Structural Elucidation of (Silica)-O-Rh(allyl)2 by Correlated 1H and 13C NMR

H. Eric Fischer; Steven A. King; C. E. Bronnimann; Jeffrey Schwartz

doi:10.1021/la00026a007

Structural Elucidation of (Silica)-O-Rh(allyl)₂ by Correlated ¹H and ¹³C NMR

H. Eric Fischer, Steven A. King, C. E. Bronnimann, Jeffrey Schwartz

Research output: Contribution to journal › Letter › peer-review

11 Scopus citations

Abstract

The combined rotation and multiple pulse sequence technique was used to obtain ¹H NMR spectra of (silica)-O-Rh(allyl)₂, a reactive organometallic complex bound in low concentration on the surface of the oxide, and a model compound, [(η³-allyl)₂RhCl]₂. By spectral comparison with the model compound, a bis(η³-allyl)Rh structure seemed possible for the surface-bound complex, but broad line widths precluded a more definite structural assignment. The ¹³C-labeled complex (η³-allyl)(η³-[¹³C]allyl)₂Rh (in which either terminus of the allyl ligand was labeled) was prepared and deposited on silica. The resulting labeled surface complex was analyzed by both ¹³C cross-polarization magic angle spinning and the 2D ¹H-¹³C heteronuclear correlation technique. Spectral data were compared with those obtained for [(η³-[¹³C] allyl)₂-RhCl]₂ and support the bis(η³-allyl)Rh complex structural assignment for (silica)-O-Rh(allyl)₂.

Original language	English (US)
Pages (from-to)	391-393
Number of pages	3
Journal	Langmuir
Volume	9
Issue number	2
DOIs	https://doi.org/10.1021/la00026a007
State	Published - 1993

All Science Journal Classification (ASJC) codes

General Materials Science
Condensed Matter Physics
Surfaces and Interfaces
Spectroscopy
Electrochemistry

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10.1021/la00026a007

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@article{0388e2a937924e39872f736036acc2f8,

title = "Structural Elucidation of (Silica)-O-Rh(allyl)2 by Correlated 1H and 13C NMR",

abstract = "The combined rotation and multiple pulse sequence technique was used to obtain 1H NMR spectra of (silica)-O-Rh(allyl)2, a reactive organometallic complex bound in low concentration on the surface of the oxide, and a model compound, [(η3-allyl)2RhCl]2. By spectral comparison with the model compound, a bis(η3-allyl)Rh structure seemed possible for the surface-bound complex, but broad line widths precluded a more definite structural assignment. The 13C-labeled complex (η3-allyl)(η3-[13C]allyl)2Rh (in which either terminus of the allyl ligand was labeled) was prepared and deposited on silica. The resulting labeled surface complex was analyzed by both 13C cross-polarization magic angle spinning and the 2D 1H-13C heteronuclear correlation technique. Spectral data were compared with those obtained for [(η3-[13C] allyl)2-RhCl]2 and support the bis(η3-allyl)Rh complex structural assignment for (silica)-O-Rh(allyl)2.",

author = "Fischer, {H. Eric} and King, {Steven A.} and Bronnimann, {C. E.} and Jeffrey Schwartz",

year = "1993",

doi = "10.1021/la00026a007",

language = "English (US)",

volume = "9",

pages = "391--393",

journal = "Langmuir",

issn = "0743-7463",

publisher = "American Chemical Society",

number = "2",

}

TY - JOUR

T1 - Structural Elucidation of (Silica)-O-Rh(allyl)2 by Correlated 1H and 13C NMR

AU - Fischer, H. Eric

AU - King, Steven A.

AU - Bronnimann, C. E.

AU - Schwartz, Jeffrey

PY - 1993

Y1 - 1993

N2 - The combined rotation and multiple pulse sequence technique was used to obtain 1H NMR spectra of (silica)-O-Rh(allyl)2, a reactive organometallic complex bound in low concentration on the surface of the oxide, and a model compound, [(η3-allyl)2RhCl]2. By spectral comparison with the model compound, a bis(η3-allyl)Rh structure seemed possible for the surface-bound complex, but broad line widths precluded a more definite structural assignment. The 13C-labeled complex (η3-allyl)(η3-[13C]allyl)2Rh (in which either terminus of the allyl ligand was labeled) was prepared and deposited on silica. The resulting labeled surface complex was analyzed by both 13C cross-polarization magic angle spinning and the 2D 1H-13C heteronuclear correlation technique. Spectral data were compared with those obtained for [(η3-[13C] allyl)2-RhCl]2 and support the bis(η3-allyl)Rh complex structural assignment for (silica)-O-Rh(allyl)2.

AB - The combined rotation and multiple pulse sequence technique was used to obtain 1H NMR spectra of (silica)-O-Rh(allyl)2, a reactive organometallic complex bound in low concentration on the surface of the oxide, and a model compound, [(η3-allyl)2RhCl]2. By spectral comparison with the model compound, a bis(η3-allyl)Rh structure seemed possible for the surface-bound complex, but broad line widths precluded a more definite structural assignment. The 13C-labeled complex (η3-allyl)(η3-[13C]allyl)2Rh (in which either terminus of the allyl ligand was labeled) was prepared and deposited on silica. The resulting labeled surface complex was analyzed by both 13C cross-polarization magic angle spinning and the 2D 1H-13C heteronuclear correlation technique. Spectral data were compared with those obtained for [(η3-[13C] allyl)2-RhCl]2 and support the bis(η3-allyl)Rh complex structural assignment for (silica)-O-Rh(allyl)2.

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U2 - 10.1021/la00026a007

DO - 10.1021/la00026a007

M3 - Letter

AN - SCOPUS:0000224601

SN - 0743-7463

VL - 9

SP - 391

EP - 393

JO - Langmuir

JF - Langmuir

IS - 2

ER -

Structural Elucidation of (Silica)-O-Rh(allyl)₂ by Correlated ¹H and ¹³C NMR

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