# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Mary F. Mahon' _publ_contact_author_email m.f.mahon@bath.ac.uk loop_ _publ_author_name A.D.Burrows D.J.Kelly M.F.Mahon P.R.Raithby C.Richardson ; A.J.Stevenson ; data_Compound-1-k07adb23 _database_code_depnum_ccdc_archive 'CCDC 804679' #TrackingRef '- stevenson-rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H20 Ag2 N4 O8' _chemical_formula_weight 636.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pcab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x+1/2, -y, -z+1/2' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x-1/2, y, z-1/2' 'x-1/2, -y-1/2, z' _cell_length_a 7.3890(1) _cell_length_b 15.9620(3) _cell_length_c 17.7590(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2094.55(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 19582 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.017 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 1.925 # Absorption correction _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.781 _exptl_absorpt_correction_T_max 0.910 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39756 _diffrn_reflns_av_R_equivalents 0.0814 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 27.42 _reflns_number_total 2380 _reflns_number_gt 1687 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (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^)+(0.0566P)^2^+1.2963P] 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 2380 _refine_ls_number_parameters 147 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0642 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.1014 _refine_ls_wR_factor_gt 0.0868 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 Ag1 Ag 0.72332(5) 0.430406(18) 0.349259(18) 0.04015(15) Uani 1 1 d . . . O1 O 0.7624(3) 0.32613(14) 0.49224(13) 0.0282(6) Uani 1 1 d . . . N1 N 0.7377(4) 0.31393(19) 0.41470(16) 0.0276(7) Uani 1 1 d . . . C1 C 0.8335(5) 0.2523(3) 0.60607(19) 0.0348(8) Uani 1 1 d . . . H1A H 0.9330 0.2911 0.6170 0.052 Uiso 1 1 calc R . . H1B H 0.8661 0.1959 0.6232 0.052 Uiso 1 1 calc R . . H1C H 0.7240 0.2709 0.6323 0.052 Uiso 1 1 calc R . . O2 O 0.5455(4) 0.54916(17) 0.34610(14) 0.0385(6) Uani 1 1 d . . . N2 N 0.4491(4) 0.54955(19) 0.28818(16) 0.0297(7) Uani 1 1 d . . . C2 C 0.7996(4) 0.2508(2) 0.52386(19) 0.0267(7) Uani 1 1 d . . . O3 O 0.3634(4) 0.61382(18) 0.27046(16) 0.0461(7) Uani 1 1 d . . . C3 C 0.7975(4) 0.1900(2) 0.46996(18) 0.0219(7) Uani 1 1 d . . . O4 O 0.4399(4) 0.48622(18) 0.24828(16) 0.0484(7) Uani 1 1 d . . . C4 C 0.7581(4) 0.2340(2) 0.40227(19) 0.0261(8) Uani 1 1 d . . . C5 C 0.7398(5) 0.1995(3) 0.3238(2) 0.0357(9) Uani 1 1 d . . . H5A H 0.6258 0.1684 0.3196 0.053 Uiso 1 1 calc R . . H5B H 0.8414 0.1618 0.3132 0.053 Uiso 1 1 calc R . . H5C H 0.7402 0.2457 0.2875 0.053 Uiso 1 1 calc R . . C6 C 0.8318(4) 0.0977(2) 0.4786(2) 0.0255(7) Uani 1 1 d . . . H6A H 0.9124 0.0888 0.5225 0.031 Uiso 1 1 calc R . . H6B H 0.8959 0.0771 0.4333 0.031 Uiso 1 1 calc R . . C7 C 0.5742(4) 0.0444(2) 0.55895(18) 0.0235(7) Uani 1 1 d . . . H7 H 0.6244 0.0747 0.6000 0.028 Uiso 1 1 calc R . . C8 C 0.6599(4) 0.0463(2) 0.48956(19) 0.0225(7) Uani 1 1 d . . . C9 C 0.5850(4) 0.00137(19) 0.43052(19) 0.0251(7) Uani 1 1 d . . . H9 H 0.6421 0.0017 0.3826 0.030 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 Ag1 0.0493(2) 0.0295(2) 0.0416(2) 0.01054(12) 0.01152(13) 0.00586(13) O1 0.0317(13) 0.0213(13) 0.0315(14) -0.0018(11) 0.0000(10) 0.0001(10) N1 0.0296(16) 0.0234(16) 0.0299(16) 0.0019(12) 0.0005(12) -0.0024(11) C1 0.035(2) 0.035(2) 0.034(2) -0.0004(16) -0.0045(16) -0.0040(17) O2 0.0423(16) 0.0404(16) 0.0328(14) -0.0016(12) -0.0118(12) 0.0062(12) N2 0.0309(16) 0.0329(17) 0.0252(16) 0.0012(14) 0.0001(12) -0.0042(13) C2 0.0188(17) 0.0286(19) 0.0325(18) 0.0024(16) -0.0007(13) -0.0008(13) O3 0.0461(16) 0.0428(17) 0.0495(17) 0.0112(13) -0.0092(13) 0.0059(14) C3 0.0183(15) 0.0206(17) 0.0267(18) -0.0002(13) 0.0020(12) -0.0044(13) O4 0.0605(19) 0.0461(18) 0.0386(16) -0.0080(14) -0.0066(14) -0.0017(14) C4 0.0234(17) 0.0267(19) 0.0283(18) -0.0010(14) 0.0028(13) -0.0013(13) C5 0.045(2) 0.034(2) 0.0274(18) 0.0041(17) -0.0010(15) 0.0001(17) C6 0.0221(16) 0.0228(18) 0.0314(19) 0.0019(14) 0.0003(14) -0.0003(14) C7 0.0234(17) 0.0195(16) 0.0277(18) -0.0017(14) -0.0016(13) 0.0030(13) C8 0.0210(15) 0.0171(16) 0.0293(18) 0.0025(14) 0.0018(13) 0.0019(13) C9 0.0266(17) 0.0211(17) 0.0275(18) 0.0034(14) 0.0033(14) 0.0007(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.195(3) . ? Ag1 O2 2.307(3) . ? Ag1 O3 2.468(3) 3_565 ? O1 C2 1.355(4) . ? O1 N1 1.403(4) . ? N1 C4 1.303(5) . ? C1 C2 1.482(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? O2 N2 1.251(4) . ? N2 O4 1.236(4) . ? N2 O3 1.246(4) . ? C2 C3 1.363(5) . ? O3 Ag1 2.468(3) 3_465 ? C3 C4 1.422(5) . ? C3 C6 1.504(4) . ? C4 C5 1.505(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C8 1.525(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.386(5) . ? C7 C9 1.397(4) 5_656 ? C7 H7 0.9500 . ? C8 C9 1.386(5) . ? C9 C7 1.397(4) 5_656 ? C9 H9 0.9500 . ? 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 N1 Ag1 O2 137.42(10) . . ? N1 Ag1 O3 101.16(10) . 3_565 ? O2 Ag1 O3 116.93(9) . 3_565 ? C2 O1 N1 108.1(2) . . ? C4 N1 O1 106.7(3) . . ? C4 N1 Ag1 138.2(2) . . ? O1 N1 Ag1 114.1(2) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N2 O2 Ag1 110.4(2) . . ? O4 N2 O3 120.0(3) . . ? O4 N2 O2 119.9(3) . . ? O3 N2 O2 120.1(3) . . ? O1 C2 C3 109.8(3) . . ? O1 C2 C1 115.4(3) . . ? C3 C2 C1 134.9(3) . . ? N2 O3 Ag1 101.3(2) . 3_465 ? C2 C3 C4 104.2(3) . . ? C2 C3 C6 128.6(3) . . ? C4 C3 C6 127.2(3) . . ? N1 C4 C3 111.3(3) . . ? N1 C4 C5 120.3(3) . . ? C3 C4 C5 128.3(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 C8 113.6(3) . . ? C3 C6 H6A 108.8 . . ? C8 C6 H6A 108.8 . . ? C3 C6 H6B 108.8 . . ? C8 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? C8 C7 C9 121.0(3) . 5_656 ? C8 C7 H7 119.5 . . ? C9 C7 H7 119.5 5_656 . ? C9 C8 C7 118.6(3) . . ? C9 C8 C6 121.0(3) . . ? C7 C8 C6 120.4(3) . . ? C8 C9 C7 120.4(3) . 5_656 ? C8 C9 H9 119.8 . . ? C7 C9 H9 119.8 5_656 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.866 _refine_diff_density_min -1.186 _refine_diff_density_rms 0.179 #===end data_Compound-2a-k07adb24(CCDC-804680) _database_code_depnum_ccdc_archive 'CCDC 804680' #TrackingRef '- stevenson-rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20.50 H22 Ag F3 N2 O4.50' _chemical_formula_weight 533.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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 10.3470(2) _cell_length_b 10.8430(2) _cell_length_c 11.2920(2) _cell_angle_alpha 64.703(1) _cell_angle_beta 70.872(1) _cell_angle_gamma 82.471(1) _cell_volume 1082.09(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13466 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.637 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 538 _exptl_absorpt_coefficient_mu 0.989 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 0.96 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22067 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 30.03 _reflns_number_total 6297 _reflns_number_gt 5570 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (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. The asymmetric unit in this structure consists of one silver centre, one trifluoroacetate anion, two crystallographically independent ligand halves, and a fragment of methanol in which the oxygen is located at an inversion centre. With regards to the solvent, the carbon position necessitates disorder of the methyl oxygen over 2 sites. The hydrogens in this solvent moiety could not be reliably located and hence were omitted from the final least squares. The electron density map in the region of the fluorines is very smeared, also due to disorder. Optimal modelling was achieved by treating each fluorine as being located over 3 sites. C-F and F?F bond distance restraints served to converge the model. The largest residual electron density maximum is also in this region. ; _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^)+(0.0798P)^2^+1.6850P] 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 0.008(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6297 _refine_ls_number_parameters 300 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1409 _refine_ls_wR_factor_gt 0.1344 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.103 _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 Ag1 Ag 0.58426(2) 0.89274(2) 0.58407(2) 0.02802(11) Uani 1 1 d . . . F1 F 0.1768(6) 1.1663(7) 0.8438(7) 0.0311(15) Uiso 0.30 1 d PD A 1 F2 F 0.3837(15) 1.1438(15) 0.8666(17) 0.145(8) Uiso 0.30 1 d PD A 1 F3 F 0.2410(15) 0.9739(13) 0.9719(10) 0.132(7) Uiso 0.30 1 d PD A 1 O1 O 0.6345(2) 0.5629(2) 0.7123(2) 0.0251(4) Uani 1 1 d . . . O2 O 0.8027(3) 0.9845(3) 0.6780(2) 0.0319(5) Uani 1 1 d . . . O3 O 0.3634(3) 1.1537(3) 0.6072(3) 0.0428(7) Uani 1 1 d . . . O4 O 0.3931(3) 0.9373(3) 0.7468(3) 0.0361(6) Uani 1 1 d . . . O5 O 0.5924(13) 1.5831(14) 0.3678(15) 0.112(4) Uani 0.50 1 d P . . N1 N 0.6068(3) 0.6752(3) 0.7480(3) 0.0240(5) Uani 1 1 d . . . N2 N 0.7342(3) 1.0406(3) 0.5777(3) 0.0349(7) Uani 1 1 d . . . C1 C 0.6795(3) 0.4598(3) 0.8106(3) 0.0232(6) Uani 1 1 d . . . C2 C 0.6818(3) 0.4996(3) 0.9085(3) 0.0218(5) Uani 1 1 d . . . C3 C 0.6355(3) 0.6368(3) 0.8633(3) 0.0226(5) Uani 1 1 d . . . C4 C 0.7145(4) 0.3310(4) 0.7912(4) 0.0324(7) Uani 1 1 d . . . H4A H 0.7938 0.3468 0.7094 0.049 Uiso 1 1 calc R . . H4B H 0.6364 0.3004 0.7793 0.049 Uiso 1 1 calc R . . H4C H 0.7364 0.2608 0.8720 0.049 Uiso 1 1 calc R . . C5 C 0.6176(4) 0.7324(3) 0.9306(3) 0.0288(6) Uani 1 1 d . . . H5A H 0.7072 0.7672 0.9149 0.043 Uiso 1 1 calc R . . H5B H 0.5734 0.6842 1.0296 0.043 Uiso 1 1 calc R . . H5C H 0.5604 0.8088 0.8916 0.043 Uiso 1 1 calc R . . C6 C 0.7249(3) 0.4203(3) 1.0358(3) 0.0267(6) Uani 1 1 d . . . H6A H 0.7237 0.3216 1.0577 0.032 Uiso 1 1 calc R . . H6B H 0.6586 0.4358 1.1141 0.032 Uiso 1 1 calc R . . C7 C 0.8676(3) 0.4618(3) 1.0176(3) 0.0236(6) Uani 1 1 d . . . C8 C 0.8861(3) 0.5533(4) 1.0677(3) 0.0277(6) Uani 1 1 d . . . H8 H 0.8085 0.5904 1.1144 0.033 Uiso 1 1 calc R . . C9 C 0.9832(3) 0.4089(3) 0.9497(3) 0.0274(6) Uani 1 1 d . . . H9 H 0.9726 0.3463 0.9149 0.033 Uiso 1 1 calc R . . C10 C 0.9152(3) 1.0617(3) 0.6343(3) 0.0283(6) Uani 1 1 d . . . C11 C 0.9240(3) 1.1652(3) 0.5093(3) 0.0261(6) Uani 1 1 d . . . C12 C 0.8061(4) 1.1476(4) 0.4805(4) 0.0326(7) Uani 1 1 d . . . C13 C 1.0000(5) 1.0220(5) 0.7273(5) 0.0447(9) Uani 1 1 d . . . H13A H 1.0935 1.0569 0.6740 0.067 Uiso 1 1 calc R . . H13B H 1.0015 0.9223 0.7740 0.067 Uiso 1 1 calc R . . H13C H 0.9614 1.0604 0.7958 0.067 Uiso 1 1 calc R . . C14 C 0.7580(6) 1.2351(5) 0.3588(5) 0.0535(12) Uani 1 1 d . . . H14A H 0.7006 1.1804 0.3450 0.080 Uiso 1 1 calc R . . H14B H 0.8372 1.2711 0.2767 0.080 Uiso 1 1 calc R . . H14C H 0.7046 1.3110 0.3752 0.080 Uiso 1 1 calc R . . C15 C 1.0348(4) 1.2715(4) 0.4200(4) 0.0322(7) Uani 1 1 d . . . H15A H 1.0350 1.3062 0.3233 0.039 Uiso 1 1 calc R . . H15B H 1.1244 1.2285 0.4253 0.039 Uiso 1 1 calc R . . C16 C 1.0182(3) 1.3910(3) 0.4606(3) 0.0250(6) Uani 1 1 d . . . C17 C 0.9252(3) 1.4936(3) 0.4214(3) 0.0265(6) Uani 1 1 d . . . H17 H 0.8736 1.4899 0.3671 0.032 Uiso 1 1 calc R . . C18 C 1.0929(3) 1.3982(3) 0.5391(4) 0.0271(6) Uani 1 1 d . . . H18 H 1.1570 1.3291 0.5663 0.032 Uiso 1 1 calc R . . C19 C 0.3570(4) 1.0558(4) 0.7195(4) 0.0331(7) Uani 1 1 d D A . C20 C 0.2890(4) 1.0822(4) 0.8465(5) 0.079(2) Uani 1 1 d D . . C21 C 0.5000 1.5000 0.5000 0.083(3) Uani 1 2 d S . . F1A F 0.2197(8) 1.2033(5) 0.8283(7) 0.0574(17) Uiso 0.45 1 d PD A 2 F2A F 0.3813(7) 1.0701(9) 0.9155(8) 0.0657(18) Uiso 0.45 1 d PD A 2 F3A F 0.1885(8) 0.9851(8) 0.9379(7) 0.072(2) Uiso 0.45 1 d PD A 2 F1B F 0.2998(16) 1.2186(6) 0.8168(18) 0.100(6) Uiso 0.25 1 d PD A 3 F2B F 0.3315(11) 1.0229(10) 0.9622(7) 0.039(2) Uiso 0.25 1 d PD A 3 F3B F 0.1504(5) 1.058(2) 0.910(2) 0.23(2) Uiso 0.25 1 d PD A 3 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 Ag1 0.03187(16) 0.02289(15) 0.02741(15) -0.00698(10) -0.01159(10) 0.00127(9) O1 0.0270(11) 0.0236(11) 0.0245(10) -0.0082(9) -0.0098(8) 0.0005(8) O2 0.0389(13) 0.0258(12) 0.0266(11) -0.0034(9) -0.0113(10) -0.0079(10) O3 0.0604(18) 0.0339(14) 0.0399(15) -0.0171(12) -0.0249(13) 0.0138(13) O4 0.0369(13) 0.0297(13) 0.0394(14) -0.0146(11) -0.0099(11) 0.0047(10) O5 0.089(8) 0.124(10) 0.156(12) -0.090(10) -0.032(8) -0.007(7) N1 0.0232(12) 0.0238(12) 0.0247(12) -0.0090(10) -0.0083(9) 0.0010(9) N2 0.0442(17) 0.0271(14) 0.0314(14) -0.0036(12) -0.0165(13) -0.0102(12) C1 0.0193(12) 0.0209(13) 0.0247(13) -0.0051(11) -0.0057(10) -0.0020(10) C2 0.0177(12) 0.0212(13) 0.0221(13) -0.0047(11) -0.0047(10) -0.0037(10) C3 0.0166(12) 0.0241(14) 0.0228(13) -0.0061(11) -0.0040(10) -0.0034(10) C4 0.0358(17) 0.0258(16) 0.0325(16) -0.0120(13) -0.0061(13) -0.0001(13) C5 0.0302(15) 0.0267(16) 0.0268(15) -0.0094(12) -0.0065(12) -0.0022(12) C6 0.0245(14) 0.0260(15) 0.0233(14) -0.0015(11) -0.0094(11) -0.0042(11) C7 0.0226(13) 0.0235(14) 0.0206(13) -0.0034(11) -0.0085(10) -0.0011(10) C8 0.0232(14) 0.0318(16) 0.0278(15) -0.0125(13) -0.0081(11) 0.0031(12) C9 0.0285(15) 0.0268(15) 0.0291(15) -0.0116(13) -0.0109(12) -0.0003(12) C10 0.0304(15) 0.0252(15) 0.0289(15) -0.0118(13) -0.0059(12) -0.0038(12) C11 0.0320(15) 0.0195(14) 0.0252(14) -0.0106(11) -0.0035(12) -0.0030(11) C12 0.048(2) 0.0234(15) 0.0271(15) -0.0069(12) -0.0128(14) -0.0088(14) C13 0.047(2) 0.044(2) 0.043(2) -0.0101(18) -0.0214(18) -0.0032(17) C14 0.079(3) 0.034(2) 0.045(2) 0.0038(17) -0.037(2) -0.021(2) C15 0.0333(16) 0.0275(16) 0.0327(16) -0.0172(14) 0.0043(13) -0.0091(13) C16 0.0253(14) 0.0221(14) 0.0252(14) -0.0106(12) -0.0010(11) -0.0064(11) C17 0.0266(14) 0.0275(15) 0.0264(14) -0.0101(12) -0.0083(11) -0.0057(11) C18 0.0255(14) 0.0212(14) 0.0302(15) -0.0074(12) -0.0072(11) -0.0004(11) C19 0.0376(18) 0.0370(18) 0.0368(17) -0.0228(15) -0.0197(14) 0.0107(14) C20 0.121(6) 0.083(4) 0.063(3) -0.051(3) -0.058(4) 0.054(4) C21 0.086(7) 0.095(7) 0.081(6) -0.038(6) -0.028(5) -0.025(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 O3 2.303(3) 2_676 ? Ag1 N1 2.335(3) . ? Ag1 N2 2.337(3) . ? Ag1 O4 2.377(3) . ? Ag1 Ag1 3.0640(5) 2_676 ? F1 C20 1.3790(11) . ? F2 C20 1.3803(11) . ? F3 C20 1.3793(11) . ? O1 C1 1.357(4) . ? O1 N1 1.407(3) . ? O2 C10 1.351(4) . ? O2 N2 1.407(4) . ? O3 C19 1.246(5) . ? O3 Ag1 2.303(3) 2_676 ? O4 C19 1.223(4) . ? O5 C21 1.447(15) . ? N1 C3 1.310(4) . ? N2 C12 1.306(4) . ? C1 C2 1.355(4) . ? C1 C4 1.485(5) . ? C2 C3 1.424(4) . ? C2 C6 1.506(4) . ? C3 C5 1.490(5) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.523(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.393(5) . ? C7 C9 1.394(5) . ? C8 C9 1.392(5) 2_767 ? C8 H8 0.9500 . ? C9 C8 1.392(5) 2_767 ? C9 H9 0.9500 . ? C10 C11 1.360(5) . ? C10 C13 1.476(5) . ? C11 C12 1.416(5) . ? C11 C15 1.502(4) . ? C12 C14 1.498(5) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.522(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C18 1.384(5) . ? C16 C17 1.392(5) . ? C17 C18 1.395(5) 2_786 ? C17 H17 0.9500 . ? C18 C17 1.395(5) 2_786 ? C18 H18 0.9500 . ? C19 C20 1.507(5) . ? C20 F1A 1.3782(11) . ? C20 F2B 1.3782(11) . ? C20 F2A 1.3793(11) . ? C20 F3B 1.3797(11) . ? C20 F1B 1.3804(11) . ? C20 F3A 1.3820(11) . ? C21 O5 1.447(15) 2_686 ? 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 O3 Ag1 N1 99.88(10) 2_676 . ? O3 Ag1 N2 116.19(12) 2_676 . ? N1 Ag1 N2 108.25(10) . . ? O3 Ag1 O4 140.68(11) 2_676 . ? N1 Ag1 O4 91.07(9) . . ? N2 Ag1 O4 95.35(11) . . ? O3 Ag1 Ag1 78.37(7) 2_676 2_676 ? N1 Ag1 Ag1 150.82(7) . 2_676 ? N2 Ag1 Ag1 98.26(8) . 2_676 ? O4 Ag1 Ag1 74.17(7) . 2_676 ? C1 O1 N1 107.9(2) . . ? C10 O2 N2 108.2(3) . . ? C19 O3 Ag1 117.6(2) . 