Abstract
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+^/H~3~L were investigated. The HT‐study led to five new compounds Pb~2~[(O~3~P‐C~6~H~4~‐SO~3~)(OH)] (1), Cu~1.5~[(O~3~P‐C~6~H~4~‐SO~3~)(H~2~O)] (2), NaCu(O~3~P‐C~6~H~4~‐SO~3~)(H~2~O)~3~ (3), Cu~2~[(O~3~P‐C~6~H~4~‐SO~3~)(OH)(H~2~O)] (4) and Cu~3~[(O~3~P‐C~6~H~4~‐SO~3~)~2~(H~2~O)~2~] (5). Metal ion screening showed lead(II) and copper(II) to be suitable metal ions. The utilization of discovery and focused arrays allowed to determine the optimal formation fields of the respective compounds. The crystal structures were determined from single‐crystal X‐ray diffraction and revealed the presence of various MO__~x~__ polyhedra that form clusters, chains or layers which are connected through the organic linker. IR spectra, thermogravimetric studies, magnetic susceptibility measurements and elemental analyses were conducted to further characterize the compounds 1, 3, 4 and 5.