# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Kehr, Gerald' 'Frohlich, Roland' 'Erker, G' 'Ekkert, Olga' _publ_contact_author_name 'Dr Gerald Kehr' _publ_contact_author_email kehrald@uni-muenster.de _publ_section_title ; Phosphirenium Borate Zwitterion: Formation in the 1,1 Carboboration Reaction of Phosphinylalkynes ; # Attachment '- 3c.cif' data_erk5812 _database_code_depnum_ccdc_archive 'CCDC 826907' #TrackingRef '- 3c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H29 P' _chemical_formula_weight 384.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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 10.1751(5) _cell_length_b 10.6783(4) _cell_length_c 11.6493(7) _cell_angle_alpha 96.462(2) _cell_angle_beta 107.570(4) _cell_angle_gamma 109.165(4) _cell_volume 1107.87(10) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3486 _cell_measurement_theta_min 0.88 _cell_measurement_theta_max 68.25 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.153 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 412 _exptl_absorpt_coefficient_mu 1.142 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7633 _exptl_absorpt_correction_T_max 0.9451 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15949 _diffrn_reflns_av_R_equivalents 0.048 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.10 _diffrn_reflns_theta_max 66.89 _reflns_number_total 3784 _reflns_number_gt 3388 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0665P)^2^+0.4553P] 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 3784 _refine_ls_number_parameters 260 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1227 _refine_ls_wR_factor_gt 0.1178 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 0.31544(5) 0.63889(5) 0.17816(4) 0.03461(16) Uani 1 1 d . . . C1 C 0.4790(2) 0.66526(19) 0.30368(17) 0.0397(4) Uani 1 1 d . . . C2 C 0.5900(2) 0.6579(2) 0.37232(17) 0.0404(4) Uani 1 1 d . . . C3 C 0.7278(2) 0.65474(18) 0.44971(16) 0.0373(4) Uani 1 1 d . . . C4 C 0.8574(2) 0.7122(2) 0.42527(18) 0.0448(5) Uani 1 1 d . . . H4 H 0.8549 0.7554 0.3591 0.054 Uiso 1 1 calc R . . C5 C 0.9896(2) 0.7064(2) 0.49711(18) 0.0471(5) Uani 1 1 d . . . H5 H 1.0759 0.7454 0.4787 0.057 Uiso 1 1 calc R . . C6 C 0.9981(2) 0.64450(19) 0.59583(17) 0.0408(4) Uani 1 1 d . . . C7 C 0.8691(2) 0.5866(2) 0.61995(17) 0.0436(5) Uani 1 1 d . . . H7 H 0.8725 0.5436 0.6863 0.052 Uiso 1 1 calc R . . C8 C 0.7353(2) 0.5907(2) 0.54844(17) 0.0421(4) Uani 1 1 d . . . H8 H 0.6489 0.5503 0.5663 0.051 Uiso 1 1 calc R . . C9 C 1.1442(2) 0.6413(2) 0.6742(2) 0.0550(5) Uani 1 1 d . . . H9A H 1.2061 0.7298 0.7306 0.082 Uiso 1 1 calc R . . H9B H 1.1950 0.6197 0.6212 0.082 Uiso 1 1 calc R . . H9C H 1.1257 0.5724 0.7213 0.082 Uiso 1 1 calc R . . C11 C 0.40683(19) 0.68960(18) 0.06647(15) 0.0333(4) Uani 1 1 d . . . C12 C 0.5136(2) 0.82120(18) 0.08397(17) 0.0369(4) Uani 1 1 d . . . C13 C 0.5785(2) 0.8470(2) -0.00457(18) 0.0435(5) Uani 1 1 d . . . H13 H 0.6479 0.9351 0.0061 0.052 Uiso 1 1 calc R . . C14 C 0.5447(2) 0.7474(2) -0.10800(18) 0.0459(5) Uani 1 1 d . . . C15 C 0.4422(2) 0.6191(2) -0.12232(17) 0.0426(4) Uani 1 1 d . . . H15 H 0.4192 0.5503 -0.1915 0.051 Uiso 1 1 calc R . . C16 C 0.3716(2) 0.58753(18) -0.03790(16) 0.0362(4) Uani 1 1 d . . . C17 C 0.5624(2) 0.9353(2) 0.19563(19) 0.0478(5) Uani 1 1 d . . . H17A H 0.6305 1.0182 0.1862 0.072 Uiso 1 1 calc R . . H17B H 0.6123 0.9110 0.2696 0.072 Uiso 1 1 calc R . . H17C H 0.4758 0.9500 0.2028 0.072 Uiso 1 1 calc R . . C18 C 0.6188(3) 0.7766(3) -0.2020(2) 0.0717(7) Uani 1 1 d . . . H18A H 0.7007 0.7455 -0.1850 0.108 Uiso 1 1 calc R . . H18B H 0.6566 0.8739 -0.1967 0.108 Uiso 1 1 calc R . . H18C H 0.5466 0.7290 -0.2845 0.108 Uiso 1 1 calc R . . C19 C 0.2585(2) 0.44436(19) -0.06568(18) 0.0458(5) Uani 1 1 d . . . H19A H 0.2626 0.4162 0.0112 0.069 Uiso 1 1 calc R . . H19B H 0.2807 0.3829 -0.1178 0.069 Uiso 1 1 calc R . . H19C H 0.1594 0.4419 -0.1083 0.069 Uiso 1 1 calc R . . C21 C 0.24189(19) 0.76990(18) 0.21331(16) 0.0343(4) Uani 1 1 d . . . C22 C 0.1342(2) 0.78320(19) 0.11065(17) 0.0390(4) Uani 1 1 d . . . C23 C 0.0610(2) 0.8683(2) 0.12914(19) 0.0446(5) Uani 1 1 d . . . H23 H -0.0101 0.8764 0.0601 0.053 Uiso 1 1 calc R . . C24 C 0.0887(2) 0.9415(2) 0.2452(2) 0.0449(5) Uani 1 1 d . . . C25 C 0.1925(2) 0.9258(2) 0.34480(19) 0.0440(5) Uani 1 1 d . . . H25 H 0.2130 0.9751 0.4245 0.053 Uiso 1 1 calc R . . C26 C 0.2684(2) 0.84070(19) 0.33302(17) 0.0381(4) Uani 1 1 d . . . C27 C 0.0923(2) 0.7069(2) -0.02001(18) 0.0520(5) Uani 1 1 d . . . H27A H -0.0011 0.7094 -0.0718 0.078 Uiso 1 1 calc R . . H27B H 0.0809 0.6129 -0.0211 0.078 Uiso 1 1 calc R . . H27C H 0.1700 0.7492 -0.0514 0.078 Uiso 1 1 calc R . . C28 C 0.0076(3) 1.0335(3) 0.2623(3) 0.0658(7) Uani 1 1 d . . . H28A H -0.0061 1.0341 0.3412 0.099 Uiso 1 1 calc R . . H28B H -0.0889 1.0003 0.1958 0.099 Uiso 1 1 calc R . . H28C H 0.0658 1.1254 0.2610 0.099 Uiso 1 1 calc R . . C29 C 0.3707(2) 0.8255(2) 0.45036(17) 0.0479(5) Uani 1 1 d . . . H29A H 0.3664 0.8784 0.5216 0.072 Uiso 1 1 calc R . . H29B H 0.4721 0.8583 0.4516 0.072 Uiso 1 1 calc R . . H29C H 0.3392 0.7302 0.4533 0.072 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 P1 0.0333(3) 0.0372(3) 0.0346(3) 0.00980(19) 0.01247(19) 0.0145(2) C1 0.0434(11) 0.0440(10) 0.0384(10) 0.0127(8) 0.0166(8) 0.0222(9) C2 0.0455(11) 0.0462(11) 0.0356(9) 0.0107(8) 0.0155(8) 0.0240(9) C3 0.0407(10) 0.0412(10) 0.0328(9) 0.0078(8) 0.0115(8) 0.0211(8) C4 0.0490(11) 0.0529(12) 0.0400(10) 0.0194(9) 0.0188(9) 0.0235(10) C5 0.0421(11) 0.0585(12) 0.0466(11) 0.0156(9) 0.0206(9) 0.0213(10) C6 0.0422(11) 0.0428(10) 0.0364(10) 0.0033(8) 0.0092(8) 0.0216(9) C7 0.0493(11) 0.0471(11) 0.0351(10) 0.0159(8) 0.0127(8) 0.0197(9) C8 0.0403(10) 0.0487(11) 0.0396(10) 0.0141(8) 0.0162(8) 0.0169(9) C9 0.0484(12) 0.0659(14) 0.0486(12) 0.0073(10) 0.0067(10) 0.0312(11) C11 0.0309(9) 0.0392(9) 0.0337(9) 0.0113(7) 0.0110(7) 0.0180(8) C12 0.0337(9) 0.0390(10) 0.0398(10) 0.0116(8) 0.0115(8) 0.0171(8) C13 0.0406(10) 0.0444(11) 0.0508(11) 0.0185(9) 0.0198(9) 0.0172(9) C14 0.0446(11) 0.0598(13) 0.0454(11) 0.0204(9) 0.0225(9) 0.0266(10) C15 0.0439(11) 0.0536(12) 0.0372(10) 0.0095(8) 0.0144(8) 0.0280(10) C16 0.0344(9) 0.0415(10) 0.0353(9) 0.0101(8) 0.0086(7) 0.0209(8) C17 0.0473(11) 0.0394(10) 0.0521(12) 0.0078(9) 0.0192(9) 0.0107(9) C18 0.0823(18) 0.0869(18) 0.0655(15) 0.0268(14) 0.0491(14) 0.0332(15) C19 0.0469(11) 0.0404(10) 0.0442(11) 0.0020(8) 0.0124(9) 0.0155(9) C21 0.0291(9) 0.0369(9) 0.0380(9) 0.0090(7) 0.0142(7) 0.0122(7) C22 0.0331(9) 0.0423(10) 0.0410(10) 0.0096(8) 0.0131(8) 0.0141(8) C23 0.0355(10) 0.0462(11) 0.0523(12) 0.0149(9) 0.0128(8) 0.0176(9) C24 0.0388(11) 0.0403(10) 0.0593(12) 0.0116(9) 0.0212(9) 0.0167(9) C25 0.0445(11) 0.0408(10) 0.0465(11) 0.0036(8) 0.0218(9) 0.0133(9) C26 0.0339(9) 0.0399(10) 0.0409(10) 0.0092(8) 0.0162(8) 0.0121(8) C27 0.0467(12) 0.0691(14) 0.0401(11) 0.0096(10) 0.0063(9) 0.0317(11) C28 0.0634(15) 0.0611(14) 0.0816(17) 0.0082(12) 0.0262(13) 0.0371(12) C29 0.0518(12) 0.0579(12) 0.0348(10) 0.0057(9) 0.0139(9) 0.0251(10) _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 1.7657(19) . ? P1 C11 1.8464(17) . ? P1 C21 1.8515(18) . ? C1 C2 1.204(3) . ? C2 C3 1.433(3) . ? C3 C4 1.390(3) . ? C3 C8 1.398(3) . ? C4 C5 1.379(3) . ? C4 H4 0.9400 . ? C5 C6 1.384(3) . ? C5 H5 0.9400 . ? C6 C7 1.383(3) . ? C6 C9 1.505(3) . ? C7 C8 1.383(3) . ? C7 H7 0.9400 . ? C8 H8 0.9400 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C11 C16 1.406(2) . ? C11 C12 1.413(3) . ? C12 C13 1.390(3) . ? C12 C17 1.509(3) . ? C13 C14 1.386(3) . ? C13 H13 0.9400 . ? C14 C15 1.378(3) . ? C14 C18 1.512(3) . ? C15 C16 1.393(3) . ? C15 H15 0.9400 . ? C16 C19 1.508(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C21 C26 1.411(3) . ? C21 C22 1.414(2) . ? C22 C23 1.388(3) . ? C22 C27 1.504(3) . ? C23 C24 1.380(3) . ? C23 H23 0.9400 . ? C24 C25 1.383(3) . ? C24 C28 1.507(3) . ? C25 C26 1.392(3) . ? C25 H25 0.9400 . ? C26 C29 1.510(3) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? 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 C11 96.85(8) . . ? C1 P1 C21 109.04(8) . . ? C11 P1 C21 106.90(8) . . ? C2 C1 P1 165.01(17) . . ? C1 C2 C3 176.1(2) . . ? C4 C3 C8 118.20(17) . . ? C4 C3 C2 120.19(17) . . ? C8 C3 C2 121.57(17) . . ? C5 C4 C3 120.65(18) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 121.40(19) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C7 C6 C5 118.08(17) . . ? C7 C6 C9 121.44(18) . . ? C5 C6 C9 120.48(19) . . ? C6 C7 C8 121.33(17) . . ? C6 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? C7 C8 C3 120.33(18) . . ? C7 C8 H8 119.8 . . ? C3 C8 H8 119.8 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C16 C11 C12 119.47(16) . . ? C16 C11 P1 116.78(13) . . ? C12 C11 P1 123.67(13) . . ? C13 C12 C11 118.79(17) . . ? C13 C12 C17 118.16(17) . . ? C11 C12 C17 123.04(16) . . ? C14 C13 C12 122.35(18) . . ? C14 C13 H13 118.8 . . ? C12 C13 H13 118.8 . . ? C15 C14 C13 117.98(18) . . ? C15 C14 C18 120.4(2) . . ? C13 C14 C18 121.6(2) . . ? C14 C15 C16 122.35(18) . . ? C14 C15 H15 118.8 . . ? C16 C15 H15 118.8 . . ? C15 C16 C11 119.03(17) . . ? C15 C16 C19 117.32(17) . . ? C11 C16 C19 123.64(17) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C26 C21 C22 118.71(16) . . ? C26 C21 P1 125.48(14) . . ? C22 C21 P1 115.17(13) . . ? C23 C22 C21 119.64(17) . . ? C23 C22 C27 117.41(17) . . ? C21 C22 C27 122.94(16) . . ? C24 C23 C22 122.45(18) . . ? C24 C23 H23 118.8 . . ? C22 C23 H23 118.8 . . ? C23 C24 C25 117.22(17) . . ? C23 C24 C28 121.3(2) . . ? C25 C24 C28 121.53(19) . . ? C24 C25 C26 123.29(18) . . ? C24 C25 H25 118.4 . . ? C26 C25 H25 118.4 . . ? C25 C26 C21 118.64(17) . . ? C25 C26 C29 117.70(16) . . ? C21 C26 C29 123.63(16) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 P1 C1 C2 -68.9(7) . . . . ? C21 P1 C1 C2 -179.4(7) . . . . ? P1 C1 C2 C3 86(3) . . . . ? C1 C2 C3 C4 -5(3) . . . . ? C1 C2 C3 C8 177(3) . . . . ? C8 C3 C4 C5 -0.3(3) . . . . ? C2 C3 C4 C5 -178.23(18) . . . . ? C3 C4 C5 C6 -0.4(3) . . . . ? C4 C5 C6 C7 0.8(3) . . . . ? C4 C5 C6 C9 -179.06(19) . . . . ? C5 C6 C7 C8 -0.4(3) . . . . ? C9 C6 C7 C8 179.43(18) . . . . ? C6 C7 C8 C3 -0.3(3) . . . . ? C4 C3 C8 C7 0.6(3) . . . . ? C2 C3 C8 C7 178.56(17) . . . . ? C1 P1 C11 C16 115.08(14) . . . . ? C21 P1 C11 C16 -132.59(13) . . . . ? C1 P1 C11 C12 -61.65(16) . . . . ? C21 P1 C11 C12 50.68(16) . . . . ? C16 C11 C12 C13 1.5(2) . . . . ? P1 C11 C12 C13 178.13(13) . . . . ? C16 C11 C12 C17 -177.64(16) . . . . ? P1 C11 C12 C17 -1.0(2) . . . . ? C11 C12 C13 C14 -1.4(3) . . . . ? C17 C12 C13 C14 177.74(18) . . . . ? C12 C13 C14 C15 0.3(3) . . . . ? C12 C13 C14 C18 -178.71(19) . . . . ? C13 C14 C15 C16 0.8(3) . . . . ? C18 C14 C15 C16 179.81(19) . . . . ? C14 C15 C16 C11 -0.7(3) . . . . ? C14 C15 C16 C19 178.38(17) . . . . ? C12 C11 C16 C15 -0.5(2) . . . . ? P1 C11 C16 C15 -177.34(13) . . . . ? C12 C11 C16 C19 -179.47(16) . . . . ? P1 C11 C16 C19 3.7(2) . . . . ? C1 P1 C21 C26 -24.43(18) . . . . ? C11 P1 C21 C26 -128.13(16) . . . . ? C1 P1 C21 C22 164.93(13) . . . . ? C11 P1 C21 C22 61.24(15) . . . . ? C26 C21 C22 C23 2.1(3) . . . . ? P1 C21 C22 C23 173.38(14) . . . . ? C26 C21 C22 C27 -176.97(18) . . . . ? P1 C21 C22 C27 -5.7(2) . . . . ? C21 C22 C23 C24 -0.1(3) . . . . ? C27 C22 C23 C24 178.94(19) . . . . ? C22 C23 C24 C25 -0.8(3) . . . . ? C22 C23 C24 C28 179.8(2) . . . . ? C23 C24 C25 C26 -0.2(3) . . . . ? C28 C24 C25 C26 179.19(19) . . . . ? C24 C25 C26 C21 2.1(3) . . . . ? C24 C25 C26 C29 -175.74(18) . . . . ? C22 C21 C26 C25 -3.0(3) . . . . ? P1 C21 C26 C25 -173.29(14) . . . . ? C22 C21 C26 C29 174.71(18) . . . . ? P1 C21 C26 C29 4.