scholarly journals Solvatomorphism of Moxidectin

Molecules ◽  
2021 ◽  
Vol 26 (16) ◽  
pp. 4869
Author(s):  
Toni Grell ◽  
Mauro Barbero ◽  
Franco Pattarino ◽  
Giovanni Battista Giovenzana ◽  
Valentina Colombo
Keyword(s):  
Diffraction Analysis ◽  
Crystal Structures ◽  
Variable Temperature ◽  
Thermal Characterization ◽  
Active Pharmaceutical Ingredient ◽  
X Ray Diffraction ◽  
X Ray ◽  
Anthelmintic Drug

The solvatomorphism of the anthelmintic drug moxidectin is investigated, and a new solvatomorph with nitromethane is reported. Moreover, the hitherto unknown crystal structures of the solvatomorphs with ethanol and 2-propanol are reported and discussed. The thermal characterization of these solvatomorphs through variable-temperature powder X-ray diffraction analysis (VT-PXRD) is also described, providing new insights into the crystallochemistry of this active pharmaceutical ingredient.

B(C6F5)3-guided cyclotrimerization-rearrangement of phenylacetylene. Evidence of the (C6F5)3B−–C(H)=C+Ph intermediate in a 1,1-carboboration reaction

2016 ◽  
Vol 71 (10) ◽  
pp. 1029-1041
Author(s):  
Wanli Nie ◽  
Guofeng Sun ◽  
Chong Tian ◽  
Maxim V. Borzov
Keyword(s):  
Nmr Spectroscopy ◽  
Diffraction Analysis ◽  
Crystal Structures ◽  
Variable Temperature ◽  
Spectroscopy Study ◽  
X Ray Diffraction ◽  
X Ray ◽  
Spectral Evidence ◽  
A Minor ◽  
Zwitterionic Intermediate

AbstractIn presence of 2,2,6,6-tetramethylpiperidinium ([TMPH]+) chlorotris(pentafluorophenyl)borate ([TMPH]+[ClB(C6F5)3]−, 3), phenylacetylene undergoes an unusual cyclotrimerization-rearrangement leading to tris(pentafluorophenyl)(3,4,5-triphenylphenyl)borate anion (1) as a minor product which can be isolated and purified in a form of salts [1·(TMPH)n·Cl(n–1)] (n=3 or 5). A variable temperature and concentration NMR spectroscopy study of 3 in CDCl3 unambiguously demonstrated its ability to liberate free B(C6F5)3, which initiates cyclotrimerization and guides rearrangements towards formation of the tetraarylborate anion 1. For the previously studied “spectator” reaction between phenylacetylene and B(C6F5)3 in CDCl3, 1H, 19F, and 11B NMR-spectral evidence of the (C6F5)3B−–C(H)=C+Ph zwitterionic intermediate of the 1,1-carboboration reaction has been demonstrated. The crystal structures of [1·(TMPH)3·Cl2], the salt 3, and a 1:1 adduct of 1,3,5-tris(4-fluorophenyl)benzene and 2,4,6-tris(pentafluorophenyl)-1,3,5,2,4,6-trioxatriborinane (2) have been established by X-ray diffraction analysis.

scholarly journals Reactions of Dihaloboranes with Electron-Rich 1,4-Bis(trimethylsilyl)-1,4-diaza-2,5-cyclohexadienes

Molecules ◽  
2020 ◽  
Vol 25 (12) ◽  
pp. 2875
Author(s):  
Li Ma ◽  
Xiaolin Zhang ◽  
Wenbo Ming ◽  
Shengxin Su ◽  
Xiaoyong Chang ◽  
...  
Keyword(s):  
Double Bond ◽  
Nmr Spectroscopy ◽  
Diffraction Analysis ◽  
1H Nmr Spectroscopy ◽  
Variable Temperature ◽  
Organosilicon Compounds ◽  
X Ray Diffraction ◽  
X Ray ◽  
Multinuclear Nmr Spectroscopy ◽  
Bond Character

The reactions of electron-rich organosilicon compounds 1,4-bis(trimethylsilyl)-1,4-diaza-2,5-cyclohexadiene (1), 2,3,5,6-tetramethyl-1,4-bis(trimethylsilyl)-1,4-diaza-2,5-cyclohexadiene (2), and 1,1′-bis(trimethylsilyl)-1,1′-dihydro-4,4′-bipyridine (12) with B-amino and B-aryl dihaloboranes afforded a series of novel B=N-bond-containing compounds 3–11 and 13. The B=N rotational barriers of 7 (>71.56 kJ/mol), 10 (58.79 kJ/mol), and 13 (58.65 kJ/mol) were determined by variable-temperature 1H-NMR spectroscopy, thus reflecting different degrees of B=N double bond character in the corresponding compounds. In addition, ring external olefin isomers 11 were obtained by a reaction between 2 and DurBBr2. All obtained B=N-containing products were characterized by multinuclear NMR spectroscopy. Compounds 5, 9, 10a, 11, and 13a were also characterized by single-crystal X-ray diffraction analysis.

