# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_1-30 _database_code_depnum_ccdc_archive 'CCDC 890733' #TrackingRef 'web_deposit_cif_file_0_DiSun_1341553643.p1-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H9 Ag2 N3 O6' _chemical_formula_sum 'C8 H9 Ag2 N3 O6' _chemical_formula_weight 458.92 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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' 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 7.1277(13) _cell_length_b 21.708(4) _cell_length_c 7.7585(14) _cell_angle_alpha 90.00 _cell_angle_beta 102.497(3) _cell_angle_gamma 90.00 _cell_volume 1172.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4556 _cell_measurement_theta_min 5.630 _cell_measurement_theta_max 57.152 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 3.369 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.3459 _exptl_absorpt_correction_T_max 0.5522 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 5728 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2042 _reflns_number_gt 2002 _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^)+(0.0378P)^2^+2.3420P] 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 2042 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0286 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0729 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 0.56258(5) 0.528575(14) 0.67012(4) 0.02312(12) Uani 1 1 d . . . Ag2 Ag 0.13355(5) 0.566148(16) 0.54545(5) 0.02886(13) Uani 1 1 d . . . C1 C 0.8181(6) 0.7554(2) 1.3456(6) 0.0267(10) Uani 1 1 d . . . H1A H 0.8432 0.7881 1.4287 0.032 Uiso 1 1 calc R . . C2 C 0.8374(6) 0.76483(19) 1.1768(6) 0.0241(9) Uani 1 1 d . . . H2A H 0.8762 0.8037 1.1405 0.029 Uiso 1 1 calc R . . C3 C 0.7990(6) 0.71634(19) 1.0605(6) 0.0201(9) Uani 1 1 d . . . C4 C 0.7383(5) 0.65856(18) 1.1026(6) 0.0178(8) Uani 1 1 d . . . C5 C 0.7194(5) 0.65038(19) 1.2748(6) 0.0181(8) Uani 1 1 d . . . C6 C 0.7622(6) 0.6984(2) 1.3970(6) 0.0220(9) Uani 1 1 d . . . H6A H 0.7529 0.6920 1.5159 0.026 Uiso 1 1 calc R . . C7 C 0.6542(6) 0.5903(2) 1.3383(6) 0.0216(9) Uani 1 1 d . . . C8 C 0.6948(5) 0.60743(18) 0.9668(5) 0.0168(8) Uani 1 1 d . . . N1 N 0.8395(5) 0.72546(17) 0.8843(5) 0.0232(8) Uani 1 1 d . . . N2 N 0.1605(5) 0.55652(17) 0.8204(5) 0.0241(8) Uani 1 1 d . . . H2B H 0.0457 0.5649 0.8486 0.036 Uiso 1 1 calc R . . H2C H 0.2511 0.5832 0.8780 0.036 Uiso 1 1 calc R . . H2D H 0.1962 0.5172 0.8531 0.036 Uiso 1 1 calc R . . N3 N 0.1389(5) 0.59283(18) 0.2832(5) 0.0283(8) Uani 1 1 d . . . H3A H 0.2580 0.5859 0.2627 0.042 Uiso 1 1 calc R . . H3B H 0.1101 0.6336 0.2687 0.042 Uiso 1 1 calc R . . H3C H 0.0508 0.5704 0.2058 0.042 Uiso 1 1 calc R . . O1 O 0.5255(4) 0.56164(13) 1.2321(4) 0.0228(6) Uani 1 1 d . . . O2 O 0.7297(4) 0.57464(15) 1.4911(4) 0.0301(7) Uani 1 1 d . . . O3 O 0.5490(4) 0.61497(13) 0.8463(4) 0.0224(6) Uani 1 1 d . . . O4 O 0.8053(4) 0.56262(13) 0.9854(4) 0.0216(6) Uani 1 1 d . . . O5 O 0.9101(5) 0.68296(15) 0.8196(4) 0.0311(7) Uani 1 1 d . . . O6 O 0.8038(5) 0.77558(15) 0.8132(5) 0.0375(8) 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 0.0281(2) 0.01816(19) 0.0238(2) -0.00212(12) 0.00727(15) -0.00635(12) Ag2 0.0220(2) 0.0321(2) 0.0313(2) 0.00452(14) 0.00324(15) 0.00029(14) C1 0.022(2) 0.021(2) 0.036(3) -0.0106(19) 0.0024(19) 0.0000(17) C2 0.020(2) 0.014(2) 0.035(3) -0.0016(18) 0.0011(18) -0.0030(16) C3 0.0142(18) 0.020(2) 0.026(2) 0.0020(17) 0.0018(17) 0.0011(16) C4 0.0091(17) 0.016(2) 0.026(2) 0.0005(16) -0.0004(16) 0.0042(15) C5 0.0116(18) 0.018(2) 0.025(2) -0.0014(16) 0.0049(16) 0.0033(15) C6 0.020(2) 0.024(2) 0.022(2) -0.0027(17) 0.0047(17) -0.0027(17) C7 0.017(2) 0.023(2) 0.028(2) 0.0018(18) 0.0098(18) 0.0007(17) C8 0.0159(19) 0.017(2) 0.019(2) 0.0019(15) 0.0060(16) -0.0044(15) N1 0.0184(17) 0.024(2) 0.026(2) 0.0040(16) 0.0027(15) -0.0060(15) N2 0.0189(18) 0.0252(19) 0.028(2) 0.0008(15) 0.0054(15) 0.0009(15) N3 0.0189(18) 0.030(2) 0.035(2) 0.0024(17) 0.0042(16) 0.0023(16) O1 0.0234(15) 0.0200(15) 0.0247(16) -0.0009(12) 0.0044(13) -0.0065(12) O2 0.0242(16) 0.0386(19) 0.0271(18) 0.0096(14) 0.0046(14) -0.0075(14) O3 0.0199(14) 0.0197(15) 0.0247(16) -0.0038(12) -0.0014(12) 0.0011(12) O4 0.0184(14) 0.0207(16) 0.0259(17) -0.0005(12) 0.0053(13) 0.0024(12) O5 