The effects of a new antidiabetic glycinium [(pyridine-2, 6-dicarboxylato) oxovanadate (V)] complex in high-fat diet of streptozotocin-induced diabetic rats.

OBJECTIVE: The present study aimed to evaluate the antidiabetic effects of glycinium [(pyridine-2, 6-dicarboxylato) oxovanadate (V)] complex in type 2 diabetes rat model. MATERIALS AND METHODS: Rats were allocated into 6 groups. Group I, nondiabetic rats; Group II, diabetic rats; Group III, diabetic rats receiving an intraperitoneal (i.p.) injection of metformin (45 mg/kg); Groups IV, V and VI were diabetic rats receiving i.p. injection of 5, 10, and 20 mg/kg of the complex for 3 weeks, respectively. Fasting blood glucose (FBG), insulin, liver enzymes, malondialdehyde (MDA), total antioxidant capacity (TAC), lipid profile, and HbA1c were measured. RESULTS: AST, ALT and GGT activities and MDA levels were increased, while TAC was decreased in diabetic animals. Treatment of diabetic rats improved the HOMA-IR and returned HbA1c level to the normal value as well as elevated TAC and reduced MDA level. CONCLUSION: We found that the complex possesses antidiabetic properties in experimental diabetes.

Monitoring of atropine anticholinergic drug using voltammetric sensor amplified with NiO@Pt/SWCNTs and ionic liquid.

In this work, the synergic impact of 1-ethyl-3-methylimidazolium methyl sulfate (EMMS) and NiO doped Pt decorated SWCNTs (NiO@Pt/SWCNTs) in carbon paste matrix was examined as an analytical tool for investigating electrochemical behavior of atropine. The voltammetric results revealed that NiO@Pt/SWCNTs/EMMS/CPE exhibited an excellent electrocatalytic activity towards redox reaction of atropine in aqueous solution pH = 10.0. The NiO@Pt/SWCNTs/EMMS/CPE offered the best electro-analytical conditions for monitoring of atropine in the concentration range of 4.0 nM-220 µM with an increase in oxidation current about 5.93 times. On the other hand, NiO@Pt/SWCNTs/EMMS/CPE displayed a long time stability (about 60 days) for monitoring of atropine. The ability of NiO@Pt/SWCNTs/EMMS/CPE as an electroanalytical tool for monitoring of atropine was investigated, and the recovery range was detected as to be 97.6%-104.25% for this goal.

New Pd/Co-Ni electrocatalysts for formic acid electrooxidation and their fabrication from inorganic precursor [Co0.14Ni1.86(dipic)2(phen)2(H2O)2]·4H2O.

Novel Pd/Co-Ni oxide composites were developed as electrocatalysts for formic acid electro-oxidation as a process that can be utilised in fuel cells and electrochemical sensors. For achieving this goal, the new complex [Co0.14Ni1.86(dipic)2(phen)2(H2O)2]·4H2O (1) was synthesised and used as an inorganic precursor for producing a Co-Ni mixed metal promoter. In the following, palladium nanoparticles were anchored on Co-Ni mixed metal oxides via a reaction of chemical reduction with four different loadings. The electrocatalytic activity of the electrocatalysts was investigated for HCOOH electro-oxidation by electrochemical studies. Compared with single component electrocatalysts, the new electrocatalysts exhibited higher current, improved absorption/desorption of hydrogen, and a higher loading for metal oxides.

Pt-Pd-doped NiO nanoparticle decorated at single-wall carbon nanotubes: An excellent, powerful electrocatalyst for the fabrication of An electrochemical sensor to determine nalbuphine in the presence of tramadol as two opioid analgesic drugs.

