Systematic Hydrothermal Investigation of Metal Phosphonatobenzenesulfonates by High‐Throughput Methods

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+

Bismuth Tri‐ and Tetraarylcarboxylates: Crystal Structures, In Situ X‐ray Diffraction, Intermediates and Luminescence

“…High‐throughput (HT) methods allow the systematic and efficient investigation of parts of this complex parameter space 17. 18 Thus, these methods have been used for the systematic study of the influence of the pH,19–22 temperature,23, 24 linker geometry and size,25, 26 concentration21, 22 or ionic radii 27. In addition to the discovery of new compounds, the systematic variation of synthesis parameters allowed synthesis–structure relationships to be established.…”

“…[17,18] Thus, these methods have been used for the systematic study of the influence of the pH, [19][20][21][22] temperature, [23,24] linker geometry and size, [25,26] concentration [21,22] or ionic radii. [27] In addition to the discovery of new compounds, the systematic variation of synthesis parameters allowed synthesis-structure relationships to be established. Although HT methods are very valuable in finding new compounds, no information about crystallisation is obtained, and thus a deeper understanding of the processes leading to the final product is not possible.…”

Synthesis and Characterization of the Mixed‐Linker Copper(II) Coordination Polymer [Cu(HO3PC6H4SO3)(C10N2H8)]·H2O

“…The counterions of the copper salts affect the pH of the reaction mixture and can also induce in situ side‐reactions such as oxidation during the synthesis 18. In addition, the deployment of the suitable copper(II) salt could also prevent the co‐crystallization of unwanted phases 36. In a HT‐screening experiment with 24 individual reactions, other copper salts in addition to Cu(NO 3 ) 2 ·3H 2 O were tested with 4,4′‐ bipy under hydrothermal conditions (Tab.…”

“…Due to the large amounts of data, reaction and structural trends can be derived. Our recent work on 4‐phosphonobenzenesulfonic acid (H 3 L ) with HT methods has highlighted the discovery of several compounds incorporating this linker and Cu 2+ ions 36. Various CuO clusters ranging from mononuclear CuO 6 , binuclear Cu 2 O 8 , hexanuclear Cu 6 O 24 to infinite chains of edge‐sharing CuO 5 /CuO 6 were observed in these phosphonosulfonate compounds.…”

Five New Coordination Polymers with a Bifunctional Phosphonate‐Sulfonate Linker Molecule

“…acids [7][8][9][10][11][12][13][14][15][16][17][18] or rigid m-or p-phosphonobenzenesulfonic acid. [19][20][21][22][23][24][25][26][27][28][29][30][31][32][33][34] First studies on 2-phosphonoethanesulfonic and 4-phosphonobutanesulfonic acids were carried out in the group of Alberti et al [7] Subsequently, high-throughput investigations allowed to identify fields of product formation and to establish synthesis-structure relationships of a variety of new CPs. [9][10][11][12][13][14]16,17] In addition, in situ X-ray diffraction studies were carried out to study the crystallization process in detail.…”