Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global #=========================================================== _audit_creation_date 19-06-98 # 1. SUBMISSION DETAILS _journal_coden_Cambridge 186 _publ_contact_author_name 'Prof Dominique Matt' _publ_contact_author_address ; Prof D Matt Lab de Chimie Inorganique Moleculaire, UMR 7513 CNRS Universite Louis Pasteur 1 rue Blaise Pascal F-67008 Strasbourg Cedex FRANCE ; _publ_contact_author_phone '+33 3 88 41 68 71' _publ_contact_author_email dmatt@chimie.u-strasbg.fr _publ_requested_journal 'J. Chem. Soc. Dalton Trans.' _publ_contact_letter ; Please consider this CIF submission for publication as a new structure paper in J. Chem. Soc. Dalton Trans. The figures, chemical structure diagram (scheme), Transfert of Copyright Agreement form and structure factors will be sent on receipt of your acknowledgement letter ; _publ_requested_category FM #=========================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=========================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Calix[4]arene-derived diphosphines, diphosphinites and diphosphites as chelating ligands for transition metal ions. Encapsulation of silver(I) in a calixcrown-diphosphite ; loop_ _publ_author_name _publ_author_address 'Jeunesse, Catherine' ; Universite Louis Pasteur, Laboratoire de Chimie Inorganique Moleculaire, UMR 7513 CNRS, 1, rue Blaise Pascal, F-67008 Strasbourg Cedex, France ; 'Dieleman, Cedric' ; Universite Louis Pasteur, Laboratoire de Chimie Inorganique Moleculaire, UMR 7513 CNRS, 1, rue Blaise Pascal, F-67008 Strasbourg Cedex, France ; 'Steyer, Stephane' ; Universite Louis Pasteur, Laboratoire de Chimie Inorganique Moleculaire, UMR 7513 CNRS, 1, rue Blaise Pascal, F-67008 Strasbourg Cedex, France ; 'Matt, Dominique' ; Universite Louis Pasteur, Laboratoire de Chimie Inorganique Moleculaire, UMR 7513 CNRS, 1, rue Blaise Pascal, F-67008 Strasbourg Cedex, France ; # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. OpenMoleN, Interactive Intelligent Structure solution (1997) Nonius B.V., Delft, The Netherlands. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #============================================================== #================ # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. data_st195 #============================================================== #================ # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C44 H56 Ag B F4 O11 P2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C44 H56 Ag B F4 O11 P2' _chemical_formula_weight 1017.55 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 B ? 