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A heterometallic metal-organic framework (MOF) of [Cd 6 Ca 4 (BTB) 6 (HCOO) 2 (DEF) 2 (H 2 O) 12 ]∙DEF∙ x Sol ( 1 , H 3 BTB = benzene-1,3,5-tribenzoic acid; DEF = N , N '-diethylformamide; x Sol. = undefined solvates within the pore) was prepared by solvothermal reaction of Cd(NO 3 ) 2 ·4H 2 O, CaO and H 3 BTB in a mixed solvent of DEF/H 2 O/HNO 3 . The compatibility of these two divalent cations from different blocks of the periodic table results in a solid-state structure consisting of an unusual combination of a discrete V-shaped heptanuclear cluster of [Cd 2 Ca] 2 Ca' and an infinite one-dimensional (1D) chain of [Cd 2 CaCa'] n that are orthogonally linked via a corner-shared Ca 2+ ion (denoted as Ca'), giving rise to an unprecedented branched-chain secondary building unit (SBU). These SBUs propagate via tridentate BTB to yield a three-dimensional (3D) structure featuring a corner-truncated P 4 1 helix in MOF 1 . This outcome highlights the unique topologies possible via the combination of carefully chosen s- and d-block metal ions with polydentate ligands.

A Heterometallic Three-Dimensional Metal−Organic Framework Bearing an Unprecedented One-Dimensional Branched-Chain Secondary Building Unit