Study by IR spectroscopy and x-ray diffraction analysis of the structural-phase changes during recalcination of kaolinite

1976 ◽  
Vol 25 (2) ◽  
pp. 1005-1009
Author(s):  
I. Kh. Moroz ◽  
Kh. S. Valeev

2006 ◽  
Vol 61 (1) ◽  
pp. 29-32 ◽  
Author(s):  
Holger Braunschweig ◽  
Holger Bera ◽  
Daniel Götz ◽  
Krzysztof Radacki

The reaction of the 1,2-dihalodiborane(4) B2(NMe2)2Cl2 with the lithium tungsten salts Li[(η5- C5H5)(R3P)(OC)2W] [R = Me (3a), Ph (3b)] yields via alkali salt elimination the phosphinesubstituted diborane(4)yl tungsten complexes [(η5-C5H5)(R3P)(OC)2W-{B(NMe2)-B(NMe2)Cl}] [R = Me (4a), Ph (4b)]. Both compounds have been fully characterized in solution by NMR and IR spectroscopy and 4a additionally by X-ray diffraction analysis.



Synthesis ◽  
2017 ◽  
Vol 49 (11) ◽  
pp. 2389-2393 ◽  
Author(s):  
Stefanie Pelzer ◽  
Beate Neumann ◽  
Hans-Georg Stammler ◽  
Nikolai Ignat’ev ◽  
Reint Eujen ◽  
...  

This paper describes the synthesis and comprehensive characterization of tetrakis(pentafluoroethyl)germane. In addition to a complete NMR spectroscopic characterization, including the rarely used 73Ge NMR spectroscopy, Ge(C2F5)4 was studied by IR spectroscopy, mass spectrometry as well as X-ray diffraction analysis. A 73Ge NMR investigation as well as an X-ray diffraction study of the related germane Ge(CF3)4 are also included.



2021 ◽  
Vol 47 (9) ◽  
pp. 593-600
Author(s):  
A. A. Lysova ◽  
V. A. Dubskikh ◽  
K. D. Abasheeva ◽  
A. A. Vasileva ◽  
D. G. Samsonenko ◽  
...  

Abstract Three new metal−organic frameworks based on scandium(III) cations and 2,5-thiophenedicarboxylic acid (H2Tdc) are synthesized: [Sc(Tdc)(OH)]·1.2DMF (I), [Sc(Tdc)(OH)]·2/3DMF (II), and (Me2NH2)[Sc3(Tdc)4(OH)2]·DMF (III) (DMF is N,N-dimethylformamide). The structures of the compounds are determined by single-crystal X-ray structure analysis (CIF file CCDC nos. 2067819 (I), 2067820 (II), and 2067821 (III)). The chemical and phase purity of compound I is proved by elemental analysis, thermogravimetry, X-ray diffraction analysis, and IR spectroscopy.



Synthesis ◽  
2020 ◽  
Vol 52 (07) ◽  
pp. 1025-1034 ◽  
Author(s):  
Marvin Linnemannstöns ◽  
Beate Neumann ◽  
Hans-Georg Stammler ◽  
Norbert W. Mitzel

Starting from trichloro(phenylethyl)silane, six differently fluorinated triaryl(phenylethyl)silanes were synthesized by salt elimination reactions and their structures were determined by X-ray diffraction analysis. Tris(pentafluorophenyl)(phenylethyl)silane reveals a folded structure due to intramolecular π-stacking interactions, while those with a lower degree of fluorination show either intermolecular π-stacking or no interplay between the aryl groups. A similar folded structure was observed for (4-methylphenethyl)tris(pentafluorophenyl)silane and [2-(naphth-2-yl)ethyl]tris(pentafluorophenyl)silane, both generated from the corresponding trichlorosilanes. In contrast, the inversely fluorinated [2-(pentafluorophenyl)ethyl]triphenylsilane only revealed intermolecular π-stacking interactions. Compounds with tetrafluoropyridyl substituents behave differently; with these compounds, π-stacking is only observed between the fluorinated units. All compounds were analyzed by NMR and IR spectroscopy, elemental analyses and single-crystal X-ray diffraction, and found to have strong H/C/N/F···F and N···C contacts.



Author(s):  
Petar Stanic ◽  
Marko Rodic ◽  
Tanja Soldatovic ◽  
Aleksandar Pavic ◽  
Natasa Radakovic ◽  
...  

