论文部分内容阅读
在石油醚和丙酮溶液中,配合物Ni[S2P(OCH2CH2PH)2]2与1,10-邻菲啰啉(phen)反应得到了绿色的氮碱加合物1,10-林菲啰啉.双(O,O-(二2-苯乙基)二硫代磷酸)合镍(Ⅱ),用元素分析、紫外-可见光谱、红外光谱、热分析和X-射线单晶衍射进行了表征。加合物属单斜晶系,P21/c空间群。晶胞参数为a=1.0987(9)nm,b=2.1432(9)nm,c=1.9025(5)nm,β=98.68(1)°,V=4.429(4)nm3,Z=4,Dc=1.370 Mg/m3,F(000)=1904,μ=0.743mm-1,可观测衍射点为3498,R=0.057,wR=0.1492(I(2σ(Ⅰ))。加合物为畸变八面体构型,配位原子来自于两个O,O’-二(2-苯乙基)二硫代磷酸根的4个硫原子和配体phen的2个氮原子。Ni-S键的键长在0.2474(2)-0.2505(17)nm范围内,Ni-N键的键长分别为0.2081(4)nm和0.2090(5)nm。因分子间存在π-π堆积、C-H…O和C-H…S氢键作用,加合物的晶体结构形成了一维链对和一维双链螺旋链。一维链对和一维双链螺旋链通过C-H…O氢键作用进一步延展为三维结构。
The complex of Ni [S2P (OCH2CH2PH) 2] 2 with 1,10-phenanthroline (phen) was obtained as the green base-adduct 1,10-linphenanthroline in petroleum ether and acetone solutions. The nickel (Ⅱ) complexes were characterized by elemental analysis, UV-Vis, IR, thermal analysis and single crystal X-ray diffraction. Adduct is a monoclinic, P21 / c space group. The cell parameters are a = 1.0987 (9) nm, b = 2.1432 (9) nm, c = 1.9025 (5) nm, β = 98.68 1.370 Mg / m3, F (000) = 1904, μ = 0.743mm-1, the observed diffraction point is 3498, R = 0.057, wR = 0.1492 (I (2σ (Ⅰ) Type, the coordination atoms are derived from the two sulfur atoms of O, O’-bis (2-phenylethyl) phosphorodithioate and the two nitrogen atoms of the ligand phen. The bond length of the Ni-S bond is between 0.2474 (2) -0.2505 (17) nm, the bond lengths of Ni-N bond are 0.2081 (4) nm and 0.2090 (5) nm, respectively. Due to the π-π stacking between the molecules, CH ... O and CH ... S Hydrogen bond and the adduct crystal structure forms a one-dimensional chain and a one-dimensional double-stranded helical chain.The one-dimensional chain pair and the one-dimensional double-stranded helical chain further extend to the three-dimensional structure through the CH ... O hydrogen bonding.