A new mixed-valence iron(III)-zinc(II) diphosphate, Zn2+Fe3+ (P2O7)(2), has been prepared by a dry way and characterized structurally by several techniques. Analysis of the powder diffraction pattern of the synthesized di phosphate showed that it is isostructural with the iron(III)-iron(II) diphosphate, Fe2+Fe3+(P2O7)(2), crystallizing in an orthorhombic symmetry in the Pnma space group. Other physical properties were characterized using Mossbauer spectroscopy and Vibrating Sample Magnetometer measurements, which showed that this new phosphate with Fe3+ ions in VI coordination has a paramagnetic behavior at room temperature. Infrared and Raman spectroscopies were also used in this study to help characterizing structurally the new synthesized material.