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DOI: 10.1039/A607212G (Paper) Reference Section for: J. Chem. Soc., Dalton Trans., 1997, 1219-1224

Deprotonation of the carbaborane nido-7-NH2But-7-CB10 H12: crystal structures of nido-7-NH2But-7-CB10 H12 and [NEt3(CH2Ph)][ nido-7-NHBut-7-CB10H12 ]

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John C. Jeffery, Paul A. Jelliss, James Karban, Vyacheslav Lebedev and F. Gordon A. Stone

Abstract

The crystal structure of nido-7-NH2But-7-CB10H12 1 has been determined by X-ray diffraction. The compound crystallises in the orthorhombic space group Pbca [a = 10.507(5), b = 13.805(6), c = 18.093(9) Å]. The nido-icosahedral structure was established with two endo-B–H–B and two NH2 hydrogen atoms located in Fourier-difference maps and refined. The structure determination is also supported by 11B-{1H}–11B-{ 1H} correlation NMR spectroscopy. A molecular orbital calculation and frontier density analysis of 1 indicated that deprotonation should initially occur at the exo-nitrogen atom. Treatment of 1 with 1 equivalent of LiBun, followed by addition of [NEt3(CH2Ph)]Cl, gave [NEt3(CH2Ph)][nido-7-NHBut -7-CB10H12] 2 as the only product and single crystals were grown for an X-ray diffraction study. The salt crystallises in the monoclinic space group P21/n [a = 10.651(2), b = 11.652(2), c = 20.926(3) Å, β = 101.77(2)°]. The 1H, 13C-{1H} and 11B-{1H} NMR spectra of 1 and 2 have also been recorded.

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