Phosphanchalkogenide und ihre Metallkomplexe. III. Halogenierungsprodukte der Gold(I)komplexe Ph3PEAuX (E = S oder Se; X = Cl, Br oder I)

2015 ◽  
Vol 70 (12) ◽  
pp. 911-927 ◽  
Author(s):  
Christina Taouss ◽  
Peter G. Jones ◽  
Daniel Upmann ◽  
Dirk Bockfeld
Keyword(s):  
Diffuse Scattering ◽  
The Novel ◽  
Iodine Molecule ◽  
X Ray ◽  
Ionic Compounds ◽  
Structure Decomposition ◽  
Elemental Iodine

AbstractThe complexes Ph3PEAuI (E = S, Se; 1, 2) were obtained from the reaction of Ph3PEAuCl with KI; they are appreciably less stable than their chloro and bromo analogues. The X-ray structures were determined, whereby 1 proved to be contaminated by a small amount of Ph3PS·I2. Oxidation of 1 and 2 with elemental iodine led to the adducts Ph3PEAuI·0.5I2 (3 and 4), but X-ray investigation of a crystal initially assumed to be 3 proved it to be a 1:1 mixture of 3 with the adduct Ph3PS·1.5I2, while in 4 the iodine molecule was severely disordered, which prevented successful refinement of the structure. Decomposition of 4 by loss of gold led to Ph3PSeI2·1.5I24a. Complexes Ph3PEAuX (E = S, Se; X = Br, Cl) were oxidized by elemental bromine (X = Br) or PhICl2 (X = Cl) to Ph3PEAuX3 (5, 6, 9, 10); none of these X-ray structures could be refined satisfactorily because of diffuse scattering phenomena. Further oxidation led to the ionic compounds [Ph3PEX]+ [AuX4]– (X = Br, E = S, Se: 7, 8; X = Cl, E = S, 11) or [Ph3PSeCl]+ 0.5[Au4Cl10Se2]2– (12), containing the novel groupings P–E–X. X-ray structures confirmed the nature of all four of these compounds, which display longer P–E bonds than the gold(I) starting materials and short X···X and/or E···X contacts between cations and anions.

Crystal structure and enantiomeric layer disorder of a copper(I) nitrate π-coordination compound

2021 ◽  
Vol 77 (2) ◽  
Author(s):  
Dorota A. Kowalska ◽  
Vasyl Kinzhybalo ◽  
Yuriy I. Slyvka ◽  
Marek Wołcyrz
Keyword(s):  
Coordination Compound ◽  
Local Structure ◽  
Diffuse Scattering ◽  
Weak Interactions ◽  
The Novel ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structure Solution ◽  
First Time ◽  
Layer Disorder

The novel π-coordination compound [CuI(m-dmphast)NO3], where m-dmphast = 5-(allylthio)-1-(3,5-dimethylphenyl)-1H-tetrazole, is characterized using single-crystal X-ray diffraction and crystallizes in a noncentrosymmetric space group. Additionally, for the first time in this group of materials, the streaks of X-ray diffuse scattering in the reciprocal space sections were observed and described. This gave the possibility for a deeper insight into the local structure of the title compound. The conjecture about the origin of diffuse scattering was derived from average structure solution. It was then confirmed using the local structure modelling. The extended [Cu(m-dmphast)NO3]∞ chains, connected by weak interactions, produce layers which can exist in two enantiomeric forms, one of which predominates.

