scholarly journals Hydrogen Bond Studies. 125. A Deuteron Magnetic Resonance Study of Strontium Formate Dihydrate, Sr(HCOO)2 · 2D2O

1977 ◽  
Vol 32 (9) ◽  
pp. 1025-1029 ◽  
Author(s):  
Bo Berglund ◽  
Jörgen Tegenfeldt
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Magnetic Resonance ◽  
Electric Field Gradient ◽  
Room Temperature ◽  
Coupling Constants ◽  
Water Molecules ◽  
Magnetic Resonance Study ◽  
Quadrupole Coupling ◽  
Asymmetry Parameters

AbstractA room temperature (25 °C) deuteron magnetic resonance (DMR) study of a single crystal of Sr (HCOO)2 · 2 D2O is reported. Signals from all water molecules in the unit cell have been detected, and all four independent electric field gradient (EFG) tensors at the water deuterons have been determined from 409 quadrupole splittings. All spectra were recorded by rotating the crystal about one arbitrarily selected axis. The following quadrupole coupling constants and asymmetry parameters for the deuterons were obtained: 213.5(4), 189.3(4), 195.7(4) and 200.7(5) kHz and 0.117(3), 0.110(4), 0.116(4) and 0.098(3). The directions of the eigenvalues are qualitatively consistent with the crystal structure refined by Galigné 1; the result is in disagreement, however, with the earlier DMR study of Sr (DCOO)2 · 2 D2O (Reference 2).

Experimental Study of Nuclear Electric Quadrupole Splittings of 59Co in Co(NH3)6Cl3

1974 ◽  
Vol 52 (15) ◽  
pp. 1398-1404 ◽  
Author(s):  
E. C. Reynhardt
Keyword(s):  
Experimental Study ◽  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Electric Field Gradient ◽  
Room Temperature ◽  
Electric Quadrupole ◽  
Coupling Constants ◽  
Principal Axes ◽  
Quadrupole Coupling ◽  
Asymmetry Parameters

The nuclear magnetic resonance of 59Co in a single crystal of Co(NH3)6Cl3 has been investigated at room temperature at 15 kG. Observed quadrupolar perturbations have been analyzed by the method of Volkoff for three orthogonal planes to yield five electric field gradient tensors. The cobalt sites associated with these tensors are nonequivalent. The quadrupole coupling constants and asymmetry parameters vary from 1.0 to 17.2 MHz and 0.10 to 0.57 respectively. One of the principal axes of each tensor is found to coincide with the crystallographic b axis of the monoclinic unit cell.

The Electric Field Gradient at the Site of the Halogen Ion and Structure of Amino Acid Hydrobromides and Hydroiodides

1992 ◽  
Vol 47 (7-8) ◽  
pp. 887-917
Author(s):  
Armin Kehrer ◽  
Shi-qi Dou ◽  
Alarieh Weiss
Keyword(s):  
Electric Field ◽  
Electric Field Gradient ◽  
Field Gradient ◽  
Room Temperature ◽  
Low Frequency ◽  
Coupling Constants ◽  
Coupling Constant ◽  
Resonance Frequencies ◽  
Quadrupole Coupling ◽  
Frequency Coupling

