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A three-dimensional (3D) zinc metal-organic framework (MOF),Zn4(μ4-O)(bcd)3 (complex 1) has been synthesized by using 1-[bis(4-carboxylphenyl)methyl]-1,3-diazole (H2bcd) and Zn(NO3)2·6H2O under hydrothermal conditions.The structure has been determined by single-crystal X-ray diffraction analyses and further characterized by elemental analyses,IR spectra,powder X-ray diffraction (PXRD) and thermogravimetric analyses (TGA).Single-crystal X-ray diffraction analyses reveal that complex 1 crystallizes in trigonal system,space group R(3) with a =23.0521(6),b =23.0521(6),c =15.3326(6) (A),γ =120°,V =7056.2(4) (A)3,Z =6,C54H36N6O13Zn4,Mr=1242.37,Dc.=1.754 g/cm3,F(000) =3756,the final R =0.0411 and wR =0.1007 for 2743 observed reflections (Ⅰ ＞ 2σ(Ⅰ)).Complex 1 consists ofa 3D network constructed by four nuclear clusters Zn4(μ4-O)(COO)6N3 and the bcd2-ligand.Interestingly,1 exhibits strong luminescent emission in solid state at room temperature and could be used as a qualitative fluorescence enhancing sensor for ammonia vapor in air.