The preparations of the N,N-dialkylcarbamato complexes with analytical formulae [Ln(O 2 CNR 2 ) 3 ] (Ln = Pr, Nd, Eu, Gd, Ho, Er, Yb, Lu, R = iPr; Ln = Nd, Eu, Gd, R = Bu; Ln = Nd, R = Et), using [LnCl 3 (ether) x ] (ether = THF or dimethoxyethane, DME), NHR 2 , and CO 2 are reported. X-ray diffraction of the diisopropylcarbamato derivatives, including a reinvestig-