| Resumo: | The solvothermal reaction between FeCl3·6H2O, NiCl2·6H2O, 2‐hydroxynaphthaldehyde, and glycine (gly) in MeOH results in the formation of the trinuclear heterometallic cluster [FeΙΙΙ2NiΙΙ(L1)4(MeOH)4] (1) in good yield, while the same reaction upon replacing gly with methyl‐alanine (mAla), results in the formation of the closely related quasi 1D coordination polymer {[FeΙΙΙ2NiΙΙ(L2)4(MeOH)2]n} (2) (L1, L2: the dianionic form of the Schiff‐base ligand derived from the condensation of 2‐hydroxynaphthaldehyde and gly (L1 for 1), or mAla (L2 for 2)). The structure of 1 describes a linear trimetallic {FeIII2Ni} unit, whereas complex 2 consists of repeating linear {FeIII2Ni} units with each one connected to two neighboring units via four coordination bonds, forming a quasi‐1D chain. The structural similarity between complex 1 and the repeating unit of complex 2 is remarkable. However, their magnetic properties differ significantly, with complex 1 displaying dominant ferromagnetic interactions, and complex 2 showing antiferromagnetic interactions.
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