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

{"title":"Crystal Structure of (E)-4-Bromo-2-[(4-hydroxyphenyl)iminomethyl]-phenylen-1-olate","authors":"Işın Kılıç, A. Agar, Ferda Erşahin, Ş. Işık","doi":"10.2116/ANALSCIX.24.X151","DOIUrl":"https://doi.org/10.2116/ANALSCIX.24.X151","url":null,"abstract":"The title compound, (E)-4-bromo-2-[(4-hydroxyphenyl)iminomethyl]phenylen-1-olate, C13H10BrNO2, is in a zwitterionic form with a strong intramolecular N+-H…O- hydrogen bond. The title compound crystallizes in the monoclinic space group P21/c with the following unit-cell parameters: a = 12.6746(11)A, b = 12.8195(15)A, c = 7.1576(7)A, β = 94.993(7)° and V = 1158.6(2)A3. The crystal structure of this compound was solved by direct methods and refined to a final R = +0.0362 for 2285 reflections with I > 2σ(I).","PeriodicalId":7796,"journal":{"name":"Analytical Sciences: X-ray Structure Analysis Online","volume":"36 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2008-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82816070","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 N-(3-Methyl-5-phenyl-3,5-dihydro-4H- 1,2,4-triazol-4-yl)benzamide","authors":"O. Şahin, O. Büyükgüngör, S. Şaşmaz, Nurhan Gümrükçüoğlu, C. Kantar","doi":"10.2116/ANALSCIX.24.X219","DOIUrl":"https://doi.org/10.2116/ANALSCIX.24.X219","url":null,"abstract":"","PeriodicalId":7796,"journal":{"name":"Analytical Sciences: X-ray Structure Analysis Online","volume":"33 2","pages":""},"PeriodicalIF":0.0,"publicationDate":"2008-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"91512683","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-Bis(p-methylphenyl)-2-flouro-1,3,2-diazaphospholidine-2-oxide","authors":"K. Gholivand, F. Mojahed","doi":"10.2116/ANALSCIX.24.X17","DOIUrl":"https://doi.org/10.2116/ANALSCIX.24.X17","url":null,"abstract":"Diazaphospholidines have the ability to bind with metals and to inhibit cholinesterase (ChE), an enzyme that has a vital role in nerve impulse transition. The crystal structure of 1,3-bis(p-methylphenyl)-2-flouro-1,3,2-diazaphospholidine-2-oxide (1) was determind using single-crystal X-ray diffraction. The five-membered ring containing phosphorus, nitrogen and carbon atoms is slightly puckered. The coordination environment around the phosphorus atom in this compound is approximately tetrahedral.","PeriodicalId":7796,"journal":{"name":"Analytical Sciences: X-ray Structure Analysis Online","volume":"8 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2008-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"83704777","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 Bis[O,O′-di(p-tolyl)thiophosphoryl]disulfide, [(p-MeC6H4O)2PS2]2","authors":"Chitra Gurnani, Seema Maheshwari, R. Ratnani, J. Drake","doi":"10.2116/ANALSCIX.24.X197","DOIUrl":"https://doi.org/10.2116/ANALSCIX.24.X197","url":null,"abstract":"The structural chemistry of metal complexes with bis(thiophosphoryl) and bis(thiophosphinyl) disulfides has been extensively reviewed.1 The reactive –S–S– functional moiety determines the chemical properties of these thermally stable disulfides, and their photolytic properties are important in photochemically activated reactions. Bis(thiophosphoryl)disulfides act as potentially significant stabilizers for polymer composition, as vulcanization accelerators, and as antioxidants. These disulfides also act as antiwear additives in ash-less and extreme pressure engine lubricants, and are involved in the mechanism of the antioxidant action of metal dithiophosphate lubricant oil additives. Some bis(thiophosphoryl)disulfides show fungicidal activity. Due to the significance of the disulfide bond in natural products, the physiochemical properties of –S–S– linkages have been extensively studied over the last few decades. Molecular structures of several organothiophosphoryl disulfides have been determined, including [{(i-Pr)O}2PS2]2, [(PhO)2PS2]2, and [OCMe2CMe2OPS2]2 which provide for comparisons with the structure of bis[O,O¢-di(p-tolyl)thiophosphoryl]disulfide, [(p-MeC6H4O)2PS2]2. The title compound was prepared by a literature method.5 An orange block crystal of [(p-MeC6H4O)2PS2]2 was mounted in a