# 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_a1 _database_code_depnum_ccdc_archive 'CCDC 892432' #TrackingRef '1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H42 Ag4 N8 O4, 2(N O3), 10(H2 O)' _chemical_formula_sum 'C48 H62 Ag4 N10 O20' _chemical_formula_weight 1530.56 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 Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.143(4) _cell_length_b 11.404(4) _cell_length_c 14.197(6) _cell_angle_alpha 104.95(4) _cell_angle_beta 107.92(3) _cell_angle_gamma 104.48(4) _cell_volume 1409.5(10) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4952 _cell_measurement_theta_min 3.0042 _cell_measurement_theta_max 27.4855 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.803 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 1.453 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.4967 _exptl_absorpt_correction_T_max 0.8450 _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 ; Rigaku Mercury CCD Saturn724 ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number None _diffrn_standards_interval_count None _diffrn_standards_interval_time None _diffrn_standards_decay_% None _diffrn_reflns_number 6199 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4869 _reflns_number_gt 4628 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _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^)+(0.0309P)^2^+3.7590P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4869 _refine_ls_number_parameters 344 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.0959 _refine_ls_wR_factor_gt 0.0942 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.071 _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 0.00942(4) 0.04722(3) 0.13098(3) 0.04467(12) Uani 1 1 d . . . Ag2 Ag 0.31074(5) 0.24877(3) 0.35179(3) 0.05472(14) Uani 1 1 d . . . N4 N 0.3211(4) 1.0696(3) 0.3751(3) 0.0405(8) Uani 1 1 d . . . N3 N 0.3264(4) 0.4505(3) 0.3829(3) 0.0409(8) Uani 1 1 d . . . N2 N 0.0012(4) 0.8562(3) 0.1329(3) 0.0370(8) Uani 1 1 d . . . N1 N 0.0132(4) 0.2417(3) 0.1467(3) 0.0356(8) Uani 1 1 d . . . C16 C 0.4245(5) 1.0247(4) 0.3571(3) 0.0390(9) Uani 1 1 d . . . H16A H 0.4940 1.0750 0.3397 0.047 Uiso 1 1 calc R . . C17 C 0.4335(5) 0.9081(4) 0.3630(3) 0.0356(9) Uani 1 1 d . . . H17A H 0.5074 0.8813 0.3494 0.043 Uiso 1 1 calc R . . C18 C 0.3316(4) 0.8301(4) 0.3894(3) 0.0328(8) Uani 1 1 d . . . C19 C 0.2261(5) 0.8789(4) 0.4101(4) 0.0412(10) Uani 1 1 d . . . H19A H 0.1565 0.8318 0.4292 0.049 Uiso 1 1 calc R . . C20 C 0.2244(5) 0.9957(4) 0.4025(4) 0.0460(11) Uani 1 1 d . . . H20A H 0.1528 1.0256 0.4169 0.055 Uiso 1 1 calc R . . C15 C 0.2252(6) 0.4959(4) 0.4032(4) 0.0476(11) Uani 1 1 d . . . H15A H 0.1509 0.4422 0.4147 0.057 Uiso 1 1 calc R . . C14 C 0.2244(6) 0.6178(4) 0.4081(4) 0.0470(11) Uani 1 1 d . . . H14A H 0.1505 0.6442 0.4221 0.056 Uiso 1 1 calc R . . C13 C 0.3337(5) 0.7013(4) 0.3922(3) 0.0325(8) Uani 1 1 d . . . C12 C 0.4415(5) 0.6556(4) 0.3750(4) 0.0435(10) Uani 1 1 d . . . H12A H 0.5196 0.7086 0.3665 0.052 Uiso 1 1 calc R . . C11 C 0.4336(5) 0.5317(4) 0.3703(4) 0.0484(11) Uani 1 1 d . . . H11A H 0.5071 0.5033 0.3578 0.058 Uiso 1 1 calc R . . C6 C 0.1144(4) 0.8186(4) 0.1278(3) 0.0345(9) Uani 1 1 d . . . H6A H 0.1928 0.8753 0.1222 0.041 Uiso 1 1 calc R . . C7 C 0.1208(4) 0.7005(4) 0.1304(3) 0.0328(8) Uani 1 1 d . . . H7A H 0.2019 0.6788 0.1264 0.039 Uiso 1 1 calc R . . C8 C 0.0054(4) 0.6133(4) 0.1391(3) 0.0298(8) Uani 1 1 d . . . C9 C -0.1119(5) 0.6532(4) 0.1441(4) 0.0430(10) Uani 1 1 d . . . H9A H -0.1918 0.5987 0.1499 0.052 Uiso 1 1 calc R . . C10 C -0.1103(5) 0.7721(4) 0.1406(4) 0.0474(11) Uani 1 1 d . . . H10A H -0.1905 0.7959 0.1438 0.057 Uiso 1 1 calc R . . C5 C -0.0920(5) 0.2848(4) 0.1638(4) 0.0411(10) Uani 1 1 d . . . H5A H -0.1642 0.2320 0.1775 0.049 Uiso 1 1 calc R . . C4 C -0.0987(5) 0.4035(4) 0.1619(4) 0.0399(10) Uani 1 1 d . . . H4A H -0.1744 0.4288 0.1736 0.048 Uiso 1 1 calc R . . C3 C 0.0087(4) 0.4855(3) 0.1425(3) 0.0289(8) Uani 1 1 d . . . C2 C 0.1182(4) 0.4401(4) 0.1261(3) 0.0316(8) Uani 1 1 d . . . H2A H 0.1926 0.4914 0.1132 0.038 Uiso 1 1 calc R . . C1 C 0.1174(4) 0.3210(4) 0.1289(3) 0.0348(9) Uani 1 1 d . . . H1A H 0.1923 0.2936 0.1179 0.042 Uiso 1 1 calc R . . C21 C 0.3632(5) 0.1334(4) 0.1247(4) 0.0410(10) Uani 1 1 d . . . C22 C 0.4181(5) 0.0777(4) -0.0391(4) 0.0431(10) Uani 1 1 d . . . H22A H 0.4154 0.1598 -0.0454 0.052 Uiso 1 1 calc R . . H22B H 0.3183 0.0137 -0.0783 0.052 Uiso 1 1 calc R . . C23 C 0.4680(5) 0.0928(4) 0.0768(3) 0.0351(9) Uani 1 1 d . . . H23A H 0.5670 0.1605 0.1160 0.042 Uiso 1 1 calc R . . C24 C 0.4786(5) -0.0353(5) 0.0876(4) 0.0459(11) Uani 1 1 d . . . H24A H 0.5156 -0.0243 0.1622 0.055 Uiso 1 1 calc R . . H24B H 0.3806 -0.1024 0.0522 0.055 Uiso 1 1 calc R . . O1 O 0.2284(4) 0.0682(3) 0.0785(3) 0.0576(9) Uani 1 1 d . . . O2 O 0.4209(4) 0.2327(4) 0.2098(3) 0.0643(10) Uani 1 1 d . . . OW1 O 0.4691(5) 0.5822(4) 0.9015(4) 0.0839(13) Uani 1 1 d . . . H1 H 0.5246 0.6497 0.8987 0.101 Uiso 1 1 d R . . H2 H 0.5094 0.5250 0.8991 0.101 Uiso 1 1 d R . . OW2 O 0.5662(4) 0.3709(4) 0.9000(3) 0.0701(11) Uani 1 1 d . . . H3 H 0.4853 0.3161 0.8501 0.084 Uiso 1 1 d R . . H4 H 0.5609 0.3732 0.9590 0.084 Uiso 1 1 d R . . OW3 O 0.3152(5) 0.1933(4) 0.7165(4) 0.0800(12) Uani 1 1 d . . . H5 H 0.2607 0.1152 0.6987 0.096 Uiso 1 1 d R . . H6 H 0.2650 0.2305 0.6835 0.096 Uiso 1 1 d R . . OW4 O 0.1800(6) 0.3449(5) 0.6225(4) 0.116(2) Uani 1 1 d . . . H7 H 0.1062 0.3166 0.5634 0.139 Uiso 1 1 d R . . H8 H 0.2284 0.4240 0.6361 0.139 Uiso 1 1 d R . . OW5 O 0.2888(4) 0.6142(3) 0.6711(2) 0.0899(14) Uani 1 1 d . . . H9 H 0.2155 0.6398 0.6618 0.108 Uiso 1 1 d R . . H10 H 0.3676 0.6792 0.7124 0.108 Uiso 1 1 d R . . N5 N 0.1070(4) 0.8492(3) 0.6309(2) 0.0857(16) Uani 1 1 d RD . . O8 O 0.2342(4) 0.8947(3) 0.6847(2) 0.118(2) Uiso 0.656(9) 1 d PRD . . O7 O 0.0552(4) 0.9190(3) 0.5930(2) 0.118(2) Uiso 0.656(9) 1 d PRD . . O6 O 0.0665(4) 0.7326(3) 0.5858(2) 0.118(2) Uiso 0.656(9) 1 d PRD . . O3 O 0.1187(4) 0.9559(3) 0.7052(2) 0.112(4) Uiso 0.344(9) 1 d PRD . . O5 O -0.0383(4) 0.7912(3) 0.5996(2) 0.112(4) Uiso 0.344(9) 1 d PRD . . O4 O 0.2037(4) 0.8180(3) 0.6214(2) 0.112(4) Uiso 0.344(9) 1 d PRD . . 