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Marc B. Taraban Daniel J. Deredge Margaret E. Smith Katharine T. Briggs Yu Li Zhong-Xing Jiang Patrick L. Wintrode Yihua Bruce Yu 《Magnetic resonance in chemistry : MRC》2019,57(10):861-872
The conformational transition of a fluorinated amphiphilic dendrimer is monitored by the 1H signal from water, alongside the 19F signal from the dendrimer. High-field NMR data (chemical shift δ, self-diffusion coefficient D, longitudinal relaxation rate R1, and transverse relaxation rate R2) for both dendrimer (19F) and water (1H) match each other in detecting the conformational transition. Among all parameters for both nuclei, the water proton transverse-relaxation rate R2(1H2O) displays the highest relative scale of change upon conformational transition of the dendrimer. Hydrogen/deuterium-exchange mass spectrometry reveals that the compact form of the dendrimer has slower proton exchange with water than the extended form. This result suggests that the sensitivity of R2(1H2O) toward dendrimer conformation originates, at least partially, from the difference in proton exchange efficiency between different dendrimer conformations. Finally, we also demonstrated that this conformational transition could be conveniently monitored using a low-field benchtop NMR spectrometer via R2(1H2O). The 1H2O signal thus offers a simple way to monitor structural changes of macromolecules using benchtop time-domain NMR. 相似文献
3.
15N n.m.r. spectra have been recorded from salts of 15N enriched ammonium ions in aqueous solution. Shifts of the resonance frequency have been attributed to direct interaction between the ammonium and its counter ion in solution. 相似文献
4.
The thermodynamic properties of a crystal lattice in the harmonic approximation are expressed in terms of a dispersion function conjugate to the spectral distribution of normal-mode vibrations. Frequency moments of the normal-mode distribution provide the necessary and sufficient information for construction of accurate bounds on the dispersion function and on the associated thermodynamic properties. This clarifies the successful employment of moment expansions and approximate frequency spectra in determinations of thermodynamic properties, and establishes the equivalence of recently devised continued-fraction and moment-theory techniques for investigating crystal lattice vibrations. When sufficient numbers of frequency moments are available, accurate histogram approximations to the normal-mode distribution, which correctly image band gaps and van Hove singularities, are obtained from Stieltjes inversion of the dispersion function, thereby providing an alternative to the more customary root-sampling techniques. 相似文献
5.
Benjamin D. Egleston Konstantin V. Luzyanin Michael C. Brand Rob Clowes Michael E. Briggs Rebecca L. Greenaway Andrew I. Cooper 《Angewandte Chemie (International ed. in English)》2020,59(19):7362-7366
Control of pore window size is the standard approach for tuning gas selectivity in porous solids. Here, we present the first example where this is translated into a molecular porous liquid formed from organic cage molecules. Reduction of the cage window size by chemical synthesis switches the selectivity from Xe‐selective to CH4‐selective, which is understood using 129Xe, 1H, and pulsed‐field gradient NMR spectroscopy. 相似文献
6.
Stephanie Greed Edward L. Briggs Dr. Fahima I. M. Idiris Dr. Andrew J. P. White Dr. Ulrich Lücking Dr. James A. Bull 《Chemistry (Weinheim an der Bergstrasse, Germany)》2020,26(55):12533-12538
Sulfonimidamides present exciting opportunities as chiral isosteres of sulfonamides, with potential for additional directional interactions. Here, we present the first modular enantioselective synthesis of sulfonimidamides, including the first stereoselective synthesis of enantioenriched sulfonimidoyl fluorides, and studies on their reactivity. A new route to sulfonimidoyl fluorides is presented from solid bench-stable, N-Boc-sulfinamide (Boc=tert-butyloxycarbonyl) salt building blocks. Enantioenriched arylsulfonimidoyl fluorides are shown to be readily racemised by fluoride ions. Conditions are developed, which trap fluoride and enable the stereospecific reaction of sulfonimidoyl fluorides with primary and secondary amines (100 % es, es=enantiospecificity) generating sulfonimidamides with up to 99 % ee. Aryl and alkyl sulfonimidoyl fluoride reagents are suitable for mild late stage functionalisation reactions, exemplified by coupling with a selection of complex amines in marketed drugs. 相似文献
7.
A study is presented of the localisation of excitonic states on extended molecular aggregates composed of identical monomers arising, not from disorder due to statistical energy shifts of the monomers, induced by environmental interactions (Anderson localisation), but rather simply due to changes in the orientation and geometrical arrangement of the transition dipoles. It is shown further that such small changes nevertheless can have a drastic effect on the shape of the vibronic spectrum of the aggregate. The vibronic spectra are calculated using the ‘coherent exciton scattering’ (CES) approximation whose derivation we generalise to be applicable to aggregates of arbitrary size and geometry. 相似文献
8.
Edward L. Briggs Arianna Tota Marco Colella Leonardo Degennaro Renzo Luisi James A. Bull 《Angewandte Chemie (Weinheim an der Bergstrasse, Germany)》2019,131(40):14441-14448
Sulfonimidamides are intriguing new motifs for medicinal and agrochemistry, and provide attractive bioisosteres for sulfonamides. However, there remain few operationally simple methods for their preparation. Here, the synthesis of NH‐sulfonimidamides is achieved directly from sulfenamides, themselves readily formed in one step from amines and disulfides. A highly chemoselective and one‐pot NH and O transfer is developed, mediated by PhIO in iPrOH, using ammonium carbamate as the NH source, and in the presence of 1 equivalent of acetic acid. A wide range of functional groups are tolerated under the developed reaction conditions, which also enables the functionalization of the antidepressants desipramine and fluoxetine and the preparation of an aza analogue of the drug probenecid. The reaction is shown to proceed via different and concurrent mechanistic pathways, including the formation of novel S≡N sulfanenitrile species as intermediates. Several alkoxy‐amino‐λ6‐sulfanenitriles are prepared with different alcohols, and shown to be alkylating agents to a range of nucleophiles. 相似文献
9.
The low velocity and low energy impact response of two common sheet mold compound (SMC) material systems—SMC-R27, and SMC-R37—were
investigated. In addition to characterizing the low velocity impact response and failure progression of the material systems,
the edge effects of diamond saw cutting, waterjet cutting and abrasive waterjet cutting were investigated using optical microscopy
and contact surface profilometry. Impact force–time and displacement–time responses were measured and used to characterize
energy absorption capabilities and potential correlation to post processing operation and fiber volume fraction. Pre and post-impact
edge surface micrographs were examined to relate the failure behavior on the machined surfaces. Experiments and measurements
all show that the failure zone size and growth behavior are clearly dependent on the edge finishing process. 相似文献
10.