In this study, a Pt-Pd-doped NiO nanoparticle decorated at the surface of single-wall carbon nanotubes (Pt-Pd/NiO-NPs/SWCNTs) was synthesized using a simple chemical precipitation method and characterized by XRD, TEM, and EDS methods. The results confirmed that Pt-Pd/NiO-NPs/SWCNTs were synthesized with good purity and at the nanoscale size. Moreover, a highly sensitive electroanalytical sensor was fabricated by incorporating synthesized Pt-Pd/NiO-NPs/SWCNT nanocomposites into a carbon paste electrode (CPE) in the presence of 1-ethyl-3-methylimidazolium methanesulfonate (EMICH3SO3-) as binder. The Pt-Pd/NiO-NPs/SWCNTs/EMICH3SO3-/CPE showed a powerful electro-catalytic activity for electro-oxidation of nalbuphine, and the results confirmed that the oxidation of nalbuphine was improved 6.34 times and relative oxidation potential was decreased about 110 mV compared to unmodified electrodes. The Pt-Pd/NiO-NPs/SWCNTs/EMICH3SO3-/CPE also showed good catalytic activity for the determination of nalbuphine in the presence of tramadol and the oxidation potential of these opioid analgesic drugs separated with ΔE =460 mV. In the final step, the Pt-Pd/NiO-NPs/SWCNTs/EMICH3SO3-/CPE was used to determine nalbuphine with a detection limit of 0.9 nM and tramadol with a detection limit of 50.0 nM in drug samples. The results confirmed the powerful and interesting ability of the sensor in the analysis of a real sample.

Design and fabrication of novel thiourea coordination compounds as potent inhibitors of bacterial growth.

A new thiourea ligand (HL), namely N-(4-chlorophenyl)morpholine-4-carbothioamide and its Co(III), Ni(II) and Ag(I) complexes (1a, 1b and 1c) were synthesized and investigated by Fourier-transform infrared, 1H NMR and UV-visible spectroscopies. The compounds HL and 1c were characterized by single-crystal X-ray crystallography revealing the triclinic space group P[Formula: see text] for both compounds. The inhibitory effect of HL ligand, 1a, 1b, and 1c complexes was investigated with in vitro tests on Gram-positive and Gram-negative bacteria. For the 1c complex, the results showed that the coordination of the HL to Ag(I) ion increased its antibacterial effect especially against E. coli. The assays also indicated that for the same bacteria strains, the new complexes showed higher activity than the ligand, with the relative activity 1c > 1b > 1a > HL. Moreover, all samples were more suitable antimicrobial agents against the Gram-negative than those of the Gram-positive bacteria. Eventually, the relationship between the structure and bactericidal activities of these specimens was examined by calculating frontier molecular orbital (HOMO and LUMO) energies using density functional theory method at the 6-31 G*/LANL2DZ level of theory.

Binding interaction of a heteroleptic silver(I) complex with DNA: A joint experimental and computational study.

A new heteroleptic Ag(I) complex formulated as [Ag(daf)(phen)]NO3, where daf and phen stand for 4,5-diazafluoren-9-one and 1,10-phenanthroline, respectively, has been prepared and structurally characterized by elemental analysis, spectroscopic methods (IR, 1HNMR, and UV-Vis) and cyclic voltammetry. The geometry optimization around Ag(I) at the level of DFT has demonstrated that the Ag(I) center has been nested in a tetrahedral N4 coordination geometry which found to be in close agreement with the experimentally proposed structure. The bond lengths, angles, and the HOMO/LUMO energies have been calculated to substantiate the geometry of the complex. The DNA binding property of the Ag(I) complex has been explored in detail both theoretically (DFT and molecular docking) and experimentally (UV-Vis absorption spectroscopy, circular dichroism spectroscopy, luminescence quenching, competitive binding with ethidium bromide, cyclic voltammetry, and gel electrophoresis), indicating the good affinity of the Ag(I) complex for the intercalation (Kb (binding constant) = 3.45 × 105 M-1). Providing a fuller picture of Ag(I) complex-DNA interaction, the energy-minimized structure of the complex has been docked to the DNA with a d(AGACGTCT)2 sequence and the results are in close agreement with experimental achievements and make a deeper insight into the relationship between the structure and biological activity of the complex.

Electronic and fluorescent studies on the interaction of DNA and BSA with a new ternary praseodymium complex containing 2,9-dimethyl 1,10-phenanthroline and antibacterial activities testing.

