Monosaccharide (D-Glc, D-Fru, D-Gal, D-Xyl, D-Rib) and disaccharide (Mall complexes of Ni(II) were synthesised using [NEt4]2[NiCl2Br2] or NiCl2 · 6H2O in nonaqueous medium. The compounds synthesised from these two starting materials are different. The isolated complexes were characterized by diffuse reflectance, aqueous solution absorbance, CD, FTIR, magnetic susceptibility, and EXAFS and XANES studies.