) 0.0475(7) Uani 1 1 d . . . C14 C 0.1078(2) 0.3271(2) 0.14141(17) 0.0547(8) Uani 1 1 d . . . C15 C 0.0899(2) 0.3596(2) 0.0629(2) 0.0661(9) Uani 1 1 d . . . C16 C 0.1000(2) 0.4364(3) 0.0557(2) 0.0707(10) Uani 1 1 d . . . C17 C 0.1243(2) 0.4859(2) 0.1239(3) 0.0714(10) Uani 1 1 d . . . C18 C 0.1399(2) 0.4509(2) 0.2033(2) 0.0596(8) Uani 1 1 d . . . C19 C 0.26910(19) 0.35446(16) 0.37179(16) 0.0452(6) Uani 1 1 d . . . C20 C 0.3515(2) 0.3288(2) 0.35808(19) 0.0582(8) Uani 1 1 d . . . C21 C 0.4463(2) 0.3455(3) 0.4121(3) 0.0817(12) Uani 1 1 d . . . C22 C 0.4594(3) 0.3903(3) 0.4820(3) 0.0891(13) Uani 1 1 d . . . C23 C 0.3813(3) 0.4175(2) 0.4977(2) 0.0793(11) Uani 1 1 d . . . C24 C 0.2875(2) 0.39884(18) 0.44341(18) 0.0561(8) Uani 1 1 d . . . C25 C -0.1572(2) 0.34830(17) 0.48078(18) 0.0516(7) Uani 1 1 d . . . C26 C -0.1028(3) 0.42597(18) 0.4804(2) 0.0719(9) Uani 1 1 d . . . H26A H -0.1510 0.4669 0.4528 0.108 Uiso 1 1 calc R . . H26B H -0.0585 0.4186 0.4494 0.108 Uiso 1 1 calc R . . H26C H -0.0643 0.4416 0.5388 0.108 Uiso 1 1 calc R . . C27 C -0.2273(2) 0.3335(2) 0.38861(19) 0.0655(9) Uani 1 1 d . . . H27A H -0.2710 0.3787 0.3681 0.098 Uiso 1 1 calc R . . H27B H -0.2669 0.2865 0.3865 0.098 Uiso 1 1 calc R . . H27C H -0.1885 0.3258 0.3528 0.098 Uiso 1 1 calc R . . C28 C -0.2204(3) 0.3587(2) 0.5359(2) 0.0711(9) Uani 1 1 d . . . H28A H -0.2634 0.4045 0.5161 0.107 Uiso 1 1 calc R . . H28B H -0.1771 0.3665 0.5951 0.107 Uiso 1 1 calc R . . H28C H -0.2608 0.3118 0.5314 0.107 Uiso 1 1 calc R . . C29 C -0.1210(2) 0.17229(16) 0.53676(17) 0.0493(7) Uani 1 1 d . . . C30 C -0.2186(2) 0.1594(2) 0.46139(19) 0.0651(9) Uani 1 1 d . . . H30A H -0.2457 0.1080 0.4666 0.098 Uiso 1 1 calc R . . H30B H -0.2064 0.1617 0.4084 0.098 Uiso 1 1 calc R . . H30C H -0.2657 0.2004 0.4613 0.098 Uiso 1 1 calc R . . C31 C -0.1435(2) 0.17455(19) 0.61855(18) 0.0620(8) Uani 1 1 d . . . H31A H -0.1741 0.1250 0.6248 0.093 Uiso 1 1 calc R . . H31B H -0.1886 0.2180 0.6155 0.093 Uiso 1 1 calc R . . H31C H -0.0820 0.1821 0.6673 0.093 Uiso 1 1 calc R . . C32 C -0.0551(3) 0.10192(18) 0.5393(2) 0.0691(9) Uani 1 1 d . . . H32A H -0.0867 0.0539 0.5484 0.104 Uiso 1 1 calc R . . H32B H 0.0087 0.1086 0.5856 0.104 Uiso 1 1 calc R . . H32C H -0.0451 0.0982 0.4854 0.104 Uiso 1 1 calc R . . C33 C 0.0448(2) 0.29772(18) 0.62008(17) 0.0559(8) Uani 1 1 d . . . C34 C 0.0118(3) 0.3410(2) 0.6846(2) 0.0841(11) Uani 1 1 d . . . H34A H 0.0695 0.3530 0.7353 0.126 Uiso 1 1 calc R . . H34B H -0.0338 0.3078 0.7001 0.126 Uiso 1 1 calc R . . H34C H -0.0215 0.3899 0.6595 0.126 Uiso 1 1 calc R . . C35 C 0.1066(2) 0.2259(2) 0.66319(19) 0.0731(10) Uani 1 1 d . . . H35A H 0.1667 0.2433 0.7090 0.110 Uiso 1 1 calc R . . H35B H 0.1244 0.1961 0.6215 0.110 Uiso 1 1 calc R . . H35C H 0.0681 0.1924 0.6865 0.110 Uiso 1 1 calc R . . C36 C 0.1130(2) 0.3512(2) 0.5914(2) 0.0841(11) Uani 1 1 d . . . H36A H 0.1660 0.3719 0.6414 0.126 Uiso 1 1 calc R . . H36B H 0.0745 0.3948 0.5577 0.126 Uiso 1 1 calc R . . H36C H 0.1414 0.3207 0.5571 0.126 Uiso 1 1 calc R . . C37 C -0.00187(18) 0.24404(16) 0.44562(15) 0.0409(6) Uani 1 1 d . . . B1 B 0.0023(2) 0.26462(17) 0.30246(18) 0.0387(6) Uani 1 1 d . . . B2 B 0.1606(2) 0.33658(17) 0.30740(18) 0.0402(7) 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 P1 0.0356(3) 0.0402(4) 0.0354(3) -0.0006(3) 0.0130(3) -0.0056(3) F1 0.0857(12) 0.0489(10) 0.0453(9) -0.0060(7) 0.0111(8) 0.0144(9) F2 0.0733(12) 0.0793(13) 0.0430(9) -0.0006(9) -0.0010(8) 0.0006(10) F3 0.0677(11) 0.0694(12) 0.0710(11) 0.0287(10) 0.0040(9) 0.0162(9) F4 0.1082(15) 0.0416(10) 0.0816(12) 0.0142(9) 0.0307(11) 0.0195(10) F5 0.0928(12) 0.0411(9) 0.0495(9) -0.0030(7) 0.0182(9) -0.0016(9) F6 0.0423(9) 0.0616(11) 0.1067(14) 0.0025(10) 0.0324(9) 0.0061(8) F7 0.0724(13) 0.0632(12) 0.1451(19) 0.0005(12) 0.0443(13) 0.0317(10) F8 0.1057(15) 0.0367(10) 0.0977(14) -0.0030(9) 0.0277(12) 0.0056(10) F9 0.0702(12) 0.0644(12) 0.1094(15) -0.0182(11) 0.0342(11) -0.0291(10) F10 0.0396(8) 0.0626(11) 0.0861(12) -0.0157(9) 0.0257(8) -0.0025(8) F11 0.1061(15) 0.0706(13) 0.0635(11) -0.0084(10) 0.0350(11) -0.0059(11) F12 0.1013(16) 0.153(2) 0.0517(11) -0.0076(12) 0.0313(11) -0.0012(15) F13 0.0732(13) 0.174(2) 0.0784(13) 0.0687(15) 0.0282(11) 0.0118(14) F14 0.0949(16) 0.0792(16) 0.147(2) 0.0550(15) 0.0267(15) -0.0048(13) F15 0.0867(14) 0.0546(11) 0.0987(15) 0.0018(11) 0.0231(11) -0.0061(10) F16 0.0850(13) 0.1229(18) 0.0744(13) 0.0092(12) 0.0494(11) 0.0298(13) F17 0.0523(12) 0.184(3) 0.170(2) 0.088(2) 0.0524(14) 0.0307(15) F18 0.0754(15) 0.166(3) 0.137(2) 0.0648(19) -0.0407(14) -0.0554(16) F19 0.180(3) 0.1013(18) 0.0636(13) -0.0144(13) 0.0007(14) -0.0612(18) F20 0.1096(16) 0.0769(14) 0.0814(13) -0.0266(11) 0.0516(12) -0.0117(12) O1 0.0408(9) 0.0454(10) 0.0406(9) 0.0026(8) 0.0156(8) -0.0045(8) O2 0.0415(9) 0.0393(10) 0.0356(9) 0.0042(7) 0.0158(7) 0.0036(8) O3 0.0563(12) 0.0868(16) 0.0553(12) 0.0238(11) 0.0253(10) 0.0324(12) C1 0.0370(13) 0.0399(14) 0.0390(13) 0.0038(11) 0.0164(11) 0.0007(11) C2 0.0460(15) 0.0399(15) 0.0431(14) 0.0011(12) 0.0168(12) 0.0035(12) C3 0.0433(15) 0.0566(18) 0.0396(14) 0.0057(13) 0.0112(12) -0.0017(13) C4 0.0398(15) 0.0514(17) 0.0551(17) 0.0186(14) 0.0116(13) 0.0070(13) C5 0.0579(17) 0.0371(15) 0.0604(18) 0.0097(13) 0.0260(15) 0.0072(13) C6 0.0501(15) 0.0395(15) 0.0398(14) -0.0005(12) 0.0181(12) -0.0027(12) C7 0.0359(13) 0.0388(14) 0.0356(12) 0.0047(11) 0.0125(10) 0.0038(11) C8 0.0380(14) 0.0478(17) 0.0519(15) 0.0084(13) 0.0160(12) 0.0061(12) C9 0.0539(18) 0.0479(18) 0.0631(18) 0.0078(14) 0.0190(14) 0.0214(15) C10 0.071(2) 0.0341(15) 0.0555(17) 0.0031(13) 0.0171(15) 0.0078(15) C11 0.0535(17) 0.0458(17) 0.0524(16) 0.0020(13) 0.0181(13) -0.0075(14) C12 0.0372(14) 0.0463(16) 0.0444(14) 0.0021(12) 0.0157(11) 0.0033(12) C13 0.0364(14) 0.0551(18) 0.0524(16) 0.0116(14) 0.0179(12) -0.0013(13) C14 0.0431(15) 0.080(2) 0.0434(16) 0.0095(15) 0.0187(12) -0.0030(15) C15 0.0502(18) 0.097(3) 0.0532(19) 0.0025(19) 0.0219(14) -0.0020(18) C16 0.0384(16) 0.104(3) 0.064(2) 0.033(2) 0.0122(15) 0.0039(18) C17 0.0402(16) 0.073(2) 0.096(3) 0.038(2) 0.0185(17) -0.0028(16) C18 0.0445(16) 0.064(2) 0.0636(19) 0.0084(17) 0.0119(14) -0.0056(15) C19 0.0445(15) 0.0494(16) 0.0429(14) 0.0081(13) 0.0176(12) -0.0052(13) C20 0.0486(17) 0.077(2) 0.0536(17) 0.0212(16) 0.0240(14) 0.0054(15) C21 0.0413(18) 0.106(3) 0.097(3) 0.055(3) 0.0243(19) 0.0064(19) C22 0.061(2) 0.098(3) 0.081(3) 0.036(2) -0.006(2) -0.026(2) C23 0.104(3) 0.068(2) 0.0468(19) 0.0066(17) 0.0045(19) -0.035(2) C24 0.0631(19) 0.0533(18) 0.0524(17) 0.0008(14) 0.0218(15) -0.0144(15) C25 0.0499(16) 0.0475(17) 0.0610(17) 0.0028(14) 0.0248(14) 0.0074(13) C26 0.086(2) 0.0450(18) 0.093(2) 0.0058(17) 0.042(2) 0.0043(17) C27 0.0487(17) 0.081(2) 0.0619(19) 0.0145(17) 0.0139(14) 0.0171(16) C28 0.072(2) 0.070(2) 0.086(2) -0.0018(18) 0.0469(19) 0.0147(18) C29 0.0543(16) 0.0454(16) 