Synthesis and crystal structure of bis(thiomorpholinyldithiocarbamato)Cu(II) complex and its use as precursor for CuS nanoparticles photocatalyst for the degradation of organic dyes
TL;DR: Bis(thiomorpholinyldithicarbamate)Cu(II) complex was prepared and characterized by single crystal X-ray crystallography as mentioned in this paper, which revealed a mononuclear copper ion bonded to two...
About: This article is published in Journal of Sulfur Chemistry.The article was published on 2021-03-04. It has received 10 citations till now. The article focuses on the topics: Crystal structure & Single crystal.
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TL;DR: In this paper, the effect of thermolysis time on the morphological and optical properties of CuS nanoparticles prepared from Cu(II) dithiocarbamate single-source precursor was reported.
Abstract: We report the effect of thermolysis time on the morphological and optical properties of CuS nanoparticles prepared from Cu(II) dithiocarbamate single-source precursor. The as-prepared copper sulfide nanoparticles were used as photocatalysts for the degradation of crystal violet (CV), methylene blue (MB), rhodamine B (RhB), and a ternary mixture of the three dyes (CV/MB/RhB). Powder XRD patterns confirmed the hexagonal covellite phase for the CuS nanoparticles. At the same time, HRTEM images revealed mixed shapes with a particle size of 31.47 nm for CuS1 prepared at 30 min while CuS2 prepared at 1 h consists of mixtures of hexagonal and nanorods shaped particles with an average size of 21.59 nm. Mixed hexagonal and spherically shaped particles with a size of 17.77 nm were obtained for CuS3 prepared at 2 h. The optical bandgaps of the nanoparticles are 3.00 eV for CuS1, 3.26 eV for CuS2 and 3.13 eV for CuS3. The photocatalytic degradation efficiency showed that CuS3 with the smallest particle size is the most efficient photocatalyst and degraded 85% of CV, 100% of MB, and 81% of RhB. The as-prepared CuS showed good stability and recyclability and also degraded ternary dyes mixture (CV/MB/RhB) effectively. The byproducts of the dye degradation were evaluated using ESI-mass spectrometry.
23 citations
10 Sep 2021
TL;DR: Copper dithiocarbamates have been known for ca. 120 years and find relevance in biology and medicine, especially as anticancer agents and applications in materials science as a single-source precursor (SSPs) to nanoscale copper sulfides as mentioned in this paper.
Abstract: Copper dithiocarbamate complexes have been known for ca. 120 years and find relevance in biology and medicine, especially as anticancer agents and applications in materials science as a single-source precursor (SSPs) to nanoscale copper sulfides. Dithiocarbamates support Cu(I), Cu(II) and Cu(III) and show a rich and diverse coordination chemistry. Homoleptic [Cu(S2CNR2)2] are most common, being known for hundreds of substituents. All contain a Cu(II) centre, being either monomeric (distorted square planar) or dimeric (distorted trigonal bipyramidal) in the solid state, the latter being held together by intermolecular C···S interactions. Their d9 electronic configuration renders them paramagnetic and thus readily detected by electron paramagnetic resonance (EPR) spectroscopy. Reaction with a range of oxidants affords d8 Cu(III) complexes, [Cu(S2CNR2)2][X], in which copper remains in a square-planar geometry, but Cu–S bonds shorten by ca. 0.1 A. These show a wide range of different structural motifs in the solid-state, varying with changes in anion and dithiocarbamate substituents. Cu(I) complexes, [Cu(S2CNR2)2]−, are (briefly) accessible in an electrochemical cell, and the only stable example is recently reported [Cu(S2CNH2)2][NH4]·H2O. Others readily lose a dithiocarbamate and the d10 centres can either be trapped with other coordinating ligands, especially phosphines, or form clusters with tetrahedral [Cu(μ3-S2CNR2)]4 being most common. Over the past decade, a wide range of Cu(I) dithiocarbamate clusters have been prepared and structurally characterised with nuclearities of 3–28, especially exciting being those with interstitial hydride and/or acetylide co-ligands. A range of mixed-valence Cu(I)–Cu(II) and Cu(II)–Cu(III) complexes are known, many of which show novel physical properties, and one Cu(I)–Cu(II)–Cu(III) species has been reported. Copper dithiocarbamates have been widely used as SSPs to nanoscale copper sulfides, allowing control over the phase, particle size and morphology of nanomaterials, and thus giving access to materials with tuneable physical properties. The identification of copper in a range of neurological diseases and the use of disulfiram as a drug for over 50 years makes understanding of the biological formation and action of [Cu(S2CNEt2)2] especially important. Furthermore, the finding that it and related Cu(II) dithiocarbamates are active anticancer agents has pushed them to the fore in studies of metal-based biomedicines.
