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A three-dimensional coordination polymer, [Ni(Hbyip ion is five-coordinated by three carboxylate O atoms from three different 5-(benzoic acid-4-yldiazenyl)isophthalate (Hbyip anions and each Hbyip ions affording a 36-membered inorganic ring.These rings are further arranged into an undulated two-dimensional layer parallel to the (101) plane.Adjacent two-dimensional networks are linked by bix ligands into a three- dimensional {6} {6,8} network interpenetrates with two others in a parallel fashion to generate a 3-fold interpenetrating network.