We report am etal-organic framework where an ordered arrayoftwo linkers with differing length and geometry connect [Zr 6 (OH) 4 O 4 ] 12+ clusters into at welve-connected fcu net that is rhombohedrally distorted from cubic symmetry.The ordered binding of equal numbers of terephthalate and fumarate ditopic carboxylate linkers at the trigonal antiprismatic Zr 6 core creates close-packed layers of fumarateconnected clusters that are connected along the single remaining threefold axis by terephthalates.T his well-defined linker arrangement retains the three-dimensional porosity of the Zr cluster-based UiO family while creating two distinct windows within the channelst hat define two distinct guest diffusion paths.T he ordered material is accessed by ar estricted combination of composition and process parameters that were identified by high-throughput synthesis.

We report am etal-organic framework where an ordered arrayoftwo linkers with differing length and geometry connect [Zr 6 (OH) 4 O 4 ] 12+ clusters into at welve-connected fcu net that is rhombohedrally distorted from cubic symmetry.The ordered binding of equal numbers of terephthalate and fumarate ditopic carboxylate linkers at the trigonal antiprismatic Zr 6 core creates close-packed layers of fumarateconnected clusters that are connected along the single remaining threefold axis by terephthalates.T his well-defined linker arrangement retains the three-dimensional porosity of the Zr cluster-based UiO family while creating two distinct windows within the channelst hat define two distinct guest diffusion paths.T he ordered material is accessed by ar estricted combination of composition and process parameters that were identified by high-throughput synthesis.