0.0364(18) 0.0273(18) 0.0320(19) -0.0003(14) 0.0128(15) -0.0021(15) O6 0.042(2) 0.0270(18) 0.043(2) 0.0159(15) 0.0088(16) 0.0007(15) _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 2.239(3) 3_667 ? Ag1 O2 2.251(3) 1_554 ? Ag1 O3 2.335(3) . ? Ag1 Ag1 2.8783(8) 3_666 ? Ag1 Ag2 3.1101(7) . ? Ag2 N2 2.110(4) . ? Ag2 N3 2.124(4) . ? C1 C2 1.362(6) . ? C1 C6 1.383(6) . ? C1 H1A 0.9500 . ? C2 C3 1.375(6) . ? C2 H2A 0.9500 . ? C3 C4 1.388(6) . ? C3 N1 1.471(5) . ? C4 C5 1.383(6) . ? C4 C8 1.515(6) . ? C5 C6 1.398(6) . ? C5 C7 1.502(6) . ? C6 H6A 0.9500 . ? C7 O2 1.239(5) . ? C7 O1 1.257(5) . ? C8 O4 1.240(5) . ? C8 O3 1.250(5) . ? N1 O5 1.211(5) . ? N1 O6 1.222(5) . ? N2 H2B 0.9100 . ? N2 H2C 0.9100 . ? N2 H2D 0.9100 . ? N3 H3A 0.9100 . ? N3 H3B 0.9100 . ? N3 H3C 0.9100 . ? O1 Ag1 2.239(3) 3_667 ? O2 Ag1 2.251(3) 1_556 ? 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 O2 145.36(12) 3_667 1_554 ? O1 Ag1 O3 117.00(11) 3_667 . ? O2 Ag1 O3 95.68(11) 1_554 . ? O1 Ag1 Ag1 83.10(8) 3_667 3_666 ? O2 Ag1 Ag1 74.09(9) 1_554 3_666 ? O3 Ag1 Ag1 147.05(7) . 3_666 ? O1 Ag1 Ag2 90.33(8) 3_667 . ? O2 Ag1 Ag2 107.92(8) 1_554 . ? O3 Ag1 Ag2 78.98(7) . . ? Ag1 Ag1 Ag2 74.871(15) 3_666 . ? N2 Ag2 N3 168.20(15) . . ? N2 Ag2 Ag1 77.96(10) . . ? N3 Ag2 Ag1 98.59(10) . . ? C2 C1 C6 120.5(4) . . ? C2 C1 H1A 119.8 . . ? C6 C1 H1A 119.8 . . ? C1 C2 C3 117.9(4) . . ? C1 C2 H2A 121.0 . . ? C3 C2 H2A 121.0 . . ? C2 C3 C4 124.4(4) . . ? C2 C3 N1 117.1(4) . . ? C4 C3 N1 118.3(4) . . ? C5 C4 C3 116.3(4) . . ? C5 C4 C8 122.0(4) . . ? C3 C4 C8 121.7(4) . . ? C4 C5 C6 120.4(4) . . ? C4 C5 C7 122.0(4) . . ? C6 C5 C7 117.6(4) . . ? C1 C6 C5 120.4(4) . . ? C1 C6 H6A 119.8 . . ? C5 C6 H6A 119.8 . . ? O2 C7 O1 126.5(4) . . ? O2 C7 C5 116.8(4) . . ? O1 C7 C5 116.7(4) . . ? O4 C8 O3 126.5(4) . . ? O4 C8 C4 117.7(3) . . ? O3 C8 C4 115.9(3) . . ? O5 N1 O6 123.8(4) . . ? O5 N1 C3 117.8(3) . . ? O6 N1 C3 118.4(4) . . ? Ag2 N2 H2B 109.5 . . ? Ag2 N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? Ag2 N2 H2D 109.5 . . ? H2B N2 H2D 109.5 . . ? H2C N2 H2D 109.5 . . ? Ag2 N3 H3A 109.5 . . ? Ag2 N3 H3B 109.5 . . ? H3A N3 H3B 109.5 . . ? Ag2 N3 H3C 109.5 . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? C7 O1 Ag1 115.4(3) . 3_667 ? C7 O2 Ag1 122.3(3) . 1_556 ? C8 O3 Ag1 101.5(2) . . ? 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 N2 H2B O4 0.91 2.20 3.077(5) 160.9 1_455 N2 H2C O3 0.91 2.30 3.013(5) 135.5 . N2 H2D O4 0.91 2.14 2.977(5) 152.3 3_667 N3 H3C O4 0.91 2.17 3.007(5) 152.2 1_454 N3 H3A O1 0.91 2.04 2.947(5) 173.7 1_554 N3 H3B O6 0.91 2.39 3.079(5) 132.6 4_575 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.776 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.112 data_2-60 _database_code_depnum_ccdc_archive 'CCDC 890734' #TrackingRef 'web_deposit_cif_file_0_DiSun_1341553643.p1-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H6 Ag2 N2 O6' _chemical_formula_weight 441.89 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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' 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 13.7150(5) _cell_length_b 10.8413(4) _cell_length_c 7.3319(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.586(4) _cell_angle_gamma 90.00 _cell_volume 1063.97(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3549 _cell_measurement_theta_min 2.8408 _cell_measurement_theta_max 28.7996 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.759 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 3.703 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.5246 _exptl_absorpt_correction_T_max 0.8365 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 4700 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2087 _reflns_number_gt 1924 _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^)+(0.0341P)^2^+0.2446P] 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 2087 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0326 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0714 _refine_ls_wR_factor_gt 0.0696 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.119 _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 0.49127(2) 0.46489(3) 0.20812(4) 0.01460(11) Uani 1 1 d . . . Ag2 Ag 0.41223(2) 0.71853(3) -0.01208(4) 0.01710(12) Uani 