Preparation and X-Ray Structure of Cubane-Type Mixed Metal Aqua Ion, [Mo3NiS4(H2O)10]4+

Abstract

We have recently reported that the incomplete cubane-type aqua ion, Mo₃S₄(H₂O)₉]⁴⁺ (A), reacts with metals (Fe,¹ Cu,², and Hg³) to give cubane-type mixed metal aqua ions, the core structures of which have been verified by the X-ray structure analyses of the complexes derived from the aqua ions. In addition, it was found that the reaction of A with metallic magnesium gave a double cubane-type aqua ion.⁴ We now present the preparation, properties, and X-ray structure of a new cubane-type molybdenum-nickel-sulfur mixed metal cluster compound, Mo₃NiS₄(H₂O)₁₀](CH₃°C₆H₄·SO₃)₄·6H₂O (B), prepared from the aqua ion A and metallic nickel. Mo₂Ni₂Cp₂(CO)₂ is the only compound so far reported to have the cubane-type Mo-Ni-S core.⁵