Halogen-free GeO2 conversion: electrochemical reduction vs. complexation in (DTBC)2Ge[Py(CN)n] (n = 0…2) complexes

Elena N. Nikolaevskaya; Evgeniya A. Saverina; Alyona A. Starikova; Amel Farhati; Mikhail A. Kiskin; Mikhail A. Syroeshkin; Mikhail P. Egorov; Viatcheslav V. Jouikov

doi:10.1039/C8DT03397H

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Halogen-free GeO₂ conversion: electrochemical reduction vs. complexation in (DTBC)₂Ge[Py(CN)_n] (n = 0…2) complexes†

Elena N. Nikolaevskaya,

^a Evgeniya A. Saverina,^ab Alyona A. Starikova,^c Amel Farhati,^b Mikhail A. Kiskin,

^d Mikhail A. Syroeshkin,

*^a Mikhail P. Egorov^a and Viatcheslav V. Jouikov

*^b

Author affiliations

* Corresponding authors

^a N.D. Zelinsky Institute of Organic Chemistry RAS, Moscow, Russia
E-mail: syroeshkin@ioc.ac.ru

^b UMR CNRS 6226 ISCR, University of Rennes 1, Rennes, France
E-mail: vjouikov@univ-rennes1.fr

^c Institute of Physical and Organic Chemistry at Southern Federal University, Rostov on Don, Russia

^d N.S. Kurnakov Institute of General and Inorganic Chemistry RAS, Moscow, Russia

Abstract

3,5-di-tert-Butylcatecholate (DTBC) germanium complexes (DTBC)₂Ge[Py(CN)_n]₂ (n = 0…2) have been synthesized from GeO₂, 3,5-di-tert-butylcatechol and cyano-substituted pyridines Py(CN)_n and characterized by elemental analysis, NMR, IR and UV-VIS spectroscopy. The structure of 1 (with 4-cyanopyridine) has been determined by X-ray single crystal analysis. UV-VIS spectra have shown that these complexes are stable in CH₃CN, toluene and CH₂Cl₂ solutions; in contrast, they are rapidly decomposed by dimethylformamide and tetrahydrofuran. Complexes 1 and 2 (with 4-cyano and 3-cyanopyridine) are electrochemically reducible in toluene/1 M Bu₄NPF₆ at E = −1.3…−1.7 V vs. AgCl. The quantum-chemical study of these complexes is in accordance with the unsuccessful attempts to obtain analogous derivatives with 2-cyanopyridine and 2,6-dicyanopyridine.

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Article information

DOI: https://doi.org/10.1039/C8DT03397H
Article type: Paper
Submitted: 20 Aug 2018
Accepted: 05 Nov 2018
First published: 06 Nov 2018

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Dalton Trans., 2018,47, 17127-17133

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Halogen-free GeO₂ conversion: electrochemical reduction vs. complexation in (DTBC)₂Ge[Py(CN)_n] (n = 0…2) complexes

E. N. Nikolaevskaya, E. A. Saverina, A. A. Starikova, A. Farhati, M. A. Kiskin, M. A. Syroeshkin, M. P. Egorov and V. V. Jouikov, Dalton Trans., 2018, 47, 17127 DOI: 10.1039/C8DT03397H

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