Coordination compounds of rare-earth Nitrates with N,N-dimethylacetamide

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Аннотация

Coordination compounds of rare-earth nitrates with N,N-dimethylacetamide (DMAA), [Sc(H2O)(DMAA)2(NO3)(μ-OH)2Sc(NO3)(DMAA)2(H2O)](NO3)2, [La(DMAA)4(NO3)3], [Ce(DMAA)5(NO3)2][Ce(DMAA)2(NO3)4] and [Ln(DMAA)3(NO3)3] (Ln = Pr, Nd, Sm–Lu, Y), have been synthesized. Using physicochemical analysis methods (elemental analysis, IR spectroscopy, XRD, XRD, TGA-DSC), the compositions and structural features were determined; thermal decomposition of the compounds was studied in a wide temperature range (50–900°C). Complexes [Ln(DMAA)3(NO3)3] form two isostructural series: crystals with Ln = Pr–Dy belong to the monoclinic symmetry, and with Ln = Ho–Lu, Y – to the orthorhombic symmetry. It is shown that the coordination compounds can be used as precursors for the production of nanoscale REE oxides (from 12 to 50 nm) with a specific surface area of 18–65 m2/g.

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Авторлар туралы

M. Polukhin

MIREA—Russian Technological University

Email: savinkina@mirea.ru

Lomonosov Institute of Fine Chemical Technologies

Ресей, Moscow, 119571

I. Karavaev

MIREA—Russian Technological University

Email: savinkina@mirea.ru

Lomonosov Institute of Fine Chemical Technologies

Ресей, Moscow, 119571

E. Savinkina

MIREA—Russian Technological University

Хат алмасуға жауапты Автор.
Email: savinkina@mirea.ru

Lomonosov Institute of Fine Chemical Technologies

Ресей, Moscow, 119571

G. Buzanov

Kurnakov Institute of General and Inorganic Chemistry

Email: savinkina@mirea.ru
Ресей, Moscow, 119991

A. Kubasov

Kurnakov Institute of General and Inorganic Chemistry

Email: savinkina@mirea.ru
Ресей, Moscow, 119991

M. Grigoriev

Frumkin Institute of Physical Chemistry and Electrochemistry

Email: savinkina@mirea.ru
Ресей, Moscow, 119071

E. Turyshev

Kurnakov Institute of General and Inorganic Chemistry

Email: savinkina@mirea.ru
Ресей, Moscow, 119991

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2. Fig. 1. Structural series of synthesized complexes.

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3. Fig. 2. Experimental (a) and theoretical (b) diffraction patterns of the samples [Sc(H2O(DMAA)2(NO3)(μ-OH)2Sc(NO3)(DMAA)2(H2O)](NO3)2 (1), [La(DMAA)4(NO3)3] (2), [Ce(DMAA)5(NO3)2][Ce(DMAA)2(NO3)4] (3), [Eu(DMAA)3(NO3)3](monocle) (4) and [Er(DMAA)3(NO3)3](diamond) (5).

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4. Fig. 3. ORTEP view of coordination compounds I (a), II (b), III (c), VII (d), XII (d), hydrogen atoms are not shown.

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5. Fig. 4. Thermograms of the complexes [Pr(DMAA)3(NO3)3] (a) and [Eu(DMAA)3(NO3)3] (b); 1 – mass loss curve, 2 – differential curve.

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6. Fig. 5. Powder diffraction patterns of Pr6O11 (1), Eu2O3 (2), Ho2O3 (3), Er2O3 (4) and Y2O3 (5).

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7. Fig. 6. Micrographs of oxides Nd2O3 (a), Eu2O3 (b), Tb4O7 (c), Er2O3 (d).

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8. Fig. 7. Isotherms of N2 adsorption and desorption on the surface of La2O3 (a) and CeO2 (b).

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9. Fig. S1. IR spectra of the complexes: (a) – [Ln(DMAA)3(NO3)3] (monocle): Ln = Gd (1), Eu (2), Dy (3), Tb (4), Sm (5), Nd (6), Pr (7); (b) – [Ln’(DMAA)3(NO3)3] (diamond): Ln’ = Lu (1), Er (2), Ho (3), Yb (4), Y (5), Tm (6); (c): [Ce(DMAA)5(NO3)2][Ce(DMAA)2(NO3)4] (1), [Sc(H2O)(DMAA)2(NO3)(μ-OH)2(NO3)(DMAA)2(H2O)Sc](NO3)2 (2), [La(DMAA)3.7(NO3)3] (3)

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10. Fig. S2. Thermograms of the complexes: (a) – [La(DMAA)4(NO3)3], (b) – [Ce(DMAA)5(NO3)2][Ce(DMAA)2(NO3)4], (c) – [Nd(DMAA)3(NO3)3], (d) – [Y(DMAA)3(NO3)3], (e) – [Ho(DMAA)3(NO3)3], (f) – [Er(DMAA)3(NO3)3], (g) – [Tb(DMAA)3(NO3)3]: a – mass loss curve, b – differential curve

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11. Figure S3. IR spectrum of products of VII thermolysis at 315°C

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12. Supplementary materials
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13. Supplementary materials
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