X-ray Structure Analysis Online最新文献

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Crystal Structure of a Lantern-type Diruthenium(II,III) Complex with Axial Thiocyanato and DMF Ligands, [Ru2(O2CCMe3)4(NCS)(DMF)] 具有轴向硫氰酸盐和DMF配体[Ru2（O2CCMe3）4（NCS）（DMF）]的Lantern型Diruthenium（II，III）配合物的晶体结构

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X-ray Structure Analysis Online

Pub Date : 2020-10-10 DOI: 10.2116/xraystruct.36.39

M. Handa, H. Ishida, D. Yoshioka, Fumiaki Kugita, I. Hiromitsu, K. Kasuga, M. Mikuriya

The title compound of a lantern-type ruthenium(II,III) dinuclear complex, [Ru 2 (O 2 CCMe 3 ) 4 (NCS)(DMF)], was isolated and the crystal structure was determined by the single-crystal X-ray diffraction method at 293 K. It crystallizes in the monoclinc space group P 2 1 /n with a = 11.549(6)Å, b = 9.849(5)Å, c = 14.250(8)Å, β = 91.898(7) ° , V = 1619.9(15)Å 3 , D x = 1.513 g/cm 3 , and Z = 2. The R 1 [ I > 2 σ ( I )] and wR 2 (all data) values are 0.0389 and 0.0916, respectively, for all 3860 independent reflections. The axial sites of the dinuclear core are occupied by NCS – and DMF ligands with distances of Ru–N ax (NCS – ) = 2.29(3)Å and Ru–O ax (DMF) = 2.201(19)Å, respectively. The Ru–Ru distance is 2.2713(10)Å, of which the value is in the range of those for the other lantern-type diruthenium(II,III) tetracarboxylate complexes.

分离出灯笼型钌（II，III）双核配合物[Ru2（O2CCMe3）4（NCS）（DMF）]的标题化合物，并在293K下用单晶X射线衍射法测定了晶体结构，并且Z＝2。对于所有3860个独立反射，R1[I>2σ（I）]和wR2（所有数据）值分别为0.0389和0.0916。双核核的轴向位置被NCS–和DMF配体占据，距离分别为Ru–N ax（NCS–）=2.29（3）Å和Ru–O ax（DMF）=2.201（19）Å。Ru–Ru距离为2.2713（10）Å，其值在其他灯笼型四羧酸二钌（II，III）配合物的范围内。

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Crystal Structure Refinement of 1,4,5,8-Tetrabromonaphthalene: A Twisted Chiral Naphthalene Induced by Steric Repulsion 1,4,5,8-四溴萘的晶体结构改进:空间斥力诱导的扭曲手性萘

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X-ray Structure Analysis Online

Pub Date : 2020-09-10 DOI: 10.2116/xraystruct.36.35

A. Hossain, K. Hirabayashi, T. Nishinaga, Toshio Shimizu, K. Sugiura

The molecular structure of sterically crowded 1,4,5,8-tetrabromonaphthalene 1 was refined. The compound crystallized in a monoclinic system and was characterized as follows: P 2 1 / c , a = 9.470(3), b = 15.530(4), c = 7.340(2)Å, β = 92.147(9) ° , Z = 4, V = 1078.7(5)Å 3 . The crystal structure was solved by direct methods and refined by full-matrix least-squares on

改进了空间拥挤的1,4,5,8-四溴-萘1的分子结构。该化合物在单斜晶系中结晶，表征如下:P 21 / c, a = 9.470(3)， b = 15.530(4)， c = 7.340(2)Å， β = 92.147(9)°，Z = 4, V = 1078.7(5)Å 3。用直接法求解晶体结构，并用全矩阵最小二乘法对其进行细化

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Synthesis and Crystal Structure of Tris[2-(2-imidazolinyl)phenolato]ruthenium(III) 三[2-(2-咪唑啉基)苯酚]钌(III)的合成与晶体结构

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X-ray Structure Analysis Online

Pub Date : 2020-09-10 DOI: 10.2116/xraystruct.36.33

R. Mitsuhashi, M. Mikuriya

The crystal data are included in Table 1. X-ray crystallographic data were collected on a Bruker smart APEX CCD diffractometer at 90(2)K. The integrated and scaled data were empirically corrected with SADABS. 5 The initial structure was solved by The crystal structure of the Ru(III) complex with 2-(2-imidazolinyl)phenolate was determined by X-ray crystallography. The title compound was synthesized by a reaction of RuCl 3 · n H 2 O and 2-(2-imidazolinyl)phenolate in ethanol. The compound crystallized in the monoclinic space group P 2 1 / c and Z = 4 with cell parameters a = 10.2053(18)Å, b = 33.277(6)Å, c = 8.8733(15)Å, β = 113.904(3) ° , V = 2754.9(8)Å 3 . The R 1 [ I > 2 σ ( I )] and wR 2 (all data) values are 0.0711 and 0.1487, respectively, for all 6316 independent reflections. The title compound was found to take a meridional configuration. In the crystal, a centrosymmetric dimer structure was formed by intermolecular hydrogen-bonds between the coordinating phenolate-O atom (O2) of a ligand and a noncoordinating N–H bond (N5–H5A) in the symmetry equivalent ligand.

