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以MoO3, H2MoO4, Ni(OAc)2·6H2O 和 1, 10-邻菲咯林(1, 10-phen)为原料, 用水热法合成出了八钼氧酸盐支撑的镍-邻菲咯啉配合物[{Ni(phen)2}2(ξ?Mo8O26)]. 化合物的晶体属于单斜晶系P21/n空间群, a = 1.2952(2), b = 1.6659(10), c = 1.3956(12) nm, ? =106.273(8)°, V = 2.8906(5) nm3, Z = 2. 由5604个可观测衍射(I ＞2? (I ))用于精修所有的结构参数, 得一致性因子R1 = 0.0414, WR2 = 0.0815. 结构测定结果表明, 化合物中的八钼氧酸盐具有新奇的前所未有的结构类型(称之为?-isomer), 其特点是它由Mo6O6环和环中两侧处于戴帽位置的2个MoO6八面体组成. Mo6O6环含有2个八面体配位的MoⅥ原子和4个三角双锥配位的MoⅥ原子. 每个?-[Mo8O26]4?结构单位通过Mo6O6环中八面体配位的Mo原子的端氧和相邻的三角双锥配位的Mo原子的端氧与2个[Ni(phen)2]2+单位相键合. 测定了化合物的IR和UV-Vis光谱, 并用EHMO方法对其电子结构进行了研究.
The octamolybdate supported nickel-phenanthroline was synthesized by hydrothermal method using MoO3, H2MoO4, Ni (OAc) 2.6H2O and 1,10-phenanthroline (1,10-phen) as starting materials The complex belongs to the monoclinic P21 / n space group, a = 1.2952 (2), b = 1.6659 (10), c = 1.3956 12) nm,? = 106.273 (8) °, V = 2.8906 (5) nm3, Z = 2. The 5604 observable diffractions (I> 2? Sexual factors R1 = 0.0414, WR2 = 0.0815. The results of the structure determination showed that the octamolybdate in the compound has a novel and unprecedented structure type (called? -isomer), which is characterized in that it consists of Mo6O6 rings and two rings MoO6O6 ring contains two octahedral Mo VI atoms and four triangular double cone Mo atoms.Each of the [Mo8O26] 4? Units are formed by Mo6O6 The terminal oxygen of the Mo atom in the octahedral coordination ring and the terminal oxygen of the Mo atom coordinated by the adjacent triangular bipyramids are bonded to two [Ni (phen) 2] 2+ units. The IR and UV-Vis spectra, and its electronic structure was studied by EHMO method.