Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _publ_contact_author 'Hanton, Lyall R.' _publ_contact_author_email lhanton@alkali.otago.ac.nz _publ_author_address ; Department of Chemistry University of Otago PO Box 56 Dunedin New Zealand ; _publ_section_title ; Co-ordination polymers and isomerism; a study using silver(I) and a pi-stacked ligand. ; loop_ _publ_author_name 'Caradoc-Davies, Paula L.' 'Hanton, Lyall R.' 'Henderson, William' _journal_coden_Cambridge 186 _journal_name_full 'Dalton Transactions' _journal_volume ? _journal_page_first ? _journal_page_last ? _journal_year ? _ccdc_journal_depnumber ? data_[Ag(L)](ClO4) Compound 1 _database_code_CSD 167258 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H18 Ag Cl N4 O4 S2' _chemical_formula_weight 561.80 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.371(5) _cell_length_b 10.844(5) _cell_length_c 13.407(5) _cell_angle_alpha 66.954(5) _cell_angle_beta 80.260(5) _cell_angle_gamma 73.600(5) _cell_volume 1072.0(9) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 4302 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 26.45 _exptl_crystal_description irregular-block _exptl_crystal_colour 'pale-yellow' _exptl_crystal_size_max 0.84 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.741 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 564 _exptl_absorpt_coefficient_mu 1.293 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5003 _exptl_absorpt_correction_T_max 0.7622 _exptl_absorpt_process_details 'SADABS (sheldrick 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 13364 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0174 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 26.45 _reflns_number_total 4302 _reflns_number_gt 3983 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0528P)^2^+0.7913P] 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 4302 _refine_ls_number_parameters 294 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0331 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0865 _refine_ls_wR_factor_gt 0.0851 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 0.05356(2) 0.80167(2) 0.306790(15) 0.04381(9) Uani 1 1 d . . . Cl1 Cl 0.43093(7) 1.19224(7) 0.19462(5) 0.03960(15) Uani 1 1 d . . . O11 O 0.2576(4) 1.2029(6) 0.1881(4) 0.1363(19) Uani 1 1 d . . . O12 O 0.4449(7) 1.2256(5) 0.2833(3) 0.0939(15) Uani 0.844(6) 1 d P . . O13 O 0.5055(5) 1.0428(4) 0.2280(3) 0.0778(11) Uani 0.844(6) 1 d P . . O14 O 0.5033(5) 1.2668(4) 0.0958(3) 0.0869(13) Uani 0.844(6) 1 d P . . O21 O 0.404(3) 1.1069(19) 0.1636(18) 0.073(6) Uani 0.156(6) 1 d P . . O22 O 0.310(3) 1.284(2) 0.226(3) 0.110(12) Uani 0.156(6) 1 d P . . O23 O 0.596(4) 1.154(3) 0.232(2) 0.118(9) Uiso 0.156(6) 1 d P . . S1 S -0.21172(7) 0.75228(6) 0.44071(5) 0.03230(14) Uani 1 1 d . . . S2 S 0.35235(7) 0.74892(7) 0.20844(5) 0.03720(15) Uani 1 1 d . . . N1 N 0.1732(2) 0.6277(2) 0.50164(17) 0.0315(4) Uani 1 1 d . . . N2 N 0.0118(2) 0.95421(19) 0.41412(16) 0.0315(4) Uani 1 1 d . . . N3 N 0.0288(3) 0.6446(2) 0.20838(18) 0.0366(5) Uani 1 1 d . . . N4 N 0.0172(3) 0.9597(2) 0.11120(16) 0.0340(4) Uani 1 1 d . . . C1 C 0.3271(3) 0.6356(3) 0.5116(2) 0.0359(5) Uani 1 1 d . . . H1 H 0.4101 0.6244 0.4580 0.043 Uiso 1 1 calc R . . C2 C 0.3688(3) 0.6594(3) 0.5969(2) 0.0393(6) Uani 1 1 d . . . H2 H 0.4771 0.6636 0.6004 0.047 Uiso 1 1 calc R . . C3 C 0.2463(4) 0.6769(3) 0.6770(2) 0.0426(6) Uani 1 1 d . . . H3 H 0.2702 0.6938 0.7351 0.051 Uiso 1 1 calc R . . C4 C 0.0866(3) 0.6684(3) 0.6684(2) 0.0358(5) Uani 1 1 d . . . H4 H 0.0020 0.6789 0.7213 0.043 Uiso 1 1 calc R . . C5 C 0.0544(3) 0.6440(2) 0.57978(18) 0.0274(4) Uani 1 1 d . . . C6 C -0.1184(3) 0.6339(2) 0.5674(2) 0.0320(5) Uani 1 1 d . . . H6A H -0.1924 0.6504 0.6272 0.038 Uiso 1 1 calc R . . H6B H -0.1114 0.5404 0.5737 0.038 Uiso 1 1 calc R . . C7 C -0.2715(3) 0.9141(3) 0.4633(2) 0.0353(5) Uani 1 1 d . . . H7A H -0.3275 0.9856 0.4008 0.042 Uiso 1 1 calc R . . H7B H -0.3508 0.9053 0.5260 0.042 Uiso 1 1 calc R . . C8 C -0.1272(3) 0.9591(2) 0.48163(19) 0.0304(5) Uani 1 1 d . . . C9 C 0.1368(3) 0.9952(2) 0.4332(2) 0.0320(5) Uani 1 1 d . . . H9 H 0.2339 0.9930 0.3878 0.038 Uiso 1 1 calc R . . C10 C -0.1252(3) 0.6606(3) 0.1814(2) 0.0426(6) Uani 1 1 d . . . H10 H -0.2138 0.6672 0.2327 0.051 Uiso 1 1 calc R . . C11 C -0.1594(4) 0.6679(3) 0.0820(3) 0.0494(7) Uani 1 1 d . . . H11 H -0.2683 0.6805 0.0663 0.059 Uiso 1 1 calc R . . C12 C -0.0282(5) 0.6562(4) 0.0065(3) 0.0626(9) Uani 1 1 d . . . H12 H -0.0470 0.6612 -0.0616 0.075 Uiso 1 1 calc R . . C13 C 0.1325(4) 0.6366(3) 0.0333(2) 0.0507(7) Uani 1 1 d . . . H13 H 0.2230 0.6262 -0.0161 0.061 Uiso 1 1 calc R . . C14 C 0.1568(3) 0.6328(2) 0.1341(2) 0.0338(5) Uani 1 1 d . . . C15 C 0.3299(3) 0.6152(3) 0.1658(2) 0.0407(6) Uani 1 1 d . . . H15A H 0.4089 0.6123 0.1044 0.049 Uiso 1 1 calc R . . H15B H 0.3596 0.5269 0.2246 0.049 Uiso 1 1 calc R . . C16 C 0.3241(3) 0.8990(3) 0.0841(2) 0.0370(5) Uani 1 1 d . . . H16A H 0.3506 0.9735 0.0959 0.044 Uiso 1 1 calc R . . H16B H 0.4040 0.8776 0.0283 0.044 Uiso 1 1 calc R . . C17 C 0.1518(3) 0.9506(2) 0.04141(19) 0.0304(5) Uani 1 1 d . . . C18 C -0.1332(3) 1.0092(2) 0.06900(19) 0.0348(5) Uani 1 1 d . . . H18 H -0.2284 1.0167 0.1154 0.042 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.03737(13) 0.07352(17) 0.02544(12) -0.02329(10) 0.00675(8) -0.01811(10) Cl1 0.0323(3) 0.0612(4) 0.0290(3) -0.0236(3) 0.0005(2) -0.0078(3) O11 0.0536(18) 0.215(5) 0.102(3) -0.020(3) -0.0216(19) -0.019(3) O12 0.126(4) 0.131(3) 0.065(2) -0.064(2) 0.012(2) -0.061(3) O13 0.076(2) 0.068(2) 0.083(3) -0.0320(18) 0.014(2) -0.0129(17) O14 0.095(3) 0.089(2) 0.0503(18) -0.0132(16) 0.0416(17) -0.0271(19) O21 0.086(13) 0.064(11) 0.112(15) -0.070(12) 0.009(11) -0.036(10) O22 0.097(17) 0.110(16) 0.17(3) -0.121(19) 0.097(18) -0.052(14) S1 0.0258(3) 0.0461(3) 0.0311(3) -0.0194(2) 0.0004(2) -0.0114(2) S2 0.0281(3) 0.0574(4) 0.0253(3) -0.0107(3) -0.0023(2) -0.0149(3) N1 0.0275(9) 0.0326(10) 0.0316(10) -0.0127(8) -0.0018(8) -0.0018(7) N2 0.0312(10) 0.0272(9) 0.0308(10) -0.0096(8) 0.0062(8) -0.0051(8) N3 0.0325(10) 0.0402(11) 0.0347(11) -0.0092(9) -0.0023(8) -0.0112(9) N4 0.0368(11) 0.0336(10) 0.0262(9) -0.0098(8) 0.0063(8) -0.0066(8) C1 0.0255(11) 0.0389(12) 0.0381(13) -0.0132(10) -0.0009(10) -0.0015(9) C2 0.0305(12) 0.0434(13) 0.0403(14) -0.0091(11) -0.0091(10) -0.0081(10) C3 0.0497(15) 0.0485(14) 0.0334(13) -0.0139(11) -0.0098(11) -0.0145(12) C4 0.0393(13) 0.0391(12) 0.0282(12) -0.0121(10) 0.0029(10) -0.0115(10) C5 0.0280(11) 0.0231(10) 0.0280(11) -0.0074(8) -0.0007(8) -0.0048(8) C6 0.0306(11) 0.0314(11) 0.0326(12) -0.0105(9) 0.0040(9) -0.0105(9) C7 0.0241(11) 0.0372(12) 0.0400(13) -0.0141(10) 0.0005(9) -0.0020(9) C8 0.0273(11) 0.0232(10) 0.0333(12) -0.0073(9) 0.0029(9) -0.0022(8) C9 0.0286(11) 0.0272(10) 0.0354(12) -0.0118(9) 0.0088(9) -0.0054(9) C10 0.0349(13) 0.0405(13) 0.0503(16) -0.0105(12) -0.0062(11) -0.0128(11) C11 0.0515(16) 0.0427(14) 0.0584(18) -0.0122(13) -0.0225(14) -0.0157(12) C12 0.087(3) 0.068(2) 0.0440(17) -0.0202(15) -0.0195(17) -0.0266(19) C13 0.0618(18) 0.0545(17) 0.0402(15) -0.0217(13) 0.0030(13) -0.0180(14) C14 0.0389(13) 0.0253(10) 0.0338(12) -0.0062(9) -0.0013(10) -0.0095(9) C15 0.0322(12) 0.0376(13) 0.0433(14) -0.0081(11) 0.0010(11) -0.0064(10) C16 0.0337(12) 0.0420(13) 0.0344(13) -0.0103(10) 0.0064(10) -0.0181(10) C17 0.0342(12) 0.0244(10) 0.0300(11) -0.0086(9) 0.0052(9) -0.0091(9) C18 0.0351(12) 0.0344(12) 0.0270(11) -0.0089(9) 0.0087(9) -0.0061(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.509(2) . ? Ag1 N4 2.523(2) . ? Ag1 N3 2.596(2) . ? Ag1 S2 2.6436(14) . ? Ag1 S1 2.6480(12) . ? Cl1 O21 1.237(12) . ? Cl1 O22 1.348(16) . ? Cl1 