The use of half-sandwich iridium dithiolate and diselenolate complexes, Cp*Ir(L)(ER)(2) (L = CO, PMe3, PPh3; ER = SPh, SePh, SeMe), for the synthesis of heterodimetallic compounds. The molecular structure of Cp*Ir(CO)(mu-SePh)(2)[Mo(CO)(4)]

Carbonyl-iridium half-sandwich compounds, Cp*Ir(CO)(EPh)(2) (E = S, Se), were prepared by the photo-induced reaction of Cp*Ir(CO)(2) with the diphenyl dichalcogenides, E2Ph2, and used as neutral chelating ligands in carbonylmetal complexes such as Cp*Ir(CO)(mu-EPh)(2)[Cr(CO)(4)], Cp*Ir(CO)(mu-EPh)(2)[Mo(CO)(4)] and Cp*Ir(CO)(mu-EPh)(2)[Fe(CO)(3)], respectively. A trimethylphosphane - iridium analogue, Cp*Ir(PMe3)(mu-SeMe)(2)[Cr(CO)(4)], was also obtained. The new heterodimetallic complexes were characterized by IR and NMR spectroscopy, and the molecular geometry of Cp*Ir(CO)(mu-SePh)(2)[Mo(CO)(4)] has been determined by a single crystal X-ray structure analysis. According to the long Ir...Mo distance (395.3(1) Angstrom), direct metal-metal interactions appear to be absent. (C) 1998 Elsevier Science S.A. All rights reserved.

Synthesis and characterization of a new double-cubane Mo-Fe-S cluster compound, [NEt(4)](3)[Mo2Fe6S8(mu-OMe)(3)(SPh)(3)Cl-3]

The new double-cubane cluster compound [NEt(4)](3)[Mo2Fe6S8(mu-OMe)(3)(SPh)(3)Cl-3] is synthesized from (NH4)(2)MoS4, FeCl3, Fe powder, S powder, NaSPh and NEt(4)Br in MeOH-DMF, its crystal structure is determined by X-ray crystallography, and results of XPS indicate a valence state of +4 for Mo.

Syndiospecific polymerization of styrene with multi-nuclear titanium complexes

Two multi-nuclear titanium complexes [Ti(eta(5)-Cp-*) Cl(mu-O)](3) ( 1) and [(eta(5)-(CpTiCl)-Ti-*)(mu-O)(2)(eta(5)-(CpTi)-Ti-*)(2)(mu-O)(mu-O)(2)](2)Ti (Cp-* = C5Me5) ( 2) have been investigated as the precatalysts for syndiospecific polymerization of styrene. In the presence of modified methylaluminoxane ( MMAO) as a cocatalyst, complexes 1 and 2 display much higher catalytic activities towards styrene polymerization, and produce the higher molecular weight polystyrenes with higher syndiotacticities and melting temperatures ( T-m) than the mother complex (CpTiCl3)-Ti-* does when the polymerization temperature is above 70 degrees C and the Al/Ti molar ratio is in the low range especially.

尖吻蝮蛇蛇毒出血毒素DaHT-3的纯化与性质

通过Sephadex G-75,DEAE-Sephadex A-50,Sephadex G-200和两次PBE聚焦层析,从尖吻蝮蛇(Dienagkistrodon acutus)蛇毒中纯化到一个分子量为56 000的出血毒素(DaHT-3),经氨基酸组成测定计算,由487个氨基酸残基组成。此成分在SDS-PAGE上显示出一条均一的蛋白染色带,用等电聚焦电泳测定,其pI为5.50。该出血成分的最小出血剂量是2.6#mu#g,具有蛋白水解酶活力,其活力为3.68,但没有精氨酸酯酶和磷脂酶A_(2)活力。用红外光谱仪研究DaHT-3在溶液中酰胺Ⅰ带的吸收谱,该毒素含有31.8%的#alpha#螺旋、56.1%的#beta#折叠和12.1%的转角;当加入EDTA螯合剂去除金属离子后,它们的#alpha#螺旋、#beta#折叠、转角和无规卷曲分别变为11%、26.4%、46.2%和16.5%,而出血活力和蛋白水解酶活力均丧失,表明该出血毒素是金属蛋白酶。

Syntheses and crystal structures of novel di- and trinuclear rhodium complexes bridged by pyrazine

Never di- and trinuclear Rh complexes, [Rh-2(PPh3)(4)(H)(4)(Me2CO)(2)(mu -pyz)](ClO4)(2). EtOH and [Rh-3(PPh3),(mu -pyz)(3)](ClO4)(3). EtOH were selectively isolated from the reaction of [Rh(PPh3)(2)(H)(2)(Me2Co)(EtOH)]ClO4 with pyrazine (pyz) in Me2CO and THF, respectively. Their structures were crystallographically characterized.

