Triarylantimony(V) di(N‐phenylglycinates) (PhNHCH2COO)2SbAr3 (Ar = Ph, p‐CH3C6H4, p‐ClC6H4, and p‐FC6H4) have been synthesized and characterized by elemental analysis, IR, 1H NMR, and mass spectra. The crystal structure of (PhNHCH2COO)2Sb(C6H4F‐p)3 has been determined by X‐ray diffraction. The in vitro antitumor activities of these compounds against three cancer cell lines are reported. © 2003 Wiley Periodicals, Inc. Heteroatom Chem 15:32–36, 2004; Published online in Wiley InterScience (www.interscience.wiley.com). DOI 10.1002/hc.10208