SYNTHESIS, B-11 NMR, VIBRATIONAL-SPECTRA, AND CRYSTAL-STRUCTURE OF (PPH4)[1-(NO)B10H9]

By reaction of (n-Bu4N)(2)[B10H10] in aqueous acetonitrile with NO2 a reaction mixture is formed from which [1-(NO)B10H9](-) has been isolat ed by ion exchange chromatography on diethylaminoethyl(DEAE) cellulose . The X-ray structure determination of (PPh4)[1-(NO)B10H9] (triclinic, space group P (1) over bar, a = 7.6553(11), b = 13.179(2), c = 14.122 (3) Angstrom, alpha = 69.853(13), beta = 82.445(14), gamma = 87.230(13 )degrees, Z = 2) reveals the coordination of the NO group via N in an apical position of the B-10 cluster with B1-N = 1.457(5) and N-O = 1.1 01(4) Angstrom. The B-11 NMR spectrum exhibits the characteristic feat ure (1:1:4:4) of a in 1 position substituted B-10 cluster with a stron g downfield shift of the ipso-B atom at +6.5 ppm. The IR and Raman spe ctra show a strong NO stretching vibration at 2219 cm(-1).