20.1: Organization
- Page ID
- 332821
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\(\newcommand{\avec}{\mathbf a}\) \(\newcommand{\bvec}{\mathbf b}\) \(\newcommand{\cvec}{\mathbf c}\) \(\newcommand{\dvec}{\mathbf d}\) \(\newcommand{\dtil}{\widetilde{\mathbf d}}\) \(\newcommand{\evec}{\mathbf e}\) \(\newcommand{\fvec}{\mathbf f}\) \(\newcommand{\nvec}{\mathbf n}\) \(\newcommand{\pvec}{\mathbf p}\) \(\newcommand{\qvec}{\mathbf q}\) \(\newcommand{\svec}{\mathbf s}\) \(\newcommand{\tvec}{\mathbf t}\) \(\newcommand{\uvec}{\mathbf u}\) \(\newcommand{\vvec}{\mathbf v}\) \(\newcommand{\wvec}{\mathbf w}\) \(\newcommand{\xvec}{\mathbf x}\) \(\newcommand{\yvec}{\mathbf y}\) \(\newcommand{\zvec}{\mathbf z}\) \(\newcommand{\rvec}{\mathbf r}\) \(\newcommand{\mvec}{\mathbf m}\) \(\newcommand{\zerovec}{\mathbf 0}\) \(\newcommand{\onevec}{\mathbf 1}\) \(\newcommand{\real}{\mathbb R}\) \(\newcommand{\twovec}[2]{\left[\begin{array}{r}#1 \\ #2 \end{array}\right]}\) \(\newcommand{\ctwovec}[2]{\left[\begin{array}{c}#1 \\ #2 \end{array}\right]}\) \(\newcommand{\threevec}[3]{\left[\begin{array}{r}#1 \\ #2 \\ #3 \end{array}\right]}\) \(\newcommand{\cthreevec}[3]{\left[\begin{array}{c}#1 \\ #2 \\ #3 \end{array}\right]}\) \(\newcommand{\fourvec}[4]{\left[\begin{array}{r}#1 \\ #2 \\ #3 \\ #4 \end{array}\right]}\) \(\newcommand{\cfourvec}[4]{\left[\begin{array}{c}#1 \\ #2 \\ #3 \\ #4 \end{array}\right]}\) \(\newcommand{\fivevec}[5]{\left[\begin{array}{r}#1 \\ #2 \\ #3 \\ #4 \\ #5 \\ \end{array}\right]}\) \(\newcommand{\cfivevec}[5]{\left[\begin{array}{c}#1 \\ #2 \\ #3 \\ #4 \\ #5 \\ \end{array}\right]}\) \(\newcommand{\mattwo}[4]{\left[\begin{array}{rr}#1 \amp #2 \\ #3 \amp #4 \\ \end{array}\right]}\) \(\newcommand{\laspan}[1]{\text{Span}\{#1\}}\) \(\newcommand{\bcal}{\cal B}\) \(\newcommand{\ccal}{\cal C}\) \(\newcommand{\scal}{\cal S}\) \(\newcommand{\wcal}{\cal W}\) \(\newcommand{\ecal}{\cal E}\) \(\newcommand{\coords}[2]{\left\{#1\right\}_{#2}}\) \(\newcommand{\gray}[1]{\color{gray}{#1}}\) \(\newcommand{\lgray}[1]{\color{lightgray}{#1}}\) \(\newcommand{\rank}{\operatorname{rank}}\) \(\newcommand{\row}{\text{Row}}\) \(\newcommand{\col}{\text{Col}}\) \(\renewcommand{\row}{\text{Row}}\) \(\newcommand{\nul}{\text{Nul}}\) \(\newcommand{\var}{\text{Var}}\) \(\newcommand{\corr}{\text{corr}}\) \(\newcommand{\len}[1]{\left|#1\right|}\) \(\newcommand{\bbar}{\overline{\bvec}}\) \(\newcommand{\bhat}{\widehat{\bvec}}\) \(\newcommand{\bperp}{\bvec^\perp}\) \(\newcommand{\xhat}{\widehat{\xvec}}\) \(\newcommand{\vhat}{\widehat{\vvec}}\) \(\newcommand{\uhat}{\widehat{\uvec}}\) \(\newcommand{\what}{\widehat{\wvec}}\) \(\newcommand{\Sighat}{\widehat{\Sigma}}\) \(\newcommand{\lt}{<}\) \(\newcommand{\gt}{>}\) \(\newcommand{\amp}{&}\) \(\definecolor{fillinmathshade}{gray}{0.9}\)Spectral Problems with 2D Spectra: Organization
Data Tables and Partial Structures
Compiling data tables is a critical first step in solving complex spectral problems. There is a standard expected format for reporting NMR data.
Showing all of the steps and the correlations is the best way to organize your data (and demonstrate mastery of these learning outcomes!).
*All spectra are either from SDBS (Japan National Institute of Advanced Industrial Science and Technology) or simulated.
An example of compiling the data and showing your work on a simple structure.
1. Complete the table for the 1D 1H NMR including all of the coupling and integration information. Also be sure to include partial structures.
| Letter assignment | Chemical Shift | Integration | Multiplicity | 3JHH | Part Structure |
|---|---|---|---|---|---|
| A | 2.4 | 2H | q | CH3-CH2-C=O | |
| B | 2.1 | 3H | s | CH3-C=O | |
| C | 1.0 | 3H | t | CH3-CH2 |
2. Add H,C HMQC information.
3. Add the COSY Correlations. Confirm the partial structure from the 1H NMR.
| Assignment | Shift | Integ. | Mult | 1JHC | 3JHH | Part Structure |
|---|---|---|---|---|---|---|
| 3 | 2.4 | 2H | q | C3 (36) | 4 | CH3-CH2-C=O |
| 1 | 2.1 | 3H | s | C1 (27) | CH3-C=O | |
| 4 | 1.0 | 3H | t | C4 (7) | 3 | CH3-CH2 |
4. Add the HMBC Correlations. Use this information to put together spin systems.
| Assignment | Shift | Integ. | Mult | 1JHC | 3JHH | 2-4JHC | Part Structure |
|---|---|---|---|---|---|---|---|
| 3 | 2.4 | 2H | q | C3 (36) | 4 | C1, C4, C2 | CH3-CH2- C=O |
| 1 | 2.1 | 3H | s | C1 (27) | C2, C3 | CH3-C=O | |
| 4 | 1.0 | 3H | t | C4 (7) | 3 | C2, C3 | CH3-CH2 |
5. If any piece of data doesn’t fit, then go back through the data and revise the structure.