Pentaamminechlororuthenium III Chloride

Solutions of pentaammine(nitrogen)ruthenium(II) have been prepared from ruthenium (III) chloride and hydrazine hydrate.1,2 These solutions have been used to prepare pentaammine-haloruthenium(III) salts [Ru(NH3)6X]X2 (X = Cl, Br, I). [Ru(NH3)5C1]C12 has been converted to pure pentaammine-(nitrogen)ruthenium(II) salts—[Ru(NH3)5N2]X2 (X- = Cl-, Br-, I-, BF4-, PFg-)—via the reaction between azide ion and aquopentaammineruthenium(III).2 Hexaammineruthe-nium(III) salts—rRu(NH8)6]X3 (X = I-, BF4-)—have been prepared by the reaction between pentaamminechlororuthenium-(III) chloride and hydrazine monohydrochloride. 

The product is recrystallized by heating an aqueous slurry (3 g. in 10 ml. of water) to 60°C. and adding concentrated ammonia dropwise until the yellow complex dissolves to give a wine-red solution. The solution is filtered hot and then cooled in an ice bath. To the cold solution concentrated hydrochloric acid is added dropwise to reprecipitate the mustard-yellow pentaamminechlororuthenium(III) chloride. The product is collected by filtration, washed once with 6 M hydrochloric acid, and then quickly washed with water, alcohol, and acetone. Finally it is dried at 78°C. over P208 in vacuo. Yield is 1.1 g., 39%. Anal. Calcd. for CUHuNsRu H, 5.19 N, 23.98 Cl, 36.35. Found H, 5.30 N, 24.53 Cl, 34.84. 

A slurry of pentaamminechlororuthenium(III) chloride (1.0 g., 3.4 mmoles), in water (25 ml.) is heated to 60°C. Concentrated ammonia is added dropwise, and the temperature is kept at 60°C. until all the yellow complex dissolves to give a wine-red solution. This solution is cooled in an ice bath it is then stirred vigorously while methanesulfonic acid is added drop-wise to the ice-cold solution until the pH is 2. The solution becomes colorless to pale pink.f... 

See Pentaamminechlororuthenium chloride Sodium azide Hydrazine Ruthenium(III) chloride... 

---