Evolution structurale de la nacrite en fonction de la nature des molécules organiques intercalees

2000 ◽  
Vol 33 (6) ◽  
pp. 1351-1359 ◽  
Author(s):  
A. Ben Haj Amara ◽  
H. Ben Rhaiem ◽  
A. Plançon
Keyword(s):  
Ir Spectroscopy ◽  
Hydrogen Bonds ◽  
Dimethyl Sulfoxide ◽  
Organic Molecules ◽  
Interlayer Space ◽  
X Ray Diffraction ◽  
X Ray ◽  
Intercalated Compounds ◽  
Xrd Study ◽  
Intercalation Process

Nacrite has been intercalated with two polar organic molecules: dimethyl sulfoxide (DMSO) andN-methylacetamide (NMA). The homogeneous nacrite complexes have been studied by X-ray diffraction (XRD) and infrared (IR) spectroscopy. The XRD study is based on a comparison between experimental and calculated patterns. The structures of the intercalated compounds have been determined, including the mutual positions of the layers after intercalation and the positions of the intercalated molecules in the interlayer space. It has been shown that the intercalation process causes not only a swelling of the interlayer space but also a shift in the mutual in-plane positions of the layers. This shift depends on the nature of the intercalated molecules and is related to their shape and the hydrogen bonds which are established with the surrounding surfaces. For a given molecule, the intercalation process is the same for the different polytypes of the kaolinite family. These XRD results are consistent with those of IR spectroscopy.

scholarly journals First crystal structure of a Pigment Red 52 compound: DMSO solvate hydrate of the monosodium salt

2021 ◽  
Vol 77 (4) ◽  
pp. 402-405
Author(s):  
Lukas Tapmeyer ◽  
Daniel Eisenbeil ◽  
Michael Bolte ◽  
Martin U. Schmidt
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Dimethyl Sulfoxide ◽  
Double Layers ◽  
Ionic Interactions ◽  
Cooh Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Monosodium Salt ◽  
Printing Inks

Pigment Red 52, Na2[C18H11ClN2O6S], is an industrially produced hydrazone-laked pigment. It serves as an intermediate in the synthesis of the corresponding Ca2+ and Mn2+ salts, which are used commercially for printing inks and lacquers. Hitherto, no crystal structure of any salt of Pigment Red 52 is known. Now, single crystals have been obtained of a dimethyl sulfoxide solvate hydrate of the monosodium salt of Pigment Red 52, namely, monosodium 2-[2-(3-carboxy-2-oxo-1,2-dihydronaphthalen-1-ylidene)hydrazin-1-yl]-5-chloro-4-methylbenzenesulfonate dimethyl sulfoxide monosolvate monohydrate, Na+·C18H12ClN2O6S−·H2O·C2H6OS, obtained from in-house synthesized Pigment Red 52. The crystal structure was determined by single-crystal X-ray diffraction at 173 K. In this monosodium salt, the SO3 − group is deprotonated, whereas the COOH group is protonated. The residues form chains via ionic interactions and hydrogen bonds. The chains are arranged in polar/non-polar double layers.

Carbacylamidophosphates: Synthesis, Properties, and Structure of Dimorfolido-N-trichloroacetylphosphorylamide

1998 ◽  
Vol 53 (4) ◽  
pp. 481-484 ◽  
Author(s):  
Vladimir A Ovchynnikov ◽  
Vladimir M Amirkhanov ◽  
Taras P Timoshenko ◽  
Tadeusz Glowiak ◽  
Henryk Kozlowskib
Keyword(s):  
Ir Spectroscopy ◽  
Hydrogen Bonds ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Space Group ◽  
X Ray ◽  
Synthesis Properties ◽  
First Time ◽  
Centrosymmetric Dimers ◽  
Ir Bands

Abstract Dimorpholido-N-trichloroacetylphosphorylamide: CCl3C(O)NHP(O)[N(CH2CH2)2O]2 [HL] and its sodium [NaL] and morpholine [HN(CH2-CH2)2O•HL] salts were synthesized for the first time. The compounds were studied by IR spectroscopy and assignments of the characteristic IR bands have been made. The structure of [HL] was determined by X-ray diffraction. Crystals are monoclinic, a = 11.412(2) Å, b = 16.056(3) Å, c = 9.622(2) Å, β = 108.55(3)°, space group P21/c; Z = 4. The refinement of the structure converged at R = 0.066. The molecules are connected into centrosymmetric dimers via hydrogen bonds formed by the phosphorylic oxygen atoms and hydrogen atoms of amide groups.

