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Wisian-Neilson P Johnson RS Zhang H Jung JH Neilson RH Ji J Watson WH Krawiec M 《Inorganic chemistry》2002,41(18):4775-4779
The reactions of Me(3)SiN=P(OR")RR'(R" = Ph, CH(2)CF(3); R, R' = Me, Ph) with alcohols were investigated. With nonequivalent amounts of CF(3)CH(2)OH, the reactions produced high yields of the cyclic phosphazene (Me(2)PN)(3) and both the cis and trans isomers of nongeminally substituted [(Ph)(Me)PN](3). The isomers of this new cyclic phosphazene were separated by column chromatography and characterized by NMR and IR spectroscopy, elemental analysis, and X-ray crystallography. Crystals of the cis isomer 6a have a monoclinic crystal system, while the trans isomer 6b has a triclinic crystal system with two different molecules in an asymmetric unit. The bond lengths and bond angles are very similar to those of the simpler cyclic trimers (Me(2)PN)(3) and (Ph(2)PN)(3.) A likely pathway for the formation of these compounds is discussed. 相似文献
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Hardy JC Iacob VE Sanchez-Vega M Neilson RG Azhari A Gagliardi CA Mayes VE Tang X Trache L Tribble RE 《Physical review letters》2003,91(8):082501
The half-life, 3.8755(12) s, and superallowed branching ratio, 0.5315(12), for 22Mg beta decay have been measured with high precision. The latter depended on gamma-ray intensities being measured with an HPGe detector calibrated for relative efficiencies to an unprecedented 0.15%. Previous precise measurements of 0+ --> 0+ transitions have been restricted to the nine that populate stable daughter nuclei. No more such cases exist, and any improvement in a critical Cabibbo-Kobayashi-Maskawa unitarity test must depend on precise measurements of more exotic nuclei. With this branching-ratio measurement, we show those to be possible for T(z)=-1 parents. We obtain a corrected Ft value of 3071(9) s, in good agreement with expectations. 相似文献
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Increased interest in potential health-protective activities of flavonoid-rich tea has created the need to take advantage of HPLC column and system advances in order to optimize methodologies for flavonoid analysis. Two new RP-C18 methods for HPLC-DAD analysis of tea flavonoids were developed to facilitate separation of catechins within 5 min and separation of catechins and theaflavins within 10 min total analysis time. Calibration results indicate that these methods have on-column limits of detection on the order of 1-10 pmol for most tea catechins, and method replication generally resulted in intraday and interday peak area variation of <5% for catechins and <9% for theaflavins in green and black tea infusions. These new methods are therefore sensitive, reproducible, and represent a 2-4-fold reduction in HPLC analysis time from existing analytical methods. These improvements are readily achievable with commonly used HPLC equipment, thus facilitating increased sample throughput and efficiency across a broad range of experimental applications. 相似文献
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Bin Wang John R. Klaehn Robert H. Neilson 《Phosphorus, sulfur, and silicon and the related elements》2013,188(4-5):821-825
Silicon-nitrogen-phosphorus compounds of the type Me 3 SiN═PR(R′)X(X= Cl, Br, OCH2CF 3 , OPh), known as N-silylphosphoranimines,are useful precursors to both cyclic and polymeric phosphazenes.Depending on the leaving group (X), thermolysis reactions afford either cyclic trimers, [N═PR(R′)] 3 (when X = Cl, Br), or linear polymers,[N═PR(R′)]n (when X = OCH 2 CF 3 or OPh). Treatment of the P-trifluoroethoxy and P-phenoxy derivatives, Me 3 SiN═PR(R′)X (X = OCH 2 CF 3 , OPh), with alcohols at lower temperature usually results in the formation of cyclic phosphazene trimers via silyl ether elimination. Recently, we have applied these synthetic methods to the preparation of some new phosphazene systems including a series of 4-aryl-functionalized trimers and polymers and a variety of non-geminal, mixed-substituent cyclic trimers. Representative examples of the synthesis, structural characterization, and reactivity of these new phosphazenes and their Si─N─P precursors are reported here. 相似文献
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Classical crystallization calculations were performed to determine the possibility of forming a particular type of laser glass with the avoidance of devitrification in an outer space laboratory. Although the laser glass in question readily crystallizes in an earth environment, it is demonstrated that under the homogeneous nucleating conditions obtainable in a zero gravity laboratory this laser glass may be easily quenched to a virtually crystal-free product. Use of this material as a host in a neodymium glass laser would result in a more than 10% increase in efficiency when compared to laser glass rods of similar composition currently commercially available. 相似文献
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The GRANIT system operates by applying an impulse of known force by means of an impact device that is attached to the tendon of the anchorage. The vibration response signals resulting from this impulse are complex in nature and require analysis to be undertaken in order to extract information from the vibrational response signatures that is relevant to the condition of the anchorage. In the system, the complicated relationship that exists between characteristics of an anchorage and its response to an impulse is identified and learned by a novel artificial intelligence network based on artificial intelligence techniques.The results presented in this paper demonstrate the potential of the GRANIT system to diagnose the integrity of ground anchorages at a site near Stone, England, by using a trained neural network capable of diagnosing the post-tension level of the anchorage. This neural network was used for the diagnosis of load in a second ground anchorage adjacent to the original anchorage used for the training of the neural network. Further tests were taken with a different anchor head configuration of the anchorage and a different relationship between the signature response of the anchorage to an applied impulse and its post-tension level was found.Problems encountered during the diagnosis of this second set of test signatures by the trained neural network are investigated with the use of a lumped parameter dynamic model. This model is able to identify the parameters in the anchorage system that affect this change in response signature. The results from the investigation lead to a new form of classification for the installed anchorages, based on their anchor head configuration.Laboratory strand anchorage tests were undertaken in order to compare with and validate the results obtained from the field tests and the lumped parameter dynamic model. 相似文献
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Electron paramagnetic resonance spectra of homoleptic and mixed-ligand molybdenum tris(dithiolene) complex anions [Mo(tfd)(m)(bdt)(n)](-) (n + m = 3; bdt = S(2)C(6)H(4); tfd = S(2)C(2)(CF(3))(2)) reveal that the spin density has mixed metal-ligand character with more ligand-based spin for [Mo(tfd)(3)](-) and a higher degree of metal-based spin for [Mo(bdt)(3)](-): the magnitude of the isotropic (95,97)Mo hyperfine interaction increases continuously, by a factor of 2.5, on going from the former to the latter. The mixed complexes fall in between, and the metal character of the spin increases with the bdt content. The experiments were corroborated by density functional theory computations, which reproduce this steady increase in metal-based character. 相似文献