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合成了配合物{[Cu(hmtade)][Ni(dmit)2]}2.4DMSO(1)(hmtade为5,7,7,12,14,14-六甲基-1,4,8,11-四氮杂环十四-4,11-二烯;dmit为1,3-二硫杂环戊二烯-2-硫酮-4,5-二硫醇;DMSO为二甲亚砜),采用元素分析、红外光谱和紫外-可见光谱进行了表征,并用X射线衍射法测定了晶体结构.该晶体属于单斜晶系,P21/n空间群;晶胞参数:a=1.49952(6)nm,b=1.77229(7)nm,c=3.1275(1)nm,β=102.442(1)°,V=8.1163(5)nm3,Dc=1.558Mg/m3,Z=8,F(000)=3944,μ(MoKα)=1.637mm-1,S=1.016,(Δ/σ)max=0.001,R1=0.0673,wR2=0.1672[I>2σ(I)].晶体结构研究表明,配合物{[Cu(hmtade)].[Ni(dmit)2]}2.4DMSO包含2个[Cu(hmtade)][Ni(dmit)2]子单元.每个子单元中,1个dmit中的1个S原子与Cu及Ni配位,形成异双核Cu—Ni配合物.其中Cu(Ⅱ)为五配位的四方锥构形,Cu—N键长在0.1949(5)～0.2007(4)nm范围内,Cu—S键长分别为0.28913(18)和0.28952(18)nm;配阴离子[Ni(dmit)2]2-为畸变四方形,Ni—S键长在0.21729(16)～0.21905(17)nm范围内.溶剂分子DMSO与配体hmtade形成了N—H…O氢键.通过分子内S…S和S…H短接触形成了二聚体,二聚体之间通过S…S短接触形成一维链状结构,并通过S…S,S…H和C…H短接触进一步形成二维和三维结构.
The complexes {[Cu (hmtade)] [Ni (dmit) 2]} 2.4DMSO (1) (hmtade is 5,7,7,12,14,14-hexamethyl-1,4,8,11 -tetraazacyclotetra-4,11-diene; dmit is 1,3-dithiol-2-thione-4,5-dithiol; DMSO is dimethyl sulfoxide) The crystal structure was characterized by elemental analysis, IR and UV-Vis spectra and the crystal structure was determined by X-ray diffraction. The crystal belongs to the monoclinic space group P21 / n. The unit cell parameters are a = 1.49952 (6) nm , b = 1.77229 (7) nm, c = 3.1275 (1) nm, β = 102.442 (1) °, V = 8.1163 (5) nm3, Dc = 1.558 Mg / m3, Z = 8 and F (000) = 3944 , (MoKα) = 1.637mm-1, S = 1.016, (Δ / σ) max = 0.001, R1 = 0.0673, wR2 = 0.1672 [I> 2σ (I) (Ni (dmit) 2]} 2.4DMSO contains two [Cu (hmtade)] [Ni (dmit) 2] subunits. In each subunit, one S atom in one dmiter and one Cu atom in Cu And Ni to form a heterobinuclear Cu-Ni complex, in which Cu (Ⅱ) is a five-coordinate tetragonal conformation with a Cu-N bond length in the range of 0.1949 (5) -0.2007 (4) S bond lengths were 0.28913 (18) and 0.28952 (18) nm, respectively. The anions [Ni (dmit) 2] 2- were distorted tetragonal with Ni-S bond lengths ranging from 0.21729 (16) to 0.21905 Soluble The molecular agent DMSO forms a N-H ... O hydrogen bond with the hmtade ligand and forms a dimer by short contacts within the molecule S ... S and S ... H, forming a one-dimensional chain by short contact between the dimers Like structure and further forming two-dimensional and three-dimensional structures by short contacts of S ... S, S ... H and C ... H.