HYDROTHERMAL SYNTHESIS AND CRYSTAL-STRUCTURE OF AN ORGANICALLY TEMPLATED OPEN-FRAMEWORK VANADIUM PHOSPHATE - (H3NCH2CH2NH3)(4)[V-III(H2O)(2)(V(IV)O)(6)(OH)(2)(HPO4)(3)(PO4)(5)]CENTER-DOT-3H(2)O

An ethylenediamine encapsulated open-framework vanadium phosphate, (H3NCH2CH2-NH3)(4)[V-III(H2O)(2)((VO)-O-IV)(6)( OH)(2)(HPO4)(3)(PO4)(5)]. 3H(2)O (1) has been synthesized from the hydrothermal reaction of V2O5:H3PO4:H2NCH2CH2NH2:H2O in a mole ratio of 1:6.9:3.6:265 at 170 degrees C for 5 days, and its structure determined by single-crystal X-ray crystallography. Phosphate 1 is monoclinic, space group C2/c, a = 20.674 (2) Angstrom, b = 9.956 (2) Angstrom, c = 23.694 (1) Angstrom, beta = 101.154 (5) Angstrom. Z = 4, V = 4784.8 (10) Angstrom(3). Refinement with 3757 observed reflections for which I greater than or equal to 3 sigma(I) gave R = 0.039 and R(w) = 0.040. The structure consists of layers built from V(IV) square pyramids and mu(2)-OH bridged V(IV) pyramids with (HPO4)(2-) and (PO4)(3-) tetrahedra connected together by V(III) octahedra to give rise to the formation of very large interconnected tunnels parallel to the b axis and [101] direction. The tunnels are occupied by ethylenediammonium and water molecules.