Trinuclear μ-oxo-centered iron(III) isobutyrate clusters readily react with polyalcohol organic ligands under one-pot synthesis conditions. Depending on the ligand, solvent, and temperature, a range of hexa-, dodeca-, and doicosanuclear iron(III) oxo-hydroxo condensation products, isolated as (mdeaH)[FeO(thme)Cl]·0.5(MeCN)·0.5(HO) (1), [FeO(OH)(teda)(N)(MeO)]N(NO)(MeO)·2.5(HO) (2), [FeO(teda)Cl]·6(CHCl) (3), [FeO(OH)(OCCHMe)(bdea)(EtO)(HO)]·2(EtOH)·5(MeCN)·6(HO) (4), and [FeO(OH)(OCCHMe)(mdea)(EtO)(HO)](NO)·EtOH·HO (5), where tedaH = N, N, N', N'-tetrakis(2-hydroxyethyl)ethylenediamine; thmeH = 1,1,1-tris(hydroxymethyl)ethane; mdeaH = N-methyldiethanolamine; and bdeaH = N-butyldiethanolamine. Complete carboxylate metathesis in the {Fe} precursor complexes by thme or teda and the agglomeration of the formed species under solvothermal conditions afforded carboxylate-free {Fe} product (1) in MeCN/CHCl or {Fe} complexes (2 and 3) in MeOH/EtOH and CHCl/thf, respectively (thf = tetrahydrofuran). Single-crystal X-ray diffraction analyses revealed that 1 contains a [FeO(thme)Cl] cluster anion with a Lindqvist-type {Fe(μ-O)} core motif, charge-compensated by two protonated mdeaH cations. 2 comprises a [FeO(OH)(teda)(N)(MeO)] cation with a {FeO(OH)} core, whereas 3 contains a charge-neutral [FeO(teda)(Cl)] complex with an {FeO} core. Finally, employing flexible bdeaH or mdeaH ligands under soft reaction conditions afforded giant {Fe} oxo-hydroxo complexes (4 and 5) with a central {Fe} layer sandwiched between two outer {Fe} groups. Magnetic studies of 1-5 revealed strong antiferromagnetic coupling between the Fe spin centers in all clusters.
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