scholarly journals Inference of principal species in caustic aluminate solutions through solid-state spectroscopic characterization

2020 ◽  
Vol 49 (18) ◽  
pp. 5869-5880 ◽  
Author(s):  
Mateusz Dembowski ◽  
Micah P. Prange ◽  
Maxime Pouvreau ◽  
Trent R. Graham ◽  
Mark E. Bowden ◽  
...  
Keyword(s):  
Solid State ◽  
Spectroscopic Characterization ◽  
Ir And Raman ◽  
Principal Species

Tetrahedrally coordinated Al(OH)4− and Al2O(OH)62− have been isolated in the solid-state and interrogated using XRD, NMR, XAS, IR, and Raman.

Neutral 4-phenyl-1-[phenyl(pyridin-2-yl)methylidene]semicarbazide and its salt forms with inorganic anions

2019 ◽  
Vol 75 (1) ◽  
pp. 1-7
Author(s):  
Vinicius Oliveira Araujo ◽  
Bárbara Tirloni ◽  
Lívia Streit ◽  
Vânia Denise Schwade
Keyword(s):  
Solid State ◽  
Spectroscopic Characterization ◽  
Water Molecules ◽  
Keto Form ◽  
Chloride Dihydrate ◽  
Ir And Nmr Spectroscopy ◽  
Tautomeric Forms ◽  
Counter Ions ◽  
Salt Forms ◽  
Good Agreement

Semicarbazones can exist in two tautomeric forms. In the solid state, they are found in the keto form. This work presents the synthesis, structures and spectroscopic characterization (IR and NMR spectroscopy) of four such compounds, namely the neutral molecule 4-phenyl-1-[phenyl(pyridin-2-yl)methylidene]semicarbazide, C19H16N4O, (I), abbreviated as HBzPyS, and three different hydrated salts, namely the chloride dihydrate, C19H17N4O+·Cl−·2H2O, (II), the nitrate dihydrate, C19H17N4O+·NO3 −·2H2O, (III), and the thiocyanate 2.5-hydrate, C19H17N4O+·SCN−·2.5H2O, (IV), of 2-[phenyl({[(phenylcarbamoyl)amino]imino})methyl]pyridinium, abbreviated as [H2BzPyS]+·X −·nH2O, with X = Cl− and n = 2 for (II), X = NO3 − and n = 2 for (III), and X = SCN− and n = 2.5 for (IV), showing the influence of the anionic form in the intermolecular interactions. Water molecules and counter-ions (chloride or nitrate) are involved in the formation of a two-dimensional arrangement by the establishment of hydrogen bonds with the N—H groups of the cation, stabilizing the E isomers in the solid state. The neutral HBzPyS molecule crystallized as the E isomer due to the existence of weak π–π interactions between pairs of molecules. The calculated IR spectrum of the hydrated [H2BzPyS]+ cation is in good agreement with the experimental results.

Gallium-containing Heusler phases ScRh2Ga, ScPd2Ga, TmRh2Ga and LuRh2Ga – magnetic and solid state NMR-spectroscopic characterization

2017 ◽  
Vol 72 (8) ◽  
pp. 609-615
Author(s):  
Lukas Heletta ◽  
Stefan Seidel ◽  
Christopher Benndorf ◽  
Hellmut Eckert ◽  
Rainer Pöttgen
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
Spectroscopic Characterization ◽  
Structural Disorder ◽  
X Ray Diffraction ◽  
Temperature Dependent ◽  
Phase Purity ◽  
X Ray ◽  
Arc Melting ◽  
Pauli Paramagnetism

