# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1970 data_complex1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H20 Ag Cl N2 O5 S2' _chemical_formula_weight 599.84 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' 'Cl' 'Cl' 0.1484 0.1585 '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 10.618(2) _cell_length_b 11.047(2) _cell_length_c 11.621(2) _cell_angle_alpha 69.48(3) _cell_angle_beta 68.38(3) _cell_angle_gamma 72.25(3) _cell_volume 1162.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used CCD _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 604 _exptl_absorpt_coefficient_mu 1.199 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.653 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart 1k CCD ' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5192 _diffrn_reflns_av_R_equivalents 0.0169 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 23.30 _reflns_number_total 3323 _reflns_number_gt 2716 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0873P)^2^+0.5073P] 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 3323 _refine_ls_number_parameters 295 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1289 _refine_ls_wR_factor_gt 0.1231 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.115 _refine_ls_shift/su_max 0.003 _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 -0.22310(5) -0.32466(4) 0.32972(4) 0.0642(2) Uani 1 1 d . . . S1 S -0.01035(13) -0.51369(13) 0.27655(13) 0.0491(4) Uani 1 1 d . . . S2 S -0.46573(15) -0.32824(17) 0.51369(15) 0.0626(4) Uani 1 1 d . . . N1 N -0.2450(4) -0.3673(4) 0.1576(4) 0.0457(10) Uani 1 1 d . . . N2 N -0.2431(4) -0.1601(4) 0.4126(4) 0.0467(10) Uani 1 1 d . . . O1 O -0.1871(4) -0.5238(4) 0.5609(4) 0.0603(10) Uani 1 1 d . . . C1 C -0.3379(6) -0.2890(6) 0.0992(5) 0.0629(16) Uani 1 1 d . . . H1 H -0.3778 -0.2064 0.1143 0.075 Uiso 1 1 calc R . . C2 C -0.3793(7) -0.3234(8) 0.0163(6) 0.078(2) Uani 1 1 d . . . H2 H -0.4438 -0.2646 -0.0242 0.093 Uiso 1 1 calc R . . C3 C -0.3232(6) -0.4446(7) -0.0041(5) 0.0669(17) Uani 1 1 d . . . H3 H -0.3515 -0.4706 -0.0572 0.080 Uiso 1 1 calc R . . C4 C -0.2230(5) -0.5311(6) 0.0542(5) 0.0511(13) Uani 1 1 d . . . C5 C -0.1587(6) -0.6562(6) 0.0329(5) 0.0607(15) Uani 1 1 d . . . H5 H -0.1863 -0.6857 -0.0180 0.073 Uiso 1 1 calc R . . C6 C -0.0565(6) -0.7346(6) 0.0859(6) 0.0612(15) Uani 1 1 d . . . H6 H -0.0152 -0.8175 0.0718 0.073 Uiso 1 1 calc R . . C7 C -0.0137(6) -0.6899(5) 0.1615(5) 0.0541(13) Uani 1 1 d . . . H7 H 0.0588 -0.7427 0.1943 0.065 Uiso 1 1 calc R . . C8 C -0.0753(5) -0.5707(5) 0.1884(5) 0.0427(11) Uani 1 1 d . . . C9 C -0.1831(5) -0.4872(5) 0.1343(4) 0.0413(11) Uani 1 1 d . . . C10 C -0.0182(6) -0.6462(6) 0.4239(5) 0.0608(15) Uani 1 1 d . . . H10A H 0.0080 -0.7297 0.4028 0.073 Uiso 1 1 calc R . . H10B H 0.0494 -0.6447 0.4610 0.073 Uiso 1 1 calc R . . C11 C -0.1569(7) -0.6399(6) 0.5231(5) 0.0610(15) Uani 1 1 d . . . H11A H -0.2269 -0.6386 0.4874 0.073 Uiso 1 1 calc R . . H11B H -0.1551 -0.7166 0.5965 0.073 Uiso 1 1 calc R . . C12 C -0.3065(7) -0.5116(6) 0.6686(5) 0.0632(16) Uani 1 1 d . . . H12A H -0.3038 -0.4434 0.7018 0.076 Uiso 1 1 calc R . . H12B H -0.3020 -0.5940 0.7357 0.076 Uiso 1 1 calc R . . C13 C -0.4409(7) -0.4789(6) 0.6407(6) 0.0690(17) Uani 1 1 d . . . H13A H -0.5153 -0.4706 0.7187 0.083 Uiso 1 1 calc R . . H13B H -0.4480 -0.5519 0.6168 0.083 Uiso 1 1 calc R . . C14 C -0.4537(5) -0.2124(5) 0.5800(5) 0.0494(13) Uani 1 1 d . . . C15 C -0.5559(6) -0.1881(6) 0.6895(5) 0.0640(16) Uani 1 1 d . . . H15 H -0.6297 -0.2312 0.7240 0.077 Uiso 1 1 calc R . . C16 C -0.5516(8) -0.1020(7) 0.7492(6) 0.0733(19) Uani 1 1 d . . . H16 H -0.6207 -0.0897 0.8240 0.088 Uiso 1 1 calc R . . C17 C -0.4476(7) -0.0355(6) 0.6994(6) 0.0678(17) Uani 1 1 d . . . H17 H -0.4453 0.0223 0.7403 0.081 Uiso 1 1 calc R . . C18 C -0.3411(6) -0.0531(5) 0.5842(5) 0.0537(14) Uani 1 1 d . . . C19 C -0.2345(7) 0.0171(6) 0.5284(7) 0.0704(18) Uani 1 1 d . . . H19 H -0.2303 0.0758 0.5672 0.084 Uiso 1 1 calc R . . C20 C -0.1380(7) -0.0004(6) 0.4186(7) 0.0709(17) Uani 1 1 d . . . H20 H -0.0671 0.0468 0.3802 0.085 Uiso 1 1 calc R . . C21 C -0.1456(6) -0.0904(5) 0.3628(6) 0.0590(15) Uani 1 1 d . . . H21 H -0.0785 -0.1015 0.2866 0.071 Uiso 1 1 calc R . . C22 C -0.3440(5) -0.1418(5) 0.5242(5) 0.0443(12) Uani 1 1 d . . . Cl1 Cl -0.2422(2) 0.07540(17) 0.87608(18) 0.0877(6) Uani 1 1 d D . . O14 O -0.1682(6) -0.0054(6) 0.7947(6) 0.123(2) Uani 1 1 d D A . O11 O -0.3472(8) 0.1653(8) 0.8067(9) 0.110(3) Uiso 0.60 1 d PD A 1 O12 O -0.1596(9) 0.1600(9) 0.8641(9) 0.113(3) Uiso 0.60 1 d PD A 1 O13 O -0.3110(13) 0.0131(12) 0.9958(8) 0.193(6) Uiso 0.60 1 d PD A 1 O11' O -0.2378(19) 0.2044(8) 0.8377(17) 0.245(15) Uiso 0.40 1 d PD A 2 O12' O -0.1780(14) 0.0131(15) 0.9875(10) 0.131(5) Uiso 0.40 1 d PD A 2 O13' O -0.3797(8) 0.0491(13) 0.9464(11) 0.100(4) Uiso 0.40 1 d PD A 2 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 0.0893(4) 0.0531(3) 0.0489(3) -0.0255(2) -0.0109(2) -0.0104(2) S1 0.0535(7) 0.0488(8) 0.0479(8) -0.0130(6) -0.0164(6) -0.0125(6) S2 0.0598(9) 0.0851(11) 0.0580(9) -0.0272(8) -0.0160(7) -0.0275(8) N1 0.051(2) 0.041(2) 0.038(2) -0.0131(18) -0.007(2) -0.0040(19) N2 0.046(2) 0.045(2) 0.048(3) -0.0172(19) -0.010(2) -0.0062(19) O1 0.078(3) 0.057(2) 0.050(2) -0.0116(18) -0.016(2) -0.0259(19) C1 0.060(3) 0.063(4) 0.050(3) -0.018(3) -0.014(3) 0.010(3) C2 0.066(4) 0.108(6) 0.049(4) -0.022(4) -0.026(3) 0.008(4) C3 0.065(4) 0.100(5) 0.044(3) -0.030(3) -0.018(3) -0.013(3) C4 0.057(3) 0.066(3) 