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Volumn 14, Issue 5, 2011, Pages 697-701

A new 3D framework constructed from oxo-bridged Keggin chains and metallamacrocyclic polymer chains

Author keywords

Flexible bis(triazole) ligand; Hydrothermal synthesis; Keggin polyoxometalate; Metallamacrocyclic structure

Indexed keywords


EID: 79954424204     PISSN: 13877003     EISSN: None     Source Type: Journal    
DOI: 10.1016/j.inoche.2011.02.009     Document Type: Article
Times cited : (15)

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    • note
    • Compound 1 was prepared under hydrothermal condition. The mixture of Na2WO4•2H2O (0.8 g, 2.4 mmol), Cu(CH3COO)2•2H2O (0.24 g, 1.1 mmol), btp (0.09 g, 0.5 mmol), and 0.2 mL of H3PO4 (85%) was dissolved in 10 mL of distilled water at room temperature. When the pH value of the mixture was adjusted to about 4.1 with 1.0 mol•L-1 HCl, the suspension was put into a Teflon-lined autoclave and kept under autogenous pressure at 160 °C for 3 days. After slow cooling to room temperature, orange block crystals were filtered and washed with distilled water (40% yield based on W). Anal. Calcd for C28H48Cu6N24O43PW11 (3843): C 8.75, H 1.25, N 8.75. Found: C 8.68, H 1.22, N 8.65.
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    • note
    • Crystal data for compound 1: C28H48Cu6N24O43PW11, FW = 3843, Triclinic, space group P1, a = 10.9698(9) Å, b = 13.6642(12) Å, c = 13.9254(12) Å, α = 64.8830(10)o, β = 73.1470(10)o, γ = 69.8210(10)o, V = 1748.5(3) Å3, Z = 1, Dcalc = 3.642 mg/m3, λ = 0.71073 Å, T = 293(2)K, R1 (wR2) = 0.0602 (0.1619), Bruker Smart Apex-II CCD area detector, Mo Kα radiation. The structure was solved by direct methods and refined on F2 by full-matrix least squares methods using SHELXTL 97. CCDC reference number 801255.
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