Wideline 1H NMR Study on Hydrated Layered Sulfides K0.5(H2O)y[NbS2] and Na0.5(H2O)y[NbS2]

1977 ◽  
Vol 32 (9) ◽  
pp. 1033-1037 ◽  
Author(s):  
Anton Lerf ◽  
Paul Burkert ◽  
Jürgen O. Besenhard ◽  
Robert Schöllhorn
Keyword(s):  
1H Nmr ◽  
Nmr Spectra ◽  
Room Temperature ◽  
Interlayer Space ◽  
Water Molecules ◽  
Structural Scheme ◽  
H Nmr ◽  
Nmr Study

H NMR spectra of different hydration stages show that the water molecules in hydrated layered niobium sulfides A0.5(H2O)y[NbS2] are rather mobile at room temperature. A structural scheme of water arrangement in the interlayer space is proposed with the C2-axis of the H2O molecules parallel to the basal planes of the NbS2 layer units.

A 15N, 13C, and 1H NMR study of reaction products from arylguanidines and chloroformate esters

1991 ◽  
Vol 56 (7) ◽  
pp. 1505-1511 ◽  
Author(s):  
Antonín Lyčka ◽  
Karel Palát
Keyword(s):  
1H Nmr ◽  
Nmr Spectra ◽  
Reaction Products ◽  
H Nmr ◽  
Nmr Study

The 15N, 13C, and 1H NMR spectra of the reaction products from arylguanidines with two mols of chloroformate esters have been measured. With application of the corresponding 15N isotopomer it has been proved that the reaction products have the structures IIIa-IIIc.

Nuclear magnetic resonance studies of the methylammonium hexahalotellurates

1992 ◽  
Vol 70 (3) ◽  
pp. 849-855 ◽  
Author(s):  
Mark R. MacIntosh ◽  
Marco L. H. Gruwel ◽  
Katherine N. Robertson ◽  
Roderick E. Wasylishen
Keyword(s):  
Line Shape ◽  
Nmr Spectra ◽  
Room Temperature ◽  
Solid Phase ◽  
Variable Temperature ◽  
Spin Lattice Relaxation ◽  
Temperature Phase ◽  
H Nmr ◽  
Nmr Study ◽  
Correlated Motion

A 2H and 14N NMR study of the solid methylammonium hexahalotellurates, (MA)2TeX6 (MA = CH3ND3+ or CD3NH3+, X = Cl, Br, and I), has been undertaken to characterize the dynamics of the methylammonium (MA) ion as a function of temperature. At room temperature, the MA ion in the hexachlorotellurate (solid II) is confined to C3 jumps about the C—N axis while a small angle libration of the C—N axis is occurring. In the room temperature phase, solid I, of (MA)2TeBr6 and (MA)2TeI6 the MA ions are performing overall reorientations on the ps time scale, averaging the 2H nuclear quadrupolar interactions to zero. Variable temperature 2H NMR spin-lattice relaxation times, T1, indicate an activation energy, EA, for "isotropic" reorientations of the CH3ND3+ ion of 5.2 ± 0.5 and 2.6 ± 0.3 kJ mol−1 for X = Br and I, respectively. Deuterium T1 values for C-deuterated MA ion in the hexaiodotellurate indicate an EA for whole-ion reorientation of 3.1 ± 0.3 kJ mol−1. At any given temperature, the correlation time, τc, derived from the T1 results was found to be the same for the two deuterium-labelled hexaiodotellurates. The similarity of both the EA and the τc values implies correlated motion of the methyl and ammonium groups. The 14N T1 results for solid I of (MA)2TeI6 indicate that C—N axis motions, with an EA = 5.6 ± 0.6 kJ mol−1, are more hindered than N—D or C—D bond dynamics. The 2H NMR spectra for (MA)2TeI6 (solid II) and (MA)2TeBr6 (solids II, III, and IV) are characterized by a Pake doublet line shape. The measured peak-to-peak splittings are less than what is predicted by C3 motion about the molecular symmetry axis. It is possible to model these line shapes by postulating that C3 rotations of the methyl and ammonium groups occur as the C—N axis librates in an effective cone about the position of the static molecular axis. For (CH3ND3)2TeBr6 and (CD3NH3)3TeBr6 the peak-to-peak splittings in the 2H NMR spectra were measured as a function of temperature in solid phases II, III, and IV and were found to be similar. Finally, the 2H NMR line shape relaxation for (MA)2TeBr6 (solid III) displays an orientation dependence indicating that rotations about the C—N axis are discrete rather than diffusive in nature. For solid phase II of (MA)2TeCl6, the line shape is observed to relax isotropically, implying that continuous C3 rotations are taking place. Keywords: 2H and 14N NMR, methylammonium hexahalotellurates, molecular motion.

