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排序方式: 共有463条查询结果,搜索用时 15 毫秒
1.
Florence Robaut Alexandre Crisci Madeleine Durand-Charre Danielle Jouanne 《Microscopy and microanalysis》2006,12(4):331-334
The carbon contents in carburized steels were investigated by electron probe microanalysis (EPMA) for a range of carbon levels in the solid solution less than 1 wt%. This article describes the difficulties encountered with the classic analytical procedure using the k ratio of X-ray intensities and the phi(rhoz) model. Here, a suitable calibration curve method is presented with emphasis on the metallographic study of standard specimens and on the carbon decontamination of samples. 相似文献
2.
A noncoded amino acid of cyclomarin A (1) was synthesized in a racemic fashion. The method employs a six-membered ring template to control the relative stereochemistry and introduction of the functional groups. Ultimately, Pd-catalyzed fragmentation of the lactone provided gamma,delta-unsaturated and delta,epsilon-unsaturated alpha-amino acids. A Pd-catalyzed ring opening of a gamma-lactone is also reported. 相似文献
3.
4.
Madeleine Gasperin 《Journal of solid state chemistry》1985,60(3):316-319
β-Na2UO4 single crystals were synthesized from a melt with U, Nb, and Na ions. They are orthorhombic Fmmm with a = 5.802(2), B = 5.969(2), and c = 11.699(3) Å, and Z = 4. The structure was refined to R = 0.075 and Rw = 0.096 for 603 independent reflexions with I ≥ 3σ(I). The study shows that Na and O atoms are delocalized and that the structure results from the juxtaposition of four P21/b domains. 相似文献
5.
The condensation of ethyl trifluoroacetoacetate with various heterocyclic amines yielded 2-(trifluoromethyl)phenanthrolin-4-ones. The structures of these compounds were established from a study of their infrared and ultraviolet spectra. Substituted phenanthrolines were prepared by nucleophilic attack on a chlorophenanthroline. The oxidation of 5-methoxy-2-trifluoromethyl-1,10-phenanthroline yielded an o-quinone which was treated with typical quinone reagents. A molecular orbital calculation was carried out in an attempt to explain the ease of reduction of the 1,10-phenanthroline system and the colors of the reduced compounds. 相似文献
6.
Madeleine Gasperin 《Journal of solid state chemistry》1984,53(1):144-147
TiNb2O7 is monoclinic with a = 20.351(3), b = 3.801(2), c = 11.882(2) Å, β = 120.19°, Z = 6. The structure, determined by Wadsley in 1961 from visual estimation of intensities, has been refined to R = 0.065 for 915 reflexions with I ≥ 3σI. This study shows that Ti and Nb are not randomly distributed: like several niobo or tantalotitanates with edge-sharing octahedra, this one shows preferential occupation of one type of site by the titanium atoms. 相似文献
7.
Gaunt AJ May I Helliwell M Richardson S 《Journal of the American Chemical Society》2002,124(45):13350-13351
The reaction between PW9O349- and NpO2+ has yielded the first structurally characterized neptunyl(V) polyoxometalate complex, [Na2(NpO2)2(A-PW9O34)2]14-. This complex is isostructural with the uranyl(VI) analogue, and there is also spectroscopic evidence for its existence in solution. The complex is readily extracted into toluene, and this may have significance in the sequestering and/or separation of the neptunyl ion in terms of nuclear waste management. 相似文献
8.
Jiang J Sarsfield MJ Renshaw JC Livens FR Collison D Charnock JM Helliwell M Eccles H 《Inorganic chemistry》2002,41(10):2799-2806
Eight uranyl compounds containing the dicarboxylate ligands iminodiacetate (IDA) or oxydiacetate (ODA) have been characterized in the solid state. The published polymeric structures for [UO(2)(C(4)H(6)NO(4))(2)] and [UO(2)(C(4)H(4)O(5))](n) have been confirmed, while Ba[UO(2)(C(4)H(5)NO(4))(2)] x 3H(2)O, [(CH(3))(2)NH(CH(2))(2)NH(CH(3))(2)][UO(2)(C(4)H(4)O(5))(2)] [orthorhombic space group Pnma, a = 10.996(5) A, b = 21.42(1) A, c = 8.700(3) A, Z = 4], and [C(2)H(5)NH(2)(CH(2))(2)NH(2)C(2)H(5)][UO(2)(C(4)H(4)O(5))(2)] [monoclinic space group P2(1)/n, a = 6.857(3) A, b = 9.209(5) A, c = 16.410(7) A, beta = 91.69(3), Z = 2] contain monomeric anions. The distance from the uranium atom to the central heteroatom (O or N) in the ligand varies. Crystallographic study shows that U-heteroatom (O/N) distances fall into two groups, one 2.6-2.7 A in length and one 3.1-3.2 A, the latter implying no bonding interaction. By contrast, EXAFS analysis of bulk samples suggests that either a long U-heteroatom (O/N) distance (2.9 A) or a range of distances may be present. Three possible structural types, two symmetric and one asymmetric, are identified on the basis of these results and on solid-state (13)C NMR spectroscopy. The two ligands in the complex can be 1,4,7-tridentate, giving five-membered rings, or 1,7-bidentate, to form an eight-membered ring. (C(4)H(12)N(2))[(UO(2))(2)(C(4)H(5)NO(4))(2)(OH)(2)] x 8H(2)O [monoclinic space group P2(1)/a, a = 7.955(9) A, b = 24.050(8) A, c = 8.223(6) A, beta = 112.24(6), Z = 2], (C(2)H(10)N(2))[(UO(2))(2)(C(4)H(5)NO(4))(2)(OH)(2)] x 4H(2)O, and (C(6)H(13)N(4))(2)[(UO(2))(2)(C(4)H(4)O(5))(2)(OH)(2)] x 2H(2)O [monoclinic space group C2/m, a = 19.024(9) A, b = 7.462(4) A, c = 2.467(6) A, beta = 107.75(4), Z = 4] have a dimeric structure with two capping tridentate ligands and two mu(2)-hydroxo bridges, giving edge-sharing pentagonal bipyramids. 相似文献
9.
Cammidge AN Nekelson F Helliwell M Heeney MJ Cook MJ 《Journal of the American Chemical Society》2005,127(47):16382-16383
A mixed condensation of a substituted and unsubstituted silicon phthalocyanine monomer, in which the former serves as a "cap" to a growing oligomeric chain, provides unprecedented access to a mixed dimer, trimers, and a tetramer. An important element of product control can be achieved by changing the ratio of the precursor monomers. 相似文献
10.
Soumen Ghosh Rupa Mukhopadhyay Madeleine Helliwell Alok K. Mukherjee 《Acta Crystallographica. Section C, Structural Chemistry》2007,63(8):o496-o500
The pyrazine ring in two N‐substituted quinoxaline derivatives, namely (E)‐2‐(2‐methoxybenzylidene)‐1,4‐di‐p‐tosyl‐1,2,3,4‐tetrahydroquinoxaline, C30H28N2S2O5, (II), and (E)‐methyl 2‐[(1,4‐di‐p‐tosyl‐1,2,3,4‐tetrahydroquinoxalin‐2‐ylidene)methyl]benzoate, C31H28N2S2O6, (III), assumes a half‐chair conformation and is shielded by the terminal tosyl groups. In the molecular packing of the compounds, intermolecular C—H...O hydrogen bonds between centrosymmetrically related molecules generate dimeric rings, viz. R22(22) in (II) and R22(26) in (III), which are further connected through C—H...π(arene) hydrogen bonds and π–π stacking interactions into novel supramolecular frameworks. 相似文献