capillary within a glove box, thus maintaining a dry, O2-free environment for each crystal. No statistically significant change over the duration of the data collection was observed. Experimental details and results are given in Table 1. All of the non-hydrogen atoms were treated anisotropically. Hydrogen atoms were included at idealized positions with isotropic thermal parameters. The distances and bond angles are given in Table 2. The ORTEP diagram in Fig. 2 shows the previously described2 essentially planar zigzag array of the S–P–S–S–P–S linkages X-ray Structure Analysis Online","PeriodicalId":7796,"journal":{"name":"Analytical Sciences: X-ray Structure Analysis Online","volume":"16 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2008-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"90429084","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 the Salen Cobalt(III) Azido Complex Na[Co(salen)(N3)2]","authors":"M. Weil, A. D. Khalaji","doi":"10.2116/ANALSCIX.24.X19","DOIUrl":"https://doi.org/10.2116/ANALSCIX.24.X19","url":null,"abstract":"The cobalt(III) azido complex, Na[Co(salen)(N3)2], contains a Co(III) cation in a distorted octahedral coordination. The equatorial plane of the octahedron is defined by two N and two O atoms from the tetradentate salen ligand, and the axial ligands belong to two terminal N atoms from two different azide anions. Via interactions between the Na+ cations and the N and O atoms of the ligands, the [Co(salen)(N3)2]- anions are connected into a polymeric structure, forming corrugated ribbons parallel to [100].","PeriodicalId":7796,"journal":{"name":"Analytical Sciences: X-ray Structure Analysis Online","volume":"15 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2008-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"75013242","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 Molecular Structure of trans-Dichlorodi((4-fluorophenyl)-methanamine)palladium(II)","authors":"Caleb D. Martin, F. Appoh, C. Vogels, A. Decken, S. Westcott","doi":"10.2116/ANALSCIX.24.X223","DOIUrl":"https://doi.org/10.2116/ANALSCIX.24.X223","url":null,"abstract":"The use of palladium complexes to catalyze the coupling of organoboron compounds with aryl or vinyl halides has become one of the most widely used tools in organic synthesis. The scope and utility of the Suzuki–Miyaura reaction has been the subject of several excellent reviews.1 The use of boronic acids in this cross coupling process is especially advantageous as these compounds are relatively nontoxic and thermally, airand moisture-stable.2 Numerous advances have been made to this reaction since its discovery. For instance, the use of aryl chlorides as substrates and the ability to conduct the reaction at low temperature and at low catalyst loading have greatly increased the versatility of the Suzuki–Miyaura cross coupling reaction. Catalyst development has also played a significant role in improving this reaction as traditional palladium complexes used to catalyze this transformation contain airsensitive phosphine ligands. In recent years, a considerable amount of research has also focused on designing new catalysts that can be used to carry out this reaction in alternative solvents.3 We report here on the synthesis and molecular structure of a palladium complex containing fluorinated benzylamines for its potential use in the Suzuki–Miyaura cross-coupling reaction. A suspension of PdCl2 (150 mg, 0.85 mmol) in MeOH (15 mL) was treated with NaCl (100 mg, 1.71 mmol) at RT and stirred for 1 h. A MeOH (2 mL) solution of 4fluorobenzylamine (212 mg, 1.69 mmol) was added dropwise to the reaction mixture and stirred for 1 h resulting in the formation of a yellow precipitate. The solid was collected by suction filtration and washed with MeOH (5 mL) and hexane (10 mL) to afford the title compound. Crystals were obtained by recrystallization from DMSO at RT. Yield: 290 mg (80%); m.p. = 495 – 497 K (decomposition). Spectroscopic NMR data (in DMSO-d6): 1H d: 7.50 (br m, 4H, Ar), 7.14 (br m, 4H, Ar), 3.97 (br s, 4H, CH2), 3.58 (br s, 4H, NH2); 13C{1H} d: 162.0 (d, JC-F = 240 Hz, CF), 135.1, 131.3 (d, JC-F = 8 Hz, Ar), 115.4 (d, JC-F = 