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31.
Four new low melting salts, “Ionic Liquids” consisting of the [CrIII(NCS)4(Phen)]? complex monoanion and imidazolium based cations A, with A = 1-ethyl-3-methylimidazolium (EMIm), 1-butyl-3-methylimidazolium (BMIm), 1,3-dimethyl-2,4,5-triphenylimidazolium (DML), and 1,2,3,4,5-pentamethyl-imidazolium (PMIm), were investigated. Single-crystal X-ray investigations established the structures of the four compounds. (EMIm)[Cr(NCS)4(Phen)] (I): triclinic, \(P\bar 1\), a = 8.1382(6), b = 10.4760(8), c = 16.003(1) Å, α = 90.330(4)°, β = 94.759(4)°, γ = 107.305(4)°, Z = 2, R 1(F)/wR 2(F 2) = 0.0650/0.1770; (BMIm)[Cr(NCS)4(Phen)] (II): triclinic, \(P\bar 1\), a = 8.5545(4), b = 9.8620(4), c = 16.6762(6) Å, α = 92.503(2)°, β = 97.517(2)°, γ = 91.249(2)°, Z = 2, R 1(F)/wR 2(F 2) = 0.0393/0.0848; (DML)[Cr(NCS)4(Phen)] · C3H6O (III): triclinic, \(P\bar 1\), a = 11.0475(9), b = 13.589(1), c = 14.582(1) Å, α = 83.013(4)°, β = 87.116(4)°, γ = 70.333(5)°, Z = 2, R 1(F)/wR 2(F 2) = 0.0407/0.1023; (PMIm)[Cr(NCS)4(Phen)] · C3H6O (IV): orthorhombic, Pbca, a = 17.379(1), b = 16.514(1), c = 22.304(1) Å, Z = 8, R 1(F)/wR 2(F 2) = 0.0460/0.1107 (in addition III and IV contain co-crystallized acetone molecules). Each compound was characterized by elemental analysis, NMR, IR, und UV-Vis spectroscopy. Magnetic properties were derived from NMR investigations (EVANS method). All four compounds are paramagnetic with effective magnetic moments of spin-only CrIII. Melting points were obtained from DSC measurements. All melting points are higher than required for “Ionic Liquids”, but nevertheless “low” for molten salts. 相似文献
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Platinum Iodides PtI2 and Pt3I8 Powder samples of tetragonal Pt3I8 (a = 1166.4(1); c = 1068.2(2) pm) and the cubic α-form of PtI2 (a = 1109 pm) were obtained by thermal decomposition of PtI4 in closed quarz ampoules at a I2 pressure of 2–3 bar and 8 bar, respectively, and at 320°C and 430°C and 430°C, respectively. Single crystals of the monoclinic α-Form of PtI2 (a = 658.77(6); b = 871.50(34), c = 688.94(11) pm; β = 102.76°; Z = 4) were formed by hydrothermal synthesis from PtI4, KI, and I2 at 420°C. In the crystal structure of β-PtI2 two square planar PtI4-units are connected by a common edge to planar Pt2I6 groups which are linked by common corners to puckered layers. Crystals of Pt3I8 synthesized by hydrothermal synthesis from PtI4, KI, and I2 at 350°C were twinned and showed defects. As the result of X-ray studies the compound can be formulated as a mixed-valence platinum(II,IV) iodide PtI4 · 2 PtI2. Octahedral PtI6 and square planar PtI4 units are linked together to a three dimensional skeleton. 相似文献
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Tetramethyldisilane-1,2-diyl bridged Dicyclopentadienyl and Diindenyl Metal Dichlorides of the Group 4 Metals – Crystal Structure of Dicyclopentadienyl and diindenyl metal dichlorides of the type Cp′? SiMe2SiMe2? Cp′MCl2 (Cp′ = C5H4, M = Ti ( 1 ), Zr ( 2 ), Hf ( 3 ); Cp′ = C9H7, M = Zr ( 4 ), Hf ( 5 )) were synthesized and characterized by means of their 1H, 13C, 29Si-n.m.r., MS, and IR spectra. The crystal structure of 2 was determined. 相似文献
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Monomeric and Dimeric Oxovanadium(IV)-phenolate Complexes: Synthesis, Structure, and Reaction with a Reducing and Arylation Agent Reaction of [OVCl2(THF)2] with LiOMes yields dimeric [Li(Et2O)2OVCl2(μ-OMes)]2 ( 1 ) which can be converted with excess LiOMes to the substitution product [Li(THF)2OV(OMes)3(THF)] ( 2 ). Treatment of ( 1 ) with LiMes results in the formation of complexes [Li(THF)3OVMes3] ( 3 ) and [Li(THF)3OVMes2(OMes)] ( 4 ). Complex [{Li(THF)2OV(OMes)2(μ-OH)}2 · 2 THF] ( 6 ) has been isolated as a by-product of an unknown reaction of [OV(OMes)3] and Li. The structures of 1 , 2 , 3 , and 6 have been determined by X-ray analysis. In 1 (monoclinic, P21/c, a = 9.522(1) Å, b = 19.777(2) Å, c = 12.311(1) Å, β = 104.45(1)°, Z = 2) the vanadium atoms which are bridged by the phenolate ligands show a square-pyramidal coordination sphere. The central atom in 2 (monoclinic, P21/c, a = 17.755(2) Å, b = 11.629(1) Å, c = 20.956(3) Å, β = 113.98(1)°, Z = 4) has a bipyramidal environment which is realized by coordination of a THF donor molecule. The (THF)2Li fragment is bound via bridging phenolate ligands. The structure of 3 (orthorhombic, P212121, a = 15.465(2) Å, b = 15.456(2) Å, c = 15.469(2) Å, Z = 4) is built up by two tetrahedrons linked by the oxo atom. Dimeric 6 (triclinic, P1, a = 10.780(4) Å, b = 11.428(2) Å, c = 13.734(3) Å, α = 77.24(2)°, β = 84.79(2)°, γ = 74.35(2)°, Z = 1) has a structure similar to 1 . The vanadium atoms are bridged by two OH groups while phenolate ligands link the lithium cations with the vanadium atoms. 相似文献
38.
Contributions to the Chemistry of Transition Metal Alkyl Compounds. 58 On 2-(Dimethylaminomethyl)ferrocenyl Compounds of Vanadium, Molybdenum, Tungsten, Thorium, and Uranium Earlier results according to which dimethylaminomethylferrocenyl groups (FcN) are able to form stable organometallic chelate compounds were confirmed by synthesis of the heterobimetallic chelate compounds (FcN)2VO · Li(acac) II , (FcN)MoO2(acac) III , (FcN)WOCl3 IV , (FcN)Th(acac)3 V , and (FcN)UO2(acac) VI from the corresponding metal acetylacetonates or oxidchlorides and (FcN)Li I . The new compounds were characterized by elemental analysis, the i.r., 1H-n.m.r., and electron spectra and by their effective magnetic moments. 相似文献
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