PREPARATION, B-11, C-13 NMR AND VIBRATION AL-SPECTRA OF YLHEXAHYDRO-CLOSO-HEXABORATE(1-),[B6H6(CH2CN)](-), AND THE CRYSTAL-STRUCTURE OF [P(C6H5)(4)][B6H6(CH2CN)]

By reaction of[B6H6](2-) with chloroacetonitrile in dichloromethane th e cyanomethylhexsthy-dro-closo-hexaborate(1-), [B6H6(CH2CN)](-) is for med. The compound has been separated from excess [B6H6](2-) by ion exc hange chromatography on diethylaminoethyl cellulose. The crystal struc ture of [P(C6H5)(4)][B6H6(CH2CN)] has been determined by single crysta l X-ray diffraction analysis; triclinic, space group P (1) over bar wi th a = 7.503(3), b = 12.0949(8), c = 14.6572(11)Angstrom, alpha = 79.3 99(6)degrees, beta = 79.19(2)degrees, gamma = 89.2(2)degrees. The B-11 NMR spectrum is consistent with a mono hetero substituted octahedral B-6 cage. In the C-13 NMR spectrum of Cs-2[B6H5(CH2CN)] a singlet at 1 31.9 ppm (CN) and a quartet at 2.97 ppm with (1)J(C,B) = 54.7 Hz (CH2) are observed. The IR and Raman spectra exhibit a very strong CN stret ching band at 2218 cm(-1).