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Abstract <p>Insertion of a bulky carbodiimide, ArN=C=NAr (Ar&#xa0;=&#xa0;C<sub>6</sub>H<sub>3</sub><i>i</i>Pr<sub>2</sub>-2,6) into the Li–N bond of LiN[CH(CH<sub>3</sub>)<sub>2</sub>]<sub>2</sub> in THF and subsequent extraction with hexane leads to lithium guanidinate complex, [Li{ArNC(N<i>i</i>Pr<sub>2</sub>)NAr}(THF)] (<b>1</b>). Salt metathesis reaction between equimolar ratios of <b>1</b> and CrCl<sub>2</sub> in THF and extraction with hexane resulted in a mono(guanidinate) chloride-bridged dimeric chromium complex, [Cr{ArNC(N<i>i</i>Pr<sub>2</sub>)NAr}(µ-Cl)]<sub>2</sub> (<b>2</b>). X-ray analysis confirms <b>1</b> to be monomeric in which guanidinate ligand shows η<sup>1</sup> and η<sup>3</sup> coordination through one of the N atoms and an arene moiety. In complex <b>2</b> guanidinate ligand adopts η<sup>2</sup> coordination mode, thus Cr atom is four-coordinated with distorted square planar geometry. Extraction of chromium with ether instead leads to an “ate” complex, [Cr{ArNC(N<i>i</i>Pr<sub>2</sub>)NAr}(µ-Cl)<sub>2</sub>Li(THF)<sub>2</sub>] (<b>3</b>). Hirshfeld surface analysis indicated that H⋯H interactions and H⋯C/C⋯H H-bonding were the two main contributors to the intermolecular interactions in the solid state.</p>

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Lithium and Chromium Complexes of a Bulky Guanidinate – Synthesis and Structure

  • 期刊论文

  • 发表日期：

    2025年6月1日

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  • S. Qayyum,
  • A. Noor

摘要

Abstract

Insertion of a bulky carbodiimide, ArN=C=NAr (Ar = C6H3iPr2-2,6) into the Li–N bond of LiN[CH(CH3)2]2 in THF and subsequent extraction with hexane leads to lithium guanidinate complex, [Li{ArNC(NiPr2)NAr}(THF)] (1). Salt metathesis reaction between equimolar ratios of 1 and CrCl2 in THF and extraction with hexane resulted in a mono(guanidinate) chloride-bridged dimeric chromium complex, [Cr{ArNC(NiPr2)NAr}(µ-Cl)]2 (2). X-ray analysis confirms 1 to be monomeric in which guanidinate ligand shows η1 and η3 coordination through one of the N atoms and an arene moiety. In complex 2 guanidinate ligand adopts η2 coordination mode, thus Cr atom is four-coordinated with distorted square planar geometry. Extraction of chromium with ether instead leads to an “ate” complex, [Cr{ArNC(NiPr2)NAr}(µ-Cl)2Li(THF)2] (3). Hirshfeld surface analysis indicated that H⋯H interactions and H⋯C/C⋯H H-bonding were the two main contributors to the intermolecular interactions in the solid state.