An electroless method of nickel hydroxide synthesis through the complexation-precipitation route which yields a fine particle material having a specific surface area of 178 m2g-1 The morphology of this material as revealed by electron microscopy is distinctly different from the turbostratic nature of electrosynthesized nickel hydroxide. While the long range structure as shown by the X-ray diffraction pattern is similar to that of beta-Ni(OH)2, the short range structure as revealed by infrared spectroscopy incorporates characteristics similar to that of alpha-Ni(OH)2. Cyclic voltammetry studies show that the electroless nickel hydroxide has a higher coulombic efficiency (> 90%), a more anodic reversible potential and a higher degree of reversibility compared to the electrosynthesized nickel hydroxide and conventionally prepared nickel hydroxide.