Crystallographic studies on the binding of coenzyme analogs to D-glyceraldehyde-3-phosphate dehydrogenase from Palinurus versicolor

In contrast with the coezyme, two coenzyme analogs, ADP-ribose and SNAD, bind non-cooperatively to D-glyceraldehyde-3-phosphate dehydrogenase (GAPDH). Palinurus versicolor (PV) GAPDH complexed with ADP-ribose and SNAD has been crystallized by the method of sitting-drop vapor diffusion. X-ray diffraction data analysis reveals that both crystals belong to the same space group (C2), and have similar cell dimensions: a =152.80(A), b =100.35(A), c =128.31(A), b =110.28° and a =153.41(A), b =100.51(A), c =128.44(A), b =110.48° , respectively. It is estimated that the asymmetric unit in each crystal contains 4 subunits. This is a novel crystal form which is quite different from that previously reported for holo- and apo-GAPDH from the same source. The result suggests that the binding of the two coenzyme analogs to GAPDH may lead to some significant conformational changes, which are different from those induced by the coenzyme binding. The self-rotation function indicates that the tetramer of these two GAPDH complexes also has good 222 symmetry. The structural analysis and the comparison with holo- and apo-GAPDH may give a clue to the cooperative mechanism of the enzyme.     

Crystal structure determining of 7-ADCA based on X-ray powder diffraction

Traditionally, crystal structure data can be collected and determined from single-crystal X-ray diffraction. However, in the fields of organic and macromolecular crystallography, it is often difficult or impractical to grow single crystals with suitable sizes and purity. Therefore, it will be benefited from the newly growing analytical tool that combining X-ray powder diffraction based on polycrystalline samples and ab initio calcula- tion[1]. 7-ADCA is one of the most important intermediate…     

Synthesis and characterization of a three-ring bent-core compound

To investigate the vacuum-deposited films of the banana-shaped mesogens, we prepared a three-ring bent-core （that is, banana-shaped） compound m-bis（4-p-octoxysryrenyl）benzene （m-OSB） and used it as a prototype for studying the related film physics. Herein the synthesis and the structural characterization of m-OSB are reported.^13C and ^1H NMR spectra and ^1R spectrum confirm that m-OSB has a symmetric and all-trans conformation. The results of differential scanning calorimetry, polarizing optical microscopy and X-ray diffractometry indicate that no liquid crystalline phase but two crystalline phases are present in this material： phase Ⅰ （T〈66℃） and phase Ⅱ （66~C〈T〈157℃）; an isotropic state is observed at above 157℃. Combining the X-ray diffraction and the electronic diffraction, we assign the room-temperature crystalline phase I to orthorhombie system and P212121 space group with cell parameters of a = 7.43A°. b=6.34A°, c=72.07A°, and α=β=γ=90°. Molecular modeling reveals that the molecules in the unit cell adopt a layered structure with an antiferro-eleetrie alignment. The structure of phase Ⅱ is very similar to that of phase Ⅰ. Nonlinear optical measurement shows that m-OSB is active for the second harmonic generation （SHG）. Such characterization of the bulk material is necessary for the understanding of the growth and microstructures in the films.     

Crystal structure, magnetic and photoelectric properties of coordination polymer[ Co2（C3H4N2）4（ C10H2O8） ]n

The coordination polymer is designed and synthe-sized through the choice of organic ligand and coordina-tion geometry of metal ion as well as the control over theinfinite network topology structure, which usually con-tains both the characteristic of the organic molecules andmetal ions. So, it exhibits more singular function and haspotential application in optics, electrics, information, ca-talysis, medicament, metallurgy, novel material and lifesciences fields. And it has been the confluence m…     

Comparative crystal structure determination of griseofulvin: Powder X-ray diffraction versus single-crystal X-ray diffraction

In an attempt to compare crystal structure determination from powder data and single-crystal data,crystal structure of griseofulvin(C 17 H 17 ClO 6) was tested by both powder and single-crystal X-ray diffraction.Lattice parameters of griseofulvin are α=90.0°,a=b=8.9757,c=19.9345,V=1605.99 3 from powder data coinciding with α=90.0°,a=b=8.9714,c=19.8848,V=1600.46 3 from single-crystal data.Main processes of structure elucidating of griseofulvin by the two approaches were analyzed.Powder X-ray diffraction was demonstrated to be a powerful auxiliary implement to single-crystal X-ray diffraction in structure characterization,and its application can be popularized in the field of structure research of small organic molecules.     