19 citations
TL;DR: In this article , the photocatalytic degradation of the as-prepared CuS-GNs has been investigated based on Fenton-like and photocatalysis reactions.
12 citations
TL;DR: In this article, the synthesis and morphological studies of lead sulphide nanoparticles prepared from lead(II) complexes of morpholine dithiocarbamate (PbS1), thiomorpholine ditiocaramate (pbS2), and N-(2-hydroxyethyl)phenyl dithIocarbamates (PBS3) are reported.
Abstract: We report the synthesis and morphological studies of lead sulphide nanoparticles prepared from lead(II) complexes of morpholine dithiocarbamate (PbS1), thiomorpholine dithiocarbamate (PbS2), and N-(2-hydroxyethyl)phenyl dithiocarbamate (PbS3). Powder X-ray diffraction patterns (p-XRD) of the PbS nanoparticles are indexed to face-centered cubic phase of PbS. High-resolution transmission electron microscopy (HRTEM) micrograph revealed quasi-spherical PbS nanoparticles with particle size in the range 13.86–36.06 nm while scanning electron microscopy (SEM) revealed flaky/spherical/rough surface morphology. Photocatalytic degradation of methylene blue dye by the PbS nanoparticles showed degradation efficiency of 72.6 % for PbS1, 75.9 % for PbS2, and 47.4 % for PbS3. The photodegradation efficiency shows a correlation between efficiency and morphological properties. Total organic content removal by PbS2 is 69.5 % while that of PbS1 is 64.2 % and PbS3 is 40.1 %. The as-prepared PbS nanoparticles exhibited remarkable photostability in the recyclability studies.
10 citations
DOI•
TL;DR: In this article , the synthesis of copper sulfide and cadmium sulfide (CdS) bimetal sulfide composite by single source precursor using diethyl dithiocarbamate ligand was reported.
Abstract: Metal sulfides conjugated graphene oxide (GO) have captivated researchers owing to the elaborated opto‐electrochemical and photocatalytic properties. Current research reports the synthesis of Copper sulfide (CuS) and cadmium sulfide (CdS) bimetal sulfide GO composite by single‐source precursor using diethyl dithiocarbamate ligand. The synthesized alloy was deposited through electron beam deposition system. Characterization of the thin films was done by various techniques including, XRD, UV‐visible spectrophotometry, fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM)‐energy dispersive X‐ray analysis (EDX). Electrochemical properties were investigated through cyclic voltammetry and linear sweep voltammetry using 3‐M KOH. Degradation of toxicants such as methyl red dye, pesticide isopyrazam, and phenol was done by the thin film to evaluate its photocatalytic characteristic. (CuS‐CdS)GO thin film showed separate bandgaps for CuS and CdS as 2.04 and 3.3 eV. A hexagonal crystal system for (Cu2S‐CdS)GO was observed through XRD with an average crystal size of 50 nm. A cubic shape with globular edges was detected by SEM investigation. An impressive specific capacitance value of 35 F g−1 at 100 mV s−1 proved it as a promising electrode for supercapacitors. A remarkable photocatalytic degradation rate was obtained by the thin film for all the toxicants with the highest rate for pesticide, that is, 81% under just 60 minutes, which remained >70% even after four successive cycles. The profound electrochemical and photocatalytic properties of (Cu2S‐CdS)GO thin film make it an auspicious material for optical, electrical, and photo‐devices.
10 citations
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TL;DR: This paper could serve as a general literature citation when one or more of the open-source SH ELX programs (and the Bruker AXS version SHELXTL) are employed in the course of a crystal-structure determination.
