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Issue 37, 2009
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Synthesis and solid-state characterization of platinum complexes with hexadentate amino- and iminophosphine ligands

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Abstract

Hexadentate ligands cis,cis-C6H9(N[double bond, length as m-dash]CHC6H4(PPh2))3 (1) and cis,cis-C6H9(NHCH2C6H4(PPh2))3 (2) were synthesized starting from cis,cis-1,3,5-triaminocyclohexane, and characterized using NMR spectroscopy and single-crystal X-ray diffraction. These ligands can bind both Pt(0) and Pt(II) metal centers using either or both of the soft phosphine moieties and the hard amine/imine moieties. In many cases the resulting complexes are negligibly soluble; hence, 31P and 195Pt solid-state NMR (SSNMR) spectroscopy was applied to analyse the bonding modes of the hexadentate ligands. The 195Pt SSNMR spectroscopy of these complexes is particularly challenging, since 1H–195Pt cross polarization is extremely inefficient, the 195Pt longitudinal relaxation times are extremely long and the 195Pt powder patterns are expected to be quite broad due to platinum chemical shift anisotropy. It is demonstrated that the ultra-wideline 195Pt SSNMR spectra can be efficiently acquired with a combination of frequency-stepped piecewise acquisitions and cross-polarization/Carr–Purcell Meiboom–Gill (CP/CPMG) NMR experiments. The 195Pt and 31P SSNMR data are correlated to important structural features in both Pt(0) and Pt(II) species.

Graphical abstract: Synthesis and solid-state characterization of platinum complexes with hexadentate amino- and iminophosphine ligands

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Publication details

The article was received on 17 Apr 2009, accepted on 29 Jun 2009 and first published on 29 Jul 2009


Article type: Paper
DOI: 10.1039/B907737E
Citation: Dalton Trans., 2009,0, 7701-7716
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    Synthesis and solid-state characterization of platinum complexes with hexadentate amino- and iminophosphine ligands

    M. Thibault, B. E.G. Lucier, R. W. Schurko and F. Fontaine, Dalton Trans., 2009, 0, 7701
    DOI: 10.1039/B907737E

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