(Z)-1[2-(苯基二溴化锡基)乙烯基]-1-环己醇的合成及晶体结构

报道了标题化合物〔C14H18Br2OSn〕的合成及晶体结构。该晶体属于单斜晶系，空间点群为P21/c，晶胞参数a=11.711(2)，b=9．114（2），c=16．864（3）A，β=102.94（1）°，V=1604.55（0）A3，Mr=480．78，Z=4，Dc=1．99g／cm3，u=65．20cm－1，F（000）=919，R=0．050，Rw=0．050．晶体结构由直接法解出。标题化合物分子中的锡原子被配体的2个碳、2个溴和1个氧原子配位，配位原子呈畸变的三角双锥构型，环已基为椅式构象，五员杂环为信封构象。

Crystal structure and mechanism of (Z)-1-[2-(phenyl-bromide-chloride)vinyl]-1-cyclohexanol

The crystal structure and mechanism of the title molecule are described. This crystal is orthorhombic, belonging to space group PC21/B with a=1,002 1(2) nm, b=1.483 0(3) nm, c=2.173 6(4) nm, V=3.230 39(2) nm(3), Z=2, D-c=1.80 g/cm(3), R=0.069 3. The structure was solved by direct method. The tin atom of the title compound exists in two distorted-trigonal-bipyramidal geometry, defined by two carbon, one bromide, one chloride and one oxygen atoms leading to a five-membered chelate ring. In the structure, the five-membered ring containing the intermolecular O-->Sn has a half chair conformation.

Synthesis and chemical properties of [Z]-1-[2-(triaryl stannyl)vinyl]cyclooctanol

The compounds of [Z]-1-[2-(triphenyl stannyl) vinyl] cyclooctanol (1) and [Z]-1-[2-(tri-p-tolyl stannyl) vinyl] cyclooctanol (2) were synthesized by the reactions of triphenyltin hydride and tri-p-tolyltin hydride with 1-ethynyl cyclooctanol. The crystal structure of compound 1 was determined. The reactions of compound 1 and 2 with IC1, Br-2, I-2 formed nine organotin halides. The organotin oxide or hydroxide were prepared by the reactions of [Z]-1-[2-(phenyl dibromo stannyl) vinyl] cyclooctanol (6) and [Z]-1-[2-(diphenyl monobromo stannyl) vinyl] cyclooctanol (5) with KOH. Three complexes were obtained by the reactions of [Z]-1-[2-(phenyl diiodide stannyl) vinyl] cyclooctanol (8) with three ligands (2,2'-bipyridyl,5-nitro-1,10-phenanthroline,8-Hydroxyquinoline). The sixteen new compounds synthesized in this paper were characterized by means of elemental analysis, IR, H-1 NMR. The reaction mechanism of triphenyltin hydride and tri-p-tolyltin hydride with 1-ethynyl cyclooctanol were also proposed.

[Z]-1-[2-(三芳基锡基)乙烯基]环辛醇的合成和性质

本文用三苯基氢化锡、三对甲苯基氢化锡作为锡氢化试剂与1-乙炔基环辛醇进行反应,合成了两个有机锡化合物:[Z]-1-[2-(三苯基锡基)乙烯基]环辛醇(1)和[Z]-1-[2-(三对甲苯基锡基)乙烯基]环辛醇(2),并测定了1的晶体结构.1和2分别与ICl,Br_2,I_2反应,得到六个有机锡一卤化物和三个有机锡二卤化物(3～11).有机锡二卤化物6和一卤化物5与KOH乙醇溶液反应,分别得到相应的锡氧化物和锡氢氧化物(12,13).有机锡二卤化物8分别与含氮双齿配体[2,2-联吡啶(Bipy),5-硝基-1,10-邻菲罗啉(Nphen),8-羟基喹啉(Oxin)]反应,得到三个相应的配合物(14～16).十六个新化合物通过元素分析、锡含量测定、IR、~1HNMR测定对其结构进行了表征,同时提出了1和2的生成反应历程.

Z=105质量数为259的新同位素的合成和鉴别(英文)

利用 1 2 0MeV的2 2 Ne离子束轰击2 41　Am靶 ,通过2 41　Am(2 2 Ne ,4n) 2 5 9　Db反应合成了一个Z =1 0 5,质量数为 2 59的新同位素 .反应产物是用氦喷嘴技术和转动轮装置传输收集的 .借助一系列金硅面垒探测器探测到了反应产物及其子核的α衰变 .新同位素的原子序数Z和质量数A是借助该同位素和已知的2 5 5 　Lr核之间的遗传关系得到了确定的鉴别 .新同位素2 5 9　Db的测量半衰期为 (0 51± 0 1 6)s;它的α粒子能量为 9 4 7MeV .由本实验导出的2 5 9　Db的Qα 值同理论预言结果能够较好地符合

