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The formation of the REE(III)-Ni(II) heterometallic complexes with compartmental Schiff bases [(NiQ)nLnL3] in solutions NiQ – LnL3·nH2O (Q2- = acacen2-, salen2-, mosalen2-; Ln = La, Eu, Lu; L- = NO3 -, CH3COO-, (CH3)3COO-; n = 1, 2) was studied by ESI- and LDI-MS. Composition and thermal behavior of solid Ln(III)-Ni(II) heteronuclear complexes (Ln = La, Nd, Sm) isolated from these solutions were analyzed. The role of anions L- in intermolecular interactions was studied on examples of [(Ni(mosalen))Sm(NO3)3](H2O)0.2, [(Ni(mosalen))Sm(NO3)2(CH3COO)](C2H5OH) and [Ni(mosalen)Sm(tBuCOO)3](C2H5OH)2.5 crystal structures.