Synthesis and X-ray Crystal Structure of the First Mononuclear Nickel(II) Alkane Thiolate Complex with a Mixed (S,N,N,O) Ligand Field

1996 ◽  
Vol 129 (10) ◽  
pp. 1183-1189 ◽  
Author(s):  
Albrecht Berkessel ◽  
Michael Bolte ◽  
Thomas Neumann ◽  
Lutz Seidel
Keyword(s):  
Crystal Structure ◽  
Ligand Field ◽  
X Ray

Missing Link in the Ligand-Field Photolysis of [Mo(CN)8]4-:  Synthesis, X-ray Crystal Structure, and Physicochemical Properties of [Mo(CN)6]2-

2007 ◽  
Vol 46 (23) ◽  
pp. 9531-9533 ◽  
Author(s):  
Janusz Szklarzewicz ◽  
Dariusz Matoga ◽  
Agnieszka Niezgoda ◽  
Daisuke Yoshioka ◽  
Masahiro Mikuriya
Keyword(s):  
Crystal Structure ◽  
Physicochemical Properties ◽  
Ligand Field ◽  
Missing Link ◽  
X Ray

Synthesis, Spectroscopy and Structure of the Cobalt(III) Complex of the Hexadentate Ligand 5-(4-Amino-2-thiabutyl)-5-methyl-3,7-dithianonane-1,9-diamine

1993 ◽  
Vol 46 (11) ◽  
pp. 1799 ◽  
Author(s):  
TM Donlevy ◽  
LR Gahan ◽  
TW Hambley ◽  
KL Mcmahon ◽  
R Stranger
Keyword(s):  
Crystal Structure ◽  
Progressive Increase ◽  
Ligand Field ◽  
Octahedral Symmetry ◽  
X Ray Diffraction ◽  
X Ray ◽  
Hexadentate Ligand ◽  
Symmetry Result ◽  
Ligand Field Parameters ◽  
Systematic Reduction

A revised synthesis of the hexadentate ligand 5-(4-amino-2-thiabutyl)-5-methyl-3,7-dithianon- ane-1,9-diamine (N3S3) is reported. Reaction between the sodium salt of 2-aminoethanethiol and 1,1,1-tris([( tolylsulfonyl )oxy]methyl)ethane in refluxing ethanol results in the formation of the hexadentate ligand N3S3. The preparation of the nickel(II) and cobalt(III) complexes is reported. The crystal structure of [Co(N3S3)](ClO4)3.H2O has been determined by X-ray diffraction methods and refined to a residual of 0.044 for 3696 independent observed reflections. The crystals are monoclinic, P21/n, a 9.314(4), b 15.581(6), c 17.026(3) Ǻ, β 90.30(4)°. Low temperature (c.10 K) absorption spectra are reported for [Co(N3S3)]3+ and the analogous encapsulated complex [Co(AMN3S3sarH)]4+ where both the spin-allowed 1A1g → 1T1g, 1T2g and spin-forbidden 1A1g → 3T1g, 3T2g were observed. Ligand -field calculations based on octahedral symmetry result in the ligand -field parameters B 461, C 3075, Dq 2303 cm-1, and B 462, C 3085, Dq 2266 cm-1 for the [Co(N3S3)]3+ and [Co(AMN3S3sarH)]4+ complexes, respectively. A systematic reduction occurs in the Racah B parameter of between 25 and 30 cm-1 for each additional thioether donor in the series of complexes N6-xSx (x = 0, 1, 2, 3). In addition, there is evidence for a progressive increase in the Racah C/B ratio with increasing number of thioether donors in this series.

Studies of β-Diketone Complexes of Rhenium. I. Trispentane-2,4-dionatorhenium(III) and Tris(1,1,1,5,5,5-hexafluoropentane-2,4-dionato)rhenium(III)

1972 ◽  
Vol 50 (1) ◽  
pp. 8-17 ◽  
Author(s):  
W. D. Courrier ◽  
W. Forster ◽  
C. J. L. Lock ◽  
G. Turner
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Magnetic Susceptibility ◽  
Infrared Spectroscopy ◽  
Physical Properties ◽  
Ligand Field ◽  
X Ray Diffraction ◽  
Rhenium Atom ◽  
X Ray ◽  
Monoclinic Cell

Pure samples2 of Re(hfac)3 and Re(acac)3 have been prepared and their physical properties studied by ultraviolet–visible and infrared spectroscopy, mass spectrometry, magnetic susceptibility measurements, and X-ray diffraction. The compounds are monomeric and the physical properties may be explained if the rhenium atom sits in an essentially octahedral ligand field. Re(hfac)3 has a hexagonal unit cell and the acetyl-acetone complex adopts the monoclinic cell of the α-form of the three typical crystal structure types which Astbury (1) observed for trispentane-2,4-dionatometal(III) compounds. The properties observed for trispentane-2,4-dionatorhenium(III) differ from those reported previously (2, 3). The difficulties experienced in obtaining pure Re(C5H7O2)3 were caused by the ease with which the material is oxidized.

A study on α-RuCl3 crystal structure by scanning tunneling microscopy

1989 ◽  
Vol 47 ◽  
pp. 30-31
Author(s):  
H.-J. Cantow ◽  
H. Hillebrecht ◽  
S. Magonov ◽  
H. W. Rotter ◽  
G. Thiele
Keyword(s):  
Crystal Structure ◽  
Density Distribution ◽  
Scanning Tunneling Microscopy ◽  
Electron Density ◽  
Structure Determination ◽  
Electron Density Distribution ◽  
Scanning Tunneling ◽  
Monoclinic Space Group ◽  
Tunneling Microscopy ◽  
X Ray

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.

X-ray Crystal Structure of ?9-THC-tosylate

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

Crystal structure of an inclusion complex between chiral monoaza-15-crown-5 and S(–)-1-phenyl-ethyl ammonium percholorate

2003 ◽  
Vol 218 (5) ◽  
Author(s):  
Süheyla Özbey ◽  
F. B. Kaynak ◽  
M. Toğrul ◽  
N. Demirel ◽  
H. Hoşgören
Keyword(s):  
Crystal Structure ◽  
Inclusion Complex ◽  
Single Crystal ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
New Type

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

Single Crystal Growth of High-Pressure Phases of Ice and Salt Hydrate Far Below the Original Melting Point by Mixing Alcohol: Crystal Structure Determination of Magnesium Chloride Heptahydrate

2020 ◽  
Author(s):  
Keishiro Yamashita ◽  
Kazuki Komatsu ◽  
Hiroyuki Kagi
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
Crystal Growth ◽  
Single Crystal ◽  
Room Temperature ◽  
Growth Technique ◽  
Salt Hydrate ◽  
X Ray

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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