scholarly journals Structure cristalline et analyses thermique et de surface Hirshfeld du diperchlorate de 4-azaniumyl-2,2,6,6-tétraméthylpipéridin-1-ium

2017 ◽  
Vol 73 (10) ◽  
pp. 1453-1457 ◽  
Author(s):  
Hammouda Chebbi ◽  
Abdessalem Boumakhla ◽  
Mohamed Faouzi Zid ◽  
Abderrahmen Guesmi
Keyword(s):  
Crystal Packing ◽  
Chair Conformation ◽  
Hirshfeld Surface ◽  
Piperidine Ring ◽  
Dsc Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dimensional Network ◽  
Graph Set ◽  
Mixed Layers

The synthesis of 4-azaniumyl-2,2,6,6-tetramethylpiperidin-1-ium diperchlorate, C9H22N22+·2ClO4−, was carried out from an aqueous reaction of perchloric acid with 4-amino-2,2,6,6-tetramethylpiperidine. This compound was characterized by TGA–DSC analysis and single-crystal X-ray diffraction. The piperidine ring of the dication adopts a chair conformation and the orientation of the C—NH3bond is equatorial. One of the two crystallographically independent perchlorate anions exhibits disorder [occupancies 0.625 (7) and 0.375 (7)]. The crystal packing is constituted by a succession of mixed layers parallel to the (-102) plane, made up of C9H22N22+dications and ClO4−anions. These ions are linked by normal and bifurcated N—H...O hydrogen bonds withR44(12) graph-set motifs, generating a two-dimensional network. The intermolecular interactions in the crystal structure were quantified and analysed using Hirshfeld surface analysis.

scholarly journals Pressure-induced polymorphism in cyclopropylamine

2005 ◽  
Vol 61 (6) ◽  
pp. 717-723 ◽  
Author(s):  
Patricia Lozano-Casal ◽  
David R. Allan ◽  
Simon Parsons
Keyword(s):  
Crystal Structure ◽  
Crystal Packing ◽  
Hirshfeld Surface ◽  
Amino Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
Cell Dimensions ◽  
Graph Set ◽  
Unit Cell Dimensions

The crystal structure of cyclopropylamine at 1.2 GPa has been determined by X-ray diffraction methods. The structure of this phase is orthorhombic, space group Pbca and the unit-cell dimensions are a =  5.0741 (10), b  =  9.7594 (10) and c  =  13.305 (2) Å. Only one of the two H atoms of the amino group actively participates in the formation of the hydrogen-bonded chains, C(2) in graph-set notation, which lie parallel to the crystallographic a axis. Additionally, the topology of the crystal packing is studied using both Voronoi–Dirichlet polyhedra and Hirshfeld surface analyses for the low-temperature and the high-pressure structures of cyclopropylamine and the results are compared.

scholarly journals Structure cristalline, caractérisation spectroscopique, calcul DFT et analyse de surface Hirshfeld du perchlorate de p-toluidinium

2018 ◽  
Vol 74 (2) ◽  
pp. 91-97 ◽  
Author(s):  
Meriam Ben Jomaa ◽  
Hammouda Chebbi ◽  
Noura Fakhar Bourguiba ◽  
Mohamed Faouzi Zid
Keyword(s):  
Theoretical Study ◽  
Dft Method ◽  
Hirshfeld Surface ◽  
X Ray Diffraction ◽  
X Ray ◽  
Vis Spectroscopy ◽  
Two Component ◽  
Graph Set ◽  
Molecular Layers ◽  
Good Agreement

The synthesis of p-toluidinium perchlorate (systematic name: 4-methylanilinium perchlorate), C7H10N+·ClO4 −, was carried out from an aqueous reaction of perchloric acid with p-toluidine. This compound was characterized by powder XRD, IR and UV–Vis spectroscopy. The structure was further confirmed by a single-crystal X-ray diffraction study. The crystal structure is formed by a succession of two-dimensional molecular layers consisting of perchlorate anions and organic cations parallel to the (100) plane and located at x = 2n + ½ (n ∈ Z). Each mixed layer is formed by infinite chains {C7H10N+·ClO4 −} n parallel to the [010] direction and developing along the c axis, generating R 2 4(8), R 2 2(4) and R 4 4(12) graph-set motifs. The results of a theoretical study using the DFT method at the B3LYP/6–311++G(d,p) level are in good agreement with the experimental data. Hirshfeld surface and fingerprint plots reveal that the structure is dominated by O...H/H...O (54.2%), H...H (26.9%) and C—H ...π (14.3%) contacts. The studied crystal was refined as a two-component twin

