Search results for "magnetic resonance spectroscopy"
showing 10 items of 1362 documents
Chemical Reaction Monitoring Using Zero-Field Nuclear Magnetic Resonance Enables Study of Heterogeneous Samples in Metal Containers
2020
Abstract We demonstrate that heterogeneous/biphasic chemical reactions can be monitored with high spectroscopic resolution using zero‐field nuclear magnetic resonance spectroscopy. This is possible because magnetic susceptibility broadening is negligible at ultralow magnetic fields. We show the two‐step hydrogenation of dimethyl acetylenedicarboxylate with para‐enriched hydrogen gas in conventional glass NMR tubes, as well as in a titanium tube. The low frequency zero‐field NMR signals ensure that there is no significant signal attenuation arising from shielding by the electrically conductive sample container. This method paves the way for in situ monitoring of reactions in complex heteroge…
Di-n-octyltin(IV) complexes with 5-[(E)-2-(aryl)-1-diazenyl]-2-hydroxybenzoic acid: Syntheses and assessment of solid state structures by 119Sn Mössb…
2007
Abstract Reactions of 5-[( E )-2-(aryl)-1-diazenyl]-2-hydroxybenzoic acids (LHH′, where the aryl group is an R-substituted phenyl ring such that for L 1 HH′: X = H; L 2 HH′: X=2′-OCH 3 ; L 3 HH′: X = 3′-CH 3 ; L 4 HH′: X = 4′-CH 3 ; L 5 HH′:X = 4′-Cl) with n Oct 2 SnO in 2:1 and 1:1 molar ratios have been investigated. Two types of complexes, n Oct 2 Sn(LH) 2 and {[ n Oct 2 Sn(LH)] 2 O} 2 , were isolated and they have been characterized by 1 H, 13 C, 119 Sn NMR, ESI-MS, IR and 119m Sn Mossbauer spectroscopic techniques in combination with elemental analyses. The crystal structures of n Oct 2 Sn(L 1 H) 2 ( 1 ), {[ n Oct 2 Sn(L 2 H)] 2 O} 2 ( 3 ) and {[ n Oct 2 Sn(L 3 H)] 2 O} 2 ( 4 ) were de…
13C-Decoupled J-Coupling Spectroscopy Using Two-Dimensional Nuclear Magnetic Resonance at Zero-Field
2017
We present a two-dimensional method for obtaining 13C-decoupled, 1H-coupled nuclear magnetic resonance (NMR) spectra in zero magnetic field using coherent spin-decoupling. The result is a spectrum determined only by the proton–proton J-coupling network. Detection of NMR signals in zero magnetic field requires at least two different nuclear spin species, but the proton J-spectrum is independent of isotopomer, thus potentially simplifying spectra and thereby improving the analytical capabilities of zero-field NMR. The protocol does not rely on a difference in Larmor frequency between the coupled nuclei, allowing for the direct determination of J-coupling constants between chemically equivalen…
1H, 13C NMR spectral and single crystal structural studies of toxaphene congeners. Quantum chemical calculations for preferred conformers of 2,5-endo…
2005
Abstract The 1H and 13C NMR chemical shifts for six toxaphene congeners: 2-exo,3-endo,6-exo,8,9,10-hexachloro- (1), 2-exo,3-endo,5-exo,9,9,10,10-heptachloro- (2), 2-exo,3-endo,6-exo,8,9,10,10-heptachloro- (3), 2-exo,3-endo,5-exo,6-endo,8,9,10-heptachloro- (4), 2-exo,3-endo,5-exo,6-endo,8,9,9,10-octachlorobornane (5) and 2,5-endo,6-exo,8,9,9,10,10-octachloro-2-bornene (6) are reported. Their chemical shift assignments have been obtained by means of Pulsed Field Gradient (PFG) Double Quantum Filtered (DQF) 1H,1H correlation spectroscopy (COSY), PFG 1H,13C Heteronuclear Multiple Quantum Coherence (HMQC) and PFG 1H,13C Heteronuclear Multiple Bond Correlation (HMBC) experiments. A single crystal…
Comparative multinuclear magnetic resonance spectroscopic study of transition metal (Cr, W and Mn) mesitylene tricarbonyls and transition metal (Ru a…
1993
Abstract Three mononuclear 1,3,5-trimethylbenzene (mesitylene) carbonyl transition metal complexes, mesitylene tricarbonyl chromium, (CH 3 ) 3 C 6 H 3 Cr(CO) 3 ( 1 ), mesitylene tricarbonyl tungsten, (CH 3 ) 3 C 6 H 3 W(CO) 3 ( 2 ), mesitylene tricarbonyl manganese tetra-fluoroborate, [(CH 3 ) 3 C 6 H 3 Mn(CO) 3 ]BF 4 ( 3 ); and three clusters, mesitylene nonacarbonyl tetracobalt, (CH 3 ) 3 C 6 H 3 Co 4 (CO) 9 ( 4 ), mesitylene carbido tetradecacarbonyl hexaruthenium, (CH 3 ) 3 C 6 H 3 Ru 6 C(CO) 14 ( 5 ) and carbido heptadecacarbonyl hexaruthenium, Ru 6 C(CO) 17 ( 6 ), have been studied by means of 1 H, 13 C and natural abundance 17 O NMR spectroscopy. Generally, the 1 H and 13 C NMR chemi…
17O NMR study of chlorinated anisoles
1988
The 17O NMR chemical shifts of anisole and all 19 chlorinated anisoles measured in CDCI3 at ambient temperature show a dispersion of approximately 40 ppm. The substituent chemical shifts (SCS) of di- or more highly chlorinated compounds cannot be reproduced by addition of single substituent effects. Theoretical calculations of the 17O NMR chemical shifts have been attempted by molecular mechanical and semi-empirical molecular orbital methods at the INDO level, but the results are not satisfactory.
NMR spectroscopy in environmental chemistry:1H and13C NMR parameters of tricyclic polychlorinated C10 hydrocarbons and their oxy derivatives based on…
1999
Two-dimensional homo- and heteronuclear NMR chemical shift correlation techniques were applied in the characterization of five tricyclic polychlorinated C10 hydrocarbons, chlordene (1), heptachlor (2), trans-nonachlor (3), α-chlordene (4) and γ-chlordene (5), which are spread globally in the environment owing to their use as insecticides. Approximate and partly contradictory 1H and 13C NMR chemical shifts reported in the literature were corrected in this work. The chemical shift assignments of 1–5 were based on DQF COSY, HMQC and HMBC experiments. In addition, an INADEQUATE experiment was needed to ascertain the 13C chemical shifts assignment of 2. The nJ(H,H)s of 1–5 were solved by compute…
Synthesis and 1H-NMR configurational study of δ3-thiazolines from 2-aza-1,3-dienes
1992
Abstract A [4+1] heterocyclization process involving 2-aza-1,3-dienes and elemental sulphur leading to the synthesis of Δ3-thiazolines with excellent yields is described. A 1D TOCSY and 1D NOESY study of these systems was made in order to establish the configurations of the diastereoisomeric mixture.
Preparation and Photochemistry of Dendrimers with Isolated Stilbene Chromophores
2005
In addition to the model compounds 4a and 4b, the dendrimers 11 and 14 with trans-stilbene chromophores in the core and on the periphery of the dendrons were prepared and their photochemistry was studied in solution and in neat films. Due to the flexibility of the arms, intramolecular and intermolecular CC bonds are formed on irradiation. Thus, the generation of nanoparticles, which represent small oligomers, is much more likely than for the cross-linking of rigid, cross-conjugated stilbenoid dendrimers. The photoreactions in solution were studied by UV and NMR spectroscopy, the transformation of the films was studied by AFM. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 200…
Yttrium Hydrido Complexes that Contain a Less “Constrained Geometry” Ligand: Synthesis, Structure, and Efficient Hydrosilylation Catalysis
2001
σ-Bond metathesis of the new linked amino-cyclopentadiene (C5Me4H)CH2SiMe2NHCMe3 with Y(CH2SiMe3)3(THF)2 gave the alkyl-yttrium complex [Y(η5:η1-C5Me4CH2SiMe2NCMe3)(CH2SiMe3)(THF)] (1) in 66% yield. Compound 1 was characterized by NMR spectroscopy and X-ray crystal structure analysis. By hydrogenolysis, 1 was quantitatively converted into the dimeric hydride [Y(η5:η1-C5Me4CH2SiMe2NCMe3)(THF)(μ-H)]2 (2). X-ray crystal structure analysis revealed a Y2H2 core connected to two [Y(η5:η1-C5Me4CH2SiMe2NCMe3)(THF)] fragments in a skewed manner, with a relatively long yttrium−yttrium distance of 3.7085(8) A. In solution, two diastereomers were observed by 1H NMR spectroscopy at −78 °C. Dimer 2 was s…