Unimolecular Precursors to Binary Metal Sulfides: Mechanistic and Structural Correlations

1995 ◽  
Vol 410 ◽  
Author(s):  
Rodney D. Schluter ◽  
Gertrude Kräuter ◽  
William S. Rees
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Metal Sulfides ◽  
X Ray Diffraction ◽  
Decomposition Products ◽  
X Ray ◽  
Binary Metal ◽  
Solid State Decomposition

ABSTRACTThe roles which ligand size and stability play in influencing solid-state thermolyses products and phases are developed for a group of metal thiolate compounds. The exploration includes Pb(SR)2 [R = t-Bu, i-Bu, s-Bu], Cd(SR*)2 [ R* = i-Pr, I-Bu, Bz], ClHgSR** [ R** = i- Pr, neo-Pent, Bz] and In(SR***)3 [R*** = 2,4,6-(i-Pr)3C6H2, 2-CH3O-5-CH3C6H3, o- C6H4CH2N(CH3)2]. In several examples, the precursors have been characterized by single crystal X-ray diffraction. In most cases, solid-state decomposition products have been identified by XRPD, and volatile decomposition products have been identified by GC/MS. All precursors have been studied by TGA.

Group 12 Thiolates: Syntheses, Characterization and Decomposition Pathways

1993 ◽  
Vol 327 ◽  
Author(s):  
Gertrud KrÄuter ◽  
Virgil L. Goedken ◽  
Bernhard NeumÜller ◽  
W. S. Rees
Keyword(s):  
Particle Size ◽  
Thermal Treatment ◽  
Single Crystal ◽  
Metal Sulfides ◽  
Size Determination ◽  
X Ray Diffraction ◽  
X Ray ◽  
Binary Metal ◽  
Group 12 ◽  
Particle Size Determination

AbstractZinc- and cadmium bis(alkylthiolate) compounds have been prepared and converted into the appropriate binary metal sulfides by thermal treatment. Several mercury chlorothiolates have been synthesized and characterized by single crystal X-ray diffraction. Their decomposition pathways are discussed. The prepared binary metal sulfides have been studied by XRPD and - in selected cases - by particle size determination. The volatile co-products have been isolated and characterized by GC/MS.

Preparation and Characterization of Group 12 Thiolate Complexes and Evaluation of Their Potential as Precursors for II-VI Semiconductors

1992 ◽  
Vol 283 ◽  
Author(s):  
William S. Rees ◽  
Gertrud Kräutern ◽  
Virgil L. Goedken
Keyword(s):  
Solid State ◽  
Metal Sulfides ◽  
X Ray Diffraction ◽  
Decomposition Products ◽  
X Ray ◽  
Molecular Precursors ◽  
Group 12 ◽  
Potential Sources ◽  
Thiolate Complexes

ABSTRACTWe have prepared compounds having the general formula M(SR)2 (M = Zn, Cd; R = i-Pr, t-Bu, Bz) and Hg(SR)CI (R = i-Pr, Bz) and investigated their use as potential sources in the preparation of metal sulfides from molecular precursors. Selected examples of the prepared compounds have been studied by single crystal x-ray diffraction. Decomposition has been carried out both in the solid state and by heating a suspension of a metal thiolate in a high boiling hydrocarbon. The decomposition products have been studied by GC/MS (liquids) and XRD (solids).

Processable, Chemical Routes to Binary Metal Sulfides

1993 ◽  
Vol 327 ◽  
Author(s):  
William S. Rees ◽  
Gertrud Krauter
Keyword(s):  
Particle Size ◽  
Solid State ◽  
Single Crystal ◽  
General Formula ◽  
Metal Sulfides ◽  
Spectroscopic Techniques ◽  
Size Determination ◽  
X Ray Diffraction ◽  
X Ray ◽  
Particle Size Determination

AbstractMetal thiolates of the general formula M(SR)2 (M = Pb, Zn, Cd) and Cl-Hg-SR (R = alkyl) have been prepared and characterized by spectroscopic techniques, TGA and, in selected cases, single crystal X-ray diffraction. The metal bis(thiolate) compounds can be converted into the related metal sulfides by thermolyses. The solid state materials have been characterized by XRPD, SEM and, in selected cases, by particle size determination. The volatile pyrolytic co-products have been isolated and characterized by GC/MS. The decomposition pathways of mercury chlorothiolates are more complicated and depend on the nature of the organic group present in Cl-Hg-SR.

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.

Multinuclear NMR and Powder X-ray Diffraction Studies of Si and Sn Clathrates of Alkali Metals: Vacancies, Disorder and Knight Shifts

2001 ◽  
Vol 691 ◽  
Author(s):  
Michael J. Ferguson ◽  
Igor L. Moudrakovski ◽  
Christopher I. Ratcliffe ◽  
John S. Tse
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
Nmr Spectra ◽  
Alkali Metals ◽  
Rietveld Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Multinuclear Nmr ◽  
Binary Metal ◽  
Knight Shifts

ABSTRACTThe Structure I type binary metal clathrates of K/Si, Rb/Si and Cs/Sn have been synthesised and studied by powder X-ray diffraction and solid state NMR. Rietveld analysis shows that in all three materials some of the cages are empty, and that in the Cs/Sn clathrate there are vacancies in the Sn framework. The NMR results yield Knight shifts for 29Si and 39K and confirm that the Cs/Sn clathrate is not conducting. Many of the features of the NMR spectra can be understood in terms of the distributions of atom vacancies.

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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