# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1691 data_c25 loop_ _publ_author_name 'Quan-Ming Wang' 'Thomas C.W. Mak' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H6 Ag6 F13 N3 O8' _chemical_formula_weight 1226.43 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.4835(10) _cell_length_b 10.0013(7) _cell_length_c 9.9918(7) _cell_angle_alpha 90.00 _cell_angle_beta 106.259(2) _cell_angle_gamma 90.00 _cell_volume 1389.46(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.931 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 4.275 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9031 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 28.01 _reflns_number_total 3346 _reflns_number_gt 2584 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0467P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0036(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3346 _refine_ls_number_parameters 206 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0861 _refine_ls_wR_factor_gt 0.0809 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.967 _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 -0.00151(3) 0.26171(3) 0.05708(4) 0.04574(14) Uani 1 1 d . . . Ag2 Ag -0.00231(3) 0.05792(4) 0.26094(4) 0.04572(14) Uani 1 1 d . . . Ag3 Ag 0.18523(3) 0.49631(4) 0.07270(4) 0.04875(14) Uani 1 1 d . . . F1 F 0.0000 0.5000 0.0000 0.0437(10) Uani 1 2 d S . . C1 C -0.0007(5) 0.0393(5) 0.0388(5) 0.0553(14) Uani 1.08 1 d P . . O1 O -0.1309(3) 0.1965(4) 0.3021(4) 0.0535(10) Uani 1 1 d . . . O2 O -0.1294(3) 0.3554(4) 0.1444(4) 0.0511(9) Uani 1 1 d . . . C2 C -0.1629(4) 0.2937(5) 0.2269(5) 0.0437(12) Uani 1 1 d . . . C3 C -0.2641(5) 0.3427(5) 0.2312(6) 0.075(2) Uani 1 1 d D . . F2 F -0.2752(5) 0.4722(5) 0.2076(8) 0.143(3) Uani 1 1 d D . . F3 F -0.3342(4) 0.2781(7) 0.1399(7) 0.139(2) Uani 1 1 d D . . F4 F -0.2781(5) 0.3242(6) 0.3550(6) 0.129(2) Uani 1 1 d D . . O3 O 0.1275(3) 0.1970(4) 0.4057(4) 0.0495(9) Uani 1 1 d . . . O4 O 0.1285(3) 0.3542(4) 0.2479(4) 0.0506(9) Uani 1 1 d . . . C4 C 0.1621(4) 0.2915(5) 0.3587(5) 0.0411(11) Uani 1 1 d . . . C5 C 0.2618(5) 0.3377(6) 0.4459(5) 0.071(2) Uani 1 1 d D . . F5 F 0.3305(4) 0.2715(8) 0.4103(8) 0.149(3) Uani 1 1 d . . . F6 F 0.2760(5) 0.3155(6) 0.5801(4) 0.137(3) Uani 1 1 d D . . F7 F 0.2775(5) 0.4663(5) 0.4342(5) 0.129(2) Uani 1 1 d D . . N1 N 0.3478(5) 0.5091(8) 0.1444(8) 0.091(2) Uani 1 1 d . . . C6 C 0.4201(7) 0.5440(12) 0.1831(15) 0.141(5) Uani 1 1 d D . . C7 C 0.5187(13) 0.605(3) 0.232(5) 0.245(18) Uani 0.70 1 d PD . . C7' C 0.514(4) 0.524(7) 0.293(9) 0.24(5) Uani 0.30 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0665(3) 0.02609(18) 0.0471(2) 0.00148(15) 0.01981(19) -0.00045(16) Ag2 0.0663(3) 0.0429(2) 0.03080(19) 0.00127(15) 0.01815(17) -0.00177(18) Ag3 0.0486(3) 0.0477(3) 0.0494(3) -0.00119(17) 0.01270(18) -0.00335(18) F1 0.061(3) 0.034(2) 0.038(2) -0.0001(16) 0.0169(19) 0.0007(18) C1 0.093(4) 0.039(3) 0.039(2) -0.0120(19) 0.027(3) -0.002(3) O1 0.065(3) 0.047(2) 0.053(2) 0.0126(18) 0.0233(19) 0.0054(18) O2 0.058(2) 0.049(2) 0.052(2) 0.0110(17) 0.0236(18) 0.0075(17) C2 0.048(3) 0.042(3) 0.043(3) -0.002(2) 0.016(2) -0.002(2) C3 0.078(5) 0.071(4) 0.090(5) 0.028(4) 0.048(4) 0.023(4) F2 0.165(6) 0.096(4) 0.215(7) 0.069(4) 0.133(5) 0.083(4) F3 0.061(3) 0.195(7) 0.156(6) 0.026(5) 0.022(3) 0.013(4) F4 0.159(5) 0.133(5) 0.143(5) 0.045(4) 0.120(4) 0.060(4) O3 0.052(2) 0.046(2) 0.047(2) 0.0111(16) 0.0094(17) -0.0036(17) O4 0.054(2) 0.047(2) 0.048(2) 0.0079(17) 0.0095(17) -0.0052(17) C4 0.048(3) 0.038(2) 0.037(2) 0.001(2) 0.012(2) -0.001(2) C5 0.067(5) 0.073(4) 0.060(4) 0.015(3) -0.002(3) -0.022(4) F5 0.055(3) 0.175(6) 0.203(7) -0.019(5) 0.013(4) 0.002(3) F6 0.147(5) 0.163(5) 0.065(3) 0.027(3) -0.030(3) -0.086(4) F7 0.148(5) 0.094(3) 0.111(4) 0.013(3) -0.020(4) -0.073(4) N1 0.056(4) 0.111(5) 0.099(5) -0.008(4) 0.012(3) -0.006(4) C6 0.050(6) 0.163(11) 0.200(13) -0.066(9) 0.018(6) 0.009(6) C7 0.062(12) 0.21(3) 0.44(5) -0.08(3) 0.05(2) -0.049(16) C7' 0.07(3) 0.17(6) 0.42(12) -0.03(6) -0.04(5) -0.06(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 C1 2.232(5) . ? Ag1 O2 2.444(4) . ? Ag1 F1 2.4520(4) . ? Ag1 O4 2.455(4) . ? Ag1 Ag2 2.8838(5) . ? Ag2 C1 2.234(5) . ? Ag2 O1 2.447(4) . ? Ag2 F1 2.4490(4) 2_545 ? Ag2 O3 2.458(4) . ? Ag3 N1 2.265(7) . ? Ag3 O3 2.537(3) 4_565 ? Ag3 O4 2.562(4) . ? Ag3 O2 2.565(4) 3_565 ? Ag3 F1 2.5759(5) . ? Ag3 O1 2.596(4) 2 ? F1 Ag2 2.4490(4) 2 ? F1 Ag2 2.4490(4) 4_565 ? F1 Ag1 2.4520(4) 3_565 ? F1 Ag3 2.5759(5) 3_565 ? C1 C1 1.108(9) 3 ? O1 C2 1.238(6) . ? O1 Ag3 2.596(4) 2_545 ? O2 C2 1.232(6) . ? O2 Ag3 2.565(4) 3_565 ? C2 C3 1.557(8) . ? C3 F2 1.319(4) . ? C3 F4 1.321(4) . ? C3 F3 1.328(5) . ? O3 C4 1.223(6) . ? O3 Ag3 2.537(3) 4_566 ? O4 C4 1.247(6) . ? C4 C5 1.535(8) . ? C5 F7 1.317(4) . ? C5 F6 1.318(4) . ? C5 F5 1.324(10) . ? N1 C6 1.068(11) . ? C6 C7 1.502(9) . ? C6 C7' 1.503(10) . ? C7 C7' 1.03(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ag1 O2 115.64(19) . . ? C1 Ag1 F1 161.61(13) . . ? O2 Ag1 F1 76.56(9) . . ? C1 Ag1 O4 114.77(18) . . ? O2 Ag1 O4 94.08(14) . . ? F1 Ag1 O4 76.08(8) . . ? C1 Ag1 Ag2 49.81(13) . . ? O2 Ag1 Ag2 82.26(9) . . ? F1 Ag1 Ag2 148.570(19) . . ? O4 Ag1 Ag2 82.62(8) . . ? C1 Ag2 O1 115.74(18) . . ? C1 Ag2 F1 161.48(13) . 