Synthesis and characterization of ruthenium acetate complexes containing triphosphines

A series of ruthenium(II) acetate complexes were synthesized and characterized by 31P[1H],1H, and 13C[1H] NMR and IR spectroscopy. Treatment of RuCl2(Cyttp) (Cyttp = PhP(CH2CH2CH2P(c-C6H11)2)2) with 1 equiv of AgO2CMe at room temperature gives mer-RuCl(O2CMe)(Cyttp) and with excess NaO2CMe in refluxing methanol produces/ac-RuCl(O2CMe)(Cyttp). fac-RuCl(O2CMe)(ttp) (ttp = PhP(CH2CH2CH2PPh2)2) was isolated when (RuCl2(ttp), was treated either with 1 equiv of AgO2CMe at room temperature or with excess NaO2CMe in refluxing methanol. Reaction of (RuCl2(ttp))x with excess AgO2CMe at room temperature gives/ac-Ru(O2CMe)2(ttp). The structure ofac-RuCl(O2CMe)(Cyttp) was determined by X-ray diffraction. fac-RuCl(02CMe)(Cyttp)-CH30H crystallized in the space group P21/c with cell parameters a = 17.534 (6) Å, b = 10.371 (4) Å, c = 22.983 (8) Å, β = 92.35 (3)°, V = 4175.7 (20) Å96, and Z = 4 and with R(F) = 0.038 and Rw(F) = 0.040.