data_luca _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ag16 As6 Hg0 S12 Te2' _chemical_formula_weight 2815.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 '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' 'Te' 'Te' -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Hg' 'Hg' -2.3894 9.2266 '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' _cell_length_a 7.832(5) _cell_length_b 8.606(4) _cell_length_c 10.755(5) _cell_angle_alpha 95.563(9) _cell_angle_beta 95.880(5) _cell_angle_gamma 116.79(4) _cell_volume 635.3(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 7.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1246 _exptl_absorpt_coefficient_mu 23.011 _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 ? _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 8404 _diffrn_reflns_av_R_equivalents 0.1247 _diffrn_reflns_av_sigmaI/netI 0.7900 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 43.09 _reflns_number_total 5635 _reflns_number_gt 795 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0418P)^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 5635 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1012 _refine_ls_R_factor_gt 0.0826 _refine_ls_wR_factor_ref 0.2104 _refine_ls_wR_factor_gt 0.1733 _refine_ls_goodness_of_fit_ref 0.700 _refine_ls_restrained_S_all 0.700 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_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_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 -0.0372(4) 0.5057(3) 0.3695(3) 0.0453(9) Uani 1 1 d . . . Ag2 Ag 0.5761(4) 0.9562(4) 0.3442(3) 0.0600(10) Uani 1 1 d . . . Ag3 Ag 0.2110(4) 0.6290(3) 0.1574(4) 0.0665(12) Uani 1 1 d . . . Hg4 Hg 0.5000 0.5000 0.5000 0.0240(16) Uiso 0.50 2 d SP . . Ag4 Ag 0.5814(6) 0.5688(5) 0.6241(4) 0.0192(10) Uiso 0.50 1 d P . . Ag5 Ag 0.5248(4) 0.2238(4) 1.1972(4) 0.0787(14) Uani 1 1 d . . . As1 As 0.1403(4) 0.9740(4) 0.3703(3) 0.0205(8) Uani 1 1 d . . . As2 As -0.2694(4) 0.6768(4) 0.1302(3) 0.0237(8) Uani 1 1 d . . . As3 As -0.0383(4) 1.1421(4) 0.1233(3) 0.0190(7) Uani 1 1 d . . . S1 S -0.1650(10) 0.7423(9) 0.3469(8) 0.028(2) Uani 1 1 d . . . S2 S 0.0524(11) 1.1946(9) 0.3412(9) 0.032(2) Uani 1 1 d . . . S3 S -0.1406(9) 0.3513(8) 0.1274(7) 0.0161(16) Uani 1 1 d . . . S4 S -0.3441(11) 0.9075(10) 0.1133(8) 0.030(2) Uani 1 1 d . . . S5 S -0.5701(10) 0.4765(9) 0.1487(9) 0.028(2) Uani 1 1 d . . . S6 S 0.2186(10) 0.9285(10) 0.1780(8) 0.0238(18) Uani 1 1 d . . . Te1 Te 0.3521(3) 0.7157(3) 0.4993(2) 0.0258(8) Uani 0.942(10) 1 d P . . SE1 S 0.3521(3) 0.7157(3) 0.4993(2) 0.0258(8) Uani 0.058(10) 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 0.0385(17) 0.0421(17) 0.061(2) 0.0058(15) 0.0020(15) 0.0253(15) Ag2 0.060(2) 0.066(2) 0.077(3) 0.0210(19) 0.0385(18) 0.0421(19) Ag3 0.0380(18) 0.0290(16) 0.146(4) 0.0166(19) 0.039(2) 0.0221(15) Ag5 0.0334(18) 0.048(2) 0.174(4) 0.040(2) 0.046(2) 0.0255(16) As1 0.0165(16) 0.0228(17) 0.027(2) 0.0048(14) 0.0038(14) 0.0135(14) As2 0.0103(15) 0.0104(15) 0.052(3) 0.0120(15) 0.0102(15) 0.0043(13) As3 0.0137(15) 0.0127(15) 0.033(2) 0.0066(14) 0.0077(14) 0.0069(13) S1 0.018(4) 0.014(4) 0.049(6) 0.007(4) 0.007(4) 0.004(3) S2 0.024(4) 0.014(4) 0.059(7) 0.006(4) 0.012(4) 0.008(4) S3 0.007(3) 0.004(3) 0.033(5) 0.007(3) -0.002(3) -0.001(3) S4 0.022(4) 0.029(5) 0.046(6) 0.002(4) -0.001(4) 0.020(4) S5 0.015(4) 0.016(4) 0.057(6) 0.011(4) 0.008(4) 0.009(3) S6 0.015(4) 0.033(5) 0.026(5) 0.008(4) 0.000(3) 0.013(4) Te1 0.0217(13) 0.0238(13) 0.0366(16) 0.0079(10) 0.0062(10) 0.0137(10) SE1 0.0217(13) 0.0238(13) 0.0366(16) 0.0079(10) 0.0062(10) 0.0137(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 S1 2.664(8) . ? Ag1 S3 2.670(8) . ? Ag1 Ag1 2.827(6) 2_566 ? Ag1 Te1 2.860(4) . ? Ag1 SE1 2.950(4) 2_566 ? Ag1 Te1 2.950(4) 2_566 ? Ag1 Ag3 3.103(5) . ? Ag1 Ag5 3.378(5) 1_454 ? Ag2 S4 2.662(9) 1_655 ? Ag2 Te1 2.853(4) . ? Ag2 SE1 2.928(4) 2_676 ? Ag2 Te1 2.928(4) 2_676 ? Ag2 Ag5 3.061(5) 1_564 ? Ag2 Ag3 3.257(5) . ? Ag3 S6 2.539(8) . ? Ag3 S5 2.589(7) 1_655 ? Ag3 S3 2.671(7) . ? Hg4 Ag4 1.367(4) . ? Hg4 Ag4 1.367(4) 2_666 ? Hg4 Te1 2.594(2) . ? Hg4 SE1 2.594(2) 2_666 ? Hg4 Te1 2.594(2) 2_666 ? Ag4 S5 2.516(10) 2_566 ? Ag4 S2 2.623(9) 2_676 ? Ag4 Ag4 2.735(9) 2_666 ? Ag4 Ag5 2.928(5) 2_667 ? Ag4 Te1 2.916(5) . ? Ag4 SE1 