Analysis of compounds: NMR

The experiments which can be performed in the NMR Service, depending on the instrument and the available probes, (http://www.cenquior.csic.es/cenquior/rmn/experimentosrealizables), are:
- Monodimensional experiments for different nuclei: 1H, 13C, 15N, 29Si, 19F, 31P, 11B.
- Bidimensional experiments: homonuclear correlation (COSY, TOCSY), heteronuclear correlation (HSQC, HMBC) and hybrid experiments (HSQC-TOCSY).
- Nuclear Overhauser Effect experiments: monodimensional (NOE, ROE) and bidimensional (NOESY, ROESY).
- Diffusion experiments (DOSY).
Even, variable temperature experiments can be done, from -100 to +100 ºC, depending on the instrument.
EQUIPMENT:
BRUKER AVANCE III-400
9.395T superconducting equipment, which can get both proton and heteronuclear spectra, mono or two-dimensionals. It has a probe with gradients, and a variable temperature unit.
JEOL JNM-ECZ400R
9.395T superconducting equipment, which can get both proton and heteronuclear spectra, mono or two-dimensionals. It has a royal probe with gradients, and a variable temperature unit.
VARIAN INOVA-300
7.046T superconducting equipment, which can get both proton and heteronuclear spectra, mono or two-dimensionals. It has an inverse detection probe and a direct detection multinuclear probe, and a variable temperature unit. It is accessible to authorized internal users.
BRUKER AVANCE-300
7.046T superconducting equipment, which can get proton and carbon-13 spectra, mono or two-dimensionals. It has an inverse detection probe, a variable temperature unit and an automated sample changer.

NMR (500 and 400 MHz)
Analysis of compounds by NMR 1H, 13C, 15N, 19F and 31P
Equipment:
spectrometer Bruker Avance NEO 500 and Avance 400

Structural elucidation of small molecules. Connectivity, stereochemical configuration and conformation
Structural characterization of macromolecules
Structural characterization of solids (Structural elucidation of non soluble solids; Characterization of immobilized compounds in solids; Molecular mobility studies in solids)
Mixtures analysis, components quantification and identification
Study of chemical reaction mechanisms, characterization of reaction intermediates, determination of kinetic and thermodynamic parameters
Study of intermolecular interactions, host-guest affinity, molecular recognition in enzyme-substrate systems

Nuclear Magnetic Resonance (NMR) spectroscopy is a non-destructive technique, based on the magnetic properties of matter and applicable to any substance in a liquid or solid state that contains nuclei with nuclear spin values other than zero (1H, 13C, 15N, 19F, 31P, etc.), which can be used to solve various problems of research in chemistry, biology, biomedicine and material sciences, as well as quality control of research and / or commercial products.
The NMR in liquid medium (available in the CIB) comprises a versatile set of techniques and experiments applicable to the structural elucidation, the conformational determination and stereochemical analysis of organic and inorganic molecules, the structural and three-dimensional characterization of biomolecules (proteins, nucleic acids, carbohydrates, lipids, etc.), the study of molecular recognition processes and interactions between biomolecules and molecules of biological and biomedical interest, the analysis of chemical equilibria, the monitoring of chemical and biochemical reaction kinetics and the analysis and quantification of mixtures, among others. The tests are carried out in solution, in water or other solvents, with the possibility of carrying out experiments at different temperatures when the investigation so requires.
EXPERIMENTS THAT CAN BE CARRIED OUT IN THE CIB NMR FACILITY:
1H, 13C, 15N, 19F-monodimensional experiments
Bidimensional experiments of homonuclear correlation (COSY, TOCSY, etc.), heteronuclear correlation (HSQC, HMBC, etc.) and hybrids (HSQC-TOCSY, etc.)
Nuclear Overhauser Effect experiments both in the monodimensional (NOE, ROE) and bidimensional forms (NOESY, ROESY, etc.)
Experiments of Saturation Transfer Difference (STD)
Experiments for determination of molecular size by diffusion (DOSY)
The range of working temperatures, depending on the equipment used, varies between -10 and 80 ºC.
The CIB NMR Facility has three NMR spectrometers of the Bruker brand, two 600 MHz and one 500 MHz:
TECHNICAL EQUIPMENT OF THE CIB NMR SERVICE:
NMR Spectrometers:
Bruker AV 500MHz
Bruker AV 600MHz, with cryoprobe
Bruker AV III 600MHz, with Sample Case Standard, cooled, available for 24 samples
Available Probes:
SEF 500MHz S2 5mm with Z-gradient (in use in the AV 500MHz)
TXI 600MHz S3 5mm with Z-gradient (in use in the AVIII 600MHz)
CP TXI 600 S3 H-C/N-D-05 Z (in use in the AV 600MHz)
TXI 500MHz S2 5mm with Z-gradient
TXI 600MHz S3 5mm with Z-gradient; BTO
SEF 600MHz S3 5mm with Z-gradient
Software for acquisition and processing:
TopSpin 2.1 in the AV 500MHz and AV 600 MHz with cryoprobe
TopSpin 3.5 pl5 in the AVIII 600 MHz
IconNMR 5.0 in the AVIII 600 MHz

Identification and semi-quantification of primary and secondary metabolites by 1D and 2D experiments by 1H-NMR 2D 1H- 13C HSQC with the addition of external standard (TSP-d4 or DSS-d6).

Spectra adquisition on 400 MHz NMR spectrometer for small molecule structural characterization, in open access mode using the automatic sampler.