Solid-state phosphorus-31 NMR studies of mercury(II) phosphonates. Anisotropies of the phosphorus-31 chemical shift and the phosphorus-31-mercury-199 indirect spin-spin coupling

1991 ◽  
Vol 30 (15) ◽  
pp. 2997-3002 ◽  
Author(s):  
William P. Power ◽  
Michael D. Lumsden ◽  
Roderick E. Wasylishen
Keyword(s):  
Solid State ◽  
Chemical Shift ◽  
Spin Coupling ◽  
Nmr Studies ◽  
Spin Spin Coupling

X-ray diffraction and solid-state 119Sn CP-MAS NMR studies of some triaryltin(IV) chlorides

2003 ◽  
Vol 81 (11) ◽  
pp. 1187-1195 ◽  
Author(s):  
Jordan M Geller ◽  
Ian S Butler ◽  
Denis FR Gilson ◽  
Frederick G Morin ◽  
Ivor Wharf ◽  
...  
Keyword(s):  
Solid State ◽  
Chemical Shift ◽  
Magic Angle Spinning ◽  
Mas Nmr ◽  
Spin Coupling ◽  
Magic Angle ◽  
X Ray ◽  
Tin Chloride ◽  
Angle Spinning ◽  
Spin Spin Coupling

The solid-state 119Sn cross-polarization (CP) magic angle spinning (MAS) NMR spectra of a series of triaryltin chlorides of the form Ar3SnCl have been acquired. The indirect spin-spin coupling constants (J(119Sn-35Cl)), quadrupolar-dipolar shifts (d(119Sn-35Cl)), and the 119Sn chemical shift tensors were extracted. For the spectrum of triphenyltin chloride (I) the validity of the first-order perturbation approximation was tested by comparing results of both the perturbation and cubic-equation approaches and a variable-temperature NMR study undertaken to investigate the influence of the previously reported molecular motion in the solid. The X-ray crystal structures of the tris(o-tolyl)tin chloride (II) and tris(p-tolyl)tin chloride (IV) complexes have been examined. They belong to the monoclinic and triclinic space groups P21/n and P[Formula: see text], respectively, which are different from the previously reported tris(m-tolyl)tin chloride (III) complex, which crystallizes in the space group R3 and has threefold molecular symmetry. The structures and NMR properties of the complexes with meta-substituents are quite different from those with ortho- or para-substituents having axially symmetric shift tensors with small spans and larger J values.Key words: aryltin chlorides, magic angle spinning NMR, tin-chlorine spin-spin coupling, 119Sn chemical shift tensor, crystal structure.

Solid-state nuclear magnetic resonance studies of triphenylsilyl-, triphenyltin-, and triphenyllead(pentacarbonyl)manganese(I) complexes

1999 ◽  
Vol 77 (11) ◽  
pp. 1892-1898 ◽  
Author(s):  
Dharamdat Christendat ◽  
Ian S Butler ◽  
Denis FR Gilson ◽  
Frederick G Morin
Keyword(s):  
Solid State ◽  
Chemical Shift ◽  
Dipolar Coupling ◽  
Chemical Shifts ◽  
Chemical Shift Anisotropy ◽  
Coupling Constants ◽  
Spin Coupling ◽  
Chemical Shift Tensors ◽  
Lead Compounds ◽  
Spin Spin Coupling

The solid-state CP MAS (29Si, 119Sn, and 207Pb) NMR spectra of the triphenylsilyl-, triphenyltin-, and triphenyllead(pentacarbonyl)manganese(I) complexes, (Ph3E)Mn(CO)5 (E = Si, Sn, Pb), have been analyzed to give the chemical shifts, one-bond spin-spin coupling constants, 1JE-Mn, the "effective-dipolar" coupling constants (D - ΔJ/3), the chemical shift tensors, and the spin-spin anisotropy (ΔJ), where the analysis permits. For the tin and lead compounds, three and four sets of chemical shifts, respectively, were observed, and two different polymorphs occur for the lead complex, depending on the solvent used for recrystallization. The average values of the reduced coupling constants, 1KMn-Si (2.64 × 1020 T2 J-1), 1KSn-Mn (1.25 × 1020 T2 J-1), and 1KPb-Mn (4.18 × 1020 T2 J-1) showed a linear correlation with the s-electron densities at the respective metal nuclei. The principal components of the chemical shift tensors have been determined for the tin and lead compounds.Key words: manganese-group-14 compounds, solid-state 29Si, 119Sn, and 207Pb CP MAS NMR, spin-spin coupling, chemical shift anisotropy, quadrupole coupling.

