# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1712 data_complex1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H87 Ag3 La N9 O12 S12 W3' _chemical_formula_weight 2236.94 _chemical_melting_point ? _chemical_compound_source ? 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' 'La' 'La' -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.5919(5) _cell_length_b 17.6515(6) _cell_length_c 26.1720(9) _cell_angle_alpha 90.00 _cell_angle_beta 92.7390(10) _cell_angle_gamma 90.00 _cell_volume 7194.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.39 _cell_measurement_theta_max 25.05 _exptl_crystal_description 'rectangular' _exptl_crystal_colour 'red' _exptl_crystal_size_max .70 _exptl_crystal_size_mid .08 _exptl_crystal_size_min .08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.065 _exptl_crystal_density_method ? _exptl_crystal_F_000 4296 _exptl_absorpt_coefficient_mu 6.555 _exptl_absorpt_correction_type 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .5282 _exptl_absorpt_correction_T_max 1.0000 _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 'Siemens SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 21960 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_sigmaI/netI 0.1186 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 25.05 _reflns_number_total 11974 _reflns_number_observed 6809 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0674P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11974 _refine_ls_number_parameters 664 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1235 _refine_ls_R_factor_obs 0.0606 _refine_ls_wR_factor_all 0.1578 _refine_ls_wR_factor_obs 0.1336 _refine_ls_goodness_of_fit_all 0.955 _refine_ls_goodness_of_fit_obs 1.090 _refine_ls_restrained_S_all 0.955 _refine_ls_restrained_S_obs 1.090 _refine_ls_shift/esd_max -0.019 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W1 W 0.75891(4) 0.56429(3) 0.06393(2) 0.0363(2) Uani 1 d . . W2 W 0.80468(4) 0.23204(3) 0.08103(2) 0.0445(2) Uani 1 d . . W3 W 0.74702(4) -0.10000(3) 0.08416(2) 0.0405(2) Uani 1 d . . Ag1 Ag 0.78959(9) 0.39891(7) 0.06845(5) 0.0575(4) Uani 1 d . . Ag2 Ag 0.77457(9) 0.06660(7) 0.09131(5) 0.0669(4) Uani 1 d . . Ag3 Ag 0.74985(9) 0.73288(7) 0.06913(5) 0.0597(4) Uani 1 d . . S11 S 0.6659(3) 0.4845(2) 0.0950(2) 0.0594(12) Uani 1 d . . S12 S 0.8656(3) 0.5071(2) 0.02696(15) 0.0491(10) Uani 1 d . . S13 S 0.8150(3) 0.6301(2) 0.1278(2) 0.0597(12) Uani 1 d . . S14 S 0.6903(3) 0.6352(2) 0.00565(15) 0.0529(11) Uani 1 d . . S21 S 0.8960(3) 0.1468(2) 0.0557(2) 0.0603(12) Uani 1 d . . S22 S 0.8752(3) 0.3131(3) 0.1305(2) 0.0753(15) Uani 1 d . . S23 S 0.7453(3) 0.2865(2) 0.01295(15) 0.0535(11) Uani 1 d . . S24 S 0.7021(4) 0.1822(3) 0.1247(2) 0.091(2) Uani 1 d . . S31 S 0.8106(3) -0.0437(2) 0.1503(2) 0.0586(12) Uani 1 d . . S32 S 0.6804(3) -0.0191(2) 0.0320(2) 0.0635(13) Uani 1 d . . S33 S 0.6505(3) -0.1770(2) 0.1136(2) 0.0580(12) Uani 1 d . . S34 S 0.8456(3) -0.1591(3) 0.0419(2) 0.0692(14) Uani 1 d . . La La 0.23061(5) 0.22357(5) 0.29190(3) 0.0366(2) Uani 1 d . . O1 O 0.1647(7) 0.1710(6) 0.3682(4) 0.064(3) Uani 1 d . . O2 O 0.1645(7) 0.3295(6) 0.3337(4) 0.061(3) Uani 1 d . . O3 O 0.3485(6) 0.2023(6) 0.3544(4) 0.053(3) Uani 1 d . . O4 O 0.0949(7) 0.1609(7) 0.2676(4) 0.073(4) Uani 1 d . . O5 O 0.1779(7) 0.2774(7) 0.2112(4) 0.072(4) Uani 1 d . . O10 O 0.3511(8) 0.2014(6) 0.2317(4) 0.075(4) Uani 1 d . . O11 O 0.3262(6) 0.3447(6) 0.2845(4) 0.055(3) Uani 1 d . . O12 O 0.2612(6) 0.0779(6) 0.2764(4) 0.061(3) Uani 1 d . . N1 N 0.0763(12) 0.1153(10) 0.4190(5) 0.097(6) Uani 1 d . . N2 N 0.0978(8) 0.3881(8) 0.3988(5) 0.057(4) Uani 1 d . . N3 N 0.4345(9) 0.1745(11) 0.4193(6) 0.081(5) Uani 1 d . . N4 N -0.0410(12) 0.1331(14) 0.2644(6) 0.120(9) Uani 1 d . . N5 N 0.1356(17) 0.2923(18) 0.1293(11) 0.058(8) Uiso 0.50 d P . N51 N 0.1518(21) 0.3402(22) 0.1429(14) 0.086(10) Uiso 0.50 d P . C11 C 0.1458(13) 0.1211(14) 0.3992(7) 0.088(8) Uani 1 d . . C12 C 0.2115(10) 0.0553(9) 0.4142(6) 0.062(5) Uani 1 d . . C13 C 0.0509(10) 0.0573(10) 0.4568(6) 0.071(5) Uani 1 d . . C14 C 0.0067(11) 0.1805(11) 0.4025(7) 0.084(7) Uani 1 d . . C21 C 0.1054(10) 0.3710(9) 0.3491(7) 0.055(4) Uani 1 d . . C22 C 0.0422(13) 0.4069(12) 0.3122(7) 0.102(8) Uani 1 d . . C23 C 0.0340(11) 0.4398(10) 0.4188(7) 0.076(6) Uani 1 d . . C24 C 0.1631(12) 0.3499(11) 0.4359(7) 0.088(7) Uani 1 d . . C31 C 0.3892(11) 0.2206(15) 0.3955(7) 0.089(8) Uani 1 d . . C32 C 0.3897(12) 0.3039(10) 0.4173(6) 0.066(5) Uani 1 d . . C33 C 0.4861(10) 0.1886(10) 0.4692(6) 0.067(5) Uani 1 d . . C34 C 0.4439(11) 0.0927(10) 0.3963(7) 0.068(5) Uani 1 d . . C41 C 0.0312(17) 0.1199(21) 0.2726(8) 0.137(13) Uani 1 d . . C42 C 0.0417(14) 0.0312(10) 0.2923(8) 0.090(7) Uani 1 d . . C43 C -0.0536(14) 0.2217(16) 0.2477(10) 0.126(10) Uani 1 d . . C44 C -0.1233(12) 0.0919(13) 0.2685(9) 0.113(8) Uani 1 d . . C51 C 0.1593(16) 0.2926(17) 0.1711(12) 0.121(9) Uiso 1 d . . C52 C 0.1082(14) 0.2089(13) 0.1340(8) 0.102(7) Uiso 1 d . . C53 C 0.1178(15) 0.3398(15) 0.0835(10) 0.129(9) Uiso 1 d . . C54 C 0.1937(16) 0.4038(15) 0.1724(10) 0.132(9) Uiso 1 d . . O6 O 0.1869(7) 0.0005(7) 0.1921(5) 0.073(4) Uani 1 d . . N6 N 0.1154(10) 0.0062(9) 0.1154(7) 0.084(5) Uani 1 d . . C61 C 0.1850(15) 0.0163(10) 0.1466(9) 0.082(7) Uani 1 d . . C62 C 0.2670(11) 0.0458(11) 0.1234(9) 0.103(8) Uani 1 d . . C63 C 0.1107(14) 0.0220(12) 0.0588(7) 0.095(7) Uani 1 d . . C64 C 0.0330(11) -0.0131(11) 0.1415(8) 0.082(6) Uani 1 d . . O7 O 0.0087(6) 0.8563(6) 0.2503(4) 0.062(3) Uani 1 d . . N7 N -0.1289(8) 0.8211(7) 0.2553(5) 0.051(3) Uani 1 d . . C71 C -0.0517(10) 0.8183(10) 0.2327(6) 0.055(5) Uani 1 d . . C72 C -0.0456(10) 0.7704(10) 0.1849(6) 0.071(6) Uani 1 d . . C73 C -0.1417(11) 0.8712(11) 0.3006(7) 0.078(6) Uani 1 d . . C74 C -0.2094(10) 0.7814(11) 0.2346(7) 0.075(6) Uani 1 d . . O8 O 0.4408(7) 0.0731(7) 0.2614(5) 0.079(4) Uani 1 d . . N8 N 0.5708(11) 0.0304(14) 0.2587(10) 0.136(11) Uani 1 d . . C81 C 0.5143(15) 0.0616(19) 0.2518(13) 0.164(18) Uani 1 d . . C82 C 0.5432(17) 0.1192(14) 0.1992(9) 0.132(11) Uani 1 d . . C83 C 0.6568(13) 0.0155(18) 0.2483(14) 0.218(20) Uani 1 d . . C84 C 0.5381(18) -0.0262(11) 0.3080(9) 0.112(9) Uani 1 d . . O9 O 0.6447(11) 0.7789(11) -0.1309(5) 0.139(7) Uani 1 d . . N9 N 0.5478(14) 0.7607(15) -0.0748(8) 0.129(8) Uani 1 d . . C91 C 0.5891(16) 0.7362(18) -0.1115(10) 0.114(10) Uani 1 d . . C92 C 0.5828(21) 0.6520(15) -0.1291(11) 0.167(14) Uani 1 d . . C93 C 0.4791(15) 0.7112(17) -0.0498(10) 0.157(13) Uani 1 d . . C94 C 0.5626(24) 0.8436(16) -0.0579(12) 0.196(17) 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 W1 0.0480(4) 0.0273(3) 0.0338(3) -0.0013(3) 0.0024(3) -0.0009(3) W2 0.0664(5) 0.0267(4) 0.0415(4) 0.0024(3) 0.0136(3) -0.0008(3) W3 0.0435(4) 0.0270(4) 0.0516(4) 0.0042(3) 0.0072(3) -0.0017(3) Ag1 0.0847(10) 0.0273(7) 0.0608(8) 0.0006(6) 0.0062(7) -0.0012(7) Ag2 0.0940(10) 0.0296(8) 0.0780(10) 0.0048(7) 0.0127(8) -0.0038(7) Ag3 0.0751(9) 0.0277(7) 0.0763(10) -0.0009(6) 0.0038(7) -0.0009(7) S11 0.063(3) 0.044(3) 0.074(3) 0.009(2) 0.024(2) 0.000(2) S12 0.054(3) 0.040(2) 0.054(3) -0.001(2) 0.013(2) -0.004(2) S13 0.083(3) 0.047(3) 