Xieite, a new mineral of high-pressure FeCr2O4 polymorph

Xieite, a new mineral, occurs in the shock vein of the Suizhou meteorite. The mineral has an orthorhombic structure and its space group is Bbmm. The cell parameters are a = 9.462（6） A, b = 9.562（9） A, c = 2.916（1）A. The crystal-chemical formula is （Fe0.87Mg0.13Mn0.01）1.01（Cr1.62AI0.25Ti0.08V0.02）1.97O4, or simply formula FeCr2O4. Stronger X-ray diffraction lines are [d （A）, I/Io]： （2.675, 100）, （2.389, 20）, （2.089, 10）, （1.953, 90）, （1.566, 60）, （1.439, 15）, （1.425, 15）, （1.337, 40）. Xieite is a high pressure polymorph of FeCr2O4 and formed by solid-state transformation of chromite under shock-induced high pressure and temperature, in association with other high-pressure minerals including ringwoodite, majorite, lingunite and tuite. The P-Tcondition for the formation of xieite is estimated to be 18--23 GPa and 1800--1950℃, respectively. Xieite has recently been approved by the Commission on New Minerals, Nomenclature and Classification of the International Mineralogical Association （IMA 2007-056）. The mineral name, xieite, is named after Xiande Xie.     

Crystallization and preliminary X-ray analysis of an anti-insect toxin BmK 16 fromButhus martensii Karsch scorpion

An excitatory anti-insect toxin from BmK scorpion, named BmK 16, has been purified and crystallized recently. Two crystal forms have been obtained by using ammonium sulfate as precipitant at different pH, one of which is single crystal. Diffraction data have been collected for the single crystal on a Mar Research 345 Image Plate. The analyses of the data show that the crystal can diffract to 0.28 nm resolution and belongs to the space group C2 with unit cell parameters a = 4.65 nm,b = 8.52 nm,c = 3.26 nm, α = γ = 90°, β = 110.5°. There are 2 molecules per asymmetric unit according to its unit cell volume and molecular weight.     

Synthesis and characterization of two new types of oxovanadium complexes with pyrazole as ligand

Coordination chemistry of pyrazole-base ligands has been extensively studied since the poly(pyrazole)borate was invented by Trofimenko in 1966[1―4]. A variety of bidentate or multidentate pyrazole-derived ligands have been employed in coordination chemis…     

β-Ｄ-吡喃葡萄糖叠氮化物的合成及晶体结构

合成了β-Ｄ-O四乙酰基糖基叠氮化合物， 并得到单晶， 经X射线衍射方法解析， 其晶系属于单斜晶系，P2₁空间群， 其中a=0.759　6(6) nm,b=1.518　4(13) nm，c=1.641　2(14) nm，V=1.893　0(3) nm³，α=90.00°，β=90.045(1)°，γ=90.00° ，Z=2. 在晶体结构中， 六元糖环采取经典⁴C₁椅式构象， 糖环上所有 的取代基均以平伏键存在， 其中叠氮基不是以直线型结构存在， 呈现一定的弯曲现象.     

Hydrothermal synthesis and characterization of new hybrid open-framework indium phosphate-oxalates

Crystalline open-framework inorganic materials have been widely studied because of the wide variety of the structures as well as their applications in heterogeneous catalysis, adsorption and ion exchange[1,2]. Of many open-framework solids, metal phosphates are an important family of materials, a large number of aluminum phos-phates[3,4], gallium phosphates[5—7], zinc phosphates[8—10], cobalt phosphate[11], beryllium phosphates[12—14] have been prepared and characterized. Recently, open-fra…     

Facile synthesis of nanosized sodium magnesium hydride, NaMgH3

The ternary magnesium hydride NaMgH 3 has been synthesised via reactive milling techniques.The method employed neither a reactive H2 atmosphere nor high pressure sintering or other post-treatment processes.The formation of the ternary hydride was studied as a function of milling time and ball:powder ratio.High purity NaMgH 3 powder(orthorhombic space group Pnma,a 5.437(2),b 7.705(5),c 5.477(2) ;Z 4) was prepared in 5 h at high ball:powder ratios and characterised by powder X-ray diffraction(PXD),Raman spectroscopy and scanning electron microscopy/energy dispersive X-ray spectroscopy(SEM/EDX).The products formed sub-micron scale(typically 200-400 nm in size) crystallites that were approximately isotropic in shape.The dehydrogenation behaviour of the ternary hydride was investigated by temperature programmed desorption(TPD).The nanostructured hydride releases hydrogen in two steps with an onset temperature for the first step of 513 K.     

