From neutral to ionic species: Syntheses and X-ray crystallographic and multinuclear NMR spectroscopic studies of Li⋯P(SiMe3)- PtBu2 and Its Solvent Complexes

Ewald Sattler, Eberhard Matern, Alexander Rothenberger, Alexander Okrut, P. Bombicz, Ignacio Fernández, Ilona Kovács

Research output: Contribution to journalArticle

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Abstract

Li(THF)3P(SiMe3)-PtBu2 (1, THF = tetrahydrofuran) has been prepared by the reaction of (Me3Si) 2P-PtBu2 with n-butyllithium in THF and isolated in good yields. Compound 1 eliminates THF in vacuo to yield the dimeric [Li(THF)P(SiMe3)-PtBu2]2 (2). By metalation of H(SiMe3)P-PtBu2 with n-butyllithium in hexane, the solvent-free derivative [Li(Me3Si)P-PtBu2]4 (3) has been prepared. Compounds 1-3 form the ionic species [Li(TMEDA) 2]+[(Me3Si)P-PtBu2]- [4, TMEDA = Me2N(CH2)2NMe2] and [Li(12-crown-4)2]+[(SiMe3)P-PtBu 2]- (5) with TMEDA and 12-crown-4, respectively, in solution. The molecular structures of 1-5 were established by single-crystal X-ray diffraction. Compound 3 forms a cyclic tetramer with a flat butterfly geometry. Extensive solution NMR spectroscopic investigations have shown that all species except for 3 exist in the same form in solution as in the solid state. Moreover, multinuclear variable-temperature NMR studies showed that 2 is involved in a rapid conversion between conformers at 298 K, which can be slowed down on the NMR timescale at 183 K.

Original languageEnglish
Pages (from-to)221-232
Number of pages12
JournalEuropean Journal of Inorganic Chemistry
Issue number1
DOIs
Publication statusPublished - Jan 2014

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Nuclear magnetic resonance
X rays
Hexanes
Molecular structure
Single crystals
Derivatives
X ray diffraction
Geometry
phenyllithium
Temperature
n-butyllithium
12-crown-4
tetrahydrofuran

Keywords

  • Donor ligands
  • Lithium
  • NMR spectroscopy
  • P ligands
  • Structure elucidation

ASJC Scopus subject areas

  • Inorganic Chemistry

Cite this

From neutral to ionic species : Syntheses and X-ray crystallographic and multinuclear NMR spectroscopic studies of Li⋯P(SiMe3)- PtBu2 and Its Solvent Complexes. / Sattler, Ewald; Matern, Eberhard; Rothenberger, Alexander; Okrut, Alexander; Bombicz, P.; Fernández, Ignacio; Kovács, Ilona.

In: European Journal of Inorganic Chemistry, No. 1, 01.2014, p. 221-232.

Research output: Contribution to journalArticle

Sattler, Ewald ; Matern, Eberhard ; Rothenberger, Alexander ; Okrut, Alexander ; Bombicz, P. ; Fernández, Ignacio ; Kovács, Ilona. / From neutral to ionic species : Syntheses and X-ray crystallographic and multinuclear NMR spectroscopic studies of Li⋯P(SiMe3)- PtBu2 and Its Solvent Complexes. In: European Journal of Inorganic Chemistry. 2014 ; No. 1. pp. 221-232.
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