Hydrothermal Synthesis and Crystal Structure of a New Supramolecular Channel Framework Based on Cu Complexes and Polyoxovanadate:[Cu(I)(phen)_2]_5[HV_(15)O_(36)(Cl)]_(0.65)[H_3V_(16)O_(38)(Cl)]_(0.35)·2H_2O

A new compound [Cu(I)(phen)2]5[HV15O36(Cl)]0.65[H3V16O38(Cl)]0.352H2O 1 (phen = 1,10-phenanthroline) has been prepared from the hydrothermal reaction of V2O5, CuCl, phen, H2C2O42H2O, THMAM (tris(hydroxymethyl)aminomethane) and H2O in the molar ratio of 3:1:1:0.5:2.5:1400. Compound 1 crystallizes in the space group P42212 of the tetragonal system with a = b = 21.5009(8), c = 28.401(2) , V = 13129.5(12) 3, Z = 4, Dc = 1.800 g/cm3, μ(MoKα) = 1.932 mm-1, λ(MoKα) = 0.71073 , F(000) = 7063.4, C120H81.20ClCu5N20O38.7V15.35, Mr = 3557.58, the final R = 0.0594 and wR = 0.1320 for 7761 observed reflections (I 2σ(I)). Structure analysis shows that 1 exhibits a 3D channel framework formed by the supramolecular assembly of Cu complexes and polyoxovanadate clusters via intermolecular hydrogen bonding, and the channels contain Cu complexes. Other characterizations by elemental analysis, XPS, IR, XRD and thermal analysis are also described.