| Construct of complexes with novel architectures and excellent properties has become ahotspot in the field of coordination chemistry, structural chemistry and materials chemistry.Azido anion can coordinate to more than one metal center, displaying multiple bridgecoordination modes which can mediate differernt magnetic coupling effectively. With theassistance of appropriate ligands,synthesis of novel heterometallic complexes may beadvanced material, if we can combine with a variety of metals of different merits, such asfavorable optical, electrical and magnetism properties of3d metal and larger radius andanisotropy of4f metal. Therefor, the great interest of the design and synthesis of metal-azidocompounds and heterometallic complexes is increasing radically. In this work, one-stepsolvothermal route overcomes the difficulty in systhesis through decreasing reaction steps.The main points are summarized as follows:1. Azido chosen as the main bridge ligand reacts with transition metal salts under thesolvothermal condition with the assistance of other five coligands, respectively, then eightunprecedented metal-azido compounds are obtained. Complex1reveals a3Dcoordination network by azido with EE mode. Complex2shows a2D herringbone layerstructure through azido with μ1,1(EO)and μ1,1,3modes. Howerer, complex3-8have a1Dchain structure.2. Six novel heterometallic complexes are obtained by solvothermal reaction of threeappropriate ligands and different metals, respectively. Both3d-4f heterometalliccomplexes9and10built by transition metal (Co and Ni) and lanthanide metal metal (Tband Dy) together, revealing0D cluster structure. Complex12is also a3d-4f (Cu-Ce)heterometallic complex with a highly symmetrical3D coordination network. Complexes13and14are two isostructural main group (Na)-transition (Co and Ni) heterometalliccomplexes.3. Magnetic susceptibility measurement reveals dominant antiferromagnetic coupling existbetween the MnIIions in1. |