0.000 0.001 International_Tables_Vol_IV_Table_2.3.1 F ? 0.014 0.010 International_Tables_Vol_IV_Table_2.3.1 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 Ag ? -1.085 1.101 International_Tables_Vol_IV_Table_2.3.1 #============================================================== #================ # 6. CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c n' _symmetry_space_group_name_Hall '-P 2ab 2ac' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 1/2-x,1/2-y,+z -x,1/2+y,1/2-z 1/2+x,-y,1/2-z -x,-y,-z 1/2+x,1/2+y,-z +x,1/2-y,1/2+z 1/2-x,+y,1/2+z _cell_length_a 11.9325(2) _cell_length_b 17.6619(2) _cell_length_c 21.2455(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4477.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used 39738 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 29.6 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.51 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 0.588 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #============================================================== #================ # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 180 frames, 60 sec/frame, delta phi = 1.0 deg. Each frame measured 2 times. Detector to crystal distance 25 mm. ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 39738 _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 29.57 _reflns_number_total 6677 _reflns_number_gt 4299 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #============================================================== #================ # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4299 _refine_ls_number_parameters 312 _refine_ls_number_restraints 4 _refine_ls_number_constraints 0 _refine_ls_abs_structure_details ; ? ; _refine_ls_R_factor_all 0.066 _refine_ls_R_factor_gt 0.049 _refine_ls_wR_factor_all 0.101 _refine_ls_wR_factor_ref 0.062 _refine_ls_goodness_of_fit_all 1.757 _refine_ls_goodness_of_fit_ref 1.158 _refine_ls_shift/su_max 0.066 _refine_ls_shift/esd_mean 0.003 _refine_diff_density_max 0.794 _refine_diff_density_min -1.313 #============================================================== #================ # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol AG 0.2500 0.2500 0.17069(1) 0.0373(1) 0.500 Uani ? ? Ag P 0.38306(7) 0.16415(4) 0.21377(4) 0.0361(3) 1.000 Uani ? ? P O1 0.3658(2) 0.0743(1) 0.2043(1) 0.042(1) 1.000 Uani ? ? O C1 0.3719(4) 0.0470(2) 0.1398(2) 0.057(2) 1.000 Uani ? ? C C2 0.2984(4) -0.0176(3) 0.1304(2) 0.073(2) 1.000 Uani ? ? C O2 0.5141(2) 0.1743(1) 0.2022(1) 0.046(1) 1.000 Uani ? ? O C3 0.5983(3) 0.1156(2) 0.2136(2) 0.058(2) 1.000 Uani ? ? C C4 0.7091(4) 0.1496(3) 0.2263(3) 0.070(3) 1.000 Uani ? ? C