晶体数据如表1所示。x射线晶体学数据在90(2)K的Bruker智能APEX CCD衍射仪上收集。利用SADABS对整合后的数据进行实证校正。用x射线晶体学测定了Ru(III)与2-(2-咪唑啉基)苯酚配合物的晶体结构。该化合物由3·n h2o与2-(2-咪唑啉基)酚酸酯在乙醇中反应合成。晶胞参数为a = 10.2053(18)Å， b = 33.277(6)Å， c = 8.8733(15)Å， β = 113.904(3)°，V = 2754.9(8)Å。所有6316个独立反射的R 1 [I > 2 σ (I)]和wR 2(所有数据)值分别为0.0711和0.1487。标题化合物被发现呈子午形。在晶体中，配位的苯酚- o原子(O2)与对称等效配位的非配位N-H键(N5-H5A)之间的分子间氢键形成中心对称二聚体结构。

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Crystal Structure and Chromic Properties of an Iron(II) Complex Salt of a N-Salicylideneaniline Derivative N-亚水杨基苯胺衍生物的铁（II）配合盐的晶体结构和色度性质

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X-ray Structure Analysis Online

Pub Date : 2020-08-10 DOI: 10.2116/xraystruct.36.31

Haruki Sugiyama, H. Uekusa

The crystal structure of salt, 3 2 was determined by single crystal X-ray structural analysis. It was revealed: monoclinic, C 2/ c , a = 26.951(3), b =

通过单晶X射线结构分析，确定了盐3 2的晶体结构。结果表明：单斜晶系，C2/C，a=26.951（3），b=

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Synthesis and Crystal Structure Determination of a Dimeric Complex of Dimethylammoniumbis(p-tert-butylcatecholato) borate 双（对叔丁基邻苯二酚）硼酸二甲基铵二聚物的合成及晶体结构测定

IF 0.2 Q4 CRYSTALLOGRAPHY

X-ray Structure Analysis Online

Pub Date : 2020-08-10 DOI: 10.2116/xraystruct.36.27

M. Tombul, M. Bıyıkoğlu, Adnan Bulut, K. Güven, Özer Işılar

For decades, there has been growing interest in borates mainly due to the fact that B atoms are capable of forming both the BO3 triangles or the BO4 tetrahedra. Through polymerization these B–O groups can result in constructing one dimensional (1D) chains, 2D layers, and 3D networks.1 The wide range of applications of borates virtually stems from the structureproperty relationship that render possible their huge structural varieties and the functionality of the BO units.2 Such structure diversities make the structure chemistry of borates extraordinary. Thus far, a series of borate materials have been reported for a number of utilizations, including, birefringence, piezoelectric, pyroelectric, and nonlinear optics.3–6 Boron compounds formed by a non-metallic support unit can be displayed in a binary fashion composed of an anionic borate structural unit and a cationic interstitial complex.7 The role of non-metal cations differs from metal cations, since they generally do not coordinate to oxygen in the same way, and may act instead as hydrogen bond donors to the structural unit. Continuation persistently our progressing work on borates,8–11 the process of the self-assembly of organic and inorganic moieties has been performed under DMF solution conditions, and yielded original borate with organic amine, namely dimethyl ammonium bis(p-tertbutylcatecholato) borate. The aforesaid compound (Fig. 1) was prepared by employing a DMF solution (10 mL) of 4-tert-butylcatechole (4.65 mmol), onto which was afterwards added solid boric acid (2.15 mmol) with strong stirring. The reaction mixture was allowed to be stirred at 120°C for 3 h, resulting in the formation of a colorless material. The crude product was crystallized from a water/ acetone mixture. Crystals of the title compound were obtained by slow evaporation. X-ray crystallography was performed at 223.15 K on a RIGAKU AFC73 diffractometer employing graphitemonochromated fine focussed sealed-tube Mo-Kα radiation. Crystal data and details related to the data collection are given in Table 1. The structure was solved by an intrinsic phasing 2020 © The Japan Society for Analytical Chemistry