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 66.89 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.223 _refine_diff_density_min -0.235 _refine_diff_density_rms 0.043 # Attachment '- 4c.cif' data_erk5924 _database_code_depnum_ccdc_archive 'CCDC 826908' #TrackingRef '- 4c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H29 B F15 P' _chemical_formula_weight 896.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 12.4342(5) _cell_length_b 13.4995(6) _cell_length_c 14.2303(6) _cell_angle_alpha 82.805(2) _cell_angle_beta 66.678(2) _cell_angle_gamma 64.037(2) _cell_volume 1968.75(14) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6212 _cell_measurement_theta_min 0.88 _cell_measurement_theta_max 68.25 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 1.570 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7442 _exptl_absorpt_correction_T_max 0.9256 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28030 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 66.95 _reflns_number_total 6739 _reflns_number_gt 6261 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0623P)^2^+0.6806P] 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 6739 _refine_ls_number_parameters 566 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.1086 _refine_ls_wR_factor_gt 0.1059 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 0.02529(4) 0.63527(3) 0.21497(3) 0.03249(12) Uani 1 1 d . . . B1 B 0.01652(18) 0.77396(15) 0.27467(14) 0.0353(4) Uani 1 1 d . . . C1 C 0.11321(15) 0.76876(13) 0.15542(12) 0.0350(3) Uani 1 1 d . . . C2 C 0.12562(15) 0.68338(13) 0.10500(12) 0.0355(3) Uani 1 1 d . . . C3 C 0.20252(15) 0.64383(14) -0.00364(12) 0.0382(4) Uani 1 1 d . . . C4 C 0.27599(17) 0.53273(15) -0.03399(14) 0.0446(4) Uani 1 1 d . . . H4 H 0.2749 0.4797 0.0155 0.054 Uiso 1 1 calc R . . C5 C 0.35095(18) 0.49900(17) -0.13640(15) 0.0518(5) Uani 1 1 d . . . H5 H 0.4014 0.4232 -0.1550 0.062 Uiso 1 1 calc R . . C6 C 0.35346(17) 0.57408(19) -0.21207(14) 0.0520(5) Uani 1 1 d . . . C7 C 0.27861(19) 0.68547(18) -0.18198(14) 0.0523(5) Uani 1 1 d . . . H7 H 0.2785 0.7381 -0.2319 0.063 Uiso 1 1 calc R . . C8 C 0.20418(18) 0.72036(16) -0.07984(13) 0.0451(4) Uani 1 1 d . . . H8 H 0.1542 0.7962 -0.0614 0.054 Uiso 1 1 calc R . . C9 C 0.4327(2) 0.5362(3) -0.32384(16) 0.0737(7) Uani 1 1 d . . . H9A H 0.5054 0.4654 -0.3295 0.111 Uiso 1 1 calc R . . H9B H 0.4646 0.5900 -0.3594 0.111 Uiso 1 1 calc R . . H9C H 0.3791 0.5289 -0.3544 0.111 Uiso 1 1 calc R . . C11 C -0.13872(15) 0.67489(13) 0.22391(13) 0.0355(3) Uani 1 1 d . . . C12 C -0.17415(16) 0.69518(13) 0.13893(13) 0.0384(4) Uani 1 1 d . . . C13 C -0.30463(17) 0.74181(15) 0.15507(15) 0.0465(4) Uani 1 1 d . . . H13 H -0.3285 0.7579 0.0981 0.056 Uiso 1 1 calc R . . C14 C -0.40046(17) 0.76535(15) 0.25238(16) 0.0500(5) Uani 1 1 d . . . C15 C -0.36298(17) 0.73830(16) 0.33541(15) 0.0480(4) Uani 1 1 d . . . H15 H -0.4272 0.7508 0.4018 0.058 Uiso 1 1 calc R . . C16 C -0.23409(16) 0.69343(14) 0.32408(13) 0.0395(4) Uani 1 1 d . . . C17 C -0.07638(17) 0.66325(16) 0.03127(13) 0.0450(4) Uani 1 1 d . . . H17A H -0.1174 0.6595 -0.0129 0.068 Uiso 1 1 calc R . . H17B H -0.0065 0.5917 0.0293 0.068 Uiso 1 1 calc R . . H17C H -0.0419 0.7179 0.0077 0.068 Uiso 1 1 calc R . . C18 C -0.54103(19) 0.8148(2) 0.2669(2) 0.0710(7) Uani 1 1 d . . . H18A H -0.5550 0.8666 0.2145 0.106 Uiso 1 1 calc R . . H18B H -0.5942 0.8530 0.3341 0.106 Uiso 1 1 calc R . . H18C H -0.5644 0.7566 0.2615 0.106 Uiso 1 1 calc R . . C19 C -0.20059(18) 0.65937(16) 0.41746(13) 0.0458(4) Uani 1 1 d . . . H19A H -0.2785 0.6902 0.4787 0.069 Uiso 1 1 calc R . . H19B H -0.1393 0.6864 0.4156 0.069 Uiso 1 1 calc R . . H19C H -0.1624 0.5795 0.4182 0.069 Uiso 1 1 calc R . . C21 C 0.10510(15) 0.48545(13) 0.22691(12) 0.0353(3) Uani 1 1 d . . . C22 C 0.23031(16) 0.44060(14) 0.22975(13) 0.0403(4) Uani 1 1 d . . . C23 C 0.29172(18) 0.32859(15) 0.24191(14) 0.0459(4) Uani 1 1 d . . . H23 H 0.3741 0.3003 0.2449 0.055 Uiso 1 1 calc R . . C24 C 0.23639(18) 0.25728(14) 0.24984(14) 0.0454(4) Uani 1 1 d . . . C25 C 0.11549(18) 0.30150(14) 0.24474(13) 0.0434(4) Uani 1 1 d . . . H25 H 0.0768 0.2538 0.2499 0.052 Uiso 1 1 calc R . . C26 C 0.04782(16) 0.41275(13) 0.23246(12) 0.0370(3) Uani 1 1 d . . . C27 C 0.30759(18) 0.50585(16) 0.21449(17) 0.0505(4) Uani 1 1 d . . . H27A H 0.3597 0.4773 0.2558 0.076 Uiso 1 1 calc R . . H27B H 0.2491 0.5828 0.2351 0.076 Uiso 1 1 calc R . . H27C H 0.3637 0.4993 0.1428 0.076 Uiso 1 1 calc R . . C28 C 0.3059(2) 0.13516(16) 0.26037(18) 0.0598(5) Uani 1 1 d . . . H28A H 0.3661 0.0991 0.1933 0.090 Uiso 1 1 calc R . . H28B H 0.2433 0.1042 0.2905 0.090 Uiso 1 1 calc R . . H28C H 0.3530 0.1238 0.3041 0.090 Uiso 1 1 calc R . . C29 C -0.07877(17) 0.44120(15) 0.22218(14) 0.0423(4) Uani 1 1 d . . . H29A H -0.0870 0.3739 0.2178 0.064 Uiso 1 1 calc R . . H29B H -0.0804 0.4808 0.1606 0.064 Uiso 1 1 calc R . . H29C H -0.1501 0.4872 0.2815 0.064 Uiso 1 1 calc R . . C31 C 0.18708(17) 0.83628(14) 0.10799(12) 0.0391(4) Uani 1 1 d . . . C32 C 0.32143(17) 0.78794(15) 0.06309(13) 0.0433(4) Uani 1 1 d . . . F32 F 0.38749(10) 0.67796(9) 0.06105(9) 0.0557(3) Uani 1 1 d . . . C33 C 0.39354(19) 0.84740(18) 0.02024(15) 0.0525(5) Uani 1 1 d . . . F33 F 0.52314(12) 0.79511(12) -0.02161(11) 0.0735(4) Uani 1 1 d . . . C34 C 0.3321(2) 0.96006(19) 0.02086(16) 0.0571(5) Uani 1 1 d . . . F34 F 0.39921(15) 1.01970(13) -0.02319(12) 0.0845(4) Uani 1 1 d . . . C35 C 0.2004(2) 1.01148(17) 0.06659(16) 0.0536(5) Uani 1 1 d . . . F35 F 0.13879(15) 1.12215(10) 0.07060(12) 0.0753(4) Uani 1 1 d . . . C36 C 0.12985(18) 0.95111(15) 0.10862(14) 0.0445(4) Uani 1 1 d . . . F36 F 0.00101(11) 1.00782(9) 0.15060(9) 0.0575(3) Uani 1 1 d . . . C41 C 0.07893(15) 0.76604(14) 0.35799(12) 0.0367(4) Uani 1 1 d . . . C42 C 0.09691(16) 0.85579(14) 0.37451(13) 0.0387(4) Uani 1 1 d . . . F42 F 0.06110(11) 0.94728(8) 0.32232(8) 0.0499(3) Uani 1 1 d . . . C43 C 0.14521(17) 0.86124(15) 0.44457(14) 0.0449(4) Uani 1 1 d . . . F43 F 0.15760(12) 0.95243(10) 0.45671(9) 0.0591(3) Uani 1 1 d . . . C44 C 0.1814(2) 0.77273(18) 0.50178(15) 0.0532(5) Uani 1 1 d . . . F44 F 0.23203(16) 0.77497(13) 0.56875(11) 0.0817(4) Uani 1 1 d . . . C45 C 0.1657(2) 0.68137(17) 0.48917(15) 0.0508(4) Uani 1 1 d . . . F45 F 0.20222(15) 0.59330(11) 0.54387(11) 0.0749(4) Uani 1 1 d . . . C46 C 0.11319(17) 0.68041(14) 0.42037(13) 0.0410(4) Uani 1 1 d . . . F46 F 0.09406(11) 0.59009(9) 0.41759(8) 0.0522(3) Uani 1 1 d . . . C51 C -0.13036(16) 0.87240(13) 0.30749(12) 0.0359(3) Uani 1 1 d . . . C52 C -0.21019(16) 0.91204(14) 0.40827(13) 0.0385(4) Uani 1 1 d . . . F52 F -0.17268(10) 0.86355(8) 0.48603(7) 0.0454(2) Uani 1 1 d . . . C53 C -0.33018(17) 0.99983(16) 0.43763(14) 0.0470(4) Uani 1 1 d . . . F53 F -0.40130(11) 1.03300(10) 0.53675(9) 0.0632(3) Uani 1 1 d . . . C54 C -0.37807(18) 1.05386(16) 0.36470(16) 0.0520(5) Uani 1 1 d . . . F54 F -0.49360(12) 1.14148(11) 0.39147(11) 0.0759(4) Uani 1 1 d . . . C55 C -0.30565(18) 1.01715(15) 0.26373(15) 0.0478(4) Uani 1 1 d . . . F55 F -0.35137(12) 1.06896(10) 0.19149(10) 0.0664(3) Uani 1 1 d . . . C56 C -0.18635(16) 0.92808(14) 0.23755(13) 0.0398(4) Uani 1 1 d . . . F56 F -0.12393(10) 0.89784(8) 0.13659(7) 0.0470(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 P1 0.0316(2) 0.0312(2) 0.0328(2) -0.00236(15) -0.01243(16) -0.01063(16) B1 0.0387(9) 0.0312(9) 0.0365(9) -0.0005(7) -0.0156(8) -0.0137(8) C1 0.0338(8) 0.0324(8) 0.0360(8) 0.0007(6) -0.0145(7) -0.0104(6) C2 0.0319(8) 0.0333(8) 0.0377(8) -0.0003(6) -0.0141(7) -0.0095(6) C3 0.0328(8) 0.0440(9) 0.0357(8) -0.0041(7) -0.0104(7) -0.0153(7) C4 0.0410(9) 0.0429(10) 0.0441(9) -0.0058(7) -0.0127(8) -0.0139(8) C5 0.0401(9) 0.0547(11) 0.0511(11) -0.0183(9) -0.0112(8) -0.0120(8) C6 0.0379(9) 0.0782(14) 0.0389(10) -0.0126(9) -0.0089(8) -0.0247(9) C7 0.0542(11) 0.0695(13) 0.0387(9) 0.0040(9) -0.0177(8) -0.0313(10) C8 0.0483(10) 0.0471(10) 0.0388(9) -0.0007(7) -0.0168(8) -0.0185(8) C9 0.0549(12) 0.112(2) 0.0431(11) -0.0200(12) -0.0090(9) -0.0285(13) C11 0.0353(8) 0.0300(8) 0.0401(8) -0.0044(6) -0.0148(7) -0.0111(6) C12 0.0393(8) 0.0315(8) 0.0444(9) -0.0034(7) -0.0186(7) -0.0114(7) C13 0.0440(9) 0.0414(10) 0.0553(11) -0.0065(8) -0.0262(8) -0.0106(8) C14 0.0356(9) 0.0437(10) 0.0653(12) -0.0163(9) -0.0195(9) -0.0069(8) C15 0.0360(9) 0.0485(10) 0.0503(10) -0.0155(8) -0.0075(8) -0.0134(8) C16 0.0385(8) 0.0352(9) 0.0416(9) -0.0081(7) -0.0117(7) -0.0136(7) C17 0.0446(9) 0.0508(10) 0.0413(9) -0.0009(8) -0.0215(8) -0.0164(8) C18 0.0376(10) 0.0762(15) 0.0855(16) -0.0268(13) -0.0238(11) -0.0043(10) C19 0.0471(10) 0.0508(11) 0.0369(9) -0.0034(7) -0.0095(8) -0.0227(8) C21 0.0364(8) 0.0340(8) 0.0331(8) -0.0022(6) -0.0133(6) -0.0119(7) C22 0.0391(9) 0.0390(9) 0.0406(9) -0.0014(7) -0.0170(7) -0.0122(7) C23 0.0411(9) 0.0404(10) 0.0499(10) 0.0018(8) -0.0217(8) -0.0080(8) C24 0.0501(10) 0.0360(9) 0.0419(9) 0.0021(7) -0.0181(8) -0.0109(8) C25 0.0501(10) 0.0364(9) 0.0419(9) 0.0000(7) -0.0153(8) -0.0183(8) C26 0.0398(8) 0.0352(8) 0.0333(8) -0.0020(6) -0.0122(7) -0.0143(7) C27 0.0409(9) 0.0454(10) 0.0697(12) 0.0035(9) -0.0296(9) -0.0147(8) C28 0.0626(12) 0.0382(10) 0.0660(13) 0.0054(9) -0.0250(10) -0.0111(9) C29 0.0437(9) 0.0398(9) 0.0468(10) -0.0028(7) -0.0174(8) -0.0192(8) C31 0.0463(9) 0.0406(9) 0.0342(8) 0.0018(7) -0.0173(7) -0.0199(8) C32 0.0458(9) 0.0476(10) 0.0400(9) 0.0018(7) -0.0177(8) -0.0213(8) F32 0.0418(6) 0.0486(6) 0.0692(7) -0.0010(5) -0.0175(5) -0.0150(5) C33 0.0498(11) 0.0710(14) 0.0458(10) 0.0048(9) -0.0186(8) -0.0335(10) F33 0.0517(7) 0.0950(10) 0.0774(9) 0.0036(7) -0.0149(6) -0.0426(7) C34 0.0751(14) 0.0696(14) 0.0538(11) 0.0186(10) -0.0317(10) -0.0517(12) F34 0.0983(11) 0.0943(11) 0.1001(11) 