O3 0.3609(2) 0.1748(1) 0.2871(1) 0.0342(9) 1.000 Uani ? ? O C5 0.4183(3) 0.1412(2) 0.3370(1) 0.035(1) 1.000 Uani ? ? C C6 0.3741(3) 0.0749(2) 0.3620(1) 0.039(1) 1.000 Uani ? ? C C7 0.4331(3) 0.0420(2) 0.4113(2) 0.045(2) 1.000 Uani ? ? C C8 0.5299(3) 0.0752(2) 0.4344(2) 0.049(2) 1.000 Uani ? ? C C9 0.5677(3) 0.1430(2) 0.4107(2) 0.046(2) 1.000 Uani ? ? C C10 0.5120(3) 0.1789(2) 0.3613(1) 0.038(1) 1.000 Uani ? ? C C11 0.5479(3) 0.2563(2) 0.3375(1) 0.041(1) 1.000 Uani ? ? C C12 0.4815(3) 0.3196(2) 0.3679(1) 0.040(1) 1.000 Uani ? ? C C13 0.4012(3) 0.3627(2) 0.3354(1) 0.036(1) 1.000 Uani ? ? C C14 0.3355(3) 0.4163(2) 0.3673(1) 0.040(1) 1.000 Uani ? ? C C15 0.3604(3) 0.4314(2) 0.4305(2) 0.048(2) 1.000 Uani ? ? C C16 0.4439(3) 0.3925(2) 0.4619(2) 0.050(2) 1.000 Uani ? ? C C17 0.5023(3) 0.3361(2) 0.4313(2) 0.046(2) 1.000 Uani ? ? C C18 0.2642(3) 0.0427(2) 0.3386(2) 0.041(2) 1.000 Uani ? ? C O4 0.3859(2) 0.3492(1) 0.27113(9) 0.037(1) 1.000 Uani ? ? O C19 0.4434(3) 0.4015(2) 0.2305(2) 0.042(2) 1.000 Uani ? ? C C20 0.4798(3) 0.3642(2) 0.1698(2) 0.043(2) 1.000 Uani ? ? C O5 0.3869(2) 0.3519(1) 0.1284(1) 0.042(1) 1.000 Uani ? ? O C21 0.4212(4) 0.3140(2) 0.0713(2) 0.054(2) 1.000 Uani ? ? C C22 0.3237(4) 0.2977(2) 0.0301(2) 0.053(2) 1.000 Uani ? ? C O6 0.2326(4) 0.2687(2) 0.0611(2) 0.045(2) 0.500 Uani ? ? O B1 0.2349(8) 0.817(1) 0.4512(5) 0.070(6) 0.500 Uani ? ? B F1 0.1278(5) 0.8266(6) 0.4313(3) 0.096(4) 0.500 Uani ? ? F F2 0.2414(4) 0.7742(3) 0.5059(3) 0.073(3) 0.500 Uani ? ? F F3 0.2757(7) 0.8815(4) 0.4578(5) 0.196(5) 0.500 Uani ? ? F F4 0.3018(8) 0.776(1) 0.4094(4) 0.185(9) 0.500 Uani ? ? F H1 0.4468 0.0324 0.1308 0.0756 1.000 Uiso calc C1 H H2 0.3500 0.0865 0.1121 0.0756 1.000 Uiso calc C1 H H3 0.3038 -0.0344 0.0880 0.0956 1.000 Uiso calc C2 H H4 0.3200 -0.0575 0.1579 0.0956 1.000 Uiso calc C2 H H5 0.2232 -0.0033 0.1392 0.0956 1.000 Uiso calc C2 H H6 0.6035 0.0841 0.1775 0.0761 1.000 Uiso calc C3 H H7 0.5761 0.0861 0.2488 0.0761 1.000 Uiso calc C3 H H8 0.7624 0.1105 0.2335 0.0960 1.000 Uiso calc C4 H H9 0.7318 0.1790 0.1911 0.0960 1.000 Uiso calc C4 H H10 0.7045 0.1810 0.2625 0.0960 1.000 Uiso calc C4 H H11 0.4067 -0.0038 0.4294 0.0602 1.000 Uiso calc C7 H H12 0.5707 0.0509 0.4670 0.0660 1.000 Uiso calc C8 H H13 0.6328 0.1657 0.4283 0.0620 1.000 Uiso calc C9 H H14 0.5369 0.2583 0.2932 0.0549 1.000 Uiso calc C11 H H15 0.6251 0.2634 0.3467 0.0549 1.000 Uiso calc C11 H H16 0.3191 0.4692 0.4523 0.0628 1.000 Uiso calc C15 H H17 0.4610 0.4045 0.5044 0.0684 1.000 Uiso calc C16 H H18 0.5574 0.3080 0.4535 0.0619 1.000 Uiso calc C17 H H19 0.2603 -0.0094 0.3496 0.0552 1.000 Uiso calc C18 H H20 0.2611 0.0477 0.2941 0.0552 