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Inorganic Chemistry

Volumn 47, Issue 1, 2008, Pages 26-28

Structural characterization of Pu[N(SiMe3)2] 3, a synthetically useful nonaqueous plutonium(III) precursor

(5) Gaunt, Andrew J a Enriquez, Alejandro E a Reilly, Sean D a Scott, Brian L a Neu, Mary P a

a LOS ALAMOS NATIONAL LABORATORY (United States)

Author keywords

[No Author keywords available]

Indexed keywords

LIGAND; ORGANOMETALLIC COMPOUND; ORGANOSILICON DERIVATIVE; PLUTONIUM;

ARTICLE; CHEMICAL STRUCTURE; CHEMISTRY; SYNTHESIS; X RAY CRYSTALLOGRAPHY;

CRYSTALLOGRAPHY, X-RAY; LIGANDS; MODELS, MOLECULAR; ORGANOMETALLIC COMPOUNDS; ORGANOSILICON COMPOUNDS; PLUTONIUM;

EID: 38749130898 PISSN: 00201669 EISSN: None Source Type: Journal
DOI: 10.1021/ic701673e Document Type: Article

Times cited : (40)

References (22)

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- Plutonium of weapons-grade isotopic composition was used in this research. The work was conducted in a radiological facility approved to contain high specific activity, α-particle-emitting radionuclides, with appropriate analyses of hazards and implementation of controls for the safe handling and manipulation of radioactive materials
- Safety note! Plutonium of weapons-grade isotopic composition was used in this research. The work was conducted in a radiological facility approved to contain high specific activity, α-particle-emitting radionuclides, with appropriate analyses of hazards and implementation of controls for the safe handling and manipulation of radioactive materials.
- Safety note

12
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- Synthesis of Pu[N(SiMe3)2]3 (1, Inside a negative-pressure helium-atmosphere drybox, α-phase plutonium metal (0.0257 g, 0.107 mmol) was suspended in Et2O (5 cm3) and iodine (0.0382 g, 0.151 mmol) added. The mixture was stirred at room temperature for 2 days, resulting in a very pale-blue powder, a small piece of unreacted plutonium metal (<2 mg, and a colorless solution, which indicated quantitative iodine consumption. Na[N(SiMe3)2, 0.0552 g, 0.301 mmol) in Et2O (2 cm3) was added and stirred for 45 min to give an orange solution with a white precipitate of NaI. The solution was filtered, the solvent removed in vacuo from the filtrate, and the residue dissolved in hexanes (5 cm3, The resultant orange solution was filtered and the solvent removed in vacuo to give an orange powder 0.0628 g, 87% yield based on iodine, Identification of the orange powder as 1 was m
- 9 Single-crystals suitable for X-ray diffraction were grown from a concentrated n-pentane solution of 1 stored at -30°C for several days.

13
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- Crystallographic data collection details: The crystal was coated with Paratone N and mounted inside a 0.5 mm capillary, which was sealed with wax and whose external surface was coated with a thin film of acrylic dissolved in ethyl acetate (Hard as Nails nail polish) to provide appropriate containment of the radioactive material. The data were collected on a Bruker SMART APEX II CCD X-ray diffractometer with a KRYOFLEX liquid-nitrogen vapor cooling device at 141(2) K. The instrument was equipped with a Mo Kα X-ray source γ, 0.710 73 Å, with MonoCap X-ray source optics. A hemisphere of data was collected using ω scans, with 5 s frame exposures at 0.3° frame widths. Data collection and initial indexing and cell refinement were handled with APEX II software.18 Frame integration, including Lorentz-polarization corrections and final cell parameter calculations, was carried out using SAINT+ software.19 The data were corrected for abs
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18
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- in press
- Gaunt, A. J.; Reilly, S. D.; Enriquez, A. E.; Scott, B. L.; Ibers, J. A.; Sekar, P.; Ingram, K. I. M.; Kaltsoyannis, N.; Neu, M. P. Inorg. Chem. 2007, in press.
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- Gaunt, A.J.¹ Reilly, S.D.² Enriquez, A.E.³ Scott, B.L.⁴ Ibers, J.A.⁵ Sekar, P.⁶ Ingram, K.I.M.⁷ Kaltsoyannis, N.⁸ Neu, M.P.⁹

19
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- APEX II, version 1.08; Bruker AXS, Inc, Madison, WI, 2004
- APEX II, version 1.08; Bruker AXS, Inc.: Madison, WI, 2004.

20
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21
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22
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* 이 정보는 Elsevier사의 SCOPUS DB에서 KISTI가 분석하여 추출한 것입니다.