High-pressure polymorph of TiO2-II from the Xiuyan crater of China

Abundant TiO2-II, a high-pressure polymorph of titanium dioxide, was found in the gneiss fragments of impact-produced breccias from the Xiuyan crater. Rutile in the gneiss was severely fragmented and fine-grained clasts less than 2 ~tm in size had been transformed to TiO2-II. Irregular thin layered TiO2-II is also observed in coarse-grained ruffle fragments, where the TiO2-II layers distributes along fractures and cracks in rutile, About 30 percent of rutile in the gneiss had been transformed to TiO2-II. Fine grains of TiO2-II display light bluish grey to light yellow brown in plane-polarized reflected light. Crystallographic investigation shows that TiO2-II has an orthorhombic structure with space group Pbcn. The cell parameters are a=4.543（1）/~, b=5.491（9）/~ and c=4.895（2） ,~. Its empirical formula calculated on the basis of two oxygen atoms can be written as （Tio.985Feo.oosNbo.oor- Si0.003Zr0.0Ol）l.0O302, or simply formula TiO2. According to the shock effects of quartz and feldspars, the peak shock pressure and post-shock temperature in the TiO2-II-bearing gneiss are estimated to be between 35 and 43 GPa and 300-900~C, respectively. The finding of TiO2-II in the shock-metamorphosed gneiss provides another mineral physics evidence for shock origin of the Xiuyan crater.     

Chenguodaite （Ag9FeTe2S4）： a new tellurosulfide mineral from the gold district of East Shandong Peninsula,China

Chenguodaite, approved by IMA-CNMMN （2004-042a）, was discovered in the Bunan quartz vein-type gold deposit in the gold district of East Shandong Peninsula. The mineral occurs in high grade Au-Ag-Cu ores, coexisting with galena, chalcopyrite, hessite, electrum, unnamed Ag6TeS2 and AglsFeBiTe3Se, enclosed and replaced by native silver and acanthite. In the reflected light microscope, the mineral has light gray color, indistinguishable anistropism and hardness around 2-3. The color indices of chenguodaite relative to ICE C illuminator are： x=0.3027, y=0.3076, Y=25.78%,λd=474 nm, Pe=3.68%, similar to those of canfieldite. The average chemical composition from 16 microprobe analyses is Ag8.97Fe1.00Te1.99S4.04, idealized to AggFeTe2S4. The polycrystalline X-ray diffraction of chenguodaite by Gandolfi camera and synchrotron oscillation photography results in 67 reflections with the 12 strongest being （relative intensity in bracket）： 6.742（69）, 6.416（39）, 5.951（33）, 3.265（100）, 2.981（24）, 2.649（22）, 2.25（24）, 2.188（71）, 2.142（22）, 2.123（31）, 2.044（23）, 1.949（33）, which are indexed to a primitive orthorhombic cell with a=12.769 （2） A, b= 14.814（2） A, c= 16.233 （1） A, V= 3070.6 A^3, Z= 9, Dcal.=6.85 g/cm^3. The name is for the late Prof. Chen Guoda, a famous Chinese geologist and the founder of Diwa-Geodepression theory of tectonics.     

Syntheses, characterization, crystal structure and magnetic properties of copper(Ⅱ)α, β-unsaturated carboxylate complexes with trimethyl phosphate

Two ternary complexes Cu2A4[OP(OCH₃)₃]₂ (A represents CH₂== CH—COO- and CH₂== C(CH₃)—COO-) have been synthesized, and elemental analyses, IR, ESR, electronic reflectance spectra and magnetic studies were carried out. The single crystal X-ray diffraction shows that Cu₂[CH₂== C(CH₃)—COO]₄[OP(OCH₃)₃]₂ is triclinic, with space group P1, a = 1.05128(13), b = 1.7559(5), c = 1.94479(3) nm, α = 91.263(14)°, β = 102.559(6)°, γ = 106.339(13)°, Z = 4 and R = 0.0668. Two copper(Ⅱ) atoms are bridged by four a -methacrylate groups, and each copper(Ⅱ) atom is coordinated with a trimethyl phosphate molecule in the axial position, forming a distorted square pyramidal configuration. The symmetric center is between the two copper(Ⅱ) atoms, and the Cu-Cu bond distance is 0.26098(6) nm. The Cu-Cu distance and magnetic studies suggest that there exist antiferromagnetic interactions between the two copper(Ⅱ) atoms.     