2.947(5) 2_666 ? Ag4 Te1 2.947(5) 2_666 ? Ag5 S6 2.560(8) 1_546 ? Ag5 S3 2.571(7) 1_656 ? Ag5 S5 2.675(8) 1_656 ? Ag5 Ag4 2.928(5) 2_667 ? Ag5 Ag2 3.061(5) 1_546 ? Ag5 Te1 3.230(5) 2_667 ? Ag5 Ag1 3.378(5) 1_656 ? As1 S6 2.265(9) . ? As1 S1 2.289(8) . ? As1 S2 2.329(8) . ? As2 S5 2.249(8) . ? As2 S4 2.327(8) . ? As2 S1 2.314(9) . ? As3 S3 2.275(7) 1_565 ? As3 S4 2.317(9) . ? As3 S2 2.317(10) . ? S2 Ag4 2.623(9) 2_676 ? S3 As3 2.275(7) 1_545 ? S3 Ag5 2.571(7) 1_454 ? S4 Ag2 2.662(9) 1_455 ? S5 Ag4 2.516(10) 2_566 ? S5 Ag3 2.589(7) 1_455 ? S5 Ag5 2.675(8) 1_454 ? S6 Ag5 2.560(8) 1_564 ? Te1 Ag2 2.928(4) 2_676 ? Te1 Ag1 2.950(4) 2_566 ? Te1 Ag4 2.947(5) 2_666 ? Te1 Ag5 3.230(5) 2_667 ? 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 S1 Ag1 S3 97.4(2) . . ? S1 Ag1 Ag1 107.8(2) . 2_566 ? S3 Ag1 Ag1 151.2(2) . 2_566 ? S1 Ag1 Te1 102.95(19) . . ? S3 Ag1 Te1 125.66(18) . . ? Ag1 Ag1 Te1 62.48(11) 2_566 . ? S1 Ag1 SE1 94.3(2) . 2_566 ? S3 Ag1 SE1 105.91(17) . 2_566 ? Ag1 Ag1 SE1 59.31(12) 2_566 2_566 ? Te1 Ag1 SE1 121.79(12) . 2_566 ? S1 Ag1 Te1 94.3(2) . 2_566 ? S3 Ag1 Te1 105.91(17) . 2_566 ? Ag1 Ag1 Te1 59.31(12) 2_566 2_566 ? Te1 Ag1 Te1 121.79(12) . 2_566 ? SE1 Ag1 Te1 0.00(14) 2_566 2_566 ? S1 Ag1 Ag3 91.7(2) . . ? S3 Ag1 Ag3 54.49(17) . . ? Ag1 Ag1 Ag3 135.89(16) 2_566 . ? Te1 Ag1 Ag3 74.91(11) . . ? SE1 Ag1 Ag3 160.16(12) 2_566 . ? Te1 Ag1 Ag3 160.16(12) 2_566 . ? S1 Ag1 Ag5 83.41(18) . 1_454 ? S3 Ag1 Ag5 48.58(16) . 1_454 ? Ag1 Ag1 Ag5 119.74(16) 2_566 1_454 ? Te1 Ag1 Ag5 172.48(12) . 1_454 ? SE1 Ag1 Ag5 60.93(10) 2_566 1_454 ? Te1 Ag1 Ag5 60.93(10) 2_566 1_454 ? Ag3 Ag1 Ag5 101.15(13) . 1_454 ? S4 Ag2 Te1 132.2(2) 1_655 . ? S4 Ag2 SE1 129.1(2) 1_655 2_676 ? Te1 Ag2 SE1 98.10(11) . 2_676 ? S4 Ag2 Te1 129.1(2) 1_655 2_676 ? Te1 Ag2 Te1 98.10(11) . 2_676 ? SE1 Ag2 Te1 0.00(11) 2_676 2_676 ? S4 Ag2 Ag5 72.33(19) 1_655 1_564 ? Te1 Ag2 Ag5 134.82(13) . 1_564 ? SE1 Ag2 Ag5 65.21(11) 2_676 1_564 ? Te1 Ag2 Ag5 65.21(11) 2_676 1_564 ? S4 Ag2 Ag3 67.8(2) 1_655 . ? Te1 Ag2 Ag3 72.59(11) . . ? SE1 Ag2 Ag3 136.95(12) 2_676 . ? Te1 Ag2 Ag3 136.95(12) 2_676 . ? Ag5 Ag2 Ag3 91.33(14) 1_564 . ? S6 Ag3 S5 142.9(3) . 