Ten novel diorganotin dicarboxylates containing germanium in the carboxylate ligand have been synthesized and their structures have been characterized by IR, Mossbauer and multinuclear NMR (H-1, C-13, Sn-119) spectroscopies and X-ray diffraction. Also, the twodiastereotopic protons of the methylene group which are directly attached to the chiral center in these compounds have been successfully analyzed for the first time. The resulted ABX system gives three coupling constants and three chemical shifts. The single crystal X-ray analysis of precursor (p-CH3C6H4)(3)GeCH(p-CH3C6H4)CH2COOH revealed the dimeric structure of the molecule through H-bonding between carboxylic acid groups in a conventional manner. The results of their biological activity suggest that the materials have potential to be used as drugs. (C) 2004 Elsevier B.V. All rights reserved.