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Structural insights for vanadium catecholates and iron‑sulfur clusters obtained from multiple data analysis methods

Thacien Ngendahimana1, Richard Ayikpoe1, John A Latham1

  • 1Department of Chemistry and Biochemistry, University of Denver, Denver, CO 80210, United States of America.

Journal of Inorganic Biochemistry
|September 11, 2019
PubMed
Summary

Electron paramagnetic resonance (EPR) inversion recovery analysis reveals that stretched exponential and sum of two exponentials models fit data equally well. The UPEN model offers insights into relaxation rate distributions for metal-ligand systems and iron-sulfur clusters.

Keywords:
Distribution of exponentialsHydrogenase maturaseIron‑sulfur clustersMycofactocin maturasePyruvate formate lyase activating enzymeVanadium(IV) catecholate

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Area of Science:

  • * Biophysical chemistry
  • * Spectroscopic methods
  • * Inorganic chemistry

Background:

  • * Electron paramagnetic resonance (EPR) is a powerful technique for studying paramagnetic species.
  • * Analyzing EPR inversion recovery curves provides insights into spin-lattice relaxation processes.
  • * Various models exist for analyzing relaxation data, each with strengths and limitations.

Purpose of the Study:

  • * To compare the efficacy of three models (sum of two exponentials, stretched exponential, and UPEN) for analyzing EPR inversion recovery data.
  • * To investigate the structural and dynamic information provided by these models for vanadium catecholates and iron-sulfur clusters.
  • * To explore the utility of the UPEN model in elucidating complex relaxation behaviors.

Main Methods:

  • * Analysis of electron paramagnetic resonance (EPR) inversion recovery curves.
  • * Application and comparison of three kinetic models: sum of two exponentials, stretched exponential, and model-free distribution of exponentials (UPEN).
  • * Investigation of temperature dependence of spin-lattice relaxation.

Main Results:

  • * Stretched exponential and sum of two exponentials models provided statistically indistinguishable fits, outperforming single exponential fits.
  • * The UPEN model revealed insights into spectral diffusion in vanadium complexes and contributions from rapidly relaxing species in iron-sulfur clusters.
  • * Broad relaxation rate distributions were observed for [4Fe-4S]+ clusters, potentially due to protein dynamics and environmental heterogeneity.

Conclusions:

  • * Stretched exponential and sum of two exponentials models are robust for analyzing EPR relaxation data.
  • * The UPEN model is valuable for dissecting complex relaxation phenomena, including spectral diffusion and contributions from multiple species.
  • * EPR relaxation analysis, particularly with UPEN, provides detailed insights into the dynamics and environments of metalloenzymes and metal complexes.