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We have discovered a metal−organic framework containing cationic inorganic layers. The metal fluoride−organodisulfonate structure, Pb2F2C2H4(SO3)2, was synthesized hydrothermally. The lead fluoride cationic layers are covalently connected by 1,2-ethanedisulfonate chains oriented perpendicular to the layers. The material is thermally stable to ca. 325 °C, above which the material collapses to phase-pure -PbF2. This material is a rare example of the use of organosulfonates as organic linker and the first metal−organic framework to contain lead fluoride connectivity. The existence of extended cationic inorganic moieties embedded within a metal−organic framework material further diversifies the possible structure types of this rapidly growing class of materials. [ABSTRACT FROM AUTHOR]