Phase behaviour and crystal structures of 2′,3′-difluorinated p-terphenyl derivatives

2021 ◽  
Vol 77 (7) ◽  
Author(s):  
Sakuntala Gupta ◽  
Partha Pratim Das ◽  
Przemysław Kula ◽  
Emmanuele Parisi ◽  
Roberto Centore
Keyword(s):  
Crystal Structures ◽  
Crystal Packing ◽  
Phase Behaviour ◽  
Dsc Analysis ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Space Group ◽  
X Ray ◽  
Independent Molecules ◽  
Derivatives Of

The crystal structures of difluorine derivatives of p-terphenyls (nTm) have been determined by single-crystal X-ray diffraction. For the unsymmetrical substituted compounds 2′,3′-difluoro-4-methyl-p-terphenyl (1T0, C19H14F2) and 4-ethyl-2′,3′-difluoro-4′′-methyl-p-terphenyl (1T2, C21H18F2), the crystal structure is disordered, with molecules statistically entering the crystal in up and down orientations, with full superposition of all the atoms, except for those of the terminal groups (H/methyl for 1T0 and methyl/ethyl for 1T2). For triclinic 2′,3′-difluoro-4,4′′-dimethyl-p-terphenyl (1T1, C20H16F2), with the space group P\overline{1}, the two crystallographically independent molecules have the same conformation, which is different from monoclinic 1T0 (space group C2) and 1T2 (space group C2/c). A common feature of the conformation of the three compounds is the noncoplanar twisted arrangement of the three rings of the p-terphenyl moiety. Two-dimensional (2D) Hirshfeld fingerprint plots are consistent with H...H and C...H contacts in the crystal packing. For the three compounds, the phase behaviour has been investigated by POM (Petra/Osiris/Molinspiration) and differential scanning calorimetry (DSC) analysis. 1T2 is mesogenic, with enantiotropic nematic behaviour.

Three new amidophosphoric acid esters with a P(O)[OCH2C(CH3)2CH2O] segment: X-ray diffraction, DFT, AIM and Hirshfeld surface investigations of bi- and tri-furcated (three and four-center) hydrogen bond interactions

2020 ◽  
Vol 235 (3) ◽  
pp. 69-84 ◽  
Author(s):  
Marjan Sadat Bozorgvar ◽  
Atekeh Tarahhomi ◽  
Arie van der Lee
Keyword(s):  
Hydrogen Bond ◽  
Crystal Packing ◽  
Closed Shell ◽  
Hirshfeld Surface ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
X Ray ◽  
Hydrogen Bond Interactions ◽  
Amidophosphoric Acid ◽  
Acid Esters

AbstractStructural and packing features of three new amidophosphoric acid esters having a common part XP(O)[OCH2C(CH3)2CH2O], with X = [(CH3)3CNH] (1), [(CH3)2HCNH] (2) and [C6H11(CH3)N] (3), are investigated by single crystal X-ray diffraction. The results illustrate that the compounds 1 and 3 crystallize with one independent molecule in the asymmetric unit; whereas, for 2, the compound crystallizes with three independent molecules in the asymmetric unit. The crystal structures are mostly stabilized via tri-furcated hydrogen bond interactions (C–H · · ·)2(N–H · · ·)O=P in 1 and (C–H · · ·)3O=P in 3, while the stability is given by bi-furcated hydrogen bond interactions (C–H · · ·)(N–H · · ·)O=P in 2. For a better understanding of the nature, strength and energetics associated with the formation of the quoted multi-center hydrogen bond interactions, the Natural Bond Order (NBO) method from Density Functional Theory (DFT) and a topological analysis by means of Atoms In Molecules (AIM) and Hirshfeld surface procedures were performed. These studies reveal that the studied multi-center hydrogen bond interactions of the type O · · · H are favoured in the crystal packing displaying enrichment ratios larger than unity. The detailed nature of the different interactions in these multi-center interactions is studied for the first time in such compounds. It is shown that the N–H · · · O interaction is rather non-covalent closed-shell whereas the C–H · · · O interaction is more van der Waals closed-shell. Stronger hydrogen bond interactions are observed for a lower multiple H-atom acceptor oxygen in three-center hydrogen bond interactions (C–H · · ·)(N–H · · ·)O=P of 2 than for four-center interactions in 1 [i.e. (C–H · · ·)2(N–H · · ·)O=P] and 3 [i.e. (C–H · · ·)3O=P]. The better H-atom acceptability of the O atom of P=O compared with the esteric O atom is explained by the richer s-character of the hybrid orbital of the O atom acceptor of P=O coupled with enhance of the polarization and charge. The obtained results are also confirmed by Molecular Electrostatic Potential (MEP).