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 0.0549(2) 0.02823(18) 0.0696(3) 0.02647(16) 0.03407(19) 0.02436(16) Ag2 0.0747(3) 0.0317(2) 0.0717(3) 0.02666(18) 0.0316(2) 0.02998(19) N4 0.053(2) 0.0287(18) 0.045(2) 0.0159(16) 0.0186(17) 0.0221(17) N3 0.057(2) 0.0273(18) 0.043(2) 0.0155(15) 0.0186(17) 0.0212(17) N2 0.0418(19) 0.0277(17) 0.054(2) 0.0211(16) 0.0239(17) 0.0191(15) N1 0.0372(18) 0.0249(17) 0.049(2) 0.0154(15) 0.0173(16) 0.0148(14) C16 0.045(2) 0.029(2) 0.041(2) 0.0142(18) 0.0158(19) 0.0117(18) C17 0.042(2) 0.029(2) 0.041(2) 0.0131(17) 0.0203(19) 0.0179(18) C18 0.041(2) 0.0250(19) 0.032(2) 0.0104(16) 0.0123(17) 0.0150(17) C19 0.048(2) 0.037(2) 0.057(3) 0.025(2) 0.030(2) 0.024(2) C20 0.054(3) 0.041(3) 0.061(3) 0.025(2) 0.030(2) 0.030(2) C15 0.070(3) 0.032(2) 0.058(3) 0.023(2) 0.040(3) 0.020(2) C14 0.066(3) 0.033(2) 0.062(3) 0.022(2) 0.041(3) 0.025(2) C13 0.043(2) 0.0250(19) 0.033(2) 0.0118(16) 0.0153(17) 0.0171(17) C12 0.044(2) 0.030(2) 0.064(3) 0.022(2) 0.026(2) 0.0176(19) C11 0.050(3) 0.033(2) 0.070(3) 0.020(2) 0.025(2) 0.026(2) C6 0.036(2) 0.028(2) 0.044(2) 0.0175(18) 0.0183(18) 0.0117(17) C7 0.031(2) 0.030(2) 0.044(2) 0.0161(17) 0.0166(17) 0.0150(17) C8 0.034(2) 0.0250(19) 0.036(2) 0.0140(16) 0.0155(16) 0.0140(16) C9 0.042(2) 0.036(2) 0.073(3) 0.032(2) 0.036(2) 0.0212(19) C10 0.045(2) 0.040(2) 0.084(3) 0.035(2) 0.040(2) 0.027(2) C5 0.038(2) 0.029(2) 0.067(3) 0.023(2) 0.027(2) 0.0149(18) C4 0.037(2) 0.032(2) 0.063(3) 0.022(2) 0.027(2) 0.0195(18) C3 0.032(2) 0.0219(18) 0.033(2) 0.0105(15) 0.0116(16) 0.0109(15) C2 0.033(2) 0.028(2) 0.042(2) 0.0159(17) 0.0187(17) 0.0136(16) C1 0.036(2) 0.032(2) 0.044(2) 0.0173(18) 0.0170(18) 0.0186(18) C21 0.055(3) 0.035(2) 0.058(3) 0.026(2) 0.036(2) 0.029(2) C22 0.052(3) 0.041(2) 0.062(3) 0.030(2) 0.034(2) 0.032(2) C23 0.036(2) 0.028(2) 0.051(2) 0.0161(18) 0.0249(19) 0.0160(17) C24 0.060(3) 0.055(3) 0.055(3) 0.034(2) 0.037(2) 0.040(2) O1 0.050(2) 0.050(2) 0.094(3) 0.0290(19) 0.050(2) 0.0227(17) O2 0.069(2) 0.067(2) 0.063(2) 0.0113(19) 0.0325(19) 0.042(2) OW1 0.118(4) 0.061(3) 0.105(3) 0.044(2) 0.064(3) 0.044(3) OW2 0.072(3) 0.068(3) 0.088(3) 0.038(2) 0.045(2) 0.028(2) OW3 0.071(3) 0.075(3) 0.108(3) 0.035(3) 0.052(3) 0.025(2) OW4 0.125(4) 0.088(4) 0.092(4) 0.039(3) 0.006(3) 0.011(3) OW5 0.100(3) 0.066(3) 0.097(3) 0.022(2) 0.034(3) 0.032(3) N5 0.086(4) 0.091(4) 0.082(4) 0.049(3) 0.018(3) 0.036(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.160(3) . ? Ag1 N2 2.167(3) 1_545 ? Ag1 O1 2.528(3) . ? Ag1 Ag2 3.366(3) . ? Ag2 N4 2.175(3) 1_545 ? Ag2 N3 2.183(3) . ? Ag2 O2 2.578(4) . ? N4 C16 1.339(6) . ? N4 C20 1.347(6) . ? N4 Ag2 2.175(3) 1_565 ? N3 C11 1.331(6) . ? N3 C15 1.333(6) . ? N2 C6 1.338(5) . ? N2 C10 1.341(5) . ? N2 Ag1 2.167(3) 1_565 ? N1 C5 1.342(5) . ? N1 C1 1.343(5) . ? C16 C17 1.378(6) . ? C16 H16A 0.9300 . ? C17 C18 1.397(6) . ? C17 H17A 0.9300 . ? C18 C19 1.396(6) . ? C18 C13 1.484(5) . ? C19 C20 1.367(6) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C15 C14 1.377(6) . ? C15 H15A 0.9300 . ? C14 C13 1.387(6) . ? C14 H14A 0.9300 . ? C13 C12 1.383(6) . ? C12 C11 1.378(6) . ? C12 H12A 0.9300 . ? C11 H11A 0.9300 . ? C6 C7 1.374(5) . ? C6 H6A 0.9300 . ? C7 C8 1.394(5) . ? C7 H7A 0.9300 . ? C8 C9 1.392(5) . ? C8 C3 1.479(5) . ? C9 C10 1.365(6) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C5 C4 1.378(6) . ? C5 H5A 0.9300 . ? C4 C3 1.394(6) . ? C4 H4A 0.9300 . ? C3 C2 1.393(5) . ? C2 C1 1.368(5) . ? C2 H2A 0.9300 . ? C1 H1A 0.9300 . ? C21 O1 1.241(6) . ? C21 O2 1.270(6) . ? C21 C23 1.528(5) . ? C22 C23 1.513(6) . ? C22 C24 1.527(6) 2_655 ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.534(6) . ? C23 H23A 0.9800 . ? C24 C22 1.527(6) 2_655 ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? OW1 H1 0.8505 . ? OW1 H2 0.8509 . ? OW2 H3 0.8507 . ? OW2 H4 0.8503 . ? OW3 H5 0.8450 . ? OW3 H6 0.8492 . ? OW4 H7 0.8503 . ? OW4 H8 0.8507 . ? OW5 H9 0.8512 . ? OW5 H10 0.8507 . ? N5 O4 1.1579 . ? N5 O8 1.1714 . ? N5 O7 1.2068 . ? N5 O6 1.2137 . ? N5 O5 1.3282 . ? N5 O3 1.3393 . ? O8 O4 0.9786 . ? O8 O3 1.5678 . ? O7 O3 1.4206 . ? O7 O5 1.5702 . ? O6 O4 1.3326 . ? O6 O5 1.4249 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N2 173.03(13) . 1_545 ? N1 Ag1 O1 95.41(12) . . ? N2 Ag1 O1 89.70(12) 1_545 . ? N1 Ag1 Ag2 73.82(10) . . ? N2 Ag1 Ag2 103.19(11) 1_545 . ? O1 Ag1 Ag2 73.96(10) . . ? N4 Ag2 N3 161.89(13) 1_545 . ? N4 Ag2 O2 97.10(13) 1_545 . ? N3 Ag2 O2 96.19(14) . . ? N4 Ag2 Ag1 83.78(11) 1_545 . ? N3 Ag2 Ag1 110.88(11) . . ? O2 Ag2 Ag1 78.92(9) . . ? C16 N4 C20 116.6(4) . . ? C16 N4 Ag2 119.5(3) . 1_565 ? C20 N4 Ag2 123.9(3) . 1_565 ? C11 N3 C15 116.5(4) . . ? C11 N3 Ag2 119.3(3) . . ? C15 N3 Ag2 123.8(3) . . ? C6 N2 C10 116.9(3) . . ? C6 N2 Ag1 119.0(3) . 1_565 ? C10 N2 Ag1 124.2(3) . 1_565 ? C5 N1 C1 117.0(3) . . ? C5 N1 Ag1 123.4(3) . . ? C1 N1 Ag1 119.3(3) . . ? N4 C16 C17 123.6(4) . . ? N4 C16 H16A 118.2 . . ? C17 C16 H16A 118.2 . . ? C16 C17 C18 119.9(4) . . ? C16 C17 H17A 120.0 . . ? C18 C17 H17A 120.0 . . ? C19 C18 C17 116.1(4) . . ? C19 C18 C13 122.3(4) . . ? C17 C18 C13 121.6(4) . . ? C20 C19 C18 120.4(4) . . ? C20 C19 H19A 119.8 . . ? C18 C19 H19A 119.8 . . ? N4 C20 C19 123.4(4) . . ? N4 C20 H20A 118.3 . . ? C19 C20 H20A 118.3 . . ? N3 C15 C14 123.6(4) . . ? N3 C15 H15A 118.2 . . ? C14 C15 H15A 118.2 . . ? C15 C14 C13 120.0(4) . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C12 C13 C14 116.1(4) . . ? C12 C13 C18 121.9(4) . . ? C14 C13 C18 121.9(4) . . ? C11 C12 C13 120.2(4) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? N3 C11 C12 123.5(4) . . ? N3 C11 H11A 118.3 . . ? C12 C11 H11A 118.3 . . ? N2 C6 C7 123.4(4) . . ? N2 C6 H6A 118.3 . . ? C7 C6 H6A 118.3 . . ? C6 C7 C8 119.8(4) . . ? C6 C7 H7A 120.1 . . ? C8 C7 H7A 120.1 . . ? C9 C8 C7 116.4(3) . . ? C9 C8 C3 122.3(4) . . ? C7 C8 C3 121.4(3) . . ? C10 C9 C8 120.3(4) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? N2 C10 C9 123.3(4) . . ? N2 C10 H10A 118.3 . . ? C9 C10 H10A 118.3 . . ? N1 C5 C4 123.3(4) . . ? N1 C5 H5A 118.3 . . ? C4 C5 H5A 118.3 . . ? C5 C4 C3 119.7(4) . . ? C5 C4 H4A 120.2 . . ? C3 C4 H4A 120.2 . . ? C2 C3 C4 116.4(3) . . ? C2 C3 C8 122.0(3) . . ? C4 C3 C8 121.6(3) . . ? C1 C2 C3 120.6(4) . . ? C1 C2 H2A 119.7 . . ? C3 C2 H2A 119.7 . . ? N1 C1 C2 122.9(4) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? O1 C21 O2 124.3(4) . . ? O1 C21 C23 118.5(4) . . ? O2 C21 C23 117.2(4) . . ? C23 C22 C24 111.8(4) . 2_655 ? C23 C22 H22A 109.3 . . ? C24 C22 H22A 109.3 2_655 . ? C23 C22 H22B 109.3 . . ? C24 C22 H22B 109.3 2_655 . ? H22A C22 H22B 107.9 . . ? C22 C23 C21 111.6(3) . . ? C22 C23 C24 109.4(3) . . ? C21 C23 C24 110.5(3) . . ? C22 C23 H23A 108.4 . . ? C21 C23 H23A 108.4 . . ? C24 C23 H23A 108.4 . . ? C22 C24 C23 111.1(4) 2_655 . ? C22 C24 H24A 109.4 2_655 . ? C23 C24 H24A 109.4 . . ? C22 C24 H24B 109.4 2_655 . ? C23 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? C21 O1 Ag1 134.5(3) . . ? C21 O2 Ag2 121.0(3) . . ? H1 OW1 H2 110.0 . . ? H3 OW2 H4 108.5 . . ? H5 OW3 H6 108.8 . . ? H7 OW4 H8 108.4 . . ? H9 OW5 H10 108.4 . . ? O4 N5 O8 49.7 . . ? O4 N5 O7 127.5 . . ? O8 N5 O7 115.7 . . ? O4 N5 O6 68.3 . . ? O8 N5 O6 111.8 . . ? O7 N5 O6 123.8 . . ? O4 N5 O5 136.2 . . ? O8 N5 O5 160.6 . . ? O7 N5 O5 76.4 . . ? O6 N5 O5 68.0 . . ? O4 N5 O3 126.5 . . ? O8 N5 O3 77.0 . . ? O7 N5 O3 67.6 . . ? O6 N5 O3 153.7 . . ? O5 N5 O3 95.4 . . ? O4 O8 N5 64.4 . . ? O4 O8 O3 120.6 . . ? N5 O8 O3 56.3 . . ? N5 O7 O3 60.6 . . ? N5 O7 O5 55.3 . . ? O3 O7 O5 82.4 . . ? N5 O6 O4 53.9 . . ? N5 O6 O5 59.8 . . ? O4 O6 O5 113.6 . . ? N5 O3 O7 51.8 . . ? N5 O3 O8 46.7 . . ? O7 O3 O8 84.6 . . ? N5 O5 O6 52.2 . . ? N5 O5 O7 48.3 . . ? O6 O5 O7 90.8 . . ? O8 O4 N5 65.9 . . ? O8 O4 O6 116.6 . . ? N5 O4 O6 57.8 . . ? 