scholarly journals Prevalence of the thioamide {⋯H–N–CS}2 synthon—solid-state (X-ray crystallography), solution (NMR) and gas-phase (theoretical) structures of O-methyl-N-aryl-thiocarbamides

CrystEngComm ◽  
2005 ◽  
Vol 7 (113) ◽  
pp. 682 ◽  
Author(s):  
Soo Yei Ho ◽  
Ryan P. A. Bettens ◽  
Dainis Dakternieks ◽  
Andrew Duthie ◽  
Edward R. T. Tiekink
Keyword(s):  
Solid State ◽  
Gas Phase ◽  
Solution Nmr ◽  
X Ray ◽  
X Ray Crystallography

scholarly journals Bleaching the Record: After 200 Years, Single Crystal X-Ray Crystallography Reveals the Structure and Hydrogen-Bonding Properties of Hypochlorite and Hypobromite Ions in the Solid State

2021 ◽  
Author(s):  
Filip Topic ◽  
Joseph Marrett ◽  
Tristan Borchers ◽  
Hatem M. Titi ◽  
Christopher J. Barrett ◽  
...  
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Gas Phase ◽  
X Ray ◽  
X Ray Crystallography ◽  
Single Crystal Structures ◽  
Hypohalous Acids ◽  
Bonding Properties ◽  
Insight Into

<div>We report the first single crystal structures of hypochlorite and hypobromite salts, including hydrated sodium hypochlorite - a ubiquitous bleaching and disinfection agent in use for almost 200 years. The structures represent the first characterization of fundamentally important hypochlorite and hypobromite anions in the solid state, by X-ray crystallography and are supported by Raman spectroscopy on individual crystals. The structural analysis provides insight into supramolecular chemistry of the hypohalite ions in the hydrated environment of the NaOCl<sup>.</sup>5H<sub>2</sub>O and NaOBr<sup>.</sup>5H<sub>2</sub>O solid salts, and reveals measured Cl-O and Br-O bond lengths of 1.69 A and 1.82 A, respectively, which are significantly longer than those for corresponding higher-valence oxoanions, and in agreement with the values spectroscopically determined for hypohalous acids and corresponding oxides in the gas phase.<br></div>

scholarly journals Bleaching the Record: After 200 Years, Single Crystal X-Ray Crystallography Reveals the Structure and Hydrogen-Bonding Properties of Hypochlorite and Hypobromite Ions in the Solid State

2021 ◽  
Author(s):  
Filip Topic ◽  
Joseph Marrett ◽  
Tristan Borchers ◽  
Hatem M. Titi ◽  
Christopher J. Barrett ◽  
...  
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Gas Phase ◽  
X Ray ◽  
X Ray Crystallography ◽  
Single Crystal Structures ◽  
Hypohalous Acids ◽  
Bonding Properties ◽  
Insight Into

<div>We report the first single crystal structures of hypochlorite and hypobromite salts, including hydrated sodium hypochlorite - a ubiquitous bleaching and disinfection agent in use for almost 200 years. The structures represent the first characterization of fundamentally important hypochlorite and hypobromite anions in the solid state, by X-ray crystallography and are supported by Raman spectroscopy on individual crystals. The structural analysis provides insight into supramolecular chemistry of the hypohalite ions in the hydrated environment of the NaOCl<sup>.</sup>5H<sub>2</sub>O and NaOBr<sup>.</sup>5H<sub>2</sub>O solid salts, and reveals measured Cl-O and Br-O bond lengths of 1.69 A and 1.82 A, respectively, which are significantly longer than those for corresponding higher-valence oxoanions, and in agreement with the values spectroscopically determined for hypohalous acids and corresponding oxides in the gas phase.<br></div>

Structures of the 2:1 adducts of benzyne with 2-methylanisole and benzene

2007 ◽  
Vol 85 (7-8) ◽  
pp. 461-465
Author(s):  
Christopher O Bender ◽  
René T Boeré ◽  
Peter W Dibble ◽  
Ryan T McKay
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Gas Phase ◽  
Nmr Spectra ◽  
X Ray Diffraction ◽  
Dft Methods ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Data Points

