Three new tetrahedral hetero-metal carbonyl clusters were synthesized by refluxing a solution of precursor PhCCo~3(CO)~9 with complexes NaMo(CO)~3(RCp)(R=HCO, CH~3CO, C~2H~5OCO) in THF using metal exchange reaction. Compared with metal exchange reagent NaMo(CO)~3Cp, the results exhibited the electron-withdrawing group C=O on cyclopentadienyl decrease exchange activity of metal exchange reagent NaMo(CO)~3(RCp) and conversion degree to product was accelerated thermally. The results further showed the generality of this kind of metal exchange reaction. The clusters were characterized by C/H analysis, IR and ^1H NMR spectra and X-ray structure determination of cluster PhCCo~2Mo(CO)~8(C~2H~5OCOCp). This cluster is monoclinic space group P2~1/c with α=1.1356(2)nm, b=1.4030(2)m, c=1.6076(3)nm, β=107.19(1)°, Z=4, D~c=1.80g/cm^3, R=0.048 and Rw=0.057.

Key words: STRUCTURAL ANALYSIS, EXCHANGE REACTION, TRANSITION METAL COMPLEX