# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 1145/127 #Preparation, Crystal Structures, EHT Band Calculations And Physical #Properties of \k-(EDS-EDT-TTF)2[Ag2(CN)3] and \a-(BETS)2Ag(CN)2. # #Stephane Golhen, Lahcene Ouahab et al. # data_kappa _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H16 Ag2 N3 S12 Se4' _chemical_formula_weight 1250.69 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' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.157(9) _cell_length_b 8.7321(18) _cell_length_c 13.507(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.94(3) _cell_angle_gamma 90.00 _cell_volume 1788(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 4.849 _cell_measurement_theta_max 10.223 _exptl_crystal_description octaedric _exptl_crystal_colour black _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1194 _exptl_absorpt_coefficient_mu 5.894 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Enraf Nonius CAD4' _diffrn_measurement_method \q-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 250 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 5402 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0844 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 29.97 _reflns_number_total 5191 _reflns_number_gt 2572 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf Nonius CAD4' _computing_cell_refinement MolEN _computing_data_reduction MolEN _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^)+(0.0473P)^2^+3.5339P] 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 SHELXL _refine_ls_extinction_coef 0.0018(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5191 _refine_ls_number_parameters 205 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1592 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1337 _refine_ls_wR_factor_gt 0.1069 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.50561(4) 0.23201(6) 0.37378(4) 0.0596(2) Uani 1 1 d . . . Se1 Se 1.30766(8) 0.4369(2) 0.51839(13) 0.1068(8) Uani 0.770(4) 1 d P . . Se2 Se 1.18932(9) 0.16911(16) 0.66714(10) 0.0717(5) Uani 0.686(3) 1 d P . . S3 S 1.13083(11) 0.4667(2) 0.41037(12) 0.0472(4) Uani 1 1 d . . . S4 S 1.03822(10) 0.2410(2) 0.53059(12) 0.0432(4) Uani 1 1 d . . . S5 S 0.95862(11) 0.4753(2) 0.25797(12) 0.0442(4) Uani 1 1 d . . . S6 S 0.87563(10) 0.2407(2) 0.37937(12) 0.0429(4) Uani 1 1 d . . . Se7 Se 0.81346(9) 0.49839(17) 0.10578(9) 0.0678(6) Uani 0.638(3) 1 d P . . Se8 Se 0.70791(5) 0.20044(10) 0.25695(6) 0.0473(3) Uani 0.839(3) 1 d P . . C1 C 1.2992(7) 0.2431(13) 0.6815(9) 0.116(5) Uani 1 1 d . . . H1A H 1.2956 0.3340 0.7225 0.050 Uiso 1 1 calc R . . H1B H 1.3331 0.1680 0.7188 0.050 Uiso 1 1 calc R . . C2 C 1.3484(6) 0.2818(14) 0.5982(10) 0.119(5) Uani 1 1 d . . . H2A H 1.3537 0.1907 0.5577 0.050 Uiso 1 1 calc R . . H2B H 1.4073 0.3090 0.6209 0.050 Uiso 1 1 calc R . . C3 C 1.1908(4) 0.3806(8) 0.5065(5) 