data_bill_final _audit_creation_method SHELXL-97 _chemical_name_systematic ; billingsleyite ; _chemical_name_common billingsleyite _chemical_melting_point ? _chemical_formula_moiety 'Ag7 As0.75 Cu0 S6 Sb0.25' _chemical_formula_sum 'Ag7 As0.75 Cu0 S6 Sb0.25' _chemical_formula_weight 1034.08 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' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'P 21 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' 'y, z, x' '-y+1/2, -z, x+1/2' 'y+1/2, -z+1/2, -x' '-y, z+1/2, -x+1/2' 'z, x, y' '-z, x+1/2, -y+1/2' '-z+1/2, -x, y+1/2' 'z+1/2, -x+1/2, -y' _cell_length_a 10.4760(8) _cell_length_b 10.4760(8) _cell_length_c 10.4760(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1149.70(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 458 _cell_measurement_theta_min 5.29 _cell_measurement_theta_max 13.62 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.974 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1850 _exptl_absorpt_coefficient_mu 15.424 _exptl_absorpt_correction_type 'gaussian' _exptl_absorpt_correction_T_min 0.237 _exptl_absorpt_correction_T_max 0.462 _exptl_absorpt_process_details 'ABSPACK (Oxford Diffraction, 2006)' _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 'Oxford Xcalibur 3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 10 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9623 _diffrn_reflns_av_R_equivalents 0.0654 _diffrn_reflns_av_sigmaI/netI 0.2920 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.35 _diffrn_reflns_theta_max 28.51 _reflns_number_total 902 _reflns_number_gt 419 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis (Oxford Diffraction, 2006)' _computing_cell_refinement 'Crysalis (Oxford Diffraction, 2006)' _computing_data_reduction 'Crysalis (Oxford Diffraction, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Xtaldraw (Downs & Hall-Wallace, 2003)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0159P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.28(4) _refine_ls_number_reflns 902 _refine_ls_number_parameters 46 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0191 _refine_ls_R_factor_gt 0.0164 _refine_ls_wR_factor_ref 0.0303 _refine_ls_wR_factor_gt 0.0298 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.39542(6) 0.39542(6) 0.39542(6) 0.0198(4) Uani 0.979(12) 3 d SP . . Cu1 Cu 0.39542(6) 0.39542(6) 0.39542(6) 0.0198(4) Uani 0.021(12) 3 d SP . . Ag2 Ag 0.23157(6) 0.02321(5) 0.25897(6) 0.02123(17) Uani 1 1 d . . . Ag3 Ag 0.34660(5) 0.82461(6) 0.98492(6) 0.02174(17) Uani 1 1 d . . . As As 0.99834(7) 0.99834(7) 0.99834(7) 0.0202(6) Uani 0.886(14) 3 d SP . . Sb Sb 0.99834(7) 0.99834(7) 0.99834(7) 0.0202(6) Uani 0.114(14) 3 d SP . . S1 S 0.53042(19) 0.53042(19) 0.53042(19) 0.0213(8) Uani 1 3 d S . . S2 S 0.87632(18) 0.87632(18) 