0.0340(9) -0.0448(9) -0.0756(9) C35 0.0756(14) 0.0483(11) 0.0544(11) 0.0134(9) -0.0353(10) -0.0347(10) F35 0.1045(10) 0.0448(7) 0.0974(10) 0.0218(6) -0.0534(9) -0.0409(7) C36 0.0527(10) 0.0408(10) 0.0426(9) 0.0044(7) -0.0203(8) -0.0207(8) F36 0.0552(6) 0.0377(6) 0.0706(7) 0.0036(5) -0.0224(6) -0.0138(5) C41 0.0347(8) 0.0377(9) 0.0352(8) -0.0046(6) -0.0123(7) -0.0124(7) C42 0.0373(8) 0.0378(9) 0.0372(8) -0.0019(7) -0.0125(7) -0.0133(7) F42 0.0636(7) 0.0395(5) 0.0523(6) 0.0031(4) -0.0270(5) -0.0226(5) C43 0.0441(9) 0.0483(10) 0.0461(10) -0.0080(8) -0.0155(8) -0.0217(8) F43 0.0655(7) 0.0575(7) 0.0677(7) -0.0113(5) -0.0276(6) -0.0321(6) C44 0.0578(11) 0.0673(13) 0.0480(10) -0.0010(9) -0.0299(9) -0.0286(10) F44 0.1118(11) 0.0942(10) 0.0817(9) 0.0117(8) -0.0716(9) -0.0512(9) C45 0.0600(11) 0.0531(11) 0.0464(10) 0.0104(8) -0.0295(9) -0.0240(9) F45 0.1114(11) 0.0706(8) 0.0721(8) 0.0292(7) -0.0651(8) -0.0438(8) C46 0.0456(9) 0.0413(9) 0.0396(9) 0.0013(7) -0.0178(7) -0.0199(8) F46 0.0720(7) 0.0460(6) 0.0540(6) 0.0122(5) -0.0340(5) -0.0318(5) C51 0.0384(8) 0.0311(8) 0.0377(8) -0.0049(6) -0.0136(7) -0.0134(7) C52 0.0392(9) 0.0389(9) 0.0388(9) -0.0045(7) -0.0155(7) -0.0154(7) F52 0.0469(5) 0.0503(6) 0.0343(5) -0.0049(4) -0.0136(4) -0.0165(5) C53 0.0402(9) 0.0480(10) 0.0440(10) -0.0160(8) -0.0087(8) -0.0130(8) F53 0.0470(6) 0.0704(8) 0.0492(6) -0.0247(5) -0.0059(5) -0.0092(5) C54 0.0378(9) 0.0430(10) 0.0624(12) -0.0142(9) -0.0182(9) -0.0027(8) F54 0.0472(7) 0.0639(8) 0.0839(9) -0.0214(7) -0.0248(6) 0.0106(6) C55 0.0458(10) 0.0438(10) 0.0537(11) -0.0012(8) -0.0273(9) -0.0107(8) F55 0.0607(7) 0.0597(7) 0.0671(7) 0.0005(6) -0.0393(6) -0.0018(6) C56 0.0420(9) 0.0365(9) 0.0397(9) -0.0041(7) -0.0163(7) -0.0135(7) F56 0.0513(6) 0.0460(6) 0.0379(5) -0.0028(4) -0.0205(4) -0.0113(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 P1 C11 1.8215(16) . ? P1 C2 1.8265(17) . ? P1 C21 1.8423(16) . ? P1 B1 2.0941(18) . ? B1 C41 1.626(2) . ? B1 C1 1.634(2) . ? B1 C51 1.635(2) . ? C1 C2 1.353(2) . ? C1 C31 1.489(2) . ? C2 C3 1.476(2) . ? C3 C4 1.386(2) . ? C3 C8 1.401(3) . ? C4 C5 1.385(3) . ? C4 H4 0.9400 . ? C5 C6 1.384(3) . ? C5 H5 0.9400 . ? C6 C7 1.390(3) . ? C6 C9 1.511(3) . ? C7 C8 1.384(3) . ? C7 H7 0.9400 . ? C8 H8 0.9400 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C11 C12 1.402(2) . ? C11 C16 1.411(2) . ? C12 C13 1.389(2) . ? C12 C17 1.498(2) . ? C13 C14 1.382(3) . ? C13 H13 0.9400 . ? C14 C15 1.388(3) . ? C14 C18 1.507(3) . ? C15 C16 1.390(2) . ? C15 H15 0.9400 . ? C16 C19 1.506(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C21 C22 1.418(2) . ? C21 C26 1.423(2) . ? C22 C23 1.388(2) . ? C22 C27 1.508(3) . ? C23 C24 1.380(3) . ? C23 H23 0.9400 . ? C24 C25 1.382(3) . ? C24 C28 1.510(3) . ? C25 C26 1.392(2) . ? C25 H25 0.9400 . ? C26 C29 1.512(2) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C31 C32 1.389(3) . ? C31 C36 1.393(2) . ? C32 F32 1.343(2) . ? C32 C33 1.377(3) . ? C33 F33 1.341(2) . ? C33 C34 1.370(3) . ? C34 F34 1.336(2) . ? C34 C35 1.365(3) . ? C35 F35 1.344(2) . ? C35 C36 1.371(3) . ? C36 F36 1.339(2) . ? C41 C46 1.385(2) . ? C41 C42 1.387(2) . ? C42 F42 1.351(2) . ? C42 C43 1.375(2) . ? C43 F43 1.345(2) . ? C43 C44 1.367(3) . ? C44 F44 1.343(2) . ? C44 C45 1.373(3) . ? C45 F45 1.342(2) . ? C45 C46 1.379(3) . ? C46 F46 1.348(2) . ? C51 C52 1.389(2) . ? C51 C56 1.394(2) . ? C52 F52 1.353(2) . ? C52 C53 1.374(2) . ? C53 F53 1.340(2) . ? C53 C54 1.372(3) . ? C54 F54 1.342(2) . ? C54 C55 1.373(3) . ? C55 F55 1.343(2) . ? C55 C56 1.378(3) . ? C56 F56 1.3490(19) . ? 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 C11 P1 C2 115.87(7) . . ? C11 P1 C21 110.11(7) . . ? C2 P1 C21 112.44(7) . . ? C11 P1 B1 104.73(7) . . ? C2 P1 B1 75.91(7) . . ? C21 P1 B1 134.20(7) . . ? C41 B1 C1 114.37(14) . . ? C41 B1 C51 111.89(13) . . ? C1 B1 C51 115.81(13) . . ? C41 B1 P1 122.71(12) . . ? C1 B1 P1 79.17(9) . . ? C51 B1 P1 109.45(11) . . ? C2 C1 C31 123.53(15) . . ? C2 C1 B1 107.88(14) . . ? C31 C1 B1 128.38(14) . . ? C1 C2 C3 129.07(15) . . ? C1 C2 P1 97.00(11) . . ? C3 C2 P1 133.88(12) . . ? C4 C3 C8 117.96(16) . . ? C4 C3 C2 122.45(16) . . ? C8 C3 C2 119.59(15) . . ? C5 C4 C3 120.76(18) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C6 C5 C4 121.62(18) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C7 117.73(17) . . ? C5 C6 C9 121.2(2) . . ? C7 C6 C9 121.1(2) . . ? C8 C7 C6 121.24(19) . . ? C8 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? C7 C8 C3 120.67(18) . . ? C7 C8 H8 119.7 . . ? C3 C8 H8 119.7 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C11 C16 120.14(15) . . ? C12 C11 P1 123.82(13) . . ? C16 C11 P1 115.86(12) . . ? C13 C12 C11 118.97(16) . . ? C13 C12 C17 118.52(15) . . ? C11 C12 C17 122.43(15) . . ? C14 C13 C12 122.02(17) . . ? C14 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? C13 C14 C15 118.05(16) . . ? C13 C14 C18 120.53(19) . . ? C15 C14 C18 121.38(19) . . ? C14 C15 C16 122.48(17) . . ? C14 C15 H15 118.8 . . ? C16 C15 H15 118.8 . . ? C15 C16 C11 118.14(16) . . ? C15 C16 C19 119.28(16) . . ? C11 C16 C19 122.44(15) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 C21 C26 118.58(15) . . ? C22 C21 P1 118.15(12) . . ? C26 C21 P1 123.27(12) . . ? C23 C22 C21 119.74(16) . . ? C23 C22 C27 115.97(15) . . ? C21 C22 C27 124.21(15) . . ? C24 C23 C22 122.45(17) . . ? C24 C23 H23 118.8 . . ? C22 C23 H23 118.8 . . ? C23 C24 C25 117.31(16) . . ? C23 C24 C28 121.79(18) . . ? C25 C24 C28 120.88(18) . . ? C24 C25 C26 123.67(17) . . ? C24 C25 H25 118.2 . . ? C26 C25 H25 118.2 . . ? C25 C26 C21 118.19(15) . . ? C25 C26 C29 114.48(15) . . ? C21 C26 C29 127.28(15) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C32 C31 C36 114.67(16) . . ? C32 C31 C1 121.42(15) . . ? C36 C31 C1 123.85(16) . . ? F32 C32 C33 116.67(17) . . ? F32 C32 C31 120.02(15) . . ? C33 C32 C31 123.31(18) . . ? F33 C33 C34 120.38(18) . . ? F33 C33 C32 120.04(19) . . ? C34 C33 C32 119.59(19) . . ? F34 C34 C35 119.8(2) . . ? F34 C34 C33 121.0(2) . . ? C35 C34 C33 119.20(18) . . ? F35 C35 C34 119.99(18) . . ? F35 C35 C36 119.5(2) . . ? C34 C35 C36 120.51(19) . . ? F36 C36 C35 116.72(17) . . ? F36 C36 C31 120.59(16) . . ? C35 C36 C31 122.68(18) . . ? C46 C41 C42 113.47(15) . . ? C46 C41 B1 127.92(15) . . ? C42 C41 B1 118.55(15) . . ? F42 C42 C43 115.90(15) . . ? F42 C42 C41 119.52(15) . . ? C43 C42 C41 124.53(16) . . ? F43 C43 C44 119.97(16) . . ? F43 C43 C42 120.58(17) . . ? C44 C43 C42 119.45(17) . . ? F44 C44 C43 120.55(18) . . ? F44 C44 C45 120.64(19) . . ? C43 C44 C45 118.81(17) . . ? F45 C45 C44 119.54(17) . . ? F45 C45 C46 120.47(18) . . ? C44 C45 C46 119.99(17) . . ? F46 C46 C45 115.89(15) . . ? F46 C46 C41 120.43(15) . . ? C45 C46 C41 123.67(17) . . ? C52 C51 C56 113.10(15) . . ? C52 C51 B1 123.04(14) . . ? C56 C51 B1 123.81(14) . . ? F52 C52 C53 115.02(15) . . ? F52 C52 C51 120.52(15) . . ? C53 C52 C51 124.46(16) . . ? F53 C53 C54 119.60(16) . . ? F53 C53 C52 120.75(17) . . ? C54 C53 C52 119.65(16) . . ? F54 C54 C53 120.60(17) . . ? F54 C54 C55 120.44(18) . . ? C53 C54 C55 118.96(16) . . ? F55 C55 C54 119.66(16) . . ? F55 C55 C56 120.73(17) . . ? C54 C55 C56 119.60(17) . . ? F56 C56 C55 114.85(15) . . ? F56 C56 C51 120.99(14) . . ? C55 C56 C51 124.15(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 P1 B1 C41 133.06(13) . . . . ? C2 P1 B1 C41 -113.42(14) . . . . ? C21 P1 B1 C41 -5.67(19) . . . . ? C11 P1 B1 C1 -114.83(9) . . . . ? C2 P1 B1 C1 -1.31(9) . . . . ? C21 P1 B1 C1 106.44(11) . . . . ? C11 P1 B1 C51 -1.10(13) . . . . ? C2 P1 B1 C51 112.43(12) . . . . ? C21 P1 B1 C51 -139.83(11) . . . . ? C41 B1 C1 C2 122.95(15) . . . . ? C51 B1 C1 C2 -104.70(16) . . . . ? P1 B1 C1 C2 1.80(12) . . . . ? C41 B1 C1 C31 -51.8(2) . . . . ? C51 B1 C1 C31 80.6(2) . . . . ? P1 B1 C1 C31 -172.92(15) . . . . ? C31 C1 C2 C3 -4.6(3) . . . . ? B1 C1 C2 C3 -179.66(15) . . . . ? C31 C1 C2 P1 172.99(13) . . . . ? B1 C1 C2 P1 -2.04(13) . . . . ? C11 P1 C2 C1 101.33(11) . . . . ? C21 P1 C2 C1 -130.81(11) . . . . ? B1 P1 C2 C1 1.56(10) . . . . ? C11 P1 C2 C3 -81.24(17) . . . . ? C21 P1 C2 C3 46.62(18) . . . . ? B1 P1 C2 C3 179.00(17) . . . . ? C1 C2 C3 C4 136.72(19) . . . . ? P1 C2 C3 C4 -40.0(2) . . . . ? C1 C2 C3 C8 -42.2(2) . . . . ? P1 C2 C3 C8 141.10(15) . . . . ? C8 C3 C4 C5 1.5(3) . . . . ? C2 C3 C4 C5 -177.42(16) . . . . ? C3 C4 C5 C6 -1.3(3) . . . . ? C4 C5 C6 C7 0.5(3) . . . . ? C4 C5 C6 C9 -178.29(18) . . . . ? C5 C6 C7 C8 0.1(3) . . . . ? C9 C6 C7 C8 178.89(19) . . . . ? C6 C7 C8 C3 0.1(3) . . . . ? C4 C3 C8 C7 -0.9(3) . . . . ? C2 C3 C8 C7 178.04(16) . . . . ? C2 P1 C11 C12 27.96(16) . . . . ? C21 P1 C11 C12 -101.04(14) . . . . ? B1 P1 C11 C12 109.19(14) . . . . ? C2 P1 C11 C16 -147.06(12) . . . . ? C21 P1 C11 C16 83.93(13) . . . . ? B1 P1 C11 C16 -65.83(14) . . . . ? C16 C11 C12 C13 5.1(2) . . . . ? P1 C11 C12 C13 -169.76(13) . . . . ? C16 C11 C12 C17 -171.79(16) . . . . ? P1 C11 C12 C17 13.4(2) . . . . ? C11 C12 C13 C14 -2.2(3) . . . . ? C17 C12 C13 C14 174.72(17) . . . . ? C12 C13 C14 C15 -1.7(3) . . . . ? C12 C13 C14 C18 -179.30(19) . . . . ? C13 C14 C15 C16 2.9(3) . . . . ? C18 C14 C15 C16 -179.50(19) . . . . ? C14 C15 C16 C11 -0.1(3) . . . . ? C14 C15 C16 C19 -176.01(17) . . . . ? C12 C11 C16 C15 -3.9(2) . . . . ? P1 C11 C16 C15 171.33(13) . . . . ? C12 C11 C16 C19 171.85(15) . . . . ? P1 C11 C16 C19 -12.9(2) . . . . ? C11 P1 C21 C22 -175.18(12) . . . . ? C2 P1 C21 C22 53.98(14) . . . . ? B1 P1 C21 C22 -37.98(18) . . . . ? C11 P1 C21 C26 5.40(16) . . . . ? C2 P1 C21 C26 -125.45(14) . . . . ? B1 P1 C21 C26 142.60(13) . . . . ? C26 C21 C22 C23 -2.6(2) . . . . ? P1 C21 C22 C23 178.00(13) . . . . ? C26 C21 C22 C27 173.92(16) . . . . ? P1 C21 C22 C27 -5.5(2) . . . . ? C21 C22 C23 C24 1.1(3) . . . . ? C27 C22 C23 C24 -175.67(17) . . . . ? C22 C23 C24 C25 0.3(3) . . . . ? C22 C23 C24 C28 178.44(18) . . . . ? C23 C24 C25 C26 -0.2(3) . . . . ? C28 C24 C25 C26 -178.33(17) . . . . ? C24 C25 C26 C21 -1.3(3) . . . . ? C24 C25 C26 C29 176.31(16) . . . . ? C22 C21 C26 C25 2.6(2) . . . . ? P1 C21 C26 C25 -177.95(12) . . . . ? C22 C21 C26 C29 -174.66(16) . . . . ? P1 C21 C26 C29 4.8(2) . . . . ? C2 C1 C31 C32 -55.4(2) . . . . ? B1 C1 C31 C32 118.60(19) . . . . ? C2 C1 C31 C36 127.61(18) . . . . ? B1 C1 C31 C36 -58.4(2) . . . . ? C36 C31 C32 F32 177.83(15) . . . . ? C1 C31 C32 F32 0.6(2) . . . . ? C36 C31 C32 C33 -1.4(3) . . . . ? C1 C31 C32 C33 -178.67(17) . . . . ? F32 C32 C33 F33 0.6(3) . . . . ? C31 C32 C33 F33 179.85(17) . . . . ? F32 C32 C33 C34 -179.27(17) . . . . ? C31 C32 C33 C34 0.0(3) . . . . ? F33 C33 C34 F34 2.4(3) . . . . ? C32 C33 C34 F34 -177.72(18) . . . . ? F33 C33 C34 C35 -178.09(18) . . . . ? C32 C33 C34 C35 