data_litochlebite _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ag2 Bi4 Pb Se8' _chemical_formula_weight 1890.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Se' 'Se' -0.0929 2.2259 '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' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Bi' 'Bi' -4.1077 10.2566 '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)/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 13.203(4) _cell_length_b 4.1862(12) _cell_length_c 15.280(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.164(4) _cell_angle_gamma 90.00 _cell_volume 797.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 27°C _cell_measurement_reflns_used 1126 _cell_measurement_theta_min 0.95 _cell_measurement_theta_max 20.8 _exptl_crystal_description irregular _exptl_crystal_colour mettalic-black _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas no _exptl_crystal_density_diffrn 7.871 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 75.093 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 27 _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 APEX _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 3793 _diffrn_reflns_av_R_equivalents 0.1068 _diffrn_reflns_av_sigmaI/netI 0.0713 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 20.84 _reflns_number_total 938 _reflns_number_gt 745 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+59.8306P] 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 0.00004(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 938 _refine_ls_number_parameters 104 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.0953 _refine_ls_wR_factor_gt 0.0865 _refine_ls_goodness_of_fit_ref 0.837 _refine_ls_restrained_S_all 0.837 _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 Pb Pb 0.23178(12) 0.2500 0.32670(13) 0.0369(5) Uani 1 2 d S . . Bi1 Bi 0.04205(11) 0.2500 0.88507(10) 0.0205(5) Uani 1 2 d S . . Bi2 Bi 0.56705(11) 0.2500 0.29737(10) 0.0201(5) Uani 1 2 d S . . Bi3 Bi 0.70818(11) 0.2500 0.90388(10) 0.0212(5) Uani 1 