A series of arylantimony ferrocenecarboxylates with the formula (C 5 H 5 FeC 5 H 4 CO 2 ) n SbAr (5-n) (n = 1, 2; Ar = C 6 H 5 , 4-CH 3 C 6 H 4 , 3-CH 3 C 6 H 4 , 2-CH 3 C 6 H 4 , 4-ClC 6 H 4 , 4-FC 6 H 4 ) were synthesized and characterized by elemental analysis, IR, 1 H NMR and mass spectra. The crystal structures of (C 5 H 5 FeC 5 H 4 CO 2 ) 2 Sb(4-CH 3 C 6 H 4 ) 3 and C 5 H 5 FeC 5 H 4 CO 2 SbPh 4 were determined by X-ray diffraction. Four human neoplastic cell lines (HL-60, Bel-7402, KB and Hela) were used to screen these compounds. The results indicate that these compounds at 10 μM show certain in vitro antitumor activities.