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Updated: Jun 30, 2026
Magnetometric Characterization of Intermediates in the Solid-State Electrochemistry of Redox-Active Metal-Organic Frameworks
Published on: June 9, 2023
From a paramagnetic, mononuclear supersulfidonickel(II) complex to a diamagnetic dimer with a four-sulfur
Shenglai Yao1, Carsten Milsmann, Eckhard Bill
1Metalorganics and Inorganic Materials, Institute of Chemistry, Technische Universität Berlin, Strasse des 17, Juni 135, Sekr. C2, D-10623 Berlin, Germany.
Abstract:
The first isolable "side-on" supersulfidonickel(II) complex 1(1) with the elusive S2-. ligand has been synthesized by facile oxidation of the corresponding nickel(I) precursor [LNi] with elemental sulfur. Remarkably, paramagnetic 1(1) associates voluntarily to give the diamagnetic dimer 1(2) with a four-sulfur two-electron bond as proven by X-ray diffraction analysis, spectroscopic measurements (1H NMR, EPR, SQUID), and DFT calculations. Gentle sulfur transfer of 1(1) to Ph3P or its reaction with [LNi] affords solely the genuine disulfide complex 3 having a Ni2(mu-mu2:mu2-S2) core.
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