The 3-arylidene-2-thiohydantoin derivative, 3-[(2-hydroxybenzyl-idene)amino]-2-thioxoimidazolidin-4-one, was synthesized in a two-step condensation reaction of 2-hydroxybenzaldehyde, thiosemicarbazide and ethyl chloroacetate. The ligand was structurally characterized by NMR and IR spectroscopy, as well as elemental analysis. In the reaction of the well-known polymeric trans-[CuCl2(DMSO)2]n complex with the polydentate thiohydantoin type ligand, instead of the corresponding copper thiohydantoin complex, unexpectedly, the dinuclear cis-[{CuCl(DMSO)2}(m-Cl)]2 complex (1) was formed predominantly as the final stable product. The structure of the complex 1 was confirmed by single crystal X-ray diffraction analysis. The cis-complex is obtained through assisted isomerization of the trans-form, in which the thiohydantoin derivative has a crucial role.



2013 ◽  
Vol 17 (08n09) ◽  
pp. 673-681 ◽  
Author(s):  
Chunhua Huang ◽  
Yi Zhang ◽  
Junshan Sun ◽  
Yongzhong Bian ◽  
Dennis P. Arnold

Bis/tris(phthalocyaninato) europium double- and triple-decker complexes Eu [ Pc (β- SC 6 H 13)8]2 (1) and Eu 2[ Pc (β- SC 6 H 13)8]3 (2) [ Pc (β- SC 6 H 13)8 = 2, 3, 9, 10, 16, 17, 23, 24-octakis(hexylthio)phthalocyaninate] have been synthesized and characterized by a series of spectroscopic methods including mass, NMR, electronic absorption and IR spectroscopy in addition to elemental analysis. Their molecular structures have been determined by single crystal X-ray diffraction analysis and electrochemical properties studied by cyclic voltammetry.



2008 ◽  
Vol 2008 ◽  
pp. 1-10 ◽  
Author(s):  
L. F. Krylova ◽  
L. M. Kovtunova ◽  
G. V. Romanenko

A sequence of stages in the syntheses of isomeric bisamino acid complexes of Pt(II) with -aminopropionic acid (-alanine = -AlaH) has been studied by the NMR spectroscopy. The techniques have been developed of the synthesis of thecis- andtrans-bischelates of Pt(II) and Pd(II) with -alanine as well as of the halide complexes oftrans- (M = Pt, Pd) andtrans- types. The NMR spectroscopy and IR spectroscopy (in the nuclei of ) and X-ray diffraction analysis have been used to examine the structures of the synthesized compounds.



1998 ◽  
Vol 31 (6) ◽  
pp. 845-850 ◽  
Author(s):  
Pavla Čapková ◽  
Ludvi´k Beneš ◽  
Klára Melánová ◽  
Henk Schenk

Molecular simulation supported by X-ray diffraction and IR spectroscopy has been used to analyse the structure of α-zirconium phosphate intercalated by ethanol, Zr(HPO4)2.2C2H5OH. Molecular-mechanics simulations using theCrystal Packermodule in theCerius2modelling environment revealed the crystal packing in the interlayer,i.e.the positions of ethanol with respect to the Zr(HPO4)2layers and the layer stacking in the intercalated structure. The average interlayer distanced\,=\,14.03 (13) Å obtained by modelling is in agreement with the experimentaldvalue of 14.05 (4) Å obtained from the X-ray diffraction analysis. The disorder in the Zr(HPO4)2.2C2H5OH structure found by molecular simulation has been confirmed by the character of the X-ray diffraction pattern.



2005 ◽  
Vol 19 (13) ◽  
pp. 2161-2166
Author(s):  
C. PELSHENKE ◽  
A. V. POP ◽  
O. COZAR

The influence of partial substitution of Nd by Gd on the temperature dependence of the lattice parameters of the optimal doped Nd 1.85 Ce 0.15 CuO 4n-type superconductor (maximum value of Tc) was studied by using X-ray diffraction measurements function of temperature. The transition from the structural normal phase (I4/mmm) to the distortion phase (Acam) was evidenced above y = 0.65 Gd substitution level in ( Nd 1-y Gd y)1.85 Ce 0.15 CuO 4. The structural phase transition temperature TI-A from undistorted phase to the distorted phase changes function of Gd concentration. The structural phase diagram for thermal controlled distortion by Gd ions, TI-A = f(y) was obtained, and compared by the superconducting phase diagram Tc(y).



1989 ◽  
Vol 03 (09) ◽  
pp. 685-693 ◽  
Author(s):  
S.L. YUAN ◽  
W.Y. GUAN ◽  
Z.J. CHEN ◽  
Y.L. HUANG ◽  
Y.B. JIA ◽  
...  

The results of X-ray diffraction analysis at low temperatures for bismuth-based high-Tc oxide superconductors are reported in this letter. There is no significant structural phase transition during superconducting transition. However, it appears that the cell parameters change anomalously before superconducting transition. This anomalous change in cell parameters is repeated for different bismuth-based high-Tc oxide superconductors.



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