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[Display omitted] • A series of "Dy(hfa) 3 ∙glyme" adducts have been prepared through a one-pot reaction and the relationship between the coordination framework and the magnetic and luminescent properties has been deeply investigated. • Both investigations point to a diverse behavior that can be related to differences in the Dy coordination sphere. • The magnetic measurements indicate that all the three derivatives show slow magnetic relaxation in zero field, and a Raman dominant path is evident from the temperature dependence of the relaxation time measured in-field. • All the "Dy(hfa) 3 ∙glyme" samples show an interesting sharp yellow emission around 545 nm, that is more than 70% of the total emission in the visible range. Dysprosium β-diketonate compounds have recently gained a lot of attention due to their intriguing multifunctional properties. In this paper, a series of "Dy(hfa) 3 •glyme" adducts have been prepared through a one-pot reaction, in dichloromethane, from dysprosium (III) acetate monohydrate, hexafluoroacetylacetone and glyme [Hhfa = 1,1,1,5,5,5-hexafluoroacetylacetone, glyme = bis-(2-methoxyethyl)ether, 2,5,8,11-tetraoxadodecane, 2,5,8,11,14-pentaoxapentadecane]. Based on the length of the polyether, various coordination frameworks have been obtained going from a mononuclear [Dy(hfa) 3 •diglyme] adduct, to a polymeric chain system for the [Dy(hfa) 3 •2H 2 O•triglyme], and an ionic structure for the [Dy(hfa) 2 •tetraglyme]+[Dy(hfa) 4 ]−. The relationship between the coordination framework in the "Dy(hfa) 3 •glyme" series and the magnetic and luminescent properties has been deeply investigated. [ABSTRACT FROM AUTHOR]