| In this thesis, numerous Mo-O cluster compounds synthesized by hydrothermal technique in recent years are summarized and a number of typical structures among them are analyzed. Based on this, two inorganic-organic hybrid compounds, [{Cu(2,2'-bipy)2}2Mo8O26] and [{Cu(4,4'-bpy)}2Mo2O7], have been prepared from raw materials including molybdenum oxide under basic conditions by means of the medium-temperature hydrothermal technique. The two crystals have been structurally characterized by single crystal X-ray diffraction. The structure of [{Cu(2,2'-bipy)2}2Mo8O26J consists of a P-[Mo8O26]4 polyanion coordinated to two {Cu(2,2'-bipy)2}2+ complex cations via bridging oxo groups. The copper centers exhibit a distorted {CuN4O2} octahedral coordination geometry. This compound presents the first example of new hybrid materials constructed by the coordination of an octamolybdate with transition metal complex cations via bridging oxygen atoms. The spectral and thermal properties of the above complex have been determined by ESR% UV/DRS> FT-H^ Rama^ TG^ ICP-AES elemental analysis, which confirm the accuracy of the crystal structure solution.The reaction mechanism of the hydrothermal synthesis is concluded and the other hybrid compound [{Cu(4,4'-bpy)}2Mo2O7] is obtained. The structure of [{Cu(4,4'-bpy)}2Mo2O7] consists of linear {Cu(4,4'- bpy)}+chains linked through [Mo2O7]2 clusters into a double chained ribbon. The dimolybdate subunit consists of corner-sharing {MoO4} tetrahedra, each of which employs an oxo-group to bond to a copper center of two adjacent and parallel {Cu(4,4'-bpy)}nn+ chains. Consequently, the Cu(I) sites of[{Cu(4,4'-bpy)}2 Mo2O7] exhibit 'T'-shaped {CuN2O} coordination geometry. The resulting 30-membered ring structure produces an oval projection when viewed parallel to the b axis. |