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 OW1 H1 O2 0.85 2.39 3.134(6) 147.0 2_666 OW1 H2 OW2 0.85 1.98 2.820(6) 167.3 . OW2 H3 OW3 0.85 1.99 2.827(7) 169.6 . OW2 H4 OW1 0.85 2.05 2.880(6) 165.3 2_667 OW3 H5 O3 0.85 2.06 2.866(5) 159.0 1_545 OW3 H5 O7 0.85 2.37 3.164(6) 157.0 1_545 OW3 H5 O8 0.85 2.41 3.171(6) 150.2 1_545 OW3 H6 OW4 0.85 1.97 2.810(7) 169.8 . OW4 H7 O5 0.85 2.11 2.826(6) 141.2 2_566 OW4 H7 O6 0.85 2.12 2.963(6) 173.2 2_566 OW4 H8 OW5 0.85 1.98 2.806(6) 163.6 . OW5 H9 O6 0.85 2.23 3.010 153.2 . OW5 H9 O4 0.85 2.27 2.849 125.4 . OW5 H10 O2 0.85 1.93 2.724(5) 154.9 2_666 _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.100 _refine_diff_density_min -0.946 _refine_diff_density_rms 0.083 data_a2 _database_code_depnum_ccdc_archive 'CCDC 892433' #TrackingRef '2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H26 Ag2 N4 O4, 14(H2 O)' _chemical_formula_sum 'C28 H54 Ag2 N4 O18' _chemical_formula_weight 950.49 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 Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_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 6.8206(14) _cell_length_b 22.830(5) _cell_length_c 25.065(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.38(3) _cell_angle_gamma 90.00 _cell_volume 3885.8(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13745 _cell_measurement_theta_min 3.0302 _cell_measurement_theta_max 27.4932 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 1.085 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8122 _exptl_absorpt_correction_T_max 0.8808 _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 ; Rigaku Mercury CCD Saturn724 ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number None _diffrn_standards_interval_count None _diffrn_standards_interval_time None _diffrn_standards_decay_% None _diffrn_reflns_number 9015 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8802 _reflns_number_gt 8561 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _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^)+(0.0190P)^2^+14.8139P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8802 _refine_ls_number_parameters 466 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.0940 _refine_ls_wR_factor_gt 0.0931 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.002 _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 -0.01455(4) 0.467886(10) 0.232180(10) 0.02219(7) Uani 1 1 d . . . Ag2 Ag 0.48206(4) 0.521010(10) 0.260087(10) 0.02182(7) Uani 1 1 d . . . N1 N -0.0018(4) 0.37322(12) 0.24435(11) 0.0181(5) Uani 1 1 d . . . N2 N 0.0169(4) 0.06312(12) 0.26102(11) 0.0191(6) Uani 1 1 d . . . N3 N 0.5057(4) 0.42639(12) 0.25529(12) 0.0197(6) Uani 1 1 d . . . N4 N 0.5209(4) 0.11573(11) 0.24916(11) 0.0171(5) Uani 1 1 d . . . C1 C 0.0453(5) 0.34634(14) 0.29192(13) 0.0195(6) Uani 1 1 d . . . H1A H 0.0721 0.3694 0.3223 0.023 Uiso 1 1 calc R . . C2 C 0.0552(5) 0.28624(14) 0.29728(13) 0.0187(6) Uani 1 1 d . . . H2A H 0.0892 0.2695 0.3307 0.022 Uiso 1 1 calc R . . C3 C 0.0139(5) 0.25060(13) 0.25204(13) 0.0158(6) Uani 1 1 d . . . C4 C -0.0334(5) 0.27869(14) 0.20296(13) 0.0175(6) Uani 1 1 d . . . H4A H -0.0606 0.2568 0.1718 0.021 Uiso 1 1 calc R . . C5 C -0.0396(5) 0.33921(14) 0.20100(14) 0.0201(7) Uani 1 1 d . . . H5A H -0.0714 0.3572 0.1680 0.024 Uiso 1 1 calc R . . C6 C -0.0093(5) 0.09611(14) 0.30442(13) 0.0199(7) Uani 1 1 d . . . H6A H -0.0273 0.0773 0.3365 0.024 Uiso 1 1 calc R . . C7 C -0.0105(5) 0.15653(14) 0.30336(13) 0.0196(6) Uani 1 1 d . . . H7A H -0.0292 0.1777 0.3342 0.024 Uiso 1 1 calc R . . C8 C 0.0167(5) 0.18584(14) 0.25536(13) 0.0163(6) Uani 1 1 d . . . C9 C 0.0451(5) 0.15128(14) 0.21107(13) 0.0192(6) Uani 1 1 d . . . H9A H 0.0652 0.1688 0.1785 0.023 Uiso 1 1 calc R . . C10 C 0.0434(5) 0.09112(14) 0.21541(13) 0.0199(7) Uani 1 1 d . . . H10A H 0.0616 0.0689 0.1852 0.024 Uiso 1 1 calc R . . C11 C 0.5651(5) 0.39530(14) 0.29938(14) 0.0208(7) Uani 1 1 d . . . H11A H 0.6052 0.4155 0.3307 0.025 Uiso 1 1 calc R . . C12 C 0.5693(5) 0.33482(14) 0.30040(13) 0.0199(7) Uani 1 1 d . . . H12A H 0.6100 0.3151 0.3320 0.024 Uiso 1 1 calc R . . C13 C 0.5118(5) 0.30363(13) 0.25365(13) 0.0164(6) Uani 1 1 d . . . C14 C 0.4511(5) 0.33593(14) 0.20785(13) 0.0189(6) Uani 1 1 d . . . H14A H 0.4114 0.3168 0.1759 0.023 Uiso 1 1 calc R . . C15 C 0.4501(5) 0.39641(14) 0.20996(13) 0.0197(6) Uani 1 1 d . . . H15A H 0.4096 0.4172 0.1790 0.024 Uiso 1 1 calc R . . C16 C 0.5008(5) 0.14446(14) 0.29504(13) 0.0193(6) Uani 1 1 d . . . H16A H 0.4887 0.1228 0.3260 0.023 Uiso 1 1 calc R . . C17 C 0.4974(5) 0.20496(14) 0.29828(13) 0.0189(6) Uani 1 1 d . . . H17A H 0.4842 0.2231 0.3310 0.023 Uiso 1 1 calc R . . C18 C 0.5139(5) 0.23865(13) 0.25245(13) 0.0154(6) Uani 1 1 d . . . C19 C 0.5331(5) 0.20844(14) 0.20449(13) 0.0192(6) Uani 1 1 d . . . H19A H 0.5435 0.2289 0.1728 0.023 Uiso 1 1 calc R . . C20 C 0.5365(5) 0.14804(14) 0.20482(13) 0.0203(7) Uani 1 1 d . . . H20A H 0.5503 0.1286 0.1728 0.024 Uiso 1 1 calc R . . C21 C -0.0589(5) 0.46775(13) 0.11005(13) 0.0182(6) Uani 1 1 d . . . C22 C 0.0787(6) 0.44402(15) 0.02179(13) 0.0243(7) Uani 1 1 d . . . H22A H 0.2096 0.4553 0.0368 0.029 Uiso 1 1 calc R . . H22B H 0.0626 0.4024 0.0280 0.029 Uiso 1 1 calc R . . C23 C -0.0758(5) 0.47843(15) 0.04962(13) 0.0205(7) Uani 1 1 d . . . H23A H -0.2066 0.4655 0.0347 0.025 Uiso 1 1 calc R . . C24 C -0.0569(6) 0.54382(15) 0.03838(13) 0.0232(7) Uani 1 1 d . . . H24A H -0.1576 0.5651 0.0553 0.028 Uiso 1 1 calc R . . H24B H 0.0706 0.5576 0.0537 0.028 Uiso 1 1 calc R . . C25 C 0.4992(5) 0.51550(14) 0.38365(13) 0.0192(6) Uani 1 1 d . . . C26 C 0.3863(5) 0.54728(15) 0.47151(13) 0.0213(7) Uani 1 1 d . . . H26A H 0.4793 0.5795 0.4738 0.026 Uiso 1 1 calc R . . H26B H 0.2652 0.5608 0.4520 0.026 Uiso 1 1 calc R . . C27 C 0.4710(5) 0.49597(14) 0.44087(13) 0.0193(6) Uani 1 1 d . . . H27A H 0.3719 0.4648 0.4383 0.023 Uiso 1 1 calc R . . C28 C 0.6550(5) 0.47147(16) 0.47197(13) 0.0232(7) Uani 1 1 d . . . H28A H 0.7576 0.5010 0.4744 0.028 Uiso 1 1 calc R . . H28B H 0.7018 0.4380 0.4530 0.028 Uiso 1 1 calc R . . O1 O 0.1052(4) 0.47334(11) 0.13667(9) 0.0225(5) Uani 1 1 d . . . O2 O -0.2159(4) 0.45496(11) 0.13143(10) 0.0236(5) Uani 1 1 d . . . O3 O 0.3473(4) 0.51797(11) 0.35117(9) 