2017
DOI: 10.1039/c6dt04475a
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A base-free synthetic route to anti-bimetallic lanthanide pentalene complexes

Abstract: Homobimetallic complexes of Yb, Eu and Sm bridged by a silylated pentalene ligand have been prepared and intermetallic communication studied by magnetic measurements and cyclic voltammetry.

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Cited by 13 publications
(2 citation statements)
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“…Most of the complexes obtained with these starting materials are homoleptic derivatives, with varying coordination numbers depending on the presence of coordinated solvents, ligand denticity, and steric properties. Salt elimination reactions have been employed for several decades in the preparation of cyclopentadienyl derivatives, such as the archetypal [Ln­(Cp*) 2 (THF) 2 ] ( 93-Ln ; Ln = Sm, Yb; Slv = Et 2 O, THF). , Metallocene-type Ln­(Cp) 2 complexes can be obtained by reacting group 1 cyclopentadienyl salts with SmI 2 , EuI 2 , and YbI 2 ( 93-Yb can also be obtained from YbCl 2 ) and are isolated either as solvent-free or solvated adducts of formula [Ln­(Cp R ) 2 (Slv) x ] ( x = 0–2; 1 , Cp R = Cp; 73-Ln , Cp R = Cp iPr5 ; 93-Ln Cp R = Cp*; 102 R -Ln , Cp′, Cp″, Cp‴, Cp Naph , Cp SiPh3 , Cp SiPh2Me , Cp tt , Cp ttt , Cp iPr4 , Cp Bn5 ,) (Cp′ = {C 5 H 3 SiMe 3 } − , Cp″ = {C 5 H 3 (SiMe 3 ) 2 -1,3} − , Cp‴ = {C 5 H 3 (SiMe 3 ) 3 -1,2,4} − , Cp tt = {C 5 H 3 t Bu 2 -1,3} − , Cp ttt = {C 5 H 3 t Bu 3 -1,3} − , Cp Bn5 = {C 5 (CH 2 Ph) 5 } − ) (Scheme ). These methodologies are more problematic with the highly reducing salts NdI 2 , DyI 2 , and TmI 2 .…”
Section: Halidessupporting
confidence: 65%
“…Most of the complexes obtained with these starting materials are homoleptic derivatives, with varying coordination numbers depending on the presence of coordinated solvents, ligand denticity, and steric properties. Salt elimination reactions have been employed for several decades in the preparation of cyclopentadienyl derivatives, such as the archetypal [Ln­(Cp*) 2 (THF) 2 ] ( 93-Ln ; Ln = Sm, Yb; Slv = Et 2 O, THF). , Metallocene-type Ln­(Cp) 2 complexes can be obtained by reacting group 1 cyclopentadienyl salts with SmI 2 , EuI 2 , and YbI 2 ( 93-Yb can also be obtained from YbCl 2 ) and are isolated either as solvent-free or solvated adducts of formula [Ln­(Cp R ) 2 (Slv) x ] ( x = 0–2; 1 , Cp R = Cp; 73-Ln , Cp R = Cp iPr5 ; 93-Ln Cp R = Cp*; 102 R -Ln , Cp′, Cp″, Cp‴, Cp Naph , Cp SiPh3 , Cp SiPh2Me , Cp tt , Cp ttt , Cp iPr4 , Cp Bn5 ,) (Cp′ = {C 5 H 3 SiMe 3 } − , Cp″ = {C 5 H 3 (SiMe 3 ) 2 -1,3} − , Cp‴ = {C 5 H 3 (SiMe 3 ) 3 -1,2,4} − , Cp tt = {C 5 H 3 t Bu 2 -1,3} − , Cp ttt = {C 5 H 3 t Bu 3 -1,3} − , Cp Bn5 = {C 5 (CH 2 Ph) 5 } − ) (Scheme ). These methodologies are more problematic with the highly reducing salts NdI 2 , DyI 2 , and TmI 2 .…”
Section: Halidessupporting
confidence: 65%
“…While the cyclopentadienyl rings of the Cp iPr5 ligands show small differences in C–C bond distances, the LnCp 2 core possesses approximate D 5 d symmetry, excluding isopropyl groups, with a dihedral angle of approximately 36° (dihedral angle ranges from 35.8(3) to 36.2(3)° in 1-Gd ). Of note, a linear geometry is uncommon for lanthanide metallocene complexes. Even in the crystal structure of Sm­(Cp BIG ) 2 (Cp BIG = (4- n Bu-C 6 H 4 ) 5 C 5 ), which features parallel Cp rings, the thermal displacement parameters of the Sm 2+ center are expanded in the plane between the cyclopentadienyl ligands, suggesting a deviation from linearity. , In contrast, the thermal displacement parameters of the Ln 2+ in 1-Ln are not expanded in this manner. The linear coordination geometry of the 1-Ln complexes likely arises from the high symmetry, steric bulk, and strong ligand field of the Cp iPr5 ligand.…”
Section: Resultsmentioning
confidence: 99%