NMR Spectra of 1-Vinylimidazole, Transformed by Paramagnetic Complexes

2018 ◽  
Vol 50 (4) ◽  
pp. 569-577
Author(s):  
Vladimir K. Voronov ◽  
Igor A. Ushakov ◽  
Evgenia A. Funtikova
1985 ◽  
Vol 40 (10) ◽  
pp. 1362-1370 ◽  
Author(s):  
Johann W. Buchler ◽  
Stefan Pfeifer

A series of novel alkyl or aryiimidovanadium(IV) 5,10,15,20-tetra(p-tolyl)porphyrinates, VNR(TTP) (4a-4g), is described. They are obtained from the vanadyl complex, VO(TTP) (2a) via the reactive intermediate VCl2(TTP) (3b) which undergoes aminolysis with the respective primary amines RNH2 (R = tBu, Ph, pTol, pClPh, pAnis, pBiph, ptBuPh)**. The formulae are proved by elemental analyses and mass spectra. The paramagnetic complexes are stable to water and may thus be purified by chromatography but are hydrolyzed to give 2 a on treatment with acetic acid. The UV/VIS and 1H NMR spectra of 4a-4g are of the same type as 2a, but the former are slightly hypsochromically shifted, and the latter do not show the proton resonances of the organylimide ligands due to the proximity of the paramagnetic metal center.


Polyhedron ◽  
1990 ◽  
Vol 9 (10) ◽  
pp. 1249-1256 ◽  
Author(s):  
Martin A. Fedotov ◽  
Boris Z. Pertsikov ◽  
David K. Danovich

2001 ◽  
Vol 05 (05) ◽  
pp. 442-448 ◽  
Author(s):  
M. J. CHEN ◽  
R. J. KLINGLER ◽  
J. W. RATHKE

The paramagnetic complexes ( FPc )( Me ) Rh - (4) and (FPc)( PMe 3)( Me ) Rh - (10) have been prepared by reducing ( FPc )( Me ) Rh (1) and ( FPc )( PMe 3)( Me ) Rh (2) with NaBH 4 in methanol-d4 [ FPc 2- = dianion of 1,4,8,11,15,18,22,25-octakis(trifluoromethyl)phthalocyanine]. Compounds 4 and 10 are further reduced by NaBH 4 to complexes, which are assigned to ( DFPc )( Me ) Rh - (5) and ( DFPc )( PMe 3)( Me ) Rh - (11), respectively. Based on the 1 H NMR spectra of these complexes, 4 and 10 are assigned to the Rh (III) complexes of the singly reduced radical anion FPc ·3-, while 5 and 11 are assigned to the Rh (III) complexes of the doubly reduced, antiaromatic anion DFPc 3-, which has the deuteron bonded to one of its meso nitrogens. As expected, the antiaromatic complexes 5 and 11 are not stable. At -40 °C, 5 was transformed successively into three aromatic compounds, the first of which was assigned to the ring-contracted α,β,γ-triazatetrabenzocorrole complex ( TBC )( Me ) Rh - [ TBC 3- = trianion of 3,6,10,13,17,20,24,27-octakis(trifluoromethyl)-α,β,γ-triazatetrabenzocorrole]. Cyclic voltammetry of 1 and 2 was also carried out. Two reversible one-electron reduction waves were observed for both 1 and 2.


1975 ◽  
Vol 30 (7-8) ◽  
pp. 649-650 ◽  
Author(s):  
Frank H. Köhler

1H CW NMR spectra of paramagnetic compounds are frequently disturbed by sidebands. This problem is circumvented by variation of the nuclear single sideband technique or by application of a variable sideband oscillator. Both methods are demonstrated by the 1H spectrum of Bis-(h5-ethylcyclopentadienyl)cobalt.


2005 ◽  
Vol 54 (6) ◽  
pp. 1473-1476
Author(s):  
V. K. Voronov ◽  
I. A. Ushakov ◽  
L. V. Baikalova

2001 ◽  
Vol 79 (10) ◽  
pp. 1477-1482 ◽  
Author(s):  
Craig Anderson

2-Methylimidazole (2-MeIm) reacts with RuCl3 in aqueous acidic ethanolic medium to give (2-MeImH)2[RuCl5(2-MeIm)] (1) and (2-MeImH)[RuCl4(2-MeIm)2] (2) (2-MeImH = protonated 2-methylimidazole), the ratio depending on reaction conditions used. Molecule 1 crystallizes in the space group Pnma: a = 14.046(2), b = 17.294(2), and c = 8.2778(12) Å. The 1H NMR spectra of these ruthenium(III) complexes have been measured and show peaks with large isotropic shifts and large line broadening characteristic of such paramagnetic complexes. The aquation of complexes 1 and 2 were followed by proton NMR spectroscopy. 1,2-Dimethyl imidazole (1,2-diMeIm) reacts with RuCl3 in methanolic solution to give [RuCl3(1,2-diMeIm)(H2O)S] (S=H2O (3a) or CH3OH (3b)). The aquation reactions of complexes 3a and 3b were followed by 1H NMR.Key words: ruthenium, paramagnetic, antitumour, NMR.


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