2 d S . . Bi4 Bi 0.92528(11) 0.2500 0.37861(11) 0.0239(5) Uani 1 2 d S . . Se1 Se 0.1219(3) 0.2500 0.5106(2) 0.0153(9) Uani 1 2 d S . . Se2 Se 0.1333(3) 0.2500 0.1143(2) 0.0174(9) Uani 1 2 d S . . Se3 Se 0.3034(3) 0.2500 0.7300(3) 0.0177(9) Uani 1 2 d S . . Se4 Se 0.4329(3) 0.2500 0.0765(2) 0.0184(9) Uani 1 2 d S . . Se5 Se 0.6186(3) 0.2500 0.7102(2) 0.0194(9) Uani 1 2 d S . . Se6 Se 0.6569(3) 0.2500 0.4835(3) 0.0324(11) Uani 1 2 d S . . Se7 Se 0.8163(3) 0.2500 0.1196(3) 0.0204(9) Uani 1 2 d S . . Se8 Se 0.9523(3) 0.2500 0.6953(2) 0.0155(9) Uani 1 2 d S . . Ag1 Ag 0.3799(4) 0.2500 0.9026(3) 0.061(3) Uani 0.856(19) 2 d SP . . Ag2 Ag 0.3739(12) -0.069(13) 0.9021(13) 0.076(19) Uani 0.144(19) 1 d P . . Ag3 Ag 0.4708(5) 0.2500 0.5256(5) 0.093(4) Uani 0.764(19) 2 d SP . . Ag4 Ag 0.5000 0.0000 0.5000 0.076(10) Uiso 0.236(19) 2 d SP . . 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 Pb 0.0308(9) 0.0238(10) 0.0572(13) 0.000 0.0161(8) 0.000 Bi1 0.0204(8) 0.0215(9) 0.0183(9) 0.000 0.0045(6) 0.000 Bi2 0.0236(8) 0.0204(9) 0.0175(9) 0.000 0.0084(7) 0.000 Bi3 0.0216(8) 0.0209(9) 0.0190(9) 0.000 0.0040(6) 0.000 Bi4 0.0220(8) 0.0218(9) 0.0245(10) 0.000 0.0031(7) 0.000 Se1 0.0099(18) 0.018(2) 0.017(2) 0.000 0.0030(15) 0.000 Se2 0.0172(19) 0.014(2) 0.021(2) 0.000 0.0064(16) 0.000 Se3 0.0193(19) 0.018(2) 0.017(2) 0.000 0.0073(16) 0.000 Se4 0.0181(19) 0.018(2) 0.019(2) 0.000 0.0049(16) 0.000 Se5 0.022(2) 0.018(2) 0.019(2) 0.000 0.0073(17) 0.000 Se6 0.027(2) 0.057(3) 0.015(2) 0.000 0.0094(18) 0.000 Se7 0.0189(19) 0.018(2) 0.023(2) 0.000 0.0040(17) 0.000 Se8 0.0171(18) 0.0147(19) 0.014(2) 0.000 0.0045(16) 0.000 Ag1 0.058(4) 0.109(10) 0.014(3) 0.000 0.008(2) 0.000 Ag2 0.004(10) 0.16(5) 0.057(14) -0.001(13) 0.004(8) 0.004(9) Ag3 0.066(4) 0.125(8) 0.078(5) 0.000 0.012(3) 0.000 _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 Pb Se5 3.056(3) 3_666 ? Pb Se5 3.056(3) 3_656 ? Pb Se2 3.075(4) . ? Pb Se8 3.141(3) 3_656 ? Pb Se8 3.141(3) 3_666 ? Bi1 Se8 2.748(4) 1_455 ? Bi1 Se7 2.824(3) 3_666 ? Bi1 Se7 2.824(3) 3_656 ? Bi1 Se2 3.124(3) 3_556 ? Bi1 Se2 3.124(3) 3_566 ? Bi2 Se6 2.699(4) . ? Bi2 Se3 2.820(3) 3_666 ? Bi2 Se3 2.820(3) 3_656 ? Bi2 Se5 3.196(3) 3_656 ? Bi2 Se5 3.196(3) 3_666 ? Bi2 Se4 3.256(4) . ? Bi2 Ag2 3.47(2) 3_656 ? Bi2 Ag2 3.47(2) 2_656 ? Bi3 Se5 2.803(4) . ? Bi3 Se4 2.882(3) 3_656 ? Bi3 Se4 2.882(3) 3_666 ? Bi3 Se2 3.036(3) 3_666 ? Bi3 Se2 3.036(3) 3_656 ? Bi3 Se7 3.133(4) 1_556 ? Bi4 Se1 2.715(4) 1_655 ? Bi4 Se1 2.886(3) 3_666 ? Bi4 Se1 2.886(3) 3_656 ? Bi4 Se8 3.077(3) 3_766 ? Bi4 Se8 3.077(3) 3_756 ? Se1 Bi4 2.715(4) 1_455 ? Se1 Bi4 2.886(3) 3_666 ? Se1 Bi4 2.886(3) 3_656 ? Se2 Bi3 3.036(3) 3_666 ? Se2 Bi3 3.036(3) 3_656 ? Se2 Bi1 3.124(3) 3_556 ? Se2 Bi1 3.124(3) 3_566 ? Se3 Ag1 2.496(6) . ? Se3 Bi2 2.820(3) 3_666 ? Se3 Bi2 2.820(3) 3_656 ? Se3 Ag2 2.82(3) 4_565 ? Se3 Ag2 2.82(3) . ? Se4 Ag1 2.515(6) 1_554 ? Se4 Ag2 2.577(19) 2_656 ? Se4 Ag2 2.577(19) 3_656 ? Se4 Bi3 2.882(3) 3_656 ? Se4 Bi3 2.882(3) 3_666 ? Se4 Ag2 2.85(3) 1_554 ? Se4 Ag2 2.85(3) 4_564 ? Se5 Ag3 2.855(7) . ? Se5 Pb 3.056(3) 3_666 ? Se5 Pb 3.056(3) 3_656 ? Se5 Bi2 3.196(3) 3_656 ? Se5 Bi2 3.196(3) 3_666 ? Se6 Ag4 2.406(3) . ? Se6 Ag4 2.406(3) 2_656 ? Se6 Ag3 2.662(5) 3_656 ? Se6 Ag3 2.662(5) 3_666 ? Se6 Ag3 2.736(8) . ? Se7 Ag2 2.54(2) 3_656 ? Se7 Ag2 2.54(2) 2_656 ? Se7 Bi1 2.824(3) 3_666 ? Se7 Bi1 2.824(3) 3_656 ? Se7 Bi3 3.133(4) 1_554 ? Se8 Bi1 2.748(4) 1_655 ? Se8 Bi4 3.077(3) 3_766 ? Se8 Bi4 3.077(3) 3_756 ? Se8 Pb 3.141(3) 3_656 ? Se8 Pb 3.141(3) 3_666 ? Ag1 Ag2 1.34(6) 4_565 ? Ag1 Ag2 1.34(6) . ? Ag1 Se4 2.515(6) 1_556 ? Ag1 Ag2 2.85(6) 1_565 ? Ag1 Ag2 2.85(6) 4 ? Ag2 Ag2 1.51(11) 4 ? Ag2 Se7 2.54(2) 3_656 ? Ag2 Se4 2.577(19) 3_656 ? Ag2 Ag2 2.67(11) 4_565 ? Ag2 Ag1 2.85(6) 1_545 ? Ag2 Se4 2.85(3) 1_556 ? Ag2 Bi2 3.47(2) 3_656 ? Ag3 Ag4 1.223(4) 2_656 ? Ag3 Ag4 1.223(4) . ? Ag3 Ag3 2.447(8) 3_666 ? Ag3 Ag3 2.447(7) 3_656 ? Ag3 Se6 2.662(5) 3_656 ? Ag3 Se6 2.662(5) 3_666 ? Ag3 Ag4 3.2029(17) 1_565 ? Ag3 Ag4 3.2029(17) 2_646 ? Ag4 Ag3 1.223(4) 3_656 ? Ag4 Ag4 2.0931(6) 2_656 ? Ag4 Ag4 2.0931(6) 2_646 ? Ag4 Se6 2.406(3) 3_656 ? Ag4 Ag3 3.2029(17) 3_666 ? Ag4 Ag3 3.2029(17) 1_545 ? 