二(4-甲氧基苯基)-羟乙酸甲酯的合成及其晶体结构

提出了一种合成标题化合物的新方法,用IR、1HNMR及X-ray单晶衍射方法对其结构进行了表征。晶体结构分析表明,化合物为正交晶系,空间群P212121,晶胞参数a=0.7749(4)nm,b=1.2680(6)nm,c=1.5462(7)nm,β=90°,V=1.5193(13)nm3,Z=4,Dc=1.322g/cm3,F(000)=640,μ=0.097mm-1,R1=0.0531,wR2=0.1129。     

二苄基锡双(对氨基苯甲酸)酯的合成及结构研究

二苄基氧化锡与对氨基苯甲酸反应合成了二苄基锡双 (对氨基苯甲酸 )酯 ,经X- 射线方法测定了新化合物的晶体结构 ,属单斜晶系 ,空间群为P2 ( 1) /n ,晶体学参数 :a =1 .12 0 9(4)nm ,b =0 . 86 0 2 (3)nm ,c =2. 6 5 2 0 (10 )nm ,β =93. 95 3(5 )° ,V =2. 5 5 12 (17)nm3 ,Z =4 ,Dc =1. 4 92g/cm3 ,μ(MoKα) =10 .38cm-1,F(0 0 0 ) =116 0 ,R1=0 . 0 4 6 8,wR2 =0 . 0 896。在化合物中 ,锡原子呈六配位的畸变八面体构型。     

Synthesis,crystal structure and characterization of trivacant-Keggin-polyoxometalate-based carbonyl manganese derivative

A novel trivacant polyoxometalate-based carbonyl manganese derivative, (NH₄)₃H₃[{Mn(CO)₃}(Mn(H₂O)₂)(Mn(H₂O)₃)(TeW₉O₃₃)]₂·31H₂O (1), was successfully isolated in the mixed solvent of acetonitrile and water at room temperature. The composition and structure of the product were characterized by elemental analysis, X-ray powder diffraction (XRPD), thermogravimetric analysis (TGA), IR, UV–vis, CV and single crystal X-ray diffraction.     

Synthesis,characterization and crystal structure of a zinc bis-dithiocarboxylate derivative

The zinc(II) complex, Zn(3,5-di-t-butyl-4-hydroxybenzene-dithiocarboxylate)₂(pyridine) (3) was obtained by the reaction of Zn(CH₃CN)₄(BF₄)₂ with the sodium salt of 3,5-di-t-butyl-4-hydroxybenzene-dithiocarboxylate (1) with subsequent recrystallization from pyridine. The latter salt (1) was prepared by the deprotonation of 2,6-di-t-butylphenol with NaH in THF, followed by reaction with carbon disulfide at ambient temperature. The structure of complex 3 was established by X-ray crystallography and shown to be of a distorted trigonal bipyramidal geometry with one sulfur atom from each of the dithiocarboxylate ligands occupying the axial sites. By way of contrast, Na(2,4-di-t-butylphenolate) was found to react with CS₂ to afford the xanthate derivative, Na(O-2,4-di-t-butylphenyldithiocarbonate) (4).     

Synthesis,characterization and crystal structure of bis(acetylacetonato)dimethanolnickel(II): [Ni(acac)2(MeOH)2]

Bis(acetylacetonato)dimethanolnickel(II) was isolated as turquoise needle-like crystals by recrystallization of bis(acetylacetonato)nickel(II) from methanol solution and fully characterized by ¹H and ¹³C NMR, FT-IR spectroscopy, and single crystal X-ray diffraction. The X-ray structure analysis gives essentially a triclinic unit cell of bis(acetylacetonato)dimethanolnickel(II) containing one centrosymmetric molecule of the formula Ni[(O₂C₅H₇)₂(OHCH₃)₂]. The Ni(II) ion is located at the inversion centre of a tetragonally distorted octahedral coordination sphere. The equatorial plane of the tetragonally distorted octahedral coordination sphere includes four O-donor atoms of two acetylacetonato ligands and the axial positions are occupied by two oxygen atoms of two methanol ligands.     

