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}
A N,N′-o-phenylenebis(salicylideneimine) (Salophen) macrocycle with a solvent was prepared and its crystal structure was analyzed. In the structure, an acetonitrile is stabilized in the cavity of the salophen macrocycle by hydrogen bonds. In the packing, intermolecular C-H…O, C-H…N, O-H…N hydrogen bondings, C-H…π interactions, and π…π stacking interactions were observed.
{"title":"Crystal Structure of N,N′-o-Phenylenebis(salicylideneimine) (Salophen) with a Solvent","authors":"Il Yoon, T. Shimizu, M. Asakawa","doi":"10.2116/ANALSCIX.24.X11","DOIUrl":"https://doi.org/10.2116/ANALSCIX.24.X11","url":null,"abstract":"A N,N′-o-phenylenebis(salicylideneimine) (Salophen) macrocycle with a solvent was prepared and its crystal structure was analyzed. In the structure, an acetonitrile is stabilized in the cavity of the salophen macrocycle by hydrogen bonds. In the packing, intermolecular C-H…O, C-H…N, O-H…N hydrogen bondings, C-H…π interactions, and π…π stacking interactions were observed.","PeriodicalId":7796,"journal":{"name":"Analytical Sciences: X-ray Structure Analysis Online","volume":"312 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2008-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76275861","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.X211
O. Şahin, O. Büyükgüngör, D. A. Köse, B. Zümreoğlu-Karan
The title compound, tetraquaorotatonickel(II) monohydrate, C5H12N2O9Ni, crystallizes in the monoclinic space group P1 with the following unit-cell parameters: a = 7.2282(4)A, b = 8.2959(4)A, c = 10.0611(5)A, α = 80.115(4)°, β = 70.479(4)°, γ = 65.779(4)° and Z = 2. The NiII ion is coordinated by a deprotonated N atom and the carboxylate O atom of the orotate ligand and four aqua ligands in a distorted octahedral geometry. Intermolecular N-H…O and O-H…O hydrogen bonds produce R22(8), R22(12), R22(16), R32(8), R43(8) and R44(12) rings, which lead to a one-dimensional polymeric chains. An extensive three-dimensional network of N-H…O and O-H…O hydrogen bonds, π-π and N-H…π interactions are responsible for crystal stabilization.
标题化合物C5H12N2O9Ni在单斜空间群P1中结晶，晶胞参数为:a = 7.2282(4) a, b = 8.2959(4) a, c = 10.0611(5) a， α = 80.115(4)°，β = 70.479(4)°，γ = 65.779(4)°，Z = 2。NiII离子是由一个去质子化的N原子和一个羧酸O原子配位的旋合配体和四个水配体在一个扭曲的八面体几何。分子间N-H…O和O- h…O氢键形成R22(8)、R22(12)、R22(16)、R32(8)、R43(8)和R44(12)环，形成一维聚合物链。N-H…O和O- h…O氢键、π-π和N-H…π相互作用的广泛三维网络是晶体稳定的原因。
{"title":"Synthesis and Crystal Structure of Tetraquaorotatonickel(II) Monohydrate","authors":"O. Şahin, O. Büyükgüngör, D. A. Köse, B. Zümreoğlu-Karan","doi":"10.2116/ANALSCIX.24.X211","DOIUrl":"https://doi.org/10.2116/ANALSCIX.24.X211","url":null,"abstract":"The title compound, tetraquaorotatonickel(II) monohydrate, C5H12N2O9Ni, crystallizes in the monoclinic space group P1 with the following unit-cell parameters: a = 7.2282(4)A, b = 8.2959(4)A, c = 10.0611(5)A, α = 80.115(4)°, β = 70.479(4)°, γ = 65.779(4)° and Z = 2. The NiII ion is coordinated by a deprotonated N atom and the carboxylate O atom of the orotate ligand and four aqua ligands in a distorted octahedral geometry. Intermolecular N-H…O and O-H…O hydrogen bonds produce R22(8), R22(12), R22(16), R32(8), R43(8) and R44(12) rings, which lead to a one-dimensional polymeric chains. An extensive three-dimensional network of N-H…O and O-H…O hydrogen bonds, π-π and N-H…π interactions are responsible for crystal stabilization.","PeriodicalId":7796,"journal":{"name":"Analytical Sciences: X-ray Structure Analysis Online","volume":"76 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2008-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74459590","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.X229
M. K. Rofouei, Tahereh Hashempur
The crystal structure of [Cu2I2L2], L = 1,3-bis(2-methoxyphenyl)triazene was determined by X-ray diffraction. The complex crystallizes in the monoclinic system, space group P21/c with a = 9.0976(8), b = 12.4229(12), c = 14.4204(11)A, β = 106.582(3)°, V = 1562.0(2)A3, Z = 2. The structure was solved by the full-matrix least-squares on F2 and had a refined R value of 0.0245 for 3486 reflections (I > 2σ(I)). The Cu2I2 moiety is coordinated by two molecules of the ligand via azide nitrogen and oxygen from a methoxy group in a trigonal pyramidal geometry.
