Recent Results

Below are some brief summaries of recent work undertaken by the NMR service for the various groups in the Department. There is also a poster , highlighting some of the recent work.

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More unusual organometallic complexes

In the laboratory of Dr J. Robin Fulton a number of novel compounds comprising main group metals and the β-diketiminate ligand been prepared recently. We have employed variable temperature 1H and 199Hg NMR understand the ligand binding modes and to compare solution structure with solid state X-ray crystallographic data.

  1. L. Ferro, M. P. Coles, I. J. Day and J. R. Fulton.
    Taking advantage of Hg-C bonds: synthesis of the first homoleptic bis-β-diketiminate complex bound through the γ-carbons Organometallics, In Press, 2010 [ DOI ]


Small molecule structure elucidation

In collaboration with Dr Clive Penkett we have been involved in determining the solution structure of a variety of novel small molecules. These compounds have been formed in only a small number of synthetic operations using photochemical methods which yield molecules with high degrees of structural complexity. Modern 2-dimensional NMR techniques have been applied alongside X-ray crystallography to determine the structures of these fenestrane structures.

  1. C. S. Penkett, J. Woolford, I. J. Day, and M. P. Coles.
    The double [3+2] photocycloaddition reaction. J. Am. Chem. Soc., 132(1):4-5, 2010 [ DOI ]


Unusual organometallic complexes

Dr Martyn Coles is interested in small organometallic complexes as polymerisation catalysts. We have recently investigated a novel ether-free dialkyl calcium (II) complex synthesised in the Coles group. This is a rare example of a calcium (II) complex which does not contain a coordinating solvent molecule. A series of detailed variable temperature measurements have demonstrated that the metallocycle is transiently open in toluene.

  1. M. P. Coles, S. E. Sozerli, J. D. Smith, P. B. Hitchcock, and I. J. Day.
    An ether-free, internally coordinated dialkylcalcium(II) complex. Organometallics, 28(5):1579-1581, 2009 [ DOI ]


Reactions of Organo-Uranium compounds with small molecules

Work in the group of Prof. Geoff Cloke FRS is concerned with organometallic uranium complexes and their reactions with small molecules such as CO, CO2 etc. We undertook some detailed NMR studies of the mechanisms of these reactions, particularly the formation of a ynediolate complex bridging two uranium centres.

  1. A. S. Frey, F. G. N. Cloke, P. B. Hitchcock, I. J. Day, J. C. Green, and G. Aitken.
    Mechanistic studies on the reductive cyclooligomerisation of CO by U(III) mixed sandwich complexes; the molecular structure of [(U(η-C8H6{SiiPr3-1,4}2)(η-Cp*)]2(μ-η1:η1-C2O2).
    J. Am. Chem. Soc., 130(42):13816-13817, 2008. [ DOI ]