The unsaturated clusters Fe4(CO)11(μ4-PR)2 (R = Ph, Tol) insert terminal alkynes HC2R′ (R′ = Me, Ph) between iron and phosphorus to form clusters Fe4(CO)11(μ4-PR)(μ4-RP−CR′−CH) in which according to a structure determination the RP -CR′−CH ligand has the phosphorus μ2-bridging to two irons, the CR′−CH unit η2-bonding to the third and the CH unit o-bonding to the fourth iron. Under CO these clusters lose one iron unit to form Fe3(CO)9(PR)(RP−CR′−CH).
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