Dinitrogen, Butadiene and Related Complexes of Molybdenum. Crystal Sructures of and (η4-C4H6)(PEt3)2>

DOI: 10.1039/DT9950003801

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 3801 - 3808 (1995)

Update date:2022-08-03

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Authors:

Galindo, Agustin

Gutierrez, Enrique

Monge, Angeles

Paneque, Margarita

Pastor, Antonio

et al. et al.

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Article abstract of DOI:10.1039/DT9950003801

The sodium amalgam reduction of prepared in situ, under 2-3 atm of N2, yielded the dimeric complex <2(μ-N2)> 1, which reacted with 3 and with 4 equivalents of PMe3 to produce trans- 2 and trans- 3, respectively.In the presence of an excess of PMe3 (>5 equivalents, under Ar) the known 4a was the final product.This synthetic methodology allowed the preparation, for the first time, of the pure trans-bis(dinitrogen) compound 3.Complexes of the type (L-L=Me2PCH2PMe2 4b, Me2PCH2CH2PMe2 4c or Et2PCH2CH2PEt2 4d) and > 4e were also synthesized and structurally characterized by spectroscopic methods.Upon reaction with C2H4, under mild conditions, 1 gave the bis(butadiene) derivative 4-C4H6)2(PEt3)2> 5a.Protonation of 5a, and of its PMe2Ph analogue 5b, produced the cationic but-2-enyls <<*>(η⁴-C4H6)(L2> (L=PEt3 6a or PMe2Ph 6b) in which the butenyl ligand exhibits the classical η³-allylic co-ordination in addition to an agostic Me-Mo interaction.Compounds 4a and 6a were structurally characterized by X-ray crystallography.The Mo atom of 4a resides on a crystallographic mirror plane and is bound to the N2 moiety with a Mo-N separation of 2.02(3) Angstroem.The Mo-C and Mo-H separations within the agostic unit of 6a are 2.48(2) and 1.9(2) Angstroem, respectively.

Full text of DOI:10.1039/DT9950003801

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