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April 17, 2021 at 6:20:33 AM

Irreversible transformations of 3d lead(ii) coordination polymers via mechanochemistry; precursors for the preparation of lead(ii) chloride/bromide/sulfide nanoparticles

Irreversible crystal-to-crystal transformations of 3D lead(II) coordination polymers with the ligand 1H-1,2,4-
triazole-3-carboxylic acid (HL), from [Pb(L)(µ2-Cl)(H2O)]n (1) to [Pb(L)(µ2-Br)(H2O)]n (2) and [Pb(L)(µ1,1-NCS)(H2O)]n (3)
by solid-state anion-replacement processes under mechanochemical reactions, have been studied. These irreversible solidstate structural transformations of compound 1 to compounds 2 and 3, have been verified by PXRD measurements. PbCl2,
PbBr2 and PbS nanoparticles were obtained by thermal decomposition of compounds 1, 2 and 3 in oleic acid as surfactant at
200 °C under air atmosphere, respectively.

Material Science Letters



Coordination polymers are a class of materials
composed of metals or metal clusters (the ‘‘node’’)
coordinated to multi-functional organic ligands (the
‘‘linker’’) [1].During the last two decades, design and
synthesis of novel metal–organic coordination
polymers are attracting more attention, not only for
their interesting molecular topologiesbut also for their
potential applications as functional materials, ions
exchange, catalysis, molecular recognition, nonlinear
optics, molecular magnetic materials, electrical
conductivity, separation and gas storage [2]. Solidstate crystal-to-crystal transformations involving
coordination polymers induced by light, heat, guest
removal, uptake or exchange, expansion of
coordination numbers, oxidation of metal centers,
condensation, or reactions between the ligands are
very fascinating and one of the hot topics in solidstate chemistry [3]. Solid state reactions by manual or
mechanical grinding solid reactants together with
either no added solvent or only nominal amounts for
molecular synthesis have triggered lots of
attention.Mechanochemical synthesis, a burgeoning
field in coordination polymers, has been utilized to
synthesize various coordination polymers from the
reactants without solvents [4].


In summary, a3D lead(II) coordination polymer
[Pb(L)(µ2- Cl)(H2O)]n (1) polymerize on grinding the
solid with KBr and KSCN to form the 3D
coordination polymers, [Pb(L)(µ2-Br)(H2O)]n (2) and
[Pb(L)(µ1,1-NCS)(H2O)]n(3), respectively. PbCl2,
PbBr2 and cubic-shaped PbS nanoparticles were
obtained by thermolysis of compounds 1, 2 and 3 in
oleic acid as surfactant at 200 °C under air
atmosphere, respectively.


[1]. M.-L. Hu, A. Morsali and L. Aboutorabi, Coord. Chem. Rev.
255, 2821(2011)
[2]. M. J. Zaworotko, New J. Chem.34,2355 (2010).
[3]. M. Nagarathinam, A. Chanthapally, S. H. Lapidus, P. W.
Stephens and J. J. Vittal, Chem. Commun. 48, 2585(2012).
[4]. S. L. James, C. J. Adams, C. Bolm, D. Braga, P. Collier, T.
Friscic, F. Grepioni, K. D. M. Harris, G. Hyett, W. Jones, A.
Krebs, J. Mack, L. Maini, A. G. Orpen, I. P. Parkin, W. C.
Shearouse, J. W. Steed and D. C. Waddell, Chem. Soc. Rev.
41, 413 (2012).

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