0.032(3) -0.017(2) -0.003(2) -0.023(3) C5 0.074(4) 0.070(4) 0.046(3) -0.028(3) -0.003(3) -0.029(3) C6 0.074(4) 0.051(3) 0.056(3) -0.030(3) -0.002(3) -0.013(3) C7 0.058(3) 0.045(3) 0.052(3) -0.016(2) -0.011(3) -0.003(2) C8 0.045(3) 0.042(3) 0.037(3) -0.013(2) -0.004(2) -0.010(2) C9 0.044(3) 0.047(3) 0.028(2) -0.010(2) -0.001(2) -0.014(2) C10 0.080(4) 0.050(3) 0.057(3) -0.011(3) -0.035(3) -0.004(3) C11 0.086(4) 0.052(3) 0.047(3) -0.007(3) -0.017(3) -0.027(3) C12 0.092(4) 0.054(3) 0.041(3) -0.011(2) -0.009(3) -0.027(3) C13 0.081(4) 0.076(4) 0.054(4) -0.020(3) 0.001(3) -0.045(3) C14 0.050(3) 0.058(3) 0.039(3) -0.012(2) -0.016(2) -0.008(2) C15 0.052(3) 0.077(4) 0.047(3) -0.014(3) -0.009(3) 0.000(3) C16 0.087(5) 0.075(4) 0.043(3) -0.025(3) -0.018(3) 0.015(4) C17 0.089(5) 0.060(4) 0.058(4) -0.031(3) -0.033(4) 0.013(3) C18 0.065(3) 0.043(3) 0.055(3) -0.018(2) -0.029(3) 0.007(3) C19 0.096(5) 0.047(3) 0.087(5) -0.026(3) -0.045(4) -0.009(3) C20 0.077(4) 0.057(4) 0.086(5) -0.013(3) -0.027(4) -0.026(3) C21 0.051(3) 0.051(3) 0.066(4) -0.012(3) -0.011(3) -0.010(3) C22 0.050(3) 0.044(3) 0.041(3) -0.014(2) -0.023(2) 0.002(2) Cl1 0.1005(13) 0.0633(10) 0.0815(12) -0.0364(9) 0.0106(10) -0.0184(9) O14 0.117(4) 0.147(5) 0.123(5) -0.095(4) -0.046(4) 0.030(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.263(4) . ? Ag1 N1 2.312(4) . ? Ag1 S1 2.6163(17) . ? Ag1 S2 2.6747(18) . ? Ag1 O1 2.881(4) . ? S1 C8 1.778(5) . ? S1 C10 1.815(6) . ? S2 C14 1.764(6) . ? S2 C13 1.821(7) . ? N1 C1 1.320(7) . ? N1 C9 1.360(6) . ? N2 C21 1.316(7) . ? N2 C22 1.378(6) . ? O1 C11 1.407(7) . ? O1 C12 1.427(7) . ? C1 C2 1.392(9) . ? C2 C3 1.355(10) . ? C3 C4 1.401(8) . ? C4 C5 1.406(8) . ? C4 C9 1.419(7) . ? C5 C6 1.361(9) . ? C6 C7 1.399(8) . ? C7 C8 1.368(7) . ? C8 C9 1.427(7) . ? C10 C11 1.498(8) . ? C12 C13 1.490(9) . ? C14 C15 1.383(8) . ? C14 C22 1.424(7) . ? C15 C16 1.378(9) . ? C16 C17 1.349(10) . ? C17 C18 1.429(9) . ? C18 C19 1.394(9) . ? C18 C22 1.400(7) . ? C19 C20 1.344(9) . ? C20 C21 1.399(9) . ? Cl1 O11' 1.346(7) . ? Cl1 O13 1.352(7) . ? Cl1 O14 1.388(4) . ? Cl1 O12 1.407(6) . ? Cl1 O13' 1.449(7) . ? Cl1 O11 1.519(6) . ? Cl1 O12' 1.534(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N1 143.25(15) . . ? N2 Ag1 S1 129.08(11) . . ? N1 Ag1 S1 75.91(11) . . ? N2 Ag1 S2 76.86(11) . . ? N1 Ag1 S2 107.85(11) . . ? S1 Ag1 S2 131.49(6) . . ? N2 Ag1 O1 92.16(13) . . ? N1 Ag1 O1 124.11(13) . . ? S1 Ag1 O1 69.03(9) . . ? S2 Ag1 O1 70.01(9) . . ? C8 S1 C10 102.6(3) . . ? C8 S1 Ag1 97.24(16) . . ? C10 S1 Ag1 106.7(2) . . ? C14 S2 C13 100.1(3) . . ? C14 S2 Ag1 97.05(17) . . ? C13 S2 Ag1 106.5(2) . . ? C1 N1 C9 119.0(5) . . ? C1 N1 Ag1 120.5(4) . . ? C9 N1 Ag1 119.0(3) . . ? C21 N2 C22 118.3(5) . . ? C21 N2 Ag1 119.2(4) . . ? C22 N2 Ag1 122.0(3) . . ? C11 O1 C12 115.1(4) . . ? C11 O1 Ag1 101.2(3) . . ? C12 O1 Ag1 111.9(3) . . ? N1 C1 C2 123.6(6) . . ? C3 C2 C1 118.4(6) . . ? C2 C3 C4 120.4(6) . . ? C3 C4 C5 122.6(5) . . ? C3 C4 C9 117.8(5) . . ? C5 C4 C9 119.6(5) . . ? C6 C5 C4 120.8(5) . . ? C5 C6 C7 119.7(5) . . ? C8 C7 C6 121.9(5) . . ? C7 C8 C9 119.3(5) . . ? C7 C8 S1 120.2(4) . . ? C9 C8 S1 120.2(4) . . ? N1 C9 C4 120.7(5) . . ? N1 C9 C8 120.7(4) . . ? C4 C9 C8 118.6(5) . . ? C11 C10 S1 114.7(4) . . ? O1 C11 C10 107.7(5) . . ? O1 C12 C13 114.7(5) . . ? C12 C13 S2 114.7(4) . . ? C15 C14 C22 118.8(5) . . ? C15 C14 S2 118.6(4) . . ? C22 C14 S2 122.5(4) . . ? C16 C15 C14 122.0(6) . . ? C17 C16 C15 120.2(6) . . ? C16 C17 C18 120.5(6) . . ? C19 C18 C22 118.7(5) . . ? C19 C18 C17 121.8(6) . . ? C22 C18 C17 119.5(6) . . ? C20 C19 C18 119.9(6) . . ? C19 C20 C21 119.0(6) . . ? N2 C21 C20 123.3(6) . . ? N2 C22 C18 120.7(5) . . ? N2 C22 C14 120.4(5) . . ? C18 C22 C14 118.9(5) . . ? O11' Cl1 O13 123.9(10) . . ? O11' Cl1 O14 121.1(7) . . ? O13 Cl1 O14 114.9(6) . . ? O11' Cl1 O12 39.2(9) . . ? O13 Cl1 O12 118.0(6) . . ? O14 Cl1 O12 109.2(5) . . ? O11' Cl1 O13' 113.5(7) . . ? O13 Cl1 O13' 41.5(7) . . ? O14 Cl1 O13' 111.8(5) . . ? O12 Cl1 O13' 139.0(6) . . ? O11' Cl1 O11 65.0(9) . . ? O13 Cl1 O11 108.5(6) . . ? O14 Cl1 O11 100.4(4) . . ? O12 Cl1 O11 103.7(5) . . ? O13' Cl1 O11 68.6(6) . . ? O11' Cl1 O12' 106.2(7) . . ? O13 Cl1 O12' 56.7(7) . . ? O14 Cl1 O12' 102.6(5) . . ? O12 Cl1 O12' 73.2(7) . . ? O13' Cl1 O12' 98.1(6) . . ? O11 Cl1 O12' 156.5(6) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 23.30 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.973 _refine_diff_density_min -0.609 _refine_diff_density_rms 0.082 #======================================================================END data_complex2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H24 Ag Cl N2 O6 S2' _chemical_formula_weight 643.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 9.0880(10) _cell_length_b 11.0640(10) _cell_length_c 14.898(2) _cell_angle_alpha 92.90(1) _cell_angle_beta 105.69(2) _cell_angle_gamma 113.98(2) _cell_volume 1295.