Darstellung, Reaktionen und 51V-NMR-spektroskopische Untersuchungen der Imidovanadium(V)-trichloride: RN=VCl3 (R = H, SiMe3, Alkyl)

Preuß, Fritz; Fischbeck, Uwe; Tabellion, Frank; Pemer, Jens; Frank, Walter; Reiß, Guido J.

doi:10.1515/znb-2001-0307

Cited by 6 publications

(7 citation statements)

References 6 publications

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“…The two shift ranges are well separated from each other and from those of nitrido and tertiary amine ligands to allow unambiguous identification of the different types of nitrogen ligands in a complex from 14 …”

Section: Discussionmentioning

confidence: 99%

“…The value of 2 J( 51 V, 31 P) (30.3 š 1 Hz) in the cyclic imidovanadium complex 23 (Fig. 4), which is a key intermediate during the catalytic trimerization of phosphaalkynes, 6 could be determined from lineshape analysis of a 31 Pf 1 H, 14 Ng spectrum and is nearly an order of magnitude smaller than the 1 J(P,V) coupling in 6 and 7.…”

Section: Coupling Constants Tomentioning

confidence: 99%

“…Experimental conditions: 64 experiments of 120 scans and 256 data points were collected (7 min of instrument time); spectral width 2450 Hz in F 2 and 2500 Hz in F 1 ; dephasing delay (INEPT) 0.9 ms, relaxation delay 2 ms, acquisition time 52 ms, zero-filling to 512W in F 2 and 128W in F 1 , shifted sine-square multiplication in both dimensions. The spectrum is displayed in magnitude mode; the projections constitute one-dimensional 31 Pf 1 H, 14 Ng and 51 V NMR spectra of 23.…”

Section: Prospect Of 31 P 51 V Correlation Spectroscopymentioning

confidence: 99%

“…Anticipating that nitrogen NMR spectroscopy should be better suited for this task, 7,8 we set out to perform a systematic study of nitrogen NMR spectra of a series of mono-and dinuclear vanadium complexes containing different types of nitrogen ligands. Although 15 N NMR frequently affords greater structural information, we chose to observe 14 N NMR spectra, considering that the observation of 15 3 respectively. The simultaneous occurrence of highly abundant 51 V and 31 P isotopes in one molecule stimulated further the investigation of the prospect of heteronuclear 31 P, 51 V correlation spectroscopy, and some comments concerning the application of this technique will also be given.…”

Section: Introductionmentioning

confidence: 99%

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Multinuclear magnetic resonance study of some imidovanadium complexes

Gudat

Fischbeck

Tabellion

et al. 2001

Magnetic Reson in Chemistry

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Section: Discussionmentioning

confidence: 99%

Section: Coupling Constants Tomentioning

confidence: 99%

Section: Prospect Of 31 P 51 V Correlation Spectroscopymentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 2 more Smart Citations

Multinuclear magnetic resonance study of some imidovanadium complexes

Gudat

Fischbeck

Tabellion

et al. 2001

Magnetic Reson in Chemistry

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“…M elting points are uncorrected (heating rate 2°/m in). N [23], 4b [24], 4d,e [25,26], 5a,b [27,28], 21a [29], 21b [30] and 15a [31] w ere p rep ared by p u b lished m ethods.…”

Section: Methodsmentioning

confidence: 99%

Organophosphorus Compounds, Part 146* Imidovanadium(V) Complexes as Reaction Partners for Kinetically Stabilized Phosphaalkynes. Synthesis and Reactivity of 3-Aza-l,2,4,6-tetraphospha-quadricyclanes

Peters

Tabellion

Nachbauer

et al. 2001

Zeitschrift Für Naturforschung B

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The Lewis base adducts of imidovanadium(V) compounds 5a,b undergo chemoselective cyclooligomerization reactions with the kinetically stabilized phosphaalkynes 4a-e to furnish the azatetraphosphaquadricyclanes 6a-f with incorporation of the imido fragment. The reac tivity of this novel class of heteropolycyclic compounds has been examined exemplarily for compound 6a. Complexation of one and two phosphorus atoms was achieved by reaction with nonacarbonyldiiron or the tungsten pentacarbonyl-THF complex resulting in the forma tion of the transition metal compounds 17-20. Reactions of 6a with the sulfonyl azides 21ac furnished the Staudinger products 22a-c. The reaction of 6a with two equivalents of tosyl azide gave a surprising result. No double complexation leading to a symmetrical product was achieved, and compound 23 was obtained instead in which the two phosphorus atoms of one diphosphirane ring are functionalized. Oxidative cleavage of a P/P bond in 6a to furnish product 24 is observed in the reaction of 6a with the Lewis base-free imidovanadium(V) species 15a. Intro d u ctio nCage com pounds, som e of which have highly sym m etrical skeletons, have always been of great in terest to chemists. T heir often tedious, m ulti stage syntheses have p resented a challenge to ex p erim ental tech n iq u es and the unusual bonding relationships have gen erated new im pulses for theoretical considerations.Thus, it is n o t surprising that th e construction of phosphoru s-carb o n cage com pounds has devel oped into an im p o rta n t field in th e chem istry of kinetically stabilized phosphaalkynes. In contrast to their all-carbon analogues, how ever, access to the phosp h o ru s-carb o n cage system s has only b e com e possible in th e past ten years w ith the ph o s phaalkynes being indispensable starting com pounds. * Part 145: S. G. Ruf, U. Bergsträsser, M. Regitz, Eur. J. Org. Chem. 2000, 2219. M ajor b reakthroughs in this developm ent in clude the syntheses of the tetrap h o sp h acu b an e 1 [1 ], the tetrap hosphabishom oprism ane 2 [2 ], and the h ex aphosphapentaprism ane 3 [3] (Schem e 1).The cubane 1 was of p articular in terest on account of its high sym m etry and its at first inexplicable spectral properties. A ccordingly, the rem arkably stable cubane 1 has, on th e one hand, b een the subject of num erous th eo retical bonding studies [4 -6 ] and, on the o th er hand, the starting point for m any functionalization reactions at the ph o s phorus atom s [7 -9 ]. A lthough the first syntheses of the phosphaalkyne te tra m ers 1 and 2 w ere based on the therm olysis of the fe/t-butylphosphaalkyne 4a, m any novel synthetic strategies have since been developed for the specific con struction of polycyclic phosphorus-carbon systems. These now provide selective and high-yield access to the cage com pounds 1 and 2. The synthetic p rin ciples em ployed include transition m etal-(-> 1 [10,11]), base-(-»• 2 [12]), and Lewis acid-m ediated processes (-* ■ 3 [3]).

