分别以二水合氯化铜,4-氯苯甲酸(4-CBAH),2,2-联吡啶(2,2-bipy)和二水合氯化锌,4-溴苯甲酸(4-BBAH),1,10-邻菲咯林(1,10-phen)为原料,经溶剂蒸发法合成了2个新型的混配型配合物[Cu(4-CBA)2(2,2-bipy)(H2O)]n(1)和[Zn(4-BBA)2(1,10-phen)(H2O)]n(2),其结构和性能经IR,元素分析,X-单晶衍射,X-粉末衍射和TGA表征。1(CCDC:1 013 762)和2(CCDC:1 013763)均属三斜晶系,空间群P-1;1的晶胞参数a=8.087(7),b=9.999(9),c=15.431(13),α=78.051(14)°,β=81.996(13)°,γ=70.714(14)°,V=1 148.8(17)3,Z=2,Dc=1.587 g·cm^-3,R1=0.060 7,ωR2=0.174 4。2的晶胞参数a=7.971(16),b=10.783(2),c=15.053(3),α=99.847(3)°,β=95.516(4)°,γ=107.485(3)°,V=1 200.8(4)3,Z=2,Dc=1.835 g·cm^-3,R1=0.035 0,ωR2=0.084 7。1和2均为扭曲的四方锥构型{MO3N2}单元;单元内,水分子的两个氢原子与未参与配位的羧酸氧原子形成分子内氢键;相邻单元间经π┉π作用形成一维超分子结构。TGA分析表明:1于120℃开始分解,800℃失重率85.10%;2于150℃开始分解,800℃失重率85.25%。
Two novel coordination complexes,[Cu( 4-CBA)2( 2,2-bipy)( H2O) ]n( 1) and [Zn( 4-BBA)2( 1,10-phen)( H2O) ]n( 2),were synthesized by solvent evaporation method,using Cu Cl2·2H2O,4-CBAH,2,2-bipy and Zn Cl2·2H2O,4-BBAH,1,10-phen as materials. The structures and properties were characterized by IR,elemental analysis,single-crystal X-ray,powder X-ray diffraction and TGA. 1( CCDC: 1 013 762) and 2( CCDC: 1 013763) both belong to triclinic system and space group P-1. The cell parameters of 1 and 2 were a = 8. 087( 7) ,b = 9. 999( 9) ,c =15. 431( 13) ,α = 78. 051( 14) °,β = 81. 996( 13) °,γ = 70. 714( 14) °,V = 1 148. 8( 17) 3,Z = 2,Dc = 1. 587 g·cm- 3,R1= 0. 060 7,ωR2= 0. 174 4 and a = 7. 971( 16) ,b = 10. 783( 2),c = 15. 053( 3) ,α = 99. 847( 3) °,β = 95. 516( 4) °,γ = 107. 485( 3) °,V = 1 200. 8( 4) 3,Z = 2,Dc = 1. 835 g · cm^- 3,R1= 0. 035 0,ωR2= 0. 084 7,respectively. 1 and 2 were twisted quartet cone conformation { MO3N2} unit. Intra-molecule hydrogen bond was constituted by two hydrogen atom of H2 O and one oxygen atom of non-ligand carboxylic acid in unit. 1D supramolecular structure was formed by π┉π effect between neighboring unit. TGA analysis indicated that 1 began to decompose at 120 ℃ and weight loss ratio was 85. 10% at 800 ℃. 2 began to decompose at 140℃ and weight loss ratio was 85. 25% at 800 ℃.