TY - JOUR

T1 - Double complex salts based on [Rh(NH 3 ) 6 ] 3+ as precursors of alloy systems Rh–Nb and Rh–V: synthesis, structure, and thermal properties

AU - Bautina, Sof'ya

AU - Vorobyeva, Sofia Navilevna

AU - Rudzis, Zakhar V.

AU - Rudneva, Yuliya

AU - Nadolinnyi, Vladimir A.

AU - Plyusnin, Pavel E

AU - Sukhikh, Taisiya Sergeevna

AU - Zhurenok, Angelina V

AU - Kozlova, Ekaterina

AU - Korenev, Sergey

N1 - Double complex salts based on [Rh(NH 3 ) 6 ] 3+ as precursors of alloy systems Rh–Nb and Rh–V: synthesis, structure, and thermal properties / S. Bautina, S. Vorobyeva, Z. Rudzis, Y. Rudneva, V. Nadolinny, P. Plusnin, T. Sukhikh, A. Zhurenok, E. Kozlova, S. Korenev // New Journal of Chemistry. - 2025. DOI 10.1039/d5nj03210e

PY - 2025

Y1 - 2025

N2 - The complex [Rh(NH 3 ) 6 ](NO 3 ) 3 (I) has been synthesized, and its crystal structure has been determined for the first time. The syntheses of double complex salts (DCS) [Rh(NH 3 ) 6 ][NbO(C 2 O 4 ) 3 ]∙4H 2 O (II) and [Rh(NH 3 ) 6 ] 2 [(μ 2 -C 2 O 4 )(VO(C 2 O 4 ) 2 ) 2 ]∙6H 2 O (III)... The complex [Rh(NH 3 ) 6 ](NO 3 ) 3 (I) has been synthesized, and its crystal structure has been determined for the first time. The syntheses of double complex salts (DCS) [Rh(NH 3 ) 6 ][NbO(C 2 O 4 ) 3 ]∙4H 2 O (II) and [Rh(NH 3 ) 6 ] 2 [(μ 2 -C 2 O 4 )(VO(C 2 O 4 ) 2 ) 2 ]∙6H 2 O (III) were carried out. The complexes were characterized by single-crystal and powder X-ray diffraction, IR, UV-VIS (III), diffuse reflectance spectroscopy (III), and EPR (III). The processes of thermal decomposition of DCS II and III in inert and reducing atmospheres were studied. Thermal decomposition of [Rh(NH 3 ) 6 ][NbO(C 2 O 4 ) 3 ]∙4H 2 O (II) in a hydrogen atmosphere results in the formation of bimetallic solid solution Rh 0.83 Nb 0.17 and NbO 2 , while in the case of [Rh(NH 3 ) 6 ] 2 [(μ 2 -C 2 O 4 )(VO(C 2 O 4 ) 2 ) 2 ]∙6H 2 O (III) - a phase with the structure of intermetallic Rh 3 V and V 2 O 3 . The photocatalytic activity of thermolysis products in Rh-Nb and Rh-V systems was tested in the process of hydrogen production. Rh-Nb/g-C 3 N 4 catalyst shows a rate of H 2 evolution about 0.69 mmol∙h -1 ∙gcat -1 , Rh-Nb/TiO 2 catalysts – about 0.29 mmol∙h -1 ∙gcat -1 under 410 nm.

AB - The complex [Rh(NH 3 ) 6 ](NO 3 ) 3 (I) has been synthesized, and its crystal structure has been determined for the first time. The syntheses of double complex salts (DCS) [Rh(NH 3 ) 6 ][NbO(C 2 O 4 ) 3 ]∙4H 2 O (II) and [Rh(NH 3 ) 6 ] 2 [(μ 2 -C 2 O 4 )(VO(C 2 O 4 ) 2 ) 2 ]∙6H 2 O (III)... The complex [Rh(NH 3 ) 6 ](NO 3 ) 3 (I) has been synthesized, and its crystal structure has been determined for the first time. The syntheses of double complex salts (DCS) [Rh(NH 3 ) 6 ][NbO(C 2 O 4 ) 3 ]∙4H 2 O (II) and [Rh(NH 3 ) 6 ] 2 [(μ 2 -C 2 O 4 )(VO(C 2 O 4 ) 2 ) 2 ]∙6H 2 O (III) were carried out. The complexes were characterized by single-crystal and powder X-ray diffraction, IR, UV-VIS (III), diffuse reflectance spectroscopy (III), and EPR (III). The processes of thermal decomposition of DCS II and III in inert and reducing atmospheres were studied. Thermal decomposition of [Rh(NH 3 ) 6 ][NbO(C 2 O 4 ) 3 ]∙4H 2 O (II) in a hydrogen atmosphere results in the formation of bimetallic solid solution Rh 0.83 Nb 0.17 and NbO 2 , while in the case of [Rh(NH 3 ) 6 ] 2 [(μ 2 -C 2 O 4 )(VO(C 2 O 4 ) 2 ) 2 ]∙6H 2 O (III) - a phase with the structure of intermetallic Rh 3 V and V 2 O 3 . The photocatalytic activity of thermolysis products in Rh-Nb and Rh-V systems was tested in the process of hydrogen production. Rh-Nb/g-C 3 N 4 catalyst shows a rate of H 2 evolution about 0.69 mmol∙h -1 ∙gcat -1 , Rh-Nb/TiO 2 catalysts – about 0.29 mmol∙h -1 ∙gcat -1 under 410 nm.

UR - https://www.mendeley.com/catalogue/799cccc9-6b45-346f-af38-bd964bf1c0e9/

U2 - 10.1039/d5nj03210e

DO - 10.1039/d5nj03210e

M3 - Article

JO - New Journal of Chemistry

JF - New Journal of Chemistry

SN - 1144-0546

ER -