New inorganic - organic layered compounds were prepared by ion-exchange reactions of zinc-nitrate and copper-nitrate HDSs with organic carboxylic acids whose interlayer spacings increased depending on the sizes of carboxylic acids. The amounts of ion-exchanged 2-naphthoic acid and 2,6-naphthalene dicarboxylic acid were larger than those of 1-naphthoic acid and 2,7-naphthalene dicarboxylic acid, respectively, indicating the molecule recognition ability of the HDSs.