Abstract: | A new layered zinc phosphite with the formula (NH4){Zn(H2O)4}0.5Zn2(HPO3)3] has been synthesized under hydrothermal conditions. Its structure was determined by single‐crystal X‐ray diffraction. The compound crystallizes in the triclinic system, space group (No. 2), a = 7.2507(4), b = 9.7982(6), c = 10.2642(6) Å, α = 63.425(2), β = 87.165(2), γ = 72.999(3)°, V = 620.84(6) Å3, Z = 2. The connectivity of ZnO4 tetrahedra, HPO3 pseudo pyramids and ZnO2(H2O)4 octahedra results in macroanionic layers with 4.8 net. |