X-ray Structure Analysis Online最新文献

{"title":"10 Structure solution methods","authors":"","doi":"10.1515/9783110610833-010","DOIUrl":"https://doi.org/10.1515/9783110610833-010","url":null,"abstract":"","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2021-11-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80642892","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":"2 Geometry and coordinate systems","authors":"","doi":"10.1515/9783110610833-002","DOIUrl":"https://doi.org/10.1515/9783110610833-002","url":null,"abstract":"","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2021-11-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81840410","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":"4 Symmetry","authors":"","doi":"10.1515/9783110610833-004","DOIUrl":"https://doi.org/10.1515/9783110610833-004","url":null,"abstract":"","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2021-11-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87163461","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":"Disorder of the Water Molecules and Sulfate Anion in the Crystal Structure of Fe-substituted Synthetic Chalcanthite Crystals (Cu1–xFex)SO4·5H2O (x = 0.1 and 0.20)","authors":"V. Sabirov, M. Jumaev, Djumanali Irkabaev, J. Ashurov","doi":"10.2116/xraystruct.37.59","DOIUrl":"https://doi.org/10.2116/xraystruct.37.59","url":null,"abstract":"The isomorphism and isodimorphism of the d metal sulfates are of particular importance for the crystal chemistry of minerals, materials science, solid solutions physics and processing of the ores. The thermodynamic theory of solid-solution aqueoussolution interactions and available the effects of ionic substitutions on the thermodynamic properties of binary sulfate solid solutions were discussed before in detail.1 Chalcanthite is paramagnetic compound, and doping another paramagnetic atom, Fe2+, to it allow to modify it’s magnetic susceptibility.2 Crystals of chalcanthite have an optical band pass with a transmission band of 0.280 – 0.570 nm with a maximal transmission of 75%; they can be successfully used as an optical bandpass in higher resolution spectral devices.3 Some Fe-containing chalcanthite crystals were studied by the single crystal X-ray diffraction method and the distribution of the Cu and Fe atoms over the crystallographic sites are determined by using of the results of analytical chemistry or according to the degree of the distortion of the coordination polyhedrons around sites.4,5 Site occupations of the Cu and Fe atoms are not possible because of the similar scattering-factors of these elements. To except the problems of non-distinguishability of Cu and Fe during an X-ray diffraction study, we have synthesized the solid solutions of chalcanthite with a priory known chemical compositions, (Cu0.90Fe0.10)SO4·5H2O (I) and (Cu0.80Fe0.20) SO4·5H2O (II), and have studied (Fig. 1). The influence of substituting Cu for Fe ion on the structural disorders of the subunits in the crystal of chalcanthite was not performed. For this reason, this work is aimed at an X-ray diffraction study of the crystal structure of these compounds. Single crystals of (I) and (II) were synthesized by stirring 0.01 M sulfuric acid solution of CuSO4·5H2O and FeSO4·7H2O in molar of ratios of 9:1 and 8:2 at a temperature of ∼45°C, respectively. The X-ray diffraction data were collected on a Xcalibur, Ruby diffractometer using graphite-monochromated Cu-Kα radiation. Crystal and experimental data details are given in the Table 1. The values of the |E2 – 1| statistical parameters show that both crystals are centrosymmetric, and because it’s crystal structures were solved in the space group P1 and refined by a full-matrix least-squares method.6 The hydrogen atoms were found from difference maps, though not refined. Disorder manifests itself as a splitting of the O atoms sites and trigonal planar configuration of the O atoms of aqua ligands. The perceptible residual