# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 # Attachment '- CIFs.cif' #============================================================================= # 1. SUBMISSION DETAILS _publ_contact_author_name 'Jian-Fang Ma' _publ_contact_author_address ; Department of Chemistry Northeast Normal University Changchun 130024 P.R.China ; _publ_contact_author_email jianfangma@yahoo.com.cn _publ_contact_author_fax +86-431-85098620 _publ_contact_author_phone +86-431-85098620 _publ_author_name 'Jian-Fang Ma' #============================================================================= # Attachment 'bai.cif' data_compound-1 _database_code_depnum_ccdc_archive 'CCDC 800206' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8.5 H10 Ag1 N4, N O3, 0.5 (H2 O)' _chemical_formula_sum 'C8.50 H11 Ag N5 O3.50' _chemical_formula_weight 347.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_hall '-C 2yc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 7.759(5) _cell_length_b 23.455(5) _cell_length_c 13.184(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 97.128(5) _cell_angle_gamma 90.000(5) _cell_volume 2380.8(19) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2754 _cell_measurement_theta_min 4.4 _cell_measurement_theta_max 29.1 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.937 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 1.706 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.669 _exptl_absorpt_correction_T_max 0.783 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5440 _diffrn_reflns_av_R_equivalents 0.0208 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.42 _diffrn_reflns_theta_max 29.13 _reflns_number_total 2754 _reflns_number_gt 1925 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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. For O4, O4', o4'', O5, O5', N6 and O1W atoms, some anisotropic displacement ellipsoids were rather elongated which led us to use the ISOR restraints. ; _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^)+(0.0789P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2754 _refine_ls_number_parameters 210 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1217 _refine_ls_wR_factor_gt 0.1155 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.968 _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 0.32797(5) 0.839611(13) 0.11211(3) 0.05301(18) Uani 1 1 d . . . C1 C 0.2163(5) 0.72986(15) 0.2130(3) 0.0355(9) Uani 1 1 d . . . H1 H 0.1508 0.7510 0.2539 0.043 Uiso 1 1 calc R . . C2 C 0.3838(6) 0.70689(17) 0.1027(3) 0.0379(9) Uani 1 1 d . . . H2 H 0.4561 0.7095 0.0517 0.045 Uiso 1 1 calc R . . C3 C 0.3368(5) 0.65804(16) 0.1466(3) 0.0352(9) Uani 1 1 d . . . H3 H 0.3715 0.6212 0.1324 0.042 Uiso 1 1 calc R . . C4 C 0.1597(5) 0.63589(15) 0.2908(2) 0.0269(7) Uani 1 1 d . . . H4A H 0.1277 0.6595 0.3459 0.032 Uiso 1 1 calc R . . H4B H 0.2522 0.6107 0.3197 0.032 Uiso 1 1 calc R . . C5 C 0.0000 0.59861(18) 0.2500 0.0214(9) Uani 1 2 d S . . C6 C -0.0497(5) 0.56309(14) 0.3409(2) 0.0245(7) Uani 1 1 d . . . H6A H -0.0592 0.5889 0.3974 0.029 Uiso 1 1 calc R . . H6B H -0.1639 0.5469 0.3211 0.029 Uiso 1 1 calc R . . C7 C 0.0284(5) 0.46068(14) 0.3663(2) 0.0282(8) Uani 1 1 d . . . H7 H -0.0754 0.4468 0.3325 0.034 Uiso 1 1 calc R . . C8 C 0.2241(5) 0.51995(16) 0.4340(3) 0.0335(8) Uani 1 1 d . . . H8 H 0.2828 0.5531 0.4560 0.040 Uiso 1 1 calc R . . C9 C 0.2801(5) 0.46582(18) 0.4524(3) 0.0408(9) Uani 1 1 d . . . H9 H 0.3860 0.4555 0.4887 0.049 Uiso 1 1 calc R . . O1 O 0.8825(5) 0.96586(15) 0.1990(3) 0.0639(9) Uani 1 1 d . . . O2 O 1.0000 1.0443(2) 0.2500 0.0656(14) Uani 1 2 d S . . O1W O 0.0000 0.8504(4) 0.2500 0.126(3) Uani 1 2 d SU . . O3 O 0.6069(18) 0.7843(7) -0.0234(9) 0.138(6) Uani 0.50 1 d P . . O4' O 0.793(3) 0.8510(7) 0.0463(14) 0.043(4) Uani 0.18 1 d PU . . O4'' O 0.729(4) 0.8450(11) 0.086(2) 0.037(7) Uani 0.12 1 d PU . . O4 O 0.708(3) 0.8424(7) 0.0510(15) 0.037(4) Uani 0.20 1 d PU . . O5' O 0.869(3) 0.7747(9) 0.0804(15) 0.061(5) Uani 0.20 1 d PU . . O5 O 0.836(2) 0.7518(7) 0.0548(11) 0.060(4) Uani 0.30 1 d PU . . N1 N 0.3074(5) 0.75185(13) 0.1459(3) 0.0394(8) Uani 1 1 d . . . N2 N 0.2291(4) 0.67339(12) 0.2153(2) 0.0281(6) Uani 1 1 d . . . N3 N 0.0681(4) 0.51661(11) 0.3782(2) 0.0243(6) Uani 1 1 d . . . N4 N 0.1563(4) 0.42864(13) 0.4088(2) 0.0335(7) Uani 1 1 d . . . N5 N 1.0000 0.9923(2) 0.2500 0.0389(11) Uani 1 2 d S . . N6 N 0.7241(15) 0.7969(5) 0.0339(8) 0.070(2) Uani 0.50 1 d PU . . 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 0.0673(3) 0.0231(2) 0.0688(3) 0.00805(14) 0.00897(19) -0.01477(15) C1 0.039(2) 0.0194(16) 0.049(2) -0.0011(16) 0.0090(17) -0.0050(15) C2 0.039(2) 0.034(2) 0.042(2) 0.0040(17) 0.0111(17) -0.0102(17) C3 0.036(2) 0.0264(19) 0.045(2) -0.0038(16) 0.0127(17) -0.0043(16) C4 0.033(2) 0.0228(17) 0.0252(16) 0.0031(14) 0.0043(14) -0.0047(14) C5 0.023(2) 0.013(2) 0.028(2) 0.000 0.0056(18) 0.000 C6 0.0264(18) 0.0183(15) 0.0301(15) 0.0034(13) 0.0083(13) 0.0033(13) C7 0.036(2) 0.0199(15) 0.0291(17) 0.0016(14) 0.0034(14) 0.0003(14) C8 0.038(2) 0.0232(17) 0.040(2) 0.0060(16) 0.0063(16) -0.0029(16) C9 0.031(2) 0.038(2) 0.053(2) 0.0160(19) 0.0008(17) 0.0038(17) O1 0.043(2) 0.056(2) 0.089(2) -0.0079(18) -0.0108(18) -0.0039(17) O2 0.058(3) 0.033(2) 0.108(4) 0.000 0.016(3) 0.000 O1W 0.126(3) 0.124(3) 0.126(3) 0.000 0.0137(11) 0.000 O3 0.121(10) 0.185(14) 0.104(8) 0.082(9) -0.001(8) -0.064(10) O4' 0.043(4) 0.043(4) 0.043(4) 0.0001(10) 0.0049(11) 0.0000(10) O4'' 0.037(7) 0.037(7) 0.037(7) -0.0002(10) 0.0045(13) 0.0003(10) O4 0.037(4) 0.037(4) 0.037(4) -0.0002(10) 0.0045(11) 0.0003(10) O5' 0.061(5) 0.061(5) 0.061(5) 0.0003(10) 0.0076(12) 0.0002(10) O5 0.060(4) 0.060(4) 0.060(4) 0.0004(10) 0.0075(11) -0.0004(10) N1 0.045(2) 0.0223(16) 0.0509(18) 0.0081(14) 0.0078(15) -0.0098(14) N2 0.0280(17) 0.0213(14) 0.0353(15) -0.0022(12) 0.0050(12) -0.0059(12) N3 0.0323(17) 0.0149(12) 0.0274(14) 0.0017(11) 0.0112(11) -0.0005(11) N4 0.041(2) 0.0195(15) 0.0411(16) 0.0023(13) 0.0109(14) 0.0081(13) N5 0.031(3) 0.033(3) 0.052(3) 0.000 0.005(2) 0.000 N6 0.070(3) 0.071(3) 0.070(3) 0.0018(10) 0.0090(10) -0.0006(10) _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 N4 2.112(3) 4 ? Ag1 N1 2.117(3) . ? C1 N1 1.305(5) . ? C1 N2 1.328(4) . ? C1 H1 0.9300 . ? C2 C3 1.354(5) . ? C2 N1 1.368(6) . ? C2 H2 0.9300 . ? C3 N2 1.355(5) . ? C3 H3 0.9300 . ? C4 N2 1.479(4) . ? C4 C5 1.557(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.547(4) 2 ? C5 C6 1.547(4) . ? C5 C4 1.557(4) 2 ? C6 N3 1.468(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N4 1.314(5) . ? C7 N3 1.352(4) . ? C7 H7 0.9300 . ? C8 N3 1.338(5) . ? C8 C9 1.354(5) . ? C8 H8 0.9300 . ? C9 N4 1.370(5) . ? C9 H9 0.9300 . ? O1 N5 1.231(4) . ? O2 N5 1.220(6) . ? O3 O5 1.062(18) 7_665 ? O3 N6 1.147(14) . ? O3 O5' 1.60(3) 7_665 ? O3 O4 1.80(3) . ? O4' O4 0.70(2) . ? O4' O4'' 0.78(3) . ? O4' N6 1.38(2) . ? O4'' N6 1.32(3) . ? O4 N6 1.101(18) . ? O5' O5 0.67(2) . ? O5' N6 1.32(2) . ? O5' O3 1.60(3) 7_665 ? O5 O3 1.062(18) 7_665 ? O5 N6 1.376(18) . ? O5 N6 1.66(2) 7_665 ? N4 Ag1 2.112(3) 4_545 ? N5 O1 1.231(4) 2_755 ? N6 O5 1.66(2) 7_665 ? 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 N4 Ag1 N1 175.09(12) 4 . ? N1 C1 N2 111.4(3) . . ? N1 C1 H1 124.3 . . ? N2 C1 H1 124.3 . . ? C3 C2 N1 108.7(4) . . ? C3 C2 H2 125.6 . . ? N1 C2 H2 125.6 . . ? C2 C3 N2 106.4(3) . . ? C2 C3 H3 126.8 . . ? N2 C3 H3 126.8 . . ? N2 C4 C5 116.2(2) . . ? N2 C4 H4A 108.2 . . ? C5 C4 H4A 108.2 . . ? N2 C4 H4B 108.2 . . ? C5 C4 H4B 108.2 . . ? H4A C4 H4B 107.4 . . ? C6 C5 C6 114.8(4) 2 . ? C6 C5 C4 107.81(19) 2 . ? C6 C5 C4 107.40(18) . . ? C6 C5 C4 107.40(18) 2 2 ? C6 C5 C4 107.81(19) . 2 ? C4 C5 C4 111.7(4) . 2 ? N3 C6 C5 117.1(3) . . ? N3 C6 H6A 108.0 . . ? C5 C6 H6A 108.0 . . ? N3 C6 H6B 108.0 . . ? C5 C6 H6B 108.0 . . ? H6A C6 H6B 107.3 . . ? N4 C7 N3 110.9(3) . . ? N4 C7 H7 124.6 . . ? N3 C7 H7 124.6 . . ? N3 C8 C9 107.0(3) . . ? N3 C8 H8 126.5 . . ? C9 C8 H8 126.5 . . ? C8 C9 N4 109.2(4) . . ? C8 C9 H9 125.4 . . ? N4 C9 H9 125.4 . . ? O5 O3 N6 97.3(19) 7_665 . ? O5 O3 O5' 17.8(13) 7_665 7_665 ? N6 O3 O5' 113.9(17) . 7_665 ? O5 O3 O4 129.9(17) 7_665 . ? N6 O3 O4 35.9(10) . . ? O5' O3 O4 147.7(14) 7_665 . ? O4 O4' O4'' 37(2) . . ? O4 O4' N6 52(2) . . ? O4'' O4' N6 69(3) . . ? O4' O4'' N6 77(3) . . ? O4' O4 N6 97(3) . . ? O4' O4 O3 121(3) . . ? N6 O4 O3 37.7(11) . . ? O5 O5' N6 80(3) . . ? O5 O5' O3 29(2) . 7_665 ? N6 O5' O3 105.3(16) . 7_665 ? O5' O5 O3 133(3) . 7_665 ? O5' O5 N6 71(2) . . ? O3 O5 N6 144.9(17) 7_665 . ? O5' O5 N6 165(3) . 7_665 ? O3 O5 N6 43.3(11) 7_665 7_665 ? N6 O5 N6 105.8(11) . 7_665 ? C1 N1 C2 106.1(3) . . ? C1 N1 Ag1 126.1(3) . . ? C2 N1 Ag1 127.9(3) . . ? C1 N2 C3 107.5(3) . . ? C1 N2 C4 125.1(3) . . ? C3 N2 C4 126.7(3) . . ? C8 N3 C7 107.3(3) . . ? C8 N3 C6 128.6(3) . . ? C7 N3 C6 123.9(3) . . ? C7 N4 C9 105.5(3) . . ? C7 N4 Ag1 124.2(3) . 4_545 ? C9 N4 Ag1 129.5(3) . 4_545 ? O2 N5 O1 120.2(3) . 2_755 ? O2 N5 O1 120.2(3) . . ? O1 N5 O1 119.5(5) 2_755 . ? O4 N6 O3 106.4(18) . . ? O4 N6 O5' 113.6(18) . . ? O3 N6 O5' 140.0(16) . . ? O4 N6 O4'' 20.3(14) . . ? O3 N6 O4'' 122(2) . . ? O5' N6 O4'' 97.2(18) . . ? O4 N6 O5 142.3(17) . . ? O3 N6 O5 111.3(13) . . ? O5' N6 O5 28.7(10) . . ? O4'' N6 O5 125.1(18) . . ? O4 N6 O4' 30.4(11) . . ? O3 N6 O4' 125.4(15) . . ? O5' N6 O4' 90.7(15) . . ? O4'' N6 O4' 33.6(13) . . ? O5 N6 O4' 117.3(15) . . ? O4 N6 O5 141.4(15) . 7_665 ? O3 N6 O5 39.4(11) . 7_665 ? O5' N6 O5 101.9(13) . 7_665 ? O4'' N6 O5 160.7(18) . 7_665 ? O5 N6 O5 74.2(11) . 7_665 ? O4' N6 O5 142.0(11) . 7_665 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 1.1(5) . . . . ? N2 C4 C5 C6 55.5(4) . . . 