Mechanochemical synthesis and X-ray structural characterization of three 3-nitrophenol cocrystals with three aminal cage azaadamantanes: the role of the stereoelectronic effect on intermolecular hydrogen-bonding patterns

2019 ◽  
Vol 75 (12) ◽  
pp. 1635-1643
Author(s):  
Augusto Rivera ◽  
Jicli José Rojas ◽  
John Sadat-Bernal ◽  
Jaime Ríos-Motta ◽  
Michael Bolte
Keyword(s):  
Hydrogen Bonds ◽  
Slow Evaporation ◽  
X Ray Diffraction ◽  
X Ray ◽  
Stereoelectronic Effect ◽  
Supramolecular Architectures ◽  
Grinding Method ◽  
Aminal Cage

The structures of the cocrystalline adducts of 3-nitrophenol (3-NP) with 1,3,5,7-tetraazatricyclo[3.3.1.13,7]decane [HMTA, (1)] as the 2:1:1 hydrate, 2C6H5NO3·C6H12N4·H2O, (1a), with 1,3,6,8-tetraazatricyclo[4.3.1.13,8]undecane [TATU (2)] as the 2:1 cocrystal, 2C6H5NO3·C7H14N4, (2a), and with 1,3,6,8-tetraazatricyclo[4.4.1.13,8]dodecane [TATD, (3)] as the 2:1 cocrystal, 2C6H5NO3·C8H16N4, (3a), are reported. In the binary crystals (2a) and (3a), the 3-nitrophenol molecules are linked via O—H...N hydrogen bonds into aminal cage azaadamantanes. In (1a), the structure is stabilized by O—H...N and O—H...O hydrogen bonds, and generates ternary cocrystals. There are C—H...O hydrogen bonds present in all three cocrystals, and in (1a), there are also C—H...O and C—H...π interactions present. The presence of an ethylene bridge in the structures of (2) and (3) defines the formation of a hydrogen-bonded motif in the supramolecular architectures of (2a) and (3a). The differences in the C—N bond lengths of the aminal cage structures, as a result of hyperconjugative interactions and electron delocalization, were analysed. These three cocrystals were obtained by the solvent-free assisted grinding method. Crystals suitable for single-crystal X-ray diffraction were grown by slow evaporation from a mixture of hexanes.

Growth and Characterization of Ammonium Dihydrogen Phosphate (ADP) Doped with H3BO3 Crystals Grown by Slow Evaporation Method

2016 ◽  
Vol 675-676 ◽  
pp. 573-576 ◽  
Author(s):  
Pratya Thongpanit ◽  
Weerapong Chewpraditkul ◽  
Nakarin Pattanaboonmee
Keyword(s):  
Boric Acid ◽  
Temperature Stability ◽  
Hardness Measurement ◽  
Dihydrogen Phosphate ◽  
Ammonium Dihydrogen Phosphate ◽  
Slow Evaporation ◽  
X Ray Diffraction ◽  
X Ray ◽  
Evaporation Method

Ammonium dihydrogen phosphate (ADP) crystals is very interesting due to its nonlinear optical property. This study investigated on improving of material for academic use by adding boric acid to modify ADP crystals. Slow evaporation method in aqueous solutions of pure ADP and ADP doped with three concentrations of H3BO3 as 0.1, 1.0, 5.0 %wt were studied. The grown crystals were confirmed tetragonal structure by powder X-ray diffraction studies. The FTIR spectrum analysis presented various functional groups of boron in three conditions of doped ADP. TGA study was comfirned the temperature stability at 220 °C for both pure and doped ADP crytals. The machanical stress was analyzed by Vicker’s hardness measurement. The results of this analysis showed boric acid doped 1.0 %wt had superior machanical stress from 10 to 75 grams. ADP doped with boric acid at 1.0 %wt was accepted in all test properties.

scholarly journals Perbaikan Kelarutan Albendazol Melalui Pembentukan Kristal Multikomponen dengan Asam Malat

2020 ◽  
Vol 6 (1) ◽  
pp. 114-123
Author(s):  
Fikri Alatas ◽  
Fahmi Abdul Azizsidiq ◽  
Titta Hartyana Sutarna ◽  
Hestyari Ratih ◽  
Sundani Nurono Soewandhi
Keyword(s):  
Phase Solubility ◽  
Crystal Formation ◽  
Solubility Curve ◽  
X Ray Diffraction ◽  
Ethanol Mixture ◽  
X Ray ◽  
Grinding Method ◽  
Diffraction Patterns ◽  
Phase Solubility Curve