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used CCD _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.651 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 1.085 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.891 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD ' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7637 _diffrn_reflns_av_R_equivalents 0.0087 _diffrn_reflns_av_sigmaI/netI 0.0150 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5511 _reflns_number_gt 4848 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+0.5406P] 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 5511 _refine_ls_number_parameters 352 _refine_ls_number_restraints 93 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0868 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.121 _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 1.43458(3) 0.21388(2) 1.212290(14) 0.05428(9) Uani 1 1 d . . . S1 S 1.60728(10) 0.20797(8) 1.37775(5) 0.05835(18) Uani 1 1 d . . . S2 S 1.24160(8) 0.09151(7) 1.04546(5) 0.04779(15) Uani 1 1 d . . . N1 N 1.2650(3) 0.2229(3) 1.31256(17) 0.0556(6) Uani 1 1 d . . . N2 N 1.6228(3) 0.2797(2) 1.10962(17) 0.0515(5) Uani 1 1 d . . . O1 O 1.6158(3) 0.4681(2) 1.29863(16) 0.0683(6) Uani 1 1 d . . . O2 O 1.3347(3) 0.3964(2) 1.12914(16) 0.0604(5) Uani 1 1 d . . . C1 C 1.1227(4) 0.2352(4) 1.2795(2) 0.0702(9) Uani 1 1 d . . . H1 H 1.0979 0.2574 1.2196 0.084 Uiso 1 1 d R . . C2 C 1.0069(5) 0.2167(4) 1.3292(3) 0.0760(9) Uani 1 1 d . . . H2 H 0.9084 0.2268 1.3026 0.091 Uiso 1 1 d R . . C3 C 1.0399(4) 0.1844(3) 1.4155(3) 0.0682(9) Uani 1 1 d . . . H3 H 0.9637 0.1714 1.4491 0.082 Uiso 1 1 d R . . C4 C 1.1911(4) 0.1702(3) 1.4555(2) 0.0581(7) Uani 1 1 d . . . C5 C 1.2353(6) 0.1387(3) 1.5460(2) 0.0726(10) Uani 1 1 d . . . H5 H 1.1623 0.1238 1.5819 0.087 Uiso 1 1 d R . . C6 C 1.3830(6) 0.1299(4) 1.5812(2) 0.0786(11) Uani 1 1 d . . . H6 H 1.4107 0.1094 1.6415 0.094 Uiso 1 1 d R . . C7 C 1.4958(5) 0.1512(3) 1.5287(2) 0.0676(8) Uani 1 1 d . . . H7 H 1.5968 0.1443 1.5544 0.081 Uiso 1 1 d R . . C8 C 1.4585(4) 0.1820(3) 1.43982(18) 0.0518(6) Uani 1 1 d . . . C9 C 1.3037(4) 0.1918(3) 1.40040(18) 0.0489(6) Uani 1 1 d . . . C10 C 1.7506(4) 0.3853(4) 1.4237(3) 0.0742(9) Uani 1 1 d . . . H10A H 1.7941 0.3979 1.4922 0.089 Uiso 1 1 d R . . H10B H 1.8465 0.4086 1.4001 0.089 Uiso 1 1 d R . . C11 C 1.6739(5) 0.4813(4) 1.3986(3) 0.0760(10) Uani 1 1 d . . . H11A H 1.5798 0.4616 1.4232 0.091 Uiso 1 1 d R . . H11B H 1.7582 0.5728 1.4267 0.091 Uiso 1 1 d R . . C12 C 1.5381(6) 0.5531(4) 1.2686(3) 0.0868(11) Uani 1 1 d . . . H12A H 1.6194 0.6466 1.2924 0.104 Uiso 1 1 d R . . H12B H 1.4438 0.5351 1.2928 0.104 Uiso 1 1 d R . . C13 C 1.4756(5) 0.5267(3) 1.1619(3) 0.0796(10) Uani 1 1 d . . . H13A H 1.4407 0.5947 1.1394 0.096 Uiso 1 1 d R . . H13B H 1.5659 0.5304 1.1377 0.096 Uiso 1 1 d R . . C14 C 1.2857(4) 0.3555(3) 1.0301(2) 0.0578(7) Uani 1 1 d . . . H14A H 1.3846 0.3679 1.0117 0.069 Uiso 1 1 d R . . H14B H 1.2354 0.4101 0.9976 0.069 Uiso 1 1 d R . . C15 C 1.1595(4) 0.2103(3) 1.0025(2) 0.0574(7) Uani 1 1 d . . . H15A H 1.1142 0.1876 0.9339 0.069 Uiso 1 1 d R . . H15B H 1.0659 0.1989 1.0260 0.069 Uiso 1 1 d R . . C16 C 1.3868(4) 0.1142(3) 0.98162(18) 0.0477(6) Uani 1 1 d . . . C17 C 1.3245(5) 0.0401(3) 0.8919(2) 0.0657(8) Uani 1 1 d . . . H17 H 1.2099 -0.0196 0.8676 0.079 Uiso 1 1 d R . . C18 C 1.4289(7) 0.0522(4) 0.8363(3) 0.0828(12) Uani 1 1 d . . . H18 H 1.3839 0.0003 0.7759 0.099 Uiso 1 1 d R . . C19 C 1.5940(6) 0.1383(4) 0.8697(3) 0.0768(11) Uani 1 1 d . . . H19 H 1.6627 0.1459 0.8320 0.092 Uiso 1 1 d R . . C20 C 1.6658(4) 0.2181(3) 0.9620(2) 0.0614(8) Uani 1 1 d . . . C21 C 1.8362(5) 0.3117(4) 0.9992(3) 0.0783(11) Uani 1 1 d . . . H21 H 1.9083 0.3235 0.9630 0.094 Uiso 1 1 d R . . C22 C 1.8967(4) 0.3848(4) 1.0869(4) 0.0824(12) Uani 1 1 d . . . H22 H 2.0105 0.4464 1.1118 0.099 Uiso 1 1 d R . . C23 C 1.7835(4) 0.3667(4) 1.1418(3) 0.0676(8) Uani 1 1 d . . . H23 H 1.8258 0.4184 1.2021 0.081 Uiso 1 1 d R . . C24 C 1.5609(4) 0.2057(3) 1.02030(19) 0.0473(6) Uani 1 1 d . . . Cl1 Cl 1.95389(13) 0.22417(15) 1.71797(7) 0.1004(4) Uani 1 1 d D . . O6 O 1.7974(5) 0.1191(5) 1.7114(3) 0.1466(16) Uani 1 1 d D A . O5 O 2.1053(16) 0.2882(16) 1.7842(9) 0.231(9) Uani 0.50 1 d PDU A 1 O4 O 1.8987(17) 0.3303(14) 1.7247(15) 0.280(10) Uani 0.50 1 d PDU A 1 O3 O 1.957(3) 0.226(2) 1.6287(9) 0.203(10) Uani 0.50 1 d PDU A 1 O5' O 2.0712(11) 0.1576(12) 1.7393(7) 0.139(3) Uani 0.50 1 d PDU A 2 O4' O 1.9974(14) 0.3109(7) 1.7993(5) 0.105(3) Uani 0.50 1 d PDU A 2 O3' O 1.9614(17) 0.2881(19) 1.6427(8) 0.151(7) Uani 0.50 1 d PDU A 2 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 0.07364(16) 0.05949(14) 0.04071(12) 0.01160(9) 0.02473(10) 0.03524(11) S1 0.0648(4) 0.0751(5) 0.0465(4) 0.0086(3) 0.0161(3) 0.0427(4) S2 0.0477(3) 0.0518(3) 0.0484(3) 0.0127(3) 0.0199(3) 0.0229(3) N1 0.0615(14) 0.0736(15) 0.0443(12) 0.0171(11) 0.0230(10) 0.0368(12) N2 0.0473(12) 0.0582(13) 0.0563(13) 0.0200(11) 0.0220(10) 0.0257(10) O1 0.0844(15) 0.0553(12) 0.0628(13) 0.0025(10) 0.0239(11) 0.0291(11) O2 0.0716(13) 0.0551(11) 0.0661(13) 0.0188(10) 0.0321(10) 0.0314(10) C1 0.0676(19) 0.103(3) 0.0570(18) 0.0234(18) 0.0265(15) 0.0489(19) C2 0.064(2) 0.102(3) 0.074(2) 0.014(2) 0.0302(17) 0.044(2) C3 0.0644(19) 0.0685(19) 0.077(2) 0.0045(16) 0.0417(17) 0.0229(15) C4 0.079(2) 0.0452(14) 0.0489(15) 0.0037(11) 0.0334(14) 0.0178(13) C5 0.108(3) 0.0578(17) 0.0539(18) 0.0120(14) 0.0449(19) 0.0261(18) C6 0.132(3) 0.068(2) 0.0397(15) 0.0186(14) 0.0338(19) 0.042(2) C7 0.098(2) 0.0635(18) 0.0414(15) 0.0092(13) 0.0139(15) 0.0413(18) C8 0.0713(17) 0.0502(14) 0.0370(13) 0.0064(10) 0.0174(12) 0.0296(13) C9 0.0634(16) 0.0458(13) 0.0412(13) 0.0064(10) 0.0235(12) 0.0231(12) C10 0.0564(18) 0.090(2) 0.0563(18) -0.0014(17) 0.0095(14) 0.0200(17) C11 0.080(2) 0.0639(19) 0.065(2) -0.0104(16) 0.0223(17) 0.0171(17) C12 0.113(3) 0.0533(18) 0.094(3) -0.0006(18) 0.030(2) 0.039(2) C13 0.102(3) 0.0495(17) 0.091(3) 0.0236(17) 0.030(2) 0.0365(18) C14 0.0637(17) 0.0695(18) 0.0655(18) 0.0316(15) 0.0310(14) 0.0446(15) C15 0.0521(15) 0.0718(18) 0.0597(17) 0.0190(14) 