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Ionothermal synthesis is a little used method for the preparation of coordination polymers. By this method, two cadmium compounds were synthesized, 1 , with formula Cd 3 (ox)F 2 (Ina) 2 (Ina = isonicotinate) and 2 , Cd(NO 3 ) 2 (4,4'-Bpy) (4,4'-Bpy = 4,4'-Bipyridine). The modification of the reaction conditions has allowed to obtain 2 as a pure phase. The structure of both compounds was determined by a single-crystal X-ray diffraction. Compound 1 is isostructural to the previously reported Cd 2 Zn(ox)(OH) 2 (Ina) 2 . It crystallizes in the monoclinic space group P 2 1 /n and present a three-dimensional (3D) network, built-up from [Cd 3 (ox)F 2 ] n 2n+ layers, linked by isonicotinate ligands. Crystals of 2 are formed by twins of two components which are rotated ca. 180° to each other. This compound crystallizes in the triclinic P -1 space group and its structure can be describe as a two-dimensional (2D) 4 connected 'sql' net. The layers are composed by [Cd(NO 3 ) 2 ] n chains linked through 4,4'-Bpy ligands, and are pillared along the [011] direction. The thermal decomposition of 2 was studied by thermogravimetric and thermodiffractiometric techniques. The compound decomposes gradually starting from 160 °C, and due to heating, the structure suffers slight reversible changes in the bond distances and angles.