21 Hz, Ar), 47.4 (CH2); 19F{1H} d: –115.3. FT-IR (Nujol): 3257, X-ray Structure Analysis Online","PeriodicalId":7796,"journal":{"name":"Analytical Sciences: X-ray Structure Analysis Online","volume":"220 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2008-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76286469","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 Tl2[(S0.6Se0.4)O4]Te(OH)6","authors":"M. Abdelhedi, M. Dammak, A. Kolsi, A. Cousson","doi":"10.2116/ANALSCIX.24.X93","DOIUrl":"https://doi.org/10.2116/ANALSCIX.24.X93","url":null,"abstract":"The crystal structure of the thallium sulfate selenate tellurate Tl2[(S0.6Se0.4)O4]Te(OH)6 was determined with single-crystal X-ray diffraction data. The title compound crystallizes in the monoclinic system with the P21/c space group. The unit-cell dimensions at 298 K are a = 12.3580(10)A, b = 7.2310(10)A, c = 11.9860(10)A, β = 111.090(10)°, V = 999.33(19)A3, Dx = 5.029 g/cm3, and Z = 4. The R value is 0.047 for 1799 reflections. The anions are disposed in a number of sheets of pure (S,Se)O4 tetrahedra, alterning with sheets of pure Te(OH)6 octahedra. All of those planes are intercalated in a bidimensional arrangement by Tl+ cations.","PeriodicalId":7796,"journal":{"name":"Analytical Sciences: X-ray Structure Analysis Online","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2008-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"72893393","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 New Mixed-Chelate Complex of [Cu(diamine)(acac)]ClO4","authors":"H. Golchoubian","doi":"10.2116/ANALSCIX.24.X169","DOIUrl":"https://doi.org/10.2116/ANALSCIX.24.X169","url":null,"abstract":"The title compound was synthesized and characterized by single-crystal X-ray diffraction. This complex was solved in the tetragonal system, space group P41212, with the following unit-cell parameters: a = 13.6010(3)A, c = 13.1885(6)A, Z = 4, V = 2439.70(13)A3. The final R value was R1 = 0.0259 for 27567 measured reflections.","PeriodicalId":7796,"journal":{"name":"Analytical Sciences: X-ray Structure Analysis Online","volume":"40 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2008-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"73845342","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 (4SR,5RS)-5-(4-Cyanophenyl)-4-trimethylsilyl-3-methylisoxazoline","authors":"T. Akimoto, H. Hara, T. Nakano,, N. Hirayama","doi":"10.2116/ANALSCIX.24.X165","DOIUrl":"https://doi.org/10.2116/ANALSCIX.24.X165","url":null,"abstract":"The crystal of the title compound, C14H18N2OSi, belongs to space group P1 with cell dimensions of a = 6.2639(3), b = 10.818(1), c = 12.085(1)A, α = 69.976(4), β = 76.959(5), and γ = 81.566(3)°. The final R value is 0.0486. The isoxazoline ring takes an envelope conformation. The dihedral angle between the isoxazoline and phenyl rings is 103.9(1)°. The Si-C bond bridging the isoxazoline ring and trimethylsilyl group is significantly longer than the other three Si-C bonds.","PeriodicalId":7796,"journal":{"name":"Analytical Sciences: X-ray Structure Analysis Online","volume":"19 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2008-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"73923862","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 1-2 Diphenyl ethylenediammonium Chloride","authors":"S. Zouari, F. Zouari, N. Chniba-Boudjada, P. Bordet","doi":"10.2116/ANALSCIX.24.X215","DOIUrl":"https://doi.org/10.2116/ANALSCIX.24.X215","url":null,"abstract":"The salt 1-2 diphenyl ethylenediammonium chloride crystallizes at room temperature in the monoclinic system with polar space group P21; the unit-cell dimensions are: a = 8.720(2), b = 6.243(2), c = 13.972(5)A, β = 106.67(3)° with Z = 2. The structure consists of [C14H18N2]2+ cations and isolated chlorine anions. These entities are linked together through N-H…Cl hydrogen bonds, forming a three-dimentional network.","PeriodicalId":7796,"journal":{"name":"Analytical Sciences: X-ray Structure Analysis Online","volume":"22 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2008-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74041020","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}