In this study, fluorescence emission spectra, UV-vis absorption spectra, ethidium bromide (EB)-competition experiment, and iodide quenching experiment were used for the interaction study of the Fish salmon DNA (FS-DNA) with [Pr(dmp)2Cl3(OH2)] where dmp is 2,9-dimethyl 1,10-phenanthroline. The binding constant and the number of binding sites of the complex with FS-DNA were 6.09 ± 0.04 M-1 and 1.18, respectively. The free energy, enthalpy, and entropy changes (ΔG°, ΔH°, and ΔS°) in the binding process of the Pr(III) complex with FS-DNA were -8.02 kcal mol-1, +39.44 kcal mol-1, and +159.56 cal mol-1 K-1, respectively. Based on these results, the interaction process between FS-DNA with [Pr(dmp)2Cl3(OH2)] was spontaneous and the main binding interaction force was groove binding mode. Also, Fluorescence and electronic absorption spectroscopy were used in order to evaluate the binding characteristics, stoichiometry, and interaction mode of praseodymium(III) (Pr(III)) complex with bovine serum albumin (BSA). Title complex showed good binding propensity to BSA presenting moderately high Kb values. The fluorescence quenching of BSA by Pr(III) complex has been observed to be the static process. The positive ΔH° and ΔS° values showed that the hydrophobic interaction is the main force in the binding of Pr(III) complex and BSA. Eventually, the average aggregation number, , of BSA potentially induced by title complex confirmed the 1:1 stoichiometry for title complex-BSA adducts. In vitro, antimicrobial activity of title complex was indicated that the complex is more active against both Escherichia coli and Enterococcus faecalis bacterial strains than Staphylococcus aureus, and Pseudomonas aeruginosa. Communicated by Ramaswamy H. Sarma.

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), [Pb2(L)2(I)4]n, L  =  C4H6N2 (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 Pb2+ 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), [Pb2(L)2(Br)2]n·H2O (1), [Pb2(HL/)(L/)(H2O)2]n·H2O (2), where L = C6H5NO2 (2-pyridinecarboxylic acid) and L/ = C9H6O6 (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 Pb2+ 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.

Evaluation of DNA, BSA binding, and antimicrobial activity of new synthesized neodymium complex containing 29-dimethyl 110-phenanthroline.

In order to evaluate biological potential of a novel synthesized complex [Nd(dmp)2Cl3.OH2] where dmp is 29-dimethyl 110-phenanthroline, the DNA-binding, cleavage, BSA binding, and antimicrobial activity properties of the complex are investigated by multispectroscopic techniques study in physiological buffer (pH 7.2).The intrinsic binding constant (Kb) for interaction of Nd(III) complex and FS-DNA is calculated by UV-Vis (Kb = 2.7 ± 0.07 × 105) and fluorescence spectroscopy (Kb = 1.13 ± 0.03 × 105). The Stern-Volmer constant (KSV), thermodynamic parameters including free energy change (ΔG°), enthalpy change (∆H°), and entropy change (∆S°), are calculated by fluorescent data and Vant' Hoff equation. The experimental results show that the complex can bind to FS-DNA and the major binding mode is groove binding. Meanwhile, the interaction of Nd(III) complex with protein, bovine serum albumin (BSA), has also been studied by using absorption and emission spectroscopic tools. The experimental results show that the complex exhibits good binding propensity to BSA. The positive ΔH° and ∆S° values indicate that the hydrophobic interaction is main force in the binding of the Nd(III) complex to BSA, and the complex can quench the intrinsic fluorescence of BSA remarkably through a static quenching process. Also, DNA cleavage was investigated by agarose gel electrophoresis that according to the results cleavage of DNA increased with increasing of concentration of the complex. Antimicrobial screening test gives good results in the presence of Nd(III) complex system.

Nanocomposites: Synthesis, characterization and its application to removal azo dyes using ultrasonic assisted method: Modeling and optimization.

