Complex [Cu 2 (ben) 4 ·2THF−(η 1 -O 2 )] ∞ (2) (ben = C 6 H 5 CO 2 − benzoate; THF = tetrahydrofuran) was isolated when a solution of Cu 2 (ben) 4 ·2THF (1) in THF upon natural sunlight irradiation yields crystals suitable for single-crystal X-ray diffraction analysis. 2, crystallized in the C2/c monoclinic space group, Z = 8, V = 3394.2 (4) Å 3 , and the unit cell parameters a = 9.7935 (7) Å, b = 19.0055 (13) Å, c = 18.2997 (13) Å, α = 90°, β = 94.7996 (11)º and γ = 90°. This is the first example of a polymeric copper(II) carboxylate compound stabilizing a peroxo group via its apical ligand (THF molecule). Additionally, 2 was also characterized by elemental analysis, Fourier-transformed infrared spectroscopy (FTIR) and Raman spectroscopy. Graphical AbstractUpon sunlight irradiation a solution of Cu 2 (ben) 4 ·2THF (ben = C 6 H 5 CO 2 − , benzoate; THF = tetrahydrofuran) in THF yields [Cu 2 (ben) 4 ·2THF-(η 1 -O 2 )] ∞ as a polymeric copper(II) carboxylate compound stabilizing a peroxo group via its apical ligand (THF molecule).

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