The title compound, sodium dioxidomolybdenum(VI) arsenate(V), β-NaMoO2AsO4, was prepared by solid-state reaction at 953 K. In the crystal structure, the AsO4 tetrahedra and MoO6 octahedra (both with m symmetry) share corner atoms to form a three-dimensional framework that delimits cavities parallel to [010] where disordered six-coordinated sodium cations (half-occupation) are located. Structural relationships between the different orthoarsenates of the AMoO2AsO4 series (A = Ag, Li, Na, K and Rb) are discussed.
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