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Reverse Microemulsion-mediated Synthesis of Monometallic and Bimetallic Early Transition Metal Carbide and Nitride Nanoparticles
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Mononuclear and Terminally Bound Titanium Nitrides.

Maria E Carroll1, Balazs Pinter1, Patrick J Carroll1

  • 1Department of Chemistry, University of Pennsylvania, 231 South 34th Street, Philadelphia, Pennsylvania 19104, United States.

Journal of the American Chemical Society
|July 2, 2015
PubMed
Summary
This summary is machine-generated.

Researchers synthesized titanium nitride salts from a titanium azide complex using KC8 reduction. Different crown ethers and cryptands were used to isolate mononuclear and terminal titanium nitride species, confirmed by structural and spectroscopic methods.

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Area of Science:

  • Organometallic Chemistry
  • Inorganic Synthesis
  • Computational Chemistry

Background:

  • Titanium nitride complexes are of interest due to their unique bonding and potential applications.
  • Previous synthetic routes to titanium nitrides often involve harsh conditions or limited scope.
  • Understanding the electronic structure of the Ti-N bond is crucial for reactivity prediction.

Purpose of the Study:

  • To develop a new synthetic route to titanium nitride complexes from a titanium(III) azido precursor.
  • To isolate and characterize different titanium nitride species, including dimeric, mononuclear, and terminal nitrides.
  • To investigate the influence of alkali metal encapsulation on the structure and bonding of titanium nitrides.

Main Methods:

  • Reduction of the Ti(III) azido complex (PN)2Ti(N3) using KC8.
  • Isolation of titanium nitride salts using 18-crown-6 and 2,2,2-Kryptofix.
  • Structural characterization via X-ray crystallography and spectroscopic analysis (NMR, IR).
  • Theoretical investigation using Density Functional Theory (DFT) methods to probe Ti-Nnitride bonding.

Main Results:

  • Efficient synthesis of a dimeric titanium nitride salt [μ2-K(OEt2)]2[(PN)2Ti≡N]2 via KC8 reduction.
  • Isolation of a mononuclear nitride [K(18-crown-6)][(PN)2Ti≡N] and a terminal nitride salt [K(2,2,2-Kryptofix)][(PN)2Ti≡N].
  • Structural and spectroscopic data confirmed the formation of the desired titanium nitride species.
  • DFT calculations provided insights into the electronic structure and bonding characteristics of the Ti-Nnitride moiety.

Conclusions:

  • A versatile synthetic strategy for accessing titanium nitride complexes has been established.
  • The degree of alkali metal encapsulation significantly influences the structure of the titanium nitride species.
  • Theoretical studies complement experimental findings, elucidating the nature of the Ti-Nnitride bond.