100682-41-5Relevant academic research and scientific papers
Synthesis and characterization of [Co4(CO)11C(O)Me]-. The X-ray crystal structure of tetraphenylphosphonium tris(μ-carbonyl)octacarbonylacetyl-tetrahedro-tetracobaltate(1-)
Went, Michael J.,Brock, Carolyn P.,Shriver, Duward F.
, p. 755 - 760 (2008/10/08)
The alkylidyne complex Co3(CO)9COC(O)Me decomposes in THF to produce [Co(CO)4]-, Co4(CO)12, and an unidentified intermediate which reacts with [Co(CO)4]- to produce [Co4(CO)11C(O)Me]- (I). Complex I is also produced by the reaction of Co4(CO)12 with MeLi and has been characterized by IR and NMR spectroscopy and by a single-crystal X-ray diffraction study, as a tetraphenylphosphonium salt. The salt crystallizes in the monoclinic space group P21/c, with a = 12.026 (1) ?, b = 23.835 (3) ?, c = 12.788 (2) ?, β = 90.492 (9)°, and Z = 4. The structure has been solved from 4949 reflections with I > 3σ(I) and refined by least-squares calculations to R = 3.7%. The structure of the anion is derived from that of Co4(CO)12, with a mean cobalt-cobalt distance of 2.512 (3) ?. Three of the carbonyl groups are edge bridging, defining a basal triangle, while the remaining eight are terminal. The acetyl ligand is terminally bound in an axial position on the basal triangle, with a cobalt-carbon distance of 1.953 (4) ?.