2_545 ? O1 Ag2 F1 76.89(9) . 2_545 ? C1 Ag2 O3 114.39(18) . . ? O1 Ag2 O3 94.23(14) . . ? F1 Ag2 O3 76.15(9) 2_545 . ? C1 Ag2 Ag1 49.76(13) . . ? O1 Ag2 Ag1 82.66(8) . . ? F1 Ag2 Ag1 148.697(19) 2_545 . ? O3 Ag2 Ag1 82.07(8) . . ? N1 Ag3 O3 111.9(2) . 4_565 ? N1 Ag3 O4 108.6(2) . . ? O3 Ag3 O4 85.26(12) 4_565 . ? N1 Ag3 O2 106.8(2) . 3_565 ? O3 Ag3 O2 85.21(12) 4_565 3_565 ? O4 Ag3 O2 144.40(13) . 3_565 ? N1 Ag3 F1 175.47(19) . . ? O3 Ag3 F1 72.56(9) 4_565 . ? O4 Ag3 F1 72.09(9) . . ? O2 Ag3 F1 72.32(9) 3_565 . ? N1 Ag3 O1 103.4(2) . 2 ? O3 Ag3 O1 144.66(13) 4_565 2 ? O4 Ag3 O1 84.25(13) . 2 ? O2 Ag3 O1 83.99(12) 3_565 2 ? F1 Ag3 O1 72.10(9) . 2 ? Ag2 F1 Ag2 180.0 2 4_565 ? Ag2 F1 Ag1 90.092(14) 2 . ? Ag2 F1 Ag1 89.908(14) 4_565 . ? Ag2 F1 Ag1 89.908(14) 2 3_565 ? Ag2 F1 Ag1 90.092(14) 4_565 3_565 ? Ag1 F1 Ag1 180.000(4) . 3_565 ? Ag2 F1 Ag3 90.022(14) 2 3_565 ? Ag2 F1 Ag3 89.978(14) 4_565 3_565 ? Ag1 F1 Ag3 90.178(14) . 3_565 ? Ag1 F1 Ag3 89.822(14) 3_565 3_565 ? Ag2 F1 Ag3 89.978(14) 2 . ? Ag2 F1 Ag3 90.022(14) 4_565 . ? Ag1 F1 Ag3 89.822(14) . . ? Ag1 F1 Ag3 90.178(14) 3_565 . ? Ag3 F1 Ag3 180.000(19) 3_565 . ? C1 C1 Ag1 139.9(7) 3 . ? C1 C1 Ag2 139.6(7) 3 . ? Ag1 C1 Ag2 80.43(15) . . ? C2 O1 Ag2 121.1(4) . . ? C2 O1 Ag3 141.8(4) . 2_545 ? Ag2 O1 Ag3 89.54(12) . 2_545 ? C2 O2 Ag1 121.8(3) . . ? C2 O2 Ag3 139.9(4) . 3_565 ? Ag1 O2 Ag3 90.61(12) . 3_565 ? O2 C2 O1 130.4(5) . . ? O2 C2 C3 114.3(4) . . ? O1 C2 C3 115.2(5) . . ? F2 C3 F4 105.2(5) . . ? F2 C3 F3 108.9(7) . . ? F4 C3 F3 106.7(6) . . ? F2 C3 C2 111.8(5) . . ? F4 C3 C2 112.0(5) . . ? F3 C3 C2 111.9(5) . . ? C4 O3 Ag2 122.6(3) . . ? C4 O3 Ag3 138.3(3) . 4_566 ? Ag2 O3 Ag3 90.73(12) . 4_566 ? C4 O4 Ag1 121.6(3) . . ? C4 O4 Ag3 140.0(4) . . ? Ag1 O4 Ag3 90.07(12) . . ? O3 C4 O4 129.1(5) . . ? O3 C4 C5 115.9(4) . . ? O4 C4 C5 115.1(4) . . ? F7 C5 F6 105.9(5) . . ? F7 C5 F5 107.7(7) . . ? F6 C5 F5 105.9(6) . . ? F7 C5 C4 113.7(5) . . ? F6 C5 C4 112.3(5) . . ? F5 C5 C4 110.9(5) . . ? C6 N1 Ag3 163.7(9) . . ? N1 C6 C7 175(2) . . ? N1 C6 C7' 145(3) . . ? C7 C6 C7' 40(3) . . ? C7' C7 C6 70.1(15) . . ? C7 C7' C6 