Research on coordination polymers (CPs) using 2-deoxy-d-ribose derivatives as ligands has not been documented to the best of our knowledge. Herein, the new ligand L (1,3,4-trikisisoniacyl-2-deoxy-β-d-ribopyranose) was designed and synthesized from 2-deoxy-d-ribose, and four CPs {[MnL 2Cl2]·4CH3OH}∞ (1), {[CoL 2Cl2]·4CH3OH}∞ (2), {[NiL 2Cl2]·4CH3OH}∞ (3) and {[CoL 2Br2]·4CH3OH}∞ (4) were prepared using L as the bridging ligand. Single-crystal X-ray analyses showed that the above four CPs crystallize in the trigonal space group P3121 and have the same 2D grid structures with the same 1D meso-helices and the same 3D supramolecular architectures, and each metal center bonds with four pyridyl rings to form a Δ-propeller configuration in 1–4. The same space groups, structures, and chiral types of the propellers of 1–4 suggest that L is a powerful ligand in controlling the structures and chiralities of its metal complexes. Interestingly, 3 gave weaker emission in the solid state but much stronger emission in suspension, and 2–4 showed the ability to sense Fe3+ with LODs of 2.75, 0.12, and 0.87 μM and quenching constants of 1.07 × 104, 1.67 × 104, and 3.33 × 104 M–1, respectively, and high interference resistance, indicating their potential to be used as sensitive fluorescence sensors for detecting Fe3+. The different metal centers of 1–4 should be the main factors that make them distinct in fluorescent properties and probe functions due to the similarities in compositions and structures of the four CPs.

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A pair of enantiomeric ligands, (2R,3R)‐dibenzyl‐2,3‐bis(isonicotinoyloxy)succinate ((R,R)‐L) and (2S,3S)‐dibenzyl‐2,3‐bis(isonicotinoyloxy)succinate ((S,S)‐L), are designed and synthesized. Seven copper (II) coordination polymers {[Cu((R,R)‐L)Br2(THF)] ⋅ CH3CN} n (1 a) and {[Cu((S,S)‐L)Br2(THF)] ⋅ CH3CN}n (1 b), {[Cu((R,R)‐L)Cl2(THF)] ⋅ CH3CN}n (2 a) and {[Cu((S,S)‐L)Cl2(THF)] ⋅ CH3CN}n (2 b), {[Cu((R,R)‐L)(NO3)2(CH3CN)]}n (3 a) and {[Cu((S,S)‐L)(NO3)2(CH3CN)]}n (3 b), {[Cu((R,R)‐L)2(CH3CN)2](ClO4)2 ⋅ 3CH3CN}n (4) were obtained through the assemblies with CuBr2, CuCl2 ⋅ 2H2O, Cu(NO3)2 ⋅ 3H2O, Cu(ClO4)2 ⋅ 6H2O, respectively. Single‐crystal X‐ray diffraction and circular dichroism analysis demonstrate that 1 a–3 a, 1 b–3 b have a mono chiral one‐dimensional (1D) chain‐like spiral structure, while 4 have 1D chain‐like structure whose metal centers have chiral propeller coordination environment. Ligand structure, anions and solvent systems have a regulatory effect on the formation of chiral helical structure. Further investigation has proved that 1 a can be used as circular dichroism spectrum probe for monitoring L‐/D‐cysteine and L‐/D‐penicillamine configuration and concentration in aqueous media based on ligand interchange mechanism.

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