期刊
DALTON TRANSACTIONS
卷 41, 期 2, 页码 581-589出版社
ROYAL SOC CHEMISTRY
DOI: 10.1039/c1dt10985e
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资金
- Slovenian Research Agency [P2-0145, P2-030]
- Slovene Human Resources Development and Scholarship Fund
The title compound has been synthesized under solvothermal conditions by reacting vanadium(V) oxytriisopropoxide with terephthalic acid in N, N-dimethylformamide. A combination of synchrotron powder diffraction, infrared spectroscopy, scanning and transmission electron microscopy, and thermal and chemical analysis elucidated the chemical, structural and microstructural features of a new 2D layered inorganic-organic framework. Due to the low-crystallinity of the final material, its crystal structure has been solved from synchrotron X-ray powder diffraction data using a direct space global optimization technique and subsequent constraint Rietveld refinement. [V4O4(OH)(2)(O2CC6H4CO2)(4)]center dot DMF crystallizes in the monoclinic system (space group P2/m (No. 10)); cell parameters: a = 20.923(4) angstrom, b = 5.963(4) angstrom, c = 20.425(1) angstrom, beta = 123.70(6)degrees, V = 2120.1(9) angstrom(3), Z = 2. The overall structure can be described as an array of parallel 2D layers running along [-101] direction, consisting of two types of vanadium oxidation states and coordination polyhedra: face-shared trigonal prisms (V4+) and distorted corner-shared square pyramids (V5+). Both configurations form independent parallel chains oriented along the 2-fold symmetry crystallographic b-axis mutually interlinked with terephthalate ligands in a monodentate mode perpendicular to it. The morphology of the compound exhibits long nanofibers, with the growth direction along the layered [-101] axis. The magnetic susceptibility measurements show that the magnetic properties of [V4O4(OH)(2)(O2CC6H4CO2)(4)]center dot DMF can be described by a linear antiferromagnetic chain model, with the isotropic exchange interaction of J = -75 K between the nearest V4+ neighbours of S = 1/2.
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