# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_2 _database_code_depnum_ccdc_archive 'CCDC 875487' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H16 Ag4 N2 O11' _chemical_formula_weight 783.74 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' 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 'P b c n' _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 25.0570(16) _cell_length_b 11.1882(4) _cell_length_c 13.0591(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3661.0(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1535 _cell_measurement_theta_min 3.0374 _cell_measurement_theta_max 29.1810 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.844 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2976 _exptl_absorpt_coefficient_mu 4.277 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4817 _exptl_absorpt_correction_T_max 0.5132 _exptl_absorpt_process_details SADABS _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 8683 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3224 _reflns_number_gt 2342 _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^)+(0.2000P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3224 _refine_ls_number_parameters 264 _refine_ls_number_restraints 58 _refine_ls_R_factor_all 0.1059 _refine_ls_R_factor_gt 0.0815 _refine_ls_wR_factor_ref 0.2981 _refine_ls_wR_factor_gt 0.2761 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 0.75079(4) 0.48524(11) 0.32996(13) 0.0508(5) Uani 1 1 d . . . Ag2 Ag 0.70944(6) 0.23585(12) 0.30914(15) 0.0627(6) Uani 1 1 d . . . Ag3 Ag 0.60571(6) 0.22655(14) 0.17543(12) 0.0554(5) Uani 1 1 d . . . C1 C 0.5539(5) 0.6016(12) 0.3954(10) 0.032(3) Uani 1 1 d . . . C2 C 0.6039(4) 0.6657(12) 0.4027(10) 0.032(3) Uani 1 1 d D A . C3 C 0.6050(5) 0.7948(12) 0.4065(11) 0.031(3) Uani 1 1 d . . . C4 C 0.5559(5) 0.8597(9) 0.4042(10) 0.030(3) Uani 1 1 d D . . C5 C 0.5076(5) 0.7981(12) 0.3966(10) 0.026(3) Uani 1 1 d U . . H5 H 0.4757 0.8401 0.3928 0.031 Uiso 1 1 calc R . . C6 C 0.5075(5) 0.6743(13) 0.3946(11) 0.035(3) Uani 1 1 d . . . H6 H 0.4745 0.6360 0.3927 0.042 Uiso 1 1 calc R . . C7 C 0.5510(6) 0.4735(12) 0.3876(14) 0.045(4) Uani 1 1 d U . . C8 C 0.6541(5) 0.5978(12) 0.4017(12) 0.037(3) Uani 1 1 d D . . C9 C 0.6563(6) 0.8566(11) 0.4077(13) 0.038(4) Uani 1 1 d . . . C10 C 0.5563(5) 0.9904(9) 0.4102(10) 0.027(3) Uani 1 1 d DU . . C11 C 0.6214(7) 0.2377(12) 0.4496(14) 0.042(4) Uani 1 1 d U . . H11A H 0.6088 0.3087 0.4830 0.063 Uiso 1 1 calc R B . H11B H 0.6097 0.1687 0.4870 0.063 Uiso 1 1 calc R . . H11C H 0.6074 0.2345 0.3812 0.063 Uiso 1 1 calc R . . N1 N 0.6078(6) 0.4147(15) 0.1673(12) 0.064(4) Uani 1 1 d . . . H1A H 0.6239 0.4370 0.1097 0.096 Uiso 1 1 calc R B . H1B H 0.6257 0.4434 0.2208 0.096 Uiso 1 1 calc R . . H1C H 0.5746 0.4432 0.1681 0.096 Uiso 1 1 calc R . . N2 N 0.5990(6) 0.0371(13) 0.1790(10) 0.054(4) Uani 1 1 d . . . H2A H 0.5668 0.0168 0.2022 0.081 Uiso 1 1 calc R B . H2B H 0.6239 0.0071 0.2201 0.081 