Synthesis, B-11 NMR and vibrational spectra of mononitrooctahydro-closo-nonaborate (2-) and monoaminooctahydro-closo-nonaborate(2-) and crystal structure of (Ph4P)(2)[1-(NO2)B9H8]center dot CH3CN

By electrochemical oxidation of (n-Bu4N)(2)[B9H9] in the presence of nitrit e ions and the base DBU in dichloromethane solution [1-(NO2)B9H8](2-) is fo rmed. X-ray diffraction analysis has been performed on a single crystal of (Ph4P)(2)[1-(NO2)B9H8] . CH3CN (monoclinic, space group P2(1): a = 10.643(5 ), b = 32.661(5), c = 13.924(5) Angstrom, beta = 96.68 degrees. Z = 4). By reduction of [1-(NO2)B9H8](2-) with FeSO4 in aqueous alkaline solution the amino derivative [1-(NH2)B9H8](2-) is formed. The B-11 NMR spectra of both compounds are consistent with a monosubstituted tricapped trigonal prism. T he IR and Raman spectra exhibit characteristic BE, BH, NO and NH vibrations , respectively.