Ab initio Structure Determination of [Co(NH_3)_5Br]Br_2 Using Conventional X-ray Powder Diffraction

The crystal structure of [Co(NH3)5Br]Br2 has been determined ab initio from the conventional X-ray powder diffraction data. The approximate structure with all 7 indeyendent non-H atoms was solved by direct methods. The final orthorhombic unit-cell parameters after Rietveld refinement are: a=13.6927, b=10.7071, c=6.9400A, V=1017.47A3, F30=93(0.0075,43), M20=49, Z=4. Space group is Pnma. The structure agreement factors are: Rp=0.066,Rwp=0.090, RF=0.041, RB=0.042.

SYNTHESIS AND STRUCTURE DETERMINATION OF NEODYMIUM COMPLEXES WITH CYCLOHEXANECARBOXYLIC ACID

Two complexes,NdL_3·2C_2H_5OH and NdL_3·2H_2O where L=cyclohexane-carboxylate anion,were synthesized and the structure of the former was determined by the single-crystal X-ray diffration method. The crystal is triclinic,Pspace group with the cell parameters:a=1.2385(6),b=1.2385(6),c=0.9421(5) nm.α=91.69(4)°,β=98.49(4)°,γ=99.16(5)°,Z=2,V=1.436 nm^3.The structure was refined to R value of 0.0866.Each Nd atom is connected with other two Nd atoms by two bidentate and two tridentate carboxyl groups to form a linear polymer.The Nd atom is further coordinated by a chelating carboxyl and two ethanol molecules.So the central atom is nine-coordinated with a distorted monocapped square-antiprism geometry.The infrared spectra and the thermal analysis of the complexes were also studied.

ISOLATION AND STRUCTURE DETERMINATION OF XF-1,A NEW ANTHRACYCLINE ANTIBIOTIC

A new Mutactimycin group antibiotic(XF-1)was isolated from the mycelium of Streptomyces sp.80-115 and its structure has been determined on the basis of its spectroscopical and chemical properties. XF-1 showed active against some Gram positive bacteria.

APPLICATION OF 2D-NMR TECHNIQUES IN THE STRUCTURE DETERMINATION OF HYPODEMATINE

An alkaloid with a novel structure,named Hypodematine,was isolated from Hypodematium sinense Iwatsuki(belonging to Thelypterdaceae).Its structure was elucidated by means of the ~1H-~1H COSY' ~1H-^(13)C COSY and long-range ~1H-^(13)C COSY spectroscopy to have the skeleton of benzo-aza-cyclooctatetraene with a phenyl substituent.Such basic structure has not been found in the na- tural product before.

ISOLATION AND STRUCTURE DETERMINATION OF LAMIOPHLOMICL C,A NEW HIGHLY OXYGENATED IRIDOID FROM LAMIOPHLOMIS ROTATA

A new highly oxygenated iridoid,lamiophlomiol C,was isolated from the roots of Lamiophlomis rotata and its structure was elucidated by spectrosoopic techniques and X-ray diffraction.

Development of “Parameter space screening”-based single-wavelength anomalous diffraction phasing and structure determination pipeline

In this paper, we present a highly efficient structure determination pipeline software suite(X^2 DF) that is based on the "Parameter space screening" method, by combining the popular crystallographic structure determination programs and high-performance parallel computing. The phasing method employed in X^2 DF is based on the single-wavelength anomalous diffraction(SAD) theory. In the X^2 DF, the choice of crystallographic software, the input parameters to this software and the results display layout, are all parameters which users can select and screen automatically. Users may submit multiple structure determination jobs each time, and each job uses a slightly different set of input parameters or programs. Upon completion, the results of the calculation performed can be displayed, harvested, and analyzed by using the graphical user interface(GUI) of the system. We have applied the X^2 DF successfully to many cases including the cases that the structure solutions fail to be yielded by using manual approaches.

