A 3-D network is self-assembled from a square-planar Ni(II) macrocyclic complex containing hydroxyl pendent chains and a terephthalato (tp(2-)) ligand. In the crystal, two series of linear chains extending different directions are alternately packed and interconnected by the hydrogen-bonding interactions between the pendent hydroxyl groups and the secondary amines of the macrocycles. The solid is able to bind water reversibly.