scholarly journals Enaminone Substituted Resorcin[4]arene—Sealing of an Upper-Rim with a Directional System of Hydrogen-Bonds

2020 ◽  
Vol 21 (20) ◽  
pp. 7494
Author(s):  
Anna Szafraniec ◽  
Marcin Grajda ◽  
Hanna Jędrzejewska ◽  
Agnieszka Szumna ◽  
Waldemar Iwanek
Keyword(s):  
Crystal Structure ◽  
Experimental Data ◽  
Solid State ◽  
Hydrogen Bonds ◽  
Theoretical Calculations ◽  
The Other ◽  
Thermally Activated ◽  
Intramolecular Hydrogen ◽  
Semi Empirical ◽  
Upper Rim

The paper presents the synthesis of an enaminone resorcin[4]arene via a thermally activated o-quinomethide. The crystal structure indicates that in the solid state all enaminone units participate in a unidirectional seam of 12 intramolecular hydrogen bonds that are formed around the cavity. The molecule exhibits C2 symmetry, with two opposite-laying enaminone units directed inside the cavity (“in”), and the other two units outside the cavity (“out”). In the solution the enaminone resorcin[4]arene exists as a mixture of conformers with distribution controlled by temperature and solvent. The experimental data are compared with the results of theoretical calculations using DFT B3LYP/6-31G(d,p) and fast semi-empirical DFTB/GFN2-xTB method in various solvents.

scholarly journals Crystal structure of the co-crystalline adduct 1,3,6,8-tetraazatricyclo[4.4.1.13,8]dodecane (TATD)–4-bromophenol (1/2)

2015 ◽  
Vol 71 (5) ◽  
pp. 463-465 ◽  
Author(s):  
Augusto Rivera ◽  
Juan Manuel Uribe ◽  
Jicli José Rojas ◽  
Jaime Ríos-Motta ◽  
Michael Bolte
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Hydrogen Bonds ◽  
Rotation Axis ◽  
The Other ◽  
Two Dimensional ◽  
Asymmetric Unit ◽  
Species Association ◽  
Crystalline Adduct ◽  
Aminal Cage

The structure of the 1:2 co-crystalline adduct C8H16N4·2C6H5BrO, (I), from the solid-state reaction of 1,3,6,8-tetraazatricyclo[4.4.1.13,8]dodecane (TATD) and 4-bromophenol, has been determined. The asymmetric unit of the title co-crystalline adduct comprises a half molecule of aminal cage polyamine plus a 4-bromophenol molecule. A twofold rotation axis generates the other half of the adduct. The primary inter-species association in the title compound is through two intermolecular O—H...N hydrogen bonds. In the crystal, the adducts are linked by weak non-conventional C—H...O and C—H...Br hydrogen bonds, giving a two-dimensional supramolecular structure parallel to thebcplane.

Synthon preference in the cocrystal of 3,4,5-trifluorophenylboronic acid with urea

2017 ◽  
Vol 73 (11) ◽  
pp. 889-895 ◽  
Author(s):  
Karolina Kopczyńska ◽  
Paulina H. Marek ◽  
Bartłomiej Banaś ◽  
Izabela D. Madura
Keyword(s):  
Crystal Structure ◽  
Experimental Data ◽  
Hydrogen Bonds ◽  
Crystal Engineering ◽  
Boronic Acid ◽  
Theoretical Calculations ◽  
Boronic Acids ◽  
Vector Model ◽  
Comprehensive Description ◽  
Model Calculations

The comprehensive description of the crystal structure of a novel 1:1 cocrystal of 3,4,5-trifluorophenylboronic acid with urea, C6H4BF3O2·CH4N2O, is presented. Both components are good candidates for crystal engineering as they can create a variety of supramolecular synthons. The preference for the formation of different hetrosynthons is verified based on theoretical calculations. The syn–anti conformation of boronic acid has been found to be the most favourable in the formation of intermolecular interactions with urea. Moreover, the distortions present in the boron coordination sphere have been described quantitatively based on experimental data according to bond-valence vector model calculations. The results revealed that the deformation of the sphere is typical for a syn–anti conformation of boronic acids. The supramolecular structure of the cocrystal is composed of large synthons in the form of layers made up of O—H...O and N—H...O hydrogen bonds. The layers are joined via N—H...F hydrogen bonds which are unusual for urea cocrystal structures.

