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A. Weidinger J. Erxmeyer H. Glückler Ch. Niedermayer O. Laforsch J. Groß M. Mehring 《Hyperfine Interactions》1994,86(1):609-614
Hydrogenated YBa2Cu3O7 with [H]/cell=2.0 was studied by X-ray diffraction, SR and1H-NMR. For the first time, the hydride phase (16% larger c-axis) known from thin film experiments was seen in a bulk sample. A comparison of the SR and NMR results shows that the 15 mT site (2 MHz in SR) is the stable position for the proton and muon. The three other muon sites (4 MHz line and two exponentially decaying components) are metastable. 相似文献
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The bismuth tris(triorganosilanolates) [Bi(OSiR3)3] ( 1 , R = Me; 2 , R = Et; 3 , R = iPr) were prepared by reaction of R3SiOH with [Bi(OtBu)3]. Compound 1 crystallizes in the triclinic space group with Z = 2 and the lattice constants a = 10.323(1) Å, b = 13.805(1) Å, c = 21.096(1) Å and α = 91.871(4)°, β = 94.639(3)°, γ = 110.802(3)°. In the solid state compound 1 is a trimer as result of weak intermolecular bismuth‐oxygen interactions with Bi–O distances in the range 2.686(6)–3.227(3) Å. The coordination at the bismuth atoms Bi(1) and Bi(3) is best described as 3 + 2 coordination whereas Bi(2) shows a 3 + 3 coordination. The intramolecular Bi–O distances fall in the range 2.041(3)–2.119(3) Å. Compound 3 crystallizes in the orthorhombic space group Pbcm with Z = 4 and the lattice constants a = 7.201(1) Å, b = 23.367(5) Å and c = 20.893(1) Å, whereas the triethylsilyl‐derivative 2 is liquid. In contrast to [Bi(OSiMe3)3] ( 1 ) compound 3 is monomeric in the solid state, but shows similar intramolecular Bi–O distances in the range 1.998(2)–2.065(5) Å. The bismuth silanolates are highly soluble in common organic solvents and strongly moisture sensitive. Compound 1 shows the lowest thermal stability. 相似文献
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Michael Mehring Christian LÖW Ioannis Vrasidas Markus SchÜRmann Klaus Jurkschat 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1):311-318
Recent results are reported on the application of the novel O,C,O-coordinating pincer ligand {2,6-[P(O)(OEt)2]2-4-tert-Bu-C6H2} (A) for the synthesis of hypercoordinate organotin(IV) compounds ASnR3 (R = Ph, Cl), heteroleptic stannylenes ASnR (R = Cl, CH2SiMe3) and intramolecularly coordinated 1,2,5-oxaphosphastannolanes. 相似文献
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The quadrupole part of the spin echo signal is measured in the case of doped (Cu63+3.2 mol % Sn) and of highly deformed (i.e. distorted dislocation) bulk metals (Al27), where the NMR-signal is distorted by the skin effect. Theoretical expressions for the quadrupolar part due to point defects and dislocations are found to be in agreement with the experimental curves. 相似文献
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We have applied 13C cross-polarization (CP) powder- and MAS-NMR to cis- and trans-polyacetylene. All three elements of the chemical shift tensor (σ11, σ22, σ33) were determined in p.p.m. with respect to TMS as: (a) Cis; σ11 = ?228, σ22 = ?139, σ33 = ?17; (b) Trans; σ11 = ?234, σ22 = ?146, σ33 = ?34. 相似文献
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The structure of tert-butylphosphonic acid in the solid, in solution, and in the gas phase was studied by single-crystal X-ray diffraction, (1)H and (31)P NMR spectroscopic studies in solution, solid-state (31)P NMR spectroscopy, and electrospray ionization mass spectrometry. In addition, density functional theory (DFT) calculations at the B3LYP/6-31G*, B3LYP/6-31+G*, and B3LYP/6-311+G* level of theory for a large number of H-bonded aggregates of the type (tBuPO(3)H(2))(n) (C(n), P(n); n=1-7) support the experimental work. Crystallization of tBuPO(3)H(2) from polar solvents such as CH(3)CN or THF gives the H-bonded one-dimensional polymer 2, whereas crystallization from the less polar solvent CDCl(3) favors the formation of the H-bonded cluster (tBuPO(3)H(2))(6).CDCl(3) (1). In CDCl(3) the hexamer (tBuPO(3)H(2))(6) (C(6)) is replaced by smaller aggregates down to the monomer with decreasing concentration. DFT calculations and natural bond orbital (NBO) analyses for the clusters C(1)-C(7) and the linear arrays P(1)-P(7) reveal the hexamer C(6) to be the energetically favored structure resulting from cooperative strengthening of the hydrogen bonds in the H-bonded framework. However, the average hydrogen bond strengths calculated for C(6) and P(2) do not differ significantly (42-43 kJ mol(-1)). The average distances r(O.O), r(Obond;H), r(Pdbond;O), and r(Pbond;OH) in C(1)-C(7) and P(1)-P(7) are closely related to the hydrogen bond strength. Electrospray ionization mass spectrometry shows the presence of different anionic species of the type [(tBuPO(3)H(2))(n)-H](-) (A(1)-A(7), n=1-7) depending on the instrumental conditions. DFT calculations at the B3LYP/6-31G* level of theory were carried out for A(1)-A(6). We suggest the dimer [(tBuPO(3)H(2))(2)-H](-) (A(2)) and the trimer [(tBuPO(3)H(2))(3)-H](-) (A(3)) are the energetically favored anionic structures. A hydrogen bond energy of approximately 83 kJ mol(-1) was calculated for A(2). Electrospray ionization mass spectrometry is not suitable to study the assembling process of neutral H-bonded tert-butylphosphonic acid since the removal of a proton from the neutral aggregates has a large influence on the hydrogen bond strength and the cluster structure. 相似文献
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H. Mehring 《Fresenius' Journal of Analytical Chemistry》1900,39(3):162-163
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