O14 1.393(3) . ? Cl1 O12 1.403(3) . ? Cl1 O11 1.437(4) . ? Cl1 O23 1.44(3) . ? Cl1 O13 1.474(4) . ? O11 O22 1.37(2) . ? O11 O21 1.451(19) . ? O12 O22 1.33(3) . ? O12 O23 1.50(3) . ? O13 O21 1.18(2) . ? O13 O23 1.61(3) . ? S1 C7 1.814(3) . ? S1 C6 1.822(3) . ? S2 C16 1.810(3) . ? S2 C15 1.818(3) . ? N1 C5 1.346(3) . ? N1 C1 1.347(3) . ? N2 C9 1.342(3) . ? N2 C8 1.350(3) . ? N3 C10 1.344(3) . ? N3 C14 1.348(3) . ? N4 C17 1.345(3) . ? N4 C18 1.347(3) . ? C1 C2 1.384(4) . ? C2 C3 1.385(4) . ? C3 C4 1.393(4) . ? C4 C5 1.396(3) . ? C5 C6 1.522(3) . ? C7 C8 1.511(3) . ? C8 C9 1.395(3) 2_576 ? C9 C8 1.395(3) 2_576 ? C10 C11 1.378(4) . ? C11 C12 1.376(5) . ? C12 C13 1.388(5) . ? C13 C14 1.383(4) . ? C14 C15 1.519(4) . ? C16 C17 1.514(4) . ? C17 C18 1.393(3) 2_575 ? C18 C17 1.393(3) 2_575 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N4 106.47(7) . . ? N2 Ag1 N3 167.51(7) . . ? N4 Ag1 N3 75.20(7) . . ? N2 Ag1 S2 116.73(5) . . ? N4 Ag1 S2 75.80(5) . . ? N3 Ag1 S2 75.75(5) . . ? N2 Ag1 S1 75.13(5) . . ? N4 Ag1 S1 119.92(6) . . ? N3 Ag1 S1 93.21(5) . . ? S2 Ag1 S1 158.33(3) . . ? O21 Cl1 O22 124.1(15) . . ? O21 Cl1 O14 96.2(10) . . ? O22 Cl1 O14 106.8(11) . . ? O21 Cl1 O12 146.9(11) . . ? O22 Cl1 O12 57.7(15) . . ? O14 Cl1 O12 115.4(3) . . ? O21 Cl1 O11 65.2(10) . . ? O22 Cl1 O11 59.0(12) . . ? O14 Cl1 O11 112.1(3) . . ? O12 Cl1 O11 108.1(3) . . ? O21 Cl1 O23 113.0(16) . . ? O22 Cl1 O23 119.2(18) . . ? O14 Cl1 O23 84.6(12) . . ? O12 Cl1 O23 63.5(12) . . ? O11 Cl1 O23 163.3(12) . . ? O21 Cl1 O13 50.7(11) . . ? O22 Cl1 O13 141.1(11) . . ? O14 Cl1 O13 112.0(2) . . ? O12 Cl1 O13 104.8(3) . . ? O11 Cl1 O13 103.4(3) . . ? O23 Cl1 O13 67.1(11) . . ? O22 O11 Cl1 57.3(9) . . ? O22 O11 O21 107.9(12) . . ? Cl1 O11 O21 50.7(6) . . ? O22 O12 Cl1 59.1(7) . . ? O22 O12 O23 116.6(13) . . ? Cl1 O12 O23 59.5(11) . . ? O21 O13 Cl1 54.2(6) . . ? O21 O13 O23 105.3(13) . . ? Cl1 O13 O23 55.4(10) . . ? O13 O21 Cl1 75.1(11) . . ? O13 O21 O11 120.1(14) . . ? Cl1 O21 O11 64.1(7) . . ? O12 O22 Cl1 63.2(12) . . ? O12 O22 O11 116.7(16) . . ? Cl1 O22 O11 63.7(7) . . ? Cl1 O23 O12 57.0(11) . . ? Cl1 O23 O13 57.4(11) . . ? O12 O23 O13 94.3(16) . . ? C7 S1 C6 101.34(12) . . ? C7 S1 Ag1 97.09(8) . . ? C6 S1 Ag1 102.32(8) . . ? C16 S2 C15 102.19(13) . . ? C16 S2 Ag1 98.93(9) . . ? C15 S2 Ag1 99.52(9) . . ? C5 N1 C1 117.5(2) . . ? C9 N2 C8 116.9(2) . . ? C9 N2 Ag1 123.08(15) . . ? C8 N2 Ag1 116.81(16) . . ? C10 N3 C14 117.7(2) . . ? C10 N3 Ag1 115.66(18) . . ? C14 N3 Ag1 112.32(16) . . ? C17 N4 C18 116.9(2) . . ? C17 N4 Ag1 116.56(16) . . ? C18 N4 Ag1 121.75(15) . . ? N1 C1 C2 123.8(2) . . ? C1 C2 C3 118.7(2) . . ? C2 C3 C4 118.4(2) . . ? C3 C4 C5 119.5(2) . . ? N1 C5 C4 122.2(2) . . ? N1 C5 C6 116.6(2) . . ? C4 C5 C6 121.1(2) . . ? C5 C6 S1 115.61(16) . . ? C8 C7 S1 114.19(16) . . ? N2 C8 C9 120.3(2) . 2_576 ? N2 C8 C7 118.8(2) . . ? C9 C8 C7 120.8(2) 2_576 . ? N2 C9 C8 122.7(2) . 2_576 ? N3 C10 C11 123.8(3) . . ? C12 C11 C10 118.2(3) . . ? C11 C12 C13 119.1(3) . . ? C14 C13 C12 119.3(3) . . ? N3 C14 C13 121.9(3) . . ? N3 C14 C15 116.9(2) . . ? C13 C14 C15 121.2(3) . . ? C14 C15 S2 115.20(18) . . ? C17 C16 S2 116.11(16) . . ? N4 C17 C18 120.5(2) . 2_575 ? N4 C17 C16 119.1(2) . . ? C18 C17 C16 120.4(2) 2_575 . ? N4 C18 C17 122.6(2) . 2_575 ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 26.45 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.634 _refine_diff_density_min -0.819 _refine_diff_density_rms 0.080 #===END data_[Ag2(L)](NO3)2 Compound 2 _database_code_CSD 167259 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H36 Ag4 N12 O13 S4' _chemical_formula_weight 1404.