Reaction of group 12 metal dihalides in ethanolic media with 2‐acetylpyridine ⁴N‐phenylthiosemicarbazone (H4PL) and 2‐acetylpyridine‐N‐oxide ⁴N‐phenylthiosemicarbazone (H4PLO) afforded the compounds [M(H4PL)X₂] (X = Cl, Br, M = Zn, Cd, Hg; X = I, M = Zn, Cd) (1–8), [Hg(4PL)I]₂ (9) and [M(H4PLO)X₂] (X = Cl, Br, I, M = Zn, Cd, Hg) (10–18). H4PL, H4PLO and their complexes were characterized by elemental analysis and by IR and ¹H and ¹³C NMR spectroscopy (and the cadmium complexes by ¹¹³Cd NMR spectroscopy), and H4PL, H4PLO, (5 · DMSO) and (9) were additionally studied by X‐ray diffraction. H4PL is N,N,S‐tridentate in all its complexes, including 9, in which it is deprotonated, and H4PLO is in all cases O,N,S‐tridentate. In all the complexes, the metal atoms are pentacoordinate and the coordination polyhedra are redistorted tetragonal pyramids. In assays of antifungal activity against Aspergillus niger and Paecilomyces variotii, the only compound to show any activity was [Hg(H4PLO)I₂] (18).