1 1 d . . . O4 O 0.3633(2) 1.0310(3) 0.1460(4) 0.0170(6) Uani 1 1 d . . . O2 O 0.1005(2) 0.8569(3) -0.3224(4) 0.0251(7) Uani 1 1 d . . . O3 O 0.3648(2) 0.9345(2) -0.1259(4) 0.0151(6) Uani 1 1 d . . . C2 C 0.1838(3) 1.2952(4) -0.2370(5) 0.0130(8) Uani 1 1 d . . . H2A H 0.1926 1.3818 -0.2449 0.016 Uiso 1 1 calc R . . C4 C 0.0791(3) 1.1180(4) -0.3064(6) 0.0163(9) Uani 1 1 d . . . H4A H 0.0172 1.0807 -0.3631 0.020 Uiso 1 1 calc R . . N1 N 0.1395(2) 0.9162(3) -0.1845(5) 0.0164(8) Uani 1 1 d . . . C5 C 0.1566(3) 1.0490(4) -0.2069(6) 0.0136(8) Uani 1 1 d . . . O1 O 0.1632(2) 0.8732(3) -0.0269(4) 0.0236(7) Uani 1 1 d . . . C6 C 0.2499(3) 1.0959(3) -0.1240(5) 0.0106(8) Uani 1 1 d . . . C3 C 0.0938(3) 1.2437(4) -0.3217(6) 0.0151(8) Uani 1 1 d . . . H3A H 0.0419 1.2941 -0.3904 0.018 Uiso 1 1 calc R . . C8 C 0.3343(3) 1.0135(3) -0.0274(6) 0.0110(8) Uani 1 1 d . . . C1 C 0.2624(3) 1.2236(3) -0.1398(5) 0.0109(8) Uani 1 1 d . . . O5 O 0.4384(2) 1.2228(2) -0.0752(4) 0.0181(7) Uani 1 1 d . . . O6 O 0.3596(2) 1.3833(2) 0.0243(4) 0.0136(6) Uani 1 1 d . . . C7 C 0.3622(3) 1.2821(3) -0.0559(5) 0.0096(8) Uani 1 1 d . . . N2 N 0.2715(3) 0.6267(3) -0.0762(5) 0.0193(8) Uani 1 1 d . . . H2B H 0.2840 0.5461 -0.0527 0.023 Uiso 1 1 d R . . H2C H 0.2409 0.6325 -0.1976 0.023 Uiso 1 1 d R . . H2D H 0.2301 0.6508 -0.0032 0.023 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 0.01262(18) 0.01657(19) 0.01383(18) -0.00399(13) 0.00118(13) -0.00293(12) Ag2 0.01272(18) 0.01403(19) 0.0245(2) -0.00278(13) 0.00402(14) -0.00119(11) O4 0.0127(14) 0.0246(16) 0.0122(14) 0.0011(12) -0.0004(12) 0.0021(12) O2 0.0254(17) 0.0191(16) 0.0292(18) -0.0093(14) 0.0024(15) -0.0097(13) O3 0.0163(14) 0.0118(14) 0.0188(15) 0.0013(13) 0.0073(12) 0.0038(12) C2 0.014(2) 0.0124(19) 0.0133(19) 0.0011(17) 0.0052(17) 0.0017(15) C4 0.0126(19) 0.022(2) 0.014(2) -0.0023(18) 0.0026(17) 0.0002(17) N1 0.0109(16) 0.0150(18) 0.024(2) 0.0015(16) 0.0052(15) -0.0032(14) C5 0.016(2) 0.0122(19) 0.014(2) 0.0011(16) 0.0055(17) 0.0000(16) O1 0.0269(17) 0.0205(16) 0.0217(16) 0.0069(14) 0.0016(14) -0.0032(13) C6 0.0134(19) 0.0133(19) 0.0055(17) -0.0008(15) 0.0030(15) 0.0018(16) C3 0.0097(19) 0.020(2) 0.015(2) 0.0006(17) 0.0010(17) 0.0032(17) C8 0.0083(18) 0.0105(19) 0.015(2) 0.0046(17) 0.0034(16) -0.0041(15) C1 0.0105(19) 0.012(2) 0.0106(18) -0.0021(16) 0.0023(16) 0.0003(15) O5 0.0114(14) 0.0157(15) 0.0264(16) -0.0066(13) 0.0021(13) -0.0006(11) O6 0.0151(14) 0.0111(14) 0.0140(14) -0.0015(12) 0.0019(12) -0.0002(11) C7 0.0119(19) 0.010(2) 0.0065(17) 0.0000(16) 0.0018(15) -0.0011(15) N2 0.0167(18) 0.0150(17) 0.026(2) 0.0005(16) 0.0041(16) -0.0014(14) _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 O4 2.169(3) 2_645 ? Ag1 O6 2.191(3) 1_545 ? Ag1 O3 2.569(3) 4_576 ? Ag1 Ag2 2.9328(4) 3_665 ? Ag1 Ag1 3.2046(6) 3_665 ? Ag1 Ag2 3.2528(4) . ? Ag2 O5 2.107(3) 3_675 ? Ag2 N2 2.131(3) . ? Ag2 O3 2.523(3) . ? Ag2 Ag1 2.9328(4) 3_665 ? O4 C8 1.261(5) . ? O4 Ag1 2.169(3) 2_655 ? O2 N1 1.219(4) . ? O3 C8 1.249(5) . ? O3 Ag1 2.569(3) 4_575 ? C2 C3 1.373(6) . ? C2 C1 1.393(5) . ? C2 H2A 0.9500 . ? C4 C5 1.372(6) . ? C4 C3 1.386(6) . ? C4 H4A 0.9500 . ? N1 O1 1.222(4) . ? N1 C5 1.473(5) . ? C5 C6 1.388(6) . ? C6 C1 1.402(5) . ? C6 C8 1.511(5) . ? C3 H3A 0.9500 . ? C1 C7 1.513(5) . ? O5 C7 1.261(5) . ? O5 Ag2 2.107(3) 3_675 ? O6 C7 1.249(4) . ? O6 Ag1 2.191(3) 1_565 ? N2 H2B 0.8999 . ? N2 H2C 0.9000 . ? N2 H2D 0.9000 . ? 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 O4 Ag1 O6 169.37(10) 2_645 1_545 ? O4 Ag1 O3 105.64(10) 2_645 4_576 ? O6 Ag1 O3 84.91(9) 1_545 4_576 ? O4 Ag1 Ag2 90.05(8) 2_645 3_665 ? O6 Ag1 Ag2 79.90(7) 1_545 3_665 ? O3 Ag1 Ag2 160.63(6) 4_576 3_665 ? O4 Ag1 Ag1 98.03(8) 2_645 3_665 ? O6 Ag1 Ag1 74.51(7) 1_545 3_665 ? O3 Ag1 Ag1 123.27(6) 4_576 3_665 ? Ag2 Ag1 Ag1 63.830(11) 3_665 3_665 ? O4 Ag1 Ag2 97.86(8) 2_645 . ? O6 Ag1 Ag2 83.97(7) 1_545 . ? O3 Ag1 Ag2 71.94(6) 4_576 . ? Ag2 Ag1 Ag2 117.847(11) 3_665 . ? Ag1 Ag1 Ag2 54.017(11) 3_665 . ? O5 Ag2 N2 169.06(12) 3_675 . ? O5 Ag2 O3 89.09(10) 3_675 . ? N2 Ag2 O3 101.81(11) . . ? O5 Ag2 Ag1 80.84(8) 3_675 3_665 ? N2 Ag2 Ag1 93.36(10) . 3_665 ? O3 Ag2 Ag1 125.36(6) . 3_665 ? O5 Ag2 Ag1 84.69(8) 3_675 . ? N2 Ag2 Ag1 84.40(9) . . ? O3 Ag2 Ag1 169.34(7) . . ? Ag1 Ag2 Ag1 62.153(12) 3_665 . ? C8 O4 Ag1 120.1(2) . 