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Synthetic methodology was developed to construct amino acid-[2]rotaxanes that have phenylalanine and 3,5-di-tert-butylbenzene as blocking groups and dibenzo-24-crown-8, derivatized with either N-acetylargininyl or a carboxylic group, as the ring. A relative measure of the intramolecular interaction energies between the functional groups in DMSO/water mixtures is obtained by comparing their pK(a) values. Rotaxane structures were investigated through 2D NMR analysis and molecular dynamics simulations. Association constants for complexes of amino acids and rotaxanes in various protonation states were determined in a variety of solvent systems by (1)H NMR analysis. The unique intracomponent interactions that exist in the rotaxanes and their ability to act as artificial receptors are discussed. 相似文献
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The reaction equilibria [H(4)L](2+) + Zn(OAc)(2) right harpoon over left harpoon [Zn(H(2)L)](2+) + 2HOAc (K(1)) and [Zn(H(2)L)](2+) + Zn(OAc)(2) right harpoon over left harpoon [Zn(2)L](2+) + 2HOAc (K(2)), involving zinc acetate and the perchlorate salts of the tetraiminodiphenol macrocycles [H(4)L(1)(-)(3)](ClO(4))(2), the lateral (CH(2))(n)() chains of which vary between n = 2 and n = 4, have been studied by spectrophotometric and spectrofluorimetric titrations in acetonitrile. The photoluminescence behavior of the complexes [Zn(2)L(1)](ClO(4))(2), [Zn(2)L(2)(H(2)O)(2)](ClO(4))(2), [Zn(2)L(2)(mu-O(2)CR)](ClO(4)) (R = CH(3), C(6)H(5), p-CH(3)C(6)H(4), p-OCH(3)C(6)H(4), p-ClC(6)H(4), p-NO(2)C(6)H(4)), and [Zn(2)L(3)(mu-OAc)](ClO(4)) have been investigated. The X-ray crystal structures of the complexes [Zn(2)L(2)(H(2)O)(2)](ClO(4))(2), [Zn(2)L(3)(mu-OAc)](ClO(4)), and [Zn(2)L(2)(mu-OBz)(OBz)(H(3)O)](ClO(4)) have been determined. The complex [Zn(2)L(2)(mu-OBz)(OBz)(H(3)O)](ClO(4)) in which the coordinated water molecule is present as the hydronium ion (H(3)O(+)) on deprotonation gives rise to the neutral dibenzoate-bridged compound [Zn(2)L(2)(mu-OBz)(2)].H(2)O. The equilibrium constants (K) for the reaction [Zn(2)L(2)(H(2)O)(2)](2+) + A(-) right harpoon over left harpoon [Zn(2)L(2)A](+) + 2H(2)O (K), where A(-) = acetate, benzoate, or the carboxylate moiety of the amino acids glycine, l-alanine, l-histidine, l-valine, and l-proline, have been determined spectrofluorimetrically in aqueous solution (pH 6-7) at room temperature. The binding constants (K) evaluated for these systems vary in the range (1-8) x 10(5). 相似文献
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Arkadiusz Bula Sebastian Jurczyk Błażej Chmielnicki Jacek Hulimka Marcin Kozłowski 《International Journal of Polymer Analysis and Characterization》2019,24(2):169-177
The paper presents the results of Dynamic-Mechanical Thermal Analysis (DMTA) for a selected methacrylate adhesive at the frequency range from 1 to 50?Hz and the heating rate of 1 and 3?°C/min, in the range from –70?°C to 180?°C. On the basis of the test results, the glass transition temperature was evaluated for three calculation methods. Master curves were also designated for three different reference temperatures: –20, +20 and +60?°C. Master curves were calculated using shift factors aT - calculated by numerical method. 相似文献
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Analía G. Dall’Asén Sophia I. Dimas Sarah Tyler Jessica F. Johnston Timothy R. Anderton Inese I. Ivans 《光谱学快报》2017,50(8):417-425
Meteorites provide precious clues about the formation of planets in the solar system. Here, an analytical method to study chondritic meteorites using low- and high-resolution micro-Raman spectroscopy is presented. An approach in mapping the distribution of mineral compositions of a sample is introduced by measuring ~104 Raman spectra along linear, micron-wide paths that traverse the sample to capture detail on small and large spatial scales (from micrometers to millimeters). To refine these analytical procedures, a well-defined chondrule and surrounding matrix of the carbonaceous chondrite Northwest Africa 3118 are analyzed. The morphology and elemental composition of the sample are also studied using scanning electron microscopy with energy-dispersive X-ray spectroscopy and creating composite maps with the images obtained by these techniques along the same Raman linear path. The Raman line scan maps of this sample show clear spatial segregation of constituents including pyroxene and olivine, both within and outside the chondrule. Graphitic carbon is also present and appears clustered in domains of a few hundred microns both in the matrix and in the central core of the chondrule. The results obtained with the scanning electron microscopy and energy-dispersive X-ray spectroscopy techniques show that iron is most abundant in the matrix surrounding the chondrule, while the chondrule is enhanced in silicon, magnesium, calcium, aluminum, and sodium. These findings provide a detailed identification of the elemental and mineralogical, spatial composition of the analyzed regions of Northwest Africa 3118. 相似文献