2_676 ? C19 O4 Ag1 117.8(3) . . ? C3 N1 O1 106.4(2) . . ? C3 N1 Ag1 130.7(2) . . ? O1 N1 Ag1 120.21(17) . . ? C12 N2 O2 106.0(3) . . ? C12 N2 Ag1 134.0(3) . . ? O2 N2 Ag1 115.62(19) . . ? C2 C1 O1 110.1(3) . . ? C2 C1 C4 133.8(3) . . ? O1 C1 C4 116.1(3) . . ? C1 C2 C3 104.3(3) . . ? C1 C2 C6 128.9(3) . . ? C3 C2 C6 126.8(3) . . ? N1 C3 C2 111.3(3) . . ? N1 C3 C5 120.5(3) . . ? C2 C3 C5 128.2(3) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C2 C6 C7 111.8(2) . . ? C2 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? C2 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C8 C7 C9 118.4(3) . . ? C8 C7 C6 121.2(3) . . ? C9 C7 C6 120.4(3) . . ? C9 C8 C7 120.8(3) 2_767 . ? C9 C8 H8 119.6 2_767 . ? C7 C8 H8 119.6 . . ? C8 C9 C7 120.8(3) 2_767 . ? C8 C9 H9 119.6 2_767 . ? C7 C9 H9 119.6 . . ? O2 C10 C11 110.0(3) . . ? O2 C10 C13 116.8(3) . . ? C11 C10 C13 133.2(3) . . ? C10 C11 C12 104.0(3) . . ? C10 C11 C15 128.2(3) . . ? C12 C11 C15 127.7(3) . . ? N2 C12 C11 111.8(3) . . ? N2 C12 C14 119.8(4) . . ? C11 C12 C14 128.3(3) . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 113.2(3) . . ? C11 C15 H15A 108.9 . . ? C16 C15 H15A 108.9 . . ? C11 C15 H15B 108.9 . . ? C16 C15 H15B 108.9 . . ? H15A C15 H15B 107.8 . . ? C18 C16 C17 118.9(3) . . ? C18 C16 C15 120.7(3) . . ? C17 C16 C15 120.3(3) . . ? C16 C17 C18 120.6(3) . 2_786 ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 2_786 . ? C16 C18 C17 120.4(3) . 2_786 ? C16 C18 H18 119.8 . . ? C17 C18 H18 119.8 2_786 . ? O4 C19 O3 131.1(3) . . ? O4 C19 C20 112.4(3) . . ? O3 C19 C20 116.5(3) . . ? F1A C20 F2B 116.2(6) . . ? F1A C20 F1 23.8(3) . . ? F2B C20 F1 120.7(6) . . ? F1A C20 F3 116.7(8) . . ? F2B C20 F3 46.5(7) . . ? F1 C20 F3 101.7(7) . . ? F1A C20 F2A 109.6(5) . . ? F2B C20 F2A 28.6(4) . . ? F1 C20 F2A 126.0(5) . . ? F3 C20 F2A 75.0(7) . . ? F1A C20 F3B 69.3(9) . . ? F2B C20 F3B 98.3(9) . . ? F1 C20 F3B 46.9(8) . . ? F3 C20 F3B 59.3(8) . . ? F2A C20 F3B 123.6(10) . . ? F1A C20 F2 84.5(8) . . ? F2B C20 F2 57.7(7) . . ? F1 C20 F2 106.4(8) . . ? F3 C20 F2 103.2(8) . . ? F2A C20 F2 31.6(6) . . ? F3B C20 F2 132.0(13) . . ? F1A C20 F1B 34.7(6) . . ? F2B C20 F1B 100.5(8) . . ? F1 C20 F1B 58.5(6) . . ? F3 C20 F1B 129.5(11) . . ? F2A C20 F1B 81.9(8) . . ? F3B C20 F1B 101.9(9) . . ? F2 C20 F1B 52.2(9) . . ? F1A C20 F3A 103.0(5) . . ? F2B C20 F3A 77.0(6) . . ? F1 C20 F3A 81.4(5) . . ? F3 C20 F3A 30.8(6) . . ? F2A C20 F3A 105.7(5) . . ? F3B C20 F3A 34.5(7) . . ? F2 C20 F3A 131.6(8) . . ? F1B C20 F3A 132.2(8) . . ? F1A C20 C19 116.6(4) . . ? F2B C20 C19 122.9(5) . . ? F1 C20 C19 116.4(4) . . ? F3 C20 C19 119.6(8) . . ? F2A C20 C19 110.9(4) . . ? F3B C20 C19 119.4(11) . . ? F2 C20 C19 108.2(8) . . ? F1B C20 C19 110.4(8) . . ? F3A C20 C19 110.3(4) . . ? O5 C21 O5 180.000(5) 2_686 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.479 _refine_diff_density_min -1.545 _refine_diff_density_rms 0.153 #===end data_Compound-2b-k09adb04 _database_code_depnum_ccdc_archive 'CCDC 804681' #TrackingRef '- stevenson-rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H43 Ag2 F6 N5 O8' _chemical_formula_weight 1075.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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 10.7180(2) _cell_length_b 11.2600(2) _cell_length_c 20.7660(5) _cell_angle_alpha 75.779(1) _cell_angle_beta 81.104(1) _cell_angle_gamma 64.377(1) _cell_volume 2187.07(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 34727 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 25.028 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1084 _exptl_absorpt_coefficient_mu 0.978 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.828 _exptl_absorpt_correction_T_max 0.932 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28707 _diffrn_reflns_av_R_equivalents 0.0574 _diffrn_reflns_av_sigmaI/netI 0.0536 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7585 _reflns_number_gt 5709 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski, Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick 1990)' _computing_structure_refinement 'SHELXL-97/2 (Sheldrick 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle 1995)' _computing_publication_material 'SHELXL-97/2 (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. The fluorines attached to C4 disordered in a 45:55 ratio. Partial atoms refined anisotropically, subject to C-F, F...F and ADP restraints. The methyl group based on C2 disordered over 2 sites in a 75:25 ratio. 75% fractions refined anisotropically. C-F and F...F distance restraints employed in the final least squares cycles. Some disordered solvent in the lattice, which did not lend itself readily to being modeled, and hence PLATON SQUEEZE was employed. This algorithm indicated 2 small voids in the asymmetric unit, each with a volume of 67\%A3. As CH3CN was one of the solvents used in the recrystallisation, it is a reasonable assumption that each void contains one such solvent molecule, and the data presented are based on this thesis. ; _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^)+(0.0443P)^2^+1.6092P] 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 7585 _refine_ls_number_parameters 592 _refine_ls_number_restraints 97 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.0972 _refine_ls_wR_factor_gt 0.0899 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.038 _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 Ag1 Ag 0.37344(3) 0.36124(3) 0.216760(17) 0.03776(12) Uani 1 1 d . . . Ag2 Ag 0.60167(3) 0.10755(3) 0.290856(16) 0.03118(11) Uani 1 1 d . . . O5 O 0.9382(3) -0.0362(2) 0.31507(13) 0.0292(6) Uani 1 1 d . . . O7 O 0.0484(3) 0.5273(2) 0.17769(13) 0.0281(6) Uani 1 1 d . . . O8 O 0.4749(3) 0.5789(3) 0.09952(14) 0.0352(7) Uani 1 1 d . . . C32 C 0.7244(5) 0.2348(4) 0.1195(2) 0.0452(12) Uani 1 1 d . . . H32A H 0.8135 0.2217 0.1335 0.068 Uiso 1 1 calc R . . H32B H 0.7406 0.1880 0.0830 0.068 Uiso 1 1 calc R . . H32C H 0.6749 0.1986 0.1571 0.068 Uiso 1 1 calc R . . N3 N 0.1614(3) 0.5456(3) 0.19410(16) 0.0280(7) Uani 1 1 d . . . N1 N 0.8300(3) -0.0648(3) 0.30151(15) 0.0252(7) Uani 1 1 d . . . O3 O 0.4403(3) 0.4303(3) 0.29687(14) 0.0369(7) Uani 1 1 d . . . C35 C 0.5562(4) 0.5906(4) 0.0439(2) 0.0287(9) Uani 1 1 d . . . C40 C 1.1026(4) 0.4106(4) 0.0426(2) 0.0302(9) Uani 1 1 d . . . H40 H 1.1728 0.3483 0.0718 0.036 Uiso 1 1 calc R . . C39 C 0.9951(4) 0.3807(4) 0.0335(2) 0.0290(9) Uani 1 1 d . . . H39 H 0.9924 0.2979 0.0570 0.035 Uiso 1 1 calc R . . C6 C 0.8731(4) -0.1961(4) 0.31713(18) 0.0250(9) Uani 1 1 d . . . O6 O 0.5120(3) -0.1055(3) 0.39551(15) 0.0394(7) Uani 1 1 d . . . O2 O 0.5556(3) 0.0341(3) 0.20410(15) 0.0388(7) Uani 1 1 d . . . C18 C 0.4571(5) -0.2737(5) 0.4765(3) 0.0527(13) Uani 1 1 d . . . H18A H 0.4200 -0.3009 0.4451 0.079 Uiso 1 1 calc R . . H18B H 0.4088 -0.2833 0.5203 0.079 Uiso 1 1 calc R . . H18C H 0.5563 -0.3310 0.4802 0.079 Uiso 1 1 calc R . . O1 O 0.3534(3) 0.2043(3) 0.17311(17) 0.0474(8) Uani 1 1 d . . . C25 C -0.0087(4) 0.7474(4) 0.15634(18) 0.0256(9) Uani 1 1 d . . . C26 C -0.0513(4) 0.6516(4) 0.15491(18) 0.0260(9) Uani 1 1 d . . . C21 C 0.0379(4) 0.1031(4) 0.4683(2) 0.0330(10) Uani 1 1 d . . . H21 H 0.0637 0.1744 0.4464 0.040 Uiso 1 1 calc R . . C7 C 1.0094(4) -0.2590(4) 0.34086(18) 0.0269(9) Uani 1 1 d . . . C29 C -0.0409(4) 0.9508(4) 0.06483(19) 0.0267(9) Uani 1 1 d . . . O4 O 0.6617(3) 0.2770(3) 0.29710(18) 0.0484(8) Uani 1 1 d . . . C24 C 0.1262(4) 0.6756(4) 0.18100(19) 0.0255(9) Uani 1 1 d . . . C17 C 0.4362(4) -0.1306(4) 0.4521(2) 0.0360(10) Uani 1 1 d . . . C23 C 0.2232(4) 0.7305(4) 0.1926(2) 0.0293(9) Uani 1 1 d . . . H23A H 0.2953 0.6609 0.2215 0.044 Uiso 1 1 calc R . . H23B H 0.1718 0.8080 0.2140 0.044 Uiso 1 1 calc R . . H23C H 0.2662 0.7588 0.1499 0.044 Uiso 1 1 calc R . . C20 C 0.1210(4) 0.0018(4) 0.51687(19) 0.0297(9) Uani 1 1 d . . . N4 N 0.5291(4) 0.4435(3) 0.13321(18) 0.0382(9) Uani 1 1 d . . . C31 C -0.0623(4) 1.0013(4) -0.0537(2) 0.0291(9) Uani 1 1 d . . . H31 H -0.1057 1.0016 -0.0903 0.035 Uiso 1 1 calc R . . C3 C 0.5662(5) 0.3875(4) 0.3028(2) 0.0364(10) Uani 1 1 d . A . C34 C 0.6599(4) 0.4698(4) 0.0384(2) 0.0275(9) Uani 1 1 d . . . C8 C 1.0431(4) -0.1547(4) 0.33915(19) 0.0279(9) Uani 1 1 d . . . C5 C 0.7841(4) -0.2611(4) 0.3083(2) 0.0341(10) Uani 1 1 d . . . H5A H 0.7474 -0.2937 0.3520 0.051 Uiso 1 1 calc R . . H5B H 0.8390 -0.3370 0.2863 0.051 Uiso 1 1 calc R . . H5C H 0.7070 -0.1957 0.2810 0.051 Uiso 1 1 calc R . . C37 C 0.7715(4) 0.4361(4) -0.0161(2) 0.0355(10) Uani 1 1 d . . . H37A H 0.7308 0.4870 -0.0594 0.043 Uiso 1 1 calc R . . H37B H 0.8069 0.3391 -0.0163 0.043 Uiso 1 1 calc R . . N2 N 0.4775(3) 0.0339(3) 0.37970(18) 0.0372(9) Uani 1 1 d . . . C16 C 0.3566(4) -0.0159(4) 0.4739(2) 0.0321(10) Uani 1 1 d . . . C22 C -0.0817(4) 0.1018(4) 0.45149(19) 0.0310(9) Uani 1 1 d . . . H22 H -0.1368 0.1718 0.4183 0.037 Uiso 1 1 calc R . . C30 C -0.1020(4) 0.9532(4) 0.0105(2) 0.0292(9) Uani 1 1 d . . . H30 H -0.1727 0.9213 0.0172 0.035 Uiso 1 1 calc R . . C33 C 0.6400(4) 0.3806(4) 0.0967(2) 0.0322(10) Uani 1 1 d . . . C28 C -0.0855(4) 0.8981(4) 0.13541(19) 0.0287(9) Uani 1 1 d . . . H28A H -0.0683 0.9424 0.1667 0.034 Uiso 1 1 calc R . . H28B H -0.1863 0.9219 0.1379 0.034 Uiso 1 1 calc R . . C13 C 1.0418(4) -0.4770(4) 0.5542(2) 0.0374(11) Uani 1 1 d . . . H13 H 1.0716 -0.4608 0.5907 0.045 Uiso 1 1 calc R . . C19 C 0.2539(4) 0.0015(5) 0.5328(2) 0.0373(10) Uani 1 1 d . . . H19A H 0.2336 0.0872 0.5457 0.045 Uiso 1 1 calc R . . H19B H 0.2944 -0.0726 0.5709 0.045 Uiso 1 1 calc R . . C12 C 1.0853(4) -0.4348(4) 0.4896(2) 0.0364(10) Uani 1 1 d . . . H12 H 1.1443 -0.3891 0.4827 0.044 Uiso 1 1 calc R . . C15 C 0.3856(4) 0.0852(4) 0.4259(2) 0.0341(10) Uani 1 1 d . . . C1 C 0.4452(4) 0.0895(4) 0.1768(2) 0.0331(10) Uani 1 1 d D . . C9 C 1.1683(4) -0.1463(5) 0.3558(2) 0.0414(11) Uani 1 1 d . . . H9A H 1.1874 -0.0772 0.3223 0.062 Uiso 1 1 calc R . . H9B H 1.2476 -0.2334 0.3565 0.062 Uiso 1 1 calc R . . H9C H 1.1526 -0.1228 0.3997 0.062 Uiso 1 1 calc R . . C11 C 1.0460(4) -0.4569(4) 0.4346(2) 0.0315(10) Uani 1 1 d . . . C27 C -0.1806(4) 0.6532(4) 0.1359(2) 0.0363(10) Uani 1 1 d . . . H27A H -0.1609 0.6158 0.0957 0.054 Uiso 1 1 calc R . . H27B H -0.2510 0.7459 0.1273 0.054 Uiso 1 1 calc R . . H27C H -0.2148 0.5988 0.1723 0.054 Uiso 1 1 calc R . . C10 C 1.0913(4) -0.4069(4) 0.3645(2) 0.0347(10) Uani 1 1 d . . . H10A H 1.1908 -0.4256 0.3629 0.042 Uiso 1 1 calc R . . H10B H 1.0802 -0.4566 0.3341 0.042 Uiso 1 1 calc R . . C36 C 0.5166(5) 0.7280(4) 0.0027(2) 0.0448(12) Uani 1 1 d . . . H36A H 0.5593 0.7755 0.0191 0.067 Uiso 1 1 calc R . . H36B H 0.4156 0.7770 0.0055 0.067 Uiso 1 1 calc R . . H36C H 0.5489 0.7221 -0.0437 0.067 Uiso 1 1 calc R . . C38 C 0.8914(4) 0.4680(4) -0.00884(19) 0.0262(9) Uani 1 1 d . . . C14 C 0.3264(5) 0.2307(4) 0.4246(3) 0.0459(12) Uani 1 1 d . . . H4A1 H 0.3950 0.2666 0.4042 0.069 Uiso 1 1 calc R . . H4A2 H 0.3011 0.2463 0.4701 0.069 Uiso 1 1 calc R . . H4A3 H 0.2436 0.2760 0.3985 0.069 Uiso 1 1 calc R . . C4 C 0.6129(5) 0.4858(4) 0.3208(2) 0.0470(12) Uani 1 1 d D . . F5 F 0.5669(15) 0.6013(10) 0.2807(6) 0.094(5) Uani 0.45 1 d PDU A 1 F4 F 0.5590(19) 0.5070(17) 0.3802(5) 0.129(5) Uani 0.45 1 d PDU A 1 F6 F 0.7429(9) 0.4459(12) 0.3236(10) 0.128(7) Uani 0.45 1 d PDU A 1 F5A F 0.5219(10) 0.6087(8) 0.3170(6) 0.091(4) Uani 0.55 1 d PDU A 2 F4A F 0.6584(12) 0.4463(9) 0.3817(4) 0.072(2) Uani 0.55 1 d PDU A 2 F6A F 0.7230(9) 0.4910(11) 0.2829(5) 0.087(3) Uani 0.55 1 d PDU A 2 F1 F 0.3026(6) 0.0579(6) 0.1096(4) 0.100(3) Uani 0.75 1 d PD B 1 F2 F 0.4355(7) -0.1175(5) 0.1757(3) 0.0892(19) Uani 0.75 1 d PD B 1 F3 F 0.5238(5) -0.0311(4) 0.0877(2) 0.0759(13) Uani 0.75 1 d PD B 1 F1A F 0.2813(16) -0.0109(18) 0.1855(8) 0.105(5) Uiso 0.25 1 d PD C 2 F2A F 0.4852(17) -0.1184(19) 0.1508(10) 0.091(8) Uiso 0.25 1 d PD C 2 F3A F 0.3512(18) 0.055(2) 0.0889(8) 0.072(6) Uiso 0.25 1 d PD C 2 C2 C 0.4280(9) -0.0002(6) 0.1353(5) 0.052(2) Uani 0.75 1 d PD B 1 C2A C 0.3904(19) 0.0043(19) 0.1505(9) 0.045(9) Uiso 0.25 1 d PD C 2 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 Ag1 0.03348(19) 0.02810(18) 0.0470(2) -0.01082(15) -0.01273(16) -0.00316(15) Ag2 0.02917(18) 0.02693(18) 0.0349(2) -0.00447(14) -0.00502(14) -0.00906(14) O5 0.0309(15) 0.0264(14) 0.0278(15) -0.0032(12) -0.0028(12) -0.0102(13) O7 0.0282(14) 0.0234(14) 0.0286(15) -0.0023(12) -0.0023(12) -0.0082(12) O8 0.0294(15) 0.0302(15) 0.0414(18) -0.0130(13) 0.0077(13) -0.0081(13) C32 0.038(2) 0.033(2) 0.055(3) -0.006(2) 0.006(2) -0.010(2) N3 0.0295(18) 0.0262(18) 0.0250(18) -0.0010(14) -0.0027(14) -0.0103(15) N1 0.0248(17) 0.0249(18) 0.0251(18) -0.0046(14) -0.0040(14) -0.0088(15) O3 0.0342(17) 0.0376(16) 0.0391(18) -0.0081(14) -0.0038(13) -0.0142(14) C35 0.024(2) 0.031(2) 0.033(2) -0.0083(18) 0.0017(18) -0.0129(19) C40 0.025(2) 0.033(2) 0.028(2) -0.0074(18) -0.0003(18) -0.0068(19) C39 0.031(2) 0.030(2) 0.029(2) -0.0056(18) 0.0053(18) -0.0168(19) C6 0.027(2) 0.025(2) 0.018(2) -0.0062(16) 0.0047(16) -0.0068(18) O6 0.0323(15) 0.0356(16) 0.0431(19) -0.0088(14) 0.0075(14) -0.0100(14) O2 0.0313(16) 0.0352(16) 0.0479(19) -0.0100(14) -0.0168(14) -0.0062(14) C18 0.047(3) 0.038(3) 0.066(4) 0.000(2) -0.004(3) -0.016(2) O1 0.0423(18) 0.0310(17) 0.068(2) -0.0130(15) -0.0219(17) -0.0069(16) C25 0.029(2) 0.024(2) 0.018(2) -0.0052(16) 0.0053(16) -0.0067(18) C26 0.026(2) 0.027(2) 0.018(2) -0.0018(16) -0.0001(16) -0.0066(18) C21 0.037(2) 0.035(2) 0.030(2) -0.0067(19) 0.0042(19) -0.020(2) C7 0.029(2) 0.027(2) 0.018(2) -0.0050(16) 0.0031(16) -0.0065(18) C29 0.028(2) 0.0162(18) 0.026(2) -0.0024(16) 0.0018(17) -0.0022(17) O4 0.0358(17) 0.0270(16) 0.083(3) -0.0108(16) -0.0133(17) -0.0102(15) C24 0.027(2) 0.021(2) 0.020(2) -0.0045(16) 0.0042(16) -0.0042(17) C17 0.031(2) 0.042(3) 0.035(3) -0.006(2) -0.002(2) -0.017(2) C23 0.029(2) 0.025(2) 0.030(2) -0.0056(17) 0.0005(18) -0.0075(18) C20 0.027(2) 0.042(2) 0.024(2) -0.0151(19) 0.0061(17) -0.016(2) N4 0.034(2) 0.0300(19) 0.044(2) -0.0035(17) 0.0042(17) -0.0109(17) C31 0.034(2) 0.024(2) 0.027(2) -0.0023(17) -0.0077(18) -0.0100(19) C3 0.039(3) 0.029(2) 0.041(3) 0.0016(19) -0.011(2) -0.016(2) C34 0.025(2) 0.036(2) 0.030(2) -0.0136(18) 0.0001(17) -0.0170(19) C8 0.025(2) 0.032(2) 0.020(2) -0.0049(17) 0.0009(16) -0.0066(19) C5 0.042(2) 0.031(2) 0.034(2) -0.0088(19) 0.002(2) -0.019(2) C37 0.034(2) 0.043(2) 0.037(3) -0.018(2) 0.0052(19) -0.020(2) N2 0.0274(18) 0.033(2) 0.046(2) -0.0051(17) 0.0026(17) -0.0100(16) C16 0.025(2) 0.044(3) 0.032(2) -0.008(2) -0.0028(18) -0.018(2) C22 0.031(2) 0.034(2) 0.022(2) -0.0008(18) -0.0003(18) -0.0103(19) C30 0.029(2) 0.026(2) 0.030(2) -0.0023(17) 0.0019(18) -0.0121(18) C33 0.025(2) 0.032(2) 0.041(3) -0.012(2) 0.0016(19) -0.0126(19) C28 0.030(2) 0.0209(19) 0.025(2) -0.0026(17) 0.0037(17) -0.0037(17) C13 0.045(3) 0.033(2) 0.027(2) -0.0024(19) 0.000(2) -0.011(2) C19 0.036(2) 0.053(3) 0.030(2) -0.011(2) 0.0000(19) -0.023(2) C12 0.037(2) 0.030(2) 0.034(3) 0.0012(19) -0.001(2) -0.011(2) C15 0.021(2) 0.040(2) 0.042(3) -0.009(2) -0.0025(19) -0.0120(19) C1 0.033(2) 0.028(2) 0.039(3) -0.0026(19) -0.007(2) -0.014(2) C9 0.034(2) 0.043(3) 0.046(3) -0.010(2) -0.007(2) -0.013(2) C11 0.030(2) 0.021(2) 0.028(2) -0.0007(17) -0.0002(18) 0.0015(18) C27 0.036(2) 0.037(2) 0.033(2) -0.0033(19) -0.0008(19) -0.015(2) C10 0.038(2) 0.025(2) 0.027(2) -0.0015(18) 0.0028(19) -0.0035(19) C36 0.043(3) 0.035(2) 0.048(3) -0.004(2) -0.005(2) -0.009(2) C38 0.0220(19) 0.032(2) 0.027(2) -0.0122(18) 0.0059(17) -0.0117(18) C14 0.039(3) 0.041(3) 0.060(3) -0.016(2) 0.002(2) -0.016(2) C4 0.051(3) 0.037(3) 0.054(3) -0.010(2) -0.011(3) -0.017(3) F5 0.141(12) 0.052(7) 0.116(10) 0.020(6) -0.047(8) -0.071(8) F4 0.222(15) 0.155(13) 0.098(10) -0.066(10) 0.024(10) -0.147(12) F6 0.064(7) 0.063(7) 0.28(2) -0.049(11) -0.081(11) -0.011(5) F5A 0.081(5) 0.029(4) 0.161(11) -0.034(6) -0.054(7) 0.001(4) F4A 0.110(6) 0.068(5) 0.058(5) -0.004(4) -0.028(5) -0.054(5) F6A 0.107(8) 0.098(8) 0.103(6) -0.051(5) 0.048(6) -0.088(7) F1 0.057(4) 0.080(4) 0.180(7) -0.072(5) -0.066(4) 0.001(3) F2 0.132(5) 0.056(3) 0.114(5) -0.005(3) -0.024(5) -0.071(3) F3 0.093(3) 0.066(3) 0.073(3) -0.049(2) -0.016(3) -0.014(2) C2 0.035(4) 0.026(4) 0.096(7) -0.012(4) -0.031(5) -0.006(3) _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 Ag1 O1 2.273(3) . ? Ag1 O3 2.318(3) . ? Ag1 N3 2.338(3) . ? Ag1 N4 2.511(4) . ? Ag1 Ag2 3.0777(4) . ? Ag2 O4 2.298(3) . ? Ag2 N2 2.304(4) . ? Ag2 O2 2.352(3) . ? Ag2 N1 2.378(3) . ? O5 C8 1.357(4) . ? O5 N1 