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951.
X. F. Wang Y. F. Wang J. Wang Zh. H. Zhang J. Gao B. Liu Y. Ch. Jiang X. D. Zhang 《Russian Journal of Coordination Chemistry》2008,34(8):555-563
The title complexes, K3[Cd(Dtpa)] (H5Dtpa = diethylenetriamine-N,N,N,N′,N′-pentaacetic acid, (I)), K2[Cd(H2O)4][Cd(Edta)(H2O)]2 · 2H2O (H4Edta = ethylenediamine-N,N,N′,N′-tetraacetic acid, (II)), and Na2[Cd(H2O)4][Cd(Edta)(H2O)]2 · 2H2O (III), were prepared, and their compositions and structures were determined by elemental analyses, IR spectra, and single-crystal X-ray diffraction techniques, respectively. In complex I, the Cd is seven-coordinated by one Dtpa ligand yielding a pseudo-monocapped trigonal prism conformation, and the complex crystallizes in the triclinic crystal system with the Pi space group. The crystal data are as follows: a = 8.7300(17), b = 9.1200(18), c = 15.110(3) Å, α = 95.52(3)°, β = 96.59(3)°, γ = 99.63(3)°, V = 1170.0(4) Å3, Z = 2, ρ = 1.754 g/cm3, μ = 1.519 mm?1, F(000) = 616, R = 0.0644 and wR = 0.1712 for 3842 observed reflections with I ≥ 2σ(I). For complex II, in the [Cd(Edta)(H2O)]2? complex anion the Cd2+ ion is seven-coordinated by one Edta ligand and one water molecule, yielding a pseudo-pentagonal bipyramid conformation. In the [Cd(H2O)4]2+ cation, the bridged Cd is six-coordinated, yielding an almost standard octahedral conformation. The complex crystallizes in the monoclinic system with P21/n space group. The crystal data are as follows: a = 9.098(3), b = 16.442(6), c = 12.023(4) Å, β = 91.053(6)°, V = 1798.3(12) Å3, Z = 2, ρ = 2.098 g/cm3, μ = 2.086 mm?1, F(000) =1124, R = 0.0406 and wR = 0.1152 for 3680 observed reflections with I ≥ 2σ(I). In complex III, the conformations of Cd2+ ions are similar to those of the potassium salt complex, and the complex also crystallizes in the monoclinic crystal system with the P21/n space group. The crystal data are as follows: a = 9.134(7), b = 16.500(13), c = 12.075(10) Å, β = 91.054(12)°, V = 1820(2) Å3, Z = 2, ρ = 2.015 g/cm3, μ = 1.856 mm?1, F(000) = 1092, R = 0.0363 and wR = 0.0879 for 3707 observed reflections with I ≥ 2σ(I). 相似文献
952.
Jinzhang Gao Haifeng Fan Wu Yang Xiangli Sun Chongyang Li Xuefeng Mao Jie Wang Rong Wang Zhengping Jia 《Central European Journal of Chemistry》2008,6(4):617-621
A rapid, simple and reliable capillary electrophoresis method for the separation and quantitation of inorganic cations with
indirect UV detection at 214 nm was developed. The electrolyte was: 12 mM imidazole as background absorbance provider; 5 mM
malic acid and 1.0 mM 18-crown-6 ether as complexing agents; and 20% D2O (v/v) to improve ion mobility. The pH was 4.25. The applied voltage was 22 kV at 22°C. Nine ions were completely separated
and determined with correlation coefficients of 0.9979-0.9992. The relative standard deviations (RSD) were less than 0.5%
for migration time and less than 5.2% for peak area (n=8). The detection limits (S/N=3) were from 0.08 mg L−1 (for Na+) to 0.51 mg L−1 (for Cu2+). To assess the reliability atomic absorption (AA) was also used to determine the same samples. Satisfactory results were
obtained for real samples of jasmine tea drink and coconut milk.
相似文献
953.
采用快速溶剂萃取(ASE)技术和高效液相色谱法测定某球形药中叠氮硝胺(DIANP)、硝化甘油(NG)和Ⅱ号中定剂(C2)的含量.ASE提取条件:二氯甲烷做萃取溶剂,萃取温度100℃,静态萃取10min,萃取2次.HPLC测定条件:YWGC18柱(150×4.6mm,10μm),以甲醇和水作为流动相,梯度洗脱,流速1 mL/min,检测波长210nm.测定结果表明DIANP、NG、C2平均回收率分别为99.6%、100.3%、99.4%,RSD分别为0.7%、0.8%、0.9%(n=5),检出限分别为2.1、1.5和0.2mg/L,线性范围分别为0.02~0.98g/L,0.03~1.38g/L,0.002~0.124g/L.用此方法共检测某批球形发射药样品5份,检测结果与滴析-HPLC法检测结果相当. 相似文献
954.
Jian Gao 《Tetrahedron》2008,64(40):9377-9383
Facile routes to several enantiomerically pure flexible chiral building blocks carrying a hidden syn or anti 1,3-diol motif were developed with the inexpensive and readily available carbohydrate d-xylose as the starting material. Application of the newly developed chiral building blocks in total synthesis is exemplified through a synthesis of (2S,4S)- and (2S,4R)-avocadotriol. Both triols were selectively acetylated on the primary hydroxyl group in high yields with Novozyme 435/vinyl acetate. On the basis of comparison of the 1H NMR, optical rotation, and melting point data, the natural avocadotriol 1-monoacetate was assigned to be of (2R,4R) configuration. 相似文献
955.