几十年来，人们对硼酸盐越来越感兴趣，这主要是因为B原子能够形成BO3三角形或BO4四面体。通过聚合，这些B–O基团可以导致构建一维（1D）链、2D层，和3D网络。1硼酸盐的广泛应用实际上源于结构-性质关系，这使得它们的巨大结构变化和BO单元的功能成为可能。2这种结构多样性使硼酸盐的结构化学非同寻常。到目前为止，已经报道了一系列硼酸盐材料用于多种用途，包括双折射、压电、热电、，和非线性光学。3-6由非金属支撑单元形成的硼化合物可以以由阴离子硼酸盐结构单元和阳离子填隙复合物组成的二元方式显示。7非金属阳离子的作用与金属阳离子不同，因为它们通常不会以相同的方式与氧配位，而是可以作为结构单元的氢键供体。继续我们在硼酸盐方面不断进展的工作，8–11有机和无机部分的自组装过程是在DMF溶液条件下进行的，并产生了具有有机胺的原始硼酸盐，即双（对叔丁基儿茶酚酸酯）硼酸二甲基铵。上述化合物（图1）是通过使用4-叔丁基邻苯二酚（4.65mmol）的DMF溶液（10mL）制备的，然后在强烈搅拌下向其上加入固体硼酸（2.15mmol）。将反应混合物在120°C下搅拌3小时，形成无色物质。粗产物从水/丙酮混合物中结晶。通过缓慢蒸发获得标题化合物的晶体。用RIGAKU AFC73衍射仪在223.15K的温度下进行了X射线晶体学研究，该衍射仪采用石墨单色精细聚焦密封管Mo-Kα辐射。表1中给出了晶体数据和与数据收集相关的详细信息。该结构通过内在阶段解决2020©日本分析化学学会

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Crystal Structure of 1,9-Dibromo-5-phenyldipyrrin, Tetrapyrrole Synthesis Derivative and Free Base Ligand of BODIPY Building Blocks 1,9-二溴-5-苯基二吡咯的晶体结构、四吡咯合成衍生物和BODIPY构建块的游离碱配体

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X-ray Structure Analysis Online

Pub Date : 2020-07-10 DOI: 10.2116/xraystruct.36.21

D. O’Shea, R. Sommer, M. Taniguchi, J. Lindsey

引用次数: 0

Crystal Structure of (μ-Phenoxo)bis(μ-pentafluorobenzoate)dicobalt(II, III) Complex with a Dinucleating Ligand 二核配体(μ-苯氧基)双(μ-五氟苯甲酸酯)二钴(II, III)配合物的晶体结构

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X-ray Structure Analysis Online

Pub Date : 2020-07-10 DOI: 10.2116/xraystruct.36.23

Naho Shinde, H. Furutachi, Y. Sakata, Shigehisa Akine, S. Fujinami, Masatatsu Suzuki

The end-off type dinucleating ligands, having a phenolic and alcoholic oxygen as an endogenous bridge, have been used for modeling carboxylate-bridged bimetallic active sites of metalloproteins,1–4 such as hemerythrin (Hr)5 and methane monooxygenase (MMO).6 The bimetallic active centers of metalloproteins have been known to exhibit various oxidation states: dimetal(II, II), dimetal(II, III), dimetal(III, III), dimetal (III, IV), and dimetal(IV, IV).1–6 Synthetic model complexes with various oxidation states are of particular importance for obtaining fundamental insights into structural and spectroscopic properties of the active centers in metalloproteins.1–4 Previously, we reported on the synthesis and characterization of mixed-valence complexes, [FeFe(bpmp)(RCO2)2] and [MnMn(bpmp)(RCO2)2] (R = CH3 and C6H5), having an end-off type dinucleating ligand with pyridyl groups (bpmp).7,8 In this paper, we report on the crystal structure of the dicobalt(II, III) mixed-valence complex [CoCo(bpmp)(C6F5CO2)2](ClO4)2·C2H5OC2H5 (1) (Fig. 1). A mixture of Co(ClO4)2·6H2O (0.183 g, 0.5 mmol) and Hbpmp (0.133 g, 0.25 mmol) in methanol (20 mL) was added a methanol solution (5 mL) containing C6F5CO2H (0.106 g, 0.5 mmol) and triethylamine (69 μL, 0.5 mmol) to give a darkbrown solution under air. Diethyl ether (30 mL) was added to the resulting dark-brown solution to give a black powder, which was recrystallized from acetonitrile/diethyl ether to give single crystals of [CoCo(bpmp)(C6F5CO2)2](ClO4)2·C2H5OC2H5 (1) suitable for X-ray crystallography. Yield: 0.09 g, 27% (Anal. Found: C, 44.49; H, 3.37; N, 7.68%. Calcd for [CoIICoIII(bpmp)(C6F5CO2)2](ClO4)2·1.5CH3CN·1.5H2O, C50H40.5Cl2Co2F10N7.5O14.5: C, 44.25; H, 3.01; N, 7.74%.). It was picked up on a hand-made cold copper plate mounted inside a liquid N2 Dewar vessel and mounted on a glass rod at –80°C. X-ray diffraction measurements were made on a Bruker D8 VENTURE diffractometer (Cu Kα radiation) at 90 K. The structure was solved by a direct method (SHELXT)9 and expanded using a Fourier technique. The structure was refined by a full-matrix least-squares method by using SHELXL 201410 (Yadokari-XG).11 All non-hydrogen atoms were refined with anisotropic displacement parameters. The hydrogen atoms were included using a riding model. The crystal data are summarized in Table 1. The X-ray crystallography of 1 reveals that the asymmetric unit contains a complex cation [CoCo(bpmp)(C6F5CO2)2], two ClO4, and a diethyl ether molecule, where one of ClO4 is disordered over two orientations. An ORTEP drawing of the complex cation, [CoCo(bpmp)(C6F5CO2)2] of 1, is shown in Fig. 2. Selected bond distances (Å) and angles (°) are given in Table 2. The complex cation of 1 has distinct cobalt centers that are triply bridged by phenoxide oxygen of bpmp, and two pentafluorobenzoate groups as found for closely related dimetal(II, III) mixed valence complexes, [FeIIFeIII(bpmp)(C2H5CO2)2] (2)12 and [MnMn(bpmp)(C6H5CO2)2] (3).8 2020 © The Ja

