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Design and Synthesis of “Dumb-bell” and “Triangular” Inorganic–Organic Hybrid Nanopolyoxometalate Clusters and Their Characterisation through ESI-MS Analyses

Authors

  • Dr. Chullikkattil P. Pradeep,

    1. WestCHEM, Department of Chemistry, The University of Glasgow, G12 8QQ (UK), Fax: (+44) 141-330-4888
    2. Present Address: School of Basic Sciences, Indian Institute of Technology—Mandi, Mandi 175 001, Himachal Pradesh (India)
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  • Dr. Feng-Yan Li,

    1. WestCHEM, Department of Chemistry, The University of Glasgow, G12 8QQ (UK), Fax: (+44) 141-330-4888
    2. Key Laboratory of Polyoxometalate Science of Ministry of Education, Department of Chemistry, Northeast Normal University, Changchun, Jilin (P. R. China)
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  • Claire Lydon,

    1. WestCHEM, Department of Chemistry, The University of Glasgow, G12 8QQ (UK), Fax: (+44) 141-330-4888
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  • Dr. Haralampos N. Miras,

    1. WestCHEM, Department of Chemistry, The University of Glasgow, G12 8QQ (UK), Fax: (+44) 141-330-4888
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  • Dr. De-Liang Long,

    1. WestCHEM, Department of Chemistry, The University of Glasgow, G12 8QQ (UK), Fax: (+44) 141-330-4888
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  • Prof. Dr. Lin Xu,

    1. Key Laboratory of Polyoxometalate Science of Ministry of Education, Department of Chemistry, Northeast Normal University, Changchun, Jilin (P. R. China)
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  • Prof. Dr. Leroy Cronin

    Corresponding author
    1. WestCHEM, Department of Chemistry, The University of Glasgow, G12 8QQ (UK), Fax: (+44) 141-330-4888
    • WestCHEM, Department of Chemistry, The University of Glasgow, G12 8QQ (UK), Fax: (+44) 141-330-4888
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Abstract

A series of tris(hydroxymethyl)aminomethane (TRIS)-based linear (bis(TRIS)) and triangular (tris(TRIS)) ligands has been synthesised and were covalently attached to the Wells–Dawson type cluster [P2V3W15O62]9− to generate a series of nanometer-sized inorganic–organic hybrid polyoxometalate clusters. These huge hybrids, with a molecular mass similar to that of small proteins in the range of ≈10–16 kDa, were unambiguously characterised by using high-resolution ESI-MS. The ESI-MS spectra of these compounds revealed, in negative ion mode, a characteristic pattern showing distinct groups of peaks corresponding to different anionic charge states ranging from 3 to 8 for the hybrids. Each peak in these individual groups could be unambiguously assigned to the corresponding hybrid cluster anion with varying combinations of tetrabutylammonium (TBA) and other cations. This study therefore highlights the prowess of the high-resolution ESI-MS for the unambiguous characterisation of large, nanoscale, inorganic–organic hybrid clusters that have huge mass, of the order of 10–16 kDa. Also, the designed synthesis of these compounds points to the fact that we were able to achieve a great deal of structural pre-design in the synthesis of these inorganic–organic hybrid polyoxometalates (POMs) by means of a ligand design route, which is often not possible in traditional “one-pot” POM synthesis.

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