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 Se5 Pb Se5 86.47(10) 3_666 3_656 ? Se5 Pb Se2 83.11(9) 3_666 . ? Se5 Pb Se2 83.11(9) 3_656 . ? Se5 Pb Se8 164.01(11) 3_666 3_656 ? Se5 Pb Se8 92.77(6) 3_656 3_656 ? Se2 Pb Se8 80.95(8) . 3_656 ? Se5 Pb Se8 92.77(6) 3_666 3_666 ? Se5 Pb Se8 164.01(11) 3_656 3_666 ? Se2 Pb Se8 80.95(8) . 3_666 ? Se8 Pb Se8 83.59(9) 3_656 3_666 ? Se8 Bi1 Se7 91.89(10) 1_455 3_666 ? Se8 Bi1 Se7 91.89(9) 1_455 3_656 ? Se7 Bi1 Se7 95.67(12) 3_666 3_656 ? Se8 Bi1 Se2 86.56(9) 1_455 3_556 ? Se7 Bi1 Se2 174.10(8) 3_666 3_556 ? Se7 Bi1 Se2 90.07(7) 3_656 3_556 ? Se8 Bi1 Se2 86.56(9) 1_455 3_566 ? Se7 Bi1 Se2 90.07(7) 3_666 3_566 ? Se7 Bi1 Se2 174.10(8) 3_656 3_566 ? Se2 Bi1 Se2 84.15(9) 3_556 3_566 ? Se6 Bi2 Se3 94.50(10) . 3_666 ? Se6 Bi2 Se3 94.50(10) . 3_656 ? Se3 Bi2 Se3 95.86(11) 3_666 3_656 ? Se6 Bi2 Se5 96.01(10) . 3_656 ? Se3 Bi2 Se5 167.42(10) 3_666 3_656 ? Se3 Bi2 Se5 90.21(7) 3_656 3_656 ? Se6 Bi2 Se5 96.01(10) . 3_666 ? Se3 Bi2 Se5 90.21(7) 3_666 3_666 ? Se3 Bi2 Se5 167.42(10) 3_656 3_666 ? Se5 Bi2 Se5 81.84(9) 3_656 3_666 ? Se6 Bi2 Se4 173.60(11) . . ? Se3 Bi2 Se4 89.79(9) 3_666 . ? Se3 Bi2 Se4 89.79(9) 3_656 . ? Se5 Bi2 Se4 79.20(8) 3_656 . ? Se5 Bi2 Se4 79.20(8) 3_666 . ? Se6 Bi2 Ag2 141.1(3) . 3_656 ? Se3 Bi2 Ag2 73.1(8) 3_666 3_656 ? Se3 Bi2 Ag2 52.1(7) 3_656 3_656 ? Se5 Bi2 Ag2 102.5(7) 3_656 3_656 ? Se5 Bi2 Ag2 120.1(6) 3_666 3_656 ? Se4 Bi2 Ag2 44.9(3) . 3_656 ? Se6 Bi2 Ag2 141.1(3) . 2_656 ? Se3 Bi2 Ag2 52.1(7) 3_666 2_656 ? Se3 Bi2 Ag2 73.1(8) 3_656 2_656 ? Se5 Bi2 Ag2 120.1(6) 3_656 2_656 ? Se5 Bi2 Ag2 102.5(7) 3_666 2_656 ? Se4 Bi2 Ag2 44.9(3) . 2_656 ? Ag2 Bi2 Ag2 25.2(18) 3_656 2_656 ? Se5 Bi3 Se4 92.67(9) . 3_656 ? Se5 Bi3 Se4 92.67(9) . 3_666 ? Se4 Bi3 Se4 93.15(11) 3_656 3_666 ? Se5 Bi3 Se2 88.19(9) . 3_666 ? Se4 Bi3 Se2 176.85(7) 3_656 3_666 ? Se4 Bi3 Se2 89.84(7) 3_666 3_666 ? Se5 Bi3 Se2 88.19(9) . 3_656 ? Se4 Bi3 Se2 89.84(7) 3_656 3_656 ? Se4 Bi3 Se2 176.85(8) 3_666 3_656 ? Se2 Bi3 Se2 87.16(9) 3_666 3_656 ? Se5 Bi3 Se7 178.02(11) . 