Manicum, Amanda-Lee EzaSchutte-Smith, MarietjieMalan, Frederick P.Visser, Hendrik Gideon2024-10-172024-10-172022-05-090022-2860https://doi.org/10.1016/j.molstruc.2022.133278https://hdl.handle.net/20.500.14519/863Re(I) tricarbonyl complexes, with coordinated β-diketones, are the center of attention as they form part of a library of promising cancer therapeutic and diagnostic agents. In this study, we present three new Re(I) crystal structures. {fac [Re(Benzac)(CO)3(PCy3)] (4), fac-[Re(Tfaa)(CO)3(PCy3)] (5), and fac-[Re(Hfaa)(CO)3(PCy3)] (6); benzoylacetone = Benzac; trifluoroacetylacetone = Tfaa and hexafluoroacetylacetone = Hfaa; PCy3 = tricyclohexylphosphine}. The three reported complexes were synthesized with ease and good yield, involving the "2 + 1" mixed ligand approach. The complexes were characterized using analytical tools: IR, NMR, UV/Vis, single-crystal X-ray diffraction. The Tolman cone angles (θ) were calculated as 141.93°, 148.77°, and 149°; and compared to the Equivalent cone angles obtained from DFT calculations. These were 131.25°, 134.34°, and 134.28° for (4), (5), and (6), respectively. The DFT analysis observed that the Re-P bond distances decrease as the number of electron-withdrawing groups (CF3) on the β-diketonato ligands increase. In general, the theoretical and experimental Re-P and Re-OOO bond distances compared well among the complexes, with the most significant deviation occurring for 4 (relative differences of 0.055 A˚ (Re-P) and 0.015 A˚ (average Re-O)). Hirshfeld surface analysis was used to obtain the fingerprint plots, and the Hirshfeld surfaces were mapped with dnorm for 4, 5, and 6.1-13 PagesenAttribution-NonCommercial-ShareAlike 4.0 Internationalhttp://creativecommons.org/licenses/by-nc-sa/4.0/Re(I) tricarbonylβ-diketonestricyclohexylphosphineTolman cone angleDFT calculationsArticle