Synthesis and Characterization of Tetraphenylphosphonium Tetraazidoborate

2002 ◽  
Vol 57 (6) ◽  
pp. 621-624 ◽  
Author(s):  
Wolfgang Fraenk ◽  
Heinrich Nöth ◽  
Thomas M. Klapötke ◽  
Max Suter
Keyword(s):  
Single Crystal ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray

AbstractTetraphenylphosphonium tetraazidoborate, [P(C6H5)4][B(N3)4], was obtained from B(N3)3 - in situ prepared from BH3 · O(C2H5)2 and HN3 - and [P(C6H5)4][N3]. Recrystallization from an acetonitrile / hexane mixture yielded colorless crystals in 60% yield. The molecular structurewas determined by single crystal X-ray diffraction and the [B(N3)4]- anionwas shown to possess S4 symmetry.

Synthesis and Characterization of the PANI/ITO Conducting Nanocomposites

2010 ◽  
Vol 663-665 ◽  
pp. 542-545 ◽  
Author(s):  
Bing Jie Zhu ◽  
Xin Wei Wang ◽  
Mei Fang Zhu ◽  
Qing Hong Zhang ◽  
Yao Gang Li ◽  
...  
Keyword(s):  
Doping Concentration ◽  
In Situ Polymerization ◽  
Synthesis And Characterization ◽  
Conductivity Measurements ◽  
X Ray Diffraction ◽  
X Ray ◽  
Maximum Conductivity ◽  
Scanning Electron

The PANI/ITO conducting nanocomposites have been synthesized by in-situ polymerization. The obtained nanocomposites were characterized by X-ray diffraction pattern, scanning electron microscopy and Fourier transform infrared. Electrical conductivity measurements on the samples pressed into pellets showed that the maximum conductivity attained 2.0 ± 0.05 S/cm for PANI/ITO nanocomposites, at ITO doping concentration of 10 wt%. The results of the present work may provide a simple, rapid and efficient approach for preparing PANI/ITO nanocomposites.

Synthesis and characterization of the pentazolate anion cyclo-N5ˉ in (N5)6(H3O)3(NH4)4Cl

Science ◽  
2017 ◽  
Vol 355 (6323) ◽  
pp. 374-376 ◽  
Author(s):  
Chong Zhang ◽  
Chengguo Sun ◽  
Bingcheng Hu ◽  
Chuanming Yu ◽  
Ming Lu
Keyword(s):  
Thermal Analysis ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Decomposition Temperature ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Onset Decomposition Temperature ◽  
The Stability

Pentazole (HN5), an unstable molecular ring comprising five nitrogen atoms, has been of great interest to researchers for the better part of a century. We report the synthesis and characterization of the pentazolate anion stabilized in a (N5)6(H3O)3(NH4)4Cl salt. The anion was generated by direct cleavage of the C–N bond in a multisubstituted arylpentazole using m-chloroperbenzoic acid and ferrous bisglycinate. The structure was confirmed by single-crystal x-ray diffraction analysis, which highlighted stabilization of the cyclo-N5ˉ ring by chloride, ammonium, and hydronium. Thermal analysis indicated the stability of the salt below 117°C on the basis of thermogravimetry-measured onset decomposition temperature.

Synthesis and Characterization of Copper(II) Complexes with Long Chain Dithiocarbamates

2014 ◽  
Vol 976 ◽  
pp. 164-168 ◽  
Author(s):  
Nayely Torres-Gomez ◽  
Alfredo R. Vilchis-Nestor ◽  
Rosa Maria Gomez-Espinosa ◽  
Ivan Garcia-Orozco
Keyword(s):  
Infrared Spectroscopy ◽  
Copper Complexes ◽  
Nanocrystalline Structure ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Long Chain ◽  
Scanning Electron

Copper complexes of dithiocarbamates ligands were obtained from RNH2 (R = C6H13-, C12H25- y C18H37-) and an excess of CS2 in the presence of NaOH. Sodium hexyldithiocarbamate is not possible to isolate from solution but the other two were obtained and characterizedby infrared spectroscopy, UV-vis and powder X-ray diffraction. Copper complexes were obtained in situ from ligand solution as greenish powders. All the complexes were characterized by infrared spectroscopy, UV-vis, powder X-ray diffraction and Scanning Electron Microscopy. The complexes show an amorphous phase in the case of DCu12 and nanocrystalline structure for DCu18, as observed in XRD.

scholarly journals Lactide polymerization with iron alkoxide complexes

2015 ◽  
Vol 93 (6) ◽  
pp. 594-601 ◽  
Author(s):  
Arek Keuchguerian ◽  
Berline Mougang-Soume ◽  
Frank Schaper ◽  
Davit Zargarian
Keyword(s):  
Single Crystal ◽  
Room Temperature ◽  
Side Reactions ◽  
X Ray Diffraction ◽  
Iron Cluster ◽  
X Ray ◽  
H Nmr ◽  
Exchange Product

