A new complex of N-(2,3,4,6-tetra-O-acetyl-β-D-glucopyranosyl)-thiocarbamic 4-hydroxy-benzoyl hydrazine dihydrate, C_22H_27N_3O_10S·2H_2O, was synthesized and its structure was determined by X-ray crystallography and TG/DTG methods. The compound belongs to the orthorhombic system, which crystallizes in space group P2_12_12_1, with a=1.0275(3), b=1.3419(4), c=2.0234(6), V=2.7899(16) nm~3, and Z=4. The hexopyranosyl ring adopts a ~4%C%_1 conformation. All the substituents are at equatorial positions. The molecules are linked into a three-dimensional framework via intermolecular interactions. Atoms O5 and O9 show positional disorders. A new complex of N- (2,3,4,6-tetra-O-acetyl-β-D-glucopyranosyl) -thiocarbamic 4-hydroxy- benzoyl hydrazine dihydrate, C_22H_27N_3O_10S · 2H_2O, was synthesized and its structure was determined by X The compound belongs to the orthorhombic system, which crystallizes in space group P2_12_12_1 with a = 1.0275 (3), b = 1.3419 (4), c = 2.0234 (6), V = 2.7899 16) nm ~ 3, and Z = 4. The hexopyranosyl ring adopts a ~ 4% C% _1 conformation. All the substituents are at equatorial positions. The molecules are linked into a three- dimensional framework via intermolecular interactions. Atoms O5 and O9 show positional disorders.