Structural and catalytic performance of a polyoxometalate-based metal-organic framework having a lanthanide nanocage as a secondary building block

Inorganic Chemistry

Volumn 49, Issue 4, 2010, Pages 1280-1282

  Dang, Dongbin ^a,b   Bai, Yan ^b   He, Cheng ^a   Wang, Jian ^a   Duan, Chunying ^a   Niu, Jingyang ^b  

^a DALIAN UNIVERSITY OF TECHNOLOGY   (China)

^b HENAN UNIVERSITY   (China)

Author keywords

[No Author keywords available]

Indexed keywords

EID: 77249162788     PISSN: 00201669     EISSN: None     Source Type: Journal    
DOI: 10.1021/ic901504q     Document Type: Article

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46. Compound 1 was prepared from a hydrothermal reaction by putting R-HoH2BW12O40 3 nH2O, HoCl3 36H2O, 4, 40-bipyridine-N, N0-dioxide hydrate, hexahydropyrazine, and water with a molar ratio of 1:3:3:7:1600 into a Teflon-lined stainless steel autoclave and keeping the resulting mixture under autogenous pressure at 120Ćfor 3 days. Yellow crystals suitable for single-crystal X-ray structure analysis were isolated and washed with distilled water (about 70% yield based on HoH2BW12O40 3 nH2O). Anal. Calcd for C128H175B3Ho4N28O172W36: C, 12.63; H, 1.45; N, 3.22; B, 0.27; W, 54.39; Ho, 5.42. Found: C, 12.55; H, 1.50; N, 3.20; B, 0.25; W, 54.19; Ho, 5.52. IR (KBr, cm-1): three characteristic asymmetric vibrations from heteropolyanions, ν (W-Oc) 809, ν (B-Oa) 905, ν (B-Od) 955; four characteristic vibrations from dpdo molecules, ν (N-O) 1227, ν (ring) 1473, ν (C-H, in-plane) 1180, ν (N-O) 839.
47. Crystal data of 1 for C128H175B3Ho4N28O172W36, Mr = 12 168.71, triclinic, space group P1 with a = 18.922 (1) A °, b = 20.038 (1) A °, c = 20.789 (1) A °, V=6160.4 (3) A ° 3; Z=1; Fcalcd=3.280 g cm-3; T=293 (2) K. The final refinement gave R1=0.0598, wR2=0.1270, and GOF=1.03 for 11 697 observed reflections with I > 2σ (I) Hydrolysis of BNPP in the absence of a metal complex was almost negligible, compared to that of the catalytic reaction; however, the final value of kobs was also adjusted for the background cleavage.
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49. The pH of the solutions was adjusted with hydrochloric acid and NaOH and measured before and after the hydrolysis reaction.
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