Single‐Crystalline and Near‐Monodispersed NaMF3 (M=Mn,Co, Ni,Mg) and LiMAlF6 (M=Ca,Sr) Nanocrystals from Cothermolysis of Multiple Trifluoroacetates in Solution

We report the synthesis of single‐crystalline and near‐monodispersed NaMF₃ (M=Mn, Co, Ni, Mg), LiMAlF₆ (M=Ca, Sr), and NaMgF₃:Yb,Er nanocrystals (quasisquare nanoplates, nanorods, and nanopolygons) by the cothermolysis of multiple trifluoroacetates in hot combined organic solvents (oleic acid, oleylamine, and 1‐octadecene). The nanocrystals were characterized by XRD, TEM, superconductive quantum interference device (SQUID), and upconversion luminescence spectroscopy. By regulating the polarity of the dispersant, the NaMF₃ (M=Mn, Co, Ni) nanoplates were partially aligned to form nanoarrays on copper TEM grids. The sizes of the NaMF₃ nanocrystals were easily tuned by the use of proper synthetic conditions such as reaction temperature and time and solvent composition. On the basis of a series of experiments in which the reaction conditions were varied, together with GC–MS and FTIR analysis, the reaction pathways for the formation of these nanocrystals from trifluoroacetate precursors were proposed. The magnetic measurements showed that the differently sized NaMnF₃ square plates displayed interesting weak ferromagnetic behavior on the nanometer scale. The strong red upconversion luminescence emitted from the NaMgF₃:Yb,Er nanorods under 980‐nm near‐IR laser excitation suggests that NaMgF₃ may be a good candidate host material for red upconversion luminescence.     

Determination of Levofloxacin in Human Urine with Capillary Electrophoresis and Fluorescence Detector

In this study, we developed an analytical method for the enantioseparation of ofloxacin, using capillary electrophoresis with fluorescence detection. The optimum background electrolyte was obtained to be 60 mM hydroxylpropyl‐β‐cyclodextrin (HP‐β‐CD) in 50 mM phosphate buffer at pH 2.30. Under these conditions, the (+) and (‐) ofloxacin were completely separated, with the detection limit of 10 nM when the sample was prepared in deionized water. The linear ranges of levofloxacin in deionized water and untreated urine were 10^?7 to 5 × 10^?3 M with R² = 0.9989 and 5 × 10^?6to 5 × 10^?3 M with R² = 0.9943, respectively. We also applied this method to investigate the purity of a commercial drug. The results revealed that the ratio between (+)‐ofloxacin and (‐)‐ofloxacin (levofloxacin) was 99.9:0.1, and there is about 93 mg levofloxacin per tablet (200 mg). The concentration of levofloxacin in patient's urine was founded to be 7.9 × 10^?4M, and the ratio between the two optical isomers was 99.3:0.7.     

Helicity‐Encoded Molecular Strands: Efficient Access by the Hydrazone Route and Structural Features

Control over the folding of molecular strands may be achieved by appropriate choice of the constituting subunits, in particular for chains of specific heterocycles such as sequences of directly connected pyridine (py) and pyrimidine (pym) rings, which are known to fold into extended helical structures. Since the hydrazone (hyz) group represents an isomorphic analogue of a py site, the condensation of hydrazine and carboxaldehyde derivatives of pym offers a very efficient approach to strands incorporating hyz instead of py units and constituted by sequences of alternating hyz and pym groups. A series of such strands of different lengths, up to ten hyz units, i.e., 1 – 7 , were synthesized. Their spectral properties indicate that they fold indeed into helical shapes. Extensive characterization was performed in solution by ¹HNMR spectroscopy and in the solid state by determination of the crystal structures of eight such strands. They all display the expected helical geometry with up to 3 ¹/₃ turns and direct stacking contacts. The efficiency and flexibility of the synthetic approach as well as its wide potential for generation of diversity through lateral decoration make the (hyz? pym) subunit a particularly attractive helicity codon.     

水相中乙醇对胶体泡沫性质的影响

用不同比例的水-乙醇混合物作水相制备了胶体泡沫（CLA）,实验观察并测定了CLA的形态、粒径分布、半衰期、Zeta电位、水相溶液的粘度和水相/油相之间的界面张力等性质.结果表明，水相中加入乙醇会影响CLA的稳定性和粒径大小,但对CLA的Zeta电位影响不大.乙醇对CLA稳定性的影响主要是由于乙醇分子嵌入到界面膜中导致膜的强度变化以及水相粘度发生变化导致CLA粒子间隙的排液过程发生变化.     