High-throughput structure determination of polycrystalline functional materials:a platform for automated 3DED/MicroED data collection

Structure determination plays the most crucial role in the discovery of novel functional materials,because only by knowing the intrinsic structures can we accurately and completely understand their properties and applications.However,most new materials are obtained in polycrystalline form or even as mixtures with multiple phases when first synthesized,presenting significant challenges in their structure determination and phase elucidation.Fortunately,the developed three-dimensional electron diffraction(3DED/MicroED)has provided a promising solution to overcome these challenges.In this study,we have constructed a state-of-the-art 3DED/MicroED data acquisition equipment by integrating a hybrid-pixel detector with a script developed for Serial EM,and thus successfully developed an automated 3DED/MicroED method for the high-throughput structure determination.To demonstrate its effectiveness,a multiphase sample with complex porous structures is employed,showcasing that individual phases and their structures can be identified and determined,respectively.One remarkable finding is the identification of an impurity metal-organic framework(MOF)that is completely invisible to traditional powder X-ray diffraction in a supposedly“pure”commercial MOF sample.Additionally,our method also enables the atomic-resolution structure determination of flexible covalent organic framework materials,which are highly sensitive to electron beams.Moreover,a new microporous aluminoborate is discovered using this rapid structure determination method.These experimental results highlight the enormous potential of our 3DED/MicroED method in the field of new materials discovery,offering a powerful tool for the structure determination of polycrystalline functional materials.

Cryo-EM combined with image deconvolution to determine ZIF-8 crystal structure

Metal–organic frameworks(MOFs) are crystalline porous materials with tunable properties, exhibiting great potential in gas adsorption, separation and catalysis.[1,2]It is challenging to visualize MOFs with transmission electron microscopy(TEM) due to their inherent instability under electron beam irradiation. Here, we employ cryo-electron microscopy(cryoEM) to capture images of MOF ZIF-8, revealing inverted-space structural information at a resolution of up to about 1.7A and enhancing its critical electron dose to around 20 e^(-)/A^(2). In addition, it is confirmed by electron-beam irradiation experiments that the high voltage could effectively mitigate the radiolysis, and the structure of ZIF-8 is more stable along the [100] direction under electron beam irradiation. Meanwhile, since the high-resolution electron microscope images are modulated by contrast transfer function(CTF) and it is difficult to determine the positions corresponding to the atomic columns directly from the images. We employ image deconvolution to eliminate the impact of CTF and obtain the structural images of ZIF-8. As a result, the heavy atom Zn and the organic imidazole ring within the organic framework can be distinguished from structural images.

An Ultrastable π-π Stacked Porous Organic Molecular Framework as a Crystalline Sponge for Rapid Molecular Structure Determination

The crystalline sponge method is a pragmatic and promising strategy for molecular structure determination.However,the dominant metal-organic framework crystal sponge platforms always face poor chemical stability,especially solvent instability,hampering their application in a vaster domain.Herein,we report an ultrastable π-π stacked porous organic molecular framework which exhibits permanent porosity,high thermal stability,and good chemical resistance.It can efficiently implement an approach to molecular structure determination via a single-crystal-to-single-crystal transformation.This is the first example utilizing π-π stacked porous organic molecular framework as“crystalline sponge”to determine a wide variety of guests,ranging from hydrophilic to hydrophobic,and from aliphatic to aromatic,which complements the crystalline sponges based on the famous metal-organic frameworks.More importantly,it can achieve rapid structure determination of small molecules within 3 h.

Accelerating the cryo-EM structure determination in RELION on GPU cluster

The cryo-electron microscopy(cryo-EM)is one of the most powerful technologies available today for structural biology.The RELION(Regularized Likelihood Optimization)implements a Bayesian algorithm for cryo-EM structure determination,which is one of the most widely used software in this field.Many researchers have devoted effort to improve the performance of RELION to satisfy the analysis for the ever-increasing volume of datasets.In this paper,we focus on performance analysis of the most time-consuming computation steps in RELION and identify their performance bottlenecks for specific optimizations.We propose several performance optimization strategies to improve the overall performance of RELION,including optimization of expectation step,parallelization of maximization step,accelerating the computation of symmetries,and memory affinity optimization.The experiment results show that our proposed optimizations achieve significant speedups of RELION across representative datasets.In addition,we perform roofline model analysis to understand the effectiveness of our optimizations.

