Hydrothermal synthesis and characterization of a novel two-dimensional framework materials constructed from polyoxometalate and coordination groups: [H₂Mo_5.5V_10.5O₄₀(PO ₄)][Cu(en)₂]₄·7H₂O

A novel compound [H₂Mo_5.5V_10.5O₄₀(PO ₄)][Cu(en)₂]₄·7H₂O (1) was synthesized from V₂O₅, MoO₃, CuCl₂·2H₂O, en, H₃PO₄ and H₂O in an aqueous solution via the hydrothermal method and characterized by means of single-crystal X-ray diffraction, elemental analyses, IR, EPR spectra and thermal analyses. C₁₆H₈₀Cu₄Mo_5.5 N₁₆O₅₁PV_10.5 crystallized in a triclinic system, the space group is P1̄ with M = 2660.63, a = 1.283590(10) nm, b = 1.289910(10) nm, c = 1.387870(10) nm, V = 1.80942(2) nm³, Z = 2, D_x = 4.883 g/cm³, F(000) = 2599, μ=6. 956 mm^-1, (Δ/σ) = 0.000, S = 1.089. The crystal structure was solved by the direct methods with the final R = 0.0752 and ωR = 0.1988 for 6311 observed reflections with I≥2σ(I). The X-ray crystallography reveals that compound 1 is a novel two-dimensional framework material constructed from the mixed Mo/V polyoxometalate and coordination groups.