Synthesis,properties and structural characterization of 4-(2-ammonioethyl)piperazin-1-ium tetrasulfidotungstate hemihydrate and 1-ethylpiperazinediium tetrasulfidotungstate |
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Authors: | Bikshandarkoil R Srinivasan Ashish R Naik Sunder N Dhuri Christian Näther Wolfgang Bensch |
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Institution: | 1. Department of Chemistry, Goa University PO, Goa 403 206, India;2. Institut für Anorganische Chemie, Christian-Albrechts-Universität Kiel, Max-Eyth Straße 2, D-24118 Kiel, Germany |
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Abstract: | The reaction of ammonium tetrasulfidotungstate with 2-piperazin-1-ylethanamine or 1-ethylpiperazine results in the formation of 4-(2-ammonioethyl)piperazin-1-ium tetrasulfidotungstate hemihydrate (C6H17N3)WS4]·½H2O 1 or 1-ethylpiperazinediium tetrasulfidotungstate (C6H16N2)WS4] 2. The hemihydrate 1 can be dehydrated to the anhydrous compound (C6H17N3)WS4] 1a, which can be rehydrated to 1. Both 1 and 2 decompose to amorphous carbon containing tungsten disulphide. Compound 1 crystallizes in the centrosymmetric monoclinic space group C2/c, while compound 2 crystallizes in the centrosymmetric orthorhombic space group Pbca. The structures of 1 and 2 consist of a slightly distorted tetrahedral WS4]2? anion and 4-(2-ammonioethyl)piperazin-1-ium (1) or 1-ethylpiperazinediium dication (2) and additionally a lattice water in 1. In the crystal structure of 1 and 2 the organic cation and the WS4]2? anion are linked to each other via several weak N–H?S and C–H?S bonding interactions. The lattice water serves as a link between pairs of cations and pairs of anions with the aid of O–H?S and N–H?O interactions in compound 1. |
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