scholarly journals Different Coordination Modes of a Tripod Phosphine in Gold(I) and Silver(I) Complexes

1999 ◽  
Vol 6 (4-5) ◽  
pp. 211-221 ◽  
Author(s):  
P. Sevillano ◽  
M. E. García ◽  
A. Habtemariam ◽  
S. Parsons ◽  
P. J. Sadler
Keyword(s):  
Mass Spectrometry ◽  
Infrared Spectroscopy ◽  
Nmr Spectroscopy ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
X Ray ◽  
Fab Mass Spectrometry ◽  
Intramolecular Distance ◽  
Spectroscopy Studies ◽  
Linear Coordination

The following gold(I) and silver(I) complexes of the tritertiary phosphine 1,1,1- tris(diphenylphosphinomethyl)ethane, tripod , have been synthesised: Au3(tripod)X3 [X = Cl(1), Br(2), I(3)]; [Au3  (tripod)2Cl2  ]Cl (4); Au(tripod)X [X = Br(5), I(6)]; Ag3(tripod)(NO3)3 (7), Ag(tripod)NO3 (8). They were characterized by X-ray diffraction (complexes 2, 3 and 4), P31 NMR spectroscopy, electrospray and FAB mass spectrometry and infrared spectroscopy. Complexes 2 and 3 show a linear coordination geometry for Au(I), with relatively short Au-P bond distances. Complex 3 has a Au•••Au intramolecular distance of 3.326 A° , while complex 2 had a short Au•••Au intermolecular interaction of 3.048 A° . Complexes 4-6 were found by P31 NMR spectroscopy studies to contain a mixture of species in solution, one of which crystallised as [Au3(tripod|)2Cl2]Cl which was shown by X-ray diffraction to contain both tetrahedral and linear Au(I), the first example of a Au(I) complex containing such a mixture of geometries. The reaction of [Au3(tripod)Cl3] (1) with tripod led successfully to the formation of [Au3(tripod)Cl3][Au3(tripod|)2Cl2]+ and [Au3(tripod|)3Cl]2+ . The silver(I) complexes, 7 and 8 appear to contain linear and tetrahedral Ag(I), respectively.

Thiocarbonyl Complexes of Rhenium. Part I.

1993 ◽  
Vol 48 (6) ◽  
pp. 771-777 ◽  
Author(s):  
Ulrich Abram ◽  
Bernd Lorenz
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
Rhenium Atom ◽  
Space Group ◽  
X Ray ◽  
Monomeric Complex ◽  
Structure Solution ◽  
R Value

Novel rhenium complexes with terminal thiocarbonyl groups have been synthesized from ReCl3(Me2PhP)3 and sodium diethyldithiocarbamate. mer-(Diethyldithiocarbamato)tris-(dimethylphenylphosphine)(thiocarbonyl)rhenium(I), mer-[Re(CS)(Me2PhP)3(Et2dtc)], and tris(diethyldithiocarbamato)(thiocarbonyl)rhenium(III), [Re(CS)(Et2dtc)3] have been studied by infrared and NMR spectroscopy, mass spectrometry and X-ray diffraction.mer-[Re(CS)(Me2PhP)3(Et2dtc)] crystallizes orthorhombic in the space group Pna21 with a = 1516.1(2), b = 2189.8(2) and c = 1035.6(1) pm. Structure solution and refinement converged at R = 0.042. The coordination geometry is a distorted octahedron. The Re—C bond length is found to be 184(2) pm.[Re(CS)(Et2dtc)3] crystallizes monoclinic in the space group P21/c with a = 962.2(6), b = 1744.0(2), c = 1537.4(6) pm and β = 96.21(1)°. The final R value is 0.028. In the monomeric complex the rhenium atom is seven-coordinate with an approximate pentagonal-bipyramidal coordination sphere and a rhenium-carbon distance of 181(1) pm.

scholarly journals Exploring the Structural Chemistry of Pyrophosphoramides: N,N′,N″,N‴-Tetraisopropylpyrophosphoramide

Chemistry ◽  
2021 ◽  
Vol 3 (1) ◽  
pp. 149-163
Author(s):  
Duncan Micallef ◽  
Liana Vella-Zarb ◽  
Ulrich Baisch
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nuclear Magnetic Resonance ◽  
Hydrogen Bonding ◽  
Nmr Spectroscopy ◽  
Ir Spectroscopy ◽  
Room Temperature ◽  
Intermolecular Hydrogen Bonding ◽  
X Ray Diffraction ◽  
X Ray

