双核镨(III)配合物N,N ' -双(2-羟基-3,5-二甲基苄基)-N,N ' -二甲基-1,2-乙二胺

IF 0.1 Q4 CRYSTALLOGRAPHY
M. Mikuriya, Chika Kawai, Kana Nagai, Akiko Morita, Asuka Kanemori, D. Yoshioka, M. Tsuboi
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In this study, we successfully synthesized a praseodymium complex with hdde2– and determined the crystal structure in order to elucidate the dinuclear molecule (Fig. 1). The ligand H2hdde was synthesized by a method described in the literature.11 The complex was prepared by a reaction of H2hdde and praseodymium(III) salt. To a methanol solution (5 cm3) of H2hdde (53.9 mg, 0.15 mmol) was added 35.9 mg (0.1 mmol) of praseodymium(III) acetate dihydrate, and then six drops of triethylamine were added into the reaction mixture to obtain a pale-green precipitate. The precipitate was collected and dried under a vacuum. Yield, 51.2 mg (84.6%). Anal. Found: C, 49.21; H, 6.35; N, 4.25%. Calcd for C50H78N4O12Pr2[Pr2(hdde)2(CH3COO)2(CH3OH)2]·2H2O: C, 49.67; H, 6.50; N, 4.63%. IR (KBr, cm–1): 3320 ν(OH), 2980 νas(CH3), 2916 νas(CH2), 2854 νs(CH3), 2808 νs(CH2), 1556 νas(COO), 1476 δ(CH3), 1425 νs(COO). X-ray quality crystals were grown by recrystallization from methanol–dichloromethane. X-ray diffraction data were collected on a Bruker CCD X-ray diffractometer (SMART APEX) using graphite-monochromated Mo-Kα radiation. Crystal data and details concerning the data collection are given in Table 1. The structure was solved by an intrinsic phasing method and refined by full-matrix least-squares methods. The hydrogen atoms were inserted at their calculated positions, and fixed there, except for the hydrogen atom attached to the O5 atom of the coordinated methanol molecule, which was located from a D-Fourier map. All of the calculations were carried out on a Windows 7 Core i5 computer utilizing the SHELXT-201412 and SHELXL-2014.13 Crystallographic data have been deposited with Cambridge Crystallographic Data Centre (Deposit number CCDC-2091175). Copies of the data can be obtained free of charge via http://www.ccdc.cam.ac.uk/conts/ retrieving.html (or from the Cambridge Crystallographic Data Centre, 12, Union Road, Cambridge, CB2 1EZ, UK; Fax, +44 1223 336033; e-mail, deposit@ccdc.cam.ac.uk). A single-crystal X-ray structure analysis revealed that the molecule is a centrosymmetric dinuclear praseodymium complex. The asymmetric unit consists of one half of a [Pr2(hdde)2(CH3COO)2(CH3OH)2] complex and one dichloromethane molecule. 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The ligand H2hdde was synthesized by a method described in the literature.11 The complex was prepared by a reaction of H2hdde and praseodymium(III) salt. To a methanol solution (5 cm3) of H2hdde (53.9 mg, 0.15 mmol) was added 35.9 mg (0.1 mmol) of praseodymium(III) acetate dihydrate, and then six drops of triethylamine were added into the reaction mixture to obtain a pale-green precipitate. The precipitate was collected and dried under a vacuum. Yield, 51.2 mg (84.6%). Anal. Found: C, 49.21; H, 6.35; N, 4.25%. Calcd for C50H78N4O12Pr2[Pr2(hdde)2(CH3COO)2(CH3OH)2]·2H2O: C, 49.67; H, 6.50; N, 4.63%. IR (KBr, cm–1): 3320 ν(OH), 2980 νas(CH3), 2916 νas(CH2), 2854 νs(CH3), 2808 νs(CH2), 1556 νas(COO), 1476 δ(CH3), 1425 νs(COO). X-ray quality crystals were grown by recrystallization from methanol–dichloromethane. X-ray diffraction data were collected on a Bruker CCD X-ray diffractometer (SMART APEX) using graphite-monochromated Mo-Kα radiation. 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引用次数: 0

