Triorganotin and -lead derivatives of X-benzoylglveine (BzGlyH) and N-formylglycine (ForGlyH), R3MBzGly and R3MForGly (M = Sn; R = Me, Ph. M = Pb; R = Ph) have been prepared from R3MOH and BzGlyH or ForGlyH, respectively. According to spectroscopic data the Me3Sn groups are essentially planar; molecules of R3SnForGly are bridged by unidentate carboxylate groups and formyl-C = O groups in the solid state, while Ph3PbForGly and benzoylglycinates are bridged by bidentate carboxylate groups. NH does not coordinate to M. Pentacoordination and a polymeric nature in the solid state is also indicated by Mößbauer data of Me3SnForGly and Me3SnBzGly. In solution all compounds are monomeric.