Using solvothermal synthesis, eight new 3D microporous lanthanide-ions-based MOFs constructed from 4,4′-oxybisbenzoic acid were obtained and displayed two types of architecture.

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Four temperature-dependent K I -induced K I -Ln III heterometallic coordination polymers, {[LnKIJOBA) 2 IJμ 2 -OH 2 )]•4H 2 O} n (Ln = TbIJ1), DyIJ2), H 2 OBA = 4,4′-oxybisbenzoic acid) and {[Ln 3 KIJOBA) 4 IJμ 2 -HCOO)IJμ 3 -HCOO) 2 ]•2H 2 O} n (Ln = TbIJ3), DyIJ4)), have been synthesized under hydrothermal conditions by controlling the temperature. Notably, compounds 1 and 2, consisting of an unique nine-nuclear cluster secondary building unit (SBU), [Ln 4 K 5 IJ-CO 2 ) 16 IJμ 2 -H 2 O) 4 ], linked to each other by OBA 2− , can be simplified as a highly 12-connected three-dimensional (3D) network with fcu topology. Comparably, compounds 3 and 4 consist of a rare four-nuclear cluster SBU, [Ln 3 KIJ-CO 2 ) 6 IJμ 2 -HCOO) 2 IJμ 3 -HCOO) 4 ], which are linked to each other by OBA 2− resulting in a highly 10-connected tcg topology. The luminescent properties of 1 and 3 were studied and the solid-state magnetic measurements reveal antiferromagnetic behaviors of 2 and 4.