Analytical Sciences: X-ray Structure Analysis Online最新文献

{"title":"Structural Characterization of a New Schiff-Base Ligand, 1,4-Bis-(5-methyl-4-methylenamino-2,4-dihydro-[1,2,4]triazol-3-thion)-benzene [C14H14N8S2·2C2H6OS]","authors":"M. Tabatabaee, M. Ghassemzadeh, Nazanin Soleimani","doi":"10.2116/ANALSCIX.24.X173","DOIUrl":"https://doi.org/10.2116/ANALSCIX.24.X173","url":null,"abstract":"The title compound, C14H14N8S2·2C2H6OS, crystallizes in the monoclinic space group P21/c with a = 12.866(5), b = 8.126(3), c = 11.833(4)A, β = 101.239(9)°, Z = 2, Dx = 1.409 g cm-3. In the solid states, N2-H2A…O1 and C4-H4A…S1 hydrogen bonds link 2 molecules of solvent (Me2SO) to I.","PeriodicalId":7796,"journal":{"name":"Analytical Sciences: X-ray Structure Analysis Online","volume":"359 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2008-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77409067","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 Di-iso-butylammonium Thiolactatotriphenylstannate","authors":"Olaniran Atchade, Xueqing Song, R. Pike, G. Eng","doi":"10.2116/ANALSCIX.24.X77","DOIUrl":"https://doi.org/10.2116/ANALSCIX.24.X77","url":null,"abstract":"The title compounds, [(iso-C4H9)2NH2][SnPh3(O2CCH(CH3)S)], crystallized in a monoclinic space group P21/n with the following cell parameters: a = 9.8537(2)A, b = 16.7775(3)A, c = 17.5845(3)A, β = 103.7740(10)°, V = 2823.48(9)A3, Z = 4 and Dx = 1.375 Mg m-3. The structure was refined to a final R value of 0.0222 for 5042 reflections [I > 2σ(I)]. The structure of the complex is ionic consisting of an anionic triphenyltin moiety and a cationic di-iso-butylammonium portion. In addition, a hydrogen bonding network between the cations and anions was observed.","PeriodicalId":7796,"journal":{"name":"Analytical Sciences: X-ray Structure Analysis Online","volume":"11 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2008-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"79751925","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":"Guanidinium Bis(pyridine-2,6-dicarboxylato-N,O,O)manganese(II)","authors":"D. Boghaei, M. Najafpour","doi":"10.2116/ANALSCIX.24.X23","DOIUrl":"https://doi.org/10.2116/ANALSCIX.24.X23","url":null,"abstract":"Numerous complexes of pyridinecarboxylic acids with transition metals have been investigated because of their interesting structural, redox and water oxidation properties. 1,2 Pyridine-2,6-dicarboxylic (dipicolinic) acid has been demonstrated in spores of aerobic and anaerobic bacteria. It is released during the germination of spores of aerobes. Pyridine-2,6-dicarboxylic forms a metal complex with divalent metal ions, especially with manganese and calcium. 3 Also the guanidinium cation has an important role in enzymes; for example, X-ray structural evidence places the guanidinium cation of the conserved arginine 357 residue of CP43 within a few Å to the Mn 4 Ca cluster of the water-oxidizing complex (WOC) in photosystem II. 4 The title complex was synthesized and structurally characterized by single-crystal X-ray diffraction. This complex was solved in the triclinic system, space group P 1 , with the following unit-cell parameters: a = 8.5657(4)Å, b = 10.9848(5)Å, c = 13.1681(6)Å, α = 112.617(1)˚, β = 99.646(1)˚, δ = 90.849(1)˚, Z = 2, V = 1123.28(9)Å 3 . The final R value was R 1 = 0.0344 for 15675 measured reflections.","PeriodicalId":7796,"journal":{"name":"Analytical Sciences: X-ray Structure Analysis Online","volume":"108 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2008-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87584199","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, Characterization, and Crystal Structure of trans-3-Cyclohexylamino-4-methoxy-γ-butyrolactone","authors":"Zhao-Lian Yu, Yuhan Fu, Jian-ge Wang, Sen‐Lan Li","doi":"10.2116/ANALSCIX.24.X297","DOIUrl":"https://doi.org/10.2116/ANALSCIX.24.X297","url":null,"abstract":"The title compound was synthesized and characterized by elemental analysis, spectroscopic data such as IR, 1H NMR, 13C NMR, and X-ray diffraction analysis. The compound crystallizes in the orthorhombic crystal class in the space group Pbca. The final residual factor, R1, is 0.0510. The molecule has trans-stereochemistry and two chiral centers, and thus represents a racemic