N,N′,N″,N‴-Tetraisopropylpyrophosphoramide 1 is a pyrophosphoramide with documented butyrylcholinesterase inhibition, a property shared with the more widely studied octamethylphosphoramide (Schradan). Unlike Schradan, 1 is a solid at room temperature making it one of a few known pyrophosphoramide solids. The crystal structure of 1 was determined by single-crystal X-ray diffraction and compared with that of other previously described solid pyrophosphoramides. The pyrophosphoramide discussed in this study was synthesised by reacting iso-propyl amine with pyrophosphoryl tetrachloride under anhydrous conditions. A unique supramolecular motif was observed when compared with previously published pyrophosphoramide structures having two different intermolecular hydrogen bonding synthons. Furthermore, the potential of a wider variety of supramolecular structures in which similar pyrophosphoramides can crystallise was recognised. Proton (1H) and Phosphorus 31 (31P) Nuclear Magnetic Resonance (NMR) spectroscopy, infrared (IR) spectroscopy, mass spectrometry (MS) were carried out to complete the analysis of the compound.

Synthesis and Characterization of Tetrakis(pentafluoroethyl)germane

Synthesis ◽  
2017 ◽  
Vol 49 (11) ◽  
pp. 2389-2393 ◽  
Author(s):  
Stefanie Pelzer ◽  
Beate Neumann ◽  
Hans-Georg Stammler ◽  
Nikolai Ignat’ev ◽  
Reint Eujen ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Ir Spectroscopy ◽  
Diffraction Analysis ◽  
Spectroscopic Characterization ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Comprehensive Characterization

This paper describes the synthesis and comprehensive characterization of tetrakis(pentafluoroethyl)germane. In addition to a complete NMR spectroscopic characterization, including the rarely used 73Ge NMR spectroscopy, Ge(C2F5)4 was studied by IR spectroscopy, mass spectrometry as well as X-ray diffraction analysis. A 73Ge NMR investigation as well as an X-ray diffraction study of the related germane Ge(CF3)4 are also included.

Boron Carbide-Based Ceramics Via Polymer Route Synthesis

1991 ◽  
Vol 249 ◽  
Author(s):  
Haixing Zheng ◽  
Kevin Thorne ◽  
J.D. Mackenzie ◽  
Xiaoguang Yang ◽  
M.F. Hawthome
Keyword(s):  
Thermal Analysis ◽  
Infrared Spectroscopy ◽  
High Temperature ◽  
Nmr Spectroscopy ◽  
Physical Properties ◽  
Boron Carbide ◽  
X Ray Diffraction ◽  
Polymeric Precursors ◽  
X Ray ◽  
Crystalline Boron

ABSTRACTBoron carbide is a ceramic material with excellent high temperature physical properties. As compared to conventional techniques, the preparation of boron carbide from polymeric precursors is attractive as this technique offers a number of unique advantages. In this paper, the screening of polymeric precursors to boron carbide will be discussed. Two promising boron carbide, carborane containing polymeric precursors have resulted in 60-70 wt.% ceramic yields. The chemistry of polymer synthesis and the transformations from the polymer to amorphous and crystalline boron carbide were investigated with infrared spectroscopy, NMR spectroscopy, thermal analysis, and x ray diffraction.

Synchrotron X-ray Diffraction and Infrared Spectroscopy Studies of C60H18under High Pressure

2010 ◽  
Vol 1 (4) ◽  
pp. 714-719 ◽  
Author(s):  
Honglei Ma ◽  
Xuemei Zhang ◽  
Bingbing Liu ◽  
Quanjun Li ◽  
Qifeng Zeng ◽  
...  
Keyword(s):  
High Pressure ◽  
Infrared Spectroscopy ◽  
X Ray Diffraction ◽  
X Ray ◽  
Spectroscopy Studies

Structural Identification of Products from the Chloromethylation of Salicylaldehyde

Synlett ◽  
2018 ◽  
Vol 30 (01) ◽  
pp. 44-48 ◽  
Author(s):  
Muhammad Bala ◽  
Ebrahim Kadwa ◽  
Holger Friedrich
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
High Resolution Mass Spectrometry ◽  
Structural Identification ◽  
Spectroscopic Techniques ◽  
X Ray Diffraction ◽  
X Ray ◽  
Multinuclear Nmr Spectroscopy ◽  
Ir Spectroscopic ◽  
Resolution Mass

In the functionalization of salicylaldehyde to give 5-(chloromethyl)salicylaldehyde, two byproducts [5-(hydroxymethyl)salicylaldehyde and 5,5′-methylenebis(salicylaldehyde)] were also isolated. ­Detailed characterizations and structural analyses of all three products by single-crystal X-ray diffraction, multinuclear NMR spectroscopy, high-resolution mass spectrometry, and IR spectroscopic techniques are presented and discussed. A strategy is presented for the preferential isolation of the two byproducts through column chromatography.

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