scholarly journals Molecular co-crystals of 2-aminothiazole derivatives

1999 ◽  
Vol 55 (5) ◽  
pp. 758-766 ◽  
Author(s):  
Daniel E. Lynch ◽  
Laura J. Nicholls ◽  
Graham Smith ◽  
Karl A. Byriel ◽  
Colin H. L. Kennard
Keyword(s):  
Hydrogen Bonding ◽  
Carboxylic Acid ◽  
Ir Spectroscopy ◽  
Proton Transfer ◽  
Powder Diffraction ◽  
X Ray Diffraction ◽  
X Ray ◽  
Carboxylate Oxygen ◽  
Carboxylate Groups ◽  
Graph Set

A series of molecular adducts of 2-aminothiazole derivatives – 2-aminothiazole, 2-amino-2-thiazoline and 2-aminobenzothiazole with the carboxylic-acid-substituted heterocyclics indole-2-carboxylic acid, N-methylpyrrole-2-carboxylic acid and thiophene-2-carboxylic acid – have been prepared and characterized using X-ray powder diffraction and in five cases by single-crystal X-ray diffraction methods. These five compounds are the adducts of 2-amino-2-thiazolium with indole-2-carboxylate [(C3H7N2S)+(C9H6NO2)−], and N-methylpyrrole-2-carboxylate [(C3H7N2S)+-(C6H6NO2)−], 2-aminobenzothiazolium with indole-2-carboxylate [(C7H7N2S)+(C9H6NO2)−], N-methylpyrrole-2-carboxylate [(C7H7N2S)+(C6H6NO2)−] and thiophene-2-carboxylate [(C7H7N2S)+(C5H3O2S)−]. All complexes involve proton transfer, as indicated by IR spectroscopy, while the five crystal structures display similar hydrogen-bonding patterns with the dominant interaction being an R^2_2(8) graph set dimer association between carboxylate groups and the amine/heterocyclic nitrogen sites. Futhermore, in each case a subsiduary interaction between an amino proton and a carboxylate oxygen completes a linear hydrogen-bonded chain. In addition to this, the indole-2-carboxylate molecules in the adduct structure with 2-amino-2-thiazolium form associated dimers which add to the hydrogen-bonding network.

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.

A New Supramolecular Synthon Using N-Methylaniline. The Crystal Structure of the 1 : 1 Adduct of N-Methylaniline with 5-Nitrofuran-2-carboxylic Acid

1998 ◽  
Vol 51 (9) ◽  
pp. 867 ◽  
Author(s):  
Daniel E. Lynch ◽  
Lisa C. Thomas ◽  
Graham Smith ◽  
Karl A. Byriel ◽  
Colin H. L. Kennard
Keyword(s):  
Crystal Structure ◽  
Carboxylic Acid ◽  
Proton Transfer ◽  
Single Crystal ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Supramolecular Synthon ◽  
X Ray ◽  
C 23 ◽  
A Cell

The crystal structure of the 1 : 1 adduct of N-methylaniline with 5-nitrofuran-2-carboxylic acid has been determined by single-crystal X-ray diffraction. Crystals are monoclinic, space group P21/c with Z 4 in a cell of dimensions a 8·467(5), b 6·106(2), c 23·95(1) Å, β 94·48(3)°. The molecules associate in a tetrameric, proton-transfer formation which has potential as a new supramolecular synthon.

The Crystal and Molecular Structure of the 1:1 Adduct Hydrate of Pyrazine-2,3-dicarboxylic Acid with 1,1-Diethylurea

2000 ◽  
Vol 53 (12) ◽  
pp. 999 ◽  
Author(s):  
Graham Smith ◽  
Colin H. L. Kennard
Keyword(s):  
Hydrogen Bonding ◽  
Carboxylic Acid ◽  
Dicarboxylic Acid ◽  
Lattice Water Molecule ◽  
Crystal And Molecular Structure ◽  
Acid Group ◽  
X Ray Diffraction ◽  
Carboxylic Acid Group ◽  
X Ray ◽  
Bonding Interaction

The adduct hydrate of 1,1-diethylurea with pyrazine-2,3-dicarboxylic acid, [(C6H4N2O4)(C5H12N2O)].H2O has been prepared and characterized using low-temperature single-crystal X-ray diffraction methods. A primary asymmetric cyclic hydrogen-bonding interaction, similar to those found in other adducts of 1,1-diethylurea with the nitro-substituted aromatic acids, was found between the amide group of the substituted urea and one carboxylic acid group of the acid. Further peripheral hydrogen-bonding associations involving both the f irst and the second carboxylic acid groups, urea and the lattice water molecule result in a ribbon polymer structure.