1H NMR study of the solvolysis of the paramagnetic tetrachloro-bis(imidazole)ruthenium(III) anion in water, methanol, and dimethyl sulfoxide

1995 ◽  
Vol 73 (4) ◽  
pp. 471-482 ◽  
Author(s):  
Craig Anderson ◽  
André L. Beauchamp
Keyword(s):  
Dimethyl Sulfoxide ◽  
1H Nmr ◽  
Room Temperature ◽  
Single Species ◽  
X Ray Diffraction ◽  
Chloro Complexes ◽  
X Ray ◽  
H Nmr ◽  
Nmr Study ◽  
Nmr Signals

The 1H NMR signals of the Ru(III) species present in solution are considerably broadened and shifted by paramagnetism, but they can be used to follow chloride displacement in the trans-[RuCl4Im2]− ion. This anion remains predominant for several hours at room temperature in D2O, but its signals are progressively replaced by those of a monoaqua [RuCl3(D2O)Im2] complex. Over a period of days, two new sets of peaks appear, corresponding to two isomers of [RuCl2(D2O)2Im2]+. The same behaviour is observed for the 1-methyl-and 4-methylimidazole analogues. These reactions can be driven backwards by addition of KCl, but [RuCl4Im2]− is not quantitatively regenerated in solution even for 6 M NaCl. Within several months, the [RuCl2(D2O)2Im2]+ isomers further aquate to a single species [RuCl(D2O)3Im2]2+. In CD3OD, displacement of the first chloride of [RuCl4Im2]− takes place faster, over several hours, but substitution stops at the [RuCl3(CD3OD)Im2] stage. In DMSO, substitution occurs very slowly. The [RuCl3(DMSO)Im2]:[RuCl4Im2]−mixture (1:2) obtained after 12 days starts to show very slow reduction to two Ru(II) species, one of which precipitates as yellow crystals. From X-ray diffraction work (monoclinic, P21/n, a = 9.951, b = 8.564, c = 10.527 Å, β = 92.95°, R = 0.033), the compound was identified as [RuCl2(DMSO-d6)2Im2], where the metal has a trans-trans-trans coordination and the DMSO ligands are S-bonded. Keywords: paramagnetic ruthenium anion, solvolysis, chloro complexes.

Dynamics of Water in Crystal Hydrates

1967 ◽  
Vol 22 (9) ◽  
pp. 1433-1440 ◽  
Author(s):  
Ingo Berthold ◽  
Alarich Weiss
Keyword(s):  
Single Crystals ◽  
Nmr Spectra ◽  
Room Temperature ◽  
Dynamical Behaviour ◽  
Water Molecules ◽  
H Nmr ◽  
Direction Cosines ◽  
Infrared Data

The 1H-NMR spectra of Na2S2O62 H20 and Li2S2Oe· 2 H20 single crystals have been investi-· gated at room temperature. The influence on the NMR spectra by the dynamical behaviour of the water molecules is discussed. The direction cosines of the different p—p lines were determined with a modified PAKE formula given by PEDERSEN. The parameters of the librational motions of the water molecules were calculated by the help of infrared data. The equilibrium H —H-distance in the water molecules was found to be 1.52 A.

An 1H NMR Study on the Cationic Motion in Solid tert-Butylammonium Chloride and Bromide

1991 ◽  
Vol 46 (3) ◽  
pp. 265-268 ◽  
Author(s):  
Hiroyuki Ishida ◽  
Syuichi Inada ◽  
Naomi Hayama ◽  
Daiyu Nakamura ◽  
Ryuichi Ikeda
Keyword(s):  
Relaxation Time ◽  
1H Nmr ◽  
Room Temperature ◽  
Lattice Relaxation ◽  
Lattice Relaxation Time ◽  
Spin Lattice Relaxation ◽  
X Ray ◽  
Spin Lattice ◽  
H Nmr ◽  
Nmr Study

AbstractThe 1H spin-lattice relaxation time (T1) in solid (CD3)3CNH3Cl and (CD3)3CNH3Br was measured above room temperature and the motional parameters for the reorientation of the NH3+ groups were determined. The 1H NMR absorptions measured in the same temperature range for (CH3)3CNH3Cl and (CH3)3CNH3Br indicate the presence of superimposed several cationic motions commonly taking place in both compounds. From X-ray powder patterns taken at room temperature, the bromide was found to be isomorphous with the chloride

1H NMR, 31P NMR and Raman Study of CaHPO4 and SrHPO4

2005 ◽  
Vol 60 (1-2) ◽  
pp. 121-126 ◽  
Author(s):  
B. Louati ◽  
K. Guidara ◽  
M. Gargouri ◽  
M. Fourati
Keyword(s):  
1H Nmr ◽  
Nmr Spectra ◽  
Room Temperature ◽  
31P Nmr ◽  
Cross Polarization ◽  
Nmr Spectrum ◽  
H Nmr ◽  
Nmr Techniques ◽  
Raman Study

CaHPO4 and SrHPO4 were investigated using Raman, 1H NMR and 31P NMR techniques to study the environment of their PO3−4 tetrahedra and the percentage of mobile protons. 1H NMR spectra at room temperature suggest the presence of three types of protons, in agreement with RX investigation. The percentage of mobile protons in SrHPO4 is greater than in CaHPO4 because Sr2+ is bigger than Ca2+. 31P NMR spectra at room temperature show two lines in the spectrum of SrHPO4, revealing an equal environment of two sets of pairs of PO3− 4 . The 31P NMR spectrum of CaHPO4, however, exhibits three lines. This result was confirmed using a cross polarization (CP) sequence program. The first peak is attributed to the first set of pairs of P(1)O4 units and the two other ones to P(2)O4 and P(2)O4 units.

