Air-Stable, Well-SolubleAI2[Nb6Cl18] Cluster Compounds (AI= Organic Cation): A New Route for Preparation, Single-Crystal Structures, Properties, and ESI-Mass Spectra
| Autor: | Ina Dartsch, Eva Guillamón, Jonas König, Rosa Llusar, Martin Köckerling, Anke Topp |
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| Rok vydání: | 2016 |
| Předmět: |
Dehydration
010405 organic chemistry Chemistry Niobium Inorganic chemistry ESI-MS 010402 general chemistry 01 natural sciences Chloride 0104 chemical sciences Inorganic Chemistry Solvent Crystallography chemistry.chemical_compound Thionyl chloride Solubility Cluster Mass spectrum medicine Cluster (physics) Molecule Single crystal medicine.drug |
| Zdroj: | Zeitschrift für anorganische und allgemeine Chemie. 642:572-578 |
| ISSN: | 0044-2313 |
| DOI: | 10.1002/zaac.201600039 |
| Popis: | Five niobium cluster compounds of the AI2[Nb6Cl18] type (AI = organic cation: [nPr4N]+, [nBu4N]+, [BMIm]+, [Ph4P]+, and [PPN]+) are obtained through treatment of [Nb6Cl14(H2O)4]·4H2O with excess of thionyl chloride in the presence of an organic chloride, AICl. Single-crystal structure studies show that the compounds consist of discrete cations and cluster [Nb6Cl18]2– anions. The cluster unit of the hydrated cluster starting material is oxidized by two electrons. Powder diffraction studies and NMR spectroscopic measurements show all compounds to crystallize without co-crystallized solvent molecules. They are air and water stable. The solubility in organic solvents changes to a great extent on changing the type of cation. The ESI-MS spectra of [nPr4N]2[Nb6Cl18] and [Ph4P]2[Nb6Cl18] show the pseudomolecular peak of the anionic cluster as well as additional signals, which involve simultaneously chloride mass loss and reduction processes Financial support from the Deutsche Forschungsgemeinschaft (Priority Program SPP 1708, Material Synthesis near Room Temperature) is gratefully acknowledged. The financial support of the Universitat Jaume I (Research Project P1.1B2013–40) and Generalitat Valenciana (PrometeoII/2014/022) is gratefully acknowledged |
| Databáze: | OpenAIRE |
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