An effort to improve the solubility of albendazole (ABZ), an anthelmintic drug has been successfully carried out through the formation of multicomponent crystal with dl-malic acid (MAL). Construction of phase solubility curve of ABZ in MAL solution and crystal morphological observations after recrystallization in the acetone-ethanol (9:1) mixture were performed for initial prediction of multicomponent crystal formation. ABZ-MAL multicomponent crystal was prepared by wet grinding or also known as solvent-drop grinding (SDG) with acetone-ethanol (9:1) mixture as a solvent followed by characterization of the multicomponent crystal formation by powder X-ray diffraction and Fourier transform infrared (FTIR) methods. The solubility of ABZ-MAL multicomponent crystal was tested in water at ambient temperature and in pH 1.2, 4.5 and 6.8 of buffered solutions at 37°C. The phase solubility curve of the ABZ in the MAL solution showed type Bs. The ABZ-MAL mixture has a different crystalline morphology than pure ABZ and MAL after recrystallization in the acetone-ethanol mixture (9:1). The powder X-ray diffraction pattern and the FTIR spectrum of ABZ-MAL from SDG different from intact ABZ and MAL powder X-ray diffraction patterns and these results can indicate the ABZ-MAL multicomponent crystal formation. The ABZ-MAL multicomponent crystal has better solubility than pure ABZ in all media used. These results can be concluded that ABZ-MAL multicomponent crystal can be prepared by solvent-drop grinding method with acetone-ethanol (9:1) mixture as a solvent and can increase the solubility of albendazole.

Characterization of Titanium Dioxide Nanopowder Synthesized by Sol Gel Grinding Method

2012 ◽  
Vol 626 ◽  
pp. 425-429 ◽  
Author(s):  
N.N. Hafizah ◽  
Mohamed Zahidi Musa ◽  
Mohamad Hafiz Mamat ◽  
M. Rusop
Keyword(s):  
Electron Microscopy ◽  
Anatase Phase ◽  
Sol Gel ◽  
Precursor Concentration ◽  
X Ray Diffraction ◽  
X Ray ◽  
Grinding Method ◽  
Fesem Micrographs ◽  
Scanning Electron

In this study, TiO2nanopowder was synthesized via a sol-gel grinding method. The effects of TiO2precursor concentration of TiO2nanopowder were investigated. The TiO2nanopowder obtained were characterized using X-ray diffraction (XRD), Raman spectroscopy and field emission scanning electron microscopy (FESEM) for their structural properties. From the calculation of the crystallite size in XRD, the size of the nanoparticles obtained is 49.55 nm at the highest TiO2precursor concentration. In contrast, at the lower concentration of 0.4 molar give the cryatallite size of 12.84 nm. Further, XRD and Raman spectrum results confirmed the TiO2nanopowder obtain composed of only anatase phase. The FESEM micrographs of TiO2nanopowder also were discussed in this paper.

Synthesis and Characterization of Three Novel Nitrogen-containing Macrolides

2011 ◽  
Vol 66 (9) ◽  
pp. 930-934
Author(s):  
Xin Leng ◽  
Bingqin Yang ◽  
Yuanyuan Liu ◽  
Yi Xie ◽  
Jie Tong
Keyword(s):  
Nmr Spectroscopy ◽  
Hydrogen Bonds ◽  
1H Nmr Spectroscopy ◽  
Mass Spectra ◽  
Synthesis And Characterization ◽  
Stacking Interactions ◽  
X Ray Diffraction ◽  
Preparation Methods ◽  
X Ray

Three novel nitrogen-containing macrolides have been synthesized by esterification. All of them have been characterized by infrared (IR), elemental analysis, mass spectra (MS), and 1H NMR spectroscopy, and their crystal structures were determined by single-crystal X-ray diffraction. The preparation methods and the intermolecular associations based on C-H・・・O hydrogen bonds and π- π stacking interactions are discussed.

