Synthesis and Characterization of Ferrocenyl Substituted Styryl Octasilsesquioxane

4-(2-Ferrocenylethenyl)-phenyl-POSS Fc-CH=CH-C6H6-(C5H9)7Si8O12 (FEPS, Fc: ferrocene), containing metal and C=C double bond, was firstly synthesized as a mixture of E/Z isomers by the Wittig reaction. The chemical structure of FEPS was characterized by FTIR, 1H-, 13Cand 29Si-NMR.     

Synthesis and Characterization of New α,ω-Bis(Maleimide-Ester) Substituted Siloxane Oligomers

Abstract

Organofunctional siloxane oligomers containing maleimide were synthesized by condensation reaction of α. ω-hydroxypropylsiloxane oligomers with n-[4-(chlorocarbonyl)phenyl]maleimide. A model compound [bis(maleimide-ester)disiloxane] was obtained to facilitate the characerization of the oligomers. Then, the heterogeneous catalyzed ring-opening cationic polymerization technique was applied to obtain an oligomer starting from the model compound and octamethylcyclotetrasiloxane.

The structures of the resulting oligomers were confirmed by elemental analysis, IR and ¹H-NMR spectroscopy. They were characterized by determining softening points, solubility and studying their thermal behavior by thermogravimetric (TGA and differential scanning calorimetry (DSC) measurements.     

Synthesis and Characterization of Magnesium Substituted Aluminophosphate Molecular Sieves with AEL Structure

MAPO-11 molecular sieves were synthesized by hydrothermal methods. The influence of precursor of magnesium, Mg/Al ratio, synthesis temperature, synthesis time and the type of template on the formation and properties of MAPO-11 molecular sieves was examined. The samples were characterized by the techniques of X-ray diffraction (XRD), scanning electron microscopy (SEM), thermogravimetric/differential thermogravimetric analysis (TG-DGA), etc. The results show that the shape and size of crystal were influenced by the precursor of Mg, the Mg/Al ratio and the type of template, and the TG-DGA analysis shows that MAPO-11 molecular sieves as-synthesized have poor thermal stability.     

Synthesis and Characterization of AmmoniumMolybdostibophosphate

以简单酸铵盐为原料，采用不同的磷钼锑比，在控制反应温度７０～８０℃、溶液酸度２．５～３．０Ｎ的条件下，进行分步反应的方法，首次合成了以锑原子取代的钼锑磷杂多酸铵。通过元素分析，确定了它们的组成；用ｐＨ滴定曲线、电子吸收光谱和Ｘ射线等方法研究了它们的性质。     

Synthesis and Characterization of One-dimensional and Two-Dimensional Porphyrin Polymers (Ⅰ)

Porphyrin polymers are of interest in relation to conductive materials[1, 2], catalysts for photosynthetic charge separation[3], or the fundamental features in biological systems[4]. There have been many versatile studies about them[5.6]. The one-dimensional "Shish Kebab"porphyrin polymers synthesized with a new method different from those reported and Schiff-base porphyrin polymers with two-dimensional nano-structure have provided a new field of study. The present paper covers highly ordered…     

Synthesis and Characterization of Poly(hydrogen halide) Halogenates (–I)

Herein, we report the synthesis and characterization of a variety of novel poly(hydrogen halide) halogenates (−I). The bifluoride ion, which is known to have the highest hydrogen bond energy of ≈160 kJ mol⁻¹, is the most famous among many examples of [X(HX)_n]⁻ anions (X=F, Cl) known in the literature. In contrast, little is known about poly(hydrogen halide) halogenates containing two different halogens, ([X(HY)_n]⁻). In this work we present the synthesis of anions of the type [X(HY)_n]⁻ (X=Br, I, ClO₄; Y=Cl, Br, CN) stabilized by the [PPh₄]⁺ and [PPN]⁺ cation. The obtained compounds have been characterized by single-crystal X-ray diffraction, Raman spectroscopy and quantum-chemical calculations. In addition, the behavior of halide ions in hydrogen fluoride was investigated by using experimental and quantum-chemical methods in order to gain knowledge on the acidity of hydrogen halides in HF.     

