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Inorganics 2018, 6(3), 66; https://doi.org/10.3390/inorganics6030066

Synthesis, Structural, and Magnetic Characterization of a Mixed 3d/4f 12-Metallacrown-4 Family of Complexes

1
Institute of Inorganic and Analytical Chemistry, Johannes Gutenberg University Mainz, Duesbergweg 10-14, D-55128 Mainz, Germany
2
Graduate School Materials Science in Mainz, Staudinger Weg 9, D-55128 Mainz, Germany
*
Author to whom correspondence should be addressed.
Received: 21 June 2018 / Revised: 2 July 2018 / Accepted: 5 July 2018 / Published: 7 July 2018
(This article belongs to the Special Issue Organometallic Macrocycles and Their Applications)
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Abstract

A new family of complexes (tBu4N){[LnIII(O2CBut)4][12-MC-Mn(III)N(shi)-4]}·5CH2Cl2 (Ln = Gd (1) and Tb (2)), (tBu4N)2{[YIII(O2CBut)4][12-MC-Mn(III)N(shi)-4]}(ClO4) (3); where shiH3 = salicylhydroxamic acid; ButCO2 = pivalate ions; tBu4N = tetrabutylammonium and ClO4 = perchlorate ions, has been isolated. The reaction of salicylhydroxamic acid with Mn(O2CBut)2·2H2O, Ln(NO3)3·xH2O, tBu4NClO4 in the presence of morpholine (C4H9NO) led to the isolation of compounds 13. The complexes belong to the 12-MC-4 family of Metallacrowns (MCs) possessing a central {Mn4IIILnIII(µ-NO)4}11+ core with the four MnIII atoms occupying the periphery positions, while the formed [Mn–N–O] repeating unit, assists in the accommodation of the LnIII atom in the center of the ring. Peripheral ligation is provided by four η11:μ pivalate ions. Direct current magnetic susceptibility (dc) measurements revealed the presence of predominant antiferromagnetic exchange interactions within the metal centers. A 1-J fitting model was used in order to quantify the MnIII–MnIII interactions and fitting of the data, for the diamagnetic YIII analogue, gave J = −3.74 cm−1 and gMn(III) = 2.07. Fitting of the {Mn4Gd} compound using a 2-J model, counting additionally for the MnIII–GdIII interactions, revealed values of J1 = −3.52 cm−1, J2 = −0.45 cm−1, and gMn(III) = 1.99. View Full-Text
Keywords: metallacrowns; single-molecule magnets (SMMs); heterometallic complexes; inorganic synthesis; coordination chemistry metallacrowns; single-molecule magnets (SMMs); heterometallic complexes; inorganic synthesis; coordination chemistry
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Athanasopoulou, A.A.; Carrella, L.M.; Rentschler, E. Synthesis, Structural, and Magnetic Characterization of a Mixed 3d/4f 12-Metallacrown-4 Family of Complexes. Inorganics 2018, 6, 66.

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