N-phenyl b-nitrobenzo hydroxamic acid had been prepared by coupling reaction of the prepared of N-phenyl hydroxylamine and methyl nitro benzoate in alkaline media was characterized by melting point (205-206⁰C), characters iron and copper color test, FT-IR characteristics spectral bands at 3112cm^-1 (OH),1693 cm^-1 (C=O) and 931 cm^-1 (N-O). The ¹H NMR spectrum shows the characteristic attachment of the proton of the hydroxyl group to the nitrogen atom in the region(7.43 – 7.70) ppm, the shift of the resonance signal of hydroxyl proton to lower field to support intermolecular hydrogen bonding, the appearance of protons of aromatic ring in the region (8.06 – 8.35) ppm. The ¹³C NMR spectra exhibit absorption signal due to carbonyl (C=O) nearly 166.26 ppm. The chemical shifts of aromatic carbons appear in the region (122.49 – 150.45) ppm. Beside these signals, a signal nearly 16 ppm appeared which corresponding to carbon atom of alkyl group. Iron (III) and copper (II) N-phenyl b-nitrobenzo hydro xamate complexes were prepared by reacting, N-phenyl b-nitro benzo hydroxamic acids with corresponding metal salts at pH= 3. Showing the characteristic colors. They show absorbance at a wavelength of maximum (λ_max) 415nm, 425 nm for Fe³⁺,Cu²⁺ complexes respectively indicating that the metal ligand complexes were formed from both.