Crystallization and preliminary X-ray analysis of an anti-insect toxin BmK I6 from Buthus martensii Karsch scorpion

An excitatory anti-insect toxin from BmK scorpion, named BmK I6, 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.     

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.     

Determination of crystal structure of omphacite

The chemical formula of omphacite was expressed with (MⅡ MⅠ ) (Si, AI)2O6. Cations that occupied the MⅡ site were large cations such as Ca or Na, and (Na/(Na+Ca)) ratio ranged from 0.2 to 0.8; the 6-coordinated MⅠ site accommodated cations such as Mg, Fe2+, Al, Fe3+ ,and(AI/(AI+Fe3+)) ratio was more than 0.5. Omphacite space groups reported were C2/ c, P2, P2/n, P2/c, cell parameters are α0 = 0.9600-0.9630 nm,b0 = 0.8750-0.8830 nm,c0 = 0.5230-0.5290 nm,β = 106°40′-107°10'. The sample was picked up from the eclogites in Zhucheng County, Shangdong Province. The intensity data were collected with the RIGAKU RASA Ⅱ -S four-circle single crystal diffractometer.The correct structure model was obtained by using the Patterson method and Fourier synthesis, SHELX-76 program, structure refinement with 905 independent diffraction points (| F0 |> 3σ |F0 |). After the structure parameter refinement, the R-factor reduced to 0.0515. The crystal structure analysis indicates that omphacite has a new space group-Pn space group.     

Preparation,crystal structure and quantum chemical investigation of [Li(NTO) (H2O)]

[Li(NTO)(H₂O)₂] was prepared by mixing the aqueous solution of 3-nitro-1,2,4-triazol-5-one (NTO) and lithium hydroxide. The crystal structure of [Li(NTO)(H₂O)₂] was determined by single crystal diffraction analysis. The crystal is monoclinic, space group P2₁/n with crystal parameters of a = 0.742 0(2) nm, b = 0.344 9(1) nm,c = 2.490 6(3) nm, β= 94.89(1)°, Z = 4,D _c , = 1.799 g cm⁻³,V = 0.635 nm³, μ = 1.591 cm⁻¹, F(000) = 392. The finalR is 0.051. The MNDO MO calculation shows that the coordinate bonds of title compound possess certain extent of covalent character. O₂ atom of NTO anion is bonded to Li atom; the nitro group will be lost first when NTO is decomposed.     

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.     

Refinement of the crystal structure for a new mineral──antimonselite

The crystal structure of a new mineral of the stibnite group, Sb-2Se-3, has been determined. The cell constants, obtained by least-squares calculation from direct θ -value's measurements on the diffractometer are: a =1.158 8(5), b =1.174 4(4), c =0.395 5(2) nm; orthorhombic; V =0.538 23 nm+3; Z =4. The space group is Pbnm. X-ray single crystal data, using Mo K α radiation, were measured on a RIGAKU RASA-5RP automated diffractometer and refined to a final R index of 0.048 1. Sb-2Se-3 is isostructural with Sb-2S-3 and Bi-2S-3. Each Sb(1) atom is six-coordinated by 3 Se(1), 1 Se(2) and 2 Se(3) atoms at distances 0.266 0-0.323 6 nm. Each Sb(2) atom is seven-coordinated by 2 Se(1), 2 Se(2) and 3 Se(3) atoms at distances of 0.258 1- 0.346 7 nm. The crystal structure consists of chains parallel to c or needle axis. The strongest bonds (shortest separations) are within the chains. Many important physical properties of antimonselite (optical, ferroelectric, etc.) are related to its crystal structure.     

Preparation by a rheological phase reaction method and thermal decomposition reaction mechanism of nickelous salicylate tetrahydrate

0　IntroductionInrecentyears,studiesonBinghamfluid ,suchasElec trorheologicalfluid ,areactivelypursued[1 6] .Rheologicaltechniqueshavebeenplayinganimportantroleinsyntheticchem istry .Therheologicalphasereactionmethodisthe processofpreparingcompoundsormaterialsfromasolid liquidrheologicalmixture.Thatis,thesolidreactantsarefullymixedinapropermolarratio ,andmadeupbyaproperamountofwaterorothersolventstoaBinghambodyinwhichthesolidparticlesandliquidsubstanceareuniformlydistributed ,sothattheprodu…     

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.     

