A novel dimer - Heteropolytungstate with a vanadium atom as the centre - Synthesis and structural characterization of (H3O)(4)[VW12O40Na (H2O)(4)](2)

A novel dimer-tungstovanadate, (H3O)(4)[VW12O40Na (H2O)(4)](2), was hydrothermally synthesized and structurally characterized by single crystal X-ray diffraction, IR spectra, TGA-DSC thermal analysis and polarograpy. The yellowish crystal crystallized in the triclinic system, space group P1, a = 1.464 5(3) nm, b = 1.468 6(3) nm, c = 1.411 1(3) nm, alpha = 111.82(2)degrees, beta = 93.17(3)degrees, gamma = 117.47(3)degrees, V = 2.210 6(8) nm(3), Z = 1, D-c = 4.552 g . cm(-3), lambda (Mo K alpha) = 0.071 073 nm, mu = 31.402 mm(-1) F(000) = 2 6481 R = 0.078 0. The title compound consists of two Keggin structure units linked together with two hydrated sodium cations to form a dimer with a porous structure with the pore dimension of 0.766 nm X 0.778 5 nm.

环戊二烯—12-钼硅杂多四丁基铵电荷转移盐的合成、表征与晶体结构

以环戊二烯与 1 2 钼硅杂多四丁基铵为原料 ,采用光化学法合成了一种新型电荷转移盐 (Bu4N) 4(C5 H6 ) [HSiMoVI11MoVO40 ]。用元素分析、IR、CV、固体漫反射电子光谱、ESR进行了表征。X 射线晶体结构测定其晶体属三斜晶系 ,空间群P1 ,晶胞参数a =1 4.347(3) ,b =1 4.42 3(3) ,c =2 7.1 5 8(5 ) ,α =96 .90 (3) ,β =1 0 4.1 8(3) ,γ =98.2 0 (3)° ,V =5 32 2 (2 ) 3,Z =2 ,Mr=2 85 5 .30 ,Dc=1 .782 g·cm-3,F(0 0 0 ) =2 86 0 ,R =0 .0 71 9,wR =0 .1 983。标题化合物由 1个环戊二烯、4个Bu4N+阳离子和 1个 [SiMoVI11MoVO40 ]4 -阴离子构成。

Studies on the structure of tricyclohexyltin-2-(1,2-dithioethylene)methylene-3-oxo-5-aryl-4-pentenicate

Three title compounds were prepared and the structure of title compound 2 was characterized by IR, H-1 NMR, C-13 NMR, Sn-119 NMR spectroscopy and the crystal structure of compound 2a was determined by X-ray analysis with the final R indices[I >2 sigma (I)] R-1 = 0.0350 and R-2,R-omega = 0.0888. The crystal of compound 2a belongs to triclinic system, space group P1 with a = 1.0598(6) nm, b = 1.307 4(10) nm, c = 1.378 6(10) nm, alpha = 62.666(7)degrees, beta = 72.530(2)degrees, gamma = 80. 680(2)degrees, V = 1.618 0 nm(3), D-x = 1. 444 g (.) cm(-3), Z = 1, F (000) = 728. The bond length of Sn1-O1 is 0. 2076 nm and Sn1 . . . O2 distance is 0.301 3 nm. The coordination about the tin atom can be considered as a distorted tetrahedral. The detail values of H-1 NMR, C-13 NMR, Sn-119 NMR, (2)J(119Sn-1H) and J(119Sn-13C) were obtained. delta (119Sn) = 23.836, (2)J(119Sn-1H) = 88.0 Hz, (1)J(119Sn-13C) = 347.1 Hz, (2)J(119Sn-13C) = 45.6 Hz.

H_8[P_4W_(14)O_(58)Na_4(H_2O)_(20)]·16H_2O的合成、晶体结构与性质

用水热法合成了 H8[P4 W14 O58Na4 (H2 O) 2 0 ]· 16 H2 O,通过 X射线单晶衍射、元素分析和IR进行了结构表征 ,用 TG- DTA研究了热稳定性 .晶体属三斜晶系 ,P1空间群 ,a=1.1379(2 )nm,b=1.36 32 (3) nm,c=1.6 2 71(3) nm;α=78.2 0 (3)°,β=71.2 0 (3)°,γ=71.6 2 (3)°;V=2 .2 52 5(8) nm3 ,Z=1,Mr=4 374 .38,Dc=3.2 2 5mg/ cm3 ,μ=18.0 0 7mm-1,F(0 0 0 ) =1972 ,R=0 .0 74 2 ,Rw=0 .2 0 0 4 .标题化合物的阴离子是由两个 PW7O2 9Na2 (H2 O) 10 亚单元通过与两个磷原子上键合的氧连接而成 ,分子内形成了一个 0 .6 6 14nm× 0 .3189nm的微孔.

