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Three series of fourteen cyanobridged 2D LnIII–FeIIIor LnIII–CoIIIcomplexes, [Lndmso2H2OμCN4FeCN2]n[Ln = Gd 1 and Er 2], [Lndmso2H2O3μCN3MCN3]n[La–Fe 3 and Pr–Co 4], [Lndmf2H2O3μCN3MCN3]n·nH2O [Nd–Fe 5, Gd–Fe 6, Dy–Fe 7, Er–Fe 8, Nd–Co 9, and Gd–Co 10], [Lndmso2H2O3μCN3CoCN3]n·nH2O [Ln = Pr 11, Nd 12, and Sm 13], and [ErdmfH2O3μCN4CoCN2]n·nH2O 14 dmso = dimethyl sulfoxide; dmf = N,N′dimethylformamide were rationally prepared by the ballmilling method, and their structures were characterized. The crystal structures of 1and 2reveal a sevenfold coordination environment of the Ln3+ions and a 2D stairlike structure, while those of 3–13show an eightfold coordination environment of the Ln3+ions and a 2D monolayered brickwalllike topology and that of 14exhibits an eightfold coordination environment of the Er3+ions and a 2D bilayered topology. The relationship between the crystal structures and the controllable synthesis was also discussed.