含羧酸配体的鼓形有机锡氧簇合物：六聚苯基锡氧3-吲哚丁酸酯的合成及晶体结构

利用Ph3SnOH和3-吲哚丁酸以1：1摩尔比反应，合成了新型含羧酸配体的鼓形 有机锡氧簇合物：六聚苯基锡氧3-吲哚西酸酯。通过元素分析、红外光谱和X射线 单晶衍射对其结构进行了表征。测试结果表明：该化合物为三斜晶系，空间群P1， a=1.1722(6),b=1.5694（8）nm，c=1.7227(9)nm，α=116.251（8）°，β=100. 854（10）°，γ=95.606（9）°，Z=1，V=2.732(3)nm^3，Dc=1.554g·cm^-3，μ =1.420mm^-1，F(000)=1276，R=0.0630，ωR=0.0762。晶体结构中，六配位的锡原 子呈畸变的八面体构型。     

一种电流失配自适应补偿宽带锁相环设计

针对宽带自偏置锁相环(PLL)中存在严重的电荷泵电流失配问题,提出了一种电流失配自适应补偿自偏置锁相环。锁相环通过放大并提取参考时钟与反馈时钟的锁定相位误差脉冲,利用误差脉冲作为误差判决电路的控制时钟,通过逐次逼近方法自适应控制补偿电流的大小,逐渐减小鉴相误差,从而减小了锁相环输出时钟信号抖动。锁相环基于40 nm CMOS工艺进行设计,后仿真结果表明,当输出时钟频率为5 GHz时,电荷泵输出噪声从-115.7 dBc/Hz@1 MHz降低至-117.7 dBc/Hz@1 MHz,均方根抖动从4.6 ps降低至1.6 ps,峰峰值抖动从10.3 ps降低至4.7 ps。锁相环输出时钟频率为2～5 GHz时,补偿电路具有良好的补偿效果。     

一种多相延迟锁相环的自校准方案

芯片间数据传输速率的不断提高,导致系统对时钟信号的要求越来越高.延迟锁相环在各种高速通信系统中提供多相位时钟,其相位精度直接影响到数据的误比特率.然而,因鉴相器器件失配引起的相位误差问题在时钟频率提高的同时愈发明显.针对一种基于OTA的延迟锁相环电路鉴相器失配问题,提出了一种环路自校准方案,同时给出校准电路的Verilog-A行为级模型.当鉴相器中两个或门电路之间存在失配误差时,将会在OTA输入端以失调电压的形式引起输出相位偏移;校准电路能够对该失调电压实现检测与计算,并补偿至环路中,使得理想反馈时钟条件下,OTA输入端电压保持相同,压控延迟线延时不再改变,最终能够有效减小因鉴相器失配引起的输出时钟相位误差.基于TSMC 40nm CMOS工艺完成了4相DLL电路的设计,其工作频率范围能够达到10 GHz~12 GHz;联合校准电路模型,通过电路-模型混合仿真结果显示:校准前后,输出时钟相位误差均方值从300fs降低至30fs.     

大孔径阳离子交换树脂用于富集白酒中碱性含氮化合物的研究

采用大孔径阳离子交换树脂富集白酒中碱性含氮化合物,研究了影响回收率的各种因素并予以改进,使几种低挥发性吡嗪化合物的回收率达80%以上。用本法富集和气相色谱分离定量测定了几种酱香型白酒中吡嗪化合物的含量。     

具有S…S、S…Cl作用的一维链状有机锡化合物氯代二苄基锡哌啶荒酸酯的合成、表征及晶体结构

The chlorodibenzyltin dithiopiperidylcarbamate was synthesized by the reaction of dibenzyltin dichloride with dithiopiperidylcarbamate and was characterized by elemental analysis， IR and ¹H NMR. The crystal structure was determined by X-ray single crystal diffraction. The crystallographic data are as follows： monoclinic， space group P2₁， a=0.63464(13)nm， b=1.9110(4)nm， c=0.87367(17)nm， β=97.67(3)°， Z=2， V=1.0501(4)nm³，D_c=1.571g·cm^-3， μ=1.546mm^-1， F(000)=500， R=0.0209， wR=0.0381 [I≥ 2σ(I)]. The str- uctures consist of discrete molecules containing five-coordinate tin atoms in a seriously distorted trigonal bipyramidal configuration. The molecules are packed in the unit cell in one-dimensional chain complex through a weak inter-action between the chlorine atom， the sulfur atom and one of the other sulfurs of an adjacent molecule. CCDC： 180034.     

