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61.
D. O. Zakir’yanov V. A. Chernyshev I. D. Zakir’yanova 《Physics of the Solid State》2016,58(2):325-332
IR and Raman spectra of Pb3O2Cl2 in the range of 50–600 cm–1 have been detected for the first time. Ab initio calculations of the crystal structure and the phonon spectrum of Pb3O2Cl2 in the framework of LCAO approach have been performed by the Hartree–Fock method and in the framework of the density functional theory with the use of hybrid functionals. The results of calculations have made it possible to interpret the experimental vibration spectra and reveal silent modes, which do not manifest themselves in these spectra but influence the optical properties of the crystal. 相似文献
62.
Emira J. Visser Priyadarshini Jaishankar Eline Sijbesma Marloes A. M. Pennings Edmee M. F. Vandenboorn Xavier Guillory R. Jeffrey Neitz John Morrow Shubhankar Dutta Adam R. Renslo Luc Brunsveld Michelle R. Arkin Christian Ottmann 《Angewandte Chemie (International ed. in English)》2023,62(37):e202308004
Small-molecule stabilization of protein-protein interactions (PPIs) is a promising strategy in chemical biology and drug discovery. However, the systematic discovery of PPI stabilizers remains a largely unmet challenge. Herein we report a fragment-linking approach targeting the interface of 14-3-3 and a peptide derived from the estrogen receptor alpha (ERα) protein. Two classes of fragments—a covalent and a noncovalent fragment—were co-crystallized and subsequently linked, resulting in a noncovalent hybrid molecule in which the original fragment interactions were largely conserved. Supported by 20 crystal structures, this initial hybrid molecule was further optimized, resulting in selective, 25-fold stabilization of the 14-3-3/ERα interaction. The high-resolution structures of both the single fragments, their co-crystal structures and those of the linked fragments document a feasible strategy to develop orthosteric PPI stabilizers by linking to an initial tethered fragment. 相似文献
63.
64.
Hansen RK Broadhurst RW Skelton PC Arkin IT 《Journal of the American Society for Mass Spectrometry》2002,13(12):1376-1387
We demonstrate here that the hydrogen/deuterium solvent exchange (HDX) properties of the transmembrane fragment of the M2 protein of Influenza A (M2-TM) incorporated into lipid vesicles or detergent micelles can be studied with straightforward electrospray (ESI) and nanospray mass spectrometry (MS) configurations provided that key factors, including sample preparation techniques, are optimized. Small unilamellar vesicle preparations were obtained by solubilizing dimyristoyl phosphatidylcholine (DMPC) and the M2-TM peptide in aqueous solution with n-octyl-β-D-glycopyranoside, followed by dialysis to remove the detergent. Electron microscopy experiments revealed that subsequent concentration by centrifugation introduced large multilamellar aggregates that were not compatible with ESI-MS. By contrast, a lyophilization-based concentration procedure, followed by thawing above the liquid crystal transition temperature of the lipid component, maintained the liposome size profile and yielded excellent ion fluxes in both ESI-MS and nano-ESI-MS. Using these methods the global HDX profile of M2-TM in aqueous DMPC vesicles was compared with that in methanol, demonstrating that several amide sites were protected from exchange by the lipid membrane. We also show that hydrophobic peptides can be detected by ESI-MS in the presence of a large molar excess of the detergent Triton X-100. The rate of HDX of M2-TM in Triton X-100 micelles was faster than that in DMPC vesicles but slower than when the peptide had been denatured in methanol. These results indicate that the accessibility of backbone amide sites to the solvent can be profoundly affected by membrane protein structure and dynamics, as well as the properties of model bilayer systems. 相似文献
65.
