Synthesis and Crystal Structure of Bis[O,O'-bis(4-tert-butylphenyl)dithiophosphate]nickel(Ⅱ)  

作　　者：张秀兰 邹立科 谢斌 赖川 李玉龙 

机构地区：[1]Institute of Functional Materials,Sichuan University of Science & Engineering [2]University Key Laboratory of Green Chemistry of Sichuan Province [3]College of Chemistry and Pharmaceutical Engineering,Sichuan University of Science & Engineering [4]College of Chemistry and chemical Engineering,Chongqing University

出　　处：《Chinese Journal of Structural Chemistry》2013年第5期779-785,共7页结构化学（英文）

基　　金：supported by theDepartment of Science and Technology of Sichuan Province (No. 2011JY0052,No. 2010GZ0130);Sichuan University of Science and Engineering (No. 2012PY04, No. 2012PY14);Key Laboratory of Material Corrosion and Protection of Sichuan Province (No.2011CL003)

摘　　要：A new O,O＇-bis（4-tert-butylphenyl）dithiophosphate complex Ni[SSP（OC6H4But- p）2]2 （1） was synthesized and characterized by elemental analysis, IR, 1H NMR, thermogravimetric analysis （TGA） and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 12.8440（3）, b = 6.18686（12）, c=26.3018（5） , β=92.6135（18）°, V = 2087.87（7） 3, Z = 2, Dc = 1.345 g/cm3, μ = 0.780 mm-1, the final R = 0.0316 and wR = 0.0748 （Ⅰ 〉2σ（Ⅰ））. A total of 4269 unique reflections were collected, of which 3621 with Ⅰ 〉 2σ（Ⅰ） were observed. The NiII atom lies on an inversion center and is chelated by two （p-ButC6H4O）2PSS-ligands in a [NiS4] square-planar geometry with Ni-S bonds of 2.2408（5） and 2.2444（5） , respectively. A stepwise 1D chain structure is constructed via intermolecular S…S and C-H…S interactions. According to our knowledge this is the first case that intermolecular S…S interaction is observed in mononuclear transition metal complex of O,O＇-dialkyldithiophosphates.A new O,O＇-bis（4-tert-butylphenyl）dithiophosphate complex Ni[SSP（OC6H4But- p）2]2 （1） was synthesized and characterized by elemental analysis, IR, 1H NMR, thermogravimetric analysis （TGA） and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 12.8440（3）, b = 6.18686（12）, c=26.3018（5） , β=92.6135（18）°, V = 2087.87（7） 3, Z = 2, Dc = 1.345 g/cm3, μ = 0.780 mm-1, the final R = 0.0316 and wR = 0.0748 （Ⅰ 〉2σ（Ⅰ））. A total of 4269 unique reflections were collected, of which 3621 with Ⅰ 〉 2σ（Ⅰ） were observed. The NiII atom lies on an inversion center and is chelated by two （p-ButC6H4O）2PSS-ligands in a [NiS4] square-planar geometry with Ni-S bonds of 2.2408（5） and 2.2444（5） , respectively. A stepwise 1D chain structure is constructed via intermolecular S…S and C-H…S interactions. According to our knowledge this is the first case that intermolecular S…S interaction is observed in mononuclear transition metal complex of O,O＇-dialkyldithiophosphates.

关 键 词：O O＇-dialkyldithiophosphate nickel（ll） complex synthesis crystal structure 

分 类 号：O641.4[理学—物理化学]