Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_p97 _database_code_CSD 192176 _journal_coden_Cambridge 182 loop_ _publ_author_name 'Quan-Ming Wang' 'Thomas C. W. Mak' _publ_contact_author_name 'Prof Thomas C. W. Mak' _publ_contact_author_address ; Chemistry The Chinese University of Hong Kong Shatin, New Territories Hong Kong SAR 852 CHINA ; _publ_contact_author_email 'TCWMAK@CUHK.EDU.HK' _publ_requested_journal 'Chemical Communications' _publ_section_title ; A novel organometallic columnar complex containing endohedral silver(I)-ethynediyl binding and exterior silver(I)-aromatic interaction ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H16 Ag7 F18 N O12' _chemical_formula_weight 1607.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.6465(16) _cell_length_b 18.708(3) _cell_length_c 23.258(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.049(3) _cell_angle_gamma 90.00 _cell_volume 3704.4(12) _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 prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.882 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3016 _exptl_absorpt_coefficient_mu 3.773 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.568 _exptl_absorpt_correction_T_max 1.000 _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 24840 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 28.04 _reflns_number_total 8964 _reflns_number_gt 6599 _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^)+(0.0728P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8964 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0600 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.1210 _refine_ls_wR_factor_gt 0.1143 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 0.50800(4) -0.07431(2) 0.008386(19) 0.03589(11) Uani 1 1 d . . . Ag2 Ag 0.20201(5) -0.12992(2) 0.033913(19) 0.04025(12) Uani 1 1 d . . . Ag3 Ag -0.03465(7) -0.03266(4) -0.06086(2) 0.06644(18) Uani 1 1 d . . . Ag4 Ag 0.22223(6) 0.03050(3) -0.11037(2) 0.05523(15) Uani 1 1 d . . . Ag5 Ag 0.36668(6) -0.02825(2) 0.11468(2) 0.04543(13) Uani 1 1 d . . . Ag6 Ag 0.15773(5) 0.13918(2) -0.02377(2) 0.04743(13) Uani 1 1 d . . . Ag7 Ag 0.38322(6) -0.25741(3) -0.02228(3) 0.05779(15) Uani 1 1 d . . . C1 C 0.2726(6) -0.0207(3) 0.0159(2) 0.0377(12) Uani 1 1 d . . . C2 C 0.2231(6) 0.0314(3) -0.0117(3) 0.0389(12) Uani 1 1 d . . . C11 C 0.0303(7) -0.2750(3) 0.0498(3) 0.0418(13) Uani 1 1 d . . . C12 C 0.0289(8) -0.3539(4) 0.0660(4) 0.061(2) Uani 1 1 d . . . C21 C 0.1584(7) -0.1252(3) 0.1688(3) 0.0437(13) Uani 1 1 d . . . C22 C 0.1026(8) -0.1745(4) 0.2138(3) 0.0589(18) Uani 1 1 d . . . C31 C 0.5752(6) -0.1788(3) 0.1141(2) 0.0377(12) Uani 1 1 d . . . C32 C 0.5722(8) -0.2474(3) 0.1510(3) 0.0478(14) Uani 1 1 d . . . C41 C 0.5559(6) 0.1245(3) 0.1227(3) 0.0361(12) Uani 1 1 d . . . C42 C 0.6003(8) 0.1762(3) 