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A new binuclear cobalt(Ⅱ) complex,[Co2(C10H6NO2)2(C12H8N2)2(N3)2]·H2O (1,C10H6NO2-:isoquinoline-1-carboxylate,C12H8N2:1,10-phenanthroline (phen);N3-:azide),has been synthesized though a mixed-solvothermal method using the pentanol and distilled water as solvent.The complex was characterized by elemental analysis,IR spectrum and single-crystal X-ray diffraction.It crystallizes in triclinic system,space group P(1) with Z =2,a =1.777(5),b =11.815(5),c =17.141(7) (A),α =74.496(6)°,β =70.537(6)°,γ =67.861(6)°,V=2055.4(14) (A)3,Mr=922.66,Dc=1.491 g/cm3,λ =0.71073 (A),μ =0.870 mm-1,F(000) =942,R =0.0455 and wR =0.1147 for 4960 observed reflections with I ＞ 2σ(I) and S =1.129.Its molecular structure is constructed by two Co2+ cations,two chelating phen ligands,two chelating isoquinoline-1-carboxylate ligands,two bridging linear azide anions and two uncoordinated half-occupied water molecules.The 3-D supramolecular network results from the multiple hydrogen bonds and π-π stacking interactions among three types of ligands.More importantly,its thermal stability,luminescent properties and magnetic properties have also been studied in detail.