Sonochemical synthesis and characterization of a novel hetro-binuclear metal organic nano polymer based on picolinic acid ligand

Nanoparticles of one new lead and K coordination polymer (CP), {[Pb(pyc)(N)K].½HO} (1) Hpyc = picolinic acid ligand, has been synthesized by use of a sonochemical process and characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRPD), Fourier transform infrared spectroscopy (FTIR) spectroscopy and elemental analyses. The single crystal X-ray data of compound 1 imply that the Pb ion is seven coordinated. The thermal stability of compound 1 has been studied by thermogravimetric (TG) and differential scanning calorimetry (DSC). The role of temperature, reaction time and ultrasound irradiation power on the size and morphfology of the nano-structured compound obtained from 1, have been investigated. Results indicate that an increase of temperature and sonication power and a decrease in time reaction led to a decrease of particle size

Synthesis and characterization of a new nano lead(II) 0-D coordination supramolecular compound : a precursor to produce pure phase nano-sized lead(II) oxide

Nano-structure of a new 0D Pb(II) coordination supramolecular compound, [Pb(8-Quin)](ClO)(1), L = 8-HQuin = 8-hydroxyquinolin ligand has been synthesized by use of a sonochemical process and characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRPD), Fourier transform infrared spectroscopy (FTIR) and elemental analyses. The structure of compound 1 was determined by single-crystal X-ray diffraction. The single crystal X-ray data of compound 1 implies that the Pb ions are five coordinated. Each lead atom is coordinated to nitrogen and oxygen atoms of 8-hydroxyquinolin ligand. Topological analysis shows that the compound 1 is 1,2,3,4,4M12-1net. Nanoparticles of lead(II) oxide have been prepared by calcination of lead(II) coordination polymer at 500 °C that were characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRPD) and IR spectroscopy

Sonochemical synthesis of a novel nanoscale 1D lead(II) [Pb2(L)2(I)4]n coordination Polymer, survey of temperature, reaction time parameters

One new lead(II) coordination supramolecular complex (CSC) (1D), [Pb(L)(I)], L = CHN (1-methyl imidazole), has been synthesized under different experimental conditions. Micrometric crystals (bulk) or nano-sized materials have been obtained depending on using the branch tube method or sonochemical irradiation. All materials have been characterized by scanning electron microscopy (SEM), powder X-ray diffraction (PXRD) and FT-IR spectroscopy. Single crystal X-ray analyses on complex 1 showed that Pb ion is 4-coordinated. Topological analysis shows that the complex 1 is 2,3,5C2 net. Finally, the role of reaction time and temperature on the growth and final morphology of the structures obtained by sonochemical irradiation have been studied

Sonochemical synthesis of two novel Pb(II) 2D metal coordination polymer complexes : new precursor for facile fabrication of lead(II) oxide/bromide micro-nanostructures

Two new lead(II) coordination polymer complexes (CSCs) (2D), [Pb(L)(Br)]·HO (1), [Pb(HL)(L)(HO)]·HO (2), where L = CHNO (2-pyridinecarboxylic acid) and L = CHO (1,3,5-tricarboxylic acid), have been synthesized under different experimental conditions. Micrometric crystals (bulk) or microsized materials have been obtained depending on using the branch tube method or sonochemical irradiation. All materials have been characterized by scanning electron microscopy (SEM), powder X-ray diffraction (PXRD) and FT-IR spectroscopy. Single crystal X-ray analyses on complexes 1 and 2 shows that Pb ions are 8-coordinated, 7 and 9-coordinated, respectively. Topological analysis shows that the compound 1 and 2 are 4,6L26 and bnn net, respectively. However, neither the shape nor the morphology is maintained, showing the role of sonochemistry to modulate both morphology and dimensions of the resulting crystalline material, independently of whether we have a 2D coordination polymer (CP). Finally, micro structuration of lead(II) bromide oxide and lead(II) oxide have been prepared by calcination of two different lead (II) CPs at 700 °C that were characterized by SEM and XRD