The 2:1 adduct of benzyne with 2-methylanisole is shown to have the bisbenzotricyclic structure 6,6a,11,11a-tetrahydro-5-methoxy-6-methyl-5,6,11-metheno-5H-benzo[a]fluorene by a single-crystal X-ray diffraction study (C20H18O: Pca21, a = 15.0497(17), b = 9.87783(11), c = 9.6846(11); Z = 4; 1672 data points, R1 = 0.0325). This structure is compared to an unpublished crystal structure of the parent hydrocarbon 6,6a,11,11a-tetrahydro-5,6,11-metheno-5H-benzo[a]fluorene, C18H14. Both structures have also been computed by DFT methods at the B3LYP/6-311(d,p) level of theory. Bond distances and angles between the solid-state measurements and gas-phase calculations are found to agree well; average deviations are well below 1%. The 1H NMR spectra show surprisingly small 3JHH couplings in the central tricyclic cage, but can be assigned using 2D spectroscopy.Key words: Hydrocarbon cages, strained rings, cyclopropane, X-ray crystallography, NMR.

The Structure of 1H-Perimidin-2(3H)-one and Its Derivatives in the solid state (x-ray crystallography and CP/MAS13C-NMR), in solution (13C-NMR), and in the gas phase (mass spectrometry)

1994 ◽  
Vol 77 (1) ◽  
pp. 121-139 ◽  
Author(s):  
Rosa M. Claramunt ◽  
Julio Dotor ◽  
Dionisia Sanz ◽  
Concepci�n Foces-Foces ◽  
Antonio L. Llamas-Saniz ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Solid State ◽  
Gas Phase ◽  
13C Nmr ◽  
X Ray ◽  
X Ray Crystallography

Solid-state and gas-phase structures of two conformers of N-(4-methylphenyl)-N′,N′′-bis(morpholinyl) phosphoric triamide; insights from X-ray crystallography and DFT calculations

2011 ◽  
Vol 67 (3) ◽  
pp. 238-243 ◽  
Author(s):  
Khodayar Gholivand ◽  
Hamid Reza Mahzouni
Keyword(s):  
Hydrogen Bonding ◽  
Solid State ◽  
Dft Calculations ◽  
Gas Phase ◽  
Bond Critical Point ◽  
X Ray ◽  
X Ray Crystallography ◽  
Equal Chance ◽  
Phosphoric Triamide ◽  
Hydrogen Bonded

A phosphoric triamide with the formula (4-CH3—C6H4NH)P(O)(NC4H8O)2 has been synthesized and characterized. X-ray crystallography at 120 K reveals that the title compound is composed of two symmetrically independent molecules in the solid state. Density functional theory (DFT) calculations reveal that two conformers A and B are very close to each other from an energy point of view. Thus there is equal chance that the presence of two conformers in the lattice may lead to hydrogen-bonded chains with an ABABAB arrangement. Hydrogen bonds of the type OP...H—N (OP being the phosphoryl O atom) are established between the two conformers with binding energies of −18.8 and −20.3 kJ mol−1 (at B3LYP/6–31+G*). The electronic delocalization LP(OP) → σ*(N—H), LP(OP) being the lone pair of OP, leads to a decrease in the strength of the N—H bond during hydrogen bonding between the conformers. The charge density (ρ) at the bond critical point (b.c.p.) of N—H decreases by ∼ 0.012–0.014 e Å–3 when the molecule participates in hydrogen bonding. This may explain the red shift of the ν(N—H) stretching frequency from a single molecule in the gas phase to a hydrogen-bonded one in the solid state.

scholarly journals A Mixed-metal Mixed-halide Complex Prepared from Zerovalent Copper and Lead Salts: Solution and Solid-state Chemistry

