外型-1,4-氧桥-环己基-2,3-二羧酸的晶体及分子结构

外型-1,4-氧桥-环己基-2,3-二羧酸晶体属单斜晶系,空间群为P2_1/n;晶胞参数为:α=5.594(3)A,b=11.178(7)A,c=14.675(11)A,β=91.46(5)°;Ζ=4.从直接法得到结构的初始模型,经块矩阵最小二乘修正后,最后的R值为0.072.在晶体中,分子间的O—H…O氢键将分子连接成层型氢键体系.使用自编的CNDO/2程序,计算得电子的能量、分子的总能量、偶极矩及各原子的电荷密度和净电荷.     

Crystalline and molecular structure ofDL-2-amino-4-phosphonobutyric acid monohydrate

The crystalline and molecular structure ofDL-2-amino-4-phosphonobutyric acid monohydrate has been studied by means of x-ray diffraction analysis. The acid molecule exists in a zwitterionic form with a deprotonated PO₃H₂ group. In the crystalline structure there is a branched system of intermolecular hydrogen bonding and the unusual intermolecular bond C–H...O=C forming part of it has been found.Institute of Physiologically Active Compounds, Russian Academy of Sciences, 142432 Chernogolovka. Translated fromIzvestiya Akademii Nauk, Seriya Khimicheskaya, No. 11, pp. 2561–2565, November, 1992.     

Molecular and crystalline structure of 4-phenylthiosemicarbazidodiacetic acid monohydrate

Institute of Chemistry, Moldavian Academy of Sciences. Translated from Zhurnal Strukturnoi Khimii, Vol. 33, No. 2, pp. 177–180, March–April, 1992.     

Preparation,crystal structure and characterization of 2,4,6-trinitro-3,5-dimethylbenzoic acid monohydrate

In the present work, we synthesized 2,4,6-trinitro-3,5-dimethylbenzoic acid (TNDMBA). Single crystal of TNDMBA·H₂O was cultured from aqueous solution using a slow evaporation method at 30°C. The crystal structure was determined by X-ray single-crystal diffraction analysis. The crystal belongs to the monoclinic system with space group P2(1)/c having unit cell parameters of a = 17.24(3) Å, b = 6.032(1) Å, and c = 16.359(4) Å. There are two kinds of intermolecular H-bond interactions between H₂O and TNDMBA, which is different from typical carboxylic acids that form H-bond dimers across crystallographic centers of inversion. The title compound was characterized by FT-IR, DSC, and TG-DTG technologies, and calculated by using density functional theory (DFT) method. The calculated results show that the structural parameters from the theory are close to those of the crystal structure from the experiments. The compound is composed of three nitro groups and one carboxyl group, and it can be used as a potential energetic combustion catalyst in industry.     

Synthesis and crystal structure of benzyltrimethylammonium dicitratoborate monohydrate

Benzyltrimethylammonium dicitratoborate [C₆H₅CH₂N(CH₃)₃][(C₆H₆O₇)₂B] · H₂O (I) has been synthesized and separated out in the form of single crystals for the first time. Its crystal structure has been studied by X-ray diffraction. Crystals are triclinic with a = 10.0832(2) Å, b = 11.1232(3) Å, c = 11.9617(3) Å, α = 84.874(1)°, β = 73.520(1)°, γ = 85.550(1)°, Z = 2, space group P-1. The structure has been solved by direct methods and refined by the full-matrix least-squares technique in the anisotropic approximation up to R = 0.0485 (Bruker-Nonius KappaCCD automatic diffractometer, λMoK _α). The crystal structure of compound I is based on centrosymmetric dimers that consist of complex anions and water molecules and linked by the system of hydrogen bonds into a three-dimensional framework. The crystals of compound I contains five asymmetric O-H...O hydrogen bonds. A specific feature of the structure is the formation of -COO...H...H₂O hydrogen bonds, in which the carboxyl proton is considerably shifted towards the water molecule.     

Crystal and molecular structure of chlorohydroxyiminoacetamide monohydrate

Institute of Physiologically Active Substances, Academy of Sciences of the USSR. Translated from Zhurnal Strukturnoi Khimii, Vol. 31, No. 5, pp. 171–174, September–October, 1990.     