electron density remain around the M2 site on the distance 0.52 Å. Both crystal structures are composed of the square-planar [Cu(H2O)4] located at the M1(0,0,0) site and [(Cu,Fe)(H2O)4] at the M2(0,1/2,–1/2) site. The SO4 tetrahedra acts as a μ2-bridging ligand between these cations, which lead to a chain structure (Figs. 2 and 3). The water of crystallization takes place in the hydrogen bonds. Selected Cu–O ","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2021-10-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45421064","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-(3-Ferrocenyl-2-methylpyrrolo[1,2-a]quinoxalin-4-yl)piperazin-4-ium Chloride","authors":"J. Guillon, N. Pinaud, Solène Savrimoutou, M. Marchivie, S. Moreau, Sandra Albenque-Rubio, P. Sonnet","doi":"10.2116/xraystruct.37.65","DOIUrl":"https://doi.org/10.2116/xraystruct.37.65","url":null,"abstract":"The X-ray crystal structure of the antimalarial 1-(3-ferrocenyl-2-methylpyrrolo[1,2- a ]quinoxalin-4-yl)piperazin-4-ium chloride has been established. It crystallizes in the tetragonal space group P -42 1 c with cell parameters a = 24.6705(19)Å, b = 24.6705(19)Å, c = 7.4533(6)Å, α = 90 ° , β = 90 ° , γ = 90 ° V = 4536.3(8)Å 3 and Z = 8. The crystal structure was refined to final values of R 1 = 0.0354 and wR 2 = 0.0837. An X-ray crystal structure analysis revealed that each molecule features intermolecular N–H···Cl hydrogen bonds interactions between the ammonium group and the chloride anion to form tetramers.","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2021-10-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42489179","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":"Dinuclear Zinc(II) Complex with a Cyclam-based Ligand with Four Schiff-base Pendant Arms","authors":"Shusaku Wada, D. Yoshioka, M. Tsuboi, M. Mikuriya","doi":"10.2116/xraystruct.37.61","DOIUrl":"https://doi.org/10.2116/xraystruct.37.61","url":null,"abstract":"Dinuclear zinc(II) complex with 1,4,8,11-tetrakis(salicylideneaminoethyl)-1,4,8,11-tetraazacyclotetradecane (H 4 tsaec), [Zn 2 (tsaec)]·2CHCl 3 , was synthesized. The crystal structure was determined by the single-crystal X-ray diffraction method at 293 K. The complex crystallizes in the monoclinic space group P 2 1 / c with a = 9.496(3), b = 11.568(3), c = 23.338(7)Å, β = 96.270(4) ° , V = 2548.3(12)Å 3 , D calcd = 1.505 g/cm 3 , Z = 2. The R 1 [ I > 2 σ ( I )] and wR 2 (all data) values are 0.0407 and 0.1034, respectively, for all 6119 independent reflections. The two zinc(II) atoms are bound to the tsaec ligand outside the central teraazacyclotetradecane ring with an intramolecular Zn···Zn distance of 9.426(2)Å, where each zinc(II) atom is coordinated by two Schiff-base pendant arms with two phenolato-oxygen and two imino-nitrogen atoms to form a distorted tetrahedral geometry.","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2021-10-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48361562","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 Tetrakis(μ-2,3,6-trimethoxybenzoato-κO:κO′)bis[(methanol)copper(II)]: Largely Rotated Benzoate Ring to the Carboxylato Bridge","authors":"M. Mikuriya, C. Yamakawa, Kensuke Tanabe, Raigo Nukita, D. Yoshioka, R. Mitsuhashi, M. Handa, M. Tsuboi","doi":"10.2116/xraystruct.37.49","DOIUrl":"https://doi.org/10.2116/xraystruct.37.49","url":null,"abstract":"X-ray for the crystal Bruker X-ray diffractometer (SMART APEX) α radiation. Crystal data The structure intrinsic with SHELXT-2014, methods Hydrogen atoms at their calculated the A dinuclear copper(II) carboxylate with 2,3,6-trimethoxybenzoic acid (H236-tmbz), tetrakis( μ -2,3,6-trimethoxybenzoato-κ O : κ O ′ )bis[(methanol)copper(II)], [Cu 2 (236-tmbz) 4 (CH 3 OH) 2 ], was prepared, and the crystal structure was determined by a single-crystal X-ray structure analysis at 90 K. It crystallizes in the triclinic space group P 1 with a = 7.4282(11)Å, b = 12.2389(18)Å, c = 13.3158(19)Å, α = 