AbstractThe gallium-containing Heusler phases ScRh2Ga, ScPd2Ga, TmRh2Ga and LuRh2Ga have been synthesized by arc-melting of the elements followed by different annealing sequences to improve phase purity. The samples have been studied by powder X-ray diffraction. The structures of Lu0.97Rh2Ga1.03 (Fm3̅m, a=632.94(5) pm, wR2=0.0590, 46 F2 values, seven variables) and Sc0.88Rh2Ga1.12 (a=618.91(4) pm, wR2=0.0284, 44 F2 values, six variables) have been refined from single crystal X-ray diffractometer data. Both gallides show structural disorder through Lu/Ga and Sc/Ga mixing. Temperature dependent magnetic susceptibility measurements showed Pauli paramagnetism for ScRh2Ga, ScPd2Ga, and LuRh2Ga and Curie-Weiss paramagnetism for TmRh2Ga. 45Sc and 71Ga solid state MAS NMR spectroscopic investigations of the Sc containing compounds confirmed the site mixing effects typically observed for Heusler phases. The data indicate that the effect of mixed Sc/Ga occupancy is significantly stronger in ScRh2Ga than in ScPd2Ga.

Solid-State Spectroscopic Characterization of α-Chitins Deacetylated in Homogeneous Solutions

2012 ◽  
Vol 116 (15) ◽  
pp. 4584-4592 ◽  
Author(s):  
Kai Zhang ◽  
Andreas Geissler ◽  
Steffen Fischer ◽  
Erica Brendler ◽  
Ernst Bäucker
Keyword(s):  
Solid State ◽  
Spectroscopic Characterization ◽  
Homogeneous Solutions

Polysulfonylamine, XXXVI Trimethylsilyl-dimesylamin: Darstellung, NMR-spektroskopische Charakterisierung und Reaktionsfähigkeit als Silylierungsreagens / Polysulfonylamines, XXXVI Trimethylsilyl Dimesylamine: Preparation, NMR-Spectroscopic Characterization, and Reactivity as a Silylating Agent

1992 ◽  
Vol 47 (12) ◽  
pp. 1693-1700 ◽  
Author(s):  
Armand Blaschette ◽  
Elke Wieland ◽  
Thomas Hamann ◽  
Robin K. Harris
Keyword(s):  
Solid State ◽  
Room Temperature ◽  
Spectroscopic Characterization ◽  
Equilibrium Mixture ◽  
Molar Ratio ◽  
Efficient Catalyst ◽  
Kinetic Measurements ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Silylating Agent

(CH3)3SiN(SO2CH3)2 (1), m. p. 69-70 °C, is obtained by metathesis of AgN(SO2CH3)2 with (CH3)3SiCl (improvement of a known procedure) or, more conveniently, by silylation of HN(SO2CH3)2 with [(CH3)3Si]2NH. The 1H, 13C and 29Si NMR solution spectra and the 29Si NMR solid-state spectrum suggest the constitution of 1 in solution (CDC13, CD2C12, CDCl2–CDCl2) to be an equilibrium mixture of the N-silylated form (CH3)3Si–N(SO2CH3)2 (I) and the O-silylated form (CH3)3Si–O–S(O)(CH3)=NSO2CH3 (II) in a molar ratio of 2:1 at room temperature, whereas in the known crystal structure of 1 only form I is present. The solid-state NMR experiment acted as a bridge between X-ray crystallography and solution-state NMR, enabling assignments of the resonances to be made with confidence to the tautomers. At room temperature, form II undergoes a rapid intramolecular 1.5-migration of silicon between oxygen centers of the two sulfonyl groups. As shown by kinetic measurements using 1H NMR spectroscopy, 1 is a highly reactive agent for silylating ketones in the presence of triethylamine. Hydroxy and thiol functions, even when sterically hindered, are silylated by 1 in uncatalyzed reactions. It is further shown that HN(SO2CH3)2 is an efficient catalyst for silylations with [(CH3)3Si]2NH.

Mefenamic Acid Anti-Inflammatory Drug: Probing Its Polymorphs by Vibrational (IR and Raman) and Solid-State NMR Spectroscopies

2014 ◽  
Vol 118 (16) ◽  
pp. 4333-4344 ◽  
Author(s):  
Vanessa R. R. Cunha ◽  
Celly M. S. Izumi ◽  
Philippe A. D. Petersen ◽  
Alviclér Magalhães ◽  
Marcia L. A. Temperini ◽  
...  
Keyword(s):  
Solid State ◽  
Mefenamic Acid ◽  
Solid State Nmr ◽  
Inflammatory Drug ◽  
Anti Inflammatory ◽  
Ir And Raman
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