Insensitivity of Magnetic Coupling to Ligand Substitution in a Series of Tetraoxolene Radical-Bridged Fe2 Complexes

Thorarinsdottir, Agnes E.; Bjornsson, Ragnar; Harris, T. David

doi:10.1021/acs.inorgchem.9b03736

Title: Insensitivity of Magnetic Coupling to Ligand Substitution in a Series of Tetraoxolene Radical-Bridged Fe₂ Complexes

Journal Article · Fri Mar 20 00:00:00 EDT 2020 · Inorganic Chemistry

DOI:https://doi.org/10.1021/acs.inorgchem.9b03736· OSTI ID:1803720

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Northwestern Univ., Evanston, IL (United States)
Max-Planck-Inst. für Chemische Energiekonversion, Mülheim an der Ruhr (Germany)
Northwestern Univ., Evanston, IL (United States); Univ. of California, Berkeley, CA (United States)

The elucidation of magnetostructural correlations between bridging ligand substitution and strength of magnetic coupling is essential to the development of high-temperature molecule-based magnetic materials. Toward this end, we report the series of tetraoxolene-bridged Fe^II₂ complexes [(Me₃TPyA)₂Fe₂(^RL)]ⁿ⁺ (Me₃TPyA = tris(6-methyl-2-pyridylmethyl)amine; n = 2: ^OMeLH₂ = 3,6-dimethoxy-2,5-dihydroxo-1,4-benzoquinone, ^ClLH₂ = 3,6-dichloro-2,5-dihydroxo-1,4-benzoquinone, Na₂[^NO₂L] = sodium 3,6-dinitro-2,5-dihydroxo-1,4-benzoquinone; n = 4: ^SMe₂L = 3,6-bis(dimethylsulfonium)-2,5-dihydroxo-1,4-benzoquinone diylide) and their one-electron-reduced analogues. Furthermore, variable-temperature dc magnetic susceptibility data reveal the presence of weak ferromagnetic superexchange between Fe^II centers in the oxidized species, with exchange constants of J = +1.2(2) (R = OMe, Cl) and +0.3(1) (R = NO₂, SMe₂) cm^–1. In contrast, X-ray diffraction, cyclic voltammetry, and Mössbauer spectroscopy establish a ligand-centered radical in the reduced complexes. Magnetic measurements for the radical-bridged species reveal the presence of strong antiferromagnetic metal–radical coupling, with J = -57(10), -60(7), -58(6), and -65(8) cm^–1 for R = OMe, Cl, NO₂, and SMe₂, respectively. The minimal effects of substituents in the 3- and 6-positions of ^RL^x–• on the magnetic coupling strength is understood through electronic structure calculations, which show negligible spin density on the substituents and associated C atoms of the ring. Finally, the radical-bridged complexes are single-molecule magnets, with relaxation barriers of U_eff = 50(1), 41(1), 38(1), and 33(1) cm^–1 for R = OMe, Cl, NO₂, and SMe₂, respectively. Taken together, these results provide the first examination of how bridging ligand substitution influences magnetic coupling in semiquinoid-bridged compounds, and they establish design criteria for the synthesis of semiquinoid-based molecules and materials.

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Research Organization:: Northwestern Univ., Evanston, IL (United States)

Sponsoring Organization:: USDOE Office of Science (SC); National Science Foundation (NSF)

Grant/Contract Number:: SC0019356; NNCI-1542205

OSTI ID:: 1803720

Journal Information:: Inorganic Chemistry, Vol. 59, Issue 7; ISSN 0020-1669

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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Heterospin single-molecule magnets with extra-large anisotropic barrier Yoshihara, Daisuke; Karasawa, Satoru; Koga, Noboru Polyhedron, Vol. 30, Issue 18 https://doi.org/10.1016/j.poly.2011.04.013	journal	November 2011
Cation exchange at the secondary building units of metal–organic frameworks Brozek, C. K.; Dincă, M. Chem. Soc. Rev., Vol. 43, Issue 16 https://doi.org/10.1039/C4CS00002A	journal	January 2014
Conductivity, Doping, and Redox Chemistry of a Microporous Dithiolene-Based Metal−Organic Framework Kobayashi, Yoji; Jacobs, Benjamin; Allendorf, Mark D. Chemistry of Materials, Vol. 22, Issue 14 https://doi.org/10.1021/cm101238m	journal	July 2010
Magnetic Properties of the Dicationic Iron o-Quinone Complexes with the Pyridinophane Ligands: A Quantum Chemical Study Starikov, A. G.; Chegerev, M. G.; Starikova, A. A. Russian Journal of Coordination Chemistry, Vol. 45, Issue 10 https://doi.org/10.1134/S1070328419090082	journal	October 2019
High-spin molecules based on metal complexes of organic free radicals Vostrikova, Kira E. Coordination Chemistry Reviews, Vol. 252, Issue 12-14 https://doi.org/10.1016/j.ccr.2007.08.024	journal	July 2008
Characterization of the Chloranilate(•3−) π Radical as a Strong Spin-Coupling Bridging Ligand Min, Kil Sik; Rheingold, Arnold L.; DiPasquale, Antonio Inorganic Chemistry, Vol. 45, Issue 16 https://doi.org/10.1021/ic061076k	journal	August 2006

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Quinoxaline radical-bridged transition metal complexes with very strong antiferromagnetic coupling Alexandropoulos, Dimitris I.; Vignesh, Kuduva R.; Xie, Haomiao Chemical Communications, Vol. 56, Issue 64 https://doi.org/10.1039/d0cc03713c	journal	January 2020
Dinuclear Ru ^II complexes with quinonoid bridges: tuning the electrochemical and spectroscopic properties of redox-switchable NIR dyes through judicious bridge design Chandra, Shubhadeep; Weisser, Fritz; Klenk, Sinja Dalton Transactions, Vol. 49, Issue 24 https://doi.org/10.1039/d0dt01351j	journal	January 2020

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37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
Chemistry
Redox reactions
Ligands
Substituents
Magnetic properties
Quantum mechanics

CCDC 1926459: Experimental Crystal Structure Determination E., Thorarinsdottir, Agnes; Ragnar, Bjornsson,; David, Harris, T. https://doi.org/10.5517/ccdc.csd.cc22nmv7 The current record is supplemented by this dataset	dataset	January 2020
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Title: Insensitivity of Magnetic Coupling to Ligand Substitution in a Series of Tetraoxolene Radical-Bridged Fe2 Complexes

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