0.0179(13) 0.0371(14) C16 0.0621(15) 0.0566(14) 0.0413(13) 0.0187(11) 0.0247(11) 0.0357(13) C17 0.097(2) 0.0662(18) 0.0445(15) 0.0137(13) 0.0264(15) 0.0434(18) C18 0.143(4) 0.087(3) 0.0531(19) 0.0257(18) 0.054(2) 0.068(3) C19 0.137(3) 0.094(3) 0.069(2) 0.050(2) 0.075(2) 0.087(3) C20 0.080(2) 0.0778(19) 0.078(2) 0.0502(17) 0.0553(17) 0.0609(18) C21 0.080(2) 0.102(3) 0.109(3) 0.067(3) 0.064(2) 0.067(2) C22 0.0455(16) 0.089(3) 0.128(4) 0.061(3) 0.036(2) 0.0335(17) C23 0.0509(16) 0.0697(19) 0.081(2) 0.0291(17) 0.0191(15) 0.0252(15) C24 0.0636(16) 0.0591(15) 0.0493(14) 0.0284(12) 0.0337(12) 0.0434(13) Cl1 0.0725(6) 0.1385(10) 0.0578(5) -0.0063(6) 0.0235(5) 0.0162(6) O6 0.128(3) 0.134(3) 0.140(4) 0.007(3) 0.056(3) 0.015(3) O5 0.153(10) 0.220(15) 0.145(11) 0.080(11) -0.046(9) -0.033(10) O4 0.163(12) 0.257(18) 0.30(2) -0.123(16) -0.005(14) 0.047(12) O3 0.195(13) 0.38(3) 0.091(7) 0.022(10) 0.072(8) 0.168(16) O5' 0.116(6) 0.231(10) 0.133(7) 0.045(7) 0.053(5) 0.126(7) O4' 0.130(7) 0.084(4) 0.065(4) -0.013(3) 0.024(4) 0.018(5) O3' 0.104(6) 0.273(17) 0.078(6) 0.089(9) 0.045(5) 0.067(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.444(2) . ? Ag1 N2 2.512(2) . ? Ag1 S2 2.5412(8) . ? Ag1 S1 2.5595(8) . ? Ag1 O1 2.646(2) . ? Ag1 O2 2.752(2) . ? S1 C8 1.776(3) . ? S1 C10 1.822(4) . ? S2 C16 1.772(3) . ? S2 C15 1.821(3) . ? N1 C1 1.318(4) . ? N1 C9 1.360(4) . ? N2 C23 1.312(4) . ? N2 C24 1.367(4) . ? O1 C12 1.413(5) . ? O1 C11 1.417(4) . ? O2 C14 1.411(4) . ? O2 C13 1.430(4) . ? C1 C2 1.400(5) . ? C2 C3 1.340(5) . ? C3 C4 1.418(5) . ? C4 C5 1.404(5) . ? C4 C9 1.432(4) . ? C5 C6 1.347(6) . ? C6 C7 1.406(5) . ? C7 C8 1.371(4) . ? C8 C9 1.421(4) . ? C10 C11 1.501(6) . ? C12 C13 1.504(6) . ? C14 C15 1.499(5) . ? C16 C17 1.372(4) . ? C16 C24 1.417(4) . ? C17 C18 1.390(5) . ? C18 C19 1.339(6) . ? C19 C20 1.421(5) . ? C20 C21 1.397(6) . ? C20 C24 1.426(3) . ? C21 C22 1.343(6) . ? C22 C23 1.439(5) . ? Cl1 O5 1.331(9) . ? Cl1 O3 1.339(11) . ? Cl1 O3' 1.358(9) . ? Cl1 O4' 1.364(6) . ? Cl1 O6 1.397(4) . ? Cl1 O4 1.461(12) . ? Cl1 O5' 1.502(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N2 161.95(9) . . ? N1 Ag1 S2 110.10(6) . . ? N2 Ag1 S2 74.67(6) . . ? N1 Ag1 S1 75.77(6) . . ? N2 Ag1 S1 109.44(6) . . ? S2 Ag1 S1 149.23(3) . . ? N1 Ag1 O1 81.00(8) . . ? N2 Ag1 O1 83.85(8) . . ? S2 Ag1 O1 135.83(6) . . ? S1 Ag1 O1 74.32(6) . . ? N1 Ag1 O2 83.54(7) . . ? N2 Ag1 O2 81.02(7) . . ? S2 Ag1 O2 74.68(5) . . ? S1 Ag1 O2 135.78(5) . . ? O1 Ag1 O2 64.01(7) . . ? C8 S1 C10 101.05(15) . . ? C8 S1 Ag1 101.05(10) . . ? C10 S1 Ag1 102.19(12) . . ? C16 S2 C15 100.11(13) . . ? C16 S2 Ag1 103.06(10) . . ? C15 S2 Ag1 102.00(11) . . ? C1 N1 C9 118.7(3) . . ? C1 N1 Ag1 122.2(2) . . ? C9 N1 Ag1 118.20(18) . . ? C23 N2 C24 118.5(3) . . ? C23 N2 Ag1 123.2(2) . . ? C24 N2 Ag1 117.44(17) . . ? C12 O1 C11 113.0(3) . . ? C12 O1 Ag1 114.2(2) . . ? C11 O1 Ag1 112.3(2) . . ? C14 O2 C13 112.1(3) . . ? C14 O2 Ag1 106.86(15) . . ? C13 O2 Ag1 107.98(19) . . ? N1 C1 C2 123.8(3) . . ? C3 C2 C1 119.2(3) . . ? C2 C3 C4 119.9(3) . . ? C5 C4 C3 123.1(3) . . ? C5 C4 C9 119.4(3) . . ? C3 C4 C9 117.5(3) . . ? C6 C5 C4 120.4(3) . . ? C5 C6 C7 121.2(3) . . ? C8 C7 C6 120.7(3) . . ? C7 C8 C9 119.6(3) . . ? C7 C8 S1 118.2(3) . . ? C9 C8 S1 122.3(2) . . ? N1 C9 C8 120.4(2) . . ? N1 C9 C4 120.9(3) . . ? C8 C9 C4 118.7(3) . . ? C11 C10 S1 115.4(2) . . ? O1 C11 C10 109.2(3) . . ? O1 C12 C13 108.3(3) . . ? O2 C13 C12 108.7(3) . . ? O2 C14 C15 109.5(2) . . ? C14 C15 S2 115.5(2) . . ? C17 C16 C24 120.3(3) . . ? C17 C16 S2 117.6(2) . . ? C24 C16 S2 122.1(2) . . ? C16 C17 C18 121.5(4) . . ? C19 C18 C17 120.1(3) . . ? C18 C19 C20 120.9(3) . . ? C21 C20 C19 123.1(3) . . ? C21 C20 C24 117.2(3) . . ? C19 C20 C24 119.6(3) . . ? C22 C21 C20 120.5(3) . . ? C21 C22 C23 119.2(3) . . ? N2 C23 C22 122.3(4) . . ? N2 C24 C16 120.3(2) . . ? N2 C24 C20 122.2(3) . . ? C16 C24 C20 117.4(3) . . ? O5 Cl1 O3 114.6(13) . . ? O5 Cl1 O3' 106.8(9) . . ? O3 Cl1 O3' 29.5(14) . . ? O5 Cl1 O4' 51.8(9) . . ? O3 Cl1 O4' 139.8(11) . . ? O3' Cl1 O4' 111.7(9) . . ? O5 Cl1 O6 136.1(6) . . ? O3 Cl1 O6 105.5(11) . . ? O3' Cl1 O6 116.9(7) . . ? O4' Cl1 O6 105.3(5) . . ? O5 Cl1 O4 97.0(10) . . ? O3 Cl1 O4 96.8(11) . . ? O3' Cl1 O4 69.2(12) . . ? O4' Cl1 O4 55.4(7) . . ? O6 Cl1 O4 95.1(7) . . ? O5 Cl1 O5' 60.5(9) . . ? O3 Cl1 O5' 92.2(9) . . ? O3' Cl1 O5' 113.9(7) . . ? O4' Cl1 O5' 105.6(6) . . ? O6 Cl1 O5' 102.3(5) . . ? O4 Cl1 O5' 157.4(7) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.551 _refine_diff_density_min -0.863 _refine_diff_density_rms 0.055 #====================================================================END data_complex3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H48 Ag4 N8 O16 S4' _chemical_formula_weight 1552.66 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 Orthorhombic _symmetry_space_group_name_H-M Pcab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x+1/2, -y, -z+1/2' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x-1/2, y, z-1/2' 'x-1/2, -y-1/2, z' _cell_length_a 14.981(4) _cell_length_b 16.923(4) _cell_length_c 21.999(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5577(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 7 _cell_measurement_theta_max 15 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.849 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3088 _exptl_absorpt_coefficient_mu 1.608 _exptl_absorpt_correction_type 'Semi-empirical based on psi-scan' _exptl_absorpt_correction_T_min 0.553 _exptl_absorpt_correction_T_max 