0.047(3) -0.009(2) -0.017(2) 0.004(2) S14 0.068(3) 0.043(3) 0.046(2) 0.006(2) -0.007(2) -0.001(2) S21 0.064(3) 0.045(3) 0.074(3) 0.010(2) 0.023(2) 0.010(2) S22 0.115(4) 0.047(3) 0.061(3) 0.000(2) -0.030(3) 0.010(3) S23 0.069(3) 0.045(3) 0.045(2) -0.002(2) -0.007(2) -0.004(2) S24 0.130(5) 0.041(3) 0.110(4) 0.013(3) 0.080(4) 0.006(3) S31 0.071(3) 0.053(3) 0.051(3) 0.005(2) -0.007(2) -0.007(2) S32 0.071(3) 0.056(3) 0.063(3) 0.017(2) -0.015(2) -0.003(2) S33 0.052(3) 0.041(3) 0.083(3) 0.006(2) 0.017(2) -0.005(2) S34 0.078(3) 0.045(3) 0.087(3) 0.004(2) 0.037(3) 0.002(2) La 0.0390(5) 0.0411(5) 0.0299(5) 0.0063(4) 0.0047(4) 0.0006(4) O1 0.089(9) 0.060(8) 0.047(7) 0.019(6) 0.034(6) -0.004(7) O2 0.064(7) 0.056(8) 0.065(8) -0.006(6) 0.021(6) 0.025(6) O3 0.044(6) 0.076(8) 0.038(6) 0.018(6) -0.013(5) -0.009(6) O4 0.056(8) 0.086(10) 0.077(9) 0.020(7) 0.009(6) -0.020(7) O5 0.096(9) 0.074(9) 0.043(7) 0.024(6) -0.025(6) -0.019(7) O10 0.100(9) 0.067(8) 0.064(8) 0.004(6) 0.051(7) 0.019(7) O11 0.046(6) 0.053(7) 0.068(7) 0.003(6) 0.014(5) -0.004(5) O12 0.057(7) 0.047(7) 0.079(8) -0.006(6) 0.005(6) 0.005(6) N1 0.126(15) 0.116(16) 0.049(10) -0.030(10) 0.017(10) -0.070(13) N2 0.059(9) 0.056(10) 0.058(9) 0.002(8) 0.009(7) -0.015(7) N3 0.037(9) 0.155(18) 0.053(10) 0.021(11) 0.021(8) -0.006(10) N4 0.068(13) 0.229(28) 0.064(12) -0.014(14) 0.011(10) -0.056(16) C11 0.075(15) 0.140(22) 0.051(12) -0.039(13) 0.024(11) -0.051(15) C12 0.055(11) 0.056(12) 0.076(12) 0.027(10) 0.003(9) 0.022(9) C13 0.071(12) 0.083(14) 0.061(11) 0.027(10) 0.036(9) -0.020(11) C14 0.054(12) 0.094(16) 0.104(16) 0.010(12) 0.009(11) 0.054(11) C21 0.059(11) 0.038(10) 0.070(13) 0.012(9) 0.011(10) -0.010(9) C22 0.112(17) 0.130(20) 0.059(13) 0.013(13) -0.039(12) 0.046(15) C23 0.074(12) 0.058(13) 0.100(15) -0.013(11) 0.029(11) 0.022(11) C24 0.114(16) 0.085(15) 0.062(13) 0.002(11) -0.024(11) 0.049(13) C31 0.029(10) 0.185(27) 0.054(13) 0.052(15) 0.013(10) 0.003(13) C32 0.102(15) 0.045(11) 0.053(11) 0.000(9) 0.011(10) 0.013(10) C33 0.069(12) 0.104(16) 0.026(9) -0.006(9) -0.024(8) 0.014(11) C34 0.076(13) 0.049(12) 0.077(13) -0.007(10) -0.012(10) -0.004(10) C41 0.074(18) 0.292(44) 0.044(13) -0.057(19) 0.014(13) -0.048(24) C42 0.132(19) 0.040(12) 0.099(17) 0.011(11) 0.034(14) -0.014(12) C43 0.093(17) 0.144(24) 0.139(23) 0.073(19) -0.006(15) 0.047(17) C44 0.057(13) 0.149(23) 0.134(21) 0.030(17) 0.012(13) -0.035(14) O6 0.084(9) 0.057(8) 0.078(9) 0.006(7) 0.005(7) -0.016(7) N6 0.066(11) 0.058(11) 0.129(17) -0.015(10) -0.003(11) 0.008(9) C61 0.112(19) 0.029(11) 0.107(19) 0.022(12) 0.037(16) 0.027(12) C62 0.055(12) 0.088(17) 0.170(22) 0.008(15) 0.051(13) -0.020(12) C63 0.140(19) 0.104(18) 0.044(12) 0.021(11) 0.031(12) 0.020(14) C64 0.046(11) 0.088(16) 0.113(17) 0.014(12) 0.022(11) -0.008(10) O7 0.039(7) 0.079(9) 0.069(8) -0.030(6) 0.010(6) -0.016(6) N7 0.055(9) 0.051(9) 0.048(8) 0.005(7) 0.012(7) -0.012(7) C71 0.036(10) 0.083(14) 0.047(10) -0.002(9) 0.011(8) 0.013(9) C72 0.043(10) 0.103(15) 0.067(12) -0.055(11) 0.017(9) -0.001(10) C73 0.086(14) 0.087(15) 0.065(13) -0.023(11) 0.033(10) -0.007(11) C74 0.042(10) 0.114(17) 0.068(12) 0.009(11) -0.011(9) -0.027(10) O8 0.049(7) 0.087(10) 0.102(10) -0.010(8) 0.016(7) 0.016(7) N8 0.030(11) 0.174(25) 0.201(25) -0.138(21) -0.004(13) 0.009(12) C81 0.036(14) 0.197(34) 0.258(41) -0.170(32) -0.011(20) -0.013(18) C82 0.173(24) 0.107(20) 0.124(21) -0.020(16) 0.098(19) -0.061(18) C83 0.037(14) 0.247(36) 0.368(48) -0.205(34) -0.021(20) 0.020(17) C84 0.192(25) 0.057(14) 0.082(16) -0.002(12) -0.060(16) 0.024(16) O9 0.136(15) 0.215(20) 0.069(10) -0.005(11) 0.043(10) -0.071(14) N9 0.112(17) 0.192(26) 0.083(15) 0.054(16) -0.004(13) 0.031(17) C91 0.080(18) 0.193(33) 0.069(17) 0.006(19) -0.006(14) 0.014(19) C92 0.263(37) 0.079(20) 0.152(27) -0.018(18) -0.073(24) -0.004(22) C93 0.090(18) 0.217(31) 0.168(25) 0.111(23) 0.048(17) -0.023(19) C94 0.342(48) 0.086(21) 0.162(30) -0.059(21) 0.040(29) 0.015(26) _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 W1 S13 2.184(4) . ? W1 S11 2.204(4) . ? W1 S12 2.208(4) . ? W1 S14 2.210(4) . ? W1 Ag1 2.9596(13) . ? W1 Ag3 2.9826(13) . ? W2 S22 2.190(5) . ? W2 S23 2.191(4) . ? W2 S21 2.196(4) . ? W2 S24 2.194(4) . ? W2 Ag1 2.9720(13) . ? W2 Ag2 2.9720(14) . ? W3 S31 2.192(4) . ? W3 S33 2.195(4) . ? W3 S34 2.199(4) . ? W3 S32 2.202(4) . ? W3 Ag2 2.9765(14) . ? W3 Ag3 2.9766(14) 1_545 ? Ag1 S12 2.521(4) . ? Ag1 S23 2.535(4) . ? Ag1 S22 2.550(5) . ? Ag1 S11 2.570(4) . ? Ag2 S24 2.510(5) . ? Ag2 S31 2.531(4) . ? Ag2 S21 2.574(4) . ? Ag2 S32 2.576(5) . ? Ag3 S14 2.539(4) . ? Ag3 S33 2.541(4) 1_565 ? Ag3 S34 2.544(5) 1_565 ? Ag3 S13 2.556(4) . ? Ag3 W3 2.9766(14) 1_565 ? S33 Ag3 2.541(4) 1_545 ? S34 Ag3 2.544(5) 1_545 ? La O5 2.424(11) . ? La O2 2.421(10) . ? La O3 2.432(10) . ? La O4 2.445(12) . ? La O1 2.469(10) . ? La O10 2.538(9) . ? La O11 2.619(10) . ? La O12 2.650(10) . ? O1 C11 1.24(2) . ? O2 C21 1.26(2) . ? O3 C31 1.26(2) . ? O4 C41 1.24(3) . ? O5 C51 1.11(3) . ? N1 C11 1.23(2) . ? N1 C13 1.49(2) . ? N1 C14 1.63(2) . ? N2 C21 1.35(2) . ? N2 C23 1.47(2) . ? N2 C24 1.53(2) . ? N3 C31 1.23(2) . ? N3 C33 1.52(2) . ? N3 C34 1.57(2) . ? N4 C41 1.16(3) . ? N4 C44 1.48(2) . ? N4 C43 1.63(3) . ? N5 C51 1.14(4) . ? N5 C52 1.54(3) . ? N51 C51 1.12(4) . ? N51 C54 1.50(4) . ? N51 C53 1.62(4) . ? C11 C12 1.59(3) . ? C21 C22 1.49(2) . ? C31 C32 1.58(3) . ? C41 C42 1.65(4) . ? C51 C52 1.92(3) . ? O6 C61 1.22(2) . ? N6 C61 1.34(2) . ? N6 C63 1.51(2) . ? N6 C64 1.52(2) . ? C61 C62 1.53(2) . ? O7 C71 1.23(2) . ? N7 C71 1.37(2) . ? N7 C73 1.50(2) . ? N7 C74 1.52(2) . ? C71 C72 1.52(2) . ? O8 C81 1.20(2) . ? N8 C81 1.05(3) . ? N8 C83 1.41(3) . ? N8 C84 1.73(3) . ? C81 C82 1.79(4) . ? O9 C91 1.27(3) . ? N9 C91 1.26(3) . ? N9 C93 1.55(3) . ? N9 C94 1.54(3) . ? C91 C92 1.56(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S13 W1 S11 107.7(2) . . ? S13 W1 S12 107.2(2) . . ? S11 W1 S12 113.07(15) . . ? S13 W1 S14 113.0(2) . . ? S11 W1 S14 108.1(2) . . ? S12 W1 S14 107.8(2) . . ? S13 W1 Ag1 115.85(12) . . ? S11 W1 Ag1 57.50(11) . . ? S12 W1 Ag1 56.16(10) . . ? S14 W1 Ag1 131.19(11) . . ? S13 W1 Ag3 56.80(11) . . ? S11 W1 Ag3 125.98(11) . . ? S12 W1 Ag3 120.94(10) . . ? S14 W1 Ag3 56.20(11) . . ? Ag1 W1 Ag3 171.98(4) . . ? S22 W2 S23 112.0(2) . . ? S22 W2 S21 108.2(2) . . ? S23 W2 S21 108.0(2) . . ? S22 W2 S24 108.2(2) . . ? S23 W2 S24 108.0(2) . . ? S21 W2 S24 112.5(2) . . ? S22 W2 Ag1 56.81(12) . . ? S23 W2 Ag1 56.40(11) . . ? S21 W2 Ag1 134.00(11) . . ? S24 W2 Ag1 113.53(13) . . ? S22 W2 Ag2 131.75(12) . . ? S23 W2 Ag2 116.26(11) . . ? S21 W2 Ag2 57.42(11) . . ? S24 W2 Ag2 55.72(12) . . ? Ag1 W2 Ag2 166.38(5) . . ? S31 W3 S33 107.2(2) . . ? S31 W3 S34 108.2(2) . . ? S33 W3 S34 113.0(2) . . ? S31 W3 S32 112.2(2) . . ? S33 W3 S32 107.9(2) . . ? S34 W3 S32 108.4(2) . . ? S31 W3 Ag2 56.20(11) . . ? S33 W3 Ag2 133.54(12) . . ? S34 W3 Ag2 113.46(12) . . ? S32 W3 Ag2 57.35(12) . . ? S31 W3 Ag3 123.02(12) . 1_545 ? S33 W3 Ag3 56.47(11) . 1_545 ? S34 W3 Ag3 56.52(12) . 1_545 ? S32 W3 Ag3 124.78(12) . 1_545 ? Ag2 W3 Ag3 169.87(4) . 