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Crystal Structure of Hexafluosilicates of Protonated Thiosemicarbazide and 2,5-Diamino-1,3,4-thiadiazole Produced in the Reaction of Thiosemicarbazide with Fluosilicic Acid

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Abstract

The structure of the crystal complex (L1H)2(L2H)(SiF6)1.5(L1is thiosemicarbazide, L2is 2,5-diamino-1,3,4-thiadiazole) was studied by X-ray diffraction analysis. The complex was prepared by reacting an aqueous solution of L1with 45% fluosilicic acid. The crystals are monoclinic: a= 16.080(3) Å, b= 5.4860(8) Å, c= 20.079(4) Å, β = 91.46(1)°, Z= 4, space group P2/n, R= 0.0427. The components of the ionic structure of the complex are L1H+and L2H+cations and SiF2– 6anions combined by a system of H bonds of the NH···S and NH···F types, the β-nitrogen atom of the hydrazine fragment and the endocyclic nitrogen atom of the heterocycle being the protonation centers in L1H+and L2H+, respectively. The bond lengths in the SiF2– 6anions range within 1.621(6)–1.691(2) Å.

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Gel'mbol'dt, V.O., Ilyukhin, A.B., Ganin, E.V. et al. Crystal Structure of Hexafluosilicates of Protonated Thiosemicarbazide and 2,5-Diamino-1,3,4-thiadiazole Produced in the Reaction of Thiosemicarbazide with Fluosilicic Acid. Russian Journal of Coordination Chemistry 27, 537–541 (2001). https://doi.org/10.1023/A:1011345626840

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