Ten-Vertex Polyhedral Monocarbaborane Chemistry. The Novel High-Yield Formation of the Ten-Vertex closo Compound [6-(PMe2Ph)-closo-1-CB9H9] from the Thermolysis of [8,8-(PMe2Ph)2-nido-8,7-PtCB9H11]

1993 ◽  
Vol 58 (12) ◽  
pp. 2924-2935 ◽  
Author(s):  
Jane H. Jones ◽  
Bohumil Štíbr ◽  
John D. Kennedy ◽  
Mark Thornton-Pett
Keyword(s):  
Nmr Spectroscopy ◽  
Diffraction Analysis ◽  
High Yield ◽  
Monoclinic Space Group ◽  
The Novel ◽  
X Ray Diffraction ◽  
Metal Centre ◽  
X Ray ◽  
Yield Formation ◽  
Boiling Toluene

Thermolysis of [8,8-(PMe2Ph)2-nido-8,7-PtCB9H11] in boiling toluene solution results in an elimination of the platinum centre and cluster closure to give the ten-vertex closo species [6-(PMe2Ph)-closo-1-CB9H9] in 85% yield as a colourles air stable solid. The product is characterized by NMR spectroscopy and single-crystal X-ray diffraction analysis. Crystals (from hexane-dichloromethane) are monoclinic, space group P21/c, with a = 903.20(9), b = 1 481.86(11), c = 2 320.0(2) pm, β = 97.860(7)° and Z = 8, and the structure has been refined to R(Rw) = 0.045(0.051) for 3 281 observed reflections with Fo > 2.0σ(Fo). The clean high-yield elimination of a metal centre from a polyhedral metallaborane or metallaheteroborane species is very rare.

scholarly journals Some Novel Cobalt Diphenylphosphine Complexes: Synthesis, Characterization, and Behavior in the Polymerization of 1,3-Butadiene

Molecules ◽  
2021 ◽  
Vol 26 (13) ◽  
pp. 4067
Author(s):  
Giovanni Ricci ◽  
Giuseppe Leone ◽  
Giorgia Zanchin ◽  
Benedetta Palucci ◽  
Alessandra Forni ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
The Novel ◽  
X Ray Diffraction ◽  
X Ray ◽  
And Behavior

Some novel cobalt diphenylphosphine complexes were synthesized by reacting cobalt(II) chloride with (2-methoxyethyl)diphenylphosphine, (2-methoxyphenyl)diphenylphosphine, and 2-(1,1-dimethylpropyl)-6-(diphenylphosphino)pyridine. Single crystals suitable for X-ray diffraction studies were obtained for the first two complexes, and their crystal structure was determined. The novel compounds were then used in association with methylaluminoxane (MAO) for the polymerization of 1,3-butadiene, and their behavior was compared with that exhibited in the polymerization of the same monomer by the systems CoCl2(PnPrPh2)2/MAO and CoCl2(PPh3)2/MAO. Some significant differences were observed depending on the MAO/Co ratio used, and a plausible interpretation for such a different behavior is proposed.

scholarly journals Reproducibility of protein x-ray diffuse scattering and potential utility for modeling atomic displacement parameters

2021 ◽  
Vol 8 (4) ◽  
pp. 044701
Author(s):  
Zhen Su ◽  
Medhanjali Dasgupta ◽  
Frédéric Poitevin ◽  
Irimpan I. Mathews ◽  
Henry van den Bedem ◽  
...  
Keyword(s):  
Diffuse Scattering ◽  
Atomic Displacement ◽  
Potential Utility ◽  
X Ray ◽  
Protein X ◽  
Atomic Displacement Parameters

scholarly journals The Influence of Varying Fluorination Patterns on the Thermodynamics and Kinetics of Benzenesulfonamide Binding to Human Carbonic Anhydrase II

Biomolecules ◽  
2020 ◽  
Vol 10 (4) ◽  
pp. 509 ◽  
Author(s):  
Steffen Glöckner ◽  
Khang Ngo ◽  
Björn Wagner ◽  
Andreas Heine ◽  
Gerhard Klebe
Keyword(s):  
Carbonic Anhydrase ◽  
Carbonic Anhydrase Ii ◽  
The Novel ◽  
Binding Modes ◽  
X Ray ◽  
Structure Activity ◽  
Small Set ◽  
Novel Method ◽  
Human Carbonic Anhydrase ◽  
Kinetics Of