1_556 ? Se4 Bi3 Se7 88.69(9) 3_656 1_556 ? Se4 Bi3 Se7 88.69(9) 3_666 1_556 ? Se2 Bi3 Se7 90.38(9) 3_666 1_556 ? Se2 Bi3 Se7 90.38(9) 3_656 1_556 ? Se1 Bi4 Se1 84.39(9) 1_655 3_666 ? Se1 Bi4 Se1 84.39(9) 1_655 3_656 ? Se1 Bi4 Se1 92.99(11) 3_666 3_656 ? Se1 Bi4 Se8 77.49(9) 1_655 3_766 ? Se1 Bi4 Se8 87.85(7) 3_666 3_766 ? Se1 Bi4 Se8 161.69(10) 3_656 3_766 ? Se1 Bi4 Se8 77.49(9) 1_655 3_756 ? Se1 Bi4 Se8 161.69(10) 3_666 3_756 ? Se1 Bi4 Se8 87.85(7) 3_656 3_756 ? Se8 Bi4 Se8 85.72(9) 3_766 3_756 ? Bi4 Se1 Bi4 95.61(9) 1_455 3_666 ? Bi4 Se1 Bi4 95.61(9) 1_455 3_656 ? Bi4 Se1 Bi4 92.99(11) 3_666 3_656 ? Bi3 Se2 Bi3 87.16(9) 3_666 3_656 ? Bi3 Se2 Pb 91.79(8) 3_666 . ? Bi3 Se2 Pb 91.79(8) 3_656 . ? Bi3 Se2 Bi1 174.93(13) 3_666 3_556 ? Bi3 Se2 Bi1 94.14(3) 3_656 3_556 ? Pb Se2 Bi1 93.07(9) . 3_556 ? Bi3 Se2 Bi1 94.14(3) 3_666 3_566 ? Bi3 Se2 Bi1 174.93(13) 3_656 3_566 ? Pb Se2 Bi1 93.07(9) . 3_566 ? Bi1 Se2 Bi1 84.15(9) 3_556 3_566 ? Ag1 Se3 Bi2 95.85(12) . 3_666 ? Ag1 Se3 Bi2 95.85(12) . 3_656 ? Bi2 Se3 Bi2 95.86(11) 3_666 3_656 ? Ag1 Se3 Ag2 28.3(10) . 4_565 ? Bi2 Se3 Ag2 75.9(8) 3_666 4_565 ? Bi2 Se3 Ag2 117.3(8) 3_656 4_565 ? Ag1 Se3 Ag2 28.3(10) . . ? Bi2 Se3 Ag2 117.3(8) 3_666 . ? Bi2 Se3 Ag2 75.9(7) 3_656 . ? Ag2 Se3 Ag2 57(2) 4_565 . ? Ag1 Se4 Ag2 93.1(5) 1_554 2_656 ? Ag1 Se4 Ag2 93.1(5) 1_554 3_656 ? Ag2 Se4 Ag2 34(2) 2_656 3_656 ? Ag1 Se4 Bi3 98.33(12) 1_554 3_656 ? Ag2 Se4 Bi3 147.9(12) 2_656 3_656 ? Ag2 Se4 Bi3 114.8(12) 3_656 3_656 ? Ag1 Se4 Bi3 98.33(12) 1_554 3_666 ? Ag2 Se4 Bi3 114.8(12) 2_656 3_666 ? Ag2 Se4 Bi3 147.9(12) 3_656 3_666 ? Bi3 Se4 Bi3 93.15(11) 3_656 3_666 ? Ag1 Se4 Ag2 28.0(10) 1_554 1_554 ? Ag2 Se4 Ag2 102.2(5) 2_656 1_554 ? Ag2 Se4 Ag2 86.3(6) 3_656 1_554 ? Bi3 Se4 Ag2 76.7(8) 3_656 1_554 ? Bi3 Se4 Ag2 116.7(7) 3_666 1_554 ? Ag1 Se4 Ag2 28.0(10) 1_554 4_564 ? Ag2 Se4 Ag2 86.3(6) 2_656 4_564 ? Ag2 Se4 Ag2 102.2(5) 3_656 4_564 ? Bi3 Se4 Ag2 116.7(7) 3_656 4_564 ? Bi3 Se4 Ag2 76.7(8) 3_666 4_564 ? Ag2 Se4 Ag2 56(2) 1_554 4_564 ? Ag1 Se4 Bi2 164.29(18) 1_554 . ? Ag2 Se4 Bi2 71.9(4) 2_656 . ? Ag2 Se4 Bi2 71.9(4) 3_656 . ? Bi3 Se4 Bi2 92.43(9) 3_656 . ? Bi3 Se4 Bi2 92.43(9) 3_666 . ? Ag2 Se4 Bi2 149.0(9) 1_554 . ? Ag2 Se4 Bi2 149.0(9) 4_564 . ? Bi3 Se5 Ag3 163.3(2) . . ? Bi3 Se5 Pb 96.92(9) . 