70.0(16) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.324 _refine_diff_density_min -0.621 _refine_diff_density_rms 0.145 data_N14 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H4 Ag6 F13 N O10' _chemical_formula_weight 1180.35 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 monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.4455(17) _cell_length_b 9.9378(7) _cell_length_c 9.8962(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.002(2) _cell_angle_gamma 90.00 _cell_volume 2305.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 5.149 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.6628 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17536 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0475 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 0.87 _diffrn_reflns_theta_max 30.04 _reflns_number_total 6532 _reflns_number_gt 3986 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0470P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00121(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6532 _refine_ls_number_parameters 353 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0741 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0996 _refine_ls_wR_factor_gt 0.0867 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.953 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 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 0.25001(2) 0.56533(5) 0.11238(4) 0.04290(14) Uani 1 1 d . . . Ag2 Ag 0.24998(3) 0.73886(4) -0.18121(5) 0.04294(15) Uani 1 1 d . . . Ag3 Ag 0.25005(2) 0.44828(4) -0.36266(4) 0.03929(13) Uani 1 1 d . . . Ag4 Ag 0.25002(3) 0.26440(4) -0.06404(5) 0.03988(14) Uani 1 1 d . . . Ag5 Ag 0.36029(2) 0.50184(5) -0.12074(5) 0.04073(13) Uani 1 1 d . . . Ag6 Ag 0.13969(2) 0.50186(5) -0.12080(5) 0.04089(13) Uani 1 1 d . . . F1 F 0.24990(15) 0.5079(3) -0.1210(3) 0.0323(7) Uani 1 1 d . . . C1 C 0.2500(4) 0.5421(5) 0.3317(6) 0.0436(17) Uani 1 1 d . . . N1 N 0.2503(3) 0.4619(6) 0.4094(5) 0.0614(18) Uani 1 1 d . . . O11 O 0.3304(2) 0.7009(5) 0.0178(4) 0.0457(11) Uani 1 1 d . . . O12 O 0.3295(2) 0.8590(4) 0.1802(4) 0.0450(11) Uani 1 1 d . . . C11 C 0.3516(3) 0.7921(6) 0.0871(5) 0.0332(13) Uani 1 1 d . . . C12 C 0.4129(3) 0.8295(5) 0.0532(5) 0.0525(18) Uani 1 1 d D . . F11 F 0.4277(3) 0.8010(9) -0.0718(6) 0.138(3) Uani 1 1 d D . . F12 F 0.4251(3) 0.9577(5) 0.0707(7) 0.118(2) Uani 1 1 d D . . F13 F 0.4491(3) 0.7664(9) 0.1329(8) 0.146(3) Uani 1 1 d