Activation of a ring methyl substituent in pentamethylcyclopentadienyl rhenium(V) compounds: Synthesis and characterization of the 1,2,3,4-tetramethyl-5,6-dihydrofulvene-5,6-dithiolato complex [ReO{(S)(SCH2)C(5)Me(4)}(C(5)Me(5))]

Reaction of the half-sandwich rhenium(v) complexes [Re-Cl-4(C(5)Me(5))] or [Re(O)Cl-2(C(5)Me(5))] with H2S in chloroform in the presence of pyridine leads to the chiral dithiolato complex [ReO((S)(SCH2)C(5)Me(4))(C(5)Me(5))] 1.

灰盔累枝虫形态学及表膜下纤维系的研究

利用活体观察及蛋白银染色技术对灰盔累枝虫(Epistylisgalea)的形态学及表膜下纤维系进行了研究。该种主要鉴别特征为:活体个员的表膜柔软,虫体充分伸展时呈倒长锥形,体长200—300μm,体宽70—90μm;大核“J”字形,呈纵位。单一伸缩泡,直径21—25μm,背位。纵向纤维细密。口围盘纤维呈网状,与纵向纤维直接相连,并在整体上呈兜网状。与本属其他相近种相比,本种第3咽膜(P3)明显要长,其后1/3超出第1咽膜后继续向下呈弧形弯曲。本文对该种上述特征在分类学上的意义及其与相近种类之间的关系进行了

微囊藻栅藻资源竞争的动力学过程Ⅰ.光能和磷营养的半饱和参数及其生长率动态

以Tilman提出的“资源竞争机制学说”为依据 ,在单因子 (光、磷 )限制条件下 ,测定并计算铜绿微囊藻 (Microcystisaeruginosa)和斜生栅藻 (Scenedesmusobliquus)的半饱和常数 ,以双因子交互作用模型预测它们的生长动态 .结果表明 :在光强为 10 .0～ 17.1μE和磷浓度为 3.10～ 2 0 .0 μmol的范围内 ,微囊藻的生长率大于栅藻的生长率 .说明磷的增加是微囊藻成为水华的充分条件 ,但不是必要条件 ,至少低光强是一个重要的作用因子 .

A novel fast lock-in phase-locked loop frequency synthesizer with direct frequency presetting circuit

This paper proposes a novel, fast lock-in, phase-locked loop (PLL) frequency synthesizer. The synthesizer includes a novel mixed-signal voltage-controlled oscillator (VCO) with a direct frequency presetting circuit. The frequency presetting circuit can greatly speed up the lock-in process by accurately the presetting oscillation frequency of the VCO. We fully integrated the synthesizer in standard 0.35 mu m, 3.3 V complementary metal-oxide-semiconductors (CMOS) process. The entire chip area is only 0.4 mm(2). The measured results demonstrate that the synthesizer can speed up the lock-in process significantly and the lock-in time is less than 10 mu s over the entire oscillation frequency range. The measured phase noise of the synthesizer is -85 dBc/Hz at 10 kHz offset. The synthesizer avoids the tradeoff between the lock-in speed and the phase noise/spurs. The synthesizer monitors the chip temperature and automatically compensates for the variation in frequency with temperature.

A novel fast lock-in phase-locked loop frequency synthesizer with direct frequency presetting circuit

This paper proposes a novel, fast lock-in, phase-locked loop (PLL) frequency synthesizer. The synthesizer includes a novel mixed-signal voltage-controlled oscillator (VCO) with a direct frequency presetting circuit. The frequency presetting circuit can greatly speed up the lock-in process by accurately the presetting oscillation frequency of the VCO. We fully integrated the synthesizer in standard 0.35 mu m, 3.3 V complementary metal-oxide-semiconductors (CMOS) process. The entire chip area is only 0.4 mm(2). The measured results demonstrate that the synthesizer can speed up the lock-in process significantly and the lock-in time is less than 10 mu s over the entire oscillation frequency range. The measured phase noise of the synthesizer is -85 dBc/Hz at 10 kHz offset. The synthesizer avoids the tradeoff between the lock-in speed and the phase noise/spurs. The synthesizer monitors the chip temperature and automatically compensates for the variation in frequency with temperature.