0.0513(15) -0.0002(13) 0.0231(13) -0.0124(13) C30 0.064(2) 0.063(2) 0.0653(19) -0.0118(16) 0.0194(16) -0.0251(16) C31 0.0662(19) 0.068(2) 0.0612(18) 0.0090(16) 0.0341(16) -0.0145(16) C32 0.083(2) 0.0428(18) 0.086(2) 0.0036(16) 0.0363(19) -0.0025(16) C33 0.0529(17) 0.0632(19) 0.0442(15) -0.0035(14) 0.0091(13) -0.0199(15) C34 0.097(3) 0.093(3) 0.0536(19) -0.0287(19) 0.0177(18) -0.023(2) C35 0.0527(18) 0.099(3) 0.0512(17) 0.0161(18) -0.0004(14) -0.0103(18) C36 0.058(2) 0.090(3) 0.087(2) 0.008(2) 0.0061(18) -0.0378(19) C37 0.0357(13) 0.0489(16) 0.0382(13) 0.0069(12) 0.0138(11) -0.0003(12) B1 0.0362(15) 0.0399(16) 0.0411(15) 0.0017(13) 0.0154(12) -0.0020(13) B2 0.0433(16) 0.0376(16) 0.0430(16) -0.0026(13) 0.0197(13) 0.0007(13) _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 P1 C29 1.881(3) . ? P1 C37 1.886(3) . ? P1 C25 1.886(3) . ? P1 C33 1.892(3) . ? F1 C2 1.354(3) . ? F2 C3 1.340(3) . ? F3 C4 1.342(3) . ? F4 C5 1.349(3) . ? F5 C6 1.354(3) . ? F6 C8 1.346(3) . ? F7 C9 1.340(3) . ? F8 C10 1.347(3) . ? F9 C11 1.343(3) . ? F10 C12 1.363(3) . ? F11 C14 1.325(4) . ? F12 C15 1.346(4) . ? F13 C16 1.355(4) . ? F14 C17 1.319(4) . ? F15 C18 1.348(4) . ? F16 C20 1.348(4) . ? F17 C21 1.348(4) . ? F18 C22 1.346(4) . ? F19 C23 1.346(4) . ? F20 C24 1.342(4) . ? O1 B2 1.307(3) . ? O1 B1 1.453(3) . ? O2 C37 1.296(3) . ? O2 B1 1.550(3) . ? O3 C37 1.194(3) . ? C1 C6 1.381(4) . ? C1 C2 1.384(3) . ? C1 B1 1.648(4) . ? C2 C3 1.383(4) . ? C3 C4 1.363(4) . ? C4 C5 1.368(4) . ? C5 C6 1.370(4) . ? C7 C8 1.381(3) . ? C7 C12 1.388(3) . ? C7 B1 1.629(4) . ? C8 C9 1.378(4) . ? C9 C10 1.367(4) . ? C10 C11 1.366(4) . ? C11 C12 1.367(4) . ? C13 C18 1.356(4) . ? C13 C14 1.397(4) . ? C13 B2 1.600(4) . ? C14 C15 1.379(4) . ? C15 C16 1.329(5) . ? C16 C17 1.370(5) . ? C17 C18 1.415(5) . ? C19 C24 1.373(4) . ? C19 C20 1.377(4) . ? C19 B2 1.588(4) . ? C20 C21 1.380(5) . ? C21 C22 1.365(6) . ? C22 C23 1.345(6) . ? C23 C24 1.378(5) . ? C25 C27 1.544(4) . ? C25 C28 1.546(4) . ? C25 C26 1.546(4) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C32 1.529(4) . ? C29 C31 1.541(4) . ? C29 C30 1.541(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.538(5) . ? C33 C35 1.539(4) . ? C33 C36 1.555(4) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? 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 C29 P1 C37 104.64(12) . . ? C29 P1 C25 112.65(13) . . ? C37 P1 C25 110.90(12) . . ? C29 P1 C33 113.13(13) . . ? C37 P1 C33 101.82(12) . . ? C25 P1 C33 112.81(14) . . ? B2 O1 B1 139.5(2) . . ? C37 O2 B1 120.88(19) . . ? C6 C1 C2 113.1(2) . . ? C6 C1 B1 120.9(2) . . ? C2 C1 B1 125.9(2) . . ? F1 C2 C3 114.5(2) . . ? F1 C2 C1 121.2(2) . . ? C3 C2 C1 124.4(2) . . ? F2 C3 C4 120.6(2) . . ? F2 C3 C2 120.2(3) . . ? C4 C3 C2 119.3(2) . . ? F3 C4 C3 120.0(3) . . ? F3 C4 C5 121.1(3) . . ? C3 C4 C5 118.9(2) . . ? F4 C5 C4 119.4(2) . . ? F4 C5 C6 120.7(3) . . ? C4 C5 C6 119.9(3) . . ? F5 C6 C5 116.3(2) . . ? F5 C6 C1 119.4(2) . . ? C5 C6 C1 124.3(2) . . ? C8 C7 C12 113.1(2) . . ? C8 C7 B1 126.6(2) . . ? C12 C7 B1 120.2(2) . . ? F6 C8 C9 115.8(2) . . ? F6 C8 C7 120.6(2) . . ? C9 C8 C7 123.6(3) . . ? F7 C9 C10 119.2(3) . . ? F7 C9 C8 121.0(3) . . ? C10 C9 C8 119.8(3) . . ? F8 C10 C11 120.2(3) . . ? F8 C10 C9 120.3(3) . . ? C11 C10 C9 119.6(3) . . ? F9 C11 C10 120.0(3) . . ? F9 C11 C12 121.5(3) . . ? C10 C11 C12 118.4(3) . . ? F10 C12 C11 116.1(2) . . ? F10 C12 C7 118.5(2) . . ? C11 C12 C7 125.4(2) . . ? C18 C13 C14 115.6(3) . . ? C18 C13 B2 120.9(3) . . ? C14 C13 B2 123.4(3) . . ? F11 C14 C15 117.9(3) . . ? F11 C14 C13 120.1(2) . . ? C15 C14 C13 122.0(3) . . ? C16 C15 F12 119.9(3) . . ? C16 C15 C14 119.9(3) . . ? F12 C15 C14 120.1(4) . . ? C15 C16 F13 120.6(4) . . ? C15 C16 C17 122.2(3) . . ? F13 C16 C17 117.3(4) . . ? F14 C17 C16 122.6(3) . . ? F14 C17 C18 120.9(4) . . ? C16 C17 C18 116.5(3) . . ? F15 C18 C13 118.9(3) . . ? F15 C18 C17 117.4(3) . . ? C13 C18 C17 123.7(3) . . ? C24 C19 C20 115.2(3) . . ? C24 C19 B2 122.5(2) . . ? C20 C19 B2 122.3(3) . . ? F16 C20 C19 118.6(3) . . ? F16 C20 C21 118.3(3) . . ? C19 C20 C21 123.1(3) . . ? F17 C21 C22 122.0(4) . . ? F17 C21 C20 119.3(4) . . ? C22 C21 C20 118.7(4) . . ? C23 C22 F18 120.0(5) . . ? C23 C22 C21 120.5(3) . . ? F18 C22 C21 119.6(5) . . ? C22 C23 F19 120.5(4) . . ? C22 C23 C24 119.6(4) . . ? F19 C23 C24 119.9(4) . . ? F20 C24 C19 119.5(3) . . ? F20 C24 C23 117.6(3) . . ? C19 C24 C23 122.9(3) . . ? C27 C25 C28 108.2(2) . . ? C27 C25 C26 106.6(3) . . ? C28 C25 C26 109.0(3) . . ? C27 C25 P1 112.4(2) . . ? C28 C25 P1 111.4(2) . . ? C26 C25 P1 109.0(2) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C32 C29 C31 109.6(2) . . ? C32 C29 C30 106.9(2) . . ? C31 C29 C30 108.3(2) . . ? C32 C29 P1 112.2(2) . . ? C31 C29 P1 110.13(19) . . ? C30 C29 P1 109.6(2) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C35 109.0(3) . . ? C34 C33 C36 110.2(3) . . ? C35 C33 C36 106.6(3) . . ? C34 C33 P1 111.9(2) . . ? C35 C33 P1 110.8(2) . . ? C36 C33 P1 108.2(2) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O3 C37 O2 128.4(2) . . ? O3 C37 P1 116.78(18) . . ? O2 C37 P1 114.87(18) . . ? O1 B1 O2 105.31(19) . . ? O1 B1 C7 111.7(2) . . ? O2 B1 C7 108.1(2) . . ? O1 B1 C1 113.0(2) . . ? O2 B1 C1 103.93(19) . . ? C7 B1 C1 113.9(2) . . ? O1 B2 C19 118.5(2) . . ? O1 B2 C13 126.0(2) . . ? C19 B2 C13 115.5(2) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.511 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.050 #===end data_((Cl2B)2CCMe2(O2CPBu3) _database_code_depnum_ccdc_archive 'CCDC 803525' #TrackingRef '- all-cifs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H33 B2 Cl4 O2 P' _chemical_formula_weight 463.82 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' P P 0.1023 0.0942 '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 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 11.9094(6) _cell_length_b 17.2458(8) _cell_length_c 22.7590(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4674.4(4) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5505 _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 26.42 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 0.585 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6890 _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 38835 _diffrn_reflns_av_R_equivalents 0.0669 _diffrn_reflns_av_sigmaI/netI 0.0506 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5345 _reflns_number_gt 3689 _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^)+(0.0423P)^2^+3.2536P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5345 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0788 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1078 _refine_ls_wR_factor_gt 0.0944 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 P1 P 0.69754(5) 0.09129(4) 0.62286(3) 0.01820(15) Uani 1 1 d . . . Cl1 Cl 0.51966(6) 0.35813(5) 0.59849(3) 