一水合二甲基磷酸镧的合成和晶体结构

用改进的重结晶及晶体与母液分离的方法合成了标题化合物La[PO2(OCH3)2]3·H2O, 其单晶的结构分析用Patterson 法及差值Fourier 合成, 并经分块矩阵最小二乘法对非氢原子进行修正解出,R=0.054, 属三斜品系, 空间群PI, a=11.342(4), b=10.399(4),c=9.619(3)A, a=62.01(3), β=72.39(3), λ=66.60(3),V=909.9(6)A3, Z=2, Dw=1.94g·cm^-^3。该晶体中每个La原子有七个氧原子配位, 其中六个氧原子分别由六个二甲基磷酸根提供, 另一个氧原子由水分子提供; 这个配位多面体呈扭曲的单帽三棱柱体, 远程结构呈二维网状, 系因每两个La 原子共用一个二甲基磷酸根离子延伸连接而成。     

The crystal and molecular structure of phenothiazine-10-propionic acid

The crystal structure of phenothiazine-10-propionic acid, C₁₂H₈SNC₂H₄COOH, was determined from three-dimensional X-ray diffraction data collected with a manual diffractomer using MoKα (λ 0.71069 Å) radiation. The space group is P2₁/c with a = 7.888 (2)Å, b = 8.703 (2)Å, c = 19.700 (8)Å, β = 101.42 (1)°, Z = 4, D_meas = 1.35(2) g. cm^?3 and D_calc = 1.36 g. cm^?3 at 23°. The structure was determined by the direct method and refined with 500 observed reflections by full-matrix least squares to an R of 0.072. The molecule is folded along the S-N axis and the dihedral angle is 136.5°. The C-S-C angle is 98.5(7)° and the average C-S bond is 1.77(2)Å. The shortening of the C-S bond, the small value of the C-S-C angle and the folding of the molecule are typical of the phenothiazine class of compounds and are assumed to be due to sulfur d orbital participation in ring bonding.     

Sparfloxacindium tetrabromidocuprate(II) monohydrate crystal structure

Structure solution has been carried out for a compound containing doubly charged sparfloxacindium cation, namely ((C₁₉H₂₄F₂N₄O₃)[CuBr₄] · H₂O (I), where C₁₉H₂₂F₂N₄O₃ is sparfloxacin. The crystals of I are orthorhombic with a = 14.533(4) Å, b = 12.557(4) Å, c = 29.370(9) Å, V = 2360(3) ų, space group Pbca, Z = 8. In compound I, unlike in similar compounds of other fluoroquinolones, the second proton is attached to the sparfloxacin through the amino nitrogen atom instead of being attached through the ketone oxygen atom. This specific protonation feature of SfH is manifested in the specifics of supramolecular organization of I.     

Synthesis and molecular structure of potassium 3,5-dinitrophloroglucinolsulfonate monohydrate

A novel coordination polymer, potassium 3,5-dinitrophloroglucinolsulfonate monohydrate ([K(DNPGS) (H₂O)] _n ), was synthesized by the reaction of 3,5-dinitrophloroglucinolsulfonic acid (DNPGS) with potassium hydroxide in aqueous solution and the structure was determined by elemental analysis, IR and x-ray single-crystal diffraction analysis. The crystal belongs to orthorhombic system with space group Pca2(1). Its unit cell parameters are as follows: a=1.0819(14) nm, b=0.56563(11) nm, c=1.8979(4) nm; V=1.1615(4) nm³, Z=4, D _c =2.015 g/cm³, F(000)=712, chemical formula C₆H₅KN₂O₁₁S and M _r =352.28. The bridging potassium ion coordinates with nine oxygen atoms originating from the sulfonic groups, phenolic hydroxyl groups, nitro-groups of five DNPGS⁻ anions and two water molecules simultaneously, and a stable cross-linked three-dimensional network is formed. The thermal analysis of the complex show that it dehydrates at about 100°C, and only has an intense exothermic process at 204.2–245.2°C with exothermic enthalpy 1383.4 kJ mol⁻¹.     

Synthesis and crystal structure of the complex N,N-dimethylanilinium dicitratoborate monohydrate

N,N-Dimethylanilinium dicitratoborate monohydrate [C₆H₅NH(CH₃)₂][(C₆H₆O₇)₂B]·H₂O (I) was synthesized for the first time. Single crystals were obtained in an aqueous solution; the crystal structure was studied by X-ray crystallography. Crystals of I are triclinic, space group $P\bar 1$ , a = 9.7017(2) ?, b = 11.0475(2) ?, c = 12.6282(2) ?, ?? = 106.595(2)°, ?? = 106.931(1)°, ?? = 103.568(1)°, V = 1163.97(4) ?³, Z = 2, ??_calc = 1.516 g/cm³. The structural units of compound 1 are large complex dicitratoborate anions with a spiran structure, N,N-dimethylanilinium cations, and crystal water molecules. The crystal packing is a three-dimensional framework. A hydrogen-bond system is formed by seven independent contacts O(N)-H??O.