S-doped and Cu- and Co-doped TiO2 was synthesized by a sol-gel method and characterized by FE-SEM, XRD, EDX and FTIR. The Co/Cu/S-TiO2 nanocomposite loaded on the activated carbon as new nanoadsorbent was used for simultaneous removal of methylene blue (MB) and sunset yellow (SY) from aqueous solution by ultrasonic-assisted adsorption method. In this work, central composite design (CCD) and adaptive neuro-fuzzy inference system (ANFIS) as a support tool for examining data and making prediction are used to recognize and predict the removal percentage in MB and SY dye solution of different concentrations. The predictive capabilities of CCD and ANFIS are compared in terms of square correlation coefficient (R2), root mean square error (RMSE), mean absolute error (MAE) and absolute average deviation (AAD) against the empirical data. It is found that the ANFIS model shows the better prediction accuracy than the CCD model. In addition to, the optimization of ultrasound-assisted simultaneous removal of methylene blue (MB) and sunset yellow (SY) on the Co/Cu/S-TiO2/AC nanocomposite by response surface methodology (RSM) for the optimization of the process variables, such as MB and SY concentrations, Co/Cu/S-TiO2/AC nanocomposite dose and sonication time, was investigated. Various isotherm and kinetic models were used in the experimental data. The results revealed that the langmuir isotherm and pseudo-second-order model had a better correlation than the other models.

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)2]n (1) and [Hg2(L')2(SCN)2]·2H2O (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 Hg2+ 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.

Ultrasound irradiation effect on morphology and size of two new potassium coordination supramolecule compounds.

Two new potassium coordination supramolecular compounds (2D and 1D), [K(H3L)(H2L)(H2O)]n·H2O (1) and [K(H2L')(HL')(H2O)2]·H2O (2), (L=1,3,5-tricarboxylic acid, L'=2,6-pyridinedicarboxylic 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 microscopy (FE-SEM), scanning electron microscopy (SEM), powder X-ray diffraction (PXRD), FT-IR spectroscopy and elemental analyses. Single crystal X-ray analyses on compounds 1 and 2 show that K+ ions are 3- and 7-coordinated, respectively. Additionally, H-bonds incorporate the layers and chains in 1 and 2 into 3D and 2D (along (0,0,1) direction) frameworks. Topological analysis shows that the compound 1 and 2 are 3,6-coordinated kgd and 2,4-coordinated 2,4C4 net. The thermal stability of compounds 1 and 2 in bulk and nano-size has been studied by thermal gravimetric (TG) and differential thermal analyses (DTA) and compared each other. The role of different parameters like temperature, reaction time and ultrasound irradiation power on the growth and morphology of the nano-structures are studied. Results suggest that an increase of temperature, sonication power and reduction of reaction time led to a particle size decrease.

Influences of temperature, power ultrasound and reaction time on the morphological properties of two new mercury(II) coordination supramolecular compounds.

Nanoparticles of two new coordination compounds, [Hg2(L)2(Br)4]n (1) and [Hg(L')(SCN)2] (2), (L=2-amino-4-methylpyridine, L'=2,6-pyridinedicarboxlic acid), have been synthesized by use of a sonochemical process and characterized by scanning electron microscopy (SEM), field emission scanning electron microscopy(FESEM), X-ray powder diffraction (XRPD), Fourier transform infrared spectroscopy (FTIR) spectroscopy and elemental analyses. The single crystal X-ray data of compounds 1 and 2 imply that the Hg(II) ions are four and five coordinated, respectively. Topological analysis shows that 1D and 0D coordination networks of 1 and 2 can be classified as underlying nets of topological types 2C1 and 1,3M4-1, respectively. The thermal stability of compounds 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 "nano-structures" 1 and 2, has been investigated. Results claim that an increase of temperature, sonication power and decrease in reaction time leads to a decrease of particle size.

Synthesis, characterization, X-ray crystal structure, DFT calculation and antibacterial activities of new vanadium(IV, V) complexes containing chelidamic acid and novel thiourea derivatives.