0.1738(3) 0.0482(14) Uani 1 1 d . . . C51 C 0.0541(7) -0.2182(3) -0.0861(3) 0.0446(13) Uani 1 1 d . . . C52 C -0.0997(8) -0.2314(4) -0.1282(3) 0.0553(16) Uani 1 1 d . . . C61 C -0.0451(7) -0.0366(3) -0.1965(3) 0.0431(13) Uani 1 1 d . . . C62 C -0.1226(8) -0.0604(4) -0.2589(3) 0.0515(15) Uani 1 1 d . . . O11 O 0.1592(5) -0.2465(2) 0.0543(2) 0.0471(10) Uani 1 1 d . . . O12 O -0.1021(5) -0.2498(2) 0.0329(2) 0.0576(12) Uani 1 1 d . . . O21 O 0.0670(5) -0.1180(3) 0.12250(19) 0.0529(11) Uani 1 1 d . . . O22 O 0.2912(5) -0.0984(3) 0.1848(2) 0.0563(12) Uani 1 1 d . . . O31 O 0.5348(5) -0.1859(2) 0.06010(17) 0.0467(10) Uani 1 1 d . . . O32 O 0.6163(5) -0.1235(2) 0.14115(19) 0.0479(10) Uani 1 1 d . . . O41 O 0.5269(5) 0.1507(2) 0.07262(18) 0.0450(9) Uani 1 1 d . . . O42 O 0.5566(5) 0.0603(2) 0.1366(2) 0.0500(10) Uani 1 1 d . . . O51 O 0.0748(6) -0.1582(3) -0.0646(2) 0.0637(13) Uani 1 1 d . . . O52 O 0.1447(5) -0.2698(3) -0.0800(2) 0.0557(11) Uani 1 1 d . . . O61 O 0.0840(5) -0.0079(3) -0.1950(2) 0.0577(12) Uani 1 1 d . . . O62 O -0.1219(5) -0.0489(2) -0.15760(19) 0.0522(11) Uani 1 1 d . . . F11 F 0.0029(10) -0.3947(3) 0.0188(3) 0.138(3) Uani 1 1 d . . . F12 F -0.0780(7) -0.3710(3) 0.0954(4) 0.135(3) Uani 1 1 d . . . F13 F 0.1597(6) -0.3772(3) 0.0970(3) 0.111(2) Uani 1 1 d . . . F21 F 0.1422(12) -0.2381(3) 0.2083(4) 0.176(4) Uani 1 1 d . . . F22 F -0.0433(7) -0.1726(5) 0.2126(4) 0.150(3) Uani 1 1 d . . . F23 F 0.1564(10) -0.1582(5) 0.2672(3) 0.157(3) Uani 1 1 d . . . F31 F 0.4556(19) -0.2889(8) 0.1303(6) 0.091(4) Uani 0.60 1 d P . . F32 F 0.568(4) -0.2376(9) 0.2040(7) 0.112(9) Uani 0.60 1 d P . . F33 F 0.7001(13) -0.2846(7) 0.1489(8) 0.099(5) Uani 0.60 1 d P . . F31' F 0.432(3) -0.2515(14) 0.1634(19) 0.132(9) Uani 0.40 1 d P . . F32' F 0.643(5) -0.2402(18) 0.2015(10) 0.129(16) Uani 0.40 1 d P . . F33' F 0.590(6) -0.3047(8) 0.1266(10) 0.136(11) Uani 0.40 1 d P . . F41 F 0.5275(7) 0.1624(3) 0.2167(2) 0.0992(18) Uani 1 1 d . . . F42 F 0.5670(7) 0.2433(2) 0.1592(2) 0.0873(15) Uani 1 1 d . . . F43 F 0.7512(6) 0.1734(3) 0.1931(3) 0.110(2) Uani 1 1 d . . . F51 F -0.1471(5) -0.2988(2) -0.1258(2) 0.0840(14) Uani 1 1 d . . . F52 F -0.0875(6) -0.2149(3) -0.1822(2) 0.0963(17) Uani 1 1 d . . . F53 F -0.2156(5) -0.1913(3) -0.1142(3) 0.0865(15) Uani 1 1 d . . . F61 F -0.0286(6) -0.0995(3) -0.2836(2) 0.0959(17) Uani 1 1 d . . . F62 F -0.1560(7) -0.0039(3) -0.2936(2) 0.0905(16) Uani 1 1 d . . . F63 F -0.2541(6) -0.0944(4) -0.2604(2) 0.106(2) Uani 1 1 d . . . N1 N 0.1538(7) -0.4531(3) -0.1801(2) 0.0527(13) Uani 1 1 d . . . C01 C 0.5054(8) -0.3991(4) -0.1001(4) 0.066(2) Uani 1 1 d . . . H01A H 0.5371 -0.3969 -0.1363 0.079 Uiso 1 1 calc R . . C02 C 0.5861(10) -0.3604(5) -0.0533(5) 0.079(2) Uani 1 1 d . . . H02A H 0.6684 -0.3308 -0.0591 0.095 Uiso 1 1 calc R . . C03 C 0.5475(9) -0.3650(4) 0.0007(4) 