The ligand design factors that may influence the isolation of metallosupramolecular helicates or mesocates still deserve to be investigated. In this sense, dinuclear nickel( ii ), copper( ii ) and zinc( ii ) compounds were obtained by electrochemical synthesis using a family of five Schiff base ligands, H 2 L n ( n = 1-5), derived from bisphenylmethane and functionalized with bulky tert -butyl groups in the periphery and ethyl groups in the spacer. Six of the new complexes were characterized by X-ray crystallography, thus demonstrating that the helicate structure is predominant in the solid state. 1 H NMR studies were performed for the zinc complexes to analyze if the helical architecture of the metal complexes is retained in solution. These studies reveal that the presence of a tert -butyl group in the ortho position with respect to the OH group is an essential factor identified for the existence of a helicate conformation in solution. The number and position of bulky groups in the skeleton of the ligand precursor influence whether helicates or mesocates are obtained.