0.0414(2) Uani 1 1 d . . . Cl2 Cl 0.48926(6) 0.30684(4) 0.72518(3) 0.03454(18) Uani 1 1 d . . . Cl3 Cl 0.27360(6) 0.07860(4) 0.62560(3) 0.03229(17) Uani 1 1 d . . . Cl4 Cl 0.34147(6) 0.16417(4) 0.51363(3) 0.02987(17) Uani 1 1 d . . . O1 O 0.48170(15) 0.12002(10) 0.59884(8) 0.0248(4) Uani 1 1 d . . . O2 O 0.57198(15) 0.21866(10) 0.64154(8) 0.0322(4) Uani 1 1 d . . . C1 C 0.5666(2) 0.15142(14) 0.62014(10) 0.0197(5) Uani 1 1 d . . . C2 C 0.3561(2) 0.24023(13) 0.62693(10) 0.0190(5) Uani 1 1 d . . . C3 C 0.2585(2) 0.27957(14) 0.63228(10) 0.0216(5) Uani 1 1 d . . . C4 C 0.2475(2) 0.35908(15) 0.65981(12) 0.0295(6) Uani 1 1 d . . . H4A H 0.3224 0.3792 0.6692 0.044 Uiso 1 1 calc R . . H4B H 0.2030 0.3553 0.6959 0.044 Uiso 1 1 calc R . . H4C H 0.2101 0.3942 0.6322 0.044 Uiso 1 1 calc R . . C5 C 0.1461(2) 0.25069(16) 0.61145(12) 0.0307(6) Uani 1 1 d . . . H5A H 0.1563 0.2027 0.5890 0.046 Uiso 1 1 calc R . . H5B H 0.1111 0.2900 0.5863 0.046 Uiso 1 1 calc R . . H5C H 0.0977 0.2406 0.6454 0.046 Uiso 1 1 calc R . . C6 C 0.6470(2) 0.00329(14) 0.66545(10) 0.0224(5) Uani 1 1 d . . . C7 C 0.5779(2) -0.05112(15) 0.62631(11) 0.0280(6) Uani 1 1 d . . . H7A H 0.5492 -0.0943 0.6499 0.042 Uiso 1 1 calc R . . H7B H 0.6256 -0.0714 0.5948 0.042 Uiso 1 1 calc R . . H7C H 0.5148 -0.0225 0.6092 0.042 Uiso 1 1 calc R . . C8 C 0.5694(2) 0.02908(16) 0.71612(11) 0.0303(6) Uani 1 1 d . . . H8A H 0.5444 -0.0166 0.7382 0.045 Uiso 1 1 calc R . . H8B H 0.5039 0.0561 0.7000 0.045 Uiso 1 1 calc R . . H8C H 0.6105 0.0640 0.7424 0.045 Uiso 1 1 calc R . . C9 C 0.7470(2) -0.04266(16) 0.69037(11) 0.0308(6) Uani 1 1 d . . . H9A H 0.7196 -0.0902 0.7092 0.046 Uiso 1 1 calc R . . H9B H 0.7866 -0.0109 0.7194 0.046 Uiso 1 1 calc R . . H9C H 0.7985 -0.0562 0.6584 0.046 Uiso 1 1 calc R . . C10 C 0.8058(2) 0.15062(15) 0.66312(11) 0.0253(6) Uani 1 1 d . . . C11 C 0.7719(3) 0.15762(17) 0.72819(12) 0.0360(7) Uani 1 1 d . . . H11A H 0.8244 0.1923 0.7485 0.054 Uiso 1 1 calc R . . H11B H 0.7740 0.1063 0.7466 0.054 Uiso 1 1 calc R . . H11C H 0.6957 0.1788 0.7309 0.054 Uiso 1 1 calc R . . C12 C 0.8186(2) 0.23421(15) 0.63897(12) 0.0305(6) Uani 1 1 d . . . H12A H 0.8734 0.2626 0.6628 0.046 Uiso 1 1 calc R . . H12B H 0.7459 0.2607 0.6407 0.046 Uiso 1 1 calc R . . H12C H 0.8445 0.2321 0.5981 0.046 Uiso 1 1 calc R . . C13 C 0.9209(2) 0.11021(16) 0.65862(12) 0.0320(6) Uani 1 1 d . . . H13A H 0.9744 0.1359 0.6849 0.048 Uiso 1 1 calc R . . H13B H 0.9483 0.1134 0.6181 0.048 Uiso 1 1 calc R . . H13C H 0.9132 0.0557 0.6700 0.048 Uiso 1 1 calc R . . C14 C 0.7364(2) 0.07112(14) 0.54388(10) 0.0205(5) Uani 1 1 d . . . C15 C 0.7896(2) 0.14323(16) 0.51682(11) 0.0295(6) Uani 1 1 d . . . H15A H 0.7995 0.1353 0.4745 0.044 Uiso 1 1 calc R . . H15B H 0.8629 0.1526 0.5351 0.044 Uiso 1 1 calc R . . H15C H 0.7407 0.1881 0.5235 0.044 Uiso 1 1 calc R . . C16 C 0.6323(2) 0.05185(15) 0.50695(10) 0.0254(6) Uani 1 1 d . . . H16A H 0.6554 0.0395 0.4667 0.038 Uiso 1 1 calc R . . H16B H 0.5816 0.0966 0.5065 0.038 Uiso 1 1 calc R . . H16C H 0.5935 0.0071 0.5241 0.038 Uiso 1 1 calc R . . C17 C 0.8199(2) 0.00338(16) 0.54123(11) 0.0295(6) Uani 1 1 d . . . H17A H 0.8449 -0.0041 0.5006 0.044 Uiso 1 1 calc R . . H17B H 0.7833 -0.0440 0.5553 0.044 Uiso 1 1 calc R . . H17C H 0.8849 0.0150 0.5661 0.044 Uiso 1 1 calc R . . B1 B 0.4712(3) 0.27761(17) 0.64631(12) 0.0215(6) Uani 1 1 d . . . B2 B 0.3611(2) 0.15860(17) 0.59508(12) 0.0218(6) 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 P1 0.0222(3) 0.0180(3) 0.0144(3) 0.0009(2) -0.0009(2) 0.0001(3) Cl1 0.0386(4) 0.0427(4) 0.0429(4) 0.0180(3) -0.0057(3) -0.0182(4) Cl2 0.0380(4) 0.0413(4) 0.0244(3) -0.0087(3) -0.0036(3) -0.0032(3) Cl3 0.0403(4) 0.0238(3) 0.0328(4) -0.0015(3) 0.0060(3) -0.0101(3) Cl4 0.0465(4) 0.0249(3) 0.0182(3) -0.0028(3) -0.0053(3) 0.0052(3) O1 0.0253(10) 0.0195(9) 0.0296(10) -0.0056(8) -0.0056(8) 0.0019(8) O2 0.0256(10) 0.0264(10) 0.0447(12) -0.0128(9) -0.0041(9) 0.0019(8) C1 0.0249(13) 0.0200(13) 0.0142(11) 0.0018(10) 0.0026(10) 0.0003(11) C2 0.0248(13) 0.0192(12) 0.0128(11) -0.0008(9) 0.0020(10) -0.0034(10) C3 0.0277(14) 0.0203(13) 0.0169(11) 0.0014(10) 0.0025(10) -0.0026(11) C4 0.0332(16) 0.0257(14) 0.0294(14) -0.0023(12) 0.0004(12) 0.0067(12) C5 0.0235(14) 0.0297(14) 0.0390(16) -0.0022(12) 0.0009(12) 0.0006(12) C6 0.0282(14) 0.0219(13) 0.0172(12) 0.0041(10) 0.0030(11) 0.0008(11) C7 0.0358(16) 0.0218(13) 0.0263(14) 0.0016(11) 0.0035(12) -0.0031(12) C8 0.0374(17) 0.0326(15) 0.0209(13) 0.0038(11) 0.0091(12) -0.0013(13) C9 0.0365(16) 0.0302(15) 0.0257(13) 0.0102(12) 0.0009(12) 0.0037(13) C10 0.0283(14) 0.0258(14) 0.0217(12) 0.0005(11) -0.0074(11) -0.0051(12) C11 0.0436(18) 0.0428(17) 0.0217(13) -0.0034(12) -0.0080(13) -0.0088(15) C12 0.0325(16) 0.0244(14) 0.0345(15) 0.0013(12) -0.0087(12) -0.0049(12) C13 0.0276(15) 0.0347(16) 0.0337(15) 0.0067(13) -0.0096(12) -0.0028(13) C14 0.0239(13) 0.0245(13) 0.0132(11) 0.0003(10) 0.0011(10) 0.0022(11) C15 0.0338(16) 0.0336(15) 0.0211(13) 0.0065(11) 0.0021(11) -0.0034(13) C16 0.0319(15) 0.0277(14) 0.0167(12) -0.0034(11) -0.0018(11) 0.0036(12) C17 0.0296(15) 0.0340(15) 0.0249(13) -0.0034(12) 0.0017(11) 0.0073(13) B1 0.0255(16) 0.0192(14) 0.0199(14) -0.0035(11) 0.0033(12) -0.0004(12) B2 0.0223(15) 0.0233(15) 0.0198(14) -0.0012(12) -0.0015(11) -0.0030(12) _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 P1 C1 1.874(3) . ? P1 C10 1.884(3) . ? P1 C14 1.888(2) . ? P1 C6 1.899(2) . ? Cl1 B1 1.856(3) . ? Cl2 B1 1.877(3) . ? Cl3 B2 1.863(3) . ? Cl4 B2 1.871(3) . ? O1 C1 1.245(3) . ? O1 B2 1.585(3) . ? O2 C1 1.259(3) . ? O2 B1 1.577(3) . ? C2 C3 1.352(4) . ? C2 B1 1.577(4) . ? C2 B2 1.585(4) . ? C3 C5 1.504(4) . ? C3 C4 1.513(3) . ? C6 C7 1.533(4) . ? C6 C9 1.539(4) . ? C6 C8 1.543(3) . ? C10 C11 1.540(4) . ? C10 C13 1.541(4) . ? C10 C12 1.550(3) . ? C14 C15 1.526(3) . ? C14 C16 1.534(3) . ? C14 C17 1.536(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 C1 P1 C10 106.57(11) . . ? C1 P1 C14 105.93(11) . . ? C10 P1 C14 113.29(12) . . ? C1 P1 C6 101.25(11) . . ? C10 P1 C6 113.76(11) . . ? C14 P1 C6 114.61(11) . . ? C1 O1 B2 125.04(19) . . ? C1 O2 B1 125.5(2) . . ? O1 C1 O2 126.3(2) . . ? O1 C1 P1 116.62(18) . . ? O2 C1 P1 117.01(19) . . ? C3 C2 B1 121.1(2) . . ? C3 C2 B2 121.3(2) . . ? B1 C2 B2 117.3(2) . . ? C2 C3 C5 124.8(2) . . ? C2 C3 C4 124.5(2) . . ? C5 C3 C4 110.7(2) . . ? C7 C6 C9 108.3(2) . . ? C7 C6 C8 106.8(2) . . ? C9 C6 C8 109.7(2) . . ? C7 C6 P1 111.26(16) . . ? C9 C6 P1 110.74(18) . . ? C8 C6 P1 109.94(17) . . ? C11 C10 C13 109.4(2) . . ? C11 C10 C12 107.1(2) . . ? C13 C10 C12 108.0(2) . . ? C11 C10 P1 109.32(18) . . ? C13 C10 P1 109.32(18) . . ? C12 C10 P1 113.56(17) . . ? C15 C14 C16 106.9(2) . . ? C15 C14 C17 109.6(2) . . ? C16 C14 C17 109.7(2) . . ? C15 C14 P1 109.62(17) . . ? C16 C14 P1 111.32(17) . . ? C17 C14 P1 109.65(16) . . ? O2 B1 C2 112.2(2) . . ? O2 B1 Cl1 101.84(17) . . ? C2 B1 Cl1 114.33(19) . . ? O2 B1 Cl2 98.72(17) . . ? C2 B1 Cl2 118.49(18) . . ? Cl1 B1 Cl2 108.91(15) . . ? C2 B2 O1 112.5(2) . . ? C2 B2 Cl3 117.79(18) . . ? O1 B2 Cl3 100.14(16) . . ? C2 B2 Cl4 113.76(18) . . ? O1 B2 Cl4 100.86(16) . . ? Cl3 B2 Cl4 109.71(14) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.772 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.070 #===end data_((C6F5)2B)2CCMe2(O2CPBu3) _database_code_depnum_ccdc_archive 'CCDC 803526' #TrackingRef '- all-cifs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41.50 H34 B2 Cl F20 O2 P' _chemical_formula_weight 1032.73 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' B B 0.0013 0.0007 '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' 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 11.3566(4) _cell_length_b 11.5364(5) _cell_length_c 33.8526(13) _cell_angle_alpha 86.446(2) _cell_angle_beta 83.838(2) _cell_angle_gamma 80.780(2) _cell_volume 4348.