0.746 _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 'Siemens R3m' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 5641 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5458 _reflns_number_gt 3331 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+9.9252P] 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 5458 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1000 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1238 _refine_ls_wR_factor_gt 0.1035 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.85414(4) 0.01590(3) 0.00429(2) 0.06222(17) Uani 1 d . . . Ag2 Ag 1.00196(4) -0.11252(4) -0.17825(3) 0.0801(2) Uani 1 d . . . S1 S 0.88909(11) -0.01706(9) -0.11375(7) 0.0579(4) Uani 1 d . . . S2 S 0.86760(11) 0.04344(9) 0.12371(7) 0.0560(4) Uani 1 d . . . N1 N 0.8513(4) 0.1369(3) -0.0440(2) 0.0619(13) Uani 1 d . . . N2 N 0.8970(4) -0.1037(3) 0.0486(2) 0.0590(13) Uani 1 d . . . C1 C 0.8354(5) 0.2006(4) -0.0110(3) 0.080(2) Uani 1 d . . . H1A H 0.8291 0.1936 0.0321 0.080 Uiso 1 d R . . C2 C 0.8275(5) 0.2759(4) -0.0345(4) 0.086(2) Uani 1 d . . . H2A H 0.8158 0.3197 -0.0079 0.080 Uiso 1 d R . . C3 C 0.8363(5) 0.2866(4) -0.0950(4) 0.080(2) Uani 1 d . . . H3A H 0.8296 0.3385 -0.1121 0.080 Uiso 1 d R . . C4 C 0.8554(4) 0.2218(4) -0.1332(3) 0.0626(16) Uani 1 d . . . C5 C 0.8670(5) 0.2301(4) -0.1961(3) 0.074(2) Uani 1 d . . . H5A H 0.8610 0.2812 -0.2147 0.080 Uiso 1 d R . . C6 C 0.8864(5) 0.1670(4) -0.2307(3) 0.078(2) Uani 1 d . . . H6A H 0.8956 0.1734 -0.2736 0.080 Uiso 1 d R . . C7 C 0.8931(5) 0.0916(4) -0.2043(3) 0.0645(17) Uani 1 d . . . H7A H 0.9067 0.0470 -0.2297 0.080 Uiso 1 d R . . C8 C 0.8811(4) 0.0801(3) -0.1437(3) 0.0529(15) Uani 1 d . . . C9 C 0.8629(4) 0.1458(3) -0.1057(3) 0.0488(13) Uani 1 d . . . C10 C 0.7858(5) -0.0617(4) -0.1383(3) 0.0710(18) Uani 1 d . . . H10A H 0.7858 -0.1159 -0.1255 0.100 Uiso 1 d R . . H10B H 0.7848 -0.0614 -0.1820 0.100 Uiso 1 d R . . C11 C 0.7045(5) -0.0249(5) -0.1153(3) 0.085(2) Uani 1 d . . . H11A H 0.6531 -0.0511 -0.1319 0.100 Uiso 1 d R . . H11B H 0.7030 0.0295 -0.1276 0.100 Uiso 1 d R . . C12 C 0.6299(6) 0.0118(8) -0.0287(5) 0.155(5) Uani 1 d . . . H12A H 0.6362 0.0633 -0.0465 0.100 Uiso 1 d R . . H12B H 0.5762 -0.0112 -0.0448 0.100 Uiso 1 d R . . C13 C 0.6224(6) 0.0279(7) 0.0280(5) 0.135(4) Uani 1 d . . . H13A H 0.6128 -0.0230 0.0461 0.100 Uiso 1 d R . . H13B H 0.5708 0.0599 0.0360 0.100 Uiso 1 d R . . C14 C 0.6868(5) 0.0486(5) 0.1214(4) 0.097(3) Uani 1 d . . . H14A H 0.6332 0.0732 0.1360 0.100 Uiso 1 d R . . H14B H 0.6835 -0.0068 0.1302 0.100 Uiso 1 d R . . C15 C 0.7629(4) 0.0824(4) 0.1513(3) 0.0695(19) Uani 1 d . . . H15A H 0.7623 0.1386 0.1454 0.100 Uiso 1 d R . . H15B H 0.7588 0.0725 0.1942 0.100 Uiso 1 d R . . C16 C 0.8679(4) -0.0555(3) 0.1503(2) 0.0495(14) Uani 1 d . . . C17 C 0.8563(5) -0.0714(4) 0.2107(3) 0.0671(17) Uani 1 d . . . H17A H 0.8465 -0.0281 0.2381 0.100 Uiso 1 d R . . C18 C 0.8607(5) -0.1488(4) 0.2334(3) 0.076(2) Uani 1 d . . . H18A H 0.8492 -0.1586 0.2757 0.100 Uiso 1 d R . . C19 C 0.8784(5) -0.2090(4) 0.1953(3) 0.075(2) Uani 1 d . . . H19A H 0.8821 -0.2617 0.2112 0.100 Uiso 1 d R . . C20 C 0.8917(4) -0.1963(3) 0.1327(3) 0.0573(15) Uani 1 d . . . C21 C 0.9127(5) -0.2571(4) 0.0923(3) 0.081(2) Uani 1 d . . . H21A H 0.9175 -0.3102 0.1072 0.100 Uiso 1 d R . . C22 C 0.9250(6) -0.2414(4) 0.0331(3) 0.087(2) Uani 1 d . . . H22A H 0.9400 -0.2828 0.0050 0.100 Uiso 1 d R . . C23 C 0.9167(5) -0.1640(4) 0.0131(3) 0.081(2) Uani 1 d . . . H23A H 0.9263 -0.1531 -0.0292 0.100 Uiso 1 d R . . C24 C 0.8863(4) -0.1183(3) 0.1092(3) 0.0505(14) Uani 1 d . . . O1 O 0.7036(3) -0.0309(3) -0.0506(2) 0.0862(15) Uani 1 d . . . O2 O 0.6945(3) 0.0618(4) 0.0565(2) 0.1022(19) Uani 1 d . . . N3 N 1.0216(5) -0.2719(4) -0.1267(3) 0.0795(19) Uani 1 d . . . O3 O 0.9506(4) -0.2345(3) -0.1355(3) 0.0974(17) Uani 1 d . . . O4 O 1.0931(4) -0.2405(3) -0.1412(3) 0.1079(19) Uani 1 d . . . O5 O 1.0208(4) -0.3377(4) -0.1057(4) 0.134(3) Uani 1 d . . . N4 N 0.9938(5) -0.0828(3) -0.3082(3) 0.0765(18) Uani 1 d . . . O6 O 0.9258(4) -0.0826(3) -0.2753(2) 0.0994(18) Uani 1 d . . . O7 O 1.0685(4) -0.0947(3) -0.2845(3) 0.1001(18) Uani 1 d . . . O8 O 0.9880(4) -0.0730(3) -0.3634(2) 0.1028(19) Uani 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 0.0708(3) 0.0654(3) 0.0505(3) 0.0053(2) -0.0028(3) 0.0030(3) Ag2 0.0989(4) 0.0696(3) 0.0717(3) 0.0000(3) -0.0071(3) -0.0064(3) S1 0.0654(10) 0.0538(8) 0.0545(8) -0.0014(8) 0.0040(8) 0.0037(8) S2 0.0671(10) 0.0511(8) 0.0499(8) -0.0037(7) -0.0002(8) 0.0045(7) N1 0.078(4) 0.056(3) 0.051(3) -0.003(2) 0.008(3) -0.004(3) N2 0.071(4) 0.059(3) 0.047(3) -0.007(2) -0.004(3) 0.016(3) C1 0.108(6) 0.062(4) 0.069(4) -0.012(4) 0.021(4) -0.007(4) C2 0.106(7) 0.058(5) 0.096(6) -0.021(4) 0.026(5) -0.002(4) C3 0.080(5) 0.046(4) 0.115(6) 0.004(4) 0.005(5) 0.002(3) C4 0.049(4) 0.056(4) 0.083(5) 0.003(3) 0.001(4) -0.008(3) C5 0.079(5) 0.065(5) 0.079(5) 0.024(4) -0.011(4) -0.010(4) C6 0.099(6) 0.080(5) 0.056(4) 0.013(4) -0.003(4) -0.014(4) C7 0.078(5) 0.072(5) 0.043(3) -0.006(3) 0.000(3) -0.004(4) C8 0.053(4) 0.055(3) 0.051(3) 0.001(3) 0.003(3) -0.006(3) C9 0.037(3) 0.052(3) 0.057(3) 0.002(3) 0.004(3) 0.000(3) C10 0.080(5) 0.068(4) 0.065(4) -0.008(3) -0.002(4) -0.011(4) C11 0.076(5) 0.088(5) 0.090(5) 0.000(5) -0.029(4) -0.019(4) C12 0.050(6) 0.298(17) 0.116(8) -0.069(10) -0.001(5) -0.009(7) C13 0.058(6) 0.196(11) 0.150(9) -0.057(9) 0.011(6) 0.021(7) C14 0.080(6) 0.100(6) 0.112(7) -0.017(5) 0.025(5) 0.011(5) C15 