Symmetry-based 29Si dipolar recoupling magic angle spinning NMR spectroscopy: a new method for investigating three-dimensional structures of zeolite frameworks |
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Authors: | Brouwer Darren H Kristiansen Per Eugen Fyfe Colin A Levitt Malcolm H |
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Institution: | School of Chemistry, University of Southampton, Southampton, United Kingdom, SO17 1BJ. |
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Abstract: | A new 29Si solid-state MAS NMR experiment is described for investigating the framework structures of pure silica zeolites. The symmetry-based homonuclear dipolar recoupling sequence SR26411 has been incorporated into a two-dimensional NMR experiment to probe the Si-O-Si bonding connectivities and long-range Si-Si distances in zeolite frameworks. This dipolar recoupling sequence is shown to have a number of advantages over the J-coupling-based INADEQUATE experiment. For the clathrasil Sigma-2, it is demonstrated that there is excellent agreement between experimental double-quantum build-up curves obtained from a series of two-dimensional double-quantum correlation spectra and simulated curves which consider all Si-Si distances out to 8 A. This result suggests that this experiment could be used to solve zeolite frameworks with unknown structures. |
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