The Mg 7.5 Ni 6 H 3 (AsO 4 ) 8 (OH) 6 and Mg 8 Ni 4 H 6 (PO 4 ) 8 (OH) 6 compounds have been synthesized by using hydrothermal techniques at high pressure and temperature. The crystal structure of the arsenate phase has been refined with the Rietveld method. The compounds are isostructural. The structure consists of a three-dimensional framework in which the presence of triangular and hexagonal channels is observed. Reflectance diffuse measurements confirm the hexacoordination of the Ni(II) ions in both compounds. The magnetic behaviour indicates the presence of antiferromagnetic interactions between the Ni(II) ions placed in the double chains.