Klaus Eichele Publication Abstracts 2001

 

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[UP]	D. L. Bryce, G. M. Bernard, M. Gee, M. D. Lumsden, K. Eichele, R. E. Wasylishen: Practical Aspects of Modern Routine Solid-State Multinuclear Magnetic Resonance Spectroscopy: One-Dimensional Experiments. Can. J. Anal. Sci. Spectrosc. 2001, 46, 46-82.

For a "reprint", see this page!

New solid-state NMR (SSNMR) methods and applications continue to blossom such that a diverse array of physical, chemical, and biological problems are now being addressed using a variety of SSNMR experiments. While SSNMR is far from routine for chemists in the manner that a technique such as solution NMR is, there are nevertheless numerous applications of SSNMR which would be beneficial to many "non-specialists" e.g., synthetic chemists seeking to characterize their materials. This article gathers together practical details for those one-dimensional experiments which, in a broad sense, are considered "routine" in a modern SSNMR laboratory. Emphasis is placed on providing information and over 300 key references in a manner which will be useful for the novice and the non-specialist. For practising SSNMR spectroscopists, it is hoped that this article will serve as a valuable reference in the laboratory. In addition to providing a brief review of pulsed Fourier transform NMR, the article discusses experimental details relating to the study of solid samples containing spin-1/2 nuclei, non-integer quadrupolar nuclei, and deuterium.

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[UP]	B. Thomas, S. Paasch, S. Steuernagel, K. Eichele: Residual 31P, 35,37Cl Dipolar Coupling in 31P MAS Spectra of Chlorocyclophosphazenes. Solid State Nucl. Magn. Reson. 2001, 20, 108-117. DOI 10.1006/snmr.2001.0034

In ³¹P MAS NMR spectra of chlorocyclophosphazenes, characteristic splittings have been observed for PCl or PCl₂ groups. At different applied magnetic fields, the fine structure and total width of the patterns change in a characteristic way, demonstrating that the splittings are due to indirect spin-spin and residual dipolar interactions with the chlorine nuclei directly bonded to phosphorus. For trans- nongeminal N₃P₃Cl₃(NMe₂)₃ and N₃P₃Cl₆ as examples, the spectra have been analyzed to obtain information on chlorine nuclear quadrupole coupling constants and ^35,37Cl, ³¹P indirect spin-spin coupling constants. Neglect of these interactions may result in misinterpretations of the multiplicity in ³¹P MAS spectra of chlorophosphazenes.

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[UP]	N. Kuhn, K. Eichele, M. Walker: Synthesis and Structure of 1,3-Diisopropyl-4,5-dimethylimidazolium-2-sulfonate: A Carbene Adduct of Sulfur Trioxide. Z. Anorg. Allg. Chem. 2001, 627, 2565-2567. DOI 10.1002/1521-3749(200112)627:12<2565::AID-ZAAC2565>3.0.CO;2-I

The stable betaine 1,3-diisopropyl-4,5-dimethylimidazolium-2-sulfonate (5) is obtained through hydrolysis of the 2-chloro-1,3-diisopropyl-4,5-dimethylimidazolium chloro-sulfite salt (4 b) in the presence of cyanide. The crystal structure analysis of 5 is reported.