115.128(2) ° , β = 95.396(3) ° , γ = 91.086(2) ° , V = 1088.8(3)Å 3 , D x = 1.580 g/cm 3 , and Z = 1. The R 1 [ I > 2 σ ( I )] and wR 2 (all data) values are 0.0513 and 0.1207, respectively, for all 4894 independent reflections. The two copper atoms are bridged by four 2,3,6-trimethoxybenzoato ligands in a syn - syn mode to form a dinuclear cluster (Cu···Cu 2.6071(8)Å) with the apical methanol molecules. The benzoate phenyl rings are largely rotated to the bridging OCO moieties with a rotation angle ( f rot ) of 74.9(2) and 44.6(3) ° .","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2021-09-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47916747","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 2-(Pyridin-2-ylamino)pyridinium Trifluoromethanesulfonate","authors":"Mari Toyama, Noriharu Nagao","doi":"10.2116/xraystruct.37.53","DOIUrl":"https://doi.org/10.2116/xraystruct.37.53","url":null,"abstract":"The compound 2-(pyridin-2-ylamino)pyridine, known as di-2pyridylamine (Hdpa), has been widely used as a bidentate ligand with various transition metal ions. The first crystal structure of a complex with the Hdpa ligand, which was a Cu(II)-Hdpa complex, [Cu(Hdpa)2](ClO4)2, was reported by J. E. Jonson, T. A. Beineke, and R. A. Jacobson in 1971.1 They then also determined the crystal structure of uncoordinated Hdpa.2 Up to now many chemists have revealed many crystal structures of transition metal complexes with Hdpa,1,3,4 and a few crystal polymorphisms of uncoordinated Hdpa.5,6 Moreover, about eighty crystal structures of compounds containing a protonated Hdpa cation, H2dpa, 2-(pyridin-2-ylamino)pyridinium, are reported, such as (H2dpa)2[CoCl4] by F. A. Cotton and co-workers in 1998,3 and (H2dpa)(NCS)·CH3CN by B. Schmitt and co-workers in 2011,7 as well as we know. We determined the crystal structure of a 2-(pyridin-2-ylamino)pyridinium trifluoromethanesulfonate, H2dpa(OTf ) (OTf– = CF3SO3, Fig. 1). Single crystals of H2dpa(OTf ) were obtained from a thermal reaction of an aqueous solution of cis-[Co(CO3)(Hdpa)2](OTf ) in the presence of an excess amount of (HOTf )aq. Although we expected the reaction to afford cis-[Co(Hdpa)2(OH2)2](OTf )3, an unexpected decomposition reaction occurred to afford free Hdpa, of which the reaction with excess HOTf afforded H2dpa(OTf ). Colorless crystals of H2dpa(OTf ) suitable for X-ray crystallography were obtained by allowing the reaction mixture to evaporate under reduce pressure. The crystals of H2dpa(OTf ) were also obtained from the mixture of an ethanol solution of Hdpa with HOTf at 278 K without stirring for several days. X-ray crystallography was performed at 173 K on a Rigaku Mercury70 diffractometer using graphite-monochromated MoKα radiation. The structure was solved by direct methods (SIR2014), and refined by full-matrix least-squares techniques with anisotropic thermal parameters for all non-hydrogen atoms. The C–H hydrogen atoms and the N–H hydrogen atom of an amino group were located in the difference Fourier map, and their coordinate and isotropic thermal parameters were refined. The H7a and H7b hydrogen atoms associated with N2 and N3, 2021 © The Japan Society for Analytical Chemistry","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2021-09-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48348870","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 2-(1-Benzoylazetidin-3-yl)thio-1,3-thiazoline","authors":"K. Sugiura, Yoshimi Ichimaru, Koichi Kato, Masanori Imai, H. Kurosaki, Kazuhiko Hayashi","doi":"10.2116/xraystruct.37.57","DOIUrl":"https://doi.org/10.2116/xraystruct.37.57","url":null,"abstract":"Tebipenem pivoxil is an oral 1β-methylcarbapenem antibiotic with a broad spectrum and potent antibacterial activity against various bacteria, except for Pseudomonas aeruginosa, which has the [1-(1,3-thiazolin-2-yl)azetidin-3-yl]thio moiety as the pendant at the C-2 position.1 The pendant moiety of Tebipenem pivoxil was introduced using 