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71.
In order to achieve a better agreement between the calculated and experimental results of crystal production by the SSD-process, it was essential to extend the application of the modell presented earlier (Weinert et al.). The thermal and geometrical conditions, which vary strongly during the course of the process and influence the GaP crystallisation, have never been taken into consideration. It has been attempted, in the present work, to consider these changes by dividing the total time of crystallisation into so small durations (Δt), that the evaluation model presented earlier for instant times can be successfully applied. The results of crystallisation for the total period can then be obtained through a mathematical analysis named as sequence correction of process parameters. It has been shown that an exact knowledge of the temperature distribution in the furnace will yield results which are in very good agreement with the experimental values. Moreover, the changes in the process parameters during the whole time of crystallisation have been represented graphically. — Application of this model to other systems, for example to GaAs, is also possible. 相似文献
72.
Cycloaddition reactions of distibene [L(Me2N)GaSb]2 (L = HC[C(Me)NDipp]2; Dipp = 2,6-i-Pr2C6H3) with a series of organoazides RN3 (R = Ph, p-CF3Ph, 1-adamantyl (ada)) yielded azadistibiranes [L(Me2N)GaSb]2NR (R = Ph 1, p-CF3Ph 2, ada 3), whereas Me3SiN3 reacted with insertion into one Ga–Sb bond and formation of L(Me2N)GaSbSb(NSiMe3)Ga(NMe2)L (4). Analogous compounds 5 and 6 formed after heating of 1 and 2 above 60 °C. Prolonged heating of 5 resulted in a [2 + 2] cycloaddition accompanied by elimination of LGa(NMe2)2 and formation of tetrastibacyclobutane 7, while the reaction of 5 with a second equivalent of PhN3 gave heteroleptic azadistibirane 9, which isomerized at elevated temperature to distibene 10. Cycloaddition also occurred in reactions of [L(X)GaSb]2 (X = NMe2, OEt, Cl) with Me3Si(H)CN2, yielding distibiranes [L(X)GaSb]2C(H)SiMe3 (X = NMe211, OEt 12, Cl 13). Compounds 1–13 were characterized by IR, UV-Vis and NMR spectroscopy and sc-XRD. The mechanism of the reaction of [L(Me2N)GaSb]2 with PhN3 and Me3SiN3 and the electronic nature of the resulting compounds were studied by DFT calculations.Azadistibiranes and distibiranes formed in cycloaddition reactions of distibene [L(Me2N)GaSb]2 with RN3 and Me3Si(H)CN2. The mechanism of the reactions with PhN3 and Me3SiN3 and the electronic nature of the products were studied by DFT calculations. 相似文献
73.
Monika L. Amadoruge Curtis Moore Charles S. Weinert 《Journal of organometallic chemistry》2010,695(14):1813-3726
The synthesis of four new oligogermanes containing para-tolyl-substituents has been achieved via the hydrogermolysis reaction, including the digermane Tol3GeGePh3, the trigermanes Tol3GeGePh2GeTol3 and Tol3GeGeTol2GeTol3, and the tetragermane Tol3GeGePh2GePh2GeTol3 (Tol = p-CH3C6H4). These four oligogermanes have been structurally characterized and their structures have been compared with those of their per-phenyl-substituted analogs. The digermane Tol3GeGePh3 exhibits an unusually short Ge-Ge bond distance of 2.408(1) Å. The four para-tolyl-substituted oligogermanes have also been characterized by UV/visible spectroscopy and cyclic voltammetry. The expected red shift in the absorbance maximum with increasing catenation was observed for this series of compounds. Their cyclic voltammograms each contain n − 1 irreversible oxidation waves (n = the number of Ge atoms), which is atypical since oligogermanes generally exhibit only one irreversible oxidation wave regardless of the degree of catenation. 相似文献
74.
Inside Cover: Regulating Molecular Recognition with C‐Shaped Strips Attained by Chirality‐Assisted Synthesis (Angew. Chem. Int. Ed. 43/2015) 下载免费PDF全文
75.
Motivated by work of Erd?s, Milner and Rado, we investigate symmetric and asymmetric partition relations for linear orders without the axiom of choice. The relations state the existence of a subset in one of finitely many given order types that is homogeneous for a given colouring of the finite subsets of a fixed size of a linear order. We mainly study the linear orders 〈 α 2,< l e x 〉, where α is an infinite ordinal and < l e x is the lexicographical order. We first obtain the consistency of several partition relations that are incompatible with the axiom of choice. For instance we derive partition relations for 〈 ω 2,< l e x 〉 from the property of Baire for all subsets of ω 2 and show that the relation \(\langle ^{\kappa }{2}, <_{lex}\rangle \longrightarrow (\langle ^{\kappa }{2}, <_{lex}\rangle )^{2}_{2}\) is consistent for uncountable regular cardinals κ with κ <κ = κ. We then prove a series of negative partition relations with finite exponents for the linear orders 〈 α 2,< l e x 〉. We combine the positive and negative results to completely classify which of the partition relations \(\langle ^{\omega }{2}, <_{lex}\rangle \longrightarrow (\bigvee _{\nu <\lambda }K_{\nu },\bigvee _{\nu <\mu }M_{\nu })^{m}\) for linear orders K ν ,M ν and m≤4 and 〈 ω 2,< l e x 〉→(K,M) n for linear orders K,M and natural numbers n are consistent. 相似文献
76.