Uiso 1 1 calc R . . H2C H 0.6034 0.0081 0.1161 0.081 Uiso 1 1 calc R . . O1 O 0.5079(4) 0.4268(8) 0.3693(7) 0.0313(16) Uani 1 1 d U B . O2 O 0.5906(6) 0.4157(13) 0.4128(11) 0.085(4) Uani 1 1 d U . . O3 O 0.6740(4) 0.5719(9) 0.3171(8) 0.042(3) Uani 1 1 d . A . O4 O 0.6647(13) 0.543(3) 0.483(2) 0.060(5) Uani 0.50(3) 1 d PU A 1 O4' O 0.6844(12) 0.594(3) 0.487(2) 0.060(5) Uani 0.50(3) 1 d PU A 2 O5 O 0.6854(5) 0.8492(11) 0.4872(10) 0.067(4) Uani 1 1 d . . . O6 O 0.6721(4) 0.8993(8) 0.3240(8) 0.037(2) Uani 1 1 d . . . O7 O 0.5921(4) 1.0439(9) 0.4518(9) 0.056(3) Uani 1 1 d . . . O8 O 0.5162(4) 1.0422(9) 0.3675(8) 0.039(2) Uani 1 1 d . . . O9 O 0.6693(6) 0.2391(11) 0.4464(15) 0.081(5) Uani 1 1 d . B . H9 H 0.6886 0.2417 0.5072 0.098 Uiso 1 1 calc R . . O2W O 0.7644(6) 0.5258(13) 0.5957(13) 0.096(5) Uani 1 1 d . . . H2WA H 0.7363 0.5393 0.5611 0.115 Uiso 1 1 d R . . H2WB H 0.7818 0.4689 0.5683 0.144 Uiso 1 1 d R . . O1W O 0.790(2) 0.237(3) 0.206(4) 0.083(7) Uani 0.39(3) 1 d PU B 1 H1WA H 0.8175 0.2399 0.2446 0.124 Uiso 0.39(3) 1 d PR B 1 H1WB H 0.7900 0.2913 0.1718 0.124 Uiso 0.39(3) 1 d PR B 1 O1W' O 0.7555(15) 0.241(2) 0.182(2) 0.083(7) Uani 0.61(3) 1 d PU B 2 H1WC H 0.7500 0.1787 0.1465 0.124 Uiso 0.61(3) 1 d PR B 2 H1WD H 0.7477 0.3026 0.1469 0.124 Uiso 0.61(3) 1 d PR B 2 Ag4 Ag 0.51757(5) 0.23396(9) 0.37170(12) 0.0448(5) Uani 1 1 d U . . 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 0.0246(8) 0.0444(8) 0.0833(12) -0.0020(6) 0.0013(5) 0.0091(5) Ag2 0.0513(10) 0.0465(9) 0.0902(14) 0.0007(7) -0.0102(8) -0.0031(6) Ag3 0.0415(9) 0.0666(10) 0.0580(10) 0.0030(7) -0.0095(6) -0.0038(6) C1 0.032(7) 0.038(7) 0.025(7) -0.003(6) 0.004(6) 0.004(6) C2 0.022(7) 0.048(8) 0.026(7) 0.002(7) 0.011(6) 0.018(6) C3 0.020(7) 0.030(6) 0.042(8) -0.014(7) 0.000(6) 0.008(5) C4 0.035(8) 0.030(7) 0.026(7) 0.001(6) -0.003(6) -0.007(6) C5 0.026(3) 0.026(3) 0.026(3) -0.0002(10) 0.0003(10) 0.0006(10) C6 0.026(7) 0.038(8) 0.039(8) 0.010(7) 0.006(6) 0.005(6) C7 0.041(9) 0.024(7) 0.071(11) 0.018(7) 0.026(8) 0.017(6) C8 0.031(8) 0.033(7) 0.048(9) 0.003(7) -0.012(7) 0.013(6) C9 0.029(8) 0.027(7) 0.059(10) -0.003(7) 0.014(8) -0.003(6) C10 0.027(3) 0.027(3) 0.027(3) -0.0001(10) 0.0008(10) -0.0007(10) C11 0.042(4) 0.042(4) 0.043(4) 0.0003(10) -0.0001(10) 0.0001(10) N1 0.045(9) 0.073(11) 0.074(11) -0.003(8) -0.015(8) -0.006(7) N2 0.048(8) 0.067(10) 0.046(8) 0.003(7) -0.009(6) -0.005(7) O1 0.0327(19) 0.0285(16) 0.0327(19) -0.0002(10) -0.0005(10) 0.0010(10) O2 0.084(4) 0.084(4) 0.085(4) 0.0004(10) 0.0002(10) 0.0003(10) O3 0.035(6) 0.048(6) 0.045(6) -0.010(5) 0.002(5) 0.012(5) O4 0.060(5) 0.060(5) 0.060(5) 0.0000(7) 0.0000(7) 0.0002(7) O4' 0.060(5) 0.060(5) 0.060(5) 0.0000(7) 0.0000(7) 0.0002(7) O5 0.053(7) 0.081(9) 0.066(8) 0.011(7) -0.028(6) -0.018(7) O6 0.031(5) 0.028(5) 0.053(6) -0.006(5) 0.010(5) -0.012(4) O7 0.052(7) 0.042(6) 0.073(8) -0.003(6) -0.007(6) -0.022(5) O8 0.034(6) 0.032(5) 0.051(6) 0.001(5) -0.012(5) -0.001(4) O9 0.049(9) 