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Tetragonal to triclinic--a phase change for [Fe(TPP)(NO)].

Nathan J Silvernail1, Marilyn M Olmstead, Bruce C Noll

  • 1Department of Chemistry and Biochemistry, University of Notre Dame, Notre Dame, Indiana 46556, USA.

Inorganic Chemistry
|January 9, 2009
PubMed
Summary

The crystalline phase of iron(II) tetraphenylporphyrin nitrosyl complex transitions from tetragonal to triclinic below 250 K. This ordering reveals subtle molecular geometry changes, including an off-axis nitrosyl ligand tilt.

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Area of Science:

  • Coordination Chemistry
  • Solid-State Chemistry
  • Crystallography

Background:

  • (Nitrosyl)(tetraphenylporphinato)iron(II), [Fe(TPP)(NO)], is an iron porphyrin complex.
  • Understanding the temperature-dependent crystalline phases is crucial for its properties.

Purpose of the Study:

  • To investigate the temperature dependence of the crystalline phase of [Fe(TPP)(NO)] from 33 K to 293 K.
  • To characterize the structural changes and molecular ordering during the phase transition.

Main Methods:

  • X-ray diffraction studies were employed to analyze crystal structures at various temperatures.
  • Differential scanning calorimetry (DSC) was used to confirm the phase transition thermodynamics.

Main Results:

  • The complex exhibits a tetragonal crystal system at higher temperatures and a triclinic system at lower temperatures.
  • A reversible phase transition occurs around 250 K, involving increased ordering of the nitrosyl ligand.
  • The transition reveals an off-axis tilt of the Fe-N(NO) bond from the heme normal due to partial ordering.

Conclusions:

  • The crystalline phase of [Fe(TPP)(NO)] is temperature-dependent, transitioning from a disordered tetragonal phase to a more ordered triclinic phase.
  • The observed structural changes provide insights into the molecular geometry and ligand behavior in the solid state.
  • The study confirms a reversible phase transition with implications for the material's properties.