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Structural Phase Transitions in closo-Dicarbadodecaboranes C2B10H12.

Matteo Brighi1, Fabrizio Murgia1, Zbigniew Łodziana2

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This study reveals the crystal structures of closo-dicarbadodecaboranes isomers, detailing their thermal polymorphism and rotational dynamics. These findings aid in designing novel solid electrolytes with tunable properties.

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Area of Science:

  • Materials Science
  • Solid-state Chemistry
  • Crystallography

Background:

  • Thermal polymorphism in closo-dicarbadodecaboranes (C2B10H12) isomers influences their solid-state properties.
  • Understanding the rotational dynamics of these icosahedral clusters is crucial for materials design.

Purpose of the Study:

  • To determine the crystal structures of three thermal polymorphs (I, II, III) for ortho-, meta-, and para-isomers of C2B10H12.
  • To elucidate the relationship between molecular structure, rotational dynamics, and thermal behavior.
  • To explore the potential of these compounds in designing advanced solid electrolytes.

Main Methods:

  • Synchrotron radiation X-ray powder diffraction was employed to analyze crystal structures.
  • Density functional theory (DFT) calculations complemented experimental diffraction data.
  • Calorimetric and spectroscopic studies were used for validation.

Main Results:

  • Crystal structures of three thermal polymorphs (I, II, III) were determined for all C2B10H12 isomers.
  • Phase I exhibits isotropic rotations, while Phase II shows anisotropic rotations of the clusters.
  • Phase III represents ordered, deformed structures of the cubic unit cells from Phases I and II.
  • The ortho-isomer's ordering in Phase III creates a superstructure due to its dipole moment.
  • Thermal polymorphism is explained by dispersive and anisotropic local interactions, modulated by cluster dynamics.
  • C2B10H12 clusters demonstrate good oxidation resistance, comparable to CB11H12- anions.

Conclusions:

  • The study provides a comprehensive structural and dynamic understanding of C2B10H12 thermal polymorphism.
  • The findings support the design of mixed compounds, such as Na(CB11H12)(C2B10H12), for solid electrolytes.
  • Tuning cation content in these electrolytes can lower the transition temperature to disordered conducting phases.