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    Structural Variations in the Complete Series of Lanthanoid Complexes of a Calix[4]arene Trisamide

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    Access Status
    Open access
    Authors
    Nealon, G.
    McIldowie, M.
    Skelton, B.
    Mocerino, Mauro
    Massi, Massimiliano
    Ogden, Mark
    Date
    2017
    Type
    Journal Article
    
    Metadata
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    Citation
    Nealon, G. and McIldowie, M. and Skelton, B. and Mocerino, M. and Massi, M. and Ogden, M. 2017. Structural Variations in the Complete Series of Lanthanoid Complexes of a Calix[4]arene Trisamide. Australian Journal of Chemistry.
    Source Title
    Australian Journal of Chemistry
    DOI
    10.1071/CH17484
    ISSN
    0004-9425
    School
    School of Molecular and Life Sciences (MLS)
    URI
    http://hdl.handle.net/20.500.11937/69510
    Collection
    • Curtin Research Publications
    Abstract

    Lanthanoid picrate (pic) complexes of 5,11,17,23-tetra-tert-butyl-25-hydroxy-26,27,28-tris(diethylcarbamoylmethoxy)calix[4]arene (LH) have been synthesised and structurally characterised, to complete this series for all lanthanoids (other than promethium). From cerium to lutetium, three structural types are observed: Type I, [Ln(L)(O,O'-pic)](pic), Ln = Ce-Dy; Type II, [Ln(L)(O-pic)](pic), Ln = Tb, Ho; Type III, [Ln(L)(HOEt)](pic)2, Ln = Er-Lu. With lanthanum, three different ten-coordinate complexes were characterised; [Ln(L)(O,O'-pic)(HOEt)](pic), [Ln(L)(O,O'-pic)(OH2)](pic), and [Ln(L)(O,O'-pic)(HOMe)](pic). The crystallisation of Type I and II observed for terbium shows that the stability of the different structures are sensitively poised at the transition points. Nevertheless, the structures show that the vacant space in the coordination sphere left by the trisamide L tends to reduce across the series as expected. It is occupied by a bidentate picrate anion and unidentate solvent molecule with lanthanum, a bidentate picrate anion for cerium to dysprosium (Type I), a unidentate picrate anion for terbium and holmium (Type II), and finally a unidentate solvent molecule from erbium to lutetium (Type III). The coordination number thus reduces from 10 to 8 across the series.

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