Isolation of ionic products in the reaction of carbon dioxide with

Isolation of ionic products in the reaction of carbon dioxide with (tetrahydroborato)copper(I) complexes: synthesis and reactions of [(biL)(Ph3P)2Cu][...
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Inorg. Chem. 1985, 24, 3920-3923

3920

Extraction of supported organometallics with various solvents was carried out as about 30 mg of solid were added to 3 mL of solvent. The suspensions were allowed to stand in a drybox, and liquid samples were withdrawn periodically for infrared analysis. All samples were filtered before being placed in the infrared cell (0.202-mm path length). Solid-state and solution ' H N M R spectra of supported rhenium species were obtained with a spectrometer operated at a frequency of 56.41 MHz for the proton resonance. An extract of the surface species was prepared by bringing 40 mg of solid in contact with 0.4 mL of methanol-d, (distilled from magnesium turnings under N2) for 0.5 h. A silica blank was also characterized. The magnet had an external deuterium lock to minimize field drift (