Synthesis and spectral studies on N,N,N′,N′-tetramethylethylenediamine adducts of M(II) heterocyclic dithiocarbamates (M=zinc, cadmium): single crystal X-ray structure analysis of bis(1,2,3,4-tetrahydroquinolinecarbodithioato-S,S′)(N,N,N′,N′-tetramethylethylenediamine) cadmium(II)
摘要:
Zn(thqdtc)(2)(TMEDA) (1), Cd(thqdtc)(2)(TMEDA) (2), Zn(2-mpipdtc)(2)(TMEDA) (3), and Cd(2-mpipdtc)(2)(TMEDA) (4) (where thqdtc=1,2,3,4-tetrahydroquinolinedithiocarbamate, 2-mpipdtc=2-methylpiperidinedithiocarbamate, and TMEDA=N,N,N',N'-tetramethylethylenediamine) have been synthesized and characterized by infrared (IR) and nuclear magnetic resonance (H-1 and C-13) spectra. A single crystal X-ray structural analysis was carried out for complex 2. IR spectra of the complexes show the contribution of the thioureide form to the structures. The (NCS2)-C-13 chemical shifts of Zn(dtc)(2)(TMEDA) are additionally deshielded compared with Zn(dtc)(2) (dtc=thqdtc, 2-mpipdtc) owing to the increase in coordination number. Single crystal X-ray structure analysis of 2 showed that cadmium is in a distorted octahedral environment with a CdS4N2 chromophore. The acceptance of an additional neutral ligand by the tetrahedral dithiocarbamato complex of cadmium to form an octahedral adduct causes an increase in the Cd-S bond lengths.
Synthesis of multi-podal CdS nanostructures using heterocyclic dithiocarbamato complexes as precursors
摘要:
Bis(dipiperidinyldithiocarbamato)cadmium(II) (1) and bis(ditetrahydroquinolinyldithio-carbamato)cadmium(II) (2) were used as precursors for the synthesis of oleylamine (OA), decylamine (DA) and dodecylamine (DDA) capped CdS nanoparticles. The optical properties of these particles have been studied. The absorption spectra for the amine capped CdS particles are blue shifted in relation to the bulk material. The corresponding photoluminescence spectra show a narrow band edge emission. High quality crystalline CdS particles of different shapes, ranging from short nanorods and elongated nanorods (rods, bipods, tripods and tetrapods) to nanocubes were obtained when the reaction temperature was varied between 180 and 270 degrees C. A decrease in the length of the rods and bipodal nanoparticles was observed with an increase in the length of the chain of the amine (capping agent) used. The p-XRD patterns revealed the hexagonal phase of CdS to be dominant in all the samples. Infra-red studies suggest that the mode of bonding of the amines (oleylamine, decylamine and dodecylamine) on the CdS nanoparticle surfaces is through electron donation from the nitrogen atoms. (C) 2013 Elsevier Ltd. All rights reserved.
Aerosol assisted chemical vapor deposition (AACVD) of CdS thin films from heterocyclic cadmium(II) complexes
作者:Sixberth Mlowe、Linda D. Nyamen、Peter T. Ndifon、M. Azad Malik、James Raftery、Paul O’Brien、Neerish Revaprasadu
DOI:10.1016/j.ica.2015.05.024
日期:2015.8
Cadmium dithiocarbamato complexes of piperidine (1) and tetrahydroquinoline (2) were synthesized and characterized by elemental analysis, FT-IR spectroscopy, NMR and TGA analyses. The X-ray single crystal structure of bis(piperidinedithiocarbamato)cadmium(II) complex (1) was determined. The synthesized compounds were used as single source precursors to deposit CdS films on glass substrates at 350, 400 and 450 degrees C using the aerosol assisted chemical vapor deposition (AACVD) method. The surface morphology and the size of the CdS films were determined by AFM and SEM analyses; the crystalline phases by p-XRD analyses and the elemental composition by EDX measurements. The particle sizes were found to be in the range between 50-110 nm and 100-220 nm for complex (1) and (2), respectively. The electronic properties of the CdS films were analyzed by UV-Vis and Raman spectroscopic methods. Results revealed that the morphology, size and composition of the films are influenced by the deposition temperature. (C) 2015 Elsevier B.V. All rights reserved.