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1.
The detailed characterization of multifunctional hybrid organosilazane/organosilylamine telechelic oligomers by IR and 1H, 13C and 29Si NMR spectroscopy in one and two dimenions has been undertaken. The specific multifunctional oligomers, comprising NH/NH2 or SiCl functionalities depending on the monomer feed-ratio, were prepared from mono- and di-functionally reacted dichlorodimethylsilane (DDS) and mono-, di-, tri- and tetra-functionally reacted ethylenediamine (EDA). Varying the feed-ratio afforded control of the microstructures of the oligomers and the preparation of oligomers with, in some cases, conterminously located silicon–chlorine (SiCl) groups. The combination of the NMR methods with the IR technique has enabled the detailed microstructural characterization of the oligomers and the identification of the functionalities therein. This approach and the knowledge gained from the DDS/EDA system has been applied to the microstructural characterization of other hybrid organosilazane/silylamine preceramic telechelic oligomers. 相似文献
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Reactions of two preformed trinuclear W/Cu/S clusters, [A](2)[WS(4)(CuCN)(2)] (1: A = Et(4)N; 2: A = PPh(4)), with different concentrations of acetic acid in MeCN generate two interesting 2D polymeric clusters [Et(4)N](3)[(WS(4)Cu(2))(2)(mu-CN)(3)].2MeCN (3), and [PPh(4)][WS(4)Cu(3)(mu-CN)(2)].MeCN (4), respectively. Compound 4 can also be readily obtained in a high yield from the reaction of 2 with equimolar [Cu(MeCN)(4)]PF(6) in MeCN. These compounds have been characterized by elemental analysis, IR spectra, thermal analysis, and single-crystal X-ray diffraction. An X-ray analysis reveals that compound 3 retains the WS(4)Cu(2) cluster core, which serves as a 3-connecting node to link equivalent nodes via single cyanide bridges, forming an anionic 2D (6,3) net. Compound 4 consists of a T-shaped WS(4)Cu(3) core, which also acts as a 3-connecting node, with links to 3 equivalent clusters either through single or double cyanide bridges, affording a different anionic 2D (6,3) network. The acetic acid induced aggregation of 3 and 4 from the two cluster precursors 1 and 2 suggests that this simple synthetic strategy is likely to be applicable to many related systems. 相似文献
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Assembly of a supramolecular cube, [(Cp*WS3Cu3)8 Cl8(CN)12Li4] from a preformed incomplete cubane-like compound [PPh4][Cp*WS3(CuCN)3 总被引:2,自引:0,他引:2
Lang JP Xu QF Chen ZN Abrahams BF 《Journal of the American Chemical Society》2003,125(42):12682-12683
A supramolecular cube has been formed by linking WS3Cu3 clusters with bidentate ligands. Eight WS3Cu3 clusters, which have an incomplete cubane-like structure, serve as the three connecting nodes of the cube, while 12 bridging cyanide anions coordinated to copper centers lie along the edges of the cube. Eight chloride anions and four lithium cations are located inside the cube. 相似文献
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The structure of γ-Li3AsO4 has been refined by Rietveld analysis of high resolution powder neutron diffraction data collected at 770 and 850°C. The structure is related to that of γ-Li3PO4, being a distorted hexagonal close-packed arrangement of oxide ions with half the tetrahedral sites filled by cations. Arsenic occupies the same sites as phosphorus in γ-Li3PO4, Li+ ions show positional disorder; Li(1) ions are split into central and off-center positions within their tetrahedral sites; Li(2) ions are distributed over pairs of face sharing tetrahedral sites at 850°C while occupying only one site at 770°C. The powder neutron data show anisotropic broadening of hkl peaks with h = 2n + 1. The broadening has been accounted for using a modified Rietveld code. The broadened peaks correspond to those reflections that are not common to the related low temperature β-phase and are associated with a doubling of the a-axis during the β-γ transition. The origin of the broadening is the small size of the γ-phase domains in the a -direction; adjacent domains are probably connected by antiphase boundaries. 相似文献
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Cobalt iodate, Co(IO3)2, is pyroelectric at room temperature and crystallizes in the trigonal space group P3 with four formulas in the unit cell. The pyroelectric coefficient p3 = 5.1(5) × 10?5 Cm?2 K?1, and the lattice constants at 298 K are a = 10.9597(1) and c = 5.0774(1)Å. The crystal structure was solved from the Patterson function and a consideration of the structural similarities among the anhydrous 3d-transition metal iodates. Refinement was by the method of least squares using 1825 observed reflections measured with a four-circle diffractometer. The final agreement factor R = 0.050. Two of the three independent octahedrally coordinated cobalt atoms are disordered. The absolute orientation of the polar axis was determined with respect to the crystal morphology. The iodine atoms in the trigonal pyramidal iodate ions point toward the morphologically undeveloped end of the crystals, as does the positive sense of the spontaneous polarization: It is this end that develops a positive polarization on heating. The spontaneous polarization is estimated at about 22 × 10?2 Cm?2. The iodate ion arrangement is very similar to that in α-LiIO3. The anhydrous noncentrosymmetric 3d-iodates may be classified into three isomorphous sets, with space group P63 and corresponding maximal subgroups P3 and P21. All three sets are isostructural with α-LiIO3 except for the cation distribution. The ability of the iodate ion framework to accept a range of cations of different valences is discussed in terms of the tricapped trigonal-prismatic environment about the iodine atoms. 相似文献
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Natasha Willoughby William J. Parnell Andrew L. Hazel I. David Abrahams 《International Journal of Solids and Structures》2012,49(13):1421-1433
In this article a fibre-reinforced composite material is modelled via an approach employing a representative volume element with periodic boundary conditions. The effective elastic moduli of the material are thus derived. In particular, the method of asymptotic homogenization is used where a finite number of fibres are randomly distributed within the representative periodic cell. The study focuses on the efficacy of such an approach in representing a macroscopically random (hence transversely isotropic) material. Of particular importance is the sensitivity of the method to cell shape, and how this choice affects the resulting (configurationally averaged) elastic moduli. The averaging method is shown to yield results that lie within the Hashin–Shtrikman variational bounds for fibre-reinforced media and compares well with the multiple scattering and (classical) self-consistent approximations with a deviation from the latter in the larger volume fraction cases. Results also compare favourably with well-known experimental data from the literature. 相似文献