Two new complexes, [Zn(phen)(2)(H2O)(2)]2L(.)H(2)O (1) and [Cu(phen)(L)(H2O)2]L(.)3H(2)O (2), where HL= 4-aminobenzenesulfonic acid and phen = o-phenanthroline, have been synthesized and their crystal structures determined by X-ray diffraction. In the complexes the Cu(II) and Zn(II) atoms revealed two different coordination environments. Complex 1 consists of a cation [Zn(phen)(2)(H2O)(2))(2+), in which Zn(II) is six-coordinated by four nitrogen atoms from two o-phenanthroline molecules and by two water molecules. Complex 2 has two crystallographically unique Cu(II) ions, where Cu(II) ion is five-coordinate with two nitrogen atoms of o-phenanthroline, two water molecules and one sulfonate oxygen atom. The electrochemical behavior and FT-IR of the two compounds have also been studied in detail.