1.8(3) . . . . ? F34 C34 C35 F35 -2.5(3) . . . . ? C33 C34 C35 F35 178.01(18) . . . . ? F34 C34 C35 C36 177.47(18) . . . . ? C33 C34 C35 C36 -2.0(3) . . . . ? F35 C35 C36 F36 0.9(3) . . . . ? C34 C35 C36 F36 -179.01(17) . . . . ? F35 C35 C36 C31 -179.51(16) . . . . ? C34 C35 C36 C31 0.5(3) . . . . ? C32 C31 C36 F36 -179.32(15) . . . . ? C1 C31 C36 F36 -2.1(3) . . . . ? C32 C31 C36 C35 1.1(3) . . . . ? C1 C31 C36 C35 178.34(17) . . . . ? C1 B1 C41 C46 -111.15(19) . . . . ? C51 B1 C41 C46 114.66(18) . . . . ? P1 B1 C41 C46 -18.5(2) . . . . ? C1 B1 C41 C42 71.86(19) . . . . ? C51 B1 C41 C42 -62.33(19) . . . . ? P1 B1 C41 C42 164.48(12) . . . . ? C46 C41 C42 F42 -176.66(14) . . . . ? B1 C41 C42 F42 0.7(2) . . . . ? C46 C41 C42 C43 0.7(2) . . . . ? B1 C41 C42 C43 178.12(16) . . . . ? F42 C42 C43 F43 -1.5(2) . . . . ? C41 C42 C43 F43 -178.96(15) . . . . ? F42 C42 C43 C44 178.83(16) . . . . ? C41 C42 C43 C44 1.4(3) . . . . ? F43 C43 C44 F44 -1.4(3) . . . . ? C42 C43 C44 F44 178.24(18) . . . . ? F43 C43 C44 C45 178.90(17) . . . . ? C42 C43 C44 C45 -1.4(3) . . . . ? F44 C44 C45 F45 -0.5(3) . . . . ? C43 C44 C45 F45 179.20(18) . . . . ? F44 C44 C45 C46 179.78(19) . . . . ? C43 C44 C45 C46 -0.5(3) . . . . ? F45 C45 C46 F46 4.2(3) . . . . ? C44 C45 C46 F46 -176.09(17) . . . . ? F45 C45 C46 C41 -176.90(17) . . . . ? C44 C45 C46 C41 2.8(3) . . . . ? C42 C41 C46 F46 176.08(15) . . . . ? B1 C41 C46 F46 -1.0(3) . . . . ? C42 C41 C46 C45 -2.8(3) . . . . ? B1 C41 C46 C45 -179.93(17) . . . . ? C41 B1 C51 C52 -24.8(2) . . . . ? C1 B1 C51 C52 -158.25(15) . . . . ? P1 B1 C51 C52 114.65(15) . . . . ? C41 B1 C51 C56 152.51(15) . . . . ? C1 B1 C51 C56 19.0(2) . . . . ? P1 B1 C51 C56 -68.07(18) . . . . ? C56 C51 C52 F52 176.90(14) . . . . ? B1 C51 C52 F52 -5.6(2) . . . . ? C56 C51 C52 C53 -2.5(2) . . . . ? B1 C51 C52 C53 175.02(16) . . . . ? F52 C52 C53 F53 0.6(2) . . . . ? C51 C52 C53 F53 -179.99(16) . . . . ? F52 C52 C53 C54 -179.12(16) . . . . ? C51 C52 C53 C54 0.3(3) . . . . ? F53 C53 C54 F54 2.0(3) . . . . ? C52 C53 C54 F54 -178.33(18) . . . . ? F53 C53 C54 C55 -178.29(18) . . . . ? C52 C53 C54 C55 1.4(3) . . . . ? F54 C54 C55 F55 -0.5(3) . . . . ? C53 C54 C55 F55 179.80(18) . . . . ? F54 C54 C55 C56 179.01(18) . . . . ? C53 C54 C55 C56 -0.7(3) . . . . ? F55 C55 C56 F56 -1.4(3) . . . . ? C54 C55 C56 F56 179.18(17) . . . . ? F55 C55 C56 C51 177.72(16) . . . . ? C54 C55 C56 C51 -1.8(3) . . . . ? C52 C51 C56 F56 -177.76(14) . . . . ? B1 C51 C56 F56 4.7(2) . . . . ? C52 C51 C56 C55 3.2(3) . . . . ? B1 C51 C56 C55 -174.29(16) . . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 66.95 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.229 _refine_diff_density_min -0.258 _refine_diff_density_rms 0.037 # Attachment '- 5.cif' data_erk5928 _database_code_depnum_ccdc_archive 'CCDC 826909' #TrackingRef '- 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H36 B Cl F15 P' _chemical_formula_weight 975.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 21.7497(6) _cell_length_b 22.5390(4) _cell_length_c 17.9477(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8798.3(4) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 13279 _cell_measurement_theta_min 0.88 _cell_measurement_theta_max 68.25 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3968 _exptl_absorpt_coefficient_mu 1.998 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5673 _exptl_absorpt_correction_T_max 0.9244 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47800 _diffrn_reflns_av_R_equivalents 0.074 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 67.18 _reflns_number_total 14469 _reflns_number_gt 12099 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (bruekrAXS, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0758P)^2^+8.0364P] 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 SHELXL _refine_ls_extinction_coef 0.00076(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.50(2) _refine_ls_number_reflns 14469 _refine_ls_number_parameters 1206 _refine_ls_number_restraints 58 _refine_ls_R_factor_all 0.0736 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1567 _refine_ls_wR_factor_gt 0.1419 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.047 _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 P1A P 0.57621(5) 0.99291(5) 0.91638(7) 0.0440(3) Uani 1 1 d . . . B1A B 0.4685(3) 1.0928(2) 0.9039(3) 0.0475(12) Uani 1 1 d . . . C1A C 0.5354(2) 1.0597(2) 0.8937(3) 0.0439(10) Uani 1 1 d . . . C2A C 0.5863(2) 1.0523(2) 0.8543(3) 0.0433(10) Uani 1 1 d . . . C3A C 0.6262(2) 1.0792(2) 0.7979(3) 0.0437(10) Uani 1 1 d . . . C4A C 0.6883(2) 1.0886(2) 0.8130(3) 0.0556(12) Uani 1 1 d . . . H4A H 0.7049 1.0768 0.8590 0.067 Uiso 1 1 calc R . . C5A C 0.7254(2) 1.1153(3) 0.7606(3) 0.0625(14) Uani 1 1 d . . . H5A H 0.7672 1.1212 0.7716 0.075 Uiso 1 1 calc R . . C6A C 0.7031(3) 1.1336(2) 0.6923(3) 0.0575(13) Uani 1 1 d . . . C7A C 0.6411(2) 1.1245(2) 0.6778(3) 0.0524(12) Uani 1 1 d . . . H7A H 0.6247 1.1368 0.6319 0.063 Uiso 1 1 calc R . . C8A C 0.6031(2) 1.0977(2) 0.7297(3) 0.0468(11) Uani 1 1 d . . . H8A H 0.5612 1.0920 0.7186 0.056 Uiso 1 1 calc R . . C9A C 0.7450(3) 1.1621(3) 0.6359(4) 0.085(2) Uani 1 1 d . . . H9AA H 0.7606 1.1992 0.6555 0.128 Uiso 1 1 calc R . . H9AB H 0.7223 1.1696 0.5903 0.128 Uiso 1 1 calc R . . H9AC H 0.7792 1.1357 0.6254 0.128 Uiso 1 1 calc R . . C11A C 0.6294(2) 0.9846(2) 0.9927(3) 0.0482(11) Uani 1 1 d . . . C12A C 0.6859(2) 0.9569(2) 0.9752(3) 0.0512(12) Uani 1 1 d . . . C13A C 0.7277(2) 0.9480(2) 1.0328(3) 0.0560(12) Uani 1 1 d . . . H13A H 0.7653 0.9293 1.0221 0.067 Uiso 1 1 calc R . . C14A C 0.7161(3) 0.9659(3) 1.1059(3) 0.0628(14) Uani 1 1 d . . . C15A C 0.6600(3) 0.9933(3) 1.1204(3) 0.0613(14) Uani 1 1 d . . . H15A H 0.6517 1.0059 1.1693 0.074 Uiso 1 1 calc R . . C16A C 0.6164(2) 1.0026(2) 1.0665(3) 0.0511(12) Uani 1 1 d . . . C17A C 0.7022(3) 0.9371(3) 0.8982(3) 0.0623(14) Uani 1 1 d . . . H17A H 0.6742 0.9060 0.8826 0.093 Uiso 1 1 calc R . . H17B H 0.7440 0.9220 0.8978 0.093 Uiso 1 1 calc R . . H17C H 0.6991 0.9704 0.8642 0.093 Uiso 1 1 calc R . . C18A C 0.7622(3) 0.9557(3) 1.1666(4) 0.0835(19) Uani 1 1 d . . . H18A H 0.7828 0.9181 1.1584 0.125 Uiso 1 1 calc R . . H18B H 0.7414 0.9549 1.2144 0.125 Uiso 1 1 calc R . . H18C H 0.7923 0.9875 1.1662 0.125 Uiso 1 1 calc R . . C19A C 0.5564(3) 1.0302(3) 1.0917(3) 0.0656(15) Uani 1 1 d . . . H19A H 0.5352 1.0030 1.1247 0.098 Uiso 1 1 calc R . . H19B H 0.5308 1.0382 1.0486 0.098 Uiso 1 1 calc R . . H19C H 0.5648 1.0670 1.1178 0.098 Uiso 1 1 calc R . . C21A C 0.5446(2) 0.9233(2) 0.8840(3) 0.0462(11) Uani 1 1 d . . . C22A C 0.5135(2) 0.8867(2) 0.9362(3) 0.0521(12) Uani 1 1 d . . . C23A C 0.4830(2) 0.8365(2) 0.9099(4) 0.0608(14) Uani 1 1 d . . . H23A H 0.4629 0.8120 0.9445 0.073 Uiso 1 1 calc R . . C24A C 0.4811(3) 0.8213(2) 0.8350(4) 0.0624(14) Uani 1 1 d . . . C25A C 0.5136(3) 0.8568(2) 0.7862(3) 0.0573(13) Uani 1 1 d . . . H25A H 0.5144 0.8460 0.7356 0.069 Uiso 1 1 calc R . . C26A C 0.5452(2) 0.9079(2) 0.8078(3) 0.0509(11) Uani 1 1 d . . . C27A C 0.5112(3) 0.8990(3) 1.0187(3) 0.0671(15) Uani 1 1 d . . . H27A H 0.5519 0.8940 1.0399 0.101 Uiso 1 1 calc R . . H27B H 0.4830 0.8714 1.0423 0.101 Uiso 1 1 calc R . . H27C H 0.4972 0.9393 1.0270 0.101 Uiso 1 1 calc R . . C28A C 0.4441(3) 0.7681(3) 0.8097(5) 0.083(2) Uani 1 1 d . . . H28A H 0.4502 0.7356 0.8444 0.125 Uiso 1 1 calc R . . H28B H 0.4576 0.7561 0.7604 0.125 Uiso 1 1 calc R . . H28C H 0.4009 0.7784 0.8080 0.125 Uiso 1 1 calc R . . C29A C 0.5777(3) 0.9428(2) 0.7492(3) 0.0568(13) Uani 1 1 d . . . H29A H 0.5813 0.9190 0.7043 0.085 Uiso 1 1 calc R . . H29B H 0.6184 0.9535 0.7668 0.085 Uiso 1 1 calc R . . H29C H 0.5545 0.9785 0.7383 0.085 Uiso 1 1 calc R . . C31A C 0.4667(2) 1.1377(2) 0.9751(3) 0.0502(11) Uani 1 1 d . . . C32A C 0.5165(3) 1.1592(2) 1.0136(3) 0.0587(13) Uani 1 1 d . . . F32A F 0.57421(14) 1.13942(15) 0.99845(19) 0.0701(9) Uani 1 1 d . . . C33A C 0.5129(3) 1.2001(3) 1.0717(3) 0.0698(16) Uani 1 1 d . . . F33A F 0.5640(2) 1.21687(19) 1.1081(2) 0.0967(12) Uani 1 1 d . . . C34A C 0.4573(4) 1.2229(3) 1.0902(4) 0.0738(17) Uani 1 1 d . . . F34A F 0.4524(2) 1.26337(17) 1.1451(2) 0.1051(14) Uani 1 1 d . . . C35A C 0.4053(3) 1.2048(3) 1.0523(4) 0.0724(17) Uani 1 1 d . . . F35A F 0.3501(2) 1.22733(19) 1.0693(2) 0.0998(13) Uani 1 1 d . . . C36A C 0.4111(3) 1.1631(2) 0.9954(3) 0.0566(13) Uani 1 1 d . . . F36A F 0.35945(15) 1.14658(14) 0.96004(19) 0.0696(8) Uani 1 1 d . . . C41A C 0.4562(2) 1.1356(2) 0.8308(3) 0.0500(12) Uani 1 1 d . . . C42A C 0.4992(2) 1.1785(2) 0.8110(3) 0.0537(12) Uani 1 1 d . . . F42A F 0.55009(14) 1.18518(13) 0.8532(2) 0.0664(8) Uani 1 1 d . . . C43A C 0.4941(3) 1.2146(2) 0.7502(4) 0.0653(15) Uani 1 1 d . . . F43A F 0.53906(18) 1.25331(15) 0.7332(2) 0.0881(12) Uani 1 1 d . . . C44A C 0.4437(3) 1.2096(2) 0.7037(3) 0.0670(16) Uani 1 1 d . . . F44A F 0.4390(2) 1.24300(16) 0.6426(2) 0.0972(13) Uani 1 1 d . . . C45A C 0.3978(3) 1.1710(3) 0.7226(3) 0.0649(15) Uani 1 1 d . . . F45A F 0.34773(18) 1.16630(17) 0.6799(2) 0.0899(11) Uani 1 1 d . . . C46A C 0.4045(2) 1.1352(2) 0.7849(3) 0.0550(12) Uani 1 1 d . . . F46A F 0.35618(13) 1.09938(14) 0.80013(19) 0.0645(8) Uani 1 1 d . . . C51A C 0.4221(2) 1.0348(2) 0.9086(3) 0.0444(10) Uani 1 1 d . . . C52A C 0.3928(2) 1.0139(2) 0.9716(3) 0.0481(11) Uani 1 1 d . . . F52A F 0.39776(15) 1.04273(14) 1.03761(17) 0.0646(8) Uani 1 1 d . . . C53A C 0.3577(2) 0.9628(2) 0.9734(3) 0.0584(13) Uani 1 1 d . . . F53A F 0.33080(17) 0.94545(16) 1.0371(2) 0.0827(10) Uani 1 1 d . . . C54A C 0.3522(2) 0.9296(2) 0.9106(4) 0.0616(14) Uani 1 1 d . . . F54A F 0.31959(16) 0.87810(15) 0.9117(3) 0.0866(11) Uani 1 1 d . . . C55A C 0.3816(2) 0.9474(2) 0.8459(3) 0.0547(12) Uani 1 1 d . . . F55A F 0.37626(15) 0.91462(14) 0.7835(2) 0.0725(9) Uani 1 1 d . . . C56A C 0.4153(2) 0.9983(2) 0.8479(3) 0.0480(11) Uani 1 1 d . . . F56A F 0.44392(13) 1.01248(13) 0.78263(16) 0.0561(7) Uani 1 1 d . . . P1B P 0.47378(5) 0.51305(5) 0.35731(6) 0.0373(2) Uani 1 1 d . . . B1B B 0.3624(2) 0.4947(2) 0.4742(3) 0.0382(10) Uani 1 1 d . . . C1B C 0.4307(2) 0.48963(18) 0.4377(2) 0.0388(10) Uani 1 1 d . . . C2B C 0.4824(2) 0.45936(19) 0.4266(2) 0.0400(10) Uani 1 1 d . . . C3B C 0.5189(2) 0.40904(18) 0.4555(2) 0.0381(9) Uani 1 1 d . . . C4B C 0.4901(2) 0.3595(2) 0.4836(3) 0.0474(11) Uani 1 1 d . . . H4B H 0.4469 0.3570 0.4835 0.057 Uiso 1 1 calc R . . C5B C 0.5250(3) 0.3132(2) 0.5124(3) 0.0573(13) Uani 1 1 d . . . H5B H 0.5049 0.2798 0.5322 0.069 Uiso 1 1 calc R . . C6B C 0.5882(3) 0.3150(2) 0.5125(3) 0.0560(13) Uani 1 1 d . . . C7B C 0.6169(2) 0.3643(2) 0.4826(3) 0.0582(13) Uani 1 1 d . . . H7B H 0.6601 0.3662 0.4814 0.070 Uiso 1 1 calc