Résumé : Triorganoantimony(V) salicylates, [5‐Y‐2‐(HO)‐C6H3COO]2SbR3 (R=Me, Ph; Y=H, Me, MeO), were obtained by reacting R3SbCl2 with the appropriate sodium salt. The compounds have been characterized by IR, MS, 1H and 13C NMR spectroscopy. The molecular structure of the three substituted trimethylantimony(V) disalicylates has been determined by X‐ray diffraction. The salicylate ligands are mono‐coordinated to antimony through an oxygen atom of each carboxylate, leading to a trigonal bipyramidal geometry, with the antimony‐methyl groups in equatorial positions and the oxygen atoms in axial positions. The trimethylantimony compounds tested in vitro against a series of human tumour cell lines were found to be inactive. Copyright © 1995 John Wiley & Sons, Ltd.