scholarly journals Crystal structure and Hirshfeld surface analysis of dimethyl (3aS,6R,6aS,7S)-2-(2,2,2-trifluoroacetyl)-2,3-dihydro-1H,6H,7H-3a,6:7,9a-diepoxybenzo[de]isoquinoline-3a1,6a-dicarboxylate

2018 ◽  
Vol 74 (11) ◽  
pp. 1599-1604 ◽  
Author(s):  
Zeliha Atioğlu ◽  
Mehmet Akkurt ◽  
Flavien A. A. Toze ◽  
Pavel V. Dorovatovskii ◽  
Narmina A. Guliyeva ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Surface Analysis ◽  
Dominant Role ◽  
Three Dimensional ◽  
Chair Conformation ◽  
Hirshfeld Surface ◽  
Hirshfeld Surface Analysis ◽  
Piperidine Ring ◽  
Dimensional Network

The title molecule, C18H16F3NO7, comprises a fused cyclic system containing four five-membered (two dihydrofuran and two tetrahydrofuran) rings and one six-membered (piperidine) ring. The five-membered dihydrofuran and tetrahydrofuran rings adopt envelope conformations, and the six-membered piperidine ring adopts a distorted chair conformation. Intramolecular O...F interactions help to stabilize the conformational arrangement. In the crystal structure, molecules are linked by weak C—H...O and C—H...F hydrogen bonds, forming a three-dimensional network. The Hirshfeld surface analysis confirms the dominant role of H...H contacts in establishing the packing.

scholarly journals Crystal structure, optical property and Hirshfeld surface analysis of bis[1-(prop-2-en-1-yl)-1H-imidazol-3-ium] hexachloridostannate(IV)

2020 ◽  
Vol 76 (10) ◽  
pp. 1624-1628
Author(s):  
Hela Ferjani
Keyword(s):  
Surface Analysis ◽  
Crystal Packing ◽  
Three Dimensional ◽  
Hirshfeld Surface ◽  
Molecular Surface ◽  
Hirshfeld Surface Analysis ◽  
X Ray Diffraction ◽  
Visible Absorption ◽  
X Ray ◽  
Uv Visible

A new 0D organic–inorganic hybrid material bis[1-(prop-2-en-1-yl)-1H-imidazol-3-ium] hexachloridostannate(IV), (C6H9N2)2[SnCl6], has been prepared and characterized by single-crystal X-ray diffraction, Hirshfeld surface analysis and UV–visible spectroscopy. The structure consists of isolated [SnCl6]2− octahedral anions separated by layers of organic 1-(prop-2-en-1-yl)-1H-imidazol-3-ium cations. The 1-(prop-2-en-1-yl) fragment in the organic cation exhibits disorder over two sets of atomic sites having occupancies of 0.512 (9) and 0.488 (9). The crystal packing of the title compound is established by intermolecular N/C–H...Cl hydrogen bond and π– π stacking interactions. Hirshfeld surface analysis employing three-dimensional molecular surface contours and two-dimensional fingerprint plots has been used to analyse the intermolecular interactions present in the structure. The optical properties of the crystal were studied using UV–visible absorption spectroscopy, showing one intense band at 208 nm, which is attributed to π–π* transitions in the cations.

Structural reinvestigation of the photoluminescent complex [NdCl2(H2O)6]Cl

2013 ◽  
Vol 69 (9) ◽  
pp. 1002-1005 ◽  
Author(s):  
Kuan-Ying Hsieh ◽  
El-Eulmi Bendeif ◽  
Sebastien Pillet ◽  
Abdelatif Doudouh ◽  
Dominik Schaniel ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Local Structure ◽  
Pair Distribution Function ◽  
Structural Model ◽  
Crystal Packing ◽  
Three Dimensional ◽  
Crystalline Material ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dimensional Network

The structure of the photoluminescent compound hexaaquadichloridoneodymium(III) chloride has been redetermined from single-crystal X-ray diffraction data at 100 K, with the aim of providing an accurate structural model for the bulk crystalline material. The crystal structure may be described as a network of [NdCl2(H2O)6]+cations with distorted square-antiprism geometry around the NdIIIcentre. The NdIIIcation and the nonbonded Cl−anion are both located on twofold symmetry axes. The crystal packing consists of three different neodymium pairs linked by a three-dimensional network of O—H...Cl intermolecular interactions. The pair distribution function (PDF) calculated from the experimentally determined structure is used for the discussion of the local structure.