3_666 ? Ag3 Se5 Pb 95.23(13) . 3_666 ? Bi3 Se5 Pb 96.92(9) . 3_656 ? Ag3 Se5 Pb 95.23(13) . 3_656 ? Pb Se5 Pb 86.47(10) 3_666 3_656 ? Bi3 Se5 Bi2 95.24(9) . 3_656 ? Ag3 Se5 Bi2 72.36(13) . 3_656 ? Pb Se5 Bi2 167.59(14) 3_666 3_656 ? Pb Se5 Bi2 94.55(4) 3_656 3_656 ? Bi3 Se5 Bi2 95.24(9) . 3_666 ? Ag3 Se5 Bi2 72.36(13) . 3_666 ? Pb Se5 Bi2 94.55(4) 3_666 3_666 ? Pb Se5 Bi2 167.59(14) 3_656 3_666 ? Bi2 Se5 Bi2 81.84(9) 3_656 3_666 ? Ag4 Se6 Ag4 51.57(8) . 2_656 ? Ag4 Se6 Ag3 27.34(13) . 3_656 ? Ag4 Se6 Ag3 78.22(16) 2_656 3_656 ? Ag4 Se6 Ag3 78.22(16) . 3_666 ? Ag4 Se6 Ag3 27.34(13) 2_656 3_666 ? Ag3 Se6 Ag3 103.7(3) 3_656 3_666 ? Ag4 Se6 Bi2 90.84(12) . . ? Ag4 Se6 Bi2 90.84(12) 2_656 . ? Ag3 Se6 Bi2 83.87(17) 3_656 . ? Ag3 Se6 Bi2 83.87(17) 3_666 . ? Ag4 Se6 Ag3 26.54(5) . . ? Ag4 Se6 Ag3 26.54(5) 2_656 . ? Ag3 Se6 Ag3 53.88(15) 3_656 . ? Ag3 Se6 Ag3 53.88(15) 3_666 . ? Bi2 Se6 Ag3 97.46(19) . . ? Ag2 Se7 Ag2 35(2) 3_656 2_656 ? Ag2 Se7 Bi1 148.5(12) 3_656 3_666 ? Ag2 Se7 Bi1 114.3(12) 2_656 3_666 ? Ag2 Se7 Bi1 114.3(12) 3_656 3_656 ? Ag2 Se7 Bi1 148.5(12) 2_656 3_656 ? Bi1 Se7 Bi1 95.67(12) 3_666 3_656 ? Ag2 Se7 Bi3 76.9(4) 3_656 1_554 ? Ag2 Se7 Bi3 76.9(4) 2_656 1_554 ? Bi1 Se7 Bi3 92.87(10) 3_666 1_554 ? Bi1 Se7 Bi3 92.87(10) 3_656 1_554 ? Bi1 Se8 Bi4 106.91(9) 1_655 3_766 ? Bi1 Se8 Bi4 106.91(9) 1_655 3_756 ? Bi4 Se8 Bi4 85.72(9) 3_766 3_756 ? Bi1 Se8 Pb 99.42(9) 1_655 3_656 ? Bi4 Se8 Pb 153.53(13) 3_766 3_656 ? Bi4 Se8 Pb 89.34(5) 3_756 3_656 ? Bi1 Se8 Pb 99.42(9) 1_655 3_666 ? Bi4 Se8 Pb 89.34(5) 3_766 3_666 ? Bi4 Se8 Pb 153.53(13) 3_756 3_666 ? Pb Se8 Pb 83.59(9) 3_656 3_666 ? Ag2 Ag1 Ag2 173.3(14) 4_565 . ? Ag2 Ag1 Se3 89.5(9) 4_565 . ? Ag2 Ag1 Se3 89.5(9) . . ? Ag2 Ag1 Se4 90.1(9) 4_565 1_556 ? Ag2 Ag1 Se4 90.1(9) . 