R . . C8B C 0.5826(2) 0.4111(2) 0.4542(3) 0.0493(11) Uani 1 1 d . . . H8B H 0.6027 0.4444 0.4341 0.059 Uiso 1 1 calc R . . C9B C 0.6255(3) 0.2647(3) 0.5456(4) 0.085(2) Uani 1 1 d . . . H9BA H 0.6010 0.2288 0.5461 0.127 Uiso 1 1 calc R . . H9BB H 0.6374 0.2748 0.5961 0.127 Uiso 1 1 calc R . . H9BC H 0.6621 0.2584 0.5157 0.127 Uiso 1 1 calc R . . C11B C 0.5275(2) 0.57432(19) 0.3592(2) 0.0400(9) Uani 1 1 d . . . C12B C 0.5129(2) 0.6304(2) 0.3909(3) 0.0443(10) Uani 1 1 d . . . C13B C 0.5608(2) 0.6721(2) 0.3960(3) 0.0537(12) Uani 1 1 d . . . H13B H 0.5523 0.7097 0.4161 0.064 Uiso 1 1 calc R . . C14B C 0.6200(2) 0.6596(2) 0.3724(3) 0.0561(13) Uani 1 1 d . . . C15B C 0.6319(2) 0.6055(2) 0.3405(3) 0.0557(13) Uani 1 1 d . . . H15B H 0.6721 0.5972 0.3243 0.067 Uiso 1 1 calc R . . C16B C 0.5867(2) 0.5624(2) 0.3313(3) 0.0458(11) Uani 1 1 d . . . C17B C 0.4509(2) 0.6496(2) 0.4140(3) 0.0518(12) Uani 1 1 d . . . H17D H 0.4525 0.6652 0.4643 0.078 Uiso 1 1 calc R . . H17E H 0.4230 0.6160 0.4124 0.078 Uiso 1 1 calc R . . H17F H 0.4363 0.6802 0.3804 0.078 Uiso 1 1 calc R . . C18B C 0.6705(3) 0.7053(3) 0.3809(4) 0.0820(19) Uani 1 1 d . . . H18D H 0.6821 0.7082 0.4329 0.123 Uiso 1 1 calc R . . H18E H 0.6558 0.7436 0.3636 0.123 Uiso 1 1 calc R . . H18F H 0.7059 0.6934 0.3516 0.123 Uiso 1 1 calc R . . C19B C 0.6026(2) 0.5061(2) 0.2896(3) 0.0561(13) Uani 1 1 d . . . H19D H 0.5867 0.5085 0.2392 0.084 Uiso 1 1 calc R . . H19E H 0.5844 0.4724 0.3148 0.084 Uiso 1 1 calc R . . H19F H 0.6469 0.5014 0.2880 0.084 Uiso 1 1 calc R . . C21B C 0.44886(19) 0.49228(19) 0.2649(2) 0.0385(9) Uani 1 1 d . . . C22B C 0.4237(2) 0.5361(2) 0.2177(3) 0.0417(10) Uani 1 1 d . . . C23B C 0.4031(2) 0.5194(2) 0.1476(3) 0.0472(11) Uani 1 1 d . . . H23B H 0.3863 0.5487 0.1163 0.057 Uiso 1 1 calc R . . C24B C 0.4060(2) 0.4613(2) 0.1216(3) 0.0473(11) Uani 1 1 d . . . C25B C 0.4305(2) 0.4190(2) 0.1694(3) 0.0487(11) Uani 1 1 d . . . H25B H 0.4324 0.3794 0.1533 0.058 Uiso 1 1 calc R . . C26B C 0.4522(2) 0.4327(2) 0.2400(3) 0.0435(10) Uani 1 1 d . . . C27B C 0.4175(2) 0.6009(2) 0.2393(3) 0.0512(12) Uani 1 1 d . . . H27D H 0.3913 0.6210 0.2036 0.077 Uiso 1 1 calc R . . H27E H 0.4578 0.6194 0.2396 0.077 Uiso 1 1 calc R . . H27F H 0.3994 0.6038 0.2886 0.077 Uiso 1 1 calc R . . C28B C 0.3839(3) 0.4443(3) 0.0455(3) 0.0619(14) Uani 1 1 d . . . H28D H 0.4178 0.4465 0.0105 0.093 Uiso 1 1 calc R . . H28E H 0.3515 0.4712 0.0300 0.093 Uiso 1 1 calc R . . H28F H 0.3680 0.4041 0.0467 0.093 Uiso 1 1 calc R . . C29B C 0.4780(3) 0.3820(2) 0.2856(3) 0.0545(12) Uani 1 1 d . . . H29D H 0.5189 0.3922 0.3028 0.082 Uiso 1 1 calc R . . H29E H 0.4801 0.3466 0.2550 0.082 Uiso 1 1 calc R . . H29F H 0.4515 0.3747 0.3281 0.082 Uiso 1 1 calc R . . C31B C 0.3489(2) 0.43800(19) 0.5297(2) 0.0400(9) Uani 1 1 d . . . C32B C 0.3905(2) 0.4245(2) 0.5869(3) 0.0434(10) Uani 1 1 d . . . F32B F 0.44284(12) 0.45616(12) 0.59315(15) 0.0514(6) Uani 1 1 d . . . C33B C 0.3830(2) 0.3790(2) 0.6376(3) 0.0482(11) Uani 1 1 d . . . F33B F 0.42713(15) 0.36738(14) 0.68743(17) 0.0665(8) Uani 1 1 d . . . C34B C 0.3297(3) 0.3468(2) 0.6360(3) 0.0535(12) Uani 1 1 d . . . F34B F 0.32007(17) 0.30313(14) 0.68676(19) 0.0736(9) Uani 1 1 d . . . C35B C 0.2858(2) 0.3586(2) 0.5839(3) 0.0495(11) Uani 1 1 d . . . F35B F 0.23374(15) 0.32736(13) 0.5818(2) 0.0715(9) Uani 1 1 d . . . C36B C 0.2967(2) 0.4035(2) 0.5314(3) 0.0449(10) Uani 1 1 d . . . F36B F 0.25124(12) 0.41169(12) 0.48098(16) 0.0544(7) Uani 1 1 d . . . C41B C 0.35243(19) 0.55262(18) 0.5276(2) 0.0376(9) Uani 1 1 d . . . C42B C 0.39916(19) 0.5840(2) 0.5624(3) 0.0412(10) Uani 1 1 d . . . F42B F 0.45875(11) 0.57141(12) 0.54730(16) 0.0521(7) Uani 1 1 d . . . C43B C 0.3894(2) 0.6292(2) 0.6122(3) 0.0470(11) Uani 1 1 d . . . F43B F 0.43716(14) 0.65780(13) 0.6434(2) 0.0686(9) Uani 1 1 d . . . C44B C 0.3309(2) 0.6455(2) 0.6305(3) 0.0495(11) Uani 1 1 d . . . F44B F 0.31999(16) 0.69008(14) 0.67844(18) 0.0711(9) Uani 1 1 d . . . C45B C 0.2823(2) 0.6153(2) 0.5985(3) 0.0455(11) Uani 1 1 d . . . F45B F 0.22411(13) 0.63076(14) 0.61602(18) 0.0640(8) Uani 1 1 d . . . C46B C 0.29449(19) 0.5704(2) 0.5493(2) 0.0395(9) Uani 1 1 d . . . F46B F 0.24454(11) 0.54118(12) 0.52216(16) 0.0520(6) Uani 1 1 d . . . C51B C 0.32149(19) 0.49407(19) 0.3965(2) 0.0393(10) Uani 1 1 d . . . C52B C 0.2946(2) 0.5429(2) 0.3621(3) 0.0434(10) Uani 1 1 d . . . F52B F 0.29594(14) 0.59651(11) 0.39640(16) 0.0561(7) Uani 1 1 d . . . C53B C 0.2676(2) 0.5419(2) 0.2924(3) 0.0491(11) Uani 1 1 d . . . F53B F 0.24263(16) 0.59134(14) 0.26468(18) 0.0704(9) Uani 1 1 d . . . C54B C 0.2668(2) 0.4905(2) 0.2531(3) 0.0503(12) Uani 1 1 d . . . F54B F 0.24114(15) 0.48864(15) 0.18433(17) 0.0689(8) Uani 1 1 d . . . C55B C 0.2925(2) 0.4404(2) 0.2827(3) 0.0480(11) Uani 1 1 d . . . F55B F 0.29158(15) 0.38882(13) 0.24431(16) 0.0630(8) Uani 1 1 d . . . C56B C 0.3186(2) 0.44336(19) 0.3521(3) 0.0425(10) Uani 1 1 d . . . F56B F 0.34473(13) 0.39244(12) 0.37772(16) 0.0536(7) Uani 1 1 d . . . C101 C 0.8395(6) 0.7831(5) 1.5031(6) 0.150(4) Uani 1 1 d DU . . H10A H 0.8639 0.7552 1.5318 0.226 Uiso 1 1 calc R . . H10B H 0.8002 0.7892 1.5276 0.226 Uiso 1 1 calc R . . H10C H 0.8611 0.8206 1.4996 0.226 Uiso 1 1 calc R . . C102 C 0.8302(6) 0.7616(4) 1.4354(5) 0.127(3) Uani 1 1 d DU . . H10D H 0.8235 0.7191 1.4436 0.153 Uiso 1 1 calc R . . H10E H 0.7900 0.7776 1.4210 0.153 Uiso 1 1 calc R . . C103 C 0.8626(4) 0.7638(4) 1.3739(5) 0.119(3) Uani 1 1 d DU . . H10F H 0.8951 0.7340 1.3791 0.142 Uiso 1 1 calc R . . H10G H 0.8830 0.8026 1.3736 0.142 Uiso 1 1 calc R . . C104 C 0.8385(6) 0.7563(5) 1.3049(6) 0.164(5) Uani 1 1 d DU . . H10H H 0.8730 0.7436 1.2735 0.197 Uiso 1 1 calc R . . H10I H 0.8111 0.7220 1.3089 0.197 Uiso 1 1 calc R . . C105 C 0.8078(4) 0.7961(4) 1.2642(6) 0.109(3) Uani 1 1 d DU . . H10J H 0.7679 0.8034 1.2867 0.163 Uiso 1 1 calc R . . H10K H 0.8021 0.7809 1.2140 0.163 Uiso 1 1 calc R . . H10L H 0.8309 0.8329 1.2622 0.163 Uiso 1 1 calc R . . C201 C 0.1973(6) 0.7464(6) 0.8666(9) 0.167(5) Uani 1 1 d U . . H20A H 0.1736 0.7139 0.8446 0.200 Uiso 1 1 calc R . . H20B H 0.1826 0.7838 0.8454 0.200 Uiso 1 1 calc R . . Cl1 Cl 0.2705(2) 0.73780(15) 0.8482(3) 0.1843(15) Uani 1 1 d U . . Cl2 Cl 0.18699(17) 0.7469(2) 0.9694(2) 0.1766(13) Uani 1 1 d U . . 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 P1A 0.0428(6) 0.0493(6) 0.0400(6) -0.0009(5) 0.0031(5) 0.0023(5) B1A 0.047(3) 0.045(3) 0.051(3) -0.002(2) 0.006(2) 0.001(2) C1A 0.043(2) 0.048(2) 0.041(2) -0.002(2) 0.000(2) -0.002(2) C2A 0.042(2) 0.049(2) 0.039(2) -0.006(2) 0.003(2) -0.0031(19) C3A 0.044(2) 0.048(3) 0.039(2) 0.000(2) 0.000(2) -0.002(2) C4A 0.047(3) 0.063(3) 0.057(3) 0.005(2) -0.002(2) -0.001(2) C5A 0.041(3) 0.078(4) 0.069(4) 0.016(3) 0.001(2) -0.005(3) C6A 0.057(3) 0.054(3) 0.061(3) 0.007(3) 0.010(3) -0.008(2) C7A 0.061(3) 0.052(3) 0.044(3) 0.005(2) -0.001(2) 0.004(2) C8A 0.043(3) 0.052(3) 0.046(3) -0.003(2) 0.002(2) 0.001(2) C9A 0.082(4) 0.081(4) 0.092(5) 0.026(4) 0.026(4) -0.004(4) C11A 0.044(3) 0.058(3) 0.043(3) 0.000(2) -0.001(2) 0.003(2) C12A 0.045(3) 0.055(3) 0.054(3) -0.005(2) 0.004(2) 0.000(2) C13A 0.046(3) 0.064(3) 0.058(3) 0.007(3) -0.008(2) 0.006(2) C14A 0.055(3) 0.073(3) 0.060(3) 0.014(3) -0.010(3) 0.000(3) C15A 0.064(3) 0.078(4) 0.042(3) 0.001(2) -0.003(2) 0.001(3) C16A 0.054(3) 0.058(3) 0.042(3) 0.000(2) 0.002(2) 0.001(2) C17A 0.056(3) 0.073(3) 0.058(3) 0.002(3) 0.009(3) 0.012(3) C18A 0.072(4) 0.110(5) 0.069(4) 0.013(4) -0.022(3) 0.006(4) C19A 0.070(4) 0.080(4) 0.047(3) -0.002(3) 0.007(3) 0.015(3) C21A 0.042(2) 0.045(2) 0.052(3) 0.001(2) 0.004(2) 0.007(2) C22A 0.047(3) 0.050(3) 0.060(3) 0.003(2) 0.004(2) 0.005(2) C23A 0.059(3) 0.041(3) 0.081(4) 0.009(3) 0.005(3) 0.003(2) C24A 0.060(3) 0.046(3) 0.081(4) -0.003(3) 0.002(3) -0.001(2) C25A 0.062(3) 0.054(3) 0.055(3) -0.007(2) 0.003(3) 0.002(2) C26A 0.053(3) 0.045(3) 0.055(3) -0.003(2) 0.005(2) 0.003(2) C27A 0.074(4) 0.066(3) 0.061(3) 0.013(3) 0.013(3) -0.006(3) C28A 0.093(5) 0.053(3) 0.104(5) -0.012(3) 0.002(4) -0.011(3) C29A 0.066(3) 0.062(3) 0.042(3) -0.011(2) 0.004(2) -0.005(3) C31A 0.057(3) 0.044(2) 0.049(3) -0.004(2) 0.006(2) 0.003(2) C32A 0.063(3) 0.055(3) 0.058(3) -0.014(3) 0.005(3) 0.002(2) F32A 0.0586(19) 0.075(2) 0.076(2) -0.0245(17) 0.0032(16) -0.0071(15) C33A 0.087(4) 0.061(3) 0.061(4) -0.015(3) 0.006(3) -0.011(3) F33A 0.104(3) 0.093(3) 0.093(3) -0.041(2) -0.005(2) -0.019(2) C34A 0.105(5) 0.054(3) 0.063(4) -0.018(3) 0.014(4) 0.001(3) F34A 0.153(4) 0.074(2) 0.088(3) -0.041(2) 0.017(3) 0.010(2) C35A 0.089(4) 0.057(3) 0.071(4) -0.007(3) 0.022(3) 0.026(3) F35A 0.107(3) 0.096(3) 0.096(3) -0.017(2) 0.023(2) 0.045(2) C36A 0.056(3) 0.057(3) 0.057(3) -0.002(2) 0.008(3) 0.008(2) F36A 0.0605(19) 0.074(2) 0.074(2) 0.0006(17) 0.0063(16) 0.0159(16) C41A 0.052(3) 0.042(3) 0.056(3) 0.002(2) 0.005(2) 0.003(2) C42A 0.057(3) 0.039(2) 0.064(3) -0.001(2) 0.010(3) -0.001(2) F42A 0.0624(18) 0.0565(17) 0.080(2) -0.0040(16) 0.0108(17) -0.0106(14) C43A 0.073(4) 0.043(3) 0.081(4) 0.006(3) 0.022(3) -0.002(3) F43A 0.093(3) 0.0558(19) 0.116(3) 0.018(2) 0.031(2) -0.0153(17) C44A 0.089(4) 0.047(3) 0.065(4) 0.017(3) 0.013(3) 0.012(3) F44A 0.135(3) 0.072(2) 0.085(3) 0.040(2) 0.018(2) 0.013(2) C45A 0.072(4) 0.060(3) 0.063(3) 0.017(3) 0.000(3) 0.007(3) F45A 0.092(3) 0.089(2) 0.089(3) 0.034(2) -0.023(2) 0.004(2) C46A 0.052(3) 0.056(3) 0.057(3) 0.009(2) 0.001(2) 0.003(2) F46A 0.0506(16) 0.0681(18) 0.075(2) 0.0188(16) -0.0042(15) -0.0022(14) C51A 0.040(2) 0.049(2) 0.044(3) 0.004(2) 0.0007(19) 0.007(2) C52A 0.043(3) 0.057(3) 0.044(3) 0.003(2) 0.000(2) 0.002(2) F52A 0.0703(19) 0.0740(19) 0.0495(17) 0.0054(15) 0.0050(15) 0.0003(15) C53A 0.050(3) 0.063(3) 0.062(3) 0.024(3) 0.006(2) -0.003(2) F53A 0.085(2) 0.087(2) 0.077(2) 0.0344(19) 0.0101(19) -0.0155(19) C54A 0.055(3) 0.049(3) 0.081(4) 0.014(3) -0.012(3) -0.009(2) F54A 0.080(2) 0.0621(19) 0.118(3) 0.021(2) -0.019(2) -0.0287(17) C55A 0.058(3) 0.045(3) 0.061(3) -0.005(2) -0.009(3) -0.002(2) F55A 0.066(2) 0.0652(19) 0.086(2) -0.0127(18) -0.0188(17) -0.0099(15) C56A 0.042(2) 0.047(3) 0.054(3) 0.004(2) 0.002(2) 0.0010(19) F56A 0.0576(16) 0.0617(17) 0.0491(16) -0.0056(13) 0.0019(13) -0.0016(13) P1B 0.0376(6) 0.0371(5) 0.0371(5) 0.0020(5) 0.0030(5) 0.0018(4) B1B 0.039(3) 0.042(3) 0.033(2) -0.002(2) 0.008(2) -0.003(2) C1B 0.041(2) 0.037(2) 0.038(2) 0.0044(18) -0.0069(18) -0.0025(18) C2B 0.042(2) 0.041(2) 0.037(2) -0.0045(19) -0.0006(19) 0.0053(19) C3B 0.043(2) 0.038(2) 0.033(2) -0.0011(17) -0.0003(18) 0.0030(18) C4B 0.052(3) 0.046(3) 0.044(2) 0.004(2) 0.006(2) 0.005(2) C5B 0.078(4) 0.039(3) 0.055(3) 0.007(2) 0.004(3) 0.004(2) C6B 0.068(3) 0.045(3) 0.056(3) -0.001(2) -0.014(3) 0.009(2) C7B 0.051(3) 0.052(3) 0.072(4) 0.003(3) -0.021(3) 