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A new sulfonylcalixarene-based coordination container 1 was designed and synthesized from the self-assembly reaction of p-tert-butylsulfonylcalix[4]arene (TBSC),Co(Ⅱ) ion,and 2,6-naphthalenedicarboxylic acid (NDC).It crystallizes in tetragonal system,space group I4/m with a =b =30.9119(19)(A),c =43.565(3) (A),V=41628(6) (A)3,Dc =0.731 g/cm3,Mr =9162.36,C384H348Co24O126S24,Z =2,F(000) =9384,μ =0.566 mmn-1,the final GOOF =1.027,R =0.0987 and wR =0.2474 for 7240 observed reflections with I ＞ 2σ(I).Structural analyses indicate that 1 adopts an edge-directed octahedral geometry and consists of six TBSC-supported Co4 tetranuclear units locating on the vertices and twelve NDC bridging ligands occupying the edges.The new compound exhibits outstanding performance for the C2 hydrocarbons separation over CH4.