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1.
H. Weiner H.-J. Lunk J. Fuchs B. Ziemer R. Stsser C. Pietzsch P. Reich 《无机化学与普通化学杂志》1991,594(1):191-201
Synthesis and Structure Studies of Ba2H[α-FeO4W12O36] · 26 H2O The heteropolyanion compound Ba2H[α-FeO4W12O36] · 26 H2O (I) crystallizes in the tetragonal space group P4 n2 with the lattice parameters a = 12.398(6), c = 18.721(6) Å; Z = 2; Dx = 4.128 g · cm?3. The structure was solved on a twinned crystal from 1029 observed reflections and refined to an index R of 7.6%. The calculations were done by means of a modified ORFLS-programme by Eitel and Bärnighausen. The heteropolyanion [α-FeO4W12O36]5? has the well known α-Keggin structure. The average distance of the four central oxygen atoms to the FeIII position (0, 0, 0) is 1.84 Å. The angles ? O? Fe? O are 112.3° (4X) and 103.9 (2X), respectively, which leads to an disphenoidal distortion of the FeO4 tetrahedron. The powder and single crystal ESR spectra of I show the anisotropy of the FeIII fine structure transition 1/2 ? ?1/2. The Mößbauer spectra confirm the tetragonal distortion of the central FeO4 tetrahedron (quadrupole splitting Δ ≈ 0.50 mm · s?1). 相似文献
2.
Results of phase generation and carbide formation after a shock wave treatment of the C80W2 steel are reported. It is shown that the reactions follow the energy supply to the steel by shock wave treatment. 相似文献
3.
Vasil"ev A. A. Vielhauer O. Engman L. Pietzsch M. Serebryakov E. P. 《Russian Chemical Bulletin》2002,51(3):481-487
Acylation of meso-2,3-dimethylbutane-1,4-diol with vinyl acetate in the presence of porcine pancreatic lipase (PPL) leads to the dextrorotatory monoacetate of the above diol with enatiomeric excess (ee) 58—64%. Absolute configuration of this scalemic specimen was determined by its sequential transformation to levorotatory lasiol, a metabolite of the Lasius ants. Partial hydrolysis of the corresponding meso-diacetate, mediated by PPL or by the Pseudomonas sp. lipase affords the monoacetate of opposite configuration with ee 72—86%, a formal intermediate in the synthesis of (3S,4R)-faranal. Other microbial lipases used are distinctive in low chemoselectivity. 相似文献
4.
This work is part of an effort to develop chelating agents for stable binding and easy conjugation of Re-188 to biologically interesting structures. Starting from the well-known in vivo stability of [(188)ReO(DMSA)(2)](-), we want to exploit this coordination system for the design of (188)ReO(V) chelates, which are stable toward reoxidation to perrhenate and toward ligand exchange under all conditions of radiopharmaceutical development. Therefore, a new type of tetradentate ligand has been synthesized by bridging two molecules of N,N'-diisobutyl-2,3-dimercaptosuccinamide with N-(3-aminopropyl)propane-1,3-diamine. The resulting stereoisomeric tetrathiolato S(4) ligand of composition ((i)()Bu)(2)N(O)C-C(SH)-C(SH)-C(O)NH-(CH(2))(3)-NH-(CH(2))(3)-NHC(O)-C(SH)-C(SH)-C(O)N((i)Bu)(2) forms anionic five-coordinate oxorhenium(V) complexes by a ligand-exchange reaction of NBu(4)[ReOCl(4)] in methanol. In the absence of a base, the compounds were isolated as "betaine", [ReO(S(4))], with the protonated nitrogen of the bridge serving as an internal "counterion". Two representatives have been fully characterized in both the solid and solution states and found to adopt the expected square-pyramidal coordination geometry. The equatorial plane is formed by four thiolate sulfur atoms, whereas the oxygen occupies the apical position. The orientation of the metal oxo group is exo in relation to the carbamido groups in both isomers. Both complexes are stereoisomeric regarding the junction of the triamine chain. 相似文献
5.