The Synthesis and Characterization of Oxide Free Tin Nanoparticles

2014 ◽  
Vol 670-671 ◽  
pp. 26-29
Author(s):  
Zhi Long Pan ◽  
Shi Liang Ao ◽  
Jian Ping Jia
Keyword(s):  
Reduction Method ◽  
Chemical Reduction ◽  
Thermal Characterization ◽  
X Ray Diffraction ◽  
Chemical Reduction Method ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Xrd Study ◽  
Tin Nanoparticles

Oxide free Tin nanoparticles were synthesized from a chemical reduction method. Their morphological and thermal characterizations were studied in this paper. The X-ray diffraction (XRD) study showed that no oxides of Tin nanoparticles were formed. The thermal characterization by differential scanning calorimetry (DSC) exhibited the size dependency of the melting points. The melting point was as low as 202.16°C.

New Cu(II), Co(II), and Ni(II) complexes with thieno[2,3-b]pyridine and 2-methylthieno[2,3-b]pyridine as ligands: Synthesis and crystal structures

2009 ◽  
Vol 63 (3) ◽  
Author(s):  
Ján Halgaš ◽  
Viera Kolenová ◽  
Zuzana Števíková ◽  
Lucia Perašínová ◽  
Jozef Kožíšek
Keyword(s):  
Single Crystal ◽  
Diffraction Analysis ◽  
Crystal Structures ◽  
Elemental Analysis ◽  
Zinc Chloride ◽  
Coordination Compounds ◽  
Biological Activities ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ft Ir

AbstractAlthough thienopyridines attract attention because of their biological activities, they have not been used as ligands in coordination compounds. Thieno[2,3-b]pyridine was prepared by known procedures; by reduction of 2-nitrothiophene, and reaction of the resulting 2-thienyl ammonium salt with malondialdehyde tetramethylacetal in the presence of zinc chloride. The same procedure was used for the preparation of a new derivative, 2-methylthieno[2,3-b]pyridine, starting from 2-methyl-5-nitrothiophene. The thienopyridines were used in the synthesis of coordination compounds. Chlorides, isothiocyanates, acetates, and chloroacetates of copper(II), nickel(II), or cobalt(II) were used as starting salts. The prepared complexes were characterized by elemental analysis and FT IR. Structures of the four complexes were determined by single-crystal X-ray diffraction analysis.

Molecular Cocrystals of Carboxylic Acids. XIII. Spectral Characterization of the Adducts of Triphenylphosphine Oxide With Substituted Benzoic Acids and the Crystal Structures of the 1 : 1 Adducts With 2,4,6-Trinitrobenzoic Acid and 3,5-Dinitrobenzoic Acid

1993 ◽  
Vol 46 (10) ◽  
pp. 1535 ◽  
Author(s):  
DE Lynch ◽  
G Smith ◽  
NJ Calos ◽  
CHL Kennard ◽  
AK Whittaker ◽  
...  
Keyword(s):  
Crystal Structures ◽  
Triphenylphosphine Oxide ◽  
Benzoic Acids ◽  
X Ray Diffraction ◽  
X Ray ◽  
Acid Proton ◽  
Phosphoryl Oxygen ◽  
Substituted Benzoic Acids ◽  
Convenient Technique

The 1:1 adducts of triphenylphosphine oxide with the 2-, 3- and 4-nitro-, 3,5-dinitro-, and 2,4,6-trinitro-substituted benzoic acids have been prepared, and characterized by infrared and 31P n.m.r. spectroscopy. The crystal structures of two of these adducts, (triphenylphosphine oxide-3,5-dinitrobenzoic acid) and ( triphenylphosphine oxide-2,4,6-trinitrobenzoic acid), have been determined by X-ray diffraction. In all examples, the presence of single directed hydrogen bonds between the phosphoryl oxygen and the carboxylic acid proton is confirmed. For the X-ray structures, the O…O distances are 2.54(4) and 2.55(1)Ǻ respectively. Solid-state 31P n.m.r. spectroscopy has also proved a convenient technique for the detection of the presence of a single conformational adduct type in cocrystals.

Synthesis and Characterization of Tetrakis(pentafluoroethyl)germane

Synthesis ◽  
2017 ◽  
Vol 49 (11) ◽  
pp. 2389-2393 ◽  
Author(s):  
Stefanie Pelzer ◽  
Beate Neumann ◽  
Hans-Georg Stammler ◽  
Nikolai Ignat’ev ◽  
Reint Eujen ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Ir Spectroscopy ◽  
Diffraction Analysis ◽  
Spectroscopic Characterization ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Comprehensive Characterization

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.

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.

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