Inhibitors of the geotropic response in plants. The crystal structures of 2-[(Naphthalen-2-yl)carbamoyl]benzoic acid (β-Naptalam), 2-(Phenylcarbamoyl)-benzoic acid and 2-(5-Phenyl-1,3,4-oxadiazol-2-yl)benzoic acid

1983 ◽  
Vol 36 (12) ◽  
pp. 2455 ◽  
Author(s):  
G Smith ◽  
CHL Kennard ◽  
GF Katekar
Keyword(s):  
Hydrogen Bonding ◽  
Carboxylic Acid ◽  
Benzoic Acid ◽  
Crystal Structures ◽  
Carboxylic Acids ◽  
Intermolecular Hydrogen Bonding ◽  
X Ray Diffraction ◽  
X Ray ◽  
Carboxylic Acid Groups ◽  
Phthalamic Acid

The crystal structures of three geotropically active phthalamic acid derivatives have been determined by means of X-ray diffraction and the structural systematics for the series compared. The three acids are conformationally similar and, in contrast to the tendency among carboxylic acids to form hydrogen-bonded dimers, they exist as monomers with intermolecular hydrogen bonding between the carboxylic acid groups and the nitrogen or oxygen of the amide side chains.

Some aspects of the crystal-chemistry of apatites

1993 ◽  
Vol 57 (389) ◽  
pp. 709-719 ◽  
Author(s):  
Yu Liu ◽  
Paola Comodi
Keyword(s):  
Ir Spectroscopy ◽  
Powder Diffraction ◽  
Sedimentary Rock ◽  
Early Stage ◽  
Alkaline Rock ◽  
Ir Absorption ◽  
X Ray Diffraction ◽  
X Ray ◽  
Si Content ◽  
Absorption Features

AbstractTwenty-four apatite (Ap) samples mainly from carbonatite and alkaline rocks were studied by electron microprobe, IR spectroscopy and X-ray powder diffraction. The crystal structures of six were refined using single crystal X-ray diffraction data to R = 1.7-2.5%. The generally high Si content of Ap from carbonatite and alkaline rock has been related to the presence of characteristic Si-O absorptions in IR spectra. Bands, whose intensities change with Si content, were observed at 520, 650, 930 and 1160 cm-1. The IR absorption features of v3 CO3 mode of Ap from carbonatite are different from those of v3 CO3 mode of Ap from sedimentary rock. This phenomenon is probably due to the different effects of F and OH on the CO3 substitution for PO4. The structural refinements yield more information on the CO3=PO4 substitution, which is now supported also by the geometrical evolution of the tetrahedron with increasing CO3 content: the tetrahedral size decreases and the angle distortion increases with C-content. It is likely that the triangular planar CO3 group is disordered on the four faces of PO43-tetrahedron. It was observed also that Ap from early-stage carbonatite is OH-dominant with considerable LREE, Si, CO3 and negligible Mn, Fe, Mg, K, S and C1 contents. They have high Sr/Mn, Si/S and C/S ratios.

scholarly journals Supramolecular frameworks based on [60]fullerene hexakisadducts

2017 ◽  
Vol 13 ◽  
pp. 1-9 ◽  
Author(s):  
Andreas Kraft ◽  
Johannes Stangl ◽  
Ana-Maria Krause ◽  
Klaus Müller-Buschbaum ◽  
Florian Beuerle
Keyword(s):  
Hydrogen Bonding ◽  
Solid State ◽  
Carboxylic Acid ◽  
Structural Integrity ◽  
Structure Stability ◽  
Side Chains ◽  
X Ray Diffraction ◽  
X Ray

[60]Fullerene hexakisadducts possessing 12 carboxylic acid side chains form crystalline hydrogen-bonding frameworks in the solid state. Depending on the length of the linker between the reactive sites and the malonate units, the distance of the [60]fullerene nodes and thereby the spacing of the frameworks can be controlled and for the most elongated derivative, continuous channels are obtained within the structure. Stability, structural integrity and porosity of the material were investigated by powder X-ray diffraction, thermogravimetry and sorption measurements.

scholarly journals Hydrogen bonding-based 3D supramolecular architecture of [Cu(CHA)2][TCM]·11H2O

