X-ray Structure Analysis Online最新文献

英文中文

Crystal Structure of a Lantern-type Dirhodium(II) Complex with Axial Pyridine Molecules cis-[Rh2(4-Me-pf )2(O2CCMe3)2(py)2], 4-Me-pf− = N,N′-Di-p-tolylformamidinate Anion Lantern型铱（II）与吡啶轴分子顺式-[Rh2（4-Me-pf）配合物的晶体结构 )2（O2CCMe3）2（py）2]，4-Me-pf−=N，N′-二对甲苯磺酰亚胺阴离子

IF 0.2 Q4 Materials Science

X-ray Structure Analysis Online

Pub Date : 2021-11-10 DOI: 10.2116/xraystruct.37.69

M. Handa, Makoto Kano, Natsumi Yano, M. Mikuriya, Y. Kataoka

The complexes [M2(O2CR)4] (m = 0 – 2), in which two transition metal ions are bridged with four μ-carboxylato bidentate ligands, are called lantern-type (or paddlewheel type) diuclear complexes from the view point of their molecular structures.1 The axial sites of the dinuclear complexes are coordinated by linkage ligands, such as pyrazine, to produce the assembled polymer complexes. The polymer complexes have been attracting many chemists concerning their interesting properties. For instance, nitrogen gas occulusion properties have been found for polymer complexes [Cu2(O2CPh)4(pyz)]n and [Rh2(O2CPh)4(pyz)]n. N,N′-Diarylformamidinato ions (R-pf–) also work as bidentate ligands for metal ions to give lantern-type dinuclear complexes. We have reported on the polymer complexes [Rh2(4-Me-pf )4(1,4-dib)]n (4-Me-pf– = N,N′-di-p-tolylformamidinate anion; 1,4-dib = 1,4-diisocyanobenzene) and cis-[Rh2(4-Me-pf )2(O2CR)2(L)]n (R = CF3 and CMe3; L = pyz and 4,4′-bipyridine (4,4′-bpy)).4,5 We also reported on the bis-adduct complexes 4-phenylpyridine (4-phpy) cis-[Rh2(4-Me-pf )2(O2CR)4(4-phpy)2] (R = CF3 and CMe3) and cis-[Rh2(4-Me-pf )2(O2CCMe3)2(4-phpy)2]BF4. A pyridine adduct complex, cis-[Rh2(4-Me-pf )2(O2CCF3)4(py)2], has been synthesized, but not reported concerning its crystal structure.6 In this report, we here report on the synthesis and crystal structure of cis-[Rh2(4-Me-pf )2(O2CCMe3)4(py)2] (1). The chemical structure of the title compound 1 is depicted in Fig. 1. The starting material, cis-[Rh2(4-Me-pf )2(O2CCMe3)2], was prepared according to a method described in the literature.7 To a solution of cis-[Rh2(4-Me-pf )2(O2CCMe3)2] (96.0 mg (0.11 mmol) in chloroform (5.0 mL) and methanol (15.0 mL) was added pyridine (1.0 mL), and the mixture was stirred for 3 h at room temperature. To the resultant solution was added water (1.0 mL), and the reaction mixture was evaporatd to ca. 3 mL. The evapotated solution was left at room temperature until red microcrystals were deposited. The deposited microcrytals were collected by suction, washed with a small portion of water, and dried over P2O5 in a vaccum desicater for 3 h. The yield was 76.3 mg (68.2% base on cis-[Rh2(4-Mepf )2(O2CCMe3)2]). Anal. Found: C, 59.12; H, 5.34; N, 8.26. Calcd for C50H58N6O4Rh2: C, 59.29; H, 5.77; N, 8.30%. IR (KBr, cm–1): 2983 w, 2917 w, 2859 w (CH), 1622 s, 1592 s (Ar), 1504 s, 1480 m, 1412 s, 1333 m (COO), 1222 s (Ar). X-ray quality crystals of 1 were obtained by recrystallization from dichlroromethane solution with several drops of pyridine. X-ray crystallographic data (Table 1) were collected for a single crystal of 1 at 150 K on a RIGAKU HyPix6000 CCD system equipped with a Mo rotating-anode X-ray generator (λ = 2021 © The Japan Society for Analytical Chemistry

从分子结构的角度来看，两个过渡金属离子与四个μ-羧酸二齿配体桥接的配合物[M2（O2CR）4]（m=0–2）被称为灯笼型（或桨轮型）双核配合物。聚合物配合物以其有趣的性质吸引了许多化学家。例如，已经发现聚合物络合物[Cu2（O2CPh）4（pyz）]n和[Rh2（O2CPh）4（pyz）]n。N、 N′-二芳基甲酰胺基离子（R-pf–）也作为金属离子的双齿配体，产生灯笼型双核配合物。我们已经报道了聚合物配合物[Rh2（4-Me-pf）4（1,4-二b）]n（4-Me-p–=n，n′-二对甲苯磺酰甲脒阴离子；1,4-二b=1,4-二异氰基苯）和顺式-[Rh2（4-Me-p）2（O2CR）2（L）]n y）2]（R＝CF3和CMe3）和顺式-[Rh2（4-Me-pf）2（O2CCMe3）2（4-hpy）2]BF4。吡啶加合物顺式-[Rh2（4-Me-pf）2（O2CCF3）4（py）2]已被合成，但其晶体结构尚未报道。6在本报告中，我们报道了顺式-[Lh2（4-Me-pf）2-（O2CCMe3）4（py]2]（1）的合成和晶体结构。标题化合物1的化学结构如图所示。1。根据文献中描述的方法制备起始材料顺式-[Rh2（4-Me-pf）2（O2CCMe3）2]。7向顺式-[Lh2（4-Me-pf）2-（O2CCMe3）2]（96.0mg（0.11mmol））在氯仿（5.0mL）和甲醇（15.0mL）中的溶液中加入吡啶（1.0mL），并在室温下搅拌混合物3小时。向所得溶液中加入水（1.0mL），将反应混合物蒸发至约3mL。将蒸发的溶液置于室温下，直到沉积红色微晶。通过抽吸收集沉积的微晶，用少量水洗涤，并在真空干燥器中用P2O5干燥3小时。产率为76.3 mg（68.2%基于顺式-[Rh2（4-Mepf）2（O2CCMe3）2]）。Anal。发现：C，59.12；H、 5.34；N、 8.26。计算C50H58N6O4Rh2:C，59.29；H、 5.77；N、 8.30%。IR（KBr，cm–1）：2983 w、2917 w、2859 w（CH）、1622 s、1592 s（Ar）、1504 s、1480 m、1412 s、1333 m（COO）、1222 s（氩）。用几滴吡啶从二氯甲烷溶液中重结晶得到X射线质量的1晶体。在配备Mo旋转阳极X射线发生器（λ=2021©日本分析化学学会）的RIGAKU HyPix6000 CCD系统上，在150 K下收集1单晶的X射线晶体学数据（表1）

