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-
Hydrothermal Synthesis, Structure, and Electrochemical Properties of a Three-Dimensional Vanadium-Nickel Phosphate (C2H10N2)4[H2Ni(H2O)2(VO)8(OH)4(PO4)8]·H2O. -The title compound is prepared by hydrothermal reaction of an aq. solution of V2O5, NiNO3, H3PO4, ethylenediamine, and ortho-phthalic acid in a molar ratio of 1:1.5:4.5:4:0.5 (autoclave, 165°C, 5 d; 83% yield). The crystal structure of (H 2 en) 4 [H 2 Ni(H 2 O) 2 (VO) 8 (OH) 4 (PO 4 ) 8 ]·H 2 O (monoclinic, space group P21/n, Z = 2; single-crystal XRD) consists of macroanionic V-Ni-P layers constructed from VO5 square pyramids, NiO6 octahedra, and PO4 tetrahedra. Protonated en molecules and water molecules further increase the stability of the structure. Its electron sponge behavior is proved by cyclovoltammetric tests and charge-discharge profiles.
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