We report synthesis of new single-source heterometallic precursors [NaLn(TFA)(4)(diglyme)] (Ln = Y, Er, Tm, Yb; TFA = trifluoroacetate), which decompose in 1-octadecene at significantly low temperature, without using any surfactant or capping reagent, to give sub-50 nm particles of cubic and/or hexagonal NaYF(4) : Yb(3+), Er(3+)/Tm(3+) materials forming well-dispersed colloidal solutions in dichloromethane and exhibiting green/blue upconversion luminescence.