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Fourteen Ni/Co-Ln heterometallic coordination polymers were successfully synthesized. All CPs are bridged into the 3D network structure by 2,3-pydc2- and ox2- and exhibit characteristic emission bands of the corresponding Ln(III) ion. [Display omitted] • A series of heterometallic NiII/CoII-LnIII coordination polymers have been synthesized by using pyridine-2,3-dicarboxylic acid as main ligand. • They exhibit characteristic luminescence of Ln(III) ions. • NIR emission bands of Ln(III) ions in some polymers present shift, split and broad under the double influence from the crystal field and Ni(II) or Co(II) ions. Fourteen isomorphic heterometallic coordination polymers (CPs) with general formulas of {[LnM(2,3-pydc) 2 (ox) 0.5 (H 2 O) 3 ]·3H 2 O} n (M = Ni, Ln = Pr 1 , Nd 2 , Sm 3 , Eu 4 , Gd 5 , Tb 6 , Dy 7 ; M = Co, Ln = Pr 8 , Nd 9 , Sm 10 , Eu 11 , Gd 12 , Tb 13 , Dy 14 ; 2,3-pydc2– = fully deprotonated pyridine-2,3-dicarboxylic acid, ox2– = fully deprotonated oxalic acid) have been synthesized by hydrothermal methods. All the CPs crystallize in triclinic P -1 space group and exhibit a 3D network formed by 2,3-pydc2– and ox2– bridging Ln(III) and Ni(II)/Co(II) ions. Meamwhile the room temperature photoluminescent properties have been explored. Except for CPs 5 and 12 , the other CPs exhibit characteristic luminescence of Ln(III) ions. [ABSTRACT FROM AUTHOR]