A new ionic pair complex,1,2′-dinithile-1,2′-dithiolene nickel(II) containing substituted benzylpyridinium [Bz(Me)Py]2[Ni(mnt)2],is prepared and characterized by elemental analyses,IR,UV-VIS and single crystal X-ray...A new ionic pair complex,1,2′-dinithile-1,2′-dithiolene nickel(II) containing substituted benzylpyridinium [Bz(Me)Py]2[Ni(mnt)2],is prepared and characterized by elemental analyses,IR,UV-VIS and single crystal X-ray diffraction.Where [Bz(Me)Py]+ was 1-(1′-phenylethyl)-pyridinium and mnt2-is 1,2′-dinithile-1,2′-dithiolene.The crystal structure was solved by direct method and refined by full-matrix least-squares methods for All the nonhydrogen atoms.The final R1 and wR2 for all data were 0.0450 and 0.1236,respectively.The complex is composed of two [Bz(Me)Py]+ cations and a [Ni(mnt)2]2-anion.The [Ni(mnt)2]2-anions form a stepwise structure by π-π stacking interactions between the CN groups.The cation-anion C-H···N hydrogen bonds and cation-cation C-H···π interactions give further rise to a network structure.展开更多
The title compound has been synthesized by the reaction of [Ni(trans[14]diene)]I2 with Na[Ni(mnt)2] in water and THF, where [trans[14]diene]= 5, 7,7, 12, 14, 14-hexamethyl-1, 4, 8, 11-tetraazacyclotetradeca-4, 11-dien...The title compound has been synthesized by the reaction of [Ni(trans[14]diene)]I2 with Na[Ni(mnt)2] in water and THF, where [trans[14]diene]= 5, 7,7, 12, 14, 14-hexamethyl-1, 4, 8, 11-tetraazacyclotetradeca-4, 11-diene and mnt2- = cis-1, 2-dicyano-1,2-ethylenedithiolato. Its crystal structure has been determined by X-raycrystallography analysis with 4827 independent reflections (Fo>4σ(F0). The bimetallic complex salt [Ni (trans [14] diene )] [Ni (mnt )2] (C24 H32N8Ni2S4, Mr = 678. 24 )crystallizes in the triclinic system with space group P1, a = 9. 2911 (9), b= 11. 7075(12), c=15. 799(2) A, α=68. 384(7), β=79. 324(7), γ=67. 581(6)°, V=1474. 9(3) A3, Dc=1. 527 Mg/m3, Z=2, λ=0. 71073 A, μ=1. 589mm-1, F(000) =704,R=0. 0367. The structure consists of slightly distorted Square planar units [Ni(trans[14]diene)]2+ and [Ni(mnt)2]2-.展开更多
文摘A new ionic pair complex,1,2′-dinithile-1,2′-dithiolene nickel(II) containing substituted benzylpyridinium [Bz(Me)Py]2[Ni(mnt)2],is prepared and characterized by elemental analyses,IR,UV-VIS and single crystal X-ray diffraction.Where [Bz(Me)Py]+ was 1-(1′-phenylethyl)-pyridinium and mnt2-is 1,2′-dinithile-1,2′-dithiolene.The crystal structure was solved by direct method and refined by full-matrix least-squares methods for All the nonhydrogen atoms.The final R1 and wR2 for all data were 0.0450 and 0.1236,respectively.The complex is composed of two [Bz(Me)Py]+ cations and a [Ni(mnt)2]2-anion.The [Ni(mnt)2]2-anions form a stepwise structure by π-π stacking interactions between the CN groups.The cation-anion C-H···N hydrogen bonds and cation-cation C-H···π interactions give further rise to a network structure.
文摘合成了10种含膦胺配体的1,2-二芳基乙烯-1,2-二硫醇的镍配合物[(p-XC_(6)H_(4)N(PPh_(2))2)Ni(S_(2)C_(2)(C_(6)H_(4)Y-p)2)](1:X=Br,Y=CH_(3)O;2:X=Br,Y=CH 3;3:X=Br,Y=H;4:X=Br,Y=Br;5:X=Br,Y=F;6:X=F,Y=CH_(3)O;7:X=F,Y=CH 3;8:X=F,Y=H;9:X=F,Y=Br;10:X=F,Y=F),通过元素分析、核磁共振谱、红外光谱和紫外-可见吸收光谱对镍配合物的结构进行了表征.配合物l DMF的X-射线单晶衍射分析表明镍原子处于近乎完美的四方平面构型的S_(2)P_(2)配位环境中,通过循环伏安法测定了配合物在DMF溶液中的电化学性质以及在三氟乙酸(TFA)存在时的电催化制氢性能.研究结果表明:0.25 mmol配合物1-10在添加67.317 mM TFA时,其电催化制氢的转换频率和过电位分别为299.3~809.7 s^(-1)和0.867~0.995 V.
文摘The title compound has been synthesized by the reaction of [Ni(trans[14]diene)]I2 with Na[Ni(mnt)2] in water and THF, where [trans[14]diene]= 5, 7,7, 12, 14, 14-hexamethyl-1, 4, 8, 11-tetraazacyclotetradeca-4, 11-diene and mnt2- = cis-1, 2-dicyano-1,2-ethylenedithiolato. Its crystal structure has been determined by X-raycrystallography analysis with 4827 independent reflections (Fo>4σ(F0). The bimetallic complex salt [Ni (trans [14] diene )] [Ni (mnt )2] (C24 H32N8Ni2S4, Mr = 678. 24 )crystallizes in the triclinic system with space group P1, a = 9. 2911 (9), b= 11. 7075(12), c=15. 799(2) A, α=68. 384(7), β=79. 324(7), γ=67. 581(6)°, V=1474. 9(3) A3, Dc=1. 527 Mg/m3, Z=2, λ=0. 71073 A, μ=1. 589mm-1, F(000) =704,R=0. 0367. The structure consists of slightly distorted Square planar units [Ni(trans[14]diene)]2+ and [Ni(mnt)2]2-.
