High-resolution dipolar n.m.r. spectra in solids

1981 ◽  
Vol 299 (1452) ◽  
pp. 547-563 ◽  
Keyword(s):  
Molecular Structure ◽  
Solid State ◽  
High Resolution ◽  
Single Crystal ◽  
Two Dimensional ◽  
Dipolar Interactions ◽  
Recent Advances ◽  
Powder Samples ◽  
Successful Observation

Recent advances in solid state n.m.r. spectroscopy permit obervation of high-resolution dipolar spectra, and thus renewed consideration can be given to solid state n.m.r. as a tool for determining molecular structure. This is illustrated with 13 C and 14 N single-crystal spectra obtained with both one- and two-dimensional n.m.r. techniques. The successful observation of these spectra is due to the fact that many dipolar interactions are inhomogeneous, and for this reason it is also possible to obtain high-resolution dipolar spectra from powder samples. Methods that accomplish this goal are described and illustrated with 13 C - 1 H dipolar spectra.

Preparation of single-crystal metal substrates for the growth of high-quality two-dimensional materials

2021 ◽  
Vol 8 (1) ◽  
pp. 182-200
Author(s):  
Yanglizhi Li ◽  
Luzhao Sun ◽  
Haiyang Liu ◽  
Yuechen Wang ◽  
Zhongfan Liu
Keyword(s):  
Single Crystal ◽  
2D Materials ◽  
Controlled Growth ◽  
Two Dimensional ◽  
High Quality ◽  
Metal Substrates ◽  
Recent Advances ◽  
Two Dimensional Materials

Recent advances on preparing single-crystal metals and their crucial roles in controlled growth of high-quality 2D materials are reviewed.

One- and two-dimensional high-resolution solid-state NMR studies of zeolite lattice structures

1991 ◽  
Vol 91 (7) ◽  
pp. 1525-1543 ◽  
Author(s):  
C. A. Fyfe ◽  
Y. Feng ◽  
H. Grondey ◽  
G. T. Kokotailo ◽  
H. Gies
Keyword(s):  
Solid State ◽  
High Resolution ◽  
Solid State Nmr ◽  
Lattice Structures ◽  
Two Dimensional ◽  
Nmr Studies ◽  
Zeolite Lattice

ChemInform Abstract: One- and Two-Dimensional High-Resolution Solid-State NMR Studies of Zeolite Lattice Structures

ChemInform ◽  
2010 ◽  
Vol 23 (5) ◽  
pp. no-no
Author(s):  
C. A. FYFE ◽  
Y. FENG ◽  
H. GRONDEY ◽  
G. T. KOKOTAILO ◽  
H. GIES
Keyword(s):  
Solid State ◽  
High Resolution ◽  
Solid State Nmr ◽  
Lattice Structures ◽  
Two Dimensional ◽  
Nmr Studies ◽  
Zeolite Lattice

scholarly journals Exploration and exploitation of homologous series of bis(acrylamido)alkanes containing pyridyl and phenyl groups: β-sheetversustwo-dimensional layers in solid-state photochemical [2 + 2] reactions

IUCrJ ◽  
2015 ◽  
Vol 2 (5) ◽  
pp. 523-533 ◽  
Author(s):  
Mousumi Garai ◽  
Kumar Biradha
Keyword(s):  
Hydrogen Bonding ◽  
Solid State ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Crystal Structures ◽  
Homologous Series ◽  
Bonding Layer ◽  
Two Dimensional ◽  
Systematic Analysis ◽  
Small Change

The homologous series of phenyl and pyridyl substituted bis(acrylamido)alkanes have been synthesized with the aim of systematic analysis of their crystal structures and their solid-state [2 + 2] reactivities. The changes in the crystal structures with respect to a small change in the molecular structure, that is by varying alkyl spacers between acrylamides and/or by varying the end groups (phenyl, 2-pyridyl, 3-pyridyl, 4-pyridyl) on the C-terminal of the amide, were analyzed in terms of hydrogen-bonding interference (N—H...NpyversusN—H...O=C) and network geometries. In this series, a greater tendency towards the formation of N—H...O hydrogen bonds (β-sheets and two-dimensional networks) over N—H...N hydrogen bonds was observed. Among all the structures seven structures were found to have the required alignments of double bonds for the [2 + 2] reaction such that the formations of single dimer, double dimer and polymer are facilitated. However, only four structures were found to exhibit such a solid-state [2 + 2] reaction to form a single dimer and polymers. The two-dimensional hydrogen-bonding layerviaN—H...O hydrogen bonds was found to promote solid-state [2 + 2] photo-polymerization in a single-crystal-to-single-crystal manner. Such two-dimensional layers were encountered only when the spacer between acryl amide moieties is butyl. Only four out of the 16 derivatives were found to form hydrates, two each from 2-pyridyl and 4-pyridyl derivatives. The water molecules in these structures govern the hydrogen-bonding networks by the formation of an octameric water cluster and one-dimensional zigzag water chains. The trends in the melting points and densities were also analyzed.

