2-Carboxyphenylacetate (cpa 2 – ) and 1,2-phenylenediacetate (1,2-pda 2 – ) have been reacted with uranyl cations under solvo-hydrothermal conditions to generate six homo- or heterometallic complexes. Both [UO 2 (cpa)] ( 1 ) and [UO 2 (cpa)(phen)] ( 2 ), where phen is 1,10-phenanthroline, crystallize as monoperiodic coordination polymers. [Ni(bipy) 3 ][(UO 2 ) 2 (cpa) 3 ]×2.5H 2 O ( 3 ), is a diperiodic network with the hcb topology, in which the hexagonal cells distort to accommodate the counterions. [UO 2 (cpa) 2 Ni( R,S -Me 6 cyclam)] ( 4 ) crystallizes as a heterometallic diperiodic network, in which uranyl dicarboxylate chains are assembled by bridging Ni II cations. While [dmaepH 2 ][(UO 2 ) 2 (1,2-pda) 3 ]×3H 2 O ( 5 ), where dmaep is 1,4-bis(2ʹ-dimethylaminoethyl)piperazine, is a diperiodic hcb network, [QH] 2 [(UO 2 ) 2 (1,2-pda) 3 ]×3CH 3 CN ( 6 ), where Q is quinuclidine, is the first example of a triperiodic framework in the uranyl–phenylenediacetate family, its topological type being bto . The complex involving the related ligand 1,4-phenylenediacetate (1,4-pda 2 – ), [QH] 2 [(UO 2 ) 2 (1,4-pda) 3 ]×2CH 3 CN ( 7 ), is a daisy-chain-like monoperiodic polymer. These and previously reported results are discussed in terms of ligand flexibility and ability to form large chelate rings.