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The gallides Ca 3 Ni 4 Ga 4  and Sr 3 Ni 3 Ga 4  were synthesized from arc-melted Ni x Ga y  precursor alloys and the respective alkaline earth metal in sealed niobium tubes in an induction furnace. Redetermination of the Ca 3 Ni 4 Ga 4  structure from X-ray single crystal diffractometer data confirmed the X-ray powder data: Na 3 Pt 4 Ge 4  type,  I 4̅3 m ,  a =740.6(1) pm,  wR 2=0.0245, 169 F 2  values, 9 variables. The nickel atoms build tetrahedral Ni 4  clusters (256 pm Ni–Ni) that are end-on coordinated by gallium atoms (234 pm Ni–Ga). These [Ni 4 Ga 4 ] units show a  bcc  packing and leave cavities Ca@Ga 4 Ni 4 Ga 4  for the calcium atoms. Sr 3 Ni 3 Ga 4  crystallizes with a new structure type:  R 3 m ,  a =1039.8(2),  c =698.2(1) pm,  wR 2=0.1048, 636 F 2  values, 23 variables. The structure shows twinning by inversion with a domain ratio of 79/21. The structures of Sr 3 Ni 3 Ga 4  and Ca 3 Ni 4 Ga 4  are related by a group–subgroup scheme ( R 3 m  is a  translationengleiche  subgroup of  I 4̅3 m ). The 8 c  Ni and Ga subcell sites split into site 3 a  and 9 b  each. This allows formation of ordered Ni 3 Ga tetrahedra (264 pm Ni–Ga) along with ordered gallium vacancies.

Ni 4 and Ni 3 Ga clusters as building units in Ca 3 Ni 4 Ga 4 and Sr 3 Ni 3 □Ga 4