1.000 Uiso calc C18 H H21 0.5078 0.4202 0.2517 0.0555 1.000 Uiso calc C19 H H22 0.3946 0.4424 0.2209 0.0555 1.000 Uiso calc C19 H H23 0.5134 0.3168 0.1793 0.0559 1.000 Uiso calc C20 H H24 0.5329 0.3958 0.1494 0.0559 1.000 Uiso calc C20 H H25 0.4570 0.2678 0.0819 0.0719 1.000 Uiso calc C21 H H26 0.4722 0.3456 0.0492 0.0719 1.000 Uiso calc C21 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol AG 0.0418(1) 0.0472(2) 0.0263(1) 0.0047(1) 0.0000 0.0000 Ag P 0.0384(3) 0.0381(3) 0.0320(3) 0.0014(3) 0.0000(3) 0.0026(3) P O1 0.052(1) 0.040(1) 0.036(1) -0.000(1) 0.001(1) -0.0028(9) O C1 0.069(2) 0.063(2) 0.042(2) -0.002(2) 0.003(2) -0.013(2) C C2 0.070(2) 0.076(2) 0.075(2) -0.003(2) -0.000(2) -0.035(2) C O2 0.041(1) 0.046(1) 0.052(1) 0.002(1) 0.010(1) 0.002(1) O C3 0.046(2) 0.060(2) 0.070(2) 0.012(2) 0.002(2) -0.011(2) C C4 0.049(2) 0.067(2) 0.105(3) 0.005(2) 0.006(2) -0.007(3) C O3 0.0356(9) 0.0341(9) 0.0328(9) 0.0016(8) -0.0040(8) 0.0043(8) O C5 0.037(1) 0.037(1) 0.030(1) 0.006(1) -0.002(1) 0.002(1) C C6 0.049(2) 0.037(1) 0.033(1) 0.007(1) 0.002(1) 0.000(1) C C7 0.063(2) 0.041(1) 0.035(1) 0.012(1) 0.002(1) 0.004(1) C C8 0.058(2) 0.060(2) 0.034(1) 0.022(2) -0.003(1) 0.006(1) C C9 0.039(2) 0.067(2) 0.037(2) 0.011(2) -0.006(1) 0.000(1) C C10 0.034(1) 0.050(2) 0.033(1) 0.007(1) -0.000(1) 0.001(1) C C11 0.033(1) 0.056(2) 0.038(1) -0.006(1) -0.002(1) -0.000(1) C C12 0.039(1) 0.047(1) 0.035(1) -0.011(1) -0.001(1) -0.001(1) C C13 0.041(1) 0.040(1) 0.029(1) -0.011(1) 0.000(1) -0.002(1) C C14 0.048(2) 0.039(1) 0.035(1) -0.011(1) -0.002(1) -0.001(1) C C15 0.055(2) 0.052(2) 0.039(2) -0.007(2) 0.001(1) -0.011(1) C C16 0.057(2) 0.068(2) 0.033(2) -0.010(2) -0.003(1) -0.008(1) C C17 0.047(2) 0.061(2) 0.035(1) -0.008(2) -0.006(1) 0.000(1) C C18 0.057(2) 0.032(1) 0.038(1) -0.004(1) 0.000(1) 0.003(1) C O4 0.044(1) 0.040(1) 0.0287(9) -0.0101(9) 0.0020(9) 0.0008(8) O C19 0.053(2) 0.039(1) 0.036(1) -0.012(1) 0.003(1) 0.003(1) C C20 0.045(2) 0.047(2) 0.038(1) -0.005(1) 0.005(1) 0.005(1) C O5 0.049(1) 0.051(1) 0.0297(9) 0.002(1) 0.0024(9) 0.0019(9) O C21 0.064(2) 0.063(2) 0.038(2) -0.006(2) 0.013(2) -0.002(2) C C22 0.068(2) 0.070(2) 0.032(2) -0.006(2) 0.004(2) 0.003(2) C O6 0.055(3) 0.054(3) 0.030(2) -0.005(2) 0.000(2) -0.004(2) O B1 0.051(5) 0.19(1) 0.036(4) -0.039(6) 0.004(4) 0.005(6) B F1 0.054(3) 0.248(8) 0.066(3) -0.039(4) -0.010(3) 0.014(4) F F2 0.066(3) 0.074(3) 0.080(3) -0.013(3) -0.001(3) 0.010(2) F F3 0.207(6) 0.122(3) 0.300(7) -0.104(4) -0.164(5) 0.142(4) F F4 0.133(7) 0.46(2) 0.102(5) 0.04(1) 0.063(4) 0.020(9) F # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag AG P 2.3785(8) . . ? AG P 2.3785(8) . 