TY - JOUR
T1 - The triruthenium cluster anion [Ru3H(CO)11]-
T2 - Preparation, structure, and fluxionality
AU - Johnson, Brian F.G.
AU - Lewis, Jack
AU - Raithby, Paul R.
AU - Süss, Georg
PY - 1979/12/31
Y1 - 1979/12/31
N2 - The cluster anion [Ru3H(CO)11]- has been prepared in high yields by the reaction of [Ru3(CO)12] with Na[BH4] in tetrahydrofuran. The anion is isolated as the tetraethylammonium and the bis (triphenylphosphine) iminium salts. The salt [N(PPh3)2][Ru3H(CO)11] crystallizes in the monoclinic space group P21/c, with the cell dimensions a = 16.355(5), b = 17.057(4), c = 17.715(5) Å, β = 106.29(2)°, and Z = 4. The structure has been solved by a combination of multisolution sign-expansion and Fourier-difference methods, and refined to R 0.053 for 4 341 observed intensities. The three ruthenium atoms define an isosceles triangle, the shortest edge of which is symmetrically bridged by a carbonyl group and a hydride ligand. A variable-temperature 13C n.m.r. study of [NEt4][Ru3H(CO)11] reveals the anion to be fluxional in solution; the spectra are indicative of several dynamic processes occurring over the range -116 to 32 °C which are distinctly different from those proposed for the iron analogue [Fe3H(CO)11]-.
AB - The cluster anion [Ru3H(CO)11]- has been prepared in high yields by the reaction of [Ru3(CO)12] with Na[BH4] in tetrahydrofuran. The anion is isolated as the tetraethylammonium and the bis (triphenylphosphine) iminium salts. The salt [N(PPh3)2][Ru3H(CO)11] crystallizes in the monoclinic space group P21/c, with the cell dimensions a = 16.355(5), b = 17.057(4), c = 17.715(5) Å, β = 106.29(2)°, and Z = 4. The structure has been solved by a combination of multisolution sign-expansion and Fourier-difference methods, and refined to R 0.053 for 4 341 observed intensities. The three ruthenium atoms define an isosceles triangle, the shortest edge of which is symmetrically bridged by a carbonyl group and a hydride ligand. A variable-temperature 13C n.m.r. study of [NEt4][Ru3H(CO)11] reveals the anion to be fluxional in solution; the spectra are indicative of several dynamic processes occurring over the range -116 to 32 °C which are distinctly different from those proposed for the iron analogue [Fe3H(CO)11]-.
UR - http://www.scopus.com/inward/record.url?scp=37049100372&partnerID=8YFLogxK
U2 - 10.1039/DT9790001356
DO - 10.1039/DT9790001356
M3 - Article
AN - SCOPUS:37049100372
SN - 1472-7773
SP - 1356
EP - 1361
JO - Journal of the Chemical Society, Dalton Transactions
JF - Journal of the Chemical Society, Dalton Transactions
IS - 9
ER -