A new compound based on Preyssler-type P5W30 anion modified by CoII and flexible bis(benzimidazole) ligand

Inorganic Chemistry Communications

Volumn 14, Issue 1, 2011, Pages 103-106

  Wang, Xiuli ^a   Li, Jin ^a   Tian, Aixiang ^a   Lin, Hongyan ^a   Liu, Guocheng ^a   Hu, Hailiang ^a  

^a BOHAI UNIVERSITY   (China)

Author keywords

Benzimidazole; Cobalt cation; Electrochemical property; Polyoxometalates; Preyssler type anions

Indexed keywords

EID: 78651287825     PISSN: 13877003     EISSN: None     Source Type: Journal    
DOI: 10.1016/j.inoche.2010.09.042     Document Type: Article

References (50)

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39. Compound 1 was prepared by hydrothermal reaction of mixture of K12.5Na1.5[NaP5W30O110]•15H2O [15] (0.20 g, 0.03 mmol), CoCl2•6H2O (0.10 g, 0.42 mmol), bbbm (0.02 g, 0.07 mmol) and 10 mL of distilled water. After the pH value of the mixture was adjusted to about 6.4 with 0.1 mol•L-1 NaOH, the suspension was put into a Teflon-lined autoclave and kept under autogenous pressure at 160 °C for three days. After slow cooling to room temperature, red block crystals of 1 were obtained, washed with water (ca. 63% yield based on Co). Anal. Calcd for C234H308Co2N52O244P10W60: C 14.6, H 1.6, N 3.8. Found: C 14.8, H 1.5, N 3.9%.
40. Crystal data for 1: C234H308Co2N52O244P10W60, Mr = 19211.88, Triclinic, space group P-1, a = 16.4322(6) Å, b = 18.4361(7) Å, c = 34.1166(12) Å, α = 76.2370(10)° β = 88.9430(10)° γ = 71.9220(10)° V = 9526.0(6) Å 3, Z = 1, Dc = 3.362 g m-3, 1.74 < θ < 25.00, F(000) = 8712. Data collection T = 185(2) K, of 58, 460 reflections measured (- 19 ≤ h ≤ 19, - 21 ≤ k ≤ 21, - 35 ≤ l ≤ 40), 33, 423 [R(int) = 0.0328] independent reflections were used to solve the structure. Based on these data, final R1 = 0.0573 (all data), wR2 = 0.1481, and the goodness-of-fit on F2 is 1.051. The X-ray diffraction data were collected on a Bruker Smart 1000 CCD diffractometer with Mo Kα (λ = 0.71073 Å) by ω and θ scan mode at 296 K. The structure was solved by direct methods and refined on F2 by full-matrix least-squares using SHELXL-97 package [10]. All of the non-hydrogen atoms were refined anisotropically. Positions of the hydrogen atoms on carbon or nitrogen atoms were calculated theoretically.
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49. Electrochemical measurements were performed witn a CHI 440 Electrochemical Quartz Crystal Microbalance. A conventional three-electrode cell was used at room temperature. The modified electrode was used as working electrode. A SCE and a platinum wire were used as reference and auxiliary electrodes, respectively. The compound 1 bulk-modified carbon paste electrode (1-CPE) was fabricated as follows [20]: 0.50 g graphite powder and 0.030 g compound 1 was mixed and ground together by agate mortar and pestle for approximately 20 min to achieve an even, dry mixture; to the mixture 0.13 mL paraffin oil was added and stirred with a glass rod; then the homogenized mixture was used to pack 3 mm inner diameter glass tubes to a length of 0.8 cm, the surface of the modified CPE was wiped with weighing paper, and the electrical contact was established with the copper stick. The same procedure was used for preparation of bare CPE without compound 1.
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