NDLI: Hydrazinium lanthanide oxalates: synthesis, structure and thermal reactivity of $N_{2}H_{5}[Ln_{2}(C_{2}O_{4})_{4}(N_{2}H_{5})]·4H

Content Provider	World Health Organization (WHO)-Global Index Medicus
Author	Grandjean, Stéphane De Almeida, Lucie Patisson, Fabrice Abraham, Francis Rivenet, Murielle
Description	Author Affiliation: De Almeida L ( CEA, Nuclear Energy Division, Marcoule, RadioChemistry & Process Department, BP17171, 30207 Bagnols-sur-Cèze, France.)
Abstract	New hydrazinium lanthanide oxalates $N_{2}H_{5}[Ln_{2}(C_{2}O_{4})_{4}(N_{2}H_{5})]·4H_{2}O,$ Ln = Ce (Ce-HyOx) and Nd (Nd-HyOx), were synthesized by hydrothermal reaction at 150 °C between lanthanide nitrate, oxalic acid and hydrazine solutions. The structure of the Nd compound was determined from single-crystal X-ray diffraction data, space group $P2_{1}/c$ with a = 16.315(4), b = 12.127(3), c = 11.430(2) Å, β = 116.638(4)°, V = 2021.4(7) $Å^{3},$ Z = 4, and $R_{1}$ = 0.0313 for 4231 independent reflections. Two distinct neodymium polyhedra are formed, $NdO_{9}$ and $NdO_{8}N,$ an oxygen of one monodentate oxalate in the former being replaced by a nitrogen atom of a coordinated hydrazinium ion in the latter. The infrared absorption band at 1005 $cm^{−1}$ confirms the coordination of $N_{2}H_{5}^{+}$ to the metal. These polyhedra are connected through μ2 and μ3 oxalate ions to form an anionic three-dimensional neodymium-oxalate arrangement. A non-coordinated charge-compensating hydrazinium ion occupies, with water molecules, the resulting tunnels. The N–N stretching frequencies of the infrared spectra demonstrate the existence of the two types of hydrazine ions. Thermal reactivity of these hydrazinium oxalates and of the mixed isotypic Ce/Nd (CeNd-HyOx) oxalate were studied by using thermogravimetric and differential thermal analyses coupled with gas analyzers, and high temperature X-ray diffraction. Under air, fine particles of $CeO_{2}$ and $Ce_{0.5}Nd_{0.5}O_{1.75}$ are formed at low temperature from Ce-HyOx and CeNd-HyOx, respectively, thanks to a decomposition/oxidation process. Under argon flow, dioxymonocyanamides $Ln_{2}O_{2}CN_{2}$ are formed.
ISSN	14779226
Issue Number	12
Journal	Dalton Trans.
Volume Number	43
e-ISSN	13645447
Language	English
Publisher	Royal Society of Chemistry
Publisher Date	2014-03-28
Publisher Place	Great Britain (UK)
Access Restriction	Subscribed
Subject Keyword	Chemistry
Content Type	Text
Resource Type	Article
Subject	Inorganic Chemistry

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