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.445(5) _cell_length_b 13.146(5) _cell_length_c 17.529(5) _cell_angle_alpha 100.182(5) _cell_angle_beta 92.571(5) _cell_angle_gamma 115.658(5) _cell_volume 2317.8(15) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 26.45 _exptl_crystal_description wedge _exptl_crystal_colour 'pale-yellow' _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.012 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 1.921 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6506 _exptl_absorpt_correction_T_max 0.7941 _exptl_absorpt_process_details 'SADABS (sheldrick 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30447 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 26.45 _reflns_number_total 9379 _reflns_number_gt 6229 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0625P)^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 9379 _refine_ls_number_parameters 682 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0659 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.1061 _refine_ls_wR_factor_gt 0.0979 _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_restrained_S_all 0.959 _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 C1 C 1.9425(5) 0.9197(4) 1.0410(3) 0.0418(12) Uani 1 1 d . . . H1 H 1.9046 0.8647 1.0708 0.050 Uiso 1 1 calc R . . C2 C 1.9338(5) 0.9882(4) 0.9304(3) 0.0386(11) Uani 1 1 d . . . C3 C 1.8644(5) 0.9806(4) 0.8532(3) 0.0441(12) Uani 1 1 d . . . H3A H 1.9297 1.0219 0.8221 0.053 Uiso 1 1 calc R . . H3B H 1.8107 1.0205 0.8630 0.053 Uiso 1 1 calc R . . C4 C 1.8813(5) 0.7904(5) 0.7590(3) 0.0528(14) Uani 1 1 d . . . H4A H 1.8364 0.7217 0.7175 0.063 Uiso 1 1 calc R . . H4B H 1.9436 0.8505 0.7362 0.063 Uiso 1 1 calc R . . C5 C 1.9556(5) 0.7643(4) 0.8195(3) 0.0467(13) Uani 1 1 d . . . C6 C 2.0849(5) 0.8419(5) 0.8504(4) 0.0579(15) Uani 1 1 d . . . H6 H 2.1276 0.9093 0.8323 0.069 Uiso 1 1 calc R . . C7 C 2.1490(6) 0.8178(6) 0.9081(4) 0.0677(17) Uani 1 1 d . . . H7 H 2.2341 0.8699 0.9304 0.081 Uiso 1 1 calc R . . C8 C 2.0844(6) 0.7148(6) 0.9321(4) 0.0655(17) Uani 1 1 d . . . H8 H 2.1262 0.6953 0.9696 0.079 Uiso 1 1 calc R . . C9 C 1.9562(6) 0.6415(5) 0.8990(3) 0.0603(15) Uani 1 1 d . . . H9 H 1.9125 0.5732 0.9161 0.072 Uiso 1 1 calc R . . C10 C 1.6315(6) 0.3290(5) 0.8952(4) 0.0561(15) Uani 1 1 d . . . H10 H 1.7206 0.3728 0.9124 0.067 Uiso 1 1 calc R . . C11 C 1.5651(6) 0.2274(5) 0.9216(4) 0.0581(15) Uani 1 1 d . . . H11 H 1.6088 0.2041 0.9554 0.070 Uiso 1 1 calc R . . C12 C 1.4347(7) 0.1632(5) 0.8966(4) 0.0651(17) Uani 1 1 d . . . H12 H 1.3875 0.0958 0.9140 0.078 Uiso 1 1 calc R . . C13 C 1.3721(6) 0.1990(5) 0.8449(3) 0.0569(15) Uani 1 1 d . . . H13 H 1.2836 0.1549 0.8260 0.068 Uiso 1 1 calc R . . C14 C 1.4454(5) 0.3031(4) 0.8218(3) 0.0448(12) Uani 1 1 d . . . C15 C 1.3793(5) 0.3434(5) 0.7665(3) 0.0547(14) Uani 1 1 d . . . H15A H 1.2867 0.3095 0.7714 0.066 Uiso 1 1 calc R . . H15B H 1.3874 0.3126 0.7135 0.066 Uiso 1 1 calc R . . C16 C 1.3753(4) 0.5315(4) 0.8683(3) 0.0403(12) Uani 1 1 d . . . H16A H 1.3874 0.6106 0.8769 0.048 Uiso 1 1 calc R . . H16B H 1.2821 0.4812 0.8623 0.048 Uiso 1 1 calc R . . C17 C 1.4406(4) 0.5168(4) 0.9386(3) 0.0316(10) Uani 1 1 d . . . C18 C 1.6240(4) 0.5768(4) 1.0265(3) 0.0336(10) Uani 1 1 d . . . H18 H 1.7107 0.6282 1.0459 0.040 Uiso 1 1 calc R . . C19 C 1.0885(5) 0.4766(5) 0.7364(3) 0.0497(13) Uani 1 1 d . . . H19 H 1.0345 0.4604 0.7752 0.060 Uiso 1 1 calc R . . C20 C 1.1582(6) 0.5896(5) 0.7310(3) 0.0573(15) Uani 1 1 d . . . H20 H 1.1520 0.6484 0.7661 0.069 Uiso 1 1 calc R . . C21 C 1.2382(6) 0.6158(5) 0.6728(3) 0.0574(15) Uani 1 1 d . . . H21 H 1.2876 0.6920 0.6689 0.069 Uiso 1 1 calc R . . C22 C 1.2422(5) 0.5268(5) 0.6217(3) 0.0484(13) Uani 1 1 d . . . H22 H 1.2936 0.5418 0.5816 0.058 Uiso 1 1 calc R . . C23 C 1.1693(5) 0.4132(4) 0.6294(3) 0.0431(12) Uani 1 1 d . . . C24 C 1.1740(5) 0.3134(5) 0.5741(3) 0.0506(14) Uani 1 1 d . . . H24A H 1.2050 0.2730 0.6046 0.061 Uiso 1 1 calc R . . H24B H 1.2380 0.3446 0.5395 0.061 Uiso 1 1 calc R . . C26 C 1.0114(5) 