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Dinitrogen Complexes of Tungsten with Bulky Phosphine Co-ligands. Preparation and Crystal Structures of 2(μ-N2)>, trans-*C4H8O, and 6-C6H5PPrn2)(N2)(PPrn2Ph)2> and their Reactions to give Hydrazine or Ammonia

DOI: 10.1039/DT9860000245

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 245 - 252 (1986)

Update date:2022-07-31

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Authors:

Anderson, Stewart N.Anderson, Stewart N.

Richards, Raymond L.Richards, Raymond L.

Hughes, David L.Hughes, David L.

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Article abstract of DOI:10.1039/DT9860000245

Reduction of WCl6 or (R=Et or Prn) with Mg in the presence of PR2Ph under N2 in tetrahydrofuran (thf) gives a mixture of dinitrogen complexes: <2(μ-N2)> (1), trans- (2), and 6-C6H5PR2)(N2)(PR2Ph)2> (3) which can be observed in the (15)N n.m.r. spectra of the reaction solutions and isolated in most cases in moderate yield.Compound (1a) (R=Et) is shown to be a dimer by X-ray analysis but the structure could be refined only with constraints on interatomic distances.Compounds (1) react with anhydrous HCl (thf, 20 deg C) to give hydrazine (0.2 mol/W atom) and dinitrogen (2 mol/W atom).Compound (2a) (R=Et) crystallizes as a thf solvate with W-N=1.986(6) and 1.994(6), N-N=1.146(7) and 1.139(7) Angstroem.Complex (2a) gives ammonia (1.8 mol/W atom) and N2 (1 mol/W atom) on treatment with H2SO4-MeOH.Compound (3b) (R=Prn) has W-N=1.980(8) and N-N=1.126(10) Angstroem and loses N2 quantitatively on treatment with anhydrous HCl in thf.

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Product name:W(C6H5P(C2H5)2)(N2)(P(C2H5)2(C6H5))2

Cas No:103407-77-8

103407-77-8

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