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 69357 _cell_measurement_theta_min 1.79 _cell_measurement_theta_max 28.70 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2084 _exptl_absorpt_coefficient_mu 0.248 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6941 _exptl_absorpt_correction_T_max 0.7458 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 69357 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.1008 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 28.70 _reflns_number_total 22022 _reflns_number_gt 12060 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0948P)^2^+0.8418P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22022 _refine_ls_number_parameters 1255 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1421 _refine_ls_R_factor_gt 0.0687 _refine_ls_wR_factor_ref 0.1984 _refine_ls_wR_factor_gt 0.1637 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 P1 P 0.05688(7) 0.68945(7) 0.38408(2) 0.01670(18) Uani 1 1 d . . . P2 P 0.93242(7) 0.79948(7) 0.11924(2) 0.01616(17) Uani 1 1 d . . . F1 F -0.04368(15) 0.33080(16) 0.34492(5) 0.0243(4) Uani 1 1 d . . . F2 F -0.18781(16) 0.22623(17) 0.39798(6) 0.0298(5) Uani 1 1 d . . . F3 F -0.10037(17) 0.10572(17) 0.46286(6) 0.0329(5) Uani 1 1 d . . . F4 F 0.13871(18) 0.08346(18) 0.47137(6) 0.0347(5) Uani 1 1 d . . . F5 F 0.28459(16) 0.18045(17) 0.41867(6) 0.0283(4) Uani 1 1 d . . . F6 F 0.25005(17) 0.50782(16) 0.28214(5) 0.0289(4) Uani 1 1 d . . . F7 F 0.2195(2) 0.4951(2) 0.20581(6) 0.0446(6) Uani 1 1 d . . . F8 F 0.14231(19) 0.3058(2) 0.17962(6) 0.0488(6) Uani 1 1 d . . . F9 F 0.10531(19) 0.1216(2) 0.23223(7) 0.0439(6) Uani 1 1 d . . . F10 F 0.12408(17) 0.13647(16) 0.30877(6) 0.0330(5) Uani 1 1 d . . . F11 F 0.23648(15) 0.41199(16) 0.43582(5) 0.0231(4) Uani 1 1 d . . . F12 F 0.30085(17) 0.34646(18) 0.50794(5) 0.0348(5) Uani 1 1 d . . . F13 F 0.53339(18) 0.33199(19) 0.52357(6) 0.0387(5) Uani 1 1 d . . . F14 F 0.70031(16) 0.38738(18) 0.46459(6) 0.0339(5) Uani 1 1 d . . . F15 F 0.63911(15) 0.45457(17) 0.39213(5) 0.0277(4) Uani 1 1 d . . . F16 F 0.47173(16) 0.67391(16) 0.38176(5) 0.0255(4) Uani 1 1 d . . . F17 F 0.59720(19) 0.80859(18) 0.33285(6) 0.0379(5) Uani 1 1 d . . . F18 F 0.6770(2) 0.7431(2) 0.25753(7) 0.0502(6) Uani 1 1 d . . . F19 F 0.6223(2) 0.5414(2) 0.23186(6) 0.0497(6) Uani 1 1 d . . . F20 F 0.49357(18) 0.40834(18) 0.27837(6) 0.0335(5) Uani 1 1 d . . . F21 F 0.33727(15) 1.02273(17) 0.10436(5) 0.0287(4) Uani 1 1 d . . . F22 F 0.26089(16) 1.09947(17) 0.03452(6) 0.0326(5) Uani 1 1 d . . . F23 F 0.41083(18) 1.17835(18) -0.02484(6) 0.0372(5) Uani 1 1 d . . . F24 F 0.64708(17) 1.17277(18) -0.01379(5) 0.0338(5) Uani 1 1 d . . . F25 F 0.72596(15) 1.09939(16) 0.05589(5) 0.0240(4) Uani 1 1 d . . . F26 F 0.49647(18) 1.06913(18) 0.21578(6) 0.0352(5) Uani 1 1 d . . . F27 F 0.3869(2) 0.9209(2) 0.26301(6) 0.0531(6) Uani 1 1 d . . . F28 F 0.3466(2) 0.7146(2) 0.23641(7) 0.0489(6) Uani 1 1 d . . . F29 F 0.42051(17) 0.66060(17) 0.15938(7) 0.0369(5) Uani 1 1 d . . . F30 F 0.51770(16) 0.81347(16) 0.10972(5) 0.0273(4) Uani 1 1 d . . . F31 F 0.74055(16) 0.97112(15) 0.20594(5) 0.0250(4) Uani 1 1 d . . . F32 F 0.76586(18) 0.97605(18) 0.28299(6) 0.0342(5) Uani 1 1 d . . . F33 F 0.83472(17) 1.16602(19) 0.31277(5) 0.0349(5) Uani 1 1 d . . . F34 F 0.86936(18) 1.35609(18) 0.26324(6) 0.0348(5) Uani 1 1 d . . . F35 F 0.85402(17) 1.35055(16) 0.18612(6) 0.0296(4) Uani 1 1 d . . . F36 F 1.02442(16) 1.16295(16) 0.14228(6) 0.0280(4) Uani 1 1 d . . . F37 F 1.15986(18) 1.27413(19) 0.08879(7) 0.0399(5) Uani 1 1 d . . . F38 F 1.0608(2) 1.4049(2) 0.02751(7) 0.0494(6) Uani 1 1 d . . . F39 F 0.8193(2) 1.43167(18) 0.02421(6) 0.0405(5) Uani 1 1 d . . . F40 F 0.68215(17) 1.32567(16) 0.07731(6) 0.0304(5) Uani 1 1 d . . . O1 O 0.12928(17) 0.47159(17) 0.35595(6) 0.0166(4) Uani 1 1 d . . . O2 O 0.27550(17) 0.56440(17) 0.37268(6) 0.0168(4) Uani 1 1 d . . . O3 O 0.70977(17) 0.92714(17) 0.11828(6) 0.0169(4) Uani 1 1 d . . . O4 O 0.85401(18) 1.02419(17) 0.13428(6) 0.0176(4) Uani 1 1 d . . . C1 C 0.1686(3) 0.5557(3) 0.36881(8) 0.0155(6) Uani 1 1 d . . . C2 C 0.3468(3) 0.3429(3) 0.35113(9) 0.0188(7) Uani 1 1 d . . . C3 C 0.4271(3) 0.2456(3) 0.34422(9) 0.0229(7) Uani 1 1 d . . . C4 C 0.3960(3) 0.1304(3) 0.33282(11) 0.0331(8) Uani 1 1 d . . . H4A H 0.3096 0.1305 0.3387 0.050 Uiso 1 1 calc R . . H4B H 0.4397 0.0654 0.3480 0.050 Uiso 1 1 calc R . . H4C H 0.4185 0.1205 0.3043 0.050 Uiso 1 1 calc R . . C5 C 0.5612(3) 0.2377(3) 0.34571(12) 0.0340(9) Uani 1 1 d . . . H5A H 0.5811 0.3169 0.3470 0.051 Uiso 1 1 calc R . . H5B H 0.6037 0.2013 0.3218 0.051 Uiso 1 1 calc R . . H5C H 0.5853 0.1900 0.3693 0.051 Uiso 1 1 calc R . . C6 C 0.1289(3) 0.2633(3) 0.37857(9) 0.0189(7) Uani 1 1 d . . . C7 C 0.0063(3) 0.2688(3) 0.37577(9) 0.0203(7) Uani 1 1 d . . . C8 C -0.0707(3) 0.2160(3) 0.40270(10) 0.0223(7) Uani 1 1 d . . . C9 C -0.0263(3) 0.1551(3) 0.43562(9) 0.0232(7) Uani 1 1 d . . . C10 C 0.0940(3) 0.1445(3) 0.43967(9) 0.0236(7) Uani 1 1 d . . . C11 C 0.1686(3) 0.1970(3) 0.41162(9) 0.0208(7) Uani 1 1 d . . . C12 C 0.1864(3) 0.3248(3) 0.30011(9) 0.0194(7) Uani 1 1 d . . . C13 C 0.2104(3) 0.4104(3) 0.27147(9) 0.0229(7) Uani 1 1 d . . . C14 C 0.1961(3) 0.4059(3) 0.23152(10) 0.0289(8) Uani 1 1 d . . . C15 C 0.1586(3) 0.3103(3) 0.21814(10) 0.0302(8) Uani 1 1 d . . . C16 C 0.1387(3) 0.2191(3) 0.24466(10) 0.0288(8) Uani 1 1 d . . . C17 C 0.1509(3) 0.2290(3) 0.28461(10) 0.0226(7) Uani 1 1 d . . . C18 C 0.4343(3) 0.4340(3) 0.40937(9) 0.0178(6) Uani 1 1 d . . . C19 C 0.3547(3) 0.4061(3) 0.44103(9) 0.0178(6) Uani 1 1 d . . . C20 C 0.3841(3) 0.3721(3) 0.47899(9) 0.0233(7) Uani 1 1 d . . . C21 C 0.5015(3) 0.3647(3) 0.48680(9) 0.0253(7) Uani 1 1 d . . . C22 C 0.5857(3) 0.3924(3) 0.45700(10) 0.0250(7) Uani 1 1 d . . . C23 C 0.5509(3) 0.4267(3) 0.41951(9) 0.0196(7) Uani 1 1 d . . . C24 C 0.4743(3) 0.5330(3) 0.33323(9) 0.0190(7) Uani 