D . . O21 O 0.3259(2) 0.3068(4) -0.2681(4) 0.0432(10) Uani 1 1 d . . . O22 O 0.3259(2) 0.1443(4) -0.4245(4) 0.0436(10) Uani 1 1 d . . . C21 C 0.3453(3) 0.2065(6) -0.3259(5) 0.0344(13) Uani 1 1 d . . . C22 C 0.4017(4) 0.1536(6) -0.2704(6) 0.071(2) Uani 1 1 d D . . F21 F 0.4072(3) 0.1741(7) -0.1400(5) 0.116(2) Uani 1 1 d D . . F22 F 0.4095(3) 0.0235(5) -0.2924(6) 0.114(2) Uani 1 1 d D . . F23 F 0.4452(3) 0.2171(8) -0.3270(8) 0.135(3) Uani 1 1 d D . . O31 O 0.1703(2) 0.6412(4) -0.3199(4) 0.0457(11) Uani 1 1 d . . . O32 O 0.1697(2) 0.7998(5) -0.4813(4) 0.0465(11) Uani 1 1 d . . . C31 C 0.1481(3) 0.7068(6) -0.4127(6) 0.0333(12) Uani 1 1 d . . . C32 C 0.0866(3) 0.6701(5) -0.4469(5) 0.0558(19) Uani 1 1 d D . . F31 F 0.0752(3) 0.5414(5) -0.4293(7) 0.119(2) Uani 1 1 d D . . F32 F 0.0720(3) 0.6974(9) -0.5721(6) 0.147(3) Uani 1 1 d D . . F33 F 0.0505(3) 0.7329(9) -0.3664(8) 0.147(3) Uani 1 1 d D . . O41 O 0.1738(2) 0.3554(4) 0.0746(4) 0.0443(11) Uani 1 1 d . . . O42 O 0.1743(2) 0.1932(4) 0.2318(4) 0.0453(11) Uani 1 1 d . . . C41 C 0.1547(3) 0.2943(6) 0.1748(5) 0.0324(12) Uani 1 1 d . . . C42 C 0.0984(4) 0.3465(6) 0.2292(6) 0.070(2) Uani 1 1 d D . . F41 F 0.0545(3) 0.2843(9) 0.1727(8) 0.135(3) Uani 1 1 d D . . F42 F 0.0913(3) 0.4770(5) 0.2080(6) 0.116(3) Uani 1 1 d D . . F43 F 0.0925(3) 0.3262(6) 0.3595(5) 0.111(2) Uani 1 1 d D . . O1W O 0.4610(3) 0.4731(7) -0.1183(7) 0.092(2) Uani 1 1 d . . . O2W O 0.0394(3) 0.4721(8) -0.1179(7) 0.092(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0614(4) 0.0445(3) 0.0228(2) -0.00346(17) 0.0002(2) 0.0000(2) Ag2 0.0607(4) 0.0229(2) 0.0452(3) 0.00510(17) 0.0005(3) 0.0000(2) Ag3 0.0541(3) 0.0400(2) 0.0238(2) -0.00281(17) 0.0003(2) 0.0003(2) Ag4 0.0557(4) 0.0242(2) 0.0398(3) 0.00124(17) -0.0001(2) 0.0001(2) Ag5 0.0393(3) 0.0418(3) 0.0411(3) -0.00024(19) -0.0011(2) 0.0012(2) Ag6 0.0398(3) 0.0413(3) 0.0416(3) -0.00032(19) 0.0016(2) -0.0017(2) F1 0.0421(19) 0.0259(14) 0.0291(15) 0.0004(12) 0.0007(14) 0.0001(14) C1 0.083(5) 0.020(2) 0.027(3) 0.007(2) 0.000(3) 0.002(3) N1 0.104(6) 0.043(3) 0.037(3) 0.004(2) 0.003(3) 0.001(4) O11 0.046(3) 0.046(3) 0.045(2) -0.014(2) 0.000(2) 0.000(2) O12 0.044(3) 0.046(2) 0.045(2) -0.014(2) 0.005(2) -0.002(2) C11 0.037(4) 0.030(3) 0.032(3) 0.000(2) -0.001(3) -0.002(3) C12 0.055(5) 0.048(4) 0.055(4) -0.007(3) 0.011(4) -0.007(4) F11 0.118(6) 0.193(7) 0.102(4) -0.060(5) 0.071(4) -0.075(6) F12 0.107(5) 0.084(4) 0.163(6) -0.020(4) 0.051(4) -0.054(4) F13 