0.070(5) 0.075(4) 0.064(4) -0.002(3) 0.008(4) 0.023(4) C16 0.048(3) 0.051(3) 0.050(3) -0.001(3) 0.000(3) 0.004(3) C17 0.082(5) 0.065(4) 0.055(4) -0.002(3) 0.005(4) 0.010(4) C18 0.093(5) 0.073(5) 0.062(4) 0.012(4) 0.006(4) 0.006(4) C19 0.092(6) 0.060(4) 0.075(5) 0.017(4) -0.014(4) 0.002(4) C20 0.058(4) 0.054(4) 0.060(4) 0.000(3) -0.010(3) 0.007(3) C21 0.102(6) 0.055(4) 0.085(5) -0.002(4) -0.019(5) 0.010(4) C22 0.131(7) 0.058(5) 0.072(5) -0.021(4) -0.005(5) 0.018(5) C23 0.113(6) 0.069(5) 0.059(4) -0.012(4) -0.001(4) 0.024(4) C24 0.044(3) 0.053(3) 0.054(3) -0.002(3) -0.009(3) 0.005(3) O1 0.068(3) 0.128(4) 0.063(3) -0.017(3) 0.004(2) -0.022(3) O2 0.053(3) 0.168(6) 0.086(4) -0.035(4) -0.006(3) 0.007(3) N3 0.119(7) 0.056(4) 0.064(4) -0.006(3) 0.000(4) -0.009(4) O3 0.112(5) 0.076(4) 0.105(4) -0.007(3) 0.000(4) 0.001(3) O4 0.113(5) 0.084(4) 0.126(5) -0.014(4) 0.018(4) -0.030(4) O5 0.141(6) 0.071(4) 0.191(7) 0.038(4) 0.027(5) 0.002(4) N4 0.120(6) 0.046(3) 0.063(4) -0.009(3) -0.006(4) 0.003(4) O6 0.136(5) 0.076(4) 0.086(4) -0.014(3) 0.026(4) -0.001(3) O7 0.122(5) 0.092(4) 0.086(4) -0.002(3) -0.026(4) 0.006(4) O8 0.141(5) 0.104(4) 0.063(3) 0.008(3) 0.003(3) 0.023(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.308(5) . ? Ag1 N2 2.336(5) . ? Ag1 S2 2.6757(17) . ? Ag1 S1 2.7071(17) . ? Ag2 O3 2.396(6) . ? Ag2 O6 2.473(6) . ? Ag2 O7 2.558(6) . ? Ag2 S2 2.5739(17) 5_755 ? Ag2 S1 2.7354(17) . ? S1 C8 1.775(6) . ? S1 C10 1.804(7) . ? S2 C16 1.775(6) . ? S2 C15 1.806(6) . ? S2 Ag2 2.5739(17) 5_755 ? N1 C1 1.322(8) . ? N1 C9 1.378(7) . ? N2 C23 1.319(7) . ? N2 C24 1.366(7) . ? C1 C2 1.380(10) . ? C2 C3 1.349(10) . ? C3 C4 1.412(9) . ? C4 C5 1.403(9) . ? C4 C9 1.424(8) . ? C5 C6 1.343(9) . ? C6 C7 1.406(9) . ? C7 C8 1.360(8) . ? C8 C9 1.416(7) . ? C10 C11 1.458(9) . ? C11 O1 1.428(8) . ? C12 C13 1.283(13) . ? C12 O1 1.404(10) . ? C13 O2 1.374(10) . ? C14 C15 1.434(10) . ? C14 O2 1.451(9) . ? C16 C17 1.365(8) . ? C16 C24 1.422(7) . ? C17 C18 1.404(9) . ? C18 C19 1.346(9) . ? C19 C20 1.407(9) . ? C20 C21 1.396(8) . ? C20 C24 1.419(8) . ? C21 C22 1.343(9) . ? C22 C23 1.388(9) . ? N3 O5 1.206(8) . ? N3 O4 1.237(7) . ? N3 O3 1.252(8) . ? N4 O8 1.230(7) . ? N4 O6 1.249(8) . ? N4 O7 1.251(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N2 165.00(19) . . ? N1 Ag1 S2 107.38(12) . . ? N2 Ag1 S2 73.76(12) . . ? N1 Ag1 S1 75.21(12) . . ? N2 Ag1 S1 99.72(12) . . ? S2 Ag1 S1 164.39(6) . . ? O3 Ag2 O6 111.55(19) . . ? O3 Ag2 O7 125.81(18) . . ? O6 Ag2 O7 50.7(2) . . ? O3 Ag2 S2 116.88(15) . 5_755 ? O6 Ag2 S2 131.28(14) . 5_755 ? O7 Ag2 S2 94.40(14) . 5_755 ? O3 Ag2 S1 96.13(15) . . ? O6 Ag2 S1 92.40(14) . . ? O7 Ag2 S1 130.18(13) . . ? S2 Ag2 S1 87.66(6) 5_755 . ? C8 S1 C10 102.7(3) . . ? C8 S1 Ag1 98.72(19) . . ? C10 S1 Ag1 102.0(2) . . ? C8 S1 Ag2 113.4(2) . . ? C10 S1 Ag2 97.3(2) . . ? Ag1 S1 Ag2 137.63(6) . . ? C16 S2 C15 103.6(3) . . ? C16 S2 Ag2 105.86(19) . 5_755 ? C15 S2 Ag2 109.7(2) . 5_755 ? C16 S2 Ag1 99.20(19) . . ? C15 S2 Ag1 109.1(2) . . ? Ag2 S2 Ag1 126.44(7) 5_755 . ? C1 N1 C9 118.4(5) . . ? C1 N1 Ag1 118.3(4) . . ? C9 N1 Ag1 123.3(4) . . ? C23 N2 C24 117.6(5) . . ? C23 N2 Ag1 119.0(4) . . ? C24 N2 Ag1 122.2(4) . . ? N1 C1 C2 124.2(7) . . ? C3 C2 C1 119.0(7) . . ? C2 C3 C4 120.2(7) . . ? C5 C4 C3 122.3(6) . . ? C5 C4 C9 119.9(6) . . ? C3 C4 C9 117.7(6) . . ? C6 C5 C4 120.4(6) . . ? C5 C6 C7 120.2(6) . . ? C8 C7 C6 121.7(6) . . ? C7 C8 C9 119.4(6) . . ? C7 C8 S1 119.1(5) . . ? C9 C8 S1 121.5(4) . . ? N1 C9 C8 121.3(5) . . ? N1 C9 C4 120.4(5) . . ? C8 C9 C4 118.3(5) . . ? C11 C10 S1 115.7(5) . . ? O1 C11 C10 108.9(6) . . ? C13 C12 O1 120.7(10) . . ? C12 C13 O2 117.7(9) . . ? C15 C14 O2 109.0(7) . . ? C14 C15 S2 113.0(5) . . ? C17 C16 C24 119.8(5) . . ? C17 C16 S2 120.4(5) . . ? C24 C16 S2 119.7(4) . . ? C16 C17 C18 121.6(6) . . ? C19 C18 C17 119.6(6) . . ? C18 C19 C20 121.4(6) . . ? C21 C20 C19 122.8(6) . . ? C21 C20 C24 117.8(6) . . ? C19 C20 C24 119.4(6) . . ? C22 C21 C20 120.3(7) . . ? C21 C22 C23 118.7(7) . . ? N2 C23 C22 124.3(6) . . ? N2 C24 C20 121.2(5) . . ? N2 C24 C16 120.5(5) . . ? C20 C24 C16 118.3(5) . . ? C12 O1 C11 108.2(7) . . ? C13 O2 C14 108.8(7) . . ? O5 N3 O4 120.3(8) . . ? O5 N3 O3 121.1(8) . . ? O4 N3 O3 118.6(7) . . ? N3 O3 Ag2 102.9(5) . . ? O8 N4 O6 120.9(7) . . ? O8 N4 O7 119.8(7) . . ? O6 N4 O7 119.2(7) . . ? N4 O6 Ag2 97.1(5) . . ? N4 O7 Ag2 92.9(5) . . ? _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.905 _refine_diff_density_max 0.582 _refine_diff_density_min -0.555 _refine_diff_density_rms 0.080 #================================================================END data_complex4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H46 Ag4 N8 O16 S4' _chemical_formula_weight 1526.63 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 Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.211(3) _cell_length_b 14.572(3) _cell_length_c 21.810(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5469.9(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used CCD _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.854 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3032 _exptl_absorpt_coefficient_mu 1.638 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.756 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart CCD ' _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 35063 _diffrn_reflns_av_R_equivalents 0.0717 _diffrn_reflns_av_sigmaI/netI 0.0538 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 27.51 _reflns_number_total 6266 _reflns_number_gt 2426 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1039P)^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 6266 _refine_ls_number_parameters 353 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.1541 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.2264 _refine_ls_wR_factor_gt 0.1868 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.056 _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 0.0000 0.40608(4) 0.2500 0.08778(18) Uani 1 2 d S . . Ag2 Ag 0.0000 0.15014(5) 0.2500 0.0967(2) Uani 1 2 d SD . . Ag3 Ag 0.11052(3) 0.24442(4) 0.072328(19) 0.1243(2) Uani 1 1 d . . . S1 S 0.02925(6) 0.37173(11) 0.13148(5) 0.0878(4) Uani 1 1 d . . . N1 N -0.12139(18) 0.4172(2) 0.20117(14) 0.0714(11) Uani 1 1 d . . . O1 O 0.03928(18) 0.5614(2) 0.19148(13) 0.0922(11) Uani 1 1 d . . . C1 C -0.1830(2) 0.4406(3) 0.2335(2) 0.0835(15) Uani 1 1 d . . . H1 H -0.1761 0.4566 0.2744 0.100 Uiso 1 1 calc R . . C2 C -0.2577(3) 0.4425(3) 0.2096(2) 0.0925(16) Uani 1 1 d . . . H2 H -0.2997 0.4546 0.2351 0.111 Uiso 1 1 calc R . . C3 C -0.2693(2) 0.4270(3) 0.1492(2) 0.0810(15) Uani 1 1 d . . . H3 H -0.3188 0.4324 0.1324 0.097 Uiso 1 1 calc R . . C4 C -0.2062(2) 0.4026(3) 0.11209(18) 0.0669(13) Uani 1 1 d . . . C5 C -0.2156(2) 0.3828(3) 0.05020(18) 0.0784(15) Uani 1 1 d . . . H5 H -0.2646 0.3854 0.0324 0.094 Uiso 1 1 calc R . . C6 C -0.1527(3) 0.3596(3) 0.0159(2) 0.0845(15) Uani 1 1 d . . . H6 H -0.1590 0.3461 -0.0255 0.101 Uiso 1 1 calc R . . C7 C -0.0786(2) 0.3559(3) 0.04211(18) 0.0810(15) Uani 1 1 d . . . H7 H -0.0363 0.3379 0.0184 0.097 Uiso 1 1 calc R . . C8 C -0.0681(2) 0.3784(3) 0.10224(17) 0.0696(13) Uani 1 1 d . . . C9 C -0.1316(2) 0.3998(3) 0.13939(17) 0.0591(12) Uani 1 1 d . . . C10 C 0.0681(3) 0.4793(4) 0.1040(2) 0.1029(19) Uani 1 1 d . . . H10A H 0.1227 0.4823 0.1148 0.123 Uiso 1 1 calc R . . H10B H 0.0646 0.4800 0.0596 0.123 Uiso 1 1 calc R . . C11 C 0.0300(3) 0.5601(4) 0.1275(2) 0.107(2) Uani 1 1 d . . . H11A H 0.0529 0.6148 0.1096 0.128 Uiso 1 1 calc R . . H11B H -0.0248 0.5589 0.1170 0.128 Uiso 1 1 calc R . . C12 C 0.0007(4) 0.6373(5) 0.2139(3) 0.144(3) Uani 1 1 d . . . H12A H -0.0521 0.6376 0.1985 0.172 Uiso 1 1 calc R . . H12B H 0.0263 0.6926 0.1995 0.172 Uiso 1 1 calc R . . S1' S 0.02845(7) 0.11792(11) 0.13417(5) 0.1012(5) Uani 1 1 d D . . O2 O 0.0000 -0.0341(4) 0.2500 0.230(4) Uani 1 2 d SDU . . N1' N -0.1181(2) 0.1716(2) 0.20316(15) 0.0758(11) Uani 1 1 d . . . C1' C -0.1779(3) 0.1963(4) 0.2369(2) 0.0951(18) Uani 1 1 d . . . H1' H -0.1690 0.2130 0.2774 0.114 Uiso 1 1 calc R . . C2' C -0.2535(3) 0.1986(4) 0.2151(2) 0.1008(18) Uani 1 1 d . . . H2' H -0.2942 0.2140 0.2413 0.121 Uiso 1 1 calc R . . C3' C -0.2679(3) 0.1785(4) 0.1554(2) 0.1003(18) Uani 1 1 d . . . H3' H -0.3181 0.1814 0.1396 0.120 Uiso 1 1 calc R . . C4' C -0.2041(2) 0.1527(3) 0.11780(19) 0.0753(14) Uani 1 1 d . . . C5' C -0.2168(3) 0.1298(3) 0.0546(2) 0.0880(16) Uani 1 1 d . . . H5' H -0.2664 0.1328 0.0378 0.106 Uiso 1 1 calc R . . C6' C -0.1554(3) 0.1039(4) 0.0199(2) 0.0971(18) Uani 1 1 d . . . H6' H -0.1629 0.0884 -0.0210 0.117 Uiso 1 1 calc R . . C7' C -0.0821(3) 0.1005(3) 0.04477(19) 0.0851(15) Uani 1 1 d . . . H7' H -0.0412 0.0815 0.0200 0.102 Uiso 1 1 calc R . . C8' C -0.0664(2) 0.1237(3) 0.10440(18) 0.0707(13) Uani 1 1 d . . . C9' C -0.1306(2) 0.1492(3) 0.14294(18) 0.0645(13) Uani 1 1 d . . . C10' C 0.0446(4) -0.0115(3) 0.1364(3) 0.179(3) Uani 1 1 d DU . . H10C H 0.0030 -0.0419 0.1143 0.214 Uiso 1 1 calc R . . H10D H 0.0932 -0.0262 0.1162 0.214 Uiso 1 1 calc R . . C11' C 0.0467(3) -0.0468(4) 0.2023(2) 0.150(2) Uani 1 1 d DU . . H11C H 0.0494 -0.1130 0.1980 0.180 Uiso 1 1 calc R . . H11D H 0.0974 -0.0283 0.2172 0.180 Uiso 1 1 calc R . . N3 N 0.2699(2) 0.2760(3) 0.12084(18) 0.1020(15) Uani 1 1 d . . . O3 O 0.2377(2) 0.2030(3) 0.10675(19) 0.1280(15) Uani 1 1 d . . . O4 O 0.2289(3) 0.3429(3) 0.1134(2) 0.162(2) Uani 1 1 d . . . O5 O 0.3356(2) 0.2751(3) 0.1374(2) 0.161(2) Uani 1 1 d . . . N4 N 0.0829(2) 0.2183(3) -0.05835(15) 0.0740(11) Uani 1 1 d . . . O6 O 0.08808(19) 0.1494(3) -0.02673(16) 0.1070(13) Uani 1 1 d . . . O7 O 0.0906(2) 0.2959(3) -0.03380(16) 0.1040(13) Uani 1 1 d . . . O8 O 0.0715(2) 0.2156(3) -0.11413(14) 0.1086(13) Uani 1 1 d . . . O1W O 0.2206(8) 0.0211(8) 0.1439(7) 0.228(5) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0735(3) 0.1430(5) 0.0468(2) 0.000 -0.0050(2) 0.000 Ag2 0.0956(4) 0.1355(5) 0.0591(3) 0.000 -0.0020(3) 0.000 Ag3 0.0694(2) 0.2371(6) 0.0664(2) -0.0191(3) 0.00694(19) -0.0054(3) S1 0.0546(6) 0.1625(12) 0.0463(6) -0.0068(7) 0.0021(5) 0.0084(7) N1 0.0586(19) 0.101(3) 0.0550(18) -0.0122(18) 0.0087(15) 0.0032(19) O1 0.092(2) 0.114(2) 0.0705(19) -0.0055(17) 0.0080(17) 0.0039(19) C1 0.061(2) 0.108(3) 0.081(3) -0.022(3) 0.010(2) 0.005(3) C2 0.068(3) 0.112(3) 0.097(3) -0.030(3) 0.024(2) -0.006(3) C3 0.057(2) 0.082(3) 0.104(3) -0.011(3) 0.003(2) -0.001(2) C4 0.054(2) 0.076(3) 0.072(3) 0.004(2) 0.004(2) -0.015(2) C5 0.060(3) 0.104(3) 0.071(3) -0.002(3) -0.001(2) -0.012(2) C6 0.079(3) 0.112(4) 0.063(2) 0.008(3) -0.020(2) -0.024(3) C7 0.068(3) 0.121(4) 0.054(2) 0.001(2) 0.004(2) -0.005(3) C8 0.061(2) 0.097(3) 0.050(2) 0.008(2) 0.0014(19) 0.007(2) C9 0.058(2) 0.067(2) 0.053(2) 0.003(2) 0.0013(18) -0.007(2) C10 0.061(3) 0.194(5) 0.054(2) -0.001(3) 0.011(2) -0.012(3) C11 0.082(3) 0.177(5) 0.061(3) 0.031(3) 0.010(2) 0.003(3) C12 0.187(6) 0.144(5) 0.100(4) 0.008(4) -0.053(4) -0.009(5) S1' 0.0764(8) 0.1668(13) 0.0605(7) -0.0147(8) 0.0107(6) 0.0152(8) O2 0.234(6) 0.225(6) 