Christian R. Samanamu Charles S. Weinert 《Journal of organometallic chemistry》2011,696(23):3721-3726
The formation of 3-aminocrotononitrile and 4-amino-2,6-dimethylaminopyrimidine has been observed during the course of the hydrogermolysis reaction between a germanium amide and a germanium hydride, either as the free amines or bound to germanium as ligands consisting of their conjugate bases. These species arise from the dimerization or trimerization of acetonitrile, and have only been detected when germanium amides having substantial steric bulk at the germanium center are employed in the reaction. The isolation of germanium-bound 3-aminocrotononitrile compounds suggests that α-germyl nitrile species R3GeCH2CN that result from the reaction of the germanium amides R3GeNMe2 with CH3CN solvent also can further react with CH3CN to generate the 3-aminocrotononitrile and 4-amido-2,6-dimethylaminopyrimidine species. The two germanes Ph3Ge[NHC(CH3)CHCN] and 2,6-dimethyl-4-(triphenylgermylamino)pyrimidine have been prepared and structurally characterized, and the conversion of Ph3GeCH2CN to Ph3Ge[NHC(CH3)CHCN] and 2,6-dimethylamino-4-(triphenylgermylamino)pyrimidine as well as the conversion of Ph3Ge[NHC(CH3)CHCN] to 2,6-dimethyl-4-(triphenylgermylamino)pyrimidine in acetonitrile solvent has been observed using 1H NMR spectroscopy. 相似文献
77.
Patrícia Los Weinert Jo?o Roberto Fernandes Leonardo Pezza Helena Redigolo Pezza 《Analytical sciences》2007,23(12):1383-1389
A sensitive flow-injection (FI) procedure with spectrophotometric detection in a micellar medium is proposed for the determination of novalgin. The method is based on the instantaneous formation of a red-orange product (lambda(max) = 510 nm) after the reaction between novalgin and p-dimethylaminocinnamaldehyde (p-DAC) in a dilute acid medium. The sensitivity of this reaction was increased by a factor of 5.6 in the presence of sodium dodecyl sulfate (SDS). Experimental design methodologies were used to optimize the chemical and FI variables. The calibration curve was linear in the range of 1.45 x 10(-6) to 2.90 x 10(-5) mol L(-1) with an excellent correlation coefficient (r = 0.9999). The detection limit was 1.31 x 10(-7) mol L(-1) (n = 20, RSD = 2.0%). No interferences were observed from the common excipients. The results obtained by the proposed method were favorably compared with those given by the iodometric reference method at 95% confidence level. 相似文献
78.
Dedkov YS Laubschat C Khmelevskyi S Redinger J Mohn P Weinert M 《Physical review letters》2007,99(4):047204
Here we report on results of a spin-resolved photoelectron spectroscopic (SRPES) study of YCo2 thin films (150 A-thick) grown on a W(110) substrate. The films were prepared by co-deposition of stoichiometric amounts of Y and Co onto a clean W surface followed by thermal annealing leading to (2x2) overstructure with respect to W(110) in the low-energy electron diffraction pattern indicated formation of a structurally ordered YCo2(111) surface. While no clear spin asymmetry was observed for bulk-sensitive SRPES data taken at hnu=1253.6 eV, the more surface-sensitive SRPES data obtained at hnu=21.2 eV photon energy revealed a clear spin-asymmetry probing the validity of the recent theoretical prediction. 相似文献
79.
Formation of [Bi11]3−, A Homoatomic,Polycyclic Bismuth Polyanion,by Pyridine‐Assisted Decomposition of [GaBi3]2− 下载免费PDF全文
Dipl.‐Chem. Bastian Weinert Armin Rainer Eulenstein Dr. Rodica Ababei Prof. Dr. Stefanie Dehnen 《Angewandte Chemie (International ed. in English)》2014,53(18):4704-4708
Until now, polycyclic bismuth polyanions have not been known—thus discriminating bismuth from its lighter congeners. However, the synthesis of [K([2.2.2]crypt)]3(Bi11)?2 py?tol, allows us to present the first structurally characterized homoatomic, polycyclic bismuth polyanion, which exhibits the [P11]3? “ufosan” structure. It was obtained upon treatment of [K([2.2.2]crypt)]2(GaBi3)?en with the solvent pyridine. The binary Zintl anion [GaBi3]2? decomposes under oxidative coupling of pyridine molecules and release of H2 to form the title compound. The unprecedented reaction, its products and by‐products were investigated by means of spectroscopy, spectrometry, and DFT studies. All findings reveal the specific reaction conditions to be crucial for the formation of the [Bi11]3? ion—and indicate the possibility of the generation and isolation of further, large bismuth polyanions. 相似文献
80.
Marcelo Lazzarotto Patrícia Los Weinert Márcio Lazzarotto 《Journal of inclusion phenomena and macrocyclic chemistry》2014,80(3-4):313-322
The Gibbs energy of extraction experiments of ionophoric calixarenes with alkali metals from the literature have been correlated with electronic parameters of their “monomeric” structures calculated by AM1, PM3 and PM7 algorithms: energies of molecular orbitals and charge densities of oxygen and nitrogen atoms. We observed general correlations of the extraction constants with the charge on the carbonyl oxygen and specific correlations with MO-energy using the covalent term of the Klopman–Salem equation. The correlations for calixarenes with 5 and 6 phenolic units were very poor, and we attributed to the structural flexibility, which allow different optimized conformations for metal binding. 相似文献