A new ligand 1,4-bis(2-hydroxymethylphenyl)-1,4-dioxabutane was synthesized by reducing 1,4-bis(2-formylphenyl)-1,4-dioxabutane with NaBH4 in absolute methanol solution. The crystal structure of the title compound C16H18O4 has been determined by single-crystal X-ray diffraction. The ligand crystallizes in the orthorhombic system, space group Pbcn with a = 13.777(1), b = 11.731(1), c = 9.076(8) ? V = 1466.8(2) ?, Mr = 274.30, Z = 4, F(000) = 548, Dc = 1.24 g/cm3, T = 293 K, m = 8.9 cm-1 and l = 0.71073 ? The structure was refined to R = 0.0324 and wR = 0.1025 for 1112 observed reflections with I > 2s(I). The two benzene rings are not on the same plane, and the dihedral angle between them is 60.6? The ligand has C2 symmetry axis which passes through the center of C(8)C(8a). The molecules are linked to each other by hydrogen bonding network to form supramolecular chain. The ligands connect to each other through the hydrogen bonds to form one-dimensional chains which further connect through the hydrogen bonds to form two- and three-dimensional structures. A new ligand 1,4-bis (2-hydroxymethylphenyl) -1,4-dioxabutane was synthesized by reducing 1,4-bis (2-formylphenyl) -1,4-dioxabutane with NaBH4 in absolute methanol solution. the title compound C16H18O4 has been determined by single-crystal X-ray diffraction. The ligand crystallizes in the orthorhombic system, space group Pbcn with a = 13.777 (1), b = 11.731 (1), c = 9.076 = 1466.8 (2)?, Mr = 274.30, Z = 4, F (000) = 548, Dc = 1.24 g / cm3, T = 293 K, m = 8.9 cm-1 and l = 0.71073? The structure was refined to R = 0.0324 and wR = 0.1025 for 1112 observed reflections with I> 2s (I). The two benzene rings are not on the same plane, and the dihedral angle between them is 60.6 · The ligand has a C2 symmetry axis which passes through the center of C (8) C (8a). The molecules are linked to each other by hydrogen bonding network to form supramolecular chain. The ligands connect to each other through the hydrogen bonds to form one-dimensional chains which further connect throug h the hydrogen bonds to form two- and three-dimensional structures.