1.414(4) . ? O7 C26 1.364(4) . ? O7 N3 1.416(4) . ? O8 C35 1.350(5) . ? O8 N4 1.410(4) . ? C32 C33 1.485(6) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? N3 C24 1.311(5) . ? N1 C6 1.313(5) . ? O3 C3 1.237(5) . ? C35 C34 1.353(5) . ? C35 C36 1.483(6) . ? C40 C39 1.382(5) . ? C40 C38 1.399(6) 2_765 ? C40 H40 0.9500 . ? C39 C38 1.381(6) . ? C39 H39 0.9500 . ? C6 C7 1.426(5) . ? C6 C5 1.485(6) . ? O6 C17 1.365(5) . ? O6 N2 1.410(4) . ? O2 C1 1.227(5) . ? C18 C17 1.492(6) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? O1 C1 1.232(5) . ? C25 C26 1.348(5) . ? C25 C24 1.422(5) . ? C25 C28 1.513(5) . ? C26 C27 1.490(6) . ? C21 C22 1.387(6) . ? C21 C20 1.394(6) . ? C21 H21 0.9500 . ? C7 C8 1.361(6) . ? C7 C10 1.501(5) . ? C29 C30 1.378(6) . ? C29 C31 1.394(6) 2_575 ? C29 C28 1.526(5) . ? O4 C3 1.242(5) . ? C24 C23 1.493(6) . ? C17 C16 1.348(6) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C20 C22 1.390(6) 2_556 ? C20 C19 1.510(5) . ? N4 C33 1.322(5) . ? C31 C30 1.386(6) . ? C31 C29 1.394(6) 2_575 ? C31 H31 0.9500 . ? C3 C4 1.535(6) . ? C34 C33 1.423(6) . ? C34 C37 1.501(6) . ? C8 C9 1.483(6) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C37 C38 1.513(5) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? N2 C15 1.308(5) . ? C16 C15 1.429(6) . ? C16 C19 1.503(6) . ? C22 C20 1.390(6) 2_556 ? C22 H22 0.9500 . ? C30 H30 0.9500 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C13 C12 1.389(6) . ? C13 C11 1.394(6) 2_746 ? C13 H13 0.9500 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C12 C11 1.385(6) . ? C12 H12 0.9500 . ? C15 C14 1.473(6) . ? C1 C2A 1.552(16) . ? C1 C2 1.562(7) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C11 C13 1.394(6) 2_746 ? C11 C10 1.514(6) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C38 C40 1.399(6) 2_765 ? C14 H4A1 0.9800 . ? C14 H4A2 0.9800 . ? C14 H4A3 0.9800 . ? C4 F6 1.272(9) . ? C4 F5 1.293(9) . ? C4 F5A 1.295(8) . ? C4 F4 1.310(9) . ? C4 F4A 1.326(8) . ? C4 F6A 1.329(8) . ? F1 C2 1.345(7) . ? F2 C2 1.356(8) . ? F3 C2 1.303(10) . ? F1A C2A 1.333(14) . ? F2A C2A 1.313(14) . ? F3A C2A 1.318(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ag1 O3 153.32(11) . . ? O1 Ag1 N3 102.32(11) . . ? O3 Ag1 N3 98.43(10) . . ? O1 Ag1 N4 104.34(12) . . ? O3 Ag1 N4 88.41(11) . . ? N3 Ag1 N4 99.50(11) . . ? O1 Ag1 Ag2 80.97(7) . . ? O3 Ag1 Ag2 74.10(7) . . ? N3 Ag1 Ag2 161.25(8) . . ? N4 Ag1 Ag2 97.48(8) . . ? O4 Ag2 N2 118.59(13) . . ? O4 Ag2 O2 135.06(12) . . ? N2 Ag2 O2 101.77(12) . . ? O4 Ag2 N1 95.34(10) . . ? N2 Ag2 N1 103.43(11) . . ? O2 Ag2 N1 93.56(10) . . ? O4 Ag2 Ag1 76.75(7) . . ? N2 Ag2 Ag1 102.14(8) . . ? O2 Ag2 Ag1 76.18(7) . . ? N1 Ag2 Ag1 153.91(8) . . ? C8 O5 N1 107.8(3) . . ? C26 O7 N3 107.5(3) . . ? C35 O8 N4 108.3(3) . . ? C33 C32 H32A 109.5 . . ? C33 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C33 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C24 N3 O7 106.4(3) . . ? C24 N3 Ag1 132.3(3) . . ? O7 N3 Ag1 120.0(2) . . ? C6 N1 O5 106.4(3) . . ? C6 N1 Ag2 130.4(3) . . ? O5 N1 Ag2 119.8(2) . . ? C3 O3 Ag1 116.7(3) . . ? O8 C35 C34 110.5(3) . . ? O8 C35 C36 115.9(3) . . ? C34 C35 C36 133.5(4) . . ? C39 C40 C38 120.3(4) . 2_765 ? C39 C40 H40 119.8 . . ? C38 C40 H40 119.8 2_765 . ? C40 C39 C38 121.7(4) . . ? C40 C39 H39 119.1 . . ? C38 C39 H39 119.1 . . ? N1 C6 C7 111.3(3) . . ? N1 C6 C5 120.6(3) . . ? C7 C6 C5 128.1(3) . . ? C17 O6 N2 107.7(3) . . ? C1 O2 Ag2 123.4(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C1 O1 Ag1 122.0(3) . . ? C26 C25 C24 104.9(3) . . ? C26 C25 C28 128.0(4) . . ? C24 C25 C28 127.1(4) . . ? C25 C26 O7 110.1(3) . . ? C25 C26 C27 134.4(4) . . ? O7 C26 C27 115.4(3) . . ? C22 C21 C20 121.3(4) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C8 C7 C6 104.2(3) . . ? C8 C7 C10 129.2(4) . . ? C6 C7 C10 126.5(4) . . ? C30 C29 C31 118.2(4) . 2_575 ? C30 C29 C28 121.0(4) . . ? C31 C29 C28 120.7(4) 2_575 . ? C3 O4 Ag2 117.5(3) . . ? N3 C24 C25 111.1(3) . . ? N3 C24 C23 120.5(3) . . ? C25 C24 C23 128.4(3) . . ? C16 C17 O6 110.4(4) . . ? C16 C17 C18 133.8(4) . . ? O6 C17 C18 115.8(4) . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C20 C21 118.6(4) 2_556 . ? C22 C20 C19 120.6(4) 2_556 . ? C21 C20 C19 120.7(4) . . ? C33 N4 O8 105.6(3) . . ? C33 N4 Ag1 132.1(3) . . ? O8 N4 Ag1 118.5(2) . . ? C30 C31 C29 120.4(4) . 2_575 ? C30 C31 H31 119.8 . . ? C29 C31 H31 119.8 2_575 . ? O3 C3 O4 130.5(4) . . ? O3 C3 C4 115.1(4) . . ? O4 C3 C4 114.3(4) . . ? C35 C34 C33 104.1(3) . . ? C35 C34 C37 128.4(4) . . ? C33 C34 C37 127.5(4) . . ? O5 C8 C7 110.2(3) . . ? O5 C8 C9 116.2(4) . . ? C7 C8 C9 133.5(4) . . ? C6 C5 H5A 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C6 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C34 C37 C38 113.2(3) . . ? C34 C37 H37A 108.9 . . ? C38 C37 H37A 108.9 . . ? C34 C37 H37B 108.9 . . ? C38 C37 H37B 108.9 . . ? H37A C37 H37B 107.8 . . ? C15 N2 O6 106.2(3) . . ? C15 N2 Ag2 137.2(3) . . ? O6 N2 Ag2 116.4(2) . . ? C17 C16 C15 104.1(4) . . ? C17 C16 C19 127.4(4) . . ? C15 C16 C19 128.4(4) . . ? C21 C22 C20 120.1(4) . 2_556 ? C21 C22 H22 120.0 . . ? C20 C22 H22 120.0 2_556 . ? C29 C30 C31 121.4(4) . . ? C29 C30 H30 119.3 . . ? C31 C30 H30 119.3 . . ? N4 C33 C34 111.5(4) . . ? N4 C33 C32 119.3(4) . . ? C34 C33 C32 129.2(4) . . ? C25 C28 C29 112.2(3) . . ? C25 C28 H28A 109.2 . . ? C29 C28 H28A 109.2 . . ? C25 C28 H28B 109.2 . . ? C29 C28 H28B 109.2 . . ? H28A C28 H28B 107.9 . . ? C12 C13 C11 119.8(4) . 2_746 ? C12 C13 H13 120.1 . . ? C11 C13 H13 120.1 2_746 . ? C16 C19 C20 111.1(3) . . ? C16 C19 H19A 109.4 . . ? C20 C19 H19A 109.4 . . ? C16 C19 H19B 109.4 . . ? C20 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? C11 C12 C13 122.5(4) . . ? C11 C12 H12 118.8 . . ? C13 C12 H12 118.8 . . ? N2 C15 C16 111.6(4) . . ? N2 C15 C14 120.6(4) . . ? C16 C15 C14 127.8(4) . . ? O2 C1 O1 131.3(4) . . ? O2 C1 C2A 119.5(8) . . ? O1 C1 C2A 108.4(8) . . ? O2 C1 C2 112.2(4) . . ? O1 C1 C2 116.2(4) . . ? C2A C1 C2 17.1(8) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C11 C13 117.8(4) . 2_746 ? C12 C11 C10 121.7(4) . . ? C13 C11 C10 120.5(4) 2_746 . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C7 C10 C11 112.2(3) . . ? C7 C10 H10A 109.2 . . ? C11 C10 H10A 109.2 . . ? C7 C10 H10B 109.2 . . ? C11 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C39 C38 C40 117.9(3) . 2_765 ? C39 C38 C37 121.0(4) . . ? C40 C38 C37 121.0(4) 2_765 . ? C15 C14 H4A1 109.5 . . ? C15 C14 H4A2 109.5 . . ? H4A1 C14 H4A2 109.5 . . ? C15 C14 H4A3 109.5 . . ? H4A1 C14 H4A3 109.5 . . ? H4A2 C14 H4A3 109.5 . . ? F6 C4 F5 108.2(9) . . ? F6 C4 F5A 125.6(8) . . ? F5 C4 F5A 37.5(6) . . ? F6 C4 F4 106.0(8) . . ? F5 C4 F4 106.6(8) . . ? F5A C4 F4 69.8(8) . . ? F6 C4 F4A 64.7(8) . . ? F5 C4 F4A 132.9(8) . . ? F5A C4 F4A 105.9(7) . . ? F4 C4 F4A 43.9(7) . . ? F6 C4 F6A 39.3(8) . . ? F5 C4 F6A 74.9(7) . . ? F5A C4 F6A 106.6(7) . . ? F4 C4 F6A 136.6(8) . . ? F4A C4 F6A 102.6(6) . . ? F6 C4 C3 115.8(7) . . ? F5 C4 C3 111.5(7) . . ? F5A C4 C3 116.6(6) . . ? F4 C4 C3 108.3(6) . . ? F4A C4 C3 112.9(5) . . ? F6A C4 C3 111.1(6) . . ? F3 C2 F1 109.3(7) . . ? F3 C2 F2 107.0(6) . . ? F1 C2 F2 106.0(7) . . ? F3 C2 C1 113.3(6) . . ? F1 C2 C1 111.5(6) . . ? F2 C2 C1 109.4(6) . . ? F2A C2A F3A 106.3(13) . . ? F2A C2A F1A 105.1(13) . . ? F3A C2A F1A 104.9(12) . . ? F2A C2A C1 111.7(16) . . ? F3A C2A C1 113.3(16) . . ? F1A C2A C1 114.8(15) . . ? 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 O1 Ag1 Ag2 O4 158.90(13) . . . . ? O3 Ag1 Ag2 O4 -30.70(12) . . . . ? N3 Ag1 Ag2 O4 -99.3(3) . . . . ? N4 Ag1 Ag2 O4 55.49(13) . . . . ? O1 Ag1 Ag2 N2 -84.21(13) . . . . ? O3 Ag1 Ag2 N2 86.19(12) . . . . ? N3 Ag1 Ag2 N2 17.6(3) . . . . ? N4 Ag1 Ag2 N2 172.37(12) . . . . ? O1 Ag1 Ag2 O2 15.11(12) . . . . ? O3 Ag1 Ag2 O2 -174.49(10) . . . . ? N3 Ag1 Ag2 O2 116.9(3) . . . . ? N4 Ag1 Ag2 O2 -88.31(12) . . . . ? O1 Ag1 Ag2 N1 84.19(19) . . . . ? O3 Ag1 Ag2 N1 -105.41(18) . . . . ? N3 Ag1 Ag2 N1 -174.0(3) . . . . ? N4 Ag1 Ag2 N1 -19.23(19) . . . . ? C26 O7 N3 C24 0.0(4) . . . . ? C26 O7 N3 Ag1 -168.7(2) . . . . ? O1 Ag1 N3 C24 -148.0(3) . . . . ? O3 Ag1 N3 C24 48.9(4) . . . . ? N4 Ag1 N3 C24 -40.9(4) . . . . ? Ag2 Ag1 N3 C24 113.8(4) . . . . ? O1 Ag1 N3 O7 17.3(3) . . . . ? O3 Ag1 N3 O7 -145.8(2) . . . . ? N4 Ag1 N3 O7 124.4(2) . . . . ? Ag2 Ag1 N3 O7 -81.0(4) . . . . ? C8 O5 N1 C6 -0.4(4) . . . . ? C8 O5 N1 Ag2 161.0(2) . . . . ? O4 Ag2 N1 C6 162.6(3) . . . . ? N2 Ag2 N1 C6 41.5(3) . . . . ? O2 Ag2 N1 C6 -61.5(3) . . . . ? Ag1 Ag2 N1 C6 -126.9(3) . . . . ? O4 Ag2 N1 O5 6.2(3) . . . . ? N2 Ag2 N1 O5 -114.9(2) . . . . ? O2 Ag2 N1 O5 142.1(2) . . . . ? Ag1 Ag2 N1 O5 76.8(3) . . . . ? O1 Ag1 O3 C3 66.3(4) . . . . ? N3 Ag1 O3 C3 -152.9(3) . . . . ? N4 Ag1 O3 C3 -53.5(3) . . . . ? Ag2 Ag1 O3 C3 44.7(3) . . . . ? N4 O8 C35 C34 1.1(4) . . . . ? N4 O8 C35 C36 -178.5(3) . . . . ? C38 C40 C39 C38 0.4(7) 2_765 . . . ? O5 N1 C6 C7 -0.3(4) . . . . ? Ag2 N1 C6 C7 -159.1(3) . . . . ? O5 N1 C6 C5 -179.5(3) . . . . ? Ag2 N1 C6 C5 21.8(5) . . . . ? O4 Ag2 O2 C1 -78.6(4) . . . . ? N2 Ag2 O2 C1 75.7(3) . . . . ? N1 Ag2 O2 C1 -179.8(3) . . . . ? Ag1 Ag2 O2 C1 -24.1(3) . . . . ? O3 Ag1 O1 C1 -37.8(5) . . . . ? N3 Ag1 O1 C1 -178.1(3) . . . . ? N4 Ag1 O1 C1 78.6(4) . . . . ? Ag2 Ag1 O1 C1 -16.9(3) . . . . ? C24 C25 C26 O7 0.6(4) . . . . ? C28 C25 C26 O7 179.7(3) . . . . ? C24 C25 C26 C27 178.9(4) . . . . ? C28 C25 C26 C27 -2.0(7) . . . . ? N3 O7 C26 C25 -0.4(4) . . . . ? N3 O7 C26 C27 -179.1(3) . . . . ? N1 C6 C7 C8 0.9(4) . . . . ? C5 C6 C7 C8 -180.0(4) . . . . ? N1 C6 C7 C10 178.8(4) . . . . ? C5 C6 C7 C10 -2.1(6) . . . . ? N2 Ag2 O4 C3 -61.7(4) . . . . ? O2 Ag2 O4 C3 89.4(4) . . . . ? N1 Ag2 O4 C3 -170.2(3) . . . . ? Ag1 Ag2 O4 C3 35.1(3) . . . . ? O7 N3 C24 C25 0.4(4) . . . . ? Ag1 N3 C24 C25 167.1(3) . . . . ? O7 N3 C24 C23 -179.8(3) . . . . ? Ag1 N3 C24 C23 -13.1(6) . . . . ? C26 C25 C24 N3 -0.6(4) . . . . ? C28 C25 C24 N3 -179.7(4) . . . . ? C26 C25 C24 C23 179.6(4) . . . . ? C28 C25 C24 C23 0.5(6) . . . . ? N2 O6 C17 C16 -0.8(4) . . . . ? N2 O6 C17 C18 179.2(4) . . . . ? C22 C21 C20 C22 0.0(6) . . . 2_556 ? C22 C21 C20 C19 177.5(4) . . . . ? C35 O8 N4 C33 0.2(4) . . . . ? C35 O8 N4 Ag1 -160.4(2) . . . . ? O1 Ag1 N4 C33 -38.8(4) . . . . ? O3 Ag1 N4 C33 117.5(4) . . . . ? N3 Ag1 N4 C33 -144.2(4) . . . . ? Ag2 Ag1 N4 C33 43.8(4) . . . . ? O1 Ag1 N4 O8 115.8(3) . . . . ? O3 Ag1 N4 O8 -88.0(3) . . . . ? N3 Ag1 N4 O8 10.3(3) . . . . ? Ag2 Ag1 N4 O8 -161.7(2) . . . . ? Ag1 O3 C3 O4 -35.3(6) . . . . ? Ag1 O3 C3 C4 145.4(3) . . . . ? Ag2 O4 C3 O3 -11.2(7) . . . . ? Ag2 O4 C3 C4 168.2(3) . . . . ? O8 C35 C34 C33 -1.8(4) . . . . ? C36 C35 C34 C33 177.7(4) . . . . ? O8 C35 C34 C37 178.5(3) . . . . ? C36 C35 C34 C37 -2.0(7) . . . . ? N1 O5 C8 C7 1.0(4) . . . . ? N1 O5 C8 C9 179.3(3) . . . . ? C6 C7 C8 O5 -1.2(4) . . . . ? C10 C7 C8 O5 -179.0(4) . . . . ? C6 C7 C8 C9 -179.0(4) . . . . ? C10 C7 C8 C9 3.2(8) . . . . ? C35 C34 C37 C38 81.5(5) . . . . ? C33 C34 C37 C38 -98.1(5) . . . . ? C17 O6 N2 C15 0.1(4) . . . . ? C17 O6 N2 Ag2 175.1(2) . . . . ? O4 Ag2 N2 C15 30.9(4) . . . . ? O2 Ag2 N2 C15 -128.7(4) . . . . ? N1 Ag2 N2 C15 134.7(4) . . . . ? Ag1 Ag2 N2 C15 -50.5(4) . . . . ? O4 Ag2 N2 O6 -142.1(2) . . . . ? O2 Ag2 N2 O6 58.4(3) . . . . ? N1 Ag2 N2 O6 -38.2(3) . . . . ? Ag1 Ag2 N2 O6 136.5(2) . . . . ? O6 C17 C16 C15 1.1(4) . . . . ? C18 C17 C16 C15 -178.9(5) . . . . ? O6 C17 C16 C19 177.3(4) . . . . ? C18 C17 C16 C19 -2.6(8) . . . . ? C20 C21 C22 C20 0.0(7) . . . 2_556 ? C31 C29 C30 C31 0.2(6) 2_575 . . . ? C28 C29 C30 C31 179.8(3) . . . . ? C29 C31 C30 C29 -0.2(6) 2_575 . . . ? O8 N4 C33 C34 -1.4(4) . . . . ? Ag1 N4 C33 C34 155.5(3) . . . . ? O8 N4 C33 C32 178.5(4) . . . . ? Ag1 N4 C33 C32 -24.6(6) . . . . ? C35 C34 C33 N4 2.0(5) . . . . ? C37 C34 C33 N4 -178.3(4) . . . . ? C35 C34 C33 C32 -177.9(4) . . . . ? C37 C34 C33 C32 1.8(7) . . . . ? C26 C25 C28 C29 -97.3(5) . . . . ? C24 C25 C28 C29 81.6(5) . . . . ? C30 C29 C28 C25 86.3(4) . . . . ? C31 C29 C28 C25 -94.1(4) 2_575 . . . ? C17 C16 C19 C20 -77.4(5) . . . . ? C15 C16 C19 C20 98.0(5) . . . . ? C22 C20 C19 C16 113.4(4) 2_556 . . . ? C21 C20 C19 C16 -64.1(5) . . . . ? C11 C13 C12 C11 -0.6(7) 2_746 . . . ? O6 N2 C15 C16 0.6(4) . . . . ? Ag2 N2 C15 C16 -172.9(3) . . . . ? O6 N2 C15 C14 -180.0(4) . . . . ? Ag2 N2 C15 C14 6.6(6) . . . . ? C17 C16 C15 N2 -1.0(5) . . . . ? C19 C16 C15 N2 -177.2(4) . . . . ? C17 C16 C15 C14 179.6(4) . . . . ? C19 C16 C15 C14 3.3(7) . . . . ? Ag2 O2 C1 O1 21.2(7) . . . . ? Ag2 O2 C1 C2A -147.4(8) . . . . ? Ag2 O2 C1 C2 -164.6(4) . . . . ? Ag1 O1 C1 O2 3.2(7) . . . . ? Ag1 O1 C1 C2A 172.8(8) . . . . ? Ag1 O1 C1 C2 -170.7(5) . . . . ? C13 C12 C11 C13 0.6(6) . . . 2_746 ? C13 C12 C11 C10 178.3(4) . . . . ? C8 C7 C10 C11 98.6(5) . . . . ? C6 C7 C10 C11 -78.7(5) . . . . ? C12 C11 C10 C7 -77.4(5) . . . . ? C13 C11 C10 C7 100.2(4) 2_746 . . . ? C40 C39 C38 C40 -0.4(6) . . . 2_765 ? C40 C39 C38 C37 -177.6(4) . . . . ? C34 C37 C38 C39 81.4(5) . . . . ? C34 C37 C38 C40 -95.7(5) . . . 2_765 ? O3 C3 C4 F6 -176.3(11) . . . . ? O4 C3 C4 F6 4.2(12) . . . . ? O3 C3 C4 F5 -52.1(9) . . . . ? O4 C3 C4 F5 128.5(9) . . . . ? O3 C3 C4 F5A -11.2(9) . . . . ? O4 C3 C4 F5A 169.4(8) . . . . ? O3 C3 C4 F4 64.9(11) . . . . ? O4 C3 C4 F4 -114.6(10) . . . . ? O3 C3 C4 F4A 111.7(7) . . . . ? O4 C3 C4 F4A -67.7(8) . . . . ? O3 C3 C4 F6A -133.6(7) . . . . ? O4 C3 C4 F6A 47.0(7) . . . . ? O2 C1 C2 F3 -60.6(6) . . . . ? O1 C1 C2 F3 114.5(5) . . . . ? C2A C1 C2 F3 -179(3) . . . . ? O2 C1 C2 F1 175.7(7) . . . . ? O1 C1 C2 F1 -9.2(10) . . . . ? C2A C1 C2 F1 57(3) . . . . ? O2 C1 C2 F2 58.7(8) . . . . ? O1 C1 C2 F2 -126.2(6) . . . . ? C2A C1 C2 F2 -60(3) . . . . ? O2 C1 C2A F2A -11.3(16) . . . . ? O1 C1 C2A F2A 177.7(11) . . . . ? C2 C1 C2A F2A 57(3) . . . . ? O2 C1 C2A F3A -131.3(11) . . . . ? O1 C1 C2A F3A 57.8(14) . . . . ? C2 C1 C2A F3A -62(3) . . . . ? O2 C1 C2A F1A 108.2(13) . . . . ? O1 C1 C2A F1A -62.7(14) . . . . ? C2 C1 C2A F1A 177(4) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.101 _refine_diff_density_min -0.747 _refine_diff_density_rms 0.085 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.034 0.242 0.259 67 20 ' ' 2 -0.035 0.758 0.741 67 20 ' ' _platon_squeeze_details ; ; #===end data_Compound-6_New_k08adb03(CCDC-804682) _database_code_depnum_ccdc_archive 'CCDC 804682' #TrackingRef '- stevenson-rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C117.60 H144 Ag4 B4 F16 N12 O14.40' _chemical_formula_weight 2734.