Abstract The 79,81Br and 127I NQR spectra of several hydrobromides, respectively hydroiodides, of amino acides and dipeptides were studied, mostly as functions of temperature in the range 77 < T/K <420. The investigated compounds are: L-Arg • HBr • H2O, L-Cys • HBr • H2O , L - Cys - S - S - L - Cys • 2HBr, ethanolamine • HBr, L-Glu • HBr, L-His • HBr, L-His • 2HBr, L-Ile HBr • H2O , Sar • HBr, (Sar)2 • HBr, L-Val • HBr • H2O , Gly • LiBr, Gly-Gly • LiBr, ethanolamine HI, Sar • HI, (Sar)2 • HI, (Gly)2 • HI, (L-Val)2 • HI, Gly-L-Leu • HI • H2O . A phase transition with hysteresis was observed for L-Val • HBr • H2O (Tc.up = 318 K, Tc.down = 242 K). Two solid phases of Sar • HI have been studied by NQR, one crystallized from melt, the other one from aqueous solution. For three of the title compounds the crystal structure was determined at room temperature: L-His - 2HBr, P212121 , Z = 4, aj pm = 1652, b/pm = 916, c/pm = 721; L-Cys HBr H2O , P212121 , Z = 4, a/pm = 1955, b/pm = 746, c/pm = 550; Gly-L-Leu • HI • H2O , P2X, Z = 2, a / p m = 1289, b/pm = 914, c/pm = 615, ß/° = 99.In most cases the halogen ion in the studied hydrohalides is polycoordinated by hydrogen bonds of the type N - H • • • X⊖ and O - H • • • X⊖ , X = Br, I. The NQR frequencies and, for iodine, the nuclear quadrupole coupling constants depend on this coordination. A low frequency (coupling constant) region is found for pure N - H • • • X⊖ coordination. Replacing one N - H • • • X⊖ bond by O - H • • • X⊖ rises the electric field gradient, EFG, respectively the resonance frequencies. The dependence of the EFG on the hydrogen bond coordination N - H • • • X⊖ plus O - H • • • X⊖ is discussed for the title compounds including information from literature

(CH3)3CCOOSbCl4: Structure Determination by Zeeman Perturbed NQR

1986 ◽  
Vol 41 (1-2) ◽  
pp. 129-133 ◽  
Author(s):  
Maria L. S. Garcia ◽  
Edwin A. C. Lucken
Keyword(s):  
Molecular Structure ◽  
Magnetic Field ◽  
Crystal Structure ◽  
Single Crystal ◽  
Structure Determination ◽  
Organic Ligand ◽  
Coupling Constants ◽  
Zero Field ◽  
Quadrupole Coupling ◽  
Asymmetry Parameters

A single crystal of tetrachloro(0,0-pivaloylato)antimony(V) has been studied at 77 K, byZeeman perturbed 35Cl NQR, using a FT-NQR pulsed spectrometer. The four lines at zero-field, ν1 = 27.6468, ν2= 27.3070, ν3= 25.7341 and ν4= 25.3438 MHz yield eight EFG tensors in themagnetic field, related by a twofold symmetry element in the crystal. The correspondingasymmetry parameters are η1, = 0.134, η2 = 0.13, η3= 0.07, and η4 = 0.09. The molecular structurededuced from the relative orientations of the principal Z-axes of the EFG tensors confirms that thehigher quadrupole coupling constants are associated with the chlorine atoms in equatorial positions,relative to the plane of the organic ligand, as predicted from NQR powder studies. It is concludedthat the crystal structure is monoclinic with two (class m or 2) or four (class 2/m) moleculesper unit cell. The molecular packing is such that the planes formed by equatorial or axial chlorineatoms are approximately at right angles to their symmetry related images.

Nuclear Quadrupole Resonance of Antimony in Ln3Sb5O12 Crystals

1994 ◽  
Vol 49 (6) ◽  
pp. 687-689 ◽  
Author(s):  
A. M. Raevsky ◽  
A. G. Gukalova ◽  
G. K. Semin
Keyword(s):  
Electric Field ◽  
Electric Field Gradient ◽  
Coupling Constants ◽  
Spectral Parameters ◽  
Compression Effect ◽  
Quadrupole Coupling ◽  
Quadrupole Resonance ◽  
Nuclear Quadrupole ◽  
Asymmetry Parameters ◽  
Lanthanide Compression

Abstract Complete 121,123Sb NQR spectra of crystalline rate earth antimonites Ln3Sb5O12 (Ln = La, Nd, Er, Lu) were recorded at 77 K. The quadrupole coupling constants and asymmetry parameters of the electric field gradient were measured. A “lanthanide compression” effect on the antimony NQR was observed. Using relations found for the antimonites under study, the Sb spectral parameters of other lanthanide compounds can be predicted.