末端型双核配体以酚氧和醇氧为内源性桥接，已被用于模拟金属蛋白的羧酸桥接双金属活性位点1-4，如甲氰菊酯(Hr)5和甲烷单加氧酶(MMO) 6已知金属蛋白的双金属活性中心具有不同的氧化态:二金属(II, II)、二金属(II, III)、二金属(III, III)、二金属(III, III)、二金属(III, IV)和二金属(IV, IV)。1 - 6具有不同氧化态的合成模型配合物对于获得金属蛋白活性中心的结构和光谱性质的基本见解特别重要。1-4之前，我们报道了混合价配合物[FeFe(bpmp)(RCO2)2]和[MnMn(bpmp)(RCO2)2] (R = CH3和C6H5)的合成和表征，它们具有末端型吡啶基二核配体(bpmp)。在本文中，我们报道了二钴(II, III)混合价配合物[CoCo(bpmp)(C6F5CO2)2](ClO4)2·C2H5OC2H5(1)的晶体结构(图1)。将Co(ClO4)2·6H2O (0.183 g, 0.5 mmol)和Hbpmp (0.133 g, 0.25 mmol)在甲醇(20 mL)中的混合物加入含有C6F5CO2H (0.106 g, 0.5 mmol)和三乙胺(69 μL, 0.5 mmol)的甲醇溶液(5 mL)中，得到空气下的深棕色溶液。在得到的深棕色溶液中加入乙醚(30ml)得到黑色粉末，由乙腈/乙醚重结晶得到适合x射线结晶学的[CoCo(bpmp)(C6F5CO2)2](ClO4)2·C2H5OC2H5(1)单晶。收率:0.09 g, 27%。发现:C, 44.49;H, 3.37;N, 7.68%。[CoIICoIII(bpmp)(C6F5CO2)2](ClO4)2·1.5CH3CN·1.5H2O, C50H40.5Cl2Co2F10N7.5O14.5: C, 44.25;H, 3.01;N, 7.74%)。在-80°C的温度下，将其置于液态氮气杜瓦容器内的手工制作的冷铜板上，并安装在玻璃棒上。用Bruker D8 VENTURE衍射仪(Cu Kα辐射)在90k下进行了x射线衍射测量。该结构采用直接法(SHELXT)9求解，并采用傅里叶技术展开。采用SHELXL 201410 (Yadokari-XG)，采用全矩阵最小二乘法对结构进行优化所有非氢原子均采用各向异性位移参数进行细化。氢原子是用骑乘模型计算出来的。晶体数据汇总于表1。1的x射线晶体学显示，不对称单元包含一个配合阳离子[CoCo(bpmp)(C6F5CO2)2]，两个ClO4和一个乙醚分子，其中一个ClO4在两个方向上无序。图2为1的络合阳离子[CoCo(bpmp)(C6F5CO2)2]的ORTEP图。所选键距(Å)和键角(°)见表2。1的配合物阳离子具有明显的钴中心，由bpmp的苯氧氧三桥接，并在密切相关的二金属(II, III)混合价配合物中发现两个五氟苯甲酸基团，[FeIIFeIII(bpmp)(C2H5CO2)2](2)12和[MnMn(bpmp)(C6H5CO2)2](3)。8 2020©日本分析化学学会

