Preparation and crystal and molecular structure of [MoO(SCH2CH2PPh2)2]

Joseph Chatt, Jonathan R. Dilworth, James A. Schmutz, Jon A Zubieta

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Abstract

The title complex has been prepared by reaction of [MoO2(acac)2] (acac = pentane-2,4-dionate) with an excess of Ph2PCH2CH2SH in methanol or toluene. The oxo-group can be protonated with anhydrous HBF4 in benzene to give [Mo(OH2)(SCH2CH2PPh2) 2][BF4]2 but does not undergo condensation-type reactions with hydrazines even under forcing conditions. The complex [MoO(SCH2CH2PPh2)2] crystallises in the orthorhombic space group P212121 with four molecules in a unit cell of dimensions a = 10.263(3), b = 10.246(1), and c = 26.657(5) Å. The structure has been solved using 2 179 symmetry-independent reflections with I > 2.58σ(I) collected by counter techniques using Cu-Kα radiation. Refinement by full-matrix least squares, using anisotropic temperature factors for all non-carbon and non-hydrogen atoms, gives a final R factor of 0.063. The co-ordination polyhedron is intermediate between trigonal-bipyramidal and square-pyramidal geometries. The bond distances to Mo are Mo-O 1.733(9), Mo-S(av.) 2.360(4), and Mo-P(av.) 2.484(4) Å.

Original languageEnglish (US)
Pages (from-to)1595-1599
Number of pages5
JournalJournal of the Chemical Society - Dalton Transactions
Issue number10
DOIs
StatePublished - 1979
Externally publishedYes

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Hydrazines
R Factors
Toluene
Benzene
Molecular structure
Methanol
Condensation
Crystal structure
Radiation
Atoms
Molecules
Geometry
Temperature
molybdenum dioxide
pentane

ASJC Scopus subject areas

  • Chemistry(all)

Cite this

Preparation and crystal and molecular structure of [MoO(SCH2CH2PPh2)2]. / Chatt, Joseph; Dilworth, Jonathan R.; Schmutz, James A.; Zubieta, Jon A.

In: Journal of the Chemical Society - Dalton Transactions, No. 10, 1979, p. 1595-1599.

Research output: Contribution to journalArticle

Chatt, Joseph ; Dilworth, Jonathan R. ; Schmutz, James A. ; Zubieta, Jon A. / Preparation and crystal and molecular structure of [MoO(SCH2CH2PPh2)2]. In: Journal of the Chemical Society - Dalton Transactions. 1979 ; No. 10. pp. 1595-1599.
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abstract = "The title complex has been prepared by reaction of [MoO2(acac)2] (acac = pentane-2,4-dionate) with an excess of Ph2PCH2CH2SH in methanol or toluene. The oxo-group can be protonated with anhydrous HBF4 in benzene to give [Mo(OH2)(SCH2CH2PPh2) 2][BF4]2 but does not undergo condensation-type reactions with hydrazines even under forcing conditions. The complex [MoO(SCH2CH2PPh2)2] crystallises in the orthorhombic space group P212121 with four molecules in a unit cell of dimensions a = 10.263(3), b = 10.246(1), and c = 26.657(5) {\AA}. The structure has been solved using 2 179 symmetry-independent reflections with I > 2.58σ(I) collected by counter techniques using Cu-Kα radiation. Refinement by full-matrix least squares, using anisotropic temperature factors for all non-carbon and non-hydrogen atoms, gives a final R factor of 0.063. The co-ordination polyhedron is intermediate between trigonal-bipyramidal and square-pyramidal geometries. The bond distances to Mo are Mo-O 1.733(9), Mo-S(av.) 2.360(4), and Mo-P(av.) 2.484(4) {\AA}.",
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N2 - The title complex has been prepared by reaction of [MoO2(acac)2] (acac = pentane-2,4-dionate) with an excess of Ph2PCH2CH2SH in methanol or toluene. The oxo-group can be protonated with anhydrous HBF4 in benzene to give [Mo(OH2)(SCH2CH2PPh2) 2][BF4]2 but does not undergo condensation-type reactions with hydrazines even under forcing conditions. The complex [MoO(SCH2CH2PPh2)2] crystallises in the orthorhombic space group P212121 with four molecules in a unit cell of dimensions a = 10.263(3), b = 10.246(1), and c = 26.657(5) Å. The structure has been solved using 2 179 symmetry-independent reflections with I > 2.58σ(I) collected by counter techniques using Cu-Kα radiation. Refinement by full-matrix least squares, using anisotropic temperature factors for all non-carbon and non-hydrogen atoms, gives a final R factor of 0.063. The co-ordination polyhedron is intermediate between trigonal-bipyramidal and square-pyramidal geometries. The bond distances to Mo are Mo-O 1.733(9), Mo-S(av.) 2.360(4), and Mo-P(av.) 2.484(4) Å.

AB - The title complex has been prepared by reaction of [MoO2(acac)2] (acac = pentane-2,4-dionate) with an excess of Ph2PCH2CH2SH in methanol or toluene. The oxo-group can be protonated with anhydrous HBF4 in benzene to give [Mo(OH2)(SCH2CH2PPh2) 2][BF4]2 but does not undergo condensation-type reactions with hydrazines even under forcing conditions. The complex [MoO(SCH2CH2PPh2)2] crystallises in the orthorhombic space group P212121 with four molecules in a unit cell of dimensions a = 10.263(3), b = 10.246(1), and c = 26.657(5) Å. The structure has been solved using 2 179 symmetry-independent reflections with I > 2.58σ(I) collected by counter techniques using Cu-Kα radiation. Refinement by full-matrix least squares, using anisotropic temperature factors for all non-carbon and non-hydrogen atoms, gives a final R factor of 0.063. The co-ordination polyhedron is intermediate between trigonal-bipyramidal and square-pyramidal geometries. The bond distances to Mo are Mo-O 1.733(9), Mo-S(av.) 2.360(4), and Mo-P(av.) 2.484(4) Å.

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