scholarly journals Assembly of Imidazolyl-Substituted Nitronyl Nitroxides into Ferromagnetically Coupled Chains

Crystals ◽  
2019 ◽  
Vol 9 (4) ◽  
pp. 219 ◽  
Author(s):  
Vasily Romanov ◽  
Irina Bagryanskaya ◽  
Nina Gritsan ◽  
Dmitry Gorbunov ◽  
Yulia Vlasenko ◽  
...  
Keyword(s):  
Hydrogen Bonds ◽  
Single Crystal ◽  
Spin Density ◽  
Crystalline Form ◽  
Intermolecular Hydrogen Bonds ◽  
X Ray ◽  
Nitronyl Nitroxides

New nitronyl nitroxides, namely, 2-(4,5-dimethylimidazol-2-yl)- and 2-(4,5-dichloroimidazol-2-yl)-4,4,5,5-tetramethyl-4,5-dihydro-1H-imidazol-3-oxide-1-oxyl, were prepared in crystalline form. According to single-crystal X-ray data, intra- and intermolecular hydrogen bonds are formed between NH groups of the imidazole cycles and O atoms of the nitroxide moieties. The intermolecular H-bonds contribute to the alignment of molecules into chains along the a-axis; this alignment causes short intrachain contacts between O and C atoms carrying spin density of opposite signs. Such an arrangement of nitroxides induces ferromagnetic intrachain interactions (J ≈ 10 cm−1) between neighboring radicals.

Heterocyclic Tautomerism. II. 4-Acylpyrazolones. X-Ray Crystal Structures of 4-Benzoyl-5-methyl-2-phenylpyrazol-3(2H)-one and 4-Acetoacetyl-3-methyl-1-phenylpyrazol-5-ol

1985 ◽  
Vol 38 (3) ◽  
pp. 401 ◽  
Author(s):  
MJ O'Connell ◽  
CG Ramsay ◽  
PJ Steel
Keyword(s):  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Room Temperature ◽  
Crystalline Form ◽  
Intermolecular Hydrogen Bonds ◽  
Intramolecular Hydrogen Bonds ◽  
X Ray ◽  
Intramolecular Hydrogen

The colourless crystalline form of the benzoylpyrazolone (2) has molecules with the NH structure (2c) stabilized by intermolecular hydrogen bonds. At room temperature crystals are monoclinic: P21/c, a 13.508(5), b 9.124(4), c 11.451(3)Ǻ, β 90.80(3)°, Z4; the structure was refined to R 0.059, Rw 0.048. The acetoacetylpyrazolone (3) has the OH structure (3c) with two intramolecular hydrogen bonds. At 193 K crystals are triclinic: Pī , a 7.142(2), b 13.704(8), c 14.699(7)Ǻ, α 117.36(3), β 96.87(3), γ 93.73(3)°, Z 4; the structure was refined to R 0.049, Rw 0.054.

scholarly journals ISOLATION AND STRUCTURAL ELUCIDATION OF A NEW DEPSIDE OF LICHEN Everniopsis trulla

2021 ◽  
Vol 87 (2) ◽  
pp. 97-106
Author(s):  
Olivio Nino Castro ◽  
Jesús López Rodilla ◽  
Sofia Pombal ◽  
Francisca Sanz González ◽  
Julio Santiago Contreras
Keyword(s):  
Mass Spectrometry ◽  
Melting Point ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Spectroscopic Data ◽  
Intermolecular Forces ◽  
X Ray Diffraction ◽  
Intermolecular Hydrogen Bonds ◽  
X Ray ◽  
Uv Visible

In this research, a new depside of the lichen Everniopsis trulla has been isolated. The extraction was carried out to 400 g of dry sample and ground with ethanol for 3 repetitions, then, it was fractionated by applying column chromatography with the CHCl3-MeOH system and purified by recrystallization with MeOH-Acetone (1: 1); Finally, white crystals in the form of needles (solid C) with a melting point of 198 ° C were obtained, whose structure was elucidated based on spectroscopic data (UV-Visible, IR, NMR-H1, NMR-C13, mass spectrometry and single crystal X-ray diffraction). According to the Science Finder databases, it is a new depside, called trullarin, and it is observed that molecular packing is influenced by both intramolecular and intermolecular forces. Intermolecular hydrogen bonds of O - H -O type binds neighboring molecules forming dimers.

