Dehydrogenation of organolanthanide alkoxides and X-ray crystal structures of the reaction product [{(C5H5)2Ln(μ-O(Me)CCHCH3)}2] (Ln Dy Yb)

Zhongzhi Wu, Xu Zheng, You Xiaozeng, Zhou Xigeng, Huang Xiaoying

Research output: Contribution to journalArticle

30 Citations (Scopus)

Abstract

Reaction Of Cp3Ln (CpC5H5; Ln Dy, Yb) with 2-butanol in THF (THF = tetrahydrofuran) at room temperature yielded the complexes [Cp2Ln(μ-OCH(Me)CH2CH3)]2 [Ln Dy (1, Yb (2)], which have been characterized by elemental analysis, IR and MS spectra. The complexes 1 and 2 have been dehydrogenated to give the new enolate complexes [Cp2Ln(μ-O(Me)CCHCH3)]2 [Ln Dy (3), Yb (4)] upon refluxing in THF solution. The new complexes 3 and 4 have been structurally characterized by single-crystal diffraction studies. Complexes 3 and 4 crystallize from THF solution as isomorphous crystals of space group Pnnm with the following unit cell parameters: 3[4]; a = 9.910(5X9.853 (3)], b = 10.940(2)[10.917(3)] c = 12.258(2) [12.151(3)] Å, V= 1329(1)1307(1)] Å3, Z = 2, Dc = 1.82[1.90] g cm-3, R = 0.025[0.042], Rw = 0.036[0.0491. The molecules are oxygen-bridged dimers. The bridging unit Ln2O2 is completely planar. The metal atom is coordinated by two η5-Cp groups and two oxygen atoms of enolate ligands to form a pseudotetrahedral geometry. The average LnC bond lengths for 3 and 4 are 2.668(6) and 2.629(9) Å, respectively. The LnC distances of 3 and 4 are 2.256(4) and 2.210(2) Å, respectively. Complex 4 has been hydrolysed to give the organic compound CH3COCH2CH3, which has been confirmed by NMR spectra.

Original languageEnglish (US)
Pages (from-to)107-113
Number of pages7
JournalJournal of Organometallic Chemistry
Volume483
Issue number1-2
DOIs
StatePublished - Dec 13 1994

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alkoxides
Dehydrogenation
dehydrogenation
Reaction products
reaction products
Crystal structure
X-Rays
Oxygen
X rays
Atoms
crystal structure
Bond length
tetrahydrofuran
Butenes
organic compounds
Organic compounds
Dimers
oxygen atoms
x rays
Diffraction

All Science Journal Classification (ASJC) codes

  • Biochemistry
  • Physical and Theoretical Chemistry
  • Organic Chemistry
  • Inorganic Chemistry
  • Materials Chemistry

Cite this

Dehydrogenation of organolanthanide alkoxides and X-ray crystal structures of the reaction product [{(C5H5)2Ln(μ-O(Me)CCHCH3)}2] (Ln Dy Yb). / Wu, Zhongzhi; Zheng, Xu; Xiaozeng, You; Xigeng, Zhou; Xiaoying, Huang.

In: Journal of Organometallic Chemistry, Vol. 483, No. 1-2, 13.12.1994, p. 107-113.

Research output: Contribution to journalArticle

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title = "Dehydrogenation of organolanthanide alkoxides and X-ray crystal structures of the reaction product [{(C5H5)2Ln(μ-O(Me)CCHCH3)}2] (Ln Dy Yb)",
abstract = "Reaction Of Cp3Ln (CpC5H5; Ln Dy, Yb) with 2-butanol in THF (THF = tetrahydrofuran) at room temperature yielded the complexes [Cp2Ln(μ-OCH(Me)CH2CH3)]2 [Ln Dy (1, Yb (2)], which have been characterized by elemental analysis, IR and MS spectra. The complexes 1 and 2 have been dehydrogenated to give the new enolate complexes [Cp2Ln(μ-O(Me)CCHCH3)]2 [Ln Dy (3), Yb (4)] upon refluxing in THF solution. The new complexes 3 and 4 have been structurally characterized by single-crystal diffraction studies. Complexes 3 and 4 crystallize from THF solution as isomorphous crystals of space group Pnnm with the following unit cell parameters: 3[4]; a = 9.910(5X9.853 (3)], b = 10.940(2)[10.917(3)] c = 12.258(2) [12.151(3)] {\AA}, V= 1329(1)1307(1)] {\AA}3, Z = 2, Dc = 1.82[1.90] g cm-3, R = 0.025[0.042], Rw = 0.036[0.0491. The molecules are oxygen-bridged dimers. The bridging unit Ln2O2 is completely planar. The metal atom is coordinated by two η5-Cp groups and two oxygen atoms of enolate ligands to form a pseudotetrahedral geometry. The average LnC bond lengths for 3 and 4 are 2.668(6) and 2.629(9) {\AA}, respectively. The LnC distances of 3 and 4 are 2.256(4) and 2.210(2) {\AA}, respectively. Complex 4 has been hydrolysed to give the organic compound CH3COCH2CH3, which has been confirmed by NMR spectra.",
author = "Zhongzhi Wu and Xu Zheng and You Xiaozeng and Zhou Xigeng and Huang Xiaoying",
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T1 - Dehydrogenation of organolanthanide alkoxides and X-ray crystal structures of the reaction product [{(C5H5)2Ln(μ-O(Me)CCHCH3)}2] (Ln Dy Yb)