2_555 ? AG O6 2.360(5) . . ? AG O6 2.360(5) . 2_555 ? P O1 1.612(2) . . ? P O2 1.593(2) . . ? P O3 1.592(2) . . ? O1 C1 1.455(4) . . ? C1 C2 1.453(6) . . ? O2 C3 1.464(4) . . ? C3 C4 1.477(6) . . ? O3 C5 1.395(3) . . ? C5 C6 1.389(4) . . ? C5 C10 1.399(4) . . ? C6 C7 1.389(4) . . ? C6 C18 1.515(5) . . ? C7 C8 1.385(6) . . ? C8 C9 1.374(6) . . ? C9 C10 1.397(4) . . ? C10 C11 1.520(5) . . ? C11 C12 1.516(5) . . ? C12 C13 1.405(5) . . ? C12 C17 1.398(4) . . ? C13 C14 1.404(5) . . ? C13 O4 1.398(3) . . ? C14 C15 1.402(4) . . ? C14 C18 1.520(5) . 2_555 ? C15 C16 1.382(5) . . ? C16 C17 1.380(5) . . ? O4 C19 1.438(4) . . ? C19 C20 1.512(5) . . ? C20 O5 1.432(4) . . ? O5 C21 1.444(4) . . ? C21 C22 1.483(6) . . ? C22 O6 1.370(7) . . ? C22 O6 1.503(7) . 2_555 ? B1 F1 1.36(1) . . ? B1 F2 1.39(1) . . ? B1 F3 1.24(2) . . ? B1 F4 1.40(2) . . ? B1 F4 1.92(2) . 2_565 ? F4 F4 1.54(3) . 2_565 ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P AG P 134.74(4) . . 2_555 ? P AG O6 121.8(1) . . . ? P AG O6 103.4(1) . . 2_555 ? P AG O6 103.4(1) . 2_555 . ? P AG O6 121.8(1) . 2_555 2_555 ? O6 AG O6 19.0(2) . . 2_555 ? O1 P O2 102.5(1) . . . ? O1 P O3 102.5(1) . . . ? O2 P O3 107.5(1) . . . ? P O1 C1 115.9(2) . . . ? O1 C1 C2 111.1(3) . . . ? P O2 C3 124.6(2) . . . ? O2 C3 C4 110.9(3) . . . ? P O3 C5 127.8(2) . . . ? O3 C5 C6 117.5(3) . . . ? O3 C5 C10 118.0(3) . . . ? C6 C5 C10 124.3(3) . . . ? C5 C6 C7 116.6(3) . . . ? C5 C6 C18 121.4(3) . . . ? C7 C6 C18 121.9(3) . . . ? C6 C7 C8 120.8(3) . . . ? C7 C8 C9 120.9(3) . . . ? C8 C9 C10 121.0(3) . . . ? C5 C10 C9 116.2(3) . . . ? C5 C10 C11 122.1(3) . . . ? C9 C10 C11 121.6(3) . . . ? C10 C11 C12 112.0(3) . . . ? C11 C12 C13 123.1(3) . . . ? C11 C12 C17 118.1(3) . . . ? C13 C12 C17 118.8(3) . . . ? C12 C13 C14 120.6(3) . . . ? C12 C13 O4 118.5(3) . . . ? C14 C13 O4 120.9(3) . . . ? C13 C14 C15 118.2(3) . . . ? C13 C14 C18 124.3(3) . . 2_555 ? C15 C14 C18 117.4(3) . . 2_555 ? C14 C15 C16 121.4(3) . . . ? C15 C16 C17 119.7(3) . . . ? C12 C17 C16 121.0(3) . . . ? C6 C18 C14 111.5(3) . . 2_555 ? C13 O4 C19 114.5(2) . . . ? O4 C19 C20 111.6(3) . . . ? C19 C20 O5 111.6(3) . . . ? C20 O5 C21 111.5(3) . . . ? O5 C21 C22 111.3(3) . . . ? C21 C22 O6 114.3(4) . . . ? C21 C22 O6 104.2(3) . . 2_555 ? O6 C22 O6 31.1(4) . . 2_555 ? C22 O6 C22 115.8(4) . . 2_555 ? F1 B1 F2 112.2(8) . . . ? F1 B1 F3 107(1) . . . ? F1 B1 F4 113(1) . . . ? F1 B1 F4 75.1(8) . . 2_565 ? F2 B1 F3 112(1) . . . ? F2 B1 F4 102(1) . . . ? F2 B1 F4 85(1) . . 2_565 ? F3 B1 F4 109(1) . . . ? F3 B1 F4 157(1) . . 2_565 ? F4 B1 F4 52(1) . . 2_565 ? B1 F4 B1 91(1) . . 2_565 ? B1 F4 F4 81.6(9) . . 2_565 ? B1 F4 F4 46(1) . 2_565 2_565 ?