在卵磷脂溶液中仿生合成无定形碳酸钙

在含有卵磷脂的水溶液中仿生合成了无定形碳酸钙.所得样品用扫描电镜(SEM)、傅立叶红外光谱(FT-IR)、X射线衍射(XRD)和热重分析(TG)等分析方法进行了表征.研究表明:具有一定浓度的卵磷脂可以利用其端基磷酸根基团稳定无定形碳酸钙,这为理解在生物体内的环境中生物矿物的形成机理提供了一种新的途径.     

X-ray and synchrotron methods in studies of cultural heritage sites

X-ray and synchrotron methods that are most widely used in studies of cultural heritage objects (including archaeological sites)—X-ray diffraction analysis, X-ray spectroscopy, and visualization techniques— have been considered. The reported examples show high efficiency and informativeness of natural science studies when solving most diverse problems of archaeology, history, the study of art, museology, etc.     

Methods for studying the coherent 4D structural dynamics of free molecules and condensed state of matter

Studies in the coupled 4D spatial and temporal continuum are necessary for understanding the dynamic features of molecular systems with a complex profile of the potential energy surface. The introduction of time sweep into diffraction methods and the development of principles for studying coherent processes have revealed new approaches to the analysis of the dynamics of wave packets, the intermediate products and the transition state of the reaction center, and short-lived compounds in gaseous and condensed media. The use of picosecond and femtosecond electron probe pulses, synchronized with excitation laser pulses, determined the development of ultrafast electron crystallography, time-resolved X-ray diffraction, and dynamic transmission electron microscopy (DTEM). One of the most promising applications of the developed diffraction methods is the characterization and visualization of the processes occurring upon the photoexcitation of free molecules and biological objects and the analysis of surface and thin films. The whole set of spectral and diffraction methods based on different physical principles, which are complementary and make it possible to perform the photoexcitation of nuclei and electrons and carry out diagnostics of their dynamics at ultrashort time sequences, reveal new possibilities for studies with the necessary integration of the “structure-dynamics-function” triad in chemistry, biology, and materials science.     

The uniqueness of determination of the space group symmetry by means of the vibrational spectroscopy methods

Vibrational spectroscopy methods are used to solve the most fundamental crystallographic problem—determination of crystal symmetry. It is shown that if X-ray diffraction methods do not make it possible to unambiguously choose the symmetry group, it can be successfully done on the basis of joint analysis of the vibrational spectroscopy and X-ray diffraction data. Irreducible representations of vibrations for all systems are systematized, and the cases are indicated where the ambiguity in assignment of crystal structures to the space groups with unified diffraction extinction rules can be avoided.     

Magnetization and structural studies of Mn doped ZnO nanoparticles: Prepared by reverse micelle method

Single phase Mn (2.5 at%) doped ZnO nanocrystalline samples were synthesized by reverse micelle method as characterized by Rietveld refinement analysis of X-ray diffraction data, high resolution transmission electron microscopy and selected area electron diffraction analyses. The X-ray photoelectron spectroscopy and electron paramagnetic resonance (EPR) studies indicated that manganese exist as Mn²⁺ in ZnO lattice. DC magnetization measurements as a function of field and temperature, of 2.5 at% Mn doped ZnO nanoparticles annealed at 675 K, showed room temperature ferromagnetism (RTF). This observation is further confirmed by the EPR spectrum of the sample, which shows a distinct ferromagnetic resonance signal at room temperature. These results indicate that the observed RTF in Mn-doped ZnO may be attributed to the substitutional incorporation of Mn at Zn sites.     

Experimental (X-ray,FT-IR,and UV-Vis Spectroscopy) and Theoretical Methods (DFT Study) of N'-(Dipyridin-2-ylmethylene)-4-methylbenzenesulfonohydrazide

Crystallography Reports - A new hydrazone derivative was synthesized and characterized by IR, UV-Vis spectroscopy, elemental analysis and single-crystal X-ray diffraction. The compound was...     

Electron crystallography as an informative method for studying the structure of nanoparticles

The overwhelming majority of modern nanotechnologies deal with nanoparticles owing to the great variety of their unusual properties, which make them irreplaceable in various fields of science and technology. Since the physical properties of nanoparticles depend on their composition, structure, and shape, the problem of monitoring these parameters both after and during formation of nanoparticles is very important. Methods of electron crystallography are most informative and appropriate for studying and monitoring nanoparticle parameters. In this review, we briefly report the main modern methods based on the use of electron diffraction and electron microscopy, along with examples of their applications for nanoparticles, to solve a number of urgent structural problems of nanomaterials science.     

