Preparation and Characterization of Bis(dialkyldithiocarbamato)[hydrotris(3,5-dimethyl-1-pyrazolyl)borato]molybdenum(III) Complexes Produced by the Oxidative Decarbonylation of [{HB(3,5-Me2C3N2H)3}Mo(CO)3]- by Tetraaikylthiuram Disulfides. Crystal Structure of {HB(3,5-Me2C3N2H)3}Mo(η2-S2CNEt2)(η1-S2CNEt2)

Charles G. Young, Sue A. Roberts, John H. Enemark

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Abstract

The reactions of Et4N[(HB(Me2pz)3}Mo(CO)3] [HB(Me2pz)3-= hydrotris(3,5-dimethyl-1-pyrazolyl)borate anion] and tetraaikylthiuram disulfides in refluxing acetonitrile produce the yellow or orange, air-sensitive compounds {HB(Me2pz)3}Mo(η2-S2CNR2)(η1-S2CNR2) (1, R = Me; 2, R = Et). The compounds are monomeric, paramagnetic (μeff: 1, 3.93 μB, 2, 3.84 μB) and exhibit infrared bands characteristic of both mono- and bidentate dithiocarbamate ligands. Complex 2 crystallizes in triclinic space group P1 with a = 10.162 (4) Å, b = 11.089 (4) Å, c = 31.10 (1) Å, α = 88.49 (3)°, β = 86.34 (3)°, γ = 68.37 (3)°, V = 3251 (3) Å3, and Z = 4. The structure was solved by Patterson and Fourier methods, followed by least-squares refinement, using 5547 reflections, to a conventional R value of 0.043 (Rw= 0.049). The complex possesses a distorted octahedral fac-N3-fac-S3 coordination sphere composed of tridentate HB(Me2pz)3-, bidentate S2CNEt2-, and monodentate S2CNEt2- ligands. Structural comparison of the two dithiocarbamate ligands indicates considerable thioureide character in the η1 -ligand framework.

Original languageEnglish (US)
Pages (from-to)3667-3671
Number of pages5
JournalInorganic Chemistry
Volume25
Issue number20
DOIs
StatePublished - Sep 1986

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ASJC Scopus subject areas

  • Physical and Theoretical Chemistry
  • Inorganic Chemistry

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