The fluorination of lead-like compounds is a common tool in medicinal chemistry to alter molecular properties in various ways and with different goals. We herein present a detailed study of the binding of fluorinated benzenesulfonamides to human Carbonic Anhydrase II by complementing macromolecular X-ray crystallographic observations with thermodynamic and kinetic data collected with the novel method of kinITC. Our findings comprise so far unknown alternative binding modes in the crystalline state for some of the investigated compounds as well as complex thermodynamic and kinetic structure-activity relationships. They suggest that fluorination of the benzenesulfonamide core is especially advantageous in one position with respect to the kinetic signatures of binding and that a higher degree of fluorination does not necessarily provide for a higher affinity or more favorable kinetic binding profiles. Lastly, we propose a relationship between the kinetics of binding and ligand acidity based on a small set of compounds with similar substitution patterns.

Evolution of Interfacial Roughness Correlations of Fe Au Films Grown on Mgo(001) Substrates

1996 ◽  
Vol 440 ◽  
Author(s):  
P. C. Chow ◽  
R. Paniago ◽  
R. Forrest ◽  
S. C. Moss ◽  
S. S. P. Parkin ◽  
...  
Keyword(s):  
Thin Films ◽  
Diffuse Scattering ◽  
Perfect Match ◽  
Grazing Incidence ◽  
Interface Roughness ◽  
Metallic Structures ◽  
X Ray ◽  
Dimensional Image ◽  
X Ray Scattering ◽  
Image Plate Detector

AbstractThe growth by sputtering of a series of thin films of Fe/Au on MgO(001) substrates was analyzed using Bragg and diffuse X-ray scattering. The Fe (bcc) layer grows rotated by 45° with respect to the MgO – Au(fcc) (001) epitaxial orientation, resulting in an almost perfect match between the two metallic structures. By collecting the X-ray diffuse scattering under grazing incidence using a 2-dimensional image plate detector, we mapped the reciprocal space of these films. We characterized the correlated interface roughness starting with a buffer of Fe in which only three interfaces are present. The propagation of the roughness was subsequently characterized for Fe/Au multilayers with 40 and 100 bilayers. We observe an enlargement of the surface features as a function of time, evidenced by the longer lateral cutoff length measured for thicker films.

scholarly journals Insertion of Phosphenium Ions into a Bicyclo[1.1.0]Tetraphosphabutane Iron Complex

Molecules ◽  
2021 ◽  
Vol 26 (13) ◽  
pp. 3920
Author(s):  
Martin Weber ◽  
Gábor Balázs ◽  
Alexander V. Virovets ◽  
Eugenia Peresypkina ◽  
Manfred Scheer
Keyword(s):  
Diffraction Analysis ◽  
Room Temperature ◽  
31P Nmr ◽  
Spectroscopic Studies ◽  
Iron Complex ◽  
The Novel ◽  
X Ray Diffraction ◽  
X Ray ◽  
Phosphenium Ions

By reacting [{Cp‴Fe(CO)2}2(µ,η1:1-P4)] (1) with in situ generated phosphenium ions [Ph2P][A] ([A]− = [OTf]− = [O3SCF3]−, [PF6]−), a mixture of two main products of the composition [{Cp‴Fe(CO)2}2(µ,η1:1-P5(C6H5)2)][PF6] (2a and 3a) could be identified by extensive 31P NMR spectroscopic studies at 193 K. Compound 3a was also characterized by X-ray diffraction analysis, showing the rarely observed bicyclo[2.1.0]pentaphosphapentane unit. At room temperature, the novel compound [{Cp‴Fe}(µ,η4:1-P5Ph2){Cp‴(CO)2Fe}][PF6] (4) is formed by decarbonylation. Reacting 1 with in situ generated diphenyl arsenium ions gives short-lived intermediates at 193 K which disproportionate at room temperature into tetraphenyldiarsine and [{Cp‴Fe(CO)2}4(µ4,η1:1:1:1-P8)][OTf]2 (5) containing a tetracyclo[3.3.0.02,7.03,6]octaphosphaoctane ligand.

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