mixture.","PeriodicalId":7796,"journal":{"name":"Analytical Sciences: X-ray Structure Analysis Online","volume":"140 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2008-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"86585016","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 the Complex of 1,3-Bis(2-methoxybenzene)-triazene with Mercury(II) Bromide","authors":"M. Hematyar, M. K. Rofouei","doi":"10.2116/ANALSCIX.24.X117","DOIUrl":"https://doi.org/10.2116/ANALSCIX.24.X117","url":null,"abstract":"","PeriodicalId":7796,"journal":{"name":"Analytical Sciences: X-ray Structure Analysis Online","volume":"18 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2008-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"75321895","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 Dichlorobis(N-{4-[(2-pyrimidinyl-κN-amino)-sulfonyl]phenyl}acetamide)copper(II)","authors":"J. Obaleye, M. Caira, A. Tella","doi":"10.2116/ANALSCIX.24.X63","DOIUrl":"https://doi.org/10.2116/ANALSCIX.24.X63","url":null,"abstract":"The X-ray structure of the complex dichlorobis(N-{4-[(2-pyrimidinyl-κN-amino)sulfonyl]phenyl}acetamide)copper(II), containing a metabolite N4-acetylsulfadiazine (or N-{4-[(2-pyrimidinylamino)sulfonyl]phenyl}acetamide) of the antibacterial sulfadiazine as ligand, is reported. The complex crystallizes in the space group P21/n with a = 12.7531(3)A, b = 8.0777(2)A, c = 14.8548(3)A, β = 112.237(1)°, and Z = 2, requiring it to be centrosymmetric. Two chloride ions and two N4-acetylsulfadiazine molecules are coordinated to the metal center, each organic moiety being bonded to Cu(II) through a pyrimidinyl nitrogen atom. The metal coordination sphere includes carbonyl oxygen atoms from symmetry-related complex molecules at the apical sites of the square-planar unit, CuN2Cl2, giving a tetragonally-distorted octahedral geometry around Cu(II). Although N4-acetylsulfadiazine, itself, has not demonstrated antibacterial activity, the title complex showed moderate growth inhibition of several bacteria in in vitro assays.","PeriodicalId":7796,"journal":{"name":"Analytical Sciences: X-ray Structure Analysis Online","volume":"52 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2008-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"90153812","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":"Basic Metal Complexes: Crystal Structures of Cyclopentadienylcobalt(I)-bis(trimethylphosphine) and Cyclopentadienylcobalt(I)-(trimethylphosphine)(ethylene)","authors":"H. Wadepohl","doi":"10.2116/ANALSCIX.24.X225","DOIUrl":"https://doi.org/10.2116/ANALSCIX.24.X225","url":null,"abstract":"The Lewis and Bronstedt basicity of transition metal in organometallic complexes is a concept widely used to rationalize stoichiometric and catalytic reactivity. [(C5H5)Co(PMe3)2] 1 is one of the prototypal representatives of basic metal complexes, and its chemistry has been extensively studied. The metal and/ or carbon-centered nucleophilic reactivity in the series [(C5H5)M(PMe3)2–n(C2H4)n] (M = Co, Rh, Ir; n = 1, 2) is of particular importance. For example, as a consequence of the variation of the metal basicity, the protonation of [(C5H5)Rh(PMe3)(C2H4)] 2a occurs at the metal to give the hydrido complex cation [(C5H5)Rh(H)(PMe3)(C2H4)], whereas in [(C5H5)Co(PMe3)(C2H4)] 2b a metal carbon bond is protonated to form an agostic ethyl complex, viz. [(C5H5)Co(PMe3)(h-C2H5)] 3.1 Here we report on the crystal and molecular structures of 1 and 2b, the latter being the precursor to 3, one of the best mechanistically characterized late-metal polymerization catalysts. Apart from catalytic applications, the series [(C5H5)Co(PMe3)2–n(C2H4)n] (n = 0 – 2) constitutes important reference molecules for MO-theoretical calculations, due to their relative simplicity and symmetrical structures. The title complexes were prepared in quantitative yield by the slow addition of two or one, respectively, molar equivalents of PMe3 to a hexane solution of [(C5H5)Co(C2H4)2] at –20 ̊C, followed by warming up to ambient temperature and removal of the solvent in vacuo. Single crystals suitable for intensity data collection were obtained by cooling pentane solutions to –20 ̊C. The structures were solved by the heavy atom method combined with structure expansion by direct