Chemistry of trivalent uranium. 2. Synthesis of UCl/sub 3/(18-crown-6) and U(BH/sub 4/)/sub 3/(18-crown-6)
The synthesis of UCl/sub 3/(18-crown-6) is reported. /sup 1/HNMR studies are underway for the purpose of establishing the coordination of the uranium in the complex. Although the substance is insoluble in tetrahydrofuran, a dispersed solution will react with sodium borohydride to yield a soluble product, U(BH/sub 4/)/sub 3/(18-crown-6). Analytical data suggest that the stoichiometry of the complex is probably correct. The /sup 1/HNMR spectrum supports the formulation as a 1 : 1 adduct with an integration of BH/sub 4//sup -/ to crown ether protons of 1 : 2. The 12 BH/sub 4//sup -/ protons are equivalent on the NMR time scale, and are shifted downfield due to the paramagnetic U(III) center. The complex has been recrystallized from THF/ethyl ether solutions. Preliminary x-ray diffraction results establish a stoichiometry of U(BH/sub 4/)/sub 3/(18-crown-6), and show that the uranium is actually located inside the crown ether cavity for 2 of the 3 different U atoms in the unit cell.
- Research Organization:
- Los Alamos Scientific Lab., NM
- OSTI ID:
- 6210038
- Journal Information:
- Inorg. Chem.; (United States), Vol. 18:1
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
BOROHYDRIDES
CHEMICAL REACTIONS
SODIUM COMPOUNDS
URANIUM COMPLEXES
CHEMICAL REACTION YIELD
STRUCTURAL CHEMICAL ANALYSIS
ADDUCTS
COORDINATION NUMBER
FURANS
NUCLEAR MAGNETIC RESONANCE
ORGANIC SOLVENTS
POLYETHYLENE GLYCOLS
STOICHIOMETRY
SYNTHESIS
X-RAY DIFFRACTION
ACTINIDE COMPLEXES
ALKALI METAL COMPOUNDS
BORON COMPOUNDS
COHERENT SCATTERING
COMPLEXES
DIFFRACTION
HETEROCYCLIC COMPOUNDS
HYDROGEN COMPOUNDS
MAGNETIC RESONANCE
ORGANIC COMPOUNDS
ORGANIC OXYGEN COMPOUNDS
ORGANIC POLYMERS
POLYMERS
RESONANCE
SCATTERING
SOLVENTS
YIELDS
400702* - Radiochemistry & Nuclear Chemistry- Properties of Radioactive Materials