Synthesis of [MnCl<Subscript>3</Subscript>(H<Subscript>2</Subscript>O)<Subscript>2</Subscript>(Hatz)]·H<Subscript>2</Subscript>O and investigation of its structure via X-ray diffraction,spectroscopic measurements and DFT calculations

The 3-amino-1,2,4-triazole (atz)-based manganese complex was prepared and characterized through single-crystal X-ray diffraction, IR, EPR, and UV–visible spectroscopy. In the crystal structure, individual complex are interconnected through N(O)–H…Cl hydrogen bonds into 1D undulating chains running parallel to the [110] direction of the unit cell. Chains further grow into 2D supramolecular layers by way of the lattice water molecules of coordination and the chloride anions (O–H…Cl). Layers pack along the b-axis of the unit cell mediated by O–H…Cl(N) and N–H…O(Cl) hydrogen bonds forming a 3D supramolecular architecture. The theoretical calculations were also performed to optimize the structure of the complexes in the gas phase to confirm the structures proposed by X-ray crystallography. In addition, IR and UV–visible spectra of complex were calculated and compared with the corresponding experimental spectra to complete the experimental structural identification. The three-dimensional Hirshfeld surface (3D-HS) and their relative two-dimensional fingerprint plots (2D-FP) reveal that the structure is dominated by H…Cl/Cl…H (50.5%), H…O/O…H (11.3%) and N…O/O…N (10.2%) contacts.     

Natural frequencies and mode shapes of initially curved carbon nanotube resonators under electric excitation

Estimating accurately the natural frequencies of electrically actuated carbon nanotubes (CNTs) has been an active research subject over the past few years. Despite the importance of the topic, robust knowledge is still missing in the understanding of the role of various physical parameters affecting the natural frequencies, such as the stretching of doubly clamped CNTs, the DC electrostatic force, and the initial curvature of slack CNTs. In this investigation, we use a 2D nonlinear curved beam model in the form of an arch to simulate the coupled in-plane and out-of-plane motions of a CNT with curvature. We calculate the variation of its natural frequencies and mode shapes with the level of slackness and the DC electrostatic load. Towards this end, we derive a reduced-order model using a multimode Galerkin procedure. We show various scenarios of mode crossing and mode veering as the levels of slackness and DC load are varied. Finally, we tackle the forced vibration problem of a curved CNT when actuated by small DC and AC loads. The results show the transfer of energy among the vibration modes involved in the veering phenomenon.     

Two‐Step Synthesis of Multifunctional γ‐Lactams from γ‐Lactone

We present herein an efficient and rapid method for the synthesis of N,1‐dialkyl‐4‐(2‐hydroxyethyl)‐5‐oxopyrrolidine‐3‐carboxamides based on the conversion of γ‐lactone to γ‐lactam via the conjugate addition of primary amines to an ethyl α‐functionalized acrylate followed by intramolecular cyclization.     

A conductometric biosensor for the estimation of the number of cleaving sites in peptides and proteins

A conductometric enzyme biosensor using proteinase K was developed and then tested to relate its electrical signal to the number of proteinase K hydrolysis sites in bovine serum albumin (BSA) and angiotensin, a ten amino acid peptide, with one cleaving site.The conductometric sensor presents a large linear range of response for BSA and angiotensin ranging from 0.5 to 8 mg/l and from 4 to 8 mg/l, respectively. For a same tested concentration (mg/l), the response for native BSA is 12 times higher than for angiotensin. Aspartam was used as negative test and no response was obtained with the proteinase K biosensor. The conductometric sensor permitted also to detect difference on enzyme activity on native and non-native BSA, a response three times higher was obtained for non-native BSA.     