0.067(2) Uani 1 1 d . . . H03A H 0.6052 -0.3405 0.0321 0.081 Uiso 1 1 calc R . . C04 C 0.4224(9) -0.4063(5) 0.0079(3) 0.067(2) Uani 1 1 d . . . H04A H 0.3928 -0.4091 0.0444 0.081 Uiso 1 1 calc R . . C05 C 0.3386(8) -0.4444(4) -0.0388(3) 0.0538(16) Uani 1 1 d . . . H05A H 0.2543 -0.4727 -0.0330 0.065 Uiso 1 1 calc R . . C06 C 0.3784(7) -0.4407(3) -0.0931(3) 0.0441(13) Uani 1 1 d . . . C07 C 0.2971(8) -0.4856(4) -0.1426(3) 0.0557(17) Uani 1 1 d . . . H07A H 0.2659 -0.5302 -0.1266 0.067 Uiso 1 1 calc R . . H07B H 0.3723 -0.4972 -0.1676 0.067 Uiso 1 1 calc R . . C08 C 0.0943(11) -0.5059(5) -0.2269(4) 0.084(3) Uani 1 1 d . . . H08A H 0.0012 -0.4875 -0.2509 0.126 Uiso 1 1 calc R . . H08B H 0.0701 -0.5501 -0.2095 0.126 Uiso 1 1 calc R . . H08C H 0.1733 -0.5141 -0.2505 0.126 Uiso 1 1 calc R . . C09 C 0.0276(9) -0.4411(4) -0.1450(4) 0.0663(19) Uani 1 1 d . . . H09A H -0.0620 -0.4201 -0.1693 0.099 Uiso 1 1 calc R . . H09B H 0.0653 -0.4096 -0.1131 0.099 Uiso 1 1 calc R . . H09C H -0.0020 -0.4860 -0.1301 0.099 Uiso 1 1 calc R . . C010 C 0.1898(14) -0.3841(5) -0.2071(4) 0.106(4) Uani 1 1 d . . . H01B H 0.0948 -0.3643 -0.2288 0.158 Uiso 1 1 calc R . . H01C H 0.2634 -0.3924 -0.2329 0.158 Uiso 1 1 calc R . . H01D H 0.2342 -0.3512 -0.1770 0.158 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 0.0333(2) 0.0295(2) 0.0456(2) 0.00237(16) 0.00887(16) -0.00225(15) Ag2 0.0432(2) 0.0309(2) 0.0448(2) 0.00299(17) 0.00218(18) -0.01103(17) Ag3 0.0585(3) 0.1004(5) 0.0437(3) -0.0035(3) 0.0180(2) 0.0040(3) Ag4 0.0627(3) 0.0635(4) 0.0388(3) -0.0054(2) 0.0069(2) -0.0173(2) Ag5 0.0524(3) 0.0407(3) 0.0398(2) 0.00133(18) -0.00146(19) -0.01001(19) Ag6 0.0419(2) 0.0311(2) 0.0716(3) 0.0107(2) 0.0162(2) 0.00802(17) Ag7 0.0517(3) 0.0404(3) 0.0759(4) -0.0043(2) -0.0039(2) 0.0003(2) C1 0.040(3) 0.032(3) 0.040(3) 0.003(2) 0.006(2) -0.003(2) C2 0.031(3) 0.040(3) 0.045(3) 0.004(2) 0.005(2) -0.001(2) C11 0.051(3) 0.026(3) 0.050(3) 0.005(2) 0.013(3) -0.001(2) C12 0.044(3) 0.033(4) 0.107(6) 0.016(4) 0.018(4) 0.005(3) C21 0.044(3) 0.038(3) 0.052(4) 0.005(3) 0.014(3) 0.007(2) C22 0.052(4) 0.069(5) 0.056(4) 0.021(3) 0.007(3) -0.001(3) C31 0.036(3) 0.039(3) 0.037(3) 0.005(2) 0.005(2) 0.001(2) C32 0.063(4) 0.036(3) 0.042(3) 0.000(2) 0.001(3) 0.001(3) C41 0.033(3) 0.033(3) 0.044(3) -0.003(2) 0.009(2) -0.005(2) C42 0.064(4) 0.039(4) 0.042(3) -0.003(3) 0.008(3) -0.006(3) C51 0.049(3) 0.047(4) 0.038(3) -0.003(3) 0.005(3) -0.002(3) C52 0.050(4) 0.054(4) 0.059(4) -0.008(3) 0.003(3) 0.000(3) C61 0.046(3) 0.039(3) 0.043(3) -0.003(2) 0.001(3) 0.006(2) C62 0.054(4) 0.055(4) 0.043(3) -0.004(3) 0.001(3) -0.010(3) O11 0.049(2) 0.030(2) 0.063(3) 0.0089(18) 0.010(2) -0.0018(17) O12 0.048(2) 0.033(2) 0.091(4) 0.006(2) 0.008(2) 0.0035(18) O21 0.054(3) 0.065(3) 0.037(2) 0.005(2) 0.003(2) -0.003(2) O22 0.045(2) 0.065(3) 0.058(3) 