scholarly journals Crystal Structure, Spectroscopy, SEM Analysis, and Computational Studies of N-(1,3-Dioxoisoindolin-2yl)benzamide

2015 ◽  
Vol 2015 ◽  
pp. 1-6
Author(s):  
Hakan Bülbül ◽  
Yavuz Köysal ◽  
Necmi Dege ◽  
Sümeyye Gümüş ◽  
Erbil Ağar
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Hydrogen Bonds ◽  
Theoretical Calculations ◽  
Sem Analysis ◽  
Monoclinic Space Group ◽  
Computational Studies ◽  
X Ray Diffraction ◽  
Ethanolic Solution ◽  
X Ray

The compound N-(1,3-dioxoisoindolin-2yl)benzamide, C15H10N2O3, was prepared by the heating of an ethanolic solution of 2-hydroxy-1H-isoindole-1,3(2H)-dione and 4-chloroaniline. The product was characterised using a combination of IR spectroscopy, SEM, and single crystal X-ray diffraction techniques. In addition to the experimental analysis, theoretical calculations were used to investigate the crystal structure in order to compare experimental and theoretical values. The X-ray diffraction analysis shows that the compound crystallises in the monoclinic space group P21/c with the geometric parameters of a=13.5324(11) Å, b=9.8982(8) Å, c=9.7080(8) Å, and β=95.425(6)°. The crystal structure is held together by a network of N-H⋯O hydrogen bonds involving the carboxamide group.

Comparing the strength of covalent bonds, intermolecular hydrogen bonds and other intermolecular interactions for organic molecules: X-ray diffraction data and quantum chemical calculations

2016 ◽  
Vol 40 (8) ◽  
pp. 6848-6853 ◽  
Author(s):  
Angelo Gavezzotti
Keyword(s):  
Hydrogen Bonds ◽  
Diffraction Data ◽  
Chemical Bonding ◽  
Quantum Chemical ◽  
Organic Molecules ◽  
X Ray Diffraction ◽  
Intermolecular Hydrogen Bonds ◽  
Covalent Bonds ◽  
X Ray ◽  
Different Types

The chemical bonding landscape for organic molecules clearly demonstrates the different ranges of stability and predictability for the different types of interactions.

Supramolecular synthesis based on piperidone derivatives and pharmaceutically acceptable co-formers

2013 ◽  
Vol 69 (4) ◽  
pp. 421-427 ◽  
Author(s):  
Bhupinder Sandhu ◽  
Sergiu Draguta ◽  
Tiffany L. Kinnibrugh ◽  
Victor N. Khrustalev ◽  
Tatiana V. Timofeeva
Keyword(s):  
Crystal Structure ◽  
Melting Point ◽  
Ir Spectroscopy ◽  
Hydrogen Bonds ◽  
Crystal Packing ◽  
Aqueous Solubility ◽  
Active Pharmaceutical Ingredient ◽  
Ethanol Solution ◽  
X Ray Diffraction ◽  
X Ray

The target complexes, bis{(E,E)-3,5-bis[4-(diethylamino)benzylidene]-4-oxopiperidinium} butanedioate, 2C27H36N3O+·C4H4O42−, (II), and bis{(E,E)-3,5-bis[4-(diethylamino)benzylidene]-4-oxopiperidinium} decanedioate, 2C27H36N3O+·C10H16O42−, (III), were obtained by solvent-mediated crystallization of the active pharmaceutical ingredient (API) (E,E)-3,5-bis[4-(diethylamino)benzylidene]-4-piperidone and pharmaceutically acceptable dicarboxylic (succinic and sebacic) acids from ethanol solution. They have been characterized by melting point, IR spectroscopy and single-crystal X-ray diffraction. For the sake of comparison, the structure of the starting API, (E,E)-3,5-bis[4-(diethylamino)benzylidene]-4-piperidone methanol monosolvate, C27H35N3O·CH4O, (I), has also been studied. Compounds (II) and (III) represent salts containing H-shaped centrosymmetric hydrogen-bonded synthons, which are built from two parallel piperidinium cations and a bridging dicarboxylate dianion. In both (II) and (III), the dicarboxylate dianion resides on an inversion centre. The two cations and dianion within the H-shaped synthon are linked by two strong intermolecular N+—H...−OOC hydrogen bonds. The crystal structure of (II) includes two crystallographically independent formula units,AandB. The cation geometries of unitsAandBare different. The main N—C6H4—C=C—C(=O)—C=C—C6H4—N backbone of cationAhas a C-shaped conformation, while that of cationBadopts an S-shaped conformation. The same main backbone of the cation in (III) is practically planar. In the crystal structures of both (II) and (III), intermolecular N+—H...O=C hydrogen bonds between different H-shaped synthons further consolidate the crystal packing, forming columns in the [100] and [10\overline 1] directions, respectively. Salts (II) and (III) possess increased aqueous solubility compared with the original API and thus enhance the bioavailability of the API.

