Synthesis of Lactam-containing Amido(ethoxy)methylphosphonates

Russian Journal of General Chemistry -     

Synthesis and Characterization of Some New Triorganophosphorus, -Arsenic and -Antimony(V) Amido Derivatives

A number of triorganophosphorus, -arsenic, and -antimony(V) amido derivatives of the general formula R 2 R'ML 2 [where R = C 6 F 5 , C 6 H 5 ; R' = C 6 F 5 , C 6 H 4 CH 3 - p ; M = P, As or Sb and L = imidazole, benzimidazole, 2-methyl benzimidazole, indazole, and 1,2,3,4-tetrahydrocarbazole] have been synthesized by the metathetical reaction of triorganophosphorus, -arsenic, and -antimony(V) halides and the corresponding imidazoles in the presence of triethyl amine. These compounds have been characterized by elemental analysis, IR and NMR ( 1 H and 19 F) spectroscopy, conductance, and molecular weight data. The Van't Hoff factor "i" and molar conductance data of the compounds revealed them to be monomeric and nonionic in nature. On the basis of spectroscopic studies, a tentative trigonal bipyramidal structure has been assigned for these amido derivatives.     

Synthesis and Structural Characterization of a Novel Heterodinuclear Vanadium(IV)‐Nickel(II) Complex

A novel V^IV‐Ni^II heterodinuclear complex [VO(cat)₂][Ni(1, 2‐PDA)₂H₂O] ( 1 ) (cat = catechol; 1, 2‐PDA = 1, 2‐propane diamine) was synthesized at low temperature (10 °C) and characterized by IR spectroscopy and X‐ray diffraction. A novel Ni–O=V structure exists in the complex, the vanadyl–catechol moiety and the nickel–diamine moiety are connected by an oxygen bridge; all molecules are further assembled into crystallites by O–H ··· O hydrogen bonds.     

两种有机-无机复合杂多化合物的水热合成及结构表征

利用水热法制备了基于饱和Keggin结构阴离子构筑的有机-无机复合多金属氧酸盐(4,4′-bipy)4H4[PMo12O40](CH3COO).1.5H2O(1)和(4,4′-Hbipy)2(4,4′-bipy)2H[PW12O40].3.5H2O(2)(4,4′-bipy=4,4′-联吡啶),并借助元素分析、红外光谱、紫外光谱、热分析和X射线单晶衍射分析了两种化合物的组成和结构.结果表明,化合物1和2均属于单斜晶系,P2(1)/c空间群.化合物的晶胞参数为:a=1.869 40(13)nm,b=1.404 23(9)nm,c=2.707 76(18)nm,β=105.848 0(10)°,V=6.837 9(8)nm3,Z=4,R1=0.095 4;化合物2的晶胞参数为:a=1.884 80(12)nm,b=1.409 89(9)nm,c=2.664 92(17)nm,β=105.368 0(10)°,V=6.828 4(8)nm3,Z=2,R1=0.097 2.两种化合物结构类似,其结构单元均是由饱和Keggin阴离子与游离的4,4′-联吡啶分子通过静电作用相结合形成的.     

Synthesis and Characterization of Diphenyltin(IV) Dicarboxylates Containing Germanium

Twelve new germanium substituted diphenyltin dipropionates with the general formula (R¹GeCHR²‐CHR³COO)₂SnPh₂ where R¹ = N(CH₂CH₂O)₃, (C₆H₅)₃ and (CH₃C₆H₄)₃, R² = H, CH₃, C₆H₅, p‐CH₃C₆H₄, p‐CH₃OC₆H₄, p‐ClC₆H₄, and R³ = H, CH₃ have been synthesized by the reaction of diphenyltin oxide with a germanium substituted propionic acid. All the compounds were characterized by elemental analysis, IR, multi‐nuclear (¹H, ¹³C, ¹¹⁹Sn) NMR and Mössbauer spectroscopies as well as mass spectrometry. The in vitro antibacterial activity of selected compounds is also reported.     