0.017(2) 0.004(2) -0.007(2) O31 0.062(3) 0.038(2) 0.037(2) 0.0038(17) -0.0004(19) -0.0100(19) O32 0.058(3) 0.041(3) 0.046(2) -0.0014(18) 0.010(2) -0.0126(19) O41 0.054(2) 0.038(2) 0.043(2) 0.0003(17) 0.0078(19) -0.0043(18) O42 0.046(2) 0.033(2) 0.066(3) 0.005(2) -0.002(2) -0.0048(17) O51 0.080(3) 0.042(3) 0.058(3) -0.003(2) -0.018(2) -0.007(2) O52 0.048(2) 0.058(3) 0.058(3) -0.009(2) 0.001(2) 0.010(2) O61 0.048(3) 0.073(3) 0.051(3) -0.017(2) 0.006(2) -0.009(2) O62 0.061(3) 0.048(3) 0.048(3) 0.002(2) 0.008(2) -0.005(2) F11 0.217(8) 0.039(3) 0.154(6) -0.019(3) 0.019(6) 0.003(4) F12 0.114(4) 0.066(4) 0.249(9) 0.083(4) 0.103(5) 0.027(3) F13 0.069(3) 0.066(3) 0.193(6) 0.064(4) 0.006(4) 0.013(2) F21 0.301(11) 0.055(4) 0.219(9) 0.057(5) 0.176(9) 0.035(5) F22 0.074(4) 0.211(8) 0.175(7) 0.109(6) 0.053(4) 0.006(4) F23 0.201(8) 0.208(9) 0.059(4) 0.040(4) 0.016(4) -0.071(6) F31 0.105(9) 0.064(8) 0.087(8) 0.037(6) -0.036(7) -0.051(7) F32 0.25(3) 0.043(6) 0.054(9) 0.004(5) 0.068(14) -0.008(11) F33 0.080(6) 0.063(8) 0.153(14) 0.046(8) 0.020(6) 0.025(5) F31' 0.098(13) 0.088(15) 0.23(3) 0.075(16) 0.073(18) -0.006(11) F32' 0.19(3) 0.112(19) 0.058(16) 0.049(15) -0.061(18) -0.034(18) F33' 0.32(4) 0.029(7) 0.084(13) 0.006(7) 0.10(2) 0.019(17) F41 0.169(5) 0.077(4) 0.067(3) -0.013(2) 0.065(3) -0.024(3) F42 0.154(5) 0.035(2) 0.070(3) -0.0095(19) 0.012(3) -0.004(3) F43 0.075(3) 0.129(5) 0.110(4) -0.068(4) -0.029(3) -0.001(3) F51 0.071(3) 0.057(3) 0.116(4) -0.012(3) -0.009(3) -0.019(2) F52 0.092(4) 0.142(5) 0.047(3) 0.001(3) -0.011(2) -0.021(3) F53 0.046(2) 0.082(3) 0.128(4) -0.012(3) 0.006(2) 0.005(2) F61 0.110(4) 0.099(4) 0.073(3) -0.045(3) 0.001(3) 0.017(3) F62 0.117(4) 0.086(4) 0.056(3) 0.016(2) -0.020(3) -0.004(3) F63 0.093(4) 0.151(5) 0.066(3) -0.004(3) -0.008(3) -0.072(4) N1 0.064(3) 0.045(3) 0.047(3) -0.004(2) 0.005(3) -0.008(3) C01 0.058(4) 0.075(5) 0.067(5) -0.012(4) 0.020(4) -0.017(4) C02 0.063(5) 0.066(6) 0.104(7) -0.007(5) 0.003(5) -0.023(4) C03 0.063(4) 0.063(5) 0.065(5) -0.018(4) -0.016(4) 0.025(4) C04 0.066(5) 0.085(6) 0.048(4) -0.003(4) 0.003(3) 0.023(4) C05 0.052(4) 0.061(4) 0.047(4) 0.010(3) 0.006(3) 0.004(3) C06 0.045(3) 0.033(3) 0.054(4) -0.002(3) 0.008(3) 0.003(2) C07 0.057(4) 0.046(4) 0.065(4) -0.011(3) 0.012(3) 0.001(3) C08 0.088(6) 0.092(7) 0.068(5) -0.036(5) 0.002(5) -0.003(5) C09 0.068(5) 0.051(4) 0.076(5) -0.012(4) 0.003(4) 0.003(3) C010 0.145(9) 0.093(7) 0.067(6) 0.032(5) -0.011(6) -0.054(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 Ag1 C1 2.303(6) . ? Ag1 O41 2.342(4) 3_655 ? Ag1 O31 2.400(4) . ? Ag1 C2 2.449(5) 3_655 ? Ag1 Ag1 2.8076(9) 3_655 ? Ag1 Ag2 2.9971(7) . ? Ag1 Ag5 3.0662(8) . ? Ag1 Ag6 3.0973(8) 3_655 ? Ag1 Ag4 3.1318(8) 3_655 ? Ag2 C1 2.194(5) . ? Ag2 O11 2.275(4) . ? Ag2 O51 2.421(5) . ? Ag2 O21 2.549(4) . ? Ag2 Ag5 2.8706(7) . ? Ag2 Ag6 