AU - Wu, Zhongzhi

AU - Zheng, Xu

AU - Xiaozeng, You

AU - Xigeng, Zhou

AU - Xiaoying, Huang

PY - 1994/12/13

Y1 - 1994/12/13

N2 - Reaction Of Cp3Ln (CpC5H5; Ln Dy, Yb) with 2-butanol in THF (THF = tetrahydrofuran) at room temperature yielded the complexes [Cp2Ln(μ-OCH(Me)CH2CH3)]2 [Ln Dy (1, Yb (2)], which have been characterized by elemental analysis, IR and MS spectra. The complexes 1 and 2 have been dehydrogenated to give the new enolate complexes [Cp2Ln(μ-O(Me)CCHCH3)]2 [Ln Dy (3), Yb (4)] upon refluxing in THF solution. The new complexes 3 and 4 have been structurally characterized by single-crystal diffraction studies. Complexes 3 and 4 crystallize from THF solution as isomorphous crystals of space group Pnnm with the following unit cell parameters: 3[4]; a = 9.910(5X9.853 (3)], b = 10.940(2)[10.917(3)] c = 12.258(2) [12.151(3)] Å, V= 1329(1)1307(1)] Å3, Z = 2, Dc = 1.82[1.90] g cm-3, R = 0.025[0.042], Rw = 0.036[0.0491. The molecules are oxygen-bridged dimers. The bridging unit Ln2O2 is completely planar. The metal atom is coordinated by two η5-Cp groups and two oxygen atoms of enolate ligands to form a pseudotetrahedral geometry. The average LnC bond lengths for 3 and 4 are 2.668(6) and 2.629(9) Å, respectively. The LnC distances of 3 and 4 are 2.256(4) and 2.210(2) Å, respectively. Complex 4 has been hydrolysed to give the organic compound CH3COCH2CH3, which has been confirmed by NMR spectra.

AB - Reaction Of Cp3Ln (CpC5H5; Ln Dy, Yb) with 2-butanol in THF (THF = tetrahydrofuran) at room temperature yielded the complexes [Cp2Ln(μ-OCH(Me)CH2CH3)]2 [Ln Dy (1, Yb (2)], which have been characterized by elemental analysis, IR and MS spectra. The complexes 1 and 2 have been dehydrogenated to give the new enolate complexes [Cp2Ln(μ-O(Me)CCHCH3)]2 [Ln Dy (3), Yb (4)] upon refluxing in THF solution. The new complexes 3 and 4 have been structurally characterized by single-crystal diffraction studies. Complexes 3 and 4 crystallize from THF solution as isomorphous crystals of space group Pnnm with the following unit cell parameters: 3[4]; a = 9.910(5X9.853 (3)], b = 10.940(2)[10.917(3)] c = 12.258(2) [12.151(3)] Å, V= 1329(1)1307(1)] Å3, Z = 2, Dc = 1.82[1.90] g cm-3, R = 0.025[0.042], Rw = 0.036[0.0491. The molecules are oxygen-bridged dimers. The bridging unit Ln2O2 is completely planar. The metal atom is coordinated by two η5-Cp groups and two oxygen atoms of enolate ligands to form a pseudotetrahedral geometry. The average LnC bond lengths for 3 and 4 are 2.668(6) and 2.629(9) Å, respectively. The LnC distances of 3 and 4 are 2.256(4) and 2.210(2) Å, respectively. Complex 4 has been hydrolysed to give the organic compound CH3COCH2CH3, which has been confirmed by NMR spectra.

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