Präparation und Charakterisierung neuer Halogenopalladate mit besonderem Schwergewicht bezüglich mehrkerniger Halogenopalladatgruppen
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Date
2000-05-11
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Universität Dortmund
Abstract
Diese Dissertation beschäftigt sich mit der Präparation und Charakterisierung neuer ternärer Halogenopalladate und den Verknüpfungsprinzipien von ([PdX4]2-)-Baugruppen (X = Cl, Br, I) zu neuartigen mehrkernigen komplexen Anionen. Die Kristallstrukturen der größtenteils durch Solvothermalsynthese dargestellten Verbindungen wurden mittels Röntgenbeugungsuntersuchungen an Pulvern und Einkristallen ermittelt. Die weitere Charakterisierung der Halogenopalladate erfolgte mit schwingungsspektroskopischen und thermoanalytischen Methoden. Als mehrkernige Halogenopalladatgruppen wurden [Pd2X6]2- (X = Cl, Br), [Pd3X8]2- (X = Br, I), sowie [(PdCl2Cl2/2)4]4- erhalten.
Besonders hervorzuheben sind die Ergebnisse in den Systemen CsI/PdI2 und RbI/PdI2. Durch Bildung von Verbindungen mit gleichen Summenformeln - M2PdI4 · I2 und M2PdI6 (M = Rb, Cs) - stellen diese Modellsysteme zum Studium von Redoxreaktionen im Festkörper dar. Energiedispersive Röntgenbeugungsuntersuchungen mit Synchrotronstrahlung zeigen den Reaktion von Cs2PdI4 · I2 durch Anwendung von Druck zu Cs2PdI6.
This PhD-thesis reports on the preparation and characterization of new ternary halogenopalladates and the connectivity principles of ([PdX4]2-)-building units to novel polynuclear complex anions. The compounds were mainly obtained by solvothermal syntheses and their crystal structures determined via X-ray diffraction on powders and single crystals. For the further characterization spectroscopic and thermal analytic techniques were employed. The polynuclear halogenopalladate anions obtained were [Pd2X6]2- (X = Cl, Br), [Pd3X8]2- (X = Br, I), and [(PdCl2Cl2/2)4]4-. Remarkable are the results on the systems CsI/PdI2 and RbI/PdI2. Compounds with identical formula sums - M2PdI4 · I2 and M2PdI6 (M = Rb, Cs) - are utilized as models to study redox reactions in solid state. Energy disperse X-ray diffraction with synchrotron radiation proves the pressure induced reaction of Cs2PdI4 · I2 to Cs2PdI6.
This PhD-thesis reports on the preparation and characterization of new ternary halogenopalladates and the connectivity principles of ([PdX4]2-)-building units to novel polynuclear complex anions. The compounds were mainly obtained by solvothermal syntheses and their crystal structures determined via X-ray diffraction on powders and single crystals. For the further characterization spectroscopic and thermal analytic techniques were employed. The polynuclear halogenopalladate anions obtained were [Pd2X6]2- (X = Cl, Br), [Pd3X8]2- (X = Br, I), and [(PdCl2Cl2/2)4]4-. Remarkable are the results on the systems CsI/PdI2 and RbI/PdI2. Compounds with identical formula sums - M2PdI4 · I2 and M2PdI6 (M = Rb, Cs) - are utilized as models to study redox reactions in solid state. Energy disperse X-ray diffraction with synchrotron radiation proves the pressure induced reaction of Cs2PdI4 · I2 to Cs2PdI6.
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Halogenopalladate, Ternäre Verbindungen, Solvothermalsynthese, Kristallstruktur, Mehrkernige Halogenopalladatgruppen, Druckinduzierte Redoxreaktion, halogenopalladates, ternary compounds, solvothermal synthesis, crystal structure, polynuclear halogenopalladate groups, pressure induced redox-reaction