READ ME File For 'Data set for Novel Electrolytes for Magnesium Metal Battery' Dataset DOI: https://doi.org/10.5258/SOTON/D3497 ReadMe Author: MEGAN REBECCA DAW, University of Southampton ORCID ID 0000-0003-0043-7096 This dataset supports the thesis entitled: Novel Electrolyte Materials for Rechargeable Magnesium Metal Batteries AWARDED BY: Univeristy of Southampton DATE OF AWARD: 2025 DESCRIPTION OF THE DATA This data set includes: Electrochemical data (cyclic voltammetry, galvanostatic cyclic, potentiostatic electrochemical impedance spectroscopy and open circiut potentials) as .txt files that can be viewed in biologic EC-Lab software or equivalent. Nuclear magnetic resonance (NMR): 1H, 19F, 19F{1H}, 13C, 11B, 27Al, data analysis in ACD-Labs Spectrus Processor. Spectra were collected using a Bruker AVII400 or Bruker AVIIIHD400 FT-NMR spectrometers in the indicated solvent at 298 K. Chemical shifts for proton and carbon spectra are reported on the delta scale in ppm and were referenced to a residual solvent reference or internal TMS reference. 19F NMR spectra were referenced to CFCl3 in CDCl3. 27Al NMR spectra were referenced to Al(NO3)3 in D2O. Mass spectrometry: Samples were analysed by mass spectrometry using a MaXis (Bruker Daltonics, Bremen, Germany) time of flight (TOF) mass spectrometer. Samples were infused using a syringe driver at a constant flow rate of 3 μL min-1. Ultrahigh performance liquid chromatography was performed using a Waters UPLC BEH C18 (50 mm x 2.1 mm 1.7 µm) column. Gradient elution from 20 % acetonitrile (0.2 % formic acid) to 100 % acetonitrile (0.2 % formic acid) was performed in five minutes at a flow rate of 0.6 mL min-1. High resolution negative ion electrospray ionisation mass spectra were recorded. Infrared spectroscopy: Generated in ACD-Labs Spectrus Processor. IR spectroscopy was carried out in Nujol between CsI plates using a Perkin-Elmer Spectrum 100 spectrometer over a range of 4000-200 cm-1. SEM images: SEM images of electrode surfaces and powders were collected on a ZEISS Sigma 500 VP FE-SEM. EDS maps were collected using an Ultim170 (Oxford instruments) detector. Powder X-ray diffraction: Powder samples from synthesis were characterised by powder X-ray diffraction (XRD) on a Bruker D2 Phaser diffractometer (Cu Kα radiation, λ = 1.5418 Å) at room temperature with a 0.2 s step rate, and 2θ range 5 - 80°, using Bragg-Brentano geometry. Rietveld refinement was carried out using GSAS-II software, and patterns were compared to CIF files from the ICSD crystallographic database. Single-crystal X-ray diffraction: Data was collected on a Rigaku