2_655 ? C8 O3 Ag2 122.7(2) . . ? C8 O3 Ag1 109.2(2) . 4_575 ? Ag2 O3 Ag1 113.47(10) . 4_575 ? C3 C2 C1 121.6(4) . . ? C3 C2 H2A 119.2 . . ? C1 C2 H2A 119.2 . . ? C5 C4 C3 118.0(4) . . ? C5 C4 H4A 121.0 . . ? C3 C4 H4A 121.0 . . ? O2 N1 O1 124.2(3) . . ? O2 N1 C5 118.3(3) . . ? O1 N1 C5 117.5(3) . . ? C4 C5 C6 124.5(4) . . ? C4 C5 N1 117.9(4) . . ? C6 C5 N1 117.6(3) . . ? C5 C6 C1 116.4(3) . . ? C5 C6 C8 121.8(3) . . ? C1 C6 C8 121.8(3) . . ? C2 C3 C4 119.7(4) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? O3 C8 O4 127.9(4) . . ? O3 C8 C6 116.9(3) . . ? O4 C8 C6 115.2(3) . . ? C2 C1 C6 119.8(3) . . ? C2 C1 C7 120.4(3) . . ? C6 C1 C7 119.8(3) . . ? C7 O5 Ag2 125.9(2) . 3_675 ? C7 O6 Ag1 122.6(2) . 1_565 ? O6 C7 O5 127.6(4) . . ? O6 C7 C1 116.3(3) . . ? O5 C7 C1 116.0(3) . . ? Ag2 N2 H2B 106.7 . . ? Ag2 N2 H2C 113.0 . . ? H2B N2 H2C 106.6 . . ? Ag2 N2 H2D 113.0 . . ? H2B N2 H2D 106.6 . . ? H2C N2 H2D 110.4 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.627 _refine_diff_density_min -0.970 _refine_diff_density_rms 0.181 data_3-42 _database_code_depnum_ccdc_archive 'CCDC 890735' #TrackingRef 'web_deposit_cif_file_0_DiSun_1341553643.p1-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H3 Ag N O6, H4 N, H2 O' _chemical_formula_sum 'C8 H9 Ag N2 O7' _chemical_formula_weight 353.04 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' _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_H-M_alt 'P b c a' _space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.132(3) _cell_length_b 6.9261(14) _cell_length_c 24.512(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2229.5(8) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2354 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 45.21 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.104 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 1.839 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8375 _exptl_absorpt_correction_T_max 0.8375 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 8678 _diffrn_reflns_av_R_equivalents 0.0659 _diffrn_reflns_av_sigmaI/netI 0.0622 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1954 _reflns_number_gt 1654 _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^)+(0.0376P)^2^+7.3978P] 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 1954 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1092 _refine_ls_wR_factor_gt 0.1026 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 0.74147(3) 0.52582(7) 0.237866(14) 0.0356(2) Uani 1 1 d . . . C1 C 0.6280(4) 0.2190(6) 0.42182(19) 0.0222(10) Uani 1 1 d . . . C2 C 0.5909(4) 0.2196(6) 0.47501(18) 0.0264(11) Uani 1 1 d . . . H2A H 0.6353 0.1972 0.5049 0.032 Uiso 1 1 calc R . . C3 C 0.4884(4) 0.2532(7) 0.48358(18) 0.0291(12) Uani 1 1 d . . . H3A H 0.4620 0.2566 0.5196 0.035 Uiso 1 1 calc R . . C4 C 0.4248(4) 0.2818(6) 0.43962(18) 0.0254(10) Uani 1 1 d . . . H4A H 0.3545 0.3061 0.4456 0.030 Uiso 1 1 calc R . . C5 C 0.4623(3) 0.2754(6) 0.38633(17) 0.0188(9) Uani 1 1 d . . . C6 C 0.5653(3) 0.2429(6) 0.37633(18) 0.0187(9) Uani 1 1 d . . . C7 C 0.3873(3) 0.2883(6) 0.33976(18) 0.0215(10) Uani 1 1 d . . . C8 C 0.6068(3) 0.2379(6) 0.31883(18) 0.0201(10) Uani 1 1 d . . . N1 N 0.7386(3) 0.1981(5) 0.41528(17) 0.0242(9) Uani 1 1 d . . . N2 N 0.5120(3) 0.7628(5) 0.30973(15) 0.0241(9) Uani 1 1 d . . . H2C H 0.5488 0.6631 0.3142 0.029 Uiso 1 1 d R . . H2D H 0.4810 0.7523 0.2794 0.029 Uiso 1 1 d R . . H2E H 0.5490 0.8635 0.3096 0.029 Uiso 1 1 d R . . H2B H 0.4692 0.7720 0.3356 0.029 Uiso 1 1 d R . . O1 O 0.3988(2) 0.1756(5) 0.30053(13) 0.0275(7) Uani 1 1 d . . . O2 O 0.3163(2) 0.4127(5) 0.34443(12) 0.0261(7) Uani 1 1 d . . . O1W O 0.3617(3) 0.7630(5) 0.39365(14) 0.0308(8) Uani 1 1 d . . . H1WA H 0.3575 0.6487 0.3996 0.037 Uiso 1 1 d R . . H1WB H 0.3112 0.8268 0.3896 0.037 Uiso 1 1 d R . . O3 O 0.6031(2) 0.3908(4) 0.29147(12) 0.0232(7) Uani 1 1 d . . . O4 O 0.6405(2) 0.0778(4) 0.30223(12) 0.0255(7) Uani 1 1 d . . . O5 O 0.7781(3) 0.2695(5) 0.37476(16) 0.0342(9) Uani 1 1 d . . . O6 O 0.7857(3) 0.1138(5) 0.45139(14) 0.0355(8) 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 0.0185(3) 0.0658(4) 0.0225(3) 0.00630(18) -0.00091(14) 0.00391(17) C1 0.015(2) 0.024(2) 