| Summary: | Tetranuclear hetero-metal Mn<sup>III</sup><sub>2</sub>Ni<sup>II</sup><sub>2</sub> complexes, [Mn<sub>2</sub>Ni<sub>2</sub>(L)<sub>4</sub>(OAc)<sub>2</sub>] (<b>1</b>) and [Mn<sub>2</sub>Ni<sub>2</sub>(L)<sub>4</sub>(NO<sub>3</sub>)<sub>2</sub>] (<b>2</b>) [H<sub>2</sub>L = <i>N</i>-(2-hydroxymethylphenyl)-5,6-benzosalicylideneimine], have been synthesized and characterized by X-ray crystal structure analyses, infrared spectra, and elemental analyses. The structure analyses revealed that the complexes have a defective double-cubane metal core connected by μ<sub>3</sub>-alkoxo bridges. Complexes consist of two bis-μ-alkoxo bridged Mn<sup>III</sup>Ni<sup>II</sup> heteronuclear units making a dimer-of-dimers structure. The double-cubane cores are significantly distorted due to an effect of <i>syn–syn</i> mode acetato or nitrato bridges. Magnetic measurements indicate that weak antiferromagnetic interactions (Mn-Ni = −0.66 ~ −4.19 cm<sup>–1</sup>) are dominant in the hetero-metal core.
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