Uranyl tris-(carbohydrazide) nitrate [UO2((N2H3)2CO)3](NO3)2: synthesis, structure and properties
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Darya Y. Leshok
Abstract
Uranyl tris-(carbohydrazide) nitrate [UO2((N2H3)2CO)3](NO3)2 was prepared by the reaction of water solution of dioxouranium(VI) nitrate UO2(NO3)2(H2O)6 with ethanol solution of carbohydrazide (N2H3)2CO in a molar ratio of 1 to 3 in an neutral medium. The substance was characterized by elemental, thermal analysis and IR and 15N MAS CP NMR spectroscopy. Ab initio crystal structure determination was carried out using X-ray powder diffraction techniques. The compound crystallizes in monoclinic lattice with unit cell parameters: a = 15.193(1) Å, b = 12.005(1) Å, c = 10.842(1) Å, β = 109.15(1)○, V = 1868.11 Å3, Z = 4, SG = Cc. The type of carbohydrazide coordination was additionally confirmed by 15N MAS CP NMR and IR spectroscopy. In the complex ion [UO2((N2H3)2CO)3]2+ three carbohydrazide ligands coordinate to UO22+ through oxygen and nitrogen forming three five-membered chelate rings. The carbohydrazide rings are tuned to the equatorial plane of complex. The crystal structure consists of zig-zag chains of [UO2((N2H3)2CO)3]2+ cations stretched along c-axis. The cations in the chain are linked by the hydrogen bonds between the cations themselves. The anions are located in the pores between chains and participate in hydrogen bonding between adjacent chains and additionally link the chain sections. The length of the chain section is 5.768 Å and the angle between sections is 140○. The substance [UO2((N2H3)2CO)3](NO3)2 is thermally stable up to 215 ℃ and then decomposes with an explosion.
Supplementary material
the online version of this article (DOI: 10.1515/ract-2014-2337) provides supplementary material for authorized users.
Acknowledgement
The authors are grateful to reviewers for valuable comments which allowed us to significantly improve the results. The study was performed with the financial support of the Ministry of Science and Education PF, projects 1025, 3098, “Fund for Assistance to Small Innovative Enterprises in Science and Technology” (Grant program “UMNIK” 2013 II half GU1/2014), ICDD (Grant-in-Aid #10-93).
©2015 Walter de Gruyter Berlin/Boston
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Articles in the same Issue
- Frontmatter
- Removal of americium from effluent generated during the purification of plutonium by anion exchange
- Uranyl tris-(carbohydrazide) nitrate [UO2((N2H3)2CO)3](NO3)2: synthesis, structure and properties
- Nuclear forensic analysis of uranium oxide powders interdicted in Victoria, Australia
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