0.2871(4) 0.4409(3) 0.0471(13) Uani 1 1 d . . . H26A H 1.0880 0.3047 0.4142 0.057 Uiso 1 1 calc R . . H26B H 0.9352 0.2369 0.4026 0.057 Uiso 1 1 calc R . . C27 C 1.0032(5) 0.3989(4) 0.4721(3) 0.0374(11) Uani 1 1 d . . . C28 C 1.0767(4) 0.4980(4) 0.4447(3) 0.0380(11) Uani 1 1 d . . . H28 H 1.1296 0.4945 0.4066 0.046 Uiso 1 1 calc R . . C30 C 0.5375(5) 0.1722(4) 0.6367(3) 0.0428(12) Uani 1 1 d . . . H30A H 0.4687 0.1375 0.6678 0.051 Uiso 1 1 calc R . . H30B H 0.5256 0.2340 0.6201 0.051 Uiso 1 1 calc R . . C31 C 0.5198(4) 0.0815(4) 0.5644(3) 0.0348(11) Uani 1 1 d . . . C32 C 0.3993(4) -0.0116(4) 0.5385(3) 0.0383(11) Uani 1 1 d . . . H32 H 0.3300 -0.0181 0.5663 0.046 Uiso 1 1 calc R . . C33 C 0.6772(5) 0.1135(4) 0.7410(3) 0.0481(13) Uani 1 1 d . . . H33A H 0.7462 0.1414 0.7847 0.058 Uiso 1 1 calc R . . H33B H 0.5943 0.0838 0.7615 0.058 Uiso 1 1 calc R . . C34 C 0.6838(5) 0.0157(4) 0.6850(3) 0.0416(12) Uani 1 1 d . . . C35 C 0.5757(5) -0.0878(4) 0.6588(3) 0.0508(14) Uani 1 1 d . . . H35 H 0.4973 -0.1010 0.6782 0.061 Uiso 1 1 calc R . . C36 C 0.5832(6) -0.1726(5) 0.6035(4) 0.0610(16) Uani 1 1 d . . . H36 H 0.5097 -0.2426 0.5840 0.073 Uiso 1 1 calc R . . C37 C 0.7023(6) -0.1514(5) 0.5777(4) 0.0614(16) Uani 1 1 d . . . H37 H 0.7104 -0.2070 0.5405 0.074 Uiso 1 1 calc R . . C38 C 0.8084(6) -0.0470(5) 0.6080(3) 0.0522(14) Uani 1 1 d . . . H38 H 0.8885 -0.0329 0.5907 0.063 Uiso 1 1 calc R . . N1 N 1.8773(4) 0.9077(3) 0.9727(2) 0.0412(10) Uani 1 1 d . A . N2 N 1.8929(4) 0.6641(4) 0.8442(3) 0.0479(11) Uani 1 1 d . . . N3 N 1.5741(4) 0.3668(3) 0.8463(2) 0.0435(10) Uani 1 1 d . . . N4 N 1.5654(3) 0.5952(3) 0.9660(2) 0.0314(8) Uani 1 1 d . A . N5 N 1.0951(4) 0.3886(3) 0.6878(2) 0.0425(10) Uani 1 1 d . . . N6 N 0.9272(3) 0.4014(3) 0.5278(2) 0.0361(9) Uani 1 1 d . . . N7 N 0.6216(4) 0.0930(3) 0.5254(2) 0.0357(9) Uani 1 1 d . . . N8 N 0.8004(4) 0.0355(3) 0.6616(2) 0.0442(10) Uani 1 1 d . . . N11 N 1.1466(4) 0.0426(4) 0.6740(3) 0.0501(11) Uani 1 1 d . . . N22 N 1.0266(4) 0.3369(4) 0.8842(2) 0.0482(11) Uani 1 1 d . . . O1 O 1.3261(10) 0.8896(10) 0.7321(6) 0.238(5) Uani 1 1 d . . . O11 O 1.1684(6) 0.0836(5) 0.6163(3) 0.1039(18) Uani 1 1 d . . . O12 O 1.1803(5) -0.0350(4) 0.6797(3) 0.0902(15) Uani 1 1 d . . . O13 O 1.0915(4) 0.0726(4) 0.7267(3) 0.0652(11) Uani 1 1 d . . . O21 O 0.9158(4) 0.3207(4) 0.8610(3) 0.0793(13) Uani 1 1 d . . . O22 O 1.0930(4) 0.4208(4) 0.9395(2) 0.0719(12) Uani 1 1 d . . . O23 O 1.0769(4) 0.2753(3) 0.8501(2) 0.0522(9) Uani 1 1 d . . . S1 S 1.76179(13) 0.83662(11) 0.79572(7) 0.0461(3) Uani 1 1 d . A . S2 S 1.43788(12) 0.49912(12) 0.77818(7) 0.0454(3) Uani 1 1 d . . . S3 S 1.02077(12) 0.20883(11) 0.51456(8) 0.0443(3) Uani 1 1 d . . . S4 S 0.69292(13) 0.23502(10) 0.69870(7) 0.0435(3) Uani 1 1 d . . . Ag1 Ag 1.67000(4) 0.74931(3) 0.91325(2) 0.04681(12) Uani 1 1 d . . . Ag2 Ag 1.68025(4) 0.54303(3) 0.80581(2) 0.04963(13) Uani 1 1 d . A . Ag3 Ag 0.82935(4) 0.24007(3) 0.58320(2) 0.04955(13) Uani 1 1 d . . . Ag4 Ag 0.98390(4) 0.20406(3) 0.70546(2) 0.05070(13) Uani 1 1 d . . . N33 N 1.5259(19) 0.9044(16) 0.9085(14) 0.068(4) Uani 0.52(2) 1 d PU A 1 O31 O 1.459(2) 0.7937(19) 0.8559(16) 0.156(10) Uani 0.52(2) 1 d PU A 1 O32 O 1.492(2) 0.9600(17) 0.8815(17) 0.178(10) Uani 0.52(2) 1 d PU A 1 O33 O 1.6142(14) 0.9141(17) 0.9426(8) 0.104(6) Uani 0.52(2) 1 d PU A 1 N331 N 1.4988(16) 0.8824(14) 0.8735(11) 0.044(5) Uani 0.48(2) 1 d PU A 2 O331 O 1.488(2) 0.807(2) 0.9016(14) 0.110(9) Uani 0.48(2) 1 d P A 2 O332 O 1.435(2) 0.915(2) 0.8389(12) 0.121(9) Uani 0.48(2) 1 d P A 2 O333 O 1.6133(18) 0.9776(15) 0.9083(19) 0.174(12) Uani 0.48(2) 1 d P A 2 N44 N 1.6018(3) 0.4636(2) 0.59450(17) 0.0069(6) Uiso 1 1 d D . . O41 O 1.6949(8) 0.5142(8) 0.6565(4) 0.062(2) Uani 0.653(8) 1 d PDU B 3 O42 O 1.4846(5) 0.4006(5) 0.6034(4) 0.065(2) Uani 0.653(8) 1 d PD B 3 O43 O 1.6188(9) 