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1,2-Bis(dimethylphosphino)ethane (dmpe) Alkyl Compounds of Zirconium(IV) and Hafnium(IV). Crystal Structures of ZrMe4(dmpe)2 and Zr(CH2Ph)4(dmpe)

DOI: 10.1039/DT9840002789

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 2789 - 2794 (1984)

Update date:2022-09-26

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Authors:

Girolami, Gregory S.Girolami, Gregory S.

Wilkinson, GeoffreyWilkinson, Geoffrey

Thornton-Pett, MarkThornton-Pett, Mark

Hursthouse, Michael B.Hursthouse, Michael B.

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Article abstract of DOI:10.1039/DT9840002789

The reaction of ZrCl4(dmpe)2 with excess MgMe2 gives the dialkyldichloro-complex ZrMe2Cl2(dmpe)2, whereas interaction with excess LiMe gives the tetra-alkyl ZrMe4(dmpe)2.N.m.r. data indicate a rigid structure for the latter molecule at -60 deg C, while the X-ray crystal structure shows the molecule, which has crystallographic C2 symmetry, to have dodecahedral geometry with the methyl groups at the (B) sites and the phosphines at the (A) sites: Zr-C 2.440(6), Zr-P 2.814(1) Angstroem.Alkylation of ZrCl4(dmpe)2 with excess LiCH2SiMe3 leads to the six-co-ordinate complex Zr(CH2SiMe3)4(dmpe); the analogous compound Zr(CH2Ph)4(dmpe) can be prepared from Zr(CH2Ph)4 and dmpe.The X-ray crystal structure of Zr(CH2Ph)4(dmpe) shows a severely distorted octahedral geometry consisting of three ?-benzyl groups and one partially ?-bonded benzyl group: Zr-C(?) 2.264(7)-2.368(5), Zr-Cα(?) 2.359(6), Zr<*>Cβ(?) 2.788(8), Zr-P 2.862(4), 2.885(4) Angstroem.The preparations and characterizations of some Hafnium analogues are also described.

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Product name:tetrabenzyl[1,2-bis(dimethylphosphino)ethane-PP']zirconium(IV)

Cas No:95827-43-3

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