钴配位聚合物{Co(H2O)(phen)(C7H2O2F2Br)2}n的水热合成与结构表征

Hydrothermal Synthesis and Structural Characterization of{Co(H 2 O)(phen)(C 7 H 2 O 2 F 2 Br)2}n

新制备的CoCO3·xH2O加入溶有2,6-二氟-4-溴苯甲酸、邻菲咯啉的CH3OH/H2O(5∶1,V/V)混合溶剂中进行水热法反应,得到一新的钴配位聚合物{Co(H2O)(phen)(C7H2O2F2Br)2}n晶体.化合物结构经单晶X-衍射表征,结果表明配合物结晶于单斜晶系,P21/c空间群,晶胞参数为:a=17.702(3)A,b=6.670(3)A,c=22.559(4)A,β=111.15(3)°,V=2484.2(8)A3,C26H14O5N2F4Br2Co,Mr=729.14,Z=4,Dc=1.950 g·cm-3,F(000)=1428.最后残余因子R1=0.0538,wR2=0.1334.晶体结构中,中心Co(Ⅱ)原子六配位模式形成畸变的八面体结构,分子间经过钴与其中一个2,6-二氟-4-溴苯甲酸羧基的2个O原子配位桥联作用沿b方向形成一维链聚合物,一维双链间存在π-π芳环堆积作用构筑形成bc层.

Hydrothermal reaction of a freshly prepared CoCO3·xH2O,4-bromo-2,6-difluorobenzoic acid and 1,10-phenanthroline(phen)in CH3OH/H2O(5∶1,V/V)yielded{Co(H2O)(phen)(C7H2O2F2Br)2}n.The cobalt coordination polymer was structurally characterized by single-crystal X-ray diffraction,it crystallizes in monoclinic system,space group P21/c,with a=17.702(3)A,b=6.670(3)A,c=22.559(4)A,β=111.15(3)°,V=2484.2(8)A3,C26H14O5N2F4Br2Co,Mr=729.14,Z=4,Dc=1.950 g·cm-3,F(000)=1428,R1=0.0538 and wR2=0.1334 for 3834 observed reflections(I≥2σ(I))of 4357 unique reflections.Within the complex,each Co(Ⅱ)atom has a distorted octahedral geometry which was six-coordinated by two N atoms and four O atoms.The chains bridged by 4-bromo-2,6-difluorobenzoato carboxylate anions extend in the b direction,the bc layers are assembled by inter-chainsπ-πpacking interaction with aromatic rings.