We synthesized and characterized the ligand N,N'-bis[(2,2'-dihydroxybiphen-3-yl)methyl]-N,N'-dimethylethylenediamine (L), which contains two biphenol moieties linked as side arms to an dimethylethylenediamine scaffold. The ligand is highly soluble in a 50/50 (v/v) water/ethanol mixture and, in its deprotonated form H-2L2-, is able to coordinate transition-metal ions such as Ni-II, Z(II), Cu-II, Cd-II, and Pd-II. The crystal structures of [Ni(H-2L)center dot 2n-BuOH], [Ni(H-2L)center dot 2MeOH], [Cd-(H-2L)center dot 2DMF], [Cu(H-2L)(DMF)], and [Pd(H-2L)(DMF)] were also determined and described. Potentiometric titrations were carried out in a mixed solvent with Zn-II, Cu-II, and Ni-II metal ions to determine the acid-base and stability constants. L was highly fluorescent in the visible range (400 nm). Moreover, its emission intensity increased upon the addition of Zn-II or Cd-II ions in an ethanol/water solution and behaved as a chemosensor for the presence of these ions in the solution.