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81.
Conan F Le Gall B Kerbaol JM Le Stang S Sala-Pala J Le Mest Y Bacsa J Ouyang X Dunbar KR Campana CF 《Inorganic chemistry》2004,43(12):3673-3681
Under strictly anhydrous conditions, no reaction occurs between Mo(2)(O(2)CCMe(3))(4) and tetracyanoethylene, TCNE, at room temperature, but after addition of 1 equiv of water, a reaction proceeds to form [Mo(2)(O(2)CCMe(3))(3)((NC)(2)CC(CN)CONH)], 1. The compound contains a quadruple-bonded Mo(2) unit and the 2,3,3-tricyanoacrylamidate anion as a ligand (TC3A), a very unusual hydrolyzed form of TCNE. Two different solid-state structures were obtained after crystallization of 1. Crystals obtained from CH(2)Cl(2) consist of a two-dimensional network, and crystals grown from a C(6)H(6) solution form a 1-D chain motif. In both cases, the TC3A ligand acts as a polydentate ligand involving a bidentate OCN bridging unit and two CN groups. The electrochemical and spectroscopic (IR, UV/vis/near-IR, NMR, EPR) properties of 1 support the formulation in solution as a discrete 1:1 complex of the TC3A donor ligand and a Mo(2) unit with no charge transfer. The coordinated TC3A ligand exhibits redox properties similar to those of free TCNE. 相似文献
82.
Two discrete neutral dimanganese(II) and tetrazinc(II) complexes were synthesized from a rigid organic clip and the corresponding metal acetates. The compounds were characterized by elemental analysis and single crystal X-ray diffraction study. The manganese species is a dinuclear discrete product with two disordered acetates bridging two manganese centers, while the zinc one consists of two octahedral and two tetrahedral Zn(II) centers with both bridging acetates and triply micro(3)-hydroxides. Variable temperature magnetic measurement reveals the existence of weak antiferromagnetic interaction (J = -1.6 cm(-)(1); H = -2JS(1).S(2)) within the manganese complex. 相似文献
83.
Discrete, nanoscopic 3-D cages are prepared in high yield via coordination-driven self-assembly from a variety of building blocks, including bidentate 3-substituted pyridines, chiral, and silicon-based tripods. All are characterized by NMR ((31)P, (1)H) and electrospray ionization mass spectrometry. 相似文献
84.
Sylvie Le Stang 《Journal of fluorine chemistry》2003,119(2):141-149
The aldehydic benzyl ethers PhCH2OC6H4CHO (2; a/b = para/meta series) are readily available from the corresponding phenols and react with Wittig reagents derived from [Ph3PCH2CH2Rf8]+I− (Rf8=(CF2)7CF3) to give PhCH2OC6H4CHCHCH2Rf8 (86-93%, Z major). Reactions with H2 over Pd/C give the fluorous phenols HOC6H4(CH2)3Rf8(4a,b; 87-91%). Condensations with PCl3 and NEt3 (3.0:1.0:3.3 mol ratio) give the fluorous phosphites P[OC6H4(CH2)3Rf8]3(5a,b; 92-94%), but traces of 4a,b are difficult to remove. The phthalate-based benzyl ethers PhCH2OC6H3(COOR)2 (7; ,5/3,4 OC6H3-3,n-(R)2 series) are easily accessed and reduced with LiAlH4 to the diols PhCH2OC6H3(CH2OH)2(8c,d; 89-90%). Diol 8c and the Dess-Martin periodinane react to give the dialdehyde PhCH2OC6H3(CHO)2 (9c; 95%). This is elaborated by a sequence analogous to 2→4→5 to the fluorous phenol HOC6H3((CH2)3Rf8)2 (11c; 97%/96%, two steps) and phosphite P[OC6H3((CH2)3Rf8)2]3 (12c, 92%), from which traces of 11c are difficult to remove. Diol 8d can be similarly elaborated to 11d, but the dialdehyde 9d is labile and the combined yield of the Dess-Martin/Wittig steps is 32%. The CF3C6F11/toluene partition coefficients of 11c,d, and 12c (two pony tails; 70:30, 72:28, 92:8) are much higher than those of 4a and b (one pony tail; 12:88, 14:86). 相似文献
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87.
The synthesis of six new, functionalized 180 degrees pyridyl donor ligands and their coordination-driven self-assembly into supramolecular rectangles is reported. Three of the new donors have been functionalized with hydrophobic straight chain alkane units (C6, C12, and C18) while the remaining three have been functionalized with derivatized di-, tetra-, and hexaethylene glycol hydrophilic units (DEG, TEG, and HEG, respectively). The resulting self-assembled hydrophobic and hydrophilic supramolecular rectangles have been fully characterized by multinuclear NMR and electrospray ionization mass spectrometry. Molecular force field modeling suggests that the functionalized rectangles range in size from roughly 3.0 x 2.9 to 3.0 x 6.0 nm2 in size. 相似文献
88.
Ghosh K Zhao Y Yang HB Northrop BH White HS Stang PJ 《The Journal of organic chemistry》2008,73(21):8553-8557
The design and synthesis of two new hexakisferrocenyl hexagons has been achieved via coordination-driven self-assembly wherein the size and relative distribution of six ferrocene moieties has been precisely controlled. Insight into the structure and electronic properties of these supramolecules was obtained through electrochemical studies. 相似文献
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