3-(水杨酰肼)-丁基-2-酮肟和两个镍的酮肟配合物的合成和晶体结构

Syntheses and Crystal Structures of 3-(salicyloylhydrazono)butan-2-one Oxime and Two Nickel Complexes with 3-(salicyloylhydrazono)butan-2-one Oxime

合成了3鄄(水杨酰肼)鄄丁基鄄2鄄酮肟H2L(1,C11H13N3O3)和2个镍的3鄄(水杨酰肼)鄄丁基鄄2鄄酮肟化合物[Ni(HL)(CH3COO-)(C5H5N)2](2)和[Ni(HL)2]·2C3H7NO(3)。化合物1晶体属单斜晶系,空间群为P21/n,晶体学参数为:a=0.45187(2)nm,b=2.0868(1)nm,c=1.22448(9)nm,β=94.974(3)°,V=1.1503(1)nm3,Z=4,Dc=1.358g·cm-3,μ=0.101mm-1,F(000)=496,R=0.0435,wR=0.1425。化合物2晶体属单斜晶系,空间群为P21/n,晶体学参数为:a=1.36239(8)nm,b=1.34537(6)nm,c=1.43854(7)nm,β=113.138(3)°,V=2.4246(2)nm3,Z=4,Dc=1.398g·cm-3,μ=0.843mm-1,F(000)=1064,R=0.0424,wR=0.1166。化合物3晶体属单斜晶系,空间群为P21/c,晶体学参数为:a=1.10422(7)nm,b=2.8601(1)nm,c=1.11413(7)nm,β=114.589(5)°,V=3.1995(3)nm3,Z=4,Dc=1.398g·cm-3,μ=0.667mm-1,F(000)=1416,R=0.0576,wR=0.1535。在化合物1晶体中,酮肟分子之间通过分子间氢键形成二维网状结构。在化合物2中,每个镍髤离子由1个3鄄(水杨酰肼)鄄丁基鄄2鄄酮肟的2个氮原子和1个氧原子,2个吡啶分子中的2个氮原子和1个乙酸根中的1个氧原子形成畸变的NiN4O2八面体配位构型,存在分子内氢键O-H(肟)…O(乙酸根)和O鄄H(酚)…N(酰肼)。在化合物3晶体中,每个镍髤离子由2个3鄄(?

3-(salicyloylhydrazono)butan-2-one oxime H2L (1, C11H13N3O3) and two nickel complexes with 3-(salicyloylhydrazono)butan-2-one oxime, [Ni (HL) (C5H5N)(2)(CH3COO-)] (2) and [Ni(HL)(2)] . 2DMF (3), have been prepared and characterized. The crystallographic data are space group P2(1)/n, a=0.451 87(2) nm, b=2.086 8(1) nm, c=1.224 48(9) nm, beta=94.974(3)degrees, V=1.1503(1) nm(3), Z=4, D-e=1.358 g (.) cm(-3), F(000)=496, mu=0.101 mm(-1), R=0.0435, and wR= 0.1425 for compound 1; space group P2(1)/n, a=1.362 39(8) nm, b=1.345 37(6) nm, c=1.438 54(7) nm, beta=113.138 (3)degrees, V=2.424 6(2) nm(3), Z =4, D,=1.398 g (.) cm(3), F(000)=1064, mu=0.843 mm(-1), R=0.042 4, and wR=0.1166 for compound 2; space group P2(1)/c, a=1.104 22(7) nm, b=2.860 1(1) nm, c=1.114 13(7) nm, beta=114.589(5)degrees, V=3.199 5 (3) nm(3), Z=4, D-e=1.398 g (.) cm(-3), mu=0.667 mm(-1), F(000)=1416, R=0.057 6, and wR=0.153 5 for compound 3. The neighboring molecules of compound 1 are connected together with intermolecular hydrogen bonds, forming a two-dimensional supramolecular architecture. The Ni atom in compound 2 has a distorted octahedral coordination. Three donors (carbonyl oxygen, hydrazide nitrogen and oxime nitrogen) of the ligand HL- and one acetate oxygen comprise the basal plane. Two nitrogen atoms of two pyridine molecules occupy axial positions. There are two intramolecular hydrogen bonds of O-H(oxime)...O(acetate) and O-H(phenol)...N(hydrazide) in the molecule of compound 2. The Ni atom in compound 3 is octahedrally coordinated by four N atoms and two O atoms from two ligands HL-. There are intramolecular hydrogen bonds of O-H...O and O-H...N and intermolecular hydrogen bond of O-H...O in compound 3.