Eight di-n-butyltin(IV) complexes with glycolic, 2-hydroxy-propionic, succinic and malic acids, have been prepared by two different procedures. The compounds were characterised by elemental analysis, FTIR, Raman and119Sn Mössbauer spectroscopy. The IR and Raman data indicated the presence of bidentate and/or monodentate carboxylate groups, non linear C−Sn−C bonds, and Sn−O bonds within the complexes. The results of Mössbauer spectroscopic measurements, based on point-charge model calculations, have shown the occurrence of trigonal bipyramidal environment in the central tin(IV) atom, besides the octahedral and tetrahedral structure.