1_655 ? S6 Ag3 S3 115.6(2) . . ? S5 Ag3 S3 101.4(2) 1_655 . ? S6 Ag3 Ag1 94.2(2) . . ? S5 Ag3 Ag1 109.0(2) 1_655 . ? S3 Ag3 Ag1 54.47(18) . . ? S6 Ag3 Ag2 62.35(18) . . ? S5 Ag3 Ag2 86.7(2) 1_655 . ? S3 Ag3 Ag2 149.1(2) . . ? Ag1 Ag3 Ag2 94.61(13) . . ? Ag4 Hg4 Ag4 180.000(1) . 2_666 ? Ag4 Hg4 Te1 89.26(18) . . ? Ag4 Hg4 Te1 90.74(18) 2_666 . ? Ag4 Hg4 SE1 90.74(18) . 2_666 ? Ag4 Hg4 SE1 89.26(18) 2_666 2_666 ? Te1 Hg4 SE1 180.000(1) . 2_666 ? Ag4 Hg4 Te1 90.74(18) . 2_666 ? Ag4 Hg4 Te1 89.26(18) 2_666 2_666 ? Te1 Hg4 Te1 180.000(1) . 2_666 ? SE1 Hg4 Te1 0.00(11) 2_666 2_666 ? Hg4 Ag4 S5 146.6(3) . 2_566 ? Hg4 Ag4 S2 114.4(3) . 2_676 ? S5 Ag4 S2 96.4(3) 2_566 2_676 ? Hg4 Ag4 Ag4 0.00(9) . 2_666 ? S5 Ag4 Ag4 146.6(3) 2_566 2_666 ? S2 Ag4 Ag4 114.4(3) 2_676 2_666 ? Hg4 Ag4 Ag5 127.7(2) . 2_667 ? S5 Ag4 Ag5 58.27(19) 2_566 2_667 ? S2 Ag4 Ag5 94.1(2) 2_676 2_667 ? Ag4 Ag4 Ag5 127.7(2) 2_666 2_667 ? Hg4 Ag4 Te1 62.78(16) . . ? S5 Ag4 Te1 121.1(2) 2_566 . ? S2 Ag4 Te1 108.2(2) 2_676 . ? Ag4 Ag4 Te1 62.78(16) 2_666 . ? Ag5 Ag4 Te1 67.09(13) 2_667 . ? Hg4 Ag4 SE1 61.63(16) . 2_666 ? S5 Ag4 SE1 105.2(2) 2_566 2_666 ? S2 Ag4 SE1 94.3(2) 2_676 2_666 ? Ag4 Ag4 SE1 61.63(16) 2_666 2_666 ? Ag5 Ag4 SE1 162.27(18) 2_667 2_666 ? Te1 Ag4 SE1 124.41(16) . 2_666 ? Hg4 Ag4 Te1 61.63(16) . 2_666 ? S5 Ag4 Te1 105.2(2) 2_566 2_666 ? S2 Ag4 Te1 94.3(2) 2_676 2_666 ? Ag4 Ag4 Te1 61.63(16) 2_666 2_666 ? Ag5 Ag4 Te1 162.27(18) 2_667 2_666 ? Te1 Ag4 Te1 124.41(16) . 2_666 ? SE1 Ag4 Te1 0.00(4) 2_666 2_666 ? S6 Ag5 S3 139.8(3) 1_546 1_656 ? S6 Ag5 S5 110.2(3) 1_546 1_656 ? S3 Ag5 S5 99.0(2) 1_656 1_656 ? S6 Ag5 Ag4 97.7(2) 1_546 2_667 ? S3 Ag5 Ag4 122.2(2) 1_656 2_667 ? S5 Ag5 Ag4 53.1(2) 1_656 2_667 ? S6 Ag5 Ag2 65.33(19) 1_546 1_546 ? S3 Ag5 Ag2 96.34(18) 1_656 1_546 ? S5 Ag5 Ag2 158.3(2) 1_656 1_546 ? Ag4 Ag5 Ag2 105.40(17) 2_667 1_546 ? S6 Ag5 Te1 97.0(2) 1_546 2_667 ? S3 Ag5 Te1 100.8(2) 1_656 2_667 ? S5 Ag5 Te1 106.3(2) 1_656 2_667 ? Ag4 Ag5 Te1 56.28(12) 2_667 2_667 ? Ag2 Ag5 Te1 55.41(10) 1_546 2_667 ? S6 Ag5 Ag1 146.2(2) 1_546 1_656 ? S3 Ag5 Ag1 51.17(18) 1_656 1_656 ? S5 Ag5 Ag1 94.7(2) 1_656 1_656 ? Ag4 Ag5 Ag1 