Soleimannejad Janet, Aghabozorg Hossein, Golenji Yaghoub Mohammadzadeh Azar, Attar Gharamaleki Jafar, Adams Harry
Acta Crystallogr Sect E Struct Rep Online. 2008 Jan 23;64(Pt 2):m387-8. doi: 10.1107/S1600536808001372.
The reaction of anti-mony(III) chloride, 4,4'-bipyridine (4,4'-bipy) and pyridine-2,6-dicarboxylic acid (pydcH(2)), in a 1:2:2 molar ratio in an aqueous solution, resulted in the formation of the title centrosymmetric disordered mixed-valence Sb(III)/Sb(V) compound, (C(10)H(9)N(2))(2)[Sb(2)(C(7)H(3)NO(4))(2)(OH)(6)]·8H(2)O or (4,4'-bipyH)(2)Sb(pydc)(OH)(2)(μ-OH)·8H(2)O. The seven donor atoms of the (pydc)(2-) groups and the hydroxido ligands form a distorted penta-gonal-bipyramidal arrangement around the Sb(III)/Sb(V) centers. C-H⋯π stacking inter-actions between CH groups of the complex dianion and the aromatic rings of the (4,4'-bipyH)(+) cations, with a distance of 2.89 Å, are observed. In the crystal structure, a wide range of noncovalent inter-actions, consisting of O-H⋯O, N-H⋯O and C-H⋯O hydrogen bonds [D⋯A ranging from 2.722 (2) to 3.137 (3) Å], ion pairing, π-π stacking [centroid-centroid distance of 3.4363 (13) Å] and C-H⋯π inter-actions, connect the various components into a supra-molecular structure.
在水溶液中，按1:2:2的摩尔比使三氯化锑（III）、4,4'-联吡啶（4,4'-bipy）和吡啶-2,6-二羧酸（pydcH₂）发生反应，生成了标题中心对称的无序混合价态Sb(III)/Sb(V)化合物，(C₁₀H₉N₂)₂[Sb₂(C₇H₃NO₄)₂(OH)₆]·8H₂O或(4,4'-bipyH)₂[Sb(pydc)(OH)₂(μ-OH)]₂·8H₂O。(pydc)²⁻基团的七个供体原子和羟基配体在Sb(III)/Sb(V)中心周围形成了扭曲的五角双锥排列。观察到配合物二价阴离子的CH基团与(4,4'-bipyH)⁺阳离子的芳香环之间存在C-H⋯π堆积相互作用，距离为2.89 Å。在晶体结构中，由O-H⋯O、N-H⋯O和C-H⋯O氢键[D⋯A范围为2.722(2)至3.137(3) Å]、离子对、π-π堆积[质心-质心距离为3.4363(13) Å]和C-H⋯π相互作用组成的多种非共价相互作用，将各种组分连接成一个超分子结构。