Supramolecular architectures in two 1:1 cocrystals of 5-fluorouracil with 5-bromothiophene-2-carboxylic acid and thiophene-2-carboxylic acid

2017 ◽  
Vol 73 (6) ◽  
pp. 481-485 ◽  
Author(s):  
Marimuthu Mohana ◽  
Packianathan Thomas Muthiah ◽  
Colin D. McMillen
Keyword(s):  
Solid State ◽  
Carboxylic Acid ◽  
Hydrogen Bonds ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
Base Pairs ◽  
X Ray ◽  
Supramolecular Architectures ◽  
Acid Acid ◽  
Carboxylic Acid Dimer

In solid-state engineering, cocrystallization is a strategy actively pursued for pharmaceuticals. Two 1:1 cocrystals of 5-fluorouracil (5FU; systematic name: 5-fluoro-1,3-dihydropyrimidine-2,4-dione), namely 5-fluorouracil–5-bromothiophene-2-carboxylic acid (1/1), C5H3BrO2S·C4H3FN2O2, (I), and 5-fluorouracil–thiophene-2-carboxylic acid (1/1), C4H3FN2O2·C5H4O2S, (II), have been synthesized and characterized by single-crystal X-ray diffraction studies. In both cocrystals, carboxylic acid molecules are linked through an acid–acid R 2 2(8) homosynthon (O—H...O) to form a carboxylic acid dimer and 5FU molecules are connected through two types of base pairs [homosynthon, R 2 2(8) motif] via a pair of N—H...O hydrogen bonds. The crystal structures are further stabilized by C—H...O interactions in (II) and C—Br...O interactions in (I). In both crystal structures, π–π stacking and C—F...π interactions are also observed.

Synthesis and Characterization of the nido-Platinaborane 7,7-(PPh3)2-7-PtB10H11-11-OC(O)Me

2011 ◽  
Vol 66 (4) ◽  
pp. 387-391
Author(s):  
Jinling Miao ◽  
Yong Nie ◽  
Haiyan Chen ◽  
Daqi Wang ◽  
Markus Enders ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Chain Structure ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ir And Nmr Spectroscopy

The reaction of closo-B10H102− with PtCl2(PPh3)2 in the presence of MeCOSH afforded the title platinaborane nido-7,7-(PPh3)2-7-PtB10H11-11-OC(O)Me (1), which has been characterized by IR and NMR spectroscopy, MS, elemental analysis, and single-crystal X-ray diffraction. In contrast to the known products having exo-polyhedral Pt-S-C-O-B ring(s) from the same reaction with Ph- COSH, compound 1 has a B-acetoxy group on the open PtB4 face of the nido-PtB10 cluster. The structure of 1 features both intramolecular/intermolecular C-H· · ·O hydrogen bonds and intramolecular C-H· · ·H-B dihydrogen bonds, which link the molecules into a 1-D chain structure.

Synthesis and characterization of dicarboranylmethylammonium polyoxometallates

2010 ◽  
Vol 75 (11) ◽  
pp. 1075-1096 ◽  
Author(s):  
Ramón Macías ◽  
John D. Kennedy ◽  
Jonathan Bould ◽  
Mark Thornton-Pett
Keyword(s):  
Hydrogen Bonds ◽  
Single Crystal ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Pyridinium Cation ◽  
Network Of Hydrogen Bonds ◽  
Work Up ◽  
Acetone Hexane

The reaction of [C2B10H11CH2NH3]Cl (3) with [NH4]6[Mo7O24][H2O]4 in water instantly afforded a white precipitate: crystallization from acetone–hexane thence gave the hybrid dicarborane octamolybdate salt, [C2B10H11CH2NH3]2[C2B10H11CH2NH=CMe2]2[Mo8O26][Me2CO]4.5 (5), whereas crystallization from acetonitrile–ether gave three further salts: [C2B10H11CH2NH3]2[C2B10H11CH2NH2CHMe2]2[Mo8O26][MeCN]2 (6), [C2B10H11CH2NH3]4[Mo8O26][MeCN]2[Et2O]2 (7) and [C2B10H11CH2NH3]2[C2B10H11CH2NH2Et]2[Mo8O26][MeCN]2 (8). Similarly, treatment of an acidified solution of Na2WO4 with [C2B10H11CH2NH3]Cl (3) in water also yielded a white precipitate: crystallization from acetone–hexane afforded the salt [C2B10H11CH2NH=CHMe2]4[W10O32][H2O]2[Me2CO]4 (10), whereas crystallization from acetonitrile–ether gave the double salt [C2B10H11CH2NH3]2[C5H5NH]2[W10O32][MeCN]2-[Et2O] (11). All these ‘globule–globule’ salts 5, 6, 8, 10 and 11 have been characterized by single-crystal X-ray diffraction analyses. Crystal structures reveal the presence of various small solvate molecules, together with an extensive network of hydrogen bonds between ammonium groups and oxygen atoms of the isopolyoxometallates. The isopropyl substituent in one of the carborane cations of the salts 6 and the ethyl substituent in one of the carborane cations of salts 8 may result from occluded isopropanol and ethanol in the starting salt 3 with alkylations of the primary ammonium group being assisted by isopolymolybdate anions. The presence of the pyridinium cation in 11 is believed to arise from contamination during work-up the reaction mixture.