0.028(2) -0.0001(19) -0.0010(19) 0.0014(18) C2 0.032(3) 0.031(3) 0.017(2) 0.0015(19) -0.005(2) 0.002(2) C3 0.031(3) 0.038(3) 0.019(2) 0.002(2) 0.004(2) 0.002(2) C4 0.021(3) 0.030(2) 0.025(2) -0.002(2) 0.002(2) -0.0016(19) C5 0.016(2) 0.022(2) 0.018(2) -0.0002(17) 0.0000(17) -0.0009(17) C6 0.016(2) 0.019(2) 0.021(2) 0.0013(17) 0.0014(18) 0.0006(17) C7 0.014(2) 0.027(2) 0.023(2) 0.003(2) 0.0002(18) -0.0047(18) C8 0.013(2) 0.026(2) 0.021(2) 0.0022(19) -0.0008(18) -0.0026(18) N1 0.021(2) 0.022(2) 0.030(2) -0.0041(18) -0.0039(17) 0.0031(16) N2 0.021(2) 0.025(2) 0.0260(19) -0.0004(16) 0.0024(17) -0.0013(16) O1 0.0196(18) 0.0344(18) 0.0285(17) -0.0113(15) -0.0026(13) -0.0017(14) O2 0.0196(17) 0.0334(18) 0.0252(16) 0.0002(14) -0.0040(13) 0.0055(14) O1W 0.024(2) 0.0356(19) 0.0326(19) 0.0023(15) 0.0005(15) 0.0042(14) O3 0.0211(18) 0.0261(17) 0.0225(15) 0.0049(14) 0.0038(13) 0.0011(13) O4 0.0263(19) 0.0199(16) 0.0303(17) -0.0018(14) 0.0096(14) 0.0035(14) O5 0.024(2) 0.039(2) 0.040(2) 0.0055(16) 0.0050(17) -0.0013(15) O6 0.030(2) 0.040(2) 0.0361(19) -0.0012(17) -0.0140(16) 0.0087(16) _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 O4 2.241(3) 8_765 ? Ag1 O1 2.314(3) 3_655 ? Ag1 O2 2.377(3) 6_656 ? Ag1 O3 2.430(3) . ? C1 C2 1.392(7) . ? C1 C6 1.396(6) . ? C1 N1 1.469(6) . ? C2 C3 1.381(7) . ? C2 H2A 0.9500 . ? C3 C4 1.378(7) . ? C3 H3A 0.9500 . ? C4 C5 1.396(6) . ? C4 H4A 0.9500 . ? C5 C6 1.393(6) . ? C5 C7 1.510(6) . ? C6 C8 1.512(6) . ? C7 O1 1.248(5) . ? C7 O2 1.274(6) . ? C8 O3 1.254(5) . ? C8 O4 1.261(5) . ? N1 O5 1.225(5) . ? N1 O6 1.228(5) . ? N2 H2C 0.8500 . ? N2 H2D 0.8499 . ? N2 H2E 0.8500 . ? N2 H2B 0.8499 . ? O1 Ag1 2.314(3) 3_645 ? O2 Ag1 2.377(3) 6_556 ? O1W H1WA 0.8069 . ? O1W H1WB 0.8029 . ? O4 Ag1 2.241(3) 8_755 ? 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 O4 Ag1 O1 139.91(12) 8_765 3_655 ? O4 Ag1 O2 111.36(12) 8_765 6_656 ? O1 Ag1 O2 97.58(11) 3_655 6_656 ? O4 Ag1 O3 101.45(11) 8_765 . ? O1 Ag1 O3 78.29(11) 3_655 . ? O2 Ag1 O3 129.90(11) 6_656 . ? C2 C1 C6 122.8(5) . . ? C2 C1 N1 116.7(4) . . ? C6 C1 N1 120.5(4) . . ? C3 C2 C1 118.9(4) . . ? C3 C2 H2A 120.5 . . ? C1 C2 H2A 120.5 . . ? C2 C3 C4 119.7(4) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? C3 C4 C5 120.9(5) . . ? C3 C4 H4A 119.5 . . ? C5 C4 H4A 119.5 . . ? C6 C5 C4 120.8(4) . . ? C6 C5 C7 120.6(4) . . ? C4 C5 C7 118.4(4) . . ? C5 C6 C1 116.8(4) . . ? C5 C6 C8 121.2(4) . . ? C1 C6 C8 122.0(4) . . ? O1 C7 O2 125.5(4) . . ? O1 C7 C5 117.8(4) . . ? O2 C7 C5 116.7(4) . . ? O3 C8 O4 125.7(4) . . ? O3 C8 C6 117.7(4) . . ? O4 C8 C6 116.6(4) . . ? O5 N1 O6 124.3(4) . . ? O5 N1 C1 117.9(4) . . ? O6 N1 C1 117.8(4) . . ? H2C N2 H2D 108.4 . . ? H2C N2 H2E 110.0 . . ? H2D N2 H2E 110.0 . . ? H2C N2 H2B 110.0 . . ? H2D N2 H2B 110.0 . . ? H2E N2 H2B 108.5 . . ? C7 O1 Ag1 119.8(3) . 3_645 ? C7 O2 Ag1 116.7(3) . 6_556 ? H1WA O1W H1WB 120.4 . . ? C8 O3 Ag1 125.8(3) . . ? C8 O4 Ag1 127.6(3) . 8_755 ? 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 N2 H2C O3 0.85 2.09 2.875(5) 153.2 . N2 H2E O4 0.85 1.92 2.764(5) 173.3 1_565 N2 H2D O3 0.85 2.27 3.037(5) 149.9 3_655 N2 H2B O1W 0.85 2.01 2.851(5) 173.1 . O1W H1WB O2 0.80 2.09 2.828(5) 151.9 8_665 O1W H1WA O2 0.81 2.19 2.774(5) 129.7 . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.656 _refine_diff_density_min -1.224 _refine_diff_density_rms 0.131 data_4-53 _database_code_depnum_ccdc_archive 'CCDC 890736' #TrackingRef 'web_deposit_cif_file_0_DiSun_1341553643.p1-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H18 Ag4 N6 O12, H2 O' _chemical_formula_sum 'C16 H20 Ag4 N6 O13' _chemical_formula_weight 935.86 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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' 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 6.7018(13) _cell_length_b 22.923(5) _cell_length_c 15.748(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.49(3) _cell_angle_gamma 90.00 _cell_volume 2403.