摘要

N,N ' -双(2-羟基-3,5-二甲基苄基)-N,N ' -二甲基-1,2乙二胺(H2hdde)是一种四齿N2O2配体,类似于著名的四齿希夫碱,N,N ' -乙烯双(水杨基亚胺),H2salen,但具有两个饱和的C-N键,不同于H2salen配体迄今为止,关于H2hdde配体已报道了单核钒、2核锰、3核铁、4核钼配合物,双核钒、2核铁、6核锰、3,7核锰、3核锌、8核镉、8核镍、9核镍、9和七核镍配合物。在我们的实验室里,我们的目标是将这种配体的配位化学扩展到稀土元素。在本研究中,我们成功地合成了一种与hdde2 -的镨配合物,并测定了晶体结构,以阐明双核分子(图1)。配体H2hdde的合成方法见文献该配合物由H2hdde和镨(III)盐反应制备。在H2hdde (53.9 mg, 0.15 mmol)的甲醇溶液(5 cm3)中加入35.9 mg (0.1 mmol)的二水合醋酸镨(III),再加入6滴三乙胺,得到淡绿色沉淀。沉淀物被收集起来,在真空下干燥。产率:51.2 mg(84.6%)。分析的发现:C, 49.21;H, 6.35;N, 4.25%。C50H78N4O12Pr2[Pr2(hdde)2(CH3COO)2(CH3OH)2]·2H2O: C, 49.67;H, 6.50;N, 4.63%。IR (KBr, cm-1): 3320 ν(OH), 2980 νas(CH3), 2916 νas(CH2), 2854 νs(CH3), 2808 νs(CH2), 1556 νas(COO), 1476 δ(CH3), 1425 νs(COO)。用甲醇-二氯甲烷重结晶法生长出x射线质量的晶体。采用石墨-单铬化Mo-Kα辐射,在Bruker CCD x射线衍射仪(SMART APEX)上采集x射线衍射数据。晶体数据和有关数据收集的详细信息见表1。该结构采用内禀相位法求解,并采用全矩阵最小二乘法进行细化。氢原子被插入到它们计算的位置,并固定在那里,除了氢原子附着在配位甲醇分子的O5原子上,这是根据d -傅里叶图定位的。所有的计算都是在一台Windows 7 Core i5计算机上进行的,使用的是SHELXT-201412和SHELXL-2014.13晶体学数据已存放在剑桥晶体学数据中心(保存号为CCDC-2091175)。数据副本可通过http://www.ccdc.cam.ac.uk/conts/ retrieving.html免费获得(或从剑桥晶体学数据中心,12,Union Road, Cambridge, CB2 1EZ, UK;传真:+44 1223 336033;电子邮件deposit@ccdc.cam.ac.uk)。单晶x射线结构分析表明该分子为中心对称双核镨配合物。不对称单元由一半的[Pr2(hdde)2(CH3COO)2(CH3OH)2]配合物和一个二氯甲烷分子组成。由ORTEP绘制的分子结构显示于2021年©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。
Dinuclear Praseodymium(III) Complex with N,N′-Bis(2-hydroxy-3,5-dimethylbenzyl)-N,N′-dimethyl-1,2-ethanediamine
N,N′-Bis(2-hydroxy-3,5-dimethylbenzyl)-N,N′-dimethyl-1,2ethanediamine (H2hdde) is a tetradentate N2O2 ligand similar to the famous tetradentate Schiff-base, N,N′-ethylenebis(salicylideneimine), H2salen, but with two saturated C–N bonds, being different from the H2salen ligand.1 So far, mononuclear vanadium,2 manganese,3 iron,4 and molybdenum5 complexes, dinuclear vanadium,2 dinuclear iron,6 trinuclear manganese,3,7 tetranuclear manganese,3 tetranuclear zinc,8 tetranuclear cadmium,8 tetranuclear nickel,9 hexanuclear nickel,9 and heptanuclear nickel10 complexes were reported concerning the H2hdde ligand. In our laboratory, we have aimed to extend the coordination chemistry of this ligand to the rare-earth elements. In this study, we successfully synthesized a praseodymium complex with hdde2– and determined the crystal structure in order to elucidate the dinuclear molecule (Fig. 1). The ligand H2hdde was synthesized by a method described in the literature.11 The complex was prepared by a reaction of H2hdde and praseodymium(III) salt. To a methanol solution (5 cm3) of H2hdde (53.9 mg, 0.15 mmol) was added 35.9 mg (0.1 mmol) of praseodymium(III) acetate dihydrate, and then six drops of triethylamine were added into the reaction mixture to obtain a pale-green precipitate. The precipitate was collected and dried under a vacuum. Yield, 51.2 mg (84.6%). Anal. Found: C, 49.21; H, 6.35; N, 4.25%. Calcd for C50H78N4O12Pr2[Pr2(hdde)2(CH3COO)2(CH3OH)2]·2H2O: C, 49.67; H, 6.50; N, 4.63%. IR (KBr, cm–1): 3320 ν(OH), 2980 νas(CH3), 2916 νas(CH2), 2854 νs(CH3), 2808 νs(CH2), 1556 νas(COO), 1476 δ(CH3), 1425 νs(COO). X-ray quality crystals were grown by recrystallization from methanol–dichloromethane. X-ray diffraction data were collected on a Bruker CCD X-ray diffractometer (SMART APEX) using graphite-monochromated Mo-Kα radiation. Crystal data and details concerning the data collection are given in Table 1. The structure was solved by an intrinsic phasing method and refined by full-matrix least-squares methods. The hydrogen atoms were inserted at their calculated positions, and fixed there, except for the hydrogen atom attached to the O5 atom of the coordinated methanol molecule, which was located from a D-Fourier map. All of the calculations were carried out on a Windows 7 Core i5 computer utilizing the SHELXT-201412 and SHELXL-2014.13 Crystallographic data have been deposited with Cambridge Crystallographic Data Centre (Deposit number CCDC-2091175). Copies of the data can be obtained free of charge via http://www.ccdc.cam.ac.uk/conts/ retrieving.html (or from the Cambridge Crystallographic Data Centre, 12, Union Road, Cambridge, CB2 1EZ, UK; Fax, +44 1223 336033; e-mail, deposit@ccdc.cam.ac.uk). A single-crystal X-ray structure analysis revealed that the molecule is a centrosymmetric dinuclear praseodymium complex. The asymmetric unit consists of one half of a [Pr2(hdde)2(CH3COO)2(CH3OH)2] complex and one dichloromethane molecule. The molecular structure, drawn by ORTEP, is shown 2021 © The Japan Society for Analytical Chemistry
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CiteScore
0.60
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