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"MoCl3(dme)" Revisited: Improved Synthesis, Characterization, and X-ray and Electronic Structures.

Thomas E Shaw1,2, Timothy J Diethrich3, Brian L Scott4

  • 1Department of Chemistry, University of Central Florida, Orlando, Florida 32816, United States.

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|August 6, 2021
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Summary
This summary is machine-generated.

The synthesis of Mo2Cl6(dme)2 was achieved using dimethylphenylsilane, clarifying the structure of the molybdenum precursor MoCl3(dme). This study also demonstrates organosilanes as effective reductants in inorganic synthesis.

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Area of Science:

  • Inorganic Chemistry
  • Organometallic Chemistry
  • Materials Science

Background:

  • The precursor "MoCl3(dme)" (dme = 1,2-dimethoxyethane) is crucial for midvalent molybdenum chemistry, especially for Mo-Mo triple bonds.
  • The precise structural identity of "MoCl3(dme)" has remained elusive for over fifty years.

Purpose of the Study:

  • To establish a convenient, large-scale synthesis for "MoCl3(dme)".
  • To definitively determine the structure of the molybdenum precursor.
  • To explore the utility of organosilanes as reducing agents in inorganic synthesis.

Main Methods:

  • Reduction of trans-MoCl4(Et2O)2 in dme using dimethylphenylsilane (Me2PhSiH).
  • Isolation and purification of the product, Mo2Cl6(dme)2.
  • X-ray crystallography for structural determination.
  • Gouy method and SQUID magnetometry for magnetic property analysis.
  • Density functional theory (DFT) calculations for electronic structure analysis.

Main Results:

  • A high-yield (∼90%) synthesis of khaki Mo2Cl6(dme)2 was developed using dimethylphenylsilane.
  • Two distinct crystal morphologies were identified, both belonging to the P21/n space group, revealing an edge-shared bioctahedral structure with a Mo-Mo bond length of approximately 2.8 Å.
  • The bulk material was found to be diamagnetic.
  • DFT calculations indicated a σ2π2δ*2 ground state with diamagnetism arising from a singlet diradical electronic configuration.

Conclusions:

  • The structure of "MoCl3(dme)" has been definitively assigned.
  • Dimethylphenylsilane is presented as an effective and convenient reducing agent for inorganic synthesis.
  • The study provides insights into the electronic structure and bonding of midvalent molybdenum dimers.