{"title":"Crystal Structure of (μ-Phenoxo)bis(μ-pentafluorobenzoate)dicobalt(II, III) Complex with a Dinucleating Ligand","authors":"Naho Shinde, H. Furutachi, Y. Sakata, Shigehisa Akine, S. Fujinami, Masatatsu Suzuki","doi":"10.2116/xraystruct.36.23","DOIUrl":"https://doi.org/10.2116/xraystruct.36.23","url":null,"abstract":"The end-off type dinucleating ligands, having a phenolic and alcoholic oxygen as an endogenous bridge, have been used for modeling carboxylate-bridged bimetallic active sites of metalloproteins,1–4 such as hemerythrin (Hr)5 and methane monooxygenase (MMO).6 The bimetallic active centers of metalloproteins have been known to exhibit various oxidation states: dimetal(II, II), dimetal(II, III), dimetal(III, III), dimetal (III, IV), and dimetal(IV, IV).1–6 Synthetic model complexes with various oxidation states are of particular importance for obtaining fundamental insights into structural and spectroscopic properties of the active centers in metalloproteins.1–4 Previously, we reported on the synthesis and characterization of mixed-valence complexes, [FeFe(bpmp)(RCO2)2] and [MnMn(bpmp)(RCO2)2] (R = CH3 and C6H5), having an end-off type dinucleating ligand with pyridyl groups (bpmp).7,8 In this paper, we report on the crystal structure of the dicobalt(II, III) mixed-valence complex [CoCo(bpmp)(C6F5CO2)2](ClO4)2·C2H5OC2H5 (1) (Fig. 1). A mixture of Co(ClO4)2·6H2O (0.183 g, 0.5 mmol) and Hbpmp (0.133 g, 0.25 mmol) in methanol (20 mL) was added a methanol solution (5 mL) containing C6F5CO2H (0.106 g, 0.5 mmol) and triethylamine (69 μL, 0.5 mmol) to give a darkbrown solution under air. Diethyl ether (30 mL) was added to the resulting dark-brown solution to give a black powder, which was recrystallized from acetonitrile/diethyl ether to give single crystals of [CoCo(bpmp)(C6F5CO2)2](ClO4)2·C2H5OC2H5 (1) suitable for X-ray crystallography. Yield: 0.09 g, 27% (Anal. Found: C, 44.49; H, 3.37; N, 7.68%. Calcd for [CoIICoIII(bpmp)(C6F5CO2)2](ClO4)2·1.5CH3CN·1.5H2O, C50H40.5Cl2Co2F10N7.5O14.5: C, 44.25; H, 3.01; N, 7.74%.). It was picked up on a hand-made cold copper plate mounted inside a liquid N2 Dewar vessel and mounted on a glass rod at –80°C. X-ray diffraction measurements were made on a Bruker D8 VENTURE diffractometer (Cu Kα radiation) at 90 K. The structure was solved by a direct method (SHELXT)9 and expanded using a Fourier technique. The structure was refined by a full-matrix least-squares method by using SHELXL 201410 (Yadokari-XG).11 All non-hydrogen atoms were refined with anisotropic displacement parameters. The hydrogen atoms were included using a riding model. The crystal data are summarized in Table 1. The X-ray crystallography of 1 reveals that the asymmetric unit contains a complex cation [CoCo(bpmp)(C6F5CO2)2], two ClO4, and a diethyl ether molecule, where one of ClO4 is disordered over two orientations. An ORTEP drawing of the complex cation, [CoCo(bpmp)(C6F5CO2)2] of 1, is shown in Fig. 2. Selected bond distances (Å) and angles (°) are given in Table 2. The complex cation of 1 has distinct cobalt centers that are triply bridged by phenoxide oxygen of bpmp, and two pentafluorobenzoate groups as found for closely related dimetal(II, III) mixed valence complexes, [FeIIFeIII(bpmp)(C2H5CO2)2] (2)12 and [MnMn(bpmp)(C6H5CO2)2] (3).8 2020 © The Ja","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":" ","pages":""},"PeriodicalIF":0.2,"publicationDate":"2020-07-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46840550","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 1

Crystal Structure and Magnetic Property of Manganese(II) Hexafluorosilicate Hexahydrate 六水六氟硅酸锰(II)的晶体结构和磁性能

IF 0.2 Q4 CRYSTALLOGRAPHY

X-ray Structure Analysis Online

Pub Date : 2020-06-10 DOI: 10.2116/xraystruct.36.17

M. Mikuriya, Nanami Watanabe, Yoshiki Koyama, D. Yoshioka, J. Ogawa, R. Mitsuhashi, M. Handa

The chemistry of manganese complexes has attracted much attention of many researchers because of the various oxidation numbers and diverse nuclearities, having relevance to model complexes of active centers in manganese enzymes, such as Mn SOD (superoxide dismutase), Mn catalase, and Mn4CaO5 cluster in Photosystem II.1–3 Manganese(II) hexafluorosilicate may be useful as one of the metal source to make manganese complexes. However, the crystal structure of this metal source has not yet been disclosed so far. To our knowledge, unexpectedly only one report concerning manganese(II) triflate has appeared in the literature concerning crystal structures of simple manganese(II) salts.4 In this study, we determined the crystal structure of manganese(II) hexafluorosilicate hexahydrate, which shows an octahedral hexaaquamanganese(II) ion with an octahedral hexafluorosilicate ion, as shown in Fig. 1. This paper describes the crystal structure and temperature dependence of the magnetic susceptibility of [Mn(H2O)6]SiF6 (1). Manganese(II) hexafluorosilicate hexahydrate was recrystallized from distilled water to give pale-pink crystals. IR (cm–1): ν(OH) 3400 (br), δ(H2O) 1624 (s), ν(SiF) 743 (s), 469 (s). A preliminary examination was made, and data were collected 2020 © The Japan Society for Analytical Chemistry

