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101.
Single crystals of the first anhydrous thallium nickel phosphates were prepared by reaction of heterogeneous Tl/Ni/P alloys with oxygen. TlNi4(PO4)3 (pale‐yellow, orthorhombic, space group Cmc21, a = 6.441(2)Å, b = 16.410(4)Å, c = 9.624(2)Å, Z = 4) crystallizes with a structure closely related to that of NaNi4(PO4)3. Tl4Ni7(PO4)6 (yellow‐brown, monoclinic, space group Cm, a = 10.711(1)Å, b = 14.275(2)Å, c = 6.688(2)Å, β = 103.50(2)°, Z = 8) is isotypic with Na4Ni7(PO4)6, and Tl2Ni4(P2O7)(PO4)2 (brown, monoclinic, space group C2/c, a = 10.389(2)Å, b = 13.888(16)Å, c = 18.198(3)Å, β = 103.1(2)°, Z = 8) adopts the K2Ni4(P2O7)(PO4)2 structure. Tl2Ni4(P2O7)(PO4)2 could also be prepared in nearly single phase form by reaction of Tl2CO3, NiO, and (NH4)2HPO4. 相似文献
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Schumm BA Koetke DS Adolphsen CE Alexander JP Averill D Barish BC Barklow T Barnett BA Blockus D Boyarski A Brabson B Breakstone A Bulos F Burchat PR Burke DL Cence RJ Chapman J Chmeissani M Cords D Coupal DP Dauncey P DeStaebler HC Dorfan JM Drell PS Drewer DC Durrett D Elia R Feldman GJ Field RC Ford WT Fordham C Frey R Fujino D Gan KK Gero E Gidal G Glanzman T Goldhaber G Gomez Cadenas JJ Gratta G Hanson G Harr R Harral B Harris FA Hayes K Hearty C Heusch CA Hildreth MD Himel T Hinshaw DA 《Physical review D: Particles and fields》1992,46(1):453-456
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A series of “push-pull” porphyrins with 4-nitrophenyl and 4-aminophenyl substituents were synthesized and separated by flash column chromatographic techniques. They were fully characterized by elemental analysis, FAB-MS, FTIR, UV-visible, and 1H NMR spectroscopies. The unsymmetrical π-electron distribution of the porphyrins caused by the donor (amino) and acceptor (nitro) substituents were investigated by 1H NMR technique. The pyrrole-H resonance positions can be correlated to the Hammett σ constants of the substituents. Although with strong donor and acceptor substituents, UV-visible spectra show the push-pull porphyrins have rather weak solvatochromism and hence limited intramolecular charge-transfer character. 相似文献
109.
A facile total synthesis of (+)-hernandulcin (1) was accomplished from (−)-isopulegol in 6 steps with 15% overall yield. Epoxidation of (−)-isopulegol with m-chloroperbenzoic acid followed by opening of the epoxide 3a with prenyl Grignard afforded the tertiary alcohol 4a with correct C-6 and C-1′ stereochemistry as a major product. Oxidation of the secondary alcohol in compound 4a to the ketone 5a was accomplished in high yield by using TPAP and N-methylmorpholine N-oxide. Conversion of the ketone 5a to α,β-unsaturated ketone via organoselenium intermediate gave (+)-hernandulcin (1). This method was also successfully applied to the synthesis of (+)-epihernandulcin (2). 相似文献
110.
J. M. Hur S. B. Park C. S. Seo K. J. Jung S. W. Park 《Journal of Radioanalytical and Nuclear Chemistry》2006,270(3):489-493
Summary The electrochemical reduction of uranium oxide in the treatment of spent nuclear fuel requires a characterization of the LiCl-Li2O salt used as a reaction medium. Physical properties, melting and vaporization are important for the application of the salt
and thus they have been investigated by differential scanning calorimetry (DSC) and thermogravimetry (TG), respectively. Experimental
data suggest LiCl and Li2O compound formations, leading to a melting point depression of the LiCl and a co-vaporization of the LiCl-Li2O salt. 相似文献