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题配合物的合成是将金属高氯酸盐1.25毫摩溶于35毫升乙酸乙酯和15毫升乙醇-原甲酸三乙酯混合溶剂内,然后加6-氧基嘌吟(hxH)2.5毫摩(对于M~(2+))或3.75毫摩(对于M~(3+));将整个混合物回流6小时,冷至室温后,加无水乙醚15—20毫升,加微热以使体积减至约20毫升,将固体过滤分出,用乙醚30毫升洗涤,贮于真空无水CaSO_4干燥器内,所得产物含较高的氧基嘌吟与金属比(4:1或3:1),根据分析结果,分下列类型:[M(hx)(hxH)(Cl0_4)ClO_4(M=Cr,Fe),[M(hx)(hxH)_3(H_2O)]ClO_4(M=Mn,Cu,Zn),[M(hx)(hxH_2)(H_2O)(ClO_4)](M=Fe,Ni)和[Co(hx)(hxH)]ClO_4。这些新配合物皆不溶于有机溶剂。光谱表征表明高氯酸根在M=Mn~(2+),Co~(2+),Cu~(2+),Zn~(2+)配合物内皆为外界离子,而在M=Fe~(2+),Ni~(2+)配合物内则为单齿配体,在M~(3+)(Cr,Fe)配合物内,一为离子,另一为单配体。除Co为5配位外,余皆为6配位。所有这些新配合物皆以hx为桥连配体,通过N_3,N_7,形成链状聚合物。
The title complex was synthesized by dissolving 1.25 mmol of metal perchlorate in 35 ml of ethyl acetate and 15 ml of ethanol-triethyl orthoformate mixed solvent and then adding 6-oxypurine (hxH) 2.5 mmol (For M 2+) or 3.75 mmol (for M 3+); the whole mixture was refluxed for 6 hours, cooled to room temperature, and then 15-20 ml of anhydrous diethyl ether was added. Reduced to about 20 ml. The solid was separated by filtration, washed with 30 ml of ether and stored in a vacuum anhydrous CaSO 4 drier. The resulting product contained a higher ratio of oxy-purine to metal (4: 1 or 3: 1) According to the analysis results, the following types are classified: [M (hx) (hxH) (Cl0 4) ClO 4 (M = Cr, Fe), [M (hx) (hxH) 3 (H 2 O)] ClO 4 (M = Zn], [M (hx) (hxH_2) (H_2O) (ClO_4)] (M = Fe, Ni) and [Co (hx) (hxH)] ClO_4. These new complexes are insoluble in organic solvents. Spectroscopic characterization indicated that perchlorate is an external ion in the complexes of M = Mn ~ (2 +), Co ~ (2 +), Cu ~ (2 +) and Zn ~ (2+) (2 +), Ni ~ (2+) complex is a monodentate ligand, in the M ~ (3 +) (Cr, Fe) complex, one ion, the other is a single ligand. In addition to Co for the 5 coordination, I are more than 6 coordination. All of these new complexes are hx bridged ligand, through N_3, N_7, forming a chain polymer.