Complexing of nickel(II) with 2,6-dimercapto-4-methylphenol (DMMP) and hydrophobic amines was studied using physicochemical methods. Hydroxyl-containing amines-aminophenols (AP) were used as a hydrophobic amine. On the part of aminophenols, 2 (N, N-dimethylaminomethyl) -4-methylphenol (AP1 ), 2 (N, N-dimethylaminomethyl)-4-chlorophenol (AP2 ), and 2 (N, N-dimethylaminomethyl) -4-bromophenol (AP3 ) were used. Mixed-ligand complexes were formed in a weakly acidic medium (pHopt 4.6–6.4).