The Preparation and Crystal Structures of the 1 : 1 Adducts of 5-Nitrosalicylic Acid and 2-Chloro-3,5- dinitrobenzoic Acid with Triphenylphosphine Oxide

1998 ◽  
Vol 51 (5) ◽  
pp. 437 ◽  
Author(s):  
Graham Smith ◽  
Daniel E. Lynch ◽  
Colin H. L. Kennard ◽  
Karl A. Byriel
Keyword(s):  
Hydrogen Bond ◽  
Hydrogen Bonding ◽  
Triphenylphosphine Oxide ◽  
Monoclinic Space Group ◽  
Intermolecular Hydrogen Bonding ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
X Ray ◽  
Hydrogen Bonding Interactions ◽  
Phosphoryl Oxygen

The (1 : 1) adducts of 5-nitrosalicylic acid (5-nsa) and 2-chloro-3,5-dinitrobenzoic acid (cdnba) with triphenylphosphine oxide (tppo), [(5-nsa)(tppo)] (1) and [(cdnba)(tppo)] (2), have been prepared and their structures determined by X-ray diffraction and reffned to residuals R 0·045 (1) and 0·043 (2) for 2540 and 3265 observed reflections respectively. Crystals of both adducts are monoclinic, space group P21/c (1) and P21/a (2), with 4 dimer units in cells of dimensions a 16·217(1), b 7·6807(8), c 19·697(4) Å, β 113·357(8)° [for (1)] and a 16·009(5), b 8·687(1), c 17·640(5) Å, β 90·30(1)o [for (2)]. In both examples, the two molecules comprising the asymmetric unit are linked by a single hydrogen bond between the proton of the carboxylic acid and the phosphoryl oxygen of tppo [O- - -O, 2·524(3) Å (1); 2·72(3) Å (2)], while, in each case, the additional functional groups of the acid are not involved in any other intermolecular hydrogen-bonding interactions.

scholarly journals Single-crystal X-ray diffraction study of a host–guest system comprising monofunctionalized-hydroxy pillar[5]arene and 1-octanamine

2018 ◽  
Vol 74 (8) ◽  
pp. 1117-1120
Author(s):  
Talal F. Al-Azemi ◽  
Mickey Vinodh ◽  
Abdirahman A. Mohamod ◽  
Fatemeh H. Alipour
Keyword(s):  
Hydrogen Bonding ◽  
Alkyl Chain ◽  
Supramolecular Interactions ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
X Ray ◽  
Hydrogen Bonding Interactions ◽  
Guest Species ◽  
Guest System ◽  
Macrocycle Cavity

Co-crystallization of a monofunctionalized hydroxy pillar[5]arene with 1-octanamine resulted in the formation of an inclusion complex where the alkyl chain is threaded in the macrocycle cavity, namely 1,2,3,4-(1,4-dimethoxy)-5-(1-hydroxy-4-methoxy)-pillar[5]arene–1-octanamine–water (1/1/1), C44H48O10·C8H19N·H2O. The guest compound is stabilized inside the cavity by hydrogen-bonding and C—H...π interactions. The water molecule in the asymmetric unit mediates the formation of a supramolecular dimer by hydrogen-bonding interactions. These functionalized-pillararene hosts expand the possibility of exploring more supramolecular interactions with various guest species.

A molecular crown analogue templated by Keggin polyanions: synthesis, structure, and electrochemical and luminescent properties

2015 ◽  
Vol 70 (8) ◽  
pp. 547-553 ◽  
Author(s):  
Chunyan Zhao ◽  
Huiyuan Ma ◽  
Haijun Pang ◽  
Yan Yu ◽  
Shaobin Li ◽  
...  
Keyword(s):  
Hydrogen Bonding ◽  
Infrared Spectroscopy ◽  
Luminescent Properties ◽  
Intermolecular Hydrogen Bonding ◽  
X Ray Diffraction ◽  
Hydrothermal Conditions ◽  
Hybrid Compound ◽  
X Ray ◽  
Hydrogen Bonding Interactions ◽  
Elemental Analyses

