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Orthorhombic single crystals of CsCu 3 Dy 2 S 5  (a = 397.54(4), b = 1414.8(1), c = 1685.7(2) pm) and CsCu 3 Er 2 S 5  (a = 394.82(4), b= 1410.9(1), c = 1667.2(2) pm; both Cmcm, Z = 4) are obtained as by-products (pale yellow or pink transparent needles) in attempts to synthesize CuMS 2  (M = Dy and Er) through the oxidation of elemental copper, dysprosium and erbium, respectively, with sulfur (molar ratios: 1:1:2 ) in the presence of equimolar amounts of cesium chloride (CsCl) as fluxing agent at 900 °C within fourteen days from torch-sealed evacuated silica tubes. Their crystal structure contains octahedral [MS 6 ] 9-  units (d(M-S) = 269 - 282 pm) which share edges and vertices to form layers  2  ∞ {(M 2 S 5 ) 4- } parallel (010). These are three-dimensionally interconnected along [010] by two crystallographically different Cu +  cations in tetrahedral coordination of S 2-  anions (d(Cu-S) = 227 - 269 pm) according to  3  ∞ {(Cu 3 M 2 S 5 ) -  }. Thereby a likewise layered substructure  2  ∞ {(Cu 3 S 5 ) 7- } is formed parallel (010) by edge- and vertexlinking of all [CuS 4 ] 7-  tetrahedra. Large channels within the  3  ∞ {(Cu 3 M 2 S 5 ) - } network spread along [100] and suit well to take up the highly coordinated Cs +  cations, which are surrounded by eight plus one S 2-  anions at distances between 340 and 358 pm (8x) with the ninth ligand 420 - 421 pm apart in the shape of (2+1)-fold capped trigonal prisms.

zeitschrift für naturforschung b

CsCu 3 Dy 2 S 5  und CsCu 3 Er 2 S 5  : Zwei isotype quaternäre Sulfide der Lanthanoide mit Kanalstrukturen / CsCu 3 Dy 2 S 5  and CsCu 3 Er 2 S 5 : Two Isotypic Quaternary Sulfides of the Lanthanides with Channel Structures