#=============================================================================== data_global #=============================================================================== _audit_creation_date 3-04-00 # 1. SUBMISSION DETAILS _publ_contact_author_name # Name of author for correspondance ; ; _publ_contact_author_address # Address of author for correspondance ; ; _publ_contact_author_phone 'xxxxxxxxxx' _publ_contact_author_fax 'xxxxxxxxxx' _publ_contact_author_email xxx@xx.xx.xx _publ_requested_journal 'Organometallics' _publ_contact_letter ; Please consider this CIF submission for publication as a new structure paper in Acta Crystallographica Section C. 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 ; Transmetalation of Aryl Units from Gold(I) to Cobalt(III), A Clean Route to the Synthesis of Anion Cobaltoreceptors ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Mike Robitzer' ;CNRS UMR 7513 Laboratoire de Syntheses Metallo-Induites Universite Louis Pasteur 4 rue Blaise Pascal 67000 Strasbourg France ; 'Imenne Bouamaied' ;CNRS UMR 7513 Laboratoire de Syntheses Metallo-Induites Universite Louis Pasteur 4 rue Blaise Pascal 67000 Strasbourg France ; 'Claude Sirlin' ;CNRS UMR 7513 Laboratoire de Syntheses Metallo-Induites Universite Louis Pasteur 4 rue Blaise Pascal 67000 Strasbourg France ; 'Preston A. Chase' ;Department of Metal-Mediated Synthesis Debye Institute Utrecht University Padulaan 8 3584 CH Utrecht The Netherlands ; 'Gerard van Koten' ; Department of Metal-Mediated Synthesis Debye Institute Utrecht University Padulaan 8 3584 CH Utrecht The Netherlands ; 'Michel Pfeffer' ;CNRS UMR 7513 Laboratoire de Syntheses Metallo-Induites Universite Louis Pasteur 4 rue Blaise Pascal 67000 Strasbourg 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_st586 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C21 H33 Cl Co F6 N2 P' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C21 H33 Cl Co F6 N2 P' _chemical_formula_weight 552.86 _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 Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1 Co ? 0.299 0.973 International_Tables_Vol_IV_Table_2.3.1 F ? 0.014 0.010 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 1/2-x,-y,1/2+z -x,1/2+y,1/2-z 1/2+x,1/2-y,-z -x,-y,-z 1/2+x,+y,1/2-z +x,1/2-y,1/2+z 1/2-x,1/2+y,+z _cell_length_a 14.2005(3) _cell_length_b 20.7594(5) _cell_length_c 16.4489(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4849.0(4) _cell_formula_units_Z 8 _cell_measurement_temperature 173 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'violet' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.51 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 2288 _exptl_absorpt_coefficient_mu 0.942 _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 ; 6153 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 1.5 deg 1 scans of 30 sec per frame. Data collection was divided into 3 set(s) with the following starting angles and number of frames : Set 1 Theta = 6.40 Omega = 