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15656 _cell_measurement_theta_min 6.12 _cell_measurement_theta_max 55.00 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 3.291 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5590 _exptl_absorpt_correction_T_max 0.8527 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 25577 _diffrn_reflns_av_R_equivalents 0.0896 _diffrn_reflns_av_sigmaI/netI 0.0596 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4211 _reflns_number_gt 3242 _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^)+(0.0543P)^2^+2.2395P] 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 0.00054(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4211 _refine_ls_number_parameters 360 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0576 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1141 _refine_ls_wR_factor_gt 0.0991 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 0.61640(8) 0.51204(2) 0.82585(3) 0.02757(17) Uani 1 1 d . . . Ag2 Ag 0.88212(8) 0.500145(19) 0.68427(3) 0.02664(17) Uani 1 1 d . . . Ag3 Ag 0.5000 0.5000 1.0000 0.0305(2) Uani 1 2 d S . . Ag4 Ag 1.0000 0.5000 0.5000 0.0305(2) Uani 1 2 d S . . Ag5 Ag 0.38840(8) 0.502047(19) 0.64184(3) 0.03257(19) Uani 1 1 d . . . C1 C 0.2098(8) 0.3554(2) 0.7994(4) 0.0202(13) Uani 1 1 d . . . C2 C 0.1796(9) 0.3073(3) 0.7455(4) 0.0280(15) Uani 1 1 d . . . H2A H 0.1807 0.3124 0.6857 0.034 Uiso 1 1 calc R . . C3 C 0.1478(10) 0.2520(3) 0.7772(4) 0.0313(16) Uani 1 1 d . . . H3A H 0.1250 0.2199 0.7392 0.038 Uiso 1 1 calc R . . C4 C 0.1493(9) 0.2437(3) 0.8634(4) 0.0275(15) Uani 1 1 d . . . H4A H 0.1310 0.2058 0.8855 0.033 Uiso 1 1 calc R . . C5 C 0.1778(9) 0.2913(3) 0.9182(4) 0.0255(14) Uani 1 1 d . . . C6 C 0.2071(8) 0.3481(2) 0.8887(4) 0.0189(13) Uani 1 1 d . . . C7 C 0.2496(8) 0.4139(3) 0.7617(4) 0.0235(14) Uani 1 1 d . . . C8 C 0.2467(9) 0.4003(3) 0.9472(4) 0.0230(14) Uani 1 1 d . . . C11 C 0.3121(10) 0.7758(3) 0.4960(4) 0.0293(15) Uani 1 1 d . . . H11A H 0.3060 0.8151 0.5150 0.035 Uiso 1 1 calc R . . C12 C 0.2931(10) 0.7627(3) 0.4096(4) 0.0306(15) Uani 1 1 d . . . H12A H 0.2803 0.7933 0.3686 0.037 Uiso 1 1 calc R . . C13 C 0.2928(9) 0.7052(3) 0.3827(4) 0.0280(15) Uani 1 1 d . . . H13A H 0.2724 0.6964 0.3234 0.034 Uiso 1 1 calc R . . C14 C 0.3223(8) 0.6602(2) 0.4422(4) 0.0207(13) Uani 1 1 d . . . C15 C 0.3538(8) 0.6724(2) 0.5307(4) 0.0201(13) Uani 1 1 d . . . C16 C 0.3400(9) 0.7307(3) 0.5536(4) 0.0222(13) Uani 1 1 d . . . C17 C 0.3141(9) 0.5977(3) 0.4110(4) 0.0238(14) Uani 1 1 d . . . C18 C 0.4069(9) 0.6235(3) 0.5936(4) 0.0223(13) Uani 1 1 d . . . N1 N 0.1856(8) 0.2794(2) 1.0104(3) 0.0286(12) Uani 1 1 d . . . N2 N 0.3463(8) 0.7459(2) 0.6456(3) 0.0267(12) Uani 1 1 d . . . N3 N 0.7355(8) 0.4266(2) 0.8424(3) 0.0277(12) Uani 1 1 d . . . H3B H 0.8545 0.4280 0.8765 0.041 Uiso 1 1 calc R . . H3C H 0.7556 0.4115 0.7906 0.041 Uiso 1 1 calc R . . H3D H 0.6476 0.4037 0.8672 0.041 Uiso 1 1 calc R . . N4 N 0.4971(8) 0.5982(2) 0.8235(3) 0.0329(13) Uani 1 1 d . . . H4B H 0.5806 0.6217 0.8579 0.049 Uiso 1 1 calc R . . H4C H 0.3738 0.5977 0.8425 0.049 Uiso 1 1 calc R . . H4D H 0.4858 0.6122 0.7691 0.049 Uiso 1 1 calc R . . N5 N 0.9521(7) 0.5879(2) 0.7218(3) 0.0257(12) Uani 1 1 d . . . H5A H 1.0587 0.6005 0.6957 0.039 Uiso 1 1 calc R . . H5B H 0.9834 0.5895 0.7795 0.039 Uiso 1 1 calc R . . H5C H 0.8441 0.6111 0.7061 0.039 Uiso 1 1 calc R . . N6 N 0.8696(8) 0.5848(2) 0.4896(3) 0.0324(13) Uani 1 1 d . . . H6A H 0.8452 0.5949 0.4335 0.049 Uiso 1 1 calc R . . H6B H 0.9557 0.6110 0.5174 0.049 Uiso 1 1 calc R . . H6C H 0.7522 0.5847 0.5135 0.049 Uiso 1 1 calc R . . O1 O 0.2014(6) 0.45962(18) 0.7980(3) 0.0307(10) Uani 1 1 d . . . O1W O -0.1286(6) 0.44094(19) 1.1015(3) 0.0340(11) Uani 1 1 d . . . H1WA H -0.0514 0.4439 1.0625 0.041 Uiso 1 1 d R . . H1WB H -0.1356 0.4739 1.1257 0.041 Uiso 1 1 d R . . O2 O 0.3303(6) 0.41313(17) 0.6933(3) 0.0292(10) Uani 1 1 d . . . O3 O 0.1058(6) 0.42922(19) 0.9693(3) 0.0320(11) Uani 1 1 d . . . O4 O 0.4337(6) 0.41047(17) 0.9659(3) 0.0263(10) Uani 1 1 d . . . O5 O 0.2040(7) 0.3202(2) 1.0604(3) 0.0390(12) Uani 1 1 d . . . O6 O 0.1702(8) 0.2282(2) 1.0328(3) 0.0426(13) Uani 1 1 d . . . O7 O 0.1863(6) 0.58913(18) 0.3455(3) 0.0284(10) Uani 1 1 d . . . O8 O 0.4217(6) 0.55933(17) 0.4492(2) 0.0273(10) Uani 1 1 d . . . O9 O 0.2632(6) 0.59095(17) 0.6099(3) 0.0256(10) Uani 1 1 d . . . O10 O 0.5848(6) 0.61813(19) 0.6226(3) 0.0334(11) Uani 1 1 d . . . O11 O 0.3536(7) 0.79763(19) 0.6650(3) 0.0365(11) Uani 1 1 d . . . O12 O 0.3370(7) 0.70639(19) 0.6969(3) 0.0378(12) 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 