scholarly journals Synthesis and Characterization of a (−)-Epicatechin and Barbituric Acid Cocrystal: Single-Crystal X-ray Diffraction and Vibrational Spectroscopic Studies

ACS Omega ◽  
2021 ◽  
Author(s):  
Iwona Budziak-Wieczorek ◽  
Urszula Maciołek
Keyword(s):  
Single Crystal ◽  
Barbituric Acid ◽  
Spectroscopic Studies ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray

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 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 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 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.

Synthesis and characterization of a hexaphyrin(1.0.1.0.0.0) bearing both meso- and β-substituents

2007 ◽  
Vol 11 (04) ◽  
pp. 287-293 ◽  
Author(s):  
Jonathan L. Sessler ◽  
Patricia J. Melfi ◽  
Vincent M. Lynch
Keyword(s):  
Crystal Structure ◽  
Ring Current ◽  
Spectroscopic Studies ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Planar Conformation ◽  
Hydrogen Bound

The synthesis of an isoamethyrin-type expanded porphyrin bearing both meso- and β-substituents is presented. The diprotonated form of this macrocycle was characterized by conventional spectroscopic means and via a single crystal X-ray diffraction analysis. This species is observed to adopt a planar conformation in the solid state. Nonetheless, the inner ring current, as inferred from 1 H NMR spectroscopic studies, is found to be severely diminished as compared to isoamethyrin, by the presence of the two meso-phenyl moieties. A second crystal structure, in which a molecule of water is hydrogen-bound to a pyrrole NH , was also solved.

Synthesis and Characterization of o-Carboranylthioether Derivatives

2011 ◽  
Vol 66 (9) ◽  
pp. 947-952
Author(s):  
Meiling Xu ◽  
Yong Nie ◽  
Jinling Miao ◽  
Zhenwei Zhang ◽  
Bin Peng ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Solid State ◽  
Single Crystal ◽  
Uv Light ◽  
Chloroform Solution ◽  
Alkyl Halides ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray

The reactions of the dithiolato-o-carborane salt (Et3NH)2(S2C2B10H10) (2) with alkyl halides BrCH2CH=CH2, BrCH2CH2CH2Cl and C6H5CH2Cl, afford the o-carboranyl-bisthioether derivatives 3a - c, which have been characterized by IR and NMR (1H, 13C, 11B) spectroscopy, mass spectrometry, and single-crystal X-ray diffraction (3c). The photoluminescent properties of the known compound 3c has been investigated. It exhibits a violet (chloroform solution) or blue (solid state) emission when excited with UV light.

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