Study on Novel Structure of Nitric Acid Phenanthroline Vanadium Monohydrate: [ V(C12H8N2) ·O2·(H2O)]·NO3·H2O

2012 ◽  
Vol 554-556 ◽  
pp. 852-855
Author(s):  
Hai Xing Liu ◽  
Jing Zhong Xiao ◽  
Lan Xu ◽  
Vitor Hugo Nunes Rodrigues ◽  
Manuela Ramos Marques da Silva ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Nitric Acid ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Vanadium Complex ◽  
X Ray Diffraction ◽  
Intermolecular Hydrogen Bonds ◽  
X Ray ◽  
Simple Reaction ◽  
Novel Structure

A new vanadium complex [ V(C12H8N2) ·O2·(H2O)]·NO3·H2O h as been synthesized from a simple reaction and the crystal structure has been determined by means of single-crystal X-ray diffraction. Monoclinic, P2(1)/c. a = 9.5137(2) Å b = 19.3181(4) Å c = 7.51800(10) Å α=γ=90 β= 93.6830. V= 1378.85(4) Å3. Z=2. Rgt(F) = 0.0255, wRref(F2) = 0.0809. T= 273(2) K. The compound consisted of a [ V(C12H8N2) ·O2·(H2O)]+ cation, one NO3-anion and one water molecular. Molecule structure is stabilized by OHN , OHO intramolecular and intermolecular hydrogen bonds.

scholarly journals Carbamoyl Derivatives of a Pyridine-Based Tetraamine

2007 ◽  
Vol 62 (4) ◽  
pp. 519-522 ◽  
Author(s):  
Anvarhusen K. Bilakhiya ◽  
Frank W. Heinemann ◽  
Andreas Grohmann
Keyword(s):  
Hydrogen Bonds ◽  
Single Crystal ◽  
Structure Determination ◽  
Spectroscopic Data ◽  
Intermolecular Hydrogen Bonds ◽  
X Ray ◽  
Phenyl Derivative ◽  
High Yields ◽  
Derivatives Of

The reaction of four equivalents of phenyl or tert-butyl isocyanate with the pyridine-derived tetraamine 2,6-C3H3N[CMe(CH2NH2)2]2 in toluene gives high yields of the quadruply ureido substituted products 2,6-C5H3N[CMe(CH2R)2]2 [R = -NH(CO)NHPh and -NH(CO)NHtBu]. Full spectroscopic data for both compounds are given. A single crystal X-ray structure determination of the phenyl derivative reveals an intricate network of both intra- and intermolecular hydrogen bonds involving the C=O and both NH functionalities in all ureido groups.

Study on Novel Structure of Yttrium Complex: C4H12K2O22S2Y2

2012 ◽  
Vol 557-559 ◽  
pp. 394-397
Author(s):  
Hai Xing Liu ◽  
Ting Yan Zhuang ◽  
Qing Zhi Pan ◽  
Hui Juan Yue ◽  
Guang Zeng ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
X Ray Diffraction ◽  
Intermolecular Hydrogen Bonds ◽  
X Ray ◽  
Novel Structure ◽  
Single Solution ◽  
Solution Reaction

A novel Yttrium complex C4H12K2O22S2Y2 has been synthesized from a single solution reaction and the crystal structure has been determined by means of single-crystal X-ray diffraction. The Y1 atom is coordinated by eight O atoms. The crystal is stable by the help of O-H…O intra- and intermolecular hydrogen bonds interaction.

