A carbonyl ligand of [Ru(bpy)2(CO)2]( 6>2 (1) (bpy = 2,2,-bipyridine) or [Ru(bpy)(trpy)(CO)](PF6)2 (2) (trpy = 2,2':6',2"-terpyridine) is reversibly converted to hydroxycarbonyl and r;1-C02 moieties by treatment with OH-. 1 and 2 also react with NaBH4 to afford CH3OH via formyl and hydroxymethyl complexes, and the molecular structures of 2 and [Ru(bpy)2(CO)(CH2OH)]PFé (3) were determined by X-ray structure analysis. Crystal data: 2, C26H1 9NsOP2Fi2Ru, monoclinic, space group C2/c, a = 34.683
The controlled potential electrolysis of [Ru(bpy)(napy) (CO) ](BF ) (1; bpy=2,2'-bipyridine, napy=1,8-naphthyridine) in the presence of LiBF in CO -saturated DMSO at -1.65 V (vs. Ag/Ag ) produced CO and Li CO [Eq. (a)], while similar electrolysis in the presence of (CH ) NBF resulted in formation of acetone together with (CH ) N and {(CH ) N} CO [Eq. (b)]. This represents the first almost selective generation of acetone upon electrochemical reduction of CO . The selectivity is ascribed to depression of reductive cleavage of the Ru-CO bond of 1 due to an attack of the nonbonded nitrogen atom of napy at the carbonyl carbon atom.
UVSOR is a Japanese low-energy synchrotron light source that has been operational since 1983. It has 750 MeV electron beam energy and a circumference of 53 m. The machine has undergone two major upgrades and is now called UVSOR-III, with a moderately small emittance of 17 nm·rad and is operated in the top-up mode at 300 mA. It has six undulators. Three in-vacuum undulators provide high-brightness VUV-SX light to the beamlines BL3U, BL4U, and BL6U. BL3U and BL4U are actively used for chemistry and life sciences using in situ and operando measurements, such as soft X-ray absorption and photoelectron spectroscopy. Since 2020, a unique photoelectron analyzer called the Momentum Microscope has been in operation in BL6U. Two variable polarization undulators provide high-brightness VUV light to the beamlines, BL5U and BL7U, which are used for solid-state physics through angle- and spin-resolved photoelectron spectroscopy. BL1U is equipped with two APPLE-II undulators in tandem and is used for various research purposes, including laser Compton scattering gamma rays. In addition to these beamlines, eight beamlines are operational which use bending magnet radiation, ranging from THz to tender X-rays. In 38 years of operation, we have dealt with and properly resolved machine problems, such as water leakage from magnet coils and cooling water flow paths in ultrahigh vacuum. Considering the machine’s declining competitiveness as a light source due to its aging and emerging demands in the low-energy area, we have started a design study on the future plan, as well as discussing it closely with the user community.
Electrochemical reduction of CO 2 aimed at carbon-carbon bond formation was examined. Polypyridyl-ruthenium-carbonyl complexes catalyze electrochemical reduction of CO 2 to produce CO and CO 3 2À in organic solvents. Among those metal complexes, a ruthenium carbonyl complex with monodentate naphthyridine showed a unique redox behavior. Oneelectron reduction of the complex resulted in intramolecular nucleophilic attack of the nonbonded nitrogen of naphthyridine to the carbonyl carbon to form a five-membered ring. Such metallacyclization greatly served for activation of the Ru-CO bond derived from CO 2 without accompanying reductive cleavage of the bond (CO evolution). Electrochemical reduction of CO 2 catalyzed by [Ru(bpy)(napy) 2 (CO) 2 ] 2 in the presence of (CH 3 ) 4 NBF 4 produced only CH 3 C(O)CH 3 and CO 3 2À , where (CH 3 ) 4 N worked as not only the electrolyte but also the methylation reagent.
Controlled potential electrolysis of [Ru(bpy)(trpy)(CO)]2+ (bpy = 2,2′-bipyridine; trpy = 2,2′:6′,2″-terpyridine) at −1.70 V vs. Ag|Ag+ in CO2-saturated C2H5OH/H2O (8:2v/v) at −20 °C produced not only HCOOH and CO but also HC(O)H, CH3OH, H(O)CCOOH, and HOCH2COOH.
Electrochemical reduction of CO 2 aimed at carbon-carbon bond formation was examined. Polypyridyl-ruthenium-carbonyl complexes catalyze electrochemical reduction of CO 2 to produce CO and CO 3 2À in organic solvents. Among those metal complexes, a ruthenium carbonyl complex with monodentate naphthyridine showed a unique redox behavior. Oneelectron reduction of the complex resulted in intramolecular nucleophilic attack of the nonbonded nitrogen of naphthyridine to the carbonyl carbon to form a five-membered ring. Such metallacyclization greatly served for activation of the Ru-CO bond derived from CO 2 without accompanying reductive cleavage of the bond (CO evolution). Electrochemical reduction of CO 2 catalyzed by [Ru(bpy)(napy) 2 (CO) 2 ] 2 in the presence of (CH 3 ) 4 NBF 4 produced only CH 3 C(O)CH 3 and CO 3 2À , where (CH 3 ) 4 N worked as not only the electrolyte but also the methylation reagent.
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