SYNTHESIS AND REACTIVITY OF RUTHENIUM HYDRIDE COMPLEXES OF CHELATING TRIPHOSPHINES .3. SYNTHESIS AND CHARACTERIZATION OF NEW RUTHENIUM HYDRIDE COMPLEXES CONTAINING C6H5P(CH2CH2CH2P(C-C6H11)2)2 (CYTTP)

The hydride complex RuH(BH4)(Cyttp) was produced from the reaction of RuCl2(Cyttp) with excess NaBH4. A series of six-coordinate RuHC1(L)(Cyttp) complexes (L = CO, P(OMe)3, CH3CN) were synthesized from RuHC1(Cyttp), which was prepared from the reaction of RuCl2(Cyttp) and excess lithium hydride in THF. Ruthenium dihydride complexes RuH2(L)(Cyttp) (L = CO, N2, CNCH2C6H5, P(OMe)3, and P(OPh)3) were synthesized from RuH2(H2)(Cyttp), which was prepared from the reaction of RuCl2(Cyttp) with NaH in THF under a H2 atmosphere. The new compounds were characterized by microanalyses and infrared and H-1 and P-31 NMR spectroscopy. In addition, the single-crystal X-ray structure of cis-mer-RuH2(N2)(Cyttp) has been determined. RuH2(N2)(Cyttp) crystallizes in space group Pnma with cell parameters a = 16.383 (4) angstrom, b = 20.659 (4) angstrom, c = 10.907 (3) angstrom, V = 3692 angstrom 3, Z = 4, R(F) = 0.040, and R(w)(F) = 0.043 for the 2442 intensities with F(o)2 > 3-sigma(F(O)2) and the 211 variables.