Microwave‐assisted Synthesis, Crystal Structures, and Thermal Stability of C₁₁H₁₀N₂Cu₂Br₃ and C₂₂H₂₀N₄Cu₈I₁₀

Abstract

Complexes of C11H10N2Cu2Br3 (1) and C22H20N4Cu8I10 (2) [C22H20N4 = 1,1"‐(1,2‐ethanediyl)‐bis‐4,4′‐bipyridinium] were synthesized via the microwave‐assisted solvo‐thermal reactions of C22H20N4Br2, CuSO4·5H2O, and NaX (X = Br, I) and characterized by XRD, FTIR, and thermogravimetric analysis. The crystal structures were determined by single‐crystal X‐ray diffraction analyses. C11H10N2Cu2Br3 crystallized in the monoclinic space group C2/c (no. 15) with lattice parameters a = 24.658(3) Å, b = 6.71(9) Å, c = 17.368(9) Å, β = 98.274(1)°, V = 2847.7(1) Å3, whereas C22H20N4Cu8I10 crystallized in the monoclinic space group P21/n (no. 14) with lattice parameters a = 7.392(2) Å, b = 20.809(7) Å, c = 25.412(7) Å, β = 92.06(8) °, V = 3906.6(8) Å3. Complex 1 showed a 2D layered structure composed of [Cu4Br6]– chains connected via 1,1"‐(1,2‐ethanediyl)‐bis‐4,4′‐bipyridinium ligands. Complex 2 possessed a 3D framework, in which puckered [Cu8I10]2– layers were linked by organic ligands. The thermogravimetric analysis indicated that both two complexes were stable up to 230 °C and 170 °C, respectively.