0.4-1.2A GeV能区重离子碰撞中的直接流系统性研究

直接流是研究重离子碰撞动力学演变和压缩形成的高密核物质性质很好的探针，本论文系统地研究了0.4、0.8和1.16A GeV的Ni+Ni和Pb+Pb碰撞中的直接流。实验是在德国重离子研究中心(GSI)的FOPI探测装置上完成的。论文中，简单总结了中高能区重离子碰撞的现状和描述集体流的主要理论模型，介绍了FOPI探测系统，给出了详细的实验数据分析过程，对所得到的物理结果进行了讨论。本论文工作的重点如下：基于FOPI系统的实验数据，发展了一套质量相关(Z=1离子)的直接流的提取方法。提取了各碰撞系统出射P、D和T粒子在不同碰撞中心度下的微分直接流和积分直接流。研究了P、D和T的直接流对碰撞中心度、系统尺寸和碰撞能量的依赖性，以及对核物质状态方程的敏感性。结果表明：直接流敏感地依赖于碰撞中心度，近中心碰撞具有更强直接流信号；对于轻重两种系统，用常用的AP1/3+AT1/3系数对积分直接流进行了标度，观察到一定的标度性，但不能完全标度；通过研究直接流对碰撞能量的依赖性发现，在0.4－1.2A GeV能区内，随能量升高，直接流在已经达到了饱和，并开始下降，并且P、D和T的变化趋势相同。实验数据与输运模型IQMD计算比较发现，直接流的变化趋势和最大密度变化趋势相同，说明直接流是核物质压缩程度的一个良好探针。计算得到的P、D和T微分和积分的V1值表明，与质量相关的直接流，无论是微分值还是积分值都敏感依赖于模型中EoS参数。比较发现，不同碰撞能量下，重的Pb+Pb系统的数据和软的EoS符合很好，说明核物质不可压缩系数在210 MeV附近，这与文献中的结果相吻合，说明与质量相关的直接流是EoS的敏感探针。对于轻Ni＋Ni系统，目前的IQMD还不能重现数据，但其趋向于硬的EoS，需要发展描述碰撞过程更为精细的理论模型。数据整体趋势表明，随者系统变重，中子比例的增加，EoS变软，难以给出同一组IQMD参数来同时解释全部的实验数据。对于所研究的碰撞系统，比较中心快度区斜率行为时发现，P、D和T的直接流与出射粒子质量数呈线性关系，并且出射粒子的积分直接流可以很好的用常数(A+1)/2进行标度。如果出射粒子的直接流用IQMD计算的核阻止进行归一，归一后的直接流与碰撞能量成正比。这证明核阻止与直接流有线性关联，反映了核阻止对于碰撞中核物质达到的最高密度起决定性的作用。论文工作的另一部分是完成了FOPI探测装置中飞行时间探测器的升级工作。研制了新型的玻璃MMRPC，完成了性能的批量测试，并研究了该探测器的高计数率行为。测量结果显示，在实验计数率(0.1 kHz/cm2)条件下，MMRPC时间分辨达到75 ps，探测效率达到98％。当计数率达到3－5 kHz/cm2时，时间分辨和探测效率降至约110 ps和75％。高计数率探测效率变差的幅度可以用DC模型进行解释，然而时间分辨的变化幅度用DC模型难以解释

Crystal structures of EtEDTB center dot 1.4C(2)H(5)OH center dot 5H(2)O and H4EtEDTB(ClO4)(4)center dot C2H5OH (EtEDTB=N, N, N ', N '-tetrakis[2-(1-ethylbenzimidazolyl)methyl]-1,2-ethanediamine)

The crystal structures of EtEDTB.1.4C(2)H(5)OH.5H(2)O 1 and H4EtEDTB(ClO4)(4).C2H5OH 2 (EtEDTB = N, N,N',N'-tetrakis[2-(1-ethylbenzimidazolyl)methyl]-1,2-ethanediamine) have been determined by single-crystal X-ray diffraction method. Compound 1 crystallizes in the space group P(1) over bar with a = 11.489(2), b = 11.866(3), c = 12.002(3) Angstrom, alpha = 97.47(2), beta = 114.564(13), gamma = 114.11(2)degrees, V = 1266.6(5) Angstrom(3), Z = 1, M-r = 847.48, D-c = 1.111 g/cm(3), F(000) = 456 and mu(MoKalpha) = 0.076 mm(-1). A total of 5207 reflections were measured for 1, of which 4323 were independent. The structure of 1 was solved by direct methods and refined by full-matrix least-squares technique to the final R = 0.0706 and wR = 0.1802 for 1318 observed reflections with I > 2sigma(I). In the structure of 1, centrosymmetric EtEDTB molecules are linked by hydrogen bonds through water and ethanol to form 2-dimensional network. Compound 2 crystallizes in the space group C2/c with a = 24.260(5), b = 13.040(3), c = 17.680(4) Angstrom, beta = 97.50(3)degrees, V = 5545.2(2) Angstrom(3), Z = 4, M-r = 1140.80, D-c = 1.366 g/cm(3), F(000) = 2384 and mu(MoKalpha) = 0.289 mm(-1).

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.

