PREPARATION, B-11 NMR AND VIBRATIONAL-SPE CTRA OF MONOCYANOMONONITROTETRAHYDRO-CLOSO-HEXABORATE(2-), CIS-[B6H4(CN)(NO2)(2-), U-NITROSO-BIS(MONOCYANOTETRAHYDRO-HEXABORATE)(3-), CIS-[(CN)B6H4(NO)B6H4(CN)](3-) AND THE CRYSTAL-STRUCTURE OF [AS(C6H5)(4)](2)-CIS-[B6H4(CN)(NO2)]
A. Franken et W. Preetz, PREPARATION, B-11 NMR AND VIBRATIONAL-SPE CTRA OF MONOCYANOMONONITROTETRAHYDRO-CLOSO-HEXABORATE(2-), CIS-[B6H4(CN)(NO2)(2-), U-NITROSO-BIS(MONOCYANOTETRAHYDRO-HEXABORATE)(3-), CIS-[(CN)B6H4(NO)B6H4(CN)](3-) AND THE CRYSTAL-STRUCTURE OF [AS(C6H5)(4)](2)-CIS-[B6H4(CN)(NO2)], Zeitschrift fur Naturforschung. B, A journal of chemical sciences, 50(9), 1995, pp. 1362-1368
By electrochemical oxidation of [B6H5(CN)](2-) in the presence of nitr
ite ions and of the base DBU in dichloromethane solution Cis-[B6H4(CN)
(NO2)](2-) and cis- [(CN)B6H4(NO)B6H4(CN)](3-) are formed and can be i
solated by ion exchange chromatography on diethylaminoethyl cellulose.
The crystal structure of the tetraphenylarsonium salt has been determ
ined by single crystal X-ray diffraction analysis. [As(C6H5)(4)](2)-ci
s-[B6H4(CN)(NO2)] is monoclinic, space group P2(1)/a with a = 20.343(5
), b = 10.896(2), c = 21.572(5) Angstrom and beta = 107.30(2)degrees.
The B-11 NMR spectra are consistent with disubstituted octahedral B-6
cages with local C-2v symmetry. The IR and Raman spectra exhibit chara
cteristic NO2, NO, CN, BH, and B-6 vibrations.