1_556 ? Se3 Ag1 Se4 172.7(2) . 1_556 ? Ag2 Ag1 Ag2 1.8(4) 4_565 1_565 ? Ag2 Ag1 Ag2 175.1(10) . 1_565 ? Se3 Ag1 Ag2 89.8(4) . 1_565 ? Se4 Ag1 Ag2 90.0(4) 1_556 1_565 ? Ag2 Ag1 Ag2 175.1(10) 4_565 4 ? Ag2 Ag1 Ag2 1.8(4) . 4 ? Se3 Ag1 Ag2 89.8(4) . 4 ? Se4 Ag1 Ag2 90.0(4) 1_556 4 ? Ag2 Ag1 Ag2 176.9(7) 1_565 4 ? Ag1 Ag2 Ag2 176.7(7) . 4 ? Ag1 Ag2 Se7 110.7(14) . 3_656 ? Ag2 Ag2 Se7 72.6(12) 4 3_656 ? Ag1 Ag2 Se4 103.8(14) . 3_656 ? Ag2 Ag2 Se4 72.9(12) 4 3_656 ? Se7 Ag2 Se4 146(2) 3_656 3_656 ? Ag1 Ag2 Ag2 3.3(7) . 4_565 ? Ag2 Ag2 Ag2 180.00(7) 4 4_565 ? Se7 Ag2 Ag2 107.4(12) 3_656 4_565 ? Se4 Ag2 Ag2 107.1(13) 3_656 4_565 ? Ag1 Ag2 Ag1 175.1(10) . 1_545 ? Ag2 Ag2 Ag1 1.6(3) 4 1_545 ? Se7 Ag2 Ag1 74.2(13) 3_656 1_545 ? Se4 Ag2 Ag1 71.4(12) 3_656 1_545 ? Ag2 Ag2 Ag1 178.4(3) 4_565 1_545 ? Ag1 Ag2 Se3 62.2(12) . . ? Ag2 Ag2 Se3 118.3(10) 4 . ? Se7 Ag2 Se3 90.6(5) 3_656 . ? Se4 Ag2 Se3 105.5(7) 3_656 . ? Ag2 Ag2 Se3 61.7(10) 4_565 . ? Ag1 Ag2 Se3 118.5(12) 1_545 . ? Ag1 Ag2 Se4 61.9(12) . 1_556 ? Ag2 Ag2 Se4 117.9(10) 4 1_556 ? Se7 Ag2 Se4 102.5(6) 3_656 1_556 ? Se4 Ag2 Se4 93.7(6) 3_656 1_556 ? Ag2 Ag2 Se4 62.1(10) 4_565 1_556 ? Ag1 Ag2 Se4 117.8(12) 1_545 1_556 ? Se3 Ag2 Se4 124(2) . 1_556 ? Ag1 Ag2 Bi2 101.1(13) . 3_656 ? Ag2 Ag2 Bi2 77.4(9) 4 3_656 ? Se7 Ag2 Bi2 108.5(10) 3_656 3_656 ? Se4 Ag2 Bi2 63.2(5) 3_656 3_656 ? Ag2 Ag2 Bi2 102.6(9) 4_565 3_656 ? Ag1 Ag2 Bi2 76.7(9) 1_545 3_656 ? Se3 Ag2 Bi2 52.0(3) . 3_656 ? Se4 Ag2 Bi2 148.5(11) 1_556 3_656 ? Ag4 Ag3 Ag4 117.6(6) 2_656 . ? Ag4 Ag3 Ag3 0.0(3) 2_656 3_666 ? Ag4 Ag3 Ag3 117.6(6) . 3_666 ? Ag4 Ag3 Ag3 117.6(6) 2_656 3_656 ? Ag4 Ag3 Ag3 0.0(4) . 3_656 ? Ag3 Ag3 Ag3 117.6(6) 3_666 3_656 ? Ag4 Ag3 Se6 156.5(4) 2_656 3_656 ? Ag4 Ag3 Se6 64.61(17) . 3_656 ? Ag3 Ag3 Se6 156.5(4) 3_666 3_656 ? Ag3 Ag3 Se6 64.61(17) 3_656 3_656 ? Ag4 Ag3 Se6 64.61(17) 2_656 3_666 ? Ag4 Ag3 Se6 156.5(4) . 