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• 作者：Sebastian Bauer ; Thomas Bein ; Norbert Stock
• 关键词：Cadmium ; Combinatorial chemistry ; Crystal structure ; High-throughput methods ; Inorganic– ; organic hybrid compounds ; Metal phosphonates
• 刊名：Solid State Sciences
• 出版年：2008
• 出版时间：July 2008
• 年：2008
• 卷：10
• 期：7
• 页码：837-846
• 全文大小：5683 K

文摘

High-throughput (HT) methods in materials synthesis enable fast and systematic investigations of parameter space – compositional as well as process parameters – while consuming only small amounts of starting materials. We have developed a new work-up tool, a 48-parallel-filtration device, which was integrated into our HT methodology for the investigation of solvothermal reactions. Employing HT methods, we have studied the system CdCl₂/(H₂O₃PCH₂)₂N–CH₂C₆H₄–COOH (H₅L)/NaOH leading to the discovery of four new compounds Cd[(HO₃PCH₂)₂N(H)–CH₂C₆H₄–COOH]₂ (1), Cd(H₂O)[H(O₃PCH₂)₂N(H)–CH₂C₆H₄–COOH] (2), Cd₂[(O₃PCH₂)₂N–CH₂C₆H₄–COOH]·3H₂O (3), and Cd₃(OH)[(O₃PCH₂)₂N–CH₂C₆H₄–COO]·4.5H₂O (4). The structures of 1 and 2 could be elucidated from laboratory X-ray powder diffraction data. All four title compounds were characterized using XRD, IR spectroscopy, as well as elemental, EDX, and thermogravimetric analyses. The pH of the starting mixture has a decisive influence on the product formation. Increasing amounts of NaOH lead to a gradual deprotonation of H₅L and therefore an increasing molar ratio of Cd²⁺:ligand in the reaction products.