Solvent-tuned ultrasonic synthesis of 2D coordination polymer nanostructures and flakes

Altres ajuts: the ICN2 is funded by the CERCA programme / Generalitat de Catalunya. Noemí Contreras Pereda's project that gave rise to these results received the support of a fellowship from "laCaixa" Foundation (ID 100010434). The fellowship code is LCF/BQ/ES17/11600012.Herein, a new 2-dimensional coordination polymer based on copper (II), {Cu₂(L)(DMF₂)}n, where L stands for 1,2,4,5-benzenetetracarboxylate (complex 1) is synthesized. Interestingly, we demonstrate that both solvent and sonication are relevant in the top-down fabrication of nanostructures. Water molecules are intercalated in suspended crystals of complex 1 modifying not only the coordination sphere of Cu(II) ions but also the final chemical formula and crystalline structure obtaining {[Cu(L)(H₂O)₃]·H₂O}n (complex 2). On the other hand, ultrasound is required to induce the nanostructuration. Remarkably, different morphologies are obtained using different solvents and interconversion from one morphology to another seems to occur upon solvent exchange. Both complexes 1 and 2, as well as the corresponding nanostructures, have been fully characterized by different means such as infrared spectroscopy, x-ray diffraction and microscopy

Nano-Fabrication Methods

In the field of investigating nano-fabrication, it is not possible to reach a single and separate definition compared to macro-fabrication. Nano-fabrication can be defined as an assembly process to produce a one-dimensional, two-dimensional, or three-dimensional structure at the nanometer scale. The importance of recognizing and examining nanofabrication techniques considering the revolution that nanofabrication compounds have in molecular adsorption, catalysis, magnetism, luminescence, nonlinear optics, and molecular sensing, have been known because they provide the possibility of reproducible mass production in this field. In this chapter, to create a general understanding of nano-fabrication and the challenge of creating nanometer size reduction, we will review new tools and techniques for the production of nanostructures, which are divided into three major parts: thin film, lithography, and engraving

Association of Cytochrome P450 2E1 and N-Acetyltransferase 2 Genotypes with Serum Isoniazid Level and Anti-Tuberculosis Drug-Induced Hepatotoxicity: A Cross-Sectional Study

Background: Anti-tuberculosis drug-induced hepatotoxicity can result from genetic polymorphism of the isoniazid (INH) metabolizing enzyme. This study aimed to determine the effect of genetic polymorphism of N-acetyltransferase 2 (NAT2) and cytochrome P450 2E1 (CYP2E1) genes on serum isoniazid level and drug-induced hepatotoxicity. Methods: A cross-sectional study was conducted on 120 patients (with and without hepatotoxicity) with pulmonary tuberculosis from June 2019 to April 2022 in Tehran (Iran). High-performance liquid chromatography was used to measure the serum concentration of INH and acetylisoniazid (AcINH). NAT2 and CYP2E1 genotypes were determined using polymerase chain reaction and restriction fragment length polymorphism methods. Data were analyzed using SPSS software (version 22.0) with independent two-sample t test, Chi square test, or Fisher’s exact test. P<0.05 was considered statistically significant.Results: A total of 40 patients showed hepatotoxicity. The risk of anti-tuberculosis drug-induced hepatotoxicity was significantly higher in patients who are slow acetylator (SA) phenotype than in rapid or intermediate acetylator (P<0.001). NAT2*4/*4 genotypes were not found in patients with hepatotoxicity. The frequency of NAT2*5 and NAT2*6 haplotypes and serum INH concentration was significantly higher in patients with hepatotoxicity than in those without (P=0.003, P<0.001, and P<0.001, respectively). NAT2*4 haplotype was correlated with protection against hepatotoxicity. A combination of SA and CYP2E1 C1/C1 genotype was significantly associated with hepatotoxicity (P<0.001). Conclusion: Hepatotoxicity in Iranian patients with tuberculosis was confirmed due to the presence of NAT2 SA polymorphism. Determining NAT2 and CYP2E1 genotypes and/or INH concentration can be a valuable tool to identify patients susceptible to hepatotoxicity

