Zakharchenko Borys V, Khomenko Dmytro M, Doroshchuk Roman O, Bargan Alexandra, Vassilyeva Olga Yu, Lampeka Rostyslav D
Department of Chemistry, Taras Shevchenko National University of Kyiv, Volodymyrska str. 64/13, 01601 Kyiv, Ukraine.
Enamine Ltd. (www.enamine.net), Winston Churchill str. 78, 02094 Kyiv, Ukraine.
Acta Crystallogr E Crystallogr Commun. 2024 May 3;80(Pt 6):567-571. doi: 10.1107/S205698902400392X. eCollection 2024 May 1.
The new palladium(II) complex, Pd(CHNO)·2CFCOOH, crystallizes in the triclinic space group with the asymmetric unit containing half the cation (Pd site symmetry ), one tri-fluoro-actetate anion and one co-crystallized tri-fluoro-acetic acid mol-ecule. Two neutral chelating 2-[5-(3,4,5-tri-meth-oxy-phen-yl)-4-1,2,4-triazol-3-yl]pyridine ligands coordinate to the Pd ion through the triazole-N and pyridine-N atoms in a distorted -PdN square-planar configuration [Pd-N 1.991 (2), 2.037 (2) Å; N-Pd-N 79.65 (8), 100.35 (8)°]. The complex cation is quite planar, except for the methoxo groups (δ = 0.117 Å for one of the C atoms). The planar configuration is supported by two intra-molecular C-H⋯N hydrogen bonds. In the crystal, the π-π-stacked cations are arranged in sheets parallel to the plane that are flanked on both sides by the tri-fluoro-acetic acid-tri-fluoro-acetate anion pairs. Apart from classical N/O-H⋯O hydrogen-bonding inter-actions, weak C-H⋯F/N/O contacts consolidate the three-dimensional architecture. Both tri-fluoro-acetic moieties were found to be disordered over two resolvable positions with a refined occupancy ratio of 0.587 (1):0.413 (17) and 0.530 (6):0.470 (6) for the protonated and deprotonated forms, respectively.
新型钯（II）配合物Pd(CHNO)·2CFCOOH以三斜晶系空间群结晶，不对称单元包含半个阳离子（钯位点对称性 ）、一个三氟乙酸根阴离子和一个共结晶的三氟乙酸分子。两个中性螯合的2-[5-(3,4,5-三甲氧基苯基)-4-1,2,4-三唑-3-基]吡啶配体通过三唑-N和吡啶-N原子以扭曲的 -PdN平面正方形构型与钯离子配位[Pd-N 1.991 (2)，2.037 (2) Å；N-Pd-N 79.65 (8)，100.35 (8)°]。除了甲氧基（其中一个C原子的δ = 0.117 Å）外，配合物阳离子相当平面。这种平面构型由两个分子内C-H⋯N氢键支撑。在晶体中，π-π堆积的阳离子排列成平行于 平面的片层，两侧是三氟乙酸-三氟乙酸根阴离子对。除了经典的N/O-H⋯O氢键相互作用外，弱的C-H⋯F/N/O接触巩固了三维结构。发现两个三氟乙酸部分在两个可分辨位置上无序排列，质子化和去质子化形式的精修占有率分别为0.587 (1):0.413 (17)和0.530 (6):0.470 (6)。