0.00 Kappa = 0.00 106 frames Set 2 Theta = -2.80 Kappa = -172.00 Phi = 0.00 31 frames Set 3 Theta = -6.40 Kappa = -55.00 Phi = 0.00 64 frames Friedel pairs were averaged. Internal R = 0.06 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6153 _diffrn_reflns_av_R_equivalents 0.060 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6153 _reflns_number_gt 3008 _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 '4Fo^2^/(sigma^2^(Fo^2^)+0.0004 Fo^4^)+0.2' _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 3008 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.147 _refine_ls_R_factor_gt 0.082 _refine_ls_wR_factor_all 0.446 _refine_ls_wR_factor_ref 0.099 _refine_ls_goodness_of_fit_all 7.992 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_shift/su_max 0.022 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 2.517 _refine_diff_density_min -0.958 #=============================================================================== # 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_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol CO 0.88275(8) 0.26500(6) 0.99842(8) 0.0317(5) Uani ? ? Co CL 1.0290(1) 0.20884(8) 0.9695(1) 0.0205(8) Uani ? ? Cl N1 0.9075(5) 0.3466(4) 0.9266(5) 0.037(4) Uani ? ? N C1 0.9417(8) 0.4047(5) 0.9718(6) 0.047(6) Uani ? ? C C2 1.0385(9) 0.3977(6) 1.0078(8) 0.064(7) Uani ? ? C C3 0.9726(7) 0.3320(4) 0.8564(6) 0.038(5) Uani ? ? C C4 0.9810(8) 0.3854(5) 0.7910(6) 0.051(6) Uani ? ? C C5 0.8021(5) 0.2419(4) 0.9056(5) 0.028(4) Uani ? ? C C6 0.7714(6) 0.2975(5) 0.8638(6) 0.037(5) Uani ? ? C C7 0.8107(7) 0.3598(5) 0.8956(6) 0.044(5) Uani ? ? C C8 0.7115(7) 0.2952(5) 0.7975(6) 0.042(5) Uani ? ? C C9 0.6781(6) 0.2356(5) 0.7715(6) 0.042(5) Uani ? ? C C10 0.7066(7) 0.1797(5) 0.8100(6) 0.040(5) Uani ? ? C C11 0.7698(6) 0.1815(4) 0.8769(5) 0.033(4) Uani ? ? C C12 0.8012(6) 0.1184(4) 0.9128(5) 0.032(4) Uani ? ? C N2 0.9002(5) 0.1006(3) 0.8867(4) 0.030(4) Uani ? ? N C13 0.9331(7) 0.0391(4) 0.9279(5) 0.035(5) Uani ? ? C C14 0.8878(8) -0.0216(5) 0.8943(7) 0.049(6) Uani ? ? C C15 0.9105(7) 0.1006(5) 0.7950(5) 0.036(5) Uani ? ? C C16 1.0103(7) 0.0847(5) 0.7697(6) 0.047(6) Uani ? ? C C17 0.8627(8) 0.2037(5) 1.0977(6) 0.051(6) Uani ? ? C C18 0.9196(8) 0.2591(6) 1.1247(6) 0.055(6) Uani ? ? C C19 0.8691(9) 0.3156(5) 1.1118(6) 0.048(6) Uani ? ? C C20 0.7809(8) 0.2978(5) 1.0769(6) 0.046(6) Uani ? ? C C21 0.7769(7) 0.2302(5) 1.0720(5) 0.044(5) Uani ? ? C P 0.7528(2) 0.0112(1) 1.1371(1) 0.033(1) Uani ? ? P F1 0.8598(4) 0.0355(3) 1.1280(4) 0.050(3) Uani ? ? F F2 0.6457(4) -0.0128(3) 1.1457(4) 0.057(3) Uani ? ? F F3 0.7661(5) 0.0098(5) 1.2326(4) 0.081(5) Uani ? ? F F4 0.7396(5) 0.0136(4) 1.0413(3) 0.067(4) Uani ? ? F F5 0.7853(5) -0.0608(3) 1.1314(6) 0.077(5) Uani ? ? F F6 0.7196(5) 0.0841(3) 1.1412(6) 0.080(5) Uani ? ? F H1 0.8987 0.4134 1.0147 0.0638 Uiso calc C1 H H2 0.9425 0.4401 0.9352 0.0638 Uiso calc C1 H H3 1.0551 0.4362 1.0353 0.0843 Uiso calc C2 H H4 1.0388 0.3628 1.0451 0.0843 Uiso calc C2 H H5 1.0826 0.3895 0.9656 0.0843 