| Summary: | Ionothermal synthesis is a little used method for the preparation of coordination polymers. By this method, two cadmium compounds were synthesized, <b>1</b>, with formula Cd<sub>3</sub>(ox)F<sub>2</sub>(Ina)<sub>2</sub> (Ina = isonicotinate) and <b>2</b>, Cd(NO<sub>3</sub>)<sub>2</sub>(4,4′-Bpy) (4,4′-Bpy = 4,4′-Bipyridine). The modification of the reaction conditions has allowed to obtain <b>2</b> as a pure phase. The structure of both compounds was determined by a single-crystal X-ray diffraction. Compound <b>1</b> is isostructural to the previously reported Cd<sub>2</sub>Zn(ox)(OH)<sub>2</sub>(Ina)<sub>2</sub>. It crystallizes in the monoclinic space group P<i>2</i><sub>1</sub><i>/n</i> and present a three-dimensional (3D) network, built-up from [Cd<sub>3</sub>(ox)F<sub>2</sub>]<sub>n</sub><sup>2n+</sup> layers, linked by isonicotinate ligands. Crystals of <b>2</b> are formed by twins of two components which are rotated ca. 180° to each other. This compound crystallizes in the triclinic P<i>-1</i> space group and its structure can be describe as a two-dimensional (2D) 4 connected <i>‘sql’</i> net. The layers are composed by [Cd(NO<sub>3</sub>)<sub>2</sub>]<sub>n</sub> chains linked through 4,4′-Bpy ligands, and are pillared along the [011] direction. The thermal decomposition of <b>2</b> 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.
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