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Ferrocenyl-based di- and trinuclear lanthanide complexes: solid state structures, (spectro)electrochemical and DFT

Ahmed Khalladi1, Eduard Kovalski1, Mohammad A Abdulmalic1

  • 1Technische Universität, Research Centre for Materials, Architectures and Integration of Nanomembranes (MAIN), Research Group Organometallic Chemistry, Rosenbergstraße 6, D-09126 Chemnitz, Germany. heinrich.lang@chemie.tu-chemnitz.de.

Dalton Transactions (Cambridge, England : 2003)
|November 27, 2023
PubMed
Summary

New dinuclear and trinuclear ferrocenylcarboxylato-bridged lanthanide complexes were synthesized. Electrochemical studies revealed superimposed redox events for dinuclear complexes and distinct events for trinuclear complexes, influenced by spatial proximity.

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Area of Science:

  • Coordination Chemistry
  • Organometallic Chemistry
  • Materials Science

Background:

  • Lanthanide complexes with ferrocenylcarboxylato ligands are of interest for their unique structural and electronic properties.
  • Understanding the relationship between structure, coordination modes, and electrochemical behavior is crucial for designing new functional materials.

Purpose of the Study:

  • To synthesize and characterize novel dinuclear and trinuclear ferrocenylcarboxylato-bridged lanthanide complexes.
  • To investigate the structural features, coordination chemistry, and electrochemical properties of these new complexes.
  • To elucidate the factors governing the redox behavior of the ferrocenylcarboxylato ligands within these lanthanide frameworks.

Main Methods:

  • Synthesis of dinuclear and trinuclear lanthanide complexes using lanthanide chlorides and ferrocenylcarboxylic acid.
  • Single crystal X-ray structure determination to elucidate molecular structures and coordination modes.
  • Infrared (IR) spectroscopy to confirm structural motifs.
  • Electrochemical studies including cyclic voltammetry (CV) and square-wave voltammetry (SWV).
  • UV-Vis/NIR spectroelectrochemical measurements.
  • Density Functional Theory (DFT) calculations.

Main Results:

  • Successful synthesis of dinuclear [Ln(μO:κ2OO'-O2CFc)(O2CFc)2(H2O)(dmf)]2·(dmf)2 and trinuclear [Bu4N][Ln3(μ-O2CFc)3(μO:κ2OO'-O2CFc)3(O2CFc)3(μ3-OH)]·[Bu4N]Cl complexes.
  • X-ray crystallography revealed intricate bridging of lanthanide ions by ferrocenylcarboxylato units and specific coordination numbers and geometries.
  • Electrochemical studies showed superimposed redox events for dinuclear complexes and three distinct events for trinuclear complexes, with redox behavior correlating to mononuclear analogues.
  • Spectroelectrochemical measurements indicated no electron transfer between ferrocenyl units or lanthanides in the trinuclear terbium complex.
  • DFT calculations highlighted the importance of spatial distance over binding mode in determining the order of redox events in trinuclear complexes.

Conclusions:

  • The study successfully synthesized and characterized novel ferrocenylcarboxylato-bridged dinuclear and trinuclear lanthanide complexes.
  • The structural diversity and coordination modes significantly influence the electrochemical properties of these complexes.
  • Redox behavior in trinuclear complexes is primarily governed by the spatial arrangement of ferrocenyl units, as supported by DFT calculations.