1-(1,3-thiazolin-2-yl)azetidine-3thiol, and was also introduced into the antibiotic T405 under development.2 However, no chrystallographic studies of 1-(1,3-thiazolin-2-yl)azetidine-3-thiol and its synthetic precursors have been reported, except for Tebipenem pivoxil, which has the thio group.3 In this paper, we describe the X-ray crystal structure of 2-(1-benzoylazetidin-3-yl)thio-1,3-thiazoline (Fig. 1), which is a synthetic precursor of 1-(1,3-thiazolin-2-yl)azetidine-3-thiol. The title compound was synthesized by reacting 1-azabicyclo[1.1.0] butane and 3-benzoyl-1,3-thiazolidine-2-thione in the presence of a Lewis acid, such as Mg(OTf )2. Then, the crude compound was purified using column chromatography, followed by recrystallization from diethyl ether. Crystal data were collected on a Rigaku XtaLAB Synergy-i diffractometer (Rigaku Co., Tokyo, Japan) using the graphitemonochromated Cu-Kα radiation at 93.15 K, which are provided in Table 1. The initial structure was solved using an intrinsic phasing method with SHELXT-2018.5 All non-hydrogen atoms were refined using the full-matrix least-squares method on F2 by utilizing SHELXL-2018.6 All calculations were performed using Olex2 crystallographic software.7 Crystallographic data have been deposited to the Cambridge Crystallographic Data Center (CCDC-2075942). The absolute structure of this crystal was determined by X-ray diffraction method (Flack’s parameter: 0.006(11)). The ORTEP drawing is shown in Fig. 2, and selected bond lengths and angles are listed in Table 2. The S1– C4 bond length is 1.778(3)Å as a reasonable single-bond. The N2–C4 bond length of 1.256(4)Å is shorter than the N2–C6 bond length [1.472(4)Å] and is considered to form a double-bond. The thiazoline ring, defined by S1–C4–N2–C6–C5, forms a distorted five-membered ring from the ring strain (C4–S1–C5, 2021 © The Japan Society for Analytical Chemistry","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2021-09-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49547737","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 a Mixed-valent Hexanuclear Manganese Complex Made-up from Two Oxido-centered Triangular MnIIMnIII2 Cores","authors":"M. Mikuriya, Sayuri Ono, Yoshiki Koyama, R. Mitsuhashi, M. Tsuboi","doi":"10.2116/xraystruct.37.41","DOIUrl":"https://doi.org/10.2116/xraystruct.37.41","url":null,"abstract":"A hexanuclear Mn II2 Mn III4 complex with 2-(5-nitro-2-hydroxyphenyl)-1,3-bis(2-(5-nitro-2-hydroxybenzylideneamino)-ethyl)imidazolidine (H 3 L NO2 ) and its hydrolyzed ligand, 1,10-bis(5-nitrosalicylideneamino)-4,7-azadecane (H 2 L NO2 ′ ), was isolated. The crystal structure was determined by the single-crystal X-ray diffraction method at 90 K. The complex crystallized as [{Mn 3 ( μ 3 -O)( μ -CH 3 COO) 2 ( μ -L NO2 )} 2 (L NO2 ′ )]·2.5THF·CH 3 OH in the monoclinic space group C 2/ c with a = 21.253(3), b = 16.630(2), c = 29.508(4)Å, β = 93.147(2) ° , V = 10413(2)Å 3 , D calcd = 1.551 g/cm 3 , Z = 4. The R 1 [ I > 2 σ ( I )] and wR 2 (all data) values are 0.0836 and 0.2500, respectively, for all 11924 independent reflections. The complex is a hexanuclear manganese molecule which has a crystallographic inversion center at the midpoint of the ethylenediamine backbone of L NO2 ′ 2– ligand. In the asymmetric unit, three manganese atoms (Mn1, Mn2, and Mn3) are arranged in a μ 3 -oxido-centered triangle, and the Mn1 and Mn2 atoms are further bridged by a phenolato-oxygen atom of L NO23– , and both of the Mn1 and Mn3 atoms and the Mn2 and Mn3 atoms are further bridged by an acetato ligand in a syn - syn mode. The charge balance and a bond valence sum calculation supported the mixed-valent Mn II2 Mn III4 state with the Mn II state for the Mn1 atom and the Mn III state for the Mn2 and Mn3 atoms, respectively.","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2021-08-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47440868","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}