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Journal ArticleDOI: 10.1080/17415993.2020.1822838

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

04 Mar 2021-Journal of Sulfur Chemistry (Taylor & Francis)-Vol. 42, Iss: 2, pp 167-179
Abstract: Bis(thiomorpholinyldithicarbamate)Cu(II) complex was prepared and characterized by single crystal X-ray crystallography. The molecular structure revealed a mononuclear copper(II) ion bonded to two ...

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Topics: Crystal structure (55%), Single crystal (54%), Copper (51%)
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5 results found


Open accessJournal ArticleDOI: 10.3390/NANO11082000
04 Aug 2021-Nanomaterials
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.

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Topics: Rhodamine B (53%), Copper sulfide (51%), Particle size (51%) ... show more

4 Citations


Open accessJournal ArticleDOI: 10.3390/INORGANICS9090070
10 Sep 2021-
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.

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Topics: Dithiocarbamate (55%), Coordination complex (52%), Copper (51%) ... show more

3 Citations


Journal ArticleDOI: 10.1007/S10904-021-01957-8
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.

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1 Citations



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29 results found


Open accessJournal ArticleDOI: 10.1107/S0108767307043930
George M. Sheldrick1Institutions (1)
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.

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Topics: Personal computer (55%), Literature citation (53%)

77,177 Citations


Open accessJournal ArticleDOI: 10.1107/S2053229614024218
George M. Sheldrick1Institutions (1)
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.

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21,137 Citations


Journal ArticleDOI: 10.1107/S0021889808042726
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.

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Topics: User interface (59%), Graphical user interface (54%), Visualization (52%) ... show more

14,922 Citations


Journal ArticleDOI: 10.1021/AR500277Z
Thomas Heine1Institutions (1)
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...

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Topics: Graphene (56%), Band gap (55%), Direct and indirect band gaps (54%) ... show more

222 Citations


Journal ArticleDOI: 10.1021/JA028887H
Narayan Pradhan1, Shlomo Efrima1Institutions (1)
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%).

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Topics: Nanoparticle (53%), Cadmium sulfide (52%), Sulfide (52%) ... show more

159 Citations