用x射线衍射法测定了[Cu2I2L2]， L = 1,3-双(2-甲氧基苯基)三氮杂烯的晶体结构。该配合物在单斜晶系中结晶，空间群为P21/c, a = 9.0976(8)， b = 12.4229(12)， c = 14.4204(11) a， β = 106.582(3)°，V = 1562.0(2)A3, Z = 2。利用全矩阵最小二乘在F2上求解，得到3486次反射(I > 2σ(I))的精确R值为0.0245。Cu2I2部分由两个配体分子通过叠氮氮和甲氧基氧在三角锥体几何结构中配位。
{"title":"Synthesis and Crystal Structure of Bis[1,3-bis(2-methoxyphenyl)triazene]-copper(I) Iodide","authors":"M. K. Rofouei, Tahereh Hashempur","doi":"10.2116/ANALSCIX.24.X229","DOIUrl":"https://doi.org/10.2116/ANALSCIX.24.X229","url":null,"abstract":"The crystal structure of [Cu2I2L2], L = 1,3-bis(2-methoxyphenyl)triazene was determined by X-ray diffraction. The complex crystallizes in the monoclinic system, space group P21/c with a = 9.0976(8), b = 12.4229(12), c = 14.4204(11)A, β = 106.582(3)°, V = 1562.0(2)A3, Z = 2. The structure was solved by the full-matrix least-squares on F2 and had a refined R value of 0.0245 for 3486 reflections (I > 2σ(I)). The Cu2I2 moiety is coordinated by two molecules of the ligand via azide nitrogen and oxygen from a methoxy group in a trigonal pyramidal geometry.","PeriodicalId":7796,"journal":{"name":"Analytical Sciences: X-ray Structure Analysis Online","volume":"38 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2008-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77699451","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.X259
P. Kanwal, V. Gupta, P. Sharma, N. Satti, K. A. Suri, G. Qazi
The title compound, 3-ethyl-2-methyl-1H-[1,10]phenanthrolin-4-one, C15H14N2O, crystallizes in the monoclinic space group P21/n with unit-cell parameters: a = 8.1941(8), b = 12.3569(12), c = 11.9673(12)A, β = 105.214(2)°, Z = 4. The crystal structure was solved by direct methods using single-crystal X-ray diffraction data collected at 100 K and refined by full-matrix least-squares procedures to a final R-value of 0.0577 for 1818 observed reflections. There is a strong intramolecular hydrogen bond between the two phenanthroline N atoms. The characteristic pattern observed in the packing diagram is the appearance of chains of molecules packed together to form well-defined layers.
标题化合物3-乙基-2-甲基- 1h -[1,10]phenanthrolin-4-one, C15H14N2O在单斜空间群P21/n中结晶，单位胞参数为:a = 8.1941(8)， b = 12.3569(12)， c = 11.9673(12) a， β = 105.214(2)°，Z = 4。利用在100 K下收集的单晶x射线衍射数据，通过全矩阵最小二乘程序对1818个观测反射的最终r值进行了优化，得到了0.0577的晶体结构。在两个邻菲罗啉N原子之间存在很强的分子内氢键。在包装图中观察到的特征图案是分子链的外观，这些分子链聚集在一起形成定义良好的层。
{"title":"Crystal Structure of 3-Ethyl-2-methyl-1H-[1,10]phenanthrolin-4-one","authors":"P. Kanwal, V. Gupta, P. Sharma, N. Satti, K. A. Suri, G. Qazi","doi":"10.2116/ANALSCIX.24.X259","DOIUrl":"https://doi.org/10.2116/ANALSCIX.24.X259","url":null,"abstract":"The title compound, 3-ethyl-2-methyl-1H-[1,10]phenanthrolin-4-one, C15H14N2O, crystallizes in the monoclinic space group P21/n with unit-cell parameters: a = 8.1941(8), b = 12.3569(12), c = 11.9673(12)A, β = 105.214(2)°, Z = 4. The crystal structure was solved by direct methods using single-crystal X-ray diffraction data collected at 100 K and refined by full-matrix least-squares procedures to a final R-value of 0.0577 for 1818 observed reflections. There is a strong intramolecular hydrogen bond between the two phenanthroline N atoms. The characteristic pattern observed in the packing diagram is the appearance of chains of molecules packed together to form well-defined layers.","PeriodicalId":7796,"journal":{"name":"Analytical Sciences: X-ray Structure Analysis Online","volume":"72 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2008-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"72885720","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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