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Synthesis and crystal structure of bis-cis-(+)-2-(4-methoxyphenyl)-4-oxo-2,3,4,5-tetrahydro-1,5-benzothiazepine-3-yl-oxalate 双顺式-(+)-2-(4-甲氧基苯基)-4-氧-2,3,4,5-四氢-1,5-苯并噻唑-3-草酸酯的合成与晶体结构
Pub Date : 2008-01-01 DOI: 10.2116/ANALSCIX.24.X113
P. Kumaradhas, A. D. Stephen, K. Nirmala, N. Kalyanam
The crystal structure of bis-cis-(+)-2-(4-methoxyphenyl)-4-oxo-2,3,4,5-tetrahydro-1,5-benzothiazepine-3-yl-oxalate was determined as being orthorhombic, space group P212121, with lattice parameters a = 9.654(6)A, b = 13.256(1)A, c = 25.841(3)A, Z = 4, V = 3307.1(6)A3 and Dcalc = 1.355 Mg m-3. The compound crystallizes with one disordered water molecule. The carbonyl groups in the oxalate bridge are trans oriented, as indicated by the torsion angle [O(20)=C(19)-C(19′)=O(20′)] -151.5(3)°. Both 1,5-benzothiazepine rings in the molecule adopt a similar type of twist boat conformation.
确定了双顺式-(+)-2-(4-甲氧基苯基)-4-氧-2,3,4,5-四氢-1,5-苯并噻吩-3-草酸酯的晶体结构为正交结构,空间群为P212121,晶格参数为a = 9.654(6) a, b = 13.256(1) a, c = 25.841(3) a, Z = 4, V = 3307.1(6)A3, Dcalc = 1.355 Mg m-3。这种化合物与一个无序的水分子结晶。草酸桥中的羰基是反取向的,由扭转角[O(20)=C(19)-C(19’)=O(20’)]-151.5(3)°表示。分子中的两个1,5-苯并噻吩环都采用类似的扭船构象。
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引用次数: 1
Crystal Structure of 3-(4-(Dimethylamino)benzylidene)pentane-2,4-dione 3-(4-(二甲氨基)苄基)戊烷-2,4-二酮的晶体结构
Pub Date : 2008-01-01 DOI: 10.2116/ANALSCIX.24.X285
M. Habibi, K. Barati, Hossein Etedali Habibabadi, R. Harrington, W. Clegg
The title compound (I), C14H17NO2, was synthesized and the structure was investigated by X-ray crystallography. The compound was obtained by an Aldol condensation, and crystallized in the orthorhombic space group P212121 with cell parameters a = 6.6758(9), b = 11.6866(15), c = 16.348(2)A, V = 1275.4(3)A3 and Z = 4. The crystal structure is stabilized by inter and intramolecular C-H…O hydrogen bonds.
合成了标题化合物C14H17NO2,并用x射线晶体学对其结构进行了研究。该化合物通过Aldol缩合得到,晶胞参数为a = 6.6758(9), b = 11.6866(15), c = 16.348(2) a, V = 1275.4(3)A3, Z = 4,在正交空间群P212121中结晶。分子间和分子内的C-H - O氢键稳定了晶体结构。
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引用次数: 0
A New Pentaheterocyclic System: Cyclobuta[4,5]pyrrolo[1,2-a][1,10]phenanthroline 一个新的五杂环系:环丁[4,5]吡咯[1,2- A][1,10]菲罗啉
Pub Date : 2008-01-01 DOI: 10.2116/ANALSCIX.24.X27
F. Dumitrascu, M. Caira, L. Barbu, B. Miu, B. Draghici
A derivative of the new heterocyclic system cyclobuta[4,5]pyrrolo[1,2-a][1,10]phenanthroline was obtained by condensation between 2,9-dimethyl-1,10-phenanthroline and dimethyl acetylenedicarboxylate, and its structure was assigned by X-ray analysis. The strained molecular conformation observed for this pentaheterocyclic framework can be attributed to a series of repulsive intramolecular interactions that render both the phenanthroline system and the four-membered ring non-planar.
由2,9-二甲基-1,10-菲罗啉与二甲基乙酰二羧酸盐缩合得到了新的杂环体系环丁基[4,5]吡咯罗[1,2- A][1,10]菲罗啉的衍生物,并通过x射线分析确定了其结构。在这个五杂环框架中观察到的张力分子构象可以归因于一系列排斥的分子内相互作用,这些相互作用使得菲罗啉体系和四元环都是非平面的。
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引用次数: 0
Crystal Structure of N,N'-Bis(3,4,5-trimethoxybenzylidene)-ethylenediaminediiodozinc(II) N,N'-双(3,4,5-三甲氧基苄基)-乙二胺二碘化(II)的晶体结构
Pub Date : 2008-01-01 DOI: 10.2116/ANALSCIX.24.X91
A. D. Khalaji, F. Jian, Hailian Xiao, Somayyeh Mojdekanlou
The title complex, [Zn((3,4,5-MeO-ba)2en)I2], has been synthesized and structurally characterized by single crystal X-ray diffraction. The geometry around the zinc atom is a distorted tetrahedron. This structure consists of intermolecular hydrogen bonds of the type C-H…I and C-H…O.
