A Mono-, Di-, and Trivanadocene Phosphorus Oxide Series: Synthesis, Magnetism, and Chemical/Electrochemical Properties

Inorganic Chemistry
Timothy G CarrollGabriel Ménard

Abstract

In this Article, we outline the synthesis of B(C6F5)3-coordinated mono-, di-, and trivanadocene phosphorus oxide complexes, Cp2VOP(OB(C6F5)3)Ph2 (2), (Cp2VO)2P(OB(C6F5)3)Ph (3), and (Cp2VO)3P(OB(C6F5)3) (4), respectively (Cp = η5-cyclopentadienyl). The complexes were synthesized from the known reagents, Cp2VF and Ph2P(O)OSiMe3 (for 2) or PhP(O)(OSiMe3)2 (for 3) or (Me3SiO)3PO (for 4), via Me3SiF elimination and in the presence of B(C6F5)3. The multimetallic complexes (3 and 4) could not be synthesized without the capping B(C6F5)3 Lewis acid, whereas the uncapped version of 2, Cp2VOP(O)Ph2 (1), has previously been reported by us. Spectroscopic and crystallographic analyses of 2-4 support an increasingly Lewis basic P═O bond upon substitution of -Ph for -OVCp2 fragments (2-4). The increased metal nuclearity also results in increasingly reducing complexes as evidenced by cyclic voltammetry (CV). Magnetic measurements (SQUID) further revealed high-spin complexes with negligible magnetic exchange between V centers. Chemical oxidation of 2 with 0.5 equiv of [Ag][B(C6F5)4] resulted in a ligand rearrangement reaction producing the VIV product, Cp2V(OP(OB(C6F5)3)Ph2)2 (7). In contrast, the oxidation of 4 with the trityl salt, [Ph3C][B(C...Continue Reading

References

May 27, 2006·Angewandte Chemie·Sandra FeyelHelmut Schwarz
May 29, 2009·Angewandte Chemie·Nicolas DietlHelmut Schwarz
Nov 26, 2013·The Journal of Organic Chemistry·Katarzyna M Błażewska
Jan 8, 2014·Chemical Communications : Chem Comm·Mu-Jeng ChengWilliam A Goddard
Jan 13, 2015·Journal of the American Chemical Society·Justin T HenthornTheodor Agapie
May 1, 2016·Chemical Science·Kenichi ShimizuRichard G Compton

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Citations

Mar 14, 2019·Chemical Communications : Chem Comm·Timothy G CarrollGabriel Ménard

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