0.051(4) 0.190(8) 0.197(8) 0.078(6) -0.017(5) 0.007(4) O21 0.047(3) 0.040(2) 0.043(2) -0.0120(19) -0.010(2) 0.007(2) O22 0.048(3) 0.043(2) 0.039(2) -0.0084(18) -0.008(2) 0.008(2) C21 0.035(3) 0.035(3) 0.033(3) -0.002(2) 0.000(3) 0.003(3) C22 0.073(6) 0.062(5) 0.079(6) -0.019(4) -0.027(5) 0.015(5) F21 0.144(6) 0.129(5) 0.074(3) -0.030(3) -0.055(4) 0.069(5) F22 0.126(6) 0.084(4) 0.132(5) -0.037(3) -0.060(4) 0.066(4) F23 0.042(4) 0.170(7) 0.192(7) -0.022(6) -0.022(4) 0.010(4) O31 0.050(3) 0.044(2) 0.043(2) 0.0104(19) -0.008(2) -0.001(2) O32 0.051(3) 0.044(2) 0.045(2) 0.014(2) 0.001(2) -0.005(2) C31 0.037(3) 0.028(3) 0.035(3) -0.004(2) 0.000(3) -0.003(3) C32 0.061(5) 0.056(4) 0.051(4) 0.006(3) -0.009(4) -0.004(4) F31 0.112(5) 0.081(4) 0.165(6) 0.024(4) -0.052(4) -0.053(4) F32 0.128(6) 0.210(8) 0.104(4) 0.067(5) -0.077(4) -0.081(6) F33 0.049(4) 0.195(8) 0.195(8) -0.075(7) 0.019(5) 0.004(4) O41 0.047(3) 0.045(2) 0.041(2) 0.0101(19) 0.009(2) 0.007(2) O42 0.051(3) 0.039(2) 0.046(2) 0.0094(19) 0.010(2) 0.012(2) C41 0.036(3) 0.031(3) 0.031(3) -0.002(2) 0.001(2) 0.001(3) C42 0.072(6) 0.069(5) 0.071(5) 0.022(4) 0.023(5) 0.032(5) F41 0.049(4) 0.179(7) 0.179(7) 0.029(6) 0.012(4) 0.008(4) F42 0.136(6) 0.083(4) 0.130(5) 0.038(3) 0.064(4) 0.067(4) F43 0.138(6) 0.124(5) 0.072(3) 0.030(3) 0.056(4) 0.068(4) O1W 0.047(4) 0.108(5) 0.120(5) -0.005(4) -0.002(4) -0.001(4) O2W 0.043(3) 0.119(5) 0.115(5) -0.006(4) 0.005(3) -0.001(4) _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 C1 2.183(6) . ? Ag1 F1 2.379(3) . ? Ag1 O32 2.490(5) 4_576 ? Ag1 O11 2.498(5) . ? Ag1 Ag2 2.8213(6) 4_576 ? Ag1 Ag2 3.3786(6) . ? Ag2 C1 2.181(5) 4_575 ? Ag2 F1 2.371(3) . ? Ag2 O12 2.511(4) 4_575 ? Ag2 O31 2.512(4) . ? Ag2 Ag1 2.8213(6) 4_575 ? Ag3 N1 2.260(5) 1_554 ? Ag3 O42 2.451(4) 4_565 ? Ag3 O21 2.453(4) . ? Ag3 F1 2.464(3) . ? Ag3 Ag4 2.9050(6) 4_565 ? Ag4 N1 2.264(6) 4_565 ? Ag4 O22 2.428(4) 4_566 ? Ag4 O41 2.428(4) . ? Ag4 F1 2.484(3) . ? Ag4 Ag3 2.9050(6) 4_566 ? Ag5 O1W 2.378(6) . ? Ag5 O11 2.507(4) . ? Ag5 O12 2.513(4) 4_575 ? Ag5 O22 2.556(4) 4_566 ? Ag5 O21 2.556(4) . ? Ag6 O2W 2.371(6) . ? Ag6 O32 2.507(4) 4_576 ? Ag6 O31 2.513(4) . ? Ag6 O41 2.549(4) . ? Ag6 O42 2.558(4) 4_565 ? C1 N1 1.108(8) . ? C1 Ag2 2.181(5) 4_576 ? N1 Ag3 2.260(5) 1_556 ? N1 Ag4 2.264(6) 4_566 ? O11 C11 1.241(7) . ? O12 C11 1.248(7) . ? O12 Ag2 2.511(4) 4_576 ? O12 Ag5 2.513(4) 4_576 ? C11 C12 1.521(9) . ? C12 F11 1.316(4) . ? C12 F13 1.317(5) . ? C12 F12 