0.87632(18) 0.0213(9) Uani 1 3 d S . . S3 S 0.26377(18) 0.26377(18) 0.26377(18) 0.0219(8) Uani 1 3 d S . . S4 S 0.1226(2) 0.87305(19) 0.1085(2) 0.0241(5) 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 0.0198(4) 0.0198(4) 0.0198(4) -0.0004(3) -0.0004(3) -0.0004(3) Cu1 0.0198(4) 0.0198(4) 0.0198(4) -0.0004(3) -0.0004(3) -0.0004(3) Ag2 0.0208(4) 0.0215(3) 0.0214(4) 0.0003(3) 0.0000(3) -0.0001(3) Ag3 0.0213(4) 0.0220(4) 0.0219(4) -0.0001(3) -0.0002(3) 0.0000(3) As 0.0202(6) 0.0202(6) 0.0202(6) -0.0004(3) -0.0004(3) -0.0004(3) Sb 0.0202(6) 0.0202(6) 0.0202(6) -0.0004(3) -0.0004(3) -0.0004(3) S1 0.0213(8) 0.0213(8) 0.0213(8) 0.0009(10) 0.0009(10) 0.0009(10) S2 0.0213(9) 0.0213(9) 0.0213(9) -0.0002(9) -0.0002(9) -0.0002(9) S3 0.0219(8) 0.0219(8) 0.0219(8) 0.0002(9) 0.0002(9) 0.0002(9) S4 0.0245(12) 0.0249(12) 0.0230(11) 0.0013(10) 0.0012(10) 0.0005(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 S3 2.389(3) . ? Ag1 S1 2.449(4) . ? Ag1 Ag3 3.0701(8) 11_664 ? Ag1 Ag3 3.0701(8) 4_646 ? Ag1 Ag3 3.0701(8) 7_466 ? Ag2 S4 2.503(2) 1_545 ? Ag2 S3 2.543(2) . ? Ag2 S4 2.563(2) 11_554 ? Ag2 Ag3 2.9690(9) 2_564 ? Ag2 Ag3 3.1098(9) 12_456 ? Ag2 Ag2 3.3086(10) 5 ? Ag2 Ag2 3.3086(10) 9 ? Ag3 S1 2.5168(10) 4_656 ? Ag3 S2 2.5770(9) 3_467 ? Ag3 S4 2.728(2) 1_556 ? Ag3 S3 2.7498(6) 2_565 ? Ag3 Ag2 2.9690(9) 2_565 ? Ag3 Ag1 3.0701(8) 4_656 ? Ag3 Cu1 3.0701(8) 4_656 ? Ag3 Ag2 3.1098(9) 6_565 ? As S4 2.179(2) 9_665 ? As S4 2.179(2) 5_566 ? As S4 2.179(2) 1_656 ? As S2 2.214(3) . ? S1 Ag3 2.5168(10) 7_466 ? S1 Ag3 2.5168(10) 4_646 ? S1 Ag3 2.5168(10) 11_664 ? S2 Ag3 2.5770(9) 10_756 ? S2 Ag3 2.5770(9) 3_567 ? S2 Ag3 2.5770(9) 6_675 ? S3 Ag2 2.543(2) 9 ? S3 Ag2 2.543(2) 5 ? S3 Ag3 2.7498(6) 12_456 ? S3 Ag3 2.7498(6) 2_564 ? S3 Ag3 2.7498(6) 8_645 ? S4 Sb 2.179(2) 1_454 ? S4 As 2.179(2) 1_454 ? S4 Ag2 2.503(2) 1_565 ? S4 Ag2 2.563(2) 8 ? S4 Ag3 2.728(2) 1_554 ? 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 S3 Ag1 S1 180.00(6) . . ? S3 Ag1 Ag3 127.19(2) . 11_664 ? S1 Ag1 Ag3 52.81(2) . 11_664 ? S3 Ag1 Ag3 127.19(2) . 4_646 ? S1 Ag1 Ag3 52.81(2) . 4_646 ? Ag3 Ag1 Ag3 87.24(3) 11_664 4_646 ? S3 Ag1 Ag3 127.19(2) . 7_466 ? S1 Ag1 Ag3 52.81(2) . 7_466 ? Ag3 Ag1 Ag3 87.24(3) 11_664 7_466 ? Ag3 Ag1 Ag3 87.24(3) 4_646 7_466 ? S4 Ag2 S3 134.10(8) 1_545 . ? S4 Ag2 S4 102.56(11) 1_545 11_554 ? S3 Ag2 S4 119.64(8) . 11_554 ? S4 Ag2 Ag3 135.54(5) 1_545 2_564 ? S3 Ag2 Ag3 59.25(3) . 2_564 ? S4 Ag2 Ag3 97.38(5) 11_554 2_564 ? S4 Ag2 Ag3 119.19(5) 1_545 12_456 ? S3 Ag2 Ag3 57.16(2) . 12_456 ? S4 Ag2 Ag3 80.49(5) 11_554 12_456 ? Ag3 Ag2 Ag3 102.97(3) 2_564 12_456 ? S4 Ag2 Ag2 96.52(5) 1_545 5 ? S3 Ag2 Ag2 49.42(4) . 5 ? S4 Ag2 Ag2 156.44(5) 11_554 5 ? Ag3 Ag2 Ag2 59.09(2) 2_564 5 ? Ag3 Ag2 Ag2 102.194(18) 12_456 5 ? S4 Ag2 Ag2 89.09(5) 1_545 9 ? S3 Ag2 Ag2 49.42(4) . 