Synthesis and crystal structures of copper(I) iodide complexes chelating with bis(ethylamidophosphine)

Two copper(I) iodide complexes with polydentate bis(ethylamidophosphine) ligands were synthesized, characterized with crystal structures. They include a dimeric complex [Cu(μ-I)(CH₂NHCOC₂H₄PPh₂)₂]₂ 1 containing a planar Cu₂I₂ rhombohedron with two doubly bridged ligands and a tetrameric complex {Cu₄(μ-I)₄[(CH₂NHCOC₂H₄PPh₂)₂]₂} 3 with all the coppers and iodines forming a highly distorted cubane geometry.     

亚磷酸三(2,4-二叔丁基苯基)酯的合成及其晶体结构

由2,4-二叔丁基酚与PCl3在二甲苯溶剂中反应合成了亚磷酸三(2,4-二叔丁基苯基)酯,其分子式为C42H63O3P.通过Nonius CAD4型X-射线衍射仪检测,其晶体结构测定结果如下:该晶体属于三斜晶系,P-1空间群,a=1.329 9(3)nm,b=1.350 3(3)nm,c=1.385 2(3)nm,α=112.20(3)°,β=104.66(3)°,γ=102.31(3)°,Dc=1.027 g/cm3,Z=2,F(000)=708,μ=0.098 mm-1,最终偏差因子分别为R=0.096 5,wR=0.245 0.X-射线衍射分析表明,分子内部分相邻原子间形成C—H…O氢键.     

有机锡化合物二丁基锡(Ⅳ)二噻吩甲酸酯的合成表征及晶体结构

利用二丁基氧化锡与噻吩甲酸以1∶2物质的量比反应,合成了二丁基锡(Ⅳ)二噻吩甲酸酯。通过元素分析、红外光谱、核磁共振氢谱和锡谱对其结构进行了表征。用X-射线单晶衍射测定了该化合物的晶体结构,结果表明,分子中锡原子为6配位的歪斜梯形双锥构型,并且化合物以弱桥联二聚体存在。该化合物晶体属P21/c空间群,晶胞参数为:a=1.8709(3)nm,b=2.2337(4)nm,c=1.0517(16)nm,β=93.917(2),°Z=8,F(000)=1968,V=4.3826(12)nm3,μ=1.374mm-1,S=1.051,R1=0.0447,wR2=0.1112。     

Synthesis, optical characterization and crystal and molecular X-ray structure of a phenylazojulolidine derivative

The synthesis, spectroscopic characterization, and X-ray crystal structure of [4-(2,3,6,7-tetrahydro-1H,5H-pyrido[3,2,1-ij]quinolin-9-ylazo)-phenyl]-methanol azodye are reported. A 37-47 nm bathochromic shift has been observed by comparison with analogous azodyes where diethylamino or dimethylamino groups act as donor moiety in agreement with the larger electronic donating properties of julolidine. The azobenzene skeleton adopts a planar trans-configuration and intra- and inter-molecular hydrogen bonds have been detected. A correlation between the spectroscopic and the molecular features has been attempted.     

Synthesis,crystal structure and electrocatalytic activity of discrete and polymeric copper(II) complexes with bitopic bis(pyrazol-1-yl)methane ligands

New coordination copper(II) compounds containing bitopic bis(pyrazol-1-yl)methane ligands, namely 1,1,2,2-tetrakis(pyrazol-1-yl)ethane, 1,4-bis[bis(pyrazol-1-yl)methyl]benzene and 1,4-bis[bis(3,5-dimethylpyrazol-1-yl)methyl]benzene were prepared. Reactions of ligands with Cu^2 + ions in 1:2 ratio gave discrete homodinuclear complexes, while 1:1 ligand-to-metal ratio lead to the formation of coordination polymers. Electrocatalytic activity of compounds in oxygen electroreduction reaction on the surface of modified carbon paste electrode was evaluated.     

2-(2-羟苯基)苯并咪唑的新颖合成和晶体结构

基于2-(2-1羟苯基)苯并咪唑(HPBI)在生物学、药理学及光电材料等方面的性质和应用意义,查阅大量文献,报道了配体HPBI新颖的合成方法,采用单晶衍射进行表征,并进行了该配体的晶体结构测定.结果表明,晶体属于单斜晶系,空间群P2(1),晶胞参数:α=3.8541(10)A°,b=2.2170(6)A°,c=5.86...     

