A new method has been developed to synthesise bis η5-cyclopentadienyl dithiolene complexes of molybdenum and tungsten. This procedure involves the in situthermolysis of the azo compounds, 2,2′-azobisisobutyronitrile (AIBN) or 1,1′-azobiscyclohexanecarbonitrile (ACCN) (R′2N2, R′ = CMe2CN or C6H10CN, respectively), which initiates a reaction between [Cp2M(S4)] (M = Mo or W) and an alkyne (HC2R, R = Ph, 2-pyridyl or 2-quinoxalinyl) and produce the corresponding [Cp2M(S2C2RR′)] compound.
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