Four metal-organic frameworks have been isolated and structurally characterised from the reaction between Zn({NO3)(2)center} dot {6H(2)O} and the bis(beta-diketone) 3,4-diacetyl-2,5-dioxohexane in the presence of triethylamine. When the reaction was carried out in {DMF/chloroform} or {DMSO/methanol} the one-dimensional coordination polymers \{[Zn(L)({DMF)]center} dot {0.65CHCl(3)center} dot {0.35DMF\}(infinity)} 1 and \{[Zn-3(L)(3)({MeOH)(DMSO)(4.2)]center} dot {0.8DMSO\}(infinity)} 2, respectively, were isolated in low yield. When the reaction was carried out in methanol, three products were isolated-\{[Zn-2(L)(2)({MeOH)(2)]center} dot {2MeOH\}(infinity)} 3, \{[Zn-2(L)(2)({MeOH)]center} dot {2H(2)O\}(infinity)} 4 and \{[Zn-2(L)(2)({OH2)(2)]\}(infinity)} 5. Compounds 3 and 4 have structures in which Zn-2(mu-beta-diketonate)(2)(beta-diketonate)(2) dimers are interlinked into similar two-dimensional networks. Analyses suggest 5 has a similar structure, though with terminal aqua ligands instead of methanol ligands. The reaction between Cd({NO3)(2)center} dot {4H(2)O}, 3,4-diacetyl-2,5-dioxohexane and triethylamine in methanol gave \{[Cd-2(L)(2)({H2O)(2)]center} dot {2.5H(2)O\}(infinity)} 6, which has a similar network structure to 3 and 4. These compounds are the first structurally characterised network structures based on bis(beta-diketonate) ligands, and they demonstrate that these ligands can behave in an analogous manner to dicarboxylates. ; 10