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The synthesis, structure and properties of the bimetallic layered coordination polymer, [KDy(C8H3NO6)3(C8H5NO6)]n·2n(C10H9N2)·5n(H2O) = [KDy(Hptc)3(H3ptc)]n·2n(Hbipy)·5n(H2O), are described. The Dy3+ ion is coordinated by three O,N,O-tridentate doubly-deprotonated pyridine tri-carboxylate (Hptc) ligands to generate a fairly regular DyO6N3 tri-capped trigonal prism, with the N atoms acting as the caps. The potassium ion is coordinated by an O,N,O-tridentate H3ptc molecule as well as monodentate and bidentate Hptc ligands to result in an irregular KNO9 coordination geometry. The ligands bridge the metal-atom nodes into a bimetallic, layered, coordination polymer, which extends as corrugated layers in the (010) plane, with the mono-protonated bipyridine cations and water molecules occupying the inter-layer regions: Unlike related structures, there are no dysprosium–water bonds. Many O–HLO and N–HLO hydrogen bonds consolidate the structure. Characterization and bioactivity data are described. Crystal data: C52H42DyKN8O29, Mr = 1444.54, triclinic,  (No. 2), Z = 2, a = 9.188(2) Å, b = 15.7332(17) Å, c = 19.1664(19) Å, α = 92.797(6)°, β = 92.319(7)°, γ = 91.273(9)°, V = 2764.3(7) Å3, R(F) = 0.029, wR(F2) = 0.084

crystals

[KDy(Hptc)3(H3ptc)]n·2n(Hbipy)·5n(H2O), a Layered Coordination Polymer Containing DyO6N3 Tri-Capped Trigonal Prisms (H3ptc = Pyridine 2,4,6-Tricarboxylic Acid, C8H5NO6; Bipy = 2,2'-Bipyridine, C10H8N2)