Half-sandwich complexes of the type [(RCOCp)M(CO)(3)] with M = Re and (99(m))Tc were synthesized from [M(OH(2))(3)(CO)(3)](+) in water. The R group can be an organic residue or a receptor binding biomolecule with a spacer to cyclopentadienyl (Cp). This provides a general route to Cp complexes of technetium without the need for starting from [TcBr(CO)(5)]. The X-ray structure of [(C(6)H(5)CH(2)COC(5)H(4))Tc(CO)(3)] has been elucidated. The compound crystallizes in the monoclinic space group P2(1)/c with a = 16.1454(9), b = 7.6300(6), and c = 12.3922(7) A and beta = 107.792(6) degrees. We have chosen a serotonergic receptor ligand (WAY) as an example for the derivatization of Cp with a bioactive molecule. WAY is linked to Cp by an aliphatic chain of variable length. The half-sandwich complexes were prepared from water and organic solvents. The structure of [(WAY4-Cp)Re(CO)(3)] could be elucidated. The compound crystallizes in the monoclinic space group P2(1)/c with a = 15.7112(6), b = 6.8775(3), and c = 25.5217(12) A and beta = 103.778(5) degrees. Quantification of inhibition constants gave a clear structure-activity relationship. A single methylene group between the receptor binding site and the half-sandwich complex gave an IC(50) of 217 nM for HT(1A), whereas a butylene linker resulted in retention of the inhibition constant with an IC(50) of 6 nM with respect to underivatized WAY. For use as radiopharmaceuticals, the compounds have also been prepared with (99m)Tc in quantitative yield. 相似文献
6.
The nature of protein crystals is discussed. Since protein crystals contain not only proteins but also other substances the usage of conventional terms (of industrial crystallization) of naming such crystals is questioned. The proof that there are other components than the protein itself in a protein crystal is given. It is suggested to use a procedure like in biotechnology to guarantee the production of the right protein crystals according to the PAT concept. It is suggested not to use other established names like “hydrates”, “solvates”, “but crystals for proteins since the definitions do not fit the nature of the protein crystals. 相似文献
7.
Beumer R Bubert C Cabrele C Vielhauer O Pietzsch M Reiser O 《The Journal of organic chemistry》2000,65(26):8960-8969
The synthesis of diastereo- and enantiomerically pure beta-aminocyclopropanecarboxylic acids (beta-ACCs) is described. Starting from pyrrole, (rac)-4 is readily obtained, which was kinetically resolved by enzymatic hydrolysis. Subsequent oxidation of (-)-4 and deformylation gives rise to the cis-beta-ACC derivative (ent)-9, while (+)-10 was converted to the trans-beta-ACC derivative 8. Both 8 and (ent)-9 and their benzyl esters 13 and 16, being conformationally restricted beta-alanine or gamma-aminobutyric acid (GABA) derivatives, represent useful building blocks for peptides containing unnatural amino acids. 相似文献
8.
The thermal switching behavior of individual perpendicularly magnetized nanoscale Fe islands consisting of 200-600 atoms only is studied by low-temperature spin-polarized scanning tunneling microscopy. Our results reveal that the switching rate is strongly affected by the particle shape; i.e., elongated islands switch much more rapidly than compact islands of the same volume. This observation is explained by different processes of magnetization reversal. Our results suggest that compact magnetic particles are an ideal choice for future perpendicular magnetic recording media because they are robust against thermal magnetization reversal. 相似文献
9.
Pietzsch J Kopprasch S Bergmann R 《Rapid communications in mass spectrometry : RCM》2003,17(8):767-770
N(O,S)-ethoxycarbonyltrifluoroethyl amino acid esters are formed by the reaction of amino acids with ethylchloroformate plus trifluoroethanol plus pyridine. The use of these derivatives for a rapid and sensitive determination of 3-chlorotyrosine, a highly specific marker of myeloperoxidase-catalyzed protein oxidation, by using standard gas chromatography/electron impact mass spectrometry, is discussed. 相似文献
10.
Qi Wang Hongjun Ni Annette Pietzsch Franz Hennies Yongping Bao Yimin Chao 《Journal of nanoparticle research》2011,13(1):405-413
Water-dispersible silicon nanoparticles (Si-NPs) are desirable for applications in biological techniques. A simplified method
to synthesize such particles is reported here. The resulting Si-NPs are water-dispersible and luminescent. Under the excitation
of UV light, the Si-NPs emit strong red light with a peak maximum at 606 nm and a quantum yield of 6%. They are highly stable,
and remain so over several weeks. Fourier Transform Infrared (FTIR) spectroscopy shows a visible Si–CH2 scissoring vibration mode. Furthermore, the surface chemical bondings were confirmed by X-ray photoelectron spectroscopy
(XPS). In the Si2p and C1s core levels, Si–C components are observed. The diameters of the synthesized Si-NPS as measured by atomic force microscope (AFM) are approximately
5 nm. Furthermore, the nanoparticles can be taken up by cultured cells. Fluorescence images of Si-NPs within MCF-7 human breast
cancer cells show they are distributed throughout the cell tissue. 相似文献