A new Mn2Ni2 cubane complex has been synthesized and characterized by single-crystal X-ray diffraction, FT IR spectra and elemental analysis. The title compound [(Mn2Ni2II)-Ni-III(hmp)(4)(N-3)(4)(O2CR)(2)] (hmp(-) is the anion of 2-pyridinemethanol and O2CR- is a-naphthaleneacetate) crystallizes in the monoclinic system, space group P2(1)/c with a = 10.519(5), b = 22.109(10), c = 23.235(9) angstrom, beta = 106.096(17)degrees, C48H42Mn2Ni6Ni2O8, M-r = 1198.28, V = 5192(4) angstrom(3), D-c = 1.533 g/cm(3), F(000) = 2448, mu = 1.258 cm(-1), Z = 4, the fmal R = 0.0875 and wR = 0.2020 for 3398 reflections with I > 2 sigma(I). X-ray diffraction analysis reveals that each Mn(Ill) center is octahedrally coordinated by two nitrogen atoms of azide anions and three oxygen atoms from three 2-pyridinemethanol anion ligands together with one oxygen atom from naphthaleneacetate. Each Ni(II) is octahedrally coordinated by two nitrogen atoms of 2-pyridinemethanol anion ligands as well as three oxygen atoms from three 2-pyridinemethanol anion ligands and one oxygen atom from naphthaleneacetate.