Thermal-induced transformation of glutamic acid to pyroglutamic acid and self-cocrystallization: a charge–density analysis

2022 ◽  
Vol 78 (2) ◽  
Author(s):  
Sehrish Akram ◽  
Arshad Mehmood ◽  
Sajida Noureen ◽  
Maqsood Ahmed
Keyword(s):  
Hydrogen Bonds ◽  
Glutamic Acid ◽  
Single Crystal ◽  
Diffraction Data ◽  
Density Functional ◽  
Quantitative Estimation ◽  
Topological Analysis ◽  
Pyroglutamic Acid ◽  
X Ray Diffraction ◽  
X Ray

Thermal-induced transformation of glutamic acid to pyroglutamic acid is well known. However, confusion remains over the exact temperature at which this happens. Moreover, no diffraction data are available to support the transition. In this article, we make a systematic investigation involving thermal analysis, hot-stage microscopy and single-crystal X-ray diffraction to study a one-pot thermal transition of glutamic acid to pyroglutamic acid and subsequent self-cocrystallization between the product (hydrated pyroglutamic acid) and the unreacted precursor (glutamic acid). The melt upon cooling gave a robust cocrystal, namely, glutamic acid–pyroglutamic acid–water (1/1/1), C5H7NO3·C5H9NO4·H2O, whose structure has been elucidated from single-crystal X-ray diffraction data collected at room temperature. A three-dimensional network of strong hydrogen bonds has been found. A Hirshfeld surface analysis was carried out to make a quantitative estimation of the intermolecular interactions. In order to gain insight into the strength and stability of the cocrystal, the transferability principle was utilized to make a topological analysis and to study the electron-density-derived properties. The transferred model has been found to be superior to the classical independent atom model (IAM). The experimental results have been compared with results from a multipolar refinement carried out using theoretical structure factors generated from density functional theory (DFT) calculations. Very strong classical hydrogen bonds drive the cocrystallization and lend stability to the resulting cocrystal. Important conclusions have been drawn about this transition.

scholarly journals Crystal structure of tris(pyridine)(salicylaldehyde semicarbazonato(2-))cobalt(III)-trichloropyridinecobaltate(II) at 293 and 120K

2007 ◽  
Vol 72 (1) ◽  
pp. 63-71 ◽  
Author(s):  
Goran Bogdanovic ◽  
Vukadin Leovac ◽  
Ljiljana Vojinovic-Jesic ◽  
Biré-Spasojevic De
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Intermolecular Interaction ◽  
Complex Anion ◽  
Octahedral Geometry ◽  
Pyridine Ligand ◽  
Similar Composition ◽  
X Ray ◽  
Preferential Position

The crystal structure of [CoIII(L)(py)3][CoIICl3(py)] (H2L=salicylaldehyde semicarbazone)was determined by X-ray analysis based on two single crystal X-ray experiments performed at 120 K and 293 K, respectively. It was found that the pyridine ligand of the complex anion is disordered over two positions. The preferential position of this pyridine found at120Kwas explained in terms of the C-H...Cl intermolecular interaction between the tetrahedral [CoII(py)Cl3]- anions. The mer-octahedral geometry of the cation in the presented crystal structure was compared with previously published structures of similar composition, [CoIII(L1)(py)3]+[CoIICl3(py)]-?EtOH and [CoIII(LI)(py)3]+I3-(H2LI = salicylaldehyde S-methylisothiosemicarbazone). Although the tetrahedral [CoIICl3(py)]- anions possess the same charge, they mutually form different intermolecular interactions which can be realized either by C-H...Cl hydrogen bonds or by ?-? interactions between the pyridine rings.

Honeycomb molecular network based upon a hydrate of 4,6-dichlororesorcinol and the photoproduct rtct-tetrakis(pyridin-4-yl)cyclobutane

2021 ◽  
Vol 77 (2) ◽  
pp. 111-115
Author(s):  
Carlos L. Santana ◽  
Jessica D. Battle ◽  
Daniel K. Unruh ◽  
Ryan H. Groeneman
Keyword(s):  
Hydrogen Bonds ◽  
Water Molecule ◽  
Single Crystal ◽  
Organic Materials ◽  
Molecular Network ◽  
Molecular Solids ◽  
X Ray ◽  
Bridging Ligand ◽  
Metal Organic ◽  
Cyclobutane Ring

