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Synthesis and characterization of an organoyttrium dimer produced via an Arbuzov dealkylation reaction

(1992) ORGANOMETALLICS. 11(10). p.3459-3462
Author
Organization
Abstract
The reaction of anhydrous YCl3 with 2 equiv of the sodium salt of the anionic tripod complex [(eta5-C5H5)CO{(CH3CH2O)2P=O}3}- (L(OEt)) in tetrahydrofuran, under anaerobic conditions, leads to the high-yield formation of [L(OEt)Y{(C5H5)Co(P(=O)(OEt)2)2(P(=O)(OEt)(O))}2YL(Oet)] (1). The complex has been characterized by standard analytical techniques. Nuclear magnetic resonance spectroscopic studies show a reduction of local symmetry of one of the ligands. To clearly illustrate the structural features of the isolated complex in the solid state, a low-temperature data collection X-ray crystallographic investigation was performed. This study reveals 1 to be a dimer with bridging phosphonate oxygens (monoclinic system, space group P2(1)/n, with a = 12.261 (4) angstrom, b = 21.110 (5) angstrom, c = 19.529 (5) angstrom, beta = 94.77 (2)-degrees, V = 5037 (6) angstrom3, Z = 2, T = 102 (2) K, and D(calcd) = 1.477 g/cm3). The structure also shows that one of the phosphonate ethyl groups has been cleaved in the course of the reaction. Analysis of the volatiles generated during the reaction clearly shows the formation of ethyl chloride, indicating that 1 is produced in con with the elimination of a phosphonate ethyl group in an Arbuzov-type dealkylation.
Keywords
METAL-OXIDE ANALOGS, ATOMICALLY DISPERSED IRIDIUM(I), TERTIARY PHOSPHINE COMPLEXES, RAY CRYSTAL-STRUCTURE, OXYGEN TRIPOD LIGAND, O-DONOR LIGAND, F-BLOCK METALS, TRISUBSTITUTED HETEROPOLYTUNGSTATES, ORGANOMETALLIC CHEMISTRY, ALKYNE HYDROSILYLATION

Citation

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Chicago
Liang, L, ED Stevens, and Steven Nolan. 1992. “Synthesis and Characterization of an Organoyttrium Dimer Produced via an Arbuzov Dealkylation Reaction.” Organometallics 11 (10): 3459–3462.
APA
Liang, L., Stevens, E., & Nolan, S. (1992). Synthesis and characterization of an organoyttrium dimer produced via an Arbuzov dealkylation reaction. ORGANOMETALLICS, 11(10), 3459–3462.
Vancouver
1.
Liang L, Stevens E, Nolan S. Synthesis and characterization of an organoyttrium dimer produced via an Arbuzov dealkylation reaction. ORGANOMETALLICS. 1992;11(10):3459–62.
MLA
Liang, L, ED Stevens, and Steven Nolan. “Synthesis and Characterization of an Organoyttrium Dimer Produced via an Arbuzov Dealkylation Reaction.” ORGANOMETALLICS 11.10 (1992): 3459–3462. Print.
@article{8171461,
  abstract     = {The reaction of anhydrous YCl3 with 2 equiv of the sodium salt of the anionic tripod complex [(eta5-C5H5)CO\{(CH3CH2O)2P=O\}3\}- (L(OEt)) in tetrahydrofuran, under anaerobic conditions, leads to the high-yield formation of [L(OEt)Y\{(C5H5)Co(P(=O)(OEt)2)2(P(=O)(OEt)(O))\}2YL(Oet)] (1). The complex has been characterized by standard analytical techniques. Nuclear magnetic resonance spectroscopic studies show a reduction of local symmetry of one of the ligands. To clearly illustrate the structural features of the isolated complex in the solid state, a low-temperature data collection X-ray crystallographic investigation was performed. This study reveals 1 to be a dimer with bridging phosphonate oxygens (monoclinic system, space group P2(1)/n, with a = 12.261 (4) angstrom, b = 21.110 (5) angstrom, c = 19.529 (5) angstrom, beta = 94.77 (2)-degrees, V = 5037 (6) angstrom3, Z = 2, T = 102 (2) K, and D(calcd) = 1.477 g/cm3). The structure also shows that one of the phosphonate ethyl groups has been cleaved in the course of the reaction. Analysis of the volatiles generated during the reaction clearly shows the formation of ethyl chloride, indicating that 1 is produced in con with the elimination of a phosphonate ethyl group in an Arbuzov-type dealkylation.},
  author       = {Liang, L and Stevens, ED and Nolan, Steven},
  issn         = {0276-7333},
  journal      = {ORGANOMETALLICS},
  language     = {eng},
  number       = {10},
  pages        = {3459--3462},
  title        = {Synthesis and characterization of an organoyttrium dimer produced via an Arbuzov dealkylation reaction},
  url          = {http://dx.doi.org/10.1021/om00046a055},
  volume       = {11},
  year         = {1992},
}

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