| Summary: | A new tetradentate mixed aza-thioether macrocyclic ligand 2,6-dithia[7](2,9)-1,10-phenanthrolinophane ([13]ane(phenN<sub>2</sub>)S<sub>2</sub>) was successfully synthesized. Reacting metal precursors [Fe(CH<sub>3</sub>CN)<sub>2</sub>(OTf)<sub>2</sub>], Ni(ClO<sub>4</sub>)<sub>2</sub>·6H<sub>2</sub>O, and Cu(ClO<sub>4</sub>)<sub>2</sub>·6H<sub>2</sub>O with one equivalent of [13]ane(phenN<sub>2</sub>)S<sub>2</sub> afforded [Fe([13]ane(phenN<sub>2</sub>)S<sub>2</sub>)(OTf)<sub>2</sub>] (<b>1</b>), [Ni([13]ane(phenN<sub>2</sub>)S<sub>2</sub>)](ClO<sub>4</sub>)<sub>2</sub> (<b>2</b>(ClO<sub>4</sub>)<sub>2</sub>), and [Cu([13]ane(phenN<sub>2</sub>)S<sub>2</sub>)(OH<sub>2</sub>)](ClO<sub>4</sub>)<sub>2</sub> (<b>3</b>(ClO<sub>4</sub>)<sub>2</sub>), respectively. The structures of [13]ane(phenN<sub>2</sub>)S<sub>2</sub> and all of its metal complexes were investigated by X-ray crystallography. The [13]ane(phenN<sub>2</sub>)S<sub>2</sub> was found to behave as a tetradentate ligand via its donor atoms N and S.
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