A conductometric immunosensor based on functionalized magnetite nanoparticles for E. coli detection

We report a new approach for immunoassays based on magnetite nanoparticles for Escherichia coli (E. coli) detection using conductometric measurements. Biotinylated antibodies, anti-E. coli, were immobilized on streptavidin modified magnetite nanoparticles by biotin–streptavidin interaction. A layer of functionalized nanoparticles were directly immobilized on the conductometric electrode using glutaraldehyde cross-linking.The specific test with E. coli cells and the non specific test using Staphylococcus epidermidis (S. epidermidis) were investigated by conductometric measurements. Results show a good response as a function of antigen additions. The detection of 1 CFU/ml of E. coli induces a conductivity variation of 35 μS. The negative test shows good selectivity using the conductometric immunosensor. Conductometric measurements allow to detect 500 CFU/l.     

Infrared and polarized Raman spectra of a noncentrosymmetric compound "sodium samarium fluorosilicate" NaSmSiO4.0.25NaF

Chemical preparation, infrared and Raman spectra of sodium samarium fluorosilicate, NaSmSiO(4).0.25NaF are presented. The spectra are analyzed with regard to the symmetry, and the numbers of the SiO(4)(4-) internal vibrational modes observed in the Raman and infrared spectra are consistent with the predictions.     

Crystal structure and thermal study of the new hydrated cadmium-cerium(III) chloride CeCd4Cl11·13H2O

The new double-salt CeCd₄Cl₁₁·13H₂O in the ternary system CeCl₃-CdCl₂-H₂O has been prepared from aqueous solution upon evaporation at 5°C and characterized based on elemental analysis, spectroscopic data, thermal studies and X-ray powder and single-crystal diffraction. CeCd₄Cl₁₁·13H₂O crystallizes in the monoclinic space group P2₁ with a=7.667(2), b=17.351(3), c=11.970(2)Å, β=101.61(3)° and Z=2. After refinement of the structure the reliability factor R in the final cycle is 0.064. The structure can be regarded as consisting of endless double chains of CdCl₆ and CdOCl₅ octahedra and isolated tricapped triangular prisms surrounding the cerium cations. Differential scanning calorimetry showed that the title compound exhibits five endothermic anomalies interpreted from thermogravimetry. A comparison with the structure of SrCd₂Cl₆·8H₂O is proposed.     

Action des hydrazines fluoroalkylées sur les phosphoallènes: synthèse d’hydrazones N-fluoroalkylées β-phosphonatées

Ten phosphorylated β-hydrazones of structure R₂P(O)C(NNHR_F)CHR₂′ were prepared in 54-91% yield by heating the allenes R₂P(O)CHCCR₂′ with fluorinated hydrazines H₂NNHR_F in chloroform or methanol [R=Ph, OCH₂C(Me)₂CH₂O or OCH₂C(Me)(Pr)CH₂O, R′=H or Me and R_F=CH₂CF₃ or C₆F₅]. Two cyclohexyl derivatives were prepared similarly from R₂P(O)CHCCy. The triphenyl derivatives Ph₂P(O)CH₂C(NNHCH₂CF₃)Ph and Ph₂P(O)CH₂C(NNHC₆F₅)Ph were made in 91 and 68% yield by heating the ketones Ph₂P(O)CH₂C(O)Ph with an ethanol solution of the corresponding hydrazines. The stereochemistry of the hydrazones was determined by multinuclear NMR experiments. Compounds with C(NNHR_F)Me groups exist as a mixture of Z and E isomers, with the Z form predominating (fluorinated group syn to phosphorus). Those with C(NNHR_F)CHMe₂, C(NNHR_F)Cy or C(NNHR_F)Ph groups were formed selectively, the Z isomers being the only products. The results are explained by steric hindrance, the bulkier isopropyl, cyclohexyl or phenyl group disfavouring the E configuration. , , , NMR data, coupling constants and IR data are reported.     

Dynamical analysis and anti-oscillation-based adaptive control of the FO arch MEMS with optimality

Nonlinear Dynamics - This paper mainly investigates dynamical analysis and anti-oscillation-based adaptive control issues of the fractional-order (FO) arch microelectromechanical system (MEMS) with...