0.092(10) 0.103(13) -0.005(8) -0.006(9) -0.008(6) O2W 0.094(11) 0.106(11) 0.089(12) -0.025(10) -0.023(10) 0.026(9) O1W 0.083(7) 0.083(7) 0.083(7) 0.0000(7) 0.0000(7) 0.0000(7) O1W' 0.083(7) 0.083(7) 0.083(7) 0.0000(7) 0.0000(7) 0.0000(7) Ag4 0.0512(9) 0.0158(6) 0.0675(10) -0.0006(5) -0.0061(7) -0.0011(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 O6 2.159(9) 8_755 ? Ag1 O3 2.161(10) . ? Ag1 Ag2 2.9881(18) 8_765 ? Ag1 Ag2 2.9887(18) . ? Ag2 O1W' 2.02(3) . ? Ag2 O9 2.056(19) . ? Ag2 O1W 2.43(5) . ? Ag2 Ag1 2.9881(18) 8_755 ? Ag2 Ag3 3.133(2) . ? Ag3 N1 2.109(17) . ? Ag3 N2 2.127(15) . ? Ag3 Ag4 3.1508(19) 3_655 ? Ag3 Ag4 3.384(2) . ? C1 C6 1.419(18) . ? C1 C7 1.439(19) . ? C1 C2 1.447(18) . ? C2 C3 1.44(2) . ? C2 C8 1.469(9) . ? C3 C4 1.428(17) . ? C3 C9 1.461(18) . ? C4 C5 1.396(17) . ? C4 C10 1.465(9) . ? C5 C6 1.39(2) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 O1 1.225(18) . ? C7 O2 1.228(19) . ? C8 O3 1.247(17) . ? C8 O4 1.25(3) . ? C8 O4' 1.35(3) . ? C9 O6 1.257(18) . ? C9 O5 1.27(2) . ? C10 O7 1.208(16) . ? C10 O8 1.285(16) . ? C11 O9 1.20(2) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? N1 H1A 0.8900 . ? N1 H1B 0.8900 . ? N1 H1C 0.8900 . ? N2 H2A 0.8900 . ? N2 H2B 0.8900 . ? N2 H2C 0.8900 . ? O1 Ag4 2.172(9) . ? O6 Ag1 2.159(9) 8_765 ? O8 Ag4 2.146(10) 1_565 ? O9 H9 0.9300 . ? O2W H2WA 0.8499 . ? O2W H2WB 0.8500 . ? O1W H1WA 0.8498 . ? O1W H1WB 0.7500 . ? O1W' H1WB 1.0386 . ? O1W' H1WC 0.8499 . ? O1W' H1WD 0.8500 . ? Ag4 O8 2.146(10) 1_545 ? Ag4 Ag3 3.1508(19) 3_655 ? Ag4 Ag4 3.298(3) 3_655 ? 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 O6 Ag1 O3 173.5(4) 8_755 . ? O6 Ag1 Ag2 96.7(3) 8_755 8_765 ? O3 Ag1 Ag2 82.4(3) . 8_765 ? O6 Ag1 Ag2 83.8(3) 8_755 . ? O3 Ag1 Ag2 95.9(3) . . ? Ag2 Ag1 Ag2 169.53(10) 8_765 . ? O1W' Ag2 O9 173.9(11) . . ? O1W' Ag2 O1W 21.6(13) . . ? O9 Ag2 O1W 152.9(14) . . ? O1W' Ag2 Ag1 84.9(8) . 8_755 ? O9 Ag2 Ag1 95.8(4) . 8_755 ? O1W Ag2 Ag1 77.3(9) . 8_755 ? O1W' Ag2 Ag1 81.3(7) . . ? O9 Ag2 Ag1 94.2(4) . . ? O1W Ag2 Ag1 75.8(8) . . ? Ag1 Ag2 Ag1 138.78(6) 8_755 . ? O1W' Ag2 Ag3 91.0(11) . . ? O9 Ag2 Ag3 94.6(4) . . ? O1W Ag2 Ag3 112.5(13) . . ? Ag1 Ag2 Ag3 107.23(6) 8_755 . ? Ag1 Ag2 Ag3 111.67(6) . . ? N1 Ag3 N2 176.5(6) . . ? N1 Ag3 Ag2 88.5(4) . . ? N2 Ag3 Ag2 95.0(4) . . ? N1 Ag3 Ag4 89.3(4) . 3_655 ? N2 Ag3 Ag4 87.3(4) . 3_655 ? Ag2 Ag3 Ag4 157.12(7) . 3_655 ? N1 Ag3 Ag4 91.7(4) . . ? N2 Ag3 Ag4 87.5(4) . . ? Ag2 Ag3 Ag4 96.80(6) . . ? Ag4 Ag3 Ag4 60.50(5) 3_655 . ? C6 C1 C7 122.0(13) . . ? C6 C1 C2 115.2(12) . . ? C7 C1 C2 122.8(12) . . ? C1 C2 C3 120.9(9) . . ? C1 C2 C8 118.9(12) . . ? C3 C2 C8 120.1(11) . . ? C4 C3 C2 119.4(10) . . ? C4 C3 C9 121.2(11) . . ? C2 C3 C9 119.4(10) . . ? C5 C4 C3 119.8(10) . . ? C5 C4 C10 120.1(12) . . ? C3 C4 C10 120.1(12) . . ? C4 C5 C6 119.8(11) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C5 C6 C1 124.7(12) . . ? C5 C6 H6 117.6 . . ? C1 C6 H6 117.6 . . ? O1 C7 O2 122.7(14) . . ? O1 C7 C1 