Crystal structure and magnetism of the binuclear Gd(III) complex Gd2(C12H8N2)2(C6H5COO)6

In the medium of H₂O, C₂H₅OH and HAC, the reaction of Gd(NO₃)₃·6H₂O with C₆H₅COONa and C₁₂H₈N₂ produced a novel binuclear Gd(III) complex in formula [Gd₂(C₁₂H₈N₂)₂ (C₆H₅COO)₆]. Crystallographic data: crystal system, triclinic; space group, P1; unit cell dimensions, a=1.191 9(2) nm,b =1.244 2(2) nm,c = 1.080 4(2) nm, α = 93.57(3)°, β= 113.33(3)°, γ= 105.06(3)°, Z=l. The finalR =0.037 6. The magnetic measurement of the crystal powder in the temperature region of 1.5–300 K shows that this complex possesses antiferromagnetic property with fitting magnetic parametersJ = −0.471 andg =1.975.     

Hydrothermal synthesis and crystal structure of copper （Ⅱ） coordination polymer composed of helix-like chains： [Cu（NIeH）（bpy）]

Hydrothermal reactions of Cu （Ⅱ） acetate, 2,2＇-bipyridyl （bpy） with 5-nitroisophthalic acid （H2NIPH） resulted in a new coordination polymer [Cu（NIPH）（bpy）] 1. Single crystal X-ray diffraction experiment indicates that 1 possesses a single helixlike chains, of which Cu atoms are coordinated by NIPH ligands and bpy ligands. Compound 1 crystallizes in the space group P2（ 1）/c, a = 0.955（19） nm, b = 1.259（3） nm, c = 1.3737（3） nm, ,6= 95.13（3）°, V= 1.6455（6） nm^3 and Z = 4. The TGA analysis shows that 1 has no remarkable weight loss up to 284℃, as a result of its high thermal stability. Magnetic measurements indicate an antiferromagnetic behavior of compound 1.     

[Ag(C_5H_6N_2)_2]·(C_7H_5O_2Cl)·2H_2O的合成和结构

合成出标题配合[Ag(C5H6N2)]·(C7H5O2Cl)·2H2O．配合物经X射线单晶结构分析结果表明,属三斜晶系, 空间群为P-1,a=0．736 8(4),b=0．955 3(6),c=1．5 56 6(9)nm,α=73．301(10),β=76．591(11),γ=75．961(10), V=1．024(10)nm3,Z=2,最终偏差因子R[I>2(I)]a,R1=0．076 6,wR2=0．145 4．     

Synthesis,Structure and Antitumor Activities of [Ni（dien）2][Ni（CN）4] Complex

Ni(II)-dien complex was prepared and characterized by X-ray diffraction. The crystal belongs to triclinic system, space group P-1, with crystallographic parametersa=0.888 13(18) nm,b=0.890 10(18) nm,c=1. 591 8(3) nm, α=77.71(3)°, β=89.12(3)°, γ=61.24(3)°,Z=2. The two dien molecules coordinate to the central Ni atom, the six nitrogen atoms form a distorted octahedron. Preliminary pharmacological tests showed this complex had antitumor activity against HepG₂ and HL-60 cell linesin vitro. Foundation item, Supported by the National Natural Science Foundation of China (29972034) Biography: Li Tao (1976-), male, Ph. D candidate, research direction: ophthalmology and chemicalbiology.     

High-pressure and high-temperature synthesis of MgB2 and its superconductivity

The single-phase sample of MgB₂ was prepared successfully at the temperature of 900℃ and under the pressure of 3 GPa. The structure of the sample was investigated using powder X-ray diffraction and Rietveld analysis. The results show that the structure of the sample belongs to the hexagonal structure with space group of P6/mmm, a=3.0861(5) Å, c=3.5222(8) Å. The magnetic and resistance measurements indicate that the superconducting transition temperature T_c is 39 K.     

1-甲基海因的合成及其晶体结构分析

以甲胺、 氯乙酸钠、 氰酸钠等为原料, 用“一锅法”合成1-甲基海因, 合成总收率为62.9%.单晶经X射线衍射方法解析, 其晶体属于单斜 晶系, P2₁空间群, 其中a=0.558 9(3) nm, b=1.217 6(6) nm, c=0.809 0(4) nm;β=105.330(7)°;V=0.531 0(5) nm³;Z=4, D_c=1.427 mg/m³, μ=0.116 mm^-1, F(000)=240.