Preparation and structure of tetraphenylphosphonium aquatetrachlorothionitrosylruthenate, [PPh4][Ru(NS)Cl4(H2O)]

Abstract

The preparation and structural characterization of [PPh₄][Ru(NS) Cl₄(H₂O)] are reported. Reaction of S₃N₃Cl₃ with ruthenium trichloride yielded a brown crude product [Ru(NS)Cl₃]. The salt [PPh₄][Ru(NS) Cl₄(H₂O)] was prepared by the addition of PPh₄Cl to an aqueous solution of [Ru(NS)Cl₃] followed by recrystallization of the brown precipitate from water—methanol (1 : 1). The crystals are triclinic, space group P, with unit-cell dimensions a= 10.173(5), b= 11.756(4), c= 12.793(10)Å, α= 66.24(6), β= 78.89(6), γ= 72.58(4)°, and Z= 2 (110 ± 2 K). The [Ru(NS)Cl₄(H₂O)]^– anion forms an octahedron with H₂O trans to the thionitrosyl group. The Ru–N–S group is approximately linear [170.9(3)°] with Ru–N and N–S bond distances of 1.729(4) and 1.504(4)Å, respectively.