本文分兩個部分，第一部分利用多牙不對稱三酮基配基H2pppt (H2pppt = 1-(phenyl)-5-(pyridin-2-yl)pentane-1,3,5-trione)與過氯酸鈷、醋酸鎳與醋酸鑭系反應合成一系列第三週期過渡金屬與鑭系金屬的混金屬多核團簇[LnIII2CoII(pppt)2(μ2-OAc)2(OAc)2(MeOH)4] (LnIII = Gd(1·Gd), Tb(2·Tb), Dy(3·Dy))和[DyIII2NiII(pppt)2(μ2-OAc)2(OAc)2(MeOH)4](4·Dy)。以單晶X 光繞射鑑定其結構為兩個pppt2-、兩個μ2-OAc-、兩個OAc-以及兩個配位甲醇所形成的三核直線型無結晶溶劑之錯合物。直流磁化率的測量在低溫下出現驟升現象顯示分子內金屬間鐵磁性作用的存在。交流磁化率的測量顯示出3·Dy 與4·Dy 在無外加磁場下的磁緩現象，其磁異向能(Ueff)分別為166.6 K 與26.2 K。另於外加磁場下，4·Dy 則相較於零場之下表現更大的磁異向能(Ueff)為167.5 K。
第二部分是利用銅(II)金屬以及鑭系(III)金屬離子與三酮配基形成四銅二
鑭系金屬的六核團簇[LnIII2CuII4(L)4(μ4-O)(μ2-OAc)2(μ2-Cl)(MeOH)2]Cl(LnIII = Gd(5·Gd), 與Dy(6·Dy))，並以X 光繞射鑑定其結構為四個pppt2-、一個μ4-O、兩個μ2-OAc-、一個Cl-與兩個甲醇所形成的六核蹺蹺板型錯合物。直流磁化率在低溫表現驟升的行為顯示有分子內金屬間的鐵磁性作用存在。交流磁化率的測量顯示出6·Dy 在有無外加場下皆於低溫出現拖尾現象，利用Bartolomé 公式求出其磁異向能(Ueff)為9.30K。

This work contains two parts. For the first part, a series of heterometallic clusters [LnIII2CoII(pppt)2(μ2-OAc)2(OAc)2(MeOH)4] (LnIII = Gd(1·Gd), Tb(2·Tb), Dy(3·Dy)) and [DyIII2NiII(pppt)2(μ2-OAc)2(OAc)2(MeOH)4] (4·Dy), which are synthesized by using polydentate, unsymmetrical triketonate ligand to react with cobalt(II)
perchlorate, nickel(II) acetate and lanthanide(III) acetate are reported. Single-crystal X-ray diffraction studies show that the structures are bridged by two pppt2 ligand and acetate group to form a linear type metal core without lattice solvent. Direct current magnetic susceptibilities measurements show the existence of ferromagnetic interactions at lower temperature. The ac susceptibility measurement shows that 1· Gd and 2·Tb have no maximum signal was observed. Complexes 3·Dy and 4·Dy show strong out-of-phase component at zero dc field and the energy barrier were determined to be 166.6 and 26.2 K as fitted to Arrhenius Law. Under 1000 Oe applied field, the energy barrier of 4·Dy is found to be 167.5 K.
For the second part, we replace CoII and NiII as CuII ion to react with triketonate ligand and lanthanide salt and obtain two LnIII2CuII4 complexes, which are found to be isostructural. The hexanuclear complexes are bridged by four triketonate ligands and form a seesaw type metal core shell. Direct current magnetic susceptibilities measurements show the existence of ferromagnetic interactions at lower temperature. The ac susceptibility measurements show tailing signal of 6·Dy under both zero and external dc field. The energy barrier are found to be 9.30 K by fitting with Bartolomé equation.

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