115461-84-2Relevant academic research and scientific papers
Cluster synthesis. 22. Synthesis and structural characterization of Ru7(CO)19(μ-CNMe2)(μ6-H) containing an interstitial hydride ligand and Ru5(CO)12(PMe2Ph)2(μ 4-η2-CNMe2)(μ-H) containing a quadruply bridging (dimethylamino)carbyne ligand
Adams, Richard D.,Babin, James E.,Tanner, James T.
, p. 2027 - 2033 (2008/10/08)
The reaction of Ru4(CO)12(μ4-η2-CNMe 2)(μ-H) (1) with Ru(CO)5 at 68°C yielded the two higher nuclearity cluster complexes Ru7(CO)19(μ-CNMe2)(μ6-H) (2, 28%) and Ru5(CO)14(μ4η2-CNMe 2)(μ-H) (3, 35%). Compound 2 was obtained from 3 in 63% yield by reaction with Ru(CO)5. Compounds 2 and 3 were characterized by IR and 1H NMR spectroscopy. Compound 2 was also characterized by a single-crystal X-ray diffraction analysis. The structural characterization of 3 was achieved via its bis(dimethylphenyl)phosphine derivative Ru4(CO)12(PMe2Ph)2(μ 4-η2-CNMe2)(μ-H) (4). For 2: space group P21/c, a = 14.590 (1) A?, b = 9.845 (2) A?, c = 22.381 (3) A?, β = 90.122 (9)°, V = 3214 (1) A?3, Z = 4. The structure was solved by direct methods and was refined (4777) reflections to R = 0.025 and Rw = 0.023. The molecule consists of a capped octahedral cluster of seven ruthenium atoms with the hydride (located and refined) on the interior of the octahedron. It appears that the hydride ligand does not lie in the exact center of the octahedron but is displaced slightly toward the capping metal atom. This hydride does exhibit the usual low-field 1H NMR shift, δ 11.42. For 4: space group P21/c, a = 15.607 (6) A?, b = 12.255 (3) A?, c = 20.608 (9) A?, β = 106.27 (3)°, V = 3783 (2) A?3, Z = 4. The structure was solved by direct methods and was refined (3123 reflections) to R = 0.035 and Rw = 0.035. The molecule consists of a capped butterfly tetrahedron of five metal atoms with a quadruply briding (dimethylamino)carbyne ligand, C-N = 1.43 (1) A?, lying in the fold of the butterfly.
