Tetrametallic molecular rectangles have been synthesized by combining rhenium(I) thiolate dimers with difunctional pyridyl and pyrazyl type ligands. The proposed rectangular structures are supported by H-1 NMR, MS, and IR absorption measurements. In addition, crystal structures of two of the rectangles are presented showing frameworks with dimensions 3.81 x 11.57 and 3.69 x 7.22 Angstrom, as defined by the rhenium atoms.