methods applied to difference structure factors2 and refined by full-matrix leastsquares methods based on F2.3 All non-hydrogen atoms were given anisotropic displacement parameters. All hydrogen atoms were located in difference Fourier syntheses. During refinement, the hydrogens of the methyl groups were treated as variable metric rigid groups, with ideal bond angles. All other hydrogen atoms were freely refined. Both 1 and 2b adopt the two-legged piano-stool geometry (Fig. 2). The coordination geometry around the cobalt atom is remarkably similar in both complexes. The plane of the C5H5 X-ray Structure Analysis Online","PeriodicalId":7796,"journal":{"name":"Analytical Sciences: X-ray Structure Analysis Online","volume":"85 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2008-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"90289639","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 Novel Coordination Polymer of 2-Hydroxy-N′-(propan-2-ylidene)benzohydrazide with Cadmium(II)","authors":"X. Qiu, Weisheng Liu, Hailiang Zhu","doi":"10.2116/ANALSCIX.24.X231","DOIUrl":"https://doi.org/10.2116/ANALSCIX.24.X231","url":null,"abstract":"A novel coordination polymer of cadmium(II) with 2-hydroxy-N′-(propan-2-ylidene)benzohydrazide was synthesized and the structure was characterized by X-ray analysis. The title complex was crystallized in a monoclinic system, space group C2/c with a = 12.4693(8)A, b = 8.9986(8)A, c = 21.6986(18)A, β = 99.480(2)°, V = 2401.5(3)A3, Z = 4. The central Cd(II) atoms are six-coordinated by four O atoms and two N atoms, giving approximately octahedral environments. In the crystal packing of the title complex, molecules are connected by intramolecular O-H…N and intermolecular O-H…O hydrogen bonds, forming a two-dimensional layer parallel to the ab plane.","PeriodicalId":7796,"journal":{"name":"Analytical Sciences: X-ray Structure Analysis Online","volume":"29 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2008-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78818600","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 Aqua[N,N′-bis(3-methoxysalicylidene)propane-1,2-diaminato]methanolmanganese(III) Perchlorate","authors":"H. Kara","doi":"10.2116/ANALSCIX.24.X79","DOIUrl":"https://doi.org/10.2116/ANALSCIX.24.X79","url":null,"abstract":"The title compound, a hydrogen-bonded pseudo-dimer, Mn(C19H18N2O4)(CH4O)(H2O)]ClO4, (I), has been structurally characterized. Complex (I) affords an elongated octahedral coordination environment, with axial Mn-O(CH3OH) = 2.296(5) and Mn-O(water) = 2.208(3)A.","PeriodicalId":7796,"journal":{"name":"Analytical Sciences: X-ray Structure Analysis Online","volume":"28 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2008-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76687738","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 PbI2(ethylenediamine)2, catena-μ-Ethylenediamine-ethylenediaminediiodolead(II) at -150°C","authors":"Hiroaki Yamanaka, G. Hihara, H. Miyamae","doi":"10.2116/ANALSCIX.24.X121","DOIUrl":"https://doi.org/10.2116/ANALSCIX.24.X121","url":null,"abstract":"The title complex is triclinic, P1, a = 7.585(3), b = 7.688(4), c = 12.737(6)A, α = 83.22(2), β = 73.731(19), γ = 63.38(2)°, V = 637.4(5)°3, and Z = 2 at -150°C; R is 0.0242. The structure shows a one-dimensional polymer extending along [111] with two crystallographically independent inversion centers lying at the middle of the C-C bond of each bridging ethylenediamine (en). The Pb atom is coordinated by two I atoms and four N atoms: the two I atoms occupy a cis-position, the two N atoms of a chelating en lie opposed to them, and the four atoms lie in a plane containing the Pb atom; the other two N atoms of the bridging en ligands lie at both axial positions. Since the I-Pb-I angle is 144.57(1)° wide, the Pb environment geometry might be described as being a distorted pentagonal bipyramid, providing a stereochemically active lone pair of electrons of the Pb atom may occupy one coordination site.","PeriodicalId":7796,"journal":{"name":"Analytical Sciences: X-ray Structure Analysis Online","volume":"34 5","pages":""},"PeriodicalIF":0.0,"publicationDate":"2008-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"91468929","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}