0.0250(5) Uani 1 1 d . . . O4 O 0.6691(4) 0.52864(11) 0.37146(10) 0.0233(5) Uani 1 1 d . . . OW1 O 0.5458(4) 0.02900(11) 0.38099(11) 0.0281(6) Uani 1 1 d . . . H1 H 0.6479 0.0101 0.3743 0.034 Uiso 1 1 d R . . H2 H 0.4459 0.0071 0.3740 0.034 Uiso 1 1 d R . . OW2 O 0.0150(4) 0.46084(11) 0.37493(11) 0.0269(5) Uani 1 1 d . . . H3 H -0.0779 0.4855 0.3758 0.032 Uiso 1 1 d R . . H4 H 0.1151 0.4784 0.3649 0.032 Uiso 1 1 d R . . OW3 O 0.0734(4) 0.38328(12) 0.45645(11) 0.0295(6) Uani 1 1 d . . . H5 H 0.0503 0.4086 0.4318 0.035 Uiso 1 1 d R . . H6 H -0.0256 0.3606 0.4562 0.035 Uiso 1 1 d R . . OW4 O 0.3926(4) 0.31050(12) 0.45158(12) 0.0360(7) Uani 1 1 d . . . H7 H 0.3756 0.2764 0.4384 0.043 Uiso 1 1 d R . . H8 H 0.2980 0.3321 0.4389 0.043 Uiso 1 1 d R . . OW5 O 0.2648(4) 0.20280(12) 0.41645(11) 0.0306(6) Uani 1 1 d . . . H9 H 0.1545 0.1961 0.4285 0.037 Uiso 1 1 d R . . H10 H 0.3435 0.1753 0.4267 0.037 Uiso 1 1 d R . . OW6 O 0.5535(4) 0.12083(11) 0.44872(11) 0.0289(6) Uani 1 1 d . . . H11 H 0.5533 0.0875 0.4335 0.035 Uiso 1 1 d R . . H12 H 0.5497 0.1154 0.4821 0.035 Uiso 1 1 d R . . OW7 O 0.8811(4) 0.19358(12) 0.44460(13) 0.0359(6) Uani 1 1 d . . . H13 H 0.7913 0.1679 0.4389 0.043 Uiso 1 1 d R . . H14 H 0.9105 0.1962 0.4782 0.043 Uiso 1 1 d R . . OW8 O 0.7689(3) 0.30683(8) 0.42161(8) 0.0323(6) Uani 1 1 d . . . H15 H 0.8140 0.2759 0.4371 0.039 Uiso 1 1 d R . . H16 H 0.6614 0.3157 0.4342 0.039 Uiso 1 1 d R . . OW9 O 0.1114(3) 0.38774(8) 0.56894(8) 0.0281(6) Uani 1 1 d R . . H17 H 0.1788 0.4155 0.5839 0.034 Uiso 1 1 d R . . H18 H 0.1046 0.3928 0.5352 0.034 Uiso 1 1 d R . . OW10 O 0.4126(4) 0.30707(12) 0.56162(12) 0.0332(6) Uani 1 1 d . . . H19 H 0.3222 0.3308 0.5684 0.040 Uiso 1 1 d R . . H20 H 0.4138 0.3047 0.5278 0.040 Uiso 1 1 d R . . OW11 O 0.2891(4) 0.19746(12) 0.58700(11) 0.0302(6) Uani 1 1 d . . . H21 H 0.1653 0.1960 0.5790 0.036 Uiso 1 1 d R . . H22 H 0.3305 0.2304 0.5770 0.036 Uiso 1 1 d R . . OW12 O 0.5825(4) 0.12463(12) 0.56162(11) 0.0303(6) Uani 1 1 d . . . H23 H 0.6133 0.0969 0.5834 0.036 Uiso 1 1 d R . . H24 H 0.4640 0.1344 0.5648 0.036 Uiso 1 1 d R . . OW13 O 0.8890(4) 0.20179(12) 0.55499(12) 0.0345(6) Uani 1 1 d . . . H25 H 0.8587 0.2369 0.5620 0.041 Uiso 1 1 d R . . H26 H 0.7901 0.1801 0.5589 0.041 Uiso 1 1 d R . . OW14 O 0.8107(4) 0.30992(11) 0.59248(11) 0.0294(6) Uani 1 1 d . . . H27 H 0.6897 0.3180 0.5849 0.035 Uiso 1 1 d R . . H28 H 0.8777 0.3408 0.5888 0.035 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 0.03351(16) 0.01070(11) 0.02299(13) 0.00116(9) 0.00604(10) -0.00001(10) Ag2 0.03194(15) 0.01084(11) 0.02301(13) 0.00070(9) 0.00434(10) 0.00046(10) N1 0.0230(14) 0.0125(12) 0.0195(13) 0.0008(10) 0.0060(11) -0.0003(11) N2 0.0222(14) 0.0106(12) 0.0242(14) -0.0001(10) 0.0005(11) 0.0004(10) N3 0.0220(14) 0.0137(13) 0.0238(14) -0.0015(10) 0.0043(11) 0.0003(11) N4 0.0199(14) 0.0128(12) 0.0189(13) -0.0011(10) 0.0029(10) 0.0004(10) C1 0.0257(17) 0.0150(15) 0.0179(15) -0.0004(12) 0.0023(13) 0.0004(13) C2 0.0226(17) 0.0159(15) 0.0173(15) 0.0018(12) 0.0015(12) 0.0008(12) C3 0.0167(15) 0.0118(14) 0.0190(15) -0.0002(11) 0.0027(12) 0.0005(11) C4 0.0219(16) 0.0151(15) 0.0158(14) 0.0002(11) 0.0032(12) -0.0002(12) C5 0.0235(17) 0.0165(15) 0.0205(16) 0.0014(12) 0.0030(13) 0.0003(13) C6 0.0273(18) 0.0143(15) 0.0185(15) 0.0010(12) 0.0047(13) -0.0007(13) C7 0.0247(17) 0.0165(15) 0.0174(15) -0.0012(12) 0.0007(13) 0.0003(13) C8 0.0157(15) 0.0143(14) 0.0185(15) 0.0021(11) 0.0001(12) -0.0010(12) C9 0.0247(17) 0.0154(15) 0.0180(15) -0.0002(12) 0.0039(13) 0.0012(13) C10 0.0238(17) 0.0175(15) 0.0185(15) -0.0023(12) 0.0030(13) 0.0005(13) C11 0.0278(18) 0.0135(15) 0.0209(16) -0.0041(12) 0.0022(13) -0.0013(13) C12 0.0247(17) 0.0159(15) 0.0188(15) -0.0003(12) 0.0005(13) 0.0010(13) C13 0.0183(15) 0.0126(14) 0.0184(15) -0.0003(11) 0.0014(12) 0.0003(12) C14 0.0241(17) 0.0148(15) 0.0182(15) 0.0013(12) 0.0034(13) 0.0007(12) C15 0.0214(17) 0.0177(15) 0.0200(15) 0.0010(12) 0.0027(13) 0.0016(13) C16 0.0228(17) 0.0163(15) 0.0187(15) 0.0006(12) 0.0017(13) -0.0003(13) C17 0.0240(17) 0.0154(15) 0.0171(15) -0.0002(12) 0.0011(12) 0.0017(12) C18 0.0159(15) 0.0122(14) 0.0185(14) 0.0005(11) 0.0036(11) -0.0004(11) C19 0.0237(17) 0.0174(15) 0.0168(15) -0.0014(12) 0.0033(12) -0.0009(13) C20 0.0263(18) 0.0160(15) 0.0188(15) -0.0014(12) 0.0033(13) 0.0004(13) C21 0.0252(17) 0.0128(14) 0.0172(14) 0.0022(11) 0.0044(13) 0.0035(12) C22 0.037(2) 0.0167(15) 0.0197(16) 0.0036(12) 0.0068(14) 0.0076(14) C23 0.0233(17) 0.0228(16) 0.0155(14) 0.0010(12) 0.0020(12) -0.0017(13) C24 0.0303(19) 0.0201(16) 0.0201(16) 0.0019(13) 0.0071(14) 0.0043(14) C25 0.0234(17) 0.0162(15) 0.0190(15) 0.0011(12) 0.0063(13) 0.0035(13) C26 0.0236(17) 0.0225(16) 0.0186(15) 0.0040(12) 0.0058(13) 0.0054(13) C27 0.0237(17) 0.0179(15) 0.0165(15) 0.0014(12) 0.0030(12) -0.0010(13) C28 0.0263(18) 0.0240(17) 0.0202(15) 0.0039(13) 0.0074(13) 0.0076(14) O1 0.0222(12) 0.0244(12) 0.0211(11) 0.0021(9) 0.0027(10) -0.0004(10) O2 0.0241(13) 0.0270(13) 0.0204(12) 0.0036(10) 0.0054(10) 0.0008(10) O3 0.0239(13) 0.0327(14) 0.0185(11) 0.0044(10) 0.0020(10) 0.0005(11) O4 0.0223(12) 0.0274(13) 0.0211(11) 0.0052(10) 0.0060(10) -0.0004(10) OW1 0.0227(13) 0.0212(12) 0.0401(15) -0.0051(11) 0.0025(11) -0.0004(10) OW2 0.0237(13) 0.0226(12) 0.0349(14) 0.0021(11) 0.0051(11) 0.0006(10) OW3 0.0270(14) 0.0264(13) 0.0347(15) 0.0067(11) 0.0013(11) -0.0024(11) OW4 0.0319(15) 0.0273(14) 0.0495(18) -0.0002(13) 0.0073(13) 0.0047(12) OW5 0.0306(14) 0.0318(14) 0.0297(14) 0.0002(11) 0.0041(11) 0.0002(11) OW6 0.0329(15) 0.0257(13) 0.0284(13) -0.0026(11) 0.0038(11) -0.0003(11) OW7 0.0320(15) 0.0292(14) 0.0467(17) -0.0022(13) 0.0056(13) -0.0044(12) OW8 0.0297(15) 0.0339(15) 0.0331(15) 0.0042(12) 0.0026(11) 0.0020(12) OW9 0.0298(14) 0.0257(13) 0.0290(13) -0.0021(10) 0.0036(11) -0.0049(11) OW10 0.0300(15) 0.0268(14) 0.0426(16) 0.0033(12) 0.0026(12) 0.0019(11) OW11 0.0275(14) 0.0335(15) 0.0293(14) 0.0039(11) 0.0005(11) 0.0004(11) OW12 0.0286(14) 0.0283(14) 0.0339(14) 0.0037(11) 0.0029(11) 0.0054(11) OW13 0.0283(15) 0.0262(14) 0.0483(18) -0.0042(12) 0.0008(13) -0.0010(11) OW14 0.0309(14) 0.0249(13) 0.0314(14) 0.0032(11) -0.0019(11) -0.0022(11) _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 N2 2.181(3) 2 ? Ag1 N1 2.183(3) . ? Ag2 N3 2.170(3) . ? Ag2 N4 2.175(3) 2_655 ? Ag2 O3 2.541(2) . ? N1 C5 1.341(4) . ? N1 C1 1.352(4) . ? N2 C10 1.337(4) . ? N2 C6 1.348(4) . ? N2 Ag1 2.181(3) 2_545 ? N3 C11 1.343(4) . ? N3 C15 1.350(4) . ? N4 C16 1.342(4) . ? N4 C20 1.346(4) . ? N4 Ag2 2.175(3) 2_645 ? C1 C2 1.380(4) . ? C1 H1A 0.9300 . ? C2 C3 1.403(4) . ? C2 H2A 0.9300 . ? C3 C4 1.398(4) . ? C3 C8 1.481(4) . ? C4 C5 1.383(4) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 C7 1.380(4) . ? C6 