新型笼状钼磷超分子化合物的水热合成与晶体结构

用水热法首次合成了含有２ 种有机胺的新型笼状钼磷超分子化合物〔NH3(CH2)6NH3〕7〔NH3(CH2)2NH3〕2(H3O)6〔P2Mo5O23〕4·11H2O，并通过元素分析、红外和X-射线单晶衍射法进行了结构表征．晶体属三斜晶系，空间群p1杂多阴离子中的每个〔P2Mo5O23〕6-是由5 个MoO6八面体和两个PO4四面体键合而成，其中Mo，P原子成一个畸变五角双锥构型.

Synthesis, properties and crystal structure of organic-inorganic radical salt (DBTTF)(6)HPMo12O40 center dot 2H(2)O

Organic-inorganic radical salt (DBTTF)(6)PMo12O40 . 2H(2)O was synthesized by electrocrystallization and characterized by IR spectrum, electronic spectrum and ESR technology, Its magnetic property, conductivity and crystal structure were determined. The title compound crystallized in a triclinic system with P1 space group, a = 1.378 7(7), b = 1.420 4 (2), c = 1.570 2(2) nm, alpha = 104.57(1)degrees, beta = 103.41(2)degrees, gamma = 95.80(2)degrees, V = 2.853(2) nm(3) Z = 1 and a final R = 0.072 7.

Syntheses and structures of Na-2[Zn-II(ida)(2)].7H(2)O and Na-4[Hg-II(nta)(2)].7H(2)O

The title complexes were synthesized and the crystal structures of their salts were determined by single-crystal X-ray structure analyses. Na-2[Zn-I(ida)(2)]. 7H(2)O: Triclinic, P1, a=0.523 4(2) nm, b=0.897 10(10) nm, c=1.069 10(10) nm, alpha=85.910(10)degrees, beta= 76.380(10)degrees, gamma=83.52(2)degrees, V=0.484 2(2) nm(3), Z=1. The complex anion [Zn-I (ida)(2)](2-) has a pseudo-octahedral structure in which the two N atoms: are in a trans configuration. Na-4[Hg-I(nta)(2)]. 7H(2)O: Monoclinic, C-c, a = 1.795 0(4) nm, b = 0.892 9(2)nm, c = 1.575 4(2) nm, beta = 92.78 (3)degrees, V = 2.526 2(9) nm(3), Z = 4. The complex anion [Hg-I (nta)(2)](4-) has a pseudo-bicapped-octahedral structure in which the two N atoms are in a trans configuration.

{[Sm_2(Gly)_6(H_2O)_4](ClO_4)_6(H_2O)_5}_n的合成和晶体结构

本文合成了标题配合物,对其红外光谱进行了研究.测定了配合物的晶体结构,结果表明,晶体属三斜晶系,P1空间群,单胞参数:α=11.549(2)(?),b=14.122(3)(?),c=15.654(?),α=97.01(2)°,β=102.70(2)°,γ=105.43(2)°,V=2355.94(0.87)(?)~3,Z=2.晶体结构是采用Patterson法和差值Fourier合成解出.经全矩阵最小二乘法修正,最后偏差因子R=0.0337,R_w=0.0364.晶体中甘氨酸与Sm原子的结合方式有三种:第一种甘氨酸的羧基离子以螯合桥式与Sm原子配位;第二种甘氨酸以羧基桥式与同一单元的两个Sm原子配位;第三种甘氨酸以酸基桥式连结两个相邻单元中的相邻Sm原子而形成一维无限长链结构.此外,每个Sm原子还与两个水分子成键,其配位数为9.