NMR spectroscopy of the solid-state isomerization of nitrito- and nitro-pentamminecobalt(III) chloride

2006 ◽  
Vol 84 (2) ◽  
pp. 300-308 ◽  
Author(s):  
Kristopher J Ooms ◽  
Roderick E Wasylishen
Keyword(s):  
Solid State ◽  
Chemical Shift ◽  
Nmr Spectra ◽  
Spin Coupling ◽  
Chemical Shift Tensor ◽  
Coupling Constant ◽  
Line Shapes ◽  
Quadrupolar Coupling ◽  
Shielding Tensor ◽  
Spin Spin Coupling

Cobalt-59 and nitrogen-15 NMR spectra of the nitritopentamminecobalt(III) chloride, [(NH3)5Co-ONO]Cl2, and nitropentamminecobalt(III) chloride, [(NH3)5Co-NO2]Cl2, isomers in the solid state have been obtained at several applied magnetic field strengths. The 59Co NMR line shapes indicate that both the cobalt nuclear quadrupolar coupling constant (CQ) and the span of the chemical shift tensor (Ω) decrease when the complex isomerizes from [(NH3)5Co-ONO]2+ to [(NH3)5Co-NO2]2+; CQ decreases from 23 to 10.3 MHz and Ω changes from 1650 to 260 ppm. The 15N NMR line shapes also show a significant change in the nitrogen magnetic shielding tensor upon isomerization, with Ω decreasing from 710 to 547 ppm; also, an indirect spin-spin coupling, 1J(59Co,15N) = 63 Hz, is observed in the 15N NMR spectra of the nitro isomer. The NMR parameters are rationalized based on differences in the molecular structure of the two isomers. NMR spectra have also been recorded as the isomerization progresses with time and demonstrate the practicality of the technique for the study of solid-state isomerizations.Key words: 15N, 59Co, solid-state NMR, linkage isomerization, chemical shift tensor, electric field gradient tensor.

A solid-state 31P NMR study of 1:1 silver–triphenylphosphine complexes — Interpretation of 1J(107,109Ag,31P) values,

2009 ◽  
Vol 87 (7) ◽  
pp. 1090-1101 ◽  
Author(s):  
Fu Chen ◽  
Se-Woung Oh ◽  
Roderick E. Wasylishen
Keyword(s):  
Solid State ◽  
Spin Coupling ◽  
Coupling Mechanism ◽  
P Values ◽  
X Ray Crystallography ◽  
Phosphine Complexes ◽  
Nmr Study ◽  
Fermi Contact ◽  
Spin Spin Coupling ◽  
Cp Mas Nmr

High-resolution solid-state 31P NMR spectroscopy was used to investigate a series of 1:1 silver–triphenylphosphine complexes, [Ph3PAgX]n, where X is a monovalent anion and n = 1, 2, 3, 4, or ∞. The 31P CP MAS NMR spectra reveal the number of distinct phosphorus sites in these complexes as well as the |1J(109Ag,31P)| values, which range from 401 ± 10 Hz (X = N3–) to 869 ± 10 Hz (X = SO3CF3–). The data obtained here and in earlier investigations indicate that |1J(109Ag,31P)| values for silver–tertiary phosphine complexes decrease as Ag–P bond lengths increase. This experimental conclusion is supported by DFT calculations, which also indicate that the Fermi-contact mechanism is the only important spin–spin coupling mechanism for 1J(109Ag,31P) in these complexes. In addition, the crystal structure of a silver–triphenylphosphine trifluoroacetate tetramer was determined using X-ray crystallography, and the structure of a silver–triphenylphosphine chloride tetramer was reinvestigated.

scholarly journals Spying on the boron–boron triple bond using spin–spin coupling measured from 11B solid-state NMR spectroscopy

2015 ◽  
Vol 6 (6) ◽  
pp. 3378-3382 ◽  
Author(s):  
Frédéric A. Perras ◽  
William C. Ewing ◽  
Theresa Dellermann ◽  
Julian Böhnke ◽  
Stefan Ullrich ◽  
...  
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Solid State Nmr ◽  
Triple Bond ◽  
Coupling Constants ◽  
Spin Coupling ◽  
Solid State Nmr Spectroscopy ◽  
Spin Spin Coupling ◽  
Insight Into

Boron–boron J coupling constants provide new insight into the nature of the boron–boron triple bond.

scholarly journals Solid-State NMR Studies of the Succinate-Acetate Permease from Citrobacter Koseri in Liposomes and Native Nanodiscs

Life ◽  
2021 ◽  
Vol 11 (9) ◽  
pp. 908
Author(s):  
Xing-Qi Dong ◽  
Jing-Yu Lin ◽  
Peng-Fei Wang ◽  
Yi Li ◽  
Jian Wang ◽  
...  
Keyword(s):  
Solid State ◽  
Chemical Shift ◽  
Solid State Nmr ◽  
Protein Structures ◽  
Anion Channel ◽  
Transmembrane Domains ◽  
Helical Structures ◽  
Nmr Studies ◽  
Two Samples ◽  
Lipid Environment

The succinate-acetate permease (SatP) is an anion channel with six transmembrane domains. It forms different oligomers, especially hexamers in the detergent as well as in the membrane. Solid-state NMR studies of SatP were carried out successfully on SatP complexes by reconstructing the protein into liposomes or retaining the protein in the native membrane of E. Coli., where it was expressed. The comparison of 13C-13C 2D correlation spectra between the two samples showed great similarity, opening the possibility to further study the acetate transport mechanism of SatP in its native membrane environment. Solid-state NMR studies also revealed small chemical shift differences of SatP in the two different membrane systems, indicating the importance of the lipid environment in determining the membrane protein structures and dynamics. Combining different 2D SSNMR spectra, chemical shift assignments were made on some sites, consistent with the helical structures in the transmembrane domains. In the end, we pointed out the limitation in the sensitivity for membrane proteins with such a size, and also indicated possible ways to overcome it.

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