Abstract: A new reduced molybdenum phosphate, ［Ni(phen) ₃］₂［Ni(PO₄)₂(H₂PO₄)6(OH)₆(MoO₂)₁₂］(phen: 1,10\|phenanthroline), was synthesized by mild hydrothermal techniques, and the crystal structure was determined by singlecrystal X-ray diffraction analysis. The compound crystallized in the triclinic space groupP1 with a=1.404 2(3) nm,b=1.405 0(3) nm, c=1.408 2(3) nm, α=74.53(3)°, β=74.72(3)°, γ=74.81(3)°, V=2.527 6(9) nm3, Z=1, R1=0.076 2, wR2=0.168 6.

Key words: polyoxometalate, reduced molybdenum phosphate, hydrothermal synthesis, crystal structure