2014 ◽  
Vol 12 (1) ◽  
pp. 14-24
Author(s):  
Mihaela Vlassa ◽  
Gheorghe Borodi ◽  
Cristian Silvestru ◽  
Mircea Vlassa
Keyword(s):  
Hydrogen Bonding ◽  
Supramolecular Network ◽  
Water Mixture ◽  
Coordination Geometry ◽  
Supramolecular Architecture ◽  
X Ray Diffraction ◽  
Apical Position ◽  
X Ray ◽  
Anionic Ligand ◽  
Carboxylate Groups

AbstractReaction of Na4TCM (1) (H4TCM = tetra[4-(carboxyphenyl)oxamethyl]methane) with [Cu(CHA)](ClO4)2 (2)(CHA = 1,3,6,8,11,14-hexaaz atricyclo[12.2.1.1.8,11] octadecane) in a DMF-water mixture yields [Cu(CHA)]2[TCM] (3). Structural analysis of [Cu(CHA)]2[TCM]·11H2O (3·11H2O) by single crystal X-ray diffraction reveals strong copper-oxygen bonds between two complex cations and the tetraanion leading to a 3D coordination network (zwitterionic structure), consolidated through additional NH...O=C hydrogen bonding within the cation/anion association. The resulting coordination geometry around a copper atom is a distorted square pyramidal with an oxygen atom of the anionic ligand in the apical position. A 3D supramolecular network is developed in the crystal based only on NH...OC hydrogen bonds between the macrocyclic metallic tecton and the carboxylate groups of neighboring 3D coordinated (zwitterionic) moieties. The pseudotetrahedral TCM4− tetraanionic ligand induces a diamondoid architecture formed of large distorted adamantanoid cages.

Molecular Cocrystals of Carboxylic Acids. XXXI Adducts of 2-Aminopyrimidine and 3-Amino-1,2,4-triazole with Heterocyclic Carboxylic Acids

1998 ◽  
Vol 51 (5) ◽  
pp. 403 ◽  
Author(s):  
Daniel E. Lynch ◽  
Tariq Latif ◽  
Graham Smith ◽  
Karl A. Byriel ◽  
Colin H. L. Kennard ◽  
...  
Keyword(s):  
Acetic Acid ◽  
Carboxylic Acid ◽  
Single Crystal ◽  
Carboxylic Acids ◽  
Powder Diffraction ◽  
X Ray Diffraction ◽  
X Ray ◽  
Indole 3 Acetic Acid ◽  
Molecular Adducts

A series of molecular adducts of 2-aminopyrimidine and 3-amino-1,2,4-triazole with heterocyclic carboxylic acids have been prepared and characterized by using X-ray powder diffraction and in four cases by single-crystal X-ray diffraction methods. These four compounds are the (1 : 1) adducts of 2-aminopyrimidine with indole-3-acetic acid [(C4H5N3)(C10H9NO2)], N-methylpyrrole-2-carboxylic acid [(C4H5N3)(C6H7NO2)] and thiophen-2-carboxylic acid [(C4H5N3)(C5H4O2S)], and the (1 : 1) adduct of 3-amino-1,2,4-triazole with thiophen-2-carboxylic acid [(C2H4N4)(C5H4O2S)]. Other compounds described are the (1 : 1) adducts of 3-amino-1,2,4-triazole with indole-3-acetic acid and N-methylpyrrole-2-carboxylic acid.

Crystal structure of dicadmium(II) ethylenediphosphinetetraacetate octahydrate

1991 ◽  
Vol 56 (7) ◽  
pp. 1454-1460 ◽  
Author(s):  
Jaroslav Podlaha ◽  
Jana Podlahová
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Single Crystal ◽  
Diffraction Data ◽  
Title Compound ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
Coordination Polyhedra ◽  
X Ray ◽  
Carboxylate Groups

The crystal structure of the title compound containing a phosphorus analogue of EDTA as the ligand was determined from single-crystal X-ray diffraction data and refined to R = 0.028 for 1 920 observed reflections. The crystals are monocyclic, space group P21/c,a = 8.6169(8), b = 16.0539(9), c = 8.2504(6)Å, β = 103.458(7)° and Z = 2. The structure is completely different from that of the nitrogen prototype, [CdEDTA]2-. It consists of double-stranded polymeric layers which are composed of metal coordination polyhedra linked by μ6-hexadentate ligands; the layers lie parallel to the bc plane and are joined along the a axis through hydrogen bonding donated by water molecules. Because of steric requirements of phosphorus, the coordination polyhedron around Cd is greatly distorted and can best be described as a 5 + 3 type. One P atom, two oxygen atoms from two monodentate carboxylate groups and two water molecules form an approximate trigonal bipyramid and further three more remote carboxylate oxygens complete the arrangement, resulting in an O7P distorted bicapped trigonal prism.

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