Abstract: | Synthesis and Crystal Structure of Cs3AuO2 Bright orange single crystals of Cs3AuO2, sensitive to moisture and atmosphere, are obtained by reacting CsAu with a 1 : 1 molar mixture of Cs2O and CsO2 (CsAu : Cs2O : CsO2 = 3 : 2 : 2) in sealed silver crucibles under argon atmosphere at 380 °C for a period of 6 days. The crystal structure (Pearsoncode mP72, P21/n, a = 1019.6(3), b = 1984.3(7), c = 1028.5(4) pm, β = 93.96(1)°, Z = 12, 2562 reflections mit Io > 2σ(I), R1 = 0.0662, wR2 = 0.1660) is characterized by the presence of dumb‐bell‐shaped O–Au–O]‐moieties (d(Au–O) = 200,8(2) pm), a common feature of oxoaurates(I). |