129521-34-2Relevant academic research and scientific papers
Cluster chemistry. Study of the pyrolysis of Ru3(μ-dppf)(CO)10 (dppf = 1,1′-bis(diphenylphosphino)ferrocene). X-ray structures of Ru3(μ-H){μ3-(η1,η 2-C6H4)PPh(η-C5H 4)Fe(η-C5H4PPh2 ...
Bruce, Michael I.,Humphrey, Paul A.,Bin Shawkataly, Omar,Snow, Michael R.,Tiekink, Edward R. T.,Cullen, William R.
, p. 2910 - 2919 (2008/10/08)
Full title: Cluster chemistry. Study of the pyrolysis of Ru3(μ-dppf)(CO)10 (dppf = 1,1′-bis(diphenylphosphino)ferrocene). X-ray structures of Ru3(μ-H){μ3-(η1,η 2-C6H4)PPh(η-C5H 4)Fe(η-C5H4PPh2)}(CO) 8, Ru3{(μ-P(C6H4)-η-C5H 4)Fe(η-C5H4PPh 2)}(μ-CO)(CO)8, Ru3(μ3-η1,η1η 2-C6H4)(μ-PPh 2)(μ-PPhFc)(CO)7, Ru3(μ-H){μ3-(η1,η 5-PPh2C5H3)Fe(η-C 5H4PPh2)}(CO)7, and Ru4(μ4-PFc)(μ4-C6H 4)(μ-CO)(CO)10 (Fc = Fe(η-C5H5)(η-C5H4)). Pyrolysis of Ru3(CO)10(dppf) (cyclohexane, 81°C, 2 h) gave six major products, of which the title complexes were fully characterized by X-ray crystallographic studies. Structural features include metalated η1- and μ-η1,η2-C6H4 groups, μ3-η1,η1,η2- and μ4-η1,η1,η 2,η2-benzyne ligands, and a metalated ferrocene nucleus that further interacts with an Ru3 cluster via a direct Fe-Ru donor bond. These complexes are formed by reactions involving addition of C-H bonds to clusters, C-H, P-(C5 ring), and P-(C6 ring) bond cleavage, and migration of H to C5 ring carbons to give ferrocenyl (Fe(η-C5H4)(η-C5H5)) groups. Crystal data are as follows. Ru3(μ-H){μ3-(η1,η 2-C6H4)PPh(η-C5H 4)Fe(η-C5H4PPh2)}(CO) 8: monoclinic, space group P21/c, a = 17.318 (4) A?, b = 11.635 (2) , c = 21.009 (9) A?, β = 110.72 (2)°, V = 3959.4 A?3, Z = 4; 3472 data with I ≥ 2.5σ(I) were refined to R = 0.071, Rw = 0.071. Ru3{(?-(C6H4)P-σ-C5H 4)Fe(σ-C5H4PPh 2)}(?-CO)(CO)8: monoclinic, space group C2/c, a = 16.050 (4) A?, b = 12.982 (7) A?, c = 35.317 (10) A?, β = 101.29 (2)°, V = 7216.3 A?3, Z = 8; 2932 data with I ≥ 2.5σ(I) were refined to R = 0.048, Rw = 0.039. Ru3(μ3-η1,η1,η 2-C6H4)(μ-PPh 2)(μ-PPhFc)(CO)7: monoclinic, space group P21/c, a = 11.090 (4) A?, b = 14.337 (3) A?, c = 24.680 (6) A?, β = 94.42 (4)°, V = 3912.4 A?3, Z = 4; 5887 data with I ≥ 2.5σ(I) were refined to R = 0.066, Rw = 0.066. Ru3(μ-H){μ-(η1,η5-PPh 2C5H3)Fe(η-C5H 4PPh2)}(CO)8: monoclinic, space group P21/c, a = 13.166 (5) A?, b = 14.665 (3) A?, c = 22.832 (10) A?, β = 96.59 (3)°, V = 4379.3 A?3, Z = 4; 3421 data with I ≥ 2.5σ(I) were refined to R = 0.068, Rw = 0.072. Ru4(μ4-PFc)(μ4-C6H 4)(μ-CO)(CO)10: monoclinic, space group P21/c, a = 14.872 (14) A?, b = 9.008 (6) A?, c = 22.600 (28) A?, β = 91.8 (1)°, V = 3026.1 A?3, Z = 4; 1993 data were refined to R = 0.111, Rw = 0.114, as a result of difficulties with modeling disordered electron density peaks associated with the heavy atoms.
