Synthesis and characterization five-coordinate molybdenum compounds bearing bi- or tridentate substituted pyrrole ligands: Molecular structures of {Mo(NC6H3Pri2-2,6)2 R[NC4H3(CH2NMe2)-2]}

Jui Hsien Huang, Hsing Jen Chen, Chung Ching Hsieh, Gene Hsiang Lee, Shie Ming Peng

Research output: Contribution to journalArticle

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Abstract

Reacting [Mo(NC6H3Pri2-2,6)2Cl 2(dme)] with 1 equiv. of Li [NC4H3(CH2NMe2)-2] in diethyl ether at -78°C yields a red crystalline solid of {Mo(NC6H3Pri2-2,6)2Cl [NC4H3(CH2NMe2)-2]} 1 in 86% yield. Alkylation of 1 with RLi in diethyl ether generates {Mo(NC6H3Pri2-2,6)2 R[NC4H3(CH2NMe2)-2]} (2a, R = Me; 2b, R = Bu) in high yield. Similarly, reacting [Mo(NC6H3Pri2-2,6)2Cl 2(dme)] with 1 equiv. of Li[NC4H2(CH2NMe2)2- 2,5] in diethyl ether at -78°C affords dark red crystals of {Mo(NC6H3Pri2-2,6)2Cl [NC4H2(CH2NMe2)2-2,5]} 3 in 92% yield, in which one NMe2 unit of the pyrrole ligand of 3 coordinates to molybdenum whilst the other one dangles outside the coordination sphere. Variable-temperature 1H NMR study of 3 reveals fluxional behavior of the two NMe2 units of the pyrrole ligand. The activation energy of the fluxionality has been determined as ΔG = 10.5 kcal mol-1. Compounds 1, 2a, 2b and 3 have been characterized by NMR spectroscopy and X-ray crystallography.

Original languageEnglish
Pages (from-to)142-148
Number of pages7
JournalInorganica Chimica Acta
Volume321
Issue number1-2
DOIs
Publication statusPublished - 2001 Sep 10

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Bearings (structural)
Molybdenum compounds
molybdenum compounds
diethyl ether
Pyrroles
pyrroles
Ether
Molecular structure
Ethers
molecular structure
Ligands
ligands
synthesis
nuclear magnetic resonance
Molybdenum
X ray crystallography
alkylation
Alkylation
Nuclear magnetic resonance spectroscopy
crystallography

All Science Journal Classification (ASJC) codes

  • Physical and Theoretical Chemistry
  • Inorganic Chemistry
  • Materials Chemistry

Cite this

@article{5183bca4ea304ecbb71938b91c97dbf2,
title = "Synthesis and characterization five-coordinate molybdenum compounds bearing bi- or tridentate substituted pyrrole ligands: Molecular structures of {Mo(NC6H3Pri2-2,6)2 R[NC4H3(CH2NMe2)-2]}",
abstract = "Reacting [Mo(NC6H3Pri2-2,6)2Cl 2(dme)] with 1 equiv. of Li [NC4H3(CH2NMe2)-2] in diethyl ether at -78°C yields a red crystalline solid of {Mo(NC6H3Pri2-2,6)2Cl [NC4H3(CH2NMe2)-2]} 1 in 86{\%} yield. Alkylation of 1 with RLi in diethyl ether generates {Mo(NC6H3Pri2-2,6)2 R[NC4H3(CH2NMe2)-2]} (2a, R = Me; 2b, R = Bu) in high yield. Similarly, reacting [Mo(NC6H3Pri2-2,6)2Cl 2(dme)] with 1 equiv. of Li[NC4H2(CH2NMe2)2- 2,5] in diethyl ether at -78°C affords dark red crystals of {Mo(NC6H3Pri2-2,6)2Cl [NC4H2(CH2NMe2)2-2,5]} 3 in 92{\%} yield, in which one NMe2 unit of the pyrrole ligand of 3 coordinates to molybdenum whilst the other one dangles outside the coordination sphere. Variable-temperature 1H NMR study of 3 reveals fluxional behavior of the two NMe2 units of the pyrrole ligand. The activation energy of the fluxionality has been determined as ΔG≠ = 10.5 kcal mol-1. Compounds 1, 2a, 2b and 3 have been characterized by NMR spectroscopy and X-ray crystallography.",
author = "Huang, {Jui Hsien} and Chen, {Hsing Jen} and Hsieh, {Chung Ching} and Lee, {Gene Hsiang} and Peng, {Shie Ming}",
year = "2001",
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language = "English",
volume = "321",
pages = "142--148",
journal = "Inorganica Chimica Acta",
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}