Synthesis and Structural Characterization of Neutral Hexacoordinate Silicon(IV) Complexes with SiO2N4 Skeletons

Surrounded by six : A series of novel neutral hexacoordinate silicon(IV ) complexes with SiO₂N₄ skeletons, containing two bidentate monoanionic O,N ligands and two monoanionic NCX (X = O, S) ligands, was synthesized. The formation of the title compounds involved some unexpected transformations of the bidentate O,N ligands.

     

Dilithium Hexaorganostannate(IV) Compounds

Hypercoordination of main‐group elements such as the heavier Group 14 elements (silicon, germanium, tin, and lead) usually requires strong electron‐withdrawing ligands and/or donating groups. Herein, we present the synthesis and characterization of two hexaaryltin(IV) dianions in form of their dilithium salts [Li₂(thf)₂{Sn(2‐py^Me)₆}] (py^Me=C₅H₃N‐5‐Me) ( 2 ) and [Li₂{Sn(2‐py^OtBu)₆}] (py^OtBu=C₅H₃N‐6‐OtBu) ( 3 ). Both complexes are stable in the solid state and solution under inert conditions. Theoretical investigations of compound 2 reveal a significant valence 5s‐orbital contribution of the tin atom forming six strongly polarized tin–carbon bonds.     

Electrochemical Studies of Tantalum(V) Chlorides and Bromides in Acetonitrile. Electrochemical Generation of Tantalum(IV) Species

The electrochemical properties of tantalum halides, TaX₅ Et₄NTaCI₆ and Bu₄NTaBr₆ (X = Cl^? and Br^?) were investigated in rigorously dried acetonitrile using cyclic voltammetry and constant potential electrolysis. A special vacuum electrochemical cel1 equipped with a sample loading device and an AI₂O₃ column was used in order to prevent the hydrolysis of tantalum halides with the small amount of water present in “dry” acetonitrile. Two one-electron reduction waves were observed for al1 tantalum(V) species which correspond to consecutive Ta(V) → Ta(IV) and Ta(IV) → Ta(III) reduction. The E_1/2 values for the Ta(V) → Ta(IV) reduction process are criticalIy dependent on the number of CI^? ligands coordinated to the tantalum atom. As the number of Cl^? is increased from 4 to 5 and 6, it becomes more difficult, by 0.4 V, to reduce Ta(V) to Ta(IV). Constant potential electrolysis at –20°C generates Ta(IV) species; thus TaCl₆ ^2-. TaBr₆ ^2-, TaCl₅NCMe^?, TaBr₅NCMe^? and TaCI₄(NCMe)₂, are obtained in acetonitrile solution after electrolysis. It was found that the reduction product of TaCl₅NCMe depends upon the temperature. At a higher temperature (0°C) the initial electron transfer step is fol1owed by a chemical reaction in which some of the product, TaCI₅NCMe^?, reacts with the starting material, TaCI₅NCMe. to produce TaCl₆ ^? and TaCl₄(NCMe)₂. At lower temperatures (–20°C) the rate of the folIowing chemical reaction is much slower and the reduction product is almost exclusively TaCl₅NCMe^?.     

Synthesis,Spectroscopic Properties and Crystal Structural Characterization of a Triphenyltin(IV) Complex with 5-Bromonicotinic Acid

1 INTRODUCTION Organotin esters of carboxylic acids are widely used as biocides, fungicides and homogeneous ca- talysts in industry[1～3]. Recently, pharmaceutical pro- perties of organotin esters of carboxylic acids have been investigated for their antitumour activity[4, 5]. Studies on organotin compounds containing car- boxylate ligands with additional donor atoms (e.g. N, O or S) that are available for coordination to the tin atom have revealed that new structural types may lead to di…     

