ssNMR_spectra_exp_&_fit

Solid-State Nuclear Magnetic Resonance (ssNMR) Spectroscopy of NaMO₂F₂ (M = Nb, Ta)

Author: Ouail Zakary
ORCID: 0000-0002-7793-3306
E-mail: [email protected]
Website: Ouail Zakary - webpage

This folder contains the solid-state nuclear magnetic resonance (ssNMR) spectroscopy data for the compounds NaNbO₂F₂ and NaTaO₂F₂, recorded for the nuclei ¹⁹F, ²³Na, and ⁹³Nb.

Overview of the Data

The dataset is divided into two main folders for NaNbO₂F₂ and NaTaO₂F₂, with subfolders for each nucleus. The NMR spectra were recorded and fitted using Bruker TopSpin and DMFit software, respectively.

Folders and Data Structure

1. NaNbO₂F₂

   • ¹⁹F Nucleus:
     Path: ./NaNbO2F2/19F
     Fit File: 1R.fxml

   • ²³Na Nucleus:
     Path: ./NaNbO2F2/23Na
     Fit File: 1R.fxml

   • ⁹³Nb Nucleus:
     Path: ./NaNbO2F2/93Nb
     Fit File: 1R.fxml

2. NaTaO₂F₂

   • ¹⁹F Nucleus:
     Path: ./NaTaO2F2/19F
     Fit File: 1R.fxml

   • ²³Na Nucleus:
     Path: ./NaTaO2F2/23Na
     Fit File: 1R.fxml

Methods

¹⁹F (I = 1/2) MAS NMR spectra were recorded using a Bruker Avance III spectrometer operating at 7 T (Larmor frequency of 282.4 MHz) and a 1.3 mm CP-MAS probe-head. The Hahn echo sequence was applied with an interpulse delay of one rotor period and a recycle delay of 20 s. A 90° pulse (RF field: 160 kHz, pulse duration: 1.56 μs) was used. For NaNbO₂F₂, SPINAL-64 decoupling of ⁹³Nb was employed during acquisition (RF field: ~106 kHz).

²³Na (I = 3/2) MAS NMR spectra were recorded at 20 T (Larmor frequency: 224.9 MHz) with a 2.5 mm CP-MAS probe-head. The spectra were acquired using a heteronuclear ²³Na–¹⁹F SPINAL-64 decoupling sequence at a RF field of 132 kHz, with a 1 s recycle delay and a small pulse flip angle of 10° (pulse duration: 0.35 μs).

⁹³Nb (I = 9/2) MAS NMR spectra were recorded using a 1.3 mm CP-MAS probe-head at 20 T (Larmor frequency: 208.1 MHz). The Hahn echo sequence was applied with a 1 s recycle delay, using a CT 90° selective pulse (RF field: 125 kHz, pulse duration: 2 μs).

References:

• ¹⁹F spectra were referenced to CFCl₃.
• ²³Na spectra were referenced to a 1 M NaCl aqueous solution.
• ⁹³Nb spectra were referenced to a saturated K[NbCl₆]/CH₃CN solution.

Data Analysis

The raw ssNMR data was processed using Bruker TopSpin software and fitted using DMFit. The fitting files (1R.fxml) for each experiment are provided in their respective directories, and the fits can be visualized using DMFit.

Raw Data and Fits:

• NaNbO₂F₂:

  • ¹⁹F: Raw Data and Fit
  • ²³Na: Raw Data and Fit
  • ⁹³Nb: Raw Data and Fit

• NaTaO₂F₂:

  • ¹⁹F: Raw Data and Fit
  • ²³Na: Raw Data and Fit

Requirements

To acquire, analyze, and visualize the ssNMR data, the following equipment and software are required:

• Equipment Requirements:

  • Bruker Avance III spectrometer (7 T and 20 T) or equivalent, along with CP-MAS probe-heads.

• Software Requirements:

  • Bruker TopSpin: Required to process and visualize the raw NMR data. You can obtain the software from Bruker's website.
  • DMFit: Required to fit the NMR spectra. The software is available for download at the DMFit website.

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For further details, please refer to the respective folders or contact the author via the provided email.