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合成了含四氮杂大环hm ta(hm ta=5,7,7,12,14,14-六甲基-1,4,8,11-四氮杂环十四烷)和O,O’-二苯基二硫代磷酸的配合物[M(hm ta).SSP(OPh)2 2)](M=Cu(Ⅱ),1;N i(Ⅱ),2),通过元素分析、红外光谱1、H核磁共振谱、电子光谱和差热分析对其进行了表征,并用X-和射线衍射法测定了1的晶体结构。配合物1属单斜晶系,空间群为P21/n,晶胞参数为:a=9.026(2),b=21.610(6),c=11.736(3),β=105.65(2)°,V=2204.2(10)3,Z=4,Dc=1.372g/cm-3,F(000)=958,μ(MoKα)=8.01 cm-1,S=0.915,(Δ/σ)max=0.002。最终偏离因子(I>2σ(I)),R=0.0391,wR=0.0937,相应的可观测反射数为1914。测定结果表明:配合物中的(PhO)2PSS-为单齿配体,金属离子与配体(PhO)2PSS-的疏和hm ta的氮形成了变型的八面体,配合物具有中心对称性;两配体之间形成了N-H…S氢键。
Synthesis of a tetraazamacrocycle containing hm ta (hm ta = 5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane) and O, O (M = Cu (Ⅱ), 1; Ni (Ⅱ), 2) by diphenyl dithiophosphoric acid (M = hm ta) The structure of 1 was characterized by FTIR, 1HNMR, EDS and DTA. The crystal structure of 1 was determined by X- and X-ray diffraction. The complex 1 belongs to the monoclinic system with a space group of P21 / n with unit cell parameters of a = 9.026 (2), b = 21.610 (6), c = 11.736 (3) and β = 105.65 V = 2204.2 (10) 3, Z = 4, Dc = 1.372 g / cm -3, F (000) = 958, μ (MoKα) = 8.01 cm -1, S = 0.915, (Δ / σ) max = 0.002 . The final deviation factor (I> 2σ (I)), R = 0.0391, wR = 0.0937, and the corresponding observable reflectance is 1914. The results show that the (PhO) 2PSS- in the complex is a monodentate ligand, and the nitrogen of the metal ion and the hydrophobic hm ta of the ligand (PhO) 2PSS- form a modified octahedron. The complex has center symmetry. Between the two ligands formed NH ... S hydrogen bonds.