Issue 48, 2021

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

Abstract

Self-assembly of (Bu4N)4[β-Mo8O26], AgNO3 and 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, OP demonstrates 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), MoO3 and Ag2Mo4O13 upon thermal decomposition. The Ag-NPs were studied by SEM. Exfoliation of the resulting mixture in water gives a Ag-NP and MoO3 mixed colloid system studied by TEM.

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

Supplementary files

Article information

Article type
Paper
Submitted
26 Aug. 2021
Accepted
02 Nov. 2021
First published
09 Nov. 2021

CrystEngComm, 2021,23, 8527-8537

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

P. A. Abramov, V. Yu. Komarov, D. A. Pischur, V. S. Sulyaeva, E. Benassi and M. N. Sokolov, CrystEngComm, 2021, 23, 8527 DOI: 10.1039/D1CE01152A

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