Revista Boliviana de Química
versión On-line ISSN 0250-5460
Rev. Bol. Quim vol.34 no.4 La Paz 2017
LOS COMENTARIOS Y/O ARTÍCULOS TEÓRICOS
NMR Mestrenova, short manual for beginners
NMR Mestrenova, pequeño manual para debutantes
José A. Bravo1,*, José L. Vila2, Yonny Flores3
1Natural Product Laboratory, Phytochemistry, Chemical Sciences Department, School of Pure and Natural Science FCPN,
Universidad Mayor de San Andrés UMSA, P.O. Box 303, Calle Andrés Bello s/n, Ciudad Universitaria Cota Cota,
phone +59122792238, La Paz, Bolivia, jabravo@umsa.bo, www.umsa.bo
2Natural Product Laboratory, Green Chemistry, Chemical Sciences Department, School of Pure and Natural Science FCPN,
Universidad Mayor de San Andrés UMSA, P.O. Box 303, Calle Andrés Bello s/n, Ciudad Universitaria Cota Cota,
phone +59122772269, La Paz, Bolivia, jlvila@umsa.bo, www.umsa.bo
3NMR Laboratory, Chemical Research Institute IIQ, Chemical Sciences Department, School of Pure and Natural Science FCPN,
Universidad Mayor de San Andrés UMSA, P.O. Box 303, Calle Andrés Bello s/n, Ciudad Universitaria Cota Cota,
phone +59122795878, La Paz, Bolivia, yflores@umsa.bo, www.umsa.bo
*Corresponding author: joseabravo@outlook.comjoseabravo@outlook.com
Received 10 22 2017 Accepted 10 28 2017 Published 10 30 2017
ABSTRACT
This short review presents in a very compact manner the few steps to manipulate 1D and consequently 2D NMR spectra generated in the MestReNova® system. The manual explains how easily we can transform spectral data into different expositive manners. In this sense, we started showing the way to put together 13C and DEPT spectra in the same page with peaks aligned. The way to write, erase or edit the name of spectra is also explained. The way to manipulate 1H NMR spectra is exposed. The treatment and development of most common use 2D spectra is detailed; this includes COSY/NOESY spectra as well as HSQC/HMBC spectra.
Keywords: NMR, MestReNova, Short manual, COSY, HMBC, HSQC, DEPT.
RESUMEN
La presente breve reseña expone de manera muy compacta los pocos pasos para manipular espectros RMN 1D y, en consecuencia, los espectros RMN 2D generados en el sistema MestReNova®. El manual explica con qué facilidad podemos transformar los datos espectrales en diferentes maneras expositivas. En este sentido, comenzamos a exponer la manera de armar los espectros 13C y DEPT en la misma página con los picos alineados. También se explica la forma de escribir, borrar o editar el nombre de los espectros. La forma de manipular los espectros de 1H RMN también está expuesta. El tratamiento y desarrollo de los espectros 2D de uso más común se detalla; esto incluye los espectros COSY / NOESY así como los espectros HSQC / HMBC.
13C NMR
To put
Opening of files. In MestReNova select open in the toolbar and open the folder containing the
Click over the shorter size DEPT spectrum at left. It appears on screen. Chose the same spectral window as the one defined for the
Defining of the spectral window. To prepare a doubly 1D spectrum (or two spectra in the same page) we use the same ppm values to define a zoom by means of the Manual Zoom option, in the
Accommodation of both spectra in the same screen, and peak-picking. Click over the shorter size DEPT spectrum at left. It appears on screen. Click once on the spectrum on the screen, the spectrum becomes reducible. Using the mouse click on the small green square on top and slide the mouse downwards until the spectrum is half the size of the original spectrum. Next, click over the shorter size
Now youre free to displace any of the spectra downwards or upwards using the shifting arrows on your PC keyboard. We see:
Once separated one spectrum from each other (i.e. put the DEPT in the upper region of the screen and the
Select in the toolbar the option File. Select the option save as. A new window named Save as appears on the screen. Choose either the folder containing the
Transfer of the just generated screen containing both spectra with aligned peaks. Select edit in the toolbar and then select the select all option. The full screen containing both spectra already displaced and accommodated results selected. Unroll the edit option in the toolbar. Select the copy option. Open a new document in Word. Paste in the current document of Word. The picture is ready to be manipulated as any figure on that page of Word. You can rotate it and reduce or enlarge the picture containing both spectra.
TITLE
To put, edit or erase a title of a spectrum [1]
The spectrum appears after clicking open and choosing a file or a spectrum (called 1r if 1D or 2rr if 2D). In MestReNova do double click over the spectrum. The window Properties appears on screen. Choose option common in the menu. Click option title if a title is desired or unclick if not. If the option title is chosen then pick up a font and then click in option . The Macro editor option appears and you can write a title in Text and click OK. The windows Properties appears, and click in Apply and OK. The title appears on the left upper corner of the spectrum.
