Triorganoantimony(V) complex (C 5 H 5 FeC 5 H 4 C(CH 3 )NO) 2 SbPh 3 (1) has been prepared by the reaction of Ph 3 SbCl 2 with acetylferroceneoxime C 5 H 5 FeC 5 H 4 C(CH 3 )NOH (2) in 1:2 molar ratio in anhydrous toluene. The complexes have been characterized by elemental analyses, IR and NMR ( 1 H and 13 C) spectroscopic studies, and biologic activity was measured. And crystal structures of 1, 2 were reported. The coordination geometry around the antimony atom in 1 was slightly distorted trigonal bipyramidal with the carbon atoms of the SbPh 3 unit in equatorial positions and the two oxygen atoms of the oxime group occupying axial positions. The free oxime was clearly hydrogen bonded (H–N 2.10Å/2.04Å in 2) to essentially form a dimer.