This report presents the results of a study on the preparation of iron alkoxide complexes chelated by diiminopyridine ligands and their role in the room temperature polymerization of rac-lactide. Reaction of N,N′-(p-R-C6H4CH2)2-diiminopyridines (R = H (1), F (2)) with FeX2 (X = Cl, Br) yielded the homoleptic complexes [(1)2Fe][FeX4] or [(2)2Fe][FeX4], respectively. Treating the latter with Na[BPh4] afforded the anion exchange product [(2)2Fe][BPh4]2, which was characterized by 1H NMR and absorption spectroscopy, combustion analysis, and single crystal X-ray diffraction. Various attempts to grow crystals of [(1)2Fe][FeX4] and [(2)2Fe][FeX4] culminated in the isolation of single crystals of [(2)2Fe][Cl6Fe2O] that was characterized by X-ray diffraction. Attempted synthesis of well-defined, mononuclear alkoxide derivatives from [(1)2Fe]2+ or [(2)2Fe]2+ gave mostly intractable products, but in one case we obtained the crystallographically characterized sodium iron cluster Na4Fe2(OC6H4F)8(THF)2. An aryloxide derivative proved accessible by reaction of NaOC6H4F with the mono-ligand precursor LFeCl2 (L = N,N′-dimesityl-diiminopyridine), but characterization of LFe(OC6H4F)2 was limited to a single crystal X-ray diffraction analysis, owing to unsuccessful attempts at isolating pure samples. The difficulties encountered in the isolation of pure alkoxide derivatives prompted us to use in-situ generated LFe(OEt)2 for studying the polymerization of rac-lactide. This system was found to be moderately active at room temperature and with a slight preference for the formation of a heterotactic polymer (Pr = 0.54–0.65). Large polydispersities of 1.5–2.0 indicated the presence of transesterification side-reactions, which were confirmed by the presence of peaks with m/z = n 144 + M(EtOH) + M(Na+) and m/z = (n + 0.5) 144 + M(EtOH) + M(Na+) in MALDI-MS.

Synthesis and Characterization of the nido-Platinaborane 7,7-(PPh3)2-7-PtB10H11-11-OC(O)Me

2011 ◽  
Vol 66 (4) ◽  
pp. 387-391
Author(s):  
Jinling Miao ◽  
Yong Nie ◽  
Haiyan Chen ◽  
Daqi Wang ◽  
Markus Enders ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Chain Structure ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ir And Nmr Spectroscopy

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.

Synthesis and Characterization of Composite Structure Zeolite Y

2011 ◽  
Vol 233-235 ◽  
pp. 1790-1793 ◽  
Author(s):  
Wei Shen ◽  
Bao Jian Shen
Keyword(s):  
Silica Gel ◽  
Composite Structure ◽  
Zeolite Y ◽  
Synthesis And Characterization ◽  
Organic Additives ◽  
X Ray Diffraction ◽  
Y Zeolite ◽  
X Ray

Y zeolite was synthesized form silica gel microsphere by in- situ hydrothermal method, with appropriate amount of other constituents, such as sodium silicate, water, without adding any organic additives. The as-synthesized samples were characterized using powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and N2 sorption. The results show that the synthesized sample not only has a composite structure with zeolite Y and silica gel, but also retains the shape of silica gel microsphere. The pore distribution of the composite materials indicated that the composite material contains two types of pore that are micropores and large pores.

Synthesis and characterization of dicarboranylmethylammonium polyoxometallates

2010 ◽  
Vol 75 (11) ◽  
pp. 1075-1096 ◽  
Author(s):  
Ramón Macías ◽  
John D. Kennedy ◽  
Jonathan Bould ◽  
Mark Thornton-Pett
Keyword(s):  
Hydrogen Bonds ◽  
Single Crystal ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Pyridinium Cation ◽  
Network Of Hydrogen Bonds ◽  
Work Up ◽  
Acetone Hexane

The reaction of [C2B10H11CH2NH3]Cl (3) with [NH4]6[Mo7O24][H2O]4 in water instantly afforded a white precipitate: crystallization from acetone–hexane thence gave the hybrid dicarborane octamolybdate salt, [C2B10H11CH2NH3]2[C2B10H11CH2NH=CMe2]2[Mo8O26][Me2CO]4.5 (5), whereas crystallization from acetonitrile–ether gave three further salts: [C2B10H11CH2NH3]2[C2B10H11CH2NH2CHMe2]2[Mo8O26][MeCN]2 (6), [C2B10H11CH2NH3]4[Mo8O26][MeCN]2[Et2O]2 (7) and [C2B10H11CH2NH3]2[C2B10H11CH2NH2Et]2[Mo8O26][MeCN]2 (8). Similarly, treatment of an acidified solution of Na2WO4 with [C2B10H11CH2NH3]Cl (3) in water also yielded a white precipitate: crystallization from acetone–hexane afforded the salt [C2B10H11CH2NH=CHMe2]4[W10O32][H2O]2[Me2CO]4 (10), whereas crystallization from acetonitrile–ether gave the double salt [C2B10H11CH2NH3]2[C5H5NH]2[W10O32][MeCN]2-[Et2O] (11). All these ‘globule–globule’ salts 5, 6, 8, 10 and 11 have been characterized by single-crystal X-ray diffraction analyses. Crystal structures reveal the presence of various small solvate molecules, together with an extensive network of hydrogen bonds between ammonium groups and oxygen atoms of the isopolyoxometallates. The isopropyl substituent in one of the carborane cations of the salts 6 and the ethyl substituent in one of the carborane cations of salts 8 may result from occluded isopropanol and ethanol in the starting salt 3 with alkylations of the primary ammonium group being assisted by isopolymolybdate anions. The presence of the pyridinium cation in 11 is believed to arise from contamination during work-up the reaction mixture.

Sign in / Sign up

Export Citation Format

Share Document