Solvothermal Synthesis, Crystal Structure, and Properties of the New Oxothiomolybdate Ni(dien)2[Mo2O2S6] |
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Authors: | Jan Ellermeier Wolfgang Bensch |
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Institution: | Institut für Anorganische Chemie der Christian-Albrechts-Universit?t Kiel, D-24098 Kiel, Germany, DE
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Abstract: | Summary. The reaction of NiCl2 · 6H2O, Na2MoO4 ċ 2H2O, and sulfur in a mixture of diethylenetriamine and 0.2 M ammonia solution (1:4) under solvothermal conditions leads to the formation of orange-red crystals of the oxothiomolybdate
Ni(dien)2Mo2O2S6] (dien = diethylenetriamine) in nearly 100% yield. The structure consists of Ni(dien)2]2+ cations and discrete dimeric Mo2O2S6]2− anions. The compound crystallizes in the monoclinic space group P21/c (a = 8.726(2), b = 18.111(4), c = 14.419(3) ?, β = 101.686(3)°). Upon heating the compound decomposes in a single step starting at about 250°C. The final
decomposition product was identified by X-ray powder diffractometry as MoS2 and Ni3S2. Spectroscopic data as well as detailed synthetic procedures for Ni(dien)2Mo2O2S6] are reported.
Received November 6, 2000. Accepted November 17, 2000 |
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Keywords: | , ,Thiomolybdates, Solvothermal synthesis, Crystal structure, Physical properties, |
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