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Two novel three-dimensional (3D) coordination polymers Zn1.5Dy26(IN)25(CH3COO)8(CO3)11(OH)26(H2O)29 (1) and Zn1.5Gd26(IN)26(CH3COO)7(CO3)11(OH)26(H2O)28 (2) based on the linkages of large nanosized spherical hydroxo Ln26 clusters and zinc centers by organic ligands have been hydrothermally synthesized. Metal organic framework (MOF) 1 crystallizes in the triclinic space group P1̅, with a = 21.107(2) Å, b = 21.185(2) Å, c = 36.323(4) Å, α = 89.001(2)°, β = 82.486(2)°, γ = 68.359(2)°, V = 14960(3) Å3, Z = 2. MOF 2 crystallizes in the triclinic space group P1̅, a = 19.6213(15) Å, b = 22.1850(17) Å, c = 34.654(3) Å, α = 88.5340(210)°, β = 85.6520(10)°, γ = 72.9790(19)° V = 14382.5(19) Å3, Z = 2. Structural analysis indicates that both 3D polymers can be constructed using the building unit of CO3@Ln26 (Dy for 1, Gd for 2) and exhibit similar topological frameworks. During the synthesis, three ligands were used. CO3 2− plays a very important role in the formation of the spherical Ln26 cluster. CH3COO− makes the Ln26 cluster stable and reduces steric restriction. The isonicotinate (IN) stabilizes the cluster and links the clusters and the Zn centers.

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