Preparation and 1H NMR study of soluble alkoxy, alkyl and arylamido derivatives of sodium tetraamidoaluminate

1982 ◽  
Vol 47 (2) ◽  
pp. 384-391 ◽  
Author(s):  
Otomar Kříž ◽  
František Mareš ◽  
Bohuslav Čásenský
Keyword(s):  
1H Nmr ◽  
Aromatic Amines ◽  
Nmr Spectra ◽  
Pyridine Solution ◽  
Molecular Weights ◽  
H Nmr ◽  
Nmr Study ◽  
Derivatives Of

Sodium tetraamidoaluminate reacts with alcohols and aromatic amines under formation of sodium alkoxyimidoaluminates or amido(arylamido)aluminates, respectively. The corresponding sodium amido(alkylamido)aluminates were prepared from sodium tetraamidoaluminate and sodium tetrakis(alkylamido)aluminates in 1,2-dimethoxyethane or pyridine solution. 1H NMR spectra and in some cases also the cryoscopic molecular weights of the prepared compounds were measured.

119Sn, 15N, 13C, and 1H NMR Study of the Intramolecular Sn-N Donor-Acceptor Interaction in [2-(Dimethylaminomethyl)phenyl]stannanes

1998 ◽  
Vol 63 (7) ◽  
pp. 977-989 ◽  
Author(s):  
Aleš Růžička ◽  
Vladimír Pejchal ◽  
Jaroslav Holeček ◽  
Antonín Lyčka ◽  
Klaus Jacob
Keyword(s):  
1H Nmr ◽  
Nmr Spectra ◽  
Intramolecular Interaction ◽  
Coupling Constants ◽  
Acceptor Interaction ◽  
H Nmr ◽  
Nmr Parameters ◽  
Nmr Study ◽  
Donor Acceptor ◽  
Characteristic Values

119Sn, 15N, 13C, and 1H NMR spectra were studied for [2-(dimethylaminomethyl)phenyl]stannanes, R1R2R3R4Sn or R1R2R24Sn, where R1, R2, and R3 are 1-butyl, Cl or Br, the same or different, and R4 is 2-(dimethylaminomethyl)phenyl. The occurrence of intramolecular interaction between the nitrogen and tin atoms was demonstrated based on changes in the characteristic values of the NMR parameters of these nuclides (δ(15N), δ(119Sn), J(119Sn,15N), and their interrelations, as well as on the relatively high values of the coupling constants 3J(119Sn,13C(CH2)).

1H NMR Study of 3,5-Disubstituted 6-Oxo-1,6-dihydro-1,2,4-triazines

1995 ◽  
Vol 60 (2) ◽  
pp. 251-256
Author(s):  
Karel Nálepa ◽  
Aleš Halama ◽  
Taťjana Nevěčná ◽  
Vojtěch Bekárek
Keyword(s):  
Temperature Dependence ◽  
1H Nmr ◽  
Nmr Spectra ◽  
Thermodynamic Characteristics ◽  
H Nmr ◽  
Nmr Study

1H NMR spectra have been measured of seven 3,5-disubstituted 6-oxo-1,6-dihydro-1,2,4-triazines, and tautomerism of these compounds has been evaluated in connection with the nature of substituents, medium, and temperature. The title compounds exist in their benzyl or benzylidene forms or as a mixture of both forms. Thermodynamic characteristics of the transition between the two forms have been determined from the temperature dependence of NMR spectra of three derivatives.

scholarly journals 1H-NMR study of some new acetyl dimethylbiphenyls: unambiguous signal assignment for the methyl groups

1997 ◽  
Vol 13 (2) ◽  
pp. 125-129 ◽  
Author(s):  
Fadhil S. Kamounah ◽  
Salam J. Titinchi
Keyword(s):  
1H Nmr ◽  
Structure Elucidation ◽  
Nmr Spectra ◽  
Methyl Groups ◽  
H Nmr ◽  
Signal Assignment ◽  
Nmr Study

The abundance1H-NMR spectra of some new mono- and diacetyl compounds derived from 2,2′-dimethyl-, 3,3′-dimethyl-, and 4,4′-dimethylbiphenyls were recorded. Unambiguous signal assignment of the methyl groups of the aromatic biphenyl rings were made for the structure elucidation.

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