合成了标题配合物[Zn((3,4,5- meo -ba)2en)I2],并用单晶x射线衍射对其进行了结构表征。锌原子周围的几何形状是一个扭曲的四面体。这种结构由C-H…I和C-H…O型分子间氢键组成。
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引用次数: 6
Crystal Structure of [Pb(μ3-Nic)2]n, HNic = 4-nicotinic acid [Pb(μ3-Nic)2]n, HNic = 4-烟酸的晶体结构
Pub Date : 2008-01-01 DOI: 10.2116/ANALSCIX.24.X125
G. Shahverdizadeh, S. Masoudian, A. Soudi, A. Morsali, P. Retailleau
The crystal structure of [Pb(μ3-Nic)2]n, (HNic = 4-nicotinic acid) is orthorhombic, space group Pbcn with a = 16.595(1), b = 10.028(1), c = 14.635(1)A and Z = 2. The crystal structure was solved by direct methods and refined by full-matrix least squares to final values of R1 = 0.0277 and wR2 = 0.0609 with 3553 reflections I >2σ(I). The lead(II) ion in [Pb(μ3-Nic)2]n is eight-coordinate and the direction of the Pb-N and Pb-O bonds shows that the coordination around the lead(II) ion is holodirected.
[Pb(μ3-Nic)2]n, (HNic = 4-烟酸)的晶体结构为正交结构,空间群Pbcn为a = 16.595(1), b = 10.028(1), c = 14.635(1) a, Z = 2。采用直接法求解晶体结构,并用全矩阵最小二乘法将其细化至最终值R1 = 0.0277和wR2 = 0.0609,反射频率为3553,反射频率为>2σ(I)。[Pb(μ3-Nic)2]n中的铅(II)离子为八坐标,Pb- n和Pb- o键的方向表明铅(II)离子周围的配位是全向的。
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引用次数: 3
Crystal Structure of Naptalam Naptalam的晶体结构
Pub Date : 2008-01-01 DOI: 10.2116/ANALSCIX.24.X45
Keiichirou Nemoto, Taira Kimino, Y. Mano, I. Fujii
The crystal structure of Naptalam, which is a pre-emergent herbicide, has been determined. A tilted amide group connects two planar moieties, which make a stepwise conformation with a dihedral angle of 3.76(7)° from naphtyl and phenyl groups. The molecules correlated with 21-axis make a dimmer. The crystal structure is stabilized by an infinite-intermolecular hydrogen-bond and π-π interaction.
测定了一种萌发前除草剂萘talam的晶体结构。一个倾斜的酰胺基团连接两个平面基团,由萘基和苯基组成一个二面角为3.76(7)°的阶梯构象。与21轴相关的分子形成一个调光体。晶体结构由分子间的氢键和π-π相互作用稳定。
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引用次数: 0
Crystal Structure of a Hydrate Complex of Phthalic Acid [phth = o-phthalate] 邻苯二甲酸[phth =邻苯二甲酸酯]水合物配合物的晶体结构
Pub Date : 2008-01-01 DOI: 10.2116/ANALSCIX.24.X95
Jimin Xie, Wu Wen, Ya-wen Xuan
In an attempt to grow crystals of sodium acid phthalate, the title compound, (phth)2(H2O)3 (1) [phth=phthalate], was obtained which crystallizes in the monoclinic system; space group C2/c, β = 113.65(3)°, V = 1812.9(6)A3, Z = 4, Dc = 1.415 g/cm3, the final R = 0.0781 and wR = 0.2367. O-H groups of phthalate rings form strong hydrogen bonds with lattice water which stabilizes the crystal structure.