0.0451(16) Uani 1 1 d . . . C4 C 1.1479(4) 0.2782(8) 0.5628(5) 0.0424(15) Uani 1 1 d . . . C5 C 1.0359(4) 0.3585(7) 0.4264(4) 0.0374(14) Uani 1 1 d . . . C6 C 0.9653(4) 0.3600(7) 0.3626(4) 0.0366(14) Uani 1 1 d . . . C7 C 0.8161(4) 0.3010(7) 0.2745(4) 0.0369(14) Uani 1 1 d . . . C8 C 0.8548(4) 0.4088(7) 0.2191(4) 0.0394(14) Uani 1 1 d . . . C9 C 0.7224(5) 0.3643(10) 0.0755(5) 0.062(2) Uani 1 1 d . . . H9A H 0.6884 0.4075 0.0208 0.050 Uiso 1 1 calc R . . H9B H 0.7482 0.2696 0.0522 0.050 Uiso 1 1 calc R . . C10 C 0.6610(4) 0.3262(9) 0.1543(5) 0.0519(18) Uani 1 1 d . . . H10A H 0.6103 0.2747 0.1249 0.050 Uiso 1 1 calc R . . H10B H 0.6402 0.4208 0.1835 0.050 Uiso 1 1 calc R . . N12 N 0.5031(4) 0.0514(7) 0.4740(5) 0.0524(17) Uani 0.50 1 d P . . C12 C 0.5031(4) 0.0514(7) 0.4740(5) 0.0524(17) Uani 0.50 1 d P . . C11 C 0.4882(5) 0.4452(8) 0.3136(5) 0.0456(16) Uani 1 1 d . . . N1 N 0.5227(5) 0.0596(7) 0.2247(5) 0.0649(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0662(4) 0.0436(3) 0.0687(4) 0.0152(3) -0.0090(3) -0.0009(3) Se1 0.0388(7) 0.1345(14) 0.1466(15) 0.0454(11) -0.0138(7) -0.0288(7) Se2 0.0623(8) 0.0711(9) 0.0809(10) 0.0212(7) -0.0274(6) 0.0001(6) S3 0.0357(8) 0.0625(11) 0.0434(9) 0.0020(9) 0.0016(7) -0.0127(8) S4 0.0333(8) 0.0485(9) 0.0477(9) 0.0066(8) -0.0051(7) -0.0056(7) S5 0.0372(9) 0.0556(10) 0.0397(9) 0.0087(8) 0.0013(7) -0.0121(8) S6 0.0362(8) 0.0507(10) 0.0417(9) 0.0133(8) -0.0062(7) -0.0086(8) Se7 0.0689(9) 0.0764(10) 0.0575(8) 0.0297(7) -0.0169(6) -0.0228(7) Se8 0.0358(5) 0.0534(5) 0.0523(5) 0.0135(4) -0.0085(3) -0.0070(4) C1 0.107(9) 0.083(7) 0.156(11) 0.027(8) -0.092(8) -0.010(7) C2 0.044(5) 0.119(10) 0.195(14) -0.043(10) -0.029(7) 0.007(6) C3 0.032(3) 0.055(4) 0.048(4) -0.008(3) -0.003(3) -0.002(3) C4 0.029(3) 0.048(4) 0.050(4) -0.008(3) -0.005(3) 0.001(3) C5 0.035(3) 0.043(3) 0.034(3) -0.002(3) 0.001(3) -0.004(3) C6 0.034(3) 0.039(3) 0.036(3) 0.003(3) 0.004(3) -0.007(3) C7 0.030(3) 0.043(3) 0.037(3) 0.008(3) -0.006(3) 0.002(3) C8 0.036(3) 0.044(3) 0.038(3) 0.004(3) 0.001(3) -0.006(3) C9 0.051(4) 0.079(6) 0.055(4) 0.009(4) -0.013(4) 0.001(4) C10 0.041(4) 0.063(4) 0.052(4) 0.016(4) 0.000(3) 0.001(3) N12 0.052(4) 0.044(4) 0.061(5) 0.009(3) -0.002(3) 0.000(3) C12 0.052(4) 0.044(4) 0.061(5) 0.009(3) -0.002(3) 0.000(3) C11 0.053(4) 0.042(4) 0.042(4) -0.002(3) -0.003(3) 0.002(3) N1 0.075(5) 0.047(4) 0.072(5) -0.009(3) -0.006(4) -0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 C11 2.047(7) . ? Ag1 N12 2.079(6) . ? Ag1 N1 2.531(7) . ? Se1 C2 1.831(13) . ? Se1 C3 1.843(6) . ? Se2 C1 1.794(10) . ? Se2 C4 1.805(7) . ? S3 C5 1.737(6) . ? S3 C3 1.743(7) . ? S4 C5 1.741(6) . ? S4 C4 1.743(6) . ? S5 C6 1.736(6) . ? S5 C8 1.750(6) . ? S6 C6 1.730(6) . ? S6 C7 1.748(6) . ? Se7 C8 1.821(6) . ? Se7 C9 1.851(8) . ? Se8 C7 1.872(6) . ? Se8 C10 1.898(7) . ? C1 C2 1.401(15) . ? C3 C4 1.347(9) . ? C5 C6 1.364(8) . ? C7 C8 1.343(8) . ? C9 C10 1.464(10) . ? N12 C12 1.145(11) 3_656 ? N12 N12 1.145(11) 3_656 ? C11 N1 1.136(9) 2_655 ? N1 C11 1.136(9) 2_645 ? 