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A new tetrairon(III) single-molecule magnet with enhanced volatility and processability was obtained by partial fluorination of the ancillary β-diketonato ligands. Fluorinated proligand Hpta = pivaloyltrifluoroacetone was used to assemble the bis(alkoxido)-bridged dimer [Fe₂(OEt)₂(pta)₄] (1) in crystalline form, from which the new tetranuclear complex [Fe₄(L)₂(pta)₆] (2) was synthesized in a one-pot reaction with H₃L = 2-hydroxymethyl-2-phenylpropane-1,3-diol, NaOEt, and FeCl₃ in a Et₂O:EtOH solvent mixture. The structure of compound 2 was inferred from ¹H NMR, mass spectrometry, magnetic measurements, and DFT calculations. Direct current magnetic data are consistent with the expected metal-centered triangular topology for the iron(III) ions, with an antiferromagnetic coupling constant J = 16.20(6) cm^–1 between the central iron and the peripheral ones and consequent stabilization of an S = 5 spin ground …