混合配体钒(Ⅳ)配合物[VO(INTH)(dipic)]·EtOH的合成与晶体结构

Synthesis and Crystal Structure of the Mixed-Ligands Oxovanadium(Ⅳ) Complex [VO(INTH)(dipic)]· EtOH

合成了一种新的钒(Ⅳ)与吡啶-2,6_二羧酸和异烟酰肼混配体配合物,[VO(INTH)(dipic)].EtOH,并测定其晶体结构.该晶体属单斜晶系,C2/c群.晶胞参数为:a=2.942 1(4)nm,b=0.809 09(10)nm,c=1.497 87(19)nm,β=107.037(2)°,V=3.409 1(7)nm3,Z=8,F(000)=1 1 696,Mr=414.25,Dc=1.614 g/cm3,μ(Mo kα)=0.631 mm-1,Rl=0.039 7,wR2=0.115 2.三齿配体(吡啶-2,6-二羧酸)和二齿配体(异烟酰肼)分别以ONO和ON的模式与中心酰钒离子配位,形成[VO(ONO)(ON)]结构,并呈变形八面体构型.分子间形成O—H…O和N—H…O氢键,构成两维网状结构.

The reaction of VOSO4 · x H2O with isonicotinyl hydrazine （INTH） and pyridine-2,6-dicarboxylic acid in a H2O EtOH mixture yields bright red crystals of a vanadyl complex [ VO （INTH） （dipic） ]·EtOH （ dipic^2- = pyridine-2,6- dicarboxylate）. It was characterized by Uv-vis, IR spectroscopy and single crystal X-ray diffraction methods. The complex crystallizes in monoclinic space group C2/c with a=2.942l（4）nm,b=0.80909（10）nm,c=1.49787（19）nm,β=107.037（2）°,V=3.4091（7）nm^3,Z=8,F（000）=11696,Mc=414.25,Dc=1.614g/cm^3,μ（Mo kα）=0.631mm^-1,Rt=0.0397,wR2=0.1152. It is a monomeric neutral complex containing vanadyl ion, pyridine-2,6-dicarboxylate acid and isonicotinyl hydrazine ligands, possessing distorted octahedral geometry. The hydrogen bonding interaction between [ VO （INTH） （dipic）] and EtOH is found in the crystal lattice.