Molecule modification and mass deposition induced by the implantation of low energy Fe+ ion beams into amino acids

Fe⁺ ion beams with the energy of 110 keV were implanted into films of L(+)-cysteine (HSCH₂CH(NH₂)COOH). One of the single crystals grown in hydrochloric acid solution with the implanted samples through slow evaporation was structurally characterized by the X-ray crystallography. The crystal is monoclinic, space group C2, with a = 1.8534(4) nm, b = 0.5234(1) nm, c = 0.7212(1) nm, β= 103.72°, V = 0.67965(3) nm³, Z = 4, F(000) = 144.0, D{clac} = 1.763 g · cm⁻³, μ(MoK _a = 1.06 mm⁻¹, T = 293(2) K. R = 0.0379, wR = 0.0835 for 660 observed reflections (I > 2σ(I)). The structural formula of the crystal compound is (CH₂CH(NH₂)NO₂)ClFe (M _r = 180.38 u). Products of heavy ion beam irradiation were purified and it was directly confirmed that the implanted Fe⁺ ions had been deposited in the novel molecules. The same doses of Fe⁺ ion beams of the same energy were implanted into films of L(+)-cysteine hydrochloride monohydrate. FTIR spectroscopy of the implanted samples proved that some of the original molecules were seriously damaged and significant modifications were induced.     

New crystal structure of molecular complex 1-piperidine carboxylate-piperidinium-H<Subscript>2</Subscript>O studied by X-ray single crystal diffraction

Piperidine absorbs CO2 and H2O in air to form a molecular complex： piperidium-l-piperidinecarboxylate-H2O. The structure of the complex was characterized by X-ray single crystal diffraction. The crystal structure was determined to be triclinic, space group P1^-with a=0.648 6（8） nm, b=0.809 200） nm, c= 1.357 1（16） nm, a=96.96706）°, β =102.506（15）°,γ=104.202 05）°, Z=2. The complex is stabilized via five hydrogen bonds between the three components, N-O electrostatic interaction and O-O interaction （electron transfer） betweenl-piperidinecarboxylate and H2O. Due to electron transference of carbamate ion, the oxygen atom in water molecule is strongly negatively charged and the O-H bond is considerably shorter than that of the free molecule of water. The formation of the molecular complex is a reversible process and will decompose upon heating. The mechanism of formation and stabilization is further investigated herein.     

Synthesis, crystal structure and properties of binuclear manganese complex [(bipy)2Mn2(μ-O)(μ-Ac)2(H2O)2](ClO4)2

Binuclear manganese complex [(bipy)₂Mn₂(μ-O)(μ-Ac)₂(H₂O)₂](ClO₄)₂ was synthesized by the reaction of MnAc₃ · 2H₂O with 2,2′-bipyridine in the HAc-NaAc buffer (pH = 4.0). X-ray diffraction result for the single crystal shows that the crystal is monoclinic, space group C₂/C, with a = 3.408 2(7),b = 0.864 4(2),c = 2.174 9(4) nm, β= 105.2∘, V=6.186(2) nm³, Z= 8. There are two very strong peaks of UV-Vis spectrum in the range of 400–600 nm, which are similar to those of Mn catalase and Mn ribonuleotide reductase extracted from organisms. Cyclic voltammogram shows that the complex in CH₃CN undergoes quasi-reversible one-electron reduction and oxidation at E_1/2=1.15V.     

The ring-substituted phthalo-cyanines and its metal com-plexes: Crystal structure of 1,4, 8,11,15,18,22,25-octa-butoxyphthalocyani-natocopper(Ⅱ)

Crystal structure of 1, 4, 8, 11, 15, 18, 22, 25-octa-butoxyphthalocyaninato- copper (Ⅱ) (1) was determined by X-ray diffraction methods. The crystal system is mono-clinic, space group is P2₁/c, Z = 4, a = 1.3741(1) nm, b = 2.6737(1) nm, c = 1.6690(1) nm, β= 101.278(1)°. The steric congestion between the neighbouring butoxyl groups causes the distortion of the ring core of phthalocyanine (Pc) into a saddle shape conformation. In the crystal structure, molecules stack along a axis forming one-dimensional packing structure and there are two molecular overlap types which appear in turn with different distances between molecules, overlap area and angle.     

