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  • Author: Gabriele Hornung x
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The reaction of [tBuN=VCp(PMe3)2] (1) with S8, Se, Te or I2 have been studied. Via this pathway dinuclear diamagnetic tert-butylimidovanadium(IV) complexes are formed: [(μ-E)(μ- NtBu)2V2Cp2] (E=S, Se, Te), [(μ-η1−E2)(μ-NtBu)2V2Cp2] {E=Se (3), Te}, [(μ-NtBu)2V2Cp2I2]. In addition the vanadium(V) complexes [tBuN=VCp (S5)] (9a) and tBuN=VCpI2 could be isolated. The synthesis of tBuN=VCpF2 is also described. All compounds obtained have been characterized by spectroscopic methods (MS; 1H, 13C, 51V NMR), 3 and 9b by single crystal X-ray diffraction analysis.

The imidovanadium(III) complexes [tBuN=VCp(PR3)2], [tBuN=VCp{P(OR)3}2] and [tBuN= VCp(CO)2] have been prepared starting from tBuN=VCpCl2 by reductive dehalogenation with magnesium. The reaction of [tBuN=VCp(PMe3)2] (2a) with carbon monoxide, alkynes, alkenes, tert-butylphosphaalkyne, nitriles, ketones and carbon disulfide furnished the complexes [tBuN=VCp(PMe3) (L)], while the vanadium(V) compound tBuN=VCp(O2C2Ph2) is formed with benzil. All vanadium(III) complexes obtained are diamagnetic (d2, low-spin configuration) and have been characterized by spectroscopic methods (MS; 1H, 13C, 31P, 51V NMR).

N,N′-Bis(trimethylsilyl)benzamidinato complexes of vanadium(V), niobium(V) and tantalum( V) have been prepared starting from tBuN=MCl3 · n py and tBuN=MCpCl2, respectively: tBuN=V[PhC(NSiMe3)2] nCl3-n (n = 1, 2); tBuN=M[RC(NSiMe3)2]Cl · py [M = Nb. Ta; R = C6H5, C6H4(4-CF3)]; tBuN=MCp[RC(NSiMe3)2]Cl [M = V. Nb, Ta; R = C6H5, C6H4- (4-CF3)]; tBuN=VCp[PhC(NSiMe3)2](OtBu). The syntheses of silylated tert-butylamido complexes tBuN=M[NtBu-SiMe2-NHtBu]Cl2 · py (M = Nb, Ta), tBuN=V[NtBu-SiMe2-OtBu]Cl2 and tBuN=M[NtBu-SiMe2-OtBu]Cl2 · py [M = Nb, Ta (20)] are also described. The compounds have been investigated by 1H NMR data,51V NMR data, mass spectra. X-ray data diffraction analysis.