FR-E+ Ultra High Flux Diffractometer with a universal goniometer (UG2), Intelligent Goniometer Head (IGH) and a HyPix-6000HE detector. SuperBright molybdenum (Mo Kα, λ = 0.71073 Å) X-ray generator with a highly focused beam (70 µm) achieved with VHF Varimax optics. Structures were solved using Olex2 software This dataset contains: File name: 3_2-electrode Mg_1_SEM.TIF Description: SEM image of a Mg RE after GCPL in a 2-electrode cell, with APC electrolyte, Mg CE RE | Mo6S8 WE File name: 3_2-electrode Mg_2_SEM.TIF Description: SEM image of a Mg RE after GCPL in a 2-electrode cell, with APC electrolyte, Mg CE RE | Mo6S8 WE File name: 3_2-electrode Mg_3_SEM.TIF Description: SEM image of a Mg RE after GCPL in a 2-electrode cell, with APC electrolyte, Mg CE RE | Mo6S8 WE File name: 3_2-electrode MgAZ31_1_SEM.TIF Description: SEM image of a Mg RE after GCPL in a 2-electrode cell, with APC electrolyte, MgAZ31 CE RE | Mo6S8 WE File name: 3_2-electrode MgAZ31_2_SEM.TIF Description: SEM image of a Mg RE after GCPL in a 2-electrode cell, with APC electrolyte, MgAZ31 CE RE | Mo6S8 WE File name: 3_3-electrode Mg_1_SEM.TIF Description: SEM image of a Mg RE after GCPL in a 3-electrode cell, with APC electrolyte, Mg CE | Mg RE | Mo6S8 WE File name: 3_3-electrode Mg_2_SEM.TIF Description: SEM image of a Mg RE after GCPL in a 3-electrode cell, with APC electrolyte, Mg CE | Mg RE | Mo6S8 WE File name: 3_3-electrode MgAZ31_1_SEM.TIF Description: SEM image of a MgAZ31 RE after GCPL in a 3-electrode cell, with APC electrolyte, Mg CE | MgAZ31 RE | Mo6S8 WE File name: 3_3-electrode MgAZ31_2_SEM.TIF Description: SEM image of a MgAZ31 RE after GCPL in a 3-electrode cell, with APC electrolyte, Mg CE | MgAZ31 RE | Mo6S8 WE File name: 3_exp_Mo6S8_PXRD.txt Description: Powder XRD of synthesised Mo6S8 File name: 3_exp_Mo6Se8_PXRD.txt Description: Powder XRD of synthesised Mo6Se8 File name: 3_Figure 22_Front 3-electrode_OCV.txt Description: OCV, 8 h, APC electrolyte, Mg CE/RE | Mg WE (Front Orientation) File name: 3_Figure 23a_Mg Mg_OCV.txt Description: OCV, 8 h, APC electrolyte, Mg CE/RE | Mg WE File name: 3_Figure 23a_Mg MgAZ31_OCV.txt Description: OCV, 8 h, APC electrolyte, Mg CE/RE | MgAZ31 WE File name: 3_Figure 23a_Mg SS_OCV.txt Description: OCV, 8 h, APC electrolyte, Mg CE/RE | SS WE File name: 3_Figure 23a_MgAZ31 SS_OCV.txt Description: OCV, 8 h, APC electrolyte, MgAZ31 CE/RE | SS WE File name: 3_Figure 23b_Mg Mg SS_OCV.txt Description: OCV, 8 h, APC electrolyte, Mg CE | Mg RE | SS WE File name: 3_Figure 23b_Mg MgAZ31 SS_OCV.txt Description: OCV, 8 h, APC electrolyte, Mg CE | MgAZ31 RE | SS WE File