对位取代苯甲酸与2,2′-联吡啶配体构筑的两种二价铅配合物的合成、晶体结构及性质(英文)

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水热条件下,合成了2个含对位取代苯甲酸和2,2′-联吡啶配体的二价铅配合物[Pb(4-HOBA)2(2,2′-bipy)]·H2O(4-HOBAH=4-hydroxybenzoicacid,2,2′-bipy=2,2′-bipyridine)(1)及[Pb(4-MBA)2(2,2′-bipy)](4-MBAH=4-methylbenzoicacid)(2),并通过X-射线单晶结构分析、元素分析、红外光谱、紫外光谱、荧光光谱以及热重分析等手段对配合物进行了表征与研究。X-射线单晶结构测定表明,2种晶体的不对称单元中,六配位的二价铅离子分别与来自1个2,2′-联吡啶的2个N原子和2个对位取代苯甲酸的4个O原子螯合。配合物1属单斜晶系,P21/c空间群,a=1.09483(4)nm,b=1.75194(6)nm,c=1.20479(4)nm,β=100.334(2)°,V=2.27339(14)nm3,Z=4,finalR1=0.0254,wR2=0.0674。广泛存在的分子间氢键和弱π…π堆积作用将配合物1组装成稳定的三维超分子结构。配合物2属三斜晶系,P1空间群,a=0.95510(11)nm,b=1.00805(12)nm,c=1.32483(15)nm,α=109.865(1)°,β=97.322(1)°,γ=90.643(1)°,V=1.1878(2)nm3,Z=2,finalR1=0.0284,wR2=0.0508。配合物2经由一对Pb…O(0.3185(2)nm)弱相互作用被组装成二聚体结构,弱的Pb…O相互作用及与配合物1中类似的π…π堆积作用共同构筑了配合物2的三维结构。在配合物1和2中,铅的6s孤电子均显示了立体化学活性,使配位键分布于半球型区域。同时,两种配合物固体均具有光致发光特性,并在蓝光区有较强发射。 Under hydrothermal conditions, two divalent lead complexes [Pb (4-HOBA) 2 (2,2’-bipy)] · H2O with para-substituted benzoic acid and 2,2’- (4-MBBA = 4 (4-MBA) 2 (2,2’-bipy)] with 4-hydroxybiphenyl (4-HOBAH = 4-hydroxybenzoic acid, 2,2’-bipy = 2,2’-bipyridine) -methylbenzoic acid) (2). The complex was characterized and studied by X-ray single crystal structure analysis, elemental analysis, IR, UV, FTIR and TG analysis. X-ray single crystal structure determination showed that two kinds of crystal asymmetric unit, the hexacoordination of the two lead ions respectively from a 2,2’-dipyridyl 2 N atoms and two para-substituted benzene 4 O atoms of formic acid chelate. Complex 1 belongs to the monoclinic system with a = 1.09483 (4) nm, b = 1.75194 (6) nm, c = 1.20479 (4) nm and β = 100.334 (2) °, P = 2.27339 (14) nm3, Z = 4, finalR1 = 0.0254, wR2 = 0.0674. Widely existing intermolecular hydrogen bonding and weak π ... π stacking effect complex 1 into a stable three-dimensional supramolecular structure. The complex 2 belongs to the triclinic system with a = 0.95510 (11) nm and b = 1.00805 (12) nm, c = 1.32483 (15) nm and α = 109.865 ) °, γ = 90.643 (1) °, V = 1.1878 (2) nm3, Z = 2, finalR1 = 0.0284, wR2 = 0.0508. Complex 2 is assembled into a dimeric structure via a pair of weak interactions of Pb ... O (0.3185 (2) nm), a weak Pb ... O interaction and a similar pi ... stacking effect in complex 1 Three-dimensional structure of complex 2. In complexes 1 and 2, the 6s lone lead of lead all showed the stereochemical activity, which made the coordination bond distribute in the hemispherical region. At the same time, both complexes have photoluminescence properties and strong emission in the blue region.
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