PREPARATION, B-11 NMR AND VIBRATIONAL-SPE CTRA OF CIS-DINITROTETRAHYDRO-CLOSO-HEXABORATE(2-), CIS-[B6H4(NO2)(2)](2-), AND THE CRYSTAL-STRUCTURE OF CIS-CS-2[B6H4(NO2)(2)]
A. Franken et W. Preetz, PREPARATION, B-11 NMR AND VIBRATIONAL-SPE CTRA OF CIS-DINITROTETRAHYDRO-CLOSO-HEXABORATE(2-), CIS-[B6H4(NO2)(2)](2-), AND THE CRYSTAL-STRUCTURE OF CIS-CS-2[B6H4(NO2)(2)], Zeitschrift fur Naturforschung. B, A journal of chemical sciences, 50(7), 1995, pp. 1030-1034
By electrochemical oxidation of [B6H6](2-) in the presence of nitrite
ions and of the base DBU in dichloromethane solution apart from [B6H5(
NO2)](2-) and [B6H5(NO)B6H5](3-) the dinitro anion cis-[B6H4(NO2)(2)](
2-) is formed and can be isolated by ion exchange chromatography on di
ethylaminoethyl cellulose. The crystal structure of the Cs salt has be
en determined from single crystal X-ray diffraction analyses. cis-Cs-2
[B6H4(NO2)(2)] is tetragonal, space group P $($) over bar$$ 42(1)m wit
h a = 10.0656(4), c = 11.0127(13) Angstrom. The B-11 NMR spectrum is c
onsistent with a disubstituted octahedral B-6 cage with local C-2v sym
metry. The IR and Raman spectra exhibit characteristic NO2, B-H and B-
6, vibrations.