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 C11 Ag1 N12 160.9(3) . . ? C11 Ag1 N1 103.9(2) . . ? N12 Ag1 N1 94.0(2) . . ? C2 Se1 C3 99.7(4) . . ? C1 Se2 C4 101.8(4) . . ? C5 S3 C3 95.5(3) . . ? C5 S4 C4 95.6(3) . . ? C6 S5 C8 95.2(3) . . ? C6 S6 C7 96.2(3) . . ? C8 Se7 C9 99.1(3) . . ? C7 Se8 C10 98.0(3) . . ? C2 C1 Se2 120.4(8) . . ? C1 C2 Se1 118.2(8) . . ? C4 C3 S3 117.1(5) . . ? C4 C3 Se1 126.8(5) . . ? S3 C3 Se1 116.0(4) . . ? C3 C4 S4 116.7(5) . . ? C3 C4 Se2 128.8(5) . . ? S4 C4 Se2 114.5(4) . . ? C6 C5 S3 124.0(5) . . ? C6 C5 S4 121.5(5) . . ? S3 C5 S4 114.6(3) . . ? C5 C6 S6 121.4(5) . . ? C5 C6 S5 123.7(5) . . ? S6 C6 S5 114.9(3) . . ? C8 C7 S6 116.0(5) . . ? C8 C7 Se8 130.3(5) . . ? S6 C7 Se8 113.7(3) . . ? C7 C8 S5 117.6(5) . . ? C7 C8 Se7 128.5(5) . . ? S5 C8 Se7 113.9(3) . . ? C10 C9 Se7 117.7(6) . . ? C9 C10 Se8 115.3(5) . . ? C12 N12 N12 0.0(9) 3_656 3_656 ? C12 N12 Ag1 175.6(9) 3_656 . ? N12 N12 Ag1 175.6(9) 3_656 . ? N1 C11 Ag1 176.1(6) 2_655 . ? C11 N1 Ag1 150.4(6) 2_645 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Se7 Se8 Se2 Se1 -3.97(5) . . . . ? Se7 C10 C9 Se8 70.8(7) . . . . ? Se2 C1 C2 Se1 63.5(14) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.97 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.874 _refine_diff_density_min -0.792 _refine_diff_density_rms 0.140 #===END data_bets _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H16 Ag N2 S8 Se8' _chemical_formula_weight 1304.40 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' 'Se' 'Se' -0.0929 2.2259 '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' 'N' 'N' 0.0061 0.0033 '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, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 9.5839(8) _cell_length_b 4.983(3) _cell_length_c 34.645(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1654.4(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.695 _cell_measurement_theta_max 13.496 _exptl_crystal_description plates _exptl_crystal_colour black _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1218 _exptl_absorpt_coefficient_mu 9.937 _exptl_absorpt_correction_type 'Semi empirical \y scan' _exptl_absorpt_correction_T_min 0.319109 _exptl_absorpt_correction_T_max 0.999389 _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 'Enraf-Nonius CAD4' _diffrn_measurement_method \q-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 250 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 4179 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1538 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 55 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 34.92 _reflns_number_total 4179 _reflns_number_gt 1136 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf nonius CAD4' _computing_cell_refinement MolEN _computing_data_reduction MolEN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP III' _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^)+(0.0660P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.10(3) _refine_ls_number_reflns 4179 _refine_ls_number_parameters 175 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2658 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1738 _refine_ls_wR_factor_gt 0.1158 _refine_ls_goodness_of_fit_ref 0.926 _refine_ls_restrained_S_all 0.926 _refine_ls_shift/su_max 2.689 _refine_ls_shift/su_mean 0.178 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 0.0000 0.0000 0.7500(2) 0.0598(5) Uani 1 d S . . Se1 Se 0.8712(3) 0.2996(9) 0.07227(10) 0.0331(10) Uani 1 d . . . Se2 Se 0.8701(3) 0.3031(8) -0.02550(10) 0.0327(9) Uani 1 d . . . S1 S 0.8547(6) 0.284(2) 0.1602(2) 0.040(2) Uani 1 d . . . S2 S 0.8540(8) 0.2890(19) -0.1132(2) 0.036(2) Uani 1 d . . . C1 C 0.945(3) 0.426(9) 0.1968(8) 0.14(2) Uani 1 d . . . H1A H 0.8763 0.5314 0.2107 0.050 Uiso 1 calc R . . H1B H 0.9684 0.2776 0.2137 0.050 Uiso 1 calc R . . C2 C 0.9430(18) 0.409(4) 0.1196(7) 0.016(4) Uiso 1 d . . . C3 C 1.0000 0.5000 0.0427(10) 0.030(11) Uani 1 d S . . C4 C 1.0000 0.5000 0.0009(9) 0.036(10) Uani 1 d S . . C5 C 0.937(2) 0.415(6) -0.0739(9) 0.029(6) Uiso 1 d . . . C6 C 0.976(3) 0.354(6) -0.1522(6) 0.045(8) Uani 1 d . . . H6A H 1.0563 0.2373 -0.1495 0.050 Uiso 1 calc R . . H6B H 0.9315 0.3135 -0.1767 0.050 Uiso 1 calc R . . Se3 Se 0.3722(3) 0.7964(10) 0.57233(11) 0.0375(10) Uani 1 d . . . Se4 Se 0.3696(3) 0.7993(8) 0.47457(11) 0.0340(9) Uani 1 d . . . S3 S 0.3591(8) 0.783(3) 0.6598(3) 0.053(3) Uani 1 d . . . S4 S 0.3553(8) 0.785(2) 0.3875(2) 0.039(2) Uani 1 d . . . C7 C 0.485(5) 0.871(8) 0.6981(8) 0.104(15) Uani 1 d . . . H7A H 0.4469 0.8211 0.7230 0.050 Uiso 1 calc R . . H7B H 0.5706 0.7692 0.6943 0.050 Uiso 1 calc R . . C8 C 0.450(3) 0.927(9) 0.6214(8) 0.068(13) Uani 1 d . . . C9 C 0.5000 1.0000 0.5442(11) 0.036(13) Uani 1 d S . . C10 C 0.5000 1.0000 0.5061(10) 0.020(7) Uiso 1 d S . . C11 C 0.453(2) 0.920(6) 0.4264(7) 0.023(5) Uani 1 d . . . C12 C 0.472(2) 0.869(5) 0.3487(6) 0.029(6) Uani 1 d . . . H12A H 0.5492 0.7426 0.3492 0.050 Uiso 1 calc R . . H12B H 0.4229 0.8419 0.3246 0.050 Uiso 1 calc R . . N N -0.2311(13) -0.524(8) 0.7505(17) 0.090(7) Uani 1 d . . . C C -0.1544(13) -0.290(6) 0.7499(6) 0.074(8) 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 0.0620(9) 0.0812(14) 0.0362(7) 0.000 0.000 -0.016(3) Se1 0.0352(16) 0.044(3) 0.0206(19) 0.001(2) 0.0005(14) 0.0012(19) Se2 0.0379(16) 0.038(2) 0.0225(18) 0.003(2) 0.0025(14) -0.0060(18) S1 0.022(3) 0.073(7) 0.024(4) 0.015(5) 0.001(3) -0.005(4) S2 0.042(3) 0.044(6) 0.021(5) -0.011(5) -0.003(4) -0.016(4) C1 0.16(3) 0.23(5) 0.031(15) -0.02(2) 0.022(15) -0.18(4) C3 0.05(2) 0.03(2) 