118.8(13) . . ? O2 C7 C1 117.8(16) . . ? O3 C8 O4 123.5(15) . . ? O3 C8 O4' 120.0(15) . . ? O3 C8 C2 118.1(12) . . ? O4 C8 C2 115.3(17) . . ? O4' C8 C2 119.4(16) . . ? O6 C9 O5 123.7(13) . . ? O6 C9 C3 116.6(15) . . ? O5 C9 C3 118.9(14) . . ? O7 C10 O8 123.5(11) . . ? O7 C10 C4 121.5(12) . . ? O8 C10 C4 115.0(11) . . ? O9 C11 H11A 109.5 . . ? O9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Ag3 N1 H1A 109.5 . . ? Ag3 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? Ag3 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? Ag3 N2 H2A 109.5 . . ? Ag3 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? Ag3 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C7 O1 Ag4 108.8(8) . . ? C8 O3 Ag1 113.1(8) . . ? C9 O6 Ag1 114.8(9) . 8_765 ? C10 O8 Ag4 115.3(8) . 1_565 ? C11 O9 Ag2 121.2(16) . . ? C11 O9 H9 119.4 . . ? Ag2 O9 H9 119.4 . . ? H2WA O2W H2WB 109.5 . . ? Ag2 O1W H1WA 109.9 . . ? Ag2 O1W H1WB 109.1 . . ? H1WA O1W H1WB 109.5 . . ? Ag2 O1W H1WC 73.2 . . ? H1WA O1W H1WC 154.6 . . ? H1WB O1W H1WC 92.3 . . ? Ag2 O1W' H1WB 126.6 . . ? Ag2 O1W' H1WC 109.4 . . ? H1WB O1W' H1WC 120.5 . . ? Ag2 O1W' H1WD 109.5 . . ? H1WB O1W' H1WD 71.7 . . ? H1WC O1W' H1WD 109.5 . . ? O8 Ag4 O1 172.3(4) 1_545 . ? O8 Ag4 Ag3 87.3(2) 1_545 3_655 ? O1 Ag4 Ag3 85.0(2) . 3_655 ? O8 Ag4 Ag4 88.4(3) 1_545 3_655 ? O1 Ag4 Ag4 87.5(2) . 3_655 ? Ag3 Ag4 Ag4 63.26(5) 3_655 3_655 ? O8 Ag4 Ag3 88.1(3) 1_545 . ? O1 Ag4 Ag3 95.0(2) . . ? Ag3 Ag4 Ag3 119.42(5) 3_655 . ? Ag4 Ag4 Ag3 56.24(5) 3_655 . ? 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 O6 Ag1 Ag2 O1W' -56.4(11) 8_755 . . . ? O3 Ag1 Ag2 O1W' 117.0(11) . . . . ? Ag2 Ag1 Ag2 O1W' 36.5(11) 8_765 . . . ? O6 Ag1 Ag2 O9 119.3(5) 8_755 . . . ? O3 Ag1 Ag2 O9 -67.3(5) . . . . ? Ag2 Ag1 Ag2 O9 -147.8(5) 8_765 . . . ? O6 Ag1 Ag2 O1W -35.1(14) 8_755 . . . ? O3 Ag1 Ag2 O1W 138.3(14) . . . . ? Ag2 Ag1 Ag2 O1W 57.8(14) 8_765 . . . ? O6 Ag1 Ag2 Ag1 15.6(3) 8_755 . . 8_755 ? O3 Ag1 Ag2 Ag1 -171.0(3) . . . 8_755 ? Ag2 Ag1 Ag2 Ag1 108.5(2) 8_765 . . 8_755 ? O6 Ag1 Ag2 Ag3 -144.0(3) 8_755 . . . ? O3 Ag1 Ag2 Ag3 29.4(3) . . . . ? Ag2 Ag1 Ag2 Ag3 -51.1(2) 8_765 . . . ? O1W' Ag2 Ag3 N1 -85.2(8) . . . . ? O9 Ag2 Ag3 N1 92.3(6) . . . . ? O1W Ag2 Ag3 N1 -87.2(10) . . . . ? Ag1 Ag2 Ag3 N1 -170.2(4) 8_755 . . . ? Ag1 Ag2 Ag3 N1 -4.1(4) . . . . ? O1W' Ag2 Ag3 N2 95.2(8) . . . . ? O9 Ag2 Ag3 N2 -87.3(5) . . . . ? O1W Ag2 Ag3 N2 93.2(9) . . . . ? Ag1 Ag2 Ag3 N2 10.2(4) 8_755 . . . ? Ag1 Ag2 Ag3 N2 176.3(4) . . . . ? O1W' Ag2 Ag3 Ag4 -169.9(7) . . . 3_655 ? O9 Ag2 Ag3 Ag4 7.6(4) . . . 3_655 ? O1W Ag2 Ag3 Ag4 -171.9(9) . . . 3_655 ? Ag1 Ag2 Ag3 Ag4 105.07(15) 8_755 . . 3_655 ? Ag1 Ag2 Ag3 Ag4 -88.85(16) . . . 