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research article

Dynamics of silica-supported catalysts determined by combining solid-state NMR spectroscopy and DFT calculations

Blanc, Frederic
•
Basset, Jean-Marie
•
Coperet, Christophe
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2008
Journal of the American Chemical Society

The molecular dynamics of a series of organometallic complexes covalently bound to amorphous silica surfaces is determined experimentally using solid-state nuclear magnetic resonance (NMR) spectroscopy and density functional theory calculations (DFT). The determination is carried out for a series of alkylidene-based catalysts having the general formula [( SiO)M(ER)(=CHtBu)(R')] (M = Re, Ta, Mo or W; ER = CtBu, NAr or CH(2)tBu; R' = CH2tBu, NPh2, NC4H4). Proton-carbon dipolar coupling constants and carbon chemical shift anisotropies (CSA) are determined experimentally by solid-state NMR. Room-temperature molecular dynamics is quantified through order parameters determined from the experimental data. For the chemical shift anisotropy data, we validate and use a method that integrates static values for the CSA obtained computationally by DFT, obviating the need for low-temperature measurements. Comparison of the room-temperature data with the calculations shows that the widths of the calculated static limit dipolar couplings and CSAs are always greater than the experimentally determined values, providing a clear indication of motional averaging on the NMR time scale. Moreover, the dynamics are found to be significantly different within the series of molecular complexes, with order parameters ranging from = 0.5 for [( SiO)Ta(=CHtBu)(CH(2)tBu)(2)] and [( SiO)Re( CtBu)(=CHtBu)(CH(2)tBu)] to = 0.9 for [( SiO)Mo( NAr)(=CHtBu)(R') with R' = CH(2)tBu, NPh2, NC4H4. The data also show that the motion is not isotropic and could be either a jump between two sites or more likely restricted librational motion. The dynamics are discussed in terms of the molecular structure of the surface organometallic complexes, and the orientation of the CSAs tensor at the alkylidene carbon is shown to be directly related to the magnitude of the alpha-alkylidene CH agostic interation.

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Type
research article
DOI
10.1021/ja077749v
Web of Science ID

WOS:000255629400027

Author(s)
Blanc, Frederic
Basset, Jean-Marie
Coperet, Christophe
Sinha, Amritanshu
Tonzetich, Zachary J.
Schrock, Richard R.
Solans-Monfort, Xavier
Clot, Eric
Eisenstein, Odile
Lesage, Anne
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Date Issued

2008

Publisher

AMER CHEMICAL SOC

Published in
Journal of the American Chemical Society
Volume

130

Issue

18

Start page

5886

End page

5900

Editorial or Peer reviewed

REVIEWED

Written at

OTHER

EPFL units
LRM  
Available on Infoscience
January 8, 2015
Use this identifier to reference this record
https://infoscience.epfl.ch/handle/20.500.14299/110055
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