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Nitrogen-15 NMR
Nitrogen-15 nuclear magnetic resonance spectroscopy (nitrogen-15 NMR spectroscopy, or just simply 15N NMR) is a version of nuclear magnetic resonance spectroscopy that examines samples containing the 15N nucleus.Witanowski, M (1974). “Nitrogen N.M.R. Spectroscopy”. Pure and Applied Chemistry. 37, pp. 225-233. 15N NMR differs in several ways from the more common 13C and 1H NMR. To circumvent the difficulties associated with measurement of the quadrupolar, spin-1 14N nuclide, 15N NMR is employed in samples for detection since it has a ground-state spin of ½. Since14N is 99.64% abundant, incorporation of 15N into samples often requires novel synthetic techniques. Nitrogen-15 is frequently used in nuclear magnetic resonance spectroscopy (NMR), because unlike the more abundant nitrogen-14, that has an integer nuclear spin and thus a quadrupole moment, 15N has a fractional nuclear spin of one-half, which offers advantages for NMR like narrower line width. Proteins can be isotopical ...
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Nuclear Magnetic Resonance Spectroscopy
Nuclear magnetic resonance spectroscopy, most commonly known as NMR spectroscopy or magnetic resonance spectroscopy (MRS), is a spectroscopic technique to observe local magnetic fields around atomic nuclei. The sample is placed in a magnetic field and the NMR signal is produced by excitation of the nuclei sample with radio waves into nuclear magnetic resonance, which is detected with sensitive radio receivers. The intramolecular magnetic field around an atom in a molecule changes the resonance frequency, thus giving access to details of the electronic structure of a molecule and its individual functional groups. As the fields are unique or highly characteristic to individual compounds, in modern organic chemistry practice, NMR spectroscopy is the definitive method to identify monomolecular organic compounds. The principle of NMR usually involves three sequential steps: # The alignment (polarization) of the magnetic nuclear spins in an applied, constant magnetic field B0. # The ...
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Backbone Walk For NCACX, NCOCX, And CANcoCX For SS-NMR
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Two-dimensional Nuclear Magnetic Resonance Spectroscopy
Two-dimensional nuclear magnetic resonance spectroscopy (2D NMR) is a set of nuclear magnetic resonance spectroscopy (NMR) methods which give data plotted in a space defined by two frequency axes rather than one. Types of 2D NMR include correlation spectroscopy (COSY), J-spectroscopy, exchange spectroscopy (EXSY), and nuclear Overhauser effect spectroscopy (NOESY). Two-dimensional NMR spectra provide more information about a molecule than one-dimensional NMR spectra and are especially useful in determining the structure of a molecule, particularly for molecules that are too complicated to work with using one-dimensional NMR. The first two-dimensional experiment, COSY, was proposed by Jean Jeener, a professor at the Université Libre de Bruxelles, in 1971. This experiment was later implemented by Walter P. Aue, Enrico Bartholdi and Richard R. Ernst, who published their work in 1976. Fundamental concepts Each experiment consists of a sequence of radio frequency (RF) pulses with d ...
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Heteronuclear Single Quantum Coherence Spectroscopy
The heteronuclear single quantum coherence or heteronuclear single quantum correlation experiment, normally abbreviated as HSQC, is used frequently in NMR spectroscopy of organic molecules and is of particular significance in the field of protein NMR. The experiment was first described by Geoffrey Bodenhausen and D. J. Ruben in 1980. The resulting spectrum is two-dimensional (2D) with one axis for proton (1H) and the other for a heteronucleus (an atomic nucleus other than a proton), which is usually 13C or 15N. The spectrum contains a peak for each unique proton attached to the heteronucleus being considered. The 2D HSQC can also be combined with other experiments in higher-dimensional NMR experiments, such as NOESY-HSQC or TOCSY-HSQC. General scheme The HSQC experiment is a highly sensitive 2D-NMR experiment and was first described in a 1H—15N system, but is also applicable to other nuclei such as 1H—13C and 1H—31P. The basic scheme of this experiment involves the tra ...
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Nuclear Overhauser Effect
The nuclear Overhauser effect (NOE) is the transfer of nuclear spin polarization from one population of spin-active nuclei (e.g. 1H, 13C, 15N etc.) to another via cross-relaxation. A phenomenological definition of the NOE in nuclear magnetic resonance spectroscopy (NMR) is the change in the integrated intensity (positive or negative) of one NMR resonance that occurs when another is saturated by irradiation with an RF field. The change in resonance intensity of a nucleus is a consequence of the nucleus being close in space to those directly affected by the RF perturbation. The NOE is particularly important in the assignment of NMR resonances, and the elucidation and confirmation of the structures or configurations of organic and biological molecules. The 1H two-dimensional NOE SpectroscopY (NOESY) experiment and its extensions are important tools to identify stereochemistry of proteins and other biomolecules in solution, whereas in solid form crystal x-ray diffraction typicall ...
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Insensitive Nuclei Enhanced By Polarization Transfer
Insensitive nuclei enhancement by polarization transfer (INEPT) is a signal enhancement method used in NMR spectroscopy. It involves the transfer of nuclear spin polarization from spins with large Boltzmann population differences to nuclear spins of interest with lower Boltzmann population differences. INEPT uses J-coupling for the polarization transfer in contrast to Nuclear Overhauser effect (NOE), which arises from dipolar cross- relaxation. This method of signal enhancement was introduced by Ray Freeman in 1979. Due to its usefulness in signal enhancement, pulse sequences used in heteronuclear NMR experiments often contain blocks of INEPT or INEPT-like sequences. Background The sensitivity of NMR signal detection depends on the gyromagnetic ratio (γ) of the nucleus. In general, the signal intensity produced from a nucleus with a gyromagnetic ratio of γ is proportional to γ3 because the magnetic moment, the Boltzmann populations, and the nuclear precession frequency all inc ...
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INEPT Pulse Sequence
Insensitive nuclei enhancement by polarization transfer (INEPT) is a signal enhancement method used in NMR spectroscopy. It involves the transfer of nuclear spin polarization from spins with large Boltzmann population differences to nuclear spins of interest with lower Boltzmann population differences. INEPT uses J-coupling for the polarization transfer in contrast to Nuclear Overhauser effect (NOE), which arises from dipolar cross- relaxation. This method of signal enhancement was introduced by Ray Freeman in 1979. Due to its usefulness in signal enhancement, pulse sequences used in heteronuclear NMR experiments often contain blocks of INEPT or INEPT-like sequences. Background The sensitivity of NMR signal detection depends on the gyromagnetic ratio (γ) of the nucleus. In general, the signal intensity produced from a nucleus with a gyromagnetic ratio of γ is proportional to γ3 because the magnetic moment, the Boltzmann populations, and the nuclear precession frequency all incr ...
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Solid-state Nuclear Magnetic Resonance
Solid-state NMR (ssNMR) spectroscopy is a technique for characterizing atomic level structure in solid materials e.g. powders, single crystals and amorphous samples and tissues using nuclear magnetic resonance (NMR) spectroscopy. The anisotropic part of many spin interactions are present in solid-state NMR, unlike in solution-state NMR where rapid tumbling motion averages out many of the spin interactions. As a result, solid-state NMR spectra are characterised by larger linewidths than in solution state NMR, which can be utilized to give quantitative information on the molecular structure, conformation and dynamics of the material. Solid-state NMR is often combined with magic angle spinning to remove anisotropic interactions and improve the resolution as well as the sensitivity of the technique. Nuclear spin interactions The resonance frequency of a nuclear spin depends on the strength of the magnetic field at the nucleus, which can be modified by isotropic (e.g. chemical shift, i ...
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Tautomerization And 15N-NMR
Tautomers () are structural isomers (constitutional isomers) of chemical compounds that readily interconvert. The chemical reaction interconverting the two is called tautomerization. This conversion commonly results from the relocation of a hydrogen atom within the compound. The phenomenon of tautomerization is called tautomerism, also called desmotropism. Tautomerism is for example relevant to the behavior of amino acids and nucleic acids, two of the fundamental building blocks of life. Care should be taken not to confuse tautomers with depictions of "contributing structures" in chemical Resonance (chemistry), resonance. Tautomers are distinct chemical species that can be distinguished by their differing atomic connectivities, molecular geometries, and physicochemical and spectroscopic properties, whereas resonance forms are merely alternative Lewis structure (valence bond theory) depictions of a single chemical species, whose true structure is best described as the "average" of ...
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Nuclear Spin
In atomic physics, the spin quantum number is a quantum number (designated ) which describes the intrinsic angular momentum (or spin angular momentum, or simply spin) of an electron or other particle. The phrase was originally used to describe the fourth of a set of quantum numbers (the principal quantum number , the azimuthal quantum number , the magnetic quantum number , and the spin quantum number ), which completely describe the quantum state of an electron in an atom. The name comes from a physical spinning of the electron about an axis, as proposed by Uhlenbeck and Goudsmit. The value of is the component of spin angular momentum parallel to a given direction (the –axis), which can be either +1/2 or –1/2 (in units of the reduced Planck constant). However this simplistic picture was quickly realized to be physically impossible because it would require the electrons to rotate faster than the speed of light. It was therefore replaced by a more abstract quantum-mechanical ...
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Gyromagnetic Nuclei Precession
A magneto-optic effect is any one of a number of phenomena in which an electromagnetic wave propagates through a medium that has been altered by the presence of a quasistatic magnetic field. In such a medium, which is also called gyrotropic or gyromagnetic, left- and right-rotating elliptical polarizations can propagate at different speeds, leading to a number of important phenomena. When light is transmitted through a layer of magneto-optic material, the result is called the Faraday effect: the plane of polarization can be rotated, forming a Faraday rotator. The results of reflection from a magneto-optic material are known as the magneto-optic Kerr effect (not to be confused with the nonlinear Kerr effect). In general, magneto-optic effects break time reversal symmetry locally (i.e. when only the propagation of light, and not the source of the magnetic field, is considered) as well as Lorentz reciprocity, which is a necessary condition to construct devices such as optical ...
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International Union Of Pure And Applied Chemistry
The International Union of Pure and Applied Chemistry (IUPAC ) is an international federation of National Adhering Organizations working for the advancement of the chemical sciences, especially by developing nomenclature and terminology. It is a member of the International Science Council (ISC). IUPAC is registered in Zürich, Switzerland, and the administrative office, known as the "IUPAC Secretariat", is in Research Triangle Park, North Carolina, United States. This administrative office is headed by IUPAC's executive director, currently Lynn Soby. IUPAC was established in 1919 as the successor of the International Congress of Applied Chemistry for the advancement of chemistry. Its members, the National Adhering Organizations, can be national chemistry societies, national academies of sciences, or other bodies representing chemists. There are fifty-four National Adhering Organizations and three Associate National Adhering Organizations. IUPAC's Inter-divisional Committee on ...
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