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Synthesis and characteriaztion of novel zirconium(iv) derivatives containing the bis-amido ligand SiMe2(NRR?)2 (Articolo in rivista)

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Synthesis and characteriaztion of novel zirconium(iv) derivatives containing the bis-amido ligand SiMe2(NRR?)2 (Articolo in rivista) (literal)

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Passarelli V. 1, Benetollo F. 2, Zanella P. 3, Carta G. 4, Rossetto G. 5 (2003)
Synthesis and characteriaztion of novel zirconium(iv) derivatives containing the bis-amido ligand SiMe2(NRR?)2
in Dalton transactions (2003. Print)
(literal)

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Passarelli V. 1, Benetollo F. 2, Zanella P. 3, Carta G. 4, Rossetto G. 5 (literal)

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The aminolysis of the Si-Cl bond in SiMe2Cl2 readily affords the bis-amido derivatives SiMe2(NRR')2 [NRR' = NMe2, NEt2, NC4H8, NMeBu, NHEt, NHiPr, NHtBu]. As far as their ligating ability towards the zirconium(IV) centre is concerned, this study has shown that coordination compounds containing the above mentioned species as neutral, monoanionic and dianionic ligand can be prepared.The Lewis adducts ZrCl4[(NRR')2SiMe2] [NRR' = NMe2, NC4H8, NHEt, NHiPr (13), NHtBu, NMeBu (15)] result from the treatment of SiMe2(NRR')2 with ZrCl4. If R # R', the [ZrN2Si] ring contains two stereogenic nitrogen atoms, and, as a consequence, the diasterotopicity of the NCH2 protons in 15 and the non?equivalency of the methyls in the isopropyl groups of 13 have been observed. The reaction of SiMe2(NHtBu)2 and Zr(NMe2)4 yields the mixed amido derivative Zr(NMe2)3(NHMe2)[(NtBu)SiMe2-(NHiBu)) (9), containing the monodentate monoanionic ligand (NtBu)SiMe2(NHtBu). Reasonably because of the bulky tert-butyl groups, the chelation of the ligand is not observed and correspondingly the transfer of only one proton from the silicon species to the coordinated NMe2 groups occurs. Finally, the dianionic ligand SiMe2(NiPr)2 coordinates zirconium(IV) yielding the binary dimer derivative {Zr[(NiPr)2 SiMe2)2z}, (8), whose molecular structure has been elucidated both in the solid state (X-ray diffraction analysis) and in solution (1 D and 2D) multinuclear NMR spectroscopy). (literal)

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Titolo

Synthesis and characteriaztion of novel zirconium(iv) derivatives containing the bis-amido ligand SiMe2(NRR?)2 (literal)

Abstract

The silicon compounds SiMe2(NRR')(2) [NRR' = NMe2 (1), NEt2 (2), NC4H8 (3), NHEt (4), (NHPr)-Pr-i (5), (NHBu)-Bu-t (6), NMeBu (7)] have been synthesised via aminolysis of the dichloro species SiMe2Cl2 and their ligating ability has been investigated towards zirconium(IV). The dimer zirconium compound {Zr[((NPr)-Pr-i)(2)SiMe2](2)}(2) (8) has been synthesised by reacting ZrCl4 with the lithium salt Li-2[((NPr)-Pr-i)(2)SiMe2] and its molecular structure has been determined in the solid state by X-ray diffraction analysis. The reaction of ZrCl4 with SiMe2(NRR')(2) yields the Lewis adducts ZrCl4[(NRR')(2)SiMe2] [NRR' = NMe2 (10), NC4H8 (11), NHEt (12), (NHPr)-Pr-i (13), (NHBu)-Bu-t (14), NMeBu (15)]. On the other hand, the mixed amido derivative Zr(NMe2)(3)(NHMe)[((NBu)-Bu-t) SiMe2((NHBu)-Bu-t)] (9) has been obtained from the reaction of Zr(NMe2)(4) with SiMe2((NHBu)-Bu-t)(2). The solution molecular structure and dynamics of the zirconium derivatives have been elucidated by 1D and 2D multinuclear NMR spectroscopy. (literal)

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