3.0829(8) 3 ? Ag2 Ag7 3.2506(8) . ? Ag2 Ag3 3.2835(8) . ? Ag3 O62 2.265(5) . ? Ag3 O51 2.539(5) . ? Ag3 C2 2.541(6) 3 ? Ag3 C2 2.611(6) . ? Ag3 C1 2.660(6) 3 ? Ag3 Ag4 2.9238(8) . ? Ag3 Ag3 3.0453(12) 3 ? Ag3 Ag6 3.1158(8) 3 ? Ag3 Ag5 3.1390(9) 3 ? Ag4 O61 2.236(4) . ? Ag4 C2 2.295(6) . ? Ag4 O32 2.416(4) 3_655 ? Ag4 Ag6 2.9822(8) . ? Ag4 Ag1 3.1318(8) 3_655 ? Ag5 O22 2.276(4) . ? Ag5 C1 2.304(6) . ? Ag5 O42 2.325(4) . ? Ag5 Ag3 3.1390(9) 3 ? Ag6 C2 2.100(6) . ? Ag6 O12 2.127(4) 3 ? Ag6 Ag2 3.0829(8) 3 ? Ag6 Ag1 3.0973(8) 3_655 ? Ag6 Ag3 3.1158(8) 3 ? Ag7 O52 2.268(4) . ? Ag7 C03 2.468(7) . ? Ag7 O41 2.505(4) 3_655 ? Ag7 O31 2.511(4) . ? C1 C2 1.203(8) . ? C1 Ag3 2.660(6) 3 ? C2 Ag1 2.449(5) 3_655 ? C2 Ag3 2.541(6) 3 ? C11 O11 1.223(7) . ? C11 O12 1.237(7) . ? C11 C12 1.524(8) . ? C12 F12 1.282(8) . ? C12 F13 1.305(8) . ? C12 F11 1.325(11) . ? C21 O21 1.227(7) . ? C21 O22 1.249(7) . ? C21 C22 1.533(9) . ? C22 F21 1.251(10) . ? C22 F22 1.257(8) . ? C22 F23 1.285(10) . ? C31 O32 1.231(7) . ? C31 O31 1.251(7) . ? C31 C32 1.546(8) . ? C32 F32' 1.23(2) . ? C32 F33' 1.235(15) . ? C32 F32 1.251(15) . ? C32 F31 1.297(11) . ? C32 F31' 1.301(17) . ? C32 F33 1.316(12) . ? C41 O42 1.244(7) . ? C41 O41 1.248(7) . ? C41 C42 1.530(8) . ? C42 F41 1.294(7) . ? C42 F43 1.304(8) . ? C42 F42 1.319(8) . ? C51 O51 1.229(8) . ? C51 O52 1.235(8) . ? C51 C52 1.527(9) . ? C52 F52 1.317(9) . ? C52 F51 1.330(8) . ? C52 F53 1.336(8) . ? C61 O61 1.233(7) . ? C61 O62 1.234(7) . ? C61 C62 1.553(9) . ? C62 F63 1.299(8) . ? C62 F61 1.300(8) . ? C62 F62 1.330(8) . ? O12 Ag6 2.127(4) 3 ? O32 Ag4 2.416(4) 3_655 ? O41 Ag1 2.342(4) 3_655 ? O41 Ag7 2.505(4) 3_655 ? F31 F31' 1.09(3) . ? F31 F33' 1.21(3) . ? F32 F32' 0.66(5) . ? F32 F31' 1.40(3) . ? F33 F33' 1.07(4) . ? F33 F32' 1.62(4) . ? N1 C09 1.488(10) . ? N1 C010 1.492(10) . ? N1 C08 1.495(9) . ? N1 C07 1.513(9) . ? C01 C06 1.379(9) . ? C01 C02 1.390(11) . ? C02 C03 1.357(12) . ? C03 C04 1.363(12) . ? C04 C05 1.392(10) . ? C05 C06 1.365(9) . ? C06 C07 1.498(9) . ? 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 O41 109.61(18) . 3_655 ? C1 Ag1 O31 110.51(17) . . ? O41 Ag1 O31 81.94(14) 3_655 . ? C1 Ag1 C2 134.6(2) . 3_655 ? O41 Ag1 C2 102.34(17) 3_655 3_655 ? O31 Ag1 C2 105.16(17) . 3_655 ? C1 Ag1 Ag1 63.66(14) . 3_655 ? O41 Ag1 Ag1 119.76(10) 3_655 3_655 ? O31 Ag1 Ag1 158.28(10) . 3_655 ? C2 Ag1 Ag1 72.72(13) 3_655 3_655 ? C1 Ag1 Ag2 46.67(14) . . ? O41 Ag1 Ag2 87.32(10) 3_655 . ? O31 Ag1 Ag2 67.07(10) . . ? C2 Ag1 Ag2 166.90(14) 3_655 . ? Ag1 Ag1 Ag2 110.33(2) 3_655 . ? C1 Ag1 Ag5 48.28(14) . . ? O41 Ag1 Ag5 143.76(10) 3_655 . ? O31 Ag1 Ag5 81.82(10) . . ? C2 Ag1 Ag5 113.11(14) 3_655 . ? Ag1 Ag1 Ag5 79.45(2) 3_655 . ? Ag2 Ag1 Ag5 56.501(15) . . ? C1 Ag1 Ag6 168.85(14) . 3_655 ? O41 Ag1 Ag6 80.82(10) 3_655 3_655 ? O31 Ag1 Ag6 66.09(10) . 