The synthesis and characterization of Re3(μ-H) 3(CO)9 - N(PMe3)n3- η222-C60) (n = 2, 3) complexes

Hongkyu Kang, Bo Keun Park, Md Arzu Miah, Hyunjoon Song, David G. Churchill, Sangwoo Park, Moon-Gun Choi, Joon T. Park

Research output: Contribution to journalArticle

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Abstract

Treatment of Re3(μ-H)3(CO) 9322: η2-C60) (1) with 2.2 equiv. of Me3NO in the presence of excess PMe3 in chlorobenzene (CB) gave the bisphosphine-substituted complex 1,2-Re3(μ-H)3(CO) 7(PMe3)232: η22-C60) as two diastereomers, 2a (major, 38%) and 2b (minor, 11%). The corresponding reaction of 1 with 3.3 equiv. of Me3NO, produced the trisphosphine-substituted isomeric product 1,2,3-Re3(μ-H)3(CO)6(PMe 3)3322: η2-C60) as two diastereomers, 3a (major, 37%) and 3b (minor, 15%). Complexes 2a-3b have been characterized by spectroscopic methods and elemental analyses. Single crystal X-ray diffraction studies were carried out for 2a and 3b. The hydrides were confirmed by 1H NMR spectroscopic method and directly located only for 3a by X-ray diffraction. The molecular structure of 2a confirms a face-capping μ3- η222-C60 ligand with one axial and one equatorial PMe3 ligand on adjacent rhenium atoms, whereas that for 3b exhibits pseudo-Cs symmetry with an additional equatorial PMe3 on the third rhenium atom. Molecular structures for 2b and 3a are proposed by axial PMe3 ligand placement and subsequent equatorial PMe3 placement, based on earlier observations of facile ligand site-exchange in closely related systems and were verified by 1H NMR spectroscopic method.

Original languageEnglish
Pages (from-to)4704-4711
Number of pages8
JournalJournal of Organometallic Chemistry
Volume690
Issue number21-22
DOIs
Publication statusPublished - 2005 Nov 1

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Carbon Monoxide
Ligands
Rhenium
ligands
rhenium
synthesis
Molecular Structure
X-Ray Diffraction
Molecular structure
molecular structure
Nuclear magnetic resonance
X ray diffraction
Atoms
nuclear magnetic resonance
chlorobenzenes
diffraction
Hydrides
hydrides
atoms
x rays

All Science Journal Classification (ASJC) codes

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

Cite this

Kang, Hongkyu ; Park, Bo Keun ; Miah, Md Arzu ; Song, Hyunjoon ; Churchill, David G. ; Park, Sangwoo ; Choi, Moon-Gun ; Park, Joon T. / The synthesis and characterization of Re3(μ-H) 3(CO)9 - N(PMe3)n3- η222-C60) (n = 2, 3) complexes. In: Journal of Organometallic Chemistry. 2005 ; Vol. 690, No. 21-22. pp. 4704-4711.
@article{4f77b3cd1098471e8db4073cffd7277f,
title = "The synthesis and characterization of Re3(μ-H) 3(CO)9 - N(PMe3)n(μ3- η2:η2:η2-C60) (n = 2, 3) complexes",
abstract = "Treatment of Re3(μ-H)3(CO) 9(μ3-η2:η2: η2-C60) (1) with 2.2 equiv. of Me3NO in the presence of excess PMe3 in chlorobenzene (CB) gave the bisphosphine-substituted complex 1,2-Re3(μ-H)3(CO) 7(PMe3)2(μ3-η2: η2:η2-C60) as two diastereomers, 2a (major, 38{\%}) and 2b (minor, 11{\%}). The corresponding reaction of 1 with 3.3 equiv. of Me3NO, produced the trisphosphine-substituted isomeric product 1,2,3-Re3(μ-H)3(CO)6(PMe 3)3(μ3-η2:η2: η2-C60) as two diastereomers, 3a (major, 37{\%}) and 3b (minor, 15{\%}). Complexes 2a-3b have been characterized by spectroscopic methods and elemental analyses. Single crystal X-ray diffraction studies were carried out for 2a and 3b. The hydrides were confirmed by 1H NMR spectroscopic method and directly located only for 3a by X-ray diffraction. The molecular structure of 2a confirms a face-capping μ3- η2:η2:η2-C60 ligand with one axial and one equatorial PMe3 ligand on adjacent rhenium atoms, whereas that for 3b exhibits pseudo-Cs symmetry with an additional equatorial PMe3 on the third rhenium atom. Molecular structures for 2b and 3a are proposed by axial PMe3 ligand placement and subsequent equatorial PMe3 placement, based on earlier observations of facile ligand site-exchange in closely related systems and were verified by 1H NMR spectroscopic method.",
author = "Hongkyu Kang and Park, {Bo Keun} and Miah, {Md Arzu} and Hyunjoon Song and Churchill, {David G.} and Sangwoo Park and Moon-Gun Choi and Park, {Joon T.}",
year = "2005",
month = "11",
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doi = "10.1016/j.jorganchem.2005.07.052",
language = "English",
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journal = "Journal of Organometallic Chemistry",
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Kang, H, Park, BK, Miah, MA, Song, H, Churchill, DG, Park, S, Choi, M-G & Park, JT 2005, 'The synthesis and characterization of Re3(μ-H) 3(CO)9 - N(PMe3)n3- η222-C60) (n = 2, 3) complexes', Journal of Organometallic Chemistry, vol. 690, no. 21-22, pp. 4704-4711. https://doi.org/10.1016/j.jorganchem.2005.07.052

