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The new sulfido antimonates(III) (Rb=Cs) 3 SbS 3  were prepared from the alkali metal sulfides Rb 2 S=Cs 2 S 2  and elemental antimony and sulfur or Sb 2 S 3  at reaction temperatures of about 700 °C. The known isotypic potassium compound was similarily synthesized from the elements. The structures of the light-yellow crystals were refined using single-crystal X-ray data. Both compounds are isotypic to the respective Na salt forming the Na 3 AsS 3  structure type (cubic, space group P2 1 3, K/Rb/Cs: a = 947:21(7)=982:28(5)=1025:92(5) pm, Z = 4, R1 = 0:0159=0:0560=0:0582). The Ψ - tetrahedral SbS 3-  3  anions with Sb-S bond lengths of 242 pm are arranged in a cubic face centered packing, in which the three crystallographically different A +  cations occupy the tetrahedral and octahedral voids, overall exhibiting a distorted octahedral sulfur coordination. The chemical bonding and the characteristics of the stereochemically active lone electron pair have been investigated by means of FP-LAPW band structure calculations. Needle-shaped crystals of the monohydrate of the antimony(V) salt Cs 3 SbS 4  · H 2 O were obtained from a suspension of Sb 2 O 3 , CsOH and elemental sulfur. Cs 3 SbS 4  · H2O crystallizes in a new structure type (monoclinic, space group P2 1 /c, a = 987:17(10), b = 994:83(7), c = 1600:46(14) pm, β = 126:895(8)°, Z = 4, R1 = 0:0234). As expected, the Sb-S distances (233.1 - 234.7 pm) in the nearly ideally tetrahedral anion SbS 3-  4  are considerably shorter than in the antimonates(III) but match the bond lengths in the anhydrous sulfido antimonate(V) Cs 3 SbS 4 . Due to their similar fcc-like anion packing and the stereochemically active lone electron pair of Sb in the antimonates(III), the whole series of compounds A 3 Sb III,V S 3/4  shows a uniform structure relation, which is elucidated using crystallographic group-subgroup relations

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Neue Sulfido-Antimonate der schweren Alkalimetalle: Synthese, Kristallstruktur und chemische Bindung von (K=Rb=Cs) 3 SbS 3  und Cs 3 SbS 4  · H 2 O / New Sulfido Antimonates of the Heavy Alkali Metals: Synthesis, Crystal Structure and Chemical Bonding of (K=Rb=Cs) 3 SbS 3  and Cs 3 SbS 4  · H 2 O