Reaction of Ni(O(2)CMe)(2) . 4H(2)O with 1 molar equiv of Na(dbm) (dbmH = dibenzoylmethane) and NaOH in refluxing MeOH affords a green precipitate of [Ni-4(OMe)(4)(dbm)(4)(MeOH)(4)] (1), which can be recrystallized from chlorinated solvents; recrystallized yield 70%. Crystals of 1 . 2CH(2)Cl(2) have the following cell parameters at -111 degrees C : triclinic, P $($) over bar$$ 1, a = 14.566(2), b = 20.661(4), c = 13.367(2) Angstrom; alpha = 92.58(1), beta = 117.17(1), gamma = 72.87(1)degrees; V = 3433.2 Angstrom(3); Z = 2. The structure was solved and refined by employing 4631 reflections with F > 2.33 sigma(F) to final values of R (R(w)) of 6.00% (5.21%). The molecule consists of a [Ni-4(OMe)(4)](4+) cubane, each Ni-II ion being bound to three mu(3)-OMe(-) ions, one chelating dbm(-) group, and one terminal MeOH.