Synthesis and Crystal Structure of Compound [Fe(Phen)_3][(μ-oxo)Fe_2Cl_6]DMF

The synthesis and structure of [Fe(Phen)3][(μ-oxo)Fe2Cl6]稤MF are reported. The crystal data for the compound: monoclinic, P2l /c,a =15.491(1),b = 13.217(1),c = 20.748(2)牛?= 93.83(3),V = 4239(2)?,Z = 4,Dc = 1.562g/cm3,μ(MoK)=1.44 mm-1,F(000)= 2040.0, (C39H31Cl6Fe3N7O2) and Mr = 1009.96. X-ray crystallographic studies reveal that the title compound contains complexes of [Fe(Phen)3]2+ and [Fe2(μ-oxo)Cl6]2- which consists of two [FeCl3] fragments connected by an oxo bridge,with the bond distances of Fe(3)O(1) 1.744(4) and Fe(2)O(1) 1.754(4)牛琣nd a bond angle Fe(2)O(1)Fe(3) of 162.9(3). In the [Fe2(μ-oxo)Cl6]2- complex, the two iron (Ⅲ) centres exhibit tetrahedral coordination, with the distorted tetrahedra formed by three Cl atoms and an oxo bridge. The bond lengths to the donor atoms lie in the range 2.211(1)～2.226(1)?for FeCl, and the non-bonded Fe…Fe distance is 3.459?

Synthesis and Crystal Structure of Compound [Ni(bipy)_3][(μ-oxo)Fe_2Cl_6]

The title compound [Ni(bipy)3][(-oxo)Fe2Cl6] (bipy = 2, 2?bispyridine) was synthesized and its crystal structure was determined by X-ray diffraction method. It crystallizes in monoclinic, space group P2l/c with unit cell parameters: a = 9.7085(7),b = 26.409(2), c = 14.014(1) ,?= 100.237(3), V = 3535.9(2) 3,Z = 4,C30H24Cl6Fe2N6NiO,Mr = 867.66, Dc = 1.630 g/cm3,F(000) = 1744, (MoK? = 1.824 mm-1, the final R = 0.0394 and wR = 0.0475 for 2750 observed reflections with I ≥ 2(I). The title compound contains cation of [Ni(bipy)3]2+ and anion of [(-oxo)Fe2Cl6] 2- which consists of two [FeCl3] fragments connected by an oxo bridge with the bond distances of Fe(2)O(1) 1.752(2) and Fe(1)O(1) 1.763(2) , and the bond angle of Fe(2)O(1)Fe(1) 148.6(2)? In the [Fe2(-oxo)Cl6]2- complex, the two iron(Ⅲ) centers exhibit a tetrahedral coordination with the distorted tetrahedron formed by three Cl atoms and one oxo bridge.

[Ni(bipy)_3][(μ-oxo)Fe_2Cl_6]化合物的制备与研究

标题化合物是由 [Ni(bipy) 3 ]2 +络合物与FeCl2 在MeOH、DMF及异丙醇混合溶剂中直接反应得到的 ,它可溶于水、乙醇和DMF等极性溶剂 ,不溶于乙醚 .X -射线结晶学研究表明 :标题物中含有 [Ni(bipy) 3 ]2 +和 [(μ -oxo)Fe2 Cl6]2 - 离子 ,晶胞参数 :单斜 ,P2 1 c,a=0 .970 9nm ,b =2 .6 40 9nm ,c =1.40 14nm ,β =10 0 .2 4° ,V =3.5 36nm3 ,Z =4,Dc =1.6 30g cm3 ,F (0 0 0 ) =1744 ,μ =1.82 4nm- 1 .化学实验式为 :C3 0 H2 4Cl6Fe2 N6NiO .分子量 Mr=86 7.6 6 .对标题物进行X -荧光元素分析、红外、可见吸收光谱和磁化率的研究 .