Synthesis of high-nuclearity carbonyl–phosphine clusters of palladium under mild conditions and X-ray crystal structure of Pd38(µ3-CO)4(µ2-CO)24(PEt3)12

Author(s):  
Eugenii G. Mednikov ◽  
Nikolai K. Eremenko ◽  
Yuri L. Slovokhotov ◽  
Yuri T. Struchkov
1990 ◽  
Vol 43 (1) ◽  
pp. 79 ◽  
Author(s):  
MA Rizzacasa ◽  
MV Sargent ◽  
BW Skelton ◽  
AH White

Henry reaction between 3,5-dimethoxybenzaldehyde (2) and nitroethane gave (E)-2-(3,5-dimethoxyphenyl)-1-methyl-1-nitroethene (3). Under mild conditions the erythro and threo nitro aldols intermediate in this reaction could be isolated as their acetates. The threo isomer was obtained in diastereoisomeric excess. The nitrostyrene (3) was converted in several steps into cis-(20) and trans-5-bromo-6,8-dimethoxy-1,2,3-trimethyl-1,2,3,4-tetrahydroisoquinoline (18). The single-crystal X-ray structure of compound (18) is reported.


2005 ◽  
Vol 77 (9) ◽  
pp. 1529-1538 ◽  
Author(s):  
George I. Chilas ◽  
Haralampos N. Miras ◽  
Manolis J. Manos ◽  
J. Derek Woollins ◽  
Alexandra M. Z. Slawin ◽  
...  

Reaction of VIVOCl2 in strongly acidic aqueous solution with either (NH4)2SO3 or Na2SO3 and Bu4NBr at ~70°C in the pH range 2.5-4.5 gives the clusters (NH4)2{[V4IV(μ4-O)2(μ3-OH)2](VIVO)2(μ3-SO3)4O4(H2O)2} and (n-Bu4N)2{[V4IV(μ4-O)2(μ3-OH)2](VIVO)2(μ3-SO3)4O4(H2O)2}, respectively. Reaction of NH4VVO3 with (NH4)2SO3 resulted in the isolation of the first compound. When the latter reaction is carried out in the presence of MgO, compound (NH4)[VIVO(SO3)1.5H2O]∞.2.5H2O was isolated instead. Compound (n-Bu4N)2{[V4IV(μ4-O)2(μ3-OH)2](VIVO)2(μ3-SO3)4O4(H2O)2} and (NH4)[VIVO(SO3)1.5H2O]∞.2.5H2O were characterized by X-ray structure analysis. The crystal structure of species (n-Bu4N)2{[V4IV(μ4-O)2(μ3-OH)2](VIVO)2(μ3-SO3)4O4(H2O)2} revealed a unprecedented hexanuclear cluster consisting of a cubane core [M4(μ4-O)2(μ3-OH)2] connected to two other metal atoms through the core oxo-groups and four μ3-SO3 bridges. Compound (NH4)[VIVO(SO3)1.5H2O]∞.2.5H2O represents a rare example of an open-framework species prepared under mild conditions. Cyclic voltammetric examination of compound (n-Bu4N)2{[V4IV(μ4-O)2(μ3-OH)2](VIVO)2(μ3-SO3)4O4(H2O)2} revealed a redox process which was assigned to the oxidation of one core of vanadium(IV) to vanadium(V).


2013 ◽  
Vol 750-752 ◽  
pp. 1104-1108 ◽  
Author(s):  
Feng Rao Lang ◽  
Li Yan You

The Zn (II) complex [Zn (O2CFcCO2)(H2O)2]H2O was synthesized with ferrocenedicarboxylic acid under mild conditions. Its crystal structure was characterized by elemental analysis, IR data and X-ray diffraction single crystal structure analyses. The Zn (II) coordination units are connected, forming one-dimensional chain. At the meanwhile, the luminescence properties and the electronic properties were determined.


Author(s):  
H.-J. Cantow ◽  
H. Hillebrecht ◽  
S. Magonov ◽  
H. W. Rotter ◽  
G. Thiele

From X-ray analysis, the conclusions are drawn from averaged molecular informations. Thus, limitations are caused when analyzing systems whose symmetry is reduced due to interatomic interactions. In contrast, scanning tunneling microscopy (STM) directly images atomic scale surface electron density distribution, with a resolution up to fractions of Angstrom units. The crucial point is the correlation between the electron density distribution and the localization of individual atoms, which is reasonable in many cases. Thus, the use of STM images for crystal structure determination may be permitted. We tried to apply RuCl3 - a layered material with semiconductive properties - for such STM studies. From the X-ray analysis it has been assumed that α-form of this compound crystallizes in the monoclinic space group C2/m (AICI3 type). The chlorine atoms form an almost undistorted cubic closed package while Ru occupies 2/3 of the octahedral holes in every second layer building up a plane hexagon net (graphite net). Idealizing the arrangement of the chlorines a hexagonal symmetry would be expected. X-ray structure determination of isotypic compounds e.g. IrBr3 leads only to averaged positions of the metal atoms as there exist extended stacking faults of the metal layers.


Planta Medica ◽  
2008 ◽  
Vol 74 (03) ◽  
Author(s):  
W Gul ◽  
P Carvalho ◽  
D Slade ◽  
M Avery ◽  
JR Duchek ◽  
...  
Keyword(s):  

Author(s):  
Süheyla Özbey ◽  
F. B. Kaynak ◽  
M. Toğrul ◽  
N. Demirel ◽  
H. Hoşgören

AbstractA new type of inclusion complex, S(–)-1 phenyl ethyl ammonium percholorate complex of R-(–)-2-ethyl - N - benzyl - 4, 7, 10, 13 - tetraoxa -1- azacyclopentadecane, has been prepared and studied by NMR, IR and single crystal X-ray diffraction techniques. The compound crystallizes in space group


2020 ◽  
Author(s):  
Keishiro Yamashita ◽  
Kazuki Komatsu ◽  
Hiroyuki Kagi

An crystal-growth technique for single crystal x-ray structure analysis of high-pressure forms of hydrogen-bonded crystals is proposed. We used alcohol mixture (methanol: ethanol = 4:1 in volumetric ratio), which is a widely used pressure transmitting medium, inhibiting the nucleation and growth of unwanted crystals. In this paper, two kinds of single crystals which have not been obtained using a conventional experimental technique were obtained using this technique: ice VI at 1.99 GPa and MgCl<sub>2</sub>·7H<sub>2</sub>O at 2.50 GPa at room temperature. Here we first report the crystal structure of MgCl2·7H2O. This technique simultaneously meets the requirement of hydrostaticity for high-pressure experiments and has feasibility for further in-situ measurements.


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