name: 3_Figure 23b_SS Mg Mg_OCV.txt Description: OCV, 8 h, APC electrolyte, SS CE | Mg RE | Mg WE File name: 3_Figure 23b_SS MgAZ31 Mg_OCV.txt Description: OCV, 8 h, APC electrolyte, SS CE | MgAZ31 RE | Mg WE File name: 3_Figure 24a_2-electrode Mg Mo6S8_CV.txt Description: CV, 10 mV s-1, APC electrolyte, Mg CE/RE | Mo6S8 WE File name: 3_Figure 24b_3-electrode Mg Mg Mo6S8_CV.txt Description: CV, 10 mV s-1, APC electrolyte, Mg CE | Mg RE | Mo6S8 WE File name: 3_Figure 24c_3-electrode Mg MgAZ31 Mo6S8_CV.txt Description: CV, 10 mV s-1, APC electrolyte, Mg CE | MgAZ31 RE | Mo6S8 WE File name: 3_Figure 25a_Mg Mo6S8_CV.txt Description: CV, 10 mV s-1, APC electrolyte, Mg CE/RE | Mo6S8 WE (6hr OCV hold) File name: 3_Figure 25b_Mg Mg Mo6S8_CV.txt Description: CV, 10 mV s-1, APC electrolyte, Mg CE | Mg RE | Mo6S8 WE (6hr OCV hold) File name: 3_Figure 25c_Mg MgAZ31_CV.txt Description: CV, 10 mV s-1, APC electrolyte, Mg CE | MgAZ31 RE | Mo6S8 WE (6hr OCV hold) File name: 3_Figure 26a_2-electrode Mg Mo6S8_GCPL.txt Description: GCPL, 0.1C, APC electrolyte, Mg CE/RE | Mo6S8 WE File name: 3_Figure 26b_3-electrode Mg Mg Mo6S8_GCPL.txt Description: GCPL, 0.1C, APC electrolyte, Mg CE | Mg RE | Mo6S8 WE File name: 3_Figure 26c_3-electrode Mg MgAZ31 Mo6S8_GCPL.txt Description: GCPL, 0.1C, APC electrolyte, Mg CE | MgAZ31 RE | Mo6S8 WE File name: 3_Figure 31_Mg Mg Mo6Se8_GCPL.txt Description: GCPL. 0.1C, APC electrolyte, Mg CE | Mg CE | Mo6Se8 WE File name: 3_Mo6S8 cathode_SEM.TIF Description: SEM image of a Mo6S8 cathode (8:1:1, AM:Binder:Carbon, on stainless steel foil) File name: 3_Mo6S8 powder_SEM.TIF Description: SEM image of Mo6S8 powder mounted in carbon tape File name: 3_Mo6Se8 cathode_SEM.TIF Description: SEM image of a Mo6Se8 cathode (8:1:1, AM:Binder:Carbon, on stainless steel foil) File name: 3_Mo6Se8 powder_SEM.TIF Description: SEM image of Mo6Se8 powder mounted in carbon tape File name: 3_Pristine Mg_SEM.TIF Description: SEM image of pristine Mg surface File name: 3_Pristine MgAZ31_SEM.TIF Description: SEM image of pristine MgAZ31 surface File name: 4_[Mg(DME)3][Al(HFIP)4]2_19F NMR.txt Description: 19F{1H} NMR of [Mg(DME)3][Al(HFIP)4]2 in CDCl3 File name: 4_[Mg(DME)3][Al(HFIP)4]2_1H NMR.txt Description: 1H NMR of [Mg(DME)3][Al(HFIP)4]2 in CDCl3 File name: 4_[Mg(DME)3][Al(HFIP)4]2_27Al NMR.txt Description: 27Al NMR of [Mg(DME)3][Al(HFIP)4]2 File name: 4_[Mg(DME)3][Al(HFIP)4]2_ESI MS.pdf Description: Negative ion ESI-MS of [Mg(DME)3][Al(HFIP)4]2 File name: 4_AlDMEHFIP_19F NMR.txt Description: 19F{1H} NMR of [Al(DME)(HFIP)3] in CDCl3 File name: 4_AlDMEHFIP_1H NMR.txt Description: 1H NMR of [Al(DME)(HFIP)3] in CDCl3 File name: 4_AlDMEHFIP_27Al NMR.txt Description: 27Al NMR of [Al(DME)(HFIP)3] in CDCl3 File name: 4_AlTHFHFIP_19F NMR.txt Description: 19F{1H} NMR of [Al(THF)(HFIP)3] in CDCl3 File name: 4_AlTHFHFIP_1H NMR.txt Description: 1H NMR of [Al(THF)(HFIP)3] in CDCl3 File name: 4_AlTHFHFIP_27Al NMR.txt Description: 27Al NMR of [Al(THF)(HFIP)3] File name: 4_AlTHFHFIP_PXRD.txt Description: PXRD of [Al(THF)(HFIP)3] File name: 4_Li[Al(OtBuF)4]_19F NMR.txt Description: 19F NMR of Li[Al(OtBuF)4] in MeCN File name: 4_Li[Al(OtBuF)4]_1H NMR.txt Description: 1H NMR of Li[Al(OtBuF)4] in MeCN File name: 4_Li[Al(OtBuF)4]_ESI MS.pdf Description: Negative ion ESI-MS of Li[Al(OtBuF)4] in MeCN File name: 4_Mg(AlH4)2_BM 1h_PXRD.txt Description: PXRD of Mg(AlH4)2 from ball-milling for 1 h at 500 rpm File name: 4_Mg(AlH4)2_BM 3h_PXRD.txt Description: PXRD of Mg(AlH4)2 from ball-milling for 3 h at 500 rpm File name: 4_Mg(AlH4)2_HM_PXRD.txt Description: PXRD of Mg(AlH4)2 from hand-milling NaAlH4 / MgCl2 File name: 4_Mg(HFIP)2_19F NMR.txt Description: 19F{1H} NMR of [Mg(HFIP)2] in MeNO2 File name: 4_Mg(HFIP)2_1H NMR.txt Description: 1H NMR of [Mg(HFIP)2] in MeCN File name: 4_Mg[Al(OtBuF)4]2_NaCl_19F NMR.txt Description: 19F{1H} NMR of Mg[Al(OtBuF)4]2 target in CDCl3 File name: 4_Mg[Al(OtBuF)4]2_NaCl_1H NMR.txt Description: 1H NMR of Mg[Al(OtBuF)4]2 target in CDCl3 File name: 4_Mg[Al(OtBuF)4]2_NaCl_CV.txt Description: Plating/Stripping CV of 0.1 mol dm-3 Mg[Al(OtBuF)4]2 (with NaCl impurity) in DME, 10 mV s-1, Mg CE | Mg RE | Au WE File name: 4_Mg[Al(OtBuF)4]2_NaCl_ESI MS.pdf Description: Negative ESI-MS of Mg[Al(OtBuF)4]2 target in CDCl3 File name: 4_MgDMEAlHFIP_salt_CV.txt Description: CV, 10 mV s-1, 0.25 mol dm-3 [Mg(DME)3][Al(HFIP)4]2 / DME, Mg | Mg | Au, from redissolved salt File name: 4_MgDMEAlHFIP_solution_CV.txt Description: CV, 10 mV s-1, 0.25 mol dm-3 [Mg(DME)3][Al(HFIP)4]2 / DME, Mg | Mg | Au, from reaction solution File name: 4_MgTHFAlHFIP_19F NMR.txt Description: 19F{H} NMR of [Mg(THF)6][Al(HFIP)4]2 in CDCl3 File name: 4_MgTHFAlHFIP_1H NMR.txt Description: 1H NMR of [Mg(THF)6][Al(HFIP)4]2 in CDCl3 File name: 4_MgTHFAlHFIP_27Al NMR.txt Description: 27Al NMR of [Mg(THF)6][Al(HFIP)4]2 File name: 4_MgTHFAlHFIP_Mg Au_CV.txt Description: CV, 10 mV s-1, 0.65 mol dm-3 [Mg(THF)6][Al(HFIP)4]2 / THF, Mg | Mg | Au File name: 4_MgTHFAlHFIP_Mg Au_GCPL.txt Description: GCPL, 0.1C, 0.65 mol dm-3 [Mg(THF)6][Al(HFIP)4]2 / THF, Mg | Mg | Au File name: 4_MgTHFAlHFIP_Mg Au_PEIS.txt Description: PEIS, 0.65 mol dm-3 [Mg(THF)6][Al(HFIP)4]2 / THF, Mg | Mg | Au File name: 4_MgTHFAlHFIP_Mg Mg_CV.txt