H6A 0.9300 . ? C7 C8 1.404(4) . ? C7 H7A 0.9300 . ? C8 C9 1.390(4) . ? C9 C10 1.378(4) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.381(4) . ? C11 H11A 0.9300 . ? C12 C13 1.396(4) . ? C12 H12A 0.9300 . ? C13 C14 1.394(4) . ? C13 C18 1.484(4) . ? C14 C15 1.382(4) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 C17 1.384(4) . ? C16 H16A 0.9300 . ? C17 C18 1.396(4) . ? C17 H17A 0.9300 . ? C18 C19 1.403(4) . ? C19 C20 1.379(4) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 O1 1.255(4) . ? C21 O2 1.275(4) . ? C21 C23 1.528(4) . ? C22 C24 1.527(4) 3_565 ? C22 C23 1.533(5) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.527(5) . ? C23 H23A 0.9800 . ? C24 C22 1.527(4) 3_565 ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 O3 1.257(4) . ? C25 O4 1.262(4) . ? C25 C27 1.531(4) . ? C26 C28 1.531(4) 3_666 ? C26 C27 1.542(4) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.521(5) . ? C27 H27A 0.9800 . ? C28 C26 1.531(4) 3_666 ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? OW1 H1 0.8501 . ? OW1 H2 0.8500 . ? OW2 H3 0.8500 . ? OW2 H4 0.8501 . ? OW3 H5 0.8499 . ? OW3 H6 0.8500 . ? OW4 H7 0.8501 . ? OW4 H8 0.8500 . ? OW5 H9 0.8500 . ? OW5 H10 0.8500 . ? OW6 H11 0.8501 . ? OW6 H12 0.8500 . ? OW7 H13 0.8500 . ? OW7 H14 0.8501 . ? OW8 H15 0.8500 . ? OW8 H16 0.8500 . ? OW9 H17 0.8502 . ? OW9 H18 0.8499 . ? OW10 H19 0.8499 . ? OW10 H20 0.8500 . ? OW11 H21 0.8500 . ? OW11 H22 0.8499 . ? OW12 H23 0.8501 . ? OW12 H24 0.8500 . ? OW13 H25 0.8501 . ? OW13 H26 0.8500 . ? OW14 H27 0.8499 . ? OW14 H28 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 N2 Ag1 N1 167.52(10) 2 . ? N3 Ag2 N4 169.66(11) . 2_655 ? N3 Ag2 O3 93.31(10) . . ? N4 Ag2 O3 97.03(9) 2_655 . ? C5 N1 C1 117.6(3) . . ? C5 N1 Ag1 117.3(2) . . ? C1 N1 Ag1 125.1(2) . . ? C10 N2 C6 117.5(3) . . ? C10 N2 Ag1 123.1(2) . 2_545 ? C6 N2 Ag1 119.4(2) . 2_545 ? C11 N3 C15 117.6(3) . . ? C11 N3 Ag2 119.9(2) . . ? C15 N3 Ag2 122.3(2) . . ? C16 N4 C20 117.5(3) . . ? C16 N4 Ag2 125.2(2) . 2_645 ? C20 N4 Ag2 117.2(2) . 2_645 ? N1 C1 C2 122.9(3) . . ? N1 C1 H1A 118.6 . . ? C2 C1 H1A 118.6 . . ? C1 C2 C3 119.6(3) . . ? C1 C2 H2A 120.2 . . ? C3 C2 H2A 120.2 . . ? C4 C3 C2 117.2(3) . . ? C4 C3 C8 120.5(3) . . ? C2 C3 C8 122.2(3) . . ? C5 C4 C3 119.6(3) . . ? C5 C4 H4A 120.2 . . ? C3 C4 H4A 120.2 . . ? N1 C5 C4 123.2(3) . . ? N1 C5 H5A 118.4 . . ? C4 C5 H5A 118.4 . . ? N2 C6 C7 123.0(3) . . ? N2 C6 H6A 118.5 . . ? C7 C6 H6A 118.5 . . ? C6 C7 C8 119.5(3) . . ? C6 C7 H7A 120.3 . . ? C8 C7 H7A 120.3 . . ? C9 C8 C7 117.0(3) . . ? C9 C8 C3 121.6(3) . . ? C7 C8 C3 121.5(3) . . ? C10 C9 C8 120.0(3) . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? N2 C10 C9 123.2(3) . . ? N2 C10 H10A 118.4 . . ? C9 C10 H10A 118.4 . . ? N3 C11 C12 123.2(3) . . ? N3 C11 H11A 118.4 . . ? C12 C11 H11A 118.4 . . ? C11 C12 C13 119.4(3) . . ? C11 C12 H12A 120.3 . . ? C13 C12 H12A 120.3 . . ? C14 C13 C12 117.4(3) . . ? C14 C13 C18 121.0(3) . . ? C12 C13 C18 121.7(3) . . ? C15 C14 C13 120.0(3) . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? N3 C15 C14 122.5(3) . . ? N3 C15 H15A 118.8 . . ? C14 C15 H15A 118.8 . . ? N4 C16 C17 122.8(3) . . ? N4 C16 H16A 118.6 . . ? C17 C16 H16A 118.6 . . ? C16 C17 C18 119.9(3) . . ? C16 C17 H17A 120.0 . . ? C18 C17 H17A 120.0 . . ? C17 C18 C19 117.1(3) . . ? C17 C18 C13 122.2(3) . . ? C19 C18 C13 120.7(3) . . ? C20 C19 C18 119.3(3) . . ? C20 C19 H19A 120.4 . . ? C18 C19 H19A 120.4 . . ? N4 C20 C19 123.4(3) . . ? N4 C20 H20A 118.3 . . ? C19 C20 H20A 118.3 . . ? O1 C21 O2 122.8(3) . . ? O1 C21 C23 119.4(3) . . ? O2 C21 C23 117.7(3) . . ? C24 C22 C23 110.4(3) 3_565 . ? C24 C22 H22A 109.6 3_565 . ? C23 C22 H22A 109.6 . . ? C24 C22 H22B 109.6 3_565 . ? C23 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? C24 C23 C21 109.8(3) . . ? C24 C23 C22 110.1(3) . . ? C21 C23 C22 112.2(3) . . ? C24 C23 H23A 108.2 . . ? C21 C23 H23A 108.2 . . ? C22 C23 H23A 108.2 . . ? C22 C24 C23 111.0(3) 3_565 . ? C22 C24 H24A 109.4 3_565 . ? C23 C24 H24A 109.4 . . ? C22 C24 H24B 109.4 3_565 . ? C23 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? O3 C25 O4 123.5(3) . . ? O3 C25 C27 116.8(3) . . ? O4 C25 C27 119.7(3) . . ? C28 C26 C27 111.0(3) 3_666 . ? C28 C26 H26A 109.4 3_666 . ? C27 C26 H26A 109.4 . . ? C28 C26 H26B 109.4 3_666 . ? C27 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C28 C27 C25 114.7(3) . . ? C28 C27 C26 110.7(3) . . ? C25 C27 C26 109.3(3) . . ? C28 C27 H27A 107.3 . . ? C25 C27 H27A 107.3 . . ? C26 C27 H27A 107.3 . . ? C27 C28 C26 111.3(3) . 3_666 ? C27 C28 H28A 109.4 . . ? C26 C28 H28A 109.4 3_666 . ? C27 C28 H28B 109.4 . . ? C26 C28 H28B 109.4 3_666 . ? H28A C28 H28B 108.0 . . ? C25 O3 Ag2 103.7(2) . . ? H1 OW1 H2 108.4 . . ? H3 OW2 H4 108.4 . . ? H5 OW3 H6 108.4 . . ? H7 OW4 H8 108.4 . . ? H9 OW5 H10 108.4 . . ? H11 OW6 H12 108.1 . . ? H13 OW7 H14 108.4 . . ? H15 OW8 H16 108.4 . . ? H17 OW9 H18 108.4 . . ? H19 OW10 H20 108.4 . . ? H21 OW11 H22 108.4 . . ? H23 OW12 H24 108.4 . . ? H25 OW13 H26 108.4 . . ? H27 OW14 H28 108.4 . . ? 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 OW1 H1 O1 0.85 1.92 2.770(4) 174.1 2_645 OW1 H2 O2 0.85 1.96 2.808(4) 172.0 2_545 OW2 H3 O4 0.85 1.98 2.816(4) 167.4 1_455 OW2 H4 O3 0.85 1.88 2.729(4) 173.4 . OW3 H5 OW2 0.85 1.86 2.705(4) 175.2 . OW3 H6 OW8 0.85 2.00 2.790(3) 154.3 1_455 OW4 H7 OW5 0.85 1.90 2.727(4) 163.4 . OW4 H8 OW3 0.85 2.01 2.751(4) 145.4 . OW5 H9 OW7 0.85 1.95 2.781(4) 167.5 1_455 OW5 H10 OW6 0.85 1.94 2.782(4) 171.6 . OW6 H11 OW1 0.85 1.87 2.695(4) 162.0 . OW6 H12 OW12 0.85 1.99 2.820(4) 163.3 . OW7 H13 OW6 0.85 1.98 2.794(4) 159.9 . OW7 H14 OW13 0.85 1.95 2.769(4) 162.1 . OW8 H15 OW7 0.85 1.94 2.742(3) 157.2 . OW8 H16 OW4 0.85 1.93 2.742(3) 160.3 . OW9 H17 O4 0.85 1.93 2.774(3) 170.7 3_666 OW9 H18 OW3 0.85 1.98 2.809(3) 165.6 . OW10 H19 OW9 0.85 1.94 2.778(3) 168.8 . OW10 H20 OW4 0.85 1.91 2.750(4) 170.9 . OW11 H21 OW13 0.85 1.93 2.773(4) 172.3 1_455 OW11 H22 OW10 0.85 1.89 2.734(4) 173.7 . OW12 H23 O2 0.85 1.99 2.793(4) 158.3 4_666 OW12 H24 OW11 0.85 1.98 2.723(4) 145.2 . OW13 H25 OW14 0.85 1.88 2.712(4) 167.7 . OW13 H26 OW12 0.85 1.91 2.751(4) 172.7 . OW14 H27 OW10 0.85 1.94 2.754(4) 159.6 . OW14 H28 OW9 0.85 2.02 2.817(3) 155.7 1_655 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.770 _refine_diff_density_min -0.837 _refine_diff_density_rms 0.098 data_a3 _database_code_depnum_ccdc_archive 'CCDC 892434' #TrackingRef '3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H26 Ag2 N4 O4, 2(H2 O), 3(C2 H6 O2)' _chemical_formula_sum 'C34 H48 Ag2 N4 O12' _chemical_formula_weight 920.50 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' 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 Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7488(17) _cell_length_b 9.867(2) _cell_length_c 11.657(2) _cell_angle_alpha 102.01(3) _cell_angle_beta 93.04(3) _cell_angle_gamma 104.10(3) _cell_volume 948.9(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3481 _cell_measurement_theta_min 3.1312 _cell_measurement_theta_max 27.5126 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.611 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 470 _exptl_absorpt_coefficient_mu 1.097 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.6239 _exptl_absorpt_correction_T_max 0.7305 _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 ; Rigaku Mercury CCD Saturn724 ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number None _diffrn_standards_interval_count None _diffrn_standards_interval_time None _diffrn_standards_decay_% None _diffrn_reflns_number 7965 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 27.51 _reflns_number_total 4191 _reflns_number_gt 3957 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _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^)+(0.0268P)^2^+1.4979P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4191 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.0903 _refine_ls_wR_factor_gt 0.0881 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 0.15721(3) -0.05089(3) 0.49933(2) 0.04733(10) Uani 1 1 d . . . N1 N 0.9826(3) 0.7393(3) 0.4824(2) 0.0371(6) Uani 1 1 d . . . N2 N 0.3628(3) 0.1232(3) 0.4838(2) 0.0378(6) Uani 1 1 d . . . C1 C 0.8785(4) 0.6739(3) 0.3871(3) 0.0454(8) Uani 1 1 d . . . H1A H 0.8869 0.7132 0.3210 0.054 Uiso 1 1 calc R . . C2 C 0.7596(4) 0.5516(3) 0.3817(3) 0.0444(8) Uani 1 1 d . . . H2A H 0.6905 0.5101 0.3131 0.053 Uiso 1 1 calc R . . C3 C 0.7426(3) 0.4898(3) 0.4787(3) 0.0321(6) Uani 1 1 d . . . C4 C 0.8506(4) 0.5584(3) 0.5776(3) 0.0364(6) Uani 1 1 d . . . H4A H 0.8438 0.5225 0.6454 0.044 Uiso 1 1 calc R . . C5 C 0.9678(4) 0.6795(3) 0.5754(3) 0.0380(7) Uani 1 1 d . . . H5A H 1.0403 0.7218 0.6421 0.046 Uiso 1 1 calc R . . C6 C 0.3741(4) 0.1834(4) 0.3911(3) 0.0455(8) Uani 1 1 d . . . H6A H 0.2960 0.1449 0.3274 0.055 Uiso 1 1 calc R . . C7 C 0.4953(4) 0.2994(4) 0.3847(3) 0.0452(8) Uani 1 1 d . . . H7A H 0.4980 0.3368 0.3178 0.054 Uiso 1 1 calc R . . C8 C 0.6138(3) 0.3607(3) 0.4785(3) 0.0325(6) Uani 1 1 d . . . C9 C 0.6031(4) 0.2955(4) 0.5728(3) 0.0560(10) Uani 1 1 d . . . H9A H 0.6806 0.3302 0.6371 0.067 Uiso 1 1 calc R . . C10 C 0.4783(4) 0.1795(4) 0.5719(3) 0.0575(11) Uani 1 1 d . . . H10A H 0.4744 0.1381 0.6368 0.069 Uiso 1 1 calc R . . C11 C 0.0970(4) 0.0060(3) 0.7646(2) 0.0381(7) Uani 1 1 d . . . C12 C 0.0972(4) 0.1313(3) 0.9744(2) 0.0407(7) Uani 1 1 d . . . H12A H 0.0174 0.1759 0.9503 0.049 Uiso 1 1 calc R . . H12B H 0.2006 0.1935 0.9708 0.049 Uiso 1 1 calc R . . C13 C 0.0777(4) -0.0135(3) 0.8900(2) 0.0351(6) Uani 1 1 d . . . H13A H 0.1621 -0.0546 0.9140 0.042 Uiso 1 1 calc R . . C14 C -0.0812(4) -0.1155(3) 0.8987(2) 0.0403(7) Uani 1 1 d . . . H14A H -0.0898 -0.2088 0.8477 0.048 Uiso 1 1 calc R . . H14B H -0.1668 -0.0790 0.8719 0.048 Uiso 1 1 calc R . . O1 O -0.0133(3) 0.0346(3) 0.70971(19) 0.0481(6) Uani 1 1 d . . . O2 O 0.2225(3) -0.0089(3) 0.7226(2) 0.0607(7) Uani 1 1 d . . . OW1 O 0.2245(3) 0.8112(3) 0.2104(3) 0.0654(7) Uani 1 1 d . . . H1 H 0.3090 0.8603 0.1910 0.079 Uiso 1 1 d R . . H2 H 0.1627 0.8652 0.2274 0.079 Uiso 1 1 d R . . C15 C 0.5165(7) 0.5315(7) 0.0636(5) 0.0940(17) Uani 1 1 d . . . H15A H 0.6281 0.5453 0.0878 0.113 Uiso 1 1 calc R . . H15B H 0.4943 0.6248 0.0801 0.113 Uiso 1 1 calc R . . O5 O 0.1369(4) 0.5281(3) 0.1335(3) 0.0709(8) Uani 1 1 d . . . H5 H 0.1789 0.6140 0.1427 0.085 Uiso 1 1 calc R . . C16 C -0.0113(5) 0.4913(5) 0.0608(4) 0.0647(11) Uani 1 1 d . . . H16A H -0.0768 0.5520 0.0955 0.078 Uiso 1 1 calc R . . H16B H -0.0666 0.3925 0.0581 0.078 Uiso 1 1 calc R . . O6 O 0.4239(4) 0.4430(4) 0.1304(3) 0.0822(10) Uani 1 1 d . . . H6 H 0.3368 0.4599 0.1340 0.099 Uiso 1 1 calc R . . O7A O 0.4989(4) -0.0305(4) 0.1519(3) 0.0623(9) Uani 0.80 1 d P . . H7 H 0.5872 -0.0141 0.1874 0.093 Uiso 0.80 1 d PR . . O7B O 0.544(2) 0.2046(15) 0.0739(12) 0.070(4) Uani 0.20 1 d P . . H7B H 0.4723 0.2420 0.0940 0.084 Uiso 0.20 1 d PR . . C17A C 0.515(2) 0.075(2) -0.0257(19) 0.104(5) Uiso 0.35 1 d P . . C17B C 0.5079(11) 0.0554(11) 0.0620(9) 0.092(2) Uiso 0.65 1 d P . . 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 0.04701(17) 0.03990(15) 0.04129(15) 0.01173(10) 0.00245(11) -0.01606(11) N1 0.0347(14) 0.0295(12) 0.0407(13) 0.0094(10) 0.0039(11) -0.0049(10) N2 0.0315(13) 0.0322(13) 0.0416(14) 0.0116(11) -0.0003(10) -0.0085(10) C1 0.051(2) 0.0390(17) 0.0379(16) 0.0166(13) -0.0012(14) -0.0083(15) C2 0.0462(19) 0.0391(17) 0.0387(16) 0.0149(13) -0.0043(14) -0.0093(14) C3 0.0289(14) 0.0280(13) 0.0367(14) 0.0097(11) 0.0043(11) 0.0002(11) C4 0.0364(16) 0.0326(15) 0.0352(15) 0.0099(12) 0.0033(12) -0.0020(13) C5 0.0367(16) 0.0333(15) 0.0367(15) 0.0068(12) -0.0005(12) -0.0025(13) C6 0.0436(19) 0.0432(18) 0.0371(16) 0.0069(13) -0.0032(13) -0.0089(15) C7 0.0472(19) 0.0457(18) 0.0323(15) 0.0133(13) 0.0000(13) -0.0103(15) C8 0.0296(14) 0.0288(14) 0.0358(14) 0.0092(11) 0.0033(11) 0.0002(12) C9 0.046(2) 0.057(2) 0.053(2) 0.0300(17) -0.0188(16) -0.0212(17) C10 0.054(2) 0.056(2) 0.053(2) 0.0330(18) -0.0169(17) -0.0181(18) C11 0.0420(17) 0.0375(16) 0.0266(13) 0.0061(12) 0.0042(12) -0.0039(13) C12 0.0515(19) 0.0338(15) 0.0290(14) 0.0096(12) 0.0041(13) -0.0054(14) C13 0.0400(16) 0.0374(15) 0.0272(13) 0.0102(11) 0.0030(11) 0.0067(13) C14 0.0507(19) 0.0352(16) 0.0261(14) 0.0057(12) 0.0021(12) -0.0041(14) O1 0.0571(15) 0.0556(14) 0.0325(11) 0.0202(10) 0.0014(10) 0.0084(12) O2 0.0494(15) 0.088(2) 0.0364(12) 0.0111(13) 0.0129(11) 0.0037(14) OW1 0.0543(16) 0.0539(16) 0.083(2) 0.0133(14) -0.0011(14) 0.0089(13) C15 0.076(3) 0.115(5) 0.083(3) 0.019(3) 0.007(3) 0.014(3) O5 0.078(2) 0.0591(17) 0.0729(19) 0.0112(15) -0.0165(16) 0.0222(16) C16 0.072(3) 0.053(2) 0.066(3) 0.010(2) 0.005(2) 0.015(2) O6 0.077(2) 0.096(3) 0.084(2) 0.039(2) 0.0170(19) 0.025(2) O7A 0.0337(16) 0.103(3) 0.0516(18) 0.0319(19) 0.0042(13) 0.0077(17) O7B 0.107(12) 0.056(8) 0.057(8) 0.023(7) 0.010(8) 0.029(8) _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 N2 2.208(3) . ? Ag1 N1 2.217(3) 1_445 ? Ag1 O2 2.559(3) . ? Ag1 Ag1 3.1495(9) 2_556 ? N1 C5 1.336(4) . ? N1 C1 1.338(4) . ? N1 Ag1 2.217(3) 1_665 ? N2 C10 1.328(4) . ? N2 C6 1.335(4) . ? C1 C2 1.376(4) . ? C1 H1A 0.9300 . ? C2 C3 1.390(4) . ? C2 H2A 0.9300 . ? C3 C4 1.388(4) . ? C3 C8 1.481(4) . ? C4 C5 1.378(4) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 C7 1.376(4) . ? C6 H6A 0.9300 . ? C7 C8 1.391(4) . ? C7 H7A 0.9300 . ? C8 C9 1.380(4) . ? C9 C10 1.374(5) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 O1 1.249(4) . ? C11 O2 1.254(4) . ? C11 C13 1.527(4) . ? C12 C13 1.522(4) . ? C12 C14 1.529(4) 2_557 ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.527(4) . ? C13 H13A 0.9800 . ? C14 C12 1.529(4) 2_557 ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? OW1 H1 0.8499 . ? OW1 H2 0.8500 . ? C15 O6 1.425(6) . ? C15 C15 1.467(10) 2_665 ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? O5 C16 1.435(5) . ? O5 H5 0.8200 . ? C16 C16 1.480(8) 2_565 ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? O6 H6 0.8200 . ? O7A C17A 1.43(2) 2_655 ? O7A C17B 1.472(11) . ? O7A H7 0.8200 . ? O7B C17B 1.404(16) . ? O7B C17A 1.50(2) . ? O7B H7B 0.8200 . ? C17A C17B 1.081(19) . ? C17A C17B 1.230(19) 2_655 ? C17A O7A 1.43(2) 2_655 ? C17A C17A 1.68(4) 2_655 ? C17B C17A 1.230(19) 2_655 ? C17B C17B 1.597(19) 2_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 N2 Ag1 N1 164.79(10) . 