Sonochemical synthesis, characterization, and effects of temperature, power ultrasound and reaction time on the morphological properties of two new nanostructured mercury(II) coordination supramolecule compounds

Two new mercury(II) coordination supramolecular compounds (CSCs) (1D and 0D), [Hg(L)(I)] (1) and [Hg(L')(SCN)]·2HO (2) (L = 2-amino-4-methylpyridine and L' = 2,6-pyridinedicarboxlic acid), have been synthesized under different experimental conditions. Micrometric crystals (bulk) or nano-sized materials have been obtained depending on using the branch tube method or sonochemical irradiation. All materials have been characterized by field emission scanning electron microscope (FESEM), scanning electron microscopy (SEM), powder X-ray diffraction (PXRD) and FT-IR spectroscopy. Single crystal X-ray analyses on compounds 1 and 2 show that Hg ions are 4-coordinated and 5-coordinated, respectively. Topological analysis shows that the compound 1 and 2 have 2C1, sql net. The thermal stability of compounds 1 and 2 in bulk and nano-size has been studied by thermal gravimetric (TG), differential thermal analyses (DTA) for 1 and differential scanning calorimetry (DSC) for 2, respectively. Also, by changing counter ions were obtained various structures 1 and 2 (1D and 0D, respectively). The role of different parameters like power of ultrasound irradiation, reaction time and temperature on the growth and morphology of the nano-structures are studied. Results suggest that increasing power ultrasound irradiation and temperature together with reducing reaction time and concentration of initial reagents leads to a decrease in particle size

Achieving Different Morphologies for a Zinc(II) Coordination Polymer by Green Sonochemical Synthesis and New Precursors for the Preparation of Zinc(II) oxide

A new 2D zinc(II) coordination polymer(CP) 1, [Zn(N3)(L)]n(1), [L= 2-picolinate] has been synthesized using branch tube approach. Nano and micro structures of CP 1 were synthesized using sonochemical technique in diverse conditions (different times and solvents) and they were identified by elemental analysis, FT-IR spectra, scanning electron microscopy (SEM) and powder X-ray diffraction (PXRD). Single-crystal X-ray studies show that CP1 contains Zn(II) atoms with different coordination geometries (tetrahedral and octahedral). The effects of solvents and reaction time on the morphology and size of the nano and microstructure of CP 1 were also evaluated. The results showed that change in reaction time has almost no effect on the size of particles, but change in solvent leads to changes in the morphology of particles

Survey of temperature, reaction time and ultrasound irradiation power on sonochemical synthesis of two new nanostructured lead(II) coordination supramolecule compounds

Nanoparticles of two new 0D, lead(II) coordination supramolecular compounds, [Pb(L)2(I)2] (1) and [Pb(L)(L/)(H2O)]3H2O (2), (L = 1,10- phenanthroline monohydrate, L/ = 2,6-pyridinedicarboxlic acid), have been synthesized by a sonochemical process and characterized by scanning electron microscopy (SEM), field emission scanning electron microscopy (FE-SEM), X-ray powder diffraction (XRPD), FT-IR spectroscopy and elemental analyses. The single crystal X-ray data of compounds show that the Pb ion is six coordinated in both 1 and 2. The thermal stability of compound 1 and 2 has been studied by thermal gravimetric (TG) and differential thermal analyses (DTA). The role of temperature, reaction time and ultrasound irradiation power on the size and morphology of the nano-structured compound obtained from 1 and 2, have been investigated. Results indicate that an increase of temperature and sonication power and a decrease in time reaction led to a decrease of particle size. Topological analysis shows that the compound 1 and 2 are new topology for net: 1,4M5-1 and nch, respectively