Gold(I)-triphenylphosphine-arylazoimidazole: Synthesis and spectral (H,C, COSY,HMQC NMR) characterization |
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Authors: | P Byabartta M Laguna |
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Institution: | (1) Departmento de Quimica Inorganica-Instituto de Ciencia de Materiales de Aragon, Universidad de Zaragoza-CSIC, Zaragoza, 50009, Spain |
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Abstract: | The reaction of Au(OSO2CF3)(PPh3)] with arylazoimidazole in dichloromethane followed by NH4PF6 leads to Au(RAaiR′)(PPh3)]PF6 (RAaiR′ = p-R-N=N-C3H2-NN-1-R′), abbreviated as N,N′/-chelator, where N (imidazole) and N (azo) represent N and N′, respectively; R = H (a), Me
(b), Cl (c), and R′ = Me (I), CH2CH3 (II), CH2Ph (III)]. IR spectra of the complexes show -C=H- and -N=N-stretchings at 1590 and 1370 and at 1100, 755, 695, 545, and 505
cm−1 due to the presence of the triphenylphosphine ring. The 1H NMR spectral measurements suggest that methylene (-CH2-) in (RAai)Et gives a complex of the AB type multiplet with a coupling constant of ∼7.6 Hz while in RAaiCH2Ph it shows AB type quartets with coupling constant of av. 7.2 Hz. Considering the arylazoimidazole moity, there are different
carbon atoms in the molecule giving different peaks in the 13C NMR spectrum of the complexes. In the 1H-1H COSY spectrum of the present complexes, the absence of any off-diagonal peaks extending from δ = 14.12 and 9.55 ppm confirms
their assignment of no proton on N(1) and N(3), respectively. Contour peaks in the 1H-13C HMQC spectrum in the present complexes, the absence of any contours at δ = 157.12, 160.76, 155.67, and 157.68–160.2 ppm
assign them to the C(2), C(6), C(12), and C(PPh3) carbon atoms, respectively. The solution structure and stereoretentive transformation in each step have been established
from the 1H NMR results.
The article was submitted by the authors in English. |
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