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sodium thioantimoniate : ウィキペディア英語版
sodium thioantimoniate

Sodium thioantimoniate, also known as Schlippe's salt, is an inorganic compound with the formula Na3SbS4.9H2O. This sulfosalt is named after K. F. Schlippe (1799–1867). Sodium thioantimoniate is used to make "quinsulfide antimony," Sb2S5. This salt consists of the tetrahedral SbS43− anion (rSb-S = 2.33 Å) and sodium cations, which are hydrated.〔Krebs, B., "Thio- and Seleno Compounds of Main Group Elements - New Inorganic Oligomers and Polymers", Angewandte Chemie, 1983, volume 95, pages 113-34.〕〔K. Mereiter, A. Preisinger and H. Guth "Hydrogen bonds in Schlippe's salt: refinement of the crystal structures of Na3SbS4.9H2O by X-ray diffraction and Na3SbS4.9D2O by neutron diffraction at room temperature" Acta Crystallographica 1979, vol. B35, 19-25. .〕 Related salts are known for different cations including ammonium and potassium.
==Preparation==
Sodium thioantimoniate is prepared by the reaction of antimony trisulfide, elemental sulfur, and aqueous sulfide source.
:3 Na2S + 2 S + Sb2S3 + 9 H2O → 2 Na3SbS4·9 H2O
The sulfide can be generated indirectly by the thermal reaction of elemental sulfur with sodium hydroxide or even charcoal:
:Sb2S3 + 8 NaOH + 6 S → 2 Na3SbS4 + Na2SO4 + 4 H2O
In the latter route, a mixture of sodium sulfate (16 parts) is reduced by fusion with charcoal (4-5 parts) in the presence of antimony sulfide (13 parts). The melt is extracted into water which is treated with sulfur (4 parts). Upon evaporation of the solution, the salt crystallizes as large tetrahedra, which are easily soluble in water. The anhydrous salt melts easily on heating, and in the hydrated condition, on exposure to moist air becomes coated with a red film.
The required antimony(III) sulfide is prepared in the usual way by treatment of virtually any Sb(III) compound with sulfide sources:
:2 SbCl3 + 3 H2S → Sb2S3 + 6 HCl

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