0.233(6) 0.000 0.015(5) 0.000 N1' 0.082(2) 0.085(2) 0.060(2) 0.0032(19) 0.0170(18) 0.010(2) C1' 0.092(3) 0.119(4) 0.073(3) 0.001(3) 0.018(3) 0.012(3) C2' 0.083(3) 0.129(4) 0.091(3) -0.003(3) 0.031(3) 0.021(3) C3' 0.080(3) 0.125(4) 0.096(3) 0.020(3) 0.028(3) 0.024(3) C4' 0.069(3) 0.084(3) 0.073(3) 0.016(2) 0.007(2) 0.015(2) C5' 0.088(3) 0.098(3) 0.078(3) 0.014(3) -0.025(3) -0.006(3) C6' 0.091(3) 0.124(4) 0.076(3) -0.016(3) 0.012(3) 0.001(3) C7' 0.089(3) 0.109(3) 0.058(2) -0.019(3) 0.006(2) 0.017(3) C8' 0.066(3) 0.080(3) 0.066(2) -0.002(2) 0.012(2) -0.002(2) C9' 0.069(2) 0.073(3) 0.052(2) -0.002(2) 0.0057(19) 0.002(2) C10' 0.174(5) 0.193(5) 0.170(5) -0.085(4) -0.024(4) 0.049(4) C11' 0.185(4) 0.141(4) 0.125(4) -0.004(3) 0.033(4) 0.071(4) N3 0.058(2) 0.179(4) 0.070(2) 0.003(3) 0.0142(19) -0.020(2) O3 0.095(3) 0.150(3) 0.138(3) -0.009(3) 0.035(2) -0.007(2) O4 0.105(3) 0.173(4) 0.209(5) -0.018(4) -0.003(3) 0.027(3) O5 0.074(2) 0.269(5) 0.140(4) 0.036(3) -0.028(2) -0.028(3) N4 0.0521(18) 0.113(3) 0.0573(19) -0.011(2) 0.0004(16) -0.0055(19) O6 0.094(2) 0.136(3) 0.090(2) 0.025(2) 0.0143(19) 0.003(2) O7 0.094(2) 0.131(3) 0.087(2) -0.029(2) 0.0032(19) -0.003(2) O8 0.109(3) 0.155(3) 0.0623(19) -0.006(2) -0.0116(19) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.351(3) . ? Ag1 N1 2.351(3) 3 ? Ag1 S1 2.6807(12) . ? Ag1 S1 2.6807(12) 3 ? Ag1 O1 2.685(3) 3 ? Ag1 O1 2.685(3) . ? Ag2 N1' 2.297(3) . ? Ag2 N1' 2.297(3) 3 ? Ag2 S1' 2.6157(13) . ? Ag2 S1' 2.6157(13) 3 ? Ag2 O2 2.685(5) . ? Ag3 O3 2.392(4) . ? Ag3 O7 2.457(4) . ? Ag3 O6 2.595(4) . ? Ag3 O4 2.648(5) . ? Ag3 S1 2.6574(14) . ? Ag3 S1' 2.6856(16) . ? S1 C8 1.795(4) . ? S1 C10 1.806(5) . ? N1 C1 1.318(5) . ? N1 C9 1.383(5) . ? O1 C12 1.380(7) . ? O1 C11 1.405(5) . ? C1 C2 1.387(6) . ? C2 C3 1.351(7) . ? C3 C4 1.399(6) . ? C4 C5 1.390(5) . ? C4 C9 1.416(5) . ? C5 C6 1.359(6) . ? C6 C7 1.399(6) . ? C7 C8 1.364(5) . ? C8 C9 1.396(5) . ? C10 C11 1.442(7) . ? C12 C12 1.573(11) 3 ? S1' C8' 1.760(4) . ? S1' C10' 1.907(5) . ? O2 C11' 1.327(5) . ? O2 C11' 1.327(5) 3 ? N1' C1' 1.315(6) . ? N1' C9' 1.370(5) . ? C1' C2' 1.385(7) . ? C2' C3' 1.358(7) . ? C3' C4' 1.421(6) . ? C4' C9' 1.379(6) . ? C4' C5' 1.434(6) . ? C5' C6' 1.352(6) . ? C6' C7' 1.374(6) . ? C7' C8' 1.370(6) . ? C8' C9' 1.437(5) . ? C10' C11' 1.528(8) . ? N3 O5 1.188(5) . ? N3 O4 1.215(6) . ? N3 O3 1.238(6) . ? N4 O6 1.222(5) . ? N4 O8 1.233(4) . ? N4 O7 1.258(5) . ? 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 N1 172.08(17) . 3 ? N1 Ag1 S1 75.11(8) . . ? N1 Ag1 S1 106.43(8) 3 . ? N1 Ag1 S1 106.43(8) . 3 ? N1 Ag1 S1 75.11(8) 3 3 ? S1 Ag1 S1 158.48(7) . 3 ? N1 Ag1 O1 86.18(10) . 3 ? N1 Ag1 O1 87.15(11) 3 3 ? S1 Ag1 O1 131.54(7) . 3 ? S1 Ag1 O1 69.62(7) 3 3 ? N1 Ag1 O1 87.15(11) . . ? N1 Ag1 O1 86.18(10) 3 . ? S1 Ag1 O1 69.62(7) . . ? S1 Ag1 O1 131.54(7) 3 . ? O1 Ag1 O1 65.09(13) 3 . ? N1' Ag2 N1' 164.35(18) . 3 ? N1' Ag2 S1' 76.15(9) . . ? N1' Ag2 S1' 106.76(9) 3 . ? N1' Ag2 S1' 106.76(9) . 3 ? N1' Ag2 S1' 76.15(9) 3 3 ? S1' Ag2 S1' 159.32(8) . 3 ? N1' Ag2 O2 97.83(9) . . ? N1' Ag2 O2 97.83(9) 3 . ? S1' Ag2 O2 79.66(4) . . ? S1' Ag2 O2 79.66(4) 3 . ? O3 Ag3 O7 120.04(13) . . ? O3 Ag3 O6 105.24(12) . . ? O7 Ag3 O6 50.06(12) . . ? O3 Ag3 O4 47.67(15) . . ? O7 Ag3 O4 105.08(14) . . ? O6 Ag3 O4 133.25(13) . . ? O3 Ag3 S1 120.37(10) . . ? O7 Ag3 S1 99.82(9) . . ? O6 Ag3 S1 134.29(8) . . ? O4 Ag3 S1 82.09(10) . . ? O3 Ag3 S1' 98.65(10) . . ? O7 Ag3 S1' 127.54(9) . . ? O6 Ag3 S1' 88.49(8) . . ? O4 Ag3 S1' 127.37(11) . . ? S1 Ag3 S1' 87.62(5) . . ? C8 S1 C10 100.4(2) . . ? C8 S1 Ag3 110.90(14) . . ? C10 S1 Ag3 104.46(15) . . ? C8 S1 Ag1 99.04(13) . . ? C10 S1 Ag1 103.16(15) . . ? Ag3 S1 Ag1 134.21(5) . . ? C1 N1 C9 117.8(3) . . ? C1 N1 Ag1 119.4(3) . . ? C9 N1 Ag1 122.8(2) . . ? C12 O1 C11 108.0(4) . . ? C12 O1 Ag1 112.7(3) . . ? C11 O1 Ag1 115.6(3) . . ? N1 C1 C2 123.3(4) . . ? C3 C2 C1 120.0(4) . . ? C2 C3 C4 119.4(4) . . ? C5 C4 C3 121.6(4) . . ? C5 C4 C9 120.5(4) . . ? C3 C4 C9 117.9(4) . . ? C6 C5 C4 119.6(4) . . ? C5 C6 C7 120.7(4) . . ? C8 C7 C6 120.3(4) . . ? C7 C8 C9 120.5(4) . . ? C7 C8 S1 116.9(3) . . ? C9 C8 S1 122.5(3) . . ? N1 C9 C8 120.4(3) . . ? N1 C9 C4 121.3(3) . . ? C8 C9 C4 118.2(3) . . ? C11 C10 S1 115.0(3) . . ? O1 C11 C10 108.2(4) . . ? O1 C12 C12 111.3(4) . 3 ? C8' S1' C10' 101.0(3) . . ? C8' S1' Ag2 100.02(14) . . ? C10' S1' Ag2 100.4(2) . . ? C8' S1' Ag3 105.68(15) . . ? C10' S1' Ag3 128.0(2) . . ? Ag2 S1' Ag3 117.41(6) . . ? C11' O2 C11' 164.0(7) . 3 ? C11' O2 Ag2 98.0(4) . . ? C11' O2 Ag2 98.0(4) 3 . ? C1' N1' C9' 118.5(4) . . ? C1' N1' Ag2 118.8(3) . . ? C9' N1' Ag2 122.2(3) . . ? N1' C1' C2' 123.4(5) . . ? C3' C2' C1' 119.6(5) . . ? C2' C3' C4' 118.0(5) . . ? C9' C4' C3' 119.3(4) . . ? C9' C4' C5' 120.9(4) . . ? C3' C4' C5' 119.8(4) . . ? C6' C5' C4' 118.9(4) . . ? C5' C6' C7' 120.4(5) . . ? C8' C7' C6' 123.1(4) . . ? C7' C8' C9' 117.9(4) . . ? C7' C8' S1' 121.4(3) . . ? C9' C8' S1' 120.7(3) . . ? N1' C9' C4' 121.1(4) . . ? N1' C9' C8' 120.1(4) . . ? C4' C9' C8' 118.8(4) . . ? C11' C10' S1' 111.1(4) . . ? O2 C11' C10' 132.5(5) . . ? O5 N3 O4 127.1(5) . . ? O5 N3 O3 119.5(5) . . ? O4 N3 O3 113.4(4) . . ? N3 O3 Ag3 105.7(3) . . ? N3 O4 Ag3 93.3(3) . . ? O6 N4 O8 122.8(4) . . ? O6 N4 O7 119.4(4) . . ? O8 N4 O7 117.7(4) . . ? N4 O6 Ag3 92.4(3) . . ? N4 O7 Ag3 98.1(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.419 _refine_diff_density_min -0.656 _refine_diff_density_rms 0.093 #===================================================================END