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Related Experiment Videos

Triorganophosphine-dithiomonometaphosphoryl halides.

Annegrit Rabis1, Burkhard Ziemer, Dirk Wulff-Molder

  • 1Max Planck Institut für Chemische Physik fester Stoffe, Nöthnitzer Strasse 40, D-01187 Dresden, Germany.

Acta Crystallographica. Section C, Crystal Structure Communications
|April 5, 2002
PubMed
Summary

The first phosphine-stabilized dithiomonometaphosphoryl halides were structurally characterized. Their P-->P bond length varies with halide and phosphine group size, aligning with 31P NMR data.

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Area of Science:

  • Organophosphorus chemistry
  • Coordination chemistry
  • Halide chemistry

Background:

  • Phosphine-stabilized compounds offer unique structural and electronic properties.
  • Dithiomonometaphosphoryl halides represent a class of compounds with limited structural data.
  • Understanding the P-P bond characteristics is crucial for predicting reactivity and stability.

Purpose of the Study:

  • To structurally characterize novel phosphine-stabilized dithiomonometaphosphoryl halides.
  • To investigate the influence of halide and phosphine substituents on the P-->P donor-acceptor bond length.
  • To correlate structural findings with spectroscopic data (31P NMR).

Main Methods:

  • Single-crystal X-ray diffraction was employed for detailed structural analysis.

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  • 31P Nuclear Magnetic Resonance (NMR) spectroscopy was used to complement structural data.
  • Crystallographic data analysis focused on bond lengths, angles, and symmetry elements.

    • Main Results:

    • The study reports the first structural characterization of ethyldiphenylphosphine- and tris-n-propylphosphine-dithiomonometaphosphoryl halides.
    • A trend in P-->P bond length was observed: bromo < chloro < fluoro in tris-n-propylphosphine derivatives.
    • A longer P-->P bond was noted when using the bulkier ethyldiphenylphosphine group compared to tris-n-propylphosphine.
    • In tris-n-propylphosphine derivatives, the P-P bond aligned with the crystallographic threefold axis, indicating disorder.

    Conclusions:

    • The structural data provide fundamental insights into the bonding of phosphine-stabilized dithiomonometaphosphoryl halides.
    • The P-->P bond length is sensitive to both the halide and the steric bulk of the phosphine ligand.
    • Observed structural trends are consistent with the electronic and steric effects influencing the P-->P interaction, as supported by 31P NMR data.