9 ? S4 Ag2 Ag2 133.20(5) 11_554 9 ? Ag3 Ag2 Ag2 105.36(2) 2_564 9 ? Ag3 Ag2 Ag2 55.00(2) 12_456 9 ? Ag2 Ag2 Ag2 60.0 5 9 ? S1 Ag3 S2 132.37(8) 4_656 3_467 ? S1 Ag3 S4 108.14(5) 4_656 1_556 ? S2 Ag3 S4 89.32(9) 3_467 1_556 ? S1 Ag3 S3 116.74(9) 4_656 2_565 ? S2 Ag3 S3 104.54(7) 3_467 2_565 ? S4 Ag3 S3 95.78(6) 1_556 2_565 ? S1 Ag3 Ag2 68.30(7) 4_656 2_565 ? S2 Ag3 Ag2 157.17(5) 3_467 2_565 ? S4 Ag3 Ag2 92.36(5) 1_556 2_565 ? S3 Ag3 Ag2 52.64(5) 2_565 2_565 ? S1 Ag3 Ag1 50.84(8) 4_656 4_656 ? S2 Ag3 Ag1 81.99(2) 3_467 4_656 ? S4 Ag3 Ag1 121.24(5) 1_556 4_656 ? S3 Ag3 Ag1 142.70(5) 2_565 4_656 ? Ag2 Ag3 Ag1 116.01(3) 2_565 4_656 ? S1 Ag3 Cu1 50.84(8) 4_656 4_656 ? S2 Ag3 Cu1 81.99(2) 3_467 4_656 ? S4 Ag3 Cu1 121.24(5) 1_556 4_656 ? S3 Ag3 Cu1 142.70(5) 2_565 4_656 ? Ag2 Ag3 Cu1 116.01(3) 2_565 4_656 ? Ag1 Ag3 Cu1 0.00(2) 4_656 4_656 ? S1 Ag3 Ag2 87.84(2) 4_656 6_565 ? S2 Ag3 Ag2 101.45(7) 3_467 6_565 ? S4 Ag3 Ag2 146.59(5) 1_556 6_565 ? S3 Ag3 Ag2 50.99(5) 2_565 6_565 ? Ag2 Ag3 Ag2 65.90(3) 2_565 6_565 ? Ag1 Ag3 Ag2 91.745(19) 4_656 6_565 ? Cu1 Ag3 Ag2 91.745(19) 4_656 6_565 ? S4 As S4 111.25(5) 9_665 5_566 ? S4 As S4 111.25(5) 9_665 1_656 ? S4 As S4 111.25(5) 5_566 1_656 ? S4 As S2 107.63(5) 9_665 . ? S4 As S2 107.63(5) 5_566 . ? S4 As S2 107.63(5) 1_656 . ? Ag1 S1 Ag3 76.36(8) . 7_466 ? Ag1 S1 Ag3 76.36(8) . 4_646 ? Ag3 S1 Ag3 114.62(6) 7_466 4_646 ? Ag1 S1 Ag3 76.36(8) . 11_664 ? Ag3 S1 Ag3 114.62(6) 7_466 11_664 ? Ag3 S1 Ag3 114.62(6) 4_646 11_664 ? As S2 Ag3 102.45(7) . 10_756 ? As S2 Ag3 102.45(7) . 3_567 ? Ag3 S2 Ag3 115.48(5) 10_756 3_567 ? As S2 Ag3 102.45(7) . 6_675 ? Ag3 S2 Ag3 115.48(5) 10_756 6_675 ? Ag3 S2 Ag3 115.48(5) 3_567 6_675 ? Ag1 S3 Ag2 131.31(6) . 9 ? Ag1 S3 Ag2 131.31(6) . 5 ? Ag2 S3 Ag2 81.16(9) 9 5 ? Ag1 S3 Ag2 131.31(6) . . ? Ag2 S3 Ag2 81.16(9) 9 . ? Ag2 S3 Ag2 81.16(9) 5 . ? Ag1 S3 Ag3 87.18(7) . 12_456 ? Ag2 S3 Ag3 68.11(3) 9 12_456 ? Ag2 S3 Ag3 141.43(13) 5 12_456 ? Ag2 S3 Ag3 71.85(3) . 12_456 ? Ag1 S3 Ag3 87.18(7) . 2_564 ? Ag2 S3 Ag3 141.43(13) 9 2_564 ? Ag2 S3 Ag3 71.85(3) 5 2_564 ? Ag2 S3 Ag3 68.11(3) . 2_564 ? Ag3 S3 Ag3 119.760(12) 12_456 2_564 ? Ag1 S3 Ag3 87.18(7) . 8_645 ? Ag2 S3 Ag3 71.85(3) 9 8_645 ? Ag2 S3 Ag3 68.11(3) 5 8_645 ? Ag2 S3 Ag3 141.43(13) . 8_645 ? Ag3 S3 Ag3 119.760(12) 12_456 8_645 ? Ag3 S3 Ag3 119.760(12) 2_564 8_645 ? Sb S4 As 0.00(3) 1_454 1_454 ? Sb S4 Ag2 103.15(8) 1_454 1_565 ? As S4 Ag2 103.15(8) 1_454 1_565 ? Sb S4 Ag2 105.74(8) 1_454 8 ? As S4 Ag2 105.74(8) 1_454 8 ? Ag2 S4 Ag2 98.82(8) 1_565 8 ? Sb S4 Ag3 111.99(8) 1_454 1_554 ? As S4 Ag3 111.99(8) 1_454 1_554 ? Ag2 S4 Ag3 91.34(6) 1_565 1_554 ? Ag2 S4 Ag3 137.41(9) 8 1_554 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.51 _diffrn_measured_fraction_theta_full 0.910 _refine_diff_density_max 0.597 _refine_diff_density_min -0.525 _refine_diff_density_rms 0.130