Synthesis, structure and characterization of five new organically templated metal sulfates with 2-aminopyridinium

2016 ◽  
Vol 72 (5) ◽  
pp. 432-441 ◽  
Author(s):  
Tamara J. Bednarchuk ◽  
Vasyl Kinzhybalo ◽  
Adam Pietraszko
Keyword(s):  
Materials Science ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
Hydrogen Bond Formation ◽  
Unit Cells ◽  
Science Community ◽  
Type 3

The chemistry of organically templated metal sulfates has attracted interest from the materials science community and the development of synthetic strategies for the preparation of organic–inorganic hybrid materials with novel structures and special properties is of current interest. Sulfur–oxygen–metal linkages provide the possibility of using sulfate tetrahedra as building units to form new solid-state materials. A series of novel organically templated metal sulfates of 2-aminopyridinium (2ap) with aluminium(III), cobalt(II), magnesium(II), nickel(II) and zinc(II) were obtained from the respective aqueous solutions and studied by single-crystal X-ray diffraction. The compounds crystallize in centrosymmetric triclinic unit cells in three structure types: type 1 for 2-aminopyridinium hexaaquaaluminium(III) bis(sulfate) tetrahydrate, (C5H7N2)[Al(H2O)6](SO4)2·4H2O, (I); type 2 for bis(2-aminopyridinium) tris[hexaaquacobalt(II)] tetrakis(sulfate) dihydrate, (C5H7N2)2[Co(H2O)6]3(SO4)4·2H2O, (II), and bis(2-aminopyridinium) tris[hexaaquamagnesium(II)] tetrakis(sulfate) dihydrate, (C5H7N2)2[Mg(H2O)6]3(SO4)4·2H2O, (III); and type 3 for bis(2-aminopyridinium) hexaaquanickel(II) bis(sulfate), (C5H7N2)2[Ni(H2O)6](SO4)2, (IV), and bis(2-aminopyridinium) hexaaquazinc(II) bis(sulfate), (C5H7N2)2[Zn(H2O)6](SO4)2, (V). The templating role of the 2ap cation in all of the reported crystalline substances is governed by the formation of characteristic charge-assisted hydrogen-bonded pairs with sulfate anions and the presence of π–π interactions between the cations. Additionally, both coordinated and uncoordinated water molecules are involved in hydrogen-bond formation. As a consequence, extensive three-dimensional hydrogen-bonding patterns are formed in the reported crystal structures.

Characterization of New Inorganic- Organic Hybrid Compounds: (C6H10N2).Cl2 (I), [C6H10N2]2ZnCl4 (II): Crystal Structure, Hirschfield Surface, IR and NMR spectroscopy Analysis.

2021 ◽  
Author(s):  
nejeh hannachi ◽  
faouzi hlel
Keyword(s):  
Nmr Spectroscopy ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
Spectroscopy Analysis ◽  
Absorption Bands ◽  
Monoclinic System ◽  
Xrd Pattern ◽  
Organic Hybrid ◽  
C Nmr

Abstract Two new organic-inorganic hybrid materials, (C6H10N2).Cl2 (I) and [C6H10N2]2ZnCl4 (II), have been synthesized by hydrothermal method and characterized by single-crystal X-ray diffraction and XRD pattern investigations. These two compounds are crystallized in the monoclinic system; C2/c space group. In the both structures, the anionic-cationic entities are interconnected by hydrogen bonding contacts and p-p Interaction forming three-dimensional networks. Intermolecular interactions were investigated by Hirshfeld surfaces and the contacts of the four different chloride atoms in (II) were compared. The vibrational absorption bands were identified by infrared spectroscopy. These compounds were also investigated by solid state 13C NMR spectroscopy.

scholarly journals Structural characterization of quaternary selenites of tungsten(VI), A 2W3SeO12 (A = NH4, Cs, Rb, K or Tl)

