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In this paper, two 3D anionic metal-organic frameworks, [(CH3CH2)2NH2]·[Zn(BTC)1/3(PyC)]·1/2CH3CN·2H2O (NKU-102) and [(CH3CH2)2NH2]·[Zn2(BTC) (PyC)]·1.5H2O·DEF (NKU-103), were constructed from the same reaction system at different temperature. Though both are of anionic framework, NKU-102 possesses a sealed 3D framework based on octahedral cage and shows negligible adsorption capacity of organic dyes, whereas NKU-103 features an open triangular microchannel surrounded by two types of helical chains, and thus exhibits outstanding size-selective adsorption toward small cationic organic dyes. [ABSTRACT FROM AUTHOR]