Reaction of diphenylbis((methylthio)methyl)borate (Ph(2)Bt(-)) with Ni(BF4)(2) . 6H(2)O yielded square planar [Ph(2)Bt]Ni-2, 1. Chemical reduction of 1 with Na/Hg produced a species which represents a uniquely stable (NiS4)-S-I chromophore. X-band EPR data: g(1) = 2.27, g(2) = 2.11, g(3) = 2.03.