0.5535(7) 0.5556(5) 0.096(3) Uani 0.653(8) 1 d PDU B 3 O441 O 1.6298(10) 0.3910(9) 0.5354(5) 0.062(4) Uani 0.347(8) 1 d PD B 4 O442 O 1.6609(18) 0.5649(15) 0.6003(10) 0.186(11) Uani 0.347(8) 1 d PDU B 4 O443 O 1.6768(14) 0.4636(11) 0.6633(7) 0.044(4) Uani 0.347(8) 1 d PDU A 4 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 C1 0.050(3) 0.027(3) 0.037(3) 0.012(2) 0.009(2) 0.006(2) C2 0.041(3) 0.026(2) 0.039(3) 0.009(2) 0.008(2) 0.005(2) C3 0.046(3) 0.036(3) 0.042(3) 0.015(2) 0.004(2) 0.008(2) C4 0.060(3) 0.041(3) 0.038(3) 0.012(2) 0.016(3) 0.002(3) C5 0.045(3) 0.044(3) 0.042(3) 0.007(2) 0.014(2) 0.012(2) C6 0.047(3) 0.046(3) 0.065(4) 0.013(3) 0.018(3) 0.005(3) C7 0.042(3) 0.067(4) 0.073(4) 0.003(3) 0.007(3) 0.011(3) C8 0.047(3) 0.073(4) 0.068(4) 0.019(3) 0.004(3) 0.018(3) C9 0.061(4) 0.056(4) 0.059(4) 0.025(3) 0.010(3) 0.018(3) C10 0.050(3) 0.052(4) 0.077(4) 0.016(3) 0.019(3) 0.030(3) C11 0.071(4) 0.040(3) 0.071(4) 0.017(3) 0.014(3) 0.030(3) C12 0.093(5) 0.029(3) 0.066(4) 0.013(3) 0.027(4) 0.019(3) C13 0.057(3) 0.039(3) 0.054(3) -0.002(3) 0.010(3) 0.007(3) C14 0.054(3) 0.036(3) 0.036(3) 0.000(2) 0.013(2) 0.015(2) C15 0.054(3) 0.046(3) 0.044(3) 0.004(3) 0.001(3) 0.007(3) C16 0.035(3) 0.043(3) 0.042(3) 0.019(2) 0.004(2) 0.013(2) C17 0.030(2) 0.029(2) 0.033(2) 0.0046(19) 0.0060(19) 0.0113(19) C18 0.026(2) 0.029(2) 0.037(3) 0.006(2) 0.0062(19) 0.0054(19) C19 0.053(3) 0.045(3) 0.037(3) 0.006(2) 0.001(2) 0.011(3) C20 0.070(4) 0.038(3) 0.051(3) -0.002(3) -0.009(3) 0.018(3) C21 0.058(4) 0.035(3) 0.061(4) 0.012(3) -0.006(3) 0.005(3) C22 0.037(3) 0.046(3) 0.050(3) 0.021(3) 0.000(2) 0.004(2) C23 0.036(3) 0.043(3) 0.041(3) 0.011(2) -0.005(2) 0.009(2) C24 0.037(3) 0.054(3) 0.052(3) 0.015(3) 0.007(2) 0.011(2) C26 0.062(3) 0.037(3) 0.035(3) 0.004(2) 0.009(2) 0.016(3) C27 0.042(3) 0.039(3) 0.027(2) 0.009(2) 0.006(2) 0.013(2) C28 0.036(3) 0.043(3) 0.033(3) 0.012(2) 0.012(2) 0.015(2) C30 0.048(3) 0.038(3) 0.040(3) 0.002(2) 0.011(2) 0.019(2) C31 0.034(2) 0.032(3) 0.040(3) 0.012(2) 0.008(2) 0.015(2) C32 0.034(2) 0.041(3) 0.040(3) 0.008(2) 0.010(2) 0.017(2) C33 0.049(3) 0.046(3) 0.040(3) 0.016(2) 0.007(2) 0.011(2) C34 0.046(3) 0.030(3) 0.041(3) 0.015(2) 0.000(2) 0.007(2) C35 0.047(3) 0.040(3) 0.057(3) 0.020(3) 0.005(3) 0.009(2) C36 0.065(4) 0.031(3) 0.066(4) 0.010(3) -0.006(3) 0.003(3) C37 0.071(4) 0.035(3) 0.067(4) -0.002(3) -0.001(3) 0.019(3) C38 0.058(3) 0.042(3) 0.052(3) 0.008(3) 0.008(3) 0.020(3) N1 0.041(2) 0.031(2) 0.037(2) 0.0122(18) 0.0041(18) 0.0022(18) N2 0.038(2) 0.045(3) 0.049(3) 0.015(2) 0.008(2) 0.006(2) N3 0.042(2) 0.036(2) 0.052(3) 0.010(2) 0.017(2) 0.016(2) N4 0.0279(19) 0.029(2) 0.032(2) 0.0073(16) 0.0087(16) 0.0072(16) N5 0.043(2) 0.037(2) 0.035(2) 0.0080(19) -0.0015(19) 0.0082(19) N6 0.031(2) 0.039(2) 0.033(2) 0.0119(18) 0.0053(17) 0.0081(17) N7 0.034(2) 0.031(2) 0.037(2) 0.0031(18) 0.0050(17) 0.0108(17) N8 0.047(3) 0.030(2) 0.046(2) 0.011(2) 0.000(2) 0.0088(19) N11 0.048(3) 0.031(2) 0.056(3) 0.008(2) 0.003(2) 0.004(2) N22 0.037(2) 0.060(3) 0.038(2) 0.018(2) 0.007(2) 0.010(2) O1 0.202(10) 0.278(13) 0.233(11) -0.002(9) 0.042(8) 0.129(10) O11 0.157(5) 0.090(4) 0.070(3) 0.041(3) 0.040(3) 0.050(4) O12 0.124(4) 0.071(3) 0.085(3) 0.010(3) 0.021(3) 0.053(3) O13 0.051(2) 0.070(3) 0.068(3) 0.005(2) 0.017(2) 0.025(2) O21 0.039(2) 0.098(4) 0.086(3) 0.015(3) -0.001(2) 0.021(2) O22 0.060(3) 0.088(3) 0.049(2) -0.008(2) 0.002(2) 0.025(2) O23 0.064(2) 0.047(2) 0.046(2) 0.0148(18) 0.0144(19) 0.023(2) S1 0.0467(7) 0.0388(7) 0.0387(7) 0.0139(6) 0.0003(6) 0.0048(6) S2 0.0436(7) 0.0491(8) 0.0346(7) 0.0143(6) 0.0019(5) 0.0111(6) S3 0.0459(7) 0.0324(7) 0.0467(7) 0.0074(6) 0.0061(6) 0.0111(6) S4 0.0492(7) 0.0310(7) 0.0374(7) 0.0024(5) 0.0055(6) 0.0081(6) Ag1 0.0451(2) 0.0344(2) 0.0472(2) 0.01484(18) 0.00901(18) 0.00294(17) Ag2 0.0450(2) 0.0429(2) 0.0482(2) 0.01152(19) 