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  • Analytical Chemistry and Spectroscopy  (2)
  • 1
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 27 (1989), S. 44-49 
    ISSN: 0749-1581
    Keywords: γ-Butyrolactone ; 1H NMR analysis ; Conformational analysis ; Molecular mechanics ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The 60 and 100 MHz 1H NMR spectra of γ-butyrolactone were analysed in detail. The best set of coupling values (Hz ± 0.03) is 3JABc = 7.86, 3JABt = 6.27, 3JBCc = 9.52, 3JBCt = 6.86, 4JACc + 4JACt = -0.18, 2JA - 2JB = 3.89 and 2JB - 2JC = 4.86 (A, B and C refer to α, β and γ protons, with respect to the ring oxygen, and c and t mean the same and opposite side of the ring, respectively). The 3J values support the conclusion that the molecule is interconverting between two equivalent conformations of near envelope type with the β-carbon out of the mean plane defined by the fragment C—O—CO—C.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 0749-1581
    Keywords: 2D NMR ; Spin-spin coupling ; Coordination-induced shift ; 1H—13C ; HETCOR ; ortho-Metalation ; Cyclometallation ; Polypyridyl ; 2,2′-Bipyridine ; π-Back-bonding ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Complete 1H and 13C NMR assignments and coordination-induced shift [CIS, δ(complex) - δ(free ligand)] calculations for carbon σ-bonded ortho-metalated rhodium(III) and iridium(III) complexes are described. NMR parameters are used as probes of van der Waals interactions and ring current anisotropy in the ligand's environmental framework and to monitor σ-donation and π-back-bonding within the ligand in this family of ortho-metalated complexes. CIS measurements indicate large charge redistribution within the ligands as a result of ortho-metalation to the rhodium(III) or iridium(III) cationic metal centers. The pulse sequences, attached proton test (APT), 1H—1H homonuclear correlation spectroscopy (COSY), single-frequency off-resonance decoupling (SFORD) and 1H—13C heteronuclear correlation spectroscopy (HETCOR), were utilized to assign all proton and carbon resonances of [Rh(ppy)2Cl]2, [Ir(ppy)2Cl]2, [Ir(ptpy)2Cl]2, [Ir(mppy)2Cl]2, [Rh(ppy)2bpy]+, [Ir(ppy)2bpy]+, [Ir(ptpy)2bpy]+ and [Ir(mppy)2bpy]+, where ppy is 2-phenylpyridine, ptpy is 2-(p-tolyl)pyridine, mppy is 3-methyl-2-phenylpyridine and bpy is 2,2′-bipyridine.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
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