Premium
Complex Hydrothermal Reaction Systems: A Systematic Investigation of Copper Phosphonatoethanesulfonates by High‐Throughput Methods
Author(s) -
Sonnauer Andreas,
Stock Norbert
Publication year - 2008
Publication title -
european journal of inorganic chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.667
H-Index - 136
eISSN - 1099-0682
pISSN - 1434-1948
DOI - 10.1002/ejic.200800315
Subject(s) - chemistry , hydrothermal circulation , copper , ligand (biochemistry) , molar ratio , crystallography , crystal structure , hydrothermal synthesis , hydrothermal reaction , nuclear chemistry , stereochemistry , catalysis , organic chemistry , chemical engineering , biochemistry , receptor , engineering
The polyfunctional ligand 2‐phosphonoethanesulfonic acid, H 2 O 3 P–C 2 H 4 –SO 3 H (H 3 L ), was used in a high‐throughput (HT) investigation of a new class of compounds, the copper phosphonatosulfonates. An extensive HT study comprising 288 individual hydrothermal reactions was performed to systematically investigate the influence of temperature, pH, and molar ratio of Cu 2+ /H 3 L in the reaction system Cu(NO 3 ) 2 /H 3 L /NaOH/H 2 O/temperature. The HT investigation led to five new compounds Cu 2 [(O 3 P–C 2 H 4 –SO 3 )(OH)(H 2 O)](H 2 O) ( 1 ), Cu 2.5 (O 3 P–C 2 H 4 –SO 3 )(OH) 2 ( 2 ), Cu 1.5 [(O 3 P–C 2 H 4 –SO 3 )(H 2 O)] · H 2 O ( 3 ), Cu 2 [(O 3 P–C 2 H 4 –SO 3 )(OH)(H 2 O) 2 ] · 3H 2 O ( 4 ), and NaCu(O 3 P–C 2 H 4 –SO 3 )(H 2 O) 3 ( 5 ). Their fields of formation were established unequivocally and from the large amount of data reaction trends were extracted. Furthermore, a new compound Cu 1.5 (O 3 P–C 2 H 4 –SO 3 )(H 2 O) ( 6 ) was synthesized under hydrothermal reaction conditions in a glass reactor. For compounds 1 , 2 , and 6 crystal structures were determined by single‐crystal X‐ray diffraction. The compounds exhibit a large structural variety. Thus, CuO 4 , CuO 5 , and CuO 6 units are observed. Corner‐, edge‐ as well as face‐sharing polyhedra form chains, layers, or Cu 3 O 12 clusters that are connected by the –CH 2 CH 2 – group of the ligand. Thermogravimetric investigations, magnetic measurements, IR spectra as well as chemical analyses of compounds 1 , 3 , 4 , 5 , and 6 are also presented.(© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2008)