Two bis(triorganotin) 2,6-pyridinedicarboxylates, 2,6-C 5 H 3 N(COOSnR 3 ) 2 (R = C 6 H 11 -c, 1; C 6 H 5 C(CH 3 ) 2 CH 2 , 2), have been synthesized by the reaction of 2,6-pyridinedicarboxylic acid with triorganotin hydroxide in toluene-ethanol and characterized by means of elemental analysis, FT-IR, 1 H NMR spectroscopy, and single crystal X-ray diffraction analysis. In the compounds, a 2,6-pyridinedicarboxylate dianion binds two triorganotin units in a monodentate manner and both tin atoms exist in a distorted tetrahedral environment. Bioassay results have shown that the compounds possess good in vitro cytotoxic activity against two human tumor cell lines, Hela and MCF-7.