AbstractA hybrid compound, [CuI4(bpmb)4][PWVI11WVO40] (1) (bpmb = 1,4-bis(pyrazol-1-ylmethyl)benzene), has been synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction analysis, infrared spectroscopy, elemental analyses and powder X-ray diffraction. In compound 1 crown-like [Cu4(bpmb)4]4+ macrocycles templated by Keggin-type [PWVI11WVO40]4− polyanions (abbreviated PW12) exist. Supramolecular layers are formed by intermolecular hydrogen bonding interactions of discrete crown-like [Cu4(bpmb)4]4+ macrocycles and [PWVI11WVO40]4− polyanions. The electrochemical and luminescence properties of compound 1 were investigated.

Molecular Cocrystals of Carboxylic Acids. XIV. The Crystal Structures of the Adducts of Pyrazine-2,3-dicarboxylic Acid With 4-Aminobenzoic Acid, 3-Hydroxypyridine and 3-Amino-1,2,4-triazole

1994 ◽  
Vol 47 (2) ◽  
pp. 309 ◽  
Author(s):  
DE Lynch ◽  
G Smith ◽  
KA Byriel ◽  
CHL Kennard ◽  
AK Whittaker
Keyword(s):  
Hydrogen Bonding ◽  
Dicarboxylic Acid ◽  
Crystal Structures ◽  
Molecular Hydrogen ◽  
Triphenylphosphine Oxide ◽  
Spectroscopic Methods ◽  
Aminobenzoic Acid ◽  
X Ray Diffraction ◽  
X Ray ◽  
Hydrogen Bonding Interactions

The 1:1 molecular adducts of pyrazine-2,3-dicarboxylic acid with 4-aminobenzoic acid, [(C6H3N2O4)-(C7H8NO2)+], 3-hydroxypyridine, [(C6H4N2O4) (C5H5NO)], and 3-amino-1,2,4-triazole, [(C6H3N2O4)-(C2H5N4)+] have been prepared, and their structures determined by X-ray diffraction methods. All structures involve intra- and inter-molecular hydrogen-bonding interactions. The 1:2 complex of pyrazine-2,3-dicarboxylic acid with triphenylphosphine oxide has also been prepared, and characterized by using spectroscopic methods.

scholarly journals Exploring the Structural Chemistry of Pyrophosphoramides: N,N′,N″,N‴-Tetraisopropylpyrophosphoramide

Chemistry ◽  
2021 ◽  
Vol 3 (1) ◽  
pp. 149-163
Author(s):  
Duncan Micallef ◽  
Liana Vella-Zarb ◽  
Ulrich Baisch
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nuclear Magnetic Resonance ◽  
Hydrogen Bonding ◽  
Nmr Spectroscopy ◽  
Ir Spectroscopy ◽  
Room Temperature ◽  
Intermolecular Hydrogen Bonding ◽  
X Ray Diffraction ◽  
X Ray

N,N′,N″,N‴-Tetraisopropylpyrophosphoramide 1 is a pyrophosphoramide with documented butyrylcholinesterase inhibition, a property shared with the more widely studied octamethylphosphoramide (Schradan). Unlike Schradan, 1 is a solid at room temperature making it one of a few known pyrophosphoramide solids. The crystal structure of 1 was determined by single-crystal X-ray diffraction and compared with that of other previously described solid pyrophosphoramides. The pyrophosphoramide discussed in this study was synthesised by reacting iso-propyl amine with pyrophosphoryl tetrachloride under anhydrous conditions. A unique supramolecular motif was observed when compared with previously published pyrophosphoramide structures having two different intermolecular hydrogen bonding synthons. Furthermore, the potential of a wider variety of supramolecular structures in which similar pyrophosphoramides can crystallise was recognised. Proton (1H) and Phosphorus 31 (31P) Nuclear Magnetic Resonance (NMR) spectroscopy, infrared (IR) spectroscopy, mass spectrometry (MS) were carried out to complete the analysis of the compound.

