READ ME File For 'Synthesis and properties of metal trifluoride complexes with amide-functionalised tacn macrocycles and radiofluorination of [GaF3(L1)] by 18F/19F isotopic exchange' Dataset DOI: 10.5258/SOTON/D3162 Date that the file was created: October, 2025 ------------------- GENERAL INFORMATION ------------------- ReadMe Author: Charley O'Callaghan, University of Southampton ORCID ID 0000-0002-1839-0591 Date of data collection: 06/2021 - 10/2024 Information about geographic location of data collection: University of Southampton, Southampton, UK; St Thomas' Hospital, London, UK Related projects: EPSRC/520009101 -------------------------- SHARING/ACCESS INFORMATION -------------------------- Licenses/restrictions placed on the data, or limitations of reuse: CC-BY (no restrictions, full citation required where appropriate) Recommended citation for the data: C. O'Callaghan, V. K. Greenacre, R. P. King, J. Grigg, J. M. Herniman, G. McRobbie, G. Reid, Dalton Trans., 2024, 53, 14897-14909 This dataset supports the publication: AUTHORS: Charley O'Callaghan, Victoria K. Greenacre, Rhys P. King, Julian Grigg, Julie M. Herniman, Graeme McRobbie and Gillian Reid TITLE: Synthesis and properties of metal trifluoride complexes with amide-functionalised tacn macrocycles and radiofluorination of [GaF3(L1)] by 18F/19F isotopic exchange JOURNAL: Dalton Transactions PAPER DOI IF KNOWN: 10.1039/D4DT02074J Links to other publicly accessible locations of the data: https://www.rsc.org/suppdata/d4/dt/d4dt02074j/d4dt02074j1.pdf Links/relationships to ancillary or related data sets: 10.5258/SOTON/D3321 (in relation to Charley O'Callaghan's thesis), crystal structures uploaded to the CCDC with reference numbers 2355936–2355941. -------------------- DATA & FILE OVERVIEW -------------------- This dataset contains: One PDF document containing: all spectra related to compounds described in the text (L1, L2, L3, [AlF3(L1)], [GaF3(L1)], [FeF3(L1)], [AlF3(L2)], [GaF3(L2)], [FeF3(L2)], [AlF3(L3)], [GaF3(L3)], [FeF3(L3)] - IR, 1H NMR, 13C{1H} NMR, 135-DEPT 13C{1H} NMR, 19F{1H} NMR, 27Al NMR, 71Ga NMR, HR ESI+ MS, ESI+ MS) and; UV-HPLC chromatogram of the reference [GaF3(L1)] compound and UV- and radio-HPLC chromatograms of the optimised crude and purified [Ga18F19F2(L1)] compound. Additional related data collected that was not included in the current data package: cif files and checkcif files which are accessible via the CCDC with reference numbers 2355936–2355941. -------------------------- METHODOLOGICAL INFORMATION -------------------------- Description of methods used for collection/generation of data: Infrared spectra were recorded as Nujol mulls between CsIplates using a PerkinElmer Spectrum 100 spectrometer over the range 4000–200 cm−1. 1H, 13C{1H}, 19F{1H}, 27Al and 71GaNMR spectra were recorded using a Bruker AV400 spectrometer and referenced to SiMe4 via the residual solvent resonance (1H and 13C), external CFCl3(19F), aqueous [Al(H2O)6]3+ (27Al) and aqueous [Ga(H2O)6]3+ (71Ga), respectively. Low resolution mass spectrawere obtained in MeOH by positive ion electrospray MS using a Waters (Manchester, UK) Acquity TQD tandem quadrupolemass spectrometer. Samples were introduced to the massspectrometer via an Acquity H-Class quaternary solvent manager (with TUV detector at 254 nm, sample and column manager). Ultra-high performance liquid chromatography wasundertaken using Waters BEH C18 column (50 mm × 2.1 mm1.7 μm). Gradient elution from 20% acetonitrile/80% water(0.2% formic acid) to 100% acetonitrile (0.2% formic acid) was performed over five min at a flow rate of 0.6 mL min−1. High resolution positive ion electrospray mass spectra were recordedusing a MaXis (Bruker Daltonics, Bremen, Germany) time offlight (TOF) mass spectrometer. Samples were infused into the ion source using a syringe driver at a constant flow rate of 3 μLmin−1. Duplicate microanalyses were undertaken at Medac Ltd. Methods for processing the data: IR and NMR spectroscopic data analysed using ACD Labs Spectrus software; mass spectrometry data analysed using the open access RemoteAnalyzer (low resolution) or PDF report (high resolution). Environmental/experimental conditions: All methods under atmospheric conditions. Data collected at room temperature (NMR collected at 298 K). People involved with sample collection, processing, analysis and/or submission: Charley O'Callaghan, Victoria K. Greenacre, Rhys P. King, Julie M. Herniman, Graeme McRobbie.