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21.
Zinc K-edge X-ray absorption fine structure (XAFS) experiments were performed in the solid and solution states at low temperature (10 K), on dimeric and monomeric anti-inflammatory Zn(II) complexes of indomethacin [1-(4-chlorobenzoyl)-5-methoxy-2-methyl-1H-indole-3-acetic acid=IndoH] of the formula [Zn2(Indo)4L2] [L=pyridine (Py), N,N-dimethylacetamide (DMA)], [Zn(Indo)2L2] [L=ethanol (EtOH), methanol (MeOH)], and Zn(II) acetate dihydrate [Zn(OAc)2(OH2)2]. The bond distances and angles obtained from multiple-scattering fits to the XAFS data of the Zn(II) dimeric complexes in the solid and solution states exhibit excellent correspondence with those obtained from single crystal diffraction studies. The Zn...Zn separations of 2.97 and 2.96 A and carboxylate group O-C-O angles of 125 degrees for powdered [Zn2(Indo)4(Py)2] and [Zn2(Indo)4(DMA)2] agree well with the XRD values of 2.969(1) and 2.9686(6) A and 125.8(4) degrees and 126.1(2) degrees, respectively. The calculated Zn-O(RCOO) and Zn-L bond distances of 2.03 and 2.04 A, or 2.02 and 1.98 A for Py or DMA complexes, respectively, also agree well with crystallographic data. The X-ray powder diffraction data on samples of the monomers exhibited additional reflections apart from those due to the crystallographically characterized cis-[Zn(eta2-O,O'-Indo)2L2], but microanalyses were consistent with this formulation. Therefore, mixed models that contained the cis complex and a second component consisting of a trans-six-coordinate complex, a five-coordinate complex, or a four-coordinate complex were used to model the XAFS. The best fits to the XAFS data were obtained with a mixture of the cis-six-coordinate complex and a four-coordinate complex containing two monodentate Indo ligands. The bond lengths for the six-coordinate structure were consistent with those determined on a single crystal, and those for the four-coordinate complexes were consistent with related four-coordinate structures with two monodentate carboxylate ligands. Dissolution of the dimer (DMA adduct) in DMF resulted in a mixture of dimer and monomer species as shown by MS XAFS fitting. This is the first time that solution structures have been determined for anti-inflammatory Zn(II) complexes, and this is an important first step in understanding the pharmacology of the complexes. 相似文献
22.
We make a conjecture that the number of isolated local minimum points of a 2n-degree or (2n+1)-degree r-variable polynomial is not greater than n
r when n 2. We show that this conjecture is the minimal estimate, and is true in several cases. In particular, we show that a cubic polynomial of r variables may have at most one local minimum point though it may have 2r critical points. We then study the global minimization problem of an even-degree multivariate polynomial whose leading order coefficient tensor is positive definite. We call such a multivariate polynomial a normal multivariate polynomial. By giving a one-variable polynomial majored below a normal multivariate polynomial, we show the existence of a global minimum of a normal multivariate polynomial, and give an upper bound of the norm of the global minimum and a lower bound of the global minimization value. We show that the quartic multivariate polynomial arising from broad-band antenna array signal processing, is a normal polynomial, and give a computable upper bound of the norm of the global minimum and a computable lower bound of the global minimization value of this normal quartic multivariate polynomial. We give some sufficient and necessary conditions for an even order tensor to be positive definite. Several challenging questions remain open. 相似文献
23.
V. A. Makara L. P. Steblenko V. V. Obukhovskii N. Ya. Gorid’ko V. V. Lemeshko 《Physics of the Solid State》2000,42(5):877-881
It is shown that the passage of an electric current through crystalline silicon may lead to the so-called galvanoplasticization, as well as the galvanostrengthening, effect. It is found that the effect is sensitive to the temperature regime of deforming and to the preliminary high-temperature treatment of the samples. The motion delay time for short dislocations and starting stresses are significantly affected by the current. The relation of these effects to the change in the electric state of the Cottrell atmosphere as a result of the passage of the current through the crystal is considered. 相似文献
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25.
A 'living' controlled hydrogel formation method was first reported to create loose and compact in situ biodegradable hydrogels. The method executed under mild reaction conditions can conveniently tailor the hydrogel properties, and it has the potential to develop into a powerful tool for the design, synthesis, and self-assembly of novel tailor-made biomaterials and drug delivery systems. 相似文献
26.
Leonardo Manzoni Luigi Lay Richard R. Schmidt 《Journal of carbohydrate chemistry》2013,32(4-5):739-758
Abstract Thexyldimethylsilyl 4,6-O-benzylidene-2-deoxy-2-trichloroethoxycarbonylamino-β-D- glucopyranoside (4), having the 3-hydroxy group unprotected, is a versatile starting material for the synthesis of glucosamine containing oligosaccharides. Thus, reaction with galactosyl donor 5 or fucosyl donor 6 afforded the desired β(1-3)- and α(1-3)-linked disaccharides 7 and 8, respectively, in high yields. Reductive opening of the benzylidene moieties in 7 and 8 gave access to the 4-hydroxy groups in 9 and 10. Ensuing fucosylation of 9 or galactosylation of 10 led to Lewis A (Lea) and Lewis X (Lex) trisaccharide building blocks 13 and 14, respectively. Their transformation into glycosyl donors 19 and 20 and subsequent reaction with 3b-O-unprotected lactose derivative 23 as acceptor furnished the Lea? and Lex pentasaccharide precursors 24 and 25. Exchange of the N-trichloroethoxycarbonyl group for an N-acetyl group and removal of the O-benzyl and O-acetyl protective groups afforded the desired Lea? and Lex? pentasaccharides 1 and 2. 相似文献
27.
R. F. Kiefl J. H. Brewer I. Affleck J. F. Carolan P. Dosanjh W. N. Hardy T. Hsu R. Kadono J. R. Kempton S. R. Kreitzman Q. Li A. H. O'Reilly T. M. Riseman P. Schleger P. C. E. Stamp H. Zhou L. P. Le G. M. Luke B. Sternlieb Y. J. Uemura H. R. Hart K. W. Lay 《Hyperfine Interactions》1991,63(1-4):139-144
We have searched for anomalous internal magnetic fields in highT
c materials which are predicted to occur in anyon and flux phase models of superconductivity. The magnitude, anisotropy and
temperature dependence of the observed fields inc-axis oriented samples of sintered YBa2CuO3O7 and of thick-film Bi2Sr2CaCu2O8 are consistent with a conventional nuclear dipolar origin. An upper limit of ≲0.08 mT is set for any anomalous magnetic fields
along thec-axis atμ
+ sites in bulk CuO2 superconductors. 相似文献
28.
The effect of x-ray scattering by neutron-irradiated and reference (unirradiated) silicon crystals grown by the Czochralski method and annealed at temperatures of 850–1050°C on the defect formation is comparatively investigated using triple-crystal x-ray diffractometry. The sizes and concentrations of clusters composed of point defects and dislocation loops formed during decomposition of an oxygen-containing solid solution and subsequent clusterization of the point defects are calculated. 相似文献
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