2 ? N2 C4 C5 C6 179.8(3) . . . . ? N2 C4 C5 C4 -62.2(2) . . . 2 ? C6 C5 C6 N3 48.4(2) 2 . . . ? C4 C5 C6 N3 -71.4(4) . . . . ? C4 C5 C6 N3 168.1(3) 2 . . . ? N3 C8 C9 N4 -1.0(5) . . . . ? O4 O4' O4'' N6 55(4) . . . . ? O4'' O4' O4 N6 -106(5) . . . . ? O4'' O4' O4 O3 -137(5) . . . . ? N6 O4' O4 O3 -31.1(13) . . . . ? O5 O3 O4 O4' 27(4) 7_665 . . . ? N6 O3 O4 O4' 57(3) . . . . ? O5' O3 O4 O4' 30(4) 7_665 . . . ? O5 O3 O4 N6 -29(2) 7_665 . . . ? O5' O3 O4 N6 -27(2) 7_665 . . . ? N6 O5' O5 O3 150(3) . . . 7_665 ? O3 O5' O5 N6 -150(3) 7_665 . . . ? N6 O5' O5 N6 81(11) . . . 7_665 ? O3 O5' O5 N6 -69(10) 7_665 . . 7_665 ? N2 C1 N1 C2 -0.2(5) . . . . ? N2 C1 N1 Ag1 179.4(2) . . . . ? C3 C2 N1 C1 -0.6(5) . . . . ? C3 C2 N1 Ag1 179.9(3) . . . . ? N4 Ag1 N1 C1 26.1(18) 4 . . . ? N4 Ag1 N1 C2 -154.5(14) 4 . . . ? N1 C1 N2 C3 0.9(4) . . . . ? N1 C1 N2 C4 172.3(3) . . . . ? C2 C3 N2 C1 -1.2(4) . . . . ? C2 C3 N2 C4 -172.4(3) . . . . ? C5 C4 N2 C1 109.4(4) . . . . ? C5 C4 N2 C3 -80.9(5) . . . . ? C9 C8 N3 C7 2.1(4) . . . . ? C9 C8 N3 C6 178.1(3) . . . . ? N4 C7 N3 C8 -2.5(4) . . . . ? N4 C7 N3 C6 -178.8(3) . . . . ? C5 C6 N3 C8 74.6(4) . . . . ? C5 C6 N3 C7 -110.0(3) . . . . ? N3 C7 N4 C9 1.9(4) . . . . ? N3 C7 N4 Ag1 -168.9(2) . . . 4_545 ? C8 C9 N4 C7 -0.6(4) . . . . ? C8 C9 N4 Ag1 169.6(3) . . . 4_545 ? O4' O4 N6 O3 -134(2) . . . . ? O4' O4 N6 O5' 44(3) . . . . ? O3 O4 N6 O5' 178(2) . . . . ? O4' O4 N6 O4'' 82(5) . . . . ? O3 O4 N6 O4'' -144(5) . . . . ? O4' O4 N6 O5 44(4) . . . . ? O3 O4 N6 O5 178(3) . . . . ? O3 O4 N6 O4' 134(2) . . . . ? O4' O4 N6 O5 -111(3) . . . 7_665 ? O3 O4 N6 O5 22.7(16) . . . 7_665 ? O5 O3 N6 O4 157.7(16) 7_665 . . . ? O5' O3 N6 O4 164.6(14) 7_665 . . . ? O5 O3 N6 O5' -19(2) 7_665 . . . ? O5' O3 N6 O5' -12(3) 7_665 . . . ? O4 O3 N6 O5' -177(3) . . . . ? O5 O3 N6 O4'' 172(2) 7_665 . . . ? O5' O3 N6 O4'' 178.5(19) 7_665 . . . ? O4 O3 N6 O4'' 14(2) . . . . ? O5 O3 N6 O5 -20.8(19) 7_665 . . . ? O5' O3 N6 O5 -13.9(16) 7_665 . . . ? O4 O3 N6 O5 -178(2) . . . . ? O5 O3 N6 O4' 131.1(17) 7_665 . . . ? O5' O3 N6 O4' 138.0(15) 7_665 . . . ? O4 O3 N6 O4' -26.6(15) . . . . ? O5' O3 N6 O5 6.9(13) 7_665 . . 7_665 ? O4 O3 N6 O5 -157.7(16) . . . 7_665 ? O5 O5' N6 O4 -180(2) . . . . ? O3 O5' N6 O4 -165.1(15) 7_665 . . . ? O5 O5' N6 O3 -3(4) . . . . ? O3 O5' N6 O3 12(3) 7_665 . . . ? O5 O5' N6 O4'' 168(3) . . . . ? O3 O5' N6 O4'' -177.5(17) 7_665 . . . ? O3 O5' N6 O5 14.7(17) 7_665 . . . ? O5 O5' N6 O4' -159(2) . . . . ? O3 O5' N6 O4' -144.5(13) 7_665 . . . ? O5 O5' N6 O5 -15(3) . . . 7_665 ? O3 O5' N6 O5 -0.6(16) 7_665 . . 7_665 ? O4' O4'' N6 O4 -65(5) . . . . ? O4' O4'' N6 O3 -107(3) . . . . ? O4' O4'' N6 O5' 80(3) . . . . ? O4' O4'' N6 O5 87(3) . . . . ? O4' O4'' N6 O5 -91(5) . . . 7_665 ? O5' O5 N6 O4 0(4) . . . . ? O3 O5 N6 O4 -140(3) 7_665 . . . ? N6 O5 N6 O4 -164(2) 7_665 . . . ? O5' O5 N6 O3 178(2) . . . . ? O3 O5 N6 O3 38(4) 7_665 . . . ? N6 O5 N6 O3 13.5(13) 7_665 . . . ? O3 O5 N6 O5' -140(5) 7_665 . . . ? N6 O5 N6 O5' -164(3) 7_665 . . . ? O5' O5 N6 O4'' -15(3) . . . . ? O3 O5 N6 O4'' -155(3) 7_665 . . . ? N6 O5 N6 O4'' -179(2) 7_665 . . . ? O5' O5 N6 O4' 24(3) . . . . ? O3 O5 N6 O4' -117(3) 7_665 . . . ? N6 O5 N6 O4' -140.8(13) 7_665 . . . ? O5' O5 N6 O5 164(3) . . . 7_665 ? O3 O5 N6 O5 24(3) 7_665 . . 7_665 ? N6 O5 N6 O5 0.000(2) 7_665 . . 7_665 ? O4'' O4' N6 O4 38(3) . . . . ? O4 O4' N6 O3 58(3) . . . . ? O4'' O4' N6 O3 97(3) . . . . ? O4 O4' N6 O5' -140(3) . . . . ? O4'' O4' N6 O5' -102(3) . . . . ? O4 O4' N6 O4'' -38(3) . . . . ? O4 O4' N6 O5 -152(3) . . . . ? O4'' O4' N6 O5 -113(3) . . . . ? O4 O4' N6 O5 109(3) . . . 7_665 ? O4'' O4' N6 O5 147(3) . . . 7_665 ? _diffrn_measured_fraction_theta_max 0.857 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.951 _refine_diff_density_min -1.244 _refine_diff_density_rms 0.114 #===END data_compound-2 _database_code_depnum_ccdc_archive 'CCDC 800207' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4.25 H5 Ag Br N2 ' _chemical_formula_sum 'C4.25 H5 Ag Br N2' _chemical_formula_weight 271.88 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' Br Br -0.2901 2.4595 '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 tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_hall "-I 4ad'" loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-y+3/4, x+1/4, z+1/4' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+3/4, z+3/4' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' 'y-3/4, -x-1/4, -z-1/4' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 14.335(5) _cell_length_b 14.335(5) _cell_length_c 12.058(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2477.8(16) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1640 _cell_measurement_theta_min 4.4 _cell_measurement_theta_max 29.2 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.915 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 9.590 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.173 _exptl_absorpt_correction_T_max 0.486 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20585 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0194 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 4.42 _diffrn_reflns_theta_max 29.22 _reflns_number_total 1640 _reflns_number_gt 1279 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0306P)^2^+3.2905P] 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 1640 _refine_ls_number_parameters 84 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0628 _refine_ls_wR_factor_gt 0.0610 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 0.42483(4) 0.16831(4) 0.29070(5) 0.05823(16) Uani 0.90 1 d P . . Ag1' Ag 0.3796(4) 0.1678(3) 0.2802(5) 0.0549(12) Uani 0.10 1 d P . . C1 C 0.3530(2) -0.0512(2) 0.0480(2) 0.0318(6) Uani 1 1 d . . . H1 H 0.3162 -0.0777 -0.0072 0.038 Uiso 1 1 calc R . . C2 C 0.3354(2) 0.0277(2) 0.1060(3) 0.0347(6) Uani 1 1 d . . . H2 H 0.2826 0.0647 0.0975 0.042 Uiso 1 1 calc R . . C3 C 0.4658(2) -0.0246(2) 0.1634(3) 0.0359(7) Uani 1 1 d . . . H3 H 0.5217 -0.0304 0.2019 0.043 Uiso 1 1 calc R . . C4 C 0.48460(18) -0.16717(18) 0.0442(2) 0.0251(5) Uani 1 1 d . . . H4A H 0.5451 -0.1480 0.0161 0.030 Uiso 1 1 calc R . . H4B H 0.4488 -0.1898 -0.0185 0.030 Uiso 1 1 calc R . . C5 C 0.5000 -0.2500 0.1250 0.0214(10) Uani 1 4 d S . . N1 N 0.40560(18) 0.04495(16) 0.1783(2) 0.0349(6) Uani 1 1 d . . . N2 N 0.43721(15) -0.08379(14) 0.08822(18) 0.0242(5) Uani 1 1 d . . . Br1 Br 0.36431(2) 0.33775(2) 0.24304(3) 0.04319(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 0.0863(4) 0.0363(2) 0.0521(2) -0.01152(15) -0.0139(3) 0.0016(3) Ag1' 0.078(3) 0.0227(14) 0.064(2) -0.0119(13) -0.029(2) 0.008(2) C1 0.0296(14) 0.0317(14) 0.0342(15) 0.0044(12) -0.0088(12) 0.0026(12) C2 0.0335(15) 0.0318(15) 0.0388(16) 0.0069(13) -0.0011(13) 0.0064(12) C3 0.0318(15) 0.0330(15) 0.0430(17) 0.0052(13) -0.0108(13) 0.0022(13) C4 0.0266(13) 0.0273(13) 0.0214(12) 0.0024(10) 0.0016(10) 0.0032(10) C5 0.0228(15) 0.0228(15) 0.019(2) 0.000 0.000 0.000 N1 0.0443(14) 0.0251(12) 0.0353(13) 0.0003(10) -0.0029(11) 0.0015(10) N2 0.0239(11) 0.0207(10) 0.0279(11) 0.0075(9) 0.0015(9) 0.0055(9) Br1 0.0507(2) 0.04058(19) 0.03832(19) 0.00753(13) 0.00026(14) 0.00578(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 Ag1' 0.661(4) . ? Ag1 N1 2.245(2) . ? Ag1 Br1 2.6424(11) . ? Ag1 Br1 2.7261(12) 12_656 ? Ag1 Ag1 3.0327(12) 12_656 ? Ag1 Ag1 3.0327(12) 11_666 ? Ag1 Br1 3.0781(12) 2_655 ? Ag1 Ag1' 3.172(5) 12_656 ? Ag1 Ag1 3.1827(16) 2_655 ? Ag1' N1 2.179(5) . ? Ag1' Br1 2.487(4) . ? Ag1' Br1 2.878(5) 12_656 ? Ag1' Ag1 3.172(5) 11_666 ? C1 C2 1.353(4) . ? C1 N2 1.383(3) . ? C1 H1 0.9300 . ? C2 N1 1.354(4) . ? C2 H2 0.9300 . ? C3 N2 1.307(4) . ? C3 N1 1.330(4) . ? C3 H3 0.9300 . ? C4 N2 1.474(3) . ? C4 C5 1.552(3) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C4 1.552(3) 2_645 ? C5 C4 1.552(3) 15_655 ? C5 C4 1.552(3) 16_545 ? Br1 Ag1 2.7261(12) 11_666 ? Br1 Ag1' 2.878(5) 11_666 ? Br1 Ag1 3.0781(12) 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 Ag1' Ag1 N1 75.8(4) . . ? Ag1' Ag1 Br1 69.3(4) . . ? N1 Ag1 Br1 123.53(7) . . ? Ag1' Ag1 Br1 96.6(5) . 12_656 ? N1 Ag1 Br1 110.23(7) . 12_656 ? Br1 Ag1 Br1 116.57(2) . 12_656 ? Ag1' Ag1 Ag1 148.9(5) . 12_656 ? N1 Ag1 Ag1 121.33(7) . 12_656 ? Br1 Ag1 Ag1 111.156(19) . 12_656 ? Br1 Ag1 Ag1 54.31(3) 12_656 12_656 ? Ag1' Ag1 Ag1 96.1(5) . 11_666 ? N1 Ag1 Ag1 170.04(7) . 11_666 ? Br1 Ag1 Ag1 56.92(3) . 11_666 ? Br1 Ag1 Ag1 64.36(3) 12_656 11_666 ? Ag1 Ag1 Ag1 63.30(3) 12_656 11_666 ? Ag1' Ag1 Br1 158.1(5) . 2_655 ? N1 Ag1 Br1 89.18(7) . 2_655 ? Br1 Ag1 Br1 107.92(2) . 2_655 ? Br1 Ag1 Br1 103.624(19) 12_656 2_655 ? Ag1 Ag1 Br1 52.98(3) 12_656 2_655 ? Ag1 Ag1 Br1 100.157(16) 11_666 2_655 ? Ag1' Ag1 Ag1' 145.7(5) . 12_656 ? N1 Ag1 Ag1' 111.13(13) . 12_656 ? Br1 Ag1 Ag1' 122.86(9) . 12_656 ? Br1 Ag1 Ag1' 49.16(8) 12_656 12_656 ? Ag1 Ag1 Ag1' 11.96(8) 12_656 12_656 ? Ag1 Ag1 Ag1' 72.27(10) 11_666 12_656 ? Br1 Ag1 Ag1' 54.81(9) 2_655 12_656 ? Ag1' Ag1 Ag1 132.3(4) . 2_655 ? N1 Ag1 Ag1 131.51(7) . 2_655 ? Br1 Ag1 Ag1 62.996(19) . 2_655 ? Br1 Ag1 Ag1 104.699(16) 12_656 2_655 ? Ag1 Ag1 Ag1 58.350(14) 12_656 2_655 ? Ag1 Ag1 Ag1 58.350(14) 11_666 2_655 ? Br1 Ag1 Ag1 49.895(17) 2_655 2_655 ? Ag1' Ag1 Ag1 69.34(7) 12_656 2_655 ? Ag1 Ag1' N1 87.1(5) . . ? Ag1 Ag1' Br1 96.3(5) . . ? N1 Ag1' Br1 134.8(3) . . ? Ag1 Ag1' Br1 70.2(5) . 12_656 ? N1 Ag1' Br1 107.01(18) . 12_656 ? Br1 Ag1' Br1 116.52(17) . 12_656 ? Ag1 Ag1' Ag1 71.9(4) . 11_666 ? N1 Ag1' Ag1 158.2(2) . 11_666 ? Br1 Ag1' Ag1 56.03(9) . 