0.005(16) 0.000 0.000 -0.025(15) C4 0.060(17) 0.044(18) 0.005(9) 0.000 0.000 0.028(14) C6 0.058(14) 0.05(2) 0.024(10) 0.000(11) 0.035(10) 0.002(14) Se3 0.0412(17) 0.053(3) 0.0188(19) -0.002(2) -0.0018(14) -0.004(2) Se4 0.0424(17) 0.043(2) 0.017(2) -0.001(2) 0.0032(15) -0.0052(19) S3 0.052(4) 0.087(9) 0.018(4) 0.001(6) 0.001(4) -0.014(5) S4 0.036(3) 0.056(6) 0.024(5) 0.005(5) 0.001(4) -0.008(5) C7 0.19(3) 0.11(3) 0.020(10) 0.019(14) -0.025(18) 0.01(4) C8 0.062(15) 0.12(3) 0.017(8) -0.017(12) -0.010(7) 0.016(16) C9 0.029(16) 0.06(3) 0.02(2) 0.000 0.000 0.034(16) C11 0.019(6) 0.044(12) 0.008(6) -0.007(6) -0.002(5) 0.002(7) C12 0.036(10) 0.021(13) 0.031(11) -0.011(10) -0.024(8) -0.001(10) N 0.049(7) 0.131(19) 0.090(11) 0.005(18) 0.00(2) -0.049(16) C 0.034(7) 0.16(2) 0.032(7) -0.002(16) 0.012(8) 0.015(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 C 2.07(2) . ? Ag1 C 2.07(2) 2 ? Se1 C2 1.86(2) . ? Se1 C3 1.89(2) . ? Se2 C4 1.830(16) . ? Se2 C5 1.88(3) . ? S1 C1 1.69(3) . ? S1 C2 1.75(2) . ? S2 C5 1.70(3) . ? S2 C6 1.82(2) . ? C1 C1 1.28(4) 2_765 ? C2 C2 1.42(4) 2_765 ? C3 C4 1.45(5) . ? C3 Se1 1.89(2) 2_765 ? C4 Se2 1.830(16) 2_765 ? C5 C5 1.48(5) 2_765 ? C6 C6 1.53(6) 2_765 ? Se3 C9 1.86(2) . ? Se3 C8 1.97(3) . ? Se4 C10 1.94(2) . ? Se4 C11 1.94(2) . ? S3 C8 1.75(3) . ? S3 C7 1.85(4) . ? S4 C11 1.77(2) . ? S4 C12 1.80(2) . ? S4 Se3 2.619(9) ? ? C7 C7 1.32(8) 2_675 ? C8 C8 1.20(7) 2_675 ? C9 C10 1.32(5) . ? C9 Se3 1.86(2) 2_675 ? C10 Se4 1.94(2) 2_675 ? C11 C11 1.21(5) 2_675 ? C12 C12 1.41(5) 2_675 ? N C 1.38(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 C Ag1 C 180.0(11) . 2 ? C2 Se1 C3 94.7(11) . . ? C4 Se2 C5 93.2(12) . . ? C1 S1 C2 101.9(11) . . ? C5 S2 C6 103.4(13) . . ? C1 C1 S1 131.3(9) 2_765 . ? C2 C2 S1 126.6(8) 2_765 . ? C2 C2 Se1 118.1(6) 2_765 . ? S1 C2 Se1 115.1(11) . . ? C4 C3 Se1 122.9(9) . 2_765 ? C4 C3 Se1 122.9(9) . . ? Se1 C3 Se1 114.3(18) 2_765 . ? C3 C4 Se2 120.0(9) . . ? C3 C4 Se2 120.0(9) . 2_765 ? Se2 C4 Se2 120.1(17) . 2_765 ? C5 C5 S2 126.5(10) 2_765 . ? C5 C5 Se2 116.6(7) 2_765 . ? S2 C5 Se2 116.6(14) . . ? C6 C6 S2 111.4(18) 2_765 . ? C9 Se3 C8 91.2(15) . . ? C10 Se4 C11 93.5(11) . . ? C8 S3 C7 97.0(15) . . ? C11 S4 C12 98.8(11) . . ? C11 S4 Se3 95.3(8) . ? ? C12 S4 Se3 162.1(8) . ? ? C7 C7 S3 112(3) 2_675 . ? C8 C8 S3 130.4(10) 2_675 . ? C8 C8 Se3 120.2(9) 2_675 . ? S3 C8 Se3 109.3(17) . . ? C10 C9 Se3 121.5(10) . 2_675 ? C10 C9 Se3 121.5(10) . . ? Se3 C9 Se3 117(2) 2_675 . ? C9 C10 Se4 124.3(9) . . ? C9 C10 Se4 124.3(9) . 2_675 ? Se4 C10 Se4 111.3(17) . 2_675 ? C11 C11 S4 130.2(9) 2_675 . ? C11 C11 Se4 120.8(7) 2_675 . ? S4 C11 Se4 108.7(12) . . ? C12 C12 S4 116.8(16) 2_675 . ? N C Ag1 166.5(17) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 34.92 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.207 _refine_diff_density_min -1.373 _refine_diff_density_rms 0.251