1 1 d . . . C25 C 0.5054(3) 0.6376(3) 0.34426(9) 0.0208(7) Uani 1 1 d . . . C26 C 0.5712(3) 0.7090(3) 0.31985(10) 0.0258(7) Uani 1 1 d . . . C27 C 0.6111(3) 0.6759(3) 0.28167(10) 0.0312(8) Uani 1 1 d . . . C28 C 0.5839(3) 0.5737(3) 0.26918(10) 0.0328(8) Uani 1 1 d . . . C29 C 0.5163(3) 0.5053(3) 0.29425(9) 0.0241(7) Uani 1 1 d . . . C30 C -0.0948(3) 0.6448(3) 0.38363(10) 0.0252(7) Uani 1 1 d . . . C31 C -0.1179(3) 0.6223(3) 0.34076(11) 0.0326(8) Uani 1 1 d . . . H31A H -0.1929 0.5901 0.3414 0.049 Uiso 1 1 calc R . . H31B H -0.0514 0.5661 0.3289 0.049 Uiso 1 1 calc R . . H31C H -0.1239 0.6965 0.3248 0.049 Uiso 1 1 calc R . . C32 C -0.1014(3) 0.5309(3) 0.40985(10) 0.0287(8) Uani 1 1 d . . . H32A H -0.1559 0.4853 0.3994 0.043 Uiso 1 1 calc R . . H32B H -0.1311 0.5513 0.4372 0.043 Uiso 1 1 calc R . . H32C H -0.0213 0.4841 0.4095 0.043 Uiso 1 1 calc R . . C33 C -0.1968(3) 0.7398(3) 0.40036(12) 0.0356(9) Uani 1 1 d . . . H33A H -0.2739 0.7119 0.4004 0.053 Uiso 1 1 calc R . . H33B H -0.1971 0.8123 0.3837 0.053 Uiso 1 1 calc R . . H33C H -0.1840 0.7552 0.4276 0.053 Uiso 1 1 calc R . . C34 C 0.0842(3) 0.7295(3) 0.43523(9) 0.0220(7) Uani 1 1 d . . . C35 C 0.0340(3) 0.6474(3) 0.46803(10) 0.0319(8) Uani 1 1 d . . . H35A H 0.0536 0.6681 0.4939 0.048 Uiso 1 1 calc R . . H35B H 0.0696 0.5658 0.4631 0.048 Uiso 1 1 calc R . . H35C H -0.0533 0.6559 0.4680 0.048 Uiso 1 1 calc R . . C36 C 0.0215(3) 0.8563(3) 0.44185(11) 0.0327(8) Uani 1 1 d . . . H36A H 0.0350 0.8792 0.4682 0.049 Uiso 1 1 calc R . . H36B H -0.0648 0.8608 0.4402 0.049 Uiso 1 1 calc R . . H36C H 0.0543 0.9095 0.4214 0.049 Uiso 1 1 calc R . . C37 C 0.2183(3) 0.7223(3) 0.44020(10) 0.0285(8) Uani 1 1 d . . . H37A H 0.2274 0.7545 0.4656 0.043 Uiso 1 1 calc R . . H37B H 0.2560 0.7678 0.4184 0.043 Uiso 1 1 calc R . . H37C H 0.2569 0.6400 0.4398 0.043 Uiso 1 1 calc R . . C38 C 0.0908(3) 0.8054(3) 0.34465(9) 0.0236(7) Uani 1 1 d . . . C39 C 0.1199(4) 0.7480(3) 0.30427(10) 0.0369(9) Uani 1 1 d . . . H39A H 0.1305 0.8087 0.2832 0.055 Uiso 1 1 calc R . . H39B H 0.0539 0.7074 0.2992 0.055 Uiso 1 1 calc R . . H39C H 0.1939 0.6912 0.3046 0.055 Uiso 1 1 calc R . . C40 C 0.2030(3) 0.8581(3) 0.35184(11) 0.0330(8) Uani 1 1 d . . . H40A H 0.2225 0.9118 0.3294 0.049 Uiso 1 1 calc R . . H40B H 0.2708 0.7947 0.3543 0.049 Uiso 1 1 calc R . . H40C H 0.1870 0.9013 0.3764 0.049 Uiso 1 1 calc R . . C41 C -0.0156(3) 0.9049(3) 0.34260(11) 0.0325(8) Uani 1 1 d . . . H41A H 0.0059 0.9658 0.3229 0.049 Uiso 1 1 calc R . . H41B H -0.0361 0.9389 0.3687 0.049 Uiso 1 1 calc R . . H41C H -0.0847 0.8736 0.3349 0.049 Uiso 1 1 calc R . . C42 C 0.8142(3) 0.9351(3) 0.12491(8) 0.0150(6) Uani 1 1 d . . . C43 C 0.6331(3) 1.1462(3) 0.14159(8) 0.0184(6) Uani 1 1 d . . . C44 C 0.5506(3) 1.2401(3) 0.15078(10) 0.0242(7) Uani 1 1 d . . . C45 C 0.4167(3) 1.2443(3) 0.15112(12) 0.0362(9) Uani 1 1 d . . . H45A H 0.3992 1.1650 0.1481 0.054 Uiso 1 1 calc R . . H45B H 0.3876 1.2963 0.1291 0.054 Uiso 1 1 calc R . . H45C H 0.3766 1.2742 0.1764 0.054 Uiso 1 1 calc R . . C46 C 0.5798(3) 1.3558(3) 0.16319(11) 0.0343(9) Uani 1 1 d . . . H46A H 0.6654 1.3586 0.1564 0.051 Uiso 1 1 calc R . . H46B H 0.5601 1.3621 0.1920 0.051 Uiso 1 1 calc R . . H46C H 0.5326 1.4212 0.1492 0.051 Uiso 1 1 calc R . . C47 C 0.5367(3) 1.0579(3) 0.08444(9) 0.0197(7) Uani 1 1 d . . . C48 C 0.4190(3) 1.0601(3) 0.07649(9) 0.0221(7) Uani 1 1 d . . . C49 C 0.3762(3) 1.1003(3) 0.04040(10) 0.0250(7) Uani 1 1 d . . . C50 C 0.4516(3) 1.1401(3) 0.00994(9) 0.0258(7) Uani 1 1 d . . . C51 C 0.5695(3) 1.1374(3) 0.01593(9) 0.0234(7) Uani 1 1 d . . . C52 C 0.6088(3) 1.0975(3) 0.05232(9) 0.0195(7) Uani 1 1 d . . . C53 C 0.5139(3) 0.9505(3) 0.15948(9) 0.0204(7) Uani 1 1 d . . . C54 C 0.4780(3) 0.9715(3) 0.19918(10) 0.0270(8) Uani 1 1 d . . . C55 C 0.4205(3) 0.8944(4) 0.22472(10) 0.0347(9) Uani 1 1 d . . . C56 C 0.4004(3) 0.7904(3) 0.21160(11) 0.0316(8) Uani 1 1 d . . . C57 C 0.4352(3) 0.7640(3) 0.17279(10) 0.0260(7) Uani 1 1 d . . . C58 C 0.4883(3) 0.8442(3) 0.14796(9) 0.0218(7) Uani 1 1 d . . . C59 C 0.7953(3) 1.1607(3) 0.19158(9) 0.0188(6) Uani 1 1 d . . . C60 C 0.7746(3) 1.0700(3) 0.21855(9) 0.0210(7) Uani 1 1 d . . . C61 C 0.7870(3) 1.0689(3) 0.25871(9) 0.0244(7) Uani 1 1 d . . . C62 C 0.8200(3) 1.1653(3) 0.27409(9) 0.0254(7) Uani 1 1 d . . . C63 C 0.8385(3) 1.2598(3) 0.24880(10) 0.0250(7) Uani 1 1 d . . . C64 C 0.8287(3) 1.2549(3) 0.20873(9) 0.0217(7) Uani 1 1 d . . . C65 C 0.8460(3) 1.2340(3) 0.11276(9) 0.0193(7) Uani 1 1 d . . . C66 C 0.9690(3) 1.2277(3) 0.11324(9) 0.0233(7) Uani 1 1 d . . . C67 C 1.0421(3) 1.2825(3) 0.08552(10) 0.0276(8) Uani 1 1 d . . . C68 C 0.9922(3) 1.3496(3) 0.05478(10) 0.0320(8) Uani 1 1 d . . . C69 C 0.8706(3) 1.3625(3) 0.05325(9) 0.0290(8) Uani 1 1 d . . . C70 C 0.8003(3) 1.3058(3) 0.08156(9) 0.0232(7) Uani 1 1 d . . . C71 C 0.8503(3) 0.6692(3) 0.12206(9) 0.0223(7) Uani 1 1 d . . . C72 C 0.7566(3) 0.6737(3) 0.15864(10) 0.0276(8) Uani 1 1 d . . . H72A H 0.6993 0.6206 0.1554 0.041 Uiso 1 1 calc R . . H72B H 0.7139 0.7541 0.1611 0.041 Uiso 1 1 calc R . . H72C H 0.7970 0.6491 0.1826 0.041 Uiso 1 1 calc R . . C73 C 0.7852(3) 0.6684(3) 0.08434(10) 0.0269(8) Uani 1 1 d . . . H73A H 0.7386 0.6034 0.0868 0.040 Uiso 1 1 calc R . . H73B H 0.8445 0.6584 0.0610 0.040 Uiso 1 1 calc R . . H73C H 0.7314 0.7430 0.0812 0.040 Uiso 1 1 calc R . . C74 C 0.9382(3) 0.5537(3) 0.12543(11) 0.0304(8) Uani 1 1 d . . . H74A H 0.8944 0.4870 0.1256 0.046 Uiso 1 1 calc R . . H74B H 0.9764 0.5507 0.1502 0.046 Uiso 1 1 calc R . . H74C H 0.9996 0.5497 0.1027 0.046 Uiso 1 1 calc R . . C75 C 1.0125(3) 0.8275(3) 0.06860(9) 0.0240(7) Uani 1 1 d . . . C76 C 0.9195(3) 0.8770(3) 0.03921(10) 0.0337(9) Uani 1 1 d . . . H76A H 0.9602 0.8829 0.0123 0.050 Uiso 1 1 calc R . . H76B H 0.8797 0.9551 0.0471 0.050 Uiso 1 1 calc R . . H76C H 0.8597 0.8243 0.0397 0.050 Uiso 1 1 calc R . . C77 C 1.0868(3) 0.7147(3) 0.05202(10) 0.0305(8) Uani 1 1 d . . . H77A H 1.1343 0.7341 0.0273 0.046 Uiso 1 1 calc R . . H77B H 1.0330 0.6603 0.0467 0.046 Uiso 1 1 calc R . . H77C H 1.1407 0.6776 0.0715 0.046 Uiso 1 1 calc R . . C78 C 1.0934(3) 0.9202(3) 0.07060(12) 0.0377(9) Uani 1 1 d . . . H78A H 1.1250 0.9427 0.0436 0.056 Uiso 1 1 calc R . . H78B H 1.1600 0.8879 0.0862 0.056 Uiso 1 1 calc R . . H78C H 1.0470 0.9895 0.0833 0.056 Uiso 1 1 calc R . . C79 C 1.0329(3) 0.7897(3) 0.16066(10) 0.0274(8) Uani 1 1 d . . . C80 C 1.1513(3) 0.7072(3) 0.14833(12) 0.0379(9) Uani 1 1 d . . . H80A H 1.1992 0.6915 0.1710 0.057 Uiso 1 1 calc R . . H80B H 1.1967 0.7450 0.1263 0.057 Uiso 1 1 calc R . . H80C H 1.1328 0.6330 0.1398 0.057 Uiso 1 1 calc R . . C81 C 1.0675(3) 0.9101(3) 0.16919(12) 0.0367(9) Uani 1 1 d . . . H81A H 1.1312 0.8975 0.1871 0.055 Uiso 1 1 calc R . . H81B H 0.9972 0.9600 0.1817 0.055 Uiso 1 1 calc R . . H81C H 1.0960 0.9486 0.1442 0.055 Uiso 1 1 calc R . . C82 C 0.9722(4) 0.7420(3) 