Synthesis and Structure Characterization of some Triorganotin Esters of Heteroaromatic Carboxlic Acid and Crystal Structure of Triphenyltin Esters 5-Chloro-6-Hydroxynicotinic Acid

2012 ◽  
Vol 466-467 ◽  
pp. 463-468
Author(s):  
Hong Tao Gao

Reactions of (R3Sn)2O (R=Ph, 2-ClC6H4CH2, 2-FC6H4CH2, 4-CNC6H4CH2) with 5-chloro-6-hydroxynicotinic acid in 1/2 stoichiometry yielded eight triorganotin compounds. These compounds have been characterized by elemental analysis, IR and NMR spectroscopy. The crystal structures of triphenyltin esters of 5-chloro-6-hydroxynicotinic acid were determined by single crystal X-ray diffraction. In the compound, the tin atoms are rendered five-coordinated in a trigonal bipyramidal structure by coordinating though the three phenyl carbon atoms and two oxygen atoms one from carboxylate and other from the phenolic hydroxide. The resulting structure is one-dimensional linear polymers through an interaction between the O atoms of phenolic hydroxide and tin atoms of an adjacent molecule.

2013 ◽  
Vol 834-836 ◽  
pp. 309-314
Author(s):  
Zi Fan Xiao ◽  
Jin Shu Cheng ◽  
Jun Xie

A glass-ceramic belonging to the CaO-Al2O3-SiO2(CAS) system with different composition of spodumene and doping the Li2O with amount between 0~2.5 % (mass fraction) were prepared by onestage heat treatment, under sintering and crystallization temperature at 1120 °C for two hours. In this paper, differential thermal analysis, X-ray diffraction, scanning electron microscopy, energy dispersive spectrometry and bending strength test were employed to investigate the microstructure and properties of all samples. β-wollastonite crystals were identified as the major crystalline phases, and increasing Li2O was found to be benefit for the crystallization and tiny crystalline phases remelting, resulting in the content of major crystalline phases increased first and then decreased with increasing the expense of spodumene. Meanwhile, the crystal size can be positively related with the content of Li2O. The preferable admixed dosage of spodumene can be obtained, besides the strength of glass-ceramics can be more than 90 MPa.


2011 ◽  
Vol 322 ◽  
pp. 369-372
Author(s):  
Zhi Xiang Ji

A chain Ni (II) coordination polymer material was prepared and characterized by elemental analysis and single-crystal X-ray diffraction. It crystallizes in monoclinic, space group C2/c with a = 1.24348(13) nm, b = 1.29477(12) nm, c = 1.51480(17) nm and Dc = 1.401 g•cm-3. The results of structural analysis indicated that each Ni (II) ion forms six-coordinated with nitrogen atoms of pyridine and thiocyanate, and the Ni (II) coordination polymer material formed one dimensional chain structure by the interaction of pyridine rings.


2018 ◽  
Vol 34 (6) ◽  
pp. 3088-3094 ◽  
Author(s):  
Abdul Wahid Wahab ◽  
Abdul Karim ◽  
Nursiah La Nafie ◽  
Nurafni Nurafni ◽  
I. Wayan Sutapa

Silver nanoparticles have been synthesized by reduction method using extract of Muntingia calabura L. leaf a bioreductor. The process of silver nanoparticles formation was monitored by UV-Vis method. The results showed that the absorbance values increased according to the increase of reaction time. Maximum absorption of silver nanoparticle was obtained at a wavelength of 41-421 nm. The size of silver nanoparticles was determined using a PSA (Particle Size Analyzer) with a particle size distribution of 97.04 nm. The functional groups compound that contribute in the synthesis was analyzed using Fourier Transform Infrared Spectroscopy (FTIR). Morphology of the silver nanoparticles was observed by an Scanning Electron Microscope instrument and the structure characterization of the compounds were analyzed using X-Ray Diffraction. The glucose nanosensor based on silver nanoparticles have the measurement range of 1 mM - 4 mM with the regretion (R2) is 0,9516, the detection limit of sensor is 3,2595 mM, the sensitivity of sensor is 2,0794 A. mM-1. mM-2.


