Citation: JIANG Qi-Fei, YANG Wen-Bin, WU Xiao-Yuan, LU Can-Zhong. Syntheses and Structural Characterizations of a Series of Capped Keggin Derivatives[J]. Chinese Journal of Structural Chemistry, ;2014, 33(11): 1703-1712. doi: 10.14102/j.cnki.0254-5861.2011-0353 shu

Syntheses and Structural Characterizations of a Series of Capped Keggin Derivatives

1.
State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002, China

Corresponding author: YANG Wen-Bin, LU Can-Zhong,
Received Date: 25 April 2014
Available Online: 15 July 2014
Fund Project: Supported by the 973 key program of the MOST (2010CB933501, 2012CB821705) (2010CB933501, 2012CB821705) the Chinese Academy of Sciences (KJCX2-YW-319, KJCX2-EW-H01) (KJCX2-YW-319, KJCX2-EW-H01) the National Natural Science Foundation of China (21373221, 21221001, 91022008, 91122027, 51172232) (21373221, 21221001, 91022008, 91122027, 51172232)the Natural Science Foundation of Fujian Province (2011HZ0001-1, 2012J06006, 2006L2005) (2011HZ0001-1, 2012J06006, 2006L2005)

Hydrothermal reactions of Na₂MoO₂·2H₂O and NH₄VO₃ (or V₂O₅) with appropriate reducing agents such as organic amines, NH₂OH·HCl and Mo(CO)₆ gave rise to the formation of a series of capped Keggin derivatives, [N(CH₃)₄]₂Na₃(NH₄)₂[(V^ⅤO₄)Mo₈^ⅥV₄^ⅣO₃₆(V^ⅣO)₂]·13H₂O (1), [NH₄]₇[(V^ⅤO₄)Mo₈^ⅥV₄^ⅣO₃₆(V^ⅣO)₂]·7H₂O (2), [HN(CH₂CH₂)₃NH][(PO₄)Mo₃^ⅤMo₉^ⅥO₃₆(V^ⅣO)₂]·3[N(CH₂CH₂)₃N]·(en)·4.5H₂O (3) and [HNH₂OH][NH₄]₂[(V^ⅤO₄)Mo₈^ⅥV₄^ⅣO₃₆(V^ⅣO)₄]·24H₂O (4). Single-crystal X-ray diffraction analysis revealed that the anions in 1~3 are two-capped Keggin derivatives with characteristic trans vanadium-oxygen caps, whereas the heteropoly anion in 4 is a tetra-capped α-Keggin derivative with characteristic vanadium-oxygen caps on the equatorial plane.
- heteropoly polyoxometalates,
- capped Keggin derivatives,
- hydrothermal synthesis and crystal structures
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