0.007(2) C8B 0.050(3) 0.046(2) 0.053(3) 0.006(2) -0.008(2) 0.002(2) C9B 0.104(5) 0.054(3) 0.097(5) 0.011(3) -0.031(4) 0.021(3) C11B 0.043(2) 0.042(2) 0.035(2) 0.0050(19) 0.0001(19) 0.0027(19) C12B 0.045(3) 0.048(2) 0.040(2) 0.005(2) 0.000(2) -0.005(2) C13B 0.062(3) 0.049(3) 0.050(3) 0.002(2) -0.002(2) -0.008(2) C14B 0.048(3) 0.067(3) 0.053(3) 0.007(3) -0.003(2) -0.017(2) C15B 0.043(3) 0.069(3) 0.055(3) 0.003(3) 0.002(2) -0.007(2) C16B 0.042(3) 0.049(3) 0.046(3) 0.006(2) 0.004(2) 0.004(2) C17B 0.057(3) 0.043(2) 0.056(3) -0.002(2) 0.011(2) 0.003(2) C18B 0.064(4) 0.088(4) 0.094(5) -0.001(4) -0.002(3) -0.029(3) C19B 0.050(3) 0.058(3) 0.060(3) -0.003(3) 0.013(2) 0.004(2) C21B 0.035(2) 0.042(2) 0.039(2) 0.0042(18) 0.0037(18) 0.0025(18) C22B 0.039(2) 0.043(2) 0.043(2) 0.0036(19) 0.0034(19) -0.0002(19) C23B 0.048(3) 0.057(3) 0.037(2) 0.005(2) 0.000(2) 0.003(2) C24B 0.040(3) 0.062(3) 0.040(3) -0.004(2) 0.001(2) 0.003(2) C25B 0.058(3) 0.049(3) 0.040(3) -0.006(2) -0.001(2) 0.003(2) C26B 0.047(3) 0.045(2) 0.039(2) 0.0026(19) 0.003(2) 0.004(2) C27B 0.060(3) 0.045(3) 0.048(3) 0.006(2) -0.007(2) 0.004(2) C28B 0.064(3) 0.077(4) 0.045(3) -0.009(3) -0.010(2) 0.006(3) C29B 0.079(3) 0.041(2) 0.043(3) -0.006(2) -0.001(2) 0.014(2) C31B 0.041(2) 0.041(2) 0.038(2) -0.0043(18) 0.0050(19) 0.0012(18) C32B 0.044(2) 0.049(2) 0.037(2) 0.000(2) 0.0000(19) -0.002(2) F32B 0.0478(15) 0.0602(16) 0.0463(15) 0.0001(13) -0.0070(12) -0.0062(13) C33B 0.061(3) 0.047(2) 0.036(2) 0.004(2) 0.002(2) 0.002(2) F33B 0.084(2) 0.0692(19) 0.0462(16) 0.0101(14) -0.0127(15) 0.0032(16) C34B 0.070(3) 0.045(2) 0.045(3) 0.008(2) 0.008(2) -0.001(2) F34B 0.100(3) 0.0578(17) 0.0625(19) 0.0222(15) 0.0100(18) -0.0085(17) C35B 0.051(3) 0.043(2) 0.055(3) 0.002(2) 0.012(2) -0.011(2) F35B 0.069(2) 0.0596(17) 0.086(2) 0.0122(16) 0.0079(17) -0.0226(15) C36B 0.042(2) 0.049(2) 0.044(2) -0.002(2) 0.002(2) -0.003(2) F36B 0.0417(14) 0.0606(16) 0.0611(17) 0.0021(13) -0.0053(13) -0.0069(13) C41B 0.038(2) 0.041(2) 0.034(2) 0.0010(18) 0.0012(18) -0.0012(18) C42B 0.032(2) 0.047(2) 0.044(2) -0.002(2) -0.0030(18) 0.0013(19) F42B 0.0391(14) 0.0545(15) 0.0628(17) -0.0129(13) -0.0026(12) -0.0027(12) C43B 0.049(3) 0.043(2) 0.048(3) -0.009(2) -0.002(2) -0.006(2) F43B 0.0667(19) 0.0619(18) 0.077(2) -0.0211(16) -0.0171(16) -0.0095(15) C44B 0.068(3) 0.041(2) 0.039(2) -0.011(2) 0.005(2) 0.007(2) F44B 0.091(2) 0.0600(18) 0.0626(19) -0.0282(15) 0.0015(17) 0.0112(16) C45B 0.039(3) 0.053(3) 0.045(3) -0.002(2) 0.007(2) 0.010(2) F45B 0.0545(17) 0.0767(19) 0.0609(18) -0.0113(15) 0.0090(14) 0.0162(15) C46B 0.033(2) 0.047(2) 0.039(2) -0.0010(19) -0.0011(18) -0.0014(18) F46B 0.0368(14) 0.0642(16) 0.0551(16) -0.0066(13) 0.0018(12) -0.0014(12) C51B 0.035(2) 0.047(2) 0.035(2) -0.0008(19) 0.0032(18) -0.0020(18) C52B 0.047(2) 0.046(2) 0.037(2) -0.001(2) -0.002(2) 0.000(2) F52B 0.0727(18) 0.0446(14) 0.0511(16) 0.0010(12) -0.0086(14) 0.0042(13) C53B 0.044(3) 0.059(3) 0.044(3) 0.007(2) -0.004(2) 0.001(2) F53B 0.088(2) 0.0684(18) 0.0545(18) 0.0137(15) -0.0196(16) 0.0141(17) C54B 0.053(3) 0.069(3) 0.029(2) -0.001(2) -0.007(2) -0.006(2) F54B 0.072(2) 0.094(2) 0.0397(15) -0.0007(15) -0.0151(14) -0.0043(17) C55B 0.051(3) 0.054(3) 0.038(2) -0.012(2) 0.001(2) -0.009(2) F55B 0.075(2) 0.0657(17) 0.0485(16) -0.0202(14) -0.0071(14) -0.0090(15) C56B 0.044(2) 0.044(2) 0.040(2) 0.000(2) 0.000(2) 0.0060(19) F56B 0.0627(17) 0.0479(14) 0.0503(15) -0.0080(12) -0.0046(13) 0.0050(12) C101 0.188(8) 0.122(6) 0.141(7) 0.007(6) -0.031(7) -0.040(6) C102 0.173(8) 0.098(5) 0.110(6) -0.003(5) -0.001(6) -0.035(5) C103 0.119(6) 0.088(5) 0.149(7) -0.010(5) 0.011(6) -0.029(4) C104 0.174(8) 0.160(8) 0.158(8) 0.011(7) -0.022(7) -0.042(7) C105 0.122(6) 0.079(4) 0.125(6) 0.002(4) -0.009(5) -0.010(4) C201 0.132(7) 0.142(7) 0.226(9) 0.065(7) 0.017(7) -0.017(6) Cl1 0.201(3) 0.131(2) 0.221(4) -0.012(2) 0.072(3) -0.006(2) Cl2 0.152(3) 0.229(4) 0.149(3) -0.029(3) 0.000(2) 0.001(2) _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 P1A C2A 1.755(5) . ? P1A C1A 1.793(5) . ? P1A C11A 1.802(5) . ? P1A C21A 1.809(5) . ? B1A C31A 1.630(7) . ? B1A C1A 1.647(7) . ? B1A C41A 1.650(8) . ? B1A C51A 1.653(7) . ? C1A C2A 1.325(6) . ? C2A C3A 1.464(7) . ? C3A C8A 1.387(7) . ? C3A C4A 1.395(7) . ? C4A C5A 1.377(8) . ? C4A H4A 0.9400 . ? C5A C6A 1.381(8) . ? C5A H5A 0.9400 . ? C6A C7A 1.388(7) . ? C6A C9A 1.506(8) . ? C7A C8A 1.385(7) . ? C7A H7A 0.9400 . ? C8A H8A 0.9400 . ? C9A H9AA 0.9700 . ? C9A H9AB 0.9700 . ? C9A H9AC 0.9700 . ? C11A C16A 1.414(7) . ? C11A C12A 1.415(7) . ? C12A C13A 1.391(7) . ? C12A C17A 1.494(8) . ? C13A C14A 1.396(8) . ? C13A H13A 0.9400 . ? C14A C15A 1.391(8) . ? C14A C18A 1.499(8) . ? C15A C16A 1.372(7) . ? C15A H15A 0.9400 . ? C16A C19A 1.514(7) . ? C17A H17A 0.9700 . ? C17A H17B 0.9700 . ? C17A H17C 0.9700 . ? C18A H18A 0.9700 . ? C18A H18B 0.9700 . ? C18A H18C 0.9700 . ? C19A H19A 0.9700 . ? C19A H19B 0.9700 . ? C19A H19C 0.9700 . ? C21A C26A 1.411(7) . ? C21A C22A 1.419(7) . ? C22A C23A 1.393(8) . ? C22A C27A 1.508(8) . ? C23A C24A 1.389(9) . ? C23A H23A 0.9400 . ? C24A C25A 1.381(8) . ? C24A C28A 1.513(8) . ? C25A C26A 1.396(7) . ? C25A H25A 0.9400 . ? C26A C29A 1.492(7) . ? C27A H27A 0.9700 . ? C27A H27B 0.9700 . ? C27A H27C 0.9700 . ? C28A H28A 0.9700 . ? C28A H28B 0.9700 . ? C28A H28C 0.9700 . ? C29A H29A 0.9700 . ? C29A H29B 0.9700 . ? C29A H29C 0.9700 . ? C31A C32A 1.375(8) . ? C31A C36A 1.387(7) . ? C32A F32A 1.359(6) . ? C32A C33A 1.394(8) . ? C33A F33A 1.342(7) . ? C33A C34A 1.355(9) . ? C34A F34A 1.346(7) . ? C34A C35A 1.383(10) . ? C35A F35A 1.340(7) . ? C35A C36A 1.393(8) . ? C36A F36A 1.343(6) . ? C41A C42A 1.390(7) . ? C41A C46A 1.393(7) . ? C42A F42A 1.350(7) . ? C42A C43A 1.366(8) . ? C43A F43A 1.345(6) . ? C43A C44A 1.384(9) . ? C44A F44A 1.335(7) . ? C44A C45A 1.366(9) . ? C45A F45A 1.336(7) . ? C45A C46A 1.386(7) . ? C46A F46A 1.354(6) . ? C51A C56A 1.374(7) . ? C51A C52A 1.381(7) . ? C52A F52A 1.355(6) . ? C52A C53A 1.384(7) . ? C53A F53A 1.342(6) . ? C53A C54A 1.357(9) . ? C54A F54A 1.361(6) . ? C54A C55A 1.386(8) . ? C55A F55A 1.346(6) . ? C55A C56A 1.361(7) . ? C56A F56A 1.365(6) . ? P1B C2B 1.746(4) . ? P1B C1B 1.799(5) . ? P1B C21B 1.807(5) . ? P1B C11B 1.809(4) . ? B1B C1B 1.629(7) . ? B1B C41B 1.634(6) . ? B1B C31B 1.646(7) . ? B1B C51B 1.654(7) . ? C1B C2B 1.330(6) . ? C2B C3B 1.477(6) . ? C3B C4B 1.376(6) . ? C3B C8B 1.387(7) . ? C4B C5B 1.391(7) . ? C4B H4B 0.9400 . ? C5B C6B 1.375(8) . ? C5B H5B 0.9400 . ? C6B C7B 1.384(8) . ? C6B C9B 1.516(7) . ? C7B C8B 1.388(7) . ? C7B H7B 0.9400 . ? C8B H8B 0.9400 . ? C9B H9BA 0.9700 . ? C9B H9BB 0.9700 . ? C9B H9BC 0.9700 . ? C11B C16B 1.407(6) . ? C11B C12B 1.422(6) . ? C12B C13B 1.406(7) . ? C12B C17B 1.475(7) . ? C13B C14B 1.385(7) . ? C13B H13B 0.9400 . ? C14B C15B 1.373(8) . ? C14B C18B 1.512(7) . ? C15B C16B 1.392(7) . ? C15B H15B 0.9400 . ? C16B C19B 1.513(7) . ? C17B H17D 0.9700 . ? C17B H17E 0.9700 . ? C17B H17F 0.9700 . ? C18B H18D 0.9700 . ? C18B H18E 0.9700 . ? C18B H18F 0.9700 . ? C19B H19D 0.9700 . ? C19B H19E 0.9700 . ? C19B H19F 0.9700 . ? C21B C22B 1.411(6) . ? C21B C26B 1.418(6) . ? C22B C23B 1.388(7) . ? C22B C27B 1.518(7) . ? C23B C24B 1.393(7) . ? C23B H23B 0.9400 . ? C24B C25B 1.389(7) . ? C24B C28B 1.497(7) . ? C25B C26B 1.386(7) . ? C25B H25B 0.9400 . ? C26B C29B 1.512(7) . ? C27B H27D 0.9700 . ? C27B H27E 0.9700 . ? C27B H27F 0.9700 . ? C28B H28D 0.9700 . ? C28B H28E 0.9700 . ? C28B H28F 0.9700 . ? C29B H29D 0.9700 . ? C29B H29E 0.9700 . ? C29B H29F 0.9700 . ? C31B C36B 1.375(6) . ? C31B C32B 1.402(6) . ? C32B F32B 1.348(5) . ? C32B C33B 1.380(6) . ? C33B F33B 1.338(6) . ? C33B C34B 1.369(7) . ? C34B F34B 1.358(6) . ? C34B C35B 1.361(8) . ? C35B F35B 1.334(5) . ? C35B C36B 1.404(7) . ? C36B F36B 1.353(5) . ? C41B C46B 1.379(6) . ? C41B C42B 1.387(6) . ? C42B F42B 1.354(5) . ? C42B C43B 1.373(6) . ? C43B F43B 1.343(5) . ? C43B C44B 1.365(7) . ? C44B F44B 1.343(5) . ? C44B C45B 1.384(7) . ? C45B F45B 1.350(5) . ? C45B C46B 1.369(6) . ? C46B F46B 1.360(5) . ? C51B C52B 1.391(6) . ? C51B C56B 1.394(6) . ? C52B F52B 1.357(5) . ? C52B C53B 1.382(7) . ? C53B F53B 1.336(6) . ? C53B C54B 1.355(7) . ? C54B F54B 1.356(5) . ? C54B C55B 1.367(7) . ? C55B F55B 1.352(5) . ? C55B C56B 1.371(7) . ? C56B F56B 1.361(5) . ? C101 C102 1.323(8) . ? C101 H10A 0.9700 . ? C101 H10B 0.9700 . ? C101 H10C 0.9700 . ? C102 C103 1.311(7) . ? C102 H10D 0.9800 . ? C102 H10E 0.9800 . ? C103 C104 1.355(8) . ? C103 H10F 0.9800 . ? C103 H10G 0.9800 . ? C104 C105 1.336(8) . ? C104 H10H 0.9800 . ? C104 H10I 0.9800 . ? C105 H10J 0.9700 . ? C105 H10K 0.9700 . ? C105 H10L 0.9700 . ? C201 Cl1 1.636(12) . ? C201 Cl2 1.858(16) . ? C201 H20A 0.9800 . ? C201 H20B 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 C2A P1A C1A 43.8(2) . . ? C2A P1A C11A 118.8(2) . . ? C1A P1A C11A 125.2(2) . . ? C2A P1A C21A 120.3(2) . . ? C1A P1A C21A 117.8(2) . . ? C11A P1A C21A 113.5(2) . . ? C31A B1A C1A 112.9(4) . . ? C31A B1A C41A 104.9(4) . . ? C1A B1A C41A 108.7(4) . . ? C31A B1A C51A 115.8(4) . . ? C1A B1A C51A 100.7(4) . . ? C41A B1A C51A 113.9(4) . . ? C2A C1A B1A 148.8(5) . . ? C2A C1A P1A 66.6(3) . . ? B1A C1A P1A 142.5(4) . . ? C1A C2A C3A 144.4(5) . . ? C1A C2A P1A 69.6(3) . . ? C3A C2A P1A 146.0(4) . . ? C8A C3A C4A 118.5(4) . . ? C8A C3A C2A 121.3(4) . . ? C4A C3A C2A 120.1(4) . . ? C5A C4A C3A 120.0(5) . . ? C5A C4A H4A 120.0 . . ? C3A C4A H4A 120.0 . . ? C4A C5A C6A 122.1(5) . . ? C4A C5A H5A 118.9 . . ? C6A C5A H5A 118.9 . . ? C5A C6A C7A 117.6(5) . . ? C5A C6A C9A 120.8(5) . . ? C7A C6A C9A 121.7(6) . . ? C8A C7A C6A 121.3(5) . . ? C8A C7A H7A 119.4 . . ? C6A C7A H7A 119.4 . . ? C7A C8A C3A 120.5(5) . . ? C7A C8A H8A 119.8 . . ? C3A C8A H8A 119.8 . . ? C6A C9A H9AA 109.5 . . ? C6A C9A H9AB 109.5 . . ? H9AA C9A H9AB 109.5 . . ? C6A C9A H9AC 109.5 . . ? H9AA C9A H9AC 109.5 . . ? H9AB C9A H9AC 109.5 . . ? C16A C11A C12A 120.6(4) . . ? C16A C11A P1A 123.6(4) . . ? C12A C11A P1A 115.8(4) . . ? C13A C12A C11A 117.7(5) . . ? C13A C12A C17A 119.3(5) . . ? C11A C12A C17A 122.9(5) . . ? C12A C13A C14A 122.6(5) . . ? C12A C13A H13A 118.7 . . ? C14A C13A H13A 118.7 . . ? C15A C14A C13A 117.5(5) . . ? C15A C14A C18A 121.3(6) . . ? C13A C14A C18A 121.2(5) . . ? C16A C15A C14A 122.9(5) . . ? C16A C15A H15A 118.6 . . ? C14A C15A H15A 118.6 . . ? C15A C16A C11A 118.6(5) . . ? C15A C16A C19A 116.7(5) . . ? C11A C16A C19A 124.7(5) . . ? C12A C17A H17A 109.5 . . ? C12A C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? C12A C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? C14A C18A H18A 109.5 . . ? C14A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? C14A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? C16A C19A H19A 109.5 . . ? C16A C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C16A C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? C26A C21A C22A 120.1(5) . . ? C26A C21A P1A 121.4(4) . . ? C22A C21A P1A 118.2(4) . . ? C23A C22A C21A 118.4(5) . . ? C23A C22A C27A 117.7(5) . . ? C21A C22A C27A 123.9(5) . . ? C24A C23A C22A 122.9(5) . . ? C24A C23A H23A 118.6 . . ? C22A C23A H23A 118.6 . . ? C25A C24A C23A 117.0(5) . . ? C25A C24A C28A 122.8(6) . . ? C23A C24A C28A 120.2(6) . . ? C24A C25A C26A 123.7(5) . . ? C24A C25A H25A 118.1 . . ? C26A C25A H25A 118.1 . . ? C25A C26A C21A 117.9(5) . . ? C25A C26A C29A 118.2(5) . . ? C21A C26A C29A 123.9(5) . . ? C22A C27A H27A 109.5 . . ? C22A C27A H27B 109.5 . . ? H27A C27A H27B 109.5 . . ? C22A C27A H27C 109.5 . