A new trimetallic compound with formula (NH 4 )Ni 2.4 Co 0.6 O(OH)(MoO 4 ) 2 •1.5H 2 O was obtained by hydrothermal synthesis. The solid was characterized by X-ray diffraction, thermal analysis (thermogravimetric analysis and differential thermal analysis), Fourier-transformed infrared spectroscopy, Laser Raman spectroscopy, and chemical analysis by atomic absorption, confirming the formation of the layered phase ϕ y . Crystallographic studies showed that the compound obtained is trigonal with hexagonal unit-cell parameters, a = 6.0468 ± 0.0016 Å and c = 21.8433 ± 0.0001 Å, and space group R -3 m .