Two new supramolecular compounds were synthesized and characterized with the formula of [Cu(bipy) 2 (OAc)]Á(DBrS) 1/2 Á5H 2 O 1, [Co(phen) 2 (CO 3 )]Á(DBrS) 1/2 Á 5H 2 O 2 (H 2 DBS = meso-2,3-dibromosuccinic acid; bipy = 2,2'-bipyridine; phen = 1,10-phenanthroline). The crystal structures of complexes were determined by X-ray single-crystal diffraction. Complex 1 represents R6 water clusters and complex 2 stabilizes in a 1D water tape notated T4(2)6(2). For 2, the 2D layer is defined as a 2D (3,4,6)-connected network with the Schläfli symbol of (4Á5Á6) 4 (4 2 Á5Á6Á7 2 )(4 2 Á5) 2 (4 4 Á5 2 Á6 2 Á7 4 Á9 3 ). Results about i.r. spectra and elemental analyses are presented.