A Comparative Nuclear Magnetic Resonance Study of the Solvation of CuClO4 in Binary Mixtures of Acetonitrile with Pyridine and Picolines at 298K

2012 ◽  
Vol 67 (5) ◽  
pp. 303-307 ◽  
Author(s):  
Dip Singh Gill ◽  
Dilbag Singh Rana ◽  
Mohinder Singh Chauhan
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Binary Mixtures ◽  
Nuclear Magnetic Resonance Study ◽  
Coupling Constants ◽  
Mixed Complex ◽  
Magnetic Resonance Study ◽  
Quadrupole Coupling ◽  
Ubbelohde Viscometer ◽  
Nuclear Magnetic

63Cu nuclear magnetic resonance (NMR) and viscosity studies of 0:064M CuClO4 solutions have been reported in binary mixtures of acetonitrile (AN) with pyridine (Py) and 2, 3, and 4-picolines (2,3,4-Pic) at 298 K using a Bruker 500 MHz NMR spectrometer and an Ubbelohde viscometer, respectively. Chemical shift d and linewidth D for the 63Cu signals have been recorded referenced to a 0:064M CuClO4 solution in anhydrous AN. The copper quadrupole coupling constants (e2Qq=h) have been calculated in all cases. The variation of the d and e2Qq=h values as a function of mol fraction of the co-solvent show that all these bases interact with Cu+ more strongly than AN. They replace AN from the Cu+ complexed with AN in the form [Cu(AN)4]+ and form a mixed complex of the type [Cu(AN)4-x(S)x]+ (x=1 - 4) where S stands for the base. At relatively high mole fraction of the co-solvents, the mixed solvated complex gradually changes to a more symmetrical complex of the type [Cu(S)4]+ which remains stable in the solution. The solvating effect of 2-Pic and 4-Pic is observed to be stronger than that of Py and 3-Pic.

Quadrupoleffekte der magnetischen Kernresonanz an 11B in Bor-Stickstoffverbindungen

1969 ◽  
Vol 24 (4) ◽  
pp. 566-572 ◽  
Author(s):  
Klaus Wiedemann ◽  
Jürgen Voitländer
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Quadrupole Interaction ◽  
Second Order ◽  
Coupling Constants ◽  
Quadrupole Coupling ◽  
Wide Line ◽  
Nuclear Quadrupole ◽  
Asymmetry Parameters ◽  
Nuclear Magnetic

Abstract First and second-order quadrupole effects of the 11B nuclear magnetic resonance have been measured in polycrystalline samples of dimere dimethylaminoboranes and tetramethylboracene. With the theory of powder patterns for first and second-order quadrupole interaction the nuclear quadrupole coupling constants e2 q Q/h and asymmetry parameters η of 11B have been determined. For these measurements boron-free inserts had to be constructed for the probes of the Varian Wide Line Spectrometer DA 60.

scholarly journals Crystal Structure Refinement and Single Crystal 81Br Zeeman NQR Study of KHgBr3· H2O

1996 ◽  
Vol 51 (12) ◽  
pp. 1197-1202 ◽  
Author(s):  
Hiromitu Terao ◽  
Tsutomu Okuda ◽  
Sachiyo Uyama ◽  
Hisao Negita ◽  
Shi-qi Dou ◽  
...  
Keyword(s):  
Single Crystal ◽  
Room Temperature ◽  
Structure Refinement ◽  
Zeeman Effect ◽  
Coupling Constants ◽  
X Ray ◽  
Quadrupole Coupling ◽  
Nuclear Quadrupole ◽  
Asymmetry Parameters ◽  
Good Agreement