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P63/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z+1/2' '-y, x-y, z' '-x, -y, z+1/2' '-x+y, -x, z' 'y, -x+y, z+1/2' '-x, -y, -z' '-x+y, -x, -z-1/2' 'y, -x+y, -z' 'x, y, -z-1/2' 'x-y, x, -z' '-y, x-y, -z-1/2' _cell_length_a 14.3960(2) _cell_length_b 14.3960(2) _cell_length_c 35.3830(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6350.51(18) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 76331 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Colorless _exptl_crystal_colour Tabloid _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2802 _exptl_absorpt_coefficient_mu 0.694 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43636 _diffrn_reflns_av_R_equivalents 0.0926 _diffrn_reflns_av_sigmaI/netI 0.0678 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 3.70 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4919 _reflns_number_gt 2692 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski, Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick 1990)' _computing_structure_refinement 'SHELXL-97/2 (Sheldrick 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle 1995)' _computing_publication_material 'SHELXL-97/2 (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^)+(0.0258P)^2^+16.5869P] 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 4919 _refine_ls_number_parameters 269 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1332 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1268 _refine_ls_wR_factor_gt 0.1050 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.0000 0.0000 0.043238(17) 0.03685(17) Uani 1 3 d S . . Ag2 Ag 0.0000 0.0000 0.137166(18) 0.03854(18) Uani 1 3 d S . . F1 F -0.3333 0.3333 0.1007(3) 0.125(3) Uani 1 3 d S . . F2 F -0.2344(5) 0.3488(6) 0.1498(2) 0.175(3) Uani 1 1 d . . . F3 F 0.2992(2) 0.7356(2) 0.08736(9) 0.0589(8) Uani 1 1 d . . . F4 F 0.3333 0.6667 0.13973(13) 0.0428(12) Uani 1 3 d S . . O1 O -0.1494(2) 0.0890(3) 0.05718(10) 0.0448(9) Uani 1 1 d . . . O2 O 0.1711(3) 0.2404(3) 0.13550(10) 0.0445(9) Uani 1 1 d . . . O3 O 0.3014(18) 0.2342(14) 0.2500 0.189(6) Uani 0.80 2 d SP . . N1 N -0.0415(3) 0.1279(3) 0.04716(12) 0.0394(10) Uani 1 1 d . . . N2 N 0.0597(3) 0.1751(3) 0.14114(12) 0.0432(10) Uani 1 1 d . . . C1 C -0.1603(4) 0.1753(4) 0.06688(15) 0.0437(13) Uani 1 1 d . . . C2 C -0.0648(4) 0.2666(4) 0.06353(13) 0.0359(11) Uani 1 1 d . . . C3 C 0.0074(4) 0.2331(4) 0.05089(13) 0.0343(11) Uani 1 1 d . . . C4 C -0.2706(4) 0.1492(5) 0.07724(18) 0.0619(17) Uani 1 1 d . . . H4A H -0.2717 0.2157 0.0820 0.093 Uiso 1 1 calc R . . H4B H -0.2931 0.1048 0.1001 0.093 Uiso 1 1 calc R . . H4C H -0.3197 0.1098 0.0565 0.093 Uiso 1 1 calc R . . C5 C 0.1234(4) 0.3025(4) 0.04161(14) 0.0439(13) Uani 1 1 d . . . H5A H 0.1554 0.2574 0.0369 0.066 Uiso 1 1 calc R . . H5B H 0.1602 0.3508 0.0628 0.066 Uiso 1 1 calc R . . H5C H 0.1307 0.3448 0.0190 0.066 Uiso 1 1 calc R . . C6 C -0.0388(4) 0.3800(4) 0.07014(13) 0.0411(12) Uani 1 1 d . . . H6A H 0.0257 0.4166 0.0864 0.049 Uiso 1 1 calc R . . H6B H -0.0990 0.3795 0.0838 0.049 Uiso 1 1 calc R . . C7 C -0.0185(4) 0.4425(4) 0.03367(13) 0.0351(11) Uani 1 1 d . . . C8 C 0.0762(4) 0.5372(4) 0.02776(14) 0.0416(13) Uani 1 1 d . . . H8 H 0.1299 0.5632 0.0468 0.050 Uiso 1 1 calc R . . C9 C -0.0944(4) 0.4056(4) 0.00504(13) 0.0387(12) Uani 1 1 d . . . H9 H -0.1598 0.3399 0.0082 0.046 Uiso 1 1 calc R . . C10 C 0.0239(4) 0.2377(4) 0.15275(13) 0.0355(11) Uani 1 1 d . . . C11 C 0.1097(4) 0.3458(4) 0.15503(13) 0.0351(11) Uani 1 1 d . . . C12 C 0.1979(4) 0.3426(4) 0.14464(14) 0.0413(12) Uani 1 1 d . . . C13 C -0.0908(4) 0.1943(4) 0.16288(16) 0.0506(14) Uani 1 1 d . . . H13A H -0.1333 0.1208 0.1533 0.076 Uiso 1 1 calc R . . H13B H -0.1167 0.2393 0.1516 0.076 Uiso 1 1 calc R . . H13C H -0.0979 0.1941 0.1904 0.076 Uiso 1 1 calc R . . C14 C 0.3140(4) 0.4221(4) 0.14156(18) 0.0568(15) Uani 1 1 d . . . H14A H 0.3272 0.4921 0.1505 0.085 Uiso 1 1 calc R . . H14B H 0.3365 0.4280 0.1151 0.085 Uiso 1 1 calc R . . H14C H 0.3549 0.3987 0.1570 0.085 Uiso 1 1 calc R . . C15 C 0.1021(4) 0.4420(4) 0.16767(14) 0.0423(12) Uani 1 1 d . . . H15A H 0.0355 0.4365 0.1574 0.051 Uiso 1 1 calc R . . H15B H 0.1637 0.5080 0.1573 0.051 Uiso 1 1 calc R . . C16 C 0.1016(4) 0.4505(3) 0.21047(14) 0.0372(12) Uani 1 1 d . . . C17 C 0.0071(4) 0.4123(4) 0.23046(14) 0.0476(13) Uani 1 1 d . . . H17 H -0.0588 0.3857 0.2172 0.057 Uiso 1 1 calc R . . C18 C 0.1959(4) 0.4927(4) 0.23055(15) 0.0525(14) Uani 1 1 d . . . H18 H 0.2621 0.5223 0.2173 0.063 Uiso 1 1 calc R . . C19 C 0.101(2) 0.161(2) 0.2500 0.214(13) Uani 0.80 2 d SPD . . H19A H 0.0502 0.1868 0.2500 0.321 Uiso 0.80 2 calc SPR . . H19B H 0.0900 0.1168 0.2726 0.321 Uiso 0.40 1 calc PR . . H19C H 0.0900 0.1168 0.2274 0.321 Uiso 0.40 1 calc PR . . C20 C 0.215(2) 0.2551(18) 0.2500 0.218(15) Uani 0.80 2 d SPD . . H20A H 0.2227 0.2993 0.2275 0.262 Uiso 0.40 1 calc PR . . H20B H 0.2227 0.2993 0.2725 0.262 Uiso 0.40 1 calc PR . . C22 C 0.401(2) 0.319(2) 0.2500 0.30(2) Uani 0.80 2 d SPD . . H22A H 0.4098 0.3637 0.2726 0.355 Uiso 0.40 1 calc PR . . H22B H 0.4098 0.3637 0.2274 0.355 Uiso 0.40 1 calc PR . . C23 C 0.490(3) 0.2914(18) 0.2500 0.216(13) Uani 0.80 2 d SPD . . H23A H 0.5603 0.3575 0.2500 0.323 Uiso 0.80 2 calc SPR . . H23B H 0.4841 0.2493 0.2274 0.323 Uiso 0.40 1 calc PR . . H23C H 0.4841 0.2493 0.2726 0.323 Uiso 0.40 1 calc PR . . B1 B -0.3333 0.3333 0.1393(8) 0.117(7) Uani 1 3 d S . . B2 B 0.3333 0.6667 0.0996(3) 0.038(2) Uani 1 3 d S . . 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 Ag1 0.0341(2) 0.0341(2) 0.0423(4) 0.000 0.000 0.01707(11) Ag2 0.0340(2) 0.0340(2) 0.0476(4) 0.000 0.000 0.01702(11) F1 0.108(4) 0.108(4) 0.158(9) 0.000 0.000 0.054(2) F2 0.158(6) 0.213(6) 0.188(6) -0.044(5) -0.067(5) 0.119(5) F3 0.067(2) 0.062(2) 0.062(2) 0.0222(17) 0.0167(17) 0.0428(17) F4 0.0425(18) 0.0425(18) 0.043(3) 0.000 0.000 0.0213(9) O1 0.0297(19) 0.0346(19) 0.066(2) 0.0073(17) 0.0021(17) 0.0134(16) O2 0.041(2) 0.034(2) 0.059(2) 0.0035(17) 0.0050(17) 0.0186(17) O3 0.28(2) 0.172(14) 0.146(12) 0.000 0.000 0.136(16) N1 0.032(2) 0.033(2) 0.055(3) 0.007(2) 0.000(2) 0.0168(19) N2 0.043(3) 0.034(2) 0.050(3) 0.000(2) 0.000(2) 0.017(2) C1 0.049(3) 0.046(3) 0.046(3) 0.009(3) 0.001(3) 0.031(3) C2 0.040(3) 0.035(3) 0.037(3) 0.006(2) -0.003(2) 0.022(3) C3 0.034(3) 0.030(3) 0.038(3) 0.005(2) -0.003(2) 0.016(2) C4 0.040(3) 0.061(4) 0.089(5) 0.009(4) 0.004(3) 0.029(3) C5 0.045(3) 0.036(3) 0.051(3) 0.003(2) 0.001(3) 0.020(2) C6 0.055(3) 0.041(3) 0.037(3) 0.002(2) -0.002(2) 0.031(3) C7 0.050(3) 0.029(3) 0.037(3) -0.004(2) -0.004(2) 0.027(3) C8 0.048(3) 0.041(3) 0.043(3) -0.006(2) -0.017(2) 0.027(3) C9 0.044(3) 0.033(3) 0.037(3) -0.002(2) -0.009(2) 0.017(2) C10 0.040(3) 0.034(3) 0.035(3) 0.003(2) -0.001(2) 0.021(2) C11 0.047(3) 0.032(3) 0.030(3) 0.004(2) 0.000(2) 0.022(2) C12 0.051(3) 0.033(3) 0.042(3) 0.006(2) 0.003(3) 0.023(3) C13 0.048(3) 0.048(3) 0.056(3) -0.002(3) 0.001(3) 0.024(3) C14 0.042(3) 0.039(3) 0.090(5) 0.008(3) 0.005(3) 0.020(3) C15 0.050(3) 0.029(3) 0.045(3) 0.009(2) 0.005(2) 0.018(2) C16 0.049(3) 0.020(2) 0.042(3) 0.003(2) 0.002(2) 0.017(2) C17 0.049(3) 0.049(3) 0.048(3) -0.002(3) -0.008(3) 0.028(3) C18 0.047(3) 0.046(3) 0.052(3) 0.001(3) 0.005(3) 0.014(3) C19 0.19(2) 0.35(4) 0.088(14) 0.000 0.000 0.13(3) C20 0.38(4) 0.24(3) 0.21(3) 0.000 0.000 0.29(3) C22 0.17(3) 0.10(2) 0.47(6) 0.000 0.000 -0.04(2) C23 0.24(3) 0.114(18) 0.30(3) 0.000 0.000 0.09(2) B1 0.114(11) 0.114(11) 0.12(2) 0.000 0.000 0.057(6) B2 0.036(4) 0.036(4) 0.043(6) 0.000 0.000 0.0180(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.207(4) 5 ? Ag1 N1 2.207(4) 3 ? Ag1 N1 2.207(4) . ? Ag1 Ag1 3.0597(12) 7 ? Ag1 Ag2 3.3234(9) . ? Ag2 N2 2.224(4) 3 ? Ag2 N2 2.224(4) . ? Ag2 N2 2.224(4) 5 ? F1 B1 1.37(2) . ? F2 B1 1.378(8) . ? F3 B2 1.380(4) . ? F4 B2 1.420(11) . ? O1 C1 1.371(6) . ? O1 N1 1.407(5) . ? O2 C12 1.362(5) . ? O2 N2 1.411(5) . ? O3 C22 1.35(2) . ? O3 C20 1.42(2) . ? N1 C3 1.319(6) . ? N2 C10 1.309(6) . ? C1 C2 1.351(7) . ? C1 C4 1.483(7) . ? C2 C3 1.418(6) . ? C2 C6 1.500(6) . ? C3 C5 1.492(6) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.516(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.380(7) . ? C7 C9 1.386(6) . ? C8 C9 1.371(6) 7_565 ? C8 H8 0.9500 . ? C9 C8 1.371(6) 7_565 ? C9 H9 0.9500 . ? C10 C11 1.425(6) . ? C10 C13 1.488(7) . ? C11 C12 1.343(7) . ? C11 C15 1.510(6) . ? C12 C14 1.484(7) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.520(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C18 1.375(7) . ? C16 C17 1.381(7) . ? C17 C17 1.382(10) 10_556 ? C17 H17 0.9500 . ? C18 C18 1.377(10) 10_556 ? C18 H18 0.9500 . ? C19 C20 1.516(10) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C22 C23 1.527(10) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? B1 F2 1.377(8) 5_455 ? B1 F2 1.377(8) 3_565 ? B2 F3 1.380(4) 3_665 ? B2 F3 1.380(4) 5_565 ? 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 N1 Ag1 N1 119.61(2) 5 3 ? N1 Ag1 N1 119.61(2) 5 . ? N1 Ag1 N1 119.61(2) 3 . ? N1 Ag1 Ag1 93.60(11) 5 7 ? N1 Ag1 Ag1 93.60(11) 3 7 ? N1 Ag1 Ag1 93.60(11) . 7 ? N1 Ag1 Ag2 86.40(11) 5 . ? N1 Ag1 Ag2 86.40(11) 3 . ? N1 Ag1 Ag2 86.40(11) . . ? Ag1 Ag1 Ag2 180.0 7 . ? N2 Ag2 N2 119.60(2) 3 . ? N2 Ag2 N2 119.60(2) 3 5 ? N2 Ag2 N2 119.60(2) . 5 ? N2 Ag2 Ag1 93.63(11) 3 . ? N2 Ag2 Ag1 93.63(11) . . ? N2 Ag2 Ag1 93.63(11) 5 . ? C1 O1 N1 107.8(3) . . ? C12 O2 N2 107.4(3) . . ? C22 O3 C20 117(2) . . ? C3 N1 O1 106.3(4) . . ? C3 N1 Ag1 138.8(3) . . ? O1 N1 Ag1 112.9(2) . . ? C10 N2 O2 107.1(4) . . ? C10 N2 Ag2 137.7(3) . . ? O2 N2 Ag2 114.4(3) . . ? C2 C1 O1 109.7(4) . . ? C2 C1 C4 135.1(5) . . ? O1 C1 C4 115.2(5) . . ? C1 C2 C3 105.0(4) . . ? C1 C2 C6 128.6(5) . . ? C3 C2 C6 126.3(4) . . ? N1 C3 C2 111.1(4) . . ? N1 C3 C5 121.5(4) . . ? C2 C3 C5 127.3(4) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C2 C6 C7 112.5(4) . . ? C2 C6 H6A 109.1 . . ? C7 C6 H6A 109.1 . . ? C2 C6 H6B 109.1 . . ? C7 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? C8 C7 C9 117.9(4) . . ? C8 C7 C6 121.1(4) . . ? C9 C7 C6 121.0(4) . . ? C9 C8 C7 121.3(4) 7_565 . ? C9 C8 H8 119.4 7_565 . ? C7 C8 H8 119.4 . . ? C8 C9 C7 120.8(4) 7_565 . ? C8 C9 H9 119.6 7_565 . ? C7 C9 H9 119.6 . . ? N2 C10 C11 110.2(4) . . ? N2 C10 C13 121.5(4) . . ? C11 C10 C13 128.3(4) . . ? C12 C11 C10 105.4(4) . . ? C12 C11 C15 128.0(5) . . ? C10 C11 C15 126.6(4) . . ? C11 C12 O2 109.9(4) . . ? C11 C12 C14 135.5(5) . . ? O2 C12 C14 114.6(4) . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 112.0(4) . . ? C11 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? C11 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C18 C16 C17 118.0(5) . . ? C18 C16 C15 120.5(5) . . ? C17 C16 C15 121.4(5) . . ? C16 C17 C17 120.8(3) . 10_556 ? C16 C17 H17 119.6 . . ? C17 C17 H17 119.6 10_556 . ? C16 C18 C18 121.1(3) . 10_556 ? C16 C18 H18 119.4 . . ? C18 C18 H18 119.4 10_556 . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O3 C20 C19 118.4(18) . . ? O3 C20 H20A 107.7 . . ? C19 C20 H20A 107.7 . . ? O3 C20 H20B 107.7 . . ? C19 C20 H20B 107.7 . . ? H20A C20 H20B 107.1 . . ? O3 C22 C23 114(3) . . ? O3 C22 H22A 108.6 . . ? C23 C22 H22A 108.6 . . ? O3 C22 H22B 108.6 . . ? C23 C22 H22B 108.6 . . ? H22A C22 H22B 107.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? F1 B1 F2 105.6(12) . . ? F1 B1 F2 105.6(12) . 5_455 ? F2 B1 F2 113.0(10) . 5_455 ? F1 B1 F2 105.6(12) . 3_565 ? F2 B1 F2 113.0(10) . 3_565 ? F2 B1 F2 113.0(10) 5_455 3_565 ? F3 B2 F3 110.6(4) . 3_665 ? F3 B2 F3 110.6(4) . 5_565 ? F3 B2 F3 110.6(4) 3_665 5_565 ? F3 B2 F4 108.3(4) . . ? F3 B2 F4 108.3(4) 3_665 . ? F3 B2 F4 108.3(4) 5_565 . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.564 _refine_diff_density_min -0.556 _refine_diff_density_rms 0.078 #===end data_Compound-7-h08adb08 _database_code_depnum_ccdc_archive 'CCDC 804683' #TrackingRef '- stevenson-rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H50 Ag F6 N5 O5 P' _chemical_formula_weight 993.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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 13.5620(1) _cell_length_b 14.2000(1) _cell_length_c 14.2460(2) _cell_angle_alpha 103.616(1) _cell_angle_beta 113.747(1) _cell_angle_gamma 103.917(1) _cell_volume 2260.62(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 58879 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1022 _exptl_absorpt_coefficient_mu 0.556 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38548 _diffrn_reflns_av_R_equivalents 0.0734 _diffrn_reflns_av_sigmaI/netI 0.0705 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.67 _diffrn_reflns_theta_max 27.46 _reflns_number_total 10256 _reflns_number_gt 7231 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (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^)+(0.0469P)^2^+0.0000P] 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 0.0047(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10256 _refine_ls_number_parameters 633 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0770 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.0944 _refine_ls_wR_factor_gt 0.0833 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 Ag1 Ag 0.962142(17) 0.264587(14) 0.172180(15) 0.03621(9) Uani 1 1 d . . . P1 P 1.15510(6) 0.87060(5) 0.40355(6) 0.04133(18) Uani 1 1 d . . . F1 F 1.0211(4) 0.8310(6) 0.3514(5) 0.107(2) Uani 0.60 1 d P A 1 F2 F 1.1194(10) 0.7740(8) 0.4327(9) 0.110(4) Uani 0.60 1 d P A 1 F3 F 1.1425(6) 0.7952(5) 0.2938(4) 0.071(2) Uani 0.60 1 d P A 1 F4 F 1.1660(10) 0.9627(7) 0.3600(10) 0.107(4) Uani 0.60 1 d P A 1 F5 F 1.1718(6) 0.9413(4) 0.5136(4) 0.0793(17) Uani 0.60 1 d P A 1 F6 F 1.2909(4) 0.9039(5) 0.4547(5) 0.0966(15) Uani 0.60 1 d P A 1 F1A F 1.0403(9) 0.8360(7) 0.2957(8) 0.145(4) Uani 0.40 1 d P A 2 F2A F 1.1521(15) 0.7815(14) 0.4512(13) 0.096(5) Uani 0.40 1 d P A 2 F3A F 1.1971(14) 0.8059(10) 0.3405(12) 0.152(7) Uani 0.40 1 d P A 2 F4A F 1.2027(15) 0.9671(8) 0.3802(13) 0.110(6) Uani 0.40 1 d P A 2 F5A F 1.1041(10) 0.9409(7) 0.4659(9) 0.102(3) Uani 0.40 1 d P A 2 F6A F 1.2681(10) 0.9152(9) 0.5193(9) 0.168(5) Uani 0.40 1 d P A 2 O1 O 1.03805(14) 0.35175(11) 0.01259(13) 0.0318(4) Uani 1 1 d . . . O2 O 1.77952(15) 0.66415(12) 0.62791(14) 0.0385(4) Uani 1 1 d . . . O3 O 0.90824(15) 0.02499(12) 0.09732(14) 0.0369(4) Uani 1 1 d . . . O4 O 0.10894(16) -0.43661(13) -0.28218(16) 0.0475(5) Uani 1 1 d . . . O5 O 0.4128(2) 0.37437(17) -0.0124(2) 0.0695(6) Uani 1 1 d . . . N1 N 1.05489(17) 0.38270(15) 0.12148(16) 0.0329(5) Uani 1 1 d . . . N2 N 1.89280(17) 0.73435(15) 0.66568(16) 0.0352(5) Uani 1 1 d . . . N3 N 0.87844(18) 0.09794(14) 0.05089(17) 0.0346(5) Uani 1 1 d . . . N4 N 0.14731(18) -0.32624(15) -0.23992(17) 0.0387(5) Uani 1 1 d . . . N5 N 0.3048(2) 0.29127(19) -0.1001(2) 0.0543(7) Uani 1 1 d . . . C1 C 1.1633(2) 0.53900(19) 0.2898(2) 0.0408(6) Uani 1 1 d . . . H1A H 1.1161 0.4977 0.3138 0.061 Uiso 1 1 calc R . . H1 H 1.1541 0.6064 0.2984 0.061 Uiso 1 1 calc R . . H1C H 1.2453 0.5510 0.3350 0.061 Uiso 1 1 calc R . . C2 C 1.1246(2) 0.48130(17) 0.17183(19) 0.0303(5) Uani 1 1 d . . . C3 C 1.1552(2) 0.51935(18) 0.09885(19) 0.0296(5) Uani 1 1 d . . . C4 C 1.1007(2) 0.43629(18) 0.00315(19) 0.0299(5) Uani 1 1 d . . . C5 C 1.0972(2) 0.4174(2) -0.1054(2) 0.0401(6) Uani 1 1 d . . . H5A H 1.1156 0.4838 -0.1161 0.060 Uiso 1 1 calc R . . H5B H 1.0192 0.3690 -0.1646 0.060 Uiso 1 1 calc R . . H5C H 1.1543 0.3869 -0.1071 0.060 Uiso 1 1 calc R . . C6 C 1.2264(2) 0.63081(18) 0.1256(2) 0.0347(6) Uani 1 1 d . . . H6A H 1.1943 0.6772 0.1569 0.042 Uiso 1 1 calc R . . H6B H 1.2174 0.6389 0.0558 0.042 Uiso 1 1 calc R . . C7 C 1.3556(2) 0.66771(18) 0.20598(19) 0.0311(5) Uani 1 1 d . . . C8 C 1.4221(2) 0.61157(19) 0.1892(2) 0.0348(6) Uani 1 1 d . . . H8 H 1.3854 0.5456 0.1300 0.042 Uiso 1 1 calc R . . C9 C 1.5409(2) 0.6509(2) 0.2576(2) 0.0381(6) Uani 1 1 d . . . H9 H 1.5850 0.6118 0.2445 0.046 Uiso 1 1 calc R . . C10 C 1.5974(2) 0.74723(19) 0.3460(2) 0.0352(6) Uani 1 1 d . . . C11 C 1.5310(2) 0.80205(19) 0.3634(2) 0.0379(6) Uani 1 1 d . . . H11 H 1.5676 0.8675 0.4233 0.046 Uiso 1 1 calc R . . C12 C 1.4115(2) 0.76292(19) 0.2947(2) 0.0353(6) Uani 1 1 d . . . H12 H 1.3673 0.8017 0.3085 0.042 Uiso 1 1 calc R . . C13 C 1.7273(2) 0.7892(2) 0.4218(2) 0.0405(6) Uani 1 1 d . . . H13A H 1.7647 0.7707 0.3771 0.049 Uiso 1 1 calc R . . H13B H 1.7559 0.8664 0.4542 0.049 Uiso 1 1 calc R . . C14 C 1.7650(2) 0.74975(18) 0.51409(19) 0.0313(5) Uani 1 1 d . . . C15 C 1.7048(2) 0.67607(18) 0.5372(2) 0.0330(5) Uani 1 1 d . . . C16 C 1.5814(2) 0.6078(2) 0.4904(2) 0.0449(7) Uani 1 1 d . . . H16A H 1.5307 0.6403 0.4514 0.067 Uiso 1 1 calc R . . H16B H 1.5670 0.5984 0.5504 0.067 Uiso 1 1 calc R . . H16C H 1.5649 0.5395 0.4386 0.067 Uiso 1 1 calc R . . C17 C 1.8822(2) 0.78450(18) 0.59844(19) 0.0304(5) Uani 1 1 d . . . C18 C 1.9845(2) 0.8660(2) 0.6129(2) 0.0428(6) Uani 1 1 d . . . H18A H 2.0536 0.8771 0.6803 0.064 Uiso 1 1 calc R . . H18B H 1.9712 0.9315 0.6188 0.064 Uiso 1 1 calc R . . H18C H 1.9962 0.8434 0.5490 0.064 Uiso 1 1 calc R . . C19 C 0.7885(3) 0.1077(2) -0.1300(2) 0.0460(7) Uani 1 1 d . . . H19A H 0.8068 0.1799 -0.0852 0.069 Uiso 1 1 calc R . . H19B H 0.7042 0.0728 -0.1788 0.069 Uiso 1 1 calc R . . H19C H 0.8276 0.1082 -0.1747 0.069 Uiso 1 1 calc R . . C20 C 0.8290(2) 0.05073(18) -0.0563(2) 0.0315(5) Uani 1 1 d . . . C21 C 0.8230(2) -0.05418(18) -0.0857(2) 0.0347(6) Uani 1 1 d . . . C22 C 0.8731(2) -0.06527(18) 0.0119(2) 0.0368(6) Uani 1 1 d . . . C23 C 0.8994(3) -0.1516(2) 0.0444(3) 0.0566(8) Uani 1 1 d . . . H23A H 0.9657 -0.1226 0.1193 0.085 Uiso 1 1 calc R . . H23B H 0.9183 -0.1919 -0.0073 0.085 Uiso 1 1 calc R . . H23C H 0.8314 -0.1975 0.0427 0.085 Uiso 1 1 calc R . . C24 C 0.7738(2) -0.1334(2) -0.2002(2) 0.0490(7) Uani 1 1 d . . . H24A H 