Synthesis and Characterization of a Novel Phosph(V)azane-Tin(IV) Complex

Abstract

The reaction of bis(anilino)phosphine oxide (C₆H₅NH)₂P(O)H, 1 with Bu₂ ⁿSnCl₂ in the presence of an excess of triethylamine (TEA) in dry tetrahydrofurane (THF) yields the novel N,O-bonded tin complex Bu₂ ⁿSn[NPh(O)P(H)NPh(HNEt₃)]₂, 2. TEA is used as a base to deprotonate the phosphazane ligand and is separated as Et₃NH⁺Cl^?, whereas HTEA⁺ exists in the final product 2 and act as a charge balancing and H-bond structure–directing agent. This new compound has been fully characterized by means of IR, MS, and multinuclear (¹H, ³¹P, and ¹¹⁹Sn NMR) spectroscopy.     

Synthesis of Macrocyclic Compounds Using Diorganotin(IV) Dicarboxylates as Covalent Templates

A series of new macrocyclic compounds have been prepared by treating di- n -butyltin(IV) dicarboxylates of diphenic acid (biphenyl-2,2′-dicarboxylic acid), thiodiacetic acid and maleic anhydride with succinyl, adipoyl and sebacoyl dichlorides. The compounds have been characterized with the help of elemental analyses and spectral data (mass, IR, ^IH and ¹³C NMR).     

Tantalum(v) oxoalkoxides. Synthesis and structure

Anodic oxidation of tantalum in isopropyl alcohol or prolonged reflux of an alcohol solution of Ta(OPrⁱ)₅ afford crystalline oxoisopropoxide Ta₂O(OPrⁱ)₈ · PrⁱOH (1). In its molecule, two octahedra about Ta atoms are linkedvia the shared edge [(OPrⁱ)O]. Compound1 is the first example of oxoalkoxide containing such a small number of metal atoms. Unlike the known polynuclear molecules M _n O _m (OR) _p , oxoalkoxide1 is stable in solutions; on transition to the gas phase, this compound is desolvated to form a very stable molecule Ta₂O(OPrⁱ)₈ (apparently, consisting of two octahedra with a shared edge). According to the data of mass spectrometry, analogous molecules exist in the gas phase over Ta(OAlk)₅ (Alk = Me, Et, Prⁱ, or Bu¹¹). When compound1 is heated invacuo (10^–2–10^–3 Torr), Ta(OPrⁱ)₅ is sublimated. Crystals of Ta₇O₉(OPrⁱ)₁₇ (2) were formed upon prolonged storage of solutions of1 in PrⁱOH. Heptanuclear molecule2 consists of two [Ta₄] tetrahedra with a shared vertex. These tetrahedra are additionally linked togethervia one ₃-oxo and two ₂-OPrⁱ groups. Complex2 is a representative of heptameric oxoalkoxides of a new structural type.Deceased in I995.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 1, pp. 125–131, January, 1996.     

Synthesis and Characterization of Th(IV) and U(VI) Complexes with O-Vanillin-P-Phenylenediamine

Two new solid complexes, [ThL(NO₃)₂](NO₃)₂, [UO₂L(NO₃)]NO₃ (L=o-vanillin-p-phenylenediamine) have been synthesized and characterized by elemental analyses, DTA-TG, IR spectra, UV spectra and molar conductance. Possible structures of the two complexes are proposed.     