Uiso calc C2 H H6 0.9504 0.2940 0.8305 0.0499 Uiso calc C3 H H7 1.0337 0.3244 0.8780 0.0499 Uiso calc C3 H H8 1.0233 0.3717 0.7497 0.0667 Uiso calc C4 H H9 0.9209 0.3933 0.7679 0.0667 Uiso calc C4 H H10 1.0041 0.4237 0.8154 0.0667 Uiso calc C4 H H11 0.8133 0.3908 0.8532 0.0581 Uiso calc C7 H H12 0.7722 0.3756 0.9385 0.0581 Uiso calc C7 H H13 0.6935 0.3336 0.7703 0.0574 Uiso calc C8 H H14 0.6355 0.2333 0.7271 0.0587 Uiso calc C9 H H15 0.6835 0.1394 0.7914 0.0533 Uiso calc C10 H H16 0.7592 0.0855 0.8956 0.0414 Uiso calc C12 H H17 0.7995 0.1216 0.9704 0.0414 Uiso calc C12 H H18 0.9186 0.0420 0.9842 0.0466 Uiso calc C13 H H19 0.9994 0.0357 0.9212 0.0466 Uiso calc C13 H H20 0.9114 -0.0581 0.9226 0.0663 Uiso calc C14 H H21 0.8215 -0.0193 0.9011 0.0663 Uiso calc C14 H H22 0.9022 -0.0255 0.8381 0.0663 Uiso calc C14 H H23 0.8945 0.1420 0.7748 0.0488 Uiso calc C15 H H24 0.8690 0.0694 0.7727 0.0488 Uiso calc C15 H H25 1.0146 0.0850 0.7121 0.0639 Uiso calc C16 H H26 1.0522 0.1159 0.7916 0.0639 Uiso calc C16 H H27 1.0268 0.0432 0.7895 0.0639 Uiso calc C16 H H28 0.8803 0.1595 1.0977 0.0674 Uiso calc C17 H H29 0.9811 0.2567 1.1474 0.0767 Uiso calc C18 H H30 0.8895 0.3581 1.1239 0.0713 Uiso calc C19 H H31 0.7330 0.3267 1.0598 0.0621 Uiso calc C20 H H32 0.7239 0.2061 1.0540 0.0583 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 CO 0.0352(5) 0.0316(5) 0.0285(5) -0.0025(6) -0.0008(6) 0.0011(6) Co CL 0.0239(8) 0.0067(7) 0.054(1) -0.0039(7) 0.0215(9) -0.0079(9) Cl N1 0.037(4) 0.034(4) 0.041(4) 0.002(3) 0.003(4) 0.003(4) N C1 0.065(6) 0.034(5) 0.048(5) -0.014(5) 0.012(5) -0.005(5) C C2 0.072(7) 0.055(6) 0.067(7) -0.023(6) 0.004(7) -0.009(6) C C3 0.042(5) 0.037(5) 0.037(5) -0.002(4) 0.004(5) 0.000(4) C C4 0.060(6) 0.054(6) 0.040(5) -0.009(5) 0.005(5) 0.013(5) C C5 0.020(4) 0.037(4) 0.030(4) 0.005(4) 0.002(3) -0.002(4) C C6 0.030(4) 0.042(5) 0.041(5) 0.002(4) 0.010(4) 0.005(5) C C7 0.042(5) 0.040(5) 0.052(6) 0.008(5) 0.005(5) 0.009(5) C C8 0.033(5) 0.063(6) 0.036(5) 0.012(5) 0.002(4) 0.010(5) C C9 0.032(5) 0.069(6) 0.035(5) 0.008(5) -0.005(4) 0.005(5) C C10 0.033(5) 0.050(5) 0.039(5) -0.006(5) -0.001(4) -0.008(5) C C11 0.029(4) 0.033(4) 0.036(5) 0.001(4) 0.000(4) 0.001(4) C C12 0.032(4) 0.031(4) 0.033(5) -0.002(4) 0.003(4) -0.003(4) C N2 0.031(4) 0.036(4) 0.024(3) 0.001(3) 0.001(3) 0.001(3) N C13 0.044(5) 0.030(4) 0.033(5) 0.003(4) -0.003(4) 0.006(4) C C14 0.061(6) 0.031(5) 0.061(6) -0.002(5) -0.001(6) 0.001(5) C C15 0.044(5) 0.045(5) 0.023(4) 0.006(4) 0.000(4) -0.001(4) C C16 0.039(5) 0.073(7) 0.036(5) 0.004(5) 0.005(5) 0.005(5) C C17 0.067(7) 0.049(6) 0.040(5) -0.014(5) -0.001(5) 0.015(5) C C18 0.067(6) 0.078(7) 0.032(5) -0.019(6) -0.012(5) 0.009(6) C C19 0.095(8) 0.040(5) 0.030(5) -0.016(6) 0.009(6) -0.006(4) C C20 0.065(6) 0.041(5) 0.037(5) -0.002(5) 0.019(5) -0.003(5) C C21 0.049(5) 0.055(6) 0.031(4) -0.009(5) 0.017(4) -0.002(5) C P 0.035(1) 0.035(1) 0.030(1) -0.003(1) 0.004(1) 0.002(1) P F1 0.038(3) 0.055(3) 0.062(4) -0.006(3) 0.006(3) 0.004(3) F F2 0.043(3) 