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? C24A C28A H28A 109.5 . . ? C24A C28A H28B 109.5 . . ? H28A C28A H28B 109.5 . . ? C24A C28A H28C 109.5 . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? C26A C29A H29A 109.5 . . ? C26A C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? C26A C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? C32A C31A C36A 114.2(5) . . ? C32A C31A B1A 126.5(5) . . ? C36A C31A B1A 118.9(5) . . ? F32A C32A C31A 120.8(4) . . ? F32A C32A C33A 114.8(5) . . ? C31A C32A C33A 124.4(5) . . ? F33A C33A C34A 120.8(5) . . ? F33A C33A C32A 120.2(6) . . ? C34A C33A C32A 119.0(6) . . ? F34A C34A C33A 120.5(6) . . ? F34A C34A C35A 119.7(6) . . ? C33A C34A C35A 119.8(5) . . ? F35A C35A C34A 120.6(5) . . ? F35A C35A C36A 120.3(6) . . ? C34A C35A C36A 119.1(5) . . ? F36A C36A C31A 119.3(5) . . ? F36A C36A C35A 117.3(5) . . ? C31A C36A C35A 123.4(6) . . ? C42A C41A C46A 113.3(5) . . ? C42A C41A B1A 120.1(5) . . ? C46A C41A B1A 126.6(4) . . ? F42A C42A C43A 116.6(5) . . ? F42A C42A C41A 119.1(5) . . ? C43A C42A C41A 124.4(6) . . ? F43A C43A C42A 120.7(6) . . ? F43A C43A C44A 119.5(5) . . ? C42A C43A C44A 119.8(5) . . ? F44A C44A C45A 120.6(6) . . ? F44A C44A C43A 120.6(6) . . ? C45A C44A C43A 118.8(5) . . ? F45A C45A C44A 120.2(5) . . ? F45A C45A C46A 120.3(5) . . ? C44A C45A C46A 119.5(6) . . ? F46A C46A C45A 115.3(5) . . ? F46A C46A C41A 120.7(4) . . ? C45A C46A C41A 124.0(5) . . ? C56A C51A C52A 113.2(4) . . ? C56A C51A B1A 120.0(4) . . ? C52A C51A B1A 126.4(4) . . ? F52A C52A C51A 121.0(4) . . ? F52A C52A C53A 115.0(4) . . ? C51A C52A C53A 123.9(5) . . ? F53A C53A C54A 120.6(5) . . ? F53A C53A C52A 120.2(5) . . ? C54A C53A C52A 119.2(5) . . ? C53A C54A F54A 120.2(5) . . ? C53A C54A C55A 119.8(5) . . ? F54A C54A C55A 119.9(6) . . ? F55A C55A C56A 122.1(5) . . ? F55A C55A C54A 119.9(5) . . ? C56A C55A C54A 118.0(5) . . ? C55A C56A F56A 114.9(5) . . ? C55A C56A C51A 125.8(5) . . ? F56A C56A C51A 119.3(4) . . ? C2B P1B C1B 44.0(2) . . ? C2B P1B C21B 120.5(2) . . ? C1B P1B C21B 120.3(2) . . ? C2B P1B C11B 116.5(2) . . ? C1B P1B C11B 123.0(2) . . ? C21B P1B C11B 114.2(2) . . ? C1B B1B C41B 114.4(4) . . ? C1B B1B C31B 110.6(4) . . ? C41B B1B C31B 104.0(3) . . ? C1B B1B C51B 98.7(3) . . ? C41B B1B C51B 115.5(4) . . ? C31B B1B C51B 114.1(4) . . ? C2B C1B B1B 150.2(4) . . ? C2B C1B P1B 65.8(3) . . ? B1B C1B P1B 141.0(3) . . ? C1B C2B C3B 142.6(4) . . ? C1B C2B P1B 70.1(3) . . ? C3B C2B P1B 147.1(3) . . ? C4B C3B C8B 119.2(4) . . ? C4B C3B C2B 120.5(4) . . ? C8B C3B C2B 120.3(4) . . ? C3B C4B C5B 119.8(5) . . ? C3B C4B H4B 120.1 . . ? C5B C4B H4B 120.1 . . ? C6B C5B C4B 121.5(5) . . ? C6B C5B H5B 119.2 . . ? C4B C5B H5B 119.2 . . ? C5B C6B C7B 118.4(5) . . ? C5B C6B C9B 120.9(5) . . ? C7B C6B C9B 120.7(5) . . ? C6B C7B C8B 120.6(5) . . ? C6B C7B H7B 119.7 . . ? C8B C7B H7B 119.7 . . ? C3B C8B C7B 120.4(5) . . ? C3B C8B H8B 119.8 . . ? C7B C8B H8B 119.8 . . ? C6B C9B H9BA 109.5 . . ? C6B C9B H9BB 109.5 . . ? H9BA C9B H9BB 109.5 . . ? C6B C9B H9BC 109.5 . . ? H9BA C9B H9BC 109.5 . . ? H9BB C9B H9BC 109.5 . . ? C16B C11B C12B 121.1(4) . . ? C16B C11B P1B 116.0(3) . . ? C12B C11B P1B 122.8(3) . . ? C13B C12B C11B 117.0(4) . . ? C13B C12B C17B 117.6(4) . . ? C11B C12B C17B 125.3(4) . . ? C14B C13B C12B 122.3(5) . . ? C14B C13B H13B 118.9 . . ? C12B C13B H13B 118.9 . . ? C15B C14B C13B 118.9(5) . . ? C15B C14B C18B 120.7(5) . . ? C13B C14B C18B 120.4(5) . . ? C14B C15B C16B 122.4(5) . . ? C14B C15B H15B 118.8 . . ? C16B C15B H15B 118.8 . . ? C15B C16B C11B 118.1(5) . . ? C15B C16B C19B 118.8(4) . . ? C11B C16B C19B 123.1(4) . . ? C12B C17B H17D 109.5 . . ? C12B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? C12B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? C14B C18B H18D 109.5 . . ? C14B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C14B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C16B C19B H19D 109.5 . . ? C16B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C16B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C22B C21B C26B 119.6(4) . . ? C22B C21B P1B 119.0(3) . . ? C26B C21B P1B 121.3(3) . . ? C23B C22B C21B 118.6(4) . . ? C23B C22B C27B 117.6(4) . . ? C21B C22B C27B 123.8(4) . . ? C22B C23B C24B 123.0(4) . . ? C22B C23B H23B 118.5 . . ? C24B C23B H23B 118.5 . . ? C25B C24B C23B 117.0(4) . . ? C25B C24B C28B 120.8(5) . . ? C23B C24B C28B 122.2(5) . . ? C26B C25B C24B 122.9(4) . . ? C26B C25B H25B 118.5 . . ? C24B C25B H25B 118.5 . . ? C25B C26B C21B 118.7(4) . . ? C25B C26B C29B 116.9(4) . . ? C21B C26B C29B 124.3(4) . . ? C22B C27B H27D 109.5 . . ? C22B C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? C22B C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? C24B C28B H28D 109.5 . . ? C24B C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? C24B C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? C26B C29B H29D 109.5 . . ? C26B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C26B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C36B C31B C32B 113.2(4) . . ? C36B C31B B1B 126.8(4) . . ? C32B C31B B1B 119.7(4) . . ? F32B C32B C33B 116.0(4) . . ? F32B C32B C31B 119.4(4) . . ? C33B C32B C31B 124.5(4) . . ? F33B C33B C34B 121.2(4) . . ? F33B C33B C32B 120.1(4) . . ? C34B C33B C32B 118.7(4) . . ? F34B C34B C35B 119.6(5) . . ? F34B C34B C33B 120.0(5) . . ? C35B C34B C33B 120.3(4) . . ? F35B C35B C34B 120.8(4) . . ? F35B C35B C36B 120.4(5) . . ? C34B C35B C36B 118.9(4) . . ? F36B C36B C31B 120.8(4) . . ? F36B C36B C35B 115.0(4) . . ? C31B C36B C35B 124.2(5) . . ? C46B C41B C42B 113.2(4) . . ? C46B C41B B1B 121.2(4) . . ? C42B C41B B1B 125.1(4) . . ? F42B C42B C43B 115.7(4) . . ? F42B C42B C41B 120.3(4) . . ? C43B C42B C41B 124.0(4) . . ? F43B C43B C44B 119.4(4) . . ? F43B C43B C42B 120.5(4) . . ? C44B C43B C42B 120.1(4) . . ? F44B C44B C43B 121.4(4) . . ? F44B C44B C45B 119.9(4) . . ? C43B C44B C45B 118.7(4) . . ? F45B C45B C46B 121.5(4) . . ? F45B C45B C44B 119.5(4) . . ? C46B C45B C44B 119.0(4) . . ? F46B C46B C45B 115.7(4) . . ? F46B C46B C41B 119.2(4) . . ? C45B C46B C41B 125.0(4) . . ? C52B C51B C56B 112.1(4) . . ? C52B C51B B1B 126.4(4) . . ? C56B C51B B1B 120.8(4) . . ? F52B C52B C53B 115.8(4) . . ? F52B C52B C51B 119.6(4) . . ? C53B C52B C51B 124.6(4) . . ? F53B C53B C54B 120.9(4) . . ? F53B C53B C52B 119.7(4) . . ? C54B C53B C52B 119.3(4) . . ? C53B C54B F54B 120.4(5) . . ? C53B C54B C55B 119.9(4) . . ? F54B C54B C55B 119.7(4) . . ? F55B C55B C54B 120.4(4) . . ? F55B C55B C56B 120.8(4) . . ? C54B C55B C56B 118.8(4) . . ? F56B C56B C55B 116.0(4) . . ? F56B C56B C51B 118.7(4) . . ? C55B C56B C51B 125.3(4) . . ? C102 C101 H10A 109.5 . . ? C102 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C102 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? C103 C102 C101 132.6(11) . . ? C103 C102 H10D 104.1 . . ? C101 C102 H10D 104.1 . . ? C103 C102 H10E 104.1 . . ? C101 C102 H10E 104.1 . . ? H10D C102 H10E 105.5 . . ? C102 C103 C104 123.9(10) . . ? C102 C103 H10F 106.4 . . ? C104 C103 H10F 106.4 . . ? C102 C103 H10G 106.4 . . ? C104 C103 H10G 106.4 . . ? H10F C103 H10G 106.4 . . ? C105 C104 C103 127.6(11) . . ? C105 C104 H10H 105.4 . . ? C103 C104 H10H 105.4 . . ? C105 C104 H10I 105.4 . . ? C103 C104 H10I 105.4 . . ? H10H C104 H10I 106.0 . . ? C104 C105 H10J 109.5 . . ? C104 C105 H10K 109.5 . . ? H10J C105 H10K 109.5 . . ? C104 C105 H10L 109.5 . . ? H10J C105 H10L 109.5 . . ? H10K C105 H10L 109.5 . . ? Cl1 C201 Cl2 108.6(8) . . ? Cl1 C201 H20A 110.0 . . ? Cl2 C201 H20A 110.0 . . ? Cl1 C201 H20B 110.0 . . ? Cl2 C201 H20B 110.0 . . ? H20A C201 H20B 108.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C31A B1A C1A C2A -112.7(8) . . . . ? C41A B1A C1A C2A 3.2(10) . . . . ? C51A B1A C1A C2A 123.2(8) . . . . ? C31A B1A C1A P1A 94.7(6) . . . . ? C41A B1A C1A P1A -149.4(5) . . . . ? C51A B1A C1A P1A -29.5(7) . . . . ? C11A P1A C1A C2A 96.6(3) . . . . ? C21A P1A C1A C2A -105.9(3) . . . . ? C2A P1A C1A B1A 164.9(7) . . . . ? C11A P1A C1A B1A -98.5(6) . . . . ? C21A P1A C1A B1A 59.0(6) . . . . ? B1A C1A C2A C3A 20.8(13) . . . . ? P1A C1A C2A C3A -177.0(8) . . . . ? B1A C1A C2A P1A -162.2(8) . . . . ? C11A P1A C2A C1A -112.2(3) . . . . ? C21A P1A C2A C1A 99.9(3) . . . . ? C1A P1A C2A C3A 176.8(8) . . . . ? C11A P1A C2A C3A 64.6(7) . . . . ? C21A P1A C2A C3A -83.3(7) . . . . ? C1A C2A C3A C8A -54.1(9) . . . . ? P1A C2A C3A C8A 131.0(6) . . . . ? C1A C2A C3A C4A 123.5(7) . . . . ? P1A C2A C3A C4A -51.4(9) . . . . ? C8A C3A C4A C5A -0.7(8) . . . . ? C2A C3A C4A C5A -178.4(5) . . . . ? C3A C4A C5A C6A 0.3(9) . . . . ? C4A C5A C6A C7A 0.2(9) . . . . ? C4A C5A C6A C9A -179.3(6) . . . . ? C5A C6A C7A C8A -0.4(8) . . . . ? C9A C6A C7A C8A 179.2(5) . . . . ? C6A C7A C8A C3A 0.0(8) . . . . ? C4A C3A C8A C7A 0.5(7) . . . . ? C2A C3A C8A C7A 178.2(4) . . . . ? C2A P1A C11A C16A 100.6(5) . . . . ? C1A P1A C11A C16A 48.9(5) . . . . ? C21A P1A C11A C16A -109.4(5) . . . . ? C2A P1A C11A C12A -81.0(4) . . . . ? C1A P1A C11A C12A -132.7(4) . . . . ? C21A P1A C11A C12A 69.0(4) . . . . ? C16A C11A C12A C13A 0.2(7) . . . . ? P1A C11A C12A C13A -178.2(4) . . . . ? C16A C11A C12A C17A -179.8(5) . . . . ? P1A C11A C12A C17A 1.8(7) . . . . ? C11A C12A C13A C14A -0.7(8) . . . . ? C17A C12A C13A C14A 179.3(5) . . . . ? C12A C13A C14A C15A 0.4(8) . . . . ? C12A C13A C14A C18A -179.9(6) . . . . ? C13A C14A C15A C16A 0.6(9) . . . . ? C18A C14A C15A C16A -179.1(6) . . . . ? C14A C15A C16A C11A -1.1(8) . . . . ? C14A C15A C16A C19A 177.0(5) . . . . ? C12A C11A C16A C15A 0.7(8) . . . . ? P1A C11A C16A C15A 179.0(4) . . . . ? C12A C11A C16A C19A -177.3(5) . . . . ? P1A C11A C16A C19A 1.0(8) . . . . ? C2A P1A C21A C26A 20.1(5) . . . . ? C1A P1A C21A C26A 70.6(5) . . . . ? C11A P1A C21A C26A -129.4(4) . . . . ? C2A P1A C21A C22A -153.9(4) . . . . ? C1A P1A C21A C22A -103.5(4) . . . . ? C11A