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The reactions of Co2(CO)8 with 1-ethynylcyclohexanol (HCCC6H10OH, ECY) in benzene led mainly to Co2(CO)6(ECY) 1 and to smaller amounts of the methylidyne complex Co3(CO)9[μ3-CCH2(C6H10OH)] 2. The reactions of Fe3(CO)12 with ECY in the same solvent led to binuclear metallacyclic derivatives Fe2(CO)6(ECY)2 (isomers 3a, 3b) or Fe2(CO)6[(ECY)2 − H2O] 3c as the main products; small yields of trinuclear complexes Fe3(CO)9(μ-CO)[μ3-η2-1,2-HCC(C6H10OH)] 4, Fe3(CO)9(μ-CO)[μ3-η2-1,2-CC(C6H10)] 5 and Fe3(CO)7[μ3-η7-(C6H10OH)CCHCHC(C6H9)] 6 {containing respectively a parallel alkynol, an allenylidene and a dimeric metallacyclic ligand} were also obtained, together with 7, a thermal decomposition product of 6. Finally, when Co2(CO)8 was treated with ECY in benzene, and Fe3(CO)12 was added, the heterometallic complex Co2Fe(CO)6(μ-CO)[μ3-η7-(C6H9)CC(H)C(H)C(H)(C6H10)] 8 was obtained in low yields. The complexes have been characterized by means of IR and 1H NMR spectroscopies and by mass spectrometry. The structures of 2, 5, 8 have been determined by X-ray diffraction. Complex 2 contains an “hydrogenated” ECY ligand, 5 an allenylidene ligand formed upon dehydration of ECY (loss of the OH and of the terminal hydrogen), whereas 8 contains a ligand formed by tail-to-tail coupling of two ECY molecules, with loss of water and oxygen and shift of hydrogen. The elemental analysis of complex 8 gave a Co ∶ Fe ratio of 2 ∶ 1; on the basis of this analysis, the refinement of the diffraction data allowed a hypothesis on the distribution of the metal atoms in the cluster. Reaction pathways for the formation of these clusters are proposed and dehydration mechanisms for the ligand discussed.

journal of the chemical society dalton transactions

Activation of alkynols on transition metal carbonyl clusters. Reactions of 1-ethynylcyclohexanol with Fe3(CO)12 and Co2(CO)8. Crystal structures of Co3(CO)9[μ3-CCH2(C6H10OH)], Fe3(CO)9(μ-CO)[μ3-η2-CC(C6H10)] and Co2Fe(CO)6(μ-CO)[μ3-η7-(C6H9)CC(H)C(H)C(H)(C6H10)]