Abstract
Structure determination of PbSb2Se4 is reported, Mr = 766.5, orthorhombic space group Pnnm, a = 21.206(9)Å, b = 26.660(9)Å, c = 4.068(1) Å, V = 2300(1) Å3, Z = 12, Dx = 6.641 g cm-1, MoKα radiation, λ = 0.7107 Å, μ = 477.8 cm-1, F(000) = 3840, room temperature, R = 0.063, Rw = 0.069 for 1119 independent observed reflections. The crystal was prepared by annealing at 773 K for 2 weeks in vacuum-sealed ampoules. The structure of PbSb2Se4 is isotypic with SnSb2Se4. The cation distribution was determined by X-ray site-occupancy refinement and by bond-valence analysis. The distribution of cations in the tin analogue was also determined by the bond-valence analysis and is similar to that in PbSb2Se4.
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