1_545 ? S12 Ag1 S23 117.84(14) . . ? S12 Ag1 S22 118.8(2) . . ? S23 Ag1 S22 91.16(14) . . ? S12 Ag1 S11 92.59(13) . . ? S23 Ag1 S11 115.27(15) . . ? S22 Ag1 S11 123.6(2) . . ? S12 Ag1 W1 46.68(9) . . ? S23 Ag1 W1 135.22(11) . . ? S22 Ag1 W1 133.61(11) . . ? S11 Ag1 W1 46.32(9) . . ? S12 Ag1 W2 139.67(10) . . ? S23 Ag1 W2 46.05(9) . . ? S22 Ag1 W2 45.95(11) . . ? S11 Ag1 W2 127.50(10) . . ? W1 Ag1 W2 173.62(5) . . ? S24 Ag2 S31 120.2(2) . . ? S24 Ag2 S21 91.73(15) . . ? S31 Ag2 S21 119.89(15) . . ? S24 Ag2 S32 115.7(2) . . ? S31 Ag2 S32 91.13(14) . . ? S21 Ag2 S32 120.8(2) . . ? S24 Ag2 W2 46.23(10) . . ? S31 Ag2 W2 141.21(11) . . ? S21 Ag2 W2 45.96(9) . . ? S32 Ag2 W2 127.61(11) . . ? S24 Ag2 W3 139.40(12) . . ? S31 Ag2 W3 46.03(10) . . ? S21 Ag2 W3 128.82(11) . . ? S32 Ag2 W3 46.03(10) . . ? W2 Ag2 W3 171.13(6) . . ? S14 Ag3 S33 120.86(15) . 1_565 ? S14 Ag3 S34 121.75(15) . 1_565 ? S33 Ag3 S34 92.17(14) 1_565 1_565 ? S14 Ag3 S13 91.93(13) . . ? S33 Ag3 S13 113.76(14) 1_565 . ? S34 Ag3 S13 118.6(2) 1_565 . ? S14 Ag3 W3 138.77(10) . 1_565 ? S33 Ag3 W3 46.04(9) 1_565 1_565 ? S34 Ag3 W3 46.13(10) 1_565 1_565 ? S13 Ag3 W3 129.20(10) . 1_565 ? S14 Ag3 W1 46.32(9) . . ? S33 Ag3 W1 132.59(10) 1_565 . ? S34 Ag3 W1 134.85(11) 1_565 . ? S13 Ag3 W1 45.64(9) . . ? W3 Ag3 W1 174.77(5) 1_565 . ? W1 S11 Ag1 76.18(12) . . ? W1 S12 Ag1 77.17(12) . . ? W1 S13 Ag3 77.56(13) . . ? W1 S14 Ag3 77.48(12) . . ? W2 S21 Ag2 76.62(13) . . ? W2 S22 Ag1 77.24(14) . . ? W2 S23 Ag1 77.55(12) . . ? W2 S24 Ag2 78.05(14) . . ? W3 S31 Ag2 77.76(13) . . ? W3 S32 Ag2 76.62(13) . . ? W3 S33 Ag3 77.50(13) . 1_545 ? W3 S34 Ag3 77.35(13) . 1_545 ? O5 La O2 87.5(4) . . ? O5 La O3 149.4(3) . . ? O2 La O3 98.0(4) . . ? O5 La O4 72.4(4) . . ? O2 La O4 94.8(4) . . ? O3 La O4 136.3(4) . . ? O5 La O1 135.7(4) . . ? O2 La O1 73.8(4) . . ? O3 La O1 74.2(3) . . ? O4 La O1 69.6(4) . . ? O5 La O10 75.5(4) . . ? O2 La O10 138.0(4) . . ? O3 La O10 80.5(4) . . ? O4 La O10 115.2(4) . . ? O1 La O10 142.4(4) . . ? O5 La O11 77.6(3) . . ? O2 La O11 70.1(3) . . ? O3 La O11 76.2(3) . . ? O4 La O11 147.0(3) . . ? O1 La O11 128.8(3) . . ? O10 La O11 68.8(3) . . ? O5 La O12 107.6(4) . . ? O2 La O12 154.4(3) . . ? O3 La O12 79.5(3) . . ? O4 La O12 71.4(4) . . ? O1 La O12 81.1(3) . . ? O10 La O12 67.1(3) . . ? O11 La O12 132.3(3) . . ? C11 O1 La 156.2(12) . . ? C21 O2 La 158.2(11) . . ? C31 O3 La 150.0(13) . . ? C41 O4 La 157.6(14) . . ? C51 O5 La 169.3(19) . . ? C11 N1 C13 127.2(22) . . ? C11 N1 C14 115.0(19) . . ? C13 N1 C14 117.8(15) . . ? C21 N2 C23 125.3(15) . . ? C21 N2 C24 115.4(14) . . ? C23 N2 C24 119.3(14) . . ? C31 N3 C33 126.5(21) . . ? C31 N3 C34 118.4(19) . . ? C33 N3 C34 115.1(15) . . ? C41 N4 C44 136.3(31) . . ? C41 N4 C43 110.3(26) . . ? C44 N4 C43 113.3(20) . . ? C51 N5 C52 90.5(28) . . ? C51 N51 C54 101.0(35) . . ? C51 N51 C53 130.5(40) . . ? C54 N51 C53 128.0(30) . . ? N1 C11 O1 125.2(24) . . ? N1 C11 C12 114.1(21) . . ? O1 C11 C12 120.7(16) . . ? O2 C21 N2 122.6(16) . . ? O2 C21 C22 120.9(17) . . ? N2 C21 C22 116.4(16) . . ? N3 C31 O3 121.1(25) . . ? N3 C31 C32 116.2(20) . . ? O3 C31 C32 122.7(18) . . ? N4 C41 O4 129.6(37) . . ? N4 C41 C42 109.2(27) . . ? O4 C41 C42 121.1(24) . . ? O5 C51 N51 145.2(41) . . ? O5 C51 N5 165.2(39) . . ? N51 C51 N5 49.6(25) . . ? O5 C51 C52 112.1(24) . . ? N51 C51 C52 102.4(32) . . ? N5 C51 C52 53.2(22) . . ? N5 C52 C51 36.4(14) . . ? C61 N6 C63 125.1(19) . . ? C61 N6 C64 115.6(18) . . ? C63 N6 C64 118.8(16) . . ? O6 C61 N6 123.0(21) . . ? O6 C61 C62 118.8(23) . . ? N6 C61 C62 118.1(21) . . ? C71 N7 C73 121.2(13) . . ? C71 N7 C74 123.9(14) . . ? C73 N7 C74 114.6(13) . . ? O7 C71 N7 119.5(15) . . ? O7 C71 C72 122.5(14) . . ? N7 C71 C72 118.0(15) . . ? C81 N8 C83 150.2(42) . . ? C81 N8 C84 99.0(29) . . ? C83 N8 C84 110.8(26) . . ? N8 C81 O8 148.8(47) . . ? N8 C81 C82 101.0(30) . . ? O8 C81 C82 110.1(30) . . ? C91 N9 C93 121.2(29) . . ? C91 N9 C94 118.0(27) . . ? C93 N9 C94 120.6(24) . . ? N9 C91 O9 119.0(31) . . ? N9 C91 C92 121.8(30) . . ? O9 C91 C92 118.8(25) . . ? _refine_diff_density_max 1.949 _refine_diff_density_min -1.817 _refine_diff_density_rms 0.232 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA ; data_complex2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C80 H176 Ag10 La2 N16 O16 S32 W8' _chemical_formula_weight 5471.61 _chemical_melting_point ? _chemical_compound_source ? 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' 'La' 'La' -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 21.6534(3) _cell_length_b 18.11250(10) _cell_length_c 22.1818(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.5310(10) _cell_angle_gamma 90.00 _cell_volume 8248.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.14 _cell_measurement_theta_max 25.01 _exptl_crystal_description 'rhombic' _exptl_crystal_colour 'red' _exptl_crystal_size_max 1.20 _exptl_crystal_size_mid .40 _exptl_crystal_size_min .40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.203 _exptl_crystal_density_method ? _exptl_crystal_F_000 5168 _exptl_absorpt_coefficient_mu 7.664 _exptl_absorpt_correction_type 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .0505 _exptl_absorpt_correction_T_max .1477 _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 'Siemens SMART CCD' _diffrn_measurement_method ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 22388 _diffrn_reflns_av_R_equivalents 0.0524 _diffrn_reflns_av_sigmaI/netI 0.1020 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 25.01 _reflns_number_total 12480 _reflns_number_observed 6559 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 10 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0690P)^2^+49.1613P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12470 _refine_ls_number_parameters 560 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.1648 _refine_ls_R_factor_obs 0.0840 _refine_ls_wR_factor_all 0.2034 _refine_ls_wR_factor_obs 0.1668 _refine_ls_goodness_of_fit_all 1.045 _refine_ls_goodness_of_fit_obs 1.215 _refine_ls_restrained_S_all 1.064 _refine_ls_restrained_S_obs 1.217 _refine_ls_shift/esd_max -0.231 _refine_ls_shift/esd_mean 0.010 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W1 W 0.71630(4) 0.41407(5) 0.45943(4) 0.0804(3) Uani 1 d . . W2 W 0.54131(4) 0.62529(5) 0.28298(5) 0.0889(4) Uani 1 d . . W3 W 0.36807(4) 0.85537(5) 0.13148(4) 0.0696(3) Uani 1 d . . W4 W 0.18623(5) 0.64244(5) -0.04006(5) 0.0858(3) Uani 1 d . . Ag1 Ag 0.63199(9) 0.51983(11) 0.36982(10) 0.1135(7) Uani 1 d . . Ag2 Ag 0.45213(9) 0.74115(10) 0.21207(9) 0.0991(6) Uani 1 d . . Ag3 Ag 0.28368(9) 0.74485(10) 0.04027(9) 0.0960(6) Uani 1 d . . Ag4 Ag 0.11563(10) 0.75933(12) -0.12760(11) 0.1251(8) Uani 1 d . . Ag5 Ag 0.28421(8) 0.96272(10) 0.04121(9) 0.0939(6) Uani 1 d . . S11 S 0.6877(5) 0.3145(5) 0.4938(5) 0.184(4) Uani 1 d . . S12 S 0.6910(4) 0.4034(4) 0.3566(3) 0.133(3) Uani 1 d . . S13 S 0.6652(3) 0.5086(4) 0.4901(3) 0.107(2) Uani 1 d . . S14 S 0.8222(3) 0.4208(3) 0.4992(3) 0.102(2) Uani 1 d . . S21 S 0.5108(3) 0.5173(4) 0.3079(4) 0.139(3) Uani 1 d . . S22 S 0.5078(4) 0.6328(4) 0.1795(4) 0.130(3) Uani 1 d . . S23 S 0.4951(3) 0.7091(4) 0.3284(3) 0.099(2) Uani 1 d . . S24 S 0.6490(3) 0.6359(3) 0.3121(4) 