1H NMR
1H Peak-picking [1]
In the 1H spectrum proceed as explained above for the
1H Integration [1]
Double click on the spectrum on screen. The window Properties appears. Choose in the vertical toolbar at left the option integrals. Mark on integrals and select: Font, decimals, position, margin, for the label. Mark color, position, maximum height for the curve. Do apply and OK. Go to the tool bar and select Integrations and there click on manual. In order to set the number of protons for the integral of a signal, right-click the mouse on the integral curve on the spectrum. Choose edit integral option. The Integral manager window appears on screen. Choose in Normalized the number of protons for the signal and apply to all. Youre done. Save as explained.
HOMONUCLEAR 2D SPECTRA
A COSY/NOESY spectrum [1]
Opening of files. In MestReNova select open in the toolbar and open the folder containing the COSY/NOESY data, then open sequentially: pdata,
Symmetrizing and choosing size of crosspeaks in COSY. Before defining the spectral window it is convenient to symmetrize the COSY spectrum. Click on the small COSY spectrum at the left of the screen. The COSY spectrum appears on screen. Click in the COSY spectrum in the screen. Search in the toolbar the option processing then choose symmetrize and then the sub-option COSY-like. The COSY spectrum symmetrized appears on screen. Choose the desired and most fitting intensity of the COSY contour plot by means of the mouses wheel (to increase or decrease the crosspeaks size) or by pressing on the + (increase) or - (decrease) keys on your PC keyboard.
Choosing size of crosspeaks in NOESY. The 1H spectrum is on the screen. Click over the shorter size NOESY spectrum at the left of the full screen. The NOESY spectrum appears on screen. Choose the desired and most fitting intensity of the NOESY contour plot by means of the mouses wheel (to increase or decrease the crosspeaks size) or by pressing on the + (increase) or - (decrease) keys on your PC keyboard. We see:
Defining of the spectral window. Click on the COSY/NOESY spectrum on screen. Select zoom in in the toolbar. Select a spectral window on the COSY/NOESY pressing the left key of the mouse and moving throughout the spectrum including all pertinent crosspeak. Release the mouses key. The spectral window appears on screen. We see:
Plotting the proton projection and applying the Contour Plot option. Check for the vertical toolbar at the left side of the screen of MestReNova. Look for the Bitmap Plot icon. Click on the two arrows below such icon. An extra icon appears at the right side of the Bitmap Plot icon under the name Show traces. Unfold Show traces and choose Setup. The window Setup traces appears on screen. Click on the title of the 1H spectrum appearing in the square Available 1D spectra:. Select the horizontal trace by clicking in the corresponding box. Click again on the title of the 1H spectrum appearing in the square Available 1D spectra:. Select the vertical trace by clicking in the corresponding box. Click OK and the current window disappears. The COSY/NOESY spectrum appears on screen with both projections (traces). Check for the vertical toolbar at the left side of the screen of MestReNova. Look for the Bitmap Plot icon and unfold the corresponding menu clicking on the button at right, four options appear, chose contour plot. Save as the current COSY/NOESY spectrum. The window Save as appears on screen. Choose the folder containing the COSY/NOESY data. Open sequentially the folders data and
You can zoom on this spectrum on screen with zoom in in the toolbar. Save as: _____ this zoom. We see:
HETERONUCLEAR 2D SPECTRA
A HSQC/HMBC spectrum [1]
Opening of files. In MestReNova select open in the toolbar and open the folder containing the HSQC/HMBC data, then open sequentially: pdata,
Choosing size of crosspeaks in HSQC/HMBC. The
Defining of the spectral window. Click on the HSQC/HMBC spectrum on screen. Select zoom in in the toolbar. Select a spectral window on the HSQC/HMBC pressing the left key of the mouse and moving throughout the spectrum including all pertinent crosspeak. Release the mouses key. The spectral window appears on screen. We see:
Plotting the proton and carbon projections. Check for the vertical toolbar at the left side of the screen of MestReNova. Look for the Bitmap Plot icon. Click on the two arrows below such icon. An extra icon appears at the right side of the Bitmap Plot icon under the name Show traces. Unfold Show traces and choose Setup. The window Setup traces appears on screen. Click on the title of the 1H spectrum appearing in the square Available 1D spectra:. Select the horizontal trace by clicking in the corresponding box. Click on the title of the
You can zoom on this spectrum on screen with zoom in in the toolbar. Save as: _____ this zoom. We see:
REFERENCES
1. MNOVA, MESTRELAB. 2010, MestReNova Manual, MestreNova 6.2.1. [ Links ]