Moon Dohyun, Choi Jong-Ha
Beamline Department, Pohang Accelerator Laboratory, POSTECH, Pohang 37673, Republic of Korea.
Department of Chemistry, Andong National University, Andong 36729, Republic of Korea.
Acta Crystallogr E Crystallogr Commun. 2021 Apr 30;77(Pt 5):569-572. doi: 10.1107/S2056989021004382. eCollection 2021 May 1.
The crystal structure of the novel hydrated Cu salt, [Cu()(HO)]Cl·4HO ( = 3,14-diethyl-2,6,13,17-tetra-aza-tri-cyclo-[16.4.0.0]docosane, CHN) has been determined using synchrotron radiation. The asymmetric unit contains one half of the [Cu()(HO)] cation (completed by crystallographic inversion symmetry), one chloride anion and two lattice water mol-ecules. The copper(II) atom exists in a tetra-gonally distorted octa-hedral environment with the four N atoms of the macrocyclic ligand in equatorial and two O atoms from water mol-ecules in axial positions. The latter exhibit a long axial Cu-O bond length of 2.7866 (16) Å due to the Jahn-Teller distortion. The macrocyclic ring adopts a stable -III conformation with typical Cu-N bond lengths of 2.0240 (11) and 2.0441 (3) Å. The complex is stabilized by hydrogen bonds formed between the O atoms of coordinated water mol-ecules and the NH groups as donors, and chloride anions as acceptors. The chloride anions are further connected to the lattice water solvent molecules through O-H⋯Cl hydrogen bonds, giving rise to a three-dimensional network structure.
新型水合铜盐[Cu()(HO)]Cl·4HO（= 3,14 - 二乙基 - 2,6,13,17 - 四氮杂三环[16.4.0.0]二十二烷，CHN）的晶体结构已通过同步辐射确定。不对称单元包含[Cu()(HO)]阳离子的一半（通过晶体学反演对称性完成）、一个氯离子阴离子和两个晶格水分子。铜（II）原子存在于一个四方畸变的八面体环境中，大环配体的四个N原子处于赤道位置，来自水分子的两个O原子处于轴向位置。由于 Jahn - Teller 畸变，后者呈现出较长的轴向 Cu - O 键长，为 2.7866 (16) Å。大环环采用稳定的 -III 构象，典型的 Cu - N 键长为 2.0240 (11) 和 2.0441 (3) Å。该配合物通过配位水分子的 O 原子与作为供体的 NH 基团以及作为受体的氯离子阴离子之间形成的氢键得以稳定。氯离子阴离子通过 O - H⋯Cl 氢键进一步与晶格水溶剂分子相连，形成三维网络结构。
