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  • 1
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 31 (1993), S. 380-387 
    ISSN: 0749-1581
    Keywords: Solid state Mercury-199 Off-magic angle spinning Mercury(II) acetate Mercury lactate Mercury citrate Mercury salicylate ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The effects of small deviations from the magic angle on 199Hg solid-state NMR spectra with large chemical shift anisotropy are shown by computation and illustrated with spectra of mercury(II) acetate. These are shown to give the false appearance of multiple species, and place great importance on very precise angle setting (much better than ± 0.1°) for heavy atom solid-state NMR. Chemical shift tensor principal components have been derived from spinning sideband analysis, and the difficulties of this are discussed; revised values for the anisotropy and asymmetry of mercury(II) acetate are -1732 ppm and 0.08, respectively. 199Hg spectra are also given for mercury(II) lactate and citrate.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
    Library Location Call Number Volume/Issue/Year Availability
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  • 2
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 31 (1993), S. 1064-1071 
    ISSN: 0749-1581
    Keywords: NMR ; 205Tl ; Solid state ; Zeolites A. X and Y ; Thallium ; Frequency-stepped spin-echo integral method (FUSSI) ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Thallium-205 NMR is reported for several zeolite samples (A, X and Y; hydrated and dehydrated) with thallium(I) exchanged for sodium. Detection at high field (7.05 T) clarifies the spectrum appearance, and it is seen that chemical shift anisotropy (CSA) dominates some of the band shapes. The large CSAs dictate that the spectrum is recorded piecewise by a frequency-stepped spin-echo integral (FUSSI) method. Magic-angle sample spinning has been observed to give only a very minor line-narrowing effect. Threefold-coordinated zeolite A Tl+ sites adjacent to six-membered rings [Tl(1) and Tl(3)] are both assigned to a resonance which has large CSA (δiso 1183, δδ - 1842), while the remaining zeolite A site [Tl(2)] gives an isotropic line shape (δiso 300). Dehydrated zeolite X gives an isotropic peak (δiso 854) which is assigned to the double six-ring Tl(I), and a broader anisotropic resonance which is tentatively attributed to supercage Tl(III). Data for dehydrated zeolite Y indicate that this has a disordered cation distribution.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    Library Location Call Number Volume/Issue/Year Availability
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