A new two-dimensional inorganic-organic hybrid ortho-phenylenediamine cobalt hypophosphite chloride, [Co(H 2 PO 2 )(C 12 N 4 H 16 )]Cl 2 , has been prepared by slow evaporation from an aqueous solution. It was investigated by means of single-crystal X-ray diffraction, infrared spectroscopy and thermal analysis. The title compound crystallise in orthorhombic space group Pbcn, with unit cell parameters at 298(1) K of a = 9.5538(19) Å , b = 9.1466(18) Å , c = 21.9222(4) Å , V = 1915.7(7) Å 3 , Z = 2. Its structure is characterised by inorganic layers parallel to (001) of alternating CoO 4 N 2 octahedra and H 2 PO 2 tetrahedra establishing eight-membered ring cavities. This mixed-polyhedral motive is decorated with the ortho-phenylenediamine ligands towards the inter-layer region thus forming a cationic organic-inorganic hybrid layer charge compensated by the chlorine anions. Infrared spectroscopy revealed absorption bands corresponding to the ortho-phenylenediamine molecule and the hypophosphite anion. The compound was proven to be stable up to 474 K under N 2 atmosphere. Graphical Abstract A new two-dimensional inorganicorganic hybrid ortho-phenylenediamine cobalt hypophosphite chloride, [Co(H 2 PO 2 )(C 12 N 4 H 16 )]Cl 2 , has been prepared by slow evaporation from an aqueous solution and characterized by means of single-crystal X-ray diffraction, infrared spectroscopy and thermal analysis.
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