11_666 ? Br1 Ag1' Ag1 60.93(9) 12_656 11_666 ? C2 C1 N2 105.3(3) . . ? C2 C1 H1 127.4 . . ? N2 C1 H1 127.4 . . ? C1 C2 N1 110.3(3) . . ? C1 C2 H2 124.8 . . ? N1 C2 H2 124.8 . . ? N2 C3 N1 112.2(3) . . ? N2 C3 H3 123.9 . . ? N1 C3 H3 123.9 . . ? N2 C4 C5 117.39(19) . . ? N2 C4 H4A 108.0 . . ? C5 C4 H4A 108.0 . . ? N2 C4 H4B 108.0 . . ? C5 C4 H4B 108.0 . . ? H4A C4 H4B 107.2 . . ? C4 C5 C4 113.22(10) 2_645 15_655 ? C4 C5 C4 102.2(2) 2_645 . ? C4 C5 C4 113.22(10) 15_655 . ? C4 C5 C4 113.22(10) 2_645 16_545 ? C4 C5 C4 102.2(2) 15_655 16_545 ? C4 C5 C4 113.22(10) . 16_545 ? C3 N1 C2 104.9(2) . . ? C3 N1 Ag1' 142.4(2) . . ? C2 N1 Ag1' 112.5(2) . . ? C3 N1 Ag1 126.3(2) . . ? C2 N1 Ag1 128.6(2) . . ? Ag1' N1 Ag1 17.10(12) . . ? C3 N2 C1 107.3(2) . . ? C3 N2 C4 129.2(2) . . ? C1 N2 C4 123.4(2) . . ? Ag1' Br1 Ag1 14.40(11) . . ? Ag1' Br1 Ag1 74.80(12) . 11_666 ? Ag1 Br1 Ag1 68.77(2) . 11_666 ? Ag1' Br1 Ag1' 87.99(14) . 11_666 ? Ag1 Br1 Ag1' 81.70(11) . 11_666 ? Ag1 Br1 Ag1' 13.19(10) 11_666 11_666 ? Ag1' Br1 Ag1 81.51(11) . 2_655 ? Ag1 Br1 Ag1 67.11(2) . 2_655 ? Ag1 Br1 Ag1 62.655(19) 11_666 2_655 ? Ag1' Br1 Ag1 64.26(9) 11_666 2_655 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Br1 Ag1 Ag1' N1 134.8(3) . . . . ? Br1 Ag1 Ag1' N1 -109.25(14) 12_656 . . . ? Ag1 Ag1 Ag1' N1 -128.3(6) 12_656 . . . ? Ag1 Ag1 Ag1' N1 -174.06(9) 11_666 . . . ? Br1 Ag1 Ag1' N1 48.1(11) 2_655 . . . ? Ag1' Ag1 Ag1' N1 -106.8(6) 12_656 . . . ? Ag1 Ag1 Ag1' N1 134.0(4) 2_655 . . . ? N1 Ag1 Ag1' Br1 -134.8(3) . . . . ? Br1 Ag1 Ag1' Br1 115.96(17) 12_656 . . . ? Ag1 Ag1 Ag1' Br1 96.9(7) 12_656 . . . ? Ag1 Ag1 Ag1' Br1 51.1(2) 11_666 . . . ? Br1 Ag1 Ag1' Br1 -86.7(10) 2_655 . . . ? Ag1' Ag1 Ag1' Br1 118.4(6) 12_656 . . . ? Ag1 Ag1 Ag1' Br1 -0.8(7) 2_655 . . . ? N1 Ag1 Ag1' Br1 109.25(14) . . . 12_656 ? Br1 Ag1 Ag1' Br1 -115.96(17) . . . 12_656 ? Ag1 Ag1 Ag1' Br1 -19.0(6) 12_656 . . 12_656 ? Ag1 Ag1 Ag1' Br1 -64.81(8) 11_666 . . 12_656 ? Br1 Ag1 Ag1' Br1 157.3(11) 2_655 . . 12_656 ? Ag1' Ag1 Ag1' Br1 2.4(6) 12_656 . . 12_656 ? Ag1 Ag1 Ag1' Br1 -116.8(5) 2_655 . . 12_656 ? N1 Ag1 Ag1' Ag1 174.06(9) . . . 11_666 ? Br1 Ag1 Ag1' Ag1 -51.1(2) . . . 11_666 ? Br1 Ag1 Ag1' Ag1 64.81(8) 12_656 . . 11_666 ? Ag1 Ag1 Ag1' Ag1 45.8(7) 12_656 . . 11_666 ? Br1 Ag1 Ag1' Ag1 -137.8(11) 2_655 . . 11_666 ? Ag1' Ag1 Ag1' Ag1 67.2(6) 12_656 . . 11_666 ? Ag1 Ag1 Ag1' Ag1 -52.0(4) 2_655 . . 11_666 ? N2 C1 C2 N1 0.8(3) . . . . ? N2 C4 C5 C4 159.9(3) . . . 2_645 ? N2 C4 C5 C4 -78.0(3) . . . 15_655 ? N2 C4 C5 C4 37.8(3) . . . 16_545 ? N2 C3 N1 C2 -0.7(3) . . . . ? N2 C3 N1 Ag1' 175.3(3) . . . . ? N2 C3 N1 Ag1 -176.58(19) . . . . ? C1 C2 N1 C3 -0.1(3) . . . . ? C1 C2 N1 Ag1' -177.5(3) . . . . ? C1 C2 N1 Ag1 175.6(2) . . . . ? Ag1 Ag1' N1 C3 22.7(8) . . . . ? Br1 Ag1' N1 C3 118.7(4) . . . . ? Br1 Ag1' N1 C3 -45.5(5) 12_656 . . . ? Ag1 Ag1' N1 C3 7.4(10) 11_666 . . . ? Ag1 Ag1' N1 C2 -161.4(5) . . . . ? Br1 Ag1' N1 C2 -65.4(4) . . . . ? Br1 Ag1' N1 C2 130.3(2) 12_656 . . . ? Ag1 Ag1' N1 C2 -176.8(6) 11_666 . . . ? Br1 Ag1' N1 Ag1 96.0(7) . . . . ? Br1 Ag1' N1 Ag1 -68.3(4) 12_656 . . . ? Ag1 Ag1' N1 Ag1 -15.4(3) 11_666 . . . ? Ag1' Ag1 N1 C3 -163.0(6) . . . . ? Br1 Ag1 N1 C3 144.2(2) . . . . ? Br1 Ag1 N1 C3 -71.1(3) 12_656 . . . ? Ag1 Ag1 N1 C3 -11.3(3) 12_656 . . . ? Ag1 Ag1 N1 C3 -126.5(4) 11_666 . . . ? Br1 Ag1 N1 C3 33.1(3) 2_655 . . . ? Ag1' Ag1 N1 C3 -18.3(3) 12_656 . . . ? Ag1 Ag1 N1 C3 62.3(3) 2_655 . . . ? Ag1' Ag1 N1 C2 22.2(6) . . . . ? Br1 Ag1 N1 C2 -30.6(3) . . . . ? Br1 Ag1 N1 C2 114.1(2) 12_656 . . . ? Ag1 Ag1 N1 C2 173.8(2) 12_656 . . . ? Ag1 Ag1 N1 C2 58.7(5) 11_666 . . . ? Br1 Ag1 N1 C2 -141.7(2) 2_655 . . . ? Ag1' Ag1 N1 C2 166.9(2) 12_656 . . . ? Ag1 Ag1 N1 C2 -112.5(2) 2_655 . . . ? Br1 Ag1 N1 Ag1' -52.8(5) . . . . ? Br1 Ag1 N1 Ag1' 91.9(5) 12_656 . . . ? Ag1 Ag1 N1 Ag1' 151.7(5) 12_656 . . . ? Ag1 Ag1 N1 Ag1' 36.5(6) 11_666 . . . ? Br1 Ag1 N1 Ag1' -163.9(5) 2_655 . . . ? Ag1' Ag1 N1 Ag1' 144.7(5) 12_656 . . . ? Ag1 Ag1 N1 Ag1' -134.7(5) 2_655 . . . ? N1 C3 N2 C1 1.3(3) . . . . ? N1 C3 N2 C4 177.1(2) . . . . ? C2 C1 N2 C3 -1.3(3) . . . . ? C2 C1 N2 C4 -177.4(2) . . . . ? C5 C4 N2 C3 66.6(4) . . . . ? C5 C4 N2 C1 -118.2(3) . . . . ? N1 Ag1' Br1 Ag1 -92.1(7) . . . . ? Br1 Ag1' Br1 Ag1 71.0(5) 12_656 . . . ? Ag1 Ag1' Br1 Ag1 63.2(5) 11_666 . . . ? Ag1 Ag1' Br1 Ag1 -63.2(5) . . . 11_666 ? N1 Ag1' Br1 Ag1 -155.4(3) . . . 11_666 ? Br1 Ag1' Br1 Ag1 7.78(15) 12_656 . . 11_666 ? Ag1 Ag1' Br1 Ag1' -63.6(5) . . . 11_666 ? N1 Ag1' Br1 Ag1' -155.8(3) . . . 11_666 ? Br1 Ag1' Br1 Ag1' 7.37(19) 12_656 . . 11_666 ? Ag1 Ag1' Br1 Ag1' -0.41(10) 11_666 . . 11_666 ? Ag1 Ag1' Br1 Ag1 0.6(5) . . . 2_655 ? N1 Ag1' Br1 Ag1 -91.5(3) . . . 2_655 ? Br1 Ag1' Br1 Ag1 71.63(16) 12_656 . . 2_655 ? Ag1 Ag1' Br1 Ag1 63.85(3) 11_666 . . 2_655 ? N1 Ag1 Br1 Ag1' 55.6(5) . . . . ? Br1 Ag1 Br1 Ag1' -87.0(6) 12_656 . . . ? Ag1 Ag1 Br1 Ag1' -146.7(6) 12_656 . . . ? Ag1 Ag1 Br1 Ag1' -112.5(6) 11_666 . . . ? Br1 Ag1 Br1 Ag1' 156.9(6) 2_655 . . . ? Ag1' Ag1 Br1 Ag1' -143.9(5) 12_656 . . . ? Ag1 Ag1 Br1 Ag1' 179.3(6) 2_655 . . . ? Ag1' Ag1 Br1 Ag1 112.5(6) . . . 11_666 ? N1 Ag1 Br1 Ag1 168.08(9) . . . 11_666 ? Br1 Ag1 Br1 Ag1 25.41(3) 12_656 . . 11_666 ? Ag1 Ag1 Br1 Ag1 -34.20(3) 12_656 . . 11_666 ? Br1 Ag1 Br1 Ag1 -90.60(2) 2_655 . . 11_666 ? Ag1' Ag1 Br1 Ag1 -31.41(10) 12_656 . . 11_666 ? Ag1 Ag1 Br1 Ag1 -68.229(16) 2_655 . . 11_666 ? Ag1' Ag1 Br1 Ag1' 115.2(5) . . . 11_666 ? N1 Ag1 Br1 Ag1' 170.82(12) . . . 11_666 ? Br1 Ag1 Br1 Ag1' 28.15(9) 12_656 . . 11_666 ? Ag1 Ag1 Br1 Ag1' -31.46(9) 12_656 . . 11_666 ? Ag1 Ag1 Br1 Ag1' 2.74(10) 11_666 . . 11_666 ? Br1 Ag1 Br1 Ag1' -87.86(10) 2_655 . . 11_666 ? Ag1' Ag1 Br1 Ag1' -28.67(15) 12_656 . . 11_666 ? Ag1 Ag1 Br1 Ag1' -65.49(9) 2_655 . . 11_666 ? Ag1' Ag1 Br1 Ag1 -179.3(6) . . . 2_655 ? N1 Ag1 Br1 Ag1 -123.69(9) . . . 2_655 ? Br1 Ag1 Br1 Ag1 93.64(2) 12_656 . . 2_655 ? Ag1 Ag1 Br1 Ag1 34.03(3) 12_656 . . 2_655 ? Ag1 Ag1 Br1 Ag1 68.229(16) 11_666 . . 2_655 ? Br1 Ag1 Br1 Ag1 -22.37(3) 2_655 . . 2_655 ? Ag1' Ag1 Br1 Ag1 36.82(9) 12_656 . . 2_655 ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.583 _refine_diff_density_min -0.710 _refine_diff_density_rms 0.082 #===END data_compound-3 _database_code_depnum_ccdc_archive 'CCDC 800208' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H20 Ag2 N8, C4 H2 O4, 6.25(H2 O)' _chemical_formula_sum 'C21 H34.50 Ag2 N8 O10.25' _chemical_formula_weight 778.81 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 'C 2/c' _symmetry_space_group_name_hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.3312(14) _cell_length_b 27.3761(14) _cell_length_c 13.1924(9) _cell_angle_alpha 90.00 _cell_angle_beta 114.059(9) _cell_angle_gamma 90.00 _cell_volume 6375.1(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5801 _cell_measurement_theta_min 4.1 _cell_measurement_theta_max 25.4 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3140 _exptl_absorpt_coefficient_mu 1.289 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.804 _exptl_absorpt_correction_T_max 0.913 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12797 _diffrn_reflns_av_R_equivalents 0.1000 _diffrn_reflns_av_sigmaI/netI 0.2800 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.12 _diffrn_reflns_theta_max 25.35 _reflns_number_total 5801 _reflns_number_gt 1739 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^ > 2\s(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. H atoms of water were located in difference Fourier maps and refined isotropically with distance restraints of O---H = 0.85+-0.03 \%A with U~iso~ = 1.5U~eq~(O). The distance of H1WC...HW1D was restrained to 1.44+-0.05 \%A. In order to give reasonable C...O distances, the distances of C21---O3, C21---O4 and O4---C20 were restrained to 1.25+-0.02 \%A, 1.25+-0.02 \%A and 2.4+-0.02 \%A, repectively. In order to give a reasonable C...C distance, the distance of C19---C20 was restrained to 1.3+-0.02 \%A. In order to give a reasonable O...O distance, the distance of O1---O6w was restrained to 2.8+-0.02 \%A. For C6, C7 and O4w atoms, some anisotropic displacement ellipsoids were rather elongated which led us to use the ISOR or SIMU restraints. ; _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^)+(0.0779P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5801 _refine_ls_number_parameters 354 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.2070 _refine_ls_R_factor_gt 0.0616 _refine_ls_wR_factor_ref 0.1690 _refine_ls_wR_factor_gt 0.1408 _refine_ls_goodness_of_fit_ref 0.721 _refine_ls_restrained_S_all 0.727 _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 0.93506(5) 0.16778(3) 0.79648(7) 0.0707(4) Uani 1 1 d . . . Ag2 Ag 1.02009(6) 0.52665(4) 0.88529(7) 0.0786(4) Uani 1 1 d . . . C1 C 0.7234(5) 0.3135(3) 0.6251(8) 0.047(3) Uani 1 1 d . . . H1A H 0.6884 0.2934 0.6425 0.057 Uiso 1 1 calc R . . H1B H 0.6975 0.3243 0.5488 0.057 Uiso 1 1 calc R . . C2 C 0.8106(6) 0.2435(4) 0.6993(8) 0.047(3) Uani 1 1 d . . . H2 H 0.7885 0.2325 0.7459 0.057 Uiso 1 1 calc R . . C3 C 0.8323(7) 0.2868(4) 0.5780(8) 0.053(3) Uani 1 1 d . . . H3 H 0.8298 0.3103 0.5258 0.063 Uiso 1 1 calc R . . C4 C 0.8805(6) 0.2492(4) 0.6118(9) 0.050(3) Uani 1 1 d . . . H4 H 0.9179 0.2428 0.5862 0.060 Uiso 1 1 calc R . . C5 C 0.5609(6) 0.3590(4) 0.5184(9) 0.054(3) Uani 1 1 d . . . H5 H 0.5522 0.3295 0.5465 0.064 Uiso 1 1 calc R . . C6 C 0.5502(6) 0.4178(4) 0.4133(9) 0.064(2) Uani 1 1 d U . . H6 H 0.5326 0.4386 0.3522 0.077 Uiso 1 1 calc R . . C7 C 0.6089(6) 0.4281(4) 0.5112(9) 0.064(2) Uani 1 1 d U . . H7 H 0.6389 0.4560 0.5283 0.077 Uiso 1 1 calc R . . C8 C 0.6704(5) 0.3828(3) 0.6911(8) 0.050(3) Uani 1 1 d . . . H8A H 0.6478 0.3625 0.7297 0.060 Uiso 1 1 calc R . . H8B H 0.6817 0.4142 0.7281 