The triphenyllead carboxylates, Ph3PbO2CR (R = C6F5, 4-MeOC6F4, 4-EtOC6F4, 2, 4-(NO2)2C6H3, or C6Cl5) have been obtained by reactions of triphenyllead acetate with the appropriate carboxylic acids. The first four compounds are monomeric with unidentate carboxylate coordination in chloroform, and all are probably polymeric with bridging carboxylate groups in the solid state. The compounds, Ph3PbO2CR (R = C6F5, 4-RieOC6F4, or 4-EtOC6F4), undergo decarboxylation in boiling pyridine to give the corresponding polyfluoroaryltriphenyllead derivatives, but the other carboxylates do not decompose in a similar manner. The phenylmercuric carboxylates, PhHgO2CR (R = 4-MeOC6F4 or 4-EtOC6F4), have also been prepared and shown to decarboxylate to the corresponding 4-alkoxytetrafluorophenylphenylmercurials. Cleavage of the compounds, Ph3PbR (R = C5F6 or 4-1MeOC6F4), with pentafluorobenzoic acid yields diphenyllead bispentafluorobenzoate.