Nonaqueous Synthesis and Characterization of a Novel Layered Zirconium Phosphate Templated with Mixed Organic and Inorganic Cations

A novel layered zirconium phosphate templated with organic diprotonated ethylendiamine
and inorganic ammonium cations, [NH4]2[H3N(CH2)2NH3]2[Zr3(OH)6(PO4)4], has been synthesized in a nonaqueous medium and characterized by single-crystal and powder X-ray
diffractions, thermal analysis, CHN elemental analysis, and infrared spectrum. The
compound crystallizes in the triclinic space group P1̄ (Z = 1), with a = 9.383(3) Å, b = 9.923(3) Å, c = 8.342(2) Å, α = 97.85(2)°, β = 111.75(2)°, γ = 113.01(2)°, and V = 627.0(4) Å3 (R
= 0.051 and Rw = 0.056). In this compound, the layer consists of eight- and four-membered
rings, which are formed by corner-sharing ZrO4(OH)2 octahedra and PO4 terahedra. Organic
diprotonated ethylendiamine and inorganic ammonium cations lie above and below the eight-
and four-membered windows within the layers, respectively. The two template cations are
arranged alternately over the layer surface and link adjacent layers through hydrogen bonds
of NH3+ and NH4+ groups.