Synthesis and Complexation of a New 14‐Membered N 2 O 2 Macrocycle with vic ‐Dioxime Moieties

The new vic ‐dioxime ligand 2 (LH 4 ) carrying a 14‐membered N 2 O 2 macrocycle has been prepared. Mononuclear complex (LH 3 ) 2 Ni, trinuclear complexes (LH) 2 Cu 3 , (LH) 2 Co 3 , (LH) 2 ‐Pd 3 , and (LH) 2 Co 3 (py) 3 Cl 3 , dinuclear complex (LH 3 ) 2 ‐(UO 2 ) 2 (OH) 2 , and pentanuclear complex [L 2 Cu 5 (phen) 2 ]‐(NO 3 ) 2 have been synthesized from LH 4 . The electrochemical properties of tri‐ and pentanuclear complexes were investigated by cyclic voltammetry. For (LH) 2 Cu 3 two reduction waves appeared at 0.215 and ‐0.870 V. [L 2 Cu 5 (phen) 2 ](NO 3 ) 2 exhibited four reduction waves at 0.200, ‐0.025, ‐0.670, and ‐1.170 V.