Two new bimetallic and trimetallic compounds (NH4)1.5Ni2V2O7(OH)1.5 · H2O and (NH4)1.5Cu1.125 Ni1.125V2O7(OH)2 · H2O were synthesized by hydrothermal method and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), thermogravimetric analysis (TGA), and X-Ray fluorescence (XRF). Crystallographic studies showed that both compounds are hexagonal with space group P-62c.