2014 ◽  
Vol 936 ◽  
pp. 915-918
Author(s):  
Hui Duan Li

A novel zinc organophosphonate was synthesized under solvothermal conditions by using [piperazine-1,4-diyldi (methylene)] bis (phosphonic acid) as a organic ligand. Single-crystal X-ray diffraction analysis reveals that compound 1 crystallized in the triclinic space group P-1 (No. 2). Compound 1 formulated as Zn (O3PCH2NHC4H8NHCH2PO3)·H2O. Compound 1 featured a 3D open-framework. Notably, the structure of compound 1 featured one-dimensional channel in the [00 direction. Water molecules were located in these channels. Further characterizations of compound 1 have been performed, including X-ray powder diffraction, IR, ICP and CHN analyses.


2014 ◽  
Vol 1004-1005 ◽  
pp. 542-545
Author(s):  
Ya Bing Liu ◽  
Li Guang Xiao

A new bi-capped Keggin heteropoly molybdovanadated derivative, [Co (en)3]2[SiMo8V6O42]∙6H2O (1) (en = ethylendiamine) has been hydrothermally synthesized and structurally characterized by the elemental analysis, IR, XPS and single crystal X-ray diffraction. The crystal structure analysis reveals that compound 1 consists of [Co (en)3]2+transition metal coordination fragment and the [SiMo8V6O42]4-building blocks, which are linked together via hydrogen-bonding interactions to form a new 3-D supramolecular networks.


2021 ◽  
Vol 26 (1(77)) ◽  
pp. 16-25
Author(s):  
Yu. I. Slyvka ◽  
E. A. Goreshnik ◽  
N. T. Pokhodylo ◽  
М. G. Mys’kiv

This work is focused on the synthesis and structure characterization of the novel Cu(I) π-complex [Cu2(Thiaz1)2(ClO4)2] (1) with 2-allylamino-5-methyl-1,3,4-thiadiazole (Thiaz1) ligand. The crystals of the compound were obtained by means of the alternating-current electrochemical technique and studied using single crystal X-ray diffraction. The crystal structure of the complex 1 is constructed from the centrosymmetric dimers, in which two copper(I) ions are coordinated by two Thiaz1 molecules through thiadiazole N atoms and allylic C=C bond. Energy framework computational analysis for structure 1 has been performed.  


2020 ◽  
Vol 51 (5) ◽  
pp. 1420-1427
Author(s):  
Al-Sabbagh & et al.

The element-substituted calcium Deficient hydroxyapatite samples were synthesized using liquid-phase precipitation method. Different element ions (Mg+2, Zn+2, and Cu+2) were added at constant ratio (5% wt.). The phase composition of the element-substituted calcium hydroxyapatite samples was investigated by using X-ray diffraction. A comparison with known characteristics of the synthetic ion-substituted forms of hydroxyapatite was conducted. It was determined, that the investigated materials are single-phase solid solutions of the element-substituted hydroxyapatite. By the methods of IR spectroscopy and Raman scattering (RS) it was discovered the dependence of incorporation of the carbonate anion that occupies a positions of phosphorus-oxygen groups in the hydroxyapatite structure as a result of embedding element ions (Zn+2, Cu+2, Mg+2) in the crystal lattice. Besides, It was determined, that the ratio of the intensities for the C03 group mode to the P04 groups mode depended on the nature of the element atom, which replace the calcium in the lattice of HAP, and reduced by substituting the calcium atoms by the atoms of Zn, Cu, and Mg from 0.15 to 0.06. Modeling of the vibration modes of Raman spectroscopy showed that incorporation of carbon atoms to the hydroxyapatite structure correlate with the Zn, Cu and Mg atomic radius, charge, and activity   


Crystals ◽  
2018 ◽  
Vol 8 (8) ◽  
pp. 305
Author(s):  
Le-Qing Fan ◽  
Xiao-Tong Zhu

