SYNTHESIS, CHARACTERIZATION AND CRYSTAL STRUCTURE OF A NOVEL DECAVANADATE SALT, [V0.50(H2O)5]2[H2(V10O28)]·4(H2O)

SYNTHESIS, CHARACTERIZATION AND CRYSTAL STRUCTURE OF A NOVEL DECAVANADATE SALT, [V0.50(H2O)5]2[H2(V10O28)]·4(H2O)

ABSTRACT A novel decavanadate salt, [V0.50(H2O)5]2[H2(V10O28)]·4(H2O), was obtained by the reaction of NH4VO3 with chinhydrone in an acidic medium. The title compound was characterized in the solid and solution phases by FT-IR, single crystal X-ray diffraction, voltammetry, UV-Vis., EPR and NMR meas...

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Autores principales: BICER,ENDER, DEGE,NECMI, COSKUN,EMINE
Lenguaje:English
Publicado: Sociedad Chilena de Química 2017
Materias:
Decavanadate
V(V) and V(IV) units
chinhydrone
single crystal
water-bridged dimer
Acceso en línea:http://www.scielo.cl/scielo.php?script=sci_arttext&pid=S0717-97072017000303610
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spelling oai:scielo:S0717-970720170003036102017-09-08SYNTHESIS, CHARACTERIZATION AND CRYSTAL STRUCTURE OF A NOVEL DECAVANADATE SALT, [V0.50(H2O)5]2[H2(V10O28)]·4(H2O)BICER,ENDERDEGE,NECMICOSKUN,EMINE Decavanadate V(V) and V(IV) units chinhydrone single crystal water-bridged dimer ABSTRACT A novel decavanadate salt, [V0.50(H2O)5]2[H2(V10O28)]·4(H2O), was obtained by the reaction of NH4VO3 with chinhydrone in an acidic medium. The title compound was characterized in the solid and solution phases by FT-IR, single crystal X-ray diffraction, voltammetry, UV-Vis., EPR and NMR measurements. The crystal data of the compound are: H30O42V11, triclinic, Pī, a = 8.4906 (4) Å, b = 10.4236 (5) Å, c = 11.2861 (6) Å, α = 68.490 (4)°, β = 87.251 (4)°, γ = 67.145 (4)°, V = 851.11 (8) Å3, and Z = 1. In the structure, [H2(V10O28)]4− anion is bound via hydrogen bonds to the dimer state of [V0.50(H2O)5]2+ cations and the water molecules. At this dimer moiety, it has been thought that the oxygen atoms of two water molecules form the bridges between two V(IV) center ions. The presence of high spin V(IV) (I = 7/2) in the compound was verified by EPR measurements. In addition, decavanadate unit gave a shoulder at about 400 nm on the UV-Vis. spectrum of the compound. Moreover, at the FT-IR spectrum, the symmetric and asymmetric stretching vibrations of the bridging V–O–V units were observed. On the cyclic voltammogram of the compound, two reduction peaks (V(V)-V(IV) and V(IV)-V(II) reduction steps, respectively) at −1.03 and −1.35 V were observed at the cathodic scan; however, one oxidation peak (V(II)-V(III) oxidation step) at −1.22 V showed at the anodic scan. NMR results also support that the synthesized salt includes the coordinated water molecules and hydroxo groups.info:eu-repo/semantics/openAccessSociedad Chilena de QuímicaJournal of the Chilean Chemical Society v.62 n.3 20172017-09-01text/htmlhttp://www.scielo.cl/scielo.php?script=sci_arttext&pid=S0717-97072017000303610en10.4067/s0717-97072017000303610
institution Scielo Chile
collection Scielo Chile
language English
topic Decavanadate
V(V) and V(IV) units
chinhydrone
single crystal
