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  • 1
    Electronic Resource
    Electronic Resource
    Fully Chlorinated N-Silyl Amides of Titanium and Tungsten  -  Crystal Structure of Cl3SiNW(Cl3)N(SiCl3)2 (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 701-704 
    Details
    ISSN: 0009-2940
    Keywords: N-Silyl amides ; Precursor ; 14N-NMR ; Titanium ; Tungsten ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of hexachlorodisilazanyllithium (Cl3Si)2NLi (1), with TiCl4 leads selectively to the novel fully chlorinated amides (Cl3Si)2NTiCl3 (2) or [(Cl3Si)2N]2 TiCl2 (3), respectively, depending on the molar ratio of the starting materials. The analogous reaction of 1 with WCl6 yielded the amide imide Cl3SiN=W(Cl3)N(SiCl3)2 (5) by elimination of SiCl4. The relative amounts of the starting materials had no effect on the formation of 5. 14/15N- and 29Si-NMR data on the starting materials and products show significantly different effects, when compared with those of analogous N-trimethylsilyl derivatives, due to the lower energy of the electrons in the N—Si and N—M ß bonds. The crystal structure of 5 (triclinic, space group P1) was determined by X-ray structure analysis.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971300605
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  • 2
    Electronic Resource
    Electronic Resource
    Multinuclear magnetic resonance study of N,N′,N″-tris(trimethylsilyl)borazine (1995)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 33 (1995), S. 557-560 
    Details
    ISSN: 0749-1581
    Keywords: NMR ; 14N NMR ; 11B NMR ; borazines ; coupling constants 1J(29Si14N),1J(14N11B) ; coupling signs ; 14N electric field gradient ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The nuclear spin relaxation rate of the quadrupolar 14N nuclei in N,N′,N″-tris(trimethylsilyl)borazine (1) is surprisingly slow [T1(14N)=0.1 s]. This allows one to measure 1J(29Si14N) (9.6 Hz) directly from the 29Si NMR spectra and also to compare signs of coupling constants 1J(29Si14N) (〈0) and 3J(14NSiC1H) (〉0) by 2D 29Si/1H HETCOR experiments. Since the transverse relaxation time T2(14N) in 1 is governed by scalar relaxation of the second kind, the magnitude of 1J(14N11B) can be evaluated (23 ± 0.5 Hz). 11B, 14N and 29Si NMR data for N,N′-bis(trimethylsilyl)borazine (2) were also obtained, and 11B and 14N NMR spectra of the parent borazine [HBNH]3 (3), and of [HBNMe]3 (4) were remeasured. Calculation of the tensor components of the 14N electric field gradient shows that eqzz in 1 and in 2 for 14N(Si) is significantly smaller than for other borazines [HBNR]3, e.g. with R=H (3) or Me (4), in agreement with the experimental results.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1260330711
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    Paper (German National Licenses)
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