锰配合物的化学性质因其不同的氧化值和不同的核性质而受到许多研究者的关注，与锰酶活性中心的模型配合物有关，如Mn SOD(超氧化物歧化酶)、Mn过氧化氢酶和光系统II中的Mn4CaO5簇。1 - 3六氟硅酸锰可以作为制造锰配合物的金属来源之一。然而，这种金属源的晶体结构至今尚未公开。据我们所知，在有关简单锰盐晶体结构的文献中，意外地只出现了一篇关于三酸锰的报道在本研究中，我们确定了六水六氟硅酸锰(II)的晶体结构，其晶体结构为一个八面体六氟硅酸锰离子与一个八面体六氟硅酸锰离子，如图1所示。本文描述了[Mn(H2O)6]SiF6(1)的晶体结构和磁化率对温度的依赖关系。将六水六氟硅酸锰(II)从蒸馏水中重结晶，得到淡粉色晶体。IR (cm-1): ν(OH) 3400 (br)， δ(H2O) 1624 (s)， ν(SiF) 743 (s)， 469 (s)。进行了初步检验，数据收集于2020©The Japan Society for Analytical Chemistry

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引用次数: 0

Analytical, Spectroscopic and Crystallographic Characterization of 3-[(2E)-3-Phenylprop-2-en-1-ylidene]pentane-2,4-dione 3-[（2E）-3-苯基丙-2-烯-1-基]戊烷-2,4-二酮的分析、光谱和晶体学表征

IF 0.2 Q4 CRYSTALLOGRAPHY

X-ray Structure Analysis Online

Pub Date : 2020-05-10 DOI: 10.2116/xraystruct.36.15

P. S. Resende, M. R. Couri, F. B. Miguel, A. Cuin

Knoevenagel condensation is widely the main method to obtain a carbon–carbon double-bond reacting aldehyde or ketone with organic acid compounds. The condensation between formaldehyde and diethyl malonate, in the presence of diethylamine, appears to be the 1st example of this reaction.1 Doebner modification, for instance, is used to synthesize α-, βunsaturated compounds with advantageous since the reaction can be performed at room temperature, tolerate a variety of functional groups, and avoid unnecessary reactions.2 Another modification of the Knoevenagel reaction is known as the Weiss–Cook reaction, which is an extremely versatile reaction used for the synthesis of a high number of natural products.3,4 The title compound (Fig. 1) was obtained by following the literature.3 Briefly, about 10.3 mL (0.1 mol) of acetylacetone was mixed with 13.3 mL of cinnamaldehyde (0.1 mol), and the mixture was stirred under an ice bath. After 2 h, only one drop of pyrrolidine was added to the reaction solution, and stirring at room temperature (25°C) continued for 10 min. The solution was washed 3 times with a mixture of 10 mL of a HCl aqueous solution (1.0 mol L–1) and 10 mL of CH2Cl2. The organic layer was concentrated, yielding a residue which was purified by column chromatography using n-hexane and ethyl-acetate as an eluent (95:5) to afford the product in solution. Light-yellow crystals were obtained by slow evaporation of the solvent. The yield was 72%, m.p.: 105 – 107o C. Anal. Calcd (%) for C14H14O2: C, 78.5; H, 6.59; Found (%): C, 78.3; H, 6.61. IR bands: νC=O, 1700 cm–1; νC=C + νCCaromatic at 1607, 1541 and 1345 cm–1; νC–O at 1198 cm–1. 1H NMR (500 MHz, DMSO-d6) δ (ppm): 2.34 (s, 3H, CH3) and 2.40 (s, 3H, CH3); 7.035 (dd, 1H, J = 13.5 Hz, –HC=CH–CH=); 7.49 (J = 11.4Hz, 1H, –HC=CH–CH=) and 7.32 (J = 15.4 Hz, 1H, –HC=CH–CH=); 7.61 (d, 2H, J = 7.2, Haromatic); 7.42 (m, 3H, Haromatic). 13C (125 MHz, DMSO-d6) δ (ppm) 203 and 198 (C=O); 145, 142.6 and 124 (–HC=CH–CH=); 142, 135, 128.3, 129.5 and 130.3 (Caromatic and Cnon-hydrogenated). UV-Vis: 332 nm (π-π* transition). The X-ray measurements were performed on an Enraf-Nonius Kappa-CCD diffractometer with graphite-monochromated Mo Kα (λ = 0.71073 Å) radiation. Diffraction data were collected (φ and ω scans with κ-offsets) with COLLECT.5 Integration, scaling and reduction of the diffraction intensities were performed with HKL DENZO-SCALEPACK6 suite of programs. The data were corrected empirically for absorption effects with the multi-scan method.7 The unit cell parameters were obtained by leastsquares refinement based on the angular settings for all collected reflections using HKL SCALEPACK.8 The structure was solved by direct methods with SHELXS-979 and the molecular model refined by the full-matrix least-squares procedure on F2 with SHELXL-97.10 The compound belongs to the monoclinic system. The a, b and c axes are: 12.7006(4)Å, 10.0271(5)Å and 20.1044(10)Å, respectively, and the β angle is 106.525(3)°. Cryst

