X-ray Structure Analysis Online最新文献

{"title":"Crystal Structure of a Lantern-type Diruthenium(II,III) Complex with Axial Thiocyanato and DMF Ligands, [Ru2(O2CCMe3)4(NCS)(DMF)]","authors":"M. Handa, H. Ishida, D. Yoshioka, Fumiaki Kugita, I. Hiromitsu, K. Kasuga, M. Mikuriya","doi":"10.2116/xraystruct.36.39","DOIUrl":"https://doi.org/10.2116/xraystruct.36.39","url":null,"abstract":"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.","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2020-10-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48226664","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}

{"title":"Crystal Structure Refinement of 1,4,5,8-Tetrabromonaphthalene: A Twisted Chiral Naphthalene Induced by Steric Repulsion","authors":"A. Hossain, K. Hirabayashi, T. Nishinaga, Toshio Shimizu, K. Sugiura","doi":"10.2116/xraystruct.36.35","DOIUrl":"https://doi.org/10.2116/xraystruct.36.35","url":null,"abstract":"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","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2020-09-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43092073","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}

{"title":"Synthesis and Crystal Structure of Tris[2-(2-imidazolinyl)phenolato]ruthenium(III)","authors":"R. Mitsuhashi, M. Mikuriya","doi":"10.2116/xraystruct.36.33","DOIUrl":"https://doi.org/10.2116/xraystruct.36.33","url":null,"abstract":"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.","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2020-09-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43840575","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}

{"title":"Crystal Structure and Chromic Properties of an Iron(II) Complex Salt of a N-Salicylideneaniline Derivative","authors":"Haruki Sugiyama, H. Uekusa","doi":"10.2116/xraystruct.36.31","DOIUrl":"https://doi.org/10.2116/xraystruct.36.31","url":null,"abstract":"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 =","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2020-08-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42909662","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}

{"title":"Synthesis and Crystal Structure Determination of a Dimeric Complex of Dimethylammoniumbis(p-tert-butylcatecholato) borate","authors":"M. Tombul, M. Bıyıkoğlu, Adnan Bulut, K. Güven, Özer Işılar","doi":"10.2116/xraystruct.36.27","DOIUrl":"https://doi.org/10.2116/xraystruct.36.27","url":null,"abstract":"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","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2020-08-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46164660","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}

{"title":"Crystal Structure of 1,9-Dibromo-5-phenyldipyrrin, Tetrapyrrole Synthesis Derivative and Free Base Ligand of BODIPY Building Blocks","authors":"D. O’Shea, R. Sommer, M. Taniguchi, J. Lindsey","doi":"10.2116/xraystruct.36.21","DOIUrl":"https://doi.org/10.2116/xraystruct.36.21","url":null,"abstract":"","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2020-07-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49071262","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}

{"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":null,"pages":null},"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}

{"title":"Crystal Structure and Magnetic Property of Manganese(II) Hexafluorosilicate Hexahydrate","authors":"M. Mikuriya, Nanami Watanabe, Yoshiki Koyama, D. Yoshioka, J. Ogawa, R. Mitsuhashi, M. Handa","doi":"10.2116/xraystruct.36.17","DOIUrl":"https://doi.org/10.2116/xraystruct.36.17","url":null,"abstract":"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","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2020-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47577144","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}

{"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":null,"pages":null},"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}

{"title":"Crystal Structure of 3-(3-Methyl-1H-indole-1-yl)phthalonitrile","authors":"Samia Ayari, K. Hirabayashi, Toshio Shimizu, B. Jamoussi, Mehmet F. Sağlam, D. Atilla, K. Sugiura","doi":"10.2116/xraystruct.36.11","DOIUrl":"https://doi.org/10.2116/xraystruct.36.11","url":null,"abstract":"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","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2020-04-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.2116/xraystruct.36.11","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43125222","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}