A new series of diorganotin(IV) derivatives of the general formula (1R3GeCH2RCH2COO)2Sn3R2 has been prepared by the reaction of diorganotin chlorides/oxides with substituted germyl propionic acids in 1:2 mole ratios. These compounds have been characterized by elemental analyses and various spectroscopic techniques (IR, multinuclear NMR (1H, 13C, 119Sn), 119mSn Mössbauer spectroscopies and mass spectrometry). The single crystal structure of the precursor Ph3GeCHRFCH2COOH (RF = 4‐FC6H4) has been determined by X‐ray diffraction. Biological studies such as cytotoxicity, antibacterial, and cytotoxicity were also investigated. © 2008 Wiley Periodicals, Inc. Heteroatom Chem 19:163–170, 2008; Published online in Wiley InterScience (www.interscience.wiley.com). DOI 10.1002/hc.20402