0.060 Uiso 1 1 calc R . . C9 C 0.7442(5) 0.3595(3) 0.7027(8) 0.045(3) Uani 1 1 d . . . C10 C 0.7921(6) 0.3921(4) 0.6651(9) 0.058(3) Uani 1 1 d . . . H10A H 0.8335 0.3722 0.6643 0.070 Uiso 1 1 calc R . . H10B H 0.7614 0.4009 0.5886 0.070 Uiso 1 1 calc R . . C11 C 0.7921(7) 0.4786(5) 0.7405(9) 0.067(3) Uani 1 1 d . . . H11 H 0.7404 0.4828 0.7196 0.081 Uiso 1 1 calc R . . C12 C 0.8468(8) 0.5119(4) 0.7919(9) 0.069(4) Uani 1 1 d . . . H12 H 0.8392 0.5432 0.8130 0.082 Uiso 1 1 calc R . . C13 C 0.9004(7) 0.4473(4) 0.7670(10) 0.065(4) Uani 1 1 d . . . H13 H 0.9368 0.4249 0.7676 0.077 Uiso 1 1 calc R . . C14 C 0.8081(8) 0.4347(5) 1.0240(10) 0.071(4) Uani 1 1 d . . . H14 H 0.7920 0.4566 1.0640 0.085 Uiso 1 1 calc R . . C15 C 0.7643(7) 0.4036(5) 0.9487(10) 0.067(4) Uani 1 1 d . . . H15 H 0.7125 0.3992 0.9268 0.081 Uiso 1 1 calc R . . C16 C 0.8806(6) 0.3956(4) 0.9632(9) 0.056(3) Uani 1 1 d . . . H16 H 0.9226 0.3847 0.9521 0.068 Uiso 1 1 calc R . . C17 C 0.7892(6) 0.3402(4) 0.8242(8) 0.060(3) Uani 1 1 d . . . C18 C 0.878(2) 0.3528(12) 0.339(3) 0.244(13) Uiso 1 1 d . . . C19 C 0.9026(13) 0.3482(8) 0.263(2) 0.161(8) Uiso 1 1 d D . . C20 C 0.9015(14) 0.3092(10) 0.209(2) 0.211(10) Uiso 1 1 d D . . C21 C 0.8836(16) 0.2553(11) 0.2543(18) 0.199(10) Uiso 1 1 d D . . N1 N 0.7880(5) 0.2838(3) 0.6343(7) 0.041(2) Uani 1 1 d . . . N2 N 0.8680(5) 0.2218(3) 0.6878(7) 0.055(3) Uani 1 1 d . . . N3 N 0.5207(4) 0.3732(3) 0.4166(7) 0.054(3) Uani 1 1 d . . . N4 N 0.6153(4) 0.3900(3) 0.5787(6) 0.048(2) Uani 1 1 d . . . N5 N 0.8263(5) 0.4382(3) 0.7250(7) 0.048(2) Uani 1 1 d . . . N6 N 0.9157(6) 0.4917(3) 0.8076(7) 0.062(3) Uani 1 1 d . . . N7 N 0.8803(5) 0.4297(4) 1.0336(7) 0.062(3) Uani 1 1 d . . . N8 N 0.8088(5) 0.3796(3) 0.9101(7) 0.052(2) Uani 1 1 d . . . O1 O 0.9362(10) 0.3736(6) 0.4379(14) 0.210(6) Uiso 1 1 d D . . O2 O 0.8140(9) 0.3577(5) 0.3499(11) 0.167(5) Uiso 1 1 d . . . O3 O 0.9098(8) 0.2534(5) 0.3572(12) 0.159(5) Uiso 1 1 d D . . O4 O 0.821(2) 0.2422(12) 0.176(3) 0.241(16) Uiso 0.50 1 d PD . . O4' O 0.8834(18) 0.2179(12) 0.206(3) 0.181(11) Uiso 0.50 1 d P . . O3W O 0.6908(8) 0.3600(5) 0.1615(12) 0.182(6) Uani 1 1 d . . . O7W O 0.8333(13) 0.2190(8) -0.0170(14) 0.128(8) Uani 0.50 1 d P . . O1W O 1.0228(6) 0.3355(3) 0.6633(8) 0.108(3) Uani 1 1 d D . . O2W O 1.0369(7) 0.2564(4) 0.5303(9) 0.138(4) Uani 1 1 d . . . O4W O 0.6342(9) 0.5487(6) 0.5786(13) 0.082(5) Uani 0.50 1 d PU . . O5W O 0.6093(12) 0.4976(7) 0.7507(18) 0.136(8) Uani 0.50 1 d P . . O6W O 0.9012(11) 0.4392(6) 0.5521(15) 0.113(6) Uiso 0.50 1 d PD . . O8W O 1.0000 0.1555(12) 0.2500 0.155(12) Uiso 0.50 2 d SP . . O9W O 0.7366(15) 0.4278(10) 0.402(2) 0.172(10) Uiso 0.50 1 d P . . O10W O 0.5484(19) 0.5566(12) 0.367(3) 0.209(12) Uiso 0.50 1 d P . . H1C H 0.996(15) 0.326(9) 0.598(8) 0.314 Uiso 1 1 d D . . H1D H 1.030(16) 0.314(7) 0.714(14) 0.314 Uiso 1 1 d 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 0.0557(6) 0.0654(6) 0.0728(6) 0.0139(5) 0.0075(5) 0.0143(5) Ag2 0.0804(7) 0.0854(7) 0.0597(6) -0.0171(5) 0.0180(5) -0.0432(6) C1 0.036(6) 0.034(6) 0.055(6) -0.022(5) 0.001(5) -0.005(5) C2 0.053(7) 0.031(6) 0.055(7) 0.005(5) 0.018(6) -0.003(5) C3 0.080(9) 0.037(7) 0.043(6) 0.009(5) 0.027(7) 0.009(6) C4 0.039(7) 0.050(7) 0.060(7) -0.005(6) 0.019(6) -0.004(6) C5 0.048(7) 0.045(6) 0.062(7) 0.003(6) 0.016(6) -0.006(6) C6 0.063(2) 0.063(2) 0.064(2) 0.0006(10) 0.0244(12) -0.0012(10) C7 0.063(3) 0.063(3) 0.064(3) 0.0005(14) 0.0233(16) -0.0018(14) C8 0.043(6) 0.040(6) 0.050(6) -0.004(5) 0.003(5) -0.013(5) C9 0.030(6) 0.034(6) 0.067(7) -0.008(5) 0.014(5) -0.003(5) C10 0.053(7) 0.044(7) 0.071(7) -0.015(6) 0.019(6) -0.005(6) C11 0.054(7) 0.071(9) 0.070(8) 0.006(7) 0.018(6) -0.007(7) C12 0.074(9) 0.047(7) 0.072(8) -0.016(6) 0.017(7) -0.030(7) C13 0.052(8) 0.037(7) 0.097(9) 0.000(7) 0.021(7) -0.009(6) C14 0.067(9) 0.092(10) 0.060(8) -0.014(7) 0.033(7) 0.014(8) C15 0.049(8) 0.097(10) 0.058(8) -0.011(7) 0.025(7) -0.013(8) C16 0.040(7) 0.056(7) 0.056(7) -0.018(6) 0.003(6) -0.016(6) C17 0.058(7) 0.058(7) 0.041(6) -0.012(6) -0.003(5) 0.001(6) N1 0.040(5) 0.037(5) 0.039(5) -0.014(4) 0.010(5) -0.005(4) N2 0.052(6) 0.047(6) 0.055(6) 0.004(5) 0.010(5) 0.014(5) N3 0.037(5) 0.039(5) 0.067(6) -0.012(5) 0.004(5) -0.018(4) N4 0.043(5) 0.033(5) 0.054(5) -0.003(4) 0.004(4) -0.002(4) N5 0.046(6) 0.041(5) 0.056(5) -0.026(4) 0.021(5) -0.017(5) N6 0.059(7) 0.051(6) 0.077(7) -0.012(5) 0.028(6) -0.031(5) N7 0.053(7) 0.071(7) 0.054(6) -0.012(5) 0.015(5) -0.022(5) N8 0.042(6) 0.050(6) 0.056(6) -0.009(5) 0.012(5) -0.012(5) O3W 0.165(12) 0.173(11) 0.218(13) 0.077(10) 0.089(10) 0.024(10) O7W 0.155(19) 0.137(17) 0.085(13) 0.009(12) 0.042(13) -0.068(15) O1W 0.099(7) 0.095(7) 0.116(7) 0.011(6) 0.030(6) -0.031(6) O2W 0.143(10) 0.148(9) 0.147(9) -0.012(8) 0.082(8) -0.021(8) O4W 0.081(5) 0.081(5) 0.082(5) -0.0002(10) 0.033(2) -0.0002(10) O5W 0.130(17) 0.128(16) 0.161(18) -0.033(14) 0.072(14) 0.087(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 2.090(7) 8_556 ? Ag1 N2 2.100(8) . ? Ag1 Ag1 3.212(2) 2_756 ? Ag2 N6 2.086(8) . ? Ag2 N7 2.146(9) 5_767 ? Ag2 Ag2 3.3294(19) 2_756 ? C1 N1 1.454(12) . ? C1 C9 1.567(12) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.322(13) . ? C2 N1 1.356(11) . ? C2 H2 0.9300 . ? C3 C4 1.336(13) . ? C3 N1 1.345(13) . ? C3 H3 0.9300 . ? C4 N2 1.350(13) . ? C4 H4 0.9300 . ? C5 N3 1.306(11) . ? C5 N4 1.334(11) . ? C5 H5 0.9300 . ? C6 C7 1.357(13) . ? C6 N3 1.357(12) . ? C6 H6 0.9300 . ? C7 N4 1.343(13) . ? C7 H7 0.9300 . ? C8 N4 1.443(10) . ? C8 C9 1.512(13) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.508(14) . ? C9 C17 1.571(13) . ? C10 N5 1.493(11) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N5 1.347(13) . ? C11 C12 1.351(13) . ? C11 H11 0.9300 . ? C12 N6 1.378(14) . ? C12 H12 0.9300 . ? C13 N6 1.314(12) . ? C13 N5 1.330(12) . ? C13 H13 0.9300 . ? C14 C15 1.321(14) . ? C14 N7 1.357(14) . ? C14 H14 0.9300 . ? C15 N8 1.338(14) . ? C15 H15 0.9300 . ? C16 N7 1.317(13) . ? C16 N8 1.349(12) . ? C16 H16 0.9300 . ? C17 N8 1.496(12) . ? C18 C19 1.28(4) . ? C18 O2 1.30(4) . ? C18 O1 1.45(3) . ? C19 C20 1.274(17) . ? C20 C21 1.68(3) . ? C21 O4' 1.20(3) . ? C21 O3 1.241(16) . ? C21 O4 1.285(18) . ? N3 Ag1 2.090(7) 8_455 ? N7 Ag2 2.146(8) 5_767 ? O4 O4' 1.29(4) . ? O1W H1C 0.85(3) . ? O1W H1D 0.85(3) . ? 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 N2 166.7(3) 8_556 . ? N3 Ag1 Ag1 77.8(3) 8_556 2_756 ? N2 Ag1 Ag1 95.7(3) . 2_756 ? N6 Ag2 N7 172.9(4) . 5_767 ? N6 Ag2 Ag2 73.6(3) . 2_756 ? N7 Ag2 Ag2 107.7(3) 5_767 2_756 ? N1 C1 C9 114.4(7) . . ? N1 C1 H1A 108.7 . . ? C9 C1 H1A 108.7 . . ? N1 C1 H1B 108.7 . . ? C9 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? N2 C2 N1 111.2(10) . . ? N2 C2 H2 124.4 . . ? N1 C2 H2 124.4 . . ? C4 C3 N1 106.5(10) . . ? C4 C3 H3 126.8 . . ? N1 C3 H3 126.8 . . ? C3 C4 N2 111.4(11) . . ? C3 C4 H4 124.3 . . ? N2 C4 H4 124.3 . . ? N3 C5 N4 114.7(9) . . ? N3 C5 H5 122.7 . . ? N4 C5 H5 122.7 . . ? C7 C6 N3 110.8(10) . . ? C7 C6 H6 124.6 . . ? N3 C6 H6 124.6 . . ? N4 C7 C6 106.6(10) . . ? N4 C7 H7 126.7 . . ? C6 C7 H7 126.7 . . ? N4 C8 C9 115.7(9) . . ? N4 C8 H8A 108.4 . . ? C9 C8 H8A 108.4 . . ? N4 C8 H8B 108.4 . . ? C9 C8 H8B 108.4 . . ? H8A C8 H8B 107.4 . . ? C10 C9 C8 113.5(8) . . ? C10 C9 C1 106.8(9) . . ? C8 C9 C1 107.0(7) . . ? C10 C9 C17 112.1(8) . . ? C8 C9 C17 110.6(9) . . ? C1 C9 C17 106.5(7) . . ? N5 C10 C9 121.6(9) . . ? N5 C10 H10A 106.9 . . ? C9 C10 H10A 106.9 . . ? N5 C10 H10B 106.9 . . ? C9 C10 H10B 106.9 . . ? H10A C10 H10B 106.7 . . ? N5 C11 C12 107.4(11) . . ? N5 C11 H11 126.3 . . ? C12 C11 H11 126.3 . . ? C11 C12 N6 108.3(11) . . ? C11 C12 H12 125.8 . . ? N6 C12 H12 125.8 . . ? N6 C13 N5 111.6(11) . . ? N6 C13 H13 124.2 . . ? N5 C13 H13 124.2 . . ? C15 C14 N7 108.9(11) . . ? C15 C14 H14 125.6 . . ? N7 C14 H14 125.6 . . ? C14 C15 N8 106.8(11) . . ? C14 C15 H15 126.6 . . ? N8 C15 H15 126.6 . . ? N7 C16 N8 107.3(10) . . ? N7 C16 H16 126.4 . . ? N8 C16 H16 126.4 . . ? N8 C17 C9 113.3(8) . . ? C19 C18 O2 141(4) . . ? C19 C18 O1 110(3) . . ? O2 C18 O1 106(3) . . ? C20 C19 C18 126(3) . . ? C19 C20 C21 120(3) . . ? O4' C21 O3 117(3) . . ? O4' C21 O4 62(2) . . ? O3 C21 O4 135(3) . . ? O4' C21 C20 121(3) . . ? O3 C21 C20 112(2) . . ? O4 C21 C20 102.9(19) . . ? C3 N1 C2 106.6(9) . . ? C3 N1 C1 129.6(9) . . ? C2 N1 C1 123.5(10) . . ? C2 N2 C4 104.4(9) . . ? C2 N2 Ag1 123.4(9) . . ? C4 N2 Ag1 130.7(8) . . ? C5 N3 C6 102.7(8) . . ? C5 N3 Ag1 125.1(7) . 8_455 ? C6 N3 Ag1 132.2(7) . 8_455 ? C5 N4 C7 105.2(8) . . ? C5 N4 C8 126.7(8) . . ? C7 N4 C8 128.1(8) . . ? C13 N5 C11 107.1(9) . . ? C13 N5 C10 123.2(10) . . ? C11 N5 C10 129.5(9) . . ? C13 N6 C12 105.5(9) . . ? C13 N6 Ag2 129.6(9) . . ? C12 N6 Ag2 124.9(7) . . ? C16 N7 C14 107.9(9) . . ? C16 N7 Ag2 119.0(8) . 5_767 ? C14 N7 Ag2 132.0(9) . 5_767 ? C15 N8 C16 109.1(9) . . ? C15 N8 C17 129.7(10) . . ? C16 N8 C17 121.2(11) . . ? C21 O4 O4' 56(2) . . ? C21 O4' O4 61.9(18) . . ? H1C O1W H1D 114(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C3 C4 N2 0.6(11) . . . . ? N3 C6 C7 N4 -1.8(13) . . . . ? N4 C8 C9 C10 69.0(10) . . . . ? N4 C8 C9 C1 -48.4(11) . . . . ? N4 C8 C9 C17 -164.0(8) . . . . ? N1 C1 C9 C10 64.0(11) . . . . ? N1 C1 C9 C8 -174.2(9) . . . . ? N1 C1 C9 C17 -55.9(12) . . . . ? C8 C9 C10 N5 66.2(12) . . . . ? C1 C9 C10 N5 -176.2(8) . . . . ? C17 C9 C10 N5 -60.0(12) . . . . ? N5 C11 C12 N6 0.4(13) . . . . ? N7 C14 C15 N8 -0.8(14) . . . . ? C10 C9 C17 N8 67.6(11) . . . . ? C8 C9 C17 N8 -60.1(11) . . . . ? C1 C9 C17 N8 -176.0(9) . . . . ? O2 C18 C19 C20 -78(6) . . . . ? O1 C18 C19 C20 127(3) . . . . ? C18 C19 C20 C21 -14(5) . . . . ? C19 C20 C21 O4' -179(3) . . . . ? C19 C20 C21 O3 -34(4) . . . . ? C19 C20 C21 O4 116(3) . . . . ? C4 C3 N1 C2 -1.2(10) . . . . ? C4 C3 N1 C1 -176.0(8) . . . . ? N2 C2 N1 C3 1.4(10) . . . . ? N2 C2 N1 C1 176.6(7) . . . . ? C9 C1 N1 C3 -89.8(11) . . . . ? C9 C1 N1 C2 96.2(10) . . . . ? N1 C2 N2 C4 -1.0(10) . . . . ? N1 C2 N2 Ag1 166.4(6) . . . . ? C3 C4 N2 C2 0.3(11) . . . . ? C3 C4 N2 Ag1 -165.8(7) . . . . ? N3 Ag1 N2 C2 -108.2(18) 8_556 . . . ? Ag1 Ag1 N2 C2 -168.4(7) 2_756 . . . ? N3 Ag1 N2 C4 56(2) 8_556 . . . ? Ag1 Ag1 N2 C4 -4.6(8) 2_756 . . . ? N4 C5 N3 C6 -2.4(13) . . . . ? N4 C5 N3 Ag1 176.5(7) . . . 