1999 ◽  
Vol 23 (11) ◽  
pp. 670-671
Author(s):  
Larisa A. Kovbasyuk ◽  
Olga Yu. Vassilyeva ◽  
Vladimir N. Kokozay ◽  
Wolfgang Linert ◽  
Paul R. Raithby
Keyword(s):  
Solid State ◽  
Direct Interaction ◽  
Solid State Chemistry ◽  
X Ray ◽  
Mixed Metal ◽  
X Ray Crystallography ◽  
Halide Complex ◽  
Layer Arrangement ◽  
Lead Salts

The mixed-metal mixed-halide complex [CuPbBrlL2]2 has been prepared by the direct interaction of zerovalent copper with lead halides and 2-dimethylaminoethanol (HL) in dmso and has been characterized by X-ray crystallography; the structure shows a layer arrangement of the tetranuclear metal units through the μ3-halogen bridging.

Bis(1-phenyl-1-propyne) complexes of tungsten(II): crystal structures of [WI2(CO)(NCR)(η2-MeC2Ph)2] (R = Me, Et, or Ph)

2001 ◽  
Vol 79 (3) ◽  
pp. 263-271
Author(s):  
Paul K Baker ◽  
Michael GB Drew ◽  
Deborah S Evans
Keyword(s):  
Carbon Monoxide ◽  
Solid State ◽  
Crystal Structures ◽  
Octahedral Geometry ◽  
X Ray ◽  
X Ray Crystallography ◽  
Alkyne Complexes ◽  
First Time

Reaction of [WI2(CO)3(NCMe)2] with two equivalents of 1-phenyl-1-propyne (MeC2Ph) in CH2Cl2, and in the absence of light, gave the bis(1-phenyl-1-propyne) complex [WI2(CO)(NCMe)(η2-MeC2Ph)2] (1) in 77% yield. Treatment of equimolar quantities of 1 and NCR (R = Et, i-Pr, t-Bu, Ph) in CH2Cl2 afforded the nitrile-exchanged products, [WI2(CO)(NCR)(η2-MeC2Ph)2] (2-5) (R = Et (2), i-Pr (3), t-Bu (4), Ph (5)). Complexes 1, 2, and 5 were structurally characterized by X-ray crystallography. All three structures have the same pseudo-octahedral geometry, with the equatorial sites being occupied by cis and parallel alkyne groups, which are trans to the cis-iodo groups. The trans carbon monoxide and acetonitrile ligands occupy the axial sites. In structures 1 and 2, the methyl and phenyl substituents of the 1-phenyl-1-propyne ligands are cis to each other, whereas for the bulkier NCPh complex (5), the methyl and phenyl groups are trans to one another. This is the first time that this arrangement has been observed in the solid state in bis(alkyne) complexes of this type.Key words: bis(1-phenyl-1-propyne), carbonyl, nitrile, diiodo, tungsten(II), crystal structures.

Synthesis and structural characterization of a magnesium phthalocyanine(3–) anion

2012 ◽  
Vol 16 (01) ◽  
pp. 154-162 ◽  
Author(s):  
Edwin W.Y. Wong ◽  
Daniel B. Leznoff
Keyword(s):  
Absorption Spectrum ◽  
Solid State ◽  
Single Crystal ◽  
Structural Characterization ◽  
Heterometallic Complex ◽  
State Structure ◽  
Solid State Structure ◽  
X Ray ◽  
X Ray Crystallography

The reduction of magnesium phthalocyanine (MgPc) with 2.2 equivalents of potassium graphite in 1,2-dimethoxyethane (DME) gives [K2(DME)4]PcMg(OH)(1) in 67% yield. Compound 1 was structurally characterized using single crystal X-ray crystallography and was found to be a monomeric, heterometallic complex consisting of a μ3-OH ligand that bridges a [MgIIPc3-]- anion to two potassium cations solvated by four DME molecules. An absorption spectrum of 1 confirms the Pc ligand is singly reduced and has a 3–charge. The solid-state structure of 1 does not indicate breaking of the aromaticity of the Pc ligand. Compound 1 is only the second Pc3- complex and the first reduced MgPc to be isolated and structurally characterized.

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