3_655 ? O1W' Ag2 Ag3 Ag4 -176.7(7) . . . . ? O9 Ag2 Ag3 Ag4 0.8(4) . . . . ? O1W Ag2 Ag3 Ag4 -178.7(9) . . . . ? Ag1 Ag2 Ag3 Ag4 98.28(7) 8_755 . . . ? Ag1 Ag2 Ag3 Ag4 -95.64(7) . . . . ? C6 C1 C2 C3 -1.2(18) . . . . ? C7 C1 C2 C3 177.6(14) . . . . ? C6 C1 C2 C8 -178.7(13) . . . . ? C7 C1 C2 C8 0(2) . . . . ? C1 C2 C3 C4 0.6(19) . . . . ? C8 C2 C3 C4 178.0(14) . . . . ? C1 C2 C3 C9 -176.4(14) . . . . ? C8 C2 C3 C9 1(2) . . . . ? C2 C3 C4 C5 -1(2) . . . . ? C9 C3 C4 C5 176.0(14) . . . . ? C2 C3 C4 C10 178.7(12) . . . . ? C9 C3 C4 C10 -4(2) . . . . ? C3 C4 C5 C6 2.0(19) . . . . ? C10 C4 C5 C6 -177.7(12) . . . . ? C4 C5 C6 C1 -2.9(19) . . . . ? C7 C1 C6 C5 -176.5(14) . . . . ? C2 C1 C6 C5 2.4(19) . . . . ? C6 C1 C7 O1 8(2) . . . . ? C2 C1 C7 O1 -171.2(14) . . . . ? C6 C1 C7 O2 -163.1(15) . . . . ? C2 C1 C7 O2 18(2) . . . . ? C1 C2 C8 O3 86.0(17) . . . . ? C3 C2 C8 O3 -91.5(17) . . . . ? C1 C2 C8 O4 -75(2) . . . . ? C3 C2 C8 O4 108(2) . . . . ? C1 C2 C8 O4' -112(2) . . . . ? C3 C2 C8 O4' 71(2) . . . . ? C4 C3 C9 O6 -76.9(17) . . . . ? C2 C3 C9 O6 100.0(15) . . . . ? C4 C3 C9 O5 113.1(17) . . . . ? C2 C3 C9 O5 -69.9(18) . . . . ? C5 C4 C10 O7 153.2(14) . . . . ? C3 C4 C10 O7 -27(2) . . . . ? C5 C4 C10 O8 -27.3(19) . . . . ? C3 C4 C10 O8 153.0(13) . . . . ? O2 C7 O1 Ag4 -7(2) . . . . ? C1 C7 O1 Ag4 -176.7(12) . . . . ? O4 C8 O3 Ag1 -26(3) . . . . ? O4' C8 O3 Ag1 13(2) . . . . ? C2 C8 O3 Ag1 175.2(10) . . . . ? Ag2 Ag1 O3 C8 -93.0(10) 8_765 . . . ? Ag2 Ag1 O3 C8 97.4(10) . . . . ? O5 C9 O6 Ag1 -8.9(18) . . . 8_765 ? C3 C9 O6 Ag1 -178.4(8) . . . 8_765 ? O7 C10 O8 Ag4 1.4(18) . . . 1_565 ? C4 C10 O8 Ag4 -178.1(9) . . . 1_565 ? O1W Ag2 O9 C11 179(2) . . . . ? Ag1 Ag2 O9 C11 -108.2(12) 8_755 . . . ? Ag1 Ag2 O9 C11 111.8(12) . . . . ? Ag3 Ag2 O9 C11 -0.3(13) . . . . ? C7 O1 Ag4 Ag3 179.0(10) . . . 3_655 ? C7 O1 Ag4 Ag4 -117.6(10) . . . 3_655 ? C7 O1 Ag4 Ag3 -61.8(10) . . . . ? N1 Ag3 Ag4 O8 177.6(4) . . . 1_545 ? N2 Ag3 Ag4 O8 1.0(4) . . . 1_545 ? Ag2 Ag3 Ag4 O8 -93.7(2) . . . 1_545 ? Ag4 Ag3 Ag4 O8 89.3(2) 3_655 . . 1_545 ? N1 Ag3 Ag4 O1 4.6(4) . . . . ? N2 Ag3 Ag4 O1 -171.9(4) . . . . ? Ag2 Ag3 Ag4 O1 93.4(2) . . . . ? Ag4 Ag3 Ag4 O1 -83.6(2) 3_655 . . . ? N1 Ag3 Ag4 Ag3 91.7(4) . . . 3_655 ? N2 Ag3 Ag4 Ag3 -84.8(4) . . . 3_655 ? Ag2 Ag3 Ag4 Ag3 -179.56(4) . . . 3_655 ? Ag4 Ag3 Ag4 Ag3 3.47(7) 3_655 . . 3_655 ? N1 Ag3 Ag4 Ag4 88.3(4) . . . 3_655 ? N2 Ag3 Ag4 Ag4 -88.3(4) . . . 3_655 ? Ag2 Ag3 Ag4 Ag4 176.97(5) . . . 3_655 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2W H2WB O5 0.85 1.89 2.737(19) 170.6 8_755 O2W H2WA O4 0.85 2.06 2.91(3) 170.5 . O1W H1WB O2W 0.75 2.36 3.08(4) 161.5 7_565 O1W H1WA O6 0.85 2.08 2.56(5) 115.2 8_755 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.775 _refine_diff_density_min -1.997 _refine_diff_density_rms 0.256 data_3 _database_code_depnum_ccdc_archive 'CCDC 875488' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H5 Ag5 O12' _chemical_formula_weight 868.50 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' 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 'P b c n' _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 18.1669(13) _cell_length_b 13.5876(7) _cell_length_c 6.4273(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1586.54(17) _cell_formula_units_Z 