0.8131 -0.1838 -0.1955 0.059 Uiso 1 1 calc R . . H24B H 0.7912 -0.0969 -0.2463 0.059 Uiso 1 1 calc R . . C25 C 0.6431(2) -0.1934(2) -0.2567(2) 0.0416(6) Uani 1 1 d . . . C26 C 0.5972(2) -0.2746(2) -0.2294(2) 0.0436(6) Uani 1 1 d . . . H26 H 0.6480 -0.2919 -0.1734 0.052 Uiso 1 1 calc R . . C27 C 0.4787(2) -0.3306(2) -0.2827(2) 0.0428(6) Uani 1 1 d . . . H27 H 0.4495 -0.3860 -0.2627 0.051 Uiso 1 1 calc R . . C28 C 0.4014(2) -0.3074(2) -0.3650(2) 0.0412(6) Uani 1 1 d . . . C29 C 0.4473(3) -0.2256(2) -0.3905(2) 0.0491(7) Uani 1 1 d . . . H29 H 0.3967 -0.2068 -0.4451 0.059 Uiso 1 1 calc R . . C30 C 0.5663(3) -0.1702(2) -0.3376(2) 0.0481(7) Uani 1 1 d . . . H30 H 0.5957 -0.1149 -0.3576 0.058 Uiso 1 1 calc R . . C31 C 0.2717(2) -0.3716(2) -0.4278(2) 0.0460(7) Uani 1 1 d . . . H31A H 0.2333 -0.3415 -0.4815 0.055 Uiso 1 1 calc R . . H31B H 0.2587 -0.4436 -0.4706 0.055 Uiso 1 1 calc R . . C32 C 0.2133(2) -0.3781(2) -0.3579(2) 0.0374(6) Uani 1 1 d . . . C33 C 0.2081(2) -0.29348(19) -0.2856(2) 0.0344(6) Uani 1 1 d . . . C34 C 0.2600(2) -0.1801(2) -0.2614(2) 0.0446(7) Uani 1 1 d . . . H34A H 0.2441 -0.1402 -0.2068 0.067 Uiso 1 1 calc R . . H34B H 0.2259 -0.1667 -0.3296 0.067 Uiso 1 1 calc R . . H34C H 0.3442 -0.1586 -0.2320 0.067 Uiso 1 1 calc R . . C35 C 0.1501(2) -0.4641(2) -0.3531(2) 0.0465(7) Uani 1 1 d . . . C36 C 0.1167(3) -0.5788(2) -0.4069(3) 0.0713(10) Uani 1 1 d . . . H36A H 0.1471 -0.5913 -0.4586 0.107 Uiso 1 1 calc R . . H36B H 0.0318 -0.6134 -0.4472 0.107 Uiso 1 1 calc R . . H36C H 0.1494 -0.6072 -0.3503 0.107 Uiso 1 1 calc R . . C37 C 0.2388(3) 0.1125(3) -0.2208(3) 0.0763(10) Uani 1 1 d . . . H37A H 0.2214 0.0614 -0.1884 0.114 Uiso 1 1 calc R . . H37B H 0.2635 0.0845 -0.2735 0.114 Uiso 1 1 calc R . . H37C H 0.1691 0.1267 -0.2593 0.114 Uiso 1 1 calc R . . C38 C 0.3339(3) 0.2115(2) -0.1315(3) 0.0567(8) Uani 1 1 d . . . C39 C 0.4531(3) 0.2356(2) -0.0714(3) 0.0516(8) Uani 1 1 d . . . C40 C 0.4970(3) 0.3369(2) 0.0007(3) 0.0530(8) Uani 1 1 d . . . C41 C 0.6166(3) 0.4098(3) 0.0841(3) 0.0674(9) Uani 1 1 d . . . H41A H 0.6197 0.4387 0.1553 0.101 Uiso 1 1 calc R . . H41B H 0.6400 0.4668 0.0605 0.101 Uiso 1 1 calc R . . H41C H 0.6696 0.3723 0.0919 0.101 Uiso 1 1 calc R . . C42 C 0.5182(3) 0.1676(2) -0.0854(3) 0.0638(9) Uani 1 1 d . . . H42A H 0.6018 0.2125 -0.0479 0.077 Uiso 1 1 calc R . . H42B H 0.4924 0.1361 -0.1653 0.077 Uiso 1 1 calc R . . C43 C 0.5058(2) 0.08021(19) -0.0420(2) 0.0378(6) Uani 1 1 d . . . C44 C 0.4530(2) 0.0727(2) 0.0229(2) 0.0412(6) Uani 1 1 d . . . H44 H 0.4202 0.1222 0.0393 0.049 Uiso 1 1 calc R . . C45 C 0.5522(2) 0.0060(2) -0.0640(2) 0.0407(6) Uani 1 1 d . . . H45 H 0.5885 0.0096 -0.1085 0.049 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 Ag1 0.04769(15) 0.03016(12) 0.03447(13) 0.01106(9) 0.02309(10) 0.01602(9) P1 0.0512(5) 0.0371(4) 0.0398(4) 0.0154(3) 0.0246(4) 0.0179(3) F1 0.054(3) 0.179(6) 0.105(4) 0.066(5) 0.043(3) 0.052(3) F2 0.199(9) 0.044(3) 0.119(8) 0.034(4) 0.119(7) 0.016(4) F3 0.116(5) 0.040(2) 0.050(2) 0.0045(16) 0.053(2) 0.010(3) F4 0.227(9) 0.098(6) 0.117(6) 0.088(5) 0.130(6) 0.124(7) F5 0.149(6) 0.045(2) 0.065(3) 0.016(2) 0.075(4) 0.032(3) F6 0.051(2) 0.116(4) 0.088(4) 0.026(4) 0.022(3) 0.010(2) F1A 0.109(7) 0.117(6) 0.088(6) 0.024(6) -0.041(5) 0.026(6) F2A 0.155(9) 0.075(8) 0.061(5) 0.049(5) 0.031(5) 0.062(7) F3A 0.245(17) 0.104(10) 0.277(18) 0.098(12) 0.234(16) 0.122(12) F4A 0.209(12) 0.031(5) 0.103(8) 0.015(4) 0.118(9) 0.000(6) F5A 0.170(10) 0.083(5) 0.159(10) 0.073(7) 0.137(9) 0.088(7) F6A 0.135(9) 0.154(9) 0.104(7) 0.062(7) -0.029(6) 0.021(7) O1 0.0375(10) 0.0269(8) 0.0289(9) 0.0080(7) 0.0164(8) 0.0108(8) O2 0.0453(11) 0.0350(9) 0.0389(10) 0.0153(8) 0.0233(9) 0.0142(9) O3 0.0442(10) 0.0320(9) 0.0384(10) 0.0168(8) 0.0204(9) 0.0165(8) O4 0.0548(12) 0.0335(10) 0.0645(13) 0.0129(9) 0.0399(11) 0.0190(9) O5 0.0793(17) 0.0574(14) 0.0985(18) 0.0397(14) 0.0555(15) 0.0359(14) N1 0.0406(12) 0.0294(11) 0.0271(11) 0.0085(9) 0.0166(10) 0.0123(10) N2 0.0352(12) 0.0398(12) 0.0329(12) 0.0142(10) 0.0174(10) 0.0158(10) N3 0.0452(13) 0.0251(10) 0.0369(12) 0.0134(9) 0.0215(11) 0.0142(10) N4 0.0448(13) 0.0329(11) 0.0426(13) 0.0096(10) 0.0248(11) 0.0195(10) N5 0.0448(15) 0.0456(14) 0.0861(19) 0.0370(14) 0.0335(15) 0.0236(13) C1 0.0490(17) 0.0368(14) 0.0295(14) 0.0099(12) 0.0153(13) 0.0141(13) C2 0.0315(14) 0.0274(12) 0.0290(13) 0.0099(11) 0.0115(11) 0.0128(11) C3 0.0286(13) 0.0301(12) 0.0308(13) 0.0133(11) 0.0125(11) 0.0135(11) C4 0.0277(13) 0.0323(13) 0.0329(14) 0.0155(11) 0.0137(11) 0.0151(11) C5 0.0437(16) 0.0421(15) 0.0336(14) 0.0136(12) 0.0190(13) 0.0150(13) C6 0.0362(15) 0.0315(13) 0.0335(14) 0.0151(11) 0.0133(12) 0.0116(11) C7 0.0315(14) 0.0283(12) 0.0287(13) 0.0120(11) 0.0119(11) 0.0073(11) C8 0.0362(15) 0.0324(13) 0.0278(13) 0.0061(11) 0.0133(12) 0.0097(12) C9 0.0364(16) 0.0430(15) 0.0377(15) 0.0159(13) 0.0188(13) 0.0171(13) C10 0.0332(15) 0.0350(14) 0.0335(14) 0.0160(12) 0.0134(12) 0.0084(12) C11 0.0400(16) 0.0309(13) 0.0298(14) 0.0078(11) 0.0112(12) 0.0063(12) C12 0.0390(16) 0.0321(13) 0.0351(14) 0.0129(12) 0.0179(13) 0.0137(12) C13 0.0325(15) 0.0407(15) 0.0380(15) 0.0166(12) 0.0108(12) 0.0071(12) C14 0.0331(14) 0.0284(12) 0.0303(13) 0.0085(11) 0.0155(12) 0.0106(11) C15 0.0372(14) 0.0307(13) 0.0316(14) 0.0084(11) 0.0192(12) 0.0121(11) C16 0.0463(17) 0.0356(15) 0.0454(17) 0.0115(13) 0.0248(14) 0.0032(13) C17 0.0344(14) 0.0313(12) 0.0271(13) 0.0087(11) 0.0158(11) 0.0155(11) C18 0.0325(15) 0.0480(16) 0.0424(16) 0.0169(13) 0.0155(13) 0.0115(13) C19 0.0518(18) 0.0465(16) 0.0425(16) 0.0219(14) 0.0234(14) 0.0168(14) C20 0.0324(14) 0.0314(13) 0.0337(14) 0.0114(11) 0.0194(12) 0.0116(11) C21 0.0322(14) 0.0301(13) 0.0414(15) 0.0063(11) 0.0230(12) 0.0090(11) C22 0.0345(15) 0.0266(13) 0.0556(17) 0.0144(12) 0.0273(14) 0.0126(11) C23 0.058(2) 0.0393(16) 0.089(2) 0.0312(17) 0.0423(19) 0.0260(15) C24 0.0487(18) 0.0415(15) 0.0500(17) -0.0011(13) 0.0331(15) 0.0083(14) C25 0.0455(17) 0.0361(14) 0.0395(16) 0.0002(12) 0.0279(14) 0.0101(13) C26 0.0414(17) 0.0468(16) 0.0383(15) 0.0092(13) 0.0204(14) 0.0148(14) C27 0.0432(17) 0.0472(16) 0.0397(16) 0.0155(13) 0.0244(14) 0.0129(14) C28 0.0383(16) 0.0493(16) 0.0334(15) 0.0054(13) 0.0212(13) 0.0157(13) C29 0.056(2) 0.0539(18) 0.0412(16) 0.0157(14) 0.0258(15) 0.0252(16) C30 0.059(2) 0.0421(16) 0.0467(17) 0.0137(14) 0.0328(16) 0.0157(15) C31 0.0414(16) 0.0555(17) 0.0339(15) 0.0054(13) 0.0186(13) 0.0173(14) C32 0.0322(14) 0.0400(15) 0.0300(14) 0.0028(11) 0.0121(12) 0.0130(12) C33 0.0268(13) 0.0400(14) 0.0339(14) 0.0118(12) 0.0126(12) 0.0144(11) C34 0.0450(17) 0.0420(15) 0.0512(17) 0.0163(13) 0.0259(14) 0.0199(13) C35 0.0438(17) 0.0407(16) 0.0469(17) 0.0027(13) 0.0229(14) 0.0146(14) C36 0.070(2) 0.0387(17) 0.097(3) -0.0001(17) 0.050(2) 0.0164(16) C37 0.088(3) 0.061(2) 0.083(3) 0.037(2) 0.046(2) 0.018(2) C38 0.068(2) 0.0504(19) 0.074(2) 0.0413(18) 0.0440(19) 0.0234(17) C39 0.069(2) 0.0572(19) 0.071(2) 0.0461(18) 0.0521(19) 0.0383(17) C40 0.069(2) 0.0521(19) 0.068(2) 0.0373(17) 0.0458(19) 0.0328(17) C41 0.070(2) 0.083(2) 0.057(2) 0.037(2) 0.0321(19) 0.028(2) C42 0.094(3) 0.069(2) 0.094(3) 0.060(2) 0.074(2) 0.056(2) C43 0.0424(16) 0.0377(14) 0.0456(16) 0.0209(13) 0.0271(13) 0.0194(13) C44 0.0489(17) 0.0401(15) 0.0538(17) 0.0245(13) 0.0334(15) 0.0257(13) C45 0.0462(16) 0.0449(15) 0.0455(16) 0.0226(13) 0.0303(14) 0.0207(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N3 2.2532(19) . ? Ag1 N1 2.2813(19) . ? Ag1 N4 2.2983(19) 2_655 ? Ag1 N2 2.348(2) 2_866 ? P1 F3A 1.500(11) . ? P1 F4A 1.538(11) . ? P1 F1A 1.542(7) . ? P1 F5 1.543(4) . ? P1 F1 1.547(5) . ? P1 F2 1.549(8) . ? P1 F2A 1.570(12) . ? P1 F6A 1.573(8) . ? P1 F4 1.574(8) . ? P1 F6 1.576(4) . ? P1 F3 1.590(6) . ? P1 F5A 1.634(8) . ? O1 C4 1.363(3) . ? O1 N1 1.413(2) . ? O2 C15 1.363(3) . ? O2 N2 1.410(3) . ? O3 C22 1.363(3) . ? O3 N3 1.408(2) . ? O4 C35 1.363(3) . ? O4 N4 1.414(2) . ? O5 C40 1.337(3) . ? O5 N5 1.449(3) . ? N1 C2 1.309(3) . ? N2 C17 1.306(3) . ? N2 Ag1 2.348(2) 2_866 ? N3 C20 1.306(3) . ? N4 C33 1.308(3) . ? N4 Ag1 2.2983(19) 2_655 ? N5 C38 1.325(4) . ? C1 C2 1.485(3) . ? C1 H1A 0.9800 . ? C1 H1 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.431(3) . ? C3 C4 1.345(3) . ? C3 C6 1.506(3) . ? C4 C5 1.485(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.522(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C12 1.389(3) . ? C7 C8 1.391(3) . ? C8 C9 1.379(3) . ? C8 H8 0.9500 . ? C9 C10 1.397(3) . ? C9 H9 0.9500 . ? C10 C11 1.380(3) . ? C10 C13 1.512(4) . ? C11 C12 1.388(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.498(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.354(3) . ? C14 C17 1.421(3) . ? C15 C16 1.485(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.481(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.487(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.422(3) . ? C21 C22 1.346(3) . ? C21 C24 1.506(3) . ? C22 C23 1.479(3) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.522(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C30 1.377(4) . ? C25 C26 1.389(4) . ? C26 C27 1.382(4) . ? C26 H26 0.9500 . ? C27 C28 1.394(4) . ? C27 H27 0.9500 . ? C28 C29 1.380(4) . ? C28 C31 1.518(4) . ? C29 C30 1.386(4) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.507(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C35 1.348(4) . ? C32 C33 1.423(3) . ? C33 C34 1.485(3) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.491(4) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.491(5) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.394(4) . ? C39 C40 1.371(4) . ? C39 C42 1.488(4) . ? C40 C41 1.475(4) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.516(3) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.386(3) . ? C43 C45 1.388(3) . ? C44 C45 1.378(3) 2_655 ? C44 H44 0.9500 . ? C45 C44 1.378(3) 2_655 ? C45 H45 0.9500 . ? 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 N3 Ag1 N1 114.72(7) . . ? N3 Ag1 N4 117.09(7) . 2_655 ? N1 Ag1 N4 111.42(7) . 2_655 ? N3 Ag1 N2 105.55(7) . 2_866 ? N1 Ag1 N2 105.97(7) . 2_866 ? N4 Ag1 N2 100.14(7) 2_655 2_866 ? F3A P1 F4A 92.7(8) . . ? F3A P1 F1A 89.5(7) . . ? F4A P1 F1A 88.3(7) . . ? F3A P1 F5 150.6(7) . . ? F4A P1 F5 90.8(6) . . ? F1A P1 F5 119.8(6) . . ? F3A P1 F1 113.9(6) . . ? F4A P1 F1 111.4(7) . . ? F1A P1 F1 35.5(4) . . ? F5 P1 F1 91.8(3) . . ? F3A P1 F2 84.6(7) . . ? F4A P1 F2 174.5(8) . . ? F1A P1 F2 96.5(6) . . ? F5 P1 F2 89.2(5) . . ? F1 P1 F2 74.2(5) . . ? F3A P1 F2A 80.2(9) . . ? F4A P1 F2A 160.4(9) . . ? F1A P1 F2A 109.7(7) . . ? F5 P1 F2A 86.8(7) . . ? F1 P1 F2A 88.2(7) . . ? F2 P1 F2A 14.2(9) . . ? F3A P1 F6A 96.6(9) . . ? F4A P1 F6A 90.0(7) . . ? F1A P1 F6A 173.7(8) . . ? F5 P1 F6A 54.1(6) . . ? F1 P1 F6A 140.8(7) . . ? F2 P1 F6A 85.5(6) . . ? F2A P1 F6A 72.9(7) . . ? F3A P1 F4 99.0(7) . . ? F4A P1 F4 16.3(10) . . ? F1A P1 F4 73.5(6) . . ? F5 P1 F4 92.5(5) . . ? F1 P1 F4 95.1(5) . . ? F2 P1 F4 169.2(6) . . ? F2A P1 F4 176.6(8) . . ? F6A P1 F4 104.1(6) . . ? F3A P1 F6 63.4(6) . . ? F4A P1 F6 71.4(7) . . ? F1A P1 F6 144.3(6) . . ? F5 P1 F6 90.3(3) . . ? F1 P1 F6 176.5(4) . . ? F2 P1 F6 103.1(5) . . ? F2A P1 F6 89.1(7) . . ? F6A P1 F6 39.9(6) . . ? F4 P1 F6 87.6(5) . . ? F3A P1 F3 26.6(7) . . ? F4A P1 F3 90.7(6) . . ? F1A P1 F3 62.9(5) . . ? F5 P1 F3 176.9(4) . . ? F1 P1 F3 90.2(3) . . ? F2 P1 F3 89.0(5) . . ? F2A P1 F3 90.8(7) . . ? F6A P1 F3 123.2(7) . . ? F4 P1 F3 89.7(5) . . ? F6 P1 F3 87.7(3) . . ? F3A P1 F5A 176.9(7) . . ? F4A P1 F5A 86.2(7) . . ? F1A P1 F5A 87.6(6) . . ? F5 P1 F5A 32.5(3) . . ? F1 P1 F5A 63.9(5) . . ? F2 P1 F5A 96.8(5) . . ? F2A P1 F5A 101.8(8) . . ? F6A P1 F5A 86.3(7) . . ? F4 P1 F5A 79.2(5) . . ? F6 P1 F5A 118.9(5) . . ? F3 P1 F5A 150.4(5) . . ? C4 O1 N1 107.69(16) . . ? C15 O2 N2 108.24(16) . . ? C22 O3 N3 107.08(17) . . ? C35 O4 N4 107.74(18) . . ? C40 O5 N5 106.9(2) . . ? C2 N1 O1 106.50(17) . . ? C2 N1 Ag1 134.18(16) . . ? O1 N1 Ag1 119.31(13) . . ? C17 N2 O2 105.84(18) . . ? C17 N2 Ag1 138.96(17) . 2_866 ? O2 N2 Ag1 115.08(12) . 2_866 ? C20 N3 O3 106.70(17) . . ? C20 N3 Ag1 136.44(15) . . ? O3 N3 Ag1 114.73(13) . . ? C33 N4 O4 105.93(18) . . ? C33 N4 Ag1 135.22(16) . 2_655 ? O4 N4 Ag1 113.73(13) . 2_655 ? C38 N5 O5 105.3(2) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1 109.5 . . ? H1A C1 H1 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1 C1 H1C 109.5 . . ? N1 C2 C3 110.9(2) . . ? N1 C2 C1 121.0(2) . . ? C3 C2 C1 128.1(2) . . ? C4 C3 C2 104.8(2) . . ? C4 C3 C6 129.5(2) . . ? C2 C3 C6 125.7(2) . . ? C3 C4 O1 110.16(19) . . ? C3 C4 C5 134.4(2) . . ? O1 C4 C5 115.4(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 C7 115.37(19) . . ? C3 C6 H6A 108.4 . . ? C7 C6 H6A 108.4 . . ? C3 C6 H6B 108.4 . . ? C7 C6 H6B 108.4 . . ? H6A C6 H6B 107.5 . . ? C12 C7 C8 118.4(2) . . ? C12 C7 C6 120.0(2) . . ? C8 C7 C6 121.5(2) . . ? C9 C8 C7 120.6(2) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 121.1(2) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C11 C10 C9 118.1(2) . . ? C11 C10 C13 120.9(2) . . ? C9 C10 C13 120.9(2) . . ? C10 C11 C12 121.0(2) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C11 C12 C7 120.8(2) . . ? C11 C12 H12 119.6 . . ? C7 C12 H12 119.6 . . ? C14 C13 C10 114.9(2) . . ? C14 C13 H13A 108.5 . . ? C10 C13 H13A 108.5 . . ? C14 C13 H13B 108.5 . . ? C10 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? C15 C14 C17 104.4(2) . . ? C15 C14 C13 131.7(2) . . ? C17 C14 C13 123.8(2) . . ? C14 C15 O2 109.6(2) . . ? C14 C15 C16 136.7(2) . . ? O2 C15 C16 113.7(2) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 C14 111.9(2) . . ? N2 C17 C18 121.3(2) . . ? C14 C17 C18 126.9(2) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 C21 111.3(2) . . ? N3 C20 C19 120.1(2) . . ? C21 C20 C19 128.5(2) . . ? C22 C21 C20 104.2(2) . . ? C22 C21 C24 128.3(2) . . ? C20 C21 C24 127.5(2) . . ? C21 C22 O3 110.7(2) . . ? C21 C22 C23 134.1(3) . . ? O3 C22 C23 115.2(2) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 C25 113.6(2) . . ? C21 C24 H24A 108.9 . . ? C25 C24 H24A 108.9 . . ? C21 C24 H24B 108.9 . . ? C25 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? C30 C25 C26 117.7(3) . . ? C30 C25 C24 121.4(3) . . ? C26 C25 C24 121.0(3) . . ? C27 C26 C25 120.9(3) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 C28 121.2(2) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? C29 C28 C27 117.6(2) . . ? C29 C28 C31 120.7(2) . . ? C27 C28 C31 121.7(2) . . ? C28 C29 C30 121.0(3) . . ? C28 C29 H29 119.5 . . ? C30 C29 H29 119.5 . . ? C25 C30 C29 121.6(3) . . ? C25 C30 H30 119.2 . . ? C29 C30 H30 119.2 . . ? C32 C31 C28 115.6(2) . . ? C32 C31 H31A 108.4 . . ? C28 C31 H31A 108.4 . . ? C32 C31 H31B 108.4 . . ? C28 C31 H31B 108.4 . . ? H31A C31 H31B 107.4 . . ? C35 C32 C33 104.4(2) . . ? C35 C32 C31 128.3(2) . . ? C33 C32 C31 127.2(2) . . ? N4 C33 C32 111.7(2) . . ? N4 C33 C34 120.5(2) . . ? C32 C33 C34 127.7(2) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 O4 110.2(2) . . ? C32 C35 C36 134.6(3) . . ? O4 C35 C36 115.2(2) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 H37A 109.5 . . ? C38 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C38 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N5 C38 C39 112.1(3) . . ? N5 C38 C37 117.7(3) . . ? C39 C38 C37 130.3(3) . . ? C40 C39 C38 104.5(3) . . ? C40 C39 C42 127.9(3) . . ? C38 C39 C42 127.6(3) . . ? O5 C40 C39 111.2(3) . . ? O5 C40 C41 116.6(3) . . ? C39 C40 C41 132.1(3) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C39 C42 C43 116.3(2) . . ? C39 C42 H42A 108.2 . . ? C43 C42 H42A 108.2 . . ? C39 C42 H42B 108.2 . . ? C43 C42 H42B 108.2 . . ? H42A C42 H42B 107.4 . . ? C44 C43 C45 117.8(2) . . ? C44 C43 C42 122.7(2) . . ? C45 C43 C42 119.5(2) . . ? C45 C44 C43 120.5(2) 2_655 . ? C45 C44 H44 119.8 2_655 . ? C43 C44 H44 119.8 . . ? C44 C45 C43 121.7(2) 2_655 . ? C44 C45 H45 119.1 2_655 . ? C43 C45 H45 119.1 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.554 _refine_diff_density_min -0.736 _refine_diff_density_rms 0.152 #===end data_Compound-8-h09adb04(CCDC-804684) _database_code_depnum_ccdc_archive 'CCDC 804684' #TrackingRef '- stevenson-rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H50 Ag F6 N5 O5 Sb' _chemical_formula_weight 1084.