In this study, Ni(II) and Co(II) complexes Co(H 2 O) 2 L 2 ( 1 ), Ni(H 2 O) 2 L 2 ( 2 ), Co(phen)L 2 ( 3 ), Ni(phen)L 2 ·2H 2 O·EtOH ( 4·2H 2 O ), and Ni(phen) 2 (H 2 O)L·L·2H 2 O ( 5 ), where L—4,5-dichloro-isothiazole-3-carboxylate anion and phen—1,10-phenanthroline are reported. All complexes have been characterized by physicochemical and spectroscopic methods. Mass spectrometry and UV–Vis spectroscopy have been used to show the behavior of complexes in ethanol solution and phosphate buffer saline. Crystal structures of mononuclear complexes 1 , 4 and 5 have been determined by single-crystal X-ray diffraction. In the structure of 4 , mononuclear units have been found to form infinite zigzag chains due to the presence of Cl•••Cl non-covalent interactions which can be regarded as halogen bonding. All complexes have been screened in vitro for their cytotoxic activity against Hep2 cancer cell line. The complexes obtained showed no activity (IC 50  > 50 µM) in comparison with structurally related Cu(II) complex Cu(phen)(H 2 O)L 2 exhibiting dose-dependent toxicity comparable to that of cisplatin (IC 50  = 3.06 ± 0.07 µM (Cu(II) complex), IC 50  = 9.2 ± 0.5 µM (cisplatin)). DNA binding constants were determined using absorption titration: Cu(II), Ni(II) and Co(II) complexes possessed similar DNA binding efficacy (K b  ~ 10 4 ).