scholarly journals Crystal structure of di-μ-chlorido-bis[dichlorido(L-histidinium-κO)cadmium(II)]

2019 ◽  
Vol 75 (6) ◽  
pp. 823-825
Author(s):  
Nacira Mohamedi ◽  
Slim Elleuch ◽  
Sihem Boufas ◽  
Messaoud Legouira ◽  
Faiçal Djazi
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Spectroscopic Data ◽  
Theoretical Calculations ◽  
Three Dimensional ◽  
Chloride Ions ◽  
The Other ◽  
Coordination Polyhedra ◽  
Dimensional Network ◽  
Axial Site

In the title compound, [Cd2(C6H9N3O2)2Cl6], the coordination polyhedra around the CdII cations are distorted trigonal bipyramids. Two of the chloride ions (one axial and one equatorial) are bridging to the other metal atom, leading to a Cd...Cd separation of 3.9162 (4) Å. The O atom of the L-histidinium cation lies in an axial site. In the crystal, numerous N—H...Cl, N—H...O, C—H...O and C—H...Cl hydrogen bonds link the molecules into a three-dimensional network. Theoretical calculations and spectroscopic data are available as supporting information.

scholarly journals Organotin(IV) selenate derivatives – Crystal structure of [{(Ph3Sn)2SeO4} ⋅ CH3OH] n

2021 ◽  
Vol 44 (1) ◽  
pp. 213-217
Author(s):  
Waly Diallo ◽  
Hélène Cattey ◽  
Laurent Plasseraud
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Hydrogen Bonds ◽  
Point Of View ◽  
Intermolecular Hydrogen Bonds

Abstract Crystallization of [(Ph3Sn)2SeO4] ⋅ 1.5H2O in methanol leads to the formation of [{(Ph3Sn)2SeO4} ⋅ CH3OH] n (1) which constitutes a new specimen of organotin(IV) selenate derivatives. In the solid state, complex 1 is arranged in polymeric zig-zag chains, composed of alternating Ph3Sn and SeO4 groups. In addition, pendant Ph3Sn ⋅ CH3OH moieties are branched along chains according to a syndiotactic organization and via Sn-O-Se connections. From a supramolecular point of view, intermolecular hydrogen bonds established between the selenate groups (uncoordinated oxygen) and the hydroxyl functions (CH3OH) of the pendant groups link the chains together.

scholarly journals Crystal structure of atazanavir, C38H52N6O7

2020 ◽  
Vol 35 (2) ◽  
pp. 129-135
Author(s):  
James A. Kaduk ◽  
Amy M. Gindhart ◽  
Thomas N. Blanton
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Powder Diffraction ◽  
Density Functional ◽  
Carbonyl Oxygen ◽  
Hydroxyl Group ◽  
Amide Nitrogen ◽  
Classical Hydrogen Bond ◽  
Intramolecular Hydrogen ◽  
Atazanavir Sulfate

The crystal structure of atazanavir has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Atazanavir crystallizes in space group P21 (#4) with a = 15.33545(7), b = 5.90396(3), c = 21.56949(13) Å, β = 96.2923(4)°, V = 1941.134(11) Å3, and Z = 2. Despite being labeled as “atazanavir sulfate”, the commercial reagent sample consisted of atazanavir free base. The structure consists of an array of extended-conformation molecules parallel to the ac-plane. Although the atazanavir molecule contains only four classical hydrogen bond donors, hydrogen bonding is, surprisingly, important to the crystal energy. Both intra- and intermolecular hydrogen bonds are significant. The hydroxyl group forms bifurcated intramolecular hydrogen bonds to a carbonyl oxygen atom and an amide nitrogen. Several amide nitrogens act as donors to the hydroxyl group and carbonyl oxygen atoms. An amide nitrogen acts as a donor to another amide nitrogen. Several methyl, methylene, methyne, and phenyl hydrogens participate in hydrogen bonds to carbonyl oxygens, an amide nitrogen, and the pyridine nitrogen. The powder pattern is included in the Powder Diffraction File™ as entry 00-065-1426.

