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New nanophenolic oxime complexes of the type [M(κ2‐Saly)2] {where HSaly = salicyl‐aldoxime; M = Co(1), Ni(2), Cu(3), Pd(4), Pt(5), Zn(6), Cd(7), and Hg(8)} were prepared and characterized by different spectroscopic methods. The surface morphology and the micrographs of the investigated complexes were checked by the scanning electron microscopy (SEM) and X‐ray diffraction (XRD) analysis. The results indicate the successful preparation of nanocomplexes with nanoparticles size. In addition, the antibacterial activity was studied against three different pathogenic bacteria, and the Pt(II) complex displayed the highest activity compared with free salicylaldoxime ligand and other complexes. Magnetic susceptibility and ultraviolet (UV)–visible spectroscopic measurements were used to deduce the geometry of the complexes, which was then validated by density functional theory (DFT) calculations. The in vitro antitumor activity was investigated by MTT assays against HepG‐2 cell lines. The Zn(II) and Pt(II) complexes displayed good activity with IC50 values at 17.31 ± 0.95 and 11.78 ± 0.54 μM, respectively. In contrast, the [Cu(Saly)2] and [Ni(Saly)2] complexes showed the lowest activity against tested cells. [ABSTRACT FROM AUTHOR]