We adapted literature salt metathesis protocols for the synthesis of the dinuclear Sm(II) complex [Sm{P(SiMe3)2}{μ-P(SiMe3)2}3Sm(THF)3] from [SmI2(THF)2] and 2 eq. K{P(SiMe3)2} in THF to prepare 1-Ln and 2-Yb from parent [LnI2(THF)2] (Ln = Sm, Eu, Yb) and 2 or 3 eq. of K{P(SiMe3)2} in diethyl ether (Scheme 1). Reactions were initiated at -78 °C and reaction mixtures were allowed to stir for 1 hr at this temperature before allowing to warm to room temperature briefly, before volatiles were removed in vacuo and the products extracted into pentanes. Under these conditions recrystallization from saturated solutions reproducibly gave poor isolated yields of 1-Ln (ca. 15%); 2-Yb was only characterized by single crystal XRD (see below). These 'ate' complexes were the only Ln-containing complexes that we were able to identify in the reaction mixtures, though if either excess pyridine or stoichiometric 18-crown-6 is added before work-up then the respective solvated adducts 3-Ln and 4-Ln form, with concomitant loss of K{P(SiMe3)2} incomplete combustion arising from carbide formation, which is a common feature for highly air-and moisture-sensitive complexes. For 3-Ln the hydrogen and nitrogen values obtained are consistent with the loss of one bound pyridine upon drying samples in vacuo, with low carbon values again assigned to carbide formation; the low carbon and hydrogen values observed in elemental analysis results of [Yb(PPh2)2(THF)4] was previously assigned to the partial loss of THF in vacuo. The ATR-IR spectra of 1-Ln, 3-Ln and 4-Ln show largely overlapping absorption bands for each separate family, indicating that the bulk samples show similar features in the solid state.