Two new supramolecular compounds were synthesized and characterized with the formula of [Cu(bipy)(OAc)]·(DBrS)·5HO 1, [Co(phen)(CO)]·(DBrS)·5HO 2 (HDBS = 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 (4·5·6)(4·5·6·7)(4·5)(4·5·6·7·9). Results about i.r. spectra and elemental analyses are presented. [ABSTRACT FROM AUTHOR]