0.01456(18) 0.00673(18) Ag3 0.0381(2) 0.0439(2) 0.0486(2) 0.01869(19) 0.00614(18) -0.00128(17) Ag4 0.0485(2) 0.0376(2) 0.0499(3) 0.01352(18) 0.00248(19) 0.00350(18) N33 0.064(8) 0.068(10) 0.078(11) 0.044(7) 0.019(8) 0.023(8) O31 0.173(15) 0.057(9) 0.20(2) 0.032(11) -0.005(13) 0.015(9) O32 0.22(2) 0.103(11) 0.22(2) 0.000(12) -0.077(17) 0.105(13) O33 0.105(9) 0.127(15) 0.109(10) 0.030(8) 0.022(7) 0.077(10) N331 0.048(6) 0.037(6) 0.057(6) 0.019(4) 0.014(4) 0.023(4) O331 0.122(16) 0.085(14) 0.17(2) 0.091(15) 0.096(15) 0.059(13) O332 0.148(16) 0.19(2) 0.124(15) 0.107(15) 0.083(13) 0.134(16) O333 0.104(12) 0.091(11) 0.37(3) 0.091(16) 0.099(16) 0.063(10) O41 0.066(5) 0.070(6) 0.060(5) 0.029(4) 0.040(4) 0.031(4) O42 0.048(4) 0.051(4) 0.083(5) 0.014(3) -0.024(3) 0.015(3) O43 0.112(7) 0.082(5) 0.068(5) 0.052(5) 0.021(5) 0.004(5) O441 0.052(7) 0.053(7) 0.038(6) -0.001(5) -0.015(5) -0.010(5) O442 0.23(2) 0.40(3) 0.047(10) 0.003(17) -0.012(13) 0.27(2) O443 0.051(5) 0.046(5) 0.034(5) 0.013(4) 0.003(4) 0.021(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.329(6) . ? C1 C2 1.399(6) 2_977 ? C2 N1 1.348(6) . ? C2 C1 1.399(6) 2_977 ? C2 C3 1.502(6) . ? C3 S1 1.809(5) . ? C4 C5 1.505(7) . ? C4 S1 1.821(6) . ? C5 N2 1.360(6) . ? C5 C6 1.396(7) . ? C6 C7 1.381(8) . ? C7 C8 1.386(9) . ? C8 C9 1.385(8) . ? C9 N2 1.328(7) . ? C10 N3 1.340(7) . ? C10 C11 1.395(8) . ? C11 C12 1.361(8) . ? C12 C13 1.394(8) . ? C13 C14 1.404(7) . ? C14 N3 1.343(6) . ? C14 C15 1.503(8) . ? C15 S2 1.825(6) . ? C16 C17 1.498(6) . ? C16 S2 1.821(5) . ? C17 N4 1.350(5) . ? C17 C18 1.398(6) 2_867 ? C18 N4 1.341(5) . ? C18 C17 1.398(6) 2_867 ? C19 N5 1.342(7) . ? C19 C20 1.372(7) . ? C20 C21 1.390(8) . ? C21 C22 1.361(8) . ? C22 C23 1.396(7) . ? C23 N5 1.352(6) . ? C23 C24 1.510(7) . ? C24 S3 1.816(5) . ? C26 C27 1.519(7) . ? C26 S3 1.813(5) . ? C27 N6 1.344(6) . ? C27 C28 1.394(6) . ? C28 N6 1.345(6) 2_766 ? C30 C31 1.517(6) . ? C30 S4 1.807(5) . ? C31 N7 1.343(6) . ? C31 C32 1.375(6) . ? C32 N7 1.336(6) 2_656 ? C33 C34 1.506(7) . ? C33 S4 1.821(5) . ? C34 N8 1.343(6) . ? C34 C35 1.365(7) . ? C35 C36 1.377(8) . ? C36 C37 1.383(8) . ? C37 C38 1.371(7) . ? C38 N8 1.343(7) . ? N1 Ag1 2.405(4) . ? N2 Ag2 2.242(4) . ? N3 Ag2 2.359(4) . ? N4 Ag1 2.248(4) . ? N5 Ag4 2.287(4) . ? N6 C28 1.345(6) 2_766 ? N6 Ag3 2.337(4) . ? N7 C32 1.336(6) 2_656 ? N7 Ag3 2.352(4) . ? N8 Ag4 2.266(4) . ? N11 O11 1.214(6) . ? N11 O13 1.243(6) . ? N11 O12 1.255(6) . ? N22 O21 1.228(5) . ? N22 O22 1.250(5) . ? N22 O23 1.268(6) . ? O13 Ag4 2.583(4) . ? O23 Ag4 2.548(4) . ? S1 Ag1 2.5790(14) . ? S2 Ag2 2.5799(18) . ? S3 Ag3 2.6939(17) . ? S4 Ag3 2.6043(15) . ? Ag1 O33 2.490(17) . ? Ag1 O331 2.52(2) . ? Ag1 Ag2 3.0666(11) . ? Ag2 O443 2.523(13) . ? Ag3 Ag4 2.9477(9) . ? N33 O33 1.10(2) . ? N33 O32 1.13(3) . ? N33 O31 1.43(4) . ? N331 O331 1.15(3) . ? N331 O332 1.181(18) . ? N331 O333 1.38(3) . ? N44 O442 1.187(17) . ? N44 O42 1.269(6) . ? N44 O41 1.337(8) . ? N44 O43 1.413(8) . ? N44 O441 1.425(11) . ? N44 O443 1.449(11) . ? 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 C1 C2 122.4(4) . 2_977 ? N1 C2 C1 119.7(4) . 2_977 ? N1 C2 C3 120.5(4) . . ? C1 C2 C3 119.8(4) 2_977 . ? C2 C3 S1 116.3(3) . . ? C5 C4 S1 114.8(4) . . ? N2 C5 C6 120.8(5) . . ? N2 C5 C4 118.3(4) . . ? C6 C5 C4 120.9(5) . . ? C7 C6 C5 119.6(5) . . ? C6 C7 C8 118.9(5) . . ? C9 C8 C7 118.6(6) . . ? N2 C9 C8 123.1(6) . . ? N3 C10 C11 123.7(5) . . ? C12 C11 C10 118.2(6) . . ? C11 C12 C13 119.7(5) . . ? C12 C13 C14 118.6(5) . . ? N3 C14 C13 122.0(5) . . ? N3 C14 C15 118.7(5) . . ? C13 C14 C15 119.3(5) . . ? C14 C15 S2 117.4(4) . . ? C17 C16 S2 113.3(3) . . ? N4 C17 C18 121.0(4) . 2_867 ? N4 C17 C16 117.8(4) . . ? C18 C17 C16 121.2(4) 2_867 . ? N4 C18 C17 122.4(4) . 