0.125(3) Uani 1 d . . S31 S 0.3292(2) 0.7534(3) 0.1637(3) 0.076(2) Uani 1 d . . S32 S 0.3513(4) 0.8537(3) 0.0269(3) 0.102(2) Uani 1 d . . S33 S 0.3228(3) 0.9492(3) 0.1612(3) 0.093(2) Uani 1 d . . S34 S 0.4727(3) 0.8685(3) 0.1758(4) 0.115(3) Uani 1 d . . S41 S 0.1456(5) 0.5571(6) 0.0017(5) 0.179(4) Uani 1 d . . S42 S 0.1471(4) 0.6286(4) -0.1431(3) 0.122(3) Uani 1 d . . S43 S 0.1599(3) 0.7515(4) -0.0071(3) 0.129(3) Uani 1 d . . S44 S 0.2909(3) 0.6244(3) -0.0120(3) 0.094(2) Uani 1 d . . La La 0.47069(5) 0.22555(6) 0.20722(6) 0.0629(3) Uani 1 d . . O3 O 0.4332(8) 0.1162(10) 0.2503(9) 0.129(7) Uani 1 d . . O4 O 0.5680(7) 0.2955(11) 0.2065(9) 0.124(6) Uani 1 d . . O5 O 0.4576(8) 0.2236(11) 0.0938(8) 0.119(6) Uani 1 d . . O6 O 0.4515(8) 0.2962(9) 0.2942(8) 0.102(5) Uani 1 d . . O7 O 0.3511(7) 0.2193(9) 0.1628(7) 0.100(5) Uani 1 d . . N3 N 0.4364(12) 0.0295(13) 0.3213(11) 0.130(8) Uani 1 d . . N4 N 0.6346(10) 0.3772(11) 0.1857(10) 0.114(7) Uani 1 d . . N5 N 0.4306(8) 0.2463(9) -0.0086(10) 0.090(5) Uani 1 d . . N6 N 0.4572(9) 0.3475(12) 0.3863(9) 0.105(6) Uani 1 d . . N7 N 0.2580(10) 0.1841(12) 0.1694(12) 0.136(9) Uani 1 d D . C3 C 0.4477(11) 0.0525(15) 0.2720(12) 0.100(8) Uani 1 d . . C4 C 0.5834(11) 0.3622(17) 0.2063(12) 0.102(8) Uani 1 d . . C5 C 0.4174(14) 0.2314(13) 0.0425(13) 0.094(8) Uani 1 d . . C6 C 0.4843(13) 0.3249(12) 0.3436(13) 0.087(8) Uani 1 d . . C7 C 0.3064(10) 0.1714(15) 0.1489(12) 0.103(9) Uani 1 d . . C31 C 0.4432(34) 0.1025(38) 0.3967(33) 0.337(33) Uiso 1 d . . C32 C 0.3945(29) 0.0931(33) 0.3517(29) 0.272(26) Uiso 1 d . . C33 C 0.4751(28) -0.0526(31) 0.3631(25) 0.253(24) Uiso 1 d . . C34 C 0.4278(30) -0.0825(34) 0.3534(29) 0.294(29) Uiso 1 d . . C41 C 0.6737(18) 0.3170(21) 0.1640(17) 0.168(13) Uiso 1 d . . C42 C 0.7293(18) 0.2929(19) 0.2251(18) 0.178(13) Uiso 1 d . . C43 C 0.6510(15) 0.4615(18) 0.1893(16) 0.151(11) Uiso 1 d . . C44 C 0.6213(16) 0.4924(19) 0.1244(17) 0.165(12) Uiso 1 d . . C51 C 0.3765(17) 0.2713(19) -0.0733(17) 0.161(12) Uiso 1 d . . C52 C 0.3722(19) 0.2191(22) -0.1140(19) 0.192(15) Uiso 1 d . . C53 C 0.4994(14) 0.2431(16) -0.0115(13) 0.127(9) Uiso 1 d . . C54 C 0.5275(15) 0.3195(18) 0.0029(15) 0.147(11) Uiso 1 d . . C61 C 0.3847(15) 0.3371(17) 0.3750(14) 0.136(10) Uiso 1 d . . C62 C 0.3555(19) 0.4051(23) 0.3495(18) 0.195(15) Uiso 1 d . . C63 C 0.4956(16) 0.3954(19) 0.4433(17) 0.156(11) Uiso 1 d . . C64 C 0.5021(19) 0.3546(21) 0.5003(20) 0.190(15) Uiso 1 d . . C71 C 0.2068(26) 0.1145(26) 0.1745(29) 0.258(27) Uiso 1 d D . C72 C 0.1648(34) 0.1303(35) 0.1572(33) 0.315(37) Uiso 1 d . . C73 C 0.2609(20) 0.2459(26) 0.2207(21) 0.211(17) Uiso 1 d . . C74 C 0.2285(22) 0.3063(27) 0.1777(22) 0.235(19) Uiso 1 d . . C8 C 0.3990(14) 0.3987(18) 0.1759(13) 0.157(15) Uani 1 d D . O8 O 0.4323(8) 0.3528(8) 0.1635(8) 0.105(5) Uani 1 d D . N8 N 0.3719(10) 0.4554(10) 0.1366(10) 0.123(8) Uani 1 d D . C81 C 0.3524(21) 0.4421(23) 0.0670(19) 0.256(22) Uiso 1 d D . C82 C 0.4168(18) 0.4687(20) 0.0569(16) 0.180(14) Uiso 1 d D . C83 C 0.3477(17) 0.5328(19) 0.1532(17) 0.191(15) Uiso 1 d D . C84 C 0.2821(18) 0.5113(21) 0.1474(18) 0.206(16) Uiso 1 d D . C1 C 0.5071(15) 0.0769(22) 0.1430(19) 0.237 Uiso 1 d D . O1 O 0.5320(13) 0.1210(15) 0.1858(13) 0.218 Uiso 1 d D . N1 N 0.5561(15) 0.0487(17) 0.1185(14) 0.246 Uiso 1 d D . C11 C 0.6225(21) 0.0503(26) 0.1734(20) 0.282(24) Uiso 1 d D . C12 C 0.6566(21) 0.0948(30) 0.1302(25) 0.302(26) Uiso 1 d D . C13 C 0.5558(24) -0.0260(28) 0.0821(24) 0.381 Uiso 1 d D . C14 C 0.4960(23) -0.0097(26) 0.0286(17) 0.243(21) Uiso 1 d D . C2 C 0.6107(12) 0.1990(14) 0.3346(14) 0.125(11) Uani 1 d D . O2 O 0.5558(9) 0.1930(11) 0.3055(9) 0.140(7) Uani 1 d D . N2 N 0.6450(9) 0.1498(11) 0.3757(11) 0.131(8) Uani 1 d D . C21 C 0.6085(25) 0.0856(25) 0.3915(27) 0.372(36) Uiso 1 d D . C22 C 0.5928(31) 0.1276(35) 0.4490(27) 0.366(35) Uiso 1 d D . C23 C 0.7200(18) 0.1390(25) 0.4125(22) 0.275(24) Uiso 1 d D . C24 C 0.7241(29) 0.0784(36) 0.3661(33) 0.423(42) Uiso 1 d D . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0824(6) 0.0644(6) 0.0727(7) -0.0040(5) -0.0061(5) -0.0012(4) W2 0.0679(6) 0.0759(6) 0.1022(8) 0.0183(6) -0.0024(5) 0.0060(4) W3 0.0602(5) 0.0647(5) 0.0805(7) 0.0157(5) 0.0176(4) 0.0058(4) W4 0.0883(7) 0.0884(7) 0.0781(8) -0.0181(6) 0.0227(5) 0.0017(5) Ag1 0.0971(13) 0.0958(14) 0.113(2) 0.0175(12) -0.0147(12) 0.0224(11) Ag2 0.0860(12) 0.0905(13) 0.100(2) 0.0259(11) -0.0005(10) 0.0202(9) Ag3 0.0936(13) 0.0869(12) 0.0944(15) -0.0087(11) 0.0112(10) 0.0030(10) Ag4 0.1048(15) 0.113(2) 0.125(2) -0.0085(14) -0.0092(13) 0.0212(12) Ag5 0.0894(12) 0.0824(12) 0.0929(14) 0.0204(10) 0.0048(10) 0.0130(9) S11 0.216(10) 0.117(7) 0.206(10) 0.010(7) 0.046(8) -0.066(7) S12 0.173(7) 0.110(5) 0.083(5) -0.007(4) -0.006(5) 0.049(5) S13 0.068(4) 0.130(5) 0.105(5) -0.034(4) 0.001(3) 0.020(4) S14 0.079(4) 0.084(4) 0.119(6) -0.010(4) -0.002(4) 0.029(3) S21 0.078(4) 0.101(5) 0.188(8) 0.048(5) -0.030(4) -0.026(4) S22 0.150(7) 0.124(6) 0.110(6) 0.002(5) 0.032(5) 0.044(5) S23 0.068(4) 0.127(5) 0.084(5) 0.000(4) -0.001(3) 0.015(3) S24 0.078(4) 0.081(4) 0.206(9) 0.014(5) 0.030(5) 0.001(3) S31 0.063(3) 0.083(4) 0.070(4) 0.020(3) 0.005(3) -0.010(3) S32 0.154(6) 0.068(4) 0.104(5) 0.019(4) 0.071(5) 0.017(4) S33 0.094(4) 0.093(4) 0.077(4) -0.005(3) 0.009(3) 0.031(3) S34 0.060(3) 0.091(5) 0.187(8) 0.040(5) 0.028(4) -0.003(3) S41 0.204(10) 0.205(10) 0.155(9) -0.015(7) 0.095(8) -0.076(8) S42 0.156(7) 0.103(5) 0.093(6) -0.037(4) 0.021(5) -0.002(4) S43 0.086(4) 0.152(6) 0.114(6) -0.059(5) -0.018(4) 0.053(4) S44 0.100(4) 0.075(4) 0.107(5) 0.008(4) 0.033(4) 0.029(3) La 0.0555(6) 0.0651(7) 0.0697(9) 0.0067(7) 0.0223(6) 0.0018(5) O3 0.106(13) 0.124(14) 0.152(18) 0.066(13) 0.033(12) -0.021(11) O4 0.072(10) 0.149(17) 0.151(17) 0.021(14) 0.035(10) -0.027(11) O5 0.115(14) 0.190(19) 0.051(12) -0.005(12) 0.028(10) 0.006(12) O6 0.139(14) 0.107(13) 0.064(12) -0.026(10) 0.036(10) 0.009(10) O7 0.063(9) 0.118(12) 0.113(13) 0.009(10) 0.018(8) -0.004(9) N3 0.172(22) 0.127(19) 0.111(19) 0.019(16) 0.073(17) -0.018(16) N4 0.114(16) 0.106(16) 0.106(17) 0.041(13) 0.009(13) -0.052(13) N5 0.081(12) 0.081(13) 0.094(16) 0.014(11) 0.008(11) 0.009(9) N6 0.079(13) 0.161(19) 0.060(14) -0.024(13) 0.003(10) -0.014(12) N7 0.095(16) 0.124(18) 0.206(26) -0.052(18) 0.072(16) -0.057(13) C3 0.087(16) 0.126(22) 0.090(20) 0.057(17) 0.034(14) -0.018(15) C4 0.071(16) 0.137(25) 0.090(20) 0.034(18) 0.015(14) -0.013(15) C5 0.156(26) 0.091(17) 0.059(19) 0.001(15) 0.069(19) -0.026(17) C6 0.159(24) 0.056(14) 0.070(19) 0.013(13) 0.070(19) 0.039(14) C7 0.038(12) 0.139(22) 0.122(22) 0.037(17) 0.012(13) -0.021(13) C8 0.107(23) 0.240(41) 0.144(30) 0.101(30) 0.067(21) 0.069(25) O8 0.088(12) 0.095(12) 0.109(14) 0.031(10) -0.001(10) 0.014(9) N8 0.132(18) 0.075(13) 0.124(20) 0.020(13) -0.015(14) 0.018(12) C2 0.090(19) 0.112(21) 0.152(29) 0.062(20) 0.010(19) 0.027(17) O2 0.102(13) 0.166(18) 0.117(16) 0.036(13) -0.016(12) 0.001(13) N2 0.080(14) 0.106(16) 0.185(25) -0.009(16) 0.011(15) 0.005(12) _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 W1 S11 2.125(8) . ? W1 S12 2.179(7) . ? W1 S14 2.183(6) . ? W1 S13 2.258(6) . ? W1 Ag1 2.941(2) . ? W1 