Abstract Three 81Br NQR resonance lines of KHgBr3 ·H2O were detected between 77 K and room temperature. From the Zeeman effect measurement on a single crystal the nuclear quadrupole coupling constants (e2qQ/h) and the asymmetry parameters (ƞ) were obtained, which are 228.42 MHz and 0.005, 226.24 MHz and 0.005, and 108.76 MHz and 0.465 for e2qQ/h and ƞ at 295 K, respectively. Large deviations of the observed directions of electric field gradient tensors from the directions expected from previous X-ray results have been found. With the present X-ray redetermination, 81Br NQR and structure are in good agreement. The structure and bonding in the compound are discussed.

scholarly journals Crystal structure of the sesquihydrate of dehydroepiandrosterone propan-2-ylidene hydrazone: Participation of the hydrazonyl nitrogen atoms as acceptors in the elaborate hydrogen bond scheme

2021 ◽  
Vol 12 (1) ◽  
pp. 81-85
Author(s):  
James Lewis Wardell ◽  
John Nicholson Low
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Hydrogen Bonds ◽  
Room Temperature ◽  
Water Molecules ◽  
Torsional Angle ◽  
Orthorhombic Space Group ◽  
The Difference ◽  
Torsional Angles ◽  
Water Hydrogen

The crystal structure of the sesquihydrate of dehydroepiandrosterone propan-2-ylidene hydrazone, [(7)2·(H2O)3], isolated from a solution of dehydroepiandrosterone propan-2-ylidene hydrazone, (7), in moist ethanol at room temperature, has been determined from data collected at 100 K. The sesquihydrate recrystallizes in the orthorhombic space group, P212121 with Z = 8. The asymmetric unit of [(7)2·(H2O)3] consists of two independent molecules of the steroid, Mol A and Mol B, and three moles of water. The six membered saturated rings, A and C, in both molecules have ideal or near ideal chair shapes, the unsaturated rings, B, have the expected half-chair shapes, while the five-membered rings, D, have envelope shapes with flaps at C114 and C214 for Mol A and Mol B, respectively. Differences in the conformations of the two molecules reside essentially completely within the hydrazonyl fragments with significantly different torsional angles, C117-N120-N121-C122 (in Mol A) and C217-N220-N221-C222 (in Mol B), of 149.19(14) and -93.08(17)°, respectively. The difference in this torsional angle is reflected in the hydrogen bonds involving the nitrogen atoms in the hydrazonyl units: it is of interest that the hydrazonyl nitrogen atoms partake as acceptors in hydrogen bonding with water molecules. The only intermolecular interactions in these molecules are hydrogen bonds -all classical O-H-O and OH···N hydrogen bonds with just one exception, a C-H···O(water) hydrogen bond. Of interest, there are no direct steroid-steroid links: molecules are linked solely by hydrogen bonds involving the hydrate molecules. All three hydrate molecules take part in the indirect linking of the steroid molecules, but each has its own set of contacts.

Proton and deuteron magnetic resonance in single crystals of Fe(NH4)2(SO4)2∙6H2O

1983 ◽  
Vol 61 (1) ◽  
pp. 44-48 ◽  
Author(s):  
T. F. S. Raj ◽  
C. R. K. Murthy
Keyword(s):  
Magnetic Resonance ◽  
Room Temperature ◽  
Water Molecules ◽  
Hydrogen Atoms ◽  
Proton Proton ◽  
Coupling Tensor ◽  
Quadrupole Coupling ◽  
Resonance Data ◽  
Proton Magnetic Resonance Study ◽  
Crystallographic Axes

Single crystal proton and deuteron magnetic resonance in Fe(NH4)2(SO4)2∙6H2O and Fe(ND4)2(SO4)2∙6D2O, respectively, are studied at room temperature. From the proton magnetic resonance study are found the orientations of the proton–proton vectors of the water molecules with respect to the crystallographic axes. Proton resonance data are used to determine the positions of the hydrogen atoms belonging to the water molecules in the crystal. A deuteron resonance study shows that the D2O molecules are flipping fast at room temperature. The quadrupole coupling tensor at the deuteron sites of D2O in the crystal are determined. The positions of the hydrogen atoms are also determined from the directions of the principal components of the quadrupole coupling tensor.

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