TY - JOUR
T1 - Synthesis and structural characterization of mesitylphosphinidene-capped ruthenium and osmium clusters
AU - Kakizawa, Taeko
AU - Hashimoto, Hisako
AU - Tobita, Hiromi
N1 - Funding Information:
This work was supported by the 21st century Center of Excellence (COE) program ‘Giant Molecules and Complex Systems’ of MEXT hosted at Tohoku University.
PY - 2006/2/1
Y1 - 2006/2/1
N2 - Thermal reaction of [Ru3(CO)12] with PH 2Mes (Mes = mesityl) in refluxing toluene afforded mesitylphosphinidene-capped ruthenium carbonyl clusters, [Ru 3(CO)9(μ-H)2(μ3-PMes)] (1), [Ru3(CO)8(PH2Mes)(μ-H)2(μ 3-PMes)] (2), [Ru3(CO)9(μ 3-PMes)2] (3), [Ru4(CO) 10(μ-CO)(μ4-PMes)2] (4), and [Ru 5(CO)10H2(μ4-PMes)(μ 3-PMes)2] (5). All products were fully characterized and structurally confirmed by X-ray crystal structure analysis. Complexes 2-4 were also obtained in high yields by stepwise reaction starting from 1. Fluxional behavior of carbonyl groups was observed in case of 4. Complex 5 reveals a new type of skeletal structure, bicapped-octahedron having μ3- and μ4-phosphinidene ligands at the capping positions. Similar reaction of [Os3(CO)12] with PH2Mes yielded a phosphido-bridged osmium cluster [Os3(CO) 10(μ-H)(μ-PHMes)] (6) and a phosphinidene-capped cluster [Os3(CO)9(μ-H)2(μ3-PMes)] (7).
AB - Thermal reaction of [Ru3(CO)12] with PH 2Mes (Mes = mesityl) in refluxing toluene afforded mesitylphosphinidene-capped ruthenium carbonyl clusters, [Ru 3(CO)9(μ-H)2(μ3-PMes)] (1), [Ru3(CO)8(PH2Mes)(μ-H)2(μ 3-PMes)] (2), [Ru3(CO)9(μ 3-PMes)2] (3), [Ru4(CO) 10(μ-CO)(μ4-PMes)2] (4), and [Ru 5(CO)10H2(μ4-PMes)(μ 3-PMes)2] (5). All products were fully characterized and structurally confirmed by X-ray crystal structure analysis. Complexes 2-4 were also obtained in high yields by stepwise reaction starting from 1. Fluxional behavior of carbonyl groups was observed in case of 4. Complex 5 reveals a new type of skeletal structure, bicapped-octahedron having μ3- and μ4-phosphinidene ligands at the capping positions. Similar reaction of [Os3(CO)12] with PH2Mes yielded a phosphido-bridged osmium cluster [Os3(CO) 10(μ-H)(μ-PHMes)] (6) and a phosphinidene-capped cluster [Os3(CO)9(μ-H)2(μ3-PMes)] (7).
KW - Cluster
KW - Mesitylphosphine
KW - Phosphinidene ligand
KW - X-ray structure study
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U2 - 10.1016/j.jorganchem.2005.10.011
DO - 10.1016/j.jorganchem.2005.10.011
M3 - Article
AN - SCOPUS:30844465007
SN - 0022-328X
VL - 691
SP - 726
EP - 736
JO - Journal of Organometallic Chemistry
JF - Journal of Organometallic Chemistry
IS - 4
ER -