Ben Khélifa Arbia, Giorgi Michel, Belkhiria Mohamed Salah
Acta Crystallogr Sect E Struct Rep Online. 2012 Jul 1;68(Pt 7):m938-9. doi: 10.1107/S1600536812025949. Epub 2012 Jun 16.
The title complex, Ce(C(2)H(6)OS)(8)Mo(6)O(19)·4C(2)H(6)OS, was obtained as a byproduct of the reaction of (C(4)H(9))(4)N[Mo(6)O(19)] with Ce(NO(3))(3)·6H(2)O and phthalic acid in dimethyl-sulfoxide solution. The asymmetric unit consists of a complex Ce(C(2)H(6)OS)(8) cation, one and a half of the Lindqvist-type Mo(6)O(19) polyanions and two dimethyl-sulfoxide solvent mol-ecules; the half polyanion lies on an inversion center. The Ce(3+) ion is coordinated by eight dimethyl-sulfoxide ligands through the O atoms in the form of a distorted square antiprism. The Ce-O bond lengths range from 2.429 (6) to 2.550 (5) Å. The cohesion of the structure is ensured by S⋯O [3.115 (6), 3.242 (10) and 3.12 (3) Å], O⋯O [3.037 (10) Å] and C-H⋯O inter-actions between cations and anions. The S and C atoms of a dmso ligand are disordered over three sites in a 0.45:0.30:0.25 ratio. The dimethyl-sulfoxide solvent mol-ecules are highly disordered and could not be modelled successfully; their contribution was therefore removed from the refinement using the SQUEEZE routine in PLATON [Spek (2009 ▶). Acta Cryst. D65, 148-155]. Potential solvent-accessible voids of 500.0 Å(3) occur in the crystal structure.
标题配合物[Ce(C₂H₆OS)₈]₂[Mo₆O₁₉]₃·4C₂H₆OS是[(C₄H₉)₄N]₂[Mo₆O₁₉]与Ce(NO₃)₃·6H₂O及邻苯二甲酸在二甲基亚砜溶液中反应的副产物。不对称单元由一个[Ce(C₂H₆OS)₈]³⁺阳离子配合物、一个半Lindqvist型[Mo₆O₁₉]²⁻聚阴离子和两个二甲基亚砜溶剂分子组成；半个聚阴离子位于对称中心上。Ce³⁺离子通过O原子与八个二甲基亚砜配体配位，呈扭曲的四方反棱柱形式。Ce - O键长范围为2.429(6)至2.550(5)Å。阳离子和阴离子之间的S⋯O[3.115(6)、3.242(10)和3.12(3)Å]、O⋯O[3.037(10)Å]和C - H⋯O相互作用确保了结构的凝聚性。一个二甲基亚砜配体的S和C原子在三个位置上无序排列，比例为0.45:0.30:0.25。二甲基亚砜溶剂分子高度无序，无法成功建模；因此使用PLATON中的SQUEEZE程序[Spek(2009 ▶). Acta Cryst. D65, 148 - 155]从精修中去除了它们的贡献。晶体结构中存在500.0 ų的潜在溶剂可及空隙。
