摘要
在丙酮溶剂中,双((O,O’-二苯乙基)二硫代磷酸)合镍配合物与双齿桥联氮碱配体4,4’-联吡啶(4,4’-bipy)反应,得到了一维配位聚合物[Ni{S2P(OCH2CH2Ph)2}2(4,4’-bipy)]n,用元素分析、红外光谱、1H NMR、13C NMR、31P NMR和X-射线衍射技术对其结构进行了表征。该化合物属单斜晶系,C 2/c空间群,晶胞参数为a=29.500(4),b=11.289(3),c=13.407(4),β=99.44(4)°,V=4404.4(18)3,Z=4,C42H44N2NiO4P2S4,Mr=889.68,Dc=1.342 g/cm3,F(000)=1856,μ(MoKα)=0.744 mm-1。可观测衍射点为2550个,R=0.052,wR=0.1329(I>2σ(I)),所有数据的R=0.0971,wR=0.1489。
A ternary coordination polymer[ Ni { S2P( OCH2CHzPh) 2 } 2 (4, 4' -bipy) ] is synthesized by treatment of Bis [ O, O' -di (2-phenylethyl) dithiophosphato ] Nickel (II) complex [ Ni { S2 P ( OCH2 CH2 Ph) 2 } 2 ] with 4, 4' -Bipyridine in ace- tone and fully characterized by elemental analysis and IR, I H NMR, ^13C NMR ,31p NMR spectroscopies. In addition, the molecular structure of the complex is established by X-ray crystallography. The crystal of coordination polymer crystallizes in monoclinic, spaeegroup C 2/cwith a =29. 500 (4), b = 11. 289 (3), c = 13. 407 (4) A, β =99.44(4)°, V= 4404.4( 18)A3, Z = 4, C42 H44 N2NiO4P2S4, Mr = 889.68, Dc = 1. 342 g/em3, F (000) = 1856 and/z (MoKct) = 0. 744 mm-J. The results are that the final R = 0. 0520 and wR = 0. 1329 for 2550 observed reflections with I 〉 2o-(I) and R =0.0971 and wR =0. 1498 for all data.
出处
《四川理工学院学报(自然科学版)》
CAS
2013年第2期20-24,共5页
Journal of Sichuan University of Science & Engineering(Natural Science Edition)
基金
四川省科技厅项目(2012JY0115
2011JY0052)
四川理工学院引进人才项目(2011RC06)
关键词
O
O’-二苯乙基二硫代磷酸
配位聚合物
晶体结构
0, O' -di (2-phenylethyl) dithiophosphato
coordination polymer
crystal structure