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Hydrothermal reaction of copper bromide with 4‐aminopyridine in DMF solution yields a new mononuclear copper complex [Cu(C5H6N2)4]2Br.2(C3H7NO) abbreviated Cu‐4AP‐Br. The product was characterized, structurally, by single‐crystal X‐ray diffraction analysis and, thermally, by DSC‐ATG measurement. The inorganic–organic hybrid compound Cu‐4AP‐Br crystallizes in the centrosymmetric space group Pbcn, exhibiting a supramolecular network. Simultaneous DSC‐ATG analysis shows that this compound remains stable up to 100 °C and then performs a successive decompositions accompanied with endothermic peaks. The complex Cu‐4AP‐Br was applied as a catalyst in the Heck coupling reaction under ultrasonic irradiation in various reaction conditions. The yields, obtained for a short period of time, allow us to consider this complex, generating selectivity on the external position of styrene with a preference of the trans form over cis, as an excellent catalyst for this type of reaction. Interestingly, Cu‐4AP‐Br displayed important antibacterial (Gram‐positive and Gram‐negative) and antioxidant activities (β‐carotene bleaching inhibition, scavenging effect on DPPH free radical, and reducing power).

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The aromatic diamine 4-aminopirydine was used for the synthesis of a series of supramolecular metal-organic sulfate salts. The obtained compounds with the formulacrystallize with a triclinic symmetry (S.G. P1 � ). These complexes possess a hybrid structure type with an interlayer distance that varies from 10 to 12 Å depending on the metal. The fact that the crystal structure is supramolecular, the mineral layer is built from hydrogen bonds only and the interlayer space is filled with aromatic diamines that form chains through π…π interactions. The thermal study in-situ of all metal compounds revealed an important stability with the formation of crystalline phases during heating. The dehydration proceeds differently according to the metal incorporated into the structure.