Pharmaceutical Salts of Fluoroquinolone Antibacterial Drugs with Acesulfame Sweetener

Novel organic salts of norfloxacin and ciprofloxacin with artificial sweeteners such as saccharin and acesulfame were prepared. The two salts 1 and 2 were characterized by differential scanning calorimetry (DSC) and powder X-ray diffraction (PXRD). Finally, the crystal structures were solved by single crystal X-ray diffraction data and the structures were analyzed in terms of supramolecular synthons. In norfloxacin acesulfamate 1, two norfloxacin cations and two acesulfame anions form an eight membered cyclic tetramer supramolecular synthon. The salt, ciprofloxacin acesulfamate 2, has a similar structure as salt 1. This study contributes the importance of crystal engineering and supramolecular chemistry to the pharmaceutical applications in terms of interactions and structural correlations in the design of new solid phases.

Supplemental materials are available for this article. Go to the publisher's online edition of Molecular Crystals and Liquid Crystals to view the free supplemental file.     

Synthesis,growth and characterization of organic nonlinear optical bis-glycine maleate (BGM) single crystals

A new organic compound of bis-glycine maleate was synthesized in the alkaline medium of 10% ammonium hydroxide solution. The bulk single crystals of Bis-Glycine Maleate (BGM) have been grown by slow cooling method. The grown crystals were characterized by employing single crystal and powder X-ray diffraction, Fourier transform infrared, optical absorption spectral studies and thermo gravimetric analysis. The microhardness studies confirmed that the BGM has a fairly high Vicker’s hardness number value (41 kg mm⁻²) in comparison to other organic NLO crystals. Second harmonic generation efficiency of the crystal measured by Kurtz–Perry powder method using Nd:YAG laser is found to be comparable to that of potassium dihydrogen phosphate (KDP). Frequency dependent dielectric studies were carried out along the major growth axis.     

N-(4-吡啶甲基)-L-丝氨酸铜配合物的合成、晶体结构和磁性

氨基酸还原希夫碱HL (N-(4-吡啶甲基)-L-丝氨酸)与CuCl2·2H2O在室温条件通过扩散法合成了配位聚合物{[Cu2(L)2(Cl)2]·H2O}n(I).采用元素分析、红外光谱、X-射线单晶衍射、粉末衍射和热重分析进行了表征.两个结晶学独立Cu(II) 包含于其晶体结构中,Cu1为变形八面体CuO2N2Cl2几何构型;Cu2则呈现略有变形的四方锥结构.Cu1和Cu2通过配体L-的吡啶氮原子以及氯离子的桥连作用连接为2D网状结构.变温磁化率实验表明在温度为2~300 K,配合物I表现为铁磁性耦合.     

A method for automated determination of the crystal structures from X-ray powder diffraction data

An algorithm is proposed for determining the crystal structure of compounds. In the framework of this algorithm, X-ray powder diffraction patterns are compared using a new similarity index. Unlike the indices traditionally employed in X-ray powder diffraction analysis, the new similarity index can be applied even in the case of overlapping peaks and large differences in unit cell parameters. The capabilities of the proposed procedure are demonstrated by solving the crystal structures of a number of organic pigments (PY111, PR181, Me-PR170).     

Synthesis,crystal structure,thermal behavior and luminescence property of a cobalt(II) complex of pyridine-2,6-dicarboxylic acid containing benzimidazole as auxiliary ligand

The new cobalt(II) complex [Co(pydca)(bim)₃] (1) (where H₂pydca = pyridine-2,6-dicarboxylic, bim = benzimidazole) has been synthesized and characterized by elemental analysis, Infrared spectroscopy, X-ray single crystal analysis, thermogravimetric and fluorescent analysis. Single crystal X-ray diffraction analysis reveals that the mononuclear complexes are linked by N–H…O hydrogen bonds. Fluorescent analysis reveals that complex 1 exhibits intense luminescence in ethanol solution at room temperature.     

X-ray diffraction topography for materials science

In this paper, which is dedicated to the 100th anniversary of the discovery of X-ray diffraction (which occurs in 2012), the role and significance of X-ray diffraction topography for materials science are described. The basic principles, methods, and history of the development of X-ray topography (XRT) are briefly stated. A wide experience of practical application of XRT to study the mechanisms of formation of real structure in bulk single crystals and thin films is summarized. Examples of the application of topography methods for investigating and optimizing the production technology of a variety of practically important materials and microelectronic devices are presented.     