An Ultra Low Power Non-volatile Memory in Standard CMOS Process for Passive RFID Tags

An ultra low power non-volatile memory is designed in a standard CMOS process for passive RFID tags. The memory can operate in a new low power operating scheme under a wide supply voltage and clock frequency range. In the charge pump circuit the threshold voltage effect of the switch transistor is almost eliminated and the pumping efficiency of the circuit is improved. An ultra low power 192-bit memory with a register array is implemented in a 0.18 mu M standard CMOS process. The measured results indicate that, for the supply voltage of 1.2 volts and the clock frequency of 780KHz, the current consumption of the memory is 1.8 mu A (3.6 mu A) at the read (write) rate of 1.3Mb/s (0.8Kb/s).

桃树茎直径变化及其与气象因子关系

用线性差分径向变化仪连续监测充分灌溉条件下的仕女红桃树茎直径变化,结合同步观测的气象因子数据,分析2007年3月中旬～10月下旬的仕女红桃树茎直径变化规律,为基于果树直径变化的灌溉管理提供基础依据。结果表明:仕女红桃树茎直径具有很好的时间变化规律,日变化曲线呈均匀"U"型,日最大值出现在黎明前后,日最小值出现在下午4时左右;季节变化方面,MDS呈低—高—低变化规律,从萌芽—开花期到果实成熟期的不同生长阶段,MDS平均值依次为87μm、200.84μm、253.75μm、171.67μm、138.67μm和94.34μm,坐果—展叶期和第一次果实膨大期MDS值居全生育期最高,需水量最大。桃树直径生长呈慢—快—慢变化规律,3月中下旬,开始生长,平均日生长量从12.68μm逐渐增加大36.84μm,7月24日～8月23日之间生长最快,平均日生长量达73.67μm,然后迅速下降,到生长末期平均日生长量仅为7.36μm。3～5月和7～9月可分别采用DI和MDS作为灌溉控制指标。茎直径变化与气象因子响应强烈,但不同生长阶段对茎直径变化产生主要影响的气象因子不同,对MDS产生主要影响的气象因子依次为:Rn、Tmax、Tma...

Topological Diversity of Coordination Polymers Containing the Rigid Terephthalate and a Flexible N,N'-Type Ligand: Interpenetration, Polyrotaxane, and Polythreading

Reactions of zinc(II) or cadmium(II) salts with terephthalic acid (H(2)tp) and 1,3-bis(4-pyridyl) propane (bpp) have afforded four coordination polymers at room temperature, [Zn(mu-tp)(mu-bpp)](n)center dot 2nH(2)O (1), [Cd-2(mu-tp)(2)(mu-bpp)(3)](n)center dot 2nH(2)O (2), [Cd(mu-tp)(mu-bpp)(H2O)](n)center dot nH(2)O (3), and [Cd-2(mu-tp)(mu-bpp)(2)(bpp)(2)Br-2](n) (4). Single-crystal X-ray diffraction has revealed interesting topological features for these compounds.

Synthesis and structural characterization of beta-diketiminate-lanthanide Amides and their catalytic activity for the polymerization of methyl methacrylate and epsilon-caprolactone

The synthesis and catalytic activity of lanthanide monoamido complexes supported by a beta-diketiminate ligand are described. Donor solvents, such as DME, can cleave the chloro bridges of the dinuclear beta-diketiminate ytterbium dichloride {[(DIPPh)(2)nacnac]YbCl(mu-Cl)(3)Yb[(DIPPh)(2)nacnac](THF)} (1) [(DIPPh)(2)nacnac = N,N-diisopropylphenyl-2,4-pentanediimine anion] to produce the monomeric complex [(DIPPh)(2)nacnac]YbCl2(DME) (2) in high isolated yield. Complex 2 is a useful precursor for the synthesis of beta-diketiminate-ytterbium monoamido derivatives. Reaction of complex 2 with 1 equiv of LiNPr2i in THF at room temperature, after crystallization in THF/toluene mixed solvent, gave the anionic beta-diketiminate-ytterbium amido complex [(DIPPh)(2)nacnac]Yb(NPr2i)(mu-Cl)(2)Li(THF)(2) (3), while similar reaction of complex 2 with LiNPh2 produced the neutral complex [(DIPPh)(2)nacnac]Yb(NPh2)Cl(THF) (4). Recrystallization of complex 3 from toluene solution at elevated temperature led to the neutral beta-diketiminate-lanthanide amido complex [{(DIPPh)(2)nacnac}Yb(NPr2i)(mu-Cl)](2) (5). The reaction medium has a significant effect on the outcome of the reaction.