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5300(3) _cell_length_b 14.3010(4) _cell_length_c 14.3670(3) _cell_angle_alpha 103.860(1) _cell_angle_beta 113.574(1) _cell_angle_gamma 103.746(1) _cell_volume 2293.51(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 29587 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1094 _exptl_absorpt_coefficient_mu 1.090 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.612 _exptl_absorpt_correction_T_max 0.725 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38829 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 27.54 _reflns_number_total 10477 _reflns_number_gt 7989 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski, Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick 1990)' _computing_structure_refinement 'SHELXL-97/2 (Sheldrick 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle 1995)' _computing_publication_material 'SHELXL-97/2 (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^)+(0.0329P)^2^+0.9476P] 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 0.0045(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10477 _refine_ls_number_parameters 634 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0783 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 Sb1 Sb -0.840602(17) -0.624685(14) -0.092087(15) 0.03549(7) Uani 1 1 d . . . Ag1 Ag 0.035808(18) 0.235358(15) 0.327157(16) 0.03263(7) Uani 1 1 d . . . F1 F -0.8483(9) -0.7323(9) -0.0401(8) 0.071(2) Uani 0.70 1 d P A 1 F2 F -0.8329(10) -0.5215(6) -0.1464(8) 0.102(3) Uani 0.70 1 d P A 1 F3 F -0.8544(5) -0.7139(5) -0.2196(4) 0.0657(15) Uani 0.70 1 d P A 1 F4 F -0.6815(4) -0.5874(4) -0.0344(4) 0.0927(15) Uani 0.70 1 d P A 1 F5 F -0.8198(5) -0.5409(3) 0.0377(3) 0.0847(16) Uani 0.70 1 d P A 1 F6 F -0.9980(4) -0.6709(5) -0.1534(4) 0.0968(17) Uani 0.70 1 d P A 1 F1A F -0.886(2) -0.7358(18) -0.056(2) 0.104(9) Uani 0.30 1 d P A 2 F2A F -0.797(2) -0.5100(12) -0.1273(18) 0.099(8) Uani 0.30 1 d P A 2 F3A F -0.8018(19) -0.7017(13) -0.1745(17) 0.162(10) Uani 0.30 1 d P A 2 F4A F -0.7014(14) -0.5692(10) 0.0319(13) 0.180(9) Uani 0.30 1 d P A 2 F5A F -0.8939(12) -0.5404(9) -0.0143(11) 0.095(4) Uani 0.30 1 d P A 2 F6A F -0.9839(14) -0.6693(10) -0.2107(11) 0.184(9) Uani 0.30 1 d P A 2 O1 O 0.10610(17) 0.06322(14) 0.21806(17) 0.0434(5) Uani 1 1 d . . . O2 O 0.90871(16) 0.52617(13) 0.59878(15) 0.0341(4) Uani 1 1 d . . . O3 O -0.03868(15) 0.14819(13) 0.48607(13) 0.0292(4) Uani 1 1 d . . . O4 O -0.77602(16) -0.16543(14) -0.12944(15) 0.0354(4) Uani 1 1 d . . . O5 O 0.5844(2) 0.12663(17) 0.5128(2) 0.0585(6) Uani 1 1 d . . . N1 N 0.1459(2) 0.17252(17) 0.25975(19) 0.0364(5) Uani 1 1 d . . . N2 N 0.87900(19) 0.59847(16) 0.55281(18) 0.0317(5) Uani 1 1 d . . . N3 N -0.05720(19) 0.11761(16) 0.37730(17) 0.0311(5) Uani 1 1 d . . . N4 N -0.88990(19) -0.23354(17) -0.16717(18) 0.0340(5) Uani 1 1 d . . . N5 N 0.6920(2) 0.2095(2) 0.5991(2) 0.0458(6) Uani 1 1 d . . . C1 C 0.1137(3) -0.0794(3) 0.0958(4) 0.0697(11) Uani 1 1 d . . . H1A H 0.1469 -0.0929 0.0470 0.104 Uiso 1 1 calc R . . H1B H 0.0287 -0.1121 0.0533 0.104 Uiso 1 1 calc R . . H1C H 0.1424 -0.1082 0.1521 0.104 Uiso 1 1 calc R . . C2 C 0.1490(3) 0.0349(2) 0.1492(3) 0.0425(7) Uani 1 1 d . . . C3 C 0.2144(2) 0.1189(2) 0.1451(2) 0.0333(6) Uani 1 1 d . . . C4 C 0.2094(2) 0.2050(2) 0.2163(2) 0.0305(6) Uani 1 1 d . . . C5 C 0.2642(2) 0.3174(2) 0.2422(2) 0.0384(6) Uani 1 1 d . . . H5A H 0.2505 0.3577 0.2982 0.058 Uiso 1 1 calc R . . H5B H 0.2302 0.3324 0.1758 0.058 Uiso 1 1 calc R . . H5C H 0.3481 0.3366 0.2698 0.058 Uiso 1 1 calc R . . C6 C 0.2748(2) 0.1238(2) 0.0772(2) 0.0417(7) Uani 1 1 d . . . H6A H 0.2361 0.1515 0.0218 0.050 Uiso 1 1 calc R . . H6B H 0.2640 0.0521 0.0373 0.050 Uiso 1 1 calc R . . C7 C 0.4041(2) 0.1894(2) 0.1402(2) 0.0350(6) Uani 1 1 d . . . C8 C 0.4819(2) 0.1682(2) 0.2223(2) 0.0381(6) Uani 1 1 d . . . H8 H 0.4534 0.1133 0.2424 0.046 Uiso 1 1 calc R . . C9 C 0.6001(2) 0.2252(2) 0.2755(2) 0.0388(6) Uani 1 1 d . . . H9 H 0.6513 0.2086 0.3312 0.047 Uiso 1 1 calc R . . C10 C 0.6455(2) 0.3066(2) 0.2488(2) 0.0365(6) Uani 1 1 d . . . C11 C 0.5673(3) 0.3280(2) 0.1671(3) 0.0444(7) Uani 1 1 d . . . H11 H 0.5955 0.3828 0.1468 0.053 Uiso 1 1 calc R . . C12 C 0.4489(3) 0.2708(2) 0.1144(2) 0.0449(7) Uani 1 1 d . . . H12 H 0.3974 0.2879 0.0594 0.054 Uiso 1 1 calc R . . C13 C 0.7754(2) 0.3675(2) 0.3045(2) 0.0433(7) Uani 1 1 d . . . H13A H 0.8160 0.3182 0.3097 0.052 Uiso 1 1 calc R . . H13B H 0.7921 0.4033 0.2584 0.052 Uiso 1 1 calc R . . C14 C 0.8239(2) 0.4469(2) 0.4177(2) 0.0319(6) Uani 1 1 d . . . C15 C 0.8741(2) 0.43612(19) 0.5146(2) 0.0331(6) Uani 1 1 d . . . C16 C 0.9000(3) 0.3502(2) 0.5470(3) 0.0512(8) Uani 1 1 d . . . H16A H 0.9657 0.3789 0.6215 0.077 Uiso 1 1 calc R . . H16B H 0.9199 0.3103 0.4962 0.077 Uiso 1 1 calc R . . H16C H 0.8316 0.3046 0.5445 0.077 Uiso 1 1 calc R . . C17 C 0.8293(2) 0.5510(2) 0.4466(2) 0.0297(5) Uani 1 1 d . . . C18 C 0.7897(3) 0.6078(2) 0.3733(2) 0.0418(7) Uani 1 1 d . . . H18A H 0.8040 0.6783 0.4175 0.063 Uiso 1 1 calc R . . H18B H 0.7063 0.5711 0.3218 0.063 Uiso 1 1 calc R . . H18C H 0.8328 0.6113 0.3325 0.063 Uiso 1 1 calc R . . C19 C -0.1674(3) -0.0368(2) 0.2101(2) 0.0378(6) Uani 1 1 d . . . H19A H -0.1223 0.0051 0.1853 0.057 Uiso 1 1 calc R . . H19B H -0.2500 -0.0500 0.1666 0.057 Uiso 1 1 calc R . . H19C H -0.1563 -0.1031 0.2007 0.057 Uiso 1 1 calc R . . C20 C -0.1272(2) 0.02005(19) 0.3276(2) 0.0281(5) Uani 1 1 d . . . C21 C -0.1571(2) -0.01799(19) 0.3999(2) 0.0261(5) Uani 1 1 d . . . C22 C -0.1012(2) 0.06446(19) 0.4957(2) 0.0275(5) Uani 1 1 d . . . C23 C -0.0959(3) 0.0833(2) 0.6039(2) 0.0374(6) Uani 1 1 d . . . H23A H -0.1510 0.1157 0.6078 0.056 Uiso 1 1 calc R . . H23B H -0.0170 0.1295 0.6619 0.056 Uiso 1 1 calc R . . H23C H -0.1161 0.0171 0.6135 0.056 Uiso 1 1 calc R . . C24 C -0.2291(2) -0.12776(19) 0.3742(2) 0.0305(6) Uani 1 1 d . . . H24A H -0.2195 -0.1351 0.4438 0.037 Uiso 1 1 calc R . . H24B H -0.1979 -0.1748 0.3425 0.037 Uiso 1 1 calc R . . C25 C -0.3579(2) -0.16351(19) 0.2961(2) 0.0277(5) Uani 1 1 d . . . C26 C -0.4150(2) -0.2585(2) 0.2081(2) 0.0329(6) Uani 1 1 d . . . H26 H -0.3717 -0.2982 0.1942 0.039 Uiso 1 1 calc R . . C27 C -0.5345(2) -0.2961(2) 0.1403(2) 0.0346(6) Uani 1 1 d . . . H27 H -0.5718 -0.3614 0.0811 0.042 Uiso 1 1 calc R . . C28 C -0.5999(2) -0.2401(2) 0.1576(2) 0.0313(6) Uani 1 1 d . . . C29 C -0.5427(2) -0.1441(2) 0.2447(2) 0.0338(6) Uani 1 1 d . . . H29 H -0.5863 -0.1044 0.2577 0.041 Uiso 1 1 calc R . . C30 C -0.4232(2) -0.1058(2) 0.3128(2) 0.0317(6) Uani 1 1 d . . . H30 H -0.3858 -0.0398 0.3710 0.038 Uiso 1 1 calc R . . C31 C -0.7293(2) -0.2801(2) 0.0825(2) 0.0351(6) Uani 1 1 d . . . H31A H -0.7596 -0.3570 0.0532 0.042 Uiso 1 1 calc R . . H31B H -0.7664 -0.2576 0.1262 0.042 Uiso 1 1 calc R . . C32 C -0.7650(2) -0.24463(19) -0.0124(2) 0.0282(5) Uani 1 1 d . . . C33 C -0.8817(2) -0.28014(19) -0.0975(2) 0.0284(5) Uani 1 1 d . . . C34 C -0.9858(2) -0.3592(2) -0.1124(2) 0.0389(6) Uani 1 1 d . . . H34A H -1.0528 -0.3735 -0.1825 0.058 Uiso 1 1 calc R . . H34B H -1.0017 -0.3332 -0.0525 0.058 Uiso 1 1 calc R . . H34C H -0.9717 -0.4233 -0.1123 0.058 Uiso 1 1 calc R . . C35 C -0.7030(2) -0.17503(19) -0.0368(2) 0.0302(6) Uani 1 1 d . . . C36 C -0.5790(2) -0.1076(2) 0.0105(2) 0.0414(7) Uani 1 1 d . . . H36A H -0.5641 -0.0382 0.0577 0.062 Uiso 1 1 calc R . . H36B H -0.5623 -0.1026 -0.0489 0.062 Uiso 1 1 calc R . . H36C H -0.5290 -0.1377 0.0538 0.062 Uiso 1 1 calc R . . C37 C 0.3799(3) 0.0902(3) 0.4173(3) 0.0552(8) Uani 1 1 d . . . H37A H 0.3664 0.0862 0.3439 0.083 Uiso 1 1 calc R . . H37B H 0.3243 0.1148 0.4328 0.083 Uiso 1 1 calc R . . H37C H 0.3696 0.0212 0.4209 0.083 Uiso 1 1 calc R . . C38 C 0.5000(3) 0.1634(2) 0.4997(3) 0.0437(7) Uani 1 1 d . . . C39 C 0.5435(3) 0.2645(2) 0.5700(2) 0.0396(7) Uani 1 1 d . . . C40 C 0.6629(3) 0.2888(2) 0.6295(3) 0.0458(7) Uani 1 1 d . . . C41 C 0.7555(3) 0.3871(3) 0.7175(3) 0.0613(9) Uani 1 1 d . . . H41A H 0.8258 0.3742 0.7565 0.092 Uiso 1 1 calc R . . H41B H 0.7293 0.4144 0.7689 0.092 Uiso 1 1 calc R . . H41C H 0.7726 0.4379 0.6853 0.092 Uiso 1 1 calc R . . C42 C 0.4779(3) 0.3324(2) 0.5834(3) 0.0478(8) Uani 1 1 d . . . H42A H 0.5026 0.3636 0.6623 0.057 Uiso 1 1 calc R . . H42B H 0.3942 0.2881 0.5454 0.057 Uiso 1 1 calc R . . C43 C 0.4919(2) 0.4197(2) 0.5406(2) 0.0321(6) Uani 1 1 d . . . C44 C 0.4474(2) 0.4946(2) 0.5637(2) 0.0335(6) Uani 1 1 d . . . H44 H 0.4114 0.4919 0.6083 0.040 Uiso 1 1 calc R . . C45 C 0.4542(2) 0.5733(2) 0.5235(2) 0.0341(6) Uani 1 1 d . . . H45 H 0.4217 0.6230 0.5397 0.041 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 Sb1 0.04797(13) 0.02946(11) 0.03416(11) 0.01331(8) 0.02385(9) 0.01431(9) Ag1 0.04383(13) 0.02664(11) 0.03195(12) 0.01081(9) 0.02198(10) 0.01421(9) F1 0.104(5) 0.059(4) 0.060(3) 0.041(3) 0.037(3) 0.032(4) F2 0.211(8) 0.090(6) 0.127(6) 0.091(5) 0.132(6) 0.112(6) F3 0.102(3) 0.038(2) 0.0494(18) 0.0024(14) 0.0482(19) 0.008(2) F4 0.0442(19) 0.108(4) 0.088(3) 0.025(3) 0.022(2) -0.002(2) F5 0.166(5) 0.0365(18) 0.064(3) 0.0097(18) 0.082(3) 0.020(3) F6 0.051(2) 0.164(5) 0.102(4) 0.068(4) 0.041(3) 0.057(3) F1A 0.17(2) 0.027(6) 0.122(17) 0.025(8) 0.102(16) 0.000(10) F2A 0.202(17) 0.019(5) 0.090(9) 0.008(5) 0.113(11) 0.003(7) F3A 0.30(3) 0.096(13) 0.31(3) 0.111(16) 0.28(2) 0.138(16) F4A 0.136(13) 0.075(7) 0.142(13) 0.034(9) -0.077(10) 0.001(8) F5A 0.178(12) 0.070(6) 0.150(11) 0.071(8) 0.143(11) 0.084(8) F6A 0.173(14) 0.072(7) 0.113(11) 0.011(8) -0.084(9) 0.034(8) O1 0.0479(12) 0.0273(10) 0.0638(14) 0.0119(10) 0.0378(11) 0.0143(9) O2 0.0413(11) 0.0275(9) 0.0361(10) 0.0146(8) 0.0195(9) 0.0130(8) O3 0.0360(10) 0.0239(9) 0.0267(9) 0.0078(8) 0.0166(8) 0.0089(8) O4 0.0432(11) 0.0323(10) 0.0369(11) 0.0166(9) 0.0235(9) 0.0129(9) O5 0.0708(16) 0.0447(13) 0.0804(17) 0.0294(13) 0.0474(14) 0.0293(13) N1 0.0423(13) 0.0283(12) 0.0449(14) 0.0112(11) 0.0264(12) 0.0166(11) N2 0.0427(13) 0.0236(11) 0.0344(13) 0.0133(10) 0.0214(11) 0.0138(10) N3 0.0389(13) 0.0274(11) 0.0260(11) 0.0086(9) 0.0168(10) 0.0102(10) N4 0.0364(13) 0.0361(12) 0.0355(13) 0.0157(11) 0.0202(11) 0.0162(11) N5 0.0408(14) 0.0430(15) 0.0710(18) 0.0345(14) 0.0305(14) 0.0242(13) C1 0.067(2) 0.0341(18) 0.103(3) 0.0025(19) 0.053(2) 0.0139(17) C2 0.0383(16) 0.0346(16) 0.0519(19) 0.0033(14) 0.0262(15) 0.0140(13) C3 0.0291(14) 0.0369(15) 0.0290(14) 0.0052(12) 0.0136(12) 0.0126(12) C4 0.0254(13) 0.0332(14) 0.0280(14) 0.0088(11) 0.0096(11) 0.0118(11) C5 0.0409(16) 0.0343(15) 0.0408(16) 0.0120(13) 0.0210(14) 0.0152(13) C6 0.0391(16) 0.0479(18) 0.0309(15) 0.0045(13) 0.0176(13) 0.0141(14) C7 0.0366(15) 0.0395(15) 0.0298(14) 0.0053(12) 0.0210(13) 0.0146(13) C8 0.0402(16) 0.0373(15) 0.0369(16) 0.0123(13) 0.0227(14) 0.0092(13) C9 0.0377(16) 0.0434(17) 0.0331(15) 0.0110(13) 0.0181(13) 0.0131(13) C10 0.0425(16) 0.0289(14) 0.0355(15) -0.0003(12) 0.0262(14) 0.0087(12) C11 0.0562(19) 0.0350(16) 0.0479(18) 0.0133(14) 0.0337(16) 0.0136(14) C12 0.0488(19) 0.0484(18) 0.0420(17) 0.0173(15) 0.0229(15) 0.0235(16) C13 0.0404(16) 0.0367(16) 0.0480(18) 0.0005(14) 0.0307(15) 0.0058(13) C14 0.0306(14) 0.0275(13) 0.0391(15) 0.0063(12) 0.0226(13) 0.0092(11) C15 0.0325(14) 0.0229(13) 0.0492(17) 0.0112(12) 0.0262(13) 0.0099(11) C16 0.0526(19) 0.0377(17) 0.080(2) 0.0290(17) 0.0393(19) 0.0243(15) C17 0.0288(13) 0.0299(13) 0.0318(14) 0.0099(12) 0.0185(12) 0.0083(11) C18 0.0474(17) 0.0410(16) 0.0396(17) 0.0195(14) 0.0220(14) 0.0148(14) C19 0.0482(17) 0.0313(14) 0.0261(14) 0.0083(12) 0.0153(13) 0.0097(13) C20 0.0309(14) 0.0236(13) 0.0258(13) 0.0078(11) 0.0113(11) 0.0098(11) C21 0.0248(13) 0.0274(13) 0.0284(13) 0.0130(11) 0.0124(11) 0.0116(11) C22 0.0269(13) 0.0278(13) 0.0299(14) 0.0132(11) 0.0135(11) 0.0116(11) C23 0.0435(16) 0.0389(16) 0.0317(15) 0.0129(13) 0.0212(13) 0.0136(13) C24 0.0308(14) 0.0260(13) 0.0313(14) 0.0116(11) 0.0124(12) 0.0088(11) C25 0.0293(13) 0.0261(13) 0.0261(13) 0.0113(11) 0.0129(11) 0.0071(11) C26 0.0356(15) 0.0271(13) 0.0363(15) 0.0108(12) 0.0185(13) 0.0117(12) C27 0.0374(15) 0.0260(13) 0.0298(14) 0.0062(11) 0.0127(12) 0.0052(12) C28 0.0312(14) 0.0310(14) 0.0314(14) 0.0164(12) 0.0140(12) 0.0086(12) C29 0.0357(15) 0.0331(14) 0.0375(15) 0.0150(13) 0.0195(13) 0.0159(12) C30 0.0390(15) 0.0250(13) 0.0271(14) 0.0061(11) 0.0159(12) 0.0093(12) C31 0.0306(14) 0.0358(15) 0.0332(15) 0.0170(12) 0.0115(12) 0.0060(12) C32 0.0321(14) 0.0215(12) 0.0302(14) 0.0074(11) 0.0163(12) 0.0092(11) C33 0.0319(14) 0.0276(13) 0.0288(13) 0.0091(11) 0.0170(12) 0.0135(11) C34 0.0298(14) 0.0427(16) 0.0387(16) 0.0153(14) 0.0139(13) 0.0097(13) C35 0.0379(15) 0.0251(13) 0.0301(14) 0.0084(11) 0.0194(12) 0.0123(11) C36 0.0418(16) 0.0338(15) 0.0439(17) 0.0128(13) 0.0243(14) 0.0021(13) C37 0.061(2) 0.061(2) 0.051(2) 0.0304(18) 0.0292(18) 0.0229(18) C38 0.060(2) 0.0438(17) 0.0516(19) 0.0312(16) 0.0371(17) 0.0268(16) C39 0.0566(19) 0.0410(16) 0.0509(18) 0.0319(15) 0.0384(16) 0.0290(15) C40 0.0534(19) 0.0444(18) 0.056(2) 0.0324(16) 0.0328(17) 0.0194(16) C41 0.069(2) 0.053(2) 0.064(2) 0.0304(19) 0.033(2) 0.0161(19) C42 0.068(2) 0.0455(18) 0.069(2) 0.0389(17) 0.0513(19) 0.0340(17) C43 0.0375(15) 0.0328(14) 0.0366(15) 0.0189(12) 0.0228(13) 0.0158(12) C44 0.0389(15) 0.0386(15) 0.0384(15) 0.0197(13) 0.0275(13) 0.0184(13) C45 0.0414(15) 0.0351(14) 0.0434(16) 0.0210(13) 0.0279(14) 0.0230(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sb1 F3A 1.744(13) . ? Sb1 F4A 1.811(11) . ? Sb1 F6 1.817(4) . ? Sb1 F6A 1.822(11) . ? Sb1 F5 1.827(3) . ? Sb1 F2 1.828(7) . ? Sb1 F1A 1.83(2) . ? Sb1 F4 1.850(4) . ? Sb1 F2A 1.861(18) . ? Sb1 F1 1.864(9) . ? Sb1 F3 1.875(5) . ? Sb1 F5A 1.906(9) . ? Ag1 N2 2.257(2) 2_666 ? Ag1 N3 2.289(2) . ? Ag1 N1 2.310(2) . ? Ag1 N4 2.345(2) 2_455 ? O1 C2 1.363(3) . ? O1 N1 1.409(3) . ? O2 C15 1.362(3) . ? O2 N2 1.407(3) . ? O3 C22 1.364(3) . ? O3 N3 1.415(3) . ? O4 C35 1.366(3) . ? O4 N4 1.408(3) . ? O5 C38 1.333(4) . ? O5 N5 1.447(3) . ? N1 C4 1.312(3) . ? N2 C17 1.307(3) . ? N2 Ag1 2.257(2) 2_666 ? N3 C20 1.307(3) . ? N4 C33 1.313(3) . ? N4 Ag1 2.345(2) 2_455 ? N5 C40 1.321(4) . ? C1 C2 1.491(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.342(4) . ? C3 C4 1.434(4) . ? C3 C6 1.506(4) . ? C4 C5 1.484(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.519(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C12 1.382(4) . ? C7 C8 1.386(4) . ? C8 C9 1.382(4) . ? C8 H8 0.9500 . ? C9 C10 1.394(4) . ? C9 H9 0.9500 . ? C10 C11 1.386(4) . ? C10 C13 1.517(4) . ? C11 C12 1.386(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.508(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.348(4) . ? C14 C17 1.421(4) . ? C15 C16 1.482(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.490(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.485(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.428(3) . ? C21 C22 1.351(3) . ? C21 C24 1.502(3) . ? C22 C23 1.481(3) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.515(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.392(4) . ? C25 C30 1.393(4) . ? C26 C27 1.388(4) . ? C26 H26 0.9500 . ? C27 C28 1.379(4) . ? C27 H27 0.9500 . ? C28 C29 1.395(4) . ? C28 C31 1.508(4) . ? C29 C30 1.389(4) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.508(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C35 1.349(3) . ? C32 C33 1.423(4) . ? C33 C34 1.481(4) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.487(4) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.482(5) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.370(4) . ? C39 C40 1.395(4) . ? C39 C42 1.492(4) . ? C40 C41 1.479(5) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.524(4) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.384(4) . ? C43 C45 1.392(3) 2_666 ? C44 C45 1.384(4) . ? C44 H44 0.9500 . ? C45 C43 1.392(3) 2_666 ? C45 H45 0.9500 . ? 