Three new thiourea ligands derived from the condensation of aroyl- and aryl-isothiocyanate derivatives with 2,6-diaminopyridine, named 1,1'-(pyridine-2,6-diyl)bis(3-(benzoyl)thiourea) (L1), 1,1'-(pyridine-2,6-diyl)bis(3-(2-chlorobenzoyl)thiourea) (L2) and 1,1'-(pyridine-2,6-diyl)bis(3-(4-chlorophenyl)thiourea) (L3), their oxido-vanadium(IV) complexes, namely [VO(L1('))(H2O)] (C1), [VO(L2('))(H2O)] (C2) and [VO(L3('))(H2O)] (C3), and also, dioxo-vanadium(V) complex containing 4-hydroxy-2,6-pyridine dicarboxylic acid (chelidamic acid, H2dipic-OH) and metformin (N,N-dimethylbiguanide, Met), named [H2Met][VO2(dipic-OH)]2·H2O (C4), were synthesized and characterized by elemental analysis, FTIR and (1)H NMR and UV-visible spectroscopies. Proposed structures for free thiourea ligands and their vanadium complexes were corroborated by applying geometry optimization and conformational analysis. Solid state structure of complex [H2Met][VO2(dipic-OH)]2·H2O (triclinic, Pi) was fully determined by single crystal X-ray diffraction analysis. In this complex, metformin is double protonated and acted as counter ion. The antibacterial properties of these compounds were investigated in vitro against standard Gram-positive and Gram-negative bacterial strains. The experiments showed that vanadium(IV) complexes had the superior antibacterial activities than novel thiourea derivatives and vanadium(V) complex against all Gram-positive and Gram-negative bacterial strains.

Dichlorido(6-methyl-2,2'-bipyridine-κ(2)N,N')cobalt(II).

In the title compound, [CoCl(2)(C(11)H(10)N(2))], the Co(II) atom is four-coordinated in a distorted tetra-hedral geometry by two N atoms from a 6-methyl-2,2'-bipyridine ligand and two terminal Cl atoms. Inter-molecular C-H⋯Cl hydrogen bonds and π-π stacking inter-actions between the pyridine rings [centroid-centroid distance = 3.745 (3) Å] are present in the crystal.

Dichlorido(2,9-dimethyl-1,10-phenanthroline-κN,N')cobalt(II).

In the title compound, [CoCl(2)(C(14)H(12)N(2))], the Co(II) atom is four-coordinated in a distorted tetra-hedral geometry by two N atoms from a 2,9-dimethyl-1,10-phenanthroline ligand and two Cl atoms. The Co atom and the phenanthroline unit are located on a mirror plane. The methyl H atoms are disordered about the mirror plane and areeach half-occupied. In the crystal structure, π-π inter-actions between the pyridine and benzene rings and between the pyridine rings [centroid-centroid distances = 3.8821 (9) and 3.9502 (10) Å, respectively] stabilize the structure.

Dichlorido(6,6'-dimethyl-2,2'-bipyridine-κN,N')cobalt(II).

In the title compound, [CoCl(2)(C(12)H(12)N(2))], the Co(II) atom is four-coordinated in a distorted tetra-hedral geometry by two N atoms from a 6,6'-dimethyl-2,2'-bipyridine ligand and two terminal Cl atoms. Inter-molecular C-H⋯Cl hydrogen bonds and π-π stacking inter-actions between the pyridine rings [centroid-centroid distances = 3.788 (1) and 3.957 (1) Å] are present in the crystal structure.

(Acetyl-acetonato)(dicyanamido)(1,10-phenanthroline)copper(II) dihydrate.

In the title compound, [Cu(C(5)H(7)O(2))(C(2)N(3))(C(12)H(8)N(2))]·2H(2)O, the Cu(II) atom is five-coordinated in a square-pyramidal geometry with two acetyl-acetonate O and two phenanthroline N atoms forming the base. The apical position is occupied by the central N atom of the dicyanamide ligand. The dicyanamide N atoms are each involved in hydrogen bonds to water mol-ecules. There are also hydrogen bonds between both the water mol-ecules and their centrosymmetric pairs, creating a hydrogen-bonded chain along the b-axis direction.