CRYSTAL-STRUCTURE OF 1, 10-DECANEDIAMMONIUM TETRACHLOROZINCATE

The crystal structure of the title compound has been determined from single crystal X-ray diffraction. The complex crystallizes in the triclinic space group P1 with Z=2. Lattice parameters are: a = 0.7296(1), b = 1.0110(3), c = 1.2814(4) nm; alpha = 90.84(2), beta = 101.17(2), gamma = 92.52(2)-degrees. Intensity data were collected on a Nicolet R3M/E four-circle diffractometer using MoK alpha (lambda = 0.071073 nm) radiation. The structure was solved by Patterson and Fourier techniques and refined by least-squares techniques to R = 0.065. The structure of the complex consists of tetrahedral ZnCl42- anions which form a two-dimensional sheets. Tetrahedral ZnCl42- anions are sandwiched between two hydrocarbon layers which consist of [NH3(CH2)10NH3]2+ cations. Each [NH3(CH2)10NH3]2+ group is in a gauche bond between C atoms near NH3 polar heads.

四氯合锌酸1,10-癸二铵配合物的晶体结构

合成了[NH_3(CH_2)_(10)NH_3]ZnCl_4配合物(简称DDAZn),用X射线衍射法研究了它的晶体结构,晶体属三斜晶系,空间群为P1,晶胞参数为:α=0.7296(1),b=1.0110(3),c=1.2814(4)nm;α=90.84(2),β=101.17(2),γ=92.52(2)°;Z=2.该配合物为层型结构.由单个四面体阴离子ZnCl_4~(2-)构成的阴离子层被夹在烷基铵阳离子层之间,形成“夹心面包”型体系.在层之间的烷基铵链在垂直于层的方向上倾斜排列.

η~6—芳烃希土有机配合物的合成、结构及性能研究——Ⅰ.Sm(η~6—C_6H_6)(AlCl_4)_3的合成及晶体结构

经过铝粉加热活化的AlCl_3与SmCl_3在苯中反应,得到了Sm(η~6—C_6H_6)(AlCl_4)_3·C_6H_6单晶.其晶体属于三斜晶系,P1空间群,晶胞参数a=9.456(2)(?),b=9.765(3)(?),c=16.776(4)(?),α=96.00(2)°,β=93.76(2)°,γ=111.66(2)°,V=1422.55(?)~3,Z=2.晶体结构是采用Patterson和Fourier合成法解出的,所有非氢原子的坐标及各向异性热振动参数经块矩阵最小二乘法修正,最后偏离因子R=0.031,R_ω=0.035.分子结构中,中心离子Sm(Ⅲ)与六个Cl原子及一个苯环上的六个C原子成键.Sm-C键平均距离2.92(?),Sm-Cl平均距离2.83(?).与希土相连的六个Cl原子,其中之五构成平面五边形,整个分子呈大致的五角双锥形.

一种新型稀土苯甲酸铽配合物的合成、表征及其晶体结构

本文报道一种新型稀土苯甲酸配合物,[Tb(C_7H_5O_2)_3(C_7H_6O_2)(H_2O)]_2的合成。用元素分析、DTA、TG、DTG和IR光谱对其性质进行了表征,并测定了其晶体结构。晶体属三斜晶系,空间群为P1,Z=1。晶胞参数为:a=9.148(1),b=11.460(2),c=13.506(2)A;α=112.76(1),β=91.83(1),γ=91.99(1)°;V=1303.3(4)A~3。稀土离子形成九配位的单帽正方反棱柱型配合物,稍有崎变。

STUDY OF BIMETALLIC COMPLEXES OF RARE-EARTH LITHIUM - SYNTHESIS AND CRYSTAL-STRUCTURE OF THE (LACL)DME(MU-2-CL)5(MU-3-CL) (LA.DME)LI(THF)2

The reaction between LaCl_3 and LiCl in THF at room temperature, with hexane as precipitant and glycol dimethyl ether as complexing agent, has been studied. A complex with the composition of (LaCl)DME(μ_2-Cl)_5(μ_3-Cl)(La·DME)Li(THF)_2 has been synthesized, its structure was studied by single crystal X-ray diffraction technique. The diffraction intensities were collected at about —100℃. The complex belongs to the triclinic space group P1 with α=11.123(3), 6=16.564(5), c=8.653(3)A, α=95.16(3), β=...

