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The published procedure for the synthesis of pyrrolidone-5-hydroxamic acid was improved. The acidity constant of the pyrrolidone-5-hydroxamic acid was determined as pKa = 8.65. In an aqueous solution of iron (III) ions, pyrrolidone-5-hydroxamic acid binds ferric ion, forming a mixture of mono-, bis-, and tris(pyrrolidone-5-hydroxamato)iron (III) complexes. These complexes were studied by potentiometric and spectrophotometric methods. The tris compound was isolated as dark orange-red crystals and identified according to elemental analysis and IR spectral data as C15H21FeN6O9.6H2O, having the magnetic moment of 5.67 B.M.