Pacifico Jessica, Stoeckli-Evans Helen
Institute of Chemistry, University of Neuchâtel, Av. de Bellevaux 51, CH-2000 Neuchâtel, Switzerland.
Institute of Physics, University of Neuchâtel, rue Emile-Argand 11, CH-2000 Neuchâtel, Switzerland.
Acta Crystallogr E Crystallogr Commun. 2021 Apr 9;77(Pt 5):480-490. doi: 10.1107/S2056989021003479. eCollection 2021 May 1.
Two polymorphs of the title tetra-kis-substituted pyrazine carb-oxy-lic acid, 3,3',3'',3'''-{[pyrazine-2,3,5,6-tetra-yltetra-kis-(methyl-ene))tetra-kis-(sulfanedi-yl]}tetra-propionic acid, CHNOS, (), have been obtained, and . Each structure crystallized with half a mol-ecule in the asymmetric unit of a triclinic unit cell. The whole mol-ecules are generated by inversion symmetry, with the pyrazine rings being located about inversion centers. The crystals of were of poor quality, but the X-ray diffraction analysis does show the change in conformation of the -CH-S-CH-CH- side chains compared to those in polymorph . In the crystal of , mol-ecules are linked by two pairs of O-H⋯O hydrogen bonds, enclosing (8) ring motifs forming layers parallel to plane (100), which are linked by C-H⋯O hydrogen bonds to form a supra-molecular framework. In the crystal of , mol-ecules are also linked by two pairs of O-H⋯O hydrogen bonds enclosing (8) ring motifs, however here, chains are formed propagating in the [001] direction and stacking up the -axis. Reaction of with Hg(NO) in the presence of a potassium acetate buffer did not produce the expected binuclear complex, instead crystals of a potassium-organic framework were obtained, poly[(μ-3-{[(3,5,6-tris-{[(2-carb-oxy-eth-yl)sulfan-yl]meth-yl}pyrazin-2-yl)meth-yl]sulfan-yl}propano-ato)potassium], [K(CHNOS)] (). The organic mono-anion possesses inversion symmetry with the pyrazine ring being located about an inversion center. A carb-oxy H atom is disordered by symmetry and the charge is compensated for by a potassium ion. A similar reaction with Zn(NO) resulted in the formation of crystals of a dipotassium-organic framework, poly[(μ-3,3'-{[(3,6-bis-{[(2-carb-oxy-eth-yl)sulfan-yl]meth-yl}pyrazine-2,5-di-yl)bis(methyl-ene)]bis-(sulfanedi-yl)}dipropionato)dipotassium], [K(CHNOS)] (). Here, the organic di-anion possesses inversion symmetry with the pyrazine ring being located about an inversion center. Two symmetry-related acid groups are deprotonated and the charges are compensated for by two potassium ions.
已获得标题化合物四 - (3,3',3'',3'''-{[吡嗪 - 2,3,5,6 - 四亚甲基)四 - (亚磺酰二基]}四丙酸)吡嗪羧酸的两种多晶型物,即CHNOS,()。每个结构在三斜晶胞的不对称单元中以半个分子结晶。整个分子通过反演对称性产生,吡嗪环位于反演中心周围。的晶体质量较差,但X射线衍射分析确实显示出与多晶型物中的相比,-CH - S - CH - CH - 侧链构象的变化。在的晶体中,分子通过两对O - H⋯O氢键相连,形成(8)环 motif,形成平行于(100)平面的层,这些层通过C - H⋯O氢键相连形成超分子框架。在的晶体中,分子也通过两对O - H⋯O氢键相连,形成(8)环 motif,然而在这里,链沿[001]方向延伸并沿轴堆积。在醋酸钾缓冲液存在下,与Hg(NO)反应未产生预期的双核配合物,而是得到了一种钾 - 有机骨架晶体,聚[(μ - 3 - {[(3,5,6 - 三 - {[(2 - 羧基乙基)磺酰基]甲基}吡嗪 - 2 - 基)甲基]磺酰基}丙酸根)钾],[K(CHNOS)] ()。有机单阴离子具有反演对称性,吡嗪环位于反演中心周围。一个羧基H原子通过对称性无序排列,电荷由一个钾离子补偿。与Zn(NO)的类似反应导致形成二钾 - 有机骨架晶体,聚[(μ - 3,3'-{[(3,6 - 双 - {[(2 - 羧基乙基)磺酰基]甲基}吡嗪 - 2,5 - 二亚基)双(亚甲基)]双(亚磺酰二基)}二丙酸根)二钾],[K(CHNOS)] ()。在这里,有机二阴离子具有反演对称性,吡嗪环位于反演中心周围。两个对称相关的酸基团去质子化,电荷由两个钾离子补偿。