The neutral ruthenium complexes Cp′Ru(PR 3 ) 2 Cl [Cp′ ) Cp, PR 3 ) PPh 3 , PMe 3 , or 1/2 dppe; Cp′ ) Cp*, PR 3 ) PMe 3 ] react with [p-MeOC 6 H 4 N 2 ][BF 4 ] in acetone to give new cyclopentadienyl ruthenium aryldiazenido dicationic complexes [Cp′Ru(PR 3 ) 2 (N 2 C 6 H 4 OMe)]-[BF 4 ] 2 [Cp′ ) Cp, PR 3 ) PPh 3 (1), PMe 3 (2), or 1/2 dppe (3); Cp′ ) Cp*, PR 3 ) PMe 3 (4)] in good yields. The dicationic complexes 1-3 may also be conveniently isolated in better yield by treatment of the acetonitrile ruthenium complexes [CpRu(PR 3 ) 2 (NCMe)][BF 4 ] with the arenediazonium salt. When the reaction of Cp′Ru(PPh 3 ) 2 Cl (Cp′ 5) or Cp* ( 6)]. Further, if the reaction of Cp*Ru(PPh 3 ) 2 Cl with diazonium salt is carried out in acetone, the binuclear complex [Cp*RuCl(N 2 C 6 H 4 OMe)] 2 [Cl] 2 (7) can be isolated in low yield in addition to 6. All new complexes 1-7 were fully characterized by NMR, FT-IR, and mass spectroscopies. The structure of [CpRu(PPh 3 ) 2 (N 2 C 6 H 4 OMe)][BF 4 ] 2 ‚0.93CHCl 3 (1‚ 0.93CHCl 3 ) was determined by single-crystal X-ray diffraction. The structure exhibits a nearlinear Ru-N-N-C geometry for the coordinated aryldiazenido group, with the NNC angle having a value of 159°, compared to the "sp 2 " value of approximately 120°commonly exhibited by other "singly bent" aryldiazenido complexes. On the basis of NMR spectroscopic data, 1 reacts with NaBH 4 at low temperature to give an arylhydrazido(2-) complex [CpRu(PPh 3 ) 2 -{NN(H)C 6 H 4 OMe}][BF 4 ], which readily converts to the corresponding aryldiazene complex [CpRu(PPh 3 ) 2 (NHdNC 6 H 4 OMe)][BF 4 ] by a hydrogen shift; at room temperature, the only product is the hydrido complex CpRuH(PPh 3 ) 2 .
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