0.19953(10) 0.0385(9) Uani 1 1 d . . . H82A H 1.0222 0.7453 0.2212 0.058 Uiso 1 1 calc R . . H82B H 0.9619 0.6603 0.1966 0.058 Uiso 1 1 calc R . . H82C H 0.8936 0.7897 0.2057 0.058 Uiso 1 1 calc R . . B1 B 0.2088(3) 0.3399(3) 0.34660(10) 0.0180(7) Uani 1 1 d . . . B2 B 0.3899(3) 0.4590(3) 0.36463(10) 0.0179(7) Uani 1 1 d . . . B3 B 0.5906(3) 1.0310(3) 0.12780(10) 0.0189(7) Uani 1 1 d . . . B4 B 0.7718(3) 1.1520(3) 0.14476(10) 0.0186(7) Uani 1 1 d . . . C83 C 0.5300(13) 1.4828(15) -0.0219(3) 0.136(6) Uiso 0.50 1 d PD . . H83A H 0.4557 1.5460 -0.0169 0.163 Uiso 0.50 1 d P . . H83B H 0.5451 1.4298 -0.0014 0.163 Uiso 0.50 1 d P . . C84 C 0.5044(18) 0.003(3) 0.4735(6) 0.275(16) Uiso 0.50 1 d PD . . H84A H 0.4398 0.0800 0.4732 0.330 Uiso 0.50 1 d P . . H84B H 0.4963 -0.0395 0.4973 0.330 Uiso 0.50 1 d P . . Cl1 Cl 0.5536(9) 1.4405(7) -0.0701(2) 0.282(5) Uani 0.50 1 d PD . . Cl2 Cl 0.6454(9) 1.5540(6) -0.0408(3) 0.302(6) Uani 0.50 1 d PD . . Cl3 Cl 0.6405(6) 0.0362(6) 0.4563(3) 0.238(4) Uani 0.50 1 d PD . . Cl4 Cl 0.5044(8) -0.0686(7) 0.4300(2) 0.245(4) Uani 0.50 1 d PD . . 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 P1 0.0146(4) 0.0172(4) 0.0180(4) 0.0003(3) -0.0016(3) -0.0020(3) P2 0.0164(4) 0.0148(4) 0.0170(4) 0.0007(3) -0.0013(3) -0.0023(3) F1 0.0208(10) 0.0281(11) 0.0251(10) 0.0048(8) -0.0056(7) -0.0075(8) F2 0.0183(10) 0.0373(12) 0.0348(11) -0.0019(9) 0.0017(8) -0.0097(8) F3 0.0332(11) 0.0363(12) 0.0288(11) 0.0050(9) 0.0089(8) -0.0143(9) F4 0.0389(12) 0.0364(12) 0.0282(11) 0.0133(9) -0.0043(9) -0.0086(9) F5 0.0213(10) 0.0321(11) 0.0312(11) 0.0085(8) -0.0062(8) -0.0047(8) F6 0.0411(12) 0.0223(11) 0.0247(10) 0.0022(8) 0.0001(8) -0.0131(9) F7 0.0584(15) 0.0504(15) 0.0239(11) 0.0110(10) -0.0037(10) -0.0105(12) F8 0.0425(13) 0.0855(18) 0.0226(11) -0.0156(11) -0.0058(9) -0.0160(12) F9 0.0396(13) 0.0521(14) 0.0465(13) -0.0295(11) 0.0008(10) -0.0198(11) F10 0.0389(12) 0.0240(11) 0.0397(12) -0.0067(9) 0.0003(9) -0.0164(9) F11 0.0147(9) 0.0317(11) 0.0236(9) 0.0010(8) -0.0005(7) -0.0076(8) F12 0.0313(11) 0.0501(14) 0.0217(10) 0.0073(9) 0.0052(8) -0.0114(10) F13 0.0395(12) 0.0549(14) 0.0225(10) 0.0116(9) -0.0118(9) -0.0092(10) F14 0.0214(10) 0.0514(14) 0.0315(11) 0.0039(9) -0.0128(8) -0.0088(9) F15 0.0152(9) 0.0409(12) 0.0271(10) 0.0052(8) -0.0009(8) -0.0086(8) F16 0.0274(10) 0.0273(11) 0.0239(10) -0.0044(8) -0.0003(8) -0.0109(8) F17 0.0442(13) 0.0321(12) 0.0422(12) 0.0028(9) -0.0035(10) -0.0226(10) F18 0.0588(15) 0.0603(16) 0.0369(13) 0.0089(11) 0.0084(11) -0.0391(13) F19 0.0635(16) 0.0684(17) 0.0216(11) -0.0049(10) 0.0152(10) -0.0351(13) F20 0.0403(12) 0.0400(12) 0.0231(10) -0.0098(9) 0.0082(9) -0.0191(10) F21 0.0165(10) 0.0428(12) 0.0275(10) 0.0032(9) -0.0002(8) -0.0100(8) F22 0.0237(11) 0.0403(12) 0.0361(11) -0.0017(9) -0.0118(9) -0.0054(9) F23 0.0440(13) 0.0450(13) 0.0237(10) 0.0048(9) -0.0139(9) -0.0055(10) F24 0.0350(12) 0.0412(13) 0.0229(10) 0.0067(9) 0.0042(8) -0.0065(9) F25 0.0176(10) 0.0265(11) 0.0273(10) 0.0008(8) 0.0000(7) -0.0042(8) F26 0.0410(12) 0.0439(13) 0.0223(10) -0.0092(9) 0.0058(9) -0.0140(10) F27 0.0622(16) 0.0769(18) 0.0216(11) -0.0016(11) 0.0142(10) -0.0276(13) F28 0.0472(14) 0.0544(15) 0.0462(14) 0.0204(11) 0.0065(11) -0.0269(12) F29 0.0293(11) 0.0261(12) 0.0563(14) 0.0044(10) -0.0016(10) -0.0117(9) F30 0.0278(11) 0.0273(11) 0.0288(10) -0.0072(8) 0.0016(8) -0.0108(8) F31 0.0321(11) 0.0222(10) 0.0233(10) 0.0001(8) -0.0038(8) -0.0117(8) F32 0.0402(12) 0.0415(13) 0.0228(10) 0.0102(9) -0.0060(9) -0.0142(10) F33 0.0347(12) 0.0540(14) 0.0184(10) -0.0070(9) -0.0070(8) -0.0089(10) F34 0.0401(12) 0.0350(12) 0.0335(11) -0.0144(9) -0.0074(9) -0.0109(10) F35 0.0409(12) 0.0210(10) 0.0295(11) -0.0029(8) -0.0017(9) -0.0129(9) F36 0.0232(10) 0.0284(11) 0.0337(11) 0.0027(8) -0.0044(8) -0.0083(8) F37 0.0290(12) 0.0428(13) 0.0492(14) -0.0064(10) 0.0089(10) -0.0169(10) F38 0.0620(16) 0.0473(14) 0.0390(13) 0.0064(10) 0.0183(11) -0.0278(12) F39 0.0635(15) 0.0293(12) 0.0269(11) 0.0085(9) -0.0001(10) -0.0082(10) F40 0.0337(12) 0.0269(11) 0.0294(11) 0.0054(8) -0.0053(9) -0.0017(9) O1 0.0153(11) 0.0171(11) 0.0180(10) -0.0015(8) -0.0011(8) -0.0041(9) O2 0.0137(11) 0.0190(11) 0.0183(10) -0.0011(8) -0.0009(8) -0.0051(9) O3 0.0150(11) 0.0179(11) 0.0181(10) -0.0006(8) -0.0008(8) -0.0042(9) O4 0.0188(11) 0.0147(11) 0.0198(11) -0.0011(8) -0.0017(8) -0.0043(9) C1 0.0166(16) 0.0176(16) 0.0129(14) 0.0011(11) 0.0005(11) -0.0064(13) C2 0.0198(16) 0.0220(17) 0.0142(14) -0.0009(12) 0.0014(12) -0.0047(13) C3 0.0202(17) 0.0224(18) 0.0261(17) -0.0011(13) -0.0014(13) -0.0037(14) C4 0.031(2) 0.024(2) 0.044(2) -0.0077(16) -0.0022(16) -0.0023(16) C5 0.0178(18) 0.035(2) 0.047(2) -0.0096(18) 0.0015(16) -0.0001(15) C6 0.0199(16) 0.0186(17) 0.0192(15) -0.0026(12) -0.0016(12) -0.0054(13) C7 0.0232(17) 0.0189(17) 0.0201(15) -0.0020(12) -0.0027(13) -0.0067(13) C8 0.0202(17) 0.0207(18) 0.0275(17) -0.0060(13) -0.0005(13) -0.0068(13) C9 0.0274(18) 0.0202(18) 0.0221(16) -0.0033(13) 0.0073(13) -0.0095(14) C10 0.0297(19) 0.0195(18) 0.0222(16) 0.0024(13) -0.0019(14) -0.0074(14) C11 0.0206(17) 0.0186(17) 0.0233(16) 0.0003(13) -0.0029(13) -0.0037(13) C12 0.0147(15) 0.0221(17) 0.0217(16) -0.0038(13) -0.0013(12) -0.0035(13) C13 0.0245(18) 0.0235(18) 0.0215(16) -0.0038(13) -0.0022(13) -0.0054(14) C14 0.0261(19) 0.035(2) 0.0237(17) 0.0029(15) 0.0006(14) -0.0033(16) C15 0.0197(18) 0.051(2) 0.0210(17) -0.0116(16) -0.0024(13) -0.0053(16) C16 0.0229(18) 0.035(2) 0.0314(19) -0.0190(16) -0.0011(14) -0.0066(15) C17 0.0196(17) 0.0209(18) 0.0273(17) -0.0030(13) 0.0021(13) -0.0053(14) C18 0.0152(15) 0.0198(17) 0.0188(15) 0.0010(12) -0.0015(12) -0.0044(13) C19 0.0105(15) 0.0199(17) 0.0228(16) -0.0013(12) -0.0013(12) -0.0018(12) C20 0.0247(18) 0.0260(19) 0.0183(15) 0.0013(13) 0.0052(13) -0.0071(14) C21 0.0273(18) 0.031(2) 0.0192(16) 0.0027(13) -0.0077(13) -0.0066(15) C22 0.0184(17) 0.031(2) 0.0264(17) -0.0005(14) -0.0066(13) -0.0037(14) C23 0.0163(16) 0.0233(18) 0.0192(15) -0.0016(13) 0.0007(12) -0.0046(13) C24 0.0127(15) 0.0254(18) 0.0185(15) 0.0030(12) -0.0009(12) -0.0037(13) C25 0.0181(16) 0.0269(19) 0.0175(15) 0.0001(13) -0.0020(12) -0.0043(14) C26 0.0251(18) 0.0244(19) 0.0311(18) 0.0042(14) -0.0081(14) -0.0120(15) C27 0.031(2) 0.040(2) 0.0253(18) 0.0105(15) -0.0013(14) -0.0189(17) C28 0.033(2) 0.047(2) 0.0186(17) -0.0012(15) 0.0064(14) -0.0139(18) C29 0.0248(18) 0.0273(19) 0.0221(16) -0.0009(14) -0.0014(13) -0.0105(15) C30 0.0124(16) 0.032(2) 0.0321(18) -0.0023(15) -0.0026(13) -0.0047(14) C31 0.0248(19) 0.039(2) 0.037(2) -0.0025(16) -0.0123(15) -0.0064(16) C32 0.0236(18) 0.030(2) 0.0327(19) -0.0037(15) 0.0024(14) -0.0085(15) C33 0.0146(17) 0.041(2) 0.049(2) -0.0030(18) 0.0018(16) -0.0005(16) C34 0.0230(17) 0.0251(18) 0.0179(15) -0.0049(13) -0.0026(13) -0.0016(14) C35 0.036(2) 0.039(2) 0.0193(17) 0.0003(15) -0.0019(14) -0.0021(17) C36 