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The Ga/In phase width ( y ) and the distribution of the two triels within the polyanions of known binary ( x  = 1, 2) and new ternary ‘intermediate’ ( x  = 1–2) alkali trielides  A x  (Ga 1−   y  In  y  ) 3  ( A  = K, Rb, Cs) was investigated in a synthetic (slow cooling of the melts of the three elements), crystallographic (X-ray single crystal) and bond theoretical (FP-LAPW DFT bandstructure calculation) study. The Cs 2 In 3 -type structure ( x  = 2, series  A , tetragonal,  I  4/ mmm ) exhibits layers of four-connected  closo  octahedra [ M  6 ] 4− . Ternary K compounds of this type were yielded within a large range ( y  = 0–0.87), whereas isotypic Rb/Cs trielides exist only at higher In contents (&gt;52/69%). Geometric criteria determine not only the Ga/In stability ranges but also the occurrence of a commensurate superstructure at approx. 33% In (K 2 Ga 2.17 In 0.83 :  P  4 2 / ncm ,  a  = 879.83(4),  c  = 1557.66(10) pm,  R  1 = 0.0887), in which the octahedra are slightly tilted against the layers. Cesium compounds of the RbGa 3 -type structure ( x  = 1,  C , tetragonal,  I  4̅ m 2), which exhibits a 3D network of all- exo  bonded  closo  dodecahedra [ M  8 ] 2−  and four-bonded  M  −  anions, are stable throughout the whole substitutional range CsGa 3 –CsIn 3 . The maximum possible In content increases with increasing size of  A  +  (Cs: 100%, Rb: 30%, K: 8% In). The similarities between these two tetragonal structures are consistent with the occurrence of two new structure types of ‘intermediate’ compounds  A  7  M  15  ( x  = 1.4,  1  B / 2  B ), which differ in the stacking sequences of double layers of novel six-fold  exo -bonded pentagonal bipyramidal  closo  clusters [ M  7 ] 3−  connected  via  four-bonded  M  −  (e.g.  1  B : Cs 7 Ga 8.4 In 6.6 ,  P  4̅ m 2,  a  = 656.23(3),  c  = 1616.0(1) pm,  R  1 = 0.0742;  2  B : Rb 7 Ga 8.1 In 6.9 ,  P  4 2 / nmc ,  a  = 665.64(2),  c  = 3140.9(2) pm,  R  1 = 0.0720). The Rb/Cs compounds of these types are only stable in a limited Ga/In region and with a distinct Ga/In distribution within the [ M  7 ] clusters. According to the close relation between the structures  A ,  B  and  C , the structure family is characterised by the occurrence of stacking faults and diffuse scattering, indicating the existence of further members of this series. The new compound Cs 5 Ga 3.1 In 5.9  ( x  = 1.667,  P  4̅ m 2,  a  = 654.62(2),  c  = 3281.5(2) pm,  R  1 = 0.1005) is a reasonably periodically ordered stacking variant containing layers  A  and double layers  B  in parallel.

Stacking polytypes of mixed alkali gallides/indides A 1–2 (Ga/In) 3 ( A =K, Rb, Cs): synthesis, crystal chemistry and chemical bonding