Reaction of RCCo3(CO)9 (R=CH3, C2H5, C6H5) with Na2[Fe(CO)4] in THF solution leads to the formation of the new mixed-metal alkylidyne clusters RCFeCo2(CO)9H (R=CH3, C2H5, C6H5) in yields of 31-48%. Spectral data suggest that these have structures similar to those of the parent RCCo3(CO)9 cluster, i.e., an FeCo2 triangle triply bridged by the alkylidyne carbon. The possible location of the hydride ligand is discussed on the basis of electron-count, infrared, and 1H and 13C NMR spectra. The reaction of HCCo3(CO)9 with Na2[Fe(CO)4], which gave a complex mixture of products, is also discussed. © 1979, American Chemical Society. All rights reserved.