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Investigation of the quaternary system, Ca⁻Eu⁻Cd⁻Sb, led to a discovery of the new solid solutions, Ca 1- x  Eu  x  Cd₂Sb₂, with the CaAl₂Si₂ structure type ( x ≈ 0.3⁻0.9, hP 5, P 3 ¯ m 1, a = 4.6632(5)⁻4.6934(3) Å, c = 7.630(1)⁻7.7062(7) Å), Ca 2- x  Eu  x  CdSb₂ with the Yb₂CdSb₂ type ( x ≈ 0.6, oS 20, Cmc 2₁, a = 4.646(2) Å, b = 17.733(7) Å, c = 7.283(3) Å), and Eu 11- x  Ca  x  Cd₆Sb 12 with the Sr 11 Cd₆Sb 12 type ( x ≈ 1, mS 58, C 2/ m , a = 32.407(4) Å, b = 4.7248(5) Å, c = 12.377(1) Å, β = 109.96(1)°). Systematic crystallographic studies of the Ca 1- x  Eu  x  Cd₂Sb₂ series indicated expansion of the unit cell upon an increase in the Eu content, in accordance with a larger ionic radius of Eu 2+ vs. Ca 2+ . The Ca 2- x  Eu  x  CdSb₂ composition with x ≈ 0.6 adopts the non-centrosymmetric space group, Cmc 2₁, although the parent ternary phase, Ca₂CdSb₂, crystallizes in the centrosymmetric space group, Pnma . Two non-equivalent Ca sites in the layered crystal structure of Ca 2- x  Eu  x  CdSb₂ get unevenly occupied by Eu, with a preference for the interlayer position, which offers a larger available volume. Similar size-driven preferred occupation is observed in the Eu 11- x  Ca  x  Cd₆Sb 12 solid solution with x ≈ 1.

Exploratory Work in the Quaternary System of Ca–Eu–Cd–Sb: Synthesis, Crystal, and Electronic Structures of New Zintl Solid Solutions