8_455 ? C7 C6 N3 C5 2.5(13) . . . . ? C7 C6 N3 Ag1 -176.2(8) . . . 8_455 ? N3 C5 N4 C7 1.3(13) . . . . ? N3 C5 N4 C8 -176.5(10) . . . . ? C6 C7 N4 C5 0.3(12) . . . . ? C6 C7 N4 C8 178.2(10) . . . . ? C9 C8 N4 C5 91.1(12) . . . . ? C9 C8 N4 C7 -86.3(13) . . . . ? N6 C13 N5 C11 -0.8(14) . . . . ? N6 C13 N5 C10 174.8(9) . . . . ? C12 C11 N5 C13 0.2(13) . . . . ? C12 C11 N5 C10 -175.0(10) . . . . ? C9 C10 N5 C13 122.9(11) . . . . ? C9 C10 N5 C11 -62.5(15) . . . . ? N5 C13 N6 C12 1.0(14) . . . . ? N5 C13 N6 Ag2 179.2(7) . . . . ? C11 C12 N6 C13 -0.8(13) . . . . ? C11 C12 N6 Ag2 -179.1(7) . . . . ? N7 Ag2 N6 C13 178(3) 5_767 . . . ? Ag2 Ag2 N6 C13 76.6(10) 2_756 . . . ? N7 Ag2 N6 C12 -4(4) 5_767 . . . ? Ag2 Ag2 N6 C12 -105.6(9) 2_756 . . . ? N8 C16 N7 C14 -0.1(12) . . . . ? N8 C16 N7 Ag2 -169.6(6) . . . 5_767 ? C15 C14 N7 C16 0.6(14) . . . . ? C15 C14 N7 Ag2 168.3(8) . . . 5_767 ? C14 C15 N8 C16 0.8(13) . . . . ? C14 C15 N8 C17 179.9(10) . . . . ? N7 C16 N8 C15 -0.5(12) . . . . ? N7 C16 N8 C17 -179.6(8) . . . . ? C9 C17 N8 C15 73.3(14) . . . . ? C9 C17 N8 C16 -107.8(10) . . . . ? O3 C21 O4 O4' -102(5) . . . . ? C20 C21 O4 O4' 119(3) . . . . ? O3 C21 O4' O4 128(4) . . . . ? C20 C21 O4' O4 -89(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1C O1 0.85(3) 2.35(19) 2.95(2) 127(20) . O1W H1D O1W 0.85(3) 2.3(2) 2.77(2) 113(21) 2_756 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.036 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.113 #===END data_compound-4 _database_code_depnum_ccdc_archive 'CCDC 800209' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H24 Ag2 N8 O4, 4(H2 O)' _chemical_formula_sum 'C25 H32 Ag2 N8 O8' _chemical_formula_weight 788.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 11.468(5) _cell_length_b 11.741(5) _cell_length_c 12.142(5) _cell_angle_alpha 85.682(5) _cell_angle_beta 65.808(5) _cell_angle_gamma 77.330(5) _cell_volume 1454.8(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6631 _cell_measurement_theta_min 4.4 _cell_measurement_theta_max 29.3 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.800 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 1.408 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.852 _exptl_absorpt_correction_T_max 0.860 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10728 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 4.42 _diffrn_reflns_theta_max 29.26 _reflns_number_total 6631 _reflns_number_gt 4901 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^ > 2\s(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. H atoms of water molecule were refined isotropically with distance restraints of O---H = 0.85+-0.02 \%A and H...H = 1.44+-0.02 \%A. ; _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^)+(0.0554P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6631 _refine_ls_number_parameters 412 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0990 _refine_ls_wR_factor_gt 0.0939 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 0.81156(3) 0.68947(2) 0.56141(2) 0.04884(11) Uani 1 1 d . . . Ag2 Ag 0.49009(3) 0.20125(3) 0.34363(2) 0.05234(11) Uani 1 1 d . . . C1 C 0.7461(3) 0.4726(2) 0.7296(3) 0.0323(7) Uani 1 1 d . . . H1 H 0.6565 0.4968 0.7515 0.039 Uiso 1 1 calc R . . C2 C 0.9350(3) 0.3678(3) 0.7152(3) 0.0319(7) Uani 1 1 d . . . H2 H 0.9997 0.3088 0.7234 0.038 Uiso 1 1 calc R . . C3 C 0.9519(3) 0.4678(3) 0.6525(3) 0.0335(7) Uani 1 1 d . . . H3 H 1.0318 0.4894 0.6100 0.040 Uiso 1 1 calc R . . C4 C 0.7401(3) 0.2807(2) 0.8396(2) 0.0270(6) Uani 1 1 d . . . H4A H 0.6595 0.3183 0.9040 0.032 Uiso 1 1 calc R . . H4B H 0.7965 0.2370 0.8766 0.032 Uiso 1 1 calc R . . C5 C 0.7082(3) 0.1941(2) 0.7709(2) 0.0226(6) Uani 1 1 d . . . C6 C 0.5989(3) 0.2648(2) 0.7350(3) 0.0284(6) Uani 1 1 d . . . H6A H 0.5243 0.2945 0.8085 0.034 Uiso 1 1 calc R . . H6B H 0.6295 0.3317 0.6896 0.034 Uiso 1 1 calc R . . C7 C 0.5639(3) 0.2373(3) 0.5520(3) 0.0324(7) Uani 1 1 d . . . H7 H 0.6070 0.2952 0.5085 0.039 Uiso 1 1 calc R . . C8 C 0.4821(3) 0.1194(3) 0.6981(3) 0.0311(6) Uani 1 1 d . . . H8 H 0.4584 0.0807 0.7713 0.037 Uiso 1 1 calc R . . C9 C 0.4525(3) 0.1021(3) 0.6039(3) 0.0352(7) Uani 1 1 d . . . H9 H 0.4044 0.0487 0.6017 0.042 Uiso 1 1 calc R . . C10 C 0.8357(3) 0.1437(2) 0.6625(2) 0.0284(6) Uani 1 1 d . . . H10A H 0.8602 0.2063 0.6064 0.034 Uiso 1 1 calc R . . H10B H 0.9043 0.1176 0.6915 0.034 Uiso 1 1 calc R . . C11 C 0.8244(3) 0.0533(2) 0.4856(2) 0.0281(6) Uani 1 1 d . . . H11 H 0.8207 0.1200 0.4395 0.034 Uiso 1 1 calc R . . C12 C 0.8239(3) -0.0555(2) 0.4563(3) 0.0298(6) Uani 1 1 d . . . H12 H 0.8191 -0.0764 0.3861 0.036 Uiso 1 1 calc R . . C13 C 0.8376(3) -0.0662(2) 0.6288(3) 0.0303(7) Uani 1 1 d . . . H13 H 0.8452 -0.0950 0.6995 0.036 Uiso 1 1 calc R . . C14 C 0.6660(3) 0.0935(2) 0.8587(2) 0.0251(6) Uani 1 1 d . . . H14A H 0.6307 0.0450 0.8241 0.030 Uiso 1 1 calc R . . H14B H 0.7428 0.0454 0.8662 0.030 Uiso 1 1 calc R . . C15 C 0.4379(3) 0.1788(3) 1.0144(3) 0.0320(7) Uani 1 1 d . . . H15 H 0.3912 0.1873 0.9662 0.038 Uiso 1 1 calc R . . C16 C 0.3896(3) 0.2094(3) 1.1322(3) 0.0359(7) Uani 1 1 d . . . H16 H 0.3029 0.2424 1.1796 0.043 Uiso 1 1 calc R . . C17 C 0.5955(3) 0.1382(3) 1.0764(3) 0.0347(7) Uani 1 1 d . . . H17 H 0.6780 0.1130 1.0769 0.042 Uiso 1 1 calc R . . C18 C 0.7466(3) 0.6032(3) 0.3375(3) 0.0352(7) Uani 1 1 d . . . C19 C 0.7836(3) 0.6030(3) 0.2028(3) 0.0366(7) Uani 1 1 d . . . C20 C 0.8185(3) 0.7003(3) 0.1350(3) 0.0354(7) Uani 1 1 d . . . H20 H 0.8165 0.7664 0.1739 0.042 Uiso 1 1 calc R . . C21 C 0.8563(3) 0.7014(3) 0.0104(3) 0.0422(8) Uani 1 1 d . . . C22 C 0.8897(4) 0.8088(4) -0.0626(3) 0.0523(10) Uani 1 1 d . . . C23 C 0.8620(4) 0.6003(4) -0.0464(3) 0.0562(11) Uani 1 1 d . . . H23 H 0.8890 0.5985 -0.1298 0.067 Uiso 1 1 calc R . . C24 C 0.8285(5) 0.5040(4) 0.0187(4) 0.0699(13) Uani 1 1 d . . . H24 H 0.8330 0.4374 -0.0209 0.084 Uiso 1 1 calc R . . C25 C 0.7875(4) 0.5040(3) 0.1440(3) 0.0531(10) Uani 1 1 d . . . H25 H 0.7629 0.4384 0.1878 0.064 Uiso 1 1 calc R . . O1 O 0.6935(2) 0.5209(2) 0.3969(2) 0.0485(6) Uani 1 1 d . . . O2 O 0.7726(2) 0.6825(2) 0.3808(2) 0.0420(6) Uani 1 1 d . . . O3 O 0.8664(3) 0.9016(3) -0.0041(3) 0.0677(8) Uani 1 1 d . . . O4 O 0.9318(4) 0.8008(3) -0.1738(2) 0.0843(11) Uani 1 1 d . . . N1 N 0.8330(3) 0.5323(2) 0.6614(2) 0.0340(6) Uani 1 1 d . . . N2 N 0.8036(2) 0.37105(19) 0.7639(2) 0.0274(5) Uani 1 1 d . . . N3 N 0.5535(2) 0.2050(2) 0.6643(2) 0.0270(5) Uani 1 1 d . . . N4 N 0.5054(3) 0.1765(2) 0.5122(2) 0.0349(6) Uani 1 1 d . . . N5 N 0.8313(2) 0.04661(19) 0.5960(2) 0.0245(5) Uani 1 1 d . . . N6 N 0.8315(3) -0.1304(2) 0.5473(2) 0.0320(6) Uani 1 1 d . . . N7 N 0.5687(2) 0.13293(19) 0.97927(19) 0.0251(5) Uani 1 1 d . . . N8 N 0.4901(3) 0.1837(2) 1.1705(2) 0.0389(7) Uani 1 1 d . . . O1W O 0.5161(3) 0.5535(3) 0.6369(2) 0.0545(7) Uani 1 1 d D . . H1C H 0.451(3) 0.532(4) 0.633(4) 0.082 Uiso 1 1 d D . . H1D H 0.576(3) 0.544(4) 0.565(2) 0.082 Uiso 1 1 d D . . O2W O 0.9918(5) 1.0765(4) -0.1357(3) 0.0940(12) Uani 1 1 d D . . H2D H 0.969(7) 1.118(5) -0.072(4) 0.141 Uiso 1 1 d D . . H2C H 0.964(7) 1.014(4) -0.112(6) 0.141 Uiso 1 1 d D . . O3W O 0.7780(4) 0.1336(6) 0.2234(4) 0.1193(17) Uani 1 1 d D . . H3C H 0.798(8) 0.188(5) 0.172(7) 0.179 Uiso 1 1 d D . . H3D H 0.842(6) 0.076(5) 0.208(8) 0.179 Uiso 1 1 d D . . O4W O 0.8655(4) 0.3074(3) 0.3858(5) 0.135(2) Uani 1 1 d D . . H4D H 0.827(9) 0.377(3) 0.395(8) 0.203 Uiso 1 1 d D . . H4C H 0.901(10) 0.286(7) 0.312(3) 0.203 Uiso 1 1 d 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 0.0685(2) 0.02450(13) 0.03646(15) 0.00250(10) -0.00519(13) -0.00857(12) Ag2 0.0587(2) 0.0757(2) 0.02646(13) -0.00495(13) -0.02565(13) -0.00287(15) C1 0.0402(18) 0.0242(14) 0.0374(15) 0.0031(12) -0.0192(14) -0.0098(13) C2 0.0332(17) 0.0335(15) 0.0307(14) -0.0022(12) -0.0127(13) -0.0101(13) C3 0.0358(17) 0.0375(16) 0.0287(14) -0.0010(13) -0.0100(13) -0.0160(13) C4 0.0385(17) 0.0250(13) 0.0232(13) 0.0020(11) -0.0153(12) -0.0129(12) C5 0.0299(15) 0.0202(12) 0.0209(12) 0.0001(10) -0.0125(11) -0.0068(11) C6 0.0395(17) 0.0235(13) 0.0280(14) 0.0017(11) -0.0184(13) -0.0087(12) C7 0.0357(17) 0.0413(16) 0.0230(13) 0.0063(12) -0.0168(13) -0.0053(14) C8 0.0372(17) 0.0324(15) 0.0264(14) 0.0018(12) -0.0143(13) -0.0103(13) C9 0.0347(17) 0.0408(16) 0.0356(16) -0.0065(13) -0.0182(14) -0.0082(14) C10 0.0343(16) 0.0263(13) 0.0253(13) -0.0021(11) -0.0093(12) -0.0123(12) C11 0.0353(16) 0.0263(13) 0.0201(12) 0.0024(11) -0.0100(12) -0.0046(12) C12 0.0325(16) 0.0323(15) 0.0249(13) -0.0026(12) -0.0137(13) -0.0022(12) C13 0.0411(18) 0.0243(13) 0.0234(13) 0.0021(11) -0.0129(13) -0.0035(12) C14 0.0276(15) 0.0238(13) 0.0223(12) -0.0004(11) -0.0080(11) -0.0060(11) C15 0.0282(16) 0.0468(17) 0.0241(13) -0.0011(13) -0.0127(12) -0.0091(13) C16 0.0330(17) 0.0472(18) 0.0243(14) -0.0017(13) -0.0101(13) -0.0044(14) C17 0.0361(18) 0.0462(18) 0.0255(14) 0.0050(13) -0.0169(13) -0.0084(14) C18 0.0271(16) 0.0375(16) 0.0367(16) -0.0027(14) -0.0127(13) 0.0023(13) C19 0.0323(17) 0.0405(17) 0.0340(16) -0.0057(14) -0.0126(14) -0.0008(14) C20 