Synthesis and Characterization of 2-Decyl-DTPA and Its Gd(Ⅲ) Chelate

IntroductionGadoliniumchelatesareveryimportantbecauseoftheirpotentialbiologicalapplicationsintheareaofmagneticresonanceimaging(MRI) .Thegadoliniumchelateofdiethylenetriaminepentaaceticacid(DTPA )wasthefirstMRIcontrastagentinclinicaluse .How ever,Gd DTPA ,asanextracellularcontrastagent,hasnoliver specificity .Theintroductionofanaddi tionallipophilicsubstitutenttoanyoneofthefivemethylenesoftheaceticacidresiduesortoanyoneofthefourcarbonatomsofthebackboneinDTPAmaychangethetissuespecificity…     

Synthesis and Characterization of 2-Decyl-DTPA and Its Gd(Ⅲ) Chelate

The present paper covers the synthesis and the characterization of ligand 2-decyl-3, 6, 9-tris(carboxymethyl)-3,6,9-triazaundecan-1,11-dioic acid, H5L, and its Gd(Ⅲ) chelate. The protonation constants for H5L(lgKHi=10.90, 8.50, 4.55, 2.92, 2.20) and the stability constant for GdL2- (lgKGdL2-=22.80) were determined by means of potentiometric titration. They are similar to the corresponding values of DTPA and Gd-DTPA, respectively. The results obtained show that the basicity of the ligand and the stability constant of its Gd(Ⅲ) chelate are not obviously altered after the introduction of a linear chain decyl group into the terminal acetic acid residue of DTPA. The Gd(Ⅲ) chelate may be a potential contrast agent with liver-specificity for magnetic resonance imaging(MRI).     

Syntheses,Structures and Magnetic Properties of Three New Extended Iron‐containing Heteropolytungstates

Three new extended iron‐containing heteropolytungstates were synthesized and structurally characterized: K₆[{Fe^II(H₂O)₄}₂(H₂W₁₂O₄₂)]·15H₂O ( 1 ), Na₅[{Fe(H₂O)₃}₂{Fe(H₂O)₄}_0.5(H₂W₁₂O₄₂)]·30H₂O ( 2 ) and (H₃O)⁺₂[{Fe(H₂O)₄Fe(H₂O)₃}₂(H₂W₁₂O₄₂)]·20H₂O ( 3 ). 1 and 3 crystallize in the monoclinic system, space group P2₁/n with a = 14.9967(5), b = 10.3872(3), c = 18.8237(6)Å, β = 93.407(1)°, V = 2927.1(2)ų and D_c = 4.151 g cm^—3 for 1 , and space group P2₁/c with a = 12.1794(4), b = 22.4938(4), c = 11.6941(3) Å, β = 105.731(2)°, V = 3083.7(1) ų, and D_c = 4.043 g cm^—3 for 3 . 2 is triclinic, space group P1¯, with a = 12.121(2), b = 12.426(3), c = 13.247(3)Å, α = 68.33(3), β = 71.33(3), γ = 71.44(3)°, V = 1710.7(6)ų and D_c = 3.735 g cm^—3. In all cases, the structures are based on paradodecatungstate polyoxoanions, which are linked by iron ions into chains, layers and a three‐dimensional structure for 1 , 2 and 3 , respectively.     

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.     

钴镍取代杂多酸盐甘氨酸超分子化合物的合成及性质

Supermolecular compounds of glycine monosubstituted heteropolytungstates isomer with Keggin structure β_i-K_6-n(HGly)_n[SiW₁₁M(H₂O)O₃₉]·xH₂O (M=Co²⁺, Ni²⁺； β_i=β₂, β₃) were synthesized and characterized by means of elementary analysis, IR, UV, TG-DTA, X-ray diffraction, polarography and CV. The results indicate that glycin combines the electrostatic effect with heteropolytungstates isomer. The heteropoly anion still remains its Keggin structure in supermolecular compounds. The electrochemical behavior of the compound in 1 mol·L^-1 HAc-NaAc shows that two redox waves correspond to two two-electron processes attributing to the reduction of [SiW₁₁Co(H₂O)O₃₉]^6-. Steady-state fluorescence spectrum shows two intenser fluorescence emission peaks in 447 nm and 486 nm appeared after the supermolecular compound being excited by the excitation wavelength in 274 nm.     