Knoevenagel缩合是醛或酮与有机酸化合物反应获得碳-碳双键的主要方法。甲醛和丙二酸二乙酯在二乙胺存在下的缩合反应似乎是该反应的第一个例子。1例如，Doebner修饰被用于合成α-、β不饱和化合物，因为该反应可以在室温下进行，可以耐受各种官能团，并避免不必要的反应。2 Knoevenagel反应的另一种修饰被称为Weiss–Cook反应，这是一种用于合成大量天然产物的用途极其广泛的反应。3，4标题化合物（图1）是根据文献获得的。3简言之，将约10.3 mL（0.1 mol）乙酰丙酮与13.3 mL肉桂醛（0.1 mol，并在冰浴下搅拌该混合物。2小时后，仅向反应溶液中加入一滴吡咯烷，并在室温（25°C）下继续搅拌10分钟。用10 mL HCl水溶液（1.0 mol L–1）和10 mL CH2Cl2的混合物洗涤溶液3次。浓缩有机层，得到残留物，用正己烷和乙酸乙酯作为洗脱剂（95∶5）通过柱色谱法纯化，得到溶液中的产物。通过溶剂的缓慢蒸发获得浅黄色晶体。产率为72%，m.p.:105–107o C.Anal。C14H14O2:C的计算值（%），78.5；H、 6.59；发现（%）：C，78.3；H、 6.61。红外波段：μC=O，1700 cm–1；在1607、1541和1345 cm–1时，¦ΑC=C+¦ΑCC芳香族；在1198 cm–1处的ΓC–O。1H NMR（500MHz，DMSO-d6）δ（ppm）：2.34（s，3H，CH3）和2.40（s，1H，CH三）；7.035（dd，1H，J=13.5 Hz，–HC=CH–CH=）；7.49（J=11.4Hz，1H，-HC=CH–CH=）和7.32；7.61（d，2H，J=7.2，Harromatic）；7.42（m，3H，Haromatic）。13C（125MHz，DMSO-d6）δ（ppm）203和198（C=O）；145、142.6和124（–HC=CH–CH=）；142135128.3129.5和130.3（Caromatic和Cnon氢化）。UV-Vis:332nm（π-π*跃迁）。X射线测量是在Enraf Nonius Kappa CCD衍射仪上用石墨单色Mo Kα（λ=0.71073Å）辐射进行的。使用COLLECT收集衍射数据（带κ-偏移的φ和ω扫描）。5使用HKL DENZO-SCALEPACK6程序集进行衍射强度的积分、缩放和降低。使用多扫描方法对数据进行吸收效应的经验校正。7基于使用HKL SCALEPACK收集的所有反射的角度设置，通过最小二乘法精细化获得晶胞参数。8使用SHELXS-979通过直接方法求解结构，使用SHELXL-97.10通过F2上的全矩阵最小二乘程序精细化分子模型该化合物属于单斜晶系。a、b和c轴分别为：12.7006（4）Å、10.0271（5）Å和20.1044（10）Å，β角为106.525（3）°。晶体学数据如表1所示，一些扭转角如表2所示。这种结构中没有溶剂分子，晶胞中有两个独立的不对称单元（Z=8）。两个不对称单元之间的微小差异只能在酮基的扭转角中观察到。C12–C11–C111–C112的角度为-121.3°，而在类似的不对称单元中为-122.2°（C22–C21–C213–C214）。此外，C12–C11–C113–C114的角度为13.6°，而C22-C21-C211-C212的角度为9.4°。仅一个分子的ORTEP 3表示如图所示。2。2020©日本分析化学学会

