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/sup 31/P and /sup 13/C solid-state NMR of tertiary phosphine-palladium complexes bound to silica

Journal Article · · Inorg. Chem.; (United States)
DOI:https://doi.org/10.1021/ic00242a019· OSTI ID:7252295
; ;
Phosphorus-31 and carbon-13 NMR spectra with cross polarization and magic-angle spinning are used to characterize palladium-tertiary phosphine complexes and their precursors covalently bound to silica. Phosphorus-31 NMR is a good probe of complex formation and geometry, whereas /sup 13/C NMR is a good probe of ligand structure. The 36.44-MHz /sup 31/P spectrum of (identical with SiOSiCH/sub 2/CH/sub 2/PPh/sub 2/)/sub 2/PdCl/sub 2/ shows two, barely resolved peaks at about 21 and 30 ppm assigned to the trans and cis complexes, respectively. These assignments are based on the chemical shifts of model compounds in both solution and the solid state. Uncomplexed phosphine and phosphine oxide are observed when complexes are prepared from phosphinated silica but not when the complexes are preformed and then attached to silica. The palladium dichloride complexes of bis(diphenylphosphino)methane, -ethane, and -propane, all of which have an approximately square-planar configuration, were examined as solid-state models for strained cis complexes on the silica surface. As in solution, the solid-state /sup 31/P chemical shifts of these compounds occur over a range of 127 ppm while the P-Pd-P angle varies from 73 to 91/sup 0/. Hence, the /sup 31/P chemical shift is a very sensitive measure of strain in such complexes and confirms that the structures in solution are similar to those in the solid state.
Research Organization:
BF Goodrich Research and Development Center, Brecksville, OH
OSTI ID:
7252295
Journal Information:
Inorg. Chem.; (United States), Journal Name: Inorg. Chem.; (United States) Vol. 25:22; ISSN INOCA
Country of Publication:
United States
Language:
English

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Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400201* -- Chemical & Physicochemical Properties
CARBON 13
CARBON ISOTOPES
CHALCOGENIDES
CHEMICAL SHIFT
COMPLEXES
COUPLING CONSTANTS
DATA
EVEN-ODD NUCLEI
EXPERIMENTAL DATA
INFORMATION
ISOTOPES
LIGANDS
LIGHT NUCLEI
MAGNETIC RESONANCE
MINERALS
NMR SPECTRA
NUCLEAR MAGNETIC RESONANCE
NUCLEI
NUMERICAL DATA
ODD-EVEN NUCLEI
OXIDE MINERALS
OXIDES
OXYGEN COMPOUNDS
PALLADIUM COMPLEXES
PHOSPHINES
PHOSPHORUS 31
PHOSPHORUS COMPOUNDS
PHOSPHORUS ISOTOPES
RESONANCE
SILICA
SILICON COMPOUNDS
SILICON OXIDES
SOLIDS
SPECTRA
STABLE ISOTOPES
STRUCTURAL CHEMICAL ANALYSIS
TRANSITION ELEMENT COMPLEXES