A New Organic-Inorganic Hybrid Based on L-Arginine and Polyoxoanion

2015 ◽  
Vol 1105 ◽  
pp. 335-338
Author(s):  
Qiong Wu ◽  
Jing Lu ◽  
Xiao Lin Ji ◽  
Tao Yu Zou ◽  
Zhen Fang Qiao ◽  
...  
Keyword(s):  
Hydrogen Bonding ◽  
Sodium Cation ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
Inorganic Hybrid ◽  
X Ray ◽  
Hydrogen Bonding Interactions ◽  
Photocatalytic Activities ◽  
Metal Organic ◽  
Supramolecular Networks

Modifying polyoxometalates with organic and/or metal-organic moieties is a widely adopted method for broading the range of properties. In this work a new polyoxometalate constructed from Anderson-type polyoxoanions and L-arginine (Arg =L-arginine) molecules Na [CrMo6(OH)6O18]}(H2Arg)2·8H2O(1) has been synthesized via conventional method and characterized by routine techniques. Single-crystal X-Ray diffraction analysis shows that compound 1 is constructed by chiralL-arginine grafted Anderson-type clusters, sodium cation and water molecules which are further stabilized by hydrogen bonding interactions constitute 3D supramolecular networks. In addition, both antitumor behavior and photocatalytic activities of compound 1 were investigated.

A New POM-Based Supramolecular Compound: Synthesis, Structure and Adsorptive Property of [Cu(phen)2]3[W6O19]

2014 ◽  
Vol 919-921 ◽  
pp. 2013-2016 ◽  
Author(s):  
Ya Bing Liu ◽  
Hong Jie Wang ◽  
Hong Kai Zhao
Keyword(s):  
Three Dimensional ◽  
Building Blocks ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Hybrid Compound ◽  
Adsorptive Property ◽  
X Ray ◽  
Hydrogen Bonding Interactions ◽  
Compound Synthesis ◽  
Metal Organic

A POM - based organice - inorganic hybrid compound with the chemical formula of[Cu (phen)2]3[W6O19] (phen = 1,10-phenanthroline) (1) has been hydrothermally synthesized andstructurally characterized by the elemental analysis, and single crystal X-ray diffraction. Compound 1 crystallizes in the monoclinic space groupC2/c witha=18.319(4) Å,b= 17.311(4) Å,c= 22.248(4) Å,β= 112.40(3) o,V= 6523(2) Å3,Z= 4, R1= 0.0448, andwR2=0.1218. Compound 1 consists of the [W6O19]3-building blocks and [Cu (phen)2]+metal organic cationic moieties, which are packed together via the extensive hydrogen-bonding interactions to form a three-dimensional supramolecular framework. The adsorption of methylene blue (MB) under UV irradiation with 1 as the heterogeneous adsorbent has been investigated, showing a good adsorptive property of 1 for MB degradation.

Study on Novel Structure of Praseodymium Complex, C5H13O11Pr

2013 ◽  
Vol 834-836 ◽  
pp. 515-518
Author(s):  
Hai Xing Liu ◽  
Qing Liu ◽  
Ting Ting Huang ◽  
Yang Xu ◽  
Lin Tong Wang ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Single Crystal ◽  
Hydrothermal Reaction ◽  
Crystal Packing ◽  
X Ray Diffraction ◽  
X Ray ◽  
Hydrogen Bonding Interactions ◽  
Novel Structure ◽  
Praseodymium Complex

A novel praseodymium complex C5H13O11Pr has been synthesized from hydrothermal reaction and the crystal structure has been determined by means of single-crystal X-ray diffraction. The Pr1 atom is nine coordinated by nine O atoms. The crystal packing is stabilized by O-H...O hydrogen bonding interactions.

The preparation, characterization, structure and dissolution analysis of apremilast solvatomorphs

2017 ◽  
Vol 73 (4) ◽  
pp. 305-313 ◽  
Author(s):  
Yun-Deng Wu ◽  
Xiao-Lei Zhang ◽  
Xiao-Hong Liu ◽  
Jian Xu ◽  
Mei Zhang ◽  
...  
Keyword(s):  
Differential Scanning Calorimetry ◽  
Hydrogen Bonding ◽  
Psoriatic Arthritis ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Dissolution Rates ◽  
X Ray ◽  
Similarity Factor ◽  
Hydrogen Bonding Interactions

