Abstract: A new two-dimensional layered zinc phosphate (ZnHPO₄) was synthesized by means of hydrothermal method. The as-synthesized product was characterized by means of powder X-ray diffraction and IR spectroscopy. Single-crystal X-ray diffraction analysis shows that the title compound crystallized in the monoclinic space group P2(1)/c (No.14), with the parameters a=0.462　51(14) nm, b=1.360　8(4) nm, c=0.582　84(18) nm, β=98.752(5)°, V=0.362　56(19) nm³, Z=2, M＝161.35， R₁＝0.074　2， wR₂＝0.229　6. Its structure was built up by infinite four-remembered ring chains sharing vertices, generating a new two-dimensional layer structure.

Key words: hydrothermal synthesis, zinc phosphate, crystal structure