0.0309(17) 0.0414(17) 0.0319(15) -0.0045(13) -0.0141(13) 0.0009(14) C21 0.0352(18) 0.056(2) 0.0366(17) -0.0003(15) -0.0202(15) 0.0008(16) C22 0.055(2) 0.065(2) 0.044(2) 0.0081(19) -0.0296(18) -0.0080(19) C23 0.069(3) 0.065(2) 0.0373(18) -0.0060(18) -0.0267(19) -0.006(2) C24 0.104(4) 0.061(3) 0.051(2) -0.020(2) -0.034(2) -0.017(2) C25 0.070(3) 0.047(2) 0.048(2) -0.0059(17) -0.026(2) -0.0145(19) O1 0.0508(15) 0.0475(13) 0.0433(13) 0.0045(11) -0.0141(12) -0.0134(12) O2 0.0422(13) 0.0475(13) 0.0375(12) -0.0039(10) -0.0178(11) -0.0068(11) O3 0.086(2) 0.0663(18) 0.0601(17) 0.0147(15) -0.0366(17) -0.0237(16) O4 0.114(3) 0.095(2) 0.0393(15) 0.0188(15) -0.0341(17) -0.013(2) N1 0.0448(16) 0.0283(12) 0.0326(13) 0.0024(10) -0.0163(12) -0.0139(11) N2 0.0328(14) 0.0237(11) 0.0282(12) -0.0005(10) -0.0125(11) -0.0103(10) N3 0.0340(14) 0.0291(12) 0.0207(11) 0.0006(9) -0.0144(10) -0.0055(10) N4 0.0345(15) 0.0460(15) 0.0249(12) -0.0040(11) -0.0161(11) -0.0004(12) N5 0.0291(13) 0.0214(11) 0.0213(10) -0.0015(9) -0.0083(9) -0.0052(9) N6 0.0420(15) 0.0240(12) 0.0288(12) 0.0005(10) -0.0129(11) -0.0075(11) N7 0.0308(13) 0.0284(12) 0.0195(10) 0.0041(9) -0.0126(10) -0.0093(10) N8 0.0426(16) 0.0547(17) 0.0215(12) 0.0010(12) -0.0158(12) -0.0086(13) O1W 0.0575(18) 0.0638(17) 0.0456(14) 0.0063(13) -0.0229(13) -0.0173(14) O2W 0.142(4) 0.096(3) 0.085(2) 0.038(2) -0.077(3) -0.055(3) O3W 0.071(3) 0.198(5) 0.081(3) -0.005(3) -0.034(2) -0.006(3) O4W 0.087(3) 0.061(2) 0.173(4) 0.059(3) 0.015(3) -0.001(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 2.157(3) . ? Ag1 N6 2.163(3) 1_565 ? Ag1 O2 2.422(2) . ? Ag1 Ag2 3.1542(14) 2_666 ? Ag2 N4 2.119(3) . ? Ag2 N8 2.127(3) 1_554 ? Ag2 Ag1 3.1542(14) 2_666 ? C1 N1 1.309(4) . ? C1 N2 1.355(4) . ? C1 H1 0.9300 . ? C2 C3 1.357(4) . ? C2 N2 1.367(4) . ? C2 H2 0.9300 . ? C3 N1 1.372(4) . ? C3 H3 0.9300 . ? C4 N2 1.464(4) . ? C4 C5 1.551(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C10 1.543(4) . ? C5 C6 1.545(4) . ? C5 C14 1.551(4) . ? C6 N3 1.455(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N4 1.312(4) . ? C7 N3 1.351(4) . ? C7 H7 0.9300 . ? C8 C9 1.359(4) . ? C8 N3 1.368(4) . ? C8 H8 0.9300 . ? C9 N4 1.380(4) . ? C9 H9 0.9300 . ? C10 N5 1.467(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.354(4) . ? C11 N5 1.371(4) . ? C11 H11 0.9300 . ? C12 N6 1.379(4) . ? C12 H12 0.9300 . ? C13 N6 1.321(4) . ? C13 N5 1.349(4) . ? C13 H13 0.9300 . ? C14 N7 1.463(3) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.349(4) . ? C15 N7 1.371(4) . ? C15 H15 0.9300 . ? C16 N8 1.381(4) . ? C16 H16 0.9300 . ? C17 N8 1.315(4) . ? C17 N7 1.343(4) . ? C17 H17 0.9300 . ? C18 O2 1.247(4) . ? C18 O1 1.271(4) . ? C18 C19 1.513(4) . ? C19 C20 1.389(5) . ? C19 C25 1.393(5) . ? C20 C21 1.391(4) . ? C20 H20 0.9300 . ? C21 C23 1.393(5) . ? C21 C22 1.512(6) . ? C22 O4 1.236(5) . ? C22 O3 1.265(5) . ? C23 C24 1.363(6) . ? C23 H23 0.9300 . ? C24 C25 1.395(6) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? N6 Ag1 2.163(3) 1_545 ? N8 Ag2 2.127(3) 1_556 ? O1W H1C 0.852(19) . ? O1W H1D 0.855(19) . ? O2W H2D 0.86(2) . ? O2W H2C 0.85(2) . ? O3W H3C 0.86(2) . ? O3W H3D 0.85(2) . ? O4W H4D 0.83(2) . ? O4W H4C 0.85(2) . ? 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 N6 142.88(10) . 1_565 ? N1 Ag1 O2 119.76(9) . . ? N6 Ag1 O2 96.96(9) 1_565 . ? N1 Ag1 Ag2 107.08(7) . 2_666 ? N6 Ag1 Ag2 84.10(7) 1_565 2_666 ? O2 Ag1 Ag2 78.46(6) . 2_666 ? N4 Ag2 N8 166.80(10) . 1_554 ? N4 Ag2 Ag1 98.58(7) . 2_666 ? N8 Ag2 Ag1 88.07(8) 1_554 2_666 ? N1 C1 N2 111.1(3) . . ? N1 C1 H1 124.5 . . ? N2 C1 H1 124.5 . . ? C3 C2 N2 106.2(3) . . ? C3 C2 H2 126.9 . . ? N2 C2 H2 126.9 . . ? C2 C3 N1 109.5(3) . . ? C2 C3 H3 125.2 . . ? N1 C3 H3 125.2 . . ? N2 C4 C5 114.3(2) . . ? N2 C4 H4A 108.7 . . ? C5 C4 H4A 108.7 . . ? N2 C4 H4B 108.7 . . ? C5 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? C10 C5 C6 114.0(2) . . ? C10 C5 C14 108.5(2) . . ? C6 C5 C14 113.6(2) . . ? C10 C5 C4 107.5(2) . . ? C6 C5 C4 106.1(2) . . ? C14 C5 C4 106.6(2) . . ? N3 C6 C5 117.7(2) . . ? N3 C6 H6A 107.9 . . ? C5 C6 H6A 107.9 . . ? N3 C6 H6B 107.9 . . ? C5 C6 H6B 107.9 . . ? H6A C6 H6B 107.2 . . ? N4 C7 N3 111.3(3) . . ? N4 C7 H7 124.4 . . ? N3 C7 H7 124.4 . . ? C9 C8 N3 106.6(3) . . ? C9 C8 H8 126.7 . . ? N3 C8 H8 126.7 . . ? C8 C9 N4 109.0(3) . . ? C8 C9 H9 125.5 . . ? N4 C9 H9 125.5 . . ? N5 C10 C5 116.1(2) . . ? N5 C10 H10A 108.3 . . ? C5 C10 H10A 108.3 . . ? N5 C10 H10B 108.3 . . ? C5 C10 H10B 108.3 . . ? H10A C10 H10B 107.4 . . ? C12 C11 N5 106.9(2) . . ? C12 C11 H11 126.5 . . ? N5 C11 H11 126.5 . . ? C11 C12 N6 109.0(3) . . ? C11 C12 H12 125.5 . . ? N6 C12 H12 125.5 . . ? N6 C13 N5 111.2(2) . . ? N6 C13 H13 124.4 . . ? N5 C13 H13 124.4 . . ? N7 C14 C5 114.0(2) . . ? N7 C14 H14A 108.7 . . ? C5 C14 H14A 108.7 . . ? N7 C14 H14B 108.7 . . ? C5 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? C16 C15 N7 107.1(3) . . ? C16 C15 H15 126.4 . . ? N7 C15 H15 126.4 . . ? C15 C16 N8 108.7(3) . . ? C15 C16 H16 125.7 . . ? N8 C16 H16 125.7 . . ? N8 C17 N7 111.3(3) . . ? N8 C17 H17 124.3 . . ? N7 C17 H17 124.3 . . ? O2 C18 O1 125.5(3) . . ? O2 C18 C19 117.5(3) . . ? O1 C18 C19 117.0(3) . . ? C20 C19 C25 118.9(3) . . ? C20 C19 C18 120.6(3) . . ? C25 C19 C18 120.5(3) . . ? C19 C20 C21 121.8(3) . . ? C19 C20 H20 119.1 . . ? C21 C20 H20 119.1 . . ? C20 C21 C23 118.1(4) . . ? C20 C21 C22 121.7(3) . . ? C23 C21 C22 120.2(3) . . ? O4 C22 O3 125.0(4) . . ? O4 C22 C21 118.1(4) . . ? O3 C22 C21 116.8(3) . . ? C24 C23 C21 120.8(3) . . ? C24 C23 H23 119.6 . . ? C21 C23 H23 119.6 . . ? C23 C24 C25 121.0(4) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C19 C25 C24 119.4(4) . . ? C19 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? C18 O2 Ag1 131.0(2) . . ? C1 N1 C3 106.1(3) . . ? C1 N1 Ag1 130.3(2) . . ? C3 N1 Ag1 123.2(2) . . ? C1 N2 C2 107.1(3) . . ? C1 N2 C4 127.6(3) . . ? C2 N2 C4 125.3(2) . . ? C7 N3 C8 107.0(3) . . ? C7 N3 C6 123.2(3) . . ? C8 N3 C6 129.4(2) . . ? C7 N4 C9 106.1(2) . . ? C7 N4 Ag2 124.6(2) . . ? C9 N4 Ag2 129.1(2) . . ? C13 N5 C11 106.9(2) . . ? C13 N5 C10 127.2(2) . . ? C11 N5 C10 125.9(2) . . ? C13 N6 C12 106.0(2) . . ? C13 N6 Ag1 127.69(19) . 1_545 ? C12 N6 Ag1 125.9(2) . 1_545 ? C17 N7 C15 106.7(2) . . ? C17 N7 C14 124.8(2) . . ? C15 N7 C14 128.4(2) . . ? C17 N8 C16 106.1(3) . . ? C17 N8 Ag2 122.9(2) . 1_556 ? C16 N8 Ag2 130.9(2) . 1_556 ? H1C O1W H1D 105(4) . . ? H2D O2W H2C 106(5) . . ? H3C O3W H3D 111(5) . . ? H4D O4W H4C 112(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C2 C3 N1 -0.3(3) . . . . ? N2 C4 C5 C10 53.6(3) . . . . ? N2 C4 C5 C6 -68.8(3) . . . . ? N2 C4 C5 C14 169.8(2) . . . . ? C10 C5 C6 N3 59.4(3) . . . . ? C14 C5 C6 N3 -65.6(3) . . . . ? C4 C5 C6 N3 177.6(2) . . . . ? N3 C8 C9 N4 0.0(3) . . . . ? C6 C5 C10 N5 -71.5(3) . . . . ? C14 C5 C10 N5 56.1(3) . . . . ? C4 C5 C10 N5 171.1(2) . . . . ? N5 C11 C12 N6 -0.5(3) . . . . ? C10 C5 C14 N7 164.1(2) . . . . ? C6 C5 C14 N7 -68.1(3) . . . . ? C4 C5 C14 N7 48.5(3) . . . . ? N7 C15 C16 N8 0.5(4) . . . . ? O2 C18 C19 C20 -13.6(4) . . . . ? O1 C18 C19 C20 167.7(3) . . . . ? O2 C18 C19 C25 164.3(3) . . . . ? O1 C18 C19 C25 -14.5(5) . . . . ? C25 C19 C20 C21 0.4(5) . . . . ? C18 C19 C20 C21 178.2(3) . . . . ? C19 C20 C21 C23 -1.7(5) . . . . ? C19 C20 C21 C22 177.8(3) . . . . ? C20 C21 C22 O4 174.7(4) . . . . ? C23 C21 C22 O4 -5.8(6) . . . . ? C20 C21 C22 O3 -8.4(5) . . . . ? C23 C21 C22 O3 171.1(4) . . . . ? C20 C21 C23 C24 1.5(6) . . . . ? C22 C21 C23 C24 -178.0(4) . . . . ? C21 C23 C24 C25 0.1(7) . . . . ? C20 C19 C25 C24 1.2(6) . . . . ? C18 C19 C25 C24 -176.7(4) . . . . ? C23 C24 C25 C19 -1.4(7) . . . . ? O1 C18 O2 Ag1 24.3(5) . . . . ? C19 C18 O2 Ag1 -154.3(2) . . . . ? N1 Ag1 O2 C18 9.5(3) . . . . ? N6 Ag1 O2 C18 -176.2(3) 1_565 . . . ? Ag2 Ag1 O2 C18 -93.7(3) 2_666 . . . ? N2 C1 N1 C3 -1.0(3) . . . . ? N2 C1 N1 Ag1 172.45(18) . . . . ? C2 C3 N1 C1 0.8(3) . . . . ? C2 C3 N1 Ag1 -173.22(19) . . . . ? N6 Ag1 N1 C1 117.4(3) 1_565 . . . ? O2 Ag1 N1 C1 -72.0(3) . . . . ? Ag2 Ag1 N1 C1 14.3(3) 2_666 . . . ? N6 Ag1 N1 C3 -70.2(3) 1_565 . . . ? O2 Ag1 N1 C3 100.4(2) . . . . ? Ag2 Ag1 N1 C3 -173.3(2) 2_666 . . . ? N1 C1 N2 C2 0.8(3) . . . . ? N1 C1 N2 C4 -179.8(2) . . . . ? C3 C2 N2 C1 -0.3(3) . . . . ? C3 C2 N2 C4 -179.7(2) . . . . ? C5 C4 N2 C1 82.4(3) . . . . ? C5 C4 N2 C2 -98.3(3) . . . . ? N4 C7 N3 C8 -0.9(3) . . . . ? N4 C7 N3 C6 -174.3(2) . . . . ? C9 C8 N3 C7 0.5(3) . . . . ? C9 C8 N3 C6 173.3(3) . . . . ? C5 C6 N3 C7 -118.0(3) . . . . ? C5 C6 N3 C8 70.2(4) . . . . ? N3 C7 N4 C9 0.9(3) . . . . ? N3 C7 N4 Ag2 177.51(18) . . . . ? C8 C9 N4 C7 -0.6(3) . . . . ? C8 C9 N4 Ag2 -177.0(2) . . . . ? N8 Ag2 N4 C7 131.1(5) 1_554 . . . ? Ag1 Ag2 N4 C7 -109.2(2) 2_666 . . . ? N8 Ag2 N4 C9 -53.1(6) 1_554 . . . ? Ag1 Ag2 N4 C9 66.5(2) 2_666 . . . ? N6 C13 N5 C11 -1.7(4) . . . . ? N6 C13 N5 C10 -179.6(3) . . . . ? C12 C11 N5 C13 1.3(3) . . . . ? C12 C11 N5 C10 179.3(3) . . . . ? C5 C10 N5 C13 -78.0(4) . . . . ? C5 C10 N5 C11 104.4(3) . . . . ? N5 C13 N6 C12 1.4(4) . . . . ? N5 C13 N6 Ag1 -171.24(19) . . . 1_545 ? C11 C12 N6 C13 -0.5(4) . . . . ? C11 C12 N6 Ag1 172.3(2) . . . 1_545 ? N8 C17 N7 C15 0.4(4) . . . . ? N8 C17 N7 C14 176.1(3) . . . . ? C16 C15 N7 C17 -0.6(3) . . . . ? C16 C15 N7 C14 -176.0(3) . . . . ? C5 C14 N7 C17 -99.8(3) . . . . ? C5 C14 N7 C15 74.9(4) . . . . ? N7 C17 N8 C16 -0.1(4) . . . . ? N7 C17 N8 Ag2 177.6(2) . . . 1_556 ? C15 C16 N8 C17 -0.3(4) . . . . ? C15 C16 N8 Ag2 -177.7(2) . . . 