1_445 ? N2 Ag1 O2 93.14(10) . . ? N1 Ag1 O2 94.51(10) 1_445 . ? N2 Ag1 Ag1 111.16(7) . 2_556 ? N1 Ag1 Ag1 80.72(7) 1_445 2_556 ? O2 Ag1 Ag1 98.15(7) . 2_556 ? C5 N1 C1 116.7(3) . . ? C5 N1 Ag1 119.3(2) . 1_665 ? C1 N1 Ag1 123.6(2) . 1_665 ? C10 N2 C6 116.4(3) . . ? C10 N2 Ag1 120.4(2) . . ? C6 N2 Ag1 123.0(2) . . ? N1 C1 C2 123.4(3) . . ? N1 C1 H1A 118.3 . . ? C2 C1 H1A 118.3 . . ? C1 C2 C3 120.1(3) . . ? C1 C2 H2A 119.9 . . ? C3 C2 H2A 119.9 . . ? C4 C3 C2 116.3(3) . . ? C4 C3 C8 121.5(3) . . ? C2 C3 C8 122.1(3) . . ? C5 C4 C3 120.1(3) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? N1 C5 C4 123.4(3) . . ? N1 C5 H5A 118.3 . . ? C4 C5 H5A 118.3 . . ? N2 C6 C7 123.4(3) . . ? N2 C6 H6A 118.3 . . ? C7 C6 H6A 118.3 . . ? C6 C7 C8 120.0(3) . . ? C6 C7 H7A 120.0 . . ? C8 C7 H7A 120.0 . . ? C9 C8 C7 116.1(3) . . ? C9 C8 C3 121.7(3) . . ? C7 C8 C3 122.2(3) . . ? C10 C9 C8 120.2(3) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? N2 C10 C9 123.8(3) . . ? N2 C10 H10A 118.1 . . ? C9 C10 H10A 118.1 . . ? O1 C11 O2 124.0(3) . . ? O1 C11 C13 118.2(3) . . ? O2 C11 C13 117.7(3) . . ? C13 C12 C14 111.4(2) . 2_557 ? C13 C12 H12A 109.3 . . ? C14 C12 H12A 109.3 2_557 . ? C13 C12 H12B 109.3 . . ? C14 C12 H12B 109.3 2_557 . ? H12A C12 H12B 108.0 . . ? C12 C13 C11 110.2(2) . . ? C12 C13 C14 110.2(3) . . ? C11 C13 C14 112.4(2) . . ? C12 C13 H13A 108.0 . . ? C11 C13 H13A 108.0 . . ? C14 C13 H13A 108.0 . . ? C13 C14 C12 111.0(2) . 2_557 ? C13 C14 H14A 109.4 . . ? C12 C14 H14A 109.4 2_557 . ? C13 C14 H14B 109.4 . . ? C12 C14 H14B 109.4 2_557 . ? H14A C14 H14B 108.0 . . ? C11 O2 Ag1 104.7(2) . . ? H1 OW1 H2 108.4 . . ? O6 C15 C15 112.0(6) . 2_665 ? O6 C15 H15A 109.2 . . ? C15 C15 H15A 109.2 2_665 . ? O6 C15 H15B 109.2 . . ? C15 C15 H15B 109.2 2_665 . ? H15A C15 H15B 107.9 . . ? C16 O5 H5 109.5 . . ? O5 C16 C16 111.8(5) . 2_565 ? O5 C16 H16A 109.3 . . ? C16 C16 H16A 109.3 2_565 . ? O5 C16 H16B 109.3 . . ? C16 C16 H16B 109.3 2_565 . ? H16A C16 H16B 107.9 . . ? C15 O6 H6 109.5 . . ? C17A O7A C17B 50.1(7) 2_655 . ? C17A O7A H7 117.2 2_655 . ? C17B O7A H7 109.1 . . ? C17B O7B C17A 43.6(8) . . ? C17B O7B H7B 115.5 . . ? C17A O7B H7B 121.7 . . ? C17B C17A C17B 87.2(17) . 2_655 ? C17B C17A O7A 153(2) . 2_655 ? C17B C17A O7A 66.6(13) 2_655 2_655 ? C17B C17A O7B 63.6(14) . . ? C17B C17A O7B 151(2) 2_655 . ? O7A C17A O7B 142.8(16) 2_655 . ? C17B C17A C17A 47.1(12) . 2_655 ? C17B C17A C17A 40.1(10) 2_655 2_655 ? O7A C17A C17A 106.6(19) 2_655 2_655 ? O7B C17A C17A 111(2) . 2_655 ? C17A C17B C17A 92.8(17) . 2_655 ? C17A C17B O7B 72.8(15) . . ? C17A C17B O7B 165.3(17) 2_655 . ? C17A C17B O7A 155.9(16) . . ? C17A C17B O7A 63.4(12) 2_655 . ? O7B C17B O7A 130.7(9) . . ? C17A C17B C17B 50.3(12) . 2_655 ? C17A C17B C17B 42.5(10) 2_655 2_655 ? O7B C17B C17B 123.0(12) . 2_655 ? O7A C17B C17B 105.8(10) . 2_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 OW1 H1 O7A 0.85 1.88 2.732(4) 178.5 1_565 OW1 H2 O1 0.85 1.91 2.749(4) 168.3 2_566 O5 H5 OW1 0.82 1.88 2.653(4) 157.9 . O6 H6 O5 0.82 2.02 2.834(5) 171.3 . O7A H7 O2 0.82 1.86 2.675(4) 173.8 2_656 O7B H7B O6 0.82 2.09 2.774(15) 140.7 . _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 0.536 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.072 data_a4 _database_code_depnum_ccdc_archive 'CCDC 892435' #TrackingRef '4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H26 Ag2 N4 O4, (C8 H12 O4)' _chemical_formula_sum 'C36 H38 Ag2 N4 O8' _chemical_formula_weight 870.44 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 Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1893(16) _cell_length_b 10.168(2) _cell_length_c 11.644(2) _cell_angle_alpha 114.55(3) _cell_angle_beta 90.57(3) _cell_angle_gamma 103.62(3) _cell_volume 850.8(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3039 _cell_measurement_theta_min 3.0308 _cell_measurement_theta_max 27.4932 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.699 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 440 _exptl_absorpt_coefficient_mu 1.210 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8049 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Rigaku Mercury CCD Saturn724 ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number None _diffrn_standards_interval_count None _diffrn_standards_interval_time None _diffrn_standards_decay_% None _diffrn_reflns_number 3763 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3762 _reflns_number_gt 3505 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _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^)+(0.0351P)^2^+0.7550P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3762 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0899 _refine_ls_wR_factor_gt 0.0862 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 0.39801(3) 0.16051(3) 0.05932(3) 0.05210(11) Uani 1 1 d . . . N1 N 1.1860(3) 0.9788(3) 0.0530(2) 0.0359(5) Uani 1 1 d . . . N2 N 0.5798(3) 0.3574(3) 0.0592(2) 0.0371(5) Uani 1 1 d . . . C1 C 1.1495(4) 0.8435(3) -0.0451(3) 0.0397(6) Uani 1 1 d . . . H1A H 1.2072 0.8309 -0.1157 0.048 Uiso 1 1 calc R . . C2 C 1.0306(4) 0.7216(3) -0.0467(3) 0.0396(6) Uani 1 1 d . . . H2A H 1.0116 0.6288 -0.1164 0.048 Uiso 1 1 calc R . . C3 C 0.9393(3) 0.7375(3) 0.0558(3) 0.0313(5) Uani 1 1 d . . . C4 C 0.9734(4) 0.8798(3) 0.1563(3) 0.0405(6) Uani 1 1 d . . . H4A H 0.9136 0.8970 0.2263 0.049 Uiso 1 1 calc R . . C5 C 1.0968(4) 0.9949(3) 0.1510(3) 0.0434(7) Uani 1 1 d . . . H5A H 1.1191 1.0890 0.2195 0.052 Uiso 1 1 calc R . . C6 C 0.6188(4) 0.3642(3) -0.0497(3) 0.0378(6) Uani 1 1 d . . . H6A H 0.5666 0.2834 -0.1258 0.045 Uiso 1 1 calc R . . C7 C 0.7323(4) 0.4847(3) -0.0552(3) 0.0374(6) Uani 1 1 d . . . H7A H 0.7546 0.4846 -0.1334 0.045 Uiso 1 1 calc R . . C8 C 0.8132(3) 0.6067(3) 0.0572(3) 0.0314(5) Uani 1 1 d . . . C9 C 0.7723(4) 0.6001(3) 0.1707(3) 