STRUCTURE DETERMINATION OF KANGLEMEISU A BY X-RAY DIFFRACTION METHOD

Kanglemeisu A (C50H63O19N·CH3OH) is the product of an actinomyces species from a soil sample gathered in China. Kanglemeisu A belongs to the triclinic system, space group P1,unit cell:a=12.760（3）, b=10.287（2）, c=9.926（2） , α=88.39（2）,β=78.64（2）, γ=89.14（2）. RANTAN direct method is used to solve the structure.The final discrepancy factor is R=0.0689, after atom coordinates and temperature factors have been refined with full matrix least squares.The structure skeleton consists of four parts, the naphthalene nucleus connected to the 5-membered ring, a 17-membered ring connected to C2, a dimethyl butane diacid extended out from C20, β-D-3,4-OO’ methylenedigitoxose passing through an oxygen bridge O6 and linked to C27 of ansa ring.

Cryo-EM advances in RNA structure determination

Cryo-electron microscopy(cryo-EM)has emerged as an unprecedented tool to resolve protein structures at atomic resolution.Structural insights of biological samples not accessible by conventional X-ray crystallography and NMR can be explored with cryo-EM because measurements are carried out under near-native crystal-free conditions,and large protein complexes with conformational and compositional heterogeneity are readily resolved.RNA has remained underexplored in cryo-EM,despite its essential role in various biological processes.This review highlights current challenges and recent progress in using cryo-EM singleparticle analysis to determine protein-free RNA structures,enabled by improvement in sample preparation and integration of multiple structural and biochemical methods.

Chemical synthesis and structure determination of venom toxins

Venom toxins are widely spread in nature, adopting diverse structures and functions. They often function by blocking or modulating important membrane protein targets thus can be promising therapeutic candidates and biophysical probes. In this review, we briefly discuss the total chemical synthesis of venom toxins including the different refolding strategies reported during the past decade as well as innovative approaches for structure determination.

Laser-phase determination methods and transfer equations for direct temporal structure measurements of atto- and femtosecond XUV pulses

In this paper the laser-phase determination methods and transfer equations are presented to directly reconstruct the detailed temporal structures of ultra-short extreme ultraviolet （xuv） pulses from the measured photoelectron energy spectra （PES）. Each transfer equation includes one of PID （proportional-integral-differential） terms of PES. The intensity and instantaneous frequency of attosecond xuv can be retrieved from the integral term of PES. The intensity profiles of narrow bandwidth atto- and femtosecond xuvs can be rebuilt from the proportional and differential terms of PES respectively. The methods and equations may be used to improve time resolutions in measuring ultrashort pulses.

A Comparative Study of Dispersion Characteristics Determination of a Trapezoidally Corrugated Slow Wave Structure Using Different Techniques

The linear dispersion relation of a trapezoidally corrugated slow wave structure （TCSWS） is analyzed and presented. The size parameters of the TCSWS are chosen in such a way that they operate in the x-band frequency range. The dispersion relation is solved by utilizing the Rayleigh-Fourier method by expressing the radial function in terms of the Fourier series. A highly accurate synthetic technique is also applied to determine the complete dispersion characteristics from experimentally measured resonances （cold test）. Periodic structures resonate at specific frequencies when the terminals are shorted numerical calculation, synthetic technique and cold appropriately. The dispersion characteristics obtained from test are compared, and an excellent agreement is achieved.