2021 ◽  
Vol 77 (4) ◽  
pp. 406-411
Author(s):  
Vineela Balisetty ◽  
Kanamaluru Vidyasagar
Keyword(s):  
Three Dimensional ◽  
Spectroscopic Studies ◽  
Solid State Reactions ◽  
Dimensional Structure ◽  
X Ray Diffraction ◽  
Compound K ◽  
Three Dimensional Structure ◽  
Thermal And Spectroscopic Studies ◽  
Anionic Framework

The quaternary A 2W3SeO12 (A = NH4, Cs, Rb, K or Tl) selenites have been prepared in the form of single crystals by hydrothermal and novel solid-state reactions. They were characterized by X-ray diffraction, thermal and spectroscopic studies. All of them have a hexagonal tungsten oxide (HTO) related [W3SeO12]2− anionic framework with pyramidally coordinated Se4+ ions. The known A 2W3SeO12 (A = NH4, Cs or Rb) compounds are isostructural with the Cs2W3TeO12 compound and have a non-centrosymmetric layered structure containing intra-layer Se—O bonds. The new compound K2W3SeO12(α) is isostructural with the K2W3TeO12 compound and has a centrosymmetric three-dimensional structure containing interlayer Se—O bonds. It is inferred that the new Tl2W3SeO12 compound has the same three-dimensional structure as K2W3SeO12(α).

scholarly journals Appearance of efficient luminescence energy transfer in doped orthovanadate nanocrystals

2017 ◽  
Vol 50 (3) ◽  
pp. 787-794 ◽  
Author(s):  
Swati Bishnoi ◽  
G. Swati ◽  
Paramjeet Singh ◽  
V. V. Jaiswal ◽  
Mukesh K. Sahu ◽  
...  
Keyword(s):  
Energy Transfer ◽  
Band Gap ◽  
Photoluminescence Intensity ◽  
X Ray Diffraction ◽  
Synthesis Mechanism ◽  
Enhanced Photoluminescence ◽  
Nir Absorption ◽  
Decay Parameters

This paper reports the detailed synthesis mechanism and the structural, morphological and optical characterization of ultraviolet (∼311 nm) excitable samarium doped gadolinium yttrium orthovanadate, (Gd,Y)VO4:Sm3+, nanocrystals. X-ray diffraction and Rietveld refinement studies confirmed that the synthesized samples crystallize in a tetragonal structure withI41/amdspace group. The enhanced photoluminescence intensity of (Gd,Y)VO4:Sm3+compared with the existing YVO4:Sm3+phosphor clearly indicates the significant role of Gd3+ions. This has been attributed to the sensitization of the6PJenergy level of Gd3+ions by energy transfer from orthovanadate (VO43−) ions and subsequent energy trapping by Sm3+ions. The energy transfer from VO43−to Sm3+viaGd3+ions as intermediates and concentration quenching of Gd3+luminescence are discussed in detail. The optical band gap of the as-prepared nanocrystals has been estimated using UV–vis–NIR absorption spectroscopy, which reveals a slightly higher band gap (3.75 eV) for YVO4as compared to GdYVO4(3.50 eV). Furthermore, confocal microcopy, decay parameters and Commission Internationale de l'Eclairage chromatic coordinates have supplemented these studies, which established the suitability of these nanophosphors for achieving spectral conversion in silicon solar cells.

Structure Characterization of Sulfate and Oxysulfate Phases Formed During Sulfuric Acid Digestion of Ilmenites

1996 ◽  
Vol 49 (7) ◽  
pp. 801 ◽  
Author(s):  
IE Grey ◽  
MR Lanyon ◽  
R Stranger
Keyword(s):  
Sulfuric Acid ◽  
Rietveld Method ◽  
Three Dimensional ◽  
Structure Characterization ◽  
Acid Digestion ◽  
X Ray Diffraction ◽  
Titanium Sulfate ◽  
Structural Relationships ◽  
Concentrated Sulfuric Acid

