A ternary adduct Cu[S2P（OCH2CH2Ph）2]2·bipy（bipy=α,α＇-bipyridine） was syn-thesized and characterized by elemental analysis,IR and single-crystal X-ray diffraction.The crystal belongs to the triclinic system...A ternary adduct Cu[S2P（OCH2CH2Ph）2]2·bipy（bipy=α,α＇-bipyridine） was syn-thesized and characterized by elemental analysis,IR and single-crystal X-ray diffraction.The crystal belongs to the triclinic system,space group P1 with a=10.2320（2）,b=11.5249（3）,c=18.0916（3）,α=98.95（1）,β =103.601（1）,γ=91.272（2）°,V=2044.49（7）3,Z=2,Dc=1.453 g/cm3,T=153（2） K,C42H44CuN2O4P2S4,Mr=894.51,λ（MoKα）=0.71073,μ=0.86 mm-1,S=0.999,（△/σ）max=0.002,the final R=0.0243 and wR=0.0704.A total of 9221 unique reflections were collected,of which 8573 with Ⅰ 〉2σ（Ⅰ） were observed.The Cu（Ⅱ） atom is five-coordinated in a rather distorted trigonal bipyramidal geometry（τ value=0.537）.The Cu-S distances range from 2.3491（4） to 2.4829（4） ,and the Cu-N distances are 1.9987（12） and 2.0584（11） ,respectively.An interesting feature of this adduct resides in its two-dimensional（2D） open framework constructing through hydrogen bonding and π-π interactions.展开更多
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-...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.展开更多
基金supported by the Education Committee of Sichuan Province (No.09ZA057)Department of Science and Technology of Sichuan Province (No. 2009JY0071 and 2010GZ0130)+1 种基金Science and Technology Office of Zigong City (No. 08X01)Key Laboratory of Material Corrosion and Protection of Sichuan Colleges and Universities (No. 2008CL04)
文摘A ternary adduct Cu[S2P（OCH2CH2Ph）2]2·bipy（bipy=α,α＇-bipyridine） was syn-thesized and characterized by elemental analysis,IR and single-crystal X-ray diffraction.The crystal belongs to the triclinic system,space group P1 with a=10.2320（2）,b=11.5249（3）,c=18.0916（3）,α=98.95（1）,β =103.601（1）,γ=91.272（2）°,V=2044.49（7）3,Z=2,Dc=1.453 g/cm3,T=153（2） K,C42H44CuN2O4P2S4,Mr=894.51,λ（MoKα）=0.71073,μ=0.86 mm-1,S=0.999,（△/σ）max=0.002,the final R=0.0243 and wR=0.0704.A total of 9221 unique reflections were collected,of which 8573 with Ⅰ 〉2σ（Ⅰ） were observed.The Cu（Ⅱ） atom is five-coordinated in a rather distorted trigonal bipyramidal geometry（τ value=0.537）.The Cu-S distances range from 2.3491（4） to 2.4829（4） ,and the Cu-N distances are 1.9987（12） and 2.0584（11） ,respectively.An interesting feature of this adduct resides in its two-dimensional（2D） open framework constructing through hydrogen bonding and π-π interactions.
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)
文摘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.