1.317(4) . ? O21 C21 1.236(7) . ? O22 C21 1.242(7) . ? O22 Ag4 2.428(4) 4_565 ? O22 Ag5 2.556(4) 4_565 ? C21 C22 1.526(10) . ? C22 F21 1.313(4) . ? C22 F22 1.323(4) . ? C22 F23 1.324(5) . ? O31 C31 1.241(7) . ? O32 C31 1.253(7) . ? O32 Ag1 2.490(5) 4_575 ? O32 Ag6 2.507(4) 4_575 ? C31 C32 1.526(9) . ? C32 F32 1.314(4) . ? C32 F31 1.317(4) . ? C32 F33 1.319(5) . ? O41 C41 1.246(7) . ? O42 C41 1.241(7) . ? O42 Ag3 2.451(4) 4_566 ? O42 Ag6 2.558(4) 4_566 ? C41 C42 1.517(9) . ? C42 F43 1.313(4) . ? C42 F42 1.324(4) . ? C42 F41 1.325(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ag1 F1 160.04(15) . . ? C1 Ag1 O32 115.3(2) . 4_576 ? F1 Ag1 O32 76.52(12) . 4_576 ? C1 Ag1 O11 115.4(2) . . ? F1 Ag1 O11 76.50(12) . . ? O32 Ag1 O11 98.09(15) 4_576 . ? C1 Ag1 Ag2 49.68(14) . 4_576 ? F1 Ag1 Ag2 150.27(7) . 4_576 ? O32 Ag1 Ag2 84.16(9) 4_576 4_576 ? O11 Ag1 Ag2 84.23(9) . 4_576 ? C1 Ag1 Ag2 155.38(14) . . ? F1 Ag1 Ag2 44.58(6) . . ? O32 Ag1 Ag2 53.50(11) 4_576 . ? O11 Ag1 Ag2 53.32(10) . . ? Ag2 Ag1 Ag2 105.698(15) 4_576 . ? C1 Ag2 F1 162.09(16) 4_575 . ? C1 Ag2 O12 114.7(2) 4_575 4_575 ? F1 Ag2 O12 76.29(12) . 4_575 ? C1 Ag2 O31 114.7(2) 4_575 . ? F1 Ag2 O31 76.28(12) . . ? O12 Ag2 O31 95.97(15) 4_575 . ? C1 Ag2 Ag1 49.74(15) 4_575 4_575 ? F1 Ag2 Ag1 148.17(7) . 4_575 ? O12 Ag2 Ag1 82.62(9) 4_575 4_575 ? O31 Ag2 Ag1 82.59(9) . 4_575 ? C1 Ag2 Ag1 117.34(15) 4_575 . ? F1 Ag2 Ag1 44.75(7) . . ? O12 Ag2 Ag1 105.78(9) 4_575 . ? O31 Ag2 Ag1 105.82(9) . . ? Ag1 Ag2 Ag1 167.081(19) 4_575 . ? N1 Ag3 O42 114.7(2) 1_554 4_565 ? N1 Ag3 O21 114.4(2) 1_554 . ? O42 Ag3 O21 92.93(15) 4_565 . ? N1 Ag3 F1 162.67(15) 1_554 . ? O42 Ag3 F1 76.50(12) 4_565 . ? O21 Ag3 F1 76.61(12) . . ? N1 Ag3 Ag4 50.11(14) 1_554 4_565 ? O42 Ag3 Ag4 81.04(9) 4_565 4_565 ? O21 Ag3 Ag4 81.08(9) . 4_565 ? F1 Ag3 Ag4 147.23(6) . 4_565 ? N1 Ag4 O22 115.8(2) 4_565 4_566 ? N1 Ag4 O41 116.0(2) 4_565 . ? O22 Ag4 O41 94.50(15) 4_566 . ? N1 Ag4 F1 160.22(14) 4_565 . ? O22 Ag4 F1 76.45(12) 4_566 . ? O41 Ag4 F1 76.38(12) . . ? N1 Ag4 Ag3 49.99(13) 4_565 4_566 ? O22 Ag4 Ag3 83.20(10) 4_566 4_566 ? O41 Ag4 Ag3 83.31(10) . 4_566 ? F1 Ag4 Ag3 149.79(7) . 4_566 ? O1W Ag5 O11 111.5(2) . . ? O1W Ag5 O12 111.0(2) . 4_575 ? O11 Ag5 O12 85.09(14) . 4_575 ? O1W Ag5 O22 103.7(2) . 4_566 ? O11 Ag5 O22 86.80(14) . 4_566 ? O12 Ag5 O22 144.86(15) 4_575 4_566 ? O1W Ag5 O21 103.2(2) . . ? O11 Ag5 O21 145.29(15) . . ? O12 Ag5 O21 83.08(14) 4_575 . ? O22 Ag5 O21 84.43(14) 4_566 . ? O2W Ag6 O32 111.7(2) . 