Determination of the Seismogenic Structure of the 1861 East of Pulandian M6.0 earthquake

The 1861 M6. 0 earthquake occurring in the east of Pulandian is another strong earthquake with M ≥ 6. 0 besides the 1975 Haicheng MT. 3 earthquake in the Liaodong peninsula. Through repeated investigations, the epicenter of the 1861 earthquake was located at Gupao, a village east of Pulandian. Based on the analyses of damage survey and precise location of modern instrumental earthquake data, the activity and seismic risk of the Jinzhou fault, Pulandian bay fault and the NW-trending Pulandian fault were analyzed. And by comparing the deep seismogenic environment between Pulandian and Haicheng, it is found that, as a neogenic active fault, the NW-trending fault, conjugated with the Jinzhou fault, has a higher seismic risk. The NW-trending fault is the seismogenic structure of the 1861 M6. 0 earthquake. And the Jinzhou fault, as a major fault in the Liaodong Peninsula, has controlled the seismicity of the region. The Pulandian bay fault is relatively inactive, with weak seismicity, and unrelated to the earthquake.

DETERMINANTS OF STRUCTURE IN AQUATIC NON-PELAGIC PROTOZOAN COMMUNITIES

Although microbes have traditionally been used as models for testing ecological theory, research on the organization of these communities has largely been isolated from other areas of community ecology. Early studies indicated that microbial populations can form dynamic, interacting assemblages. Observations of distributional patterns suggest that certain deterministic forces regulate community structure. It appears that protozoans are tolerant of a wide range of environmental conditions although evidence for this is largely based on gross environmental analyses. Laboratory studies have suggested the importance of negative and positive biotic interactions in determining community membership, but little field evidence for this exists. The importance of transport processes in controlling community composition is being increasingly recognized. All three types of processes likely act to regulate the colonization and successional dynamics of these communities. A simple model is presented to promote the

Structured Equation Model of Tuberculosis Incidence Based on Its Social Determinants and Risk Factors in Bandar Lampung, Indonesia

World Health Organization through tuberculosis (TB) control averted up to six million deaths and cured thirty-six million people in 1995-2008, but had less success in reducing TB incidence, especially in thirteen high burden countries, including Indonesia. Therefore, TB control will need to have more emphasis on the issues of social determinants, as social determinants affect TB’s incidence directly and/-or through TB’s risk factors. This study aimed to identify a significant effect of social determinants and the risk factors of TB incidence. The research setting was at twenty-seven primary health centers and one hospital that have implemented the Directly Observed Treatment Short Course (DOTS) strategy in Bandar Lampung municipality, Indonesia. Respondents of this research were 238 smear-positive TB patients as case group and 238 patients without TB as control group. Research variables consisted of “social determinants”, “housing condition”, “household food security” and “health access” which were set as latent variables and measured through their indicators. Data had been collected by using questionnaire and then was analyzed with Structural Equation Modeling using SmartPLS 2.0 software. The result showed that “social determinants” through “housing condition” and “household food security” affected “TB incidence”. Moreover, “social determinants”, “housing condition” and “household food security” can be used to explain 34.1% variation of “TB incidence”. In conclusion, the knowledge can be used to support the TB control program, particularly to implement the DOTS strategy together with improving social determinants, housing condition and household food security.

Determinants of Capital Structure in the Nigerian Listed Insurance Firms

The paper investigates the determinants of capital structure in Nigerian listed insurance firms using data obtained from annual report of the sampled firms for the period of 2001-2010. It used five explanatory variables to measure their effects on debt ratio. Multiple regression is employed as a tool of analysis. The result reveals that all the explanatory variables have statistically and significantly influenced the explained variable. The results approve the prediction of pecking order theory in the case of profitability and trade-off theory in case of tangibility variables. The growth variable supports the agency theory hypothesis whereas size variable confirms to the asymmetry of information theory. It is therefore recommended that the management of listed insurance firms in Nigeria should always consider their positions using these capital structure determinants as important inputs before embarking on debt financing decision.

The Determinants of Capital Structure： an Empirical Study of Publicly Listed Medicine Manufacturing Companies in China

This paper attempts to analyze the important determinants of capital structure in the medicine manufacturing industry of China. Two measures including the ratio of long-term debt to asset and the ratio of total debt to asset are used as the proxies of leverage, while dependent variables used are asset structure, growth, firm size, profitability and risk. The evidences presented here indicate that asset structure and size significantly influence the capital structure choice.