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

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.

2020 ◽  
pp. 1-9
Author(s):  
Dickron R. Nahhas ◽  
John F. Corrigan

This work describes the synthesis of group 11 metal trimethylsilylchalcogenolate complexes [(ITr)M-ESiMe3] stabilized by the large NHC ligand bis-1,3-tritylimidazole-2-ylidene (ITr). The thiolates and selenolates of Cu, Ag, and Au are accessed from either [(ITr)MOAc] (M = Cu, Ag) and E(SiMe3)2 or [(ITr)AuCl] and Li[ESiMe3] (E = S, Se). All complexes were characterized spectroscopically and, for the copper coordination compounds, via single crystal X-ray diffraction analysis.


2002 ◽  
Vol 57 (6) ◽  
pp. 621-624 ◽  
Author(s):  
Wolfgang Fraenk ◽  
Heinrich Nöth ◽  
Thomas M. Klapötke ◽  
Max Suter

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 ◽  
2017 ◽  
Vol 49 (11) ◽  
pp. 2389-2393 ◽  
Author(s):  
Stefanie Pelzer ◽  
Beate Neumann ◽  
Hans-Georg Stammler ◽  
Nikolai Ignat’ev ◽  
Reint Eujen ◽  
...  

This paper describes the synthesis and comprehensive characterization of tetrakis(pentafluoroethyl)germane. In addition to a complete NMR spectroscopic characterization, including the rarely used 73Ge NMR spectroscopy, Ge(C2F5)4 was studied by IR spectroscopy, mass spectrometry as well as X-ray diffraction analysis. A 73Ge NMR investigation as well as an X-ray diffraction study of the related germane Ge(CF3)4 are also included.


2000 ◽  
Vol 55 (9) ◽  
pp. 882-886 ◽  
Author(s):  
Martin Jansen ◽  
Sascha Vensky

The silver(I,II,III) oxide clathrate Ag7O8HCO3 was synthesized by anodic oxidation of silver(I) in a suspension of Ag2CO3 in an aqueous AgF solution. The title compound was characterized by single crystal X-ray diffraction (cubic, Fm3̄m, a = 9.8085(3) Å, Z = 4), scanning electron microscopy, thermal analysis, IR spectroscopy, 1H-solid state-NMR and measurement of the magnetic susceptibility


1999 ◽  
Vol 13 (12n13) ◽  
pp. 451-453
Author(s):  
K. JEYABALAN ◽  
L. K. KALIYAPERUMAL

Synthesis and characterization of La 2 Ca 3 Cu 4 O y compound is reported here. The powder X-ray diffraction analysis shows that the system belongs to an orthorhombic structure and the lattice parameters are a = 3.814(4)Å, b = 3.930(5)Å and c = 34.772(3)Å.


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