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Preparation, characterization, and X-ray structure analysis of diethylenetriammonium tetrathiomolybdate

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Abstract

The interaction of H2S gas with aqueous ammonium heptamolybdate solution in the presence of diethylenetriamine (dien) led to the formation of diethylenetriammonium tetrathiomolybdate crystals. The elemental analyses, UV-Visible, IR, and 1H NMR spectra suggested the presence of organic cation and (MoS4)2− moiety. The 1H NMR revealed the presence of two sets of symmetrical A2X2 multiple patterns. The compound crystallizes in the monoclinic system with space group Pn, a = 7.196(6), b = 7.532(3), c = 11.525(10) Å, α = 90°, β = 90.17(3)°, γ = 90°, V = 624.78(8) Å3, and Z = 2, wR 1 = 0.0261 and wR 2 = 0.0698. The structure consists of tetrahedral tetrathiomolybdate anions, which form an extended three-dimensional network in the solid state with Mo–S⋅⋅⋅H–N hydrogen bonding with the organic cation.

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Correspondence to K. S. Nagaraja.

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Pokhrel, S., Nagaraja, K.S. & Varghese, B. Preparation, characterization, and X-ray structure analysis of diethylenetriammonium tetrathiomolybdate. Journal of Chemical Crystallography 33, 903–908 (2003). https://doi.org/10.1023/A:1027470115878

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