Topochemical Studies. XVI. Direct Observation of the Solid-State Photoreaction ofα-(Acetylamino)cinnamic Acid Dihydrate by Single Crystal X-Ray Diffraction

1993 ◽  
Vol 66 (8) ◽  
pp. 2190-2195 ◽  
Author(s):  
Tetsuyuki Iwamoto ◽  
Setsuo Kashino
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Direct Observation ◽  
Cinnamic Acid ◽  
X Ray Diffraction ◽  
X Ray

Photodimerization of the α′-polymorph of ortho-ethoxy-trans-cinnamic acid in the solid state. I. Monitoring the reaction at 293 K

2004 ◽  
Vol 60 (3) ◽  
pp. 315-324 ◽  
Author(s):  
M. A. Fernandes ◽  
D. C. Levendis
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Cinnamic Acid ◽  
Structural Changes ◽  
Uv Light ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cell Parameters ◽  
Short Period

Structural changes that occur during the [2 + 2] photodimerization of the metastable α′-polymorph of ortho-ethoxy-trans-cinnamic acid at 293 K are presented here. Crystals of the α′-polymorph were first stabilized by exposing the α-polymorph to UV light for a short period of time at 343 K. The photodimerization reaction was then carried out at 293 K and observed in situ by single-crystal X-ray diffraction. The α′-polymorph contains three molecules in the asymmetric unit, labelled A, B and C, which are arranged to form two potential reaction sites. The intermolecular distance between the C=C bonds of molecules A and B (making up the AB site) is 3.6 Å, and these were observed to undergo photodimerization at 293 K. The corresponding distance between centrosymmetrically related C=C bonds in the CC site (made up of C molecules) is 4.6 Å, and these remain unreacted even after 60 h irradiation at 293 K. The crystal of the final product, which corresponds to a 66.7% conversion (only two out of three molecules in the asymmetric unit take part in the photodimerization reaction at 293 K), contains an ordered arrangement of the photodimer and unreacted monomer. The crystal retains many structural features of the original monomer crystal, including carboxylic acid hydrogen bonds and C—H...O interactions. Single-crystal X-ray diffraction was used to monitor changes in the unit-cell parameters, reacting molecules and molecular conformations as the reaction progressed. The conformation of the photodimer obtained from the solid-state reaction differs from that of the photodimer obtained by recrystallization from solution.

N–O Bond Cleavage During the Deprotonation of N,O-Bis(trimethylsilyl)hydroxylamine

2008 ◽  
Vol 63 (3) ◽  
pp. 339-341 ◽  
Author(s):  
Ajay Venugopal ◽  
Alexander Willner ◽  
Norbert W. Mitzel
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Bond Cleavage ◽  
State Structure ◽  
X Ray Diffraction ◽  
Solid State Structure ◽  
X Ray ◽  
Potassium Hydride ◽  
Oxygen Atoms

The reaction of N,O-bis(trimethylsilyl)hydroxylamine with potassium hydride in pentane affords a product of the formula {K6[OSiMe3]4[ON(SiMe3)2]2}, resulting from deprotonation followed by N-O bond cleavage and 1,2-silylshift. The compound was characterised by elemental analysis and by single crystal X-ray diffraction. The aggregate consists of a K3O3 bis-cubane core, with N(SiMe3)2 groups at the oxygen atoms shared by the two cubes, andMe3Si groups attached to the four O vertices. Two weak K···N interactions are also detected in the solid state structure.

Crystal structures of some eriostyl/nitrobenzoate derivatives

1980 ◽  
Vol 33 (2) ◽  
pp. 313 ◽  
Author(s):  
PR Jefferies ◽  
BW Skelton ◽  
B Walter ◽  
AH White
Keyword(s):  
Charge Transfer ◽  
Solid State ◽  
Single Crystal ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structure Determinations

Following the suggestion made earlier, on the basis of solution spectroscopy, that a number of eriostyl/nitrobenzoate compounds form charge-transfer self-complexes, a number of these have been investigated structurally by single-crystal X-ray diffraction methods in order to ascertain the presence or otherwise of such interactions in the solid state. The substances thus studied were eriostyl 3,5-dinitrobenzoate (1), eriostyl p-nitrobenzoate (2), tetrahydroeriostyl 3,5-dinitrobenzoate (3), and eriostemyl 3,5-dinitrobenzoate (4);* structure determinations in all cases, although displaying the presence of strong charge-transfer interactions from the two moieties of each molecule, show that the interactions in the solid state are intermolecular in nature.

Notizen: Solid State Structure of N,N-Dibenzylhydroxylamine

1995 ◽  
Vol 50 (4) ◽  
pp. 699-701 ◽  
Author(s):  
Norbert W. Mitzel ◽  
Jürgen Riede ◽  
Klaus Angermaier ◽  
Hubert Schmidbaur
Keyword(s):  
Solid State ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
State Structure ◽  
X Ray Diffraction ◽  
Space Group ◽  
Solid State Structure ◽  
X Ray

The solid-state structure of N,N-dibenzylhydroxylamine (1) has been determined by single crystal X-ray diffraction. The compound crystallizes in the monoclinic space group P 21/n with four formula units in the unit cell. N,N-dibenzylhydroxylamine dimerizes to give N2O2H2 sixmembered rings as a result of the formation of two hydrogen bonds O - H ··· N in the solid state.

scholarly journals A combined single crystal neutron/X-ray diffraction and solid-state nuclear magnetic resonance study of the hybrid perovskites CH3NH3PbX3 (X = I, Br and Cl)

2015 ◽  
Vol 3 (17) ◽  
pp. 9298-9307 ◽  
Author(s):  
Tom Baikie ◽  
Nathan S. Barrow ◽  
Yanan Fang ◽  
Philip J. Keenan ◽  
Peter R. Slater ◽  
...  
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Solid State ◽  
Single Crystal ◽  
Solid State Nmr ◽  
Variable Temperature ◽  
Neutron Diffraction Study ◽  
Nuclear Magnetic Resonance Study ◽  
X Ray Diffraction ◽  
Magnetic Resonance Study ◽  
X Ray

This article describes a variable temperature solid-state NMR and single crystal X-ray/neutron diffraction study of the hybrid perovskites (CH3NH3)PbX3 (X = I, Br and Cl).

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