0.0386(6) Uani 1 1 d . . . H9A H 0.8231 0.6791 0.2482 0.046 Uiso 1 1 calc R . . C10 C 0.6556(4) 0.4753(3) 0.1677(3) 0.0405(7) Uani 1 1 d . . . H10A H 0.6287 0.4733 0.2444 0.049 Uiso 1 1 calc R . . C11 C 0.5720(4) 0.0777(3) 0.2871(3) 0.0372(6) Uani 1 1 d . . . C12 C 0.3625(4) -0.0053(4) 0.4149(3) 0.0418(7) Uani 1 1 d . . . H12A H 0.2866 0.0438 0.3939 0.050 Uiso 1 1 calc R . . H12B H 0.3374 -0.1078 0.3501 0.050 Uiso 1 1 calc R . . C13 C 0.5458(4) 0.0759(3) 0.4160(3) 0.0365(6) Uani 1 1 d . . . H13A H 0.5666 0.1800 0.4798 0.044 Uiso 1 1 calc R . . C14 C 0.6671(4) 0.0053(4) 0.4556(3) 0.0421(7) Uani 1 1 d . . . H14A H 0.7827 0.0606 0.4598 0.051 Uiso 1 1 calc R . . H14B H 0.6517 -0.0970 0.3922 0.051 Uiso 1 1 calc R . . C15 C 0.2858(4) 0.4005(3) 0.3791(3) 0.0395(6) Uani 1 1 d . . . C16 C 0.0834(4) 0.5636(4) 0.4172(3) 0.0451(7) Uani 1 1 d . . . H16A H 0.1696 0.6393 0.4055 0.054 Uiso 1 1 calc R . . H16B H 0.0188 0.4957 0.3350 0.054 Uiso 1 1 calc R . . C17 C 0.1682(4) 0.4767(3) 0.4677(3) 0.0374(6) Uani 1 1 d . . . H17A H 0.2356 0.5478 0.5493 0.045 Uiso 1 1 calc R . . C18 C 0.0338(4) 0.3611(3) 0.4918(3) 0.0447(7) Uani 1 1 d . . . H18A H -0.0321 0.2873 0.4118 0.054 Uiso 1 1 calc R . . H18B H 0.0887 0.3095 0.5276 0.054 Uiso 1 1 calc R . . O1 O 0.6187(4) -0.0238(3) 0.2040(2) 0.0552(6) Uani 1 1 d . . . O2 O 0.5419(3) 0.1882(3) 0.2719(2) 0.0458(5) Uani 1 1 d . . . O3 O 0.2961(3) 0.3961(3) 0.2744(2) 0.0622(7) Uani 1 1 d . . . O4 O 0.3690(3) 0.3360(3) 0.4257(2) 0.0546(6) Uani 1 1 d . . . H4 H 0.4233 0.2895 0.3719 0.082 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 0.04556(16) 0.04711(16) 0.06401(18) 0.03694(13) 0.00252(11) -0.01153(11) N1 0.0307(11) 0.0350(12) 0.0444(13) 0.0255(11) 0.0030(10) -0.0027(9) N2 0.0341(12) 0.0353(12) 0.0430(13) 0.0240(10) 0.0055(10) -0.0023(9) C1 0.0348(14) 0.0408(16) 0.0461(16) 0.0253(13) 0.0107(12) 0.0016(12) C2 0.0437(16) 0.0331(14) 0.0407(15) 0.0191(12) 0.0113(12) 0.0015(12) C3 0.0271(12) 0.0321(13) 0.0388(14) 0.0217(11) 0.0030(10) 0.0030(10) C4 0.0414(16) 0.0390(15) 0.0415(16) 0.0210(13) 0.0127(12) 0.0041(12) C5 0.0475(17) 0.0320(14) 0.0447(16) 0.0168(13) 0.0070(13) -0.0012(12) C6 0.0381(15) 0.0332(14) 0.0384(15) 0.0184(12) 0.0017(12) -0.0026(11) C7 0.0401(15) 0.0352(14) 0.0366(14) 0.0211(12) 0.0035(11) -0.0014(12) C8 0.0285(13) 0.0332(13) 0.0381(14) 0.0226(11) 0.0070(10) 0.0047(10) C9 0.0387(15) 0.0393(15) 0.0358(14) 0.0196(12) 0.0043(11) -0.0001(12) C10 0.0382(15) 0.0467(16) 0.0400(15) 0.0278(13) 0.0087(12) -0.0002(12) C11 0.0356(14) 0.0417(15) 0.0383(15) 0.0230(13) 0.0096(12) 0.0065(12) C12 0.0356(15) 0.0549(18) 0.0467(17) 0.0332(15) 0.0083(12) 0.0114(13) C13 0.0398(15) 0.0377(14) 0.0385(15) 0.0235(12) 0.0104(12) 0.0083(12) C14 0.0359(15) 0.0541(18) 0.0497(17) 0.0343(15) 0.0161(13) 0.0130(13) C15 0.0397(15) 0.0396(15) 0.0397(15) 0.0207(13) 0.0059(12) 0.0045(12) C16 0.0508(18) 0.0459(17) 0.0496(18) 0.0302(15) 0.0189(14) 0.0134(14) C17 0.0415(15) 0.0361(14) 0.0330(14) 0.0164(12) 0.0058(11) 0.0041(12) C18 0.0528(18) 0.0398(15) 0.0508(18) 0.0279(14) 0.0145(14) 0.0128(14) O1 0.0784(17) 0.0515(14) 0.0448(13) 0.0251(11) 0.0254(12) 0.0242(13) O2 0.0534(13) 0.0522(13) 0.0483(12) 0.0347(11) 0.0131(10) 0.0184(10) O3 0.0710(17) 0.0896(19) 0.0561(15) 0.0483(14) 0.0294(13) 0.0424(15) O4 0.0687(16) 0.0606(15) 0.0501(13) 0.0310(12) 0.0148(12) 0.0311(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.193(2) 1_445 ? Ag1 N2 2.196(2) . ? N1 C1 1.334(4) . ? N1 C5 1.335(4) . ? N1 Ag1 2.193(2) 1_665 ? N2 C6 1.337(4) . ? N2 C10 1.339(4) . ? C1 C2 1.377(4) . ? C1 H1A 0.9300 . ? C2 C3 1.387(4) . ? C2 H2A 0.9300 . ? C3 C4 1.392(4) . ? C3 C8 1.486(4) . ? C4 C5 1.378(4) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 C7 1.378(4) . ? C6 H6A 0.9300 . ? C7 C8 1.392(4) . ? C7 H7A 0.9300 . ? C8 C9 1.391(4) . ? C9 C10 1.384(4) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 O1 1.229(4) . ? C11 O2 1.284(4) . ? C11 C13 1.526(4) . ? C12 C14 1.529(4) 2_656 ? C12 C13 1.531(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.522(4) . ? C13 H13A 0.9800 . ? C14 C12 1.529(4) 2_656 ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 O3 1.206(4) . ? C15 O4 1.299(4) . ? C15 C17 1.517(4) . ? C16 C18 1.524(4) 2_566 ? C16 C17 1.524(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.530(4) . ? C17 H17A 0.9800 . ? C18 C16 1.524(4) 2_566 ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? O4 H4 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N2 171.00(9) 1_445 . ? C1 N1 C5 117.1(2) . . ? C1 N1 Ag1 121.17(19) . 1_665 ? C5 N1 Ag1 121.54(19) . 1_665 ? C6 N2 C10 117.3(2) . . ? C6 N2 Ag1 121.07(19) . . ? C10 N2 Ag1 121.61(18) . . ? N1 C1 C2 123.2(3) . . ? N1 C1 H1A 118.4 . . ? C2 C1 H1A 118.4 . . ? C1 C2 C3 119.9(3) . . ? C1 C2 H2A 120.1 . . ? C3 C2 H2A 120.1 . . ? C2 C3 C4 116.9(2) . . ? C2 C3 C8 120.8(3) . . ? C4 C3 C8 122.3(3) . . ? C5 C4 C3 119.3(3) . . ? C5 C4 H4A 120.3 . . ? C3 C4 H4A 120.3 . . ? N1 C5 C4 123.6(3) . . ? N1 C5 H5A 118.2 . . ? C4 C5 H5A 118.2 . . ? N2 C6 C7 123.4(3) . . ? N2 C6 H6A 118.3 . . ? C7 C6 H6A 118.3 . . ? C6 C7 C8 119.5(3) . . ? C6 C7 H7A 120.3 . . ? C8 C7 H7A 120.3 . . ? C9 C8 C7 117.2(2) . . ? C9 C8 C3 121.5(3) . . ? C7 C8 C3 121.3(2) . . ? C10 C9 C8 119.6(3) . . ? C10 C9 H9A 120.2 . . ? C8 C9 H9A 120.2 . . ? N2 C10 C9 123.0(3) . . ? N2 C10 H10A 118.5 . . ? C9 C10 H10A 118.5 . . ? O1 C11 O2 123.5(3) . . ? O1 C11 C13 119.9(3) . . ? O2 C11 C13 116.6(3) . . ? C14 C12 C13 111.0(2) 2_656 . ? C14 C12 H12A 109.4 2_656 . ? C13 C12 H12A 109.4 . . ? C14 C12 H12B 109.4 2_656 . ? C13 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? C14 C13 C11 112.8(2) . . ? C14 C13 C12 110.2(2) . . ? C11 C13 C12 110.2(2) . . ? C14 C13 H13A 107.8 . . ? C11 C13 H13A 107.8 . . ? C12 C13 H13A 107.8 . . ? C13 C14 C12 111.4(2) . 2_656 ? C13 C14 H14A 109.3 . . ? C12 C14 H14A 109.3 2_656 . ? C13 C14 H14B 109.3 . . ? C12 C14 H14B 109.3 2_656 . ? H14A C14 H14B 108.0 . . ? O3 C15 O4 123.7(3) . . ? O3 C15 C17 123.2(3) . . ? O4 C15 C17 113.1(3) . . ? C18 C16 C17 111.3(3) 2_566 . ? C18 C16 H16A 109.4 2_566 . ? C17 C16 H16A 109.4 . . ? C18 C16 H16B 109.4 2_566 . ? C17 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C15 C17 C16 112.5(2) . . ? C15 C17 C18 110.2(2) . . ? C16 C17 C18 110.0(3) . . ? C15 C17 H17A 108.0 . . ? C16 C17 H17A 108.0 . . ? C18 C17 H17A 108.0 . . ? C16 C18 C17 110.8(2) 2_566 . ? C16 C18 H18A 109.5 2_566 . ? C17 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 2_566 . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? C15 O4 H4 109.5 . . ? 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 O4 H4 O2 0.82 1.69 2.507(3) 174.2 . _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.382 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.065