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1、精品论文Crystal structure, thermogravimetric analysis and electrochemical properties of the cobalt() complex of1-(4-methoxybenzyl)-2-(4-5methoxyphenyl)benzimidazoleYANG Hongwei, YUE Fan, WANG Jide(Key Laboratory of Oil and Gas Fine Chemicals, Ministry of Education and Xinjiang UyghurAutonomous Region, C
2、ollege of Chemistry and Chemical Engineering, Xinjiang University,10Urumqi, 830046)Abstract: Cobalt (II) complex of 1-(4-methoxybenzyl)-2-(4-methoxyphenyl)benzimidazole have been synthesized and characterized by IR, X-ray diffraction, thermogravimetric analysis, and cyclic voltammetry. This complex
3、crystallized in the monoclinic space group P2/n with the cobalt atom adopting a four-coordinate distorted-tetrahedral environment, crystal of the complex: a=12.88 (),15b=9.83( ),c=15.44( ), =90, V=1953.0(5) 3. The cobalt adopts a four-coordinate distorted-tetrahedral environment by two nitrogen atom
4、s and two terminal chlorine atoms. The electrochemical characteristics have been studied by cyclic voltammetry, and the result proved that the coordination of the ligand with cobalt(II) increased the electrochemical activity of the ligand. Thecomplex was characterized by thermogravimetric analysis r
5、evealed it has good thermal stability.20Key words: Benzimidazole derivative; Schiff base; crystal structure; Co(II) Complex0IntroductionBenzimidazoles are of considerable chemical and biological interest as their derivatives have found wide use as anthelmintic agents in both human and veterinary med
6、icine.The coordination chemistry of azoles acting as ligands in transition metal compounds has led to the extensive study25of chelating ligands incorporating benzimidazole groups for modeling biological systems 1-3.We have reported that the reaction ofp-methoxybenzaldehyde with o-phenylenediamine yi
7、elded the benzimidazole derivative (1-(4-methoxybenzyl)-2 -(4-methoxyphenyl)benzimidazole) 1 4. In order to examine the characteristics of the corresponding complexes of this ligand, the cobalt(II) complex 2 has been synthesized and characterized by X-ray diffraction, DTA-TG and cyclic30voltammetry.
8、We report our observations in this communication.NMeONOMe1Foundations: Specialized Research Fund for the Doctoral Program of Higher Education(No. 20096501110001) Brief author introduction:YANG Hongwei(1980-),male,research field:applied chemistryCorrespondance author: WANG Jide(1958-),male,Professor,
9、research field:applied chemistry. E-mail:- 6 -1Experimental351.1MaterialsThe IR spectra were recorded on a Bio-Rad FTS-40 spectrophotometer.The thermogravimetric analysis of the compound was studied (35-900C, 10k/min) with an air/30/N2/0 flow with NETZSCH STA 449C.1-(4-methoxybenzyl)-2-(4-methoxyphe
10、nyl)benzimidazole (1).40Prepared as previously reported and characterized by IR spectroscopy and x-ray diffraction4.1-(4-methoxybenzyl)-2-(4-methoxyphenyl)benzimidazole, cobalt(II) chloride complex (2). CoCl2 (1mmol) methanol solution was added to a methanol solution containing1-(4-methoxybenzyl)-2-
11、(4-methoxyphenyl)benzimidazole (2mmol). The solution was refluxed for454 h.After cooling to ambient temperature, blue crystals formed upon overnight standing.M.P.240-243 C. Anal. calc.for C44H40N4O4CoCl2: C,64.55; H,4.92; N,6.84.Found: C,64.68; H,5.18; N,6.87. IR(KBr):(C=N) (Imid),1454 cm-1 (s); (C-
12、N)(ph),1302 cm-1 (s); C-H (ph),3069 cm-1 (s); C-O-C(Ph-OCH3); 1027 cm-1; 819 cm-1.501.2X-ray data collectionCrystals were mounted on a Siemens P4 four-circle diffractometer, which employed graphite-monochromated MoK radiation (0.7103 ).Intensities were collected using the 2 scan mode. Absorption cor
13、rections were applied to the data set of each crystal using the -scan technique.The structures were solved by direct methods with successive Fourier syntheses.55Full-matrix least-squares refinement on F 2 was performed using SHELXTL-97 with anisotropic thermal parameters for all non-hydrogen atoms 5
14、-7. During data collection, three standard reflections were monitored for intensity variation.Table 1. Crystal Data and Structure Refinements for Complex 2. Empirical formula C44H40Cl2N4O4Co (2) Formula weight 818.63Temperature (K) 293(2)Crystal system MonoclinicSpace group P2/nCrystal size/mm 0.330
15、.270.09a ( ) 12.88 b/ 9.83 c/ 15.44/(o) 92.86V ( 3)1953.0(5)Z 2Dcalc. (mg/ m3) 1.39Absorption coefficient(cm-1) 6.25F(000) 850Index ranges -15h14,-11k12,-15l19 range for data collection 2.01 26.00 Parameters refined 278Goodness-of-fit 1.111Final R indices I 2(I)R indices (all data)R1=0.0693,R2 = 0.1
16、952R1=0.0895,R2 = 0.206960Table 2. Selected bond Lengths () and Bond Angles (deg) for complex 2. bond lengths ()Co-N1Co-N1Co-ClCo-Cl2.052(3)2.052(3)2.2580(2)2.2580(2)Angles ()N1-Co-N1N1-Co-Cl N1-Co-Cl N1-Co-Cl N1-Co-Cl Cl-Co-Cl C1-N1-CoC2-N1-Co110.98(2)113.02(1)107.10(1)107.10(1)113.02(1)105.59(1)12
17、9.5(2)124.4(2)1.3Electrochemical Measurements65Electrochemical measurements were carried out using traditional three-electrode system.In the fabrication of the electrodes, a mixture containing the freshly prepared complex, graphite and acetylene black (weight ratio of 8:2:1) was first mixed and grou
18、nded in an agate mortar. Then 1 wt.% PTFE solution was added to the mixture as a binder and it was pressed on a nickel substrate whose area wass about 1cm2 at 3107 kg/cm2 for 5 min to prepare the working electrode,70(thickness 1mm). A Hg/HgO electrode was used as the reference electrode, a platinum
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