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 F3A Sb1 F4A 97.1(11) . . ? F3A Sb1 F6 109.7(8) . . ? F4A Sb1 F6 147.6(8) . . ? F3A Sb1 F6A 88.5(10) . . ? F4A Sb1 F6A 174.1(8) . . ? F6 Sb1 F6A 29.3(7) . . ? F3A Sb1 F5 154.8(8) . . ? F4A Sb1 F5 58.2(8) . . ? F6 Sb1 F5 92.6(2) . . ? F6A Sb1 F5 116.4(7) . . ? F3A Sb1 F2 96.8(7) . . ? F4A Sb1 F2 101.7(6) . . ? F6 Sb1 F2 93.2(4) . . ? F6A Sb1 F2 75.5(6) . . ? F5 Sb1 F2 93.6(3) . . ? F3A Sb1 F1A 87.6(12) . . ? F4A Sb1 F1A 90.7(9) . . ? F6 Sb1 F1A 73.0(9) . . ? F6A Sb1 F1A 91.6(10) . . ? F5 Sb1 F1A 87.7(10) . . ? F2 Sb1 F1A 166.2(9) . . ? F3A Sb1 F4 66.7(8) . . ? F4A Sb1 F4 34.3(8) . . ? F6 Sb1 F4 175.8(3) . . ? F6A Sb1 F4 149.4(8) . . ? F5 Sb1 F4 90.5(2) . . ? F2 Sb1 F4 89.3(4) . . ? F1A Sb1 F4 104.4(9) . . ? F3A Sb1 F2A 94.2(9) . . ? F4A Sb1 F2A 89.7(9) . . ? F6 Sb1 F2A 105.8(9) . . ? F6A Sb1 F2A 87.9(9) . . ? F5 Sb1 F2A 90.9(6) . . ? F2 Sb1 F2A 12.7(11) . . ? F1A Sb1 F2A 178.1(13) . . ? F4 Sb1 F2A 76.9(9) . . ? F3A Sb1 F1 81.6(7) . . ? F4A Sb1 F1 78.9(5) . . ? F6 Sb1 F1 87.0(4) . . ? F6A Sb1 F1 104.0(6) . . ? F5 Sb1 F1 88.0(4) . . ? F2 Sb1 F1 178.3(5) . . ? F1A Sb1 F1 14.1(11) . . ? F4 Sb1 F1 90.4(4) . . ? F2A Sb1 F1 167.2(9) . . ? F3A Sb1 F3 21.6(8) . . ? F4A Sb1 F3 118.4(8) . . ? F6 Sb1 F3 90.1(2) . . ? F6A Sb1 F3 67.0(7) . . ? F5 Sb1 F3 176.1(3) . . ? F2 Sb1 F3 89.1(4) . . ? F1A Sb1 F3 90.3(10) . . ? F4 Sb1 F3 86.6(2) . . ? F2A Sb1 F3 91.1(6) . . ? F1 Sb1 F3 89.2(4) . . ? F3A Sb1 F5A 174.6(8) . . ? F4A Sb1 F5A 87.8(8) . . ? F6 Sb1 F5A 66.5(5) . . ? F6A Sb1 F5A 86.6(8) . . ? F5 Sb1 F5A 30.5(4) . . ? F2 Sb1 F5A 79.9(4) . . ? F1A Sb1 F5A 94.7(11) . . ? F4 Sb1 F5A 117.2(5) . . ? F2A Sb1 F5A 83.5(7) . . ? F1 Sb1 F5A 101.7(5) . . ? F3 Sb1 F5A 153.3(5) . . ? N2 Ag1 N3 115.41(7) 2_666 . ? N2 Ag1 N1 116.69(8) 2_666 . ? N3 Ag1 N1 110.87(8) . . ? N2 Ag1 N4 105.78(8) 2_666 2_455 ? N3 Ag1 N4 105.52(8) . 2_455 ? N1 Ag1 N4 100.63(8) . 2_455 ? C2 O1 N1 107.4(2) . . ? C15 O2 N2 107.46(19) . . ? C22 O3 N3 107.76(18) . . ? C35 O4 N4 108.29(18) . . ? C38 O5 N5 106.9(2) . . ? C4 N1 O1 106.7(2) . . ? C4 N1 Ag1 135.56(18) . . ? O1 N1 Ag1 113.12(15) . . ? C17 N2 O2 106.54(19) . . ? C17 N2 Ag1 136.49(17) . 2_666 ? O2 N2 Ag1 114.74(14) . 2_666 ? C20 N3 O3 106.39(19) . . ? C20 N3 Ag1 134.51(17) . . ? O3 N3 Ag1 119.07(14) . . ? C33 N4 O4 105.9(2) . . ? C33 N4 Ag1 137.83(18) . 2_455 ? O4 N4 Ag1 116.29(14) . 2_455 ? C40 N5 O5 105.5(2) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 O1 110.7(2) . . ? C3 C2 C1 134.5(3) . . ? O1 C2 C1 114.8(3) . . ? C2 C3 C4 104.4(2) . . ? C2 C3 C6 128.7(3) . . ? C4 C3 C6 126.8(2) . . ? N1 C4 C3 110.8(2) . . ? N1 C4 C5 120.8(2) . . ? C3 C4 C5 128.4(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 C7 115.7(2) . . ? C3 C6 H6A 108.4 . . ? C7 C6 H6A 108.4 . . ? C3 C6 H6B 108.4 . . ? C7 C6 H6B 108.4 . . ? H6A C6 H6B 107.4 . . ? C12 C7 C8 117.5(3) . . ? C12 C7 C6 120.6(3) . . ? C8 C7 C6 121.8(3) . . ? C9 C8 C7 121.4(3) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C8 C9 C10 121.2(3) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C11 C10 C9 117.3(3) . . ? C11 C10 C13 121.3(3) . . ? C9 C10 C13 121.4(3) . . ? C12 C11 C10 121.3(3) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C7 C12 C11 121.3(3) . . ? C7 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C14 C13 C10 113.8(2) . . ? C14 C13 H13A 108.8 . . ? C10 C13 H13A 108.8 . . ? C14 C13 H13B 108.8 . . ? C10 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? C15 C14 C17 104.3(2) . . ? C15 C14 C13 127.9(3) . . ? C17 C14 C13 127.8(3) . . ? C14 C15 O2 110.3(2) . . ? C14 C15 C16 134.1(3) . . ? O2 C15 C16 115.6(3) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 C14 111.3(2) . . ? N2 C17 C18 120.0(2) . . ? C14 C17 C18 128.6(2) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 C21 111.2(2) . . ? N3 C20 C19 120.8(2) . . ? C21 C20 C19 128.0(2) . . ? C22 C21 C20 104.7(2) . . ? C22 C21 C24 128.7(2) . . ? C20 C21 C24 126.5(2) . . ? C21 C22 O3 109.9(2) . . ? C21 C22 C23 134.7(2) . . ? O3 C22 C23 115.4(2) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 C25 115.6(2) . . ? C21 C24 H24A 108.4 . . ? C25 C24 H24A 108.4 . . ? C21 C24 H24B 108.4 . . ? C25 C24 H24B 108.4 . . ? H24A C24 H24B 107.4 . . ? C26 C25 C30 118.3(2) . . ? C26 C25 C24 120.0(2) . . ? C30 C25 C24 121.6(2) . . ? C27 C26 C25 120.9(2) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C28 C27 C26 121.0(2) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 118.3(2) . . ? C27 C28 C31 120.9(2) . . ? C29 C28 C31 120.8(2) . . ? C30 C29 C28 121.1(2) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C29 C30 C25 120.3(2) . . ? C29 C30 H30 119.8 . . ? C25 C30 H30 119.8 . . ? C32 C31 C28 114.8(2) . . ? C32 C31 H31A 108.6 . . ? C28 C31 H31A 108.6 . . ? C32 C31 H31B 108.6 . . ? C28 C31 H31B 108.6 . . ? H31A C31 H31B 107.6 . . ? C35 C32 C33 104.8(2) . . ? C35 C32 C31 131.5(2) . . ? C33 C32 C31 123.7(2) . . ? N4 C33 C32 111.5(2) . . ? N4 C33 C34 121.0(2) . . ? C32 C33 C34 127.6(2) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 O4 109.6(2) . . ? C32 C35 C36 136.9(2) . . ? O4 C35 C36 113.5(2) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 H37A 109.5 . . ? C38 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C38 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O5 C38 C39 111.2(3) . . ? O5 C38 C37 116.6(3) . . ? C39 C38 C37 132.1(3) . . ? C38 C39 C40 104.5(3) . . ? C38 C39 C42 127.9(3) . . ? C40 C39 C42 127.5(3) . . ? N5 C40 C39 111.9(3) . . ? N5 C40 C41 118.7(3) . . ? C39 C40 C41 129.4(3) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C39 C42 C43 116.1(2) . . ? C39 C42 H42A 108.3 . . ? C43 C42 H42A 108.3 . . ? C39 C42 H42B 108.3 . . ? C43 C42 H42B 108.3 . . ? H42A C42 H42B 107.4 . . ? C44 C43 C45 117.9(2) . 2_666 ? C44 C43 C42 119.4(2) . . ? C45 C43 C42 122.7(2) 2_666 . ? C45 C44 C43 121.6(2) . . ? C45 C44 H44 119.2 . . ? C43 C44 H44 119.2 . . ? C44 C45 C43 120.5(2) . 2_666 ? C44 C45 H45 119.8 . . ? C43 C45 H45 119.8 2_666 . ? 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 C2 O1 N1 C4 -0.2(3) . . . . ? C2 O1 N1 Ag1 159.63(18) . . . . ? N2 Ag1 N1 C4 -49.1(3) 2_666 . . . ? N3 Ag1 N1 C4 176.0(2) . . . . ? N4 Ag1 N1 C4 64.7(3) 2_455 . . . ? N2 Ag1 N1 O1 159.06(15) 2_666 . . . ? N3 Ag1 N1 O1 24.18(19) . . . . ? N4 Ag1 N1 O1 -87.11(17) 2_455 . . . ? C15 O2 N2 C17 0.1(3) . . . . ? C15 O2 N2 Ag1 -165.82(15) . . . 2_666 ? C22 O3 N3 C20 -0.3(2) . . . . ? C22 O3 N3 Ag1 -178.78(15) . . . . ? N2 Ag1 N3 C20 169.8(2) 2_666 . . . ? N1 Ag1 N3 C20 -54.7(3) . . . . ? N4 Ag1 N3 C20 53.4(3) 2_455 . . . ? N2 Ag1 N3 O3 -12.25(19) 2_666 . . . ? N1 Ag1 N3 O3 123.26(16) . . . . ? N4 Ag1 N3 O3 -128.63(16) 2_455 . . . ? C35 O4 N4 C33 0.2(3) . . . . ? C35 O4 N4 Ag1 -179.65(15) . . . 2_455 ? C38 O5 N5 C40 -0.5(3) . . . . ? N1 O1 C2 C3 0.7(3) . . . . ? N1 O1 C2 C1 -179.1(3) . . . . ? O1 C2 C3 C4 -0.8(3) . . . . ? C1 C2 C3 C4 178.9(4) . . . . ? O1 C2 C3 C6 -177.7(3) . . . . ? C1 C2 C3 C6 2.0(6) . . . . ? O1 N1 C4 C3 -0.3(3) . . . . ? Ag1 N1 C4 C3 -153.4(2) . . . . ? O1 N1 C4 C5 179.4(2) . . . . ? Ag1 N1 C4 C5 26.3(4) . . . . ? C2 C3 C4 N1 0.7(3) . . . . ? C6 C3 C4 N1 177.6(2) . . . . ? C2 C3 C4 C5 -178.9(3) . . . . ? C6 C3 C4 C5 -2.0(4) . . . . ? C2 C3 C6 C7 -126.2(3) . . . . ? C4 C3 C6 C7 57.5(4) . . . . ? C3 C6 C7 C12 -122.9(3) . . . . ? C3 C6 C7 C8 59.4(4) . . . . ? C12 C7 C8 C9 -0.9(4) . . . . ? C6 C7 C8 C9 176.8(2) . . . . ? C7 C8 C9 C10 0.2(4) . . . . ? C8 C9 C10 C11 0.1(4) . . . . ? C8 C9 C10 C13 -178.2(2) . . . . ? C9 C10 C11 C12 0.2(4) . . . . ? C13 C10 C11 C12 178.5(3) . . . . ? C8 C7 C12 C11 1.2(4) . . . . ? C6 C7 C12 C11 -176.6(3) . . . . ? C10 C11 C12 C7 -0.9(4) . . . . ? C11 C10 C13 C14 103.6(3) . . . . ? C9 C10 C13 C14 -78.2(3) . . . . ? C10 C13 C14 C15 95.2(3) . . . . ? C10 C13 C14 C17 -86.2(3) . . . . ? C17 C14 C15 O2 0.0(3) . . . . ? C13 C14 C15 O2 178.8(2) . . . . ? C17 C14 C15 C16 -178.7(3) . . . . ? C13 C14 C15 C16 0.1(5) . . . . ? N2 O2 C15 C14 -0.1(3) . . . . ? N2 O2 C15 C16 178.9(2) . . . . ? O2 N2 C17 C14 -0.1(3) . . . . ? Ag1 N2 C17 C14 161.18(19) 2_666 . . . ? O2 N2 C17 C18 -178.5(2) . . . . ? Ag1 N2 C17 C18 -17.2(4) 2_666 . . . ? C15 C14 C17 N2 0.0(3) . . . . ? C13 C14 C17 N2 -178.8(2) . . . . ? C15 C14 C17 C18 178.3(3) . . . . ? C13 C14 C17 C18 -0.6(4) . . . . ? O3 N3 C20 C21 -0.4(3) . . . . ? Ag1 N3 C20 C21 177.75(17) . . . . ? O3 N3 C20 C19 178.6(2) . . . . ? Ag1 N3 C20 C19 -3.2(4) . . . . ? N3 C20 C21 C22 0.9(3) . . . . ? C19 C20 C21 C22 -178.0(3) . . . . ? N3 C20 C21 C24 -175.7(2) . . . . ? C19 C20 C21 C24 5.3(4) . . . . ? C20 C21 C22 O3 -1.1(3) . . . . ? C24 C21 C22 O3 175.5(2) . . . . ? C20 C21 C22 C23 177.2(3) . . . . ? C24 C21 C22 C23 -6.2(5) . . . . ? N3 O3 C22 C21 0.9(3) . . . . ? N3 O3 C22 C23 -177.8(2) . . . . ? C22 C21 C24 C25 112.3(3) . . . . ? C20 C21 C24 C25 -71.8(3) . . . . ? C21 C24 C25 C26 132.1(2) . . . . ? C21 C24 C25 C30 -51.1(3) . . . . ? C30 C25 C26 C27 -1.6(4) . . . . ? C24 C25 C26 C27 175.3(2) . . . . ? C25 C26 C27 C28 0.5(4) . . . . ? C26 C27 C28 C29 0.4(4) . . . . ? C26 C27 C28 C31 178.8(2) . . . . ? C27 C28 C29 C30 -0.2(4) . . . . ? C31 C28 C29 C30 -178.6(2) . . . . ? C28 C29 C30 C25 -0.9(4) . . . . ? C26 C25 C30 C29 1.8(4) . . . . ? C24 C25 C30 C29 -175.1(2) . . . . ? C27 C28 C31 C32 -91.5(3) . . . . ? C29 C28 C31 C32 86.8(3) . . . . ? C28 C31 C32 C35 -7.7(4) . . . . ? C28 C31 C32 C33 174.7(2) . . . . ? O4 N4 C33 C32 0.6(3) . . . . ? Ag1 N4 C33 C32 -179.55(18) 2_455 . . . ? O4 N4 C33 C34 -179.2(2) . . . . ? Ag1 N4 C33 C34 0.7(4) 2_455 . . . ? C35 C32 C33 N4 -1.2(3) . . . . ? C31 C32 C33 N4 177.0(2) . . . . ? C35 C32 C33 C34 178.5(2) . . . . ? C31 C32 C33 C34 -3.3(4) . . . . ? C33 C32 C35 O4 1.3(3) . . . . ? C31 C32 C35 O4 -176.7(3) . . . . ? C33 C32 C35 C36 -179.0(3) . . . . ? C31 C32 C35 C36 3.0(5) . . . . ? N4 O4 C35 C32 -1.0(3) . . . . ? N4 O4 C35 C36 179.2(2) . . . . ? N5 O5 C38 C39 0.5(3) . . . . ? N5 O5 C38 C37 -177.8(2) . . . . ? O5 C38 C39 C40 -0.3(3) . . . . ? C37 C38 C39 C40 177.7(3) . . . . ? O5 C38 C39 C42 -178.2(2) . . . . ? C37 C38 C39 C42 -0.3(5) . . . . ? O5 N5 C40 C39 0.4(3) . . . . ? O5 N5 C40 C41 -179.6(2) . . . . ? C38 C39 C40 N5 -0.1(3) . . . . ? C42 C39 C40 N5 177.9(3) . . . . ? C38 C39 C40 C41 179.9(3) . . . . ? C42 C39 C40 C41 -2.1(5) . . . . ? C38 C39 C42 C43 -108.5(3) . . . . ? C40 C39 C42 C43 74.0(4) . . . . ? C39 C42 C43 C44 -170.9(3) . . . . ? C39 C42 C43 C45 10.5(4) . . . 2_666 ? C45 C43 C44 C45 1.0(5) 2_666 . . . ? C42 C43 C44 C45 -177.6(3) . . . . ? C43 C44 C45 C43 -1.0(5) . . . 2_666 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.608 _refine_diff_density_min -0.959 _refine_diff_density_rms 0.178 #===end data_Compound-9-h08adb01 _database_code_depnum_ccdc_archive 'CCDC 804685' #TrackingRef '- stevenson-rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H40 Ag F6 N4 O4 Sb' _chemical_formula_weight 936.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.7220(3) _cell_length_b 11.4650(2) _cell_length_c 15.4820(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.394(1) _cell_angle_gamma 90.00 _cell_volume 3852.31(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 24070 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 1.281 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_T_max 0.76 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41679 _diffrn_reflns_av_R_equivalents 0.0600 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 30.03 _reflns_number_total 5618 _reflns_number_gt 4492 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (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. The asymmetric unit consists of 1 Ag centre located on a crystallographic 2-fold axis, 2 independent ligand halves (the remainder of each generated via an inversion centre in the middle of the 6-membered ring), 1 half of a hexafluoroantimony anion fragment wherein, the central atom, is located at an inversion centre. ; _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^)+(0.0394P)^2^+1.7844P] 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 0.00168(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5618 _refine_ls_number_parameters 242 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0440 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0730 _refine_ls_wR_factor_gt 0.0675 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 Sb1 Sb 1.2500 0.2500 0.5000 0.03365(7) Uani 1 2 d S . . Ag1 Ag 1.5000 0.421228(15) 0.2500 0.02381(7) Uani 1 2 d S . . F1 F 1.21540(9) 0.34666(17) 0.41441(12) 0.0778(5) Uani 1 1 d . . . F2 F 1.23964(12) 0.12582(17) 0.42432(14) 0.0944(7) Uani 1 1 d . . . F3 F 1.32755(8) 0.2800(2) 0.45959(14) 0.0920(7) Uani 1 1 d . . . O1 O 1.43275(6) 0.18038(11) 0.24139(9) 0.0281(3) Uani 1 1 d . . . O2 O 1.43138(6) 0.53152(11) 0.40520(8) 0.0259(3) Uani 1 1 d . . . N1 N 1.41654(7) 0.29714(13) 0.25559(10) 0.0247(3) Uani 1 1 d . . . N2 N 1.48223(8) 0.55790(13) 0.35550(10) 0.0272(3) Uani 1 1 d . . . C1 C 1.51347(9) 0.63908(15) 0.39727(12) 0.0251(4) Uani 1 1 d . . . C2 C 1.48572(8) 0.66818(14) 0.47575(11) 0.0227(3) Uani 1 1 d . . . C3 C 1.43502(8) 0.59976(15) 0.47685(11) 0.0233(3) Uani 1 1 d . . . C4 C 1.56993(11) 0.68972(19) 0.36065(14) 0.0387(5) Uani 1 1 d . . . H4A H 1.5797 0.6473 0.3080 0.058 Uiso 1 1 calc R . . H4B H 1.6045 0.6831 0.4032 0.058 Uiso 1 1 calc R . . H4C H 1.5627 0.7721 0.3467 0.058 Uiso 1 1 calc R . . C5 C 1.38418(9) 0.58545(18) 0.53677(13) 0.0326(4) Uani 1 1 d . . . H5A H 1.4012 0.5810 0.5963 0.049 Uiso 1 1 calc R . . H5B H 1.3615 0.5136 0.5226 0.049 Uiso 1 1 calc R . . H5C H 1.3562 0.6523 0.5311 0.049 Uiso 1 1 calc R . . C6 C 1.50988(10) 0.75178(14) 0.54372(12) 0.0270(4) Uani 1 1 d . . . H6A H 1.5537 0.7332 0.5575 0.032 Uiso 1 1 calc R . . H6B H 1.4870 0.7393 0.5969 0.032 Uiso 1 1 calc R . . C7 C 1.50502(8) 0.88001(14) 0.51886(11) 0.0231(3) Uani 1 1 d . . . C8 C 1.55168(9) 0.95730(16) 0.54453(13) 0.0296(4) Uani 1 1 d . . . H8 H 1.5875 0.9289 0.5750 0.036 Uiso 1 1 calc R . . C9 C 1.45360(9) 0.92460(15) 0.47394(13) 0.0305(4) Uani 1 1 d . . . H9 H 1.4214 0.8732 0.4555 0.037 Uiso 1 1 calc R . . C10 C 1.35727(8) 0.30459(15) 0.23872(11) 0.0239(3) Uani 1 1 d . . . C11 C 1.33225(9) 0.19494(16) 0.21170(12) 0.0270(4) Uani 1 1 d . . . C12 C 1.38128(9) 0.12184(16) 0.21533(12) 0.0289(4) Uani 1 1 d . . . C13 C 1.32416(10) 0.41694(17) 0.24988(13) 0.0324(4) Uani 1 1 d . . . H13A H 1.3529 0.4755 0.2739 0.049 Uiso 1 1 calc R . . H13B H 1.2906 0.4056 0.2894 0.049 Uiso 1 1 calc R . . H13C H 1.3072 0.4437 0.1937 0.049 Uiso 1 1 calc R . . C14 C 1.39054(12) -0.00460(18) 0.19793(17) 0.0440(5) Uani 1 1 d . . . H14A H 1.4192 -0.0138 0.1511 0.066 Uiso 1 1 calc R . . H14B H 1.3509 -0.0405 0.1810 0.066 Uiso 1 1 calc R . . H14C H 1.4077 -0.0427 0.2503 0.066 Uiso 1 1 calc R . . C15 C 1.26748(9) 0.1707(2) 0.17924(14) 0.0379(5) Uani 1 1 d . . . H15A H 1.2383 0.2114 0.2164 0.045 Uiso 1 1 calc R . . H15B H 1.2593 0.0859 0.1829 0.045 Uiso 1 1 calc R . . C16 C 1.25686(9) 0.21093(17) 0.08631(13) 0.0314(4) Uani 1 1 d . . . C17 C 1.22503(9) 0.31368(18) 0.06563(14) 0.0346(4) Uani 1 1 d . . . H17 H 1.2076 0.3581 0.1104 0.042 Uiso 1 1 calc R . . C18 C 1.28157(9) 0.14812(17) 0.01917(14) 0.0340(4) Uani 1 1 d . . . H18 H 1.3034 0.0779 0.0317 0.041 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 Sb1 0.02860(11) 0.02905(11) 0.04269(13) 0.00963(7) -0.00588(8) -0.00195(7) Ag1 0.03039(11) 0.01840(10) 0.02264(10) 0.000 0.00120(7) 0.000 F1 0.0748(11) 0.0769(12) 0.0798(12) 0.0378(10) -0.0171(9) 0.0121(9) F2 0.1353(19) 0.0601(11) 0.0870(14) -0.0224(10) -0.0054(13) -0.0107(12) F3 0.0395(9) 0.156(2) 0.0805(13) 0.0278(13) 0.0031(9) -0.0192(11) O1 0.0285(7) 0.0213(6) 0.0337(7) 0.0003(5) -0.0057(5) 0.0000(5) O2 0.0293(6) 0.0245(6) 0.0239(6) -0.0057(5) 0.0018(5) -0.0026(5) N1 0.0278(8) 0.0203(7) 0.0258(7) 0.0002(6) -0.0014(6) -0.0011(6) N2 0.0333(8) 0.0240(7) 0.0248(7) -0.0044(6) 0.0059(6) -0.0048(6) C1 0.0330(9) 0.0176(8) 0.0248(8) 0.0002(6) 0.0010(7) -0.0011(7) C2 0.0322(9) 0.0153(7) 0.0203(8) 0.0003(6) -0.0037(7) 0.0034(6) C3 0.0299(9) 0.0193(8) 0.0204(8) -0.0018(6) -0.0022(7) 0.0059(7) C4 0.0459(12) 0.0312(10) 0.0397(11) -0.0030(9) 0.0093(9) -0.0126(9) C5 0.0320(10) 0.0361(10) 0.0299(9) -0.0021(8) 0.0041(8) 0.0031(8) C6 0.0425(11) 0.0175(8) 0.0205(8) -0.0023(6) -0.0054(8) -0.0003(7) C7 0.0315(9) 0.0170(8) 0.0208(8) -0.0037(6) -0.0001(7) 0.0005(7) C8 0.0310(10) 0.0231(9) 0.0339(10) -0.0026(7) -0.0089(8) 0.0027(7) C9 0.0333(10) 0.0210(9) 0.0366(10) -0.0021(7) -0.0079(8) -0.0043(7) C10 0.0270(9) 0.0250(9) 0.0195(8) 0.0029(6) 0.0014(7) -0.0018(7) C11 0.0278(9) 0.0257(9) 0.0271(9) 0.0041(7) -0.0015(7) -0.0069(7) C12 0.0329(10) 0.0240(9) 0.0292(9) 0.0027(7) -0.0047(8) -0.0061(7) C13 0.0329(10) 0.0309(10) 0.0336(10) -0.0024(8) 0.0021(8) 0.0043(8) C14 0.0528(14) 0.0224(9) 0.0558(14) -0.0012(9) -0.0110(11) -0.0009(9) C15 0.0304(10) 0.0423(12) 0.0405(11) 0.0100(9) -0.0038(9) -0.0122(9) C16 0.0234(9) 0.0308(10) 0.0391(11) 0.0027(8) -0.0082(8) -0.0091(8) C17 0.0276(10) 0.0337(10) 0.0420(11) -0.0041(9) -0.0065(8) -0.0016(8) C18 0.0297(10) 0.0252(9) 0.0463(12) 0.0010(8) -0.0103(9) -0.0014(7) _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 Sb1 F2 1.8516(19) 7_756 ? Sb1 F2 1.8516(19) . ? Sb1 F3 1.8535(17) . ? Sb1 F3 1.8535(17) 7_756 ? Sb1 F1 1.8616(15) . ? Sb1 F1 1.8616(15) 7_756 ? Ag1 N2 2.3075(15) . ? Ag1 N2 2.3075(15) 2_855 ? Ag1 N1 2.3089(15) . ? Ag1 N1 2.3089(15) 2_855 ? O1 C12 1.351(2) . ? O1 N1 1.4038(19) . ? O2 C3 1.357(2) . ? O2 N2 1.405(2) . ? N1 C10 1.306(2) . ? N2 C1 1.307(2) . ? C1 C2 1.419(3) . ? C1 C4 1.490(3) . ? C2 C3 1.353(3) . ? C2 C6 1.502(2) . ? C3 C5 1.481(3) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.522(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C9 1.389(3) . ? C7 C8 1.392(3) . ? C8 C9 1.388(3) 5_876 ? C8 H8 0.9500 . ? C9 C8 1.388(3) 5_876 ? C9 H9 0.9500 . ? C10 C11 1.425(2) . ? C10 C13 1.489(3) . ? C11 C12 1.355(3) . ? C11 C15 1.500(3) . ? C12 C14 1.490(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.519(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C18 1.391(3) . ? C16 C17 1.396(3) . ? C17 C18 1.386(3) 7_755 ? C17 H17 0.9500 . ? C18 C17 1.386(3) 7_755 ? C18 H18 0.9500 . ? 