By electrochemical oxidation of (n-Bu4N)[B6H5Hfac(C2H5)] in the presence of nitrite ions and of the base DBU in dichloromethane solution cis-[B6H4(C2H5)(NO2)]2- is formed. X-ray diffraction analysis has been performed on a single crystal of cis-(Ph4 As)2[B6H4(C2H5)(NO2)] (triclinic, space group P1; a = 10.673(4). b = 10.907(4), c = 21.237(4) A, α = 80.789(4), β = 83.117(4), γ = 66.548(2)°, Z = 2). The 11B NMR spectrum is consistent with a disubstituted octahedral B6 cage with local Cs symmetry. The IR and Raman spectra exhibit characteristic CH3, CH2, NO2, BN, BH and B6 vibrations