The structures and powder X-ray reference diffraction patterns of the “natural superlattice” series Bi1−x Pbx OCuSe (x = 0, 0.02, 0.04, 0.06, 0.08, and 0.10) have been investigated. As the ionic radius of Pb2+ is greater than that of Bi3+, the unit-cell volume of Bi1−x Pbx OCuSe increases progressively from x = 0 to 0.1, namely, from 137.868(5) to 139.172(11) Å3, as expected. The structure of Bi1−x Pbx OCuSe is built from [Bi2(1−x)Pb2x O2]2(1−x)+ layers normal to the c-axis alternating with [Cu2Se2]2(1−x)− fluorite-like layers. Pb substitution in the Bi site of Bi1−x Pbx OCuSe leads to the weakening of the “bonding” between the [Bi2(1−x)Pb2x O2]2(1−x)+ and the [Cu2Se2]2(1−x)− layers. Powder patterns of Bi1−x Pbx OCuSe were submitted to be included in the Powder Diffraction File.