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…     

Syntheses and lyotropic liquid crystal properties of a series of sandwich-type tungstoarsenates heteropoly compounds with As/W ratio of 4/30

A series of sandwich-type tungstoarsenates heteropoly compounds with As/W ratio of 4/30, Na16[As4W30M4(H2O)2O112]·XH2O (M = Zn,Cu,Co,Ni,Mn and Cd), have been synthesized for the first time and structurally characterized by elemental analysis, IR and 183W NMR spectra. The crystal structure of Na16[As4W30Cu4(H2O)2O112]·63H2O was determined to be a triclinic system, of P1 symmetry, a = 1.2721(3) nm, b = 2.451 6(5) nm, c = 2.6450(5) nm, α= 89.90(3)°,β= 77.32(3)°, γ= 89.96(3)°, 2=2. Using tetrahepty lammonium bromide as a phase transfer reagent, [As4W30Cu4(H2O)2O112]16- was transferred from aqueous solution to organic phase (benzene), and the heteropolyanion lost the coordination water molecules to form the coordination-unsaturated ion. After lactic acid was added to the benzene solution, the coordination-saturation was recovered. By esterification reaction between lactic acid and cholesterin, the latter was attached to the heteropolyanion indirectly. Therefore, a new type of lyotropic liquid crystal was obtained, which was characterized by a polarimicroscope, DSC and variable temperature wide-angle X-ray diffraction.     

3-(β-二茂铁基乙基)-2-(二茂铁甲酰基)呋喃的合成、表征及晶体结构

在钌化合物RuH2(CO)(PPh3)3的催化作用下,2-(二茂铁甲酰基)呋喃与二茂铁乙烯反应,合成了3-(β-二茂铁基乙基)-2-(二茂铁甲酰基)呋喃,其结构经元素分析、核磁共振谱和质谱得到表征.应用X射线衍射分析方法确定了产物的晶体结构和结构参数.     

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.     

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.     

［Ni(phen) 3］2［Ni(PO4)2(H2PO4)6(OH)6(MoO2)12］的合成和晶体结构

利用中温水热技术合成一种新型还原型钼磷酸盐： ［Ni(phen) ₃］₂［Ni(PO₄)₂(H₂PO₄)6(OH)₆(MoO₂)₁₂］(phen: 邻菲啰啉), 并通过单晶X射线衍射技术测定了该化合物的晶体结构.该化合物属于三斜晶系, P1空间群, 晶胞参数: a=1.404 2(3) nm, b=1.405 0(3) nm, c=1.408 2(3) nm, α=74.53(3)°, β=74.72(3)°,γ=74.81(3)°, V=2.527 6(9) nm3, Z=1, R1=0.076 2, wR2=0.168 6.     

New Early Triassic paleomagnetic data from Huangben section, Guangdong and its tectonic implications

Continent China is composed of several blocks of variable sizes during different geological times, inwhich South China Block is composed of three tectonic units: Yangtze Block, Jiangnan Fold Belt and Southeast China Coastal Fold Belt (Fig. 1(a)), the last…     

Fabrication and Photocatalytic Characteristics of TiO2 Films on Silicon Substrates

Silicon ( 111 ) and Silicon (100) have been employed for fabrication of TiO2 films by metal organic chemical vapor deposition (MOCVD). Titanium (Ⅳ) isopropoxide (Ti[O (C3H7)4 ])was used as a precursor. The as-deposited TiO2 films have been characterized with Field emission scanning electron microscopy (FE-SEM), X ray diffraction (XRD) and atomic force microscopy (AFM). The photocatalytic properties were investigated by decomposition of aqueous orange Ⅱ. The crystalline and structural properties of TiO2 film had crucial influences on the photodegradation efficiency. For MOCVD in-situ deposited films on Si substrates, thephotoactivities varied following a shape of “M”: At lower (350 ℃ ) middle (500 ℃) and higher (800 ℃) temperature of deposition, relative lower photodegradation activities have been observed. At 400 ℃ and 700 ℃ of deposition, relative higher efficiencies of degradation have been obtained, because one predominant crystallite orientation could be obtained as deposition at those two temperatures, especially a single anatase crystalline TiO2 film could be obtained at 700 ℃ growth.