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The high-temperature polymorph of the trisulfide Cs 2 S 3 , which has been synthesized from Cs 2 S 2  and elemental sulfur, crystallizes in a new structure type (monoclinic, space group  P 2 1 / c ,  a =999.97(4),  b =1029.30(5),  c =2642.07(12) pm,  β =90.083(2)°,  Z =16,  R 1=0.0324). The structure contains four crystallographically independent angledS  3   2  −${\rm{S}}_3^{2 - }$    trisulfide ions with S–S distances of 205.7–208.3 pm. The distorted b.c.c. packing of the anions and their insertion in the five-membered rings of 3.5 3 +3.5.3.5. (1:1) Cs nets are similarly found in the r.t. form ( Cmc 2 1 , K 2 S 3 -type structure) and the two polymorphs differ mainly in the orientation of the S 3  groups. The second title compound, K 37 Te 28 , was synthesized from stoichiometric melts of the elements. It forms a complex (3+1)D modulated tetragonal structure (space group  I 4 1 / amd  (00 σ  3 ) s 0 s 0,  q =(0, 0, 0.5143),  a =1923.22(2),  c =2626.66(4) pm,  Z =4,  R 1 all =0.0837). According to K 37 Te 28 =K 37 [Te(1 X )] 8 [Te(2 X ) 2 ] 6 [Te(3 X ) 8 ] the structure contains three different types of Te anions: The two crystallographically different isolated telluride anions [Te(1 X )] 2−  are coordinated by 9/10 K +  cations. Three [Te(2 X ) 2 ] 2−  dumbbells ( d  Te-Te =277.9/286.4 pm) are arranged to ‘hexamers’. The Te(31) and Te(32) atoms are located in columns of face-sharing K square antiprisms. Their  z  position modulation, which is accompanied by a smaller shift of the surrounding K +  cations, results in the decomposition of the [Te(3 X ) 8 ] 2  chain in a sequence |:Te 3 –Te 2 –Te 2 –Te 3 –Te 2 –Te 2 –Te 2 :| of dumbbells Te 2  2−  ( d  Te–Te =304 pm) and hypervalent linear trimers Te 3  4−  ( d  Te–Te =325 pm).

Crystal structure of the high-temperature form of the trisulfide Cs 2 S 3 and the (3+1)D modulated structure of the telluride K 37 Te 28