The formation of a self-interpenetrated honeycomb molecular network based upon 4,6-dichlororesorcinol (4,6-diCl res), a water molecule, and the photoproduct rtct-tetrakis(pyridin-4-yl)cyclobutane ( rtct -TPCB) is reported. Interestingly, only three of the four pyridine rings on the central cyclobutane ring are found to engage in O—H...N hydrogen bonds with either the 4,6-diCl res or an included water molecule, resulting in a three-connected net. Notably, the solid (4,6-diCl res)·( rtct -TPCB)·(H2O), C6H4Cl2O2·C24H20N4·H2O, contains channels that run along the crystallographic b axis, which are found to be interpenetrated. Although rtct -TPCB has been employed as a bridging ligand in the formation of numerous metal–organic materials, surprisingly neither the single-component X-ray structure nor any multi-component molecular solids based upon this stereoisomer have been reported previously. Lastly, the single-crystal X-ray structure of the photoproduct rtct -TPCB is also reported.

scholarly journals 1-[N-Methyl-N-(Phenyl)amino]-3- (4-Methylphenyl)Thiourea

Molbank ◽  
10.3390/m1052 ◽  
2019 ◽  
Vol 2019 (1) ◽  
pp. M1052 ◽  
Author(s):  
Chien Yeo ◽  
Edward Tiekink
Keyword(s):  
Hydrogen Bond ◽  
Solid State ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Title Compound ◽  
Molecular Conformation ◽  
Phenyl Hydrazine ◽  
X Ray ◽  
X Ray Crystallography

The title compound, 1-[N-methyl-N-(phenyl)amino]-3-(4-methylphenyl)thiourea (1), was synthesized by the reaction of 1-methyl-1-phenyl hydrazine and 4-tolyl isothiocyanate, and was characterized by spectroscopy (1H and 13C{1H} NMR, IR, and UV), elemental analysis as well as by single crystal X-ray crystallography. In the solid state, the molecule exists as the thioamide tautomer and features an anti-disposition of the thioamide–N–H atoms; an intramolecular N–H⋯N hydrogen bond is noted. The molecular conformation resembles that of the letter L. In the molecular packing, thioamide-N1–H⋯S1(thione) hydrogen bonds lead to centrosymmetric eight-membered {⋯HNCS}2 synthons. The dimers are assembled into a supramolecular layer in the bc-plane by phenyl- and methyl-C–H⋯π(phenyl) interactions.

Zum System Wasser—Fluorwasserstoff: Phasenverhalten und Kristallstruktur von 2 D2O• 3 DF, einer deuterierten Verbindung ohne protoniertes Analogon / Concerning the System Water—Hydrogen Fluoride: Phase Behaviour and Crystal Structure of 2 D2O· 3 DF, a Deuterated Compound Lacking the Protonated Analogue

1989 ◽  
Vol 44 (11) ◽  
pp. 1359-1364 ◽  
Author(s):  
Wolfgang Poll ◽  
Michaela Lohmeyer ◽  
Dietrich Mootz
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Phase Behaviour ◽  
X Ray ◽  
Quasibinary System ◽  
Molecular Adduct ◽  
Oxonium Salt ◽  
System Water ◽  
Additional Phase

The melting diagram of the quasibinary system D2O— DF was determined by low-temperature DTA and X-ray powder diffraction. It was found to be largely similar to that of the corresponding non-deuterated system H2O—HF with the striking exception of an additional phase with a composition of its own, 2D2O· 3 DF, and stable between ca. —78 and —71°C. Its structure, determined from single-crystal MoKā diffractometer data at —150°C, is rhombohedral (space group R3c, Z = 6, a = 769.9, c = 1242.1 pm) and strongly related to that of NH, · 4 HF or NH4[F(HF)3] with also seven H (as to be compared to D) and five non-H (non-D) atoms per formula unit. But with the O atom involved in four hydrogen bonds, one O · · · O and three O · · · F. at distances of 273.9 and 259.5 pm, respectively, the compound appears to be a molecular adduct rather than an oxonium salt. The D atoms in the hydrogen bonds are distributed over two positions each. — The remaining intermediary phases of the deuterated system, i. e. D2O · DF, D2O· 2 DF and D2O · 4 DF, are isotypic to their protonated counterparts of known crystal structure. For D2O · DF and D2O-2 DF these results from powder patterns were confirmed by two more single-crystal studies. The ionic structures — D3OF and D3O[F(DF)], respectively — show no distinctive effect of the H/D substitution even on details of the interatomic geometries.

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