The synthesis of nickel hydroxide by precipitation from a suitable solution containing dissolved Ni2+ ions is described. A large matrix of precipitation conditions is explored to generate a wide range of nickel hydroxide samples. While most precipitation reactions result in the formation of β-nickel hydroxide, the samples differ from one another in the degree of structural disorder as reflected by the differences in their powder X-ray diffraction (PXRD) patterns. A correlation of the long-range structure as deduced from diffraction studies with the short-range structure as deduced from infrared (IR) spectral studies is performed. The aim is to control the synthesis conditions to obtain materials with ‘tailor-made’ structural disorders.