Processable, Chemical Routes to Binary Metal Sulfides

1993 ◽  
Vol 327 ◽  
Author(s):  
William S. Rees ◽  
Gertrud Krauter

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.

1993 ◽  
Vol 327 ◽  
Author(s):  
Gertrud KrÄuter ◽  
Virgil L. Goedken ◽  
Bernhard NeumÜller ◽  
W. S. Rees

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.


1995 ◽  
Vol 410 ◽  
Author(s):  
Rodney D. Schluter ◽  
Gertrude Kräuter ◽  
William S. Rees

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.


2015 ◽  
Vol 71 (4) ◽  
pp. 330-337 ◽  
Author(s):  
Sabina Kovač ◽  
Ljiljana Karanović ◽  
Tamara Đorđević

Two isostructural diarsenates, SrZnAs2O7(strontium zinc diarsenate), (I), and BaCuAs2O7[barium copper(II) diarsenate], (II), have been synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction. The three-dimensional open-framework crystal structure consists of corner-sharingM2O5(M2 = Zn or Cu) square pyramids and diarsenate (As2O7) groups. Each As2O7group shares its five corners with five differentM2O5square pyramids. The resulting framework delimits two types of tunnels aligned parallel to the [010] and [100] directions where the large divalent nine-coordinatedM1 (M1 = Sr or Ba) cations are located. The geometrical characteristics of theM1O9,M2O5and As2O7groups of known isostructural diarsenates, adopting the general formulaM1IIM2IIAs2O7(M1II= Sr, Ba, Pb;M2II= Mg, Co, Cu, Zn) and crystallizing in the space groupP21/n, are presented and discussed.


1999 ◽  
Vol 23 (7) ◽  
pp. 418-419
Author(s):  
Simon J. Coles ◽  
Paul Faulds ◽  
Michael B. Hursthouse ◽  
David G. Kelly ◽  
Georgia C. Ranger ◽  
...  

Nickel(II) phosphine complexes are prepared with a series of diphenylalkenylphosphine ligands and characterised by single crystal X-ray diffraction and spectroscopic techniques.


2008 ◽  
Vol 63 (3) ◽  
pp. 339-341 ◽  
Author(s):  
Ajay Venugopal ◽  
Alexander Willner ◽  
Norbert W. Mitzel

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.


1980 ◽  
Vol 33 (2) ◽  
pp. 313 ◽  
Author(s):  
PR Jefferies ◽  
BW Skelton ◽  
B Walter ◽  
AH White

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.


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