Hydrogen bonding and molecular association in 2-(quinuclidinium)-butyric acid bromide hydrate studied by X-ray diffraction, DFT calculations, FTIR and NMR spectroscopy, and potentiometric titration

2010 ◽  
Vol 975 (1-3) ◽  
pp. 357-366 ◽  
Author(s):  
Z. Dega-Szafran ◽  
A. Katrusiak ◽  
M. Szafran ◽  
P. Barczyński
Keyword(s):  
Hydrogen Bonding ◽  
Nmr Spectroscopy ◽  
Dft Calculations ◽  
Potentiometric Titration ◽  
Butyric Acid ◽  
Molecular Association ◽  
X Ray Diffraction ◽  
X Ray

scholarly journals Exploring the Structural Chemistry of Pyrophosphoramides: N,N′,N″,N‴-Tetraisopropylpyrophosphoramide

Chemistry ◽  
2021 ◽  
Vol 3 (1) ◽  
pp. 149-163
Author(s):  
Duncan Micallef ◽  
Liana Vella-Zarb ◽  
Ulrich Baisch
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nuclear Magnetic Resonance ◽  
Hydrogen Bonding ◽  
Nmr Spectroscopy ◽  
Ir Spectroscopy ◽  
Room Temperature ◽  
Intermolecular Hydrogen Bonding ◽  
X Ray Diffraction ◽  
X Ray

N,N′,N″,N‴-Tetraisopropylpyrophosphoramide 1 is a pyrophosphoramide with documented butyrylcholinesterase inhibition, a property shared with the more widely studied octamethylphosphoramide (Schradan). Unlike Schradan, 1 is a solid at room temperature making it one of a few known pyrophosphoramide solids. The crystal structure of 1 was determined by single-crystal X-ray diffraction and compared with that of other previously described solid pyrophosphoramides. The pyrophosphoramide discussed in this study was synthesised by reacting iso-propyl amine with pyrophosphoryl tetrachloride under anhydrous conditions. A unique supramolecular motif was observed when compared with previously published pyrophosphoramide structures having two different intermolecular hydrogen bonding synthons. Furthermore, the potential of a wider variety of supramolecular structures in which similar pyrophosphoramides can crystallise was recognised. Proton (1H) and Phosphorus 31 (31P) Nuclear Magnetic Resonance (NMR) spectroscopy, infrared (IR) spectroscopy, mass spectrometry (MS) were carried out to complete the analysis of the compound.

Structure of 1-methyl-2-oxo-pyrido[2,1b][3,4]dihydropyrimidinium bromide studied by X-ray diffraction, FTIR and NMR spectroscopy and DFT calculations

2007 ◽  
Vol 843 (1-3) ◽  
pp. 107-115 ◽  
Author(s):  
M. Szafran ◽  
I. Kowalczyk ◽  
E. Bartoszak-Adamska ◽  
M. Jaskólski ◽  
B. Nowak-Wydra
Keyword(s):  
Nmr Spectroscopy ◽  
Dft Calculations ◽  
X Ray Diffraction ◽  
X Ray

scholarly journals Internal dynamics in helical molecules studied by X-ray diffraction, NMR spectroscopy and DFT calculations

2017 ◽  
Vol 19 (4) ◽  
pp. 2900-2907 ◽  
Author(s):  
Martin Dračínský ◽  
Jan Storch ◽  
Vladimír Církva ◽  
Ivana Císařová ◽  
Jan Sýkora
Keyword(s):  
Nmr Spectroscopy ◽  
Dft Calculations ◽  
X Ray Diffraction ◽  
Internal Dynamics ◽  
X Ray ◽  
Solid Phases ◽  
Helical Molecules

Unexpected flexibility of helical molecules is observed both in solution and solid phases.

scholarly journals Synthesis, Crystal Structure, and DFT Calculations of 1,3-Diisobutyl Thiourea

2015 ◽  
Vol 2015 ◽  
pp. 1-5 ◽  
Author(s):  
Ataf A. Altaf ◽  
Adnan Shahzad ◽  
Zarif Gul ◽  
Sher A. Khan ◽  
Amin Badshah ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Dft Calculations ◽  
Single Crystal ◽  
Crystal Packing ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Model Support

