Abstract. Mercury(II) complexes of thiolates having the general formula [Hg(RS)Cl 2 ]− and [Hg(RS) 2 ] have been prepared and characterized by IR and NMR ( 1 H and 13 C) spectroscopy (RSH = 2-aminoethanethiol hydrochloride (Aet), cysteine (Cys), thiosalicylic acid (Ts) and 2-mercaptonicotinic acid (Mnt)). The spectral data suggests that the coordination of thiolates to mercury(II) occurs through the sulfur as indicated by the absence of S-H vibrations in IR and significant downfield shifts in the C-S resonance in 13 C NMR. However, in Mnt complexes, coordination through both sulfur and nitrogen is indicated. Antimicrobial activities of the complexes were evaluated by minimum inhibitory concentration and the results showed that the complexes exhibited a wide range of activities against gram-negative bacteria (E. coli, P. aeruginosa), while moderate activity was observed against a mold, P. citrinum.