STRUCTURAL STUDIES ON RUTHENIUM CARBONYL HYDRIDES .18. SYNTHESIS AND CHARACTERIZATION OF (MU-H)RU3(MU(3)-ETA(3)-XCCRCR')(CO)9-N(PPH3)N COMPLEXES - CRYSTAL-STRUCTURES OF (MU-H)RU3(MU(3)-ETA(3)-ET2NCCHCME)(CO)8(PPH3) AND (MU-H)RU3(MU(3)-ETA(3)-MEOCCMECME)(CO)7(PPH3)2.2CH2CL2

Substitution products HRu3(mu3-eta3-XCCRCR')(CO)9-n(PPh3)n (X = OMe, R = R'= Me, n = 1-3; X = OMe, R = H, R'= OEt, n = 2, 3; X = NEt2, R = H, R' = Me, n = 1, 2) were prepared by using ONMe3-induced ligand substitution. The products were characterized by spectroscopic methods. In addition, (mu-H)Ru3(mu3-eta3-Et2NCCHCMe)(CO)8(PPh3) (Mo Kalpha, 2theta 5.0-50.0-degrees, R(F) 5.22% for all 6,374 reflections, 2.62% for those 4,306 reflections with \F(o)\ > 6sigma(\F(o)\)) and (mu-H)Ru3(mu3-eta3-MeOCCMeCMe)(CO)7(PPh3)2 . 2CH2Cl2 (Mo Kalpha, 20 8.0-45.0, RF 9.52% for all 6,798 reflections, 6.69% for those 3,795 reflections with \F(o)\ > 6sigma(\F(o)\)) were characterized by single-crystal X-ray diffraction. Both compounds crystallize in the triclinic space group P1BAR, with a 11.277(2) angstrom, b 11.899(1) angstrom, c 15.638(2) angstrom, alpha = 70.56(1), beta = 85.23(1), gamma = 66.00(1)-degrees, V = 1802.8(4) angstrom3, and Z = 2 for the former and a = 12.960(2) angstrom, b = 13.040(2) angstrom, c = 17.683(3) angstrom, a = 98.81(1), beta = 94.50(1)-degrees, gamma = 116.50(1)-degrees, V = 2606.2(8) angstrom3, and Z = 2 for the latter. In each case the PPh3 ligands are coordinated cis to the bridging hydride and to the sigma Ru-C bond.