New members of the Mn and Mn torus-like cluster family have been prepared from a hybrid comproportionation-alcoholysis reaction of [MnO(OCR)(HO)] in alcohol in the presence of R'COH with NBuMnO or Mn salts as initiators. Reactions using MeCOH in PrOH or BuOH gave [MnO(OCMe)(OPr)(PrOH)(HO)] () and [MnO(OCMe)(OH)(OBu)(BuOH)(HO)] (), respectively, whereas EtCOH in PrOH gave [MnO(OCEt)(OPr)(PrOH)(HO)] (). They consist of alternating near-linear [Mn(μ-O)] and distorted-cubane [Mn(μ-O)(μ-OR)] units bridged by syn,syn-μ-RCO and μ-O groups and overall are [Mn] and [Mn] oligomers, the repeating unit containing two Mn and two Mn units. // possess external diameters (including organic ligands) of 4.0/4.1/4.6 nm, respectively, and crystallize as supramolecular nanotubes but with different packing arrangements. Considering all Mn/Mn tori now available, we conclude that the Mn vs Mn nuclearity is determined by the relative bulk of the carboxylates vs the alkoxides, their increasing bulk favoring Mn and Mn, respectively, with carboxylates larger than acetate giving Mn. Alternating current (ac) magnetic susceptibility studies revealed frequency-dependent χ signals below ∼2.4 K, indicating to be new members of the giant [Mn] torus family of giant single-molecule magnets (SMMs), in which Mn and Mn are the largest homometallic Mn/O clusters and SMMs to date.
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