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 F2 Sb1 F2 180.000(1) 7_756 . ? F2 Sb1 F3 89.01(12) 7_756 . ? F2 Sb1 F3 90.99(12) . . ? F2 Sb1 F3 90.99(12) 7_756 7_756 ? F2 Sb1 F3 89.01(12) . 7_756 ? F3 Sb1 F3 180.00(4) . 7_756 ? F2 Sb1 F1 91.57(10) 7_756 . ? F2 Sb1 F1 88.43(10) . . ? F3 Sb1 F1 89.69(9) . . ? F3 Sb1 F1 90.31(9) 7_756 . ? F2 Sb1 F1 88.43(10) 7_756 7_756 ? F2 Sb1 F1 91.57(10) . 7_756 ? F3 Sb1 F1 90.31(9) . 7_756 ? F3 Sb1 F1 89.69(9) 7_756 7_756 ? F1 Sb1 F1 180.00(8) . 7_756 ? N2 Ag1 N2 94.46(8) . 2_855 ? N2 Ag1 N1 103.71(5) . . ? N2 Ag1 N1 126.85(6) 2_855 . ? N2 Ag1 N1 126.85(6) . 2_855 ? N2 Ag1 N1 103.71(5) 2_855 2_855 ? N1 Ag1 N1 103.92(7) . 2_855 ? C12 O1 N1 108.10(14) . . ? C3 O2 N2 107.65(13) . . ? C10 N1 O1 106.42(14) . . ? C10 N1 Ag1 136.17(12) . . ? O1 N1 Ag1 112.29(10) . . ? C1 N2 O2 106.63(14) . . ? C1 N2 Ag1 137.30(13) . . ? O2 N2 Ag1 113.58(10) . . ? N2 C1 C2 111.15(16) . . ? N2 C1 C4 120.52(17) . . ? C2 C1 C4 128.33(16) . . ? C3 C2 C1 104.46(15) . . ? C3 C2 C6 128.47(17) . . ? C1 C2 C6 126.99(17) . . ? C2 C3 O2 110.10(16) . . ? C2 C3 C5 134.50(17) . . ? O2 C3 C5 115.39(16) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C2 C6 C7 114.88(15) . . ? C2 C6 H6A 108.5 . . ? C7 C6 H6A 108.5 . . ? C2 C6 H6B 108.5 . . ? C7 C6 H6B 108.5 . . ? H6A C6 H6B 107.5 . . ? C9 C7 C8 118.01(16) . . ? C9 C7 C6 121.87(16) . . ? C8 C7 C6 120.06(16) . . ? C9 C8 C7 120.63(17) 5_876 . ? C9 C8 H8 119.7 5_876 . ? C7 C8 H8 119.7 . . ? C8 C9 C7 121.36(17) 5_876 . ? C8 C9 H9 119.3 5_876 . ? C7 C9 H9 119.3 . . ? N1 C10 C11 111.21(16) . . ? N1 C10 C13 120.70(16) . . ? C11 C10 C13 128.08(17) . . ? C12 C11 C10 104.11(16) . . ? C12 C11 C15 128.60(18) . . ? C10 C11 C15 127.07(18) . . ? O1 C12 C11 110.15(16) . . ? O1 C12 C14 114.90(17) . . ? C11 C12 C14 134.95(18) . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 111.35(16) . . ? C11 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? C11 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C18 C16 C17 117.94(19) . . ? C18 C16 C15 120.15(19) . . ? C17 C16 C15 121.8(2) . . ? C18 C17 C16 121.0(2) 7_755 . ? C18 C17 H17 119.5 7_755 . ? C16 C17 H17 119.5 . . ? C17 C18 C16 121.10(19) 7_755 . ? C17 C18 H18 119.4 7_755 . ? C16 C18 H18 119.4 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.492 _refine_diff_density_min -0.672 _refine_diff_density_rms 0.098 #===end data_Compound-10-k08adb10 _database_code_depnum_ccdc_archive 'CCDC 804686' #TrackingRef '- stevenson-rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H40 Ag F3 N4 O7 S' _chemical_formula_weight 849.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.6760(3) _cell_length_b 11.3410(1) _cell_length_c 15.7510(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.566(1) _cell_angle_gamma 90.00 _cell_volume 3864.53(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 52761 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 0.642 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36623 _diffrn_reflns_av_R_equivalents 0.0648 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 27.52 _reflns_number_total 4424 _reflns_number_gt 3733 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (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. The asymmetric unit consists of 1/2 of a silver atom, two crystallographically independent ligand halves and a 1/2 occupancy anion which presents with 50:50 disorder proximate to an inversion centre. ; _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^)+(0.0000P)^2^+15.1973P] 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 4424 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.0952 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.204 _refine_ls_restrained_S_all 1.204 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.5000 0.07050(3) 0.7500 0.02750(11) Uani 1 2 d S . . S1 S 0.7393(3) 0.2577(6) 0.5606(5) 0.0352(11) Uani 0.50 1 d P . 1 O1 O 0.56870(10) -0.03127(19) 0.59690(13) 0.0291(5) Uani 1 1 d . . . O2 O 0.56780(10) 0.31641(19) 0.75728(14) 0.0324(5) Uani 1 1 d . . . O3 O 0.6785(7) 0.239(3) 0.5561(16) 0.065(6) Uani 0.50 1 d P A 1 O4 O 0.7549(16) 0.363(2) 0.5811(15) 0.075(6) Uani 0.50 1 d P B 1 O5 O 0.7755(7) 0.188(2) 0.6073(13) 0.062(5) Uani 0.50 1 d P C 1 N1 N 0.51763(12) -0.0608(2) 0.64331(16) 0.0305(6) Uani 1 1 d . . . N2 N 0.58296(12) 0.1966(2) 0.74674(16) 0.0278(6) Uani 1 1 d . . . C1 C 0.42979(17) -0.1952(3) 0.6318(2) 0.0428(9) Uani 1 1 d . . . H1A H 0.4186 -0.1522 0.6826 0.064 Uiso 1 1 calc R . . H1B H 0.4379 -0.2779 0.6465 0.064 Uiso 1 1 calc R . . H1C H 0.3957 -0.1906 0.5881 0.064 Uiso 1 1 calc R . . C2 C 0.48627(15) -0.1415(3) 0.5988(2) 0.0288(7) Uani 1 1 d . . . C3 C 0.51475(14) -0.1669(3) 0.52192(19) 0.0262(6) Uani 1 1 d . . . C4 C 0.56536(14) -0.0979(3) 0.52451(19) 0.0268(7) Uani 1 1 d . . . C5 C 0.61659(15) -0.0802(3) 0.4678(2) 0.0374(8) Uani 1 1 d . . . H5A H 0.6441 -0.1488 0.4716 0.056 Uiso 1 1 calc R . . H5B H 0.6399 -0.0093 0.4854 0.056 Uiso 1 1 calc R . . H5C H 0.5997 -0.0708 0.4091 0.056 Uiso 1 1 calc R . . C6 C 0.49147(17) -0.2503(3) 0.4533(2) 0.0319(7) Uani 1 1 d . . . H6A H 0.5156 -0.2382 0.4027 0.038 Uiso 1 1 calc R . . H6B H 0.4478 -0.2309 0.4369 0.038 Uiso 1 1 calc R . . C7 C 0.49553(15) -0.3796(3) 0.47898(19) 0.0278(7) Uani 1 1 d . . . C8 C 0.54836(16) -0.4253(3) 0.5202(2) 0.0379(8) Uani 1 1 d . . . H8 H 0.5822 -0.3744 0.5345 0.045 Uiso 1 1 calc R . . C9 C 0.55315(16) -0.5440(3) 0.5411(2) 0.0374(8) Uani 1 1 d . . . H9 H 0.5900 -0.5731 0.5694 0.045 Uiso 1 1 calc R . . C10 C 0.67459(15) 0.0726(3) 0.7577(2) 0.0356(7) Uani 1 1 d . . . H10A H 0.6451 0.0140 0.7339 0.053 Uiso 1 1 calc R . . H10B H 0.6908 0.0469 0.8141 0.053 Uiso 1 1 calc R . . H10C H 0.7088 0.0808 0.7202 0.053 Uiso 1 1 calc R . . C11 C 0.64282(14) 0.1883(3) 0.76493(19) 0.0273(7) Uani 1 1 d . . . C12 C 0.66879(15) 0.2995(3) 0.7886(2) 0.0322(7) Uani 1 1 d . . . C13 C 0.62056(16) 0.3750(3) 0.7827(2) 0.0344(8) Uani 1 1 d . . . C14 C 0.6120(2) 0.5035(3) 0.7971(3) 0.0541(11) Uani 1 1 d . . . H14A H 0.6522 0.5401 0.8120 0.081 Uiso 1 1 calc R . . H14B H 0.5847 0.5152 0.8436 0.081 Uiso 1 1 calc R . . H14C H 0.5935 0.5399 0.7451 0.081 Uiso 1 1 calc R . . C15 C 0.73434(16) 0.3227(4) 0.8214(2) 0.0436(9) Uani 1 1 d . . . H15A H 0.7437 0.4078 0.8160 0.052 Uiso 1 1 calc R . . H15B H 0.7631 0.2782 0.7869 0.052 Uiso 1 1 calc R . . C16 C 0.74403(15) 0.2857(3) 0.9147(2) 0.0387(8) Uani 1 1 d . . . C17 C 0.72020(16) 0.3541(3) 0.9776(2) 0.0422(9) Uani 1 1 d . . . H17 H 0.6995 0.4258 0.9630 0.051 Uiso 1 1 calc R . . C18 C 0.72636(16) 0.3184(3) 1.0621(2) 0.0407(8) Uani 1 1 d . . . H18 H 0.7100 0.3665 1.1047 0.049 Uiso 1 1 calc R . . F3A F 0.6763(8) 0.209(2) 0.5496(13) 0.074(6) Uani 0.50 1 d P D 2 F4A F 0.7389(14) 0.375(2) 0.5765(15) 0.097(7) Uani 0.50 1 d P E 2 F5A F 0.7738(8) 0.1754(19) 0.5989(13) 0.090(6) Uani 0.50 1 d P F 2 C1A C 0.7338(15) 0.252(3) 0.5444(19) 0.055(8) Uani 0.50 1 d P . 2 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 Ag1 0.03409(19) 0.02403(17) 0.02446(17) 0.000 0.00244(13) 0.000 S1 0.0321(18) 0.043(2) 0.0308(19) 0.0045(14) 0.002(2) -0.0026(14) O1 0.0332(12) 0.0287(11) 0.0257(11) -0.0049(9) 0.0034(9) -0.0028(9) O2 0.0338(12) 0.0246(11) 0.0378(13) 0.0005(10) -0.0044(10) 0.0012(9) O3 0.016(6) 0.114(16) 0.066(7) -0.008(7) 0.012(4) -0.003(6) O4 0.114(13) 0.056(10) 0.054(7) -0.030(6) -0.002(6) -0.011(9) O5 0.039(6) 0.111(12) 0.034(6) 0.020(6) 0.004(4) -0.011(7) N1 0.0384(14) 0.0260(13) 0.0278(13) -0.0062(11) 0.0080(11) -0.0051(12) N2 0.0338(14) 0.0227(13) 0.0267(13) -0.0013(11) -0.0005(11) -0.0012(11) C1 0.052(2) 0.0354(19) 0.042(2) 0.0000(16) 0.0117(17) -0.0117(17) C2 0.0387(17) 0.0203(15) 0.0274(16) -0.0009(12) 0.0012(13) -0.0026(13) C3 0.0366(17) 0.0176(14) 0.0241(15) -0.0005(12) -0.0010(13) 0.0047(13) C4 0.0339(16) 0.0255(16) 0.0208(14) -0.0014(12) -0.0007(12) 0.0069(13) C5 0.0358(17) 0.043(2) 0.0337(18) -0.0017(16) 0.0063(14) 0.0063(16) C6 0.048(2) 0.0226(15) 0.0241(16) -0.0030(12) -0.0045(14) 0.0001(14) C7 0.0416(18) 0.0215(14) 0.0201(15) -0.0040(12) -0.0009(13) 0.0027(13) C8 0.0424(19) 0.0238(16) 0.046(2) -0.0023(15) -0.0089(15) -0.0036(15) C9 0.0411(19) 0.0263(17) 0.043(2) -0.0012(14) -0.0119(16) 0.0023(14) C10 0.0350(17) 0.0347(18) 0.0375(18) 0.0024(16) 0.0055(14) 0.0032(15) C11 0.0304(16) 0.0304(16) 0.0212(15) 0.0010(13) 0.0038(12) -0.0011(13) C12 0.0321(17) 0.0352(18) 0.0289(17) 0.0054(14) -0.0017(13) -0.0078(14) C13 0.0427(19) 0.0263(17) 0.0334(18) 0.0037(14) -0.0056(15) -0.0061(15) C14 0.067(3) 0.0281(19) 0.065(3) -0.0001(18) -0.012(2) -0.0037(18) C15 0.0318(18) 0.049(2) 0.049(2) 0.0111(18) -0.0045(16) -0.0128(16) C16 0.0276(17) 0.040(2) 0.047(2) 0.0047(17) -0.0078(15) -0.0129(15) C17 0.0344(19) 0.0362(19) 0.054(2) 0.0048(17) -0.0130(17) -0.0080(15) C18 0.0338(18) 0.039(2) 0.048(2) 0.0003(17) -0.0079(16) -0.0065(15) F3A 0.066(8) 0.101(10) 0.055(6) 0.018(7) 0.004(4) -0.033(5) F4A 0.151(18) 0.057(6) 0.086(9) 0.003(5) 0.038(9) 0.017(8) F5A 0.110(10) 0.089(9) 0.068(9) 0.037(7) -0.008(6) 0.031(7) C1A 0.072(12) 0.030(7) 0.057(15) 0.004(7) -0.040(8) -0.004(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.295(2) 2_656 ? Ag1 N1 2.295(2) . ? Ag1 N2 2.301(3) . ? Ag1 N2 2.301(3) 2_656 ? S1 O4 1.28(2) . ? S1 O5 1.31(2) . ? S1 O3 1.333(18) . ? S1 S1 1.999(13) 7_656 ? O1 C4 1.366(4) . ? O1 N1 1.404(3) . ? O2 C13 1.361(4) . ? O2 N2 1.410(3) . ? N1 C2 1.316(4) . ? N2 C11 1.315(4) . ? C1 C2 1.489(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.423(4) . ? C3 C4 1.346(4) . ? C3 C6 1.500(4) . ? C4 C5 1.481(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.522(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.382(5) . ? C7 C9 1.387(5) 5_646 ? C8 C9 1.388(5) . ? C8 H8 0.9500 . ? C9 C7 1.387(5) 5_646 ? C9 H9 0.9500 . ? C10 C11 1.489(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.421(4) . ? C12 C13 1.351(5) . ? C12 C15 1.505(4) . ? C13 C14 1.488(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.530(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C18 1.382(5) 7_657 ? C16 C17 1.383(5) . ? C17 C18 1.389(5) . ? C17 H17 0.9500 . ? C18 C16 1.382(5) 7_657 ? C18 H18 0.9500 . ? F3A C1A 1.34(3) . ? F4A C1A 1.48(4) . ? F5A C1A 1.47(4) . ? C1A C1A 1.60(5) 7_656 ? 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 N1 Ag1 N1 99.09(13) 2_656 . ? N1 Ag1 N2 125.85(9) 2_656 . ? N1 Ag1 N2 102.77(9) . . ? N1 Ag1 N2 102.77(9) 2_656 2_656 ? N1 Ag1 N2 125.85(9) . 2_656 ? N2 Ag1 N2 103.14(13) . 2_656 ? O4 S1 O5 106.7(18) . . ? O4 S1 O3 114(2) . . ? O5 S1 O3 119.2(14) . . ? O4 S1 S1 104.5(14) . 7_656 ? O5 S1 S1 108.5(10) . 7_656 ? O3 S1 S1 102.8(13) . 7_656 ? C4 O1 N1 107.5(2) . . ? C13 O2 N2 107.9(2) . . ? C2 N1 O1 106.7(2) . . ? C2 N1 Ag1 137.5(2) . . ? O1 N1 Ag1 113.50(17) . . ? C11 N2 O2 106.1(2) . . ? C11 N2 Ag1 135.5(2) . . ? O2 N2 Ag1 114.08(17) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 110.9(3) . . ? N1 C2 C1 120.5(3) . . ? C3 C2 C1 128.6(3) . . ? C4 C3 C2 104.6(3) . . ? C4 C3 C6 128.7(3) . . ? C2 C3 C6 126.6(3) . . ? C3 C4 O1 110.3(3) . . ? C3 C4 C5 134.5(3) . . ? O1 C4 C5 115.2(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 C7 113.9(3) . . ? C3 C6 H6A 108.8 . . ? C7 C6 H6A 108.8 . . ? C3 C6 H6B 108.8 . . ? C7 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? C8 C7 C9 118.0(3) . 5_646 ? C8 C7 C6 121.3(3) . . ? C9 C7 C6 120.7(3) 5_646 . ? C7 C8 C9 121.6(3) . . ? C7 C8 H8 119.2 . . ? C9 C8 H8 119.2 . . ? C7 C9 C8 120.5(3) 5_646 . ? C7 C9 H9 119.8 5_646 . ? C8 C9 H9 119.8 . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 C12 111.3(3) . . ? N2 C11 C10 120.1(3) . . ? C12 C11 C10 128.6(3) . . ? C13 C12 C11 104.6(3) . . ? C13 C12 C15 128.5(3) . . ? C11 C12 C15 126.6(3) . . ? C12 C13 O2 110.1(3) . . ? C12 C13 C14 135.6(3) . . ? O2 C13 C14 114.4(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 C16 110.6(3) . . ? C12 C15 H15A 109.5 . . ? C16 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? C18 C16 C17 118.6(3) 7_657 . ? C18 C16 C15 121.4(4) 7_657 . ? C17 C16 C15 119.9(3) . . ? C16 C17 C18 120.3(3) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C16 C18 C17 121.1(4) 7_657 . ? C16 C18 H18 119.4 7_657 . ? C17 C18 H18 119.4 . . ? F3A C1A F5A 105(2) . . ? F3A C1A F4A 112(2) . . ? F5A C1A F4A 109(3) . . ? F3A C1A C1A 120(3) . 7_656 ? F5A C1A C1A 103(3) . 7_656 ? F4A C1A C1A 107(3) . 7_656 ? 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 C4 O1 N1 C2 0.0(3) . . . . ? C4 O1 N1 Ag1 -165.74(18) . . . . ? N1 Ag1 N1 C2 65.0(3) 2_656 . . . ? N2 Ag1 N1 C2 -164.9(3) . . . . ? N2 Ag1 N1 C2 -48.1(4) 2_656 . . . ? N1 Ag1 N1 O1 -135.5(2) 2_656 . . . ? N2 Ag1 N1 O1 -5.3(2) . . . . ? N2 Ag1 N1 O1 111.48(19) 2_656 . . . ? C13 O2 N2 C11 -0.6(3) . . . . ? C13 O2 N2 Ag1 159.8(2) . . . . ? N1 Ag1 N2 C11 42.9(3) 2_656 . . . ? N1 Ag1 N2 C11 -68.4(3) . . . . ? N2 Ag1 N2 C11 159.6(3) 2_656 . . . ? N1 Ag1 N2 O2 -109.70(19) 2_656 . . . ? N1 Ag1 N2 O2 138.99(18) . . . . ? N2 Ag1 N2 O2 6.96(14) 2_656 . . . ? O1 N1 C2 C3 -0.7(3) . . . . ? Ag1 N1 C2 C3 159.8(2) . . . . ? O1 N1 C2 C1 178.1(3) . . . . ? Ag1 N1 C2 C1 -21.4(5) . . . . ? N1 C2 C3 C4 1.1(4) . . . . ? C1 C2 C3 C4 -177.6(3) . . . . ? N1 C2 C3 C6 -177.5(3) . . . . ? C1 C2 C3 C6 3.8(5) . . . . ? C2 C3 C4 O1 -1.1(3) . . . . ? C6 C3 C4 O1 177.5(3) . . . . ? C2 C3 C4 C5 178.4(3) . . . . ? C6 C3 C4 C5 -3.1(6) . . . . ? N1 O1 C4 C3 0.7(3) . . . . ? N1 O1 C4 C5 -178.8(3) . . . . ? C4 C3 C6 C7 111.8(4) . . . . ? C2 C3 C6 C7 -69.9(4) . . . . ? C3 C6 C7 C8 -45.9(4) . . . . ? C3 C6 C7 C9 136.4(3) . . . 5_646 ? C9 C7 C8 C9 0.1(6) 5_646 . . . ? C6 C7 C8 C9 -177.7(3) . . . . ? C7 C8 C9 C7 -0.1(6) . . . 5_646 ? O2 N2 C11 C12 0.7(3) . . . . ? Ag1 N2 C11 C12 -153.4(2) . . . . ? O2 N2 C11 C10 -178.2(3) . . . . ? Ag1 N2 C11 C10 27.7(4) . . . . ? N2 C11 C12 C13 -0.5(4) . . . . ? C10 C11 C12 C13 178.3(3) . . . . ? N2 C11 C12 C15 173.8(3) . . . . ? C10 C11 C12 C15 -7.4(5) . . . . ? C11 C12 C13 O2 0.1(4) . . . . ? C15 C12 C13 O2 -174.1(3) . . . . ? C11 C12 C13 C14 -179.9(4) . . . . ? C15 C12 C13 C14 5.9(7) . . . . ? N2 O2 C13 C12 0.3(4) . . . . ? N2 O2 C13 C14 -179.7(3) . . . . ? C13 C12 C15 C16 96.3(4) . . . . ? C11 C12 C15 C16 -76.7(4) . . . . ? C12 C15 C16 C18 102.3(4) . . . 7_657 ? C12 C15 C16 C17 -74.4(4) . . . . ? C18 C16 C17 C18 0.3(5) 7_657 . . . ? C15 C16 C17 C18 177.1(3) . . . . ? C16 C17 C18 C16 -0.3(6) . . . 7_657 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.912 _refine_diff_density_min -0.839 _refine_diff_density_rms 0.144 #===end