Chloro bis(alkylenedithiophosphato)antimony(III) complexes of the type [OGOP(S)S] 2 SbCl(1-5) [where G = C(Me) 2 CH 2 CH(Me) {1} C(Me) 2 C(Me) 2 {2}, CH 2 C(Me) 2 CH 2 {3}, CH(Me) CH(Me) {4} and -CH(Me) CH 2 CH 2 {5}] have been synthesized by the reaction of SbCl 3 with sodium salts of alkylenedithiophosphoric acids in a 1:2 molar ratio in refluxing benzene. Reactions of chloro bis(alkylenedithiophosphato) antimony(III) compounds, [OGOP(S)S] 2 SbCl with sodium tetraisopropoxoborate, NaB(OPr i ) 4 , in a 1:1 molar ratio in refluxing benzene yielded some new heterobinuclear derivatives of antimony(III) and boron(III) of the type[OGOP(S)S] 2 Sb(µ OPr i ) 2 B(OPr i ) 2 . These newly synthesized complexes have been characterized by elemental analysis and molecular weight measurement, and their plausible structures have been proposed on the basis of IR, NMR ( 1 H, 13 C, 31 P, 11 B), and FAB-mass spectral studies. On the basis of the spectroscopic evidence, a pseudo octahedral geometry around antimony and tetrahedral geometry around boron atom has been proposed. Cyclic O,O -alkylenedithiophosphate ligands and their corresponding chloro bis(alkylenedithiophosphato)antimony(III) compounds have been screened for microbial activities. These compounds showed significant antifungal activity against Fusarium and Trichoderma and antibacterial activity against E. Coli and Pseudomonas.