Syntheses of Novel Fe/S Clusters with μ‐Aminocarbyne Ligands

The reaction of Fe 3 (CO) 12 with (C 3 H 5 ) 2 NCS 2 K in THF at room temperature afforded a red‐brown solution. Treatment of the thus‐obtained solution with MeI and PhCH 2 Br afforded clusters 1 , (μ‐MeS)Fe 2 (CO) 6 (μ 4 ‐S)Fe 2 (CO) 6 (μ‐CN(C 3 H 5 ) 2 ), and 2 , (μ‐PhCH 2 CO)Fe 2 (CO) 6 (μ 4 ‐S)Fe 2 (CO) 6 (μ‐CN(C 3 H 5 ) 2 ). Their structures were unambiguously determined by X‐ray crystallography. Therefore, this methodology provides a novel route for the syntheses of spiro‐S Fe/S clusters with aminocarbyne ligands.