Lin JM Guan YF Wang DY Dong W Wang XT Gao S 《Dalton transactions (Cambridge, England : 2003)》2008,(44):6165-6169
Seven isomorphous 1D chain Ln3+ complexes Ln(BTA)(HCOO)(H2O)3 (Ln = Pr (1), Gd (2), Eu (3), Tb (4) Dy (5), Er (6) and Yb (7)), and two formate coordinating and bridging 3D Ln3+ complexes Ln(HCOO)3 (Ln = Pr (8) and Nd (9)) have been synthesized and characterized by single crystal X-ray diffraction analysis. Although the Ln3+ ions in 1-7 have different radius, the trivalent lanthanide ions in 1-7 show the same coordinated environment. The well-defined single crystal structures of 8 and 9 are first samples for formate-bridged Ln3+ metallic complexes. The luminescent properties of solid samples of 2-5 at room temperature and the magnetic property of 2 have been also reported and discussed in this paper. 相似文献
956.
Four new heterometallic coordination polymers have been successfully synthesized, namely, {[Ho(2)(HCAM)(6)Mn(3)(H(2)O)(12)].17.5H(2)O}(n) (1), {[Er(2)(HCAM)(6)Mn(3)(H(2)O)(12)].17.5H(2)O}(n) (2), {[Ho(2)(HCAM)(6)Zn(3)(H(2)O)(12)].26H(2)O}(n) (3), and {[Er(2)(HCAM)(6)Zn(3)(H(2)O)(12)].26H(2)O}(n) (4) (H(3)CAM = chelidamic acid). X-ray crystallographic studies reveal that coordination polymers 1-4 are isostructural and crystallized in the rhombohedral crystal system, space group R3. These compounds comprise a 2D honeycomb-type framework. A 2D water sheet is first found in 3 and 4, which exhibits a novel topological motif. The magnetic results for 1-4 show that ferromagnetic interactions take place between the Ho(3+)/Er(3+) and Mn(2+) ions within 1 and 2. 相似文献
957.
The explicit polarization (X-Pol) potential is an electronic-structure-based polarization force field, designed for molecular dynamics simulations and modeling of biopolymers. In this approach, molecular polarization and charge transfer effects are explicitly treated by a combined quantum mechanical and molecular mechanical (QM/MM) scheme, and the wave function of the entire system is variationally optimized by a double self-consistent field (DSCF) method. In the present article, we introduce a QM buffer zone for a smooth transition from a QM region to an MM region. Instead of using the Mulliken charge approximation for all QM/MM interactions, the Coulombic interactions between the adjacent fragments are determined directly by electronic structure theory. The present method is designed to accelerate the speed of convergence of the total energy and charge density of the system. 相似文献
958.
Yezhelyev MV Qi L O'Regan RM Nie S Gao X 《Journal of the American Chemical Society》2008,130(28):9006-9012
We report the rational design of multifunctional nanoparticles for short-interfering RNA (siRNA) delivery and imaging based on the use of semiconductor quantum dots (QDs) and proton-absorbing polymeric coatings (proton sponges). With a balanced composition of tertiary amine and carboxylic acid groups, these nanoparticles are specifically designed to address longstanding barriers in siRNA delivery such as cellular penetration, endosomal release, carrier unpacking, and intracellular transport. The results demonstrate dramatic improvement in gene silencing efficiency by 10-20-fold and simultaneous reduction in cellular toxicity by 5-6-fold, when compared directly with existing transfection agents for MDA-MB-231 cells. The QD-siRNA nanoparticles are also dual-modality optical and electron-microscopy probes, allowing real-time tracking and ultrastructural localization of QDs during delivery and transfection. These new insights and capabilities represent a major step toward nanoparticle engineering for imaging and therapeutic applications. 相似文献
959.
Chen J Jiang J Gao X Liu G Shen G Yu R 《Chemistry (Weinheim an der Bergstrasse, Germany)》2008,14(27):8374-8382
The present study reports the proof of principle of a reagentless aptameric sensor based on surface-enhanced Raman scattering (SERS) spectroscopy with "signal-on" architecture using a model target of cocaine. This new aptameric sensor is based on the conformational change of the surface-tethered aptamer on a binding target that draws a certain Raman reporter in close proximity to the SERS substrate, thereby increasing the Raman scattering signal due to the local enhancement effect of SERS. To improve the response performance, the sensor is fabricated from a cocaine-templated mixed self-assembly of a 3'-terminal tetramethylrhodamine (TMR)-labeled DNA aptamer on a silver colloid film by means of an alkanethiol moiety at the 5' end. This immobilization strategy optimizes the orientation of the aptamer on the surface and facilitates the folding on the binding target. Under optimized assay conditions, one can determine cocaine at a concentration of 1 muM, which compares favorably with analogous aptameric sensors based on electrochemical and fluorescence techniques. The sensor can be readily regenerated by being washed with a buffer. These results suggest that the SERS-based transducer might create a new dimension for future development of aptameric sensors for sensitive determination in biochemical and biomedical studies. 相似文献
960.
Cubic boron nitride based ceramics with silicon were sintered at 1350 °C under a pressure of 5.0 GPa. The effects of post-annealing on grain morphology, surface morphology, and photoluminescence of Si–cBN ceramics were investigated by scanning electron microscope and room temperature photoluminescence measurements. The results showed that the annealing treatment had great influence on cBN grain morphology, rather than the surface morphology. The luminescence intensity increased with annealing temperature and annealing time. The void-net structure formed by continuous distribution of SiOx particulate on the ceramic surface resulted in the emission band peaking at about 701.2 nm, and the tense passivation of Si by SiOx led to the peak's low intensity. The near ultraviolet emission band peaking at about 317 nm was attributed to the oxygen vacancies formed in cBN grain surface, caused by the scavenging of oxygen from the cBN grain surface by the added Si. 相似文献