Abstract: An account is given of the development of the SHELX system of computer programs from SHELX-76 to the present day. In addition to identifying useful innovations that have come into general use through their implementation in SHELX, a critical analysis is presented of the less-successful features, missed opportunities and desirable improvements for future releases of the software. An attempt is made to understand how a program originally designed for photographic intensity data, punched cards and computers over 10000 times slower than an average modern personal computer has managed to survive for so long. SHELXL is the most widely used program for small-molecule refinement and SHELXS and SHELXD are often employed for structure solution despite the availability of objectively superior programs. SHELXL also finds a niche for the refinement of macromolecules against high-resolution or twinned data; SHELXPRO acts as an interface for macromolecular applications. SHELXC, SHELXD and SHELXE are proving useful for the experimental phasing of macromolecules, especially because they are fast and robust and so are often employed in pipelines for high-throughput phasing. This paper could serve as a general literature citation when one or more of the open-source SHELX programs (and the Bruker AXS version SHELXTL) are employed in the course of a crystal-structure determination.
81,116 citations
TL;DR: New features added to the refinement program SHELXL since 2008 are described and explained.
Abstract: The improvements in the crystal structure refinement program SHELXL have been closely coupled with the development and increasing importance of the CIF (Crystallographic Information Framework) format for validating and archiving crystal structures. An important simplification is that now only one file in CIF format (for convenience, referred to simply as `a CIF') containing embedded reflection data and SHELXL instructions is needed for a complete structure archive; the program SHREDCIF can be used to extract the .hkl and .ins files required for further refinement with SHELXL. Recent developments in SHELXL facilitate refinement against neutron diffraction data, the treatment of H atoms, the determination of absolute structure, the input of partial structure factors and the refinement of twinned and disordered structures. SHELXL is available free to academics for the Windows, Linux and Mac OS X operating systems, and is particularly suitable for multiple-core processors.
28,425 citations
TL;DR: OLEX2 seamlessly links all aspects of the structure solution, refinement and publication process and presents them in a single workflow-driven package, with the ultimate goal of producing an application which will be useful to both chemists and crystallographers.
Abstract: New software, OLEX2, has been developed for the determination, visualization and analysis of molecular crystal structures. The software has a portable mouse-driven workflow-oriented and fully comprehensive graphical user interface for structure solution, refinement and report generation, as well as novel tools for structure analysis. OLEX2 seamlessly links all aspects of the structure solution, refinement and publication process and presents them in a single workflow-driven package, with the ultimate goal of producing an application which will be useful to both chemists and crystallographers.
19,990 citations
TL;DR: The density-functional based tight-binding model is a useful tool to investigate the electronic and structural properties, including electron conductance, of large MoS2 structures, which show spontaneous rippling in finite-temperature molecular dynamics simulations.
Abstract: ConspectusAfter the discovery of graphene and the development of powerful exfoliation techniques, experimental preparation of two-dimensional (2D) crystals can be expected for any layered material that is known to chemistry. Besides graphene and hexagonal boron nitride (h-BN), transition metal chalcogenides (TMC) are among the most studied ultrathin materials. In particular, single-layer MoS2, a direct band gap semiconductor with ∼1.9 eV energy gap, is popular in physics and nanoelectronics, because it nicely complements semimetallic graphene and insulating h-BN monolayer as a construction component for flexible 2D electronics and because it was already successfully applied in the laboratory as basis material for transistors and other electronic and optoelectronic devices.Two-dimensional crystals are subject to significant quantum confinement: compared with their parent layered 3D material, they show different structural, electronic, and optical properties, such as spontaneous rippling as free-standing mo...
248 citations
TL;DR: The precise control over the particle size enables tuning the absorption and emission spectra of the particles, and the relative intensity of the narrow and broad emission associated with deep surface traps is controlled.
Abstract: We present a simple and versatile method for the synthesis of high-quality size-controlled metal sulfide nanoparticles. A single compound (metal xanthate) is the precursor. A Lewis-base solvent is used to achieve a low reaction temperature of 50-150 degrees C, usually in air. Demonstrated with CdS, the precise control over the particle size (by regulating the temperature or the concentration) enables tuning the absorption and emission spectra of the particles. We also can control the relative intensity of the narrow (30-35 nm wide) excitonic emission (tunable in the range 430-480 nm with approximately 2% fluorescence quantum efficiency) and the broad emission associated with deep surface traps (in the range 550-700 nm). Using the same precursor CdS/ZnS core/shell particles are produced with a high PL yield ( approximately 14%).
164 citations