SYNTHESIS, B-11, C-13, H-1-NMR AND VIBRAT IONAL-SPECTRA OF 2,2'-BIPYRIDYL-UNDECAHYDRO-CLOSO-DODECABORATE(1-) AND CRYSTAL-STRUCTURE OF (PH4AS)[(2,2'-C10H8N2)B12H11]CENTER-DOT-CH3CN

By reaction of (n-Bu4N)(2)[B12H12] with 2,2'-bipyridine at 190 degrees C the 2,2'-bipyridyl-undecahydro-closo-dodecaborate anion [(2,2'-C10H 8N2)B12H11](-) is formed which can be seperated from excess [B12H12](2 -) by ion exchange chromatography on diethylaminoethyl (DEAE) cellulos e. The X-ray structure determination of (Ph4As)[(2,2'-C10H8N2)B12H11] (monoclinic, space group P2(1)/c with a = 13.3190(9), b = 10.1532(14), c = 28.788(3) Angstrom, beta = 96.761(7)degrees, Z = 4) reveals that the bipyridyl substituent is bonded via one nitrogen atom. The B-11 NM R spectrum exhibits a 1:5:5:1 pattern with ipso-B1 at -0.3, B2-B6 at - 14.5, B7-B1l at -15.3 and antipodal-B 12 at -15.9 ppm. The C-13 and H- 1 NMR spectra show the characteristic patterns of the bipyridyl group in the range of 124.5 to 158.6 (C-13) and 7.4 to 9.6 ppm (H-1) respect ively. The IR and Raman spectra exhibit characteristic BH stretching v ibrations between 2445 and 2568 cm(-1) and the stretching of the CC an d CN bonds in the range of 1427 to 1619 cm(-1).