超分子化合物[Ni(C_6H_4O_2N)_2·(H_2O)_4]_n的水热合成及晶体结构

用皮考林酸和六水合氯化镍反应制备了一种三维氢键超分子配合物,经X射线衍射分析确定了单晶结构.该晶体属单斜晶系,P21/m空间群,晶胞参数为:a=0.976 0(2)nm,b=0.522 54(10)nm,c=1.450 1(3)nm,Mr=374.98,α=90.08(3)°,β=90.08(3)°,γ=90°,V=0.739 63(3)nm3,Z=2,ρ=1.684 g/cm3,F(000)=388,μ=1.357 mm-1,R=0.039 0,wR=0.090 8.共收集2 656个衍射数据,其中1 569个为独立衍射点(Rint=0.033 2),可观测点数1 382个(I>2σ(I)).结果表明,在组成该超分子体系的基本结构单元[N i(C6H4O2N)2.(H2O)4]中,N i(Ⅱ)离子形成六配位的稍拉长的八面体构型,配合物单元之间通过氢键相互连接,形成了无限延伸的具有网状结构的三维超分子体系.

Hydrothermal Synthesis and Crystal Structure of a Supermolecular compound [Ni(C6H4O2N)2·(H2 O)4]n

A supermolecular compound was synthesized with picoloy acid and NiCl_(2)·6H_(2)O.Its structure was determined by single-crystal X-ray diffraction.The crystal belongs to monoclinic system with P2_(1)/m space group.The cell parameters are: a=0.976 0(2) nm,b=0.522 54(10) nm,c=1.450 1(3) nm,M_(r)=374.98,α=β=90.08(3)°,γ=90°,V=0.739 63(3) nm~(3),Z=2,ρ=1.684 g/cm~(3),F(000)=388,μ=1.357 mm~(-1),R=0.390,wR=0.090 8.The crystal consists of [Ni(C_(6)H_(4)O_(2)N)_(2) ·(H_(2)O)_(4)] units in which the Ni(Ⅱ) ion is located in a slightly distorted octahedral center.Each units is connected by hydrogen bonds to form a three-dimensional network structure.