Hydrothermal Synthesis, Crystal Structure of a Indium(Ⅲ) Complex with Benzene-1,2-dicarboxylate

水熱合成含銦（Ⅲ）-苯-1,2-二甲酸配位錯合物及結構分析

駱詩富(Shie-Fu Lush)；沈福銘(Fwu-Ming Shen)

水熱合成 ； 苯-1,2-二甲酸 ； 銦金屬 ； 氫鍵 ； Hydrothermal Synthesis ； Benzene-1,2-dicarboxylic acid ； Indium ； Hydrogen bonding

元培學報

20期（2013 / 12 / 01）

69 - 78

英文

將In_2(SO_4)_3∙9H_2O及苯-1,2-二甲酸加水混合，在溫度423 K下，利用水熱合成反應，得到含銦（Ⅲ）的配位化合物，其化學式為[In(1,2-BDC)(μ2-OH)(H_2O)]_n (1),(1,2-BDC = 苯-1,2-二甲酸根）。利用元素分析儀、FT-IR光譜儀及X-Ray晶體繞射儀測定產物晶體結構及性質。化合物1以銦(Ⅲ)離子為配位中心，配位六個氧原子，三個來自1,2-BDC的羧酸氧原子及一個配位水分子和兩個氫氧離子配位基，配位構成六配位且些微扭曲的正八面體型幾何結構，每個1,2-BDC配位基同時鄰接三個銦金屬。配位中心銦（Ⅲ）離子經由1,2-BDC配位基的連結形成二維的結構。晶體結構中含有傳統性的氫鍵作用力（O-H･･･O），以及芳香環之間的π･･･π吸引力，使的晶體結構更穩定。其中鄰近互相平行芳香環的雙面角為1.1(2)^0，兩個1,2-BDC的中心距離為3.671(3)Å。研究指出化合物1具有對掌異構物［弗萊克（Flack）參數為：0.48(3)］。

The title polymer compound, [In(1,2-BDC)(μ2-OH)(H_2O)]_n (1) , (1,2-BDC= benzene-1,2- dicarboxylate) has been synthesized by a hydrothermal reaction using In_2(SO_4)_3∙9H_2O, benzene-1,2- dicarboxylic acid and water at 423 K. The structure of 1 was characterized by elemental analysis, FT-IR and single-crystal X-ray diffraction. The asymmetric unit of compound 1 contains a six-coordinate In(Ⅲ) ion with a slightly distorted octahedral geometry, defined by six O atoms from one water molecules, three 1,2-BDC ligands and two hydroxyl ligands. Each 1,2-BDC ligand affords a three-connecting node. The In(Ⅲ) centers are interconnected through 1,2-BDC ligands to generate a two-dimensional layered structure. Classical O-H…O hydrogen bonding is observed in the crystal structure. The crystal structure is further consolidated by π…π stacking between nearly parallel aryl ring systems [dihedral angle = 1.1(2)°], the centroid…centroid distance between aromatic rings of adjacent 1,2-BDC ligands being 3.671(3)Å. The crystal was found to be a racemic twin, and the flack parameter is 0.48(3).