The hydrothermal reaction of NH 4VO 3, CoCl 2·6H 2O, o-phen and H 2O gave a novel two-dimensional layered polyoxovanadate, [Co(o-phen)]V 2O 6·H 2O, which was constructed from {V 2O 6} chains linked by Co(o-phen) complex fragments. [Co(o-phen)]V 2O 6·H 2O was characterized by IR, TG and single-crystal X-ray diffraction. It crystallizes in monoclinic space group P2(1)/c with a= 0.785 2(9) nm, b=2.118 3(2) nm, c=0.946 3(11) nm, β=112.827(2)°, V=0.145 1(3) nm3, D c=2.074 g/cm3, Z=4, R 1=0.038 8, wR 2=0.094 1.