0.033(2) 0.030(2) 0.035(2) -0.0118(16) -0.0025(16) 0.0006(16) C37 0.0279(19) 0.030(2) 0.0294(18) -0.0095(15) -0.0088(15) -0.0028(15) C38 0.0282(18) 0.0199(18) 0.0218(16) 0.0035(13) -0.0011(13) -0.0038(14) C39 0.053(2) 0.032(2) 0.0238(18) 0.0060(15) 0.0030(16) -0.0054(18) C40 0.030(2) 0.024(2) 0.044(2) 0.0117(16) 0.0010(16) -0.0082(16) C41 0.033(2) 0.024(2) 0.040(2) 0.0093(15) -0.0084(16) -0.0018(16) C42 0.0168(15) 0.0176(16) 0.0110(13) 0.0017(11) 0.0005(11) -0.0060(12) C43 0.0208(16) 0.0203(17) 0.0139(14) -0.0002(12) 0.0002(12) -0.0041(13) C44 0.0246(18) 0.0226(18) 0.0243(17) -0.0047(13) -0.0011(13) 0.0000(14) C45 0.0222(19) 0.036(2) 0.048(2) -0.0129(18) 0.0027(16) 0.0041(16) C46 0.037(2) 0.025(2) 0.040(2) -0.0112(16) -0.0037(17) 0.0037(16) C47 0.0199(16) 0.0192(17) 0.0203(15) -0.0035(12) -0.0005(12) -0.0041(13) C48 0.0205(17) 0.0224(18) 0.0239(16) -0.0002(13) -0.0006(13) -0.0062(14) C49 0.0208(17) 0.0265(19) 0.0284(18) -0.0047(14) -0.0070(14) -0.0012(14) C50 0.034(2) 0.0257(19) 0.0181(15) -0.0015(13) -0.0087(14) -0.0024(15) C51 0.0286(19) 0.0220(18) 0.0187(16) -0.0010(13) 0.0013(13) -0.0039(14) C52 0.0147(16) 0.0193(17) 0.0246(16) -0.0032(13) -0.0013(12) -0.0027(13) C53 0.0156(16) 0.0265(18) 0.0197(15) 0.0012(13) -0.0026(12) -0.0055(13) C54 0.0224(18) 0.037(2) 0.0228(17) -0.0034(15) 0.0014(13) -0.0098(15) C55 0.028(2) 0.052(3) 0.0238(18) 0.0030(17) 0.0042(14) -0.0111(18) C56 0.0217(18) 0.039(2) 0.033(2) 0.0134(16) 0.0032(14) -0.0130(16) C57 0.0212(18) 0.0227(19) 0.0344(19) 0.0059(14) -0.0026(14) -0.0064(14) C58 0.0144(16) 0.0269(19) 0.0238(16) 0.0000(13) -0.0009(12) -0.0035(13) C59 0.0155(16) 0.0220(17) 0.0182(15) 0.0000(12) 0.0012(12) -0.0026(13) C60 0.0202(16) 0.0232(18) 0.0209(16) -0.0038(13) -0.0031(13) -0.0055(13) C61 0.0219(17) 0.030(2) 0.0217(16) 0.0030(14) -0.0029(13) -0.0047(14) C62 0.0187(17) 0.037(2) 0.0208(16) -0.0051(14) -0.0025(13) -0.0019(15) C63 0.0236(18) 0.0271(19) 0.0263(17) -0.0112(14) -0.0030(14) -0.0053(14) C64 0.0207(17) 0.0181(17) 0.0253(17) -0.0002(13) 0.0020(13) -0.0035(13) C65 0.0236(17) 0.0150(16) 0.0199(15) -0.0047(12) 0.0020(13) -0.0062(13) C66 0.0289(19) 0.0184(17) 0.0231(16) -0.0025(13) -0.0001(14) -0.0061(14) C67 0.029(2) 0.0206(18) 0.0324(19) -0.0079(14) 0.0090(15) -0.0071(15) C68 0.043(2) 0.024(2) 0.0275(18) -0.0013(15) 0.0132(16) -0.0128(17) C69 0.049(2) 0.0179(18) 0.0195(17) 0.0009(13) -0.0008(15) -0.0040(16) C70 0.0290(19) 0.0168(17) 0.0242(17) -0.0037(13) -0.0019(14) -0.0041(14) C71 0.0234(17) 0.0192(17) 0.0243(16) -0.0009(13) 0.0011(13) -0.0057(14) C72 0.0286(19) 0.0245(19) 0.0284(18) 0.0061(14) 0.0035(14) -0.0072(15) C73 0.0296(19) 0.0251(19) 0.0287(18) -0.0051(14) -0.0042(14) -0.0100(15) C74 0.035(2) 0.0193(19) 0.036(2) 0.0011(15) -0.0010(16) -0.0037(15) C75 0.0234(18) 0.0218(18) 0.0236(17) 0.0034(13) 0.0073(13) -0.0013(14) C76 0.037(2) 0.036(2) 0.0225(17) 0.0089(15) 0.0037(15) 0.0014(17) C77 0.029(2) 0.030(2) 0.0283(18) -0.0024(15) 0.0078(15) 0.0011(16) C78 0.034(2) 0.028(2) 0.048(2) 0.0044(17) 0.0136(17) -0.0073(17) C79 0.0278(19) 0.0253(19) 0.0307(18) -0.0019(14) -0.0136(15) -0.0015(15) C80 0.031(2) 0.032(2) 0.052(2) -0.0012(18) -0.0198(18) 0.0020(17) C81 0.034(2) 0.033(2) 0.047(2) -0.0107(18) -0.0239(18) -0.0011(17) C82 0.049(2) 0.043(2) 0.0226(18) 0.0018(16) -0.0143(17) -0.0003(19) B1 0.0195(18) 0.0163(19) 0.0175(16) -0.0003(13) 0.0011(13) -0.0030(14) B2 0.0118(17) 0.022(2) 0.0188(17) 0.0021(14) -0.0002(13) -0.0007(14) B3 0.0143(18) 0.024(2) 0.0169(17) -0.0008(14) 0.0010(13) -0.0016(15) B4 0.0220(19) 0.0152(19) 0.0180(17) -0.0010(13) -0.0011(14) -0.0013(14) Cl1 0.404(12) 0.190(7) 0.192(7) -0.033(5) -0.085(7) 0.177(8) Cl2 0.354(12) 0.132(5) 0.339(13) 0.093(7) 0.080(9) 0.086(6) Cl3 0.168(6) 0.209(7) 0.302(10) 0.090(7) -0.003(6) 0.021(5) Cl4 0.279(9) 0.213(7) 0.194(7) 0.009(6) -0.014(6) 0.100(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 P1 C30 1.877(3) . ? P1 C38 1.885(3) . ? P1 C34 1.889(3) . ? P1 C1 1.894(3) . ? P2 C71 1.884(3) . ? P2 C75 1.887(3) . ? P2 C79 1.888(3) . ? P2 C42 1.897(3) . ? F1 C7 1.353(3) . ? F2 C8 1.342(3) . ? F3 C9 1.343(4) . ? F4 C10 1.347(4) . ? F5 C11 1.345(3) . ? F6 C13 1.358(4) . ? F7 C14 1.347(4) . ? F8 C15 1.342(4) . ? F9 C16 1.347(4) . ? F10 C17 1.358(4) . ? F11 C19 1.364(3) . ? F12 C20 1.341(3) . ? F13 C21 1.348(3) . ? F14 C22 1.345(3) . ? F15 C23 1.354(3) . ? F16 C25 1.358(3) . ? F17 C26 1.341(4) . ? F18 C27 1.344(4) . ? F19 C28 1.347(4) . ? F20 C29 1.343(4) . ? F21 C48 1.351(4) . ? F22 C49 1.347(4) . ? F23 C50 1.335(3) . ? F24 C51 1.352(4) . ? F25 C52 1.353(3) . ? F26 C54 1.344(4) . ? F27 C55 1.351(4) . ? F28 C56 1.346(4) . ? F29 C57 1.344(4) . ? F30 C58 1.356(3) . ? F31 C60 1.368(3) . ? F32 C61 1.346(4) . ? F33 C62 1.338(3) . ? F34 C63 1.351(4) . ? F35 C64 1.354(4) . ? F36 C66 1.346(4) . ? F37 C67 1.341(4) . ? F38 C68 1.341(4) . ? F39 C69 1.349(4) . ? F40 C70 1.347(4) . ? O1 C1 1.250(3) . ? O1 B1 1.668(4) . ? O2 C1 1.256(3) . ? O2 B2 1.643(4) . ? O3 C42 1.249(3) . ? O3 B3 1.675(4) . ? O4 C42 1.257(3) . ? O4 B4 1.650(4) . ? C2 C3 1.344(4) . ? C2 B1 1.597(5) . ? C2 B2 1.605(5) . ? C3 C4 1.511(5) . ? C3 C5 1.516(4) . ? C6 C11 1.390(4) . ? C6 C7 1.396(4) . ? C6 B1 1.644(5) . ? C7 C8 1.378(4) . ? C8 C9 1.378(4) . ? C9 C10 1.373(4) . ? C10 C11 1.381(4) . ? C12 C13 1.378(4) . ? C12 C17 1.386(4) . ? C12 B1 1.645(4) . ? C13 C14 1.385(4) . ? C14 C15 1.362(5) . ? C15 C16 1.371(5) . ? C16 C17 1.388(5) . ? C18 C19 1.383(4) . ? C18 C23 1.391(4) . ? C18 B2 1.642(4) . ? C19 C20 1.380(4) . ? C20 C21 1.375(4) . ? C21 C22 1.373(5) . ? C22 C23 1.385(4) . ? C24 C25 1.392(4) . ? C24 C29 1.393(4) . ? C24 B2 1.646(5) . ? C25 C26 1.379(4) . ? C26 C27 1.379(5) . ? C27 C28 1.367(5) . ? C28 C29 1.380(5) . ? C30 C33 1.546(5) . ? C30 C32 1.546(5) . ? C30 C31 1.547(5) . ? C34 C35 1.537(5) . ? C34 C37 1.539(4) . ? C34 C36 1.539(5) . ? C38 C41 1.532(4) . ? C38 C39 1.537(5) . ? C38 C40 1.545(5) . ? C43 C44 1.342(4) . ? C43 B3 1.596(5) . ? C43 B4 1.603(5) . ? C44 C45 1.513(5) . ? C44 C46 1.519(5) . ? C47 C48 1.387(4) . ? C47 C52 1.388(4) . ? C47 B3 1.644(4) . ? C48 C49 1.389(4) . ? C49 C50 1.373(5) . ? C50 C51 1.372(5) . ? C51 C52 1.382(4) . ? C53 C54 1.387(4) . ? C53 C58 1.391(4) . ? C53 B3 1.646(5) . ? C54 C55 1.391(5) . ? C55 C56 1.365(5) . ? C56 C57 1.369(5) . ? C57 C58 1.378(4) . ? C59 C60 1.378(4) . ? C59 C64 1.386(4) . ? C59 B4 1.647(4) . ? C60 C61 1.381(4) . ? C61 C62 1.377(5) . ? C62 C63 1.373(5) . ? C63 C64 1.378(4) . ? C65 C66 1.389(4) . ? C65 C70 1.394(4) . ? C65 B4 1.646(5) . ? C66 C67 1.377(5) . ? C67 C68 1.374(5) . ? C68 C69 1.372(5) . ? C69 C70 1.382(5) . ? C71 C74 1.537(4) . ? C71 C72 1.542(4) . ? C71 C73 1.544(4) . ? C75 C78 1.526(5) . ? C75 C77 1.536(4) . ? C75 C76 1.547(5) . ? C79 C82 1.533(5) . ? C79 C80 1.551(5) . ? C79 C81 1.554(5) . ? C83 C83 1.61(2) 2_685 ? C83 Cl2 1.704(9) . ? C83 Cl1 1.715(9) . ? C84 Cl3 1.684(10) . ? C84 Cl4 1.733(10) . ? C84 C84 1.79(4) 2_656 ? Cl1 Cl2 2.145(14) . ? Cl3 Cl4 2.380(13) . ? 