Synthetic aspects of tetraorganotins and organotin(IV) halides

Organotin(IV) compounds are being used for many applications, e.g., as stabilizers in PVC, in anti-fouling paints and coatings for the protection of ship hulls and as precursors for SnO₂-coatings on glass. Tetraorganotins and especially organotin(IV) halides often serve as synthetic precursors. A wide range of methods for the synthetic preparation of these compounds has been developed since the 1940s. This review gives an overview of the available routes for the preparation of organotin(IV) compounds and discusses their selectivity and yield. In particular, monoorganotin trihalides are often not accessible in high yield.     

Synthesis,characterization and cytotoxicity of fluorescent organotin complexes of terpyridine derivatives

Five organotin complexes of terpyridine derivatives were synthesized and characterized. The mononuclear Sn（IV） complexes were six-coordinated adopting a distorted octahedral coordination geometry. A brief outline of the fluorescence spectra and the in vitro cytotoxicity of the Sn（IV） complexes have been given.     

Synthesis and structural characterization of monomeric and polymeric supramolecular organotin(IV) 4-chlorophenylethanoates

Four monomeric [n-Bu₂SnL₂ (1), Et₂SnL₂ (2), Me₂SnL₂ (3), and n-Oct₂SnL₂ (7)] and three polymeric {[n-Bu₃SnL]_n (4), [Me₃SnL]_n (5), and [Ph₃SnL]_n (6)} organotin(IV) carboxylates, where L?=?4-chlorophenylethanoate, were synthesized and characterized by elemental analysis, FT-IR, and multinuclear NMR (¹H, ¹³C, and ¹¹⁹Sn). Compounds 2 and 5 were also analyzed by X-ray single-crystal analysis showing monomeric and zigzag structures, respectively. Two types of O…H (2.641?Å) and Cl…H (2.943?Å) non-covalent interactions generate a 2-D supramolecular structure for 2. Layer-by-layer supramolecular structure was observed for 5 in which polymeric chains are connected via non-covalent interactions {Cl…H (2.869?Å), H…π (2.899?Å)}, and unconventional dihydrogen {H…H (2.381?Å)} interactions.     

Synthesis and structural characterization of organotin(IV) carboxylates based on different heterocyclic substituents

Six novel organotin(IV) carboxylates have been successfully synthesized, namely, the polymer (C₆H₅)₃Sn(L1)_∞ (1) [HL1 = 4-imidazolyl benzoic acid], the mononuclear (C₆H₅)₃Sn(L2) (2) [HL2 = 4-pyrazolylbenzoic acid], (C₆H₅)₃Sn(L3)·CH₃OH (3) [HL3 = 4-triazolylbenzoic acid] and (C₆H₅)₃Sn(L4) (4) [HL4 = 4-tetrazolyl benzoic acid] and the tetranuclear [(n-Bu₂Sn)₄(L2)₂O₂(OCH₃)₂] (5) and [(n-Bu₂Sn)₄(L3)₂O₂(OCH₃)₂] (6). X-ray diffraction analyses show 1D infinite chain of polymer 1, single molecular structures of isomorphous complexes 2 and 4, single molecule structures of complex 3 containing solvent CH₃OH molecule and similar ladder-type structures of complexes 5 and 6. The photoluminescence of ligands and 1-6 were also measured in the solid state at room temperature.     

Assembly of Three Scandium-containing Heteropolytungstates Based on a Building-block Synthetic Strategy

Three novel scandium-containing heteropolytungstates[Sc₃(H₂O)₃NO₃(PW₉O₃₄)₂]^10-(1a),[Sc₈(H₂O)₂(GeW₉O₃₄)₂(GeW₆O₂₆)₂]^12-(2a) and[Sc₁₁(W₆O₁₀)₂(OH)₂(H₂O)₁₆(BiW₉O₃₃)₆]^27-(3a) were synthesized by reactions of Sc^III ions with trilacunary Keggin precursors,[A-α-XW₉O₃₄]^n-(X=P, Ge, n=9, 10) or[B-α-BiW₉O₃₃]^9-, in NaOAc/HOAc buffer solution under conventional synthetic condition, respectively. All the three compounds were characterized by means of single-crystal X-ray diffraction(XRD), Fourier transform-infrared(FTIR) spectroscopy ultraviolet-visible(UV-Vis) spectroscopy, elemental analysis, and thermogravimetric analysis. The aqueous solution stability of the sandwich polyanion[Sc₃(H₂O)₃NO₃(PW₉O₃₄)₂]^10- was also verified by electrospray ionization mass spectrometry(ESI-MS) due to its good solubility in water.