The silyl estersCp(PPh3)(NO)ReCO2SiR3(2)are produced from treatment ofCp(PPh3)(NO)ReCOBF4with the silanolates R3SiONa (R3Si= PhMe2Si, Et3Si)in CH2Cl2 (0 C) or ofCp(PPh3)(NO)ReCO2K withR3SiCl in THF. Upon handling, 2 degraded to thebimetallocarboxylatesCp(PPh3)(NO)ReCO2Re(CO)(NO)(PPh3)(OSiR3) (3), one of which(SiR3 = SiMe2Ph) wascharacterized by X-ray crystallography as ar.gif">-rs/eta.gif" BORDER=0 >1(C(Re1)):rs/eta.gif" BORDER=0 >2(O,O'(Re2)) bimetallocarboxylate.