高温高压下Z轴水晶的电导率实验研究

电导率测量的过程历经了从直流-交流-阻抗谱的过程，已经为地球物理学家借助于高温高压手段研究固体深部物质电学性质所广泛认同的。本文首先介绍了阻抗谱法测定水晶电导率的实验原理，进而采用该方法在10^-1～10^6Hz的频率范围以及1．0—4．0GPa和823—1073K条件下，借助于YJ-3000t紧装式六面顶高压设备对沿Z轴方向生长的水晶进行了的电导率实验就位测量。实验结果表明：在选择的频率范围，样品的复阻抗的模和相角都对频率具有很强的依赖性；随着温度的升高，电阻迅速降低，电阻率降低，电导率增大；在压力1．0—4．0GPa，其活化焓分别为：0．8548eV、0．8320eV、0．8172eV、0．7834eV，独立于温度的指前因子分别为：1．003S／m、1．778S／m、3．082S／m、6．987S／m，活化焓随着压力的升高而降低，指前因子随着压力的升高而增大。

The near wall velocity measurements in microchannels with different diameter particles by microPIV/PTV. 8th International symposium on PIV

In near wall measurements with microPIV/PTV, whether seeding particles can be effectively used to detect local fluid velocity is a crucial problem. This talk presents our recent measurements in microchannels [1][2]. Based on measured velocity profiles with 200nm and 50nm in pure water, we found that the measured velocity profiles are agreed with the theoretical values in the middle of channel, but large deviations between measured data and theoretical prediction appear close to wall (0.25mm <z<1.5mm). Moreover, these deviations depend on the particle sizes. Considering the volume illumination [3] and particle physical behavious [4], we try to analysis the influence of focal plane thickness and particle concentration distribution near wall on the velocity deviation appeared in shear flows.

武汉月湖沉积物中硅藻的垂直分布与水质变化

采用活塞取样器采集了月湖湖中央2处钻孔沉积物,分析了其中硅藻种类与密度的垂直变化,同时采用210Pb/137Cs推测沉积物的沉积速率,并进行了总有机质、生物硅含量分析,以了解月湖各个不同年代的水质变化。结果表明,2个柱状沉积物中硅藻的优势属为:小环藻属、直链藻属、舟形藻属、Cyclostephanos属。Z-1钻孔优势种为:梅尼小环藻、颗粒直链藻、Navicula porifera、Cyclostephanos tholifomis。Z-2钻孔中优势种为:梅尼小环藻、颗粒直链藻、舟形藻、Cyclostep

CYCLIC PEPTIDE HEPATOTOXINS FROM FRESH-WATER CYANOBACTERIAL (BLUE-GREEN-ALGAE) WATERBLOOMS COLLECTED IN CENTRAL CHINA

Toxic cyanobacteria (blue-green algae) waterblooms have been found in several Chinese water bodies since studies began there in 1984. Waterbloom samples for this study contained Anabaena circinalis, Microcystis aeruginosa and Oscillatoria sp. Only those waterblooms dominated by Microcystis aeruginosa were toxic by the intraperitoneal (i.p.) mouse bioassay. Signs of poisoning were the same as with known hepatotoxic cyclic peptide microcystins. One toxic fraction was isolated from each Microcystis aeruginosa sample. Two hepatotoxic peptides were purified from each of the fractions by high-performance liquid chromatography and identified by amino acid analysis followed by low and high resolution fast-atom bombardment mass spectrometry (FAB-MS). LD50 i.p. mouse values for the two toxins were 245-mu-g/kg (Toxin A) and 53-mu-g/g (Toxin B). Toxin content in the cells was 0.03 to 3.95 mg/g (Toxin A) and 0.18 to 3.33 mg/kg (Toxin B). The amino acid composition of Toxin A was alanine [1], arginine [2], glutamic acid [1] and beta-methylaspartic acid [1]; for Toxin B it was the same, except one of the arginines was replaced with a leucine. Low- and high-resolution FAB-MS showed that the molecular weights were 1,037 m/z (Toxin A) and 994 m/z (Toxin B), with formulas of C49H76O12N13 (Toxin A) and C49H75O12N10 (Toxin B). It was concluded that Toxin A is microcystin-RR and Toxin B is microcystin-LR, both known cyclic heptapeptide hepatotoxins isolated from cyanobacteria in other parts of the world. Sodium borohydride reduction of microcystin-RR yielded dihydro-microcystin-RR (m/z = 1,039), an important intermediate in the preparation of tritium-labeled toxin for metabolism and fate studies.

一种生长纳米折叠结构有源区外延片的方法

一种制备具有纳米折叠有源区结构外延片的方法，其特征在于，包括如下步骤:步骤1:先制备AlxInyGazN材料模版，其中x+y+z＝1，0≤x，y，z≤1;步骤2:利用纳米加工技术，在AlInGaN材料模版上制作AlInGaN纳米柱阵列，该AlInGaN纳米柱阵列包括多个AlInGaN纳米柱;步骤3:在AlInGaN纳米柱阵列、AlInGaN纳米柱和AlInGaN材料模版的上表面生长具有纳米折叠结构的有源区层;步骤4:在具有纳米折叠结构的有源区层上生长带有纳米孔阵列的p型GaN层，该p型GaN层填满AlInGaN纳米柱阵列的缝隙，完成外延片的制作。