XRD Study of the Nacrite/CsCl/H2O Intercalation Complex

2004 ◽  
Vol 443-444 ◽  
pp. 59-64 ◽  
Author(s):  
S. Naamen ◽  
H. Ben Rhaiem ◽  
A. Ben Haj Amara
Keyword(s):  
Direct Method ◽  
Basal Spacing ◽  
X Ray Diffraction ◽  
Intercalation Complex ◽  
Xrd Pattern ◽  
X Ray ◽  
Caesium Chloride ◽  
Intercalated Compounds ◽  
Xrd Study ◽  
A Direct Method

The intercalation complex of nacrite with an alkali halide (Caesium chloride: CsCl) has been successfully prepared by mixing a CsCl saturated solution with a 8.4Å-hydrated nacrite. The homogeneous nacrite/CsCl complex has been studied by X-ray diffraction (XRD). Using an oriented clay aggregate, 10 basal reflections were obtained. The XRD pattern showed basal spacing of 10.5Å with integral series of 00l reflections indicating an ordered stacking of parallel 1:1 layers. A direct method involving a monodimensional electron density projection, along the normal to the layers, is used to determine the number and the position of intercalated compounds. The best agreement between observed and simulated p(Z) (R = 5%) is obtained by placing one Cl- ion at Z=6.7Å; one Cs+ ion at Z=8.3Å and two H O molecules at 6.3 and 7.4Å.

scholarly journals Structural, thermal, and IR studies of β-[Nd2O2](CrO4), an unexpected analog of a slag phase [Ba2F2](S6+O3S2−)

2019 ◽  
Vol 234 (1) ◽  
pp. 1-8
Author(s):  
Dmitri O. Charkin ◽  
Igor V. Plokhikh ◽  
Anastasiya I. Zadoya ◽  
Aleksandr N. Zaloga ◽  
Wulf Depmeier ◽  
...  
Keyword(s):  
Ir Spectroscopy ◽  
Transition Metal ◽  
Slag Phase ◽  
Interlayer Space ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ir Studies ◽  
Space Size ◽  
Structural Architecture ◽  
New Compounds

Abstract A family of Ln2CrO6 (Ln=Pr, Nd, Sm–Tb) compounds has been re-investigated using powder X-ray diffraction and IR spectroscopy. The structure of β-Nd2CrO6≡β-[Nd2O2](CrO4) is similar to that of the slag compound [Ba2F2](S6+O3S2−) in that it exhibits a disordered arrangement of (CrO4)2− anions between [Nd2O2]2+ litharge-type blocks. Its structural architecture is also related to other layered α- and γ-[Ln2O2](AO4) species (A=S, Cr, Mo), showing various orientations of the tetrahedral anions within the interlayer space. Size relationships between the incorporated tetrahedral anions and formation of different structure types (denoted as M1-, M2- and T-type) are reviewed. The possible existence of new compounds which are isostructural with, or structurally related to, β-[Nd2O2](CrO4) and bearing other transition metal-centred tetrahedral anions are discussed.

High Resolution Replication of Organoclay Surfaces

1982 ◽  
Vol 40 ◽  
pp. 576-577
Author(s):  
W. W. Barker ◽  
W. E. Rigsby ◽  
V. J. Hurst ◽  
W. J. Humphreys
Keyword(s):  
Clay Mineral ◽  
Organic Molecule ◽  
Organic Molecules ◽  
X Ray Diffraction ◽  
Xrd Pattern ◽  
X Ray ◽  
Naturally Occurring ◽  
Silicate Layers ◽  
Mineral Identification

Experimental clay mineral-organic molecule complexes long have been known and some of them have been extensively studied by X-ray diffraction methods. The organic molecules are adsorbed onto the surfaces of the clay minerals, or intercalated between the silicate layers. Natural organo-clays also are widely recognized but generally have not been well characterized. Widely used techniques for clay mineral identification involve treatment of the sample with H2 O2 or other oxidant to destroy any associated organics. This generally simplifies and intensifies the XRD pattern of the clay residue, but helps little with the characterization of the original organoclay. Adequate techniques for the direct observation of synthetic and naturally occurring organoclays are yet to be developed.

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