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A stable monomeric nickel borohydride.

Patrick J Desrochers1, Stacey LeLievre, Rosemary J Johnson

  • 1Department of Chemistry, University of Central Arkansas, Conway, Arkansas 72035, USA. patrickd@mail.uca.edu

Inorganic Chemistry
|November 25, 2003
PubMed
Summary
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A novel nickel borohydride complex, Tp*NiBH(4), demonstrates remarkable stability against air, water, and heat. This stable complex effectively reduces halocarbons, showcasing its potential in chemical synthesis.

Area of Science:

  • Inorganic Chemistry
  • Organometallic Chemistry
  • Materials Science

Background:

  • Borohydride complexes are crucial in catalysis and synthesis.
  • Nickel borohydrides are often unstable and difficult to characterize.
  • The hydrotris(3,5-dimethylpyrazolyl)borate (Tp*-) ligand offers steric protection and electronic tuning for metal centers.

Purpose of the Study:

  • To synthesize and characterize a stable nickel borohydride complex.
  • To investigate the reactivity of the nickel borohydride complex with halocarbons.
  • To elucidate the structural and electronic properties of the complex using spectroscopic and crystallographic methods.

Main Methods:

  • Synthesis of nickel borohydride complex using Tp*- ligand.
  • X-ray crystallography for structural determination.

Related Experiment Videos

  • Infrared (IR) spectroscopy to identify B-H and B-D bonds.
  • Nickel K-edge X-ray absorption spectroscopy (XAS) for electronic structure analysis.
  • Reactions with halocarbon substrates to study reduction pathways.

    • Main Results:

    • A stable nickel(II) borohydride complex, Tp*NiBH(4) (and its deuterated analog Tp*NiBD(4)), was successfully prepared.
    • The complex exhibits high thermal stability (mp > 230 °C) and resistance to air and boiling water.
    • X-ray crystallography revealed a six-coordinate geometry with facial coordination of borohydride.
    • IR spectroscopy confirmed bridging hydrogen atoms and showed expected shifts for the deuterated analog.
    • The complex readily reduced halocarbons with a significant kinetic isotope effect (k(H)/k(D) ≈ 3).
    • XAS studies confirmed the six-coordinate geometry of the nickel borohydride and contrasted it with a pseudotetrahedral Tp*NiCl complex.

    Conclusions:

    • The Tp*- ligand imparts significant stability to the nickel borohydride complex.
    • The stable nickel borohydride is a potent reducing agent for halocarbons.
    • This work provides a well-characterized example of a stable nickel borohydride, advancing understanding of these important compounds.