Treatment of Ln2(SO4)3·nH2O (Ln = La, Ce, Pr, Nd, Sm. Eu, Gd ; n = 8, 9) with phenelzine dihydrogen sulfate, (phzH2) SO4, in 1N H2SO4 yields polymeric complexes with the general formula [Ln(SO4)2(H2O)2(phzH)], which contain the phzH+ cation as a ligand. The compounds have been characterized by elem ental analyses, X-ray powder patterns, thermal methods, magnetic susceptibilities and spectroscopic (IR, Raman, electronic diffuse reflectance and solid-state emission f-f spectra) studies. The prepared complexes most probably consist of 7-coordinated units, formed by four bridging bidentate sulfato groups, two terminal aqua molecules and one cationic phzH+ ligand.