Three bis(triorganotin) benzenedicarboxylates, 1,n-C6H4(COOSnR3)2 (n, R=3, C6H5C(CH3)2CH2, 1; 4, C6H5C(CH3)2CH2, 2; 4, C6H11-c, 3), were synthesized by the reaction of 1,3 or 1,4-benzenedicarboxylic acid with triorganotin chlorides in the solution of CH3ONa-CH3OH and characterized by means of elemental analysis, Fourier-transform infrared spectroscopy (FT-IR), nuclear magnetic resonance (NMR) (1H, 13C, and 119Sn) spectra, and X-ray single-crystal diffraction. Compounds 1–3 are all di-nuclear tin complexes in which the carboxylate is monodentate and each tin atom possesses a distorted SnC3O tetrahedral geometry.