PREPARATION, B-11, C-13 NMR AND VIBRATION AL-SPECTRA OF AMINOMETHYLHEXAHYDRO-CLOSO-HEXABORATE(1-), [B6H6(CH2NH2)]-, AND CRYSTAL-STRUCTURES OF CS[B6H6(CH2NH2)] AND K[B6H6(CH2NH2)]

By reaction of [B6H6](2-) with N-(chloromethyl)phthalimide in dichloro methane the intermediate phthalimidomethylhexahydro-closo-hexaborate(1 -), [B6H6(CH2(NC8O2H4)](-), is formed which with an excess of hydrazin e reacts to give aminomethylhexahpdro-closo-hexaborate(1-). The crysta l structures of Cs[B6H6(CH2NH2)] and K[B6H6(CH2NH2)] have been determi ned by single crystal X-ray diffraction analysis. They are monoclinic, space group C2/ m with a = 11.123(6), b = 6.8441(11), c = 12.810(7)An gstrom, beta = 124.032(5)degrees for Cs[B6H6(CH2NH2)] and with a = 10. 767(21); b = 6.6255(6), c = 12.2648(14)Angstrom, beta = 123.880(10)deg rees for K[B6H6(CH2NH2)]. The B-11 NMR spectrum is consistent with a m ono hetero substituted octahedral B-6 cage with local C-4v symmetry. I n the C-13 NMR spectrum of Cs[B6H6(CH2NH2)] a quartet at 32.7 ppm with (1)J(C,B) 65 Hz is observed. The IR and Raman spectra exhibit charact eristic CH, NH, BH and B-6 vibrations.