The title compound, potassium diniobium vanadium phosphorus decasulfide, KNb1.75V0.25PS10, was obtained by reaction of the elements with a eutectic mixture of KCl/LiCl. It is isostructural with the quaternary KNb2PS10, but the Nb sites are occupied by statistically disordered Nb (87.5%) and V (12.5%) atoms. The structure is composed of anionic ∞ 1[M 2PS10]− chains (M = Nb/V) separated from each other by K+ ions. The chain is composed of [MS8] distorted bicapped trigonal prisms and [PS4] tetrahedra. There are no interchain bonding interactions. The crystal used for the X-ray analysis was a racemic twin
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