一个不常见的Ni(Ⅱ)的戊三酮二水杨酰腙配合物的合成和晶体结构 |
Synthesis and Crystal Structure of a Novel Nickel(Ⅱ) Complex with [Pentanetrione 2,4-Bis(Salicylhydrazonato)] |
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摘要: 合成了镍的戊三酮二水杨酰腙配合物Ni(C19H16N4O5)的两个同质异晶,测定其晶体结构。该配合物的两个晶体均属单斜晶系,空间群为C2/c,晶体1晶胞参数为:a=1.03076(9)nm,b=1.9105(1)nm,c=0.93305(8)nm,β=101.490(4)°,Z=4,μ=1.119mm-1,R=0.0370;晶体2晶胞参数为:a=2.1949(3)nm,b=0.9901(2)nm,c=0.8568(1)nm,β=92.799(6)°,Z=4,μ=1.084mm-1,R=0.0440。两个晶体中镍原子由多啮配体的二个酰氧原子和二个肼氮原子形成平面正方形配位。对配合物的红外光谱进行归属。 |
关键词: Schiff碱 镍配合物 晶体结构 |
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Abstract: The two allomers of the title complex of [pentanetrione 2,4-bis(salicylhydrazonato)] nickel(Ⅱ), Ni1C19H16N4O5, crystallize in the monoclinic system, and space group C2/c,a=1.03076(9)nm,b=1.9105(1)nm,c=0.93305(8)nm,β=101.490(4)°,V=1.8006(3)nm3,Dc=1.620g·cm-3,Z=4,F(000)=904,μ=1.119mm-1,R=0.0370,GOF=0.748(crystal 1);a=2.1949(3)nm,b=0.9901(2)nm,c=0.8568(1)nm,β=92.799(6)°,V=1.8597(5)nm3,Dc=1.568g·cm-3,Z=4,F(000)=904,μ=1.084mm-1,R=0.0440,GOF=0.849 (crystal 2). The structures were solved by direct methods and refined by least-squares techniques to a final agreement factor of 0.0370 based on 1505 observed reflections and 0.0440 on 1477 observed reflections with I≥2σ(I) for crystal 1 and crystal 2, respecially. There are different arrangements between the crystals 1 and 2, while the two crystals have same formula and similar molecular configuration. The nickel atom in the two crystals has a square-planar configuration formed by N2O2 donor atoms from the planar hydrazone ligand. |
Keywords: Schiff base Nickel(Ⅱ) complex crystal structure |
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尹华,刘世雄.一个不常见的Ni(Ⅱ)的戊三酮二水杨酰腙配合物的合成和晶体结构[J].无机化学学报,2002,18(3):269-274. |
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