Routine solution reaction of Gd3＋ and p-phenylenediamine-N,N,N′,N′-tetraacetic acid （p-PhDTA） yields a dinuclear complex [Gd2（ox）（p-PhDTA）2（H2O）10]·6H2O （ox = oxalate）, which was characterized by single-crystal X-ray diffraction （MoKα radiation, = 0.71073）, elemental analysis and IR. This complex crystallizes in the monoclinic system, space group P21/n with a = 10.2522（8）, b = 10.0053（8）, c = 23.8834（18）, = 99.1080（10）°, V = 2419.0（3）3, Z = 2, Mr = 1367.32, Dc = 1.877 g/cm3, F（000） = 1368, = 2.830 mm-1, the final R = 0.0337 and wR = 0.0794 for 4747 observed reflections （I 〉 2 （I））. The exo-tetradentate oxalate ligand, generated in situ from the oxidative coupling of methanol, is incorporated to construct a dinuclear Gd2（ox）2 unit decorated with p-PhDTA ligands on the two sides with a monodentate coordination mode. The dinuclear molecules are further connected by the lattice water molecules to form a three-dimen- sional hydrogen network.
