The cluster
[PPN][Fe3(CO)9CCOC(O)CH3],
2, reacts with [PPN][Re(CO)5] to
generate a
metalated acetylide species,
[PPN][Fe3(CO)9CCRe(CO)5],
3, which was characterized by
infrared and 13C NMR spectroscopy. A byproduct of this
reaction,
[PPN]2[Fe3(CO)9CCO],
appears to result from the attack of
[Re(CO)5]- on the acyl carbon in
compound 2, and a
strategy was devised to suppress this side reaction. The structure
of 3 was determined by
single-crystal X-ray diffraction. The central C−C bond distance
is 1.28(1) Å.