522
A.I. Poddel’sky et al. / Journal of Organometallic Chemistry 696 (2011) 517e522
3.3. Synthesis of complex 3
Cambridge Crystallographic Data Centre,12 Union Road, Cambridge
3.3.1. Oxidation of 1 by air dioxygen
A pale yellow solution of 1 in CDCl3 in NMR tube was opened to
air. A slow steam of air was bubbled through this solution several
times during two days. The colour of solution turned cherry-red.
NMR spectra were recorded for this solution. The slow evaporation
of solvent allowed to obtain dark cherry-red powder of 3.
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3.3.2. Reaction of Q-Q with Me3Sb in equimolar ratio
The toluene solutions of di-o-quinone Q-Q (0.089 g, 0.25 mmol,
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those recorded for sample of 3 prepared by method described in
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Section 3.3.1. 1H NMR (200 MHz, CDCl3,
d, ppm): 1.23 (s, 9 H, tBu),
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Me), 6.40 (s, 1 H, C6H1), 6.78 (s, 1 H, C6H1). 13C NMR (50 MHz, CDCl3,
d, ppm): 12.50 (CH3 of SbMe3), 13.14 (CH3), 13.94 (CH3), 29.29
(C(CH3)3), 30.37 (C(CH3)3), 34.42 (C(CH3)3), 34.94 (C(CH3)3), 114.29
(CH Ar of Cat moiety), 116.48 (Ar), 127.08 (Ar), 131.39 (Ar), 133.33
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The new binuclear bis-catecholate complexes of trimethyl- and
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with a quantitative yield by oxidation reaction of corresponding
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[R3Sb(Cat-SQ)]ꢁ species while air oxidation allows to obtain
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Acknowledgements
This work was made according to FSP “Scientific and scientific-
pedagogical cadres of innovation Russia” for 2009e2013 years
(GK-P982 from 27.05.2010). Authors are grateful to the Russian
FoundationforBasicResearch(grants10-03-00921and10-03-00788),
Russian President Grants (grants NSh-7065.2010.3, MK-1286.2009.3)
for financial support of work.
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Appendix A. Supplementary data
The CCDC-781881 (2 C6H12) contains the supplementary crys-
tallographic data for this paper. These data can be obtained free of