Ag5 2.956(2) 4_676 ? W2 S22 2.180(8) . ? W2 S21 2.191(6) . ? W2 S24 2.221(6) . ? W2 S23 2.227(6) . ? W2 Ag2 2.946(2) . ? W2 Ag1 2.968(2) . ? W2 Ag4 2.977(2) 4_676 ? W3 S33 2.167(6) . ? W3 S34 2.178(6) . ? W3 S32 2.230(7) . ? W3 S31 2.239(5) . ? W3 Ag2 2.953(2) . ? W3 Ag5 2.962(2) . ? W3 Ag3 3.015(2) . ? W4 S41 2.130(9) . ? W4 S44 2.175(6) . ? W4 S42 2.184(7) . ? W4 S43 2.242(6) . ? W4 Ag3 2.946(2) . ? W4 Ag4 2.950(2) . ? Ag1 S12 2.531(7) . ? Ag1 S13 2.541(7) . ? Ag1 S21 2.546(6) . ? Ag1 S24 2.549(7) . ? Ag2 S23 2.516(6) . ? Ag2 S22 2.525(7) . ? Ag2 S34 2.528(6) . ? Ag2 S31 2.545(5) . ? Ag3 S44 2.499(6) . ? Ag3 S32 2.528(7) . ? Ag3 S43 2.553(6) . ? Ag3 S31 2.602(6) . ? Ag4 S42 2.519(7) . ? Ag4 S43 2.540(8) . ? Ag4 S23 2.545(6) 4_575 ? Ag4 S24 2.555(8) 4_575 ? Ag4 W2 2.977(2) 4_575 ? Ag5 S13 2.518(6) 4_575 ? Ag5 S32 2.530(6) . ? Ag5 S33 2.535(6) . ? Ag5 S14 2.547(6) 4_575 ? Ag5 W1 2.956(2) 4_575 ? S13 Ag5 2.518(6) 4_676 ? S14 Ag5 2.547(6) 4_676 ? S23 Ag4 2.545(6) 4_676 ? S24 Ag4 2.555(8) 4_676 ? La O2 2.44(2) . ? La O1 2.44(3) . ? La O5 2.44(2) . ? La O3 2.45(2) . ? La O6 2.46(2) . ? La O4 2.46(2) . ? La O7 2.464(14) . ? La O8 2.537(14) . ? O3 C3 1.25(3) . ? O4 C4 1.26(3) . ? O5 C5 1.20(3) . ? O6 C6 1.22(3) . ? O7 C7 1.26(2) . ? N3 C3 1.27(3) . ? N3 C32 1.73(6) . ? N3 C33 1.81(5) . ? N4 C4 1.35(3) . ? N4 C41 1.55(4) . ? N4 C43 1.56(3) . ? N5 C5 1.28(2) . ? N5 C53 1.51(3) . ? N5 C51 1.60(4) . ? N6 C6 1.33(3) . ? N6 C61 1.52(3) . ? N6 C63 1.54(4) . ? N7 C7 1.29(3) . ? N7 C73 1.58(4) . ? N7 C71 1.71(3) . ? C31 C32 1.21(8) . ? C33 C34 1.12(7) . ? C41 C42 1.56(4) . ? C43 C44 1.49(4) . ? C51 C52 1.29(4) . ? C53 C54 1.50(4) . ? C61 C62 1.42(4) . ? C63 C64 1.43(4) . ? C71 C72 0.92(9) . ? C73 C74 1.47(5) . ? C8 O8 1.19(2) . ? C8 N8 1.35(2) . ? N8 C81 1.48(4) . ? N8 C83 1.58(3) . ? C81 C82 1.56(4) . ? C83 C84 1.44(4) . ? C1 O1 1.23(3) . ? C1 N1 1.43(3) . ? N1 C11 1.56(4) . ? N1 C13 1.58(4) . ? C11 C12 1.60(4) . ? C13 C14 1.48(4) . ? C14 C14 1.38(7) 3_655 ? C2 O2 1.17(2) . ? C2 N2 1.32(2) . ? N2 C21 1.51(4) . ? N2 C23 1.58(3) . ? C21 C22 1.61(4) . ? C23 C24 1.53(4) . ? 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 S11 W1 S12 107.2(4) . . ? S11 W1 S14 106.9(4) . . ? S12 W1 S14 108.1(3) . . ? S11 W1 S13 108.0(4) . . ? S12 W1 S13 113.5(2) . . ? S14 W1 S13 112.9(2) . . ? S11 W1 Ag1 127.3(3) . . ? S12 W1 Ag1 56.9(2) . . ? S14 W1 Ag1 125.7(2) . . ? S13 W1 Ag1 56.7(2) . . ? S11 W1 Ag5 124.4(3) . 4_676 ? S12 W1 Ag5 128.3(2) . 4_676 ? S14 W1 Ag5 57.1(2) . 4_676 ? S13 W1 Ag5 55.8(2) . 4_676 ? Ag1 W1 Ag5 90.22(6) . 4_676 ? S22 W2 S21 107.2(3) . . ? S22 W2 S24 105.6(3) . . ? S21 W2 S24 112.1(2) . . ? S22 W2 S23 112.7(2) . . ? S21 W2 S23 106.2(3) . . ? S24 W2 S23 113.0(3) . . ? S22 W2 Ag2 56.7(2) . . ? S21 W2 Ag2 124.9(2) . . ? S24 W2 Ag2 122.9(2) . . ? S23 W2 Ag2 56.2(2) . . ? S22 W2 Ag1 130.8(2) . . ? S21 W2 Ag1 56.8(2) . . ? S24 W2 Ag1 56.7(2) . . ? S23 W2 Ag1 116.4(2) . . ? Ag2 W2 Ag1 172.40(7) . . ? S22 W2 Ag4 125.9(2) . 4_676 ? S21 W2 Ag4 126.9(2) . 4_676 ? S24 W2 Ag4 56.7(2) . 4_676 ? S23 W2 Ag4 56.4(2) . 4_676 ? Ag2 W2 Ag4 88.82(6) . 4_676 ? Ag1 W2 Ag4 85.03(6) . 4_676 ? S33 W3 S34 106.5(3) . . ? S33 W3 S32 112.7(2) . . ? S34 W3 S32 105.8(3) . . ? S33 W3 S31 107.3(2) . . ? S34 W3 S31 112.9(2) . . ? S32 W3 S31 111.5(2) . . ? S33 W3 Ag2 128.1(2) . . ? S34 W3 Ag2 56.7(2) . . ? S32 W3 Ag2 119.0(2) . . ? S31 W3 Ag2 56.71(13) . . ? S33 W3 Ag5 56.7(2) . . ? S34 W3 Ag5 124.0(2) . . ? S32 W3 Ag5 56.2(2) . . ? S31 W3 Ag5 123.03(13) . . ? Ag2 W3 Ag5 175.17(7) . . ? S33 W3 Ag3 119.3(2) . . ? S34 W3 Ag3 134.2(2) . . ? S32 W3 Ag3 55.2(2) . . ? S31 W3 Ag3 57.11(14) . . ? Ag2 W3 Ag3 93.82(5) . . ? Ag5 W3 Ag3 82.62(5) . . ? S41 W4 S44 107.6(4) . . ? S41 W4 S42 107.2(3) . . ? S44 W4 S42 107.7(3) . . ? S41 W4 S43 108.3(4) . . ? S44 W4 S43 112.9(2) . . ? S42 W4 S43 112.8(3) . . ? S41 W4 Ag3 120.6(3) . . ? S44 W4 Ag3 56.0(2) . . ? S42 W4 Ag3 132.1(2) . . ? S43 W4 Ag3 57.0(2) . . ? S41 W4 Ag4 127.4(3) . . ? S44 W4 Ag4 124.8(2) . . ? S42 W4 Ag4 56.4(2) . . ? S43 W4 Ag4 56.6(2) . . ? Ag3 W4 Ag4 93.89(6) . . ? S12 Ag1 S13 94.1(2) . . ? S12 Ag1 S21 113.2(3) . . ? S13 Ag1 S21 117.6(3) . . ? S12 Ag1 S24 118.0(3) . . ? S13 Ag1 S24 123.8(3) . . ? S21 Ag1 S24 91.9(2) . . ? S12 Ag1 W1 46.2(2) . . ? S13 Ag1 W1 47.98(14) . . ? S21 Ag1 W1 131.7(2) . . ? S24 Ag1 W1 136.0(2) . . ? S12 Ag1 W2 135.6(2) . . ? S13 Ag1 W2 129.9(2) . . ? S21 Ag1 W2 46.04(15) . . ? S24 Ag1 W2 46.71(15) . . ? W1 Ag1 W2 176.79(9) . . ? S23 Ag2 S22 93.4(2) . . ? S23 Ag2 S34 119.5(3) . . ? S22 Ag2 S34 118.0(3) . . ? S23 Ag2 S31 116.7(2) . . ? S22 Ag2 S31 118.5(2) . . ? S34 Ag2 S31 93.0(2) . . ? S23 Ag2 W2 47.33(15) . . ? S22 Ag2 W2 46.2(2) . . ? S34 Ag2 W2 131.89(15) . . ? S31 Ag2 W2 135.07(14) . . ? S23 Ag2 W3 137.6(2) . . ? S22 Ag2 W3 129.0(2) . . ? S34 Ag2 W3 46.02(14) . . ? S31 Ag2 W3 47.34(12) . . ? W2 Ag2 W3 174.71(9) . . ? S44 Ag3 S32 120.2(2) . . ? S44 Ag3 S43 93.6(2) . . ? S32 Ag3 S43 119.1(3) . . ? S44 Ag3 S31 118.8(2) . . ? S32 Ag3 S31 92.1(2) . . ? S43 Ag3 S31 115.3(2) . . ? S44 Ag3 W4 46.20(15) . . ? S32 Ag3 W4 138.6(2) . . ? S43 Ag3 W4 47.5(2) . . ? S31 Ag3 W4 129.24(13) . . ? S44 Ag3 W3 141.0(2) . . ? S32 Ag3 W3 46.4(2) . . ? S43 Ag3 W3 125.3(2) . . ? S31 Ag3 W3 46.25(11) . . ? W4 Ag3 W3 171.43(8) . . ? S42 Ag4 S43 93.6(2) . . ? S42 Ag4 S23 116.6(2) . 4_575 ? S43 Ag4 S23 114.5(2) . 4_575 ? S42 Ag4 S24 119.6(3) . 4_575 ? S43 Ag4 S24 121.2(3) . 4_575 ? S23 Ag4 S24 93.3(2) 4_575 4_575 ? S42 Ag4 W4 46.2(2) . . ? S43 Ag4 W4 47.5(2) . . ? S23 Ag4 W4 131.9(2) 4_575 . ? S24 Ag4 W4 134.8(2) 4_575 . ? S42 Ag4 W2 133.0(2) . 4_575 ? S43 Ag4 W2 133.1(2) . 4_575 ? S23 Ag4 W2 46.8(2) 4_575 4_575 ? S24 Ag4 W2 46.57(15) 4_575 4_575 ? W4 Ag4 W2 178.49(9) . 4_575 ? S13 Ag5 S32 130.6(3) 4_575 . ? S13 Ag5 S33 116.2(2) 4_575 . ? S32 Ag5 S33 92.6(2) . . ? S13 Ag5 S14 93.9(2) 4_575 4_575 ? S32 Ag5 S14 109.6(2) . 4_575 ? S33 Ag5 S14 115.3(2) . 4_575 ? S13 Ag5 W1 47.91(15) 4_575 4_575 ? S32 Ag5 W1 134.9(2) . 4_575 ? S33 Ag5 W1 130.59(14) . 4_575 ? S14 Ag5 W1 46.02(13) 4_575 4_575 ? S13 Ag5 W3 139.4(2) 4_575 . ? S32 Ag5 W3 47.1(2) . . ? S33 Ag5 W3 45.61(13) . . ? S14 Ag5 W3 126.24(15) 4_575 . ? W1 Ag5 W3 171.42(7) 4_575 . ? W1 S12 Ag1 76.9(2) . . ? W1 S13 Ag5 76.3(2) . 4_676 ? W1 S13 Ag1 75.3(2) . . ? Ag5 S13 Ag1 111.3(3) 4_676 . ? W1 S14 Ag5 76.9(2) . 4_676 ? W2 S21 Ag1 77.2(2) . . ? W2 S22 Ag2 77.1(2) . . ? W2 S23 Ag2 76.5(2) . . ? W2 S23 Ag4 76.9(2) . 4_676 ? Ag2 S23 Ag4 110.0(3) . 4_676 ? W2 S24 Ag1 76.6(2) . . ? W2 S24 Ag4 76.8(2) . 4_676 ? Ag1 S24 Ag4 103.8(3) . 