双[2-(2-咪唑啉基)苯酚]锌(II)的合成与晶体结构

IF 0.1 Q4 CRYSTALLOGRAPHY
R. Mitsuhashi, M. Mikuriya
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引用次数: 1

摘要

钴(II)配合物在过去二十年中因其在单分子磁体中的潜在应用而得到了广泛的研究。1为了准确了解静态和动态磁性,合成和结晶具有抗磁性过渡金属离子的类似配合物是很重要的。最近,我们报道了双[2-(2-咪唑基)苯酚基]钴(II)配合物的晶体结构和单离子磁体(SIM)行为。2该配合物是3dSIM的一个罕见例子,在零场下表现出缓慢的磁弛豫。零场SIM行为的起源被认为是由配合物的氢键链结构引起的分子间磁相互作用。为了研究分子间相互作用对静态和动态磁性的影响,有必要使具有抗磁性离子的同晶配合物结晶。在这项研究中,我们报道了锌(II)类似物双[2-(2-咪唑基)苯酚基]锌(Ⅱ)的合成、晶体结构和氢键相互作用(图1)。配体前体2-(2-咪唑基)苯酚(H2imn)是通过先前报道的程序合成的。3 He报道了类似于标题化合物的锌(II)络合物,尽管该化合物包括甲醇分子作为结晶溶剂。4为了获得与[Co(Himn)2]同晶的锌(Ⅱ)络合物,我们采用了相同的合成程序,2将10mL KOtBu(45.4mg)和H2imn(65.7mg)的甲醇溶液与10mL ZnCl2(27.9mg)的空气甲醇溶液混合后,立即形成[Zn(Himn)2]的无色晶体,同时在Ar气氛下合成钴(II)类似物。产量:63.3 mg(80%)。晶体数据包含在表1中。在Bruker智能APEX CCD衍射仪上在90K下收集X射线晶体学数据。使用SADABS对积分和缩放数据进行经验校正。5使用SHELXT-2014通过本征定相法求解初始结构,6并使用SHELXL-2014在F2上使用全矩阵最小二乘法进行细化。7非氢原子进行了细化2019©日本分析化学学会
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Synthesis and Crystal Structure of Bis[2-(2-imidazolinyl)phenolato]zinc(II)
Cobalt(II) complexes have been extensively investigated in the last two decades owing to potential application to singlemolecule magnets.1 To precisely understand the static and dynamic magnetic properties, the synthesis and crystallization of an analogous complex with a diamagnetic transition metal ion is important. Recently, we have reported on the crystal structure and single-ion magnet (SIM) behavior of the bis[2-(2imidazolinyl)phenolato]cobalt(II) complex.2 This complex is a rare example of 3d SIM, which shows slow magnetic relaxation under zero field. The origin of the zero-field SIM behavior was suggested to be intermolecular magnetic interactions arising from the hydrogen-bonded chain structure of the complex. To investigate the effect of intermolecular interactions on the static and dynamic magnetic property, the crystallization of an isomorphous complex with a diamagnetic ion is necessary. In this study, we report on the synthesis, crystal structure and hydrogen-bonded interactions of a zinc(II) analogue, bis[2-(2imidazolinyl)phenolato]zinc(II) (Fig. 1). The ligand precursor, 2-(2-imidazolinyl)phenol (H2imn), was synthesized by a previously reported procedure.3 A zinc(II) complex analogous to the title compound was reported by He, although this compound includes a methanol molecule as a solvent of crystallization.4 To obtain a zinc(II) complex isomorphous to [Co(Himn)2], we employed the same synthetic procedure, except for the reaction condition.2 Colorless crystals of [Zn(Himn)2] were immediately formed upon mixing a 10-mL methanol solution of KOtBu (45.4 mg) and H2imn (65.7 mg) and a 10-mL methanol solution of ZnCl2 (27.9 mg) in air, while the cobalt(II) analogue was synthesized under an Ar atmosphere. Yield: 63.3 mg (80%). The crystal data are included in Table 1. X-ray crystallographic data were collected on a Bruker smart APEX CCD diffractometer at 90 K. The integrated and scaled data were empirically corrected with SADABS.5 The initial structure was solved by an intrinsic phasing method with SHELXT-2014,6 and refined using the full-matrix least-squares method on F2 utilizing SHELXL-2014.7 The non-hydrogen atoms were refined 2019 © The Japan Society for Analytical Chemistry
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来源期刊
CiteScore
0.60
自引率
50.00%
发文量
17
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