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.