对位取代苯酚氧甙类化合物的相转移催化合成与结构表征

为了获得新的活性化合物，以溴代四乙酰葡萄糖和对位以代苯酚为原料，溴化 四丁基铵为相转移催化剂，合成了18个对位取代苯酚氧甙类化合物，其产率为20. 0%。化合物结构经元素分析，IR，^1H NMR表征，化合物的生物活性经初步测定， 其中四种有抑制端粒酶活性。     

二正丁基锡水杨醛缩对氨基苯甲酸酯配合物的合成、表征及结构研究

The title complex {[ⁿBu₂Sn(2-OHC₆H₄CH=NC₆H₄COO)]₂O}₂·2H₂O was synthesized by the reaction of N-(4-carboxyphenyl)-salicylideneimine with dibutyltin(IV) oxide in 1∶1 molar ratio. The compound has been characterized by elemental analysis, IR, ¹H NMR spectra and X-ray single crystal diffraction. It crystallizes in triclinic system with space group P1. The crystal data are: a=1.242 9(2) nm, b=1.261 3(2) nm, c=1.594 9(3) nm, α=102.06(2)°, β=92.884(3)°, γ=95.939(3)°, Z=2, D_c=1.342 g·cm^-3, F(000)=1 000, V=2.425 2(7) nm³, R₁=0.041 5, wR₂=0.104 4. The compound is in centro-symmetric dimer structure mode with a four-member central endo-cyclic Sn₂O₂ unit in which the bridging oxygen atoms are tri-coordinated. All the tin atoms are five-coordinated with geometry of distorted trigonal bipyramid. CCDC:286105.     

Synthesis and Spectroscopic Characterisation of a New Class of Heterobimetallic Zirconocene(IV) Compounds

Reactions of Cp₂ZrCl₂ with homometallic complexes of aluminium containing one residual hydroxy group Al(OGO)(OGOH) and Al(L)(OGOH) [where G=G¹=CMe₂CMe₂ (1a); G=G²=CMe₂CH₂CHMe (1b); G= G³=CMe₂CH₂CH₂CMe₂ (1c) and L=L¹=OC₆H₄CH=NCH₂CH₂O, G=G¹ (2a); L=L¹, G=G² (2b); L=L¹, G=G³ (2c); L=L²=OC₁₀H₆CH=NCH₂CH₂O, G=G¹ (2d); L=L², G=G² (2e); L=L², G=G³ (2f)] in THF using Et₃N as HCl acceptor affords novel heterobimetallic compounds of the types Al(OGO)₂Zr(Cl)Cp₂ and Al(L)(OGO)Zr(Cl)Cp₂, respectively. All of these derivatives have been characterised by elemental analyses, molecular weight measurements, and spectroscopic [IR, NMR (¹H and ²⁷Al)] studies.     

Xenon(II) Polyfluoridotitanates(IV): Synthesis and Structural Characterization of [Xe2F3]+ and [XeF]+ Salts

Thermal reaction between XeF₂ and excess TiF₄ resulted in the unexpected formation of a highly ionized Xe^II species. The products [Xe₂F₃][Ti₈F₃₃] and [XeF]₂[Ti₉F₃₈] represent the first examples of [Xe₂F₃]⁺ and [XeF]⁺ compounds, which differ from known Xe^II salts containing discrete fluoride anions with pentavalent metalloid/metal centers. A new structural type of 2D polyanion [Ti₈F₃₃]^? and the formation and structure of the novel 1D [Ti₉F₃₈]^2? are discussed. Both products were characterized by single‐crystal X‐ray analysis and Raman spectroscopy.     

Synthesis and Characterization of Heterobimetallic Aluminum‐Germanium(IV) Disulfides

Three heterobimetallic aluminum‐germanium(IV) disulfides are synthesized. The reaction of {LAl[(SLi)₂(THF)₂]}₂ ( 1 ) (L = HC(CMeNAr)₂, Ar = 2,6‐iPr₂C₆H₃) with Ph₂GeCl₂, Me₂GeCl₂, and GeCl₄, respectively, in THF afforded LAl(μ‐S)₂GePh₂ ( 2 ), LAl(μ‐S)₂GeMe₂ ( 3 ) and LAl(μ‐S)₂Ge(μ‐S)₂AlL ( 4 ) in good yields. Compounds 2 , 3 and 4 were investigated by elemental analysis, NMR, EI‐MS and 3 was also characterized by single crystal X‐ray structural analysis.