4 _cell_measurement_temperature 296 _cell_measurement_reflns_used 1185 _cell_measurement_theta_min 2.9925 _cell_measurement_theta_max 28.9985 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 6.131 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3735 _exptl_absorpt_correction_T_max 0.4049 _exptl_absorpt_process_details SADABS(2009) _exptl_special_details ; ? ; _diffrn_ambient_temperature 296 _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 3851 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_sigmaI/netI 0.0536 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1401 _reflns_number_gt 1179 _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^)+(0.1194P)^2^+7.6477P] 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 1401 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1832 _refine_ls_wR_factor_gt 0.1742 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 0.22896(5) 0.65128(6) 0.10818(15) 0.0387(4) Uani 1 1 d . . . Ag2 Ag 0.28646(5) 0.56287(7) 0.49006(14) 0.0394(4) Uani 1 1 d . . . Ag3 Ag 0.07985(14) 0.74694(17) 0.2403(3) 0.0586(7) Uani 0.50 1 d P . . O3 O 0.3308(5) 0.7380(6) 0.0597(14) 0.0400(19) Uani 1 1 d . . . O2 O 0.3412(4) 0.7180(5) 0.4017(12) 0.0374(19) Uani 1 1 d . . . C6 C 0.3621(6) 0.7514(6) 0.2318(17) 0.025(2) Uani 1 1 d . . . O1 O 0.4570(5) 0.6065(5) 0.1274(12) 0.0396(19) Uani 1 1 d . . . C1 C 0.5000 0.7597(9) 0.2500 0.020(3) Uani 1 2 d S . . C4 C 0.5000 0.9658(9) 0.2500 0.018(3) Uani 1 2 d S . . H4 H 0.5000 1.0343 0.2500 0.021 Uiso 1 2 calc SR . . C5 C 0.5000 0.6490(10) 0.2500 0.026(3) Uani 1 2 d S . . C3 C 0.4326(5) 0.9148(6) 0.2371(14) 0.0186(18) Uani 1 1 d . . . C2 C 0.4328(5) 0.8108(7) 0.2352(12) 0.0206(19) Uani 1 1 d . . . C7 C 0.3621(6) 0.9737(7) 0.2266(14) 0.025(2) Uani 1 1 d . . . O4 O 0.3022(4) 0.9300(5) 0.2478(13) 0.0302(16) Uani 1 1 d . . . O5 O 0.3694(4) 1.0655(4) 0.2000(12) 0.0289(17) Uani 1 1 d . . . O1W O 0.3736(5) 0.4634(6) 0.3041(11) 0.0384(19) Uani 1 1 d . . . H1WA H 0.3982 0.4291 0.3901 0.058 Uiso 1 1 d R . . H1WB H 0.4025 0.5005 0.2360 0.058 Uiso 1 1 d 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 0.0348(6) 0.0289(6) 0.0524(7) 0.0092(4) -0.0107(4) -0.0145(3) Ag2 0.0414(7) 0.0381(6) 0.0386(6) 0.0066(4) 0.0066(4) -0.0065(4) Ag3 0.0662(15) 0.0608(14) 0.0487(12) -0.0102(10) 0.0053(11) 0.0010(11) O3 0.035(4) 0.028(4) 0.057(5) -0.001(4) -0.021(4) -0.008(3) O2 0.039(4) 0.015(3) 0.058(5) 0.005(3) 0.021(4) 0.000(3) C6 0.023(5) 0.006(4) 0.045(6) -0.002(4) -0.003(5) 0.004(3) O1 0.053(5) 0.021(4) 0.045(4) -0.009(3) -0.016(4) -0.004(4) C1 0.024(7) 0.013(6) 0.023(6) 0.000 0.005(6) 0.000 C4 0.030(7) 0.006(5) 0.017(6) 0.000 0.005(6) 0.000 C5 0.031(8) 0.022(7) 0.026(6) 0.000 0.003(7) 0.000 C3 0.024(5) 0.014(4) 0.018(4) 0.002(3) 0.002(4) 0.001(4) C2 0.031(5) 0.016(4) 0.014(4) 0.004(3) -0.003(4) -0.007(4) C7 0.033(6) 0.022(5) 0.019(4) -0.004(4) 0.001(4) 0.006(4) O4 0.019(3) 0.028(4) 0.043(4) 0.014(3) -0.004(3) -0.001(3) O5 