The synthesis and characterization of Re3(μ-H) 3(CO)9 - N(PMe3)n3- η222-C60) (n = 2, 3) complexes. / Kang, Hongkyu; Park, Bo Keun; Miah, Md Arzu; Song, Hyunjoon; Churchill, David G.; Park, Sangwoo; Choi, Moon-Gun; Park, Joon T.

In: Journal of Organometallic Chemistry, Vol. 690, No. 21-22, 01.11.2005, p. 4704-4711.

Research output: Contribution to journalArticle

TY - JOUR

T1 - The synthesis and characterization of Re3(μ-H) 3(CO)9 - N(PMe3)n(μ3- η2:η2:η2-C60) (n = 2, 3) complexes

AU - Kang, Hongkyu

AU - Park, Bo Keun

AU - Miah, Md Arzu

AU - Song, Hyunjoon

AU - Churchill, David G.

AU - Park, Sangwoo

AU - Choi, Moon-Gun

AU - Park, Joon T.

PY - 2005/11/1

Y1 - 2005/11/1

N2 - Treatment of Re3(μ-H)3(CO) 9(μ3-η2:η2: η2-C60) (1) with 2.2 equiv. of Me3NO in the presence of excess PMe3 in chlorobenzene (CB) gave the bisphosphine-substituted complex 1,2-Re3(μ-H)3(CO) 7(PMe3)2(μ3-η2: η2:η2-C60) as two diastereomers, 2a (major, 38%) and 2b (minor, 11%). The corresponding reaction of 1 with 3.3 equiv. of Me3NO, produced the trisphosphine-substituted isomeric product 1,2,3-Re3(μ-H)3(CO)6(PMe 3)3(μ3-η2:η2: η2-C60) as two diastereomers, 3a (major, 37%) and 3b (minor, 15%). Complexes 2a-3b have been characterized by spectroscopic methods and elemental analyses. Single crystal X-ray diffraction studies were carried out for 2a and 3b. The hydrides were confirmed by 1H NMR spectroscopic method and directly located only for 3a by X-ray diffraction. The molecular structure of 2a confirms a face-capping μ3- η2:η2:η2-C60 ligand with one axial and one equatorial PMe3 ligand on adjacent rhenium atoms, whereas that for 3b exhibits pseudo-Cs symmetry with an additional equatorial PMe3 on the third rhenium atom. Molecular structures for 2b and 3a are proposed by axial PMe3 ligand placement and subsequent equatorial PMe3 placement, based on earlier observations of facile ligand site-exchange in closely related systems and were verified by 1H NMR spectroscopic method.

AB - Treatment of Re3(μ-H)3(CO) 9(μ3-η2:η2: η2-C60) (1) with 2.2 equiv. of Me3NO in the presence of excess PMe3 in chlorobenzene (CB) gave the bisphosphine-substituted complex 1,2-Re3(μ-H)3(CO) 7(PMe3)2(μ3-η2: η2:η2-C60) as two diastereomers, 2a (major, 38%) and 2b (minor, 11%). The corresponding reaction of 1 with 3.3 equiv. of Me3NO, produced the trisphosphine-substituted isomeric product 1,2,3-Re3(μ-H)3(CO)6(PMe 3)3(μ3-η2:η2: η2-C60) as two diastereomers, 3a (major, 37%) and 3b (minor, 15%). Complexes 2a-3b have been characterized by spectroscopic methods and elemental analyses. Single crystal X-ray diffraction studies were carried out for 2a and 3b. The hydrides were confirmed by 1H NMR spectroscopic method and directly located only for 3a by X-ray diffraction. The molecular structure of 2a confirms a face-capping μ3- η2:η2:η2-C60 ligand with one axial and one equatorial PMe3 ligand on adjacent rhenium atoms, whereas that for 3b exhibits pseudo-Cs symmetry with an additional equatorial PMe3 on the third rhenium atom. Molecular structures for 2b and 3a are proposed by axial PMe3 ligand placement and subsequent equatorial PMe3 placement, based on earlier observations of facile ligand site-exchange in closely related systems and were verified by 1H NMR spectroscopic method.

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JO - Journal of Organometallic Chemistry

JF - Journal of Organometallic Chemistry

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