P1A C21A C22A 56.6(4) . . . . ? C26A C21A C22A C23A -1.4(7) . . . . ? P1A C21A C22A C23A 172.7(4) . . . . ? C26A C21A C22A C27A 178.9(5) . . . . ? P1A C21A C22A C27A -7.0(7) . . . . ? C21A C22A C23A C24A -0.8(8) . . . . ? C27A C22A C23A C24A 178.9(5) . . . . ? C22A C23A C24A C25A 3.0(8) . . . . ? C22A C23A C24A C28A -176.5(5) . . . . ? C23A C24A C25A C26A -3.0(8) . . . . ? C28A C24A C25A C26A 176.4(6) . . . . ? C24A C25A C26A C21A 0.9(8) . . . . ? C24A C25A C26A C29A -179.0(5) . . . . ? C22A C21A C26A C25A 1.4(7) . . . . ? P1A C21A C26A C25A -172.6(4) . . . . ? C22A C21A C26A C29A -178.6(5) . . . . ? P1A C21A C26A C29A 7.4(7) . . . . ? C1A B1A C31A C32A 15.6(7) . . . . ? C41A B1A C31A C32A -102.6(6) . . . . ? C51A B1A C31A C32A 131.0(5) . . . . ? C1A B1A C31A C36A -172.4(4) . . . . ? C41A B1A C31A C36A 69.4(6) . . . . ? C51A B1A C31A C36A -57.0(6) . . . . ? C36A C31A C32A F32A -178.5(5) . . . . ? B1A C31A C32A F32A -6.1(8) . . . . ? C36A C31A C32A C33A 4.0(8) . . . . ? B1A C31A C32A C33A 176.4(6) . . . . ? F32A C32A C33A F33A -0.2(8) . . . . ? C31A C32A C33A F33A 177.5(5) . . . . ? F32A C32A C33A C34A 179.1(5) . . . . ? C31A C32A C33A C34A -3.2(10) . . . . ? F33A C33A C34A F34A 0.6(10) . . . . ? C32A C33A C34A F34A -178.7(6) . . . . ? F33A C33A C34A C35A -179.7(6) . . . . ? C32A C33A C34A C35A 1.0(10) . . . . ? F34A C34A C35A F35A 0.3(9) . . . . ? C33A C34A C35A F35A -179.4(6) . . . . ? F34A C34A C35A C36A 179.7(5) . . . . ? C33A C34A C35A C36A 0.1(10) . . . . ? C32A C31A C36A F36A 178.3(5) . . . . ? B1A C31A C36A F36A 5.3(7) . . . . ? C32A C31A C36A C35A -2.9(8) . . . . ? B1A C31A C36A C35A -175.8(5) . . . . ? F35A C35A C36A F36A -0.7(8) . . . . ? C34A C35A C36A F36A 179.8(5) . . . . ? F35A C35A C36A C31A -179.6(5) . . . . ? C34A C35A C36A C31A 0.9(9) . . . . ? C31A B1A C41A C42A 65.7(6) . . . . ? C1A B1A C41A C42A -55.3(6) . . . . ? C51A B1A C41A C42A -166.7(4) . . . . ? C31A B1A C41A C46A -112.2(6) . . . . ? C1A B1A C41A C46A 126.7(5) . . . . ? C51A B1A C41A C46A 15.4(7) . . . . ? C46A C41A C42A F42A 177.1(4) . . . . ? B1A C41A C42A F42A -1.1(7) . . . . ? C46A C41A C42A C43A -4.1(8) . . . . ? B1A C41A C42A C43A 177.7(5) . . . . ? F42A C42A C43A F43A 1.8(7) . . . . ? C41A C42A C43A F43A -177.1(5) . . . . ? F42A C42A C43A C44A 178.9(5) . . . . ? C41A C42A C43A C44A 0.0(8) . . . . ? F43A C43A C44A F44A -0.5(8) . . . . ? C42A C43A C44A F44A -177.6(5) . . . . ? F43A C43A C44A C45A -178.6(5) . . . . ? C42A C43A C44A C45A 4.3(8) . . . . ? F44A C44A C45A F45A 0.0(9) . . . . ? C43A C44A C45A F45A 178.2(5) . . . . ? F44A C44A C45A C46A 177.8(5) . . . . ? C43A C44A C45A C46A -4.1(9) . . . . ? F45A C45A C46A F46A -3.6(8) . . . . ? C44A C45A C46A F46A 178.6(5) . . . . ? F45A C45A C46A C41A 177.4(5) . . . . ? C44A C45A C46A C41A -0.4(9) . . . . ? C42A C41A C46A F46A -174.7(5) . . . . ? B1A C41A C46A F46A 3.4(8) . . . . ? C42A C41A C46A C45A 4.3(8) . . . . ? B1A C41A C46A C45A -177.7(5) . . . . ? C31A B1A C51A C56A 172.6(4) . . . . ? C1A B1A C51A C56A -65.2(5) . . . . ? C41A B1A C51A C56A 50.9(6) . . . . ? C31A B1A C51A C52A -14.9(7) . . . . ? C1A B1A C51A C52A 107.2(5) . . . . ? C41A B1A C51A C52A -136.7(5) . . . . ? C56A C51A C52A F52A 176.2(4) . . . . ? B1A C51A C52A F52A 3.3(7) . . . . ? C56A C51A C52A C53A -2.6(7) . . . . ? B1A C51A C52A C53A -175.5(5) . . . . ? F52A C52A C53A F53A 1.0(7) . . . . ? C51A C52A C53A F53A 179.8(4) . . . . ? F52A C52A C53A C54A -177.3(5) . . . . ? C51A C52A C53A C54A 1.5(8) . . . . ? F53A C53A C54A F54A -0.5(8) . . . . ? C52A C53A C54A F54A 177.8(5) . . . . ? F53A C53A C54A C55A -178.3(5) . . . . ? C52A C53A C54A C55A 0.0(8) . . . . ? C53A C54A C55A F55A 180.0(5) . . . . ? F54A C54A C55A F55A 2.1(8) . . . . ? C53A C54A C55A C56A -0.2(8) . . . . ? F54A C54A C55A C56A -178.0(5) . . . . ? F55A C55A C56A F56A -1.3(7) . . . . ? C54A C55A C56A F56A 178.8(4) . . . . ? F55A C55A C56A C51A 178.7(5) . . . . ? C54A C55A C56A C51A -1.2(8) . . . . ? C52A C51A C56A C55A 2.4(7) . . . . ? B1A C51A C56A C55A 175.9(5) . . . . ? C52A C51A C56A F56A -177.5(4) . . . . ? B1A C51A C56A F56A -4.1(7) . . . . ? C41B B1B C1B C2B 123.7(8) . . . . ? C31B B1B C1B C2B 6.7(10) . . . . ? C51B B1B C1B C2B -113.2(8) . . . . ? C41B B1B C1B P1B -88.4(6) . . . . ? C31B B1B C1B P1B 154.6(4) . . . . ? C51B B1B C1B P1B 34.7(6) . . . . ? C21B P1B C1B C2B 103.9(3) . . . . ? C11B P1B C1B C2B -95.3(3) . . . . ? C2B P1B C1B B1B -163.2(6) . . . . ? C21B P1B C1B B1B -59.2(6) . . . . ? C11B P1B C1B B1B 101.5(5) . . . . ? B1B C1B C2B C3B -17.8(13) . . . . ? P1B C1B C2B C3B -176.2(7) . . . . ? B1B C1B C2B P1B 158.5(8) . . . . ? C21B P1B C2B C1B -103.5(3) . . . . ? C11B P1B C2B C1B 111.1(3) . . . . ? C1B P1B C2B C3B 175.8(8) . . . . ? C21B P1B C2B C3B 72.3(7) . . . . ? C11B P1B C2B C3B -73.1(6) . . . . ? C1B C2B C3B C4B 35.2(9) . . . . ? P1B C2B C3B C4B -138.3(6) . . . . ? C1B C2B C3B C8B -144.9(6) . . . . ? P1B C2B C3B C8B 41.6(8) . . . . ? C8B C3B C4B C5B 1.9(7) . . . . ? C2B C3B C4B C5B -178.3(4) . . . . ? C3B C4B C5B C6B -0.9(8) . . . . ? C4B C5B C6B C7B -0.5(8) . . . . ? C4B C5B C6B C9B 178.6(5) . . . . ? C5B C6B C7B C8B 1.0(8) . . . . ? C9B C6B C7B C8B -178.2(5) . . . . ? C4B C3B C8B C7B -1.4(7) . . . . ? C2B C3B C8B C7B 178.8(5) . . . . ? C6B C7B C8B C3B 0.0(8) . . . . ? C2B P1B C11B C16B 77.6(4) . . . . ? C1B P1B C11B C16B 128.3(3) . . . . ? C21B P1B C11B C16B -69.9(4) . . . . ? C2B P1B C11B C12B -98.7(4) . . . . ? C1B P1B C11B C12B -48.1(5) . . . . ? C21B P1B C11B C12B 113.7(4) . . . . ? C16B C11B C12B C13B -2.8(7) . . . . ? P1B C11B C12B C13B 173.4(4) . . . . ? C16B C11B C12B C17B 172.8(5) . . . . ? P1B C11B C12B C17B -11.0(7) . . . . ? C11B C12B C13B C14B -0.8(7) . . . . ? C17B C12B C13B C14B -176.7(5) . . . . ? C12B C13B C14B C15B 2.3(8) . . . . ? C12B C13B C14B C18B -178.3(5) . . . . ? C13B C14B C15B C16B -0.3(8) . . . . ? C18B C14B C15B C16B -179.7(5) . . . . ? C14B C15B C16B C11B -3.2(8) . . . . ? C14B C15B C16B C19B 174.7(5) . . . . ? C12B C11B C16B C15B 4.7(7) . . . . ? P1B C11B C16B C15B -171.7(4) . . . . ? C12B C11B C16B C19B -173.0(4) . . . . ? P1B C11B C16B C19B 10.5(6) . . . . ? C2B P1B C21B C22B 160.1(3) . . . . ? C1B P1B C21B C22B 108.6(4) . . . . ? C11B P1B C21B C22B -53.8(4) . . . . ? C2B P1B C21B C26B -17.8(5) . . . . ? C1B P1B C21B C26B -69.3(4) . . . . ? C11B P1B C21B C26B 128.4(4) . . . . ? C26B C21B C22B C23B -0.2(6) . . . . ? P1B C21B C22B C23B -178.1(3) . . . . ? C26B C21B C22B C27B 179.3(4) . . . . ? P1B C21B C22B C27B 1.4(6) . . . . ? C21B C22B C23B C24B 0.0(7) . . . . ? C27B C22B C23B C24B -179.6(4) . . . . ? C22B C23B C24B C25B 0.5(7) . . . . ? C22B C23B C24B C28B -179.5(5) . . . . ? C23B C24B C25B C26B -0.8(7) . . . . ? C28B C24B C25B C26B 179.2(5) . . . . ? C24B C25B C26B C21B 0.6(7) . . . . ? C24B C25B C26B C29B -179.6(5) . . . . ? C22B C21B C26B C25B 0.0(6) . . . . ? P1B C21B C26B C25B 177.9(4) . . . . ? C22B C21B C26B C29B -179.9(4) . . . . ? P1B C21B C26B C29B -2.0(6) . . . . ? C1B B1B C31B C36B -133.0(5) . . . . ? C41B B1B C31B C36B 103.8(5) . . . . ? C51B B1B C31B C36B -22.9(6) . . . . ? C1B B1B C31B C32B 53.3(5) . . . . ? C41B B1B C31B C32B -69.9(5) . . . . ? C51B B1B C31B C32B 163.5(4) . . . . ? C36B C31B C32B F32B -178.0(4) . . . . ? B1B C31B C32B F32B -3.6(6) . . . . ? C36B C31B C32B C33B 3.9(7) . . . . ? B1B C31B C32B C33B 178.3(4) . . . . ? F32B C32B C33B F33B -2.1(6) . . . . ? C31B C32B C33B F33B 176.0(4) . . . . ? F32B C32B C33B C34B 177.3(4) . . . . ? C31B C32B C33B C34B -4.5(7) . . . . ? F33B C33B C34B F34B 1.6(7) . . . . ? C32B C33B C34B F34B -177.8(4) . . . . ? F33B C33B C34B C35B -178.7(5) . . . . ? C32B C33B C34B C35B 1.8(7) . . . . ? F34B C34B C35B F35B -0.5(7) . . . . ? C33B C34B C35B F35B 179.8(5) . . . . ? F34B C34B C35B C36B -179.4(4) . . . . ? C33B C34B C35B C36B 1.0(7) . . . . ? C32B C31B C36B F36B 178.6(4) . . . . ? B1B C31B C36B F36B 4.6(7) . . . . ? C32B C31B C36B C35B -0.8(7) . . . . ? B1B C31B C36B C35B -174.8(4) . . . . ? F35B C35B C36B F36B 0.2(7) . . . . ? C34B C35B C36B F36B 179.1(4) . . . . ? F35B C35B C36B C31B 179.6(4) . . . . ? C34B C35B C36B C31B -1.5(7) . . . . ? C1B B1B C41B C46B 165.7(4) . . . . ? C31B B1B C41B C46B -73.6(5) . . . . ? C51B B1B C41B C46B 52.2(6) . . . . ? C1B B1B C41B C42B -22.5(6) . . . . ? C31B B1B C41B C42B 98.2(5) . . . . ? C51B B1B C41B C42B -136.0(4) . . . . ? C46B C41B C42B F42B 179.6(4) . . . . ? B1B C41B C42B F42B 7.2(7) . . . . ? C46B C41B C42B C43B -1.6(7) . . . . ? B1B C41B C42B C43B -174.0(4) . . . . ? F42B C42B C43B F43B -0.6(7) . . . . ? C41B C42B C43B F43B -179.6(4) . . . . ? F42B C42B C43B C44B 179.4(4) . . . . ? C41B C42B C43B C44B 0.5(8) . . . . ? F43B C43B C44B F44B 0.8(7) . . . . ? C42B C43B C44B F44B -179.2(4) . . . . ? F43B C43B C44B C45B -179.4(4) . . . . ? C42B C43B C44B C45B 0.6(7) . . . . ? F44B C44B C45B F45B -0.2(7) . . . . ? C43B C44B C45B F45B 180.0(4) . . . . ? F44B C44B C45B C46B 179.4(4) . . . . ? C43B C44B C45B C46B -0.5(7) . . . . ? F45B C45B C46B F46B -2.8(6) . . . . ? C44B C45B C46B F46B 177.6(4) . . . . ? F45B C45B C46B C41B 178.8(4) . . . . ? C44B C45B C46B C41B -0.8(7) . . . . ? C42B C41B C46B F46B -176.7(4) . . . . ? B1B C41B C46B F46B -3.9(6) . . . . ? C42B C41B C46B C45B 1.7(7) . . . . ? B1B C41B C46B C45B 174.4(4) . . . . ? C1B B1B C51B C52B -102.4(5) . . . . ? C41B B1B C51B C52B 19.9(6) . . . . ? C31B B1B C51B C52B 140.4(4) . . . . ? C1B B1B C51B C56B 67.7(5) . . . . ? C41B B1B C51B C56B -170.0(4) . . . . ? C31B B1B C51B C56B -49.6(5) . . . . ? C56B C51B C52B F52B -177.2(4) . . . . ? B1B C51B C52B F52B -6.4(7) . . . . ? C56B C51B C52B C53B 0.5(7) . . . . ? B1B C51B C52B C53B 171.3(4) . . . . ? F52B C52B C53B F53B -2.7(7) . . . . ? C51B C52B C53B F53B 179.5(4) . . . . ? F52B C52B C53B C54B 177.2(4) . . . . ? C51B C52B C53B C54B -0.5(7) . . . . ? F53B C53B C54B F54B 0.7(7) . . . . ? C52B C53B C54B F54B -179.2(4) . . . . ? F53B C53B C54B C55B -179.9(5) . . . . ? C52B C53B C54B C55B 0.2(7) . . . . ? C53B C54B C55B F55B 179.5(4) . . . . ? F54B C54B C55B F55B -1.1(7) . . . . ? C53B C54B C55B C56B 0.2(7) . . . . ? F54B C54B C55B C56B 179.6(4) . . . . ? F55B C55B C56B F56B 2.3(6) . . . . ? C54B C55B C56B F56B -178.4(4) . . . . ? F55B C55B C56B C51B -179.5(4) . . . . ? C54B C55B C56B C51B -0.1(7) . . . . ? C52B C51B C56B F56B 178.1(4) . . . . ? B1B C51B C56B F56B 6.7(6) . . . . ? C52B C51B C56B C55B -0.2(6) . . . . ? B1B C51B C56B C55B -171.5(4) . . . . ? C101 C102 C103 C104 -157.9(14) . . . . ? C102 C103 C104 C105 79.2(18) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 67.18 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.952 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.058