Two new cobalt phosphite–oxalates (1 and 2) have been synthesized under solvent-free conditions. Compound 2 possesses room temperature proton conductivity.

In the presence of the amino acid histidine, an inorganic–organic hybrid metal sulfite (compound 1), has been prepared under hydrothermal conditions. Compound 1 shows a high proton conductivity of, approximately 10−3 S cm−1 at 348 K and 98% RH.

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Two novel cobalt phosphite‐oxalates with different frameworks, which are isomeric and of stoichiometry Co(H2PO3)(C2O4)·(C2H8N) (1 and 2), were prepared under solvothermal conditions by in situ reactions. Single‐crystal X‐ray diffraction analysis reveals that 1 crystalilizes in the triclinic system space group P1 and 2 crystallizes in the monoclinic system space group P21/n. Compound 1 shows a 2D layered structure and 2 presents a 3D open‐framework. Both structures are constructed with zigzag cobalt oxalate chains and [H2PO3]– pseudopyramids. The solvent with different pH values and components plays an important role in the formation of the final structures of both compounds. Moreover, magnetic properties were also investigated.