The synthesis of tri‐heteroleptic complex of Ru(II) with diimine ligands is describe. Ten compounds [Ru(R2bpy) (biq) (L)][PF6]2 (R = H, CH3); L = 2,2′‐bipyridine (bpy), 4,4′‐dimethyl‐2,2′‐bipyridine (Me2bpy), 2,2′‐bipyrimidine (bpm), 2,2′‐biisoquinoline (biiq), 1,10‐phenanthroline (phen), dipyrido[3,2‐c:2′,3′‐e]pyridazine (taphen), 2,2′‐biquinoline (biq), 6,7‐dihydrodipyrido[2,3‐b:3,2‐j][1,10]‐phenanthroline (dinapy), 2‐(2[pyridyl)quinoline (pq), 1‐(2‐pyrimidyl)pyrazole] (pzpm), 2,2′‐biimidazole (H2biim) are characterized by elemental analysis, electronic and 1H‐NMR spectroscopy. The relative photosustitution rates of biq in MeCN are given at three temperatures.

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The synthesis of tris‐heteroleptic complexes of type (V) occurs by substitution of the acetonitrile ligands in the intermediate (III), which in turn is obtained by photolysis of (I).

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