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DOI: 10.1039/A806791K (Paper) Reference Section for: J. Chem. Soc., Dalton Trans., 1999, 229-236

Kinetically inert cryptate systems: solid state and solution NMR studies[hair space]†

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David C. Apperley, William Clegg, Simon Coles, Joanne L. Coyle, Noreen Martin, Beatrice Maubert, Vickie McKee and Jane Nelson

Abstract

Mononuclear cryptates of Pb2+, Cd2+ and Hg2+ with the small host 1,4,7,10,13,16,21,24-octaazabicyclo[8.8.8]hexacosa-4,6,13,15,21,23-hexaene (imBT) showed satellite peaks in 1H NMR solution spectra throughout the accessible (–40 to +70 °C) fluid range of solvents used indicating kinetic inertness toward decomplexation. Solid-state MAS NMR studies were made on these cryptates and on dinuclear silver(I) and copper(I) analogues, in the latter case establishing coupling of 63,65Cu to 15N. A crystal structure determination of the mercury cryptate showed a symmetrical six-co-ordinate site for Hg2+ with all imino nitrogens co-ordinated, consistent with the observation, for the isomorphous cadmium(II) complex, of a 13-line 113Cd resonance in the CP MAS NMR spectrum.

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