Transition Met Chem

2013

DOI: 10.1007/s11243-013-9796-3

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Reactivity of triosmium clusters with 3,4-dimethyl-1-phenylphosphole and cyanoethyldi-tert-butylphosphine ligands: X-ray crystal structures of [Os3(CO)9(μ-OH)(μ-H)(η1-PhPC4H2Me2)] and [Os3(CO)11(η1- t Bu2PC2H4CN)]

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Ysaura De Sanctis

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et al.

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Cited by 4 publications

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“…CO)11 PR 3 ] clusters. The Os(2)-P(1) bond length [2.349(6) Å] is very similar to those reported for related complexes[17,[37][38][39].…”

supporting

confidence: 79%

Fluxional behaviour of phosphole and phosphine ligands on triosmium clusters

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et al. 2015

Journal of Organometallic Chemistry

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The unsaturated cluster [Os 3 (µ-H) 2 (CO) 10 ] reacts with a variety of-conjugated phosphole ligands: 2,5-bis(2-thienyl)-1-phenylphosphole, 2,5-bis(2-pyridyl)-1-phenylphosphole, and 1,2,5triphenylphosphole, to give the monosubstituted [Os 3 (µ-H)(H)(CO) 10 (P)] and [Os 3 (µ-H) 2 (CO) 9 (P)] derivatives. Variable-temperature 1 H NMR studies for the decacarbonyltriosmium complexes show that the hydride ligands undergo fluxional behavior and its decarbonylation gave the nonacarbonyl unsaturated species with equivalent hydrides. An X-ray crystallographic analysis of [Os 3 (µ-H) 2 (CO) 9 (P)] (2b) (P = 1,2,5-triphenylphosphole) is reported. From 2,5-bis(2-pyridyl)-1phenylphosphole four isomers are obtained, the 1 H NMR spectrum at low temperature indicates that the phosphole ligand may occupy pseudoaxial and equatorial sites at one of the osmium atoms bearing the bridging hydride. The reaction of [Os 3 (CO) 10 (CH 3 CN) 2 ] with cyanoethyldiphenylphosphine affords mono-and bis(phosphine)-substituted clusters. The X-ray crystal structure of the monosubstituted [Os 3 (CO) 11 (η 1-PC 15 H 14 N)] (3) derivative is discussed. The dynamic behavior observed for [Os 3 (CO) 10 (η 1-PC 15 H 14 N) 2 ] (4) is studied by variable-temperature 1 H and 31 P{ 1 H} NMR spectroscopy. The latter studies show a mixture of two geometric isomers,

“…CO)11 PR 3 ] clusters. The Os(2)-P(1) bond length [2.349(6) Å] is very similar to those reported for related complexes[17,[37][38][39].…”

supporting

confidence: 79%

Fluxional behaviour of phosphole and phosphine ligands on triosmium clusters

¹

,

²

,

³

et al. 2015

Journal of Organometallic Chemistry

Self Cite

View full text Add to dashboard Cite

The unsaturated cluster [Os 3 (µ-H) 2 (CO) 10 ] reacts with a variety of-conjugated phosphole ligands: 2,5-bis(2-thienyl)-1-phenylphosphole, 2,5-bis(2-pyridyl)-1-phenylphosphole, and 1,2,5triphenylphosphole, to give the monosubstituted [Os 3 (µ-H)(H)(CO) 10 (P)] and [Os 3 (µ-H) 2 (CO) 9 (P)] derivatives. Variable-temperature 1 H NMR studies for the decacarbonyltriosmium complexes show that the hydride ligands undergo fluxional behavior and its decarbonylation gave the nonacarbonyl unsaturated species with equivalent hydrides. An X-ray crystallographic analysis of [Os 3 (µ-H) 2 (CO) 9 (P)] (2b) (P = 1,2,5-triphenylphosphole) is reported. From 2,5-bis(2-pyridyl)-1phenylphosphole four isomers are obtained, the 1 H NMR spectrum at low temperature indicates that the phosphole ligand may occupy pseudoaxial and equatorial sites at one of the osmium atoms bearing the bridging hydride. The reaction of [Os 3 (CO) 10 (CH 3 CN) 2 ] with cyanoethyldiphenylphosphine affords mono-and bis(phosphine)-substituted clusters. The X-ray crystal structure of the monosubstituted [Os 3 (CO) 11 (η 1-PC 15 H 14 N)] (3) derivative is discussed. The dynamic behavior observed for [Os 3 (CO) 10 (η 1-PC 15 H 14 N) 2 ] (4) is studied by variable-temperature 1 H and 31 P{ 1 H} NMR spectroscopy. The latter studies show a mixture of two geometric isomers,

Synthesis and characterization of trinuclear osmium clusters containing diallylphosphines as hemilabile ligands: Experimental and theoretical studies of their reactivity with nucleophilic molecules

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et al. 2014

Journal of Organometallic Chemistry

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Reactivity of dirhenium and triruthenium carbonyls toward a biphosphole ligand: M–M, P–P and C–H bonds cleavage

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et al. 2017

Journal of Organometallic Chemistry

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International audienceThe reaction of [Re2(CO)8(CH3CN)2] with bis(2-thienyl)biphosphole in refluxing n-octane affords the complex [Re(CO)3(η5-PC16H14S2)] (1) where cleavage of the Re–Re and P–P bonds occurs; its molecular structure confirms the formation of a rhenium mononuclear compound with a η5-coordinated phospholyl unit and three carbonyl groups oriented in a tripod. On the other hand, bis(2-thienyl)biphosphole reacts with [Ru3(CO)12] in refluxing cyclohexane to affording two new compounds [Ru3(CO)9(μ:η1:η5-PC16H13S2)] (2) and [Ru4(CO)13(μ:η1-PC16H14S2)2] (3). Spectroscopic data and theoretical studies of 2 suggest the formation of an open Ru3 cluster with two metal–metal bonds bridged by a (η1:η5-PC16H13S2) unit and a C-H bond activation of one of the thienyl substituents. X-ray structure of 3 reveals a novel tetranuclear ruthenium cluster containing 13 terminal carbonyl ligands and two phospholyl units coordinated as μ-phosphide

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