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Volumn 48, Issue 23, 2009, Pages 10907-10909

Crown and bowl-shaped clusters of uranyl polyhedra

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EID: 72949094951 PISSN: 00201669 EISSN: None Source Type: Journal
DOI: 10.1021/ic9020355 Document Type: Article

Times cited : (55)

References (22)

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- Synthesis of U16. Method 1, A total of 1.00 mL of 0.5 M uranyl nitrate hexahydrate in water, 1.00 mL of 30% H2O 2, 0.80 mL of 4 M NaOH in water, and 0.020 mL of 2 M CsOH in water were combined in a 20 mL scintillation vial. The solution evaporated slowly in air until crystals appeared in solution, and then the vial was capped. Method 2: A total of 1.00 mL of 0.5 M uranyl nitrate hexahydrate in water, l.00 mL of 30% H2O2, 0.80 mL of 4 M NaOH in water, and 0.10 mL of 2 M CsOH in water were combined in a 20 mL scintillation vial. The solution was left open to air until crystals formed, after which the vial was capped. Synthesis of U20R. A total of 1.00 mL of 30, H2O2 was combined with 1.25 mL of 5 M KOH in water in a 20 mL scintillation vial. A total of 1.00 mL of a 0.5 M uranyl nitrate hexahydrate solution in water was added dropwise, resulting in a solution with pH 13. The solution was left
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14
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- Crystals immersed in oil were placed on cryoloops and cooled in a stream of nitrogen gas to 120 K. A sphere of three-dimensional single-crystal X-ray diffraction data was collected for each using a Bruker Platform, gomiometer, an APEX CCD-based detector, and Mo Kα radiation. Data were integrated and corrected for background, Lorentz, and polarization effects using the APEX II. SADABS was used to apply corrections for absorption. Structure solutions and refinements were done using SHELXTL. Final refinement cycles on the basis of F2 included all atomic positional coordinates, anisotropic displacement parameters for U sites, and a mixture of anisotropic and isotropic displacement parameters for the remaining atoms. U16: P4/mnc, a, 20.547(1) Å,c, 40.710(3) Å, R1, 5.60, wR2, 16.50, S, 0.91. U20R: C2/c, a, 36.346(2) Å, b, 16.963(1) Å, c, 37.788(2) Å, β
- 1/c, a = 20.369(6) Å, b = 19.760(6) Å, c = 32.864(7) Å, β = 124.98(1)°, R1 = 7.04, wR2-18.35, S-0.73.

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