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引用次数: 0

Crystal Structure and Hirshfeld Surface Analysis of 1-(4-Chlorophenyl)-5-{4-[(2-methylphenyl)methoxy]phenyl}-1H-Pyrazole 1-(4-氯苯基)-5-{4-[(2-甲基苯基)甲氧基]苯基}- 1h -吡唑的晶体结构和Hirshfeld表面分析

IF 0.2 Q4 Materials Science

X-ray Structure Analysis Online

Pub Date : 2021-11-10 DOI: 10.2116/xraystruct.37.77

A. Aydın, M. Akkurt, Sümeyye Turanlı, E. Banoglu, N. Ozcelik

The aim of the study is to explore the crystal structure and performe Hirshfeld surface analysis of 1-(4-chlorophenyl)-5-{4-[(2-methylphenyl)methoxy]phenyl}-1 H -pyrazole. In the title compound, C 23 H 19 ClN 2 O, the 4-chlorophenyl, 2-methylphenyl and benzene rings are oriented with dihedral angles of 71.22(10), 31.82(9) and 59.76(9) ° , respectively, with respect to the pyrazole ring. Pairs of molecules are linked by intermolecular C–H···O hydrogen contacts with R 2 2 (8) ring motifs forming sheets lying parallel to (100). Furthermore C–H··· π interactions also contribute to stabilizing the molecular packing. A Hirshfeld surface analysis has been used to confirm and quantify the supramolecular interactions which indicate that the most important contributions for the crystal packing are from H···H (42.5%) and H···C/C···H (35%) and H···Cl/Cl···H (12%) interactions.

本研究的目的是探索1-(4-氯苯基)-5-{4-[(2-甲基苯基)甲氧基]苯基}-1 H -吡唑的晶体结构并进行Hirshfeld表面分析。在标题化合物c23h19cln2o中，4-氯苯基、2-甲基苯基和苯环相对于吡唑环的定向二面角分别为71.22(10)°、31.82(9)°和59.76(9)°。分子对通过分子间C-H···O氢与r22(8)环基序连接，形成平行于(100)的薄片。此外，C-H···π相互作用也有助于稳定分子堆积。Hirshfeld表面分析证实并量化了超分子相互作用，结果表明，H··H(42.5%)、H··C/C··H(35%)和H··Cl/Cl··H(12%)相互作用对晶体堆积的影响最大。

引用次数: 1

Dinuclear Praseodymium(III) Complex with N,N′-Bis(2-hydroxy-3,5-dimethylbenzyl)-N,N′-dimethyl-1,2-ethanediamine 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 0.2 Q4 Materials Science

X-ray Structure Analysis Online

Pub Date : 2021-11-10 DOI: 10.2116/xraystruct.37.73

M. Mikuriya, Chika Kawai, Kana Nagai, Akiko Morita, Asuka Kanemori, D. Yoshioka, M. Tsuboi

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

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

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引用次数: 0

Frontmatter

IF 0.2 Q4 Materials Science

X-ray Structure Analysis Online

Pub Date : 2021-11-08 DOI: 10.1515/9783110610833-fm

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9 Qualitative and quantitative evaluation of powder patterns 粉末图案的定性和定量评价

IF 0.2 Q4 Materials Science

X-ray Structure Analysis Online

Pub Date : 2021-11-08 DOI: 10.1515/9783110610833-009

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8 Powder diffraction methods 8粉末衍射法

IF 0.2 Q4 Materials Science

X-ray Structure Analysis Online

Pub Date : 2021-11-08 DOI: 10.1515/9783110610833-008

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Index 指数

IF 0.2 Q4 Materials Science

X-ray Structure Analysis Online

Pub Date : 2021-11-08 DOI: 10.1515/9783110610833-012

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3 Waves 3波

IF 0.2 Q4 Materials Science

X-ray Structure Analysis Online

Pub Date : 2021-11-08 DOI: 10.1515/9783110610833-003

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7 Single crystal methods 7单晶法

IF 0.2 Q4 Materials Science

X-ray Structure Analysis Online

Pub Date : 2021-11-08 DOI: 10.1515/9783110610833-007

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6 X-ray physics 6 x射线物理学

IF 0.2 Q4 Materials Science

X-ray Structure Analysis Online

Pub Date : 2021-11-08 DOI: 10.1515/9783110610833-006

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