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Nanoscale Electrocrystallization
Published in Klaus D. Sattler, st Century Nanoscience – A Handbook, 2019
In the case of TTF and TMTSF derivatives, we site-selectively synthesized a TTF-based nanocrystal only in the gap between the two electrodes [41,42]. To synthesize the partially oxidized TTF nanocrystal, tetrabutylammonium nitrate was used as the electrolyte to introduce the counter anion. The TMTSF-based nanocrystals were also first site-selectively synthesized using nanoscale electrocrystalliza-tion. Tetrabutylammonium perchlorate and tetrabutylam-monium nitrate were utilized as the electrolyte to introduce the counter anion. The site-selective formation of nanocrys-tals was observed using a square-waveform AC voltage of 1.0-1.5 V (peak-to-peak) and a frequency of 5.0-10.0 kHz for 5-10 min in TTF salts, and using a square-waveform AC voltage of 0.5-2.0 V (peak-to-peak) and a frequency of 2.0-5.0 kHz for 0.5-15 min in TMTSF salts (Figures 19.11a and 19.12a, respectively).
Solvothermal preparation of nano cobalt sulfide from tris (cyclohexylpiperazinedithiocarbamato)cobalt(III) and characterization, single crystal X-ray crystal structure of the precursor
Published in Journal of Coordination Chemistry, 2020
K. Ramalingam, S. Srinivasan, C. Rizzoli
IR spectra of the precursors were recorded on an Avatar Nicolet FT-IR spectrophotometer from 4000–400 cm−1 as KBr pellets. Electronic spectra were recorded in CH2Cl2 on a Hitachi U-2001 double beam spectrophotometer. 1H and 13C NMR spectra were recorded on a Bruker AMX-400 spectrometer at room temperature using CDCl3 as solvent. Scanning electron micrographs were recorded with JOEL JSM-5610 v microscopes. Cyclic voltammetric studies were carried out using a CH1604C electrochemical analyzer. Glassy carbon was used as the working electrode and the counter electrode was a platinum wire. The reference electrode was Ag/AgCl. Tetrabutylammonium perchlorate (0.01 M) was used as supporting electrolyte. Experiments were carried out under oxygen-free atmosphere by bubbling purified nitrogen gas through the solution at room temperature. Thermal analysis was carried out on an STA 409 PC Thermal Science instrument. The powder diffraction patterns were recorded in the 2θ range, 2–80°, using a Bruker D8 diffractometer equipped with Cu-Kα radiation.
Synthesis, spectral and electrochemical studies of mononuclear samarium (II), europium (II) and ytterbium (II) complexes with a NNO donor Schiff base derived from 4-methyl-2,6-dibenzoylphenol and propane-1,3-diamine
Published in Inorganic and Nano-Metal Chemistry, 2019
Cyclic voltammetric measurements were carried out with an Advanced Electrochemical System, PARSTAT 2253 instrument equipped with a three-electrode system. The micro-cell model KO264 consisted of a platinum working electrode, platinum wire as auxiliary electrode and a non-aqueous Ag/Ag+ reference electrode with 0.1 mol L−1 AgNO3 in acetonitrile as a filling solution. Tetrabutylammonium perchlorate (0.1 mol L−1 solution in CH3CN) was used as the supporting electrolyte. Cyclic voltammograms with scan speeds of 50–500 mV s−1 were run in 10 × 10−3 mol L−1 CH3CN solution under nitrogen. Under these conditions the ferrocenium/ferrocene (fc+/fc) couple shows E½ at 0.060 V.
Biological evaluation of copper(II) complexes on N(4)−substituted thiosemicarbazide derivatives and diimine co-ligands using DNA interaction, antibacterial and in vitro cytotoxicity
Published in Journal of Coordination Chemistry, 2019
Neelaveni Rajendran, Abirami Periyasamy, Nithya Kamatchi, Vasantha Solomon
In order to evaluate and confirm the structure of mixed-ligand thiosemicarbazone-copper(II) complexes the following analytical and spectral characterizations were performed. The melting point of ligands was verified with open glass capillaries. Molar conductance of ligand and their consequent copper(II) complexes (1 × 10−3 M) were determined in DMF on an Elico CM 183 EC − TDS analyzer. The purity of the thiosemicarbazone ligands and copper(II) complexes were checked by a Vario EL-III elemental analyzer. The chloride and metal contents of the complexes were verified according to the literature method [20]. 1H and 13C NMR spectra were examined by CDCl3 as a solvent on a Bruker 300 MHz spectrophotometer using TMS as an internal standard to confirm the structure of the thiosemicarbazone ligands. The electronic spectra of the ligand and copper(II) complexes in DMF (10−3 M) solutions were recorded on a JASCO V-630 UV–vis spectrophotometer for 200–800 nm. FT-IR spectra of ligands and their corresponding copper(II) complexes were obtained in KBr discs from 4000 to 400 cm−1 on a Shimadzu FT − IR spectrophotometer 8400S to discover coordinating cites of the copper(II) complexes. Electrochemical properties (cyclic voltammetry [CV] and differential pulse voltammetry [DPV]) of the copper(II) complexes were studied on a CH electrochemical analyzer on 600C version 5.01 at room temperature using three electrode system. Tetrabutylammonium perchlorate (TBAP) was used as supporting electrolyte. The redox potential (E1/2) was calculated from the anodic (Epa) and cathodic peak (Epc) potential values 0.5(Epa + EPC). The electron paramagnetic resonance (EPR) spectra of the copper(II) complexes were recorded on both room temperature as well as liquid nitrogen temperature (77 K) using a VARIAN ESR-112 spectrometer and ESR JEOL JES-FA200 in DMF.