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In this work, two rare high‐dimensional polyoxoniobates with formulas of H9[Cu(en)(H2O)2][Cu(en)2]8[Dy(H2O)4]3[Nb24‐O69(H2O)3]2 ⋅ 36H2O (1) and H9K[Cu(en)2(H2O)]5[Cu(en)2]4‐[Eu(H2O)4]3[Nb24O69(H2O)3]2 ⋅ 2en ⋅ 45H2O (2) have been obtained under hydrothermal conditions. These extended materials are constructed from lanthanide‐incorporated triangular‐prism‐like polyoxoniobate secondary building units (SBUs) {[Ln(H2O)4]3[Nb24O69(H2O)3]2} (Ln=Dy, Eu). 1 and 2 represent the first examples of high‐dimensional polyoxometalate materials based on such lanthanide‐incorporated triangular‐prism‐like polyoxoniobate SBUs. Furthermore, the proton conduction property and the luminescent emission of these materials were evaluated. [ABSTRACT FROM AUTHOR]

Two unique heterometallic cluster organic frameworks, [Cd4MnIII4MnII6(Tri)4(CH3COO)14(μ4‐O)2(μ3‐O)2(H2O)2] Cd(H2O)2⋅9 H2O (1) and Cu[Cd5Cu6(Tri)4(CH3COO)9(H2O)4]2(CH3COO)3⋅24 H2O (2) (H3Tri=2‐(hydroxymethyl)‐2‐(pyridine‐4‐yl)‐1,3‐propanediol), have been successfully prepared by employing a bifunctional tripodal alcohol ligand as a structure‐directing agent. Crystal structure analyses reveal that 1 represents a rare example of frameworks constructed from Cd−Mn heterometallic chains, and 2 is the first heterometallic MOF based on highest‐nuclear Cd−Cu heterometallic cluster building blocks. Furthermore, the magnetic properties and gas adsorption abilities of 1 and 2 were systematically studied. [ABSTRACT FROM AUTHOR]