A high-throughput (HT) investigation using the rigid bifunctional ligand 4-phosphonobenzenesulfonic acid, H 2 O 3 P-C 6 H 4 -SO 3 H (H 3 L), generated five new phosphonatobenzenesulfonates with copper(II) or lead(II) ions. A comprehensive HT study comprising the screenings of different metal ions, metal salt types and the synthesis optimization were conducted whereby the influence of pH and molar ratios M 2+