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Issue 15, 2012
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Metathesis of alkali-metal amidoborane and FeCl3 in THF

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Abstract

Metathesis of LiNH2BH3 and FeCl3 in THF solution was investigated in detail. Instead of formation of expected Fe amidoborane i.e., 3LiNH2BH3 + FeCl3 → 3LiCl + Fe(NH2BH3)3, 1.5 equiv. H2/LiNH2BH3 together with LiCl and a black precipitate was produced as a result of salt metathesis and reduction of Fe3+ by BH3. The hydrogen was desorbed in two steps involving a homogeneous interaction of the two starting chemicals to form [Fe(H2N[double bond, length as m-dash]BH2)3] precipitate and subsequent solid-state dissociation of [Fe(H2N[double bond, length as m-dash]BH2)3] to yield a polymeric product, [Fe(HN[double bond, length as m-dash]BH)3]n, respectively. FTIR evidenced the persistence of B–H and N–H stretches in the above two solid products and following the dissociation of [Fe(H2N[double bond, length as m-dash]BH2)3] to release 1 equiv. H2/LiNH2BH3 the B–N bond strengthened. Mössbauer and XAFS both indicated that Fe atoms in these solids are in very similar chemical environments, linking to the neighbouring N and B atoms and bearing slightly positive charge. Most likely, H2N[double bond, length as m-dash]BH2 in [Fe(H2N[double bond, length as m-dash]BH2)3] binds to Fe as a π-bound ligand. The mechanism of salt metathesis and reduction of Fe3+ was confirmed based on simulation work on the homogeneous reaction process.

Graphical abstract: Metathesis of alkali-metal amidoborane and FeCl3 in THF

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Publication details

The article was received on 04 Dec 2011, accepted on 16 Feb 2012 and first published on 09 Mar 2012


Article type: Paper
DOI: 10.1039/C2JM16331D
Citation: J. Mater. Chem., 2012,22, 7478-7483
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    Metathesis of alkali-metal amidoborane and FeCl3 in THF

    T. He, J. Wang, Z. Chen, A. Wu, G. Wu, J. Yin, H. Chu, Z. Xiong, T. Zhang and P. Chen, J. Mater. Chem., 2012, 22, 7478
    DOI: 10.1039/C2JM16331D

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