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441.
de Sousa GF Deflon VM Gambardella MT Francisco RH Ardisson JD Niquet E 《Inorganic chemistry》2006,45(11):4518-4525
The synthesis and the IR, NMR (1H, 13C, and 119Sn), and M?ssbauer spectroscopies and single-crystal X-ray diffraction studies of seven-coordinated diorganotin(IV) complexes, namely, [Ph2Sn(Hdapsc)]Cl.H2O.DMF [7; H(2)dapsc = 2,6-diacetylpyridine bis(semicarbazone)], [Me(2)Sn(H2,6Achexim)]Br.H2O [8; H(2)2,6Achexim = 2,6-diacetylpyridine bis(3-hexamethyleneiminylthiosemicarbazone)], [Me(2)Sn(dapmts)] [9; H(2)dapmts = 2,6-diacetylpyridine bis(4-methythiosemicarbazone)], and [nBu2Sn(dapmdtc)] [10; H(2)dapmdtc = 2,6-diacetylpyridine bis(S-methydithiocarbazate)], were done. The determination of the structures of [Ph(2)Sn(Hdapsc)]+, [Me2Sn(H2,6Achexim)]+ and [Me2Sn(dapmts)], [nBu2Sn(dapmdtc)] revealed the presence of monocationic and neutral complexes, respectively. The structures consist of monomeric units in which the Sn(IV) ions exhibit distorted pentagonal-bipyramidal geometries, with the X,N,N,N,X-donor (X = O, S) systems of the ligands lying in the equatorial plane and the organic groups in the apical positions. The C-Sn-C angle in the seven-coordinated diorganotin(IV) complexes was estimated using a correlation between M?ssbauer and X-ray data based on the point-charge model and using new values obtained in this work for [alkyl] = -1.00 mm s(-1) and [aryl] = -0.80 mm s(-1) for complexes containing O,N,N,N,O-pentadentate ligands and new values for [alkyl] = -0.87 mm s(-1) and [aryl] = -0.75 mm s(-1) for complexes containing S,N,N,N,S-pentadentate ligands. 相似文献
442.
443.
Wenzl T Karasek L Rosen J Hellenaes KE Crews C Castle L Anklam E 《Journal of chromatography. A》2006,1132(1-2):211-218
A European inter-laboratory study was conducted to validate two analytical procedures for the determination of acrylamide in bakery ware (crispbreads, biscuits) and potato products (chips), within a concentration range from about 20 microg/kg to about 9000 microgg/kg. The methods are based on gas chromatography-mass spectrometry (GC-MS) of the derivatised analyte and on high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) of native acrylamide. Isotope dilution with isotopically labelled acrylamide was an integral part of both methods. The study was evaluated according to internationally accepted guidelines. The performance of the HPLC-MS/MS method was found to be superior to that of the GC-MS method and to be fit-for-the-purpose. 相似文献
444.
An existing method was adapted to the purpose and validated in-house according to the IUPAC harmonised guideline for the determination of 15 EU priority polycyclic aromatic hydrocarbons (PAHs) in primary smoke condensates (PSCs) that are used to produce smoke flavourings for human consumption. Limits of detection (LOD) varied between 0.1 and 1.3 microg/kg, limits of quantitation (LOQ) between 0.5 and 4 microg/kg for the various PAHs in PSCs. The coefficient of variance of the repeatability was between 0.7% (benzo[a]pyrene) and 30% (dibenzo[a,h]pyrene) relative standard deviation, depending on the analyte. The recoveries varied between 100 and 102% (dibenzo[a,l]pyrene) and 69-83% (dibenzo[a,h]pyrene) over the analytical range of 5-35 microg/kg. 相似文献
445.
Czerwonka R Reddy KR Baum E Knölker HJ 《Chemical communications (Cambridge, England)》2006,(7):711-713
The first enantioselective total synthesis of neocarazostatin B, the determination of its absolute configuration and transformation into carquinostatin A are described. 相似文献
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447.
Wolfgang Jeitschko Joerg H. Albering Reinhold Brink Ursula Jakubowski‐Ripke Elke J. Reinbold 《ChemInform》2015,46(1):no-no
The new ternary phosphides ScFe5P3 (I), Sc(Ta0.18Fe0.82)Fe4P3 (II), ZrFe5P3 (III), ScRu6P4 (IV), ErRu6P4 (V), ZrCr6P4 (VI), Nd2Ru12P7 (VII), and U2Mo30P19 (VIII) are prepared from mixtures of the elements in most cases with elemental Sn as a flux (alumina crucibles, 650—950 °C, 7—10 d). 相似文献
448.
449.
450.
Jan H. Overbeck Jennifer Vögele Felix Nussbaumer Elke Duchardt-Ferner Christoph Kreutz Jens Wöhnert Remco Sprangers 《Angewandte Chemie (International ed. in English)》2023,62(23):e202218064
The synthetic neomycin-sensing riboswitch interacts with its cognate ligand neomycin as well as with the related antibiotics ribostamycin and paromomycin. Binding of these aminoglycosides induces a very similar ground state structure in the RNA, however, only neomycin can efficiently repress translation initiation. The molecular origin of these differences has been traced back to differences in the dynamics of the ligand:riboswitch complexes. Here, we combine five complementary fluorine based NMR methods to accurately quantify seconds to microseconds dynamics in the three riboswitch complexes. Our data reveal complex exchange processes with up to four structurally different states. We interpret our findings in a model that shows an interplay between different chemical groups in the antibiotics and specific bases in the riboswitch. More generally, our data underscore the potential of 19F NMR methods to characterize complex exchange processes with multiple excited states. 相似文献