Hydrothermal synthesis and structural characterization of a three-dimensional organically-templated vanadium phosphate [H3NCH2CH2NH3][(VO)3(H2O)2(PO4)2(HPO4)]

The title compound [(H3NCH2CH2NH3)][(VO)(3)(H2O)(2)(PO4)(2)(HPO4)] was synthesized from the hydrothermal reaction of V2O5:V:H3PO4:H2NCH2CH2NH2:H2O in the mole ratio of 1:1:10:5:740. The compound crystallizes in the triclinic space group P (1) over bar with unit cell parameters a=10.187(1), b=10.241(1), c=8.2137(7) Angstrom, alpha=90.398(8), beta=95.930(9) and gamma=117.325(7)degrees, V=755.7(1) Angstrom(3), Z=2, D-calc=2.570 g cm(-3), R=0.032, Rw=0.035. The data were collected by using omega-2 theta scan technique and the structure was solved by direct method. The structure consists of binuclear units of corner-sharing [VO6] octahedra and square-pyramidal [VO5] units linked by phosphate tetrahedra, forming double extended polyhedral slabs in the (101) plane with these slabs connected by corner-sharing [HPO4] tetrahedra to form a corner-sharing three-dimensional cage structure about the diammonium cations. (C) 1998 Elsevier Science S.A.