scholarly journals Synthesis, crystal structures, Hirshfeld surface analysis and physico-chemical characterization of two new ZnII and CdII halidometallates

2021 ◽  
Author(s):  
Ali Rayes ◽  
Manel Moncer ◽  
Irene Ara ◽  
Necmi Dege ◽  
Brahim Ayed
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Surface Analysis ◽  
Chemical Characterization ◽  
Chair Conformation ◽  
Hirshfeld Surface ◽  
Hirshfeld Surface Analysis ◽  
Spectroscopic Techniques ◽  
X Ray Diffraction ◽  
X Ray

Abstract Two new organic–inorganic hybrid materials, based on 1,3-CycloHexaneBis-(Methyl Amine), abbreviated CHBMA, namely (H2CHBMA)ZnCl4·2H2O (CP1) and (H2CHBMA)CdI4·2H2O (CP2), have been synthesized under mild conditions in acidic media and characterized by single-crystal X-ray diffraction, spectroscopic techniques (13C NMR, FTIR, RAMAN) and thermal analysis. The crystal structures of the two compounds were solved by single-crystal X-ray diffraction methods. Both compounds show a 3-dimensional supramolecular structure directed by various interactions between tetrahalidometallate anions (ZnCl42−, CdI42−), water molecule and organic cations (H2CHBMA)2+. For both compounds, the cyclohexane ring of the template cation is in a chair conformation with the methylammonium substituent in the equatorial positions and the two terminal ammonium groups in a cis conformation but with two different orientations (upward for CP1 and downward for CP2) which influences the supramolecular architecture of the two structures. Hirshfeld surface analysis and the associated two-dimensional finger print plots were used to explore and quantify the intermolecular interactions in the crystals.

scholarly journals 1,3,4-Tri-O-acetyl-2-N-(trifluoroacetyl)-β-L-fucose

2014 ◽  
Vol 70 (2) ◽  
pp. o134-o135
Author(s):  
David C. McCutcheon ◽  
Peter Norris ◽  
Matthias Zeller
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Room Temperature ◽  
Three Dimensional ◽  
Chair Conformation ◽  
X Ray ◽  
Compound C ◽  
Product Mixture ◽  
Dimensional Network ◽  
Graph Set

The title compound, C14H18F3NO8, was produced through conjugation of 1,3,4-tri-O-acetyl-2-azidodeoxy-α,β-L-fucose with trifluoroacetyl chloride in the presence of bis(diphenylphosphino)ethane in tetrahydrofuran at room temperature. The X-ray crystal structure reveals that the β-anomer of the product mixture crystallizes from ethyl acetate/hexanes. The compound exists in a typical chair conformation with the maximum possible number of substituents, four out of five, located in the sterically preferred equatorial positions. The major directional force facilitating packing of the molecules are N—H...O hydrogen bonds involving the amide moieties of neighboring molecules, which connect molecules stacked along thea-axis direction into infinite strands with aC11(4) graph-set motif. Formation of the strands is assisted by a number of weaker C—H...O interactions involving the methine and methyl H atoms. These strands are connected through further C—H...O and C—H...F interactions into a three dimensional network

scholarly journals Crystal structure of (R)-5-[(R)-3-(4-chlorophenyl)-5-methyl-4,5-dihydroisoxazol-5-yl]-2-methylcyclohex-2-enone

2020 ◽  
Vol 76 (3) ◽  
pp. 400-403
Author(s):  
Ali Oubella ◽  
My Youssef Ait Itto ◽  
Aziz Auhmani ◽  
Abdelkhalek Riahi ◽  
Jean-Claude Daran ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Column Chromatography ◽  
Title Compound ◽  
Crystal Packing ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Compound C ◽  
Dimensional Network

The title compound, C17H18ClNO2, was prepared and isolated as a pure diastereoisomer, using column chromatography followed by a succession of fractional crystallizations. Its exact structure was fully identified via 1H NMR and confirmed by X-ray diffraction. It is built up from a central five-membered dihydroisoxazole ring to which a p-chlorophenyl group and a cyclohex-2-enone ring are attached in the 3 and 5 positions. The cyclohex-2-one and isoxazoline rings each exhibit an envelope conformation. The crystal packing features C—H...O, C—H...N and C—H...π interactions, which generate a three-dimensional network.

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