1_556 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1C O1 0.852(19) 2.07(2) 2.914(4) 173(4) 2_666 O1W H1D O1 0.855(19) 1.93(2) 2.783(4) 173(5) . O2W H2D O3 0.86(2) 2.38(7) 2.846(5) 114(6) 2_775 O2W H2C O3 0.85(2) 1.97(3) 2.785(5) 160(6) . O4W H4D O1 0.83(2) 2.01(4) 2.803(4) 159(10) . O4W H4C O4 0.85(2) 2.07(6) 2.817(6) 146(9) 2_765 O3W H3D O2W 0.85(2) 2.23(3) 3.070(7) 170(9) 2_765 _diffrn_measured_fraction_theta_max 0.836 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.140 _refine_diff_density_min -1.185 _refine_diff_density_rms 0.084 #===END data_compound-5 _database_code_depnum_ccdc_archive 'CCDC 800210' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H20 Ag2 N8, C8 H4 O4, 8(H2 O)' _chemical_formula_sum 'C25 H39 Ag2 N8 O11.50' _chemical_formula_weight 851.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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/n' _symmetry_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 11.406(5) _cell_length_b 17.637(5) _cell_length_c 16.979(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 106.836(5) _cell_angle_gamma 90.000(5) _cell_volume 3269(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7614 _cell_measurement_theta_min 4.3 _cell_measurement_theta_max 29.3 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.730 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1724 _exptl_absorpt_coefficient_mu 1.268 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.768 _exptl_absorpt_correction_T_max 0.823 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15290 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0617 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.35 _diffrn_reflns_theta_max 29.31 _reflns_number_total 7614 _reflns_number_gt 4743 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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. H atoms of water molecule were refined isotropically with distance restraints of O---H = 0.85+-0.02 \%A and H...H = 1.44+-0.02 \%A. For O7w and o7w' atoms, some anisotropic displacement ellipsoids were rather elongated which led us to use the ISOR restraints. ; _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^)+(0.0511P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7614 _refine_ls_number_parameters 478 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0713 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0898 _refine_ls_goodness_of_fit_ref 0.904 _refine_ls_restrained_S_all 0.907 _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 0.30045(3) 0.966870(16) 0.372259(17) 0.04386(10) Uani 1 1 d . . . Ag2 Ag -0.38988(3) 1.048931(18) -0.045341(18) 0.05085(11) Uani 1 1 d . . . C1 C -0.4275(3) 0.7375(2) 0.1221(2) 0.0426(9) Uani 1 1 d . . . H1 H -0.4198 0.6850 0.1226 0.051 Uiso 1 1 calc R . . C2 C -0.5246(3) 0.7783(2) 0.0795(2) 0.0448(9) Uani 1 1 d . . . H2 H -0.5967 0.7582 0.0451 0.054 Uiso 1 1 calc R . . C3 C -0.3914(3) 0.85802(19) 0.1466(2) 0.0332(8) Uani 1 1 d . . . H3 H -0.3526 0.9029 0.1684 0.040 Uiso 1 1 calc R . . C4 C -0.2185(3) 0.7737(2) 0.21742(18) 0.0321(8) Uani 1 1 d . . . H4A H -0.2235 0.7339 0.2557 0.038 Uiso 1 1 calc R . . H4B H -0.1891 0.8190 0.2495 0.038 Uiso 1 1 calc R . . C5 C -0.1223(3) 0.75006(17) 0.17410(17) 0.0258(7) Uani 1 1 d . . . C6 C -0.0047(3) 0.72624(17) 0.24136(18) 0.0290(7) Uani 1 1 d . . . H6A H -0.0234 0.6823 0.2699 0.035 Uiso 1 1 calc R . . H6B H 0.0562 0.7109 0.2148 0.035 Uiso 1 1 calc R . . C7 C 0.0223(3) 0.79990(19) 0.37488(18) 0.0306(7) Uani 1 1 d . . . H7 H -0.0360 0.7758 0.3946 0.037 Uiso 1 1 calc R . . C8 C 0.0979(3) 0.85661(19) 0.41136(19) 0.0329(8) Uani 1 1 d . . . H8 H 0.1002 0.8785 0.4616 0.040 Uiso 1 1 calc R . . C9 C 0.1390(3) 0.8322(2) 0.29870(19) 0.0327(8) Uani 1 1 d . . . H9 H 0.1746 0.8330 0.2559 0.039 Uiso 1 1 calc R . . C10 C -0.0854(3) 0.81436(18) 0.12404(18) 0.0273(7) Uani 1 1 d . . . H10A H -0.0433 0.8530 0.1625 0.033 Uiso 1 1 calc R . . H10B H -0.0268 0.7938 0.0982 0.033 Uiso 1 1 calc R . . C11 C -0.2501(4) 0.8226(2) -0.0144(2) 0.0452(10) Uani 1 1 d . . . H11 H -0.2459 0.7737 -0.0340 0.054 Uiso 1 1 calc R . . C12 C -0.3239(4) 0.8795(2) -0.0535(2) 0.0476(10) Uani 1 1 d . . . H12 H -0.3808 0.8757 -0.1052 0.057 Uiso 1 1 calc R . . C13 C -0.2171(3) 0.92412(19) 0.0612(2) 0.0331(8) Uani 1 1 d . . . H13 H -0.1841 0.9571 0.1047 0.040 Uiso 1 1 calc R . . C14 C -0.1671(3) 0.67716(18) 0.12321(19) 0.0291(7) Uani 1 1 d . . . H14A H -0.1981 0.6423 0.1566 0.035 Uiso 1 1 calc R . . H14B H -0.2349 0.6905 0.0758 0.035 Uiso 1 1 calc R . . C15 C -0.0016(3) 0.58185(19) 0.1335(2) 0.0343(8) Uani 1 1 d . . . H15 H -0.0029 0.5623 0.1841 0.041 Uiso 1 1 calc R . . C16 C -0.0445(3) 0.6502(2) 0.02187(19) 0.0349(8) Uani 1 1 d . . . H16 H -0.0789 0.6856 -0.0188 0.042 Uiso 1 1 calc R . . C17 C 0.0443(3) 0.6005(2) 0.02241(19) 0.0355(8) Uani 1 1 d . . . H17 H 0.0820 0.5957 -0.0191 0.043 Uiso 1 1 calc R . . C18 C 0.1860(4) 0.9644(2) 0.1541(2) 0.0399(9) Uani 1 1 d . . . C19 C 0.0891(3) 0.9828(2) 0.07395(18) 0.0309(7) Uani 1 1 d . . . C20 C 0.0296(3) 1.0521(2) 0.06278(19) 0.0350(8) Uani 1 1 d . . . H20 H 0.0495 1.0877 0.1050 0.042 Uiso 1 1 calc R . . C21 C 0.0589(3) 0.9305(2) 0.00983(19) 0.0336(8) Uani 1 1 d . . . H21 H 0.0983 0.8838 0.0158 0.040 Uiso 1 1 calc R . . C22 C 0.7849(4) 0.9618(2) 0.3641(2) 0.0450(9) Uani 1 1 d . . . C23 C 0.8959(3) 0.98280(19) 0.4346(2) 0.0339(8) Uani 1 1 d . . . C24 C 0.9097(3) 0.95335(19) 0.5132(2) 0.0352(8) Uani 1 1 d . . . H24 H 0.8495 0.9220 0.5226 0.042 Uiso 1 1 calc R . . C25 C 0.9875(4) 1.0293(2) 0.4231(2) 0.0375(8) Uani 1 1 d . . . H25 H 0.9794 1.0493 0.3711 0.045 Uiso 1 1 calc R . . O1 O 0.2531(2) 0.90791(15) 0.15558(14) 0.0465(7) Uani 1 1 d . . . O2 O 0.1921(4) 1.00624(17) 0.21456(15) 0.0763(11) Uani 1 1 d . . . O3 O 0.7112(3) 0.91468(18) 0.37512(16) 0.0608(8) Uani 1 1 d . . . O4 O 0.7740(3) 0.9949(2) 0.29712(18) 0.0882(13) Uani 1 1 d . . . O6W' O 0.2178(10) 0.1603(4) 0.2425(5) 0.074(3) Uani 0.40 1 d P . . O6W O 0.1309(6) 0.1396(3) 0.2681(3) 0.0697(15) Uani 0.60 1 d P . . O7W O 0.9167(6) 0.0384(4) 0.2091(3) 0.0917(16) Uani 0.70 1 d PU . . O7W' O 0.8876(13) 0.0965(8) 0.2201(7) 0.087(4) Uani 0.30 1 d PU . . N1 N -0.5016(3) 0.85400(17) 0.09428(17) 0.0382(7) Uani 1 1 d . . . N2 N -0.3421(2) 0.78875(15) 0.16458(16) 0.0301(6) Uani 1 1 d . . . N3 N 0.0491(2) 0.78500(15) 0.30254(14) 0.0268(6) Uani 1 1 d . . . N4 N 0.1708(3) 0.87712(16) 0.36315(16) 0.0344(7) Uani 1 1 d . . . N5 N -0.1830(3) 0.85159(15) 0.05987(15) 0.0306(6) Uani 1 1 d . . . N6 N -0.3025(3) 0.94330(17) -0.00607(17) 0.0389(7) Uani 1 1 d . . . N7 N -0.0747(2) 0.63802(15) 0.09449(15) 0.0291(6) Uani 1 1 d . . . N8 N 0.0717(3) 0.55778(15) 0.09237(16) 0.0336(7) Uani 1 1 d . . . O1W O 0.4515(3) 0.89182(18) 0.29635(16) 0.0527(7) Uani 1 1 d D . . H1D H 0.402(3) 0.903(3) 0.2499(17) 0.079 Uiso 1 1 d D . . H1C H 0.523(2) 0.907(3) 0.300(3) 0.079 Uiso 1 1 d D . . O2W O 0.6978(3) 0.7710(2) 0.44281(18) 0.0675(9) Uani 1 1 d D . . H2C H 0.627(3) 0.757(3) 0.413(3) 0.101 Uiso 1 1 d D . . H2D H 0.723(5) 0.807(2) 0.416(3) 0.101 Uiso 1 1 d D . . O3W O 0.4513(4) 0.75051(19) 0.36267(18) 0.0725(10) Uani 1 1 d D . . H3C H 0.442(6) 0.7953(14) 0.344(3) 0.109 Uiso 1 1 d D . . H3D H 0.458(6) 0.722(3) 0.324(3) 0.109 Uiso 1 1 d D . . O4W O 0.5720(3) 1.0492(2) 0.1836(2) 0.0737(10) Uani 1 1 d D . . H4C H 0.628(4) 1.033(3) 0.226(2) 0.111 Uiso 1 1 d D . . H4D H 0.596(5) 1.058(4) 0.142(2) 0.111 Uiso 1 1 d D . . O5W O 0.7168(5) 0.1380(3) 0.1089(3) 0.0487(14) Uani 0.50 1 d PD . . H5D H 0.769(6) 0.144(5) 0.150(3) 0.073 Uiso 0.50 1 d PD . . H5C H 0.750(8) 0.105(4) 0.092(5) 0.073 Uiso 0.50 1 d PD . . O8W O 0.2955(3) 0.25101(17) 0.37899(17) 0.0557(8) Uani 1 1 d D . . H8C H 0.293(5) 0.240(3) 0.4282(16) 0.084 Uiso 1 1 d D . . H8D H 0.268(5) 0.2957(15) 0.369(3) 0.084 Uiso 1 1 d 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 0.04005(18) 0.03388(16) 0.05402(18) -0.00240(12) 0.00788(13) -0.01414(13) Ag2 0.04385(19) 0.0482(2) 0.0609(2) 0.02271(14) 0.01591(15) 0.02318(15) C1 0.0282(19) 0.027(2) 0.072(2) -0.0049(17) 0.0139(18) -0.0035(16) C2 0.026(2) 0.046(2) 0.058(2) -0.0083(18) 0.0056(17) -0.0003(18) C3 0.0279(19) 0.0254(18) 0.0462(19) 0.0024(14) 0.0106(15) 0.0044(15) C4 0.0260(18) 0.0339(19) 0.0333(17) 0.0012(14) 0.0039(14) 0.0065(15) C5 0.0224(16) 0.0210(16) 0.0288(16) 0.0001(12) -0.0006(13) 0.0010(13) C6 0.0259(17) 0.0203(16) 0.0337(16) -0.0008(13) -0.0026(13) 0.0019(14) C7 0.0284(18) 0.0344(19) 0.0307(17) 0.0037(14) 0.0110(14) -0.0014(15) C8 0.0328(19) 0.0337(19) 0.0294(17) -0.0015(14) 0.0044(14) 0.0050(16) C9 0.0289(19) 0.039(2) 0.0289(17) -0.0025(14) 0.0067(14) -0.0072(16) C10 0.0223(16) 0.0229(16) 0.0318(16) 0.0027(12) 0.0000(13) -0.0006(14) C11 0.050(2) 0.0295(19) 0.044(2) -0.0012(16) -0.0068(18) 0.0009(18) C12 0.043(2) 0.038(2) 0.047(2) 0.0061(17) -0.0115(17) -0.0009(19) C13 0.0327(19) 0.0262(18) 0.0398(19) 0.0057(14) 0.0096(15) 0.0036(15) C14 0.0242(17) 0.0242(17) 0.0350(17) -0.0022(13) 0.0024(14) -0.0009(14) C15 0.041(2) 0.0238(18) 0.0363(18) 0.0020(14) 0.0081(16) 0.0058(16) C16 0.039(2) 0.034(2) 0.0287(17) 0.0032(14) 0.0058(15) 0.0029(17) C17 0.040(2) 0.0323(19) 0.0332(18) -0.0044(14) 0.0092(15) 0.0051(17) C18 0.048(2) 0.038(2) 0.0325(18) 0.0037(16) 0.0101(16) -0.0032(19) C19 0.0319(19) 0.0328(19) 0.0300(17) 0.0023(14) 0.0121(14) -0.0032(16) C20 0.040(2) 0.0316(19) 0.0344(18) -0.0040(14) 0.0116(15) -0.0030(16) C21 0.037(2) 0.0280(18) 0.0371(18) 0.0037(14) 0.0129(16) 0.0033(16) C22 0.035(2) 0.049(2) 0.045(2) 0.0030(18) 0.0013(17) 0.002(2) C23 0.0299(19) 0.0262(18) 0.0410(19) -0.0021(14) 0.0032(15) 0.0055(15) C24 0.035(2) 0.032(2) 0.0391(18) 0.0024(14) 0.0096(15) -0.0014(16) C25 0.045(2) 0.033(2) 0.0315(17) 0.0033(14) 0.0067(16) 0.0010(17) O1 0.0444(16) 0.0481(17) 0.0421(14) 0.0024(12) 0.0048(12) 0.0092(14) O2 