3_666 ? Ag3 Ag3 Se6 64.61(17) 3_666 3_666 ? Ag3 Ag3 Se6 156.5(4) 3_656 3_666 ? Se6 Ag3 Se6 103.7(3) 3_656 3_666 ? Ag4 Ag3 Se6 61.5(3) 2_656 . ? Ag4 Ag3 Se6 61.5(3) . . ? Ag3 Ag3 Se6 61.5(3) 3_666 . ? Ag3 Ag3 Se6 61.5(3) 3_656 . ? Se6 Ag3 Se6 126.12(15) 3_656 . ? Se6 Ag3 Se6 126.12(15) 3_666 . ? Ag4 Ag3 Se5 97.5(3) 2_656 . ? Ag4 Ag3 Se5 97.5(3) . . ? Ag3 Ag3 Se5 97.5(3) 3_666 . ? Ag3 Ag3 Se5 97.5(3) 3_656 . ? Se6 Ag3 Se5 105.5(2) 3_656 . ? Se6 Ag3 Se5 105.5(2) 3_666 . ? Se6 Ag3 Se5 81.8(2) . . ? Ag4 Ag3 Ag4 19.78(16) 2_656 1_565 ? Ag4 Ag3 Ag4 137.4(4) . 1_565 ? Ag3 Ag3 Ag4 19.78(16) 3_666 1_565 ? Ag3 Ag3 Ag4 137.4(4) 3_656 1_565 ? Se6 Ag3 Ag4 149.8(2) 3_656 1_565 ? Se6 Ag3 Ag4 47.34(7) 3_666 1_565 ? Se6 Ag3 Ag4 79.50(12) . 1_565 ? Se5 Ag3 Ag4 92.86(11) . 1_565 ? Ag4 Ag3 Ag4 137.4(4) 2_656 2_646 ? Ag4 Ag3 Ag4 19.78(16) . 2_646 ? Ag3 Ag3 Ag4 137.4(4) 3_666 2_646 ? Ag3 Ag3 Ag4 19.78(16) 3_656 2_646 ? Se6 Ag3 Ag4 47.34(7) 3_656 2_646 ? Se6 Ag3 Ag4 149.8(2) 3_666 2_646 ? Se6 Ag3 Ag4 79.50(12) . 2_646 ? Se5 Ag3 Ag4 92.86(11) . 2_646 ? Ag4 Ag3 Ag4 157.2(3) 1_565 2_646 ? Ag3 Ag4 Ag3 180.000(1) . 3_656 ? Ag3 Ag4 Ag4 31.2(3) . 2_656 ? Ag3 Ag4 Ag4 148.8(3) 3_656 2_656 ? Ag3 Ag4 Ag4 148.8(3) . 2_646 ? Ag3 Ag4 Ag4 31.2(3) 3_656 2_646 ? Ag4 Ag4 Ag4 180.0 2_656 2_646 ? Ag3 Ag4 Se6 88.0(3) . 3_656 ? Ag3 Ag4 Se6 92.0(3) 3_656 3_656 ? Ag4 Ag4 Se6 115.78(4) 2_656 3_656 ? Ag4 Ag4 Se6 64.22(4) 2_646 3_656 ? Ag3 Ag4 Se6 92.0(3) . . ? Ag3 Ag4 Se6 88.0(3) 3_656 . ? Ag4 Ag4 Se6 64.22(4) 2_656 . ? Ag4 Ag4 Se6 115.78(4) 2_646 . ? Se6 Ag4 Se6 180.0 3_656 . ? Ag3 Ag4 Ag3 42.6(4) . 3_666 ? Ag3 Ag4 Ag3 137.4(4) 3_656 3_666 ? Ag4 Ag4 Ag3 11.41(13) 2_656 3_666 ? Ag4 Ag4 Ag3 168.59(13) 2_646 3_666 ? Se6 Ag4 Ag3 125.56(12) 3_656 3_666 ? Se6 Ag4 Ag3 54.44(12) . 3_666 ? Ag3 Ag4 Ag3 137.4(4) . 1_545 ? Ag3 Ag4 Ag3 42.6(4) 3_656 1_545 ? Ag4 Ag4 Ag3 168.59(13) 2_656 1_545 ? Ag4 Ag4 Ag3 11.41(13) 2_646 1_545 ? Se6 Ag4 Ag3 54.44(12) 3_656 1_545 ? Se6 Ag4 Ag3 125.56(12) . 1_545 ? Ag3 Ag4 Ag3 180.0 3_666 1_545 ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 20.84 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 4.649 _refine_diff_density_min -1.805 _refine_diff_density_rms 0.429