{"title":"Analytical, Spectroscopic and Crystallographic Characterization of 3-[(2E)-3-Phenylprop-2-en-1-ylidene]pentane-2,4-dione","authors":"P. S. Resende, M. R. Couri, F. B. Miguel, A. Cuin","doi":"10.2116/xraystruct.36.15","DOIUrl":"https://doi.org/10.2116/xraystruct.36.15","url":null,"abstract":"Knoevenagel condensation is widely the main method to obtain a carbon–carbon double-bond reacting aldehyde or ketone with organic acid compounds. The condensation between formaldehyde and diethyl malonate, in the presence of diethylamine, appears to be the 1st example of this reaction.1 Doebner modification, for instance, is used to synthesize α-, βunsaturated compounds with advantageous since the reaction can be performed at room temperature, tolerate a variety of functional groups, and avoid unnecessary reactions.2 Another modification of the Knoevenagel reaction is known as the Weiss–Cook reaction, which is an extremely versatile reaction used for the synthesis of a high number of natural products.3,4 The title compound (Fig. 1) was obtained by following the literature.3 Briefly, about 10.3 mL (0.1 mol) of acetylacetone was mixed with 13.3 mL of cinnamaldehyde (0.1 mol), and the mixture was stirred under an ice bath. After 2 h, only one drop of pyrrolidine was added to the reaction solution, and stirring at room temperature (25°C) continued for 10 min. The solution was washed 3 times with a mixture of 10 mL of a HCl aqueous solution (1.0 mol L–1) and 10 mL of CH2Cl2. The organic layer was concentrated, yielding a residue which was purified by column chromatography using n-hexane and ethyl-acetate as an eluent (95:5) to afford the product in solution. Light-yellow crystals were obtained by slow evaporation of the solvent. The yield was 72%, m.p.: 105 – 107o C. Anal. Calcd (%) for C14H14O2: C, 78.5; H, 6.59; Found (%): C, 78.3; H, 6.61. IR bands: νC=O, 1700 cm–1; νC=C + νCCaromatic at 1607, 1541 and 1345 cm–1; νC–O at 1198 cm–1. 1H NMR (500 MHz, DMSO-d6) δ (ppm): 2.34 (s, 3H, CH3) and 2.40 (s, 3H, CH3); 7.035 (dd, 1H, J = 13.5 Hz, –HC=CH–CH=); 7.49 (J = 11.4Hz, 1H, –HC=CH–CH=) and 7.32 (J = 15.4 Hz, 1H, –HC=CH–CH=); 7.61 (d, 2H, J = 7.2, Haromatic); 7.42 (m, 3H, Haromatic). 13C (125 MHz, DMSO-d6) δ (ppm) 203 and 198 (C=O); 145, 142.6 and 124 (–HC=CH–CH=); 142, 135, 128.3, 129.5 and 130.3 (Caromatic and Cnon-hydrogenated). UV-Vis: 332 nm (π-π* transition). The X-ray measurements were performed on an Enraf-Nonius Kappa-CCD diffractometer with graphite-monochromated Mo Kα (λ = 0.71073 Å) radiation. Diffraction data were collected (φ and ω scans with κ-offsets) with COLLECT.5 Integration, scaling and reduction of the diffraction intensities were performed with HKL DENZO-SCALEPACK6 suite of programs. The data were corrected empirically for absorption effects with the multi-scan method.7 The unit cell parameters were obtained by leastsquares refinement based on the angular settings for all collected reflections using HKL SCALEPACK.8 The structure was solved by direct methods with SHELXS-979 and the molecular model refined by the full-matrix least-squares procedure on F2 with SHELXL-97.10 The compound belongs to the monoclinic system. The a, b and c axes are: 12.7006(4)Å, 10.0271(5)Å and 20.1044(10)Å, respectively, and the β angle is 106.525(3)°. Cryst","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":" ","pages":""},"PeriodicalIF":0.2,"publicationDate":"2020-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.2116/xraystruct.36.15","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46319842","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Crystal Structure of 3-(3-Methyl-1H-indole-1-yl)phthalonitrile 3-(3-甲基- 1h -吲哚-1-基)邻苯二腈的晶体结构

IF 0.2 Q4 CRYSTALLOGRAPHY

X-ray Structure Analysis Online

Pub Date : 2020-04-10 DOI: 10.2116/xraystruct.36.11

Samia Ayari, K. Hirabayashi, Toshio Shimizu, B. Jamoussi, Mehmet F. Sağlam, D. Atilla, K. Sugiura

Indoles are naturally occurring heterocycles and thousands of derivatives have been reported so far.1–3 The chemistry has been developing from a biological perspective, and the research objective has been gradually shifting toward advanced materials chemistry because the electron-donating nature and the rich photo-excited state of indoles are suitable for applications in this field. We previously synthesized an indole-substituted phthalocyanines for photodynamic therapy.4 In this study, we synthesized a new indole derivative, 3-(3-methyl-1H-indole2020 © The Japan Society for Analytical Chemistry

吲哚是一种天然存在的杂环化合物，迄今已报道了数千种衍生物。1-3化学已经从生物学的角度发展起来，由于吲哚的给电子性质和丰富的光激发态适合在这一领域的应用，研究目标逐渐转向先进材料化学。我们先前合成了一种吲哚取代的酞菁用于光动力治疗在这项研究中，我们合成了一种新的吲哚衍生物，3-(3-甲基- 1h -indole2020©The Japan Society for Analytical Chemistry

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