Solvatomorphs of (Bu4N)2[{Ag(N2-py)}2Mo8O26]: structure, colouration and phase transition

Pavel A. Abramov, Vladislav Yu Komarov, Denis A. Pischur, Veronica S. Sulyaeva, Enrico Benassi, Maxim N. Sokolov

Research output: Contribution to journalArticlepeer-review

Abstract

Self-assembly of (Bu4N)4[β-Mo8O26], AgNO3and N2-py (N2-py = 2,6-diaminopyridine) in DMF solution results in a (Bu4N)2[β-{Ag(N2-py)}2Mo8O26] complex which crystallises as two phases: one (OP) is orange in colour and consists of [β-{Ag(N2-py)}2Mo8O26]2−monomers and [β-{Ag(N2-py)}2Mo8O26]n2n−polymeric chains in the crystal structure; the other (YP) is yellow in colour and built only with [β-{Ag(N2-py)}2Mo8O26]2−monomers. Both complexes were characterised by single crystal X-ray diffraction (SCXRD), X-ray powder diffraction (XRPD), diffuse reflectance (DR), infrared spectroscopy (IR), elemental analysis, and quantum chemical calculations. According to differential scanning calorimetry (DSC) and DR,OPdemonstrates a complicated phase transition at 130 K. Comprehensive SCXRD studies of the crystal structure change show rearrangement of the Ag+coordination sphere related with the dominant Ag-N bond distance change. TGA of both complexes confirms formation of silver nanoparticles (Ag-NPs), MoO3and Ag2Mo4O13upon thermal decomposition. The Ag-NPs were studied by SEM. Exfoliation of the resulting mixture in water gives a Ag-NP and MoO3mixed colloid system studied by TEM.

Original languageEnglish
Pages (from-to)8527-8537
Number of pages11
JournalCrystEngComm
Volume23
Issue number48
DOIs
Publication statusPublished - 28 Dec 2021

OECD FOS+WOS

  • 1.04 CHEMICAL SCIENCES
  • 1.04.FI CRYSTALLOGRAPHY

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