1,3-Diisobutyl thiourea was synthesized and characterized by single crystal X-ray diffraction. It gives a monoclinic (α=γ= 90 andβ  ≠90) structure with the space group P21/c. The unit cell dimensions area= 11.5131 (4) Å,b= 9.2355 (3) Å,c= 11.3093 (5) Å,α= 90°,β= 99.569° (2),γ= 90°,V= 1185.78 (8) Å3, andZ= 4. The crystal packing is stabilized by intermolecular (N–H⋯S) hydrogen bonding in the molecules. The optimized geometry and Mullikan's charges of the said molecule calculated with the help of DFT using B3LYP-6-311G model support the crystal structure.

Study of Molecular Dynamics and the Solid State Phase Transition Mechanism for Unsymmetrical Thiopyrophosphate Using X-ray Diffraction, DFT Calculations and NMR Spectroscopy

2006 ◽  
Vol 110 (2) ◽  
pp. 761-771 ◽  
Author(s):  
Marek J. Potrzebowski ◽  
Grzegorz D. Bujacz ◽  
Anna Bujacz ◽  
Sebastian Olejniczak ◽  
Paweł Napora ◽  
...  
Keyword(s):  
Phase Transition ◽  
Molecular Dynamics ◽  
Solid State ◽  
Nmr Spectroscopy ◽  
Dft Calculations ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transition Mechanism

Polymorphism ofN,N′′-Diacetylbiuret Studied by Solid-State13C and15N NMR Spectroscopy, DFT Calculations, and X-ray Diffraction

2007 ◽  
Vol 13 (21) ◽  
pp. 6139-6149 ◽  
Author(s):  
Sven Macholl ◽  
Dieter Lentz ◽  
Frank Börner ◽  
Gerd Buntkowsky
Keyword(s):  
Nmr Spectroscopy ◽  
Dft Calculations ◽  
X Ray Diffraction ◽  
X Ray

Conformational behaviour of 3-methyl-4-(4-methylbenzoyl)-1-phenyl-pyrazol-5-one: a sudden story of three desmotropes

RSC Advances ◽  
2015 ◽  
Vol 5 (90) ◽  
pp. 73859-73867 ◽  
Author(s):  
Vanya B. Kurteva ◽  
Boris L. Shivachev ◽  
Rositsa P. Nikolova ◽  
Svetlana D. Simova ◽  
Liudmil M. Antonov ◽  
...  
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Dft Calculations ◽  
Gas Phase ◽  
X Ray Diffraction ◽  
X Ray

The conformational behaviour of 3-methyl-4-(4-methylbenzoyl)-1-phenyl-pyrazol-5-one was studied using a combination of X-ray diffraction, NMR spectroscopy in solution and the solid state, and DFT calculations in the gas phase.

Formation of a [2]rotaxane and [2]catenane based on PdBr2L2 as a template

2009 ◽  
Vol 87 (1) ◽  
pp. 205-211 ◽  
Author(s):  
Barry A Blight ◽  
James A Wisner ◽  
Michael C Jennings
Keyword(s):  
Hydrogen Bond ◽  
Hydrogen Bonding ◽  
Nmr Spectroscopy ◽  
Supramolecular Chemistry ◽  
Self Assembly ◽  
The Self ◽  
X Ray Diffraction ◽  
Template Effect ◽  
X Ray ◽  
The Poor

Previous studies have determined that neutral palladium(II) dibromide complexes template the formation of [2]pseudorotaxanes, albeit with weaker affinities than the analogous palladium(II) dichloride species. Here, the self-assembly of both [2]rotaxane (2) and [2]catenane (5) were attempted using a PdBr2L2 centre as the template, resulting in the desired interlocked structures. The structures were confirmed by NMR spectroscopy, CSI-MS, and single crystal X-ray diffraction analyses. [2]Rotaxane 2 was isolated in 53% and [2]catenane 5 in 41% yields. The lower yields observed in comparison to the chloride analogues can be attributed to the reduced template effect of the palladium(II) dibromide subunits, caused by both the poor steric fit of the bromides in the isophthalamide cleft and bromide’s reduced capacity as a hydrogen bond acceptor.Key words: rotaxane, catenane, hydrogen bonding, interlocked, supramolecular chemistry.

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