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  • 1
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 33 (1995), S. 493-496 
    ISSN: 0749-1581
    Keywords: selenium-, silicon- and boron-containing heterocycles ; tricarbonyl(n4-heterodiene) ; tricarbonylmetal ; complexes; 2D NMR; z-filtering; Ψ-BIRD HMQC; ; determination of coupling signs ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The signs of coupling constants [1J(77Se29Si) 〉 0, 2J(77Se13CSiMe) 〉 0,3J(77Se1HSiMe) 〉 0] were determined for pentaorgano-substituted 2,5-dihydro-1,2,5-selenasilaboroles [R3 = Me, la; R3 = C(Me)=CH2, 1b], and also for derivatives in which the surroundings of the selenium atom were changed by forming a pyridine-borane adduct (2), by formation of an Se—AlCl3 adduct (3) and by π-complexation with the transition metal fragments [Fe(CO)3] (4) and [Ru(CO)3] (5). The sign determination was achieved by using various types of 2D heteronuclear shift correlations (HETCOR) with 13C, 29Si or 1H detection (HMQC). Some of these experiments had to be modified by z-filtering or by a Ψ-BIRD pulse sequence. The change in the magnitude of 1J(13C=13C) (la, 58.9 Hz; 4, 33.8 Hz) as a result of π-complexation follows the trend known for diene complexes.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 30 (1992), S. 393-397 
    ISSN: 0749-1581
    Keywords: Boron-nitrogen compounds ; 15N NMR ; Two-dimensional inverse 1H{15N} experiments ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Two types of proton-detected 1H—15N correlation experiments were compared with respect to the observation of 15N NMR resonances broadened by scalar relaxation of the second kind. Both single- and multiple-quantum experiments gave equal 15N line widths in F1, and in all cases the inverse experiments provided a dramatic increase in sensitivity and spectrometer time-saving compared with the direct observation of 15N resonances. Various aminoboranes [B(NHMe)3; B(NHNMe2)3; 2,3-dihydro-2-methyl-2-boraperimidine; organo-substituted 2,5-dihydro-1,2,5-azasilaboroles; organo-substituted 7,8-benzo-1-oxa-6-aza-2-sila-5-bora-3-cyclooctene], organo-substituted 2,5-dihydro-1,2,5-azasilaboratolates, an amine-borane adduct (organo-substituted 7,8-benzo-6-oxa-1-aza-2-sila-5-borabicyclo[3.3.0]oct-3-ene), and (ligand)transition metal π-complexes of organo-substituted 2,5-dihydro-1,2,5-azasilaboroles were studied by two-dimensional inverse 1H{15N} NMR experiments. The straightforward application to the analysis of several mixtures suggests that this technique is promising for the investigation of oligomerization and polymerization of boron - nitrogen compounds.
    Additional Material: 3 Ill.
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  • 3
    ISSN: 0749-1581
    Keywords: heterocycles ; NMR ; 15N NMR ; 29Si NMR ; Hahn-echo extended INEPT ; ψ-BIRD-HSQC and -HMQC ; 1J(29Si 15N) ; relative signs ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 15N and 29Si NMR data of 2,5-hydro-1,2,5-azasilaborole derivatives and related compounds were determined with emphasis on coupling constants 1J(29Si 15N) which cannot be measured from 15N NMR spectra of most boron-nitrogen compounds. In the case of compounds with an Si—N—H fragment ψ-Bird pulse sequences, combined with HMQC or HSQC, served for 1H detection of the 29Si resonance with preselection of the 15N-1H spin pair. This permitted the measurement of 1J(29Si 15N) and the determination of its absolute sign (〉0). In the absence of an NH group, the coupling constants 1J(29Si 15N) were measured from the 15N satellites in 29Si NMR spectra recorded by using the Hahn-echo extended (HEED) refocused INEPT pulse sequence. Isotope induced chemical shifts 1Δ 15/14N(29Si) were also measured by this technique for all the compounds. The 1J(29Si 15N) values cover the range 8.4-17.0 Hz, depending on the substituents at boron, silicon and nitrogen and on the complexation of the heterocycle.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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