water-bridged dimer
spellingShingle Decavanadate
V(V) and V(IV) units
chinhydrone
single crystal
water-bridged dimer
BICER,ENDER
DEGE,NECMI
COSKUN,EMINE
SYNTHESIS, CHARACTERIZATION AND CRYSTAL STRUCTURE OF A NOVEL DECAVANADATE SALT, [V0.50(H2O)5]2[H2(V10O28)]·4(H2O)
description ABSTRACT A novel decavanadate salt, [V0.50(H2O)5]2[H2(V10O28)]·4(H2O), was obtained by the reaction of NH4VO3 with chinhydrone in an acidic medium. The title compound was characterized in the solid and solution phases by FT-IR, single crystal X-ray diffraction, voltammetry, UV-Vis., EPR and NMR measurements. The crystal data of the compound are: H30O42V11, triclinic, Pī, a = 8.4906 (4) Å, b = 10.4236 (5) Å, c = 11.2861 (6) Å, α = 68.490 (4)°, β = 87.251 (4)°, γ = 67.145 (4)°, V = 851.11 (8) Å3, and Z = 1. In the structure, [H2(V10O28)]4− anion is bound via hydrogen bonds to the dimer state of [V0.50(H2O)5]2+ cations and the water molecules. At this dimer moiety, it has been thought that the oxygen atoms of two water molecules form the bridges between two V(IV) center ions. The presence of high spin V(IV) (I = 7/2) in the compound was verified by EPR measurements. In addition, decavanadate unit gave a shoulder at about 400 nm on the UV-Vis. spectrum of the compound. Moreover, at the FT-IR spectrum, the symmetric and asymmetric stretching vibrations of the bridging V–O–V units were observed. On the cyclic voltammogram of the compound, two reduction peaks (V(V)-V(IV) and V(IV)-V(II) reduction steps, respectively) at −1.03 and −1.35 V were observed at the cathodic scan; however, one oxidation peak (V(II)-V(III) oxidation step) at −1.22 V showed at the anodic scan. NMR results also support that the synthesized salt includes the coordinated water molecules and hydroxo groups.
author BICER,ENDER
DEGE,NECMI
COSKUN,EMINE
author_facet BICER,ENDER
DEGE,NECMI
COSKUN,EMINE
author_sort BICER,ENDER
title SYNTHESIS, CHARACTERIZATION AND CRYSTAL STRUCTURE OF A NOVEL DECAVANADATE SALT, [V0.50(H2O)5]2[H2(V10O28)]·4(H2O)
title_short SYNTHESIS, CHARACTERIZATION AND CRYSTAL STRUCTURE OF A NOVEL DECAVANADATE SALT, [V0.50(H2O)5]2[H2(V10O28)]·4(H2O)
title_full SYNTHESIS, CHARACTERIZATION AND CRYSTAL STRUCTURE OF A NOVEL DECAVANADATE SALT, [V0.50(H2O)5]2[H2(V10O28)]·4(H2O)
title_fullStr SYNTHESIS, CHARACTERIZATION AND CRYSTAL STRUCTURE OF A NOVEL DECAVANADATE SALT, [V0.50(H2O)5]2[H2(V10O28)]·4(H2O)
title_full_unstemmed SYNTHESIS, CHARACTERIZATION AND CRYSTAL STRUCTURE OF A NOVEL DECAVANADATE SALT, [V0.50(H2O)5]2[H2(V10O28)]·4(H2O)
title_sort synthesis, characterization and crystal structure of a novel decavanadate salt, [v0.50(h2o)5]2[h2(v10o28)]·4(h2o)
publisher Sociedad Chilena de Química
publishDate 2017
url http://www.scielo.cl/scielo.php?script=sci_arttext&pid=S0717-97072017000303610
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AT degenecmi synthesischaracterizationandcrystalstructureofanoveldecavanadatesaltv050h2o52h2v10o284h2o
AT coskunemine synthesischaracterizationandcrystalstructureofanoveldecavanadatesaltv050h2o52h2v10o284h2o
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