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Poorly soluble in the most part of organic solvents dimeric complexes   $${\text{M}}{{{\text{g}}}_{{\text{2}}}}{\text{L}}_{2}^{2}$$  ·4DMF ( I ) and   $${\text{N}}{{{\text{i}}}_{{\text{2}}}}{\text{L}}_{2}^{2}$$  ·4DMF ( II ) (L is 4,4'-(1,4-phenylenebis(azanylylidene))bis(3,6-di- tert -butyl-2-hydroxycyclohexa-2,5-dien-1-one dianion)) are synthesized by the reactions of magnesium and nickel acetates with the ditopic redox-active ligand of the hydroxy- para- iminoquinone type in a DMF solution. The molecular and crystal structures of the synthesized compounds are determined by X-ray diffraction analysis (CIF files CCDC nos. 2045665 ( I ) and 2045666 ( II ·3DMF)). The thermal stability is studied by thermogravimetry. The redox-active character of the organic bridging ligand in the dimeric complexes   $${\text{M}}{{{\text{g}}}_{{\text{2}}}}{\text{L}}_{2}^{2}$$  ·4DMF and   $${\text{N}}{{{\text{i}}}_{{\text{2}}}}{\text{L}}_{2}^{2}$$  ·4DMF is confirmed by the data of solid-phase electrochemistry.

Magnesium and Nickel Complexes with Bis(p-iminoquinone) Redox-Active Ligand