高氯酸化三邻菲啰啉合锌(Ⅱ)的合成及晶体结构

合成了过渡金属元素Zn与1,10-邻菲啉的配合物,并进行了元素分析、红外光谱等表征,测定了配合物的晶体结构。配合物组成为[Zn(Phen)3](ClO4)2,属于单斜晶系,P2(1)/n空间群。配合物中金属离子Zn2 处于N6的配位环境,配位构型为六配位的扭曲八面体。     

(S)-卡巴拉汀D-(+)-DTTA盐的合成与晶体结构

标题化合物由3-(1-二甲氨基乙基)苯酚与N-乙基-N-甲基氨基甲酰氯反应合成卡巴拉汀游离碱,再与(+)-O,O'-二对甲基苯甲酰-D-酒石酸(D-(+)-DTTA)成非对映体盐制得.它的晶体结构已通过单晶X-射线衍射测试得到确定.通过对3 477个sk 以观察到的独立衍射点[I>2σ(I)]的测试,结果表明:该品体属于斜方晶系,P21212空间群.α=14.608 4(7)A,6=30.787 6(14)A,c=7.544 2(3)A,α=90,β=90,γ=90,V,=3 393.1(3)A3,Z=2,Dc=1.246 mg/m3,μ=0.092mm-1,F(000)=1 352,R=0.0529,wR=0.145 9.     

Synthesis and structure determination of bis(1,3-di-tert-butylcyclopentadienyl)(divinyl)hafnium

The reaction of (t-Bu₂C₅H₃)₂HfCl₂ (1) with vinyllithium yield ivory coloured crystals identified as (t-Bu₂C₅H₃)₂Hf(CHCH₂)₂ (2). The X-ray structure analysis of 2 shows the presence of the divinyl complex, whereby one of the vinyl groups is partially replaced by chlorine (25%).     

Synthesis and crystal structure of bis(morpholino dithiocarbamato) Cd(II) complex and its use as precursor for CdS quantum dots using different capping agents

ABSTRACT

Cadmium(II) morpholine dithiocarbamate complex [Cd(morphdtc)₂] was synthesized and characterized by single crystal X-ray crystallography. The molecular structure of the complex showed Cd(II) ion in a distorted 4?+?2 octahedral geometry, in which the two morpholine dithiocarbamates act as bidentate chelating and the central Cd ion bond the sulfur atoms of adjacent morpholine acting as bridging ligands to form centrosymmetric five coordinate dimeric molecules. The Cd(II) complex was thermolysed at 180°C to prepare CdS nanoparticles using three different capping agents. The pXRD patterns revealed a mixture of hexagonal and cubic crystalline phases of CdS nanocrystals. TEM images revealed semi-spherical and spherical nanoparticles, with the size range of 4.50–5.70?nm for OLM-CdS, 3.33–5.96?nm for HDA-CdS, and 3.00–5.83?nm for ODA-CdS. The particle size distribution of the CdS nanocrystallite is within the range 1.06?nm (SD?±?0.73) for OLM-CdS, 0.68?nm, (SD?±0.73) for HDA-CdS and 1.18?nm, (SD?±?0.60) for ODA-CdS. The lattice fringes showed that the particles are almost in the same environment with the interplanar of 0.32?nm for OLM-CdS, 0.34?nm for HDA-CdS, and 0.32?nm ODA-CdS. The band gaps energy were confirmed to be 1.59?eV for OLM-CdS, 1.65?eV for HDA-CdS, and 1.62?eV for ODA-CdS nanoparticles, respectively.     

高氯酸化三邻菲啰啉合铜(Ⅱ)的合成及晶体结构

合成了过渡金属元素Cu与1,10-邻菲啉的配合物并进行了元素分析、红外光谱等表征,测定了配合物的晶体结构。配合物组成为[Cu(phen)3](ClO4)2,属于单斜晶系,P2(1)/n空间群。配合物中金属离子Cu2+处于N6的配位环境,配位构型为六配位的拉长八面体。     

Synthesis and crystal structure of hexacerium(IV) cluster-containing Keggin polyoxometalate trimer

