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配合物[Ni(spa)2](Hspa=N3-水杨酰吡啶-2-羰基氨基腙)用Hspa与Ni(Ac)2.4H2O反应制备.标题化合物的单晶X射线研究表明,Ni原子是位于两个三齿配体中的吡啶氮原子,氨基腙上的氮原子和甲氨酰基中的氧原子配位的畸变八面体形式中.该晶体属三斜晶系,P1空间群;a=1.063 58(3)nm,b=1.193 80(3)nm,c=1.26 354(3)nm,α=70.109 0(10)°,β=81.722 0(10)°,γ=87.476 0°,V=1.492 87(7)nm3,Z=2,Mr=642.32(C29H29N9O5Ni),Dc=1.429g.cm-3,μ=0.705 mm-1,F(000)=668,对于I>2σ(I)的4 487个反射点,R=0.030 8,Rw=0.080 4.在晶体结构中,存在两个羟基的O—H…N分子内氢键,此外两个N—H…O分子间氢键连接相邻的配合物形成一条平行于c轴的链,另一个N—H…O分子间氢键连接溶剂DMF分子.
The complex [Ni (SPA) 2] (Hspa = N3-salicyloylpyridine-2-carbonylamin hydrazone) was prepared by the reaction of Hspa with Ni (Ac) 2.4H2O.The single crystal X-ray study of the title compound showed that the Ni atom is Among the two tridentate ligands, the pyridine nitrogen atom, the nitrogen atom on the aminohydrazone and the oxygen atom in the carbamoyl group are in the form of distorted octahedron.The crystal belongs to the triclinic system, space group P1; a = 1.063 58 (3) nm, b = 1.193 80 (3) nm, c = 1.26 354 (3) nm, α = 70.109 ° 10 °, β = 81.722 ° 10 °, γ = 87.476 ° °, V = 1.492 87 (7) nm3, Z = 2, Mr = 642.32 (C29H29N9O5Ni), Dc = 1.429g.cm-3, μ = 0.705 mm-1 and F (000) = 668 for I> 2σ 4 487 reflection points, R = 0.030 8, Rw = 0.080 4. In the crystal structure, there are two hydroxyl O-H ... N intramolecular hydrogen bonds, in addition to the two N-H ... O intermolecular hydrogen bonding phase The adjacent complexes form a chain parallel to the c-axis and the other N-H ... O molecule is hydrogen-bonded to the solvent DMF molecule.