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 C30 P1 C38 114.12(15) . . ? C30 P1 C34 112.01(15) . . ? C38 P1 C34 112.21(15) . . ? C30 P1 C1 105.50(14) . . ? C38 P1 C1 103.38(13) . . ? C34 P1 C1 108.90(13) . . ? C71 P2 C75 113.60(14) . . ? C71 P2 C79 111.07(15) . . ? C75 P2 C79 113.00(15) . . ? C71 P2 C42 106.83(14) . . ? C75 P2 C42 102.62(13) . . ? C79 P2 C42 109.12(13) . . ? C1 O1 B1 125.5(2) . . ? C1 O2 B2 124.7(2) . . ? C42 O3 B3 124.6(2) . . ? C42 O4 B4 125.2(2) . . ? O1 C1 O2 128.0(3) . . ? O1 C1 P1 117.9(2) . . ? O2 C1 P1 114.1(2) . . ? C3 C2 B1 119.1(3) . . ? C3 C2 B2 119.9(3) . . ? B1 C2 B2 121.0(3) . . ? C2 C3 C4 124.4(3) . . ? C2 C3 C5 124.6(3) . . ? C4 C3 C5 111.0(3) . . ? C11 C6 C7 113.4(3) . . ? C11 C6 B1 126.4(3) . . ? C7 C6 B1 120.0(3) . . ? F1 C7 C8 115.9(3) . . ? F1 C7 C6 119.2(3) . . ? C8 C7 C6 124.9(3) . . ? F2 C8 C7 121.2(3) . . ? F2 C8 C9 120.0(3) . . ? C7 C8 C9 118.8(3) . . ? F3 C9 C10 121.0(3) . . ? F3 C9 C8 119.9(3) . . ? C10 C9 C8 119.1(3) . . ? F4 C10 C9 119.6(3) . . ? F4 C10 C11 120.1(3) . . ? C9 C10 C11 120.3(3) . . ? F5 C11 C10 115.0(3) . . ? F5 C11 C6 121.5(3) . . ? C10 C11 C6 123.5(3) . . ? C13 C12 C17 112.9(3) . . ? C13 C12 B1 120.0(3) . . ? C17 C12 B1 127.0(3) . . ? F6 C13 C12 119.5(3) . . ? F6 C13 C14 115.9(3) . . ? C12 C13 C14 124.7(3) . . ? F7 C14 C15 119.9(3) . . ? F7 C14 C13 120.4(3) . . ? C15 C14 C13 119.7(3) . . ? F8 C15 C14 120.3(3) . . ? F8 C15 C16 120.9(3) . . ? C14 C15 C16 118.8(3) . . ? F9 C16 C15 120.4(3) . . ? F9 C16 C17 120.2(3) . . ? C15 C16 C17 119.4(3) . . ? F10 C17 C12 120.6(3) . . ? F10 C17 C16 115.0(3) . . ? C12 C17 C16 124.4(3) . . ? C19 C18 C23 113.0(3) . . ? C19 C18 B2 120.1(3) . . ? C23 C18 B2 126.7(3) . . ? F11 C19 C20 115.0(3) . . ? F11 C19 C18 119.7(3) . . ? C20 C19 C18 125.3(3) . . ? F12 C20 C21 120.0(3) . . ? F12 C20 C19 121.3(3) . . ? C21 C20 C19 118.7(3) . . ? F13 C21 C22 120.2(3) . . ? F13 C21 C20 120.3(3) . . ? C22 C21 C20 119.5(3) . . ? F14 C22 C21 119.8(3) . . ? F14 C22 C23 120.8(3) . . ? C21 C22 C23 119.3(3) . . ? F15 C23 C22 115.4(3) . . ? F15 C23 C18 120.4(3) . . ? C22 C23 C18 124.2(3) . . ? C25 C24 C29 113.5(3) . . ? C25 C24 B2 119.9(3) . . ? C29 C24 B2 126.5(3) . . ? F16 C25 C26 115.6(3) . . ? F16 C25 C24 119.5(3) . . ? C26 C25 C24 124.8(3) . . ? F17 C26 C27 120.2(3) . . ? F17 C26 C25 121.0(3) . . ? C27 C26 C25 118.7(3) . . ? F18 C27 C28 121.0(3) . . ? F18 C27 C26 119.9(3) . . ? C28 C27 C26 119.1(3) . . ? F19 C28 C27 119.2(3) . . ? F19 C28 C29 120.2(3) . . ? C27 C28 C29 120.5(3) . . ? F20 C29 C28 115.0(3) . . ? F20 C29 C24 121.7(3) . . ? C28 C29 C24 123.3(3) . . ? C33 C30 C32 107.5(3) . . ? C33 C30 C31 108.1(3) . . ? C32 C30 C31 109.0(3) . . ? C33 C30 P1 112.1(2) . . ? C32 C30 P1 109.5(2) . . ? C31 C30 P1 110.5(2) . . ? C35 C34 C37 106.5(3) . . ? C35 C34 C36 108.9(3) . . ? C37 C34 C36 108.8(3) . . ? C35 C34 P1 111.8(2) . . ? C37 C34 P1 112.6(2) . . ? C36 C34 P1 108.0(2) . . ? C41 C38 C39 109.7(3) . . ? C41 C38 C40 108.9(3) . . ? C39 C38 C40 106.1(3) . . ? C41 C38 P1 111.2(2) . . ? C39 C38 P1 108.8(2) . . ? C40 C38 P1 111.9(2) . . ? O3 C42 O4 128.2(3) . . ? O3 C42 P2 118.0(2) . . ? O4 C42 P2 113.7(2) . . ? C44 C43 B3 119.1(3) . . ? C44 C43 B4 119.4(3) . . ? B3 C43 B4 121.4(3) . . ? C43 C44 C45 124.8(3) . . ? C43 C44 C46 124.2(3) . . ? C45 C44 C46 111.0(3) . . ? C48 C47 C52 113.3(3) . . ? C48 C47 B3 127.0(3) . . ? C52 C47 B3 119.1(3) . . ? F21 C48 C47 121.0(3) . . ? F21 C48 C49 115.4(3) . . ? C47 C48 C49 123.7(3) . . ? F22 C49 C50 119.0(3) . . ? F22 C49 C48 120.7(3) . . ? C50 C49 C48 120.3(3) . . ? F23 C50 C51 121.1(3) . . ? F23 C50 C49 120.4(3) . . ? C51 C50 C49 118.4(3) . . ? F24 C51 C50 120.0(3) . . ? F24 C51 C52 120.3(3) . . ? C50 C51 C52 119.7(3) . . ? F25 C52 C51 115.8(3) . . ? F25 C52 C47 119.5(3) . . ? C51 C52 C47 124.6(3) . . ? C54 C53 C58 113.5(3) . . ? C54 C53 B3 126.7(3) . . ? C58 C53 B3 119.6(3) . . ? F26 C54 C53 121.9(3) . . ? F26 C54 C55 115.0(3) . . ? C53 C54 C55 123.0(3) . . ? F27 C55 C56 119.6(3) . . ? F27 C55 C54 120.0(3) . . ? C56 C55 C54 120.4(3) . . ? F28 C56 C55 120.6(3) . . ? F28 C56 C57 120.2(3) . . ? C55 C56 C57 119.2(3) . . ? F29 C57 C56 120.6(3) . . ? F29 C57 C58 120.6(3) . . ? C56 C57 C58 118.9(3) . . ? F30 C58 C57 115.6(3) . . ? F30 C58 C53 119.4(3) . . ? C57 C58 C53 125.0(3) . . ? C60 C59 C64 113.3(3) . . ? C60 C59 B4 119.6(3) . . ? C64 C59 B4 127.1(3) . . ? F31 C60 C59 119.9(3) . . ? F31 C60 C61 115.2(3) . . ? C59 C60 C61 124.9(3) . . ? F32 C61 C62 119.7(3) . . ? F32 C61 C60 121.1(3) . . ? C62 C61 C60 119.1(3) . . ? F33 C62 C63 120.9(3) . . ? F33 C62 C61 120.5(3) . . ? C63 C62 C61 118.5(3) . . ? F34 C63 C62 119.7(3) . . ? F34 C63 C64 120.3(3) . . ? C62 C63 C64 120.0(3) . . ? F35 C64 C63 115.4(3) . . ? F35 C64 C59 120.6(3) . . ? C63 C64 C59 124.0(3) . . ? C66 C65 C70 113.2(3) . . ? C66 C65 B4 119.8(3) . . ? C70 C65 B4 126.7(3) . . ? F36 C66 C67 115.6(3) . . ? F36 C66 C65 119.4(3) . . ? C67 C66 C65 125.0(3) . . ? F37 C67 C68 119.8(3) . . ? F37 C67 C66 121.1(3) . . ? C68 C67 C66 119.1(3) . . ? F38 C68 C69 120.5(3) . . ? F38 C68 C67 120.6(3) . . ? C69 C68 C67 118.9(3) . . ? F39 C69 C68 119.9(3) . . ? F39 C69 C70 119.9(3) . . ? C68 C69 C70 120.2(3) . . ? F40 C70 C69 115.1(3) . . ? F40 C70 C65 121.4(3) . . ? C69 C70 C65 123.5(3) . . ? C74 C71 C72 108.1(3) . . ? C74 C71 C73 108.5(3) . . ? C72 C71 C73 108.5(3) . . ? C74 C71 P2 110.7(2) . . ? C72 C71 P2 110.8(2) . . ? C73 C71 P2 110.1(2) . . ? C78 C75 C77 109.8(3) . . ? C78 C75 C76 107.1(3) . . ? C77 C75 C76 108.3(3) . . ? C78 C75 P2 110.2(2) . . ? C77 C75 P2 111.9(2) . . ? C76 C75 P2 109.5(2) . . ? C82 C79 C80 109.9(3) . . ? C82 C79 C81 107.3(3) . . ? C80 C79 C81 107.0(3) . . ? C82 C79 P2 110.9(2) . . ? C80 C79 P2 108.5(2) . . ? C81 C79 P2 113.2(2) . . ? C2 B1 C6 121.0(3) . . ? C2 B1 C12 111.5(2) . . ? C6 B1 C12 113.1(3) . . ? C2 B1 O1 109.4(2) . . ? C6 B1 O1 96.8(2) . . ? C12 B1 O1 102.1(2) . . ? C2 B2 C18 109.1(2) . . ? C2 B2 O2 110.9(2) . . ? C18 B2 O2 101.1(2) . . ? C2 B2 C24 120.2(3) . . ? C18 B2 C24 115.2(3) . . ? O2 B2 C24 98.0(2) . . ? C43 B3 C47 109.9(3) . . ? C43 B3 C53 120.7(3) . . ? C47 B3 C53 114.2(3) . . ? C43 B3 O3 109.8(2) . . ? C47 B3 O3 103.3(2) . . ? C53 B3 O3 96.7(2) . . ? C43 B4 C65 120.8(3) . . ? C43 B4 C59 110.0(2) . . ? C65 B4 C59 115.0(3) . . ? C43 B4 O4 110.2(2) . . ? C65 B4 O4 97.3(2) . . ? C59 B4 O4 100.8(2) . . ? C83 C83 Cl2 116.2(12) 2_685 . ? C83 C83 Cl1 163.8(15) 2_685 . ? Cl2 C83 Cl1 77.7(7) . . ? Cl3 C84 Cl4 88.3(8) . . ? Cl3 C84 C84 107.5(14) . 2_656 ? Cl4 C84 C84 148(3) . 2_656 ? C83 Cl1 Cl2 50.9(4) . . ? C83 Cl2 Cl1 51.4(4) . . ? C84 Cl3 Cl4 46.7(5) . . ? C84 Cl4 Cl3 45.0(4) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.046 _refine_diff_density_min -0.973 _refine_diff_density_rms 0.088 #===end