Cube‐like 12‐MC‐4 and Offset Stacked 10‐MC‐3 Metallacrowns: Synthesis, Structure, and Magnetic Properties

Two complexes [Mn III 4 (naphthsao) 4 (naphthsaoH) 4 ] ( 1 ) and [Fe III 6 O 2 (naphthsao) 4 (O 2 CPh) 6 ] ( 2 ) [naphthsao = 1‐(1‐hydroxy‐naphthalen‐2‐yl)ethanone oxime] were obtained through the reactions of naphthsao ligand and MnCl 2 · 4H 2 O or FeCl 3 · 6H 2 O in the presence of triethylamine (Et 3 N). Their structures were determined by X‐ray single crystal diffraction, elemental analysis, and IR spectra. Complex 1 displays 12‐MC‐4 metallacrown structural type with cube‐like configuration and 2 shows an offset stacked 10‐MC‐3 structural type with the ring connectivity containing Fe–O–C–O–Fe–O–N–Fe–O–N. Magnetic susceptibility measurement reveals the ferromagnetic interactions and field‐induced slow relaxation of the magnetization for 1 , whereas out‐of‐phase signal is not observed for 2 .