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The cleavage of carbon dioxide by the tungsten alkylidyne [CF3-ONO]W≡CCtBu(THF)2 (1) {where CF3-ONO = (MeC6H3[C-(CF3)2O])2N3−}, is reported. Splitting of CO2 yields the tungsten oxo ketene complex [CF3-ONO]W(O){(CH3)3CC=C=O} (6). The proposed pathway occurs through initial cycloaddition of W≡C and C=O bonds to generate a heterometallacyclobutene, which then rearranges to yield W≡O and C=C bonds. Complex 6 was characterized by multinuclear NMR, IR, and single crystal X-ray diffraction. [ABSTRACT FROM AUTHOR]