0.0294(3) 0.0300(3) 0.0239(3) 0.0015(2) 0.0056(2) 0.0029(2) Ag2 0.0289(3) 0.0273(3) 0.0239(3) -0.00300(19) 0.0041(2) -0.0022(2) Ag3 0.0432(5) 0.0263(4) 0.0226(4) -0.0045(3) 0.0066(3) -0.0107(3) Ag4 0.0275(4) 0.0405(5) 0.0234(4) 0.0008(3) 0.0030(3) 0.0038(3) Ag5 0.0449(4) 0.0227(3) 0.0298(3) 0.0023(2) 0.0024(3) 0.0026(2) C1 0.018(3) 0.020(3) 0.023(3) 0.002(2) 0.003(3) -0.001(2) C2 0.030(4) 0.028(4) 0.025(4) -0.004(3) 0.000(3) 0.001(3) C3 0.044(4) 0.021(3) 0.028(4) -0.006(3) 0.000(3) -0.001(3) C4 0.025(4) 0.026(3) 0.032(4) 0.001(3) 0.001(3) 0.002(3) C5 0.023(3) 0.029(3) 0.024(3) 0.002(3) 0.000(3) 0.005(3) C6 0.011(3) 0.021(3) 0.024(3) -0.002(3) 0.002(2) -0.002(2) C7 0.014(3) 0.035(4) 0.021(3) -0.002(3) -0.001(3) 0.000(3) C8 0.025(4) 0.027(3) 0.017(3) 0.006(3) 0.004(3) -0.001(3) C11 0.035(4) 0.020(3) 0.032(4) -0.004(3) 0.000(3) 0.000(3) C12 0.041(4) 0.020(3) 0.031(4) 0.008(3) 0.003(3) -0.006(3) C13 0.026(3) 0.037(4) 0.021(3) 0.001(3) 0.004(3) -0.001(3) C14 0.018(3) 0.023(3) 0.021(3) 0.001(3) 0.004(3) -0.004(2) C15 0.013(3) 0.024(3) 0.024(3) 0.006(3) 0.004(2) -0.002(2) C16 0.021(3) 0.025(3) 0.020(3) 0.002(3) 0.000(3) -0.001(3) C17 0.024(3) 0.028(3) 0.020(3) -0.005(3) 0.008(3) -0.003(3) C18 0.025(3) 0.021(3) 0.021(3) -0.004(3) 0.003(3) 0.004(3) N1 0.027(3) 0.031(3) 0.027(3) 0.004(3) 0.001(2) -0.003(3) N2 0.027(3) 0.030(3) 0.023(3) -0.003(2) 0.005(2) 0.001(2) N3 0.028(3) 0.031(3) 0.025(3) 0.002(2) 0.005(2) 0.001(2) N4 0.038(3) 0.029(3) 0.032(3) -0.003(2) 0.005(3) 0.002(3) N5 0.020(3) 0.030(3) 0.027(3) 0.002(2) 0.001(2) 0.004(2) N6 0.030(3) 0.037(3) 0.030(3) -0.002(3) 0.005(2) 0.003(3) O1 0.041(3) 0.024(2) 0.027(2) -0.001(2) 0.004(2) 0.001(2) O1W 0.039(3) 0.039(3) 0.026(2) -0.001(2) 0.013(2) -0.001(2) O2 0.037(3) 0.022(2) 0.029(3) 0.0036(19) 0.009(2) -0.001(2) O3 0.033(3) 0.034(3) 0.030(3) -0.005(2) 0.009(2) 0.006(2) O4 0.027(2) 0.027(2) 0.024(2) -0.0055(18) 0.0022(19) -0.0007(19) O5 0.053(3) 0.042(3) 0.022(2) -0.002(2) 0.003(2) -0.014(2) O6 0.060(3) 0.034(3) 0.034(3) 0.013(2) 0.007(2) -0.001(3) O7 0.030(3) 0.029(2) 0.025(2) -0.0050(18) -0.002(2) -0.0010(19) O8 0.033(2) 0.026(2) 0.023(2) -0.0020(19) 0.0033(19) 0.002(2) O9 0.032(2) 0.021(2) 0.025(2) 0.0036(18) 0.007(2) -0.0013(19) O10 0.026(3) 0.042(3) 0.032(3) 0.005(2) -0.001(2) 0.006(2) O11 0.050(3) 0.026(3) 0.034(3) -0.010(2) 0.005(2) -0.002(2) O12 0.060(3) 0.027(2) 0.028(3) 0.005(2) 0.011(2) -0.007(2) _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 2.119(5) . ? Ag1 N4 2.131(5) . ? Ag1 Ag3 2.9478(8) . ? Ag1 Ag2 3.0188(11) . ? Ag1 Ag5 3.1277(12) . ? Ag2 N5 2.134(5) . ? Ag2 O7 2.138(4) 3_666 ? Ag2 Ag4 3.0924(8) . ? Ag2 Ag5 3.3010(10) . ? Ag3 O4 2.155(4) . ? Ag3 O4 2.155(4) 3_667 ? Ag3 Ag1 2.9478(8) 3_667 ? Ag4 N6 2.130(5) . ? Ag4 N6 2.130(5) 3_766 ? Ag4 Ag2 3.0924(8) 3_766 ? Ag4 Ag5 3.2331(12) 3_666 ? Ag4 Ag5 3.2331(12) 1_655 ? Ag5 O9 2.239(4) . ? Ag5 O2 2.244(4) . ? Ag5 O8 2.463(4) 3_666 ? Ag5 Ag4 3.2331(12) 1_455 ? C1 C2 1.392(8) . ? C1 C6 1.417(8) . ? C1 C7 1.504(8) . ? C2 C3 1.387(8) . ? C2 H2A 0.9500 . ? C3 C4 1.369(9) . ? C3 H3A 0.9500 . ? C4 C5 1.390(8) . ? C4 H4A 0.9500 . ? C5 C6 1.403(8) . ? C5 N1 1.473(8) . ? C6 C8 1.515(8) . ? C7 O1 1.253(7) . ? C7 O2 1.259(7) . ? C8 O3 1.236(7) . ? C8 O4 1.276(7) . ? C11 C16 1.375(8) . ? C11 C12 1.385(9) . ? C11 H11A 0.9500 . ? C12 C13 1.385(8) . ? C12 H12A 0.9500 . ? C13 C14 1.394(8) . ? C13 H13A 0.9500 . ? C14 C15 1.414(8) . ? C14 C17 1.514(8) . ? C15 C16 1.388(8) . ? C15 C18 1.512(8) . ? C16 N2 1.487(7) . ? C17 O8 1.248(7) . ? C17 O7 1.279(7) . ? C18 O10 1.234(7) . ? C18 O9 1.267(7) . ? N1 O5 1.220(6) . ? N1 O6 1.234(6) . ? N2 O12 1.220(6) . ? N2 O11 1.224(7) . ? N3 H3B 0.9100 . ? N3 H3C 0.9100 . ? N3 H3D 0.9100 . ? N4 H4B 0.9100 . ? N4 H4C 0.9100 . ? N4 H4D 0.9100 . ? N5 H5A 0.9100 . ? N5 H5B 0.9100 . ? N5 H5C 0.9100 . ? N6 H6A 0.9100 . ? N6 H6B 0.9100 . ? N6 H6C 0.9100 . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8498 . ? O7 Ag2 2.138(4) 3_666 ? O8 Ag5 2.463(4) 3_666 ? 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 N4 173.94(19) . . ? N3 Ag1 Ag3 86.24(13) . . ? N4 Ag1 Ag3 87.98(14) . . ? N3 Ag1 Ag2 76.24(13) . . ? N4 Ag1 Ag2 108.82(14) . . ? Ag3 Ag1 Ag2 156.76(2) . . ? N3 Ag1 Ag5 100.62(14) . . ? N4 Ag1 Ag5 84.76(14) . . ? Ag3 Ag1 Ag5 134.60(2) . . ? Ag2 Ag1 Ag5 64.94(2) . . ? N5 Ag2 O7 176.64(17) . 