Apremilast (AP) {systematic name: (S)-2-[1-(3-ethoxy-4-methoxyphenyl)-2-(methylsulfonyl)ethyl]-4-acetamidoisoindoline-1,3-dione} is an inhibitor of phosphodieasterase-4 (PDE4) and is indicated for the treatment of adult patients with active psoriatic arthritis. The ability of AP to form solvates has been investigated and three solvatomorphs of AP, namely, the AP ethyl acetate hemisolvate, C22H24N2O7S·0.5C4H8O2, the AP toluene hemisolvate, C22H24N2O7S·0.5C7H8, and the AP dichloromethane monosolvate, C22H24N2O7S·CH2Cl2, were obtained. The three AP solvatomorphs were characterized by X-ray powder diffraction, thermogravimetric analysis and differential scanning calorimetry. Single-crystal X-ray diffraction was used to analyze the structures, crystal symmetry, packing modes, stoichiometry and hydrogen-bonding interactions of the solvatomorphs. In addition, dissolution analyses were performed to study the dissolution rates of different AP solvatomorph tablets in vitro and to make comparisons with commercial apremilast tablets (produced by Celgene); all three solvatomorphs showed similar dissolution rates and similar values of the similarity factor f2 in a comparison of their dissolution profiles.

Synthese, Struktur und thermisches Verhalten von Thiophosphorsäuretriamid SP(NH2)3 [1] / Synthesis, Structure, and Thermal Behaviour of Phosphorothionic Triamide SP(ΝΗ2)3 [1]

1989 ◽  
Vol 44 (8) ◽  
pp. 942-945 ◽  
Author(s):  
Wolfgang Schnick
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Thermal Properties ◽  
Single Crystal ◽  
Melting Temperature ◽  
Intermolecular Hydrogen Bonding ◽  
X Ray ◽  
Hydrogen Bonding Interactions ◽  
Ray Methods ◽  
Single Bonds

Phosphorothionic triamide SP(NH2)3 is obtained by slow addition of SPCl3 dissolved in dry CH2Cl2 to a satured solution of NH3 in CH2Cl2 at —50°C. Ammonium chloride is removed from the resulting precipitate by treatment with HNEt2 followed by extraction with CH2Cl2. Coarse crystalline SP(NH2)3 is obtained after recrystallization from dry methanol. The crystal structure of SP(NH2)3 has been determined by single crystal X-ray methods (Pbca; a = 922.3(1), b = 953.8(1), c = 1058.4(2) pm, Z = 8). In the crystals the molecules show non-crystallographic point symmetry C8. The P—S bond (195.4(1) pm) is slightly longer than in SPCl3. From P—N bond lengths of about 166 pm a significant electrostatic strengthening of the P—N single bonds is assumed. Weak intermolecular hydrogen bonding interactions (N —H · · · N ≥ 329.5 pm; N — H · · · S ≥ 348.3 pm) are observed.Investigation of thermal properties shows a melting temperature of 115°C for SP(NH2)3. According to combined DTA/TG and MS investigations above this temperature the compound decomposes by evolution of H2S and NH3 to yield amorphous phosphorus(V)nitride.

Synthesis of Glycolic and Oxalic Acid Europium: [Eu (C3 H6O9)] ·2(H2O)

2012 ◽  
Vol 554-556 ◽  
pp. 792-795
Author(s):  
Hai Xing Liu ◽  
Jing Wang ◽  
Fang Fang Jian ◽  
Hui Juan Yue ◽  
Guang Zeng ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Oxalic Acid ◽  
Single Crystal ◽  
Hydrothermal Reaction ◽  
X Ray Diffraction ◽  
X Ray ◽  
Hydrogen Bonding Interactions ◽  
The Eu

A new Eu complex [Eu (C3O9H6)] ·2(H2O) has been synthesized from a hydrothermal reaction and the crystal structure has been determined by means of single-crystal X-ray diffraction. The Eu atom is coordinated by eight O atoms. The molecular is antisymmetric structure by the C3-C3 axis. It is striking that the structure of the complex exhibits extensive O-H…O hydrogen-bonding interactions.

Sign in / Sign up

Export Citation Format

Share Document