Synthesis and structural elucidation of novel uranyl-crown ether compounds isolated from nitric, hydrochloric, sulfuric, and acetic acids

Journal Article · Wed Jun 12 00:00:00 EDT 1991 · Inorganic Chemistry; (United States)

DOI:https://doi.org/10.1021/ic00012a021· OSTI ID:5713447

Rogers, R D; Bond, A H; Hipple, W G; Rollins, A N; Henry, R F ^[1]

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1. Northern Illinois Univ., DeKalb (United States)

The reactions of UO{sub 2}SO{sub 4}{times}3H{sub 2}O with 12-crown-4, 15-crown-5, benzo-15-crown-5, 18-crown-6, and dibenzo-18-crown-6 were investigated in nitric, acetic, hydrochloric, and sulfuric acids. Impurities in the nitric acid resulted in the isolation of the complexes ((H{sub 5}O{sub 2})((NO{sub 2}){sub 2} benzo-15-crown-5){sub 2}){sub 2}((UO{sub 2}(NO{sub 3}){sub 2}){sub 2}C{sub 2}O{sub 4}) (benzo-15-crown-5 was nitrated during the reaction) and ((H{sub 3}O)(18-crown-6)){sub 2}(UO{sub 2}(NO{sub 3}{sub 2}){sub 2}C{sub 2}O{sub 4}), which were crystallographically characterized. (Mg(OH{sub 2}){sub 6})((H{sub 3}O)(15-crown-5)){sub 2}((UO{sub 2}(SO{sub 4})){sub 2}C{sub 2}O{sub 4}){sub 2} was also isolated from nitric acid and partially characterized crystallographically. Reactions in acetic acid produced uranyl sulfate polymers with layers of hydrogen-bonded crown ethers in the lattice. Hydronium ion complexes of crown ethers stabilized by (UO{sub 2}Cl{sub 4}){sup 2{minus}} anions were isolated from hydrochloric acid. The complexes ((H{sub 5}O{sub 2})(H{sub 9}O{sub 4}) (benz/o-15-crown-5){sub 2})(UO{sub 2}Cl{sub 4}) and ((H{sub 5}O{sub 2}){sub 2}(18-crown-6))(UO{sub 2}Cl{sub 4}) were isolated and crystallographically characterized. Reactions in sulfuric acid for the most part produced decomposition products. ((H{sub 3}O)(dibenzo-18-crown-6))(HSO{sub 4}){times}CH{sub 3}CN was isolated by recrystallization of a purple precipitate from CH{sub 3}CN/CH{sub 3}OH (3:1). The crystal structures of the complexes are reported. 57 refs., 12 figs., 1 tab.

• OSTI ID: 5713447
• Journal Information: Inorganic Chemistry; (United States), Journal Name: Inorganic Chemistry; (United States) Vol. 30:12; ISSN 0020-1669; ISSN INOCA
• Country of Publication: United States
• Language: English

Related Subjects

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEAR CHEMISTRY
400702* -- Radiochemistry & Nuclear Chemistry-- Properties of Radioactive Materials
ACETIC ACID
ACTINIDE COMPLEXES
ALCOHOLS
CARBOXYLIC ACIDS
CHEMICAL PREPARATION
CHEMICAL REACTIONS
CHLORINE COMPOUNDS
COMPLEXES
CRYSTAL STRUCTURE
DATA
DECOMPOSITION
EXPERIMENTAL DATA
GLYCOLS
HALOGEN COMPOUNDS
HYDROCHLORIC ACID
HYDROGEN COMPOUNDS
HYDROXY COMPOUNDS
INFORMATION
INORGANIC ACIDS
MONOCARBOXYLIC ACIDS
NITRIC ACID
NUMERICAL DATA
ORGANIC ACIDS
ORGANIC COMPOUNDS
ORGANIC POLYMERS
POLYETHYLENE GLYCOLS
POLYMERS
SULFURIC ACID
SYNTHESIS
URANIUM COMPLEXES
URANYL COMPLEXES