0.028(4) 0.010(3) 0.049(4) 0.006(3) -0.002(4) 0.006(3) O1W 0.048(5) 0.039(4) 0.028(4) 0.008(3) -0.001(4) -0.005(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 O5 2.213(7) 7_655 ? Ag1 O3 2.216(8) . ? Ag1 O2 2.558(7) 2_564 ? Ag1 Ag2 2.9255(13) . ? Ag1 Ag3 3.122(3) . ? Ag1 Ag2 3.1835(12) 8_565 ? Ag2 O4 2.312(7) 2_565 ? Ag2 O2 2.399(7) . ? Ag2 O1W 2.400(8) . ? Ag2 O1W 2.589(8) 8_566 ? Ag2 Ag1 3.1835(12) 8_566 ? Ag3 Ag3 2.904(5) 4 ? O3 C6 1.257(14) . ? O2 C6 1.242(13) . ? O2 Ag1 2.558(7) 2_565 ? C6 C2 1.518(14) . ? O1 C5 1.251(9) . ? C1 C2 1.408(11) 4_655 ? C1 C2 1.408(11) . ? C1 C5 1.504(17) . ? C4 C3 1.410(11) . ? C4 C3 1.410(11) 4_655 ? C4 H4 0.9300 . ? C5 O1 1.251(9) 4_655 ? C3 C2 1.413(12) . ? C3 C7 1.513(13) . ? C7 O4 1.247(12) . ? C7 O5 1.266(12) . ? O4 Ag2 2.312(7) 2_564 ? O5 Ag1 2.213(7) 7_665 ? O1W Ag2 2.589(8) 8_565 ? O1W H1WA 0.8501 . ? O1W H1WB 0.8499 . ? 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 O5 Ag1 O3 172.6(3) 7_655 . ? O5 Ag1 O2 95.8(3) 7_655 2_564 ? O3 Ag1 O2 88.5(3) . 2_564 ? O5 Ag1 Ag2 81.27(19) 7_655 . ? O3 Ag1 Ag2 92.2(2) . . ? O2 Ag1 Ag2 153.95(18) 2_564 . ? O5 Ag1 Ag3 56.38(18) 7_655 . ? O3 Ag1 Ag3 122.8(2) . . ? O2 Ag1 Ag3 54.5(2) 2_564 . ? Ag2 Ag1 Ag3 104.63(5) . . ? O5 Ag1 Ag2 81.21(17) 7_655 8_565 ? O3 Ag1 Ag2 100.3(2) . 8_565 ? O2 Ag1 Ag2 132.43(17) 2_564 8_565 ? Ag2 Ag1 Ag2 73.00(3) . 8_565 ? Ag3 Ag1 Ag2 136.89(5) . 8_565 ? O4 Ag2 O2 114.9(2) 2_565 . ? O4 Ag2 O1W 147.1(3) 2_565 . ? O2 Ag2 O1W 95.9(3) . . ? O4 Ag2 O1W 82.7(3) 2_565 8_566 ? O2 Ag2 O1W 93.0(3) . 8_566 ? O1W Ag2 O1W 84.7(2) . 8_566 ? O4 Ag2 Ag1 109.6(2) 2_565 . ? O2 Ag2 Ag1 65.7(2) . . ? O1W Ag2 Ag1 92.80(17) . . ? O1W Ag2 Ag1 158.25(19) 8_566 . ? O4 Ag2 Ag1 68.83(17) 2_565 8_566 ? O2 Ag2 Ag1 174.63(18) . 8_566 ? O1W Ag2 Ag1 79.65(19) . 8_566 ? O1W Ag2 Ag1 83.60(18) 8_566 8_566 ? Ag1 Ag2 Ag1 117.27(4) . 8_566 ? Ag3 Ag3 Ag1 151.46(7) 4 . ? C6 O3 Ag1 109.3(7) . . ? C6 O2 Ag2 131.0(6) . . ? C6 O2 Ag1 110.7(6) . 2_565 ? Ag2 O2 Ag1 106.3(3) . 2_565 ? O2 C6 O3 125.7(9) . . ? O2 C6 C2 116.1(9) . . ? O3 C6 C2 118.1(9) . . ? C2 C1 C2 120.8(11) 4_655 . ? C2 C1 C5 119.6(5) 4_655 . ? C2 C1 C5 119.6(5) . . ? C3 C4 C3 121.0(11) . 4_655 ? C3 C4 H4 119.5 . . ? C3 C4 H4 119.5 4_655 . ? O1 C5 O1 125.0(12) . 4_655 ? O1 C5 C1 117.5(6) . . ? O1 C5 C1 117.5(6) 4_655 . ? C2 C3 C4 119.4(9) . . ? C2 C3 C7 122.1(8) . . ? C4 C3 C7 118.5(8) . . ? C1 C2 C3 119.7(8) . . ? C1 C2 C6 118.2(8) . . ? C3 C2 C6 122.0(8) . . ? O4 C7 O5 125.1(9) . . ? O4 C7 C3 118.8(8) . . ? O5 C7 C3 116.0(9) . . ? C7 O4 Ag2 120.6(6) . 2_564 ? C7 O5 Ag1 118.1(7) . 7_665 ? Ag2 O1W Ag2 93.6(3) . 8_565 ? Ag2 O1W H1WA 109.4 . . ? Ag2 O1W H1WA 138.8 8_565 . ? Ag2 O1W H1WB 109.4 . . ? Ag2 O1W H1WB 93.4 8_565 . ? H1WA O1W H1WB 109.5 . . ? 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 O5 Ag1 Ag2 O4 -43.1(3) 7_655 . . 2_565 ? O3 Ag1 Ag2 O4 133.4(3) . . . 2_565 ? O2 Ag1 Ag2 O4 42.4(4) 2_564 . . 2_565 ? Ag3 Ag1 Ag2 O4 8.70(19) . . . 