在生长邻苯二甲酸钠晶体的尝试中,获得了标题化合物(phth)2(H2O)3 (1) [phth=邻苯二甲酸盐],它在单斜体系中结晶;空间群C2/c, β = 113.65(3)°,V = 1812.9(6)A3, Z = 4, Dc = 1.415 g/cm3,最终R = 0.0781, wR = 0.2367。邻苯二甲酸酯环的O-H基团与晶格水形成强氢键,稳定了晶体结构。
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引用次数: 4
Crystal Structure of 6-Bromo-1,2,4-triazin-3,5(2H,4H)-dione 6-溴-1,2,4-三嗪-3,5(2H,4H)-二酮的晶体结构
Pub Date : 2008-01-01 DOI: 10.2116/ANALSCIX.24.X201
L. Hwang, Li-Teh Liu, Yu-Chih Su, Gene-Hsiang Lee
The title compound, C3H2BrN3O2, bearing an H2O molecule, crystallizes in the monoclinic space group P21/c with a = 11.3794(7), b = 6.7248(6), c = 8.6383(10)A, β = 98.792(5)°, V = 653.27(10)A3 and Z = 4, resulting in a density, Dcalc, of 2.135 g/cm3. Each 1,2,4-triazine molecule is linked with seven adjacent molecules, including three H2O molecules. The molecules of the title compound are linked by a combination of extensive N-H…O, O-H…O intermolecular hydrogen bonds and N…Br interactions, leading to a continuous wave framework structure. The framework layers are further stabilized by intermolecular short contacts: N…O, C…O and Br…C.
该化合物C3H2BrN3O2携带一个H2O分子,在单斜空间群P21/c中结晶,a = 11.3794(7), b = 6.7248(6), c = 8.6383(10) a, β = 98.792(5)°,V = 653.27(10)A3, Z = 4,得到密度Dcalc为2.135 g/cm3。每个1,2,4-三嗪分子与7个相邻分子连在一起,包括3个H2O分子。标题化合物的分子通过广泛的N- h…O, O- h…O分子间氢键和N…Br相互作用的组合连接,导致连续波框架结构。通过分子间的短接触:N…O, C…O和Br…C进一步稳定了框架层。
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引用次数: 1
Crystal Structure and Absolute Configuration of Pendulone 钟摆酮的晶体结构和绝对构型
Pub Date : 2008-01-01 DOI: 10.2116/ANALSCIX.24.X209
Wen-hao Chen, Zhao-yan Ren, Rui Wang, Yan-ping Shi
The complete structure of the title compound, C17H16O6, isolated from the roots of Oxytropis falcata Bunge, was confirmed unambiguously by a single-crystal X-ray analysis. The absolute configuration was established by circular dichroism (CD). The bond distances and angles are within the expected ranges. The quinone ring is linked to the chroman ring by C(3) at an equatorial position. The crystal structure is also stabilized by intermolecular hydrogen bonds.
标题化合物C17H16O6从falcata Bunge棘豆(Oxytropis falcata Bunge)的根中分离得到完整的结构,通过单晶x射线分析得到了明确的证实。用圆二色性(CD)确定了绝对构型。键距和键角均在预期范围内。醌环在赤道位置由C(3)与铬环相连。分子间氢键也稳定了晶体结构。
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引用次数: 2
Crystal Structure of a Dinuclear Sodium Complex with a Phenol-based Dinucleating Ligand with Four Methoxyethyl Chelating Arms 具有四甲氧基螯合臂的酚基双核配体双核钠配合物的晶体结构
Pub Date : 2008-01-01 DOI: 10.2116/ANALSCIX.24.X177
Jun Shibayama, H. Sakiyama, M. Yamasaki, Y. Nishida
A pair of dinucleating ligands, 2,6-bis[bis(2-methoxyethyl)aminomethyl]-4-methylphenolate (bomp-), incorporates two sodium ions to form a dinuclear sodium complex, [Na2(bomp)2] (C42H74N4Na2O10). It crystallizes in the monoclinic space group P21/c with dimensions a = 19.9993(4)A, b = 9.9700(2)A, c = 24.3473(7)A, β = 98.8492(7)°, and V = 4796.89(19)A3 and with Z = 4. The two sodium ions are bridged by two phenoxo oxygen atoms of the bomp ligands to form a bis(μ-phenoxo)-dinuclear sodium(I) core structure. The Na…Na distance is 3.3261(6)A, and each sodium ion has a distorted octahedral geometry.
一对双核配体2,6-二[二(2-甲氧基乙基)氨基甲基]-4-甲基苯酚(bomp-)结合两个钠离子形成双核钠络合物[Na2(bomp)2] (C42H74N4Na2O10)。晶型为单斜空间群P21/c,尺寸为a = 19.9993(4) a, b = 9.9700(2) a, c = 24.3473(7) a, β = 98.8492(7)°,V = 4796.89(19)A3, Z = 4。这两个钠离子被庞普配体的两个苯氧氧原子桥接,形成双(μ-苯氧)-双核钠(I)核心结构。钠离子之间的距离为3.3261(6)A,每个钠离子具有扭曲的八面体结构。
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引用次数: 1
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Analytical Sciences: X-ray Structure Analysis Online
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