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Issue 48, 2018
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Isolation of reactive Ln(II) complexes with C5H4Me ligands (CpMe) using inverse sandwich countercations: synthesis and structure of [(18-crown-6)K(μ-CpMe)K(18-crown-6)][CpMe3LnII] (Ln = Tb, Ho)

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Abstract

Although attempts to make the Y(II) complex, (CpMe3Y)1− (CpMe = C5H4Me), by reduction of CpMe3Y with potassium were unsuccessful and the products of potassium reduction of CpMe3Ln for Ln = La and Pr led to ring-opening reduction of THF, we report that crystallographically-characterizable Ln(II) complexes of Tb and Ho can be isolated by reducing CpMe3Ln(THF) with KC8 in THF in the presence of 18-crown-6 (18-c-6). X-ray crystallography revealed that these complexes are isolated with a methylcyclopentadienide inverse sandwich countercation: [(18-c-6)K(μ-CpMe)K(18-c-6)][CpMe3Ln] (Ln = Tb, Ho). Although reduction of CpMe3Ln with potassium in the presence of the 2.2.2-cryptand (crypt) chelate has not generally provided fully-characterizable, crystalline products, in the case of Dy, crystals of [K(crypt)][CpMe3Dy] could be isolated.

Graphical abstract: Isolation of reactive Ln(ii) complexes with C5H4Me ligands (CpMe) using inverse sandwich countercations: synthesis and structure of [(18-crown-6)K(μ-CpMe)K(18-crown-6)][CpMe3LnII] (Ln = Tb, Ho)

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Publication details

The article was received on 27 Sep 2018, accepted on 13 Nov 2018 and first published on 14 Nov 2018


Article type: Paper
DOI: 10.1039/C8DT03890B
Citation: Dalton Trans., 2018,47, 17285-17290
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    Isolation of reactive Ln(II) complexes with C5H4Me ligands (CpMe) using inverse sandwich countercations: synthesis and structure of [(18-crown-6)K(μ-CpMe)K(18-crown-6)][CpMe3LnII] (Ln = Tb, Ho)

    D. N. Huh, J. W. Ziller and W. J. Evans, Dalton Trans., 2018, 47, 17285
    DOI: 10.1039/C8DT03890B

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