本論文是以中溫水熱反應合成了四個新穎結構的鋅雙膦酸鹽及兩個鈷草酸雙膦酸鹽。如下所列: [(CH3)2NH(CH2)3NH(CH3)2][Zn3(Hedp)2]•H2O………………………………A1 [(CH3)2NH(CH2)2NH(CH3)2][Zn3(Hedp)2]•H2O………………………………A2 [(CH3)2NH(CH2)4NH(CH3)2][Zn2(Hedp)1.5]•0.5H2O…………………………A3 [(CH3)2NHCH2NH(CH3)2][Zn3(Hedp)2]•H2O………………………………A4 (NH3C6H10NH3)[Zn3(Hedp)2(H2O)](C2O2H6)0.5•2H2O………………………A5 [(CH3)2NH(CH2)3NH(CH3)2][Co(HedpH2)(C2O4)]……………………………B1 [(CH3)2NH(CH2)2NH(CH3)2] [Co(HedpH2) (C2O4)]…………………………B2 Hedp = (PO3)(CH3)C(OH)(PO3);其中A2與A1為等結構化合物。所有的化合物均由單晶 X 光繞射分析鑑定出結構。產物的晶相與純度可由粉末X光繞射證實。化合物中的 C、N、H 比例由元素分析加以確認。結構中的特殊官能基可用 IR 判定。並利用 TGA 配合調控的變溫粉末 X 光繞射圖譜,探討化合物的熱性質。A1 ~ A4為三維結構,多樣的孔道形式說明了雙膦酸為一個強力的配位基。A5為層狀結構,層與層之間有被質子化的有機胺,結晶水,與乙二醇分子。B1與B2為首次被合成出來的混合配位基鈷草酸雙膦酸鹽,都是一維長鏈結構。A1,A3,與A4具有相似的發光性質。而B1具有反鐵磁的特性。 This thesis describes the hydrothermal synthesis and structural characterization by single-crystal X-ray diffraction of four novel Zinc diphosphonates and two Cobalt Oxalatodiphosphonates. All the compounds are listed as following: [(CH3)2NH(CH2)3NH(CH3)2][Zn3(Hedp)2]•H2O………………………………A1 [(CH3)2NH(CH2)2NH(CH3)2][Zn3(Hedp)2]•H2O………………………………A2 [(CH3)2NH(CH2)4NH(CH3)2][Zn2(Hedp)1.5]•0.5H2O…………………………A3 [(CH3)2NHCH2NH(CH3)2][Zn3(Hedp)2]•H2O………………………………A4 (NH3C6H10NH3)[Zn3(Hedp)2(H2O)](C2O2H6)0.5•2H2O………………………A5 [(CH3)2NH(CH2)3NH(CH3)2][Co(HedpH2)(C2O4)]……………………………B1 [(CH3)2NH(CH2)2NH(CH3)2] [Co(HedpH2) (C2O4)]…………………………B2 ,where Hedp represents 1-hydroxyethylidenediphosphonate. A2 and A1 are isostructural. A1 show a 2D channel containing three kinds of 12 member rings and a interesting cage in 3D framework. A3 has a narrow 20 member ring channel along c axis which containing 16, 8, and 4 member rings outside. A4 is a 3D framework stacked by ladder-like layer structure which composited by 16 member rings. A5 exhibit interesting layer structure, build up from the [Zn3(hedp)2]n double chains and mixed coordinated Zinc polyhedrons. Both B1 and B2 contain [Co(HedpH2)(C2O4)]n infinite chains. Three four zinc diphosphonates possessing ultraviolet fluorescence, and high thermal stability. Cobalt Oxalatodiphosphonates shows an antiferromagnetic behavior between 50 ~ 300K.