Acylselenoureato bis(chelates) of lead: synthesis, structural characterization and microwave-assisted formation of PbSe nano- and microstructures

We report the synthesis of three lead( ii ) bis(acylselenoureato) complexes ( 1a-3a ), which were prepared by the reaction of the respective acylselenourea compounds ArC(O)NHC(Se)NR 2 [Ar = 4-MeC 6 H 4 , R = Et ( 1 ); 4-ClC 6 H 4 , R = n Bu ( 2 ), i Bu ( 3 )] with Pb(OAc) 2 . All three compounds wer...

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Bibliographic Details
Published in:New journal of chemistry 2020-05, Vol.44 (19), p.7719-7726
Main Authors: Klauke, Karsten, Schmitz, Alexa, Swertz, Ann-Christin, Beele, Björn B, Giesen, Beatriz, Schlüsener, Carsten, Janiak, Christoph, Mohr, Fabian
Format: Article
Language:English
Subjects:
Chelates
Chemical analysis
Crystallography
Cubes
Dispersions
Electron diffraction
Electron microscopy
Ionic liquids
Lead selenides
Microscopy
Nanoparticles
NMR spectroscopy
Propylene
Reagents
Single crystals
Structural analysis
Synthesis
Thermal analysis
X ray powder diffraction
X-ray diffraction
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Summary:We report the synthesis of three lead( ii ) bis(acylselenoureato) complexes ( 1a-3a ), which were prepared by the reaction of the respective acylselenourea compounds ArC(O)NHC(Se)NR 2 [Ar = 4-MeC 6 H 4 , R = Et ( 1 ); 4-ClC 6 H 4 , R = n Bu ( 2 ), i Bu ( 3 )] with Pb(OAc) 2 . All three compounds were confirmed by NMR spectroscopy, elemental analysis and single crystal X-ray diffraction. Furthermore, the lead( ii ) complex 3a was transformed into PbSe nanostructures in a microwave-assisted synthesis using either a mixture of trioctylphosphine (TOP), octadecene (ODC) and the ionic liquid 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide, [BMIm][NTf 2 ], a mixture of [BMIm][NTf 2 ] and propylene carbonate (PC), pure [BMIm][NTf 2 ] or pure PC. The analyses of the resulting particle dispersions indicated formation of either small PbSe nanoparticles of 19 nm, PbSe submicro-cubes between 178 nm and 366 nm as well as strongly intergrown structures depending on the stabilizing reagent used during the synthesis. The prepared PbSe particle suspensions were characterized by powder X-ray diffraction (PXRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray spectrocopy (EDX) as well as by selected area electron diffraction (SAED). Three lead( ii ) bis(acylselenoureato) complexes were prepared by reaction of the respective acylselenourea compounds with Pb(OAc) 2 . One of these lead complexes was converted into PbSe nano- and microstructures by microwave-assisted synthesis.
ISSN:1144-0546
1369-9261
DOI:10.1039/d0nj01433h