PREPARATION, B-11 NMR AND VIBRATIONAL-SPE CTRA OF AMINOHEXAHYDRO-CLOSO-HEXABORATE(1-), [B6H6(NH2)](-), AND THE CRYSTAL-STRUCTURE OF CS[B6H6(NH2)]CENTER-DOT-H2O
A. Franken et W. Preetz, PREPARATION, B-11 NMR AND VIBRATIONAL-SPE CTRA OF AMINOHEXAHYDRO-CLOSO-HEXABORATE(1-), [B6H6(NH2)](-), AND THE CRYSTAL-STRUCTURE OF CS[B6H6(NH2)]CENTER-DOT-H2O, Zeitschrift fur Naturforschung. B, A journal of chemical sciences, 50(1), 1995, pp. 11-14
By reduction of [B6H5(NO2)](2-) With Fe2+ in aqueous alkaline solution
[B6H6(NH2)](-) is formed. The compound has been separated by extracti
on with dichloromethane in the presence of tetrabutylammoniumbromid an
d precipitated from the organic phase by adding CsCH3COO/C2H5OH. The C
rystal structure of Cs[B6H6(NH2)].H2O has been determined by single cr
ystal X-ray diffraction analysis, monoclinic space group C2 with a = 2
2.1075(14), b = 6.491(2), c = 5.9570(4) Angstrom, beta = 100.168(6)deg
rees. The B-11 NMR spectrum is consistent with a mono-hetero-substitut
ed octahedral B-6 cage with local C-4v symmetry. The IR and Raman spec
tra exhibit characteristic N-H, B-H and B-6 vibrations.