scholarly journals Synthesis of Iron Oxide Nanoparticles Using Isobutanol

2016 ◽  
Vol 2016 ◽  
pp. 1-9 ◽  
Author(s):  
Diana Kostyukova ◽  
Yong Hee Chung
Keyword(s):  
Iron Oxide ◽  
Iron Oxide Nanoparticles ◽  
Ammonium Hydroxide ◽  
Oxide Nanoparticles ◽  
X Ray Diffraction ◽  
Ferrous Chloride ◽  
X Ray ◽  
Superparamagnetic Properties

Iron oxide nanoparticles were synthesized by precipitation in isobutanol with sodium hydroxide and ammonium hydroxide. The isobutanol played a role of a surfactant in the synthesis. The nanoparticles were calcined for 100 min to 5 hours in the range of 300 to 600°C. The characterization of the samples by FTIR (Fourier-transform infrared) and XRD (X-ray diffraction) confirmed the formation ofγ-Fe2O3(maghemite) from Fe3O4(magnetite) at calcination at 300°C. The morphology and particle size were studied by SEM (scanning electron microscope). Nanoparticles in the range of 11–22 nm prepared at 0.09 M of ferrous chloride exhibited superparamagnetic properties. Nanoparticles synthesized with ferrous chloride and ammonium hydroxide at 75°C and calcined at 530°C for 2 h wereα-Fe2O3(hematite).

scholarly journals Growth and Characterization of High-Quality GaN Nanowires on PZnO and PGaN by Thermal Evaporation

2011 ◽  
Vol 2011 ◽  
pp. 1-6 ◽  
Author(s):  
L. Shekari ◽  
H. Abu Hassan ◽  
S. M. Thahab ◽  
Z. Hassan
Keyword(s):  
Gallium Nitride ◽  
Thermal Evaporation ◽  
Lattice Mismatch ◽  
Growth Direction ◽  
X Ray Diffraction ◽  
X Ray ◽  
Gan Nanowires ◽  
Transmission Electron

In the current research, an easy and inexpensive method is used to synthesize highly crystalline gallium nitride (GaN) nanowires (NWs) on two different substrates [i.e., porous zinc oxide (PZnO) and porous gallium nitride (PGaN)] on Si (111) wafer by thermal evaporation without any catalyst. Microstructural studies by scanning electron microscopy and transmission electron microscope measurements reveal the role of the substrates in the nucleation and alignment of the GaN NWs. Further structural and optical characterizations were performed using high-resolution X-ray diffraction, energy-dispersive X-ray spectroscopy, and photoluminescence spectroscopy. Results indicate that the NWs have a single-crystal hexagonal GaN structure and growth direction in the (0001) plane. The quality and density of GaN NWs grown on different substrates are highly dependent on the lattice mismatch between the NWs and their substrates. Results indicate that NWs grown on PGaN have better quality and higher density compared to NWs on PZnO.

scholarly journals Synthesis and characterization of 2CuCN·DMSO and [CuII(DMSO)6][CuI 6(CN)8] 3-D framework compounds

2013 ◽  
Vol 11 (6) ◽  
pp. 1001-1009 ◽  
Author(s):  
Andrii Vakulka ◽  
Evgeny Goreshnik
Keyword(s):  
Raman Spectroscopy ◽  
Mixed Valence ◽  
Synthesis And Characterization ◽  
Ligand Molecule ◽  
X Ray Diffraction ◽  
X Ray ◽  
Anionic Framework ◽  
Framework Compounds

AbstractTwo novel complexes of CuCN were characterized by using a single-crystal X-ray diffraction technique and Raman spectroscopy. In the structure of 2CuCN·DMSO ligand molecule demonstrates unique bridging mode, being bound to two CuI centers via oxygen and sulfur atoms. The bridging role of both CN groups and DMSO molecules results in the formation of (CuCN·DMSO)n framework. Along the channels of the network are running infinite zig-zag (CuCN)n chains, which are bound to the framework by elongated Cu…(CN) bonds. A mixed-valence [CuII(DMSO)6][CuI 6(CN)8] compound is composed of 3-D [CuI 6(CN)8]n anionic framework and located in the channels of partially disordered [CuII(DMSO)6]2+ cations.

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