Synthesis and physico-chemical characterization of metal free, sodium and potassium phthalocyanine complexes

Sodium phthalocyanine (Na₂Pc), potassium phthalocyanine (K₂Pc) and hydrogen phthalocyanine (H₂Pc) are synthesized in pure state. These complexes are characterized using physico-chemical methods like electronic, IR spectral, magnetic susceptibility measurements, thermogravimetric analysis and X-ray powder diffraction studies. Kinetic and thermodynamic parameters associated with the thermal decomposition were calculated using thermogravimetric analytical data. X-ray diffraction studies revealed that these complexes are having monoclinic crystal lattice structure. Electrical conductivity studies are carried out using two-probe technique in the temperature range 298-473 K for each complex. Sodium phthalocyanine showed semiconducting behavior, whereas potassium phthalocyanine showed first metallic behavior in the temperature range 300-378 K and then semiconducting property in the temperature range 383-473 K. But hydrogen phthalocyanine showed semiconducting behavior in the temperature range 300-390 K and metallic conduction behavior in the temperature range 395-473 K.     

Solid State Synthesis and Hierarchical Supramolecular Self-assembly of Organic Salt Cocrystals

Abstract This paper describes the solid-state synthesis and systematic studies of versatile supramolecular self-assembly of 14 new series of organic salt cocrystals. Hierarchical self-assembly in the solid state utilizes the cooperative interaction of hydrogen bonding, electrostatic and π–π interactions. These salts are crystallized as a highly ordered self-assembly directed by intermolecular non-covalent interaction. Index Abstract Fourteen cocrystals of organic salt have been characterized by single crystal X-ray diffraction and their solid-state packing pattern has been compared. Electronic supplementary material The online version of this article (doi: ) contains supplementary material, which is available to authorized users.     

X-ray diffraction and X-ray standing-wave study of the lead stearate film structure

A new approach to the study of the structural quality of crystals is proposed. It is based on the use of X-ray standing-wave method without measuring secondary processes and considers the multiwave interaction of diffraction reflections corresponding to different harmonics of the same crystallographic reflection. A theory of multiwave X-ray diffraction is developed to calculate the rocking curves in the X-ray diffraction scheme under consideration for a long-period quasi-one-dimensional crystal. This phase-sensitive method is used to study the structure of a multilayer lead stearate film on a silicon substrate. Some specific structural features are revealed for the surface layer of the thin film, which are most likely due to the tilt of the upper layer molecules with respect to the external normal to the film surface.     

Structural aspects of catalytic mechanisms of endonucleases and their binding to nucleic acids

Endonucleases (EC 3.1) are enzymes of the hydrolase class that catalyze the hydrolytic cleavage of deoxyribonucleic and ribonucleic acids at any region of the polynucleotide chain. Endonucleases are widely used both in biotechnological processes and in veterinary medicine as antiviral agents. Medical applications of endonucleases in human cancer therapy hold promise. The results of X-ray diffraction studies of the spatial organization of endonucleases and their complexes and the mechanism of their action are analyzed and generalized. An analysis of the structural studies of this class of enzymes showed that the specific binding of enzymes to nucleic acids is characterized by interactions with nitrogen bases and the nucleotide backbone, whereas the nonspecific binding of enzymes is generally characterized by interactions only with the nucleic-acid backbone. It should be taken into account that the specificity can be modulated by metal ions and certain low-molecular-weight organic compounds. To test the hypotheses about specific and nonspecific nucleic-acid-binding proteins, it is necessary to perform additional studies of atomic-resolution three-dimensional structures of enzyme-nucleic-acid complexes by methods of structural biology.     

Linear trinuclear mixed valance MnIII-MnII-MnIII complex: Synthesis,crystal structure and characterization

A new linear trinuclear Mn^III-Mn^II-Mn^III complex 1 has been synthesized and characterized by elemental, spectral, X-ray and magnetic analysis. X-ray diffraction studies show that the central Mn^II ion is located at a crystallographic inversion center and is triply bridged to the terminal Mn^III ions through one methoxide, one syn-syn carboxylate and one hydroxyl oxygen bridges with the short Mn^III…Mn^II distance that is 3.047 Å. The intermolecular C-H…O, C-H…π and ring-metal interactions are observed in the hydrogen-bonded assembly of 1. Magnetic studies reveal that the mixed-valence complex 1 has S = 3/2 ground state with antiferromagnetic exchange interactions between Mn^II and Mn^III ions.     

Structural studies of sputtered Ni---As---O films

The combined results of chemical analysis, X-ray diffraction and extended X-ray absorption fine structure (EXAFS) studies demonstrate that the majority of Ni atoms in sputtered Ni---As---O films are best described as covalently bonded to six As atoms in a noncrystalline phase. The arrangement of nearest neighbors about the Ni atoms is very similar to that found in crystalline NiAs₂.