Complexes of Schiff bases with some transition metals show significant biological notification including antimicrobial, antibacterial, antifungal and anticancer activities. Azocompounds have been studied widely because of their excellent thermal, antibacterial activity and optical properties in applications such as optical recording medium, toner, ink-jet printing and oil-soluble lightfast dyes. Metal complexes of thiosemicarbazone are well known for their pharmacological applications, while quinoline derivatives (in particular, quinoline carbaldehydes) display bactericidal, insecticidal and fungicidal properties. The combination of both active moieties in one molecular entity appears promising for the preparation of biologically active compounds. In this paper, we report new four mononuclear Ni(II) and Cu(II) complexes: NiL1]I (1), [CuL1I] (2), [NiL2]I (3) and [CuL2I] (4) with N3O binding system obtained by metaldirected condensation of quinoline-8-aldehyde with acetyl or benzoylacetone mono-Smethylisothiosemicarbazone (H2L1 and H2L2). The compounds were characterized by elemental analysis, ESI MS and IR-spectroscopy. The molecular structures of 1 and 2 were established by X-ray diffraction method (Fig. 1). The investigations confirmed that the Ni(II) compounds are ionic with an iodide anion in the external sphere and the Cu(II) complexes are molecular, the iodide anion being coordinated to the metal atom. The X-ray diffraction studies revealed a square-planar structure of the Ni(II) ionic complex and a square-pyramidal structure of the Cu(II) molecular complex.