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Amidometallates of Lanthanum and Gadolinium and the Conversion of Lanthanum, Gadolinium, and Scandium with Ammonia By reaction of the metals with NsNH2 and NH3 in the hightemperature- autoclave Na3[La(NH2)6], Na3[Gd(NH2)6], and Na[Gd(NH2)4] were prepared, but not any compound of Sc. By corresponding experiments with NH4I only La(NH2)3, GdN, and ScH2 were obtained. Na3[La(NH2)6] and Na3[Gd(NH2)6] are isotypic with Na3[Y(KH2)6], Na[Gd(NH2)4] with Na[Yb((NH2)4]. The thermal behaviour of the prepared amides was characterized by DTA and tensimetry.  相似文献   

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A microanalytical method for the determination of carbon and hydrogen is described. The procedure involves the combustion of the organic substance in a stream of nitrogen and the oxidation of the decomposition products with oxygen. Halogens and sulphur are absorbed by the combustion catalyst (according to Körbl), whereas nitrogen oxides are reduced on a copper surface. The combustion products, CO2 and H2O are determined gravimetrically; in the case of radioactive samples they are appropriately absorbed and counted in a liquid scintillation counter. Strongly quenching singly and doubly labelled samples, which cannot be accurately counted even by modification of the counting device, give equally high radioactive yields (75% for 14C, 30% for 3H), since counting is not influenced by other gaseous impurities. Deuterium is quantitatively determined by measuring the intensity of the OD-signal at 2500 cm?1 with an infrared spectrometer.  相似文献   

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Synthesis of N-Methyl- and N,N-Dimethylmerucathine and of N-Methyl- and N,N--Dimethylpseudomerucathine Starting from L -Alanine Starting form L -alanine, N-methylmerucathine (= (3R,4S)-4-(methylamino)1-phenyl-1-penten-3-ol; (3R,4S,)- 6 ), N,N-dimethylmerucathine (= (3R,4S)-4-(dimethylamino)-1-phenyl-1-penten-3-ol; (3R,4S)- 9 ), N-methylpseudomerucathine (= (3S,4S)-4-(methylamino)-1-phenyl-1-penten-3-01; (3S,4S)-6), and N,N-dimethylpseudomerucathine (= (3S,4S)-4-(dimethylamino)-1-phenyl-1-penten-3-ol; (3S,4S)- 9 ) were synthesized. The four compounds were analyzed by HPLC and compared with a natural khat extract.  相似文献   

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Derivatives of Tricyanomethane 1. Synthesis, Characterization, and Decomposition of Chloro- and Bromotricyanomethane The title compounds X? C(CN)3, where X is Cl and Br, are characterized by means of electron absorption, nuclear magnetic resonance, vibrational, and mass spectra. The decompositions of the two compounds in solution have been studied kinetically at 5,0 ± 0,2 °C.  相似文献   

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Preparation, isolation, and characterization of Monoseleane and Disulphane-Diphosphonate The barium salts of monoselenane and monotellurane disulphanediphosphonate are isolated in pure state for the first time. They are characterized by analytical data and i.r. spectra.  相似文献   

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Syntheses and Crystal Structure Analyses of Tetraalkyl Phosphonium, Arsonium, and Stibonium Triiodides The reaction of Me4EI (E?P, As), Me3EtSbI, Me2Et2SbI, MeEt3SbI, or Et4SbI with I2 in absence of solvent gives Me4PI3 (E?P, As), Me3EtSbI3, Me2Et2SbI3, MeEt3SbI3, or Et4SbI3. Me4SbI3 is formed in a reversible reaction by addition of I2 to (Me4Sb)3I8 or by reaction of a solution of Me4SbI in ethanol with I2 in benzene. The crystal structures of Me4EI3 (E?P, Sb), and Me3EtSbI3 and the syntheses of the novel compounds are reported.  相似文献   

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The vanadium, niobium, and tantalum phases have been classified and their isomorphous behaviour has been studied.
  1. It has been found that many vanadium and niobium compounds crystallize with the Cr3Si structure, but just 3 compounds of tantalum have this structure.
  2. The sigma phase occurs in many compounds, and commonly is homogeneous over a wide compositional range.
  3. TheLaves phases mentioned in this work have a radius ratio of 1.66–1.30, which lies in the range mentioned byLaves (1956)23 andDwight (1961)22. One could expect some moreLaves phases in these systems, such as VCo2, VCr2, HfNb2, ZrNb2, HfTa2, TaZn2, and ZrTa2.
  4. The following structure types have more than 10 representatives: Cr3Si, MgZn2, W, sigma, CrSi2, TiAl3, MgCu2, Mn5Si3, CFe3W3, α-Mn, E-NiSiti, AuCu3, AlCu2Mn, W5Si3, Cu16Mg6Si7, and NaCl.
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Synthesis, Vibrational Spectra, and Crystal Structure Analysis of Di- and Trifluoro-tetramethylammonium Salts The tetramethylammonium salts (CH3)3NCH2F+ ( II ), (CH3)3NCHF2+ ( III ), and (CH3)3NCF3+ ( IV ) were prepared by quaternation of the corresponding fluoromethylamines. III was also generated from (CH3)3N and Zn/CF2Br2/KF in acetonitrile. II , III , and IV were characterized by NMR and vibrational spectroscopy, a normal coordinate analysis being undertaken for IV . The crystal structures of the iodides of III and IV have been determined. In both cations the N? CH3 distances are on the average ( III 1.508(2) Å; IV 1.514(5) Å) longer than the N? CF valencies ( III 1.497(4) Å; IV 1.491(6) Å).  相似文献   

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Synthesis and Properties of N,N-Dialkyl-allylaminoboranes and N,N-Dimethylaminopropylborane Complexes of the type H3B ← NR2(CH2CH?CH2) (R?CH3 I , C2H5 II ) are formed by reaction of Li[BH4] with dialkylallylammonium salts. By addition of AlCl3 I can be transformed into the chelate-stabilized N,N-dimethyl-aminopropylborane III . The i.r.-, 1H, 13C-n.m.r. and mass-spectra of I – III are reported and discussed.  相似文献   

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