| Summary: | A mononuclear Ni(II) complex, [Ni(HL1)<sub>2</sub>], (<b>1</b>) and a novel tetranuclear heterometal Mn-Ni complex, [Mn<sub>3</sub>Ni(L1)<sub>4</sub>Cl<sub>2</sub>(EtOH)<sub>2</sub>], (<b>2</b>) [H<sub>2</sub>L1 = <i>N</i>-(2-hydroxymethylphenyl)salicylideneimine], have been synthesized and characterized via X-ray crystal structure analyses, infrared spectra, and elemental analyses. The structure analyses revealed that the tridentate ligand, H<sub>2</sub>L1, coordinates in a facial mode for Ni and a mer mode for Mn, respectively. Complex <b>2</b> includes Mn(II)Mn(III)<sub>2</sub>Ni(II) tetranuclear metal core bridged by μ-phenoxo and μ-alkoxo oxygens. Magnetic measurements for <b>2</b> indicate that weak ferromagnetic interactions (<i>J</i><sub>Mn(III)Ni(II)</sub> = 2.23, <i>J</i><sub>Mn(III)Mn(II)</sub> = 0.46, <i>J</i><sub>Mn(II)Ni(II)</sub> = 1.78, and <i>J</i><sub>Mn(III)Mn(III)</sub> = 0.58 cm<sup>−1</sup>) dominate in the tetranuclear core. Additionally, in alternating current (AC) magnetic measurements, frequency-dependent out-of-phase responses were observed.
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