A novel layered zirconium phosphate [NH4](2)[Zr(OH)(3)(PO4)] has been synthesized by using nonaqueous method in an ethylene glycol medium. The as-synthesized product was further characterized by means of single-crystal and powder X-ray diffractions, TG-DTA, CHN elemental analysis, and IR. The compound consists of macroanionic layers of [ZrPO7H3](2-) separated by NH4+ cations.