Preparation ,Structural Characterization and Luminescent Property of Binucleasr Silver（Ⅰ）Complex Formed by Benzotriazole and 1—Hydroxymethyl Benzotriazole

Dinuclear silver (I) six‐membered ring complex [Ag₂ (bta)₂ ‐(hmbta)₂] (ClO₄)₂ (3) has been synthesized by the reaction of benzotriazole (bta) (1) and 1‐hydroxymethyl benzotriazole (hmbta) (2) with Ag (CH₃CN)₄ClO₄. The structures of compound 2 and Complex 3 have been studied by single crystal X‐ray diffraction analysis. The change of luminescent intensity of 1, 2 and 3 was reported. Compound 2 crystallizes in the monoclinic system with space group P2 (1)/c, a = 0.7655 (10) nm, b = 1.0126 (14) nm, c =0.9502 (13) nm, β = 95.07 (2)°, V = 0.7337 (17) nm³ and Z = 4. Complex 3 crystallizes in the triclinic system with space group P1, a = 0.73611 (18) nm, b = 0.9152 (2) nm, c = 1.2277 (3) nm, β = 87.170 (5)°, V = 0.8221 (3) nm³ and Z = 1. The main structural feature of complex 3 is a symmetric dinuclear six‐membered ring formed by two silver (I) atoms and four N‐atoms from two benzotriazoles. The second structural feature of complex 3 is the τ‐τ stacking interaction between two adjacent molecular planes, which forms the two‐dimentional layer structure. Besides, compared with 2, the luminescent intensity of complex 3 shows a remarkable enhancement.     

Surface-enhanced Raman spectra study of metal complexes of N-D-glucosamine beta-naphthaldehyde and glycine and their interaction with DNA

Copper(II), zinc(II), cobalt(II) and cobalt(III) complexes of N-D-glucosamine beta-naphthaldehyde (C17H19O6N, NG) and glycine were synthesized. The four novel metal complexes, Cu(II)C19H28O11N2(CuGNG), Zn(II)C19H24O9N2 (ZnGNG), Co(II)C19H28O11N2(Co(II)GNG) and Co(III)C21H29O12N2(Co(III)GNG) were characterized by means of infrared (IR), electronic absorption spectroscopy and NMR etc. The surface-enhanced Raman spectra of the four complexes and their interaction with DNA were studied. By comparison of the surface-enhanced Raman spectra (SERS), the information of the four complexes' SER active sites and adsorption orientation were obtained. Combined with fluorescence spectra of Ethidium bromide (EthBr) DNA system, we concluded that none of the four complexes intercalate into DNA and that the presence of the glycine ligand lowered the anticancer activity of NG series complexes.     

Experimental studies of the dynamics of the bond-forming reactions of CF2(2+) with H2O using position-sensitive coincidence spectroscopy

The dynamics of the product channels forming OCF(+)+H(+)+HF and HCF(2) (+)+H(+)+O following the collisions of CF(2) (2+) with H(2)O have been investigated with a new position-sensitive coincidence experiment at a center-of-mass collision energy of 5.6 eV. The results show the formation of OCF(+) occurs via the formation of a doubly charged collision complex [H(2)O-CF(2)](2+) which subsequently undergoes a charge separating dissociation to form H(+) and HOCF(2) (+). The HOCF(2) (+) monocation subsequently fragments to form HF+OCF(+). The lifetimes of the collision complex and the HOCF(2) (+) ion are at least of the order of their rotational period. The kinetic energy release in this reaction indicates that it involves the ground state of CF(2) (2+) and forms the ground electronic states of OCF(+) and HF. The mechanism for forming HCF(2) (+) involves the direct and rapid abstraction of a hydride ion from H(2)O by CF(2) (2+). The resulting OH(+) ion subsequently fragments to H(+)+O, on a time scale at least comparable with its rotational period.     

Studies on the Physicochemical Properties, Structure and Antitumor Activity of an Oligosaccharide Homologue SnS-2 from the Root of Scrophularia ningpoensis Hemsh

An oligosaccharide homologue named SnS-2 was isolated from the root of Scrophularia ningpoensis Hemsl.SnS-2 was purified by means of gel-permeation chromatography and ion-exchange chromatography. Its physicochemical properties, including carbohydrate content and molecular weight were determined. The structure of SnS-2 was elucidated by chemical methods along with ^1H and ^13C NMR spectroscopy, including two-dimensional DQCOSY and H-detected ^1H, ^13C HMQC experiments. These results show that SnS-2 possesses a backbone consisting of terminal α-Galp-(1→, α-Galp-(1→6), α-Glcp-(1→6) and nonreducing end β-Fruf-(2→. The bioactive assay showed that it could inhibit the growth of Lewis pulmonary carcinoma implanted in mice.     

Paraquat guest induced hydrogen-bonding modes of a hydrazide-derived bis(meta-phenylene)-32-crown-10 host in the solid state

A hydrazide-derived bis(meta-phenylene)-32-crown-10 host showed a dimeric structure via quadruple N-H?O hydrogen bonds, but a polymeric structure via two N-H?O hydrogen bonds and two C-H?O hydrogen bonds at each knot in the presence of paraquat in the solid state, which led to a novel poly(taco complex) and ordering arrangement of the guest molecules indirectly.