The bimetallic complexes of 2,2′‐malonylbis(N‐phenylhydrazine‐1‐carbothioamide) have been prepared and characterized by elemental and spectral analyses. The free ligand exists in keto‐thione form, whereas in complexes it chelated to the metal ion in binegative tetradentate and neutral tetradentate manners. The electronic spectra and magnetic moment measurements showed that all the complexes have an octahedral geometry except the [Cu2(H2L)(OAc)2]EtOH complex which has square planar structure supported by the electron spin resonance (ESR) spectral data. In addition, thermal gravimetric analysis (TGA) carried out to clarify thermal stability of the ligand and its complexes. The optical band gap (Eg) was calculated using Tauc's equation and compared with their HOMO‐LUMO gap obtained from DFT quantum chemical calculations. Furthermore, the in vitro cytotoxic activity against Hela (Epitheliod Carcinoma) and WISH (Human amnion) cell lines of isolated compounds were examined. The data indicated that the ligand has very strong activity against Hela cell line and moderate activity against WISH cell line. Accordingly, the metal complexes showed more potent effect against Hela than WISH cell lines.
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