二苄基一氯化锡二硫代氨基甲酸酯的合成

二烃基氯化锡及其衍生物具有较强的抗癌活性，日益受到人们的重视。关于含有Ｓｎ—Ｏ键的二烃基锡衍生物的合成研究已有大量报道［１］。但含Ｓｎ—Ｓ键二烃基锡衍生物的合成研究则较少［２］，而二烃基一氯化锡二硫代氨基甲酸酯的合成研究尚未见报道。为了寻找具有抗癌活...     

成形滤纸片薄样X射线荧光光谱法测定铝合金中镧铈镨钕钐

研究了用成形滤纸片薄样X射线荧光光谱法测定铝合金中的镧、铈、镨、钕、钐。方法具有准确、快速、简便、经济等优点。各元素的测定灵敏度为La 48054,Ce 65923,Pr 93953,Nd 62622,Sm107630 cps/(mg/cm~2)。定量分析下限约为0.xμg/cm~2。     

铋配合物[Bi(S2CNC5H10)2(NO3)]·[1，10-Phen]·0.5H2O的合成及晶体结构

The bismuth complex with dithiopiperdylcarbamate [Bi(S₂CNC₅H₁₀)₂(NO₃)]·[1，10-Phen]·0.5H₂O was synthesized. The crystal and molecular structure were determined by X-ray single crystal diffraction. The crystal belongs to monoiclinic with space group C2/c, a=3.140(2) nm, b=1.176 4(9) nm, c=2.021 6(15) nm, β=103.081(12)°, V=5.713(7) nm³, Z=8, F(000)=3064, D_c=1.815 g·cm^-3, μ=6.502mm^-1. The final R₁=0.0332, wR₂=0.040 3. In the complex, the bismuth atom is eight-coordinated in a capped distorted pentagonal bipyramidal geometry. CCDC: 222655.     

二聚体有机锡配合物{[n-Bu2Sn(O2CCH2CS2NC4H8)]2O}2的合成，表征及晶体结构(英)

The title compound, {[n-Bu₂Sn(O₂CCH₂CS₂NC₄H₈)]₂O}₂, has been synthesized by the reaction of (tetrahydro-pyrrodithiolocarbamoylthio)acetic acid with the di-n-bubyltin oxide in 1∶1 molar ratio. The complex has been characterized by elemental analysis, IR and NMR. The crystal structure of it has been determined by X-ray single crystal diffraction. And the results showed that the crystal belongs to triclinic system with space group P1 and some crystal parameters: a=1.220 2(9) nm, b=1.315 8(10) nm, c=1.380 4(10) nm, α=111.215(9)°， β=99.357(9)°， γ=96.075(10)°, V=2.006(2) nm³, Z=1, F(000)=908, μ=1.489 mm^-1, D_c=1.474 g·cm^-3, R₁=0.037 5, wR₂=0.0839. The complex has a centrosymmetric dimer structure mode with a four-membered central endo-cyclic Sn₂O₂ unit in which two bridged oxygen atoms both connect with an exo-cyclic tin atom which has a distorted octahedron. Each of the endo-cyclic tin atoms exhibits a distorted trigonal bipyramid coordination geometry with an additional weak coordination carboxylate oxygen. Four carboxylate ligands are divided into two types. And two of them are bidentate and connecting to each of exo-cyclic tin atoms by using both oxygen atoms, whereas the others bridge to each pair of exo-and endo-cyclic tin atoms utilizing one oxygen atom only. CCDC: 220513.     

三苄基锡二硫代氨基甲酸酯的合成

三苄基锡二硫代氨基甲酸酯的合成尹汉东马春林＊张如芬（聊城师范学院化学系聊城２５２０５９）关键词三苄基氯化锡，二硫代氨基甲酸盐，合成１９９７－０７－１０收稿，１９９７－０９－０９修回山东省自然科学基金资助项目三烃基锡衍生物是一类具有较强生物活性的有机锡...