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Samples of the quaternary chalcogenide compounds, CuNiGaSe 3 and CuNiInSe 3 , prepared by direct fusion and annealing method, were characterized by X-ray powder diffraction. In each case, the crystal structure was refined using the Rietveld method. Both compounds were found to crystallize in the tetragonal system, space group P4 -2c (N°112), with unit cell parameter values a = 5⋅6213 (1) Å, c = 11⋅0282(3) Å, V = 348⋅48(1) Å 3 and a = 5⋅7857(2) Å, c = 11⋅6287(5) Å, V = 389⋅26(3) Å 3 for CuNiGaSe 3 and CuNiInSe 3 , respectively. These compounds have a normal adamantane structures and are isostructural with CuFeInSe 3 .

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