2_867 ? N5 C19 C20 122.5(5) . . ? C19 C20 C21 119.7(5) . . ? C22 C21 C20 118.1(5) . . ? C21 C22 C23 120.1(5) . . ? N5 C23 C22 121.4(5) . . ? N5 C23 C24 117.7(4) . . ? C22 C23 C24 120.9(5) . . ? C23 C24 S3 116.1(4) . . ? C27 C26 S3 114.9(3) . . ? N6 C27 C28 120.7(4) . . ? N6 C27 C26 118.9(4) . . ? C28 C27 C26 120.4(4) . . ? N6 C28 C27 121.6(4) 2_766 . ? C31 C30 S4 116.1(3) . . ? N7 C31 C32 120.1(4) . . ? N7 C31 C30 119.9(4) . . ? C32 C31 C30 120.0(4) . . ? N7 C32 C31 122.2(4) 2_656 . ? C34 C33 S4 114.7(3) . . ? N8 C34 C35 121.7(5) . . ? N8 C34 C33 116.9(4) . . ? C35 C34 C33 121.4(5) . . ? C34 C35 C36 119.8(5) . . ? C35 C36 C37 118.6(5) . . ? C38 C37 C36 119.0(6) . . ? N8 C38 C37 122.2(5) . . ? C1 N1 C2 117.9(4) . . ? C1 N1 Ag1 126.0(3) . . ? C2 N1 Ag1 116.0(3) . . ? C9 N2 C5 118.9(5) . . ? C9 N2 Ag2 117.8(4) . . ? C5 N2 Ag2 123.0(3) . . ? C10 N3 C14 117.8(5) . . ? C10 N3 Ag2 124.7(4) . . ? C14 N3 Ag2 117.4(3) . . ? C18 N4 C17 116.6(4) . . ? C18 N4 Ag1 121.6(3) . . ? C17 N4 Ag1 121.8(3) . . ? C19 N5 C23 118.0(4) . . ? C19 N5 Ag4 120.1(3) . . ? C23 N5 Ag4 121.9(3) . . ? C27 N6 C28 117.8(4) . 2_766 ? C27 N6 Ag3 118.9(3) . . ? C28 N6 Ag3 122.9(3) 2_766 . ? C32 N7 C31 117.7(4) 2_656 . ? C32 N7 Ag3 124.2(3) 2_656 . ? C31 N7 Ag3 117.6(3) . . ? C38 N8 C34 118.6(4) . . ? C38 N8 Ag4 118.1(4) . . ? C34 N8 Ag4 123.2(3) . . ? O11 N11 O13 123.3(5) . . ? O11 N11 O12 117.9(6) . . ? O13 N11 O12 118.8(5) . . ? O21 N22 O22 118.5(5) . . ? O21 N22 O23 121.3(5) . . ? O22 N22 O23 120.1(4) . . ? N11 O13 Ag4 119.5(4) . . ? N22 O23 Ag4 109.9(3) . . ? C3 S1 C4 102.4(2) . . ? C3 S1 Ag1 95.31(16) . . ? C4 S1 Ag1 111.59(17) . . ? C16 S2 C15 100.4(2) . . ? C16 S2 Ag2 111.03(15) . . ? C15 S2 Ag2 93.41(19) . . ? C26 S3 C24 100.6(3) . . ? C26 S3 Ag3 91.73(18) . . ? C24 S3 Ag3 106.51(18) . . ? C30 S4 C33 100.7(2) . . ? C30 S4 Ag3 94.77(16) . . ? C33 S4 Ag3 107.84(18) . . ? N4 Ag1 N1 122.99(13) . . ? N4 Ag1 O33 118.9(4) . . ? N1 Ag1 O33 77.7(4) . . ? N4 Ag1 O331 97.9(4) . . ? N1 Ag1 O331 113.6(6) . . ? O33 Ag1 O331 35.9(6) . . ? N4 Ag1 S1 150.59(10) . . ? N1 Ag1 S1 77.66(10) . . ? O33 Ag1 S1 83.8(4) . . ? O331 Ag1 S1 90.7(4) . . ? N4 Ag1 Ag2 73.37(10) . . ? N1 Ag1 Ag2 116.28(10) . . ? O33 Ag1 Ag2 154.1(3) . . ? O331 Ag1 Ag2 124.9(6) . . ? S1 Ag1 Ag2 78.62(4) . . ? N2 Ag2 N3 122.62(15) . . ? N2 Ag2 O443 102.4(4) . . ? N3 Ag2 O443 98.9(3) . . ? N2 Ag2 S2 152.56(12) . . ? N3 Ag2 S2 78.50(11) . . ? O443 Ag2 S2 90.0(3) . . ? N2 Ag2 Ag1 77.69(12) . . ? N3 Ag2 Ag1 114.12(10) . . ? O443 Ag2 Ag1 140.9(3) . . ? S2 Ag2 Ag1 77.36(4) . . ? N6 Ag3 N7 118.97(13) . . ? N6 Ag3 S4 123.14(10) . . ? N7 Ag3 S4 78.34(10) . . ? N6 Ag3 S3 76.47(10) . . ? N7 Ag3 S3 111.27(10) . . ? S4 Ag3 S3 152.00(5) . . ? N6 Ag3 Ag4 119.70(9) . . ? N7 Ag3 Ag4 120.45(10) . . ? S4 Ag3 Ag4 78.56(4) . . ? S3 Ag3 Ag4 73.96(4) . . ? N8 Ag4 N5 143.40(14) . . ? N8 Ag4 O23 121.21(13) . . ? N5 Ag4 O23 89.58(13) . . ? N8 Ag4 O13 84.57(14) . . ? N5 Ag4 O13 124.45(14) . . ? O23 Ag4 O13 76.94(13) . . ? N8 Ag4 Ag3 72.48(10) . . ? N5 Ag4 Ag3 70.94(10) . . ? O23 Ag4 Ag3 142.11(9) . . ? O13 Ag4 Ag3 140.89(10) . . ? O33 N33 O32 138(3) . . ? O33 N33 O31 112(2) . . ? O32 N33 O31 103(2) . . ? N33 O33 Ag1 116.6(18) . . ? O331 N331 O332 141(2) . . ? O331 N331 O333 109(2) . . ? O332 N331 O333 107.8(17) . . ? N331 O331 Ag1 121.3(14) . . ? O442 N44 O42 131.5(10) . . ? O442 N44 O41 67.7(8) . . ? O42 N44 O41 119.8(5) . . ? O442 N44 O43 37.1(8) . . ? O42 N44 O43 115.2(5) . . ? O41 N44 O43 104.5(5) . . ? O442 N44 O441 117.2(10) . . ? O42 N44 O441 103.7(5) . . ? O41 N44 O441 112.6(6) . . ? O43 N44 O441 99.2(6) . . ? O442 N44 O443 93.9(9) . . ? O42 N44 O443 102.9(7) . . ? O41 N44 O443 26.2(5) . . ? O43 N44 O443 130.5(6) . . ? O441 N44 O443 101.0(7) . . ? N44 O443 Ag2 129.8(9) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 26.45 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.311 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.102 #===END