Synthesis and characterization five-coordinate molybdenum compounds bearing bi- or tridentate substituted pyrrole ligands : Molecular structures of {Mo(NC6H3Pri2-2,6)2 R[NC4H3(CH2NMe2)-2]}. / Huang, Jui Hsien; Chen, Hsing Jen; Hsieh, Chung Ching; Lee, Gene Hsiang; Peng, Shie Ming.

In: Inorganica Chimica Acta, Vol. 321, No. 1-2, 10.09.2001, p. 142-148.

Research output: Contribution to journalArticle

TY - JOUR

T1 - Synthesis and characterization five-coordinate molybdenum compounds bearing bi- or tridentate substituted pyrrole ligands

T2 - Molecular structures of {Mo(NC6H3Pri2-2,6)2 R[NC4H3(CH2NMe2)-2]}

AU - Huang, Jui Hsien

AU - Chen, Hsing Jen

AU - Hsieh, Chung Ching

AU - Lee, Gene Hsiang

AU - Peng, Shie Ming

PY - 2001/9/10

Y1 - 2001/9/10

N2 - Reacting [Mo(NC6H3Pri2-2,6)2Cl 2(dme)] with 1 equiv. of Li [NC4H3(CH2NMe2)-2] in diethyl ether at -78°C yields a red crystalline solid of {Mo(NC6H3Pri2-2,6)2Cl [NC4H3(CH2NMe2)-2]} 1 in 86% yield. Alkylation of 1 with RLi in diethyl ether generates {Mo(NC6H3Pri2-2,6)2 R[NC4H3(CH2NMe2)-2]} (2a, R = Me; 2b, R = Bu) in high yield. Similarly, reacting [Mo(NC6H3Pri2-2,6)2Cl 2(dme)] with 1 equiv. of Li[NC4H2(CH2NMe2)2- 2,5] in diethyl ether at -78°C affords dark red crystals of {Mo(NC6H3Pri2-2,6)2Cl [NC4H2(CH2NMe2)2-2,5]} 3 in 92% yield, in which one NMe2 unit of the pyrrole ligand of 3 coordinates to molybdenum whilst the other one dangles outside the coordination sphere. Variable-temperature 1H NMR study of 3 reveals fluxional behavior of the two NMe2 units of the pyrrole ligand. The activation energy of the fluxionality has been determined as ΔG≠ = 10.5 kcal mol-1. Compounds 1, 2a, 2b and 3 have been characterized by NMR spectroscopy and X-ray crystallography.

AB - Reacting [Mo(NC6H3Pri2-2,6)2Cl 2(dme)] with 1 equiv. of Li [NC4H3(CH2NMe2)-2] in diethyl ether at -78°C yields a red crystalline solid of {Mo(NC6H3Pri2-2,6)2Cl [NC4H3(CH2NMe2)-2]} 1 in 86% yield. Alkylation of 1 with RLi in diethyl ether generates {Mo(NC6H3Pri2-2,6)2 R[NC4H3(CH2NMe2)-2]} (2a, R = Me; 2b, R = Bu) in high yield. Similarly, reacting [Mo(NC6H3Pri2-2,6)2Cl 2(dme)] with 1 equiv. of Li[NC4H2(CH2NMe2)2- 2,5] in diethyl ether at -78°C affords dark red crystals of {Mo(NC6H3Pri2-2,6)2Cl [NC4H2(CH2NMe2)2-2,5]} 3 in 92% yield, in which one NMe2 unit of the pyrrole ligand of 3 coordinates to molybdenum whilst the other one dangles outside the coordination sphere. Variable-temperature 1H NMR study of 3 reveals fluxional behavior of the two NMe2 units of the pyrrole ligand. The activation energy of the fluxionality has been determined as ΔG≠ = 10.5 kcal mol-1. Compounds 1, 2a, 2b and 3 have been characterized by NMR spectroscopy and X-ray crystallography.

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