Maximizing Electron Exchange in a [F 3] Cluster

Hernández Sánchez, Raúl; Bartholomew, Amymarie K.; Powers, Tamara M.; Ménard, Gabriel; Betley, Theodore A.

doi:10.1021/jacs.5b12181

Maximizing Electron Exchange in a [F ₃] Cluster

Journal Article · Fri Jan 22 00:00:00 EST 2016 · Journal of the American Chemical Society

DOI:https://doi.org/10.1021/jacs.5b12181· OSTI ID:1467658

Hernández Sánchez, Raúl ^[1]; Bartholomew, Amymarie K. ^[2]; Powers, Tamara M. ^[2]; Ménard, Gabriel ^[2]; Betley, Theodore A. ^[2]

Harvard Univ., Cambridge, MA (United States); Harvard University
Harvard Univ., Cambridge, MA (United States)

The one-electron reduction of (^tbsL)Fe₃(thf)¹ furnishes [M][(^tbsL)Fe₃] ([M]⁺ = [(18-C-6)K(thf)₂]⁺ (1, 76%) or [(crypt-222)K]⁺ (2, 54%)). Upon reduction, the ligand ^tbsL^6- rearranges around the triiron core to adopt an almost ideal C₃-symmetry. Accompanying the (^tbsL) ligand rearrangement, the THF bound to the neutral starting material is expelled, and the Fe–Fe distances within the trinuclear cluster contract by ~0.13 Å in 1. Variable-temperature magnetic susceptibility data indicates a well-isolated spin ground state that persists to room temperature. Slow magnetic relaxation is observed at low temperature as evidenced by the out-of-phase component of the alternating current (ac) magnetic susceptibility data and by the appearance of hyperfine splitting in the zero-field ⁵⁷Fe Mössbauer spectra at 4.2 K. Analysis of the ac magnetic susceptibility yields an effective spin reversal barrier (U_eff) of 22.6(2) cm^-1, nearly matching the theoretical barrier of 38.7 cm^-1 calculated from the axial zero-field splitting parameter (D = -1.29 cm^-1) extracted from the reduced magnetization data. A polycrystalline sample of 1 displays three sextets in the Mössbauer spectrum at 4.2 K (H_ext = 0) which converge to a single six-line pattern in a frozen 2-MeTHF glass sample, indicating a unique iron environment and thus strong electron delocalization. The spin ground state and ligand rearrangement are discussed within the framework of a fully delocalized cluster exhibiting strong double and direct exchange interactions.

View Accepted Manuscript (DOE)

Research Organization:: Harvard Univ., Cambridge, MA (United States)

Sponsoring Organization:: USDOE Office of Science (SC)

Grant/Contract Number:: SC0008313

OSTI ID:: 1467658

Journal Information:: Journal of the American Chemical Society, Journal Name: Journal of the American Chemical Society Journal Issue: 7 Vol. 138; ISSN 0002-7863

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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