A condensation reaction of an equimolar ratio of 2-pyridinecarboxaldehyde and (6-methylpyridin-2-yl)methanol without a catalyst in a solvent-free reaction at 140°C was expected to yield 2-hydroxy-[1,2-bis(6-methylpyridin-2yl)]ethan-1-one. FT-IR spectroscopy of the yellow-brown solid reaction product indicated the presence of a -CO-COH-group. The solid compound was treated with cyclohexane and green crystals were produced. The crystals were characterised by FT-IR, 1 H NMR, EI mass spectrometry and single-crystal X-ray diffraction. The molecular and crystal structure determined by single-crystal X-ray diffraction resolved one crystal showing two molecular components [C 13 H 10 N 2 O 2 and C 14 H 12 N 2 O 2 ] at a ratio of 60.4:39.6 [C 13.40 H 10.79 N 2 O 2 ]. Both compounds co-crystallise in the triclinic space group P-1, with a = 7.859(5), b = 8.021(14), c = 9.060(5) Å, a = 101.36(2)°, b = 90.06(3)°, g = 90.92(3)°, V = 559.8( 5) Å 3 , Z = 2. The compounds were 1,2-bis(6-methylpyridin-2-yl)ethane-1,2-dione and 1-(pyridin-2-yl)-2-(6-methylpyridin-2-yl)ethane-1,2-dione. These results are important because they confirm that condensation in a solvent-and catalyst-free reaction yielded precursors that were converted into a-diketone compounds by the action of solvent and oxygen.