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A new heterometallic complex of CoII and NdIII with phenathroline [Co(Phen)3][Nd(NO3)5(H2O)][Nd(NO3)4(H2O)2]⋅H2O was synthesized for the first time by the self-assembly method. The crystal structure of the complex was determined by X-ray crystallography. The compound is an anion-cation complex and crystallizes in the monoclinic space group P21/n with unit cell parameters à=12.4251(4) Å, b=11.7206(3) Å, c=36.5374(12) Å, α=γ=900, β=90.581(3)0 . In the crystalline phase, the complex is in the form of a crystal hydrate with a composition of 1:1. The anionic part of the complex consists of two nitrate hydrated NdIII complexes: [Nd(NO3)5(H2O)][Nd(NO3)4(H2O)2]–, in which the coordination number of neodymium is 11 and 10, respectively. The [Co(Phen)3]3+ ion is a cationic part of the complex in which the CoII atom has a distorted CoN6 octahedral environment, bidentately coordinating three phenanthroline molecules. Due to intermolecular hydrogen bonds (N–H⋅⋅⋅O, O–H⋅⋅⋅O), a three-dimensional supramolecular architecture is formed in the crystal, in which the polymer layers are packed parallel along the crystallographic axis a. [ABSTRACT FROM AUTHOR]