105121-22-0Relevant articles and documents
Cluster synthesis. 17. Synthesis and structural characterizations of Ru5(CO)15(μ4-S), Ru6(CO)18(μ4-S), and Ru7(CO)21(μ4-S)
Adams, Richard D.,Babin, James E.,Tasi, Miklos
, p. 503 - 513 (2008/10/08)
When Ru3(CO)9(μ3-CO)(μ3-S) (1) was heated to 68°C in the presence of Ru(CO)5, the three new higher nuclearity clusters Ru5(CO)15(μ4-S) (2), Ru6(CO)15(μ-CO)3(μ4-S) (3), and Ru7(CO)19(μ-CO)2(μ4-S) (4) were formed. 3 was also made by heating 2 with Ru(CO)5 to 98°C, and 4 was also made by heating 3 with Ru(CO)5 to 98°C. 2, 3, and 4 were degraded by treatment with CO (1 atm)/98°C by the stepwise removal of mononuclear ruthenium carbonyl groupings. Compounds 2, 3, and 4 were characterized structurally by single-crystal X-ray diffraction analyses. For 2: space group P21/c, a = 11.896 (3) A?, b = 28.956 (9) A?, c = 13.009 (5) A?, β = 90.59 (2)°, V = 4481 (2) A?3, Z = 8, ρcalcd = 2.84 g/cm3. The structure of 2 was solved by direct methods and was refined (4012 reflections) to the final values of the residuals, R = 0.030 and RwF = 0.029. For 3: space group P1, a = 17.505 (4) A?, b = 20.303 (5) A?, c = 9.047 (2) A?, α = 91.43 (2)°, β = 103.49 (2)°, γ = 67.20 (2)°, V = 2874 (1) A?3, Z = 4, ρcalcd = 2.64 g/cm3. The structure of 3 was solved by direct methods and was refined (6319 reflections) to the final values of the residuals, R = 0.037 and RwF = 0.041. For 4: space group P21/n, a = 12.485 (5) A?, b = 16.821 (5) A?, c = 16.208 (5) A?, β = 104.06 (3)°, V = 3302 (2) A?3, Z = 4, ρcalcd = 2.67 g/cm3. The structure of 4 was solved by direct methods and was refined (2747 reflections) to the final values of residues, R = 0.048 and RwF = 0.048. Each of the structures of 2, 3, and 4 consists of square-pyramidal cluster of five ruthenium atoms with a quadruply bridging sulfido lignd spanning the square base. Compound 2 contains two symmetry-independent molecules in the crystal, and they are structurally different in the arrangement of their carbonyl ligands. Molecule A contains four bridging carbonyl ligands, one on each edge of the square base of the cluster. Molecule B has three edge-bridging carbonyl ligands and one asymmetric triply bridging carbonyl ligand. Compound 3 is similar to molecule A of 2 but has a Ru(CO)4 group in place of one of the bridging CO ligands. Compound 4 is similar to molecule A of 2 but has two Ru(CO)4 groups substituted on opposite edges of the square base for the bridging CO ligands.