Laboratory digestion of natural and upgraded ilmenites with concentrated sulfuric acid has been carried out under conditions simulating the sulfate-route pigment process. X-Ray diffraction studies on the solid digestion cakes led to the characterization of a number of different iron titanium sulfate and oxysulfate compounds, whose formation was dependent on the ilmenite composition and digestion conditions. Two different sulfate phases were identified, with structures related to those for Fe2(SO4)3 and H2O[ Zr (HPO4)2]. Four different iron titanium oxysulfates , ( Fe,Ti )(O,OH)SO4, were identified as major digestion products, three having structures related to those for β-NbOPO4, GeOHPO4 and lazulite , Mg[AlOHPO4], and the fourth being a new struture type. The structures of the oxysulfate phases were refined by the Rietveld method. Both the sulfates and the oxysulfates have three-dimensional framework structures formed by corner linking of ( Ti,Fe )O6 octahedra and SO4 tetrahedra, and containing channels or interlayer regions that can be occupied by cations such as H3O+ and Fe2+. The different structures have many features in common. Their structural relationships are discussed and mechanisms are proposed for the phase transformations encountered in the digestion studies.

scholarly journals Synthesis, Spectral, Structural and Thermal Characterization of Inorganic Crystal: Phenyl Trimethylammonium Tetrachlorocobaltate

2019 ◽  
Vol 31 (8) ◽  
pp. 1779-1784
Author(s):  
V. Mohanraj ◽  
R. Pavithra ◽  
M. Thenmozhi ◽  
R. Umarani
Keyword(s):  
Three Dimensional ◽  
Thermal Characterization ◽  
Dimensional Structure ◽  
X Ray Diffraction ◽  
Monoclinic Crystal ◽  
Evaporation Technique ◽  
Ft Ir ◽  
Thermal Stability Of ◽  
Ft Ir Spectroscopy

Phenyl trimethylammonium tetrachlorocobaltate, crystals were grown by slow evaporation technique. The crystal was bright, transparent. The three dimensional structure of the phenyl trimethylammonium tetrachlorocobaltate was obtained from single crystal X-ray diffraction studies. The molecule belongs to monoclinic crystal system with C2/c space group. The presence of functional groups and modes of vibrations were identified by FT-IR spectroscopy. 1H NMR spectroscopy was also used to characterise the compound and the thermal stability of the crystal was established by TGA/DT analysis. This work undergoes phase transition which makes the study interesting.

Synthesis and Characterization of the Manganese Pyroarsenate Mn2As2O7 · 2H2O

2001 ◽  
Vol 56 (4-5) ◽  
pp. 359-363 ◽  
Author(s):  
N. Stock ◽  
G. D. Stucky ◽  
A. K. Cheetham
Keyword(s):  
Three Dimensional ◽  
Spectroscopic Studies ◽  
Mean Value ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Raman Spectroscopic ◽  
Distorted Octahedral ◽  
Ir And Raman ◽  
Hydrothermal Methods

Abstract The manganese pyroarsenate hydrate, Mn2As2O7 · 2 H2O, has been obtained as a single phase product using hydrothermal methods and the structure has been determined by single crystal X-ray diffraction. The title compound crystallizes in the monoclinic space group P21/n with a = 6.6576(4), b = 14.555(1), c = 7.8147(5) Å, β = 94.935(1)°, V = 754.46(8) Å3 and Z = 4. The manganese ions are each coordinated to five oxygen atoms and a water molecule in a distorted octahedral arrangement. Edge-sharing MnO6 octahedra form chains which are connected to a three-dimensional framework by As2O74- ions. The pyroarsenate anion, which attains a nearly eclipsed conformation, has a mean As-O distance for the terminal As-O bonds of 1.669(2) Å, while for the bridging oxygen atom a mean value of 1.757(2) Å is observed. Magnetic susceptibility measurements indicate the presence of high-spin Mn2+ ions. Thermogravimetric as well as IR and Raman spectroscopic studies of Mn2As2O7 · 2 H2O are presented.

scholarly journals The three-dimensional structure of a class-Pi glutathione S-transferase complexed with glutathione: the active-site hydration provides insights into the reaction mechanism

1998 ◽  
Vol 333 (3) ◽  
pp. 811-816 ◽  
Author(s):  
Antonio PÁRRAGA ◽  
Isabel GARCÍA-SÁEZ ◽  
Sinead B. WALSH ◽  
Timothy J. MANTLE ◽  
Miquel COLL
Keyword(s):  
Conformational Changes ◽  
Active Site ◽  
Three Dimensional ◽  
Dimensional Structure ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
Glutathione S Transferase ◽  
X Ray ◽  
The Right

