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  • 1
    ISSN: 0749-1581
    Keywords: 2D NMR ; Proton zero quantum coherence ; Heteronuclear chemical shift correlation ; Long-range heteronuclear multiple quantum coherence ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Assignment of the congested proton and carbon NMR spectra of heterocyclic benzo[b]triphenyleno[1,2-d]thiophene was accomplished through the concerted application of several two-dimensional NMR experiments. The inherent insensitivity of homonuclear zero quantum coherence to magnetic field inhomogeneity was used to advantage in disentangling the heavily overlapped proton NMR spectrum. Direct heteronuclear pairings were established using heteronuclear correlation with broad band homonuclear vicinal proton decoupling. Limited sample availability and solubility precluded complete establishment of long-range heteronuclear correlations by conventional means. Proton-detected long-range heteronuclear multiple quantum coherence did, however, provide sufficient long-range heteronuclear correlations to complete the assignment.A comparison of the data obtained from COSY and zero quantum experiments is presented; the ability of each to establish proton connectivities is discussed. Sensitivity limitations inherent in the conventional long-range optimized heteronuclear chemical shift correlation experiment are contrasted with the advantages of the proton-detected long-range heteronuclear multiple quantum correlation experiment. Practical limitations of the latter are considered.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 0749-1581
    Keywords: 2D NMR ; Heteronuclear chemical shift correlation ; Heteronuclear relayed coherence transfer ; Proton-detected long-range heteronuclear multiple quantum coherence ; HMBC ; Low-pass J-filtration ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The 1H and 13C NMR spectra of phenanthro[9,10-b]thiophene were totally assigned using a combination of twodimensional NMR techniques. Direct hetcronuclear correlations were established using heteronuclear chemical shift correlation with semi-selective proton decoupling. Two methods were employed to establish the identity of vicinal neighboring protons: heteronuclear relayed coherence transfer and low-pass J-filtered heteronuclear relayed coherence transfer. The versatilities of the two techniques were compared. Quaternary carbon resonance assignments and the orientations of individual spin systems relative to one another were accomplished using the proton-detected long-range heteronuclear multiple quantum coherence experiment (HMBC). Key long-range inter-ring proton homonuclear spin couplings served to confirm the orientations of the proton spin systems.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    Library Location Call Number Volume/Issue/Year Availability
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