4_676 ? W3 S31 Ag2 75.95(15) . . ? W3 S31 Ag3 76.6(2) . . ? Ag2 S31 Ag3 115.7(2) . . ? W3 S32 Ag3 78.4(2) . . ? W3 S32 Ag5 76.7(2) . . ? Ag3 S32 Ag5 102.6(2) . . ? W3 S33 Ag5 77.7(2) . . ? W3 S34 Ag2 77.3(2) . . ? W4 S42 Ag4 77.3(2) . . ? W4 S43 Ag4 75.9(2) . . ? W4 S43 Ag3 75.5(2) . . ? Ag4 S43 Ag3 115.6(3) . . ? W4 S44 Ag3 77.8(2) . . ? O2 La O1 71.5(8) . . ? O2 La O5 136.5(7) . . ? O1 La O5 71.4(8) . . ? O2 La O3 72.9(6) . . ? O1 La O3 73.5(8) . . ? O5 La O3 116.5(7) . . ? O2 La O6 72.1(6) . . ? O1 La O6 142.5(7) . . ? O5 La O6 145.4(6) . . ? O3 La O6 87.4(6) . . ? O2 La O4 74.0(6) . . ? O1 La O4 83.1(8) . . ? O5 La O4 79.6(6) . . ? O3 La O4 144.1(6) . . ? O6 La O4 95.5(6) . . ? O2 La O7 138.3(6) . . ? O1 La O7 117.0(7) . . ? O5 La O7 79.9(5) . . ? O3 La O7 71.4(5) . . ? O6 La O7 85.4(5) . . ? O4 La O7 144.5(6) . . ? O2 La O8 128.7(6) . . ? O1 La O8 139.6(8) . . ? O5 La O8 72.6(6) . . ? O3 La O8 140.9(6) . . ? O6 La O8 73.2(6) . . ? O4 La O8 73.0(6) . . ? O7 La O8 73.4(5) . . ? C3 O3 La 145.3(16) . . ? C4 O4 La 136.5(17) . . ? C5 O5 La 141.9(17) . . ? C6 O6 La 137.1(16) . . ? C7 O7 La 139.1(15) . . ? C3 N3 C32 112.8(28) . . ? C3 N3 C33 121.9(28) . . ? C32 N3 C33 124.2(29) . . ? C4 N4 C41 123.5(23) . . ? C4 N4 C43 112.0(26) . . ? C41 N4 C43 124.5(23) . . ? C5 N5 C53 121.9(21) . . ? C5 N5 C51 123.1(24) . . ? C53 N5 C51 115.0(22) . . ? C6 N6 C61 120.8(21) . . ? C6 N6 C63 120.8(23) . . ? C61 N6 C63 117.8(21) . . ? C7 N7 C73 122.0(23) . . ? C7 N7 C71 120.6(29) . . ? C73 N7 C71 110.7(29) . . ? O3 C3 N3 122.9(28) . . ? O4 C4 N4 116.2(26) . . ? O5 C5 N5 124.3(26) . . ? O6 C6 N6 120.6(25) . . ? O7 C7 N7 115.9(26) . . ? C31 C32 N3 89.3(55) . . ? C34 C33 N3 93.1(54) . . ? N4 C41 C42 105.9(27) . . ? C44 C43 N4 107.2(25) . . ? C52 C51 N5 106.9(33) . . ? C54 C53 N5 107.1(22) . . ? C62 C61 N6 105.3(27) . . ? C64 C63 N6 108.0(29) . . ? C72 C71 N7 108.8(63) . . ? C74 C73 N7 99.0(34) . . ? O8 C8 N8 123.5(23) . . ? C8 O8 La 134.0(18) . . ? C8 N8 C81 117.9(23) . . ? C8 N8 C83 129.1(22) . . ? C81 N8 C83 112.4(21) . . ? N8 C81 C82 97.4(27) . . ? C84 C83 N8 97.4(25) . . ? O1 C1 N1 109.4(25) . . ? C1 O1 La 121.6(24) . . ? C1 N1 C11 107.9(23) . . ? C1 N1 C13 128.3(29) . . ? C11 N1 C13 105.6(24) . . ? N1 C11 C12 91.7(26) . . ? C14 C13 N1 95.7(27) . . ? C14 C14 C13 116.9(60) 3_655 . ? O2 C2 N2 124.7(23) . . ? C2 O2 La 145.3(20) . . ? C2 N2 C21 117.4(23) . . ? C2 N2 C23 134.4(23) . . ? C21 N2 C23 108.2(23) . . ? N2 C21 C22 94.4(28) . . ? C24 C23 N2 90.7(25) . . ? _refine_diff_density_max 0.994 _refine_diff_density_min -1.200 _refine_diff_density_rms 0.166 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA ; data_complex3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C80 H176 Ag10 N16 Nd2 O16 S32 W8' _chemical_formula_weight 5482.27 _chemical_melting_point ? _chemical_compound_source ? 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' 'Nd' 'Nd' -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monolinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 21.6360(9) _cell_length_b 17.9851(8) _cell_length_c 22.0251(9) _cell_angle_alpha 90.00 _cell_angle_beta 108.2570(10) _cell_angle_gamma 90.00 _cell_volume 8139.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.49 _cell_measurement_theta_max 23.27 _exptl_crystal_description 'rhombic' _exptl_crystal_colour 'red' _exptl_crystal_size_max .82 _exptl_crystal_size_mid .70 _exptl_crystal_size_min .55 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.237 _exptl_crystal_density_method ? _exptl_crystal_F_000 5180 _exptl_absorpt_coefficient_mu 7.880 _exptl_absorpt_correction_type 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .0255 _exptl_absorpt_correction_T_max .0776 _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 'Siemens SMART CCD' _diffrn_measurement_method ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 26838 _diffrn_reflns_av_R_equivalents 0.0668 _diffrn_reflns_av_sigmaI/netI 0.0927 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 23.27 _reflns_number_total 11501 _reflns_number_observed 7239 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 8 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0521P)^2^+110.2108P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11493 _refine_ls_number_parameters 561 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1234 _refine_ls_R_factor_obs 0.0779 _refine_ls_wR_factor_all 0.1980 _refine_ls_wR_factor_obs 0.1740 _refine_ls_goodness_of_fit_all 1.061 _refine_ls_goodness_of_fit_obs 1.202 _refine_ls_restrained_S_all 1.076 _refine_ls_restrained_S_obs 1.201 _refine_ls_shift/esd_max 0.063 _refine_ls_shift/esd_mean 0.003 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W1 W 0.81435(5) 0.35920(6) 0.54095(5) 0.0862(3) Uani 1 d . . W2 W 0.95890(4) 0.12479(5) 0.71833(5) 0.0846(3) Uani 1 d . . W3 W 0.78327(4) -0.08909(5) 0.54302(4) 0.0790(3) Uani 1 d . . W4 W 0.63304(4) 0.14432(5) 0.37058(4) 0.0668(3) Uani 1 d . . Ag1 Ag 0.71762(9) 0.25595(11) 0.46133(9) 0.0935(6) Uani 1 d . . Ag2 Ag 0.88514(11) 0.24199(13) 0.62909(11) 0.1189(8) Uani 1 d . . Ag3 Ag 0.86890(10) 0.01780(12) 0.63160(10) 0.1113(7) Uani 1 d . . Ag4 Ag 0.71741(9) 0.03643(10) 0.46177(9) 0.0908(6) Uani 1 d . . Ag5 Ag 0.54845(9) 0.25858(11) 0.28955(9) 0.0978(6) Uani 1 d . . S11 S 0.8532(5) 0.4450(7) 0.4962(5) 0.184(5) Uani 1 d . . S12 S 0.8538(4) 0.3724(4) 0.6451(3) 0.115(2) Uani 1 d . . S13 S 0.8409(3) 0.2514(5) 0.5065(3) 0.130(3) Uani 1 d . . S14 S 0.7086(3) 0.3770(4) 0.5122(3) 0.096(2) Uani 1 d . . S21 S 0.9933(4) 0.1322(5) 0.8232(3) 0.128(3) Uani 1 d . . S22 S 0.9894(3) 0.0171(4) 0.6942(4) 0.136(3) Uani 1 d . . S23 S 0.8517(3) 0.1354(4) 0.6882(5) 0.126(3) Uani 1 d . . S24 S 1.0057(3) 0.2091(4) 0.6725(3) 0.096(2) Uani 1 d . . S31 S 0.8076(6) -0.1922(5) 0.5081(5) 0.184(5) Uani 1 d . . S32 S 0.6767(3) -0.0803(4) 0.5046(3) 0.101(2) Uani 1 d . . S33 S 0.8356(3) 0.0036(4) 0.5109(3) 0.101(2) Uani 1 d . . S34 S 0.8107(4) -0.0993(4) 0.6471(3) 0.133(3) Uani 1 d . . S41 S 0.5284(3) 0.1305(4) 0.3263(4) 0.102(2) Uani 1 d . . S42 S 0.6710(3) 0.2461(3) 0.3371(3) 0.082(2) Uani 1 d . . S43 S 0.6511(3) 0.1471(3) 0.4765(3) 0.095(2) Uani 1 d . . S44 S 0.6792(3) 0.0498(3) 0.3400(3) 0.088(2) Uani 1 d . . Nd Nd 0.53216(5) 0.77646(6) 0.29519(5) 0.0637(3) Uani 1 d . . O3 O 0.5693(7) 0.8805(10) 0.2490(9) 0.115(6) Uani 1 d . . O4 O 0.6477(7) 0.7819(9) 0.3367(8) 0.093(5) Uani 1 d . . O5 O 0.5693(8) 0.6535(9) 0.3371(8) 0.104(5) Uani 1 d . . O6 O 0.4357(7) 0.7085(9) 0.2938(7) 0.093(5) Uani 1 d . . O7 O 0.5446(8) 0.7818(10) 0.4079(8) 0.107(6) Uani 1 d . . N3 N 0.5615(14) 0.9728(15) 0.1777(12) 0.143(10) Uani 1 d . . N4 N 0.7412(12) 0.8162(14) 0.3297(12) 0.133(9) Uani 1 d . . N5 N 0.6282(10) 0.5479(11) 0.3663(10) 0.107(7) Uani 1 d . . N6 N 0.3688(10) 0.6285(12) 0.3181(10) 0.107(7) Uani 1 d . . N7 N 0.5705(9) 0.7551(10) 0.5131(8) 0.087(5) Uani 1 d . . C3 C 0.5556(12) 0.9427(16) 0.2299(14) 0.104(9) Uani 1 d . . C4 C 0.6912(12) 0.8240(16) 0.3476(13) 0.103(8) Uani 1 d . . C5 C 0.5986(15) 0.6003(19) 0.3259(14) 0.127(11) Uani 1 d . . C6 C 0.4189(12) 0.6452(14) 0.2969(12) 0.096(8) Uani 1 d . . C7 C 0.5877(13) 0.7673(11) 0.4586(12) 0.085(7) Uani 1 d . . C311 C 0.5246(24) 1.0439(29) 0.1323(23) 0.210(19) Uiso 1 d . . C312 C 0.5689(26) 1.0859(31) 0.1456(24) 0.235(22) Uiso 1 d . . C321 C 0.6155(41) 0.9370(48) 0.1600(40) 0.365(43) Uiso 1 d . . C322 C 0.5767(29) 0.8912(35) 0.1241(29) 0.264(26) Uiso 1 d . . C411 C 0.7401(21) 0.7540(27) 0.2800(22) 0.202(17) Uiso 1 d . . C412 C 0.7711(22) 0.6926(27) 0.3235(22) 0.212(18) Uiso 1 d . . C421 C 0.7945(26) 0.8738(28) 0.3449(23) 0.210(19) Uiso 1 d . . C422 C 0.8354(30) 0.8826(35) 0.3240(29) 0.278(29) Uiso 1 d . . C511 C 0.6432(23) 0.5609(25) 0.4422(22) 0.202(17) Uiso 1 d . . C512 C 0.5815(25) 0.5308(28) 0.4381(22) 0.231(20) Uiso 1 d . . C521 C 0.6521(19) 0.4674(21) 0.3375(17) 0.164(13) Uiso 1 d . . C522 C 0.7137(26) 0.4860(30) 0.3482(24) 0.248(22) Uiso 1 d . . C611 C 0.3491(16) 0.5470(21) 0.3119(17) 0.157(12) Uiso 1 d . . C612 C 0.3810(18) 0.5108(22) 0.3806(18) 0.174(14) Uiso 1 d . . C621 C 0.3289(17) 0.6867(20) 0.3374(16) 0.144(11) Uiso 1 d . . C622 C 0.2736(19) 0.7085(22) 0.2760(19) 0.184(15) Uiso 1 d . . C711 C 0.6225(16) 0.7280(19) 0.5742(16) 0.146(11) Uiso 1 d . . C712 C 0.6311(17) 0.7871(20) 0.6191(17) 0.158(12) Uiso 1 d . . C721 C 0.5017(12) 0.7615(14) 0.5129(12) 0.101(7) Uiso 1 d . . C722 C 0.4725(14) 0.6820(18) 0.4979(15) 0.137(10) Uiso 1 d . . O8 O 0.5476(8) 0.7037(9) 0.2074(7) 0.100(5) Uani 1 d D . C8 C 0.5128(12) 0.6793(13) 0.1556(10) 0.093(7) Uani 1 d D . N8 N 0.5419(8) 0.6560(12) 0.1142(8) 0.101(7) Uani 1 d D . C811 C 0.6155(15) 0.6650(19) 0.1241(15) 0.150(11) Uiso 1 d D . C812 C 0.6439(19) 0.5899(24) 0.1519(21) 0.214(18) Uiso 1 d D . C821 C 0.5060(15) 0.6053(18) 0.0576(15) 0.153(12) Uiso 1 d D . C822 C 0.4995(19) 0.6537(22) 0.0041(16) 0.184(15) Uiso 1 d D . O1 O 0.4645(12) 0.8767(15) 0.3121(12) 0.183(9) Uiso 1 d D . C1 C 0.4904(19) 0.9205(30) 0.3591(25) 0.331(33) Uiso 1 d D . N1 N 0.4466(21) 0.9451(23) 0.3882(17) 0.374 Uiso 1 d D . C111 C 0.3708(22) 0.9299(29) 0.3566(27) 0.299(28) Uiso 1 d D . C112 C 0.3585(29) 0.9881(41) 0.3006(30) 0.380 Uiso 1 d D . C121 C 0.4548(25) 1.0263(25) 0.4148(24) 0.359 Uiso 1 d D . C122 C 0.5030(25) 1.0137(27) 0.4755(18) 0.227(21) Uiso 1 d D . O2 O 0.4474(8) 0.8085(11) 0.1956(10) 0.148(8) Uani 1 d D . C2 C 0.3881(12) 0.8051(17) 0.1677(14) 0.135(11) Uani 1 d D . N2 N 0.3591(10) 0.8576(16) 0.1266(12) 0.167(13) Uani 1 d D . C211 C 0.3947(27) 0.9178(28) 0.0998(32) 0.442(53) Uiso 1 d D . C212 C 0.4198(34) 0.8708(43) 0.0527(31) 0.387(41) Uiso 1 d D . C221 C 0.2839(17) 0.8635(26) 0.0995(22) 0.245(22) Uiso 1 d D . C222 C 0.2752(31) 0.9152(46) 0.1481(38) 0.462(52) Uiso 1 d D . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0975(7) 0.0893(7) 0.0737(6) -0.0116(6) 0.0297(5) -0.0041(5) W2 0.0749(6) 0.0731(7) 0.0917(7) -0.0197(6) 0.0057(5) -0.0048(5) W3 0.0863(6) 0.0630(6) 0.0702(6) 0.0014(5) -0.0008(5) 0.0021(5) W4 0.0670(5) 0.0595(5) 0.0744(6) 0.0150(5) 0.0225(4) 0.0049(4) Ag1 0.0952(13) 0.0861(13) 0.0907(13) -0.0056(11) 0.0169(10) 0.0000(10) Ag2 0.1085(15) 0.109(2) 0.116(2) -0.0103(14) 0.0005(12) 0.0233(13) Ag3 0.1006(14) 0.0972(15) 0.1058(15) -0.0137(13) -0.0111(11) -0.0195(11) Ag4 0.0929(12) 0.0763(12) 0.0912(13) 0.0192(11) 0.0116(10) 0.0108(9) Ag5 0.0950(13) 0.0876(13) 0.0959(14) 0.0270(11) 0.0084(10) 0.0199(10) S11 0.206(10) 0.215(11) 0.156(8) 0.003(8) 0.095(8) -0.086(9) S12 0.160(7) 0.089(5) 0.082(4) -0.023(4) 0.018(4) 0.004(4) S13 0.092(4) 0.171(7) 0.104(5) -0.065(5) -0.005(4) 0.055(5) S14 0.107(5) 0.079(4) 0.112(5) 0.014(4) 0.047(4) 0.034(4) S21 0.151(7) 0.133(7) 0.087(5) 0.009(5) 0.019(4) -0.041(5) S22 0.084(4) 0.100(5) 0.177(7) -0.058(5) -0.028(4) 0.025(4) S23 0.074(4) 0.087(5) 0.211(9) -0.013(5) 0.036(5) 0.006(3) S24 0.073(4) 0.123(6) 0.078(4) -0.002(4) 0.005(3) -0.011(3) S31 0.237(12) 0.111(7) 0.196(10) -0.014(7) 0.057(9) 0.075(7) S32 0.086(4) 0.088(4) 0.111(5) 0.018(4) 0.007(3) -0.024(3) S33 0.062(3) 0.128(6) 0.098(4) 0.021(4) 0.004(3) -0.012(3) S34 0.181(8) 0.111(6) 0.076(4) 0.012(4) -0.006(5) -0.045(5) S41 0.076(4) 0.087(5) 0.137(6) 0.033(4) 0.026(4) -0.002(3) S42 0.075(3) 0.088(4) 0.076(4) 0.030(3) 0.015(3) -0.016(3) S43 0.143(6) 0.070(4) 0.090(4) 0.015(4) 0.064(4) 0.010(4) S44 0.102(4) 0.085(4) 0.075(4) 0.003(3) 0.023(3) 0.024(3) Nd 0.0683(7) 0.0621(7) 0.0677(7) 0.0103(6) 0.0314(5) 0.0078(5) O3 0.094(11) 0.085(12) 0.160(17) 0.052(13) 0.031(11) -0.024(10) O4 0.071(10) 0.091(12) 0.111(12) 0.001(10) 0.018(9) -0.015(9) O5 0.116(13) 0.077(11) 0.113(13) 0.024(11) 0.028(10) 0.027(10) O6 0.081(10) 0.088(12) 0.106(12) 0.033(10) 0.024(8) -0.002(9) O7 0.117(13) 0.132(16) 0.071(10) 0.006(11) 0.025(9) 0.001(11) N3 0.195(27) 0.136(22) 0.130(20) 0.037(19) 0.093(19) 0.001(19) N4 0.117(18) 0.144(21) 0.152(21) -0.058(18) 0.064(16) -0.057(16) N5 0.128(17) 0.063(13) 0.108(16) 0.027(13) 0.005(13) 0.021(11) N6 0.104(15) 0.099(16) 0.104(15) 0.021(13) 0.014(12) -0.047(13) N7 0.102(13) 0.089(14) 0.066(12) 0.005(11) 0.020(10) 0.013(11) C3 0.093(17) 0.091(20) 0.116(21) 0.040(18) 0.015(15) -0.030(15) C4 0.067(15) 0.117(22) 0.134(23) 0.003(19) 0.046(16) 0.011(15) C5 0.148(26) 0.126(26) 0.133(25) 0.071(23) 0.081(21) 0.041(22) C6 0.090(17) 0.072(17) 0.110(20) 0.039(15) 0.008(14) -0.021(13) C7 0.137(21) 0.041(13) 0.085(17) -0.005(13) 0.047(16) -0.003(13) O8 0.135(14) 0.084(12) 0.082(11) 0.001(10) 0.037(10) 0.014(10) C8 0.151(22) 0.077(17) 0.048(13) -0.013(13) 0.028(15) -0.001(15) N8 0.089(13) 0.156(20) 0.055(11) -0.031(13) 0.018(9) -0.005(13) O2 0.084(12) 0.142(17) 0.187(20) 0.053(15) -0.002(12) -0.001(12) C2 0.079(19) 0.174(33) 0.139(26) -0.032(25) 0.015(18) -0.001(20) N2 0.108(18) 0.191(29) 0.142(22) 0.036(21) -0.046(16) 0.041(19) _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 W1 S11 2.140(9) . ? W1 S12 2.196(7) . ? W1 S14 2.198(6) . ? W1 S13 2.221(7) . ? W1 Ag1 2.933(2) . ? W1 Ag2 2.949(2) . ? W2 S22 2.165(7) . ? W2 S21 2.197(7) . ? W2 S23 2.212(6) . ? W2 S24 2.233(7) . ? W2 Ag5 2.951(2) 4_666 ? W2 Ag3 2.969(2) . ? W2 Ag2 2.981(2) . ? W3 S31 2.136(9) . ? W3 S34 2.189(7) . ? W3 S32 2.198(6) . ? W3 S33 2.251(7) . ? W3 Ag3 2.944(2) . ? W3 Ag4 2.955(2) . ? W4 S41 2.180(6) . ? W4 S44 2.182(6) . ? W4 S42 2.225(5) . ? W4 S43 2.243(6) . ? W4 Ag5 2.951(2) . ? W4 Ag4 2.972(2) . ? W4 Ag1 3.014(2) . ? Ag1 S14 2.484(7) . ? Ag1 S43 2.514(7) . ? Ag1 S13 2.538(7) . ? Ag1 S42 2.608(6) . ? Ag2 S12 2.497(7) . ? Ag2 S23 2.547(8) . ? Ag2 S24 2.550(6) . ? Ag2 S13 2.573(8) . ? Ag3 S34 2.531(8) . ? Ag3 S22 2.539(6) . ? Ag3 S33 2.540(7) . ? Ag3 S23 2.542(8) . ? Ag4 S33 2.515(6) . ? Ag4 S43 2.534(6) . ? Ag4 S44 2.558(6) . ? Ag4 S32 2.568(6) . ? Ag5 S24 2.520(6) 4_565 ? Ag5 S41 2.523(6) . ? Ag5 S21 2.527(8) 4_565 ? Ag5 S42 2.537(6) . ? Ag5 W2 2.951(2) 4_565 ? S21 Ag5 2.527(8) 4_666 ? S24 Ag5 2.520(6) 4_666 ? Nd O4 2.380(15) . ? Nd O3 2.39(2) . ? Nd O6 2.41(2) . ? Nd O7 2.41(2) . ? Nd O1 2.42(2) . ? Nd O5 2.43(2) . ? Nd O8 2.443(15) . ? Nd O2 2.45(2) . ? O3 C3 1.20(3) . ? O4 C4 1.17(3) . ? O5 C5 1.21(3) . ? O6 C6 1.20(2) . ? O7 C7 1.24(3) . ? N3 C3 1.31(3) . ? N3 C321 1.49(8) . ? N3 C311 1.67(5) . ? N4 C4 1.27(3) . ? N4 C421 1.51(5) . ? N4 C411 1.56(5) . ? N5 C5 1.32(3) . ? N5 C511 1.62(4) . ? N5 C521 1.72(4) . ? N6 C6 1.34(3) . ? N6 C621 1.50(4) . ? N6 C611 1.52(4) . ? N7 C7 1.38(3) . ? N7 C721 1.49(3) . ? N7 C711 1.54(3) . ? C311 C312 1.18(6) . ? C321 C322 1.26(9) . ? C411 C412 1.48(5) . ? C421 C422 1.13(7) . ? C511 C512 1.42(5) . ? C521 C522 1.32(5) . ? C611 C612 1.59(4) . ? C621 C622 1.55(4) . ? C711 C712 1.42(4) . ? C721 C722 1.56(4) . ? O8 C8 1.23(2) . ? C8 N8 1.33(2) . ? N8 C821 1.54(3) . ? N8 C811 1.55(3) . ? C811 C812 1.53(4) . ? C821 C822 1.44(4) . ? O1 C1 1.28(3) . ? C1 N1 1.37(3) . ? N1 C121 1.56(4) . ? N1 C111 1.59(4) . ? C111 C112 1.58(4) . ? C121 C122 1.43(4) . ? C122 C122 1.23(8) 3_676 ? O2 C2 1.24(2) . ? C2 N2 1.32(3) . ? N2 C221 1.55(3) . ? N2 C211 1.55(4) . ? C211 C212 1.56(5) . ? C221 C222 1.47(4) . ? 