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Tetrabutylammonium Salts of Aluminum(III) and Gallium(III) Phthalocyanine Radical Anions Bonded with Fluoren‐9‐olato⁻ Anions and Indium(III) Phthalocyanine Bromide Radical Anions

Konarev

Khasanov

Ishikawa

et al. 2017

Chemistry An Asian Journal

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Reduction of aluminum(III), gallium(III), and indium(III) phthalocyanine chlorides by sodium fluorenone ketyl in the presence of tetrabutylammonium cations yielded crystalline salts of the type (Bu N ) [M (HFl-O )(Pc )] (Br )⋅1.5 C H Cl [M=Al (1), Ga (2); HFl-O =fluoren-9-olato anion; Pc=phthalocyanine] and (Bu N ) [In Br(Pc )] ⋅0.875 C H Cl ⋅0.125 C H (3). The salts were found to contain Pc radical anions with negatively charged phthalocyanine macrocycles, as evidenced by the presence of intense bands of Pc in the near-IR region and a noticeable blueshift in both the Q and Soret bands of phthalocyanine. The metal(III) atoms coordinate HFl-O anions in 1 and 2 with short Al-O and Ga-O bond lengths of 1.749(2) and 1.836(6) Å, respectively. The C-O bonds [1.402(3) and 1.391(11) Å in 1 and 2, respectively] in the HFl-O anions are longer than the same bond in the fluorenone ketyl (1.27-1.31 Å). Salts 1-3 show effective magnetic moments of 1.72, 1.66, and 1.79 μ at 300 K, respectively, owing to the presence of unpaired S=1/2 spins on Pc . These spins are coupled antiferromagnetically with Weiss temperatures of -22, -14, and -30 K for 1-3, respectively. Coupling can occur in the corrugated two-dimensional phthalocyanine layers of 1 and 2 with an exchange interaction of J/k =-0.9 and -1.1 K, respectively, and in the π-stacking {[In Br(Pc )] } dimers of 3 with an exchange interaction of J/k =-10.8 K. The salts show intense electron paramagnetic resonance (EPR) signals attributed to Pc . It was found that increasing the size of the central metal atom strongly broadened these EPR signals.

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Darstellung, Reaktionen und ⁵¹V-NMR-spektroskopische Untersuchungen der Imidovanadium(V)-trichloride: RN=VCl₃ (R = H, SiMe₃, Alkyl)

Cited by 6 publications

References 6 publications

Multinuclear magnetic resonance study of some imidovanadium complexes

Multinuclear magnetic resonance study of some imidovanadium complexes

Organophosphorus Compounds, Part 146* Imidovanadium(V) Complexes as Reaction Partners for Kinetically Stabilized Phosphaalkynes. Synthesis and Reactivity of 3-Aza-l,2,4,6-tetraphospha-quadricyclanes

Tetrabutylammonium Salts of Aluminum(III) and Gallium(III) Phthalocyanine Radical Anions Bonded with Fluoren‐9‐olato⁻ Anions and Indium(III) Phthalocyanine Bromide Radical Anions

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Darstellung, Reaktionen und 51V-NMR-spektroskopische Untersuchungen der Imidovanadium(V)-trichloride: RN=VCl3 (R = H, SiMe3, Alkyl)

Cited by 6 publications

References 6 publications

Multinuclear magnetic resonance study of some imidovanadium complexes

Multinuclear magnetic resonance study of some imidovanadium complexes

Organophosphorus Compounds, Part 146* Imidovanadium(V) Complexes as Reaction Partners for Kinetically Stabilized Phosphaalkynes. Synthesis and Reactivity of 3-Aza-l,2,4,6-tetraphospha-quadricyclanes

Tetrabutylammonium Salts of Aluminum(III) and Gallium(III) Phthalocyanine Radical Anions Bonded with Fluoren‐9‐olato− Anions and Indium(III) Phthalocyanine Bromide Radical Anions

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Darstellung, Reaktionen und ⁵¹V-NMR-spektroskopische Untersuchungen der Imidovanadium(V)-trichloride: RN=VCl₃ (R = H, SiMe₃, Alkyl)

Tetrabutylammonium Salts of Aluminum(III) and Gallium(III) Phthalocyanine Radical Anions Bonded with Fluoren‐9‐olato⁻ Anions and Indium(III) Phthalocyanine Bromide Radical Anions