3_655 ? C2 Ag1 Ag6 42.53(14) 3_655 3_655 ? Ag1 Ag1 Ag6 115.24(2) 3_655 3_655 ? Ag2 Ag1 Ag6 132.79(2) . 3_655 ? Ag5 Ag1 Ag6 120.80(2) . 3_655 ? C1 Ag1 Ag4 112.32(14) . 3_655 ? O41 Ag1 Ag4 138.01(10) 3_655 3_655 ? O31 Ag1 Ag4 81.60(10) . 3_655 ? C2 Ag1 Ag4 46.59(14) 3_655 3_655 ? Ag1 Ag1 Ag4 81.85(2) 3_655 3_655 ? Ag2 Ag1 Ag4 120.49(2) . 3_655 ? Ag5 Ag1 Ag4 70.41(2) . 3_655 ? Ag6 Ag1 Ag4 57.204(18) 3_655 3_655 ? C1 Ag2 O11 173.30(18) . . ? C1 Ag2 O51 96.80(19) . . ? O11 Ag2 O51 85.65(16) . . ? C1 Ag2 O21 104.77(19) . . ? O11 Ag2 O21 78.53(15) . . ? O51 Ag2 O21 125.99(17) . . ? C1 Ag2 Ag5 52.04(15) . . ? O11 Ag2 Ag5 125.37(12) . . ? O51 Ag2 Ag5 148.84(12) . . ? O21 Ag2 Ag5 70.00(11) . . ? C1 Ag2 Ag1 49.77(15) . . ? O11 Ag2 Ag1 123.73(10) . . ? O51 Ag2 Ag1 99.17(13) . . ? O21 Ag2 Ag1 132.41(10) . . ? Ag5 Ag2 Ag1 62.963(17) . . ? C1 Ag2 Ag6 110.39(15) . 3 ? O11 Ag2 Ag6 76.31(10) . 3 ? O51 Ag2 Ag6 68.26(13) . 3 ? O21 Ag2 Ag6 57.89(10) . 3 ? Ag5 Ag2 Ag6 117.77(2) . 3 ? Ag1 Ag2 Ag6 156.65(2) . 3 ? C1 Ag2 Ag7 115.91(15) . . ? O11 Ag2 Ag7 59.21(11) . . ? O51 Ag2 Ag7 68.31(13) . . ? O21 Ag2 Ag7 135.23(11) . . ? Ag5 Ag2 Ag7 122.03(2) . . ? Ag1 Ag2 Ag7 70.788(19) . . ? Ag6 Ag2 Ag7 118.599(19) 3 . ? C1 Ag2 Ag3 61.14(15) . . ? O11 Ag2 Ag3 124.46(11) . . ? O51 Ag2 Ag3 50.11(12) . . ? O21 Ag2 Ag3 100.05(10) . . ? Ag5 Ag2 Ag3 104.59(2) . . ? Ag1 Ag2 Ag3 98.22(2) . . ? Ag6 Ag2 Ag3 58.501(17) 3 . ? Ag7 Ag2 Ag3 115.11(2) . . ? O62 Ag3 O51 84.44(16) . . ? O62 Ag3 C2 121.29(17) . 3 ? O51 Ag3 C2 108.52(18) . 3 ? O62 Ag3 C2 127.42(17) . . ? O51 Ag3 C2 98.32(17) . . ? C2 Ag3 C2 107.56(14) 3 . ? O62 Ag3 C1 107.11(17) . 3 ? O51 Ag3 C1 132.78(17) . 3 ? C2 Ag3 C1 26.62(17) 3 3 ? C2 Ag3 C1 108.38(18) . 3 ? O62 Ag3 Ag4 78.90(12) . . ? O51 Ag3 Ag4 92.69(13) . . ? C2 Ag3 Ag4 151.23(13) 3 . ? C2 Ag3 Ag4 48.58(13) . . ? C1 Ag3 Ag4 134.13(12) 3 . ? O62 Ag3 Ag3 162.66(13) . 3 ? O51 Ag3 Ag3 112.90(11) . 3 ? C2 Ag3 Ag3 54.84(13) 3 3 ? C2 Ag3 Ag3 52.72(13) . 3 ? C1 Ag3 Ag3 61.60(12) 3 3 ? Ag4 Ag3 Ag3 99.45(3) . 3 ? O62 Ag3 Ag6 116.76(12) . 3 ? O51 Ag3 Ag6 66.47(13) . 3 ? C2 Ag3 Ag6 42.07(13) 3 3 ? C2 Ag3 Ag6 112.09(13) . 3 ? C1 Ag3 Ag6 67.58(12) 3 3 ? Ag4 Ag3 Ag6 150.92(3) . 3 ? Ag3 Ag3 Ag6 72.72(3) 3 3 ? O62 Ag3 Ag5 61.94(12) . 3 ? O51 Ag3 Ag5 129.97(11) . 3 ? C2 Ag3 Ag5 67.27(13) 3 3 ? C2 Ag3 Ag5 131.25(13) . 3 ? C1 Ag3 Ag5 45.90(12) 3 3 ? Ag4 Ag3 Ag5 113.64(3) . 3 ? Ag3 Ag3 Ag5 104.06(3) 3 3 ? Ag6 Ag3 Ag5 95.43(2) 3 3 ? O62 Ag3 Ag2 130.76(12) . . ? O51 Ag3 Ag2 47.03(10) . . ? C2 Ag3 Ag2 87.50(13) 3 . ? C2 Ag3 Ag2 64.90(13) . . ? C1 Ag3 Ag2 112.23(12) 3 . ? Ag4 Ag3 Ag2 93.50(2) . . ? Ag3 Ag3 Ag2 66.41(3) 3 . ? Ag6 Ag3 Ag2 57.530(19) 3 . ? Ag5 Ag3 Ag2 152.66(2) 3 . ? O61 Ag4 C2 142.29(18) . . ? O61 Ag4 O32 102.60(17) . 3_655 ? C2 Ag4 O32 112.97(17) . 