A novel hexacerium(IV) cluster-containing polyoxometalate (POM), K₁₈[{Ce₆(μ₃-O)₄(μ₃-OH)₄(OAc)₂}(A-α-SiW₉O₃₄)₂(α-SiW₁₁O₃₉)]·37H₂O (K₁₈Ce₆-POM), was unexpectedly obtained by a reaction of the potassium salt of open-Dawson POM, K₁₃[{K(H₂O)₃}₂{K(H₂O)₂}α,α-Si₂W₁₈O₆₆]·19H₂O (K-open POM), with (NH₄)₂[Ce(NO₃)₆], in a 0.5 M KOAc/HOAc buffer solution (pH 4.8) at 80 °C, and unequivocally characterized by X-ray crystallography, ¹H, ¹³C, and ²⁹Si NMR spectroscopy, FTIR spectroscopy, complete elemental analysis, and TG/DTA. X-ray crystallography revealed that the monolacunary Keggin unit, [α-SiW₁₁O₃₉]^8 −, and the two trilacunary Keggin units, [A-α-SiW₉O₃₄]^10 −, are connected by a central Ce₆-oxo/hydroxide cluster moiety, [Ce₆(μ₃-O)₄(μ₃-OH)₄(OAc)₂]^10 +, to form a trimeric Keggin polyanion, [{Ce₆(μ₃-O)₄(μ₃-OH)₄(OAc)₂}(A-α-SiW₉O₃₄)₂(α-SiW₁₁O₃₉)]^18 − (Ce₆-POM). ¹H, ¹³C, and ²⁹Si NMR spectra in D₂O suggested that the Ce₆-POM was obtained as a single species and its molecular structure was maintained in solution.     

Synthesis and identification of bis (diacylglycero) phosphoric acid and bis (monoacylglycero) phosphoric acid

Synthesis of bis-(diacylglycero)phosphoric acid fromsn-1,2-dipalmitoylglycerol and phenylphosphoryl dichloride according to Baer (1) was revised. New data are reported about identification of the intermediate and final products: (a) bis-phosphatidic acid phenyl ester is very slowly visualized by the Zinzade reagent and can escape notice; (b) large amounts of phosphatidic acid chloride phenyl ester are also formed; and (c) very little transacylation fromsn-1,2-dipalmitoyl-glycerol to the 1,3-isomer is observed. Hydrolysis of bis-phosphatidic acid to bis-lysophosphatidic acid is much easier using phospholipase A₂ from pig pancreas than from snake or bee venom.     

Gold(I) phosphine complexes with bis(2-pyridyl)diselenoether: Synthesis and structure elucidation

Bis(2-pyridyl)diselenoether with the general formula (2-PySe)₂(CH₂) (L) reacts with Ph₃PAuCl and [(dpph)(AuCl)₂] dpph = 1,6-bis(diphenylphosphino)hexane to produce the respective complexes [(L)Au₂(PPh₃)₂](PF₆)₂ (1) and [(L)(dpph)Au₂(PF₆)₂]_n (2). These complexes were isolated in crystalline form and studied using spectroscopic and X-ray diffraction techniques. The coordination of the ligand (2-PySe)₂(CH₂) (L) to the gold(I) metal centers in complexes [(L)Au₂(PPh₃)₂](PF₆)₂ (1) and [(L)(dpph)Au₂(PF₆)₂]_n (2) occurs via the nitrogen atom of the pyridine ring, with no interaction with the selenium atoms of the bis(2-pyridyl)diselenoether. The gold derivative (Ph₃PAuCl or [(dpph)(AuCl)₂]) is responsible for the formation of a molecular complex (1) or a polymeric complex (2), and in both compounds the gold(I) metal atoms adopt an almost linear geometry.     

Synthesis and crystal structure of scandium(III) and cadmium(II) thiocyanato complexes with dimethylsulfoxide

Two novel complex compounds, molecular fac-[Sc(NCS)₃(DMSO)₃] and polymeric chain [Cd(NCS)_4/2(DMSO)₂]_∞ (DMSO = dimethylsulfoxide), were synthesized and structurally characterized. In both complexes, the metal atoms have octahedral coordination with the NCS⁻ ion serving two different functions: as a terminal ion with the coordination via N in Sc complex and as a bridge ligand with the coordination via N and S in the case of Cd compound, respectively. The DMSO ligands are coordinated by oxygen atoms.