Description: CV, 10 mV s-1, 0.65 mol dm-3 [Mg(THF)6][Al(HFIP)4]2 / THF, Mg | Mg | Mg File name: 4_MgTHFAlHFIP_Mg Mg_PEIS.txt Description: PEIS, 0.65 mol dm-3 [Mg(THF)6][Al(HFIP)4]2 / THF, Mg | Mg | Mg File name: 4_MgTHFAlHFIP_Mg Mo6S8_GCPL.txt Description: GCPL, 0.1C, 0.65 mol dm-3 [Mg(THF)6][Al(HFIP)4]2 / THF, Mg | Mg | Mo6S8 File name: 4_MgTHFAlHFIP_PXRD.txt Description: PXRD of [Mg(THF)6][Al(HFIP)4]2 File name: 4_Salt metathesis_19F NMR.txt Description: 19F NMR of salt metathesis product (Mg[Al(OtBuF)4]2 target), in CDCl3 File name: 4_Salt metathesis_1H NMR.txt Description: 1H NMR of salt metathesis product (Mg[Al(OtBuF)4]2 target), in CDCl3 File name: 4_Salt metathesis_PXRD.txt Description:PXRD of salt metathesis product (Mg[Al(OtBuF)4]2 target) File name: 5_Mg12C4AlHFIP_19F NMR.txt Description: 19F NMR of the product collected from the reaction of [Mg(THF)6][Al(HFIP)4]2 and 2eq. 12-crown-4 File name: 5_Mg12C4AlHFIP_1H NMR.txt Description: 1H NMR of the product collected from the reaction of [Mg(THF)6][Al(HFIP)4]2 and 2eq. 12-crown-4 File name: 5_Mg15C5 powder_PXRD.txt Description: PXRD of bulk powder from synthesis of [Mg(THF)6][Al(HFIP)4]2 with 15-crown-5 File name: 5_Mg15C5AlHFIP bulk powder_1H NMR.txt Description: 1H NMR of bulk powder from the reaction of [Mg(THF)6][Al(HFIP)4]2 with 15-crown-5 in CDCl3 File name: 5_Mg15C5AlHFIP crystals_1H NMR.txt Description: 1H NMR of [Mg(κ5-15-crown-5)(Al(HFIP)3)3] in CDCl3 File name: 5_Mg18C6AlHFIP _DEC_Mg Au_CV.txt Description: CV, 10 mV s-1, 0.5 mol dm-3 [Mg(18-crown-6)(THF)2][Al(HFIP)4]2 / DEC, Mg|Mg|Au File name: 5_Mg18C6AlHFIP_19F NMR.txt Description: 19F{1H} NMR of [Mg(18-crown-6)(THF)2][Al(HFIP)4]2 in CDCl3 File name: 5_Mg18C6AlHFIP_1H NMR.txt Description: 1H NMR of [Mg(18-crown-6)(THF)2][Al(HFIP)4]2 in CDCl3 File name: 5_Mg18C6AlHFIP_27Al NMR.txt Description: 27Al NMR of [Mg(18-crown-6)(THF)2][Al(HFIP)4]2 in CD2Cl2 File name: 5_Mg18C6AlHFIP_DEC_Mg Au_GCPL.txt Description: GCPL, 1 mA h-1, 0.5 mol dm-3 [Mg(18-crown-6)(THF)2][Al(HFIP)4]2 / DEC, Mg|Mg|Au, plating/stripping File name: 5_MgH218N2O4_PXRD.txt Description: PXRD of the product collected from the reaction of [Mg(THF)6][Al(HFIP)4]2 and H2[18]aneN2O4 File name: 5_MgTHF_12C4 Mg Mg Au_CV.txt Description: CV, 10 mV s-1, Mg|Mg|Au, 0.65 mol dm-3 [Mg(THF)6][Al(HFIP)4]2 + 2 eq. 12-crown-4 File name: 5_MgTHF_15C5 Mg Mg Au_CV.txt Description: CV, 10 mV s-1, Mg|Mg|Au, 0.65 mol dm-3 [Mg(THF)6][Al(HFIP)4]2 + 1 eq. 15-crown-5 File name: 5_MgTHF_18C6 Mg Mg Au_CV.txt Description: CV, 10 mV s-1, Mg|Mg|Au, 0.65 mol dm-3 [Mg(THF)6][Al(HFIP)4]2 + 1 eq. 18-crown-6 File name: 