3_655 ? O61 Ag4 Ag3 83.73(12) . . ? C2 Ag4 Ag3 58.59(14) . . ? O32 Ag4 Ag3 157.78(11) 3_655 . ? O61 Ag4 Ag6 132.78(13) . . ? C2 Ag4 Ag6 44.58(15) . . ? O32 Ag4 Ag6 83.98(10) 3_655 . ? Ag3 Ag4 Ag6 76.41(2) . . ? O61 Ag4 Ag1 164.60(12) . 3_655 ? C2 Ag4 Ag1 50.83(13) . 3_655 ? O32 Ag4 Ag1 69.11(11) 3_655 3_655 ? Ag3 Ag4 Ag1 108.91(2) . 3_655 ? Ag6 Ag4 Ag1 60.817(18) . 3_655 ? O22 Ag5 C1 130.91(18) . . ? O22 Ag5 O42 122.22(17) . . ? C1 Ag5 O42 106.72(18) . . ? O22 Ag5 Ag2 85.16(13) . . ? C1 Ag5 Ag2 48.68(14) . . ? O42 Ag5 Ag2 150.00(12) . . ? O22 Ag5 Ag1 128.34(14) . . ? C1 Ag5 Ag1 48.26(14) . . ? O42 Ag5 Ag1 90.65(12) . . ? Ag2 Ag5 Ag1 60.536(18) . . ? O22 Ag5 Ag3 97.96(11) . 3 ? C1 Ag5 Ag3 56.00(14) . 3 ? O42 Ag5 Ag3 113.00(11) . 3 ? Ag2 Ag5 Ag3 70.42(2) . 3 ? Ag1 Ag5 Ag3 104.23(2) . 3 ? C2 Ag6 O12 177.0(2) . 3 ? C2 Ag6 Ag4 50.07(16) . . ? O12 Ag6 Ag4 131.42(14) 3 . ? C2 Ag6 Ag2 101.57(15) . 3 ? O12 Ag6 Ag2 80.77(12) 3 3 ? Ag4 Ag6 Ag2 102.42(2) . 3 ? C2 Ag6 Ag1 52.01(14) . 3_655 ? O12 Ag6 Ag1 125.65(12) 3 3_655 ? Ag4 Ag6 Ag1 61.979(16) . 3_655 ? Ag2 Ag6 Ag1 153.57(2) 3 3_655 ? C2 Ag6 Ag3 54.18(15) . 3 ? O12 Ag6 Ag3 126.10(13) 3 3 ? Ag4 Ag6 Ag3 96.63(2) . 3 ? Ag2 Ag6 Ag3 63.969(17) 3 3 ? Ag1 Ag6 Ag3 95.23(2) 3_655 3 ? O52 Ag7 C03 118.3(2) . . ? O52 Ag7 O41 97.43(16) . 3_655 ? C03 Ag7 O41 122.5(2) . 3_655 ? O52 Ag7 O31 143.71(16) . . ? C03 Ag7 O31 93.7(2) . . ? O41 Ag7 O31 76.63(13) 3_655 . ? O52 Ag7 Ag2 81.98(12) . . ? C03 Ag7 Ag2 144.2(2) . . ? O41 Ag7 Ag2 79.28(10) 3_655 . ? O31 Ag7 Ag2 61.72(10) . . ? C2 C1 Ag2 140.4(5) . . ? C2 C1 Ag1 123.3(4) . . ? Ag2 C1 Ag1 83.56(19) . . ? C2 C1 Ag5 127.8(5) . . ? Ag2 C1 Ag5 79.28(18) . . ? Ag1 C1 Ag5 83.46(19) . . ? C2 C1 Ag3 71.2(4) . 3 ? Ag2 C1 Ag3 90.82(19) . 3 ? Ag1 C1 Ag3 161.4(3) . 3 ? Ag5 C1 Ag3 78.10(17) . 3 ? C1 C2 Ag6 155.7(5) . . ? C1 C2 Ag4 117.8(5) . . ? Ag6 C2 Ag4 85.3(2) . . ? C1 C2 Ag1 90.1(4) . 3_655 ? Ag6 C2 Ag1 85.46(19) . 3_655 ? Ag4 C2 Ag1 82.57(18) . 3_655 ? C1 C2 Ag3 82.2(4) . 3 ? Ag6 C2 Ag3 83.75(19) . 3 ? Ag4 C2 Ag3 140.7(2) . 3 ? Ag1 C2 Ag3 133.7(3) 3_655 3 ? C1 C2 Ag3 93.4(4) . . ? Ag6 C2 Ag3 101.1(2) . . ? Ag4 C2 Ag3 72.84(16) . . ? Ag1 C2 Ag3 153.8(3) 3_655 . ? Ag3 C2 Ag3 72.44(14) 3 . ? O11 C11 O12 129.8(5) . . ? O11 C11 C12 116.6(5) . . ? O12 C11 C12 113.6(5) . . ? F12 C12 F13 105.0(7) . . ? F12 C12 F11 105.3(7) . . ? F13 C12 F11 105.6(7) . . ? F12 C12 C11 114.3(6) . . ? F13 C12 C11 114.6(6) . . ? F11 C12 C11 111.1(7) . . ? O21 C21 O22 129.5(6) . . ? O21 C21 C22 115.7(6) . . ? O22 C21 C22 114.8(6) . . ? F21 C22 F22 108.4(8) . . ? F21 C22 F23 105.3(8) . . ? F22 C22 F23 101.9(8) . . ? F21 C22 C21 112.2(7) . . ? F22 C22 C21 113.8(6) . . ? F23 C22 C21 114.4(7) . . ? O32 C31 O31 127.4(5) . . ? O32 C31 C32 116.4(5) . . ? O31 C31 C32 116.2(5) . . ? F32' C32 F33' 117(2) . . ? F32' C32 F32 31(2) . . ? F33' C32 F32 127.4(12) . . ? F32' C32 F31 130.1(17) . . ? F33' C32 F31 