中国沿海典型区域织纹螺毒性及毒素成分研究

织纹螺（Nassarius spp.）味道鲜美，是中国及其它一些亚洲国家沿海地区居民习惯食用的一种水产品。但是，近几十年来，中国沿海频繁发生食用织纹螺中毒事件，严重威胁着人们的身体健康和生命安全。加之人们对织纹螺体内的毒素成分、来源及其毒性变化规律还没有清晰的认识，因此难以有效预防和控制食用织纹螺引起的中毒事件。本文根据文献报道，在中国沿海食用织纹螺中毒事件多发的典型区域，包括江苏省的连云港市和盐城市、浙江省的舟山市和宁波市、福建省的宁德市、厦门市和莆田市设立了监测点，于2006年和2007年间进行了连续采样，应用小鼠生物测试法调查了织纹螺毒性的消长情况，并利用高效液相色谱-质谱联用（Liquid Chromatography-Mass Spectrometry，LC-MS）和高效液相色谱技术（High Performance Liquid Chromatography，HPLC）对织纹螺体内的毒素成分进行了分析。 实验结果表明，2006年于江苏省盐城市射阳海域采集的织纹螺样品中，阳性样品检出率为56%，毒性在2-5 MU/g组织（湿重）之间变化，在2007年于同地采集的8个样品中，除一个样品毒性为3.14 MU/g组织（湿重）以外，其余样品均表现为阴性；而2007年采集自连云港市赣榆海域的织纹螺样品，在采样期间则呈现出极高的毒性，最高达到846.52 MU/g 组织（湿重），毒性在监测期间呈“M”状波动，在5月和7月下旬出现两个毒性高峰。2006年于浙江省宁波市象山港采集的织纹螺样品中，阳性样品检出率为25%，毒性均在2.5 MU/g组织（湿重）左右；而同年采集自舟山市定海的织纹螺样品中，阳性样品检出率为100%，最高毒性达18.40 MU/g组织（湿重），毒性在监测期间也呈“M”状波动，高峰期出现在6月初和7月底。2006年3-9月采集自福建省宁德霞浦、厦门同安和莆田涵江采集的织纹螺样品中，阳性样品检出率分别为20%、43%和14%，除7月中旬采集自宁德霞浦的一个样品毒性达到16.19 MU/g组织（湿重）之外，其余样品毒性均在2-5 MU/g组织（湿重）间波动。从阳性样品的时间分布规律来看，3月份和6、7月份是阳性样品集中出现的时期。根据以上调查结果可以看出，织纹螺的毒性消长呈现出较明显的地域性和季节性特征，不同地区的织纹螺毒性存在差异，而同一区域织纹螺毒性的消长则表现出明显的季节性集中趋势。除了2007年采集自连云港赣榆的织纹螺样品毒性与其平均个体组织重量有相似的变化趋势以外，其余地区的织纹螺样品毒性和个体大小无明显相关性。 利用LC-MS和HPLC技术对织纹螺样品中的毒素成分进行了分析，确定河豚毒素（tetrodotoxin, TTX）及其同系物（trideoxyTTX，4-epi-TTX，anhydroTTX，oxoTTX）是所采集织纹螺中的主要致毒成分，样品中没有检测到麻痹性贝毒毒素（Paralytic Shellfish Poison, PSP）。自不同地区采集的织纹螺中毒素成分基本一致，但组成存在一定差异。其中，采自江苏省连云港赣榆和浙江省舟山定海的织纹螺样品中，trideoxyTTX是主要的成分，其次是TTX；而从其它采样地点采集的织纹螺中，TTX都是主要的毒素成分，其次才是trideoxyTTX及其它同系物。对采集自江苏省连云港赣榆和浙江舟山定海的织纹螺体内毒素的解剖学分布进行了分析，结果表明肌肉、消化腺和剩余部分中的毒素组成基本一致，其中trideoxyTTX是主要的毒素成分，其次为TTX，但采自浙江舟山的织纹螺剩余部分中的TTX是主要的毒素成分。在监测期间，各组织中的毒素组成没有明显变化，但毒素含量随季节变化表现出了一定的差异。 综上所述，在中国沿海典型区域开展的织纹螺毒性调查结果表明其毒性消长具有一定的地域性和季节性特征。分析结果显示织纹螺体内的毒素成分是河豚毒素及其同系物，采自不同区域的织纹螺体内毒素成分基本一致，但毒素组成稍有差异。对织纹螺中毒素的解剖学分布研究显示，各组织中的毒素含量随季节变化而表现出一定差异，但毒素组成没有明显的季节性变化。这些结果显示中国沿海的织纹螺应具有相似的毒素来源，研究结果将为相关部门有效监测、预防和控制食用织纹螺中毒事件提供有力的科学依据。