The new Ni complex of sulfadimethoxine (SDMX) is prepared and investigated by infrared spectroscopy. The X-ray powder diffraction patterns of the Ni(II) complex of (SDMX) (c), Ni(CH3COO)2 (b) and (SDMX) (a) are recorded and compared. It is shown that the proposed structure for this complex derived from the infrared spectrum are consistent with the X-ray powder diffraction measurements and the elemental analysis results. Investigation of the infrared spectrum of the sample indicates that the vibrations due to the amino and sulfonamido groups are shifted with respect to the free molecule in line with their coordination to the metal.