Arkin CR Griffin TP Ottens AK Diaz JA Follistein DW Adams FW Helms WR 《Journal of the American Society for Mass Spectrometry》2002,13(8):1004-1012
This work is aimed at understanding the aspects of designing a miniature mass spectrometer (MS) system. Several types of small MS systems are evaluated and discussed, including linear quadrupole, quadrupole ion trap, time of flight, and sector. Analysis of hydrogen, helium, oxygen, and argon in a nitrogen background with the concentrations of the components of interest ranging from 0 to 5000 parts per million (ppm). The performance of each system in terms of accuracy, precision, limits of detection, response time, recovery time, scan rate, size, and weight is assessed. The relative accuracies of the systems varied from <1% to approximately 40% with an average below 10%. Relative precisions varied from 1% to 20%, with an average below 5%. The detection limits had a large distribution, ranging from 0.2 to 170 ppm. The systems had a diverse response time ranging from 4 to 210 s, as did the recovery time with a 6-to-210-s distribution. Most instruments had scan times near 1 s; however, one instrument exceeded 13 s. System weights varied from 9 to 52 kg and sizes ranged from 15 x 10(3) cm3 to 110 x 10(3) cm3. A performance scale is set up to rank each system, and an overall performance score is given to each system. 相似文献
66.
An attempt is made to remove certain omissions and inconsistencies in the recent work of Mishra and Lai (European J. Oper. Res., 178:20–26, 2007). 相似文献
67.
Bioengineering Functional Copolymers. IX. Poly[(maleic anhydride-co-hexene-1)-g-poly(ethylene oxide)
Amphiphilic bioengineering copolymers having a combination of hydrophilic/hydrophobic linkages and polyelectrolyte behavior, along with an ability to interact with biomacromolecules, in particular with the invertase enzyme, have been synthesized by (a) complex-radical copolymerization of maleic anhydride (MA, the acceptor) and hexene-1 (H-1, the donor) monomers with benzoyl peroxide as the initiator in 1,4-dioxane at 65 degrees C under high-conversion conditions and (b) subsequent grafting (polyesterification) of synthesized poly(MA-alt-H-1) with alpha-methoxy-omega-hydroxy-poly(ethylene oxide) (PEO). Copolymerizations were also carried out in the steady state, in order to essentially reduce the effect of copolymer composition drift. The values of the monomer reactivity ratios (r(1) and r(2)) determined by using the known terminal models of Fineman-Ross (FR) and Kelen-Tüd?s (KT), as well as by nonlinear regression (NLR) analysis, are: r(1) = 0.16 and r(2) = 0.30 (FR), r(1) = 0.14 and r(2) = 0.27 (KT), and r(1) = 0.15 and r(2) = 0.29 (NLR), respectively. All the copolymers and graft copolymers were characterized by FTIR spectroscopy, (1)H{(13)C} NMR spectroscopy, viscometric measurements, and chemical (acid number), thermal (DSC and TGA), and X-ray diffraction analyses. Unlike poly(MA-alt-H-1)s, PEO macrobranched graft copolymers exhibit expressed polyelectrolyte and swelling behavior in diluted and concentrated dioxane solutions, respectively. The copolymer and its PEO hyperbranched derivatives can be used as carriers for enzyme immobilization. 相似文献
68.
69.
在三乙胺作用下,N-取代苯基马来酰亚胺与α-氯代对甲氧基苯甲醛肟发生1,3-偶极环加成反应,合成了6个新型3-(对甲氧基苯基)-5-芳基-3a,6a-二氢-4,6-二氧代氮杂茂并[3',4'-d]异噁唑衍生物,其结构经1H NMR, IR和元素分析确证. 相似文献
70.
This work describes the synthesis and macromolecular reactions of citraconic anhydride (CA)–acrylamide (AAm) binary reactive copolymers with γ‐aminopropyltriethoxysilane (APTS) as a polyfunctional crosslinker. Copolymers with given composition of poly(CA‐alt‐AAm) were synthesized by radical binary copolymerization with benzoyl peroxide (BPO) as an initiator in benzene at 70°C in nitrogen atmosphere with initial monomer ratio 1 : 1. It was shown that the network structure is formed in poly(CA‐alt‐AAm)/APTS in water by intermolecular reactions between the anhydride unit and the amine group, as well as between the ethoxysilyl fragment and free carboxyl groups of the CA unit and amide unit of AAm. Swelling parameters such as beginning time of the hydrogel‐formation, initial rate of the swelling, swelling rate constant, equilibrium swelling and equilibrium water content were determined for the copolymer/APTS/water system with certain (2.75 : 1) copolymer/crosslinker ratio. Formation of a hyperbranched network structure through the fragmentation of side‐chain reactive groups in studied systems was confirmed by Fourier transform infrared spectroscopy (FT‐IR) method. Copyright © 2004 John Wiley & Sons, Ltd. 相似文献