Notes. Aqueous chemistry of platinum and palladium complexes. Synthesis and crystal structure of a palladium(II) aqua complex with a cyclometallated ligand: [PdL(H2O)(ONO2)]ClO4·H2O (L = 1-methyl-2,2′-bipyridin-3-ylium)

Abstract

Treatment of [Pd(L)Cl₂]1(L = 1-methyl-2,2′-bipyridin-3-ylium) with AgNO₃ in water yields [PdL(H₂O)₂]²⁺ and NO₃^– which on evaporation to dryness affords [PdL(ONO₂)₂]2. Addition of NaClO₄ to a solution of [PdL(H₂O)₂]²⁺ gives crystals of [PdL(H₂O)(ONO₂)]ClO₄·H₂O 3. Crystals of 3 are monoclinic, space group C2/c with a= 19.383(8), b= 11.813(5), c= 13.636(5)Å, β= 95.55(2)° and Z= 8. Refinement of 3604 reflections [I > 4σ(I)] out of a total of 4460 reflections (3 < 2θ < 64°) gave R and R′ values of 0.040 and 0.042 respectively. The nitrato group is trans to the pyridyl nitrogen atom of L with a Pd–O distance of 2.052(3)Å. The Pd–OH₂ distance is 2.132(3)Å, consistent with the higher trans influence of the carbon-bonded N-methylpyridyl moiety.