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 S11 W1 S12 108.9(4) . . ? S11 W1 S14 106.6(4) . . ? S12 W1 S14 108.3(3) . . ? S11 W1 S13 106.9(4) . . ? S12 W1 S13 113.2(3) . . ? S14 W1 S13 112.7(3) . . ? S11 W1 Ag1 119.4(3) . . ? S12 W1 Ag1 131.6(2) . . ? S14 W1 Ag1 55.7(2) . . ? S13 W1 Ag1 57.0(2) . . ? S11 W1 Ag2 128.4(3) . . ? S12 W1 Ag2 55.8(2) . . ? S14 W1 Ag2 124.9(2) . . ? S13 W1 Ag2 57.6(2) . . ? Ag1 W1 Ag2 93.85(6) . . ? S22 W2 S21 106.5(3) . . ? S22 W2 S23 112.0(3) . . ? S21 W2 S23 106.7(3) . . ? S22 W2 S24 106.3(3) . . ? S21 W2 S24 112.5(3) . . ? S23 W2 S24 112.8(3) . . ? S22 W2 Ag5 124.5(2) . 4_666 ? S21 W2 Ag5 56.5(2) . 4_666 ? S23 W2 Ag5 123.4(2) . 4_666 ? S24 W2 Ag5 56.1(2) . 4_666 ? S22 W2 Ag3 56.7(2) . . ? S21 W2 Ag3 130.8(2) . . ? S23 W2 Ag3 56.5(2) . . ? S24 W2 Ag3 116.6(2) . . ? Ag5 W2 Ag3 172.64(7) 4_666 . ? S22 W2 Ag2 127.7(2) . . ? S21 W2 Ag2 125.8(2) . . ? S23 W2 Ag2 56.4(2) . . ? S24 W2 Ag2 56.4(2) . . ? Ag5 W2 Ag2 88.55(6) 4_666 . ? Ag3 W2 Ag2 85.77(6) . . ? S31 W3 S34 106.7(4) . . ? S31 W3 S32 105.7(4) . . ? S34 W3 S32 108.5(3) . . ? S31 W3 S33 108.9(4) . . ? S34 W3 S33 113.2(3) . . ? S32 W3 S33 113.4(2) . . ? S31 W3 Ag3 129.1(3) . . ? S34 W3 Ag3 56.8(2) . . ? S32 W3 Ag3 125.1(2) . . ? S33 W3 Ag3 56.7(2) . . ? S31 W3 Ag4 124.9(3) . . ? S34 W3 Ag4 128.3(2) . . ? S32 W3 Ag4 57.6(2) . . ? S33 W3 Ag4 55.8(2) . . ? Ag3 W3 Ag4 89.22(6) . . ? S41 W4 S44 106.6(3) . . ? S41 W4 S42 112.6(2) . . ? S44 W4 S42 106.7(2) . . ? S41 W4 S43 106.6(3) . . ? S44 W4 S43 113.0(2) . . ? S42 W4 S43 111.4(2) . . ? S41 W4 Ag5 56.5(2) . . ? S44 W4 Ag5 127.8(2) . . ? S42 W4 Ag5 56.63(15) . . ? S43 W4 Ag5 119.1(2) . . ? S41 W4 Ag4 124.1(2) . . ? S44 W4 Ag4 57.1(2) . . ? S42 W4 Ag4 123.29(15) . . ? S43 W4 Ag4 56.1(2) . . ? Ag5 W4 Ag4 175.13(6) . . ? S41 W4 Ag1 134.6(2) . . ? S44 W4 Ag1 118.8(2) . . ? S42 W4 Ag1 57.4(2) . . ? S43 W4 Ag1 54.8(2) . . ? Ag5 W4 Ag1 94.01(6) . . ? Ag4 W4 Ag1 82.53(6) . . ? S14 Ag1 S43 119.5(2) . . ? S14 Ag1 S13 94.2(2) . . ? S43 Ag1 S13 119.9(3) . . ? S14 Ag1 S42 118.3(2) . . ? S43 Ag1 S42 92.1(2) . . ? S13 Ag1 S42 115.0(2) . . ? S14 Ag1 W1 47.0(2) . . ? S43 Ag1 W1 138.1(2) . . ? S13 Ag1 W1 47.2(2) . . ? S42 Ag1 W1 129.72(14) . . ? S14 Ag1 W4 140.0(2) . . ? S43 Ag1 W4 46.80(15) . . ? S13 Ag1 W4 125.7(2) . . ? S42 Ag1 W4 45.92(12) . . ? W1 Ag1 W4 171.69(8) . . ? S12 Ag2 S23 120.1(3) . . ? S12 Ag2 S24 117.1(3) . . ? S23 Ag2 S24 93.2(2) . . ? S12 Ag2 S13 93.3(2) . . ? S23 Ag2 S13 121.0(3) . . ? S24 Ag2 S13 114.2(2) . . ? S12 Ag2 W1 46.7(2) . . ? S23 Ag2 W1 134.6(2) . . ? S24 Ag2 W1 132.2(2) . . ? S13 Ag2 W1 46.8(2) . . ? S12 Ag2 W2 133.1(2) . . ? S23 Ag2 W2 46.4(2) . . ? S24 Ag2 W2 46.8(2) . . ? S13 Ag2 W2 133.3(2) . . ? W1 Ag2 W2 179.00(10) . . ? S34 Ag3 S22 113.1(3) . . ? S34 Ag3 S33 93.9(2) . . ? S22 Ag3 S33 118.3(3) . . ? S34 Ag3 S23 118.1(3) . . ? S22 Ag3 S23 91.2(2) . . ? S33 Ag3 S23 124.1(3) . . ? S34 Ag3 W3 46.4(2) . . ? S22 Ag3 W3 133.0(2) . . ? S33 Ag3 W3 47.8(2) . . ? S23 Ag3 W3 135.2(2) . . ? S34 Ag3 W2 134.9(2) . . ? S22 Ag3 W2 45.5(2) . . ? S33 Ag3 W2 130.7(2) . . ? S23 Ag3 W2 46.5(2) . . ? W3 Ag3 W2 177.84(10) . . ? S33 Ag4 S43 132.0(3) . . ? S33 Ag4 S44 115.1(2) . . ? S43 Ag4 S44 92.9(2) . . ? S33 Ag4 S32 94.0(2) . . ? S43 Ag4 S32 108.8(2) . . ? S44 Ag4 S32 115.3(2) . . ? S33 Ag4 W3 47.8(2) . . ? S43 Ag4 W3 135.0(2) . . ? S44 Ag4 W3 130.00(15) . . ? S32 Ag4 W3 46.25(14) . . ? S33 Ag4 W4 140.4(2) . . ? S43 Ag4 W4 47.24(14) . . ? S44 Ag4 W4 45.73(13) . . ? S32 Ag4 W4 125.0(2) . . ? W3 Ag4 W4 170.25(8) . . ? S24 Ag5 S41 119.6(2) 4_565 . ? S24 Ag5 S21 93.7(2) 4_565 4_565 ? S41 Ag5 S21 118.1(3) . 4_565 ? S24 Ag5 S42 116.4(2) 4_565 . ? S41 Ag5 S42 92.8(2) . . ? S21 Ag5 S42 118.4(3) 4_565 . ? S24 Ag5 W2 47.4(2) 4_565 4_565 ? S41 Ag5 W2 132.0(2) . 4_565 ? S21 Ag5 W2 46.5(2) 4_565 4_565 ? S42 Ag5 W2 135.18(15) . 4_565 ? S24 Ag5 W4 137.6(2) 4_565 . ? S41 Ag5 W4 46.13(14) . . ? S21 Ag5 W4 128.6(2) 4_565 . ? S42 Ag5 W4 47.08(13) . . ? W2 Ag5 W4 174.70(9) 4_565 . ? W1 S12 Ag2 77.6(2) . . ? W1 S13 Ag1 75.8(2) . . ? W1 S13 Ag2 75.5(2) . . ? Ag1 S13 Ag2 114.4(3) . . ? W1 S14 Ag1 77.3(2) . . ? W2 S21 Ag5 77.0(2) . 4_666 ? W2 S22 Ag3 77.8(2) . . ? W2 S23 Ag3 76.9(2) . . ? W2 S23 Ag2 77.2(2) . . ? Ag3 S23 Ag2 105.5(3) . . ? W2 S24 Ag5 76.5(2) . 4_666 ? W2 S24 Ag2 76.8(2) . . ? Ag5 S24 Ag2 109.6(3) 4_666 . ? W3 S32 Ag4 76.2(2) . . ? W3 S33 Ag4 76.4(2) . . ? W3 S33 Ag3 75.6(2) . . ? Ag4 S33 Ag3 110.1(3) . . ? W3 S34 Ag3 76.8(2) . . ? W4 S41 Ag5 77.4(2) . . ? W4 S42 Ag5 76.3(2) . . ? W4 S42 Ag1 76.7(2) . . ? Ag5 S42 Ag1 116.0(2) . . ? W4 S43 Ag1 78.4(2) . . ? W4 S43 Ag4 76.7(2) . . ? Ag1 S43 Ag4 102.9(2) . . ? W4 S44 Ag4 77.2(2) . . ? O4 Nd O3 71.2(5) . . ? O4 Nd O6 145.8(5) . . ? O3 Nd O6 142.9(5) . . ? O4 Nd O7 80.6(6) . . ? O3 Nd O7 117.6(6) . . ? O6 Nd O7 81.4(6) . . ? O4 Nd O1 121.5(7) . . ? O3 Nd O1 77.4(7) . . ? O6 Nd O1 79.4(7) . . ? O7 Nd O1 72.0(7) . . ? O4 Nd O5 73.1(6) . . ? O3 Nd O5 139.4(6) . . ? O6 Nd O5 74.1(5) . . ? O7 Nd O5 74.3(6) . . ? O1 Nd O5 139.6(7) . . ? O4 Nd O8 86.5(6) . . ? O3 Nd O8 86.3(6) . . ? O6 Nd O8 93.0(6) . . ? O7 Nd O8 146.8(6) . . ? O1 Nd O8 139.4(7) . . ? O5 Nd O8 72.7(6) . . ? O4 Nd O2 137.5(6) . . ? O3 Nd O2 72.0(6) . . ? O6 Nd O2 72.8(6) . . ? O7 Nd O2 136.3(7) . . ? O1 Nd O2 69.1(8) . . ? O5 Nd O2 128.3(7) . . ? O8 Nd O2 70.5(7) . . ? C3 O3 Nd 143.3(18) . . ? C4 O4 Nd 141.7(17) . . ? C5 O5 Nd 140.4(18) . . ? C6 O6 Nd 138.9(16) . . ? C7 O7 Nd 136.8(16) . . ? C3 N3 C321 110.6(40) . . ? C3 N3 C311 133.0(30) . . ? C321 N3 C311 116.3(38) . . ? C4 N4 C421 121.5(31) . . ? C4 N4 C411 118.1(26) . . ? C421 N4 C411 119.4(29) . . ? C5 N5 C511 119.5(26) . . ? C5 N5 C521 119.4(24) . . ? C511 N5 C521 121.0(23) . . ? C6 N6 C621 122.8(22) . . ? C6 N6 C611 114.8(25) . . ? C621 N6 C611 121.8(23) . . ? C7 N7 C721 121.8(19) . . ? C7 N7 C711 119.3(22) . . ? C721 N7 C711 118.8(20) . . ? O3 C3 N3 127.7(31) . . ? O4 C4 N4 124.9(28) . . ? O5 C5 N5 127.0(28) . . ? O6 C6 N6 121.4(26) . . ? O7 C7 N7 119.0(23) . . ? C312 C311 N3 98.2(45) . . ? C322 C321 N3 91.4(65) . . ? C412 C411 N4 100.1(34) . . ? C422 C421 N4 130.4(59) . . ? C512 C511 N5 89.9(34) . . ? C522 C521 N5 97.2(35) . . ? N6 C611 C612 106.5(27) . . ? N6 C621 C622 106.6(28) . . ? C712 C711 N7 105.8(27) . . ? N7 C721 C722 105.5(21) . . ? C8 O8 Nd 136.7(16) . . ? O8 C8 N8 117.7(21) . . ? C8 N8 C821 120.9(19) . . ? C8 N8 C811 124.0(18) . . ? C821 N8 C811 114.2(18) . . ? C812 C811 N8 103.3(25) . . ? C822 C821 N8 101.5(25) . . ? C1 O1 Nd 116.7(25) . . ? O1 C1 N1 112.5(28) . . ? C1 N1 C121 117.5(31) . . ? C1 N1 C111 120.6(25) . . ? C121 N1 C111 107.7(25) . . ? C112 C111 N1 97.2(26) . . ? C122 C121 N1 99.6(29) . . ? C122 C122 C121 129.6(69) 3_676 . ? C2 O2 Nd 143.4(20) . . ? O2 C2 N2 120.0(24) . . ? C2 N2 C221 121.9(24) . . ? C2 N2 C211 125.0(25) . . ? C221 N2 C211 113.1(24) . . ? N2 C211 C212 101.1(30) . . ? C222 C221 N2 96.9(27) . . ? _refine_diff_density_max 1.074 _refine_diff_density_min -1.125 _refine_diff_density_rms 0.172 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA ;