Proton-proton Coupling Constant

Proton-proton Coupling Constant Easily recognized splitting patterns found in various spectra provide the chemical shifts of the different sets of hydrogen that generate the signals differ by two or more ppm. The patterns are symmetrically distributed on both sides of the proton chemical shift, and the central lines are always stronger than the outer lines. The most commonly observed patterns have been given descriptive names, such as doublet (two equal intensity signals), triplet (three signals with an intensity ratio of 1:2:1) and quartet (a set of four signals with intensities of 1:3:3:1). The line separation is always constant within a given multiplet, and is called the coupling constant (J). The magnitude of J, usually given in units of Hz, is magnetic field independent. Coupling constants play an immense role in configurational and conformational studies. The relative position of protons is determining factor for Vicinal coupling constant between two protons. For example, in 1,2-disubstituted ethenes, the lar ger vicinal coupling constant was observed between the olefinic protons for the trans isomer 82a than for the cis isomer 82b [127,134]. The vicinal coupling constant depends on the dihedral angle between the protons in saturated systems. Karplus [118] gave equations 1 and 2 relating the coupling constant with dihedral angles. J1 = k1cos2à ¯Ã‚ Ã‚ ¦ c (0 à ¯Ã¢â‚¬Å¡Ã‚ £ à ¯Ã‚ Ã‚ ¦ à ¯Ã¢â‚¬Å¡Ã‚ £ 90 °) †¦ (1) J2 = k2cos2à ¯Ã‚ Ã‚ ¦ c (0 à ¯Ã¢â‚¬Å¡Ã‚ £ à ¯Ã‚ Ã‚ ¦ à ¯Ã¢â‚¬Å¡Ã‚ £ 180 °)†¦ (2) These equations were later modified as equation 3. J2 = A cos2à ¯Ã‚ Ã‚ ¦ B cos2à ¯Ã‚ Ã‚ ¦ + C †¦ (3) In equation 3, J is the coupling constant and A, B and C are constants related to the electro-negativities of the substituents attached to the C-C segment. The J value decreases markedly with increase in the electronegativities of the substituents [135-140]. 13C-NMR: Transitions of only 13C nuclei are noticed in 13C-NMR spectroscopy. Figure 3 represents different ÃŽ ´ values (in ppm), couplings, coupling constants (in Hz) and chemical shifts of 13C nuclei processing in different chemical environments. Usually, ÃŽ ´ value scale of 13C-NMR ranges from 0-220 ppm with respect to TMS as internal standard. 13C-NMR spectral interpretation can be best understood from chart given in figure 3 [126,127]. 13C Chemical shift As in the same ways of proton NMR spectrum, Chemical Shift in 13C NMR spectrum provides the hybridization (sp3, sp2, sp) of each carbon nucleus due to shielding and deshielding effects. Each carbon nucleus has its own electronic environment, different from the environment of other, non-equivalent nuclei. Figure 3: Chart representing 13C nuclei chemical shift due to different chemical environments. Electronegative atoms and pi bonds cause downfield shifts (â€Å"Thinkbook†). Spin-spin coupling provides the number of protons attached to the 13C nuclei. (i.e., primary, secondary tertiary or quaternary carbon) [126,127]. Carbon (13C) has a much broader chemical shift range. One important difference is that the aromatic and alkene regions overlap to a significant extent [126,127].Many factors such as inductive effects of substituent, hybridization state of the observed nucleus, Van der Wall’s and steric effects between closely spaced nuclei, electric fields originating from molecular dipoles or point charges, hyperconjugation, mesomeric interactions in à ¯Ã‚ Ã‚ ° electron systems (delocalization effects), diamagnetic shielding due to heavy substituents (heavy-atom effect) and anisotropy effects is known to influence the 13C Chemical shift of six-membered ring compounds. Among those factor, electrostatic effects due to the presence of a heteroatom in the cyclohexane moiety and steric perturbation effects being intrinsic importance. Lambert et al. [141] documented the effect of heteroatom in monoheterocyclohexanes 83 on the shifts of ring carbons. The à ¯Ã‚ Ã‚ ¡-shift is a steep function of electronegativity of heteroatom X. A high frequency shift of about 50 ppm is produced by an increase in one unit electronegativity. However, a small effects of heteroatom electronegativity on à ¯Ã‚ Ã‚ ¢ and à ¯Ã‚ Ã‚ §-carbons are produced, a shift of -2.5 ppm/electronegativity unit for à ¯Ã‚ Ã‚ ¢ and -5.0 ppm/electronegativity unit for à ¯Ã‚ Ã‚ §-carbon, respectively. Ramalingam et al have demonstrated the effect of introduction of heteroatom in 84a-84e [86]. The decreasing order of the deshielding effect of heteroatom on the benzylic carbon is O > NMe > NH > S. because of a field effect, the heteroatom generates a low frequency an upfield shift in the ca rbonyl resonance. Contrary to à ¯Ã‚ Ã‚ ¡ and à ¯Ã‚ Ã‚ ¢ effects, the à ¯Ã‚ Ã‚ §-effect is being a property of at least four atoms and it has a torsional component. All ÃŽ ³ anti substituents cause increased shielding on C-5 due to the presence of ÃŽ ± and ÃŽ ³ protons. The ÃŽ ³ anti effect C-3 is found to be rather deshielding. The resonating carbon and perturbing à ¯Ã‚ Ã‚ § substituent showed the dihedral angle arrangement ranging from 0-180 °. à ¯Ã‚ Ã‚ §-gauche effects is found to be almost independent of the nature of the perturbing group X and generally occur in the 60-80 ° regions, whereas à ¯Ã‚ Ã‚ §-anti effect in the 150-180 ° regions. The introduction of an axial substituent shifts the resonance of a à ¯Ã‚ Ã‚ §-carbon to lower frequencies. The à ¯Ã‚ Ã‚ §-anti effect (introduction of an equatorial substituent) is small. Interpretation of the substituent effects mainly depends on the steric and polar effects [142-144]. Based on the 13C NMR spectrum of vinylcyclohexane at low temperature, Buchanan observed the low frequency shifts in 85a relative to the equatorial counterpart 85b [145]. Based on the 13C NMR spectrum of various di-and tri-methylcyclohexanes, Dalling and Grant [146] observed an axial methyl group shifts the resonance of C(2), C(3) and C(4) at 1.40, 5.41 and 6.37 ppm and the corresponding resonance shifts for an equatorial methyl group at 5.96, 9.03 and 0.05 ppm, respectively. The shielding by an axial methyl group relative to an equatorial methyl group has been ascribed to steric interactions [142]. Furthermore, The 13C NMR data of 4 hydroxypiperidines results indicate that substituent effects are markedly influenced by steric interaction. Eliel et al. [147] study on à ¯Ã‚ Ã‚ §-effect of heteroatoms in heteracyclohexanes 86a-86d provide evidence that the à ¯Ã‚ Ã‚ §-carbon located anti to a second-row heteroatom (X=O; NH) resonates at significantly lower frequency than the analogo us carbon anti to a methylene group or a third-row heteroatom. Pandiarajan et al. [13] suggested a method of assigning the configuration of a sub ­stituent in saturated six–membered ring compounds, existing in chair conformation, from 13C chemical shift of a single epimer. Furthermore, the influence of the nearby substituents on the substituent parameters of equatorial methyl, gem-dimethyl, and equatorial and axial hydroxyl groups in several six-membered ring compounds 87a-87g has been suggested by Pandiarajan et al [13]. The magnitude of the à ¯Ã‚ Ã‚ ¡ effect of a particular substituent is significantly reduced by a nearby substituent and the magnitude of the à ¯Ã‚ Ã‚ ¡ effect decreases as the number of gauche interactions increases. Though, the à ¯Ã‚ Ã‚ ¢ and à ¯Ã‚ Ã‚ § effects are not influenced by the nearby substituents [13]. Nuclear Overhauser effect (nOe) The change in intensity of one NMR resonance that occurs when another is saturated is known as the nuclear Overhauser effect (NOE). NOE arises from dipole–dipole cross-relaxation between nuclei, and its usefulness. The strength of a given NOE enhancement is approximately correlated with internuclear separation (actually r−6 where r is the internuclear distance). However, the NOE also depends on other factors such as molecular motions [148]. In small molecules in solution, the NOE is positive and causes affected resonances to increase in intensity. NOE for small molecules is generally measured using one-dimensional experiments. In small molecules, NOE determins particular stereochemical relationships, such as substitution or ring fusion patterns in largely rigid systems. The NOE is negative for larger molecules and cause affected resonances decrease in intensity. NOE for larger molecules is usually measured using the two-dimensional NOESY experiment or one of its multidimensional variants. Using the NOE to Development of three-dimensional structural information using NOE generally depends on interpretation of an overlapping, redundant network of enhancements, rather than on calibrating precisely the distance dependence of individual enhancements. NOE determine accurate three-dimensional solution structures of biomacromoleculs such as DNA, RNA, or other proteins [149]. A spin-excited nucleus is known to transfer its spin energy to that of an adjacent nucleus resulting in spin relaxation. The efficiency of energy transfer is directly related to the distance between the two nuclei. The nOe grosses advantage of the spin energy transfer [149]. The nOe decreases as the inverse of the sixth power of the distance between the protons. An interesting application of nOe to a structural problem has been described by Hunter et al. [150] When styrene is polymerized in the presence of 4-methoxyphenol, in addition to the polymer, a 1:1 adduct is obtained by the addition of a styrene molecule to 4-methoxyphenol. However, the question of whether the addition occurs at C-2 or C-3 could not be answered from either the 1H or 13C NMR spectrum. The nOe experiment provided a decision in favour of structure 88. Irradiating the OCH3 resonance gave an increase in the intensities of the signals of the ring protons HA and HB. From this it is obvious that both these protons are ortho to the OCH3 group. In contrast the signal of the third ring proton HC showed a negative nOe. This is a case of an indirect nOe in a multi spin system. In further, nOe experiment it was shown that saturating the OH resonance increased the intensity of the HC signal, providing additional evidence for structure 88. TWO-DIMENSIONAL NMR SPECTROSCOPY COSY, a homonuclear 2D NMR correlation spectroscopy, correlates chemical shift of two hydrogen nuclei located on two different carbons that are separated by a single bond via j coupling. Thus it detects the chemical shift for hydrogen’s on both F1 and F2 axis. The most important two-dimensional NMR spectra show either 1h vs 1h or 1h vs 13c chemical shift correlations [126,127]. Here, we attempt to discuss about the some of the important types of 2-D experiments. Principle In 2D-NMR, the structural information are obtained from the interactions between two nuclei, either through the bonds which connect them (J-coupling interaction) or directly through space (NOE interaction). These interactions occur at a time by irradiating one resonance in the proton spectrum (either during the relaxation delay or during acquisition) and provide the effect on the intensity or coupling pattern of another resonance. 2D NMR essentially allows us to irradiate all of the chemical shifts in one experiment and gives us a matrix or two-dimensional map of all of the affected nuclei. All possible pairs of nuclei in the sample processed at the same time [128,129]. The basic steps in 2D experiment are as follows. 1. Preparation: Excite nucleus A, creating magnetization in the x-y plane 2. Evolution: Measure the chemical shift of nucleus A. 3. Mixing: Transfer magnetization from nucleus A to nucleus B (via J or NOE). 4. Detection: Measure the chemical shift of nucleus B. Preparation and Evolution: A 90o pulse excites all of the sample nuclei simultaneously. Detection is simply recording an FID and finding the frequency of nucleus B by Fourier transformation. To get a second dimension, we have to measure the chemical shift of nucleus A before it passes its magnetization to nucleus B. This is accomplished by simply waiting a period of time (called t1, the evolution period) and letting the nucleus A magnetization rotate in the x-y plane. The experiment is repeated many times over (for example, 512 times), recording the FID each time with the delay time t1 incremented by a fixed amount. The time course of the nucleus A magnetization as a function of t1 (determined by its effect on the final FID) is used to define how fast it rotates and thus its chemical shift. Mixing is a combination of RF pulses and/or delay periods which induce the magnetization to jump from A to B as a result of either a J coupling or an NOE interaction (close proximity in space). Di fferent 2D experiments (e.g., NOESY, COSY, HETCOR, etc.) differ primarily in the mixing sequence, since in each one we are trying to define the relationship between A and B within the molecule in a different way [128,129].

Recording, Analysing & Using HR Information Essay

This document will review the organisation’s approach to collecting, storing and using HR data. It will cover why the organisation needs to collect HR data, the different types of data that is collected and how it is beneficial to HR, different storing methods and their benefit and UK legislation relating to the recording, storage and access to HR data. HR data contains highly sensitive information such as salary, pension information, grievances, and basic personnel information (name, address, and telephone details). A fine can be enforced up to ? 500. 000 in an organisation is found to have breached data protection. Data Management: There are many different reasons why an organisation needs to collect HR data from ensuring legal requirements are meet, to provide relevant information in decision making and planning, health and safety, protection from claims, working time directive. If used correctly it can serve as a very useful management tool. Holding recruitment new starter paperwork that contains a national insurance number and passport picture is essential to proving someone is eligible to work in the UK, without proof of eligibility the organisation can face a fine. Inductions record when an employee has been through the necessary requirements to do their role such as a health and safety course, and manual handling. This can protect the organisation if a claim was to rise with regards to injury or illness. If an employee raises a grievance as they have reached an unacceptable level of sickness. We can use the data held on our systems with regard to absences to prove when they have been in work and for how long, if we keep meeting notes we can also prove how we evaluated the situation and the action that was taken which can be used if it went to a tribunal, or if HR was looking at process management. The Inland Revenue can request data at any point from mileage, expenses, salary, national insurance, therefore it is essential we keep records such as P60, payslips, expense reports so this data can be crossed checked and proof that we have paid an employee correctly. Data Storage: From the moment an application is received to the moment an employee receives their P45 an organisation holds data. We call this the ‘Life Cycle of and Employee. ’ There are two methods in which we store data: Manual Records: This can be filing cabinets and folders held within storage cupboards. His is kept mainly as a backup should electronic systems fail or where original documents must be retained as a legal requirement such as a maternity MATB1 form. The benefits of this are the data is easily accessible and will not be prone to any electrical power failures or computerised scams which corrupt data. However there is the risk of keys being lost or data being seen by unauthorised personnel if it is not put away correctly. To prevent such occurrence a clear desk policy could be implemented. Systems: This can be excel spreadsheets that hold reports and link to other systems such as SAP, which is where we hold employee information such as address, salary, pension, hours worked, absences. The benefits of this method means you do not have to search numerous files as the data is held in one place, which is useful if an employee data request is received. As a sustainable organisation it benefits the environment as we don’t use paper. Documents are easily maintained and can be moved to different servers or USB devices for storage.

Depth Analysis of the Movie Crash - 2037 Words

Abstract This paper will provide a broad analysis of the movie Crash, and yet a specific picture of visual narrative techniques and audio techniques. The categories contributing to the nucleus and major movie components are theatrical elements, cinematography, editing, and sound. The Academy Award winning movie Crash is a story about society s controversial subjects projected in an in your face depiction of lives that in some way or another, cross. Depth Analysis of the Movie Crash The over-all theme of the film is racism, which is dealt with honestly, brutally, and without justification. This 2006 release from Emmy award-winning writer/producer Paul Haggis is focused around two unsettling car accidents, a disturbing†¦show more content†¦The cast is one of the finest and consists of Sandra Bullock, Don Cheadle, Matt Dillon, Jennifer Esposito, William Fichtner, Brendan Fraser, Terrence Howard, Chris Ludacris Bridges, Thandie Newton, Ryan Phillippe, Larenz Tate, and Michael Pena. In general, actors act, and react. They act on their own, and they react to one another. After Don Cheadle s monologue in the beginning of the film, it is clear that this film is going to be a deep seated story. Films create movement out of images, time out of movement, and story from the action. The writer/director Paul Haggis has a background in television, and television has multiple stories all interweaving together. His knowledge from television helped in the editing process. In Crash, Paul Haggis had several transitions in the story lines. He compressed some scenes because if too long, the audience would lose interest in the other stories. The cinematography in the movie adds a tremendous amount of experience to the film. The film follows the lives of several characters that come from different walks of life. It is important for the mood setting of the plot to use different techniques to help the viewer assume the role of witness. 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The Characters Of Virgil And Homers The Aeneid - 973 Words

The Roman Empire is considered the greatest ancient empire and lasted from around 27 BC to 395 AD. The Romans were extremely proud of their empire, which often led them to compare themselves to those who had come before them. Virgil, a Roman poet alive during BCE, is considered Rome’s greatest poet. In one of his famous works, The Aeneid, Virgil showcases patriotism in his work. In The Aeneid, Virgil makes a comparison between the Romans and their predecessors of similar cultures, the Greeks. He uses parallels to Homer to make an argument for his point. Overall, the characters of Aeneas and Odysseus are representations of their separate cultures and through the comparison of them as heroes, Virgil attempts to show that the Romans were a†¦show more content†¦Following the Gods’ orders was his instinct even if it meant leaving his happy life behind. In leaving to create and found Rome, Aeneas will be leaving his lover Dido behind as well as his sweet life. 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