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1.
G.R. Clark T.J. Collins K. Marsden W.R. Roper 《Journal of organometallic chemistry》1983,259(2):215-232
Reaction of HgR2 with OsHCl(CS)(PPh3)3 yields red, five-coordinate, OsRCl-(CS)(PPh3)2 (R = p-tolyl). From this have been derived the compounds OsRX(CS)(PPh3)2 with X = Br, I, S2CNEt2, O2CMe, O2CCF3. These compounds add an additional ligand, MeCN, CO or CNR to form colourless, six coordinate arylthiocarbonyl complexes, which undergo migratory-insertion reactions to form red, dihapto-thioacyl complexes. The crystal structure of a representative example, Os(η2-CSR)(η1-O2CCF3)(CO)PPh3)2 has been determined. The red equant crystals are orthorhombic, space group P212121, a 11.584(1), b 19.184(2), c 18.90(1) Å, V 4199 Å3, Z 4. The structure was solved by conventional heavy-atom methods and refined by full-matrix least-squares employing anisotropic thermal parameters for all non-hydrogen atoms except the carbon atoms of the triphenylphosphines. The final R factor is 0.057 for 2868 observed reflections.The coordination geometry in the monomeric complex is that of an octahedron distorted by the constraints of the ligands. The triphenyl phosphine ligands are mutually trans; the equatorial plane contains carbonyl, monohapto-trifluoroacetate, and dihapto-thioacyl ligands. Bond distances and angles are OsP 2.405, 2.407(4) Å; POsP 173.9(1)°; OsCO 1.83(2) Å; Os-O (trifluoroacetate) 2.206(11) Å; OsC (thioacyl) 1.91(2); OsS 2.513(6); CS 1.72 Å. The CS bond length implies a reduction in bond order from 2.0 to approx. 1.5 upon coordination to the metal.The η2-thioacyl ligand in Os(η2-CSR)Cl(CNR)(PPh3)2 is methylated with methyl triflate and further reaction with LiCl produces the thiocarbene complex OsCl2(C[SMe]R)(CNR)(PPh3)2. 相似文献
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Talanova GG Roper ED Buie NM Gorbunova MG Bartsch RA Talanov VS 《Chemical communications (Cambridge, England)》2005,(45):5673-5675
A new fluorogenic, dansyl group-containing derivative of 1,3-alternate calix[4]arene-bis(crown-6-ether) provides optical recognition of Tl+ with selectivity over many other metal cations, including Na+, K+, Ca2+, Ag+, Hg2+ and Pb2+, and embodies the first example of a calixarene-based fluorescent Tl+-chemosensor. 相似文献
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E. E. Roper W. P. White H. P. Brown O. A. Sliskonskaja F. Lieneweg I. Schrodt M. Benedict und P. Neubert 《Fresenius' Journal of Analytical Chemistry》1940,120(1-2):17-18
Ohne Zusammenfassung 相似文献
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J. Somlai B. Kanyár R. Bodnár CS. Németh Z. Lendvai 《Journal of Radioanalytical and Nuclear Chemistry》1996,207(2):437-443
A significant dose contribution on the population could be derived from coal slags used as isolation material. Extremely high natural activities are measured in the coal slag, derived from the region of the settlement Ajka, Hungary. In some buildings monitored, the elevated -doses were nearly 5–10 times higher than the world average ones. The annual average indoor radon concentrations from the slag exceeded 400 Bq/m3 and in some cases up to 1200 Bq/m3. Due to the elevated exposure and the radon concentrations in the dwellings the annual dose was estimated to 8–24 mSv/y more than 5–10 times of the world average one. 相似文献
8.
Donglin He Chengxi Zhao Dr. Linjiang Chen Dr. Marc A. Little Dr. Samantha Y. Chong Rob Clowes Katherine McKie Mark G. Roper Graeme M. Day Dr. Ming Liu Prof. Andrew I. Cooper 《Chemistry (Weinheim an der Bergstrasse, Germany)》2021,27(41):10589-10594
Ethyl acetate is an important chemical raw material and solvent. It is also a key volatile organic compound in the brewing industry and a marker for lung cancer. Materials that are highly selective toward ethyl acetate are needed for its separation and detection. Here, we report a trianglimine macrocycle ( TAMC ) that selectively adsorbs ethyl acetate by forming a solvate. Crystal structure prediction showed this to be the lowest energy solvate structure available. This solvate leaves a metastable, “templated” cavity after solvent removal. Adsorption and breakthrough experiments confirmed that TAMC has adequate adsorption kinetics to separate ethyl acetate from azeotropic mixtures with ethanol, which is a challenging and energy-intensive industrial separation. 相似文献
9.
Zaharescu M. Jitianu A. Brăileanu A. Madarász J. Novák CS. Pokol G. 《Journal of Thermal Analysis and Calorimetry》2003,71(2):421-428
Hybrid materials with different amounts of organics permanently bound on the inorganic network obtained in the TEOS-MTEOS
(tetraethoxysilan-methyltriethoxysilan) system are used for obtaining coatings with different optical and mechanical properties.
To study the thermal stability of the mentioned materials, compositions with different molar ratios of the precursors were
prepared. The influence of the solvent and water amounts on the gelation process was also investigated. The gels obtained
were characterised by IR spectrometry and their decomposition temperatures were determined by DTA/TG. Thermal stability of
the gels is rather influenced by their composition than the conditions of the gelation process.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
10.
Yue GE Roper MG Balchunas C Pulsipher A Coon JJ Shabanowitz J Hunt DF Landers JP Ferrance JP 《Analytica chimica acta》2006,564(1):116-122
This work describes an integrated glass microdevice for proteomics, which directly couples proteolysis with affinity selection. Initial results with standard phosphopeptide fragments from β-casein in peptide mixtures showed selective capture of the phosphorylated fragments using immobilized metal affinity chromatography (IMAC) beads packed into a microchannel. Complete selectivity was seen with angiotensin, with capture of only the phosphorylated form. On-chip proteolysis, using immobilized trypsin beads packed into a separate channel, was directly coupled to the phosphopeptide capture and the integrated devices evaluated using β-casein. Captured and eluted fragments were analyzed using both capillary electrophoresis (CE) and capillary liquid chromatography/mass spectrometry (cLC/MS). The results show selective capture of only phosphopeptide fragments, but incomplete digestion of the protein was apparent from multiple peaks in the CE separations. The MS analysis indicated a capture bias on the IMAC column for the tetraphosphorylated peptide fragment over the monophosphorylated fragment. Application to digestion and capture of a serum fraction showed capture of material; however, non-specific binding was evident. Additional work will be required to fully optimize this system, but this work represents a novel sample preparation method, incorporating protein digestion on-line with affinity capture for proteomic applications. 相似文献