Dataset DOI: 10.5061/dryad.3ffbg79zn

Description of the data and file structure

All contained data are either the raw data directly from the instruments used to acquire the data, or aggregated collections of the data in a format sufficient for plotting and analysis in external programs. The data that are attached are compressed, zip folders of the raw data and other data used to make figures for the manuscript. Unzip these folders to access the raw data. All contained data are either the raw data directly from the instruments used to acquire the data, or aggregated collections of the data in a format sufficient for plotting and analysis in external programs. Most of the data was processed using Excel and MestreNova, with OriginPro allowing for final production of manuscript figures.

Files and variables

File: UV-Vis_Spectra.zip

This compressed folder has five different files in it. The UV-Vis summary Excel file "UV-Vis summary.xlsx" contains the final tabulated electronic absorption spectroscopy data for compounds 1-4 from the main manuscript. The data is saved as an Excel file. Data are organized in columns: wavelength (nm), absorbance (A), and molar absorptivity (epsilon) for each of the complexes, respectively. An additional column that converts the wavelength to wavenumbers is provided for convenience. The main manuscript contains the plot of epsilon versus wavenumber as Figure 3. See main manuscript for measurement conditions, used instrument, and other relevant experimental points.

The other four files, labeled as "compound name 0.1mM.csv" are the raw instrumental outputs saved in comma-delimited files that can be opened via any text editor and Excel. These data were all collected at 0.1 mM concentration. These .csv files have all experimental data. Briefly, the block of text under "summary" contains instrumental summary information (spectrometer, model, software version, sample name); "parameter" has explicit instrumental collection conditions, e.g., the wavelength window, the slit width, the scanning speed; and below that are the actual data in two columns, one of wavelength, and one of absorbance.

File: Low-field_NMR.zip

This compressed file contains two folders that constitute the worked up ("processed") and raw ("unprocessed") low-field NMR spectra.

In the unprocessed data folder, there are four subfolders labeled with the compound #s from the manuscript. Dragging one of these folders into MestreNova (see NMR program details below) will immediately open the results of the experiment. There are subfolders with instrumental parameters and a .jdx file, which is a standardized spectral formula (see NMR notes below).

The processed data folder contains the worked-up data for each compound. They are saved as tab-delimited .csv files, each with two columns, ppm on the left and spectral intensity on the right. These can be opened in any graphing program. The folder also contains all of them collected into a single MNova file as well, which can be opened with MestreNova. 

File: RT_51V_NMR_spectra.zip

This compressed data set has the room-temperature ⁵¹V NMR spectra for complexes 1-4, which are depicted in Figure 3 in the main manuscript. This folder contains ten different files.

There are four tab-delimited .csv files, one for each complex, which are the xy coordinates for the NMR spectra as depicted in Figure 3. These data are separated into two columns, left is chemical shift in ppm and the right one is the 51V NMR signal intensity. These data can be opened with any standard text edit/spreadsheet software.

There are also five folders entitled, e.g., "Compound 1 25 dC". These folders contain the raw instrumental output from the NMR for each of the four compounds, all collected at 25 degrees Celsius. These folders can be dragged, in their entirety, into the program MestreNova (see notes below) and it will give an initial process of the corresponding NMR spectrum.

The final file in this folder is "All compounds in MeCN at 25dC.mnova". This is the aggregate data set from the room temperature ⁵¹V NMR spectra, all collected in acetonitrile (MeCN) in a format that can be opened by MestreNova by simply dragging the file into the opened program window (see notes below about MestreNova and NMR processing). 

File: 2D_NMRs.zip

This compressed folder contains all of the 2-dimensional NMR spectra used to assign structure for complexes 1-4. In this folder are four compressed folders that contain relevant NMR spectra for the labeled compound.

The folder for compound 1 contains the one-dimensional proton NMR spectra, labeled as 1H and 1H D2O spike for this complex. The files including COSY and NOESY in this folder correspond to the 2D spectra depicted in the manuscript SI file.

The folder for compound 2 contains the one-dimensional 1H NMR spectrum (labeled as "1H") and the two-dimensional spectra are labeled with "COSY" and "NOESY".

The folder for compound 3 contains the one-dimensional proton ("1H") and COSY and NOESY spectra.

Compound 4 only contains the COSY and NOESY 1H spectra.

For all folders, data is supplied as folders that can be opened with MestreNova (or other appropriate NMR software, see below) or the MestreNova files themselves.

File: VT_NMR_data.zip

The compressed folder with this data contains variable-temperature NMR spectra for all complexes and tabulated variable-temperature NMR linewidths discussed in the manuscript. All temperatures are in degrees C.

There are four subfolders associated with this data set, which are labeled according to the complexes (1-4) which they correspond to. Within these subfolders, there are a set of subfolders labeled with the name of the complex, e.g., "VO(3OEtHSHED)(TBAD)" for complex 1 and then a number, ranging from 25 to 50. These folders are the solution phase NMR spectra for the complexes, and the number corresponds to the temperature of the experiment. Like with other NMR spectra collected here, these folders can be dragged into the MNova (or other) software for analysis. We have also collected the worked up variable temperature data for the compound into a single MNova file in each of these folders.

Finally, there is an Excel spreadsheet that collects the temperature dependence of peak positions and their linewidths. This spreadsheet can be opened in Excel or other spreadsheet software. The data are organized in this spreadsheet by compound (1 to 4, from left to right). The solvent of measurement is listed under the name of the compound. The top rows of variable temperature data contain the chemical shift information. Below that, in the data sets marked, e.g., "Peak 4 (SW)" we have the signal linewidths in Hz and then the same values in ppm even further down. There is a "Dd/DT" row which is the thermal sensitivity of the chemical shift for the variable temperature data sets and then a "Resolution" row even further down which contains values of thermal sensitivity divided by the linewidth.

Code/software

Data that is recorded as .csv, .txt, or in other common spreadsheet extensions can be opened in Excel or other standard plotting software.

The majority of our NMR data were analysed and processed using MNova. MestreNova (or MNova) is a common NMR-processing software. Many universities have access to it by purchasing a license, and analysis of the data can be performed simply by dragging the FID files into the program. There are alternatives for analysis, e.g. Topspin. There are also free software packages available for analysis. MNova has NMR Lite, which is a cheaper version and can be used free for an extended period. The program NUTS is also a free software package that is available from Anasazi Instruments. In some cases, NMR spectra are saved in the .jdx file type, which can be opened with many different spectral software, including the free jspecview. See here for more details.

Access information

Other publicly accessible locations of the data:

• Figures and some tabulated data are available in the SI of the manuscript at DOI: 10.1039/D6CC02350A

Data was derived from the following sources:

• N/A