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ansa-metallocene derivatives : XXV. Synthesis, crystal structure and reactions of a tetramethylethano-bridged vanadocene dichloride, (CH<sub>3</sub>)<sub>4</sub>C<sub>2</sub>(C<sub>5</sub>H<sub>4</sub>)<sub>2</sub>VCl<sub>2</sub>

ansa-metallocene derivatives : XXV. Synthesis, crystal structure and reactions of a tetramethylethano-bridged vanadocene dichloride, (CH3)4C2(C5H4)2VCl2

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DORER, Birgit, Josef DIEBOLD, Oliver WEYAND, Hans-Herbert BRINTZINGER, 1992. ansa-metallocene derivatives : XXV. Synthesis, crystal structure and reactions of a tetramethylethano-bridged vanadocene dichloride, (CH3)4C2(C5H4)2VCl2. In: Journal of Organometallic Chemistry. 427(2), pp. 245-255. ISSN 0022-328X

@article{Dorer1992ansa--23894, title={ansa-metallocene derivatives : XXV. Synthesis, crystal structure and reactions of a tetramethylethano-bridged vanadocene dichloride, (CH3)4C2(C5H4)2VCl2}, year={1992}, doi={10.1016/0022-328X(92)83088-Y}, number={2}, volume={427}, issn={0022-328X}, journal={Journal of Organometallic Chemistry}, pages={245--255}, author={Dorer, Birgit and Diebold, Josef and Weyand, Oliver and Brintzinger, Hans-Herbert} }

eng Dorer, Birgit 2013-07-31T07:28:49Z Diebold, Josef 2013-07-31T07:28:49Z Diebold, Josef Brintzinger, Hans-Herbert Brintzinger, Hans-Herbert Journal of Organometallic Chemistry ; 427 (1992), 2. - S. 245-255 deposit-license Dorer, Birgit 1992 Weyand, Oliver Weyand, Oliver The tetramethylethano-bridged vanadocene complex (CH<sub>3</sub>)<sub>4</sub>C<sub>2</sub>(C<sub>5</sub>H<sub>4</sub>)<sub>2</sub>VCl<sub>2</sub> has been made in two ways: (i) from VCl<sub>3</sub>·3THF by reaction with (CH<sub>3</sub>)<sub>4</sub>C<sub>2</sub>(C<sub>5</sub>H<sub>4</sub>MgCl·2THF)<sub>2</sub> in THF and subsequent oxidation with PCl<sub>3</sub>, and (ii) from VCl<sub>4</sub>·2THF by reaction with (CH<sub>3</sub>)<sub>4</sub>C<sub>2</sub>(C<sub>5</sub>H<sub>4</sub>Li)<sub>2</sub> or with (CH<sub>3</sub>)<sub>4</sub>C<sub>2</sub>(C<sub>5</sub>H<sub>4</sub>MgCl·2THF)<sub>2</sub> in a toluene/dimethoxyethane mixture. Its crystal structure is in accordance with expectations. Reduction of (CH<sub>3</sub>)<sub>4</sub>C<sub>2</sub>(C<sub>5</sub>H<sub>4</sub>)<sub>2</sub>VCl<sub>2</sub> with tetrakis(dimethylamino)ethene in toluene or with LiAlH<sub>4</sub> in THF yields the monochloride (CH<sub>3</sub>)<sub>4</sub>C<sub>2</sub>(C<sub>5</sub>H<sub>4</sub>)<sub>2</sub>VCl; from this V<sup>III</sup> compound cationic complexes (CH<sub>3</sub>)<sub>4</sub>C<sub>2</sub>(C<sub>5</sub>H<sub>4</sub>)<sub>2</sub>VL<sub>2</sub><sup>+</sup> with L = CO or CN<sup>t</sup>Bu are readily obtained by ligand exchange. <sup>1</sup>H NMR signals of these diamagnetic complexes have been assigned to H atoms in α and β C<sub>5</sub>-ring positions by use of selective nuclear Overhauser effects. The ring-bridged V<sup>II</sup> complex (CH<sub>3</sub>)<sub>4</sub>C<sub>2</sub>(C<sub>5</sub>H<sub>4</sub>)<sub>2</sub>V could not be prepared. Cyclovoltammetry studies indicate that (in contrast to its unbridged counterpart (C<sub>5</sub>H<sub>5</sub>)<sub>2</sub>V) this V<sup>II</sup> complex decays within seconds after its formation by electrochemical reduction of its chloro derivatives. ansa-metallocene derivatives : XXV. Synthesis, crystal structure and reactions of a tetramethylethano-bridged vanadocene dichloride, (CH<sub>3</sub>)<sub>4</sub>C<sub>2</sub>(C<sub>5</sub>H<sub>4</sub>)<sub>2</sub>VCl<sub>2</sub>

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