Triferrocenylborane – Molecular Structure in Solution and in the Solid State

1995 ◽  
Vol 50 (2) ◽  
pp. 201-204 ◽  
Author(s):  
Bernd Wrackmeyer ◽  
Udo Dörfler ◽  
Wolfgang Milius ◽  
Max Herberhold
Keyword(s):  
Molecular Structure ◽  
Solid State ◽  
Low Temperature ◽  
Single Crystal ◽  
Nmr Spectra ◽  
The Other ◽  
X Ray ◽  
Single Diastereomer ◽  
Structure In Solution ◽  
C Nmr

According to a single crystal X-ray structure determination all three ferrocenyl substituents of triferrocenylborane (1) adopt the same orientation with respect to the BC3-plane [P21/c monoclinic; Z = 4; a = 1353.5(3), b = 1695.6(3), c = 1056.4(2) pm, β = 109.27(3)°]. The simulated X-ray powder pattern of the single crystal is identical with the powder diagram of a macroscopic sample, indicating the presence of a single diastereomer (1a) in the solid state. However, at low temperature (< - 95 °C) in solution, the 13C NMR spectra suggest the presence of the second diastereomer (1b) in which one ferrocenyl group is oriented opposite to the other two with respect to the central BC3-plane.

Different forms of antiparallel stacking of hydrogen-bonded antidromic rings in the solid state: polymorphism with virtually the same unit cell and two-dimensional isostructurality with alternating layers

2004 ◽  
Vol 60 (6) ◽  
pp. 755-762 ◽  
Author(s):  
Alajos Kálmán ◽  
László Fábián ◽  
Gyula Argay ◽  
Gábor Bernáth ◽  
Zsuzsanna Cs. Gyarmati
Keyword(s):  
Hydrogen Bonding ◽  
Solid State ◽  
Single Crystal ◽  
Unit Cell ◽  
Two Dimensional ◽  
Acta Cryst ◽  
Space Group ◽  
Layer Stacking ◽  
Parallel Mode

As a continuation of a systematic structural analysis of 2-hydroxycycloalkanecarboxylic acids and their carboxamide analogs, the effects of antidromic rings [Jeffrey & Saenger (1991). Hydrogen Bonding in Biological Structures. Berlin, Heidelberg: Springer Verlag] upon the layer stacking of cyclopentane and cycloheptane derivatives are compared. Determination of the structure of trans-2-hydroxycycloheptanecarboxylic acid (2) led to the discovery of two polymorphs with virtually the same unit cell [Kálmán et al. (2003). J. Am. Chem. Soc. 125, 34–35]. (i) The layer stacking of the antidromic rings for the whole single crystal is antiparallel (2b). (ii) The antidromic rings and the 21 axis are parallel (2a), consequently the domains of the single crystal must be antiparallel. While their polymorphism is solvent-controlled, they illustrate a novel form of two-dimensional isostructurality. Antiparallel layer stacking is again demonstrated by trans-2-hydroxycycloheptanecarboxamide (3) (space group Pbca). It is built up from layers isostructural with those in the homologous trans-2-hydroxycyclopentanecarboxamide (4) [Kálmán et al. (2001). Acta Cryst. B57, 539–550], but in this structure (space group Pca21) the layers are stacked in parallel mode. Similar to (2a) and (2b), the antiparallel layer stacking in (3) versus their parallel array in (4) illustrates the two-dimensional isostructurality with alternating layer orientations. Although (3) and (4) display isostructurality, they are not isomorphous.

Sign in / Sign up

Export Citation Format

Share Document