3_666 ? N5 Ag2 Ag1 80.80(13) . . ? O7 Ag2 Ag1 96.82(11) 3_666 . ? N5 Ag2 Ag4 100.91(13) . . ? O7 Ag2 Ag4 82.20(11) 3_666 . ? Ag1 Ag2 Ag4 158.08(2) . . ? N5 Ag2 Ag5 103.15(13) . . ? O7 Ag2 Ag5 77.46(11) 3_666 . ? Ag1 Ag2 Ag5 59.13(3) . . ? Ag4 Ag2 Ag5 99.59(3) . . ? O4 Ag3 O4 180.000(2) . 3_667 ? O4 Ag3 Ag1 85.77(11) . . ? O4 Ag3 Ag1 94.23(11) 3_667 . ? O4 Ag3 Ag1 94.23(11) . 3_667 ? O4 Ag3 Ag1 85.77(11) 3_667 3_667 ? Ag1 Ag3 Ag1 180.0 . 3_667 ? N6 Ag4 N6 180.000(2) . 3_766 ? N6 Ag4 Ag2 85.71(14) . . ? N6 Ag4 Ag2 94.29(14) 3_766 . ? N6 Ag4 Ag2 94.29(14) . 3_766 ? N6 Ag4 Ag2 85.71(14) 3_766 3_766 ? Ag2 Ag4 Ag2 180.0 . 3_766 ? N6 Ag4 Ag5 70.66(14) . 3_666 ? N6 Ag4 Ag5 109.34(14) 3_766 3_666 ? Ag2 Ag4 Ag5 112.16(2) . 3_666 ? Ag2 Ag4 Ag5 67.84(2) 3_766 3_666 ? N6 Ag4 Ag5 109.34(14) . 1_655 ? N6 Ag4 Ag5 70.66(14) 3_766 1_655 ? Ag2 Ag4 Ag5 67.84(2) . 1_655 ? Ag2 Ag4 Ag5 112.16(2) 3_766 1_655 ? Ag5 Ag4 Ag5 180.0 3_666 1_655 ? O9 Ag5 O2 146.30(15) . . ? O9 Ag5 O8 126.45(14) . 3_666 ? O2 Ag5 O8 79.26(14) . 3_666 ? O9 Ag5 Ag1 105.83(11) . . ? O2 Ag5 Ag1 79.54(11) . . ? O8 Ag5 Ag1 110.52(10) 3_666 . ? O9 Ag5 Ag4 66.80(11) . 1_455 ? O2 Ag5 Ag4 94.44(11) . 1_455 ? O8 Ag5 Ag4 91.05(10) 3_666 1_455 ? Ag1 Ag5 Ag4 155.78(2) . 1_455 ? O9 Ag5 Ag2 113.51(11) . . ? O2 Ag5 Ag2 97.23(11) . . ? O8 Ag5 Ag2 62.49(10) 3_666 . ? Ag1 Ag5 Ag2 55.94(3) . . ? Ag4 Ag5 Ag2 148.21(2) 1_455 . ? C2 C1 C6 119.6(5) . . ? C2 C1 C7 119.1(5) . . ? C6 C1 C7 121.3(5) . . ? C3 C2 C1 121.4(6) . . ? C3 C2 H2A 119.3 . . ? C1 C2 H2A 119.3 . . ? C4 C3 C2 119.9(6) . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C3 C4 C5 119.5(6) . . ? C3 C4 H4A 120.3 . . ? C5 C4 H4A 120.3 . . ? C4 C5 C6 122.5(6) . . ? C4 C5 N1 117.0(5) . . ? C6 C5 N1 120.5(5) . . ? C5 C6 C1 117.1(5) . . ? C5 C6 C8 123.5(5) . . ? C1 C6 C8 119.3(5) . . ? O1 C7 O2 124.0(6) . . ? O1 C7 C1 120.0(5) . . ? O2 C7 C1 116.0(5) . . ? O3 C8 O4 126.8(6) . . ? O3 C8 C6 120.5(5) . . ? O4 C8 C6 112.7(5) . . ? C16 C11 C12 118.4(6) . . ? C16 C11 H11A 120.8 . . ? C12 C11 H11A 120.8 . . ? C13 C12 C11 120.3(6) . . ? C13 C12 H12A 119.9 . . ? C11 C12 H12A 119.9 . . ? C12 C13 C14 120.3(6) . . ? C12 C13 H13A 119.9 . . ? C14 C13 H13A 119.9 . . ? C13 C14 C15 120.7(5) . . ? C13 C14 C17 119.0(5) . . ? C15 C14 C17 120.3(5) . . ? C16 C15 C14 116.1(5) . . ? C16 C15 C18 124.1(5) . . ? C14 C15 C18 119.8(5) . . ? C11 C16 C15 124.1(6) . . ? C11 C16 N2 116.9(5) . . ? C15 C16 N2 118.9(5) . . ? O8 C17 O7 125.3(5) . . ? O8 C17 C14 120.9(5) . . ? O7 C17 C14 113.8(5) . . ? O10 C18 O9 126.2(6) . . ? O10 C18 C15 117.6(5) . . ? O9 C18 C15 116.2(5) . . ? O5 N1 O6 123.4(5) . . ? O5 N1 C5 119.0(5) . . ? O6 N1 C5 117.6(5) . . ? O12 N2 O11 123.9(5) . . ? O12 N2 C16 118.2(5) . . ? O11 N2 C16 117.9(5) . . ? Ag1 N3 H3B 109.5 . . ? Ag1 N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? Ag1 N3 H3D 109.5 . . ? H3B N3 H3D 109.5 . . ? H3C N3 H3D 109.5 . . ? Ag1 N4 H4B 109.5 . . ? Ag1 N4 H4C 109.5 . . ? H4B N4 H4C 109.5 . . ? Ag1 N4 H4D 109.5 . . ? H4B N4 H4D 109.5 . . ? H4C N4 H4D 109.5 . . ? Ag2 N5 H5A 109.5 . . ? Ag2 N5 H5B 109.5 . . ? H5A N5 H5B 109.5 . . ? Ag2 N5 H5C 109.5 . . ? H5A N5 H5C 109.5 . . ? H5B N5 H5C 109.5 . . ? Ag4 N6 H6A 109.5 . . ? Ag4 N6 H6B 109.5 . . ? H6A N6 H6B 109.5 . . ? Ag4 N6 H6C 109.5 . . ? H6A N6 H6C 109.5 . . ? H6B N6 H6C 109.5 . . ? H1WA O1W H1WB 108.7 . . ? C7 O2 Ag5 113.9(4) . . ? C8 O4 Ag3 113.7(4) . . ? C17 O7 Ag2 115.6(4) . 3_666 ? C17 O8 Ag5 115.5(4) . 3_666 ? C18 O9 Ag5 107.9(4) . . ? 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 N3 H3B O3 0.91 2.10 3.005(7) 172.1 1_655 N3 H3C O7 0.91 2.22 3.085(6) 158.0 3_666 N3 H3D O11 0.91 2.48 3.017(7) 117.7 2_646 N4 H4B O5 0.91 2.26 3.166(7) 177.9 3_667 N4 H4D O10 0.91 2.47 3.314(7) 153.5 . N4 H4C O1W 0.91 2.14 2.993(7) 155.3 3_567 N5 H5A O9 0.91 2.04 2.879(6) 152.1 1_655 N5 H5C O10 0.91 2.06 2.848(6) 143.6 . N6 H6A O2 0.91 2.21 3.037(7) 151.2 3_666 N6 H6B O9 0.91 2.43 3.072(7) 127.7 1_655 N6 H6C O8 0.91 2.40 3.054(7) 128.7 . O1W H1WA O3 0.85 1.93 2.760(6) 164.9 . O1W H1WB O1 0.85 2.02 2.848(6) 164.5 3_567 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.242 _refine_diff_density_min -1.277 _refine_diff_density_rms 0.176