57.2(17) . . ? F32 C32 F31 107.5(12) . . ? F32' C32 F31' 97(2) . . ? F33' C32 F31' 104.1(18) . . ? F32 C32 F31' 66.6(17) . . ? F31 C32 F31' 49.5(14) . . ? F32' C32 F33 79.1(19) . . ? F33' C32 F33 49.7(19) . . ? F32 C32 F33 106.4(13) . . ? F31 C32 F33 105.8(10) . . ? F31' C32 F33 143.3(10) . . ? F32' C32 C31 112.6(16) . . ? F33' C32 C31 116.7(9) . . ? F32 C32 C31 115.5(9) . . ? F31 C32 C31 112.2(6) . . ? F31' C32 C31 106.2(10) . . ? F33 C32 C31 108.8(7) . . ? O42 C41 O41 127.9(5) . . ? O42 C41 C42 114.8(5) . . ? O41 C41 C42 117.3(5) . . ? F41 C42 F43 108.6(6) . . ? F41 C42 F42 106.0(6) . . ? F43 C42 F42 106.7(6) . . ? F41 C42 C41 112.5(5) . . ? F43 C42 C41 110.0(5) . . ? F42 C42 C41 112.8(5) . . ? O51 C51 O52 128.5(6) . . ? O51 C51 C52 117.2(6) . . ? O52 C51 C52 114.3(6) . . ? F52 C52 F51 109.8(6) . . ? F52 C52 F53 106.8(6) . . ? F51 C52 F53 105.8(6) . . ? F52 C52 C51 111.6(6) . . ? F51 C52 C51 111.5(6) . . ? F53 C52 C51 111.1(6) . . ? O61 C61 O62 131.4(6) . . ? O61 C61 C62 113.0(5) . . ? O62 C61 C62 115.5(5) . . ? F63 C62 F61 108.9(7) . . ? F63 C62 F62 106.1(6) . . ? F61 C62 F62 105.4(6) . . ? F63 C62 C61 113.5(6) . . ? F61 C62 C61 111.9(5) . . ? F62 C62 C61 110.6(6) . . ? C11 O11 Ag2 125.4(4) . . ? C11 O12 Ag6 125.6(4) . 3 ? C21 O21 Ag2 112.6(4) . . ? C21 O22 Ag5 112.4(4) . . ? C31 O31 Ag1 113.4(4) . . ? C31 O31 Ag7 147.1(4) . . ? Ag1 O31 Ag7 95.11(14) . . ? C31 O32 Ag4 125.8(4) . 3_655 ? C41 O41 Ag1 119.1(4) . 3_655 ? C41 O41 Ag7 136.2(4) . 3_655 ? Ag1 O41 Ag7 96.73(15) 3_655 3_655 ? C41 O42 Ag5 131.3(4) . . ? C51 O51 Ag2 126.5(4) . . ? C51 O51 Ag3 146.1(4) . . ? Ag2 O51 Ag3 82.86(15) . . ? C51 O52 Ag7 118.8(4) . . ? C61 O61 Ag4 120.4(4) . . ? C61 O62 Ag3 125.0(4) . . ? F31' F31 F33' 120.8(19) . . ? F31' F31 C32 65.4(12) . . ? F33' F31 C32 58.9(11) . . ? F32' F32 C32 73(3) . . ? F32' F32 F31' 131(4) . . ? C32 F32 F31' 58.4(12) . . ? F33' F33 C32 61.3(12) . . ? F33' F33 F32' 100.5(17) . . ? C32 F33 F32' 48.2(11) . . ? F31 F31' C32 65.1(13) . . ? F31 F31' F32 110.6(17) . . ? C32 F31' F32 55.0(11) . . ? F32 F32' C32 76(3) . . ? F32 F32' F33 122(4) . . ? C32 F32' F33 52.7(13) . . ? F33 F33' F31 131.4(18) . . ? F33 F33' C32 69.1(15) . . ? F31 F33' C32 64.0(11) . . ? C09 N1 C010 109.1(7) . . ? C09 N1 C08 107.9(6) . . ? C010 N1 C08 109.6(7) . . ? C09 N1 C07 110.5(5) . . ? C010 N1 C07 112.4(6) . . ? C08 N1 C07 107.3(6) . . ? C06 C01 C02 120.1(7) . . ? C03 C02 C01 121.4(8) . . ? C02 C03 C04 118.5(7) . . ? C02 C03 Ag7 88.5(5) . . ? C04 C03 Ag7 92.9(5) . . ? C03 C04 C05 120.7(7) . . ? C06 C05 C04 121.0(7) . . ? C05 C06 C01 118.2(6) . . ? C05 C06 C07 121.5(6) . . ? C01 C06 C07 120.1(6) . . ? C06 C07 N1 116.4(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.04 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.841 _refine_diff_density_min -3.016 _refine_diff_density_rms 0.286