Two novel bismuth succinate hydrates, namely, poly[[diaqua(μ3-butane-1,4-dicarboxylato)hemi(μ-butane-1,4-dicarboxylato)bismuth] monohydrate], {[Bi(C4H4O4)1.5(H2O)2]·H2O}
n
(1), and poly[[μ-aqua-aqua(μ3-butane-1,4-dicarboxylato)(μ-butane-1,4-dicarboxylato)-μ-oxido-dibismuth] monohydrate], {[Bi2(C4H4O4)2O(H2O)2]·H2O}
n
(2), have been synthesized. Their crystal structures were determined by single-crystal X-ray diffraction and the compounds were characterized by IR and Raman spectroscopy, powder X-ray diffraction and thermal analysis. The crystal structure analysis revealed that the compounds are coordination polymers, with 1 having a two-dimensional layered structure and 2 displaying a three-dimensional (3D) framework. Fully deprotonated succinate anions (C4H4O4
2−) in two different conformations (trans and gauche) are included in their composition. The Bi3+ cations are surrounded by O atoms from the carboxylate groups of succinate anions and aqua ligands. BiO9 coordination polyhedra in 1 are connected in pairs by edges. These pairs are bound together by bridging succinate ligands to form layers. Bismuth coordination polyhedra of two different types (BiO9 and BiO7) in 2 are connected by edges to form infinite ribbons. Ribbons of polyhedra with bridging succinate ligands form a 3D polymeric structure.