78.93(14) 2_667 1_656 ? Ag2 Ag5 Ag1 83.03(13) 1_546 1_656 ? Te1 Ag5 Ag1 52.96(9) 2_667 1_656 ? S6 As1 S1 100.4(3) . . ? S6 As1 S2 100.1(3) . . ? S1 As1 S2 98.0(3) . . ? S5 As2 S4 95.8(3) . . ? S5 As2 S1 93.1(3) . . ? S4 As2 S1 96.9(3) . . ? S3 As3 S4 95.2(3) 1_565 . ? S3 As3 S2 93.1(3) 1_565 . ? S4 As3 S2 97.3(3) . . ? As1 S1 As2 103.9(3) . . ? As1 S1 Ag1 93.7(3) . . ? As2 S1 Ag1 98.6(3) . . ? As1 S2 As3 101.3(3) . . ? As1 S2 Ag4 90.6(3) . 2_676 ? As3 S2 Ag4 103.3(3) . 2_676 ? As3 S3 Ag5 108.3(3) 1_545 1_454 ? As3 S3 Ag3 96.5(2) 1_545 . ? Ag5 S3 Ag3 145.8(3) 1_454 . ? As3 S3 Ag1 103.6(3) 1_545 . ? Ag5 S3 Ag1 80.2(2) 1_454 . ? Ag3 S3 Ag1 71.05(19) . . ? As3 S4 As2 101.2(3) . . ? As3 S4 Ag2 102.7(3) . 1_455 ? As2 S4 Ag2 100.1(3) . 1_455 ? As2 S5 Ag4 109.5(3) . 2_566 ? As2 S5 Ag3 109.1(3) . 1_455 ? Ag4 S5 Ag3 92.3(3) 2_566 1_455 ? As2 S5 Ag5 95.8(3) . 1_454 ? Ag4 S5 Ag5 68.6(2) 2_566 1_454 ? Ag3 S5 Ag5 152.8(3) 1_455 1_454 ? As1 S6 Ag3 106.3(3) . . ? As1 S6 Ag5 97.7(3) . 1_564 ? Ag3 S6 Ag5 124.9(3) . 1_564 ? Hg4 Te1 Ag2 102.02(10) . . ? Hg4 Te1 Ag1 104.65(10) . . ? Ag2 Te1 Ag1 109.86(13) . . ? Hg4 Te1 Ag2 136.17(11) . 2_676 ? Ag2 Te1 Ag2 81.90(11) . 2_676 ? Ag1 Te1 Ag2 115.04(11) . 2_676 ? Hg4 Te1 Ag4 27.96(9) . . ? Ag2 Te1 Ag4 109.57(13) . . ? Ag1 Te1 Ag4 123.45(13) . . ? Ag2 Te1 Ag4 109.23(14) 2_676 . ? Hg4 Te1 Ag1 92.17(9) . 2_566 ? Ag2 Te1 Ag1 163.82(11) . 2_566 ? Ag1 Te1 Ag1 58.21(12) . 2_566 ? Ag2 Te1 Ag1 93.32(11) 2_676 2_566 ? Ag4 Te1 Ag1 86.61(12) . 2_566 ? Hg4 Te1 Ag4 27.64(9) . 2_666 ? Ag2 Te1 Ag4 92.00(13) . 2_666 ? Ag1 Te1 Ag4 84.25(12) . 2_666 ? Ag2 Te1 Ag4 160.70(13) 2_676 2_666 ? Ag4 Te1 Ag4 55.59(16) . 2_666 ? Ag1 Te1 Ag4 97.18(12) 2_566 2_666 ? Hg4 Te1 Ag5 83.77(8) . 2_667 ? Ag2 Te1 Ag5 122.70(12) . 2_667 ? Ag1 Te1 Ag5 123.78(11) . 2_667 ? Ag2 Te1 Ag5 59.38(10) 2_676 2_667 ? Ag4 Te1 Ag5 56.63(11) . 2_667 ? Ag1 Te1 Ag5 66.11(10) 2_566 2_667 ? Ag4 Te1 Ag5 110.69(12) 2_666 2_667 ? _diffrn_measured_fraction_theta_max 0.596 _diffrn_reflns_theta_full 43.09 _diffrn_measured_fraction_theta_full 0.596 _refine_diff_density_max 3.049 _refine_diff_density_min -4.986 _refine_diff_density_rms 0.575