二个含N-取代水杨基Schiff碱配体的镍配合物的合成和晶体结构
Syntheses and Crystal Structures of Two Nickel Complexes with N-Substituted-Salicyl Ligand
作者单位
陈小华 福州大学中心实验室福州 350002 
刘世雄 福州大学中心实验室福州 350002 
摘要: 合成了二个N-取代水杨基Schiff碱的Ni(Ⅱ)配合物[Ni2(dsh)(C5H5N)6]·2C5H5N (H4dsh=1,2-disalicyloylhydrazine) (1)和Ni(spmbh)(C5H5N) (H2spmbh=N-salicylaldehyde-N-(4-methoxybenzoyl) hydrazone) (2)。化合物1:单斜晶系,P21/c空间群,a=1.274 74(5) nm,b=1.646 31(7) nm,c=1.199 59(5) nm,β=103.344(1)°,V=2.449 5(2) nm3Z=2,Dc=1.381 g·cm-3Mr=1 018.44,μ=0.826 mm-1F(000)=1 060,R=0.033 1,wR=0.073 3;化合物2:单斜晶系,P21/c空间群,a=1.096 74(8) nm,b=0.946 44(6) nm,c=1.725 7(1) nm,β=91.006(4)°,V=1.791 0(2) nm3Z=4,Dc=1.506 g·cm-3Mr=406.08,μ=1.109 mm-1F(000)=840,R=0.031 7,wR=0.049 0。具有晶体学中心对称性的双核镍化合物1中,1,2-二水杨酰基肼通过肼基N-N单键桥联二个Ni(Ⅱ)原子,Ni…Ni原子间距为0.468 83(4) nm,每个Ni(Ⅱ)原子具有轴向伸长的八面体配位构型。化合物2中,Ni(Ⅱ)原子具有平面正方形的配位构型。
关键词: 镍配合物  N-取代水杨基配体  Schiff碱 晶体结构
基金项目: 
Abstract: Two nickel complexes, [Ni2(dsh)(C5H5N)6]·2C5H5N (1) and Ni(spmbh)(C5H5N) (2), have been synthesized and characterized, where H4dsh and H2spmbh are 1,2-disalicyloylhydrazine and N-salicylaldehyde-N′-(4-methox-ybenzoyl) hydrazone, respectively. The complex 1 crystallizes in monoclinic space group P21/c with a=1.274 74(5) nm, b=1.646 31(7) nm, c=1.199 59(5)nm, β=103.344(1)°, V=2.449 5(2)nm3, Z=2, F(000)=1 060, Dc=1.381 g·cm-3, Mr=1 018.44, μ=0.826 mm-1, R=0.033 1, wR=0.073 3. The complex 2 crystallizes in monoclinic space group P21/c with a=1.096 74(8) nm, b=0.946 44(6) nm, c=1.725 7(1) nm, β=91.006(4)°, V=1.791 0(2) nm3, Z=4, Dc=1.506 g·cm-3, Mr=406.08, μ=1.109 mm-1, F(000)=840, R=0.031 7, wR=0.049 0. The two nickel centers in the centrosymmetric binuclear complex molecule 1 are linked by the N-N single bond of the dsh4- ligand, Ni…Ni distance being 0.468 83(4) nm. All the 20 non-hydrogen atoms in the dsh4- ligand are in the same plane. Every nickel(Ⅱ) ion in 1 has an elongated octahedral Ni(ONO)(N)(N)(N) coordination. The two phenolate oxygen atoms, two carbonyl oxygen atoms and two diazine nitrogen atoms of one ligand dsh4- coordinate to two nickel ions, respectively. The nickel(Ⅱ) atom in complex 2 is coordinated by three donors (phenolate oxygen, diazine nitrogen and carbonyl oxygen) in ligand spmbh2- and one pyridine nitrogen atom, forming a square geometry. CCDC: 241833, 241834.
Keywords: nickel complex  N-substituted-salicyl ligand  Schiff base  crystal structure
投稿时间:2004-04-06 修订日期:2004-08-26
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陈小华,刘世雄.二个含N-取代水杨基Schiff碱配体的镍配合物的合成和晶体结构[J].无机化学学报,2005,21(1):15-20.
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