0.127(3) 0.0498(19) 0.0353(15) -0.0052(13) -0.0036(16) 0.030(2) O3 0.0451(18) 0.066(2) 0.0595(17) 0.0061(14) -0.0039(14) -0.0209(16) O4 0.061(2) 0.134(3) 0.0512(17) 0.038(2) -0.0132(15) -0.036(2) O6W' 0.093(7) 0.045(5) 0.063(5) 0.004(4) -0.009(5) 0.006(5) O6W 0.068(4) 0.062(4) 0.070(3) -0.005(3) 0.006(3) 0.013(3) O7W 0.0919(19) 0.0956(19) 0.0885(18) -0.0005(10) 0.0279(10) -0.0018(10) O7W' 0.087(4) 0.087(4) 0.087(4) 0.0017(10) 0.0248(14) -0.0007(10) N1 0.0282(16) 0.0389(18) 0.0485(17) 0.0080(13) 0.0125(13) 0.0128(14) N2 0.0236(15) 0.0244(15) 0.0411(15) 0.0009(11) 0.0074(12) 0.0040(12) N3 0.0213(14) 0.0264(14) 0.0294(13) 0.0017(11) 0.0021(11) -0.0004(12) N4 0.0302(16) 0.0313(16) 0.0367(15) -0.0004(12) 0.0020(12) -0.0066(13) N5 0.0285(15) 0.0225(14) 0.0356(15) 0.0067(11) 0.0009(12) 0.0034(12) N6 0.0308(16) 0.0329(17) 0.0495(17) 0.0162(13) 0.0065(14) 0.0075(14) N7 0.0273(15) 0.0232(14) 0.0341(14) -0.0011(11) 0.0046(12) 0.0022(12) N8 0.0405(18) 0.0247(15) 0.0337(15) -0.0003(12) 0.0076(13) 0.0095(13) O1W 0.0470(18) 0.063(2) 0.0440(15) 0.0045(13) 0.0060(13) -0.0040(16) O2W 0.065(2) 0.058(2) 0.066(2) 0.0019(15) -0.0006(16) 0.0151(18) O3W 0.086(3) 0.052(2) 0.066(2) 0.0049(15) 0.0014(18) -0.007(2) O4W 0.058(2) 0.089(3) 0.071(2) 0.0076(19) 0.0147(17) 0.017(2) O5W 0.063(4) 0.042(3) 0.045(3) 0.003(2) 0.023(3) -0.030(3) O8W 0.058(2) 0.0542(19) 0.0568(16) 0.0052(14) 0.0195(15) 0.0092(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 N8 2.133(3) 2 ? Ag1 N4 2.141(3) . ? Ag2 N6 2.127(3) . ? Ag2 N1 2.135(3) 3_475 ? C1 C2 1.343(5) . ? C1 N2 1.371(4) . ? C1 H1 0.9300 . ? C2 N1 1.370(5) . ? C2 H2 0.9300 . ? C3 N1 1.314(4) . ? C3 N2 1.342(4) . ? C3 H3 0.9300 . ? C4 N2 1.459(4) . ? C4 C5 1.546(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C10 1.547(4) . ? C5 C6 1.547(4) . ? C5 C14 1.551(4) . ? C6 N3 1.470(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.348(5) . ? C7 N3 1.374(4) . ? C7 H7 0.9300 . ? C8 N4 1.374(4) . ? C8 H8 0.9300 . ? C9 N4 1.315(4) . ? C9 N3 1.337(4) . ? C9 H9 0.9300 . ? C10 N5 1.468(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.355(5) . ? C11 N5 1.371(4) . ? C11 H11 0.9300 . ? C12 N6 1.364(5) . ? C12 H12 0.9300 . ? C13 N6 1.313(4) . ? C13 N5 1.339(4) . ? C13 H13 0.9300 . ? C14 N7 1.457(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N8 1.306(4) . ? C15 N7 1.340(4) . ? C15 H15 0.9300 . ? C16 C17 1.337(5) . ? C16 N7 1.390(4) . ? C16 H16 0.9300 . ? C17 N8 1.364(4) . ? C17 H17 0.9300 . ? C18 O2 1.249(4) . ? C18 O1 1.252(4) . ? C18 C19 1.519(5) . ? C19 C20 1.384(5) . ? C19 C21 1.393(5) . ? C20 C21 1.383(5) 3_575 ? C20 H20 0.9300 . ? C21 C20 1.383(5) 3_575 ? C21 H21 0.9300 . ? C22 O3 1.234(5) . ? C22 O4 1.253(5) . ? C22 C23 1.514(5) . ? C23 C25 1.386(5) . ? C23 C24 1.398(5) . ? C24 C25 1.380(5) 3_776 ? C24 H24 0.9300 . ? C25 C24 1.380(5) 3_776 ? C25 H25 0.9300 . ? O6W' O6W 1.247(11) . ? O7W O7W' 1.110(14) . ? N1 Ag2 2.135(3) 3_475 ? N8 Ag1 2.133(3) 2_545 ? O1W H1D 0.848(19) . ? O1W H1C 0.843(19) . ? O2W H2C 0.849(19) . ? O2W H2D 0.878(19) . ? O3W H3C 0.848(19) . ? O3W H3D 0.855(19) . ? O4W H4C 0.861(19) . ? O4W H4D 0.847(19) . ? O5W H5D 0.79(2) . ? O5W H5C 0.79(2) . ? O8W H8C 0.865(19) . ? O8W H8D 0.846(19) . ? 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 N8 Ag1 N4 167.85(10) 2 . ? N6 Ag2 N1 172.14(12) . 3_475 ? C2 C1 N2 106.2(3) . . ? C2 C1 H1 126.9 . . ? N2 C1 H1 126.9 . . ? C1 C2 N1 109.8(3) . . ? C1 C2 H2 125.1 . . ? N1 C2 H2 125.1 . . ? N1 C3 N2 111.1(3) . . ? N1 C3 H3 124.5 . . ? N2 C3 H3 124.5 . . ? N2 C4 C5 116.7(3) . . ? N2 C4 H4A 108.1 . . ? C5 C4 H4A 108.1 . . ? N2 C4 H4B 108.1 . . ? C5 C4 H4B 108.1 . . ? H4A C4 H4B 107.3 . . ? C4 C5 C10 114.0(3) . . ? C4 C5 C6 107.8(2) . . ? C10 C5 C6 106.8(3) . . ? C4 C5 C14 108.9(3) . . ? C10 C5 C14 113.6(2) . . ? C6 C5 C14 105.2(2) . . ? N3 C6 C5 115.2(3) . . ? N3 C6 H6A 108.5 . . ? C5 C6 H6A 108.5 . . ? N3 C6 H6B 108.5 . . ? C5 C6 H6B 108.5 . . ? H6A C6 H6B 107.5 . . ? C8 C7 N3 105.9(3) . . ? C8 C7 H7 127.0 . . ? N3 C7 H7 127.0 . . ? C7 C8 N4 109.8(3) . . ? C7 C8 H8 125.1 . . ? N4 C8 H8 125.1 . . ? N4 C9 N3 111.4(3) . . ? N4 C9 H9 124.3 . . ? N3 C9 H9 124.3 . . ? N5 C10 C5 117.9(3) . . ? N5 C10 H10A 107.8 . . ? C5 C10 H10A 107.8 . . ? N5 C10 H10B 107.8 . . ? C5 C10 H10B 107.8 . . ? H10A C10 H10B 107.2 . . ? C12 C11 N5 106.1(3) . . ? C12 C11 H11 127.0 . . ? N5 C11 H11 127.0 . . ? C11 C12 N6 110.0(3) . . ? C11 C12 H12 125.0 . . ? N6 C12 H12 125.0 . . ? N6 C13 N5 112.2(3) . . ? N6 C13 H13 123.9 . . ? N5 C13 H13 123.9 . . ? N7 C14 C5 115.2(3) . . ? N7 C14 H14A 108.5 . . ? C5 C14 H14A 108.5 . . ? N7 C14 H14B 108.5 . . ? C5 C14 H14B 108.5 . . ? H14A C14 H14B 107.5 . . ? N8 C15 N7 112.3(3) . . ? N8 C15 H15 123.9 . . ? N7 C15 H15 123.9 . . ? C17 C16 N7 105.9(3) . . ? C17 C16 H16 127.0 . . ? N7 C16 H16 127.0 . . ? C16 C17 N8 110.5(3) . . ? C16 C17 H17 124.8 . . ? N8 C17 H17 124.8 . . ? O2 C18 O1 124.4(3) . . ? O2 C18 C19 117.6(4) . . ? O1 C18 C19 118.0(3) . . ? C20 C19 C21 118.5(3) . . ? C20 C19 C18 120.8(3) . . ? C21 C19 C18 120.6(3) . . ? C21 C20 C19 121.4(3) 3_575 . ? C21 C20 H20 119.3 3_575 . ? C19 C20 H20 119.3 . . ? C20 C21 C19 120.1(3) 3_575 . ? C20 C21 H21 120.0 3_575 . ? C19 C21 H21 120.0 . . ? O3 C22 O4 124.0(4) . . ? O3 C22 C23 119.7(3) . . ? O4 C22 C23 116.4(4) . . ? C25 C23 C24 118.2(3) . . ? C25 C23 C22 121.7(3) . . ? C24 C23 C22 120.1(3) . . ? C25 C24 C23 120.1(3) 3_776 . ? C25 C24 H24 120.0 3_776 . ? C23 C24 H24 120.0 . . ? C24 C25 C23 121.7(3) 3_776 . ? C24 C25 H25 119.2 3_776 . ? C23 C25 H25 119.2 . . ? C3 N1 C2 105.8(3) . . ? C3 N1 Ag2 123.6(2) . 3_475 ? C2 N1 Ag2 130.6(2) . 3_475 ? C3 N2 C1 107.1(3) . . ? C3 N2 C4 124.8(3) . . ? C1 N2 C4 128.1(3) . . ? C9 N3 C7 107.3(3) . . ? C9 N3 C6 125.0(3) . . ? C7 N3 C6 127.7(3) . . ? C9 N4 C8 105.6(3) . . ? C9 N4 Ag1 121.6(2) . . ? C8 N4 Ag1 132.6(2) . . ? C13 N5 C11 106.5(3) . . ? C13 N5 C10 125.2(3) . . ? C11 N5 C10 128.1(3) . . ? C13 N6 C12 105.2(3) . . ? C13 N6 Ag2 131.3(3) . . ? C12 N6 Ag2 123.3(2) . . ? C15 N7 C16 105.9(3) . . ? C15 N7 C14 126.3(3) . . ? C16 N7 C14 127.8(3) . . ? C15 N8 C17 105.4(3) . . ? C15 N8 Ag1 125.8(2) . 2_545 ? C17 N8 Ag1 128.7(2) . 2_545 ? H1D O1W H1C 111(4) . . ? H2C O2W H2D 107(4) . . ? H3C O3W H3D 107(4) . . ? H4C O4W H4D 114(5) . . ? H5D O5W H5C 96(5) . . ? H8C O8W H8D 107(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C1 C2 N1 0.2(4) . . . . ? N2 C4 C5 C10 69.4(4) . . . . ? N2 C4 C5 C6 -172.1(3) . . . . ? N2 C4 C5 C14 -58.5(4) . . . . ? C4 C5 C6 N3 -58.7(4) . . . . ? C10 C5 C6 N3 64.3(3) . . . . ? C14 C5 C6 N3 -174.7(3) . . . . ? N3 C7 C8 N4 0.0(4) . . . . ? C4 C5 C10 N5 -56.2(4) . . . . ? C6 C5 C10 N5 -175.2(3) . . . . ? C14 C5 C10 N5 69.3(4) . . . . ? N5 C11 C12 N6 1.1(5) . . . . ? C4 C5 C14 N7 -166.3(2) . . . . ? C10 C5 C14 N7 65.5(3) . . . . ? C6 C5 C14 N7 -51.0(3) . . . . ? N7 C16 C17 N8 -0.3(4) . . . . ? O2 C18 C19 C20 14.4(5) . . . . ? O1 C18 C19 C20 -166.5(3) . . . . ? O2 C18 C19 C21 -166.1(4) . . . . ? O1 C18 C19 C21 13.0(5) . . . . ? C21 C19 C20 C21 0.6(6) . . . 3_575 ? C18 C19 C20 C21 -179.9(3) . . . 3_575 ? C20 C19 C21 C20 -0.6(6) . . . 3_575 ? C18 C19 C21 C20 179.9(3) . . . 3_575 ? O3 C22 C23 C25 173.2(4) . . . . ? O4 C22 C23 C25 -7.2(6) . . . . ? O3 C22 C23 C24 -5.0(6) . . . . ? O4 C22 C23 C24 174.7(4) . . . . ? C25 C23 C24 C25 -0.1(6) . . . 3_776 ? C22 C23 C24 C25 178.1(3) . . . 3_776 ? C24 C23 C25 C24 0.1(6) . . . 3_776 ? C22 C23 C25 C24 -178.1(3) . . . 3_776 ? N2 C3 N1 C2 1.3(4) . . . . ? N2 C3 N1 Ag2 -177.4(2) . . . 3_475 ? C1 C2 N1 C3 -0.9(4) . . . . ? C1 C2 N1 Ag2 177.7(3) . . . 3_475 ? N1 C3 N2 C1 -1.2(4) . . . . ? N1 C3 N2 C4 176.8(3) . . . . ? C2 C1 N2 C3 0.6(4) . . . . ? C2 C1 N2 C4 -177.3(3) . . . . ? C5 C4 N2 C3 -104.9(4) . . . . ? C5 C4 N2 C1 72.6(4) . . . . ? N4 C9 N3 C7 -0.9(4) . . . . ? N4 C9 N3 C6 -178.2(3) . . . . ? C8 C7 N3 C9 0.5(4) . . . . ? C8 C7 N3 C6 177.7(3) . . . . ? C5 C6 N3 C9 -95.0(4) . . . . ? C5 C6 N3 C7 88.3(4) . . . . ? N3 C9 N4 C8 0.9(4) . . . . ? N3 C9 N4 Ag1 -174.2(2) . . . . ? C7 C8 N4 C9 -0.5(4) . . . . ? C7 C8 N4 Ag1 173.8(2) . . . . ? N8 Ag1 N4 C9 -169.6(5) 2 . . . ? N8 Ag1 N4 C8 16.8(7) 2 . . . ? N6 C13 N5 C11 1.1(4) . . . . ? N6 C13 N5 C10 176.8(3) . . . . ? C12 C11 N5 C13 -1.3(4) . . . . ? C12 C11 N5 C10 -176.8(3) . . . . ? C5 C10 N5 C13 114.1(4) . . . . ? C5 C10 N5 C11 -71.1(4) . . . . ? N5 C13 N6 C12 -0.4(4) . . . . ? N5 C13 N6 Ag2 -176.9(2) . . . . ? C11 C12 N6 C13 -0.5(5) . . . . ? C11 C12 N6 Ag2 176.4(3) . . . . ? N1 Ag2 N6 C13 -152.9(7) 3_475 . . . ? N1 Ag2 N6 C12 31.2(10) 3_475 . . . ? N8 C15 N7 C16 0.1(4) . . . . ? N8 C15 N7 C14 179.7(3) . . . . ? C17 C16 N7 C15 0.1(4) . . . . ? C17 C16 N7 C14 -179.5(3) . . . . ? C5 C14 N7 C15 92.2(4) . . . . ? C5 C14 N7 C16 -88.3(4) . . . . ? N7 C15 N8 C17 -0.3(4) . . . . ? N7 C15 N8 Ag1 -177.7(2) . . . 2_545 ? C16 C17 N8 C15 0.4(4) . . . . ? C16 C17 N8 Ag1 177.6(2) . . . 2_545 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1D O1 0.848(19) 1.97(2) 2.790(4) 162(5) . O1W H1C O3 0.843(19) 2.16(3) 2.903(4) 146(4) . O2W H2C O3W 0.849(19) 1.95(3) 2.770(5) 163(6) . O2W H2D O3 0.878(19) 2.01(4) 2.805(5) 150(6) . O3W H3C O1W 0.848(19) 1.90(2) 2.735(5) 168(6) . O3W H3D O6W 0.855(19) 2.15(4) 2.903(7) 146(6) 2 O4W H4C O4 0.861(19) 1.87(3) 2.715(5) 165(5) . O4W H4D O5W 0.847(19) 2.15(5) 2.828(6) 137(6) 1_565 O5W H5D O7W 0.79(2) 2.51(8) 2.989(9) 120(7) . O8W H8C O2W 0.865(19) 2.17(2) 3.030(4) 171(5) 3_666 O8W H8D O1 0.846(19) 2.02(2) 2.850(4) 165(5) 2_545 _diffrn_measured_fraction_theta_max 0.851 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.830 _refine_diff_density_min -0.611 _refine_diff_density_rms 0.094 #===END