The Structure of [HSi9 ]3- in the Solid State and Its Unexpected Highly Dynamic Behavior in Solution

Angewandte Chemie
Corinna LorenzRuth M Gschwind

Abstract

We report on the first unambiguous detection of the elusive [HSi9 ]3- anion in solutions of liquid ammonia by various 29 Si and 1 H NMR experiments including chemical exchange saturation transfer (CEST). The characteristic multiplicity patterns of both the 29 Si and 1 H resonances together with CEST and a partially reduced 1 H,29 Si coupling constant indicate the presence of a highly dynamic Si8 entity and a Si-H moiety with slow proton hopping. Theoretical calculations corroborate both reorganization of Si8 on the picosecond timescale via low vibrational modes and proton hopping. In addition, in a single-crystal X-ray study of (K(DB[18]crown-6))(K([2.2.2]crypt))2 [HSi9 ]⋅8.5 NH3 , the H atom was unequivocally localized at one vertex of the basal square of the monocapped square-antiprismatic cluster. Thus experimental studies and theoretical considerations provide unprecedented insight into both the structure and the dynamic behavior of these cluster anions, which hitherto had been considered to be rigid.

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Citations

Oct 18, 2018·Chemical Communications : Chem Comm·Thomas HennebergerThomas F Fässler
Jan 12, 2019·Angewandte Chemie·Kinga I LeszczyńskaDavid Scheschkewitz
Jun 25, 2019·Chemistry : a European Journal·Christoph WallachThomas F Fässler
Aug 7, 2019·Chemical Communications : Chem Comm·Lukas KlemmerDavid Scheschkewitz
Feb 25, 2020·Angewandte Chemie·Nadine E PoitiersDavid Scheschkewitz
May 5, 2020·Dalton Transactions : an International Journal of Inorganic Chemistry·C WallachT F Fässler
May 7, 2019·Chemical Science·Yannic HeiderDavid Scheschkewitz
Jul 24, 2020·Chemistry : a European Journal·Nadine E PoitiersDavid Scheschkewitz
Jun 24, 2021·Chemical Reviews·Yannic Heider, David Scheschkewitz
Jul 27, 2021·Journal of Magnetic Resonance·Ahallya JaladeepAshok Sekhar
Nov 16, 2019·Journal of the American Chemical Society·Yannic HeiderDavid Scheschkewitz
Oct 6, 2020·Inorganic Chemistry·Felix S Geitner, Thomas F Fässler

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