3,3′-N,N′-Bis(amino)-2,2′-bipyridine — An unusually methylation-resistant amine

2011 ◽  
Vol 89 (8) ◽  
pp. 971-977
Author(s):  
Danielle M. Chisholm ◽  
Robert McDonald ◽  
J. Scott McIndoe
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Complex Mixtures ◽  
Amino Groups ◽  
Intramolecular Hydrogen Bonds ◽  
X Ray ◽  
Intramolecular Hydrogen

Methylation of aromatic amino groups is usually straightforward, but the formation of two intramolecular hydrogen bonds in 3,3′-N,N′-bis(amino)-2,2′-bipyridine and (or) the potential for ring methylation prevents the clean tetramethylation of this molecule. Numerous attempts to make 3,3′-N,N′-bis(dimethylamino)-2,2′-bipyridine produced only complex mixtures of variously methylated products, and the only isolated molecule was 3,3′-N,N′-bis(methylamino)-2,2′-bipyridine, for which an X-ray crystal structure was obtained.

scholarly journals β-Li0.37Na0.63Fe(MoO4)2

2014 ◽  
Vol 70 (2) ◽  
pp. i9-i10 ◽  
Author(s):  
Amira Souilem ◽  
Mohamed Faouzi Zid ◽  
Ahmed Driss
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Solid State Reaction ◽  
Title Compound ◽  
General Position ◽  
Site Occupancy ◽  
The Other ◽  
Main Structure ◽  
Axis Direction ◽  
A Site

The title compound, lithium/sodium iron(III) bis[orthomolybdate(VI)], was obtained by a solid-state reaction. The main structure units are an FeO6octahedron, a distorted MoO6octahedron and an MoO4tetrahedron sharing corners. The crystal structure is composed of infinite double MoFeO11chains along theb-axis direction linked by corner-sharing to MoO4tetrahedra so as to form Fe2Mo3O19ribbons. The cohesion between ribbonsviamixed Mo—O—Fe bridges leads to layers arranged parallel to thebcplane. Adjacent layers are linked by corners shared between MoO4tetrahedra of one layer and FeO6octahedra of the other layer. The Na+and Li+ions partially occupy the same general position, with a site-occupancy ratio of 0.631 (9):0.369 (1). A comparison is made withAFe(MoO4)2(A= Li, Na, K and Cs) structures.

Crystal structure of osimertinib mesylate Form B (Tagrisso), (C28H34N7O2)(CH3O3S)

2021 ◽  
pp. 1-9
Author(s):  
James A. Kaduk ◽  
Nicholas C. Boaz ◽  
Emma L. Markun ◽  
Amy M. Gindhart ◽  
Thomas N. Blanton
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Hydrogen Bonds ◽  
Powder Diffraction ◽  
Density Functional ◽  
Amino Nitrogen ◽  
Strong Hydrogen Bond ◽  
Powder Diffraction File ◽  
Dimethylamino Group ◽  
Intramolecular Hydrogen

The crystal structure of osimertinib mesylate Form B has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Osimertinib mesylate Form B crystallizes in space group P-1 (#2) with a = 11.42912(17), b = 11.72274(24), c = 13.32213(22) Å, α = 69.0265(5), β = 74.5914(4), γ = 66.4007(4)°, V = 1511.557(12) Å3, and Z = 2. The crystal structure is characterized by alternating layers of cation–anion and parallel stacking interactions parallel to the ab-planes. The cation is protonated at the nitrogen atom of the dimethylamino group, which forms a strong hydrogen bond between the cation and the anion. That hydrogen atom also participates in a weaker intramolecular hydrogen bond to an amino nitrogen. There are two additional N–H⋅⋅⋅O hydrogen bonds between the cation and the anion. Several C–H⋅⋅⋅O hydrogen bonds also link the cations and anions. The powder pattern has been submitted to ICDD® for inclusion in the Powder Diffraction File™.

scholarly journals Very Short Intramolecular Hydrogen Bonds in the Crystal Structure of 1-[Bis(4-Fluorophenyl)Methyl]Piperazinediium Dimaleate

2012 ◽  
Vol 42 (10) ◽  
pp. 1046-1051 ◽  
Author(s):  
A. S. Dayananda ◽  
Grzegorz Dutkiewicz ◽  
H. S. Yathirajan ◽  
B. Narayana ◽  
Maciej Kubicki
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Intramolecular Hydrogen Bonds ◽  
Intramolecular Hydrogen
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