0.079(4) 0.054(3) -0.022(3) 0.003(3) 0.011(3) F F3 0.089(5) 0.193(7) 0.031(3) -0.066(5) 0.000(3) 0.004(4) F F4 0.065(4) 0.135(6) 0.035(3) -0.018(4) 0.001(3) 0.009(4) F F5 0.076(4) 0.038(3) 0.156(7) -0.001(3) -0.035(5) -0.004(4) F F6 0.061(4) 0.046(4) 0.179(8) 0.007(3) 0.004(5) -0.023(5) 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 CO CL 2.429(2) . . ? CO N1 2.094(8) . . ? CO C5 1.968(9) . . ? CO C17 2.09(1) . . ? CO C18 2.15(1) . . ? CO C19 2.15(1) . . ? CO C20 2.05(1) . . ? CO C21 2.061(9) . . ? N1 C1 1.50(1) . . ? N1 C3 1.51(1) . . ? N1 C7 1.49(1) . . ? C1 C2 1.50(2) . . ? C3 C4 1.55(1) . . ? C5 C6 1.41(1) . . ? C5 C11 1.42(1) . . ? C6 C7 1.50(1) . . ? C6 C8 1.38(1) . . ? C8 C9 1.39(1) . . ? C9 C10 1.38(1) . . ? C10 C11 1.42(1) . . ? C11 C12 1.51(1) . . ? C12 N2 1.52(1) . . ? N2 C13 1.52(1) . . ? N2 C15 1.51(1) . . ? C13 C14 1.52(1) . . ? C15 C16 1.51(1) . . ? C17 C18 1.48(2) . . ? C17 C21 1.40(2) . . ? C18 C19 1.39(2) . . ? C19 C20 1.43(2) . . ? C20 C21 1.41(1) . . ? P F1 1.608(6) . . ? P F2 1.607(6) . . ? P F3 1.582(6) . . ? P F4 1.588(6) . . ? P F5 1.567(7) . . ? P F6 1.586(7) . . ? 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 CL CO N1 97.7(2) . . . ? CL CO C5 103.3(2) . . . ? CL CO C17 88.7(3) . . . ? CL CO C18 87.3(4) . . . ? CL CO C19 118.8(4) . . . ? CL CO C20 152.1(3) . . . ? CL CO C21 124.8(3) . . . ? N1 CO C5 81.8(3) . . . ? N1 CO C17 163.0(4) . . . ? N1 CO C18 123.4(4) . . . ? N1 CO C19 96.3(4) . . . ? N1 CO C20 101.8(4) . . . ? N1 CO C21 137.5(4) . . . ? C5 CO C17 112.2(4) . . . ? C5 CO C18 151.6(4) . . . ? C5 CO C19 137.7(4) . . . ? C5 CO C20 99.1(4) . . . ? C5 CO C21 86.9(4) . . . ? C17 CO C18 40.8(4) . . . ? C17 CO C19 66.9(4) . . . ? C17 CO C20 67.4(4) . . . ? C17 CO C21 39.5(4) . . . ? C18 CO C19 37.8(4) . . . ? C18 CO C20 65.3(5) . . . ? C18 CO C21 65.8(4) . . . ? C19 CO C20 39.6(5) . . . ? C19 CO C21 66.2(4) . . . ? C20 CO C21 40.0(4) . . . ? C1 N1 C3 110.0(7) . . . ? C1 N1 C7 108.6(8) . . . ? C3 N1 C7 109.9(7) . . . ? N1 C1 C2 114.4(9) . . . ? N1 C3 C4 115.8(8) . . . ? C6 C5 C11 117.5(8) . . . ? C5 C6 C7 114.7(8) . . . ? C5 C6 C8 123.1(9) . . . ? C7 C6 C8 122.2(9) . . . ? N1 C7 C6 107.6(8) . . . ? C6 C8 C9 118.8(9) . . . ? C8 C9 C10 120.4(9) . . . ? C9 C10 C11 121.2(9) . . . ? C5 C11 C10 119.1(8) . . . ? C5 C11 C12 123.0(8) . . . ? C10 C11 C12 117.9(8) . . . ? C11 C12 N2 112.0(7) . . . ? C12 N2 C13 111.3(7) . . . ? C12 N2 C15 111.9(7) . . . ? C13 N2 C15 114.5(7) . . . ? N2 C13 C14 113.8(8) . . . ? N2 C15 C16 111.4(8) . . . ? C18 C17 C21 105(1) . . . ? C17 C18 C19 109(1) . . . ? C18 C19 C20 107.2(9) . . . ? C19 C20 C21 108(1) . . . ? C17 C21 C20 109(1) . . . ? F1 P F2 179(1) . . . ? F1 P F3 89.2(4) . . . ? F1 P F4 90.6(4) . . . ? F1 P F5 90.9(4) . . . ? F1 P F6 89.2(4) . . . ? F2 P F3 91.1(4) . . . ? F2 P F4 89.1(4) . . . ? F2 P F5 89.3(4) . . . ? F2 P F6 90.6(4) . . . ? F3 P F4 179.3(5) . . . ? F3 P F5 90.4(5) . . . ? F3 P F6 90.6(5) . . . ? F4 P F5 90.3(5) . . . ? F4 P F6 88.7(5) . . . ? F5 P F6 179.0(5) . . . ?