4_576 ? O2W Ag6 O31 111.2(2) . . ? O32 Ag6 O31 85.31(14) 4_576 . ? O2W Ag6 O41 103.3(2) . . ? O32 Ag6 O41 86.75(14) 4_576 . ? O31 Ag6 O41 145.06(15) . . ? O2W Ag6 O42 103.1(2) . 4_565 ? O32 Ag6 O42 145.17(15) 4_576 4_565 ? O31 Ag6 O42 83.10(14) . 4_565 ? O41 Ag6 O42 84.29(14) . 4_565 ? Ag2 F1 Ag1 90.67(9) . . ? Ag2 F1 Ag3 89.35(9) . . ? Ag1 F1 Ag3 179.85(18) . . ? Ag2 F1 Ag4 178.55(13) . . ? Ag1 F1 Ag4 90.78(9) . . ? Ag3 F1 Ag4 89.20(9) . . ? N1 C1 Ag2 139.4(5) . 4_576 ? N1 C1 Ag1 140.0(5) . . ? Ag2 C1 Ag1 80.57(18) 4_576 . ? C1 N1 Ag3 137.4(5) . 1_556 ? C1 N1 Ag4 142.7(5) . 4_566 ? Ag3 N1 Ag4 79.90(18) 1_556 4_566 ? C11 O11 Ag1 119.3(4) . . ? C11 O11 Ag5 140.0(4) . . ? Ag1 O11 Ag5 89.46(15) . . ? C11 O12 Ag2 120.3(4) . 4_576 ? C11 O12 Ag5 138.8(4) . 4_576 ? Ag2 O12 Ag5 89.88(13) 4_576 4_576 ? O11 C11 O12 129.0(6) . . ? O11 C11 C12 115.8(5) . . ? O12 C11 C12 115.1(5) . . ? F11 C12 F13 106.9(7) . . ? F11 C12 F12 105.9(6) . . ? F13 C12 F12 103.9(7) . . ? F11 C12 C11 113.9(5) . . ? F13 C12 C11 111.1(5) . . ? F12 C12 C11 114.4(5) . . ? C21 O21 Ag3 123.5(4) . . ? C21 O21 Ag5 139.5(4) . . ? Ag3 O21 Ag5 90.66(14) . . ? C21 O22 Ag4 122.0(4) . 4_565 ? C21 O22 Ag5 139.9(4) . 4_565 ? Ag4 O22 Ag5 90.65(13) 4_565 4_565 ? O21 C21 O22 129.1(6) . . ? O21 C21 C22 115.5(5) . . ? O22 C21 C22 115.4(5) . . ? F21 C22 F22 107.5(6) . . ? F21 C22 F23 105.4(7) . . ? F22 C22 F23 106.8(7) . . ? F21 C22 C21 112.7(6) . . ? F22 C22 C21 113.4(6) . . ? F23 C22 C21 110.6(6) . . ? C31 O31 Ag2 120.9(4) . . ? C31 O31 Ag6 138.6(4) . . ? Ag2 O31 Ag6 89.84(13) . . ? C31 O32 Ag1 120.0(4) . 4_575 ? C31 O32 Ag6 139.9(4) . 4_575 ? Ag1 O32 Ag6 89.66(14) 4_575 4_575 ? O31 C31 O32 128.3(6) . . ? O31 C31 C32 115.8(5) . . ? O32 C31 C32 116.0(5) . . ? F32 C32 F31 105.8(6) . . ? F32 C32 F33 107.7(7) . . ? F31 C32 F33 104.5(7) . . ? F32 C32 C31 113.9(6) . . ? F31 C32 C31 113.2(5) . . ? F33 C32 C31 111.1(5) . . ? C41 O41 Ag4 122.2(4) . . ? C41 O41 Ag6 140.3(4) . . ? Ag4 O41 Ag6 90.86(13) . . ? C41 O42 Ag3 124.0(4) . 4_566 ? C41 O42 Ag6 139.1(4) . 4_566 ? Ag3 O42 Ag6 90.73(14) 4_566 4_566 ? O42 C41 O41 128.6(6) . . ? O42 C41 C42 115.9(5) . . ? O41 C41 C42 115.3(5) . . ? F43 C42 F42 107.0(6) . . ? F43 C42 F41 105.1(7) . . ? F42 C42 F41 106.9(7) . . ? F43 C42 C41 112.8(6) . . ? F42 C42 C41 112.9(6) . . ? F41 C42 C41 111.5(6) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.972 _refine_diff_density_min -0.984 _refine_diff_density_rms 0.157