6_Mg(BOB)2_IR.txt Description: IR (Nujol mull) of Mg(BOB)2 File name: 6_Mg(BOB)2_PXRD.txt Description: PXRD of Mg(BOB)2 File name: 6_Mg(DFOB)2_IR.txt Description: IR (Nujol mull) of Mg(DFOB)2 File name: 6_Mg(DFOB)2_PXRD.txt Description: PXRD of Mg(DFOB)2 File name: 6_MgDME_CV.txt Description: CV, 10 mV s-1, Mg|Mg|Au, 0.25 mol dm-3 [Mg(DME)3][Al(HFIP)4]2 / DME File name: 6_MgDME_Mg(BH4)2_CV.txt Description: CV, 10 mV s-1, Mg|Mg|Au, 0.25 mol dm-3 [Mg(DME)3][Al(HFIP)4]2 / DME + 50 mM Mg(BH4)2 File name: 6_MgDME_Mg(BH4)2_PEIS.txt Description: PEIS between CV cycles, Mg|Mg|Au, 0.25 mol dm-3 [Mg(DME)3][Al(HFIP)4]2 / DME + 50 mM Mg(BH4)2 File name: 6_MgDME_Mg(BOB)2_CV.txt Description: CV, 10 mV s-1, Mg|Mg|Au, 0.25 mol dm-3 [Mg(DME)3][Al(HFIP)4]2 / DME + 50 mM Mg(BOB)2 File name: 6_MgDME_Mg(DFOB)2_CV.txt Description: CV, 10 mV s-1, Mg|Mg|Au, 0.25 mol dm-3 [Mg(DME)3][Al(HFIP)4]2 / DME + 50 mM Mg(DFOB)2 File name: 6_MgDME_Mg(TFSI)2_CV.txt Description: CV, 10 mV s-1, Mg|Mg|Au, 0.25 mol dm-3 [Mg(DME)3][Al(HFIP)4]2 / DME + 50 mM Mg(TFSI)2 File name: 6_MgDME_MgTHFBHFIP_CV.txt Description: CV, 10 mV s-1, Mg|Mg|Au, 0.25 mol dm-3 [Mg(DME)3][Al(HFIP)4]2 / DME + 50 mM [Mg(THF)6][B(HFIP)4]2 File name: 6_MgDME_MgTHFBHFIP_PEIS.txt Description: PEIS between CV cycles, Mg|Mg|Au, 0.25 mol dm-3 [Mg(DME)3][Al(HFIP)4]2 / DME + 50 mM [Mg(THF)6][B(HFIP)4]2 File name: 6_MgDME_PEIS.txt Description: PEIS between CV cycles, Mg|Mg|Au, 0.25 mol dm-3 [Mg(DME)3][Al(HFIP)4]2 / DME File name: 6_MgTHFBHFIP_11B NMR.txt Description: 11B NMR of [Mg(THF)6][B(HFIP)4]2 in MeNO2 File name: 6_MgTHFBHFIP_19F NMR.txt Description: 19F NMR of [Mg(THF)6][B(HFIP)4]2 in CDCl3 File name: 6_MgTHFBHFIP_1H NMR.txt Description: 1H NMR of [Mg(THF)6][B(HFIP)4]2 in CDCl3 File name: 6_MgTHFBHFIP_PXRD.txt Description: PXRD of [Mg(THF)6][B(HFIP)4]2 File name: 6_NaDFOB_PXRD.txt Description: PXRD of NaDFOB File name: AlDME_HFIP.CIF Description: Crystal structure of [Al(DME)(HFIP)3] grown in CDCl3 File name: AlTHF_HFIP.CIF Description: Crystal structure of [Al(THF)(HFIP)3] grown in CDCl3 File name: LiTHF_AlOtBuF.CIF Description: Single crystal X-ray diffraction data of [Li(THF)4][Al(OtBuF)4] File name: Mg15C5_AlHFIP.CIF Description: Crystal structure of [Mg(κ5-15-crown-5)(Al(HFIP)3)3] grown during the reaction / layering with n-hexane File name: MgTHF_AlHFIP.CIF Description: Crystal structure of [Mg(THF)6][Al(HFIP)4]2 grown in a 1 mol dm-3 solution in THF File name: MgTHF_BHFIP.CIF Description: Crystal structure of [Mg(THF)6][B(HFIP)4]2 grown in a 1 mol dm-3 solution in THF Date of data collection: 2021 TO 2025 Date that the file was created: MARCH, 2025