A new bidentate Schiff-base ligand derived from 4-nitro-o-phenylenediamine and 3-phenylpropenal and its complexes with Co(II) and Ni(II) metal ions have been synthesized. Various methods like thermogravimetric analysis (TGA), nuclear magnetic resonance (1H- and 13C-NMR), molar conductance, furrier transform infrared (FT-IR) and Ultraviolet–Visible (UV-Vis) spectroscopies are applied for characterization of Schiff-base ligand and its complexes. Based elemental analysis data the MLX2 [M=Co(II) and Ni(II); X=Cl, Br and L=N,N'–bis((E)-3–phenylallylidene)-4-nitro-1,2-phenylenediamine] formula is supposed for these metal complexes. Low molar conductivities in DMF confirm their non-electrolytic nature of them, just in the case of NiLBr2 the slight electrolyte character might be observed. Other evidences that confirmed the formation of Schiff-base complexes are changes in the location and shape of the peaks in UV-Vis and FT-IR spectra of complexes with respect to free ligand and distorted-tetrahedral structure is suggested for metal complexes. Anticancer activities of these complexes against A549 cancer cell line demonstrated these complexes are excellent candidates in the biological systems.