摘要
Two novel supramolecular complexes,[M4L12]·（HPO4）·（PO4）2（L = 2,2＇-dibenzi-midazole,M = Co and Ni） were synthesized by the hydrothermal method and characterized by elemental analysis,IR,UV,and TG-TGA,and the crystal structures were determined by single-crystal X-ray diffraction.The results showed that both of them belong to the cubic system and space group I 4 3d.Crystal parameters of C168H121Co4N48O12P3（1）：a = b = c = 2.5104（6） nm,V = 15.820（7） nm3,Mr = 3332.75,Z = 4,Dc = 1.399 Mg/m3,μ = 0.521 mm-1,F（000） = 6852,S = 1.011,the final R = 0.0248 and wR = 0.0663 for 2120 observed reflections（I 2σ（I）） and R = 0.0315 and wR = 0.0706 for all data.Crystal parameters of C168H121Ni4N48O12P3（2）：a = b = c = 2.4977（5） nm,V = 15.581（5） nm3,Mr = 3331.87,Z = 4,Dc = 1.420 Mg/m3,μ = 0.587 mm-1,F（000） = 6868,S = 1.074,the final R = 0.0443 and wR = 0.1364 for 1774 observer reflections（I 2σ（I）） and R = 0.0647 and wR = 0.1492 for all data.Each of them consisted of four M（II） cations,twelve 2,2＇-dibenzimidazole ligands,one monohydrogen phosphate anion and two phosphate anions in the single cell.The central M（II） cation,coordinated with six alkaline nitrogen atoms from three 2,2＇-dibenzimidazole ligands,displayed the expected distorted-octahedral geometry.The 3D supramolecular system was formed by the hydrogen bond N-H...O and π-π stacking interaction between neighboring single cells.Complex 1 showed two irreversible single-electron reduction processes of the central metal ion at-0.06 and-0.42 V in DMF solution.
Two novel supramolecular complexes,[M4L12]·（HPO4）·（PO4）2（L = 2,2＇-dibenzi-midazole,M = Co and Ni） were synthesized by the hydrothermal method and characterized by elemental analysis,IR,UV,and TG-TGA,and the crystal structures were determined by single-crystal X-ray diffraction.The results showed that both of them belong to the cubic system and space group I 4 3d.Crystal parameters of C168H121Co4N48O12P3（1）：a = b = c = 2.5104（6） nm,V = 15.820（7） nm3,Mr = 3332.75,Z = 4,Dc = 1.399 Mg/m3,μ = 0.521 mm-1,F（000） = 6852,S = 1.011,the final R = 0.0248 and wR = 0.0663 for 2120 observed reflections（I 2σ（I）） and R = 0.0315 and wR = 0.0706 for all data.Crystal parameters of C168H121Ni4N48O12P3（2）：a = b = c = 2.4977（5） nm,V = 15.581（5） nm3,Mr = 3331.87,Z = 4,Dc = 1.420 Mg/m3,μ = 0.587 mm-1,F（000） = 6868,S = 1.074,the final R = 0.0443 and wR = 0.1364 for 1774 observer reflections（I 2σ（I）） and R = 0.0647 and wR = 0.1492 for all data.Each of them consisted of four M（II） cations,twelve 2,2＇-dibenzimidazole ligands,one monohydrogen phosphate anion and two phosphate anions in the single cell.The central M（II） cation,coordinated with six alkaline nitrogen atoms from three 2,2＇-dibenzimidazole ligands,displayed the expected distorted-octahedral geometry.The 3D supramolecular system was formed by the hydrogen bond N-H...O and π-π stacking interaction between neighboring single cells.Complex 1 showed two irreversible single-electron reduction processes of the central metal ion at-0.06 and-0.42 V in DMF solution.
基金
Project Supported by the Science & Technology Innovation Foundation of Henan Province (No. 092102310309)
