Abstract. The three-dimensional vanadium-nickel phosphate (C 2 H 10 N 2 ) 4 [H 2 Ni(H 2 O) 2 (VO) 8 (OH) 4 (PO 4 ) 8 ]·H 2 O (1) was prepared by hydrothermal methods and its structure and electrochemical properties were characterized. The compound crystallizes in the monoclinic system with the space group P2 1 /n and cell parameters a = 14.392(3) Å, b = 10.122(2) Å, c = 18.305(4) Å, β = 90.34(3)°, V = 2666.7(9) Å 3 , Z = 2. The structure consists of macroanionic V-Ni-P layers con-