Abstract: | The two‐ and three‐dimensional mercurous cations (Hg2)3(OH)2]4+ and (Hg2)2O]2+ crystallize with channels and cages of roughly 1 nm diameter from aqueous solutions dependent upon the acidity of the solution. Crystal structures were determined, for example, for Zn(H2O)6](Hg2)3(OH)2](NO3)6 (trigonal, space group P321, a = 1183.5(2) pm, c = 534.8(1) pm, Z = 1, R1 = 0.0351 for I0 > 2σ(I0)) and for (Hg2)2O]Pb(NO3)3]2 (cubic, space group , a = 1543.1(2) pm, Z = 8, R1 = 0.0534 I0 > 2σ(I0)). |