The structure of mouse liver glutathione S-transferase P1-1 complexed with its substrate glutathione (GSH) has been determined by X-ray diffraction analysis. No conformational changes in the glutathione moiety or in the protein, other than small adjustments of some side chains, are observed when compared with glutathione adduct complexes. Our structure confirms that the role of Tyr-7 is to stabilize the thiolate by hydrogen bonding and to position it in the right orientation. A comparison of the enzyme–GSH structure reported here with previously described structures reveals rearrangements in a well-defined network of water molecules in the active site. One of these water molecules (W0), identified in the unliganded enzyme (carboxymethylated at Cys-47), is displaced by the binding of GSH, and a further water molecule (W4) is displaced following the binding of the electrophilic substrate and the formation of the glutathione conjugate. The possibility that one of these water molecules participates in the proton abstraction from the glutathione thiol is discussed.

Reaction-path calculations and crystal structures of 1,1′-(ethylene-1,2-diyl)dipyridinium dichloride dihydrate and 1,1′-(ethylene-1,2-diyl)dipyridinium dibromide

2016 ◽  
Vol 72 (2) ◽  
pp. 112-118
Author(s):  
Mwaffak Rukiah ◽  
Mahmoud M. Al-Ktaifani ◽  
Mohammad K. Sabra
Keyword(s):  
Hydrogen Bonds ◽  
Crystal Engineering ◽  
Materials Science ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
Substitution Reactions ◽  
Nucleophilic Substitutions ◽  
Triclinic Space Group ◽  
Pyridinium Bromide ◽  
Multinuclear Nmr Spectroscopy

The design of new organic–inorganic hybrid ionic materials is of interest for various applications, particularly in the areas of crystal engineering, supramolecular chemistry and materials science. The monohalogenated intermediates 1-(2-chloroethyl)pyridinium chloride, C5H5NCH2CH2Cl+·Cl−, (I′), and 1-(2-bromoethyl)pyridinium bromide, C5H5NCH2CH2Br+·Br−, (II′), and the ionic disubstituted products 1,1′-(ethylene-1,2-diyl)dipyridinium dichloride dihydrate, C12H14N22+·2Cl−·2H2O, (I), and 1,1′-(ethylene-1,2-diyl)dipyridinium dibromide, C12H14N22+·2Br−, (II), have been isolated as powders from the reactions of pyridine with the appropriate 1,2-dihaloethanes. The monohalogenated intermediates (I′) and (II′) were characterized by multinuclear NMR spectroscopy, while (I) and (II) were structurally characterized using powder X-ray diffraction. Both (I) and (II) crystallize with half the empirical formula in the asymmetric unit in the triclinic space groupP\overline{1}. The organic 1,1′-(ethylene-1,2-diyl)dipyridinium dications, which display approximateC2hsymmetry in both structures, are situated on inversion centres. The components in (I) are linkedviaintermolecular O—H...Cl, C—H...Cl and C—H...O hydrogen bonds into a three-dimensional framework, while for (II), they are connectedviaweak intermolecular C—H...Br hydrogen bonds into one-dimensional chains in the [110] direction. The nucleophilic substitution reactions of 1,2-dichloroethane and 1,2-dibromoethane with pyridine have been investigated byab initioquantum chemical calculations using the 6–31G** basis. In both cases, the reactions occur in two exothermic stages involving consecutive SN2 nucleophilic substitutions. The isolation of the monosubstituted intermediate in each case is strong evidence that the second step is not fast relative to the first.

D-8 Materials Science Applications of the Three Dimensional X-ray Diffraction Microscope

2004 ◽  
Vol 19 (2) ◽  
pp. 197-197
Author(s):  
L. Margulies ◽  
S. Schmidt ◽  
E. M. Lauridsen ◽  
H. F. Poulsen ◽  
D. Juul Jensen ◽  
...  
Keyword(s):  
Materials Science ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
X Ray
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