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Inorganic Chemistry
Volumn 48, Issue 6, 2009, Pages 2346-2348
Expanding the crystal chemistry of actinyl peroxides: μ- η 2:η 1 Peroxide coordination in trimers of U 6+ polyhedra
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EID: 64349112756     PISSN: 00201669     EISSN: None     Source Type: Journal    
DOI: 10.1021/ic8024217     Document Type: Article
Times cited : (15)
References (22)
  • 13
    • 84869263473 scopus 로고    scopus 로고
    • Crystals of 1 were synthesized by adding 0.1973 g of MgS04 to 4 mL of a 203 mM uranyl nitrate hexahydrate aqueous solution. A total of 0.5 mL of 30% H2O2 was added, and a yellow precipitate formed. A total of 1 mL of 3.0 M LiOH was added, and the solution was stirred vigorously. The precipitate dissolved, and a clear burnt-orange solution formed that was left uncovered for 24 h under ambient conditions, after which 1 mL was placed in a 5 mL Teflon vial with the addition of 6.5 μh of 3 M KOH. The vial was placed in a Teflon-lined autoclave with 30 mL of water for counterpressure and heated at 70 °C for 24 h. After cooling to room temperature, the solution was transferred to a 4 mL glass vial, capped, and stored at room temperature for 6 weeks, after which lath-shaped crystals approximately 300 μm in length were collected
    • 2 was added, and a yellow precipitate formed. A total of 1 mL of 3.0 M LiOH was added, and the solution was stirred vigorously. The precipitate dissolved, and a clear burnt-orange solution formed that was left uncovered for 24 h under ambient conditions, after which 1 mL was placed in a 5 mL Teflon vial with the addition of 6.5 μh of 3 M KOH. The vial was placed in a Teflon-lined autoclave with 30 mL of water for counterpressure and heated at 70 °C for 24 h. After cooling to room temperature, the solution was transferred to a 4 mL glass vial, capped, and stored at room temperature for 6 weeks, after which lath-shaped crystals approximately 300 μm in length were collected.
  • 14
    • 84869279838 scopus 로고    scopus 로고
    • Crystals were mounted on a Bruker PLATFORM three-circle X-ray diffractometer equipped with a 4K APEX CCD detector and graphite-monochromatized Mo Kα radiation with a crystal-to-detector distance of 4.67 cm. A sphere of data was collected using framewidths of 0.3° in ω at 110 K. Intensity data were corrected for Lorentz, polarization, and background effects using the Bruker program APEX II. A semiempirical correction for adsorption was applied using the program SADABS. The SHELXTL version 5 series of programs was used for the solution and refinement of the crystal structures. Crystal dimensions 80 × 50 × 30 μm, triclinic, PI, a, 6.5554(18) Å, b, 8.2865(18) Å, c, 18.146(5) Å, α, 95.064(5)°, ß, 93.359(4)°, γ, 94.770(3)°. V= 976.3(4) Å3, Rl, 3.50, wR2, 7.22, 17 278 total reflections, 6385 unique reflections, 5171 uni
    • 0 > 4σ.

* 이 정보는 Elsevier사의 SCOPUS DB에서 KISTI가 분석하여 추출한 것입니다.