Pub Date : 2008-01-01DOI: 10.2116/ANALSCIX.24.X173
M. Tabatabaee, M. Ghassemzadeh, Nazanin Soleimani
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.
该化合物C14H14N8S2·2C2H6OS在单斜空间群P21/c中结晶，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。在固体状态下，N2-H2A…O1和C4-H4A…S1氢键将2分子溶剂(Me2SO)连接到I上。
{"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}
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.
题目化合物[(iso-C4H9)2NH2][SnPh3(O2CCH(CH3)S)]在单斜空间群P21/n中结晶，晶胞参数为: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, Dx = 1.375 Mg m-3。对于5042次反射，该结构的最终R值为0.0222 [I > 2σ(I)]。该配合物的结构为离子结构，由阴离子的三苯基锡部分和阳离子的二异丁基铵部分组成。此外，还观察到阳离子和阴离子之间的氢键网络。
{"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}
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.
许多吡啶羧酸与过渡金属的配合物由于其有趣的结构、氧化还原和水氧化性质而被研究。1,2吡啶-2,6-二羧酸(二吡啶酸)已在好氧和厌氧细菌的孢子中被证实。它是在需氧菌孢子萌发时释放的。吡啶-2,6-二羧酸与二价金属离子形成金属配合物，特别是与锰和钙。此外，胍离子在酶中也起着重要作用;例如，x射线结构证据表明，CP43的保守精氨酸357残基的胍离子与光系统II中水氧化配合物(WOC)的Mn 4 Ca簇的距离只有Å几个。合成了标题配合物，并用单晶x射线衍射对其进行了结构表征。该配合物在空间群p1的三斜体系中求解，单位胞参数为: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。15675个实测反射的最终R值为R 1 = 0.0344。
{"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}
Pub Date : 2008-01-01DOI: 10.2116/ANALSCIX.24.X297
Zhao-Lian Yu, Yuhan Fu, Jian-ge Wang, Sen‐Lan Li
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.
{"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}
Pub Date : 2008-01-01DOI: 10.2116/ANALSCIX.24.X117
M. Hematyar, M. K. Rofouei
{"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}
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.
报道了以抗菌磺胺嘧啶代谢物n4 -乙酰磺胺嘧啶(或N-{4-[(2-嘧啶氨基-κN-氨基)磺酰基]苯基乙酰胺)为配体的配合物二氯苯(N-{4-[(2-嘧啶氨基)磺酰基]苯基乙酰胺)铜(II)的x射线结构。配合物在P21/n空间群中结晶，a = 12.7531(3) a, b = 8.0777(2) a, c = 14.8548(3) a， β = 112.237(1)°，Z = 2，要求其中心对称。两个氯离子和两个n4 -乙酰磺胺嘧啶分子配位在金属中心，每个有机部分通过一个嘧啶基氮原子与Cu(II)结合。金属配位球包括来自对称相关络合物分子的羰基氧原子，位于方形平面单元CuN2Cl2的顶端，在Cu(II)周围形成四方扭曲的八面体几何。虽然n4 -乙酰磺胺嘧啶本身没有显示出抗菌活性，但在体外实验中，标题复合物显示出对几种细菌的适度生长抑制。
{"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}
Pub Date : 2008-01-01DOI: 10.2116/ANALSCIX.24.X225
H. Wadepohl
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
{"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}
Pub Date : 2008-01-01DOI: 10.2116/ANALSCIX.24.X231
X. Qiu, Weisheng Liu, Hailiang Zhu
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.
合成了一种新型镉(II)与2-羟基- n′-(丙烷-2-酰基)苯并肼配位聚合物，并用x射线分析对其结构进行了表征。该配合物在C2/c单斜晶系中结晶，空间群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。中心的Cd(II)原子由四个O原子和两个N原子六配位，形成近似八面体环境。在标题配合物的晶体填料中，分子通过分子内的O- h…N和分子间的O- h…O氢键连接，形成平行于ab平面的二维层。
{"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}
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.
Pub Date : 2008-01-01DOI: 10.2116/ANALSCIX.24.X121
Hiroaki Yamanaka, G. Hihara, H. Miyamae
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.
标题配合物为三斜状，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,Z = 2;R是0.0242。该结构显示了沿[111]延伸的一维聚合物，在每个桥接的乙二胺(en)的C-C键的中间有两个晶体独立的反转中心。Pb原子由2个I原子和4个N原子配位:2个I原子处于顺式位置，2个N原子处于与之相反的一个螯合面，4个原子位于包含Pb原子的一个平面内;桥接配体的另外两个N原子位于两个轴向位置。由于I-Pb-I角为144.57(1)°宽，Pb环境的几何形状可以描述为一个扭曲的五边形双金字塔，提供了一个立体化学活性的铅原子的孤对电子可能占据一个配位位。
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