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Title: Redox-Active 1D Coordination Polymers of Iron–Sulfur Clusters

Abstract

Here we describe the combination of an archetypal redox-active metal sulfide cluster, Fe4S4, with an organic linker, 1,4-benzenedithiolate, to prepare coordination polymers containing infinite chains of Fe4S4 clusters. The crystal structures of two solid materials have been solved from synchrotron X-ray powder diffraction data using simulated annealing and re-fined by a least-squares Rietveld refinement procedure. The electronic properties of these chains have also been characterized by UV-visible and Mössbauer spectroscopies. Additional experiments demonstrated that these chains can be solubilized by variation of the countercation and that the chain structure is maintained in solution. The redox-activity of the Fe4S4 clusters can be accessed with chemical reagents. Introduction of charge carriers by reduction of the Fe4S4 clusters is found to increase the electrical conductivity of the materials by up to four orders of magnitude. These results highlight the utility of Fe4S4 clusters as redox-active building blocks in preparing new classes of coordination polymers.

Authors:
 [1];  [1]; ORCiD logo [1];  [2]; ORCiD logo [3];  [4];  [1];  [1]; ORCiD logo [1]
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  1. Univ. of Chicago, Chicago, IL (United States)
  2. Saclay Institute for Matter and Radiation (IRAMIS), Gif-sur-Yvette (France)
  3. Synchrotron SOLEIL, Gif-sur-Yvette (France)
  4. Northwestern Univ., Evanston, IL (United States)
Publication Date:
Research Org.:
Univ. of Chicago, IL (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES)
OSTI Identifier:
1524597
Grant/Contract Number:  
SC0019215
Resource Type:
Accepted Manuscript
Journal Name:
Journal of the American Chemical Society
Additional Journal Information:
Journal Volume: 141; Journal Issue: 9; Related Information: http://pubs.acs.org/doi/suppl/10.1021/jacs.8b12339/suppl_file/ja8b12339_si_001.pdf; Journal ID: ISSN 0002-7863
Publisher:
American Chemical Society (ACS)
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; iron-sulfur clusters

Citation Formats

Horwitz, Noah E., Xie, Jiaze, Filatov, Alexander S., Papoular, Robert J., Shepard, William E., Zee, David Z., Grahn, Mia P., Gilder, Chloe, and Anderson, John S. Redox-Active 1D Coordination Polymers of Iron–Sulfur Clusters. United States: N. p., 2019. Web. doi:10.1021/jacs.8b12339.
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Horwitz, Noah E., Xie, Jiaze, Filatov, Alexander S., Papoular, Robert J., Shepard, William E., Zee, David Z., Grahn, Mia P., Gilder, Chloe, & Anderson, John S. Redox-Active 1D Coordination Polymers of Iron–Sulfur Clusters. United States. https://doi.org/10.1021/jacs.8b12339
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Horwitz, Noah E., Xie, Jiaze, Filatov, Alexander S., Papoular, Robert J., Shepard, William E., Zee, David Z., Grahn, Mia P., Gilder, Chloe, and Anderson, John S. Mon . "Redox-Active 1D Coordination Polymers of Iron–Sulfur Clusters". United States. https://doi.org/10.1021/jacs.8b12339. https://www.osti.gov/servlets/purl/1524597.
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@article{osti_1524597,
title = {Redox-Active 1D Coordination Polymers of Iron–Sulfur Clusters},
author = {Horwitz, Noah E. and Xie, Jiaze and Filatov, Alexander S. and Papoular, Robert J. and Shepard, William E. and Zee, David Z. and Grahn, Mia P. and Gilder, Chloe and Anderson, John S.},
abstractNote = {Here we describe the combination of an archetypal redox-active metal sulfide cluster, Fe4S4, with an organic linker, 1,4-benzenedithiolate, to prepare coordination polymers containing infinite chains of Fe4S4 clusters. The crystal structures of two solid materials have been solved from synchrotron X-ray powder diffraction data using simulated annealing and re-fined by a least-squares Rietveld refinement procedure. The electronic properties of these chains have also been characterized by UV-visible and Mössbauer spectroscopies. Additional experiments demonstrated that these chains can be solubilized by variation of the countercation and that the chain structure is maintained in solution. The redox-activity of the Fe4S4 clusters can be accessed with chemical reagents. Introduction of charge carriers by reduction of the Fe4S4 clusters is found to increase the electrical conductivity of the materials by up to four orders of magnitude. These results highlight the utility of Fe4S4 clusters as redox-active building blocks in preparing new classes of coordination polymers.},
doi = {10.1021/jacs.8b12339},
journal = {Journal of the American Chemical Society},
number = 9,
volume = 141,
place = {United States},
year = {Mon Feb 04 00:00:00 EST 2019},
month = {Mon Feb 04 00:00:00 EST 2019}
}
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FOX , `free objects for crystallography': a modular approach to ab initio structure determination from powder diffraction
journal, November 2002

  • Favre-Nicolin, Vincent; Černý, Radovan
  • Journal of Applied Crystallography, Vol. 35, Issue 6
  • DOI: 10.1107/S0021889802015236

Syntheses and structural characterizations of Fe4S4 cubane-like cluster compounds containing cycloalkylthiolate ligands
journal, December 1997

  • Liu, Qiutian; Zhang, Chunxi; Chen, Changneng
  • Science in China Series B: Chemistry, Vol. 40, Issue 6
  • DOI: 10.1007/BF02875480

X-ray crystal structures of [NHR3]2[Fe4S4X4] (X = PhS, R = Et or n Bu; X = Cl, R =  n Bu): implications for sites of protonation in Fe–S clusters
journal, April 2016

  • Al-Rammahi, Thaer M. M.; Waddell, Paul G.; Henderson, Richard A.
  • Transition Metal Chemistry, Vol. 41, Issue 5
  • DOI: 10.1007/s11243-016-0052-5

Mercury : visualization and analysis of crystal structures
journal, May 2006

  • Macrae, Clare F.; Edgington, Paul R.; McCabe, Patrick
  • Journal of Applied Crystallography, Vol. 39, Issue 3
  • DOI: 10.1107/S002188980600731X

Mercury CSD 2.0 – new features for the visualization and investigation of crystal structures
journal, March 2008

  • Macrae, Clare F.; Bruno, Ian J.; Chisholm, James A.
  • Journal of Applied Crystallography, Vol. 41, Issue 2
  • DOI: 10.1107/S0021889807067908

CCDC 1472848: Experimental Crystal Structure Determination
dataset, January 2016

  • Al-Rammahi, Thaer M. M.; Waddell, Paul G.; Henderson, Richard A.
  • Cambridge Crystallographic Data Centre
  • DOI: 10.5517/ccdc.csd.cc1lfm7w
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