Isolation and mapping of telomeric pentanucleotide (TAACC)(n) repeats of the pacific whiteleg shrimp, Penaeus vannamei, using fluorescence in situ hybridization

To develop genetic and physical maps for shrimp, accurate information on the actual number of chromosomes and a large number of genetic markers is needed. Previous reports have shown two different chromosome numbers for the Pacific whiteleg shrimp, Penaeus vannamei, the most important penaeid shrimp species cultured in the Western hemisphere. Preliminary results obtained by direct sequencing of clones from a Sau3A-digested genomic library of P. vannamei ovary identified a large number of (TAACC/GGTTA)-containing SSRs. The objectives of this study were to (1) examine the frequency of (TAACC)(n) repeats in 662 P. vannamei genomic clones that were directly sequenced, and perform homology searches of these clones, (2) confirm the number of chromosomes in testis of P. vannamei, and (3) localize the TAACC repeats in P. vannamei chromosome spreads using fluorescence in situ hybridization (FISH). Results for objective I showed that 395 out of the 662 clones sequenced contained single or multiple SSRs with three or more repeat motifs, 199 of which contained variable tandem repeats of the pentanucleotide (TAACC/GGTTA),, with 3 to 14 copies per sequence. The frequency of (TAACC)n repeats in P. vannamei is 4.68 kb for SSRs with five or more repeat motifs. Sequence comparisons using the BLASTN nonredundant and expressed sequence tag (EST) databases indicated that most of the TAACC-containing clones were similar to either the core pentanucleotide repeat in PVPENTREP locus (GenBank accession no. X82619) or portions of 28S rRNA. Transposable elements (transposase for Tn1000 and reverse transcriptase family members), hypothetical or unnamed protein products, and genes of known function such as 18S and 28S rRNAs, heat shock protein 70, and thrombospondin were identified in non-TAACC-containing clones. For objective 2, the meiotic chromosome number of P. vannamei was confirmed as N = 44. For objective 3, four FISH probes (P1 to P4) containing different numbers of TAACC repeats produced positive signals on telomeres of P. vannamei chromosomes. A few chromosomes had positive signals interstitially. Probe signal strength and chromosome coverage differed in the general order of P1 > P2 > P3 > P4, which correlated with the length of TAACC repeats within the probes: 83, 66, 35, and 30 bp, respectively, suggesting that the TAACC repeats, and not the flanking sequences, produced the TAACC signals at chromosome ends and TAACC is likely the telomere sequence for P. vannamei.

编码四种甲壳动物蜕皮抑制激素的部分cDNA的克隆和序列分析

本文分别提取了中国对虾、中华绒螯蟹、鹰爪虾和蓝对虾的眼柄总RNA。用无DNA污染的眼柄总RNA为模板，根据日本对虾的MIH设计兼并引物P1和P2，进行RT－PCR扩增，在适宜的反应条件下，均分别得到一特异性的产物。以蓝对虾基因组DNA为模板的PCR扩增也能得到一与特异性cDNA片段大小相似的特异性的DNA片段。分别将这些片段亚克隆到载体中进行测序，测得中国对虾特异性cDNA片段由203个碱基组成，中华绒螯蟹、鹰爪虾、蓝对虾的特异性cDNA片段及蓝对虾的特异性DNA片段由215个碱基组成，其中蓝对虾特异性cDNA与由蓝对虾的基因组DNA扩增得到的特异性DNA片段的碱基序列几乎完全相同。利用互联网上的在线工具Fasta3查找这些cDNA推定的氨基酸序列的相似序列，可以发现大量的甲壳动物的CHH家族的神经肽与它们相似。在所有的相似序列中，分别由中国对虾、中华绒螯蟹、鹰爪虾和蓝对虾的特异性cDNA片段推定的氨基酸序列与蜕皮抑制激素（MIH）的相似度最高，这一结果提示分别由中国对虾、中华绒螯蟹、鹰爪虾和蓝对虾的眼柄特异性cDNA片段推定的氨基酸序列可能是这四种甲壳动物的MIH片段。根据核苷酸数据和氨基酸数据，比较这四种甲壳动物的MIH以及已发表的六种MIH之间的相似度，同时分析这十种MIH的系统进化关系，结果是蓝对虾、鹰爪虾和中华绒螯蟹的MIH相似性较高，亲缘关系较近，这与物种的系统演化不相符。