2_565 ? Ag2 Ag1 Ag2 O4 -126.47(18) 8_565 . . 2_565 ? O5 Ag1 Ag2 O2 -152.4(3) 7_655 . . . ? O3 Ag1 Ag2 O2 24.1(3) . . . . ? O2 Ag1 Ag2 O2 -67.0(5) 2_564 . . . ? Ag3 Ag1 Ag2 O2 -100.61(19) . . . . ? Ag2 Ag1 Ag2 O2 124.22(19) 8_565 . . . ? O5 Ag1 Ag2 O1W 112.4(3) 7_655 . . . ? O3 Ag1 Ag2 O1W -71.1(3) . . . . ? O2 Ag1 Ag2 O1W -162.2(4) 2_564 . . . ? Ag3 Ag1 Ag2 O1W 164.1(2) . . . . ? Ag2 Ag1 Ag2 O1W 29.0(2) 8_565 . . . ? O5 Ag1 Ag2 O1W -164.9(5) 7_655 . . 8_566 ? O3 Ag1 Ag2 O1W 11.6(5) . . . 8_566 ? O2 Ag1 Ag2 O1W -79.5(6) 2_564 . . 8_566 ? Ag3 Ag1 Ag2 O1W -113.2(5) . . . 8_566 ? Ag2 Ag1 Ag2 O1W 111.7(5) 8_565 . . 8_566 ? O5 Ag1 Ag2 Ag1 32.59(18) 7_655 . . 8_566 ? O3 Ag1 Ag2 Ag1 -150.9(2) . . . 8_566 ? O2 Ag1 Ag2 Ag1 118.0(4) 2_564 . . 8_566 ? Ag3 Ag1 Ag2 Ag1 84.34(6) . . . 8_566 ? Ag2 Ag1 Ag2 Ag1 -50.82(5) 8_565 . . 8_566 ? O5 Ag1 Ag3 Ag3 -33.6(3) 7_655 . . 4 ? O3 Ag1 Ag3 Ag3 155.2(3) . . . 4 ? O2 Ag1 Ag3 Ag3 95.0(3) 2_564 . . 4 ? Ag2 Ag1 Ag3 Ag3 -102.4(2) . . . 4 ? Ag2 Ag1 Ag3 Ag3 -21.8(3) 8_565 . . 4 ? O2 Ag1 O3 C6 128.7(7) 2_564 . . . ? Ag2 Ag1 O3 C6 -25.3(6) . . . . ? Ag3 Ag1 O3 C6 83.7(7) . . . . ? Ag2 Ag1 O3 C6 -98.4(6) 8_565 . . . ? O4 Ag2 O2 C6 -143.5(9) 2_565 . . . ? O1W Ag2 O2 C6 48.2(9) . . . . ? O1W Ag2 O2 C6 133.2(9) 8_566 . . . ? Ag1 Ag2 O2 C6 -42.2(9) . . . . ? O4 Ag2 O2 Ag1 -5.6(4) 2_565 . . 2_565 ? O1W Ag2 O2 Ag1 -173.9(3) . . . 2_565 ? O1W Ag2 O2 Ag1 -88.9(3) 8_566 . . 2_565 ? Ag1 Ag2 O2 Ag1 95.7(3) . . . 2_565 ? Ag2 O2 C6 O3 37.0(14) . . . . ? Ag1 O2 C6 O3 -99.5(10) 2_565 . . . ? Ag2 O2 C6 C2 -141.0(7) . . . . ? Ag1 O2 C6 C2 82.5(9) 2_565 . . . ? Ag1 O3 C6 O2 2.9(12) . . . . ? Ag1 O3 C6 C2 -179.1(6) . . . . ? C2 C1 C5 O1 -139.2(6) 4_655 . . . ? C2 C1 C5 O1 40.8(6) . . . . ? C2 C1 C5 O1 40.8(6) 4_655 . . 4_655 ? C2 C1 C5 O1 -139.2(6) . . . 4_655 ? C3 C4 C3 C2 -0.6(6) 4_655 . . . ? C3 C4 C3 C7 179.2(9) 4_655 . . . ? C2 C1 C2 C3 -0.6(6) 4_655 . . . ? C5 C1 C2 C3 179.4(6) . . . . ? C2 C1 C2 C6 -176.6(8) 4_655 . . . ? C5 C1 C2 C6 3.4(8) . . . . ? C4 C3 C2 C1 1.2(11) . . . . ? C7 C3 C2 C1 -178.6(7) . . . . ? C4 C3 C2 C6 177.0(7) . . . . ? C7 C3 C2 C6 -2.7(13) . . . . ? O2 C6 C2 C1 76.5(10) . . . . ? O3 C6 C2 C1 -101.6(9) . . . . ? O2 C6 C2 C3 -99.4(10) . . . . ? O3 C6 C2 C3 82.4(11) . . . . ? C2 C3 C7 O4 10.8(13) . . . . ? C4 C3 C7 O4 -168.9(8) . . . . ? C2 C3 C7 O5 -170.4(8) . . . . ? C4 C3 C7 O5 9.9(11) . . . . ? O5 C7 O4 Ag2 59.4(12) . . . 2_564 ? C3 C7 O4 Ag2 -121.9(7) . . . 2_564 ? O4 C7 O5 Ag1 -15.7(13) . . . 7_665 ? C3 C7 O5 Ag1 165.6(6) . . . 7_665 ? O4 Ag2 O1W Ag2 99.1(5) 2_565 . . 8_565 ? O2 Ag2 O1W Ag2 -100.7(3) . . . 8_565 ? O1W Ag2 O1W Ag2 166.9(3) 8_566 . . 8_565 ? Ag1 Ag2 O1W Ag2 -34.79(19) . . . 8_565 ? Ag1 Ag2 O1W Ag2 82.43(19) 8_566 . . 8_565 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O1 0.85 1.92 2.742(10) 161.0 8_566 O1W H1WB O1 0.85 1.88 2.714(11) 166.0 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.639 _refine_diff_density_min -1.268 _refine_diff_density_rms 0.272