The design and synthesis of heterometallic iodoplumbates have attracted much interest due to the diverse structures and significant physical properties. A Pb/CuI/I heterometallic iodoplumbate, [PbCu2I4(bipy)]n (1) (bipy = 2,2′-bipyridine), has been synthesized by solvothermal reaction of PbI2, Cu(NO3)2, bipy, and HI, and characterized by single-crystal X-ray diffraction, powder X-ray diffraction, and thermogravimetric analysis. This compound exhibits one-dimensional neutral structure, which is built upon the linkages of Pb/I chains, Cu/I chains, and Cu(bipy) units. The yellow compound has an optical bandgap of 2.32 eV and shows fluorescent emission at 610 nm which is assigned to iodide-to-copper charge transfer.


2011 ◽  
Vol 66 (4) ◽  
pp. 387-391
Author(s):  
Jinling Miao ◽  
Yong Nie ◽  
Haiyan Chen ◽  
Daqi Wang ◽  
Markus Enders ◽  
...  

The reaction of closo-B10H102− with PtCl2(PPh3)2 in the presence of MeCOSH afforded the title platinaborane nido-7,7-(PPh3)2-7-PtB10H11-11-OC(O)Me (1), which has been characterized by IR and NMR spectroscopy, MS, elemental analysis, and single-crystal X-ray diffraction. In contrast to the known products having exo-polyhedral Pt-S-C-O-B ring(s) from the same reaction with Ph- COSH, compound 1 has a B-acetoxy group on the open PtB4 face of the nido-PtB10 cluster. The structure of 1 features both intramolecular/intermolecular C-H· · ·O hydrogen bonds and intramolecular C-H· · ·H-B dihydrogen bonds, which link the molecules into a 1-D chain structure.


Author(s):  
Vânia Denise Schwade ◽  
Bárbara Tirloni

Pyrimidine-2-thione (HSpym) reacts with lead(II) thiocyanate and lead(II) bromide in N,N-dimethylformamide (DMF) to form poly[(μ-isothiocyanato-κ2 N:S)(μ4-pyrimidine-2-thiolato-κ6 N 1,S:S:S:S,N 3)lead(II)], [Pb(C4H3N2S)(NCS)] n or [Pb(Spym)(NCS)] n , (I), and the polymeric one-dimensional (1D) compound catena-poly[[μ4-bromido-di-μ-bromido-(μ-pyrimidine-2-thiolato-κ3 N 1,S:S)(μ-pyrimidine-2-thione-κ3 N 1,S:S)dilead(II)] N,N-dimethylformamide monosolvate], {[Pb2Br3(C4H3N2S)(C4H4N2S)]·C3H7NO} n or {[Pb2Br3(Spym)(HSpym)]·DMF} n , (IIa), respectively. Poly[μ4-bromido-di-μ3-bromido-(μ-pyrimidine-2-thiolato-κ3 N 1,S:S)(μ-pyrimidine-2-thione-κ3 N 1,S:S)dilead(II)], [Pb2Br3(C4H3N2S)(C4H4N2S)] n or [Pb2Br3(Spym)(HSpym)] n , (IIb), could be obtained as a mixture with (IIa) when using a lesser amount of solvent. In the crystal structures of the pseudohalide/halide PbII stable compounds, coordination of anionic and neutral HSpym has been observed. Both Spym− (in the thiolate tautomeric form) and NCS− ligands were responsible for the two-dimensional (2D) arrangement in (I). The Br− ligands establish the 1D polymeric arrangement in (IIa). Eight-coordinated metal centres have been observed in both compounds, when considering the Pb...S and Pb...Br interactions. Both compounds were characterized by FT–IR and diffuse reflectance spectroscopies, as well as by powder X-ray diffraction. Compound (IIa) and its desolvated version (IIb) represent the first structurally characterized PbII compounds containing neutral HSpym and anionic Spym− ligands. After a prolonged time in solution, (IIa) is converted to another compound due to complete deprotonation of HSpym. The structural characterization of (I) and (II) suggests HSpym as a good candidate for the removal of PbII ions from solutions containing thiocyanate or bromide ions.


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