152227-36-6Relevant articles and documents
Controlled microwave synthesis of RuII synthons and chromophores relevant to solar energy conversion
Sun, Yali,Machala, Michael L.,Castellano, Felix N.
, p. 283 - 287 (2010)
Here we describe the efficient high yield atmospheric pressure microwave-assisted synthesis for seven distinct RuII coordination complexes relevant to solar energy conversion schemes and dye sensitized solar cells. In all instances, the reaction times have been markedly shortened, concomitant with higher yields with little or no need for subsequent purification and several multi-step reactions proceeded flawlessly in a single pot. Importantly, we observed no evidence for the decarboxylation of the essential metal oxide surface-anchoring 4,4′-diethylester-2,2′-bipyridine or 4,4′-dicarboxy-2,2′-bipyridine ligands as long as open reaction vessel conditions were utilized; these functionalities are not tolerant to sealed microwave reaction (superheated solvent/pressurized) conditions. The combined results suggest that microwave-assisted chemistry is indeed a valuable tool as far as RuII coordination chemistry is concerned and can likely be applied in the combinatorial pursuit of new dyes bearing sensitive functionalities.
Reactions of [Ru(bpy)(CO)2Cl2] in Acidic Media: Formation and Structural Characterization of [Ru(bpy)Cl3NO], [Ru2N(bpy)2Cl5(H2O)], and (H5O2)[Ru2N(bpy)2Cl6]
Haukka, Matti,Venaelaeinen, Tapani,Ahlgren, Markku,Pakkanen, Tapani A.
, p. 2931 - 2936 (2008/10/08)
Reactions of [Ru(bpy)(CO)2Cl2] in concentrated HCl/HNO3 solutions at high temperatures were studied. In acidic solutions carbonyl groups are lost and replaced by chlorine and nitrosyl, nitrido or water ligands. Formation of [Ru(bpy)Cl3(NO)] and (Ru2N(bpy)2Cl5(H2O)] was time-dependent; with shorter reaction times ( a new crystalline nitrido-bridged complex[Ru2N(bpy)2Cl5(H2O)] (2) was produced, most probably via a nitrosyl intermediate. Both 1 and 2 are practically insoluble and highly stable. However, the reaction of [Ru(bpy)(CO)2Cl2] in HCl/HNO3 solution with small amounts of [Ru(bpy)Cl3(NO)] added gave in low yield another nitrido-bridged product, (H5O2)[Ru2N(bpy)2Cl6] (3). The role of added [Ru(bpy)Cl3(NO)] in this reaction is unclear, and it is possible that (3) may also form directly from pure [Ru(bpy)(CO)2Cl2]. Crystal structures of fac(Cl)-[Ru(bpy)Cl3(NO)], mer(Cl)-[Ru(bpy)Cl3(NO)], [Ru2N(bpy)2Cl5(H2O)], and (H5O2)[Ru2N(bpy)2Cl6] showed that the ruthenium atoms are octahedrally coordinated in all complexes. Crystal data: 1a, monoclinic, space group P21/c, a = 6.798(3) ?, b = 11.993(4) ?, c = 16.760(8) ?, β =98.89(3)°, Z = 4; 1b, monoclinic. space group Pn, a = 8.175(2) ?, b = 6.733(2) ?, c = 12.594(5) ?, β = 105.06(3)°, Z = 2; 2, monoclinic, space group P21/n, a = 10.133(5) ?, b = 15.042(6) ?, c = 16.506(8) ?, β = 104.86(4)°, Z = 4; 3,triclinic. space group P1-, a = 10.281(3) ?, b = 10.776(3) ?, c= 12.527(5) ?, α = 90.78(3)°, β = 98.31(3)°, γ = 100.91(2)°, Z = 2.